# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_Revised _database_code_depnum_ccdc_archive 'CCDC 910738' _vrf_PLAT413_1_Revised ; PROBLEM: Short Inter XH3 .. XHn H56B .. H82A RESPONSE: H-atoms were introduced in calculated positions and refined on a riding model. H82A is a half-occupancy methyl proton. ; _vrf_CHEMW03_1_Revised ; 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. 8 H2O molecules and 0.5 Et3NH that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_DIFMX01_1_Revised ; PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 RESPONSE: From shelxl.lst Electron density synthesis with coefficients Fo-Fc Highest peak 12.76 at 0.1457 0.1838 0.4139 [ 0.51 A from C37 ] Deepest hole -2.63 at 0.4852 0.1521 0.2717 [ 0.76 A from GD6 ] ; _vrf_PLAT094_1_Revised ; PROBLEM: Ratio of Maximum / Minimum Residual Density ... RESPONSE: From shelxl.lst Electron density synthesis with coefficients Fo-Fc Highest peak 12.76 at 0.1457 0.1838 0.4139 [ 0.51 A from C37 ] Deepest hole -2.63 at 0.4852 0.1521 0.2717 [ 0.76 A from GD6 ] ; _vrf_PLAT097_1_Revised ; PROBLEM: Large Reported Max. (Positive) Residual Density RESPONSE: From shelxl.lst Electron density synthesis with coefficients Fo-Fc Highest peak 12.76 at 0.1457 0.1838 0.4139 [ 0.51 A from C37 ] Deepest hole -2.63 at 0.4852 0.1521 0.2717 [ 0.76 A from GD6 ] ; _vrf_DIFMX02_1_Revised ; PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 RESPONSE: From shelxl.lst Electron density synthesis with coefficients Fo-Fc Highest peak 12.76 at 0.1457 0.1838 0.4139 [ 0.51 A from C37 ] Deepest hole -2.63 at 0.4852 0.1521 0.2717 [ 0.76 A from GD6 ] ; _vrf_PLAT041_1_Revised ; 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. 8 H2O molecules and 0.5 Et3NH that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT068_1_Revised ; 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. 8 H2O molecules and 0.5 Et3NH that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_FORMU01_1_Revised ; 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. 8 H2O molecules and 0.5 Et3NH that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_CELLZ01_1_Revised ; 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. 8 H2O molecules and 0.5 Et3NH that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT002_1_Revised ; PROBLEM: Number of Distance or Angle Restraints on AtSite RESPONSE: Please see refine_special_details for information. ; _vrf_PLAT003_1_Revised ; PROBLEM: Number of Uiso or Uij Restrained Atom Sites .... RESPONSE: Please see refine_special_details for information. ; _vrf_PLAT007_1_Revised ; PROBLEM: Note: Number of Unrefined D-H Atoms ............ 7 RESPONSE: These H-atoms were introduced in calculated postions and refined using AFIX 147 for O-H, or as methine H-atom in the case of the Et3N-H. ; _vrf_PLAT606_1_Revised ; 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_PLAT860_1_Revised ; PROBLEM: Note: Number of Least-Squares Restraints ....... RESPONSE: Please see refine_special_details for information. ; _vrf_PLAT869_1_Revised ; 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. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H100 Gd6 N19 O45' _chemical_formula_sum 'C84 H100 Gd6 N19 O45' _chemical_formula_weight 3039.31 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' Gd Gd -0.1653 3.9035 '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' _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 17.8448(13) _cell_length_b 18.4743(14) _cell_length_c 20.2807(15) _cell_angle_alpha 80.002(6) _cell_angle_beta 68.785(5) _cell_angle_gamma 75.752(5) _cell_volume 6014.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 39802 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2962 _exptl_absorpt_coefficient_mu 3.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.413 _exptl_absorpt_correction_T_max 0.668 _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 51765 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.50 _reflns_number_total 24712 _reflns_number_gt 20749 _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. SIMU, DFIX, DANG and FLAT restraints were applied to the ring consisting of C35-C40 and to a ligand fragment consisting of [C49 C50 C52 N13 N14]. ISOR restraints were applied to C37 and C52. SIMU and DFIX restraints were also applied to the lattice protonated triethylamine. The nominal formula is: (L-2H)6Gd6(CH3COO)6(O)(Et3NH)(H2O)8 Which is in agreement with the dried elemental analysis results: [Gd6(C11H11N3O4)6(O)(CH3COO)6]((CH3CH2)3NH): Calc: C, 34.66; H, 3.46 ; N, 9.14. Found: C, 34.78; H, 3.34; N, 9.22 Note that only 0.5 of the triethylamine cation could be located from difference maps, and that significant disorder was observed outside the main molecular fragment. For further details, see platon_squeeze_details and iucr_refine_instructions_details. ; _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^)+(0.1358P)^2^+122.7354P] 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 24712 _refine_ls_number_parameters 1341 _refine_ls_number_restraints 182 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0925 _refine_ls_wR_factor_ref 0.2571 _refine_ls_wR_factor_gt 0.2478 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.060 _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 0.454 0.139 47 14 ' ' 2 0.006 0.546 0.861 47 14 ' ' 3 0.500 0.500 0.500 1059 242 ' ' 4 0.324 0.547 0.787 26 6 ' ' 5 0.676 0.453 0.213 25 4 ' ' _platon_squeeze_details ; The Platon SQUEEZE procedure was applied to recover 270 electrons per unit cell in three voids that were sufficiently large to contain a small molecule (total volume 1153 ^A^3); that is 135 electrons per formula unit. Void 1 and 2 are considered to each contain a water molecule (10 electrons; one water molecule per formula unit), while void 4 is sufficiently large, and contains enough electrons, to account for the missing 0.5 protonated triethylamine (51 electrons), as well as six additional water molecules. These 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 Gd1 Gd 0.79416(3) -0.20607(3) 0.26596(3) 0.02614(14) Uani 1 1 d . . . Gd2 Gd 0.87117(3) -0.02007(3) 0.25063(3) 0.01988(13) Uani 1 1 d . . . Gd3 Gd 0.93281(3) 0.17412(3) 0.23392(3) 0.02175(14) Uani 1 1 d . . . Gd4 Gd 0.63642(3) -0.01978(3) 0.25080(3) 0.02098(13) Uani 1 1 d . . . Gd5 Gd 0.71022(3) 0.18256(3) 0.23389(3) 0.02327(14) Uani 1 1 d . . . Gd6 Gd 0.49087(3) 0.17472(3) 0.23585(3) 0.02677(15) Uani 1 1 d . . . O1 O 0.6414(6) -0.3428(7) 0.1988(7) 0.062(3) Uani 1 1 d D . . O2 O 0.7514(5) -0.2737(5) 0.2087(5) 0.040(2) Uani 1 1 d . . . O3 O 0.9115(4) -0.1488(4) 0.2289(4) 0.0262(16) Uani 1 1 d . . . O4 O 1.0890(5) -0.0282(6) 0.1543(5) 0.042(2) Uani 1 1 d . . . H4 H 1.1212 -0.0465 0.1773 0.050 Uiso 1 1 calc R . . O5 O 1.2095(5) 0.0463(5) 0.1696(5) 0.043(2) Uani 1 1 d D . . O6 O 1.0658(4) 0.1293(5) 0.1757(4) 0.0305(17) Uani 1 1 d . . . O7 O 0.8231(4) 0.2458(4) 0.1933(4) 0.0248(15) Uani 1 1 d . . . O8 O 0.6383(7) 0.3315(6) 0.1185(8) 0.066(4) Uani 1 1 d . . . H8 H 0.5944 0.3239 0.1502 0.079 Uiso 1 1 calc R . . O9 O 0.4580(10) 0.4318(8) 0.1537(12) 0.107(6) Uani 1 1 d DU . . O10 O 0.4710(7) 0.2859(5) 0.1712(6) 0.052(3) Uani 1 1 d . . . O11 O 0.5259(4) 0.0472(4) 0.2103(4) 0.0211(14) Uani 1 1 d . . . O12 O 0.6185(5) -0.1632(5) 0.1591(5) 0.0352(19) Uani 1 1 d . . . H12 H 0.6498 -0.1855 0.1820 0.042 Uiso 1 1 calc R . . O13 O 0.2685(5) 0.0467(5) 0.3266(6) 0.043(2) Uani 1 1 d D . . O14 O 0.3765(5) 0.1304(6) 0.3021(5) 0.043(2) Uani 1 1 d . . . O15 O 0.5701(5) 0.2446(5) 0.2641(5) 0.0360(19) Uani 1 1 d . . . O16 O 0.7183(6) 0.3368(7) 0.3174(8) 0.064(4) Uani 1 1 d . . . H16 H 0.7637 0.3073 0.3120 0.077 Uiso 1 1 calc R . . O17 O 0.8571(7) 0.4275(5) 0.2830(6) 0.051(2) Uani 1 1 d D . . O18 O 0.9108(7) 0.2851(5) 0.2794(5) 0.044(2) Uani 1 1 d . . . O19 O 0.9519(4) 0.0454(4) 0.2808(4) 0.0241(15) Uani 1 1 d . . . O20 O 0.9542(5) -0.1672(4) 0.3637(5) 0.0351(19) Uani 1 1 d . . . H20 H 0.9393 -0.1901 0.3397 0.042 Uiso 1 1 calc R . . O21 O 1.0106(7) -0.3410(8) 0.3586(7) 0.069(3) Uani 1 1 d DU . . O22 O 0.8673(6) -0.2753(5) 0.3336(5) 0.045(2) Uani 1 1 d . . . O23 O 0.6516(4) -0.1492(4) 0.2948(4) 0.0280(17) Uani 1 1 d . . . O24 O 0.4233(5) -0.0294(6) 0.3496(6) 0.044(2) Uani 1 1 d . . . H24 H 0.4209 0.0099 0.3218 0.053 Uiso 1 1 calc R . . O25 O 0.7761(4) -0.0992(4) 0.3292(4) 0.0269(16) Uani 1 1 d . . . O26 O 0.6464(5) -0.0363(5) 0.3718(5) 0.0327(18) Uani 1 1 d . . . O27 O 0.7656(4) -0.0970(4) 0.1843(4) 0.0248(15) Uani 1 1 d . . . O28 O 0.8674(5) -0.0349(4) 0.1327(4) 0.0290(17) Uani 1 1 d . . . O29 O 0.7954(4) 0.0363(5) 0.3646(4) 0.0295(17) Uani 1 1 d . . . O30 O 0.7958(4) 0.1542(4) 0.3102(4) 0.0255(16) Uani 1 1 d . . . O31 O 0.9031(4) 0.0911(4) 0.1694(4) 0.0243(15) Uani 1 1 d . . . O32 O 0.8104(4) 0.1426(4) 0.1164(4) 0.0285(16) Uani 1 1 d . . . O33 O 0.6366(4) 0.1542(4) 0.1627(4) 0.0277(16) Uani 1 1 d . . . O34 O 0.6869(4) 0.0391(5) 0.1274(4) 0.0284(17) Uani 1 1 d . . . O35 O 0.6277(5) 0.1408(5) 0.3586(5) 0.0345(19) Uani 1 1 d . . . O36 O 0.5579(4) 0.0897(4) 0.3145(4) 0.0265(16) Uani 1 1 d . . . O37 O 0.7388(4) 0.0470(4) 0.2441(5) 0.0294(18) Uani 1 1 d . . . N1 N 0.9165(6) -0.2592(6) 0.1631(5) 0.032(2) Uani 1 1 d . . . N2 N 0.9890(6) -0.2308(6) 0.1446(5) 0.030(2) Uani 1 1 d . . . N3 N 1.0253(5) -0.0668(5) 0.1765(5) 0.0254(19) Uani 1 1 d . . . N4 N 0.9736(6) 0.2520(5) 0.1155(5) 0.0265(19) Uani 1 1 d . . . N5 N 0.9113(6) 0.2976(6) 0.0907(6) 0.034(2) Uani 1 1 d . . . N6 N 0.7035(6) 0.2982(6) 0.1421(6) 0.037(2) Uani 1 1 d . . . N7 N 0.4709(6) 0.1501(6) 0.1246(6) 0.033(2) Uani 1 1 d . . . N8 N 0.4852(6) 0.0754(6) 0.1103(5) 0.030(2) Uani 1 1 d . . . N9 N 0.5910(5) -0.0891(5) 0.1745(5) 0.0272(19) Uani 1 1 d . . . N10 N 0.4166(6) 0.2536(6) 0.3372(6) 0.036(2) Uani 1 1 d . . . N11 N 0.4578(7) 0.3017(7) 0.3541(8) 0.052(3) Uani 1 1 d . . . N12 N 0.6652(6) 0.3013(6) 0.3030(7) 0.044(3) Uani 1 1 d . . . N13 N 0.9622(5) 0.1470(5) 0.3502(5) 0.0284(17) Uani 1 1 d DU . . N14 N 0.9805(6) 0.0701(6) 0.3763(5) 0.030(2) Uani 1 1 d D . . N15 N 0.9474(5) -0.0915(5) 0.3378(5) 0.028(2) Uani 1 1 d . . . N16 N 0.6962(6) -0.2608(6) 0.3788(5) 0.030(2) Uani 1 1 d . . . N17 N 0.6116(6) -0.2320(6) 0.3952(6) 0.036(2) Uani 1 1 d . . . N18 N 0.5049(5) -0.0683(5) 0.3333(5) 0.028(2) Uani 1 1 d . . . C1 C 0.5785(15) -0.371(2) 0.1917(16) 0.126(12) Uani 1 1 d D . . H1A H 0.5538 -0.3355 0.1597 0.151 Uiso 1 1 calc R . . H1B H 0.5366 -0.3766 0.2384 0.151 Uiso 1 1 calc R . . H1C H 0.6013 -0.4194 0.1722 0.151 Uiso 1 1 calc R . . C2 C 0.7217(8) -0.3637(7) 0.1574(7) 0.039(3) Uani 1 1 d . . . C3 C 0.7469(10) -0.4194(8) 0.1124(8) 0.048(3) Uani 1 1 d . . . H3 H 0.7082 -0.4439 0.1079 0.058 Uiso 1 1 calc R . . C4 C 0.8318(11) -0.4395(9) 0.0726(8) 0.057(4) Uani 1 1 d . . . H4A H 0.8496 -0.4775 0.0410 0.069 Uiso 1 1 calc R . . C5 C 0.8883(10) -0.4052(7) 0.0792(7) 0.043(3) Uani 1 1 d . . . H5 H 0.9449 -0.4199 0.0530 0.051 Uiso 1 1 calc R . . C6 C 0.8619(8) -0.3482(6) 0.1247(7) 0.033(3) Uani 1 1 d . . . C7 C 0.7788(8) -0.3271(7) 0.1658(7) 0.036(3) Uani 1 1 d . . . C8 C 0.9260(8) -0.3115(6) 0.1243(7) 0.036(3) Uani 1 1 d . . . H8A H 0.9797 -0.3277 0.0925 0.043 Uiso 1 1 calc R . . C9 C 0.9788(7) -0.1743(7) 0.1787(7) 0.031(2) Uani 1 1 d . . . C10 C 1.0475(6) -0.1331(7) 0.1570(6) 0.028(2) Uani 1 1 d . . . C11 C 1.1329(8) -0.1680(9) 0.1166(7) 0.045(3) Uani 1 1 d . . . H11A H 1.1384 -0.1674 0.0666 0.054 Uiso 1 1 calc R . . H11B H 1.1457 -0.2200 0.1365 0.054 Uiso 1 1 calc R . . H11C H 1.1710 -0.1397 0.1199 0.054 Uiso 1 1 calc R . . C12 C 1.2844(8) -0.0079(10) 0.1581(11) 0.068(5) Uani 1 1 d D . . H12A H 1.3047 -0.0214 0.1092 0.081 Uiso 1 1 calc R . . H12B H 1.2746 -0.0528 0.1911 0.081 Uiso 1 1 calc R . . H12C H 1.3253 0.0133 0.1661 0.081 Uiso 1 1 calc R . . C13 C 1.2097(7) 0.1087(7) 0.1213(7) 0.032(3) Uani 1 1 d . . . C14 C 1.2793(7) 0.1293(6) 0.0705(7) 0.035(3) Uani 1 1 d . . . H14 H 1.3318 0.0991 0.0668 0.042 Uiso 1 1 calc R . . C15 C 1.2725(8) 0.1931(8) 0.0257(8) 0.045(3) Uani 1 1 d . . . H15 H 1.3207 0.2088 -0.0065 0.054 Uiso 1 1 calc R . . C16 C 1.1963(7) 0.2353(8) 0.0264(7) 0.036(3) Uani 1 1 d . . . H16A H 1.1927 0.2778 -0.0070 0.043 Uiso 1 1 calc R . . C17 C 1.1230(7) 0.2147(7) 0.0775(6) 0.033(3) Uani 1 1 d . . . C18 C 1.1278(7) 0.1511(6) 0.1269(6) 0.028(2) Uani 1 1 d . . . C19 C 1.0469(7) 0.2570(7) 0.0730(6) 0.029(2) Uani 1 1 d . . . H19A H 1.0500 0.2940 0.0337 0.035 Uiso 1 1 calc R . . C20 C 0.8400(7) 0.2876(6) 0.1333(7) 0.031(2) Uani 1 1 d . . . C21 C 0.7702(8) 0.3248(7) 0.1075(8) 0.039(3) Uani 1 1 d . . . C22 C 0.7811(11) 0.3781(10) 0.0403(11) 0.074(6) Uani 1 1 d . . . H22A H 0.7609 0.3607 0.0081 0.089 Uiso 1 1 calc R . . H22B H 0.8394 0.3796 0.0170 0.089 Uiso 1 1 calc R . . H22C H 0.7501 0.4285 0.0525 0.089 Uiso 1 1 calc R . . C23 C 0.469(2) 0.5056(13) 0.135(2) 0.157(11) Uani 1 1 d DU . . H23A H 0.4170 0.5387 0.1351 0.189 Uiso 1 1 calc R . . H23B H 0.5103 0.5096 0.0880 0.189 Uiso 1 1 calc R . . H23C H 0.4876 0.5204 0.1701 0.189 Uiso 1 1 calc R . . C24 C 0.4429(10) 0.3970(9) 0.1021(11) 0.060(4) Uani 1 1 d U . . C25 C 0.4233(15) 0.4350(12) 0.0425(14) 0.090(6) Uani 1 1 d U . . H25 H 0.4183 0.4879 0.0335 0.108 Uiso 1 1 calc R . . C26 C 0.4111(17) 0.3936(13) -0.0039(15) 0.099(6) Uani 1 1 d U . . H26 H 0.3983 0.4195 -0.0444 0.119 Uiso 1 1 calc R . . C27 C 0.4172(15) 0.3177(11) 0.0075(12) 0.082(5) Uani 1 1 d U . . H27 H 0.4050 0.2912 -0.0223 0.098 Uiso 1 1 calc R . . C28 C 0.4432(10) 0.2782(9) 0.0675(9) 0.052(3) Uani 1 1 d U . . C29 C 0.4532(8) 0.3180(8) 0.1166(9) 0.045(3) Uani 1 1 d U . . C30 C 0.4570(10) 0.1975(8) 0.0712(8) 0.048(4) Uani 1 1 d . . . H30 H 0.4560 0.1766 0.0321 0.058 Uiso 1 1 calc R . . C31 C 0.5154(6) 0.0291(6) 0.1547(6) 0.025(2) Uani 1 1 d . . . C32 C 0.5437(6) -0.0529(7) 0.1407(6) 0.026(2) Uani 1 1 d . . . C33 C 0.5187(9) -0.0790(8) 0.0871(8) 0.048(4) Uani 1 1 d . . . H33A H 0.5652 -0.0849 0.0427 0.058 Uiso 1 1 calc R . . H33B H 0.4728 -0.0420 0.0782 0.058 Uiso 1 1 calc R . . H33C H 0.5018 -0.1273 0.1054 0.058 Uiso 1 1 calc R . . C34 C 0.2155(9) -0.0057(9) 0.3475(10) 0.059(4) Uani 1 1 d D . . H34A H 0.2096 -0.0270 0.3964 0.070 Uiso 1 1 calc R . . H34B H 0.2389 -0.0460 0.3158 0.070 Uiso 1 1 calc R . . H34C H 0.1616 0.0198 0.3446 0.070 Uiso 1 1 calc R . . C35 C 0.2448(5) 0.1089(6) 0.3621(5) 0.036(3) Uani 1 1 d DU . . C36 C 0.1628(6) 0.1269(5) 0.4057(5) 0.051(3) Uani 1 1 d DU . . H36 H 0.1247 0.0958 0.4136 0.061 Uiso 1 1 calc R . . C37 C 0.1412(6) 0.1943(5) 0.4368(5) 0.031(2) Uani 1 1 d DU . . H37 H 0.0858 0.2115 0.4648 0.037 Uiso 1 1 calc R . . C38 C 0.2001(5) 0.2367(6) 0.4272(5) 0.045(3) Uani 1 1 d DU . . H38 H 0.1839 0.2805 0.4516 0.055 Uiso 1 1 calc R . . C39 C 0.2818(5) 0.2175(5) 0.3832(5) 0.035(3) Uani 1 1 d DU . . C40 C 0.3044(5) 0.1512(5) 0.3501(5) 0.030(2) Uani 1 1 d DU . . C41 C 0.3409(7) 0.2617(8) 0.3802(7) 0.038(3) Uani 1 1 d . . . H41 H 0.3226 0.2993 0.4122 0.045 Uiso 1 1 calc R . . C42 C 0.5348(8) 0.2895(7) 0.3158(8) 0.042(3) Uani 1 1 d . . . C43 C 0.5908(9) 0.3299(9) 0.3299(11) 0.065(5) Uani 1 1 d . . . C44 C 0.5546(11) 0.3920(17) 0.3787(18) 0.144(16) Uani 1 1 d . . . H44A H 0.5849 0.3851 0.4119 0.173 Uiso 1 1 calc R . . H44B H 0.4969 0.3906 0.4054 0.173 Uiso 1 1 calc R . . H44C H 0.5586 0.4405 0.3505 0.173 Uiso 1 1 calc R . . C45 C 0.8214(16) 0.5055(9) 0.2863(13) 0.092(7) Uani 1 1 d D . . H45A H 0.8578 0.5312 0.2961 0.111 Uiso 1 1 calc R . . H45B H 0.7681 0.5119 0.3244 0.111 Uiso 1 1 calc R . . H45C H 0.8140 0.5270 0.2409 0.111 Uiso 1 1 calc R . . C46 C 0.8828(7) 0.3939(7) 0.3357(8) 0.055(4) Uani 1 1 d D . . C47 C 0.8781(9) 0.4258(9) 0.3948(8) 0.076(6) Uani 1 1 d D . . H47 H 0.8606 0.4786 0.3964 0.092 Uiso 1 1 calc R . . C48 C 0.8989(9) 0.3817(8) 0.4525(8) 0.084(7) Uani 1 1 d D . . H48 H 0.8951 0.4046 0.4923 0.101 Uiso 1 1 calc R . . C49 C 0.9247(7) 0.3052(7) 0.4503(8) 0.062(5) Uani 1 1 d D . . H49 H 0.9386 0.2762 0.4893 0.074 Uiso 1 1 calc R . . C50 C 0.9315(6) 0.2681(6) 0.3926(6) 0.036(2) Uani 1 1 d DU . . C51 C 0.9098(6) 0.3139(6) 0.3341(6) 0.039(3) Uani 1 1 d D . . C52 C 0.9457(5) 0.1821(6) 0.4058(6) 0.0315(18) Uani 1 1 d DU . . H52 H 0.9427 0.1564 0.4513 0.038 Uiso 1 1 calc R . . C53 C 0.9719(6) 0.0259(6) 0.3391(5) 0.025(2) Uani 1 1 d . . . C54 C 0.9804(7) -0.0559(6) 0.3662(7) 0.031(2) Uani 1 1 d . . . C55 C 1.0204(9) -0.0869(8) 0.4208(8) 0.047(4) Uani 1 1 d . . . H55A H 0.9782 -0.0935 0.4673 0.057 Uiso 1 1 calc R . . H55B H 1.0529 -0.0522 0.4229 0.057 Uiso 1 1 calc R . . H55C H 1.0563 -0.1355 0.4083 0.057 Uiso 1 1 calc R . . C56 C 1.0386(18) -0.3608(18) 0.2874(12) 0.136(10) Uani 1 1 d DU . . H56A H 1.0012 -0.3311 0.2628 0.164 Uiso 1 1 calc R . . H56B H 1.0399 -0.4143 0.2881 0.164 Uiso 1 1 calc R . . H56C H 1.0938 -0.3506 0.2625 0.164 Uiso 1 1 calc R . . C57 C 0.9375(9) -0.3640(7) 0.4012(8) 0.041(3) Uani 1 1 d . . . C58 C 0.9356(10) -0.4161(7) 0.4593(8) 0.047(3) Uani 1 1 d . . . H58 H 0.9850 -0.4381 0.4691 0.057 Uiso 1 1 calc R . . C59 C 0.8625(10) -0.4368(8) 0.5035(8) 0.047(3) Uani 1 1 d . . . H59 H 0.8623 -0.4737 0.5425 0.057 Uiso 1 1 calc R . . C60 C 0.7911(10) -0.4042(7) 0.4909(8) 0.044(3) Uani 1 1 d . . . H60 H 0.7413 -0.4185 0.5212 0.052 Uiso 1 1 calc R . . C61 C 0.7907(8) -0.3482(6) 0.4322(7) 0.035(3) Uani 1 1 d . . . C62 C 0.8643(8) -0.3274(7) 0.3865(7) 0.036(3) Uani 1 1 d . . . C63 C 0.7113(7) -0.3118(6) 0.4278(6) 0.032(2) Uani 1 1 d . . . H63 H 0.6651 -0.3266 0.4644 0.038 Uiso 1 1 calc R . . C64 C 0.5965(7) -0.1745(7) 0.3489(6) 0.027(2) Uani 1 1 d . . . C65 C 0.5103(7) -0.1325(7) 0.3652(6) 0.032(3) Uani 1 1 d . . . C66 C 0.4415(8) -0.1685(10) 0.4174(7) 0.050(4) Uani 1 1 d . . . H66A H 0.4370 -0.1630 0.4660 0.060 Uiso 1 1 calc R . . H66B H 0.4532 -0.2219 0.4106 0.060 Uiso 1 1 calc R . . H66C H 0.3898 -0.1439 0.4094 0.060 Uiso 1 1 calc R . . C67 C 0.7103(7) -0.0755(8) 0.3824(6) 0.033(3) Uani 1 1 d . . . C68 C 0.7132(7) -0.0944(8) 0.4558(6) 0.035(3) Uani 1 1 d . . . H68A H 0.6815 -0.0522 0.4842 0.042 Uiso 1 1 calc R . . H68B H 0.7703 -0.1044 0.4544 0.042 Uiso 1 1 calc R . . H68C H 0.6897 -0.1391 0.4773 0.042 Uiso 1 1 calc R . . C69 C 0.8190(6) -0.0726(6) 0.1282(6) 0.026(2) Uani 1 1 d . . . C70 C 0.8247(8) -0.0906(8) 0.0576(6) 0.037(3) Uani 1 1 d . . . H70A H 0.8444 -0.0508 0.0213 0.044 Uiso 1 1 calc R . . H70B H 0.7704 -0.0945 0.0589 0.044 Uiso 1 1 calc R . . H70C H 0.8630 -0.1384 0.0462 0.044 Uiso 1 1 calc R . . C71 C 0.7831(6) 0.1060(7) 0.3672(6) 0.025(2) Uani 1 1 d . . . C72 C 0.7536(8) 0.1377(8) 0.4379(7) 0.041(3) Uani 1 1 d . . . H72A H 0.7235 0.1037 0.4750 0.050 Uiso 1 1 calc R . . H72B H 0.7174 0.1868 0.4357 0.050 Uiso 1 1 calc R . . H72C H 0.8009 0.1434 0.4490 0.050 Uiso 1 1 calc R . . C73 C 0.8823(6) 0.1115(7) 0.1123(6) 0.026(2) Uani 1 1 d . . . C74 C 0.9465(7) 0.0995(8) 0.0425(6) 0.037(3) Uani 1 1 d . . . H74A H 0.9284 0.0726 0.0153 0.044 Uiso 1 1 calc R . . H74B H 0.9972 0.0698 0.0494 0.044 Uiso 1 1 calc R . . H74C H 0.9564 0.1481 0.0166 0.044 Uiso 1 1 calc R . . C75 C 0.6687(6) 0.1082(7) 0.1138(6) 0.026(2) Uani 1 1 d . . . C76 C 0.6838(8) 0.1410(8) 0.0370(6) 0.039(3) Uani 1 1 d . . . H76A H 0.7253 0.1052 0.0054 0.047 Uiso 1 1 calc R . . H76B H 0.7034 0.1879 0.0298 0.047 Uiso 1 1 calc R . . H76C H 0.6326 0.1511 0.0265 0.047 Uiso 1 1 calc R . . C77 C 0.5694(7) 0.1101(7) 0.3660(6) 0.029(2) Uani 1 1 d . . . C78 C 0.5078(8) 0.0985(9) 0.4391(7) 0.043(3) Uani 1 1 d . . . H78A H 0.5367 0.0787 0.4734 0.052 Uiso 1 1 calc R . . H78B H 0.4756 0.0626 0.4386 0.052 Uiso 1 1 calc R . . H78C H 0.4710 0.1464 0.4529 0.052 Uiso 1 1 calc R . . N19 N 1.1684(14) 0.3578(11) 0.2119(13) 0.056(6) Uani 0.50 1 d PDU . . H19 H 1.1231 0.3598 0.1988 0.067 Uiso 0.50 1 calc PR . . C79 C 1.2046(16) 0.2751(12) 0.2099(17) 0.052(6) Uani 0.50 1 d PDU . . H79A H 1.2219 0.2619 0.1606 0.062 Uiso 0.50 1 calc PR . . H79B H 1.2540 0.2640 0.2243 0.062 Uiso 0.50 1 calc PR . . C80 C 1.1463(17) 0.2282(18) 0.2571(15) 0.057(8) Uani 0.50 1 d PDU . . H80A H 1.1204 0.2476 0.3038 0.069 Uiso 0.50 1 calc PR . . H80B H 1.1759 0.1764 0.2623 0.069 Uiso 0.50 1 calc PR . . H80C H 1.1041 0.2293 0.2364 0.069 Uiso 0.50 1 calc PR . . C81 C 1.126(3) 0.389(2) 0.2820(18) 0.082(9) Uani 0.50 1 d PDU . . H81A H 1.0877 0.3546 0.3058 0.099 Uiso 0.50 1 calc PR . . H81B H 1.1703 0.3714 0.3035 0.099 Uiso 0.50 1 calc PR . . C82 C 1.081(3) 0.457(3) 0.319(3) 0.121(16) Uani 0.50 1 d PDU . . H82A H 1.1092 0.4985 0.2962 0.145 Uiso 0.50 1 calc PR . . H82B H 1.0785 0.4471 0.3689 0.145 Uiso 0.50 1 calc PR . . H82C H 1.0252 0.4698 0.3171 0.145 Uiso 0.50 1 calc PR . . C83 C 1.220(2) 0.3965(19) 0.146(2) 0.091(11) Uani 0.50 1 d PDU . . H83A H 1.2701 0.4012 0.1539 0.110 Uiso 0.50 1 calc PR . . H83B H 1.2378 0.3637 0.1069 0.110 Uiso 0.50 1 calc PR . . C84 C 1.181(3) 0.473(2) 0.121(3) 0.126(18) Uani 0.50 1 d PDU . . H84A H 1.1658 0.4691 0.0799 0.151 Uiso 0.50 1 calc PR . . H84B H 1.2202 0.5065 0.1067 0.151 Uiso 0.50 1 calc PR . . H84C H 1.1321 0.4929 0.1592 0.151 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0200(3) 0.0243(3) 0.0310(3) -0.0021(2) -0.0031(2) -0.0073(2) Gd2 0.0132(2) 0.0238(3) 0.0210(3) -0.00078(19) -0.00240(18) -0.00673(18) Gd3 0.0163(2) 0.0259(3) 0.0246(3) 0.0011(2) -0.00724(19) -0.00888(19) Gd4 0.0123(2) 0.0256(3) 0.0237(3) -0.0067(2) -0.00120(19) -0.00576(18) Gd5 0.0152(2) 0.0259(3) 0.0309(3) -0.0067(2) -0.0075(2) -0.00545(19) Gd6 0.0141(2) 0.0303(3) 0.0376(3) -0.0155(2) -0.0060(2) -0.00286(19) O1 0.040(6) 0.057(7) 0.099(9) -0.025(6) -0.023(6) -0.015(5) O2 0.039(5) 0.040(5) 0.039(5) -0.017(4) 0.000(4) -0.015(4) O3 0.019(3) 0.022(4) 0.035(4) -0.010(3) -0.002(3) -0.006(3) O4 0.020(4) 0.051(6) 0.051(6) -0.006(4) -0.001(4) -0.018(4) O5 0.021(4) 0.034(5) 0.064(6) 0.001(4) -0.007(4) -0.002(3) O6 0.016(3) 0.035(4) 0.038(4) 0.006(3) -0.010(3) -0.005(3) O7 0.020(3) 0.023(4) 0.036(4) 0.001(3) -0.016(3) -0.006(3) O8 0.049(6) 0.049(6) 0.122(11) 0.030(7) -0.069(7) -0.015(5) O9 0.093(10) 0.050(7) 0.206(18) -0.028(10) -0.074(12) -0.018(7) O10 0.073(7) 0.031(5) 0.069(7) -0.016(5) -0.045(6) 0.000(5) O11 0.015(3) 0.027(4) 0.025(4) -0.014(3) -0.008(3) -0.001(3) O12 0.032(4) 0.028(4) 0.052(5) -0.017(4) -0.018(4) -0.002(3) O13 0.028(4) 0.042(5) 0.065(6) -0.018(5) -0.011(4) -0.012(4) O14 0.015(4) 0.054(6) 0.058(6) -0.033(5) 0.001(4) -0.007(4) O15 0.018(4) 0.039(5) 0.047(5) -0.015(4) -0.005(3) 0.000(3) O16 0.030(5) 0.063(7) 0.119(10) -0.052(7) -0.032(6) -0.003(5) O17 0.059(6) 0.040(5) 0.057(6) 0.000(5) -0.022(5) -0.015(5) O18 0.075(7) 0.025(4) 0.045(5) -0.001(4) -0.033(5) -0.015(4) O19 0.023(4) 0.026(4) 0.023(4) 0.003(3) -0.007(3) -0.008(3) O20 0.038(5) 0.023(4) 0.050(5) 0.006(4) -0.027(4) -0.006(3) O21 0.043(6) 0.074(8) 0.077(8) 0.008(7) -0.014(6) -0.010(6) O22 0.033(5) 0.043(5) 0.052(6) 0.014(4) -0.013(4) -0.007(4) O23 0.015(3) 0.025(4) 0.037(4) 0.001(3) 0.000(3) -0.009(3) O24 0.011(4) 0.051(6) 0.062(6) -0.007(5) -0.007(4) -0.002(4) O25 0.017(3) 0.026(4) 0.033(4) -0.007(3) 0.002(3) -0.008(3) O26 0.019(4) 0.038(5) 0.040(5) -0.007(4) -0.005(3) -0.009(3) O27 0.014(3) 0.022(3) 0.034(4) 0.002(3) -0.002(3) -0.007(3) O28 0.025(4) 0.030(4) 0.029(4) 0.001(3) -0.006(3) -0.007(3) O29 0.019(4) 0.036(4) 0.030(4) -0.002(3) -0.001(3) -0.010(3) O30 0.013(3) 0.037(4) 0.027(4) -0.003(3) -0.002(3) -0.013(3) O31 0.024(4) 0.023(4) 0.027(4) 0.004(3) -0.010(3) -0.008(3) O32 0.020(4) 0.031(4) 0.036(4) -0.002(3) -0.011(3) -0.006(3) O33 0.015(3) 0.031(4) 0.037(4) -0.012(3) -0.002(3) -0.008(3) O34 0.017(3) 0.033(4) 0.030(4) -0.003(3) 0.000(3) -0.009(3) O35 0.024(4) 0.044(5) 0.035(4) -0.012(4) -0.004(3) -0.007(4) O36 0.022(4) 0.033(4) 0.028(4) -0.014(3) -0.009(3) -0.003(3) O37 0.014(3) 0.023(4) 0.054(5) 0.000(3) -0.013(3) -0.010(3) N1 0.023(5) 0.035(5) 0.035(5) -0.001(4) -0.005(4) -0.010(4) N2 0.021(4) 0.033(5) 0.033(5) -0.004(4) -0.002(4) -0.007(4) N3 0.017(4) 0.036(5) 0.021(4) -0.003(4) -0.002(3) -0.008(4) N4 0.030(5) 0.033(5) 0.024(4) 0.003(4) -0.015(4) -0.012(4) N5 0.035(5) 0.030(5) 0.046(6) 0.015(4) -0.026(5) -0.015(4) N6 0.030(5) 0.030(5) 0.063(7) 0.009(5) -0.033(5) -0.006(4) N7 0.023(5) 0.032(5) 0.051(6) -0.013(5) -0.014(4) -0.006(4) N8 0.025(5) 0.032(5) 0.036(5) -0.008(4) -0.010(4) -0.008(4) N9 0.021(4) 0.023(4) 0.036(5) -0.008(4) -0.005(4) -0.004(3) N10 0.019(4) 0.039(6) 0.051(6) -0.023(5) -0.005(4) -0.004(4) N11 0.025(5) 0.056(7) 0.080(9) -0.046(7) -0.009(6) -0.003(5) N12 0.026(5) 0.040(6) 0.075(8) -0.021(6) -0.018(5) -0.008(4) N13 0.029(3) 0.027(3) 0.031(4) -0.005(3) -0.012(3) -0.006(3) N14 0.029(5) 0.031(5) 0.029(5) -0.003(4) -0.011(4) -0.002(4) N15 0.022(4) 0.023(4) 0.032(5) 0.004(4) -0.010(4) 0.001(3) N16 0.024(5) 0.035(5) 0.031(5) 0.007(4) -0.008(4) -0.014(4) N17 0.022(5) 0.037(6) 0.043(6) 0.004(5) -0.005(4) -0.007(4) N18 0.014(4) 0.032(5) 0.034(5) -0.006(4) -0.002(4) -0.005(4) C1 0.095(19) 0.20(4) 0.12(2) -0.03(2) -0.052(17) -0.06(2) C2 0.041(7) 0.039(7) 0.045(7) 0.000(6) -0.016(6) -0.022(6) C3 0.061(9) 0.041(7) 0.047(8) 0.002(6) -0.021(7) -0.017(7) C4 0.083(12) 0.052(9) 0.047(8) -0.023(7) -0.021(8) -0.019(8) C5 0.060(9) 0.027(6) 0.041(7) 0.006(5) -0.023(6) -0.005(6) C6 0.039(6) 0.021(5) 0.038(6) -0.001(5) -0.013(5) -0.005(5) C7 0.037(6) 0.036(6) 0.044(7) -0.010(5) -0.021(6) -0.007(5) C8 0.042(7) 0.023(5) 0.035(6) -0.005(5) -0.006(5) 0.000(5) C9 0.023(5) 0.029(6) 0.039(6) -0.001(5) -0.007(5) -0.012(4) C10 0.013(5) 0.038(6) 0.028(6) -0.002(5) 0.000(4) -0.004(4) C11 0.027(6) 0.056(8) 0.040(7) -0.015(6) 0.007(5) -0.006(6) C12 0.031(7) 0.061(10) 0.087(13) 0.001(9) -0.005(8) 0.005(7) C13 0.021(5) 0.039(6) 0.042(7) -0.010(5) -0.009(5) -0.012(5) C14 0.020(5) 0.023(5) 0.050(7) 0.016(5) -0.004(5) -0.006(4) C15 0.030(6) 0.037(7) 0.061(9) -0.007(6) 0.007(6) -0.023(5) C16 0.029(6) 0.045(7) 0.041(7) 0.001(5) -0.011(5) -0.023(5) C17 0.035(6) 0.038(6) 0.028(6) -0.009(5) -0.003(5) -0.018(5) C18 0.021(5) 0.032(6) 0.031(6) -0.005(5) -0.002(4) -0.016(4) C19 0.023(5) 0.039(6) 0.027(5) 0.004(5) -0.010(4) -0.013(5) C20 0.027(6) 0.023(5) 0.052(7) -0.001(5) -0.023(5) -0.006(4) C21 0.042(7) 0.025(6) 0.060(8) 0.017(6) -0.036(6) -0.012(5) C22 0.060(10) 0.071(11) 0.103(14) 0.064(11) -0.050(10) -0.049(9) C23 0.14(2) 0.103(17) 0.23(3) -0.025(19) -0.06(2) -0.013(17) C24 0.054(8) 0.042(7) 0.095(11) 0.000(8) -0.038(8) -0.012(6) C25 0.108(13) 0.055(10) 0.129(14) 0.014(10) -0.066(11) -0.029(9) C26 0.130(14) 0.068(11) 0.127(14) 0.027(11) -0.080(12) -0.038(11) C27 0.119(12) 0.068(10) 0.095(11) 0.026(9) -0.082(10) -0.038(10) C28 0.062(8) 0.055(8) 0.058(8) 0.020(7) -0.043(7) -0.029(7) C29 0.028(6) 0.038(7) 0.066(8) 0.006(6) -0.018(6) -0.007(5) C30 0.064(9) 0.045(8) 0.058(9) 0.009(7) -0.048(8) -0.019(7) C31 0.014(4) 0.028(5) 0.036(6) -0.013(5) -0.005(4) -0.005(4) C32 0.015(4) 0.041(6) 0.024(5) -0.011(5) -0.005(4) -0.007(4) C33 0.047(8) 0.049(8) 0.062(9) -0.032(7) -0.027(7) -0.004(6) C34 0.040(8) 0.052(9) 0.088(12) 0.005(8) -0.020(8) -0.028(7) C35 0.017(5) 0.039(6) 0.048(7) -0.009(5) -0.009(5) -0.001(4) C36 0.050(3) 0.051(3) 0.051(3) -0.0052(11) -0.0167(15) -0.0102(12) C37 0.029(2) 0.029(3) 0.033(3) -0.0008(10) -0.0083(12) -0.0065(11) C38 0.026(6) 0.048(7) 0.055(8) -0.013(6) -0.009(6) 0.006(5) C39 0.021(5) 0.051(7) 0.034(6) -0.011(5) -0.012(4) -0.003(5) C40 0.014(4) 0.037(6) 0.033(6) -0.006(5) -0.003(4) -0.001(4) C41 0.016(5) 0.060(8) 0.041(7) -0.035(6) -0.007(5) 0.001(5) C42 0.028(6) 0.037(7) 0.070(9) -0.032(7) -0.021(6) 0.003(5) C43 0.034(7) 0.054(9) 0.118(15) -0.062(10) -0.022(9) 0.005(6) C44 0.036(9) 0.18(3) 0.25(3) -0.18(3) -0.029(14) 0.001(12) C45 0.12(2) 0.067(13) 0.094(17) -0.009(12) -0.044(15) -0.005(13) C46 0.046(8) 0.046(8) 0.088(12) -0.028(8) -0.039(8) 0.005(6) C47 0.104(16) 0.047(10) 0.088(14) -0.026(9) -0.047(12) 0.003(10) C48 0.13(2) 0.062(12) 0.079(14) -0.022(10) -0.066(14) 0.001(12) C49 0.087(12) 0.041(8) 0.080(12) -0.020(8) -0.055(10) 0.000(8) C50 0.039(4) 0.035(4) 0.039(4) -0.008(4) -0.018(4) -0.004(4) C51 0.043(7) 0.035(7) 0.047(7) -0.017(6) -0.021(6) -0.007(5) C52 0.033(2) 0.032(2) 0.030(2) -0.0043(10) -0.0135(11) -0.0026(10) C53 0.019(5) 0.036(6) 0.019(5) 0.004(4) -0.006(4) -0.007(4) C54 0.021(5) 0.023(5) 0.046(7) 0.008(5) -0.011(5) -0.006(4) C55 0.051(8) 0.043(7) 0.065(9) 0.025(7) -0.043(7) -0.026(6) C56 0.092(16) 0.138(19) 0.131(18) 0.020(17) -0.010(15) -0.001(15) C57 0.046(7) 0.027(6) 0.050(8) 0.001(5) -0.020(6) -0.002(5) C58 0.055(8) 0.027(6) 0.058(9) -0.006(6) -0.028(7) 0.011(6) C59 0.070(10) 0.029(6) 0.040(7) 0.006(5) -0.023(7) -0.006(6) C60 0.062(9) 0.023(6) 0.045(8) 0.003(5) -0.019(7) -0.010(6) C61 0.041(7) 0.022(5) 0.043(7) -0.009(5) -0.016(6) -0.004(5) C62 0.037(6) 0.034(6) 0.042(7) -0.005(5) -0.014(5) -0.010(5) C63 0.032(6) 0.021(5) 0.034(6) -0.002(4) 0.000(5) -0.008(4) C64 0.026(5) 0.036(6) 0.024(5) -0.001(4) -0.009(4) -0.017(5) C65 0.018(5) 0.042(7) 0.032(6) -0.009(5) 0.004(4) -0.012(5) C66 0.021(6) 0.095(12) 0.028(6) 0.001(7) 0.005(5) -0.028(7) C67 0.018(5) 0.051(7) 0.029(6) -0.002(5) 0.000(4) -0.016(5) C68 0.023(5) 0.048(7) 0.029(6) 0.008(5) -0.006(5) -0.009(5) C69 0.020(5) 0.027(5) 0.027(5) 0.001(4) -0.009(4) -0.002(4) C70 0.031(6) 0.052(8) 0.028(6) -0.017(5) 0.000(5) -0.013(5) C71 0.012(4) 0.039(6) 0.028(5) -0.012(5) -0.006(4) -0.007(4) C72 0.032(6) 0.059(8) 0.033(7) -0.023(6) 0.002(5) -0.014(6) C73 0.019(5) 0.038(6) 0.027(5) -0.002(5) -0.014(4) -0.010(4) C74 0.028(6) 0.050(7) 0.032(6) -0.001(5) -0.010(5) -0.011(5) C75 0.018(5) 0.035(6) 0.024(5) -0.008(4) -0.003(4) -0.009(4) C76 0.030(6) 0.055(8) 0.029(6) -0.001(6) -0.007(5) -0.012(6) C77 0.021(5) 0.031(6) 0.033(6) -0.009(5) -0.005(4) -0.002(4) C78 0.025(6) 0.066(9) 0.037(7) -0.017(6) 0.003(5) -0.017(6) N19 0.042(11) 0.035(10) 0.089(15) -0.004(10) -0.007(11) -0.029(9) C79 0.049(13) 0.043(13) 0.080(17) -0.014(12) -0.036(12) -0.011(11) C80 0.044(15) 0.08(2) 0.045(16) -0.011(15) -0.022(13) 0.011(15) C81 0.11(2) 0.045(15) 0.11(2) -0.031(15) -0.038(17) -0.019(15) C82 0.11(3) 0.17(4) 0.08(3) -0.04(3) -0.02(3) -0.03(3) C83 0.073(18) 0.044(15) 0.12(2) 0.029(16) 0.000(18) -0.026(14) C84 0.10(3) 0.11(3) 0.14(4) 0.02(3) 0.00(3) -0.06(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O22 2.255(9) . ? Gd1 O2 2.259(9) . ? Gd1 O23 2.395(7) . ? Gd1 O3 2.397(7) . ? Gd1 O25 2.432(7) . ? Gd1 O27 2.451(7) . ? Gd1 N1 2.539(10) . ? Gd1 N16 2.547(9) . ? Gd1 Gd4 3.9182(8) . ? Gd1 Gd2 3.9290(7) . ? Gd2 O3 2.379(7) . ? Gd2 O19 2.380(7) . ? Gd2 O37 2.421(7) . ? Gd2 O31 2.445(7) . ? Gd2 O25 2.452(7) . ? Gd2 O29 2.478(8) . ? Gd2 O28 2.481(8) . ? Gd2 N15 2.601(9) . ? Gd2 N3 2.619(8) . ? Gd2 Gd3 3.9300(7) . ? Gd3 O6 2.248(7) . ? Gd3 O18 2.282(8) . ? Gd3 O19 2.393(7) . ? Gd3 O7 2.405(7) . ? Gd3 O31 2.437(7) . ? Gd3 O30 2.452(7) . ? Gd3 N4 2.534(9) . ? Gd3 N13 2.539(9) . ? Gd3 Gd5 3.9368(7) . ? Gd4 O23 2.388(8) . ? Gd4 O11 2.390(7) . ? Gd4 O37 2.398(7) . ? Gd4 O36 2.435(7) . ? Gd4 O27 2.442(7) . ? Gd4 O34 2.483(8) . ? Gd4 O26 2.485(9) . ? Gd4 N18 2.605(9) . ? Gd4 N9 2.607(9) . ? Gd4 Gd6 3.9177(8) . ? Gd5 O15 2.380(8) . ? Gd5 O7 2.393(7) . ? Gd5 O37 2.417(8) . ? Gd5 O30 2.457(7) . ? Gd5 O33 2.463(8) . ? Gd5 O32 2.509(8) . ? Gd5 O35 2.518(9) . ? Gd5 N6 2.588(10) . ? Gd5 N12 2.610(11) . ? Gd5 Gd6 3.9380(7) . ? Gd6 O14 2.257(8) . ? Gd6 O10 2.260(10) . ? Gd6 O11 2.381(7) . ? Gd6 O15 2.396(9) . ? Gd6 O33 2.454(7) . ? Gd6 O36 2.455(8) . ? Gd6 N10 2.495(10) . ? Gd6 N7 2.538(10) . ? O1 C2 1.369(17) . ? O1 C1 1.403(16) . ? O2 C7 1.313(15) . ? O3 C9 1.305(14) . ? O4 N3 1.385(12) . ? O4 H4 0.8400 . ? O5 C13 1.377(16) . ? O5 C12 1.429(13) . ? O6 C18 1.287(13) . ? O7 C20 1.299(15) . ? O8 N6 1.382(12) . ? O8 H8 0.8400 . ? O9 C23 1.392(18) . ? O9 C24 1.45(2) . ? O10 C29 1.269(18) . ? O11 C31 1.317(13) . ? O12 N9 1.386(12) . ? O12 H12 0.8400 . ? O13 C35 1.359(13) . ? O13 C34 1.425(12) . ? O14 C40 1.316(12) . ? O15 C42 1.323(15) . ? O16 N12 1.408(13) . ? O16 H16 0.8400 . ? O17 C46 1.312(17) . ? O17 C45 1.428(15) . ? O18 C51 1.304(14) . ? O19 C53 1.323(13) . ? O20 N15 1.397(12) . ? O20 H20 0.8400 . ? O21 C57 1.399(18) . ? O21 C56 1.428(18) . ? O22 C62 1.306(16) . ? O23 C64 1.288(13) . ? O24 N18 1.401(11) . ? O24 H24 0.8400 . ? O25 C67 1.315(13) . ? O26 C67 1.261(15) . ? O27 C69 1.286(13) . ? O28 C69 1.270(14) . ? O29 C71 1.259(14) . ? O30 C71 1.317(14) . ? O31 C73 1.308(13) . ? O32 C73 1.250(13) . ? O33 C75 1.294(13) . ? O34 C75 1.244(14) . ? O35 C77 1.255(14) . ? O36 C77 1.266(14) . ? N1 C8 1.291(16) . ? N1 N2 1.416(13) . ? N2 C9 1.292(15) . ? N3 C10 1.277(15) . ? N4 C19 1.296(14) . ? N4 N5 1.412(13) . ? N5 C20 1.291(16) . ? N6 C21 1.308(16) . ? N7 C30 1.326(17) . ? N7 N8 1.403(13) . ? N8 C31 1.301(16) . ? N9 C32 1.270(15) . ? N10 C41 1.304(15) . ? N10 N11 1.434(14) . ? N11 C42 1.295(17) . ? N12 C43 1.253(18) . ? N13 C52 1.303(12) . ? N13 N14 1.428(13) . ? N14 C53 1.272(15) . ? N15 C54 1.294(16) . ? N16 C63 1.299(15) . ? N16 N17 1.407(13) . ? N17 C64 1.333(16) . ? N18 C65 1.248(16) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.38(2) . ? C2 C7 1.424(16) . ? C3 C4 1.42(2) . ? C3 H3 0.9500 . ? C4 C5 1.37(2) . ? C4 H4A 0.9500 . ? C5 C6 1.400(18) . ? C5 H5 0.9500 . ? C6 C7 1.408(18) . ? C6 C8 1.463(18) . ? C8 H8A 0.9500 . ? C9 C10 1.491(15) . ? C10 C11 1.486(15) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.386(15) . ? C13 C18 1.452(16) . ? C14 C15 1.365(18) . ? C14 H14 0.9500 . ? C15 C16 1.387(19) . ? C15 H15 0.9500 . ? C16 C17 1.433(16) . ? C16 H16A 0.9500 . ? C17 C18 1.413(17) . ? C17 C19 1.415(17) . ? C19 H19A 0.9500 . ? C20 C21 1.492(15) . ? C21 C22 1.516(18) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.40(3) . ? C24 C29 1.42(2) . ? C25 C26 1.41(3) . ? C25 H25 0.9500 . ? C26 C27 1.37(3) . ? C26 H26 0.9500 . ? C27 C28 1.47(2) . ? C27 H27 0.9500 . ? C28 C29 1.42(2) . ? C28 C30 1.44(2) . ? C30 H30 0.9500 . ? C31 C32 1.516(15) . ? C32 C33 1.500(15) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.399(2) . ? C35 C40 1.400(2) . ? C36 C37 1.398(2) . ? C36 H36 0.9500 . ? C37 C38 1.401(2) . ? C37 H37 0.9500 . ? C38 C39 1.400(2) . ? C38 H38 0.9500 . ? C39 C40 1.400(2) . ? C39 C41 1.463(15) . ? C41 H41 0.9500 . ? C42 C43 1.513(18) . ? C43 C44 1.51(2) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.393(15) . ? C46 C51 1.440(13) . ? C47 C48 1.416(16) . ? C47 H47 0.9500 . ? C48 C49 1.377(15) . ? C48 H48 0.9500 . ? C49 C50 1.410(13) . ? C49 H49 0.9500 . ? C50 C51 1.447(13) . ? C50 C52 1.538(13) . ? C52 H52 0.9500 . ? C53 C54 1.507(15) . ? C54 C55 1.489(17) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.381(19) . ? C57 C62 1.425(18) . ? C58 C59 1.39(2) . ? C58 H58 0.9500 . ? C59 C60 1.36(2) . ? C59 H59 0.9500 . ? C60 C61 1.436(18) . ? C60 H60 0.9500 . ? C61 C62 1.405(18) . ? C61 C63 1.440(17) . ? C63 H63 0.9500 . ? C64 C65 1.486(16) . ? C65 C66 1.512(15) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.485(17) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.488(16) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.507(15) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.475(16) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.521(16) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.511(16) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? N19 C81 1.487(19) . ? N19 C83 1.502(19) . ? N19 C79 1.506(18) . ? N19 H19 0.9300 . ? C79 C80 1.478(19) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.48(2) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 C84 1.50(2) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 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 O22 Gd1 O2 114.6(4) . . ? O22 Gd1 O23 131.6(3) . . ? O2 Gd1 O23 78.2(3) . . ? O22 Gd1 O3 77.9(3) . . ? O2 Gd1 O3 131.8(3) . . ? O23 Gd1 O3 129.7(2) . . ? O22 Gd1 O25 88.1(3) . . ? O2 Gd1 O25 152.5(3) . . ? O23 Gd1 O25 75.0(3) . . ? O3 Gd1 O25 65.5(2) . . ? O22 Gd1 O27 152.3(3) . . ? O2 Gd1 O27 87.9(3) . . ? O23 Gd1 O27 66.2(2) . . ? O3 Gd1 O27 74.9(3) . . ? O25 Gd1 O27 75.9(3) . . ? O22 Gd1 N1 84.3(3) . . ? O2 Gd1 N1 71.7(3) . . ? O23 Gd1 N1 141.0(3) . . ? O3 Gd1 N1 63.3(3) . . ? O25 Gd1 N1 128.7(3) . . ? O27 Gd1 N1 88.2(3) . . ? O22 Gd1 N16 71.3(3) . . ? O2 Gd1 N16 85.3(3) . . ? O23 Gd1 N16 63.3(3) . . ? O3 Gd1 N16 139.8(3) . . ? O25 Gd1 N16 88.0(3) . . ? O27 Gd1 N16 129.4(3) . . ? N1 Gd1 N16 135.6(3) . . ? O22 Gd1 Gd4 144.1(3) . . ? O2 Gd1 Gd4 96.1(3) . . ? O23 Gd1 Gd4 34.95(17) . . ? O3 Gd1 Gd4 95.82(18) . . ? O25 Gd1 Gd4 57.93(19) . . ? O27 Gd1 Gd4 36.73(17) . . ? N1 Gd1 Gd4 124.7(2) . . ? N16 Gd1 Gd4 94.4(2) . . ? O22 Gd1 Gd2 96.1(3) . . ? O2 Gd1 Gd2 143.8(2) . . ? O23 Gd1 Gd2 96.08(18) . . ? O3 Gd1 Gd2 34.50(17) . . ? O25 Gd1 Gd2 36.60(17) . . ? O27 Gd1 Gd2 57.85(17) . . ? N1 Gd1 Gd2 93.9(2) . . ? N16 Gd1 Gd2 124.4(2) . . ? Gd4 Gd1 Gd2 64.483(14) . . ? O3 Gd2 O19 123.9(3) . . ? O3 Gd2 O37 117.8(3) . . ? O19 Gd2 O37 118.4(3) . . ? O3 Gd2 O31 129.7(3) . . ? O19 Gd2 O31 66.3(2) . . ? O37 Gd2 O31 76.6(2) . . ? O3 Gd2 O25 65.4(2) . . ? O19 Gd2 O25 128.5(3) . . ? O37 Gd2 O25 76.2(3) . . ? O31 Gd2 O25 152.8(3) . . ? O3 Gd2 O29 129.0(3) . . ? O19 Gd2 O29 68.2(2) . . ? O37 Gd2 O29 73.3(3) . . ? O31 Gd2 O29 101.1(3) . . ? O25 Gd2 O29 70.7(3) . . ? O3 Gd2 O28 69.7(3) . . ? O19 Gd2 O28 130.1(2) . . ? O37 Gd2 O28 72.4(3) . . ? O31 Gd2 O28 70.4(3) . . ? O25 Gd2 O28 101.3(3) . . ? O29 Gd2 O28 145.7(3) . . ? O3 Gd2 N15 71.9(3) . . ? O19 Gd2 N15 62.7(3) . . ? O37 Gd2 N15 143.6(3) . . ? O31 Gd2 N15 126.5(3) . . ? O25 Gd2 N15 77.5(3) . . ? O29 Gd2 N15 74.5(3) . . ? O28 Gd2 N15 137.9(3) . . ? O3 Gd2 N3 63.4(3) . . ? O19 Gd2 N3 71.9(3) . . ? O37 Gd2 N3 144.8(3) . . ? O31 Gd2 N3 78.3(3) . . ? O25 Gd2 N3 126.0(3) . . ? O29 Gd2 N3 136.2(3) . . ? O28 Gd2 N3 76.1(3) . . ? N15 Gd2 N3 71.7(3) . . ? O3 Gd2 Gd1 34.79(17) . . ? O19 Gd2 Gd1 149.00(18) . . ? O37 Gd2 Gd1 87.15(17) . . ? O31 Gd2 Gd1 141.84(18) . . ? O25 Gd2 Gd1 36.26(17) . . ? O29 Gd2 Gd1 106.93(18) . . ? O28 Gd2 Gd1 71.86(18) . . ? N15 Gd2 Gd1 86.3(2) . . ? N3 Gd2 Gd1 97.9(2) . . ? O3 Gd2 Gd3 148.80(17) . . ? O19 Gd2 Gd3 34.67(18) . . ? O37 Gd2 Gd3 88.66(17) . . ? O31 Gd2 Gd3 36.33(18) . . ? O25 Gd2 Gd3 142.31(17) . . ? O29 Gd2 Gd3 71.95(18) . . ? O28 Gd2 Gd3 106.68(18) . . ? N15 Gd2 Gd3 97.2(2) . . ? N3 Gd2 Gd3 85.5(2) . . ? Gd1 Gd2 Gd3 175.808(17) . . ? O6 Gd3 O18 113.4(3) . . ? O6 Gd3 O19 76.9(3) . . ? O18 Gd3 O19 134.0(3) . . ? O6 Gd3 O7 132.1(3) . . ? O18 Gd3 O7 79.6(3) . . ? O19 Gd3 O7 128.2(2) . . ? O6 Gd3 O31 86.1(3) . . ? O18 Gd3 O31 153.2(3) . . ? O19 Gd3 O31 66.2(2) . . ? O7 Gd3 O31 73.6(2) . . ? O6 Gd3 O30 150.8(3) . . ? O18 Gd3 O30 91.1(3) . . ? O19 Gd3 O30 74.6(3) . . ? O7 Gd3 O30 65.5(3) . . ? O31 Gd3 O30 77.1(2) . . ? O6 Gd3 N4 72.2(3) . . ? O18 Gd3 N4 83.7(3) . . ? O19 Gd3 N4 139.1(3) . . ? O7 Gd3 N4 63.4(3) . . ? O31 Gd3 N4 85.2(3) . . ? O30 Gd3 N4 128.7(3) . . ? O6 Gd3 N13 89.6(3) . . ? O18 Gd3 N13 71.3(3) . . ? O19 Gd3 N13 63.8(3) . . ? O7 Gd3 N13 136.6(3) . . ? O31 Gd3 N13 129.6(3) . . ? O30 Gd3 N13 83.3(3) . . ? N4 Gd3 N13 140.2(3) . . ? O6 Gd3 Gd2 93.0(2) . . ? O18 Gd3 Gd2 149.0(3) . . ? O19 Gd3 Gd2 34.45(18) . . ? O7 Gd3 Gd2 95.03(17) . . ? O31 Gd3 Gd2 36.46(17) . . ? O30 Gd3 Gd2 59.52(18) . . ? N4 Gd3 Gd2 121.4(2) . . ? N13 Gd3 Gd2 93.9(2) . . ? O6 Gd3 Gd5 142.2(2) . . ? O18 Gd3 Gd5 99.2(3) . . ? O19 Gd3 Gd5 94.42(17) . . ? O7 Gd3 Gd5 34.75(17) . . ? O31 Gd3 Gd5 57.25(17) . . ? O30 Gd3 Gd5 36.73(18) . . ? N4 Gd3 Gd5 93.8(2) . . ? N13 Gd3 Gd5 119.9(2) . . ? Gd2 Gd3 Gd5 63.941(14) . . ? O23 Gd4 O11 123.7(2) . . ? O23 Gd4 O37 118.6(3) . . ? O11 Gd4 O37 117.6(3) . . ? O23 Gd4 O36 128.9(3) . . ? O11 Gd4 O36 66.9(2) . . ? O37 Gd4 O36 76.1(3) . . ? O23 Gd4 O27 66.4(2) . . ? O11 Gd4 O27 128.3(2) . . ? O37 Gd4 O27 75.9(3) . . ? O36 Gd4 O27 152.0(2) . . ? O23 Gd4 O34 129.8(3) . . ? O11 Gd4 O34 68.3(2) . . ? O37 Gd4 O34 72.1(3) . . ? O36 Gd4 O34 101.1(3) . . ? O27 Gd4 O34 70.4(3) . . ? O23 Gd4 O26 69.5(3) . . ? O11 Gd4 O26 129.4(2) . . ? O37 Gd4 O26 73.6(3) . . ? O36 Gd4 O26 69.4(3) . . ? O27 Gd4 O26 102.1(3) . . ? O34 Gd4 O26 145.8(3) . . ? O23 Gd4 N18 62.3(3) . . ? O11 Gd4 N18 72.6(3) . . ? O37 Gd4 N18 145.3(3) . . ? O36 Gd4 N18 78.9(3) . . ? O27 Gd4 N18 126.0(3) . . ? O34 Gd4 N18 137.0(3) . . ? O26 Gd4 N18 75.2(3) . . ? O23 Gd4 N9 72.4(3) . . ? O11 