data_gr51abs _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H73.33 N15 O12.67 Pr' _chemical_formula_weight 1168.11 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pr' 'Pr' -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.486(8) _cell_length_b 14.542(8) _cell_length_c 28.702(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5629(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10764 _cell_measurement_theta_min 3 _cell_measurement_theta_max 36.6 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.462 _exptl_crystal_size_mid 0.281 _exptl_crystal_size_min 0.163 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2437 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Kuma KM4 with a CCD counter' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.3359 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42480 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 36.66 _reflns_number_total 14547 _reflns_number_gt 11000 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+7.4198P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(15) _refine_ls_number_reflns 14547 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Pr Pr 0.21732(2) 0.01878(2) 0.820687(11) 0.02606(8) Uani 1 1 d . . . N1 N 0.1690(4) 0.0556(4) 0.90639(18) 0.0329(12) Uani 1 1 d . . . N2 N 0.0720(3) 0.1445(3) 0.83123(17) 0.0276(11) Uani 1 1 d . . . H2N H 0.0819 0.1878 0.8088 0.033 Uiso 1 1 calc R . . N3 N 0.0360(3) -0.0488(3) 0.83102(16) 0.0280(11) Uani 1 1 d . . . H3 H 0.0169 -0.0638 0.8016 0.034 Uiso 1 1 calc R . . N4 N 0.1954(3) -0.1605(3) 0.82018(19) 0.0289(10) Uani 1 1 d . . . N5 N 0.3316(4) -0.0799(3) 0.76179(17) 0.0279(11) Uani 1 1 d . . . H5N H 0.3883 -0.0474 0.7571 0.034 Uiso 1 1 calc R . . N6 N 0.1644(3) 0.0268(4) 0.73067(15) 0.0265(10) Uani 1 1 d . . . H6 H 0.1081 -0.0070 0.7271 0.032 Uiso 1 1 calc R . . N7 N 0.2626(3) 0.1703(3) 0.77523(17) 0.0273(10) Uani 1 1 d . . . N8 N 0.3738(4) 0.1122(4) 0.84891(18) 0.0343(12) Uani 1 1 d . . . H8 H 0.4232 0.0921 0.8299 0.041 Uiso 1 1 calc R . . N9 N 0.3283(4) -0.0617(4) 0.88848(17) 0.0334(12) Uani 1 1 d . . . H9 H 0.3474 -0.1173 0.8770 0.040 Uiso 1 1 calc R . . C1 C 0.1121(6) 0.0911(5) 0.9967(2) 0.0510(19) Uani 1 1 d . . . H1 H 0.0932 0.1037 1.0272 0.061 Uiso 1 1 calc R . . C2 C 0.0798(5) 0.1478(5) 0.9606(2) 0.0453(17) Uani 1 1 d . . . H2 H 0.0381 0.1974 0.9664 0.054 Uiso 1 1 calc R . . C3 C 0.1109(5) 0.1286(4) 0.9166(2) 0.0318(13) Uani 1 1 d . . . C4 C 0.0861(5) 0.1917(4) 0.8767(2) 