# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 856406' _vrf_CHEMW03_1 ; PROBLEM: The ratio of given/expected molecular weight as RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 21 H2O molecules per formula unit that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT043_1 ; PROBLEM: Check Reported Molecular Weight ................ 2346.53 RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 21 H2O molecules per formula unit that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT420_1 ; PROBLEM: D-H Without Acceptor RESPONSE: These are bridging hydroxide moieties or protonated NN bridges, within the Dy4 grid. ; _vrf_PLAT041_1 ; PROBLEM: Calc. and Reported SumFormula Strings Differ ? RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 21 H2O molecules per formula unit that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT051_1 ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 1.07 Perc. RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 21 H2O molecules per formula unit that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT068_1 ; PROBLEM: Reported F000 Differs from Calcd (or Missing)... ? RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 21 H2O molecules per formula unit that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_FORMU01_1 ; PROBLEM: There is a discrepancy between the atom counts in the RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 21 H2O molecules per formula unit that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_CELLZ01_1 ; PROBLEM: Difference between formula and atom_site contents detected. RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 21 H2O molecules per formula unit that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT002_1 ; PROBLEM: Number of Distance or Angle Restraints on AtSite 16 RESPONSE: H5, H6, H7, H8, H13, H14, H15 and H16 (the bridging hydroxide H-atoms) were located in difference map positions and refined positionally with DFIX restraints, and with Uiso = 1.5Ueq of their parent O-atom. Please see iucr_refine_instructions_details for full information. ; _vrf_PLAT606_1 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details. ; _vrf_PLAT860_1 ; PROBLEM: Note: Number of Least-Squares Restraints ....... 8 RESPONSE: H5, H6, H7, H8, H13, H14, H15 and H16 (the bridging hydroxide H-atoms) were located in difference map positions and refined positionally with DFIX restraints, and with Uiso = 1.5Ueq of their parent O-atom. Please see iucr_refine_instructions_details for full information. ; _vrf_PLAT869_1 ; PROBLEM: ALERTS Related to the use of SQUEEZE Suppressed ! RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H62 Dy4 N24 O8, 2(Cl), 21(H2 O)' _chemical_formula_sum 'C60 H104 Cl2 Dy4 N24 O29' _chemical_formula_weight 2346.53 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' Dy Dy -0.1892 4.4098 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.7717(7) _cell_length_b 22.2755(8) _cell_length_c 27.8431(19) _cell_angle_alpha 110.343(8) _cell_angle_beta 95.225(7) _cell_angle_gamma 106.955(8) _cell_volume 9655.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 57310 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4648 _exptl_absorpt_coefficient_mu 3.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.332 _exptl_absorpt_correction_T_max 0.550 _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 39537 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 26.50 _reflns_number_total 39537 _reflns_number_gt 28920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_structure_solution 'SHELXS-97: Acta Cryst.2008, A64, 112-122' _computing_structure_refinement 'SHELXL-97: Acta Cryst.2008, A64, 112-122' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' _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. All H-atoms were introduced in calculated positions and refined on a riding model, except H5, H6, H7, H8, H13, H14, H15 and H16 (the bridging hydroxide H-atoms) which were located in difference map positions and refined positionally with DFIX restraints, and with Uiso = 1.5Ueq of their parent O-atom. Please see iucr_refine_instructions_details for full information. For charge balance purposes the formula is: [(L-2H)2(L-H)2Dy4(OH)4]Cl2(H2O)21 = 2(-2) + 2(-1) + 4(+3) + 4(-1) + 2(-1) = -4 -2 + 12 -4 -2 = 0 ; _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^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 39537 _refine_ls_number_parameters 1805 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.015 0.489 -0.004 3684 840 '21 H2O/Formula Unit ' _platon_squeeze_details ; The Platon SQUEEZE procedure was applied to recover 840 electrons per unit cell in one void (total volume 3684 ^A^3); that is 210 electrons per formula unit. Lattice solvent water molecules (10 electrons/H2O) were present, and the electrons recovered by SQUEEZE have been assigned as 21 water molecules per formula unit. These water molecules have been included in the formula for the calculation of intensive properties. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13. ; 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 Dy1 Dy -0.065854(18) 0.733334(14) 0.234120(12) 0.04326(8) Uani 1 1 d . . . Dy2 Dy -0.070800(17) 0.611535(14) 0.301344(12) 0.04197(8) Uani 1 1 d . . . Dy3 Dy 0.140905(19) 0.847467(14) 0.318754(12) 0.04601(9) Uani 1 1 d . . . Dy4 Dy 0.136066(18) 0.724429(14) 0.384258(12) 0.04348(8) Uani 1 1 d . . . Dy5 Dy 0.247318(18) 0.229026(14) 0.089422(11) 0.03985(8) Uani 1 1 d . . . Dy6 Dy 0.360585(16) 0.120262(13) 0.115565(11) 0.03557(7) Uani 1 1 d . . . Dy7 Dy 0.330733(16) 0.358013(13) 0.229383(10) 0.03491(7) Uani 1 1 d . . . Dy8 Dy 0.438648(18) 0.245832(14) 0.256423(11) 0.04058(8) Uani 1 1 d . . . Cl1 Cl 0.1278(2) 0.63499(14) 0.20005(12) 0.1132(9) Uani 1 1 d . . . Cl2 Cl -0.3298(3) 0.76599(18) 0.46250(19) 0.1903(19) Uani 1 1 d . . . Cl3 Cl 0.5160(3) 0.3198(3) 0.1228(2) 0.217(2) Uani 1 1 d . . . Cl4 Cl 0.1562(2) 1.14757(15) 0.21108(13) 0.1160(9) Uani 1 1 d . . . O1 O -0.0848(3) 0.61963(19) 0.22042(16) 0.0486(11) Uani 1 1 d . . . O2 O 0.2095(3) 0.7805(2) 0.33775(17) 0.0472(11) Uani 1 1 d . . . O3 O 0.0100(3) 0.8444(2) 0.29245(17) 0.0521(11) Uani 1 1 d . . . O4 O 0.0040(3) 0.6702(2) 0.38776(17) 0.0481(11) Uani 1 1 d . . . O5 O -0.0887(3) 0.7100(2) 0.30575(17) 0.0485(11) Uani 1 1 d D . . H5 H -0.099(4) 0.735(3) 0.3346(17) 0.073 Uiso 1 1 d D . . O6 O 0.0957(3) 0.8102(2) 0.38027(17) 0.0519(12) Uani 1 1 d D . . H6 H 0.062(4) 0.829(4) 0.395(3) 0.078 Uiso 1 1 d D . . O7 O 0.0679(3) 0.75461(19) 0.24628(16) 0.0425(10) Uani 1 1 d D . . H7 H 0.082(4) 0.724(3) 0.223(2) 0.064 Uiso 1 1 d D . . O8 O 0.0628(2) 0.64258(19) 0.30492(16) 0.0413(10) Uani 1 1 d D . . H8 H 0.070(4) 0.632(3) 0.2728(12) 0.062 Uiso 1 1 d D . . O9 O 0.2340(2) 0.11913(18) 0.08407(15) 0.0381(9) Uani 1 1 d . . . O10 O 0.3492(3) 0.3022(2) 0.28438(15) 0.0426(10) Uani 1 1 d . . . O11 O 0.3189(3) 0.34510(18) 0.14186(15) 0.0434(10) Uani 1 1 d . . . O12 O 0.4778(2) 0.1882(2) 0.18163(16) 0.0446(10) Uani 1 1 d . . . O13 O 0.3659(2) 0.2119(2) 0.09614(16) 0.0427(9) Uani 1 1 d D . . H13 H 0.410(3) 0.247(2) 0.101(3) 0.064 Uiso 1 1 d D . . O14 O 0.4385(2) 0.32293(19) 0.22101(14) 0.0357(9) Uani 1 1 d D . . H14 H 0.459(4) 0.325(3) 0.1947(17) 0.054 Uiso 1 1 d D . . O15 O 0.2357(2) 0.25818(19) 0.17352(15) 0.0395(9) Uani 1 1 d D . . H15 H 0.196(3) 0.233(3) 0.182(3) 0.059 Uiso 1 1 d D . . O16 O 0.3342(2) 0.15856(19) 0.19651(15) 0.0362(9) Uani 1 1 d D . . H16 H 0.292(2) 0.154(3) 0.210(2) 0.054 Uiso 1 1 d D . . N1 N -0.0591(3) 0.7822(3) 0.1641(2) 0.0578(15) Uani 1 1 d . . . N2 N -0.0716(3) 0.6539(3) 0.1422(2) 0.0526(14) Uani 1 1 d . . . N3 N -0.0768(4) 0.5867(3) 0.1325(2) 0.0549(14) Uani 1 1 d . . . N4 N -0.0763(4) 0.5153(3) 0.1744(2) 0.0619(16) Uani 1 1 d . . . N5 N -0.0743(3) 0.5090(2) 0.2227(2) 0.0479(13) Uani 1 1 d . . . N6 N -0.0688(3) 0.5056(2) 0.3174(2) 0.0531(15) Uani 1 1 d . . . N7 N 0.1904(4) 0.9243(3) 0.2695(2) 0.0636(18) Uani 1 1 d . . . N8 N 0.2640(4) 0.8409(3) 0.2810(2) 0.0577(16) Uani 1 1 d . . . N9 N 0.2985(3) 0.7951(3) 0.2860(2) 0.0615(16) Uani 1 1 d . . . N10 N 0.2903(3) 0.7156(3) 0.3216(2) 0.0541(15) Uani 1 1 d . . . N11 N 0.2517(3) 0.6884(3) 0.3531(2) 0.0538(15) Uani 1 1 d . . . N12 N 0.1700(4) 0.6386(3) 0.4151(2) 0.0617(18) Uani 1 1 d . . . N13 N -0.2163(3) 0.6894(3) 0.1935(2) 0.0605(16) Uani 1 1 d . . . N14 N -0.1388(4) 0.8172(3) 0.2638(2) 0.0628(16) Uani 1 1 d . . . N15 N -0.0974(4) 0.8807(3) 0.3028(3) 0.0742(19) Uani 1 1 d . . . N16 N 0.0294(5) 0.9487(3) 0.3573(3) 0.086(2) Uani 1 1 d . . . H16A H 0.0126 0.9823 0.3736 0.103 Uiso 1 1 calc R . . N17 N 0.1075(5) 0.9510(3) 0.3694(2) 0.0679(19) Uani 1 1 d . . . N18 N 0.2558(4) 0.9479(3) 0.3890(2) 0.0660(19) Uani 1 1 d . . . N19 N -0.2211(3) 0.5430(3) 0.2751(2) 0.0537(14) Uani 1 1 d . . . N20 N -0.1479(3) 0.6205(3) 0.3741(2) 0.0504(13) Uani 1 1 d . . . N21 N -0.1070(4) 0.6654(3) 0.4250(2) 0.0587(15) Uani 1 1 d . . . N22 N 0.0184(4) 0.7363(3) 0.4743(2) 0.0668(18) Uani 1 1 d . . . H22 H -0.0003 0.7499 0.5029 0.080 Uiso 1 1 calc R . . N23 N 0.0996(4) 0.7606(3) 0.4719(2) 0.0623(17) Uani 1 1 d . . . N24 N 0.2500(4) 0.8070(3) 0.4623(2) 0.0621(18) Uani 1 1 d . . . N25 N 0.1308(3) 0.2680(3) 0.07152(19) 0.0488(13) Uani 1 1 d . . . N26 N 0.1048(3) 0.1430(3) 0.0683(2) 0.0483(13) Uani 1 1 d . . . N27 N 0.0973(3) 0.0790(3) 0.0671(2) 0.0512(14) Uani 1 1 d . . . H27 H 0.0504 0.0462 0.0588 0.061 Uiso 1 1 calc R . . N28 N 0.1640(3) 0.0136(2) 0.0830(2) 0.0483(13) Uani 1 1 d . . . N29 N 0.2421(3) 0.0146(2) 0.0971(2) 0.0448(12) Uani 1 1 d . . . N30 N 0.3917(3) 0.0230(3) 0.1300(2) 0.0483(13) Uani 1 1 d . . . N31 N 0.2380(3) 0.4280(2) 0.2365(2) 0.0478(13) Uani 1 1 d . . . N32 N 0.2388(3) 0.3534(2) 0.29376(19) 0.0407(11) Uani 1 1 d . . . N33 N 0.2403(3) 0.3118(3) 0.3204(2) 0.0512(13) Uani 1 1 d . . . N34 N 0.3012(4) 0.2405(3) 0.3330(2) 0.0576(15) Uani 1 1 d . . . H34 H 0.2684 0.2296 0.3530 0.069 Uiso 1 1 calc R . . N35 N 0.3615(4) 0.2134(3) 0.3203(2) 0.0522(14) Uani 1 1 d . . . N36 N 0.4789(4) 0.1667(3) 0.2924(2) 0.0685(19) Uani 1 1 d . . . N37 N 0.2240(4) 0.1753(3) -0.0115(2) 0.0552(15) Uani 1 1 d . . . N38 N 0.3089(4) 0.3073(3) 0.0433(2) 0.0541(15) Uani 1 1 d . . . N39 N 0.3531(4) 0.3753(3) 0.0744(2) 0.0577(16) Uani 1 1 d . . . N40 N 0.4145(3) 0.4511(2) 0.1589(2) 0.0506(14) Uani 1 1 d . . . N41 N 0.4149(3) 0.4567(2) 0.21068(19) 0.0429(12) Uani 1 1 d . . . N42 N 0.4155(3) 0.4662(2) 0.3092(2) 0.0467(13) Uani 1 1 d . . . N43 N 0.3575(3) 0.0474(3) 0.0212(2) 0.0495(13) Uani 1 1 d . . . N44 N 0.4941(3) 0.1362(3) 0.0879(2) 0.0556(14) Uani 1 1 d . . . N45 N 0.5637(3) 0.1861(3) 0.1240(2) 0.0636(16) Uani 1 1 d . . . N46 N 0.6083(3) 0.2595(3) 0.2097(3) 0.0654(17) Uani 1 1 d . . . N47 N 0.5862(3) 0.2863(3) 0.2568(2) 0.0604(16) Uani 1 1 d . . . N48 N 0.5351(4) 0.3365(3) 0.3417(2) 0.0641(17) Uani 1 1 d . . . C1 C -0.0451(5) 0.8485(4) 0.1746(3) 0.062(2) Uani 1 1 d . . . H1 H -0.0403 0.8774 0.2099 0.074 Uiso 1 1 calc R . . C2 C -0.0373(6) 0.8778(4) 0.1392(3) 0.081(3) Uani 1 1 d . . . H2 H -0.0310 0.9246 0.1490 0.098 Uiso 1 1 calc R . . C3 C -0.0391(6) 0.8359(5) 0.0870(4) 0.090(3) Uani 1 1 d . . . H3 H -0.0298 0.8548 0.0613 0.108 Uiso 1 1 calc R . . C4 C -0.0545(6) 0.7680(4) 0.0746(3) 0.081(3) Uani 1 1 d . . . H4 H -0.0603 0.7385 0.0392 0.097 Uiso 1 1 calc R . . C5 C -0.0618(4) 0.7415(3) 0.1130(3) 0.0545(17) Uani 1 1 d . . . C6 C -0.0721(5) 0.6711(4) 0.1028(3) 0.0614(19) Uani 1 1 d . . . C7 C -0.0804(7) 0.6215(4) 0.0465(3) 0.103(4) Uani 1 1 d . . . H7A H -0.0315 0.6372 0.0340 0.123 Uiso 1 1 calc R . . H7B H -0.1270 0.6197 0.0236 0.123 Uiso 1 1 calc R . . H7C H -0.0880 0.5758 0.0459 0.123 Uiso 1 1 calc R . . C8 C -0.0792(4) 0.5761(3) 0.1767(3) 0.0537(17) Uani 1 1 d . . . C9 C -0.0624(5) 0.3959(3) 0.1783(3) 0.075(2) Uani 1 1 d . . . H9A H -0.1025 0.3523 0.1736 0.090 Uiso 1 1 calc R . . H9B H -0.0083 0.3936 0.1843 0.090 Uiso 1 1 calc R . . H9C H -0.0714 0.4053 0.1468 0.090 Uiso 1 1 calc R . . C10 C -0.0700(4) 0.4522(3) 0.2249(3) 0.0574(18) Uani 1 1 d . . . C11 C -0.0705(4) 0.4492(3) 0.2769(3) 0.0552(18) Uani 1 1 d . . . C12 C -0.0686(4) 0.3910(3) 0.2849(3) 0.0600(19) Uani 1 1 d . . . H12 H -0.0695 0.3523 0.2560 0.072 Uiso 1 1 calc R . . C13 C -0.0656(4) 0.3887(4) 0.3330(4) 0.067(2) Uani 1 1 d . . . H13A H -0.0640 0.3492 0.3383 0.081 Uiso 1 1 calc R . . C14 C -0.0651(4) 0.4466(4) 0.3744(4) 0.068(2) Uani 1 1 d . . . H14A H -0.0636 0.4467 0.4086 0.082 Uiso 1 1 calc R . . C15 C -0.0668(4) 0.5035(3) 0.3659(3) 0.0532(17) Uani 1 1 d . . . H15A H -0.0665 0.5423 0.3946 0.064 Uiso 1 1 calc R . . C16 C 0.1506(5) 0.9645(3) 0.2625(3) 0.066(2) Uani 1 1 d . . . H16B H 0.0999 0.9600 0.2721 0.079 Uiso 1 1 calc R . . C17 C 0.1816(7) 1.0133(4) 0.2413(3) 0.086(3) Uani 1 1 d . . . H17 H 0.1523 1.0409 0.2364 0.104 Uiso 1 1 calc R . . C18 C 0.2538(7) 1.0198(4) 0.2280(3) 0.082(3) Uani 1 1 d . . . H18 H 0.2767 1.0532 0.2147 0.099 Uiso 1 1 calc R . . C19 C 0.2937(6) 0.9785(4) 0.2338(3) 0.077(3) Uani 1 1 d . . . H19 H 0.3441 0.9832 0.2238 0.093 Uiso 1 1 calc R . . C20 C 0.2636(5) 0.9300(4) 0.2537(3) 0.061(2) Uani 1 1 d . . . C21 C 0.3012(5) 0.8820(4) 0.2597(3) 0.063(2) Uani 1 1 d . . . C22 C 0.3791(5) 0.8827(5) 0.2432(4) 0.085(3) Uani 1 1 d . . . H22A H 0.4160 0.8811 0.2707 0.102 Uiso 1 1 calc R . . H22B H 0.4031 0.9246 0.2375 0.102 Uiso 1 1 calc R . . H22C H 0.3692 0.8430 0.2106 0.102 Uiso 1 1 calc R . . C23 C 0.2641(4) 0.7641(4) 0.3146(3) 0.0554(18) Uani 1 1 d . . . C24 C 0.3396(5) 0.6175(4) 0.3427(4) 0.080(3) Uani 1 1 d . . . H24A H 0.3520 0.6319 0.3140 0.096 Uiso 1 1 calc R . . H24B H 0.3215 0.5676 0.3296 0.096 Uiso 1 1 calc R . . H24C H 0.3881 0.6372 0.3707 0.096 Uiso 1 1 calc R . . C25 C 0.2735(4) 0.6419(3) 0.3641(3) 0.0571(19) Uani 1 1 d . . . C26 C 0.2315(4) 0.6155(3) 0.3994(3) 0.059(2) Uani 1 1 d . . . C27 C 0.2514(5) 0.5693(4) 0.4176(3) 0.074(2) Uani 1 1 d . . . H27A H 0.2948 0.5547 0.4073 0.089 Uiso 1 1 calc R . . C28 C 0.2111(7) 0.5459(5) 0.4486(4) 0.100(4) Uani 1 1 d . . . H28 H 0.2254 0.5145 0.4602 0.120 Uiso 1 1 calc R . . C29 C 0.1486(7) 0.5667(4) 0.4643(4) 0.086(3) Uani 1 1 d . . . H29 H 0.1191 0.5500 0.4865 0.104 Uiso 1 1 calc R . . C30 C 0.1292(6) 0.6136(4) 0.4465(3) 0.077(3) Uani 1 1 d . . . H30 H 0.0859 0.6280 0.4571 0.093 Uiso 1 1 calc R . . C31 C -0.2551(4) 0.6257(4) 0.1598(3) 0.067(2) Uani 1 1 d . . . H31 H -0.2259 0.5954 0.1501 0.080 Uiso 1 1 calc R . . C32 C -0.3385(5) 0.6011(5) 0.1379(4) 0.091(3) Uani 1 1 d . . . H32 H -0.3652 0.5548 0.1146 0.109 Uiso 1 1 calc R . . C33 C -0.3799(5) 0.6458(6) 0.1510(4) 0.092(3) Uani 1 1 d . . . H33 H -0.4359 0.6310 0.1367 0.110 Uiso 1 1 calc R . . C34 C -0.3398(5) 0.7109(6) 0.1844(4) 0.082(3) Uani 1 1 d . . . H34A H -0.3673 0.7427 0.1929 0.098 Uiso 1 1 calc R . . C35 C -0.2592(5) 0.7318(5) 0.2064(3) 0.072(2) Uani 1 1 d . . . C36 C -0.2134(5) 0.8047(5) 0.2448(3) 0.074(2) Uani 1 1 d . . . C37 C -0.2545(6) 0.8563(5) 0.2598(5) 0.117(4) Uani 1 1 d . . . H37A H -0.2540 0.8715 0.2974 0.141 Uiso 1 1 calc R . . H37B H -0.3103 0.8358 0.2398 0.141 Uiso 1 1 calc R . . H37C H -0.2261 0.8956 0.2520 0.141 Uiso 1 1 calc R . . C38 C -0.0193(5) 0.8895(3) 0.3175(3) 0.062(2) Uani 1 1 d . . . C39 C 0.1368(8) 1.0678(4) 0.4347(4) 0.122(4) Uani 1 1 d . . . H39A H 0.0989 1.0726 0.4096 0.147 Uiso 1 1 calc R . . H39B H 0.1852 1.1088 0.4490 0.147 Uiso 1 1 calc R . . H39C H 0.1114 1.0618 0.4633 0.147 Uiso 1 1 calc R . . C40 C 0.1598(7) 1.0057(3) 0.4069(3) 0.081(3) Uani 1 1 d . . . C41 C 0.2410(6) 1.0031(4) 0.4182(3) 0.073(2) Uani 1 1 d . . . C42 C 0.3009(7) 1.0599(4) 0.4607(3) 0.087(3) Uani 1 1 d . . . H42 H 0.2883 1.0985 0.4807 0.104 Uiso 1 1 calc R . . C43 C 0.3718(8) 1.0575(5) 0.4713(4) 0.110(4) Uani 1 1 d . . . H43 H 0.4112 1.0942 0.4998 0.132 Uiso 1 1 calc R . . C44 C 0.3921(6) 0.9997(5) 0.4404(4) 0.110(4) Uani 1 1 d . . . H44 H 0.4443 0.9977 0.4477 0.131 Uiso 1 1 calc R . . C45 C 0.3313(5) 0.9468(4) 0.3990(3) 0.073(3) Uani 1 1 d . . . H45 H 0.3435 0.9089 0.3773 0.088 Uiso 1 1 calc R . . C46 C -0.2580(4) 0.5023(3) 0.2248(3) 0.0603(19) Uani 1 1 d . . . H46 H -0.2279 0.5039 0.1985 0.072 Uiso 1 1 calc R . . C47 C -0.3376(4) 0.4583(4) 0.2091(4) 0.071(2) Uani 1 1 d . . . H47 H -0.3613 0.4309 0.1731 0.085 Uiso 1 1 calc R . . C48 C -0.3795(5) 0.4557(4) 0.2463(4) 0.087(3) Uani 1 1 d . . . H48 H -0.4334 0.4248 0.2368 0.105 Uiso 1 1 calc R . . C49 C -0.3453(4) 0.4975(4) 0.2982(4) 0.075(2) Uani 1 1 d . . . H49 H -0.3754 0.4964 0.3246 0.090 Uiso 1 1 calc R . . C50 C -0.2650(4) 0.5419(3) 0.3115(3) 0.0604(19) Uani 1 1 d . . . C51 C -0.2241(4) 0.5889(3) 0.3676(3) 0.0544(17) Uani 1 1 d . . . C52 C -0.2693(5) 0.5988(4) 0.4104(3) 0.083(3) Uani 1 1 d . . . H52A H -0.3085 0.5548 0.4057 0.100 Uiso 1 1 calc R . . H52B H -0.2976 0.6302 0.4093 0.100 Uiso 1 1 calc R . . H52C H -0.2316 0.6180 0.4443 0.100 Uiso 1 1 calc R . . C53 C -0.0268(4) 0.6900(3) 0.4279(3) 0.0479(16) Uani 1 1 d . . . C54 C 0.1253(7) 0.8335(5) 0.5653(4) 0.137(5) Uani 1 1 d . . . H54A H 0.0872 0.7948 0.5697 0.165 Uiso 1 1 calc R . . H54B H 0.0997 0.8671 0.5660 0.165 Uiso 1 1 calc R . . H54C H 0.1731 0.8547 0.5940 0.165 Uiso 1 1 calc R . . C55 C 0.1497(6) 0.8088(4) 0.5142(3) 0.082(3) Uani 1 1 d . . . C56 C 0.2330(5) 0.8345(4) 0.5093(3) 0.075(3) Uani 1 1 d . . . C57 C 0.2916(6) 0.8868(5) 0.5515(3) 0.100(4) Uani 1 1 d . . . H57 H 0.2789 0.9059 0.5846 0.120 Uiso 1 1 calc R . . C58 C 0.3710(7) 0.9107(5) 0.5436(4) 0.109(4) Uani 1 1 d . . . H58 H 0.4121 0.9473 0.5712 0.130 Uiso 1 1 calc R . . C59 C 0.3871(5) 0.8809(5) 0.4969(4) 0.094(3) Uani 1 1 d . . . H59 H 0.4403 0.8956 0.4915 0.113 Uiso 1 1 calc R . . C60 C 0.3271(5) 0.8293(4) 0.4567(3) 0.069(2) Uani 1 1 d . . . H60 H 0.3400 0.8085 0.4240 0.083 Uiso 1 1 calc R . . C61 C 0.1422(5) 0.3335(4) 0.0773(3) 0.062(2) Uani 1 1 d . . . H61 H 0.1957 0.3638 0.0839 0.074 Uiso 1 1 calc R . . C62 C 0.0790(6) 0.3583(4) 0.0739(3) 0.074(3) Uani 1 1 d . . . H62 H 0.0901 0.4048 0.0793 0.089 Uiso 1 1 calc R . . C63 C 0.0011(6) 0.3151(5) 0.0629(3) 0.081(3) Uani 1 1 d . . . H63 H -0.0424 0.3311 0.0596 0.097 Uiso 1 1 calc R . . C64 C -0.0135(5) 0.2478(4) 0.0565(3) 0.066(2) Uani 1 1 d . . . H64 H -0.0670 0.2171 0.0492 0.079 Uiso 1 1 calc R . . C65 C 0.0536(5) 0.2258(4) 0.0611(2) 0.0572(19) Uani 1 1 d . . . C66 C 0.0401(4) 0.1559(3) 0.0579(2) 0.0523(17) Uani 1 1 d . . . C67 C -0.0442(4) 0.1047(4) 0.0444(3) 0.070(2) Uani 1 1 d . . . H67A H -0.0442 0.0589 0.0240 0.084 Uiso 1 1 calc R . . H67B H -0.0808 0.1164 0.0236 0.084 Uiso 1 1 calc R . . H67C H -0.0624 0.1055 0.0767 0.084 Uiso 1 1 calc R . . C68 C 0.1677(3) 0.0707(3) 0.0797(2) 0.0425(14) Uani 1 1 d . . . C69 C 0.1804(5) -0.1054(4) 0.0866(4) 0.086(3) Uani 1 1 d . . . H69A H 0.1304 -0.0999 0.0743 0.103 Uiso 1 1 calc R . . H69B H 0.1773 -0.1142 0.1186 0.103 Uiso 1 1 calc R . . H69C H 0.1879 -0.1440 0.0594 0.103 Uiso 1 1 calc R . . C70 C 0.2493(4) -0.0424(3) 0.0978(3) 0.0524(17) Uani 1 1 d . . . C71 C 0.3338(4) -0.0390(3) 0.1131(3) 0.0514(16) Uani 1 1 d . . . C72 C 0.3510(5) -0.0965(4) 0.1127(3) 0.067(2) Uani 1 1 d . . . H72 H 0.3095 -0.1400 0.0991 0.080 Uiso 1 1 calc R . . C73 C 0.4291(6) -0.0899(4) 0.1324(3) 0.071(2) Uani 1 1 d . . . H73 H 0.4419 -0.1285 0.1323 0.085 Uiso 1 1 calc R . . C74 C 0.4864(5) -0.0270(4) 0.1518(3) 0.063(2) Uani 1 1 d . . . H74 H 0.5397 -0.0205 0.1672 0.076 Uiso 1 1 calc R . . C75 C 0.4670(5) 0.0277(4) 0.1491(3) 0.0590(18) Uani 1 1 d . . . H75 H 0.5088 0.0710 0.1613 0.071 Uiso 1 1 calc R . . C76 C 0.2362(4) 0.4657(3) 0.2081(3) 0.0532(17) Uani 1 1 d . . . H76 H 0.2684 0.4636 0.1825 0.064 Uiso 1 1 calc R . . C77 C 0.1906(5) 0.5074(3) 0.2136(3) 0.069(2) Uani 1 1 d . . . H77 H 0.1916 0.5326 0.1921 0.082 Uiso 1 1 calc R . . C78 C 0.1441(4) 0.5121(4) 0.2501(4) 0.068(2) Uani 1 1 d . . . H78 H 0.1128 0.5410 0.2549 0.082 Uiso 1 1 calc R . . C79 C 0.1434(4) 0.4740(4) 0.2800(3) 0.068(2) Uani 1 1 d . . . H79 H 0.1119 0.4766 0.3059 0.082 Uiso 1 1 calc R . . C80 C 0.1901(4) 0.4308(3) 0.2719(3) 0.0495(16) Uani 1 1 d . . . C81 C 0.1909(4) 0.3874(3) 0.3030(3) 0.0521(16) Uani 1 1 d . . . C82 C 0.1365(5) 0.3829(4) 0.3401(3) 0.069(2) Uani 1 1 d . . . H82A H 0.0953 0.3373 0.3261 0.083 Uiso 1 1 calc R . . H82B H 0.1104 0.4171 0.3445 0.083 Uiso 1 1 calc R . . H82C H 0.1678 0.3915 0.3741 0.083 Uiso 1 1 calc R . . C83 C 0.2991(4) 0.2849(3) 0.3113(2) 0.0484(16) Uani 1 1 d . . . C84 C 0.3148(6) 0.1413(4) 0.3708(3) 0.088(3) Uani 1 1 d . . . H84A H 0.2668 0.1544 0.3690 0.105 Uiso 1 1 calc R . . H84B H 0.3441 0.1607 0.4073 0.105 Uiso 1 1 calc R . . H84C H 0.2985 0.0915 0.3570 0.105 Uiso 1 1 calc R . . C85 C 0.3687(6) 0.1682(4) 0.3383(3) 0.070(2) Uani 1 1 d . . . C86 C 0.4341(6) 0.1415(4) 0.3235(3) 0.067(2) Uani 1 1 d . . . C87 C 0.4514(7) 0.0948(4) 0.3418(4) 0.102(4) Uani 1 1 d . . . H87 H 0.4210 0.0791 0.3642 0.123 Uiso 1 1 calc R . . C88 C 0.5132(8) 0.0720(5) 0.3270(4) 0.112(4) Uani 1 1 d . . . H88 H 0.5238 0.0389 0.3382 0.134 Uiso 1 1 calc R . . C89 C 0.5608(7) 0.0966(5) 0.2958(4) 0.100(4) Uani 1 1 d . . . H89 H 0.6041 0.0818 0.2858 0.120 Uiso 1 1 calc R . . C90 C 0.5401(6) 0.1446(4) 0.2801(3) 0.074(2) Uani 1 1 d . . . H90 H 0.5719 0.1626 0.2594 0.089 Uiso 1 1 calc R . . C91 C 0.1912(5) 0.1094(4) -0.0384(3) 0.065(2) Uani 1 1 d . . . H91 H 0.1651 0.0821 -0.0209 0.077 Uiso 1 1 calc R . . C92 C 0.1919(6) 0.0766(4) -0.0908(3) 0.083(3) Uani 1 1 d . . . H92 H 0.1715 0.0282 -0.1075 0.099 Uiso 1 1 calc R . . C93 C 0.2218(7) 0.1145(5) -0.1171(3) 0.100(3) Uani 1 1 d . . . H93 H 0.2219 0.0936 -0.1532 0.121 Uiso 1 1 calc R . . C94 C 0.2533(6) 0.1862(5) -0.0906(3) 0.092(3) Uani 1 1 d . . . H94 H 0.2737 0.2145 -0.1086 0.111 Uiso 1 1 calc R . . C95 C 0.2538(5) 0.2141(4) -0.0382(3) 0.070(2) Uani 1 1 d . . . C96 C 0.2937(5) 0.2895(4) -0.0066(3) 0.068(2) Uani 1 1 d . . . C97 C 0.3141(7) 0.3365(4) -0.0352(3) 0.102(4) Uani 1 1 d . . . H97A H 0.3103 0.3807 -0.0142 0.122 Uiso 1 1 calc R . . H97B H 0.2761 0.3164 -0.0691 0.122 Uiso 1 1 calc R . . H97C H 0.3690 0.3431 -0.0409 0.122 Uiso 1 1 calc R . . C98 C 0.3624(4) 0.3900(3) 0.1275(2) 0.0473(16) Uani 1 1 d . . . C99 C 0.5180(5) 0.5724(3) 0.2364(3) 0.075(2) Uani 1 1 d . . . H99A H 0.5184 0.5566 0.1989 0.090 Uiso 1 1 calc R . . H99B H 0.5728 0.5873 0.2568 0.090 Uiso 1 1 calc R . . H99C H 0.4981 0.6108 0.2463 0.090 Uiso 1 1 calc R . . C100 C 0.4636(4) 0.5149(3) 0.2475(2) 0.0435(14) Uani 1 1 d . . . C101 C 0.4639(4) 0.5207(3) 0.3022(3) 0.0482(16) Uani 1 1 d . . . C102 C 0.5133(4) 0.5798(3) 0.3445(3) 0.0543(17) Uani 1 1 d . . . H102 H 0.5467 0.6174 0.3387 0.065 Uiso 1 1 calc R . . C103 C 0.5130(4) 0.5832(3) 0.3945(3) 0.062(2) Uani 1 1 d . . . H103 H 0.5464 0.6233 0.4234 0.075 Uiso 1 1 calc R . . C104 C 0.4651(5) 0.5293(4) 0.4030(3) 0.062(2) Uani 1 1 d . . . H104 H 0.4648 0.5309 0.4375 0.075 Uiso 1 1 calc R . . C105 C 0.4160(4) 0.4711(3) 0.3587(2) 0.0534(17) Uani 1 1 d . . . H105 H 0.3817 0.4336 0.3642 0.064 Uiso 1 1 calc R . . C106 C 0.2898(4) 0.0011(3) -0.0133(3) 0.0542(17) Uani 1 1 d . . . H106 H 0.2414 -0.0068 -0.0007 0.065 Uiso 1 1 calc R . . C107 C 0.2852(6) -0.0354(4) -0.0648(3) 0.077(2) Uani 1 1 d . . . H107 H 0.2354 -0.0672 -0.0872 0.093 Uiso 1 1 calc R . . C108 C 0.3560(8) -0.0247(6) -0.0836(4) 0.121(4) Uani 1 1 d . . . H108 H 0.3555 -0.0498 -0.1191 0.145 Uiso 1 1 calc R . . C109 C 0.4291(7) 0.0246(6) -0.0485(4) 0.117(4) Uani 1 1 d . . . H109 H 0.4783 0.0334 -0.0602 0.141 Uiso 1 1 calc R . . C110 C 0.4266(5) 0.0591(4) 0.0025(3) 0.064(2) Uani 1 1 d . . . C111 C 0.5004(5) 0.1095(4) 0.0397(3) 0.068(2) Uani 1 1 d . . . C112 C 0.5772(5) 0.1241(5) 0.0216(4) 0.097(3) Uani 1 1 d . . . H11A H 0.5706 0.1382 -0.0077 0.117 Uiso 1 1 calc R . . H11B H 0.5919 0.0830 0.0102 0.117 Uiso 1 1 calc R . . H11C H 0.6198 0.1609 0.0505 0.117 Uiso 1 1 calc R . . C113 C 0.5483(4) 0.2100(3) 0.1710(3) 0.0486(16) Uani 1 1 d . . . C114 C 0.7291(5) 0.3586(5) 0.2961(4) 0.108(4) Uani 1 1 d . . . H11D H 0.7456 0.3204 0.2765 0.130 Uiso 1 1 calc R . . H11E H 0.7612 0.3816 0.3320 0.130 Uiso 1 1 calc R . . H11F H 0.7377 0.3911 0.2789 0.130 Uiso 1 1 calc R . . C115 C 0.6416(4) 0.3325(4) 0.2971(3) 0.063(2) Uani 1 1 d . . . C116 C 0.6151(6) 0.3601(4) 0.3437(3) 0.072(2) Uani 1 1 d . . . C117 C 0.6665(6) 0.4114(5) 0.3906(4) 0.092(3) Uani 1 1 d . . . H117 H 0.7228 0.4288 0.3927 0.110 Uiso 1 1 calc R . . C118 C 0.6339(8) 0.4366(5) 0.4344(4) 0.109(4) Uani 1 1 d . . . H118 H 0.6683 0.4706 0.4664 0.131 Uiso 1 1 calc R . . C119 C 0.5557(7) 0.4129(5) 0.4310(3) 0.089(3) Uani 1 1 d . . . H119 H 0.5336 0.4311 0.4603 0.107 Uiso 1 1 calc R . . C120 C 0.5058(6) 0.3623(4) 0.3855(3) 0.074(3) Uani 1 1 d . . . H120 H 0.4498 0.3446 0.3843 0.089 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 Dy1 0.04357(17) 0.04095(15) 0.04148(17) 0.01070(13) -0.00267(13) 0.01951(13) Dy2 0.03697(16) 0.03343(14) 0.04617(17) 0.01087(12) -0.00024(13) 0.00757(12) Dy3 0.05454(19) 0.03081(14) 0.04403(17) 0.01611(13) -0.00606(14) 0.00587(13) Dy4 0.04191(17) 0.03591(15) 0.04641(17) 0.02012(13) -0.00635(13) 0.00468(12) Dy5 0.04519(17) 0.03615(14) 0.03449(15) 0.01127(12) -0.00132(12) 0.01496(12) Dy6 0.03453(15) 0.03709(14) 0.03601(15) 0.01379(12) 0.00817(11) 0.01421(11) Dy7 0.03795(15) 0.03222(13) 0.03305(14) 0.01255(11) 0.00408(11) 0.01141(11) Dy8 0.04480(17) 0.04176(15) 0.03515(15) 0.01458(12) 0.00072(12) 0.01793(13) Cl1 0.138(3) 0.1044(19) 0.124(2) 0.0565(18) 0.0359(19) 0.0633(18) Cl2 0.232(5) 0.099(2) 0.203(4) 0.010(3) 0.074(4) 0.058(3) Cl3 0.183(5) 0.175(4) 0.222(5) 0.055(4) -0.004(4) 0.004(4) Cl4 0.137(3) 0.1010(19) 0.141(3) 0.0622(19) 0.062(2) 0.0572(18) O1 0.049(3) 0.037(2) 0.044(2) 0.0051(19) -0.010(2) 0.0107(19) O2 0.041(2) 0.047(2) 0.059(3) 0.030(2) 0.007(2) 0.012(2) O3 0.068(3) 0.039(2) 0.049(3) 0.011(2) 0.001(2) 0.029(2) O4 0.046(3) 0.041(2) 0.043(2) 0.0119(19) -0.002(2) 0.0034(19) O5 0.056(3) 0.046(2) 0.045(3) 0.014(2) 0.006(2) 0.027(2) O6 0.069(3) 0.043(2) 0.043(3) 0.021(2) -0.001(2) 0.017(2) O7 0.043(2) 0.032(2) 0.044(2) 0.0101(18) -0.0002(19) 0.0101(18) O8 0.036(2) 0.035(2) 0.041(2) 0.0106(19) -0.0032(19) 0.0050(17) O9 0.033(2) 0.034(2) 0.044(2) 0.0127(17) 0.0071(17) 0.0098(17) O10 0.053(3) 0.046(2) 0.034(2) 0.0188(19) 0.0140(19) 0.021(2) O11 0.056(3) 0.032(2) 0.033(2) 0.0099(17) 0.0004(19) 0.0081(18) O12 0.037(2) 0.050(2) 0.047(2) 0.017(2) 0.0080(19) 0.0185(19) O13 0.043(2) 0.043(2) 0.043(2) 0.0167(19) 0.0095(19) 0.0153(19) O14 0.040(2) 0.038(2) 0.030(2) 0.0135(17) 0.0087(17) 0.0147(17) O15 0.035(2) 0.036(2) 0.040(2) 0.0105(18) 0.0042(18) 0.0093(17) O16 0.040(2) 0.038(2) 0.033(2) 0.0159(17) 0.0098(17) 0.0131(18) N1 0.060(4) 0.059(3) 0.057(4) 0.020(3) -0.006(3) 0.033(3) N2 0.052(3) 0.050(3) 0.043(3) 0.006(3) -0.003(3) 0.019(3) N3 0.072(4) 0.044(3) 0.046(3) 0.015(3) 0.007(3) 0.020(3) N4 0.071(4) 0.038(3) 0.064(4) 0.008(3) 0.007(3) 0.016(3) N5 0.042(3) 0.039(3) 0.055(3) 0.012(2) 0.007(2) 0.013(2) N6 0.039(3) 0.033(3) 0.080(4) 0.022(3) 0.004(3) 0.006(2) N7 0.094(5) 0.041(3) 0.047(3) 0.021(3) -0.014(3) 0.015(3) N8 0.060(4) 0.052(3) 0.053(3) 0.027(3) -0.004(3) 0.005(3) N9 0.046(3) 0.069(4) 0.072(4) 0.039(3) 0.006(3) 0.014(3) N10 0.035(3) 0.060(3) 0.073(4) 0.038(3) 0.009(3) 0.011(3) N11 0.041(3) 0.054(3) 0.062(4) 0.026(3) -0.007(3) 0.011(3) N12 0.056(4) 0.053(3) 0.073(4) 0.038(3) -0.012(3) 0.005(3) N13 0.042(3) 0.075(4) 0.060(4) 0.025(3) -0.003(3) 0.019(3) N14 0.068(4) 0.073(4) 0.061(4) 0.027(3) 0.009(3) 0.045(3) N15 0.090(5) 0.073(4) 0.065(4) 0.013(3) 0.003(4) 0.056(4) N16 0.142(7) 0.038(3) 0.065(4) -0.004(3) 0.009(4) 0.047(4) N17 0.108(6) 0.039(3) 0.051(4) 0.005(3) -0.002(4) 0.038(3) N18 0.090(5) 0.037(3) 0.051(4) 0.015(3) -0.013(3) 0.003(3) N19 0.039(3) 0.043(3) 0.065(4) 0.008(3) 0.003(3) 0.011(2) N20 0.043(3) 0.045(3) 0.057(3) 0.016(3) 0.006(3) 0.014(2) N21 0.056(4) 0.054(3) 0.056(4) 0.016(3) 0.009(3) 0.014(3) N22 0.084(5) 0.060(4) 0.040(3) 0.017(3) 0.008(3) 0.007(3) N23 0.079(4) 0.057(3) 0.041(3) 0.028(3) -0.003(3) 0.004(3) N24 0.070(4) 0.048(3) 0.055(4) 0.026(3) -0.013(3) 0.003(3) N25 0.054(3) 0.048(3) 0.036(3) 0.007(2) -0.009(2) 0.023(3) N26 0.035(3) 0.045(3) 0.047(3) 0.005(2) -0.007(2) 0.010(2) N27 0.029(3) 0.043(3) 0.061(3) 0.004(3) -0.003(2) 0.006(2) N28 0.038(3) 0.041(3) 0.060(3) 0.016(3) 0.009(3) 0.010(2) N29 0.049(3) 0.031(2) 0.055(3) 0.016(2) 0.014(2) 0.014(2) N30 0.053(3) 0.050(3) 0.045(3) 0.014(2) 0.014(3) 0.027(3) N31 0.043(3) 0.040(3) 0.051(3) 0.009(2) -0.001(3) 0.016(2) N32 0.043(3) 0.039(3) 0.038(3) 0.012(2) 0.005(2) 0.015(2) N33 0.060(4) 0.054(3) 0.040(3) 0.016(2) 0.020(3) 0.019(3) N34 0.081(4) 0.067(4) 0.042(3) 0.037(3) 0.028(3) 0.028(3) N35 0.073(4) 0.050(3) 0.041(3) 0.023(3) 0.007(3) 0.028(3) N36 0.101(5) 0.054(3) 0.046(4) 0.009(3) -0.007(3) 0.042(4) N37 0.072(4) 0.049(3) 0.035(3) 0.006(2) -0.003(3) 0.023(3) N38 0.076(4) 0.047(3) 0.037(3) 0.021(2) 0.007(3) 0.015(3) N39 0.091(5) 0.048(3) 0.037(3) 0.020(3) 0.012(3) 0.024(3) N40 0.066(4) 0.039(3) 0.045(3) 0.020(2) 0.010(3) 0.013(3) N41 0.050(3) 0.036(3) 0.041(3) 0.015(2) 0.003(2) 0.014(2) N42 0.043(3) 0.040(3) 0.048(3) 0.009(2) 0.002(2) 0.015(2) N43 0.055(3) 0.052(3) 0.043(3) 0.014(3) 0.014(3) 0.025(3) N44 0.043(3) 0.066(4) 0.052(3) 0.015(3) 0.016(3) 0.019(3) N45 0.031(3) 0.081(4) 0.067(4) 0.017(3) 0.011(3) 0.017(3) N46 0.035(3) 0.077(4) 0.065(4) 0.014(3) -0.001(3) 0.013(3) N47 0.043(3) 0.065(4) 0.064(4) 0.022(3) -0.009(3) 0.015(3) N48 0.079(5) 0.067(4) 0.043(3) 0.016(3) -0.006(3) 0.032(3) C1 0.084(6) 0.061(4) 0.047(4) 0.017(3) 0.001(4) 0.042(4) C2 0.113(7) 0.074(5) 0.076(6) 0.038(5) 0.006(5) 0.052(5) C3 0.129(8) 0.091(6) 0.073(6) 0.045(5) 0.008(6) 0.060(6) C4 0.121(8) 0.085(6) 0.048(4) 0.023(4) -0.003(5) 0.062(5) C5 0.059(4) 0.063(4) 0.042(4) 0.018(3) -0.003(3) 0.029(3) C6 0.076(5) 0.058(4) 0.049(4) 0.019(3) 0.004(4) 0.026(4) C7 0.177(11) 0.076(6) 0.053(5) 0.023(4) 0.015(6) 0.046(6) C8 0.052(4) 0.043(4) 0.046(4) 0.001(3) -0.002(3) 0.012(3) C9 0.081(6) 0.042(4) 0.093(6) 0.015(4) 0.023(5) 0.023(4) C10 0.049(4) 0.039(3) 0.073(5) 0.013(3) 0.008(4) 0.012(3) C11 0.042(4) 0.041(3) 0.078(5) 0.021(3) 0.005(3) 0.012(3) C12 0.050(4) 0.047(4) 0.090(6) 0.033(4) 0.013(4) 0.019(3) C13 0.049(4) 0.054(4) 0.106(7) 0.040(5) 0.012(4) 0.018(3) C14 0.045(4) 0.066(5) 0.105(7) 0.053(5) 0.007(4) 0.014(4) C15 0.041(4) 0.057(4) 0.061(4) 0.028(3) 0.002(3) 0.012(3) C16 0.094(6) 0.040(4) 0.057(4) 0.019(3) -0.005(4) 0.019(4) C17 0.149(10) 0.042(4) 0.055(5) 0.016(4) -0.004(6) 0.026(5) C18 0.131(9) 0.057(5) 0.049(5) 0.024(4) 0.022(5) 0.014(5) C19 0.106(7) 0.054(4) 0.064(5) 0.032(4) 0.022(5) 0.003(4) C20 0.065(5) 0.060(4) 0.040(4) 0.020(3) 0.009(3) -0.004(4) C21 0.064(5) 0.062(4) 0.053(4) 0.030(4) 0.000(4) 0.002(4) C22 0.078(6) 0.106(7) 0.088(6) 0.063(6) 0.033(5) 0.023(5) C23 0.041(4) 0.055(4) 0.061(4) 0.024(4) -0.002(3) 0.006(3) C24 0.058(5) 0.072(5) 0.112(7) 0.041(5) 0.005(5) 0.024(4) C25 0.050(4) 0.052(4) 0.064(5) 0.019(3) -0.010(3) 0.021(3) C26 0.054(4) 0.043(4) 0.066(5) 0.022(3) -0.014(4) 0.005(3) C27 0.083(6) 0.065(5) 0.078(6) 0.035(4) -0.009(5) 0.031(4) C28 0.138(10) 0.071(6) 0.089(7) 0.042(5) -0.028(7) 0.038(6) C29 0.123(8) 0.051(4) 0.075(6) 0.035(4) -0.016(6) 0.014(5) C30 0.093(6) 0.078(5) 0.067(5) 0.050(5) 0.000(5) 0.016(5) C31 0.048(4) 0.095(6) 0.065(5) 0.042(5) 0.004(4) 0.025(4) C32 0.065(6) 0.126(8) 0.072(6) 0.061(6) -0.005(5) -0.003(6) C33 0.047(5) 0.153(10) 0.086(7) 0.055(7) 0.005(5) 0.044(6) C34 0.065(5) 0.141(9) 0.074(6) 0.059(6) 0.018(5) 0.061(6) C35 0.060(5) 0.122(7) 0.069(5) 0.053(5) 0.026(4) 0.061(5) C36 0.090(6) 