Gd4 N9 62.7(3) . . ? O37 Gd4 N9 142.5(3) . . ? O36 Gd4 N9 127.2(3) . . ? O27 Gd4 N9 77.4(3) . . ? O34 Gd4 N9 74.4(3) . . ? O26 Gd4 N9 138.2(3) . . ? N18 Gd4 N9 72.2(3) . . ? O23 Gd4 Gd6 148.60(17) . . ? O11 Gd4 Gd6 34.73(16) . . ? O37 Gd4 Gd6 87.97(18) . . ? O36 Gd4 Gd6 36.94(18) . . ? O27 Gd4 Gd6 141.65(17) . . ? O34 Gd4 Gd6 71.62(18) . . ? O26 Gd4 Gd6 106.29(19) . . ? N18 Gd4 Gd6 86.4(2) . . ? N9 Gd4 Gd6 97.2(2) . . ? O23 Gd4 Gd1 35.05(17) . . ? O11 Gd4 Gd1 149.09(16) . . ? O37 Gd4 Gd1 87.72(18) . . ? O36 Gd4 Gd1 141.11(18) . . ? O27 Gd4 Gd1 36.89(18) . . ? O34 Gd4 Gd1 107.25(18) . . ? O26 Gd4 Gd1 72.18(19) . . ? N18 Gd4 Gd1 97.0(2) . . ? N9 Gd4 Gd1 86.4(2) . . ? Gd6 Gd4 Gd1 175.678(17) . . ? O15 Gd5 O7 124.1(3) . . ? O15 Gd5 O37 117.3(3) . . ? O7 Gd5 O37 118.6(2) . . ? O15 Gd5 O30 127.1(3) . . ? O7 Gd5 O30 65.6(2) . . ? O37 Gd5 O30 79.2(3) . . ? O15 Gd5 O33 65.6(3) . . ? O7 Gd5 O33 127.5(3) . . ? O37 Gd5 O33 77.1(3) . . ? O30 Gd5 O33 156.3(3) . . ? O15 Gd5 O32 129.8(3) . . ? O7 Gd5 O32 68.5(3) . . ? O37 Gd5 O32 73.0(3) . . ? O30 Gd5 O32 102.9(2) . . ? O33 Gd5 O32 70.3(2) . . ? O15 Gd5 O35 68.3(3) . . ? O7 Gd5 O35 129.7(3) . . ? O37 Gd5 O35 73.3(3) . . ? O30 Gd5 O35 70.1(2) . . ? O33 Gd5 O35 102.5(3) . . ? O32 Gd5 O35 146.3(3) . . ? O15 Gd5 N6 73.3(3) . . ? O7 Gd5 N6 63.0(3) . . ? O37 Gd5 N6 141.9(3) . . ? O30 Gd5 N6 125.7(3) . . ? O33 Gd5 N6 75.2(3) . . ? O32 Gd5 N6 73.4(3) . . ? O35 Gd5 N6 138.2(3) . . ? O15 Gd5 N12 62.4(3) . . ? O7 Gd5 N12 72.5(3) . . ? O37 Gd5 N12 145.1(4) . . ? O30 Gd5 N12 76.4(3) . . ? O33 Gd5 N12 124.6(3) . . ? O32 Gd5 N12 136.8(3) . . ? O35 Gd5 N12 75.1(4) . . ? N6 Gd5 N12 73.0(4) . . ? O15 Gd5 Gd3 148.9(2) . . ? O7 Gd5 Gd3 34.95(17) . . ? O37 Gd5 Gd3 88.55(16) . . ? O30 Gd5 Gd3 36.65(16) . . ? O33 Gd5 Gd3 141.99(17) . . ? O32 Gd5 Gd3 71.93(17) . . ? O35 Gd5 Gd3 106.74(19) . . ? N6 Gd5 Gd3 97.5(2) . . ? N12 Gd5 Gd3 86.5(2) . . ? O15 Gd5 Gd6 34.6(2) . . ? O7 Gd5 Gd6 148.78(17) . . ? O37 Gd5 Gd6 87.23(16) . . ? O30 Gd5 Gd6 141.79(16) . . ? O33 Gd5 Gd6 36.71(17) . . ? O32 Gd5 Gd6 106.96(17) . . ? O35 Gd5 Gd6 71.81(19) . . ? N6 Gd5 Gd6 85.9(2) . . ? N12 Gd5 Gd6 96.8(2) . . ? Gd3 Gd5 Gd6 175.774(18) . . ? O14 Gd6 O10 115.8(4) . . ? O14 Gd6 O11 76.8(3) . . ? O10 Gd6 O11 134.0(3) . . ? O14 Gd6 O15 132.1(3) . . ? O10 Gd6 O15 77.6(3) . . ? O11 Gd6 O15 128.6(3) . . ? O14 Gd6 O33 150.8(3) . . ? O10 Gd6 O33 88.9(4) . . ? O11 Gd6 O33 74.7(2) . . ? O15 Gd6 O33 65.5(3) . . ? O14 Gd6 O36 86.4(3) . . ? O10 Gd6 O36 150.8(3) . . ? O11 Gd6 O36 66.7(2) . . ? O15 Gd6 O36 73.4(3) . . ? O33 Gd6 O36 76.8(3) . . ? O14 Gd6 N10 72.5(3) . . ? O10 Gd6 N10 82.5(4) . . ? O11 Gd6 N10 140.6(3) . . ? O15 Gd6 N10 63.6(3) . . ? O33 Gd6 N10 129.1(3) . . ? O36 Gd6 N10 87.0(3) . . ? O14 Gd6 N7 89.3(3) . . ? O10 Gd6 N7 72.0(3) . . ? O11 Gd6 N7 63.8(3) . . ? O15 Gd6 N7 136.8(3) . . ? O33 Gd6 N7 83.8(3) . . ? O36 Gd6 N7 130.0(3) . . ? N10 Gd6 N7 138.3(3) . . ? O14 Gd6 Gd4 93.3(3) . . ? O10 Gd6 Gd4 146.9(3) . . ? O11 Gd6 Gd4 34.89(16) . . ? O15 Gd6 Gd4 95.0(2) . . ? O33 Gd6 Gd4 59.21(19) . . ? O36 Gd6 Gd4 36.58(16) . . ? N10 Gd6 Gd4 123.3(3) . . ? N7 Gd6 Gd4 94.2(2) . . ? O14 Gd6 Gd5 142.5(3) . . ? O10 Gd6 Gd5 96.3(3) . . ? O11 Gd6 Gd5 95.26(16) . . ? O15 Gd6 Gd5 34.33(19) . . ? O33 Gd6 Gd5 36.85(18) . . ? O36 Gd6 Gd5 57.36(18) . . ? N10 Gd6 Gd5 94.2(2) . . ? N7 Gd6 Gd5 120.4(2) . . ? Gd4 Gd6 Gd5 64.300(14) . . ? C2 O1 C1 121.8(17) . . ? C7 O2 Gd1 141.7(8) . . ? C9 O3 Gd2 122.0(7) . . ? C9 O3 Gd1 121.4(7) . . ? Gd2 O3 Gd1 110.7(3) . . ? N3 O4 H4 109.5 . . ? C13 O5 C12 117.0(11) . . ? C18 O6 Gd3 139.8(8) . . ? C20 O7 Gd5 122.1(6) . . ? C20 O7 Gd3 119.5(6) . . ? Gd5 O7 Gd3 110.3(3) . . ? N6 O8 H8 109.5 . . ? C23 O9 C24 117(2) . . ? C29 O10 Gd6 144.5(9) . . ? C31 O11 Gd6 120.4(7) . . ? C31 O11 Gd4 121.6(6) . . ? Gd6 O11 Gd4 110.4(3) . . ? N9 O12 H12 109.5 . . ? C35 O13 C34 118.4(11) . . ? C40 O14 Gd6 140.5(7) . . ? C42 O15 Gd5 122.5(7) . . ? C42 O15 Gd6 120.1(7) . . ? Gd5 O15 Gd6 111.1(3) . . ? N12 O16 H16 109.5 . . ? C46 O17 C45 116.2(14) . . ? C51 O18 Gd3 143.1(8) . . ? C53 O19 Gd2 122.4(6) . . ? C53 O19 Gd3 120.0(7) . . ? Gd2 O19 Gd3 110.9(3) . . ? N15 O20 H20 109.5 . . ? C57 O21 C56 113.3(17) . . ? C62 O22 Gd1 143.1(8) . . ? C64 O23 Gd4 122.2(7) . . ? C64 O23 Gd1 121.9(7) . . ? Gd4 O23 Gd1 110.0(3) . . ? N18 O24 H24 109.5 . . ? C67 O25 Gd1 124.7(7) . . ? C67 O25 Gd2 124.3(7) . . ? Gd1 O25 Gd2 107.1(3) . . ? C67 O26 Gd4 119.5(7) . . ? C69 O27 Gd4 124.3(7) . . ? C69 O27 Gd1 125.5(6) . . ? Gd4 O27 Gd1 106.4(3) . . ? C69 O28 Gd2 120.0(7) . . ? C71 O29 Gd2 120.7(7) . . ? C71 O30 Gd3 123.1(6) . . ? C71 O30 Gd5 123.2(6) . . ? Gd3 O30 Gd5 106.6(3) . . ? C73 O31 Gd3 125.3(7) . . ? C73 O31 Gd2 124.2(6) . . ? Gd3 O31 Gd2 107.2(3) . . ? C73 O32 Gd5 119.0(7) . . ? C75 O33 Gd6 123.0(6) . . ? C75 O33 Gd5 124.4(7) . . ? Gd6 O33 Gd5 106.4(3) . . ? C75 O34 Gd4 120.7(7) . . ? C77 O35 Gd5 117.3(8) . . ? C77 O36 Gd4 126.0(7) . . ? C77 O36 Gd6 124.1(7) . . ? Gd4 O36 Gd6 106.5(3) . . ? Gd4 O37 Gd5 120.5(3) . . ? Gd4 O37 Gd2 120.6(3) . . ? Gd5 O37 Gd2 118.8(3) . . ? C8 N1 N2 111.8(10) . . ? C8 N1 Gd1 130.6(8) . . ? N2 N1 Gd1 117.5(7) . . ? C9 N2 N1 112.7(9) . . ? C10 N3 O4 113.3(9) . . ? C10 N3 Gd2 118.5(7) . . ? O4 N3 Gd2 128.2(7) . . ? C19 N4 N5 113.3(9) . . ? C19 N4 Gd3 127.9(8) . . ? N5 N4 Gd3 118.8(7) . . ? C20 N5 N4 110.4(9) . . ? C21 N6 O8 113.9(10) . . ? C21 N6 Gd5 118.9(7) . . ? O8 N6 Gd5 126.7(8) . . ? C30 N7 N8 111.4(11) . . ? C30 N7 Gd6 130.1(9) . . ? N8 N7 Gd6 118.1(8) . . ? C31 N8 N7 111.7(9) . . ? C32 N9 O12 111.6(9) . . ? C32 N9 Gd4 120.3(7) . . ? O12 N9 Gd4 127.7(7) . . ? C41 N10 N11 109.4(10) . . ? C41 N10 Gd6 130.6(8) . . ? N11 N10 Gd6 119.9(7) . . ? C42 N11 N10 109.9(10) . . ? C43 N12 O16 113.6(11) . . ? C43 N12 Gd5 120.8(9) . . ? O16 N12 Gd5 125.4(7) . . ? C52 N13 N14 102.7(9) . . ? C52 N13 Gd3 137.2(8) . . ? N14 N13 Gd3 117.2(6) . . ? C53 N14 N13 112.3(9) . . ? C54 N15 O20 111.8(9) . . ? C54 N15 Gd2 120.5(7) . . ? O20 N15 Gd2 127.6(7) . . ? C63 N16 N17 111.3(9) . . ? C63 N16 Gd1 130.3(8) . . ? N17 N16 Gd1 118.4(7) . . ? C64 N17 N16 111.4(9) . . ? C65 N18 O24 112.0(9) . . ? C65 N18 Gd4 120.4(7) . . ? O24 N18 Gd4 127.6(7) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.1(12) . . ? O1 C2 C7 116.4(12) . . ? C3 C2 C7 121.4(13) . . ? C2 C3 C4 118.9(14) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 121.2(13) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 119.5(14) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C5 C6 C7 121.4(12) . . ? C5 C6 C8 115.4(12) . . ? C7 C6 C8 123.2(11) . . ? O2 C7 C6 123.4(11) . . ? O2 C7 C2 118.9(12) . . ? C6 C7 C2 117.6(11) . . ? N1 C8 C6 126.3(11) . . ? N1 C8 H8A 116.9 . . ? C6 C8 H8A 116.9 . . ? N2 C9 O3 124.6(10) . . ? N2 C9 C10 117.7(10) . . ? O3 C9 C10 117.7(10) . . ? N3 C10 C11 124.6(11) . . ? N3 C10 C9 113.7(9) . . ? C11 C10 C9 121.7(11) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O5 C12 H12A 109.5 . . ? O5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O5 C13 C14 125.0(11) . . ? O5 C13 C18 113.0(10) . . ? C14 C13 C18 122.0(11) . . ? C15 C14 C13 120.1(11) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 121.2(11) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C17 120.1(12) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C17 C19 121.9(10) . . ? C18 C17 C16 120.3(12) . . ? C19 C17 C16 117.7(12) . . ? O6 C18 C17 124.9(11) . . ? O6 C18 C13 118.9(11) . . ? C17 C18 C13 116.2(10) . . ? N4 C19 C17 128.6(11) . . ? N4 C19 H19A 115.7 . . ? C17 C19 H19A 115.7 . . ? N5 C20 O7 127.7(10) . . ? N5 C20 C21 115.1(11) . . ? O7 C20 C21 117.0(10) . . ? N6 C21 C20 113.1(10) . . ? N6 C21 C22 124.1(11) . . ? C20 C21 C22 122.1(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 . . ? O9 C23 H23A 109.5 . . ? O9 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O9 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 122.4(17) . . ? C25 C24 O9 125.3(16) . . ? C29 C24 O9 112.3(15) . . ? C24 C25 C26 119.1(19) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C25 122(2) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C28 117.8(19) . . ? C26 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? C29 C28 C30 124.3(13) . . ? C29 C28 C27 121.3(15) . . ? C30 C28 C27 114.4(14) . . ? O10 C29 C24 120.3(15) . . ? O10 C29 C28 122.9(13) . . ? C24 C29 C28 116.8(14) . . ? N7 C30 C28 125.7(13) . . ? N7 C30 H30 117.2 . . ? C28 C30 H30 117.2 . . ? N8 C31 O11 125.7(10) . . ? N8 C31 C32 117.7(10) . . ? O11 C31 C32 116.5(10) . . ? N9 C32 C33 129.1(11) . . ? N9 C32 C31 112.4(9) . . ? C33 C32 C31 118.3(10) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O13 C34 H34A 109.5 . . ? O13 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O13 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O13 C35 C36 118.0(8) . . ? O13 C35 C40 116.7(8) . . ? C36 C35 C40 125.3(10) . . ? C37 C36 C35 115.0(10) . . ? C37 C36 H36 122.5 . . ? C35 C36 H36 122.5 . . ? C36 C37 C38 120.9(10) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C39 C38 C37 123.0(10) . . ? C39 C38 H38 118.5 . . ? C37 C38 H38 118.5 . . ? C40 C39 C38 117.1(9) . . ? C40 C39 C41 123.0(8) . . ? C38 C39 C41 119.5(8) . . ? O14 C40 C39 123.5(8) . . ? O14 C40 C35 117.4(8) . . ? C39 C40 C35 118.7(9) . . ? N10 C41 C39 125.4(10) . . ? N10 C41 H41 117.3 . . ? C39 C41 H41 117.3 . . ? N11 C42 O15 126.0(11) . . ? N11 C42 C43 118.3(11) . . ? O15 C42 C43 115.7(11) . . ? N12 C43 C44 127.1(14) . . ? N12 C43 C42 112.7(11) . . ? C44 C43 C42 119.8(13) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O17 C45 H45A 109.5 . . ? O17 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O17 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O17 C46 C47 127.2(12) . . ? O17 C46 C51 114.2(11) . . ? C47 C46 C51 118.2(12) . . ? C46 C47 C48 121.7(13) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C49 C48 C47 119.4(14) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C50 122.8(13) . . ? C48 C49 H49 118.6 . . ? C50 C49 H49 118.6 . . ? C49 C50 C51 117.2(10) . . ? C49 C50 C52 114.8(10) . . ? C51 C50 C52 126.9(9) . . ? O18 C51 C46 117.1(11) . . ? O18 C51 C50 122.2(10) . . ? C46 C51 C50 120.7(10) . . ? N13 C52 C50 115.2(10) . . ? N13 C52 H52 122.4 . . ? C50 C52 H52 122.4 . . ? N14 C53 O19 126.3(10) . . ? N14 C53 C54 117.0(10) . . ? O19 C53 C54 116.6(10) . . ? N15 C54 C55 127.3(10) . . ? N15 C54 C53 111.8(10) . . ? C55 C54 C53 120.9(11) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O21 C56 H56A 109.5 . . ? O21 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O21 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 O21 120.7(13) . . ? C58 C57 C62 121.2(13) . . ? O21 C57 C62 117.9(12) . . ? C57 C58 C59 120.8(13) . . ? C57 C58 H58 119.6 . . ? C59 C58 H58 119.6 . . ? C60 C59 C58 120.0(13) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C61 120.4(14) . . ? C59 C60 H60 119.8 . . ? C61 C60 H60 119.8 . . ? C62 C61 C60 120.2(12) . . ? C62 C61 C63 123.5(12) . . ? C60 C61 C63 116.0(12) . . ? O22 C62 C61 122.9(12) . . ? O22 C62 C57 119.9(12) . . ? C61 C62 C57 117.2(12) . . ? N16 C63 C61 126.7(11) . . ? N16 C63 H63 116.6 . . ? C61 C63 H63 116.6 . . ? O23 C64 N17 124.9(10) . . ? O23 C64 C65 117.9(10) . . ? N17 C64 C65 117.0(10) . . ? N18 C65 C64 112.8(10) . . ? N18 C65 C66 127.7(12) . . ? C64 C65 C66 119.5(12) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O26 C67 O25 121.1(11) . . ? O26 C67 C68 120.2(10) . . ? O25 C67 C68 118.7(11) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O28 C69 O27 120.9(10) . . ? O28 C69 C70 120.1(10) . . ? O27 C69 C70 118.9(10) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O29 C71 O30 123.2(10) . . ? O29 C71 C72 120.0(11) . . ? O30 C71 C72 116.8(11) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O32 C73 O31 121.0(10) . . ? O32 C73 C74 120.5(10) . . ? O31 C73 C74 118.5(9) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O34 C75 O33 122.7(10) . . ? O34 C75 C76 119.5(10) . . ? O33 C75 C76 117.8(11) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? O35 C77 O36 123.2(11) . . ? O35 C77 C78 119.3(11) . . ? O36 C77 C78 117.5(10) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C81 N19 C83 126(3) . . ? C81 N19 C79 119(2) . . ? C83 N19 C79 107(2) . . ? C81 N19 H19 99.7 . . ? C83 N19 H19 99.7 . . ? C79 N19 H19 99.7 . . ? C80 C79 N19 113(2) . . ? C80 C79 H79A 109.0 . . ? N19 C79 H79A 109.0 . . ? C80 C79 H79B 109.0 . . ? N19 C79 H79B 109.0 . . ? H79A C79 H79B 107.8 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C82 C81 N19 146(4) . . ? C82 C81 H81A 100.4 . . ? N19 C81 H81A 100.4 . . ? C82 C81 H81B 100.4 . . ? N19 C81 H81B 100.4 . . ? H81A C81 H81B 104.3 . . ? 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 . . ? C84 C83 N19 117(3) . . ? C84 C83 H83A 108.0 . . ? N19 C83 H83A 108.0 . . ? C84 C83 H83B 108.0 . . ? N19 C83 H83B 108.0 . . ? H83A C83 H83B 107.3 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O4 H4 O5 . . . 2.950(16) 0.840 2.551 110 no O16 H16 O7 . . . 3.028(15) 0.840 2.594 114 no O20 H20 O3 . . . 3.038(15) 0.840 2.431 130 no O24 H24 O13 . . . 2.935(13) 0.840 2.605 105 no O24 H24 O14 . . . 2.953(14) 0.840 2.190 151 no _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 12.756 _refine_diff_density_min -2.631 _refine_diff_density_rms 0.333 _iucr_refine_instructions_details ; TITL _MUA1950 CELL 0.71075 17.84480 18.47430 20.28070 80.002 68.785 75.752 ZERR 2 0.00130 0.00140 0.00150 0.006 0.005 0.005 LATT 1 SFAC C H GD N O UNIT 168 200 12 38 90 SHEL 8.147180 0.796452 L.S. 5 FMAP 2 PLAN -75 TEMP -110.0 ACTA BOND $H SIZE 0.430 0.120 0.420 DFIX 1.4000 0.0200 C50 C49 DFIX 1.4000 0.0200 C49 C48 DFIX 1.4000 0.0200 C48 C47 DFIX 1.4000 0.0200 C47 C46 DFIX 1.4000 0.0200 C46 C51 DFIX 1.4000 0.0200 C51 C50 FLAT 0.0100 C50 C49 C48 C47 C46 C51 DANG 2.3856 0.0400 C50 C48 DANG 2.4046 0.0400 C49 C47 DANG 2.4445 0.0400 C48 C46 DANG 2.4877 0.0400 C47 C51 DANG 2.5164 0.0400 C46 C50 DANG 2.4897 0.0400 C51 C49 ISOR 0.001 0.002 C36 C37 C52 SIMU 0.025 0.05 1.7 N19 C79 SIMU 0.025 0.05 1.7 C79 C80 SIMU 0.025 0.05 1.7 N19 C83 SIMU 0.025 0.05 1.7 C83 C84 SIMU 0.025 0.05 1.7 N19 C81 SIMU 0.025 0.05 1.7 C81 C82 SIMU 0.01 0.025 1.7 O9 C23 SIMU 0.01 0.025 1.7 O21 C56 SIMU 0.005 0.01 1.7 C50 C52 SIMU 0.005 0.01 1.7 N13 C52 DFIX 1.4300 0.0200 C50 C52 DFIX 1.3000 0.0200 C52 N13 FLAT 0.0500 C49 C50 C52 N13 N14 FLAT 0.0100 C39 C40 C35 C36 C37 C38 DFIX 1.4000 0.00200 C39 C40 DFIX 1.4000 0.00200 C40 C35 DFIX 1.4000 0.00200 C35 C36 DFIX 1.4000 0.00200 C36 C37 DFIX 1.4000 0.00200 C37 C38 DFIX 1.4000 0.00200 C38 C39 DFIX 1.5000 0.0200 N19 C79 DFIX 1.5000 0.0200 C79 C80 DFIX 1.5000 0.0200 N19 C83 DFIX 1.5000 0.0200 C83 C84 DFIX 1.5000 0.0200 N19 C81 DFIX 1.5000 0.0200 C81 C82 SIMU 0.025 0.05 1.7 C39 C40 SIMU 0.025 0.05 1.7 C40 C35 SIMU 0.025 0.05 1.7 C35 C36 SIMU 0.025 0.05 1.7 C38 C39 SIMU 0.025 0.05 1.7 C24 C25 SIMU 0.025 0.05 1.7 C25 C26 SIMU 0.025 0.05 1.7 C26 C27 SIMU 0.025 0.05 1.7 C27 C28 SIMU 0.025 0.05 1.7 C28 C29 SIMU 0.025 0.05 1.7 C29 C24 DANG 2.4618 0.0400 C40 C36 DANG 2.2261 0.0400 C36 C38 DANG 2.7271 0.0400 C37 C39 DANG 2.4642 0.0400 C38 C40 DFIX 1.43 0.0200 O9 C23 DFIX 1.43 0.0200 O13 C34 DFIX 1.43 0.0200 O17 C45 DFIX 1.43 0.0200 O5 C12 DFIX 1.43 0.0200 O21 C56 DFIX 1.43 0.0200 O1 C1 SIMU 0.005 0.01 1.7 C50 C52 WGHT 0.135800 122.735390 FVAR 1.00565 GD1 3 0.794158 -0.206070 0.265956 11.00000 0.01995 0.02435 = 0.03096 -0.00214 -0.00311 -0.00732 GD2 3 0.871170 -0.020074 0.250626 11.00000 0.01321 0.02375 = 0.02104 -0.00078 -0.00240 -0.00673 GD3 3 0.932806 0.174116 0.233920 11.00000 0.01635 0.02591 = 0.02460 0.00108 -0.00724 -0.00888 GD4 3 0.636425 -0.019779 0.250805 11.00000 0.01233 0.02560 = 0.02373 -0.00673 -0.00120 -0.00576 GD5 3 0.710216 0.182557 0.233887 11.00000 0.01518 0.02586 = 0.03094 -0.00670 -0.00755 -0.00545 GD6 3 0.490868 0.174724 0.235846 11.00000 0.01414 0.03031 = 0.03755 -0.01554 -0.00604 -0.00286 O1 5 0.641379 -0.342806 0.198768 11.00000 0.03973 0.05705 = 0.09919 -0.02549 -0.02345 -0.01479 O2 5 0.751388 -0.273659 0.208724 11.00000 0.03868 0.04027 = 0.03855 -0.01688 -0.00041 -0.01522 O3 5 0.911496 -0.148795 0.228858 11.00000 0.01948 0.02233 = 0.03497 -0.01036 -0.00203 -0.00620 O4 5 1.088978 -0.028165 0.154261 11.00000 0.02036 0.05061 = 0.05073 -0.00564 -0.00094 -0.01768 AFIX 147 H4 2 1.121163 -0.046504 0.177267 11.00000 -1.20000 AFIX 0 O5 5 1.209459 0.046315 0.169625 11.00000 0.02125 0.03356 = 0.06365 0.00096 -0.00665 -0.00187 O6 5 1.065778 0.129330 0.175707 11.00000 0.01559 0.03491 = 0.03802 0.00589 -0.00979 -0.00474 O7 5 0.823054 0.245846 0.193270 11.00000 0.01974 0.02292 = 0.03630 0.00140 -0.01590 -0.00551 O8 5 0.638341 0.331475 0.118518 11.00000 0.04865 0.04860 = 0.12182 0.03023 -0.06859 -0.01518 AFIX 147 H8 2 0.594374 0.323927 0.150188 11.00000 -1.20000 AFIX 0 O9 5 0.457992 0.431786 0.153732 11.00000 0.09290 0.04977 = 0.20630 -0.02750 -0.07435 -0.01798 O10 5 0.471001 0.285910 0.171181 11.00000 0.07332 0.03110 = 0.06927 -0.01555 -0.04493 -0.00028 O11 5 0.525883 0.047240 0.210347 11.00000 0.01542 0.02683 = 0.02455 -0.01448 -0.00750 -0.00098 O12 5 0.618513 -0.163170 0.159140 11.00000 0.03207 0.02785 = 0.05236 -0.01683 -0.01827 -0.00229 AFIX 147 H12 2 0.649840 -0.185512 0.182010 11.00000 -1.20000 AFIX 0 O13 5 0.268547 0.046702 0.326566 11.00000 0.02809 0.04175 = 0.06472 -0.01814 -0.01096 -0.01233 O14 5 0.376539 0.130374 0.302066 11.00000 0.01525 0.05402 = 0.05848 -0.03313 0.00135 -0.00742 O15 5 0.570128 0.244638 0.264130 11.00000 0.01828 0.03870 = 0.04685 -0.01452 -0.00517 0.00039 O16 5 0.718268 0.336763 0.317361 11.00000 0.02979 0.06317 = 0.11863 -0.05196 -0.03159 -0.00314 AFIX 147 H16 2 0.763741 0.307332 0.312045 11.00000 -1.20000 AFIX 0 O17 5 0.857113 0.427495 0.282967 11.00000 0.05897 0.03980 = 0.05684 -0.00046 -0.02180 -0.01539 O18 5 0.910791 0.285062 0.279435 11.00000 0.07485 0.02489 = 0.04489 -0.00142 -0.03276 -0.01455 O19 5 0.951898 0.045392 0.280753 11.00000 0.02334 0.02575 = 0.02276 0.00319 -0.00744 -0.00838 O20 5 0.954165 -0.167159 0.363679 11.00000 0.03754 0.02336 = 0.05037 0.00641 -0.02652 -0.00553 AFIX 147 H20 2 0.939289 -0.190082 0.339738 11.00000 -1.20000 AFIX 0 O21 5 1.010551 -0.341014 0.358595 11.00000 0.04329 0.07420 = 0.07659 0.00754 -0.01424 -0.00988 O22 5 0.867251 -0.275310 0.333586 11.00000 0.03285 0.04311 = 0.05160 0.01355 -0.01300 -0.00715 O23 5 0.651637 -0.149239 0.294786 11.00000 0.01520 0.02514 = 0.03742 0.00073 -0.00007 -0.00896 O24 5 0.423277 -0.029401 0.349596 11.00000 0.01133 0.05080 = 0.06238 -0.00694 -0.00670 -0.00156 AFIX 147 H24 2 0.420897 0.009873 0.321830 11.00000 -1.20000 AFIX 0 O25 5 0.776070 -0.099194 0.329179 11.00000 0.01745 0.02553 = 0.03283 -0.00721 0.00190 -0.00836 O26 5 0.646356 -0.036335 0.371823 11.00000 0.01945 0.03780 = 0.03954 -0.00682 -0.00485 -0.00884 O27 5 0.765563 -0.096999 0.184302 11.00000 0.01408 0.02162 = 0.03367 0.00175 -0.00180 -0.00703 O28 5 0.867411 -0.034914 0.132669 11.00000 0.02514 0.02990 = 0.02865 0.00091 -0.00587 -0.00663 O29 5 0.795401 0.036277 0.364633 11.00000 0.01860 0.03604 = 0.02962 -0.00157 -0.00106 -0.00975 O30 5 0.795792 0.154229 0.310212 11.00000 0.01265 0.03741 = 0.02664 -0.00326 -0.00165 -0.01259 O31 5 0.903095 0.091113 0.169434 11.00000 0.02354 0.02264 = 0.02696 0.00423 -0.00994 -0.00754 O32 5 0.810378 0.142613 0.116431 11.00000 0.01991 0.03080 = 0.03594 -0.00247 -0.01058 -0.00582 O33 5 0.636564 0.154170 0.162674 11.00000 0.01532 0.03077 = 0.03655 -0.01210 -0.00190 -0.00779 O34 5 0.686864 0.039115 0.127394 11.00000 0.01747 0.03314 = 0.03028 -0.00324 -0.00024 -0.00897 O35 5 0.627746 0.140803 0.358561 11.00000 0.02418 0.04354 = 0.03466 -0.01241 -0.00437 -0.00714 O36 5 0.557906 0.089742 0.314510 11.00000 0.02188 0.03314 = 0.02795 -0.01428 -0.00872 -0.00312 O37 5 0.738784 0.046992 0.244142 11.00000 0.01437 0.02324 = 0.05427 -0.00022 -0.01301 -0.01019 N1 4 0.916509 -0.259209 0.163051 11.00000 0.02332 0.03510 = 0.03484 -0.00076 -0.00483 -0.01050 N2 4 0.989002 -0.230805 0.144586 11.00000 0.02087 0.03288 = 0.03259 -0.00396 -0.00244 -0.00697 N3 4 1.025343 -0.066815 0.176543 11.00000 0.01675 0.03561 = 0.02136 -0.00293 -0.00153 -0.00793 N4 4 0.973607 0.252045 0.115515 11.00000 0.02960 0.03270 = 0.02369 0.00252 -0.01509 -0.01176 N5 4 0.911335 0.297635 0.090681 11.00000 0.03495 0.03045 = 0.04605 0.01546 -0.02633 -0.01547 N6 4 0.703549 0.298244 0.142108 11.00000 0.02967 0.02961 = 0.06299 0.00857 -0.03309 -0.00648 N7 4 0.470950 0.150142 0.124589 11.00000 0.02269 0.03185 = 0.05060 -0.01336 -0.01380 -0.00585 N8 4 0.485230 0.075392 0.110313 11.00000 0.02505 0.03163 = 0.03637 -0.00763 -0.00960 -0.00756 N9 4 0.590977 -0.089063 0.174548 11.00000 0.02131 0.02254 = 0.03623 -0.00846 -0.00538 -0.00402 N10 4 0.416620 0.253604 0.337242 11.00000 0.01884 0.03896 = 0.05100 -0.02308 -0.00488 -0.00426 N11 4 0.457779 0.301710 0.354111 11.00000 0.02451 0.05637 = 0.08026 -0.04567 -0.00888 -0.00256 N12 4 0.665161 0.301311 0.303048 11.00000 0.02618 0.04016 = 0.07463 -0.02141 -0.01823 -0.00846 N13 4 0.962196 0.146962 0.350242 11.00000 0.02925 0.02738 = 0.03148 -0.00542 -0.01182 -0.00649 N14 4 0.980518 0.070090 0.376320 11.00000 0.02942 0.03063 = 0.02875 -0.00333 -0.01123 -0.00214 N15 4 0.947412 -0.091502 0.337778 11.00000 0.02224 0.02266 = 0.03248 0.00436 -0.00965 0.00097 N16 4 0.696249 -0.260768 0.378832 11.00000 0.02411 0.03495 = 0.03056 0.00738 -0.00752 -0.01408 N17 4 0.611574 -0.231984 0.395213 11.00000 0.02159 0.03741 = 0.04317 0.00370 -0.00525 -0.00749 N18 4 0.504862 -0.068257 0.333329 11.00000 0.01401 0.03234 = 0.03435 -0.00611 -0.00240 -0.00516 C1 1 0.578521 -0.370674 0.191735 11.00000 0.09478 0.20113 = 0.12025 -0.03134 -0.05232 -0.06032 AFIX 137 H1A 2 0.553776 -0.335471 0.159671 11.00000 -1.20000 H1B 2 0.536567 -0.376595 0.238426 11.00000 -1.20000 H1C 2 0.601322 -0.419419 0.172194 11.00000 -1.20000 AFIX 0 C2 1 0.721671 -0.363670 0.157428 11.00000 0.04135 0.03864 = 0.04496 0.00028 -0.01649 -0.02239 C3 1 0.746862 -0.419350 0.112394 11.00000 0.06149 0.04096 = 0.04714 0.00161 -0.02104 -0.01745 AFIX 43 H3 2 0.708230 -0.443889 0.107912 11.00000 -1.20000 AFIX 0 C4 1 0.831800 -0.439539 0.072646 11.00000 0.08319 0.05207 = 0.04667 -0.02288 -0.02083 -0.01937 AFIX 43 H4A 2 0.849604 -0.477497 0.041043 11.00000 -1.20000 AFIX 0 C5 1 0.888288 -0.405197 0.079173 11.00000 0.06013 0.02720 = 0.04057 0.00581 -0.02258 -0.00508 AFIX 43 H5 2 0.944888 -0.419915 0.053029 11.00000 -1.20000 AFIX 0 C6 1 0.861935 -0.348250 0.124670 11.00000 0.03905 0.02052 = 0.03846 -0.00109 -0.01289 -0.00503 C7 1 0.778811 -0.327116 0.165808 11.00000 0.03705 0.03601 = 0.04375 -0.01019 -0.02058 -0.00743 C8 1 0.925970 -0.311510 0.124316 11.00000 0.04210 0.02266 = 0.03470 -0.00450 -0.00563 0.00026 AFIX 43 H8A 2 0.979681 -0.327701 0.092520 11.00000 -1.20000 AFIX 0 C9 1 0.978831 -0.174293 0.178738 11.00000 0.02333 0.02930 = 0.03870 -0.00061 -0.00658 -0.01150 C10 1 1.047472 -0.133132 0.157026 11.00000 0.01252 0.03790 = 0.02799 -0.00197 0.00033 -0.00409 C11 1 1.132919 -0.168034 0.116560 11.00000 0.02661 0.05640 = 0.04001 -0.01479 0.00720 -0.00633 AFIX 137 H11A 2 1.138385 -0.167438 0.066625 11.00000 -1.20000 H11B 2 1.145716 -0.219967 0.136496 11.00000 -1.20000 H11C 2 1.171004 -0.139715 0.119873 11.00000 -1.20000 AFIX 0 C12 1 1.284418 -0.007927 0.158117 11.00000 0.03122 0.06110 = 0.08707 0.00105 -0.00545 0.00479 AFIX 137 H12A 2 1.304737 -0.021441 0.109165 11.00000 -1.20000 H12B 2 1.274627 -0.052805 0.191147 11.00000 -1.20000 H12C 2 1.325279 0.013278 0.166148 11.00000 -1.20000 AFIX 0 C13 1 1.209669 0.108655 0.121266 11.00000 0.02100 0.03874 = 0.04191 -0.01043 -0.00856 -0.01220 C14 1 1.279311 0.129323 0.070471 11.00000 0.01973 0.02276 = 0.05004 0.01590 -0.00439 -0.00561 AFIX 43 H14 2 1.331849 0.099100 0.066801 11.00000 -1.20000 AFIX 0 C15 1 1.272463 0.193076 0.025713 11.00000 0.03019 0.03661 = 0.06058 -0.00669 0.00665 -0.02308 AFIX 43 H15 2 1.320716 0.208812 -0.006466 11.00000 -1.20000 AFIX 0 C16 1 1.196296 0.235266 0.026403 11.00000 0.02870 0.04477 = 0.04088 0.00100 -0.01078 -0.02278 AFIX 43 H16A 2 1.192702 0.277806 -0.007003 11.00000 -1.20000 AFIX 0 C17 1 1.123016 0.214750 0.077460 11.00000 0.03500 0.03766 = 0.02789 -0.00890 -0.00253 -0.01752 C18 1 1.127816 0.151096 0.126855 11.00000 0.02128 0.03212 = 0.03095 -0.00548 -0.00182 -0.01585 C19 1 1.046931 0.257044 0.073045 11.00000 0.02311 0.03933 = 0.02697 0.00368 -0.01006 -0.01329 AFIX 43 H19A 2 1.050040 0.293996 0.033729 11.00000 -1.20000 AFIX 0 C20 1 0.840034 0.287602 0.133341 11.00000 0.02691 0.02322 = 0.05225 -0.00123 -0.02338 -0.00590 C21 1 0.770191 0.324759 0.107478 11.00000 0.04231 0.02541 = 0.06019 0.01662 -0.03567 -0.01209 C22 1 0.781127 0.378093 0.040341 11.00000 0.06019 0.07080 = 0.10270 0.06375 -0.05044 -0.04923 AFIX 137 H22A 2 0.760879 0.360723 0.008147 11.00000 -1.20000 H22B 2 0.839430 0.379563 0.016962 11.00000 -1.20000 H22C 2 0.750140 0.428463 0.052524 11.00000 -1.20000 AFIX 0 C23 1 0.469033 0.505581 0.135375 11.00000 0.13734 0.10310 = 0.22886 -0.02505 -0.06070 -0.01254 AFIX 137 H23A 2 0.416954 0.538701 0.135136 11.00000 -1.20000 H23B 2 0.510267 0.509613 0.088007 11.00000 -1.20000 H23C 2 0.487648 0.520365 0.170065 11.00000 -1.20000 AFIX 0 C24 1 0.442949 0.397049 0.102051 11.00000 0.05449 0.04161 = 0.09480 0.00027 -0.03767 -0.01212 C25 1 0.423340 0.435034 0.042544 11.00000 0.10751 0.05509 = 0.12892 0.01377 -0.06572 -0.02874 AFIX 43 H25 2 0.418311 0.487910 0.033484 11.00000 -1.20000 AFIX 0 C26 1 0.411133 0.393596 -0.003862 11.00000 0.12952 0.06824 = 0.12659 0.02678 -0.07987 -0.03797 AFIX 43 H26 2 0.398271 0.419499 -0.044370 11.00000 -1.20000 AFIX 0 C27 1 0.417190 0.317664 0.007528 11.00000 0.11947 0.06800 = 0.09483 0.02565 -0.08151 -0.03827 AFIX 43 H27 2 0.404990 0.291227 -0.022313 11.00000 -1.20000 AFIX 0 C28 1 0.443219 0.278153 0.067511 11.00000 0.06161 0.05533 = 0.05766 0.01988 -0.04287 -0.02885 C29 1 0.453223 0.318046 0.116631 11.00000 0.02766 0.03811 = 0.06614 0.00600 -0.01834 -0.00670 C30 1 0.456981 0.197543 0.071235 11.00000 0.06386 0.04518 = 0.05822 0.00945 -0.04816 -0.01945 AFIX 43 H30 2 0.455953 0.176557 0.032071 11.00000 -1.20000 AFIX 0 C31 1 0.515424 0.029063 0.154747 11.00000 0.01365 0.02769 = 0.03607 -0.01336 -0.00482 -0.00454 C32 1 0.543658 -0.052916 0.140688 11.00000 0.01489 0.04079 = 0.02418 -0.01136 -0.00489 -0.00698 C33 1 0.518735 -0.079019 0.087091 11.00000 0.04743 0.04912 = 0.06220 -0.03190 -0.02698 -0.00367 AFIX 137 H33A 2 0.565236 -0.084863 0.042673 11.00000 -1.20000 H33B 2 0.472838 -0.041956 0.078181 11.00000 -1.20000 H33C 2 0.501847 -0.127293 0.105398 11.00000 -1.20000 AFIX 0 C34 1 0.215506 -0.005724 0.347458 11.00000 0.04004 0.05244 = 0.08816 0.00483 -0.02006 -0.02774 AFIX 137 H34A 2 0.209624 -0.027017 0.396402 11.00000 -1.20000 H34B 2 0.238861 -0.046021 0.315774 11.00000 -1.20000 H34C 2 0.161566 0.019826 0.344561 11.00000 -1.20000 AFIX 0 C35 1 0.244751 0.108912 0.362144 11.00000 0.01698 0.03893 = 0.04841 -0.00868 -0.00901 -0.00132 C36 1 0.162787 0.126943 0.405703 11.00000 0.05022 0.05068 = 0.05088 -0.00518 -0.01669 -0.01017 AFIX 43 H36 2 0.124668 0.095761 0.413563 11.00000 -1.20000 AFIX 0 C37 1 0.141193 0.194306 0.436798 11.00000 0.02889 0.02913 = 0.03287 -0.00077 -0.00830 -0.00652 AFIX 43 H37 2 0.085815 0.211527 0.464837 11.00000 -1.20000 AFIX 0 C38 1 0.200120 0.236723 0.427157 11.00000 0.02624 0.04750 = 0.05455 -0.01273 -0.00931 0.00629 AFIX 43 H38 2 0.183936 0.280481 0.451566 11.00000 -1.20000 AFIX 0 C39 1 0.281821 0.217547 0.383162 11.00000 0.02146 0.05144 = 0.03362 -0.01064 -0.01163 -0.00310 C40 1 0.304448 0.151215 0.350099 11.00000 0.01424 0.03734 = 0.03274 -0.00598 -0.00275 -0.00132 C41 1 0.340918 0.261682 0.380200 11.00000 0.01632 0.06035 = 0.04148 -0.03534 -0.00720 0.00129 AFIX 43 H41 2 0.322635 0.299308 0.412198 11.00000 -1.20000 AFIX 0 C42 1 0.534777 0.289510 0.315806 11.00000 0.02767 0.03710 = 0.06977 -0.03211 -0.02084 0.00263 C43 1 0.590801 0.329943 0.329947 11.00000 0.03439 0.05362 = 0.11841 -0.06221 -0.02244 0.00504 C44 1 0.554615 0.391982 0.378744 11.00000 0.03593 0.17994 = 0.25077 -0.18486 -0.02851 0.00121 AFIX 137 H44A 2 0.584859 0.385112 0.411946 11.00000 -1.20000 H44B 2 0.496855 0.390598 0.405432 11.00000 -1.20000 H44C 2 0.558631 0.440527 0.350546 11.00000 -1.20000 AFIX 0 C45 1 0.821448 0.505527 0.286334 11.00000 0.11685 0.06654 = 0.09424 -0.00881 -0.04416 -0.00515 AFIX 137 H45A 2 0.857761 0.531220 0.296053 11.00000 -1.20000 H45B 2 0.768098 0.511945 0.324384 11.00000 -1.20000 H45C 2 0.814007 0.526969 0.240875 11.00000 -1.20000 AFIX 0 C46 1 0.882758 0.393925 0.335663 11.00000 0.04554 0.04581 = 0.08800 -0.02785 -0.03874 0.00490 C47 1 0.878133 0.425804 0.394777 11.00000 0.10416 0.04652 = 0.08818 -0.02560 -0.04694 0.00302 AFIX 43 H47 2 0.860556 0.478554 0.396441 11.00000 -1.20000 AFIX 0 C48 1 0.898941 0.381660 0.452456 11.00000 0.13217 0.06247 = 0.07864 -0.02167 -0.06605 0.00129 AFIX 43 H48 2 0.895137 0.404590 0.492313 11.00000 -1.20000 AFIX 0 C49 1 0.924735 0.305201 0.450252 11.00000 0.08669 0.04063 = 0.07960 -0.02003 -0.05457 0.00030 AFIX 43 H49 2 0.938562 0.276208 0.489253 11.00000 -1.20000 AFIX 0 C50 1 0.931498 0.268111 0.392561 11.00000 0.03864 0.03534 = 0.03887 -0.00788 -0.01841 -0.00423 C51 1 0.909825 0.313911 0.334119 11.00000 0.04275 0.03531 = 0.04732 -0.01676 -0.02051 -0.00750 C52 1 0.945694 0.182099 0.405814 11.00000 0.03341 0.03163 = 0.03027 -0.00430 -0.01350 -0.00256 AFIX 43 H52 2 0.942653 0.156409 0.451267 11.00000 -1.20000 AFIX 0 C53 1 0.971933 0.025927 0.339068 11.00000 0.01906 0.03618 = 0.01939 0.00377 -0.00632 -0.00708 C54 1 0.980369 -0.055935 0.366160 11.00000 0.02068 0.02257 = 0.04561 0.00830 -0.01060 -0.00625 C55 1 1.020365 -0.086943 0.420824 11.00000 0.05083 0.04322 = 0.06534 0.02483 -0.04312 -0.02639 AFIX 137 H55A 2 0.978218 -0.093508 0.467279 11.00000 -1.20000 H55B 2 1.052855 -0.052188 0.422895 11.00000 -1.20000 H55C 2 1.056345 -0.135541 0.408272 11.00000 -1.20000 AFIX 0 C56 1 1.038551 -0.360829 0.287389 11.00000 0.09196 0.13832 = 0.13052 0.02025 -0.00980 -0.00059 AFIX 137 H56A 2 1.001176 -0.331141 0.262785 11.00000 -1.20000 H56B 2 1.039895 -0.414300 0.288076 11.00000 -1.20000 H56C 2 1.093793 -0.350640 0.262455 11.00000 -1.20000 AFIX 0 C57 1 0.937505 -0.363993 0.401248 11.00000 0.04569 0.02678 = 0.04990 0.00149 -0.01980 -0.00168 C58 1 0.935642 -0.416118 0.459264 11.00000 0.05472 0.02742 = 0.05830 -0.00632 -0.02844 0.01066 AFIX 43 H58 2 0.984974 -0.438148 0.469075 11.00000 -1.20000 AFIX 0 C59 1 0.862483 -0.436774 0.503509 11.00000 0.07029 0.02941 = 0.04045 0.00565 -0.02254 -0.00592 AFIX 43 H59 2 0.862298 -0.473661 0.542525 11.00000 -1.20000 AFIX 0 C60 1 0.791142 -0.404171 0.490946 11.00000 0.06186 0.02316 = 0.04536 0.00346 -0.01901 -0.00992 AFIX 43 H60 2 0.741304 -0.418522 0.521214 11.00000 -1.20000 AFIX 0 C61 1 0.790737 -0.348222 0.432230 11.00000 0.04148 0.02195 = 0.04266 -0.00861 -0.01605 -0.00359 C62 1 0.864291 -0.327372 0.386541 11.00000 0.03655 0.03354 = 0.04183 -0.00526 -0.01406 -0.00989 C63 1 0.711282 -0.311791 0.427760 11.00000 0.03172 0.02108 = 0.03365 -0.00154 0.00019 -0.00840 AFIX 43 H63 2 0.665095 -0.326584 0.464352 11.00000 -1.20000 AFIX 0 C64 1 0.596469 -0.174522 0.348892 11.00000 0.02607 0.03580 = 0.02440 -0.00132 -0.00917 -0.01721 C65 1 0.510330 -0.132519 0.365166 11.00000 0.01780 0.04189 = 0.03237 -0.00853 0.00369 -0.01181 C66 1 0.441520 -0.168495 0.417380 11.00000 0.02150 0.09456 = 0.02836 0.00101 0.00484 -0.02773 AFIX 137 H66A 2 0.436969 -0.162988 0.465958 11.00000 -1.20000 H66B 2 0.453192 -0.221892 0.410627 11.00000 -1.20000 H66C 2 0.389808 -0.143918 0.409389 11.00000 -1.20000 AFIX 0 C67 1 0.710327 -0.075464 0.382428 11.00000 0.01804 0.05081 = 0.02885 -0.00225 0.00016 -0.01603 C68 1 0.713192 -0.094392 0.455810 11.00000 0.02271 0.04778 = 0.02889 0.00792 -0.00598 -0.00877 AFIX 137 H68A 2 0.681505 -0.052226 0.484154 11.00000 -1.20000 H68B 2 0.770280 -0.104380 0.454363 11.00000 -1.20000 H68C 2 0.689683 -0.139062 0.477341 11.00000 -1.20000 AFIX 0 C69 1 0.819044 -0.072617 0.128236 11.00000 0.02039 0.02710 = 0.02727 0.00120 -0.00859 -0.00159 C70 1 0.824706 -0.090615 0.057630 11.00000 0.03063 0.05205 = 0.02757 -0.01680 -0.00007 -0.01289 AFIX 137 H70A 2 0.844442 -0.050781 0.021279 11.00000 -1.20000 H70B 2 0.770400 -0.094478 0.058887 11.00000 -1.20000 H70C 2 0.863005 -0.138438 0.046237 11.00000 -1.20000 AFIX 0 C71 1 0.783076 0.105979 0.367202 11.00000 0.01176 0.03950 = 0.02843 -0.01203 -0.00565 -0.00684 C72 1 0.753647 0.137744 0.437895 11.00000 0.03150 0.05927 = 0.03296 -0.02296 0.00177 -0.01416 AFIX 137 H72A 2 0.723508 0.103665 0.474957 11.00000 -1.20000 H72B 2 0.717410 0.186827 0.435732 11.00000 -1.20000 H72C 2 0.800887 0.143397 0.448966 11.00000 -1.20000 AFIX 0 C73 1 0.882324 0.111524 0.112340 11.00000 0.01886 0.03767 = 0.02724 -0.00183 -0.01376 -0.01011 C74 1 0.946490 0.099477 0.042547 11.00000 0.02812 0.05005 = 0.03238 -0.00078 -0.01038 -0.01051 AFIX 137 H74A 2 0.928428 0.072585 0.015258 11.00000 -1.20000 H74B 2 0.997247 0.069784 0.049379 11.00000 -1.20000 H74C 2 0.956431 0.148059 0.016626 11.00000 -1.20000 AFIX 0 C75 1 0.668683 0.108168 0.113812 11.00000 0.01841 0.03524 = 0.02411 -0.00753 -0.00325 -0.00919 C76 1 0.683849 0.140985 0.037034 11.00000 0.03036 0.05486 = 0.02924 -0.00085 -0.00678 -0.01172 AFIX 137 H76A 2 0.725306 0.105164 0.005368 11.00000 -1.20000 H76B 2 0.703384 0.187857 0.029810 11.00000 -1.20000 H76C 2 0.632628 0.151079 0.026454 11.00000 -1.20000 AFIX 0 C77 1 0.569419 0.110094 0.365966 11.00000 0.02051 0.03108 = 0.03283 -0.00940 -0.00452 -0.00242 C78 1 0.507783 0.098456 0.439137 11.00000 0.02458 0.06565 = 0.03698 -0.01726 0.00343 -0.01659 AFIX 137 H78A 2 0.536704 0.078739 0.473381 11.00000 -1.20000 H78B 2 0.475626 0.062650 0.438632 11.00000 -1.20000 H78C 2 0.471037 0.146428 0.452861 11.00000 -1.20000 AFIX 0 N19 4 1.168437 0.357838 0.211892 10.50000 0.04239 0.03521 = 0.08852 -0.00380 -0.00650 -0.02861 AFIX 13 H19 2 1.123079 0.359773 0.198800 10.50000 -1.20000 AFIX 0 C79 1 1.204565 0.275147 0.209933 10.50000 0.04889 0.04280 = 0.08050 -0.01422 -0.03625 -0.01120 AFIX 23 H79A 2 1.221931 0.261932 0.160593 10.50000 -1.20000 H79B 2 1.253974 0.264012 0.224286 10.50000 -1.20000 AFIX 0 C80 1 1.146338 0.228175 0.257092 10.50000 0.04360 0.07915 = 0.04466 -0.01073 -0.02233 0.01050 AFIX 137 H80A 2 1.120384 0.247642 0.303813 10.50000 -1.20000 H80B 2 1.175888 0.176420 0.262289 10.50000 -1.20000 H80C 2 1.104131 0.229312 0.236448 10.50000 -1.20000 AFIX 0 C81 1 1.126446 0.388833 0.281973 10.50000 0.10546 0.04529 = 0.11016 -0.03149 -0.03831 -0.01946 AFIX 23 H81A 2 1.087662 0.354581 0.305768 10.50000 -1.20000 H81B 2 1.170306 0.371403 0.303456 10.50000 -1.20000 AFIX 0 C82 1 1.081002 0.456812 0.319207 10.50000 0.11427 0.16955 = 0.08312 -0.04492 -0.02323 -0.02853 AFIX 137 H82A 2 1.109180 0.498528 0.296230 10.50000 -1.20000 H82B 2 1.078527 0.447133 0.368944 10.50000 -1.20000 H82C 2 1.025203 0.469793 0.317106 10.50000 -1.20000 AFIX 0 C83 1 1.220069 0.396529 0.145760 10.50000 0.07330 0.04446 = 0.12218 0.02903 -0.00015 -0.02594 AFIX 23 H83A 2 1.270077 0.401155 0.153906 10.50000 -1.20000 H83B 2 1.237797 0.363716 0.106888 10.50000 -1.20000 AFIX 0 C84 1 1.181159 0.472873 0.120713 10.50000 0.10024 0.11440 = 0.13893 0.02479 -0.00017 -0.06488 AFIX 33 H84A 2 1.165794 0.469055 0.079872 10.50000 -1.20000 H84B 2 1.220232 0.506466 0.106703 10.50000 -1.20000 H84C 2 1.132053 0.492935 0.159216 10.50000 -1.20000 HKLF 4 REM _MUA1950 REM R1 = 0.0925 for 20749 Fo > 4sig(Fo) and 0.1023 for all 24712 data REM 1341 parameters refined using 182 restraints END WGHT 0.1358 122.8577 REM Highest difference peak 12.756, deepest hole -2.631, 1-sigma level 0.333 Q1 1 0.1457 0.1838 0.4139 11.00000 0.05 12.76 Q2 1 0.9193 0.1751 0.4170 11.00000 0.05 12.23 Q3 1 0.3626 0.1804 0.4163 11.00000 0.05 12.18 Q4 1 0.4438 -0.0213 0.0730 11.00000 0.05 10.21 Q5 1 0.2036 0.9785 0.0756 11.00000 0.05 9.31 Q6 1 0.3022 -0.0149 0.4390 11.00000 0.05 8.75 Q7 1 1.0646 -0.0156 0.4395 11.00000 0.05 8.03 Q8 1 1.0664 0.1719 0.0535 11.00000 0.05 5.34 Q9 1 1.2819 0.1807 0.0504 11.00000 0.05 4.25 Q10 1 0.5037 0.1739 0.0497 11.00000 0.05 4.16 Q11 1 0.9777 0.1944 0.3863 11.00000 0.05 2.61 Q12 1 1.0200 -0.2014 0.2796 11.00000 0.05 2.21 Q13 1 0.1568 0.1896 0.4606 11.00000 0.05 2.04 Q14 1 1.0957 -0.0163 0.2523 11.00000 0.05 2.01 Q15 1 0.4214 -0.0220 0.2561 11.00000 0.05 1.92 Q16 1 0.3613 0.7945 0.0924 11.00000 0.05 1.77 Q17 1 0.8001 -0.1949 0.2857 11.00000 0.05 1.71 Q18 1 0.1666 0.1236 0.4312 11.00000 0.05 1.49 Q19 1 1.0771 -0.3510 0.3701 11.00000 0.05 1.46 Q20 1 0.4807 0.2530 0.2493 11.00000 0.05 1.41 Q21 1 1.0437 0.2229 0.0206 11.00000 0.05 1.40 Q22 1 0.9989 -0.1646 0.2407 11.00000 0.05 1.36 Q23 1 0.9818 0.3789 0.3959 11.00000 0.05 1.34 Q24 1 0.7227 0.1053 0.2296 11.00000 0.05 1.30 Q25 1 0.2983 0.0233 0.3856 11.00000 0.05 1.27 Q26 1 0.5226 0.2263 0.1963 11.00000 0.05 1.25 Q27 1 0.6596 0.0388 0.3242 11.00000 0.05 1.25 Q28 1 0.6797 0.1239 0.2780 11.00000 0.05 1.24 Q29 1 0.2025 0.2366 0.4481 11.00000 0.05 1.23 Q30 1 1.2441 0.2358 0.2131 11.00000 0.05 1.21 Q31 1 0.1573 0.3314 0.4948 11.00000 0.05 1.20 Q32 1 0.5650 0.1578 0.2974 11.00000 0.05 1.17 Q33 1 0.8441 -0.0850 0.2928 11.00000 0.05 1.16 Q34 1 0.5131 0.3174 0.0479 11.00000 0.05 1.14 Q35 1 0.9001 0.4343 0.3139 11.00000 0.05 1.14 Q36 1 0.6463 0.1055 0.3016 11.00000 0.05 1.14 Q37 1 1.1744 0.2713 0.2470 11.00000 0.05 1.13 Q38 1 1.0775 0.1454 0.3402 11.00000 0.05 1.13 Q39 1 0.6156 0.4319 0.1082 11.00000 0.05 1.12 Q40 1 0.9077 -0.0224 0.2129 11.00000 0.05 1.11 Q41 1 0.6858 0.4185 0.0724 11.00000 0.05 1.11 Q42 1 0.6969 0.0806 0.5427 11.00000 0.05 1.10 Q43 1 0.5205 -0.0218 0.3419 11.00000 0.05 1.10 Q44 1 0.4219 -0.1895 0.3795 11.00000 0.05 1.09 Q45 1 0.6793 -0.0207 0.2036 11.00000 0.05 1.08 Q46 1 0.7804 -0.1699 0.2017 11.00000 0.05 1.08 Q47 1 1.0613 0.2609 0.0801 11.00000 0.05 1.06 Q48 1 0.5527 0.4041 0.0960 11.00000 0.05 1.06 Q49 1 0.6138 -0.0844 0.2851 11.00000 0.05 1.06 Q50 1 0.6627 0.1892 0.2811 11.00000 0.05 1.06 Q51 1 0.5059 0.0463 0.3639 11.00000 0.05 1.06 Q52 1 0.8651 0.4281 0.2130 11.00000 0.05 1.05 Q53 1 0.7786 -0.0472 0.4513 11.00000 0.05 1.05 Q54 1 0.7577 -0.0232 0.2161 11.00000 0.05 1.05 Q55 1 0.9988 0.2549 0.4470 11.00000 0.05 1.05 Q56 1 0.6622 0.1049 -0.0080 11.00000 0.05 1.05 Q57 1 0.8224 -0.2759 0.2477 11.00000 0.05 1.04 Q58 1 1.2577 0.2318 0.0252 11.00000 0.05 1.04 Q59 1 1.0850 0.4049 0.3262 11.00000 0.05 1.03 Q60 1 0.8620 0.0116 0.1890 11.00000 0.05 1.03 Q61 1 1.2044 0.3962 0.2964 11.00000 0.05 1.02 Q62 1 0.7610 -0.0278 0.2923 11.00000 0.05 1.02 Q63 1 0.7153 0.1542 0.2984 11.00000 0.05 1.02 Q64 1 0.5197 0.2585 0.0057 11.00000 0.05 1.02 Q65 1 0.8952 0.5064 0.3029 11.00000 0.05 1.02 Q66 1 0.6861 0.0686 0.2815 11.00000 0.05 1.02 Q67 1 1.1697 -0.1780 0.1690 11.00000 0.05 1.01 Q68 1 0.5826 -0.0672 0.2623 11.00000 0.05 1.01 Q69 1 0.9194 0.1436 0.3089 11.00000 0.05 1.00 Q70 1 0.9012 0.1118 0.2821 11.00000 0.05 1.00 Q71 1 0.8945 0.2740 0.3520 11.00000 0.05 1.00 Q72 1 1.0636 0.3456 0.3122 11.00000 0.05 0.99 Q73 1 0.6065 -0.1436 0.4205 11.00000 0.05 0.99 Q74 1 0.5644 0.3750 0.1988 11.00000 0.05 0.99 Q75 1 0.2212 0.1567 0.4969 11.00000 0.05 0.99 ; data_2_Revised _database_code_depnum_ccdc_archive 'CCDC 910739' #TrackingRef 'Revised_Ln6_Combined_CIF.cif' # start Validation Reply Form _vrf_CHEMW03_2_Revised ; 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. 