# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr V. Pedireddi' _publ_contact_author_address ; Division of Organic Chemistry National Chemical Laboratory Dr. Homi Bhabha Road Pune Maharashtra State 411 008 INDIA ; _publ_contact_author_email PEDIREDI@EMS.NCL.RES.IN _publ_section_title ; Hydrogen Bond Mediated Open-frame Networks in Coordination Polymers: Supramolecular Assemblies of Pr(III) and 3,5-Dinitro-4-methylbenzoic Acid with Aza-donor Compounds ; loop_ _publ_author_name 'V. Pedireddi' 'Sunil Varughese' data_1 _database_code_depnum_ccdc_archive 'CCDC 233738' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Pentaacqua-tris-(3,5-dinitro-4-methylbenzoato)praseodymium(III) complex ; _chemical_name_common ;Pentaacqua-tris-(3,5-dinitro-4- methylbenzoato)praseodymium(iii) complex ; _chemical_melting_point ? _chemical_formula_moiety '[Pr(C8H5N2O6)3(H2O)2].3(H2O)' _chemical_formula_sum 'C24 H25 N6 O23 Pr' _chemical_formula_weight 906.41 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.483(3) _cell_length_b 12.593(3) _cell_length_c 15.517(4) _cell_angle_alpha 76.89(9) _cell_angle_beta 78.10(9) _cell_angle_gamma 81.33(9) _cell_volume 1755.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 1.488 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 CCD-Area detector' _diffrn_measurement_method SMART _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14587 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.25 _reflns_number_total 5034 _reflns_number_gt 4903 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINTPLUS _computing_structure_solution 'SHELXTL (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL (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^)+(0.1127P)^2^+20.7032P] 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 5034 _refine_ls_number_parameters 500 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1889 _refine_ls_wR_factor_gt 0.1884 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.27660(4) 0.53032(3) 0.50730(3) 0.0170(2) Uani 1 1 d . . . C11 C 0.4478(9) 0.3736(7) 0.7836(6) 0.0220(19) Uani 1 1 d . . . C12 C 0.5692(10) 0.3119(7) 0.8135(6) 0.025(2) Uani 1 1 d . . . H12A H 0.6588 0.3131 0.7754 0.030 Uiso 1 1 calc R . . C13 C 0.5573(11) 0.2494(8) 0.8986(7) 0.029(2) Uani 1 1 d . . . C14 C 0.4294(11) 0.2438(8) 0.9613(6) 0.031(2) Uani 1 1 d . . . C15 C 0.3113(11) 0.3104(9) 0.9291(7) 0.035(2) Uani 1 1 d . . . C16 C 0.3170(11) 0.3714(8) 0.8426(7) 0.031(2) Uani 1 1 d . . . H16A H 0.2334 0.4107 0.8243 0.037 Uiso 1 1 calc R . . C17 C 0.4599(9) 0.4364(7) 0.6879(6) 0.0217(19) Uani 1 1 d . . . C18 C 0.4174(14) 0.1679(10) 1.0531(8) 0.050(3) Uani 1 1 d . . . H18A H 0.5113 0.1307 1.0612 0.075 Uiso 1 1 calc R . . H18B H 0.3521 0.1150 1.0571 0.075 Uiso 1 1 calc R . . H18C H 0.3813 0.2101 1.0989 0.075 Uiso 1 1 calc R . . O23A O 0.9233(7) 0.8251(5) 0.5406(5) 0.0370(17) Uani 1 1 d . . . O23B O 0.8480(7) 0.9917(5) 0.5540(4) 0.0261(14) Uani 1 1 d . . . O25A O 0.6149(8) 1.1071(6) 0.2289(5) 0.0412(18) Uani 1 1 d . . . O25B O 0.4176(8) 1.1407(6) 0.3189(5) 0.0431(19) Uani 1 1 d . . . O27A O 0.3345(6) 0.7296(5) 0.4634(4) 0.0252(14) Uani 1 1 d . . . C21 C 0.5475(9) 0.8145(7) 0.4502(6) 0.0180(18) Uani 1 1 d . . . C22 C 0.6633(9) 0.8162(7) 0.4910(6) 0.0195(18) Uani 1 1 d . . . H22A H 0.6958 0.7542 0.5303 0.023 Uiso 1 1 calc R . . C23 C 0.7304(9) 0.9107(7) 0.4728(6) 0.0186(18) Uani 1 1 d . . . C24 C 0.6966(9) 1.0046(7) 0.4102(6) 0.0193(18) Uani 1 1 d . . . C25 C 0.5796(9) 0.9959(7) 0.3700(6) 0.0193(18) Uani 1 1 d . . . C26 C 0.5025(9) 0.9069(7) 0.3911(6) 0.0188(18) Uani 1 1 d . . . H26A H 0.4209 0.9088 0.3660 0.023 Uiso 1 1 calc R . . C27 C 0.4645(9) 0.7154(7) 0.4727(5) 0.0179(18) Uani 1 1 d . . . C28 C 0.7764(10) 1.1048(7) 0.3861(6) 0.024(2) Uani 1 1 d . . . H28A H 0.8790 1.0829 0.3773 0.037 Uiso 1 1 calc R . . H28B H 0.7498 1.1447 0.4340 0.037 Uiso 1 1 calc R . . H28C H 0.7514 1.1507 0.3318 0.037 Uiso 1 1 calc R . . C31 C 0.0261(9) 0.2341(7) 0.6722(6) 0.0189(18) Uani 1 1 d . . . C32 C 0.1324(9) 0.2119(7) 0.7251(6) 0.0211(19) Uani 1 1 d . . . H32A H 0.2008 0.2606 0.7169 0.025 Uiso 1 1 calc R . . C33 C 0.1360(9) 0.1170(7) 0.7898(6) 0.0207(18) Uani 1 1 d . . . C34 C 0.0420(9) 0.0369(7) 0.8047(6) 0.0222(19) Uani 1 1 d . . . C35 C -0.0604(9) 0.0639(7) 0.7483(6) 0.0202(18) Uani 1 1 d . . . C36 C -0.0724(9) 0.1584(7) 0.6844(6) 0.0195(18) Uani 1 1 d . . . H36A H -0.1450 0.1715 0.6499 0.023 Uiso 1 1 calc R . . C37 C 0.0190(9) 0.3394(7) 0.6036(6) 0.0188(18) Uani 1 1 d . . . C38 C 0.0457(11) -0.0648(8) 0.8779(6) 0.028(2) Uani 1 1 d . . . H38A H 0.0360 -0.1271 0.8545 0.042 Uiso 1 1 calc R . . H38B H -0.0328 -0.0563 0.9269 0.042 Uiso 1 1 calc R . . H38C H 0.1361 -0.0756 0.8990 0.042 Uiso 1 1 calc R . . O33A O 0.2114(10) 0.0812(9) 0.9272(5) 0.065(3) Uani 1 1 d . . . O33B O 0.3712(7) 0.1222(6) 0.8075(5) 0.0355(16) Uani 1 1 d . . . O35A O -0.1279(8) -0.1110(5) 0.7582(5) 0.0369(17) Uani 1 1 d . . . O35B O -0.2960(7) 0.0263(6) 0.7604(5) 0.0334(16) Uani 1 1 d . . . O37A O 0.1167(7) 0.3994(5) 0.5932(4) 0.0267(14) Uani 1 1 d . . . N13 N 0.6935(13) 0.1829(9) 0.9189(8) 0.063(3) Uani 1 1 d . . . N15 N 0.1714(13) 0.3116(11) 0.9884(8) 0.070(4) Uani 1 1 d . . . N23 N 0.8429(8) 0.9097(6) 0.5261(5) 0.0213(16) Uani 1 1 d . . . N25 N 0.5354(8) 1.0887(6) 0.3004(5) 0.0212(16) Uani 1 1 d . . . N33 N 0.2480(9) 0.1044(7) 0.8456(5) 0.0307(19) Uani 1 1 d . . . N35 N -0.1696(8) -0.0137(6) 0.7567(5) 0.0255(17) Uani 1 1 d . . . O91 O 0.1928(7) 0.4261(5) 0.4025(5) 0.0299(15) Uani 1 1 d . . . O92 O 0.0822(7) 0.6418(5) 0.4402(4) 0.0258(14) Uani 1 1 d . . . O93 O 0.4132(6) 0.5597(5) 0.3556(4) 0.0244(14) Uani 1 1 d . . . O94 O 0.1021(8) 0.6351(5) 0.6168(5) 0.0346(16) Uani 1 1 d . . . O94A O 0.4718(6) 0.3782(5) 0.5002(4) 0.0214(13) Uani 1 1 d . . . O13A O 0.6927(16) 0.0854(10) 0.9453(9) 0.101(4) Uani 1 1 d . . . O13B O 0.8045(12) 0.2166(12) 0.8909(8) 0.091(4) Uani 1 1 d . . . O15A O 0.1549(12) 0.3085(10) 1.0637(6) 0.082(3) Uani 1 1 d . . . O15B O 0.0620(13) 0.3054(14) 0.9545(9) 0.113(5) Uani 1 1 d . . . O17A O 0.3452(7) 0.4766(5) 0.6593(4) 0.0270(14) Uani 1 1 d . . . O103 O 0.8575(14) 0.4548(11) 0.7875(10) 0.104(4) Uani 1 1 d . . . O101 O 0.0757(14) 0.6245(14) 0.7942(8) 0.117(5) Uani 1 1 d . . . O104 O 0.405(3) 0.3621(16) 1.1987(11) 0.072(9) Uani 0.45(2) 1 d P . . O105 O 0.638(3) 0.3527(17) 1.1726(16) 0.112(11) Uani 0.55(2) 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 Pr1 0.0133(3) 0.0163(3) 0.0212(3) 0.0002(2) -0.0046(2) -0.00466(19) C11 0.021(5) 0.023(5) 0.026(5) -0.008(4) -0.007(4) -0.007(4) C12 0.023(5) 0.023(5) 0.027(5) -0.005(4) -0.004(4) -0.003(4) C13 0.030(5) 0.024(5) 0.035(5) -0.005(4) -0.015(4) -0.001(4) C14 0.042(6) 0.031(5) 0.022(5) 0.002(4) -0.011(4) -0.015(5) C15 0.029(5) 0.050(7) 0.023(5) -0.004(5) 0.002(4) -0.009(5) C16 0.024(5) 0.036(6) 0.032(5) -0.007(4) -0.006(4) 0.000(4) C17 0.023(5) 0.021(5) 0.024(5) -0.007(4) -0.005(4) -0.007(4) C18 0.062(8) 0.054(7) 0.033(6) 0.009(5) -0.019(6) -0.013(6) O23A 0.029(4) 0.026(4) 0.064(5) -0.012(3) -0.026(3) 0.003(3) O23B 0.029(3) 0.023(3) 0.031(3) -0.008(3) -0.009(3) -0.008(3) O25A 