0.0348(14) Uani 1 1 d . . . H4A H 0.0259 0.2250 0.8843 0.042 Uiso 1 1 calc R . . H4B H 0.1390 0.2365 0.8734 0.042 Uiso 1 1 calc R . . C5 C -0.0302(4) 0.1066(3) 0.8233(2) 0.0274(11) Uani 1 1 d . . . H5 H -0.0337 0.0926 0.7900 0.033 Uiso 1 1 calc R . . C6 C -0.1152(4) 0.1741(4) 0.8327(2) 0.0378(15) Uani 1 1 d . . . H6A H -0.1145 0.1923 0.8652 0.045 Uiso 1 1 calc R . . H6B H -0.1065 0.2288 0.8138 0.045 Uiso 1 1 calc R . . C7 C -0.2128(4) 0.1297(4) 0.8213(3) 0.0401(13) Uani 1 1 d . . . H7A H -0.2659 0.1730 0.8274 0.048 Uiso 1 1 calc R . . H7B H -0.2143 0.1146 0.7883 0.048 Uiso 1 1 calc R . . C8 C -0.2302(4) 0.0440(4) 0.8491(2) 0.0355(14) Uani 1 1 d . . . H8A H -0.2933 0.0171 0.8404 0.043 Uiso 1 1 calc R . . H8B H -0.2325 0.0591 0.8820 0.043 Uiso 1 1 calc R . . C9 C -0.1465(4) -0.0253(5) 0.8400(2) 0.0339(12) Uani 1 1 d . . . H9A H -0.1553 -0.0779 0.8604 0.041 Uiso 1 1 calc R . . H9B H -0.1511 -0.0470 0.8082 0.041 Uiso 1 1 calc R . . C10 C -0.0441(4) 0.0150(4) 0.84800(18) 0.0270(11) Uani 1 1 d . . . H10 H -0.0350 0.0247 0.8815 0.032 Uiso 1 1 calc R . . C11 C 0.0351(5) -0.1367(4) 0.8563(2) 0.0352(14) Uani 1 1 d . . . H11A H -0.0296 -0.1652 0.8533 0.042 Uiso 1 1 calc R . . H11B H 0.0478 -0.1259 0.8891 0.042 Uiso 1 1 calc R . . C12 C 0.1124(4) -0.1994(4) 0.8370(2) 0.0287(13) Uani 1 1 d . . . C13 C 0.0995(5) -0.2957(4) 0.8358(2) 0.0339(14) Uani 1 1 d . . . H13 H 0.0418 -0.3223 0.8473 0.041 Uiso 1 1 calc R . . C14 C 0.1737(4) -0.3498(4) 0.8173(3) 0.0398(14) Uani 1 1 d . . . H14 H 0.1658 -0.4133 0.8157 0.048 Uiso 1 1 calc R . . C15 C 0.2603(5) -0.3093(4) 0.8010(2) 0.0354(14) Uani 1 1 d . . . H15 H 0.3119 -0.3448 0.7893 0.042 Uiso 1 1 calc R . . C16 C 0.2673(4) -0.2148(4) 0.80261(19) 0.0276(12) Uani 1 1 d . . . C17 C 0.3598(5) -0.1669(4) 0.7852(2) 0.0324(14) Uani 1 1 d . . . H17A H 0.4037 -0.1539 0.8111 0.039 Uiso 1 1 calc R . . H17B H 0.3947 -0.2065 0.7635 0.039 Uiso 1 1 calc R . . C18 C 0.2861(5) -0.0964(4) 0.71528(19) 0.0304(12) Uani 1 1 d . . . H18 H 0.2333 -0.1420 0.7191 0.036 Uiso 1 1 calc R . . C19 C 0.3610(4) -0.1344(4) 0.6799(2) 0.0380(13) Uani 1 1 d . . . H19A H 0.4165 -0.0923 0.6777 0.046 Uiso 1 1 calc R . . H19B H 0.3861 -0.1928 0.6912 0.046 Uiso 1 1 calc R . . C20 C 0.3174(6) -0.1485(5) 0.6315(2) 0.0463(18) Uani 1 1 d . . . H20A H 0.3692 -0.1680 0.6102 0.056 Uiso 1 1 calc R . . H20B H 0.2674 -0.1964 0.6326 0.056 Uiso 1 1 calc R . . C21 C 0.2712(6) -0.0602(5) 0.6139(2) 0.0489(18) Uani 1 1 d . . . H21A H 0.2388 -0.0717 