0.098(6) 0.070(5) 0.039(5) 0.026(5) 0.074(5) C37 0.098(8) 0.127(9) 0.143(10) 0.036(8) 0.027(7) 0.082(7) C38 0.092(6) 0.049(4) 0.051(4) 0.020(3) 0.012(4) 0.036(4) C39 0.182(12) 0.059(5) 0.086(7) -0.015(5) 0.002(7) 0.044(7) C40 0.135(9) 0.035(4) 0.057(5) 0.009(3) 0.015(5) 0.021(4) C41 0.101(7) 0.061(5) 0.050(5) 0.032(4) -0.002(4) 0.013(5) C42 0.125(9) 0.052(5) 0.051(5) 0.013(4) -0.009(5) 0.001(5) C43 0.123(10) 0.082(7) 0.072(7) 0.023(6) -0.035(7) -0.015(7) C44 0.089(7) 0.089(7) 0.102(8) 0.051(6) -0.029(6) -0.039(6) C45 0.077(6) 0.056(4) 0.070(5) 0.034(4) -0.013(4) -0.003(4) C46 0.052(4) 0.047(4) 0.060(5) 0.007(3) 0.004(4) 0.007(3) C47 0.037(4) 0.058(4) 0.089(6) 0.008(4) -0.003(4) 0.006(3) C48 0.035(4) 0.071(6) 0.123(8) 0.019(6) 0.006(5) 0.000(4) C49 0.033(4) 0.062(5) 0.123(8) 0.026(5) 0.021(4) 0.018(3) C50 0.042(4) 0.052(4) 0.076(5) 0.011(4) 0.006(4) 0.019(3) C51 0.054(4) 0.045(4) 0.068(5) 0.023(3) 0.016(4) 0.021(3) C52 0.060(5) 0.083(6) 0.085(6) 0.007(5) 0.026(4) 0.023(4) C53 0.051(4) 0.040(3) 0.043(4) 0.014(3) 0.004(3) 0.006(3) C54 0.145(11) 0.108(8) 0.072(7) -0.013(6) 0.018(7) -0.018(8) C55 0.106(7) 0.058(5) 0.040(4) 0.012(4) -0.009(4) -0.013(5) C56 0.091(6) 0.055(4) 0.050(5) 0.028(4) -0.023(4) -0.014(4) C57 0.112(8) 0.089(6) 0.049(5) 0.023(5) -0.016(5) -0.019(6) C58 0.103(8) 0.078(6) 0.084(7) 0.031(6) -0.045(6) -0.033(6) C59 0.058(5) 0.105(7) 0.074(6) 0.026(6) -0.023(5) -0.014(5) C60 0.059(5) 0.055(4) 0.070(5) 0.027(4) -0.016(4) -0.006(4) C61 0.072(5) 0.057(4) 0.046(4) 0.009(3) -0.010(4) 0.027(4) C62 0.121(8) 0.074(5) 0.037(4) 0.009(4) -0.001(4) 0.068(5) C63 0.110(8) 0.110(7) 0.044(4) 0.018(4) 0.011(5) 0.084(6) C64 0.063(5) 0.088(5) 0.046(4) 0.015(4) -0.005(3) 0.046(4) C65 0.079(5) 0.066(4) 0.026(3) 0.010(3) -0.005(3) 0.039(4) C66 0.052(4) 0.062(4) 0.042(4) 0.011(3) 0.002(3) 0.032(3) C67 0.046(4) 0.082(5) 0.075(5) 0.026(4) -0.004(4) 0.023(4) C68 0.030(3) 0.045(3) 0.050(4) 0.014(3) 0.007(3) 0.016(3) C69 0.083(6) 0.052(4) 0.129(8) 0.054(5) 0.007(5) 0.015(4) C70 0.069(5) 0.040(3) 0.052(4) 0.018(3) 0.013(3) 0.023(3) C71 0.058(4) 0.054(4) 0.054(4) 0.026(3) 0.012(3) 0.031(3) C72 0.086(6) 0.050(4) 0.082(6) 0.032(4) 0.029(4) 0.038(4) C73 0.111(7) 0.070(5) 0.077(5) 0.043(4) 0.045(5) 0.068(5) C74 0.073(5) 0.086(6) 0.065(5) 0.042(4) 0.031(4) 0.056(5) C75 0.071(5) 0.064(4) 0.054(4) 0.024(4) 0.016(4) 0.038(4) C76 0.065(5) 0.044(3) 0.046(4) 0.016(3) 0.001(3) 0.018(3) C77 0.079(6) 0.046(4) 0.076(5) 0.016(4) -0.009(5) 0.033(4) C78 0.042(4) 0.049(4) 0.103(7) 0.014(4) 0.001(4) 0.022(3) C79 0.044(4) 0.057(4) 0.094(6) 0.013(4) 0.008(4) 0.025(3) C80 0.032(3) 0.039(3) 0.059(4) 0.003(3) -0.005(3) 0.011(3) C81 0.039(4) 0.052(4) 0.054(4) 0.008(3) 0.015(3) 0.013(3) C82 0.058(5) 0.059(4) 0.084(6) 0.015(4) 0.034(4) 0.023(4) C83 0.062(4) 0.046(3) 0.040(4) 0.019(3) 0.012(3) 0.020(3) C84 0.145(9) 0.079(6) 0.071(6) 0.053(5) 0.040(6) 0.049(6) C85 0.103(7) 0.054(4) 0.044(4) 0.022(3) -0.005(4) 0.017(4) C86 0.105(7) 0.055(4) 0.038(4) 0.013(3) 0.001(4) 0.034(4) C87 0.164(11) 0.073(6) 0.071(6) 0.030(5) -0.015(6) 0.052(6) C88 0.183(13) 0.090(7) 0.082(7) 0.033(6) -0.008(7) 0.086(8) C89 0.131(9) 0.084(6) 0.084(7) 0.014(5) -0.017(6) 0.072(6) C90 0.095(7) 0.084(6) 0.054(5) 0.028(4) 0.007(4) 0.047(5) C91 0.086(6) 0.058(4) 0.047(4) 0.017(3) 0.005(4) 0.029(4) C92 0.127(8) 0.064(5) 0.047(5) 0.006(4) -0.005(5) 0.047(5) C93 0.158(10) 0.081(6) 0.038(4) 0.004(4) 0.006(5) 0.036(6) C94 0.142(9) 0.086(6) 0.034(4) 0.020(4) 0.014(5) 0.025(6) C95 0.098(6) 0.065(5) 0.039(4) 0.020(4) -0.002(4) 0.025(4) C96 0.097(6) 0.052(4) 0.039(4) 0.014(3) -0.004(4) 0.013(4) C97 0.168(10) 0.079(6) 0.046(5) 0.035(4) 0.008(6) 0.018(6) C98 0.063(4) 0.041(3) 0.043(4) 0.023(3) 0.008(3) 0.018(3) C99 0.079(6) 0.038(4) 0.082(6) 0.022(4) 0.001(4) -0.008(4) C100 0.045(4) 0.040(3) 0.052(4) 0.019(3) 0.016(3) 0.019(3) C101 0.038(3) 0.038(3) 0.056(4) 0.007(3) -0.001(3) 0.013(3) C102 0.042(4) 0.043(3) 0.056(4) 0.003(3) -0.001(3) 0.007(3) C103 0.050(4) 0.048(4) 0.060(5) -0.008(3) -0.011(3) 0.018(3) C104 0.071(5) 0.061(4) 0.037(4) -0.001(3) -0.003(3) 0.028(4) C105 0.065(5) 0.056(4) 0.037(4) 0.016(3) 0.003(3) 0.023(3) C106 0.058(4) 0.053(4) 0.052(4) 0.016(3) 0.016(3) 0.024(3) C107 0.082(6) 0.075(5) 0.057(5) 0.007(4) 0.012(4) 0.026(5) C108 0.141(11) 0.148(10) 0.056(6) 0.007(6) 0.057(6) 0.054(8) C109 0.096(8) 0.150(10) 0.057(6) -0.011(6) 0.022(5) 0.033(7) C110 0.075(5) 0.067(5) 0.053(4) 0.018(4) 0.034(4) 0.027(4) C111 0.059(5) 0.076(5) 0.066(5) 0.022(4) 0.037(4) 0.019(4) C112 0.074(6) 0.103(7) 0.091(7) 0.011(6) 0.040(5) 0.023(5) C113 0.028(3) 0.053(4) 0.061(4) 0.020(3) 0.013(3) 0.011(3) C114 0.046(5) 0.112(8) 0.096(7) -0.015(6) -0.014(5) 0.006(5) C115 0.045(4) 0.060(4) 0.071(5) 0.018(4) -0.007(4) 0.016(3) C116 0.079(6) 0.056(4) 0.066(5) 0.015(4) -0.018(5) 0.022(4) C117 0.074(6) 0.092(6) 0.080(7) 0.021(5) -0.034(5) 0.018(5) C118 0.146(11) 0.082(6) 0.060(6) 0.009(5) -0.053(7) 0.031(7) C119 0.116(8) 0.087(6) 0.046(5) 0.005(4) -0.009(5) 0.042(6) C120 0.108(7) 0.063(5) 0.049(5) 0.016(4) -0.007(5) 0.040(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O7 2.253(4) . ? Dy1 O5 2.272(4) . ? Dy1 O3 2.333(4) . ? Dy1 O1 2.341(4) . ? Dy1 N14 2.527(6) . ? Dy1 N2 2.528(5) . ? Dy1 N1 2.537(6) . ? Dy1 N13 2.556(5) . ? Dy2 O8 2.253(4) . ? Dy2 O5 2.269(4) . ? Dy2 O1 2.319(4) . ? Dy2 O4 2.342(4) . ? Dy2 N20 2.530(6) . ? Dy2 N5 2.535(5) . ? Dy2 N19 2.548(5) . ? Dy2 N6 2.559(5) . ? Dy3 O7 2.256(4) . ? Dy3 O6 2.262(5) . ? Dy3 O2 2.342(4) . ? Dy3 O3 2.348(4) . ? Dy3 N17 2.519(6) . ? Dy3 N8 2.532(7) . ? Dy3 N7 2.560(6) . ? Dy3 N18 2.562(6) . ? Dy4 O6 2.261(4) . ? Dy4 O8 2.278(4) . ? Dy4 O2 2.327(4) . ? Dy4 O4 2.333(4) . ? Dy4 N23 2.500(6) . ? Dy4 N11 2.534(6) . ? Dy4 N24 2.540(5) . ? Dy4 N12 2.544(5) . ? Dy5 O15 2.249(4) . ? Dy5 O13 2.251(4) . ? Dy5 O9 2.339(4) . ? Dy5 O11 2.357(4) . ? Dy5 N25 2.539(5) . ? Dy5 N26 2.558(5) . ? Dy5 N38 2.566(5) . ? Dy5 N37 2.581(5) . ? Dy6 O16 2.261(4) . ? Dy6 O13 2.265(4) . ? Dy6 O9 2.329(4) . ? Dy6 O12 2.354(4) . ? Dy6 N29 2.512(5) . ? Dy6 N44 2.526(6) . ? Dy6 N30 2.536(5) . ? Dy6 N43 2.548(5) . ? Dy7 O15 2.268(4) . ? Dy7 O14 2.272(4) . ? Dy7 O11 2.334(4) . ? Dy7 O10 2.338(4) . ? Dy7 N41 2.521(5) . ? Dy7 N32 2.541(5) . ? Dy7 N31 2.555(5) . ? Dy7 N42 2.562(5) . ? Dy8 O16 2.254(4) . ? Dy8 O14 2.259(3) . ? Dy8 O12 2.323(4) . ? Dy8 O10 2.328(4) . ? Dy8 N47 2.510(6) . ? Dy8 N35 2.515(6) . ? Dy8 N36 2.539(6) . ? Dy8 N48 2.561(6) . ? O1 C8 1.301(8) . ? O2 C23 1.285(9) . ? O3 C38 1.285(8) . ? O4 C53 1.287(8) . ? O5 H5 0.88(2) . ? O6 H6 0.88(2) . ? O7 H7 0.87(2) . ? O8 H8 0.87(2) . ? O9 C68 1.306(7) . ? O10 C83 1.275(7) . ? O11 C98 1.280(7) . ? O12 C113 1.307(7) . ? O13 H13 0.89(2) . ? O14 H14 0.86(2) . ? O15 H15 0.87(2) . ? O16 H16 0.87(2) . ? N1 C1 1.343(8) . ? N1 C5 1.384(9) . ? N2 C6 1.282(8) . ? N2 N3 1.400(7) . ? N3 C8 1.333(8) . ? N4 C8 1.351(8) . ? N4 N5 1.397(8) . ? N5 C10 1.312(8) . ? N6 C11 1.357(9) . ? N6 C15 1.365(9) . ? N7 C16 1.346(9) . ? N7 C20 1.395(10) . ? N8 C21 1.312(8) . ? N8 N9 1.373(8) . ? N9 C23 1.307(9) . ? N10 N11 1.357(7) . ? N10 C23 1.359(8) . ? N11 C25 1.322(8) . ? N12 C30 1.351(10) . ? N12 C26 1.381(10) . ? N13 C31 1.324(10) . ? N13 C35 1.357(10) . ? N14 C36 1.292(10) . ? N14 N15 1.378(8) . ? N15 C38 1.348(10) . ? N16 C38 1.363(9) . ? N16 N17 1.381(10) . ? N16 H16A 0.8800 . ? N17 C40 1.310(9) . ? N18 C41 1.333(11) . ? N18 C45 1.354(10) . ? N19 C50 1.338(9) . ? N19 C46 1.347(8) . ? N20 C51 1.293(8) . ? N20 N21 1.392(7) . ? N21 C53 1.352(9) . ? N22 C53 1.334(8) . ? N22 N23 1.402(9) . ? N22 H22 0.8800 . ? N23 C55 1.305(9) . ? N24 C56 1.343(11) . ? N24 C60 1.358(10) . ? N25 C65 1.355(9) . ? N25 C61 1.362(8) . ? N26 C66 1.294(8) . ? N26 N27 1.382(7) . ? N27 C68 1.350(7) . ? N27 H27 0.8800 . ? N28 C68 1.291(7) . ? N28 N29 1.400(7) . ? N29 C70 1.317(7) . ? N30 C71 1.348(8) . ? N30 C75 1.354(9) . ? N31 C76 1.343(8) . ? N31 C80 1.357(9) . ? N32 C81 1.283(8) . ? N32 N33 1.378(7) . ? N33 C83 1.351(9) . ? N34 C83 1.334(7) . ? N34 N35 1.392(8) . ? N34 H34 0.8800 . ? N35 C85 1.302(8) . ? N36 C90 1.345(11) . ? N36 C86 1.379(10) . ? N37 C91 1.309(8) . ? N37 C95 1.353(9) . ? N38 C96 1.283(8) . ? N38 N39 1.390(7) . ? N39 C98 1.382(8) . ? N40 C98 1.329(8) . ? N40 N41 1.401(7) . ? N41 C100 1.319(7) . ? N42 C105 1.344(8) . ? N42 C101 1.356(8) . ? N43 C106 1.346(8) . ? N43 C110 1.368(9) . ? N44 C111 1.296(9) . ? N44 N45 1.404(7) . ? N45 C113 1.318(9) . ? N46 C113 1.337(8) . ? N46 N47 1.386(9) . ? N47 C115 1.300(9) . ? N48 C116 1.353(11) . ? N48 C120 1.376(11) . ? C1 C2 1.354(10) . ? C1 H1 0.9500 . ? C2 C3 1.421(12) . ? C2 H2 0.9500 . ? C3 C4 1.365(11) . ? C3 H3 0.9500 . ? C4 C5 1.389(10) . ? C4 H4 0.9500 . ? C5 C6 1.443(9) . ? C6 C7 1.536(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.508(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.473(10) . ? C11 C12 1.397(8) . ? C12 C13 1.355(11) . ? C12 H12 0.9500 . ? C13 C14 1.397(11) . ? C13 H13A 0.9500 . ? C14 C15 1.376(9) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.409(11) . ? C16 H16B 0.9500 . ? C17 C18 1.349(13) . ? C17 H17 0.9500 . ? C18 C19 1.354(13) . ? C18 H18 0.9500 . ? C19 C20 1.376(9) . ? C19 H19 0.9500 . ? C20 C21 1.463(11) . ? C21 C22 1.496(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 C25 1.519(11) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.468(11) . ? C26 C27 1.407(9) . ? C27 C28 1.319(13) . ? C27 H27A 0.9500 . ? C28 C29 1.375(15) . ? C28 H28 0.9500 . ? C29 C30 1.410(10) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.413(11) . ? C31 H31 0.9500 . ? C32 C33 1.374(14) . ? C32 H32 0.9500 . ? C33 C34 1.349(13) . ? C33 H33 0.9500 . ? C34 C35 1.377(11) . ? C34 H34A 0.9500 . ? C35 C36 1.518(12) . ? C36 C37 1.497(11) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C39 C40 1.524(12) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.470(13) . ? C41 C42 1.441(11) . ? C42 C43 1.288(15) . ? C42 H42 0.9500 . ? C43 C44 1.443(17) . ? C43 H43 0.9500 . ? C44 C45 1.404(11) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.390(9) . ? C46 H46 0.9500 . ? C47 C48 1.338(12) . ? C47 H47 0.9500 . ? C48 C49 1.380(12) . ? C48 H48 0.9500 . ? C49 C50 1.405(10) . ? C49 H49 0.9500 . ? C50 C51 1.508(10) . ? C51 C52 1.486(11) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C54 C55 1.492(13) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.462(13) . ? C56 C57 1.392(10) . ? C57 C58 1.421(15) . ? C57 H57 0.9500 . ? C58 C59 1.340(15) . ? C58 H58 0.9500 . ? C59 C60 1.372(10) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.397(11) . ? C61 H61 0.9500 . ? C62 C63 1.370(12) . ? C62 H62 0.9500 . ? C63 C64 1.388(11) . ? C63 H63 0.9500 . ? C64 C65 1.427(10) . ? C64 H64 0.9500 . ? C65 C66 1.474(9) . ? C66 C67 1.514(10) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C69 C70 1.481(9) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.497(9) . ? C71 C72 1.398(8) . ? C72 C73 1.392(11) . ? C72 H72 0.9500 . ? C73 C74 1.354(11) . ? C73 H73 0.9500 . ? C74 C75 1.385(9) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.381(10) . ? C76 H76 0.9500 . ? C77 C78 1.364(12) . ? C77 H77 0.9500 . ? C78 C79 1.378(11) . ? C78 H78 0.9500 . ? C79 C80 1.417(9) . ? C79 H79 0.9500 . ? C80 C81 1.510(9) . ? C81 C82 1.485(9) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C84 C85 1.515(11) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C86 1.483(12) . ? C86 C87 1.402(10) . ? C87 C88 1.376(16) . ? C87 H87 0.9500 . ? C88 C89 1.403(16) . ? C88 H88 0.9500 . ? C89 C90 1.411(11) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C92 1.390(11) . ? C91 H91 0.9500 . ? C92 C93 1.332(12) . ? C92 H92 0.9500 . ? C93 C94 1.411(12) . ? C93 H93 0.9500 . ? C94 C95 1.371(10) . ? C94 H94 0.9500 . ? C95 C96 1.505(10) . ? C96 C97 1.508(10) . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C99 C100 1.509(8) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 C101 1.484(9) . ? C101 C102 1.397(8) . ? C102 C103 1.367(10) . ? C102 H102 0.9500 . ? C103 C104 1.364(10) . ? C103 H103 0.9500 . ? C104 C105 1.412(9) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C107 1.362(10) . ? C106 H106 0.9500 . ? C107 C108 1.393(13) . ? C107 H107 0.9500 . ? C108 C109 1.429(14) . ? C108 H108 0.9500 . ? C109 C110 1.372(11) . ? C109 H109 0.9500 . ? C110 C111 1.463(11) . ? C111 C112 1.483(10) . ? C112 H11A 0.9800 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? C114 C115 1.499(11) . ? C114 H11D 0.9800 . ? C114 H11E 0.9800 . ? C114 H11F 0.9800 . ? C115 C116 1.418(12) . ? C116 C117 1.407(11) . ? C117 C118 1.408(16) . ? C117 H117 0.9500 . ? C118 C119 1.316(15) . ? C118 H118 0.9500 . ? C119 C120 1.371(11) . ? C119 H119 0.9500 . ? C120 H120 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 O7 Dy1 O5 99.06(16) . . ? O7 Dy1 O3 66.75(15) . . ? O5 Dy1 O3 86.82(15) . . ? O7 Dy1 O1 88.62(14) . . ? O5 Dy1 O1 67.00(15) . . ? O3 Dy1 O1 141.06(13) . . ? O7 Dy1 N14 128.30(18) . . ? O5 Dy1 N14 86.51(17) . . ? O3 Dy1 N14 62.29(18) . . ? O1 Dy1 N14 138.43(19) . . ? O7 Dy1 N2 85.17(16) . . ? O5 Dy1 N2 129.85(17) . . ? O3 Dy1 N2 137.88(18) . . ? O1 Dy1 N2 63.16(17) . . ? N14 Dy1 N2 129.06(18) . . ? O7 Dy1 N1 90.18(17) . . ? O5 Dy1 N1 164.61(17) . . ? O3 Dy1 N1 85.56(16) . . ? O1 Dy1 N1 125.91(17) . . ? N14 Dy1 N1 78.11(19) . . ? N2 Dy1 N1 62.85(18) . . ? O7 Dy1 N13 163.57(18) . . ? O5 Dy1 N13 92.61(18) . . ? O3 Dy1 N13 125.83(19) . . ? O1 Dy1 N13 85.33(17) . . ? N14 Dy1 N13 63.6(2) . . ? N2 Dy1 N13 78.5(2) . . ? N1 Dy1 N13 81.11(19) . . ? O8 Dy2 O5 99.11(16) . . ? O8 Dy2 O1 87.14(15) . . ? O5 Dy2 O1 67.42(15) . . ? O8 Dy2 O4 68.06(15) . . ? O5 Dy2 O4 88.11(15) . . ? O1 Dy2 O4 142.20(14) . . ? O8 Dy2 N20 130.40(15) . . ? O5 Dy2 N20 84.59(17) . . ? O1 Dy2 N20 137.19(17) . . ? O4 Dy2 N20 62.63(16) . . ? O8 Dy2 N5 82.69(16) . . ? O5 Dy2 N5 130.34(16) . . ? O1 Dy2 N5 63.09(15) . . ? O4 Dy2 N5 135.63(17) . . ? N20 Dy2 N5 131.09(17) . . ? O8 Dy2 N19 162.14(17) . . ? O5 Dy2 N19 93.88(17) . . ? O1 Dy2 N19 86.58(17) . . ? O4 Dy2 N19 124.93(18) . . ? N20 Dy2 N19 62.81(18) . . ? N5 Dy2 N19 79.55(18) . . ? O8 Dy2 N6 90.00(15) . . ? O5 Dy2 N6 164.60(19) . . ? O1 Dy2 N6 125.83(17) . . ? O4 Dy2 N6 83.80(16) . . ? N20 Dy2 N6 80.06(18) . . ? N5 Dy2 N6 62.89(18) . . ? N19 Dy2 N6 80.21(17) . . ? O7 Dy3 O6 98.93(16) . . ? O7 Dy3 O2 87.51(15) . . ? O6 Dy3 O2 67.82(16) . . ? O7 Dy3 O3 66.43(15) . . ? O6 Dy3 O3 87.51(16) . . ? O2 Dy3 O3 141.15(14) . . ? O7 Dy3 N17 129.85(19) . . ? O6 Dy3 N17 83.89(19) . . ? O2 Dy3 N17 137.02(17) . . ? O3 Dy3 N17 63.68(18) . . ? O7 Dy3 N8 87.32(17) . . ? O6 Dy3 N8 128.63(17) . . ? O2 Dy3 N8 61.55(16) . . ? O3 Dy3 N8 139.25(16) . . ? N17 Dy3 N8 129.3(2) . . ? O7 Dy3 N7 95.17(16) . . ? O6 Dy3 N7 162.16(19) . . ? O2 Dy3 N7 124.0(2) . . ? O3 Dy3 N7 88.17(19) . . ? N17 Dy3 N7 78.7(2) . . ? N8 Dy3 N7 62.7(2) . . ? O7 Dy3 N18 164.2(2) . . ? O6 Dy3 N18 90.69(18) . . ? O2 Dy3 N18 84.59(18) . . ? O3 Dy3 N18 126.86(19) . . ? N17 Dy3 N18 63.3(2) . . ? N8 Dy3 N18 76.9(2) . . ? N7 Dy3 N18 78.14(17) . . ? Dy4 Dy3 Dy1 90.224(11) . . ? O6 Dy4 O8 98.04(15) . . ? O6 Dy4 O2 68.08(17) . . ? O8 Dy4 O2 86.75(15) . . ? O6 Dy4 O4 86.82(17) . . ? O8 Dy4 O4 67.79(15) . . ? O2 Dy4 O4 141.56(14) . . ? O6 Dy4 N23 81.58(18) . . ? O8 Dy4 N23 130.90(18) . . ? O2 Dy4 N23 135.25(17) . . ? O4 Dy4 N23 63.16(17) . . ? O6 Dy4 N11 130.41(18) . . ? O8 Dy4 N11 83.68(16) . . ? O2 Dy4 N11 62.53(16) . . ? O4 Dy4 N11 136.72(16) . . ? N23 Dy4 N11 132.94(19) . . ? O6 Dy4 N24 91.33(17) . . ? O8 Dy4 N24 163.9(2) . . ? O2 Dy4 N24 84.64(18) . . ? O4 Dy4 N24 126.11(19) . . ? N23 Dy4 N24 63.3(2) . . ? N11 Dy4 N24 80.3(2) . . ? O6 Dy4 N12 162.9(2) . . ? O8 Dy4 N12 92.99(16) . . ? O2 Dy4 N12 125.8(2) . . ? O4 Dy4 N12 85.35(18) . . ? N23 Dy4 N12 81.4(2) . . ? N11 Dy4 N12 63.6(2) . . ? N24 Dy4 N12 81.16(17) . . ? O6 Dy4 Dy2 84.21(12) . . ? O8 Dy4 Dy2 33.53(11) . . ? O2 Dy4 Dy2 109.58(10) . . ? O4 Dy4 Dy2 36.37(10) . . ? N23 Dy4 Dy2 98.72(14) . . ? N11 Dy4 Dy2 115.75(12) . . ? N24 Dy4 Dy2 161.97(17) . . ? N12 Dy4 Dy2 98.21(12) . . ? O6 Dy4 Dy3 33.55(13) . . ? O8 Dy4 Dy3 84.95(10) . . ? O2 Dy4 Dy3 36.29(11) . . ? O4 Dy4 Dy3 110.16(10) . . ? N23 Dy4 Dy3 113.37(13) . . ? N11 Dy4 Dy3 98.40(12) . . ? N24 Dy4 Dy3 95.98(12) . . ? N12 Dy4 Dy3 161.99(17) . . ? O15 Dy5 O13 99.59(15) . . ? O15 Dy5 O9 89.10(14) . . ? O13 Dy5 O9 67.01(13) . . ? O15 Dy5 O11 66.99(13) . . ? O13 Dy5 O11 87.36(15) . . ? O9 Dy5 O11 141.86(12) . . ? O15 Dy5 N25 88.94(16) . . ? O13 Dy5 N25 165.83(16) . . ? O9 Dy5 N25 124.85(15) . . ? O11 Dy5 N25 85.59(15) . . ? O15 Dy5 N26 85.17(15) . . ? O13 Dy5 N26 128.90(15) . . ? O9 Dy5 N26 62.20(15) . . ? O11 Dy5 N26 138.41(17) . . ? N25 Dy5 N26 62.71(17) . . ? O15 Dy5 N38 128.45(15) . . ? O13 Dy5 N38 86.09(17) . . ? O9 Dy5 N38 137.85(17) . . ? O11 Dy5 N38 62.13(15) . . ? N25 Dy5 N38 79.75(19) . . ? N26 Dy5 N38 129.68(17) . . ? O15 Dy5 N37 165.60(17) . . ? O13 Dy5 N37 90.01(17) . . ? O9 Dy5 N37 84.79(15) . . ? O11 Dy5 N37 124.60(16) . . ? N25 Dy5 N37 83.92(18) . . ? N26 Dy5 N37 80.45(18) . . ? N38 Dy5 N37 62.48(17) . . ? O16 Dy6 O13 98.39(14) . . ? O16 Dy6 O9 86.55(14) . . ? O13 Dy6 O9 66.97(13) . . ? O16 Dy6 O12 67.12(14) . . ? O13 Dy6 O12 89.21(14) . . ? O9 Dy6 O12 141.82(14) . . ? O16 Dy6 N29 85.68(15) . . ? O13 Dy6 N29 129.06(15) . . ? O9 Dy6 N29 62.61(14) . . ? O12 Dy6 N29 136.76(15) . . ? O16 Dy6 N44 129.77(16) . . ? O13 Dy6 N44 83.19(17) . . ? O9 Dy6 N44 136.82(16) . . ? O12 Dy6 N44 62.70(17) . . ? N29 Dy6 N44 131.34(18) . . ? O16 Dy6 N30 91.52(15) . . ? O13 Dy6 N30 164.22(17) . . ? O9 Dy6 N30 126.24(15) . . ? O12 Dy6 N30 83.34(15) . . ? N29 Dy6 N30 63.67(17) . . ? N44 Dy6 N30 81.03(19) . . ? O16 Dy6 N43 163.89(16) . . ? O13 Dy6 N43 92.37(16) . . ? O9 Dy6 N43 86.68(16) . . ? O12 Dy6 N43 125.29(17) . . ? N29 Dy6 N43 78.23(18) . . ? N44 Dy6 N43 63.25(18) . . ? N30 Dy6 N43 80.77(16) . . ? O15 Dy7 O14 97.18(14) . . ? O15 Dy7 O11 67.07(13) . . ? O14 Dy7 O11 87.41(14) . . ? O15 Dy7 O10 87.59(14) . . ? O14 Dy7 O10 67.11(14) . . ? O11 Dy7 O10 141.79(14) . . ? O15 Dy7 N41 129.45(15) . . ? O14 Dy7 N41 84.56(15) . . ? O11 Dy7 N41 62.54(14) . . ? O10 Dy7 N41 136.74(15) . . ? O15 Dy7 N32 85.39(15) . . ? O14 Dy7 N32 129.23(14) . . ? O11 Dy7 N32 137.54(15) . . ? O10 Dy7 N32 62.34(15) . . ? N41 Dy7 N32 131.21(16) . . ? O15 Dy7 N31 94.97(15) . . ? O14 Dy7 N31 163.15(15) . . ? O11 Dy7 N31 86.62(16) . . ? O10 Dy7 N31 125.20(17) . . ? N41 Dy7 N31 78.71(17) . . ? N32 Dy7 N31 63.35(17) . . ? O15 Dy7 N42 165.27(17) . . ? O14 Dy7 N42 90.75(15) . . ? O11 Dy7 N42 125.94(15) . . ? O10 Dy7 N42 84.08(15) . . ? N41 Dy7 N42 63.51(16) . . ? N32 Dy7 N42 79.99(16) . . ? N31 Dy7 N42 80.10(16) . . ? O16 Dy8 O14 96.75(13) . . ? O16 Dy8 O12 67.77(14) . . ? O14 Dy8 O12 86.04(14) . . ? O16 Dy8 O10 88.55(14) . . ? O14 Dy8 O10 67.50(14) . . ? O12 Dy8 O10 142.39(13) . . ? O16 Dy8 N47 131.26(18) . . ? O14 Dy8 N47 82.34(16) . . ? O12 Dy8 N47 63.54(18) . . ? O10 Dy8 N47 133.27(17) . . ? O16 Dy8 N35 83.02(16) . . ? O14 Dy8 N35 131.15(16) . . ? O12 Dy8 N35 135.93(16) . . ? O10 Dy8 N35 63.66(16) . . ? N47 Dy8 N35 132.84(18) . . ? O16 Dy8 N36 91.87(17) . . ? O14 Dy8 N36 163.9(2) . . ? O12 Dy8 N36 84.70(18) . . ? O10 Dy8 N36 126.5(2) . . ? N47 Dy8 N36 81.8(2) . . ? N35 Dy8 N36 63.3(2) . . ? O16 Dy8 N48 164.57(19) . . ? O14 Dy8 N48 93.00(16) . . ? O12 Dy8 N48 125.0(2) . . ? O10 Dy8 N48 84.15(18) . . ? N47 Dy8 N48 61.9(2) . . ? N35 Dy8 N48 81.6(2) . . ? N36 Dy8 N48 81.68(18) . . ? C8 O1 Dy2 126.2(4) . . ? C8 O1 Dy1 122.4(4) . . ? Dy2 O1 Dy1 108.44(17) . . ? C23 O2 Dy4 125.6(4) . . ? C23 O2 Dy3 124.3(4) . . ? Dy4 O2 Dy3 107.68(19) . . ? C38 O3 Dy1 125.1(5) . . ? C38 O3 Dy3 124.0(4) . . ? Dy1 O3 Dy3 107.92(16) . . ? C53 O4 Dy4 123.8(4) . . ? C53 O4 Dy2 124.0(4) . . ? Dy4 O4 Dy2 107.40(18) . . ? Dy2 O5 Dy1 112.74(19) . . ? Dy2 O5 H5 119(5) . . ? Dy1 O5 H5 128(5) . . ? Dy4 O6 Dy3 112.9(2) . . ? Dy4 O6 H6 134(5) . . ? Dy3 O6 H6 113(5) . . ? Dy1 O7 Dy3 114.17(19) . . ? Dy1 O7 H7 114(5) . . ? Dy3 O7 H7 131(5) . . ? Dy2 O8 Dy4 112.50(19) . . ? Dy2 O8 H8 108(5) . . ? Dy4 O8 H8 134(5) . . ? C68 O9 Dy6 122.1(3) . . ? C68 O9 Dy5 127.2(4) . . ? Dy6 O9 Dy5 107.94(14) . . ? C83 O10 Dy8 122.8(4) . . ? C83 O10 Dy7 124.3(4) . . ? Dy8 O10 Dy7 108.42(16) . . ? C98 O11 Dy7 122.8(4) . . ? C98 O11 Dy5 127.3(4) . . ? Dy7 O11 Dy5 107.53(14) . . ? C113 O12 Dy8 124.3(4) . . ? C113 O12 Dy6 122.4(4) . . ? Dy8 O12 Dy6 107.64(17) . . ? Dy5 O13 Dy6 113.43(17) . . ? Dy5 O13 H13 117(5) . . ? Dy6 O13 H13 127(4) . . ? Dy8 O14 Dy7 113.34(16) . . ? Dy8 O14 H14 125(4) . . ? Dy7 O14 H14 115(4) . . ? Dy5 O15 Dy7 113.83(17) . . ? Dy5 O15 H15 120(4) . . ? Dy7 O15 H15 126(5) . . ? Dy8 O16 Dy6 113.42(16) . . ? Dy8 O16 H16 109(4) . . ? Dy6 O16 H16 137(4) . . ? C1 N1 C5 116.3(6) . . ? C1 N1 Dy1 123.3(5) . . ? C5 N1 Dy1 120.1(4) . . ? C6 N2 N3 117.0(6) . . ? C6 N2 Dy1 123.6(5) . . ? N3 N2 Dy1 119.4(4) . . ? C8 N3 N2 109.6(5) . . ? C8 N4 N5 113.3(6) . . ? C10 N5 N4 118.0(6) . . ? C10 N5 Dy2 124.5(5) . . ? N4 N5 Dy2 117.4(4) . . ? C11 N6 C15 118.1(6) . . ? C11 N6 Dy2 119.9(5) . . ? C15 N6 Dy2 122.0(5) . . ? C16 N7 C20 118.4(7) . . ? C16 N7 Dy3 121.0(6) . . ? C20 N7 Dy3 120.3(4) . . ? C21 N8 N9 116.6(7) . . ? C21 N8 Dy3 124.1(5) . . ? N9 N8 Dy3 119.1(4) . . ? C23 N9 N8 111.6(7) . . ? N11 N10 C23 112.9(6) . . ? C25 N11 N10 118.6(7) . . ? C25 N11 Dy4 122.9(5) . . ? N10 N11 Dy4 118.5(4) . . ? C30 N12 C26 117.5(6) . . ? C30 N12 Dy4 122.2(6) . . ? C26 N12 Dy4 120.3(5) . . ? C31 N13 C35 117.6(7) . . ? C31 N13 Dy1 122.5(5) . . ? C35 N13 Dy1 119.9(5) . . ? C36 N14 N15 116.9(7) . . ? C36 N14 Dy1 124.3(5) . . ? N15 N14 Dy1 118.8(4) . . ? C38 N15 N14 111.8(6) . . ? C38 N16 N17 113.6(6) . . ? C38 N16 H16A 123.2 . . ? N17 N16 H16A 123.2 . . ? C40 N17 N16 118.9(7) . . ? C40 N17 Dy3 123.5(6) . . ? N16 N17 Dy3 117.6(4) . . ? C41 N18 C45 117.9(7) . . ? C41 N18 Dy3 119.3(6) . . ? C45 N18 Dy3 122.8(5) . . ? C50 N19 C46 117.4(6) . . ? C50 N19 Dy2 120.7(4) . . ? C46 N19 Dy2 121.7(5) . . ? C51 N20 N21 116.5(6) . . ? C51 N20 Dy2 125.1(5) . . ? N21 N20 Dy2 118.3(4) . . ? C53 N21 N20 111.2(6) . . ? C53 N22 N23 111.6(6) . . ? C53 N22 H22 124.2 . . ? N23 N22 H22 124.2 . . ? C55 N23 N22 117.6(7) . . ? C55 N23 Dy4 123.2(6) . . ? N22 N23 Dy4 118.4(4) . . ? C56 N24 C60 118.6(7) . . ? C56 N24 Dy4 119.5(5) . . ? C60 N24 Dy4 121.6(5) . . ? C65 N25 C61 116.8(6) . . ? C65 N25 Dy5 120.7(4) . . ? C61 N25 Dy5 122.2(4) . . ? C66 N26 N27 118.8(5) . . ? C66 N26 Dy5 123.7(4) . . ? N27 N26 Dy5 117.5(3) . . ? C68 N27 N26 114.7(5) . . ? C68 N27 H27 122.7 . . ? N26 N27 H27 122.7 . . ? C68 N28 N29 109.2(5) . . ? C70 N29 N28 116.9(5) . . ? C70 N29 Dy6 123.3(4) . . ? N28 N29 Dy6 119.8(3) . . ? C71 N30 C75 116.9(6) . . ? C71 N30 Dy6 119.9(4) . . ? C75 N30 Dy6 122.8(4) . . ? C76 N31 C80 116.7(6) . . ? C76 N31 Dy7 123.2(5) . . ? C80 N31 Dy7 120.1(4) . . ? C81 N32 N33 117.7(6) . . ? C81 N32 Dy7 124.1(4) . . ? N33 N32 Dy7 118.2(4) . . ? C83 N33 N32 111.6(5) . . ? C83 N34 N35 111.6(5) . . ? C83 N34 H34 124.2 . . ? N35 N34 H34 124.2 . . ? C85 N35 N34 117.6(7) . . ? C85 N35 Dy8 124.6(6) . . ? N34 N35 Dy8 117.5(3) . . ? C90 N36 C86 117.2(7) . . ? C90 N36 Dy8 122.9(6) . . ? C86 N36 Dy8 119.8(5) . . ? C91 N37 C95 117.0(6) . . ? C91 N37 Dy5 122.2(5) . . ? C95 N37 Dy5 120.4(4) . . ? C96 N38 N39 117.8(5) . . ? C96 N38 Dy5 123.8(4) . . ? N39 N38 Dy5 117.8(4) . . ? C98 N39 N38 113.4(5) . . ? C98 N40 N41 107.4(5) . . ? C100 N41 N40 115.6(5) . . ? C100 N41 Dy7 123.7(4) . . ? N40 N41 Dy7 120.6(3) . . ? C105 N42 C101 117.5(5) . . ? C105 N42 Dy7 122.7(4) . . ? C101 N42 Dy7 119.9(4) . . ? C106 N43 C110 116.9(6) . . ? C106 N43 Dy6 123.7(5) . . ? C110 N43 Dy6 119.2(4) . . ? C111 N44 N45 117.0(6) . . ? C111 N44 Dy6 123.2(5) . . ? N45 N44 Dy6 118.6(4) . . ? C113 N45 N44 110.6(5) . . ? C113 N46 N47 114.8(6) . . ? C115 N47 N46 118.7(7) . . ? C115 N47 Dy8 124.6(6) . . ? N46 N47 Dy8 116.6(4) . . ? C116 N48 C120 119.5(7) . . ? C116 N48 Dy8 120.2(5) . . ? C120 N48 Dy8 120.3(6) . . ? N1 C1 C2 125.8(7) . . ? N1 C1 H1 117.1 . . ? C2 C1 H1 117.1 . . ? C1 C2 C3 117.5(7) . . ? C1 C2 H2 121.3 . . ? C3 C2 H2 121.3 . . ? C4 C3 C2 118.3(8) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 120.8(8) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? N1 C5 C4 121.0(7) . . ? N1 C5 C6 115.9(6) . . ? C4 C5 C6 123.1(7) . . ? N2 C6 C5 117.3(7) . . ? N2 C6 C7 123.3(7) . . ? C5 C6 C7 119.3(6) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 N3 124.5(6) . . ? O1 C8 N4 119.3(6) . . ? N3 C8 N4 116.2(6) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 C11 114.4(6) . . ? N5 C10 C9 122.5(7) . . ? C11 C10 C9 123.1(6) . . ? N6 C11 C12 120.8(7) . . ? N6 C11 C10 118.1(6) . . ? C12 C11 C10 121.0(7) . . ? C13 C12 C11 121.6(8) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 117.4(7) . . ? C12 C13 H13A 121.3 . . ? C14 C13 H13A 121.3 . . ? C15 C14 C13 120.4(8) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? N6 C15 C14 121.8(7) . . ? N6 C15 H15A 119.1 . . ? C14 C15 H15A 119.1 . . ? N7 C16 C17 122.1(9) . . ? N7 C16 H16B 119.0 . . ? C17 C16 H16B 119.0 . . ? C18 C17 C16 118.6(9) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C17 C18 C19 119.9(8) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 122.2(10) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C19 C20 N7 118.8(8) . . ? C19 C20 C21 125.8(8) . . ? N7 C20 C21 115.4(6) . . ? N8 C21 C20 116.5(8) . . ? N8 C21 C22 123.4(7) . . ? C20 C21 C22 120.0(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 C23 N9 121.8(7) . . ? O2 C23 N10 119.8(6) . . ? N9 C23 N10 118.3(7) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 C26 116.5(7) . . ? N11 C25 C24 122.7(7) . . ? C26 C25 C24 120.7(6) . . ? N12 C26 C27 120.2(8) . . ? N12 C26 C25 116.5(6) . . ? C27 C26 C25 123.3(8) . . ? C28 C27 C26 121.3(9) . . ? C28 C27 H27A 119.3 . . ? C26 C27 H27A 119.3 . . ? C27 C28 C29 120.2(8) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C30 118.4(10) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? N12 C30 C29 122.4(10) . . ? N12 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? N13 C31 C32 122.5(9) . . ? N13 C31 H31 118.7 . . ? C32 C31 H31 118.7 . . ? C33 C32 C31 118.4(9) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C34 C33 C32 118.9(8) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 120.5(9) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? N13 C35 C34 122.0(9) . . ? N13 C35 C36 116.8(7) . . ? C34 C35 C36 121.2(8) . . ? N14 C36 C37 123.9(9) . . ? N14 C36 C35 115.1(7) . . ? C37 C36 C35 121.0(8) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O3 C38 N15 120.4(6) . . ? O3 C38 N16 120.3(8) . . ? N15 C38 N16 119.2(7) . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N17 C40 C41 115.4(8) . . ? N17 C40 C39 121.0(10) . . ? C41 C40 C39 123.6(8) . . ? N18 C41 C42 122.7(9) . . ? N18 C41 C40 118.4(7) . . ? C42 C41 C40 118.8(9) . . ? C43 C42 C41 119.1(10) . . ? C43 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? C42 C43 C44 120.9(9) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C45 C44 C43 117.1(11) . . ? C45 C44 H44 121.5 . . ? C43 C44 H44 121.5 . . ? N18 C45 C44 122.3(10) . . ? N18 C45 H45 118.9 . . ? C44 C45 H45 118.9 . . ? N19 C46 C47 124.0(8) . . ? N19 C46 H46 118.0 . . ? C47 C46 H46 118.0 . . ? C48 C47 C46 117.8(8) . . ? C48 C47 H47 121.1 . . ? C46 C47 H47 121.1 . . ? C47 C48 C49 120.5(8) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C48 C49 C50 118.9(9) . . ? C48 C49 H49 120.6 . . ? C50 C49 H49 120.6 . . ? N19 C50 C49 121.3(7) . . ? N19 C50 C51 117.2(6) . . ? C49 C50 C51 121.5(8) . . ? N20 C51 C52 124.1(7) . . ? N20 C51 C50 113.9(7) . . ? C52 C51 C50 122.0(7) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O4 C53 N22 121.7(6) . . ? O4 C53 N21 121.5(6) . . ? N22 C53 N21 116.8(7) . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N23 C55 C56 115.8(8) . . ? N23 C55 C54 122.6(9) . . ? C56 C55 C54 121.5(7) . . ? N24 C56 C57 121.6(9) . . ? N24 C56 C55 117.3(6) . . ? C57 C56 C55 121.1(9) . . ? C56 C57 C58 118.2(10) . . ? C56 C57 H57 120.9 . . ? C58 C57 H57 120.9 . . ? C59 C58 C57 119.1(8) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C58 C59 C60 120.3(10) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? N24 C60 C59 122.1(9) . . ? N24 C60 H60 119.0 . . ? C59 C60 H60 119.0 . . ? N25 C61 C62 123.3(8) . . ? N25 C61 H61 118.4 . . ? C62 C61 H61 118.4 . . ? C63 C62 C61 119.6(8) . . ? C63 C62 H62 120.2 . . ? C61 C62 H62 120.2 . . ? C62 C63 C64 119.2(7) . . ? C62 C63 H63 120.4 . . ? C64 C63 H63 120.4 . . ? C63 C64 C65 118.5(8) . . ? C63 C64 H64 120.7 . . ? C65 C64 H64 120.7 . . ? N25 C65 C64 122.6(7) . . ? N25 C65 C66 117.6(6) . . ? C64 C65 C66 119.7(7) . . ? N26 C66 C65 115.2(6) . . ? N26 C66 C67 123.9(6) . . ? C65 C66 C67 121.0(6) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N28 C68 O9 125.2(5) . . ? N28 C68 N27 117.2(5) . . ? O9 C68 N27 117.4(5) . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N29 C70 C69 124.3(7) . . ? N29 C70 C71 115.1(6) . . ? C69 C70 C71 120.6(6) . . ? N30 C71 C72 121.8(6) . . ? N30 C71 C70 116.6(5) . . ? C72 C71 C70 121.5(6) . . ? C73 C72 C71 119.8(7) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C74 C73 C72 118.2(6) . . ? C74 C73 H73 120.9 . . ? C72 C73 H73 120.9 . . ? C73 C74 C75 119.7(7) . . ? C73 C74 H74 120.2 . . ? C75 C74 H74 120.2 . . ? N30 C75 C74 123.5(7) . . ? N30 C75 H75 118.3 . . ? C74 C75 H75 118.3 . . ? N31 C76 C77 124.3(8) . . ? N31 C76 H76 117.8 . . ? C77 C76 H76 117.8 . . ? C78 C77 C76 119.4(7) . . ? C78 C77 H77 120.3 . . ? C76 C77 H77 120.3 . . ? C77 C78 C79 118.4(7) . . ? C77 C78 H78 120.8 . . ? C79 C78 H78 120.8 . . ? C78 C79 C80 119.8(8) . . ? C78 C79 H79 120.1 . . ? C80 C79 H79 120.1 . . ? N31 C80 C79 121.3(7) . . ? N31 C80 C81 116.7(6) . . ? C79 C80 C81 122.0(7) . . ? N32 C81 C82 123.2(7) . . ? N32 C81 C80 115.6(6) . . ? C82 C81 C80 121.1(6) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O10 C83 N34 123.4(6) . . ? O10 C83 N33 121.3(5) . . ? N34 C83 N33 115.3(6) . . ? C85 C84 H84A 109.5 . . ? C85 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C85 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N35 C85 C86 115.0(8) . . ? N35 C85 C84 125.0(9) . . ? C86 C85 C84 120.0(7) . . ? N36 C86 C87 121.8(9) . . ? N36 C86 C85 116.7(6) . . ? C87 C86 C85 121.5(9) . . ? C88 C87 C86 119.0(11) . . ? C88 C87 H87 120.5 . . ? C86 C87 H87 120.5 . . ? C87 C88 C89 121.3(9) . . ? C87 C88 H88 119.4 . . ? C89 C88 H88 119.4 . . ? C88 C89 C90 115.7(10) . . ? C88 C89 H89 122.1 . . ? C90 C89 H89 122.1 . . ? N36 C90 C89 125.0(9) . . ? N36 C90 H90 117.5 . . ? C89 C90 H90 117.5 . . ? N37 C91 C92 124.4(8) . . ? N37 C91 H91 117.8 . . ? C92 C91 H91 117.8 . . ? C93 C92 C91 118.5(8) . . ? C93 C92 H92 120.7 . . ? C91 C92 H92 120.7 . . ? C92 C93 C94 119.0(8) . . ? C92 C93 H93 120.5 . . ? C94 C93 H93 120.5 . . ? C95 C94 C93 118.6(8) . . ? C95 C94 H94 120.7 . . ? C93 C94 H94 120.7 . . ? N37 C95 C94 122.2(7) . . ? N37 C95 C96 116.5(6) . . ? C94 C95 C96 121.0(7) . . ? N38 C96 C95 115.2(6) . . ? N38 C96 C97 126.1(6) . . ? C95 C96 C97 118.7(6) . . ? C96 C97 H97A 109.5 . . ? C96 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C96 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? O11 C98 N40 126.4(6) . . ? O11 C98 N39 117.7(5) . . ? N40 C98 N39 115.9(5) . . ? C100 C99 H99A 109.5 . . ? C100 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C100 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? N41 C100 C101 115.6(5) . . ? N41 C100 C99 123.9(6) . . ? C101 C100 C99 120.5(6) . . ? N42 C101 C102 121.8(6) . . ? N42 C101 C100 117.3(5) . . ? C102 C101 C100 120.9(6) . . ? C103 C102 C101 119.4(6) . . ? C103 C102 H102 120.3 . . ? C101 C102 H102 120.3 . . ? C104 C103 C102 120.4(6) . . ? C104 C103 H103 119.8 . . ? C102 C103 H103 119.8 . . ? C103 C104 C105 117.7(7) . . ? C103 C104 H104 121.1 . . ? C105 C104 H104 121.1 . . ? N42 C105 C104 123.2(7) . . ? N42 C105 H105 118.4 . . ? C104 C105 H105 118.4 . . ? N43 C106 C107 125.1(8) . . ? N43 C106 H106 117.4 . . ? C107 C106 H106 117.4 . . ? C106 C107 C108 118.0(8) . . ? C106 C107 H107 121.0 . . ? C108 C107 H107 121.0 . . ? C107 C108 C109 118.9(9) . . ? C107 C108 H108 120.6 . . ? C109 C108 H108 120.6 . . ? C110 C109 C108 118.2(10) . . ? C110 C109 H109 120.9 . . ? C108 C109 H109 120.9 . . ? N43 C110 C109 122.9(8) . . ? N43 C110 C111 117.3(6) . . ? C109 C110 C111 119.8(8) . . ? N44 C111 C110 116.0(7) . . ? N44 C111 C112 124.2(7) . . ? C110 C111 C112 119.7(7) . . ? C111 C112 H11A 109.5 . . ? C111 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? C111 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? O12 C113 N45 123.4(6) . . ? O12 C113 N46 118.7(6) . . ? N45 C113 N46 117.9(6) . . ? C115 C114 H11D 109.5 . . ? C115 C114 H11E 109.5 . . ? H11D C114 H11E 109.5 . . ? C115 C114 H11F 109.5 . . ? H11D C114 H11F 109.5 . . ? H11E C114 H11F 109.5 . . ? N47 C115 C116 116.3(7) . . ? N47 C115 C114 124.1(8) . . ? C116 C115 C114 119.6(7) . . ? N48 C116 C117 119.0(9) . . ? N48 C116 C115 117.0(7) . . ? C117 C116 C115 123.9(9) . . ? C116 C117 C118 119.5(10) . . ? C116 C117 H117 120.3 . . ? C118 C117 H117 120.3 . . ? C119 C118 C117 120.0(8) . . ? C119 C118 H118 120.0 . . ? C117 C118 H118 120.0 . . ? C118 C119 C120 120.4(10) . . ? C118 C119 H119 119.8 . . ? C120 C119 H119 119.8 . . ? C119 C120 N48 121.5(10) . . ? C119 C120 H120 119.2 . . ? N48 C120 H120 119.2 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.723 _refine_diff_density_min -3.290 _refine_diff_density_rms 0.134 _iucr_refine_instructions_details ; TITL _1 CELL 0.71075 17.77170 22.27550 27.84310 110.343 95.225 106.955 ZERR 4 0.00070 0.00080 0.00190 0.008 0.007 0.008 LATT 1 SFAC C H DY N O CL UNIT 240 416 16 96 116 8 SHEL 8.147180 0.796452 L.S. 7 FMAP 2 PLAN -20 TEMP -110.0 ACTA BOND $H OMIT 0 4 4 OMIT -1 5 1 OMIT -2 3 0 DFIX 0.87 O5 H5 DFIX 0.87 O6 H6 DFIX 0.87 O7 H7 DFIX 0.87 O8 H8 DFIX 0.87 O13 H13 DFIX 0.87 O14 H14 DFIX 0.87 O15 H15 DFIX 0.87 O16 H16 SIZE 0.190 0.320 0.260 WGHT 0.076500 FVAR 1.01441 DY1 3 -0.065854 0.733334 0.234120 11.00000 0.04357 0.04095 = 0.04148 0.01070 -0.00267 0.01951 DY2 3 -0.070800 0.611535 0.301344 11.00000 0.03697 0.03343 = 0.04617 0.01087 -0.00024 0.00757 DY3 3 0.140905 0.847467 0.318754 11.00000 0.05454 0.03081 = 0.04403 0.01611 -0.00606 0.00587 DY4 3 0.136066 0.724429 0.384258 11.00000 0.04191 0.03591 = 0.04641 0.02012 -0.00635 0.00468 DY5 3 0.247318 0.229026 0.089422 11.00000 0.04519 0.03615 = 0.03449 0.01127 -0.00132 0.01496 DY6 3 0.360585 0.120262 0.115565 11.00000 0.03453 0.03709 = 0.03601 0.01379 0.00817 0.01421 DY7 3 0.330733 0.358013 0.229383 11.00000 0.03795 0.03222 = 0.03305 0.01255 0.00408 0.01141 DY8 3 0.438648 0.245832 0.256423 11.00000 0.04480 0.04176 = 0.03515 0.01458 0.00072 0.01793 CL1 6 0.127842 0.634993 0.200050 11.00000 0.13792 0.10443 = 0.12405 0.05647 0.03590 0.06326 CL2 6 -0.329775 0.765986 0.462496 11.00000 0.23185 0.09914 = 0.20307 0.00982 0.07372 0.05750 CL3 6 0.516005 0.319822 0.122832 11.00000 0.18277 0.17530 = 0.22199 0.05512 -0.00430 0.00357 CL4 6 0.156155 1.147571 0.211083 11.00000 0.13702 0.10100 = 0.14091 0.06224 0.06177 0.05723 O1 5 -0.084780 0.619628 0.220421 11.00000 0.04855 0.03671 = 0.04403 0.00509 -0.01030 0.01073 O2 5 0.209451 0.780451 0.337746 11.00000 0.04076 0.04653 = 0.05882 0.02961 0.00743 0.01157 O3 5 0.010022 0.844436 0.292452 11.00000 0.06790 0.03860 = 0.04924 0.01097 0.00102 0.02872 O4 5 0.004030 0.670237 0.387759 11.00000 0.04578 0.04095 = 0.04281 0.01187 -0.00205 0.00344 O5 5 -0.088695 0.709951 0.305755 11.00000 0.05646 0.04616 = 0.04536 0.01419 0.00635 0.02724 H5 2 -0.098848 0.735274 0.334619 11.00000 -1.50000 O6 5 0.095691 0.810227 0.380270 11.00000 0.06923 0.04289 = 0.04256 0.02093 -0.00135 0.01683 H6 2 0.061887 0.829102 0.394644 11.00000 -1.50000 O7 5 0.067915 0.754615 0.246275 11.00000 0.04302 0.03201 = 0.04424 0.01012 -0.00025 0.01005 H7 2 0.081955 0.724272 0.223198 11.00000 -1.50000 O8 5 0.062778 0.642580 0.304917 11.00000 0.03619 0.03548 = 0.04076 0.01059 -0.00317 0.00499 H8 2 0.069696 0.632346 0.272792 11.00000 -1.50000 O9 5 0.233956 0.119127 0.084073 11.00000 0.03324 0.03376 = 0.04374 0.01273 0.00709 0.00979 O10 5 0.349189 0.302201 0.284384 11.00000 0.05340 0.04631 = 0.03424 0.01880 0.01403 0.02085 O11 5 0.318942 0.345098 0.141859 11.00000 0.05598 0.03211 = 0.03265 0.00993 0.00043 0.00807 O12 5 0.477784 0.188176 0.181631 11.00000 0.03733 0.04983 = 0.04732 0.01737 0.00798 0.01847 O13 5 0.365890 0.211876 0.096142 11.00000 0.04283 0.04294 = 0.04261 0.01668 0.00953 0.01527 H13 2 0.409682 0.247041 0.101047 11.00000 -1.50000 O14 5 0.438515 0.322934 0.221006 11.00000 0.04025 0.03847 = 0.02954 0.01346 0.00869 0.01466 H14 2 0.459053 0.325113 0.194660 11.00000 -1.50000 O15 5 0.235717 0.258185 0.173524 11.00000 0.03491 0.03637 = 0.04028 0.01054 0.00418 0.00929 H15 2 0.195783 0.233102 0.181665 11.00000 -1.50000 O16 5 0.334246 0.158562 0.196505 11.00000 0.03995 0.03774 = 0.03287 0.01590 0.00983 0.01308 H16 2 0.292037 0.153679 0.210168 11.00000 -1.50000 N1 4 -0.059108 0.782153 0.164114 11.00000 0.05957 0.05944 = 0.05695 0.02006 -0.00570 0.03327 N2 4 -0.071625 0.653922 0.142195 11.00000 0.05173 0.04992 = 0.04326 0.00580 -0.00286 0.01874 N3 4 -0.076792 0.586677 0.132465 11.00000 0.07157 0.04380 = 0.04570 0.01485 0.00737 0.01973 N4 4 -0.076305 0.515262 0.174440 11.00000 0.07076 0.03773 = 0.06368 0.00843 0.00724 0.01594 N5 4 -0.074341 0.509037 0.222735 11.00000 0.04234 0.03931 = 0.05529 0.01213 0.00720 0.01347 N6 4 -0.068820 0.505615 0.317405 11.00000 0.03916 0.03311 = 0.07996 0.02167 0.00437 0.00592 N7 4 0.190405 0.924272 0.269492 11.00000 0.09413 0.04132 = 0.04660 0.02137 -0.01366 0.01486 N8 4 0.264028 0.840936 0.281035 11.00000 0.06006 0.05202 = 0.05268 0.02667 -0.00412 0.00521 N9 4 0.298517 0.795098 0.285984 11.00000 0.04592 0.06948 = 0.07243 0.03862 0.00572 0.01352 N10 4 0.290302 0.715575 0.321595 11.00000 0.03500 0.06016 = 0.07281 0.03773 0.00855 0.01138 N11 4 0.251712 0.688409 0.353082 11.00000 0.04150 0.05358 = 0.06154 0.02645 -0.00709 0.01059 N12 4 0.170042 0.638613 0.415060 11.00000 0.05574 0.05284 = 0.07251 0.03806 -0.01231 0.00457 N13 4 -0.216257 0.689370 0.193506 11.00000 0.04183 0.07456 = 0.05956 0.02450 -0.00325 0.01869 N14 4 -0.138844 0.817153 0.263833 11.00000 0.06842 0.07320 = 0.06103 0.02746 0.00862 0.04491 N15 4 -0.097418 0.880660 0.302780 11.00000 0.08982 0.07279 = 0.06489 0.01324 0.00290 0.05593 N16 4 0.029406 0.948723 0.357258 11.00000 0.14231 0.03754 = 0.06541 -0.00370 0.00946 0.04726 AFIX 43 H16A 2 0.012633 0.982320 0.373631 11.00000 -1.20000 AFIX 0 N17 4 0.107522 0.950968 0.369406 11.00000 0.10779 0.03940 = 0.05073 0.00522 -0.00208 0.03818 N18 4 0.255777 0.947873 0.389011 11.00000 0.08960 0.03665 = 0.05076 0.01530 -0.01266 0.00301 N19 4 -0.221118 0.542967 0.275055 11.00000 0.03856 0.04252 = 0.06456 0.00810 0.00253 0.01067 N20 4 -0.147912 0.620549 0.374070 11.00000 0.04331 0.04532 = 0.05715 0.01591 0.00593 0.01445 N21 4 -0.107016 0.665364 0.424952 11.00000 0.05551 0.05441 = 0.05648 0.01556 0.00912 0.01363 N22 4 0.018414 0.736305 0.474311 11.00000 0.08388 0.05992 = 0.04014 0.01657 0.00814 0.00717 AFIX 43 H22 2 -0.000322 0.749876 0.502871 11.00000 -1.20000 AFIX 0 N23 4 0.099589 0.760620 0.471888 11.00000 0.07863 0.05708 = 0.04147 0.02763 -0.00299 0.00434 N24 4 0.250016 0.806994 0.462295 11.00000 0.06969 0.04789 = 0.05519 0.02557 -0.01278 0.00256 N25 4 0.130812 0.267975 0.071517 11.00000 0.05366 0.04755 = 0.03630 0.00673 -0.00914 0.02266 N26 4 0.104805 0.143014 0.068268 11.00000 0.03548 0.04515 = 0.04688 0.00515 -0.00655 0.00994 N27 4 0.097343 0.078980 0.067090 11.00000 0.02921 0.04272 = 0.06052 0.00354 -0.00261 0.00647 AFIX 43 H27 2 0.050417 0.046205 0.058792 11.00000 -1.20000 AFIX 0 N28 4 0.164010 0.013563 0.082975 11.00000 0.03786 0.04093 = 0.05985 0.01634 0.00866 0.00964 N29 4 0.242146 0.014588 0.097115 11.00000 0.04932 0.03096 = 0.05462 0.01639 0.01401 0.01412 N30 4 0.391725 0.022960 0.130023 11.00000 0.05313 0.05007 = 0.04478 0.01358 0.01367 0.02727 N31 4 0.238044 0.428049 0.236484 11.00000 0.04256 0.04045 = 0.05129 0.00932 -0.00110 0.01563 N32 4 0.238822 0.353417 0.293765 11.00000 0.04302 0.03901 = 0.03766 0.01245 0.00550 0.01486 N33 4 0.240290 0.311827 0.320424 11.00000 0.06030 0.05363 = 0.03976 0.01640 0.01979 0.01945 N34 4 0.301165 0.240453 0.333046 11.00000 0.08102 0.06714 = 0.04232 0.03672 0.02768 0.02781 AFIX 43 H34 2 0.268437 0.229618 0.352973 11.00000 -1.20000 AFIX 0 N35 4 0.361498 0.213379 0.320299 11.00000 0.07289 0.05046 = 0.04106 0.02261 0.00749 0.02812 N36 4 0.478860 0.166731 0.292367 11.00000 0.10130 0.05432 = 0.04622 0.00882 -0.00673 0.04167 N37 4 0.224005 0.175298 -0.011489 11.00000 0.07176 0.04890 = 0.03469 0.00641 -0.00275 0.02300 N38 4 0.308883 0.307292 0.043329 11.00000 0.07612 0.04677 = 0.03742 0.02097 0.00690 0.01481 N39 4 0.353064 0.375287 0.074413 11.00000 0.09055 0.04794 = 0.03662 0.01970 0.01200 0.02354 N40 4 0.414542 0.451107 0.158948 11.00000 0.06647 0.03922 = 0.04514 0.02011 0.00968 0.01338 N41 4 0.414917 0.456650 0.210681 11.00000 0.04979 0.03583 = 0.04104 0.01508 0.00331 0.01387 N42 4 0.415479 0.466184 0.309199 11.00000 0.04341 0.04044 = 0.04770 0.00869 0.00161 0.01548 N43 4 0.357470 0.047442 0.021227 11.00000 0.05549 0.05157 = 0.04312 0.01424 0.01356 0.02533 N44 4 0.494119 0.136181 0.087909 11.00000 0.04256 0.06621 = 0.05223 0.01541 0.01604 0.01861 N45 4 0.563699 0.186143 0.124009 11.00000 0.03137 0.08066 = 0.06716 0.01737 0.01086 0.01701 N46 4 0.608296 0.259459 0.209655 11.00000 0.03500 0.07661 = 0.06521 0.01371 -0.00127 0.01299 N47 4 0.586197 0.286276 0.256818 11.00000 0.04277 0.06492 = 0.06402 0.02217 -0.00854 0.01501 N48 4 0.535121 0.336535 0.341683 11.00000 0.07853 0.06656 = 0.04314 0.01585 -0.00596 0.03199 C1 1 -0.045127 0.848465 0.174561 11.00000 0.08411 0.06069 = 0.04687 0.01681 0.00077 0.04198 AFIX 43 H1 2 -0.040256 0.877393 0.209912 11.00000 -1.20000 AFIX 0 C2 1 -0.037347 0.877810 0.139232 11.00000 0.11258 0.07383 = 0.07594 0.03826 0.00620 0.05164 AFIX 43 H2 2 -0.030961 0.924627 0.149011 11.00000 -1.20000 AFIX 0 C3 1 -0.039096 0.835945 0.086980 11.00000 0.12879 0.09066 = 0.07334 0.04468 0.00784 0.05955 AFIX 43 H3 2 -0.029778 0.854771 0.061332 11.00000 -1.20000 AFIX 0 C4 1 -0.054503 0.767993 0.074571 11.00000 0.12068 0.08522 = 0.04791 0.02341 -0.00334 0.06219 AFIX 43 H4 2 -0.060337 0.738485 0.039243 11.00000 -1.20000 AFIX 0 C5 1 -0.061752 0.741472 0.112973 11.00000 0.05884 0.06331 = 0.04172 0.01790 -0.00274 0.02887 C6 1 -0.072103 0.671119 0.102797 11.00000 0.07560 0.05840 = 0.04853 0.01918 0.00388 0.02575 C7 1 -0.080416 0.621468 0.046486 11.00000 0.17693 0.07621 = 0.05265 0.02280 0.01467 0.04588 AFIX 137 H7A 2 -0.031543 0.637172 0.033986 11.00000 -1.20000 H7B 2 -0.127010 0.619723 0.023624 11.00000 -1.20000 H7C 2 -0.087998 0.575835 0.045927 11.00000 -1.20000 AFIX 0 C8 1 -0.079170 0.576100 0.176667 11.00000 0.05203 0.04269 = 0.04583 0.00070 -0.00232 0.01167 C9 1 -0.062371 0.395914 0.178314 11.00000 0.08073 0.04229 = 0.09347 0.01515 0.02253 0.02349 AFIX 137 H9A 2 -0.102534 0.352286 0.173571 11.00000 -1.20000 H9B 2 -0.008272 0.393605 0.184300 11.00000 -1.20000 H9C 2 -0.071378 0.405258 0.146786 11.00000 -1.20000 AFIX 0 C10 1 -0.069955 0.452218 0.224911 11.00000 0.04865 0.03899 = 0.07342 0.01274 0.00777 0.01249 C11 1 -0.070517 0.449150 0.276898 11.00000 0.04181 0.04094 = 0.07761 0.02100 0.00492 0.01223 C12 1 -0.068650 0.391042 0.284913 11.00000 0.04987 0.04670 = 0.09022 0.03293 0.01323 0.01937 AFIX 43 H12 2 -0.069504 0.352254 0.255959 11.00000 -1.20000 AFIX 0 C13 1 -0.065649 0.388673 0.333000 11.00000 0.04855 0.05427 = 0.10568 0.03955 0.01160 0.01835 AFIX 43 H13A 2 -0.063973 0.349173 0.338334 11.00000 -1.20000 AFIX 0 C14 1 -0.065117 0.446582 0.374409 11.00000 0.04470 0.06626 = 0.10533 0.05339 0.00708 0.01432 AFIX 43 H14A 2 -0.063595 0.446686 0.408633 11.00000 -1.20000 AFIX 0 C15 1 -0.066785 0.503481 0.365904 11.00000 0.04140 0.05664 = 0.06051 0.02823 0.00220 0.01165 AFIX 43 H15A 2 -0.066513 0.542340 0.394557 11.00000 -1.20000 AFIX 0 C16 1 0.150564 0.964533 0.262478 11.00000 0.09366 0.03979 = 0.05659 0.01868 -0.00526 0.01858 AFIX 43 H16B 2 0.099903 0.959964 0.272115 11.00000 -1.20000 AFIX 0 C17 1 0.181616 1.013262 0.241287 11.00000 0.14907 0.04200 = 0.05484 0.01639 -0.00423 0.02598 AFIX 43 H17 2 0.152300 1.040946 0.236434 11.00000 -1.20000 AFIX 0 C18 1 0.253829 1.019761 0.228044 11.00000 0.13134 0.05685 = 0.04859 0.02421 0.02186 0.01351 AFIX 43 H18 2 0.276695 1.053213 0.214682 11.00000 -1.20000 AFIX 0 C19 1 0.293677 0.978509 0.233832 11.00000 0.10576 0.05355 = 0.06387 0.03239 0.02186 0.00348 AFIX 43 H19 2 0.344092 0.983205 0.223819 11.00000 -1.20000 AFIX 0 C20 1 0.263574 0.930016 0.253732 11.00000 0.06472 0.05995 = 0.03957 0.01963 0.00871 -0.00407 C21 1 0.301172 0.882001 0.259730 11.00000 0.06363 0.06240 = 0.05254 0.03022 -0.00009 0.00167 C22 1 0.379089 0.882731 0.243208 11.00000 0.07800 0.10618 = 0.08776 0.06257 0.03291 0.02252 AFIX 137 H22A 2 0.416014 0.881057 0.270695 11.00000 -1.20000 H22B 2 0.403122 0.924611 0.237522 11.00000 -1.20000 H22C 2 0.369180 0.843004 0.210582 11.00000 -1.20000 AFIX 0 C23 1 0.264149 0.764130 0.314593 11.00000 0.04133 0.05473 = 0.06067 0.02403 -0.00176 0.00554 C24 1 0.339644 0.617497 0.342704 11.00000 0.05814 0.07241 = 0.11243 0.04095 0.00547 0.02404 AFIX 137 H24A 2 0.352009 0.631919 0.313984 11.00000 -1.20000 H24B 2 0.321542 0.567595 0.329641 11.00000 -1.20000 H24C 2 0.388055 0.637205 0.370707 11.00000 -1.20000 AFIX 0 C25 1 0.273495 0.641942 0.364063 11.00000 0.04960 0.05239 = 0.06370 0.01895 -0.00973 0.02100 C26 1 0.231521 0.615506 0.399440 11.00000 0.05392 0.04302 = 0.06554 0.02218 -0.01423 0.00520 C27 1 0.251424 0.569307 0.417577 11.00000 0.08289 0.06530 = 0.07807 0.03535 -0.00916 0.03101 AFIX 43 H27A 2 0.294753 0.554709 0.407266 11.00000 -1.20000 AFIX 0 C28 1 0.211140 0.545860 0.448604 11.00000 0.13811 0.07126 = 0.08886 0.04159 -0.02764 0.03777 AFIX 43 H28 2 0.225392 0.514450 0.460169 11.00000 -1.20000 AFIX 0 C29 1 0.148570 0.566733 0.464269 11.00000 0.12268 0.05083 = 0.07538 0.03507 -0.01631 0.01390 AFIX 43 H29 2 0.119109 0.549998 0.486515 11.00000 -1.20000 AFIX 0 C30 1 0.129209 0.613568 0.446515 11.00000 0.09271 0.07790 = 0.06708 0.04999 0.00024 0.01587 AFIX 43 H30 2 0.085892 0.628025 0.457056 11.00000 -1.20000 AFIX 0 C31 1 -0.255149 0.625697 0.159829 11.00000 0.04756 0.09518 = 0.06536 0.04232 0.00359 0.02457 AFIX 43 H31 2 -0.225894 0.595399 0.150069 11.00000 -1.20000 AFIX 0 C32 1 -0.338486 0.601104 0.137860 11.00000 0.06484 0.12616 = 0.07218 0.06127 -0.00529 -0.00285 AFIX 43 H32 2 -0.365235 0.554814 0.114590 11.00000 -1.20000 AFIX 0 C33 1 -0.379915 0.645776 0.150971 11.00000 0.04740 0.15265 = 0.08607 0.05507 0.00464 0.04351 AFIX 43 H33 2 -0.435906 0.630987 0.136685 11.00000 -1.20000 AFIX 0 C34 1 -0.339792 0.710941 0.184445 11.00000 0.06478 0.14082 = 0.07382 0.05929 0.01799 0.06064 AFIX 43 H34A 2 -0.367337 0.742692 0.192919 11.00000 -1.20000 AFIX 0 C35 1 -0.259226 0.731803 0.206427 11.00000 0.06038 0.12167 = 0.06902 0.05265 0.02586 0.06088 C36 1 -0.213443 0.804688 0.244818 11.00000 0.09031 0.09818 = 0.07000 0.03888 0.02639 0.07362 C37 1 -0.254517 0.856339 0.259810 11.00000 0.09751 0.12704 = 0.14321 0.03630 0.02670 0.08203 AFIX 137 H37A 2 -0.253993 0.871505 0.297404 11.00000 -1.20000 H37B 2 -0.310332 0.835750 0.239836 11.00000 -1.20000 H37C 2 -0.226108 0.895565 0.252002 11.00000 -1.20000 AFIX 0 C38 1 -0.019260 0.889534 0.317501 11.00000 0.09220 0.04900 = 0.05102 0.01969 0.01197 0.03605 C39 1 0.136774 1.067776 0.434671 11.00000 0.18185 0.05852 = 0.08566 -0.01471 0.00208 0.04432 AFIX 137 H39A 2 0.098914 1.072649 0.409630 11.00000 -1.20000 H39B 2 0.185228 1.108786 0.448958 11.00000 -1.20000 H39C 2 0.111379 1.061822 0.463292 11.00000 -1.20000 AFIX 0 C40 1 0.159796 1.005675 0.406883 11.00000 0.13534 0.03521 = 0.05733 0.00869 0.01522 0.02093 C41 1 0.240984 1.003126 0.418220 11.00000 0.10146 0.06148 = 0.05037 0.03203 -0.00214 0.01287 C42 1 0.300873 1.059874 0.460721 11.00000 0.12513 0.05222 = 0.05054 0.01308 -0.00899 0.00106 AFIX 43 H42 2 0.288251 1.098513 0.480667 11.00000 -1.20000 AFIX 0 C43 1 0.371776 1.057466 0.471284 11.00000 0.12277 0.08153 = 0.07164 0.02259 -0.03530 -0.01451 AFIX 43 H43 2 0.411189 1.094173 0.499785 11.00000 -1.20000 AFIX 0 C44 1 0.392100 0.999743 0.440391 11.00000 0.08876 0.08888 = 0.10228 0.05078 -0.02943 -0.03895 AFIX 43 H44 2 0.444326 0.997659 0.447724 11.00000 -1.20000 AFIX 0 C45 1 0.331275 0.946781 0.399006 11.00000 0.07685 0.05564 = 0.07029 0.03353 -0.01290 -0.00312 AFIX 43 H45 2 0.343514 0.908872 0.377268 11.00000 -1.20000 AFIX 0 C46 1 -0.258045 0.502325 0.224788 11.00000 0.05226 0.04748 = 0.06015 0.00715 0.00428 0.00694 AFIX 43 H46 2 -0.227902 0.503859 0.198489 11.00000 -1.20000 AFIX 0 C47 1 -0.337561 0.458287 0.209066 11.00000 0.03652 0.05824 = 0.08894 0.00767 -0.00326 0.00645 AFIX 43 H47 2 -0.361343 0.430917 0.173071 11.00000 -1.20000 AFIX 0 C48 1 -0.379536 0.455684 0.246268 11.00000 0.03462 0.07134 = 0.12326 0.01899 0.00561 -0.00015 AFIX 43 H48 2 -0.433364 0.424775 0.236830 11.00000 -1.20000 AFIX 0 C49 1 -0.345257 0.497548 0.298249 11.00000 0.03291 0.06197 = 0.12274 0.02648 0.02084 0.01792 AFIX 43 H49 2 -0.375412 0.496426 0.324596 11.00000 -1.20000 AFIX 0 C50 1 -0.264991 0.541857 0.311533 11.00000 0.04210 0.05200 = 0.07580 0.01122 0.00609 0.01919 C51 1 -0.224087 0.588880 0.367583 11.00000 0.05361 0.04537 = 0.06780 0.02269 0.01617 0.02057 C52 1 -0.269314 0.598832 0.410374 11.00000 0.05994 0.08350 = 0.08457 0.00697 0.02626 0.02271 AFIX 137 H52A 2 -0.308489 0.554808 0.405732 11.00000 -1.20000 H52B 2 -0.297634 0.630230 0.409303 11.00000 -1.20000 H52C 2 -0.231639 0.618021 0.444299 11.00000 -1.20000 AFIX 0 C53 1 -0.026845 0.690050 0.427935 11.00000 0.05140 0.03972 = 0.04292 0.01415 0.00427 0.00646 C54 1 0.125321 0.833458 0.565328 11.00000 0.14540 0.10791 = 0.07204 -0.01267 0.01766 -0.01791 AFIX 137 H54A 2 0.087240 0.794832 0.569666 11.00000 -1.20000 H54B 2 0.099655 0.867067 0.565957 11.00000 -1.20000 H54C 2 0.173075 0.854689 0.593974 11.00000 -1.20000 AFIX 0 C55 1 0.149664 0.808777 0.514170 11.00000 0.10633 0.05760 = 0.04038 0.01196 -0.00931 -0.01291 C56 1 0.233037 0.834493 0.509338 11.00000 0.09136 0.05461 = 0.05040 0.02808 -0.02322 -0.01408 C57 1 0.291646 0.886782 0.551481 11.00000 0.11222 0.08905 = 0.04919 0.02326 -0.01629 -0.01876 AFIX 43 H57 2 0.278945 0.905940 0.584568 11.00000 -1.20000 AFIX 0 C58 1 0.370989 0.910699 0.543633 11.00000 0.10294 0.07840 = 0.08431 0.03083 -0.04549 -0.03254 AFIX 43 H58 2 0.412070 0.947335 0.571175 11.00000 -1.20000 AFIX 0 C59 1 0.387117 0.880914 0.496885 11.00000 0.05771 0.10452 = 0.07417 0.02552 -0.02309 -0.01418 AFIX 43 H59 2 0.440314 0.895591 0.491515 11.00000 -1.20000 AFIX 0 C60 1 0.327137 0.829311 0.456738 11.00000 0.05908 0.05474 = 0.07025 0.02659 -0.01583 -0.00593 AFIX 43 H60 2 0.339957 0.808529 0.424013 11.00000 -1.20000 AFIX 0 C61 1 0.142182 0.333467 0.077274 11.00000 0.07151 0.05706 = 0.04640 0.00934 -0.01021 0.02741 AFIX 43 H61 2 0.195724 0.363799 0.083882 11.00000 -1.20000 AFIX 0 C62 1 0.079042 0.358272 0.073947 11.00000 0.12119 0.07413 = 0.03687 0.00894 -0.00086 0.06768 AFIX 43 H62 2 0.090077 0.404784 0.079334 11.00000 -1.20000 AFIX 0 C63 1 0.001137 0.315137 0.062872 11.00000 0.11003 0.11003 = 0.04357 0.01801 0.01057 0.08429 AFIX 43 H63 2 -0.042367 0.331104 0.059616 11.00000 -1.20000 AFIX 0 C64 1 -0.013501 0.247804 0.056461 11.00000 0.06342 0.08820 = 0.04608 0.01535 -0.00494 0.04618 AFIX 43 H64 2 -0.067006 0.217068 0.049154 11.00000 -1.20000 AFIX 0 C65 1 0.053589 0.225769 0.061087 11.00000 0.07853 0.06589 = 0.02602 0.00962 -0.00516 0.03871 C66 1 0.040142 0.155894 0.057926 11.00000 0.05228 0.06241 = 0.04158 0.01142 0.00167 0.03242 C67 1 -0.044241 0.104672 0.044376 11.00000 0.04637 0.08150 = 0.07523 0.02582 -0.00366 0.02315 AFIX 137 H67A 2 -0.044192 0.058878 0.024020 11.00000 -1.20000 H67B 2 -0.080752 0.116438 0.023605 11.00000 -1.20000 H67C 2 -0.062392 0.105548 0.076731 11.00000 -1.20000 AFIX 0 C68 1 0.167745 0.070693 0.079679 11.00000 0.03005 0.04528 = 0.04995 0.01395 0.00699 0.01600 C69 1 0.180386 -0.105444 0.086557 11.00000 0.08321 0.05164 = 0.12873 0.05433 0.00718 0.01491 AFIX 137 H69A 2 0.130374 -0.099891 0.074274 11.00000 -1.20000 H69B 2 0.177285 -0.114240 0.118578 11.00000 -1.20000 H69C 2 0.187919 -0.143959 0.059388 11.00000 -1.20000 AFIX 0 C70 1 0.249256 -0.042351 0.097784 11.00000 0.06879 0.03963 = 0.05182 0.01768 0.01311 0.02319 C71 1 0.333782 -0.039009 0.113101 11.00000 0.05776 0.05449 = 0.05415 0.02582 0.01177 0.03131 C72 1 0.350992 -0.096504 0.112736 11.00000 0.08581 0.04984 = 0.08223 0.03190 0.02896 0.03752 AFIX 43 H72 2 0.309458 -0.139953 0.099084 11.00000 -1.20000 AFIX 0 C73 1 0.429133 -0.089944 0.132423 11.00000 0.11093 0.06960 = 0.07679 0.04331 0.04537 0.06808 AFIX 43 H73 2 0.441908 -0.128547 0.132273 11.00000 -1.20000 AFIX 0 C74 1 0.486449 -0.027039 0.151797 11.00000 0.07328 0.08609 = 0.06524 0.04222 0.03064 0.05620 AFIX 43 H74 2 0.539698 -0.020523 0.167157 11.00000 -1.20000 AFIX 0 C75 1 0.467048 0.027740 0.149105 11.00000 0.07131 0.06409 = 0.05378 0.02420 0.01591 0.03841 AFIX 43 H75 2 0.508786 0.070952 0.161288 11.00000 -1.20000 AFIX 0 C76 1 0.236210 0.465735 0.208089 11.00000 0.06527 0.04389 = 0.04637 0.01616 0.00074 0.01842 AFIX 43 H76 2 0.268435 0.463567 0.182547 11.00000 -1.20000 AFIX 0 C77 1 0.190582 0.507421 0.213567 11.00000 0.07943 0.04567 = 0.07581 0.01552 -0.00920 0.03291 AFIX 43 H77 2 0.191574 0.532591 0.192068 11.00000 -1.20000 AFIX 0 C78 1 0.144054 0.512133 0.250142 11.00000 0.04167 0.04867 = 0.10264 0.01408 0.00073 0.02215 AFIX 43 H78 2 0.112824 0.541035 0.254942 11.00000 -1.20000 AFIX 0 C79 1 0.143447 0.473966 0.279953 11.00000 0.04410 0.05678 = 0.09372 0.01279 0.00819 0.02505 AFIX 43 H79 2 0.111856 0.476560 0.305859 11.00000 -1.20000 AFIX 0 C80 1 0.190064 0.430840 0.271867 11.00000 0.03240 0.03911 = 0.05875 0.00302 -0.00545 0.01105 C81 1 0.190852 0.387355 0.303029 11.00000 0.03886 0.05176 = 0.05411 0.00786 0.01549 0.01334 C82 1 0.136489 0.382922 0.340081 11.00000 0.05829 0.05941 = 0.08441 0.01482 0.03392 0.02272 AFIX 137 H82A 2 0.095299 0.337264 0.326120 11.00000 -1.20000 H82B 2 0.110447 0.417116 0.344486 11.00000 -1.20000 H82C 2 0.167837 0.391458 0.374097 11.00000 -1.20000 AFIX 0 C83 1 0.299095 0.284858 0.311316 11.00000 0.06222 0.04582 = 0.04033 0.01899 0.01193 0.02033 C84 1 0.314772 0.141335 0.370802 11.00000 0.14524 0.07874 = 0.07058 0.05299 0.04015 0.04882 AFIX 137 H84A 2 0.266817 0.154402 0.369049 11.00000 -1.20000 H84B 2 0.344140 0.160717 0.407343 11.00000 -1.20000 H84C 2 0.298470 0.091477 0.357019 11.00000 -1.20000 AFIX 0 C85 1 0.368695 0.168242 0.338337 11.00000 0.10306 0.05415 = 0.04361 0.02157 -0.00477 0.01750 C86 1 0.434099 0.141452 0.323468 11.00000 0.10532 0.05498 = 0.03828 0.01329 0.00072 0.03403 C87 1 0.451434 0.094787 0.341830 11.00000 0.16403 0.07299 = 0.07063 0.03022 -0.01547 0.05229 AFIX 43 H87 2 0.421018 0.079137 0.364165 11.00000 -1.20000 AFIX 0 C88 1 0.513184 0.071972 0.327019 11.00000 0.18272 0.09004 = 0.08150 0.03285 -0.00845 0.08647 AFIX 43 H88 2 0.523777 0.038938 0.338176 11.00000 -1.20000 AFIX 0 C89 1 0.560767 0.096561 0.295769 11.00000 0.13107 0.08358 = 0.08387 0.01371 -0.01680 0.07154 AFIX 43 H89 2 0.604138 0.081831 0.285758 11.00000 -1.20000 AFIX 0 C90 1 0.540103 0.144575 0.280150 11.00000 0.09474 0.08424 = 0.05421 0.02845 0.00686 0.04733 AFIX 43 H90 2 0.571896 0.162627 0.259416 11.00000 -1.20000 AFIX 0 C91 1 0.191182 0.109380 -0.038366 11.00000 0.08602 0.05812 = 0.04706 0.01660 0.00458 0.02942 AFIX 43 H91 2 0.165120 0.082137 -0.020877 11.00000 -1.20000 AFIX 0 C92 1 0.191917 0.076576 -0.090800 11.00000 0.12738 0.06431 = 0.04743 0.00617 -0.00540 0.04734 AFIX 43 H92 2 0.171548 0.028182 -0.107476 11.00000 -1.20000 AFIX 0 C93 1 0.221816 0.114516 -0.117128 11.00000 0.15828 0.08061 = 0.03836 0.00376 0.00629 0.03552 AFIX 43 H93 2 0.221944 0.093645 -0.153227 11.00000 -1.20000 AFIX 0 C94 1 0.253303 0.186184 -0.090594 11.00000 0.14170 0.08592 = 0.03445 0.01975 0.01411 0.02511 AFIX 43 H94 2 0.273741 0.214497 -0.108649 11.00000 -1.20000 AFIX 0 C95 1 0.253756 0.214063 -0.038194 11.00000 0.09757 0.06546 = 0.03950 0.02009 -0.00172 0.02507 C96 1 0.293715 0.289530 -0.006560 11.00000 0.09685 0.05222 = 0.03883 0.01449 -0.00448 0.01321 C97 1 0.314070 0.336545 -0.035172 11.00000 0.16788 0.07906 = 0.04586 0.03478 0.00811 0.01800 AFIX 137 H97A 2 0.310311 0.380726 -0.014163 11.00000 -1.20000 H97B 2 0.276132 0.316374 -0.069084 11.00000 -1.20000 H97C 2 0.368995 0.343089 -0.040863 11.00000 -1.20000 AFIX 0 C98 1 0.362431 0.389996 0.127539 11.00000 0.06253 0.04125 = 0.04276 0.02254 0.00814 0.01793 C99 1 0.517974 0.572428 0.236411 11.00000 0.07867 0.03822 = 0.08214 0.02202 0.00078 -0.00794 AFIX 137 H99A 2 0.518408 0.556634 0.198936 11.00000 -1.20000 H99B 2 0.572759 0.587255 0.256785 11.00000 -1.20000 H99C 2 0.498079 0.610763 0.246344 11.00000 -1.20000 AFIX 0 C100 1 0.463570 0.514876 0.247453 11.00000 0.04458 0.03963 = 0.05178 0.01903 0.01621 0.01920 C101 1 0.463923 0.520681 0.302211 11.00000 0.03812 0.03751 = 0.05628 0.00674 -0.00074 0.01274 C102 1 0.513264 0.579849 0.344546 11.00000 0.04211 0.04322 = 0.05551 0.00309 -0.00065 0.00697 AFIX 43 H102 2 0.546663 0.617416 0.338672 11.00000 -1.20000 AFIX 0 C103 1 0.513032 0.583175 0.394473 11.00000 0.05013 0.04834 = 0.05952 -0.00835 -0.01098 0.01845 AFIX 43 H103 2 0.546439 0.623253 0.423420 11.00000 -1.20000 AFIX 0 C104 1 0.465126 0.529302 0.402988 11.00000 0.07063 0.06091 = 0.03746 -0.00127 -0.00314 0.02785 AFIX 43 H104 2 0.464800 0.530871 0.437501 11.00000 -1.20000 AFIX 0 C105 1 0.416024 0.471107 0.358735 11.00000 0.06498 0.05582 = 0.03705 0.01592 0.00303 0.02275 AFIX 43 H105 2 0.381700 0.433605 0.364247 11.00000 -1.20000 AFIX 0 C106 1 0.289775 0.001079 -0.013296 11.00000 0.05843 0.05258 = 0.05182 0.01603 0.01607 0.02377 AFIX 43 H106 2 0.241366 -0.006784 -0.000739 11.00000 -1.20000 AFIX 0 C107 1 0.285244 -0.035431 -0.064798 11.00000 0.08182 0.07485 = 0.05692 0.00723 0.01186 0.02580 AFIX 43 H107 2 0.235395 -0.067244 -0.087235 11.00000 -1.20000 AFIX 0 C108 1 0.355958 -0.024702 -0.083586 11.00000 0.14139 0.14831 = 0.05579 0.00707 0.05701 0.05386 AFIX 43 H108 2 0.355534 -0.049755 -0.119116 11.00000 -1.20000 AFIX 0 C109 1 0.429141 0.024644 -0.048483 11.00000 0.09600 0.14964 = 0.05667 -0.01098 0.02214 0.03272 AFIX 43 H109 2 0.478268 0.033381 -0.060163 11.00000 -1.20000 AFIX 0 C110 1 0.426567 0.059053 0.002516 11.00000 0.07472 0.06668 = 0.05291 0.01817 0.03404 0.02716 C111 1 0.500433 0.109469 0.039685 11.00000 0.05873 0.07581 = 0.06627 0.02237 0.03680 0.01858 C112 1 0.577191 0.124143 0.021632 11.00000 0.07357 0.10327 = 0.09102 0.01067 0.03981 0.02288 AFIX 137 H11A 2 0.570632 0.138158 -0.007724 11.00000 -1.20000 H11B 2 0.591886 0.083026 0.010175 11.00000 -1.20000 H11C 2 0.619775 0.160942 0.050515 11.00000 -1.20000 AFIX 0 C113 1 0.548340 0.210010 0.171041 11.00000 0.02812 0.05287 = 0.06126 0.02002 0.01307 0.01088 C114 1 0.729101 0.358639 0.296064 11.00000 0.04590 0.11239 = 0.09611 -0.01522 -0.01419 0.00590 AFIX 137 H11D 2 0.745577 0.320367 0.276540 11.00000 -1.20000 H11E 2 0.761211 0.381593 0.332047 11.00000 -1.20000 H11F 2 0.737688 0.391060 0.278943 11.00000 -1.20000 AFIX 0 C115 1 0.641621 0.332470 0.297074 11.00000 0.04518 0.05960 = 0.07076 0.01762 -0.00712 0.01600 C116 1 0.615123 0.360123 0.343692 11.00000 0.07865 0.05584 = 0.06626 0.01481 -0.01810 0.02210 C117 1 0.666528 0.411355 0.390587 11.00000 0.07387 0.09212 = 0.07964 0.02126 -0.03408 0.01814 AFIX 43 H117 2 0.722830 0.428804 0.392673 11.00000 -1.20000 AFIX 0 C118 1 0.633858 0.436554 0.434398 11.00000 0.14642 0.08193 = 0.06001 0.00909 -0.05308 0.03063 AFIX 43 H118 2 0.668251 0.470586 0.466380 11.00000 -1.20000 AFIX 0 C119 1 0.555669 0.412944 0.431020 11.00000 0.11575 0.08693 = 0.04573 0.00495 -0.00869 0.04163 AFIX 43 H119 2 0.533603 0.431096 0.460278 11.00000 -1.20000 AFIX 0 C120 1 0.505848 0.362305 0.385531 11.00000 0.10840 0.06268 = 0.04899 0.01579 -0.00720 0.03961 AFIX 43 H120 2 0.449838 0.344609 0.384262 11.00000 -1.20000 HKLF 4 REM _1 REM R1 = 0.0492 for 28920 Fo > 4sig(Fo) and 0.0663 for all 39537 data REM 1805 parameters refined using 8 restraints END WGHT 0.0765 0.0000 REM Highest difference peak 3.723, deepest hole -3.290, 1-sigma level 0.134 Q1 1 0.1133 0.8711 0.3375 11.00000 0.05 3.72 Q2 1 0.1161 0.7522 0.4071 11.00000 0.05 3.19 Q3 1 0.1619 0.8626 0.2951 11.00000 0.05 1.40 Q4 1 0.1583 0.7404 0.3621 11.00000 0.05 1.39 Q5 1 0.3232 0.3386 0.2556 11.00000 0.05 1.27 Q6 1 0.1980 0.8488 0.2902 11.00000 0.05 1.06 Q7 1 0.2382 0.2056 0.1107 11.00000 0.05 1.06 Q8 1 0.4198 0.1292 0.0883 11.00000 0.05 1.02 Q9 1 0.2012 0.7285 0.3602 11.00000 0.05 1.00 Q10 1 0.2430 0.1105 0.1582 11.00000 0.05 1.00 Q11 1 0.3985 0.3697 0.2111 11.00000 0.05 0.98 Q12 1 0.2691 0.3537 0.2521 11.00000 0.05 0.97 Q13 1 0.1861 0.6853 0.3786 11.00000 0.05 0.96 Q14 1 0.4403 0.3613 0.1856 11.00000 0.05 0.93 Q15 1 0.3656 0.1497 0.0952 11.00000 0.05 0.91 Q16 1 0.3033 0.1171 0.1434 11.00000 0.05 0.91 Q17 1 0.1563 0.9021 0.3180 11.00000 0.05 0.90 Q18 1 0.3643 0.2433 0.0470 11.00000 0.05 0.89 Q19 1 0.1789 0.3288 0.9583 11.00000 0.05 0.89 Q20 1 0.4975 0.2576 0.2326 11.00000 0.05 0.89 ; data_2 _database_code_depnum_ccdc_archive 'CCDC 856407' #TrackingRef 'Combined_CIF.cif' # start Validation Reply Form _vrf_CHEMW03_2 ; PROBLEM: The ratio of given/expected molecular weight as RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 25 H2O molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT414_2 ; PROBLEM: Short Intra D-H..H-X RESPONSE: H-atoms were introduced in calculated positions. Please see iucr_refine_instructions_details for full details. ; _vrf_PLAT043_2 ; PROBLEM: Check Reported Molecular Weight ................ 