0.043(4) 0.045(4) 0.027(4) 0.004(3) -0.003(3) 0.002(3) O25B 0.042(5) 0.036(4) 0.039(4) 0.003(3) -0.002(3) 0.012(4) O27A 0.017(3) 0.019(3) 0.040(4) -0.005(3) -0.006(3) -0.005(2) C21 0.014(4) 0.018(4) 0.023(4) -0.008(4) -0.003(3) -0.001(3) C22 0.017(4) 0.017(4) 0.024(5) -0.003(3) -0.004(3) 0.001(3) C23 0.014(4) 0.019(4) 0.024(5) -0.009(4) -0.003(3) -0.002(3) C24 0.018(4) 0.019(4) 0.022(4) -0.008(4) -0.002(4) -0.003(3) C25 0.019(4) 0.018(4) 0.020(4) -0.006(3) -0.001(3) -0.001(3) C26 0.016(4) 0.020(4) 0.023(4) -0.007(4) -0.003(3) -0.004(3) C27 0.019(5) 0.016(5) 0.019(4) -0.004(3) 0.000(3) -0.005(3) C28 0.022(5) 0.022(5) 0.030(5) -0.004(4) -0.005(4) -0.009(4) C31 0.018(4) 0.019(4) 0.021(4) -0.006(3) -0.003(3) -0.002(3) C32 0.016(4) 0.025(5) 0.023(5) -0.006(4) -0.003(4) -0.006(4) C33 0.018(4) 0.028(5) 0.018(4) -0.005(4) -0.008(3) 0.000(4) C34 0.021(5) 0.023(5) 0.022(5) -0.005(4) -0.001(4) -0.003(4) C35 0.019(4) 0.020(4) 0.021(4) -0.003(4) -0.001(4) -0.005(4) C36 0.015(4) 0.021(4) 0.023(4) -0.006(4) -0.003(3) -0.002(3) C37 0.014(4) 0.020(4) 0.022(4) -0.004(4) -0.001(4) -0.003(4) C38 0.031(5) 0.026(5) 0.026(5) 0.004(4) -0.011(4) -0.005(4) O33A 0.058(6) 0.118(8) 0.024(4) 0.011(5) -0.019(4) -0.044(6) O33B 0.022(4) 0.047(4) 0.043(4) -0.014(3) -0.013(3) -0.006(3) O35A 0.045(4) 0.021(4) 0.044(4) 0.000(3) -0.010(3) -0.011(3) O35B 0.021(4) 0.039(4) 0.040(4) 0.001(3) -0.011(3) -0.011(3) O37A 0.024(3) 0.027(3) 0.030(3) 0.003(3) -0.009(3) -0.015(3) N13 0.053(7) 0.046(7) 0.080(8) 0.032(6) -0.036(6) -0.016(5) N15 0.047(7) 0.098(10) 0.045(7) 0.011(6) 0.002(5) 0.004(6) N23 0.019(4) 0.020(4) 0.026(4) -0.003(3) -0.007(3) -0.004(3) N25 0.026(4) 0.018(4) 0.021(4) -0.001(3) -0.005(3) -0.008(3) N33 0.028(5) 0.036(5) 0.028(5) 0.002(4) -0.012(4) -0.005(4) N35 0.029(5) 0.025(5) 0.022(4) 0.004(3) -0.007(3) -0.013(4) O91 0.025(3) 0.024(3) 0.045(4) -0.007(3) -0.015(3) -0.006(3) O92 0.022(3) 0.019(3) 0.036(4) 0.002(3) -0.015(3) -0.003(2) O93 0.020(3) 0.032(4) 0.022(3) -0.003(3) -0.003(3) -0.009(3) O94 0.039(4) 0.028(4) 0.033(4) -0.005(3) -0.002(3) 0.003(3) O94A 0.023(3) 0.016(3) 0.026(3) -0.001(2) -0.007(3) -0.005(3) O13A 0.127(11) 0.060(8) 0.115(10) -0.006(7) -0.058(9) 0.022(7) O13B 0.049(6) 0.141(11) 0.078(8) -0.030(7) -0.022(6) 0.034(7) O15A 0.078(7) 0.105(8) 0.037(6) -0.006(5) 0.027(5) 0.006(6) O15B 0.049(7) 0.193(16) 0.094(9) -0.037(10) 0.006(6) -0.023(8) O17A 0.021(3) 0.035(4) 0.024(3) 0.000(3) -0.009(3) -0.005(3) O103 0.088(9) 0.083(8) 0.134(12) -0.005(8) -0.014(8) -0.020(7) O101 0.092(9) 0.199(16) 0.063(7) -0.069(9) -0.010(6) 0.034(10) O104 0.16(2) 0.054(13) 0.018(9) 0.020(8) -0.042(11) -0.050(14) O105 0.13(2) 0.082(15) 0.13(2) -0.094(15) 0.066(16) -0.056(14) _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 Pr1 O37A 2.391(6) . ? Pr1 O92 2.408(6) . ? Pr1 O93 2.418(6) . ? Pr1 O94A 2.460(6) . ? Pr1 O17A 2.495(6) . ? Pr1 O27A 2.559(6) . ? Pr1 O94 2.563(7) . ? Pr1 O91 2.610(6) . ? Pr1 O94A 2.772(6) 2_666 ? Pr1 C27 3.031(8) . ? C11 C16 1.382(13) . ? C11 C12 1.389(13) . ? C11 C17 1.506(13) . ? C12 C13 1.369(14) . ? C13 C14 1.390(14) . ? C13 N13 1.480(15) . ? C14 C15 1.402(15) . ? C14 C18 1.517(14) . ? C15 C16 1.381(14) . ? C15 N15 1.451(15) . ? C17 O17A 1.252(11) . ? C17 O93 1.254(11) 2_666 ? O23A N23 1.218(10) . ? O23B N23 1.218(9) . ? O25A N25 1.201(10) . ? O25B N25 1.221(10) . ? O27A C27 1.252(10) . ? C21 C26 1.380(12) . ? C21 C22 1.381(12) . ? C21 C27 1.511(12) . ? C22 C23 1.379(12) . ? C23 C24 1.393(12) . ? C23 N23 1.476(11) . ? C24 C25 1.409(12) . ? C24 C28 1.504(12) . ? C25 C26 1.371(12) . ? C25 N25 1.474(11) . ? C27 O94A 1.264(10) 2_666 ? C31 C32 1.385(12) . ? C31 C36 1.389(12) . ? C31 C37 1.503(12) . ? C32 C33 1.376(13) . ? C33 C34 1.396(13) . ? C33 N33 1.472(12) . ? C34 C35 1.394(13) . ? C34 C38 1.507(12) . ? C35 C36 1.372(12) . ? C35 N35 1.495(11) . ? C37 O37A 1.245(10) . ? C37 O92 1.252(11) 2_566 ? O33A N33 1.220(11) . ? O33B N33 1.224(11) . ? O35A N35 1.226(10) . ? O35B N35 1.224(10) . ? N13 O13B 1.157(16) . ? N13 O13A 1.203(15) . ? N15 O15A 1.139(15) . ? N15 O15B 1.275(17) . ? O92 C37 1.252(11) 2_566 ? O93 C17 1.254(11) 2_666 ? O94A C27 1.264(10) 2_666 ? O94A Pr1 2.772(6) 2_666 ? 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 O37A Pr1 O92 91.4(2) . . ? O37A Pr1 O93 134.3(2) . . ? O92 Pr1 O93 84.8(2) . . ? O37A Pr1 O94A 88.2(2) . . ? O92 Pr1 O94A 147.6(2) . . ? O93 Pr1 O94A 72.7(2) . . ? O37A Pr1 O17A 74.2(2) . . ? O92 Pr1 O17A 137.2(2) . . ? O93 Pr1 O17A 133.9(2) . . ? O94A Pr1 O17A 73.5(2) . . ? O37A Pr1 O27A 148.4(2) . . ? O92 Pr1 O27A 71.4(2) . . ? O93 Pr1 O27A 71.9(2) . . ? O94A Pr1 O27A 120.70(19) . . ? O17A Pr1 O27A 100.3(2) . . ? O37A Pr1 O94 76.0(2) . . ? O92 Pr1 O94 67.5(2) . . ? O93 Pr1 O94 140.7(2) . . ? O94A Pr1 O94 142.8(2) . . ? O17A Pr1 O94 69.8(2) . . ? O27A Pr1 O94 73.0(2) . . ? O37A Pr1 O91 69.4(2) . . ? O92 Pr1 O91 70.6(2) . . ? O93 Pr1 O91 66.4(2) . . ? O94A Pr1 O91 79.0(2) . . ? O17A Pr1 O91 134.6(2) . . ? O27A Pr1 O91 125.0(2) . . ? O94 Pr1 O91 123.9(2) . . ? O37A Pr1 O94A 145.19(19) . 2_666 ? O92 Pr1 O94A 119.17(19) . 2_666 ? O93 Pr1 O94A 69.63(19) . 2_666 ? O94A Pr1 O94A 74.9(2) . 2_666 ? O17A Pr1 O94A 71.90(19) . 2_666 ? O27A Pr1 O94A 48.69(18) . 2_666 ? O94 Pr1 O94A 99.3(2) . 2_666 ? O91 Pr1 O94A 133.70(19) . 2_666 ? O37A Pr1 C27 157.0(2) . . ? O92 Pr1 C27 94.9(2) . . ? O93 Pr1 C27 68.4(2) . . ? O94A Pr1 C27 98.0(2) . . ? O17A Pr1 C27 86.3(2) . . ? O27A Pr1 C27 24.0(2) . . ? O94 Pr1 C27 86.1(2) . . ? O91 Pr1 C27 133.5(2) . . ? O94A Pr1 C27 24.7(2) 2_666 . ? C16 C11 C12 118.2(9) . . ? C16 C11 C17 121.8(8) . . ? C12 C11 C17 119.9(8) . . ? C13 C12 C11 120.3(9) . . ? C12 C13 C14 124.4(9) . . ? C12 C13 N13 114.1(9) . . ? C14 C13 N13 121.5(9) . . ? C13 C14 C15 113.1(8) . . ? C13 C14 C18 123.1(10) . . ? C15 C14 C18 123.6(10) . . ? C16 C15 C14 124.4(9) . . ? C16 C15 N15 117.2(10) . . ? C14 C15 N15 118.3(9) . . ? C15 C16 C11 119.4(9) . . ? O17A C17 O93 126.9(8) . 2_666 ? O17A C17 C11 118.0(8) . . ? O93 C17 C11 115.1(8) 2_666 . ? C27 O27A Pr1 99.6(5) . . ? C26 C21 C22 119.3(8) . . ? C26 C21 C27 119.4(7) . . ? C22 C21 C27 121.2(8) . . ? C23 C22 C21 119.3(8) . . ? C22 C23 C24 124.4(8) . . ? C22 C23 N23 116.0(7) . . ? C24 C23 N23 119.6(7) . . ? C23 C24 C25 112.8(8) . . ? C23 C24 C28 124.3(8) . . ? C25 C24 C28 122.9(8) . . ? C26 C25 C24 124.6(8) . . ? C26 C25 N25 117.0(7) . . ? C24 C25 N25 118.3(7) . . ? C25 C26 C21 119.1(8) . . ? O27A C27 O94A 122.5(7) . 2_666 ? O27A C27 C21 118.3(7) . . ? O94A C27 C21 119.2(7) 2_666 . ? O27A C27 Pr1 56.4(4) . . ? O94A C27 Pr1 66.2(4) 2_666 . ? C21 C27 Pr1 174.4(6) . . ? C32 C31 C36 119.0(8) . . ? C32 C31 C37 119.6(8) . . ? C36 C31 C37 121.5(8) . . ? C33 C32 C31 119.5(8) . . ? C32 C33 C34 124.4(8) . . ? C32 C33 N33 115.1(8) . . ? C34 C33 N33 120.5(8) . . ? C35 C34 C33 112.9(8) . . ? C35 C34 C38 123.7(8) . . ? C33 C34 C38 123.3(8) . . ? C36 C35 C34 125.5(8) . . ? C36 C35 N35 115.4(7) . . ? C34 C35 N35 119.1(7) . . ? C35 C36 C31 118.7(8) . . ? O37A C37 O92 125.3(8) . 