# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name M.Mazzanti _publ_contact_author_email marinella.mazzanti@cea.fr loop_ _publ_author_name M.Mazzanti C.Camp V.Guidal J.Pecaut L.Dubois B.Biswas data_cc311 _database_code_depnum_ccdc_archive 'CCDC 877719' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H75 K N7 Nd O10' _chemical_formula_weight 1465.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7976(3) _cell_length_b 23.2598(5) _cell_length_c 20.8144(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.145(2) _cell_angle_gamma 90.00 _cell_volume 7159.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9003 _cell_measurement_theta_min 3.3723 _cell_measurement_theta_max 32.3405 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 -1 0 0.0235 -0.0001 -1.0009 0.0000 0.0071 0.0047 0.0293 1 0 0 0.3380 1.0004 -0.0004 0.0005 -0.0039 0.0474 -0.0067 -1 0 0 0.3380 -1.0004 0.0004 -0.0005 0.0039 -0.0474 0.0067 0 -1 0 0.0338 -0.0001 -1.0009 0.0000 0.0071 0.0047 0.0293 0 1 0 0.0338 0.0001 1.0009 -0.0000 -0.0071 -0.0047 -0.0293 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3028 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6047 _exptl_absorpt_correction_T_max 0.9629 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73989 _diffrn_reflns_av_R_equivalents 0.0789 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 28.28 _reflns_number_total 17732 _reflns_number_gt 12084 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 4.00 94.00 1.0000 100.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 57.0000 90.0000 90 #__ type_ start__ end____ width___ exp.time_ 2 omega 4.00 81.00 1.0000 100.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 57.0000 -180.0000 77 #__ type_ start__ end____ width___ exp.time_ 3 omega -56.00 42.00 1.0000 100.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 77.0000 90.0000 98 #__ type_ start__ end____ width___ exp.time_ 4 omega -57.00 35.00 1.0000 100.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 77.0000 -150.0000 92 #__ type_ start__ end____ width___ exp.time_ 5 omega -5.00 95.00 1.0000 100.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 77.0000 -60.0000 100 #__ type_ start__ end____ width___ exp.time_ 6 omega -103.00 -65.00 1.0000 100.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 -179.0000 -120.0000 38 ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0425P)^2^+1.7655P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17732 _refine_ls_number_parameters 1079 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.010 _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 Nd1 Nd 0.481816(12) 0.713050(8) 0.627250(8) 0.01639(5) Uani 1 1 d . . . O1 O 0.56722(15) 0.64688(10) 0.57173(11) 0.0205(5) Uani 1 1 d . . . O2 O 0.58541(16) 0.69312(10) 0.71204(11) 0.0247(5) Uani 1 1 d . . . N1 N 0.55773(18) 0.76199(12) 0.52961(13) 0.0193(6) Uani 1 1 d . . . N2 N 0.59494(19) 0.80057(12) 0.64794(13) 0.0209(6) Uani 1 1 d . . . C1 C 0.5770(2) 0.63488(15) 0.51145(16) 0.0193(7) Uani 1 1 d . . . C2 C 0.5896(2) 0.57630(15) 0.49287(17) 0.0238(8) Uani 1 1 d . . . C3 C 0.5970(2) 0.56322(18) 0.42833(19) 0.0295(9) Uani 1 1 d . . . H3 H 0.603(2) 0.5269(14) 0.4186(15) 0.014(9) Uiso 1 1 d . . . C4 C 0.5980(3) 0.60505(18) 0.3806(2) 0.0332(9) Uani 1 1 d . . . H4 H 0.600(3) 0.5947(17) 0.3343(19) 0.041(12) Uiso 1 1 d . . . C5 C 0.5910(3) 0.66142(17) 0.39798(18) 0.0286(9) Uani 1 1 d . . . H5 H 0.592(3) 0.6890(16) 0.3650(18) 0.030(11) Uiso 1 1 d . . . C6 C 0.5796(2) 0.67795(15) 0.46244(16) 0.0215(7) Uani 1 1 d . . . C7 C 0.5774(2) 0.73868(16) 0.47586(17) 0.0221(8) Uani 1 1 d . . . H7 H 0.597(2) 0.7634(14) 0.4421(15) 0.015(9) Uiso 1 1 d . . . C8 C 0.5644(2) 0.82243(15) 0.53627(16) 0.0211(7) Uani 1 1 d . . . C9 C 0.5497(3) 0.86165(16) 0.48629(18) 0.0283(8) Uani 1 1 d . . . H9 H 0.537(2) 0.8463(16) 0.4443(18) 0.030(10) Uiso 1 1 d . . . C10 C 0.5575(3) 0.92027(17) 0.4980(2) 0.0359(10) Uani 1 1 d . . . H10 H 0.545(3) 0.9441(17) 0.4645(18) 0.034(11) Uiso 1 1 d . . . C11 C 0.5782(3) 0.93998(17) 0.5586(2) 0.0365(10) Uani 1 1 d . . . H11 H 0.577(2) 0.9786(16) 0.5668(16) 0.026(10) Uiso 1 1 d . . . C12 C 0.5916(3) 0.90152(17) 0.6094(2) 0.0308(9) Uani 1 1 d . . . H12 H 0.603(3) 0.9153(17) 0.6497(19) 0.039(12) Uiso 1 1 d . . . C13 C 0.5853(2) 0.84270(15) 0.59869(17) 0.0226(7) Uani 1 1 d . . . C14 C 0.6566(3) 0.80827(17) 0.69268(18) 0.0261(8) Uani 1 1 d . . . H14 H 0.694(2) 0.8392(15) 0.6886(16) 0.021(10) Uiso 1 1 d . . . C15 C 0.6802(2) 0.77065(17) 0.74599(17) 0.0273(8) Uani 1 1 d . . . C16 C 0.7482(3) 0.7900(2) 0.7909(2) 0.0363(10) Uani 1 1 d . . . H16 H 0.771(3) 0.8258(19) 0.783(2) 0.051(14) Uiso 1 1 d . . . C17 C 0.7762(3) 0.7562(2) 0.8421(2) 0.0440(12) Uani 1 1 d . . . H17 H 0.816(3) 0.7664(19) 0.873(2) 0.049(13) Uiso 1 1 d . . . C18 C 0.7376(3) 0.7027(2) 0.85000(18) 0.0385(11) Uani 1 1 d . . . H18 H 0.759(3) 0.6796(17) 0.8865(18) 0.035(11) Uiso 1 1 d . . . C19 C 0.6727(2) 0.68101(18) 0.80761(17) 0.0300(9) Uani 1 1 d . . . C20 C 0.6423(2) 0.71482(17) 0.75334(15) 0.0240(7) Uani 1 1 d . . . C21 C 0.5927(3) 0.53133(16) 0.54415(19) 0.0340(9) Uani 1 1 d . . . H21A H 0.6500 0.5343 0.5691 0.051 Uiso 1 1 calc R . . H21B H 0.5880 0.4932 0.5243 0.051 Uiso 1 1 calc R . . H21C H 0.5422 0.5370 0.5726 0.051 Uiso 1 1 calc R . . C22 C 0.6315(3) 0.62339(18) 0.81601(18) 0.0391(11) Uani 1 1 d . . . H22A H 0.6463 0.5987 0.7797 0.059 Uiso 1 1 calc R . . H22B H 0.5657 0.6273 0.8178 0.059 Uiso 1 1 calc R . . H22C H 0.6554 0.6061 0.8561 0.059 Uiso 1 1 calc R . . O31 O 0.37719(16) 0.69424(10) 0.54324(11) 0.0228(5) Uani 1 1 d . . . O32 O 0.39895(16) 0.64660(10) 0.68359(10) 0.0205(5) Uani 1 1 d . . . N31 N 0.37008(18) 0.80222(12) 0.60599(13) 0.0203(6) Uani 1 1 d . . . N32 N 0.40685(19) 0.76348(12) 0.72440(13) 0.0201(6) Uani 1 1 d . . . C31 C 0.3228(2) 0.71724(16) 0.50057(15) 0.0210(7) Uani 1 1 d . . . C32 C 0.2937(2) 0.68376(17) 0.44539(17) 0.0265(8) Uani 1 1 d . . . C33 C 0.2306(3) 0.7062(2) 0.40247(18) 0.0341(10) Uani 1 1 d . . . H33 H 0.211(3) 0.6814(18) 0.363(2) 0.046(12) Uiso 1 1 d . . . C34 C 0.1922(3) 0.7608(2) 0.40995(19) 0.0373(10) Uani 1 1 d . . . H34 H 0.151(3) 0.7734(19) 0.378(2) 0.054(14) Uiso 1 1 d . . . C35 C 0.2209(3) 0.7939(2) 0.46107(19) 0.0330(9) Uani 1 1 d . . . H35 H 0.196(3) 0.8298(17) 0.4694(18) 0.033(11) Uiso 1 1 d . . . C36 C 0.2873(2) 0.77401(15) 0.50667(16) 0.0230(8) Uani 1 1 d . . . C37 C 0.3095(2) 0.81121(16) 0.56033(17) 0.0239(8) Uani 1 1 d . . . H37 H 0.274(2) 0.8460(16) 0.5614(16) 0.026(10) Uiso 1 1 d . . . C38 C 0.3796(2) 0.84419(15) 0.65526(16) 0.0223(7) Uani 1 1 d . . . C39 C 0.3720(3) 0.90378(16) 0.6445(2) 0.0312(9) Uani 1 1 d . . . H39 H 0.361(2) 0.9182(16) 0.6009(18) 0.029(10) Uiso 1 1 d . . . C40 C 0.3846(3) 0.94208(18) 0.6952(2) 0.0376(10) Uani 1 1 d . . . H40 H 0.373(3) 0.9778(16) 0.6885(17) 0.028(11) Uiso 1 1 d . . . C41 C 0.4055(3) 0.92158(17) 0.7566(2) 0.0353(10) Uani 1 1 d . . . H41 H 0.416(3) 0.9482(17) 0.7919(19) 0.040(12) Uiso 1 1 d . . . C42 C 0.4126(3) 0.86345(17) 0.7678(2) 0.0292(9) Uani 1 1 d . . . H42 H 0.429(3) 0.8535(16) 0.8079(18) 0.030(11) Uiso 1 1 d . . . C43 C 0.3995(2) 0.82410(14) 0.71764(16) 0.0207(7) Uani 1 1 d . . . C44 C 0.3859(2) 0.73998(16) 0.77810(17) 0.0226(8) Uani 1 1 d . . . H44 H 0.363(2) 0.7626(16) 0.8134(17) 0.030(10) Uiso 1 1 d . . . C45 C 0.3859(2) 0.67911(15) 0.79205(16) 0.0212(7) Uani 1 1 d . . . C46 C 0.3739(3) 0.66352(17) 0.85662(17) 0.0274(8) Uani 1 1 d . . . H46 H 0.367(2) 0.6927(15) 0.8896(17) 0.027(10) Uiso 1 1 d . . . C47 C 0.3702(3) 0.60726(18) 0.87548(19) 0.0341(10) Uani 1 1 d . . . H47 H 0.363(3) 0.5977(17) 0.9157(19) 0.039(12) Uiso 1 1 d . . . C48 C 0.3775(3) 0.56453(17) 0.82931(19) 0.0346(9) Uani 1 1 d . . . H48 H 0.382(3) 0.5251(17) 0.8451(18) 0.036(11) Uiso 1 1 d . . . C49 C 0.3890(3) 0.57690(15) 0.76524(17) 0.0270(8) Uani 1 1 d . . . C50 C 0.3922(2) 0.63572(15) 0.74429(16) 0.0206(7) Uani 1 1 d . . . C51 C 0.3335(3) 0.62497(16) 0.43893(18) 0.0325(9) Uani 1 1 d . . . H51A H 0.3995 0.6280 0.4376 0.049 Uiso 1 1 calc R . . H51B H 0.3097 0.6071 0.3992 0.049 Uiso 1 1 calc R . . H51C H 0.3175 0.6014 0.4758 0.049 Uiso 1 1 calc R . . C52 C 0.4027(3) 0.53021(16) 0.71602(19) 0.0425(11) Uani 1 1 d . . . H52A H 0.4030 0.4926 0.7373 0.064 Uiso 1 1 calc R . . H52B H 0.4606 0.5362 0.6956 0.064 Uiso 1 1 calc R . . H52C H 0.3535 0.5316 0.6833 0.064 Uiso 1 1 calc R . . K1 K 0.97897(5) 0.60139(4) 0.59771(4) 0.03010(19) Uani 1 1 d . . . O61 O 1.10812(16) 0.51398(11) 0.59453(13) 0.0329(6) Uani 1 1 d . . . O62 O 0.94136(17) 0.48630(11) 0.61154(13) 0.0337(6) Uani 1 1 d . . . O63 O 0.80694(16) 0.57029(11) 0.62571(12) 0.0290(6) Uani 1 1 d . . . O64 O 0.85438(15) 0.68883(11) 0.61588(12) 0.0267(6) Uani 1 1 d . . . O65 O 1.02152(15) 0.71686(11) 0.60071(12) 0.0278(5) Uani 1 1 d . . . O66 O 1.15674(17) 0.63027(11) 0.59053(13) 0.0326(6) Uani 1 1 d . . . C61 C 1.0849(2) 0.45840(16) 0.57750(18) 0.0287(8) Uani 1 1 d . . . C62 C 1.1435(3) 0.41812(19) 0.55393(19) 0.0344(9) Uani 1 1 d . . . H62 H 1.200(3) 0.4267(17) 0.5476(18) 0.035(12) Uiso 1 1 d . . . C63 C 1.1135(3) 0.36229(19) 0.54083(19) 0.0365(10) Uani 1 1 d . . . H63 H 1.156(2) 0.3353(16) 0.5266(17) 0.027(10) Uiso 1 1 d . . . C64 C 1.0250(3) 0.34817(18) 0.54937(19) 0.0356(10) Uani 1 1 d . . . H64 H 1.003(3) 0.3090(18) 0.5440(19) 0.044(12) Uiso 1 1 d . . . C65 C 0.9643(3) 0.38908(18) 0.57123(19) 0.0341(9) Uani 1 1 d . . . H65 H 0.903(3) 0.3804(16) 0.5760(18) 0.035(11) Uiso 1 1 d . . . C66 C 0.9945(3) 0.44360(16) 0.58631(17) 0.0281(8) Uani 1 1 d . . . C67 C 0.8498(3) 0.47165(18) 0.6249(2) 0.0331(9) Uani 1 1 d . . . H67A H 0.815(3) 0.4646(15) 0.5847(18) 0.029(10) Uiso 1 1 d . . . H67B H 0.849(3) 0.4305(18) 0.6481(19) 0.044(12) Uiso 1 1 d . . . C68 C 0.8112(3) 0.51975(18) 0.6634(2) 0.0338(9) Uani 1 1 d . . . H68A H 0.755(2) 0.5113(15) 0.6746(16) 0.020(9) Uiso 1 1 d . . . H68B H 0.844(3) 0.5270(17) 0.7021(19) 0.035(12) Uiso 1 1 d . . . C69 C 0.7595(3) 0.61571(18) 0.6570(2) 0.0312(9) Uani 1 1 d . . . H69A H 0.697(2) 0.6038(14) 0.6626(15) 0.016(9) Uiso 1 1 d . . . H69B H 0.782(3) 0.6168(19) 0.697(2) 0.050(14) Uiso 1 1 d . . . C70 C 0.7621(2) 0.66938(17) 0.6171(2) 0.0279(8) Uani 1 1 d . . . H70A H 0.725(3) 0.7006(15) 0.6316(17) 0.028(10) Uiso 1 1 d . . . H70B H 0.738(2) 0.6655(15) 0.5688(17) 0.025(10) Uiso 1 1 d . . . C71 C 0.8677(2) 0.74005(16) 0.58451(17) 0.0257(8) Uani 1 1 d . . . C72 C 0.7988(3) 0.77554(17) 0.56088(18) 0.0291(9) Uani 1 1 d . . . H72 H 0.740(3) 0.7635(16) 0.5665(17) 0.030(10) Uiso 1 1 d . . . C73 C 0.8198(3) 0.82621(19) 0.5296(2) 0.0364(10) Uani 1 1 d . . . H73 H 0.774(3) 0.8469(18) 0.5133(18) 0.039(12) Uiso 1 1 d . . . C74 C 0.9087(3) 0.84136(19) 0.5211(2) 0.0390(10) Uani 1 1 d . . . H74 H 0.924(3) 0.876(2) 0.494(2) 0.065(15) Uiso 1 1 d . . . C75 C 0.9779(3) 0.80547(18) 0.5442(2) 0.0330(9) Uani 1 1 d . . . H75 H 1.037(3) 0.8173(17) 0.5387(19) 0.040(12) Uiso 1 1 d . . . C76 C 0.9586(2) 0.75493(16) 0.57597(16) 0.0250(8) Uani 1 1 d . . . C77 C 1.1143(3) 0.72889(19) 0.5884(2) 0.0309(9) Uani 1 1 d . . . H77A H 1.129(3) 0.7629(18) 0.6035(18) 0.031(11) Uiso 1 1 d . . . H77B H 1.121(3) 0.7264(16) 0.5488(19) 0.031(12) Uiso 1 1 d . . . C78 C 1.1724(3) 0.68471(17) 0.6208(2) 0.0300(9) Uani 1 1 d . . . H78A H 1.157(3) 0.6832(16) 0.6638(19) 0.031(11) Uiso 1 1 d . . . H78B H 1.241(3) 0.6947(15) 0.6197(17) 0.032(11) Uiso 1 1 d . . . C79 C 1.2172(3) 0.58801(18) 0.6156(2) 0.0357(10) Uani 1 1 d . . . H79A H 1.282(3) 0.6029(18) 0.6074(19) 0.048(12) Uiso 1 1 d . . . H79B H 1.208(2) 0.5884(16) 0.6601(19) 0.029(11) Uiso 1 1 d . . . C80 C 1.1992(3) 0.5317(2) 0.5825(2) 0.0376(10) Uani 1 1 d . . . H80A H 1.238(2) 0.5054(15) 0.5977(16) 0.017(9) Uiso 1 1 d . . . H80B H 1.211(3) 0.533(2) 0.531(2) 0.069(16) Uiso 1 1 d . . . N81 N 0.9977(4) 0.6091(2) 0.7340(2) 0.0713(14) Uani 1 1 d . . . C81 C 0.9637(4) 0.6463(3) 0.7729(3) 0.0754(18) Uani 1 1 d . . . H81 H 0.9220 0.6730 0.7541 0.090 Uiso 1 1 calc R . . C82 C 0.9810(4) 0.6517(3) 0.8383(3) 0.0783(19) Uani 1 1 d . . . H82 H 0.9502 0.6791 0.8633 0.094 Uiso 1 1 calc R . . C83 C 1.0438(5) 0.6159(4) 0.8648(3) 0.099(3) Uani 1 1 d . . . H83 H 1.0594 0.6175 0.9095 0.118 Uiso 1 1 calc R . . C84 C 1.0845(6) 0.5772(5) 0.8260(4) 0.148(4) Uani 1 1 d . . . H84 H 1.1304 0.5523 0.8428 0.177 Uiso 1 1 calc R . . C85 C 1.0572(5) 0.5749(4) 0.7606(3) 0.117(3) Uani 1 1 d . . . H85 H 1.0839 0.5466 0.7344 0.140 Uiso 1 1 calc R . . N82 N 0.8733(4) 0.4329(3) 0.9789(3) 0.0901(17) Uani 1 1 d . . . C86 C 0.8113(5) 0.4697(4) 0.9985(4) 0.097(2) Uani 1 1 d . . . H86 H 0.7844 0.4628 1.0385 0.116 Uiso 1 1 calc R . . C87 C 0.7842(5) 0.5174(3) 0.9634(5) 0.104(3) Uani 1 1 d . . . H87 H 0.7388 0.5424 0.9784 0.125 Uiso 1 1 calc R . . C88 C 0.8235(5) 0.5276(3) 0.9073(4) 0.095(2) Uani 1 1 d . . . H88 H 0.8076 0.5606 0.8825 0.114 Uiso 1 1 calc R . . C89 C 0.8838(5) 0.4914(3) 0.8878(4) 0.104(3) Uani 1 1 d . . . H89 H 0.9117 0.4974 0.8479 0.125 Uiso 1 1 calc R . . C90 C 0.9063(5) 0.4459(3) 0.9240(3) 0.105(3) Uani 1 1 d . . . H90 H 0.9506 0.4206 0.9080 0.126 Uiso 1 1 calc R . . N92 N 0.0652(7) 0.6017(4) 0.2384(4) 0.152(3) Uani 1 1 d U . . C96 C 0.1546(5) 0.6859(4) 0.2310(3) 0.094(2) Uani 1 1 d U . . H96 H 0.2077 0.7076 0.2236 0.113 Uiso 1 1 calc R . . C97 C 0.0750(5) 0.7094(5) 0.2447(3) 0.129(3) Uani 1 1 d U . . H97 H 0.0745 0.7502 0.2455 0.155 Uiso 1 1 calc R . . C98 C 0.1509(6) 0.6315(4) 0.2290(4) 0.106(3) Uani 1 1 d U . . H98 H 0.2040 0.6099 0.2213 0.127 Uiso 1 1 calc R . . C99 C -0.0139(10) 0.6258(5) 0.2476(5) 0.165(4) Uani 1 1 d U . . H99 H -0.0704 0.6065 0.2481 0.198 Uiso 1 1 calc R . . C100 C 0.0006(6) 0.6861(5) 0.2568(5) 0.146(3) Uani 1 1 d U . . H100 H -0.0469 0.7091 0.2724 0.176 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 Nd1 0.01485(8) 0.01993(9) 0.01440(8) -0.00213(8) 0.00042(6) 0.00199(9) O1 0.0172(12) 0.0233(13) 0.0211(12) -0.0040(10) 0.0019(10) 0.0033(10) O2 0.0228(13) 0.0306(14) 0.0204(13) -0.0012(10) -0.0045(10) 0.0048(11) N1 0.0197(15) 0.0200(14) 0.0183(15) -0.0023(12) 0.0017(12) -0.0013(12) N2 0.0206(15) 0.0237(16) 0.0182(15) -0.0062(11) 0.0005(12) 0.0028(12) C1 0.0090(15) 0.0240(18) 0.0249(18) -0.0083(15) 0.0004(13) -0.0023(13) C2 0.0147(17) 0.028(2) 0.029(2) -0.0112(15) 0.0001(14) 0.0009(15) C3 0.0191(18) 0.030(2) 0.040(2) -0.0192(18) 0.0002(16) 0.0011(16) C4 0.029(2) 0.043(2) 0.028(2) -0.0194(19) 0.0062(17) -0.0057(18) C5 0.028(2) 0.034(2) 0.025(2) -0.0078(17) 0.0076(16) -0.0054(17) C6 0.0188(17) 0.0263(19) 0.0196(18) -0.0075(14) 0.0015(14) -0.0018(15) C7 0.0238(19) 0.0244(18) 0.0183(18) -0.0021(15) 0.0040(15) -0.0055(15) C8 0.0168(17) 0.0226(18) 0.0240(19) -0.0012(14) -0.0007(14) 0.0000(14) C9 0.035(2) 0.0246(19) 0.025(2) -0.0006(16) -0.0028(17) -0.0024(17) C10 0.048(3) 0.025(2) 0.034(2) 0.0047(18) -0.002(2) -0.0011(19) C11 0.050(3) 0.018(2) 0.042(3) -0.0019(18) 0.000(2) 0.0012(19) C12 0.034(2) 0.028(2) 0.030(2) -0.0075(17) -0.0019(17) -0.0040(17) C13 0.0209(18) 0.0215(18) 0.0255(19) -0.0048(14) 0.0032(14) -0.0015(15) C14 0.024(2) 0.028(2) 0.027(2) -0.0097(16) 0.0050(16) -0.0003(17) C15 0.0208(18) 0.040(2) 0.0206(18) -0.0100(16) -0.0028(14) 0.0047(16) C16 0.029(2) 0.043(3) 0.035(2) -0.014(2) -0.0088(17) 0.003(2) C17 0.037(3) 0.063(3) 0.030(2) -0.017(2) -0.0174(19) 0.011(2) C18 0.035(2) 0.061(3) 0.0188(19) -0.0033(19) -0.0080(16) 0.017(2) C19 0.0240(19) 0.047(2) 0.0194(19) -0.0013(17) 0.0007(15) 0.0120(18) C20 0.0204(17) 0.036(2) 0.0153(16) -0.0073(16) -0.0001(13) 0.0096(17) C21 0.033(2) 0.026(2) 0.042(2) -0.0085(17) -0.0069(18) 0.0017(17) C22 0.039(2) 0.058(3) 0.020(2) 0.0123(19) 0.0020(17) 0.014(2) O31 0.0194(13) 0.0268(13) 0.0219(13) 0.0006(10) -0.0041(10) -0.0020(10) O32 0.0263(13) 0.0188(12) 0.0165(12) -0.0015(9) 0.0026(10) -0.0008(10) N31 0.0179(14) 0.0237(16) 0.0196(15) 0.0019(11) 0.0047(12) 0.0001(12) N32 0.0203(15) 0.0205(14) 0.0195(15) -0.0040(12) 0.0007(12) 0.0027(12) C31 0.0142(15) 0.0308(19) 0.0183(16) 0.0046(15) 0.0035(13) -0.0049(15) C32 0.0214(18) 0.037(2) 0.0208(19) 0.0054(16) 0.0010(15) -0.0113(16) C33 0.030(2) 0.052(3) 0.0196(19) 0.0078(19) -0.0053(15) -0.017(2) C34 0.029(2) 0.056(3) 0.027(2) 0.017(2) -0.0106(17) -0.008(2) C35 0.0249(19) 0.044(3) 0.030(2) 0.0134(19) -0.0003(16) 0.0016(19) C36 0.0173(16) 0.032(2) 0.0196(17) 0.0080(14) 0.0026(13) -0.0013(15) C37 0.0203(18) 0.0269(19) 0.025(2) 0.0085(15) 0.0073(15) 0.0030(16) C38 0.0199(17) 0.0237(18) 0.0237(19) -0.0003(14) 0.0059(14) 0.0024(15) C39 0.034(2) 0.022(2) 0.038(2) 0.0033(17) 0.0056(18) 0.0035(17) C40 0.040(2) 0.019(2) 0.054(3) -0.0011(19) 0.006(2) 0.0050(19) C41 0.036(2) 0.028(2) 0.042(3) -0.0148(19) 0.010(2) -0.0029(19) C42 0.031(2) 0.026(2) 0.030(2) -0.0066(17) 0.0022(17) 0.0014(17) C43 0.0202(17) 0.0185(17) 0.0236(18) -0.0029(14) 0.0038(14) 0.0059(14) C44 0.0231(19) 0.0247(19) 0.0203(18) -0.0062(15) 0.0030(15) 0.0017(15) C45 0.0217(18) 0.0225(18) 0.0197(18) -0.0028(14) 0.0061(14) 0.0009(15) C46 0.033(2) 0.031(2) 0.0189(19) -0.0027(16) 0.0056(16) 0.0031(17) C47 0.051(3) 0.036(2) 0.0159(19) 0.0067(17) 0.0062(18) 0.001(2) C48 0.047(3) 0.025(2) 0.031(2) 0.0070(17) -0.0035(19) -0.0005(19) C49 0.038(2) 0.0220(19) 0.0211(19) 0.0001(15) -0.0023(16) 0.0022(16) C50 0.0183(17) 0.0225(18) 0.0212(18) -0.0020(14) 0.0007(14) 0.0026(14) C51 0.034(2) 0.039(2) 0.024(2) -0.0022(17) -0.0007(16) -0.0108(18) C52 0.074(3) 0.024(2) 0.030(2) -0.0015(17) -0.008(2) 0.012(2) K1 0.0175(4) 0.0315(4) 0.0414(5) 0.0055(4) 0.0026(3) -0.0014(3) O61 0.0157(13) 0.0327(15) 0.0502(17) -0.0055(13) 0.0027(12) -0.0032(11) O62 0.0189(13) 0.0309(15) 0.0517(18) -0.0019(13) 0.0058(12) -0.0044(11) O63 0.0213(13) 0.0321(14) 0.0340(15) 0.0026(12) 0.0085(11) -0.0011(11) O64 0.0155(12) 0.0314(14) 0.0332(15) 0.0011(11) 0.0025(10) -0.0030(11) O65 0.0161(12) 0.0309(14) 0.0366(14) 0.0039(12) 0.0021(10) -0.0029(11) O66 0.0204(13) 0.0335(15) 0.0435(16) -0.0019(12) -0.0030(11) -0.0032(12) C61 0.0251(19) 0.032(2) 0.029(2) -0.0016(16) -0.0021(16) -0.0006(16) C62 0.029(2) 0.042(2) 0.032(2) -0.0007(18) 0.0011(18) 0.0018(19) C63 0.045(3) 0.036(2) 0.028(2) -0.0047(18) -0.0001(19) 0.007(2) C64 0.048(3) 0.027(2) 0.032(2) -0.0019(17) -0.0011(19) -0.006(2) C65 0.035(2) 0.034(2) 0.033(2) 0.0013(17) -0.0002(18) -0.0052(19) C66 0.029(2) 0.026(2) 0.029(2) -0.0014(16) 0.0010(16) 0.0021(16) C67 0.022(2) 0.032(2) 0.046(3) 0.0059(19) 0.0031(18) -0.0074(17) C68 0.025(2) 0.040(2) 0.037(2) 0.0051(19) 0.0061(19) -0.0043(19) C69 0.0190(19) 0.043(2) 0.033(2) -0.0030(19) 0.0087(17) -0.0040(17) C70 0.0139(17) 0.033(2) 0.037(2) -0.0052(17) 0.0065(16) 0.0007(16) C71 0.0234(19) 0.030(2) 0.0240(19) -0.0034(16) 0.0022(15) -0.0013(16) C72 0.0192(18) 0.038(2) 0.030(2) -0.0052(16) 0.0013(15) 0.0047(17) C73 0.031(2) 0.043(3) 0.035(2) 0.0030(19) -0.0039(18) 0.010(2) C74 0.041(3) 0.033(2) 0.044(3) 0.0096(19) 0.002(2) 0.000(2) C75 0.024(2) 0.037(2) 0.038(2) 0.0020(18) 0.0017(17) -0.0049(17) C76 0.0222(19) 0.028(2) 0.0244(19) -0.0013(15) -0.0002(14) -0.0006(15) C77 0.0196(19) 0.035(2) 0.038(3) 0.0008(18) 0.0037(17) -0.0067(17) C78 0.0199(19) 0.034(2) 0.036(2) 0.0002(18) -0.0007(17) -0.0062(17) C79 0.020(2) 0.037(2) 0.050(3) 0.000(2) -0.0039(18) -0.0004(18) C80 0.018(2) 0.041(3) 0.054(3) -0.005(2) 0.0023(19) 0.0006(18) N81 0.071(3) 0.090(4) 0.052(3) 0.012(3) -0.009(2) -0.006(3) C81 0.071(4) 0.076(4) 0.076(4) -0.006(3) -0.030(3) -0.011(3) C82 0.063(4) 0.105(5) 0.067(4) -0.015(4) -0.011(3) -0.021(4) C83 0.072(5) 0.169(8) 0.054(4) 0.007(5) -0.002(4) -0.021(5) C84 0.093(6) 0.269(13) 0.080(6) 0.032(7) -0.005(5) 0.071(7) C85 0.112(6) 0.183(9) 0.056(4) 0.005(5) 0.020(4) 0.052(6) N82 0.099(4) 0.098(4) 0.074(4) 0.019(3) 0.014(3) 0.015(4) C86 0.093(6) 0.104(6) 0.096(6) -0.030(5) 0.033(5) -0.028(5) C87 0.058(4) 0.073(5) 0.184(9) -0.048(5) 0.029(5) 0.004(4) C88 0.065(5) 0.062(4) 0.156(8) 0.009(5) -0.012(5) 0.010(4) C89 0.125(7) 0.091(5) 0.098(5) 0.046(4) 0.029(5) 0.048(5) C90 0.120(6) 0.109(6) 0.090(5) 0.043(4) 0.041(5) 0.055(5) N92 0.165(8) 0.150(7) 0.144(6) 0.008(5) 0.048(6) -0.021(6) C96 0.072(5) 0.147(7) 0.063(4) 0.026(5) -0.006(3) 0.005(5) C97 0.054(4) 0.256(9) 0.079(5) 0.022(5) 0.019(4) 0.014(5) C98 0.095(6) 0.130(7) 0.093(5) 0.006(5) 0.010(4) 0.033(6) C99 0.205(10) 0.113(7) 0.179(8) 0.013(7) 0.044(8) 0.045(8) C100 0.092(6) 0.203(9) 0.148(7) 0.013(7) 0.059(5) 0.012(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 Nd1 O32 2.318(2) . ? Nd1 O1 2.326(2) . ? Nd1 O31 2.333(2) . ? Nd1 O2 2.340(2) . ? Nd1 N1 2.619(3) . ? Nd1 N32 2.620(3) . ? Nd1 N2 2.660(3) . ? Nd1 N31 2.679(3) . ? O1 C1 1.299(4) . ? O2 C20 1.284(4) . ? N1 C7 1.286(4) . ? N1 C8 1.416(4) . ? N2 C14 1.291(5) . ? N2 C13 1.421(4) . ? C1 C2 1.430(5) . ? C1 C6 1.431(5) . ? C2 C3 1.386(5) . ? C2 C21 1.494(5) . ? C3 C4 1.391(6) . ? C3 H3 0.87(3) . ? C4 C5 1.365(5) . ? C4 H4 1.00(4) . ? C5 C6 1.412(5) . ? C5 H5 0.94(4) . ? C6 C7 1.441(5) . ? C7 H7 0.96(3) . ? C8 C9 1.394(5) . ? C8 C13 1.406(5) . ? C9 C10 1.389(5) . ? C9 H9 0.96(4) . ? C10 C11 1.365(6) . ? C10 H10 0.90(4) . ? C11 C12 1.394(6) . ? C11 H11 0.91(4) . ? C12 C13 1.389(5) . ? C12 H12 0.91(4) . ? C14 C15 1.446(5) . ? C14 H14 0.92(4) . ? C15 C16 1.420(5) . ? C15 C20 1.425(5) . ? C16 C17 1.375(6) . ? C16 H16 0.92(4) . ? C17 C18 1.382(7) . ? C17 H17 0.88(4) . ? C18 C19 1.376(5) . ? C18 H18 0.97(4) . ? C19 C20 1.435(5) . ? C19 C22 1.485(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O31 C31 1.292(4) . ? O32 C50 1.296(4) . ? N31 C37 1.299(4) . ? N31 C38 1.419(4) . ? N32 C44 1.292(4) . ? N32 C43 1.421(4) . ? C31 C36 1.428(5) . ? C31 C32 1.440(5) . ? C32 C33 1.371(5) . ? C32 C51 1.497(5) . ? C33 C34 1.402(6) . ? C33 H33 1.03(4) . ? C34 C35 1.368(6) . ? C34 H34 0.93(5) . ? C35 C36 1.419(5) . ? C35 H35 0.93(4) . ? C36 C37 1.441(5) . ? C37 H37 0.96(4) . ? C38 C43 1.401(5) . ? C38 C39 1.408(5) . ? C39 C40 1.388(6) . ? C39 H39 0.98(4) . ? C40 C41 1.387(6) . ? C40 H40 0.86(4) . ? C41 C42 1.376(5) . ? C41 H41 0.97(4) . ? C42 C43 1.396(5) . ? C42 H42 0.89(4) . ? C44 C45 1.445(5) . ? C44 H44 0.97(4) . ? C45 C46 1.410(5) . ? C45 C50 1.422(5) . ? C46 C47 1.368(5) . ? C46 H46 0.98(4) . ? C47 C48 1.389(5) . ? C47 H47 0.88(4) . ? C48 C49 1.381(5) . ? C48 H48 0.98(4) . ? C49 C50 1.437(5) . ? C49 C52 1.512(5) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? K1 O66 2.725(3) . ? K1 O63 2.730(2) . ? K1 O62 2.751(3) . ? K1 O65 2.759(3) . ? K1 O64 2.781(3) . ? K1 O61 2.793(3) . ? K1 N81 2.846(5) . ? K1 C63 3.257(4) 3_766 ? K1 C64 3.277(4) 3_766 ? K1 C68 3.449(4) . ? K1 C78 3.475(4) . ? K1 C69 3.533(4) . ? O61 C61 1.381(4) . ? O61 C80 1.441(4) . ? O62 C66 1.382(4) . ? O62 C67 1.434(4) . ? O63 C68 1.413(5) . ? O63 C69 1.438(5) . ? O64 C71 1.376(4) . ? O64 C70 1.439(4) . ? O65 C76 1.371(4) . ? O65 C77 1.433(4) . ? O66 C79 1.415(5) . ? O66 C78 1.429(5) . ? C61 C62 1.379(5) . ? C61 C66 1.400(5) . ? C62 C63 1.396(6) . ? C62 H62 0.88(4) . ? C63 C64 1.369(6) . ? C63 K1 3.257(4) 3_766 ? C63 H63 0.94(4) . ? C64 C65 1.396(6) . ? C64 K1 3.277(4) 3_766 ? C64 H64 0.97(4) . ? C65 C66 1.377(5) . ? C65 H65 0.94(4) . ? C67 C68 1.502(6) . ? C67 H67A 0.98(4) . ? C67 H67B 1.07(4) . ? C68 H68A 0.89(3) . ? C68 H68B 0.94(4) . ? C69 C70 1.501(6) . ? C69 H69A 0.98(3) . ? C69 H69B 0.89(4) . ? C70 H70A 0.97(4) . ? C70 H70B 1.06(4) . ? C71 C72 1.387(5) . ? C71 C76 1.408(5) . ? C72 C73 1.387(6) . ? C72 H72 0.92(4) . ? C73 C74 1.380(6) . ? C73 H73 0.88(4) . ? C74 C75 1.393(6) . ? C74 H74 1.01(5) . ? C75 C76 1.383(5) . ? C75 H75 0.93(4) . ? C77 C78 1.485(6) . ? C77 H77A 0.88(4) . ? C77 H77B 0.84(4) . ? C78 H78A 0.93(4) . ? C78 H78B 1.04(4) . ? C79 C80 1.498(6) . ? C79 H79A 1.04(4) . ? C79 H79B 0.94(4) . ? C80 H80A 0.89(4) . ? C80 H80B 1.10(5) . ? N81 C85 1.294(8) . ? N81 C81 1.298(7) . ? C81 C82 1.381(8) . ? C81 H81 0.9500 . ? C82 C83 1.351(9) . ? C82 H82 0.9500 . ? C83 C84 1.363(11) . ? C83 H83 0.9500 . ? C84 C85 1.407(10) . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? N82 C90 1.295(7) . ? N82 C86 1.329(8) . ? C86 C87 1.379(10) . ? C86 H86 0.9500 . ? C87 C88 1.343(10) . ? C87 H87 0.9500 . ? C88 C89 1.303(9) . ? C88 H88 0.9500 . ? C89 C90 1.335(8) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? N92 C99 1.318(12) . ? N92 C98 1.464(11) . ? C96 C98 1.268(10) . ? C96 C97 1.338(9) . ? C96 H96 0.9500 . ? C97 C100 1.261(10) . ? C97 H97 0.9500 . ? C98 H98 0.9500 . ? C99 C100 1.430(13) . ? C99 H99 0.9500 . ? C100 H100 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 O32 Nd1 O1 96.76(7) . . ? O32 Nd1 O31 84.57(8) . . ? O1 Nd1 O31 82.02(8) . . ? O32 Nd1 O2 80.23(8) . . ? O1 Nd1 O2 83.73(8) . . ? O31 Nd1 O2 157.76(8) . . ? O32 Nd1 N1 158.84(8) . . ? O1 Nd1 N1 69.22(8) . . ? O31 Nd1 N1 77.98(8) . . ? O2 Nd1 N1 112.55(9) . . ? O32 Nd1 N32 70.18(8) . . ? O1 Nd1 N32 158.96(8) . . ? O31 Nd1 N32 111.98(8) . . ? O2 Nd1 N32 77.94(8) . . ? N1 Nd1 N32 127.64(8) . . ? O32 Nd1 N2 140.33(8) . . ? O1 Nd1 N2 103.67(8) . . ? O31 Nd1 N2 131.35(8) . . ? O2 Nd1 N2 68.85(9) . . ? N1 Nd1 N2 60.49(8) . . ? N32 Nd1 N2 79.31(8) . . ? O32 Nd1 N31 105.36(8) . . ? O1 Nd1 N31 140.68(8) . . ? O31 Nd1 N31 68.49(8) . . ? O2 Nd1 N31 131.36(8) . . ? N1 Nd1 N31 79.36(8) . . ? N32 Nd1 N31 60.28(8) . . ? N2 Nd1 N31 79.34(8) . . ? C1 O1 Nd1 134.8(2) . . ? C20 O2 Nd1 145.2(2) . . ? C7 N1 C8 119.1(3) . . ? C7 N1 Nd1 127.5(2) . . ? C8 N1 Nd1 112.7(2) . . ? C14 N2 C13 118.3(3) . . ? C14 N2 Nd1 130.2(3) . . ? C13 N2 Nd1 111.4(2) . . ? O1 C1 C2 119.1(3) . . ? O1 C1 C6 123.0(3) . . ? C2 C1 C6 117.8(3) . . ? C3 C2 C1 119.2(3) . . ? C3 C2 C21 122.5(3) . . ? C1 C2 C21 118.3(3) . . ? C2 C3 C4 122.8(4) . . ? C2 C3 H3 117(2) . . ? C4 C3 H3 120(2) . . ? C5 C4 C3 118.7(4) . . ? C5 C4 H4 120(2) . . ? C3 C4 H4 122(2) . . ? C4 C5 C6 121.8(4) . . ? C4 C5 H5 117(2) . . ? C6 C5 H5 121(2) . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C7 117.1(3) . . ? C1 C6 C7 123.1(3) . . ? N1 C7 C6 126.1(3) . . ? N1 C7 H7 118(2) . . ? C6 C7 H7 116(2) . . ? C9 C8 C13 119.5(3) . . ? C9 C8 N1 124.6(3) . . ? C13 C8 N1 115.8(3) . . ? C10 C9 C8 120.1(4) . . ? C10 C9 H9 123(2) . . ? C8 C9 H9 117(2) . . ? C11 C10 C9 120.4(4) . . ? C11 C10 H10 123(3) . . ? C9 C10 H10 117(3) . . ? C10 C11 C12 120.4(4) . . ? C10 C11 H11 120(2) . . ? C12 C11 H11 119(2) . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H12 120(3) . . ? C11 C12 H12 119(3) . . ? C12 C13 C8 119.4(3) . . ? C12 C13 N2 124.0(3) . . ? C8 C13 N2 116.6(3) . . ? N2 C14 C15 127.9(4) . . ? N2 C14 H14 117(2) . . ? C15 C14 H14 115(2) . . ? C16 C15 C20 119.3(4) . . ? C16 C15 C14 117.3(4) . . ? C20 C15 C14 123.3(3) . . ? C17 C16 C15 121.0(4) . . ? C17 C16 H16 124(3) . . ? C15 C16 H16 115(3) . . ? C16 C17 C18 119.5(4) . . ? C16 C17 H17 125(3) . . ? C18 C17 H17 115(3) . . ? C19 C18 C17 122.4(4) . . ? C19 C18 H18 120(2) . . ? C17 C18 H18 118(2) . . ? C18 C19 C20 119.6(4) . . ? C18 C19 C22 122.4(4) . . ? C20 C19 C22 118.0(3) . . ? O2 C20 C15 122.5(3) . . ? O2 C20 C19 119.3(4) . . ? C15 C20 C19 118.1(3) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 O31 Nd1 144.7(2) . . ? C50 O32 Nd1 133.2(2) . . ? C37 N31 C38 117.7(3) . . ? C37 N31 Nd1 130.6(2) . . ? C38 N31 Nd1 111.7(2) . . ? C44 N32 C43 119.0(3) . . ? C44 N32 Nd1 126.9(2) . . ? C43 N32 Nd1 113.6(2) . . ? O31 C31 C36 122.9(3) . . ? O31 C31 C32 119.0(3) . . ? C36 C31 C32 118.1(3) . . ? C33 C32 C31 119.3(4) . . ? C33 C32 C51 123.4(4) . . ? C31 C32 C51 117.3(3) . . ? C32 C33 C34 122.7(4) . . ? C32 C33 H33 118(2) . . ? C34 C33 H33 120(2) . . ? C35 C34 C33 118.8(4) . . ? C35 C34 H34 124(3) . . ? C33 C34 H34 117(3) . . ? C34 C35 C36 121.6(4) . . ? C34 C35 H35 122(3) . . ? C36 C35 H35 116(3) . . ? C35 C36 C31 119.3(3) . . ? C35 C36 C37 117.0(3) . . ? C31 C36 C37 123.4(3) . . ? N31 C37 C36 126.9(3) . . ? N31 C37 H37 119(2) . . ? C36 C37 H37 114(2) . . ? C43 C38 C39 119.2(3) . . ? C43 C38 N31 116.9(3) . . ? C39 C38 N31 123.9(3) . . ? C40 C39 C38 120.2(4) . . ? C40 C39 H39 120(2) . . ? C38 C39 H39 120(2) . . ? C41 C40 C39 119.9(4) . . ? C41 C40 H40 121(3) . . ? C39 C40 H40 118(3) . . ? C42 C41 C40 120.5(4) . . ? C42 C41 H41 119(2) . . ? C40 C41 H41 120(2) . . ? C41 C42 C43 120.7(4) . . ? C41 C42 H42 116(3) . . ? C43 C42 H42 124(3) . . ? C42 C43 C38 119.5(3) . . ? C42 C43 N32 124.6(3) . . ? C38 C43 N32 115.8(3) . . ? N32 C44 C45 126.2(3) . . ? N32 C44 H44 122(2) . . ? C45 C44 H44 112(2) . . ? C46 C45 C50 119.8(3) . . ? C46 C45 C44 116.4(3) . . ? C50 C45 C44 123.7(3) . . ? C47 C46 C45 121.8(3) . . ? C47 C46 H46 117(2) . . ? C45 C46 H46 121(2) . . ? C46 C47 C48 118.7(4) . . ? C46 C47 H47 122(3) . . ? C48 C47 H47 120(3) . . ? C49 C48 C47 122.3(4) . . ? C49 C48 H48 121(2) . . ? C47 C48 H48 116(2) . . ? C48 C49 C50 119.8(3) . . ? C48 C49 C52 122.0(3) . . ? C50 C49 C52 118.1(3) . . ? O32 C50 C45 123.5(3) . . ? O32 C50 C49 119.1(3) . . ? C45 C50 C49 117.4(3) . . ? C32 C51 H51A 109.5 . . ? C32 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C32 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O66 K1 O63 170.72(9) . . ? O66 K1 O62 116.43(8) . . ? O63 K1 O62 61.71(8) . . ? O66 K1 O65 62.69(7) . . ? O63 K1 O65 117.83(8) . . ? O62 K1 O65 172.61(9) . . ? O66 K1 O64 118.27(8) . . ? O63 K1 O64 62.39(7) . . ? O62 K1 O64 124.04(8) . . ? O65 K1 O64 55.72(7) . . ? O66 K1 O61 61.00(8) . . ? O63 K1 O61 117.16(8) . . ? O62 K1 O61 55.63(7) . . ? O65 K1 O61 123.61(7) . . ? O64 K1 O61 173.49(8) . . ? O66 K1 N81 88.90(12) . . ? O63 K1 N81 82.00(12) . . ? O62 K1 N81 88.26(13) . . ? O65 K1 N81 84.40(12) . . ? O64 K1 N81 81.87(13) . . ? O61 K1 N81 91.62(13) . . ? O66 K1 C63 105.19(10) . 3_766 ? O63 K1 C63 83.89(10) . 3_766 ? O62 K1 C63 105.37(10) . 3_766 ? O65 K1 C63 81.69(9) . 3_766 ? O64 K1 C63 70.85(9) . 3_766 ? O61 K1 C63 115.66(10) . 3_766 ? N81 K1 C63 152.67(14) . 3_766 ? O66 K1 C64 81.02(10) . 3_766 ? O63 K1 C64 108.07(10) . 3_766 ? O62 K1 C64 116.71(10) . 3_766 ? O65 K1 C64 70.65(9) . 3_766 ? O64 K1 C64 82.90(9) . 3_766 ? O61 K1 C64 103.11(10) . 3_766 ? N81 K1 C64 155.01(14) . 3_766 ? C63 K1 C64 24.18(10) 3_766 3_766 ? O66 K1 C68 150.28(10) . . ? O63 K1 C68 22.87(9) . . ? O62 K1 C68 43.23(9) . . ? O65 K1 C68 133.96(9) . . ? O64 K1 C68 81.83(9) . . ? O61 K1 C68 96.43(9) . . ? N81 K1 C68 71.60(13) . . ? C63 K1 C68 102.05(11) 3_766 . ? C64 K1 C68 125.41(11) 3_766 . ? O66 K1 C78 22.80(8) . . ? O63 K1 C78 152.62(9) . . ? O62 K1 C78 134.18(9) . . ? O65 K1 C78 42.93(8) . . ? O64 K1 C78 96.90(9) . . ? O61 K1 C78 81.29(9) . . ? N81 K1 C78 77.18(12) . . ? C63 K1 C78 107.12(11) 3_766 . ? C64 K1 C78 85.14(11) 3_766 . ? C68 K1 C78 148.63(11) . . ? O66 K1 C69 153.89(10) . . ? O63 K1 C69 22.15(9) . . ? O62 K1 C69 82.13(9) . . ? O65 K1 C69 96.45(9) . . ? O64 K1 C69 42.32(8) . . ? O61 K1 C69 135.70(9) . . ? N81 K1 C69 72.68(13) . . ? C63 K1 C69 85.62(11) 3_766 . ? C64 K1 C69 107.95(11) 3_766 . ? C68 K1 C69 39.51(10) . . ? C78 K1 C69 131.47(10) . . ? C61 O61 C80 116.7(3) . . ? C61 O61 K1 121.6(2) . . ? C80 O61 K1 116.2(2) . . ? C66 O62 C67 117.2(3) . . ? C66 O62 K1 122.6(2) . . ? C67 O62 K1 116.6(2) . . ? C68 O63 C69 111.8(3) . . ? C68 O63 K1 108.5(2) . . ? C69 O63 K1 112.1(2) . . ? C71 O64 C70 115.7(3) . . ? C71 O64 K1 117.48(19) . . ? C70 O64 K1 114.0(2) . . ? C76 O65 C77 116.6(3) . . ? C76 O65 K1 118.0(2) . . ? C77 O65 K1 113.9(2) . . ? C79 O66 C78 111.3(3) . . ? C79 O66 K1 114.0(2) . . ? C78 O66 K1 109.6(2) . . ? C62 C61 O61 125.0(4) . . ? C62 C61 C66 119.7(4) . . ? O61 C61 C66 115.3(3) . . ? C61 C62 C63 120.1(4) . . ? C61 C62 H62 121(3) . . ? C63 C62 H62 119(3) . . ? C64 C63 C62 119.8(4) . . ? C64 C63 K1 78.7(2) . 