0.5843 0.059 Uiso 1 1 calc R . . H21B H 0.3228 -0.0148 0.6088 0.059 Uiso 1 1 calc R . . C22 C 0.1947(5) -0.0220(5) 0.64892(19) 0.0393(14) Uani 1 1 d . . . H22A H 0.1696 0.0364 0.6376 0.047 Uiso 1 1 calc R . . H22B H 0.1393 -0.0643 0.6511 0.047 Uiso 1 1 calc R . . C23 C 0.2394(4) -0.0084(4) 0.69693(18) 0.0262(12) Uani 1 1 d . . . H23 H 0.2919 0.0379 0.6943 0.031 Uiso 1 1 calc R . . C24 C 0.1405(5) 0.1244(4) 0.7187(2) 0.0312(13) Uani 1 1 d . . . H24A H 0.1309 0.1295 0.6853 0.037 Uiso 1 1 calc R . . H24B H 0.0790 0.1418 0.7338 0.037 Uiso 1 1 calc R . . C25 C 0.2198(5) 0.1882(4) 0.7333(2) 0.0315(12) Uani 1 1 d . . . C26 C 0.2483(5) 0.2624(4) 0.7060(3) 0.0399(16) Uani 1 1 d . . . H26 H 0.2196 0.2720 0.6770 0.048 Uiso 1 1 calc R . . C27 C 0.3199(5) 0.3216(5) 0.7227(3) 0.051(2) Uani 1 1 d . . . H27 H 0.3412 0.3710 0.7046 0.062 Uiso 1 1 calc R . . C28 C 0.3598(5) 0.3070(5) 0.7665(3) 0.0473(18) Uani 1 1 d . . . H28 H 0.4054 0.3483 0.7789 0.057 Uiso 1 1 calc R . . C29 C 0.3312(5) 0.2299(4) 0.7919(2) 0.0353(15) Uani 1 1 d . . . C30 C 0.3685(4) 0.2116(4) 0.8390(2) 0.0388(16) Uani 1 1 d . . . H30A H 0.3251 0.2409 0.8615 0.047 Uiso 1 1 calc R . . H30B H 0.4340 0.2384 0.8423 0.047 Uiso 1 1 calc R . . C31 C 0.4117(4) 0.0909(5) 0.8969(2) 0.0381(16) Uani 1 1 d . . . H31 H 0.3640 0.1132 0.9200 0.046 Uiso 1 1 calc R . . C32 C 0.5132(5) 0.1380(6) 0.9051(3) 0.0515(19) Uani 1 1 d . . . H32A H 0.5574 0.1228 0.8796 0.062 Uiso 1 1 calc R . . H32B H 0.5041 0.2042 0.9053 0.062 Uiso 1 1 calc R . . C33 C 0.5607(6) 0.1090(8) 0.9505(3) 0.071(3) Uani 1 1 d . . . H33A H 0.5224 0.1335 0.9763 0.085 Uiso 1 1 calc R . . H33B H 0.6269 0.1348 0.9523 0.085 Uiso 1 1 calc R . . C34 C 0.5671(5) 0.0050(7) 0.9552(3) 0.067(3) Uani 1 1 d . . . H34A H 0.5925 -0.0110 0.9858 0.081 Uiso 1 1 calc R . . H34B H 0.6121 -0.0195 0.9319 0.081 Uiso 1 1 calc R . . C35 C 0.4639(5) -0.0366(6) 0.9486(3) 0.054(2) Uani 1 1 d . . . H35A H 0.4679 -0.1030 0.9514 0.064 Uiso 1 1 calc R . . H35B H 0.4200 -0.0141 0.9728 0.064 Uiso 1 1 calc R . . C36 C 0.4218(4) -0.0118(6) 0.9014(2) 0.0406(15) Uani 1 1 d . . . H36 H 0.4717 -0.0304 0.8784 0.049 Uiso 1 1 calc R . . C37 C 0.2606(5) -0.0813(4) 0.9275(2) 0.0362(15) Uani 1 1 d . . . H37A H 0.2993 -0.1013 0.9542 0.043 Uiso 1 1 calc R . . H37B H 0.2171 -0.1315 0.9188 0.043 Uiso 1 1 calc R . . C38 C 0.1981(3) 0.0003(4) 0.94168(19) 0.0301(15) Uani 1 1 d . . . C39 C 0.1717(5) 0.0167(6) 0.9873(2) 0.0456(15) Uani 1 1 d . . . H39 H 0.1937 -0.0215 1.0111 