2_566 ? O37A C37 C31 117.2(7) . . ? O92 C37 C31 117.5(7) 2_566 . ? C37 O37A Pr1 153.9(6) . . ? O13B N13 O13A 117.9(14) . . ? O13B N13 C13 121.0(11) . . ? O13A N13 C13 118.6(11) . . ? O15A N15 O15B 118.4(13) . . ? O15A N15 C15 124.5(13) . . ? O15B N15 C15 116.8(12) . . ? O23A N23 O23B 124.3(7) . . ? O23A N23 C23 117.2(7) . . ? O23B N23 C23 118.5(7) . . ? O25A N25 O25B 124.1(8) . . ? O25A N25 C25 118.6(7) . . ? O25B N25 C25 117.3(7) . . ? O33A N33 O33B 123.8(8) . . ? O33A N33 C33 118.1(8) . . ? O33B N33 C33 118.0(8) . . ? O35B N35 O35A 124.6(8) . . ? O35B N35 C35 116.4(7) . . ? O35A N35 C35 119.0(8) . . ? C37 O92 Pr1 155.0(6) 2_566 . ? C17 O93 Pr1 142.2(6) 2_666 . ? C27 O94A Pr1 155.1(5) 2_666 . ? C27 O94A Pr1 89.2(5) 2_666 2_666 ? Pr1 O94A Pr1 105.1(2) . 2_666 ? C17 O17A Pr1 134.4(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.580 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.228 data_2 _database_code_depnum_ccdc_archive 'CCDC 233739' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bisacqua-mono-(4,4'-bipyridyl)-tris-(3,5-dinitro-4-methylbenzoato) Praseodymium(III) complex ; _chemical_name_common ; Bisacqua-mono-(4,4'-bipyridyl)-tris-(3,5-dinitro-4- methylbenzoato) Praseodymium(iii) complex ; _chemical_melting_point ? _chemical_formula_moiety '[Pr(C8H5N2O6)3(H2O)2].(C10H8N2)' _chemical_formula_sum 'C34 H27 N8 O20 Pr' _chemical_formula_weight 1008.55 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.774(4) _cell_length_b 12.721(6) _cell_length_c 16.355(7) _cell_angle_alpha 72.01(9) _cell_angle_beta 82.90(9) _cell_angle_gamma 83.15(9) _cell_volume 1912.2(18) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 1.372 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 CCD-Area detector' _diffrn_measurement_method SMART _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16061 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 23.30 _reflns_number_total 5502 _reflns_number_gt 5183 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINTPLUS _computing_structure_solution 'SHELXTL (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL (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^)+(0.0472P)^2^+0.4468P] 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 5502 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 Pr1 Pr 0.281721(15) 0.527499(12) 0.504114(10) 0.02347(8) Uani 1 1 d . . . C11 C 0.5263(3) 0.6625(3) 0.2282(2) 0.0342(8) Uani 1 1 d . . . C12 C 0.4114(4) 0.7140(3) 0.1871(2) 0.0432(9) Uani 1 1 d . . . H12 H 0.333(4) 0.707(3) 0.213(3) 0.062(13) Uiso 1 1 d . . . C13 C 0.4268(4) 0.7732(3) 0.1008(2) 0.0484(10) Uani 1 1 d . . . C14 C 0.5516(4) 0.7903(3) 0.0517(2) 0.0497(10) Uani 1 1 d . . . C15 C 0.6635(4) 0.7384(3) 0.0967(2) 0.0450(9) Uani 1 1 d . . . C16 C 0.6538(4) 0.6752(3) 0.1827(2) 0.0393(8) Uani 1 1 d . . . H16 H 0.732(4) 0.644(3) 0.208(2) 0.038(10) Uiso 1 1 d . . . C17 C 0.5147(3) 0.5937(3) 0.3216(2) 0.0324(7) Uani 1 1 d . . . C18 C 0.5659(5) 0.8669(4) -0.0403(3) 0.0741(14) Uani 1 1 d . . . H18A H 0.4920 0.9250 -0.0479 0.111 Uiso 1 1 calc R . . H18B H 0.5617 0.8253 -0.0798 0.111 Uiso 1 1 calc R . . H18C H 0.6530 0.8987 -0.0513 0.111 Uiso 1 1 calc R . . C21 C -0.0324(3) 0.7768(2) 0.33910(19) 0.0289(7) Uani 1 1 d . . . C22 C 0.0717(3) 0.8471(3) 0.3235(2) 0.0354(8) Uani 1 1 d . . . H22 H 0.1481 0.8270 0.3555 0.042 Uiso 1 1 calc R . . C23 C 0.0605(4) 0.9480(3) 0.2593(2) 0.0394(8) Uani 1 1 d . . . C24 C -0.0459(4) 0.9828(3) 0.2058(2) 0.0436(9) Uani 1 1 d . . . C25 C -0.1477(3) 0.9090(3) 0.2253(2) 0.0375(8) Uani 1 1 d . . . C26 C -0.1443(3) 0.8099(3) 0.2901(2) 0.0325(7) Uani 1 1 d . . . H26 H -0.2171 0.7651 0.3011 0.039 Uiso 1 1 calc R . . C27 C -0.0257(3) 0.6663(2) 0.40721(19) 0.0274(7) Uani 1 1 d . . . C28 C -0.0491(5) 1.0890(4) 0.1323(3) 0.0757(15) Uani 1 1 d . . . H28A H -0.1398 1.1273 0.1331 0.114 Uiso 1 1 calc R . . H28B H -0.0269 1.0724 0.0786 0.114 Uiso 1 1 calc R . . H28C H 0.0175 1.1351 0.1385 0.114 Uiso 1 1 calc R . . C31 C 0.5479(3) 0.8150(2) 0.4568(2) 0.0294(7) Uani 1 1 d . . . C32 C 0.5018(4) 0.9143(3) 0.3986(2) 0.0349(8) Uani 1 1 d . . . H32 H 0.425(3) 0.918(3) 0.372(2) 0.032(9) Uiso 1 1 d . . . C33 C 0.5786(4) 1.0042(3) 0.3791(2) 0.0355(8) Uani 1 1 d . . . C34 C 0.6963(3) 1.0069(3) 0.4181(2) 0.0355(8) Uani 1 1 d . . . C35 C 0.7327(3) 0.9069(3) 0.4786(2) 0.0337(8) Uani 1 1 d . . . C36 C 0.6664(3) 0.8116(3) 0.4958(2) 0.0324(7) Uani 1 1 d . . . H36 H 0.7012 0.7456 0.5335 0.039 Uiso 1 1 calc R . . C37 C 0.4690(3) 0.7151(2) 0.47675(19) 0.0286(7) Uani 1 1 d . . . C38 C 0.7745(4) 1.1091(3) 0.3949(3) 0.0513(10) Uani 1 1 d . . . H38A H 0.8709 1.0898 0.3818 0.077 Uiso 1 1 calc R . . H38B H 0.7635 1.1390 0.4428 0.077 Uiso 1 1 calc R . . H38C H 0.7388 1.1636 0.3455 0.077 Uiso 1 1 calc R . . C62 C -0.1074(6) 1.3706(4) 0.1723(3) 0.0676(13) Uani 1 1 d . . . H62 H -0.027(5) 1.343(4) 0.198(3) 0.076(15) Uiso 1 1 d . . . C63 C -0.1044(5) 1.3986(4) 0.0840(3) 0.0616(12) Uani 1 1 d . . . H63 H -0.025(5) 1.388(4) 0.051(3) 0.073(15) Uiso 1 1 d . . . C64 C -0.2246(4) 1.4431(3) 0.0450(2) 0.0500(10) Uani 1 1 d . . . C65 C -0.2252(4) 1.4766(3) -0.0507(2) 0.0504(10) Uani 1 1 d . . . C66 C -0.1477(5) 1.4141(4) -0.0970(3) 0.0612(12) Uani 1 1 d . . . H66 H -0.095(4) 1.346(3) -0.068(3) 0.057(12) Uiso 1 1 d . . . C67 C -0.1473(5) 1.4486(4) -0.1871(3) 0.0695(13) Uani 1 1 d . . . H67B H -0.0942 1.4052 -0.2179 0.083 Uiso 1 1 calc R . . C62A C -0.3349(6) 1.4198(4) 0.1873(3) 0.0648(12) Uani 1 1 d . . . H62A H -0.416(5) 1.419(4) 0.229(3) 0.078(15) Uiso 1 1 d . . . C63A C -0.3420(5) 1.4533(4) 0.0990(3) 0.0611(11) Uani 1 1 d . . . H63A H -0.429(5) 1.478(4) 0.079(3) 0.081(16) Uiso 1 1 d . . . C66A C -0.2985(5) 1.5728(4) -0.0965(3) 0.0626(12) Uani 1 1 d . . . H66A H -0.358(4) 1.625(4) -0.067(3) 0.072(13) Uiso 1 1 d . . . C67A C -0.2908(5) 1.6002(4) -0.1850(3) 0.0709(13) Uani 1 1 d . . . H67A H -0.3396 1.6654 -0.2145 0.085 Uiso 1 1 calc R . . N13 N 0.2969(5) 0.8150(3) 0.0595(3) 0.0722(12) Uani 1 1 d . . . N15 N 0.8045(4) 0.7459(3) 0.0536(2) 0.0603(9) Uani 1 1 d . . . N23 N 0.1745(4) 1.0194(3) 0.2474(2) 0.0610(10) Uani 1 1 d . . . N25 N -0.2678(4) 0.9327(2) 0.1737(2) 0.0500(8) Uani 1 1 d . . . N33 N 0.5303(4) 1.1046(2) 0.3108(2) 0.0478(8) Uani 1 1 d . . . N35 N 0.8496(3) 0.8982(3) 0.5304(2) 0.0432(7) Uani 1 1 d . . . N61 N -0.2197(4) 1.3803(3) 0.2249(2) 0.0598(9) Uani 1 1 d . . . N62 N -0.2181(4) 1.5394(3) -0.2310(2) 0.0689(10) Uani 1 1 d . . . O17A O 0.3948(2) 0.58408(19) 0.35894(13) 0.0367(5) Uani 1 1 d . . . O17B O 0.6251(2) 0.5530(2) 0.35414(14) 0.0428(6) Uani 1 1 d . . . O13A O 0.2901(4) 0.7924(3) -0.0089(2) 0.0994(13) Uani 1 1 d . . . O13B O 0.2066(4) 0.8626(4) 0.0946(3) 0.1038(14) Uani 1 1 d . . . O15A O 0.8238(4) 0.7378(3) -0.0188(2) 0.0871(11) Uani 1 1 d . . . O15B O 0.8958(4) 0.7575(3) 0.0939(3) 0.0893(11) Uani 1 1 d . . . O27A O 0.0751(2) 0.64102(17) 0.45153(14) 0.0354(5) Uani 1 1 d . . . O27B O -0.1224(2) 0.60736(18) 0.41438(14) 0.0389(6) Uani 1 1 d . . . O23A O 0.1432(4) 1.1170(3) 0.2432(2) 0.0941(13) Uani 1 1 d . . . O23B O 0.2918(3) 0.9764(3) 0.2449(2) 0.0801(10) Uani 1 1 d . . . O25A O -0.2477(3) 0.9703(3) 0.0954(2) 0.0738(9) Uani 1 1 d . . . O25B O -0.3793(3) 0.9078(3) 0.2115(2) 0.0636(8) Uani 1 1 d . . . O37A