3_766 ? C62 C63 K1 92.9(3) . 3_766 ? C64 C63 H63 122(2) . . ? C62 C63 H63 118(2) . . ? K1 C63 H63 99(2) 3_766 . ? C63 C64 C65 120.6(4) . . ? C63 C64 K1 77.1(2) . 3_766 ? C65 C64 K1 94.1(3) . 3_766 ? C63 C64 H64 122(3) . . ? C65 C64 H64 117(3) . . ? K1 C64 H64 104(2) 3_766 . ? C66 C65 C64 119.7(4) . . ? C66 C65 H65 119(2) . . ? C64 C65 H65 122(2) . . ? C65 C66 O62 124.4(3) . . ? C65 C66 C61 120.0(4) . . ? O62 C66 C61 115.6(3) . . ? O62 C67 C68 107.9(3) . . ? O62 C67 H67A 110(2) . . ? C68 C67 H67A 112(2) . . ? O62 C67 H67B 109(2) . . ? C68 C67 H67B 114(2) . . ? H67A C67 H67B 103(3) . . ? O63 C68 C67 109.5(3) . . ? O63 C68 K1 48.67(16) . . ? C67 C68 K1 84.5(2) . . ? O63 C68 H68A 108(2) . . ? C67 C68 H68A 111(2) . . ? K1 C68 H68A 156(2) . . ? O63 C68 H68B 110(2) . . ? C67 C68 H68B 113(2) . . ? K1 C68 H68B 84(2) . . ? H68A C68 H68B 105(3) . . ? O63 C69 C70 109.7(3) . . ? O63 C69 K1 45.71(15) . . ? C70 C69 K1 80.90(19) . . ? O63 C69 H69A 109.0(19) . . ? C70 C69 H69A 110(2) . . ? K1 C69 H69A 154.4(19) . . ? O63 C69 H69B 106(3) . . ? C70 C69 H69B 119(3) . . ? K1 C69 H69B 91(3) . . ? H69A C69 H69B 103(3) . . ? O64 C70 C69 108.4(3) . . ? O64 C70 H70A 109(2) . . ? C69 C70 H70A 115(2) . . ? O64 C70 H70B 107.4(19) . . ? C69 C70 H70B 116.1(19) . . ? H70A C70 H70B 100(3) . . ? O64 C71 C72 124.6(3) . . ? O64 C71 C76 115.3(3) . . ? C72 C71 C76 120.1(4) . . ? C71 C72 C73 119.9(4) . . ? C71 C72 H72 117(2) . . ? C73 C72 H72 123(2) . . ? C74 C73 C72 120.6(4) . . ? C74 C73 H73 122(3) . . ? C72 C73 H73 118(3) . . ? C73 C74 C75 119.7(4) . . ? C73 C74 H74 121(3) . . ? C75 C74 H74 119(3) . . ? C76 C75 C74 120.8(4) . . ? C76 C75 H75 121(3) . . ? C74 C75 H75 118(3) . . ? O65 C76 C75 125.4(3) . . ? O65 C76 C71 115.6(3) . . ? C75 C76 C71 119.0(3) . . ? O65 C77 C78 109.1(3) . . ? O65 C77 H77A 110(3) . . ? C78 C77 H77A 110(3) . . ? O65 C77 H77B 108(3) . . ? C78 C77 H77B 108(3) . . ? H77A C77 H77B 112(4) . . ? O66 C78 C77 109.4(3) . . ? O66 C78 K1 47.62(16) . . ? C77 C78 K1 82.1(2) . . ? O66 C78 H78A 110(2) . . ? C77 C78 H78A 108(2) . . ? K1 C78 H78A 83(2) . . ? O66 C78 H78B 109(2) . . ? C77 C78 H78B 113(2) . . ? K1 C78 H78B 157(2) . . ? H78A C78 H78B 107(3) . . ? O66 C79 C80 109.8(4) . . ? O66 C79 H79A 106(2) . . ? C80 C79 H79A 111(2) . . ? O66 C79 H79B 104(2) . . ? C80 C79 H79B 116(2) . . ? H79A C79 H79B 109(3) . . ? O61 C80 C79 108.8(3) . . ? O61 C80 H80A 110(2) . . ? C79 C80 H80A 110(2) . . ? O61 C80 H80B 111(3) . . ? C79 C80 H80B 113(3) . . ? H80A C80 H80B 104(3) . . ? C85 N81 C81 114.6(6) . . ? C85 N81 K1 115.2(4) . . ? C81 N81 K1 129.6(4) . . ? N81 C81 C82 127.9(6) . . ? N81 C81 H81 116.1 . . ? C82 C81 H81 116.1 . . ? C83 C82 C81 116.4(7) . . ? C83 C82 H82 121.8 . . ? C81 C82 H82 121.8 . . ? C82 C83 C84 118.5(7) . . ? C82 C83 H83 120.8 . . ? C84 C83 H83 120.8 . . ? C83 C84 C85 118.9(8) . . ? C83 C84 H84 120.6 . . ? C85 C84 H84 120.6 . . ? N81 C85 C84 123.7(7) . . ? N81 C85 H85 118.2 . . ? C84 C85 H85 118.2 . . ? C90 N82 C86 114.0(6) . . ? N82 C86 C87 123.1(7) . . ? N82 C86 H86 118.5 . . ? C87 C86 H86 118.5 . . ? C88 C87 C86 118.4(6) . . ? C88 C87 H87 120.8 . . ? C86 C87 H87 120.8 . . ? C89 C88 C87 118.8(7) . . ? C89 C88 H88 120.6 . . ? C87 C88 H88 120.6 . . ? C88 C89 C90 119.6(7) . . ? C88 C89 H89 120.2 . . ? C90 C89 H89 120.2 . . ? N82 C90 C89 126.1(7) . . ? N82 C90 H90 116.9 . . ? C89 C90 H90 116.9 . . ? C99 N92 C98 126.7(10) . . ? C98 C96 C97 112.1(9) . . ? C98 C96 H96 123.9 . . ? C97 C96 H96 123.9 . . ? C100 C97 C96 130.5(11) . . ? C100 C97 H97 114.7 . . ? C96 C97 H97 114.7 . . ? C96 C98 N92 120.2(8) . . ? C96 C98 H98 119.9 . . ? N92 C98 H98 119.9 . . ? N92 C99 C100 107.8(12) . . ? N92 C99 H99 126.1 . . ? C100 C99 H99 126.1 . . ? C97 C100 C99 121.5(11) . . ? C97 C100 H100 119.3 . . ? C99 C100 H100 119.3 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.139 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.096 # Attachment '- 2.cif' data_vg47-2_hklf5 _database_code_depnum_ccdc_archive 'CCDC 877720' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108.10 H150.89 K N4 Nd O12' _chemical_formula_weight 1881.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.1709(13) _cell_length_b 17.5403(13) _cell_length_c 19.5362(15) _cell_angle_alpha 90.671(6) _cell_angle_beta 113.704(7) _cell_angle_gamma 96.867(6) _cell_volume 5026.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3209 _cell_measurement_theta_min 3.3687 _cell_measurement_theta_max 28.9683 _exptl_crystal_description 'long plate' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5203 _exptl_crystal_size_mid 0.1550 _exptl_crystal_size_min 0.0354 _cell_oxdiff_twin_number 2 loop_ _cell_oxdiff_twin_id _cell_oxdiff_twin_matrix_11 _cell_oxdiff_twin_matrix_12 _cell_oxdiff_twin_matrix_13 _cell_oxdiff_twin_matrix_21 _cell_oxdiff_twin_matrix_22 _cell_oxdiff_twin_matrix_23 _cell_oxdiff_twin_matrix_31 _cell_oxdiff_twin_matrix_32 _cell_oxdiff_twin_matrix_33 1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 -0.9998 -0.0001 0.0002 0.6068 0.0242 0.9752 0.6067 1.0246 -0.0253 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 1 1 0.0192 -0.0041 0.9980 0.9996 0.0023 0.0488 -0.0324 0 -1 -1 0.0162 0.0041 -0.9980 -0.9996 -0.0023 -0.0488 0.0324 1 0 0 0.2153 0.9954 0.0007 0.0014 -0.0000 0.0395 0.0275 -1 0 0 0.2203 -0.9954 -0.0007 -0.0014 0.0000 -0.0395 -0.0275 0 1 -1 0.0825 -0.0000 0.9963 -0.9964 0.0537 -0.0067 -0.0089 0 -1 1 0.0725 0.0000 -0.9963 0.9964 -0.0537 0.0067 0.0089 0 0 -1 0.0569 0.0020 -0.0009 -0.9980 0.0257 -0.0277 0.0117 0 0 1 0.0494 -0.0020 0.0009 0.9980 -0.0257 0.0277 -0.0117 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2005 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7391 _exptl_absorpt_correction_T_max 0.9787 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28488 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2504 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 26.37 _reflns_number_total 28488 _reflns_number_gt 14757 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; loop_ _diffrn_oxdiff_twin_id _diffrn_oxdiff_twin_ratio _diffrn_oxdiff_twin_reflns_isolated _diffrn_oxdiff_twin_reflns_overlapped 1 0.5476 12456 30968 2 0.4524 12505 30968 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -49.00 43.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - 17.1550 -37.0000 120.0000 92 #__ type_ start__ end____ width___ exp.time_ 2 omega -23.00 60.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - 17.1550 -101.0000 80.0000 83 #__ type_ start__ end____ width___ exp.time_ 3 omega -9.00 90.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - 17.1550 37.0000 -60.0000 99 #__ type_ start__ end____ width___ exp.time_ 4 omega -25.00 23.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - -18.8738 -99.0000 -60.0000 48 #__ type_ start__ end____ width___ exp.time_ 5 omega -92.00 -2.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - -18.8738 -19.0000 30.0000 90 ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution ; SUPERFLIP Palatinus, L. & Chapuis, G. (2007). SUPERFLIP - a computer program for the solution of crystal structures by charge flipping in arbitrary dimensions, J. Appl. Cryst. 40, 786-790. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0505P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28488 _refine_ls_number_parameters 1172 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1413 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 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 Nd1 Nd 0.56478(2) 0.79495(2) 0.20665(2) 0.01817(10) Uani 1 1 d . . . O1 O 0.4971(3) 0.7600(2) 0.2908(2) 0.0214(11) Uani 1 1 d . . . O2 O 0.4293(3) 0.7272(3) 0.1191(3) 0.0237(12) Uani 1 1 d . . . N1 N 0.5264(3) 0.9162(3) 0.2633(3) 0.0216(14) Uani 1 1 d . . . N2 N 0.4622(3) 0.8878(3) 0.1175(3) 0.0209(12) Uani 1 1 d . . . C1 C 0.5132(4) 0.7847(4) 0.3575(4) 0.0199(17) Uani 1 1 d . . . C2 C 0.5077(4) 0.7315(4) 0.4128(4) 0.0207(17) Uani 1 1 d . . . C3 C 0.5367(4) 0.7609(4) 0.4841(4) 0.0275(18) Uani 1 1 d . . . H3 H 0.5372 0.7251 0.5203 0.033 Uiso 1 1 calc R . . C4 C 0.5665(4) 0.8385(4) 0.5110(4) 0.0273(19) Uani 1 1 d . . . C5 C 0.5618(4) 0.8879(4) 0.4565(4) 0.0289(19) Uani 1 1 d . . . H5 H 0.5769 0.9415 0.4701 0.035 Uiso 1 1 calc R . . C6 C 0.5358(4) 0.8631(4) 0.3812(4) 0.0245(18) Uani 1 1 d . . . C7 C 0.5304(4) 0.9226(4) 0.3303(4) 0.0249(18) Uani 1 1 d . . . H7 H 0.5297 0.9729 0.3483 0.030 Uiso 1 1 calc R . . C8 C 0.5215(4) 0.9804(4) 0.2209(4) 0.0237(17) Uani 1 1 d . . . C9 C 0.5485(4) 1.0570(4) 0.2508(4) 0.0312(19) Uani 1 1 d . . . H9 H 0.5669 1.0687 0.3028 0.037 Uiso 1 1 calc R . . C10 C 0.5481(4) 1.1154(4) 0.2034(5) 0.041(2) Uani 1 1 d . . . H10 H 0.5668 1.1672 0.2236 0.049 Uiso 1 1 calc R . . C11 C 0.5213(5) 1.0997(4) 0.1279(5) 0.041(2) Uani 1 1 d . . . H11 H 0.5231 1.1400 0.0963 0.049 Uiso 1 1 calc R . . C12 C 0.4919(4) 1.0251(4) 0.0990(4) 0.0288(18) Uani 1 1 d . . . H12 H 0.4723 1.0144 0.0466 0.035 Uiso 1 1 calc R . . C13 C 0.4899(4) 0.9655(4) 0.1429(4) 0.0207(17) Uani 1 1 d . . . C14 C 0.3939(4) 0.8726(4) 0.0545(4) 0.0237(18) Uani 1 1 d . . . H14 H 0.3715 0.9162 0.0283 0.028 Uiso 1 1 calc R . . C15 C 0.3464(4) 0.8000(4) 0.0178(4) 0.0209(16) Uani 1 1 d . . . C16 C 0.2807(4) 0.7998(4) -0.0542(4) 0.0254(17) Uani 1 1 d . . . H16 H 0.2715 0.8478 -0.0761 0.030 Uiso 1 1 calc R . . C17 C 0.2277(4) 0.7348(4) -0.0962(4) 0.0273(18) Uani 1 1 d . . . C18 C 0.2418(4) 0.6658(4) -0.0595(4) 0.0224(16) Uani 1 1 d . . . H18 H 0.2059 0.6195 -0.0863 0.027 Uiso 1 1 calc R . . C19 C 0.3052(4) 0.6612(4) 0.0138(4) 0.0175(16) Uani 1 1 d . . . C20 C 0.3638(4) 0.7285(4) 0.0549(4) 0.0222(17) Uani 1 1 d . . . C21 C 0.4682(4) 0.6475(4) 0.3895(4) 0.0246(18) Uani 1 1 d . . . C22 C 0.5260(4) 0.6063(4) 0.3585(4) 0.034(2) Uani 1 1 d . . . H22A H 0.4972 0.5531 0.3415 0.051 Uiso 1 1 calc R . . H22B H 0.5872 0.6061 0.3980 0.051 Uiso 1 1 calc R . . H22C H 0.5306 0.6333 0.3163 0.051 Uiso 1 1 calc R . . C23 C 0.3719(4) 0.6407(4) 0.3298(4) 0.037(2) Uani 1 1 d . . . H23A H 0.3333 0.6639 0.3498 0.055 Uiso 1 1 calc R . . H23B H 0.3480 0.5863 0.3149 0.055 Uiso 1 1 calc R . . H23C H 0.3721 0.6676 0.2862 0.055 Uiso 1 1 calc R . . C24 C 0.4666(5) 0.6021(4) 0.4558(4) 0.042(2) Uani 1 1 d . . . H24A H 0.4330 0.6272 0.4796 0.063 Uiso 1 1 calc R . . H24B H 0.5292 0.6007 0.4924 0.063 Uiso 1 1 calc R . . H24C H 0.4366 0.5495 0.4378 0.063 Uiso 1 1 calc R . . C25 C 0.6046(5) 0.8629(5) 0.5934(4) 0.041(2) Uani 1 1 d . . . C26 C 0.6272(6) 0.9499(5) 0.6090(5) 0.069(3) Uani 1 1 d . . . H26A H 0.6717 0.9696 0.5889 0.104 Uiso 1 1 calc R . . H26B H 0.6529 0.9624 0.6632 0.104 Uiso 1 1 calc R . . H26C H 0.5715 0.9737 0.5849 0.104 Uiso 1 1 calc R . . C27 C 0.6928(5) 0.8298(5) 0.6332(4) 0.065(3) Uani 1 1 d . . . H27A H 0.6795 0.7741 0.6347 0.098 Uiso 1 1 calc R . . H27B H 0.7240 0.8533 0.6844 0.098 Uiso 1 1 calc R . . H27C H 0.7321 0.8407 0.6062 0.098 Uiso 1 1 calc R . . C28 C 0.5385(6) 0.8356(5) 0.6281(4) 0.075(3) Uani 1 1 d . . . H28A H 0.4828 0.8595 0.6047 0.112 Uiso 1 1 calc R . . H28B H 0.5667 0.8501 0.6820 0.112 Uiso 1 1 calc R . . H28C H 0.5233 0.7795 0.6202 0.112 Uiso 1 1 calc R . . C29 C 0.1622(5) 0.7394(4) -0.1773(4) 0.039(2) Uani 1 1 d . . . C30 C 0.1014(5) 0.8012(5) -0.1835(5) 0.066(3) Uani 1 1 d . . . H30A H 0.0589 0.8029 -0.2359 0.099 Uiso 1 1 calc R . . H30B H 0.1391 0.8514 -0.1658 0.099 Uiso 1 1 calc R . . H30C H 0.0669 0.7892 -0.1527 0.099 Uiso 1 1 calc R . . C31 C 0.2192(5) 0.7598(4) -0.2236(4) 0.052(2) Uani 1 1 d . . . H31A H 0.2584 0.7201 -0.2195 0.079 Uiso 1 1 calc R . . H31B H 0.2569 0.8097 -0.2044 0.079 Uiso 1 1 calc R . . H31C H 0.1782 0.7625 -0.2763 0.079 Uiso 1 1 calc R . . C32 C 0.1019(4) 0.6642(4) -0.2108(4) 0.041(2) Uani 1 1 d . . . H32A H 0.0619 0.6519 -0.1847 0.062 Uiso 1 1 calc R . . H32B H 0.1399 0.6232 -0.2053 0.062 Uiso 1 1 calc R . . H32C H 0.0648 0.6688 -0.2640 0.062 Uiso 1 1 calc R . . C33 C 0.3139(4) 0.5834(4) 0.0479(4) 0.0248(17) Uani 1 1 d . . . C34 C 0.4038(4) 0.5590(4) 0.0540(4) 0.039(2) Uani 1 1 d . . . H34A H 0.4135 0.5114 0.0802 0.058 Uiso 1 1 calc R . . H34B H 0.4539 0.5996 0.0821 0.058 Uiso 1 1 calc R . . H34C H 0.4018 0.5503 0.0037 0.058 Uiso 1 1 calc R . . C35 C 0.2390(4) 0.5205(4) 0.0023(4) 0.036(2) Uani 1 1 d . . . H35A H 0.2381 0.5145 -0.0479 0.055 Uiso 1 1 calc R . . H35B H 0.1802 0.5340 -0.0017 0.055 Uiso 1 1 calc R . . H35C H 0.2498 0.4720 0.0268 0.055 Uiso 1 1 calc R . . C36 C 0.3119(5) 0.5886(4) 0.1254(4) 0.042(2) Uani 1 1 d . . . H36A H 0.2543 0.6050 0.1210 0.064 Uiso 1 1 calc R . . H36B H 0.3628 0.6261 0.1584 0.064 Uiso 1 1 calc R . . H36C H 0.3175 0.5381 0.1464 0.064 Uiso 1 1 calc R . . O41 O 0.6561(3) 0.6969(2) 0.2553(2) 0.0196(11) Uani 1 1 d . . . O42 O 0.6099(3) 0.7903(2) 0.1074(2) 0.0208(12) Uani 1 1 d . . . N41 N 0.7035(3) 0.8372(3) 0.3370(3) 0.0186(13) Uani 1 1 d . . . N42 N 0.6924(3) 0.9128(3) 0.2177(3) 0.0197(14) Uani 1 1 d . . . C41 C 0.7002(4) 0.6674(4) 0.3184(4) 0.0190(16) Uani 1 1 d . . . C42 C 0.7218(4) 0.5900(4) 0.3215(4) 0.0217(17) Uani 1 1 d . . . C43 C 0.7612(4) 0.5614(4) 0.3904(4) 0.0241(18) Uani 1 1 d . . . H43 H 0.7725 0.5094 0.3916 0.029 Uiso 1 1 calc R . . C44 C 0.7864(4) 0.6023(4) 0.4595(4) 0.0214(17) Uani 1 1 d . . . C45 C 0.7738(4) 0.6788(4) 0.4562(4) 0.0229(17) Uani 1 1 d . . . H45 H 0.7933 0.7098 0.5015 0.027 Uiso 1 1 calc R . . C46 C 0.7325(4) 0.7123(4) 0.3868(4) 0.0174(16) Uani 1 1 d . . . C47 C 0.7373(4) 0.7947(4) 0.3921(4) 0.0194(17) Uani 1 1 d . . . H47 H 0.7681 0.8200 0.4407 0.023 Uiso 1 1 calc R . . C48 C 0.7293(4) 0.9171(4) 0.3499(4) 0.0189(16) Uani 1 1 d . . . C49 C 0.7523(4) 0.9600(4) 0.4177(4) 0.0235(17) Uani 1 1 d . . . H49 H 0.7516 0.9341 0.4599 0.028 Uiso 1 1 calc R . . C50 C 0.7759(4) 1.0386(4) 0.4245(4) 0.0299(19) Uani 1 1 d . . . H50 H 0.7916 1.0666 0.4709 0.036 Uiso 1 1 calc R . . C51 C 0.7765(4) 1.0760(4) 0.3631(4) 0.0312(19) Uani 1 1 d . . . H51 H 0.7945 1.1301 0.3681 0.037 Uiso 1 1 calc R . . C52 C 0.7521(4) 1.0374(4) 0.2955(4) 0.0233(17) Uani 1 1 d . . . H52 H 0.7518 1.0649 0.2538 0.028 Uiso 1 1 calc R . . C53 C 0.7272(4) 0.9571(4) 0.2870(4) 0.0190(16) Uani 1 1 d . . . C54 C 0.7221(4) 0.9356(4) 0.1679(4) 0.0245(19) Uani 1 1 d . . . H54 H 0.7639 0.9817 0.1813 0.029 Uiso 1 1 calc R . . C55 C 0.6997(4) 0.9000(4) 0.0950(4) 0.0192(14) Uani 1 1 d . . . C56 C 0.7440(4) 0.9396(4) 0.0525(4) 0.0243(15) Uani 1 1 d . . . H56 H 0.7780 0.9890 0.0708 0.029 Uiso 1 1 calc R . . C57 C 0.7383(4) 0.9083(4) -0.0131(4) 0.0265(18) Uani 1 1 d . . . C58 C 0.6879(4) 0.8351(4) -0.0375(4) 0.0257(17) Uani 1 1 d . . . H58 H 0.6843 0.8128 -0.0834 0.031 Uiso 1 1 calc R . . C59 C 0.6433(4) 0.7927(4) -0.0005(3) 0.0182(16) Uani 1 1 d . . . C60 C 0.6484(4) 0.8268(4) 0.0686(4) 0.0186(17) Uani 1 1 d . . . C61 C 0.7012(4) 0.5424(4) 0.2496(4) 0.0248(17) Uani 1 1 d . . . C62 C 0.7521(5) 0.5837(4) 0.2068(4) 0.038(2) Uani 1 1 d . . . H62A H 0.7345 0.6354 0.1970 0.057 Uiso 1 1 calc R . . H62B H 0.7365 0.5545 0.1592 0.057 Uiso 1 1 calc R . . H62C H 0.8179 0.5877 0.2368 0.057 Uiso 1 1 calc R . . C63 C 0.5993(4) 0.5291(4) 0.2011(4) 0.038(2) Uani 1 1 d . . . H63A H 0.5676 0.5011 0.2286 0.058 Uiso 1 1 calc R . . H63B H 0.5878 0.4989 0.1549 0.058 Uiso 1 1 calc R . . H63C H 0.5769 0.5788 0.1887 0.058 Uiso 1 1 calc R . . C64 C 0.7328(5) 0.4631(4) 0.2645(4) 0.041(2) Uani 1 1 d . . . H64A H 0.7984 0.4693 0.2957 0.062 Uiso 1 1 calc R . . H64B H 0.7202 0.4354 0.2168 0.062 Uiso 1 1 calc R . . H64C H 0.7000 0.4339 0.2905 0.062 Uiso 1 1 calc R . . C65 C 0.8231(5) 0.5616(4) 0.5324(4) 0.0330(18) Uani 1 1 d . . . C66 C 0.9055(5) 0.5235(5) 0.5384(4) 0.059(3) Uani 1 1 d . . . H66A H 0.9254 0.4945 0.5835 0.088 Uiso 1 1 calc R . . H66B H 0.9552 0.5631 0.5414 0.088 Uiso 1 1 calc R . . H66C H 0.8889 0.4884 0.4942 0.088 Uiso 1 1 calc R . . C67 C 0.7495(5) 0.5004(5) 0.5331(4) 0.069(3) Uani 1 1 d . . . H67A H 0.7322 0.4629 0.4905 0.104 Uiso 1 1 calc R . . H67B H 0.6962 0.5243 0.5293 0.104 Uiso 1 1 calc R . . H67C H 0.7723 0.4744 0.5799 0.104 Uiso 1 1 calc R . . C68 C 0.8539(6) 0.6188(5) 0.6005(4) 0.062(3) Uani 1 1 d . . . H68A H 0.8012 0.6410 0.6007 0.094 Uiso 1 1 calc R . . H68B H 0.8991 0.6599 0.5979 0.094 Uiso 1 1 calc R . . H68C H 0.8812 0.5921 0.6464 0.094 Uiso 1 1 calc R . . C69 C 0.7875(4) 0.9477(4) -0.0593(4) 0.0327(19) Uani 1 1 d . . . C70 C 0.8304(5) 1.0306(4) -0.0282(4) 0.051(2) Uani 1 1 d . . . H70A H 0.8585 1.0545 -0.0602 0.077 Uiso 1 1 calc R . . H70B H 0.8770 1.0300 0.0228 0.077 Uiso 1 1 calc R . . H70C H 0.7831 1.0603 -0.0275 0.077 Uiso 1 1 calc R . . C71 C 0.8641(5) 0.9018(4) -0.0552(4) 0.052(2) Uani 1 1 d . . . H71A H 0.8383 0.8487 -0.0747 0.079 Uiso 1 1 calc R . . H71B H 0.9079 0.9022 -0.0029 0.079 Uiso 1 1 calc R . . H71C H 0.8952 0.9253 -0.0853 0.079 Uiso 1 1 calc R . . C72 C 0.7203(5) 0.9504(5) -0.1405(4) 0.053(2) Uani 1 1 d . . . H72A H 0.7527 0.9737 -0.1697 0.080 Uiso 1 1 calc R . . H72B H 0.6728 0.9812 -0.1425 0.080 Uiso 1 1 calc R . . H72C H 0.6924 0.8980 -0.1616 0.080 Uiso 1 1 calc R . . C73 C 0.5931(4) 0.7118(4) -0.0299(4) 0.0273(19) Uani 1 1 d . . . C74 C 0.5990(5) 0.6856(4) -0.1033(4) 0.049(2) Uani 1 1 d . . . H74A H 0.6629 0.6842 -0.0943 0.073 Uiso 1 1 calc R . . H74B H 0.5731 0.7218 -0.1415 0.073 Uiso 1 1 calc R . . H74C H 0.5646 0.6341 -0.1206 0.073 Uiso 1 1 calc R . . C75 C 0.4918(4) 0.7082(4) -0.0465(4) 0.035(2) Uani 1 1 d . . . H75A H 0.4614 0.6555 -0.0636 0.052 Uiso 1 1 calc R . . H75B H 0.4641 0.7431 -0.0857 0.052 Uiso 1 1 calc R . . H75C H 0.4850 0.7238 -0.0009 0.052 Uiso 1 1 calc R . . C76 C 0.6342(4) 0.6550(4) 0.0273(4) 0.037(2) Uani 1 1 d . . . H76A H 0.6974 0.6532 0.0342 0.055 Uiso 1 1 calc R . . H76B H 0.5989 0.6039 0.0098 0.055 Uiso 1 1 calc R . . H76C H 0.6330 0.6711 0.0751 0.055 Uiso 1 1 calc R . . K1 K 0.90837(9) 0.23491(9) 0.72550(8) 0.0321(4) Uani 1 1 d . . . O81 O 0.8630(3) 0.2112(3) 0.8480(3) 0.0303(13) Uani 1 1 d . . . O82 O 1.0352(3) 0.2331(3) 0.8708(2) 0.0321(13) Uani 1 1 d . . . O83 O 1.0856(3) 0.2477(3) 0.7501(3) 0.0284(10) Uani 1 1 d . . . O84 O 0.9572(3) 0.2448(3) 0.6044(3) 0.0325(13) Uani 1 1 d . . . O85 O 0.7891(3) 0.2055(3) 0.5785(3) 0.0348(13) Uani 1 1 d . . . O86 O 0.7321(3) 0.1932(3) 0.6994(3) 0.0316(13) Uani 1 1 d . . . C81 C 0.9214(5) 0.2551(4) 0.9118(4) 0.0294(18) Uani 1 1 d . . . C82 C 0.8958(5) 0.2886(5) 0.9629(5) 0.049(2) Uani 1 1 d . . . H82 H 0.8336 0.2805 0.9556 0.059 Uiso 1 1 calc R . . C83 C 0.9570(5) 0.3327(5) 1.0233(5) 0.064(3) Uani 1 1 d . . . H83 H 0.9372 0.3548 1.0577 0.076 Uiso 1 1 calc R . . C84 C 1.0478(5) 0.3460(5) 1.0356(4) 0.058(3) Uani 1 1 d . . . H84 H 1.0905 0.3778 1.0776 0.070 Uiso 1 1 calc R . . C85 C 1.0753(5) 0.3120(5) 0.9854(4) 0.046(2) Uani 1 1 d . . . H85 H 1.1377 0.3201 0.9933 0.056 Uiso 1 1 calc R . . C86 C 1.0141(5) 0.2674(4) 0.9250(4) 0.030(2) Uani 1 1 d . . . C87 C 1.1290(4) 0.2488(4) 0.8812(4) 0.034(2) Uani 1 1 d . . . H87A H 1.1686 0.2279 0.9282 0.041 Uiso 1 1 calc R . . H87B H 1.1477 0.3050 0.8846 0.041 Uiso 1 1 calc R . . C88 C 1.1385(4) 0.2121(4) 0.8163(4) 0.036(2) Uani 1 1 d . . . H88A H 1.2034 0.2188 0.8240 0.043 Uiso 1 1 calc R . . H88B H 1.1166 0.1563 0.8112 0.043 Uiso 1 1 calc R . . C89 C 1.1043(4) 0.2244(4) 0.6877(4) 0.0288(19) Uani 1 1 d . . . H89A H 1.0866 0.1681 0.6762 0.035 Uiso 1 1 calc R . . H89B H 1.1702 0.2365 0.6999 0.035 Uiso 1 1 calc R . . C90 C 1.0521(4) 0.2654(4) 0.6228(4) 0.0330(19) Uani 1 1 d . . . H90A H 1.0691 0.3216 0.6346 0.040 Uiso 1 1 calc R . . H90B H 1.0660 0.2516 0.5796 0.040 Uiso 1 1 calc R . . C91 C 0.8959(5) 0.2664(4) 0.5386(4) 0.0324(19) Uani 1 1 d . . . C92 C 0.9190(6) 0.3072(4) 0.4879(4) 0.041(2) Uani 1 1 d . . . H92 H 0.9813 0.3234 0.4984 0.049 Uiso 1 1 calc R . . C93 C 0.8521(6) 0.3248(5) 0.4220(5) 0.054(2) Uani 1 1 d . . . H93 H 0.8684 0.3515 0.3862 0.065 Uiso 1 1 calc R . . C94 C 0.7623(6) 0.3040(5) 0.4078(5) 0.052(2) Uani 1 1 d . . . H94 H 0.7167 0.3179 0.3628 0.063 Uiso 1 1 calc R . . C95 C 0.7368(6) 0.2628(4) 0.4582(5) 0.046(2) Uani 1 1 d . . . H95 H 0.6744 0.2471 0.4475 0.056 Uiso 1 1 calc R . . C96 C 0.8041(5) 0.2455(4) 0.5236(4) 0.0314(19) Uani 1 1 d . . . C97 C 0.6968(4) 0.1868(4) 0.5682(4) 0.042(2) Uani 1 1 d . . . H97A H 0.6622 0.1546 0.5210 0.050 Uiso 1 1 calc R . . H97B H 0.6685 0.2345 0.5648 0.050 Uiso 1 1 calc R . . C98 C 0.6935(4) 0.1437(4) 0.6338(4) 0.038(2) Uani 1 1 d . . . H98A H 0.6295 0.1240 0.6239 0.045 Uiso 1 1 calc R . . H98B H 0.7277 0.0992 0.6405 0.045 Uiso 1 1 calc R . . C99 C 0.7189(4) 0.1570(4) 0.7595(4) 0.037(2) Uani 1 1 d . . . H99A H 0.7416 0.1064 0.7653 0.045 Uiso 1 1 calc R . . H99B H 0.6530 0.1482 0.7485 0.045 Uiso 1 1 calc R . . C100 C 0.7685(4) 0.2063(4) 0.8296(4) 0.034(2) Uani 1 1 d . . . H10A H 0.7495 0.2582 0.8227 0.041 Uiso 1 1 calc R . . H10B H 0.7544 0.1839 0.8706 0.041 Uiso 1 1 calc R . . O101 O 0.9102(4) 0.3867(3) 0.7399(4) 0.072(2) Uani 1 1 d . . . C101 C 0.8680(6) 0.4222(6) 0.7780(6) 0.086(4) Uani 1 1 d . . . H10C H 0.8338 0.3836 0.7968 0.104 Uiso 1 1 calc R . . H10D H 0.8254 0.4556 0.7451 0.104 Uiso 1 1 calc R . . C102 C 0.9443(8) 0.4689(6) 0.8414(6) 0.098(4) Uani 1 1 d . . . H10E H 0.9358 0.5239 0.8403 0.118 Uiso 1 1 calc R . . H10F H 0.9488 0.4501 0.8902 0.118 Uiso 1 1 calc R . . C103 C 1.0250(7) 0.4576(7) 0.8285(7) 0.108(5) Uani 1 1 d . . . H10G H 1.0672 0.5063 0.8390 0.129 Uiso 1 1 calc R . . H10H H 1.0577 0.4181 0.8604 0.129 Uiso 1 1 calc R . . C104 C 0.9896(7) 0.4329(7) 0.7520(7) 0.104(4) Uani 1 1 d . . . H10I H 0.9780 0.4772 0.7201 0.125 Uiso 1 1 calc R . . H10J H 1.0323 0.4037 0.7412 0.125 Uiso 1 1 calc R . . O102 O 0.9106(4) 0.0820(3) 0.7315(3) 0.0529(17) Uani 1 1 d . . . C105 C 0.9246(5) 0.0334(5) 0.6796(5) 0.051(2) Uani 1 1 d . . . H10K H 0.9461 0.0645 0.6465 0.061 Uiso 1 1 calc R . . H10L H 0.8673 0.0002 0.6482 0.061 Uiso 1 1 calc R . . C106 C 0.9941(7) -0.0136(6) 0.7246(5) 0.091(4) Uani 1 1 d . . . H10M H 1.0542 0.0064 0.7252 0.109 Uiso 1 1 calc R . . H10N H 0.9775 -0.0677 0.7038 0.109 Uiso 1 1 calc R . . C107 C 0.9968(6) -0.0084(6) 0.8024(5) 0.074(3) Uani 1 1 d . . . H10O H 0.9823 -0.0599 0.8182 0.088 Uiso 1 1 calc R . . H10P H 1.0574 0.0156 0.8390 0.088 Uiso 1 1 calc R . . C108 C 0.9273(6) 0.0397(5) 0.7955(5) 0.060(3) Uani 1 1 d . . . H10Q H 0.8706 0.0073 0.7908 0.072 Uiso 1 1 calc R . . H10R H 0.9481 0.0753 0.8407 0.072 Uiso 1 1 calc R . . C111 C 0.5265(9) 0.3809(8) 0.3311(9) 0.157(7) Uani 0.849(10) 1 d PD . . H11A H 0.5290 0.3762 0.2819 0.235 Uiso 0.849(10) 1 calc PR . . H11B H 0.5633 0.3448 0.3640 0.235 Uiso 0.849(10) 1 calc PR . . H11C H 0.5506 0.4335 0.3531 0.235 Uiso 0.849(10) 1 calc PR . . C112 C 0.4285(10) 0.3625(11) 0.3221(10) 0.198(10) Uani 0.849(10) 1 d PD . . H11D H 0.4098 0.3061 0.3131 0.237 Uiso 0.849(10) 1 calc PR . . H11E H 0.4241 0.3787 0.3691 0.237 Uiso 0.849(10) 1 calc PR . . C113 C 0.3662(9) 0.4012(8) 0.2597(8) 0.135(7) Uani 0.849(10) 1 d PD . . H11F H 0.3705 0.3850 0.2127 0.162 Uiso 0.849(10) 1 calc PR . . H11G H 0.3849 0.4575 0.2687 0.162 Uiso 0.849(10) 1 calc PR . . C114 C 0.2681(9) 0.3827(8) 0.2509(9) 0.136(7) Uani 0.849(10) 1 d PD . . H11H H 0.2305 0.4209 0.2210 0.163 Uiso 0.849(10) 1 calc PR . . H11I H 0.2647 0.3821 0.3004 0.163 Uiso 0.849(10) 1 calc PR . . C115 C 0.2360(9) 0.3021(8) 0.2096(7) 0.141(7) Uani 0.849(10) 1 d PD . . H11J H 0.2268 0.3043 0.1565 0.170 Uiso 0.849(10) 1 calc PR . . H11K H 0.2801 0.2660 0.2341 0.170 Uiso 0.849(10) 1 calc PR . . C116 C 0.1471(9) 0.2793(10) 0.2166(8) 0.236(13) Uani 0.849(10) 1 d PD . . H11L H 0.1581 0.2509 0.2617 0.353 Uiso 0.849(10) 1 calc PR . . H11M H 0.1052 0.2466 0.1724 0.353 Uiso 0.849(10) 1 calc PR . . H11N H 0.1203 0.3256 0.2203 0.353 Uiso 0.849(10) 1 calc PR . . C121 C 0.0295(5) 0.1584(5) 0.4286(5) 0.059(3) Uani 1 1 d . . . H12A H 0.0803 0.1440 0.4184 0.088 Uiso 1 1 calc R . . H12B H 0.0421 0.2130 0.4458 0.088 Uiso 1 1 calc R . . H12C H -0.0267 0.1496 0.3828 0.088 Uiso 1 1 calc R . . C122 C 0.0182(5) 0.1104(5) 0.4884(4) 0.048(2) Uani 1 1 d . . . H12D H -0.0350 0.1238 0.4967 0.058 Uiso 1 1 calc R . . H12E H 0.0728 0.1235 0.5358 0.058 Uiso 1 1 calc R . . C123 C 0.0047(5) 0.0243(4) 0.4697(4) 0.041(2) Uani 1 1 d . . . H12F H -0.0507 0.0111 0.4229 0.049 Uiso 1 1 calc R . . H12G H 0.0572 0.0112 0.4603 0.049 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 Nd1 0.0195(2) 0.0183(3) 0.0218(3) 0.00428(15) 0.0124(2) 0.00677(18) O1 0.026(2) 0.024(3) 0.021(3) 0.007(2) 0.015(2) 0.009(2) O2 0.020(3) 0.026(3) 0.023(3) 0.003(3) 0.006(2) 0.004(2) N1 0.020(3) 0.024(4) 0.022(4) -0.003(3) 0.009(3) 0.007(3) N2 0.021(3) 0.025(4) 0.019(4) 0.006(3) 0.010(3) 0.005(3) C1 0.014(3) 0.025(5) 0.023(4) -0.006(4) 0.010(3) 0.002(3) C2 0.011(3) 0.026(4) 0.026(5) -0.004(4) 0.008(3) 0.002(3) C3 0.022(4) 0.038(5) 0.024(5) 0.010(4) 0.011(4) 0.003(4) C4 0.021(4) 0.034(5) 0.027(5) -0.010(4) 0.012(4) -0.003(4) C5 0.029(4) 0.027(5) 0.042(5) 0.003(4) 0.026(4) 0.006(3) C6 0.017(4) 0.038(5) 0.023(5) 0.000(4) 0.012(3) 0.006(3) C7 0.025(4) 0.019(4) 0.031(5) -0.006(4) 0.011(4) 0.006(3) C8 0.014(4) 0.025(5) 0.034(5) 0.006(4) 0.011(4) 0.007(3) C9 0.022(4) 0.027(5) 0.043(5) 0.004(4) 0.010(4) 0.007(4) C10 0.029(4) 0.019(5) 0.067(7) -0.002(5) 0.010(5) 0.001(4) C11 0.038(5) 0.029(5) 0.052(6) 0.020(5) 0.014(4) 0.005(4) C12 0.032(4) 0.018(5) 0.031(5) 0.006(4) 0.007(4) 0.000(3) C13 0.013(3) 0.016(4) 0.032(5) 0.007(4) 0.007(3) 0.004(3) C14 0.028(4) 0.026(5) 0.028(5) 0.011(4) 0.019(4) 0.014(4) C15 0.018(4) 0.021(4) 0.028(5) 0.005(4) 0.013(4) 0.006(3) C16 0.018(4) 0.029(5) 0.028(5) 0.010(4) 0.006(4) 0.009(3) C17 0.022(4) 0.041(5) 0.020(4) 0.001(4) 0.008(3) 0.010(4) C18 0.022(4) 0.020(4) 0.026(5) 0.006(4) 0.011(4) 0.002(3) C19 0.018(4) 0.022(4) 0.018(4) 0.003(3) 0.012(3) 0.007(3) C20 0.016(4) 0.028(5) 0.022(5) -0.005(4) 0.007(3) 0.003(3) C21 0.020(4) 0.031(5) 0.028(4) 0.003(4) 0.016(3) 0.001(3) C22 0.029(4) 0.028(5) 0.050(5) 0.012(4) 0.021(4) 0.005(3) C23 0.024(4) 0.044(5) 0.048(6) -0.003(5) 0.021(4) -0.002(4) C24 0.047(5) 0.040(5) 0.042(5) 0.004(4) 0.024(4) -0.002(4) C25 0.044(5) 0.046(6) 0.026(5) -0.001(4) 0.009(4) 0.004(4) C26 0.085(7) 0.065(7) 0.052(7) -0.014(6) 0.025(6) 0.003(6) C27 0.060(6) 0.082(7) 0.036(6) -0.005(5) 0.002(5) 0.006(5) C28 0.093(7) 0.091(8) 0.046(6) -0.032(6) 0.049(6) -0.034(6) C29 0.043(5) 0.033(5) 0.034(5) 0.005(4) 0.008(4) 0.018(4) C30 0.065(6) 0.062(7) 0.051(6) 0.000(5) -0.006(5) 0.037(5) C31 0.072(6) 0.054(6) 0.028(5) 0.009(5) 0.021(5) -0.002(5) C32 0.030(4) 0.061(6) 0.022(5) 0.012(4) -0.004(4) 0.013(4) C33 0.025(4) 0.021(4) 0.025(5) 0.001(4) 0.007(3) 0.003(3) C34 0.035(4) 0.024(5) 0.044(5) 0.000(4) 0.003(4) -0.002(4) C35 0.044(5) 0.033(5) 0.036(5) 0.009(4) 0.020(4) 0.005(4) C36 0.062(5) 0.035(5) 0.031(5) 0.012(4) 0.021(4) -0.003(4) O41 0.025(2) 0.020(3) 0.016(3) 0.008(2) 0.008(2) 0.011(2) O42 0.028(3) 0.014(3) 0.026(3) 0.006(2) 0.017(2) 0.001(2) N41 0.018(3) 0.028(4) 0.017(3) 0.002(3) 0.013(3) 0.003(3) N42 0.014(3) 0.016(3) 0.035(4) 0.005(3) 0.017(3) 0.000(3) C41 0.010(3) 0.027(5) 0.026(5) 0.008(4) 0.013(3) 0.003(3) C42 0.023(4) 0.019(4) 0.028(5) 0.008(4) 0.014(4) 0.009(3) C43 0.024(4) 0.025(4) 0.028(5) 0.013(4) 0.013(4) 0.009(3) C44 0.019(4) 0.019(4) 0.032(5) 0.005(4) 0.017(4) 0.000(3) C45 0.019(4) 0.029(5) 0.017(4) 0.006(4) 0.005(3) 0.000(3) C46 0.009(3) 0.026(5) 0.016(4) 0.002(4) 0.004(3) 0.000(3) C47 0.016(4) 0.033(5) 0.010(4) -0.003(4) 0.007(3) 0.000(3) C48 0.015(3) 0.016(4) 0.027(5) 0.005(4) 0.008(3) 0.007(3) C49 0.016(4) 0.032(5) 0.022(4) 0.003(4) 0.006(3) 0.008(3) C50 0.028(4) 0.023(5) 0.040(5) -0.012(4) 0.017(4) -0.001(4) C51 0.029(4) 0.012(4) 0.050(6) 0.000(4) 0.014(4) 0.002(3) C52 0.024(4) 0.020(4) 0.025(5) 0.004(4) 0.008(4) 0.002(3) C53 0.011(3) 0.016(4) 0.029(5) 0.006(4) 0.005(3) 0.005(3) C54 0.016(4) 0.022(5) 0.038(5) 0.007(4) 0.012(4) 0.004(3) C55 0.016(4) 0.021(5) 0.022(5) 0.004(3) 0.008(4) 0.005(3) C56 0.016(4) 0.018(5) 0.039(5) 0.015(3) 0.011(4) 0.000(3) C57 0.020(4) 0.043(5) 0.017(4) 0.017(4) 0.005(3) 0.015(4) C58 0.025(4) 0.039(5) 0.017(4) 0.002(4) 0.009(3) 0.015(4) C59 0.013(3) 0.027(4) 0.013(4) 0.006(3) 0.003(3) 0.003(3) C60 0.020(4) 0.018(5) 0.021(5) 0.011(4) 0.007(4) 0.015(3) C61 0.034(4) 0.013(4) 0.025(5) 0.005(4) 0.008(4) 0.011(3) C62 0.054(5) 0.038(5) 0.034(5) 0.001(4) 0.026(4) 0.015(4) C63 0.042(5) 0.027(5) 0.039(5) -0.006(4) 0.008(4) 0.005(4) C64 0.065(5) 0.030(5) 0.032(5) -0.001(4) 0.021(4) 0.014(4) C65 0.038(4) 0.035(5) 0.023(5) 0.017(4) 0.008(4) 0.006(4) C66 0.065(6) 0.069(7) 0.044(6) 0.035(5) 0.017(5) 0.033(5) C67 0.068(6) 0.084(8) 0.044(6) 0.040(6) 0.017(5) -0.013(5) C68 0.098(7) 0.058(6) 0.024(5) 0.029(5) 0.012(5) 0.028(5) C69 0.026(4) 0.047(5) 0.035(5) 0.025(4) 0.020(4) 0.010(4) C70 0.062(5) 0.048(6) 0.062(7) 0.014(4) 0.047(5) -0.003(5) C71 0.047(5) 0.065(6) 0.071(7) 0.029(5) 0.047(5) 0.017(5) C72 0.047(5) 0.080(7) 0.045(6) 0.032(5) 0.029(5) 0.013(5) C73 0.033(4) 0.040(5) 0.015(4) 0.012(4) 0.014(4) 0.015(4) C74 0.056(5) 0.055(6) 0.044(6) -0.011(5) 0.034(5) -0.005(4) C75 0.028(4) 0.032(5) 0.043(5) 0.001(4) 0.015(4) 0.001(4) C76 0.042(5) 0.036(5) 0.027(5) 0.001(4) 0.008(4) 0.006(4) K1 0.0219(8) 0.0465(11) 0.0314(10) 0.0087(9) 0.0136(8) 0.0066(8) O81 0.015(2) 0.044(3) 0.043(3) 0.008(3) 0.022(2) 0.009(2) O82 0.020(2) 0.051(3) 0.031(3) 0.005(3) 0.016(2) 0.009(2) O83 0.027(3) 0.039(4) 0.022(3) 0.012(2) 0.010(3) 0.015(2) O84 0.027(3) 0.050(4) 0.028(3) 0.016(3) 0.017(3) 0.010(3) O85 0.018(3) 0.050(4) 0.033(3) 0.005(3) 0.005(2) 0.008(2) O86 0.026(3) 0.038(3) 0.034(3) 0.002(3) 0.015(3) 0.005(2) C81 0.030(4) 0.040(5) 0.023(5) 0.004(4) 0.014(4) 0.013(4) C82 0.030(5) 0.078(7) 0.045(6) 0.003(5) 0.016(4) 0.021(5) C83 0.048(6) 0.107(8) 0.041(6) -0.015(6) 0.021(5) 0.022(6) C84 0.038(5) 0.098(8) 0.029(5) -0.014(5) 0.005(4) 0.010(5) C85 0.029(5) 0.078(7) 0.036(6) 0.000(5) 0.015(4) 0.015(5) C86 0.030(5) 0.035(5) 0.026(5) 0.011(4) 0.008(4) 0.016(4) C87 0.016(4) 0.051(6) 0.037(5) 0.017(4) 0.013(4) 0.006(4) C88 0.023(4) 0.044(5) 0.051(6) 0.017(5) 0.023(4) 0.014(4) C89 0.021(4) 0.044(5) 0.028(5) 0.012(4) 0.015(4) 0.009(4) C90 0.041(5) 0.029(5) 0.037(5) 0.006(4) 0.025(4) 0.003(4) C91 0.043(5) 0.029(5) 0.030(5) -0.001(4) 0.018(4) 0.012(4) C92 