0.055 Uiso 1 1 calc R . . N10 N 0.5404(4) 0.0612(4) 0.7617(2) 0.0430(14) Uani 1 1 d . . . O11 O 0.5196(3) 0.0026(3) 0.79202(17) 0.0464(12) Uani 1 1 d . . . O12 O 0.5458(4) 0.1430(3) 0.7713(2) 0.0522(13) Uani 1 1 d . . . O13 O 0.5520(8) 0.0352(5) 0.7208(2) 0.124(4) Uani 1 1 d . . . N20 N 0.9413(4) 0.8802(3) 0.71812(18) 0.0317(11) Uani 1 1 d . . . O21 O 0.9562(3) 0.9646(3) 0.72073(16) 0.0410(11) Uani 1 1 d . . . O22 O 0.8766(4) 0.8507(4) 0.69055(17) 0.0526(13) Uani 1 1 d . . . O23 O 0.9870(4) 0.8269(3) 0.74318(17) 0.0483(12) Uani 1 1 d . . . N30 N 0.1697(7) 0.1794(6) 0.5737(3) 0.072(2) Uani 1 1 d . . . O31 O 0.1105(6) 0.1984(5) 0.6024(2) 0.093(3) Uani 1 1 d . . . O32 O 0.1612(11) 0.1420(8) 0.5402(3) 0.177(6) Uani 1 1 d . . . O33 O 0.2507(13) 0.208(2) 0.5837(7) 0.333(15) Uani 1 1 d . . . N40 N 1.0548(7) 0.8548(6) 0.5619(3) 0.077(2) Uani 1 1 d . . . C41 C 1.0125(8) 0.9184(6) 0.5747(3) 0.065(2) Uani 1 1 d . . . C42 C 0.9589(7) 0.9976(6) 0.5919(3) 0.073(3) Uani 1 1 d . . . H42A H 0.9449 0.9895 0.6245 0.110 Uiso 1 1 calc R . . H42B H 0.8978 1.0039 0.5751 0.110 Uiso 1 1 calc R . . H42C H 0.9985 1.0518 0.5876 0.110 Uiso 1 1 calc R . . N50 N 0.4615(8) 0.4075(8) 0.9087(3) 0.104(3) Uani 1 1 d . . . C51 C 0.3952(7) 0.4387(7) 0.8891(3) 0.067(2) Uani 1 1 d . . . C52 C 0.3125(7) 0.4799(8) 0.8643(3) 0.090(3) Uani 1 1 d . . . H52A H 0.2908 0.5339 0.8806 0.135 Uiso 1 1 calc R . . H52B H 0.2589 0.4366 0.8625 0.135 Uiso 1 1 calc R . . H52C H 0.3331 0.4965 0.8334 0.135 Uiso 1 1 calc R . . N60 N 0.4288(12) 0.7504(7) 0.8890(4) 0.157(7) Uani 1 1 d . . . C61 C 0.4908(12) 0.6997(9) 0.8758(6) 0.122(5) Uani 1 1 d . . . C62 C 0.5644(17) 0.6444(16) 0.8656(10) 0.228(12) Uani 1 1 d . . . O1W O 0.2171(12) 0.3421(9) -0.0583(5) 0.047(3) Uiso 0.33 1 d P . . O2W O 0.2637(8) 0.3251(7) -0.0297(4) 0.023(2) Uiso 0.33 1 d P . . O3W O 0.0737(10) 0.7328(9) 0.9524(5) 0.082(4) Uiso 0.50 1 d P . . O4W O 0.3196(19) 0.2975(17) 0.0005(9) 0.111(8) Uiso 0.33 1 d P . . O5W O 0.0691(18) 0.7793(16) 0.9952(9) 0.160(8) Uiso 0.50 1 d P . . O6W O 0.872(2) 0.962(2) 0.9678(9) 0.116(8) Uiso 0.33 1 d P . . O7W O 0.289(3) 0.482(3) 0.9782(12) 0.172(12) Uiso 0.33 1 d P . . O8W O 0.827(2) 0.9160(18) 0.9913(9) 0.109(8) Uiso 0.33 1 d P . . O9W O 0.260(2) 0.6524(18) 0.9674(9) 0.251(11) Uiso 0.67 1 d P . . 