O 0.3433(2) 0.72880(18) 0.46488(17) 0.0442(6) Uani 1 1 d . . . O37B O 0.5308(2) 0.61949(17) 0.50511(14) 0.0341(5) Uani 1 1 d . . . O33A O 0.6030(4) 1.1337(3) 0.2442(2) 0.0818(10) Uani 1 1 d . . . O33B O 0.4190(4) 1.1503(3) 0.3257(2) 0.0821(10) Uani 1 1 d . . . O35A O 0.9265(3) 0.8141(2) 0.5440(2) 0.0726(9) Uani 1 1 d . . . O35B O 0.8606(3) 0.9756(2) 0.55751(19) 0.0585(7) Uani 1 1 d . . . O92 O 0.1819(2) 0.43896(19) 0.40592(15) 0.0414(6) Uani 1 1 d . . . H92A H 0.1105 0.4113 0.4302 0.062 Uiso 1 1 calc R . . O93 O 0.1515(3) 0.61891(19) 0.61392(15) 0.0465(6) Uani 1 1 d . . . H93A H 0.0957 0.6688 0.5897 0.070 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 Pr1 0.02072(11) 0.02402(11) 0.02281(11) -0.00030(7) -0.00586(7) -0.00473(7) C11 0.0336(19) 0.0416(19) 0.0247(17) -0.0038(14) -0.0049(14) -0.0064(15) C12 0.031(2) 0.055(2) 0.035(2) 0.0010(17) -0.0064(17) -0.0065(18) C13 0.048(2) 0.054(2) 0.036(2) 0.0029(18) -0.0174(18) -0.0033(19) C14 0.065(3) 0.049(2) 0.0290(19) -0.0003(17) -0.0036(19) -0.011(2) C15 0.049(2) 0.044(2) 0.034(2) -0.0048(17) 0.0072(17) -0.0054(18) C16 0.040(2) 0.043(2) 0.0312(19) -0.0036(16) -0.0062(17) -0.0048(17) C17 0.035(2) 0.0373(19) 0.0247(17) -0.0052(14) -0.0082(15) -0.0063(15) C18 0.098(4) 0.071(3) 0.035(2) 0.010(2) -0.004(2) -0.005(3) C21 0.0297(17) 0.0279(17) 0.0263(16) -0.0016(13) -0.0061(14) -0.0049(14) C22 0.0308(18) 0.040(2) 0.0312(18) -0.0003(15) -0.0093(14) -0.0084(15) C23 0.039(2) 0.0340(19) 0.040(2) 0.0040(16) -0.0114(16) -0.0135(16) C24 0.048(2) 0.0351(19) 0.040(2) 0.0058(16) -0.0130(17) -0.0090(17) C25 0.0356(19) 0.0376(19) 0.0358(19) -0.0006(16) -0.0169(15) -0.0025(15) C26 0.0283(17) 0.0336(18) 0.0335(18) -0.0022(15) -0.0093(14) -0.0084(14) C27 0.0273(18) 0.0285(17) 0.0249(16) -0.0061(13) -0.0033(14) -0.0006(14) C28 0.083(3) 0.054(3) 0.072(3) 0.028(2) -0.041(3) -0.028(2) C31 0.0270(17) 0.0283(17) 0.0341(18) -0.0095(14) -0.0053(14) -0.0040(13) C32 0.0325(19) 0.0316(19) 0.041(2) -0.0069(15) -0.0132(16) -0.0053(15) C33 0.042(2) 0.0226(17) 0.0402(19) -0.0038(14) -0.0100(16) -0.0040(15) C34 0.0344(19) 0.0301(18) 0.043(2) -0.0108(16) -0.0036(16) -0.0079(15) C35 0.0282(17) 0.0338(19) 0.043(2) -0.0144(16) -0.0075(15) -0.0052(14) C36 0.0333(18) 0.0266(17) 0.0374(19) -0.0088(14) -0.0056(15) -0.0027(14) C37 0.0287(19) 0.0266(18) 0.0303(17) -0.0065(14) -0.0027(14) -0.0067(14) C38 0.055(2) 0.033(2) 0.066(3) -0.0074(18) -0.013(2) -0.0187(18) C62 0.079(4) 0.067(3) 0.055(3) -0.010(2) -0.025(3) -0.001(3) C63 0.064(3) 0.070(3) 0.047(3) -0.013(2) -0.011(2) 0.002(2) C64 0.062(3) 0.046(2) 0.044(2) -0.0154(18) -0.012(2) -0.0023(19) C65 0.060(3) 0.050(2) 0.045(2) -0.0149(19) -0.014(2) -0.007(2) C66 0.073(3) 0.061(3) 0.050(3) -0.017(2) -0.015(2) 0.004(2) C67 0.082(3) 0.079(3) 0.056(3) -0.031(3) -0.009(3) -0.010(3) C62A 0.077(3) 0.067(3) 0.051(3) -0.020(2) 0.001(3) -0.009(3) C63A 0.061(3) 0.068(3) 0.054(3) -0.019(2) -0.012(2) -0.001(2) C66A 0.073(3) 0.060(3) 0.057(3) -0.020(2) -0.018(2) 0.005(2) C67A 0.084(3) 0.067(3) 0.057(3) -0.005(2) -0.026(3) -0.002(3) N13 0.079(3) 0.074(3) 0.048(2) 0.017(2) -0.033(2) -0.015(2) N15 0.060(2) 0.058(2) 0.052(2) -0.0070(18) 0.0166(19) -0.0084(19) N23 0.064(3) 0.055(2) 0.052(2) 0.0193(17) -0.0262(18) -0.031(2) N25 0.054(2) 0.0361(17) 0.055(2) 0.0018(16) -0.0284(18) -0.0018(15) N33 0.061(2) 0.0287(16) 0.051(2) -0.0016(15) -0.0164(17) -0.0096(16) N35 0.0347(17) 0.0414(18) 0.057(2) -0.0138(15) -0.0144(14) -0.0094(15) N61 0.087(3) 0.052(2) 0.042(2) -0.0154(17) -0.012(2) -0.0036(19) N62 0.079(3) 0.079(3) 0.050(2) -0.013(2) -0.018(2) -0.016(2) O17A 0.0311(13) 0.0456(14) 0.0272(12) 0.0004(10) -0.0033(10) -0.0080(10) O17B 0.0330(14) 0.0614(16) 0.0263(12) -0.0002(11) -0.0103(10) -0.0006(12) O13A 0.130(3) 0.094(3) 0.069(2) 0.005(2) -0.061(2) -0.017(2) O13B 0.073(3) 0.136(4) 0.084(3) -0.019(3) -0.026(2) 0.045(3) O15A 0.098(3) 0.095(3) 0.058(2) -0.0225(19) 0.0365(19) -0.015(2) O15B 0.050(2) 0.116(3) 0.094(3) -0.026(2) 0.0151(19) -0.015(2) O27A 0.0311(12) 0.0314(12) 0.0392(13) 0.0008(10) -0.0158(11) -0.0025(10) O27B 0.0376(13) 0.0369(13) 0.0366(13) 0.0058(10) -0.0128(10) -0.0170(11) O23A 0.114(3) 0.047(2) 0.115(3) 0.0153(19) -0.057(2) -0.0392(19) O23B 0.051(2) 0.095(2) 0.080(2) 0.0091(19) -0.0171(17) -0.0351(19) O25A 0.089(2) 0.071(2) 0.0506(19) 0.0144(16) -0.0367(17) -0.0211(17) O25B 0.0409(17) 0.075(2) 0.077(2) -0.0191(16) -0.0238(16) -0.0028(15) O37A 0.0314(14) 0.0314(13) 0.0684(17) -0.0096(12) -0.0111(12) -0.0055(10) O37B 0.0378(13) 0.0248(12) 0.0385(13) -0.0051(10) -0.0096(10) -0.0030(10) O33A 0.093(2) 0.066(2) 0.059(2) 0.0195(17) 0.0007(19) -0.0121(18) O33B 0.090(3) 0.063(2) 0.073(2) -0.0003(17) -0.0160(19) 0.0288(19) O35A 0.0517(18) 0.0542(18) 0.123(3) -0.0315(18) -0.0504(18) 0.0114(15) O35B 0.0609(18) 0.0559(17) 0.0697(19) -0.0245(15) -0.0244(15) -0.0138(14) O92 0.0354(13) 0.0445(14) 0.0465(14) -0.0120(11) -0.0078(11) -0.0124(11) O93 0.0562(16) 0.0427(14) 0.0386(14) -0.0114(11) -0.0101(12) 0.0077(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 Pr1 O27B 2.420(2) 2_566 ? Pr1 O17A 2.421(2) . ? Pr1 O27A 2.422(2) . ? Pr1 O17B 2.467(2) 2_666 ? Pr1 O37B 2.483(2) 2_666 ? Pr1 O92 2.563(2) . ? Pr1 O93 2.563(2) . ? Pr1 O37A 2.567(2) . ? Pr1 O37B 2.828(2) . ? Pr1 C37 3.070(3) . ? C11 C16 1.369(5) . ? C11 C12 1.372(5) . ? C11 C17 1.506(4) . ? C12 C13 1.378(5) . ? C13 C14 1.376(5) . ? C13 N13 1.477(5) . ? C14 C15 1.378(5) . ? C14 C18 1.519(5) . ? C15 C16 1.386(5) . ? C15 N15 1.468(5) . ? C17 O17B 1.247(4) . ? C17 O17A 1.254(4) . ? C21 C26 1.382(4) . ? C21 C22 1.383(4) . ? C21 C27 1.501(4) . ? C22 C23 1.387(5) . ? C23 C24 1.385(5) . ? C23 N23 1.478(5) . ? C24 C25 1.389(5) . ? C24 C28 1.506(5) . ? C25 C26 1.375(4) . ? C25 N25 1.478(4) . ? C27 O27B 1.247(4) . ? C27 O27A 1.248(4) . ? C31 C36 1.380(4) . ? C31 C32 1.390(4) . ? C31 C37 1.494(4) . ? C32 C33 1.376(5) . ? C33 C34 1.391(5) . ? C33 N33 1.486(4) . ? C34 C35 1.388(5) . ? C34 C38 1.510(5) . ? C35 C36 1.378(4) . ? C35 N35 1.479(4) . ? C37 O37A 1.251(4) . ? C37 O37B 1.266(4) . ? C62 N61 1.326(6) . ? C62 C63 1.374(6) . ? C63 C64 1.383(6) . ? C64 C63A 1.378(6) . ? C64 C65 1.490(5) . ? C65 C66 1.367(6) . ? C65 C66A 1.389(6) . ? C66 C67 1.402(6) . ? C67 N62 1.321(6) . ? C62A N61 1.319(6) . ? C62A C63A 1.382(6) . ? C66A C67A 1.374(6) . ? C67A N62 1.328(6) . ? N13 O13B 1.199(5) . ? N13 O13A 1.249(5) . ? N15 O15A 1.211(5) . ? N15 O15B 1.220(5) . ? N23 O23B 1.212(5) . ? N23 O23A 1.226(5) . ? N25 O25B 1.210(4) . ? N25 O25A 1.220(4) . ? N33 O33A 1.203(4) . ? N33 O33B 1.205(4) . ? N35 O35A 1.209(4) . ? N35 O35B 1.218(4) . ? O17B Pr1 2.467(2) 2_666 ? O27B Pr1 2.420(2) 2_566 ? O37B Pr1 2.483(2) 2_666 ? 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 O27B Pr1 O17A 137.02(8) 2_566 . ? O27B Pr1 O27A 84.63(8) 2_566 . ? O17A Pr1 O27A 89.09(8) . . ? O27B Pr1 O17B 75.59(8) 2_566 2_666 ? O17A Pr1 O17B 131.75(8) . 2_666 ? O27A Pr1 O17B 135.70(8) . 2_666 ? O27B Pr1 O37B 92.23(8) 2_566 2_666 ? O17A Pr1 O37B 73.30(7) . 2_666 ? O27A Pr1 O37B 150.44(8) . 