6 H2O molecules and 1 triethylamine that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT043_2_Revised ; PROBLEM: Check Reported Molecular Weight RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 6 H2O molecules and 1 triethylamine that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_DIFMX01_2_Revised ; PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 RESPONSE: Electron density synthesis with coefficients Fo-Fc Electron density synthesis with coefficients Fo-Fc Highest peak 10.51 at 0.9032 0.1746 0.4271 [ 1.05 A from C52 ] Deepest hole -2.99 at 0.7198 0.1437 0.2512 [ 0.73 A from TB5 ] ; _vrf_PLAT097_2_Revised ; PROBLEM: Large Reported Max. (Positive) Residual Density 10.52 eA-3 RESPONSE: Electron density synthesis with coefficients Fo-Fc Highest peak 10.51 at 0.9032 0.1746 0.4271 [ 1.05 A from C52 ] Deepest hole -2.99 at 0.7198 0.1437 0.2512 [ 0.73 A from TB5 ] ; _vrf_PLAT220_2_Revised ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) RESPONSE: This is a terminal O-CH3 group. Similarity restraints have been applied. Please see refine_special_details for more details. This does not represent an incorrectly identified atom-type. ; _vrf_DIFMX02_2_Revised ; PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 RESPONSE: Electron density synthesis with coefficients Fo-Fc Highest peak 10.51 at 0.9032 0.1746 0.4271 [ 1.05 A from C52 ] Deepest hole -2.99 at 0.7198 0.1437 0.2512 [ 0.73 A from TB5 ] ; _vrf_PLAT041_2_Revised ; 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. 6 H2O molecules and 1 triethylamine that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT042_2_Revised ; PROBLEM: Calc. and Reported MoietyFormula Strings Differ RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 6 H2O molecules and 1 triethylamine that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT094_2_Revised ; PROBLEM: Ratio of Maximum / Minimum Residual Density ....3.52 RESPONSE: Electron density synthesis with coefficients Fo-Fc Highest peak 10.51 at 0.9032 0.1746 0.4271 [ 1.05 A from C52 ] Deepest hole -2.99 at 0.7198 0.1437 0.2512 [ 0.73 A from TB5 ] ; _vrf_FORMU01_2_Revised ; 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. 6 H2O molecules and 1 triethylamine that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_CELLZ01_2_Revised ; 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. 6 H2O molecules and 1 triethylamine that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT068_2_Revised ; 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. 6 H2O molecules and 1 triethylamine that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT002_2_Revised ; PROBLEM: Number of Distance or Angle Restraints on AtSite RESPONSE: Please see refine_special_details for information. ; _vrf_PLAT003_2_Revised ; PROBLEM: Number of Uiso or Uij Restrained Atom Sites RESPONSE: Please see refine_special_details for information. ; _vrf_PLAT007_2_Revised ; PROBLEM: Note: Number of Unrefined D-H Atoms RESPONSE: These H-atoms were introduced in calculated postions and refined using AFIX 147. ; _vrf_PLAT606_2_Revised ; 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_PLAT860_2_Revised ; PROBLEM: Note: Number of Least-Squares Restraints RESPONSE: Please see refine_special_details for information. ; _vrf_PLAT869_2_Revised ; 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. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H112 N19 O43 Tb6' _chemical_formula_sum 'C84 H112 N19 O43 Tb6' _chemical_formula_weight 3029.46 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 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 17.8354(13) _cell_length_b 18.4624(14) _cell_length_c 20.2003(14) _cell_angle_alpha 79.794(6) _cell_angle_beta 68.816(5) _cell_angle_gamma 76.342(5) _cell_volume 5995.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 32066 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2966 _exptl_absorpt_coefficient_mu 3.569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.430 _exptl_absorpt_correction_T_max 0.725 _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 48493 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 26.50 _reflns_number_total 24448 _reflns_number_gt 20540 _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. DFIX, DANG and FLAT restraints were applied to the ring consisting of C34-C39. ISOR restraints were applied to C36 and C51. SIMU restraints were applied to the C49-C51, N13-C51, C35-C36, C37-C36, O7-C77 and O21-C78 bonds. Further DFIX and SIMU restraints were applied to the methoxide groups. Please see iucr_refine_instructions_details for a full listing of restraints. The nominal formula is: (L-2H)6Tb6(CH3COO)6(O)(Et3NH)(H2O)6 Which is in agreement with the dried elemental analysis results: [Tb6(C11H11N3O4)6(O)(CH3COO)6]((CH3CH2)3NH): Calc: C, 34.54; H, 3.45; N, 9.11. Found: C, 34.41; H, 3.28; N, 9.15 Note that the triethylamine cation could not be located from difference maps, and that significant disorder was observed outside the main molecular fragment. For further details, see platon_squeeze_details and iucr_refine_instructions_details. ; _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^)+(0.1169P)^2^+89.7800P] 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 24448 _refine_ls_number_parameters 1276 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.2152 _refine_ls_wR_factor_gt 0.2070 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _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 0.500 0.500 0.500 1574 334 ' ' 2 0.336 0.548 0.788 18 2 ' ' 3 0.663 0.452 0.212 17 4 ' ' _platon_squeeze_details ; The Platon SQUEEZE procedure was applied to recover 334 electrons per unit cell in one void that was sufficiently large to contain a small molecule (total volume 1574 ^A^3); that is 167 electrons per formula unit. Elemental analysis indicates that the void contains a triethylamine molecule (102 electrons), while the remaining electrons are attributed to lattice solvent water molecules (6 molecules per formula unit. These 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 Tb1 Tb 0.79229(3) -0.20515(3) 0.26610(3) 0.02706(12) Uani 1 1 d . . . Tb2 Tb 0.87082(2) -0.02023(2) 0.25036(2) 0.02035(11) Uani 1 1 d . . . Tb3 Tb 0.93342(3) 0.17331(3) 0.23314(2) 0.02258(12) Uani 1 1 d . . . Tb4 Tb 0.63644(2) -0.01990(2) 0.25090(2) 0.02134(11) Uani 1 1 d . . . Tb5 Tb 0.71190(3) 0.18152(3) 0.23347(2) 0.02341(12) Uani 1 1 d . . . Tb6 Tb 0.49310(3) 0.17374(3) 0.23623(3) 0.02660(12) Uani 1 1 d . . . O1 O 0.6378(6) -0.3391(6) 0.2001(6) 0.061(3) Uani 1 1 d D . . O2 O 0.7476(5) -0.2712(5) 0.2096(4) 0.0411(18) Uani 1 1 d . . . O3 O 0.9086(4) -0.1474(4) 0.2284(4) 0.0260(14) Uani 1 1 d . . . O4 O 1.0886(4) -0.0289(5) 0.1548(4) 0.0395(18) Uani 1 1 d . . . H4 H 1.0707 0.0161 0.1631 0.047 Uiso 1 1 calc R . . O5 O 1.2087(4) 0.0460(4) 0.1711(5) 0.0420(19) Uani 1 1 d D . . O6 O 1.0655(4) 0.1288(4) 0.1762(4) 0.0319(16) Uani 1 1 d . . . O7 O 0.8238(4) 0.2448(4) 0.1928(4) 0.0281(14) Uani 1 1 d . . . O8A O 0.6403(6) 0.3298(5) 0.1173(6) 0.060(3) Uani 1 1 d . . . H8A H 0.5958 0.3270 0.1506 0.071 Uiso 1 1 calc R . . O9 O 0.4608(8) 0.4297(6) 0.1551(8) 0.091(4) Uani 1 1 d DU . . O10 O 0.4777(6) 0.2840(4) 0.1707(5) 0.048(2) Uani 1 1 d . . . O11 O 0.5267(4) 0.0466(4) 0.2111(4) 0.0270(14) Uani 1 1 d . . . O12 O 0.6180(5) -0.1629(4) 0.1605(5) 0.0384(18) Uani 1 1 d . . . H12 H 0.5795 -0.1792 0.1573 0.046 Uiso 1 1 calc R . . O13 O 0.2699(4) 0.0462(5) 0.3260(5) 0.047(2) Uani 1 1 d D . . O14 O 0.3790(4) 0.1298(5) 0.3014(4) 0.0407(19) Uani 1 1 d . . . O15 O 0.5730(4) 0.2422(4) 0.2643(4) 0.0332(16) Uani 1 1 d . . . O16 O 0.7218(5) 0.3359(6) 0.3152(6) 0.059(3) Uani 1 1 d . . . H16 H 0.7681 0.3079 0.3074 0.071 Uiso 1 1 calc R . . O17 O 0.8580(5) 0.4269(4) 0.2808(5) 0.045(2) Uani 1 1 d D . . O18 O 0.9118(5) 0.2831(4) 0.2769(4) 0.0399(18) Uani 1 1 d . . . O19 O 0.9516(4) 0.0449(4) 0.2800(4) 0.0251(13) Uani 1 1 d . . . O20 O 0.9536(5) -0.1683(4) 0.3627(4) 0.0385(18) Uani 1 1 d . . . H20 H 0.9608 -0.1933 0.3293 0.046 Uiso 1 1 calc R . . O21 O 1.0093(6) -0.3398(6) 0.3538(6) 0.068(3) Uani 1 1 d DU . . O22 O 0.8665(5) -0.2733(5) 0.3315(5) 0.0434(19) Uani 1 1 d . . . O23 O 0.6511(4) -0.1477(4) 0.2949(4) 0.0305(15) Uani 1 1 d . . . O24 O 0.4234(4) -0.0297(5) 0.3507(5) 0.045(2) Uani 1 1 d . . . H24 H 0.4222 0.0124 0.3267 0.054 Uiso 1 1 calc R . . O25 O 0.7767(4) -0.0993(4) 0.3292(4) 0.0286(14) Uani 1 1 d . . . O26 O 0.6468(4) -0.0367(4) 0.3711(4) 0.0340(16) Uani 1 1 d . . . O27 O 0.7639(4) -0.0969(4) 0.1842(4) 0.0259(14) Uani 1 1 d . . . O28 O 0.8660(4) -0.0342(4) 0.1326(4) 0.0302(15) Uani 1 1 d . . . O29 O 0.7957(4) 0.0352(4) 0.3640(4) 0.0308(15) Uani 1 1 d . . . O30 O 0.7973(4) 0.1528(4) 0.3099(3) 0.0257(14) Uani 1 1 d . . . O31 O 0.9035(4) 0.0905(4) 0.1688(3) 0.0222(13) Uani 1 1 d . . . O32 O 0.8109(4) 0.1414(4) 0.1155(4) 0.0268(14) Uani 1 1 d . . . O33 O 0.6377(4) 0.1536(4) 0.1628(4) 0.0296(15) Uani 1 1 d . . . O34 O 0.6879(4) 0.0376(4) 0.1280(4) 0.0312(15) Uani 1 1 d . . . O35 O 0.6299(4) 0.1398(4) 0.3583(4) 0.0368(17) Uani 1 1 d . . . O36 O 0.5582(4) 0.0889(4) 0.3143(4) 0.0265(14) Uani 1 1 d . . . O37 O 0.7388(4) 0.0471(4) 0.2453(4) 0.0293(15) Uani 1 1 d . . . N1 N 0.9132(5) -0.2587(5) 0.1646(5) 0.0336(19) Uani 1 1 d . . . N2 N 0.9869(5) -0.2309(5) 0.1445(5) 0.0317(19) Uani 1 1 d . . . N3 N 1.0243(5) -0.0665(5) 0.1769(4) 0.0269(17) Uani 1 1 d . . . N4 N 0.9761(5) 0.2513(5) 0.1154(4) 0.0293(18) Uani 1 1 d . . . N5 N 0.9135(5) 0.2967(5) 0.0896(5) 0.0339(19) Uani 1 1 d . . . N6 N 0.7054(5) 0.2965(5) 0.1421(5) 0.034(2) Uani 1 1 d . . . N7 N 0.4713(5) 0.1506(5) 0.1259(5) 0.0295(18) Uani 1 1 d . . . N8 N 0.4853(5) 0.0762(5) 0.1100(5) 0.0308(18) Uani 1 1 d . . . N9 N 0.5914(5) -0.0882(5) 0.1748(5) 0.0288(18) Uani 1 1 d . . . N10 N 0.4189(5) 0.2523(5) 0.3372(5) 0.035(2) Uani 1 1 d . . . N11 N 0.4615(6) 0.3009(6) 0.3530(6) 0.048(3) Uani 1 1 d . . . N12 N 0.6692(6) 0.3006(6) 0.3003(6) 0.043(2) Uani 1 1 d . . . N13 N 0.9645(5) 0.1461(5) 0.3480(5) 0.0325(17) Uani 1 1 d DU . . N14 N 0.9838(5) 0.0698(5) 0.3740(4) 0.0283(17) Uani 1 1 d D . . N15 N 0.9470(5) -0.0914(5) 0.3377(4) 0.0267(17) Uani 1 1 d . . . N16 N 0.6950(5) -0.2604(5) 0.3790(5) 0.0331(19) Uani 1 1 d . . . N17 N 0.6107(5) -0.2325(5) 0.3954(5) 0.037(2) Uani 1 1 d . . . N18 N 0.5031(5) -0.0682(5) 0.3338(5) 0.0299(18) Uani 1 1 d . . . C1 C 0.5733(11) -0.3660(14) 0.1925(13) 0.113(9) Uani 1 1 d D . . H1A H 0.5608 -0.3394 0.1502 0.136 Uiso 1 1 calc R . . H1B H 0.5245 -0.3574 0.2349 0.136 Uiso 1 1 calc R . . H1C H 0.5900 -0.4198 0.1873 0.136 Uiso 1 1 calc R . . C2 C 0.7176(8) -0.3626(7) 0.1584(7) 0.043(3) Uani 1 1 d . . . C3 C 0.7430(10) -0.4193(8) 0.1158(9) 0.062(4) Uani 1 1 d . . . H3 H 0.7041 -0.4449 0.1130 0.074 Uiso 1 1 calc R . . C4 C 0.8249(11) -0.4400(8) 0.0767(9) 0.064(4) Uani 1 1 d . . . H4A H 0.8418 -0.4780 0.0455 0.076 Uiso 1 1 calc R . . C5 C 0.8811(9) -0.4056(7) 0.0832(7) 0.049(3) Uani 1 1 d . . . H5 H 0.9375 -0.4213 0.0574 0.058 Uiso 1 1 calc R . . C6 C 0.8580(7) -0.3478(6) 0.1269(6) 0.036(2) Uani 1 1 d . . . C7 C 0.7748(7) -0.3246(6) 0.1667(6) 0.037(2) Uani 1 1 d . . . C8 C 0.9222(7) -0.3121(6) 0.1259(6) 0.035(2) Uani 1 1 d . . . H8 H 0.9757 -0.3287 0.0944 0.042 Uiso 1 1 calc R . . C9 C 0.9768(6) -0.1739(5) 0.1789(5) 0.027(2) Uani 1 1 d . . . C10 C 1.0458(5) -0.1335(6) 0.1574(5) 0.029(2) Uani 1 1 d . . . C11 C 1.1310(6) -0.1681(8) 0.1163(7) 0.053(3) Uani 1 1 d . . . H11A H 1.1405 -0.1552 0.0651 0.063 Uiso 1 1 calc R . . H11B H 1.1386 -0.2226 0.1273 0.063 Uiso 1 1 calc R . . H11C H 1.1699 -0.1491 0.1296 0.063 Uiso 1 1 calc R . . C12 C 1.2832(7) -0.0084(8) 0.1590(10) 0.067(4) Uani 1 1 d D . . H12A H 1.3035 -0.0204 0.1095 0.080 Uiso 1 1 calc R . . H12B H 1.2727 -0.0540 0.1914 0.080 Uiso 1 1 calc R . . H12C H 1.3242 0.0120 0.1680 0.080 Uiso 1 1 calc R . . C13 C 1.2101(6) 0.1069(6) 0.1217(6) 0.033(2) Uani 1 1 d . . . C14 C 1.2803(6) 0.1294(6) 0.0707(6) 0.037(2) Uani 1 1 d . . . H14 H 1.3327 0.1004 0.0684 0.044 Uiso 1 1 calc R . . C15 C 1.2749(7) 0.1920(7) 0.0246(7) 0.047(3) Uani 1 1 d . . . H15 H 1.3231 0.2071 -0.0090 0.056 Uiso 1 1 calc R . . C16 C 1.1976(6) 0.2342(7) 0.0268(6) 0.035(2) Uani 1 1 d . . . H16A H 1.1942 0.2770 -0.0066 0.042 Uiso 1 1 calc R . . C17 C 1.1253(6) 0.2146(6) 0.0771(5) 0.029(2) Uani 1 1 d . . . C18 C 1.1297(5) 0.1498(6) 0.1274(5) 0.0261(19) Uani 1 1 d . . . C19 C 1.0484(6) 0.2578(6) 0.0722(6) 0.035(2) Uani 1 1 d . . . H19 H 1.0514 0.2951 0.0328 0.042 Uiso 1 1 calc R . . C20 C 0.8415(6) 0.2870(5) 0.1328(6) 0.029(2) Uani 1 1 d . . . C21 C 0.7729(7) 0.3237(6) 0.1051(7) 0.039(3) Uani 1 1 d . . . C22 C 0.7827(9) 0.3780(9) 0.0397(9) 0.071(5) Uani 1 1 d . . . H22A H 0.7719 0.3569 0.0035 0.085 Uiso 1 1 calc R . . H22B H 0.8387 0.3877 0.0210 0.085 Uiso 1 1 calc R . . H22C H 0.7439 0.4250 0.0517 0.085 Uiso 1 1 calc R . . C23 C 0.4640(18) 0.5074(7) 0.1442(16) 0.133(8) Uani 1 1 d DU . . H23A H 0.5193 0.5146 0.1138 0.159 Uiso 1 1 calc R . . H23B H 0.4506 0.5263 0.1903 0.159 Uiso 1 1 calc R . . H23C H 0.4245 0.5349 0.1209 0.159 Uiso 1 1 calc R . . C24 C 0.4470(8) 0.3971(7) 0.1039(9) 0.052(3) Uani 1 1 d . . . C25 C 0.4219(15) 0.4351(10) 0.0496(13) 0.100(7) Uani 1 1 d . . . H25 H 0.4158 0.4881 0.0421 0.120 Uiso 1 1 calc R . . C26 C 0.4047(18) 0.3967(11) 0.0041(14) 0.121(10) Uani 1 1 d . . . H26 H 0.3889 0.4241 -0.0348 0.145 Uiso 1 1 calc R . . C27 C 0.4103(14) 0.3217(9) 0.0148(10) 0.087(6) Uani 1 1 d . . . H27 H 0.3951 0.2966 -0.0142 0.104 Uiso 1 1 calc R . . C28 C 0.4393(9) 0.2804(7) 0.0703(8) 0.050(3) Uani 1 1 d . . . C29 C 0.4551(7) 0.3176(7) 0.1190(7) 0.039(2) Uani 1 1 d . . . C30 C 0.4526(7) 0.1987(7) 0.0761(6) 0.039(3) Uani 1 1 d . . . H30 H 0.4469 0.1780 0.0387 0.047 Uiso 1 1 calc R . . C31 C 0.5147(5) 0.0292(6) 0.1555(5) 0.027(2) Uani 1 1 d . . . C32 C 0.5432(6) -0.0517(6) 0.1404(5) 0.027(2) Uani 1 1 d . . . C33 C 0.5187(7) -0.0774(7) 0.0859(7) 0.042(3) Uani 1 1 d . . . H33A H 0.5677 -0.0932 0.0457 0.051 Uiso 1 1 calc R . . H33B H 0.4822 -0.0360 0.0689 0.051 Uiso 1 1 calc R . . H33C H 0.4903 -0.1195 0.1077 0.051 Uiso 1 1 calc R . . C34 C 0.2162(8) -0.0068(8) 0.3478(10) 0.066(4) Uani 1 1 d D . . H34A H 0.2045 -0.0228 0.3989 0.079 Uiso 1 1 calc R . . H34B H 0.2425 -0.0504 0.3207 0.079 Uiso 1 1 calc R . . H34C H 0.1650 0.0166 0.3388 0.079 Uiso 1 1 calc R . . C35 C 0.2447(5) 0.1079(5) 0.3622(5) 0.033(2) Uani 1 1 d D . . C36 C 0.1646(6) 0.1284(6) 0.4071(5) 0.047(3) Uani 1 1 d DU . . H36 H 0.1261 0.0973 0.4150 0.056 Uiso 1 1 calc R . . C37 C 0.1409(6) 0.1923(6) 0.4397(5) 0.053(2) Uani 1 1 d DU . . H37 H 0.0858 0.2072 0.4692 0.063 Uiso 1 1 calc R . . C38 C 0.2024(6) 0.2377(6) 0.4280(5) 0.042(2) Uani 1 1 d DU . . H38 H 0.1874 0.2817 0.4516 0.050 Uiso 1 1 calc R . . C39 C 0.2837(6) 0.2174(6) 0.3823(5) 0.038(2) Uani 1 1 d D . . C40 C 0.3053(5) 0.1509(5) 0.3487(5) 0.032(2) Uani 1 1 d D . . C41 C 0.3435(6) 0.2611(7) 0.3790(6) 0.037(3) Uani 1 1 d . . . H41 H 0.3255 0.2993 0.4103 0.044 Uiso 1 1 calc R . . C42 C 0.5395(7) 0.2884(6) 0.3143(7) 0.039(3) Uani 1 1 d . . . C43 C 0.5956(7) 0.3284(8) 0.3284(9) 0.059(4) Uani 1 1 d . . . C44 C 0.5598(9) 0.3903(12) 0.3766(14) 0.116(10) Uani 1 1 d . . . H44A H 0.5910 0.4309 0.3571 0.139 Uiso 1 1 calc R . . H44B H 0.5625 0.3709 0.4243 0.139 Uiso 1 1 calc R . . H44C H 0.5026 0.4095 0.3798 0.139 Uiso 1 1 calc R . . C45 C 0.8226(12) 0.5046(6) 0.2842(9) 0.075(5) Uani 1 1 d D . . H45A H 0.7767 0.5114 0.3290 0.090 Uiso 1 1 calc R . . H45B H 0.8027 0.5233 0.2438 0.090 Uiso 1 1 calc R . . H45C H 0.8639 0.5326 0.2820 0.090 Uiso 1 1 calc R . . C46 C 0.8831(7) 0.3939(8) 0.3335(8) 0.050(3) Uani 1 1 d . . . C47 C 0.8834(11) 0.4263(9) 0.3899(9) 0.074(5) Uani 1 1 d . . . H47 H 0.8682 0.4792 0.3905 0.089 Uiso 1 1 calc R . . C48 C 0.9069(12) 0.3806(10) 0.4487(9) 0.077(5) Uani 1 1 d . . . H48 H 0.9020 0.4025 0.4896 0.093 Uiso 1 1 calc R . . C49 C 0.9359(10) 0.3059(8) 0.4439(9) 0.072(5) Uani 1 1 d D . . H49 H 0.9564 0.2771 0.4797 0.087 Uiso 1 1 calc R . . C50 C 0.9367(7) 0.2699(6) 0.3880(6) 0.040(2) Uani 1 1 d DU . . C51 C 0.9095(7) 0.3129(6) 0.3320(6) 0.036(2) Uani 1 1 d U . . C52 C 0.9586(5) 0.1905(6) 0.3940(5) 0.0383(18) Uani 1 1 d DU . . H52 H 0.9702 0.1671 0.4360 0.046 Uiso 1 1 calc R . . C53 C 0.9735(6) 0.0255(6) 0.3361(5) 0.027(2) Uani 1 1 d . . . C54 C 0.9806(6) -0.0562(6) 0.3641(6) 0.032(2) Uani 1 1 d . . . C55 C 1.0201(8) -0.0880(8) 0.4195(8) 0.055(4) Uani 1 1 d . . . H55A H 1.0149 -0.1407 0.4336 0.066 Uiso 1 1 calc R . . H55B H 0.9930 -0.0597 0.4613 0.066 Uiso 1 1 calc R . . H55C H 1.0781 -0.0845 0.3999 0.066 Uiso 1 1 calc R . . C56 C 1.0358(13) -0.3622(13) 0.2830(8) 0.109(6) Uani 1 1 d DU . . H56A H 1.0689 -0.4128 0.2817 0.131 Uiso 1 1 calc R . . H56B H 1.0688 -0.3272 0.2492 0.131 Uiso 1 1 calc R . . H56C H 0.9879 -0.3617 0.2698 0.131 Uiso 1 1 calc R . . C57 C 0.9369(8) -0.3620(6) 0.3992(7) 0.047(3) Uani 1 1 d . . . C58 C 0.9355(9) -0.4156(7) 0.4570(8) 0.053(3) Uani 1 1 d . . . H58 H 0.9854 -0.4388 0.4651 0.063 Uiso 1 1 calc R . . C59 C 0.8645(9) -0.4358(7) 0.5023(7) 0.050(3) Uani 1 1 d . . . H59 H 0.8648 -0.4718 0.5421 0.059 Uiso 1 1 calc R . . C60 C 0.7918(8) -0.4035(6) 0.4900(7) 0.043(3) Uani 1 1 d . . . H60 H 0.7424 -0.4187 0.5210 0.051 Uiso 1 1 calc R . . C61 C 0.7898(7) -0.3484(6) 0.4322(6) 0.033(2) Uani 1 1 d . . . C62 C 0.8643(7) -0.3258(6) 0.3839(6) 0.038(2) Uani 1 1 d . . . C63 C 0.7112(7) -0.3120(6) 0.4277(6) 0.036(2) Uani 1 1 d . . . H63 H 0.6652 -0.3273 0.4647 0.043 Uiso 1 1 calc R . . C64 C 0.5953(6) -0.1743(6) 0.3502(5) 0.027(2) Uani 1 1 d . . . C65 C 0.5093(6) -0.1338(6) 0.3668(6) 0.034(2) Uani 1 1 d . . . C66 C 0.4398(7) -0.1678(9) 0.4175(7) 0.055(4) Uani 1 1 d . . . H66A H 0.3890 -0.1418 0.4088 0.065 Uiso 1 1 calc R . . H66B H 0.4349 -0.1632 0.4665 0.065 Uiso 1 1 calc R . . H66C H 0.4494 -0.2209 0.4107 0.065 Uiso 1 1 calc R . . C67 C 0.7103(6) -0.0762(6) 0.3828(6) 0.035(2) Uani 1 1 d . . . C68 C 0.7142(6) -0.0963(7) 0.4567(6) 0.038(2) Uani 1 1 d . . . H68A H 0.6795 -0.0565 0.4866 0.057 Uiso 1 1 calc R . . H68B H 0.7708 -0.1021 0.4551 0.057 Uiso 1 1 calc R . . H68C H 0.6947 -0.1435 0.4768 0.057 Uiso 1 1 calc R . . C69 C 0.8188(6) -0.0718(5) 0.1290(5) 0.0250(19) Uani 1 1 d . . . C70 C 0.8241(7) -0.0898(7) 0.0568(6) 0.039(3) Uani 1 1 d . . . H70A H 0.8455 -0.0504 0.0200 0.058 Uiso 1 1 calc R . . H70B H 0.7695 -0.0925 0.0578 0.058 Uiso 1 1 calc R . . H70C H 0.8608 -0.1380 0.0460 0.058 Uiso 1 1 calc R . . C71 C 0.7840(6) 0.1055(6) 0.3674(6) 0.032(2) Uani 1 1 d . . . C72 C 0.7548(7) 0.1367(7) 0.4374(6) 0.041(3) Uani 1 1 d . . . H72A H 0.7238 0.1027 0.4746 0.061 Uiso 1 1 calc R . . H72B H 0.7194 0.1858 0.4347 0.061 Uiso 1 1 calc R . . H72C H 0.8019 0.1421 0.4489 0.061 Uiso 1 1 calc R . . C73 C 0.8827(6) 0.1106(5) 0.1129(5) 0.0263(19) Uani 1 1 d . . . C74 C 0.9474(7) 0.0999(7) 0.0420(6) 0.037(2) Uani 1 1 d . . . H74A H 0.9401 0.0585 0.0219 0.055 Uiso 1 1 calc R . . H74B H 1.0014 0.0883 0.0476 0.055 Uiso 1 1 calc R . . H74C H 0.9431 0.1460 0.0098 0.055 Uiso 1 1 calc R . . C75 C 0.6699(5) 0.1064(5) 0.1147(5) 0.0223(18) Uani 1 1 d . . . C76 C 0.6852(7) 0.1407(7) 0.0371(6) 0.040(3) Uani 1 1 d . . . H76A H 0.7184 0.1024 0.0049 0.060 Uiso 1 1 calc R . . H76B H 0.7143 0.1823 0.0279 0.060 Uiso 1 1 calc R . . H76C H 0.6327 0.1593 0.0290 0.060 Uiso 1 1 calc R . . C77 C 0.5696(6) 0.1095(6) 0.3676(5) 0.031(2) Uani 1 1 d . . . C78 C 0.5077(7) 0.0977(8) 0.4405(6) 0.045(3) Uani 1 1 d . . . H78A H 0.5360 0.0794 0.4755 0.067 Uiso 1 1 calc R . . H78B H 0.4765 0.0607 0.4402 0.067 Uiso 1 1 calc R . . H78C H 0.4704 0.1452 0.4533 0.067 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 0.0218(2) 0.0248(2) 0.0340(3) -0.00525(19) -0.00770(18) -0.00432(17) Tb2 0.01360(19) 0.0247(2) 0.0219(2) -0.00293(17) -0.00436(16) -0.00425(16) Tb3 0.0174(2) 0.0275(2) 0.0253(2) -0.00199(17) -0.00922(17) -0.00607(16) Tb4 0.01333(19) 0.0262(2) 0.0244(2) -0.00794(17) -0.00364(16) -0.00375(16) Tb5 0.0174(2) 0.0258(2) 0.0309(2) -0.00765(18) -0.01118(18) -0.00263(17) Tb6 0.0166(2) 0.0302(2) 0.0367(3) -0.0154(2) -0.01068(18) 0.00033(17) O1 0.067(6) 0.056(6) 0.073(7) -0.015(5) -0.029(5) -0.023(5) O2 0.039(4) 0.042(4) 0.047(5) -0.019(4) -0.011(4) -0.010(4) O3 0.018(3) 0.021(3) 0.032(4) -0.005(3) -0.001(3) 0.000(2) O4 0.024(4) 0.050(5) 0.042(4) -0.001(4) -0.003(3) -0.018(3) O5 0.018(3) 0.039(4) 0.059(5) 0.000(4) -0.007(3) -0.001(3) O6 0.017(3) 0.037(4) 0.041(4) 0.002(3) -0.009(3) -0.007(3) O7 0.021(3) 0.032(4) 0.039(4) -0.003(3) -0.019(3) -0.006(3) O8A 0.043(5) 0.049(5) 0.109(8) 0.011(5) -0.058(6) -0.010(4) O9 0.092(8) 0.046(6) 0.177(13) -0.029(7) -0.092(9) -0.004(6) O10 0.066(6) 0.029(4) 0.063(6) -0.011(4) -0.042(5) 0.000(4) O11 0.023(3) 0.031(4) 0.032(4) -0.014(3) -0.013(3) -0.002(3) O12 0.037(4) 0.030(4) 0.053(5) -0.024(4) -0.013(4) -0.004(3) O13 0.027(4) 0.043(5) 0.076(6) -0.026(4) -0.011(4) -0.008(3) O14 0.018(3) 0.043(4) 0.055(5) -0.022(4) 0.001(3) -0.002(3) O15 0.022(3) 0.040(4) 0.043(4) -0.019(3) -0.016(3) 0.002(3) O16 0.034(4) 0.057(6) 0.104(8) -0.045(6) -0.029(5) -0.007(4) O17 0.048(5) 0.034(4) 0.059(5) -0.007(4) -0.023(4) -0.005(4) O18 0.064(5) 0.031(4) 0.035(4) -0.003(3) -0.027(4) -0.011(4) O19 0.023(3) 0.023(3) 0.030(3) 0.004(3) -0.011(3) -0.006(3) O20 0.043(4) 0.027(4) 0.052(5) 0.002(3) -0.027(4) -0.006(3) O21 0.048(5) 0.076(7) 0.075(6) 0.010(6) -0.024(5) -0.010(5) O22 0.031(4) 0.041(4) 0.053(5) 0.011(4) -0.017(4) -0.005(3) O23 0.021(3) 0.026(3) 0.037(4) 0.003(3) -0.004(3) -0.005(3) O24 0.012(3) 0.051(5) 0.065(6) -0.014(4) -0.006(3) 0.001(3) O25 0.020(3) 0.030(4) 0.033(4) -0.009(3) -0.001(3) -0.007(3) O26 0.027(3) 0.041(4) 0.037(4) -0.006(3) -0.009(3) -0.012(3) O27 0.019(3) 0.022(3) 0.030(4) 0.002(3) -0.005(3) 0.000(2) O28 0.018(3) 0.037(4) 0.033(4) -0.005(3) -0.005(3) -0.004(3) O29 0.022(3) 0.036(4) 0.032(4) 0.000(3) -0.007(3) -0.006(3) O30 0.019(3) 0.035(4) 0.028(3) -0.002(3) -0.010(3) -0.010(3) O31 0.020(3) 0.027(3) 0.022(3) 0.000(3) -0.011(2) -0.004(2) O32 0.025(3) 0.029(3) 0.030(4) 0.001(3) -0.014(3) -0.007(3) O33 0.018(3) 0.034(4) 0.039(4) -0.018(3) -0.006(3) -0.005(3) O34 0.020(3) 0.034(4) 0.039(4) -0.009(3) -0.006(3) -0.009(3) O35 0.028(4) 0.044(4) 0.043(4) -0.021(4) -0.011(3) -0.006(3) O36 0.024(3) 0.032(4) 0.030(4) -0.018(3) -0.012(3) -0.001(3) O37 0.015(3) 0.027(3) 0.048(4) -0.008(3) -0.015(3) 0.000(3) N1 0.028(4) 0.036(5) 0.036(5) -0.005(4) -0.013(4) 0.000(4) N2 0.023(4) 0.039(5) 0.029(4) -0.012(4) -0.002(3) -0.004(4) N3 0.021(4) 0.032(4) 0.025(4) -0.003(3) -0.006(3) -0.004(3) N4 0.038(5) 0.029(4) 0.027(4) 0.003(3) -0.016(4) -0.013(4) N5 0.034(5) 0.033(5) 0.040(5) 0.005(4) -0.021(4) -0.009(4) N6 0.026(4) 0.027(4) 0.057(6) -0.001(4) -0.027(4) 0.002(3) N7 0.021(4) 0.036(5) 0.036(5) -0.008(4) -0.013(3) -0.007(3) N8 0.025(4) 0.032(4) 0.036(5) -0.012(4) -0.010(4) -0.001(3) N9 0.021(4) 0.026(4) 0.040(5) -0.008(4) -0.010(3) -0.003(3) N10 0.020(4) 0.039(5) 0.050(5) -0.024(4) -0.013(4) 0.004(3) N11 0.029(5) 0.052(6) 0.069(7) -0.045(6) -0.012(5) 0.004(4) N12 0.030(5) 0.041(5) 0.071(7) -0.025(5) -0.027(5) -0.003(4) N13 0.035(4) 0.032(4) 0.035(4) -0.008(3) -0.017(3) -0.001(3) N14 0.023(4) 0.032(4) 0.033(4) -0.003(4) -0.013(3) -0.004(3) N15 0.020(4) 0.028(4) 0.032(4) -0.003(3) -0.011(3) -0.002(3) N16 0.031(4) 0.039(5) 0.033(5) 0.001(4) -0.014(4) -0.011(4) N17 0.030(4) 0.036(5) 0.043(5) 0.000(4) -0.009(4) -0.009(4) N18 0.013(3) 0.040(5) 0.036(5) -0.013(4) -0.005(3) -0.004(3) C1 0.110(17) 0.14(2) 0.128(19) -0.063(17) -0.078(16) -0.002(15) C2 0.054(7) 0.036(6) 0.050(7) -0.005(5) -0.029(6) -0.008(5) C3 0.075(10) 0.049(8) 0.073(10) -0.015(7) -0.031(8) -0.017(7) C4 0.089(11) 0.046(8) 0.074(10) -0.025(7) -0.040(9) -0.012(8) C5 0.073(9) 0.041(7) 0.039(6) -0.013(5) -0.022(6) -0.013(6) C6 0.040(6) 0.027(5) 0.046(6) -0.004(4) -0.025(5) 0.001(4) C7 0.055(7) 0.026(5) 0.042(6) -0.011(4) -0.030(5) -0.004(5) C8 0.034(5) 0.027(5) 0.044(6) -0.010(4) -0.015(5) 0.003(4) C9 0.019(4) 0.027(5) 0.033(5) -0.002(4) -0.006(4) -0.004(4) C10 0.016(4) 0.046(6) 0.021(5) -0.009(4) 0.002(3) -0.004(4) C11 0.016(5) 0.068(9) 0.058(8) -0.027(7) 0.012(5) -0.001(5) C12 0.033(6) 0.050(8) 0.098(12) 0.006(8) -0.019(7) 0.015(6) C13 0.018(4) 0.043(6) 0.037(6) -0.012(5) -0.001(4) -0.008(4) C14 0.022(5) 0.041(6) 0.045(6) -0.009(5) -0.005(4) -0.007(4) C15 0.033(6) 0.053(7) 0.045(7) -0.008(6) 0.006(5) -0.020(5) C16 0.027(5) 0.052(7) 0.026(5) -0.001(5) -0.002(4) -0.019(5) C17 0.030(5) 0.041(6) 0.019(4) -0.006(4) -0.004(4) -0.014(4) C18 0.018(4) 0.036(5) 0.024(5) -0.003(4) -0.004(4) -0.010(4) C19 0.032(5) 0.044(6) 0.040(6) 0.003(5) -0.022(5) -0.019(5) C20 0.033(5) 0.020(4) 0.039(6) 0.000(4) -0.020(4) -0.005(4) C21 0.045(6) 0.028(5) 0.057(7) 0.010(5) -0.035(6) -0.012(5) C22 0.053(8) 0.073(10) 0.105(12) 0.049(9) -0.059(9) -0.036(8) C23 0.153(17) 0.097(15) 0.183(19) -0.024(15) -0.089(16) -0.031(14) C24 0.055(7) 0.027(6) 0.094(11) -0.002(6) -0.049(8) -0.007(5) C25 0.15(2) 0.042(9) 0.139(19) 0.007(10) -0.083(17) -0.031(11) C26 0.20(3) 0.051(11) 0.16(2) 0.036(12) -0.11(2) -0.061(15) C27 0.155(19) 0.058(10) 0.092(13) 0.017(9) -0.098(14) -0.031(11) C28 0.062(8) 0.045(7) 0.065(8) 0.000(6) -0.044(7) -0.019(6) C29 0.030(5) 0.038(6) 0.052(7) -0.008(5) -0.020(5) -0.003(5) C30 0.036(6) 0.044(6) 0.049(7) -0.004(5) -0.027(5) -0.011(5) C31 0.014(4) 0.039(5) 0.032(5) -0.019(4) -0.003(4) -0.006(4) C32 0.020(4) 0.041(6) 0.023(5) -0.012(4) -0.005(4) -0.009(4) C33 0.039(6) 0.045(6) 0.059(7) -0.022(6) -0.029(6) -0.005(5) C34 0.047(8) 0.055(9) 0.097(12) -0.011(8) -0.012(8) -0.028(7) C35 0.020(4) 0.038(6) 0.045(6) -0.011(5) -0.014(4) -0.001(4) C36 0.024(4) 0.044(5) 0.052(5) -0.007(4) 0.009(4) -0.001(4) C37 0.027(3) 0.038(4) 0.053(4) 0.005(4) 0.022(3) 0.005(3) C38 0.022(4) 0.042(5) 0.047(5) -0.009(4) 0.004(4) 0.000(4) C39 0.025(5) 0.050(7) 0.035(6) -0.014(5) -0.002(4) -0.007(5) C40 0.011(4) 0.044(6) 0.038(6) -0.011(5) -0.006(4) 0.000(4) C41 0.021(4) 0.058(7) 0.037(6) -0.031(5) -0.012(4) 0.004(4) C42 0.034(5) 0.034(6) 0.056(7) -0.030(5) -0.021(5) 0.009(4) C43 0.037(6) 0.052(8) 0.111(12) -0.061(8) -0.035(7) 0.006(5) C44 0.035(7) 0.132(17) 0.21(2) -0.142(18) -0.032(11) 0.007(9) C45 0.120(15) 0.038(7) 0.073(11) 0.010(7) -0.055(11) 0.000(8) C46 0.033(6) 0.052(7) 0.078(9) -0.025(7) -0.029(6) -0.001(5) C47 0.105(13) 0.047(8) 0.090(12) -0.038(8) -0.064(11) 0.025(8) C48 0.101(13) 0.072(11) 0.070(10) -0.033(9) -0.051(10) 0.019(10) C49 0.116(14) 0.040(7) 0.095(12) -0.021(8) -0.081(11) 0.005(8) C50 0.048(5) 0.037(5) 0.043(4) -0.016(4) -0.030(4) 0.009(4) C51 0.043(5) 0.033(5) 0.043(5) -0.010(4) -0.027(4) -0.005(4) C52 0.048(4) 0.037(4) 0.038(4) -0.014(3) -0.030(3) 0.009(3) C53 0.021(4) 0.031(5) 0.030(5) 0.005(4) -0.016(4) -0.004(4) C54 0.017(4) 0.024(5) 0.045(6) 0.004(4) -0.004(4) -0.003(4) C55 0.055(8) 0.061(8) 0.071(9) 0.009(7) -0.047(7) -0.022(7) C56 0.075(9) 0.108(10) 0.109(10) 0.017(9) -0.009(8) -0.004(8) C57 0.055(7) 0.025(5) 0.057(8) -0.001(5) -0.025(6) 0.006(5) C58 0.062(8) 0.040(7) 0.066(9) -0.014(6) -0.040(7) 0.006(6) C59 0.078(9) 0.030(6) 0.047(7) -0.006(5) -0.035(7) 0.003(6) C60 0.057(7) 0.020(5) 0.048(7) -0.004(5) -0.017(6) -0.001(5) C61 0.047(6) 0.026(5) 0.031(5) -0.008(4) -0.023(5) 0.001(4) C62 0.038(6) 0.036(6) 0.040(6) -0.009(5) -0.010(5) -0.006(5) C63 0.040(6) 0.028(5) 0.039(6) 0.000(4) -0.012(5) -0.012(4) C64 0.023(4) 0.032(5) 0.028(5) -0.005(4) -0.006(4) -0.014(4) C65 0.029(5) 0.039(6) 0.033(5) -0.001(4) -0.008(4) -0.010(4) C66 0.019(5) 0.079(10) 0.053(8) 0.007(7) 0.002(5) -0.018(6) C67 0.020(5) 0.037(6) 0.045(6) -0.007(5) -0.005(4) -0.011(4) C68 0.027(5) 0.050(7) 0.032(6) 0.001(5) -0.004(4) -0.009(5) C69 0.023(4) 0.025(5) 0.027(5) -0.005(4) -0.009(4) -0.002(4) C70 0.039(6) 0.043(6) 0.037(6) -0.017(5) -0.007(5) -0.012(5) C71 0.016(4) 0.043(6) 0.035(5) -0.003(5) -0.005(4) -0.009(4) C72 0.028(5) 0.058(7) 0.036(6) -0.021(5) -0.001(4) -0.011(5) C73 0.027(5) 0.025(5) 0.029(5) -0.002(4) -0.009(4) -0.009(4) C74 0.038(6) 0.041(6) 0.031(5) 0.000(5) -0.014(5) -0.005(5) C75 0.018(4) 0.028(5) 0.022(4) -0.004(4) -0.008(3) -0.005(4) C76 0.037(6) 0.045(6) 0.036(6) 0.002(5) -0.007(5) -0.019(5) C77 0.019(4) 0.045(6) 0.025(5) -0.008(4) 0.000(4) -0.005(4) C78 0.037(6) 0.059(8) 0.039(6) -0.018(6) -0.003(5) -0.016(6) _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 O22 2.230(8) . ? Tb1 O2 2.244(7) . ? Tb1 O3 2.373(6) . ? Tb1 O23 2.389(7) . ? Tb1 O25 2.427(7) . ? Tb1 O27 2.438(6) . ? Tb1 N1 2.519(9) . ? Tb1 N16 2.530(9) . ? Tb1 Tb2 3.9077(6) . ? Tb1 Tb4 3.9080(7) . ? Tb2 O19 2.360(6) . ? Tb2 O3 2.360(6) . ? Tb2 O37 2.418(6) . ? Tb2 O25 2.426(7) . ? Tb2 O31 2.431(6) . ? Tb2 O29 2.464(7) . ? Tb2 O28 2.471(7) . ? Tb2 N15 2.598(8) . ? Tb2 N3 2.615(8) . ? Tb2 Tb3 3.9113(7) . ? Tb3 O6 2.238(7) . ? Tb3 O18 2.248(7) . ? Tb3 O19 2.385(6) . ? Tb3 O7 2.405(6) . ? Tb3 O31 2.431(6) . ? Tb3 O30 2.439(6) . ? Tb3 N4 2.510(8) . ? Tb3 N13 2.515(8) . ? Tb3 Tb5 3.9156(6) . ? Tb4 O23 2.357(7) . ? Tb4 O11 2.375(6) . ? Tb4 O37 2.398(6) . ? Tb4 O36 2.433(6) . ? Tb4 O27 2.438(6) . ? Tb4 O34 2.453(7) . ? Tb4 O26 2.461(7) . ? Tb4 N9 2.580(8) . ? Tb4 N18 2.617(8) . ? Tb4 Tb6 3.9066(7) . ? Tb5 O7 2.365(6) . ? Tb5 O15 2.366(7) . ? Tb5 O37 2.399(7) . ? Tb5 O33 2.450(6) . ? Tb5 O30 2.452(6) . ? Tb5 O35 2.505(8) . ? Tb5 O32 2.512(7) . ? Tb5 N6 2.565(9) . ? Tb5 N12 2.600(9) . ? Tb5 Tb6 3.9188(6) . ? Tb6 O14 2.235(7) . ? Tb6 O10 2.240(8) . ? Tb6 O15 2.375(7) . ? Tb6 O11 2.381(7) . ? Tb6 O36 2.424(7) . ? Tb6 O33 2.444(6) . ? Tb6 N10 2.492(8) . ? Tb6 N7 2.519(8) . ? O1 C2 1.376(16) . ? O1 C1 1.422(9) . ? O2 C7 1.317(12) . ? O3 C9 1.316(11) . ? O4 N3 1.375(10) . ? O4 H4 0.8400 . ? O5 C13 1.363(14) . ? O5 C12 1.434(8) . ? O6 C18 1.301(11) . ? O7 C20 1.297(12) . ? O8A N6 1.396(10) . ? O8A H8A 0.8400 . ? O9 C24 1.402(17) . ? O9 C23 1.424(5) . ? O10 C29 1.262(14) . ? O11 C31 1.319(11) . ? O12 N9 1.394(11) . ? O12 H12 0.8400 . ? O13 C35 1.359(12) . ? O13 C34 1.433(8) . ? O14 C40 1.333(11) . ? O15 C42 1.317(12) . ? O16 N12 1.399(11) . ? O16 H16 0.8400 . ? O17 C46 1.300(16) . ? O17 C45 1.428(9) . ? O18 C51 1.311(12) . ? O19 C53 1.296(11) . ? O20 N15 1.412(11) . ? O20 H20 0.8400 . ? O21 C57 1.392(16) . ? O21 C56 1.437(10) . ? O22 C62 1.297(14) . ? O23 C64 1.309(11) . ? O24 N18 1.379(10) . ? O24 H24 0.8400 . ? O25 C67 1.325(12) . ? O26 C67 1.269(13) . ? O27 C69 1.288(11) . ? O28 C69 1.240(12) . ? O29 C71 1.274(13) . ? O30 C71 1.306(13) . ? O31 C73 1.280(11) . ? O32 C73 1.259(12) . ? O33 C75 1.301(11) . ? O34 C75 1.240(12) . ? O35 C77 1.267(12) . ? O36 C77 1.298(12) . ? N1 C8 1.310(14) . ? N1 N2 1.420(12) . ? N2 C9 1.305(13) . ? N3 C10 1.293(13) . ? N4 C19 1.289(13) . ? N4 N5 1.431(12) . ? N5 C20 1.298(13) . ? N6 C21 1.326(14) . ? N7 C30 1.304(14) . ? N7 N8 1.411(12) . ? N8 C31 1.313(14) . ? N9 C32 1.291(13) . ? N10 C41 1.293(13) . ? N10 N11 1.443(12) . ? N11 C42 1.314(14) . ? N12 C43 1.248(15) . ? N13 C52 1.305(11) . ? N13 N14 1.421(12) . ? N14 C53 1.298(13) . ? N15 C54 1.268(13) . ? N16 C63 1.305(14) . ? N16 N17 1.404(12) . ? N17 C64 1.325(14) . ? N18 C65 1.275(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.362(18) . ? C2 C7 1.436(16) . ? C3 C4 1.38(2) . ? C3 H3 0.9500 . ? C4 C5 1.361(19) . ? C4 H4A 0.9500 . ? C5 C6 1.396(15) . ? C5 H5 0.9500 . ? C6 C7 1.411(16) . ? C6 C8 1.444(15) . ? C8 H8 0.9500 . ? C9 C10 1.480(13) . ? C10 C11 1.491(13) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.402(14) . ? C13 C18 1.441(13) . ? C14 C15 1.357(18) . ? C14 H14 0.9500 . ? C15 C16 1.402(17) . ? C15 H15 0.9500 . ? C16 C17 1.403(13) . ? C16 H16A 0.9500 . ? C17 C18 1.433(14) . ? C17 C19 1.442(15) . ? C19 H19 0.9500 . ? C20 C21 1.497(13) . ? C21 C22 1.492(17) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.35(2) . ? C24 C29 1.429(16) . ? C25 C26 1.41(3) . ? C25 H25 0.9500 . ? C26 C27 1.35(2) . ? C26 H26 0.9500 . ? C27 C28 1.427(18) . ? C27 H27 0.9500 . ? C28 C29 1.431(16) . ? C28 C30 1.460(17) . ? C30 H30 0.9500 . ? C31 C32 1.509(14) . ? C32 C33 1.501(13) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.392(11) . ? C35 C40 1.409(11) . ? C36 C37 1.357(13) . ? C36 H36 0.9500 . ? C37 C38 1.463(13) . ? C37 H37 0.9500 . ? C38 C39 1.412(11) . ? C38 H38 0.9500 . ? C39 C40 1.414(12) . ? C39 C41 1.460(14) . ? C41 H41 0.9500 . ? C42 C43 1.502(14) . ? C43 C44 1.503(17) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.379(18) . ? C46 C51 1.460(17) . ? C47 C48 1.46(2) . ? C47 H47 0.9500 . ? C48 C49 1.36(2) . ? C48 H48 0.9500 . ? C49 C50 1.402(16) . ? C49 H49 0.9500 . ? C50 C52 1.421(12) . ? C50 C51 1.429(15) . ? C52 H52 0.9500 . ? C53 C54 1.506(13) . ? C54 C55 1.494(16) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.387(18) . ? C57 C62 1.424(17) . ? C58 C59 1.36(2) . ? C58 H58 0.9500 . ? C59 C60 1.383(18) . ? C59 H59 0.9500 . ? C60 C61 1.411(15) . ? C60 H60 0.9500 . ? C61 C63 1.432(15) . ? C61 C62 1.441(16) . ? C63 H63 0.9500 . ? C64 C65 1.484(14) . ? C65 C66 1.484(14) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.496(16) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.517(14) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.489(15) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.490(14) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.534(14) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.504(14) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 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 O22 Tb1 O2 115.2(3) . . ? O22 Tb1 O3 77.3(3) . . ? O2 Tb1 O3 132.1(3) . . ? O22 Tb1 O23 132.9(3) . . ? O2 Tb1 O23 78.1(3) . . ? O3 Tb1 O23 128.8(2) . . ? O22 Tb1 O25 87.9(3) . . ? O2 Tb1 O25 152.4(3) . . ? O3 Tb1 O25 65.0(2) . . ? O23 Tb1 O25 75.0(2) . . ? O22 Tb1 O27 151.9(3) . . ? O2 Tb1 O27 87.2(3) . . ? O3 Tb1 O27 74.9(2) . . ? O23 Tb1 O27 65.5(2) . . ? O25 Tb1 O27 76.5(2) . . ? O22 Tb1 N1 82.7(3) . . ? O2 Tb1 N1 72.1(3) . . ? O3 Tb1 N1 63.6(3) . . ? O23 Tb1 N1 141.5(3) . . ? O25 Tb1 N1 128.6(3) . . ? O27 Tb1 N1 89.0(3) . . ? O22 Tb1 N16 72.3(3) . . ? O2 Tb1 N16 85.1(3) . . ? O3 Tb1 N16 140.0(3) . . ? O23 Tb1 N16 63.8(3) . . ? O25 Tb1 N16 88.2(3) . . ? O27 Tb1 N16 129.3(2) . . ? N1 Tb1 N16 134.8(3) . . ? O22 Tb1 Tb2 95.4(2) . . ? O2 Tb1 Tb2 143.7(2) . . ? O3 Tb1 Tb2 34.26(15) . . ? O23 Tb1 Tb2 95.50(17) . . ? O25 Tb1 Tb2 36.37(15) . . ? O27 Tb1 Tb2 58.37(16) . . ? N1 Tb1 Tb2 94.4(2) . . ? N16 Tb1 Tb2 124.3(2) . . ? O22 Tb1 Tb4 144.6(2) . . ? O2 Tb1 Tb4 95.5(2) . . ? O3 Tb1 Tb4 95.56(15) . . ? O23 Tb1 Tb4 34.31(16) . . ? O25 Tb1 Tb4 58.39(17) . . ? O27 Tb1 Tb4 36.73(15) . . ? N1 Tb1 Tb4 125.6(2) . . ? N16 Tb1 Tb4 94.4(2) . . ? Tb2 Tb1 Tb4 64.576(12) . . ? O19 Tb2 O3 124.5(2) . . ? O19 Tb2 O37 117.7(2) . . ? O3 Tb2 O37 117.8(2) . . ? O19 Tb2 O25 128.2(2) . . ? O3 Tb2 O25 65.2(2) . . ? O37 Tb2 O25 76.4(2) . . ? O19 Tb2 O31 66.3(2) . . ? O3 Tb2 O31 129.4(2) . . ? O37 Tb2 O31 76.7(2) . . ? O25 Tb2 O31 153.1(2) . . ? O19 Tb2 O29 68.4(2) . . ? O3 Tb2 O29 129.2(2) . . ? O37 Tb2 O29 72.3(2) . . ? O25 Tb2 O29 70.5(2) . . ? O31 Tb2 O29 101.2(2) . . ? O19 Tb2 O28 130.1(2) . . ? O3 Tb2 O28 69.4(2) . . ? O37 Tb2 O28 73.0(2) . . ? O25 Tb2 O28 101.5(2) . . ? O31 Tb2 O28 70.2(2) . . ? O29 Tb2 O28 145.3(2) . . ? O19 Tb2 N15 62.7(2) . . ? O3 Tb2 N15 72.5(2) . . ? O37 Tb2 N15 143.1(3) . . ? O25 Tb2 N15 77.3(2) . . ? O31 Tb2 N15 126.4(2) . . ? O29 Tb2 N15 74.7(2) . . ? O28 Tb2 N15 138.1(2) . . ? O19 Tb2 N3 71.8(2) . . ? O3 Tb2 N3 63.6(2) . . ? O37 Tb2 N3 145.8(3) . . ? O25 Tb2 N3 125.6(2) . . ? O31 Tb2 N3 78.5(2) . . ? O29 Tb2 N3 136.1(2) . . ? O28 Tb2 N3 76.7(2) . . ? N15 Tb2 N3 71.1(2) . . ? O19 Tb2 Tb1 149.17(15) . . ? O3 Tb2 Tb1 34.47(15) . . ? O37 Tb2 Tb1 87.46(16) . . ? O25 Tb2 Tb1 36.37(16) . . ? O31 Tb2 Tb1 141.66(14) . . ? O29 Tb2 Tb1 106.86(16) . . ? O28 Tb2 Tb1 71.78(17) . . ? N15 Tb2 Tb1 86.56(18) . . ? N3 Tb2 Tb1 97.87(19) . . ? O19 Tb2 Tb3 34.68(15) . . ? O3 Tb2 Tb3 149.26(15) . . ? O37 Tb2 Tb3 88.14(16) . . ? O25 Tb2 Tb3 142.17(16) . . ? O31 Tb2 Tb3 36.43(14) . . ? O29 Tb2 Tb3 71.95(16) . . ? O28 Tb2 Tb3 106.66(17) . . ? N15 Tb2 Tb3 97.10(18) . . ? N3 Tb2 Tb3 85.66(19) . . ? Tb1 Tb2 Tb3 175.602(14) . . ? O6 Tb3 O18 113.6(3) . . ? O6 Tb3 O19 76.4(2) . . ? O18 Tb3 O19 134.9(2) . . ? O6 Tb3 O7 133.0(3) . . ? O18 Tb3 O7 78.8(3) . . ? O19 Tb3 O7 128.1(2) . . ? O6 Tb3 O31 86.2(2) . . ? O18 Tb3 O31 152.6(3) . . ? O19 Tb3 O31 66.0(2) . . ? O7 Tb3 O31 73.9(2) . . ? O6 Tb3 O30 150.5(2) . . ? O18 Tb3 O30 90.9(3) . . ? O19 Tb3 O30 74.6(2) . . ? O7 Tb3 O30 65.4(2) . . ? O31 Tb3 O30 77.4(2) . . ? O6 Tb3 N4 72.3(3) . . ? O18 Tb3 N4 82.9(3) . . ? O19 Tb3 N4 138.9(3) . . ? O7 Tb3 N4 64.4(3) . . ? O31 Tb3 N4 85.8(2) . . ? O30 Tb3 N4 129.7(2) . . ? O6 Tb3 N13 88.3(3) . . ? O18 Tb3 N13 72.1(3) . . ? O19 Tb3 N13 64.1(3) . . ? O7 Tb3 N13 136.9(3) . . ? O31 Tb3 N13 129.7(2) . . ? O30 Tb3 N13 83.8(2) . . ? N4 Tb3 N13 138.8(3) . . ? O6 Tb3 Tb2 92.79(19) . . ? O18 Tb3 Tb2 149.2(2) . . ? O19 Tb3 Tb2 34.27(15) . . ? O7 Tb3 Tb2 95.07(16) . . ? O31 Tb3 Tb2 36.44(15) . . ? O30 Tb3 Tb2 59.67(16) . . ? N4 Tb3 Tb2 121.94(19) . . ? N13 Tb3 Tb2 94.2(2) . . ? O6 Tb3 Tb5 142.71(19) . . ? O18 Tb3 Tb5 98.5(2) . . ? O19 Tb3 Tb5 94.51(15) . . ? O7 Tb3 Tb5 34.50(16) . . ? O31 Tb3 Tb5 57.62(14) . . ? O30 Tb3 Tb5 36.94(15) . . ? N4 Tb3 Tb5 94.60(19) . . ? N13 Tb3 Tb5 120.6(2) . . ? Tb2 Tb3 Tb5 64.175(12) . . ? O23 Tb4 O11 124.0(2) . . ? O23 Tb4 O37 118.2(2) . . ? O11 Tb4 O37 117.9(2) . . ? O23 Tb4 O36 129.0(2) . . ? O11 Tb4 O36 66.2(2) . . ? O37 Tb4 O36 76.2(2) . . ? O23 Tb4 O27 66.0(2) . . ? O11 Tb4 O27 128.4(2) . . ? O37 Tb4 O27 76.7(2) . . ? O36 Tb4 O27 152.9(2) . . ? O23 Tb4 O34 129.2(2) . . ? O11 Tb4 O34 69.1(2) . . ? O37 Tb4 O34 72.6(2) . . ? O36 Tb4 O34 101.7(2) . . ? O27 Tb4 O34 69.7(2) . . ? O23 Tb4 O26 69.4(3) . . ? O11 Tb4 O26 129.3(2) . . ? O37 Tb4 O26 72.9(2) . . ? O36 Tb4 O26 69.8(2) . . ? O27 Tb4 O26 102.2(2) . . ? O34 Tb4 O26 145.5(2) . . ? O23 Tb4 N9 72.7(3) . . ? O11 Tb4 N9 63.0(2) . . ? O37 Tb4 N9 142.8(3) . . ? O36 Tb4 N9 127.0(2) . . ? O27 Tb4 N9 76.7(2) . . ? O34 Tb4 N9 74.0(3) . . ? O26 Tb4 N9 138.4(3) . . ? O23 Tb4 N18 63.1(3) . . ? O11 Tb4 N18 71.9(3) . . ? O37 Tb4 N18 144.8(3) . . ? O36 Tb4 N18 78.3(3) . . ? O27 Tb4 N18 126.0(2) . . ? O34 Tb4 N18 136.9(2) . . ? O26 Tb4 N18 75.7(2) . . ? N9 Tb4 N18 72.4(3) . . ? O23 Tb4 Tb6 148.87(16) . . ? O11 Tb4 Tb6 34.81(15) . . ? O37 Tb4 Tb6 87.82(16) . . ? O36 Tb4 Tb6 36.38(16) . . ? O27 Tb4 Tb6 141.91(15) . . ? O34 Tb4 Tb6 72.47(16) . . ? O26 Tb4 Tb6 106.11(18) . . ? N9 Tb4 Tb6 97.50(18) . . ? N18 Tb4 Tb6 85.8(2) . . ? O23 Tb4 Tb1 34.83(16) . . ? O11 Tb4 Tb1 149.19(15) . . ? O37 Tb4 Tb1 87.73(16) . . ? O36 Tb4 Tb1 141.56(16) . . ? O27 Tb4 Tb1 36.72(15) . . ? O34 Tb4 Tb1 106.46(16) . . ? O26 Tb4 Tb1 72.20(18) . . ? N9 Tb4 Tb1 86.26(18) . . ? N18 Tb4 Tb1 97.6(2) . . ? Tb6 Tb4 Tb1 175.537(15) . . ? O7 Tb5 O15 124.2(2) . . ? O7 Tb5 O37 118.8(2) . . ? O15 Tb5 O37 117.0(2) . . ? O7 Tb5 O33 127.5(2) . . ? O15 Tb5 O33 65.5(2) . . ? O37 Tb5 O33 77.6(2) . . ? O7 Tb5 O30 65.8(2) . . ? O15 Tb5 O30 126.9(2) . . ? O37 Tb5 O30 78.6(2) . . ? O33 Tb5 O30 156.2(2) . . ? O7 Tb5 O35 129.5(2) . . ? O15 Tb5 O35 68.0(3) . . ? O37 Tb5 O35 73.0(2) . . ? O33 Tb5 O35 102.6(2) . . ? O30 Tb5 O35 69.9(2) . . ? O7 Tb5 O32 69.0(2) . . ? O15 Tb5 O32 129.9(2) . . ? O37 Tb5 O32 73.1(2) . . ? O33 Tb5 O32 70.1(2) . . ? O30 Tb5 O32 103.0(2) . . ? O35 Tb5 O32 146.2(2) . . ? O7 Tb5 N6 63.1(2) . . ? O15 Tb5 N6 73.4(3) . . ? O37 Tb5 N6 142.6(3) . . ? O33 Tb5 N6 75.1(3) . . ? O30 Tb5 N6 126.0(2) . . ? O35 Tb5 N6 137.9(3) . . ? O32 Tb5 N6 73.8(3) . . ? O7 Tb5 N12 71.8(3) . . ? O15 Tb5 N12 62.6(3) . . ? O37 Tb5 N12 145.4(3) . . ? O33 Tb5 N12 124.2(3) . . ? O30 Tb5 N12 77.0(3) . . ? O35 Tb5 N12 75.8(3) . . ? O32 Tb5 N12 136.4(3) . . ? N6 Tb5 N12 72.0(3) . . ? O7 Tb5 Tb3 35.16(16) . . ? O15 Tb5 Tb3 149.08(17) . . ? O37 Tb5 Tb3 88.31(14) . . ? O33 Tb5 Tb3 142.09(15) . . ? O30 Tb5 Tb3 36.71(15) . . ? O35 Tb5 Tb3 106.64(17) . . ? O32 Tb5 Tb3 72.18(14) . . ? N6 Tb5 Tb3 97.84(18) . . ? N12 Tb5 Tb3 86.51(19) . . ? O7 Tb5 Tb6 148.59(16) . . ? O15 Tb5 Tb6 34.32(17) . . ? O37 Tb5 Tb6 87.52(14) . . ? O33 Tb5 Tb6 36.73(15) . . ? O30 Tb5 Tb6 141.64(15) . . ? O35 Tb5 Tb6 71.83(16) . . ? O32 Tb5 Tb6 106.81(14) . . ? N6 Tb5 Tb6 85.67(18) . . ? N12 Tb5 Tb6 96.78(19) . . ? Tb3 Tb5 Tb6 175.820(16) . . ? O14 Tb6 O10 116.7(3) . . ? O14 Tb6 O15 132.5(3) . . ? O10 Tb6 O15 76.9(3) . . ? O14 Tb6 O11 76.8(3) . . ? O10 Tb6 O11 133.9(3) . . ? O15 Tb6 O11 128.3(2) . . ? O14 Tb6 O36 86.7(3) . . ? O10 Tb6 O36 150.2(3) . . ? O15 Tb6 O36 73.5(2) . . ? O11 Tb6 O36 66.3(2) . . ? O14 Tb6 O33 150.9(3) . . ? O10 Tb6 O33 87.6(3) . . ? O15 Tb6 O33 65.5(2) . . ? O11 Tb6 O33 74.6(2) . . ? O36 Tb6 O33 77.0(2) . . ? O14 Tb6 N10 72.5(3) . . ? O10 Tb6 N10 82.7(3) . . ? O15 Tb6 N10 64.2(3) . . ? O11 Tb6 N10 140.7(3) . . ? O36 Tb6 N10 87.7(3) . . ? O33 Tb6 N10 129.6(2) . . ? O14 Tb6 N7 88.4(3) . . ? O10 Tb6 N7 72.1(3) . . ? O15 Tb6 N7 137.2(3) . . ? O11 Tb6 N7 64.2(3) . . ? O36 Tb6 N7 130.0(2) . . ? O33 Tb6 N7 84.2(2) . . ? N10 Tb6 N7 137.2(3) . . ? O14 Tb6 Tb4 93.7(2) . . ? O10 Tb6 Tb4 145.6(2) . . ? O15 Tb6 Tb4 94.71(17) . . ? O11 Tb6 Tb4 34.71(15) . . ? O36 Tb6 Tb4 36.53(14) . . ? O33 Tb6 Tb4 59.06(18) . . ? N10 Tb6 Tb4 124.0(2) . . ? N7 Tb6 Tb4 94.5(2) . . ? O14 Tb6 Tb5 143.1(2) . . ? O10 Tb6 Tb5 95.0(2) . . ? O15 Tb6 Tb5 34.18(16) . . ? O11 Tb6 Tb5 95.13(15) . . ? O36 Tb6 Tb5 57.75(16) . . ? O33 Tb6 Tb5 36.84(16) . . ? N10 Tb6 Tb5 94.91(18) . . ? N7 Tb6 Tb5 120.75(18) . . ? Tb4 Tb6 Tb5 64.260(12) . . ? C2 O1 C1 120.2(13) . . ? C7 O2 Tb1 140.8(7) . . ? C9 O3 Tb2 122.6(6) . . ? C9 O3 Tb1 121.4(6) . . ? Tb2 O3 Tb1 111.3(2) . . ? N3 O4 H4 109.5 . . ? C13 O5 C12 116.0(9) . . ? C18 O6 Tb3 140.7(7) . . ? C20 O7 Tb5 122.7(6) . . ? C20 O7 Tb3 118.9(6) . . ? Tb5 O7 Tb3 110.3(3) . . ? N6 O8A H8A 109.5 . . ? C24 O9 C23 119.5(16) . . ? C29 O10 Tb6 144.4(7) . . ? C31 O11 Tb4 122.2(6) . . ? C31 O11 Tb6 119.8(6) . . ? Tb4 O11 Tb6 110.5(2) . . ? N9 O12 H12 109.5 . . ? C35 O13 C34 116.8(10) . . ? C40 O14 Tb6 140.8(7) . . ? C42 O15 Tb5 122.3(6) . . ? C42 O15 Tb6 121.1(6) . . ? Tb5 O15 Tb6 111.5(3) . . ? N12 O16 H16 109.5 . . ? C46 O17 C45 116.0(10) . . ? C51 O18 Tb3 143.3(7) . . ? C53 O19 Tb2 123.3(6) . . ? C53 O19 Tb3 119.7(6) . . ? Tb2 O19 Tb3 111.0(2) . . ? N15 O20 H20 109.5 . . ? C57 O21 C56 114.0(13) . . ? C62 O22 Tb1 142.6(7) . . ? C64 O23 Tb4 122.5(6) . . ? C64 O23 Tb1 121.0(6) . . ? Tb4 O23 Tb1 110.9(3) . . ? N18 O24 H24 109.5 . . ? C67 O25 Tb2 124.7(6) . . ? C67 O25 Tb1 123.7(6) . . ? Tb2 O25 Tb1 107.3(3) . . ? C67 O26 Tb4 120.3(7) . . ? C69 O27 Tb1 124.3(6) . . ? C69 O27 Tb4 124.2(6) . . ? Tb1 O27 Tb4 106.6(2) . . ? C69 O28 Tb2 119.6(6) . . ? C71 O29 Tb2 121.4(6) . . ? C71 O30 Tb3 123.6(6) . . ? C71 O30 Tb5 123.5(6) . . ? Tb3 O30 Tb5 106.4(2) . . ? C73 O31 Tb3 125.3(6) . . ? C73 O31 Tb2 124.0(6) . . ? Tb3 O31 Tb2 107.1(2) . . ? C73 O32 Tb5 117.5(6) . . ? C75 O33 Tb6 123.3(5) . . ? C75 O33 Tb5 123.4(5) . . ? Tb6 O33 Tb5 106.4(3) . . ? C75 O34 Tb4 119.6(6) . . ? C77 O35 Tb5 118.4(6) . . ? C77 O36 Tb6 123.6(6) . . ? C77 O36 Tb4 125.9(6) . . ? Tb6 O36 Tb4 107.1(2) . . ? Tb4 O37 Tb5 120.4(3) . . ? Tb4 O37 Tb2 120.2(3) . . ? Tb5 O37 Tb2 119.4(3) . . ? C8 N1 N2 110.7(8) . . ? C8 N1 Tb1 130.7(7) . . ? N2 N1 Tb1 118.5(6) . . ? C9 N2 N1 111.2(8) . . ? C10 N3 O4 112.9(8) . . ? C10 N3 Tb2 118.3(6) . . ? O4 N3 Tb2 128.8(6) . . ? C19 N4 N5 112.1(8) . . ? C19 N4 Tb3 129.7(7) . . ? N5 N4 Tb3 118.2(6) . . ? C20 N5 N4 110.8(8) . . ? C21 N6 O8A 112.4(9) . . ? C21 N6 Tb5 119.6(6) . . ? O8A N6 Tb5 127.3(7) . . ? C30 N7 N8 111.6(9) . . ? C30 N7 Tb6 129.3(7) . . ? N8 N7 Tb6 118.9(6) . . ? C31 N8 N7 110.6(8) . . ? C32 N9 O12 112.0(8) . . ? C32 N9 Tb4 120.5(7) . . ? O12 N9 Tb4 127.3(6) . . ? C41 N10 N11 110.1(8) . . ? C41 N10 Tb6 130.9(7) . . ? N11 N10 Tb6 119.0(6) . . ? C42 N11 N10 110.5(8) . . ? C43 N12 O16 112.7(9) . . ? C43 N12 Tb5 120.9(7) . . ? O16 N12 Tb5 126.1(6) . . ? C52 N13 N14 110.8(8) . . ? C52 N13 Tb3 131.1(7) . . ? N14 N13 Tb3 117.7(6) . . ? C53 N14 N13 111.2(8) . . ? C54 N15 O20 113.3(8) . . ? C54 N15 Tb2 120.0(7) . . ? O20 N15 Tb2 126.6(6) . . ? C63 N16 N17 112.2(9) . . ? C63 N16 Tb1 129.4(7) . . ? N17 N16 Tb1 118.4(6) . . ? C64 N17 N16 111.9(8) . . ? C65 N18 O24 112.9(8) . . ? C65 N18 Tb4 119.0(7) . . ? O24 N18 Tb4 128.0(7) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 124.7(12) . . ? C3 C2 C7 121.4(13) . . ? O1 C2 C7 113.7(10) . . ? C2 C3 C4 120.7(13) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.7(13) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 121.5(14) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C7 120.2(11) . . ? C5 C6 C8 116.7(11) . . ? C7 C6 C8 123.1(10) . . ? O2 C7 C6 124.2(10) . . ? O2 C7 C2 119.4(11) . . ? C6 C7 C2 116.4(10) . . ? N1 C8 C6 125.8(10) . . ? N1 C8 H8 117.1 . . ? C6 C8 H8 117.1 . . ? N2 C9 O3 124.8(9) . . ? N2 C9 C10 117.2(8) . . ? O3 C9 C10 117.9(9) . . ? N3 C10 C9 113.5(8) . . ? N3 C10 C11 124.5(10) . . ? C9 C10 C11 122.0(10) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O5 C12 H12A 109.5 . . ? O5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O5 C13 C14 126.0(10) . . ? O5 C13 C18 112.9(8) . . ? C14 C13 C18 121.1(10) . . ? C15 C14 C13 121.2(10) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 119.6(10) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 121.6(11) . . ? C15 C16 H16A 119.2 . . ? C17 C16 H16A 119.2 . . ? C16 C17 C18 119.7(10) . . ? C16 C17 C19 117.9(10) . . ? C18 C17 C19 122.1(9) . . ? O6 C18 C17 123.3(9) . . ? O6 C18 C13 120.0(9) . . ? C17 C18 C13 116.7(9) . . ? N4 C19 C17 127.1(10) . . ? N4 C19 H19 116.4 . . ? C17 C19 H19 116.4 . . ? O7 C20 N5 127.7(9) . . ? O7 C20 C21 117.5(9) . . ? N5 C20 C21 114.5(9) . . ? N6 C21 C22 125.0(10) . . ? N6 C21 C20 111.2(9) . . ? C22 C21 C20 123.5(10) . . ? 