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 Pr 0.02472(11) 0.02539(13) 0.02807(13) 0.00020(14) -0.00135(14) -0.00012(13) N1 0.035(3) 0.031(3) 0.033(3) 0.000(2) -0.006(2) -0.003(2) N2 0.022(2) 0.031(3) 0.030(3) -0.002(2) -0.0006(19) -0.0004(19) N3 0.028(2) 0.026(2) 0.029(3) -0.0039(18) 0.0052(19) -0.0023(18) N4 0.035(2) 0.024(2) 0.028(2) 0.003(2) -0.001(2) -0.0018(17) N5 0.025(2) 0.023(2) 0.036(3) 0.001(2) 0.004(2) -0.005(2) N6 0.025(2) 0.028(2) 0.026(2) 0.001(2) 0.0046(18) 0.002(2) N7 0.016(2) 0.027(2) 0.039(3) -0.002(2) 0.0055(19) 0.0040(17) N8 0.030(3) 0.039(3) 0.033(3) 0.002(2) 0.002(2) 0.004(2) N9 0.036(3) 0.034(3) 0.030(3) -0.005(2) -0.006(2) 0.008(2) C1 0.069(5) 0.060(5) 0.025(3) -0.004(3) 0.008(3) 0.005(4) C2 0.050(4) 0.053(4) 0.032(4) -0.006(3) -0.004(3) 0.006(3) C3 0.035(3) 0.030(3) 0.031(3) -0.005(3) -0.002(3) -0.001(3) C4 0.029(3) 0.037(3) 0.038(3) -0.013(3) -0.005(3) -0.002(3) C5 0.028(2) 0.025(3) 0.029(3) 0.000(3) -0.002(3) -0.003(2) C6 0.033(3) 0.032(3) 0.049(4) -0.006(3) -0.003(3) 0.001(3) C7 0.025(2) 0.031(3) 0.064(4) -0.003(3) -0.006(4) 0.007(2) C8 0.020(3) 0.044(4) 0.042(3) -0.009(3) 0.006(2) -0.004(2) C9 0.028(3) 0.035(3) 0.039(3) -0.005(3) 0.001(2) -0.002(3) C10 0.024(2) 0.031(3) 0.026(3) -0.002(3) 0.002(2) 0.006(3) C11 0.035(3) 0.034(3) 0.037(3) 0.005(3) 0.005(3) -0.004(3) C12 0.025(3) 0.030(3) 0.031(3) 0.004(2) -0.008(2) -0.001(2) C13 0.030(3) 0.026(3) 0.045(4) 0.010(3) 0.000(3) -0.004(2) C14 0.038(3) 0.026(3) 0.055(4) 0.005(3) -0.003(3) -0.002(2) C15 0.037(3) 0.025(3) 0.044(3) 0.006(3) 0.005(3) 0.006(2) C16 0.026(3) 0.029(3) 0.027(3) 0.005(2) 0.002(2) -0.001(2) C17 0.035(3) 0.031(3) 0.031(3) 0.003(3) -0.002(3) 0.005(3) C18 0.039(3) 0.023(3) 0.030(3) 0.003(2) 0.012(3) 0.007(3) C19 0.041(3) 0.035(3) 0.038(3) 0.002(3) 0.013(3) 0.011(3) C20 0.064(5) 0.038(4) 0.037(4) -0.001(3) 0.008(3) 0.011(3) C21 0.069(5) 0.045(4) 0.034(3) 0.006(3) 0.008(4) 0.017(4) C22 0.047(4) 0.046(3) 0.025(3) 0.005(3) -0.002(2) 0.008(3) C23 0.024(2) 0.026(3) 0.029(2) 0.002(2) 0.0052(19) 0.002(2) C24 0.032(3) 0.032(3) 0.030(3) 0.002(3) 0.000(3) 0.004(3) C25 0.030(3) 0.025(3) 0.040(3) 0.006(2) 0.001(3) 0.006(3) C26 0.038(3) 0.029(3) 0.053(4) 0.016(3) -0.002(3) 0.008(3) C27 0.045(4) 0.029(3) 0.080(6) 0.022(4) 0.009(4) 0.003(3) C28 0.037(4) 0.026(3) 0.078(5) 0.002(3) 0.001(4) 0.000(3) C29 0.028(3) 0.032(3) 0.046(4) 0.001(3) 0.003(3) -0.003(3) C30 0.023(3) 0.036(3) 0.058(4) -0.012(3) 0.000(3) -0.008(3) C31 0.024(3) 0.059(4) 0.031(3) -0.011(3) -0.001(3) -0.008(3) C32 0.030(3) 0.079(6) 0.046(4) -0.004(4) 0.000(3) -0.014(4) C33 0.037(4) 0.120(9) 0.057(5) 0.005(5) -0.008(4) -0.035(5) C34 0.031(3) 0.126(9) 