2_666 ? O17B Pr1 O37B 70.72(8) 2_666 2_666 ? O27B Pr1 O92 68.67(8) 2_566 . ? O17A Pr1 O92 68.95(8) . . ? O27A Pr1 O92 72.02(8) . . ? O17B Pr1 O92 131.90(8) 2_666 . ? O37B Pr1 O92 79.44(8) 2_666 . ? O27B Pr1 O93 76.98(9) 2_566 . ? O17A Pr1 O93 138.18(8) . . ? O27A Pr1 O93 67.41(8) . . ? O17B Pr1 O93 69.66(8) 2_666 . ? O37B Pr1 O93 140.36(7) 2_666 . ? O92 Pr1 O93 128.41(8) . . ? O27B Pr1 O37A 146.29(8) 2_566 . ? O17A Pr1 O37A 69.90(8) . . ? O27A Pr1 O37A 74.59(8) . . ? O17B Pr1 O37A 101.10(8) 2_666 . ? O37B Pr1 O37A 118.78(8) 2_666 . ? O92 Pr1 O37A 126.46(8) . . ? O93 Pr1 O37A 70.66(8) . . ? O27B Pr1 O37B 145.22(7) 2_566 . ? O17A Pr1 O37B 70.47(7) . . ? O27A Pr1 O37B 122.38(7) . . ? O17B Pr1 O37B 69.71(7) 2_666 . ? O37B Pr1 O37B 74.49(8) 2_666 . ? O92 Pr1 O37B 136.48(7) . . ? O93 Pr1 O37B 92.82(8) . . ? O37A Pr1 O37B 47.89(7) . . ? O27B Pr1 C37 155.33(8) 2_566 . ? O17A Pr1 C37 67.65(8) . . ? O27A Pr1 C37 98.05(8) . . ? O17B Pr1 C37 85.86(8) 2_666 . ? O37B Pr1 C37 96.89(8) 2_666 . ? O92 Pr1 C37 135.55(8) . . ? O93 Pr1 C37 81.44(8) . . ? O37A Pr1 C37 23.55(8) . . ? O37B Pr1 C37 24.35(7) . . ? C16 C11 C12 118.7(3) . . ? C16 C11 C17 119.9(3) . . ? C12 C11 C17 121.4(3) . . ? C11 C12 C13 119.3(4) . . ? C14 C13 C12 124.9(3) . . ? C14 C13 N13 119.5(3) . . ? C12 C13 N13 115.6(4) . . ? C13 C14 C15 113.2(3) . . ? C13 C14 C18 123.4(4) . . ? C15 C14 C18 123.1(4) . . ? C14 C15 C16 124.3(3) . . ? C14 C15 N15 120.4(3) . . ? C16 C15 N15 115.3(3) . . ? C11 C16 C15 119.5(3) . . ? O17B C17 O17A 126.6(3) . . ? O17B C17 C11 116.8(3) . . ? O17A C17 C11 116.6(3) . . ? C26 C21 C22 118.7(3) . . ? C26 C21 C27 119.9(3) . . ? C22 C21 C27 121.4(3) . . ? C21 C22 C23 118.9(3) . . ? C24 C23 C22 124.6(3) . . ? C24 C23 N23 119.5(3) . . ? C22 C23 N23 115.8(3) . . ? C23 C24 C25 113.5(3) . . ? C23 C24 C28 123.1(3) . . ? C25 C24 C28 123.3(3) . . ? C26 C25 C24 124.2(3) . . ? C26 C25 N25 115.2(3) . . ? C24 C25 N25 120.6(3) . . ? C25 C26 C21 119.9(3) . . ? O27B C27 O27A 125.7(3) . . ? O27B C27 C21 116.6(3) . . ? O27A C27 C21 117.8(3) . . ? C36 C31 C32 118.5(3) . . ? C36 C31 C37 121.3(3) . . ? C32 C31 C37 120.2(3) . . ? C33 C32 C31 119.1(3) . . ? C32 C33 C34 124.9(3) . . ? C32 C33 N33 116.3(3) . . ? C34 C33 N33 118.8(3) . . ? C35 C34 C33 112.9(3) . . ? C35 C34 C38 124.8(3) . . ? C33 C34 C38 122.3(3) . . ? C36 C35 C34 124.7(3) . . ? C36 C35 N35 115.6(3) . . ? C34 C35 N35 119.7(3) . . ? C35 C36 C31 119.5(3) . . ? O37A C37 O37B 122.0(3) . . ? O37A C37 C31 118.6(3) . . ? O37B C37 C31 119.4(3) . . ? O37A C37 Pr1 55.03(15) . . ? O37B C37 Pr1 67.05(16) . . ? C31 C37 Pr1 173.2(2) . . ? N61 C62 C63 124.7(5) . . ? C62 C63 C64 119.2(5) . . ? C63A C64 C63 116.6(4) . . ? C63A C64 C65 122.5(4) . . ? C63 C64 C65 120.9(4) . . ? C66 C65 C66A 117.4(4) . . ? C66 C65 C64 120.1(4) . . ? C66A C65 C64 122.5(4) . . ? C65 C66 C67 119.1(4) . . ? N62 C67 C66 123.7(5) . . ? N61 C62A C63A 123.9(5) . . ? C64 C63A C62A 119.8(5) . . ? C67A C66A C65 119.3(5) . . ? N62 C67A C66A 124.2(4) . . ? O13B N13 O13A 125.8(4) . . ? O13B N13 C13 119.0(4) . . ? O13A N13 C13 115.1(5) . . ? O15A N15 O15B 124.0(4) . . ? O15A N15 C15 118.2(4) . . ? O15B N15 C15 117.8(4) . . ? O23B N23 O23A 124.9(4) . . ? O23B N23 C23 117.5(4) . . ? O23A N23 C23 117.6(4) . . ? O25B N25 O25A 123.9(3) . . ? O25B N25 C25 117.7(3) . . ? O25A N25 C25 118.3(3) . . ? O33A N33 O33B 124.5(3) . . ? O33A N33 C33 118.4(3) . . ? O33B N33 C33 117.1(3) . . ? O35A N35 O35B 124.5(3) . . ? O35A N35 C35 117.7(3) . . ? O35B N35 C35 117.7(3) . . ? C62A N61 C62 115.8(4) . . ? C67 N62 C67A 116.4(4) . . ? C17 O17A Pr1 139.2(2) . . ? C17 O17B Pr1 141.0(2) . 2_666 ? C27 O27A Pr1 153.6(2) . . ? C27 O27B Pr1 153.3(2) . 2_566 ? C37 O37A Pr1 101.42(18) . . ? C37 O37B Pr1 152.6(2) . 2_666 ? C37 O37B Pr1 88.60(18) . . ? Pr1 O37B Pr1 105.51(8) 2_666 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.609 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.067 data_3 _database_code_depnum_ccdc_archive 'CCDC 233740' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetraacqa-hemi-(1,2-bis(4-pyridyl)ethene-tris-(3,5-dinitro-4-methyl benzoato) Praseodymium(III) complex ; _chemical_name_common ; Tetraacqa-hemi-(1,2-bis(4-pyridyl)ethene-tris-(3,5-dinitro-4- methyl benzoato) Praseodymium(iii) complex ; _chemical_melting_point ? _chemical_formula_moiety '[Pr(C8H5N2O6)3(H2O)2].0.5(C12H10N2).2(H2O)' _chemical_formula_sum 'C30 H28 N7 O22 Pr' _chemical_formula_weight 979.50 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.510(9) _cell_length_b 12.669(9) _cell_length_c 16.430(2) _cell_angle_alpha 72.28(2) _cell_angle_beta 79.06(2) _cell_angle_gamma 79.72(2) _cell_volume 1836(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.429 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 CCD-Area detector' _diffrn_measurement_method SMART _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15345 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 23.35 _reflns_number_total 5279 _reflns_number_gt 4253 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINTPLUS _computing_structure_solution 'SHELXTL (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL (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^)+(0.0292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5279 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _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 Pr1 Pr 0.27995(3) 0.53168(2) 0.506343(19) 0.02961(10) Uani 1 1 d . . . C11 C 0.5420(5) 0.6536(4) 0.2234(3) 0.0332(12) Uani 1 1 d . . . C12 C 0.4214(6) 0.7086(5) 0.1855(4) 0.0449(15) Uani 1 1 d . . . H12 H 0.329(5) 0.714(4) 0.218(3) 0.044(16) Uiso 1 1 d . . . C13 C 0.4402(6) 0.7575(5) 0.0965(4) 0.0505(16) Uani 1 1 d . . . C14 C 0.5706(7) 0.7589(5) 0.0419(4) 0.0583(17) Uani 1 1 d . . . C15 C 0.6864(6) 0.7002(5) 0.0836(4) 0.0517(16) Uani 1 1 d . . . C16 C 0.6733(6) 0.6513(5) 0.1724(4) 0.0423(14) Uani 1 1 d . . . H16 H 0.757(5) 0.613(4) 0.198(3) 0.033(14) Uiso 1 1 d . . . C17 C 0.5248(6) 0.5967(4) 0.3189(3) 0.0347(13) Uani 1 1 d . . . C18 C 0.5829(8) 0.8227(6) -0.0532(4) 0.103(3) Uani 1 1 d . . . H18A H 0.6768 0.8467 -0.0725 0.154 Uiso 1 1 calc R . . H18B H 0.5103 0.8867 -0.0614 0.154 Uiso 1 1 calc R . . H18C H 0.5694 0.7750 -0.0859 0.154 Uiso 1 1 calc R . . C21 C -0.0315(5) 0.7724(4) 0.3356(3) 0.0321(12) Uani 1 1 d . . . C22 C -0.1362(5) 0.7983(4) 0.2819(3) 0.0356(13) Uani 1 1 d . . . H22 H -0.199(4) 0.747(3) 0.293(3) 0.027(13) Uiso 1 1 d . . . C23 C -0.1350(5) 0.8931(4) 0.2142(3) 0.0414(14) Uani 1 1 d . . . C24 C -0.0389(5) 0.9707(4) 0.1960(3) 0.0394(13) Uani 1 1 d . . . C25 C 0.0598(5) 0.9418(4) 0.2541(3) 0.0376(13) Uani 1 1 d . . . C26 C 0.0675(5) 0.8457(4) 0.3215(3) 0.0380(14) Uani 1 1 d . . . H26 H 0.136(4) 0.827(3) 0.356(3) 0.018(12) Uiso 1 1 d . . . C27 C -0.0284(5) 0.6664(4) 0.4088(3) 0.0353(13) Uani 1 1 d . . . C28 C -0.0409(6) 1.0741(4) 0.1204(3) 0.0598(17) Uani 1 1 d . . . H28A H 0.0383 1.1131 0.1177 0.090 Uiso 1 1 calc R . . H28B H -0.1302 1.1217 0.1274 0.090 Uiso 1 1 calc R . . H28C H -0.0322 1.0532 0.0680 0.090 Uiso 1 1 calc R . . O51 O 0.3601(4) 0.4388(3) 0.6486(2) 0.0454(10) Uani 1 1 d . . . O61 O 0.1902(4) 0.4459(3) 0.4015(2) 0.0548(10) Uani 1 1 d . . . O71 O 0.1386(4) 0.6260(3) 