0.061(6) 0.038(5) 0.029(5) 0.017(4) 0.020(5) 0.013(4) C93 0.085(7) 0.040(6) 0.047(7) 0.019(5) 0.033(6) 0.022(5) C94 0.083(7) 0.038(6) 0.029(6) 0.022(5) 0.008(5) 0.035(5) C95 0.060(6) 0.032(5) 0.040(6) 0.004(5) 0.009(5) 0.022(5) C96 0.052(5) 0.021(5) 0.026(5) 0.006(4) 0.017(4) 0.018(4) C97 0.030(4) 0.059(6) 0.037(5) 0.001(5) 0.011(4) 0.020(4) C98 0.015(4) 0.039(5) 0.054(6) -0.012(5) 0.012(4) -0.002(4) C99 0.024(4) 0.042(6) 0.054(6) 0.012(5) 0.024(4) 0.002(4) C100 0.029(4) 0.046(5) 0.043(5) 0.013(5) 0.029(4) 0.009(4) O101 0.054(4) 0.055(4) 0.112(6) -0.024(4) 0.043(4) -0.002(3) C101 0.041(6) 0.088(9) 0.135(11) -0.012(8) 0.041(7) 0.008(6) C102 0.136(11) 0.076(9) 0.091(10) -0.027(7) 0.057(9) 0.006(8) C103 0.053(7) 0.133(12) 0.092(10) 0.059(9) -0.008(7) -0.026(7) C104 0.056(8) 0.136(12) 0.119(12) 0.025(10) 0.032(8) 0.024(8) O102 0.073(4) 0.046(4) 0.065(5) 0.021(4) 0.048(4) 0.029(3) C105 0.044(5) 0.063(7) 0.049(6) -0.001(5) 0.021(5) 0.015(5) C106 0.116(9) 0.112(10) 0.055(7) 0.000(7) 0.032(7) 0.063(8) C107 0.083(7) 0.093(8) 0.057(7) 0.023(6) 0.031(6) 0.047(6) C108 0.094(7) 0.047(6) 0.067(7) 0.029(6) 0.053(6) 0.035(5) C111 0.150(15) 0.111(14) 0.21(2) 0.047(13) 0.074(14) 0.012(12) C112 0.158(18) 0.25(2) 0.20(2) 0.110(19) 0.088(17) 0.010(17) C113 0.141(15) 0.164(17) 0.115(15) 0.022(13) 0.051(12) 0.077(14) C114 0.165(16) 0.092(13) 0.160(18) 0.003(12) 0.083(14) -0.006(12) C115 0.185(17) 0.189(19) 0.087(13) 0.095(13) 0.070(12) 0.100(15) C116 0.139(14) 0.53(4) 0.122(15) 0.18(2) 0.094(13) 0.18(2) C121 0.062(6) 0.054(6) 0.064(7) 0.003(5) 0.034(5) -0.004(5) C122 0.041(5) 0.058(6) 0.045(6) -0.004(5) 0.019(4) 0.001(4) C123 0.031(4) 0.049(6) 0.044(6) -0.005(4) 0.015(4) 0.008(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 Nd1 O42 2.334(4) . ? Nd1 O2 2.336(4) . ? Nd1 O41 2.358(4) . ? Nd1 O1 2.363(4) . ? Nd1 N2 2.613(5) . ? Nd1 N1 2.635(5) . ? Nd1 N41 2.652(5) . ? Nd1 N42 2.682(5) . ? O1 C1 1.281(7) . ? O2 C20 1.278(7) . ? N1 C7 1.287(8) . ? N1 C8 1.398(8) . ? N2 C14 1.279(7) . ? N2 C13 1.401(8) . ? C1 C6 1.403(8) . ? C1 C2 1.459(9) . ? C2 C3 1.350(8) . ? C2 C21 1.522(8) . ? C3 C4 1.409(9) . ? C4 C5 1.363(9) . ? C4 C25 1.509(9) . ? C5 C6 1.405(9) . ? C6 C7 1.435(9) . ? C8 C9 1.404(9) . ? C8 C13 1.408(9) . ? C9 C10 1.387(9) . ? C10 C11 1.373(10) . ? C11 C12 1.371(9) . ? C12 C13 1.367(8) . ? C14 C15 1.423(8) . ? C15 C16 1.380(8) . ? C15 C20 1.456(9) . ? C16 C17 1.374(8) . ? C17 C18 1.409(9) . ? C17 C29 1.521(9) . ? C18 C19 1.396(8) . ? C19 C20 1.426(8) . ? C19 C33 1.523(9) . ? C21 C23 1.514(8) . ? C21 C24 1.536(8) . ? C21 C22 1.539(8) . ? C25 C27 1.514(9) . ? C25 C28 1.517(9) . ? C25 C26 1.524(10) . ? C29 C32 1.509(9) . ? C29 C30 1.523(9) . ? C29 C31 1.547(9) . ? C33 C35 1.506(8) . ? C33 C34 1.523(8) . ? C33 C36 1.528(8) . ? O41 C41 1.300(7) . ? O42 C60 1.292(7) . ? N41 C47 1.287(8) . ? N41 C48 1.403(7) . ? N42 C54 1.293(7) . ? N42 C53 1.419(8) . ? C41 C46 1.412(9) . ? C41 C42 1.439(8) . ? C42 C43 1.368(9) . ? C42 C61 1.520(8) . ? C43 C44 1.404(8) . ? C44 C45 1.379(9) . ? C44 C65 1.529(9) . ? C45 C46 1.419(9) . ? C46 C47 1.438(9) . ? C48 C49 1.403(8) . ? C48 C53 1.413(8) . ? C49 C50 1.376(8) . ? C50 C51 1.377(9) . ? C51 C52 1.362(8) . ? C52 C53 1.406(8) . ? C54 C55 1.436(9) . ? C55 C60 1.410(9) . ? C55 C56 1.435(7) . ? C56 C57 1.352(9) . ? C57 C58 1.402(8) . ? C57 C69 1.545(8) . ? C58 C59 1.378(8) . ? C59 C60 1.437(8) . ? C59 C73 1.528(9) . ? C61 C63 1.521(8) . ? C61 C62 1.525(8) . ? C61 C64 1.528(8) . ? C65 C67 1.508(9) . ? C65 C66 1.525(9) . ? C65 C68 1.529(9) . ? C69 C72 1.527(9) . ? C69 C71 1.533(8) . ? C69 C70 1.537(10) . ? C73 C76 1.506(9) . ? C73 C75 1.530(8) . ? C73 C74 1.543(8) . ? K1 O101 2.670(6) . ? K1 O83 2.690(4) . ? K1 O102 2.690(6) . ? K1 O86 2.691(4) . ? K1 O85 2.740(5) . ? K1 O82 2.757(5) . ? K1 O84 2.780(4) . ? K1 O81 2.793(4) . ? K1 C98 3.383(6) . ? K1 C88 3.497(6) . ? K1 C99 3.515(6) . ? K1 C104 3.517(13) . ? O81 C81 1.376(7) . ? O81 C100 1.414(7) . ? O82 C86 1.387(8) . ? O82 C87 1.438(6) . ? O83 C88 1.434(7) . ? O83 C89 1.435(7) . ? O84 C91 1.361(8) . ? O84 C90 1.428(7) . ? O85 C96 1.374(8) . ? O85 C97 1.420(7) . ? O86 C98 1.410(7) . ? O86 C99 1.420(7) . ? C81 C82 1.374(9) . ? C81 C86 1.404(9) . ? C82 C83 1.351(10) . ? C83 C84 1.378(9) . ? C84 C85 1.386(9) . ? C85 C86 1.356(9) . ? C87 C88 1.485(8) . ? C89 C90 1.464(8) . ? C91 C92 1.371(9) . ? C91 C96 1.393(9) . ? C92 C93 1.377(10) . ? C93 C94 1.365(10) . ? C94 C95 1.391(10) . ? C95 C96 1.372(9) . ? C97 C98 1.512(9) . ? C99 C100 1.480(9) . ? O101 C104 1.366(10) . ? O101 C101 1.379(9) . ? C101 C102 1.494(12) . ? C102 C103 1.460(12) . ? C103 C104 1.411(13) . ? O102 C108 1.408(9) . ? O102 C105 1.421(8) . ? C105 C106 1.469(10) . ? C106 C107 1.504(10) . ? C107 C108 1.449(10) . ? C111 C112 1.516(9) . ? C112 C113 1.469(9) . ? C113 C114 1.518(8) . ? C114 C115 1.543(9) . ? C115 C116 1.505(9) . ? C121 C122 1.504(9) . ? C122 C123 1.519(9) . ? C123 C123 1.513(13) 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 O42 Nd1 O2 83.02(14) . . ? O42 Nd1 O41 86.13(14) . . ? O2 Nd1 O41 102.86(15) . . ? O42 Nd1 O1 161.86(14) . . ? O2 Nd1 O1 82.67(14) . . ? O41 Nd1 O1 86.24(13) . . ? O42 Nd1 N2 79.31(15) . . ? O2 Nd1 N2 68.85(18) . . ? O41 Nd1 N2 163.94(15) . . ? O1 Nd1 N2 105.67(13) . . ? O42 Nd1 N1 127.25(16) . . ? O2 Nd1 N1 108.84(14) . . ? O41 Nd1 N1 135.67(16) . . ? O1 Nd1 N1 68.38(16) . . ? N2 Nd1 N1 60.11(18) . . ? O42 Nd1 N41 112.63(14) . . ? O2 Nd1 N41 159.54(15) . . ? O41 Nd1 N41 66.77(15) . . ? O1 Nd1 N41 79.16(14) . . ? N2 Nd1 N41 125.32(19) . . ? N1 Nd1 N41 72.94(16) . . ? O42 Nd1 N42 67.93(14) . . ? O2 Nd1 N42 140.90(17) . . ? O41 Nd1 N42 100.74(14) . . ? O1 Nd1 N42 129.78(16) . . ? N2 Nd1 N42 80.12(16) . . ? N1 Nd1 N42 72.83(15) . . ? N41 Nd1 N42 59.55(17) . . ? C1 O1 Nd1 133.1(4) . . ? C20 O2 Nd1 144.9(4) . . ? C7 N1 C8 120.9(6) . . ? C7 N1 Nd1 124.1(5) . . ? C8 N1 Nd1 113.5(4) . . ? C14 N2 C13 116.9(6) . . ? C14 N2 Nd1 129.6(5) . . ? C13 N2 Nd1 113.4(4) . . ? O1 C1 C6 122.6(7) . . ? O1 C1 C2 120.9(6) . . ? C6 C1 C2 116.5(6) . . ? C3 C2 C1 117.0(6) . . ? C3 C2 C21 122.5(6) . . ? C1 C2 C21 120.5(6) . . ? C2 C3 C4 127.5(7) . . ? C5 C4 C3 113.9(7) . . ? C5 C4 C25 123.9(7) . . ? C3 C4 C25 122.1(7) . . ? C4 C5 C6 123.1(7) . . ? C1 C6 C5 121.3(7) . . ? C1 C6 C7 122.5(6) . . ? C5 C6 C7 116.1(7) . . ? N1 C7 C6 128.1(6) . . ? N1 C8 C9 124.8(7) . . ? N1 C8 C13 116.3(6) . . ? C9 C8 C13 118.9(7) . . ? C10 C9 C8 119.3(7) . . ? C11 C10 C9 121.2(7) . . ? C12 C11 C10 119.0(7) . . ? C13 C12 C11 122.2(7) . . ? C12 C13 N2 125.3(6) . . ? C12 C13 C8 119.3(6) . . ? N2 C13 C8 115.4(6) . . ? N2 C14 C15 129.5(7) . . ? C16 C15 C14 117.4(7) . . ? C16 C15 C20 120.6(6) . . ? C14 C15 C20 122.0(6) . . ? C17 C16 C15 124.5(7) . . ? C16 C17 C18 115.1(6) . . ? C16 C17 C29 120.7(7) . . ? C18 C17 C29 124.2(6) . . ? C19 C18 C17 124.1(6) . . ? C18 C19 C20 119.9(6) . . ? C18 C19 C33 119.5(6) . . ? C20 C19 C33 120.5(6) . . ? O2 C20 C19 123.3(7) . . ? O2 C20 C15 121.1(6) . . ? C19 C20 C15 115.6(6) . . ? C23 C21 C2 110.6(6) . . ? C23 C21 C24 108.4(5) . . ? C2 C21 C24 112.1(5) . . ? C23 C21 C22 108.5(5) . . ? C2 C21 C22 111.5(5) . . ? C24 C21 C22 105.6(5) . . ? C4 C25 C27 109.0(6) . . ? C4 C25 C28 111.8(6) . . ? C27 C25 C28 109.2(7) . . ? C4 C25 C26 112.9(7) . . ? C27 C25 C26 106.7(7) . . ? C28 C25 C26 107.0(6) . . ? C32 C29 C17 112.5(6) . . ? C32 C29 C30 108.3(6) . . ? C17 C29 C30 110.5(6) . . ? C32 C29 C31 107.9(6) . . ? C17 C29 C31 108.1(6) . . ? C30 C29 C31 109.6(7) . . ? C35 C33 C19 113.9(6) . . ? C35 C33 C34 107.5(5) . . ? C19 C33 C34 108.1(5) . . ? C35 C33 C36 106.5(5) . . ? C19 C33 C36 110.6(5) . . ? C34 C33 C36 110.0(6) . . ? C41 O41 Nd1 140.8(4) . . ? C60 O42 Nd1 147.6(4) . . ? C47 N41 C48 118.1(6) . . ? C47 N41 Nd1 126.9(4) . . ? C48 N41 Nd1 113.8(4) . . ? C54 N42 C53 117.5(5) . . ? C54 N42 Nd1 128.8(5) . . ? C53 N42 Nd1 113.6(4) . . ? O41 C41 C46 120.6(6) . . ? O41 C41 C42 122.0(6) . . ? C46 C41 C42 117.3(6) . . ? C43 C42 C41 118.1(6) . . ? C43 C42 C61 121.8(6) . . ? C41 C42 C61 120.1(6) . . ? C42 C43 C44 125.5(7) . . ? C45 C44 C43 115.9(7) . . ? C45 C44 C65 123.9(7) . . ? C43 C44 C65 120.2(6) . . ? C44 C45 C46 121.6(7) . . ? C41 C46 C45 120.8(6) . . ? C41 C46 C47 123.8(6) . . ? C45 C46 C47 114.9(6) . . ? N41 C47 C46 125.9(6) . . ? C49 C48 N41 126.1(6) . . ? C49 C48 C53 118.2(6) . . ? N41 C48 C53 115.6(6) . . ? C50 C49 C48 121.7(7) . . ? C49 C50 C51 119.0(7) . . ? C52 C51 C50 121.6(7) . . ? C51 C52 C53 120.3(7) . . ? C52 C53 C48 119.1(6) . . ? C52 C53 N42 124.6(6) . . ? C48 C53 N42 116.2(6) . . ? N42 C54 C55 128.2(6) . . ? C60 C55 C56 120.1(7) . . ? C60 C55 C54 124.4(5) . . ? C56 C55 C54 114.9(7) . . ? C57 C56 C55 121.5(7) . . ? C56 C57 C58 117.2(6) . . ? C56 C57 C69 123.2(7) . . ? C58 C57 C69 119.6(6) . . ? C59 C58 C57 125.4(6) . . ? C58 C59 C60 117.2(6) . . ? C58 C59 C73 121.7(6) . . ? C60 C59 C73 121.0(6) . . ? O42 C60 C55 120.3(6) . . ? O42 C60 C59 121.1(6) . . ? C55 C60 C59 118.6(6) . . ? C42 C61 C63 111.0(5) . . ? C42 C61 C62 109.2(5) . . ? C63 C61 C62 110.2(6) . . ? C42 C61 C64 112.4(6) . . ? C63 C61 C64 107.0(6) . . ? C62 C61 C64 106.9(5) . . ? C67 C65 C66 108.8(6) . . ? C67 C65 C68 110.2(6) . . ? C66 C65 C68 107.4(6) . . ? C67 C65 C44 109.0(6) . . ? C66 C65 C44 110.5(6) . . ? C68 C65 C44 110.9(6) . . ? C72 C69 C71 110.3(6) . . ? C72 C69 C70 108.1(6) . . ? C71 C69 C70 108.1(5) . . ? C72 C69 C57 110.2(5) . . ? C71 C69 C57 108.3(5) . . ? C70 C69 C57 111.8(6) . . ? C76 C73 C59 109.8(6) . . ? C76 C73 C75 109.2(6) . . ? C59 C73 C75 110.8(5) . . ? C76 C73 C74 107.7(6) . . ? C59 C73 C74 112.4(6) . . ? C75 C73 C74 106.8(6) . . ? O101 K1 O83 93.52(17) . . ? O101 K1 O102 171.90(19) . . ? O83 K1 O102 87.27(15) . . ? O101 K1 O86 97.32(16) . . ? O83 K1 O86 169.15(15) . . ? O102 K1 O86 81.94(15) . . ? O101 K1 O85 100.10(18) . . ? O83 K1 O85 114.90(14) . . ? O102 K1 O85 86.84(17) . . ? O86 K1 O85 63.58(14) . . ? O101 K1 O82 91.80(17) . . ? O83 K1 O82 61.69(13) . . ? O102 K1 O82 81.47(17) . . ? O86 K1 O82 117.32(14) . . ? O85 K1 O82 167.91(15) . . ? O101 K1 O84 93.26(17) . . ? O83 K1 O84 60.67(14) . . ? O102 K1 O84 94.15(15) . . ? O86 K1 O84 118.85(15) . . ? O85 K1 O84 55.27(13) . . ? O82 K1 O84 122.33(13) . . ? O101 K1 O81 91.81(17) . . ? O83 K1 O81 117.82(14) . . ? O102 K1 O81 80.72(15) . . ? O86 K1 O81 61.57(14) . . ? O85 K1 O81 124.87(14) . . ? O82 K1 O81 56.24(12) . . ? O84 K1 O81 174.79(15) . . ? O101 K1 C98 111.29(18) . . ? O83 K1 C98 148.90(17) . . ? O102 K1 C98 70.84(18) . . ? O86 K1 C98 23.50(13) . . ? O85 K1 C98 44.38(16) . . ? O82 K1 C98 132.39(17) . . ? O84 K1 C98 98.17(16) . . ? O81 K1 C98 81.08(16) . . ? O101 K1 C88 103.23(18) . . ? O83 K1 C88 22.28(13) . . ? O102 K1 C88 74.81(17) . . ? O86 K1 C88 150.91(16) . . ? O85 K1 C88 130.81(15) . . ? O82 K1 C88 42.56(14) . . ? O84 K1 C88 80.58(15) . . ? O81 K1 C88 97.09(15) . . ? C98 K1 C88 145.46(18) . . ? O101 K1 C99 103.81(18) . . ? O83 K1 C99 152.54(16) . . ? O102 K1 C99 72.66(16) . . ? O86 K1 C99 21.67(15) . . ? O85 K1 C99 83.20(16) . . ? O82 K1 C99 96.15(15) . . ? O84 K1 C99 137.44(16) . . ? O81 K1 C99 41.80(15) . . ? C98 K1 C99 39.33(17) . . ? C88 K1 C99 130.57(18) . . ? O101 K1 C104 20.14(18) . . ? O83 K1 C104 73.41(19) . . ? O102 K1 C104 159.4(2) . . ? O86 K1 C104 117.4(2) . . ? O85 K1 C104 107.5(2) . . ? O82 K1 C104 83.1(2) . . ? O84 K1 C104 82.7(2) . . ? O81 K1 C104 101.8(2) . . ? C98 K1 C104 129.7(2) . . ? C88 K1 C104 84.6(2) . . ? C99 K1 C104 122.7(2) . . ? C81 O81 C100 117.6(5) . . ? C81 O81 K1 113.4(3) . . ? C100 O81 K1 113.6(4) . . ? C86 O82 C87 115.5(5) . . ? C86 O82 K1 115.3(4) . . ? C87 O82 K1 115.5(4) . . ? C88 O83 C89 111.1(5) . . ? C88 O83 K1 112.4(3) . . ? C89 O83 K1 115.6(4) . . ? C91 O84 C90 118.7(5) . . ? C91 O84 K1 118.2(4) . . ? C90 O84 K1 115.6(4) . . ? C96 O85 C97 116.4(6) . . ? C96 O85 K1 120.1(4) . . ? C97 O85 K1 113.8(4) . . ? C98 O86 C99 110.5(5) . . ? C98 O86 K1 107.0(3) . . ? C99 O86 K1 113.9(4) . . ? C82 C81 O81 125.2(6) . . ? C82 C81 C86 117.5(7) . . ? O81 C81 C86 117.3(6) . . ? C83 C82 C81 121.6(7) . . ? C82 C83 C84 120.9(7) . . ? C83 C84 C85 118.4(7) . . ? C86 C85 C84 120.7(7) . . ? C85 C86 O82 124.5(6) . . ? C85 C86 C81 120.8(7) . . ? O82 C86 C81 114.7(6) . . ? O82 C87 C88 108.5(5) . . ? O83 C88 C87 108.4(5) . . ? O83 C88 K1 45.3(2) . . ? C87 C88 K1 82.6(3) . . ? O83 C89 C90 108.7(5) . . ? O84 C90 C89 109.0(5) . . ? O84 C91 C92 124.4(7) . . ? O84 C91 C96 116.4(7) . . ? C92 C91 C96 119.2(8) . . ? C91 C92 C93 120.1(8) . . ? C94 C93 C92 120.2(8) . . ? C93 C94 C95 121.0(8) . . ? C96 C95 C94 118.3(8) . . ? C95 C96 O85 124.7(7) . . ? C95 C96 C91 121.2(7) . . ? O85 C96 C91 114.1(7) . . ? O85 C97 C98 109.0(6) . . ? O86 C98 C97 109.7(6) . . ? O86 C98 K1 49.5(3) . . ? C97 C98 K1 84.0(4) . . ? O86 C99 C100 109.6(6) . . ? O86 C99 K1 44.4(3) . . ? C100 C99 K1 81.2(4) . . ? O81 C100 C99 108.5(5) . . ? C104 O101 C101 107.2(8) . . ? C104 O101 K1 117.6(6) . . ? C101 O101 K1 124.9(6) . . ? O101 C101 C102 104.6(7) . . ? C103 C102 C101 103.8(8) . . ? C104 C103 C102 103.8(9) . . ? O101 C104 C103 104.2(9) . . ? O101 C104 K1 42.3(5) . . ? C103 C104 K1 110.7(8) . . ? C108 O102 C105 105.3(6) . . ? C108 O102 K1 126.3(5) . . ? C105 O102 K1 125.6(5) . . ? O102 C105 C106 106.1(7) . . ? C105 C106 C107 106.1(7) . . ? C108 C107 C106 103.4(7) . . ? O102 C108 C107 108.8(7) . . ? C113 C112 C111 111.9(10) . . ? C112 C113 C114 111.8(11) . . ? C113 C114 C115 104.3(10) . . ? C116 C115 C114 102.3(10) . . ? C121 C122 C123 113.8(6) . . ? C123 C123 C122 114.1(8) 2_556 . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.407 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.123 # Attachment '- 3.cif' data_cc180 _database_code_depnum_ccdc_archive 'CCDC 877721' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C177.50 H141.50 K9 N23.50 Nd3 O12' _chemical_formula_weight 3580.26 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' Nd Nd -0.1943 3.0179 '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 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.6191(5) _cell_length_b 27.7932(8) _cell_length_c 19.0450(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.395(3) _cell_angle_gamma 90.00 _cell_volume 8198.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20802 _cell_measurement_theta_min 3.3043 _cell_measurement_theta_max 32.5042 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3636 _exptl_absorpt_coefficient_mu 1.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7280 _exptl_absorpt_correction_T_max 0.8206 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83596 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.1004 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 28.28 _reflns_number_total 40613 _reflns_number_gt 31026 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -25.00 74.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 0.0000 -120.0000 99 #__ type_ start__ end____ width___ exp.time_ 2 omega -104.00 -58.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 179.0000 -120.0000 46 #__ type_ start__ end____ width___ exp.time_ 3 omega -76.00 3.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 -77.0000 -120.0000 79 #__ type_ start__ end____ width___ exp.time_ 4 omega 65.00 101.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 179.0000 -30.0000 36 #__ type_ start__ end____ width___ exp.time_ 5 omega 57.00 94.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 179.0000 150.0000 37 #__ type_ start__ end____ width___ exp.time_ 6 omega -47.00 26.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 -37.0000 -120.0000 73 #__ type_ start__ end____ width___ exp.time_ 7 omega -52.00 40.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -27.2801 37.0000 -180.0000 92 #__ type_ start__ end____ width___ exp.time_ 8 omega -75.00 -48.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -27.2801 110.0000 -49.0000 27 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+10.1541P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.463(8) _refine_ls_number_reflns 40613 _refine_ls_number_parameters 2014 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 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 Nd1 Nd 0.05101(2) 0.45416(4) 0.103011(17) 0.02514(8) Uani 1 1 d . . . Nd2 Nd 0.43840(2) 0.49921(4) 0.400839(18) 0.02545(8) Uani 1 1 d . . . Nd3 Nd 0.76815(2) 0.46121(4) 0.735058(17) 0.02460(8) Uani 1 1 d . . . K1 K 0.28420(11) 0.43848(7) 0.22873(8) 0.0358(4) Uani 1 1 d . . . K2 K 0.11440(11) 0.50543(7) 0.33031(9) 0.0397(4) Uani 1 1 d . . . K3 K 0.43789(11) 0.55807(7) 0.22892(8) 0.0395(4) Uani 1 1 d . . . K4 K 0.54374(10) 0.45205(8) 0.59079(7) 0.0374(4) Uani 1 1 d . . . K5 K 0.69474(11) 0.54603(7) 0.51203(9) 0.0380(4) Uani 1 1 d . . . K6 K 0.78148(14) 0.33563(7) 0.57191(9) 0.0475(5) Uani 1 1 d . . . K7 K 0.88882(13) 0.50518(7) 0.93225(10) 0.0511(5) Uani 1 1 d . . . K8 K 0.93599(11) 0.36605(6) 0.90426(8) 0.0333(4) Uani 1 1 d . . . K9 K 1.05019(18) 0.52693(10) 0.72138(19) 0.0772(13) Uani 0.800(6) 1 d P . 1 K9B K 0.9879(7) 0.5456(3) 0.7862(5) 0.053(4) Uani 0.200(6) 1 d P . 2 O1 O 0.0471(3) 0.51023(17) 0.0085(2) 0.0357(12) Uani 1 1 d . . . O2 O 0.1126(3) 0.43652(17) 0.2294(2) 0.0309(11) Uani 1 1 d . . . N1 N -0.0052(4) 0.5365(2) 0.1449(3) 0.0294(13) Uani 1 1 d . . . N2 N -0.0626(4) 0.4486(2) 0.1785(3) 0.0285(12) Uani 1 1 d . . . C1 C 0.0715(5) 0.5552(2) 0.0094(3) 0.0281(15) Uani 1 1 d . . . C2 C 0.1250(6) 0.5707(3) -0.0401(4) 0.045(2) Uani 1 1 d . . . H2 H 0.1447 0.5483 -0.0705 0.053 Uiso 1 1 calc R . . C3 C 0.1491(7) 0.6183(3) -0.0448(5) 0.057(3) Uani 1 1 d . . . H3 H 0.1863 0.6272 -0.0770 0.069 Uiso 1 1 calc R . . C4 C 0.1181(6) 0.6531(3) -0.0015(4) 0.050(2) Uani 1 1 d . . . H4 H 0.1323 0.6854 -0.0053 0.060 Uiso 1 1 calc R . . C5 C 0.0654(5) 0.6379(3) 0.0474(4) 0.0378(18) Uani 1 1 d . . . H5 H 0.0432 0.6608 0.0756 0.045 Uiso 1 1 calc R . . C6 C 0.0441(5) 0.5895(2) 0.0565(3) 0.0262(15) Uani 1 1 d . . . C7 C -0.0014(5) 0.5780(3) 0.1154(4) 0.0319(16) Uani 1 1 d . . . H7 H -0.0309 0.6031 0.1341 0.038 Uiso 1 1 calc R . . C8 C -0.0408(4) 0.5316(2) 0.2103(3) 0.0249(14) Uani 1 1 d . . . C9 C -0.0407(5) 0.5690(3) 0.2579(4) 0.0361(17) Uani 1 1 d . . . H9 H -0.0222 0.5994 0.2459 0.043 Uiso 1 1 calc R . . C10 C -0.0684(5) 0.5616(3) 0.3246(4) 0.0425(19) Uani 1 1 d . . . H10 H -0.0696 0.5871 0.3561 0.051 Uiso 1 1 calc R . . C11 C -0.0937(5) 0.5164(3) 0.3426(4) 0.0378(17) Uani 1 1 d . . . H11 H -0.1107 0.5112 0.3870 0.045 Uiso 1 1 calc R . . C12 C -0.0941(4) 0.4783(3) 0.2953(4) 0.0323(15) Uani 1 1 d . . . H12 H -0.1125 0.4482 0.3087 0.039 Uiso 1 1 calc R . . C13 C -0.0677(4) 0.4836(2) 0.2271(4) 0.0288(15) Uani 1 1 d . . . C14 C -0.0695(5) 0.3995(2) 0.2026(3) 0.0300(15) Uani 1 1 d . . . H14 H -0.1262 0.3959 0.2189 0.036 Uiso 1 1 calc R . . C15 C -0.0019(5) 0.3843(2) 0.2626(3) 0.0309(15) Uani 1 1 d . . . C16 C -0.0224(5) 0.3496(3) 0.3100(4) 0.0368(17) Uani 1 1 d . . . H16 H -0.0780 0.3370 0.3033 0.044 Uiso 1 1 calc R . . C17 C 0.0334(6) 0.3324(3) 0.3663(4) 0.046(2) Uani 1 1 d . . . H17 H 0.0164 0.3088 0.3962 0.055 Uiso 1 1 calc R . . C18 C 0.1167(6) 0.3519(3) 0.3767(4) 0.052(2) Uani 1 1 d . . . H18 H 0.1565 0.3412 0.4140 0.062 Uiso 1 1 calc R . . C19 C 0.1393(6) 0.3869(3) 0.3318(4) 0.0417(19) Uani 1 1 d . . . H19 H 0.1941 0.4004 0.3411 0.050 Uiso 1 1 calc R . . C20 C 0.0844(6) 0.4036(3) 0.2727(3) 0.0351(18) Uani 1 1 d . . . O21 O -0.0757(3) 0.43119(17) 0.0161(2) 0.0299(11) Uani 1 1 d . . . O22 O 0.1965(3) 0.48269(17) 0.1173(2) 0.0304(11) Uani 1 1 d . . . N21 N 0.0174(4) 0.3689(2) 0.1133(3) 0.0285(13) Uani 1 1 d . . . N22 N 0.1456(4) 0.3962(2) 0.0378(3) 0.0335(14) Uani 1 1 d . . . C21 C -0.1437(5) 0.4033(2) 0.0256(3) 0.0279(14) Uani 1 1 d . . . C22 C -0.2183(5) 0.4038(3) -0.0231(4) 0.0310(16) Uani 1 1 d . . . H22 H -0.2199 0.4247 -0.0614 0.037 Uiso 1 1 calc R . . C23 C -0.2903(5) 0.3754(3) -0.0187(4) 0.0388(18) Uani 1 1 d . . . H23 H -0.3372 0.3767 -0.0540 0.047 Uiso 1 1 calc R . . C24 C -0.2918(6) 0.3456(3) 0.0375(4) 0.048(2) Uani 1 1 d . . . H24 H -0.3405 0.3273 0.0427 0.058 Uiso 1 1 calc R . . C25 C -0.2177(5) 0.3432(3) 0.0879(4) 0.0394(18) Uani 1 1 d . . . H25 H -0.2177 0.3222 0.1260 0.047 Uiso 1 1 calc R . . C26 C -0.1442(5) 0.3709(2) 0.0831(4) 0.0289(15) Uani 1 1 d . . . C27 C -0.0660(5) 0.3640(2) 0.1393(4) 0.0308(16) Uani 1 1 d . . . H27 H -0.0690 0.3313 0.1580 0.037 Uiso 1 1 calc R . . C28 C 0.0348(5) 0.3396(2) 0.0604(4) 0.0317(17) Uani 1 1 d . . . C29 C -0.0129(5) 0.2968(2) 0.0386(4) 0.0401(19) Uani 1 1 d . . . H29 H -0.0588 0.2878 0.0624 0.048 Uiso 1 1 calc R . . C30 C 0.0074(6) 0.2689(3) -0.0164(4) 0.044(2) Uani 1 1 d . . . H30 H -0.0240 0.2409 -0.0278 0.053 Uiso 1 1 calc R . . C31 C 0.0734(6) 0.2813(3) -0.0555(4) 0.044(2) Uani 1 1 d . . . H31 H 0.0860 0.2626 -0.0934 0.053 Uiso 1 1 calc R . . C32 C 0.1191(5) 0.3224(2) -0.0356(4) 0.0382(18) Uani 1 1 d . . . H32 H 0.1635 0.3312 -0.0613 0.046 Uiso 1 1 calc R . . C33 C 0.1034(5) 0.3516(2) 0.0200(4) 0.0304(16) Uani 1 1 d . . . C34 C 0.2198(5) 0.4054(3) 0.0165(4) 0.0372(17) Uani 1 1 d . . . H34 H 0.2452 0.3803 -0.0058 0.045 Uiso 1 1 calc R . . C35 C 0.2671(4) 0.4499(3) 0.0234(3) 0.0295(15) Uani 1 1 d . . . C36 C 0.3312(5) 0.4564(3) -0.0203(4) 0.0426(17) Uani 1 1 d . . . H36 H 0.3416 0.4317 -0.0511 0.051 Uiso 1 1 calc R . . C37 C 0.3791(5) 0.4972(3) -0.0199(4) 0.0465(19) Uani 1 1 d . . . H37 H 0.4204 0.5003 -0.0506 0.056 Uiso 1 1 calc R . . C38 C 0.3663(5) 0.5343(3) 0.0266(4) 0.0426(19) Uani 1 1 d . . . H38 H 0.3986 0.5624 0.0271 0.051 Uiso 1 1 calc R . . C39 C 0.3046(5) 0.5287(3) 0.0721(4) 0.0364(17) Uani 1 1 d . . . H39 H 0.2965 0.5533 0.1038 0.044 Uiso 1 1 calc R . . C40 C 0.2537(4) 0.4868(2) 0.0718(3) 0.0287(15) Uani 1 1 d . . . O41 O 0.4443(3) 0.4524(2) 0.2942(2) 0.0435(13) Uani 1 1 d . . . O42 O 0.5245(3) 0.52904(16) 0.5080(2) 0.0264(10) Uani 1 1 d . . . N41 N 0.5797(4) 0.5190(2) 0.3357(3) 0.0345(15) Uani 1 1 d . . . N42 N 0.4757(4) 0.5842(2) 0.3848(3) 0.0294(14) Uani 1 1 d . . . C41 C 0.5073(5) 0.4249(3) 0.2774(4) 0.042(2) Uani 1 1 d . . . C42 C 0.4884(6) 0.3773(4) 0.2530(5) 0.067(3) Uani 1 1 d . . . H42 H 0.4323 0.3656 0.2512 0.080 Uiso 1 1 calc R . . C43 C 0.5514(7) 0.3480(4) 0.2318(5) 0.076(3) Uani 1 1 d . . . H43 H 0.5372 0.3170 0.2161 0.091 Uiso 1 1 calc R . . C44 C 0.6393(6) 0.3646(3) 0.2334(4) 0.050(2) Uani 1 1 d . . . H44 H 0.6825 0.3454 0.2187 0.060 Uiso 1 1 calc R . . C45 C 0.6543(6) 0.4090(3) 0.2570(4) 0.056(3) Uani 1 1 d . . . H45 H 0.7103 0.4206 0.2578 0.067 Uiso 1 1 calc R . . C46 C 0.5929(5) 0.4409(3) 0.2815(3) 0.0386(19) Uani 1 1 d . . . C47 C 0.6224(5) 0.4877(3) 0.3070(4) 0.0418(19) Uani 1 1 d . . . H47 H 0.6791 0.4956 0.3017 0.050 Uiso 1 1 calc R . . C48 C 0.6168(5) 0.5644(3) 0.3542(4) 0.0384(18) Uani 1 1 d . . . C49 C 0.7029(6) 0.5779(4) 0.3488(5) 0.053(2) Uani 1 1 d . . . H49 H 0.7390 0.5560 0.3300 0.063 Uiso 1 1 calc R . . C50 C 0.7346(6) 0.6217(4) 0.3702(5) 0.058(2) Uani 1 1 d . . . H50 H 0.7916 0.6298 0.3664 0.070 Uiso 1 1 calc R . . C51 C 0.6818(6) 0.6535(4) 0.3970(5) 0.061(3) Uani 1 1 d . . . H51 H 0.7035 0.6836 0.4110 0.074 Uiso 1 1 calc R . . C52 C 0.5971(5) 0.6431(3) 0.4046(5) 0.047(2) Uani 1 1 d . . . H52 H 0.5639 0.6656 0.4252 0.056 Uiso 1 1 calc R . . C53 C 0.5596(5) 0.5975(3) 0.3808(4) 0.0342(17) Uani 1 1 d . . . C54 C 0.4302(4) 0.6131(2) 0.4322(3) 0.0248(15) Uani 1 1 d . . . H54 H 0.4289 0.6464 0.4154 0.030 Uiso 1 1 calc R . . C55 C 0.4748(4) 0.6124(2) 0.5088(3) 0.0301(15) Uani 1 1 d . . . C56 C 0.4750(5) 0.6554(3) 0.5469(4) 0.0411(19) Uani 1 1 d . . . H56 H 0.4473 0.6822 0.5252 0.049 Uiso 1 1 calc R . . C57 C 0.5157(6) 0.6594(3) 0.6170(4) 0.052(2) Uani 1 1 d . . . H57 H 0.5167 0.6884 0.6414 0.062 Uiso 1 1 calc R . . C58 C 0.5541(5) 0.6187(3) 0.6485(4) 0.045(2) Uani 1 1 d . . . H58 H 0.5782 0.6197 0.6958 0.054 Uiso 1 1 calc R . . C59 C 0.5571(5) 0.5764(3) 0.6104(4) 0.0378(19) Uani 1 1 d . . . H59 H 0.5872 0.5504 0.6321 0.045 Uiso 1 1 calc R . . C60 C 0.5172(4) 0.5709(2) 0.5411(3) 0.0295(15) Uani 1 1 d . . . O61 O 0.3182(3) 0.52367(16) 0.3116(2) 0.0271(10) Uani 1 1 d . . . O62 O 0.4989(3) 0.42759(17) 0.4531(3) 0.0351(12) Uani 1 1 d . . . N61 N 0.3342(4) 0.5472(2) 0.4543(3) 0.0273(13) Uani 1 1 d . . . N62 N 0.3210(3) 0.4503(2) 0.4623(3) 0.0305(13) Uani 1 1 d . . . C61 C 0.2769(4) 0.5652(2) 0.3047(3) 0.0238(13) Uani 1 1 d . . . C62 C 0.2209(4) 0.5743(3) 0.2406(4) 0.0319(16) Uani 1 1 d . . . H62 H 0.2132 0.5505 0.2059 0.038 Uiso 1 1 calc R . . C63 C 0.1775(5) 0.6180(3) 0.2292(4) 0.0381(18) Uani 1 1 d . . . H63 H 0.1430 0.6233 0.1864 0.046 Uiso 1 1 calc R . . C64 C 0.1850(5) 0.6535(3) 0.2806(4) 0.0404(19) Uani 1 1 d . . . H64 H 0.1557 0.6826 0.2733 0.048 Uiso 1 1 calc R . . C65 C 0.2373(4) 0.6441(2) 0.3428(4) 0.0328(16) Uani 1 1 d . . . H65 H 0.2424 0.6678 0.3777 0.039 Uiso 1 1 calc R . . C66 C 0.2830(4) 0.6017(2) 0.3571(3) 0.0245(14) Uani 1 1 d . . . C67 C 0.3364(4) 0.5957(2) 0.4305(3) 0.0219(13) Uani 1 1 d . . . H67 H 0.3093 0.6156 0.4639 0.026 Uiso 1 1 calc R . . C68 C 0.2580(5) 0.5297(3) 0.4684(4) 0.0325(16) Uani 1 1 d . . . C69 C 0.1831(5) 0.5588(3) 0.4756(4) 0.0330(16) Uani 1 1 d . . . H69 H 0.1866 0.5920 0.4707 0.040 Uiso 1 1 calc R . . C70 C 0.1078(6) 0.5388(3) 0.4892(4) 0.050(2) Uani 1 1 d . . . H70 H 0.0615 0.5589 0.4946 0.060 Uiso 1 1 calc R . . C71 C 0.0976(6) 0.4901(4) 0.4954(5) 0.066(3) Uani 1 1 d . . . H71 H 0.0451 0.4771 0.5039 0.079 Uiso 1 1 calc R . . C72 C 0.1673(6) 0.4610(3) 0.4886(5) 0.063(3) Uani 1 1 d . . . H72 H 0.1611 0.4279 0.4933 0.076 Uiso 1 1 calc R . . C73 C 0.2468(5) 0.4791(3) 0.4748(5) 0.044(2) Uani 1 1 d . . . C74 C 0.3207(6) 0.4053(3) 0.4776(7) 0.075(3) Uani 1 1 d . . . H74 H 0.2746 0.3939 0.4992 0.090 Uiso 1 1 calc R . . C75 C 0.3870(6) 0.3704(3) 0.4639(6) 0.059(3) Uani 1 1 d . . . C76 C 0.3636(7) 0.3212(3) 0.4655(7) 0.091(4) Uani 1 1 d . . . H76 H 0.3092 0.3127 0.4763 0.109 Uiso 1 1 calc R . . C77 C 0.4219(8) 0.2855(3) 0.4511(7) 0.091(4) Uani 1 1 d . . . H77 H 0.4074 0.2532 0.4546 0.109 Uiso 1 1 calc R . . C78 C 0.5018(7) 0.2984(3) 0.4314(7) 0.078(4) Uani 1 1 d . . . H78 H 0.5388 0.2747 0.4184 0.094 Uiso 1 1 calc R . . C79 C 0.5256(6) 0.3451(3) 0.4311(5) 0.055(2) Uani 1 1 d . . . H79 H 0.5799 0.3527 0.4192 0.067 Uiso 1 1 calc R . . C80 C 0.4710(6) 0.3833(3) 0.4484(4) 0.046(2) Uani 1 1 d . . . O81 O 0.6165(3) 0.46142(19) 0.7239(2) 0.0326(10) Uani 1 1 d . . . O82 O 0.9047(3) 0.44787(17) 0.8181(2) 0.0304(10) Uani 1 1 d . . . N81 N 0.7141(4) 0.37648(19) 0.7707(3) 0.0278(12) Uani 1 1 d . . . N82 N 0.8480(4) 0.39154(19) 0.6969(3) 0.0286(12) Uani 1 1 d . . . C81 C 0.5559(5) 0.4424(3) 0.7575(3) 0.0323(16) Uani 1 1 d . . . C82 C 0.4815(5) 0.4682(3) 0.7647(4) 0.047(2) Uani 1 1 d . . . H82 H 0.4772 0.5000 0.7496 0.056 Uiso 1 1 calc R . . C83 C 0.4146(6) 0.4480(4) 0.7934(5) 0.060(2) Uani 1 1 d . . . H83 H 0.3653 0.4662 0.7969 0.072 Uiso 1 1 calc R . . C84 C 0.4186(6) 0.4014(4) 0.8172(5) 0.063(3) Uani 1 1 d . . . H84 H 0.3728 0.3881 0.8373 0.075 Uiso 1 1 calc R . . C85 C 0.4908(6) 0.3746(3) 0.8111(4) 0.049(2) Uani 1 1 d . . . H85 H 0.4930 0.3428 0.8262 0.059 Uiso 1 1 calc R . . C86 C 0.5618(5) 0.3942(3) 0.7825(4) 0.0322(16) Uani 1 1 d . . . C87 C 0.6368(5) 0.3638(2) 0.7826(4) 0.0317(15) Uani 1 1 d . . . H87 H 0.6291 0.3315 0.7924 0.038 Uiso 1 1 calc R . . C88 C 0.7816(5) 0.3420(2) 0.7781(3) 0.0273(14) Uani 1 1 d . . . C89 C 0.7822(5) 0.3024(2) 0.8215(4) 0.0346(17) Uani 1 1 d . . . H89 H 0.7363 0.2976 0.8473 0.042 Uiso 1 1 calc R . . C90 C 0.8495(5) 0.2693(3) 0.8279(4) 0.0400(18) Uani 1 1 d . . . H90 H 0.8482 0.2425 0.8568 0.048 Uiso 1 1 calc R . . C91 C 0.9186(5) 0.2771(3) 0.7903(4) 0.0381(18) Uani 1 1 d . . . H91 H 0.9641 0.2552 0.7937 0.046 Uiso 1 1 calc R . . C92 C 0.9197(5) 0.3177(2) 0.7473(4) 0.0300(15) Uani 1 1 d . . . H92 H 0.9673 0.3227 0.7235 0.036 Uiso 1 1 calc R . . C93 C 0.8517(4) 0.3514(2) 0.7383(3) 0.0267(14) Uani 1 1 d . . . C94 C 0.9289(4) 0.4087(2) 0.6762(3) 0.0257(14) Uani 1 1 d . . . H94 H 0.9513 0.3832 0.6479 0.031 Uiso 1 1 calc R . . C95 C 0.9996(4) 0.4198(2) 0.7385(4) 0.0324(16) Uani 1 1 d . . . C96 C 1.0860(5) 0.4124(3) 0.7266(5) 0.046(2) Uani 1 1 d . . . H96 H 1.0967 0.3986 0.6842 0.055 Uiso 1 1 calc R A 1 C97 C 1.1546(5) 0.4249(3) 0.7754(5) 0.051(2) Uani 1 1 d . . . H97 H 1.2110 0.4208 0.7657 0.061 Uiso 1 1 calc R . 1 C98 C 1.1384(5) 0.4433(3) 0.8380(5) 0.054(2) Uani 1 1 d . . . H98 H 1.1845 0.4514 0.8719 0.064 Uiso 1 1 calc R B 1 C99 C 1.0547(5) 0.4504(3) 0.8533(4) 0.0390(17) Uani 1 1 d . . . H99 H 1.0460 0.4622 0.8975 0.047 Uiso 1 1 calc R C 1 C100 C 0.9816(5) 0.4399(2) 0.8022(4) 0.0305(15) Uani 1 1 d . . . O101 O 0.7190(3) 0.46368(17) 0.6047(2) 0.0267(9) Uani 1 1 d . . . O102 O 0.7445(3) 0.49520(18) 0.8429(2) 0.0321(10) Uani 1 1 d . . . N101 N 0.8829(3) 0.49266(19) 0.6681(3) 0.0279(12) Uani 1 1 d . . . N102 N 0.7751(4) 0.5546(2) 0.7245(3) 0.0291(13) Uani 1 1 d . . . C101 C 0.7611(4) 0.4458(2) 0.5544(3) 0.0281(14) Uani 1 1 d . . . C102 C 0.7154(5) 0.4309(3) 0.4881(3) 0.0351(16) Uani 1 1 d . . . H102 H 0.6559 0.4352 0.4806 0.042 Uiso 1 1 calc R . . C103 C 0.7544(5) 0.4109(3) 0.4354(3) 0.0344(16) Uani 1 1 d . . . H103 H 0.7214 0.4025 0.3930 0.041 Uiso 1 1 calc R . . C104 C 0.8416(6) 0.4030(3) 0.4438(4) 0.0391(18) Uani 1 1 d . . . H104 H 0.8679 0.3880 0.4086 0.047 Uiso 1 1 calc R . . C105 C 0.8904(5) 0.4184(3) 0.5073(4) 0.0344(16) Uani 1 1 d . . . H105 H 0.9499 0.4137 0.5134 0.041 Uiso 1 1 calc R . . C106 C 0.8520(5) 0.4404(2) 0.5614(3) 0.0304(15) Uani 1 1 d . . . C107 C 0.9119(4) 0.4532(3) 0.6280(3) 0.0292(14) Uani 1 1 d . . . H107 H 0.9673 0.4627 0.6132 0.035 Uiso 1 1 calc R . 