0.044(4) 0.023(5) -0.013(3) -0.011(4) C35 0.043(4) 0.066(5) 0.052(4) 0.013(4) -0.013(3) 0.006(4) C36 0.028(3) 0.068(5) 0.026(3) 0.003(3) -0.006(2) 0.000(3) C37 0.043(4) 0.034(3) 0.032(3) 0.004(3) -0.002(3) -0.002(3) C38 0.020(2) 0.041(4) 0.029(3) 0.003(2) -0.005(2) 0.002(2) C39 0.054(4) 0.048(4) 0.034(3) 0.008(3) -0.004(3) 0.010(4) N10 0.030(3) 0.038(3) 0.061(4) -0.012(3) 0.014(3) -0.016(2) O11 0.039(2) 0.038(3) 0.062(3) 0.006(2) 0.008(2) -0.005(2) O12 0.046(3) 0.035(3) 0.076(4) -0.005(3) 0.023(3) -0.005(2) O13 0.228(10) 0.072(5) 0.072(4) -0.024(4) 0.070(6) -0.060(6) N20 0.034(3) 0.027(3) 0.033(3) -0.002(2) 0.005(2) -0.002(2) O21 0.044(2) 0.022(2) 0.057(3) -0.007(2) 0.002(2) 0.0000(18) O22 0.042(3) 0.061(3) 0.055(3) -0.012(3) -0.010(2) -0.016(2) O23 0.054(3) 0.047(3) 0.044(3) 0.002(2) -0.009(2) 0.017(2) N30 0.087(6) 0.084(6) 0.045(4) 0.010(4) 0.005(4) 0.001(5) O31 0.138(7) 0.079(5) 0.062(4) 0.010(3) 0.049(5) 0.045(5) O32 0.286(16) 0.174(10) 0.071(6) -0.057(6) 0.049(8) 0.008(10) O33 0.172(16) 0.60(4) 0.225(19) 0.04(2) -0.005(14) -0.13(2) N40 0.121(7) 0.063(5) 0.048(4) 0.002(4) -0.014(5) -0.020(5) C41 0.100(7) 0.046(5) 0.047(5) 0.002(4) -0.011(5) -0.009(5) C42 0.088(6) 0.067(7) 0.065(5) 0.001(5) -0.009(5) -0.006(5) N50 0.096(7) 0.125(8) 0.090(7) -0.021(6) -0.040(6) 0.020(6) C51 0.056(5) 0.077(6) 0.067(6) -0.014(5) -0.001(5) 0.000(5) C52 0.099(8) 0.090(7) 0.082(6) 0.031(6) -0.006(5) 0.036(6) N60 0.281(17) 0.094(7) 0.097(7) -0.036(6) -0.114(10) 0.114(10) C61 0.137(12) 0.066(8) 0.162(14) 0.027(8) -0.039(11) 0.032(8) C62 0.168(19) 0.17(2) 0.34(3) -0.08(2) 0.14(2) -0.019(16) _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 Pr N1 2.600(6) . yes Pr N4 2.624(4) . yes Pr N7 2.633(5) . yes Pr N8 2.637(5) . yes Pr N3 2.652(5) . yes Pr N6 2.683(5) . yes Pr N2 2.698(5) . yes Pr N5 2.701(5) . yes Pr N9 2.719(5) . yes N1 C3 1.351(8) . no N1 C38 1.351(7) . no N2 C4 1.487(7) . no N2 C5 1.501(7) . no N3 C11 1.470(8) . no N3 C10 1.504(7) . no N4 C12 1.343(7) . no N4 C16 1.348(7) . no N5 C17 1.482(7) . no N5 C18 1.488(8) . no N6 C23 1.491(7) . no N6 C24 1.495(8) . no N7 C29 1.355(8) . no N7 C25 1.360(8) . no N8 C30 1.475(8) . no N8 C31 1.501(8) . no N9 C37 1.473(8) . no N9 C36 1.502(8) . no C1 C39 1.375(10) . no C1 C2 1.394(10) . no C2 C3 1.360(9) . no C3 C4 1.505(9) . no C5 C10 1.520(8) . no C5 C6 1.534(8) . no C6 C7 1.502(8) . no C7 C8 1.498(8) . no C8 C9 1.536(8) . no C9 C10 1.517(8) . no C11 C12 1.492(9) . no C12 C13 1.412(8) . no