0.6206(2) 0.0512(10) Uani 1 1 d . . . O91 O 0.1279(10) 0.5481(7) 0.2255(5) 0.211(4) Uani 1 1 d . . . O92 O 0.1852(12) 0.3469(10) 0.2250(8) 0.317(6) Uani 1 1 d . . . C31 C 0.5440(5) 0.8121(4) 0.4578(3) 0.0308(12) Uani 1 1 d . . . C32 C 0.6552(5) 0.8090(4) 0.5017(3) 0.0350(13) Uani 1 1 d . . . H32 H 0.6831 0.7447 0.5440 0.042 Uiso 1 1 calc R . . C33 C 0.7252(5) 0.9026(4) 0.4823(3) 0.0358(13) Uani 1 1 d . . . C34 C 0.6975(5) 0.9996(4) 0.4168(3) 0.0369(13) Uani 1 1 d . . . C35 C 0.5857(5) 0.9962(4) 0.3740(3) 0.0367(13) Uani 1 1 d . . . C36 C 0.5070(5) 0.9085(4) 0.3949(3) 0.0361(13) Uani 1 1 d . . . H36 H 0.428(4) 0.910(3) 0.365(2) 0.013(10) Uiso 1 1 d . . . C37 C 0.4589(5) 0.7158(4) 0.4789(3) 0.0334(12) Uani 1 1 d . . . C38 C 0.7814(6) 1.0970(4) 0.3913(4) 0.0527(16) Uani 1 1 d . . . H38A H 0.8826 1.0704 0.3896 0.079 Uiso 1 1 calc R . . H38B H 0.7521 1.1392 0.4327 0.079 Uiso 1 1 calc R . . H38C H 0.7631 1.1438 0.3352 0.079 Uiso 1 1 calc R . . C42 C 0.1792(9) 0.6252(6) 0.8341(5) 0.084(2) Uani 1 1 d . . . H42 H 0.0794 0.6393 0.8366 0.101 Uiso 1 1 calc R . . C43 C 0.2344(9) 0.5934(6) 0.9104(5) 0.086(2) Uani 1 1 d . . . H43 H 0.1731 0.5885 0.9624 0.103 Uiso 1 1 calc R . . C44 C 0.3814(10) 0.5685(5) 0.9094(5) 0.077(2) Uani 1 1 d . . . C45 C 0.4677(10) 0.5853(6) 0.8289(6) 0.077(2) Uani 1 1 d . . . H45 H 0.576(8) 0.571(6) 0.820(4) 0.10(3) Uiso 1 1 d . . . C46 C 0.3993(10) 0.6188(6) 0.7558(5) 0.072(2) Uani 1 1 d . . . H46 H 0.459(6) 0.623(4) 0.704(3) 0.049(19) Uiso 1 1 d . . . C47 C 0.4354(9) 0.5219(6) 0.9973(6) 0.104(3) Uani 1 1 d . . . O33A O 0.9050(5) 0.8065(4) 0.5622(3) 0.0851(16) Uani 1 1 d . . . O33B O 0.8440(4) 0.9780(3) 0.5582(3) 0.0647(12) Uani 1 1 d . . . O35A O 0.6318(5) 1.1171(3) 0.2362(3) 0.0733(13) Uani 1 1 d . . . O35B O 0.4263(5) 1.1454(3) 0.3134(3) 0.0694(13) Uani 1 1 d . . . O37A O 0.3324(4) 0.7352(3) 0.4636(2) 0.0480(10) Uani 1 1 d . . . O37B O 0.5180(3) 0.6174(3) 0.5121(2) 0.0374(9) Uani 1 1 d . . . O23A O -0.2075(6) 0.9301(5) 0.0801(3) 0.1033(19) Uani 1 1 d . . . O23B O -0.3691(5) 0.9004(4) 0.1920(3) 0.0725(13) Uani 1 1 d . . . O25A O 0.1237(5) 1.1163(4) 0.2382(3) 0.0844(15) Uani 1 1 d . . . O25B O 0.2932(5) 0.9755(4) 0.2443(3) 0.0765(14) Uani 1 1 d . . . O27A O 0.0653(3) 0.6463(3) 0.4570(2) 0.0401(9) Uani 1 1 d . . . O27B O -0.1228(4) 0.6055(3) 0.4165(2) 0.0503(10) Uani 1 1 d . . . N13 N 0.3041(8) 0.8135(7) 0.0647(5) 0.096(2) Uani 1 1 d . . . N15 N 0.8312(7) 0.6863(5) 0.0347(4) 0.0814(18) Uani 1 1 d . . . N23 N -0.2469(6) 0.9110(4) 0.1578(4) 0.0549(14) Uani 1 1 d . . . N25 N 0.1671(6) 1.0181(5) 0.2447(3) 0.0548(14) Uani 1 1 d . . . N33 N 0.8360(5) 0.8958(4) 0.5373(3) 0.0472(12) Uani 1 1 d . . . N35 N 0.5456(6) 1.0942(4) 0.3021(3) 0.0461(12) Uani 1 1 d . . . N41 N 0.2579(8) 0.6374(4) 0.7571(4) 0.0709(16) Uani 1 1 d . . . O13A O 0.2824(9) 0.7845(6) 0.0025(6) 0.194(4) Uani 1 1 d . . . O13B O 0.2272(8) 0.8733(9) 0.0882(5) 0.221(6) Uani 1 1 d . . . O15A O 0.9337(6) 0.6787(6) 0.0711(4) 0.124(2) Uani 1 1 d . . . O15B O 0.8435(6) 0.6791(5) -0.0380(4) 0.117(2) Uani 1 1 d . . . O17A O 0.3989(4) 0.5882(3) 0.3582(2) 0.0440(9) 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 Pr1 0.02327(16) 0.02844(17) 0.03562(18) 0.00026(12) -0.01125(12) -0.00830(11) C11 0.035(3) 0.034(3) 0.031(3) -0.003(2) -0.010(3) -0.009(3) C12 0.036(4) 0.050(4) 0.046(4) -0.006(3) -0.008(3) -0.008(3) C13 0.051(4) 0.047(4) 0.049(4) 0.005(3) -0.025(3) -0.007(3) C14 0.070(5) 0.056(4) 0.043(4) 0.000(3) -0.010(4) -0.016(4) C15 0.051(4) 0.053(4) 0.044(4) -0.005(3) 0.006(3) -0.015(3) C16 0.044(4) 0.041(4) 0.040(4) -0.001(3) -0.013(3) -0.010(3) C17 0.042(3) 0.028(3) 0.036(3) -0.004(2) -0.014(3) -0.009(3) C18 0.128(7) 0.110(6) 0.044(5) 0.014(4) -0.007(4) -0.017(5) C21 0.029(3) 0.030(3) 0.036(3) -0.002(2) -0.006(2) -0.010(2) C22 0.033(3) 0.033(3) 0.042(4) -0.003(3) -0.013(3) -0.013(3) C23 0.036(3) 0.046(4) 0.045(4) -0.005(3) -0.025(3) -0.007(3) C24 0.040(3) 0.038(3) 0.036(3) 0.001(3) -0.008(3) -0.010(3) C25 0.034(3) 0.032(3) 0.044(3) 0.003(3) -0.013(3) -0.014(3) C26 0.029(3) 0.043(4) 0.039(3) 0.001(3) -0.013(3) -0.010(3) C27 0.027(3) 0.032(3) 0.042(3) -0.004(3) -0.002(3) -0.005(3) C28 0.068(4) 0.048(4) 0.056(4) 0.010(3) -0.025(3) -0.015(3) O51 0.037(2) 0.055(2) 0.039(2) 0.0035(18) -0.0188(18) -0.0084(19) O61 0.046(2) 0.051(2) 0.074(3) -0.017(2) -0.021(2) -0.0083(19) O71 0.056(2) 0.051(2) 0.047(2) -0.0132(19) -0.017(2) 0.001(2) O91 0.252(9) 0.216(9) 0.192(8) -0.072(6) -0.097(7) -0.007(7) O92 0.285(13) 0.312(15) 0.342(15) -0.044(11) -0.075(11) -0.061(11) C31 0.028(3) 0.029(3) 0.037(3) -0.008(2) -0.009(2) -0.008(2) C32 0.035(3) 0.027(3) 0.042(3) -0.005(2) -0.009(3) -0.006(2) C33 0.026(3) 0.038(3) 0.050(4) -0.016(3) -0.015(3) -0.004(2) C34 0.034(3) 0.034(3) 0.046(4) -0.012(3) -0.005(3) -0.012(3) C35 0.040(3) 0.023(3) 0.045(3) -0.003(3) -0.011(3) -0.004(3) C36 0.031(3) 0.037(3) 0.042(3) -0.008(3) -0.010(3) -0.012(3) C37 0.036(3) 0.030(3) 0.036(3) -0.010(3) -0.008(3) -0.004(3) C38 0.049(4) 0.044(4) 0.068(4) -0.011(3) -0.011(3) -0.021(3) C42 0.099(6) 0.085(6) 0.076(6) -0.030(5) -0.041(5) 0.009(5) C43 0.102(7) 0.087(6) 0.080(6) -0.038(5) -0.030(5) 0.004(5) C44 0.114(7) 0.054(5) 0.074(6) -0.018(4) -0.044(5) -0.003(5) C45 0.085(6) 0.057(5) 0.096(7) -0.020(4) -0.037(6) -0.003(4) C46 0.101(7) 0.051(5) 0.066(6) -0.012(4) -0.028(6) -0.009(4) C47 0.144(9) 0.063(5) 0.135(7) -0.038(5) -0.096(7) 0.004(5) O33A 0.073(3) 0.059(3) 0.144(5) -0.041(3) -0.077(3) 0.023(3) O33B 0.071(3) 0.057(3) 0.082(3) -0.026(2) -0.035(2) -0.014(2) O35A 0.080(3) 0.065(3) 0.057(3) 0.006(2) 0.001(3) -0.015(3) O35B 0.061(3) 0.056(3) 0.077(3) 0.000(2) -0.019(3) 0.005(2) O37A 0.031(2) 0.032(2) 0.082(3) -0.0072(19) -0.024(2) -0.0058(17) O37B 0.036(2) 0.028(2) 0.047(2) -0.0006(17) -0.0158(18) -0.0078(17) O23A 0.114(4) 0.149(5) 0.046(3) 0.014(3) -0.036(3) -0.061(4) O23B 0.047(3) 0.081(3) 0.096(4) -0.022(3) -0.032(3) -0.006(3) O25A 0.101(4) 0.045(3) 0.109(4) 0.002(3) -0.036(3) -0.033(3) O25B 0.049(3) 0.083(3) 0.094(4) 0.005(3) -0.028(3) -0.032(3) O27A 0.031(2) 0.037(2) 0.051(2) 0.0033(17) -0.0250(19) -0.0070(16) O27B 0.044(2) 0.042(2) 0.061(3) 0.0138(19) -0.026(2) -0.0251(19) N13 0.095(6) 0.118(6) 0.060(5) 0.001(4) -0.052(4) 0.021(5) N15 0.071(5) 0.104(5) 0.056(4) -0.004(4) 0.005(4) -0.026(4) N23 0.059(4) 0.050(3) 0.056(4) 0.002(3) -0.032(3) -0.014(3) N25 0.059(4) 0.057(4) 0.046(3) 0.010(3) -0.020(3) -0.030(3) N33 0.041(3) 0.046(3) 0.061(3) -0.018(3) -0.015(3) -0.009(3) N35 0.051(3) 0.031(3) 0.055(4) -0.002(3) -0.019(3) -0.009(3) N41 0.096(5) 0.056(4) 0.066(4) -0.017(3) -0.037(4) 0.005(3) O13A 0.206(8) 0.161(7) 0.243(9) -0.059(6) -0.170(8) 0.055(6) O13B 0.161(7) 0.357(13) 0.120(6) -0.118(7) -0.085(5) 0.194(8) O15A 0.059(4) 0.197(7) 0.104(5) -0.031(4) 0.010(3) -0.028(4) O15B 0.105(4) 0.170(6) 0.063(4) -0.033(4) 0.022(3) -0.020(4) O17A 0.035(2) 0.055(2) 0.038(2) -0.0035(18) -0.0077(18) -0.0104(19) _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 Pr1 O27B 2.393(4) 2_566 ? Pr1 O27A 2.406(4) . ? Pr1 O17A 2.428(4) . ? Pr1 O51 2.472(4) . ? Pr1 O37B 2.486(4) 2_666 ? Pr1 O71 2.567(4) . ? Pr1 O37A 2.572(4) . ? Pr1 