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 . . ? O9 C23 H23A 109.5 . . ? O9 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O9 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 O9 125.4(13) . . ? C25 C24 C29 122.3(13) . . ? O9 C24 C29 112.1(12) . . ? C24 C25 C26 120.6(16) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 120.9(19) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 119.2(16) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? C27 C28 C29 121.3(13) . . ? C27 C28 C30 118.0(12) . . ? C29 C28 C30 120.8(11) . . ? O10 C29 C24 120.7(11) . . ? O10 C29 C28 123.9(11) . . ? C24 C29 C28 115.4(11) . . ? N7 C30 C28 128.3(11) . . ? N7 C30 H30 115.8 . . ? C28 C30 H30 115.8 . . ? N8 C31 O11 126.3(9) . . ? N8 C31 C32 117.2(8) . . ? O11 C31 C32 116.3(9) . . ? N9 C32 C33 129.3(10) . . ? N9 C32 C31 112.0(8) . . ? C33 C32 C31 118.6(9) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O13 C34 H34A 109.5 . . ? O13 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O13 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O13 C35 C36 122.6(9) . . ? O13 C35 C40 114.8(8) . . ? C36 C35 C40 122.6(9) . . ? C37 C36 C35 120.8(10) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C38 118.1(9) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? C39 C38 C37 121.3(9) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C38 C39 C40 118.4(9) . . ? C38 C39 C41 118.0(9) . . ? C40 C39 C41 123.1(8) . . ? O14 C40 C35 118.7(9) . . ? O14 C40 C39 122.6(8) . . ? C35 C40 C39 118.6(8) . . ? N10 C41 C39 125.5(9) . . ? N10 C41 H41 117.2 . . ? C39 C41 H41 117.2 . . ? N11 C42 O15 124.8(10) . . ? N11 C42 C43 118.2(9) . . ? O15 C42 C43 117.0(10) . . ? N12 C43 C42 112.3(9) . . ? N12 C43 C44 128.0(11) . . ? C42 C43 C44 119.6(11) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O17 C45 H45A 109.5 . . ? O17 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O17 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O17 C46 C47 127.3(13) . . ? O17 C46 C51 113.6(10) . . ? C47 C46 C51 119.0(13) . . ? C46 C47 C48 121.0(14) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? C49 C48 C47 118.8(14) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C48 C49 C50 122.4(14) . . ? C48 C49 H49 118.8 . . ? C50 C49 H49 118.8 . . ? C49 C50 C52 116.8(10) . . ? C49 C50 C51 119.6(10) . . ? C52 C50 C51 123.4(9) . . ? O18 C51 C50 122.5(10) . . ? O18 C51 C46 118.4(10) . . ? C50 C51 C46 119.0(10) . . ? N13 C52 C50 127.0(10) . . ? N13 C52 H52 116.5 . . ? C50 C52 H52 116.5 . . ? O19 C53 N14 126.7(9) . . ? O19 C53 C54 116.6(9) . . ? N14 C53 C54 116.4(9) . . ? N15 C54 C55 126.1(10) . . ? N15 C54 C53 112.4(9) . . ? C55 C54 C53 121.5(10) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O21 C56 H56A 109.5 . . ? O21 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O21 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 O21 121.8(12) . . ? C58 C57 C62 121.9(13) . . ? O21 C57 C62 116.3(11) . . ? C59 C58 C57 121.6(12) . . ? C59 C58 H58 119.2 . . ? C57 C58 H58 119.2 . . ? C58 C59 C60 119.6(12) . . ? C58 C59 H59 120.2 . . ? C60 C59 H59 120.2 . . ? C59 C60 C61 121.1(12) . . ? C59 C60 H60 119.5 . . ? C61 C60 H60 119.5 . . ? C60 C61 C63 117.6(11) . . ? C60 C61 C62 120.2(10) . . ? C63 C61 C62 122.0(10) . . ? O22 C62 C57 120.8(11) . . ? O22 C62 C61 123.5(10) . . ? C57 C62 C61 115.6(11) . . ? N16 C63 C61 127.9(10) . . ? N16 C63 H63 116.1 . . ? C61 C63 H63 116.1 . . ? O23 C64 N17 124.7(9) . . ? O23 C64 C65 118.1(9) . . ? N17 C64 C65 117.2(9) . . ? N18 C65 C64 112.8(9) . . ? N18 C65 C66 125.2(10) . . ? C64 C65 C66 121.9(10) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O26 C67 O25 120.7(10) . . ? O26 C67 C68 121.7(10) . . ? O25 C67 C68 117.5(9) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O28 C69 O27 123.1(9) . . ? O28 C69 C70 119.7(9) . . ? O27 C69 C70 117.1(8) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O29 C71 O30 121.5(10) . . ? O29 C71 C72 121.0(10) . . ? O30 C71 C72 117.4(10) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O32 C73 O31 122.6(9) . . ? O32 C73 C74 119.1(9) . . ? O31 C73 C74 118.2(9) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O34 C75 O33 124.5(9) . . ? O34 C75 C76 119.7(9) . . ? O33 C75 C76 115.8(9) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? O35 C77 O36 121.3(9) . . ? O35 C77 C78 121.1(9) . . ? O36 C77 C78 117.6(9) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O4 H4 O6 . . . 2.930(12) 0.840 2.120 162 no O8A H8A O10 . . . 2.978(14) 0.840 2.302 138 no O16 H16 O7 . . . 3.006(13) 0.840 2.540 116 no O20 H20 O3 . . . 3.034(13) 0.840 2.474 125 no O20 H20 O22 . . . 3.021(14) 0.840 2.471 124 no O24 H24 O14 . . . 2.953(12) 0.840 2.158 158 no _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 10.511 _refine_diff_density_min -2.991 _refine_diff_density_rms 0.283 _iucr_refine_instructions_details ; TITL _MUA1942 CELL 0.71075 17.83540 18.46240 20.20030 79.794 68.816 76.342 ZERR 2 0.00130 0.00140 0.00140 0.006 0.005 0.005 LATT 1 SFAC C H N O TB UNIT 168 224 38 86 12 SHEL 8.147180 0.796452 L.S. 5 FMAP 2 PLAN -25 TEMP -110.0 ACTA BOND $H OMIT 5 -4 8 OMIT 7 4 6 ISOR 0.01 0.02 C37 C51 SIMU 0.01 0.025 1.7 O9 C23 SIMU 0.005 0.01 1.7 C50 C52 SIMU 0.005 0.01 1.7 N13 C52 SIMU 0.005 0.01 1.7 C36 C37 SIMU 0.005 0.01 1.7 C38 C37 SIMU 0.005 0.01 1.7 O21 C56 DFIX 1.4000 0.0200 C40 C39 DFIX 1.4000 0.0200 C39 C38 DFIX 1.4000 0.0200 C38 C37 DFIX 1.4000 0.0200 C37 C36 DFIX 1.4000 0.0200 C36 C35 DFIX 1.4000 0.0200 C35 C40 FLAT 0.0100 C40 C35 C36 C37 C38 C39 DFIX 1.4300 0.0200 C50 C52 DFIX 1.3000 0.0200 C52 N13 FLAT 0.0500 C49 C50 C52 N13 N14 DANG 2.4456 0.0400 C40 C38 DANG 2.4456 0.0400 C39 C37 DANG 2.4441 0.0400 C38 C36 DANG 2.4391 0.0400 C37 C35 DANG 2.4448 0.0400 C36 C40 DANG 2.4410 0.0400 C35 C39 DFIX 1.43 0.0050 O9 C23 DFIX 1.43 0.0100 O13 C34 DFIX 1.43 0.0100 O17 C45 DFIX 1.43 0.0100 O5 C12 DFIX 1.43 0.0100 O21 C56 DFIX 1.43 0.0100 O1 C1 SIZE 0.330 0.090 0.340 WGHT 0.116900 89.779999 FVAR 1.00554 TB1 5 0.792291 -0.205145 0.266103 11.00000 0.02184 0.02479 = 0.03403 -0.00525 -0.00770 -0.00432 TB2 5 0.870821 -0.020229 0.250363 11.00000 0.01360 0.02474 = 0.02194 -0.00293 -0.00436 -0.00425 TB3 5 0.933424 0.173311 0.233143 11.00000 0.01740 0.02753 = 0.02531 -0.00199 -0.00922 -0.00607 TB4 5 0.636440 -0.019903 0.250904 11.00000 0.01333 0.02621 = 0.02437 -0.00794 -0.00364 -0.00375 TB5 5 0.711900 0.181519 0.233470 11.00000 0.01736 0.02576 = 0.03090 -0.00765 -0.01118 -0.00263 TB6 5 0.493099 0.173744 0.236228 11.00000 0.01663 0.03021 = 0.03671 -0.01543 -0.01068 0.00033 O1 4 0.637840 -0.339097 0.200080 11.00000 0.06742 0.05587 = 0.07277 -0.01503 -0.02895 -0.02329 O2 4 0.747631 -0.271182 0.209585 11.00000 0.03904 0.04171 = 0.04683 -0.01882 -0.01122 -0.01009 O3 4 0.908594 -0.147441 0.228439 11.00000 0.01795 0.02119 = 0.03195 -0.00539 -0.00148 0.00010 O4 4 1.088598 -0.028922 0.154820 11.00000 0.02413 0.04960 = 0.04248 -0.00098 -0.00320 -0.01778 AFIX 147 H4 2 1.070725 0.016096 0.163050 11.00000 -1.20000 AFIX 0 O5 4 1.208656 0.045993 0.171100 11.00000 0.01802 0.03916 = 0.05942 0.00003 -0.00673 -0.00112 O6 4 1.065498 0.128778 0.176219 11.00000 0.01678 0.03675 = 0.04100 0.00202 -0.00948 -0.00740 O7 4 0.823765 0.244772 0.192787 11.00000 0.02121 0.03209 = 0.03882 -0.00268 -0.01931 -0.00561 O8A 4 0.640320 0.329841 0.117345 11.00000 0.04268 0.04865 = 0.10868 0.01091 -0.05828 -0.01016 AFIX 147 H8A 2 0.595848 0.327037 0.150636 11.00000 -1.20000 AFIX 0 O9 4 0.460817 0.429715 0.155067 11.00000 0.09180 0.04590 = 0.17747 -0.02921 -0.09190 -0.00402 O10 4 0.477669 0.283976 0.170658 11.00000 0.06650 0.02877 = 0.06274 -0.01134 -0.04195 -0.00024 O11 4 0.526658 0.046577 0.211112 11.00000 0.02349 0.03118 = 0.03174 -0.01415 -0.01262 -0.00161 O12 4 0.618006 -0.162882 0.160536 11.00000 0.03656 0.03020 = 0.05340 -0.02406 -0.01309 -0.00401 AFIX 147 H12 2 0.579456 -0.179232 0.157301 11.00000 -1.20000 AFIX 0 O13 4 0.269889 0.046248 0.325999 11.00000 0.02654 0.04330 = 0.07625 -0.02574 -0.01137 -0.00833 O14 4 0.379043 0.129808 0.301381 11.00000 0.01766 0.04320 = 0.05491 -0.02200 0.00102 -0.00241 O15 4 0.573045 0.242199 0.264272 11.00000 0.02222 0.03992 = 0.04316 -0.01934 -0.01572 0.00222 O16 4 0.721829 0.335938 0.315220 11.00000 0.03398 0.05750 = 0.10362 -0.04489 -0.02861 -0.00688 AFIX 147 H16 2 0.768068 0.307945 0.307368 11.00000 -1.20000 AFIX 0 O17 4 0.858026 0.426914 0.280835 11.00000 0.04783 0.03375 = 0.05932 -0.00742 -0.02334 -0.00534 O18 4 0.911794 0.283054 0.276880 11.00000 0.06434 0.03084 = 0.03457 -0.00349 -0.02703 -0.01088 O19 4 0.951560 0.044868 0.279962 11.00000 0.02266 0.02295 = 0.03005 0.00375 -0.01112 -0.00591 O20 4 0.953572 -0.168295 0.362714 11.00000 0.04284 0.02690 = 0.05233 0.00190 -0.02690 -0.00592 AFIX 147 H20 2 0.960821 -0.193289 0.329257 11.00000 -1.20000 AFIX 0 O21 4 1.009261 -0.339836 0.353760 11.00000 0.04783 0.07566 = 0.07464 0.01050 -0.02435 -0.00971 O22 4 0.866550 -0.273331 0.331532 11.00000 0.03148 0.04054 = 0.05333 0.01123 -0.01680 -0.00514 O23 4 0.651078 -0.147689 0.294862 11.00000 0.02103 0.02586 = 0.03727 0.00317 -0.00365 -0.00528 O24 4 0.423408 -0.029691 0.350680 11.00000 0.01237 0.05072 = 0.06507 -0.01359 -0.00578 0.00105 AFIX 147 H24 2 0.422195 0.012416 0.326705 11.00000 -1.20000 AFIX 0 O25 4 0.776744 -0.099344 0.329201 11.00000 0.01969 0.03013 = 0.03302 -0.00868 -0.00106 -0.00718 O26 4 0.646842 -0.036704 0.371076 11.00000 0.02671 0.04106 = 0.03684 -0.00555 -0.00929 -0.01207 O27 4 0.763876 -0.096933 0.184186 11.00000 0.01865 0.02205 = 0.03028 0.00174 -0.00485 0.00000 O28 4 0.866038 -0.034243 0.132604 11.00000 0.01825 0.03650 = 0.03256 -0.00454 -0.00510 -0.00355 O29 4 0.795731 0.035196 0.363987 11.00000 0.02195 0.03602 = 0.03162 -0.00025 -0.00695 -0.00552 O30 4 0.797291 0.152773 0.309924 11.00000 0.01877 0.03451 = 0.02846 -0.00249 -0.01024 -0.01020 O31 4 0.903474 0.090500 0.168751 11.00000 0.01986 0.02683 = 0.02195 0.00014 -0.01076 -0.00407 O32 4 0.810914 0.141423 0.115525 11.00000 0.02482 0.02875 = 0.03011 0.00149 -0.01411 -0.00668 O33 4 0.637748 0.153626 0.162785 11.00000 0.01843 0.03445 = 0.03911 -0.01814 -0.00648 -0.00510 O34 4 0.687942 0.037617 0.127974 11.00000 0.01998 0.03447 = 0.03944 -0.00894 -0.00554 -0.00900 O35 4 0.629863 0.139824 0.358346 11.00000 0.02824 0.04402 = 0.04342 -0.02059 -0.01087 -0.00648 O36 4 0.558170 0.088906 0.314292 11.00000 0.02356 0.03247 = 0.02971 -0.01771 -0.01210 -0.00096 O37 4 0.738815 0.047137 0.245341 11.00000 0.01533 0.02725 = 0.04846 -0.00821 -0.01469 -0.00042 N1 3 0.913213 -0.258710 0.164638 11.00000 0.02792 0.03642 = 0.03607 -0.00531 -0.01337 0.00033 N2 3 0.986911 -0.230915 0.144544 11.00000 0.02322 0.03944 = 0.02913 -0.01217 -0.00225 -0.00374 N3 3 1.024324 -0.066503 0.176856 11.00000 0.02108 0.03210 = 0.02491 -0.00309 -0.00559 -0.00355 N4 3 0.976133 0.251265 0.115446 11.00000 0.03754 0.02874 = 0.02715 0.00312 -0.01580 -0.01300 N5 3 0.913487 0.296680 0.089640 11.00000 0.03404 0.03347 = 0.04000 0.00470 -0.02130 -0.00917 N6 3 0.705421 0.296529 0.142091 11.00000 0.02574 0.02668 = 0.05736 -0.00122 -0.02734 0.00156 N7 3 0.471334 0.150576 0.125879 11.00000 0.02145 0.03640 = 0.03608 -0.00845 -0.01294 -0.00702 N8 3 0.485318 0.076162 0.109976 11.00000 0.02490 0.03229 = 0.03569 -0.01158 -0.00979 -0.00067 N9 3 0.591358 -0.088190 0.174841 11.00000 0.02129 0.02592 = 0.03989 -0.00789 -0.00958 -0.00321 N10 3 0.418917 0.252301 0.337234 11.00000 0.01996 0.03912 = 0.04966 -0.02401 -0.01329 0.00367 N11 3 0.461512 0.300866 0.353035 11.00000 0.02860 0.05219 = 0.06903 -0.04493 -0.01223 0.00394 N12 3 0.669214 0.300646 0.300322 11.00000 0.03023 0.04117 = 0.07087 -0.02526 -0.02745 -0.00264 N13 3 0.964466 0.146139 0.348004 11.00000 0.03494 0.03176 = 0.03497 -0.00823 -0.01742 -0.00104 N14 3 0.983751 0.069845 0.374024 11.00000 0.02256 0.03190 = 0.03291 -0.00256 -0.01304 -0.00450 N15 3 0.947003 -0.091442 0.337657 11.00000 0.01987 0.02809 = 0.03212 -0.00259 -0.01050 -0.00177 N16 3 0.695049 -0.260364 0.379035 11.00000 0.03093 0.03870 = 0.03294 0.00145 -0.01434 -0.01058 N17 3 0.610734 -0.232465 0.395380 11.00000 0.02999 0.03587 = 0.04303 -0.00016 -0.00927 -0.00922 N18 3 0.503107 -0.068194 0.333839 11.00000 0.01345 0.04032 = 0.03590 -0.01253 -0.00469 -0.00412 C1 1 0.573268 -0.366010 0.192522 11.00000 0.11042 0.14143 = 0.12807 -0.06261 -0.07788 -0.00162 AFIX 137 H1A 2 0.560829 -0.339356 0.150151 11.00000 -1.20000 H1B 2 0.524457 -0.357443 0.234915 11.00000 -1.20000 H1C 2 0.590003 -0.419786 0.187291 11.00000 -1.20000 AFIX 0 C2 1 0.717591 -0.362597 0.158397 11.00000 0.05448 0.03644 = 0.04953 -0.00533 -0.02942 -0.00763 C3 1 0.742990 -0.419286 0.115822 11.00000 0.07470 0.04939 = 0.07270 -0.01463 -0.03125 -0.01672 AFIX 43 H3 2 0.704063 -0.444885 0.112954 11.00000 -1.20000 AFIX 0 C4 1 0.824858 -0.439983 0.076717 11.00000 0.08863 0.04585 = 0.07449 -0.02510 -0.03987 -0.01191 AFIX 43 H4A 2 0.841751 -0.478026 0.045460 11.00000 -1.20000 AFIX 0 C5 1 0.881122 -0.405621 0.083199 11.00000 0.07305 0.04131 = 0.03869 -0.01287 -0.02154 -0.01283 AFIX 43 H5 2 0.937458 -0.421322 0.057426 11.00000 -1.20000 AFIX 0 C6 1 0.857958 -0.347831 0.126852 11.00000 0.04022 0.02667 = 0.04562 -0.00436 -0.02498 0.00058 C7 1 0.774794 -0.324644 0.166659 11.00000 0.05533 0.02574 = 0.04235 -0.01060 -0.03011 -0.00428 C8 1 0.922221 -0.312081 0.125885 11.00000 0.03444 0.02662 = 0.04436 -0.01041 -0.01546 0.00284 AFIX 43 H8 2 0.975743 -0.328728 0.094374 11.00000 -1.20000 AFIX 0 C9 1 0.976821 -0.173852 0.178893 11.00000 0.01872 0.02714 = 0.03340 -0.00172 -0.00626 -0.00367 C10 1 1.045833 -0.133530 0.157386 11.00000 0.01587 0.04554 = 0.02069 -0.00888 0.00161 -0.00374 C11 1 1.131010 -0.168077 0.116330 11.00000 0.01586 0.06797 = 0.05816 -0.02718 0.01168 -0.00063 AFIX 137 H11A 2 1.140506 -0.155231 0.065121 11.00000 -1.20000 H11B 2 1.138590 -0.222645 0.127254 11.00000 -1.20000 H11C 2 1.169935 -0.149069 0.129621 11.00000 -1.20000 AFIX 0 C12 1 1.283174 -0.008392 0.159049 11.00000 0.03302 0.05013 = 0.09789 0.00589 -0.01877 0.01477 AFIX 137 H12A 2 1.303548 -0.020400 0.109509 11.00000 -1.20000 H12B 2 1.272721 -0.053971 0.191361 11.00000 -1.20000 H12C 2 1.324176 0.012027 0.168042 11.00000 -1.20000 AFIX 0 C13 1 1.210107 0.106855 0.121658 11.00000 0.01760 0.04282 = 0.03721 -0.01221 -0.00129 -0.00824 C14 1 1.280301 0.129446 0.070685 11.00000 0.02155 0.04078 = 0.04547 -0.00918 -0.00460 -0.00746 AFIX 43 H14 2 1.332670 0.100435 0.068366 11.00000 -1.20000 AFIX 0 C15 1 1.274850 0.192005 0.024569 11.00000 0.03325 0.05284 = 0.04486 -0.00780 0.00637 -0.01993 AFIX 43 H15 2 1.323069 0.207145 -0.009004 11.00000 -1.20000 AFIX 0 C16 1 1.197625 0.234154 0.026774 11.00000 0.02676 0.05187 = 0.02630 -0.00089 -0.00187 -0.01914 AFIX 43 H16A 2 1.194173 0.276979 -0.006643 11.00000 -1.20000 AFIX 0 C17 1 1.125341 0.214637 0.077113 11.00000 0.02979 0.04125 = 0.01891 -0.00574 -0.00445 -0.01352 C18 1 1.129669 0.149836 0.127441 11.00000 0.01815 0.03634 = 0.02398 -0.00282 -0.00429 -0.01025 C19 1 1.048445 0.257766 0.072229 11.00000 0.03232 0.04405 = 0.04008 0.00328 -0.02162 -0.01893 AFIX 43 H19 2 1.051387 0.295062 0.032849 11.00000 -1.20000 AFIX 0 C20 1 0.841482 0.286963 0.132767 11.00000 0.03254 0.02003 = 0.03932 0.00012 -0.01998 -0.00470 C21 1 0.772861 0.323678 0.105058 11.00000 0.04488 0.02784 = 0.05714 0.00970 -0.03484 -0.01211 C22 1 0.782672 0.377976 0.039707 11.00000 0.05330 0.07252 = 0.10523 0.04935 -0.05902 -0.03623 AFIX 137 H22A 2 0.771890 0.356935 0.003501 11.00000 -1.20000 H22B 2 0.838681 0.387671 0.021010 11.00000 -1.20000 H22C 2 0.743889 0.424994 0.051676 11.00000 -1.20000 AFIX 0 C23 1 0.464034 0.507441 0.144164 11.00000 0.15265 0.09750 = 0.18330 -0.02396 -0.08860 -0.03120 AFIX 137 H23A 2 0.519251 0.514631 0.113759 11.00000 -1.20000 H23B 2 0.450580 0.526281 0.190286 11.00000 -1.20000 H23C 2 0.424485 0.534891 0.120946 11.00000 -1.20000 AFIX 0 C24 1 0.446957 0.397086 0.103934 11.00000 0.05541 0.02671 = 0.09395 -0.00244 -0.04936 -0.00714 C25 1 0.421874 0.435050 0.049595 11.00000 0.14798 0.04227 = 0.13871 0.00727 -0.08255 -0.03082 AFIX 43 H25 2 0.415819 0.488081 0.042129 11.00000 -1.20000 AFIX 0 C26 1 0.404691 0.396729 0.004083 11.00000 0.20059 0.05114 = 0.15799 0.03645 -0.11410 -0.06122 AFIX 43 H26 2 0.388919 0.424060 -0.034789 11.00000 -1.20000 AFIX 0 C27 1 0.410281 0.321690 0.014822 11.00000 0.15458 0.05769 = 0.09244 0.01659 -0.09848 -0.03115 AFIX 43 H27 2 0.395101 0.296624 -0.014243 11.00000 -1.20000 AFIX 0 C28 1 0.439263 0.280418 0.070349 11.00000 0.06164 0.04515 = 0.06545 -0.00007 -0.04442 -0.01916 C29 1 0.455138 0.317570 0.118978 11.00000 0.02996 0.03840 = 0.05220 -0.00815 -0.01956 -0.00345 C30 1 0.452581 0.198742 0.076062 11.00000 0.03574 0.04434 = 0.04945 -0.00388 -0.02739 -0.01123 AFIX 43 H30 2 0.446851 0.178040 0.038702 11.00000 -1.20000 AFIX 0 C31 1 0.514734 0.029226 0.155542 11.00000 0.01359 0.03861 = 0.03249 -0.01892 -0.00319 -0.00650 C32 1 0.543207 -0.051744 0.140388 11.00000 0.02035 0.04072 = 0.02254 -0.01162 -0.00485 -0.00889 C33 1 0.518736 -0.077360 0.085927 11.00000 0.03866 0.04494 = 0.05919 -0.02156 -0.02935 -0.00537 AFIX 137 H33A 2 0.567726 -0.093229 0.045679 11.00000 -1.20000 H33B 2 0.482168 -0.036026 0.068883 11.00000 -1.20000 H33C 2 0.490338 -0.119549 0.107663 11.00000 -1.20000 AFIX 0 C34 1 0.216249 -0.006788 0.347823 11.00000 0.04729 0.05458 = 0.09725 -0.01074 -0.01224 -0.02783 AFIX 137 H34A 2 0.204519 -0.022826 0.398884 11.00000 -1.20000 H34B 2 0.242525 -0.050388 0.320698 11.00000 -1.20000 H34C 2 0.165015 0.016576 0.338814 11.00000 -1.20000 AFIX 0 C35 1 0.244717 0.107905 0.362164 11.00000 0.02012 0.03837 = 0.04492 -0.01078 -0.01443 -0.00121 C36 1 0.164618 0.128427 0.407065 11.00000 0.02434 0.04417 = 0.05176 -0.00653 0.00891 -0.00100 AFIX 43 H36 2 0.126067 0.097318 0.415007 11.00000 -1.20000 AFIX 0 C37 1 0.140878 0.192335 0.439658 11.00000 0.02710 0.03807 = 0.05314 0.00462 0.02247 0.00526 AFIX 43 H37 2 0.085842 0.207172 0.469220 11.00000 -1.20000 AFIX 0 C38 1 0.202430 0.237709 0.427975 11.00000 0.02233 0.04160 = 0.04721 -0.00931 0.00379 -0.00039 AFIX 43 H38 2 0.187400 0.281725 0.451619 11.00000 -1.20000 AFIX 0 C39 1 0.283716 0.217424 0.382280 11.00000 0.02509 0.04986 = 0.03513 -0.01420 -0.00183 -0.00749 C40 1 0.305253 0.150905 0.348689 11.00000 0.01107 0.04426 = 0.03842 -0.01122 -0.00649 0.00043 C41 1 0.343513 0.261148 0.379032 11.00000 0.02053 0.05826 = 0.03749 -0.03085 -0.01191 0.00389 AFIX 43 H41 2 0.325522 0.299335 0.410263 11.00000 -1.20000 AFIX 0 C42 1 0.539520 0.288433 0.314273 11.00000 0.03367 0.03351 = 0.05578 -0.02983 -0.02067 0.00903 C43 1 0.595553 0.328442 0.328435 11.00000 0.03658 0.05232 = 0.11062 -0.06110 -0.03489 0.00629 C44 1 0.559801 0.390313 0.376600 11.00000 0.03544 0.13193 = 0.21060 -0.14219 -0.03247 0.00720 AFIX 137 H44A 2 0.591044 0.430878 0.357127 11.00000 -1.20000 H44B 2 0.562457 0.370869 0.424259 11.00000 -1.20000 H44C 2 0.502595 0.409528 0.379816 11.00000 -1.20000 AFIX 0 C45 1 0.822551 0.504622 0.284181 11.00000 0.11998 0.03805 = 0.07273 0.01001 -0.05462 -0.00045 AFIX 137 H45A 2 0.776705 0.511370 0.328990 11.00000 -1.20000 H45B 2 0.802696 0.523278 0.243817 11.00000 -1.20000 H45C 2 0.863900 0.532561 0.282031 11.00000 -1.20000 AFIX 0 C46 1 0.883107 0.393882 0.333533 11.00000 0.03307 0.05169 = 0.07833 -0.02485 -0.02924 -0.00078 C47 1 0.883426 0.426336 0.389879 11.00000 0.10477 0.04652 = 0.09013 -0.03788 -0.06426 0.02524 AFIX 43 H47 2 0.868177 0.479182 0.390470 11.00000 -1.20000 AFIX 0 C48 1 0.906904 0.380560 0.448743 11.00000 0.10098 0.07175 = 0.06991 -0.03284 -0.05056 0.01869 AFIX 43 H48 2 0.901979 0.402541 0.489585 11.00000 -1.20000 AFIX 0 C49 1 0.935936 0.305886 0.443896 11.00000 0.11564 0.03998 = 0.09495 -0.02077 -0.08138 0.00543 AFIX 43 H49 2 0.956446 0.277072 0.479688 11.00000 -1.20000 AFIX 0 C50 1 0.936679 0.269936 0.388012 11.00000 0.04796 0.03746 = 0.04326 -0.01594 -0.03029 0.00857 C51 1 0.909488 0.312922 0.332005 11.00000 0.04329 0.03335 = 0.04312 -0.01049 -0.02690 -0.00483 C52 1 0.958571 0.190478 0.393987 11.00000 0.04825 0.03665 = 0.03804 -0.01359 -0.03022 0.00942 AFIX 43 H52 2 0.970155 0.167147 0.435967 11.00000 -1.20000 AFIX 0 C53 1 0.973488 0.025458 0.336135 11.00000 0.02078 0.03118 = 0.03045 0.00459 -0.01592 -0.00387 C54 1 0.980620 -0.056229 0.364119 11.00000 0.01748 0.02376 = 0.04491 0.00444 -0.00439 -0.00273 C55 1 1.020055 -0.088008 0.419492 11.00000 0.05485 0.06108 = 0.07130 0.00921 -0.04709 -0.02207 AFIX 137 H55A 2 1.014863 -0.140673 0.433592 11.00000 -1.20000 H55B 2 0.993042 -0.059740 0.461277 11.00000 -1.20000 H55C 2 1.078132 -0.084462 0.399937 11.00000 -1.20000 AFIX 0 C56 1 1.035829 -0.362168 0.282992 11.00000 0.07524 0.10803 = 0.10858 0.01654 -0.00891 -0.00444 AFIX 137 H56A 2 1.068891 -0.412832 0.281724 11.00000 -1.20000 H56B 2 1.068766 -0.327227 0.249195 11.00000 -1.20000 H56C 2 0.987947 -0.361676 0.269798 11.00000 -1.20000 AFIX 0 C57 1 0.936910 -0.362044 0.399203 11.00000 0.05463 0.02486 = 0.05731 -0.00141 -0.02547 0.00648 C58 1 0.935459 -0.415624 0.457014 11.00000 0.06190 0.04028 = 0.06619 -0.01394 -0.04022 0.00643 AFIX 43 H58 2 0.985357 -0.438789 0.465119 11.00000 -1.20000 AFIX 0 C59 1 0.864515 -0.435753 0.502265 11.00000 0.07780 0.02979 = 0.04685 -0.00636 -0.03466 0.00308 AFIX 43 H59 2 0.864788 -0.471784 0.542131 11.00000 -1.20000 AFIX 0 C60 1 0.791798 -0.403519 0.490026 11.00000 0.05679 0.02000 = 0.04829 -0.00398 -0.01717 -0.00094 AFIX 43 H60 2 0.742408 -0.418695 0.521045 11.00000 -1.20000 AFIX 0 C61 1 0.789767 -0.348446 0.432204 11.00000 0.04743 0.02636 = 0.03142 -0.00847 -0.02279 0.00148 C62 1 0.864307 -0.325753 0.383869 11.00000 0.03786 0.03598 = 0.04000 -0.00903 -0.00975 -0.00648 C63 1 0.711166 -0.312018 0.427734 11.00000 0.04019 0.02828 = 0.03875 -0.00024 -0.01175 -0.01166 AFIX 43 H63 2 0.665174 -0.327318 0.464716 11.00000 -1.20000 AFIX 0 C64 1 0.595337 -0.174285 0.350236 11.00000 0.02288 0.03248 = 0.02815 -0.00481 -0.00558 -0.01418 C65 1 0.509300 -0.133759 0.366802 11.00000 0.02871 0.03888 = 0.03263 -0.00071 -0.00757 -0.00959 C66 1 0.439760 -0.167771 0.417520 11.00000 0.01860 0.07884 = 0.05328 0.00736 0.00209 -0.01770 AFIX 137 H66A 2 0.389014 -0.141759 0.408823 11.00000 -1.20000 H66B 2 0.434948 -0.163153 0.466545 11.00000 -1.20000 H66C 2 0.449410 -0.220854 0.410674 11.00000 -1.20000 AFIX 0 C67 1 0.710311 -0.076180 0.382765 11.00000 0.02046 0.03726 = 0.04482 -0.00695 -0.00454 -0.01092 C68 1 0.714156 -0.096286 0.456696 11.00000 0.02669 0.05049 = 0.03171 0.00057 -0.00440 -0.00909 AFIX 137 H68A 2 0.679475 -0.056467 0.486594 11.00000 -1.50000 H68B 2 0.770821 -0.102078 0.455091 11.00000 -1.50000 H68C 2 0.694691 -0.143481 0.476830 11.00000 -1.50000 AFIX 0 C69 1 0.818784 -0.071841 0.128974 11.00000 0.02282 0.02513 = 0.02748 -0.00483 -0.00911 -0.00243 C70 1 0.824119 -0.089789 0.056811 11.00000 0.03897 0.04275 = 0.03705 -0.01697 -0.00662 -0.01211 AFIX 137 H70A 2 0.845469 -0.050427 0.020010 11.00000 -1.50000 H70B 2 0.769500 -0.092493 0.057800 11.00000 -1.50000 H70C 2 0.860835 -0.138046 0.045991 11.00000 -1.50000 AFIX 0 C71 1 0.783958 0.105452 0.367399 11.00000 0.01583 0.04272 = 0.03467 -0.00328 -0.00485 -0.00894 C72 1 0.754760 0.136673 0.437401 11.00000 0.02801 0.05750 = 0.03636 -0.02071 -0.00132 -0.01071 AFIX 137 H72A 2 0.723804 0.102671 0.474610 11.00000 -1.50000 H72B 2 0.719383 0.185787 0.434711 11.00000 -1.50000 H72C 2 0.801877 0.142106 0.448946 11.00000 -1.50000 AFIX 0 C73 1 0.882719 0.110589 0.112863 11.00000 0.02723 0.02451 = 0.02921 -0.00249 -0.00932 -0.00905 C74 1 0.947355 0.099931 0.041951 11.00000 0.03751 0.04143 = 0.03053 0.00031 -0.01380 -0.00455 AFIX 137 H74A 2 0.940099 0.058527 0.021860 11.00000 -1.50000 H74B 2 1.001391 0.088273 0.047565 11.00000 -1.50000 H74C 2 0.943098 0.145980 0.009774 11.00000 -1.50000 AFIX 0 C75 1 0.669929 0.106404 0.114724 11.00000 0.01849 0.02803 = 0.02198 -0.00373 -0.00778 -0.00495 C76 1 0.685231 0.140703 0.037106 11.00000 0.03725 0.04501 = 0.03618 0.00233 -0.00689 -0.01926 AFIX 137 H76A 2 0.718440 0.102432 0.004885 11.00000 -1.50000 H76B 2 0.714292 0.182296 0.027857 11.00000 -1.50000 H76C 2 0.632733 0.159287 0.029000 11.00000 -1.50000 AFIX 0 C77 1 0.569618 0.109523 0.367562 11.00000 0.01889 0.04456 = 0.02528 -0.00814 0.00016 -0.00543 C78 1 0.507713 0.097657 0.440505 11.00000 0.03693 0.05916 = 0.03923 -0.01825 -0.00319 -0.01593 AFIX 137 H78A 2 0.535990 0.079394 0.475492 11.00000 -1.50000 H78B 2 0.476458 0.060667 0.440240 11.00000 -1.50000 H78C 2 0.470356 0.145179 0.453309 11.00000 -1.50000 HKLF 4 REM _MUA1942 REM R1 = 0.0774 for 20540 Fo > 4sig(Fo) and 0.0865 for all 24448 data REM 1276 parameters refined using 73 restraints END WGHT 0.1169 89.7783 REM Highest difference peak 10.511, deepest hole -2.991, 1-sigma level 0.283 Q1 1 0.9032 0.1746 0.4271 11.00000 0.05 10.51 Q2 1 0.3475 0.1766 0.4240 11.00000 0.05 9.41 Q3 1 0.1265 0.1814 0.4234 11.00000 0.05 9.22 Q4 1 0.4637 -0.0204 0.0636 11.00000 0.05 8.14 Q5 1 0.2233 0.9784 0.0665 11.00000 0.05 7.59 Q6 1 0.2830 0.9806 0.4487 11.00000 0.05 6.90 Q7 1 1.0475 -0.0195 0.4505 11.00000 0.05 6.81 Q8 1 1.0854 0.1734 0.0431 11.00000 0.05 4.20 Q9 1 0.5261 0.1725 0.0402 11.00000 0.05 4.14 Q10 1 1.3054 0.1830 0.0416 11.00000 0.05 3.62 Q11 1 0.4197 0.9797 0.2550 11.00000 0.05 2.23 Q12 1 0.0939 0.9805 0.2505 11.00000 0.05 2.18 Q13 1 1.0158 -0.2054 0.2758 11.00000 0.05 1.85 Q14 1 0.3812 0.7957 0.0823 11.00000 0.05 1.83 Q15 1 0.7031 0.1167 0.2711 11.00000 0.05 1.79 Q16 1 0.5980 -0.0279 0.2884 11.00000 0.05 1.72 Q17 1 0.6750 0.1768 0.2678 11.00000 0.05 1.71 Q18 1 0.8015 0.3756 0.1952 11.00000 0.05 1.47 Q19 1 0.5796 0.3733 0.1992 11.00000 0.05 1.43 Q20 1 0.4524 0.1691 0.2680 11.00000 0.05 1.43 Q21 1 0.9802 0.3710 0.3954 11.00000 0.05 1.42 Q22 1 0.9052 -0.0111 0.2097 11.00000 0.05 1.37 Q23 1 1.0782 -0.3528 0.3710 11.00000 0.05 1.36 Q24 1 0.6720 -0.0105 0.2015 11.00000 0.05 1.33 Q25 1 0.7432 -0.2137 0.3125 11.00000 0.05 1.25 ; data_3 _database_code_depnum_ccdc_archive 'CCDC 910740' #TrackingRef 'Revised_Ln6_Combined_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (Et3NH)(Dy6(L4)6(OAc)6)*9CH3OH*7H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H150 Dy6 N19 O53' _chemical_formula_weight 3357.32 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.7380(17) _cell_length_b 18.4019(17) _cell_length_c 20.0747(19) _cell_angle_alpha 79.4810(10) _cell_angle_beta 68.9180(10) _cell_angle_gamma 76.3060(10) _cell_volume 5905.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 9954 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 29.49 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3322 _exptl_absorpt_coefficient_mu 3.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4585 _exptl_absorpt_correction_T_max 0.5960 _exptl_absorpt_process_details SADABS _exptl_special_details ? _diffrn_ambient_temperature 188(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46829 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.05 _reflns_number_total 20819 _reflns_number_gt 15605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The solvent electron density was modeled using PLATON/SQUEEZE (ver. 01-02-13), which located a potential solvent volume of 1072 \%A3 and an electron count of 427 electrons/cell, consistent with 16 CH3OH and 14 H2O molecules/cell. Sixteen methanol molecules and 14 water molecules were added to the content of the unit cell during the final refinement to properly calculate the crystal data ; _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^)+(0.1153P)^2^+49.6945P] 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 20819 _refine_ls_number_parameters 1357 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1472 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 0.765 _refine_ls_restrained_S_all 0.766 _refine_ls_shift/su_max 2.405 _refine_ls_shift/su_mean 0.014 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 0.49361(2) 0.67569(2) 0.23462(2) 0.02815(11) Uani 1 1 d . . . Dy2 Dy 0.71263(2) 0.68296(2) 0.23166(2) 0.02466(10) Uani 1 1 d . . . Dy3 Dy 0.63580(2) 0.48255(2) 0.249990(19) 0.02304(10) Uani 1 1 d . . . Dy4 Dy 0.93358(2) 0.67383(2) 0.232168(19) 0.02365(10) Uani 1 1 d . . . Dy5 Dy 0.87017(2) 0.48102(2) 0.249606(19) 0.02181(10) Uani 1 1 d . . . Dy6 Dy 0.79046(2) 0.29742(2) 0.26616(2) 0.02801(11) Uani 1 1 d . . . O1 O 0.7378(3) 0.5494(3) 0.2456(3) 0.0304(13) Uani 1 1 d . . . O2 O 0.7980(3) 0.6545(3) 0.3081(3) 0.0264(12) Uani 1 1 d . . . O3 O 0.7953(4) 0.5339(4) 0.3634(3) 0.0455(16) Uani 1 1 d . . . O4 O 0.5573(3) 0.5902(3) 0.3127(3) 0.0301(13) Uani 1 1 d . . . O5 O 0.6322(4) 0.6414(4) 0.3564(4) 0.0482(17) Uani 1 1 d . . . O6 O 0.6451(4) 0.4657(4) 0.3709(3) 0.0478(17) Uani 1 1 d . . . O7 O 0.7758(3) 0.4013(3) 0.3298(3) 0.0284(12) Uani 1 1 d . . . O8 O 0.7627(3) 0.4046(3) 0.1848(3) 0.0276(12) Uani 1 1 d . . . O9 O 0.8667(3) 0.4674(3) 0.1316(3) 0.0309(13) Uani 1 1 d . . . O10 O 0.8107(3) 0.6431(3) 0.1148(3) 0.0315(13) Uani 1 1 d . . . O11 O 0.9035(3) 0.5912(3) 0.1687(3) 0.0254(12) Uani 1 1 d . . . O12 O 0.6377(3) 0.6552(3) 0.1620(3) 0.0295(12) Uani 1 1 d . . . O13 O 0.6877(3) 0.5400(3) 0.1268(3) 0.0334(13) Uani 1 1 d . . . O14 O 0.6320(5) 0.1650(4) 0.2039(5) 0.067(2) Uani 1 1 d . . . O15 O 0.7431(4) 0.2331(3) 0.2107(3) 0.0420(15) Uani 1 1 d . . . O16 O 0.9065(3) 0.3545(3) 0.2277(3) 0.0268(12) Uani 1 1 d . . . O17 O 1.0873(4) 0.4721(4) 0.1555(4) 0.0447(16) Uani 1 1 d . . . H17 H 1.0696 0.5160 0.1675 0.067 Uiso 1 1 calc R . . O18 O 1.0062(5) 0.1614(5) 0.3510(5) 0.071(3) Uani 1 1 d . . . O19 O 0.8660(4) 0.2276(4) 0.3299(4) 0.0430(15) Uani 1 1 d . . . O20 O 0.6500(3) 0.3561(3) 0.2953(3) 0.0315(13) Uani 1 1 d . . . O21 O 0.4226(3) 0.4732(4) 0.3483(4) 0.0463(17) Uani 1 1 d . . . H21 H 0.4215 0.5151 0.3233 0.069 Uiso 1 1 calc R . . O22 O 1.2081(3) 0.5442(4) 0.1726(4) 0.0433(16) Uani 1 1 d . . . O23 O 1.0641(3) 0.6289(3) 0.1775(3) 0.0328(13) Uani 1 1 d . . . O24 O 0.8249(3) 0.7452(3) 0.1912(3) 0.0269(12) Uani 1 1 d . . . O25 O 0.6428(4) 0.8303(4) 0.1118(5) 0.060(2) Uani 1 1 d . . . H25 H 0.5982 0.8217 0.1427 0.089 Uiso 1 1 calc R . . O26 O 0.8576(4) 0.9286(3) 0.2777(4) 0.0444(16) Uani 1 1 d . . . O27 O 0.9138(4) 0.7832(3) 0.2745(3) 0.0392(15) Uani 1 1 d . . . O28 O 0.9502(3) 0.5461(3) 0.2796(3) 0.0266(12) Uani 1 1 d . . . O29 O 0.9528(4) 0.3321(3) 0.3618(3) 0.0362(14) Uani 1 1 d . . . H29 H 0.9354 0.3105 0.3385 0.054 Uiso 1 1 calc R . . O30 O 0.4613(7) 0.9329(5) 0.1516(8) 0.103(4) Uani 1 1 d . . . O31 O 0.4802(4) 0.7859(4) 0.1684(4) 0.0500(18) Uani 1 1 d . . . O32 O 0.5265(3) 0.5493(3) 0.2096(3) 0.0283(12) Uani 1 1 d . . . O33 O 0.6163(4) 0.3395(3) 0.1593(3) 0.0386(15) Uani 1 1 d . . . H33 H 0.6475 0.3173 0.1828 0.058 Uiso 1 1 calc R . . O34 O 0.2695(4) 0.5476(4) 0.3267(4) 0.0460(16) Uani 1 1 d . . . O35 O 0.3792(3) 0.6328(4) 0.2995(3) 0.0395(15) Uani 1 1 d . . . O36 O 0.5744(3) 0.7434(3) 0.2621(3) 0.0337(14) Uani 1 1 d . . . O37 O 0.7249(4) 0.8398(4) 0.3079(5) 0.059(2) Uani 1 1 d . . . H37A H 0.7695 0.8101 0.3056 0.089 Uiso 1 1 calc R . . O38 O 0.9709(8) 0.1241(8) 0.8254(8) 0.137(5) Uani 1 1 d . . . H38A H 0.9198 0.1395 0.8401 0.206 Uiso 1 1 calc R . . N1 N 0.9104(4) 0.2441(4) 0.1641(4) 0.0344(16) Uani 1 1 d . . . N2 N 0.9841(4) 0.2715(4) 0.1440(4) 0.0357(17) Uani 1 1 d . . . N3 N 1.0231(4) 0.4346(4) 0.1758(4) 0.0322(16) Uani 1 1 d . . . N4 N 0.6942(4) 0.2405(4) 0.3782(4) 0.0339(16) Uani 1 1 d . . . N5 N 0.6090(4) 0.2691(4) 0.3938(4) 0.0400(18) Uani 1 1 d . . . N6 N 0.5023(4) 0.4351(4) 0.3329(4) 0.0331(16) Uani 1 1 d . . . N7 N 0.9764(4) 0.7514(4) 0.1146(4) 0.0293(15) Uani 1 1 d . . . N8 N 0.9155(4) 0.7970(4) 0.0875(4) 0.0361(17) Uani 1 1 d . . . N9 N 0.7076(4) 0.7973(4) 0.1382(4) 0.0350(17) Uani 1 1 d . . . N10 N 0.9656(4) 0.6456(4) 0.3463(4) 0.0290(15) Uani 1 1 d . . . N11 N 0.9854(4) 0.5688(4) 0.3734(4) 0.0298(15) Uani 1 1 d . . . N12 N 0.9460(4) 0.4083(4) 0.3373(4) 0.0281(15) Uani 1 1 d . . . N13 N 0.4704(4) 0.6541(4) 0.1246(4) 0.0302(15) Uani 1 1 d . . . N14 N 0.4842(4) 0.5789(4) 0.1095(4) 0.0321(16) Uani 1 1 d . . . N15 N 0.5894(4) 0.4139(4) 0.1738(4) 0.0307(16) Uani 1 1 d . . . N16 N 0.4191(4) 0.7565(4) 0.3340(4) 0.0383(18) Uani 1 1 d . . . N17 N 0.4619(4) 0.8049(4) 0.3476(5) 0.046(2) Uani 1 1 d . . . N18 N 0.6713(4) 0.8025(4) 0.2968(4) 0.0380(18) Uani 1 1 d . . . N19 N 0.8319(12) 0.1323(11) 0.7916(10) 0.156(8) Uani 1 1 d D . . H19 H 0.8871 0.1202 0.7882 0.188 Uiso 1 1 calc R . . C1 C 0.7842(6) 0.6065(6) 0.3649(5) 0.044(2) Uani 1 1 d . . . C2 C 0.7555(5) 0.6400(6) 0.4354(5) 0.046(2) Uani 1 1 d . . . H2A H 0.7344 0.6025 0.4751 0.069 Uiso 1 1 calc R . . H2B H 0.7118 0.6840 0.4353 0.069 Uiso 1 1 calc R . . H2C H 0.8018 0.6553 0.4414 0.069 Uiso 1 1 calc R . . C3 C 0.5704(5) 0.6093(6) 0.3661(5) 0.040(2) Uani 1 1 d . . . C4 C 0.5079(5) 0.5993(6) 0.4394(5) 0.043(2) Uani 1 1 d . . . H4A H 0.5356 0.5861 0.4755 0.065 Uiso 1 1 calc R . . H4B H 0.4794 0.5590 0.4414 0.065 Uiso 1 1 calc R . . H4C H 0.4680 0.6463 0.4491 0.065 Uiso 1 1 calc R . . C5 C 0.7108(5) 0.4260(5) 0.3818(5) 0.039(2) Uani 1 1 d . . . C6 C 0.7148(5) 0.4041(6) 0.4564(5) 0.043(2) Uani 1 1 d . . . H6A H 0.6778 0.4421 0.4876 0.064 Uiso 1 1 calc R . . H6B H 0.7712 0.4006 0.4553 0.064 Uiso 1 1 calc R . . H6C H 0.6981 0.3552 0.4750 0.064 Uiso 1 1 calc R . . C7 C 0.8180(5) 0.4296(5) 0.1286(5) 0.0327(19) Uani 1 1 d . . . C8 C 0.8229(5) 0.4106(5) 0.0572(4) 0.035(2) Uani 1 1 d . . . H8A H 0.8391 0.4521 0.0201 0.053 Uiso 1 1 calc R . . H8B H 0.7690 0.4029 0.0600 0.053 Uiso 1 1 calc R . . H8C H 0.8637 0.3646 0.0449 0.053 Uiso 1 1 calc R . . C9 C 0.8822(5) 0.6128(5) 0.1112(5) 0.0301(18) Uani 1 1 d . . . C10 C 0.9490(5) 0.5999(5) 0.0411(4) 0.038(2) Uani 1 1 d . . . H10A H 0.9293 0.5779 0.0110 0.057 Uiso 1 1 calc R . . H10B H 0.9967 0.5654 0.0497 0.057 Uiso 1 1 calc R . . H10C H 0.9648 0.6479 0.0167 0.057 Uiso 1 1 calc R . . C11 C 0.6703(5) 0.6099(5) 0.1124(4) 0.0297(18) Uani 1 1 d . . . C12 C 0.6832(5) 0.6443(5) 0.0373(5) 0.040(2) Uani 1 1 d . . . H12A H 0.7203 0.6078 0.0043 0.059 Uiso 1 1 calc R . . H12B H 0.7076 0.6890 0.0291 0.059 Uiso 1 1 calc R . . H12C H 0.6303 0.6587 0.0289 0.059 Uiso 1 1 calc R . . C13 C 0.5674(11) 0.1329(10) 0.2044(12) 0.134(8) Uani 1 1 d . . . H13A H 0.5651 0.1387 0.1556 0.201 Uiso 1 1 calc R . . H13B H 0.5153 0.1582 0.2362 0.201 Uiso 1 1 calc R . . H13C H 0.5768 0.0792 0.2217 0.201 Uiso 1 1 calc R . . C14 C 0.7097(7) 0.1396(5) 0.1657(6) 0.049(3) Uani 1 1 d . . . C15 C 0.7365(9) 0.0822(7) 0.1211(7) 0.069(3) Uani 1 1 d . . . H15 H 0.6969 0.0578 0.1172 0.083 Uiso 1 1 calc R . . C16 C 0.8195(9) 0.0592(7) 0.0817(7) 0.071(4) Uani 1 1 d . . . H16 H 0.8358 0.0189 0.0529 0.085 Uiso 1 1 calc R . . C17 C 0.8772(8) 0.0959(6) 0.0852(6) 0.058(3) Uani 1 1 d . . . H17A H 0.9335 0.0817 0.0578 0.069 Uiso 1 1 calc R . . C18 C 0.8525(6) 0.1549(5) 0.1299(5) 0.039(2) Uani 1 1 d . . . C19 C 0.7690(6) 0.1786(5) 0.1697(5) 0.041(2) Uani 1 1 d . . . C20 C 0.9173(6) 0.1912(5) 0.1262(5) 0.041(2) Uani 1 1 d . . . H20 H 0.9701 0.1751 0.0929 0.049 Uiso 1 1 calc R . . C21 C 0.9743(5) 0.3279(5) 0.1780(4) 0.0298(18) Uani 1 1 d . . . C22 C 1.0440(5) 0.3678(5) 0.1558(4) 0.0332(19) Uani 1 1 d . . . C23 C 1.1291(5) 0.3311(6) 