C13 C14 1.379(9) . no C14 C15 1.389(8) . no C15 C16 1.378(8) . no C16 C17 1.513(8) . no C18 C23 1.521(8) . no C18 C19 1.535(8) . no C19 C20 1.522(10) . no C20 C21 1.513(9) . no C21 C22 1.544(9) . no C22 C23 1.517(8) . no C24 C25 1.476(9) . no C25 C26 1.387(8) . no C26 C27 1.379(10) . no C27 C28 1.386(11) . no C28 C29 1.390(9) . no C29 C30 1.467(10) . no C31 C36 1.505(11) . no C31 C32 1.548(9) . no C32 C33 1.511(11) . no C33 C34 1.521(14) . no C34 C35 1.529(10) . no C35 C36 1.513(9) . no C37 C38 1.511(8) . no C38 C39 1.378(8) . no N10 O12 1.223(7) . no N10 O13 1.243(8) . no N10 O11 1.249(7) . no N20 O23 1.224(7) . no N20 O21 1.246(6) . no N20 O22 1.253(7) . no N30 O32 1.110(11) . no N30 O31 1.179(10) . no N30 O33 1.204(17) . no N40 C41 1.147(12) . no C41 C42 1.447(13) . no N50 C51 1.149(12) . no C51 C52 1.452(13) . no N60 C61 1.178(19) . no C61 C62 1.31(2) . no O7W O8W 1.80(4) 4_467 no O8W O9W 1.79(4) 4_567 no O8W O7W 1.80(4) 4_567 no O9W O8W 1.79(4) 4_467 no 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 N1 Pr N4 100.47(17) . . no N1 Pr N7 110.76(16) . . no N4 Pr N7 148.77(16) . . no N1 Pr N8 78.69(16) . . no N4 Pr N8 127.14(15) . . no N7 Pr N8 62.32(15) . . no N1 Pr N3 74.89(15) . . no N4 Pr N3 61.89(14) . . no N7 Pr N3 125.39(14) . . no N8 Pr N3 153.42(15) . . no N1 Pr N6 146.64(15) . . no N4 Pr N6 90.45(16) . . no N7 Pr N6 63.14(15) . . no N8 Pr N6 119.10(16) . . no N3 Pr N6 83.01(14) . . no N1 Pr N2 64.67(15) . . no N4 Pr N2 126.32(14) . . no N7 Pr N2 69.92(14) . . no N8 Pr N2 101.40(15) . . no N3 Pr N2 64.43(14) . . no N6 Pr N2 83.40(14) . . no N1 Pr N5 147.63(16) . . no N4 Pr N5 62.14(15) . . no N7 Pr N5 90.14(14) . . no N8 Pr N5 90.54(16) . . no N3 Pr N5 113.54(14) . . no N6 Pr N5 64.68(14) . . no N2 Pr N5 147.69(15) . . no N1 Pr N9 63.24(16) . . no N4 Pr N9 68.78(16) . . no N7 Pr N9 125.97(15) . . no N8 Pr N9 64.02(16) . . no N3 Pr N9 105.54(15) . . no N6 Pr N9 148.66(15) . . no N2 Pr N9 127.69(15) . . no N5 Pr N9 84.55(15) . . no C3 N1 C38 118.3(5) . . no C3 N1 Pr 120.8(4) . . no C38 N1 Pr 120.9(4) . . no C4 N2 C5 114.8(5) . . no C4 N2 Pr 108.5(3) . . no C5 N2 Pr 113.6(3) . . no C11 N3 C10 111.8(4) . . no C11 N3 Pr 112.6(3) . . no C10 N3 Pr 118.0(3) . . no C12 N4 C16 119.2(5) . . no C12 N4 Pr 120.6(4) . . no C16 N4 Pr 120.2(3) . . no C17 N5 C18 112.0(4) . . no C17 N5 Pr 108.4(3) . . no C18 N5 Pr 114.3(3) . . no C23 N6 C24 108.8(4) . . no C23 N6 Pr 115.5(3) . . no C24 N6 Pr 108.6(3) . . no C29 N7 C25 