O61 2.628(4) . ? Pr1 O37B 2.708(4) . ? Pr1 C37 3.005(5) . ? Pr1 Pr1 4.096(4) 2_666 ? C11 C16 1.366(7) . ? C11 C12 1.382(7) . ? C11 C17 1.505(7) . ? C12 C13 1.394(8) . ? C13 C14 1.386(8) . ? C13 N13 1.468(8) . ? C14 C15 1.385(8) . ? C14 C18 1.518(8) . ? C15 C16 1.391(7) . ? C15 N15 1.467(8) . ? C17 O17A 1.254(6) . ? C17 O51 1.259(6) 2_666 ? C21 C26 1.379(6) . ? C21 C22 1.386(6) . ? C21 C27 1.505(6) . ? C22 C23 1.366(7) . ? C23 C24 1.389(7) . ? C23 N23 1.483(6) . ? C24 C25 1.390(7) . ? C24 C28 1.505(7) . ? C25 C26 1.376(7) . ? C25 N25 1.484(6) . ? C27 O27A 1.244(6) . ? C27 O27B 1.250(5) . ? O51 C17 1.259(6) 2_666 ? C31 C32 1.377(6) . ? C31 C36 1.378(7) . ? C31 C37 1.501(6) . ? C32 C33 1.386(6) . ? C33 C34 1.387(7) . ? C33 N33 1.489(6) . ? C34 C35 1.395(7) . ? C34 C38 1.498(6) . ? C35 C36 1.372(6) . ? C35 N35 1.480(6) . ? C37 O37A 1.242(5) . ? C37 O37B 1.273(5) . ? C42 N41 1.322(8) . ? C42 C43 1.370(9) . ? C43 C44 1.375(10) . ? C44 C45 1.395(10) . ? C44 C47 1.534(10) . ? C45 C46 1.389(10) . ? C46 N41 1.321(9) . ? C47 C47 1.262(14) 2_667 ? O33A N33 1.197(5) . ? O33B N33 1.210(5) . ? O35A N35 1.219(5) . ? O35B N35 1.213(5) . ? O37B Pr1 2.486(4) 2_666 ? O23A N23 1.222(6) . ? O23B N23 1.202(6) . ? O25A N25 1.217(6) . ? O25B N25 1.223(6) . ? O27B Pr1 2.393(3) 2_566 ? N13 O13B 1.063(8) . ? N13 O13A 1.249(9) . ? N15 O15B 1.207(7) . ? N15 O15A 1.212(7) . ? 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 O27B Pr1 O27A 85.30(13) 2_566 . ? O27B Pr1 O17A 133.98(12) 2_566 . ? O27A Pr1 O17A 87.52(13) . . ? O27B Pr1 O51 72.53(12) 2_566 . ? O27A Pr1 O51 135.39(12) . . ? O17A Pr1 O51 135.44(13) . . ? O27B Pr1 O37B 90.83(13) 2_566 2_666 ? O27A Pr1 O37B 148.14(12) . 2_666 ? O17A Pr1 O37B 72.62(12) . 2_666 ? O51 Pr1 O37B 72.06(12) . 2_666 ? O27B Pr1 O71 80.43(14) 2_566 . ? O27A Pr1 O71 69.27(13) . . ? O17A Pr1 O71 137.76(12) . . ? O51 Pr1 O71 69.18(13) . . ? O37B Pr1 O71 141.14(11) 2_666 . ? O27B Pr1 O37A 148.96(12) 2_566 . ? O27A Pr1 O37A 73.73(11) . . ? O17A Pr1 O37A 68.80(12) . . ? O51 Pr1 O37A 106.84(12) . . ? O37B Pr1 O37A 119.00(12) 2_666 . ? O71 Pr1 O37A 70.95(12) . . ? O27B Pr1 O61 68.44(14) 2_566 . ? O27A Pr1 O61 71.16(12) . . ? O17A Pr1 O61 66.23(13) . . ? O51 Pr1 O61 129.71(13) . . ? O37B Pr1 O61 78.00(12) 2_666 . ? O71 Pr1 O61 130.91(12) . . ? O37A Pr1 O61 122.98(12) . . ? O27B Pr1 O37B 144.19(11) 2_566 . ? O27A Pr1 O37B 122.93(12) . . ? O17A Pr1 O37B 74.02(12) . . ? O51 Pr1 O37B 71.75(11) . . ? O37B Pr1 O37B 75.96(13) 2_666 . ? O71 Pr1 O37B 89.26(12) . . ? O37A Pr1 O37B 49.20(10) . . ? O61 Pr1 O37B 137.35(11) . . ? O27B Pr1 C37 157.49(13) 2_566 . ? O27A Pr1 C37 97.89(14) . . ? O17A Pr1 C37 68.53(13) . . ? O51 Pr1 C37 90.22(13) . . ? O37B Pr1 C37 97.61(14) 2_666 . ? O71 Pr1 C37 79.93(13) . . ? O37A Pr1 C37 24.17(11) . . ? O61 Pr1 C37 133.71(13) . . ? O37B Pr1 C37 25.06(11) . . ? O27B Pr1 Pr1 123.01(9) 2_566 2_666 ? O27A Pr1 Pr1 151.03(8) . 2_666 ? O17A Pr1 Pr1 68.70(9) . 2_666 ? O51 Pr1 Pr1 66.80(9) . 2_666 ? O37B Pr1 Pr1 39.89(7) 2_666 2_666 ? O71 Pr1 Pr1 117.65(8) . 2_666 ? O37A Pr1 Pr1 82.09(8) . 2_666 ? O61 Pr1 Pr1 111.10(9) . 2_666 ? O37B Pr1 Pr1 36.08(8) . 2_666 ? C37 Pr1 Pr1 58.77(11) . 2_666 ? C16 C11 C12 118.7(5) . . ? C16 C11 C17 122.0(5) . . ? C12 C11 C17 119.3(5) . . ? C11 C12 C13 117.9(5) . . ? C14 C13 C12 125.9(5) . . ? C14 C13 N13 121.8(6) . . ? C12 C13 N13 112.3(6) . . ? C15 C14 C13 113.2(5) . . ? C15 C14 C18 124.5(6) . . ? C13 C14 C18 122.3(6) . . ? C14 C15 C16 122.9(6) . . ? C14 C15 N15 120.6(6) . . ? C16 C15 N15 116.4(6) . . ? C11 C16 C15 121.2(5) . . ? O17A C17 O51 126.4(5) . 2_666 ? O17A C17 C11 117.6(4) . . ? O51 C17 C11 116.0(5) 2_666 . ? C26 C21 C22 118.9(5) . . ? C26 C21 C27 121.1(4) . . ? C22 C21 C27 120.0(4) . . ? C23 C22 C21 119.3(5) . . ? C22 C23 C24 124.9(5) . . ? C22 C23 N23 115.4(5) . . ? C24 C23 N23 119.6(5) . . ? C23 C24 C25 112.8(4) . . ? C23 C24 C28 123.3(5) . . ? C25 C24 C28 123.9(5) . . ? C26 C25 C24 125.0(5) . . ? C26 C25 N25 115.7(4) . . ? C24 C25 N25 119.3(4) . . ? C25 C26 C21 118.9(5) . . ? O27A C27 O27B 125.1(5) . . ? O27A C27 C21 118.6(4) . . ? O27B C27 C21 116.3(4) . . ? C17 O51 Pr1 139.6(3) 2_666 . ? C32 C31 C36 118.6(4) . . ? C32 C31 C37 122.0(4) . . ? C36 C31 C37 119.4(4) . . ? C31 C32 C33 119.4(5) . . ? C32 C33 C34 124.5(4) . . ? C32 C33 N33 116.1(4) . . ? C34 C33 N33 119.4(4) . . ? C33 C34 C35 113.0(4) . . ? C33 C34 C38 124.3(5) . . ? C35 C34 C38 122.6(5) . . ? C36 C35 C34 124.5(5) . . ? C36 C35 N35 116.9(4) . . ? C34 C35 N35 118.6(4) . . ? C35 C36 C31 119.8(5) . . ? O37A C37 O37B 122.1(4) . . ? O37A C37 C31 118.6(4) . . ? O37B C37 C31 119.3(4) . . ? O37A C37 Pr1 58.0(2) . . ? O37B C37 Pr1 64.3(2) . . ? C31 C37 Pr1 175.1(3) . . ? N41 C42 C43 124.7(8) . . ? C42 C43 C44 119.3(8) . . ? C43 C44 C45 117.4(7) . . ? C43 C44 C47 116.7(8) . . ? C45 C44 C47 125.9(8) . . ? C46 C45 C44 117.9(8) . . ? N41 C46 C45 124.6(8) . . ? C47 C47 C44 120.9(12) 2_667 . ? C37 O37A Pr1 97.8(3) . . ? C37 O37B Pr1 145.9(3) . 2_666 ? C37 O37B Pr1 90.6(3) . . ? Pr1 O37B Pr1 104.04(13) 2_666 . ? C27 O27A Pr1 148.0(3) . . ? C27 O27B Pr1 155.0(3) . 2_566 ? O13B N13 O13A 119.6(8) . . ? O13B N13 C13 127.7(9) . . ? O13A N13 C13 112.7(8) . . ? O15B N15 O15A 123.0(7) . . ? O15B N15 C15 119.3(7) . . ? O15A N15 C15 117.7(6) . . ? O23B N23 O23A 124.3(5) . . ? O23B N23 C23 117.9(5) . . ? O23A N23 C23 117.8(5) . . ? O25A N25 O25B 125.7(5) . . ? O25A N25 C25 118.2(5) . . ? O25B N25 C25 116.1(5) . . ? O33A N33 O33B 124.6(5) . . ? O33A N33 C33 116.9(5) . . ? O33B N33 C33 118.3(5) . . ? O35B N35 O35A 124.8(5) . . ? O35B N35 C35 116.5(5) . . ? O35A N35 C35 118.8(5) . . ? C46 N41 C42 116.0(7) . . ? C17 O17A Pr1 138.1(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.35 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.712 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.079 data_4 _database_code_depnum_ccdc_archive 'CCDC 233741' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetraacqua-hemi-(1,2-bis(4-pyridyl)ethane)-tris-3,5-dinitro-4-methyl benzoato Praseodymium(III) complex ; _chemical_name_common ; Tetraacqua-hemi-(1,2-bis(4-pyridyl)ethane)-tris-3,5-dinitro-4- methyl benzoato Praseodymium(iii) complex ; _chemical_melting_point ? _chemical_formula_moiety '[Pr(C8H5N2O6)3(H2O)2].0.5(C12H12N2).2(H2O)' _chemical_formula_sum 'C30 H29 N7 O22 Pr' _chemical_formula_weight 980.51 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.517(2) _cell_length_b 12.747(2) _cell_length_c 16.366(3) _cell_angle_alpha 72.21(2) _cell_angle_beta 78.98(3) _cell_angle_gamma 79.84(2) _cell_volume 1840.