2463.82 RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 25 H2O molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_DIFMX01_2 ; PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 RESPONSE: Electron density synthesis with coefficients Fo-Fc Highest peak 7.68 at 0.8627 0.3089 0.9376 [ 1.48 A from N19 ] Deepest hole -3.91 at 0.2085 0.2665 0.5210 [ 0.60 A from DY7 ] ; _vrf_PLAT097_2 ; PROBLEM: Large Reported Max. (Positive) Residual Density 7.67 eA-3 RESPONSE: Electron density synthesis with coefficients Fo-Fc Highest peak 7.67 at 0.8627 0.3090 0.9375 [ 1.48 A from N2 ] Deepest hole -3.94 at 0.2085 0.2665 0.5211 [ 0.60 A from DY7 ] ; _vrf_DIFMX02_2 ; PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. RESPONSE: Electron density synthesis with coefficients Fo-Fc Highest peak 7.67 at 0.8627 0.3090 0.9375 [ 1.48 A from N2 ] Deepest hole -3.94 at 0.2085 0.2665 0.5211 [ 0.60 A from DY7 ] ; _vrf_PLAT041_2 ; PROBLEM: Calc. and Reported SumFormula Strings Differ ? RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 25 H2O molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT051_2 ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 1.10 Perc. RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 25 H2O molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT068_2 ; PROBLEM: Reported F000 Differs from Calcd (or Missing)... ? RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 25 H2O molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_FORMU01_2 ; PROBLEM: There is a discrepancy between the atom counts in the RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 25 H2O molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_CELLZ01_2 ; PROBLEM: Difference between formula and atom_site contents detected. RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 25 H2O molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT606_2 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. ; _vrf_PLAT869_2 ; PROBLEM: ALERTS Related to the use of SQUEEZE Suppressed RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H58 Dy4 N36 O5, 25(H2 O)' _chemical_formula_sum 'C60 H108 Dy4 N36 O30' _chemical_formula_weight 2463.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 19.806(9) _cell_length_b 20.037(9) _cell_length_c 27.326(15) _cell_angle_alpha 84.31(3) _cell_angle_beta 86.78(2) _cell_angle_gamma 71.967(18) _cell_volume 10257(9) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 27149 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 29.8 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4896 _exptl_absorpt_coefficient_mu 2.965 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_process_details 'Jacobson, Private Communication' _exptl_special_details ; For charge balance, the nominal formula is: [(L-H)2(L-2H)2Dy4(O)(N3)4](H2O)25 = 2(-1)+ 2(-2) + 4(+3) +(-2) + 4(-1) = (-2) + (-4) + (+12) + (-2) + (-4) = 0 ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 40060 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0948 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.50 _reflns_number_total 40060 _reflns_number_gt 24602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_structure_solution 'SHELXS-97: Acta Cryst.2008, A64, 112-122' _computing_structure_refinement 'SHELXL-97: Acta Cryst.2008, A64, 112-122' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 40060 _refine_ls_number_parameters 1907 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.1146 _refine_ls_wR_factor_ref 0.3419 _refine_ls_wR_factor_gt 0.3069 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.006 0.418 0.018 4097 1014 'Disordered lattice H2O' _platon_squeeze_details ; The Platon SQUEEZE procedure was applied to recover 1014 electrons per unit cell in one void (total volume 4097 ^A^3); that is 253.5 electrons per formula unit. Lattice solvent water molecules (18 electrons/H2O with V(liq) ~29.92^A^3/H2O) were present, and the electrons recovered by SQUEEZE have been assigned as 25 water molecules per formula unit. These water molecules have been included in the formula for the calculation of intensive properties. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13. ; 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 Dy1 Dy 0.22475(3) 0.76801(3) 0.067024(19) 0.05611(16) Uani 1 1 d . . . Dy2 Dy 0.19216(3) 0.82713(3) 0.19165(2) 0.05967(16) Uani 1 1 d . . . Dy3 Dy 0.41011(3) 0.76976(2) 0.068287(18) 0.05169(15) Uani 1 1 d . . . Dy4 Dy 0.37437(3) 0.83700(3) 0.190181(18) 0.05394(15) Uani 1 1 d . . . Dy5 Dy 0.58089(3) 0.75399(3) 0.492707(18) 0.05309(15) Uani 1 1 d . . . Dy6 Dy 0.57980(3) 0.73070(3) 0.628391(18) 0.05458(15) Uani 1 1 d . . . Dy7 Dy 0.76696(3) 0.75526(3) 0.48780(2) 0.06683(18) Uani 1 1 d . . . Dy8 Dy 0.76435(3) 0.73391(3) 0.62257(2) 0.05944(16) Uani 1 1 d . . . O1 O 0.1868(4) 0.7403(4) 0.1458(3) 0.0654(19) Uani 1 1 d . . . O2 O 0.4485(4) 0.7488(3) 0.1472(3) 0.0600(18) Uani 1 1 d . . . O3 O 0.3061(4) 0.8138(4) 0.0254(3) 0.0627(18) Uani 1 1 d . . . O4 O 0.2575(5) 0.8999(4) 0.1995(3) 0.068(2) Uani 1 1 d . . . O5 O 0.3011(4) 0.7972(4) 0.1291(3) 0.072(2) Uani 1 1 d . . . O6 O 0.5225(4) 0.8013(4) 0.5624(3) 0.0603(17) Uani 1 1 d . . . O7 O 0.7845(4) 0.8041(4) 0.5547(3) 0.0658(19) Uani 1 1 d . . . O8 O 0.6908(4) 0.7023(4) 0.4614(3) 0.0579(17) Uani 1 1 d . . . O9 O 0.6912(4) 0.6693(3) 0.6519(3) 0.0569(17) Uani 1 1 d . . . O10 O 0.6710(4) 0.7434(5) 0.5582(3) 0.079(2) Uani 1 1 d . . . N1 N 0.2419(6) 0.6954(6) -0.0061(4) 0.078(3) Uani 1 1 d . . . N2 N 0.2068(6) 0.6516(5) 0.0844(4) 0.072(3) Uani 1 1 d . . . N3 N 0.1955(6) 0.6263(6) 0.1316(4) 0.079(3) Uani 1 1 d . . . N4 N 0.1794(5) 0.6634(5) 0.2102(3) 0.063(2) Uani 1 1 d . . . H4 H 0.1779 0.6222 0.2239 0.076 Uiso 1 1 calc R . . N5 N 0.1731(6) 0.7201(5) 0.2370(3) 0.068(2) Uani 1 1 d . . . N6 N 0.1674(6) 0.8308(6) 0.2847(4) 0.082(3) Uani 1 1 d . . . N7 N 0.4593(5) 0.6952(5) -0.0009(4) 0.063(2) Uani 1 1 d . . . N8 N 0.4992(5) 0.6548(5) 0.0906(4) 0.066(2) Uani 1 1 d . . . N9 N 0.5176(6) 0.6371(5) 0.1409(4) 0.070(2) Uani 1 1 d . . . N10 N 0.4953(6) 0.6804(5) 0.2150(4) 0.072(3) Uani 1 1 d . . . H10 H 0.5228 0.6411 0.2297 0.087 Uiso 1 1 calc R . . N11 N 0.4575(6) 0.7364(5) 0.2419(4) 0.067(2) Uani 1 1 d . . . N12 N 0.3825(6) 0.8505(5) 0.2804(4) 0.072(3) Uani 1 1 d . . . N13 N 0.0955(5) 0.7997(5) 0.0427(4) 0.068(3) Uani 1 1 d . . . N14 N 0.1807(5) 0.8612(5) -0.0027(3) 0.057(2) Uani 1 1 d . . . N15 N 0.2307(5) 0.8901(4) -0.0260(3) 0.062(2) Uani 1 1 d . . . N16 N 0.3459(5) 0.8905(5) -0.0269(3) 0.059(2) Uani 1 1 d . . . N17 N 0.4092(5) 0.8601(4) -0.0019(3) 0.0534(19) Uani 1 1 d . . . N18 N 0.5260(5) 0.7986(5) 0.0467(4) 0.064(2) Uani 1 1 d . . . N19 N 0.0567(6) 0.8611(6) 0.1942(4) 0.077(3) Uani 1 1 d . . . N20 N 0.1245(6) 0.9563(6) 0.1962(4) 0.079(3) Uani 1 1 d . . . N21 N 0.1654(5) 1.0015(5) 0.1942(4) 0.071(3) Uani 1 1 d . . . N22 N 0.2780(5) 1.0086(4) 0.1899(3) 0.060(2) Uani 1 1 d . . . N23 N 0.3479(5) 0.9667(4) 0.1889(3) 0.056(2) Uani 1 1 d . . . N24 N 0.4753(5) 0.8862(5) 0.1893(3) 0.058(2) Uani 1 1 d . . . N25 N 0.1669(6) 0.8777(5) 0.1060(4) 0.074(3) Uani 1 1 d . . . N26 N 0.1199(5) 0.9279(5) 0.0914(4) 0.068(2) Uani 1 1 d . . . N27 N 0.0782(7) 0.9756(8) 0.0766(5) 0.114(5) Uani 1 1 d . . . N28 N 0.3866(5) 0.8806(4) 0.1022(3) 0.054(2) Uani 1 1 d . . . N29 N 0.4013(5) 0.9342(5) 0.0886(4) 0.068(2) Uani 1 1 d . . . N30 N 0.4163(8) 0.9836(6) 0.0725(4) 0.095(4) Uani 1 1 d . . . N31 N 0.3391(6) 0.6863(5) 0.0753(4) 0.080(3) Uani 1 1 d . . . N32 N 0.3633(5) 0.6221(5) 0.0701(3) 0.062(2) Uani 1 1 d . . . N33 N 0.3859(7) 0.5639(6) 0.0623(5) 0.093(4) Uani 1 1 d . . . N34 N 0.3069(5) 0.7595(4) 0.2294(3) 0.064(2) Uani 1 1 d . . . N35 N 0.3193(6) 0.7147(6) 0.2638(4) 0.077(3) Uani 1 1 d . . . N36 N 0.3288(7) 0.6736(6) 0.2966(5) 0.091(4) Uani 1 1 d . . . N37 N 0.5549(5) 0.8099(5) 0.4050(3) 0.061(2) Uani 1 1 d . . . N38 N 0.4874(5) 0.8760(4) 0.4824(3) 0.061(2) Uani 1 1 d . . . N39 N 0.4573(5) 0.9033(5) 0.5242(3) 0.066(2) Uani 1 1 d . . . H39 H 0.4241 0.9444 0.5241 0.080 Uiso 1 1 calc R . . N40 N 0.4566(5) 0.8923(4) 0.6083(3) 0.057(2) Uani 1 1 d . . . N41 N 0.4848(5) 0.8455(5) 0.6464(3) 0.062(2) Uani 1 1 d . . . N42 N 0.5512(6) 0.7531(5) 0.7185(3) 0.063(2) Uani 1 1 d . . . N43 N 0.7708(5) 0.8053(6) 0.3983(4) 0.077(3) Uani 1 1 d . . . N44 N 0.7813(6) 0.8774(5) 0.4727(4) 0.074(3) Uani 1 1 d . . . N45 N 0.7858(6) 0.9076(5) 0.5127(3) 0.074(3) Uani 1 1 d . . . N46 N 0.7865(5) 0.8966(5) 0.5990(4) 0.071(3) Uani 1 1 d . . . H46 H 0.7903 0.9386 0.6021 0.085 Uiso 1 1 calc R . . N47 N 0.7842(5) 0.8462(4) 0.6373(4) 0.064(2) Uani 1 1 d . . . N48 N 0.7701(5) 0.7550(4) 0.7115(4) 0.068(3) Uani 1 1 d . . . N49 N 0.4721(6) 0.7156(5) 0.4818(3) 0.067(3) Uani 1 1 d . . . N50 N 0.5958(5) 0.6452(5) 0.4484(3) 0.060(2) Uani 1 1 d . . . N51 N 0.6643(5) 0.6089(5) 0.4351(3) 0.065(2) Uani 1 1 d . . . N52 N 0.7794(5) 0.6067(5) 0.4333(4) 0.070(3) Uani 1 1 d . . . N53 N 0.8232(6) 0.6458(6) 0.4431(4) 0.072(3) Uani 1 1 d . . . N54 N 0.9001(7) 0.7178(7) 0.4710(5) 0.092(4) Uani 1 1 d . . . N55 N 0.4709(5) 0.6901(5) 0.6393(3) 0.064(2) Uani 1 1 d . . . N56 N 0.5991(5) 0.6076(5) 0.6662(3) 0.057(2) Uani 1 1 d . . . N57 N 0.6640(5) 0.5664(5) 0.6770(3) 0.065(2) Uani 1 1 d . . . N58 N 0.7795(5) 0.5707(5) 0.6768(4) 0.066(2) Uani 1 1 d . . . N59 N 0.8224(6) 0.6115(5) 0.6621(3) 0.065(2) Uani 1 1 d . . . N60 N 0.8977(6) 0.6983(6) 0.6322(5) 0.083(3) Uani 1 1 d . . . N61 N 0.5882(5) 0.6587(4) 0.5594(3) 0.064(2) Uani 1 1 d . . . N62 N 0.5722(6) 0.6055(5) 0.5577(3) 0.070(3) Uani 1 1 d . . . N63 N 0.5619(7) 0.5519(5) 0.5575(4) 0.083(3) Uani 1 1 d . . . N64 N 0.8115(5) 0.6592(5) 0.5541(3) 0.068(2) Uani 1 1 d . . . N65 N 0.8592(6) 0.6057(5) 0.5540(4) 0.074(3) Uani 1 1 d . . . N66 N 0.9047(6) 0.5541(6) 0.5519(4) 0.093(4) Uani 1 1 d . . . N67 N 0.6489(5) 0.8376(5) 0.4800(4) 0.075(3) Uani 1 1 d . . . N68 N 0.6309(6) 0.8979(4) 0.4604(4) 0.076(3) Uani 1 1 d . . . N69 N 0.6126(7) 0.9554(5) 0.4390(7) 0.120(6) Uani 1 1 d . . . N70 N 0.6499(5) 0.8096(4) 0.6401(3) 0.051(2) Uani 1 1 d . . . N71 N 0.6294(6) 0.8650(5) 0.6641(4) 0.073(3) Uani 1 1 d . . . N72 N 0.6146(6) 0.9129(5) 0.6891(4) 0.083(3) Uani 1 1 d . . . C1 C 0.2551(6) 0.7158(7) -0.0501(4) 0.067(3) Uani 1 1 d . . . H1 H 0.2532 0.7638 -0.0566 0.080 Uiso 1 1 calc R . . C2 C 0.2722(8) 0.6737(9) -0.0903(5) 0.091(4) Uani 1 1 d . . . H2 H 0.2898 0.6887 -0.1212 0.110 Uiso 1 1 calc R . . C3 C 0.2609(9) 0.6074(8) -0.0807(5) 0.096(5) Uani 1 1 d . . . H3 H 0.2649 0.5773 -0.1062 0.115 Uiso 1 1 calc R . . C4 C 0.2452(8) 0.5893(8) -0.0369(5) 0.087(4) Uani 1 1 d . . . H4A H 0.2391 0.5441 -0.0302 0.105 Uiso 1 1 calc R . . C5 C 0.2361(6) 0.6321(6) 0.0030(5) 0.069(3) Uani 1 1 d . . . C6 C 0.2185(6) 0.6045(7) 0.0518(5) 0.074(3) Uani 1 1 d . . . C7 C 0.2139(10) 0.5313(7) 0.0661(6) 0.102(5) Uani 1 1 d . . . H7A H 0.2272 0.5174 0.1004 0.153 Uiso 1 1 calc R . . H7B H 0.2464 0.4982 0.0448 0.153 Uiso 1 1 calc R . . H7C H 0.1652 0.5308 0.0621 0.153 Uiso 1 1 calc R . . C8 C 0.1881(7) 0.6765(7) 0.1612(5) 0.071(3) Uani 1 1 d . . . C9 C 0.1609(11) 0.6402(9) 0.3102(5) 0.122(7) Uani 1 1 d . . . H9A H 0.1238 0.6273 0.2946 0.183 Uiso 1 1 calc R . . H9B H 0.1485 0.6456 0.3451 0.183 Uiso 1 1 calc R . . H9C H 0.2064 0.6032 0.3069 0.183 Uiso 1 1 calc R . . C10 C 0.1671(8) 0.7101(7) 0.2848(4) 0.081(4) Uani 1 1 d . . . C11 C 0.1676(8) 0.7671(8) 0.3114(4) 0.082(4) Uani 1 1 d . . . C12 C 0.1696(12) 0.7611(11) 0.3608(6) 0.133(7) Uani 1 1 d . . . H12 H 0.1700 0.7185 0.3797 0.160 Uiso 1 1 calc R . . C13 C 0.1712(11) 0.8225(9) 0.3838(6) 0.113(6) Uani 1 1 d . . . H13 H 0.1735 0.8203 0.4185 0.136 Uiso 1 1 calc R . . C14 C 0.1694(10) 0.8825(9) 0.3565(5) 0.104(5) Uani 1 1 d . . . H14 H 0.1700 0.9226 0.3722 0.125 Uiso 1 1 calc R . . C15 C 0.1667(8) 0.8865(8) 0.3068(5) 0.082(4) Uani 1 1 d . . . H15 H 0.1642 0.9296 0.2879 0.098 Uiso 1 1 calc R . . C16 C 0.4392(5) 0.7147(6) -0.0470(5) 0.059(3) Uani 1 1 d . . . H16 H 0.4091 0.7611 -0.0555 0.071 Uiso 1 1 calc R . . C17 C 0.4620(7) 0.6678(7) -0.0829(4) 0.073(3) Uani 1 1 d . . . H17 H 0.4390 0.6785 -0.1136 0.087 Uiso 1 1 calc R . . C18 C 0.5131(8) 0.6106(9) -0.0761(6) 0.098(5) Uani 1 1 d . . . H18 H 0.5358 0.5848 -0.1029 0.117 Uiso 1 1 calc R . . C19 C 0.5344(9) 0.5872(8) -0.0282(5) 0.093(4) Uani 1 1 d . . . H19 H 0.5679 0.5420 -0.0215 0.111 Uiso 1 1 calc R . . C20 C 0.5063(6) 0.6308(6) 0.0108(4) 0.063(3) Uani 1 1 d . . . C21 C 0.5278(7) 0.6101(6) 0.0608(5) 0.070(3) Uani 1 1 d . . . C22 C 0.5775(9) 0.5342(6) 0.0767(7) 0.108(6) Uani 1 1 d . . . H22A H 0.6248 0.5279 0.0615 0.161 Uiso 1 1 calc R . . H22B H 0.5576 0.4992 0.0660 0.161 Uiso 1 1 calc R . . H22C H 0.5812 0.5282 0.1126 0.161 Uiso 1 1 calc R . . C23 C 0.4883(6) 0.6884(5) 0.1655(4) 0.060(3) Uani 1 1 d . . . C24 C 0.4998(8) 0.6683(6) 0.3173(5) 0.079(4) Uani 1 1 d . . . H24A H 0.5112 0.6268 0.2985 0.119 Uiso 1 1 calc R . . H24B H 0.4714 0.6611 0.3468 0.119 Uiso 1 1 calc R . . H24C H 0.5439 0.6752 0.3270 0.119 Uiso 1 1 calc R . . C25 C 0.4592(6) 0.7306(6) 0.2868(4) 0.058(2) Uani 1 1 d . . . C26 C 0.4134(7) 0.7916(7) 0.3108(5) 0.074(3) Uani 1 1 d . . . C27 C 0.4026(7) 0.7946(7) 0.3615(4) 0.073(3) Uani 1 1 d . . . H27 H 0.4271 0.7554 0.3830 0.088 Uiso 1 1 calc R . . C28 C 0.3582(7) 0.8518(7) 0.3805(4) 0.075(3) Uani 1 1 d . . . H28 H 0.3469 0.8505 0.4148 0.090 Uiso 1 1 calc R . . C29 C 0.3292(8) 0.9121(8) 0.3507(5) 0.082(4) Uani 1 1 d . . . H29 H 0.3006 0.9546 0.3633 0.099 Uiso 1 1 calc R . . C30 C 0.3443(6) 0.9071(6) 0.3019(5) 0.070(3) Uani 1 1 d . . . H30 H 0.3254 0.9487 0.2808 0.084 Uiso 1 1 calc R . . C31 C 0.0475(5) 0.7637(5) 0.0680(4) 0.059(3) Uani 1 1 d . . . H31 H 0.0677 0.7234 0.0900 0.071 Uiso 1 1 calc R . . C32 C -0.0242(7) 0.7841(9) 0.0621(6) 0.097(5) Uani 1 1 d . . . H32 H -0.0545 0.7615 0.0801 0.116 Uiso 1 1 calc R . . C33 C -0.0485(9) 0.8400(9) 0.0279(6) 0.106(5) Uani 1 1 d . . . H33 H -0.0982 0.8607 0.0242 0.128 Uiso 1 1 calc R . . C34 C 0.0005(8) 0.8687(9) -0.0030(6) 0.100(5) Uani 1 1 d . . . H34 H -0.0160 0.8999 -0.0313 0.120 Uiso 1 1 calc R . . C35 C 0.0725(6) 0.8495(6) 0.0098(5) 0.067(3) Uani 1 1 d . . . C36 C 0.1183(7) 0.8849(6) -0.0173(4) 0.069(3) Uani 1 1 d . . . C37 C 0.0892(8) 0.9455(8) -0.0549(5) 0.099(5) Uani 1 1 d . . . H37A H 0.1217 0.9739 -0.0597 0.149 Uiso 1 1 calc R . . H37B H 0.0426 0.9746 -0.0435 0.149 Uiso 1 1 calc R . . H37C H 0.0842 0.9274 -0.0861 0.149 Uiso 1 1 calc R . . C38 C 0.2958(6) 0.8659(6) -0.0095(4) 0.066(3) Uani 1 1 d . . . C39 C 0.4563(9) 0.9423(8) -0.0539(6) 0.100(5) Uani 1 1 d . . . H39A H 0.4068 0.9703 -0.0594 0.150 Uiso 1 1 calc R . . H39B H 0.4785 0.9240 -0.0848 0.150 Uiso 1 1 calc R . . H39C H 0.4821 0.9719 -0.0421 0.150 Uiso 1 1 calc R . . C40 C 0.4588(6) 0.8818(6) -0.0161(4) 0.063(3) Uani 1 1 d . . . C41 C 0.5240(6) 0.8518(5) 0.0136(4) 0.057(2) Uani 1 1 d . . . C42 C 0.5821(7) 0.8732(6) 0.0021(6) 0.085(4) Uani 1 1 d . . . H42 H 0.5819 0.9071 -0.0249 0.102 Uiso 1 1 calc R . . C43 C 0.6471(7) 0.8420(8) 0.0331(5) 0.087(4) Uani 1 1 d . . . H43 H 0.6870 0.8588 0.0268 0.105 Uiso 1 1 calc R . . C44 C 0.6494(8) 0.7898(8) 0.0703(5) 0.085(4) Uani 1 1 d . . . H44 H 0.6883 0.7696 0.0915 0.102 Uiso 1 1 calc R . . C45 C 0.5895(4) 0.7708(5) 0.0728(4) 0.047(2) Uani 1 1 d . . . H45 H 0.5903 0.7321 0.0962 0.056 Uiso 1 1 calc R . . C46 C 0.0167(6) 0.8168(6) 0.1931(5) 0.064(3) Uani 1 1 d . . . H46A H 0.0406 0.7678 0.1929 0.077 Uiso 1 1 calc R . . C47 C -0.0555(7) 0.8390(11) 0.1923(6) 0.092(5) Uani 1 1 d . . . H47 H -0.0784 0.8038 0.1921 0.110 Uiso 1 1 calc R . . C48 C -0.0899(9) 0.8940(12) 0.1920(6) 0.106(6) Uani 1 1 d . . . H48 H -0.1402 0.9055 0.1915 0.128 Uiso 1 1 calc R . . C49 C -0.0547(8) 0.9495(11) 0.1922(6) 0.106(5) Uani 1 1 d . . . H49 H -0.0820 0.9978 0.1890 0.127 Uiso 1 1 calc R . . C50 C 0.0201(8) 0.9300(7) 0.1974(5) 0.079(3) Uani 1 1 d . . . C51 C 0.0577(7) 0.9788(8) 0.1971(5) 0.081(4) Uani 1 1 d . . . C52 C 0.0216(10) 1.0592(8) 0.1960(10) 0.174(11) Uani 1 1 d . . . H52A H 0.0174 1.0798 0.1618 0.261 Uiso 1 1 calc R . . H52B H 0.0504 1.0802 0.2139 0.261 Uiso 1 1 calc R . . H52C H -0.0258 1.0687 0.2117 0.261 Uiso 1 1 calc R . . C53 C 0.2365(6) 0.9707(5) 0.1942(4) 0.055(2) Uani 1 1 d . . . C54 C 0.3764(8) 1.0794(6) 0.1784(5) 0.081(4) Uani 1 1 d . . . H54A H 0.3245 1.0994 0.1804 0.121 Uiso 1 1 calc R . . H54B H 0.3939 1.0941 0.1461 0.121 Uiso 1 1 calc R . . H54C H 0.3976 1.0963 0.2043 0.121 Uiso 1 1 calc R . . C55 C 0.3976(8) 0.9958(7) 0.1853(4) 0.071(3) Uani 1 1 d . . . C56 C 0.4716(7) 0.9507(7) 0.1850(4) 0.072(3) Uani 1 1 d . . . C57 C 0.5259(8) 0.9805(8) 0.1832(4) 0.082(4) Uani 1 1 d . . . H57 H 0.5149 1.0303 0.1816 0.099 Uiso 1 1 calc R . . C58 C 0.5943(7) 0.9400(8) 0.1835(4) 0.073(3) Uani 1 1 d . . . H58 H 0.6325 0.9592 0.1839 0.088 Uiso 1 1 calc R . . C59 C 0.6049(8) 0.8691(9) 0.1832(5) 0.088(4) Uani 1 1 d . . . H59 H 0.6521 0.8395 0.1784 0.105 Uiso 1 1 calc R . . C60 C 0.5545(5) 0.8397(5) 0.1891(4) 0.047(2) Uani 1 1 d . . . H60 H 0.5660 0.7899 0.1933 0.057 Uiso 1 1 calc R . . C61 C 0.5873(5) 0.7786(5) 0.3656(4) 0.051(2) Uani 1 1 d . . . H61 H 0.6138 0.7302 0.3709 0.061 Uiso 1 1 calc R . . C62 C 0.5869(6) 0.8072(7) 0.3202(5) 0.073(3) Uani 1 1 d . . . H62 H 0.6160 0.7823 0.2950 0.087 Uiso 1 1 calc R . . C63 C 0.5408(7) 0.8772(6) 0.3103(5) 0.073(3) Uani 1 1 d . . . H63 H 0.5361 0.8992 0.2777 0.087 Uiso 1 1 calc R . . C64 C 0.5037(7) 0.9118(7) 0.3484(4) 0.070(3) Uani 1 1 d . . . H64 H 0.4732 0.9588 0.3429 0.084 Uiso 1 1 calc R . . C65 C 0.5108(6) 0.8773(5) 0.3967(3) 0.059(3) Uani 1 1 d . . . C66 C 0.4744(6) 0.9110(6) 0.4398(4) 0.065(3) Uani 1 1 d . . . C67 C 0.4245(6) 0.9862(6) 0.4357(5) 0.076(3) Uani 1 1 d . . . H67A H 0.3759 0.9856 0.4313 0.113 Uiso 1 1 calc R . . H67B H 0.4393 1.0129 0.4074 0.113 Uiso 1 1 calc R . . H67C H 0.4261 1.0085 0.4658 0.113 Uiso 1 1 calc R . . C68 C 0.4817(6) 0.8626(5) 0.5674(4) 0.059(2) Uani 1 1 d . . . C69 C 0.4216(6) 0.9361(7) 0.7002(5) 0.075(3) Uani 1 1 d . . . H69A H 0.4019 0.9608 0.6690 0.112 Uiso 1 1 calc R . . H69B H 0.4488 0.9626 0.7143 0.112 Uiso 1 1 calc R . . H69C H 0.3829 0.9323 0.7231 0.112 Uiso 1 1 calc R . . C70 C 0.4706(7) 0.8623(7) 0.6912(4) 0.070(3) Uani 1 1 d . . . C71 C 0.5042(7) 0.8133(6) 0.7300(4) 0.063(3) Uani 1 1 d . . . C72 C 0.4876(9) 0.8305(7) 0.7800(5) 0.083(4) Uani 1 1 d . . . H72 H 0.4546 0.8738 0.7883 0.100 Uiso 1 1 calc R . . C73 C 0.5238(9) 0.7783(7) 0.8154(4) 0.084(4) Uani 1 1 d . . . H73 H 0.5140 0.7856 0.8492 0.101 Uiso 1 1 calc R . . C74 C 0.5709(9) 0.7197(8) 0.8035(5) 0.092(4) Uani 1 1 d . . . H74 H 0.5985 0.6871 0.8278 0.111 Uiso 1 1 calc R . . C75 C 0.5792(8) 0.7065(9) 0.7535(5) 0.086(4) Uani 1 1 d . . . H75 H 0.6069 0.6609 0.7452 0.103 Uiso 1 1 calc R . . C76 C 0.7695(6) 0.7714(6) 0.3616(4) 0.063(3) Uani 1 1 d . . . H76 H 0.7741 0.7227 0.3678 0.075 Uiso 1 1 calc R . . C77 C 0.7619(10) 0.7996(10) 0.3141(8) 0.115(6) Uani 1 1 d . . . H77 H 0.7550 0.7735 0.2887 0.138 Uiso 1 1 calc R . . C78 C 0.7646(10) 0.8659(10) 0.3047(8) 0.120(6) Uani 1 1 d . . . H78 H 0.7633 0.8861 0.2717 0.144 Uiso 1 1 calc R . . C79 C 0.7689(9) 0.9035(9) 0.3413(6) 0.094(4) Uani 1 1 d . . . H79 H 0.7671 0.9515 0.3350 0.113 Uiso 1 1 calc R . . C80 C 0.7762(8) 0.8714(8) 0.3885(5) 0.084(4) Uani 1 1 d . . . C81 C 0.7798(9) 0.9118(8) 0.4283(5) 0.090(4) Uani 1 1 d . . . C82 C 0.7761(14) 0.9886(10) 0.4241(5) 0.156(11) Uani 1 1 d . . . H82A H 0.7387 1.0140 0.4465 0.234 Uiso 1 1 calc R . . H82B H 0.7652 1.0087 0.3902 0.234 Uiso 1 1 calc R . . H82C H 0.8218 0.9928 0.4327 0.234 Uiso 1 1 calc R . . C83 C 0.7818(7) 0.8703(7) 0.5570(5) 0.076(4) Uani 1 1 d . . . C84 C 0.8153(8) 0.9254(6) 0.6909(6) 0.084(4) Uani 1 1 d . . . H84A H 0.8165 0.9557 0.6606 0.126 Uiso 1 1 calc R . . H84B H 0.8625 0.9091 0.7052 0.126 Uiso 1 1 calc R . . H84C H 0.7808 0.9521 0.7144 0.126 Uiso 1 1 calc R . . C85 C 0.7939(8) 0.8621(6) 0.6791(6) 0.083(4) Uani 1 1 d . . . C86 C 0.7858(6) 0.8130(6) 0.7221(4) 0.068(3) Uani 1 1 d . . . C87 C 0.7952(9) 0.8221(7) 0.7703(5) 0.088(4) Uani 1 1 d . . . H87 H 0.8098 0.8608 0.7775 0.106 Uiso 1 1 calc R . . C88 C 0.7831(10) 0.7735(8) 0.8100(6) 0.102(5) Uani 1 1 d . . . H88 H 0.7870 0.7808 0.8435 0.122 Uiso 1 1 calc R . . C89 C 0.7660(7) 0.7169(7) 0.7975(5) 0.081(4) Uani 1 1 d . . . H89 H 0.7549 0.6847 0.8221 0.097 Uiso 1 1 calc R . . C90 C 0.7651(6) 0.7075(6) 0.7488(5) 0.063(3) Uani 1 1 d . . . H90 H 0.7605 0.6641 0.7406 0.076 Uiso 1 1 calc R . . C91 C 0.4004(5) 0.7535(5) 0.4966(4) 0.049(2) Uani 1 1 d . . . H91 H 0.3938 0.7964 0.5110 0.059 Uiso 1 1 calc R . . C92 C 0.3439(7) 0.7347(8) 0.4923(5) 0.076(3) Uani 1 1 d . . . H92 H 0.2977 0.7633 0.5011 0.091 Uiso 1 1 calc R . . C93 C 0.3556(8) 0.6732(9) 0.4748(7) 0.100(5) Uani 1 1 d . . . H93 H 0.3161 0.6560 0.4738 0.120 Uiso 1 1 calc R . . C94 C 0.4155(8) 0.6344(7) 0.4589(6) 0.085(4) Uani 1 1 d . . . H94 H 0.4179 0.5920 0.4451 0.102 Uiso 1 1 calc R . . C95 C 0.4788(7) 0.6536(6) 0.4615(4) 0.068(3) Uani 1 1 d . . . C96 C 0.5488(7) 0.6157(6) 0.4466(4) 0.061(3) Uani 1 1 d . . . C97 C 0.5632(9) 0.5402(7) 0.4298(5) 0.095(5) Uani 1 1 d . . . H97A H 0.5987 0.5328 0.4027 0.142 Uiso 1 1 calc R . . H97B H 0.5190 0.5352 0.4186 0.142 Uiso 1 1 calc R . . H97C H 0.5811 0.5051 0.4574 0.142 Uiso 1 1 calc R . . C98 C 0.7138(7) 0.6367(6) 0.4433(4) 0.064(3) Uani 1 1 d . . . C99 C 0.9228(7) 0.5415(9) 0.4251(7) 0.107(5) Uani 1 1 d . . . H99A H 0.8846 0.5206 0.4223 0.160 Uiso 1 1 calc R . . H99B H 0.9569 0.5122 0.4491 0.160 Uiso 1 1 calc R . . H99C H 0.9470 0.5441 0.3930 0.160 Uiso 1 1 calc R . . C100 C 0.8919(6) 0.6143(8) 0.4418(5) 0.082(4) Uani 1 1 d . . . C101 C 0.9338(7) 0.6550(9) 0.4552(5) 0.084(4) Uani 1 1 d . . . C102 C 1.0064(8) 0.6321(10) 0.4487(7) 0.111(6) Uani 1 1 d . . . H102 H 1.0302 0.5893 0.4345 0.133 Uiso 1 1 calc R . . C103 C 1.0446(9) 0.6762(9) 0.4647(7) 0.104(5) Uani 1 1 d . . . H103 H 1.0951 0.6598 0.4629 0.125 Uiso 1 1 calc R . . C104 C 1.0151(8) 0.7349(9) 0.4808(6) 0.091(4) Uani 1 1 d . . . H104 H 1.0419 0.7635 0.4899 0.109 Uiso 1 1 calc R . . C105 C 0.9465(6) 0.7549(6) 0.4845(4) 0.056(2) Uani 1 1 d . . . H105 H 0.9246 0.7990 0.4974 0.067 Uiso 1 1 calc R . . C106 C 0.4015(5) 0.7292(5) 0.6294(4) 0.048(2) Uani 1 1 d . . . H106 H 0.3933 0.7782 0.6213 0.057 Uiso 1 1 calc R . . C107 C 0.3455(8) 0.7075(10) 0.6296(5) 0.093(4) Uani 1 1 d . . . H107 H 0.3004 0.7381 0.6196 0.112 Uiso 1 1 calc R . . C108 C 0.3558(9) 0.6377(8) 0.6453(5) 0.088(4) Uani 1 1 d . . . H108 H 0.3180 0.6178 0.6459 0.105 Uiso 1 1 calc R . . C109 C 0.4190(8) 0.5996(7) 0.6594(5) 0.074(3) Uani 1 1 d . . . H109 H 0.4245 0.5523 0.6717 0.089 Uiso 1 1 calc R . . C110 C 0.4794(8) 0.6222(8) 0.6580(4) 0.075(3) Uani 1 1 d . . . C111 C 0.5500(7) 0.5786(6) 0.6688(5) 0.068(3) Uani 1 1 d . . . C112 C 0.5623(8) 0.5015(6) 0.6832(5) 0.078(3) Uani 1 1 d . . . H11A H 0.5590 0.4777 0.6542 0.117 Uiso 1 1 calc R . . H11B H 0.5263 0.4956 0.7080 0.117 Uiso 1 1 calc R . . H11C H 0.6097 0.4807 0.6970 0.117 Uiso 1 1 calc R . . C113 C 0.7138(7) 0.6033(5) 0.6674(4) 0.065(3) Uani 1 1 d . . . C114 C 0.9219(8) 0.5090(6) 0.6828(6) 0.092(4) Uani 1 1 d . . . H11D H 0.9030 0.4979 0.7155 0.138 Uiso 1 1 calc R . . H11E H 0.9737 0.4976 0.6840 0.138 Uiso 1 1 calc R . . H11F H 0.9100 0.4811 0.6591 0.138 Uiso 1 1 calc R . . C115 C 0.8893(8) 0.5876(7) 0.6672(5) 0.075(3) Uani 1 1 d . . . C116 C 0.9299(6) 0.6305(7) 0.6519(6) 0.085(4) Uani 1 1 d . . . C117 C 1.0043(7) 0.6118(8) 0.6549(6) 0.095(5) Uani 1 1 d . . . H117 H 1.0295 0.5667 0.6698 0.114 Uiso 1 1 calc R . . C118 C 1.0412(9) 0.6570(10) 0.6369(8) 0.112(6) Uani 1 1 d . . . H118 H 1.0916 0.6411 0.6385 0.135 Uiso 1 1 calc R . . C119 C 1.0113(7) 0.7193(7) 0.6181(6) 0.082(4) Uani 1 1 d . . . H119 H 1.0376 0.7500 0.6057 0.099 Uiso 1 1 calc R . . C120 C 0.9448(5) 0.7375(5) 0.6171(4) 0.054(2) Uani 1 1 d . . . H120 H 0.9227 0.7846 0.6042 0.065 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 Dy1 0.0667(3) 0.0497(3) 0.0459(3) 0.0063(2) -0.0033(2) -0.0120(2) Dy2 0.0704(3) 0.0569(3) 0.0487(3) 0.0041(2) -0.0032(2) -0.0175(2) Dy3 0.0660(3) 0.0418(3) 0.0416(3) 0.00337(19) -0.0012(2) -0.0105(2) Dy4 0.0690(3) 0.0480(3) 0.0407(3) 0.0070(2) -0.0041(2) -0.0149(2) Dy5 0.0680(3) 0.0478(3) 0.0403(3) 0.0002(2) -0.0012(2) -0.0144(2) Dy6 0.0739(3) 0.0494(3) 0.0396(3) 0.0013(2) -0.0024(2) -0.0190(2) Dy7 0.0750(4) 0.0658(3) 0.0572(4) 0.0004(3) -0.0030(3) -0.0194(3) Dy8 0.0726(3) 0.0512(3) 0.0517(3) 0.0043(2) 0.0022(2) -0.0183(2) O1 0.070(4) 0.057(4) 0.071(5) 0.017(4) 0.002(4) -0.029(4) O2 0.075(5) 0.040(3) 0.051(4) 0.003(3) -0.011(3) 0.002(3) O3 0.078(5) 0.047(4) 0.055(5) 0.017(3) -0.003(4) -0.013(3) O4 0.098(6) 0.068(5) 0.050(5) 0.003(3) -0.010(4) -0.043(4) O5 0.077(5) 0.070(5) 0.069(6) -0.013(4) 0.002(4) -0.021(4) O6 0.073(4) 0.052(4) 0.048(4) -0.010(3) 0.011(3) -0.008(3) O7 0.086(5) 0.067(5) 0.054(5) -0.003(3) 0.004(4) -0.039(4) O8 0.078(5) 0.049(4) 0.047(4) 0.006(3) -0.003(3) -0.022(3) O9 0.066(4) 0.046(3) 0.056(4) 0.015(3) 0.001(3) -0.019(3) O10 0.071(5) 0.110(7) 0.048(5) 0.008(4) -0.012(4) -0.021(5) N1 0.092(7) 0.070(6) 0.055(6) 0.013(5) -0.020(5) -0.003(5) N2 0.080(6) 0.073(6) 0.067(7) 0.013(5) -0.021(5) -0.032(5) N3 0.116(9) 0.079(7) 0.058(6) 0.007(5) -0.008(6) -0.055(6) N4 0.077(6) 0.054(5) 0.055(6) 0.011(4) -0.010(4) -0.018(4) N5 0.096(7) 0.061(5) 0.049(6) 0.009(4) -0.007(5) -0.030(5) N6 0.108(8) 0.071(6) 0.054(6) -0.005(5) 0.018(5) -0.013(6) N7 0.077(6) 0.056(5) 0.055(6) -0.005(4) 0.010(4) -0.020(4) N8 0.068(6) 0.057(5) 0.064(6) -0.012(4) 0.017(4) -0.007(4) N9 0.091(7) 0.060(6) 0.056(6) 0.008(4) -0.001(5) -0.022(5) N10 0.096(7) 0.053(5) 0.062(6) 0.012(4) -0.035(5) -0.013(5) N11 0.096(7) 0.055(5) 0.048(6) 0.005(4) -0.003(5) -0.022(5) N12 0.096(7) 0.070(6) 0.045(6) 0.006(4) -0.007(5) -0.020(5) N13 0.067(5) 0.055(5) 0.074(7) 0.015(4) -0.027(5) -0.007(4) N14 0.071(6) 0.056(5) 0.044(5) -0.001(4) -0.010(4) -0.019(4) N15 0.084(6) 0.055(5) 0.038(5) 0.017(4) 0.001(4) -0.014(4) N16 0.074(6) 0.059(5) 0.043(5) 0.008(4) -0.004(4) -0.022(4) N17 0.063(5) 0.051(4) 0.038(4) 0.005(3) 0.000(4) -0.009(4) N18 0.065(5) 0.062(5) 0.059(6) -0.009(4) 0.006(4) -0.012(4) N19 0.093(7) 0.098(8) 0.047(6) 0.006(5) -0.011(5) -0.042(6) N20 0.085(7) 0.071(6) 0.066(7) 0.004(5) -0.003(5) -0.004(6) N21 0.077(6) 0.069(6) 0.066(6) -0.003(5) -0.017(5) -0.017(5) N22 0.089(6) 0.047(4) 0.047(5) 0.000(4) 0.002(4) -0.028(5) N23 0.080(6) 0.044(4) 0.039(5) 0.001(3) -0.013(4) -0.012(4) N24 0.104(7) 0.058(5) 0.023(4) 0.003(3) -0.015(4) -0.038(5) N25 0.093(7) 0.074(6) 0.046(6) 0.001(4) -0.004(5) -0.014(5) N26 0.061(5) 0.073(6) 0.054(6) 0.005(4) -0.011(4) 0.003(5) N27 0.099(9) 0.123(11) 0.088(10) -0.011(8) -0.019(7) 0.016(8) N28 0.077(6) 0.040(4) 0.048(5) -0.005(3) -0.004(4) -0.021(4) N29 0.077(6) 0.056(5) 0.064(6) -0.009(5) 0.003(5) -0.009(5) N30 0.160(12) 0.071(7) 0.060(7) 0.011(5) 0.020(7) -0.053(7) N31 0.114(8) 0.055(5) 0.094(8) -0.040(5) 0.061(6) -0.058(6) N32 0.067(5) 0.053(5) 0.056(6) -0.005(4) -0.003(4) -0.005(4) N33 0.110(9) 0.062(7) 0.097(9) -0.004(6) 0.005(7) -0.016(6) N34 0.098(7) 0.047(4) 0.040(5) 0.021(4) -0.005(4) -0.020(4) N35 0.107(8) 0.076(7) 0.050(6) -0.002(5) 0.004(5) -0.033(6) N36 0.106(9) 0.076(7) 0.078(8) 0.032(6) -0.023(6) -0.017(6) N37 0.063(5) 0.068(5) 0.047(5) -0.007(4) -0.007(4) -0.011(4) N38 0.083(6) 0.048(4) 0.045(5) 0.003(4) 0.000(4) -0.014(4) N39 0.078(6) 0.062(5) 0.041(5) -0.001(4) 0.002(4) 0.003(4) N40 0.066(5) 0.055(5) 0.050(5) -0.012(4) 0.007(4) -0.016(4) N41 0.090(6) 0.063(5) 0.030(4) 0.008(4) 0.002(4) -0.023(5) N42 0.107(7) 0.069(6) 0.024(4) 0.004(4) -0.010(4) -0.042(5) N43 0.073(6) 0.097(8) 0.060(7) 0.007(6) 0.000(5) -0.030(6) N44 0.088(7) 0.064(6) 0.074(7) 0.014(5) -0.024(5) -0.034(5) N45 0.120(8) 0.071(6) 0.039(5) 0.007(4) -0.002(5) -0.044(6) N46 0.092(7) 0.044(5) 0.067(7) 0.020(4) -0.008(5) -0.013(4) N47 0.090(7) 0.045(4) 0.059(6) 0.006(4) -0.004(5) -0.026(4) N48 0.087(6) 0.042(4) 0.062(6) 0.000(4) -0.017(5) 0.001(4) N49 0.119(8) 0.078(6) 0.017(4) -0.009(4) 0.004(4) -0.049(6) N50 0.087(6) 0.059(5) 0.028(4) -0.002(3) 0.003(4) -0.018(5) N51 0.084(6) 0.074(6) 0.036(5) -0.004(4) -0.003(4) -0.021(5) N52 0.070(6) 0.066(6) 0.068(6) -0.025(5) 0.003(5) -0.008(5) N53 0.089(7) 0.077(6) 0.046(6) -0.004(5) -0.006(5) -0.017(6) N54 0.099(9) 0.095(9) 0.087(9) 0.016(7) -0.006(7) -0.043(7) N55 0.085(6) 0.070(6) 0.049(5) 0.025(4) -0.024(4) -0.044(5) N56 0.090(6) 0.055(5) 0.027(4) 0.008(3) -0.001(4) -0.026(5) N57 0.075(6) 0.063(5) 0.054(6) 0.006(4) -0.002(4) -0.018(5) N58 0.063(5) 0.069(6) 0.061(6) -0.002(4) 0.003(4) -0.017(5) N59 0.087(7) 0.063(5) 0.039(5) -0.002(4) 0.007(4) -0.018(5) N60 0.074(6) 0.064(6) 0.103(9) -0.003(6) 0.004(6) -0.011(5) N61 0.101(7) 0.030(4) 0.057(6) -0.001(3) -0.008(5) -0.014(4) N62 0.107(7) 0.055(5) 0.034(5) 0.013(4) 0.013(4) -0.012(5) N63 0.130(9) 0.056(6) 0.070(7) 0.010(5) -0.014(6) -0.040(6) N64 0.085(6) 0.069(6) 0.043(5) -0.012(4) 0.003(4) -0.012(5) N65 0.089(7) 0.062(6) 0.052(6) -0.004(4) -0.009(5) 0.007(5) N66 0.098(8) 0.094(8) 0.056(7) -0.002(6) -0.012(6) 0.015(7) N67 0.076(6) 0.071(6) 0.103(8) -0.057(6) 0.040(5) -0.049(5) N68 0.092(7) 0.033(4) 0.096(8) 0.001(4) 0.006(6) -0.012(4) N69 0.095(8) 0.039(5) 0.211(17) 0.016(7) 0.023(9) -0.010(5) N70 0.076(5) 0.043(4) 0.040(4) 0.016(3) -0.030(4) -0.027(4) N71 0.085(7) 0.063(6) 0.069(7) 0.015(5) -0.021(5) -0.022(5) N72 0.106(8) 0.054(5) 0.080(8) -0.024(5) -0.003(6) -0.006(5) C1 0.079(7) 0.072(7) 0.051(7) 0.017(5) -0.024(5) -0.029(6) C2 0.092(9) 0.125(13) 0.058(8) -0.019(8) -0.010(7) -0.031(9) C3 0.151(14) 0.077(9) 0.041(7) -0.023(6) -0.006(7) -0.001(9) C4 0.099(10) 0.090(9) 0.072(10) -0.013(7) -0.012(7) -0.024(8) C5 0.075(7) 0.064(7) 0.070(8) 0.008(6) -0.022(6) -0.023(6) C6 0.067(7) 0.070(7) 0.084(9) -0.006(7) -0.009(6) -0.018(6) C7 0.147(14) 0.078(9) 0.098(12) -0.025(8) -0.001(10) -0.054(10) C8 0.073(7) 0.079(8) 0.060(8) -0.009(6) 0.003(5) -0.025(6) C9 0.21(2) 0.116(12) 0.055(9) 0.007(8) 0.053(10) -0.091(13) C10 0.106(10) 0.088(9) 0.039(6) 0.012(6) 0.026(6) -0.026(7) C11 0.102(9) 0.091(9) 0.042(7) -0.012(6) 0.013(6) -0.017(7) C12 0.22(2) 0.117(14) 0.063(11) -0.018(10) 0.023(12) -0.048(14) C13 0.183(18) 0.103(12) 0.062(10) -0.008(8) 0.031(10) -0.060(12) C14 0.164(16) 0.101(11) 0.050(8) -0.019(8) 0.015(9) -0.045(11) C15 0.099(10) 0.082(8) 0.075(9) -0.026(7) 0.014(7) -0.039(7) C16 0.052(5) 0.053(6) 0.073(8) -0.005(5) 0.010(5) -0.018(4) C17 0.102(9) 0.072(7) 0.040(6) -0.013(5) 0.004(6) -0.020(7) C18 0.098(10) 0.100(11) 0.082(11) -0.031(9) 0.022(8) -0.009(9) C19 0.120(11) 0.091(10) 0.057(8) -0.005(7) 0.027(7) -0.023(8) C20 0.072(7) 0.063(6) 0.058(7) -0.018(5) 0.006(5) -0.024(5) C21 0.082(8) 0.054(6) 0.065(8) -0.001(5) 0.003(6) -0.011(5) C22 0.131(13) 0.045(6) 0.121(14) 0.005(7) -0.023(10) 0.010(7) C23 0.090(7) 0.046(5) 0.039(6) 0.021(4) -0.026(5) -0.018(5) C24 0.108(10) 0.059(7) 0.062(8) 0.014(5) -0.017(7) -0.016(6) C25 0.068(6) 0.067(6) 0.037(6) 0.013(4) -0.008(4) -0.023(5) C26 0.085(8) 0.077(8) 0.063(8) 0.018(6) -0.016(6) -0.034(7) C27 0.097(9) 0.080(8) 0.035(6) 0.025(5) -0.015(5) -0.023(7) C28 0.104(9) 0.088(9) 0.035(6) -0.002(6) -0.008(6) -0.030(7) C29 0.101(10) 0.100(10) 0.043(7) 0.020(6) -0.002(6) -0.035(8) C30 0.073(7) 0.061(7) 0.066(8) 0.009(6) 0.002(6) -0.013(5) C31 0.046(5) 0.053(5) 0.078(8) 0.038(5) -0.009(5) -0.026(4) C32 0.053(7) 0.138(13) 0.092(11) 0.037(9) -0.017(7) -0.032(8) C33 0.093(11) 0.111(12) 0.089(12) -0.002(9) -0.037(9) 0.010(9) C34 0.083(9) 0.124(13) 0.078(10) -0.005(9) -0.039(8) -0.004(9) C35 0.066(7) 0.062(6) 0.068(8) 0.006(5) -0.005(5) -0.015(5) C36 0.083(8) 0.064(7) 0.049(7) 0.014(5) -0.005(5) -0.012(6) C37 0.103(10) 0.113(11) 0.055(8) 0.018(7) -0.004(7) -0.001(9) C38 0.076(7) 0.057(6) 0.042(6) 0.006(5) 0.003(5) 0.010(5) C39 0.110(11) 0.109(11) 0.079(10) 0.042(8) -0.007(8) -0.045(9) C40 0.073(7) 0.056(6) 0.048(6) 0.006(5) 0.010(5) -0.008(5) C41 0.082(7) 0.047(5) 0.046(6) 0.000(4) 0.002(5) -0.026(5) C42 0.079(8) 0.056(6) 0.115(12) -0.005(7) 0.029(8) -0.020(6) C43 0.077(8) 0.102(10) 0.081(10) 0.008(8) 0.011(7) -0.033(8) C44 0.084(9) 0.106(10) 0.080(9) -0.001(8) 0.018(7) -0.057(8) C45 0.036(4) 0.054(5) 0.046(5) 0.015(4) -0.012(4) -0.011(4) C46 0.057(6) 0.074(7) 0.077(8) 0.010(6) -0.009(5) -0.048(6) C47 0.042(7) 0.136(14) 0.105(12) -0.009(10) -0.003(7) -0.039(8) C48 0.074(10) 0.162(18) 0.065(9) 0.009(10) 0.000(7) -0.015(11) C49 0.075(9) 0.146(15) 0.088(12) -0.023(10) -0.010(8) -0.015(10) C50 0.106(10) 0.080(9) 0.051(7) 0.003(6) 0.004(6) -0.034(8) C51 0.076(8) 0.086(9) 0.060(8) 0.001(6) -0.007(6) 0.005(7) C52 0.137(16) 0.072(10) 0.26(3) -0.041(14) -0.018(17) 