1 C108 C 0.8663(5) 0.5356(2) 0.6347(3) 0.0275(14) Uani 1 1 d . . . C109 C 0.8967(5) 0.5487(3) 0.5714(4) 0.0358(17) Uani 1 1 d . . . H109 H 0.9299 0.5268 0.5498 0.043 Uiso 1 1 calc R D 1 C110 C 0.8789(5) 0.5937(3) 0.5392(4) 0.0423(19) Uani 1 1 d . . . H110 H 0.9021 0.6014 0.4980 0.051 Uiso 1 1 calc R . . C111 C 0.8284(6) 0.6259(3) 0.5678(4) 0.044(2) Uani 1 1 d . . . H111 H 0.8159 0.6555 0.5460 0.053 Uiso 1 1 calc R . . C112 C 0.7953(5) 0.6144(2) 0.6303(4) 0.0368(17) Uani 1 1 d . . . H112 H 0.7604 0.6364 0.6499 0.044 Uiso 1 1 calc R . . C113 C 0.8136(5) 0.5704(2) 0.6638(3) 0.0277(14) Uani 1 1 d . . . C114 C 0.7427(5) 0.5854(3) 0.7629(4) 0.0314(16) Uani 1 1 d . . . H114 H 0.7503 0.6175 0.7515 0.038 Uiso 1 1 calc R . . C115 C 0.6948(5) 0.5765(2) 0.8227(3) 0.0299(15) Uani 1 1 d . . . C116 C 0.6463(6) 0.6143(3) 0.8460(4) 0.050(2) Uani 1 1 d . . . H116 H 0.6482 0.6442 0.8245 0.061 Uiso 1 1 calc R . . C117 C 0.5957(6) 0.6086(4) 0.8996(5) 0.060(3) Uani 1 1 d . . . H117 H 0.5632 0.6342 0.9133 0.072 Uiso 1 1 calc R . . C118 C 0.5939(7) 0.5642(4) 0.9332(5) 0.060(3) Uani 1 1 d . . . H118 H 0.5599 0.5602 0.9695 0.071 Uiso 1 1 calc R . . C119 C 0.6418(5) 0.5264(3) 0.9132(4) 0.0415(19) Uani 1 1 d . . . H119 H 0.6400 0.4972 0.9368 0.050 Uiso 1 1 calc R . . C120 C 0.6940(4) 0.5304(2) 0.8577(3) 0.0284(15) Uani 1 1 d . . . N121 N 0.2770(5) 0.3311(3) 0.2354(4) 0.060(2) Uani 1 1 d . . . C121 C 0.2013(6) 0.3204(3) 0.1987(5) 0.060(3) Uani 1 1 d . . . H121 H 0.1710 0.3449 0.1734 0.072 Uiso 1 1 calc R . . C122 C 0.1662(11) 0.2770(4) 0.1959(9) 0.155(6) Uani 1 1 d U . . H122 H 0.1130 0.2717 0.1690 0.186 Uiso 1 1 calc R . . C123 C 0.2068(12) 0.2411(5) 0.2313(10) 0.165(6) Uani 1 1 d U . . H123 H 0.1835 0.2103 0.2282 0.198 Uiso 1 1 calc R . . C124 C 0.2838(12) 0.2498(5) 0.2728(10) 0.167(6) Uani 1 1 d U . . H124 H 0.3128 0.2257 0.3001 0.200 Uiso 1 1 calc R . . C125 C 0.3152(8) 0.2944(4) 0.2720(7) 0.090(4) Uani 1 1 d . . . H125 H 0.3679 0.3003 0.2993 0.108 Uiso 1 1 calc R . . N122 N 0.5754(5) 0.5385(3) 0.1470(3) 0.0490(18) Uani 1 1 d . . . C126 C 0.5758(6) 0.4958(3) 0.1141(4) 0.050(2) Uani 1 1 d . . . H126 H 0.5234 0.4809 0.0988 0.060 Uiso 1 1 calc R . . C127 C 0.6517(7) 0.4732(3) 0.1021(4) 0.060(3) Uani 1 1 d . . . H127 H 0.6495 0.4439 0.0784 0.072 Uiso 1 1 calc R . . C128 C 0.7285(7) 0.4935(4) 0.1246(5) 0.069(3) Uani 1 1 d . . . H128 H 0.7797 0.4783 0.1175 0.083 Uiso 1 1 calc R . . C129 C 0.7293(7) 0.5363(4) 0.1575(6) 0.071(3) Uani 1 1 d . . . H129 H 0.7815 0.5513 0.1733 0.085 Uiso 1 1 calc R . . C130 C 0.6533(6) 0.5576(4) 0.1677(5) 0.058(2) Uani 1 1 d . . . H130 H 0.6557 0.5873 0.1904 0.070 Uiso 1 1 calc R . . N123 N 0.4087(6) 0.6428(3) 0.1425(4) 0.059(2) Uani 1 1 d . . . C131 C 0.3375(7) 0.6644(3) 0.1144(5) 0.058(2) Uani 1 1 d . . . H131 H 0.2856 0.6482 0.1153 0.070 Uiso 1 1 calc R . . C132 C 0.3342(7) 0.7085(3) 0.0843(5) 0.062(3) Uani 1 1 d . . . H132 H 0.2820 0.7215 0.0637 0.074 Uiso 1 1 calc R . . C133 C 0.4094(9) 0.7335(4) 0.0852(6) 0.083(4) Uani 1 1 d . . . H133 H 0.4100 0.7645 0.0665 0.100 Uiso 1 1 calc R . . C134 C 0.4855(9) 0.7111(5) 0.1150(7) 0.097(4) Uani 1 1 d . . . H134 H 0.5383 0.7268 0.1161 0.116 Uiso 1 1 calc R . . C135 C 0.4816(5) 0.6665(3) 0.1421(3) 0.079(3) Uani 1 1 d . . . H135 H 0.5327 0.6518 0.1615 0.094 Uiso 1 1 calc R . . N124 N 0.4033(5) 0.4038(3) 0.6320(3) 0.055(4) Uani 0.50 1 d PR . . C136 C 0.3270(5) 0.4300(3) 0.6210(3) 0.071(6) Uani 0.50 1 d PR . . H136 H 0.3285 0.4629 0.6121 0.086 Uiso 0.50 1 calc PR . . C137 C 0.2483(5) 0.4071(3) 0.6234(3) 0.098(9) Uani 0.50 1 d PR . . H137 H 0.1972 0.4246 0.6161 0.117 Uiso 0.50 1 calc PR . . C138 C 0.2460(5) 0.3580(3) 0.6368(3) 0.084(7) Uani 0.50 1 d PR . . H138 H 0.1933 0.3427 0.6384 0.100 Uiso 0.50 1 calc PR . . C139 C 0.3223(5) 0.3318(3) 0.6477(3) 0.107(10) Uani 0.50 1 d PR . . H139 H 0.3208 0.2989 0.6567 0.129 Uiso 0.50 1 calc PR . . C140 C 0.4010(5) 0.3547(3) 0.6454(3) 0.083(7) Uani 0.50 1 d PR . . H140 H 0.4521 0.3372 0.6527 0.100 Uiso 0.50 1 calc PR . . N125 N 0.9389(6) 0.2810(3) 0.5762(4) 0.065(2) Uani 1 1 d . . . C141 C 1.0113(10) 0.2902(4) 0.5474(6) 0.087(4) Uani 1 1 d . . . H141 H 1.0204 0.3215 0.5328 0.104 Uiso 1 1 calc R . . C142 C 1.0729(10) 0.2563(6) 0.5382(7) 0.106(5) Uani 1 1 d . . . H142 H 1.1222 0.2645 0.5183 0.128 Uiso 1 1 calc R . . C143 C 1.0594(11) 0.2095(5) 0.5591(7) 0.107(5) Uani 1 1 d . . . H143 H 1.0995 0.1854 0.5542 0.129 Uiso 1 1 calc R . . C144 C 0.9822(12) 0.1995(5) 0.5884(7) 0.107(5) Uani 1 1 d . . . H144 H 0.9684 0.1686 0.6016 0.128 Uiso 1 1 calc R . . C145 C 0.9309(8) 0.2364(4) 0.5961(6) 0.075(3) Uani 1 1 d . . . H145 H 0.8827 0.2298 0.6186 0.090 Uiso 1 1 calc R . . N126 N 0.7499(7) 0.2693(3) 0.4542(5) 0.0814(17) Uani 1 1 d . . . C146 C 0.7325(9) 0.2257(4) 0.4632(6) 0.0814(17) Uani 1 1 d . . . H146 H 0.7090 0.2184 0.5044 0.098 Uiso 1 1 calc R . . C147 C 0.7441(9) 0.1878(4) 0.4195(6) 0.0814(17) Uani 1 1 d . . . H147 H 0.7147 0.1589 0.4224 0.098 Uiso 1 1 calc R E 1 C148 C 0.7966(19) 0.1939(9) 0.3751(12) 0.0814(17) Uani 0.501(10) 1 d P . 1 H148 H 0.8189 0.1679 0.3526 0.098 Uiso 0.501(10) 1 calc PR . 1 C149 C 0.8196(18) 0.2402(8) 0.3613(12) 0.0814(17) Uani 0.501(10) 1 d P . 1 H149 H 0.8422 0.2476 0.3198 0.098 Uiso 0.501(10) 1 calc PR . 1 C150 C 0.809(2) 0.2750(8) 0.4092(12) 0.0814(17) Uani 0.501(10) 1 d P . 1 H150 H 0.8422 0.3029 0.4109 0.098 Uiso 0.501(10) 1 calc PR . 1 C48B C 0.7246(19) 0.2001(8) 0.3495(12) 0.0814(17) Uani 0.499(10) 1 d P . 2 H48B H 0.7152 0.1765 0.3147 0.098 Uiso 0.499(10) 1 calc PR . 2 C49B C 0.7189(18) 0.2497(8) 0.3314(12) 0.0814(17) Uani 0.499(10) 1 d P . 2 H49B H 0.6994 0.2595 0.2855 0.098 Uiso 0.499(10) 1 calc PR . 2 C50B C 0.742(2) 0.2811(8) 0.3816(12) 0.0814(17) Uani 0.499(10) 1 d P . 2 H50B H 0.7538 0.3125 0.3688 0.098 Uiso 0.499(10) 1 calc PR . 2 N127 N 0.6462(7) 0.2881(4) 0.6282(4) 0.089(3) Uani 1 1 d . . . C151 C 0.6686(9) 0.2554(3) 0.6769(5) 0.074(3) Uani 1 1 d . . . H151 H 0.7272 0.2502 0.6907 0.088 Uiso 1 1 calc R . . C152 C 0.6101(10) 0.2278(4) 0.7092(6) 0.076(4) Uani 1 1 d . . . H152 H 0.6290 0.2022 0.7386 0.091 Uiso 1 1 calc R F 1 C153 C 0.5219(18) 0.2397(11) 0.6964(14) 0.064(7) Uani 0.565(19) 1 d P . 1 H153 H 0.4814 0.2208 0.7154 0.077 Uiso 0.565(19) 1 calc PR . 1 C154 C 0.4951(13) 0.2799(9) 0.6551(11) 0.075(7) Uani 0.565(19) 1 d P . 1 H154 H 0.4374 0.2891 0.6506 0.090 Uiso 0.565(19) 1 calc PR . 1 C155 C 0.5516(14) 0.3061(7) 0.6214(9) 0.063(6) Uani 0.565(19) 1 d P . 1 H155 H 0.5340 0.3335 0.5954 0.075 Uiso 0.565(19) 1 calc PR . 1 C53B C 0.532(3) 0.2254(15) 0.675(3) 0.082(14) Uani 0.435(19) 1 d P . 2 H53B H 0.4898 0.2055 0.6897 0.098 Uiso 0.435(19) 1 calc PR . 2 C54B C 0.5172(16) 0.2517(7) 0.6201(14) 0.051(6) Uani 0.435(19) 1 d P . 2 H54B H 0.4611 0.2534 0.5970 0.061 Uiso 0.435(19) 1 calc PR . 2 C55B C 0.5791(4) 0.2772(2) 0.5940(4) 0.054(7) Uani 0.435(19) 1 d P . 2 H55B H 0.5693 0.2869 0.5470 0.064 Uiso 0.435(19) 1 calc PR . 2 N128 N 0.8501(4) 0.5979(2) 0.9576(4) 0.149(4) Uani 1 1 d R . . C156 C 0.7985(4) 0.6014(2) 1.0117(4) 0.149(4) Uani 1 1 d R . . H156 H 0.7811 0.5736 1.0332 0.179 Uiso 1 1 calc R . . C157 C 0.7731(4) 0.6463(2) 1.0336(4) 0.149(4) Uani 1 1 d R . . H157 H 0.7386 0.6486 1.0698 0.179 Uiso 1 1 calc R . . C158 C 0.7992(4) 0.6877(2) 1.0015(4) 0.149(4) Uani 1 1 d R . . H158 H 0.7822 0.7177 1.0162 0.179 Uiso 1 1 calc R . . C159 C 0.8508(4) 0.6843(2) 0.9474(4) 0.149(4) Uani 1 1 d R . . H159 H 0.8683 0.7120 0.9259 0.179 Uiso 1 1 calc R . . C160 C 0.8763(4) 0.6394(2) 0.9255(4) 0.149(4) Uani 1 1 d R . . H160 H 0.9108 0.6371 0.8893 0.179 Uiso 1 1 calc R . . N129 N 1.2186(8) 0.5497(4) 0.7258(6) 0.099(4) Uani 1 1 d . . . C161 C 1.2586(9) 0.5633(5) 0.7859(6) 0.092(4) Uani 1 1 d . . . H161 H 1.2284 0.5620 0.8249 0.111 Uiso 1 1 calc R G 1 C162 C 1.3443(10) 0.5801(5) 0.7973(8) 0.100(4) Uani 1 1 d . . . H162 H 1.3709 0.5861 0.8430 0.120 Uiso 1 1 calc R . . C163 C 1.3886(10) 0.5875(5) 0.7398(9) 0.103(4) Uani 1 1 d . . . H163 H 1.4434 0.6011 0.7439 0.124 Uiso 1 1 calc R . . C164 C 1.3454(9) 0.5733(5) 0.6768(7) 0.085(4) Uani 1 1 d . . . H164 H 1.3747 0.5755 0.6374 0.102 Uiso 1 1 calc R . . C165 C 1.2625(5) 0.5560(2) 0.6661(4) 0.078(3) Uani 1 1 d . . . H165 H 1.2360 0.5486 0.6208 0.094 Uiso 1 1 calc R . . N130 N 1.0313(5) 0.6251(2) 0.7413(4) 0.198(4) Uani 1 1 d R . . C166 C 1.0542(5) 0.6496(2) 0.8046(4) 0.198(4) Uani 1 1 d R . . H166 H 1.0724 0.6326 0.8459 0.238 Uiso 1 1 calc R H 2 C167 C 1.0499(5) 0.6995(2) 0.8062(4) 0.198(4) Uani 1 1 d R . . H167 H 1.0653 0.7159 0.8485 0.238 Uiso 1 1 calc R . . C168 C 1.0227(5) 0.7250(2) 0.7445(4) 0.198(4) Uani 1 1 d R . . H168 H 1.0199 0.7584 0.7455 0.238 Uiso 1 1 calc R . . C169 C 0.9998(5) 0.7005(2) 0.6812(4) 0.198(4) Uani 1 1 d R . . H169 H 0.9816 0.7175 0.6400 0.238 Uiso 1 1 calc R . . C170 C 1.0041(5) 0.6505(2) 0.6797(4) 0.198(4) Uani 1 1 d R . . H170 H 0.9888 0.6341 0.6373 0.238 Uiso 1 1 calc R . . N131 N 0.2904(13) 0.2186(10) 0.8049(13) 0.095(7) Uani 0.50 1 d P . . C171 C 0.283(2) 0.2646(12) 0.8019(10) 0.097(11) Uani 0.50 1 d P . . H171 H 0.3300 0.2846 0.8162 0.116 Uiso 0.50 1 calc PR . . C172 C 0.204(3) 0.2829(8) 0.7768(14) 0.113(13) Uani 0.50 1 d P . . H172 H 0.1941 0.3157 0.7811 0.136 Uiso 0.50 1 calc PR . . C173 C 0.1463(15) 0.2579(11) 0.7495(16) 0.090(9) Uani 0.50 1 d P . . H173 H 0.0976 0.2715 0.7238 0.108 Uiso 0.50 1 calc PR . . C174 C 0.1533(18) 0.2125(11) 0.7565(11) 0.092(10) Uani 0.50 1 d P . . H174 H 0.1062 0.1924 0.7438 0.110 Uiso 0.50 1 calc PR . . C175 C 0.225(2) 0.1957(7) 0.7806(11) 0.093(10) Uani 0.50 1 d P . . H175 H 0.2301 0.1624 0.7804 0.112 Uiso 0.50 1 calc PR . . N132 N 0.4164(8) 0.3114(4) -0.0488(6) 0.094(3) Uani 1 1 d . . . C176 C 0.3578(9) 0.2869(5) -0.0182(6) 0.088(4) Uani 1 1 d . . . H176 H 0.3258 0.2631 -0.0438 0.106 Uiso 1 1 calc R . . C177 C 0.3442(8) 0.2956(6) 0.0470(7) 0.112(6) Uani 1 1 d . . . H177 H 0.3028 0.2779 0.0668 0.135 Uiso 1 1 calc R . . C178 C 0.3882(9) 0.3292(6) 0.0853(7) 0.104(5) Uani 1 1 d . . . H178 H 0.3774 0.3356 0.1313 0.125 Uiso 1 1 calc R . . C179 C 0.4494(8) 0.3543(5) 0.0562(7) 0.084(4) Uani 1 1 d . . . H179 H 0.4832 0.3772 0.0823 0.101 Uiso 1 1 calc R . . C180 C 0.4597(6) 0.3450(3) -0.0122(5) 0.069(3) Uani 1 1 d . . . H180 H 0.4991 0.3632 -0.0336 0.083 Uiso 1 1 calc R . . N133 N 0.3756(6) 0.7155(3) 0.7623(5) 0.36(5) Uani 0.50 1 d PR . . C181 C 0.4647(6) 0.7172(3) 0.7797(5) 0.131(16) Uani 0.50 1 d PR . . H181 H 0.5004 0.7145 0.7445 0.157 Uiso 0.50 1 calc PR . . C182 C 0.5004(6) 0.7231(3) 0.8499(5) 0.113(9) Uani 0.50 1 d PRU . . H182 H 0.5601 0.7242 0.8616 0.136 Uiso 0.50 1 calc PR . . C183 C 0.4471(6) 0.7271(3) 0.9026(5) 0.136(16) Uani 0.50 1 d PR . . H183 H 0.4710 0.7310 0.9496 0.163 Uiso 0.50 1 calc PR . . C184 C 0.3579(6) 0.7253(3) 0.8852(5) 0.131(16) Uani 0.50 1 d PR . . H184 H 0.3222 0.7280 0.9205 0.157 Uiso 0.50 1 calc PR . . C185 C 0.3222(6) 0.7195(3) 0.8150(5) 0.154(17) Uani 0.50 1 d PR . . H185 H 0.2625 0.7183 0.8033 0.184 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02265(17) 0.02404(18) 0.02757(17) -0.00066(15) -0.00118(13) -0.00042(16) Nd2 0.02213(17) 0.02406(19) 0.02863(17) -0.00286(15) -0.00266(14) 0.00485(16) Nd3 0.02047(17) 0.02581(17) 0.02667(16) 0.00288(14) -0.00024(13) 0.00096(16) K1 0.0277(8) 0.0394(9) 0.0383(8) -0.0019(7) -0.0040(7) 0.0015(7) K2 0.0330(9) 0.0375(9) 0.0480(9) -0.0014(7) 0.0030(7) -0.0005(8) K3 0.0306(9) 0.0504(10) 0.0370(9) 0.0098(7) 0.0023(7) 0.0024(8) K4 0.0308(8) 0.0462(9) 0.0337(7) 0.0083(7) -0.0016(6) -0.0041(8) K5 0.0276(9) 0.0413(9) 0.0440(9) 0.0087(7) 0.0004(7) 0.0042(7) K6 0.0647(13) 0.0342(9) 0.0439(10) -0.0012(7) 0.0080(9) -0.0058(9) K7 0.0546(11) 0.0314(9) 0.0583(10) -0.0044(8) -0.0271(9) 0.0069(9) K8 0.0395(10) 0.0243(7) 0.0346(8) 0.0009(6) -0.0011(7) 0.0010(7) K9 0.0404(16) 0.0388(14) 0.141(3) 0.0224(16) -0.0336(18) -0.0114(12) K9B 0.055(7) 0.030(5) 0.066(7) 0.013(4) -0.019(5) -0.011(4) O1 0.044(3) 0.031(3) 0.030(2) 0.002(2) -0.003(2) -0.003(2) O2 0.021(2) 0.041(3) 0.029(2) 0.008(2) -0.003(2) -0.002(2) N1 0.026(3) 0.026(3) 0.036(3) -0.002(2) 0.003(3) 0.009(3) N2 0.023(3) 0.025(3) 0.036(3) 0.000(2) -0.003(2) 0.003(2) C1 0.028(4) 0.027(3) 0.028(3) 0.006(3) -0.003(3) -0.004(3) C2 0.053(6) 0.035(4) 0.048(5) -0.006(3) 0.014(4) -0.004(4) C3 0.084(8) 0.037(5) 0.055(5) 0.003(4) 0.023(5) -0.003(5) C4 0.064(6) 0.029(4) 0.056(5) 0.011(4) 0.008(4) -0.008(4) C5 0.049(5) 0.028(4) 0.033(4) 0.000(3) -0.003(4) 0.007(4) C6 0.028(4) 0.028(4) 0.022(3) 0.003(3) -0.004(3) 0.004(3) C7 0.027(4) 0.026(4) 0.041(4) -0.003(3) 0.001(3) 0.007(3) C8 0.015(3) 0.028(3) 0.033(4) 0.000(3) 0.007(3) -0.002(3) C9 0.039(4) 0.030(4) 0.041(4) -0.003(3) 0.008(3) 0.009(3) C10 0.039(5) 0.041(4) 0.048(5) -0.004(3) 0.005(4) 0.008(4) C11 0.031(4) 0.047(5) 0.035(4) 0.001(3) 0.004(3) 0.006(4) C12 0.021(3) 0.033(4) 0.042(4) 0.004(3) 0.003(3) 0.003(3) C13 0.019(3) 0.025(3) 0.041(4) -0.001(3) 0.001(3) 0.001(3) C14 0.029(4) 0.028(3) 0.032(4) 0.002(3) 0.004(3) -0.004(3) C15 0.035(4) 0.030(4) 0.027(3) 0.004(3) 0.002(3) 0.004(3) C16 0.037(5) 0.035(4) 0.041(4) 0.003(3) 0.017(3) 0.001(3) C17 0.061(6) 0.042(4) 0.037(4) 0.019(3) 0.017(4) 0.009(4) C18 0.059(6) 0.052(5) 0.042(5) 0.018(4) 0.002(4) 0.011(5) C19 0.037(5) 0.045(5) 0.043(4) 0.014(3) 0.006(4) 0.012(4) C20 0.055(5) 0.027(4) 0.022(3) 0.003(3) -0.001(3) 0.016(4) O21 0.027(3) 0.031(2) 0.029(2) -0.0005(19) -0.005(2) -0.005(2) O22 0.029(3) 0.039(3) 0.023(2) -0.0009(19) -0.001(2) -0.007(2) N21 0.023(3) 0.019(3) 0.043(3) 0.003(2) 0.001(3) -0.004(3) N22 0.026(3) 0.037(3) 0.036(3) -0.006(3) -0.004(3) 0.008(3) C21 0.027(4) 0.028(3) 0.028(3) -0.002(3) 0.002(3) -0.004(3) C22 0.027(4) 0.036(4) 0.030(4) -0.006(3) 0.004(3) 0.002(3) C23 0.026(4) 0.049(5) 0.039(4) -0.007(3) -0.004(3) -0.009(4) C24 0.036(5) 0.055(5) 0.052(5) -0.006(4) 0.001(4) -0.007(4) C25 0.033(4) 0.045(4) 0.041(4) -0.002(3) 0.009(3) -0.005(4) C26 0.024(4) 0.023(3) 0.040(4) 0.001(3) 0.005(3) -0.007(3) C27 0.022(4) 0.021(3) 0.047(4) 0.000(3) -0.003(3) -0.005(3) C28 0.035(4) 0.019(3) 0.040(4) 0.004(3) -0.004(3) 0.003(3) C29 0.036(4) 0.025(4) 0.055(5) 0.000(3) -0.008(4) -0.002(3) C30 0.046(5) 0.024(4) 0.060(5) -0.003(3) 0.001(4) 0.001(4) C31 0.045(5) 0.035(4) 0.051(5) -0.010(4) 0.000(4) 0.007(4) C32 0.044(5) 0.025(4) 0.046(4) -0.006(3) 0.007(4) 0.006(3) C33 0.028(4) 0.021(3) 0.039(4) -0.005(3) -0.007(3) 0.005(3) C34 0.027(4) 0.039(4) 0.046(4) -0.001(3) 0.010(3) 0.007(3) C35 0.020(3) 0.032(4) 0.036(3) -0.001(3) 0.001(3) 0.001(3) C36 0.032(4) 0.052(5) 0.044(4) -0.012(4) 0.004(3) -0.001(4) C37 0.030(4) 0.063(5) 0.048(4) 0.001(4) 0.008(3) -0.013(4) C38 0.037(5) 0.048(5) 0.040(4) -0.007(4) -0.005(4) -0.010(4) C39 0.040(5) 0.036(4) 0.034(4) -0.007(3) 0.007(3) -0.015(4) C40 0.024(3) 0.036(4) 0.025(3) -0.001(3) -0.003(3) 0.004(3) O41 0.034(3) 0.054(3) 0.039(3) -0.020(3) -0.007(2) 0.015(3) O42 0.024(3) 0.024(2) 0.030(2) -0.0023(18) -0.0017(19) 0.003(2) N41 0.026(3) 0.042(4) 0.034(3) 0.005(3) 0.003(3) 0.008(3) N42 0.026(3) 0.037(4) 0.025(3) 0.002(2) 0.003(2) 0.003(3) C41 0.038(5) 0.053(5) 0.032(4) -0.014(3) -0.003(3) 0.014(4) C42 0.042(6) 0.074(7) 0.080(7) -0.044(6) -0.007(5) 0.011(5) C43 0.060(7) 0.074(7) 0.087(7) -0.047(6) -0.016(6) 0.022(6) C44 0.066(6) 0.047(5) 0.035(4) -0.012(3) -0.008(4) 0.025(5) C45 0.056(6) 0.070(6) 0.046(5) 0.016(4) 0.018(4) 0.034(5) C46 0.044(5) 0.049(5) 0.022(3) 0.000(3) 0.001(3) 0.022(4) C47 0.029(4) 0.047(5) 0.053(5) 0.011(4) 0.017(4) 0.016(4) C48 0.039(5) 0.047(5) 0.029(4) 0.013(3) 0.001(3) 0.006(4) C49 0.030(5) 0.073(6) 0.056(5) 0.003(5) 0.007(4) 0.007(5) C50 0.032(5) 0.081(7) 0.061(6) -0.004(5) 0.001(4) -0.008(5) C51 0.040(5) 0.065(6) 0.074(6) 0.009(5) -0.010(5) -0.014(5) C52 0.020(4) 0.047(5) 0.072(6) 0.000(4) 0.003(4) -0.003(4) C53 0.027(4) 0.042(4) 0.032(4) 0.012(3) -0.002(3) 0.002(3) C54 0.025(4) 0.018(3) 0.029(3) -0.006(3) -0.005(3) 0.000(3) C55 0.023(4) 0.033(4) 0.032(4) -0.007(3) -0.004(3) 0.005(3) C56 0.041(5) 0.037(4) 0.041(4) -0.015(3) -0.010(4) 0.013(4) C57 0.051(6) 0.051(5) 0.049(5) -0.024(4) -0.008(4) 0.010(4) C58 0.041(5) 0.057(5) 0.033(4) -0.012(4) -0.012(4) 0.015(4) C59 0.039(5) 0.039(4) 0.032(4) -0.003(3) -0.007(3) 0.010(4) C60 0.024(4) 0.031(4) 0.033(4) 0.002(3) 0.000(3) 0.002(3) O61 0.022(2) 0.030(2) 0.026(2) -0.0055(18) -0.0061(19) 0.002(2) O62 0.025(3) 0.029(3) 0.048(3) 0.001(2) -0.007(2) 0.003(2) N61 0.018(3) 0.029(3) 0.034(3) 0.006(2) 0.002(2) 0.005(3) N62 0.017(3) 0.020(3) 0.058(3) 0.010(3) 0.019(2) 0.004(2) C61 0.025(3) 0.015(3) 0.031(3) 0.000(2) 0.000(3) -0.004(3) C62 0.024(4) 0.040(4) 0.031(4) 0.006(3) 0.000(3) -0.002(3) C63 0.031(4) 0.041(4) 0.038(4) 0.009(3) -0.013(3) 0.003(3) C64 0.038(4) 0.027(4) 0.052(5) 0.006(3) -0.011(4) 0.005(3) C65 0.024(4) 0.027(3) 0.046(4) -0.007(3) -0.002(3) 0.002(3) C66 0.017(3) 0.022(3) 0.033(3) 0.005(3) 0.000(3) 0.004(3) C67 0.016(3) 0.021(3) 0.028(3) 0.002(2) 0.001(3) 0.001(3) C68 0.030(4) 0.029(4) 0.040(4) 0.005(3) 0.010(3) 0.004(3) C69 0.026(4) 0.037(4) 0.037(4) 0.000(3) 0.009(3) 0.005(3) C70 0.038(5) 0.052(5) 0.065(6) 0.008(4) 0.028(4) 0.012(4) C71 0.036(5) 0.070(7) 0.096(7) 0.032(6) 0.024(5) -0.004(5) C72 0.041(5) 0.038(5) 0.114(7) 0.036(5) 0.027(5) -0.003(5) C73 0.031(4) 0.032(4) 0.067(5) 0.024(4) 0.001(4) -0.001(3) C74 0.032(5) 0.031(5) 0.161(11) 0.027(6) 0.011(6) -0.003(4) C75 0.046(6) 0.033(4) 0.096(7) 0.007(5) -0.003(5) 0.003(4) C76 0.041(6) 0.033(5) 0.192(14) 0.006(7) -0.014(8) -0.001(5) C77 0.072(8) 0.019(4) 0.169(12) 0.014(6) -0.030(8) -0.001(5) C78 0.059(7) 0.025(4) 0.138(10) -0.006(5) -0.034(7) 0.007(5) C79 0.045(5) 0.027(4) 0.089(7) -0.004(4) -0.008(5) 0.011(4) C80 0.044(5) 0.027(4) 0.061(5) -0.005(3) -0.015(4) 0.009(4) O81 0.026(2) 0.036(2) 0.036(2) 0.001(2) 0.0068(18) -0.002(2) O82 0.021(2) 0.038(3) 0.031(2) 0.006(2) -0.0039(18) 0.007(2) N81 0.030(3) 0.023(3) 0.029(3) 0.009(2) 0.000(2) -0.005(2) N82 0.020(3) 0.023(3) 0.042(3) 0.005(2) 0.000(2) 0.001(2) C81 0.030(4) 0.041(4) 0.025(3) 0.000(3) 0.003(3) -0.008(3) C82 0.032(4) 0.050(5) 0.060(5) 0.012(4) 0.012(4) 0.011(4) C83 0.044(5) 0.057(6) 0.082(6) 0.003(5) 0.021(5) 0.003(5) C84 0.037(5) 0.062(6) 0.096(7) 0.007(5) 0.035(5) 0.003(5) C85 0.039(5) 0.045(5) 0.064(5) 0.006(4) 0.011(4) -0.010(4) C86 0.023(4) 0.037(4) 0.038(4) -0.003(3) 0.010(3) -0.004(3) C87 0.026(4) 0.027(3) 0.042(4) 0.004(3) 0.001(3) -0.004(3) C88 0.027(4) 0.023(3) 0.032(3) 0.000(3) 0.001(3) -0.001(3) C89 0.039(4) 0.029(4) 0.034(4) 0.002(3) -0.002(3) -0.002(3) C90 0.040(5) 0.029(4) 0.049(5) 0.010(3) -0.002(4) -0.002(3) C91 0.040(5) 0.027(4) 0.043(4) -0.003(3) -0.010(4) 0.000(3) C92 0.027(4) 0.025(3) 0.038(4) -0.005(3) 0.004(3) 0.001(3) C93 0.026(4) 0.018(3) 0.034(3) -0.003(3) -0.001(3) -0.003(3) C94 0.015(3) 0.028(3) 0.034(3) -0.002(3) 0.002(3) 0.002(3) C95 0.019(3) 0.018(3) 0.057(5) 0.011(3) -0.003(3) 0.004(3) C96 0.027(4) 0.037(4) 0.076(6) -0.004(4) 0.008(4) 0.002(4) C97 0.016(4) 0.045(5) 0.090(7) -0.004(4) -0.004(4) 0.000(4) C98 0.031(4) 0.044(5) 0.078(6) -0.006(4) -0.018(4) -0.001(4) C99 0.032(4) 0.040(4) 0.041(4) 0.004(3) -0.009(3) 0.000(4) C100 0.029(4) 0.025(3) 0.036(4) 0.009(3) -0.005(3) 0.001(3) O101 0.022(2) 0.034(2) 0.0237(19) 0.0017(19) -0.0004(16) 0.002(2) O102 0.034(3) 0.037(3) 0.024(2) 0.007(2) -0.0003(19) 0.009(2) N101 0.022(3) 0.022(3) 0.039(3) 0.006(2) -0.002(2) 0.004(2) N102 0.028(3) 0.027(3) 0.033(3) 0.002(2) 0.004(2) 0.002(3) C101 0.018(3) 0.032(4) 0.034(3) 0.004(3) 0.000(3) 0.005(3) C102 0.036(4) 0.040(4) 0.030(4) 0.003(3) 0.003(3) 0.004(3) C103 0.040(4) 0.040(4) 0.022(3) -0.004(3) 0.003(3) 0.002(4) C104 0.048(5) 0.036(4) 0.036(4) 0.004(3) 0.018(4) 0.004(4) C105 0.028(4) 0.029(4) 0.049(4) 0.010(3) 0.015(3) 0.002(3) C106 0.030(4) 0.027(3) 0.032(4) 0.006(3) 0.001(3) 0.001(3) C107 0.016(3) 0.033(4) 0.040(3) 0.007(3) 0.006(2) 0.000(3) C108 0.028(4) 0.028(3) 0.026(3) 0.004(3) -0.002(3) -0.003(3) C109 0.027(4) 0.031(4) 0.049(4) -0.002(3) 0.007(3) -0.007(3) C110 0.039(5) 0.043(4) 0.047(4) 0.015(4) 0.015(4) -0.003(4) C111 0.054(6) 0.030(4) 0.050(5) 0.011(3) 0.013(4) 0.005(4) C112 0.045(5) 0.027(3) 0.040(4) 0.000(3) 0.011(3) 0.005(3) C113 0.030(4) 0.025(3) 0.027(3) 0.003(3) -0.001(3) 0.002(3) C114 0.026(4) 0.031(4) 0.035(4) 0.002(3) -0.004(3) -0.009(3) C115 0.034(4) 0.032(4) 0.023(3) 0.004(3) 0.002(3) 0.007(3) C116 0.059(6) 0.050(5) 0.045(5) 0.009(4) 0.013(4) 0.024(5) C117 0.057(6) 0.071(6) 0.058(6) 0.002(5) 0.028(5) 0.026(5) C118 0.061(6) 0.070(6) 0.052(5) 0.000(5) 0.025(5) 0.015(5) C119 0.039(5) 0.048(5) 0.039(4) 0.007(3) 0.008(3) 0.009(4) C120 0.024(4) 0.033(4) 0.026(3) -0.003(3) -0.005(3) 0.001(3) N121 0.053(5) 0.063(5) 0.057(4) -0.002(4) -0.016(4) 0.009(4) C121 0.047(6) 0.053(5) 0.075(6) -0.008(5) -0.013(5) 0.015(5) C122 0.149(10) 0.043(5) 0.233(13) 0.025(7) -0.126(9) -0.021(6) C123 0.160(10) 0.051(5) 0.246(12) 0.039(7) -0.124(9) -0.023(6) C124 0.162(11) 0.063(7) 0.236(13) 0.049(8) -0.127(9) -0.020(7) C125 0.077(9) 0.068(7) 0.115(10) 0.011(7) -0.029(8) 0.010(7) N122 0.040(4) 0.063(5) 0.042(4) 0.000(3) -0.002(3) 0.015(4) C126 0.049(5) 0.059(5) 0.040(4) 0.001(4) -0.002(4) 0.003(5) C127 0.088(8) 0.057(6) 0.035(4) -0.002(4) 0.005(5) 0.023(5) C128 0.057(6) 0.091(8) 0.056(5) 0.001(6) -0.005(5) 0.040(7) C129 0.039(6) 0.098(9) 0.073(7) -0.008(6) -0.004(5) 0.007(6) C130 0.043(5) 0.059(6) 0.071(6) -0.013(5) 0.002(5) 0.010(5) N123 0.059(5) 0.046(4) 0.074(5) 0.010(4) 0.010(4) 0.001(4) C131 0.062(7) 0.048(5) 0.067(6) 0.001(4) 0.014(5) 0.009(5) C132 0.061(7) 0.050(6) 0.072(6) 0.016(5) 0.000(5) 0.002(5) C133 0.094(10) 0.051(6) 0.102(9) 0.017(6) -0.002(8) -0.006(6) C134 0.066(8) 0.087(9) 0.133(11) 0.045(8) -0.006(8) -0.014(7) C135 0.047(6) 0.077(8) 0.109(9) 0.037(7) 0.000(6) 0.009(6) N124 0.057(10) 0.057(9) 0.050(8) -0.007(7) -0.002(7) -0.025(8) C136 0.053(13) 0.069(13) 0.095(16) 0.023(12) 0.018(12) -0.014(11) C137 0.09(2) 0.14(2) 0.064(14) 0.013(15) 0.029(13) -0.032(19) C138 0.045(13) 0.11(2) 0.101(18) 0.003(15) 0.023(12) -0.026(14) C139 0.15(3) 0.12(2) 0.064(15) 0.000(14) 0.041(17) 0.02(2) C140 0.069(16) 0.054(12) 0.14(2) -0.003(13) 0.058(15) -0.025(12) N125 0.083(7) 0.058(5) 0.057(5) 0.011(4) 0.016(5) 0.013(5) C141 0.140(13) 0.056(6) 0.070(7) 0.027(5) 0.039(8) 0.031(8) C142 0.105(12) 0.115(12) 0.111(10) 0.034(9) 0.058(9) 0.030(10) C143 0.145(15) 0.091(10) 0.092(9) 0.004(8) 0.038(9) 0.064(10) C144 0.179(17) 0.052(7) 0.095(9) 0.013(6) 0.039(10) 0.032(9) C145 0.078(9) 0.065(7) 0.082(8) 0.000(6) 0.017(6) -0.006(6) N126 0.116(5) 0.063(3) 0.069(3) -0.011(3) 0.027(3) -0.023(4) C146 0.116(5) 0.063(3) 0.069(3) -0.011(3) 0.027(3) -0.023(4) C147 0.116(5) 0.063(3) 0.069(3) -0.011(3) 0.027(3) -0.023(4) C148 0.116(5) 0.063(3) 0.069(3) -0.011(3) 0.027(3) -0.023(4) C149 0.116(5) 0.063(3) 0.069(3) -0.011(3) 0.027(3) -0.023(4) C150 0.116(5) 0.063(3) 0.069(3) -0.011(3) 0.027(3) -0.023(4) C48B 0.116(5) 0.063(3) 0.069(3) -0.011(3) 0.027(3) -0.023(4) C49B 0.116(5) 0.063(3) 0.069(3) -0.011(3) 0.027(3) -0.023(4) C50B 0.116(5) 0.063(3) 0.069(3) -0.011(3) 0.027(3) -0.023(4) N127 0.113(9) 0.096(7) 0.049(5) 0.020(5) -0.019(5) -0.053(7) C151 0.107(10) 0.046(6) 0.068(7) -0.024(5) 0.011(7) -0.011(6) C152 0.117(11) 0.040(5) 0.073(7) 0.000(5) 0.020(7) -0.018(7) C153 0.044(13) 0.09(2) 0.059(15) -0.020(13) 0.006(11) -0.014(13) C154 0.047(12) 0.091(17) 0.084(15) 0.006(14) 0.000(10) 0.020(12) C155 0.069(13) 0.067(12) 0.044(9) -0.018(8) -0.022(9) -0.005(11) C53B 0.08(2) 0.07(2) 0.11(3) -0.05(2) 0.05(2) -0.032(19) C54B 0.050(14) 0.024(10) 0.077(16) -0.004(10) 0.005(12) -0.010(10) C55B 0.058(15) 0.052(14) 0.046(12) 0.013(10) -0.015(11) 0.001(12) N128 0.116(6) 0.097(4) 0.211(9) -0.032(5) -0.069(6) -0.008(5) C156 0.116(6) 0.097(4) 0.211(9) -0.032(5) -0.069(6) -0.008(5) C157 0.116(6) 0.097(4) 0.211(9) -0.032(5) -0.069(6) -0.008(5) C158 0.116(6) 0.097(4) 0.211(9) -0.032(5) -0.069(6) -0.008(5) C159 0.116(6) 0.097(4) 0.211(9) -0.032(5) -0.069(6) -0.008(5) C160 0.116(6) 0.097(4) 0.211(9) -0.032(5) -0.069(6) -0.008(5) N129 0.140(11) 0.066(6) 0.089(7) -0.005(5) 0.007(7) -0.010(7) C161 0.116(12) 0.101(10) 0.065(7) -0.007(7) 0.030(7) -0.049(9) C162 0.101(12) 0.099(10) 0.104(10) 0.002(8) 0.031(9) -0.016(9) C163 0.081(10) 0.105(11) 0.128(12) 0.017(9) 0.026(9) -0.005(9) C164 0.088(10) 0.088(9) 0.087(9) 0.012(7) 0.040(8) 0.035(8) C165 0.097(10) 0.070(7) 0.073(7) 0.012(6) 0.034(7) 0.029(7) N130 0.286(11) 0.096(5) 0.180(8) 0.004(5) -0.096(8) 0.037(6) C166 0.286(11) 0.096(5) 0.180(8) 0.004(5) -0.096(8) 0.037(6) C167 0.286(11) 0.096(5) 0.180(8) 0.004(5) -0.096(8) 0.037(6) C168 0.286(11) 0.096(5) 0.180(8) 0.004(5) -0.096(8) 0.037(6) C169 0.286(11) 0.096(5) 0.180(8) 0.004(5) -0.096(8) 0.037(6) C170 0.286(11) 0.096(5) 0.180(8) 0.004(5) -0.096(8) 0.037(6) N131 0.038(11) 0.13(2) 0.114(18) 0.024(15) -0.023(11) 0.025(12) C171 0.12(2) 0.12(2) 0.040(11) 0.023(12) -0.033(13) -0.09(2) C172 0.23(4) 0.026(11) 0.082(18) -0.009(10) 0.02(2) 0.042(18) C173 0.044(14) 0.10(2) 0.13(2) 0.061(19) 0.022(14) 0.047(14) C174 0.078(18) 0.13(2) 0.062(14) 0.033(14) -0.019(13) -0.060(17) C175 0.16(3) 0.035(10) 0.073(15) -0.020(10) -0.032(17) 0.048(15) N132 0.099(9) 0.083(7) 0.104(8) -0.013(6) 0.028(7) -0.017(7) C176 0.110(11) 0.092(9) 0.062(7) -0.004(6) 0.012(7) -0.038(8) C177 0.062(8) 0.206(17) 0.073(8) -0.013(9) 0.020(7) -0.055(10) C178 0.084(10) 0.151(14) 0.072(8) -0.016(8) -0.013(7) -0.028(10) C179 0.054(7) 0.084(8) 0.109(10) -0.012(7) -0.015(7) -0.002(7) C180 0.061(7) 0.065(7) 0.078(7) 0.000(6) -0.007(6) -0.008(6) N133 0.20(5) 0.07(2) 0.79(13) 0.02(4) -0.06(7) -0.09(3) C181 0.30(5) 0.033(11) 0.063(14) -0.014(10) 0.05(2) 0.000(19) C182 0.133(13) 0.092(12) 0.113(12) 0.011(9) 0.009(9) 0.016(9) C183 0.27(5) 0.054(14) 0.10(2) 0.006(14) 0.09(3) 0.07(2) C184 0.21(4) 0.10(2) 0.071(17) -0.038(16) -0.01(2) 0.07(3) C185 0.16(4) 0.07(2) 0.24(5) 0.01(3) 0.07(4) -0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.376(4) . ? Nd1 O22 2.388(5) . ? Nd1 N2 2.428(6) . ? Nd1 N21 2.440(5) . ? Nd1 O21 2.494(4) . ? Nd1 O2 2.522(4) . ? Nd1 N22 2.606(6) . ? Nd1 N1 2.612(5) . ? Nd1 K7 4.1091(16) 1_454 ? Nd1 K1 4.1163(16) . ? Nd1 K2 4.5440(16) . ? Nd2 O62 2.367(5) . ? Nd2 O41 2.423(5) . ? Nd2 N61 2.426(6) . ? Nd2 O42 2.440(4) . ? Nd2 O61 2.461(4) . ? Nd2 N42 2.461(6) . ? Nd2 N62 2.670(5) . ? Nd2 N41 2.724(6) . ? Nd2 K3 3.6593(16) . ? Nd2 K4 3.9976(15) . ? Nd2 K1 4.1666(15) . ? Nd2 K5 4.4751(17) . ? Nd3 O102 2.334(4) . ? Nd3 O81 2.351(4) . ? Nd3 N82 2.463(6) . ? Nd3 N101 2.488(6) . ? Nd3 O101 2.503(4) . ? Nd3 O82 2.514(4) . ? Nd3 N102 2.608(6) . ? Nd3 N81 2.621(5) . ? Nd3 K7 4.1627(16) . ? Nd3 K9B 4.168(9) . ? Nd3 K4 4.1737(15) . ? K1 O22 2.673(5) . ? K1 O41 2.676(5) . ? K1 O2 2.683(5) . ? K1 O61 2.857(4) . ? K1 N121 2.990(8) . ? K1 C40 3.256(6) . ? K1 C20 3.472(9) . ? K1 C19 3.489(8) . ? K1 C41 3.509(8) . ? K1 K2 3.945(2) . ? K1 K3 4.100(2) . ? K2 O2 2.711(5) . ? K2 C20 3.050(7) . ? K2 C61 3.125(7) . ? K2 C9 3.168(7) . ? K2 C62 3.174(7) . ? K2 C70 3.180(9) . ? K2 C8 3.194(7) . ? K2 C69 3.200(7) . ? K2 C71 3.216(10) . ? K2 C10 3.244(8) . ? K2 C72 3.264(9) . ? K2 O61 3.288(5) . ? K3 O61 2.764(5) . ? K3 N122 2.864(7) . ? K3 N123 2.875(7) . ? K3 N41 3.011(6) . ? K3 N42 3.040(6) . ? K3 C61 3.063(7) . ? K3 O41 3.185(6) . ? K3 C53 3.431(7) . ? K3 C48 3.437(8) . ? K3 C62 3.455(7) . ? K3 C39 3.510(7) . ? K4 O42 2.652(5) . ? K4 O81 2.653(4) . ? K4 O62 2.713(5) . ? K4 O101 2.736(4) . ? K4 N124 2.769(7) . ? K4 C81 3.168(7) . ? K4 C80 3.391(8) . ? K4 C60 3.447(7) . ? K4 C59 3.480(8) . ? K4 K5 3.943(2) . ? K5 O42 2.692(5) . ? K5 O101 2.886(4) . ? K5 C60 2.978(7) . ? K5 C101 3.046(6) . ? K5 C48 3.137(7) . ? K5 C111 3.138(8) . ? K5 C59 3.144(8) . ? K5 C110 3.149(8) . ? K5 C112 3.199(7) . ? K5 C109 3.212(7) . ? K5 C49 3.251(9) . ? K5 C102 3.253(7) . ? K6 N127 2.817(10) . ? K6 N125 2.882(9) . ? K6 N126 2.895(9) . ? K6 N82 2.920(6) . ? K6 C101 3.091(6) . ? K6 C106 3.128(7) . ? K6 C102 3.195(7) . ? K6 C105 3.199(7) . ? K6 C93 3.246(6) . ? K6 C104 3.307(7) . ? K6 C103 3.322(7) . ? K6 C94 3.491(6) . ? K7 O21 2.620(5) 1_656 ? K7 O102 2.658(4) . ? K7 O1 2.705(5) 1_656 ? K7 N128 2.705(7) . ? K7 O82 2.732(5) . ? K7 C120 3.264(7) . ? K7 C1 3.339(7) 1_656 ? K7 C21 3.416(7) 1_656 ? K7 C22 3.438(8) 1_656 ? K7 C156 3.460(8) . ? K7 C99 3.507(8) . ? K7 C100 3.528(7) . ? K8 O82 2.810(5) . ? K8 O21 2.820(5) 1_656 ? K8 C21 2.950(7) 1_656 ? K8 C100 2.976(7) . ? K8 C22 3.111(7) 1_656 ? K8 C32 3.181(8) 1_656 ? K8 C31 3.213(8) 1_656 ? K8 C99 3.216(8) . ? K8 C29 3.218(8) 1_656 ? K8 C33 3.221(7) 1_656 ? K8 C30 3.223(8) 1_656 ? K8 C89 3.227(7) . ? K9 N129 2.696(13) . ? K9 N130 2.776(6) . ? K9 N101 2.843(5) . ? K9 C95 3.108(6) . ? K9 C100 3.129(7) . ? K9 C108 3.132(7) . ? K9 C96 3.231(8) . ? K9 C99 3.285(7) . ? K9 C107 3.323(7) . ? K9 C97 3.365(8) . ? K9 C98 3.384(8) . ? K9 C161 3.478(14) . ? K9B N130 2.494(9) . ? K9B C100 2.956(8) . ? K9B N101 2.994(9) . ? K9B C99 3.062(8) . ? K9B C166 3.075(8) . ? K9B O82 3.104(10) . ? K9B C108 3.256(9) . ? K9B N102 3.389(10) . ? K9B C113 3.419(9) . ? O1 C1 1.305(8) . ? O1 K7 2.705(5) 1_454 ? O2 C20 1.344(8) . ? N1 C7 1.288(9) . ? N1 C8 1.435(9) . ? N2 C13 1.353(8) . ? N2 C14 1.448(8) . ? C1 C2 1.406(11) . ? C1 C6 1.414(10) . ? C1 K7 3.339(7) 1_454 ? C2 C3 1.380(11) . ? C3 C4 1.400(12) . ? C4 C5 1.385(11) . ? C5 C6 1.399(10) . ? C6 C7 1.439(10) . ? C8 C9 1.380(9) . ? C8 C13 1.448(9) . ? C9 C10 1.408(10) . ? C10 C11 1.375(11) . ? C11 C12 1.389(10) . ? C12 C13 1.420(9) . ? C14 C15 1.512(9) . ? C14 C27 1.564(10) . ? C15 C16 1.386(10) . ? C15 C20 1.440(11) . ? C16 C17 1.377(11) . ? C17 C18 1.400(12) . ? C18 C19 1.371(11) . ? C19 C20 1.403(10) . ? O21 C21 1.345(8) . ? O21 K7 2.620(5) 1_454 ? O21 K8 2.820(5) 1_454 ? O22 C40 1.328(8) . ? N21 C28 1.349(9) . ? N21 C27 1.459(9) . ? N22 C34 1.303(10) . ? N22 C33 1.424(9) . ? C21 C22 1.394(9) . ? C21 C26 1.418(9) . ? C21 K8 2.950(7) 1_454 ? C21 K7 3.416(7) 1_454 ? C22 C23 1.386(10) . ? C22 K8 3.111(7) 1_454 ? C22 K7 3.438(8) 1_454 ? C23 C24 1.356(11) . ? C24 C25 1.407(11) . ? C25 C26 1.395(10) . ? C26 C27 1.530(9) . ? C28 C29 1.436(10) . ? C28 C33 1.436(11) . ? C28 K8 3.254(7) 1_454 ? C29 C30 1.374(11) . ? C29 K8 3.218(8) 1_454 ? C30 C31 1.391(12) . ? C30 K8 3.223(8) 1_454 ? C31 C32 1.377(10) . ? C31 K8 3.213(8) 1_454 ? C32 C33 1.380(10) . ? C32 K8 3.181(8) 1_454 ? C33 K8 3.221(7) 1_454 ? C34 C35 1.437(10) . ? C35 C36 1.394(9) . ? C35 C40 1.413(9) . ? C36 C37 1.358(12) . ? C37 C38 1.390(11) . ? C38 C39 1.386(11) . ? C39 C40 1.409(10) . ? O41 C41 1.318(9) . ? O42 C60 1.335(8) . ? N41 C47 1.263(9) . ? N41 C48 1.413(10) . ? N42 C53 1.374(9) . ? N42 C54 1.459(9) . ? C41 C46 1.403(11) . ? C41 C42 1.421(12) . ? C42 C43 1.377(13) . ? C43 C44 1.445(14) . ? C44 C45 1.325(12) . ? C45 C46 1.427(11) . ? C46 C47 1.442(11) . ? C48 C49 1.413(11) . ? C48 C53 1.421(11) . ? C49 C50 1.359(13) . ? C50 C51 1.352(13) . ? C51 C52 1.380(12) . ? C52 C53 1.444(11) . ? C54 C55 1.535(9) . ? C54 C67 1.540(9) . ? C55 C56 1.398(9) . ? C55 C60 1.428(9) . ? C56 C57 1.408(10) . ? C57 C58 1.380(11) . ? C58 C59 1.385(10) . ? C59 C60 1.394(9) . ? O61 C61 1.322(7) . ? O62 C80 1.305(9) . ? N61 C68 1.345(9) . ? N61 C67 1.423(8) . ? N62 C74 1.284(10) . ? N62 C73 1.455(9) . ? C61 C66 1.415(9) . ? C61 C62 1.430(9) . ? C62 C63 1.394(10) . ? C63 C64 1.385(10) . ? C64 C65 1.376(9) . ? C65 C66 1.387(9) . ? C66 C67 1.542(8) . ? C68 C73 1.425(10) . ? C68 C69 1.443(10) . ? C69 C70 1.355(11) . ? C70 C71 1.370(13) . ? C71 C72 1.375(12) . ? C72 C73 1.397(11) . ? C74 C75 1.466(13) . ? C75 C76 1.416(12) . ? C75 C80 1.428(13) . ? C76 C77 1.398(15) . ? C77 C78 1.396(17) . ? C78 C79 1.351(12) . ? C79 C80 1.426(11) . ? O81 C81 1.320(8) . ? O82 C100 1.295(8) . ? N81 C87 1.305(9) . ? N81 C88 1.418(9) . ? N82 C93 1.361(8) . ? N82 C94 1.452(8) . ? C81 C82 1.388(10) . ? C81 C86 1.419(10) . ? C82 C83 1.359(11) . ? C83 C84 1.372(13) . ? C84 C85 1.368(12) . ? C85 C86 1.407(11) . ? C86 C87 1.444(10) . ? C88 C89 1.376(9) . ? C88 C93 1.435(10) . ? C89 C90 1.390(11) . ? C90 C91 1.386(11) . ? C91 C92 1.397(10) . ? C92 C93 1.410(9) . ? C94 C107 1.544(9) . ? C94 C95 1.545(9) . ? C95 C100 1.397(10) . ? C95 C96 1.411(11) . ? C96 C97 1.370(11) . ? C97 C98 1.351(12) . ? C98 C99 1.389(11) . ? C99 C100 1.431(9) . ? O101 C101 1.328(8) . ? O102 C120 1.309(8) . ? N101 C108 1.362(8) . ? N101 C107 1.443(9) . ? N102 C114 1.272(9) . ? N102 C113 1.437(9) . ? C101 C106 1.417(9) . ? C101 C102 1.428(9) . ? C102 C103 1.358(10) . ? C103 C104 1.368(11) . ? C104 C105 1.411(10) . ? C105 C106 1.397(10) . ? C106 C107 1.518(9) . ? C108 C109 1.398(10) . ? C108 C113 1.429(9) . ? C109 C110 1.405(10) . ? C110 C111 1.353(11) . ? C111 C112 1.396(10) . ? C112 C113 1.391(9) . ? C114 C115 1.462(10) . ? C115 C116 1.399(10) . ? C115 C120 1.446(9) . ? C116 C117 1.379(12) . ? C117 C118 1.392(13) . ? C118 C119 1.373(12) . ? C119 C120 1.420(10) . ? N121 C121 1.326(11) . ? N121 C125 1.333(12) . ? C121 C122 1.323(14) . ? C122 C123 1.319(16) . ? C123 C124 1.372(18) . ? C124 C125 1.332(17) . ? N122 C130 1.340(11) . ? N122 C126 1.343(11) . ? C126 C127 1.387(12) . ? C127 C128 1.344(14) . ? C128 C129 1.345(14) . ? C129 C130 1.363(13) . ? N123 C135 1.316(10) . ? N123 C131 1.317(12) . ? C131 C132 1.351(12) . ? C132 C133 1.364(15) . ? C133 C134 1.397(16) . ? C134 C135 1.347(13) . ? N124 C136 1.3900 . ? N124 C140 1.3900 . ? C136 C137 1.3900 . ? C137 C138 1.3900 . ? C138 C139 1.3900 . ? C139 C140 1.3900 . ? N125 C145 1.307(12) . ? N125 C141 1.343(15) . ? C141 C142 1.374(17) . ? C142 C143 1.383(19) . ? C143 C144 1.42(2) . ? C144 C145 1.321(16) . ? N126 C146 1.257(13) . ? N126 C150 1.35(3) . ? N126 C50B 1.41(2) . ? C146 C147 1.370(14) . ? C147 C148 1.26(3) . ? C147 C48B 1.37(2) . ? C148 C149 1.37(3) . ? C149 C150 1.36(3) . ? C48B C49B 1.42(3) . ? C49B C50B 1.31(3) . ? N127 C55B 1.200(10) . ? N127 C151 1.316(13) . ? N127 C155 1.55(2) . ? C151 C152 1.394(15) . ? C152 C53B 1.31(5) . ? C152 C153 1.41(3) . ? C153 C154 1.40(4) . ? C154 C155 1.37(3) . ? C53B C54B 1.27(6) . ? C54B C55B 1.34(2) . ? N128 C156 1.3900 . ? N128 C160 1.3901 . ? C156 C157 1.3900 . ? C157 C158 1.3900 . ? C158 C159 1.3900 . ? C159 C160 1.3900 . ? N129 C161 1.289(14) . ? N129 C165 1.412(13) . ? C161 C162 1.408(18) . ? C162 C163 1.385(18) . ? C163 C164 1.356(18) . ? C164 C165 1.372(15) . ? N130 C170 1.3900 . ? N130 C166 1.3900 . ? C166 C167 1.3900 . ? C167 C168 1.3900 . ? C168 C169 1.3900 . ? C169 C170 1.3900 . ? N131 C175 1.24(3) . ? N131 C171 1.28(3) . ? C171 C172 1.37(4) . ? C172 C173 1.20(4) . ? C173 C174 1.27(4) . ? C174 C175 1.25(3) . ? N132 C180 1.301(12) . ? N132 C176 1.334(14) . ? C176 C177 1.310(15) . ? C177 C178 1.321(17) . ? C178 C179 1.357(17) . ? C179 C180 1.358(15) . ? N133 C181 1.3900 . ? N133 C185 1.3900 . ? C181 C182 1.3900 . ? C182 C183 1.3900 . ? C183 C184 1.3900 . ? C184 C185 1.3900 . ? 