0.1175(6) 0.053(3) Uani 1 1 d . . . H23A H 1.1484 0.3574 0.0692 0.079 Uiso 1 1 calc R . . H23B H 1.1300 0.2785 0.1140 0.079 Uiso 1 1 calc R . . H23C H 1.1652 0.3333 0.1441 0.079 Uiso 1 1 calc R . . C24 C 1.077(2) 0.1478(18) 0.3665(15) 0.245(17) Uani 1 1 d . . . H24A H 1.1111 0.1010 0.3478 0.367 Uiso 1 1 calc R . . H24B H 1.0637 0.1431 0.4186 0.367 Uiso 1 1 calc R . . H24C H 1.1062 0.1895 0.3442 0.367 Uiso 1 1 calc R . . C25 C 0.9366(7) 0.1394(6) 0.3979(6) 0.049(3) Uani 1 1 d . . . C26 C 0.9357(7) 0.0858(6) 0.4560(6) 0.051(3) Uani 1 1 d . . . H26 H 0.9858 0.0637 0.4649 0.061 Uiso 1 1 calc R . . C27 C 0.8628(7) 0.0635(5) 0.5021(5) 0.047(2) Uani 1 1 d . . . H27 H 0.8629 0.0267 0.5420 0.056 Uiso 1 1 calc R . . C28 C 0.7907(7) 0.0960(5) 0.4884(5) 0.042(2) Uani 1 1 d . . . H28 H 0.7410 0.0802 0.5186 0.051 Uiso 1 1 calc R . . C29 C 0.7891(6) 0.1520(5) 0.4309(5) 0.035(2) Uani 1 1 d . . . C30 C 0.8632(6) 0.1753(5) 0.3847(5) 0.037(2) Uani 1 1 d . . . C31 C 0.7093(6) 0.1880(5) 0.4268(5) 0.035(2) Uani 1 1 d . . . H31 H 0.6631 0.1715 0.4632 0.043 Uiso 1 1 calc R . . C32 C 0.5949(5) 0.3273(5) 0.3503(4) 0.0294(18) Uani 1 1 d . . . C33 C 0.5084(5) 0.3687(5) 0.3651(4) 0.0331(19) Uani 1 1 d . . . C34 C 0.4372(6) 0.3346(7) 0.4174(6) 0.063(3) Uani 1 1 d . . . H34A H 0.3854 0.3679 0.4166 0.095 Uiso 1 1 calc R . . H34B H 0.4405 0.3283 0.4659 0.095 Uiso 1 1 calc R . . H34C H 0.4393 0.2855 0.4038 0.095 Uiso 1 1 calc R . . C35 C 1.2816(7) 0.4906(7) 0.1623(7) 0.068(3) Uani 1 1 d . . . H35A H 1.2729 0.4488 0.2006 0.102 Uiso 1 1 calc R . . H35B H 1.3251 0.5141 0.1635 0.102 Uiso 1 1 calc R . . H35C H 1.2978 0.4716 0.1157 0.102 Uiso 1 1 calc R . . C36 C 1.2088(5) 0.6066(5) 0.1241(5) 0.035(2) Uani 1 1 d . . . C37 C 1.2798(5) 0.6283(6) 0.0734(5) 0.043(2) Uani 1 1 d . . . H37 H 1.3321 0.5994 0.0727 0.051 Uiso 1 1 calc R . . C38 C 1.2756(6) 0.6909(6) 0.0242(5) 0.043(2) Uani 1 1 d . . . H38 H 1.3242 0.7042 -0.0111 0.052 Uiso 1 1 calc R . . C39 C 1.1989(6) 0.7342(6) 0.0272(5) 0.041(2) Uani 1 1 d . . . H39 H 1.1954 0.7783 -0.0054 0.049 Uiso 1 1 calc R . . C40 C 1.1264(5) 0.7137(5) 0.0778(4) 0.0308(19) Uani 1 1 d . . . C41 C 1.1308(5) 0.6497(5) 0.1275(4) 0.0316(19) Uani 1 1 d . . . C42 C 1.0496(5) 0.7574(5) 0.0720(4) 0.0333(19) Uani 1 1 d . . . H42 H 1.0533 0.7950 0.0322 0.040 Uiso 1 1 calc R . . C43 C 0.8443(5) 0.7865(5) 0.1291(5) 0.0327(19) Uani 1 1 d . . . C44 C 0.7736(6) 0.8240(5) 0.1022(5) 0.041(2) Uani 1 1 d . . . C45 C 0.7858(8) 0.8793(7) 0.0349(7) 0.074(4) Uani 1 1 d . . . H45A H 0.7644 0.8639 0.0020 0.111 Uiso 1 1 calc R . . H45B H 0.8445 0.8801 0.0114 0.111 Uiso 1 1 calc R . . H45C H 0.7563 0.9297 0.0478 0.111 Uiso 1 1 calc R . . C46 C 0.8165(8) 1.0045(6) 0.2836(7) 0.069(4) Uani 1 1 d . . . H46A H 0.7700 1.0075 0.3286 0.104 Uiso 1 1 calc R . . H46B H 0.7962 1.0230 0.2430 0.104 Uiso 1 1 calc R . . H46C H 0.8548 1.0353 0.2832 0.104 Uiso 1 1 calc R . . C47 C 0.8810(6) 0.8924(5) 0.3338(5) 0.042(2) Uani 1 1 d . . . C48 C 0.8780(8) 0.9241(6) 0.3916(6) 0.060(3) Uani 1 1 d . . . H48 H 0.8581 0.9766 0.3938 0.073 Uiso 1 1 calc R . . C49 C 0.9031(9) 0.8815(7) 0.4472(7) 0.083(4) Uani 1 1 d . . . H49 H 0.9009 0.9048 0.4865 0.099 Uiso 1 1 calc R . . C50 C 0.9312(8) 0.8054(6) 0.4448(6) 0.066(4) Uani 1 1 d . . . H50 H 0.9484 0.7763 0.4828 0.079 Uiso 1 1 calc R . . C51 C 0.9349(6) 0.7702(5) 0.3869(5) 0.041(2) Uani 1 1 d . . . C52 C 0.9100(5) 0.8120(5) 0.3305(5) 0.036(2) Uani 1 1 d . . . C53 C 0.9614(5) 0.6902(5) 0.3919(5) 0.037(2) Uani 1 1 d . . . H53 H 0.9775 0.6672 0.4323 0.045 Uiso 1 1 calc R . . C54 C 0.9734(4) 0.5249(4) 0.3362(4) 0.0264(17) Uani 1 1 d . . . C55 C 0.9801(5) 0.4440(5) 0.3631(5) 0.0309(19) Uani 1 1 d . . . C56 C 1.0201(7) 0.4119(6) 0.4197(6) 0.052(3) Uani 1 1 d . . . H56A H 1.0123 0.3598 0.4361 0.078 Uiso 1 1 calc R . . H56B H 0.9948 0.4420 0.4605 0.078 Uiso 1 1 calc R . . H56C H 1.0790 0.4131 0.3994 0.078 Uiso 1 1 calc R . . C57 C 0.460(2) 0.988(2) 0.157(2) 0.29(3) Uani 1 1 d . . . H57A H 0.4732 0.9893 0.2005 0.437 Uiso 1 1 calc R . . H57B H 0.4052 1.0179 0.1618 0.437 Uiso 1 1 calc R . . H57C H 0.5008 1.0090 0.1152 0.437 Uiso 1 1 calc R . . C58 C 0.4445(7) 0.9001(6) 0.1028(7) 0.059(3) Uani 1 1 d . . . C59 C 0.4170(10) 0.9377(7) 0.0489(9) 0.093(5) Uani 1 1 d . . . H59 H 0.4098 0.9910 0.0420 0.111 Uiso 1 1 calc R . . C60 C 0.3995(14) 0.9021(8) 0.0044(11) 0.140(9) Uani 1 1 d . . . H60 H 0.3797 0.9296 -0.0327 0.168 Uiso 1 1 calc R . . C61 C 0.4115(11) 0.8244(7) 0.0147(8) 0.095(5) Uani 1 1 d . . . H61 H 0.4008 0.7987 -0.0169 0.114 Uiso 1 1 calc R . . C62 C 0.4384(7) 0.7828(5) 0.0692(6) 0.048(3) Uani 1 1 d . . . C63 C 0.4556(5) 0.8202(5) 0.1160(6) 0.041(2) Uani 1 1 d . . . C64 C 0.4526(6) 0.7004(5) 0.0747(5) 0.042(2) Uani 1 1 d . . . H64 H 0.4480 0.6793 0.0368 0.050 Uiso 1 1 calc R . . C65 C 0.5143(4) 0.5320(5) 0.1547(4) 0.0258(17) Uani 1 1 d . . . C66 C 0.5415(5) 0.4516(5) 0.1399(5) 0.0317(19) Uani 1 1 d . . . C67 C 0.5179(5) 0.4233(5) 0.0875(5) 0.040(2) Uani 1 1 d . . . H67A H 0.5662 0.3921 0.0566 0.060 Uiso 1 1 calc R . . H67B H 0.4966 0.4658 0.0580 0.060 Uiso 1 1 calc R . . H67C H 0.4754 0.3930 0.1131 0.060 Uiso 1 1 calc R . . C68 C 0.2157(7) 0.4952(7) 0.3484(7) 0.068(4) Uani 1 1 d . . . H68A H 0.1984 0.4836 0.4007 0.102 Uiso 1 1 calc R . . H68B H 0.2443 0.4490 0.3256 0.102 Uiso 1 1 calc R . . H68C H 0.1672 0.5169 0.3337 0.102 Uiso 1 1 calc R . . C69 C 0.2438(5) 0.6112(5) 0.3612(5) 0.040(2) Uani 1 1 d . . . C70 C 0.1661(6) 0.6319(7) 0.4090(6) 0.056(3) Uani 1 1 d . . . H70 H 0.1274 0.5999 0.4200 0.067 Uiso 1 1 calc R . . C71 C 0.1427(7) 0.6966(6) 0.4413(6) 0.061(3) Uani 1 1 d . . . H71 H 0.0877 0.7121 0.4711 0.073 Uiso 1 1 calc R . . C72 C 0.2052(5) 0.7403(6) 0.4283(5) 0.042(2) Uani 1 1 d . . . H72 H 0.1920 0.7838 0.4524 0.050 Uiso 1 1 calc R . . C73 C 0.2849(5) 0.7200(5) 0.3807(5) 0.0325(19) Uani 1 1 d . . . C74 C 0.3060(5) 0.6541(5) 0.3457(5) 0.034(2) Uani 1 1 d . . . C75 C 0.3446(5) 0.7657(5) 0.3743(5) 0.034(2) Uani 1 1 d . . . H75 H 0.3258 0.8062 0.4031 0.041 Uiso 1 1 calc R . . C76 C 0.5407(5) 0.7910(5) 0.3096(5) 0.0334(19) Uani 1 1 d . . . C77 C 0.5964(6) 0.8317(6) 0.3224(6) 0.051(3) Uani 1 1 d . . . C78 C 0.5627(8) 0.8990(8) 0.3645(9) 0.099(6) Uani 1 1 d . . . H78A H 0.6067 0.9266 0.3562 0.149 Uiso 1 1 calc R . . H78B H 0.5406 0.8821 0.4157 0.149 Uiso 1 1 calc R . . H78C H 0.5187 0.9320 0.3487 0.149 Uiso 1 1 calc R . . C79 C 0.7882(13) 0.2289(10) 0.7903(9) 0.116(6) Uani 1 1 d D . . H79A H 0.7416 0.2388 0.7718 0.139 Uiso 1 1 calc R . . H79B H 0.7668 0.2435 0.8397 0.139 Uiso 1 1 calc R . . C80 C 0.8506(14) 0.2750(16) 0.7439(14) 0.215(15) Uani 1 1 d D . . H80A H 0.8252 0.3285 0.7437 0.322 Uiso 1 1 calc R . . H80B H 0.8713 0.2610 0.6948 0.322 Uiso 1 1 calc R . . H80C H 0.8963 0.2659 0.7627 0.322 Uiso 1 1 calc R . . C81 C 0.809(2) 0.105(2) 0.7255(19) 0.53(7) Uani 1 1 d D . . H81A H 0.7789 0.0630 0.7406 0.635 Uiso 1 1 calc R . . H81B H 0.7845 0.1469 0.6964 0.635 Uiso 1 1 calc R . . C82 C 0.9020(19) 0.083(3) 0.695(2) 0.28(3) Uani 1 1 d D . . H82A H 0.9173 0.0603 0.6506 0.419 Uiso 1 1 calc R . . H82B H 0.9217 0.0460 0.7303 0.419 Uiso 1 1 calc R . . H82C H 0.9270 0.1273 0.6859 0.419 Uiso 1 1 calc R . . C83 C 0.766(2) 0.108(2) 0.8709(19) 0.47(5) Uani 1 1 d D . . H83A H 0.7736 0.1223 0.9127 0.560 Uiso 1 1 calc R . . H83B H 0.7073 0.1201 0.8737 0.560 Uiso 1 1 calc R . . C84 C 0.810(4) 0.029(3) 0.851(4) 0.62(7) Uani 1 1 d D . . H84A H 0.7894 -0.0086 0.8909 0.932 Uiso 1 1 calc R . . H84B H 0.8695 0.0245 0.8406 0.932 Uiso 1 1 calc R . . H84C H 0.8008 0.0197 0.8082 0.932 Uiso 1 1 calc R . . C85 C 0.991(2) 0.0621(11) 0.8708(13) 0.26(2) Uani 1 1 d . . . H85A H 0.9508 0.0294 0.8841 0.387 Uiso 1 1 calc R . . H85B H 0.9920 0.0790 0.9141 0.387 Uiso 1 1 calc R . . H85C H 1.0460 0.0342 0.8461 0.387 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 0.02022(19) 0.0329(2) 0.0350(2) -0.01691(17) -0.00982(16) -0.00066(15) Dy2 0.02118(19) 0.0272(2) 0.0296(2) -0.00954(16) -0.01076(16) -0.00340(15) Dy3 0.01765(18) 0.0281(2) 0.0245(2) -0.00873(15) -0.00501(15) -0.00503(14) Dy4 0.02105(19) 0.0284(2) 0.0240(2) -0.00323(15) -0.00862(15) -0.00725(15) Dy5 0.01784(18) 0.0255(2) 0.02201(19) -0.00423(15) -0.00515(14) -0.00483(14) Dy6 0.0259(2) 0.0273(2) 0.0312(2) -0.00460(16) -0.00870(16) -0.00565(15) O1 0.022(3) 0.017(3) 0.056(4) -0.004(3) -0.017(3) -0.006(2) O2 0.019(3) 0.035(3) 0.027(3) -0.005(2) -0.008(2) -0.005(2) O3 0.032(3) 0.066(5) 0.036(4) -0.015(3) -0.009(3) 0.001(3) O4 0.027(3) 0.035(3) 0.034(3) -0.015(3) -0.012(2) -0.004(2) O5 0.050(4) 0.045(4) 0.044(4) -0.016(3) -0.011(3) 0.002(3) O6 0.052(4) 0.062(5) 0.037(4) -0.002(3) -0.015(3) -0.028(4) O7 0.020(3) 0.030(3) 0.032(3) -0.015(2) 0.003(2) -0.009(2) O8 0.022(3) 0.031(3) 0.023(3) -0.005(2) -0.001(2) -0.003(2) O9 0.026(3) 0.037(3) 0.029(3) -0.008(3) -0.006(2) -0.007(2) O10 0.031(3) 0.032(3) 0.034(3) -0.006(3) -0.012(3) -0.007(2) O11 0.026(3) 0.034(3) 0.019(3) 0.000(2) -0.012(2) -0.008(2) O12 0.025(3) 0.033(3) 0.034(3) -0.015(3) -0.006(2) -0.009(2) O13 0.028(3) 0.044(4) 0.030(3) -0.012(3) -0.005(3) -0.012(3) O14 0.054(5) 0.062(5) 0.105(7) -0.021(5) -0.034(5) -0.026(4) O15 0.040(4) 0.041(4) 0.050(4) -0.011(3) -0.014(3) -0.013(3) O16 0.021(3) 0.032(3) 0.025(3) -0.006(2) -0.003(2) -0.006(2) O17 0.028(3) 0.044(4) 0.061(4) -0.007(3) -0.005(3) -0.018(3) O18 0.043(5) 0.072(6) 0.101(7) 0.005(5) -0.034(5) -0.011(4) O19 0.035(3) 0.043(4) 0.050(4) 0.004(3) -0.018(3) -0.007(3) O20 0.023(3) 0.035(3) 0.033(3) -0.002(3) -0.005(2) -0.007(2) O21 0.018(3) 0.049(4) 0.064(5) -0.013(3) -0.003(3) -0.002(3) O22 0.023(3) 0.047(4) 0.053(4) 0.002(3) -0.011(3) -0.002(3) O23 0.022(3) 0.041(3) 0.033(3) 0.004(3) -0.009(2) -0.005(2) O24 0.030(3) 0.031(3) 0.027(3) -0.004(2) -0.018(2) -0.005(2) O25 0.050(4) 0.046(4) 0.102(6) 0.019(4) -0.056(5) -0.016(3) O26 0.056(4) 0.036(4) 0.050(4) -0.007(3) -0.028(3) -0.005(3) O27 0.055(4) 0.034(3) 0.039(4) -0.009(3) -0.026(3) -0.007(3) O28 0.028(3) 0.027(3) 0.027(3) 0.001(2) -0.012(2) -0.008(2) O29 0.047(4) 0.027(3) 0.041(4) 0.006(3) -0.025(3) -0.010(3) O30 0.114(8) 0.055(6) 0.190(12) -0.046(7) -0.102(9) -0.001(5) O31 0.069(5) 0.034(4) 0.064(5) -0.014(3) -0.042(4) -0.003(3) O32 0.025(3) 0.036(3) 0.029(3) -0.018(2) -0.010(2) -0.003(2) O33 0.042(4) 0.029(3) 0.048(4) -0.015(3) -0.018(3) -0.001(3) O34 0.026(3) 0.051(4) 0.065(5) -0.023(3) -0.010(3) -0.011(3) O35 0.023(3) 0.048(4) 0.050(4) -0.023(3) -0.007(3) -0.007(3) O36 0.026(3) 0.034(3) 0.044(4) -0.022(3) -0.011(3) 0.001(2) O37 0.033(4) 0.064(5) 0.103(6) -0.053(5) -0.031(4) -0.004(3) O38 0.093(10) 0.155(12) 0.125(11) 0.023(9) -0.015(8) -0.013(8) N1 0.040(4) 0.032(4) 0.033(4) -0.014(3) -0.011(3) -0.002(3) N2 0.026(4) 0.039(4) 0.039(4) -0.017(3) -0.001(3) -0.005(3) N3 0.021(3) 0.041(4) 0.034(4) -0.006(3) -0.008(3) -0.004(3) N4 0.031(4) 0.036(4) 0.036(4) -0.002(3) -0.012(3) -0.011(3) N5 0.034(4) 0.039(4) 0.039(4) -0.001(4) -0.001(3) -0.011(3) N6 0.024(4) 0.043(4) 0.036(4) -0.009(3) -0.009(3) -0.010(3) N7 0.031(4) 0.028(4) 0.032(4) -0.003(3) -0.012(3) -0.009(3) N8 0.039(4) 0.033(4) 0.041(4) 0.001(3) -0.017(4) -0.012(3) N9 0.034(4) 0.025(4) 0.056(5) -0.003(3) -0.028(4) -0.003(3) N10 0.030(4) 0.034(4) 0.029(4) -0.001(3) -0.013(3) -0.012(3) N11 0.026(4) 0.032(4) 0.035(4) -0.006(3) -0.016(3) -0.003(3) N12 0.026(3) 0.027(4) 0.032(4) -0.001(3) -0.010(3) -0.009(3) N13 0.029(4) 0.032(4) 0.034(4) -0.006(3) -0.015(3) -0.005(3) N14 0.023(3) 0.037(4) 0.043(4) -0.016(3) -0.016(3) -0.002(3) N15 0.021(3) 0.033(4) 0.041(4) -0.016(3) -0.011(3) -0.001(3) N16 0.030(4) 0.045(5) 0.046(5) -0.025(4) -0.014(3) -0.001(3) N17 0.031(4) 0.046(5) 0.069(6) -0.037(4) -0.020(4) 0.005(3) N18 0.033(4) 0.036(4) 0.054(5) -0.025(4) -0.018(4) -0.006(3) N19 0.166(18) 0.22(2) 0.112(13) 0.016(14) -0.043(13) -0.127(17) C1 0.032(5) 0.058(7) 0.047(6) -0.013(5) -0.013(4) -0.010(5) C2 0.029(5) 0.080(7) 0.030(5) -0.020(5) -0.006(4) -0.009(5) C3 0.019(4) 0.062(6) 0.041(5) -0.017(5) -0.007(4) -0.005(4) C4 0.028(5) 0.066(7) 0.037(5) -0.020(5) -0.002(4) -0.015(4) C5 0.031(5) 0.036(5) 0.048(6) -0.007(4) -0.013(4) -0.002(4) C6 0.030(5) 0.060(6) 0.036(5) -0.006(4) -0.010(4) -0.006(4) C7 0.027(4) 0.033(5) 0.035(5) -0.010(4) -0.008(4) 0.001(4) C8 0.032(5) 0.051(6) 0.021(4) -0.008(4) -0.005(4) -0.010(4) C9 0.030(5) 0.025(4) 0.034(5) -0.006(4) -0.006(4) -0.008(3) C10 0.032(5) 0.051(6) 0.022(4) -0.008(4) -0.001(4) 0.000(4) C11 0.023(4) 0.036(5) 0.032(5) -0.006(4) -0.006(4) -0.011(4) C12 0.035(5) 0.050(6) 0.030(5) -0.001(4) -0.007(4) -0.009(4) C13 0.115(14) 0.114(14) 0.23(2) -0.062(15) -0.106(16) -0.021(11) C14 0.058(7) 0.035(5) 0.066(7) -0.008(5) -0.038(6) -0.003(5) C15 0.088(10) 0.062(8) 0.081(9) -0.013(7) -0.046(8) -0.028(7) C16 0.107(11) 0.056(7) 0.068(8) -0.023(6) -0.042(8) -0.016(7) C17 0.069(7) 0.047(6) 0.065(7) -0.019(5) -0.025(6) -0.012(5) C18 0.055(6) 0.025(5) 0.047(6) -0.006(4) -0.033(5) -0.001(4) C19 0.061(6) 0.029(5) 0.046(6) -0.001(4) -0.032(5) -0.011(4) C20 0.046(5) 0.036(5) 0.040(5) -0.006(4) -0.019(4) 0.002(4) C21 0.025(4) 0.032(5) 0.029(4) -0.011(4) -0.006(3) 0.002(3) C22 0.029(4) 0.039(5) 0.028(4) -0.010(4) -0.003(4) -0.004(4) C23 0.023(5) 0.063(7) 0.065(7) -0.029(6) 0.005(5) -0.007(4) C24 0.36(6) 0.21(3) 0.14(2) -0.01(2) -0.06(3) -0.05(3) C25 0.054(6) 0.048(6) 0.049(6) -0.006(5) -0.030(5) 0.004(5) C26 0.066(7) 0.043(6) 0.050(6) -0.005(5) -0.036(6) 0.003(5) C27 0.076(7) 0.035(5) 0.038(5) -0.002(4) -0.033(5) -0.005(5) C28 0.071(7) 0.025(5) 0.034(5) -0.007(4) -0.019(5) -0.008(4) C29 0.048(5) 0.025(4) 0.035(5) -0.001(4) -0.018(4) -0.006(4) C30 0.051(6) 0.031(5) 0.034(5) -0.006(4) -0.023(4) -0.004(4) C31 0.045(5) 0.035(5) 0.028(5) 0.002(4) -0.013(4) -0.013(4) C32 0.028(4) 0.035(5) 0.026(4) 0.001(4) -0.006(4) -0.014(4) C33 0.028(4) 0.043(5) 0.025(4) 0.001(4) -0.005(4) -0.013(4) C34 0.031(5) 0.078(8) 0.070(8) 0.007(6) -0.004(5) -0.022(5) C35 0.048(7) 0.056(7) 0.087(9) -0.004(6) -0.025(6) 0.016(5) C36 0.026(4) 0.044(5) 0.038(5) -0.015(4) -0.007(4) -0.010(4) C37 0.023(4) 0.063(7) 0.043(5) -0.014(5) -0.002(4) -0.015(4) C38 0.033(5) 0.059(6) 0.033(5) -0.013(5) 0.003(4) -0.014(4) C39 0.044(5) 0.052(6) 0.027(5) -0.007(4) -0.006(4) -0.019(5) C40 0.030(4) 0.046(5) 0.023(4) -0.013(4) -0.008(3) -0.014(4) C41 0.026(4) 0.040(5) 0.029(4) -0.011(4) -0.003(4) -0.011(4) C42 0.039(5) 0.043(5) 0.025(4) 0.000(4) -0.009(4) -0.024(4) C43 0.039(5) 0.029(4) 0.040(5) -0.004(4) -0.023(4) -0.008(4) C44 0.040(5) 0.028(5) 0.060(6) 0.003(4) -0.027(5) -0.007(4) C45 0.078(8) 0.066(8) 0.104(10) 0.043(7) -0.064(8) -0.048(7) C46 0.091(9) 0.050(7) 0.073(8) -0.015(6) -0.047(7) 0.016(6) C47 0.038(5) 0.045(6) 0.048(6) -0.012(5) -0.012(4) -0.018(4) C48 0.089(9) 0.042(6) 0.068(8) -0.018(5) -0.051(7) 0.002(6) C49 0.130(13) 0.065(8) 0.078(9) -0.033(7) -0.068(9) 0.008(8) C50 0.107(10) 0.049(7) 0.069(8) -0.022(6) -0.070(8) 0.010(6) C51 0.047(5) 0.042(5) 0.042(5) -0.008(4) -0.023(5) -0.009(4) C52 0.036(5) 0.039(5) 0.045(5) -0.014(4) -0.022(4) -0.008(4) C53 0.040(5) 0.037(5) 0.039(5) -0.008(4) -0.020(4) -0.002(4) C54 0.016(4) 0.029(4) 0.033(5) 0.003(3) -0.008(3) -0.005(3) C55 0.026(4) 0.032(5) 0.039(5) 0.003(4) -0.019(4) -0.004(3) C56 0.056(6) 0.051(6) 0.066(7) 0.009(5) -0.042(6) -0.016(5) C57 0.23(4) 0.36(6) 0.39(5) -0.26(5) -0.19(4) 0.04(4) C58 0.057(7) 0.041(6) 0.095(9) 0.002(6) -0.046(7) -0.014(5) C59 0.126(13) 0.048(7) 0.139(14) 0.008(8) -0.088(12) -0.025(8) C60 0.26(3) 0.059(9) 0.19(2) 0.018(11) -0.17(2) -0.062(12) C61 0.174(16) 0.054(8) 0.111(12) 0.023(7) -0.118(12) -0.034(9) C62 0.067(7) 0.040(6) 0.058(6) 0.002(5) -0.039(6) -0.026(5) C63 0.033(5) 0.034(5) 0.061(6) -0.001(4) -0.025(5) -0.007(4) C64 0.043(5) 0.050(6) 0.040(5) -0.012(5) -0.018(4) -0.012(4) C65 0.017(4) 0.035(4) 0.028(4) -0.017(4) -0.004(3) -0.005(3) C66 0.028(4) 0.036(5) 0.036(5) -0.011(4) -0.010(4) -0.013(4) C67 0.036(5) 0.038(5) 0.056(6) -0.023(4) -0.024(4) 0.004(4) C68 0.049(7) 0.060(7) 0.094(10) -0.026(7) -0.005(6) -0.026(6) C69 0.020(4) 0.047(6) 0.054(6) -0.017(5) -0.013(4) 0.002(4) C70 0.024(5) 0.075(8) 0.068(7) -0.033(6) -0.004(5) -0.006(5) C71 0.067(7) 0.043(6) 0.042(6) -0.005(5) 0.006(5) 0.012(5) C72 0.020(4) 0.057(6) 0.048(6) -0.027(5) -0.007(4) 0.002(4) C73 0.024(4) 0.039(5) 0.035(5) -0.014(4) -0.012(4) 0.004(4) C74 0.019(4) 0.048(5) 0.030(5) -0.010(4) -0.005(3) -0.002(4) C75 0.026(4) 0.040(5) 0.037(5) -0.024(4) -0.015(4) 0.012(4) C76 0.034(5) 0.029(5) 0.043(5) -0.015(4) -0.019(4) 0.001(4) C77 0.039(5) 0.044(6) 0.085(8) -0.052(6) -0.027(5) 0.010(4) C78 0.055(8) 0.107(11) 0.157(15) -0.111(11) -0.030(9) 0.012(7) C79 0.18(2) 0.097(13) 0.081(11) -0.006(10) -0.037(12) -0.051(13) C80 0.15(2) 0.28(4) 0.16(2) 0.04(2) -0.06(2) 0.03(2) C81 1.07(19) 0.10(3) 0.20(4) -0.01(3) -0.03(8) -0.01(6) C82 0.17(3) 0.38(7) 0.23(5) 0.09(4) -0.04(3) -0.09(4) C83 0.10(2) 0.37(6) 0.87(14) -0.35(8) 0.08(5) -0.10(3) C84 0.26(7) 0.93(19) 0.50(11) -0.19(13) 0.12(7) -0.09(10) C85 0.44(5) 0.070(14) 0.14(2) 0.055(14) -0.03(3) 0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O35 2.218(6) . ? Dy1 O31 2.225(7) . ? Dy1 O36 2.362(5) . ? Dy1 O32 2.362(5) . ? Dy1 O4 2.396(6) . ? Dy1 O12 2.422(5) . ? Dy1 N16 2.489(7) . ? Dy1 N13 2.502(7) . ? Dy2 O36 2.345(5) . ? Dy2 O24 2.348(5) . ? Dy2 O1 2.374(5) . ? Dy2 O12 2.429(5) . ? Dy2 O2 2.434(5) . ? Dy2 O5 2.477(7) . ? Dy2 O10 2.481(6) . ? Dy2 N9 2.558(7) . ? Dy2 N18 2.585(7) . ? Dy3 O20 2.329(6) . ? Dy3 O32 2.359(5) . ? Dy3 O1 2.387(5) . ? Dy3 O4 2.408(5) . ? Dy3 O8 2.423(5) . ? Dy3 O13 2.439(6) . ? Dy3 O6 2.451(6) . ? Dy3 N15 2.591(6) . ? Dy3 N6 2.599(7) . ? Dy4 O23 2.201(5) . ? Dy4 O27 2.230(6) . ? Dy4 O28 2.361(5) . ? Dy4 O24 2.379(5) . ? Dy4 O11 2.408(5) . ? Dy4 O2 2.409(5) . ? Dy4 N7 2.486(7) . ? Dy4 N10 2.490(6) . ? Dy5 O16 2.343(5) . ? Dy5 O28 2.345(5) . ? Dy5 O11 2.402(5) . ? Dy5 O1 2.408(5) . ? Dy5 O7 2.430(5) . ? Dy5 O3 2.439(6) . ? Dy5 O9 2.451(5) . ? Dy5 N12 2.586(7) . ? Dy5 N3 2.599(7) . ? Dy6 O19 2.214(6) . ? Dy6 O15 2.230(6) . ? Dy6 O16 2.349(5) . ? Dy6 O20 2.371(5) . ? Dy6 O8 2.398(5) . ? Dy6 O7 2.403(5) . ? Dy6 N4 2.509(7) . ? Dy6 N1 2.510(7) . ? O2 C1 1.295(12) . ? O3 C1 1.308(12) . ? O4 C3 1.296(10) . ? O5 C3 1.303(11) . ? O6 C5 1.289(11) . ? O7 C5 1.297(10) . ? O8 C7 1.295(10) . ? O9 C7 1.252(10) . ? O10 C9 1.240(10) . ? O11 C9 1.308(10) . ? O12 C11 1.298(10) . ? O13 C11 1.254(10) . ? O14 C14 1.331(13) . ? O14 C13 1.405(15) . ? O15 C19 1.306(11) . ? O16 C21 1.311(9) . ? O17 N3 1.369(9) . ? O17 H17 0.8400 . ? O18 C24 1.35(4) . ? O18 C25 1.355(14) . ? O19 C30 1.317(11) . ? O20 C32 1.308(9) . ? O21 N6 1.371(9) . ? O21 H21 0.8400 . ? O22 C36 1.363(11) . ? O22 C35 1.409(11) . ? O23 C41 1.332(10) . ? O24 C43 1.312(10) . ? O25 N9 1.400(9) . ? O25 H25 0.8400 . ? O26 C47 1.347(11) . ? O26 C46 1.418(12) . ? O27 C52 1.301(10) . ? O28 C54 1.307(9) . ? O29 N12 1.390(8) . ? O29 H29 0.8400 . ? O30 C57 1.04(3) . ? O30 C58 1.388(14) . ? O31 C63 1.286(11) . ? O32 C65 1.302(9) . ? O33 N15 1.387(9) . ? O33 H33 0.8400 . ? O34 C69 1.368(11) . ? O34 C68 1.420(12) . ? O35 C74 1.313(10) . ? O36 C76 1.296(10) . ? O37 N18 1.394(9) . ? O37 H37A 0.8400 . ? O38 C85 1.39(2) . ? O38 H38A 0.8770 . ? N1 C20 1.299(11) . ? N1 N2 1.410(10) . ? N2 C21 1.289(10) . ? N3 C22 1.292(11) . ? N4 C31 1.295(11) . ? N4 N5 1.415(10) . ? N5 C32 1.289(11) . ? N6 C33 1.274(11) . ? N7 C42 1.289(10) . ? N7 N8 1.413(10) . ? N8 C43 1.275(11) . ? N9 C44 1.292(12) . ? N10 C53 1.308(11) . ? N10 N11 1.428(9) . ? N11 C54 1.292(10) . ? N12 C55 1.266(10) . ? N13 C64 1.273(11) . ? N13 N14 1.416(9) . ? N14 C65 1.304(11) . ? N15 C66 1.277(11) . ? N16 C75 1.267(11) . ? N16 N17 1.414(10) . ? N17 C76 1.318(11) . ? N18 C77 1.260(11) . ? N19 C83 1.66(2) . ? N19 C81 1.700(19) . ? N19 C79 1.764(17) . ? N19 H19 0.9300 . ? C1 C2 1.515(13) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.500(12) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.502(13) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.505(11) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.493(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.482(12) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.395(15) . ? C14 C19 1.438(13) . ? C15 C16 1.400(18) . ? C15 H15 0.9500 . ? C16 C17 1.381(16) . ? C16 H16 0.9500 . ? C17 C18 1.422(13) . ? C17 H17A 0.9500 . ? C18 C19 1.411(14) . ? C18 C20 1.433(13) . ? C20 H20 0.9500 . ? C21 C22 1.476(12) . ? C22 C23 1.483(12) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.382(14) . ? C25 C30 1.407(13) . ? C26 C27 1.396(15) . ? C26 H26 0.9500 . ? C27 C28 1.378(14) . ? C27 H27 0.9500 . ? C28 C29 1.404(12) . ? C28 H28 0.9500 . ? C29 C30 1.419(13) . ? C29 C31 1.440(12) . ? C31 H31 0.9500 . ? C32 C33 1.490(12) . ? C33 C34 1.509(12) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.396(12) . ? C36 C41 1.407(12) . ? C37 C38 1.380(14) . ? C37 H37 0.9500 . ? C38 C39 1.391(13) . ? C38 H38 0.9500 . ? C39 C40 1.406(12) . ? C39 H39 0.9500 . ? C40 C41 1.405(12) . ? C40 C42 1.440(12) . ? C42 H42 0.9500 . ? C43 C44 1.509(12) . ? C44 C45 1.517(14) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.369(13) . ? C47 C52 1.454(13) . ? C48 C49 1.390(16) . ? C48 H48 0.9500 . ? C49 C50 1.373(16) . ? C49 H49 0.9500 . ? C50 C51 1.405(13) . ? C50 H50 0.9500 . ? C51 C52 1.397(13) . ? C51 C53 1.432(13) . ? C53 H53 0.9500 . ? C54 C55 1.481(11) . ? C55 C56 1.511(12) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.353(17) . ? C58 C63 1.424(13) . ? C59 C60 1.354(19) . ? C59 H59 0.9500 . ? C60 C61 1.382(18) . ? C60 H60 0.9500 . ? C61 C62 1.382(14) . ? C61 H61 0.9500 . ? C62 C63 1.411(13) . ? C62 C64 1.467(13) . ? C64 H64 0.9500 . ? C65 C66 1.494(11) . ? C66 C67 1.473(11) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.379(12) . ? C69 C74 1.418(12) . ? C70 C71 1.366(14) . ? C70 H70 0.9500 . ? C71 C72 1.443(15) . ? C71 H71 0.9500 . ? C72 C73 1.399(11) . ? C72 H72 0.9500 . ? C73 C74 1.419(12) . ? C73 C75 1.460(12) . ? C75 H75 0.9500 . ? C76 C77 1.486(12) . ? C77 C78 1.507(13) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C80 1.492(17) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.52(2) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 C84 1.53(2) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9801 . ? C85 H85B 0.9801 . ? C85 H85C 0.9801 . ? 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 O35 Dy1 O31 117.1(3) . . ? O35 Dy1 O36 132.7(2) . . ? O31 Dy1 O36 76.4(2) . . ? O35 Dy1 O32 77.1(2) . . ? O31 Dy1 O32 133.7(2) . . ? O36 Dy1 O32 128.18(18) . . ? O35 Dy1 O4 86.5(2) . . ? O31 Dy1 O4 150.1(2) . . ? O36 Dy1 O4 74.03(19) . . ? O32 Dy1 O4 66.09(18) . . ? O35 Dy1 O12 151.1(2) . . ? O31 Dy1 O12 87.1(2) . . ? O36 Dy1 O12 65.15(18) . . ? O32 Dy1 O12 74.52(18) . . ? O4 Dy1 O12 77.04(19) . . ? O35 Dy1 N16 72.8(2) . . ? O31 Dy1 N16 81.7(3) . . ? O36 Dy1 N16 64.3(2) . . ? O32 Dy1 N16 141.9(2) . . ? O4 Dy1 N16 89.0(2) . . ? O12 Dy1 N16 129.5(2) . . ? O35 Dy1 N13 88.1(2) . . ? O31 Dy1 N13 72.0(2) . . ? O36 Dy1 N13 137.1(2) . . ? O32 Dy1 N13 64.4(2) . . ? O4 Dy1 N13 130.2(2) . . ? O12 Dy1 N13 84.7(2) . . ? N16 Dy1 N13 135.8(2) . . ? O36 Dy2 O24 124.64(19) . . ? O36 Dy2 O1 116.45(19) . . ? O24 Dy2 O1 118.90(18) . . ? O36 Dy2 O12 65.29(18) . . ? O24 Dy2 O12 128.19(18) . . ? O1 Dy2 O12 77.69(18) . . ? O36 Dy2 O2 126.81(18) . . ? O24 Dy2 O2 65.28(17) . . ? O1 Dy2 O2 78.61(18) . . ? O12 Dy2 O2 156.29(19) . . ? O36 Dy2 O5 68.3(2) . . ? O24 Dy2 O5 128.9(2) . . ? O1 Dy2 O5 72.3(2) . . ? O12 Dy2 O5 102.6(2) . . ? O2 Dy2 O5 69.6(2) . . ? O36 Dy2 O10 129.99(19) . . ? O24 Dy2 O10 69.00(18) . . ? O1 Dy2 O10 73.78(19) . . ? O12 Dy2 O10 70.48(18) . . ? O2 Dy2 O10 102.99(18) . . ? O5 Dy2 O10 146.1(2) . . ? O36 Dy2 N9 74.0(2) . . ? O24 Dy2 N9 63.28(19) . . ? O1 Dy2 N9 142.6(2) . . ? O12 Dy2 N9 75.1(2) . . ? O2 Dy2 N9 125.90(19) . . ? O5 Dy2 N9 138.8(2) . . ? O10 Dy2 N9 73.2(2) . . ? O36 Dy2 N18 62.8(2) . . ? O24 Dy2 N18 71.5(2) . . ? O1 Dy2 N18 145.3(2) . . ? O12 Dy2 N18 124.1(2) . . ? O2 Dy2 N18 76.9(2) . . ? O5 Dy2 N18 76.3(2) . . ? O10 Dy2 N18 135.9(2) . . ? N9 Dy2 N18 72.1(2) . . ? O20 Dy3 O32 124.39(19) . . ? O20 Dy3 O1 117.71(19) . . ? O32 Dy3 O1 117.89(18) . . ? O20 Dy3 O4 128.36(19) . . ? O32 Dy3 O4 65.95(17) . . ? O1 Dy3 O4 76.25(18) . . ? O20 Dy3 O8 65.69(18) . . ? O32 Dy3 O8 128.70(18) . . ? O1 Dy3 O8 77.31(18) . . ? O4 Dy3 O8 153.56(18) . . ? O20 Dy3 O13 129.57(19) . . ? O32 Dy3 O13 69.17(19) . . ? O1 Dy3 O13 73.11(19) . . ? O4 Dy3 O13 101.9(2) . . ? O8 Dy3 O13 70.17(19) . . ? O20 Dy3 O6 68.9(2) . . ? O32 Dy3 O6 128.9(2) . . ? O1 Dy3 O6 72.7(2) . . ? O4 Dy3 O6 69.6(2) . . ? O8 Dy3 O6 102.2(2) . . ? O13 Dy3 O6 145.8(2) . . ? O20 Dy3 N15 73.1(2) . . ? O32 Dy3 N15 62.99(19) . . ? O1 Dy3 N15 143.7(2) . . ? O4 Dy3 N15 126.42(19) . . ? O8 Dy3 N15 76.93(19) . . ? O13 Dy3 N15 74.3(2) . . ? O6 Dy3 N15 138.1(2) . . ? O20 Dy3 N6 63.2(2) . . ? O32 Dy3 N6 71.8(2) . . ? O1 Dy3 N6 144.1(2) . . ? O4 Dy3 N6 77.7(2) . . ? O8 Dy3 N6 125.8(2) . . ? O13 Dy3 N6 136.9(2) . . ? O6 Dy3 N6 75.4(2) . . ? N15 Dy3 N6 72.2(2) . . ? O23 Dy4 O27 113.1(2) . . ? O23 Dy4 O28 76.22(19) . . ? O27 Dy4 O28 135.2(2) . . ? O23 Dy4 O24 133.56(19) . . ? O27 Dy4 O24 79.0(2) . . ? O28 Dy4 O24 127.75(18) . . ? O23 Dy4 O11 86.4(2) . . ? O27 Dy4 O11 153.1(2) . . ? O28 Dy4 O11 65.49(17) . . ? O24 Dy4 O11 74.07(17) . . ? O23 Dy4 O2 150.4(2) . . ? O27 Dy4 O2 91.2(2) . . ? O28 Dy4 O2 74.59(18) . . ? O24 Dy4 O2 65.21(18) . . ? O11 Dy4 O2 77.42(17) . . ? O23 Dy4 N7 72.9(2) . . ? O27 Dy4 N7 82.5(2) . . ? O28 Dy4 N7 139.0(2) . . ? O24 Dy4 N7 64.3(2) . . ? O11 Dy4 N7 86.13(19) . . ? O2 Dy4 N7 129.4(2) . . ? O23 Dy4 N10 87.1(2) . . ? O27 Dy4 N10 72.6(2) . . ? O28 Dy4 N10 64.0(2) . . ? O24 Dy4 N10 137.6(2) . . ? O11 Dy4 N10 129.1(2) . . ? O2 Dy4 N10 84.30(19) . . ? N7 Dy4 N10 138.7(2) . . ? O16 Dy5 O28 125.32(18) . . ? O16 Dy5 O11 129.58(18) . . ? O28 Dy5 O11 65.83(17) . . ? O16 Dy5 O1 117.84(17) . . ? O28 Dy5 O1 116.80(18) . . ? O11 Dy5 O1 77.06(18) . . ? O16 Dy5 O7 65.08(17) . . ? O28 Dy5 O7 127.66(18) . . ? O11 Dy5 O7 153.71(18) . . ? O1 Dy5 O7 76.64(18) . . ? O16 Dy5 O3 128.5(2) . . ? O28 Dy5 O3 68.5(2) . . ? O11 Dy5 O3 101.9(2) . . ? O1 Dy5 O3 71.7(2) . . ? O7 Dy5 O3 69.5(2) . . ? O16 Dy5 O9 68.87(19) . . ? O28 Dy5 O9 129.89(18) . . ? O11 Dy5 O9 70.51(18) . . ? O1 Dy5 O9 74.27(19) . . ? O7 Dy5 O9 102.31(18) . . ? O3 Dy5 O9 146.00(19) . . ? O16 Dy5 N12 72.5(2) . . ? O28 Dy5 N12 63.30(19) . . ? O11 Dy5 N12 126.35(18) . . ? O1 Dy5 N12 142.5(2) . . ? O7 Dy5 N12 76.5(2) . . ? O3 Dy5 N12 74.5(2) . . ? O9 Dy5 N12 137.3(2) . . ? O16 Dy5 N3 63.8(2) . . ? O28 Dy5 N3 72.5(2) . . ? O11 Dy5 N3 78.3(2) . . ? O1 Dy5 N3 146.1(2) . . ? O7 Dy5 N3 125.5(2) . . ? O3 Dy5 N3 136.6(2) . . ? O9 Dy5 N3 75.8(2) . . ? N12 Dy5 N3 71.4(2) . . ? O19 Dy6 O15 115.1(2) . . ? O19 Dy6 O16 77.4(2) . . ? O15 Dy6 O16 132.5(2) . . ? O19 Dy6 O20 133.7(2) . . ? O15 Dy6 O20 77.7(2) . . ? O16 Dy6 O20 128.34(19) . . ? O19 Dy6 O8 151.8(2) . . ? O15 Dy6 O8 86.9(2) . . ? O16 Dy6 O8 74.63(18) . . ? O20 Dy6 O8 65.46(18) . . ? O19 Dy6 O7 88.3(2) . . ? O15 Dy6 O7 151.8(2) . . ? O16 Dy6 O7 65.45(17) . . ? O20 Dy6 O7 74.51(18) . . ? O8 Dy6 O7 77.11(19) . . ? O19 Dy6 N4 72.8(2) . . ? O15 Dy6 N4 84.0(2) . . ? O16 Dy6 N4 140.8(2) . . ? O20 Dy6 N4 64.3(2) . . ? O8 Dy6 N4 129.8(2) . . ? O7 Dy6 N4 88.6(2) . . ? O19 Dy6 N1 82.0(2) . . ? O15 Dy6 N1 72.7(2) . . ? O16 Dy6 N1 63.7(2) . . ? O20 Dy6 N1 141.5(2) . . ? O8 Dy6 N1 88.7(2) . . ? O7 Dy6 N1 129.1(2) . . ? N4 Dy6 N1 134.0(2) . . ? Dy2 O1 Dy3 120.7(2) . . ? Dy2 O1 Dy5 119.5(2) . . ? Dy3 O1 Dy5 119.8(2) . . ? C1 O2 Dy4 123.5(5) . . ? C1 O2 Dy2 122.4(5) . . ? Dy4 O2 Dy2 106.7(2) . . ? C1 O3 Dy5 119.1(6) . . ? C3 O4 Dy1 124.5(6) . . ? C3 O4 Dy3 124.1(5) . . ? Dy1 O4 Dy3 107.5(2) . . ? C3 O5 Dy2 118.1(6) . . ? C5 O6 Dy3 118.9(6) . . ? C5 O7 Dy6 125.1(5) . . ? C5 O7 Dy5 123.1(5) . . ? Dy6 O7 Dy5 106.71(19) . . ? C7 O8 Dy6 124.3(5) . . ? C7 O8 Dy3 123.9(5) . . ? Dy6 O8 Dy3 107.16(19) . . ? C7 O9 Dy5 118.7(5) . . ? C9 O10 Dy2 118.5(5) . . ? C9 O11 Dy5 124.1(5) . . ? C9 O11 Dy4 124.4(5) . . ? Dy5 O11 Dy4 107.92(19) . . ? C11 O12 Dy1 124.0(5) . . ? C11 O12 Dy2 123.4(5) . . ? Dy1 O12 Dy2 106.9(2) . . ? C11 O13 Dy3 120.1(5) . . ? C14 O14 C13 121.4(11) . . ? C19 O15 Dy6 140.1(6) . . ? C21 O16 Dy5 122.7(5) . . ? C21 O16 Dy6 121.3(5) . . ? Dy5 O16 Dy6 111.5(2) . . ? N3 O17 H17 109.5 . . ? C24 O18 C25 122.2(16) . . ? C30 O19 Dy6 142.3(6) . . ? C32 O20 Dy3 124.4(5) . . ? C32 O20 Dy6 119.8(5) . . ? Dy3 O20 Dy6 111.3(2) . . ? N6 O21 H21 109.5 . . ? C36 O22 C35 117.5(8) . . ? C41 O23 Dy4 140.9(5) . . ? C43 O24 Dy2 122.4(5) . . ? C43 O24 Dy4 118.2(5) . . ? Dy2 O24 Dy4 110.6(2) . . ? N9 O25 H25 109.5 . . ? C47 O26 C46 116.5(8) . . ? C52 O27 Dy4 142.5(6) . . ? C54 O28 Dy5 122.8(5) . . ? C54 O28 Dy4 120.5(5) . . ? Dy5 O28 Dy4 111.5(2) . . ? N12 O29 H29 109.5 . . ? C57 O30 C58 133(2) . . ? C63 O31 Dy1 143.3(6) . . ? C65 O32 Dy3 122.2(5) . . ? C65 O32 Dy1 120.2(5) . . ? Dy3 O32 Dy1 110.29(19) . . ? N15 O33 H33 109.5 . . ? C69 O34 C68 117.3(8) . . ? C74 O35 Dy1 141.0(6) . . ? C76 O36 Dy2 123.5(5) . . ? C76 O36 Dy1 120.6(5) . . ? Dy2 O36 Dy1 111.8(2) . . ? N18 O37 H37A 109.5 . . ? C85 O38 H38A 113.8 . . ? C20 N1 N2 112.0(7) . . ? C20 N1 Dy6 129.8(6) . . ? N2 N1 Dy6 118.2(5) . . ? C21 N2 N1 111.1(7) . . ? C22 N3 O17 113.7(7) . . ? C22 N3 Dy5 118.3(5) . . ? O17 N3 Dy5 128.0(5) . . ? C31 N4 N5 112.1(7) . . ? C31 N4 Dy6 130.5(6) . . ? N5 N4 Dy6 117.4(5) . . ? C32 N5 N4 111.9(7) . . ? C33 N6 O21 113.2(7) . . ? C33 N6 Dy3 118.7(5) . . ? O21 N6 Dy3 128.2(5) . . ? C42 N7 N8 111.9(7) . . ? C42 N7 Dy4 129.0(6) . . ? N8 N7 Dy4 119.2(5) . . ? C43 N8 N7 110.1(7) . . ? C44 N9 O25 112.1(7) . . ? C44 N9 Dy2 119.9(6) . . ? O25 N9 Dy2 127.3(5) . . ? C53 N10 N11 110.3(7) . . ? C53 N10 Dy4 130.8(6) . . ? N11 N10 Dy4 118.7(4) . . ? C54 N11 N10 110.3(6) . . ? C55 N12 O29 114.1(6) . . ? C55 N12 Dy5 118.8(5) . . ? O29 N12 Dy5 127.1(4) . . ? C64 N13 N14 111.0(7) . . ? C64 N13 Dy1 130.8(6) . . ? N14 N13 Dy1 118.0(5) . . ? C65 N14 N13 111.1(6) . . ? C66 N15 O33 113.2(6) . . ? C66 N15 Dy3 119.3(5) . . ? O33 N15 Dy3 127.3(5) . . ? C75 N16 N17 111.2(7) . . ? C75 N16 Dy1 130.4(6) . . ? N17 N16 Dy1 118.3(5) . . ? C76 N17 N16 110.9(7) . . ? C77 N18 O37 114.1(7) . . ? C77 N18 Dy2 119.8(5) . . ? O37 N18 Dy2 126.1(5) . . ? C83 N19 C81 109(2) . . ? C83 N19 C79 95(2) . . ? C81 N19 C79 102.9(17) . . ? C83 N19 H19 115.6 . . ? C81 N19 H19 115.7 . . ? C79 N19 H19 115.7 . . ? O2 C1 O3 123.9(9) . . ? O2 C1 C2 115.1(9) . . ? O3 C1 C2 121.0(9) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O4 C3 O5 121.6(8) . . ? O4 C3 C4 117.7(8) . . ? O5 C3 C4 120.5(8) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O6 C5 O7 122.5(9) . . ? O6 C5 C6 121.0(8) . . ? O7 C5 C6 116.5(8) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O9 C7 O8 123.2(8) . . ? O9 C7 C8 120.0(8) . . ? O8 C7 C8 116.8(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O10 C9 O11 121.7(7) . . ? O10 C9 C10 122.1(8) . . ? O11 C9 C10 116.2(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O13 C11 O12 122.1(8) . . ? O13 C11 C12 121.1(8) . . ? O12 C11 C12 116.8(8) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O14 C13 H13A 109.5 . . ? O14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O14 C14 C15 125.9(10) . . ? O14 C14 C19 115.1(9) . . ? C15 C14 C19 119.0(11) . . ? C14 C15 C16 122.5(11) . . ? C14 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C17 C16 C15 119.1(11) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 120.1(11) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C19 C18 C17 121.2(9) . . ? C19 C18 C20 123.8(8) . . ? C17 C18 C20 114.8(9) . . ? O15 C19 C18 123.6(8) . . ? O15 C19 C14 118.4(9) . . ? C18 C19 C14 118.0(9) . . ? N1 C20 C18 126.0(9) . . ? N1 C20 H20 117.0 . . ? C18 C20 H20 117.0 . . ? N2 C21 O16 125.2(8) . . ? N2 C21 C22 116.7(7) . . ? O16 C21 C22 118.0(7) . . ? N3 C22 C21 113.3(7) . . ? N3 C22 C23 125.1(8) . . ? C21 C22 C23 121.6(8) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O18 C24 H24A 109.4 . . ? O18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O18 C25 C26 123.4(9) . . ? O18 C25 C30 115.8(9) . . ? C26 C25 C30 120.8(10) . . ? C25 C26 C27 121.4(10) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 118.6(9) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C27 C28 C29 121.4(10) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C28 C29 C30 119.9(8) . . ? C28 C29 C31 116.5(8) . . ? C30 C29 C31 123.3(8) . . ? O19 C30 C25 119.2(9) . . ? O19 C30 C29 123.1(8) . . ? C25 C30 C29 117.8(8) . . ? N4 C31 C29 126.4(8) . . ? N4 C31 H31 116.8 . . ? C29 C31 H31 116.8 . . ? N5 C32 O20 126.1(8) . . ? N5 C32 C33 117.9(7) . . ? O20 C32 C33 115.9(7) . . ? N6 C33 C32 113.7(7) . . ? N6 C33 C34 124.8(8) . . ? C32 C33 C34 121.4(8) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O22 C35 H35A 109.5 . . ? O22 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O22 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O22 C36 C37 124.6(8) . . ? O22 C36 C41 115.0(7) . . ? C37 C36 C41 120.4(9) . . ? C38 C37 C36 121.3(9) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 118.9(8) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? C38 C39 C40 121.0(9) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C41 C40 C39 120.0(8) . . ? C41 C40 C42 122.8(7) . . ? C39 C40 C42 117.1(8) . . ? O23 C41 C40 122.3(7) . . ? O23 C41 C36 119.3(8) . . ? C40 C41 C36 118.4(8) . . ? N7 C42 C40 127.5(8) . . ? N7 C42 H42 116.2 . . ? C40 C42 H42 116.2 . . ? N8 C43 O24 128.2(8) . . ? N8 C43 C44 116.0(8) . . ? O24 C43 C44 115.8(8) . . ? N9 C44 C43 112.1(8) . . ? N9 C44 C45 126.2(8) . . ? C43 C44 C45 121.3(8) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O26 C46 H46A 109.5 . . ? O26 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O26 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O26 C47 C48 126.3(9) . . ? O26 C47 C52 114.1(8) . . ? C48 C47 C52 119.6(9) . . ? C47 C48 C49 121.8(10) . . ? C47 C48 H48 119.1 . . ? C49 C48 H48 119.1 . . ? C50 C49 C48 119.5(10) . . ? C50 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C49 C50 C51 120.9(10) . . ? C49 C50 H50 119.5 . . ? C51 C50 H50 119.5 . . ? C52 C51 C50 120.5(9) . . ? C52 C51 C53 123.4(8) . . ? C50 C51 C53 116.0(9) . . ? O27 C52 C51 123.7(8) . . ? O27 C52 C47 118.6(8) . . ? C51 C52 C47 117.7(8) . . ? N10 C53 C51 126.5(8) . . ? N10 C53 H53 116.8 . . ? C51 C53 H53 116.8 . . ? N11 C54 O28 126.0(7) . . ? N11 C54 C55 117.3(7) . . ? O28 C54 C55 116.6(7) . . ? N12 C55 C54 113.9(7) . . ? N12 C55 C56 125.7(8) . . ? C54 C55 C56 120.3(7) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O30 C57 H57A 109.5 . . ? O30 C57 H57B 109.4 . . ? H57A C57 H57B 109.5 . . ? O30 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 O30 125.6(11) . . ? C59 C58 C63 121.2(11) . . ? O30 C58 C63 113.2(10) . . ? C58 C59 C60 122.5(13) . . ? C58 C59 H59 118.8 . . ? C60 C59 H59 118.8 . . ? C59 C60 C61 117.8(15) . . ? C59 C60 H60 121.1 . . ? C61 C60 H60 121.1 . . ? C62 C61 C60 122.6(12) . . ? C62 C61 H61 118.7 . . ? C60 C61 H61 118.7 . . ? C61 C62 C63 119.3(10) . . ? C61 C62 C64 119.0(9) . . ? C63 C62 C64 121.6(9) . . ? O31 C63 C62 123.3(8) . . ? O31 C63 C58 120.1(9) . . ? C62 C63 C58 116.6(9) . . ? N13 C64 C62 127.1(8) . . ? N13 C64 H64 116.5 . . ? C62 C64 H64 116.5 . . ? O32 C65 N14 126.1(7) . . ? O32 C65 C66 117.0(7) . . ? N14 C65 C66 116.9(7) . . ? N15 C66 C67 125.9(8) . . ? N15 C66 C65 112.7(7) . . ? C67 C66 C65 121.3(8) . . ? 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 . . ? O34 C68 H68A 109.5 . . ? O34 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? O34 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O34 C69 C70 124.5(9) . . ? O34 C69 C74 113.9(7) . . ? C70 C69 C74 121.6(9) . . ? C71 C70 C69 122.5(10) . . ? C71 C70 H70 118.7 . . ? C69 C70 H70 118.7 . . ? C70 C71 C72 117.1(9) . . ? C70 C71 H71 121.5 . . ? C72 C71 H71 121.5 . . ? C73 C72 C71 121.4(8) . . ? C73 C72 H72 119.3 . . ? C71 C72 H72 119.3 . . ? C72 C73 C74 119.8(8) . . ? C72 C73 C75 116.9(7) . . ? C74 C73 C75 123.0(7) . . ? O35 C74 C69 119.9(8) . . ? O35 C74 C73 122.7(8) . . ? C69 C74 C73 117.4(7) . . ? N16 C75 C73 126.2(7) . . ? N16 C75 H75 116.9 . . ? C73 C75 H75 116.9 . . ? O36 C76 N17 125.2(7) . . ? O36 C76 C77 116.7(8) . . ? N17 C76 C77 118.1(7) . . ? N18 C77 C76 112.9(7) . . ? N18 C77 C78 126.0(9) . . ? C76 C77 C78 121.0(9) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.4 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C80 C79 N19 110.6(17) . . ? C80 C79 H79A 109.5 . . ? N19 C79 H79A 109.6 . . ? C80 C79 H79B 109.4 . . ? N19 C79 H79B 109.5 . . ? H79A C79 H79B 108.1 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.4 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C82 C81 N19 82(2) . . ? C82 C81 H81A 114.9 . . ? N19 C81 H81A 114.9 . . ? C82 C81 H81B 114.9 . . ? N19 C81 H81B 115.0 . . ? H81A C81 H81B 112.0 . . ? 