0.061(11) C53 0.070(6) 0.050(5) 0.036(5) -0.001(4) -0.006(4) -0.007(5) C54 0.121(11) 0.063(7) 0.072(8) -0.015(6) 0.026(7) -0.050(7) C55 0.105(9) 0.087(8) 0.033(6) -0.010(5) 0.006(5) -0.044(8) C56 0.082(8) 0.089(9) 0.041(6) 0.011(5) -0.013(5) -0.024(7) C57 0.123(12) 0.102(10) 0.042(7) -0.010(6) -0.007(6) -0.061(9) C58 0.070(8) 0.101(10) 0.050(7) 0.008(6) -0.010(5) -0.031(7) C59 0.086(9) 0.131(13) 0.053(8) -0.006(8) 0.002(6) -0.046(9) C60 0.044(5) 0.035(4) 0.062(6) -0.013(4) -0.005(4) -0.007(4) C61 0.054(5) 0.050(5) 0.048(6) -0.007(4) -0.001(4) -0.012(4) C62 0.056(6) 0.083(8) 0.083(9) -0.002(7) -0.017(6) -0.026(6) C63 0.086(8) 0.054(6) 0.072(8) 0.016(5) -0.015(6) -0.019(6) C64 0.076(7) 0.082(8) 0.050(7) 0.012(6) -0.007(5) -0.026(6) C65 0.095(8) 0.056(6) 0.027(5) 0.007(4) -0.016(5) -0.024(5) C66 0.083(7) 0.058(6) 0.051(6) 0.014(5) 0.002(5) -0.026(5) C67 0.068(7) 0.059(6) 0.086(9) 0.004(6) 0.003(6) -0.003(5) C68 0.069(6) 0.052(6) 0.054(6) 0.013(5) -0.005(5) -0.020(5) C69 0.069(7) 0.085(8) 0.067(8) -0.015(6) 0.025(6) -0.020(6) C70 0.093(8) 0.073(7) 0.051(7) -0.020(6) 0.021(6) -0.035(6) C71 0.093(8) 0.073(7) 0.040(6) -0.008(5) -0.001(5) -0.048(6) C72 0.136(12) 0.076(8) 0.048(7) -0.006(6) 0.006(7) -0.050(8) C73 0.162(13) 0.080(8) 0.017(5) -0.007(5) 0.012(6) -0.048(9) C74 0.136(13) 0.094(10) 0.050(8) 0.005(7) 0.008(8) -0.044(10) C75 0.094(9) 0.110(11) 0.075(10) -0.007(8) 0.006(7) -0.062(9) C76 0.078(7) 0.056(6) 0.047(6) -0.005(5) -0.001(5) -0.011(5) C77 0.109(12) 0.114(13) 0.141(18) -0.023(12) -0.006(11) -0.058(11) C78 0.139(15) 0.118(14) 0.099(14) 0.034(11) 0.010(11) -0.051(12) C79 0.119(12) 0.092(10) 0.086(11) -0.005(8) -0.013(9) -0.051(9) C80 0.087(9) 0.098(10) 0.072(9) 0.003(7) 0.011(7) -0.041(8) C81 0.133(12) 0.095(10) 0.067(9) 0.015(7) -0.006(8) -0.080(10) C82 0.34(3) 0.172(18) 0.032(7) 0.031(9) -0.024(11) -0.19(2) C83 0.076(8) 0.077(8) 0.082(9) 0.018(7) 0.017(6) -0.045(6) C84 0.103(10) 0.056(6) 0.089(10) -0.020(6) -0.022(8) -0.011(6) C85 0.106(10) 0.048(6) 0.090(10) -0.014(6) 0.020(8) -0.017(6) C86 0.080(7) 0.059(6) 0.060(7) 0.005(5) -0.014(6) -0.013(5) C87 0.134(12) 0.058(7) 0.075(9) -0.016(6) -0.011(8) -0.028(7) C88 0.154(15) 0.096(10) 0.068(10) -0.008(8) -0.030(9) -0.051(10) C89 0.093(9) 0.085(9) 0.046(7) 0.004(6) 0.003(6) -0.005(7) C90 0.060(6) 0.047(5) 0.083(8) -0.005(5) -0.005(5) -0.017(5) C91 0.034(4) 0.050(5) 0.056(6) 0.000(4) 0.005(4) -0.004(4) C92 0.064(7) 0.102(10) 0.072(8) -0.005(7) 0.008(6) -0.043(7) C93 0.065(8) 0.116(12) 0.124(14) -0.042(11) 0.004(8) -0.027(8) C94 0.097(10) 0.067(7) 0.103(11) 0.005(7) -0.013(8) -0.044(7) C95 0.099(9) 0.060(6) 0.053(7) -0.003(5) -0.017(6) -0.034(6) C96 0.103(9) 0.058(6) 0.032(5) 0.011(4) -0.007(5) -0.041(6) C97 0.141(13) 0.068(8) 0.056(8) -0.014(6) -0.012(8) 0.000(8) C98 0.083(8) 0.051(6) 0.053(7) -0.004(5) 0.009(5) -0.014(5) C99 0.071(8) 0.115(12) 0.111(13) -0.035(10) -0.003(8) 0.014(8) C100 0.056(7) 0.091(9) 0.078(9) 0.014(7) 0.004(6) 0.002(6) C101 0.066(7) 0.111(11) 0.075(9) -0.022(8) -0.022(6) -0.021(7) C102 0.066(8) 0.125(13) 0.112(14) 0.036(10) 0.007(8) -0.001(9) C103 0.075(9) 0.100(12) 0.141(16) 0.013(11) -0.009(9) -0.036(9) C104 0.088(10) 0.100(11) 0.094(11) 0.009(9) -0.005(8) -0.046(9) C105 0.056(6) 0.053(5) 0.067(7) 0.002(5) -0.008(5) -0.029(5) C106 0.046(5) 0.051(5) 0.047(5) -0.005(4) -0.014(4) -0.012(4) C107 0.088(9) 0.134(14) 0.071(9) -0.015(9) 0.006(7) -0.052(10) C108 0.119(12) 0.094(10) 0.049(8) 0.008(6) -0.010(7) -0.034(9) C109 0.097(9) 0.072(7) 0.054(7) 0.004(6) 0.003(6) -0.028(7) C110 0.106(10) 0.101(9) 0.029(5) -0.014(5) 0.007(5) -0.045(8) C111 0.089(8) 0.048(6) 0.061(7) 0.004(5) -0.004(6) -0.015(6) C112 0.111(10) 0.068(7) 0.063(8) 0.014(6) 0.014(7) -0.047(7) C113 0.089(8) 0.049(5) 0.040(6) 0.004(4) -0.001(5) 0.002(5) C114 0.092(9) 0.057(7) 0.114(12) 0.018(7) -0.006(8) -0.012(6) C115 0.091(9) 0.068(7) 0.059(8) 0.011(6) 0.001(6) -0.018(7) C116 0.056(7) 0.075(8) 0.116(12) -0.011(8) 0.006(7) -0.010(6) C117 0.062(7) 0.104(10) 0.125(13) 0.058(9) -0.030(7) -0.051(7) C118 0.084(10) 0.112(13) 0.140(17) -0.020(12) -0.013(10) -0.023(10) C119 0.060(7) 0.078(8) 0.104(11) -0.002(7) 0.033(7) -0.023(6) C120 0.059(6) 0.048(5) 0.066(7) 0.014(4) -0.007(5) -0.036(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O3 2.288(7) . ? Dy1 O1 2.312(8) . ? Dy1 N31 2.356(12) . ? Dy1 N25 2.458(10) . ? Dy1 N2 2.463(10) . ? Dy1 N14 2.521(9) . ? Dy1 N1 2.534(11) . ? Dy1 N13 2.548(9) . ? Dy1 O5 2.558(8) . ? Dy2 O4 2.260(7) . ? Dy2 O1 2.273(8) . ? Dy2 N25 2.470(10) . ? Dy2 N34 2.479(9) . ? Dy2 N5 2.489(9) . ? Dy2 N20 2.531(11) . ? Dy2 N19 2.554(11) . ? Dy2 N6 2.567(11) . ? Dy2 O5 2.632(8) . ? Dy3 O2 2.282(7) . ? Dy3 O3 2.310(8) . ? Dy3 N28 2.393(8) . ? Dy3 N8 2.473(9) . ? Dy3 N31 2.485(8) . ? Dy3 N7 2.492(9) . ? Dy3 N17 2.500(8) . ? Dy3 N18 2.559(9) . ? Dy3 O5 2.602(8) . ? Dy4 O4 2.281(9) . ? Dy4 O2 2.297(7) . ? Dy4 N34 2.479(9) . ? Dy4 N23 2.483(8) . ? Dy4 N24 2.487(9) . ? Dy4 N28 2.500(9) . ? Dy4 N12 2.524(10) . ? Dy4 N11 2.532(10) . ? Dy4 O5 2.603(8) . ? Dy5 O8 2.261(8) . ? Dy5 O6 2.300(7) . ? Dy5 N67 2.442(8) . ? Dy5 N61 2.481(9) . ? Dy5 N50 2.529(9) . ? Dy5 N49 2.542(10) . ? Dy5 O10 2.546(8) . ? Dy5 N37 2.553(9) . ? Dy5 N38 2.571(9) . ? Dy6 O9 2.261(7) . ? Dy6 O6 2.296(8) . ? Dy6 N61 2.454(9) . ? Dy6 N70 2.458(7) . ? Dy6 N56 2.500(8) . ? Dy6 N55 2.523(9) . ? Dy6 N42 2.549(9) . ? Dy6 N41 2.553(10) . ? Dy6 O10 2.609(9) . ? Dy7 O7 2.249(7) . ? Dy7 O8 2.278(7) . ? Dy7 N67 2.416(11) . ? Dy7 N64 2.491(10) . ? Dy7 N53 2.531(10) . ? Dy7 N54 2.536(13) . ? Dy7 N44 2.542(10) . ? Dy7 N43 2.555(11) . ? Dy7 O10 2.674(9) . ? Dy8 O9 2.290(6) . ? Dy8 O7 2.308(8) . ? Dy8 N70 2.358(9) . ? Dy8 N64 2.471(9) . ? Dy8 N47 2.474(8) . ? Dy8 N48 2.522(10) . ? Dy8 N59 2.524(10) . ? Dy8 N60 2.536(11) . ? Dy8 O10 2.575(8) . ? O1 C8 1.299(14) . ? O2 C23 1.292(11) . ? O3 C38 1.317(13) . ? O4 C53 1.344(13) . ? O6 C68 1.261(12) . ? O7 C83 1.319(14) . ? O8 C98 1.384(13) . ? O9 C113 1.293(12) . ? N1 C1 1.272(16) . ? N1 C5 1.307(15) . ? N2 C6 1.320(16) . ? N2 N3 1.371(14) . ? N3 C8 1.322(16) . ? N4 C8 1.352(15) . ? N4 N5 1.383(13) . ? N4 H4 0.8800 . ? N5 C10 1.307(15) . ? N6 C15 1.316(16) . ? N6 C11 1.405(17) . ? N7 C16 1.328(15) . ? N7 C20 1.357(15) . ? N8 C21 1.251(14) . ? N8 N9 1.424(14) . ? N9 C23 1.252(15) . ? N10 C23 1.355(14) . ? N10 N11 1.394(14) . ? N10 H10 0.8800 . ? N11 C25 1.223(14) . ? N12 C30 1.326(16) . ? N12 C26 1.368(15) . ? N13 C35 1.266(14) . ? N13 C31 1.468(13) . ? N14 C36 1.252(15) . ? N14 N15 1.391(13) . ? N15 C38 1.317(15) . ? N16 C38 1.287(15) . ? N16 N17 1.398(12) . ? N17 C40 1.222(14) . ? N18 C41 1.320(13) . ? N18 C45 1.412(13) . ? N19 C50 1.353(17) . ? N19 C46 1.364(14) . ? N20 C51 1.258(17) . ? N20 N21 1.386(15) . ? N21 C53 1.351(14) . ? N22 C53 1.276(14) . ? N22 N23 1.379(13) . ? N23 C55 1.286(15) . ? N24 C56 1.264(15) . ? N24 C60 1.556(13) . ? N25 N26 1.192(13) . ? N26 N27 1.109(14) . ? N28 N29 1.217(12) . ? N29 N30 1.156(13) . ? N31 N32 1.245(12) . ? N32 N33 1.150(13) . ? N34 N35 1.212(13) . ? N35 N36 1.137(14) . ? N37 C61 1.331(13) . ? N37 C65 1.366(14) . ? N38 C66 1.292(14) . ? N38 N39 1.343(12) . ? N39 C68 1.387(13) . ? N39 H39 0.8800 . ? N40 C68 1.317(14) . ? N40 N41 1.350(12) . ? N41 C70 1.294(14) . ? N42 C75 1.287(17) . ? N42 C71 1.331(15) . ? N43 C76 1.273(15) . ? N43 C80 1.360(17) . ? N44 N45 1.322(14) . ? N44 C81 1.330(16) . ? N45 C83 1.369(15) . ? N46 C83 1.328(17) . ? N46 N47 1.391(12) . ? N46 H46 0.8800 . ? N47 C85 1.256(17) . ? N48 C90 1.346(15) . ? N48 C86 1.355(14) . ? N49 C95 1.376(14) . ? N49 C91 1.445(14) . ? N50 C96 1.251(14) . ? N50 N51 1.374(13) . ? N51 C98 1.308(15) . ? N52 C98 1.278(15) . ? N52 N53 1.387(15) . ? N53 C100 1.312(16) . ? N54 C101 1.330(18) . ? N54 C105 1.433(15) . ? N55 C110 1.369(16) . ? N55 C106 1.382(13) . ? N56 C111 1.274(15) . ? N56 N57 1.326(13) . ? N57 C113 1.406(16) . ? N58 C113 1.291(15) . ? N58 N59 1.372(13) . ? N59 C115 1.271(17) . ? N60 C116 1.378(17) . ? N60 C120 1.416(14) . ? N61 N62 1.207(13) . ? N62 N63 1.153(13) . ? N64 N65 1.190(13) . ? N65 N66 1.146(13) . ? N67 N68 1.226(14) . ? N68 N69 1.197(15) . ? N70 N71 1.290(14) . ? N71 N72 1.186(14) . ? C1 C2 1.414(19) . ? C1 H1 0.9500 . ? C2 C3 1.41(2) . ? C2 H2 0.9500 . ? C3 C4 1.26(2) . ? C3 H3 0.9500 . ? C4 C5 1.423(18) . ? C4 H4A 0.9500 . ? C5 C6 1.459(19) . ? C6 C7 1.509(19) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.537(18) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.414(19) . ? C11 C12 1.35(2) . ? C12 C13 1.44(2) . ? C12 H12 0.9500 . ? C13 C14 1.34(2) . ? C13 H13 0.9500 . ? C14 C15 1.36(2) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.385(16) . ? C16 H16 0.9500 . ? C17 C18 1.278(19) . ? C17 H17 0.9500 . ? C18 C19 1.39(2) . ? C18 H18 0.9500 . ? C19 C20 1.423(17) . ? C19 H19 0.9500 . ? C20 C21 1.439(17) . ? C21 C22 1.568(16) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 C25 1.466(15) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.466(18) . ? C26 C27 1.395(18) . ? C27 C28 1.341(18) . ? C27 H27 0.9500 . ? C28 C29 1.373(18) . ? C28 H28 0.9500 . ? C29 C30 1.356(18) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.365(15) . ? C31 H31 0.9500 . ? C32 C33 1.37(2) . ? C32 H32 0.9500 . ? C33 C34 1.46(2) . ? C33 H33 0.9500 . ? C34 C35 1.413(18) . ? C34 H34 0.9500 . ? C35 C36 1.444(17) . ? C36 C37 1.500(17) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C39 C40 1.502(16) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.492(16) . ? C41 C42 1.358(16) . ? C42 C43 1.51(2) . ? C42 H42 0.9500 . ? C43 C44 1.377(19) . ? C43 H43 0.9500 . ? C44 C45 1.349(15) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.361(17) . ? C46 H46A 0.9500 . ? C47 C48 1.10(2) . ? C47 H47 0.9500 . ? C48 C49 1.48(3) . ? C48 H48 0.9500 . ? C49 C50 1.42(2) . ? C49 H49 0.9500 . ? C50 C51 1.40(2) . ? C51 C52 1.546(19) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C54 C55 1.590(17) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.465(19) . ? C56 C57 1.379(18) . ? C57 C58 1.347(19) . ? C57 H57 0.9500 . ? C58 C59 1.37(2) . ? C58 H58 0.9500 . ? C59 C60 1.303(17) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.313(17) . ? C61 H61 0.9500 . ? C62 C63 1.426(17) . ? C62 H62 0.9500 . ? C63 C64 1.361(18) . ? C63 H63 0.9500 . ? C64 C65 1.420(15) . ? C64 H64 0.9500 . ? C65 C66 1.459(16) . ? C66 C67 1.523(16) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C69 C70 1.532(17) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.415(18) . ? C71 C72 1.436(16) . ? C72 C73 1.398(19) . ? C72 H72 0.9500 . ? C73 C74 1.31(2) . ? C73 H73 0.9500 . ? C74 C75 1.406(19) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.36(2) . ? C76 H76 0.9500 . ? C77 C78 1.35(2) . ? C77 H77 0.9500 . ? C78 C79 1.33(2) . ? C78 H78 0.9500 . ? C79 C80 1.38(2) . ? C79 H79 0.9500 . ? C80 C81 1.44(2) . ? C81 C82 1.51(2) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C84 C85 1.524(17) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C86 1.490(18) . ? C86 C87 1.377(17) . ? C87 C88 1.45(2) . ? C87 H87 0.9500 . ? C88 C89 1.359(19) . ? C88 H88 0.9500 . ? C89 C90 1.365(17) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C92 1.299(15) . ? C91 H91 0.9500 . ? C92 C93 1.317(19) . ? C92 H92 0.9500 . ? C93 C94 1.28(2) . ? C93 H93 0.9500 . ? C94 C95 1.430(18) . ? C94 H94 0.9500 . ? C95 C96 1.418(18) . ? C96 C97 1.563(16) . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C99 C100 1.50(2) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 C101 1.41(2) . ? C101 C102 1.376(19) . ? C102 C103 1.44(2) . ? C102 H102 0.9500 . ? C103 C104 1.25(2) . ? C103 H103 0.9500 . ? C104 C105 1.293(18) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C107 1.310(16) . ? C106 H106 0.9500 . ? C107 C108 1.38(2) . ? C107 H107 0.9500 . ? C108 C109 1.30(2) . ? C108 H108 0.9500 . ? C109 C110 1.402(18) . ? C109 H109 0.9500 . ? C110 C111 1.429(18) . ? C111 C112 1.504(15) . ? C112 H11A 0.9800 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? C114 C115 1.534(17) . ? C114 H11D 0.9800 . ? C114 H11E 0.9800 . ? C114 H11F 0.9800 . ? C115 C116 1.371(18) . ? C116 C117 1.408(17) . ? C117 C118 1.37(2) . ? C117 H117 0.9500 . ? C118 C119 1.27(2) . ? C118 H118 0.9500 . ? C119 C120 1.254(16) . ? C119 H119 0.9500 . ? C120 H120 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 O3 Dy1 O1 141.8(3) . . ? O3 Dy1 N31 70.5(3) . . ? O1 Dy1 N31 94.3(3) . . ? O3 Dy1 N25 92.6(3) . . ? O1 Dy1 N25 71.0(3) . . ? N31 Dy1 N25 131.4(3) . . ? O3 Dy1 N2 137.3(3) . . ? O1 Dy1 N2 62.9(3) . . ? N31 Dy1 N2 74.1(3) . . ? N25 Dy1 N2 129.1(4) . . ? O3 Dy1 N14 62.6(3) . . ? O1 Dy1 N14 137.4(3) . . ? N31 Dy1 N14 127.5(3) . . ? N25 Dy1 N14 74.3(3) . . ? N2 Dy1 N14 129.9(3) . . ? O3 Dy1 N1 83.7(3) . . ? O1 Dy1 N1 127.2(3) . . ? N31 Dy1 N1 75.0(3) . . ? N25 Dy1 N1 150.2(3) . . ? N2 Dy1 N1 64.5(4) . . ? N14 Dy1 N1 77.8(3) . . ? O3 Dy1 N13 123.6(3) . . ? O1 Dy1 N13 86.9(3) . . ? N31 Dy1 N13 150.8(3) . . ? N25 Dy1 N13 76.4(3) . . ? N2 Dy1 N13 80.6(3) . . ? N14 Dy1 N13 61.2(3) . . ? N1 Dy1 N13 81.1(3) . . ? O3 Dy1 O5 71.0(3) . . ? O1 Dy1 O5 70.8(3) . . ? N31 Dy1 O5 65.8(3) . . ? N25 Dy1 O5 65.7(3) . . ? N2 Dy1 O5 114.5(3) . . ? N14 Dy1 O5 115.6(3) . . ? N1 Dy1 O5 138.4(3) . . ? N13 Dy1 O5 140.4(3) . . ? O3 Dy1 Dy2 110.1(2) . . ? O1 Dy1 Dy2 36.37(19) . . ? N31 Dy1 Dy2 100.5(3) . . ? N25 Dy1 Dy2 41.9(2) . . ? N2 Dy1 Dy2 98.9(3) . . ? N14 Dy1 Dy2 116.3(2) . . ? N1 Dy1 Dy2 163.4(2) . . ? N13 Dy1 Dy2 97.7(2) . . ? O5 Dy1 Dy2 45.75(18) . . ? O3 Dy1 Dy3 36.94(18) . . ? O1 Dy1 Dy3 109.85(19) . . ? N31 Dy1 Dy3 41.75(19) . . ? N25 Dy1 Dy3 98.8(3) . . ? N2 Dy1 Dy3 115.7(2) . . ? N14 Dy1 Dy3 99.2(2) . . ? N1 Dy1 Dy3 95.8(3) . . ? N13 Dy1 Dy3 160.4(2) . . ? O5 Dy1 Dy3 44.91(18) . . ? Dy2 Dy1 Dy3 90.66(3) . . ? O4 Dy2 O1 141.1(3) . . ? O4 Dy2 N25 89.8(3) . . ? O1 Dy2 N25 71.4(3) . . ? O4 Dy2 N34 70.3(3) . . ? O1 Dy2 N34 95.4(3) . . ? N25 Dy2 N34 129.7(3) . . ? O4 Dy2 N5 137.7(3) . . ? O1 Dy2 N5 63.1(3) . . ? N25 Dy2 N5 131.0(3) . . ? N34 Dy2 N5 73.7(3) . . ? O4 Dy2 N20 63.4(4) . . ? O1 Dy2 N20 135.8(3) . . ? N25 Dy2 N20 73.6(4) . . ? N34 Dy2 N20 127.9(3) . . ? N5 Dy2 N20 130.7(4) . . ? O4 Dy2 N19 126.1(3) . . ? O1 Dy2 N19 84.8(3) . . ? N25 Dy2 N19 79.8(3) . . ? N34 Dy2 N19 149.0(3) . . ? N5 Dy2 N19 79.0(3) . . ? N20 Dy2 N19 63.0(4) . . ? O4 Dy2 N6 86.3(3) . . ? O1 Dy2 N6 126.0(3) . . ? N25 Dy2 N6 151.4(4) . . ? N34 Dy2 N6 75.2(3) . . ? N5 Dy2 N6 63.3(3) . . ? N20 Dy2 N6 79.3(4) . . ? N19 Dy2 N6 79.7(4) . . ? O4 Dy2 O5 71.1(3) . . ? O1 Dy2 O5 70.1(2) . . ? N25 Dy2 O5 64.4(3) . . ? N34 Dy2 O5 65.5(3) . . ? N5 Dy2 O5 112.7(3) . . ? N20 Dy2 O5 116.6(3) . . ? N19 Dy2 O5 140.9(3) . . ? N6 Dy2 O5 139.2(3) . . ? O4 Dy2 Dy4 36.2(2) . . ? O1 Dy2 Dy4 110.30(19) . . ? N25 Dy2 Dy4 95.9(3) . . ? N34 Dy2 Dy4 42.2(2) . . ? N5 Dy2 Dy4 115.7(2) . . ? N20 Dy2 Dy4 99.3(3) . . ? N19 Dy2 Dy4 162.3(3) . . ? N6 Dy2 Dy4 97.6(3) . . ? O5 Dy2 Dy4 45.12(17) . . ? O4 Dy2 Dy1 108.0(2) . . ? O1 Dy2 Dy1 37.11(18) . . ? N25 Dy2 Dy1 41.7(2) . . ? N34 Dy2 Dy1 100.2(2) . . ? N5 Dy2 Dy1 99.5(2) . . ? N20 Dy2 Dy1 115.3(3) . . ? N19 Dy2 Dy1 98.5(2) . . ? N6 Dy2 Dy1 162.8(2) . . ? O5 Dy2 Dy1 44.13(17) . . ? Dy4 Dy2 Dy1 89.17(3) . . ? O2 Dy3 O3 140.2(3) . . ? O2 Dy3 N28 71.7(3) . . ? O3 Dy3 N28 89.7(3) . . ? O2 Dy3 N8 62.8(3) . . ? O3 Dy3 N8 138.8(3) . . ? N28 Dy3 N8 130.3(3) . . ? O2 Dy3 N31 97.0(3) . . ? O3 Dy3 N31 67.9(3) . . ? N28 Dy3 N31 129.7(3) . . ? N8 Dy3 N31 76.8(4) . . ? O2 Dy3 N7 126.6(3) . . ? O3 Dy3 N7 87.3(3) . . ? N28 Dy3 N7 148.7(3) . . ? N8 Dy3 N7 64.2(3) . . ? N31 Dy3 N7 77.3(3) . . ? O2 Dy3 N17 135.9(3) . . ? O3 Dy3 N17 63.6(3) . . ? N28 Dy3 N17 72.8(3) . . ? N8 Dy3 N17 130.5(3) . . ? N31 Dy3 N17 126.0(4) . . ? N7 Dy3 N17 78.0(3) . . ? O2 Dy3 N18 85.4(3) . . ? O3 Dy3 N18 125.9(3) . . ? N28 Dy3 N18 78.5(3) . . ? N8 Dy3 N18 78.8(3) . . ? N31 Dy3 N18 151.1(3) . . ? N7 Dy3 N18 78.2(3) . . ? N17 Dy3 N18 62.5(3) . . ? O2 Dy3 O5 70.5(3) . . ? O3 Dy3 O5 69.8(3) . . ? N28 Dy3 O5 66.7(3) . . ? N8 Dy3 O5 112.6(3) . . ? N31 Dy3 O5 63.4(3) . . ? N7 Dy3 O5 139.5(3) . . ? N17 Dy3 O5 116.9(3) . . ? N18 Dy3 O5 142.2(3) . . ? O2 Dy3 Dy4 36.93(17) . . ? O3 Dy3 Dy4 107.3(2) . . ? N28 Dy3 Dy4 42.6(2) . . ? N8 Dy3 Dy4 99.2(2) . . ? N31 Dy3 Dy4 100.3(2) . . ? N7 Dy3 Dy4 163.4(2) . . ? N17 Dy3 Dy4 115.3(2) . . ? N18 Dy3 Dy4 98.7(2) . . ? O5 Dy3 Dy4 45.22(17) . . ? O2 Dy3 Dy1 109.7(2) . . ? O3 Dy3 Dy1 36.53(18) . . ? N28 Dy3 Dy1 97.3(2) . . ? N8 Dy3 Dy1 115.6(2) . . ? N31 Dy3 Dy1 39.1(3) . . ? N7 Dy3 Dy1 98.6(2) . . ? N17 Dy3 Dy1 100.0(2) . . ? N18 Dy3 Dy1 162.4(2) . . ? O5 Dy3 Dy1 43.96(17) . . ? Dy4 Dy3 Dy1 89.11(3) . . ? O4 Dy4 O2 141.6(3) . . ? O4 Dy4 N34 70.0(3) . . ? O2 Dy4 N34 92.9(3) . . ? O4 Dy4 N23 64.1(3) . . ? O2 Dy4 N23 136.2(3) . . ? N34 Dy4 N23 129.8(3) . . ? O4 Dy4 N24 125.1(3) . . ? O2 Dy4 N24 86.7(3) . . ? N34 Dy4 N24 150.6(3) . . ? N23 Dy4 N24 61.5(3) . . ? O4 Dy4 N28 95.7(3) . . ? O2 Dy4 N28 69.5(3) . . ? N34 Dy4 N28 131.2(3) . . ? N23 Dy4 N28 73.8(3) . . ? N24 Dy4 N28 75.9(3) . . ? O4 Dy4 N12 85.4(3) . . ? O2 Dy4 N12 125.6(3) . . ? N34 Dy4 N12 78.1(3) . . ? N23 Dy4 N12 79.2(3) . . ? N24 Dy4 N12 78.4(3) . . ? N28 Dy4 N12 149.3(3) . . ? O4 Dy4 N11 133.0(3) . . ? O2 Dy4 N11 64.6(3) . . ? N34 Dy4 N11 70.9(3) . . ? N23 Dy4 N11 131.6(3) . . ? N24 Dy4 N11 82.5(3) . . ? N28 Dy4 N11 129.9(3) . . ? N12 Dy4 N11 61.7(3) . . ? O4 Dy4 O5 71.3(3) . . ? O2 Dy4 O5 70.3(3) . . ? N34 Dy4 O5 66.0(3) . . ? N23 Dy4 O5 114.3(3) . . ? N24 Dy4 O5 139.6(3) . . ? N28 Dy4 O5 65.2(3) . . ? N12 Dy4 O5 142.0(3) . . ? N11 Dy4 O5 114.0(3) . . ? O4 Dy4 Dy3 110.63(19) . . ? O2 Dy4 Dy3 36.66(17) . . ? N34 Dy4 Dy3 99.8(2) . . ? N23 Dy4 Dy3 114.1(2) . . ? N24 Dy4 Dy3 97.24(19) . . ? N28 Dy4 Dy3 40.36(17) . . ? N12 Dy4 Dy3 162.2(2) . . ? N11 Dy4 Dy3 100.7(2) . . ? O5 Dy4 Dy3 45.19(18) . . ? O4 Dy4 Dy2 35.83(18) . . ? O2 Dy4 Dy2 109.79(19) . . ? N34 Dy4 Dy2 42.2(2) . . ? N23 Dy4 Dy2 99.3(2) . . ? N24 Dy4 Dy2 160.8(2) . . ? N28 Dy4 Dy2 100.0(2) . . ? N12 Dy4 Dy2 98.6(3) . . ? N11 Dy4 Dy2 113.1(2) . . ? O5 Dy4 Dy2 45.76(18) . . ? Dy3 Dy4 Dy2 90.95(3) . . ? O8 Dy5 O6 142.1(3) . . ? O8 Dy5 N67 69.0(3) . . ? O6 Dy5 N67 93.9(3) . . ? O8 Dy5 N61 94.2(3) . . ? O6 Dy5 N61 70.3(3) . . ? N67 Dy5 N61 129.5(4) . . ? O8 Dy5 N50 63.9(3) . . ? O6 Dy5 N50 137.1(3) . . ? N67 Dy5 N50 128.1(3) . . ? N61 Dy5 N50 75.4(3) . . ? O8 Dy5 N49 125.1(3) . . ? O6 Dy5 N49 85.5(3) . . ? N67 Dy5 N49 152.8(4) . . ? N61 Dy5 N49 75.8(3) . . ? N50 Dy5 N49 61.3(3) . . ? O8 Dy5 O10 71.5(3) . . ? O6 Dy5 O10 70.6(3) . . ? N67 Dy5 O10 64.6(4) . . ? N61 Dy5 O10 64.9(3) . . ? N50 Dy5 O10 116.4(3) . . ? N49 Dy5 O10 138.9(3) . . ? O8 Dy5 N37 84.3(3) . . ? O6 Dy5 N37 125.0(3) . . ? N67 Dy5 N37 75.1(4) . . ? N61 Dy5 N37 153.0(3) . . ? N50 Dy5 N37 79.8(3) . . ? N49 Dy5 N37 83.0(3) . . ? O10 Dy5 N37 138.1(3) . . ? O8 Dy5 N38 136.3(3) . . ? O6 Dy5 N38 62.2(3) . . ? N67 Dy5 N38 74.8(3) . . ? N61 Dy5 N38 128.2(3) . . ? N50 Dy5 N38 129.9(3) . . ? N49 Dy5 N38 81.0(3) . . ? O10 Dy5 N38 113.7(3) . . ? N37 Dy5 N38 63.0(3) . . ? O8 Dy5 Dy7 35.81(18) . . ? O6 Dy5 Dy7 110.89(19) . . ? N67 Dy5 Dy7 40.3(3) . . ? N61 Dy5 Dy7 99.6(2) . . ? N50 Dy5 Dy7 99.4(2) . . ? N49 Dy5 Dy7 160.7(2) . . ? O10 Dy5 Dy7 46.46(19) . . ? N37 Dy5 Dy7 94.8(2) . . ? N38 Dy5 Dy7 115.1(2) . . ? O8 Dy5 Dy6 110.59(18) . . ? O6 Dy5 Dy6 36.55(18) . . ? N67 Dy5 Dy6 98.9(3) . . ? N61 Dy5 Dy6 41.3(2) . . ? N50 Dy5 Dy6 116.7(2) . . ? N49 Dy5 Dy6 96.72(18) . . ? O10 Dy5 Dy6 44.96(19) . . ? N37 Dy5 Dy6 161.1(2) . . ? N38 Dy5 Dy6 98.3(2) . . ? Dy7 Dy5 Dy6 91.43(3) . . ? O9 Dy6 O6 139.6(3) . . ? O9 Dy6 N61 92.1(3) . . ? O6 Dy6 N61 70.8(3) . . ? O9 Dy6 N70 68.6(2) . . ? O6 Dy6 N70 92.7(2) . . ? N61 Dy6 N70 127.6(3) . . ? O9 Dy6 N56 63.0(3) . . ? O6 Dy6 N56 138.0(3) . . ? N61 Dy6 N56 74.3(3) . . ? N70 Dy6 N56 127.5(3) . . ? O9 Dy6 N55 126.9(3) . . ? O6 Dy6 N55 85.2(3) . . ? N61 Dy6 N55 75.9(3) . . ? N70 Dy6 N55 154.2(3) . . ? N56 Dy6 N55 64.0(3) . . ? O9 Dy6 N42 86.9(3) . . ? O6 Dy6 N42 125.6(3) . . ? N61 Dy6 N42 150.9(3) . . ? N70 Dy6 N42 78.9(3) . . ? N56 Dy6 N42 79.4(3) . . ? N55 Dy6 N42 81.6(3) . . ? O9 Dy6 N41 138.1(3) . . ? O6 Dy6 N41 62.7(2) . . ? N61 Dy6 N41 128.5(3) . . ? N70 Dy6 N41 77.1(3) . . ? N56 Dy6 N41 130.7(3) . . ? N55 Dy6 N41 79.2(3) . . ? N42 Dy6 N41 63.0(3) . . ? O9 Dy6 O10 70.1(2) . . ? O6 Dy6 O10 69.5(2) . . ? N61 Dy6 O10 64.3(3) . . ? N70 Dy6 O10 63.3(3) . . ? N56 Dy6 O10 114.6(3) . . ? N55 Dy6 O10 137.8(3) . . ? N42 Dy6 O10 140.6(3) . . ? N41 Dy6 O10 114.8(3) . . ? O9 Dy6 Dy8 36.51(16) . . ? O6 Dy6 Dy8 107.87(19) . . ? N61 Dy6 Dy8 97.6(2) . . ? N70 Dy6 Dy8 39.4(2) . . ? N56 Dy6 Dy8 99.1(2) . . ? N55 Dy6 Dy8 162.9(2) . . ? N42 Dy6 Dy8 98.7(2) . . ? N41 Dy6 Dy8 116.3(2) . . ? O10 Dy6 Dy8 44.57(17) . . ? O9 Dy6 Dy5 107.94(19) . . ? O6 Dy6 Dy5 36.62(16) . . ? N61 Dy6 Dy5 41.9(2) . . ? N70 Dy6 Dy5 96.72(18) . . ? N56 Dy6 Dy5 116.10(19) . . ? N55 Dy6 Dy5 96.7(2) . . ? N42 Dy6 Dy5 162.0(2) . . ? N41 Dy6 Dy5 99.03(19) . . ? O10 Dy6 Dy5 43.59(17) . . ? Dy8 Dy6 Dy5 88.16(3) . . ? O7 Dy7 O8 139.3(3) . . ? O7 Dy7 N67 90.9(3) . . ? O8 Dy7 N67 69.2(3) . . ? O7 Dy7 N64 71.8(3) . . ? O8 Dy7 N64 92.3(3) . . ? N67 Dy7 N64 127.8(4) . . ? O7 Dy7 N53 139.3(3) . . ? O8 Dy7 N53 64.0(3) . . ? N67 Dy7 N53 128.5(3) . . ? N64 Dy7 N53 75.1(3) . . ? O7 Dy7 N54 88.6(4) . . ? O8 Dy7 N54 125.2(4) . . ? N67 Dy7 N54 152.8(4) . . ? N64 Dy7 N54 77.6(4) . . ? N53 Dy7 N54 61.4(4) . . ? O7 Dy7 N44 63.9(3) . . ? O8 Dy7 N44 134.7(3) . . ? N67 Dy7 N44 73.3(3) . . ? N64 Dy7 N44 131.4(3) . . ? N53 Dy7 N44 130.1(4) . . ? N54 Dy7 N44 82.1(4) . . ? O7 Dy7 N43 126.6(3) . . ? O8 Dy7 N43 85.3(3) . . ? N67 Dy7 N43 78.7(4) . . ? N64 Dy7 N43 150.4(3) . . ? N53 Dy7 N43 77.4(4) . . ? N54 Dy7 N43 79.8(4) . . ? N44 Dy7 N43 62.9(4) . . ? O7 Dy7 O10 70.5(3) . . ? O8 Dy7 O10 68.9(3) . . ? N67 Dy7 O10 63.0(3) . . ? N64 Dy7 O10 64.9(3) . . ? N53 Dy7 O10 115.1(3) . . ? N54 Dy7 O10 141.0(3) . . ? N44 Dy7 O10 114.6(3) . . ? N43 Dy7 O10 139.1(3) . . ? O7 Dy7 Dy8 37.03(19) . . ? O8 Dy7 Dy8 107.99(18) . . ? N67 Dy7 Dy8 96.2(3) . . ? N64 Dy7 Dy8 42.2(2) . . ? N53 Dy7 Dy8 117.2(2) . . ? N54 Dy7 Dy8 99.6(3) . . ? N44 Dy7 Dy8 100.5(3) . . ? N43 Dy7 Dy8 163.3(3) . . ? O10 Dy7 Dy8 44.63(16) . . ? O7 Dy7 Dy5 107.9(2) . . ? O8 Dy7 Dy5 35.51(19) . . ? N67 Dy7 Dy5 40.9(2) . . ? N64 Dy7 Dy5 97.3(2) . . ? N53 Dy7 Dy5 99.1(3) . . ? N54 Dy7 Dy5 160.5(3) . . ? N44 Dy7 Dy5 114.2(2) . . ? N43 Dy7 Dy5 97.7(2) . . ? O10 Dy7 Dy5 43.65(16) . . ? Dy8 Dy7 Dy5 88.28(3) . . ? O9 Dy8 O7 141.9(3) . . ? O9 Dy8 N70 70.0(2) . . ? O7 Dy8 N70 94.5(3) . . ? O9 Dy8 N64 93.0(3) . . ? O7 Dy8 N64 71.2(3) . . ? N70 Dy8 N64 131.8(3) . . ? O9 Dy8 N47 138.1(3) . . ? O7 Dy8 N47 62.5(3) . . ? N70 Dy8 N47 75.6(3) . . ? N64 Dy8 N47 128.3(3) . . ? O9 Dy8 N48 84.8(3) . . ? O7 Dy8 N48 126.5(3) . . ? N70 Dy8 N48 76.6(3) . . ? N64 Dy8 N48 148.7(3) . . ? N47 Dy8 N48 64.2(3) . . ? O9 Dy8 N59 62.8(3) . . ? O7 Dy8 N59 137.4(3) . . ? N70 Dy8 N59 127.4(3) . . ? N64 Dy8 N59 74.0(3) . . ? N47 Dy8 N59 129.1(3) . . ? N48 Dy8 N59 77.3(3) . . ? O9 Dy8 N60 126.2(3) . . ? O7 Dy8 N60 84.9(3) . . ? N70 Dy8 N60 149.6(3) . . ? N64 Dy8 N60 76.7(4) . . ? N47 Dy8 N60 77.3(3) . . ? N48 Dy8 N60 79.6(4) . . ? N59 Dy8 N60 63.5(3) . . ? O9 Dy8 O10 70.4(3) . . ? O7 Dy8 O10 71.5(3) . . ? N70 Dy8 O10 65.1(3) . . ? N64 Dy8 O10 66.7(3) . . ? N47 Dy8 O10 115.4(3) . . ? N48 Dy8 O10 139.4(3) . . ? N59 Dy8 O10 115.5(3) . . ? N60 Dy8 O10 141.0(3) . . ? O9 Dy8 Dy7 110.80(19) . . ? O7 Dy8 Dy7 35.92(18) . . ? N70 Dy8 Dy7 100.48(18) . . ? N64 Dy8 Dy7 42.6(2) . . ? N47 Dy8 Dy7 98.2(2) . . ? N48 Dy8 Dy7 162.4(2) . . ? N59 Dy8 Dy7 116.6(2) . . ? N60 Dy8 Dy7 96.6(3) . . ? O10 Dy8 Dy7 46.83(19) . . ? O9 Dy8 Dy6 35.99(17) . . ? O7 Dy8 Dy6 110.9(2) . . ? N70 Dy8 Dy6 41.38(18) . . ? N64 Dy8 Dy6 99.9(2) . . ? N47 Dy8 Dy6 116.9(2) . . ? N48 Dy8 Dy6 96.5(2) . . ? N59 Dy8 Dy6 98.6(2) . . ? N60 Dy8 Dy6 162.1(3) . . ? O10 Dy8 Dy6 45.30(19) . . ? Dy7 Dy8 Dy6 92.13(3) . . ? C8 O1 Dy2 127.7(8) . . ? C8 O1 Dy1 121.7(8) . . ? Dy2 O1 Dy1 106.5(3) . . ? C23 O2 Dy3 123.8(7) . . ? C23 O2 Dy4 126.6(7) . . ? Dy3 O2 Dy4 106.4(3) . . ? C38 O3 Dy1 129.0(8) . . ? C38 O3 Dy3 123.0(8) . . ? Dy1 O3 Dy3 106.5(3) . . ? C53 O4 Dy2 128.0(7) . . ? C53 O4 Dy4 120.7(7) . . ? Dy2 O4 Dy4 108.0(3) . . ? Dy1 O5 Dy3 91.1(3) . . ? Dy1 O5 Dy4 175.6(4) . . ? Dy3 O5 Dy4 89.6(2) . . ? Dy1 O5 Dy2 90.1(2) . . ? Dy3 O5 Dy2 178.6(3) . . ? Dy4 O5 Dy2 89.1(2) . . ? C68 O6 Dy6 121.1(7) . . ? C68 O6 Dy5 129.2(7) . . ? Dy6 O6 Dy5 106.8(3) . . ? C83 O7 Dy7 126.6(8) . . ? C83 O7 Dy8 122.6(7) . . ? Dy7 O7 Dy8 107.0(3) . . ? C98 O8 Dy5 125.7(7) . . ? C98 O8 Dy7 122.6(7) . . ? Dy5 O8 Dy7 108.7(3) . . ? C113 O9 Dy6 126.7(8) . . ? C113 O9 Dy8 123.7(8) . . ? Dy6 O9 Dy8 107.5(3) . . ? Dy5 O10 Dy8 178.4(4) . . ? Dy5 O10 Dy6 91.4(3) . . ? Dy8 O10 Dy6 90.1(2) . . ? Dy5 O10 Dy7 89.9(2) . . ? Dy8 O10 Dy7 88.5(2) . . ? Dy6 O10 Dy7 178.6(3) . . ? C1 N1 C5 118.5(12) . . ? C1 N1 Dy1 125.3(9) . . ? C5 N1 Dy1 116.2(9) . . ? C6 N2 N3 114.1(11) . . ? C6 N2 Dy1 124.0(9) . . ? N3 N2 Dy1 121.0(8) . . ? C8 N3 N2 108.8(10) . . ? C8 N4 N5 114.2(9) . . ? C8 N4 H4 122.9 . . ? N5 N4 H4 122.9 . . ? C10 N5 N4 117.3(10) . . ? C10 N5 Dy2 124.8(9) . . ? N4 N5 Dy2 117.3(7) . . ? C15 N6 C11 121.9(12) . . ? C15 N6 Dy2 120.6(9) . . ? C11 N6 Dy2 116.5(8) . . ? C16 N7 C20 120.2(10) . . ? C16 N7 Dy3 122.9(7) . . ? C20 N7 Dy3 116.8(7) . . ? C21 N8 N9 117.6(10) . . ? C21 N8 Dy3 124.3(9) . . ? N9 N8 Dy3 118.1(6) . . ? C23 N9 N8 110.1(9) . . ? C23 N10 N11 117.8(9) . . ? C23 N10 H10 121.1 . . ? N11 N10 H10 121.1 . . ? C25 N11 N10 120.4(10) . . ? C25 N11 Dy4 125.5(8) . . ? N10 N11 Dy4 113.4(6) . . ? C30 N12 C26 116.6(11) . . ? C30 N12 Dy4 123.0(8) . . ? C26 N12 Dy4 118.5(8) . . ? C35 N13 C31 120.3(9) . . ? C35 N13 Dy1 118.6(8) . . ? C31 N13 Dy1 121.0(6) . . ? C36 N14 N15 117.5(9) . . ? C36 N14 Dy1 126.3(8) . . ? N15 N14 Dy1 116.1(6) . . ? C38 N15 N14 116.8(9) . . ? C38 N16 N17 112.6(9) . . ? C40 N17 N16 116.0(9) . . ? C40 N17 Dy3 126.2(8) . . ? N16 N17 Dy3 117.7(6) . . ? C41 N18 C45 115.7(9) . . ? C41 N18 Dy3 117.9(8) . . ? C45 N18 Dy3 125.5(7) . . ? C50 N19 C46 115.9(12) . . ? C50 N19 Dy2 117.4(9) . . ? C46 N19 Dy2 126.7(9) . . ? C51 N20 N21 121.8(12) . . ? C51 N20 Dy2 122.2(11) . . ? N21 N20 Dy2 115.9(8) . . ? C53 N21 N20 116.0(10) . . ? C53 N22 N23 110.4(8) . . ? C55 N23 N22 119.2(10) . . ? C55 N23 Dy4 121.7(8) . . ? N22 N23 Dy4 119.1(6) . . ? C56 N24 C60 110.0(10) . . ? C56 N24 Dy4 126.6(9) . . ? C60 N24 Dy4 123.2(6) . . ? N26 N25 Dy1 129.2(8) . . ? N26 N25 Dy2 128.4(8) . . ? Dy1 N25 Dy2 96.4(4) . . ? N27 N26 N25 177.0(15) . . ? N29 N28 Dy3 133.2(7) . . ? N29 N28 Dy4 124.6(7) . . ? Dy3 N28 Dy4 97.1(3) . . ? N30 N29 N28 175.3(12) . . ? N32 N31 Dy1 132.9(8) . . ? N32 N31 Dy3 125.1(8) . . ? Dy1 N31 Dy3 99.1(3) . . ? N33 N32 N31 175.8(12) . . ? N35 N34 Dy4 132.6(9) . . ? N35 N34 Dy2 129.8(9) . . ? Dy4 N34 Dy2 95.6(3) . . ? N36 N35 N34 177.9(16) . . ? C61 N37 C65 116.4(9) . . ? C61 N37 Dy5 122.9(7) . . ? C65 N37 Dy5 120.4(7) . . ? C66 N38 N39 122.2(9) . . ? C66 N38 Dy5 121.7(8) . . ? N39 N38 Dy5 115.9(6) . . ? N38 N39 C68 115.8(9) . . ? N38 N39 H39 122.1 . . ? C68 N39 H39 122.1 . . ? C68 N40 N41 107.6(8) . . ? C70 N41 N40 120.5(10) . . ? C70 N41 Dy6 120.3(8) . . ? N40 N41 Dy6 118.7(6) . . ? C75 N42 C71 118.7(11) . . ? C75 N42 Dy6 121.7(10) . . ? C71 N42 Dy6 119.5(7) . . ? C76 N43 C80 116.9(12) . . ? C76 N43 Dy7 123.8(9) . . ? C80 N43 Dy7 119.2(9) . . ? N45 N44 C81 121.0(10) . . ? N45 N44 Dy7 115.1(7) . . ? C81 N44 Dy7 123.7(9) . . ? N44 N45 C83 117.2(10) . . ? C83 N46 N47 108.0(9) . . ? C83 N46 H46 126.0 . . ? N47 N46 H46 126.0 . . ? C85 N47 N46 114.6(10) . . ? C85 N47 Dy8 123.7(8) . . ? N46 N47 Dy8 121.8(7) . . ? C90 N48 C86 118.3(10) . . ? C90 N48 Dy8 122.5(7) . . ? C86 N48 Dy8 118.9(8) . . ? C95 N49 C91 114.4(10) . . ? C95 N49 Dy5 120.5(9) . . ? C91 N49 Dy5 125.1(6) . . ? C96 N50 N51 118.3(10) . . ? C96 N50 Dy5 124.4(8) . . ? N51 N50 Dy5 115.8(7) . . ? C98 N51 N50 117.1(10) . . ? C98 N52 N53 113.4(10) . . ? C100 N53 N52 117.3(11) . . ? C100 N53 Dy7 122.6(10) . . ? N52 N53 Dy7 117.0(7) . . ? C101 N54 C105 113.9(12) . . ? C101 N54 Dy7 120.8(9) . . ? C105 N54 Dy7 124.6(9) . . ? C110 N55 C106 114.4(10) . . ? C110 N55 Dy6 118.0(8) . . ? C106 N55 Dy6 127.6(7) . . ? C111 N56 N57 116.9(9) . . ? C111 N56 Dy6 121.8(8) . . ? N57 N56 Dy6 120.4(7) . . ? N56 N57 C113 110.8(9) . . ? C113 N58 N59 111.7(10) . . ? C115 N59 N58 120.8(10) . . ? C115 N59 Dy8 121.5(8) . . ? N58 N59 Dy8 117.6(7) . . ? C116 N60 C120 114.9(10) . . ? C116 N60 Dy8 116.5(8) . . ? C120 N60 Dy8 128.4(8) . . ? N62 N61 Dy6 129.8(8) . . ? N62 N61 Dy5 127.6(7) . . ? Dy6 N61 Dy5 96.8(3) . . ? N63 N62 N61 174.7(13) . . ? N65 N64 Dy8 128.9(8) . . ? N65 N64 Dy7 130.9(8) . . ? Dy8 N64 Dy7 95.2(3) . . ? N66 N65 N64 177.2(12) . . ? N68 N67 Dy7 128.6(8) . . ? N68 N67 Dy5 129.1(9) . . ? Dy7 N67 Dy5 98.8(4) . . ? N69 N68 N67 176.5(16) . . ? N71 N70 Dy8 131.3(7) . . ? N71 N70 Dy6 125.9(8) . . ? Dy8 N70 Dy6 99.3(3) . . ? N72 N71 N70 174.5(11) . . ? N1 C1 C2 126.0(13) . . ? N1 C1 H1 117.0 . . ? C2 C1 H1 117.0 . . ? C3 C2 C1 114.1(13) . . ? C3 C2 H2 122.9 . . ? C1 C2 H2 122.9 . . ? C4 C3 C2 117.7(13) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C5 124.6(15) . . ? C3 C4 H4A 117.7 . . ? C5 C4 H4A 117.7 . . ? N1 C5 C4 118.2(13) . . ? N1 C5 C6 122.9(12) . . ? C4 C5 C6 118.9(12) . . ? N2 C6 C5 112.1(11) . . ? N2 C6 C7 121.6(13) . . ? C5 C6 C7 126.3(13) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 N3 123.5(12) . . ? O1 C8 N4 116.4(11) . . ? N3 C8 N4 120.1(12) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 C11 115.8(12) . . ? N5 C10 C9 121.5(13) . . ? C11 C10 C9 122.6(12) . . ? C12 C11 N6 119.9(14) . . ? C12 C11 C10 121.9(15) . . ? N6 C11 C10 118.3(11) . . ? C11 C12 C13 116.8(17) . . ? C11 C12 H12 121.6 . . ? C13 C12 H12 121.6 . . ? C14 C13 C12 120.7(16) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.6(15) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? N6 C15 C14 120.1(15) . . ? N6 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? N7 C16 C17 120.3(11) . . ? N7 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 122.1(13) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C19 118.1(13) . . ? C17 C18 H18 121.0 . . ? C19 C18 H18 121.0 . . ? C18 C19 C20 120.1(14) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? N7 C20 C19 117.6(12) . . ? N7 C20 C21 119.8(10) . . ? C19 C20 C21 122.6(12) . . ? N8 C21 C20 114.8(11) . . ? N8 C21 C22 123.4(13) . . ? C20 C21 C22 121.5(12) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 O2 124.3(10) . . ? N9 C23 N10 119.1(9) . . ? O2 C23 N10 116.6(10) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 C26 115.0(10) . . ? N11 C25 C24 125.8(12) . . ? C26 C25 C24 119.2(10) . . ? N12 C26 C27 118.8(13) . . ? N12 C26 C25 116.2(11) . . ? C27 C26 C25 124.9(11) . . ? C28 C27 C26 121.3(11) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C29 120.2(12) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 115.5(14) . . ? C30 C29 H29 122.2 . . ? C28 C29 H29 122.2 . . ? N12 C30 C29 127.1(12) . . ? N12 C30 H30 116.4 . . ? C29 C30 H30 116.4 . . ? C32 C31 N13 124.4(10) . . ? C32 C31 H31 117.8 . . ? N13 C31 H31 117.8 . . ? C31 C32 C33 114.2(14) . . ? C31 C32 H32 122.9 . . ? C33 C32 H32 122.9 . . ? C32 C33 C34 121.4(14) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C35 C34 C33 119.2(14) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? N13 C35 C34 119.0(13) . . ? N13 C35 C36 122.3(11) . . ? C34 C35 C36 118.6(12) . . ? N14 C36 C35 111.4(10) . . ? N14 C36 C37 127.2(13) . . ? C35 C36 C37 121.2(12) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N16 C38 O3 122.5(11) . . ? N16 C38 N15 122.4(10) . . ? O3 C38 N15 115.1(11) . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N17 C40 C41 114.6(10) . . ? N17 C40 C39 126.6(12) . . ? C41 C40 C39 118.1(11) . . ? N18 C41 C42 121.7(12) . . ? N18 C41 C40 117.8(10) . . ? C42 C41 C40 120.0(11) . . ? C41 C42 C43 118.6(12) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C44 C43 C42 121.0(12) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C45 C44 C43 111.5(14) . . ? C45 C44 H44 124.3 . . ? C43 C44 H44 124.3 . . ? C44 C45 N18 130.9(11) . . ? C44 C45 H45 114.5 . . ? N18 C45 H45 114.5 . . ? C47 C46 N19 123.6(14) . . ? C47 C46 H46A 118.2 . . ? N19 C46 H46A 118.2 . . ? C48 C47 C46 126.0(18) . . ? C48 C47 H47 117.0 . . ? C46 C47 H47 117.0 . . ? C47 C48 C49 117.4(18) . . ? C47 C48 H48 121.3 . . ? C49 C48 H48 121.3 . . ? C50 C49 C48 119.7(17) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? N19 C50 C51 119.0(13) . . ? N19 C50 C49 116.7(14) . . ? C51 C50 C49 123.4(15) . . ? N20 C51 C50 118.4(13) . . ? N20 C51 C52 118.1(16) . . ? C50 C51 C52 123.5(14) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N22 C53 O4 125.0(10) . . ? N22 C53 N21 120.0(10) . . ? O4 C53 N21 115.0(10) . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N23 C55 C56 118.6(12) . . ? N23 C55 C54 118.7(12) . . ? C56 C55 C54 122.5(12) . . ? N24 C56 C57 128.8(13) . . ? N24 C56 C55 111.2(12) . . ? C57 C56 C55 119.8(13) . . ? C58 C57 C56 120.9(14) . . ? C58 C57 H57 119.5 . . ? C56 C57 H57 119.5 . . ? C57 C58 C59 115.2(13) . . ? C57 C58 H58 122.4 . . ? C59 C58 H58 122.4 . . ? C60 C59 C58 124.3(14) . . ? C60 C59 H59 117.8 . . ? C58 C59 H59 117.8 . . ? C59 C60 N24 120.1(11) . . ? C59 C60 H60 120.0 . . ? N24 C60 H60 120.0 . . ? C62 C61 N37 127.3(11) . . ? C62 C61 H61 116.4 . . ? N37 C61 H61 116.4 . . ? C61 C62 C63 117.2(13) . . ? C61 C62 H62 121.4 . . ? C63 C62 H62 121.4 . . ? C64 C63 C62 118.6(12) . . ? C64 C63 H63 120.7 . . ? C62 C63 H63 120.7 . . ? C63 C64 C65 119.5(12) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? N37 C65 C64 120.5(11) . . ? N37 C65 C66 116.3(9) . . ? C64 C65 C66 123.1(10) . . ? N38 C66 C65 118.1(10) . . ? N38 C66 C67 120.3(11) . . ? C65 C66 C67 121.6(10) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O6 C68 N40 128.7(10) . . ? O6 C68 N39 115.8(10) . . ? N40 C68 N39 115.4(9) . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N41 C70 C71 118.8(11) . . ? N41 C70 C69 118.9(12) . . ? C71 C70 C69 122.1(10) . . ? N42 C71 C70 118.1(9) . . ? N42 C71 C72 122.5(11) . . ? C70 C71 C72 119.4(12) . . ? C73 C72 C71 114.6(12) . . ? C73 C72 H72 122.7 . . ? C71 C72 H72 122.7 . . ? C74 C73 C72 122.3(11) . . ? C74 C73 H73 118.9 . . ? C72 C73 H73 118.9 . . ? C73 C74 C75 118.0(15) . . ? C73 C74 H74 121.0 . . ? C75 C74 H74 121.0 . . ? N42 C75 C74 123.2(15) . . ? N42 C75 H75 118.4 . . ? C74 C75 H75 118.4 . . ? N43 C76 C77 125.0(13) . . ? N43 C76 H76 117.5 . . ? C77 C76 H76 117.5 . . ? C78 C77 C76 117.2(18) . . ? C78 C77 H77 121.4 . . ? C76 C77 H77 121.4 . . ? C79 C78 C77 120.5(19) . . ? C79 C78 H78 119.8 . . ? C77 C78 H78 119.8 . . ? C78 C79 C80 118.6(15) . . ? C78 C79 H79 120.7 . . ? C80 C79 H79 120.7 . . ? N43 C80 C79 120.7(14) . . ? N43 C80 C81 119.7(13) . . ? C79 C80 C81 119.1(14) . . ? N44 C81 C80 114.3(12) . . ? N44 C81 C82 119.4(13) . . ? C80 C81 C82 126.1(12) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O7 C83 N46 122.8(11) . . ? O7 C83 N45 115.5(12) . . ? N46 C83 N45 120.9(11) . . ? C85 C84 H84A 109.5 . . ? C85 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C85 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N47 C85 C86 117.1(11) . . ? N47 C85 C84 127.2(13) . . ? C86 C85 C84 115.7(13) . . ? N48 C86 C87 119.5(11) . . ? N48 C86 C85 115.8(11) . . ? C87 C86 C85 124.7(12) . . ? C86 C87 C88 121.1(12) . . ? C86 C87 H87 119.5 . . ? C88 C87 H87 119.5 . . ? C89 C88 C87 117.0(13) . . ? C89 C88 H88 121.5 . . ? C87 C88 H88 121.5 . . ? C88 C89 C90 118.5(13) . . ? C88 C89 H89 120.7 . . ? C90 C89 H89 120.7 . . ? N48 C90 C89 124.9(11) . . ? N48 C90 H90 117.6 . . ? C89 C90 H90 117.6 . . ? C92 C91 N49 126.6(11) . . ? C92 C91 H91 116.7 . . ? N49 C91 H91 116.7 . . ? C91 C92 C93 115.0(13) . . ? C91 C92 H92 122.5 . . ? C93 C92 H92 122.5 . . ? C94 C93 C92 125.8(14) . . ? C94 C93 H93 117.1 . . ? C92 C93 H93 117.1 . . ? C93 C94 C95 121.2(14) . . ? C93 C94 H94 119.4 . . ? C95 C94 H94 119.4 . . ? N49 C95 C96 115.3(11) . . ? N49 C95 C94 116.8(12) . . ? C96 C95 C94 127.8(11) . . ? N50 C96 C95 117.2(10) . . ? N50 C96 C97 123.9(13) . . ? C95 C96 C97 118.9(11) . . ? C96 C97 H97A 109.5 . . ? C96 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C96 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? N52 C98 N51 122.3(11) . . ? N52 C98 O8 121.6(11) . . ? N51 C98 O8 116.1(10) . . ? C100 C99 H99A 109.5 . . ? C100 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C100 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? N53 C100 C101 115.0(13) . . ? N53 C100 C99 121.6(14) . . ? C101 C100 C99 123.3(12) . . ? N54 C101 C102 121.6(15) . . ? N54 C101 C100 117.6(12) . . ? C102 C101 C100 120.6(16) . . ? C101 C102 C103 116.6(18) . . ? C101 C102 H102 121.7 . . ? C103 C102 H102 121.7 . . ? C104 C103 C102 123.7(16) . . ? C104 C103 H103 118.2 . . ? C102 C103 H103 118.2 . . ? C103 C104 C105 116.9(15) . . ? C103 C104 H104 121.5 . . ? C105 C104 H104 121.5 . . ? C104 C105 N54 127.0(13) . . ? C104 C105 H105 116.5 . . ? N54 C105 H105 116.5 . . ? C107 C106 N55 128.6(12) . . ? C107 C106 H106 115.7 . . ? N55 C106 H106 115.7 . . ? C106 C107 C108 116.0(16) . . ? C106 C107 H107 122.0 . . ? C108 C107 H107 122.0 . . ? C109 C108 C107 118.1(16) . . ? C109 C108 H108 120.9 . . ? C107 C108 H108 120.9 . . ? C108 C109 C110 126.0(14) . . ? C108 C109 H109 117.0 . . ? C110 C109 H109 117.0 . . ? N55 C110 C109 116.3(13) . . ? N55 C110 C111 117.4(11) . . ? C109 C110 C111 125.9(13) . . ? N56 C111 C110 117.9(11) . . ? N56 C111 C112 123.5(12) . . ? C110 C111 C112 118.6(12) . . ? C111 C112 H11A 109.5 . . ? C111 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? C111 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? N58 C113 O9 123.1(12) . . ? N58 C113 N57 118.4(10) . . ? O9 C113 N57 118.5(10) . . ? C115 C114 H11D 109.5 . . ? C115 C114 H11E 109.5 . . ? H11D C114 H11E 109.5 . . ? C115 C114 H11F 109.5 . . ? H11D C114 H11F 109.5 . . ? H11E C114 H11F 109.5 . . ? N59 C115 C116 118.6(12) . . ? N59 C115 C114 118.3(12) . . ? C116 C115 C114 122.4(13) . . ? C115 C116 N60 119.7(12) . . ? C115 C116 C117 125.5(13) . . ? N60 C116 C117 114.8(12) . . ? C118 C117 C116 121.8(14) . . ? C118 C117 H117 119.1 . . ? C116 C117 H117 119.1 . . ? C119 C118 C117 123.1(15) . . ? C119 C118 H118 118.5 . . ? C117 C118 H118 118.5 . . ? C120 C119 C118 115.6(13) . . ? C120 C119 H119 122.2 . . ? C118 C119 H119 122.2 . . ? C119 C120 N60 129.7(11) . . ? C119 C120 H120 115.2 . . ? N60 C120 H120 115.2 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 7.672 _refine_diff_density_min -3.938 _refine_diff_density_rms 0.257 _iucr_refine_instructions_details ; TITL _2 CELL 0.71075 19.80600 20.03700 27.32600 84.310 86.780 71.967 ZERR 4 0.00900 0.00900 0.01500 0.030 0.020 0.018 LATT 1 SFAC H DY N O C UNIT 432 16 144 120 240 SHEL 8.147180 0.796452 L.S. 5 FMAP 2 PLAN -60 TEMP -110.0 ACTA BOND $H OMIT -2 0 2 SIZE 0.200 0.200 0.100 WGHT 0.200000 FVAR 1.04226 DY1 2 0.224754 0.768009 0.067024 11.00000 0.06675 0.04973 = 0.04590 0.00627 -0.00326 -0.01202 DY2 2 0.192156 0.827132 0.191654 11.00000 0.07040 0.05692 = 0.04871 0.00407 -0.00321 -0.01752 DY3 2 0.410108 0.769763 0.068287 11.00000 0.06602 0.04182 = 0.04163 0.00337 -0.00124 -0.01051 DY4 2 0.374373 0.837003 0.190181 11.00000 0.06902 0.04801 = 0.04073 0.00698 -0.00406 -0.01488 DY5 2 0.580894 0.753988 0.492707 11.00000 0.06802 0.04782 = 0.04028 0.00024 -0.00124 -0.01440 DY6 2 0.579799 0.730701 0.628391 11.00000 0.07388 0.04935 = 0.03961 0.00134 -0.00236 -0.01900 DY7 2 0.766965 0.755261 0.487797 11.00000 0.07498 0.06579 = 0.05721 0.00039 -0.00304 -0.01939 DY8 2 0.764352 0.733913 0.622574 11.00000 0.07263 0.05122 = 0.05172 0.00432 0.00216 -0.01830 O1 4 0.186819 0.740348 0.145814 11.00000 0.06972 0.05698 = 0.07091 0.01706 0.00249 -0.02918 O2 4 0.448547 0.748770 0.147170 11.00000 0.07550 0.04022 = 0.05055 0.00348 -0.01086 0.00161 O3 4 0.306122 0.813757 0.025398 11.00000 0.07786 0.04710 = 0.05462 0.01655 -0.00274 -0.01287 O4 4 0.257495 0.899911 0.199471 11.00000 0.09826 0.06758 = 0.04960 0.00337 -0.00976 -0.04338 O5 4 0.301145 0.797180 0.129133 11.00000 0.07738 0.07037 = 0.06896 -0.01289 0.00213 -0.02063 O6 4 0.522535 0.801256 0.562368 11.00000 0.07328 0.05200 = 0.04756 -0.00991 0.01118 -0.00802 O7 4 0.784528 0.804129 0.554679 11.00000 0.08628 0.06681 = 0.05429 -0.00321 0.00376 -0.03945 O8 4 0.690773 0.702330 0.461362 11.00000 0.07818 0.04856 = 0.04667 0.00554 -0.00306 -0.02181 O9 4 0.691174 0.669312 0.651855 11.00000 0.06603 0.04550 = 0.05586 0.01536 0.00086 -0.01892 O10 4 0.670973 0.743432 0.558190 11.00000 0.07095 0.11030 = 0.04827 0.00800 -0.01198 -0.02085 N1 3 0.241889 0.695375 -0.006106 11.00000 0.09235 0.06978 = 0.05488 0.01347 -0.02011 -0.00329 N2 3 0.206766 0.651639 0.084354 11.00000 0.08025 0.07286 = 0.06717 0.01340 -0.02097 -0.03240 N3 3 0.195526 0.626261 0.131575 11.00000 0.11606 0.07932 = 0.05828 0.00749 -0.00837 -0.05542 N4 3 0.179394 0.663358 0.210222 11.00000 0.07735 0.05438 = 0.05457 0.01108 -0.01029 -0.01848 AFIX 43 H4 1 0.177863 0.622195 0.223928 11.00000 -1.20000 AFIX 0 N5 3 0.173136 0.720119 0.236988 11.00000 0.09603 0.06105 = 0.04940 0.00935 -0.00658 -0.03008 N6 3 0.167370 0.830833 0.284729 11.00000 0.10782 0.07095 = 0.05358 -0.00507 0.01764 -0.01305 N7 3 0.459273 0.695169 -0.000912 11.00000 0.07703 0.05552 = 0.05531 -0.00478 0.01020 -0.01961 N8 3 0.499198 0.654806 0.090641 11.00000 0.06829 0.05692 = 0.06360 -0.01204 0.01680 -0.00721 N9 3 0.517606 0.637085 0.140942 11.00000 0.09073 0.05993 = 0.05594 0.00831 -0.00130 -0.02227 N10 3 0.495314 0.680371 0.214988 11.00000 0.09608 0.05273 = 0.06214 0.01193 -0.03471 -0.01349 AFIX 43 H10 1 0.522840 0.641064 0.229662 11.00000 -1.20000 AFIX 0 N11 3 0.457468 0.736417 0.241873 11.00000 0.09568 0.05534 = 0.04839 0.00499 -0.00339 -0.02202 N12 3 0.382505 0.850451 0.280352 11.00000 0.09629 0.06957 = 0.04548 0.00573 -0.00727 -0.01987 N13 3 0.095550 0.799709 0.042737 11.00000 0.06664 0.05473 = 0.07381 0.01489 -0.02695 -0.00696 N14 3 0.180672 0.861227 -0.002706 11.00000 0.07126 0.05557 = 0.04438 -0.00145 -0.01021 -0.01886 N15 3 0.230703 0.890143 -0.026008 11.00000 0.08364 0.05539 = 0.03846 0.01663 0.00054 -0.01372 N16 3 0.345891 0.890467 -0.026932 11.00000 0.07352 0.05932 = 0.04286 0.00833 -0.00440 -0.02233 N17 3 0.409236 0.860120 -0.001875 11.00000 0.06330 0.05114 = 0.03772 0.00466 -0.00022 -0.00875 N18 3 0.525971 0.798628 0.046709 11.00000 0.06521 0.06179 = 0.05937 -0.00890 0.00611 -0.01224 N19 3 0.056718 0.861149 0.194213 11.00000 0.09263 0.09782 = 0.04660 0.00556 -0.01126 -0.04177 N20 3 0.124492 0.956292 0.196209 11.00000 0.08479 0.07111 = 0.06585 0.00395 -0.00340 -0.00437 N21 3 0.165403 1.001509 0.194207 11.00000 0.07656 0.06873 = 0.06559 -0.00300 -0.01728 -0.01704 N22 3 0.278042 1.008600 0.189868 11.00000 0.08949 0.04669 = 0.04705 0.00029 0.00169 -0.02760 N23 3 0.347888 0.966657 0.188880 11.00000 0.08041 0.04426 = 0.03882 0.00080 -0.01301 -0.01170 N24 3 0.475340 0.886226 0.189310 11.00000 0.10359 0.05848 = 0.02260 0.00315 -0.01539 -0.03818 N25 3 0.166883 0.877663 0.105991 11.00000 0.09327 0.07366 = 0.04604 0.00077 -0.00391 -0.01371 N26 3 0.119863 0.927903 0.091404 11.00000 0.06122 0.07304 = 0.05362 0.00472 -0.01109 0.00331 N27 3 0.078185 0.975627 0.076637 11.00000 0.09913 0.12321 = 0.08792 -0.01115 -0.01902 0.01550 N28 3 0.386604 0.880578 0.102210 11.00000 0.07727 0.03960 = 0.04842 -0.00543 -0.00415 -0.02093 N29 3 0.401329 0.934248 0.088630 11.00000 0.07660 0.05561 = 0.06434 -0.00888 0.00269 -0.00853 N30 3 0.416255 0.983559 0.072536 11.00000 0.15987 0.07084 = 0.06006 0.01116 0.01993 -0.05301 N31 3 0.339104 0.686306 0.075310 11.00000 0.11351 0.05487 = 0.09397 -0.04042 0.06128 -0.05782 N32 3 0.363279 0.622116 0.070136 11.00000 0.06731 0.05330 = 0.05648 -0.00503 -0.00318 -0.00488 N33 3 0.385873 0.563922 0.062280 11.00000 0.11029 0.06237 = 0.09676 -0.00357 0.00497 -0.01591 N34 3 0.306905 0.759481 0.229443 11.00000 0.09791 0.04714 = 0.04026 0.02117 -0.00492 -0.02019 N35 3 0.319277 0.714667 0.263755 11.00000 0.10719 0.07555 = 0.04961 -0.00154 0.00433 -0.03283 N36 3 0.328829 0.673594 0.296555 11.00000 0.10570 0.07636 = 0.07780 0.03194 -0.02292 -0.01674 N37 3 0.554857 0.809914 0.404978 11.00000 0.06283 0.06785 = 0.04681 -0.00704 -0.00710 -0.01144 N38 3 0.487380 0.876036 0.482398 11.00000 0.08319 0.04810 = 0.04547 0.00308 0.00007 -0.01366 N39 3 0.457251 0.903297 0.524179 11.00000 0.07753 0.06188 = 0.04136 -0.00117 0.00228 0.00334 AFIX 43 H39 1 0.424096 0.944394 0.524136 11.00000 -1.20000 AFIX 0 N40 3 0.456626 0.892314 0.608262 11.00000 0.06601 0.05491 = 0.05001 -0.01208 0.00666 -0.01615 N41 3 0.484819 0.845546 0.646393 11.00000 0.08978 0.06339 = 0.02987 0.00788 0.00152 -0.02268 N42 3 0.551244 0.753062 0.718550 11.00000 0.10711 0.06919 = 0.02371 0.00415 -0.01035 -0.04182 N43 3 0.770838 0.805329 0.398332 11.00000 0.07271 0.09684 = 0.06046 0.00738 0.00034 -0.02992 N44 3 0.781330 0.877424 0.472652 11.00000 0.08793 0.06426 = 0.07442 0.01398 -0.02373 -0.03376 N45 3 0.785832 0.907557 0.512750 11.00000 0.11985 0.07140 = 0.03948 0.00652 -0.00213 -0.04366 N46 3 0.786459 0.896643 0.599011 11.00000 0.09205 0.04415 = 0.06720 0.01958 -0.00756 -0.01327 AFIX 43 H46 1 0.790299 0.938622 0.602054 11.00000 -1.20000 AFIX 0 N47 3 0.784152 0.846173 0.637319 11.00000 0.08965 0.04525 = 0.05870 0.00587 -0.00366 -0.02627 N48 3 0.770092 0.755002 0.711484 11.00000 0.08700 0.04241 = 0.06154 -0.00031 -0.01678 0.00144 N49 3 0.472124 0.715629 0.481825 11.00000 0.11865 0.07781 = 0.01690 -0.00917 0.00376 -0.04900 N50 3 0.595754 0.645177 0.448351 11.00000 0.08740 0.05935 = 0.02839 -0.00219 0.00323 -0.01848 N51 3 0.664259 0.608881 0.435059 11.00000 0.08402 0.07388 = 0.03561 -0.00386 -0.00309 -0.02053 N52 3 0.779431 0.606679 0.433323 11.00000 0.06970 0.06617 = 0.06825 -0.02512 0.00300 -0.00773 N53 3 0.823154 0.645790 0.443112 11.00000 0.08885 0.07689 = 0.04618 -0.00409 -0.00613 -0.01697 N54 3 0.900087 0.717758 0.471022 11.00000 0.09928 0.09471 = 0.08723 0.01614 -0.00646 -0.04279 N55 3 0.470907 0.690146 0.639318 11.00000 0.08457 0.07018 = 0.04858 0.02456 -0.02374 -0.04403 N56 3 0.599079 0.607622 0.666205 11.00000 0.08996 0.05519 = 0.02738 0.00825 -0.00136 -0.02613 N57 3 0.663951 0.566382 0.676989 11.00000 0.07472 0.06308 = 0.05372 0.00645 -0.00216 -0.01787 N58 3 0.779523 0.570652 0.676769 11.00000 0.06335 0.06944 = 0.06108 -0.00203 0.00258 -0.01727 N59 3 0.822448 0.611543 0.662065 11.00000 0.08682 0.06349 = 0.03871 -0.00161 0.00713 -0.01846 N60 3 0.897720 0.698278 0.632191 11.00000 0.07356 0.06421 = 0.10265 -0.00323 0.00437 -0.01117 N61 3 0.588227 0.658652 0.559372 11.00000 0.10052 0.03013 = 0.05699 -0.00104 -0.00788 -0.01441 N62 3 0.572173 0.605510 0.557693 11.00000 0.10654 0.05511 = 0.03447 0.01338 0.01250 -0.01172 N63 3 0.561949 0.551907 0.557526 11.00000 0.12985 0.05552 = 0.07008 0.00964 -0.01350 -0.04003 N64 3 0.811461 0.659200 0.554113 11.00000 0.08466 0.06899 = 0.04319 -0.01227 0.00251 -0.01182 N65 3 0.859194 0.605692 0.554005 11.00000 0.08928 0.06157 = 0.05170 -0.00392 -0.00947 0.00738 N66 3 0.904717 0.554096 0.551933 11.00000 0.09759 0.09379 = 0.05608 -0.00214 -0.01222 0.01497 N67 3 0.648856 0.837573 0.479985 11.00000 0.07556 0.07099 = 0.10289 -0.05652 0.04020 -0.04919 N68 3 0.630871 0.897922 0.460355 11.00000 0.09172 0.03253 = 0.09621 0.00133 0.00639 -0.01241 N69 3 0.612575 0.955437 0.439004 11.00000 0.09480 0.03903 = 0.21113 0.01586 0.02349 -0.00998 N70 3 0.649938 0.809615 0.640097 11.00000 0.07589 0.04319 = 0.04025 0.01594 -0.02975 -0.02682 N71 3 0.629372 0.864975 0.664147 11.00000 0.08456 0.06269 = 0.06880 0.01533 -0.02138 -0.02205 N72 3 0.614586 0.912855 0.689124 11.00000 0.10581 0.05368 = 0.07959 -0.02352 -0.00336 -0.00642 C1 5 0.255071 0.715846 -0.050139 11.00000 0.07901 0.07175 = 0.05071 0.01682 -0.02402 -0.02878 AFIX 43 H1 1 0.253239 0.763833 -0.056610 11.00000 -1.20000 AFIX 0 C2 5 0.272205 0.673723 -0.090346 11.00000 0.09193 0.12523 = 0.05847 -0.01881 -0.00962 -0.03110 AFIX 43 H2 1 0.289793 0.688725 -0.121162 11.00000 -1.20000 AFIX 0 C3 5 0.260876 0.607356 -0.080678 11.00000 0.15104 0.07679 = 0.04092 -0.02262 -0.00614 -0.00146 AFIX 43 H3 1 0.264882 0.577300 -0.106191 11.00000 -1.20000 AFIX 0 C4 5 0.245232 0.589347 -0.036925 11.00000 0.09868 0.09040 = 0.07154 -0.01270 -0.01159 -0.02375 AFIX 43 H4A 1 0.239118 0.544103 -0.030240 11.00000 -1.20000 AFIX 0 C5 5 0.236135 0.632075 0.003016 11.00000 0.07497 0.06363 = 0.07024 0.00788 -0.02165 -0.02341 C6 5 0.218514 0.604521 0.051842 11.00000 0.06682 0.06989 = 0.08449 -0.00645 -0.00949 -0.01827 C7 5 0.213943 0.531308 0.066054 11.00000 0.14686 0.07763 = 0.09769 -0.02517 -0.00052 -0.05361 AFIX 137 H7A 1 0.227219 0.517367 0.100442 11.00000 -1.50000 H7B 1 0.246416 0.498174 0.044844 11.00000 -1.50000 H7C 1 0.165225 0.530827 0.062108 11.00000 -1.50000 AFIX 0 C8 5 0.188066 0.676546 0.161186 11.00000 0.07337 0.07896 = 0.06049 -0.00853 0.00336 -0.02472 C9 5 0.160874 0.640219 0.310167 11.00000 0.21351 0.11566 = 0.05493 0.00696 0.05292 -0.09093 AFIX 137 H9A 1 0.123802 0.627324 0.294629 11.00000 -1.50000 H9B 1 0.148493 0.645565 0.345098 11.00000 -1.50000 H9C 1 0.206367 0.603186 0.306936 11.00000 -1.50000 AFIX 0 C10 5 0.167083 0.710144 0.284820 11.00000 0.10557 0.08835 = 0.03914 0.01224 0.02622 -0.02622 C11 5 0.167566 0.767066 0.311366 11.00000 0.10223 0.09147 = 0.04188 -0.01177 0.01259 -0.01673 C12 5 0.169616 0.761098 0.360804 11.00000 0.21616 0.11689 = 0.06262 -0.01778 0.02344 -0.04788 AFIX 43 H12 1 0.170022 0.718542 0.379691 11.00000 -1.20000 AFIX 0 C13 5 0.171168 0.822473 0.383756 11.00000 0.18258 0.10321 = 0.06151 -0.00845 0.03117 -0.05985 AFIX 43 H13 1 0.173496 0.820343 0.418529 11.00000 -1.20000 AFIX 0 C14 5 0.169357 0.882526 0.356479 11.00000 0.16440 0.10056 = 0.05023 -0.01943 0.01494 -0.04497 AFIX 43 H14 1 0.169979 0.922575 0.372157 11.00000 -1.20000 AFIX 0 C15 5 0.166651 0.886531 0.306799 11.00000 0.09881 0.08184 = 0.07524 -0.02550 0.01414 -0.03920 AFIX 43 H15 1 0.164233 0.929585 0.287882 11.00000 -1.20000 AFIX 0 C16 5 0.439202 0.714733 -0.047046 11.00000 0.05172 0.05323 = 0.07319 -0.00516 0.01015 -0.01799 AFIX 43 H16 1 0.409064 0.761106 -0.055493 11.00000 -1.20000 AFIX 0 C17 5 0.462026 0.667801 -0.082920 11.00000 0.10242 0.07237 = 0.03988 -0.01262 0.00415 -0.01957 AFIX 43 H17 1 0.438996 0.678485 -0.113575 11.00000 -1.20000 AFIX 0 C18 5 0.513097 0.610582 -0.076061 11.00000 0.09828 0.10046 = 0.08165 -0.03112 0.02187 -0.00856 AFIX 43 H18 1 0.535798 0.584818 -0.102939 11.00000 -1.20000 AFIX 0 C19 5 0.534420 0.587189 -0.028233 11.00000 0.12024 0.09107 = 0.05673 -0.00465 0.02745 -0.02326 AFIX 43 H19 1 0.567859 0.541973 -0.021492 11.00000 -1.20000 AFIX 0 C20 5 0.506302 0.630788 0.010754 11.00000 0.07234 0.06274 = 0.05849 -0.01758 0.00630 -0.02422 C21 5 0.527846 0.610108 0.060845 11.00000 0.08175 0.05364 = 0.06546 -0.00094 0.00336 -0.01129 C22 5 0.577542 0.534230 0.076720 11.00000 0.13112 0.04517 = 0.12070 0.00537 -0.02260 0.01030 AFIX 137 H22A 1 0.624840 0.527873 0.061462 11.00000 -1.50000 H22B 1 0.557600 0.499173 0.066019 11.00000 -1.50000 H22C 1 0.581243 0.528225 0.112601 11.00000 -1.50000 AFIX 0 C23 5 0.488337 0.688387 0.165531 11.00000 0.09034 0.04558 = 0.03939 0.02086 -0.02606 -0.01793 C24 5 0.499768 0.668282 0.317315 11.00000 0.10820 0.05854 = 0.06187 0.01382 -0.01730 -0.01552 AFIX 137 H24A 1 0.511159 0.626833 0.298508 11.00000 -1.50000 H24B 1 0.471421 0.661148 0.346789 11.00000 -1.50000 H24C 1 0.543854 0.675185 0.327046 11.00000 -1.50000 AFIX 0 C25 5 0.459183 0.730633 0.286803 11.00000 0.06839 0.06655 = 0.03698 0.01331 -0.00816 -0.02289 C26 5 0.413397 0.791596 0.310758 11.00000 0.08492 0.07746 = 0.06302 0.01820 -0.01558 -0.03370 C27 5 0.402587 0.794644 0.361473 11.00000 0.09695 0.08021 = 0.03507 0.02548 -0.01538 -0.02269 AFIX 43 H27 1 0.427138 0.755430 0.382956 11.00000 -1.20000 AFIX 0 C28 5 0.358238 0.851809 0.380521 11.00000 0.10390 0.08804 = 0.03460 -0.00177 -0.00824 -0.02986 AFIX 43 H28 1 0.346858 0.850547 0.414771 11.00000 -1.20000 AFIX 0 C29 5 0.329242 0.912143 0.350659 11.00000 0.10148 0.10000 = 0.04273 0.02026 -0.00194 -0.03517 AFIX 43 H29 1 0.300554 0.954578 0.363314 11.00000 -1.20000 AFIX 0 C30 5 0.344291 0.907112 0.301893 11.00000 0.07315 0.06083 = 0.06625 0.00876 0.00162 -0.01260 AFIX 43 H30 1 0.325386 0.948742 0.280844 11.00000 -1.20000 AFIX 0 C31 5 0.047535 0.763668 0.068032 11.00000 0.04600 0.05272 = 0.07785 0.03810 -0.00924 -0.02590 AFIX 43 H31 1 0.067721 0.723405 0.090007 11.00000 -1.20000 AFIX 0 C32 5 -0.024152 0.784138 0.062089 11.00000 0.05345 0.13832 = 0.09201 0.03739 -0.01653 -0.03221 AFIX 43 H32 1 -0.054510 0.761476 0.080148 11.00000 -1.20000 AFIX 0 C33 5 -0.048500 0.840024 0.027933 11.00000 0.09336 0.11073 = 0.08941 -0.00178 -0.03716 0.01008 AFIX 43 H33 1 -0.098233 0.860678 0.024188 11.00000 -1.20000 AFIX 0 C34 5 0.000463 0.868748 -0.003022 11.00000 0.08265 0.12424 = 0.07773 -0.00452 -0.03869 -0.00380 AFIX 43 H34 1 -0.016024 0.899941 -0.031347 11.00000 -1.20000 AFIX 0 C35 5 0.072536 0.849505 0.009753 11.00000 0.06640 0.06196 = 0.06772 0.00633 -0.00492 -0.01469 C36 5 0.118255 0.884887 -0.017273 11.00000 0.08273 0.06405 = 0.04861 0.01381 -0.00509 -0.01203 C37 5 0.089172 0.945469 -0.054898 11.00000 0.10257 0.11339 = 0.05515 0.01791 -0.00448 -0.00088 AFIX 137 H37A 1 0.121684 0.973940 -0.059700 11.00000 -1.50000 H37B 1 0.042585 0.974630 -0.043466 11.00000 -1.50000 H37C 1 0.084241 0.927431 -0.086120 11.00000 -1.50000 AFIX 0 C38 5 0.295770 0.865939 -0.009465 11.00000 0.07622 0.05714 = 0.04167 0.00588 0.00332 0.01040 C39 5 0.456344 0.942279 -0.053874 11.00000 0.11019 0.10897 = 0.07921 0.04186 -0.00655 -0.04477 AFIX 137 H39A 1 0.406790 0.970333 -0.059409 11.00000 -1.50000 H39B 1 0.478523 0.924026 -0.084787 11.00000 -1.50000 H39C 1 0.482088 0.971916 -0.042078 11.00000 -1.50000 AFIX 0 C40 5 0.458848 0.881824 -0.016083 11.00000 0.07319 0.05615 = 0.04767 0.00607 0.01037 -0.00825 C41 5 0.524033 0.851805 0.013589 11.00000 0.08230 0.04681 = 0.04636 -0.00035 0.00243 -0.02648 C42 5 0.582100 0.873214 0.002099 11.00000 0.07892 0.05556 = 0.11497 -0.00468 0.02904 -0.02030 AFIX 43 H42 1 0.581876 0.907084 -0.024856 11.00000 -1.20000 AFIX 0 C43 5 0.647093 0.842041 0.033080 11.00000 0.07739 0.10155 = 0.08126 0.00830 0.01103 -0.03289 AFIX 43 H43 1 0.686962 0.858766 0.026800 11.00000 -1.20000 AFIX 0 C44 5 0.649424 0.789762 0.070277 11.00000 0.08443 0.10574 = 0.08008 -0.00124 0.01764 -0.05706 AFIX 43 H44 1 0.688301 0.769597 0.091467 11.00000 -1.20000 AFIX 0 C45 5 0.589537 0.770786 0.072838 11.00000 0.03575 0.05441 = 0.04629 0.01495 -0.01217 -0.01110 AFIX 43 H45 1 0.590275 0.732147 0.096177 11.00000 -1.20000 AFIX 0 C46 5 0.016729 0.816841 0.193120 11.00000 0.05740 0.07414 = 0.07737 0.01043 -0.00918 -0.04822 AFIX 43 H46A 1 0.040599 0.767796 0.192889 11.00000 -1.20000 AFIX 0 C47 5 -0.055501 0.839020 0.192340 11.00000 0.04236 0.13634 = 0.10451 -0.00904 -0.00290 -0.03876 AFIX 43 H47 1 -0.078353 0.803782 0.192106 11.00000 -1.20000 AFIX 0 C48 5 -0.089920 0.894039 0.191955 11.00000 0.07389 0.16183 = 0.06490 0.00888 0.00031 -0.01545 AFIX 43 H48 1 -0.140165 0.905544 0.191467 11.00000 -1.20000 AFIX 0 C49 5 -0.054718 0.949478 0.192227 11.00000 0.07476 0.14596 = 0.08762 -0.02308 -0.01018 -0.01526 AFIX 43 H49 1 -0.082045 0.997809 0.188954 11.00000 -1.20000 AFIX 0 C50 5 0.020118 0.929954 0.197409 11.00000 0.10604 0.08024 = 0.05149 0.00311 0.00435 -0.03374 C51 5 0.057688 0.978790 0.197074 11.00000 0.07585 0.08624 = 0.05996 0.00095 -0.00661 0.00525 C52 5 0.021626 1.059224 0.196006 11.00000 0.13733 0.07174 = 0.25634 -0.04055 -0.01767 0.06133 AFIX 137 H52A 1 0.017392 1.079769 0.161819 11.00000 -1.50000 H52B 1 0.050379 1.080238 0.213872 11.00000 -1.50000 H52C 1 -0.025760 1.068668 0.211651 11.00000 -1.50000 AFIX 0 C53 5 0.236459 0.970675 0.194158 11.00000 0.06998 0.04973 = 0.03595 -0.00072 -0.00600 -0.00690 C54 5 0.376351 1.079420 0.178367 11.00000 0.12092 0.06306 = 0.07172 -0.01513 0.02636 -0.04997 AFIX 137 H54A 1 0.324536 1.099438 0.180429 11.00000 -1.50000 H54B 1 0.393894 1.094062 0.146127 11.00000 -1.50000 H54C 1 0.397551 1.096283 0.204276 11.00000 -1.50000 AFIX 0 C55 5 0.397559 0.995841 0.185289 11.00000 0.10476 0.08710 = 0.03255 -0.00952 0.00591 -0.04445 C56 5 0.471561 0.950666 0.184991 11.00000 0.08174 0.08943 = 0.04080 0.01136 -0.01307 -0.02409 C57 5 0.525892 0.980472 0.183151 11.00000 0.12299 0.10184 = 0.04174 -0.01010 -0.00703 -0.06108 AFIX 43 H57 1 0.514883 1.030257 0.181631 11.00000 -1.20000 AFIX 0 C58 5 0.594319 0.940005 0.183480 11.00000 0.06982 0.10054 = 0.04966 0.00827 -0.00963 -0.03083 AFIX 43 H58 1 0.632516 0.959210 0.183869 11.00000 -1.20000 AFIX 0 C59 5 0.604896 0.869124 0.183213 11.00000 0.08600 0.13117 = 0.05338 -0.00565 0.00230 -0.04607 AFIX 43 H59 1 0.652111 0.839470 0.178400 11.00000 -1.20000 AFIX 0 C60 5 0.554466 0.839729 0.189126 11.00000 0.04434 0.03472 = 0.06185 -0.01292 -0.00504 -0.00721 AFIX 43 H60 1 0.566028 0.789863 0.193328 11.00000 -1.20000 AFIX 0 C61 5 0.587309 0.778635 0.365565 11.00000 0.05371 0.05022 = 0.04760 -0.00735 -0.00131 -0.01231 AFIX 43 H61 1 0.613755 0.730222 0.370887 11.00000 -1.20000 AFIX 0 C62 5 0.586861 0.807192 0.320170 11.00000 0.05622 0.08323 = 0.08294 -0.00168 -0.01675 -0.02599 AFIX 43 H62 1 0.616035 0.782257 0.294970 11.00000 -1.20000 AFIX 0 C63 5 0.540773 0.877185 0.310255 11.00000 0.08641 0.05436 = 0.07246 0.01602 -0.01535 -0.01877 AFIX 43 H63 1 0.536058 0.899185 0.277657 11.00000 -1.20000 AFIX 0 C64 5 0.503676 0.911829 0.348441 11.00000 0.07566 0.08157 = 0.04960 0.01167 -0.00678 -0.02567 AFIX 43 H64 1 0.473221 0.958776 0.342868 11.00000 -1.20000 AFIX 0 C65 5 0.510842 0.877274 0.396667 11.00000 0.09482 0.05608 = 0.02735 0.00657 -0.01587 -0.02440 C66 5 0.474413 0.910993 0.439844 11.00000 0.08253 0.05830 = 0.05134 0.01443 0.00216 -0.02613 C67 5 0.424485 0.986212 0.435706 11.00000 0.06807 0.05866 = 0.08593 0.00381 0.00337 -0.00262 AFIX 137 H67A 1 0.375913 0.985644 0.431275 11.00000 -1.50000 H67B 1 0.439258 1.012939 0.407393 11.00000 -1.50000 H67C 1 0.426149 1.008467 0.465786 11.00000 -1.50000 AFIX 0 C68 5 0.481691 0.862587 0.567398 11.00000 0.06866 0.05231 = 0.05411 0.01256 -0.00547 -0.02037 C69 5 0.421614 0.936137 0.700215 11.00000 0.06861 0.08482 = 0.06728 -0.01502 0.02510 -0.01980 AFIX 137 H69A 1 0.401858 0.960794 0.668970 11.00000 -1.50000 H69B 1 0.448823 0.962586 0.714317 11.00000 -1.50000 H69C 1 0.382855 0.932270 0.723124 11.00000 -1.50000 AFIX 0 C70 5 0.470563 0.862277 0.691202 11.00000 0.09269 0.07301 = 0.05052 -0.02007 0.02089 -0.03468 C71 5 0.504219 0.813343 0.730047 11.00000 0.09256 0.07282 = 0.04025 -0.00755 -0.00084 -0.04836 C72 5 0.487585 0.830488 0.779991 11.00000 0.13598 0.07564 = 0.04819 -0.00584 0.00595 -0.04956 AFIX 43 H72 1 0.454619 0.873781 0.788327 11.00000 -1.20000 AFIX 0 C73 5 0.523810 0.778339 0.815364 11.00000 0.16174 0.08023 = 0.01673 -0.00703 0.01192 -0.04753 AFIX 43 H73 1 0.513990 0.785645 0.849187 11.00000 -1.20000 AFIX 0 C74 5 0.570875 0.719692 0.803459 11.00000 0.13588 0.09398 = 0.04957 0.00524 0.00847 -0.04402 AFIX 43 H74 1 0.598501 0.687114 0.827828 11.00000 -1.20000 AFIX 0 C75 5 0.579237 0.706454 0.753534 11.00000 0.09406 0.10969 = 0.07488 -0.00726 0.00601 -0.06225 AFIX 43 H75 1 0.606897 0.660887 0.745241 11.00000 -1.20000 AFIX 0 C76 5 0.769469 0.771437 0.361589 11.00000 0.07813 0.05632 = 0.04704 -0.00538 -0.00068 -0.01150 AFIX 43 H76 1 0.774113 0.722747 0.367817 11.00000 -1.20000 AFIX 0 C77 5 0.761874 0.799563 0.314135 11.00000 0.10897 0.11397 = 0.14143 -0.02306 -0.00622 -0.05797 AFIX 43 H77 1 0.754955 0.773479 0.288689 11.00000 -1.20000 AFIX 0 C78 5 0.764561 0.865894 0.304688 11.00000 0.13856 0.11827 = 0.09936 0.03417 0.01038 -0.05105 AFIX 43 H78 1 0.763341 0.886077 0.271664 11.00000 -1.20000 AFIX 0 C79 5 0.768927 0.903533 0.341343 11.00000 0.11906 0.09158 = 0.08595 -0.00450 -0.01292 -0.05066 AFIX 43 H79 1 0.767081 0.951543 0.335032 11.00000 -1.20000 AFIX 0 C80 5 0.776156 0.871407 0.388471 11.00000 0.08667 0.09786 = 0.07209 0.00298 0.01125 -0.04052 C81 5 0.779817 0.911796 0.428331 11.00000 0.13332 0.09519 = 0.06707 0.01549 -0.00589 -0.08028 C82 5 0.776068 0.988579 0.424065 11.00000 0.33735 0.17177 = 0.03177 0.03059 -0.02397 -0.19330 AFIX 137 H82A 1 0.738716 1.014011 0.446500 11.00000 -1.50000 H82B 1 0.765223 1.008745 0.390196 11.00000 -1.50000 H82C 1 0.821831 0.992805 0.432731 11.00000 -1.50000 AFIX 0 C83 5 0.781847 0.870345 0.557038 11.00000 0.07616 0.07745 = 0.08223 0.01811 0.01710 -0.04529 C84 5 0.815314 0.925376 0.690910 11.00000 0.10289 0.05604 = 0.08868 -0.01986 -0.02199 -0.01059 AFIX 137 H84A 1 0.816481 0.955688 0.660644 11.00000 -1.50000 H84B 1 0.862503 0.909052 0.705245 11.00000 -1.50000 H84C 1 0.780753 0.952077 0.714444 11.00000 -1.50000 AFIX 0 C85 5 0.793860 0.862095 0.679088 11.00000 0.10604 0.04772 = 0.09035 -0.01351 0.01976 -0.01731 C86 5 0.785824 0.813034 0.722107 11.00000 0.08032 0.05904 = 0.05956 0.00472 -0.01407 -0.01301 C87 5 0.795163 0.822063 0.770294 11.00000 0.13406 0.05825 = 0.07467 -0.01593 -0.01127 -0.02802 AFIX 43 H87 1 0.809768 0.860841 0.777529 11.00000 -1.20000 AFIX 0 C88 5 0.783106 0.773505 0.810037 11.00000 0.15417 0.09594 = 0.06835 -0.00781 -0.03036 -0.05137 AFIX 43 H88 1 0.786982 0.780811 0.843454 11.00000 -1.20000 AFIX 0 C89 5 0.765977 0.716924 0.797472 11.00000 0.09322 0.08499 = 0.04602 0.00446 0.00298 -0.00494 AFIX 43 H89 1 0.754885 0.684666 0.822053 11.00000 -1.20000 AFIX 0 C90 5 0.765059 0.707458 0.748770 11.00000 0.06032 0.04713 = 0.08286 -0.00537 -0.00461 -0.01710 AFIX 43 H90 1 0.760529 0.664083 0.740584 11.00000 -1.20000 AFIX 0 C91 5 0.400374 0.753470 0.496627 11.00000 0.03355 0.04983 = 0.05552 0.00045 0.00473 -0.00369 AFIX 43 H91 1 0.393795 0.796393 0.510989 11.00000 -1.20000 AFIX 0 C92 5 0.343934 0.734736 0.492284 11.00000 0.06379 0.10165 = 0.07192 -0.00507 0.00801 -0.04318 AFIX 43 H92 1 0.297701 0.763330 0.501097 11.00000 -1.20000 AFIX 0 C93 5 0.355615 0.673156 0.474756 11.00000 0.06506 0.11634 = 0.12383 -0.04166 0.00356 -0.02689 AFIX 43 H93 1 0.316074 0.656017 0.473801 11.00000 -1.20000 AFIX 0 C94 5 0.415459 0.634364 0.458901 11.00000 0.09718 0.06685 = 0.10335 0.00460 -0.01306 -0.04441 AFIX 43 H94 1 0.417864 0.591962 0.445111 11.00000 -1.20000 AFIX 0 C95 5 0.478812 0.653623 0.461542 11.00000 0.09903 0.05968 = 0.05309 -0.00262 -0.01688 -0.03435 C96 5 0.548796 0.615734 0.446647 11.00000 0.10273 0.05845 = 0.03201 0.01126 -0.00720 -0.04107 C97 5 0.563220 0.540173 0.429761 11.00000 0.14122 0.06765 = 0.05645 -0.01418 -0.01190 -0.00037 AFIX 137 H97A 1 0.598651 0.532820 0.402697 11.00000 -1.50000 H97B 1 0.518981 0.535227 0.418596 11.00000 -1.50000 H97C 1 0.581071 0.505093 0.457401 11.00000 -1.50000 AFIX 0 C98 5 0.713801 0.636696 0.443255 11.00000 0.08295 0.05089 = 0.05271 -0.00385 0.00901 -0.01371 C99 5 0.922793 0.541472 0.425099 11.00000 