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 Nd1 O22 78.44(16) . . ? O1 Nd1 N2 122.76(18) . . ? O22 Nd1 N2 135.29(16) . . ? O1 Nd1 N21 135.45(18) . . ? O22 Nd1 N21 121.62(18) . . ? N2 Nd1 N21 73.1(2) . . ? O1 Nd1 O21 74.02(16) . . ? O22 Nd1 O21 145.35(15) . . ? N2 Nd1 O21 78.35(17) . . ? N21 Nd1 O21 69.15(17) . . ? O1 Nd1 O2 145.08(15) . . ? O22 Nd1 O2 73.48(15) . . ? N2 Nd1 O2 68.95(16) . . ? N21 Nd1 O2 78.13(17) . . ? O21 Nd1 O2 139.09(15) . . ? O1 Nd1 N22 90.29(18) . . ? O22 Nd1 N22 70.77(17) . . ? N2 Nd1 N22 138.14(19) . . ? N21 Nd1 N22 65.1(2) . . ? O21 Nd1 N22 88.60(17) . . ? O2 Nd1 N22 99.48(17) . . ? O1 Nd1 N1 71.33(17) . . ? O22 Nd1 N1 91.51(18) . . ? N2 Nd1 N1 64.88(19) . . ? N21 Nd1 N1 137.9(2) . . ? O21 Nd1 N1 99.07(17) . . ? O2 Nd1 N1 88.91(16) . . ? N22 Nd1 N1 157.0(2) . . ? O1 Nd1 K7 38.83(13) . 1_454 ? O22 Nd1 K7 117.13(11) . 1_454 ? N2 Nd1 K7 93.86(13) . 1_454 ? N21 Nd1 K7 106.35(14) . 1_454 ? O21 Nd1 K7 37.58(11) . 1_454 ? O2 Nd1 K7 160.53(11) . 1_454 ? N22 Nd1 K7 99.53(13) . 1_454 ? N1 Nd1 K7 75.05(13) . 1_454 ? O1 Nd1 K1 116.39(13) . . ? O22 Nd1 K1 37.95(11) . . ? N2 Nd1 K1 107.96(12) . . ? N21 Nd1 K1 91.94(14) . . ? O21 Nd1 K1 157.83(11) . . ? O2 Nd1 K1 39.12(11) . . ? N22 Nd1 K1 72.46(13) . . ? N1 Nd1 K1 102.83(13) . . ? K7 Nd1 K1 154.98(4) 1_454 . ? O1 Nd1 K2 119.83(11) . . ? O22 Nd1 K2 72.54(10) . . ? N2 Nd1 K2 62.76(12) . . ? N21 Nd1 K2 104.54(14) . . ? O21 Nd1 K2 140.29(12) . . ? O2 Nd1 K2 30.95(11) . . ? N22 Nd1 K2 125.49(13) . . ? N1 Nd1 K2 58.34(12) . . ? K7 Nd1 K2 133.03(3) 1_454 . ? K1 Nd1 K2 53.92(3) . . ? O62 Nd2 O41 81.07(18) . . ? O62 Nd2 N61 122.62(19) . . ? O41 Nd2 N61 138.29(17) . . ? O62 Nd2 O42 77.72(15) . . ? O41 Nd2 O42 143.79(16) . . ? N61 Nd2 O42 77.85(17) . . ? O62 Nd2 O61 138.63(15) . . ? O41 Nd2 O61 71.17(15) . . ? N61 Nd2 O61 69.20(17) . . ? O42 Nd2 O61 140.64(14) . . ? O62 Nd2 N42 140.46(18) . . ? O41 Nd2 N42 112.08(19) . . ? N61 Nd2 N42 72.9(2) . . ? O42 Nd2 N42 70.34(16) . . ? O61 Nd2 N42 79.68(17) . . ? O62 Nd2 N62 69.31(17) . . ? O41 Nd2 N62 101.32(19) . . ? N61 Nd2 N62 63.99(17) . . ? O42 Nd2 N62 98.18(17) . . ? O61 Nd2 N62 86.44(17) . . ? N42 Nd2 N62 136.89(18) . . ? O62 Nd2 N41 93.34(18) . . ? O41 Nd2 N41 66.79(19) . . ? N61 Nd2 N41 134.93(19) . . ? O42 Nd2 N41 85.44(17) . . ? O61 Nd2 N41 102.73(16) . . ? N42 Nd2 N41 62.04(19) . . ? N62 Nd2 N41 160.84(17) . . ? O62 Nd2 K3 134.98(13) . . ? O41 Nd2 K3 59.06(14) . . ? N61 Nd2 K3 101.83(13) . . ? O42 Nd2 K3 122.27(11) . . ? O61 Nd2 K3 49.05(12) . . ? N42 Nd2 K3 55.49(13) . . ? N62 Nd2 K3 134.20(13) . . ? N41 Nd2 K3 53.90(12) . . ? O62 Nd2 K4 41.27(12) . . ? O41 Nd2 K4 121.79(13) . . ? N61 Nd2 K4 91.20(13) . . ? O42 Nd2 K4 40.21(11) . . ? O61 Nd2 K4 154.75(12) . . ? N42 Nd2 K4 110.51(13) . . ? N62 Nd2 K4 70.26(13) . . ? N41 Nd2 K4 102.42(12) . . ? K3 Nd2 K4 155.45(4) . . ? O62 Nd2 K1 98.57(12) . . ? O41 Nd2 K1 37.25(12) . . ? N61 Nd2 K1 101.64(14) . . ? O42 Nd2 K1 174.94(11) . . ? O61 Nd2 K1 41.93(10) . . ? N42 Nd2 K1 114.42(13) . . ? N62 Nd2 K1 77.20(13) . . ? N41 Nd2 K1 98.27(13) . . ? K3 Nd2 K1 62.79(4) . . ? K4 Nd2 K1 135.07(3) . . ? O62 Nd2 K5 76.20(12) . . ? O41 Nd2 K5 115.10(12) . . ? N61 Nd2 K5 104.42(14) . . ? O42 Nd2 K5 30.93(11) . . ? O61 Nd2 K5 143.42(11) . . ? N42 Nd2 K5 64.39(14) . . ? N62 Nd2 K5 124.31(13) . . ? N41 Nd2 K5 55.15(13) . . ? K3 Nd2 K5 101.08(4) . . ? K4 Nd2 K5 55.12(3) . . ? K1 Nd2 K5 151.82(3) . . ? O102 Nd3 O81 78.86(15) . . ? O102 Nd3 N82 136.17(17) . . ? O81 Nd3 N82 121.19(18) . . ? O102 Nd3 N101 121.01(17) . . ? O81 Nd3 N101 137.45(16) . . ? N82 Nd3 N101 72.52(18) . . ? O102 Nd3 O101 143.03(15) . . ? O81 Nd3 O101 74.54(14) . . ? N82 Nd3 O101 80.29(16) . . ? N101 Nd3 O101 68.36(15) . . ? O102 Nd3 O82 73.97(15) . . ? O81 Nd3 O82 145.18(14) . . ? N82 Nd3 O82 69.41(17) . . ? N101 Nd3 O82 76.41(16) . . ? O101 Nd3 O82 139.00(14) . . ? O102 Nd3 N102 71.22(17) . . ? O81 Nd3 N102 92.42(18) . . ? N82 Nd3 N102 137.08(19) . . ? N101 Nd3 N102 64.56(18) . . ? O101 Nd3 N102 84.63(16) . . ? O82 Nd3 N102 98.92(16) . . ? O102 Nd3 N81 92.43(17) . . ? O81 Nd3 N81 70.80(18) . . ? N82 Nd3 N81 64.05(19) . . ? N101 Nd3 N81 136.56(18) . . ? O101 Nd3 N81 102.35(16) . . ? O82 Nd3 N81 88.86(16) . . ? N102 Nd3 N81 158.88(19) . . ? O102 Nd3 K7 36.06(11) . . ? O81 Nd3 K7 114.52(11) . . ? N82 Nd3 K7 108.00(13) . . ? N101 Nd3 K7 94.97(12) . . ? O101 Nd3 K7 158.76(11) . . ? O82 Nd3 K7 39.36(11) . . ? N102 Nd3 K7 76.05(12) . . ? N81 Nd3 K7 98.83(12) . . ? O102 Nd3 K9B 77.61(16) . . ? O81 Nd3 K9B 144.06(19) . . ? N82 Nd3 K9B 94.5(2) . . ? N101 Nd3 K9B 45.26(16) . . ? O101 Nd3 K9B 110.76(14) . . ? O82 Nd3 K9B 47.89(16) . . ? N102 Nd3 K9B 54.29(13) . . ? N81 Nd3 K9B 136.74(17) . . ? K7 Nd3 K9B 50.22(15) . . ? O102 Nd3 K4 112.92(11) . . ? O81 Nd3 K4 35.85(10) . . ? N82 Nd3 K4 99.92(13) . . ? N101 Nd3 K4 106.47(12) . . ? O101 Nd3 K4 39.16(10) . . ? O82 Nd3 K4 167.89(11) . . ? N102 Nd3 K4 92.85(12) . . ? N81 Nd3 K4 81.05(12) . . ? K7 Nd3 K4 148.89(4) . . ? K9B Nd3 K4 141.70(12) . . ? O22 K1 O41 131.03(17) . . ? O22 K1 O2 66.57(14) . . ? O41 K1 O2 151.11(15) . . ? O22 K1 O61 95.59(13) . . ? O41 K1 O61 61.72(15) . . ? O2 K1 O61 97.43(15) . . ? O22 K1 N121 118.30(13) . . ? O41 K1 N121 99.39(14) . . ? O2 K1 N121 86.35(16) . . ? O61 K1 N121 144.03(14) . . ? O22 K1 C40 23.33(15) . . ? O41 K1 C40 112.68(18) . . ? O2 K1 C40 89.10(16) . . ? O61 K1 C40 99.19(16) . . ? N121 K1 C40 116.66(14) . . ? O22 K1 C20 86.26(15) . . ? O41 K1 C20 138.04(16) . . ? O2 K1 C20 20.53(14) . . ? O61 K1 C20 101.98(16) . . ? N121 K1 C20 70.79(17) . . ? C40 K1 C20 107.86(17) . . ? O22 K1 C19 109.39(17) . . ? O41 K1 C19 115.63(18) . . ? O2 K1 C19 42.95(15) . . ? O61 K1 C19 96.75(17) . . ? N121 K1 C19 62.34(17) . . ? C40 K1 C19 131.08(18) . . ? C20 K1 C19 23.26(16) . . ? O22 K1 C41 130.53(18) . . ? O41 K1 C41 19.18(15) . . ? O2 K1 C41 162.82(17) . . ? O61 K1 C41 80.54(16) . . ? N121 K1 C41 85.57(15) . . ? C40 K1 C41 108.08(19) . . ? C20 K1 C41 143.03(18) . . ? C19 K1 C41 120.06(19) . . ? O22 K1 K2 82.19(11) . . ? O41 K1 K2 110.51(11) . . ? O2 K1 K2 43.29(10) . . ? O61 K1 K2 55.06(10) . . ? N121 K1 K2 114.76(17) . . ? C40 K1 K2 103.15(13) . . ? C20 K1 K2 48.06(12) . . ? C19 K1 K2 52.54(13) . . ? C41 K1 K2 128.95(13) . . ? O22 K1 K3 82.43(11) . . ? O41 K1 K3 50.95(13) . . ? O2 K1 K3 127.00(11) . . ? O61 K1 K3 42.29(10) . . ? N121 K1 K3 146.56(16) . . ? C40 K1 K3 71.50(13) . . ? C20 K1 K3 140.42(13) . . ? C19 K1 K3 138.98(15) . . ? C41 K1 K3 61.70(15) . . ? K2 K1 K3 92.73(5) . . ? O22 K1 Nd1 33.34(10) . . ? O41 K1 Nd1 163.71(14) . . ? O2 K1 Nd1 36.39(9) . . ? O61 K1 Nd1 108.74(10) . . ? N121 K1 Nd1 95.44(14) . . ? C40 K1 Nd1 53.72(12) . . ? C20 K1 Nd1 54.14(11) . . ? C19 K1 Nd1 77.36(13) . . ? C41 K1 Nd1 159.95(13) . . ? K2 K1 Nd1 68.59(4) . . ? K3 K1 Nd1 112.88(4) . . ? O2 K2 C20 26.13(16) . . ? O2 K2 C61 101.53(16) . . ? C20 K2 C61 121.9(2) . . ? O2 K2 C9 98.52(16) . . ? C20 K2 C9 106.7(2) . . ? C61 K2 C9 103.08(19) . . ? O2 K2 C62 90.15(17) . . ? C20 K2 C62 115.6(2) . . ? C61 K2 C62 26.23(16) . . ? C9 K2 C62 81.59(19) . . ? O2 K2 C70 151.93(19) . . ? C20 K2 C70 126.2(2) . . ? C61 K2 C70 96.9(2) . . ? C9 K2 C70 97.7(2) . . ? C62 K2 C70 114.8(2) . . ? O2 K2 C8 73.49(16) . . ? C20 K2 C8 83.49(18) . . ? C61 K2 C8 108.91(17) . . ? C9 K2 C8 25.06(17) . . ? C62 K2 C8 83.07(17) . . ? C70 K2 C8 120.0(2) . . ? O2 K2 C69 155.81(17) . . ? C20 K2 C69 139.48(19) . . ? C61 K2 C69 72.50(18) . . ? C9 K2 C69 105.66(19) . . ? C62 K2 C69 92.59(19) . . ? C70 K2 C69 24.5(2) . . ? C8 K2 C69 130.70(18) . . ? O2 K2 C71 127.2(2) . . ? C20 K2 C71 101.6(2) . . ? C61 K2 C71 113.1(2) . . ? C9 K2 C71 110.2(2) . . ? C62 K2 C71 136.1(2) . . ? C70 K2 C71 24.7(2) . . ? C8 K2 C71 125.4(2) . . ? C69 K2 C71 43.7(2) . . ? O2 K2 C10 112.80(18) . . ? C20 K2 C10 109.9(2) . . ? C61 K2 C10 117.89(19) . . ? C9 K2 C10 25.33(19) . . ? C62 K2 C10 102.2(2) . . ? C70 K2 C10 75.8(2) . . ? C8 K2 C10 44.17(18) . . ? C69 K2 C10 90.09(19) . . ? C71 K2 C10 85.1(2) . . ? O2 K2 C72 111.4(2) . . ? C20 K2 C72 89.4(2) . . ? C61 K2 C72 103.38(19) . . ? C9 K2 C72 134.5(2) . . ? C62 K2 C72 129.6(2) . . ? C70 K2 C72 42.9(2) . . ? C8 K2 C72 145.6(2) . . ? C69 K2 C72 50.2(2) . . ? C71 K2 C72 24.5(2) . . ? C10 K2 C72 109.3(2) . . ? O2 K2 O61 87.35(13) . . ? C20 K2 O61 102.12(18) . . ? C61 K2 O61 23.61(13) . . ? C9 K2 O61 124.30(17) . . ? C62 K2 O61 42.86(15) . . ? C70 K2 O61 102.04(18) . . ? C8 K2 O61 122.90(15) . . ? C69 K2 O61 78.51(15) . . ? C71 K2 O61 109.17(19) . . ? C10 K2 O61 141.47(18) . . ? C72 K2 O61 91.45(17) . . ? O61 K3 N122 148.63(15) . . ? O61 K3 N123 122.70(17) . . ? N122 K3 N123 85.3(2) . . ? O61 K3 N41 89.04(15) . . ? N122 K3 N41 76.20(13) . . ? N123 K3 N41 136.94(17) . . ? O61 K3 N42 65.61(15) . . ? N122 K3 N42 120.82(13) . . ? N123 K3 N42 111.12(16) . . ? N41 K3 N42 52.60(17) . . ? O61 K3 C61 25.56(14) . . ? N122 K3 C61 171.00(15) . . ? N123 K3 C61 97.90(17) . . ? N41 K3 C61 106.40(17) . . ? N42 K3 C61 65.92(17) . . ? O61 K3 O41 56.54(13) . . ? N122 K3 O41 92.84(15) . . ? N123 K3 O41 166.67(16) . . ? N41 K3 O41 54.56(15) . . ? N42 K3 O41 81.16(14) . . ? C61 K3 O41 82.10(15) . . ? O61 K3 C53 88.42(16) . . ? N122 K3 C53 98.45(14) . . ? N123 K3 C53 104.53(16) . . ? N41 K3 C53 42.77(18) . . ? N42 K3 C53 23.53(17) . . ? C61 K3 C53 88.92(18) . . ? O41 K3 C53 88.81(15) . . ? O61 K3 C48 99.87(16) . . ? N122 K3 C48 77.77(14) . . ? N123 K3 C48 114.22(17) . . ? N41 K3 C48 24.18(17) . . ? N42 K3 C48 43.24(18) . . ? C61 K3 C48 108.23(18) . . ? O41 K3 C48 78.12(16) . . ? C53 K3 C48 23.88(18) . . ? O61 K3 C62 42.90(14) . . ? N122 K3 C62 150.51(13) . . ? N123 K3 C62 81.13(17) . . ? N41 K3 C62 130.25(17) . . ? N42 K3 C62 88.56(17) . . ? C61 K3 C62 24.41(15) . . ? O41 K3 C62 94.41(15) . . ? C53 K3 C62 110.23(18) . . ? C48 K3 C62 131.71(18) . . ? O61 K3 C39 91.91(16) . . ? N122 K3 C39 84.08(14) . . ? N123 K3 C39 70.76(16) . . ? N41 K3 C39 142.68(19) . . ? N42 K3 C39 154.95(18) . . ? C61 K3 C39 89.03(18) . . ? O41 K3 C39 95.92(15) . . ? C53 K3 C39 174.54(19) . . ? C48 K3 C39 160.5(2) . . ? C62 K3 C39 66.77(18) . . ? O61 K3 Nd2 42.24(9) . . ? N122 K3 Nd2 119.15(13) . . ? N123 K3 Nd2 149.35(16) . . ? N41 K3 Nd2 46.97(12) . . ? N42 K3 Nd2 41.84(12) . . ? C61 K3 Nd2 60.96(12) . . ? O41 K3 Nd2 40.73(8) . . ? C53 K3 Nd2 56.72(12) . . ? C48 K3 Nd2 59.60(13) . . ? C62 K3 Nd2 83.67(11) . . ? C39 K3 Nd2 126.15(13) . . ? O42 K4 O81 119.38(16) . . ? O42 K4 O62 68.40(14) . . ? O81 K4 O62 166.82(16) . . ? O42 K4 O101 89.88(11) . . ? O81 K4 O101 66.14(12) . . ? O62 K4 O101 104.73(12) . . ? O42 K4 N124 121.72(15) . . ? O81 K4 N124 91.96(17) . . ? O62 K4 N124 92.14(13) . . ? O101 K4 N124 148.11(17) . . ? O42 K4 C81 130.70(17) . . ? O81 K4 C81 24.20(16) . . ? O62 K4 C81 157.30(18) . . ? O101 K4 C81 89.00(15) . . ? N124 K4 C81 67.80(18) . . ? O42 K4 C80 88.77(17) . . ? O81 K4 C80 151.30(19) . . ? O62 K4 C80 21.18(17) . . ? O101 K4 C80 111.85(18) . . ? N124 K4 C80 76.0(2) . . ? C81 K4 C80 136.4(2) . . ? O42 K4 C60 20.44(14) . . ? O81 K4 C60 100.95(17) . . ? O62 K4 C60 88.14(15) . . ? O101 K4 C60 89.82(13) . . ? N124 K4 C60 118.05(16) . . ? C81 K4 C60 110.27(18) . . ? C80 K4 C60 107.72(17) . . ? O42 K4 C59 42.52(15) . . ? O81 K4 C59 77.75(17) . . ? O62 K4 C59 110.91(16) . . ? O101 K4 C59 80.03(14) . . ? N124 K4 C59 119.28(16) . . ? C81 K4 C59 88.96(18) . . ? C80 K4 C59 130.90(18) . . ? C60 K4 C59 23.21(15) . . ? O42 K4 K5 42.85(11) . . ? O81 K4 K5 95.44(12) . . ? O62 K4 K5 83.74(12) . . ? O101 K4 K5 47.04(9) . . ? N124 K4 K5 164.36(16) . . ? C81 K4 K5 118.42(14) . . ? C80 K4 K5 102.96(17) . . ? C60 K4 K5 46.93(12) . . ? C59 K4 K5 49.63(14) . . ? O42 K4 Nd2 36.43(9) . . ? O81 K4 Nd2 155.22(13) . . ? O62 K4 Nd2 35.13(10) . . ? O101 K4 Nd2 109.83(8) . . ? N124 K4 Nd2 99.58(14) . . ? C81 K4 Nd2 154.10(15) . . ? C80 K4 Nd2 53.47(13) . . ? C60 K4 Nd2 54.28(11) . . ? C59 K4 Nd2 77.48(12) . . ? K5 K4 Nd2 68.60(3) . . ? O42 K4 Nd3 111.32(11) . . ? O81 K4 Nd3 31.26(10) . . ? O62 K4 Nd3 137.93(12) . . ? O101 K4 Nd3 35.29(8) . . ? N124 K4 Nd3 118.14(14) . . ? C81 K4 Nd3 53.73(13) . . ? C80 K4 Nd3 136.65(15) . . ? C60 K4 Nd3 100.57(12) . . ? C59 K4 Nd3 80.52(12) . . ? K5 K4 Nd3 73.57(4) . . ? Nd2 K4 Nd3 142.06(4) . . ? O42 K5 O101 85.99(10) . . ? O42 K5 C60 26.63(16) . . ? O101 K5 C60 97.06(14) . . ? O42 K5 C101 98.53(12) . . ? O101 K5 C101 25.69(14) . . ? C60 K5 C101 117.18(14) . . ? O42 K5 C48 74.98(18) . . ? O101 K5 C48 136.03(16) . . ? C60 K5 C48 83.4(2) . . ? C101 K5 C48 118.64(16) . . ? O42 K5 C111 138.20(16) . . ? O101 K5 C111 108.95(16) . . ? C60 K5 C111 111.57(16) . . ? C101 K5 C111 111.65(19) . . ? C48 K5 C111 111.63(16) . . ? O42 K5 C59 46.79(16) . . ? O101 K5 C59 83.96(15) . . ? C60 K5 C59 26.14(17) . . ? C101 K5 C59 108.89(15) . . ? C48 K5 C59 108.4(2) . . ? C111 K5 C59 94.85(16) . . ? O42 K5 C110 163.06(15) . . ? O101 K5 C110 100.82(16) . . ? C60 K5 C110 136.43(15) . . ? C101 K5 C110 93.96(19) . . ? C48 K5 C110 108.84(16) . . ? C111 K5 C110 24.9(2) . . ? C59 K5 C110 118.00(15) . . ? O42 K5 C112 121.18(14) . . ? O101 K5 C112 91.49(15) . . ? C60 K5 C112 96.65(14) . . ? C101 K5 C112 103.73(18) . . ? C48 K5 C112 132.31(16) . . ? C111 K5 C112 25.42(19) . . ? C59 K5 C112 74.48(14) . . ? C110 K5 C112 43.9(2) . . ? O42 K5 C109 159.36(13) . . ? O101 K5 C109 75.93(15) . . ? C60 K5 C109 145.59(14) . . ? C101 K5 C109 69.05(18) . . ? C48 K5 C109 125.19(16) . . ? C111 K5 C109 44.3(2) . . ? C59 K5 C109 120.01(14) . . ? C110 K5 C109 25.50(18) . . ? C112 K5 C109 50.8(2) . . ? O42 K5 C49 100.40(18) . . ? O101 K5 C49 141.50(19) . . ? C60 K5 C49 105.5(2) . . ? C101 K5 C49 116.62(18) . . ? C48 K5 C49 25.5(2) . . ? C111 K5 C49 91.43(17) . . ? C59 K5 C49 127.7(2) . . ? C110 K5 C49 83.99(16) . . ? C112 K5 C49 115.84(18) . . ? C109 K5 C49 99.95(16) . . ? O42 K5 C102 86.50(14) . . ? O101 K5 C102 45.44(14) . . ? C60 K5 C102 111.47(14) . . ? C101 K5 C102 25.95(17) . . ? C48 K5 C102 93.37(16) . . ? C111 K5 C102 132.0(2) . . ? C59 K5 C102 115.82(16) . . ? C110 K5 C102 109.4(2) . . ? C112 K5 C102 129.33(18) . . ? C109 K5 C102 87.78(19) . . ? C49 K5 C102 96.69(18) . . ? N127 K6 N125 114.9(3) . . ? N127 K6 N126 86.2(3) . . ? N125 K6 N126 75.3(3) . . ? N127 K6 N82 98.3(2) . . ? N125 K6 N82 92.5(2) . . ? N126 K6 N82 167.8(3) . . ? N127 K6 C101 115.7(3) . . ? N125 K6 C101 126.9(2) . . ? N126 K6 C101 122.8(2) . . ? N82 K6 C101 65.30(15) . . ? N127 K6 C106 138.4(3) . . ? N125 K6 C106 100.7(2) . . ? N126 K6 C106 124.7(2) . . ? N82 K6 C106 57.71(16) . . ? C101 K6 C106 26.33(17) . . ? N127 K6 C102 111.6(3) . . ? N125 K6 C102 132.1(2) . . ? N126 K6 C102 97.4(2) . . ? N82 K6 C102 91.40(16) . . ? C101 K6 C102 26.20(17) . . ? C106 K6 C102 44.77(18) . . ? N127 K6 C105 160.9(3) . . ? N125 K6 C105 84.0(2) . . ? N126 K6 C105 101.9(2) . . ? N82 K6 C105 77.29(17) . . ? C101 K6 C105 45.50(18) . . ? C106 K6 C105 25.48(18) . . ? C102 K6 C105 50.6(2) . . ? N127 K6 C93 82.4(2) . . ? N125 K6 C93 82.2(2) . . ? N126 K6 C93 147.6(2) . . ? N82 K6 C93 24.79(15) . . ? C101 K6 C93 89.36(16) . . ? C106 K6 C93 81.90(16) . . ? C102 K6 C93 114.99(16) . . ? C105 K6 C93 98.53(18) . . ? N127 K6 C104 147.6(2) . . ? N125 K6 C104 89.8(2) . . ? N126 K6 C104 80.0(2) . . ? N82 K6 C104 101.26(18) . . ? C101 K6 C104 52.72(18) . . ? C106 K6 C104 44.74(18) . . ? C102 K6 C104 42.7(2) . . ? C105 K6 C104 24.98(19) . . ? C93 K6 C104 123.45(18) . . ? N127 K6 C103 124.5(2) . . ? N125 K6 C103 112.1(2) . . ? N126 K6 C103 78.7(2) . . ? N82 K6 C103 107.40(16) . . ? C101 K6 C103 44.81(17) . . ? C106 K6 C103 51.23(17) . . ? C102 K6 C103 23.95(17) . . ? C105 K6 C103 42.83(19) . . ? C93 K6 C103 132.19(16) . . ? C104 K6 C103 23.82(19) . . ? N127 K6 C94 121.9(2) . . ? N125 K6 C94 78.0(2) . . ? N126 K6 C94 147.6(2) . . ? N82 K6 C94 24.14(15) . . ? C101 K6 C94 62.42(16) . . ? C106 K6 C94 44.23(16) . . ? C102 K6 C94 87.09(17) . . ? C105 K6 C94 57.06(17) . . ? C93 K6 C94 41.50(16) . . ? C104 K6 C94 82.02(18) . . ? C103 K6 C94 94.99(17) . . ? O21 K7 O102 113.81(12) 1_656 . ? O21 K7 O1 66.82(15) 1_656 1_656 ? O102 K7 O1 172.00(14) . 1_656 ? O21 K7 N128 132.36(17) 1_656 . ? O102 K7 N128 91.32(14) . . ? O1 K7 N128 93.70(11) 1_656 . ? O21 K7 O82 89.65(15) 1_656 . ? O102 K7 O82 65.58(13) . . ? O1 K7 O82 106.67(15) 1_656 . ? N128 K7 O82 137.98(19) . . ? O21 K7 C120 123.08(13) 1_656 . ? O102 K7 C120 22.72(15) . . ? O1 K7 C120 163.53(12) 1_656 . ? N128 K7 C120 69.88(15) . . ? O82 K7 C120 87.37(15) . . ? O21 K7 C1 87.50(15) 1_656 1_656 ? O102 K7 C1 158.65(13) . 1_656 ? O1 K7 C1 21.87(15) 1_656 1_656 ? N128 K7 C1 73.91(13) . 1_656 ? O82 K7 C1 115.65(17) . 1_656 ? C120 K7 C1 142.95(13) . 1_656 ? O21 K7 C21 20.87(15) 1_656 1_656 ? O102 K7 C21 94.36(13) . 1_656 ? O1 K7 C21 87.15(16) 1_656 1_656 ? N128 K7 C21 130.2(2) . 1_656 ? O82 K7 C21 88.05(15) . 1_656 ? C120 K7 C21 102.22(13) . 1_656 ? C1 K7 C21 106.93(16) 1_656 1_656 ? O21 K7 C22 43.73(16) 1_656 1_656 ? O102 K7 C22 70.92(13) . 1_656 ? O1 K7 C22 110.49(16) 1_656 1_656 ? N128 K7 C22 127.6(2) . 1_656 ? O82 K7 C22 79.40(15) . 1_656 ? C120 K7 C22 80.06(13) . 1_656 ? C1 K7 C22 130.33(17) 1_656 1_656 ? C21 K7 C22 23.46(16) 1_656 1_656 ? O21 K7 C156 113.96(13) 1_656 . ? O102 K7 C156 90.03(13) . . ? O1 K7 C156 96.96(11) 1_656 . ? N128 K7 C156 21.99(8) . . ? O82 K7 C156 151.91(12) . . ? C120 K7 C156 67.34(14) . . ? C1 K7 C156 81.91(13) 1_656 . ? C21 K7 C156 108.46(14) 1_656 . ? C22 K7 C156 106.64(14) 1_656 . ? O21 K7 C99 79.10(12) 1_656 . ? O102 K7 C99 107.04(15) . . ? O1 K7 C99 65.03(11) 1_656 . ? N128 K7 C99 133.2(2) . . ? O82 K7 C99 42.08(14) . . ? C120 K7 C99 127.27(16) . . ? C1 K7 C99 74.50(13) 1_656 . ? C21 K7 C99 91.78(13) 1_656 . ? C22 K7 C99 99.22(13) 1_656 . ? C156 K7 C99 152.63(18) . . ? O21 K7 C100 87.18(12) 1_656 . ? O102 K7 C100 83.60(15) . . ? O1 K7 C100 88.49(12) 1_656 . ? N128 K7 C100 137.4(2) . . ? O82 K7 C100 18.93(14) . . ? C120 K7 C100 104.43(16) . . ? C1 K7 C100 96.78(14) 1_656 . ? C21 K7 C100 92.37(12) 1_656 . ? C22 K7 C100 90.53(12) 1_656 . ? C156 K7 C100 158.65(17) . . ? C99 K7 C100 23.47(15) . . ? O82 K8 O21 84.18(13) . 1_656 ? O82 K8 C21 96.57(17) . 1_656 ? O21 K8 C21 26.83(16) 1_656 1_656 ? O82 K8 C100 25.65(16) . . ? O21 K8 C100 95.44(14) 1_656 . ? C21 K8 C100 115.47(14) 1_656 . ? O82 K8 C22 84.28(17) . 1_656 ? O21 K8 C22 47.01(16) 1_656 1_656 ? C21 K8 C22 26.41(17) 1_656 1_656 ? C100 K8 C22 108.77(15) . 1_656 ? O82 K8 C32 126.81(18) . 1_656 ? O21 K8 C32 96.62(16) 1_656 1_656 ? C21 K8 C32 107.6(2) 1_656 1_656 ? C100 K8 C32 102.60(16) . 1_656 ? C22 K8 C32 132.9(2) 1_656 1_656 ? O82 K8 C31 142.5(2) . 1_656 ? O21 K8 C31 113.39(17) 1_656 1_656 ? C21 K8 C31 114.0(2) 1_656 1_656 ? C100 K8 C31 116.93(18) . 1_656 ? C22 K8 C31 132.3(2) 1_656 1_656 ? C32 K8 C31 24.86(19) 1_656 1_656 ? O82 K8 C99 45.36(15) . . ? O21 K8 C99 81.73(14) 1_656 . ? C21 K8 C99 107.36(14) 1_656 . ? C100 K8 C99 26.36(17) . . ? C22 K8 C99 113.45(15) 1_656 . ? C32 K8 C99 81.94(15) 1_656 . ? C31 K8 C99 102.32(17) 1_656 . ? O82 K8 C29 162.67(17) . 1_656 ? O21 K8 C29 79.42(16) 1_656 1_656 ? C21 K8 C29 70.9(2) 1_656 1_656 ? C100 K8 C29 151.14(16) . 1_656 ? C22 K8 C29 88.6(2) 1_656 1_656 ? C32 K8 C29 50.7(2) 1_656 1_656 ? C31 K8 C29 44.1(2) 1_656 1_656 ? C99 K8 C29 125.60(15) . 1_656 ? O82 K8 C33 124.43(16) . 1_656 ? O21 K8 C33 71.87(16) 1_656 1_656 ? C21 K8 C33 83.95(19) 1_656 1_656 ? C100 K8 C33 106.94(15) . 1_656 ? C22 K8 C33 110.17(19) 1_656 1_656 ? C32 K8 C33 24.89(18) 1_656 1_656 ? C31 K8 C33 44.51(18) 1_656 1_656 ? C99 K8 C33 81.30(14) . 1_656 ? C29 K8 C33 44.4(2) 1_656 1_656 ? O82 K8 C30 167.3(2) . 1_656 ? O21 K8 C30 103.64(18) 1_656 1_656 ? C21 K8 C30 94.7(2) 1_656 1_656 ? C100 K8 C30 141.89(18) . 1_656 ? C22 K8 C30 108.4(2) 1_656 1_656 ? C32 K8 C30 43.2(2) 1_656 1_656 ? C31 K8 C30 25.0(2) 1_656 1_656 ? C99 K8 C30 125.06(17) . 1_656 ? C29 K8 C30 24.63(19) 1_656 1_656 ? C33 K8 C30 51.19(19) 1_656 1_656 ? O82 K8 C89 95.51(16) . . ? O21 K8 C89 127.20(19) 1_656 . ? C21 K8 C89 102.3(2) 1_656 . ? C100 K8 C89 106.57(18) . . ? C22 K8 C89 80.3(2) 1_656 . ? C32 K8 C89 123.05(19) 1_656 . ? C31 K8 C89 98.4(2) 1_656 . ? C99 K8 C89 132.40(17) . . ? C29 K8 C89 98.82(19) 1_656 . ? C33 K8 C89 138.91(18) 1_656 . ? C30 K8 C89 87.72(19) 1_656 . ? N129 K9 N130 83.4(3) . . ? N129 K9 N101 159.7(3) . . ? N130 K9 N101 105.62(19) . . ? N129 K9 C95 118.8(2) . . ? N130 K9 C95 153.4(2) . . ? N101 K9 C95 58.81(16) . . ? N129 K9 C100 124.1(3) . . ? N130 K9 C100 130.0(2) . . ? N101 K9 C100 63.86(16) . . ? C95 K9 C100 25.88(19) . . ? N129 K9 C108 145.4(3) . . ? N130 K9 C108 83.70(19) . . ? N101 K9 C108 25.77(15) . . ? C95 K9 C108 84.31(17) . . ? C100 K9 C108 88.29(17) . . ? N129 K9 C96 93.8(3) . . ? N130 K9 C96 170.1(2) . . ? N101 K9 C96 80.12(18) . . ? C95 K9 C96 25.64(19) . . ? C100 K9 C96 44.9(2) . . ? C108 K9 C96 103.61(19) . . ? N129 K9 C99 101.7(3) . . ? N130 K9 C99 121.6(2) . . ? N101 K9 C99 89.10(16) . . ? C95 K9 C99 43.98(19) . . ? C100 K9 C99 25.64(17) . . ? C108 K9 C99 112.40(17) . . ? C96 K9 C99 49.6(2) . . ? N129 K9 C107 136.5(2) . . ? N130 K9 C107 127.33(19) . . ? N101 K9 C107 25.58(15) . . ? C95 K9 C107 46.29(17) . . ? C100 K9 C107 63.05(16) . . ? C108 K9 C107 43.65(16) . . ? C96 K9 C107 60.47(19) . . ? C99 K9 C107 87.64(17) . . ? N129 K9 C97 75.8(3) . . ? N130 K9 C97 147.4(2) . . ? N101 K9 C97 102.35(17) . . ? C95 K9 C97 44.00(18) . . ? C100 K9 C97 51.8(2) . . ? C108 K9 C97 126.97(18) . . ? C96 K9 C97 23.86(19) . . ? C99 K9 C97 42.2(2) . . ? C107 K9 C97 84.28(18) . . ? N129 K9 C98 80.1(3) . . ? N130 K9 C98 128.8(2) . . ? N101 K9 C98 106.39(17) . . ? C95 K9 C98 50.26(18) . . ? C100 K9 C98 44.14(19) . . ? C108 K9 C98 131.86(18) . . ? C96 K9 C98 41.3(2) . . ? C99 K9 C98 24.0(2) . . ? C107 K9 C98 96.31(18) . . ? C97 K9 C98 23.1(2) . . ? N129 K9 C161 19.3(3) . . ? N130 K9 C161 77.1(3) . . ? N101 K9 C161 177.3(3) . . ? C95 K9 C161 118.7(3) . . ? C100 K9 C161 114.5(2) . . ? C108 K9 C161 156.4(2) . . ? C96 K9 C161 97.2(3) . . ? C99 K9 C161 89.5(2) . . ? C107 K9 C161 152.0(3) . . ? C97 K9 C161 75.1(3) . . ? C98 K9 C161 71.6(3) . . ? N130 K9B C100 158.4(5) . . ? N130 K9B N101 109.0(3) . . ? C100 K9B N101 64.33(18) . . ? N130 K9B C99 144.6(4) . . ? C100 K9B C99 27.44(18) . . ? N101 K9B C99 90.7(2) . . ? N130 K9B C166 26.36(9) . . ? C100 K9B C166 159.6(3) . . ? N101 K9B C166 133.8(3) . . ? C99 K9B C166 132.3(3) . . ? N130 K9B O82 168.9(4) . . ? C100 K9B O82 24.51(16) . . ? N101 K9B O82 60.93(18) . . ? C99 K9B O82 44.87(16) . . ? C166 K9B O82 160.7(4) . . ? N130 K9B C108 85.7(2) . . ? C100 K9B C108 89.0(2) . . ? N101 K9B C108 24.72(14) . . ? C99 K9B C108 115.1(3) . . ? C166 K9B C108 109.3(2) . . ? O82 K9B C108 83.5(2) . . ? N130 K9B N102 96.5(3) . . ? C100 K9B N102 93.8(2) . . ? N101 K9B N102 50.05(14) . . ? C99 K9B N102 118.4(3) . . ? C166 K9B N102 105.7(3) . . ? O82 K9B N102 73.5(2) . . ? C108 K9B N102 42.68(16) . . ? N130 K9B C113 79.4(2) . . ? C100 K9B C113 103.7(2) . . ? N101 K9B C113 43.59(15) . . ? C99 K9B C113 131.1(3) . . ? C166 K9B C113 96.6(2) . . ? O82 K9B C113 89.6(2) . . ? C108 K9B C113 24.56(16) . . ? N102 K9B C113 24.36(15) . . ? N130 K9B K7 135.8(4) . . ? C100 K9B K7 65.14(18) . . ? N101 K9B K7 100.5(3) . . ? C99 K9B K7 63.75(17) . . ? C166 K9B K7 112.6(3) . . ? O82 K9B K7 48.06(17) . . ? C108 K9B K7 113.9(3) . . ? N102 K9B K7 77.7(2) . . ? C113 K9B K7 102.1(3) . . ? N130 K9B Nd3 132.1(3) . . ? C100 K9B Nd3 55.09(14) . . ? N101 K9B Nd3 36.17(11) . . ? C99 K9B Nd3 80.65(18) . . ? C166 K9B Nd3 144.2(3) . . ? O82 K9B Nd3 36.92(13) . . ? C108 K9B Nd3 51.39(13) . . ? N102 K9B Nd3 38.68(10) . . ? C113 K9B Nd3 52.73(13) . . ? K7 K9B Nd3 64.81(17) . . ? C1 O1 Nd1 129.6(4) . . ? C1 O1 K7 107.6(4) . 1_454 ? Nd1 O1 K7 107.76(19) . 1_454 ? C20 O2 Nd1 127.1(4) . . ? C20 O2 K1 115.0(4) . . ? Nd1 O2 K1 104.49(16) . . ? C20 O2 K2 91.2(4) . . ? Nd1 O2 K2 120.47(18) . . ? K1 O2 K2 93.99(15) . . ? C7 N1 C8 120.5(6) . . ? C7 N1 Nd1 128.1(5) . . ? C8 N1 Nd1 111.4(4) . . ? C13 N2 C14 116.5(5) . . ? C13 N2 Nd1 118.1(4) . . ? C14 N2 Nd1 109.8(4) . . ? O1 C1 C2 118.8(7) . . ? O1 C1 C6 123.0(6) . . ? C2 C1 C6 118.1(6) . . ? O1 C1 K7 50.6(3) . 1_454 ? C2 C1 K7 112.4(5) . 1_454 ? C6 C1 K7 104.4(5) . 1_454 ? C3 C2 C1 122.0(8) . . ? C2 C3 C4 120.3(9) . . ? C5 C4 C3 117.7(7) . . ? C4 C5 C6 123.3(7) . . ? C5 C6 C1 118.3(7) . . ? C5 C6 C7 117.3(6) . . ? C1 C6 C7 124.3(6) . . ? N1 C7 C6 126.4(7) . . ? C9 C8 N1 122.1(6) . . ? C9 C8 C13 121.7(6) . . ? N1 C8 C13 115.8(6) . . ? C9 C8 K2 76.4(4) . . ? N1 C8 K2 107.5(4) . . ? C13 C8 K2 81.2(4) . . ? C8 C9 C10 120.5(7) . . ? C8 C9 K2 78.5(4) . . ? C10 C9 K2 80.4(4) . . ? C11 C10 C9 119.4(7) . . ? C11 C10 K2 80.3(5) . . ? C9 C10 K2 74.3(4) . . ? C10 C11 C12 120.8(7) . . ? C10 C11 K2 75.5(5) . . ? C12 C11 K2 78.9(4) . . ? C11 C12 C13 122.5(7) . . ? C11 C12 K2 76.9(4) . . ? C13 C12 K2 76.5(4) . . ? N2 C13 C12 127.0(6) . . ? N2 C13 C8 117.8(6) . . ? C12 C13 C8 115.1(6) . . ? N2 C13 K2 114.7(4) . . ? C12 C13 K2 78.7(4) . . ? C8 C13 K2 73.1(4) . . ? N2 C14 C15 115.4(6) . . ? N2 C14 C27 109.7(5) . . ? C15 C14 C27 108.4(6) . . ? C16 C15 C20 117.5(7) . . ? C16 C15 C14 119.3(7) . . ? C20 C15 C14 123.2(6) . . ? C17 C16 C15 125.0(8) . . ? C16 C17 C18 117.3(7) . . ? C19 C18 C17 119.7(8) . . ? C18 C19 C20 123.7(9) . . ? C18 C19 K2 132.1(6) . . ? C20 C19 K2 66.9(4) . . ? C18 C19 K1 151.6(6) . . ? C20 C19 K1 77.7(5) . . ? K2 C19 K1 70.80(16) . . ? O2 C20 C19 120.2(8) . . ? O2 C20 C15 123.1(6) . . ? C19 C20 C15 116.7(7) . . ? O2 C20 K2 62.7(3) . . ? C19 C20 K2 88.1(5) . . ? C15 C20 K2 119.4(5) . . ? O2 C20 K1 44.4(3) . . ? C19 C20 K1 79.1(5) . . ? C15 C20 K1 157.9(5) . . ? K2 C20 K1 74.11(18) . . ? C21 O21 Nd1 129.1(4) . . ? C21 O21 K7 115.2(4) . 1_454 ? Nd1 O21 K7 106.92(17) . 1_454 ? C21 O21 K8 82.0(3) . 1_454 ? Nd1 O21 K8 122.86(19) . 1_454 ? K7 O21 K8 94.14(14) 1_454 1_454 ? C40 O22 Nd1 131.7(4) . . ? C40 O22 K1 103.8(4) . . ? Nd1 O22 K1 108.71(17) . . ? C28 N21 C27 118.2(6) . . ? C28 N21 Nd1 117.4(5) . . ? C27 N21 Nd1 109.1(4) . . ? C34 N22 C33 120.0(7) . . ? C34 N22 Nd1 127.5(5) . . ? C33 N22 Nd1 112.2(5) . . ? O21 C21 C22 120.7(6) . . ? O21 C21 C26 123.6(6) . . ? C22 C21 C26 115.7(6) . . ? O21 C21 K8 71.2(3) . 1_454 ? C22 C21 K8 83.2(4) . 1_454 ? C26 C21 K8 115.2(5) . 1_454 ? O21 C21 K7 43.9(3) . 1_454 ? C22 C21 K7 79.2(4) . 1_454 ? C26 C21 K7 160.8(4) . 1_454 ? K8 C21 K7 77.12(16) 1_454 1_454 ? C23 C22 C21 124.7(7) . . ? C23 C22 K8 121.0(5) . 1_454 ? C21 C22 K8 70.4(4) . 1_454 ? C23 C22 K7 155.1(5) . 1_454 ? C21 C22 K7 77.4(4) . 1_454 ? K8 C22 K7 74.77(16) 1_454 1_454 ? C24 C23 C22 119.6(7) . . ? C23 C24 C25 118.1(8) . . ? C26 C25 C24 122.7(7) . . ? C25 C26 C21 119.3(7) . . ? C25 C26 C27 118.4(6) . . ? C21 C26 C27 122.4(6) . . ? N21 C27 C26 114.7(6) . . ? N21 C27 C14 109.0(5) . . ? C26 C27 C14 110.9(6) . . ? N21 C28 C29 124.6(8) . . ? N21 C28 C33 119.7(6) . . ? C29 C28 C33 115.6(7) . . ? N21 C28 K8 115.3(4) . 1_454 ? C29 C28 K8 75.8(4) . 1_454 ? C33 C28 K8 75.9(4) . 1_454 ? C30 C29 C28 121.8(8) . . ? C30 C29 K8 77.9(5) . 1_454 ? C28 C29 K8 78.5(4) . 1_454 ? C29 C30 C31 121.9(8) . . ? C29 C30 K8 77.5(4) . 1_454 ? C31 C30 K8 77.1(4) . 1_454 ? C32 C31 C30 116.9(8) . . ? C32 C31 K8 76.3(5) . 1_454 ? C30 C31 K8 77.9(5) . 1_454 ? C31 C32 C33 124.2(8) . . ? C31 C32 K8 78.9(5) . 1_454 ? C33 C32 K8 79.1(4) . 1_454 ? C32 C33 N22 124.8(7) . . ? C32 C33 C28 119.6(7) . . ? N22 C33 C28 115.4(6) . . ? C32 C33 K8 76.0(4) . 1_454 ? N22 C33 K8 111.4(4) . 1_454 ? C28 C33 K8 78.5(4) . 