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 . . ? C84 C83 N19 82(3) . . ? C84 C83 H83A 115.4 . . ? N19 C83 H83A 115.0 . . ? C84 C83 H83B 114.6 . . ? N19 C83 H83B 115.0 . . ? H83A C83 H83B 112.0 . . ? C83 C84 H84A 109.4 . . ? C83 C84 H84B 109.1 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.9 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? O38 C85 H85A 109.3 . . ? O38 C85 H85B 110.3 . . ? H85A C85 H85B 109.4 . . ? O38 C85 H85C 108.9 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.243 _refine_diff_density_min -2.211 _refine_diff_density_rms 0.274 # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.500 0.000 0.500 1041 418 ' ' 2 0.355 0.052 0.798 15 4 ' ' 3 0.645 0.948 0.202 15 5 ' ' _platon_squeeze_details ; ; _iucr_refine_instructions_details ; TITL SST_142_12_DyOAcL4_09_22_2012 in P-1 CELL 0.71073 17.7380 18.4019 20.0747 79.481 68.918 76.306 ZERR 2.00 0.0017 0.0017 0.0019 0.001 0.001 0.001 LATT 1 SFAC C H N O Dy UNIT 186 300 38 106 12 OMIT -1 0 1 OMIT -3 50.1 L.S. 16 ACTA BOND $H FMAP 2 PLAN 40 SIZE 0.24 0.20 0.15 FREE Dy5 Dy4 FREE Dy5 Dy6 FREE Dy3 Dy6 FREE Dy1 Dy3 FREE Dy1 Dy2 FREE Dy2 Dy4 FREE N19 C82 DFIX 1.54 0.02 C79 C80 C81 C82 C83 C84 DFIX 1.69 0.02 C79 N19 N19 C81 N19 C83 WGHT 0.115300 49.694500 FVAR 0.469760 TEMP -85.000 MOLE 1 Dy1 5 0.493615 0.675691 0.234625 11.000000 0.020220 = 0.032860 0.035030 -0.016910 -0.009820 -0.000660 Dy2 5 0.712626 0.682962 0.231657 11.000000 0.021180 = 0.027190 0.029640 -0.009540 -0.010760 -0.003400 Dy3 5 0.635801 0.482547 0.249990 11.000000 0.017650 = 0.028130 0.024480 -0.008730 -0.005010 -0.005030 Dy4 5 0.933583 0.673832 0.232168 11.000000 0.021050 = 0.028430 0.024030 -0.003230 -0.008620 -0.007250 Dy5 5 0.870168 0.481021 0.249606 11.000000 0.017840 = 0.025460 0.022010 -0.004230 -0.005150 -0.004830 Dy6 5 0.790459 0.297423 0.266163 11.000000 0.025880 = 0.027330 0.031160 -0.004600 -0.008700 -0.005650 O1 4 0.737833 0.549400 0.245624 11.000000 0.022500 = 0.017300 0.056260 -0.004040 -0.017460 -0.005980 O2 4 0.797997 0.654522 0.308095 11.000000 0.018970 = 0.034870 0.026530 -0.005070 -0.007970 -0.005010 O3 4 0.795325 0.533878 0.363448 11.000000 0.031690 = 0.066250 0.035540 -0.015310 -0.008980 0.000760 O4 4 0.557281 0.590246 0.312747 11.000000 0.026730 = 0.034900 0.033920 -0.014730 -0.012380 -0.003510 O5 4 0.632173 0.641414 0.356359 11.000000 0.049960 = 0.045060 0.044110 -0.016210 -0.010570 0.002090 O6 4 0.645053 0.465659 0.370945 11.000000 0.052390 = 0.062360 0.037080 -0.002330 -0.015360 -0.027870 O7 4 0.775777 0.401328 0.329808 11.000000 0.019520 = 0.030480 0.032280 -0.015470 0.003080 -0.008590 O8 4 0.762656 0.404645 0.184763 11.000000 0.022480 = 0.030620 0.023400 -0.004530 -0.000760 -0.002540 O9 4 0.866691 0.467367 0.131588 11.000000 0.026430 = 0.036860 0.029010 -0.007560 -0.005850 -0.007380 O10 4 0.810734 0.643110 0.114800 11.000000 0.030810 = 0.032160 0.034280 -0.006190 -0.012390 -0.006740 O11 4 0.903465 0.591208 0.168749 11.000000 0.026110 = 0.034340 0.019410 -0.000080 -0.011830 -0.007560 O12 4 0.637714 0.655222 0.162011 11.000000 0.024940 = 0.032970 0.034070 -0.014730 -0.006410 -0.008680 O13 4 0.687698 0.539970 0.126782 11.000000 0.028300 = 0.043660 0.029970 -0.011520 -0.004620 -0.011970 O14 4 0.632040 0.165001 0.203934 11.000000 0.054100 = 0.061840 0.105050 -0.021420 -0.034290 -0.025690 O15 4 0.743052 0.233116 0.210681 11.000000 0.040220 = 0.040590 0.050190 -0.010690 -0.014460 -0.013350 O16 4 0.906482 0.354461 0.227707 11.000000 0.020750 = 0.032180 0.025310 -0.005700 -0.002890 -0.006210 O17 4 1.087302 0.472143 0.155505 11.000000 0.027910 = 0.043590 0.061380 -0.007470 -0.005090 -0.018320 AFIX 147 H17 2 1.069609 0.516050 0.167473 11.000000 -1.500000 AFIX 0 O18 4 1.006153 0.161444 0.350951 11.000000 0.042900 = 0.071840 0.100660 0.005430 -0.034320 -0.011270 O19 4 0.866046 0.227640 0.329907 11.000000 0.035470 = 0.043050 0.050020 0.003520 -0.017820 -0.007100 O20 4 0.650016 0.356059 0.295306 11.000000 0.023040 = 0.034930 0.032720 -0.001610 -0.004710 -0.007160 O21 4 0.422645 0.473182 0.348321 11.000000 0.017940 = 0.048750 0.064010 -0.012680 -0.003330 -0.001880 AFIX 147 H21 2 0.421533 0.515052 0.323256 11.000000 -1.500000 AFIX 0 O22 4 1.208103 0.544165 0.172640 11.000000 0.023280 = 0.046630 0.053500 0.002010 -0.011350 -0.002400 O23 4 1.064112 0.628938 0.177453 11.000000 0.021570 = 0.040810 0.032760 0.003820 -0.009340 -0.005050 O24 4 0.824934 0.745152 0.191193 11.000000 0.029960 = 0.031350 0.027090 -0.003920 -0.018500 -0.005300 O25 4 0.642842 0.830263 0.111798 11.000000 0.050410 = 0.046040 0.101800 0.018800 -0.056350 -0.016480 AFIX 147 H25 2 0.598236 0.821738 0.142700 11.000000 -1.500000 AFIX 0 O26 4 0.857635 0.928603 0.277700 11.000000 0.055550 = 0.035560 0.050310 -0.007430 -0.028270 -0.004610 O27 4 0.913755 0.783191 0.274520 11.000000 0.054930 = 0.034010 0.038670 -0.008580 -0.025900 -0.007090 O28 4 0.950235 0.546099 0.279596 11.000000 0.027590 = 0.027430 0.026970 0.001040 -0.011620 -0.007970 O29 4 0.952818 0.332099 0.361827 11.000000 0.047050 = 0.027180 0.041130 0.006190 -0.025410 -0.009920 AFIX 147 H29 2 0.935356 0.310465 0.338458 11.000000 -1.500000 AFIX 0 O30 4 0.461299 0.932851 0.151646 11.000000 0.113740 = 0.054690 0.189720 -0.045890 -0.101710 -0.000640 O31 4 0.480228 0.785876 0.168356 11.000000 0.068920 = 0.034130 0.063780 -0.014180 -0.042080 -0.002640 O32 4 0.526513 0.549272 0.209604 11.000000 0.024920 = 0.036490 0.028980 -0.018230 -0.010090 -0.003050 O33 4 0.616327 0.339487 0.159292 11.000000 0.042410 = 0.029110 0.048360 -0.015170 -0.018360 -0.000530 AFIX 147 H33 2 0.647490 0.317250 0.182793 11.000000 -1.500000 AFIX 0 O34 4 0.269537 0.547598 0.326699 11.000000 0.026460 = 0.051490 0.064610 -0.022920 -0.010200 -0.010550 O35 4 0.379223 0.632793 0.299527 11.000000 0.022560 = 0.048440 0.050400 -0.022710 -0.006830 -0.007290 O36 4 0.574444 0.743371 0.262121 11.000000 0.025880 = 0.034360 0.043650 -0.022110 -0.010510 0.001460 O37 4 0.724884 0.839840 0.307923 11.000000 0.033420 = 0.063720 0.102540 -0.052980 -0.030700 -0.004160 AFIX 147 H37A 2 0.769499 0.810098 0.305581 11.000000 -1.500000 AFIX 0 O38 4 0.970855 0.124100 0.825399 11.000000 0.092670 = 0.155250 0.125220 0.022980 -0.015110 -0.013460 AFIX 147 H38A 2 0.919753 0.139517 0.840113 11.000000 -1.500000 AFIX 0 N1 3 0.910351 0.244068 0.164062 11.000000 0.039720 = 0.032070 0.032580 -0.013750 -0.011230 -0.002170 N2 3 0.984107 0.271460 0.144045 11.000000 0.025970 = 0.038530 0.038980 -0.016630 -0.000940 -0.005170 N3 3 1.023088 0.434644 0.175794 11.000000 0.021270 = 0.040720 0.033870 -0.005900 -0.008460 -0.004140 N4 3 0.694219 0.240485 0.378178 11.000000 0.031100 = 0.036300 0.036340 -0.002380 -0.011500 -0.010620 N5 3 0.609035 0.269150 0.393817 11.000000 0.034220 = 0.038530 0.039290 -0.001170 -0.001270 -0.011380 N6 3 0.502290 0.435074 0.332862 11.000000 0.023900 = 0.042950 0.035560 -0.008730 -0.009080 -0.009700 N7 3 0.976449 0.751382 0.114596 11.000000 0.031120 = 0.028120 0.032270 -0.003500 -0.012440 -0.009150 N8 3 0.915468 0.797018 0.087501 11.000000 0.038610 = 0.033100 0.040970 0.000690 -0.017060 -0.012110 N9 3 0.707610 0.797278 0.138241 11.000000 0.033790 = 0.024990 0.056000 -0.003170 -0.028470 -0.003330 N10 3 0.965573 0.645615 0.346271 11.000000 0.029530 = 0.034230 0.029030 -0.001480 -0.013250 -0.012410 N11 3 0.985389 0.568786 0.373386 11.000000 0.026160 = 0.032490 0.034920 -0.006360 -0.015520 -0.002850 N12 3 0.945978 0.408257 0.337269 11.000000 0.025800 = 0.027120 0.032430 -0.000740 -0.009790 -0.008780 N13 3 0.470387 0.654065 0.124607 11.000000 0.028740 = 0.032480 0.033880 -0.005920 -0.015160 -0.004910 N14 3 0.484203 0.578904 0.109454 11.000000 0.022530 = 0.037410 0.043270 -0.015900 -0.015800 -0.001730 N15 3 0.589416 0.413924 0.173791 11.000000 0.021170 = 0.033480 0.041090 -0.015950 -0.011260 -0.001360 N16 3 0.419142 0.756540 0.334000 11.000000 0.030020 = 0.045090 0.046190 -0.024640 -0.014420 -0.000970 N17 3 0.461910 0.804926 0.347566 11.000000 0.031000 = 0.046440 0.068810 -0.036610 -0.020020 0.005050 N18 3 0.671273 0.802469 0.296846 11.000000 0.033270 = 0.036470 0.054280 -0.024600 -0.017590 -0.005540 N19 3 0.831932 0.132265 0.791585 11.000000 0.165770 = 0.222910 0.112440 0.016290 -0.043460 -0.126850 AFIX 13 H19 2 0.887063 0.120199 0.788177 11.000000 -1.200000 AFIX 0 C1 1 0.784237 0.606490 0.364922 11.000000 0.032190 = 0.057610 0.046810 -0.013480 -0.013430 -0.009710 C2 1 0.755513 0.640039 0.435406 11.000000 0.029260 = 0.080290 0.030220 -0.020220 -0.006310 -0.008650 AFIX 137 H2A 2 0.734402 0.602456 0.475109 11.000000 -1.500000 H2B 2 0.711782 0.684030 0.435277 11.000000 -1.500000 H2C 2 0.801770 0.655336 0.441437 11.000000 -1.500000 AFIX 0 C3 1 0.570433 0.609309 0.366103 11.000000 0.018790 = 0.062020 0.041430 -0.016580 -0.007250 -0.005330 C4 1 0.507934 0.599296 0.439368 11.000000 0.028310 = 0.065850 0.037490 -0.019840 -0.001940 -0.014930 AFIX 137 H4A 2 0.535603 0.586080 0.475473 11.000000 -1.500000 H4B 2 0.479401 0.558969 0.441404 11.000000 -1.500000 H4C 2 0.467975 0.646297 0.449083 11.000000 -1.500000 AFIX 0 C5 1 0.710782 0.425970 0.381768 11.000000 0.030970 = 0.036350 0.048130 -0.006580 -0.012910 -0.001870 C6 1 0.714823 0.404079 0.456391 11.000000 0.030180 = 0.060320 0.035610 -0.005750 -0.009770 -0.006450 AFIX 137 H6A 2 0.677768 0.442135 0.487573 11.000000 -1.500000 H6B 2 0.771243 0.400608 0.455284 11.000000 -1.500000 H6C 2 0.698095 0.355208 0.475018 11.000000 -1.500000 AFIX 0 C7 1 0.818040 0.429640 0.128582 11.000000 0.027120 = 0.032760 0.034980 -0.009580 -0.007520 0.000810 C8 1 0.822874 0.410627 0.057183 11.000000 0.031590 = 0.051310 0.021500 -0.008370 -0.004660 -0.009620 AFIX 137 H8A 2 0.839127 0.452070 0.020144 11.000000 -1.500000 H8B 2 0.768976 0.402866 0.060001 11.000000 -1.500000 H8C 2 0.863667 0.364564 0.044906 11.000000 -1.500000 AFIX 0 C9 1 0.882170 0.612754 0.111187 11.000000 0.030460 = 0.025290 0.034000 -0.006490 -0.006320 -0.008480 C10 1 0.948970 0.599891 0.041125 11.000000 0.032390 = 0.050730 0.022310 -0.008030 -0.001290 -0.000070 AFIX 137 H10A 2 0.929266 0.577899 0.010989 11.000000 -1.500000 H10B 2 0.996740 0.565395 0.049664 11.000000 -1.500000 H10C 2 0.964764 0.647932 0.016723 11.000000 -1.500000 AFIX 0 C11 1 0.670280 0.609851 0.112366 11.000000 0.022980 = 0.035620 0.031500 -0.005780 -0.005680 -0.010910 C12 1 0.683202 0.644256 0.037300 11.000000 0.035030 = 0.049820 0.030370 -0.001120 -0.007290 -0.009110 AFIX 137 H12A 2 0.720266 0.607848 0.004287 11.000000 -1.500000 H12B 2 0.707606 0.688997 0.029109 11.000000 -1.500000 H12C 2 0.630279 0.658673 0.028861 11.000000 -1.500000 AFIX 0 C13 1 0.567420 0.132852 0.204426 11.000000 0.114930 = 0.114380 0.232540 -0.062370 -0.106330 -0.021320 AFIX 137 H13A 2 0.565140 0.138704 0.155638 11.000000 -1.500000 H13B 2 0.515272 0.158190 0.236238 11.000000 -1.500000 H13C 2 0.576782 0.079243 0.221746 11.000000 -1.500000 AFIX 0 C14 1 0.709716 0.139588 0.165728 11.000000 0.057860 = 0.034910 0.065940 -0.008060 -0.037940 -0.003220 C15 1 0.736474 0.082233 0.121057 11.000000 0.088180 = 0.062370 0.080640 -0.013010 -0.045610 -0.028380 AFIX 43 H15 2 0.696870 0.057818 0.117208 11.000000 -1.200000 AFIX 0 C16 1 0.819469 0.059250 0.081662 11.000000 0.107140 = 0.056010 0.067520 -0.022520 -0.041640 -0.015760 AFIX 43 H16 2 0.835842 0.018942 0.052865 11.000000 -1.200000 AFIX 0 C17 1 0.877192 0.095936 0.085219 11.000000 0.069020 = 0.046620 0.065080 -0.018890 -0.024710 -0.011930 AFIX 43 H17A 2 0.933504 0.081748 0.057780 11.000000 -1.200000 AFIX 0 C18 1 0.852465 0.154920 0.129894 11.000000 0.054930 = 0.025440 0.047070 -0.005520 -0.033300 -0.001220 C19 1 0.769012 0.178643 0.169661 11.000000 0.061000 = 0.028760 0.046240 -0.000540 -0.031590 -0.011190 C20 1 0.917251 0.191179 0.126156 11.000000 0.046030 = 0.035520 0.039700 -0.006110 -0.018690 0.001600 AFIX 43 H20 2 0.970092 0.175063 0.092911 11.000000 -1.200000 AFIX 0 C21 1 0.974318 0.327858 0.178020 11.000000 0.025200 = 0.031980 0.028790 -0.011480 -0.005590 0.002140 C22 1 1.043988 0.367791 0.155808 11.000000 0.028690 = 0.038820 0.027980 -0.009870 -0.002710 -0.004330 C23 1 1.129135 0.331148 0.117518 11.000000 0.023310 = 0.062810 0.064580 -0.028600 0.004610 -0.007080 AFIX 137 H23A 2 1.148423 0.357447 0.069199 11.000000 -1.500000 H23B 2 1.130024 0.278516 0.113983 11.000000 -1.500000 H23C 2 1.165234 0.333263 0.144065 11.000000 -1.500000 AFIX 0 C24 1 1.076660 0.147816 0.366469 11.000000 0.360220 = 0.206490 0.138370 -0.009470 -0.055250 -0.047450 AFIX 137 H24A 2 1.111141 0.100974 0.347846 11.000000 -1.500000 H24B 2 1.063727 0.143081 0.418640 11.000000 -1.500000 H24C 2 1.106226 0.189513 0.344170 11.000000 -1.500000 AFIX 0 C25 1 0.936570 0.139419 0.397908 11.000000 0.053640 = 0.047580 0.049380 -0.005900 -0.030320 0.003630 C26 1 0.935683 0.085814 0.456042 11.000000 0.065780 = 0.043040 0.050290 -0.005030 -0.036420 0.003370 AFIX 43 H26 2 0.985780 0.063655 0.464859 11.000000 -1.200000 AFIX 0 C27 1 0.862777 0.063519 0.502091 11.000000 0.075810 = 0.034650 0.038420 -0.001760 -0.032820 -0.005440 AFIX 43 H27 2 0.862862 0.026729 0.541999 11.000000 -1.200000 AFIX 0 C28 1 0.790694 0.095998 0.488439 11.000000 0.071140 = 0.025040 0.033830 -0.006830 -0.019430 -0.008390 AFIX 43 H28 2 0.740970 0.080156 0.518588 11.000000 -1.200000 AFIX 0 C29 1 0.789136 0.151997 0.430939 11.000000 0.047800 = 0.024770 0.035370 -0.001470 -0.018000 -0.006370 C30 1 0.863153 0.175319 0.384695 11.000000 0.050600 = 0.031400 0.034430 -0.005840 -0.022990 -0.003720 C31 1 0.709261 0.187954 0.426762 11.000000 0.044970 = 0.034570 0.028450 0.002150 -0.013080 -0.013390 AFIX 43 H31 2 0.663087 0.171546 0.463200 11.000000 -1.200000 AFIX 0 C32 1 0.594857 0.327293 0.350281 11.000000 0.027790 = 0.034660 0.026160 0.000930 -0.006190 -0.013910 C33 1 0.508449 0.368670 0.365080 11.000000 0.028360 = 0.043130 0.025290 0.001260 -0.004650 -0.012580 C34 1 0.437157 0.334583 0.417446 11.000000 0.031230 = 0.077730 0.070360 0.006600 -0.003910 -0.022200 AFIX 137 H34A 2 0.385360 0.367882 0.416637 11.000000 -1.500000 H34B 2 0.440492 0.328274 0.465909 11.000000 -1.500000 H34C 2 0.439308 0.285451 0.403805 11.000000 -1.500000 AFIX 0 C35 1 1.281578 0.490571 0.162319 11.000000 0.048310 = 0.056080 0.086970 -0.004100 -0.024670 0.016080 AFIX 33 H35A 2 1.272927 0.448764 0.200567 11.000000 -1.500000 H35B 2 1.325102 0.514119 0.163547 11.000000 -1.500000 H35C 2 1.297802 0.471559 0.115666 11.000000 -1.500000 AFIX 0 C36 1 1.208828 0.606560 0.124052 11.000000 0.026010 = 0.043640 0.038330 -0.015070 -0.007170 -0.010420 C37 1 1.279814 0.628299 0.073353 11.000000 0.022520 = 0.062530 0.042550 -0.014440 -0.001540 -0.015310 AFIX 43 H37 2 1.332080 0.599418 0.072683 11.000000 -1.200000 AFIX 0 C38 1 1.275551 0.690901 0.024204 11.000000 0.032720 = 0.058560 0.032840 -0.013320 0.002940 -0.014210 AFIX 43 H38 2 1.324167 0.704194 -0.011089 11.000000 -1.200000 AFIX 0 C39 1 1.198853 0.734215 0.027213 11.000000 0.044470 = 0.051960 0.027300 -0.007210 -0.006440 -0.019150 AFIX 43 H39 2 1.195405 0.778333 -0.005391 11.000000 -1.200000 AFIX 0 C40 1 1.126361 0.713722 0.077750 11.000000 0.030150 = 0.046370 0.022620 -0.012930 -0.007970 -0.013720 C41 1 1.130847 0.649728 0.127485 11.000000 0.025860 = 0.039660 0.029200 -0.011040 -0.002590 -0.010630 C42 1 1.049586 0.757389 0.071987 11.000000 0.038980 = 0.042650 0.024540 -0.000250 -0.009000 -0.024130 AFIX 43 H42 2 1.053274 0.794952 0.032191 11.000000 -1.200000 AFIX 0 C43 1 0.844271 0.786524 0.129056 11.000000 0.039380 = 0.028620 0.039890 -0.004100 -0.023330 -0.007950 C44 1 0.773623 0.823978 0.102188 11.000000 0.040090 = 0.028450 0.059900 0.003010 -0.026700 -0.006930 C45 1 0.785763 0.879317 0.034889 11.000000 0.078010 = 0.066240 0.104040 0.043300 -0.064480 -0.048000 AFIX 137 H45A 2 0.764350 0.863887 0.002010 11.000000 -1.500000 H45B 2 0.844523 0.880145 0.011359 11.000000 -1.500000 H45C 2 0.756260 0.929673 0.047818 11.000000 -1.500000 AFIX 0 C46 1 0.816485 1.004473 0.283584 11.000000 0.090840 = 0.049930 0.072560 -0.015370 -0.047010 0.015570 AFIX 137 H46A 2 0.770043 1.007502 0.328638 11.000000 -1.500000 H46B 2 0.796201 1.023019 0.243014 11.000000 -1.500000 H46C 2 0.854779 1.035320 0.283167 11.000000 -1.500000 AFIX 0 C47 1 0.881005 0.892433 0.333798 11.000000 0.037840 = 0.045450 0.048250 -0.012340 -0.012130 -0.018280 C48 1 0.877956 0.924063 0.391610 11.000000 0.089490 = 0.042090 0.068080 -0.018410 -0.051010 0.002410 AFIX 43 H48 2 0.858083 0.976559 0.393799 11.000000 -1.200000 AFIX 0 C49 1 0.903138 0.881465 0.447159 11.000000 0.130030 = 0.064750 0.078340 -0.033470 -0.068200 0.007580 AFIX 43 H49 2 0.900944 0.904767 0.486493 11.000000 -1.200000 AFIX 0 C50 1 0.931213 0.805446 0.444760 11.000000 0.107490 = 0.048630 0.068730 -0.021790 -0.070060 0.009820 AFIX 43 H50 2 0.948363 0.776276 0.482753 11.000000 -1.200000 AFIX 0 C51 1 0.934939 0.770181 0.386910 11.000000 0.047200 = 0.041830 0.041910 -0.007860 -0.022920 -0.008830 C52 1 0.910017 0.811956 0.330484 11.000000 0.035970 = 0.038870 0.045150 -0.013590 -0.022400 -0.008180 C53 1 0.961374 0.690171 0.391852 11.000000 0.040140 = 0.037050 0.039110 -0.008440 -0.019960 -0.002380 AFIX 43 H53 2 0.977463 0.667162 0.432255 11.000000 -1.200000 AFIX 0 C54 1 0.973427 0.524948 0.336169 11.000000 0.015740 = 0.029100 0.032560 0.002540 -0.008070 -0.005340 C55 1 0.980071 0.443985 0.363056 11.000000 0.025780 = 0.031540 0.039290 0.002570 -0.019470 -0.003910 C56 1 1.020063 0.411884 0.419724 11.000000 0.055810 = 0.050580 0.066190 0.009060 -0.042450 -0.016210 AFIX 137 H56A 2 1.012312 0.359799 0.436082 11.000000 -1.500000 H56B 2 0.994819 0.441968 0.460466 11.000000 -1.500000 H56C 2 1.078995 0.413066 0.399377 11.000000 -1.500000 AFIX 0 C57 1 0.460109 0.988001 0.157360 11.000000 0.234520 = 0.362830 0.388510 -0.256600 -0.191640 0.041670 AFIX 33 H57A 2 0.473174 0.989307 0.200538 11.000000 -1.500000 H57B 2 0.405209 1.017853 0.161766 11.000000 -1.500000 H57C 2 0.500817 1.008989 0.115176 11.000000 -1.500000 AFIX 0 C58 1 0.444470 0.900124 0.102763 11.000000 0.057330 = 0.040510 0.094920 0.001730 -0.046380 -0.013790 C59 1 0.417037 0.937683 0.048883 11.000000 0.126080 = 0.047940 0.139460 0.008010 -0.088280 -0.025100 AFIX 43 H59 2 0.409791 0.991020 0.042027 11.000000 -1.200000 AFIX 0 C60 1 0.399527 0.902100 0.004373 11.000000 0.260390 = 0.058800 0.189780 0.018450 -0.173190 -0.062300 AFIX 43 H60 2 0.379662 0.929622 -0.032745 11.000000 -1.200000 AFIX 0 C61 1 0.411490 0.824433 0.014690 11.000000 0.173930 = 0.054130 0.110870 0.023060 -0.118170 -0.033690 AFIX 43 H61 2 0.400824 0.798684 -0.016949 11.000000 -1.200000 AFIX 0 C62 1 0.438364 0.782777 0.069237 11.000000 0.067020 = 0.040450 0.058250 0.002300 -0.039090 -0.025840 C63 1 0.455561 0.820242 0.116006 11.000000 0.032970 = 0.034160 0.061450 -0.000990 -0.025140 -0.006760 C64 1 0.452582 0.700382 0.074654 11.000000 0.043270 = 0.050350 0.039590 -0.011680 -0.018170 -0.011680 AFIX 43 H64 2 0.448002 0.679316 0.036764 11.000000 -1.200000 AFIX 0 C65 1 0.514257 0.531962 0.154749 11.000000 0.016950 = 0.034550 0.028240 -0.016930 -0.003610 -0.004820 C66 1 0.541487 0.451555 0.139891 11.000000 0.028450 = 0.035690 0.036440 -0.010520 -0.009560 -0.012810 C67 1 0.517933 0.423256 0.087505 11.000000 0.036200 = 0.037900 0.055520 -0.022640 -0.024070 0.004370 AFIX 137 H67A 2 0.566195 0.392146 0.056638 11.000000 -1.500000 H67B 2 0.496578 0.465836 0.057969 11.000000 -1.500000 H67C 2 0.475360 0.392963 0.113062 11.000000 -1.500000 AFIX 0 C68 1 0.215699 0.495199 0.348355 11.000000 0.048930 = 0.060470 0.094410 -0.026230 -0.004970 -0.026120 AFIX 137 H68A 2 0.198423 0.483552 0.400676 11.000000 -1.500000 H68B 2 0.244257 0.448967 0.325603 11.000000 -1.500000 H68C 2 0.167247 0.516904 0.333736 11.000000 -1.500000 AFIX 0 C69 1 0.243846 0.611173 0.361154 11.000000 0.019780 = 0.047040 0.054280 -0.016590 -0.013230 0.002020 C70 1 0.166150 0.631852 0.409035 11.000000 0.023770 = 0.074650 0.067520 -0.033050 -0.003510 -0.006400 AFIX 43 H70 2 0.127426 0.599851 0.419994 11.000000 -1.200000 AFIX 0 C71 1 0.142707 0.696581 0.441322 11.000000 0.067050 = 0.042590 0.041700 -0.004710 0.006290 0.012060 AFIX 43 H71 2 0.087664 0.712126 0.471079 11.000000 -1.200000 AFIX 0 C72 1 0.205223 0.740326 0.428251 11.000000 0.020120 = 0.056860 0.048360 -0.026880 -0.007090 0.001740 AFIX 43 H72 2 0.192004 0.783837 0.452416 11.000000 -1.200000 AFIX 0 C73 1 0.284908 0.719980 0.380719 11.000000 0.023990 = 0.039080 0.035100 -0.013940 -0.012100 0.004070 C74 1 0.305986 0.654051 0.345673 11.000000 0.019380 = 0.048430 0.030220 -0.010060 -0.004510 -0.001880 C75 1 0.344633 0.765728 0.374324 11.000000 0.026230 = 0.040240 0.036840 -0.024200 -0.014560 0.011830 AFIX 43 H75 2 0.325828 0.806234 0.403144 11.000000 -1.200000 AFIX 0 C76 1 0.540750 0.790988 0.309594 11.000000 0.034280 = 0.028660 0.043440 -0.014950 -0.019260 0.000890 C77 1 0.596448 0.831729 0.322413 11.000000 0.038730 = 0.044300 0.085240 -0.051830 -0.027360 0.009850 C78 1 0.562658 0.898992 0.364457 11.000000 0.054710 = 0.106690 0.156700 -0.110610 -0.030260 0.011550 AFIX 137 H78A 2 0.606700 0.926608 0.356243 11.000000 -1.500000 H78B 2 0.540629 0.882102 0.415740 11.000000 -1.500000 H78C 2 0.518668 0.932018 0.348738 11.000000 -1.500000 AFIX 0 C79 1 0.788197 0.228924 0.790259 11.000000 0.177480 = 0.096690 0.080690 -0.006160 -0.037120 -0.051350 AFIX 23 H79A 2 0.741564 0.238804 0.771768 11.000000 -1.200000 H79B 2 0.766758 0.243478 0.839737 11.000000 -1.200000 AFIX 0 C80 1 0.850598 0.275009 0.743889 11.000000 0.149660 = 0.277820 0.161770 0.039180 -0.063470 0.033980 AFIX 33 H80A 2 0.825174 0.328451 0.743693 11.000000 -1.500000 H80B 2 0.871329 0.260976 0.694797 11.000000 -1.500000 H80C 2 0.896280 0.265873 0.762719 11.000000 -1.500000 AFIX 0 C81 1 0.809119 0.105294 0.725503 11.000000 1.074820 = 0.103230 0.203540 -0.006080 -0.033680 -0.013090 AFIX 23 H81A 2 0.778936 0.062952 0.740646 11.000000 -1.200000 H81B 2 0.784541 0.146918 0.696388 11.000000 -1.200000 AFIX 0 C82 1 0.902033 0.082699 0.695403 11.000000 0.172560 = 0.382560 0.230110 0.087940 -0.037440 -0.093140 AFIX 33 H82A 2 0.917322 0.060280 0.650581 11.000000 -1.500000 H82B 2 0.921717 0.045955 0.730275 11.000000 -1.500000 H82C 2 0.927035 0.127279 0.685925 11.000000 -1.500000 AFIX 0 C83 1 0.765756 0.107703 0.870885 11.000000 0.103420 = 0.374330 0.866670 -0.353560 0.078440 -0.100520 AFIX 23 H83A 2 0.773635 0.122335 0.912665 11.000000 -1.200000 H83B 2 0.707338 0.120053 0.873661 11.000000 -1.200000 AFIX 0 C84 1 0.810403 0.028710 0.850827 11.000000 0.264240 = 0.930060 0.497210 -0.194440 0.120490 -0.087780 AFIX 33 H84A 2 0.789442 -0.008626 0.890854 11.000000 -1.500000 H84B 2 0.869520 0.024502 0.840629 11.000000 -1.500000 H84C 2 0.800840 0.019664 0.808151 11.000000 -1.500000 AFIX 0 C85 1 0.991427 0.062127 0.870764 11.000000 0.440400 = 0.070110 0.141270 0.055390 -0.030790 0.025240 AFIX 137 H85A 2 0.950808 0.029430 0.884122 11.000000 -1.500000 H85B 2 0.991966 0.079036 0.914112 11.000000 -1.500000 H85C 2 1.046034 0.034153 0.846093 11.000000 -1.500000 AFIX HKLF 4 END HKLF 4 REM SST_142_12_DyOAcL4_09_22_2012 in P-1 REM R1= 0.0465 for 15605 Fo > 4sig(Fo) and 0.0640 for all 20819 data REM 1357 parameters refined using 6 restraints ; data_4 _database_code_depnum_ccdc_archive 'CCDC 910741' #TrackingRef 'Revised_Ln6_Combined_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H26 Dy N7 O12, C3 H7 N O' _chemical_formula_sum 'C20 H33 Dy N8 O13' _chemical_formula_weight 756.04 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' Dy Dy -0.1892 4.4098 '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 7.7721(6) _cell_length_b 13.3326(5) _cell_length_c 16.0765(4) _cell_angle_alpha 113.456(2) _cell_angle_beta 101.544(18) _cell_angle_gamma 93.977(15) _cell_volume 1476.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5376 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 29.6 _exptl_crystal_description Prism _exptl_crystal_colour 'Light Yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 2.605 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_correction_T_min 0.306 _exptl_absorpt_process_details 'T. Higashi, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _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 11976 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5949 _reflns_number_gt 5786 _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 'SIR2008: J. Appl. Cryst. (2007). 40, 609-613' _computing_structure_refinement 'SHELXL-97: Acta Cryst.2008, A64, 112-122' _computing_molecular_graphics 'OLEX2: J. Appl. Cryst. (2009). 42, 339-341' _computing_publication_material 'OLEX2: J. Appl. Cryst. (2009). 42, 339-341' _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^)+(0.0309P)^2^+1.7704P] 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 5949 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.362256(17) 0.855060(10) 0.201367(9) 0.02243(6) Uani 1 1 d . . . O5 O 0.5338(3) 0.89511(19) 0.10881(17) 0.0344(5) Uani 1 1 d . . . O3 O 0.1945(3) 0.71044(17) 0.21687(16) 0.0296(5) Uani 1 1 d . . . O11 O 0.4929(3) 0.8698(2) 0.36042(18) 0.0356(5) Uani 1 1 d . . . O10 O 0.6791(3) 0.9307(2) 0.30205(18) 0.0361(6) Uani 1 1 d . . . O4 O -0.1462(3) 0.56566(19) 0.35699(18) 0.0336(5) Uani 1 1 d . . . H4 H -0.2368 0.5766 0.3783 0.050 Uiso 1 1 calc R . . N7 N 0.1397(3) 0.9143(2) 0.30105(18) 0.0225(5) Uani 1 1 d . . . O1 O 0.4614(4) 1.21996(19) 0.23702(18) 0.0378(6) Uani 1 1 d . . . N9 N 0.0649(3) 0.8295(2) 0.31982(19) 0.0251(5) Uani 1 1 d . . . H9 H -0.0026 0.8422 0.3597 0.030 Uiso 1 1 calc R . . O13 O -0.4359(3) 0.5893(2) 0.41605(19) 0.0391(6) Uani 1 1 d . . . C8 C 0.1008(4) 0.7288(2) 0.2746(2) 0.0231(6) Uani 1 1 d . . . N5 N -0.6003(4) 0.7097(2) 0.4962(2) 0.0321(6) Uani 1 1 d . . . O12 O 0.7755(3) 0.9143(2) 0.43147(18) 0.0419(6) Uani 1 1 d . . . N4 N 0.6523(4) 0.9055(2) 0.3666(2) 0.0290(6) Uani 1 1 d . . . N2 N 0.6855(3) 0.5794(2) 0.0970(2) 0.0272(6) Uani 1 1 d . . . N1 N 0.7281(4) 1.0099(3) 0.0851(2) 0.0354(7) Uani 1 1 d . . . O6 O 0.5271(3) 0.7072(2) 0.16968(19) 0.0386(6) Uani 1 1 d . . . O8 O 0.0753(4) 0.8423(2) 0.09335(19) 0.0495(7) Uani 1 1 d . . . N19 N -0.0892(4) 0.6554(2) 0.34082(19) 0.0275(6) Uani 1 1 d . . . O7 O 0.2328(4) 0.7207(2) 0.03618(19) 0.0473(7) Uani 1 1 d . . . C7 C 0.0934(4) 1.0094(3) 0.3428(2) 0.0254(6) Uani 1 1 d . . . H7 H 0.0146 1.0139 0.3819 0.030 Uiso 1 1 calc R . . C9 C 0.0316(4) 0.6356(2) 0.2947(2) 0.0237(6) Uani 1 1 d . . . C6 C 0.2830(4) 1.1148(2) 0.2850(2) 0.0243(6) Uani 1 1 d . . . C19 C -0.7018(5) 0.6281(3) 0.5148(3) 0.0409(9) Uani 1 1 d . . . H19A H -0.7025 0.6592 0.5812 0.061 Uiso 1 1 calc R . . H19B H -0.6466 0.5612 0.4995 0.061 Uiso 1 1 calc R . . H19C H -0.8243 0.6091 0.4763 0.061 Uiso 1 1 calc R . . O9 O -0.0262(5) 0.7136(3) -0.0490(2) 0.0602(9) Uani 1 1 d . . . C1 C 0.3304(4) 1.2188(3) 0.2827(2) 0.0294(7) Uani 1 1 d . . . C5 C 0.1528(4) 1.1096(2) 0.3345(2) 0.0261(6) Uani 1 1 d . . . N3 N 0.0901(4) 0.7574(3) 0.0242(2) 0.0386(7) Uani 1 1 d . . . C4 C 0.0756(5) 1.2032(3) 0.3775(3) 0.0354(8) Uani 1 1 d . . . H4A H -0.0118 1.1983 0.4100 0.042 Uiso 1 1 calc R . . C11 C 0.6356(5) 0.9846(3) 0.1361(3) 0.0342(8) Uani 1 1 d . . . H11 H 0.6471 1.0382 0.1982 0.041 Uiso 1 1 calc R . . C2 C 0.2531(5) 1.3090(3) 0.3257(3) 0.0367(8) Uani 1 1 d . . . H2 H 0.2875 1.3772 0.3230 0.044 Uiso 1 1 calc R . . C10 C 0.1062(5) 0.5309(3) 0.2599(3) 0.0334(7) Uani 1 1 d . . . H10A H 0.0800 0.4991 0.1914 0.050 Uiso 1 1 calc R . . H10B H 0.0523 0.4781 0.2796 0.050 Uiso 1 1 calc R . . H10C H 0.2355 0.5468 0.2859 0.050 Uiso 1 1 calc R . . C18 C -0.6395(5) 0.8219(3) 0.5331(3) 0.0408(8) Uani 1 1 d . . . H18A H -0.7592 0.8228 0.4997 0.061 Uiso 1 1 calc R . . H18B H -0.5520 0.8711 0.5245 0.061 Uiso 1 1 calc R . . H18C H -0.6338 0.8473 0.5999 0.061 Uiso 1 1 calc R . . C3 C 0.1243(5) 1.3010(3) 0.3732(3) 0.0428(9) Uani 1 1 d . . . H3 H 0.0708 1.3635 0.4025 0.051 Uiso 1 1 calc R . . C14 C 0.6353(4) 0.6767(3) 0.1211(2) 0.0305(7) Uani 1 1 d . . . H14 H 0.6845 0.7268 0.1001 0.037 Uiso 1 1 calc R . . C17 C -0.4729(4) 0.6836(3) 0.4514(2) 0.0320(7) Uani 1 1 d . . . H17 H -0.4048 0.7416 0.4459 0.038 Uiso 1 1 calc R . . C16 C 0.6170(5) 0.4990(3) 0.1283(3) 0.0359(8) Uani 1 1 d . . . H16A H 0.5372 0.5314 0.1682 0.054 Uiso 1 1 calc R . . H16B H 0.7167 0.4796 0.1638 0.054 Uiso 1 1 calc R . . H16C H 0.5514 0.4321 0.0737 0.054 Uiso 1 1 calc R . . C13 C 0.7167(6) 0.9333(4) -0.0100(3) 0.0491(10) Uani 1 1 d . . . H13A H 0.8163 0.8918 -0.0112 0.074 Uiso 1 1 calc R . . H13B H 0.7223 0.9744 -0.0484 0.074 Uiso 1 1 calc R . . H13C H 0.6040 0.8815 -0.0349 0.074 Uiso 1 1 calc R . . C12 C 0.8455(7) 1.1153(4) 0.1224(4) 0.0661(14) Uani 1 1 d . . . H12A H 0.8009 1.1586 0.0882 0.099 Uiso 1 1 calc R . . H12B H 0.9655 1.1023 0.1154 0.099 Uiso 1 1 calc R . . H12C H 0.8496 1.1563 0.1889 0.099 Uiso 1 1 calc R . . C15 C 0.8094(5) 0.5464(3) 0.0373(3) 0.0400(8) Uani 1 1 d . . . H15A H 0.8379 0.6049 0.0175 0.060 Uiso 1 1 calc R . . H15B H 0.7544 0.4775 -0.0180 0.060 Uiso 1 1 calc R . . H15C H 0.9188 0.5347 0.0722 0.060 Uiso 1 1 calc R . . C43 C 0.4975(7) 1.3168(3) 0.2207(3) 0.0530(11) Uani 1 1 d . . . H43A H 0.3881 1.3278 0.1852 0.080 Uiso 1 1 calc R . . H43B H 0.5884 1.3070 0.1850 0.080 Uiso 1 1 calc R . . H43C H 0.5408 1.3818 0.2809 0.080 Uiso 1 1 calc R . . O2 O 0.3609(3) 1.03192(17) 0.24517(16) 0.0281(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02497(9) 0.01774(8) 0.02801(10) 0.01033(6) 0.01207(6) 0.00490(6) O5 0.0458(14) 0.0279(12) 0.0363(13) 0.0144(10) 0.0234(11) 0.0051(10) O3 0.0350(12) 0.0200(10) 0.0368(13) 0.0107(9) 0.0186(10) 0.0040(9) O11 0.0278(12) 0.0486(15) 0.0398(14) 0.0249(12) 0.0147(10) 0.0068(10) O10 0.0311(12) 0.0447(14) 0.0408(14) 0.0266(12) 0.0102(10) 0.0017(11) O4 0.0361(13) 0.0277(12) 0.0471(15) 0.0217(11) 0.0200(11) 0.0044(10) N7 0.0210(12) 0.0199(12) 0.0297(13) 0.0128(10) 0.0081(10) 0.0025(9) O1 0.0513(15) 0.0238(11) 0.0454(15) 0.0178(11) 0.0221(12) 0.0014(10) N9 0.0265(13) 0.0214(12) 0.0312(14) 0.0135(11) 0.0110(11) 0.0021(10) O13 0.0396(14) 0.0341(13) 0.0485(15) 0.0166(12) 0.0227(12) 0.0071(11) C8 0.0204(14) 0.0213(14) 0.0288(16) 0.0119(12) 0.0062(12) 0.0022(11) N5 0.0345(15) 0.0302(14) 0.0315(15) 0.0117(12) 0.0105(12) 0.0061(12) O12 0.0300(13) 0.0584(17) 0.0387(14) 0.0249(13) 0.0027(11) 0.0059(12) N4 0.0247(13) 0.0298(14) 0.0360(15) 0.0156(12) 0.0104(12) 0.0083(11) N2 0.0249(13) 0.0253(13) 0.0355(15) 0.0150(12) 0.0104(11) 0.0070(10) N1 0.0302(15) 0.0497(18) 0.0375(16) 0.0277(15) 0.0133(12) 0.0051(13) O6 0.0403(14) 0.0345(13) 0.0526(16) 0.0210(12) 0.0258(12) 0.0199(11) O8 0.0529(17) 0.0501(17) 0.0360(15) 0.0109(13) 0.0035(13) 0.0162(14) N19 0.0279(13) 0.0241(13) 0.0344(15) 0.0159(11) 0.0095(11) 0.0011(10) O7 0.0632(19) 0.0343(14) 0.0354(15) 0.0052(11) 0.0131(13) 0.0073(13) C7 0.0210(14) 0.0252(15) 0.0295(16) 0.0109(13) 0.0071(12) 0.0019(11) C9 0.0233(14) 0.0220(14) 0.0267(15) 0.0123(12) 0.0050(12) -0.0001(11) C6 0.0240(14) 0.0195(14) 0.0265(15) 0.0083(12) 0.0033(12) 0.0024(11) C19 0.0385(19) 0.045(2) 0.044(2) 0.0207(18) 0.0179(16) -0.0001(16) O9 0.074(2) 0.0552(18) 0.0364(16) 0.0209(14) -0.0116(15) -0.0204(16) C1 0.0347(17) 0.0226(15) 0.0311(17) 0.0125(13) 0.0068(13) 0.0019(13) C5 0.0241(14) 0.0184(14) 0.0336(17) 0.0084(12) 0.0074(13) 0.0056(11) N3 0.0482(19) 0.0329(16) 0.0334(16) 0.0179(13) 0.0036(14) -0.0071(14) C4 0.0300(17) 0.0269(16) 0.050(2) 0.0128(15) 0.0161(15) 0.0097(13) C11 0.042(2) 0.0336(18) 0.0310(18) 0.0146(15) 0.0181(15) 0.0015(15) C2 0.043(2) 0.0215(15) 0.046(2) 0.0167(15) 0.0072(16) 0.0039(14) C10 0.0347(17) 0.0280(16) 0.044(2) 0.0188(15) 0.0143(15) 0.0089(13) C18 0.046(2) 0.0360(19) 0.037(2) 0.0093(16) 0.0134(16) 0.0109(16) C3 0.047(2) 0.0261(17) 0.058(3) 0.0157(17) 0.0193(19) 0.0147(15) C14 0.0321(17) 0.0256(15) 0.0377(18) 0.0154(14) 0.0124(14) 0.0065(13) C17 0.0302(17) 0.0322(17) 0.0337(18) 0.0131(14) 0.0115(14) 0.0005(13) C16 0.0410(19) 0.0297(17) 0.043(2) 0.0210(16) 0.0125(16) 0.0061(14) C13 0.050(2) 0.070(3) 0.040(2) 0.029(2) 0.0241(19) 0.017(2) C12 0.062(3) 0.073(3) 0.064(3) 0.033(3) 0.020(2) -0.022(3) C15 0.0371(19) 0.0378(19) 0.048(2) 0.0145(17) 0.0221(17) 0.0113(15) C43 0.081(3) 0.0297(19) 0.060(3) 0.0255(19) 0.031(2) 0.0001(19) O2 0.0309(11) 0.0178(10) 0.0383(13) 0.0106(9) 0.0169(10) 0.0043(8) _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 O2 2.177(2) . ? Dy1 O6 2.367(2) . ? Dy1 O5 2.367(2) . ? Dy1 O3 2.376(2) . ? Dy1 O11 2.478(2) . ? Dy1 O7 2.483(3) . ? Dy1 O8 2.486(3) . ? Dy1 O10 2.542(2) . ? Dy1 N7 2.545(3) . ? Dy1 N3 2.921(3) . ? Dy1 N4 2.926(3) . ? O5 C11 1.247(4) . ? O3 C8 1.251(4) . ? O11 N4 1.265(3) . ? O10 N4 1.262(4) . ? O4 N19 1.384(3) . ? N7 C7 1.292(4) . ? N7 N9 1.399(3) . ? O1 C1 1.372(4) . ? O1 C43 1.437(4) . ? N9 C8 1.329(4) . ? O13 C17 1.238(4) . ? C8 C9 1.495(4) . ? N5 C17 1.324(4) . ? N5 C18 1.453(5) . ? N5 C19 1.459(4) . ? O12 N4 1.227(4) . ? N2 C14 1.310(4) . ? N2 C15 1.461(4) . ? N2 C16 1.463(4) . ? N1 C11 1.314(4) . ? N1 C13 1.441(5) . ? N1 C12 1.449(5) . ? O6 C14 1.241(4) . ? O8 N3 1.264(4) . ? N19 C9 1.288(4) . ? O7 N3 1.254(4) . ? C7 C5 1.448(4) . ? C9 C10 1.489(4) . ? C6 O2 1.297(4) . ? C6 C5 1.422(4) . ? C6 C1 1.427(4) . ? O9 N3 1.224(4) . ? C1 C2 1.374(5) . ? C5 C4 1.407(4) . ? C4 C3 1.364(5) . ? C2 C3 1.398(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Dy1 O6 148.27(9) . . ? O2 Dy1 O5 78.41(8) . . ? O6 Dy1 O5 79.65(9) . . ? O2 Dy1 O3 134.96(8) . . ? O6 Dy1 O3 73.42(8) . . ? O5 Dy1 O3 144.21(8) . . ? O2 Dy1 O11 95.38(9) . . ? O6 Dy1 O11 77.92(9) . . ? O5 Dy1 O11 123.17(8) . . ? O3 Dy1 O11 73.74(8) . . ? O2 Dy1 O7 121.06(9) . . ? O6 Dy1 O7 72.69(10) . . ? O5 Dy1 O7 72.48(9) . . ? O3 Dy1 O7 77.24(9) . . ? O11 Dy1 O7 143.37(9) . . ? O2 Dy1 O8 82.02(9) . . ? O6 Dy1 O8 121.87(10) . . ? O5 Dy1 O8 93.07(10) . . ? O3 Dy1 O8 81.89(10) . . ? O11 Dy1 O8 142.57(9) . . ? O7 Dy1 O8 50.61(10) . . ? O2 Dy1 O10 80.16(9) . . ? O6 Dy1 O10 71.59(9) . . ? O5 Dy1 O10 72.75(8) . . ? O3 Dy1 O10 118.60(8) . . ? O11 Dy1 O10 50.71(8) . . ? O7 Dy1 O10 133.57(10) . . ? O8 Dy1 O10 159.11(10) . . ? O2 Dy1 N7 70.89(8) . . ? O6 Dy1 N7 132.47(8) . . ? O5 Dy1 N7 147.72(8) . . ? O3 Dy1 N7 64.23(8) . . ? O11 Dy1 N7 70.60(8) . . ? O7 Dy1 N7 115.39(9) . . ? O8 Dy1 N7 73.36(9) . . ? O10 Dy1 N7 110.50(8) . . ? O2 Dy1 N3 102.53(9) . . ? O6 Dy1 N3 97.06(10) . . ? O5 Dy1 N3 82.65(9) . . ? O3 Dy1 N3 77.81(8) . . ? O11 Dy1 N3 151.38(8) . . ? O7 Dy1 N3 25.19(10) . . ? O8 Dy1 N3 25.44(10) . . ? O10 Dy1 N3 154.28(9) . . ? N7 Dy1 N3 94.28(9) . . ? O2 Dy1 N4 89.37(8) . . ? O6 Dy1 N4 71.23(9) . . ? O5 Dy1 N4 97.80(9) . . ? O3 Dy1 N4 95.42(8) . . ? O11 Dy1 N4 25.39(7) . . ? O7 Dy1 N4 143.78(9) . . ? O8 Dy1 N4 164.52(9) . . ? O10 Dy1 N4 25.45(7) . . ? N7 Dy1 N4 91.69(8) . . ? N3 Dy1 N4 167.90(9) . . ? C11 O5 Dy1 123.5(2) . . ? C8 O3 Dy1 122.57(19) . . ? N4 O11 Dy1 97.51(18) . . ? N4 O10 Dy1 94.54(17) . . ? C7 N7 N9 114.5(2) . . ? C7 N7 Dy1 132.0(2) . . ? N9 N7 Dy1 113.31(17) . . ? C1 O1 C43 116.5(3) . . ? C8 N9 N7 116.7(2) . . ? O3 C8 N9 121.6(3) . . ? O3 C8 C9 119.1(3) . . ? N9 C8 C9 119.4(3) . . ? C17 N5 C18 121.6(3) . . ? C17 N5 C19 121.4(3) . . ? C18 N5 C19 116.9(3) . . ? O12 N4 O10 121.2(3) . . ? O12 N4 O11 122.1(3) . . ? O10 N4 O11 116.6(3) . . ? O12 N4 Dy1 172.8(2) . . ? O10 N4 Dy1 60.00(16) . . ? O11 N4 Dy1 57.10(16) . . ? C14 N2 C15 121.5(3) . . ? C14 N2 C16 120.9(3) . . ? C15 N2 C16 117.6(3) . . ? C11 N1 C13 121.0(3) . . ? C11 N1 C12 121.3(3) . . ? C13 N1 C12 117.7(3) . . ? C14 O6 Dy1 133.4(2) . . ? N3 O8 Dy1 96.9(2) . . ? C9 N19 O4 111.9(3) . . ? N3 O7 Dy1 97.4(2) . . ? N7 C7 C5 124.9(3) . . ? N19 C9 C10 126.8(3) . . ? N19 C9 C8 115.2(3) . . ? C10 C9 C8 118.0(3) . . ? O2 C6 C5 123.4(3) . . ? O2 C6 C1 120.1(3) . . ? C5 C6 C1 116.5(3) . . ? O1 C1 C2 124.5(3) . . ? O1 C1 C6 113.9(3) . . ? C2 C1 C6 121.6(3) . . ? C4 C5 C6 120.5(3) . . ? C4 C5 C7 117.3(3) . . ? C6 C5 C7 122.2(3) . . ? O9 N3 O7 122.2(4) . . ? O9 N3 O8 122.7(4) . . ? O7 N3 O8 115.1(3) . . ? O9 N3 Dy1 177.7(2) . . ? O7 N3 Dy1 57.46(17) . . ? O8 N3 Dy1 57.65(18) . . ? C3 C4 C5 121.1(3) . . ? O5 C11 N1 124.6(3) . . ? C1 C2 C3 120.5(3) . . ? C4 C3 C2 119.8(3) . . ? O6 C14 N2 123.8(3) . . ? O13 C17 N5 124.9(3) . . ? C6 O2 Dy1 145.89(19) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.958 _refine_diff_density_min -0.960 _refine_diff_density_rms 0.101 _iucr_refine_instructions_details ; TITL 4 CELL 0.71073 7.7721 13.3326 16.0765 113.456 101.544 93.977 ZERR 2 0.0006 0.0005 0.0004 0.002 0.018 0.015 LATT 1 SFAC C H N O Dy UNIT 40 66 16 26 2 L.S. 5 PLAN -15 TEMP -80 fmap 2 acta SHEL 8.14718 0.8 OMIT 0 1 1 OMIT 0 -1 2 OMIT -5 -4 2 OMIT 5 5 10 OMIT -6 -5 3 REM 4 WGHT 0.030900 1.770400 FVAR 0.62955 DY1 5 0.362256 0.855060 0.201367 11.00000 0.02497 0.01774 = 0.02801 0.01033 0.01207 0.00490 O5 4 0.533783 0.895106 0.108811 11.00000 0.04579 0.02787 = 0.03632 0.01444 0.02344 0.00513 O3 4 0.194462 0.710439 0.216870 11.00000 0.03503 0.02003 = 0.03677 0.01067 0.01861 0.00396 O11 4 0.492891 0.869765 0.360421 11.00000 0.02779 0.04859 = 0.03975 0.02489 0.01471 0.00684 O10 4 0.679147 0.930740 0.302048 11.00000 0.03106 0.04475 = 0.04083 0.02663 0.01025 0.00169 O4 4 -0.146186 0.565664 0.356985 11.00000 0.03612 0.02769 = 0.04709 0.02169 0.01998 0.00435 AFIX 147 H4 2 -0.236798 0.576605 0.378292 11.00000 -1.50000 AFIX 0 N7 3 0.139661 0.914299 0.301054 11.00000 0.02104 0.01990 = 0.02974 0.01283 0.00813 0.00249 O1 4 0.461375 1.219958 0.237020 11.00000 0.05130 0.02376 = 0.04537 0.01784 0.02206 0.00137 N9 3 0.064898 0.829495 0.319819 11.00000 0.02649 0.02144 = 0.03121 0.01352 0.01104 0.00208 AFIX 43 H9 2 -0.002600 0.842236 0.359653 11.00000 -1.20000 AFIX 0 O13 4 -0.435898 0.589341 0.416049 11.00000 0.03957 0.03410 = 0.04849 0.01658 0.02270 0.00710 C8 1 0.100778 0.728790 0.274564 11.00000 0.02042 0.02126 = 0.02878 0.01186 0.00622 0.00221 N5 3 -0.600307 0.709654 0.496196 11.00000 0.03453 0.03015 = 0.03150 0.01171 0.01054 0.00606 O12 4 0.775471 0.914267 0.431465 11.00000 0.03001 0.05835 = 0.03873 0.02490 0.00267 0.00593 N4 3 0.652255 0.905457 0.366644 11.00000 0.02470 0.02985 = 0.03596 0.01563 0.01035 0.00830 N2 3 0.685486 0.579365 0.097022 11.00000 0.02492 0.02526 = 0.03551 0.01500 0.01039 0.00699 N1 3 0.728075 1.009911 0.085075 11.00000 0.03023 0.04967 = 0.03745 0.02766 0.01328 0.00511 O6 4 0.527117 0.707174 0.169676 11.00000 0.04031 0.03446 = 0.05255 0.02104 0.02581 0.01990 O8 4 0.075273 0.842275 0.093354 11.00000 0.05291 0.05005 = 0.03602 0.01092 0.00349 0.01619 N19 3 -0.089209 0.655377 0.340825 11.00000 0.02786 0.02412 = 0.03437 0.01594 0.00955 0.00112 O7 4 0.232845 0.720718 0.036177 11.00000 0.06317 0.03427 = 0.03545 0.00523 0.01308 0.00730 C7 1 0.093430 1.009372 0.342815 11.00000 0.02095 0.02515 = 0.02949 0.01093 0.00706 0.00189 AFIX 43 H7 2 0.014587 1.013868 0.381872 11.00000 -1.20000 AFIX 0 C9 1 0.031581 0.635603 0.294685 11.00000 0.02333 0.02201 = 0.02668 0.01232 0.00498 -0.00014 C6 1 0.283017 1.114765 0.284970 11.00000 0.02404 0.01946 = 0.02650 0.00828 0.00329 0.00241 C19 1 -0.701771 0.628080 0.514826 11.00000 0.03854 0.04484 = 0.04383 0.02070 0.01790 -0.00011 AFIX 137 H19A 2 -0.702528 0.659159 0.581172 11.00000 -1.50000 H19B 2 -0.646600 0.561185 0.499498 11.00000 -1.50000 H19C 2 -0.824326 0.609110 0.476320 11.00000 -1.50000 AFIX 0 O9 4 -0.026151 0.713562 -0.049011 11.00000 0.07370 0.05519 = 0.03643 0.02088 -0.01156 -0.02035 C1 1 0.330384 1.218811 0.282669 11.00000 0.03471 0.02263 = 0.03107 0.01255 0.00683 0.00188 C5 1 0.152784 1.109579 0.334546 11.00000 0.02411 0.01841 = 0.03361 0.00839 0.00737 0.00559 N3 3 0.090088 0.757369 0.024233 11.00000 0.04819 0.03291 = 0.03340 0.01789 0.00358 -0.00712 C4 1 0.075595 1.203227 0.377487 11.00000 0.02999 0.02686 = 0.04967 0.01282 0.01609 0.00973 AFIX 43 H4A 2 -0.011842 1.198290 0.409991 11.00000 -1.20000 AFIX 0 C11 1 0.635602 0.984582 0.136125 11.00000 0.04248 0.03360 = 0.03100 0.01461 0.01809 0.00147 AFIX 43 H11 2 0.647135 1.038210 0.198203 11.00000 -1.20000 AFIX 0 C2 1 0.253099 1.308985 0.325651 11.00000 0.04334 0.02153 = 0.04569 0.01666 0.00720 0.00392 AFIX 43 H2 2 0.287474 1.377233 0.323026 11.00000 -1.20000 AFIX 0 C10 1 0.106226 0.530933 0.259944 11.00000 0.03466 0.02801 = 0.04391 0.01882 0.01428 0.00890 AFIX 137 H10A 2 0.080038 0.499051 0.191447 11.00000 -1.50000 H10B 2 0.052305 0.478109 0.279586 11.00000 -1.50000 H10C 2 0.235459 0.546753 0.285937 11.00000 -1.50000 AFIX 0 C18 1 -0.639530 0.821851 0.533067 11.00000 0.04618 0.03601 = 0.03654 0.00934 0.01339 0.01090 AFIX 137 H18A 2 -0.759191 0.822770 0.499664 11.00000 -1.50000 H18B 2 -0.552029 0.871106 0.524491 11.00000 -1.50000 H18C 2 -0.633820 0.847342 0.599913 11.00000 -1.50000 AFIX 0 C3 1 0.124269 1.301040 0.373212 11.00000 0.04662 0.02607 = 0.05804 0.01571 0.01934 0.01471 AFIX 43 H3 2 0.070791 1.363538 0.402458 11.00000 -1.20000 AFIX 0 C14 1 0.635286 0.676691 0.121075 11.00000 0.03210 0.02559 = 0.03772 0.01540 0.01242 0.00654 AFIX 43 H14 2 0.684539 0.726816 0.100098 11.00000 -1.20000 AFIX 0 C17 1 -0.472921 0.683594 0.451378 11.00000 0.03022 0.03218 = 0.03365 0.01311 0.01147 0.00054 AFIX 43 H17 2 -0.404804 0.741640 0.445935 11.00000 -1.20000 AFIX 0 C16 1 0.617032 0.498962 0.128266 11.00000 0.04104 0.02967 = 0.04342 0.02104 0.01251 0.00611 AFIX 137 H16A 2 0.537199 0.531378 0.168238 11.00000 -1.50000 H16B 2 0.716653 0.479603 0.163793 11.00000 -1.50000 H16C 2 0.551397 0.432055 0.073693 11.00000 -1.50000 AFIX 0 C13 1 0.716741 0.933259 -0.009973 11.00000 0.04995 0.06968 = 0.04042 0.02872 0.02412 0.01728 AFIX 137 H13A 2 0.816254 0.891825 -0.011239 11.00000 -1.50000 H13B 2 0.722280 0.974351 -0.048398 11.00000 -1.50000 H13C 2 0.603982 0.881485 -0.034907 11.00000 -1.50000 AFIX 0 C12 1 0.845507 1.115274 0.122398 11.00000 0.06233 0.07290 = 0.06435 0.03323 0.02050 -0.02221 AFIX 137 H12A 2 0.800883 1.158554 0.088161 11.00000 -1.50000 H12B 2 0.965455 1.102296 0.115419 11.00000 -1.50000 H12C 2 0.849627 1.156254 0.188863 11.00000 -1.50000 AFIX 0 C15 1 0.809354 0.546409 0.037257 11.00000 0.03707 0.03782 = 0.04778 0.01449 0.02209 0.01134 AFIX 137 H15A 2 0.837907 0.604928 0.017497 11.00000 -1.50000 H15B 2 0.754427 0.477469 -0.018030 11.00000 -1.50000 H15C 2 0.918789 0.534730 0.072226 11.00000 -1.50000 AFIX 0 C43 1 0.497546 1.316820 0.220731 11.00000 0.08051 0.02974 = 0.06024 0.02553 0.03118 0.00008 AFIX 137 H43A 2 0.388108 1.327813 0.185220 11.00000 -1.50000 H43B 2 0.588362 1.306961 0.185004 11.00000 -1.50000 H43C 2 0.540842 1.381764 0.280857 11.00000 -1.50000 AFIX 0 O2 4 0.360942 1.031917 0.245170 11.00000 0.03095 0.01775 = 0.03829 0.01061 0.01686 0.00429 HKLF 4 REM 4 REM R1 = 0.0281 for 5786 Fo > 4sig(Fo) and 0.0289 for all 5949 data REM 388 parameters refined using 0 restraints END WGHT 0.0309 1.7719 REM Highest difference peak 0.958, deepest hole -0.960, 1-sigma level 0.101 Q1 1 0.9169 0.4389 0.3990 11.00000 0.05 0.96 Q2 1 0.3580 0.8752 0.1293 11.00000 0.05 0.57 Q3 1 0.2083 0.8607 0.2440 11.00000 0.05 0.55 Q4 1 0.4857 0.8380 0.1496 11.00000 0.05 0.45 Q5 1 0.3808 0.9423 0.2775 11.00000 0.05 0.43 Q6 1 0.3016 0.9207 0.2481 11.00000 0.05 0.43 Q7 1 0.2677 0.7754 0.2221 11.00000 0.05 0.42 Q8 1 0.2241 0.6881 0.0837 11.00000 0.05 0.41 Q9 1 0.3785 0.8389 0.2764 11.00000 0.05 0.41 Q10 1 0.5969 0.7801 0.2078 11.00000 0.05 0.41 Q11 1 0.3009 1.1670 0.2791 11.00000 0.05 0.38 Q12 1 0.2692 0.7594 0.1301 11.00000 0.05 0.38 Q13 1 0.4254 0.7868 0.1757 11.00000 0.05 0.37 Q14 1 0.3438 0.8207 0.0505 11.00000 0.05 0.37 Q15 1 0.7014 0.9860 0.1908 11.00000 0.05 0.37 ; data_5-Revised _database_code_depnum_ccdc_archive 'CCDC 910742' #TrackingRef 'Revised_Ln6_Combined_CIF.cif' # start Validation Reply Form _vrf_PLAT003_5-Revised ; PROBLEM: RESPONSE: Please see refine_special_details for more information. ; _vrf_PLAT860_5-Revised ; PROBLEM: RESPONSE: Please see refine_special_details for more information. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H49 N9 O15 Yb2' _chemical_formula_weight 1181.90 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' Yb Yb -0.3850 5.5486 '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 8.862(2) _cell_length_b 13.616(3) _cell_length_c 18.749(5) _cell_angle_alpha 85.267(8) _cell_angle_beta 84.683(7) _cell_angle_gamma 72.526(7) _cell_volume 2145.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 8800 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour 'Light Yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 4.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.316 _exptl_absorpt_correction_T_max 0.414 _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 17939 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.1062 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8778 _reflns_number_gt 7313 _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. An isotropic restraint (ISOR 0.025 0.05 O6) was applied to atom O6, which lies between the two heavy atoms Yb1 and Yb2. For the same reason, a similarity restraing (SIMU 0.025 0.05 1.7 C14 O6) was applied to the bonded atoms O6 and C14, in order to help compensate for apparent heavy atom effects on the adjacent light atom (O6). ; _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^)+(0.0000P)^2^+129.8149P] 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 8778 _refine_ls_number_parameters 564 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.1085 _refine_ls_wR_factor_ref 0.2416 _refine_ls_wR_factor_gt 0.2338 _refine_ls_goodness_of_fit_ref 1.210 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.79514(8) 0.90947(5) 0.22666(4) 0.0199(2) Uani 1 1 d . . . Yb2 Yb 0.94897(8) 0.62289(5) 0.22333(4) 0.0190(2) Uani 1 1 d . . . O1 O 0.8961(16) 0.4834(9) 0.3773(7) 0.034(3) Uani 1 1 d . . . H1 H 0.9563 0.4414 0.3492 0.041 Uiso 1 1 calc R . . O2 O 0.8897(13) 0.7620(8) 0.2973(6) 0.020(2) Uani 1 1 d . . . O3 O 0.6286(13) 1.0644(8) 0.2233(7) 0.026(3) Uani 1 1 d . . . O4 O 0.4399(15) 1.2258(10) 0.1633(7) 0.036(3) Uani 1 1 d . . . O5 O 0.6466(16) 1.0460(9) 0.0772(8) 0.035(3) Uani 1 1 d . . . H5 H 0.7125 1.0697 0.0520 0.042 Uiso 1 1 calc R . . O6 O 0.8809(13) 0.7727(7) 0.1551(6) 0.019(2) Uani 1 1 d U . . O7 O 0.9405(13) 0.4674(8) 0.2267(7) 0.025(3) Uani 1 1 d . . . O8 O 0.8921(15) 0.3055(9) 0.2936(8) 0.034(3) Uani 1 1 d . . . O9 O 0.5799(13) 0.8442(9) 0.2333(7) 0.027(3) Uani 1 1 d . . . O10 O 0.6747(13) 0.6694(9) 0.2372(6) 0.024(2) Uani 1 1 d . . . O11 O 0.9796(14) 0.9701(10) 0.2811(7) 0.033(3) Uani 1 1 d . . . O12 O 1.0217(16) 0.9472(11) 0.1653(7) 0.038(3) Uani 1 1 d . . . O13 O 1.1770(13) 0.6256(10) 0.1458(8) 0.035(3) Uani 1 1 d . . . O14 O 1.1839(14) 0.5512(11) 0.2790(7) 0.035(3) Uani 1 1 d . . . O15 O 0.139(3) 0.7121(17) 0.4545(12) 0.078(6) Uani 1 1 d . . . N1 N 0.8819(15) 0.5826(11) 0.3499(8) 0.024(3) Uani 1 1 d . . . N2 N 0.7267(18) 0.8351(11) 0.3957(8) 0.027(3) Uani 1 1 d . . . N3 N 0.6886(16) 0.9253(10) 0.3489(8) 0.024(3) Uani 1 1 d . . . N4 N 0.7210(16) 0.9456(10) 0.1021(7) 0.020(3) Uani 1 1 d . . . N5 N 0.8379(17) 0.6929(10) 0.0575(8) 0.024(3) Uani 1 1 d . . . N6 N 0.8791(17) 0.6035(11) 0.1031(8) 0.027(3) Uani 1 1 d . . . N7 N 1.3589(18) 0.6958(13) 0.0875(8) 0.034(4) Uani 1 1 d . . . N8 N 1.4044(18) 0.4986(13) 0.3413(10) 0.038(4) Uani 1 1 d . . . N9 N 0.209(2) 0.8587(17) 0.4521(11) 0.052(5) Uani 1 1 d . . . C1 C 0.811(2) 0.6340(15) 0.4752(10) 0.034(4) Uani 1 1 d . . . H1A H 0.8102 0.5625 0.4857 0.040 Uiso 1 1 calc R . . H1B H 0.7086 0.6810 0.4911 0.040 Uiso 1 1 calc R . . H1C H 0.8952 0.6465 0.5006 0.040 Uiso 1 1 calc R . . C2 C 0.8422(18) 0.6521(12) 0.3971(9) 0.022(3) Uani 1 1 d . . . C3 C 0.8234(18) 0.7577(13) 0.3619(9) 0.022(3) Uani 1 1 d . . . C4 C 0.5810(18) 1.0010(13) 0.3766(9) 0.022(3) Uani 1 1 d . . . H4 H 0.5526 0.9927 0.4264 0.026 Uiso 1 1 calc R . . C5 C 0.4985(18) 1.0972(13) 0.3407(10) 0.024(4) Uani 1 1 d . . . C6 C 0.373(2) 1.1657(15) 0.3819(11) 0.033(4) Uani 1 1 d . . . H6 H 0.3570 1.1503 0.4318 0.039 Uiso 1 1 calc R . . C7 C 0.2772(19) 1.2529(15) 0.3502(10) 0.030(4) Uani 1 1 d . . . H7 H 0.1954 1.2982 0.3786 0.036 Uiso 1 1 calc R . . C8 C 0.297(2) 1.2763(14) 0.2772(10) 0.030(4) Uani 1 1 d . . . H8 H 0.2312 1.3382 0.2561 0.036 Uiso 1 1 calc R . . C9 C 0.414(2) 1.2090(13) 0.2348(10) 0.027(4) Uani 1 1 d . . . C10 C 0.5201(18) 1.1202(12) 0.2651(10) 0.025(4) Uani 1 1 d . . . C11 C 0.330(3) 1.3137(15) 0.1294(11) 0.041(5) Uani 1 1 d . . . H11A H 0.2208 1.3138 0.1449 0.050 Uiso 1 1 calc R . . H11B H 0.3460 1.3098 0.0772 0.050 Uiso 1 1 calc R . . H11C H 0.3468 1.3772 0.1430 0.050 Uiso 1 1 calc R . . C12 C 0.753(3) 0.8955(16) -0.0235(10) 0.038(5) Uani 1 1 d . . . H12A H 0.6411 0.9260 -0.0330 0.046 Uiso 1 1 calc R . . H12B H 0.7949 0.8296 -0.0463 0.046 Uiso 1 1 calc R . . H12C H 0.8133 0.9425 -0.0431 0.046 Uiso 1 1 calc R . . C13 C 0.7676(19) 0.8780(14) 0.0556(10) 0.028(4) Uani 1 1 d . . . C14 C 0.8346(19) 0.7748(14) 0.0895(9) 0.024(3) Uani 1 1 d U . . C15 C 0.8709(19) 0.5211(12) 0.0752(9) 0.020(3) Uani 1 1 d . . . H15 H 0.8591 0.5255 0.0251 0.025 Uiso 1 1 calc R . . C16 C 0.8779(18) 0.4245(13) 0.1131(10) 0.027(4) Uani 1 1 d . . . C17 C 0.843(2) 0.3484(15) 0.0751(12) 0.038(5) Uani 1 1 d . . . H17 H 0.8292 0.3602 0.0252 0.046 Uiso 1 1 calc R . . C18 C 0.829(3) 0.2587(16) 0.1094(12) 0.042(5) Uani 1 1 d . . . H18 H 0.8130 0.2072 0.0823 0.050 Uiso 1 1 calc R . . C19 C 0.838(2) 0.2417(13) 0.1832(13) 0.036(5) Uani 1 1 d . . . H19 H 0.8170 0.1823 0.2071 0.043 Uiso 1 1 calc R . . C20 C 0.8778(19) 0.3126(13) 0.2222(10) 0.026(4) Uani 1 1 d . . . C21 C 0.8996(18) 0.4032(13) 0.1883(11) 0.028(4) Uani 1 1 d . . . C22 C 0.859(3) 0.2167(17) 0.3352(12) 0.048(6) Uani 1 1 d . . . H22A H 0.7518 0.2157 0.3279 0.058 Uiso 1 1 calc R . . H22B H 0.8684 0.2226 0.3863 0.058 Uiso 1 1 calc R . . H22C H 0.9361 0.1528 0.3192 0.058 Uiso 1 1 calc R . . C23 C 0.5627(18) 0.7554(15) 0.2451(10) 0.028(4) Uani 1 1 d . . . C24 C 0.396(2) 0.7502(17) 0.2681(14) 0.050(6) Uani 1 1 d . . . H24A H 0.3815 0.7471 0.3206 0.060 Uiso 1 1 calc R . . H24B H 0.3815 0.6885 0.2500 0.060 Uiso 1 1 calc R . . H24C H 0.3187 0.8117 0.2485 0.060 Uiso 1 1 calc R . . C25 C 1.060(2) 0.9766(14) 0.2213(11) 0.032(4) Uani 1 1 d . . . C26 C 1.191(2) 1.0243(15) 0.2165(11) 0.035(5) Uani 1 1 d . . . H26A H 1.2829 0.9813 0.1891 0.042 Uiso 1 1 calc R . . H26B H 1.2192 1.0302 0.2649 0.042 Uiso 1 1 calc R . . H26C H 1.1560 1.0931 0.1923 0.042 Uiso 1 1 calc R . . C27 C 1.2148(19) 0.7026(16) 0.1195(10) 0.032(4) Uani 1 1 d . . . H27 H 1.1387 0.7686 0.1221 0.039 Uiso 1 1 calc R . . C28 C 1.477(3) 0.598(2) 0.0793(16) 0.065(8) Uani 1 1 d . . . H28A H 1.4254 0.5435 0.0798 0.078 Uiso 1 1 calc R . . H28B H 1.5470 0.5835 0.1189 0.078 Uiso 1 1 calc R . . H28C H 1.5400 0.5997 0.0336 0.078 Uiso 1 1 calc R . . C29 C 1.401(3) 0.789(2) 0.0608(14) 0.057(7) Uani 1 1 d . . . H29A H 1.3086 0.8494 0.0669 0.069 Uiso 1 1 calc R . . H29B H 1.4372 0.7838 0.0099 0.069 Uiso 1 1 calc R . . H29C H 1.4869 0.7956 0.0879 0.069 Uiso 1 1 calc R . . C30 C 1.250(2) 0.5442(14) 0.3343(10) 0.027(4) Uani 1 1 d . . . H30 H 1.1875 0.5734 0.3755 0.032 Uiso 1 1 calc R . . C31 C 1.472(3) 0.497(3) 0.4059(17) 0.081(10) Uani 1 1 d . . . H31A H 1.5523 0.5336 0.3985 0.097 Uiso 1 1 calc R . . H31B H 1.5212 0.4254 0.4227 0.097 Uiso 1 1 calc R . . H31C H 1.3891 0.5309 0.4418 0.097 Uiso 1 1 calc R . . C32 C 1.508(3) 0.4629(17) 0.2785(13) 0.049(6) Uani 1 1 d . . . H32A H 1.4458 0.4764 0.2363 0.059 Uiso 1 1 calc R . . H32B H 1.5601 0.3886 0.2852 0.059 Uiso 1 1 calc R . . H32C H 1.5888 0.4994 0.2713 0.059 Uiso 1 1 calc R . . C33 C 0.115(3) 0.804(2) 0.4388(14) 0.057(6) Uani 1 1 d . . . H33 H 0.0219 0.8391 0.4152 0.068 Uiso 1 1 calc R . . C34 C 0.359(3) 0.810(3) 0.4866(17) 0.072(8) Uani 1 1 d . . . H34A H 0.3748 0.7358 0.4942 0.086 Uiso 1 1 calc R . . H34B H 0.3537 0.8400 0.5329 0.086 Uiso 1 1 calc R . . H34C H 0.4473 0.8225 0.4555 0.086 Uiso 1 1 calc R . . C35 C 0.176(4) 0.970(2) 0.4315(19) 0.082(10) Uani 1 1 d . . . H35A H 0.2456 0.9788 0.3892 0.098 Uiso 1 1 calc R . . H35B H 0.1963 1.0052 0.4713 0.098 Uiso 1 1 calc R . . H35C H 0.0652 0.9984 0.4202 0.098 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 Yb1 0.0154(3) 0.0154(4) 0.0287(4) -0.0005(3) -0.0002(3) -0.0047(3) Yb2 0.0134(3) 0.0152(4) 0.0284(4) 0.0003(3) -0.0024(3) -0.0044(3) O1 0.039(8) 0.020(6) 0.040(8) 0.007(6) -0.006(6) -0.008(6) O2 0.020(5) 0.009(5) 0.027(6) 0.001(4) 0.003(5) 0.001(4) O3 0.021(6) 0.013(6) 0.040(7) -0.004(5) 0.008(5) 0.000(4) O4 0.024(6) 0.035(7) 0.037(8) 0.009(6) -0.001(6) 0.006(5) O5 0.039(7) 0.020(6) 0.040(8) 0.007(5) -0.004(6) -0.001(6) O6 0.024(5) 0.005(5) 0.026(6) -0.001(4) 0.008(4) -0.005(4) O7 0.022(6) 0.014(6) 0.039(7) 0.001(5) -0.016(5) -0.002(5) O8 0.033(7) 0.015(6) 0.056(9) 0.007(6) -0.001(6) -0.010(5) O9 0.018(6) 0.020(6) 0.046(8) -0.001(5) 0.008(5) -0.012(5) O10 0.016(5) 0.029(6) 0.026(6) 0.000(5) -0.004(5) -0.004(5) O11 0.024(6) 0.033(7) 0.041(8) -0.004(6) -0.001(6) -0.010(5) O12 0.031(7) 0.050(9) 0.037(8) 0.004(6) 0.007(6) -0.019(6) O13 0.014(6) 0.040(8) 0.051(9) 0.009(6) 0.008(6) -0.015(5) O14 0.019(6) 0.056(9) 0.029(7) 0.002(6) -0.003(5) -0.010(6) O15 0.077(14) 0.076(15) 0.096(16) -0.024(12) 0.010(12) -0.042(12) N1 0.013(6) 0.021(7) 0.034(8) 0.010(6) -0.005(6) -0.002(5) N2 0.031(8) 0.028(8) 0.020(7) 0.004(6) -0.004(6) -0.007(6) N3 0.026(7) 0.014(7) 0.029(8) 0.001(6) 0.007(6) -0.005(6) N4 0.021(7) 0.020(7) 0.013(6) 0.008(5) -0.006(5) 0.004(5) N5 0.026(7) 0.014(7) 0.030(8) 0.007(6) -0.008(6) -0.003(6) N6 0.027(8) 0.026(8) 0.028(8) 0.002(6) -0.005(6) -0.006(6) N7 0.030(8) 0.040(9) 0.028(8) 0.001(7) 0.013(7) -0.008(7) N8 0.024(8) 0.044(10) 0.054(11) 0.021(8) -0.008(7) -0.026(7) N9 0.044(11) 0.071(14) 0.049(12) 0.004(10) -0.004(9) -0.028(10) C1 0.043(11) 0.027(10) 0.028(10) 0.005(8) -0.007(8) -0.007(8) C2 0.015(7) 0.016(8) 0.027(9) -0.002(6) 0.002(6) 0.007(6) C3 0.018(7) 0.027(9) 0.022(8) -0.013(7) 0.012(6) -0.009(6) C4 0.013(7) 0.029(9) 0.021(8) -0.005(7) -0.001(6) -0.003(6) C5 0.014(7) 0.027(9) 0.031(9) -0.006(7) -0.002(7) -0.002(6) C6 0.036(10) 0.033(10) 0.033(10) -0.010(8) -0.013(8) -0.011(8) C7 0.014(8) 0.038(10) 0.031(10) -0.011(8) -0.005(7) 0.009(7) C8 0.018(8) 0.023(9) 0.042(11) -0.008(8) -0.009(8) 0.009(7) C9 0.026(9) 0.013(8) 0.043(11) -0.006(7) -0.008(8) -0.003(7) C10 0.014(7) 0.017(8) 0.049(11) -0.002(7) 0.002(7) -0.013(6) C11 0.048(12) 0.025(10) 0.037(11) 0.007(8) -0.013(9) 0.011(9) C12 0.046(12) 0.036(11) 0.032(11) 0.005(8) -0.013(9) -0.010(9) C13 0.018(8) 0.025(9) 0.041(11) 0.008(8) -0.002(7) -0.008(7) C14 0.017(7) 0.037(9) 0.021(8) 0.008(7) -0.005(6) -0.012(7) C15 0.024(8) 0.017(8) 0.019(8) -0.008(6) 0.000(6) -0.003(6) C16 0.012(7) 0.024(9) 0.043(11) -0.010(8) -0.002(7) 0.001(6) C17 0.041(11) 0.034(11) 0.046(12) -0.018(9) -0.003(9) -0.016(9) C18 0.052(13) 0.030(11) 0.051(13) -0.009(9) -0.006(10) -0.022(10) C19 0.024(9) 0.013(8) 0.077(15) 0.006(9) -0.009(9) -0.013(7) C20 0.016(8) 0.021(9) 0.045(11) -0.004(7) -0.003(7) -0.011(6) C21 0.008(7) 0.021(9) 0.057(12) -0.016(8) 0.000(7) -0.002(6) C22 0.064(15) 0.039(12) 0.035(12) 0.008(9) 0.015(10) -0.013(11) C23 0.010(7) 0.044(11) 0.036(10) 0.005(8) -0.010(7) -0.015(7) C24 0.036(11) 0.034(12) 0.084(18) -0.006(11) 0.016(11) -0.022(9) C25 0.030(9) 0.021(9) 0.042(11) 0.000(8) -0.028(9) 0.004(7) C26 0.030(9) 0.032(10) 0.054(13) -0.001(9) 0.005(9) -0.028(8) C27 0.012(8) 0.049(12) 0.036(10) 0.012(9) -0.005(7) -0.012(8) C28 0.030(11) 0.074(18) 0.081(19) 0.019(15) 0.020(12) -0.013(12) C29 0.032(11) 0.067(17) 0.069(17) 0.034(14) -0.002(11) -0.020(11) C30 0.020(8) 0.030(10) 0.027(9) 0.003(7) 0.005(7) -0.004(7) C31 0.034(13) 0.13(3) 0.08(2) 0.02(2) -0.035(14) -0.027(16) C32 0.035(11) 0.040(12) 0.065(16) 0.006(11) -0.004(11) -0.003(9) C33 0.045(13) 0.073(19) 0.056(16) -0.014(13) -0.006(11) -0.021(13) C34 0.040(14) 0.10(2) 0.08(2) 0.012(17) -0.017(13) -0.022(14) C35 0.07(2) 0.08(2) 0.10(3) 0.029(19) -0.035(18) -0.037(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O3 2.181(11) . ? Yb1 O6 2.284(10) . ? Yb1 O2 2.290(10) . ? Yb1 O9 2.324(11) . ? Yb1 O11 2.377(13) . ? Yb1 O12 2.391(12) . ? Yb1 N3 2.398(14) . ? Yb1 N4 2.456(13) . ? Yb1 C25 2.75(2) . ? Yb1 C3 3.116(17) . ? Yb1 Yb2 3.7307(12) . ? Yb2 O7 2.137(11) . ? Yb2 O6 2.267(10) . ? Yb2 O10 2.316(11) . ? Yb2 O14 2.321(12) . ? Yb2 O2 2.343(11) . ? Yb2 O13 2.385(11) . ? Yb2 N6 2.447(15) . ? Yb2 N1 2.451(14) . ? Yb2 C14 3.156(16) . ? O1 N1 1.377(18) . ? O1 H1 0.8400 . ? O2 C3 1.302(19) . ? O3 C10 1.28(2) . ? O4 C9 1.35(2) . ? O4 C11 1.44(2) . ? O5 N4 1.390(17) . ? O5 H5 0.8400 . ? O6 C14 1.33(2) . ? O7 C21 1.32(2) . ? O8 C20 1.35(2) . ? O8 C22 1.47(2) . ? O9 C23 1.26(2) . ? O10 C23 1.30(2) . ? O11 C25 1.28(2) . ? O12 C25 1.26(2) . ? O13 C27 1.25(2) . ? O14 C30 1.22(2) . ? O15 C33 1.22(3) . ? N1 C2 1.30(2) . ? N2 C3 1.31(2) . ? N2 N3 1.421(19) . ? N3 C4 1.28(2) . ? N4 C13 1.27(2) . ? N5 C14 1.30(2) . ? N5 N6 1.402(19) . ? N6 C15 1.30(2) . ? N7 C27 1.34(2) . ? N7 C28 1.44(3) . ? N7 C29 1.47(3) . ? N8 C30 1.33(2) . ? N8 C31 1.39(3) . ? N8 C32 1.45(3) . ? N9 C33 1.32(3) . ? N9 C35 1.47(3) . ? N9 C34 1.48(3) . ? C1 C2 1.48(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.50(2) . ? C4 C5 1.44(2) . ? C4 H4 0.9500 . ? C5 C6 1.43(2) . ? C5 C10 1.43(3) . ? C6 C7 1.36(3) . ? C6 H6 0.9500 . ? C7 C8 1.39(3) . ? C7 H7 0.9500 . ? C8 C9 1.39(2) . ? C8 H8 0.9500 . ? C9 C10 1.40(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.49(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.47(2) . ? C15 C16 1.43(2) . ? C15 H15 0.9500 . ? C16 C17 1.43(3) . ? C16 C21 1.44(3) . ? C17 C18 1.37(3) . ? C17 H17 0.9500 . ? C18 C19 1.39(3) . ? C18 H18 0.9500 . ? C19 C20 1.40(3) . ? C19 H19 0.9500 . ? C20 C21 1.40(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.52(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.48(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 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 Yb1 O6 138.0(4) . . ? O3 Yb1 O2 144.8(4) . . ? O6 Yb1 O2 71.3(4) . . ? O3 Yb1 O9 88.4(4) . . ? O6 Yb1 O9 76.6(4) . . ? O2 Yb1 O9 79.9(4) . . ? O3 Yb1 O11 90.5(5) . . ? O6 Yb1 O11 120.7(4) . . ? O2 Yb1 O11 84.8(4) . . ? O9 Yb1 O11 151.6(5) . . ? O3 Yb1 O12 99.0(5) . . ? O6 Yb1 O12 80.5(4) . . ? O2 Yb1 O12 106.5(4) . . ? O9 Yb1 O12 152.9(5) . . ? O11 Yb1 O12 55.0(5) . . ? O3 Yb1 N3 77.9(5) . . ? O6 Yb1 N3 132.7(4) . . ? O2 Yb1 N3 67.0(4) . . ? O9 Yb1 N3 75.0(5) . . ? O11 Yb1 N3 77.0(5) . . ? O12 Yb1 N3 132.0(5) . . ? O3 Yb1 N4 74.4(5) . . ? O6 Yb1 N4 64.4(4) . . ? O2 Yb1 N4 134.4(4) . . ? O9 Yb1 N4 79.9(5) . . ? O11 Yb1 N4 126.9(5) . . ? O12 Yb1 N4 77.1(5) . . ? N3 Yb1 N4 142.9(5) . . ? O3 Yb1 C25 94.5(5) . . ? O6 Yb1 C25 101.7(5) . . ? O2 Yb1 C25 97.2(5) . . ? O9 Yb1 C25 176.9(5) . . ? O11 Yb1 C25 27.7(5) . . ? O12 Yb1 C25 27.3(5) . . ? N3 Yb1 C25 104.7(5) . . ? N4 Yb1 C25 101.7(5) . . ? O3 Yb1 C3 123.1(4) . . ? O6 Yb1 C3 89.9(4) . . ? O2 Yb1 C3 21.7(4) . . ? O9 Yb1 C3 72.8(4) . . ? O11 Yb1 C3 84.2(4) . . ? O12 Yb1 C3 121.9(4) . . ? N3 Yb1 C3 45.7(4) . . ? N4 Yb1 C3 146.4(5) . . ? C25 Yb1 C3 104.7(5) . . ? O3 Yb1 Yb2 159.8(3) . . ? O6 Yb1 Yb2 34.8(3) . . ? O2 Yb1 Yb2 36.9(3) . . ? O9 Yb1 Yb2 71.7(3) . . ? O11 Yb1 Yb2 108.7(3) . . ? O12 Yb1 Yb2 97.3(4) . . ? N3 Yb1 Yb2 99.8(3) . . ? N4 Yb1 Yb2 97.8(3) . . ? C25 Yb1 Yb2 105.4(4) . . ? C3 Yb1 Yb2 55.3(3) . . ? O7 Yb2 O6 141.3(4) . . ? O7 Yb2 O10 86.2(4) . . ? O6 Yb2 O10 78.2(4) . . ? O7 Yb2 O14 84.3(5) . . ? O6 Yb2 O14 126.9(4) . . ? O10 Yb2 O14 145.9(4) . . ? O7 Yb2 O2 140.1(4) . . ? O6 Yb2 O2 70.6(4) . . ? O10 Yb2 O2 77.9(4) . . ? O14 Yb2 O2 88.8(4) . . ? O7 Yb2 O13 105.1(5) . . ? O6 Yb2 O13 73.4(4) . . ? O10 Yb2 O13 146.5(4) . . ? O14 Yb2 O13 67.5(5) . . ? O2 Yb2 O13 108.3(4) . . ? O7 Yb2 N6 76.0(5) . . ? O6 Yb2 N6 66.2(4) . . ? O10 Yb2 N6 77.8(5) . . ? O14 Yb2 N6 130.7(5) . . ? O2 Yb2 N6 133.7(4) . . ? O13 Yb2 N6 74.7(5) . . ? O7 Yb2 N1 75.5(5) . . ? O6 Yb2 N1 131.3(4) . . ? O10 Yb2 N1 74.0(4) . . ? O14 Yb2 N1 71.9(4) . . ? O2 Yb2 N1 65.0(4) . . ? O13 Yb2 N1 139.0(5) . . ? N6 Yb2 N1 140.8(5) . . ? O7 Yb2 C14 120.3(5) . . ? O6 Yb2 C14 21.2(4) . . ? O10 Yb2 C14 75.2(4) . . ? O14 Yb2 C14 137.0(4) . . ? O2 Yb2 C14 90.7(4) . . ? O13 Yb2 C14 72.0(4) . . ? N6 Yb2 C14 45.0(5) . . ? N1 Yb2 C14 144.0(4) . . ? O7 Yb2 Yb1 157.7(3) . . ? O6 Yb2 Yb1 35.1(3) . . ? O10 Yb2 Yb1 71.6(3) . . ? O14 Yb2 Yb1 114.1(4) . . ? O2 Yb2 Yb1 35.9(3) . . ? O13 Yb2 Yb1 94.0(3) . . ? N6 Yb2 Yb1 98.8(3) . . ? N1 Yb2 Yb1 97.5(3) . . ? C14 Yb2 Yb1 54.9(3) . . ? N1 O1 H1 109.5 . . ? C3 O2 Yb1 117.7(10) . . ? C3 O2 Yb2 121.7(10) . . ? Yb1 O2 Yb2 107.3(5) . . ? C10 O3 Yb1 137.5(11) . . ? C9 O4 C11 116.9(14) . . ? N4 O5 H5 109.5 . . ? C14 O6 Yb2 120.6(10) . . ? C14 O6 Yb1 123.5(10) . . ? Yb2 O6 Yb1 110.1(5) . . ? C21 O7 Yb2 141.2(12) . . ? C20 O8 C22 117.7(15) . . ? C23 O9 Yb1 134.5(10) . . ? C23 O10 Yb2 135.0(10) . . ? C25 O11 Yb1 92.6(11) . . ? C25 O12 Yb1 92.5(12) . . ? C27 O13 Yb2 127.5(12) . . ? C30 O14 Yb2 145.3(12) . . ? C2 N1 O1 115.0(14) . . ? C2 N1 Yb2 122.3(11) . . ? O1 N1 Yb2 122.5(11) . . ? C3 N2 N3 110.2(14) . . ? C4 N3 N2 113.1(14) . . ? C4 N3 Yb1 128.5(11) . . ? N2 N3 Yb1 117.5(10) . . ? C13 N4 O5 116.9(14) . . ? C13 N4 Yb1 122.1(11) . . ? O5 N4 Yb1 120.2(10) . . ? C14 N5 N6 112.1(14) . . ? C15 N6 N5 114.1(15) . . ? C15 N6 Yb2 128.9(12) . . ? N5 N6 Yb2 116.9(11) . . ? C27 N7 C28 121.5(17) . . ? C27 N7 C29 120.7(18) . . ? C28 N7 C29 117.8(17) . . ? C30 N8 C31 121(2) . . ? C30 N8 C32 119.5(18) . . ? C31 N8 C32 118.7(19) . . ? C33 N9 C35 123(2) . . ? C33 N9 C34 121(2) . . ? C35 N9 C34 115(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 126.2(15) . . ? N1 C2 C3 111.0(14) . . ? C1 C2 C3 122.7(14) . . ? O2 C3 N2 126.3(16) . . ? O2 C3 C2 116.6(13) . . ? N2 C3 C2 116.6(14) . . ? N2 C3 Yb1 86.5(10) . . ? C2 C3 Yb1 151.7(11) . . ? N3 C4 C5 127.2(16) . . ? N3 C4 H4 116.4 . . ? C5 C4 H4 116.4 . . ? C6 C5 C10 119.2(16) . . ? C6 C5 C4 116.5(16) . . ? C10 C5 C4 123.7(15) . . ? C7 C6 C5 120.6(18) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 120.8(16) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C7 C8 C9 120.1(16) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? O4 C9 C8 123.6(16) . . ? O4 C9 C10 115.1(15) . . ? C8 C9 C10 121.2(18) . . ? O3 C10 C9 117.7(17) . . ? O3 C10 C5 124.3(16) . . ? C9 C10 C5 118.0(16) . . ? O4 C11 H11A 109.5 . . ? O4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C14 111.2(16) . . ? N4 C13 C12 126.7(16) . . ? C14 C13 C12 122.0(17) . . ? N5 C14 O6 123.9(15) . . ? N5 C14 C13 120.6(16) . . ? O6 C14 C13 115.4(16) . . ? N5 C14 Yb2 85.9(10) . . ? C13 C14 Yb2 152.5(13) . . ? N6 C15 C16 125.9(16) . . ? N6 C15 H15 117.1 . . ? C16 C15 H15 117.1 . . ? C17 C16 C15 117.2(17) . . ? C17 C16 C21 117.8(17) . . ? C15 C16 C21 124.6(16) . . ? C18 C17 C16 121(2) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 121.1(18) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C20 119.5(17) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? O8 C20 C21 113.3(15) . . ? O8 C20 C19 125.9(16) . . ? C21 C20 C19 120.8(18) . . ? O7 C21 C20 119.0(18) . . ? O7 C21 C16 121.5(16) . . ? C20 C21 C16 119.5(16) . . ? O8 C22 H22A 109.5 . . ? O8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O9 C23 O10 125.1(14) . . ? O9 C23 C24 116.8(16) . . ? O10 C23 C24 118.1(16) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O12 C25 O11 119.8(18) . . ? O12 C25 C26 119.6(19) . . ? O11 C25 C26 120.6(17) . . ? O12 C25 Yb1 60.2(10) . . ? O11 C25 Yb1 59.6(10) . . ? C26 C25 Yb1 173.6(13) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O13 C27 N7 122.4(18) . . ? O13 C27 H27 118.8 . . ? N7 C27 H27 118.8 . . ? N7 C28 H28A 109.5 . . ? N7 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N7 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N7 C29 H29A 109.5 . . ? N7 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N7 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O14 C30 N8 125.0(17) . . ? O14 C30 H30 117.5 . . ? N8 C30 H30 117.5 . . ? N8 C31 H31A 109.5 . . ? N8 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N8 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N8 C32 H32A 109.5 . . ? N8 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N8 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O15 C33 N9 125(3) . . ? O15 C33 H33 117.4 . . ? N9 C33 H33 117.4 . . ? N9 C34 H34A 109.5 . . ? N9 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N9 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N9 C35 H35A 109.5 . . ? N9 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N9 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 4.151 _refine_diff_density_min -3.166 _refine_diff_density_rms 0.336 _iucr_refine_instructions_details ; TITL _5-Revised CELL 0.71075 8.86200 13.61600 18.74900 85.267 84.683 72.526 ZERR 2 0.00200 0.00300 0.00500 0.008 0.007 0.007 LATT 1 SFAC C H N O YB UNIT 70 98 18 30 4 SHEL 8.147180 0.796452 L.S. 5 FMAP 2 PLAN -25 TEMP -110.0 ACTA BOND $H OMIT 2 2 0 OMIT 3 -2 5 OMIT 4 2 5 OMIT -1 3 8 ISOR 0.025 0.05 O6 SIMU 0.025 0.05 1.7 C14 O6 SIZE 0.200 0.200 0.200 WGHT 0.000000 129.814896 FVAR 0.76802 YB1 5 0.795140 0.909469 0.226656 11.00000 0.01544 0.01543 = 0.02870 -0.00054 -0.00019 -0.00475 YB2 5 0.948971 0.622894 0.223329 11.00000 0.01345 0.01523 = 0.02843 0.00032 -0.00242 -0.00440 O1 4 0.896109 0.483442 0.377314 11.00000 0.03904 0.02044 = 0.04042 0.00666 -0.00650 -0.00763 AFIX 147 H1 2 0.956349 0.441362 0.349176 11.00000 -1.20000 AFIX 0 O2 4 0.889686 0.762038 0.297308 11.00000 0.02017 0.00889 = 0.02714 0.00114 0.00276 0.00089 O3 4 0.628636 1.064358 0.223256 11.00000 0.02113 0.01276 = 0.04033 -0.00445 0.00847 -0.00043 O4 4 0.439888 1.225807 0.163315 11.00000 0.02411 0.03518 = 0.03659 0.00868 -0.00136 0.00597 O5 4 0.646570 1.046002 0.077169 11.00000 0.03898 0.02001 = 0.03972 0.00702 -0.00382 -0.00105 AFIX 147 H5 2 0.712525 1.069667 0.051961 11.00000 -1.20000 AFIX 0 O6 4 0.880887 0.772744 0.155065 11.00000 0.02417 0.00475 = 0.02640 -0.00098 0.00756 -0.00452 O7 4 0.940520 0.467356 0.226662 11.00000 0.02183 0.01393 = 0.03882 0.00081 -0.01623 -0.00245 O8 4 0.892055 0.305478 0.293635 11.00000 0.03252 0.01481 = 0.05556 0.00737 -0.00126 -0.01032 O9 4 0.579917 0.844156 0.233312 11.00000 0.01758 0.02005 = 0.04568 -0.00109 0.00770 -0.01205 O10 4 0.674680 0.669360 0.237201 11.00000 0.01571 0.02899 = 0.02568 -0.00011 -0.00447 -0.00410 O11 4 0.979551 0.970073 0.281109 11.00000 0.02431 0.03331 = 0.04127 -0.00445 -0.00067 -0.01038 O12 4 1.021739 0.947197 0.165253 11.00000 0.03099 0.04959 = 0.03651 0.00384 0.00658 -0.01868 O13 4 1.176968 0.625594 0.145808 11.00000 0.01423 0.04012 = 0.05136 0.00918 0.00848 -0.01481 O14 4 1.183878 0.551180 0.278968 11.00000 0.01859 0.05586 = 0.02946 0.00177 -0.00308 -0.00956 O15 4 0.138849 0.712081 0.454541 11.00000 0.07698 0.07603 = 0.09554 -0.02372 0.01005 -0.04232 N1 3 0.881907 0.582594 0.349945 11.00000 0.01290 0.02147 = 0.03427 0.01023 -0.00516 -0.00227 N2 3 0.726693 0.835121 0.395704 11.00000 0.03104 0.02778 = 0.01963 0.00411 -0.00392 -0.00712 N3 3 0.688645 0.925332 0.348930 11.00000 0.02552 0.01398 = 0.02855 0.00136 0.00658 -0.00514 N4 3 0.721048 0.945627 0.102067 11.00000 0.02136 0.01991 = 0.01315 0.00754 -0.00586 0.00372 N5 3 0.837885 0.692922 0.057459 11.00000 0.02627 0.01361 = 0.03030 0.00703 -0.00786 -0.00290 N6 3 0.879142 0.603514 0.103090 11.00000 0.02744 0.02566 = 0.02814 0.00210 -0.00538 -0.00628 N7 3 1.358858 0.695782 0.087543 11.00000 0.03011 0.03962 = 0.02841 0.00120 0.01287 -0.00838 N8 3 1.404373 0.498636 0.341296 11.00000 0.02386 0.04366 = 0.05362 0.02124 -0.00798 -0.02600 N9 3 0.208900 0.858695 0.452099 11.00000 0.04383 0.07094 = 0.04906 0.00391 -0.00391 -0.02844 C1 1 0.811451 0.634009 0.475222 11.00000 0.04275 0.02733 = 0.02847 0.00455 -0.00717 -0.00679 AFIX 137 H1A 2 0.810237 0.562526 0.485699 11.00000 -1.20000 H1B 2 0.708555 0.680981 0.491135 11.00000 -1.20000 H1C 2 0.895163 0.646522 0.500596 11.00000 -1.20000 AFIX 0 C2 1 0.842230 0.652114 0.397118 11.00000 0.01486 0.01640 = 0.02709 -0.00216 0.00213 0.00738 C3 1 0.823440 0.757695 0.361949 11.00000 0.01765 0.02683 = 0.02179 -0.01346 0.01209 -0.00884 C4 1 0.580994 1.001025 0.376630 11.00000 0.01288 0.02939 = 0.02132 -0.00500 -0.00144 -0.00302 AFIX 43 H4 2 0.552551 0.992670 0.426375 11.00000 -1.20000 AFIX 0 C5 1 0.498536 1.097223 0.340662 11.00000 0.01375 0.02688 = 0.03127 -0.00603 -0.00237 -0.00238 C6 1 0.373427 1.165652 0.381879 11.00000 0.03628 0.03299 = 0.03289 -0.01018 -0.01280 -0.01084 AFIX 43 H6 2 0.356992 1.150315 0.431826 11.00000 -1.20000 AFIX 0 C7 1 0.277190 1.252893 0.350234 11.00000 0.01372 0.03759 = 0.03091 -0.01126 -0.00453 0.00918 AFIX 43 H7 2 0.195400 1.298233 0.378556 11.00000 -1.20000 AFIX 0 C8 1 0.297210 1.276274 0.277208 11.00000 0.01812 0.02277 = 0.04219 -0.00760 -0.00884 0.00923 AFIX 43 H8 2 0.231175 1.338248 0.256093 11.00000 -1.20000 AFIX 0 C9 1 0.414076 1.208974 0.234753 11.00000 0.02562 0.01344 = 0.04332 -0.00574 -0.00803 -0.00306 C10 1 0.520099 1.120167 0.265125 11.00000 0.01421 0.01674 = 0.04921 -0.00164 0.00198 -0.01316 C11 1 0.329534 1.313702 0.129383 11.00000 0.04810 0.02484 = 0.03702 0.00702 -0.01272 0.01078 AFIX 137 H11A 2 0.220810 1.313794 0.144902 11.00000 -1.20000 H11B 2 0.345990 1.309813 0.077155 11.00000 -1.20000 H11C 2 0.346819 1.377223 0.143036 11.00000 -1.20000 AFIX 0 C12 1 0.752956 0.895540 -0.023486 11.00000 0.04617 0.03600 = 0.03248 0.00464 -0.01290 -0.00993 AFIX 137 H12A 2 0.641060 0.926002 -0.032962 11.00000 -1.20000 H12B 2 0.794946 0.829596 -0.046273 11.00000 -1.20000 H12C 2 0.813264 0.942528 -0.043111 11.00000 -1.20000 AFIX 0 C13 1 0.767581 0.878010 0.055572 11.00000 0.01767 0.02504 = 0.04096 0.00806 -0.00170 -0.00803 C14 1 0.834583 0.774844 0.089459 11.00000 0.01693 0.03700 = 0.02064 0.00847 -0.00544 -0.01238 C15 1 0.870870 0.521082 0.075170 11.00000 0.02384 0.01744 = 0.01892 -0.00843 0.00014 -0.00282 AFIX 43 H15 2 0.859111 0.525456 0.025053 11.00000 -1.20000 AFIX 0 C16 1 0.877884 0.424514 0.113121 11.00000 0.01154 0.02411 = 0.04295 -0.01035 -0.00174 0.00094 C17 1 0.842984 0.348408 0.075122 11.00000 0.04082 0.03396 = 0.04638 -0.01755 -0.00311 -0.01578 AFIX 43 H17 2 0.829216 0.360243 0.025169 11.00000 -1.20000 AFIX 0 C18 1 0.829030 0.258749 0.109406 11.00000 0.05231 0.02991 = 0.05082 -0.00944 -0.00600 -0.02214 AFIX 43 H18 2 0.813008 0.207187 0.082345 11.00000 -1.20000 AFIX 0 C19 1 0.837880 0.241677 0.183240 11.00000 0.02360 0.01286 = 0.07694 0.00558 -0.00874 -0.01346 AFIX 43 H19 2 0.816999 0.182319 0.207108 11.00000 -1.20000 AFIX 0 C20 1 0.877809 0.312644 0.222165 11.00000 0.01628 0.02062 = 0.04472 -0.00430 -0.00312 -0.01088 C21 1 0.899615 0.403213 0.188344 11.00000 0.00755 0.02092 = 0.05733 -0.01636 0.00032 -0.00244 C22 1 0.859354 0.216744 0.335223 11.00000 0.06410 0.03943 = 0.03460 0.00804 0.01513 -0.01283 AFIX 137 H22A 2 0.751793 0.215710 0.327885 11.00000 -1.20000 H22B 2 0.868404 0.222609 0.386295 11.00000 -1.20000 H22C 2 0.936083 0.152807 0.319191 11.00000 -1.20000 AFIX 0 C23 1 0.562682 0.755394 0.245121 11.00000 0.01042 0.04413 = 0.03595 0.00506 -0.01004 -0.01545 C24 1 0.396336 0.750213 0.268076 11.00000 0.03632 0.03381 = 0.08358 -0.00610 0.01633 -0.02215 AFIX 137 H24A 2 0.381469 0.747052 0.320574 11.00000 -1.20000 H24B 2 0.381453 0.688495 0.249993 11.00000 -1.20000 H24C 2 0.318670 0.811748 0.248484 11.00000 -1.20000 AFIX 0 C25 1 1.059830 0.976557 0.221329 11.00000 0.02986 0.02120 = 0.04183 -0.00006 -0.02761 0.00430 C26 1 1.190559 1.024332 0.216481 11.00000 0.02983 0.03153 = 0.05398 -0.00141 0.00462 -0.02836 AFIX 137 H26A 2 1.282902 0.981280 0.189110 11.00000 -1.20000 H26B 2 1.219205 1.030188 0.264862 11.00000 -1.20000 H26C 2 1.156006 1.093116 0.192266 11.00000 -1.20000 AFIX 0 C27 1 1.214800 0.702600 0.119480 11.00000 0.01193 0.04918 = 0.03614 0.01166 -0.00518 -0.01246 AFIX 43 H27 2 1.138673 0.768611 0.122148 11.00000 -1.20000 AFIX 0 C28 1 1.477241 0.597863 0.079319 11.00000 0.03013 0.07408 = 0.08070 0.01872 0.01956 -0.01349 AFIX 137 H28A 2 1.425400 0.543541 0.079807 11.00000 -1.20000 H28B 2 1.547036 0.583541 0.118911 11.00000 -1.20000 H28C 2 1.540003 0.599744 0.033631 11.00000 -1.20000 AFIX 0 C29 1 1.401448 0.788850 0.060831 11.00000 0.03239 0.06738 = 0.06876 0.03432 -0.00176 -0.01976 AFIX 137 H29A 2 1.308650 0.849434 0.066881 11.00000 -1.20000 H29B 2 1.437246 0.783782 0.009856 11.00000 -1.20000 H29C 2 1.486937 0.795586 0.087891 11.00000 -1.20000 AFIX 0 C30 1 1.250397 0.544163 0.334346 11.00000 0.01959 0.03036 = 0.02699 0.00270 0.00497 -0.00442 AFIX 43 H30 2 1.187454 0.573399 0.375498 11.00000 -1.20000 AFIX 0 C31 1 1.471767 0.497032 0.405893 11.00000 0.03380 0.12837 = 0.08462 0.01928 -0.03523 -0.02744 AFIX 137 H31A 2 1.552322 0.533598 0.398543 11.00000 -1.20000 H31B 2 1.521233 0.425421 0.422701 11.00000 -1.20000 H31C 2 1.389092 0.530949 0.441817 11.00000 -1.20000 AFIX 0 C32 1 1.508144 0.462875 0.278459 11.00000 0.03503 0.03978 = 0.06519 0.00571 -0.00428 -0.00319 AFIX 137 H32A 2 1.445845 0.476413 0.236265 11.00000 -1.20000 H32B 2 1.560051 0.388617 0.285241 11.00000 -1.20000 H32C 2 1.588784 0.499387 0.271336 11.00000 -1.20000 AFIX 0 C33 1 0.115106 0.804065 0.438807 11.00000 0.04504 0.07339 = 0.05643 -0.01395 -0.00648 -0.02137 AFIX 43 H33 2 0.021907 0.839078 0.415161 11.00000 -1.20000 AFIX 0 C34 1 0.358786 0.810189 0.486568 11.00000 0.03994 0.09803 = 0.07875 0.01223 -0.01668 -0.02233 AFIX 137 H34A 2 0.374823 0.735784 0.494193 11.00000 -1.20000 H34B 2 0.353729 0.840049 0.532851 11.00000 -1.20000 H34C 2 0.447290 0.822538 0.455538 11.00000 -1.20000 AFIX 0 C35 1 0.176255 0.969560 0.431494 11.00000 0.07320 0.07809 = 0.10443 0.02875 -0.03524 -0.03740 AFIX 137 H35A 2 0.245552 0.978762 0.389229 11.00000 -1.20000 H35B 2 0.196332 1.005167 0.471319 11.00000 -1.20000 H35C 2 0.065183 0.998440 0.420239 11.00000 -1.20000 HKLF 4 REM _5-Revised REM R1 = 0.1085 for 7313 Fo > 4sig(Fo) and 0.1261 for all 8778 data REM 564 parameters refined using 12 restraints END WGHT 0.0000 129.8979 REM Highest difference peak 4.151, deepest hole -3.166, 1-sigma level 0.336 Q1 1 0.6419 1.1977 0.2286 11.00000 0.05 4.15 Q2 1 1.1009 0.3361 0.2220 11.00000 0.05 3.51 Q3 1 1.2953 0.4939 0.2191 11.00000 0.05 1.77 Q4 1 0.9449 0.9743 0.3296 11.00000 0.05 1.69 Q5 1 1.1046 0.6847 0.3322 11.00000 0.05 1.67 Q6 1 1.2673 0.9821 0.1267 11.00000 0.05 1.67 Q7 1 0.8229 0.8197 0.2631 11.00000 0.05 1.64 Q8 1 0.7677 0.9173 0.3146 11.00000 0.05 1.64 Q9 1 0.9714 0.5368 0.2524 11.00000 0.05 1.59 Q10 1 0.6218 0.9083 0.2276 11.00000 0.05 1.58 Q11 1 1.2902 0.9626 0.1474 11.00000 0.05 1.50 Q12 1 1.4629 0.5246 0.2693 11.00000 0.05 1.49 Q13 1 1.0981 0.5844 0.1799 11.00000 0.05 1.46 Q14 1 1.1497 0.7830 0.2337 11.00000 0.05 1.44 Q15 1 0.7972 0.8357 0.1619 11.00000 0.05 1.43 Q16 1 1.1196 0.6187 0.2298 11.00000 0.05 1.42 Q17 1 1.4162 0.6940 0.1381 11.00000 0.05 1.42 Q18 1 0.8533 0.6615 0.2118 11.00000 0.05 1.39 Q19 1 0.9150 0.8569 0.2418 11.00000 0.05 1.36 Q20 1 0.3888 0.8000 0.2930 11.00000 0.05 1.36 Q21 1 0.2009 0.8809 0.3529 11.00000 0.05 1.35 Q22 1 0.7878 0.9014 0.3005 11.00000 0.05 1.32 Q23 1 0.7630 0.6163 0.2266 11.00000 0.05 1.31 Q24 1 0.7901 0.7916 0.2068 11.00000 0.05 1.31 Q25 1 0.9133 0.6225 0.3076 11.00000 0.05 1.30 ; data_6-Revised _database_code_depnum_ccdc_archive 'CCDC 910743' #TrackingRef 'Revised_Ln6_Combined_CIF.cif' # start Validation Reply Form _vrf_PLAT002_6-Revised ; PROBLEM: Number of Distance or Angle Restraints on AtSite 8 RESPONSE: Oxygen bound H-atoms were introduced in calculated positions and refined positionally with distance and angle restraints, and with Uiso = 1.5 Ueq of the atom to which they were bound. For more information please see refine_special_details. ; _vrf_PLAT860_6-Revised ; PROBLEM: Note: Number of Least-Squares Restraints .......7 RESPONSE: Oxygen bound H-atoms were introduced in calculated positions and refined positionally with distance and angle restraints, and with Uiso = 1.5 Ueq of the atom to which they were bound. For more information please see refine_special_details. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H32 N6 O14 Tm2, 2(H2 O)' _chemical_formula_sum 'C26 H36 N6 O16 Tm2' _chemical_formula_weight 1026.47 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' Tm Tm -0.3139 5.2483 '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 9.044(8) _cell_length_b 14.781(11) _cell_length_c 14.491(12) _cell_angle_alpha 90.00 _cell_angle_beta 113.965(17) _cell_angle_gamma 90.00 _cell_volume 1770(3) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 2348 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.2 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.926 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 5.046 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.626 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _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 17124 _diffrn_reflns_av_R_equivalents 0.0964 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 26.50 _reflns_number_total 3661 _reflns_number_gt 3542 _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. Oxygen bound H-atoms were introduced in calculated positions and refined positionally with distance and angle restraints, and with Uiso = 1.5 Ueq of the atom to which they were bound. All other H-atoms were introduced in calculated positions and refined on a riding model. All non-hydrogen atoms were refined anisotropically. The restraints follow: DFIX 0.8400 0.0200 O1 H1 DFIX 0.8700 0.0020 O9 H9A DFIX 0.8700 0.0200 O9 H9B DFIX 0.8804 0.0200 O8 H8A DFIX 0.8803 0.0200 O8 H8B DANG 1.4725 0.0400 H8A H8B DANG 1.3829 0.0400 H9A H9B ; _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^)+(0.0236P)^2^+2.6313P] 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 3661 _refine_ls_number_parameters 244 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm1 Tm 0.856453(16) 0.099141(9) 0.450781(10) 0.01535(8) Uani 1 1 d . . . O1 O 0.9808(3) -0.31308(17) 0.4999(2) 0.0310(6) Uani 1 1 d D . . H1 H 1.084(2) -0.315(4) 0.532(3) 0.047 Uiso 1 1 d D . . O2 O 0.8777(3) -0.05352(15) 0.48406(18) 0.0178(5) Uani 1 1 d . . . O3 O 0.6992(3) 0.20728(16) 0.45686(19) 0.0256(5) Uani 1 1 d . . . O4 O 0.6208(4) 0.37525(19) 0.4061(2) 0.0322(6) Uani 1 1 d . . . O5 O 0.8629(3) 0.03495(19) 0.29977(19) 0.0287(6) Uani 1 1 d . . . O6 O 0.7941(4) 0.17795(19) 0.2951(2) 0.0381(7) Uani 1 1 d . . . O8 O 0.9072(4) 0.09726(16) 0.6206(2) 0.0248(6) Uani 1 1 d D . . H8A H 0.976(5) 0.060(3) 0.665(3) 0.037 Uiso 1 1 d D . . H8B H 0.848(5) 0.121(3) 0.651(3) 0.037 Uiso 1 1 d D . . O9 O 0.7240(3) 0.35198(19) 0.2125(2) 0.0316(6) Uani 1 1 d D . . H9A H 0.736(6) 0.3013(17) 0.245(3) 0.047 Uiso 1 1 d D . . H9B H 0.622(3) 0.363(3) 0.176(3) 0.047 Uiso 1 1 d D . . N1 N 0.9386(4) -0.22189(19) 0.4927(2) 0.0208(6) Uani 1 1 d . . . N2 N 0.6007(4) -0.0760(2) 0.4062(2) 0.0187(6) Uani 1 1 d . . . N3 N 0.6009(3) 0.02099(19) 0.4055(2) 0.0173(6) Uani 1 1 d . . . C1 C 0.6524(4) -0.2759(2) 0.4149(3) 0.0273(8) Uani 1 1 d . . . H1A H 0.6062 -0.2774 0.3409 0.033 Uiso 1 1 calc R . . H1B H 0.5676 -0.2605 0.4380 0.033 Uiso 1 1 calc R . . H1C H 0.6974 -0.3355 0.4414 0.033 Uiso 1 1 calc R . . C2 C 0.7839(4) -0.2063(2) 0.4523(3) 0.0196(7) Uani 1 1 d . . . C3 C 0.7501(4) -0.1065(2) 0.4464(3) 0.0160(7) Uani 1 1 d . . . C4 C 0.4594(4) 0.0568(2) 0.3811(3) 0.0205(7) Uani 1 1 d . . . H4 H 0.3713 0.0170 0.3699 0.025 Uiso 1 1 calc R . . C5 C 0.4242(4) 0.1544(2) 0.3692(3) 0.0222(7) Uani 1 1 d . . . C6 C 0.2591(5) 0.1797(3) 0.3198(3) 0.0338(9) Uani 1 1 d . . . H6 H 0.1781 0.1341 0.3013 0.041 Uiso 1 1 calc R . . C7 C 0.2138(5) 0.2684(3) 0.2980(3) 0.0402(10) Uani 1 1 d . . . H7 H 0.1025 0.2836 0.2648 0.048 Uiso 1 1 calc R . . C8 C 0.3321(5) 0.3369(3) 0.3250(3) 0.0329(9) Uani 1 1 d . . . H8 H 0.3005 0.3981 0.3082 0.039 Uiso 1 1 calc R . . C9 C 0.4943(5) 0.3154(3) 0.3758(3) 0.0251(7) Uani 1 1 d . . . C10 C 0.5453(4) 0.2235(2) 0.4026(2) 0.0201(7) Uani 1 1 d . . . C11 C 0.5849(6) 0.4678(3) 0.3773(4) 0.0430(11) Uani 1 1 d . . . H11A H 0.5311 0.4720 0.3036 0.052 Uiso 1 1 calc R . . H11B H 0.6856 0.5028 0.4015 0.052 Uiso 1 1 calc R . . H11C H 0.5134 0.4920 0.4072 0.052 Uiso 1 1 calc R . . C12 C 0.8248(5) 0.1098(3) 0.2520(3) 0.0237(8) Uani 1 1 d . . . C13 C 0.8128(6) 0.1173(3) 0.1464(3) 0.0404(10) Uani 1 1 d . . . H13A H 0.6987 0.1212 0.0995 0.048 Uiso 1 1 calc R . . H13B H 0.8618 0.0638 0.1303 0.048 Uiso 1 1 calc R . . H13C H 0.8699 0.1717 0.1401 0.048 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 Tm1 0.01352(11) 0.01039(12) 0.01754(12) 0.00105(4) 0.00160(8) 0.00083(4) O1 0.0286(14) 0.0106(12) 0.0492(17) -0.0013(11) 0.0110(13) 0.0020(11) O2 0.0113(10) 0.0120(11) 0.0244(12) -0.0002(9) 0.0015(9) -0.0006(8) O3 0.0214(12) 0.0179(12) 0.0310(13) -0.0009(10) 0.0041(11) 0.0058(10) O4 0.0428(16) 0.0177(12) 0.0302(14) 0.0028(11) 0.0087(13) 0.0036(12) O5 0.0339(14) 0.0273(14) 0.0226(13) 0.0022(10) 0.0093(11) 0.0075(12) O6 0.060(2) 0.0228(14) 0.0289(14) 0.0090(11) 0.0159(14) 0.0091(14) O8 0.0253(15) 0.0260(16) 0.0213(14) 0.0010(9) 0.0076(12) 0.0089(10) O9 0.0255(14) 0.0286(15) 0.0405(16) 0.0137(12) 0.0130(12) 0.0036(12) N1 0.0214(14) 0.0136(13) 0.0251(15) 0.0000(11) 0.0071(12) 0.0031(11) N2 0.0190(14) 0.0129(13) 0.0235(14) -0.0014(12) 0.0080(12) -0.0007(12) N3 0.0168(13) 0.0128(13) 0.0191(13) -0.0008(10) 0.0039(11) -0.0019(10) C1 0.0233(18) 0.0143(17) 0.041(2) -0.0022(15) 0.0099(16) -0.0018(14) C2 0.0203(16) 0.0174(17) 0.0221(16) -0.0018(13) 0.0096(14) -0.0020(13) C3 0.0157(16) 0.0170(17) 0.0145(16) -0.0014(11) 0.0052(13) -0.0026(11) C4 0.0170(15) 0.0195(18) 0.0235(16) 0.0008(13) 0.0067(13) 0.0010(13) C5 0.0210(17) 0.0243(19) 0.0209(17) 0.0038(14) 0.0080(14) 0.0068(14) C6 0.0228(18) 0.032(2) 0.044(2) 0.0055(17) 0.0107(17) 0.0062(16) C7 0.030(2) 0.038(2) 0.046(2) 0.007(2) 0.0086(18) 0.0180(18) C8 0.038(2) 0.026(2) 0.032(2) 0.0073(16) 0.0112(17) 0.0176(17) C9 0.0336(19) 0.0233(18) 0.0190(16) 0.0018(14) 0.0114(15) 0.0066(15) C10 0.0230(17) 0.0211(17) 0.0167(15) 0.0002(13) 0.0088(13) 0.0081(14) C11 0.059(3) 0.023(2) 0.039(2) 0.0064(18) 0.012(2) 0.007(2) C12 0.0193(18) 0.0262(19) 0.0203(18) 0.0014(14) 0.0026(15) -0.0033(14) C13 0.050(3) 0.048(3) 0.023(2) 0.0054(19) 0.015(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tm1 O3 2.165(3) . ? Tm1 O2 2.298(3) 3_756 ? Tm1 O2 2.299(3) . ? Tm1 O8 2.313(4) . ? Tm1 O6 2.394(3) . ? Tm1 O5 2.408(3) . ? Tm1 N3 2.424(3) . ? Tm1 N1 2.483(3) 3_756 ? Tm1 C12 2.782(5) . ? Tm1 Tm1 3.789(2) 3_756 ? O1 N1 1.393(4) . ? O1 H1 0.86(2) . ? O2 C3 1.316(4) . ? O2 Tm1 2.298(3) 3_756 ? O3 C10 1.313(4) . ? O4 C9 1.370(5) . ? O4 C11 1.428(5) . ? O5 C12 1.277(5) . ? O6 C12 1.274(5) . ? O8 H8A 0.884(19) . ? O8 H8B 0.894(19) . ? O9 H9A 0.870(2) . ? O9 H9B 0.870(19) . ? N1 C2 1.299(5) . ? N1 Tm1 2.483(3) 3_756 ? N2 C3 1.315(5) . ? N2 N3 1.433(4) . ? N3 C4 1.294(5) . ? C1 C2 1.498(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.501(5) . ? C4 C5 1.472(5) . ? C4 H4 0.9500 . ? C5 C6 1.419(5) . ? C5 C10 1.430(5) . ? C6 C7 1.372(6) . ? C6 H6 0.9500 . ? C7 C8 1.409(7) . ? C7 H7 0.9500 . ? C8 C9 1.385(6) . ? C8 H8 0.9500 . ? C9 C10 1.437(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.493(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 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 Tm1 O2 142.63(9) . 