0.07071 0.11460 = 0.11095 -0.03500 -0.00305 0.01364 AFIX 137 H99A 1 0.884624 0.520632 0.422256 11.00000 -1.50000 H99B 1 0.956907 0.512172 0.449136 11.00000 -1.50000 H99C 1 0.947003 0.544135 0.393023 11.00000 -1.50000 AFIX 0 C100 5 0.891888 0.614275 0.441788 11.00000 0.05604 0.09082 = 0.07792 0.01397 0.00422 0.00166 C101 5 0.933761 0.655015 0.455150 11.00000 0.06592 0.11126 = 0.07530 -0.02200 -0.02175 -0.02080 C102 5 1.006442 0.632083 0.448740 11.00000 0.06633 0.12522 = 0.11176 0.03621 0.00716 -0.00091 AFIX 43 H102 1 1.030198 0.589335 0.434499 11.00000 -1.20000 AFIX 0 C103 5 1.044636 0.676162 0.464710 11.00000 0.07516 0.09954 = 0.14099 0.01285 -0.00874 -0.03646 AFIX 43 H103 1 1.095068 0.659781 0.462943 11.00000 -1.20000 AFIX 0 C104 5 1.015136 0.734932 0.480815 11.00000 0.08780 0.09970 = 0.09405 0.00909 -0.00453 -0.04649 AFIX 43 H104 1 1.041932 0.763497 0.489930 11.00000 -1.20000 AFIX 0 C105 5 0.946544 0.754916 0.484459 11.00000 0.05573 0.05300 = 0.06671 0.00180 -0.00789 -0.02892 AFIX 43 H105 1 0.924584 0.799003 0.497449 11.00000 -1.20000 AFIX 0 C106 5 0.401472 0.729195 0.629377 11.00000 0.04572 0.05090 = 0.04679 -0.00516 -0.01405 -0.01247 AFIX 43 H106 1 0.393296 0.778223 0.621301 11.00000 -1.20000 AFIX 0 C107 5 0.345464 0.707540 0.629621 11.00000 0.08757 0.13404 = 0.07070 -0.01541 0.00564 -0.05232 AFIX 43 H107 1 0.300431 0.738150 0.619575 11.00000 -1.20000 AFIX 0 C108 5 0.355795 0.637705 0.645321 11.00000 0.11882 0.09383 = 0.04904 0.00780 -0.00999 -0.03416 AFIX 43 H108 1 0.317958 0.617837 0.645887 11.00000 -1.20000 AFIX 0 C109 5 0.418964 0.599646 0.659382 11.00000 0.09661 0.07179 = 0.05403 0.00414 0.00300 -0.02825 AFIX 43 H109 1 0.424539 0.552264 0.671681 11.00000 -1.20000 AFIX 0 C110 5 0.479433 0.622173 0.658033 11.00000 0.10592 0.10120 = 0.02898 -0.01432 0.00728 -0.04495 C111 5 0.549998 0.578600 0.668767 11.00000 0.08915 0.04812 = 0.06084 0.00378 -0.00385 -0.01517 C112 5 0.562311 0.501456 0.683233 11.00000 0.11093 0.06755 = 0.06309 0.01446 0.01381 -0.04662 AFIX 137 H11A 1 0.558969 0.477735 0.654188 11.00000 -1.50000 H11B 1 0.526324 0.495635 0.707974 11.00000 -1.50000 H11C 1 0.609664 0.480722 0.696965 11.00000 -1.50000 AFIX 0 C113 5 0.713786 0.603342 0.667371 11.00000 0.08876 0.04892 = 0.03960 0.00424 -0.00130 0.00232 C114 5 0.921925 0.508959 0.682843 11.00000 0.09217 0.05749 = 0.11366 0.01848 -0.00637 -0.01223 AFIX 137 H11D 1 0.902987 0.497921 0.715496 11.00000 -1.50000 H11E 1 0.973659 0.497588 0.683976 11.00000 -1.50000 H11F 1 0.910003 0.481102 0.659061 11.00000 -1.50000 AFIX 0 C115 5 0.889258 0.587621 0.667186 11.00000 0.09064 0.06755 = 0.05921 0.01061 0.00104 -0.01795 C116 5 0.929909 0.630464 0.651906 11.00000 0.05620 0.07474 = 0.11636 -0.01055 0.00592 -0.00954 C117 5 1.004251 0.611829 0.654900 11.00000 0.06185 0.10430 = 0.12454 0.05809 -0.03002 -0.05074 AFIX 43 H117 1 1.029486 0.566735 0.669811 11.00000 -1.20000 AFIX 0 C118 5 1.041247 0.657031 0.636865 11.00000 0.08437 0.11156 = 0.13962 -0.02039 -0.01306 -0.02343 AFIX 43 H118 1 1.091575 0.641119 0.638459 11.00000 -1.20000 AFIX 0 C119 5 1.011289 0.719334 0.618083 11.00000 0.06003 0.07848 = 0.10416 -0.00185 0.03279 -0.02288 AFIX 43 H119 1 1.037601 0.750038 0.605663 11.00000 -1.20000 AFIX 0 C120 5 0.944796 0.737507 0.617053 11.00000 0.05884 0.04778 = 0.06585 0.01373 -0.00710 -0.03639 AFIX 43 H120 1 0.922719 0.784644 0.604192 11.00000 -1.20000 HKLF 4 REM _2 REM R1 = 0.1146 for 24602 Fo > 4sig(Fo) and 0.1357 for all 40060 data REM 1907 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 7.672, deepest hole -3.938, 1-sigma level 0.257 Q1 1 0.1373 0.6910 0.0625 11.00000 0.05 7.67 Q2 1 0.1110 0.7521 0.1859 11.00000 0.05 7.03 Q3 1 0.8440 0.8058 0.6308 11.00000 0.05 6.73 Q4 1 0.8437 0.8287 0.4959 11.00000 0.05 5.86 Q5 1 0.2920 0.7617 0.1819 11.00000 0.05 5.12 Q6 1 0.3203 0.6984 0.0597 11.00000 0.05 4.66 Q7 1 0.4963 0.8389 0.0678 11.00000 0.05 4.24 Q8 1 0.6615 0.8204 0.4991 11.00000 0.05 4.14 Q9 1 0.4986 0.6808 0.4884 11.00000 0.05 3.76 Q10 1 0.4938 0.6600 0.6240 11.00000 0.05 3.71 Q11 1 0.4607 0.9018 0.1937 11.00000 0.05 3.16 Q12 1 0.6798 0.6674 0.6196 11.00000 0.05 2.10 Q13 1 0.3111 0.8335 0.0686 11.00000 0.05 2.09 Q14 1 0.2752 0.8918 0.1946 11.00000 0.05 1.94 Q15 1 0.8075 0.7910 0.4902 11.00000 0.05 1.74 Q16 1 0.6856 0.6910 0.4777 11.00000 0.05 1.62 Q17 1 0.7952 0.6957 0.3729 11.00000 0.05 1.61 Q18 1 0.6170 0.6582 0.5063 11.00000 0.05 1.53 Q19 1 0.3061 0.7794 0.0398 11.00000 0.05 1.37 Q20 1 0.5337 0.7313 0.4916 11.00000 0.05 1.35 Q21 1 0.7985 0.6694 0.5057 11.00000 0.05 1.28 Q22 1 0.1445 0.8040 0.1880 11.00000 0.05 1.26 Q23 1 0.8011 0.7670 0.6261 11.00000 0.05 1.26 Q24 1 0.6800 0.6989 0.6471 11.00000 0.05 1.24 Q25 1 0.3801 0.8511 0.0499 11.00000 0.05 1.23 Q26 1 0.5145 0.7141 0.6375 11.00000 0.05 1.20 Q27 1 0.6253 0.7785 0.4952 11.00000 0.05 1.20 Q28 1 0.3242 0.8205 0.1862 11.00000 0.05 1.19 Q29 1 0.7412 0.8034 0.6163 11.00000 0.05 1.17 Q30 1 0.1978 0.8393 0.0563 11.00000 0.05 1.17 Q31 1 0.6134 0.6878 0.3710 11.00000 0.05 1.13 Q32 1 0.4615 0.7897 0.0717 11.00000 0.05 1.13 Q33 1 0.2218 0.7538 0.2029 11.00000 0.05 1.11 Q34 1 0.1171 0.7761 0.0463 11.00000 0.05 1.10 Q35 1 0.5433 0.8172 0.6113 11.00000 0.05 1.09 Q36 1 0.4197 0.7858 -0.0688 11.00000 0.05 1.06 Q37 1 0.7268 0.7994 0.7462 11.00000 0.05 1.04 Q38 1 0.5004 0.7047 0.6486 11.00000 0.05 1.03 Q39 1 0.6971 0.7440 0.5086 11.00000 0.05 1.01 Q40 1 0.4212 0.8578 0.1941 11.00000 0.05 1.00 Q41 1 0.5449 0.7938 0.7484 11.00000 0.05 0.99 Q42 1 0.4037 0.7533 0.2026 11.00000 0.05 0.99 Q43 1 0.6537 0.6351 0.6486 11.00000 0.05 0.97 Q44 1 0.0603 0.2874 0.9441 11.00000 0.05 0.94 Q45 1 0.5156 0.8552 0.2003 11.00000 0.05 0.93 Q46 1 0.5457 0.7220 0.4605 11.00000 0.05 0.93 Q47 1 0.8294 0.7400 0.5760 11.00000 0.05 0.90 Q48 1 0.4472 0.8459 0.1695 11.00000 0.05 0.90 Q49 1 0.6765 0.6689 0.5218 11.00000 0.05 0.88 Q50 1 0.5624 0.7729 0.0682 11.00000 0.05 0.87 Q51 1 0.6033 0.6434 0.4628 11.00000 0.05 0.86 Q52 1 0.6940 0.7661 0.4732 11.00000 0.05 0.84 Q53 1 0.0126 0.7167 0.0660 11.00000 0.05 0.84 Q54 1 0.0988 0.7813 -0.0044 11.00000 0.05 0.84 Q55 1 0.7152 0.7123 0.6156 11.00000 0.05 0.84 Q56 1 0.6396 0.7882 0.0595 11.00000 0.05 0.84 Q57 1 0.5308 0.7448 0.5428 11.00000 0.05 0.84 Q58 1 0.1461 0.8946 0.1843 11.00000 0.05 0.83 Q59 1 0.4984 0.8277 0.6498 11.00000 0.05 0.83 Q60 1 0.4643 0.7711 0.0278 11.00000 0.05 0.83 ; data_3 _database_code_depnum_ccdc_archive 'CCDC 856408' #TrackingRef 'Combined_CIF.cif' # start Validation Reply Form _vrf_PLAT306_3 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O9 RESPONSE: Water protons could not be located from examination of difference Fourier maps, and were therefore omitted from the model (but included in the formula for the calculation of intensive properties.) ; _vrf_PLAT041_3 ; PROBLEM: Calc. and Reported SumFormula Strings Differ ? RESPONSE: Water protons could not be located from examination of difference Fourier maps, and were therefore omitted from the model (but included in the formula for the calculation of intensive properties.) ; _vrf_PLAT042_3 ; PROBLEM: Calc. and Reported SoietyFormula Strings Differ ? RESPONSE: Water protons could not be located from examination of difference Fourier maps, and were therefore omitted from the model (but included in the formula for the calculation of intensive properties.) ; _vrf_PLAT068_3 ; PROBLEM: Reported F000 Differs from Calcd (or Missing)... ? RESPONSE: Water protons could not be located from examination of difference Fourier maps, and were therefore omitted from the model (but included in the formula for the calculation of intensive properties.) ; _vrf_PLAT311_3 ; PROBLEM: Isolated Disordered Oxygen Atom (No H's ?) ..... RESPONSE: Water protons could not be located from examination of difference Fourier maps, and were therefore omitted from the model (but included in the formula for the calculation of intensive properties.) ; _vrf_FORMU01_3 ; PROBLEM: There is a discrepancy between the atom counts in the RESPONSE: Water protons could not be located from examination of difference Fourier maps, and were therefore omitted from the model (but included in the formula for the calculation of intensive properties.) ; _vrf_CELLZ01_3 ; PROBLEM: WARNING: H atoms missing from atom site list. Is this intentional? RESPONSE: Water protons could not be located from examination of difference Fourier maps, and were therefore omitted from the model (but included in the formula for the calculation of intensive properties.) ; _vrf_PLAT002_3 ; PROBLEM: Number of Distance or Angle Restraints on AtSite 4 RESPONSE: Distance and angle restraints were applied to the nitrate anion. ; _vrf_PLAT003_3 ; PROBLEM: Number of Uiso or Uij Restrained Atom Sites .... 7 RESPONSE: SIMU restraints were applied to the nitrate anion and to a lattice solvent acetonitrile. ; _vrf_PLAT860_3 ; PROBLEM: Note: Number of Least-Squares Restraints ....... 36 RESPONSE: Distance and angle restraints were applied to the nitrate anion. SIMU restraints were applied to the nitrate anion and to a lattice solvent acetonitrile. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H59 N36 O5 Tb4, C2 H3 N, N O3, 2(H2 O)' _chemical_formula_sum 'C62 H66 N38 O10 Tb4' _chemical_formula_weight 2139.15 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' 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 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.275(3) _cell_length_b 20.969(4) _cell_length_c 26.506(5) _cell_angle_alpha 90.00 _cell_angle_beta 128.219(3) _cell_angle_gamma 90.00 _cell_volume 7543(2) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 23327 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 29.9 _exptl_crystal_description Irregular _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4176 _exptl_absorpt_coefficient_mu 3.787 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.796 _exptl_absorpt_correction_T_min 0.583 _exptl_absorpt_process_details 'T. Higashi, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 97349 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.50 _reflns_number_total 15622 _reflns_number_gt 14814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_structure_solution 'SHELXS-97: Acta Cryst.2008, A64, 112-122' _computing_structure_refinement 'SHELXL-97: Acta Cryst.2008, A64, 112-122' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' _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. Distance, angle and similarity restraints were applied to the nitrate anion. Similarity restraints were also applied to the lattice solvent acetonitrile molecule. O10 and O11 are partial occupancy, disordered lattice solvent molecules. Their occupancies were refined (summed to one), however, their corresponding H-atoms were omitted from the model as these could not be located from examination of difference Fourier maps. Please see iucr_refine_instructions_details for more information. ; _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^)+(0.1029P)^2^+39.4242P] 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 15622 _refine_ls_number_parameters 1046 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1859 _refine_ls_wR_factor_gt 0.1815 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.32241(3) 0.330451(17) 0.081686(16) 0.03882(11) Uani 1 1 d . . . Tb2 Tb 0.53284(3) 0.29809(2) 0.082004(19) 0.04818(13) Uani 1 1 d . . . Tb3 Tb 0.48814(2) 0.407345(16) 0.241394(16) 0.03524(11) Uani 1 1 d . . . Tb4 Tb 0.69763(3) 0.371423(17) 0.242273(16) 0.03729(11) Uani 1 1 d . . . O1 O 0.3818(4) 0.3447(3) 0.0244(3) 0.0448(12) Uani 1 1 d . . . O2 O 0.6204(4) 0.4536(2) 0.2543(3) 0.0387(11) Uani 1 1 d . . . O3 O 0.3680(4) 0.3287(2) 0.1841(2) 0.0401(11) Uani 1 1 d . . . O4 O 0.6664(4) 0.2801(2) 0.1850(2) 0.0391(11) Uani 1 1 d . . . O5 O 0.5077(4) 0.3561(3) 0.1623(3) 0.0621(17) Uani 1 1 d . . . O6 O 0.0601(16) 0.2287(10) 0.1281(10) 0.225(7) Uani 1 1 d DU . . O7 O 0.1403(14) 0.3150(9) 0.2057(9) 0.191(6) Uani 1 1 d DU . . O8 O 0.1459(14) 0.2303(9) 0.2515(10) 0.210(6) Uani 1 1 d DU . . O9 O 0.3137(6) 0.1666(3) 0.2803(5) 0.079(2) Uani 1 1 d . . . O10 O 0.9474(13) 0.1405(8) 0.2910(14) 0.186(14) Uani 0.66(2) 1 d P A 1 O11 O 0.971(2) 0.1822(13) 0.2270(17) 0.132(17) Uani 0.34(2) 1 d P A 2 N1 N 0.1568(5) 0.3712(3) 0.0472(3) 0.0452(15) Uani 1 1 d . . . N2 N 0.2259(5) 0.4033(3) -0.0146(3) 0.0436(14) Uani 1 1 d . . . N3 N 0.2683(5) 0.4201(3) -0.0424(3) 0.0506(16) Uani 1 1 d . . . H3 H 0.2428 0.4486 -0.0734 0.061 Uiso 1 1 calc R . . N4 N 0.4002(6) 0.4026(4) -0.0405(3) 0.0518(17) Uani 1 1 d . . . N5 N 0.4868(5) 0.3683(3) -0.0103(3) 0.0477(16) Uani 1 1 d . . . N6 N 0.6515(6) 0.3004(4) 0.0535(3) 0.0517(17) Uani 1 1 d . . . N7 N 0.3575(5) 0.4652(3) 0.2376(3) 0.0461(15) Uani 1 1 d . . . N8 N 0.4940(4) 0.5266(3) 0.2417(3) 0.0387(13) Uani 1 1 d . . . N9 N 0.5660(5) 0.5577(3) 0.2407(3) 0.0439(14) Uani 1 1 d . . . N10 N 0.6986(5) 0.5340(3) 0.2450(4) 0.0499(16) Uani 1 1 d . . . H10 H 0.7099 0.5745 0.2432 0.060 Uiso 1 1 calc R . . N11 N 0.7528(5) 0.4860(3) 0.2458(3) 0.0412(13) Uani 1 1 d . . . N12 N 0.8414(5) 0.3863(3) 0.2396(3) 0.0466(15) Uani 1 1 d . . . N13 N 0.2006(5) 0.2510(3) -0.0064(3) 0.0487(16) Uani 1 1 d . . . N14 N 0.2663(5) 0.2362(3) 0.1117(3) 0.0427(14) Uani 1 1 d . . . N15 N 0.3067(5) 0.2306(3) 0.1751(3) 0.0465(15) Uani 1 1 d . . . H15 H 0.2963 0.1974 0.1905 0.056 Uiso 1 1 calc R . . N16 N 0.4112(5) 0.2751(3) 0.2744(3) 0.0446(14) Uani 1 1 d . . . N17 N 0.4670(4) 0.3293(3) 0.3049(3) 0.0397(13) Uani 1 1 d . . . N18 N 0.5811(5) 0.4311(3) 0.3610(3) 0.0451(15) Uani 1 1 d . . . N19 N 0.4417(6) 0.2151(5) -0.0080(4) 0.064(2) Uani 1 1 d . . . N20 N 0.5985(6) 0.1853(3) 0.1106(3) 0.0493(16) Uani 1 1 d . . . N21 N 0.6781(6) 0.1730(3) 0.1733(4) 0.0495(16) Uani 1 1 d . . . N22 N 0.7821(5) 0.2189(3) 0.2723(3) 0.0460(15) Uani 1 1 d . . . N23 N 0.8006(5) 0.2750(3) 0.3039(3) 0.0417(14) Uani 1 1 d . . . N24 N 0.8338(5) 0.3869(4) 0.3622(3) 0.0480(15) Uani 1 1 d . . . N25 N 0.4285(5) 0.2396(3) 0.1030(4) 0.0504(16) Uani 1 1 d . . . N26 N 0.4167(6) 0.1836(4) 0.1040(4) 0.0561(18) Uani 1 1 d . . . N27 N 0.4071(8) 0.1305(4) 0.1053(6) 0.084(3) Uani 1 1 d . . . N28 N 0.6258(5) 0.3297(3) 0.2922(3) 0.0430(14) Uani 1 1 d . . . N29 N 0.6629(5) 0.2960(3) 0.3383(4) 0.0482(16) Uani 1 1 d . . . N30 N 0.6979(7) 0.2631(4) 0.3819(4) 0.067(2) Uani 1 1 d . . . N31 N 0.3633(5) 0.4403(3) 0.1261(3) 0.0429(14) Uani 1 1 d . . . N32 N 0.3130(5) 0.4872(3) 0.1032(3) 0.0419(14) Uani 1 1 d . . . N33 N 0.2667(5) 0.5322(4) 0.0818(3) 0.0524(17) Uani 1 1 d . . . N34 N 0.6209(6) 0.4008(3) 0.1299(3) 0.0518(17) Uani 1 1 d . . . N35 N 0.6578(8) 0.4345(4) 0.1119(4) 0.081(3) Uani 1 1 d . . . N36 N 0.6911(11) 0.4677(5) 0.0940(5) 0.114(5) Uani 1 1 d . . . N37 N 0.9515(13) -0.0030(7) 0.1003(7) 0.124(5) Uani 1 1 d U . . N38 N 0.1033(17) 0.2566(11) 0.1884(11) 0.193(6) Uani 1 1 d DU . . C1 C 0.1205(6) 0.3559(4) 0.0765(4) 0.0462(18) Uani 1 1 d . . . H1 H 0.1606 0.3306 0.1141 0.055 Uiso 1 1 calc R . . C2 C 0.0307(6) 0.3730(5) 0.0580(5) 0.056(2) Uani 1 1 d . . . H2 H 0.0087 0.3597 0.0815 0.068 Uiso 1 1 calc R . . C3 C -0.0280(6) 0.4108(4) 0.0034(5) 0.056(2) Uani 1 1 d . . . H3A H -0.0922 0.4232 -0.0121 0.067 Uiso 1 1 calc R . . C4 C 0.0081(6) 0.4294(4) -0.0271(4) 0.051(2) Uani 1 1 d . . . H4 H -0.0305 0.4560 -0.0639 0.062 Uiso 1 1 calc R . . C5 C 0.1014(6) 0.4101(4) -0.0048(4) 0.0453(17) Uani 1 1 d . . . C6 C 0.1438(6) 0.4314(4) -0.0359(4) 0.0460(18) Uani 1 1 d . . . C7 C 0.0951(7) 0.4799(5) -0.0875(4) 0.061(2) Uani 1 1 d . . . H7A H 0.1453 0.5066 -0.0834 0.091 Uiso 1 1 calc R . . H7B H 0.0522 0.5065 -0.0838 0.091 Uiso 1 1 calc R . . H7C H 0.0556 0.4586 -0.1294 0.091 Uiso 1 1 calc R . . C8 C 0.3529(6) 0.3887(4) -0.0177(4) 0.0488(18) Uani 1 1 d . . . C9 C 0.5251(8) 0.4330(5) -0.0704(5) 0.065(3) Uani 1 1 d . . . H9A H 0.4567 0.4476 -0.0950 0.098 Uiso 1 1 calc R . . H9B H 0.5363 0.4160 -0.0998 0.098 Uiso 1 1 calc R . . H9C H 0.5698 0.4689 -0.0463 0.098 Uiso 1 1 calc R . . C10 C 0.5441(7) 0.3816(4) -0.0243(4) 0.0490(19) Uani 1 1 d . . . C11 C 0.6340(7) 0.3442(4) 0.0092(4) 0.052(2) Uani 1 1 d . . . C12 C 0.7002(7) 0.3495(5) -0.0047(5) 0.061(2) Uani 1 1 d . . . H12 H 0.6884 0.3800 -0.0353 0.073 Uiso 1 1 calc R . . C13 C 0.7817(7) 0.3109(6) 0.0254(6) 0.071(3) Uani 1 1 d . . . H13 H 0.8265 0.3140 0.0160 0.086 Uiso 1 1 calc R . . C14 C 0.7964(8) 0.2671(6) 0.0701(5) 0.070(3) Uani 1 1 d . . . H14 H 0.8523 0.2399 0.0922 0.084 Uiso 1 1 calc R . . C15 C 0.7315(6) 0.2637(4) 0.0818(4) 0.0501(19) Uani 1 1 d . . . H15A H 0.7430 0.2331 0.1122 0.060 Uiso 1 1 calc R . . C16 C 0.2860(6) 0.4351(5) 0.2339(4) 0.053(2) Uani 1 1 d . . . H16 H 0.2913 0.3902 0.2399 0.063 Uiso 1 1 calc R . . C17 C 0.2057(7) 0.4648(6) 0.2221(5) 0.070(3) Uani 1 1 d . . . H17 H 0.1558 0.4407 0.2183 0.084 Uiso 1 1 calc R . . C18 C 0.1988(7) 0.5279(6) 0.2160(6) 0.073(3) Uani 1 1 d . . . H18 H 0.1440 0.5493 0.2083 0.088 Uiso 1 1 calc R . . C19 C 0.2708(7) 0.5623(5) 0.2206(5) 0.063(3) Uani 1 1 d . . . H19 H 0.2669 0.6075 0.2171 0.075 Uiso 1 1 calc R . . C20 C 0.3491(6) 0.5298(5) 0.2307(4) 0.052(2) Uani 1 1 d . . . C21 C 0.4268(6) 0.5639(4) 0.2339(4) 0.0466(18) Uani 1 1 d . . . C22 C 0.4236(8) 0.6344(5) 0.2275(6) 0.068(3) Uani 1 1 d . . . H22A H 0.4105 0.6537 0.2552 0.101 Uiso 1 1 calc R . . H22B H 0.3712 0.6463 0.1827 0.101 Uiso 1 1 calc R . . H22C H 0.4871 0.6498 0.2402 0.101 Uiso 1 1 calc R . . C23 C 0.6259(5) 0.5145(3) 0.2473(4) 0.0391(15) Uani 1 1 d . . . C24 C 0.8401(12) 0.5657(6) 0.2310(9) 0.105(5) Uani 1 1 d . . . H24A H 0.7817 0.5824 0.1901 0.157 Uiso 1 1 calc R . . H24B H 0.8960 0.5651 0.2301 0.157 Uiso 1 1 calc R . . H24C H 0.8558 0.5931 0.2662 0.157 Uiso 1 1 calc R . . C25 C 0.8199(7) 0.4999(5) 0.2409(5) 0.057(2) Uani 1 1 d . . . C26 C 0.8719(7) 0.4443(5) 0.2388(4) 0.052(2) Uani 1 1 d . . . C27 C 0.9458(8) 0.4542(5) 0.2342(5) 0.066(3) Uani 1 1 d . . . H27 H 0.9678 0.4959 0.2348 0.079 Uiso 1 1 calc R . . C28 C 0.9873(9) 0.4001(6) 0.2285(6) 0.076(3) Uani 1 1 d . . . H28 H 1.0395 0.4050 0.2260 0.092 Uiso 1 1 calc R . . C29 C 0.9548(7) 0.3418(5) 0.2265(5) 0.060(2) Uani 1 1 d . . . H29 H 0.9804 0.3052 0.2202 0.073 Uiso 1 1 calc R . . C30 C 0.8849(7) 0.3365(4) 0.2338(4) 0.051(2) Uani 1 1 d . . . H30 H 0.8646 0.2948 0.2350 0.061 Uiso 1 1 calc R . . C31 C 0.1648(6) 0.2600(4) -0.0685(4) 0.0470(18) Uani 1 1 d . . . H31 H 0.1813 0.2982 -0.0792 0.056 Uiso 1 1 calc R . . C32 C 0.1071(8) 0.2167(6) -0.1154(5) 0.070(3) Uani 1 1 d . . . H32 H 0.0812 0.2255 -0.1584 0.084 Uiso 1 1 calc R . . C33 C 0.0860(8) 0.1595(5) -0.1002(5) 0.066(3) Uani 1 1 d . . . H33 H 0.0470 0.1280 -0.1322 0.079 Uiso 1 1 calc R . . C34 C 0.1227(7) 0.1493(4) -0.0377(5) 0.057(2) Uani 1 1 d . . . H34 H 0.1093 0.1105 -0.0260 0.068 Uiso 1 1 calc R . . C35 C 0.1792(6) 0.1959(4) 0.0080(4) 0.0479(18) Uani 1 1 d . . . C36 C 0.2172(6) 0.1864(4) 0.0754(4) 0.0478(18) Uani 1 1 d . . . C37 C 0.2026(8) 0.1279(4) 0.0989(5) 0.062(2) Uani 1 1 d . . . H37A H 0.2660 0.1063 0.1291 0.092 Uiso 1 1 calc R . . H37B H 0.1571 0.0996 0.0626 0.092 Uiso 1 1 calc R . . H37C H 0.1749 0.1387 0.1208 0.092 Uiso 1 1 calc R . . C38 C 0.3640(5) 0.2803(4) 0.2120(4) 0.0405(16) Uani 1 1 d . . . C39 C 0.5313(9) 0.2743(5) 0.4045(5) 0.067(3) Uani 1 1 d . . . H39A H 0.4917 0.2389 0.3753 0.100 Uiso 1 1 calc R . . H39B H 0.5069 0.2863 0.4281 0.100 Uiso 1 1 calc R . . H39C H 0.6003 0.2610 0.4349 0.100 Uiso 1 1 calc R . . C40 C 0.5236(6) 0.3289(4) 0.3673(4) 0.0438(17) Uani 1 1 d . . . C41 C 0.5827(6) 0.3864(4) 0.3991(4) 0.0503(19) Uani 1 1 d . . . C42 C 0.6365(7) 0.3950(5) 0.4632(4) 0.062(2) Uani 1 1 d . . . H42 H 0.6377 0.3630 0.4890 0.075 Uiso 1 1 calc R . . C43 C 0.6913(8) 0.4521(6) 0.4918(5) 0.074(3) Uani 1 1 d . . . H43 H 0.7290 0.4593 0.5366 0.089 Uiso 1 1 calc R . . C44 C 0.6880(7) 0.4951(5) 0.4537(4) 0.063(2) Uani 1 1 d . . . H44 H 0.7239 0.5338 0.4714 0.075 Uiso 1 1 calc R . . C45 C 0.6337(6) 0.4843(4) 0.3898(4) 0.0501(19) Uani 1 1 d . . . H45 H 0.6329 0.5161 0.3640 0.060 Uiso 1 1 calc R . . C46 C 0.3641(7) 0.2284(6) -0.0679(5) 0.067(3) Uani 1 1 d . . . H46 H 0.3469 0.2721 -0.0783 0.080 Uiso 1 1 calc R . . C47 C 0.3086(12) 0.1869(9) -0.1142(8) 0.104(5) Uani 1 1 d . . . H47 H 0.2518 0.2005 -0.1551 0.124 Uiso 1 1 calc R . . C48 C 0.3332(14) 0.1259(11) -0.1027(8) 0.138(8) Uani 1 1 d . . . H48 H 0.2963 0.0957 -0.1364 0.165 Uiso 1 1 calc R . . C49 C 0.4157(13) 0.1051(8) -0.0395(8) 0.109(5) Uani 1 1 d . . . H49 H 0.4326 0.0614 -0.0296 0.130 Uiso 1 1 calc R . . C50 C 0.4700(9) 0.1534(7) 0.0071(6) 0.077(3) Uani 1 1 d . . . C51 C 0.5546(9) 0.1362(5) 0.0725(5) 0.069(3) Uani 1 1 d . . . C52 C 0.5844(11) 0.0704(6) 0.0946(7) 0.093(4) Uani 1 1 d . . . H52A H 0.6491 0.0624 0.1056 0.139 Uiso 1 1 calc R . . H52B H 0.5360 0.0411 0.0605 0.139 Uiso 1 1 calc R . . H52C H 0.5881 0.0635 0.1326 0.139 Uiso 1 1 calc R . . C53 C 0.7070(6) 0.2253(4) 0.2095(4) 0.0411(16) Uani 1 1 d . . . C54 C 0.9164(8) 0.2158(5) 0.4030(5) 0.072(3) Uani 1 1 d . . . H54A H 0.8687 0.1821 0.3917 0.107 Uiso 1 1 calc R . . H54B H 0.9561 0.2252 0.4490 0.107 Uiso 1 1 calc R . . H54C H 0.9596 0.2014 0.3930 0.107 Uiso 1 1 calc R . . C55 C 0.8634(6) 0.2739(4) 0.3657(4) 0.0455(17) Uani 1 1 d . . . C56 C 0.8774(6) 0.3344(4) 0.3980(4) 0.0497(19) Uani 1 1 d . . . C57 C 0.9302(7) 0.3368(6) 0.4646(5) 0.072(3) Uani 1 1 d . . . H57 H 0.9605 0.2996 0.4902 0.086 Uiso 1 1 calc R . . C58 C 0.9372(9) 0.3946(7) 0.4921(5) 0.090(4) Uani 1 1 d . . . H58 H 0.9721 0.3971 0.5372 0.108 Uiso 1 1 calc R . . C59 C 0.8949(7) 0.4478(6) 0.4558(5) 0.071(3) Uani 1 1 d . . . H59 H 0.8999 0.4877 0.4746 0.085 Uiso 1 1 calc R . . C60 C 0.8453(7) 0.4419(4) 0.3917(4) 0.053(2) Uani 1 1 d . . . H60 H 0.8168 0.4792 0.3661 0.064 Uiso 1 1 calc R . . C61 C 0.9394(19) 0.0413(13) 0.1093(12) 0.165(7) Uani 1 1 d U . . C62 C 0.9261(18) 0.1136(12) 0.1162(11) 0.184(8) Uani 1 1 d U . . H62A H 0.9839 0.1373 0.1277 0.277 Uiso 1 1 calc R . . H62B H 0.9190 0.1193 0.1499 0.277 Uiso 1 1 calc R . . H62C H 0.8670 0.1297 0.0754 0.277 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 Tb1 0.0407(2) 0.0370(2) 0.03398(19) -0.00004(13) 0.02068(16) -0.00217(14) Tb2 0.0489(2) 0.0507(2) 0.0406(2) 0.00145(16) 0.02554(19) -0.00157(17) Tb3 0.03128(18) 0.03493(19) 0.03174(18) 0.00070(12) 0.01562(15) 0.00037(12) Tb4 0.03815(19) 0.0377(2) 0.03309(19) 0.00265(13) 0.02057(16) 0.00359(13) O1 0.048(3) 0.048(3) 0.037(3) 0.007(2) 0.026(2) 0.001(2) O2 0.037(2) 0.032(2) 0.049(3) -0.002(2) 0.028(2) -0.0017(19) O3 0.042(3) 0.037(3) 0.031(2) 0.0008(19) 0.017(2) -0.008(2) O4 0.044(3) 0.034(2) 0.034(2) 0.0025(19) 0.021(2) 0.006(2) O5 0.047(3) 0.064(4) 0.058(4) -0.016(3) 0.024(3) 0.002(3) O6 0.241(13) 0.210(13) 0.284(17) 0.067(12) 0.193(14) 0.015(11) O7 0.223(13) 0.193(12) 0.258(15) 0.044(12) 0.200(13) 0.022(11) O8 0.224(13) 0.188(12) 0.299(16) 0.022(12) 0.202(13) 0.051(10) O9 0.088(5) 0.049(4) 0.121(7) 0.006(4) 0.075(5) 0.003(4) O10 0.082(11) 0.062(9) 0.30(3) 0.012(13) 0.061(15) 0.019(8) O11 0.12(3) 0.066(17) 0.12(3) 0.043(17) 0.03(2) -0.017(16) N1 0.036(3) 0.047(4) 0.041(3) -0.002(3) 0.018(3) -0.003(3) N2 0.040(3) 0.045(4) 0.036(3) -0.005(3) 0.018(3) -0.004(3) N3 0.056(4) 0.051(4) 0.034(3) 0.006(3) 0.023(3) 0.001(3) N4 0.058(4) 0.055(4) 0.044(4) 0.012(3) 0.032(3) 0.001(3) N5 0.054(4) 0.046(4) 0.039(3) 0.001(3) 0.027(3) -0.008(3) N6 0.058(4) 0.054(4) 0.040(4) -0.010(3) 0.029(3) -0.007(3) N7 0.037(3) 0.050(4) 0.038(3) -0.001(3) 0.017(3) 0.004(3) N8 0.037(3) 0.037(3) 0.033(3) -0.004(2) 0.017(3) -0.001(2) N9 0.039(3) 0.040(3) 0.048(4) 0.000(3) 0.025(3) -0.001(3) N10 0.047(4) 0.038(3) 0.064(5) -0.001(3) 0.034(4) -0.004(3) N11 0.042(3) 0.037(3) 0.044(3) -0.001(3) 0.026(3) 0.001(3) N12 0.043(3) 0.051(4) 0.042(3) 0.007(3) 0.025(3) 0.009(3) N13 0.050(4) 0.048(4) 0.040(3) -0.008(3) 0.024(3) -0.004(3) N14 0.040(3) 0.043(3) 0.038(3) -0.003(3) 0.021(3) -0.007(3) N15 0.052(4) 0.044(4) 0.037(3) 0.004(3) 0.024(3) -0.006(3) N16 0.043(3) 0.050(4) 0.036(3) 0.002(3) 0.021(3) -0.004(3) N17 0.034(3) 0.049(4) 0.035(3) 0.006(3) 0.021(3) -0.001(3) N18 0.046(3) 0.044(3) 0.037(3) -0.002(3) 0.022(3) 0.005(3) N19 0.059(5) 0.087(6) 0.050(4) -0.010(4) 0.035(4) -0.003(4) N20 0.059(4) 0.048(4) 0.048(4) -0.002(3) 0.037(4) 0.005(3) N21 0.058(4) 0.042(4) 0.050(4) 0.005(3) 0.035(4) 0.009(3) N22 0.054(4) 0.042(3) 0.043(3) 0.012(3) 0.030(3) 0.011(3) N23 0.040(3) 0.041(3) 0.045(3) 0.009(3) 0.027(3) 0.009(3) N24 0.036(3) 0.058(4) 0.038(3) 0.003(3) 0.017(3) 0.002(3) N25 0.049(4) 0.039(4) 0.059(4) -0.001(3) 0.031(3) -0.003(3) N26 0.050(4) 0.045(4) 0.071(5) 0.001(3) 0.036(4) 0.001(3) N27 0.089(7) 0.041(5) 0.132(9) 0.000(5) 0.073(7) -0.007(4) N28 0.039(3) 0.044(4) 0.047(4) 0.011(3) 0.027(3) 0.009(3) N29 0.045(4) 0.049(4) 0.058(4) 0.011(3) 0.036(3) 0.009(3) N30 0.066(5) 0.073(6) 0.071(5) 0.029(5) 0.046(5) 0.019(4) N31 0.043(3) 0.038(3) 0.034(3) 0.001(2) 0.017(3) 0.004(3) N32 0.040(3) 0.037(3) 0.036(3) -0.002(3) 0.017(3) 0.000(3) N33 0.048(4) 0.049(4) 0.044(4) 0.005(3) 0.021(3) 0.009(3) N34 0.063(4) 0.042(4) 0.038(3) 0.008(3) 0.024(3) -0.001(3) N35 0.102(7) 0.054(5) 0.044(4) -0.001(4) 0.023(5) -0.007(5) N36 0.190(13) 0.082(7) 0.065(6) -0.001(5) 0.077(8) -0.070(8) N37 0.141(10) 0.092(9) 0.097(8) 0.016(8) 0.053(7) 0.020(9) N38 0.224(12) 0.192(11) 0.276(15) 0.055(11) 0.211(13) 0.027(10) C1 0.034(4) 0.048(4) 0.046(4) -0.002(3) 0.020(3) -0.010(3) C2 0.042(4) 0.059(5) 0.058(5) -0.006(4) 0.027(4) 0.000(4) C3 0.037(4) 0.055(5) 0.063(5) -0.010(4) 0.025(4) -0.001(4) C4 0.045(4) 0.042(4) 0.049(5) -0.009(3) 0.020(4) 0.006(3) C5 0.036(4) 0.042(4) 0.041(4) -0.006(3) 0.015(3) -0.001(3) C6 0.043(4) 0.048(4) 0.031(4) -0.005(3) 0.015(3) -0.004(3) C7 0.053(5) 0.080(7) 0.041(4) 0.011(4) 0.025(4) 0.020(5) C8 0.048(4) 0.054(5) 0.031(4) -0.001(3) 0.017(3) -0.005(4) C9 0.076(6) 0.073(6) 0.058(6) 0.020(5) 0.047(5) 0.005(5) C10 0.059(5) 0.053(5) 0.038(4) -0.004(3) 0.032(4) -0.010(4) C11 0.060(5) 0.054(5) 0.045(4) -0.009(4) 0.034(4) -0.014(4) C12 0.065(6) 0.065(6) 0.062(6) -0.002(4) 0.044(5) -0.014(5) C13 0.051(5) 0.092(8) 0.077(7) -0.002(6) 0.042(5) -0.007(5) C14 0.055(5) 0.080(7) 0.067(6) 0.004(5) 0.034(5) 0.003(5) C15 0.047(4) 0.055(5) 0.041(4) 0.004(4) 0.024(4) 0.004(4) C16 0.043(4) 0.061(5) 0.051(5) 0.007(4) 0.028(4) -0.005(4) C17 0.043(5) 0.096(9) 0.072(7) 0.000(6) 0.036(5) 0.000(5) C18 0.044(5) 0.089(8) 0.080(7) -0.017(6) 0.035(5) 0.007(5) C19 0.045(5) 0.062(6) 0.061(5) -0.018(4) 0.023(4) 0.012(4) C20 0.039(4) 0.065(5) 0.038(4) -0.010(4) 0.017(3) 0.007(4) C21 0.044(4) 0.045(4) 0.042(4) -0.008(3) 0.022(3) 0.005(3) C22 0.055(5) 0.048(5) 0.089(8) -0.008(5) 0.039(5) 0.005(4) C23 0.039(4) 0.032(3) 0.042(4) -0.001(3) 0.024(3) -0.004(3) C24 0.120(11) 0.062(7) 0.191(17) 0.004(9) 0.125(13) -0.008(7) C25 0.050(5) 0.051(5) 0.073(6) -0.005(4) 0.039(5) -0.007(4) C26 0.050(4) 0.058(5) 0.053(5) 0.008(4) 0.034(4) 0.001(4) C27 0.061(6) 0.070(6) 0.081(7) 0.023(5) 0.052(6) 0.012(5) C28 0.069(7) 0.102(9) 0.086(8) 0.014(7) 0.062(7) 0.010(6) C29 0.060(5) 0.081(7) 0.057(5) 0.020(5) 0.044(5) 0.018(5) C30 0.057(5) 0.054(5) 0.051(5) 0.012(4) 0.038(4) 0.016(4) C31 0.045(4) 0.047(4) 0.044(4) -0.005(3) 0.024(4) -0.008(3) C32 0.064(6) 0.082(7) 0.042(5) -0.012(5) 0.022(5) -0.016(5) C33 0.059(5) 0.060(6) 0.053(5) -0.015(4) 0.022(5) -0.018(5) C34 0.055(5) 0.045(5) 0.062(5) -0.010(4) 0.033(5) -0.013(4) C35 0.037(4) 0.055(5) 0.040(4) -0.003(3) 0.018(3) -0.001(3) C36 0.036(4) 0.046(4) 0.048(4) -0.004(3) 0.020(3) -0.005(3) C37 0.064(6) 0.043(5) 0.053(5) -0.003(4) 0.024(4) -0.015(4) C38 0.035(3) 0.037(4) 0.043(4) -0.001(3) 0.021(3) -0.003(3) C39 0.087(7) 0.069(6) 0.045(5) 0.013(4) 0.041(5) -0.001(5) C40 0.039(4) 0.055(5) 0.032(4) 0.005(3) 0.019(3) 0.001(3) C41 0.049(4) 0.057(5) 0.040(4) 0.002(4) 0.025(4) 0.005(4) C42 0.062(6) 0.076(6) 0.037(4) -0.003(4) 0.024(4) -0.014(5) C43 0.069(6) 0.090(8) 0.035(5) -0.005(5) 0.018(5) -0.003(6) C44 0.058(5) 0.063(6) 0.043(5) -0.014(4) 0.019(4) -0.006(4) C45 0.055(5) 0.047(4) 0.040(4) -0.005(3) 0.025(4) -0.003(4) C46 0.049(5) 0.093(8) 0.054(5) -0.010(5) 0.029(5) -0.013(5) C47 0.089(10) 0.125(13) 0.094(10) -0.034(10) 0.056(9) -0.007(9) C48 0.118(14) 0.17(2) 0.088(11) -0.082(13) 0.047(10) -0.053(14) C49 0.117(12) 0.103(11) 0.106(11) -0.052(9) 0.069(10) -0.039(9) C50 0.082(7) 0.097(9) 0.062(6) -0.033(6) 0.049(6) -0.025(7) C51 0.083(7) 0.063(6) 0.070(7) -0.023(5) 0.052(6) 0.001(5) C52 0.124(11) 0.053(6) 0.091(9) -0.021(6) 0.061(9) -0.008(7) C53 0.043(4) 0.038(4) 0.048(4) 0.005(3) 0.031(4) 0.004(3) C54 0.068(6) 0.066(6) 0.060(6) 0.025(5) 0.029(5) 0.020(5) C55 0.042(4) 0.052(5) 0.043(4) 0.009(3) 0.027(4) 0.007(3) C56 0.039(4) 0.060(5) 0.043(4) 0.002(4) 0.022(4) 0.004(4) C57 0.051(5) 0.087(8) 0.043(5) 0.007(5) 0.012(4) 0.010(5) C58 0.068(7) 0.126(11) 0.042(5) -0.018(6) 0.017(5) 0.003(7) C59 0.053(5) 0.081(7) 0.051(5) -0.014(5) 0.018(5) 0.007(5) C60 0.049(5) 0.051(5) 0.046(4) -0.006(4) 0.023(4) -0.002(4) C61 0.152(10) 0.137(11) 0.120(9) 0.005(10) 0.041(8) 0.012(11) C62 0.158(12) 0.162(13) 0.139(11) 0.001(12) 0.045(10) 0.013(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O3 2.313(5) . ? Tb1 O1 2.319(5) . ? Tb1 N25 2.455(7) . ? Tb1 N31 2.482(6) . ? Tb1 N2 2.522(7) . ? Tb1 N14 2.537(6) . ? Tb1 N1 2.553(7) . ? Tb1 N13 2.564(7) . ? Tb1 O5 2.576(6) . ? Tb2 O4 2.264(5) . ? Tb2 O1 2.273(6) . ? Tb2 N34 2.485(7) . ? Tb2 N25 2.511(7) . ? Tb2 N5 2.525(7) . ? Tb2 N20 2.528(7) . ? Tb2 N19 2.559(9) . ? Tb2 N6 2.587(8) . ? Tb2 O5 2.710(6) . ? Tb3 O2 2.303(5) . ? Tb3 O3 2.331(5) . ? Tb3 N28 2.481(6) . ? Tb3 N8 2.503(6) . ? Tb3 N7 2.509(7) . ? Tb3 N31 2.512(6) . ? Tb3 N17 2.532(6) . ? Tb3 O5 2.557(7) . ? Tb3 N18 2.566(6) . ? Tb4 O4 2.290(5) . ? Tb4 O2 2.319(5) . ? Tb4 N28 2.467(7) . ? Tb4 N34 2.475(7) . ? Tb4 N23 2.516(6) . ? Tb4 N12 2.547(7) . ? Tb4 N24 2.548(7) . ? Tb4 N11 2.565(6) . ? Tb4 O5 2.600(6) . ? O1 C8 1.286(10) . ? O2 C23 1.303(9) . ? O3 C38 1.283(9) . ? O4 C53 1.292(9) . ? O6 N38 1.408(16) . ? O7 N38 1.324(16) . ? O8 N38 1.455(16) . ? N1 C1 1.305(11) . ? N1 C5 1.359(10) . ? N2 C6 1.298(11) . ? N2 N3 1.369(10) . ? N3 C8 1.347(12) . ? N3 H3 0.8800 . ? N4 C8 1.317(11) . ? N4 N5 1.383(10) . ? N5 C10 1.285(11) . ? N6 C15 1.335(11) . ? N6 C11 1.369(11) . ? N7 C16 1.336(11) . ? N7 C20 1.361(12) . ? N8 C21 1.305(10) . ? N8 N9 1.419(9) . ? N9 C23 1.304(10) . ? N10 C23 1.357(10) . ? N10 N11 1.367(9) . ? N10 H10 0.8800 . ? N11 C25 1.277(11) . ? N12 C26 1.329(12) . ? N12 C30 1.351(11) . ? N13 C35 1.339(11) . ? N13 C31 1.368(11) . ? N14 C36 1.314(10) . ? N14 N15 1.368(9) . ? N15 C38 1.350(10) . ? N15 H15 0.8800 . ? N16 C38 1.320(10) . ? N16 N17 1.381(9) . ? N17 C40 1.299(10) . ? N18 C45 1.338(11) . ? N18 C41 1.365(11) . ? N19 C46 1.327(13) . ? N19 C50 1.354(16) . ? N20 C51 1.308(12) . ? N20 N21 1.375(10) . ? N21 C53 1.335(11) . ? N22 C53 1.342(10) . ? N22 N23 1.362(10) . ? N23 C55 1.288(10) . ? N24 C60 1.337(11) . ? N24 C56 1.340(11) . ? N25 N26 1.194(10) . ? N26 N27 1.130(11) . ? N28 N29 1.198(9) . ? N29 N30 1.145(10) . ? N31 N32 1.200(9) . ? N32 N33 1.136(9) . ? N34 N35 1.228(13) . ? N35 N36 1.174(14) . ? N37 C61 1.01(3) . ? C1 C2 1.353(12) . ? C1 H1 0.9500 . ? C2 C3 1.391(14) . ? C2 H2 0.9500 . ? C3 C4 1.347(14) . ? C3 H3A 0.9500 . ? C4 C5 1.391(11) . ? C4 H4 0.9500 . ? C5 C6 1.471(12) . ? C6 C7 1.479(12) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.505(12) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.452(13) . ? C11 C12 1.408(13) . ? C12 C13 1.371(15) . ? C12 H12 0.9500 . ? C13 C14 