118.7(5) . . no C29 N7 Pr 121.3(4) . . no C25 N7 Pr 120.0(4) . . no C30 N8 C31 113.3(5) . . no C30 N8 Pr 114.0(4) . . no C31 N8 Pr 116.6(4) . . no C37 N9 C36 115.2(5) . . no C37 N9 Pr 106.7(4) . . no C36 N9 Pr 115.5(4) . . no C39 C1 C2 120.1(6) . . no C3 C2 C1 118.2(7) . . no N1 C3 C2 122.8(6) . . no N1 C3 C4 116.3(5) . . no C2 C3 C4 120.8(6) . . no N2 C4 C3 114.5(5) . . no N2 C5 C10 111.4(4) . . no N2 C5 C6 115.1(4) . . no C10 C5 C6 112.7(5) . . no C7 C6 C5 110.0(5) . . no C8 C7 C6 112.2(5) . . no C7 C8 C9 109.9(5) . . no C10 C9 C8 112.9(5) . . no N3 C10 C9 111.5(5) . . no N3 C10 C5 107.5(4) . . no C9 C10 C5 112.4(5) . . no N3 C11 C12 110.1(5) . . no N4 C12 C13 120.8(5) . . no N4 C12 C11 117.3(5) . . no C13 C12 C11 121.9(5) . . no C14 C13 C12 119.0(5) . . no C13 C14 C15 119.8(5) . . no C16 C15 C14 118.0(5) . . no N4 C16 C15 123.1(5) . . no N4 C16 C17 116.6(5) . . no C15 C16 C17 120.3(5) . . no N5 C17 C16 109.3(5) . . no N5 C18 C23 110.3(4) . . no N5 C18 C19 112.4(6) . . no C23 C18 C19 110.3(5) . . no C20 C19 C18 113.5(6) . . no C21 C20 C19 110.5(6) . . no C20 C21 C22 111.3(6) . . no C23 C22 C21 111.9(5) . . no N6 C23 C22 111.4(4) . . no N6 C23 C18 110.2(4) . . no C22 C23 C18 111.7(5) . . no C25 C24 N6 112.0(5) . . no N7 C25 C26 122.0(6) . . no N7 C25 C24 116.0(5) . . no C26 C25 C24 122.0(6) . . no C27 C26 C25 119.0(7) . . no C26 C27 C28 119.4(6) . . no C27 C28 C29 119.4(7) . . no N7 C29 C28 121.4(6) . . no N7 C29 C30 116.3(6) . . no C28 C29 C30 122.2(6) . . no C29 C30 N8 111.9(5) . . no N8 C31 C36 108.3(5) . . no N8 C31 C32 110.5(5) . . no C36 C31 C32 110.2(6) . . no C33 C32 C31 112.5(6) . . no C32 C33 C34 112.2(7) . . no C33 C34 C35 109.3(7) . . no C36 C35 C34 111.0(6) . . no N9 C36 C31 112.5(5) . . no N9 C36 C35 114.9(6) . . no C31 C36 C35 110.3(6) . . no N9 C37 C38 113.4(5) . . no N1 C38 C39 122.3(6) . . no N1 C38 C37 115.3(5) . . no C39 C38 C37 122.4(5) . . no C1 C39 C38 118.3(6) . . no O12 N10 O13 120.0(7) . . no O12 N10 O11 121.3(6) . . no O13 N10 O11 118.6(6) . . no O23 N20 O21 120.4(5) . . no O23 N20 O22 120.4(5) . . no O21 N20 O22 119.1(5) . . no O32 N30 O31 130.5(13) . . no O32 N30 O33 117.9(15) . . no O31 N30 O33 111.6(14) . . no N40 C41 C42 178.7(10) . . no N50 C51 C52 178.8(12) . . no N60 C61 C62 174(2) . . no O9W O8W O7W 89.8(18) 4_567 4_567 no _diffrn_measured_fraction_theta_max 0.556 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.814 _refine_diff_density_min -1.689 _refine_diff_density_rms 0.110