3_756 ? O3 Tm1 O2 135.76(9) . . ? O2 Tm1 O2 68.99(9) 3_756 . ? O3 Tm1 O8 79.36(10) . . ? O2 Tm1 O8 80.62(10) 3_756 . ? O2 Tm1 O8 78.55(9) . . ? O3 Tm1 O6 76.81(11) . . ? O2 Tm1 O6 109.66(10) 3_756 . ? O2 Tm1 O6 130.01(9) . . ? O8 Tm1 O6 151.34(9) . . ? O3 Tm1 O5 125.94(9) . . ? O2 Tm1 O5 81.38(9) 3_756 . ? O2 Tm1 O5 76.88(10) . . ? O8 Tm1 O5 153.48(9) . . ? O6 Tm1 O5 54.45(11) . . ? O3 Tm1 N3 78.05(11) . . ? O2 Tm1 N3 134.01(10) 3_756 . ? O2 Tm1 N3 65.06(9) . . ? O8 Tm1 N3 92.14(10) . . ? O6 Tm1 N3 98.24(11) . . ? O5 Tm1 N3 86.50(10) . . ? O3 Tm1 N1 82.05(12) . 3_756 ? O2 Tm1 N1 64.06(10) 3_756 3_756 ? O2 Tm1 N1 131.32(9) . 3_756 ? O8 Tm1 N1 81.88(10) . 3_756 ? O6 Tm1 N1 79.28(11) . 3_756 ? O5 Tm1 N1 107.30(10) . 3_756 ? N3 Tm1 N1 159.97(9) . 3_756 ? O3 Tm1 C12 101.95(11) . . ? O2 Tm1 C12 95.32(11) 3_756 . ? O2 Tm1 C12 103.75(10) . . ? O8 Tm1 C12 174.35(11) . . ? O6 Tm1 C12 27.19(11) . . ? O5 Tm1 C12 27.29(10) . . ? N3 Tm1 C12 93.51(11) . . ? N1 Tm1 C12 92.83(11) 3_756 . ? O3 Tm1 Tm1 156.46(7) . 3_756 ? O2 Tm1 Tm1 34.50(6) 3_756 3_756 ? O2 Tm1 Tm1 34.49(6) . 3_756 ? O8 Tm1 Tm1 77.33(7) . 3_756 ? O6 Tm1 Tm1 126.46(8) . 3_756 ? O5 Tm1 Tm1 76.78(7) . 3_756 ? N3 Tm1 Tm1 99.53(9) . 3_756 ? N1 Tm1 Tm1 97.78(9) 3_756 3_756 ? C12 Tm1 Tm1 101.56(8) . 3_756 ? N1 O1 H1 106(4) . . ? C3 O2 Tm1 126.2(2) . 3_756 ? C3 O2 Tm1 120.8(2) . . ? Tm1 O2 Tm1 111.01(9) 3_756 . ? C10 O3 Tm1 131.6(2) . . ? C9 O4 C11 117.6(3) . . ? C12 O5 Tm1 92.9(2) . . ? C12 O6 Tm1 93.6(2) . . ? Tm1 O8 H8A 124(3) . . ? Tm1 O8 H8B 128(3) . . ? H8A O8 H8B 106(3) . . ? H9A O9 H9B 111(4) . . ? C2 N1 O1 114.7(3) . . ? C2 N1 Tm1 122.8(2) . 3_756 ? O1 N1 Tm1 122.5(2) . 3_756 ? C3 N2 N3 110.0(3) . . ? C4 N3 N2 114.0(3) . . ? C4 N3 Tm1 127.4(2) . . ? N2 N3 Tm1 118.6(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 126.3(3) . . ? N1 C2 C3 111.0(3) . . ? C1 C2 C3 122.7(3) . . ? N2 C3 O2 123.3(3) . . ? N2 C3 C2 120.8(3) . . ? O2 C3 C2 115.9(3) . . ? N3 C4 C5 125.1(3) . . ? N3 C4 H4 117.4 . . ? C5 C4 H4 117.4 . . ? C6 C5 C10 119.1(3) . . ? C6 C5 C4 116.8(3) . . ? C10 C5 C4 124.1(3) . . ? C7 C6 C5 121.5(4) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 120.1(4) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? O4 C9 C8 126.0(4) . . ? O4 C9 C10 112.9(3) . . ? C8 C9 C10 121.1(4) . . ? O3 C10 C5 123.5(3) . . ? O3 C10 C9 118.7(3) . . ? C5 C10 C9 117.8(3) . . ? O4 C11 H11A 109.5 . . ? O4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O6 C12 O5 118.9(4) . . ? O6 C12 C13 120.4(4) . . ? O5 C12 C13 120.7(4) . . ? O6 C12 Tm1 59.2(2) . . ? O5 C12 Tm1 59.8(2) . . ? C13 C12 Tm1 178.2(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.464 _refine_diff_density_min -2.319 _refine_diff_density_rms 0.181 _iucr_refine_instructions_details ; TITL _SST-45-12R CELL 0.71075 9.04400 14.78100 14.49087 90.000 113.965 90.000 ZERR 2 0.00800 0.01100 0.01201 0.000 0.017 0.000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H N O TM UNIT 52 72 12 32 4 SHEL 8.147180 0.796452 L.S. 5 FMAP 2 PLAN -15 TEMP -110.0 ACTA BOND $H OMIT 0 0 2 OMIT -1 0 2 OMIT -2 0 6 SIZE 0.310 0.170 0.200 DFIX 0.8400 0.0200 O1 H1 DFIX 0.8700 0.0020 O9 H9A DFIX 0.8700 0.0200 O9 H9B DFIX 0.8804 0.0200 O8 H8A DFIX 0.8803 0.0200 O8 H8B DANG 1.4725 0.0400 H8A H8B DANG 1.3829 0.0400 H9A H9B WGHT 0.023600 2.631300 FVAR 0.79004 TM1 5 0.856453 0.099141 0.450781 11.00000 0.01352 0.01039 = 0.01754 0.00105 0.00160 0.00083 O1 4 0.980780 -0.313079 0.499942 11.00000 0.02856 0.01059 = 0.04923 -0.00130 0.01098 0.00205 H1 2 1.084136 -0.314921 0.531729 11.00000 -1.50000 O2 4 0.877706 -0.053520 0.484063 11.00000 0.01131 0.01201 = 0.02435 -0.00023 0.00149 -0.00059 O3 4 0.699225 0.207279 0.456858 11.00000 0.02136 0.01792 = 0.03101 -0.00086 0.00408 0.00582 O4 4 0.620823 0.375255 0.406099 11.00000 0.04281 0.01768 = 0.03016 0.00282 0.00870 0.00362 O5 4 0.862948 0.034948 0.299769 11.00000 0.03386 0.02731 = 0.02263 0.00221 0.00925 0.00745 O6 4 0.794136 0.177945 0.295125 11.00000 0.06049 0.02281 = 0.02887 0.00898 0.01592 0.00910 O8 4 0.907170 0.097260 0.620599 11.00000 0.02533 0.02598 = 0.02128 0.00101 0.00764 0.00886 H8A 2 0.976128 0.059931 0.665021 11.00000 -1.50000 H8B 2 0.847744 0.121215 0.650934 11.00000 -1.50000 O9 4 0.723958 0.351985 0.212520 11.00000 0.02550 0.02855 = 0.04052 0.01368 0.01304 0.00364 H9A 2 0.736008 0.301280 0.245239 11.00000 -1.50000 H9B 2 0.622035 0.362602 0.176135 11.00000 -1.50000 N1 3 0.938559 -0.221892 0.492658 11.00000 0.02139 0.01360 = 0.02506 0.00001 0.00711 0.00311 N2 3 0.600708 -0.075967 0.406239 11.00000 0.01900 0.01290 = 0.02350 -0.00141 0.00798 -0.00068 N3 3 0.600879 0.020993 0.405524 11.00000 0.01679 0.01280 = 0.01915 -0.00084 0.00393 -0.00192 C1 1 0.652400 -0.275914 0.414924 11.00000 0.02327 0.01430 = 0.04116 -0.00223 0.00994 -0.00179 AFIX 137 H1A 2 0.606219 -0.277354 0.340945 11.00000 -1.20000 H1B 2 0.567588 -0.260486 0.437993 11.00000 -1.20000 H1C 2 0.697363 -0.335459 0.441391 11.00000 -1.20000 AFIX 0 C2 1 0.783932 -0.206262 0.452296 11.00000 0.02027 0.01737 = 0.02211 -0.00181 0.00958 -0.00199 C3 1 0.750081 -0.106508 0.446396 11.00000 0.01569 0.01697 = 0.01451 -0.00140 0.00521 -0.00258 C4 1 0.459356 0.056776 0.381060 11.00000 0.01700 0.01945 = 0.02347 0.00081 0.00671 0.00097 AFIX 43 H4 2 0.371284 0.016953 0.369914 11.00000 -1.20000 AFIX 0 C5 1 0.424195 0.154383 0.369154 11.00000 0.02101 0.02434 = 0.02086 0.00382 0.00805 0.00685 C6 1 0.259147 0.179665 0.319769 11.00000 0.02280 0.03230 = 0.04372 0.00550 0.01073 0.00622 AFIX 43 H6 2 0.178145 0.134107 0.301318 11.00000 -1.20000 AFIX 0 C7 1 0.213786 0.268376 0.298034 11.00000 0.03007 0.03765 = 0.04618 0.00710 0.00860 0.01799 AFIX 43 H7 2 0.102454 0.283593 0.264770 11.00000 -1.20000 AFIX 0 C8 1 0.332061 0.336937 0.324971 11.00000 0.03784 0.02576 = 0.03216 0.00729 0.01116 0.01759 AFIX 43 H8 2 0.300472 0.398141 0.308248 11.00000 -1.20000 AFIX 0 C9 1 0.494259 0.315379 0.375763 11.00000 0.03359 0.02326 = 0.01898 0.00180 0.01135 0.00659 C10 1 0.545289 0.223469 0.402584 11.00000 0.02301 0.02114 = 0.01675 0.00021 0.00879 0.00811 C11 1 0.584905 0.467781 0.377320 11.00000 0.05888 0.02324 = 0.03930 0.00638 0.01217 0.00713 AFIX 137 H11A 2 0.531082 0.472045 0.303572 11.00000 -1.20000 H11B 2 0.685571 0.502797 0.401469 11.00000 -1.20000 H11C 2 0.513415 0.491989 0.407172 11.00000 -1.20000 AFIX 0 C12 1 0.824772 0.109846 0.251950 11.00000 0.01926 0.02615 = 0.02034 0.00141 0.00257 -0.00330 C13 1 0.812752 0.117252 0.146386 11.00000 0.04983 0.04811 = 0.02303 0.00539 0.01467 -0.00340 AFIX 137 H13A 2 0.698669 0.121203 0.099459 11.00000 -1.20000 H13B 2 0.861764 0.063756 0.130266 11.00000 -1.20000 H13C 2 0.869932 0.171659 0.140135 11.00000 -1.20000 HKLF 4 REM _SST-45-12R REM R1 = 0.0314 for 3542 Fo > 4sig(Fo) and 0.0321 for all 3661 data REM 244 parameters refined using 7 restraints END WGHT 0.0236 2.6310 REM Highest difference peak 1.464, deepest hole -2.319, 1-sigma level 0.181 Q1 1 0.8808 0.0952 0.3950 11.00000 0.05 1.46 Q2 1 0.8808 0.0984 0.5220 11.00000 0.05 0.93 Q3 1 0.8294 0.1801 0.4191 11.00000 0.05 0.76 Q4 1 0.8228 0.0050 0.4236 11.00000 0.05 0.68 Q5 1 0.8772 0.1757 0.4833 11.00000 0.05 0.66 Q6 1 0.7704 0.0536 0.1090 11.00000 0.05 0.64 Q7 1 0.9684 0.0435 0.5775 11.00000 0.05 0.60 Q8 1 0.7972 0.0418 0.4286 11.00000 0.05 0.60 Q9 1 1.0185 0.1836 0.5036 11.00000 0.05 0.59 Q10 1 0.9697 0.1516 0.5780 11.00000 0.05 0.58 Q11 1 0.6989 0.1760 0.5802 11.00000 0.05 0.58 Q12 1 0.9270 0.0496 0.4591 11.00000 0.05 0.57 Q13 1 0.6963 0.1915 0.4015 11.00000 0.05 0.56 Q14 1 0.5232 0.1507 0.4446 11.00000 0.05 0.56 Q15 1 0.5612 -0.2538 0.3787 11.00000 0.05 0.54 ; data_7-Revised _database_code_depnum_ccdc_archive 'CCDC 910744' #TrackingRef 'Revised_Ln6_Combined_CIF.cif' # start Validation Reply Form _vrf_DIFMX01_7-Revised ; PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 RESPONSE: From shelxl.lst Electron density synthesis with coefficients Fo-Fc Highest peak 7.57 at 0.2253 0.2798 0.4637 [ 0.06 A from GD1 ] Deepest hole -3.25 at 0.3371 0.5885 0.3484 [ 0.87 A from GD2 ] The highest peak and deepest trough are therefore sensibly associated with the heaviest atom site in the structure. These do not indicate that an atom has been missed or incorrectly assigned. ; _vrf_PLAT097_7-Revised ; PROBLEM: Large Reported Max. (Positive) Residual Density RESPONSE: From shelxl.lst Electron density synthesis with coefficients Fo-Fc Highest peak 7.57 at 0.2253 0.2798 0.4637 [ 0.06 A from GD1 ] Deepest hole -3.25 at 0.3371 0.5885 0.3484 [ 0.87 A from GD2 ] The highest peak and deepest trough are therefore sensibly associated with the heaviest atom site in the structure. These do not indicate that an atom has been missed or incorrectly assigned. ; _vrf_PLAT420_7-Revised ; PROBLEM: D-H Without Acceptor RESPONSE: O5 was introduced by shelxl HFIX 147, while O13 is a water molecule and H13A does participate in H-bonding. ; _vrf_DIFMX02_7-Revised ; PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 RESPONSE: From shelxl.lst Electron density synthesis with coefficients Fo-Fc Highest peak 7.57 at 0.2253 0.2798 0.4637 [ 0.06 A from GD1 ] Deepest hole -3.25 at 0.3371 0.5885 0.3484 [ 0.87 A from GD2 ] The highest peak and deepest trough are therefore sensibly associated with the heaviest atom site in the structure. These do not indicate that an atom has been missed or incorrectly assigned. ; _vrf_PLAT094_7-Revised ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... RESPONSE: From shelxl.lst Electron density synthesis with coefficients Fo-Fc Highest peak 7.57 at 0.2253 0.2798 0.4637 [ 0.06 A from GD1 ] Deepest hole -3.25 at 0.3371 0.5885 0.3484 [ 0.87 A from GD2 ] The highest peak and deepest trough are therefore sensibly associated with the heaviest atom site in the structure. These do not indicate that an atom has been missed or incorrectly assigned. ; _vrf_PLAT003_7-Revised ; PROBLEM: Number of Uiso or Uij Restrained Atom Sites .... 2 RESPONSE: SIMU restraints were applied to the lattice solvent methanol molecule, C37-O16. ; _vrf_PLAT007_7-Revised ; PROBLEM: Note: Number of Unrefined D-H Atoms ............ 7 RESPONSE: H-atoms can be difficult to locate and refine in the presence of heavy atoms, such as Gd. For this reason, H-atoms were introduced in calculated positions and refined on a riding model. ; _vrf_PLAT860_7-Revised ; PROBLEM: Note: Number of Least-Squares Restraints ....... 6 RESPONSE: H-atoms can be difficult to locate and refine in the presence of heavy atoms, such as Gd. For this reason, H-atoms were introduced in calculated positions and refined on a riding model. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H72 Gd4 N12 O28, C H4 O' _chemical_formula_sum 'C73 H76 Gd4 N12 O29' _chemical_formula_weight 2214.47 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' Gd Gd -0.1653 3.9035 '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' _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 12.845(5) _cell_length_b 13.379(6) _cell_length_c 15.046(7) _cell_angle_alpha 74.15(2) _cell_angle_beta 66.72(2) _cell_angle_gamma 64.47(2) _cell_volume 2126.7(16) _cell_formula_units_Z 1 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 7049 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 29.7 _exptl_crystal_description Prism _exptl_crystal_colour 'Light Yellow' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 3.171 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.917 _exptl_absorpt_correction_T_min 0.736 _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 17379 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8715 _reflns_number_gt 7044 _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. A SIMU restraints were applied to the half-occupancy lattice solvent methanol molecule, C37-O16. ; _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 8715 _refine_ls_number_parameters 551 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.3015 _refine_ls_wR_factor_gt 0.2392 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.22235(4) 0.27769(3) 0.46324(3) 0.0281(2) Uani 1 1 d . . . Gd2 Gd 0.31913(4) 0.53796(3) 0.33790(3) 0.0262(2) Uani 1 1 d . . . O1 O -0.2831(7) 0.2147(6) 0.8254(5) 0.0441(17) Uani 1 1 d . . . H1 H -0.3563 0.2579 0.8378 0.053 Uiso 1 1 calc R . . O2 O 0.0900(6) 0.2246(6) 0.6116(5) 0.0384(16) Uani 1 1 d . . . O3 O 0.1876(6) 0.4425(5) 0.3576(4) 0.0285(13) Uani 1 1 d . . . O4 O 0.2733(7) 0.5418(6) 0.1855(4) 0.0345(16) Uani 1 1 d . . . O5 O 0.2710(7) 0.1704(6) 0.6905(5) 0.0405(16) Uani 1 1 d . . . H5 H 0.3234 0.1057 0.6835 0.049 Uiso 1 1 calc R . . O6 O 0.3188(6) 0.3978(5) 0.4701(5) 0.0304(14) Uani 1 1 d . . . O7 O 0.4573(6) 0.6107(5) 0.2288(5) 0.0346(14) Uani 1 1 d . . . O8 O 0.5354(7) 0.7022(7) 0.0541(5) 0.0435(17) Uani 1 1 d . . . O9 O 0.1819(7) 0.2068(6) 0.3612(6) 0.0419(18) Uani 1 1 d . . . O10 O 0.2859(13) 0.0223(8) 0.3558(8) 0.089(4) Uani 1 1 d . . . O11 O 0.4126(6) 0.2278(6) 0.3424(5) 0.0409(16) Uani 1 1 d . . . O12 O 0.4560(6) 0.3775(5) 0.2576(5) 0.0313(13) Uani 1 1 d . . . O13 O 0.3171(7) 0.0753(6) 0.4965(5) 0.0451(18) Uani 1 1 d . . . H13A H 0.2749 0.0521 0.5537 0.068 Uiso 1 1 d R . . H13B H 0.3185 0.0440 0.4520 0.068 Uiso 1 1 d R . . O14 O 0.3059(6) 0.6451(6) 0.4533(5) 0.0348(15) Uani 1 1 d . . . H14A H 0.3790 0.6260 0.4583 0.052 Uiso 1 1 d R . . H14B H 0.2786 0.7178 0.4331 0.052 Uiso 1 1 d R . . N1 N -0.2117(9) 0.2603(7) 0.7400(7) 0.0363(19) Uani 1 1 d . . . N2 N -0.0851(7) 0.3405(6) 0.5768(6) 0.0286(16) Uani 1 1 d . . . N3 N -0.0068(7) 0.3771(6) 0.4918(6) 0.0307(16) Uani 1 1 d . . . N4 N 0.3010(7) 0.2426(6) 0.6073(6) 0.0281(16) Uani 1 1 d . . . N5 N 0.5036(8) 0.3761(7) 0.4760(5) 0.0326(17) Uani 1 1 d . . . N6 N 0.5097(7) 0.4463(6) 0.3884(5) 0.0300(16) Uani 1 1 d . . . C1 C -0.0384(12) 0.1149(11) 0.7859(11) 0.067(4) Uani 1 1 d . . . H1A H -0.0885 0.1221 0.8543 0.081 Uiso 1 1 calc R . . H1B H 0.0426 0.1126 0.7764 0.081 Uiso 1 1 calc R . . H1C H -0.0306 0.0459 0.7686 0.081 Uiso 1 1 calc R . . C2 C -0.0964(9) 0.2113(9) 0.7232(8) 0.036(2) Uani 1 1 d . . . C3 C -0.0253(9) 0.2629(8) 0.6317(7) 0.033(2) Uani 1 1 d . . . C4 C -0.0582(9) 0.4367(7) 0.4284(7) 0.0313(19) Uani 1 1 d . . . H4 H -0.1416 0.4482 0.4448 0.038 Uiso 1 1 calc R . . C5 C -0.0033(9) 0.4893(8) 0.3335(7) 0.033(2) Uani 1 1 d . . . C6 C -0.0737(9) 0.5441(8) 0.2701(7) 0.037(2) Uani 1 1 d . . . H6 H -0.1540 0.5444 0.2909 0.044 Uiso 1 1 calc R . . C7 C -0.0296(10) 0.5975(9) 0.1785(7) 0.042(2) Uani 1 1 d . . . H7 H -0.0796 0.6346 0.1378 0.051 Uiso 1 1 calc R . . C8 C 0.0860(11) 0.5963(9) 0.1471(7) 0.039(2) Uani 1 1 d . . . H8 H 0.1173 0.6310 0.0837 0.047 Uiso 1 1 calc R . . C9 C 0.1577(10) 0.5454(8) 0.2067(7) 0.032(2) Uani 1 1 d . . . C10 C 0.1175(9) 0.4873(8) 0.3021(6) 0.0295(19) Uani 1 1 d . . . C11 C 0.3384(11) 0.5667(11) 0.0851(7) 0.046(3) Uani 1 1 d . . . H11A H 0.3285 0.5273 0.0446 0.055 Uiso 1 1 calc R . . H11B H 0.4250 0.5424 0.0769 0.055 Uiso 1 1 calc R . . H11C H 0.3061 0.6473 0.0653 0.055 Uiso 1 1 calc R . . C12 C 0.4566(9) 0.2334(10) 0.6700(7) 0.037(2) Uani 1 1 d . . . H12A H 0.4244 0.1836 0.7246 0.045 Uiso 1 1 calc R . . H12B H 0.4491 0.2977 0.6946 0.045 Uiso 1 1 calc R . . H12C H 0.5425 0.1930 0.6363 0.045 Uiso 1 1 calc R . . C13 C 0.3854(8) 0.2733(8) 0.5999(6) 0.0277(18) Uani 1 1 d . . . C14 C 0.4034(8) 0.3546(7) 0.5123(6) 0.0248(17) Uani 1 1 d . . . C15 C 0.6229(9) 0.4341(7) 0.3326(7) 0.0329(19) Uani 1 1 d . . . H15 H 0.6865 0.3864 0.3591 0.039 Uiso 1 1 calc R . . C16 C 0.6569(8) 0.4892(8) 0.2325(6) 0.0295(19) Uani 1 1 d . . . C17 C 0.7840(9) 0.4503(9) 0.1810(7) 0.041(2) Uani 1 1 d . . . H17 H 0.8389 0.3924 0.2117 0.049 Uiso 1 1 calc R . . C18 C 0.8283(10) 0.4968(9) 0.0853(7) 0.042(2) Uani 1 1 d . . . H18 H 0.9130 0.4712 0.0503 0.050 Uiso 1 1 calc R . . C19 C 0.7457(10) 0.5813(9) 0.0428(8) 0.038(2) Uani 1 1 d . . . H19 H 0.7751 0.6139 -0.0220 0.046 Uiso 1 1 calc R . . C20 C 0.6240(9) 0.6191(8) 0.0909(8) 0.032(2) Uani 1 1 d . . . C21 C 0.5734(8) 0.5753(8) 0.1890(7) 0.0316(19) Uani 1 1 d . . . C22 C 0.5708(12) 0.7592(13) -0.0409(9) 0.060(3) Uani 1 1 d . . . H22A H 0.6150 0.8035 -0.0411 0.071 Uiso 1 1 calc R . . H22B H 0.4982 0.8087 -0.0595 0.071 Uiso 1 1 calc R . . H22C H 0.6236 0.7047 -0.0875 0.071 Uiso 1 1 calc R . . C23 C 0.2246(10) 0.1188(8) 0.3208(8) 0.040(2) Uani 1 1 d . . . C24 C 0.2012(10) 0.1265(8) 0.2305(8) 0.040(2) Uani 1 1 d . . . C25 C 0.1152(10) 0.2233(9) 0.1991(8) 0.043(2) Uani 1 1 d . . . H25 H 0.0693 0.2831 0.2378 0.052 Uiso 1 1 calc R . . C26 C 0.0967(13) 0.2323(10) 0.1124(8) 0.055(3) Uani 1 1 d . . . H26 H 0.0410 0.2996 0.0903 0.066 Uiso 1 1 calc R . . C27 C 0.1588(14) 0.1439(11) 0.0575(9) 0.052(3) Uani 1 1 d . . . H27 H 0.1453 0.1503 -0.0018 0.063 Uiso 1 1 calc R . . C28 C 0.2400(13) 0.0468(10) 0.0891(9) 0.060(3) Uani 1 1 d . . . H28 H 0.2797 -0.0149 0.0528 0.072 Uiso 1 1 calc R . . C29 C 0.2650(13) 0.0375(10) 0.1743(9) 0.050(3) Uani 1 1 d . . . H29 H 0.3245 -0.0284 0.1937 0.060 Uiso 1 1 calc R . . C30 C 0.4777(9) 0.2741(8) 0.2735(7) 0.036(2) Uani 1 1 d . . . C31 C 0.5963(8) 0.2014(8) 0.2076(6) 0.0296(18) Uani 1 1 d . . . C32 C 0.6838(13) 0.2418(10) 0.1480(8) 0.054(3) Uani 1 1 d . . . H32 H 0.6732 0.3166 0.1481 0.064 Uiso 1 1 calc R . . C33 C 0.7890(10) 0.1738(9) 0.0869(8) 0.049(3) Uani 1 1 d . . . H33 H 0.8489 0.2036 0.0436 0.059 Uiso 1 1 calc R . . C34 C 0.8085(12) 0.0651(10) 0.0873(8) 0.058(3) Uani 1 1 d . . . H34 H 0.8834 0.0177 0.0484 0.070 Uiso 1 1 calc R . . C35 C 0.7183(11) 0.0264(9) 0.1449(7) 0.044(3) Uani 1 1 d . . . H35 H 0.7279 -0.0472 0.1418 0.053 Uiso 1 1 calc R . . C36 C 0.6152(12) 0.0897(9) 0.2066(8) 0.049(3) Uani 1 1 d . . . H36 H 0.5556 0.0591 0.2491 0.059 Uiso 1 1 calc R . . O16 O 0.1751(15) 0.8611(13) 0.4575(13) 0.052(4) Uani 0.50 1 d PU A 1 H16 H 0.2240 0.8947 0.4369 0.079 Uiso 0.50 1 calc PR A 1 C37 C 0.106(3) 0.883(2) 0.542(2) 0.092(10) Uani 0.50 1 d PU A 1 H37A H 0.1432 0.9116 0.5706 0.139 Uiso 0.50 1 calc PR A 1 H37B H 0.0941 0.8157 0.5823 0.139 Uiso 0.50 1 calc PR A 1 H37C H 0.0274 0.9403 0.5387 0.139 Uiso 0.50 1 calc PR A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0291(3) 0.0281(3) 0.0303(3) -0.0017(2) -0.0097(2) -0.0142(2) Gd2 0.0277(3) 0.0276(3) 0.0265(3) -0.0014(2) -0.0088(2) -0.0141(2) O1 0.038(4) 0.037(4) 0.051(4) 0.002(3) -0.005(3) -0.021(3) O2 0.032(4) 0.040(4) 0.039(4) 0.004(3) -0.010(3) -0.017(3) O3 0.034(3) 0.032(3) 0.021(3) 0.000(2) -0.008(3) -0.015(3) O4 0.050(4) 0.050(4) 0.015(3) 0.008(3) -0.008(3) -0.038(3) O5 0.046(4) 0.040(4) 0.034(4) 0.013(3) -0.013(3) -0.025(3) O6 0.030(3) 0.029(3) 0.036(3) 0.004(3) -0.014(3) -0.015(3) O7 0.031(3) 0.035(3) 0.039(4) 0.002(3) -0.013(3) -0.016(3) O8 0.036(4) 0.058(5) 0.035(4) 0.006(3) -0.012(3) -0.024(4) O9 0.055(5) 0.027(3) 0.049(4) -0.008(3) -0.026(4) -0.011(3) O10 0.161(12) 0.045(5) 0.078(7) -0.010(5) -0.067(8) -0.027(6) O11 0.036(4) 0.037(4) 0.043(4) -0.010(3) 0.001(3) -0.016(3) O12 0.031(3) 0.027(3) 0.031(3) -0.003(2) -0.007(3) -0.010(3) O13 0.058(5) 0.038(4) 0.036(4) 0.000(3) -0.018(4) -0.014(3) O14 0.038(4) 0.040(4) 0.032(3) -0.009(3) -0.008(3) -0.019(3) N1 0.040(5) 0.031(4) 0.034(5) 0.000(3) -0.008(4) -0.016(4) N2 0.028(4) 0.030(4) 0.036(4) -0.003(3) -0.010(3) -0.019(3) N3 0.035(4) 0.028(4) 0.033(4) -0.008(3) -0.010(3) -0.014(3) N4 0.026(4) 0.028(4) 0.033(4) 0.002(3) -0.011(3) -0.013(3) N5 0.039(4) 0.042(4) 0.026(4) -0.003(3) -0.013(3) -0.022(4) N6 0.030(4) 0.038(4) 0.026(4) -0.002(3) -0.005(3) -0.020(3) C1 0.041(7) 0.046(7) 0.086(10) 0.026(7) -0.018(7) -0.012(5) C2 0.034(5) 0.039(5) 0.041(5) -0.009(4) -0.004(4) -0.024(4) C3 0.037(5) 0.030(4) 0.031(5) 0.003(4) -0.013(4) -0.012(4) C4 0.034(5) 0.025(4) 0.030(5) -0.008(3) -0.007(4) -0.006(4) C5 0.032(5) 0.037(5) 0.039(5) -0.011(4) -0.019(4) -0.011(4) C6 0.036(5) 0.046(5) 0.033(5) -0.005(4) -0.015(4) -0.014(4) C7 0.049(6) 0.055(6) 0.035(5) 0.000(4) -0.026(5) -0.023(5) C8 0.051(6) 0.050(6) 0.025(5) 0.005(4) -0.019(4) -0.025(5) C9 0.049(6) 0.038(5) 0.028(4) 0.000(4) -0.018(4) -0.029(4) C10 0.034(5) 0.038(5) 0.027(4) -0.001(4) -0.013(4) -0.021(4) C11 0.052(7) 0.076(8) 0.023(5) -0.001(5) -0.004(4) -0.046(6) C12 0.031(5) 0.061(6) 0.033(5) 0.003(4) -0.019(4) -0.025(5) C13 0.027(4) 0.031(4) 0.027(4) -0.008(3) -0.009(4) -0.009(4) C14 0.024(4) 0.031(4) 0.022(4) 0.001(3) -0.012(3) -0.011(3) C15 0.036(5) 0.028(4) 0.032(5) -0.004(3) -0.008(4) -0.013(4) C16 0.030(5) 0.037(5) 0.026(4) 0.006(3) -0.012(4) -0.021(4) C17 0.025(5) 0.047(5) 0.037(5) 0.001(4) -0.002(4) -0.012(4) C18 0.036(5) 0.044(5) 0.038(5) 0.003(4) -0.011(4) -0.014(4) C19 0.035(5) 0.044(6) 0.036(5) -0.002(4) -0.007(4) -0.021(5) C20 0.033(5) 0.033(5) 0.042(5) 0.005(4) -0.021(4) -0.020(4) C21 0.024(4) 0.034(5) 0.032(5) -0.009(4) -0.005(4) -0.007(4) C22 0.047(7) 0.086(9) 0.042(6) 0.018(6) -0.017(5) -0.035(7) C23 0.052(6) 0.034(5) 0.046(6) -0.007(4) -0.027(5) -0.016(5) C24 0.053(6) 0.040(5) 0.042(6) -0.011(4) -0.023(5) -0.019(5) C25 0.039(6) 0.039(5) 0.042(6) -0.007(4) -0.008(5) -0.010(4) C26 0.071(8) 0.051(7) 0.039(6) -0.008(5) -0.022(6) -0.012(6) C27 0.072(9) 0.049(7) 0.040(6) 0.003(5) -0.026(6) -0.024(6) C28 0.083(10) 0.038(6) 0.053(7) -0.012(5) -0.019(7) -0.016(6) C29 0.076(9) 0.038(6) 0.046(6) -0.011(5) -0.032(6) -0.014(6) C30 0.031(5) 0.039(5) 0.036(5) -0.010(4) -0.014(4) -0.005(4) C31 0.023(4) 0.038(5) 0.031(5) 0.000(4) -0.017(4) -0.008(4) C32 0.079(9) 0.038(6) 0.038(6) -0.008(4) -0.007(6) -0.024(6) C33 0.034(5) 0.048(6) 0.045(6) 0.002(5) 0.000(5) -0.013(5) C34 0.053(7) 0.049(6) 0.049(7) -0.023(5) 0.013(5) -0.014(5) C35 0.052(7) 0.037(5) 0.026(5) 0.004(4) -0.012(5) -0.007(5) C36 0.068(8) 0.036(5) 0.041(6) -0.007(4) -0.021(5) -0.011(5) O16 0.048(9) 0.035(7) 0.069(10) -0.012(7) -0.007(7) -0.018(7) C37 0.078(15) 0.054(13) 0.083(16) 0.018(12) 0.006(13) -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 Gd1 O9 2.319(7) . ? Gd1 O3 2.320(6) . ? Gd1 O11 2.339(7) . ? Gd1 O2 2.357(7) . ? Gd1 O13 2.442(7) . ? Gd1 O6 2.456(6) . ? Gd1 N3 2.560(8) . ? Gd1 N4 2.591(8) . ? Gd1 Gd2 3.9394(17) . ? Gd2 O7 2.259(6) . ? Gd2 O6 2.331(6) . ? Gd2 O12 2.376(6) . ? Gd2 O3 2.415(6) . ? Gd2 O14 2.453(6) . ? Gd2 N6 2.540(8) . ? Gd2 O4 2.566(6) . ? Gd2 N1 2.627(9) 2_566 ? Gd2 N2 2.685(8) 2_566 ? O1 N1 1.409(10) . ? O1 H1 0.8400 . ? O2 C3 1.273(12) . ? O3 C10 1.313(11) . ? O4 C9 1.373(12) . ? O4 C11 1.434(10) . ? O5 N4 1.388(9) . ? O5 H5 0.8400 . ? O6 C14 1.313(10) . ? O7 C21 1.283(11) . ? O8 C20 1.382(12) . ? O8 C22 1.421(12) . ? O9 C23 1.275(12) . ? O10 C23 1.283(14) . ? O11 C30 1.253(12) . ? O12 C30 1.259(12) . ? O13 H13A 0.8725 . ? O13 H13B 0.8723 . ? O14 H14A 0.8890 . ? O14 H14B 0.8891 . ? N1 C2 1.282(14) . ? N1 Gd2 2.627(9) 2_566 ? N2 C3 1.302(12) . ? N2 N3 1.397(10) . ? N2 Gd2 2.685(8) 2_566 ? N3 C4 1.268(12) . ? N4 C13 1.272(12) . ? N5 C14 1.309(12) . ? N5 N6 1.389(10) . ? N6 C15 1.323(12) . ? C1 C2 1.474(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.496(13) . ? C4 C5 1.455(13) . ? C4 H4 0.9500 . ? C5 C6 1.413(13) . ? C5 C10 1.422(13) . ? C6 C7 1.388(13) . ? C6 H6 0.9500 . ? C7 C8 1.363(15) . ? C7 H7 0.9500 . ? C8 C9 1.376(13) . ? C8 H8 0.9500 . ? C9 C10 1.442(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.505(12) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.471(12) . ? C15 C16 1.467(12) . ? C15 H15 0.9500 . ? C16 C21 1.409(13) . ? C16 C17 1.423(13) . ? C17 C18 1.397(13) . ? C17 H17 0.9500 . ? C18 C19 1.386(15) . ? C18 H18 0.9500 . ? C19 C20 1.359(15) . ? C19 H19 0.9500 . ? C20 C21 1.429(13) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.472(13) . ? C24 C25 1.402(15) . ? C24 C29 1.403(15) . ? C25 C26 1.381(16) . ? C25 H25 0.9500 . ? C26 C27 1.385(18) . ? C26 H26 0.9500 . ? C27 C28 1.374(19) . ? C27 H27 0.9500 . ? C28 C29 1.401(17) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.518(13) . ? C31 C32 1.349(15) . ? C31 C36 1.411(14) . ? C32 C33 1.384(16) . ? C32 H32 0.9500 . ? C33 C34 1.364(16) . ? C33 H33 0.9500 . ? C34 C35 1.357(17) . ? C34 H34 0.9500 . ? C35 C36 1.350(16) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? O16 C37 1.26(3) . ? O16 H16 0.8400 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 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 O9 Gd1 O3 86.2(2) . . ? O9 Gd1 O11 80.0(3) . . ? O3 Gd1 O11 82.0(2) . . ? O9 Gd1 O2 97.6(3) . . ? O3 Gd1 O2 129.9(2) . . ? O11 Gd1 O2 148.0(2) . . ? O9 Gd1 O13 75.2(3) . . ? O3 Gd1 O13 152.1(2) . . ? O11 Gd1 O13 74.4(3) . . ? O2 Gd1 O13 74.2(3) . . ? O9 Gd1 O6 145.0(2) . . ? O3 Gd1 O6 66.6(2) . . ? O11 Gd1 O6 74.9(2) . . ? O2 Gd1 O6 116.6(2) . . ? O13 Gd1 O6 119.5(2) . . ? O9 Gd1 N3 74.9(3) . . ? O3 Gd1 N3 70.7(2) . . ? O11 Gd1 N3 143.7(3) . . ? O2 Gd1 N3 62.5(2) . . ? O13 Gd1 N3 122.4(2) . . ? O6 Gd1 N3 113.2(2) . . ? O9 Gd1 N4 148.8(2) . . ? O3 Gd1 N4 124.3(2) . . ? O11 Gd1 N4 97.0(3) . . ? O2 Gd1 N4 68.7(2) . . ? O13 Gd1 N4 74.1(2) . . ? O6 Gd1 N4 59.7(2) . . ? N3 Gd1 N4 118.0(2) . . ? O9 Gd1 Gd2 113.77(19) . . ? O3 Gd1 Gd2 34.49(16) . . ? O11 Gd1 Gd2 68.67(16) . . ? O2 Gd1 Gd2 137.78(18) . . ? O13 Gd1 Gd2 139.13(19) . . ? O6 Gd1 Gd2 33.61(14) . . ? N3 Gd1 Gd2 98.06(16) . . ? N4 Gd1 Gd2 93.29(16) . . ? O7 Gd2 O6 135.6(2) . . ? O7 Gd2 O12 81.8(2) . . ? O6 Gd2 O12 79.2(2) . . ? O7 Gd2 O3 144.8(2) . . ? O6 Gd2 O3 67.1(2) . . ? O12 Gd2 O3 77.2(2) . . ? O7 Gd2 O14 85.7(2) . . ? O6 Gd2 O14 83.4(2) . . ? O12 Gd2 O14 139.5(2) . . ? O3 Gd2 O14 128.0(2) . . ? O7 Gd2 N6 72.9(2) . . ? O6 Gd2 N6 63.0(2) . . ? O12 Gd2 N6 69.2(2) . . ? O3 Gd2 N6 123.5(2) . . ? O14 Gd2 N6 70.4(2) . . ? O7 Gd2 O4 83.0(2) . . ? O6 Gd2 O4 125.0(2) . . ? O12 Gd2 O4 68.6(2) . . ? O3 Gd2 O4 63.12(19) . . ? O14 Gd2 O4 147.4(2) . . ? N6 Gd2 O4 133.7(2) . . ? O7 Gd2 N1 68.9(3) . 2_566 ? O6 Gd2 N1 149.8(3) . 2_566 ? O12 Gd2 N1 128.0(3) . 2_566 ? O3 Gd2 N1 102.9(2) . 2_566 ? O14 Gd2 N1 81.4(3) . 2_566 ? N6 Gd2 N1 133.6(3) . 2_566 ? O4 Gd2 N1 66.0(3) . 2_566 ? O7 Gd2 N2 124.3(2) . 2_566 ? O6 Gd2 N2 91.8(2) . 2_566 ? O12 Gd2 N2 145.8(2) . 2_566 ? O3 Gd2 N2 69.0(2) . 2_566 ? O14 Gd2 N2 70.3(2) . 2_566 ? N6 Gd2 N2 135.1(2) . 2_566 ? O4 Gd2 N2 91.2(2) . 2_566 ? N1 Gd2 N2 58.5(3) 2_566 2_566 ? O7 Gd2 Gd1 149.68(18) . . ? O6 Gd2 Gd1 35.68(15) . . ? O12 Gd2 Gd1 68.23(15) . . ? O3 Gd2 Gd1 32.95(15) . . ? O14 Gd2 Gd1 113.88(16) . . ? N6 Gd2 Gd1 91.50(16) . . ? O4 Gd2 Gd1 90.12(13) . . ? N1 Gd2 Gd1 134.2(2) 2_566 . ? N2 Gd2 Gd1 85.22(15) 2_566 . ? N1 O1 H1 109.5 . . ? C3 O2 Gd1 123.3(6) . . ? C10 O3 Gd1 131.8(5) . . ? C10 O3 Gd2 115.3(5) . . ? Gd1 O3 Gd2 112.6(3) . . ? C9 O4 C11 117.3(7) . . ? C9 O4 Gd2 112.5(5) . . ? C11 O4 Gd2 128.4(6) . . ? N4 O5 H5 109.5 . . ? C14 O6 Gd2 123.3(5) . . ? C14 O6 Gd1 118.6(5) . . ? Gd2 O6 Gd1 110.7(2) . . ? C21 O7 Gd2 136.4(6) . . ? C20 O8 C22 119.2(9) . . ? C23 O9 Gd1 139.4(7) . . ? C30 O11 Gd1 138.8(6) . . ? C30 O12 Gd2 137.7(6) . . ? Gd1 O13 H13A 109.5 . . ? Gd1 O13 H13B 109.2 . . ? H13A O13 H13B 109.4 . . ? Gd2 O14 H14A 110.1 . . ? Gd2 O14 H14B 110.3 . . ? H14A O14 H14B 108.6 . . ? C2 N1 O1 114.8(9) . . ? C2 N1 Gd2 124.9(7) . 2_566 ? O1 N1 Gd2 117.8(6) . 2_566 ? C3 N2 N3 111.5(8) . . ? C3 N2 Gd2 118.0(6) . 2_566 ? N3 N2 Gd2 125.2(5) . 2_566 ? C4 N3 N2 113.3(8) . . ? C4 N3 Gd1 126.9(6) . . ? N2 N3 Gd1 117.5(5) . . ? C13 N4 O5 115.2(7) . . ? C13 N4 Gd1 122.3(6) . . ? O5 N4 Gd1 121.4(5) . . ? C14 N5 N6 112.4(7) . . ? C15 N6 N5 112.8(8) . . ? C15 N6 Gd2 127.6(6) . . ? N5 N6 Gd2 117.4(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 124.7(10) . . ? N1 C2 C3 112.5(9) . . ? C1 C2 C3 122.9(10) . . ? O2 C3 N2 124.9(9) . . ? O2 C3 C2 117.3(8) . . ? N2 C3 C2 117.7(9) . . ? N3 C4 C5 127.1(9) . . ? N3 C4 H4 116.5 . . ? C5 C4 H4 116.5 . . ? C6 C5 C10 119.0(9) . . ? C6 C5 C4 118.0(9) . . ? C10 C5 C4 123.0(8) . . ? C7 C6 C5 122.2(9) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C8 C7 C6 119.6(9) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 120.4(9) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? O4 C9 C8 126.2(9) . . ? O4 C9 C10 111.2(8) . . ? C8 C9 C10 122.5(9) . . ? O3 C10 C5 123.1(8) . . ? O3 C10 C9 120.5(8) . . ? C5 C10 C9 116.2(8) . . ? O4 C11 H11A 109.5 . . ? O4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C14 109.9(8) . . ? N4 C13 C12 125.5(9) . . ? C14 C13 C12 124.6(8) . . ? N5 C14 O6 122.5(7) . . ? N5 C14 C13 120.5(8) . . ? O6 C14 C13 116.9(7) . . ? N6 C15 C16 124.5(9) . . ? N6 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? C21 C16 C17 121.2(8) . . ? C21 C16 C15 124.2(8) . . ? C17 C16 C15 114.6(8) . . ? C18 C17 C16 120.2(9) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 118.4(10) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C20 C19 C18 122.1(10) . . ? C20 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C19 C20 O8 126.0(9) . . ? C19 C20 C21 122.1(9) . . ? O8 C20 C21 111.9(9) . . ? O7 C21 C16 124.7(9) . . ? O7 C21 C20 119.1(9) . . ? C16 C21 C20 116.0(8) . . ? O8 C22 H22A 109.5 . . ? O8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O9 C23 O10 123.3(10) . . ? O9 C23 C24 119.2(9) . . ? O10 C23 C24 117.6(9) . . ? C25 C24 C29 119.0(9) . . ? C25 C24 C23 120.4(9) . . ? C29 C24 C23 120.6(10) . . ? C26 C25 C24 120.5(11) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 120.5(12) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 119.8(12) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 120.8(11) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C24 119.3(11) . . ? C28 C29 H29 120.3 . . ? C24 C29 H29 120.3 . . ? O11 C30 O12 124.7(9) . . ? O11 C30 C31 118.6(9) . . ? O12 C30 C31 116.5(9) . . ? C32 C31 C36 118.8(10) . . ? C32 C31 C30 121.5(9) . . ? C36 C31 C30 119.7(9) . . ? C31 C32 C33 119.7(10) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 121.5(10) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C35 C34 C33 118.3(11) . . ? C35 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? C36 C35 C34 121.7(11) . . ? C36 C35 H35 119.1 . . ? C34 C35 H35 119.1 . . ? C35 C36 C31 119.8(11) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 O7 . . 2_566 2.651(9) 0.840 1.970 137.6(5) no O1 H1 O8 . . 2_566 2.894(9) 0.840 2.163 145.5(5) no O13 H13B O10 . . . 2.622(19) 0.872 1.779 162 no O14 H14A N5 . . 2_666 2.915(15) 0.889 2.093 153.2(5) no O14 H14B O16 . . . 2.648(16) 0.889 1.839 150.3(6) no O16 H16 O10 . . 1_565 2.85(2) 0.840 2.073 154.0(13) no _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 7.567 _refine_diff_density_min -3.247 _refine_diff_density_rms 0.490 _iucr_refine_instructions_details ; TITL _SST-9-12 CELL 0.71075 12.84500 13.37900 15.04600 74.150 66.720 64.470 ZERR 1 0.00500 0.00600 0.00700 0.020 0.020 0.020 LATT 1 SFAC C H GD N O UNIT 73 76 4 12 29 SHEL 8.147180 0.796452 L.S. 5 FMAP 2 PLAN -25 TEMP -110.0 ACTA BOND $H SIMU 0.01 0.02 1.7 O16 C37 SIZE 0.170 0.060 0.060 WGHT 0.200000 FVAR 0.56957 GD1 3 0.222347 0.277691 0.463235 11.00000 0.02910 0.02805 = 0.03027 -0.00166 -0.00975 -0.01418 GD2 3 0.319130 0.537965 0.337903 11.00000 0.02769 0.02764 = 0.02651 -0.00141 -0.00877 -0.01408 O1 5 -0.283058 0.214655 0.825363 11.00000 0.03783 0.03682 = 0.05118 0.00234 -0.00470 -0.02101 AFIX 147 H1 2 -0.356285 0.257934 0.837827 11.00000 -1.20000 AFIX 0 O2 5 0.089956 0.224650 0.611608 11.00000 0.03236 0.04021 = 0.03949 0.00352 -0.01009 -0.01680 O3 5 0.187557 0.442475 0.357616 11.00000 0.03412 0.03157 = 0.02101 -0.00017 -0.00849 -0.01521 O4 5 0.273328 0.541800 0.185497 11.00000 0.04983 0.05045 = 0.01502 0.00766 -0.00831 -0.03772 O5 5 0.271014 0.170421 0.690543 11.00000 0.04596 0.04019 = 0.03381 0.01272 -0.01260 -0.02484 AFIX 147 H5 2 0.323389 0.105683 0.683467 11.00000 -1.20000 AFIX 0 O6 5 0.318792 0.397782 0.470069 11.00000 0.03020 0.02881 = 0.03570 0.00357 -0.01414 -0.01528 O7 5 0.457339 0.610668 0.228828 11.00000 0.03060 0.03536 = 0.03918 0.00216 -0.01309 -0.01565 O8 5 0.535353 0.702238 0.054105 11.00000 0.03630 0.05841 = 0.03541 0.00619 -0.01215 -0.02362 O9 5 0.181868 0.206769 0.361222 11.00000 0.05525 0.02728 = 0.04944 -0.00817 -0.02564 -0.01066 O10 5 0.285869 0.022254 0.355846 11.00000 0.16120 0.04511 = 0.07795 -0.01044 -0.06701 -0.02675 O11 5 0.412632 0.227755 0.342389 11.00000 0.03570 0.03686 = 0.04287 -0.01042 0.00131 -0.01603 O12 5 0.456024 0.377466 0.257607 11.00000 0.03142 0.02685 = 0.03132 -0.00289 -0.00706 -0.01003 O13 5 0.317072 0.075313 0.496468 11.00000 0.05803 0.03777 = 0.03592 0.00011 -0.01847 -0.01402 AFIX 7 H13A 2 0.274912 0.052079 0.553676 11.00000 -1.50000 H13B 2 0.318543 0.044005 0.451953 11.00000 -1.50000 AFIX 0 O14 5 0.305913 0.645111 0.453327 11.00000 0.03759 0.04002 = 0.03192 -0.00897 -0.00814 -0.01881 AFIX 7 H14A 2 0.378979 0.625982 0.458326 11.00000 -1.50000 H14B 2 0.278558 0.717813 0.433079 11.00000 -1.50000 AFIX 0 N1 4 -0.211700 0.260325 0.740023 11.00000 0.03993 0.03126 = 0.03419 -0.00003 -0.00766 -0.01592 N2 4 -0.085067 0.340470 0.576780 11.00000 0.02752 0.02957 = 0.03646 -0.00309 -0.00960 -0.01853 N3 4 -0.006808 0.377088 0.491751 11.00000 0.03500 0.02811 = 0.03315 -0.00812 -0.00987 -0.01367 N4 4 0.301041 0.242614 0.607339 11.00000 0.02552 0.02844 = 0.03278 0.00153 -0.01149 -0.01329 N5 4 0.503588 0.376090 0.475963 11.00000 0.03938 0.04155 = 0.02649 -0.00255 -0.01276 -0.02227 N6 4 0.509746 0.446329 0.388416 11.00000 0.02988 0.03762 = 0.02552 -0.00162 -0.00521 -0.01975 C1 1 -0.038354 0.114885 0.785891 11.00000 0.04070 0.04618 = 0.08574 0.02600 -0.01784 -0.01226 AFIX 137 H1A 2 -0.088459 0.122118 0.854312 11.00000 -1.20000 H1B 2 0.042618 0.112554 0.776425 11.00000 -1.20000 H1C 2 -0.030622 0.045902 0.768647 11.00000 -1.20000 AFIX 0 C2 1 -0.096401 0.211257 0.723161 11.00000 0.03409 0.03907 = 0.04126 -0.00941 -0.00363 -0.02352 C3 1 -0.025257 0.262948 0.631658 11.00000 0.03668 0.02981 = 0.03062 0.00292 -0.01290 -0.01193 C4 1 -0.058182 0.436660 0.428446 11.00000 0.03359 0.02506 = 0.02977 -0.00777 -0.00670 -0.00639 AFIX 43 H4 2 -0.141600 0.448180 0.444769 11.00000 -1.20000 AFIX 0 C5 1 -0.003255 0.489305 0.333502 11.00000 0.03218 0.03728 = 0.03867 -0.01082 -0.01929 -0.01079 C6 1 -0.073722 0.544097 0.270099 11.00000 0.03571 0.04600 = 0.03321 -0.00464 -0.01548 -0.01435 AFIX 43 H6 2 -0.153972 0.544419 0.290877 11.00000 -1.20000 AFIX 0 C7 1 -0.029581 0.597474 0.178453 11.00000 0.04942 0.05519 = 0.03522 -0.00001 -0.02583 -0.02313 AFIX 43 H7 2 -0.079602 0.634566 0.137833 11.00000 -1.20000 AFIX 0 C8 1 0.086023 0.596336 0.147093 11.00000 0.05069 0.05024 = 0.02526 0.00523 -0.01888 -0.02546 AFIX 43 H8 2 0.117323 0.630966 0.083681 11.00000 -1.20000 AFIX 0 C9 1 0.157652 0.545361 0.206686 11.00000 0.04855 0.03780 = 0.02752 -0.00048 -0.01843 -0.02869 C10 1 0.117515 0.487339 0.302071 11.00000 0.03374 0.03807 = 0.02681 -0.00111 -0.01266 -0.02121 C11 1 0.338364 0.566672 0.085145 11.00000 0.05181 0.07595 = 0.02283 -0.00116 -0.00448 -0.04551 AFIX 137 H11A 2 0.328497 0.527300 0.044578 11.00000 -1.20000 H11B 2 0.424972 0.542440 0.076944 11.00000 -1.20000 H11C 2 0.306066 0.647275 0.065334 11.00000 -1.20000 AFIX 0 C12 1 0.456552 0.233404 0.669951 11.00000 0.03070 0.06083 = 0.03297 0.00291 -0.01929 -0.02461 AFIX 137 H12A 2 0.424447 0.183559 0.724602 11.00000 -1.20000 H12B 2 0.449071 0.297660 0.694588 11.00000 -1.20000 H12C 2 0.542475 0.192988 0.636281 11.00000 -1.20000 AFIX 0 C13 1 0.385391 0.273340 0.599898 11.00000 0.02677 0.03140 = 0.02650 -0.00822 -0.00876 -0.00906 C14 1 0.403442 0.354567 0.512325 11.00000 0.02434 0.03147 = 0.02182 0.00074 -0.01224 -0.01100 C15 1 0.622924 0.434104 0.332554 11.00000 0.03642 0.02834 = 0.03231 -0.00368 -0.00847 -0.01281 AFIX 43 H15 2 0.686508 0.386431 0.359064 11.00000 -1.20000 AFIX 0 C16 1 0.656911 0.489156 0.232462 11.00000 0.03015 0.03719 = 0.02647 0.00628 -0.01154 -0.02091 C17 1 0.783979 0.450273 0.180976 11.00000 0.02544 0.04686 = 0.03654 0.00099 -0.00181 -0.01188 AFIX 43 H17 2 0.838883 0.392425 0.211740 11.00000 -1.20000 AFIX 0 C18 1 0.828322 0.496845 0.085336 11.00000 0.03603 0.04385 = 0.03808 0.00265 -0.01060 -0.01397 AFIX 43 H18 2 0.913002 0.471236 0.050319 11.00000 -1.20000 AFIX 0 C19 1 0.745741 0.581311 0.042815 11.00000 0.03492 0.04441 = 0.03573 -0.00182 -0.00724 -0.02053 AFIX 43 H19 2 0.775131 0.613875 -0.022021 11.00000 -1.20000 AFIX 0 C20 1 0.624010 0.619083 0.090898 11.00000 0.03278 0.03289 = 0.04249 0.00476 -0.02052 -0.01971 C21 1 0.573378 0.575263 0.188976 11.00000 0.02406 0.03399 = 0.03225 -0.00857 -0.00513 -0.00734 C22 1 0.570792 0.759216 -0.040876 11.00000 0.04733 0.08590 = 0.04232 0.01811 -0.01694 -0.03484 AFIX 137 H22A 2 0.615020 0.803461 -0.041105 11.00000 -1.20000 H22B 2 0.498175 0.808743 -0.059523 11.00000 -1.20000 H22C 2 0.623615 0.704726 -0.087484 11.00000 -1.20000 AFIX 0 C23 1 0.224550 0.118826 0.320834 11.00000 0.05166 0.03400 = 0.04596 -0.00704 -0.02701 -0.01564 C24 1 0.201159 0.126493 0.230539 11.00000 0.05321 0.03951 = 0.04177 -0.01094 -0.02294 -0.01864 C25 1 0.115206 0.223271 0.199146 11.00000 0.03919 0.03947 = 0.04177 -0.00654 -0.00830 -0.00984 AFIX 43 H25 2 0.069347 0.283090 0.237781 11.00000 -1.20000 AFIX 0 C26 1 0.096722 0.232271 0.112449 11.00000 0.07062 0.05082 = 0.03885 -0.00793 -0.02157 -0.01214 AFIX 43 H26 2 0.041049 0.299578 0.090321 11.00000 -1.20000 AFIX 0 C27 1 0.158775 0.143870 0.057548 11.00000 0.07187 0.04912 = 0.03994 0.00310 -0.02590 -0.02400 AFIX 43 H27 2 0.145257 0.150335 -0.001804 11.00000 -1.20000 AFIX 0 C28 1 0.239964 0.046760 0.089147 11.00000 0.08265 0.03835 = 0.05318 -0.01157 -0.01868 -0.01558 AFIX 43 H28 2 0.279653 -0.014875 0.052802 11.00000 -1.20000 AFIX 0 C29 1 0.264970 0.037474 0.174297 11.00000 0.07588 0.03817 = 0.04574 -0.01110 -0.03228 -0.01359 AFIX 43 H29 2 0.324520 -0.028427 0.193722 11.00000 -1.20000 AFIX 0 C30 1 0.477742 0.274141 0.273452 11.00000 0.03131 0.03877 = 0.03614 -0.01021 -0.01396 -0.00476 C31 1 0.596312 0.201446 0.207595 11.00000 0.02289 0.03758 = 0.03104 -0.00049 -0.01706 -0.00805 C32 1 0.683751 0.241809 0.148047 11.00000 0.07858 0.03755 = 0.03783 -0.00812 -0.00696 -0.02379 AFIX 43 H32 2 0.673170 0.316588 0.148091 11.00000 -1.20000 AFIX 0 C33 1 0.788958 0.173819 0.086876 11.00000 0.03407 0.04829 = 0.04487 0.00205 -0.00021 -0.01306 AFIX 43 H33 2 0.848933 0.203574 0.043560 11.00000 -1.20000 AFIX 0 C34 1 0.808527 0.065080 0.087340 11.00000 0.05298 0.04931 = 0.04865 -0.02267 0.01283 -0.01435 AFIX 43 H34 2 0.883381 0.017679 0.048356 11.00000 -1.20000 AFIX 0 C35 1 0.718297 0.026391 0.144932 11.00000 0.05228 0.03701 = 0.02600 0.00354 -0.01190 -0.00666 AFIX 43 H35 2 0.727887 -0.047183 0.141805 11.00000 -1.20000 AFIX 0 C36 1 0.615232 0.089720 0.206571 11.00000 0.06809 0.03623 = 0.04054 -0.00749 -0.02104 -0.01121 AFIX 43 H36 2 0.555642 0.059149 0.249117 11.00000 -1.20000 AFIX 0 PART 1 O16 5 0.175116 0.861149 0.457474 10.50000 0.04808 0.03500 = 0.06891 -0.01181 -0.00667 -0.01806 AFIX 147 H16 2 0.223998 0.894735 0.436921 10.50000 -1.50000 AFIX 0 C37 1 0.106197 0.883404 0.541905 10.50000 0.07792 0.05419 = 0.08294 0.01829 0.00559 -0.01297 AFIX 137 H37A 2 0.143241 0.911579 0.570582 10.50000 -1.50000 H37B 2 0.094139 0.815675 0.582320 10.50000 -1.50000 H37C 2 0.027421 0.940328 0.538711 10.50000 -1.50000 PART 0 HKLF 4 REM _SST-9-12 REM R1 = 0.0825 for 7044 Fo > 4sig(Fo) and 0.1041 for all 8715 data REM 551 parameters refined using 6 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 7.567, deepest hole -3.247, 1-sigma level 0.490 Q1 1 0.7668 0.0977 0.2641 11.00000 0.05 3.53 Q2 1 0.8623 0.3546 0.1380 11.00000 0.05 3.29 Q3 1 0.1250 1.0173 0.5897 11.00000 0.05 3.20 Q4 1 0.5821 0.2009 0.7857 11.00000 0.05 2.93 Q5 1 0.3069 -0.0203 0.5700 11.00000 0.05 2.37 Q6 1 0.1946 0.3615 0.4286 11.00000 0.05 2.24 Q7 1 0.2830 0.5496 0.2794 11.00000 0.05 2.24 Q8 1 0.2999 0.6207 0.2970 11.00000 0.05 2.21 Q9 1 0.3211 0.0369 0.3414 11.00000 0.05 2.02 Q10 1 0.2244 0.7729 0.4717 11.00000 0.05 2.00 Q11 1 0.2589 0.2864 0.5228 11.00000 0.05 1.90 Q12 1 0.3419 0.4484 0.3708 11.00000 0.05 1.88 Q13 1 0.2419 0.1904 0.5006 11.00000 0.05 1.86 Q14 1 0.1780 0.2915 0.4087 11.00000 0.05 1.83 Q15 1 0.2557 0.4903 0.3614 11.00000 0.05 1.73 Q16 1 0.1788 0.8218 0.5286 11.00000 0.05 1.67 Q17 1 0.0937 0.9527 0.4592 11.00000 0.05 1.65 Q18 1 0.1387 0.8685 0.4443 11.00000 0.05 1.64 Q19 1 0.0043 0.4907 0.3059 11.00000 0.05 1.64 Q20 1 0.6606 0.1346 0.1814 11.00000 0.05 1.61 Q21 1 0.1959 0.8717 0.4654 11.00000 0.05 1.60 Q22 1 0.3588 0.2354 0.7388 11.00000 0.05 1.58 Q23 1 0.1265 0.9841 0.4674 11.00000 0.05 1.58 Q24 1 0.2121 0.2621 0.3335 11.00000 0.05 1.53 Q25 1 0.5392 0.1646 0.7457 11.00000 0.05 1.52 ;