1.392(16) . ? C13 H13 0.9500 . ? C14 C15 1.338(14) . ? C14 H14 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.368(14) . ? C16 H16 0.9500 . ? C17 C18 1.330(17) . ? C17 H17 0.9500 . ? C18 C19 1.374(16) . ? C18 H18 0.9500 . ? C19 C20 1.385(12) . ? C19 H19 0.9500 . ? C20 C21 1.477(13) . ? C21 C22 1.486(13) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 C25 1.487(15) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.493(13) . ? C26 C27 1.373(13) . ? C27 C28 1.398(16) . ? C27 H27 0.9500 . ? C28 C29 1.334(17) . ? C28 H28 0.9500 . ? C29 C30 1.340(13) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.354(13) . ? C31 H31 0.9500 . ? C32 C33 1.383(15) . ? C32 H32 0.9500 . ? C33 C34 1.377(14) . ? C33 H33 0.9500 . ? C34 C35 1.382(12) . ? C34 H34 0.9500 . ? C35 C36 1.487(12) . ? C36 C37 1.466(12) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C39 C40 1.464(12) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.463(12) . ? C41 C42 1.352(12) . ? C42 C43 1.420(15) . ? C42 H42 0.9500 . ? C43 C44 1.327(16) . ? C43 H43 0.9500 . ? C44 C45 1.356(12) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.314(18) . ? C46 H46 0.9500 . ? C47 C48 1.32(3) . ? C47 H47 0.9500 . ? C48 C49 1.44(3) . ? C48 H48 0.9500 . ? C49 C50 1.412(16) . ? C49 H49 0.9500 . ? C50 C51 1.462(17) . ? C51 C52 1.463(17) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C54 C55 1.477(12) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.465(12) . ? C56 C57 1.398(13) . ? C57 C58 1.383(18) . ? C57 H57 0.9500 . ? C58 C59 1.354(18) . ? C58 H58 0.9500 . ? C59 C60 1.355(13) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.56(3) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Tb1 O1 143.50(19) . . ? O3 Tb1 N25 93.1(2) . . ? O1 Tb1 N25 71.4(2) . . ? O3 Tb1 N31 70.58(19) . . ? O1 Tb1 N31 94.6(2) . . ? N25 Tb1 N31 131.2(2) . . ? O3 Tb1 N2 136.8(2) . . ? O1 Tb1 N2 62.8(2) . . ? N25 Tb1 N2 129.4(2) . . ? N31 Tb1 N2 74.6(2) . . ? O3 Tb1 N14 62.48(19) . . ? O1 Tb1 N14 135.7(2) . . ? N25 Tb1 N14 72.5(2) . . ? N31 Tb1 N14 128.8(2) . . ? N2 Tb1 N14 130.4(2) . . ? O3 Tb1 N1 85.3(2) . . ? O1 Tb1 N1 125.1(2) . . ? N25 Tb1 N1 148.6(2) . . ? N31 Tb1 N1 77.7(2) . . ? N2 Tb1 N1 62.7(2) . . ? N14 Tb1 N1 79.2(2) . . ? O3 Tb1 N13 123.4(2) . . ? O1 Tb1 N13 86.2(2) . . ? N25 Tb1 N13 77.3(2) . . ? N31 Tb1 N13 150.1(2) . . ? N2 Tb1 N13 79.4(2) . . ? N14 Tb1 N13 61.4(2) . . ? N1 Tb1 N13 77.5(2) . . ? O3 Tb1 O5 71.6(2) . . ? O1 Tb1 O5 72.0(2) . . ? N25 Tb1 O5 66.7(2) . . ? N31 Tb1 O5 64.5(2) . . ? N2 Tb1 O5 114.6(2) . . ? N14 Tb1 O5 115.0(2) . . ? N1 Tb1 O5 140.3(2) . . ? N13 Tb1 O5 142.1(2) . . ? O3 Tb1 Tb2 112.01(13) . . ? O1 Tb1 Tb2 36.04(13) . . ? N25 Tb1 Tb2 42.55(17) . . ? N31 Tb1 Tb2 100.28(16) . . ? N2 Tb1 Tb2 98.46(16) . . ? N14 Tb1 Tb2 115.01(16) . . ? N1 Tb1 Tb2 161.09(16) . . ? N13 Tb1 Tb2 97.77(16) . . ? O5 Tb1 Tb2 47.18(15) . . ? O3 Tb1 Tb3 37.26(12) . . ? O1 Tb1 Tb3 110.49(14) . . ? N25 Tb1 Tb3 97.82(17) . . ? N31 Tb1 Tb3 42.44(14) . . ? N2 Tb1 Tb3 116.88(14) . . ? N14 Tb1 Tb3 98.96(14) . . ? N1 Tb1 Tb3 99.57(15) . . ? N13 Tb1 Tb3 160.38(16) . . ? O5 Tb1 Tb3 43.62(15) . . ? Tb2 Tb1 Tb3 90.781(16) . . ? O4 Tb2 O1 140.51(19) . . ? O4 Tb2 N34 71.5(2) . . ? O1 Tb2 N34 93.2(2) . . ? O4 Tb2 N25 89.3(2) . . ? O1 Tb2 N25 71.1(2) . . ? N34 Tb2 N25 127.4(2) . . ? O4 Tb2 N5 137.8(2) . . ? O1 Tb2 N5 63.6(2) . . ? N34 Tb2 N5 73.5(2) . . ? N25 Tb2 N5 131.3(2) . . ? O4 Tb2 N20 63.2(2) . . ? O1 Tb2 N20 136.0(2) . . ? N34 Tb2 N20 129.7(2) . . ? N25 Tb2 N20 74.1(2) . . ? N5 Tb2 N20 130.6(2) . . ? O4 Tb2 N19 126.3(2) . . ? O1 Tb2 N19 83.0(2) . . ? N34 Tb2 N19 153.4(3) . . ? N25 Tb2 N19 76.3(3) . . ? N5 Tb2 N19 81.4(3) . . ? N20 Tb2 N19 63.1(3) . . ? O4 Tb2 N6 87.4(2) . . ? O1 Tb2 N6 125.7(2) . . ? N34 Tb2 N6 77.7(2) . . ? N25 Tb2 N6 151.8(2) . . ? N5 Tb2 N6 62.5(2) . . ? N20 Tb2 N6 79.4(2) . . ? N19 Tb2 N6 83.2(2) . . ? O4 Tb2 O5 70.52(18) . . ? O1 Tb2 O5 70.09(19) . . ? N34 Tb2 O5 63.6(2) . . ? N25 Tb2 O5 63.9(2) . . ? N5 Tb2 O5 113.0(2) . . ? N20 Tb2 O5 116.4(2) . . ? N19 Tb2 O5 137.1(2) . . ? N6 Tb2 O5 139.6(2) . . ? O4 Tb2 Tb4 36.32(12) . . ? O1 Tb2 Tb4 110.02(14) . . ? N34 Tb2 Tb4 41.97(16) . . ? N25 Tb2 Tb4 95.59(17) . . ? N5 Tb2 Tb4 115.42(15) . . ? N20 Tb2 Tb4 99.28(16) . . ? N19 Tb2 Tb4 161.9(2) . . ? N6 Tb2 Tb4 98.17(15) . . ? O5 Tb2 Tb4 44.88(13) . . ? O4 Tb2 Tb1 107.49(13) . . ? O1 Tb2 Tb1 36.90(13) . . ? N34 Tb2 Tb1 97.62(19) . . ? N25 Tb2 Tb1 41.39(16) . . ? N5 Tb2 Tb1 99.85(17) . . ? N20 Tb2 Tb1 115.53(17) . . ? N19 Tb2 Tb1 94.94(19) . . ? N6 Tb2 Tb1 162.31(17) . . ? O5 Tb2 Tb1 44.22(13) . . ? Tb4 Tb2 Tb1 89.038(17) . . ? O2 Tb3 O3 142.78(19) . . ? O2 Tb3 N28 70.5(2) . . ? O3 Tb3 N28 93.3(2) . . ? O2 Tb3 N8 62.93(19) . . ? O3 Tb3 N8 136.63(19) . . ? N28 Tb3 N8 129.1(2) . . ? O2 Tb3 N7 125.9(2) . . ? O3 Tb3 N7 84.2(2) . . ? N28 Tb3 N7 151.1(2) . . ? N8 Tb3 N7 63.3(2) . . ? O2 Tb3 N31 95.2(2) . . ? O3 Tb3 N31 69.75(19) . . ? N28 Tb3 N31 130.8(2) . . ? N8 Tb3 N31 74.5(2) . . ? N7 Tb3 N31 75.2(2) . . ? O2 Tb3 N17 135.31(19) . . ? O3 Tb3 N17 62.54(19) . . ? N28 Tb3 N17 72.5(2) . . ? N8 Tb3 N17 131.7(2) . . ? N7 Tb3 N17 81.0(2) . . ? N31 Tb3 N17 128.2(2) . . ? O2 Tb3 O5 71.2(2) . . ? O3 Tb3 O5 71.6(2) . . ? N28 Tb3 O5 66.5(2) . . ? N8 Tb3 O5 113.4(2) . . ? N7 Tb3 O5 137.9(2) . . ? N31 Tb3 O5 64.4(2) . . ? N17 Tb3 O5 114.8(2) . . ? O2 Tb3 N18 86.0(2) . . ? O3 Tb3 N18 124.5(2) . . ? N28 Tb3 N18 78.5(2) . . ? N8 Tb3 N18 79.0(2) . . ? N7 Tb3 N18 79.4(2) . . ? N31 Tb3 N18 149.3(2) . . ? N17 Tb3 N18 62.7(2) . . ? O5 Tb3 N18 142.7(2) . . ? O2 Tb3 Tb4 37.34(12) . . ? O3 Tb3 Tb4 109.59(14) . . ? N28 Tb3 Tb4 41.76(15) . . ? N8 Tb3 Tb4 99.62(15) . . ? N7 Tb3 Tb4 162.80(17) . . ? N31 Tb3 Tb4 99.46(16) . . ? N17 Tb3 Tb4 114.14(14) . . ? O5 Tb3 Tb4 44.89(14) . . ? N18 Tb3 Tb4 99.84(16) . . ? O2 Tb3 Tb1 110.33(13) . . ? O3 Tb3 Tb1 36.93(12) . . ? N28 Tb3 Tb1 97.92(16) . . ? N8 Tb3 Tb1 116.11(13) . . ? N7 Tb3 Tb1 97.14(15) . . ? N31 Tb3 Tb1 41.81(15) . . ? N17 Tb3 Tb1 98.69(15) . . ? O5 Tb3 Tb1 44.02(14) . . ? N18 Tb3 Tb1 161.31(16) . . ? Tb4 Tb3 Tb1 88.849(15) . . ? O4 Tb4 O2 142.42(18) . . ? O4 Tb4 N28 93.9(2) . . ? O2 Tb4 N28 70.5(2) . . ? O4 Tb4 N34 71.3(2) . . ? O2 Tb4 N34 93.2(2) . . ? N28 Tb4 N34 131.4(2) . . ? O4 Tb4 N23 62.64(19) . . ? O2 Tb4 N23 138.0(2) . . ? N28 Tb4 N23 75.8(2) . . ? N34 Tb4 N23 128.2(2) . . ? O4 Tb4 N12 85.3(2) . . ? O2 Tb4 N12 124.5(2) . . ? N28 Tb4 N12 151.8(2) . . ? N34 Tb4 N12 75.0(2) . . ? N23 Tb4 N12 78.9(2) . . ? O4 Tb4 N24 126.2(2) . . ? O2 Tb4 N24 84.2(2) . . ? N28 Tb4 N24 76.0(2) . . ? N34 Tb4 N24 149.7(2) . . ? N23 Tb4 N24 63.6(2) . . ? N12 Tb4 N24 81.7(2) . . ? O4 Tb4 N11 137.5(2) . . ? O2 Tb4 N11 62.09(19) . . ? N28 Tb4 N11 127.7(2) . . ? N34 Tb4 N11 73.8(2) . . ? N23 Tb4 N11 129.2(2) . . ? N12 Tb4 N11 62.6(2) . . ? N24 Tb4 N11 78.4(2) . . ? O4 Tb4 O5 72.27(19) . . ? O2 Tb4 O5 70.16(19) . . ? N28 Tb4 O5 66.0(2) . . ? N34 Tb4 O5 65.4(2) . . ? N23 Tb4 O5 117.3(2) . . ? N12 Tb4 O5 138.8(2) . . ? N24 Tb4 O5 139.3(2) . . ? N11 Tb4 O5 113.5(2) . . ? O4 Tb4 Tb2 35.84(12) . . ? O2 Tb4 Tb2 111.67(13) . . ? N28 Tb4 Tb2 100.60(16) . . ? N34 Tb4 Tb2 42.18(17) . . ? N23 Tb4 Tb2 98.34(16) . . ? N12 Tb4 Tb2 95.17(16) . . ? N24 Tb4 Tb2 161.97(17) . . ? N11 Tb4 Tb2 115.97(15) . . ? O5 Tb4 Tb2 47.35(14) . . ? O4 Tb4 Tb3 109.83(13) . . ? O2 Tb4 Tb3 37.04(12) . . ? N28 Tb4 Tb3 42.06(14) . . ? N34 Tb4 Tb3 98.57(19) . . ? N23 Tb4 Tb3 117.75(15) . . ? N12 Tb4 Tb3 161.09(16) . . ? N24 Tb4 Tb3 97.30(16) . . ? N11 Tb4 Tb3 98.65(14) . . ? O5 Tb4 Tb3 43.98(14) . . ? Tb2 Tb4 Tb3 91.308(16) . . ? C8 O1 Tb2 124.0(5) . . ? C8 O1 Tb1 124.6(5) . . ? Tb2 O1 Tb1 107.1(2) . . ? C23 O2 Tb3 123.0(5) . . ? C23 O2 Tb4 127.5(5) . . ? Tb3 O2 Tb4 105.61(19) . . ? C38 O3 Tb1 126.0(5) . . ? C38 O3 Tb3 121.9(4) . . ? Tb1 O3 Tb3 105.8(2) . . ? C53 O4 Tb2 125.8(5) . . ? C53 O4 Tb4 125.4(5) . . ? Tb2 O4 Tb4 107.8(2) . . ? Tb3 O5 Tb1 92.4(2) . . ? Tb3 O5 Tb4 91.13(19) . . ? Tb1 O5 Tb4 174.8(3) . . ? Tb3 O5 Tb2 177.7(3) . . ? Tb1 O5 Tb2 88.60(18) . . ? Tb4 O5 Tb2 87.77(19) . . ? C1 N1 C5 117.1(7) . . ? C1 N1 Tb1 123.4(5) . . ? C5 N1 Tb1 119.6(5) . . ? C6 N2 N3 116.9(7) . . ? C6 N2 Tb1 125.2(6) . . ? N3 N2 Tb1 117.6(5) . . ? C8 N3 N2 113.1(7) . . ? C8 N3 H3 123.5 . . ? N2 N3 H3 123.5 . . ? C8 N4 N5 112.0(7) . . ? C10 N5 N4 118.0(7) . . ? C10 N5 Tb2 124.7(6) . . ? N4 N5 Tb2 116.4(5) . . ? C15 N6 C11 118.1(8) . . ? C15 N6 Tb2 123.9(6) . . ? C11 N6 Tb2 117.9(6) . . ? C16 N7 C20 116.3(8) . . ? C16 N7 Tb3 122.9(6) . . ? C20 N7 Tb3 120.4(6) . . ? C21 N8 N9 115.2(7) . . ? C21 N8 Tb3 124.6(6) . . ? N9 N8 Tb3 119.5(4) . . ? C23 N9 N8 108.1(6) . . ? C23 N10 N11 115.0(6) . . ? C23 N10 H10 122.5 . . ? N11 N10 H10 122.5 . . ? C25 N11 N10 119.2(7) . . ? C25 N11 Tb4 123.4(6) . . ? N10 N11 Tb4 116.9(5) . . ? C26 N12 C30 116.9(8) . . ? C26 N12 Tb4 121.0(6) . . ? C30 N12 Tb4 121.9(6) . . ? C35 N13 C31 117.6(7) . . ? C35 N13 Tb1 121.2(5) . . ? C31 N13 Tb1 120.8(5) . . ? C36 N14 N15 116.0(7) . . ? C36 N14 Tb1 126.1(6) . . ? N15 N14 Tb1 116.6(5) . . ? C38 N15 N14 114.4(6) . . ? C38 N15 H15 122.8 . . ? N14 N15 H15 122.8 . . ? C38 N16 N17 109.5(6) . . ? C40 N17 N16 116.4(6) . . ? C40 N17 Tb3 123.0(5) . . ? N16 N17 Tb3 118.5(4) . . ? C45 N18 C41 117.0(7) . . ? C45 N18 Tb3 123.4(6) . . ? C41 N18 Tb3 119.4(5) . . ? C46 N19 C50 117.8(10) . . ? C46 N19 Tb2 123.8(8) . . ? C50 N19 Tb2 118.2(7) . . ? C51 N20 N21 117.0(8) . . ? C51 N20 Tb2 124.5(7) . . ? N21 N20 Tb2 117.8(5) . . ? C53 N21 N20 111.3(7) . . ? C53 N22 N23 110.9(6) . . ? C55 N23 N22 117.4(6) . . ? C55 N23 Tb4 122.7(5) . . ? N22 N23 Tb4 119.4(5) . . ? C60 N24 C56 118.6(7) . . ? C60 N24 Tb4 121.9(6) . . ? C56 N24 Tb4 117.4(6) . . ? N26 N25 Tb1 130.9(6) . . ? N26 N25 Tb2 129.9(6) . . ? Tb1 N25 Tb2 96.1(2) . . ? N27 N26 N25 178.8(10) . . ? N29 N28 Tb4 128.8(5) . . ? N29 N28 Tb3 132.0(5) . . ? Tb4 N28 Tb3 96.2(2) . . ? N30 N29 N28 179.1(12) . . ? N32 N31 Tb1 128.1(5) . . ? N32 N31 Tb3 130.4(5) . . ? Tb1 N31 Tb3 95.8(2) . . ? N33 N32 N31 178.9(8) . . ? N35 N34 Tb4 126.1(6) . . ? N35 N34 Tb2 127.0(6) . . ? Tb4 N34 Tb2 95.9(2) . . ? N36 N35 N34 178.4(14) . . ? O7 N38 O6 126(2) . . ? O7 N38 O8 99.2(17) . . ? O6 N38 O8 133(2) . . ? N1 C1 C2 125.8(9) . . ? N1 C1 H1 117.1 . . ? C2 C1 H1 117.1 . . ? C1 C2 C3 117.4(9) . . ? C1 C2 H2 121.3 . . ? C3 C2 H2 121.3 . . ? C4 C3 C2 118.7(8) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C3 C4 C5 120.4(9) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? N1 C5 C4 120.6(8) . . ? N1 C5 C6 117.9(7) . . ? C4 C5 C6 121.5(8) . . ? N2 C6 C5 114.0(7) . . ? N2 C6 C7 123.9(8) . . ? C5 C6 C7 122.1(8) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 N4 122.6(8) . . ? O1 C8 N3 119.7(8) . . ? N4 C8 N3 117.6(8) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 C11 115.4(8) . . ? N5 C10 C9 124.7(9) . . ? C11 C10 C9 119.9(8) . . ? N6 C11 C12 119.6(9) . . ? N6 C11 C10 118.2(8) . . ? C12 C11 C10 122.1(8) . . ? C13 C12 C11 120.6(10) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 117.7(10) . . ? C12 C13 H13 121.2 . . ? C14 C13 H13 121.2 . . ? C15 C14 C13 119.7(10) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? N6 C15 C14 124.3(9) . . ? N6 C15 H15A 117.8 . . ? C14 C15 H15A 117.8 . . ? N7 C16 C17 124.2(10) . . ? N7 C16 H16 117.9 . . ? C17 C16 H16 117.9 . . ? C18 C17 C16 118.8(10) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 120.2(9) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C20 118.6(10) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? N7 C20 C19 121.8(9) . . ? N7 C20 C21 117.1(7) . . ? C19 C20 C21 121.1(9) . . ? N8 C21 C20 113.9(7) . . ? N8 C21 C22 125.5(8) . . ? C20 C21 C22 120.6(8) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 C23 N9 125.3(7) . . ? O2 C23 N10 117.0(7) . . ? N9 C23 N10 117.7(7) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 C24 123.8(9) . . ? N11 C25 C26 115.4(8) . . ? C24 C25 C26 120.5(9) . . ? N12 C26 C27 122.6(9) . . ? N12 C26 C25 117.4(8) . . ? C27 C26 C25 119.9(9) . . ? C26 C27 C28 117.0(10) . . ? C26 C27 H27 121.5 . . ? C28 C27 H27 121.5 . . ? C29 C28 C27 121.1(9) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 117.7(10) . . ? C28 C29 H29 121.1 . . ? C30 C29 H29 121.1 . . ? C29 C30 N12 124.5(9) . . ? C29 C30 H30 117.8 . . ? N12 C30 H30 117.8 . . ? C32 C31 N13 122.8(9) . . ? C32 C31 H31 118.6 . . ? N13 C31 H31 118.6 . . ? C31 C32 C33 119.4(10) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C34 C33 C32 118.5(9) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C33 C34 C35 119.7(9) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? N13 C35 C34 122.0(8) . . ? N13 C35 C36 117.6(7) . . ? C34 C35 C36 120.4(8) . . ? N14 C36 C37 123.9(8) . . ? N14 C36 C35 112.2(7) . . ? C37 C36 C35 123.9(8) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O3 C38 N16 125.1(7) . . ? O3 C38 N15 118.0(7) . . ? N16 C38 N15 117.0(7) . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N17 C40 C41 115.9(7) . . ? N17 C40 C39 123.0(8) . . ? C41 C40 C39 121.1(7) . . ? C42 C41 N18 121.4(9) . . ? C42 C41 C40 121.8(8) . . ? N18 C41 C40 116.8(7) . . ? C41 C42 C43 119.7(10) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 117.8(9) . . ? C44 C43 H43 121.1 . . ? C42 C43 H43 121.1 . . ? C43 C44 C45 120.5(10) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? N18 C45 C44 123.6(9) . . ? N18 C45 H45 118.2 . . ? C44 C45 H45 118.2 . . ? C47 C46 N19 126.3(14) . . ? C47 C46 H46 116.8 . . ? N19 C46 H46 116.8 . . ? C46 C47 C48 118.7(16) . . ? C46 C47 H47 120.6 . . ? C48 C47 H47 120.6 . . ? C47 C48 C49 120.4(14) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C50 C49 C48 116.4(16) . . ? C50 C49 H49 121.8 . . ? C48 C49 H49 121.8 . . ? N19 C50 C49 120.3(13) . . ? N19 C50 C51 120.0(9) . . ? C49 C50 C51 119.7(14) . . ? N20 C51 C50 113.5(10) . . ? N20 C51 C52 122.7(11) . . ? C50 C51 C52 123.7(10) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O4 C53 N21 121.7(7) . . ? O4 C53 N22 121.3(7) . . ? N21 C53 N22 117.0(7) . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N23 C55 C56 115.6(7) . . ? N23 C55 C54 123.4(9) . . ? C56 C55 C54 120.9(8) . . ? N24 C56 C57 120.5(9) . . ? N24 C56 C55 118.7(7) . . ? C57 C56 C55 120.7(9) . . ? C58 C57 C56 118.2(10) . . ? C58 C57 H57 120.9 . . ? C56 C57 H57 120.9 . . ? C59 C58 C57 120.9(10) . . ? C59 C58 H58 119.5 . . ? C57 C58 H58 119.5 . . ? C58 C59 C60 117.5(10) . . ? C58 C59 H59 121.3 . . ? C60 C59 H59 121.3 . . ? N24 C60 C59 124.2(9) . . ? N24 C60 H60 117.9 . . ? C59 C60 H60 117.9 . . ? N37 C61 C62 170(4) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.045 _refine_diff_density_min -2.944 _refine_diff_density_rms 0.194 _iucr_refine_instructions_details ; TITL _M3 CELL 0.71075 17.27500 20.96900 26.50589 90.000 128.219 90.000 ZERR 4 0.00300 0.00400 0.00490 0.000 0.003 0.000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H N O TB UNIT 248 264 152 40 16 SHEL 8.147180 0.796452 L.S. 10 FMAP 2 PLAN -25 TEMP -110.0 OMIT -5 16 3 OMIT -1 2 6 ACTA BOND $H SIZE 0.140 0.200 0.120 SIMU 0.005 0.01 1.7 N38 O6 SIMU 0.005 0.01 1.7 N38 O7 SIMU 0.005 0.01 1.7 N38 O8 SIMU 0.005 0.01 1.7 N37 C61 SIMU 0.005 0.01 1.7 C61 C62 DFIX 1.4200 0.0200 O6 N38 DFIX 1.4200 0.0200 N38 O7 DFIX 1.4200 0.0200 N38 O8 DANG 2.3751 0.0400 O6 O7 DANG 2.3577 0.0400 O7 O8 DANG 2.4669 0.0400 O8 O6 WGHT 0.102900 39.424202 FVAR 0.13976 0.65988 TB1 5 0.322410 0.330451 0.081686 11.00000 0.04066 0.03701 = 0.03398 -0.00004 0.02068 -0.00217 TB2 5 0.532842 0.298086 0.082004 11.00000 0.04893 0.05067 = 0.04061 0.00145 0.02554 -0.00157 TB3 5 0.488140 0.407345 0.241394 11.00000 0.03128 0.03493 = 0.03174 0.00070 0.01562 0.00037 TB4 5 0.697629 0.371423 0.242273 11.00000 0.03815 0.03767 = 0.03309 0.00265 0.02057 0.00359 O1 4 0.381805 0.344724 0.024376 11.00000 0.04816 0.04779 = 0.03727 0.00734 0.02579 0.00106 O2 4 0.620363 0.453576 0.254332 11.00000 0.03743 0.03244 = 0.04874 -0.00160 0.02792 -0.00168 O3 4 0.367986 0.328717 0.184137 11.00000 0.04156 0.03714 = 0.03103 0.00083 0.01714 -0.00761 O4 4 0.666429 0.280117 0.185037 11.00000 0.04354 0.03445 = 0.03364 0.00250 0.02105 0.00624 O5 4 0.507676 0.356091 0.162292 11.00000 0.04678 0.06372 = 0.05810 -0.01577 0.02361 0.00181 O6 4 0.060133 0.228691 0.128079 11.00000 0.24128 0.21041 = 0.28420 0.06738 0.19301 0.01488 O7 4 0.140345 0.314974 0.205740 11.00000 0.22346 0.19348 = 0.25848 0.04397 0.20035 0.02214 O8 4 0.145872 0.230334 0.251466 11.00000 0.22415 0.18755 = 0.29919 0.02217 0.20240 0.05117 O9 4 0.313688 0.166554 0.280322 11.00000 0.08810 0.04942 = 0.12096 0.00601 0.07514 0.00301 PART 1 O10 4 0.947374 0.140550 0.290958 21.00000 0.08159 0.06203 = 0.29961 0.01186 0.06091 0.01925 PART 2 O11 4 0.971135 0.182160 0.226950 -21.00000 0.11670 0.06564 = 0.12477 0.04269 0.03009 -0.01716 PART 0 N1 3 0.156755 0.371196 0.047183 11.00000 0.03613 0.04681 = 0.04069 -0.00208 0.01774 -0.00293 N2 3 0.225945 0.403310 -0.014557 11.00000 0.03992 0.04501 = 0.03563 -0.00472 0.01828 -0.00394 N3 3 0.268271 0.420139 -0.042435 11.00000 0.05640 0.05070 = 0.03411 0.00616 0.02268 0.00147 AFIX 43 H3 2 0.242824 0.448562 -0.073356 11.00000 -1.20000 AFIX 0 N4 3 0.400237 0.402592 -0.040550 11.00000 0.05773 0.05502 = 0.04361 0.01174 0.03176 0.00126 N5 3 0.486845 0.368329 -0.010255 11.00000 0.05375 0.04586 = 0.03920 0.00059 0.02665 -0.00810 N6 3 0.651531 0.300409 0.053529 11.00000 0.05832 0.05399 = 0.04014 -0.01025 0.02920 -0.00700 N7 3 0.357471 0.465206 0.237560 11.00000 0.03747 0.05006 = 0.03777 -0.00110 0.01673 0.00366 N8 3 0.493982 0.526609 0.241744 11.00000 0.03689 0.03686 = 0.03270 -0.00410 0.01672 -0.00052 N9 3 0.565962 0.557701 0.240708 11.00000 0.03922 0.04019 = 0.04825 -0.00025 0.02499 -0.00061 N10 3 0.698573 0.533987 0.245049 11.00000 0.04692 0.03757 = 0.06447 -0.00135 0.03416 -0.00444 AFIX 43 H10 2 0.709921 0.574505 0.243219 11.00000 -1.20000 AFIX 0 N11 3 0.752821 0.486006 0.245788 11.00000 0.04230 0.03675 = 0.04412 -0.00063 0.02650 0.00122 N12 3 0.841350 0.386321 0.239580 11.00000 0.04330 0.05114 = 0.04231 0.00680 0.02499 0.00885 N13 3 0.200586 0.251012 -0.006358 11.00000 0.04992 0.04829 = 0.03991 -0.00798 0.02373 -0.00377 N14 3 0.266301 0.236197 0.111722 11.00000 0.04030 0.04331 = 0.03788 -0.00290 0.02093 -0.00729 N15 3 0.306744 0.230613 0.175092 11.00000 0.05169 0.04378 = 0.03747 0.00430 0.02428 -0.00638 AFIX 43 H15 2 0.296303 0.197433 0.190495 11.00000 -1.20000 AFIX 0 N16 3 0.411249 0.275138 0.274420 11.00000 0.04280 0.04957 = 0.03558 0.00155 0.02134 -0.00442 N17 3 0.467017 0.329272 0.304925 11.00000 0.03372 0.04916 = 0.03516 0.00587 0.02082 -0.00072 N18 3 0.581060 0.431108 0.361030 11.00000 0.04625 0.04415 = 0.03677 -0.00208 0.02159 0.00511 N19 3 0.441735 0.215133 -0.008017 11.00000 0.05865 0.08679 = 0.05034 -0.01015 0.03495 -0.00325 N20 3 0.598530 0.185294 0.110646 11.00000 0.05929 0.04782 = 0.04815 -0.00215 0.03698 0.00508 N21 3 0.678130 0.172960 0.173301 11.00000 0.05830 0.04225 = 0.05042 0.00508 0.03490 0.00941 N22 3 0.782055 0.218911 0.272308 11.00000 0.05380 0.04233 = 0.04279 0.01246 0.03041 0.01058 N23 3 0.800599 0.274968 0.303944 11.00000 0.04029 0.04065 = 0.04472 0.00942 0.02664 0.00927 N24 3 0.833809 0.386904 0.362193 11.00000 0.03605 0.05815 = 0.03772 0.00337 0.01674 0.00186 N25 3 0.428456 0.239555 0.102958 11.00000 0.04918 0.03908 = 0.05871 -0.00074 0.03133 -0.00340 N26 3 0.416667 0.183590 0.104001 11.00000 0.05042 0.04460 = 0.07085 0.00060 0.03629 0.00083 N27 3 0.407072 0.130452 0.105266 11.00000 0.08946 0.04080 = 0.13181 -0.00047 0.07296 -0.00732 N28 3 0.625781 0.329683 0.292156 11.00000 0.03861 0.04440 = 0.04677 0.01062 0.02675 0.00869 N29 3 0.662927 0.296019 0.338284 11.00000 0.04534 0.04904 = 0.05762 0.01148 0.03562 0.00891 N30 3 0.697919 0.263108 0.381867 11.00000 0.06635 0.07288 = 0.07106 0.02875 0.04641 0.01881 N31 3 0.363322 0.440272 0.126101 11.00000 0.04261 0.03848 = 0.03381 0.00147 0.01678 0.00429 N32 3 0.312985 0.487221 0.103210 11.00000 0.04038 0.03650 = 0.03608 -0.00185 0.01732 0.00040 N33 3 0.266686 0.532207 0.081842 11.00000 0.04807 0.04925 = 0.04415 0.00467 0.02065 0.00926 N34 3 0.620882 0.400784 0.129877 11.00000 0.06265 0.04152 = 0.03803 0.00759 0.02449 -0.00068 N35 3 0.657801 0.434536 0.111937 11.00000 0.10153 0.05434 = 0.04366 -0.00089 0.02277 -0.00694 N36 3 0.691117 0.467667 0.094019 11.00000 0.19027 0.08205 = 0.06461 -0.00124 0.07653 -0.06965 N37 3 0.951484 -0.002991 0.100305 11.00000 0.14094 0.09166 = 0.09687 0.01630 0.05267 0.02048 N38 3 0.103315 0.256631 0.188433 11.00000 0.22445 0.19218 = 0.27568 0.05477 0.21073 0.02666 C1 1 0.120458 0.355948 0.076494 11.00000 0.03414 0.04838 = 0.04585 -0.00187 0.01970 -0.01013 AFIX 43 H1 2 0.160586 0.330628 0.114149 11.00000 -1.20000 AFIX 0 C2 1 0.030716 0.372990 0.058034 11.00000 0.04243 0.05920 = 0.05843 -0.00638 0.02655 -0.00014 AFIX 43 H2 2 0.008652 0.359659 0.081475 11.00000 -1.20000 AFIX 0 C3 1 -0.027960 0.410767 0.003434 11.00000 0.03711 0.05522 = 0.06308 -0.01048 0.02454 -0.00082 AFIX 43 H3A 2 -0.092155 0.423161 -0.012060 11.00000 -1.20000 AFIX 0 C4 1 0.008064 0.429436 -0.027050 11.00000 0.04461 0.04155 = 0.04932 -0.00948 0.01971 0.00599 AFIX 43 H4 2 -0.030463 0.455964 -0.063916 11.00000 -1.20000 AFIX 0 C5 1 0.101391 0.410067 -0.004822 11.00000 0.03600 0.04216 = 0.04075 -0.00647 0.01532 -0.00149 C6 1 0.143798 0.431363 -0.035948 11.00000 0.04347 0.04750 = 0.03123 -0.00499 0.01527 -0.00377 C7 1 0.095127 0.479850 -0.087510 11.00000 0.05274 0.07993 = 0.04141 0.01054 0.02513 0.01995 AFIX 137 H7A 2 0.145251 0.506593 -0.083445 11.00000 -1.50000 H7B 2 0.052229 0.506524 -0.083849 11.00000 -1.50000 H7C 2 0.055646 0.458566 -0.129406 11.00000 -1.50000 AFIX 0 C8 1 0.352905 0.388706 -0.017658 11.00000 0.04763 0.05447 = 0.03069 -0.00140 0.01745 -0.00512 C9 1 0.525060 0.433019 -0.070400 11.00000 0.07589 0.07308 = 0.05768 0.01965 0.04700 0.00496 AFIX 137 H9A 2 0.456719 0.447646 -0.095033 11.00000 -1.50000 H9B 2 0.536259 0.416005 -0.099839 11.00000 -1.50000 H9C 2 0.569805 0.468898 -0.046321 11.00000 -1.50000 AFIX 0 C10 1 0.544096 0.381593 -0.024343 11.00000 0.05897 0.05327 = 0.03801 -0.00408 0.03161 -0.01041 C11 1 0.633969 0.344154 0.009189 11.00000 0.05993 0.05396 = 0.04522 -0.00926 0.03352 -0.01421 C12 1 0.700238 0.349461 -0.004738 11.00000 0.06457 0.06494 = 0.06154 -0.00216 0.04355 -0.01418 AFIX 43 H12 2 0.688425 0.380023 -0.035259 11.00000 -1.20000 AFIX 0 C13 1 0.781694 0.310910 0.025357 11.00000 0.05141 0.09155 = 0.07677 -0.00222 0.04238 -0.00716 AFIX 43 H13 2 0.826531 0.313959 0.016019 11.00000 -1.20000 AFIX 0 C14 1 0.796398 0.267149 0.070070 11.00000 0.05480 0.07986 = 0.06736 0.00379 0.03441 0.00252 AFIX 43 H14 2 0.852275 0.239868 0.092165 11.00000 -1.20000 AFIX 0 C15 1 0.731473 0.263696 0.081775 11.00000 0.04671 0.05540 = 0.04135 0.00398 0.02389 0.00419 AFIX 43 H15A 2 0.743041 0.233095 0.112196 11.00000 -1.20000 AFIX 0 C16 1 0.286007 0.435110 0.233917 11.00000 0.04320 0.06063 = 0.05108 0.00674 0.02751 -0.00489 AFIX 43 H16 2 0.291273 0.390201 0.239923 11.00000 -1.20000 AFIX 0 C17 1 0.205746 0.464785 0.222098 11.00000 0.04283 0.09600 = 0.07187 0.00029 0.03550 0.00038 AFIX 43 H17 2 0.155802 0.440730 0.218343 11.00000 -1.20000 AFIX 0 C18 1 0.198834 0.527923 0.215952 11.00000 0.04374 0.08915 = 0.07964 -0.01677 0.03471 0.00728 AFIX 43 H18 2 0.143977 0.549319 0.208292 11.00000 -1.20000 AFIX 0 C19 1 0.270783 0.562306 0.220644 11.00000 0.04540 0.06165 = 0.06105 -0.01789 0.02319 0.01229 AFIX 43 H19 2 0.266917 0.607470 0.217058 11.00000 -1.20000 AFIX 0 C20 1 0.349061 0.529753 0.230713 11.00000 0.03874 0.06476 = 0.03831 -0.00998 0.01731 0.00724 C21 1 0.426787 0.563910 0.233915 11.00000 0.04369 0.04478 = 0.04202 -0.00846 0.02180 0.00498 C22 1 0.423598 0.634443 0.227453 11.00000 0.05520 0.04797 = 0.08889 -0.00785 0.03925 0.00495 AFIX 137 H22A 2 0.410457 0.653717 0.255157 11.00000 -1.50000 H22B 2 0.371179 0.646331 0.182692 11.00000 -1.50000 H22C 2 0.487056 0.649796 0.240246 11.00000 -1.50000 AFIX 0 C23 1 0.625933 0.514482 0.247347 11.00000 0.03922 0.03250 = 0.04225 -0.00114 0.02359 -0.00404 C24 1 0.840085 0.565734 0.230982 11.00000 0.11967 0.06165 = 0.19085 0.00352 0.12511 -0.00766 AFIX 137 H24A 2 0.781734 0.582380 0.190109 11.00000 -1.50000 H24B 2 0.895965 0.565080 0.230103 11.00000 -1.50000 H24C 2 0.855834 0.593141 0.266174 11.00000 -1.50000 AFIX 0 C25 1 0.819942 0.499890 0.240933 11.00000 0.05016 0.05078 = 0.07268 -0.00458 0.03861 -0.00721 C26 1 0.871868 0.444261 0.238835 11.00000 0.05010 0.05757 = 0.05311 0.00789 0.03379 0.00103 C27 1 0.945825 0.454183 0.234186 11.00000 0.06110 0.07014 = 0.08137 0.02334 0.05180 0.01215 AFIX 43 H27 2 0.967836 0.495908 0.234816 11.00000 -1.20000 AFIX 0 C28 1 0.987275 0.400124 0.228484 11.00000 0.06944 0.10214 = 0.08593 0.01410 0.06213 0.01007 AFIX 43 H28 2 1.039457 0.405039 0.225955 11.00000 -1.20000 AFIX 0 C29 1 0.954804 0.341764 0.226536 11.00000 0.05970 0.08128 = 0.05684 0.02002 0.04423 0.01817 AFIX 43 H29 2 0.980350 0.305204 0.220195 11.00000 -1.20000 AFIX 0 C30 1 0.884898 0.336452 0.233827 11.00000 0.05732 0.05415 = 0.05054 0.01216 0.03752 0.01553 AFIX 43 H30 2 0.864589 0.294754 0.235032 11.00000 -1.20000 AFIX 0 C31 1 0.164840 0.259983 -0.068493 11.00000 0.04457 0.04677 = 0.04368 -0.00452 0.02438 -0.00758 AFIX 43 H31 2 0.181253 0.298224 -0.079158 11.00000 -1.20000 AFIX 0 C32 1 0.107058 0.216669 -0.115437 11.00000 0.06441 0.08233 = 0.04176 -0.01245 0.02229 -0.01574 AFIX 43 H32 2 0.081225 0.225452 -0.158431 11.00000 -1.20000 AFIX 0 C33 1 0.085980 0.159518 -0.100235 11.00000 0.05880 0.06022 = 0.05325 -0.01525 0.02220 -0.01826 AFIX 43 H33 2 0.047047 0.128000 -0.132226 11.00000 -1.20000 AFIX 0 C34 1 0.122696 0.149341 -0.037692 11.00000 0.05527 0.04454 = 0.06238 -0.01033 0.03253 -0.01318 AFIX 43 H34 2 0.109279 0.110480 -0.026007 11.00000 -1.20000 AFIX 0 C35 1 0.179159 0.195888 0.008033 11.00000 0.03748 0.05483 = 0.03996 -0.00253 0.01827 -0.00134 C36 1 0.217152 0.186401 0.075441 11.00000 0.03647 0.04601 = 0.04791 -0.00396 0.01955 -0.00549 C37 1 0.202552 0.127942 0.098920 11.00000 0.06413 0.04255 = 0.05290 -0.00311 0.02358 -0.01504 AFIX 137 H37A 2 0.265964 0.106347 0.129055 11.00000 -1.50000 H37B 2 0.157076 0.099640 0.062599 11.00000 -1.50000 H37C 2 0.174852 0.138748 0.120808 11.00000 -1.50000 AFIX 0 C38 1 0.364021 0.280261 0.212031 11.00000 0.03539 0.03715 = 0.04275 -0.00124 0.02113 -0.00298 C39 1 0.531265 0.274268 0.404475 11.00000 0.08679 0.06911 = 0.04490 0.01281 0.04088 -0.00054 AFIX 137 H39A 2 0.491727 0.238896 0.375338 11.00000 -1.50000 H39B 2 0.506870 0.286329 0.428104 11.00000 -1.50000 H39C 2 0.600310 0.260984 0.434891 11.00000 -1.50000 AFIX 0 C40 1 0.523626 0.328938 0.367263 11.00000 0.03914 0.05450 = 0.03152 0.00502 0.01869 0.00057 C41 1 0.582732 0.386398 0.399118 11.00000 0.04928 0.05664 = 0.04032 0.00217 0.02533 0.00498 C42 1 0.636541 0.394998 0.463210 11.00000 0.06223 0.07558 = 0.03651 -0.00302 0.02430 -0.01351 AFIX 43 H42 2 0.637713 0.362960 0.489017 11.00000 -1.20000 AFIX 0 C43 1 0.691298 0.452136 0.491781 11.00000 0.06858 0.08964 = 0.03541 -0.00526 0.01807 -0.00273 AFIX 43 H43 2 0.729039 0.459345 0.536640 11.00000 -1.20000 AFIX 0 C44 1 0.687993 0.495131 0.453727 11.00000 0.05801 0.06281 = 0.04283 -0.01394 0.01871 -0.00588 AFIX 43 H44 2 0.723947 0.533790 0.471432 11.00000 -1.20000 AFIX 0 C45 1 0.633665 0.484252 0.389772 11.00000 0.05491 0.04713 = 0.03953 -0.00469 0.02489 -0.00303 AFIX 43 H45 2 0.632891 0.516078 0.363955 11.00000 -1.20000 AFIX 0 C46 1 0.364065 0.228371 -0.067883 11.00000 0.04934 0.09264 = 0.05404 -0.01032 0.02947 -0.01313 AFIX 43 H46 2 0.346931 0.272078 -0.078259 11.00000 -1.20000 AFIX 0 C47 1 0.308565 0.186907 -0.114196 11.00000 0.08948 0.12538 = 0.09399 -0.03356 0.05582 -0.00661 AFIX 43 H47 2 0.251844 0.200472 -0.155119 11.00000 -1.20000 AFIX 0 C48 1 0.333178 0.125941 -0.102748 11.00000 0.11781 0.17424 = 0.08813 -0.08168 0.04708 -0.05260 AFIX 43 H48 2 0.296265 0.095660 -0.136432 11.00000 -1.20000 AFIX 0 C49 1 0.415667 0.105149 -0.039477 11.00000 0.11723 0.10349 = 0.10553 -0.05241 0.06923 -0.03879 AFIX 43 H49 2 0.432587 0.061356 -0.029610 11.00000 -1.20000 AFIX 0 C50 1 0.469985 0.153402 0.007061 11.00000 0.08213 0.09696 = 0.06246 -0.03328 0.04938 -0.02521 C51 1 0.554552 0.136180 0.072494 11.00000 0.08269 0.06304 = 0.07033 -0.02310 0.05246 0.00149 C52 1 0.584411 0.070355 0.094623 11.00000 0.12391 0.05312 = 0.09094 -0.02109 0.06128 -0.00768 AFIX 137 H52A 2 0.649143 0.062435 0.105587 11.00000 -1.50000 H52B 2 0.535957 0.041050 0.060457 11.00000 -1.50000 H52C 2 0.588132 0.063493 0.132646 11.00000 -1.50000 AFIX 0 C53 1 0.707022 0.225304 0.209473 11.00000 0.04314 0.03795 = 0.04800 0.00453 0.03110 0.00381 C54 1 0.916412 0.215762 0.403001 11.00000 0.06799 0.06556 = 0.05953 0.02465 0.02876 0.02047 AFIX 137 H54A 2 0.868716 0.182146 0.391725 11.00000 -1.50000 H54B 2 0.956114 0.225158 0.448984 11.00000 -1.50000 H54C 2 0.959579 0.201410 0.393029 11.00000 -1.50000 AFIX 0 C55 1 0.863385 0.273914 0.365710 11.00000 0.04249 0.05187 = 0.04275 0.00911 0.02670 0.00717 C56 1 0.877378 0.334440 0.398036 11.00000 0.03923 0.06030 = 0.04280 0.00167 0.02195 0.00352 C57 1 0.930214 0.336768 0.464589 11.00000 0.05124 0.08728 = 0.04326 0.00682 0.01247 0.00966 AFIX 43 H57 2 0.960499 0.299589 0.490179 11.00000 -1.20000 AFIX 0 C58 1 0.937198 0.394633 0.492150 11.00000 0.06790 0.12618 = 0.04191 -0.01846 0.01683 0.00329 AFIX 43 H58 2 0.972146 0.397136 0.537232 11.00000 -1.20000 AFIX 0 C59 1 0.894944 0.447771 0.455807 11.00000 0.05317 0.08075 = 0.05051 -0.01355 0.01816 0.00665 AFIX 43 H59 2 0.899929 0.487705 0.474552 11.00000 -1.20000 AFIX 0 C60 1 0.845282 0.441855 0.391699 11.00000 0.04941 0.05137 = 0.04593 -0.00586 0.02278 -0.00201 AFIX 43 H60 2 0.816768 0.479166 0.366055 11.00000 -1.20000 AFIX 0 C61 1 0.939421 0.041337 0.109331 11.00000 0.15227 0.13677 = 0.12031 0.00532 0.04145 0.01198 C62 1 0.926089 0.113640 0.116197 11.00000 0.15846 0.16152 = 0.13876 0.00118 0.04478 0.01268 AFIX 137 H62A 2 0.983879 0.137342 0.127677 11.00000 -1.50000 H62B 2 0.919021 0.119251 0.149874 11.00000 -1.50000 H62C 2 0.866995 0.129718 0.075351 11.00000 -1.50000 HKLF 4 REM _3 REM R1 = 0.0635 for 14814 Fo > 4sig(Fo) and 0.0666 for all 15622 data REM 1046 parameters refined using 36 restraints END WGHT 0.1029 39.4243 REM Highest difference peak 3.045, deepest hole -2.944, 1-sigma level 0.194 Q1 1 0.8231 -0.0123 0.1520 11.00000 0.05 1.64 Q2 1 0.8031 0.1064 0.1550 11.00000 0.05 1.63 Q3 1 0.4890 0.3453 0.2441 11.00000 0.05 1.58 Q4 1 0.5413 0.3588 0.0865 11.00000 0.05 1.51 Q5 1 0.9434 0.0889 0.2452 11.00000 0.05 1.42 Q6 1 0.3193 0.2760 0.0820 11.00000 0.05 1.37 Q7 1 0.9556 0.1479 0.3169 11.00000 0.05 1.34 Q8 1 0.6965 0.4332 0.2454 11.00000 0.05 1.33 Q9 1 0.8190 0.0468 0.1697 11.00000 0.05 1.18 Q10 1 0.9070 0.4040 0.2438 11.00000 0.05 1.15 Q11 1 0.6640 0.3191 0.2365 11.00000 0.05 1.11 Q12 1 0.3204 0.4805 0.0811 11.00000 0.05 1.09 Q13 1 0.8611 0.2943 0.4015 11.00000 0.05 1.07 Q14 1 0.5060 0.2468 0.0879 11.00000 0.05 1.04 Q15 1 0.5498 0.2497 0.0742 11.00000 0.05 1.02 Q16 1 0.6571 0.3329 0.4043 11.00000 0.05 1.01 Q17 1 0.1138 0.2984 0.0800 11.00000 0.05 1.01 Q18 1 0.2800 0.1693 -0.0672 11.00000 0.05 0.94 Q19 1 0.9180 0.1956 0.2306 11.00000 0.05 0.93 Q20 1 0.3509 0.4617 -0.0911 11.00000 0.05 0.93 Q21 1 0.8979 -0.0010 0.1256 11.00000 0.05 0.93 Q22 1 0.5313 0.4435 0.0807 11.00000 0.05 0.90 Q23 1 0.1849 0.2204 0.2969 11.00000 0.05 0.88 Q24 1 0.4718 0.1090 -0.0806 11.00000 0.05 0.88 Q25 1 1.0291 0.1572 0.2984 11.00000 0.05 0.86 ;