1_454 ? N22 C34 C35 127.5(7) . . ? C36 C35 C40 118.3(7) . . ? C36 C35 C34 117.1(7) . . ? C40 C35 C34 124.6(6) . . ? C37 C36 C35 122.8(8) . . ? C36 C37 C38 120.0(8) . . ? C39 C38 C37 118.9(7) . . ? C38 C39 C40 121.8(7) . . ? C38 C39 K3 97.0(5) . . ? C40 C39 K3 118.0(4) . . ? O22 C40 C39 119.7(6) . . ? O22 C40 C35 122.1(6) . . ? C39 C40 C35 118.2(7) . . ? O22 C40 K1 52.9(3) . . ? C39 C40 K1 108.7(4) . . ? C35 C40 K1 106.4(4) . . ? C41 O41 Nd2 128.7(4) . . ? C41 O41 K1 119.0(4) . . ? Nd2 O41 K1 109.51(19) . . ? C41 O41 K3 115.4(5) . . ? Nd2 O41 K3 80.21(16) . . ? K1 O41 K3 88.34(15) . . ? C60 O42 Nd2 128.3(4) . . ? C60 O42 K4 115.6(4) . . ? Nd2 O42 K4 103.37(16) . . ? C60 O42 K5 88.7(4) . . ? Nd2 O42 K5 121.30(18) . . ? K4 O42 K5 95.07(14) . . ? C47 N41 C48 120.0(7) . . ? C47 N41 Nd2 124.2(5) . . ? C48 N41 Nd2 113.4(5) . . ? C47 N41 K3 109.9(5) . . ? C48 N41 K3 95.1(4) . . ? Nd2 N41 K3 79.13(16) . . ? C53 N42 C54 115.5(6) . . ? C53 N42 Nd2 120.6(5) . . ? C54 N42 Nd2 108.1(4) . . ? C53 N42 K3 94.4(4) . . ? C54 N42 K3 133.3(4) . . ? Nd2 N42 K3 82.68(17) . . ? O41 C41 C46 122.5(7) . . ? O41 C41 C42 119.4(8) . . ? C46 C41 C42 118.1(8) . . ? O41 C41 K1 41.8(3) . . ? C46 C41 K1 152.6(6) . . ? C42 C41 K1 81.7(5) . . ? C43 C42 C41 121.3(10) . . ? C42 C43 C44 121.3(9) . . ? C45 C44 C43 115.5(9) . . ? C44 C45 C46 126.4(10) . . ? C41 C46 C45 117.4(8) . . ? C41 C46 C47 124.5(7) . . ? C45 C46 C47 118.1(8) . . ? N41 C47 C46 127.1(8) . . ? C49 C48 N41 125.6(8) . . ? C49 C48 C53 120.2(8) . . ? N41 C48 C53 114.3(7) . . ? C49 C48 K5 81.8(5) . . ? N41 C48 K5 100.9(4) . . ? C53 C48 K5 87.0(4) . . ? C49 C48 K3 131.3(5) . . ? N41 C48 K3 60.8(4) . . ? C53 C48 K3 77.8(4) . . ? K5 C48 K3 146.9(3) . . ? C50 C49 C48 121.9(9) . . ? C50 C49 K5 90.8(6) . . ? C48 C49 K5 72.7(4) . . ? C51 C50 C49 118.9(9) . . ? C50 C51 C52 122.9(9) . . ? C51 C52 C53 120.3(9) . . ? N42 C53 C48 119.5(7) . . ? N42 C53 C52 124.8(7) . . ? C48 C53 C52 115.7(7) . . ? N42 C53 K5 110.8(4) . . ? C48 C53 K5 68.2(4) . . ? C52 C53 K5 87.1(4) . . ? N42 C53 K3 62.1(4) . . ? C48 C53 K3 78.3(4) . . ? C52 C53 K3 134.7(5) . . ? K5 C53 K3 135.6(2) . . ? N42 C54 C55 112.6(6) . . ? N42 C54 C67 110.6(5) . . ? C55 C54 C67 109.3(6) . . ? C56 C55 C60 119.9(6) . . ? C56 C55 C54 116.9(6) . . ? C60 C55 C54 123.2(6) . . ? C55 C56 C57 121.9(7) . . ? C58 C57 C56 117.8(7) . . ? C57 C58 C59 120.6(7) . . ? C58 C59 C60 123.3(7) . . ? C58 C59 K5 127.7(6) . . ? C60 C59 K5 70.3(4) . . ? C58 C59 K4 153.3(6) . . ? C60 C59 K4 77.1(4) . . ? K5 C59 K4 72.86(16) . . ? O42 C60 C59 119.2(6) . . ? O42 C60 C55 124.3(6) . . ? C59 C60 C55 116.4(6) . . ? O42 C60 K5 64.7(3) . . ? C59 C60 K5 83.6(4) . . ? C55 C60 K5 120.0(5) . . ? O42 C60 K4 43.9(3) . . ? C59 C60 K4 79.7(4) . . ? C55 C60 K4 157.6(5) . . ? K5 C60 K4 75.31(16) . . ? C61 O61 Nd2 129.0(4) . . ? C61 O61 K3 89.9(4) . . ? Nd2 O61 K3 88.71(15) . . ? C61 O61 K1 128.1(4) . . ? Nd2 O61 K1 102.93(15) . . ? K3 O61 K1 93.65(14) . . ? C61 O61 K2 71.2(3) . . ? Nd2 O61 K2 123.05(17) . . ? K3 O61 K2 148.23(16) . . ? K1 O61 K2 79.53(12) . . ? C80 O62 Nd2 130.8(5) . . ? C80 O62 K4 110.1(5) . . ? Nd2 O62 K4 103.60(18) . . ? C68 N61 C67 117.6(6) . . ? C68 N61 Nd2 122.9(5) . . ? C67 N61 Nd2 110.0(4) . . ? C74 N62 C73 118.2(7) . . ? C74 N62 Nd2 128.2(6) . . ? C73 N62 Nd2 113.4(4) . . ? O61 C61 C66 124.6(5) . . ? O61 C61 C62 118.3(6) . . ? C66 C61 C62 117.0(6) . . ? O61 C61 K3 64.5(3) . . ? C66 C61 K3 113.2(4) . . ? C62 C61 K3 93.3(4) . . ? O61 C61 K2 85.2(4) . . ? C66 C61 K2 104.6(4) . . ? C62 C61 K2 78.8(4) . . ? K3 C61 K2 140.5(2) . . ? C63 C62 C61 121.2(7) . . ? C63 C62 K2 109.4(5) . . ? C61 C62 K2 75.0(4) . . ? C63 C62 K3 124.4(5) . . ? C61 C62 K3 62.2(4) . . ? K2 C62 K3 122.9(2) . . ? C64 C63 C62 121.1(6) . . ? C65 C64 C63 117.4(7) . . ? C64 C65 C66 124.3(7) . . ? C65 C66 C61 118.9(6) . . ? C65 C66 C67 118.3(6) . . ? C61 C66 C67 122.8(5) . . ? N61 C67 C54 110.6(5) . . ? N61 C67 C66 111.0(5) . . ? C54 C67 C66 112.8(5) . . ? N61 C68 C73 119.7(7) . . ? N61 C68 C69 124.5(7) . . ? C73 C68 C69 115.8(7) . . ? N61 C68 K2 116.3(5) . . ? C73 C68 K2 77.8(5) . . ? C69 C68 K2 73.4(4) . . ? C70 C69 C68 121.5(7) . . ? C70 C69 K2 76.9(5) . . ? C68 C69 K2 81.0(4) . . ? C69 C70 C71 122.3(8) . . ? C69 C70 K2 78.6(5) . . ? C71 C70 K2 79.1(6) . . ? C70 C71 C72 118.2(8) . . ? C70 C71 K2 76.2(5) . . ? C72 C71 K2 79.7(6) . . ? C71 C72 C73 122.6(8) . . ? C71 C72 K2 75.8(5) . . ? C73 C72 K2 79.4(5) . . ? C72 C73 C68 119.6(8) . . ? C72 C73 N62 125.4(7) . . ? C68 C73 N62 114.9(7) . . ? C72 C73 K2 76.1(5) . . ? C68 C73 K2 77.3(5) . . ? N62 C73 K2 114.4(5) . . ? N62 C74 C75 125.5(9) . . ? C76 C75 C80 119.6(9) . . ? C76 C75 C74 116.4(9) . . ? C80 C75 C74 124.0(8) . . ? C77 C76 C75 120.3(11) . . ? C78 C77 C76 119.8(9) . . ? C79 C78 C77 120.3(10) . . ? C78 C79 C80 122.8(10) . . ? O62 C80 C79 120.9(9) . . ? O62 C80 C75 122.0(8) . . ? C79 C80 C75 117.0(8) . . ? O62 C80 K4 48.7(4) . . ? C79 C80 K4 117.1(5) . . ? C75 C80 K4 101.4(6) . . ? C81 O81 Nd3 137.0(4) . . ? C81 O81 K4 100.3(4) . . ? Nd3 O81 K4 112.89(17) . . ? C100 O82 Nd3 128.0(4) . . ? C100 O82 K7 117.9(4) . . ? Nd3 O82 K7 104.94(16) . . ? C100 O82 K8 84.4(3) . . ? Nd3 O82 K8 123.80(18) . . ? K7 O82 K8 91.94(13) . . ? C100 O82 K9B 71.3(3) . . ? Nd3 O82 K9B 95.2(2) . . ? K7 O82 K9B 74.2(2) . . ? K8 O82 K9B 141.0(2) . . ? C87 N81 C88 119.6(6) . . ? C87 N81 Nd3 128.5(5) . . ? C88 N81 Nd3 111.9(4) . . ? C93 N82 C94 116.9(6) . . ? C93 N82 Nd3 117.3(4) . . ? C94 N82 Nd3 108.3(4) . . ? C93 N82 K6 91.1(4) . . ? C94 N82 K6 100.5(4) . . ? Nd3 N82 K6 121.2(2) . . ? O81 C81 C82 120.2(7) . . ? O81 C81 C86 121.5(7) . . ? C82 C81 C86 118.2(7) . . ? O81 C81 K4 55.5(3) . . ? C82 C81 K4 96.4(5) . . ? C86 C81 K4 114.2(4) . . ? C83 C82 C81 121.5(8) . . ? C82 C83 C84 121.2(9) . . ? C85 C84 C83 119.2(9) . . ? C84 C85 C86 121.5(8) . . ? C85 C86 C81 118.3(7) . . ? C85 C86 C87 116.9(7) . . ? C81 C86 C87 124.7(7) . . ? N81 C87 C86 127.6(7) . . ? C89 C88 N81 123.2(7) . . ? C89 C88 C93 121.1(7) . . ? N81 C88 C93 115.7(5) . . ? C89 C88 K8 76.9(4) . . ? N81 C88 K8 113.9(4) . . ? C93 C88 K8 78.9(4) . . ? C88 C89 C90 121.9(8) . . ? C88 C89 K8 78.6(4) . . ? C90 C89 K8 79.2(4) . . ? C91 C90 C89 118.9(7) . . ? C91 C90 K8 78.3(4) . . ? C89 C90 K8 76.1(4) . . ? C90 C91 C92 119.8(7) . . ? C90 C91 K8 77.2(4) . . ? C92 C91 K8 76.8(4) . . ? C91 C92 C93 122.9(7) . . ? C91 C92 K8 78.5(4) . . ? C93 C92 K8 78.8(4) . . ? N82 C93 C92 126.2(7) . . ? N82 C93 C88 118.5(6) . . ? C92 C93 C88 115.3(6) . . ? N82 C93 K6 64.1(3) . . ? C92 C93 K6 100.6(4) . . ? C88 C93 K6 107.8(4) . . ? N82 C93 K8 115.9(4) . . ? C92 C93 K8 76.3(4) . . ? C88 C93 K8 75.7(4) . . ? K6 C93 K8 176.2(3) . . ? N82 C94 C107 109.6(5) . . ? N82 C94 C95 114.6(5) . . ? C107 C94 C95 110.4(5) . . ? N82 C94 K6 55.3(3) . . ? C107 C94 K6 94.4(4) . . ? C95 C94 K6 155.1(4) . . ? C100 C95 C96 120.0(7) . . ? C100 C95 C94 123.0(6) . . ? C96 C95 C94 116.8(7) . . ? C100 C95 K9 77.9(4) . . ? C96 C95 K9 82.0(4) . . ? C94 C95 K9 106.1(4) . . ? C97 C96 C95 122.4(8) . . ? C97 C96 K9 83.6(5) . . ? C95 C96 K9 72.3(4) . . ? C98 C97 C96 118.4(8) . . ? C98 C97 K9 79.2(5) . . ? C96 C97 K9 72.5(5) . . ? C97 C98 C99 121.7(8) . . ? C97 C98 K9 77.7(5) . . ? C99 C98 K9 74.0(4) . . ? C98 C99 C100 121.3(7) . . ? C98 C99 K9B 108.4(5) . . ? C100 C99 K9B 72.1(4) . . ? C98 C99 K8 123.6(5) . . ? C100 C99 K8 67.4(4) . . ? K9B C99 K8 125.2(2) . . ? C98 C99 K9 82.0(5) . . ? C100 C99 K9 71.1(4) . . ? K9B C99 K9 31.7(2) . . ? K8 C99 K9 138.3(2) . . ? C98 C99 K7 156.7(6) . . ? C100 C99 K7 79.1(4) . . ? K9B C99 K7 64.7(2) . . ? K8 C99 K7 72.56(16) . . ? K9 C99 K7 95.89(18) . . ? O82 C100 C95 124.6(6) . . ? O82 C100 C99 119.3(6) . . ? C95 C100 C99 116.1(7) . . ? O82 C100 K9B 84.2(4) . . ? C95 C100 K9B 107.2(4) . . ? C99 C100 K9B 80.4(4) . . ? O82 C100 K8 70.0(3) . . ? C95 C100 K8 112.5(4) . . ? C99 C100 K8 86.2(4) . . ? K9B C100 K8 140.1(3) . . ? O82 C100 K9 111.7(4) . . ? C95 C100 K9 76.2(4) . . ? C99 C100 K9 83.3(4) . . ? K9B C100 K9 33.2(2) . . ? K8 C100 K9 168.7(3) . . ? O82 C100 K7 43.2(3) . . ? C95 C100 K7 164.2(5) . . ? C99 C100 K7 77.4(4) . . ? K9B C100 K7 65.4(2) . . ? K8 C100 K7 75.03(16) . . ? K9 C100 K7 98.37(17) . . ? C101 O101 Nd3 126.1(4) . . ? C101 O101 K4 117.9(4) . . ? Nd3 O101 K4 105.55(14) . . ? C101 O101 K5 83.9(3) . . ? Nd3 O101 K5 128.90(18) . . ? K4 O101 K5 89.03(12) . . ? C120 O102 Nd3 131.3(4) . . ? C120 O102 K7 105.6(4) . . ? Nd3 O102 K7 112.83(18) . . ? C108 N101 C107 118.1(5) . . ? C108 N101 Nd3 116.2(4) . . ? C107 N101 Nd3 107.5(4) . . ? C108 N101 K9 89.1(4) . . ? C107 N101 K9 96.2(4) . . ? Nd3 N101 K9 128.7(2) . . ? C108 N101 K9B 88.5(4) . . ? C107 N101 K9B 126.4(4) . . ? Nd3 N101 K9B 98.6(2) . . ? K9 N101 K9B 34.7(2) . . ? C114 N102 C113 119.7(6) . . ? C114 N102 Nd3 126.9(5) . . ? C113 N102 Nd3 113.1(4) . . ? C114 N102 K9B 107.2(4) . . ? C113 N102 K9B 79.0(4) . . ? Nd3 N102 K9B 87.03(15) . . ? O101 C101 C106 123.7(6) . . ? O101 C101 C102 120.6(6) . . ? C106 C101 C102 115.7(6) . . ? O101 C101 K5 70.4(3) . . ? C106 C101 K5 115.1(4) . . ? C102 C101 K5 85.2(4) . . ? O101 C101 K6 110.3(4) . . ? C106 C101 K6 78.3(4) . . ? C102 C101 K6 81.0(4) . . ? K5 C101 K6 164.1(2) . . ? C103 C102 C101 123.4(7) . . ? C103 C102 K6 83.3(4) . . ? C101 C102 K6 72.8(4) . . ? C103 C102 K5 124.6(5) . . ? C101 C102 K5 68.9(4) . . ? K6 C102 K5 141.0(2) . . ? C102 C103 C104 120.9(7) . . ? C102 C103 K6 72.8(4) . . ? C104 C103 K6 77.5(4) . . ? C103 C104 C105 118.1(7) . . ? C103 C104 K6 78.7(4) . . ? C105 C104 K6 73.2(4) . . ? C106 C105 C104 121.9(7) . . ? C106 C105 K6 74.4(4) . . ? C104 C105 K6 81.8(4) . . ? C105 C106 C101 119.8(6) . . ? C105 C106 C107 116.2(6) . . ? C101 C106 C107 123.8(6) . . ? C105 C106 K6 80.1(4) . . ? C101 C106 K6 75.4(4) . . ? C107 C106 K6 110.4(4) . . ? N101 C107 C106 114.8(5) . . ? N101 C107 C94 109.6(5) . . ? C106 C107 C94 110.4(6) . . ? N101 C107 K9 58.3(3) . . ? C106 C107 K9 151.7(4) . . ? C94 C107 K9 97.2(3) . . ? N101 C108 C109 124.5(7) . . ? N101 C108 C113 119.7(6) . . ? C109 C108 C113 115.8(6) . . ? N101 C108 K9 65.2(3) . . ? C109 C108 K9 94.9(5) . . ? C113 C108 K9 112.5(4) . . ? N101 C108 K9B 66.8(3) . . ? C109 C108 K9B 121.2(5) . . ? C113 C108 K9B 84.1(4) . . ? K9 C108 K9B 31.7(2) . . ? N101 C108 K5 119.4(4) . . ? C109 C108 K5 72.8(4) . . ? C113 C108 K5 76.2(4) . . ? K9 C108 K5 167.4(2) . . ? K9B C108 K5 159.7(2) . . ? C108 C109 C110 122.5(7) . . ? C108 C109 K5 82.6(4) . . ? C110 C109 K5 74.8(5) . . ? C108 C109 K9 61.9(4) . . ? C110 C109 K9 125.4(5) . . ? K5 C109 K9 144.4(2) . . ? C111 C110 C109 120.4(7) . . ? C111 C110 K5 77.1(5) . . ? C109 C110 K5 79.7(4) . . ? C110 C111 C112 119.4(7) . . ? C110 C111 K5 78.0(5) . . ? C112 C111 K5 79.8(5) . . ? C113 C112 C111 121.1(7) . . ? C113 C112 K5 81.7(4) . . ? C111 C112 K5 74.8(5) . . ? C112 C113 C108 120.7(6) . . ? C112 C113 N102 123.7(6) . . ? C108 C113 N102 115.3(5) . . ? C112 C113 K5 73.7(4) . . ? C108 C113 K5 78.9(4) . . ? N102 C113 K5 113.3(4) . . ? C112 C113 K9B 126.0(5) . . ? C108 C113 K9B 71.3(3) . . ? N102 C113 K9B 76.6(3) . . ? K5 C113 K9B 149.9(2) . . ? N102 C114 C115 128.1(6) . . ? C116 C115 C120 118.8(7) . . ? C116 C115 C114 118.2(6) . . ? C120 C115 C114 123.0(6) . . ? C117 C116 C115 122.3(8) . . ? C116 C117 C118 119.3(8) . . ? C119 C118 C117 120.5(8) . . ? C118 C119 C120 122.2(8) . . ? O102 C120 C119 121.4(6) . . ? O102 C120 C115 121.5(6) . . ? C119 C120 C115 116.9(6) . . ? O102 C120 K7 51.7(3) . . ? C119 C120 K7 104.6(4) . . ? C115 C120 K7 109.1(4) . . ? C121 N121 C125 114.3(9) . . ? C121 N121 K1 103.8(6) . . ? C125 N121 K1 140.3(7) . . ? C122 C121 N121 124.2(10) . . ? C123 C122 C121 119.9(12) . . ? C122 C123 C124 119.3(13) . . ? C125 C124 C123 117.0(12) . . ? C124 C125 N121 125.2(12) . . ? C130 N122 C126 115.4(8) . . ? C130 N122 K3 118.8(6) . . ? C126 N122 K3 118.1(6) . . ? N122 C126 C127 122.2(9) . . ? C128 C127 C126 120.3(9) . . ? C129 C128 C127 118.3(9) . . ? C128 C129 C130 119.7(10) . . ? N122 C130 C129 124.1(9) . . ? C135 N123 C131 117.0(8) . . ? C135 N123 K3 109.9(5) . . ? C131 N123 K3 132.1(7) . . ? N123 C131 C132 124.8(10) . . ? C131 C132 C133 118.2(10) . . ? C132 C133 C134 117.6(10) . . ? C135 C134 C133 119.2(11) . . ? N123 C135 C134 123.1(9) . . ? C136 N124 C140 120.0 . . ? C136 N124 K4 113.53(16) . . ? C140 N124 K4 124.59(16) . . ? N124 C136 C137 120.0 . . ? C138 C137 C136 120.0 . . ? C137 C138 C139 120.0 . . ? C138 C139 C140 120.0 . . ? C139 C140 N124 120.0 . . ? C145 N125 C141 114.6(10) . . ? C145 N125 K6 113.2(8) . . ? C141 N125 K6 130.5(7) . . ? N125 C141 C142 124.2(11) . . ? C141 C142 C143 118.2(13) . . ? C142 C143 C144 117.7(12) . . ? C145 C144 C143 116.7(13) . . ? N125 C145 C144 128.4(13) . . ? C146 N126 C150 112.3(14) . . ? C146 N126 C50B 111.4(12) . . ? C150 N126 C50B 47.8(14) . . ? C146 N126 K6 121.7(7) . . ? C150 N126 K6 110.8(11) . . ? C50B N126 K6 126.5(10) . . ? N126 C146 C147 127.6(11) . . ? C148 C147 C146 116.9(15) . . ? C148 C147 C48B 53.0(14) . . ? C146 C147 C48B 111.7(14) . . ? C147 C148 C149 118(2) . . ? C150 C149 C148 119(2) . . ? N126 C150 C149 120(2) . . ? C147 C48B C49B 118.4(19) . . ? C50B C49B C48B 118(2) . . ? C49B C50B N126 123(2) . . ? C55B N127 C151 110.0(9) . . ? C55B N127 C155 43.8(8) . . ? C151 N127 C155 116.5(12) . . ? C55B N127 K6 124.0(7) . . ? C151 N127 K6 116.6(9) . . ? C155 N127 K6 124.9(9) . . ? N127 C151 C152 124.1(13) . . ? C53B C152 C151 115(2) . . ? C53B C152 C153 25.5(12) . . ? C151 C152 C153 118.5(16) . . ? C154 C153 C152 120(2) . . ? C155 C154 C153 122(2) . . ? C154 C155 N127 117.1(16) . . ? C54B C53B C152 116(3) . . ? C53B C54B C55B 123(3) . . ? N127 C55B C54B 123.6(13) . . ? C156 N128 C160 120.0 . . ? C156 N128 K7 111.2(2) . . ? C160 N128 K7 128.8(2) . . ? N128 C156 C157 120.0 . . ? N128 C156 K7 46.79(14) . . ? C157 C156 K7 166.75(14) . . ? C156 C157 C158 120.0 . . ? C159 C158 C157 120.0 . . ? C158 C159 C160 120.0 . . ? C159 C160 N128 120.0 . . ? C161 N129 C165 116.7(11) . . ? C161 N129 K9 117.1(9) . . ? C165 N129 K9 125.3(7) . . ? N129 C161 C162 125.2(13) . . ? N129 C161 K9 43.6(8) . . ? C162 C161 K9 168.2(9) . . ? C163 C162 C161 119.3(14) . . ? C164 C163 C162 114.5(14) . . ? C163 C164 C165 125.9(12) . . ? C164 C165 N129 118.1(9) . . ? C170 N130 C166 120.0 . . ? C170 N130 K9B 132.3(2) . . ? C166 N130 K9B 100.8(2) . . ? C170 N130 K9 114.23(14) . . ? C166 N130 K9 125.47(14) . . ? K9B N130 K9 38.2(3) . . ? C167 C166 N130 120.0 . . ? C167 C166 K9B 157.6(2) . . ? N130 C166 K9B 52.81(19) . . ? C166 C167 C168 120.0 . . ? C169 C168 C167 120.0 . . ? C168 C169 C170 120.0 . . ? N130 C170 C169 120.0 . . ? C175 N131 C171 116(2) . . ? N131 C171 C172 117(2) . . ? C173 C172 C171 122(2) . . ? C172 C173 C174 119(2) . . ? C175 C174 C173 118(2) . . ? N131 C175 C174 127(2) . . ? C180 N132 C176 118.1(11) . . ? C177 C176 N132 121.6(12) . . ? C176 C177 C178 121.1(13) . . ? C177 C178 C179 118.8(13) . . ? C178 C179 C180 118.1(11) . . ? N132 C180 C179 122.2(11) . . ? C181 N133 C185 120.0 . . ? C182 C181 N133 120.0 . . ? C183 C182 C181 120.0 . . ? C182 C183 C184 120.0 . . ? C183 C184 C185 120.0 . . ? C184 C185 N133 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.026 _refine_diff_density_min -1.830 _refine_diff_density_rms 0.118 # Attachment '- 4.cif' data_cc156 _database_code_depnum_ccdc_archive 'CCDC 877722' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H53 K3 N9 O4 Tb' _chemical_formula_weight 1300.38 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' Tb Tb -0.1723 4.1537 '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 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.5693(13) _cell_length_b 30.262(3) _cell_length_c 14.6011(13) _cell_angle_alpha 90.00 _cell_angle_beta 108.494(9) _cell_angle_gamma 90.00 _cell_volume 6105.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3853 _cell_measurement_theta_min 3.4355 _cell_measurement_theta_max 32.2991 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 1.418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5955 _exptl_absorpt_correction_T_max 0.8208 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21589 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.1307 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 24.71 _reflns_number_total 10290 _reflns_number_gt 6348 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 55.00 93.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 25.4051 179.0000 -180.0000 38 #__ type_ start__ end____ width___ exp.time_ 2 omega -45.00 80.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 25.4051 0.0000 -60.0000 125 #__ type_ start__ end____ width___ exp.time_ 3 omega 50.00 78.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 25.4051 -140.0000 -108.0000 28 #__ type_ start__ end____ width___ exp.time_ 4 omega -26.00 11.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -18.7957 -77.0000 -90.0000 37 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0820P)^2^+102.2443P] 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 10290 _refine_ls_number_parameters 723 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1479 _refine_ls_R_factor_gt 0.1004 _refine_ls_wR_factor_ref 0.2722 _refine_ls_wR_factor_gt 0.2392 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.064 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.48450(5) 0.74697(2) 0.37482(5) 0.0316(2) Uani 1 1 d . . . K1 K 0.5528(3) 0.86240(11) 0.3308(3) 0.0529(9) Uani 1 1 d . . . K2 K 0.2749(2) 0.67952(12) 0.4301(3) 0.0489(8) Uani 1 1 d . . . K3 K 0.5283(2) 0.74176(11) 0.64247(19) 0.0422(8) Uani 1 1 d . . . O1 O 0.4134(6) 0.7964(3) 0.2473(5) 0.0287(19) Uani 1 1 d . . . O2 O 0.4639(6) 0.6884(3) 0.4776(6) 0.036(2) Uani 1 1 d . . . N1 N 0.4021(7) 0.7012(4) 0.2241(7) 0.030(2) Uani 1 1 d . . . N2 N 0.5743(7) 0.6861(4) 0.3530(7) 0.032(2) Uani 1 1 d . . . C1 C 0.3249(9) 0.7959(5) 0.1900(10) 0.035(3) Uani 1 1 d . . . C2 C 0.2743(9) 0.8342(5) 0.1623(9) 0.037(3) Uani 1 1 d . . . H2 H 0.3071 0.8611 0.1855 0.045 Uiso 1 1 calc R A . C3 C 0.1815(11) 0.8370(5) 0.1046(10) 0.046(4) Uani 1 1 d . . . H3 H 0.1475 0.8643 0.0965 0.055 Uiso 1 1 calc R . . C4 C 0.1358(11) 0.7982(6) 0.0562(11) 0.056(4) Uani 1 1 d . . . H4 H 0.0717 0.7995 0.0124 0.067 Uiso 1 1 calc R A . C5 C 0.1860(9) 0.7585(6) 0.0738(11) 0.048(4) Uani 1 1 d . . . H5 H 0.1560 0.7325 0.0411 0.058 Uiso 1 1 calc R . . C6 C 0.2807(9) 0.7560(4) 0.1393(10) 0.033(3) Uani 1 1 d . . . C7 C 0.3243(10) 0.7126(5) 0.1555(10) 0.042(3) Uani 1 1 d . . . H7 H 0.2927 0.6901 0.1115 0.051 Uiso 1 1 calc R . . C8 C 0.4399(9) 0.6574(5) 0.2302(9) 0.034(3) Uani 1 1 d . A . C9 C 0.3902(11) 0.6221(5) 0.1729(12) 0.050(4) Uani 1 1 d . . . H9 H 0.3290 0.6273 0.1259 0.061 Uiso 1 1 calc R A . C10 C 0.4295(12) 0.5797(5) 0.1842(11) 0.054(4) Uani 1 1 d . A . H10 H 0.3966 0.5561 0.1442 0.065 Uiso 1 1 calc R . . C11 C 0.5169(12) 0.5727(5) 0.2543(11) 0.052(4) Uani 1 1 d . . . H11 H 0.5450 0.5441 0.2618 0.063 Uiso 1 1 calc R A . C12 C 0.5640(9) 0.6062(5) 0.3133(10) 0.038(3) Uani 1 1 d . A . H12 H 0.6221 0.5994 0.3636 0.045 Uiso 1 1 calc R . . C13 C 0.5314(9) 0.6494(5) 0.3035(9) 0.035(3) Uani 1 1 d . A . C14 C 0.6539(9) 0.6772(4) 0.4420(9) 0.031(3) Uani 1 1 d . A . H14 H 0.7032 0.6589 0.4248 0.037 Uiso 1 1 calc R . . C15 C 0.6197(9) 0.6511(4) 0.5155(9) 0.034(3) Uani 1 1 d . . . C16 C 0.6827(11) 0.6202(5) 0.5713(10) 0.043(4) Uani 1 1 d . A . H16 H 0.7456 0.6174 0.5657 0.051 Uiso 1 1 calc R . . C17 C 0.6559(11) 0.5932(5) 0.6354(11) 0.052(4) Uani 1 1 d . . . H17 H 0.6999 0.5721 0.6737 0.062 Uiso 1 1 calc R A . C18 C 0.5650(11) 0.5975(5) 0.6422(10) 0.046(4) Uani 1 1 d . . . H18 H 0.5436 0.5782 0.6826 0.055 Uiso 1 1 calc R . . C19 C 0.5037(10) 0.6304(5) 0.5896(9) 0.037(3) Uani 1 1 d . . . H19 H 0.4424 0.6340 0.5988 0.045 Uiso 1 1 calc R A . C20 C 0.5273(9) 0.6585(4) 0.5240(8) 0.031(3) Uani 1 1 d . . . O21 O 0.3339(7) 0.7563(3) 0.3930(7) 0.043(2) Uani 1 1 d . . . O22 O 0.6061(6) 0.7821(3) 0.3219(6) 0.031(2) Uani 1 1 d . . . N21 N 0.4940(8) 0.8123(4) 0.4876(7) 0.034(3) Uani 1 1 d . . . N22 N 0.6314(7) 0.7505(4) 0.5058(7) 0.031(2) Uani 1 1 d . . . C21 C 0.2833(10) 0.7924(5) 0.3874(10) 0.042(4) Uani 1 1 d . . . C22 C 0.1811(10) 0.7903(6) 0.3412(11) 0.049(4) Uani 1 1 d . . . H22 H 0.1514 0.7631 0.3156 0.059 Uiso 1 1 calc R A . C23 C 0.1257(12) 0.8278(7) 0.3340(14) 0.066(5) Uani 1 1 d . A . H23 H 0.0575 0.8256 0.3050 0.080 Uiso 1 1 calc R . . C24 C 0.1656(12) 0.8688(6) 0.3676(13) 0.064(5) Uani 1 1 d . . . H24 H 0.1261 0.8944 0.3603 0.077 Uiso 1 1 calc R A . C25 C 0.2632(11) 0.8710(5) 0.4114(11) 0.051(4) Uani 1 1 d . A . H25 H 0.2916 0.8987 0.4354 0.061 Uiso 1 1 calc R . . C26 C 0.3231(11) 0.8339(5) 0.4221(10) 0.042(3) Uani 1 1 d . . . C27 C 0.4236(10) 0.8392(5) 0.4743(10) 0.043(4) Uani 1 1 d . . . H27 H 0.4407 0.8672 0.5040 0.052 Uiso 1 1 calc R . . C28 C 0.5900(10) 0.8217(6) 0.5461(10) 0.050(4) Uani 1 1 d . . . C29 C 0.6147(11) 0.8598(6) 0.6035(11) 0.056(4) Uani 1 1 d . . . H29 H 0.5660 0.8805 0.6045 0.067 Uiso 1 1 calc R A . C30 C 0.7087(13) 0.8671(7) 0.6579(16) 0.087(7) Uani 1 1 d . A . H30 H 0.7252 0.8932 0.6959 0.105 Uiso 1 1 calc R . . C31 C 0.7812(12) 0.8364(6) 0.6582(15) 0.079(6) Uani 1 1 d . . . H31 H 0.8467 0.8418 0.6951 0.094 Uiso 1 1 calc R A . C32 C 0.7561(11) 0.7995(6) 0.6054(11) 0.055(4) Uani 1 1 d . . . H32 H 0.8058 0.7793 0.6047 0.065 Uiso 1 1 calc R . . C33 C 0.6624(9) 0.7892(5) 0.5523(9) 0.036(3) Uani 1 1 d . . . C34 C 0.7022(9) 0.7222(4) 0.4834(9) 0.033(3) Uani 1 1 d . . . H34 H 0.7538 0.7157 0.5457 0.039 Uiso 1 1 calc R A . C35 C 0.7522(9) 0.7450(4) 0.4161(9) 0.033(3) Uani 1 1 d . . . C36 C 0.8470(10) 0.7379(5) 0.4303(10) 0.044(4) Uani 1 1 d . . . H36 H 0.8816 0.7194 0.4823 0.053 Uiso 1 1 calc R A . C37 C 0.8978(10) 0.7568(6) 0.3712(11) 0.054(4) Uani 1 1 d . A . H37 H 0.9643 0.7508 0.3814 0.064 Uiso 1 1 calc R . . C38 C 0.8452(10) 0.7843(6) 0.2984(11) 0.049(4) Uani 1 1 d . . . H38 H 0.8761 0.7979 0.2574 0.059 Uiso 1 1 calc R A . C39 C 0.7485(9) 0.7926(6) 0.2838(10) 0.046(4) Uani 1 1 d . . . H39 H 0.7152 0.8120 0.2330 0.055 Uiso 1 1 calc R . . C40 C 0.6970(7) 0.7736(3) 0.3405(7) 0.031(3) Uani 1 1 d . . . N41 N 0.4352(7) 0.9412(3) 0.3109(7) 0.079(5) Uani 1 1 d R . . N42 N 0.6997(8) 0.9259(3) 0.4025(8) 0.087(5) Uani 1 1 d . . . C41 C 0.3592(8) 0.9524(3) 0.2297(8) 0.086(6) Uani 1 1 d R A . H41 H 0.3557 0.9408 0.1682 0.104 Uiso 1 1 calc R . . C42 C 0.2880(8) 0.9810(3) 0.2392(8) 0.133(12) Uani 1 1 d R . . H42 H 0.2350 0.9887 0.1841 0.160 Uiso 1 1 calc R . . C43 C 0.2944(8) 0.9982(3) 0.3292(8) 0.166(18) Uani 1 1 d R A . H43 H 0.2457 1.0177 0.3357 0.199 Uiso 1 1 calc R . . C44 C 0.3719(8) 0.9869(3) 0.4097(8) 0.135(13) Uani 1 1 d R . . H44 H 0.3762 0.9987 0.4712 0.162 Uiso 1 1 calc R . . C45 C 0.4431(8) 0.9584(3) 0.4002(8) 0.124(10) Uani 1 1 d R A . H45 H 0.4966 0.9509 0.4549 0.149 Uiso 1 1 calc R . . C46 C 0.7008(15) 0.9675(7) 0.3692(17) 0.083(6) Uani 1 1 d . A . H46 H 0.6471 0.9766 0.3163 0.100 Uiso 1 1 calc R . . C47 C 0.7732(19) 0.9973(10) 0.406(3) 0.164(14) Uani 1 1 d U . . H47 H 0.7718 1.0252 0.3758 0.196 Uiso 1 1 calc R A . C48 C 0.850(2) 0.9862(13) 0.488(3) 0.166(14) Uani 1 1 d U A . H48 H 0.8984 1.0069 0.5196 0.200 Uiso 1 1 calc R . . C49 C 0.850(2) 0.9397(13) 0.525(2) 0.139(10) Uani 1 1 d U . . H49 H 0.9020 0.9289 0.5776 0.167 Uiso 1 1 calc R A . C50 C 0.771(2) 0.9133(11) 0.4775(19) 0.125(9) Uani 1 1 d U A . H50 H 0.7684 0.8843 0.5015 0.150 Uiso 1 1 calc R . . N51 N 0.1236(10) 0.6643(6) 0.2460(10) 0.065(4) Uani 1 1 d . A . C51 C 0.1557(14) 0.6339(7) 0.1974(14) 0.078(6) Uani 1 1 d . . . H51 H 0.2097 0.6165 0.2326 0.094 Uiso 1 1 calc R A . C52 C 0.1169(15) 0.6259(7) 0.1022(14) 0.077(6) Uani 1 1 d . A . H52 H 0.1455 0.6044 0.0723 0.092 Uiso 1 1 calc R . . C53 C 0.0359(14) 0.6487(7) 0.0475(15) 0.076(6) Uani 1 1 d . . . H53 H 0.0059 0.6428 -0.0192 0.092 Uiso 1 1 calc R A . C54 C 0.0018(13) 0.6798(7) 0.0942(14) 0.070(5) Uani 1 1 d . A . H54 H -0.0532 0.6971 0.0615 0.084 Uiso 1 1 calc R . . C55 C 0.0512(6) 0.6858(3) 0.1945(6) 0.067(5) Uani 1 1 d . . . H55 H 0.0272 0.7083 0.2261 0.080 Uiso 1 1 calc R A . N52 N 0.2901(6) 0.5802(3) 0.4300(6) 0.072(15) Uani 0.50 1 d PR A 1 C56 C 0.3743(6) 0.5736(3) 0.4063(6) 0.063(13) Uani 0.50 1 d PR A 1 H56 H 0.3971 0.5960 0.3734 0.076 Uiso 0.50 1 calc PR B 1 C57 C 0.4252(6) 0.5342(3) 0.4310(6) 0.057(9) Uani 0.50 1 d PR A 1 H57 H 0.4828 0.5297 0.4148 0.069 Uiso 0.50 1 calc PR C 1 C58 C 0.3919(6) 0.5014(3) 0.4792(6) 0.076(13) Uani 0.50 1 d PR A 1 H58 H 0.4267 0.4744 0.4960 0.091 Uiso 0.50 1 calc PR D 1 C59 C 0.3077(6) 0.5080(3) 0.5028(6) 0.080(14) Uani 0.50 1 d PR A 1 H59 H 0.2849 0.4855 0.5357 0.096 Uiso 0.50 1 calc PR E 1 C60 C 0.2567(6) 0.5474(3) 0.4782(6) 0.088(14) Uani 0.50 1 d PR A 1 H60 H 0.1992 0.5519 0.4943 0.106 Uiso 0.50 1 calc PR F 1 N52B N 0.2781(6) 0.5930(3) 0.4260(6) 0.071(13) Uani 0.50 1 d PR A 2 C56B C 0.3467(6) 0.5632(3) 0.4155(6) 0.076(18) Uani 0.50 1 d PR A 2 H56B H 0.4057 0.5737 0.4088 0.091 Uiso 0.50 1 calc PR G 2 C57B C 0.3290(6) 0.5180(3) 0.4148(6) 0.120(19) Uani 0.50 1 d PR A 2 H57B H 0.3759 0.4977 0.4076 0.144 Uiso 0.50 1 calc PR H 2 C58B C 0.2427(6) 0.5026(3) 0.4246(6) 0.18(4) Uani 0.50 1 d PR A 2 H58B H 0.2307 0.4717 0.4240 0.220 Uiso 0.50 1 calc PR I 2 C59B C 0.1742(6) 0.5324(3) 0.4351(6) 0.13(2) Uani 0.50 1 d PR A 2 H59B H 0.1152 0.5218 0.4418 0.150 Uiso 0.50 1 calc PR J 2 C60B C 0.1918(6) 0.5775(3) 0.4358(6) 0.12(2) Uani 0.50 1 d PR A 2 H60B H 0.1449 0.5979 0.4430 0.148 Uiso 0.50 1 calc PR K 2 N61 N -0.0771(6) 0.5458(3) 0.4380(6) 0.111(7) Uani 0.50 1 d PR L 1 C61 C 0.0142(6) 0.5571(3) 0.4345(6) 0.111(7) Uani 0.50 1 d PR L 1 H61 H 0.0668 0.5372 0.4584 0.133 Uiso 0.50 1 calc PR M 1 C62 C 0.0286(6) 0.5975(3) 0.3961(6) 0.111(7) Uani 0.50 1 d PR L 1 H62 H 0.0910 0.6053 0.3937 0.133 Uiso 0.50 1 calc PR N 1 C63 C -0.0484(6) 0.6267(3) 0.3611(6) 0.111(7) Uani 0.50 1 d PR L 1 H63 H -0.0386 0.6543 0.3349 0.133 Uiso 0.50 1 calc PR O 1 C64 C -0.1397(6) 0.6154(3) 0.3646(6) 0.111(7) Uani 0.50 1 d PR L 1 H64 H -0.1923 0.6353 0.3407 0.133 Uiso 0.50 1 calc PR P 1 C65 C -0.1540(6) 0.5749(3) 0.4030(6) 0.111(7) Uani 0.50 1 d PR L 1 H65 H -0.2164 0.5671 0.4054 0.133 Uiso 0.50 1 calc PR Q 1 N62 N 0.9764(6) 0.9634(3) 0.3130(6) 0.116(7) Uani 0.50 1 d PR R 1 C66 C 1.0300(6) 0.9742(3) 0.2526(6) 0.116(7) Uani 0.50 1 d PR R 1 H66 H 1.0739 0.9984 0.2684 0.140 Uiso 0.50 1 calc PR S 1 C67 C 1.0193(6) 0.9498(3) 0.1693(6) 0.116(7) Uani 0.50 1 d PR R 1 H67 H 1.0559 0.9572 0.1280 0.140 Uiso 0.50 1 calc PR T 1 C68 C 0.9550(6) 0.9145(3) 0.1463(6) 0.116(7) Uani 0.50 1 d PR R 1 H68 H 0.9477 0.8978 0.0893 0.140 Uiso 0.50 1 calc PR U 1 C69 C 0.9014(6) 0.9036(3) 0.2067(6) 0.116(7) Uani 0.50 1 d PR R 1 H69 H 0.8574 0.8795 0.1909 0.140 Uiso 0.50 1 calc PR V 1 C70 C 0.9121(6) 0.9281(3) 0.2900(6) 0.116(7) Uani 0.50 1 d PR R 1 H70 H 0.8754 0.9206 0.3313 0.140 Uiso 0.50 1 calc PR W 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 Tb1 0.0307(4) 0.0428(4) 0.0241(3) 0.0017(3) 0.0127(2) 0.0028(3) K1 0.072(2) 0.0376(19) 0.053(2) 0.0001(15) 0.0249(18) 0.0026(17) K2 0.0395(19) 0.046(2) 0.061(2) 0.0050(16) 0.0149(15) 0.0047(15) K3 0.0529(19) 0.055(2) 0.0204(15) 0.0068(13) 0.0141(13) 0.0111(15) O1 0.032(5) 0.034(5) 0.018(4) 0.005(3) 0.005(3) 0.004(4) O2 0.038(5) 0.041(6) 0.031(5) 0.003(4) 0.011(4) 0.009(4) N1 0.031(6) 0.035(7) 0.023(5) 0.007(4) 0.005(4) 0.000(5) N2 0.030(6) 0.028(6) 0.037(6) 0.001(5) 0.010(5) -0.004(5) C1 0.021(7) 0.036(8) 0.047(8) 0.007(6) 0.010(6) -0.002(6) C2 0.028(7) 0.038(8) 0.041(8) 0.018(6) 0.003(6) -0.011(6) C3 0.048(9) 0.044(9) 0.047(9) 0.011(7) 0.018(7) 0.008(7) C4 0.035(9) 0.072(13) 0.055(10) 0.013(9) 0.006(7) -0.002(8) C5 0.022(7) 0.068(12) 0.049(9) 0.008(8) 0.003(6) -0.007(7) C6 0.026(7) 0.036(8) 0.042(8) 0.000(6) 0.016(5) -0.004(6) C7 0.040(8) 0.037(8) 0.047(9) -0.008(6) 0.009(7) -0.008(7) C8 0.031(7) 0.041(8) 0.030(7) -0.007(6) 0.013(5) -0.011(6) C9 0.041(9) 0.029(8) 0.076(11) 0.021(7) 0.010(7) -0.009(7) C10 0.074(12) 0.041(10) 0.044(9) -0.002(7) 0.014(8) -0.020(8) C11 0.065(11) 0.039(9) 0.060(11) 0.011(8) 0.031(9) 0.008(8) C12 0.024(7) 0.045(9) 0.041(8) 0.003(6) 0.007(6) 0.000(6) C13 0.030(7) 0.043(9) 0.042(8) -0.020(6) 0.024(6) -0.016(6) C14 0.034(7) 0.029(7) 0.029(7) -0.001(5) 0.011(5) 0.014(6) C15 0.022(7) 0.034(8) 0.041(8) -0.003(6) 0.005(5) 0.001(6) C16 0.045(9) 0.042(9) 0.046(9) 0.004(7) 0.021(7) 0.017(7) C17 0.054(10) 0.054(10) 0.047(9) 0.007(7) 0.016(7) 0.021(8) C18 0.049(9) 0.045(9) 0.042(9) 0.010(7) 0.011(7) 0.007(7) C19 0.039(8) 0.037(8) 0.036(8) -0.005(6) 0.012(6) 0.005(6) C20 0.038(8) 0.032(7) 0.021(7) -0.004(5) 0.004(5) 0.005(6) O21 0.041(6) 0.057(7) 0.038(6) 0.005(5) 0.022(4) 0.005(5) O22 0.027(5) 0.033(5) 0.034(5) 0.003(4) 0.010(4) 0.005(4) N21 0.035(6) 0.035(6) 0.031(6) 0.004(5) 0.011(5) 0.008(5) N22 0.027(5) 0.038(7) 0.027(6) -0.001(5) 0.005(4) 0.005(5) C21 0.034(8) 0.055(10) 0.042(8) 0.012(7) 0.021(6) 0.013(7) C22 0.038(9) 0.053(10) 0.057(10) 0.002(8) 0.017(7) 0.001(7) C23 0.036(9) 0.080(14) 0.086(13) 0.008(11) 0.023(9) 0.017(9) C24 0.038(10) 0.064(13) 0.085(13) -0.009(10) 0.012(8) 0.018(9) C25 0.049(10) 0.041(9) 0.062(10) 0.001(7) 0.016(8) 0.011(7) C26 0.050(9) 0.031(8) 0.044(8) 0.003(6) 0.016(7) 0.018(7) C27 0.038(8) 0.051(10) 0.041(8) 0.003(7) 0.013(6) 0.011(7) C28 0.033(8) 0.079(12) 0.035(8) -0.020(8) 0.008(6) -0.009(8) C29 0.044(9) 0.062(11) 0.062(11) -0.031(9) 0.018(8) 0.006(8) C30 0.056(12) 0.070(14) 0.132(19) -0.058(13) 0.024(12) -0.006(10) C31 0.041(10) 0.072(14) 0.109(16) -0.046(12) 0.005(10) 0.011(9) C32 0.041(9) 0.068(12) 0.053(10) -0.028(8) 0.013(7) 0.005(8) C33 0.025(7) 0.056(10) 0.020(7) 0.010(6) -0.005(5) 0.007(6) C34 0.035(7) 0.035(8) 0.026(7) 0.001(5) 0.006(5) 0.005(6) C35 0.029(7) 0.039(8) 0.028(7) -0.008(6) 0.003(5) -0.004(6) C36 0.029(8) 0.058(10) 0.042(8) 0.001(7) 0.009(6) 0.008(7) C37 0.025(8) 0.081(13) 0.051(10) -0.006(8) 0.007(6) 0.004(8) C38 0.039(9) 0.063(11) 0.046(9) -0.003(7) 0.016(7) -0.013(8) C39 0.027(8) 0.070(11) 0.037(8) -0.006(7) 0.005(6) 0.008(7) C40 0.023(7) 0.028(7) 0.039(8) 0.005(6) 0.005(5) 0.000(6) N41 0.095(13) 0.061(11) 0.094(13) 0.001(9) 0.049(11) 0.015(9) N42 0.081(12) 0.069(12) 0.084(12) -0.016(9) -0.012(9) 0.006(10) C41 0.082(15) 0.063(14) 0.119(19) 0.017(13) 0.039(14) 0.002(12) C42 0.078(17) 0.11(2) 0.22(4) 0.07(2) 0.07(2) 0.024(16) C43 0.18(3) 0.12(3) 0.28(5) 0.08(3) 0.19(4) 0.05(2) C44 0.20(3) 0.074(19) 0.18(3) -0.018(19) 0.14(3) 0.00(2) C45 0.17(3) 0.09(2) 0.15(3) -0.013(18) 0.10(2) 0.003(19) C46 0.065(13) 0.054(13) 0.115(18) -0.020(12) 0.006(11) 0.003(10) C47 0.067(17) 0.078(18) 0.33(5) -0.03(2) 0.04(2) -0.008(15) C48 0.086(19) 0.17(2) 0.24(4) -0.10(3) 0.050(18) -0.02(2) C49 0.090(18) 0.21(3) 0.11(2) -0.052(19) 0.026(15) 0.024(19) C50 0.12(2) 0.15(2) 0.10(2) -0.007(18) 0.025(16) 0.009(17) N51 0.046(9) 0.083(12) 0.059(9) -0.004(8) 0.007(7) 0.001(8) C51 0.067(13) 0.092(17) 0.067(14) 0.016(11) 0.009(10) 0.008(11) C52 0.075(14) 0.092(16) 0.062(13) 0.002(11) 0.019(10) 0.010(12) C53 0.060(13) 0.087(16) 0.077(14) -0.009(12) 0.015(10) -0.017(11) C54 0.053(11) 0.073(14) 0.079(14) 0.030(10) 0.013(10) 0.001(10) C55 0.056(12) 0.064(12) 0.081(14) 0.000(10) 0.022(10) -0.009(10) N52 0.10(4) 0.03(2) 0.07(3) -0.010(15) 0.01(3) -0.04(2) C56 0.10(3) 0.03(2) 0.07(3) 0.005(18) 0.04(2) 0.01(2) C57 0.09(3) 0.031(18) 0.05(2) -0.002(15) 0.027(19) 0.004(18) C58 0.08(3) 0.06(2) 0.06(2) -0.030(19) -0.01(2) 0.03(2) C59 0.07(3) 0.04(2) 0.12(4) 0.02(2) 0.01(2) 0.00(2) C60 0.08(3) 0.08(3) 0.11(4) 0.00(3) 0.04(3) -0.03(3) N52B 0.06(3) 0.06(2) 0.09(3) 0.02(2) 0.02(2) 0.00(2) C56B 0.12(4) 0.03(2) 0.05(3) -0.011(19) -0.01(3) -0.04(3) C57B 0.13(5) 0.07(4) 0.16(6) -0.04(4) 0.05(4) 0.00(4) C58B 0.20(8) 0.11(6) 0.31(11) 0.11(6) 0.19(8) 0.06(5) C59B 0.16(5) 0.12(4) 0.14(4) -0.04(3) 0.10(4) -0.11(4) C60B 0.16(6) 0.09(4) 0.15(5) -0.06(4) 0.10(4) -0.07(4) N61 0.100(15) 0.097(16) 0.152(18) 0.018(13) 0.064(14) 0.011(12) C61 0.100(15) 0.097(16) 0.152(18) 0.018(13) 0.064(14) 0.011(12) C62 0.100(15) 0.097(16) 0.152(18) 0.018(13) 0.064(14) 0.011(12) C63 0.100(15) 0.097(16) 0.152(18) 0.018(13) 0.064(14) 0.011(12) C64 0.100(15) 0.097(16) 0.152(18) 0.018(13) 0.064(14) 0.011(12) C65 0.100(15) 0.097(16) 0.152(18) 0.018(13) 0.064(14) 0.011(12) N62 0.079(14) 0.12(2) 0.15(2) -0.024(14) 0.050(13) -0.012(11) C66 0.079(14) 0.12(2) 0.15(2) -0.024(14) 0.050(13) -0.012(11) C67 0.079(14) 0.12(2) 0.15(2) -0.024(14) 0.050(13) -0.012(11) C68 0.079(14) 0.12(2) 0.15(2) -0.024(14) 0.050(13) -0.012(11) C69 0.079(14) 0.12(2) 0.15(2) -0.024(14) 0.050(13) -0.012(11) C70 0.079(14) 0.12(2) 0.15(2) -0.024(14) 0.050(13) -0.012(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O21 2.310(9) . ? Tb1 N2 2.338(11) . ? Tb1 O1 2.357(8) . ? Tb1 N22 2.377(10) . ? Tb1 O22 2.393(8) . ? Tb1 O2 2.403(9) . ? Tb1 N21 2.549(11) . ? Tb1 N1 2.555(10) . ? Tb1 K3 3.662(3) 4_575 ? Tb1 K1 3.743(4) . ? Tb1 K3 3.758(3) . ? Tb1 K2 3.963(3) . ? K1 O22 2.568(9) . ? K1 N42 2.820(10) . ? K1 O1 2.834(9) . ? K1 N41 2.895(11) . ? K1 C18 3.066(15) 4_575 ? K1 N21 3.084(11) . ? K1 C28 3.256(16) . ? K1 C27 3.306(14) . ? K1 C19 3.372(13) 4_575 ? K1 C40 3.386(11) . ? K1 K3 4.124(5) 4_575 ? K2 O21 2.592(10) . ? K2 N52B 2.621(10) . ? K2 O2 2.631(9) . ? K2 N51 2.922(14) . ? K2 N52 3.015(10) . ? K2 C4 3.213(16) 4_576 ? K2 C3 3.285(15) 4_576 ? K2 C60B 3.326(9) . ? K2 C5 3.366(15) 4_576 ? K2 C2 3.418(14) 4_576 ? K2 C21 3.482(16) . ? K3 O22 2.605(9) 4_576 ? K3 O2 2.802(9) . ? K3 O1 2.847(8) 4_576 ? K3 N22 2.865(11) . ? K3 N1 3.029(10) 4_576 ? K3 N21 3.034(11) . ? K3 C33 3.040(14) . ? K3 C20 3.054(13) . ? K3 C28 3.073(18) . ? K3 C40 3.179(11) 4_576 ? K3 C7 3.338(14) 4_576 ? K3 C39 3.380(14) 4_576 ? O1 C1 1.295(15) . ? O1 K3 2.847(8) 4_575 ? O2 C20 1.316(15) . ? N1 C7 1.300(17) . ? N1 C8 1.426(17) . ? N1 K3 3.029(10) 4_575 ? N2 C13 1.364(16) . ? N2 C14 1.466(15) . ? C1 C2 1.363(19) . ? C1 C6 1.456(18) . ? C1 K3 3.446(13) 4_575 ? C2 C3 1.351(19) . ? C2 K2 3.418(14) 4_575 ? C3 C4 1.42(2) . ? C3 K2 3.285(15) 4_575 ? C4 C5 1.39(2) . ? C4 K2 3.213(16) 4_575 ? C5 C6 1.410(18) . ? C5 K2 3.366(15) 4_575 ? C6 C7 1.444(19) . ? C7 K3 3.338(14) 4_575 ? C8 C9 1.406(19) . ? C8 C13 1.441(19) . ? C9 C10 1.39(2) . ? C10 C11 1.37(2) . ? C11 C12 1.36(2) . ? C12 C13 1.384(19) . ? C14 C15 1.538(18) . ? C14 C34 1.564(18) . ? C15 C16 1.380(18) . ? C15 C20 1.408(18) . ? C16 C17 1.39(2) . ? C17 C18 1.37(2) . ? C18 C19 1.395(19) . ? C18 K1 3.066(15) 4_576 ? C19 C20 1.402(18) . ? C19 K1 3.372(13) 4_576 ? O21 C21 1.308(17) . ? O22 C40 1.290(12) . ? O22 K3 2.605(9) 4_575 ? N21 C27 1.274(17) . ? N21 C28 1.417(17) . ? N22 C33 1.360(17) . ? N22 C34 1.454(16) . ? C21 C26 1.41(2) . ? C21 C22 1.43(2) . ? C22 C23 1.38(2) . ? C23 C24 1.39(3) . ? C24 C25 1.36(2) . ? C25 C26 1.400(19) . ? C26 C27 1.43(2) . ? C28 C29 1.40(2) . ? C28 C33 1.42(2) . ? C29 C30 1.37(2) . ? C30 C31 1.41(2) . ? C31 C32 1.34(2) . ? C32 C33 1.375(19) . ? C34 C35 1.557(18) . ? C35 C36 1.347(18) . ? C35 C40 1.433(16) . ? C36 C37 1.42(2) . ? C37 C38 1.38(2) . ? C38 C39 1.379(19) . ? C39 C40 1.405(17) . ? C39 K3 3.380(14) 4_575 ? C40 K3 3.179(11) 4_575 ? N41 C45 1.375(14) . ? N41 C41 1.384(14) . ? N42 C50 1.30(3) . ? N42 C46 1.35(2) . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C46 C47 1.36(3) . ? C47 C48 1.40(5) . ? C48 C49 1.50(5) . ? C49 C50 1.39(4) . ? N51 C55 1.264(16) . ? N51 C51 1.33(2) . ? C51 C52 1.35(3) . ? C52 C53 1.38(3) . ? C53 C54 1.34(3) . ? C54 C55 1.42(2) . ? N52 C56 1.3907 . ? N52 C60 1.3910 . ? C56 C57 1.3901 . ? C57 C58 1.3911 . ? C58 C59 1.3904 . ? C59 C60 1.3901 . ? N52B C56B 1.3895 . ? N52B C60B 1.3898 . ? C56B C57B 1.3909 . ? C57B C58B 1.3894 . ? C58B C59B 1.3896 . ? C59B C60B 1.3909 . ? N61 C61 1.3900 . ? N61 C65 1.3900 . ? C61 C62 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? N62 C66 1.3900 . ? N62 C70 1.3900 . ? C66 C67 1.3900 . ? C67 C68 1.3900 . ? C68 C69 1.3900 . ? C69 C70 1.3900 . ? 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 O21 Tb1 N2 134.8(4) . . ? O21 Tb1 O1 79.5(3) . . ? N2 Tb1 O1 121.1(3) . . ? O21 Tb1 N22 123.2(3) . . ? N2 Tb1 N22 75.2(4) . . ? O1 Tb1 N22 131.7(3) . . ? O21 Tb1 O22 144.1(3) . . ? N2 Tb1 O22 78.6(3) . . ? O1 Tb1 O22 69.4(3) . . ? N22 Tb1 O22 70.8(3) . . ? O21 Tb1 O2 72.9(3) . . ? N2 Tb1 O2 71.9(3) . . ? O1 Tb1 O2 148.4(3) . . ? N22 Tb1 O2 77.8(3) . . ? O22 Tb1 O2 141.3(3) . . ? O21 Tb1 N21 72.0(3) . . ? N2 Tb1 N21 141.3(4) . . ? O1 Tb1 N21 86.4(3) . . ? N22 Tb1 N21 66.1(3) . . ? O22 Tb1 N21 88.3(3) . . ? O2 Tb1 N21 99.3(3) . . ? O21 Tb1 N1 87.8(3) . . ? N2 Tb1 N1 65.5(3) . . ? O1 Tb1 N1 72.3(3) . . ? N22 Tb1 N1 140.7(3) . . ? O22 Tb1 N1 99.0(3) . . ? O2 Tb1 N1 91.1(3) . . ? N21 Tb1 N1 153.1(3) . . ? O21 Tb1 K3 123.1(2) . 4_575 ? N2 Tb1 K3 71.2(3) . 4_575 ? O1 Tb1 K3 51.0(2) . 4_575 ? N22 Tb1 K3 111.3(3) . 4_575 ? O22 Tb1 K3 45.2(2) . 4_575 ? O2 Tb1 K3 137.8(2) . 4_575 ? N21 Tb1 K3 122.4(2) . 4_575 ? N1 Tb1 K3 54.9(2) . 4_575 ? O21 Tb1 K1 102.7(3) . . ? N2 Tb1 K1 121.4(3) . . ? O1 Tb1 K1 49.2(2) . . ? N22 Tb1 K1 82.9(3) . . ? O22 Tb1 K1 42.8(2) . . ? O2 Tb1 K1 152.7(2) . . ? N21 Tb1 K1 54.8(2) . . ? N1 Tb1 K1 115.9(2) . . ? K3 Tb1 K1 67.68(7) 4_575 . ? O21 Tb1 K3 74.9(2) . . ? N2 Tb1 K3 101.0(3) . . ? O1 Tb1 K3 137.3(2) . . ? N22 Tb1 K3 49.7(3) . . ? O22 Tb1 K3 117.1(2) . . ? O2 Tb1 K3 48.2(2) . . ? N21 Tb1 K3 53.4(2) . . ? N1 Tb1 K3 138.7(2) . . ? K3 Tb1 K3 160.97(10) 4_575 . ? K1 Tb1 K3 104.52(8) . . ? O21 Tb1 K2 38.5(3) . . ? N2 Tb1 K2 97.0(3) . . ? O1 Tb1 K2 108.3(2) . . ? N22 Tb1 K2 114.5(3) . . ? O22 Tb1 K2 172.3(2) . . ? O2 Tb1 K2 40.2(2) . . ? N21 Tb1 K2 99.0(2) . . ? N1 Tb1 K2 73.4(2) . . ? K3 Tb1 K2 127.49(7) 4_575 . ? K1 Tb1 K2 141.22(8) . . ? K3 Tb1 K2 69.79(7) . . ? O22 K1 N42 117.3(3) . . ? O22 K1 O1 59.8(3) . . ? N42 K1 O1 175.0(3) . . ? O22 K1 N41 162.3(3) . . ? N42 K1 N41 80.3(3) . . ? O1 K1 N41 102.5(3) . . ? O22 K1 C18 103.0(4) . 4_575 ? N42 K1 C18 79.0(4) . 4_575 ? O1 K1 C18 97.5(3) . 4_575 ? N41 K1 C18 77.6(4) . 4_575 ? O22 K1 N21 74.4(3) . . ? N42 K1 N21 114.6(3) . . ? O1 K1 N21 69.1(3) . . ? N41 K1 N21 100.6(3) . . ? C18 K1 N21 165.9(4) 4_575 . ? O22 K1 C28 74.4(4) . . ? N42 K1 C28 91.5(4) . . ? O1 K1 C28 91.5(3) . . ? N41 K1 C28 108.7(4) . . ? C18 K1 C28 167.7(4) 4_575 . ? N21 K1 C28 25.7(3) . . ? O22 K1 C27 94.2(3) . . ? N42 K1 C27 115.3(4) . . ? O1 K1 C27 69.4(3) . . ? N41 K1 C27 78.5(3) . . ? C18 K1 C27 149.4(4) 4_575 . ? N21 K1 C27 22.7(3) . . ? C28 K1 C27 42.4(3) . . ? O22 K1 C19 88.6(3) . 4_575 ? N42 K1 C19 103.2(3) . 4_575 ? O1 K1 C19 73.1(3) . 4_575 ? N41 K1 C19 85.4(3) . 4_575 ? C18 K1 C19 24.4(3) 4_575 4_575 ? N21 K1 C19 142.2(3) . 4_575 ? C28 K1 C19 161.4(4) . 4_575 ? C27 K1 C19 134.5(4) . 4_575 ? O22 K1 C40 19.5(2) . . ? N42 K1 C40 97.9(3) . . ? O1 K1 C40 79.0(3) . . ? N41 K1 C40 175.5(4) . . ? C18 K1 C40 98.0(4) 4_575 . ? N21 K1 C40 83.9(3) . . ? C28 K1 C40 75.4(3) . . ? C27 K1 C40 106.0(3) . . ? C19 K1 C40 91.0(3) 4_575 . ? O22 K1 Tb1 39.30(19) . . ? N42 K1 Tb1 141.7(3) . . ? O1 K1 Tb1 39.00(16) . . ? N41 K1 Tb1 127.2(2) . . ? C18 K1 Tb1 128.2(3) 4_575 . ? N21 K1 Tb1 42.5(2) . . ? C28 K1 Tb1 56.9(3) . . ? C27 K1 Tb1 57.1(3) . . ? C19 K1 Tb1 105.0(2) 4_575 . ? C40 K1 Tb1 56.45(18) . . ? O22 K1 K3 37.44(19) . 4_575 ? N42 K1 K3 131.6(2) . 4_575 ? O1 K1 K3 43.59(17) . 4_575 ? N41 K1 K3 129.7(2) . 4_575 ? C18 K1 K3 73.8(3) 4_575 4_575 ? N21 K1 K3 97.7(2) . 4_575 ? C28 K1 K3 107.9(3) . 4_575 ? C27 K1 K3 108.3(3) . 4_575 ? C19 K1 K3 53.7(2) 4_575 4_575 ? C40 K1 K3 48.88(19) . 4_575 ? Tb1 K1 K3 55.22(6) . 4_575 ? O21 K2 N52B 151.8(3) . . ? O21 K2 O2 64.9(3) . . ? N52B K2 O2 94.8(3) . . ? O21 K2 N51 98.8(4) . . ? N52B K2 N51 80.5(4) . . ? O2 K2 N51 132.8(4) . . ? O21 K2 N52 149.8(3) . . ? N52B K2 N52 3.0 . . ? O2 K2 N52 91.8(3) . . ? N51 K2 N52 82.9(4) . . ? O21 K2 C4 104.1(4) . 4_576 ? N52B K2 C4 104.0(4) . 4_576 ? O2 K2 C4 128.7(4) . 4_576 ? N51 K2 C4 97.5(4) . 4_576 ? N52 K2 C4 105.6(4) . 4_576 ? O21 K2 C3 123.0(4) . 4_576 ? N52B K2 C3 83.1(3) . 4_576 ? O2 K2 C3 117.8(3) . 4_576 ? N51 K2 C3 108.2(4) . 4_576 ? N52 K2 C3 84.1(3) . 4_576 ? C4 K2 C3 25.2(4) 4_576 4_576 ? O21 K2 C60B 169.7(3) . . ? N52B K2 C60B 23.41(8) . . ? O2 K2 C60B 116.5(3) . . ? N51 K2 C60B 72.7(4) . . ? N52 K2 C60B 26.09(8) . . ? C4 K2 C60B 83.1(4) 4_576 . ? C3 K2 C60B 66.2(3) 4_576 . ? O21 K2 C5 81.3(4) . 4_576 ? N52B K2 C5 125.8(4) . 4_576 ? O2 K2 C5 110.9(3) . 4_576 ? N51 K2 C5 109.5(4) . 4_576 ? N52 K2 C5 126.8(4) . 4_576 ? C4 K2 C5 24.2(4) 4_576 4_576 ? C3 K2 C5 42.7(4) 4_576 4_576 ? C60B K2 C5 106.7(3) . 4_576 ? O21 K2 C2 114.9(3) . 4_576 ? N52B K2 C2 84.7(3) . 4_576 ? O2 K2 C2 94.7(3) . 4_576 ? N51 K2 C2 130.9(4) . 4_576 ? N52 K2 C2 84.4(3) . 4_576 ? C4 K2 C2 42.0(4) 4_576 4_576 ? C3 K2 C2 23.1(3) 4_576 4_576 ? C60B K2 C2 75.3(3) . 4_576 ? C5 K2 C2 47.7(4) 4_576 4_576 ? O21 K2 C21 18.4(3) . . ? N52B K2 C21 167.1(3) . . ? O2 K2 C21 81.6(3) . . ? N51 K2 C21 92.8(4) . . ? N52 K2 C21 166.3(3) . . ? C4 K2 C21 87.8(4) 4_576 . ? C3 K2 C21 109.5(4) 4_576 . ? C60B K2 C21 161.6(3) . . ? C5 K2 C21 66.8(4) 4_576 . ? C2 K2 C21 107.9(3) 4_576 . ? O21 K2 Tb1 33.7(2) . . ? N52B K2 Tb1 119.3(2) . . ? O2 K2 Tb1 36.1(2) . . ? N51 K2 Tb1 107.4(3) . . ? N52 K2 Tb1 116.88(19) . . ? C4 K2 Tb1 132.5(3) 4_576 . ? C3 K2 Tb1 140.5(3) 4_576 . ? C60B K2 Tb1 142.48(19) . . ? C5 K2 Tb1 108.3(3) 4_576 . ? C2 K2 Tb1 120.6(2) 4_576 . ? C21 K2 Tb1 52.1(2) . . ? O22 K3 O2 128.7(3) 4_576 . ? O22 K3 O1 59.3(2) 4_576 4_576 ? O2 K3 O1 97.7(3) . 4_576 ? O22 K3 N22 124.7(3) 4_576 . ? O2 K3 N22 64.0(3) . . ? O1 K3 N22 159.9(3) 4_576 . ? O22 K3 N1 83.5(3) 4_576 4_576 ? O2 K3 N1 126.0(3) . 4_576 ? O1 K3 N1 59.1(3) 4_576 4_576 ? N22 K3 N1 137.7(3) . 4_576 ? O22 K3 N21 149.4(3) 4_576 . ? O2 K3 N21 80.5(3) . . ? O1 K3 N21 134.4(3) 4_576 . ? N22 K3 N21 54.2(3) . . ? N1 K3 N21 85.1(3) 4_576 . ? O22 K3 C33 115.6(3) 4_576 . ? O2 K3 C33 89.2(3) . . ? O1 K3 C33 173.0(3) 4_576 . ? N22 K3 C33 26.4(3) . . ? N1 K3 C33 117.0(4) 4_576 . ? N21 K3 C33 47.3(3) . . ? O22 K3 C20 105.3(3) 4_576 . ? O2 K3 C20 25.5(3) . . ? O1 K3 C20 94.1(3) 4_576 . ? N22 K3 C20 65.8(3) . . ? N1 K3 C20 143.0(3) 4_576 . ? N21 K3 C20 100.9(3) . . ? C33 K3 C20 91.9(4) . . ? O22 K3 C28 125.6(3) 4_576 . ? O2 K3 C28 97.3(3) . . ? O1 K3 C28 150.8(4) 4_576 . ? N22 K3 C28 46.7(4) . . ? N1 K3 C28 91.9(4) 4_576 . ? N21 K3 C28 26.8(3) . . ? C33 K3 C28 26.9(4) . . ? C20 K3 C28 109.9(4) . . ? O22 K3 C40 23.2(2) 4_576 4_576 ? O2 K3 C40 130.4(3) . 4_576 ? O1 K3 C40 82.4(2) 4_576 4_576 ? N22 K3 C40 102.9(3) . 4_576 ? N1 K3 C40 96.6(3) 4_576 4_576 ? N21 K3 C40 132.7(3) . 4_576 ? C33 K3 C40 92.6(3) . 4_576 ? C20 K3 C40 105.0(3) . 4_576 ? C28 K3 C40 106.1(3) . 4_576 ? O22 K3 C7 99.7(3) 4_576 4_576 ? O2 K3 C7 103.1(3) . 4_576 ? O1 K3 C7 56.7(3) 4_576 4_576 ? N22 K3 C7 132.5(3) . 4_576 ? N1 K3 C7 22.9(3) 4_576 4_576 ? N21 K3 C7 79.2(3) . 4_576 ? C33 K3 C7 122.4(4) . 4_576 ? C20 K3 C7 121.9(4) . 4_576 ? C28 K3 C7 95.5(4) . 4_576 ? C40 K3 C7 117.0(3) 4_576 4_576 ? O22 K3 C39 43.6(3) 4_576 4_576 ? O2 K3 C39 110.0(3) . 4_576 ? O1 K3 C39 98.8(3) 4_576 4_576 ? N22 K3 C39 81.3(3) . 4_576 ? N1 K3 C39 120.8(3) 4_576 4_576 ? N21 K3 C39 124.9(3) . 4_576 ? C33 K3 C39 78.1(3) . 4_576 ? C20 K3 C39 85.7(4) . 4_576 ? C28 K3 C39 99.4(4) . 4_576 ? C40 K3 C39 24.5(3) 4_576 4_576 ? C7 K3 C39 141.5(4) 4_576 4_576 ? C1 O1 Tb1 127.0(8) . . ? C1 O1 K1 135.8(8) . . ? Tb1 O1 K1 91.8(3) . . ? C1 O1 K3 106.4(7) . 4_575 ? Tb1 O1 K3 88.9(3) . 4_575 ? K1 O1 K3 93.1(3) . 4_575 ? C20 O2 Tb1 128.5(8) . . ? C20 O2 K2 124.8(8) . . ? Tb1 O2 K2 103.8(3) . . ? C20 O2 K3 88.0(7) . . ? Tb1 O2 K3 92.1(3) . . ? K2 O2 K3 108.8(3) . . ? C7 N1 C8 121.4(11) . . ? C7 N1 Tb1 125.1(9) . . ? C8 N1 Tb1 112.6(7) . . ? C7 N1 K3 92.0(8) . 4_575 ? C8 N1 K3 106.5(7) . 4_575 ? Tb1 N1 K3 81.5(3) . 4_575 ? C13 N2 C14 114.9(11) . . ? C13 N2 Tb1 122.1(8) . . ? C14 N2 Tb1 110.1(7) . . ? O1 C1 C2 121.0(13) . . ? O1 C1 C6 121.8(12) . . ? C2 C1 C6 116.3(12) . . ? O1 C1 K3 52.4(6) . 4_575 ? C2 C1 K3 129.8(9) . 4_575 ? C6 C1 K3 83.8(7) . 4_575 ? C3 C2 C1 125.4(14) . . ? C3 C2 K2 72.9(8) . 4_575 ? C1 C2 K2 91.2(9) . 4_575 ? C2 C3 C4 118.5(15) . . ? C2 C3 K2 84.0(9) . 4_575 ? C4 C3 K2 74.5(9) . 4_575 ? C5 C4 C3 119.1(14) . . ? C5 C4 K2 84.1(9) . 4_575 ? C3 C4 K2 80.2(9) . 4_575 ? C4 C5 C6 121.1(15) . . ? C4 C5 K2 71.7(9) . 4_575 ? C6 C5 K2 88.0(8) . 4_575 ? C5 C6 C7 116.4(13) . . ? C5 C6 C1 118.7(13) . . ? C7 C6 C1 124.8(12) . . ? N1 C7 C6 126.9(13) . . ? N1 C7 K3 65.1(7) . 4_575 ? C6 C7 K3 88.2(8) . 4_575 ? C9 C8 N1 123.5(12) . . ? C9 C8 C13 119.7(13) . . ? N1 C8 C13 116.7(11) . . ? C10 C9 C8 120.9(14) . . ? C11 C10 C9 118.6(15) . . ? C12 C11 C10 121.3(15) . . ? C11 C12 C13 123.2(13) . . ? N2 C13 C12 129.1(13) . . ? N2 C13 C8 114.7(13) . . ? C12 C13 C8 116.2(12) . . ? N2 C14 C15 111.9(10) . . ? N2 C14 C34 108.4(10) . . ? C15 C14 C34 112.6(10) . . ? C16 C15 C20 122.1(13) . . ? C16 C15 C14 117.2(11) . . ? C20 C15 C14 120.7(11) . . ? C15 C16 C17 121.3(13) . . ? C18 C17 C16 118.6(14) . . ? C17 C18 C19 119.7(14) . . ? C17 C18 K1 115.9(10) . 4_576 ? C19 C18 K1 90.1(9) . 4_576 ? C18 C19 C20 123.8(13) . . ? C18 C19 K1 65.4(8) . 4_576 ? C20 C19 K1 131.2(9) . 4_576 ? C18 C19 K3 124.9(10) . . ? C20 C19 K3 62.0(7) . . ? K1 C19 K3 74.4(3) 4_576 . ? O2 C20 C19 118.9(12) . . ? O2 C20 C15 126.7(12) . . ? C19 C20 C15 114.3(12) . . ? O2 C20 K3 66.5(6) . . ? C19 C20 K3 94.1(8) . . ? C15 C20 K3 110.3(8) . . ? C21 O21 Tb1 129.2(9) . . ? C21 O21 K2 123.0(8) . . ? Tb1 O21 K2 107.8(4) . . ? C40 O22 Tb1 131.2(7) . . ? C40 O22 K1 118.9(7) . . ? Tb1 O22 K1 97.9(3) . . ? C40 O22 K3 104.3(6) . 4_575 ? Tb1 O22 K3 94.1(3) . 4_575 ? K1 O22 K3 105.7(3) . 4_575 ? C27 N21 C28 123.8(13) . . ? C27 N21 Tb1 121.3(10) . . ? C28 N21 Tb1 112.7(8) . . ? C27 N21 K3 119.7(9) . . ? C28 N21 K3 78.1(8) . . ? Tb1 N21 K3 84.1(3) . . ? C27 N21 K1 88.5(8) . . ? C28 N21 K1 84.0(8) . . ? Tb1 N21 K1 82.7(3) . . ? K3 N21 K1 151.7(4) . . ? C33 N22 C34 118.2(10) . . ? C33 N22 Tb1 120.8(8) . . ? C34 N22 Tb1 108.4(7) . . ? C33 N22 K3 84.0(7) . . ? C34 N22 K3 132.0(8) . . ? Tb1 N22 K3 91.1(3) . . ? O21 C21 C26 124.4(13) . . ? O21 C21 C22 118.3(15) . . ? C26 C21 C22 117.3(14) . . ? O21 C21 K2 38.6(7) . . ? C26 C21 K2 147.6(10) . . ? C22 C21 K2 87.1(10) . . ? C23 C22 C21 119.8(16) . . ? C22 C23 C24 122.6(16) . . ? C25 C24 C23 117.7(16) . . ? C24 C25 C26 122.2(17) . . ? C25 C26 C21 120.3(14) . . ? C25 C26 C27 117.8(15) . . ? C21 C26 C27 121.8(13) . . ? N21 C27 C26 130.5(15) . . ? N21 C27 K1 68.8(7) . . ? C26 C27 K1 112.2(9) . . ? C29 C28 N21 122.8(14) . . ? C29 C28 C33 119.0(13) . . ? N21 C28 C33 118.0(13) . . ? C29 C28 K3 115.5(11) . . ? N21 C28 K3 75.1(8) . . ? C33 C28 K3 75.2(9) . . ? C29 C28 K1 101.4(12) . . ? N21 C28 K1 70.4(7) . . ? C33 C28 K1 102.5(8) . . ? K3 C28 K1 139.1(5) . . ? C30 C29 C28 120.0(15) . . ? C29 C30 C31 120.5(17) . . ? C32 C31 C30 118.8(17) . . ? C31 C32 C33 123.6(15) . . ? N22 C33 C32 126.1(13) . . ? N22 C33 C28 116.3(11) . . ? C32 C33 C28 117.6(14) . . ? N22 C33 K3 69.6(7) . . ? C32 C33 K3 121.5(10) . . ? C28 C33 K3 77.9(9) . . ? N22 C34 C35 112.9(11) . . ? N22 C34 C14 109.5(10) . . ? C35 C34 C14 112.6(10) . . ? C36 C35 C40 120.8(12) . . ? C36 C35 C34 119.6(12) . . ? C40 C35 C34 119.5(10) . . ? C35 C36 C37 123.2(14) . . ? C38 C37 C36 116.2(13) . . ? C37 C38 C39 121.4(14) . . ? C38 C39 C40 123.0(14) . . ? C38 C39 K3 139.8(10) . 4_575 ? C40 C39 K3 69.7(7) . 4_575 ? O22 C40 C39 120.0(10) . . ? O22 C40 C35 124.8(10) . . ? C39 C40 C35 115.3(10) . . ? O22 C40 K3 52.6(5) . 4_575 ? C39 C40 K3 85.8(7) . 4_575 ? C35 C40 K3 134.1(8) . 4_575 ? O22 C40 K1 41.6(5) . . ? C39 C40 K1 95.2(8) . . ? C35 C40 K1 134.5(8) . . ? K3 C40 K1 77.8(2) 4_575 . ? C45 N41 C41 121.5(10) . . ? C45 N41 K1 110.4(7) . . ? C41 N41 K1 125.1(7) . . ? C50 N42 C46 118.6(19) . . ? C50 N42 K1 114.8(16) . . ? C46 N42 K1 126.6(11) . . ? N41 C41 C42 119.1(6) . . ? C43 C42 C41 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? N41 C45 C44 119.3(6) . . ? C47 C46 N42 125(2) . . ? C46 C47 C48 119(3) . . ? C47 C48 C49 116(3) . . ? C50 C49 C48 117(3) . . ? N42 C50 C49 124(3) . . ? C55 N51 C51 114.0(14) . . ? C55 N51 K2 135.2(11) . . ? C51 N51 K2 108.0(12) . . ? N51 C51 C52 124.8(19) . . ? C51 C52 C53 121(2) . . ? C54 C53 C52 116.2(19) . . ? C53 C54 C55 117.6(17) . . ? N51 C55 C54 126.9(13) . . ? C56 N52 C60 120.0 . . ? C56 N52 K2 102.33(18) . . ? C60 N52 K2 132.40(17) . . ? C57 C56 N52 120.0 . . ? C56 C57 C58 120.0 . . ? C59 C58 C57 120.0 . . ? C60 C59 C58 120.0 . . ? C59 C60 N52 120.0 . . ? C56B N52B C60B 119.9 . . ? C56B N52B K2 132.0(2) . . ? C60B N52B K2 108.1(2) . . ? N52B C56B C57B 120.0 . . ? C58B C57B C56B 120.0 . . ? C57B C58B C59B 119.9 . . ? C58B C59B C60B 120.0 . . ? N52B C60B C59B 120.0 . . ? N52B C60B K2 48.53(17) . . ? C59B C60B K2 168.56(16) . . ? C61 N61 C65 120.0 . . ? C62 C61 N61 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 N61 120.0 . . ? C66 N62 C70 120.0 . . ? C67 C66 N62 120.0 . . ? C68 C67 C66 120.0 . . ? C67 C68 C69 120.0 . . ? C68 C69 C70 120.0 . . ? C69 C70 N62 120.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.590 _refine_diff_density_min -2.363 _refine_diff_density_rms 0.173 # Attachment '- 5.cif' data_bi250 _database_code_depnum_ccdc_archive 'CCDC 877723' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H78 I K2 N4 Nd O16' _chemical_formula_weight 1508.64 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y, -z-1/2' _cell_length_a 14.0578(5) _cell_length_b 12.1559(4) _cell_length_c 19.0780(7) _cell_angle_alpha 90.00 _cell_angle_beta 89.466(4) _cell_angle_gamma 90.00 _cell_volume 3260.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3310 _cell_measurement_theta_min 3.4971 _cell_measurement_theta_max 32.4098 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.97 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1538 _exptl_absorpt_coefficient_mu 1.467 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.3306 _exptl_absorpt_correction_T_max 0.8768 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15573 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8058 _reflns_number_gt 6051 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 60.00 92.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 25.4051 179.0000 -150.0000 32 #__ type_ start__ end____ width___ exp.time_ 2 omega -79.00 24.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 0.0000 -90.0000 103 #__ type_ start__ end____ width___ exp.time_ 3 omega 3.00 46.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 45.0000 114.0000 43 #__ type_ start__ end____ width___ exp.time_ 4 omega 61.00 93.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 179.0000 30.0000 32 #__ type_ start__ end____ width___ exp.time_ 5 omega -88.00 -58.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 131.0000 -13.0000 30 ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0854P)^2^+20.3814P] 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 8058 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1999 _refine_ls_wR_factor_gt 0.1776 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.2500 0.46328(4) 0.7500 0.01529(14) Uani 1 2 d S . . I1 I 0.2500 0.34413(7) 0.2500 0.0438(2) Uani 1 2 d S . . K1 K 0.28288(11) 0.28451(14) 0.41760(9) 0.0349(4) Uani 1 1 d . . . O1 O 0.2610(3) 0.6145(4) 0.8253(2) 0.0239(10) Uani 1 1 d . . . O2 O 0.3300(3) 0.3850(3) 0.6565(2) 0.0203(9) Uani 1 1 d . . . N1 N 0.4293(4) 0.4837(4) 0.7999(3) 0.0184(10) Uani 1 1 d . . . N2 N 0.3433(3) 0.2821(4) 0.7896(3) 0.0151(9) Uani 1 1 d . . . H2 H 0.3236 0.2688 0.8355 0.018 Uiso 1 1 calc R . . C1 C 0.3187(5) 0.6948(5) 0.8308(3) 0.0210(12) Uani 1 1 d . . . C2 C 0.2870(5) 0.8040(6) 0.8425(4) 0.0324(16) Uani 1 1 d . . . H2A H 0.2205 0.8172 0.8458 0.039 Uiso 1 1 calc R . . C3 C 0.3480(6) 0.8918(6) 0.8492(4) 0.0335(16) Uani 1 1 d . . . H3 H 0.3231 0.9638 0.8553 0.040 Uiso 1 1 calc R . . C4 C 0.4472(6) 0.8754(5) 0.8470(4) 0.0286(15) Uani 1 1 d . . . H4 H 0.4895 0.9356 0.8528 0.034 Uiso 1 1 calc R . . C5 C 0.4813(5) 0.7718(5) 0.8363(3) 0.0240(13) Uani 1 1 d . . . H5 H 0.5481 0.7606 0.8351 0.029 Uiso 1 1 calc R . . C6 C 0.4211(4) 0.6814(5) 0.8273(3) 0.0166(11) Uani 1 1 d . . . C7 C 0.4675(4) 0.5764(5) 0.8185(3) 0.0190(12) Uani 1 1 d . . . H7 H 0.5338 0.5748 0.8275 0.023 Uiso 1 1 calc R . . C8 C 0.4892(4) 0.3885(5) 0.7985(3) 0.0200(12) Uani 1 1 d . . . C9 C 0.5891(5) 0.3921(6) 0.8030(4) 0.0304(15) Uani 1 1 d . . . H9 H 0.6204 0.4612 0.8064 0.036 Uiso 1 1 calc R . . C10 C 0.6419(5) 0.2966(6) 0.8027(4) 0.0327(16) Uani 1 1 d . . . H10 H 0.7091 0.3004 0.8070 0.039 Uiso 1 1 calc R . . C11 C 0.5983(5) 0.1959(6) 0.7962(4) 0.0290(15) Uani 1 1 d . . . H11 H 0.6352 0.1304 0.7954 0.035 Uiso 1 1 calc R . . C12 C 0.5009(5) 0.1905(6) 0.7909(3) 0.0251(14) Uani 1 1 d . . . H12 H 0.4709 0.1209 0.7864 0.030 Uiso 1 1 calc R . . C13 C 0.4454(4) 0.2858(5) 0.7919(3) 0.0181(12) Uani 1 1 d . . . C14 C 0.3048(4) 0.1890(5) 0.7477(3) 0.0186(12) Uani 1 1 d . . . H14 H 0.3273 0.1194 0.7700 0.022 Uiso 1 1 calc R . . C15 C 0.3432(4) 0.1902(5) 0.6732(3) 0.0197(12) Uani 1 1 d . . . C16 C 0.3697(5) 0.0898(5) 0.6435(3) 0.0245(13) Uani 1 1 d . . . H16 H 0.3606 0.0242 0.6698 0.029 Uiso 1 1 calc R . . C17 C 0.4093(6) 0.0830(7) 0.5765(4) 0.0375(18) Uani 1 1 d . . . H17 H 0.4261 0.0137 0.5570 0.045 Uiso 1 1 calc R . . C18 C 0.4236(6) 0.1784(6) 0.5388(4) 0.0328(16) Uani 1 1 d . . . H18 H 0.4518 0.1748 0.4934 0.039 Uiso 1 1 calc R . . C19 C 0.3980(5) 0.2776(6) 0.5658(3) 0.0273(14) Uani 1 1 d . . . H19 H 0.4083 0.3420 0.5386 0.033 Uiso 1 1 calc R . . C20 C 0.3557(4) 0.2880(5) 0.6342(3) 0.0203(12) Uani 1 1 d . . . O21 O 0.4594(4) 0.2726(4) 0.3589(3) 0.0344(12) Uani 1 1 d . . . O22 O 0.4046(4) 0.4697(4) 0.4249(3) 0.0389(13) Uani 1 1 d . . . O23 O 0.2126(5) 0.4829(5) 0.4705(3) 0.0476(15) Uani 1 1 d . . . O24 O 0.1346(4) 0.2803(7) 0.5209(3) 0.0536(18) Uani 1 1 d . . . O25 O 0.1813(5) 0.0872(6) 0.4440(3) 0.0552(18) Uani 1 1 d . . . O26 O 0.3657(4) 0.0774(5) 0.3803(3) 0.0408(13) Uani 1 1 d . . . C21 C 0.5244(6) 0.3574(8) 0.3740(5) 0.045(2) Uani 1 1 d . . . H21A H 0.5779 0.3559 0.3399 0.054 Uiso 1 1 calc R . . H21B H 0.5504 0.3472 0.4216 0.054 Uiso 1 1 calc R . . C22 C 0.4735(6) 0.4640(7) 0.3697(5) 0.0404(19) Uani 1 1 d . . . H22A H 0.5193 0.5255 0.3740 0.048 Uiso 1 1 calc R . . H22B H 0.4416 0.4704 0.3238 0.048 Uiso 1 1 calc R . . C23 C 0.3489(8) 0.5658(7) 0.4204(6) 0.054(2) Uani 1 1 d . . . H23A H 0.3150 0.5671 0.3752 0.065 Uiso 1 1 calc R . . H23B H 0.3904 0.6315 0.4227 0.065 Uiso 1 1 calc R . . C24 C 0.2786(8) 0.5678(8) 0.4799(6) 0.059(3) Uani 1 1 d . . . H24A H 0.3119 0.5578 0.5249 0.071 Uiso 1 1 calc R . . H24B H 0.2454 0.6396 0.4812 0.071 Uiso 1 1 calc R . . C25 C 0.1507(7) 0.4759(10) 0.5292(4) 0.055(3) Uani 1 1 d . . . H25A H 0.1143 0.5452 0.5343 0.066 Uiso 1 1 calc R . . H25B H 0.1881 0.4647 0.5724 0.066 Uiso 1 1 calc R . . C26 C 0.0835(7) 0.3810(11) 0.5193(5) 0.062(3) Uani 1 1 d . . . H26A H 0.0345 0.3814 0.5569 0.075 Uiso 1 1 calc R . . H26B H 0.0509 0.3884 0.4737 0.075 Uiso 1 1 calc R . . C27 C 0.0736(7) 0.1882(12) 0.5163(5) 0.070(4) Uani 1 1 d . . . H27A H 0.0321 0.1954 0.4749 0.084 Uiso 1 1 calc R . . H27B H 0.0328 0.1834 0.5587 0.084 Uiso 1 1 calc R . . C28 C 0.1337(8) 0.0874(11) 0.5097(5) 0.061(3) Uani 1 1 d . . . H28A H 0.1808 0.0857 0.5479 0.074 Uiso 1 1 calc R . . H28B H 0.0931 0.0211 0.5140 0.074 Uiso 1 1 calc R . . C29 C 0.2348(9) -0.0115(9) 0.4335(6) 0.064(3) Uani 1 1 d . . . H29A H 0.1912 -0.0752 0.4301 0.077 Uiso 1 1 calc R . . H29B H 0.2776 -0.0237 0.4737 0.077 Uiso 1 1 calc R . . C30 C 0.2920(9) -0.0015(8) 0.3676(5) 0.058(3) Uani 1 1 d . . . H30A H 0.3201 -0.0735 0.3548 0.070 Uiso 1 1 calc R . . H30B H 0.2512 0.0234 0.3286 0.070 Uiso 1 1 calc R . . C31 C 0.4262(6) 0.0926(7) 0.3219(4) 0.042(2) Uani 1 1 d . . . H31A H 0.3895 0.1209 0.2817 0.051 Uiso 1 1 calc R . . H31B H 0.4555 0.0217 0.3081 0.051 Uiso 1 1 calc R . . C32 C 0.5025(6) 0.1743(8) 0.3421(4) 0.0376(18) Uani 1 1 d . . . H32A H 0.5384 0.1463 0.3827 0.045 Uiso 1 1 calc R . . H32B H 0.5475 0.1849 0.3025 0.045 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 Nd1 0.0142(2) 0.0124(2) 0.0192(2) 0.000 0.00167(16) 0.000 I1 0.0404(4) 0.0526(5) 0.0385(4) 0.000 -0.0056(3) 0.000 K1 0.0246(7) 0.0351(8) 0.0446(9) -0.0034(7) 0.0114(7) -0.0008(7) O1 0.019(2) 0.022(2) 0.031(2) -0.0101(19) -0.0007(19) -0.0004(18) O2 0.024(2) 0.0166(19) 0.020(2) -0.0007(17) 0.0054(18) 0.0028(18) N1 0.017(2) 0.019(3) 0.019(2) -0.0002(19) 0.004(2) 0.000(2) N2 0.016(2) 0.014(2) 0.015(2) -0.0019(18) 0.0011(19) -0.0002(19) C1 0.019(3) 0.022(3) 0.022(3) -0.003(2) 0.001(2) 0.000(3) C2 0.027(3) 0.024(3) 0.046(4) -0.010(3) -0.007(3) 0.002(3) C3 0.044(4) 0.018(3) 0.039(4) 0.000(3) -0.010(3) 0.001(3) C4 0.038(4) 0.019(3) 0.029(3) 0.001(3) -0.005(3) -0.011(3) C5 0.025(3) 0.021(3) 0.027(3) 0.002(3) -0.003(3) -0.010(3) C6 0.018(3) 0.017(3) 0.015(3) 0.000(2) -0.001(2) -0.005(2) C7 0.020(3) 0.019(3) 0.018(3) 0.000(2) 0.003(2) -0.001(2) C8 0.018(3) 0.024(3) 0.017(3) 0.000(2) -0.002(2) 0.002(2) C9 0.021(3) 0.025(3) 0.045(4) 0.000(3) -0.001(3) -0.004(3) C10 0.014(3) 0.041(4) 0.043(4) -0.009(3) 0.002(3) 0.007(3) C11 0.025(3) 0.028(3) 0.034(4) -0.002(3) -0.002(3) 0.011(3) C12 0.027(3) 0.024(3) 0.024(3) -0.001(3) -0.003(3) 0.007(3) C13 0.019(3) 0.020(3) 0.015(3) 0.000(2) 0.003(2) -0.001(2) C14 0.018(3) 0.012(2) 0.026(3) -0.001(2) -0.002(2) 0.001(2) C15 0.015(3) 0.019(3) 0.025(3) -0.007(2) 0.000(2) 0.002(2) C16 0.028(3) 0.017(3) 0.028(3) -0.006(3) -0.004(3) 0.008(3) C17 0.045(4) 0.030(4) 0.037(4) -0.016(3) -0.001(4) 0.009(4) C18 0.039(4) 0.040(4) 0.020(3) -0.007(3) 0.006(3) 0.010(3) C19 0.024(3) 0.037(4) 0.021(3) -0.001(3) 0.002(3) 0.004(3) C20 0.020(3) 0.024(3) 0.017(3) -0.004(2) 0.003(2) 0.001(3) O21 0.024(2) 0.035(3) 0.044(3) 0.001(2) 0.005(2) 0.002(2) O22 0.044(3) 0.035(3) 0.037(3) 0.005(2) 0.001(3) -0.004(3) O23 0.051(4) 0.055(4) 0.037(3) -0.008(3) 0.003(3) 0.017(3) O24 0.027(3) 0.098(6) 0.036(3) 0.002(3) 0.003(2) -0.007(3) O25 0.060(4) 0.071(5) 0.034(3) 0.014(3) -0.005(3) -0.030(4) O26 0.050(3) 0.035(3) 0.037(3) -0.004(2) -0.003(3) -0.004(3) C21 0.031(4) 0.061(6) 0.042(5) 0.009(4) 0.006(4) -0.010(4) C22 0.040(4) 0.033(4) 0.049(5) 0.007(4) 0.010(4) -0.009(4) C23 0.069(7) 0.030(4) 0.064(6) 0.000(4) 0.007(5) 0.007(4) C24 0.069(7) 0.042(5) 0.066(6) -0.021(5) 0.005(5) 0.010(5) C25 0.042(5) 0.091(8) 0.031(4) -0.006(5) -0.001(4) 0.034(5) C26 0.037(5) 0.118(10) 0.033(4) 0.000(5) 0.003(4) 0.024(6) C27 0.034(5) 0.148(12) 0.029(4) 0.008(6) 0.004(4) -0.036(7) C28 0.058(6) 0.089(8) 0.037(5) 0.017(5) 0.004(4) -0.031(6) C29 0.080(8) 0.048(6) 0.064(7) 0.013(5) -0.020(6) -0.026(6) C30 0.081(8) 0.038(4) 0.056(6) 0.000(4) -0.013(5) -0.023(5) C31 0.050(5) 0.045(5) 0.031(4) -0.006(3) 0.001(4) 0.016(4) C32 0.029(4) 0.059(5) 0.024(3) -0.004(3) 0.004(3) 0.010(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 Nd1 O2 2.305(4) . ? Nd1 O2 2.305(4) 4_657 ? Nd1 O1 2.340(4) . ? Nd1 O1 2.340(4) 4_657 ? Nd1 N2 2.676(5) 4_657 ? Nd1 N2 2.676(5) . ? Nd1 N1 2.713(5) . ? Nd1 N1 2.713(5) 4_657 ? I1 K1 3.3151(18) 4_656 ? I1 K1 3.3151(18) . ? K1 O21 2.717(5) . ? K1 O23 2.791(6) . ? K1 O22 2.832(6) . ? K1 O25 2.835(7) . ? K1 O24 2.856(6) . ? K1 O26 2.860(6) . ? K1 C19 3.272(7) . ? K1 C18 3.318(8) . ? O1 C1 1.274(8) . ? O2 C20 1.304(7) . ? N1 C7 1.300(8) . ? N1 C8 1.432(8) . ? N2 C13 1.437(8) . ? N2 C14 1.490(7) . ? N2 H2 0.9300 . ? C1 C2 1.417(9) . ? C1 C6 1.450(8) . ? C2 C3 1.376(10) . ? C2 H2A 0.9500 . ? C3 C4 1.408(11) . ? C3 H3 0.9500 . ? C4 C5 1.362(10) . ? C4 H4 0.9500 . ? C5 C6 1.398(8) . ? C5 H5 0.9500 . ? C6 C7 1.442(8) . ? C7 H7 0.9500 . ? C8 C13 1.397(9) . ? C8 C9 1.408(9) . ? C9 C10 1.378(10) . ? C9 H9 0.9500 . ? C10 C11 1.376(11) . ? C10 H10 0.9500 . ? C11 C12 1.375(10) . ? C11 H11 0.9500 . ? C12 C13 1.397(9) . ? C12 H12 0.9500 . ? C14 C15 1.515(8) . ? C14 C14 1.542(12) 4_657 ? C14 H14 1.0000 . ? C15 C16 1.394(8) . ? C15 C20 1.413(9) . ? C16 C17 1.393(10) . ? C16 H16 0.9500 . ? C17 C18 1.378(11) . ? C17 H17 0.9500 . ? C18 C19 1.358(10) . ? C18 H18 0.9500 . ? C19 C20 1.434(8) . ? C19 H19 0.9500 . ? O21 C32 1.376(10) . ? O21 C21 1.409(10) . ? O22 C23 1.409(11) . ? O22 C22 1.426(10) . ? O23 C24 1.400(12) . ? O23 C25 1.415(10) . ? O24 C27 1.413(13) . ? O24 C26 1.419(13) . ? O25 C28 1.416(11) . ? O25 C29 1.430(14) . ? O26 C31 1.407(10) . ? O26 C30 1.435(11) . ? C21 C22 1.484(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.498(14) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.505(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.493(17) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.490(15) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.514(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nd1 O2 131.3(2) . 4_657 ? O2 Nd1 O1 139.90(16) . . ? O2 Nd1 O1 83.32(16) 4_657 . ? O2 Nd1 O1 83.32(16) . 4_657 ? O2 Nd1 O1 139.90(16) 4_657 4_657 ? O1 Nd1 O1 76.4(2) . 4_657 ? O2 Nd1 N2 71.27(15) . 4_657 ? O2 Nd1 N2 69.01(15) 4_657 4_657 ? O1 Nd1 N2 148.83(15) . 4_657 ? O1 Nd1 N2 115.98(16) 4_657 4_657 ? O2 Nd1 N2 69.01(15) . . ? O2 Nd1 N2 71.27(15) 4_657 . ? O1 Nd1 N2 115.98(16) . . ? O1 Nd1 N2 148.83(15) 4_657 . ? N2 Nd1 N2 69.2(2) 4_657 . ? O2 Nd1 N1 82.01(16) . . ? O2 Nd1 N1 102.39(16) 4_657 . ? O1 Nd1 N1 69.25(15) . . ? O1 Nd1 N1 102.15(15) 4_657 . ? N2 Nd1 N1 129.32(15) 4_657 . ? N2 Nd1 N1 61.11(15) . . ? O2 Nd1 N1 102.39(16) . 4_657 ? O2 Nd1 N1 82.01(16) 4_657 4_657 ? O1 Nd1 N1 102.15(15) . 4_657 ? O1 Nd1 N1 69.25(15) 4_657 4_657 ? N2 Nd1 N1 61.11(15) 4_657 4_657 ? N2 Nd1 N1 129.32(15) . 4_657 ? N1 Nd1 N1 169.5(2) . 4_657 ? K1 I1 K1 154.74(7) 4_656 . ? O21 K1 O23 120.93(19) . . ? O21 K1 O22 60.85(17) . . ? O23 K1 O22 60.48(19) . . ? O21 K1 O25 119.0(2) . . ? O23 K1 O25 119.4(2) . . ? O22 K1 O25 165.38(19) . . ? O21 K1 O24 160.31(19) . . ? O23 K1 O24 60.8(2) . . ? O22 K1 O24 114.7(2) . . ? O25 K1 O24 59.9(2) . . ? O21 K1 O26 58.83(17) . . ? O23 K1 O26 172.77(19) . . ? O22 K1 O26 117.85(18) . . ? O25 K1 O26 60.2(2) . . ? O24 K1 O26 116.7(2) . . ? O21 K1 C19 84.12(17) . . ? O23 K1 C19 83.45(19) . . ? O22 K1 C19 70.97(18) . . ? O25 K1 C19 94.40(19) . . ? O24 K1 C19 76.52(17) . . ? O26 K1 C19 89.37(18) . . ? O21 K1 I1 75.48(12) . . ? O23 K1 I1 96.19(14) . . ? O22 K1 I1 87.91(12) . . ? O25 K1 I1 106.38(14) . . ? O24 K1 I1 124.19(14) . . ? O26 K1 I1 90.71(12) . . ? C19 K1 I1 156.02(13) . . ? O21 K1 C18 73.63(18) . . ? O23 K1 C18 107.16(19) . . ? O22 K1 C18 84.85(19) . . ? O25 K1 C18 81.4(2) . . ? O24 K1 C18 87.03(19) . . ? O26 K1 C18 65.64(17) . . ? C19 K1 C18 23.77(17) . . ? I1 K1 C18 147.84(13) . . ? C1 O1 Nd1 134.3(4) . . ? C20 O2 Nd1 139.3(4) . . ? C7 N1 C8 117.5(5) . . ? C7 N1 Nd1 124.3(4) . . ? C8 N1 Nd1 117.9(4) . . ? C13 N2 C14 114.2(5) . . ? C13 N2 Nd1 118.4(4) . . ? C14 N2 Nd1 107.0(3) . . ? C13 N2 H2 105.4 . . ? C14 N2 H2 105.4 . . ? Nd1 N2 H2 105.4 . . ? O1 C1 C2 122.0(6) . . ? O1 C1 C6 122.9(6) . . ? C2 C1 C6 115.0(6) . . ? C3 C2 C1 123.1(7) . . ? C3 C2 H2A 118.5 . . ? C1 C2 H2A 118.5 . . ? C2 C3 C4 120.4(7) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 118.8(6) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 122.2(6) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C7 115.9(6) . . ? C5 C6 C1 120.5(6) . . ? C7 C6 C1 123.5(5) . . ? N1 C7 C6 127.7(6) . . ? N1 C7 H7 116.1 . . ? C6 C7 H7 116.1 . . ? C13 C8 C9 118.3(6) . . ? C13 C8 N1 117.6(5) . . ? C9 C8 N1 124.1(6) . . ? C10 C9 C8 120.7(7) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 120.6(6) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 119.6(6) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 121.0(7) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C8 119.7(6) . . ? C12 C13 N2 122.1(6) . . ? C8 C13 N2 118.2(5) . . ? N2 C14 C15 111.6(5) . . ? N2 C14 C14 109.7(4) . 4_657 ? C15 C14 C14 113.6(6) . 4_657 ? N2 C14 H14 107.2 . . ? C15 C14 H14 107.2 . . ? C14 C14 H14 107.2 4_657 . ? C16 C15 C20 119.4(6) . . ? C16 C15 C14 117.7(6) . . ? C20 C15 C14 122.9(5) . . ? C17 C16 C15 121.9(7) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C18 C17 C16 118.9(6) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C17 120.8(6) . . ? C19 C18 K1 76.2(4) . . ? C17 C18 K1 127.3(6) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? K1 C18 H18 68.2 . . ? C18 C19 C20 122.0(7) . . ? C18 C19 K1 80.0(4) . . ? C20 C19 K1 125.5(4) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? K1 C19 H19 65.2 . . ? O2 C20 C15 123.8(5) . . ? O2 C20 C19 119.2(6) . . ? C15 C20 C19 117.0(6) . . ? C32 O21 C21 113.5(6) . . ? C32 O21 K1 122.7(4) . . ? C21 O21 K1 117.9(5) . . ? C23 O22 C22 111.6(6) . . ? C23 O22 K1 108.7(5) . . ? C22 O22 K1 109.4(4) . . ? C24 O23 C25 110.2(7) . . ? C24 O23 K1 116.8(5) . . ? C25 O23 K1 116.6(6) . . ? C27 O24 C26 112.0(8) . . ? C27 O24 K1 114.2(5) . . ? C26 O24 K1 109.6(5) . . ? C28 O25 C29 111.7(8) . . ? C28 O25 K1 112.9(6) . . ? C29 O25 K1 114.9(6) . . ? C31 O26 C30 112.7(7) . . ? C31 O26 K1 108.9(5) . . ? C30 O26 K1 109.8(6) . . ? O21 C21 C22 108.3(7) . . ? O21 C21 H21A 110.0 . . ? C22 C21 H21A 110.0 . . ? O21 C21 H21B 110.0 . . ? C22 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? O22 C22 C21 109.0(6) . . ? O22 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O22 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? O22 C23 C24 109.3(8) . . ? O22 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? O22 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? O23 C24 C23 108.9(8) . . ? O23 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? O23 C24 H24B 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? O23 C25 C26 109.2(8) . . ? O23 C25 H25A 109.8 . . ? C26 C25 H25A 109.8 . . ? O23 C25 H25B 109.8 . . ? C26 C25 H25B 109.8 . . ? H25A C25 H25B 108.3 . . ? O24 C26 C25 109.8(8) . . ? O24 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 . . ? O24 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? O24 C27 C28 108.2(8) . . ? O24 C27 H27A 110.1 . . ? C28 C27 H27A 110.1 . . ? O24 C27 H27B 110.1 . . ? C28 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? O25 C28 C27 109.7(8) . . ? O25 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? O25 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? O25 C29 C30 109.2(8) . . ? O25 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? O25 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? O26 C30 C29 107.2(8) . . ? O26 C30 H30A 110.3 . . ? C29 C30 H30A 110.3 . . ? O26 C30 H30B 110.3 . . ? C29 C30 H30B 110.3 . . ? H30A C30 H30B 108.5 . . ? O26 C31 C32 108.0(6) . . ? O26 C31 H31A 110.1 . . ? C32 C31 H31A 110.1 . . ? O26 C31 H31B 110.1 . . ? C32 C31 H31B 110.1 . . ? H31A C31 H31B 108.4 . . ? O21 C32 C31 108.5(6) . . ? O21 C32 H32A 110.0 . . ? C31 C32 H32A 110.0 . . ? O21 C32 H32B 110.0 . . ? C31 C32 H32B 110.0 . . ? H32A C32 H32B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.314 _refine_diff_density_min -4.005 _refine_diff_density_rms 0.193 # Attachment '- 6.cif' data_cc161 _database_code_depnum_ccdc_archive 'CCDC 877724' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.50 H45.50 K N3.50 Nd O8' _chemical_formula_weight 880.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Nd Nd -0.1943 3.0179 '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 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.3718(3) _cell_length_b 15.0596(3) _cell_length_c 19.3034(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.603(2) _cell_angle_gamma 90.00 _cell_volume 3793.53(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9737 _cell_measurement_theta_min 3.3511 _cell_measurement_theta_max 32.3768 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 1 -1 0.1891 -0.0003 1.0000 -0.9968 -0.0375 0.0098 -0.0461 0 -1 1 0.1741 0.0003 -1.0000 0.9968 0.0375 -0.0098 0.0461 1 0 -1 0.0390 0.9981 -0.0006 -0.9988 0.0274 0.0386 -0.0350 3 -1 0 0.0476 2.9960 -1.0015 -0.0018 0.1120 0.1266 0.0128 0 0 -1 0.0091 -0.0006 -0.0001 -0.9989 0.0038 -0.0103 -0.0360 0 0 1 0.0081 0.0006 0.0001 0.9989 -0.0038 0.0103 0.0360 -1 0 1 0.0390 -0.9981 0.0006 0.9988 -0.0274 -0.0386 0.0350 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 1.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5273 _exptl_absorpt_correction_T_max 0.9744 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33205 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9388 _reflns_number_gt 7219 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -39.00 98.00 1.0000 220.0000 omega____ theta____ kappa____ phi______ frames - 25.4051 0.0000 -180.0000 137 #__ type_ start__ end____ width___ exp.time_ 2 omega -8.00 73.00 1.0000 220.0000 omega____ theta____ kappa____ phi______ frames - 25.4051 -109.0000 158.0000 81 #__ type_ start__ end____ width___ exp.time_ 3 omega -3.00 95.00 1.0000 220.0000 omega____ theta____ kappa____ phi______ frames - 25.4051 77.0000 -60.0000 98 #__ type_ start__ end____ width___ exp.time_ 4 omega -104.00 -59.00 1.0000 220.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 179.0000 -30.0000 45 #__ type_ start__ end____ width___ exp.time_ 5 omega -74.00 -10.00 1.0000 220.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 109.0000 -106.0000 64 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0323P)^2^+0.7244P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_coef ? _refine_ls_number_reflns 9388 _refine_ls_number_parameters 669 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.001 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 Nd1 Nd 0.870599(8) 0.485278(8) 0.005684(6) 0.01604(3) Uani 1 1 d . . . O1 O 0.82829(11) 0.34052(10) 0.03113(8) 0.0229(4) Uani 1 1 d . . . O2 O 0.78904(11) 0.60837(10) 0.04384(8) 0.0219(4) Uani 1 1 d . . . N1 N 1.02845(13) 0.41417(11) 0.06559(9) 0.0166(4) Uani 1 1 d . . . N2 N 1.00600(13) 0.57809(11) 0.07042(9) 0.0165(4) Uani 1 1 d . . . C1 C 0.87457(17) 0.26800(14) 0.05962(11) 0.0193(5) Uani 1 1 d . . . H1 H 0.7600(18) 0.2071(15) 0.0786(11) 0.024(6) Uiso 1 1 d . . . C2 C 0.82046(18) 0.20027(16) 0.08537(12) 0.0252(6) Uani 1 1 d . . . H2 H 0.835(2) 0.0845(16) 0.1318(12) 0.037(7) Uiso 1 1 d . . . C3 C 0.8675(2) 0.12535(16) 0.11680(13) 0.0290(6) Uani 1 1 d . . . H3 H 1.0016(17) 0.0687(15) 0.1427(11) 0.021(6) Uiso 1 1 d . . . C4 C 0.9712(2) 0.11360(16) 0.12427(13) 0.0293(6) Uani 1 1 d . . . H4 H 1.0947(17) 0.1728(14) 0.1061(11) 0.016(6) Uiso 1 1 d . . . C5 C 1.02755(18) 0.17918(16) 0.09889(12) 0.0248(6) Uani 1 1 d . . . C6 C 0.98168(16) 0.25486(14) 0.06623(11) 0.0183(5) Uani 1 1 d . . . C7 C 1.04188(16) 0.32592(14) 0.03757(11) 0.0166(5) Uani 1 1 d . . . H7 H 1.1110(16) 0.3093(13) 0.0493(10) 0.012(4) Uiso 1 1 d . . . C8 C 1.09598(15) 0.45178(15) 0.12198(10) 0.0176(5) Uani 1 1 d . . . C9 C 1.17555(17) 0.41240(15) 0.17162(11) 0.0211(5) Uani 1 1 d . . . H9 H 1.1808(17) 0.3551(14) 0.1704(11) 0.018(6) Uiso 1 1 d . . . C10 C 1.24142(18) 0.46311(16) 0.22194(11) 0.0245(6) Uani 1 1 d . . . H10 H 1.2960(19) 0.4302(16) 0.2537(12) 0.034(7) Uiso 1 1 d . . . C11 C 1.23112(17) 0.55453(16) 0.22338(11) 0.0241(6) Uani 1 1 d . . . H11 H 1.2753(18) 0.5914(15) 0.2561(11) 0.022(6) Uiso 1 1 d . . . C12 C 1.15201(17) 0.59685(15) 0.17557(11) 0.0206(5) Uani 1 1 d . . . H12 H 1.1435(18) 0.6572(15) 0.1820(11) 0.023(6) Uiso 1 1 d . . . C13 C 1.08323(15) 0.54796(14) 0.12455(10) 0.0167(5) Uani 1 1 d . . . C14 C 0.99410(16) 0.67071(14) 0.04828(11) 0.0168(5) Uani 1 1 d . . . H14 H 1.0577(16) 0.7012(13) 0.0594(10) 0.012(4) Uiso 1 1 d . . . C15 C 0.91774(16) 0.72063(14) 0.08128(11) 0.0168(5) Uani 1 1 d . . . C16 C 0.94225(17) 0.80120(15) 0.11486(12) 0.0223(5) Uani 1 1 d . . . H16 H 1.0012(18) 0.8223(14) 0.1195(11) 0.019(6) Uiso 1 1 d . . . C17 C 0.87340(19) 0.85069(15) 0.14319(12) 0.0250(6) Uani 1 1 d . . . H17 H 0.8892(18) 0.9030(15) 0.1667(11) 0.022(6) Uiso 1 1 d . . . C18 C 0.77600(18) 0.81739(16) 0.13703(12) 0.0251(6) Uani 1 1 d . . . H18 H 0.737(2) 0.8421(17) 0.1560(13) 0.040(8) Uiso 1 1 d . . . C19 C 0.74838(17) 0.73646(15) 0.10474(12) 0.0219(5) Uani 1 1 d . . . H19 H 0.6825(18) 0.7126(14) 0.0972(11) 0.019(6) Uiso 1 1 d . . . C20 C 0.81720(16) 0.68526(14) 0.07616(11) 0.0179(5) Uani 1 1 d . . . K1 K 1.08213(4) 0.49697(3) 0.31773(3) 0.02782(13) Uani 1 1 d . . . O21 O 0.89172(13) 0.41757(12) 0.25595(8) 0.0359(5) Uani 1 1 d . . . O22 O 0.91238(14) 0.60253(13) 0.26481(9) 0.0406(5) Uani 1 1 d . . . O23 O 1.06550(14) 0.67486(11) 0.36805(9) 0.0360(5) Uani 1 1 d . . . O24 O 1.24602(12) 0.57243(11) 0.41666(8) 0.0266(4) Uani 1 1 d . . . O25 O 1.22806(13) 0.38899(11) 0.40526(9) 0.0310(4) Uani 1 1 d . . . O26 O 1.06911(14) 0.31201(12) 0.30494(9) 0.0353(5) Uani 1 1 d . . . C21 C 0.8380(2) 0.4768(2) 0.20312(15) 0.0537(9) Uani 1 1 d . . . H21A H 0.872(3) 0.485(2) 0.1666(17) 0.066(10) Uiso 1 1 d . . . H21B H 0.776(2) 0.4468(18) 0.1794(13) 0.043(8) Uiso 1 1 d . . . C22 C 0.8179(2) 0.5610(2) 0.23648(16) 0.0540(9) Uani 1 1 d . . . H22A H 0.781(2) 0.600(2) 0.2029(15) 0.062(10) Uiso 1 1 d . . . H22B H 0.783(2) 0.5464(18) 0.2708(13) 0.040(8) Uiso 1 1 d . . . C23 C 0.9019(2) 0.6876(2) 0.29375(17) 0.0496(9) Uani 1 1 d . . . H23A H 0.858(2) 0.7204(18) 0.2538(14) 0.050(8) Uiso 1 1 d . . . H23B H 0.876(2) 0.6807(17) 0.3332(14) 0.041(8) Uiso 1 1 d . . . C24 C 1.0053(2) 0.7283(2) 0.31505(17) 0.0473(9) Uani 1 1 d . . . H24A H 1.031(2) 0.7333(18) 0.2712(14) 0.048(9) Uiso 1 1 d . . . H24B H 1.003(2) 0.7839(19) 0.3328(14) 0.052(9) Uiso 1 1 d . . . C25 C 1.1633(2) 0.71179(17) 0.39852(15) 0.0360(7) Uani 1 1 d . . . H25A H 1.191(2) 0.7258(16) 0.3603(12) 0.032(7) Uiso 1 1 d . . . H25B H 1.153(2) 0.7689(19) 0.4190(14) 0.054(9) Uiso 1 1 d . . . C26 C 1.2211(2) 0.64988(17) 0.45123(13) 0.0321(6) Uani 1 1 d . . . H26A H 1.2811(19) 0.6757(15) 0.4766(12) 0.029(7) Uiso 1 1 d . . . H26B H 1.186(2) 0.6326(18) 0.4840(14) 0.047(8) Uiso 1 1 d . . . C27 C 1.3089(2) 0.51439(18) 0.46546(12) 0.0316(6) Uani 1 1 d . . . H27A H 1.366(2) 0.5397(19) 0.4822(15) 0.053(9) Uiso 1 1 d . . . H27B H 1.2787(17) 0.5036(13) 0.5052(11) 0.012(6) Uiso 1 1 d . . . C28 C 1.3242(2) 0.43029(18) 0.42897(13) 0.0320(7) Uani 1 1 d . . . H28A H 1.3544(18) 0.4395(15) 0.3868(11) 0.022(6) Uiso 1 1 d . . . H28B H 1.364(2) 0.3921(16) 0.4598(13) 0.034(7) Uiso 1 1 d . . . C29 C 1.2357(2) 0.30164(17) 0.37786(14) 0.0362(7) Uani 1 1 d . . . H29A H 1.2666(19) 0.3037(15) 0.3342(12) 0.028(7) Uiso 1 1 d . . . H29B H 1.280(2) 0.2737(17) 0.4117(13) 0.044(8) Uiso 1 1 d . . . C30 C 1.1312(2) 0.26235(18) 0.35890(15) 0.0421(7) Uani 1 1 d . . . H30A H 1.1032(18) 0.2601(15) 0.4048(12) 0.025(6) Uiso 1 1 d . . . H30B H 1.141(2) 0.205(2) 0.3458(15) 0.064(10) Uiso 1 1 d . . . C31 C 0.9683(2) 0.27676(19) 0.28198(18) 0.0540(9) Uani 1 1 d . . . H31A H 0.974(2) 0.2220(19) 0.2653(14) 0.050(9) Uiso 1 1 d . . . H31B H 0.939(2) 0.2711(19) 0.3207(15) 0.057(9) Uiso 1 1 d . . . C32 C 0.9079(2) 0.3341(2) 0.22675(16) 0.0531(9) Uani 1 1 d . . . H32A H 0.945(2) 0.343(2) 0.1898(16) 0.065(10) Uiso 1 1 d . . . H32B H 0.843(2) 0.308(2) 0.2057(15) 0.062(10) Uiso 1 1 d . . . N41 N 0.66190(14) 0.45995(13) -0.04946(10) 0.0255(5) Uani 1 1 d . . . C41 C 0.6067(2) 0.50840(17) -0.10216(14) 0.0324(6) Uani 1 1 d . . . H41 H 0.6441(17) 0.5477(15) -0.1238(11) 0.019(4) Uiso 1 1 d . . . C42 C 0.5017(2) 0.50163(17) -0.12420(15) 0.0381(8) Uani 1 1 d . . . H42 H 0.470(2) 0.5366(18) -0.1617(14) 0.044(8) Uiso 1 1 d . . . C43 C 0.45039(19) 0.44310(18) -0.09026(15) 0.0363(7) Uani 1 1 d . . . H43 H 0.3798(19) 0.4381(16) -0.1033(12) 0.027(7) Uiso 1 1 d . . . C44 C 0.50539(18) 0.39265(17) -0.03633(14) 0.0309(6) Uani 1 1 d . . . H44 H 0.480(2) 0.3559(19) -0.0113(13) 0.044(9) Uiso 1 1 d . . . C45 C 0.60997(18) 0.40181(16) -0.01801(13) 0.0279(6) Uani 1 1 d . . . H45 H 0.6502(17) 0.3704(14) 0.0199(11) 0.019(4) Uiso 1 1 d . . . N51 N 0.9850(5) 0.4392(4) 0.4460(3) 0.0497(19) Uani 0.50 1 d P . 1 C51 C 1.0651(2) 0.4319(2) 0.50621(16) 0.0515(9) Uani 1 1 d . . . H51 H 1.102(3) 0.388(2) 0.5174(17) 0.074(11) Uiso 1 1 d . . . C52 C 1.0732(2) 0.4929(2) 0.55888(14) 0.0454(8) Uani 1 1 d . . . H52 H 1.114(2) 0.4876(18) 0.5935(15) 0.048(9) Uiso 1 1 d . . . C53 C 1.0030(6) 0.5634(5) 0.5517(4) 0.043(2) Uani 0.50 1 d PDU . 2 H53 H 1.025(4) 0.6038(18) 0.5933(13) 0.037(15) Uiso 0.50 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01053(4) 0.01814(5) 0.02059(5) -0.00111(5) 0.00592(4) -0.00110(5) O1 0.0138(7) 0.0230(8) 0.0329(8) 0.0007(6) 0.0073(6) -0.0010(6) O2 0.0138(7) 0.0209(8) 0.0314(8) -0.0045(6) 0.0061(6) -0.0033(6) N1 0.0148(8) 0.0158(9) 0.0202(9) 0.0017(7) 0.0057(7) 0.0004(7) N2 0.0115(8) 0.0173(9) 0.0210(9) -0.0012(7) 0.0041(7) 0.0003(7) C1 0.0178(10) 0.0212(11) 0.0202(10) -0.0014(8) 0.0067(8) -0.0041(9) C2 0.0196(11) 0.0267(12) 0.0311(12) -0.0034(9) 0.0097(9) -0.0060(10) C3 0.0323(13) 0.0261(12) 0.0315(12) 0.0003(10) 0.0134(10) -0.0087(11) C4 0.0314(13) 0.0204(12) 0.0366(13) 0.0070(10) 0.0085(11) 0.0013(11) C5 0.0222(11) 0.0257(12) 0.0277(12) 0.0003(9) 0.0084(9) 0.0008(10) C6 0.0193(10) 0.0174(10) 0.0201(10) -0.0035(8) 0.0083(8) -0.0032(9) C7 0.0120(9) 0.0176(10) 0.0216(10) -0.0007(8) 0.0066(8) -0.0004(8) C8 0.0139(9) 0.0227(10) 0.0189(10) 0.0010(8) 0.0099(8) 0.0016(9) C9 0.0202(10) 0.0226(11) 0.0219(10) 0.0026(8) 0.0076(8) 0.0035(9) C10 0.0185(11) 0.0344(13) 0.0191(10) 0.0010(9) 0.0012(8) 0.0030(10) C11 0.0192(11) 0.0318(12) 0.0200(11) -0.0032(9) 0.0017(9) -0.0059(10) C12 0.0196(10) 0.0237(11) 0.0206(10) -0.0031(8) 0.0085(8) -0.0014(9) C13 0.0131(9) 0.0220(10) 0.0172(9) 0.0005(8) 0.0081(7) -0.0015(8) C14 0.0137(9) 0.0159(10) 0.0223(10) -0.0005(8) 0.0071(8) -0.0016(8) C15 0.0116(9) 0.0184(10) 0.0204(10) 0.0015(8) 0.0038(8) 0.0011(8) C16 0.0181(10) 0.0221(11) 0.0277(11) -0.0012(9) 0.0074(9) -0.0029(9) C17 0.0288(12) 0.0189(11) 0.0280(12) -0.0044(9) 0.0076(10) 0.0010(10) C18 0.0227(11) 0.0257(12) 0.0296(12) 0.0003(9) 0.0118(9) 0.0042(10) C19 0.0150(10) 0.0237(12) 0.0284(11) 0.0045(9) 0.0078(9) 0.0015(9) C20 0.0171(10) 0.0178(10) 0.0200(10) 0.0036(8) 0.0064(8) 0.0000(9) K1 0.0189(2) 0.0317(3) 0.0322(3) -0.0033(2) 0.00384(19) 0.0005(2) O21 0.0275(9) 0.0561(12) 0.0244(8) -0.0079(8) 0.0066(7) -0.0100(9) O22 0.0218(9) 0.0574(12) 0.0405(10) 0.0138(9) 0.0022(8) 0.0050(9) O23 0.0342(10) 0.0302(9) 0.0436(10) 0.0065(8) 0.0086(8) 0.0039(8) O24 0.0236(8) 0.0284(9) 0.0260(8) -0.0045(6) 0.0017(7) -0.0003(7) O25 0.0279(9) 0.0301(9) 0.0352(9) 0.0001(7) 0.0075(7) 0.0055(8) O26 0.0337(9) 0.0341(10) 0.0427(10) -0.0072(8) 0.0182(8) -0.0115(8) C21 0.0352(16) 0.093(2) 0.0277(14) 0.0090(15) -0.0051(12) -0.0178(17) C22 0.0263(15) 0.083(2) 0.0482(17) 0.0309(16) -0.0022(13) -0.0039(16) C23 0.0360(16) 0.0529(18) 0.0570(19) 0.0184(14) 0.0038(14) 0.0180(15) C24 0.0449(17) 0.0395(16) 0.0570(18) 0.0154(13) 0.0101(14) 0.0124(14) C25 0.0391(15) 0.0218(13) 0.0496(16) -0.0066(11) 0.0151(12) -0.0057(12) C26 0.0277(13) 0.0342(14) 0.0355(13) -0.0105(11) 0.0093(10) -0.0065(11) C27 0.0242(12) 0.0447(14) 0.0233(11) 0.0030(11) -0.0002(9) -0.0013(12) C28 0.0287(13) 0.0394(15) 0.0271(12) 0.0080(10) 0.0043(10) 0.0075(12) C29 0.0423(15) 0.0267(13) 0.0423(15) 0.0027(11) 0.0152(12) 0.0124(12) C30 0.0570(16) 0.0250(14) 0.0546(16) -0.0016(11) 0.0349(13) 0.0000(13) C31 0.0437(15) 0.0349(15) 0.095(2) -0.0311(14) 0.0408(15) -0.0189(13) C32 0.0290(14) 0.081(2) 0.0511(17) -0.0343(15) 0.0128(13) -0.0183(15) N41 0.0167(9) 0.0284(10) 0.0327(10) -0.0074(8) 0.0087(8) -0.0028(8) C41 0.0263(12) 0.0330(14) 0.0398(13) -0.0027(11) 0.0112(10) -0.0044(11) C42 0.0271(13) 0.0361(16) 0.0471(15) 0.0022(11) -0.0007(12) 0.0003(12) C43 0.0159(12) 0.0351(14) 0.0564(16) -0.0113(12) 0.0046(11) -0.0057(11) C44 0.0195(11) 0.0302(13) 0.0460(15) -0.0067(11) 0.0139(10) -0.0071(10) C45 0.0187(11) 0.0273(12) 0.0378(13) -0.0075(10) 0.0067(10) -0.0004(10) N51 0.042(3) 0.086(4) 0.022(3) -0.009(3) 0.008(2) -0.014(3) C51 0.0451(17) 0.062(2) 0.0510(17) 0.0134(14) 0.0176(14) 0.0206(16) C52 0.0334(14) 0.076(2) 0.0258(13) 0.0081(13) 0.0034(11) 0.0048(15) C53 0.051(4) 0.031(4) 0.050(4) 0.004(3) 0.017(3) 0.015(3) _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 Nd1 O1 2.3313(15) . ? Nd1 O2 2.3492(15) . ? Nd1 N2 2.4095(16) . ? Nd1 N1 2.4236(17) . ? Nd1 N1 2.6113(18) 3_765 ? Nd1 N2 2.6171(18) 3_765 ? Nd1 C13 2.762(2) 3_765 ? Nd1 C8 2.766(2) 3_765 ? Nd1 N41 2.7875(18) . ? Nd1 Nd1 3.5429(2) 3_765 ? O1 C1 1.315(3) . ? O2 C20 1.330(3) . ? N1 C8 1.376(3) . ? N1 C7 1.461(3) . ? N1 Nd1 2.6113(18) 3_765 ? N2 C13 1.376(2) . ? N2 C14 1.457(3) . ? N2 Nd1 2.6171(18) 3_765 ? C1 C2 1.403(3) . ? C1 C6 1.424(3) . ? C2 C3 1.367(3) . ? C2 H1 0.80(2) . ? C3 C4 1.374(4) . ? C3 H2 0.84(3) . ? C4 C5 1.395(3) . ? C4 H3 0.83(2) . ? C5 C6 1.380(3) . ? C5 H4 0.88(2) . ? C6 C7 1.515(3) . ? C7 C14 1.622(3) 3_765 ? C7 H7 0.94(2) . ? C8 C9 1.399(3) . ? C8 C13 1.461(3) . ? C8 Nd1 2.766(2) 3_765 ? C9 C10 1.389(3) . ? C9 H9 0.87(2) . ? C10 C11 1.385(3) . ? C10 K1 3.152(2) . ? C10 H10 0.98(2) . ? C11 C12 1.397(3) . ? C11 K1 3.102(2) . ? C11 H11 0.94(2) . ? C12 C13 1.401(3) . ? C12 K1 3.433(2) . ? C12 H12 0.93(2) . ? C13 Nd1 2.762(2) 3_765 ? C14 C15 1.516(3) . ? C14 C7 1.622(3) 3_765 ? C14 H14 0.95(2) . ? C15 C16 1.381(3) . ? C15 C20 1.429(3) . ? C16 C17 1.386(3) . ? C16 H16 0.84(2) . ? C17 C18 1.376(3) . ? C17 H17 0.91(2) . ? C18 C19 1.382(3) . ? C18 H18 0.79(3) . ? C19 C20 1.403(3) . ? C19 H19 0.93(2) . ? K1 O22 2.7769(19) . ? K1 O26 2.7984(18) . ? K1 O25 2.8050(17) . ? K1 O24 2.8133(16) . ? K1 O21 2.8301(18) . ? K1 O23 2.8746(18) . ? K1 C53 3.119(8) 3_766 ? K1 N51 3.159(6) . ? K1 C52 3.488(3) 3_766 ? O21 C32 1.413(4) . ? O21 C21 1.426(3) . ? O22 C22 1.408(3) . ? O22 C23 1.417(4) . ? O23 C24 1.408(3) . ? O23 C25 1.425(3) . ? O24 C27 1.419(3) . ? O24 C26 1.419(3) . ? O25 C28 1.412(3) . ? O25 C29 1.430(3) . ? O26 C30 1.398(3) . ? O26 C31 1.427(3) . ? C21 C22 1.474(5) . ? C21 H21A 0.92(4) . ? C21 H21B 0.96(3) . ? C22 H22A 0.93(3) . ? C22 H22B 0.92(3) . ? C23 C24 1.485(4) . ? C23 H23A 0.99(3) . ? C23 H23B 0.91(3) . ? C24 H24A 0.98(3) . ? C24 H24B 0.91(3) . ? C25 C26 1.469(4) . ? C25 H25A 0.92(3) . ? C25 H25B 0.97(3) . ? C26 H26A 0.93(2) . ? C26 H26B 0.91(3) . ? C27 C28 1.485(4) . ? C27 H27A 0.85(3) . ? C27 H27B 0.96(2) . ? C28 H28A 0.99(2) . ? C28 H28B 0.91(2) . ? C29 C30 1.488(4) . ? C29 H29A 1.02(2) . ? C29 H29B 0.89(3) . ? C30 H30A 1.04(2) . ? C30 H30B 0.92(3) . ? C31 C32 1.469(4) . ? C31 H31A 0.90(3) . ? C31 H31B 0.92(3) . ? C32 H32A 0.96(3) . ? C32 H32B 0.96(3) . ? N41 C41 1.336(3) . ? N41 C45 1.342(3) . ? C41 C42 1.380(4) . ? C41 H41 0.93(2) . ? C42 C43 1.368(4) . ? C42 H42 0.92(3) . ? C43 C44 1.367(4) . ? C43 H43 0.93(2) . ? C44 C45 1.373(3) . ? C44 H44 0.85(3) . ? C45 H45 0.94(2) . ? N51 C52 1.276(7) 3_766 ? N51 C51 1.403(6) . ? C51 C53 1.280(8) 3_766 ? C51 C52 1.356(4) . ? C51 H51 0.83(3) . ? C52 N51 1.276(7) 3_766 ? C52 C53 1.405(8) . ? C52 K1 3.488(3) 3_766 ? C52 H52 0.77(3) . ? C53 C51 1.280(8) 3_766 ? C53 K1 3.119(8) 3_766 ? C53 H53 1.000(17) . ? 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 Nd1 O2 121.41(5) . . ? O1 Nd1 N2 128.51(5) . . ? O2 Nd1 N2 74.18(5) . . ? O1 Nd1 N1 73.29(5) . . ? O2 Nd1 N1 127.92(5) . . ? N2 Nd1 N1 62.05(6) . . ? O1 Nd1 N1 146.14(5) . 3_765 ? O2 Nd1 N1 92.08(5) . 3_765 ? N2 Nd1 N1 61.35(5) . 3_765 ? N1 Nd1 N1 90.64(5) . 3_765 ? O1 Nd1 N2 89.37(5) . 3_765 ? O2 Nd1 N2 148.92(5) . 3_765 ? N2 Nd1 N2 90.47(5) . 3_765 ? N1 Nd1 N2 61.09(5) . 3_765 ? N1 Nd1 N2 56.91(5) 3_765 3_765 ? O1 Nd1 C13 97.76(6) . 3_765 ? O2 Nd1 C13 129.77(6) . 3_765 ? N2 Nd1 C13 106.57(6) . 3_765 ? N1 Nd1 C13 90.56(6) . 3_765 ? N1 Nd1 C13 51.80(6) 3_765 3_765 ? N2 Nd1 C13 29.48(5) 3_765 3_765 ? O1 Nd1 C8 127.01(6) . 3_765 ? O2 Nd1 C8 100.68(6) . 3_765 ? N2 Nd1 C8 90.80(6) . 3_765 ? N1 Nd1 C8 106.46(6) . 3_765 ? N1 Nd1 C8 29.46(5) 3_765 3_765 ? N2 Nd1 C8 51.73(6) 3_765 3_765 ? C13 Nd1 C8 30.64(6) 3_765 3_765 ? O1 Nd1 N41 71.56(5) . . ? O2 Nd1 N41 74.52(5) . . ? N2 Nd1 N41 148.63(6) . . ? N1 Nd1 N41 144.77(6) . . ? N1 Nd1 N41 117.89(5) 3_765 . ? N2 Nd1 N41 115.91(5) 3_765 . ? C13 Nd1 N41 91.81(6) 3_765 . ? C8 Nd1 N41 92.84(6) 3_765 . ? O1 Nd1 Nd1 114.54(4) . 3_765 ? O2 Nd1 Nd1 116.57(4) . 3_765 ? N2 Nd1 Nd1 47.62(4) . 3_765 ? N1 Nd1 Nd1 47.48(4) . 3_765 ? N1 Nd1 Nd1 43.16(4) 3_765 3_765 ? N2 Nd1 Nd1 42.85(4) 3_765 3_765 ? C13 Nd1 Nd1 63.32(4) 3_765 3_765 ? C8 Nd1 Nd1 63.39(4) 3_765 3_765 ? N41 Nd1 Nd1 154.62(4) . 3_765 ? C1 O1 Nd1 138.67(13) . . ? C20 O2 Nd1 136.95(13) . . ? C8 N1 C7 123.72(17) . . ? C8 N1 Nd1 123.27(13) . . ? C7 N1 Nd1 112.96(12) . . ? C8 N1 Nd1 81.52(12) . 3_765 ? C7 N1 Nd1 102.30(12) . 3_765 ? Nd1 N1 Nd1 89.36(5) . 3_765 ? C13 N2 C14 123.65(17) . . ? C13 N2 Nd1 123.85(13) . . ? C14 N2 Nd1 112.43(12) . . ? C13 N2 Nd1 81.11(12) . 3_765 ? C14 N2 Nd1 103.08(12) . 3_765 ? Nd1 N2 Nd1 89.53(5) . 3_765 ? O1 C1 C2 121.3(2) . . ? O1 C1 C6 121.7(2) . . ? C2 C1 C6 117.0(2) . . ? C3 C2 C1 122.3(2) . . ? C3 C2 H1 122.1(17) . . ? C1 C2 H1 115.5(17) . . ? C2 C3 C4 120.6(2) . . ? C2 C3 H2 122.2(18) . . ? C4 C3 H2 117.2(18) . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H3 122.7(17) . . ? C5 C4 H3 118.5(17) . . ? C6 C5 C4 121.7(2) . . ? C6 C5 H4 119.8(14) . . ? C4 C5 H4 118.5(14) . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C7 122.1(2) . . ? C1 C6 C7 118.26(18) . . ? N1 C7 C6 112.92(18) . . ? N1 C7 C14 108.47(16) . 3_765 ? C6 C7 C14 109.42(16) . 3_765 ? N1 C7 H7 110.4(12) . . ? C6 C7 H7 107.3(13) . . ? C14 C7 H7 108.2(12) 3_765 . ? N1 C8 C9 129.6(2) . . ? N1 C8 C13 111.96(17) . . ? C9 C8 C13 118.30(18) . . ? N1 C8 Nd1 69.02(11) . 3_765 ? C9 C8 Nd1 120.59(15) . 3_765 ? C13 C8 Nd1 74.53(11) . 3_765 ? C10 C9 C8 121.2(2) . . ? C10 C9 H9 121.5(14) . . ? C8 C9 H9 117.3(14) . . ? C11 C10 C9 120.7(2) . . ? C11 C10 K1 75.19(14) . . ? C9 C10 K1 95.32(15) . . ? C11 C10 H10 123.7(14) . . ? C9 C10 H10 115.6(14) . . ? K1 C10 H10 102.8(15) . . ? C10 C11 C12 120.3(2) . . ? C10 C11 K1 79.24(14) . . ? C12 C11 K1 91.42(14) . . ? C10 C11 H11 123.2(14) . . ? C12 C11 H11 116.5(14) . . ? K1 C11 H11 99.2(14) . . ? C11 C12 C13 120.7(2) . . ? C11 C12 K1 64.59(13) . . ? C13 C12 K1 94.60(13) . . ? C11 C12 H12 117.1(13) . . ? C13 C12 H12 121.9(13) . . ? K1 C12 H12 105.0(15) . . ? N2 C13 C12 129.0(2) . . ? N2 C13 C8 112.02(17) . . ? C12 C13 C8 118.78(18) . . ? N2 C13 Nd1 69.41(11) . 3_765 ? C12 C13 Nd1 119.48(15) . 3_765 ? C8 C13 Nd1 74.83(11) . 3_765 ? N2 C14 C15 113.07(18) . . ? N2 C14 C7 108.57(16) . 3_765 ? C15 C14 C7 109.69(16) . 3_765 ? N2 C14 H14 111.2(12) . . ? C15 C14 H14 108.6(13) . . ? C7 C14 H14 105.5(12) 3_765 . ? C16 C15 C20 118.9(2) . . ? C16 C15 C14 121.36(19) . . ? C20 C15 C14 119.72(18) . . ? C15 C16 C17 123.2(2) . . ? C15 C16 H16 120.4(16) . . ? C17 C16 H16 116.4(16) . . ? C18 C17 C16 117.9(2) . . ? C18 C17 H17 118.1(16) . . ? C16 C17 H17 124.0(16) . . ? C17 C18 C19 121.0(2) . . ? C17 C18 H18 119.4(19) . . ? C19 C18 H18 119(2) . . ? C18 C19 C20 121.9(2) . . ? C18 C19 H19 124.1(14) . . ? C20 C19 H19 113.9(14) . . ? O2 C20 C19 121.34(19) . . ? O2 C20 C15 121.50(19) . . ? C19 C20 C15 117.12(19) . . ? O22 K1 O26 120.48(6) . . ? O22 K1 O25 163.51(6) . . ? O26 K1 O25 59.86(5) . . ? O22 K1 O24 118.14(5) . . ? O26 K1 O24 119.09(5) . . ? O25 K1 O24 59.26(5) . . ? O22 K1 O21 59.92(6) . . ? O26 K1 O21 60.62(5) . . ? O25 K1 O21 116.90(5) . . ? O24 K1 O21 162.30(5) . . ? O22 K1 O23 58.23(5) . . ? O26 K1 O23 161.71(6) . . ? O25 K1 O23 115.57(5) . . ? O24 K1 O23 60.03(5) . . ? O21 K1 O23 114.04(6) . . ? O22 K1 C11 101.66(6) . . ? O26 K1 C11 105.18(6) . . ? O25 K1 C11 93.68(6) . . ? O24 K1 C11 77.33(5) . . ? O21 K1 C11 120.31(5) . . ? O23 K1 C11 92.57(6) . . ? O22 K1 C53 92.93(15) . 3_766 ? O26 K1 C53 75.78(14) . 3_766 ? O25 K1 C53 70.90(15) . 3_766 ? O24 K1 C53 86.38(15) . 3_766 ? O21 K1 C53 76.34(15) . 3_766 ? O23 K1 C53 85.99(14) . 3_766 ? C11 K1 C53 161.88(15) . 3_766 ? O22 K1 C10 118.65(6) . . ? O26 K1 C10 79.87(6) . . ? O25 K1 C10 77.83(6) . . ? O24 K1 C10 86.42(5) . . ? O21 K1 C10 110.21(6) . . ? O23 K1 C10 117.45(6) . . ? C11 K1 C10 25.57(6) . . ? C53 K1 C10 147.08(14) 3_766 . ? O22 K1 N51 90.18(12) . . ? O26 K1 N51 76.51(13) . . ? O25 K1 N51 73.69(12) . . ? O24 K1 N51 88.39(10) . . ? O21 K1 N51 74.21(10) . . ? O23 K1 N51 85.21(13) . . ? C11 K1 N51 164.56(11) . . ? C53 K1 N51 2.9(2) 3_766 . ? C10 K1 N51 149.47(13) . . ? O22 K1 C12 78.36(6) . . ? O26 K1 C12 112.83(5) . . ? O25 K1 C12 117.42(6) . . ? O24 K1 C12 93.33(5) . . ? O21 K1 C12 103.01(5) . . ? O23 K1 C12 85.20(5) . . ? C11 K1 C12 24.00(5) . . ? C53 K1 C12 169.98(14) 3_766 . ? C10 K1 C12 42.72(6) . . ? N51 K1 C12 167.81(13) . . ? O22 K1 C52 70.46(6) . 3_766 ? O26 K1 C52 93.96(7) . 3_766 ? O25 K1 C52 93.08(6) . 3_766 ? O24 K1 C52 90.60(6) . 3_766 ? O21 K1 C52 72.02(6) . 3_766 ? O23 K1 C52 68.10(7) . 3_766 ? C11 K1 C52 160.56(7) . 3_766 ? C53 K1 C52 23.71(14) 3_766 3_766 ? C10 K1 C52 170.71(7) . 3_766 ? N51 K1 C52 21.41(13) . 3_766 ? C12 K1 C52 146.41(7) . 3_766 ? C32 O21 C21 111.6(2) . . ? C32 O21 K1 109.99(15) . . ? C21 O21 K1 107.69(16) . . ? C22 O22 C23 113.4(2) . . ? C22 O22 K1 118.74(18) . . ? C23 O22 K1 121.03(15) . . ? C24 O23 C25 113.9(2) . . ? C24 O23 K1 111.17(16) . . ? C25 O23 K1 111.81(14) . . ? C27 O24 C26 111.11(18) . . ? C27 O24 K1 117.59(14) . . ? C26 O24 K1 115.02(13) . . ? C28 O25 C29 113.1(2) . . ? C28 O25 K1 113.86(14) . . ? C29 O25 K1 114.02(13) . . ? C30 O26 C31 113.5(2) . . ? C30 O26 K1 116.82(14) . . ? C31 O26 K1 115.73(15) . . ? O21 C21 C22 109.7(2) . . ? O21 C21 K1 49.71(12) . . ? C22 C21 K1 83.33(16) . . ? O21 C21 H21A 112(2) . . ? C22 C21 H21A 112.4(19) . . ? K1 C21 H21A 86(2) . . ? O21 C21 H21B 107.0(16) . . ? C22 C21 H21B 113.2(17) . . ? K1 C21 H21B 156.2(16) . . ? H21A C21 H21B 102(2) . . ? O22 C22 C21 108.6(3) . . ? O22 C22 H22A 106.5(19) . . ? C21 C22 H22A 110.7(19) . . ? O22 C22 H22B 112.4(16) . . ? C21 C22 H22B 106.1(17) . . ? H22A C22 H22B 112(3) . . ? O22 C23 C24 108.5(3) . . ? O22 C23 H23A 103.6(16) . . ? C24 C23 H23A 111.4(17) . . ? O22 C23 H23B 108.4(17) . . ? C24 C23 H23B 108.7(17) . . ? H23A C23 H23B 116(2) . . ? O23 C24 C23 108.4(2) . . ? O23 C24 H24A 114.5(16) . . ? C23 C24 H24A 106.0(16) . . ? O23 C24 H24B 108.3(17) . . ? C23 C24 H24B 112.4(19) . . ? H24A C24 H24B 107(2) . . ? O23 C25 C26 109.6(2) . . ? O23 C25 H25A 104.5(15) . . ? C26 C25 H25A 117.4(16) . . ? O23 C25 H25B 108.5(18) . . ? C26 C25 H25B 112.3(16) . . ? H25A C25 H25B 104(2) . . ? O24 C26 C25 109.7(2) . . ? O24 C26 H26A 109.1(15) . . ? C25 C26 H26A 111.2(14) . . ? O24 C26 H26B 107.7(18) . . ? C25 C26 H26B 113.0(18) . . ? H26A C26 H26B 106(2) . . ? O24 C27 C28 109.48(18) . . ? O24 C27 H27A 109(2) . . ? C28 C27 H27A 111(2) . . ? O24 C27 H27B 110.1(13) . . ? C28 C27 H27B 111.2(12) . . ? H27A C27 H27B 106(2) . . ? O25 C28 C27 108.7(2) . . ? O25 C28 H28A 107.5(13) . . ? C27 C28 H28A 113.1(13) . . ? O25 C28 H28B 107.0(16) . . ? C27 C28 H28B 110.4(16) . . ? H28A C28 H28B 110(2) . . ? O25 C29 C30 108.5(2) . . ? O25 C29 H29A 110.7(13) . . ? C30 C29 H29A 109.7(13) . . ? O25 C29 H29B 104.8(17) . . ? C30 C29 H29B 115.7(19) . . ? H29A C29 H29B 107(2) . . ? O26 C30 C29 110.1(2) . . ? O26 C30 H30A 112.9(13) . . ? C29 C30 H30A 107.3(13) . . ? O26 C30 H30B 113.4(18) . . ? C29 C30 H30B 105(2) . . ? H30A C30 H30B 108(2) . . ? O26 C31 C32 109.8(2) . . ? O26 C31 H31A 107.6(19) . . ? C32 C31 H31A 111.0(17) . . ? O26 C31 H31B 109.0(19) . . ? C32 C31 H31B 112.2(19) . . ? H31A C31 H31B 107(3) . . ? O21 C32 C31 109.9(2) . . ? O21 C32 H32A 108.6(19) . . ? C31 C32 H32A 109.2(18) . . ? O21 C32 H32B 109.5(19) . . ? C31 C32 H32B 111.4(18) . . ? H32A C32 H32B 108(2) . . ? C41 N41 C45 116.5(2) . . ? C41 N41 Nd1 123.83(16) . . ? C45 N41 Nd1 119.36(14) . . ? N41 C41 C42 123.4(2) . . ? N41 C41 H41 115.3(13) . . ? C42 C41 H41 121.3(13) . . ? C43 C42 C41 118.9(2) . . ? C43 C42 H42 123.2(19) . . ? C41 C42 H42 118.0(19) . . ? C44 C43 C42 118.7(2) . . ? C44 C43 H43 120.6(15) . . ? C42 C43 H43 120.7(15) . . ? C43 C44 C45 119.3(2) . . ? C43 C44 H44 125.5(18) . . ? C45 C44 H44 115.3(18) . . ? N41 C45 C44 123.2(2) . . ? N41 C45 H45 114.6(14) . . ? C44 C45 H45 122.0(14) . . ? C52 N51 C51 117.8(5) 3_766 . ? C52 N51 K1 94.0(3) 3_766 . ? C51 N51 K1 107.5(3) . . ? C53 C51 C52 122.8(4) 3_766 . ? C53 C51 N51 4.5(6) 3_766 . ? C52 C51 N51 119.3(4) . . ? C53 C51 H51 123(2) 3_766 . ? C52 C51 H51 114(2) . . ? N51 C51 H51 126(2) . . ? N51 C52 C51 122.7(3) 3_766 . ? N51 C52 C53 4.2(5) 3_766 . ? C51 C52 C53 119.7(4) . . ? N51 C52 K1 64.6(3) 3_766 3_766 ? C51 C52 K1 125.4(2) . 3_766 ? C53 C52 K1 63.3(4) . 3_766 ? N51 C52 H52 117(2) 3_766 . ? C51 C52 H52 120(2) . . ? C53 C52 H52 120(2) . . ? K1 C52 H52 80(2) 3_766 . ? C51 C53 C52 117.4(6) 3_766 . ? C51 C53 K1 113.9(5) 3_766 3_766 ? C52 C53 K1 93.0(4) . 3_766 ? C51 C53 H53 134(2) 3_766 . ? C52 C53 H53 108(3) . . ? K1 C53 H53 68(2) 3_766 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.158 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.103