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 986 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 CCD-Area detector' _diffrn_measurement_method SMART _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11563 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 23.27 _reflns_number_total 5293 _reflns_number_gt 5016 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINTPLUS _computing_structure_solution 'SHELXTL (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL (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^)+(0.0489P)^2^+1.2062P] 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 5293 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.220226(18) 0.468436(14) 0.493668(11) 0.02488(9) Uani 1 1 d . . . C11 C -0.0413(4) 0.3428(3) 0.7762(2) 0.0311(8) Uani 1 1 d . . . C12 C 0.0769(4) 0.2846(3) 0.8143(2) 0.0378(9) Uani 1 1 d . . . H12 H 0.1679 0.2816 0.7813 0.045 Uiso 1 1 calc R . . C13 C 0.0588(5) 0.2310(3) 0.9018(3) 0.0449(11) Uani 1 1 d . . . C14 C -0.0715(5) 0.2294(4) 0.9559(3) 0.0513(11) Uani 1 1 d . . . C15 C -0.1866(5) 0.2917(4) 0.9151(3) 0.0436(10) Uani 1 1 d . . . C16 C -0.1736(4) 0.3463(3) 0.8273(2) 0.0370(9) Uani 1 1 d . . . H16 H -0.2547 0.3855 0.8028 0.044 Uiso 1 1 calc R . . C17 C -0.0249(4) 0.4024(3) 0.6811(2) 0.0300(8) Uani 1 1 d . . . C18 C -0.0869(7) 0.1607(5) 1.0498(3) 0.0862(19) Uani 1 1 d . . . H18C H -0.0121 0.0987 1.0571 0.129 Uiso 1 1 calc R . . H18B H -0.1794 0.1341 1.0662 0.129 Uiso 1 1 calc R . . H18A H -0.0788 0.2057 1.0858 0.129 Uiso 1 1 calc R . . C21 C 0.5330(4) 0.2263(3) 0.6626(2) 0.0281(8) Uani 1 1 d . . . C22 C 0.6372(4) 0.2008(3) 0.7174(2) 0.0316(8) Uani 1 1 d . . . H22 H 0.7060 0.2481 0.7087 0.038 Uiso 1 1 calc R . . C23 C 0.6368(4) 0.1043(3) 0.7845(2) 0.0335(9) Uani 1 1 d . . . C24 C 0.5417(4) 0.0267(3) 0.8016(2) 0.0347(9) Uani 1 1 d . . . C25 C 0.4427(4) 0.0565(3) 0.7430(2) 0.0341(9) Uani 1 1 d . . . C26 C 0.4339(4) 0.1535(3) 0.6761(2) 0.0321(8) Uani 1 1 d . . . H26 H 0.3626 0.1694 0.6409 0.039 Uiso 1 1 calc R . . C27 C 0.5300(4) 0.3329(3) 0.5908(2) 0.0290(8) Uani 1 1 d . . . C28 C 0.5431(5) -0.0765(3) 0.8767(3) 0.0511(11) Uani 1 1 d . . . H28C H 0.4871 -0.1271 0.8682 0.077 Uiso 1 1 calc R . . H28B H 0.5023 -0.0574 0.9294 0.077 Uiso 1 1 calc R . . H28A H 0.6406 -0.1111 0.8805 0.077 Uiso 1 1 calc R . . C31 C -0.0440(4) 0.1877(3) 0.5421(2) 0.0287(8) Uani 1 1 d . . . C32 C -0.1569(4) 0.1910(3) 0.4988(2) 0.0319(8) Uani 1 1 d . . . H32 H -0.1862 0.2554 0.4572 0.038 Uiso 1 1 calc R . . C33 C -0.2258(4) 0.0973(3) 0.5181(2) 0.0326(8) Uani 1 1 d . . . C34 C -0.1966(4) 0.0007(3) 0.5831(2) 0.0325(8) Uani 1 1 d . . . C35 C -0.0834(4) 0.0040(3) 0.6249(2) 0.0335(9) Uani 1 1 d . . . C36 C -0.0056(4) 0.0917(3) 0.6045(2) 0.0326(8) Uani 1 1 d . . . H36 H 0.0726 0.0864 0.6327 0.039 Uiso 1 1 calc R . . C37 C 0.0398(4) 0.2842(3) 0.5207(2) 0.0300(8) Uani 1 1 d . . . C38 C -0.2781(5) -0.0982(3) 0.6082(3) 0.0468(10) Uani 1 1 d . . . H38C H -0.2484 -0.1386 0.5657 0.070 Uiso 1 1 calc R . . H38B H -0.3797 -0.0734 0.6110 0.070 Uiso 1 1 calc R . . H38A H -0.2580 -0.1456 0.6639 0.070 Uiso 1 1 calc R . . C62 C 0.3210(7) 0.3814(5) 1.1612(4) 0.0772(16) Uani 1 1 d . . . H62 H 0.4211 0.3728 1.1560 0.093 Uiso 1 1 calc R . . H63 H 0.3183 0.4121 1.0328 0.093 Uiso 1 1 d R . . H65 H -0.0665 0.4152 1.1808 0.093 Uiso 1 1 d R . . H66 H 0.0505 0.3730 1.2986 0.093 Uiso 1 1 d R . . C63 C 0.2592(8) 0.4053(5) 1.0868(4) 0.0867(19) Uani 1 1 d . . . C64 C 0.1113(8) 0.4201(4) 1.0922(4) 0.0775(18) Uani 1 1 d . . . C65 C 0.0329(7) 0.4062(4) 1.1733(4) 0.0748(16) Uani 1 1 d . . . C66 C 0.1048(7) 0.3815(4) 1.2442(3) 0.0690(15) Uani 1 1 d . . . C67 C 0.0386(11) 0.4499(6) 1.0112(5) 0.135(3) Uani 1 1 d . . . N13 N 0.1920(6) 0.1747(4) 0.9366(3) 0.0762(14) Uani 1 1 d . . . N15 N -0.3309(5) 0.3068(4) 0.9647(3) 0.0674(12) Uani 1 1 d . . . N23 N 0.7473(4) 0.0869(3) 0.8416(2) 0.0474(9) Uani 1 1 d . . . N25 N 0.3351(4) -0.0189(3) 0.7526(2) 0.0478(9) Uani 1 1 d . . . N33 N -0.3354(3) 0.1042(3) 0.4630(2) 0.0417(8) Uani 1 1 d . . . N35 N -0.0410(4) -0.0942(3) 0.6969(2) 0.0402(8) Uani 1 1 d . . . N61 N 0.2461(6) 0.3701(3) 1.2391(3) 0.0660(12) Uani 1 1 d . . . O17A O -0.1389(3) 0.4386(2) 0.64843(16) 0.0399(6) Uani 1 1 d . . . O17B O 0.1008(3) 0.4102(2) 0.64201(16) 0.0373(6) Uani 1 1 d . . . O27A O 0.6219(3) 0.3942(2) 0.58427(17) 0.0439(7) Uani 1 1 d . . . O27B O 0.4356(3) 0.3536(2) 0.54231(16) 0.0342(6) Uani 1 1 d . . . O37A O -0.0199(3) 0.38230(19) 0.48834(16) 0.0330(6) Uani 1 1 d . . . O37B O 0.1669(3) 0.2660(2) 0.53537(19) 0.0431(7) Uani 1 1 d . . . O5 O 0.3101(3) 0.5532(2) 0.59833(19) 0.0468(7) Uani 1 1 d . . . O51 O 0.3606(3) 0.3765(2) 0.37902(17) 0.0467(7) Uani 1 1 d . . . O92 O 0.3205(10) -0.3424(7) 0.7747(7) 0.228(4) Uani 1 1 d . . . O93 O -0.6320(9) 0.4466(6) 0.7736(5) 0.179(3) Uani 1 1 d . . . O13A O 0.2689(6) 0.1167(6) 0.9076(3) 0.166(3) Uani 1 1 d . . . O13B O 0.2121(7) 0.2005(5) 1.0005(4) 0.161(3) Uani 1 1 d . . . O15A O -0.4343(4) 0.3142(5) 0.9287(3) 0.1095(17) Uani 1 1 d . . . O15B O -0.3406(5) 0.3120(4) 1.0380(3) 0.1028(15) Uani 1 1 d . . . O23A O 0.7081(5) 0.0662(4) 0.9191(2) 0.0854(13) Uani 1 1 d . . . O23B O 0.8706(3) 0.0975(3) 0.8071(2) 0.0625(9) Uani 1 1 d . . . O25A O 0.3773(4) -0.1161(3) 0.7591(2) 0.0722(10) Uani 1 1 d . . . O25B O 0.2093(4) 0.0227(3) 0.7528(2) 0.0664(10) Uani 1 1 d . . . O33A O -0.4071(4) 0.1928(3) 0.4389(3) 0.0782(12) Uani 1 1 d . . . O33B O -0.3449(4) 0.0220(3) 0.4426(2) 0.0574(8) Uani 1 1 d . . . O35A O -0.1259(4) -0.1168(3) 0.7630(2) 0.0677(10) Uani 1 1 d . . . O35B O 0.0768(4) -0.1449(3) 0.6850(2) 0.0638(9) 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 Pr1 0.02094(13) 0.02461(13) 0.02689(13) 0.00054(9) -0.00731(8) -0.00692(8) C11 0.034(2) 0.031(2) 0.0294(19) -0.0046(16) -0.0071(17) -0.0092(16) C12 0.036(2) 0.041(2) 0.035(2) -0.0069(18) -0.0084(18) -0.0053(18) C13 0.053(3) 0.042(2) 0.038(2) 0.0000(19) -0.022(2) -0.005(2) C14 0.066(3) 0.050(3) 0.034(2) 0.001(2) -0.010(2) -0.018(2) C15 0.044(2) 0.050(3) 0.034(2) -0.0079(19) 0.0028(19) -0.017(2) C16 0.037(2) 0.037(2) 0.037(2) -0.0071(17) -0.0063(18) -0.0095(17) C17 0.035(2) 0.0265(19) 0.0281(19) -0.0025(15) -0.0097(17) -0.0076(16) C18 0.115(5) 0.089(4) 0.036(3) 0.014(3) -0.011(3) -0.019(4) C21 0.0252(19) 0.0281(19) 0.0284(19) -0.0028(15) -0.0039(15) -0.0054(15) C22 0.029(2) 0.031(2) 0.034(2) -0.0028(16) -0.0079(16) -0.0096(16) C23 0.032(2) 0.035(2) 0.032(2) -0.0023(17) -0.0139(16) -0.0043(17) C24 0.035(2) 0.031(2) 0.034(2) -0.0012(16) -0.0073(17) -0.0059(17) C25 0.032(2) 0.033(2) 0.036(2) -0.0020(17) -0.0068(17) -0.0123(17) C26 0.0275(19) 0.034(2) 0.033(2) -0.0005(16) -0.0102(16) -0.0092(16) C27 0.0263(19) 0.0262(19) 0.032(2) -0.0026(15) -0.0050(16) -0.0060(16) C28 0.057(3) 0.044(3) 0.045(3) 0.012(2) -0.019(2) -0.016(2) C31 0.0244(19) 0.0276(19) 0.035(2) -0.0072(16) -0.0050(15) -0.0066(15) C32 0.028(2) 0.029(2) 0.037(2) -0.0065(16) -0.0051(16) -0.0046(16) C33 0.0249(19) 0.035(2) 0.042(2) -0.0150(18) -0.0068(16) -0.0048(16) C34 0.030(2) 0.029(2) 0.041(2) -0.0121(17) -0.0033(17) -0.0075(16) C35 0.035(2) 0.028(2) 0.035(2) -0.0051(16) -0.0042(17) -0.0044(16) C36 0.028(2) 0.031(2) 0.040(2) -0.0075(17) -0.0085(17) -0.0069(16) C37 0.032(2) 0.028(2) 0.0295(19) -0.0063(16) -0.0030(16) -0.0073(16) C38 0.050(3) 0.038(2) 0.057(3) -0.008(2) -0.011(2) -0.019(2) C62 0.085(4) 0.077(4) 0.075(4) -0.031(3) -0.030(3) 0.012(3) C63 0.116(5) 0.081(4) 0.063(4) -0.030(3) -0.028(4) 0.023(4) C64 0.116(5) 0.057(3) 0.071(4) -0.027(3) -0.048(4) 0.013(3) C65 0.090(4) 0.059(3) 0.087(4) -0.023(3) -0.034(4) -0.011(3) C66 0.099(5) 0.048(3) 0.063(3) -0.011(2) -0.026(3) -0.010(3) C67 0.199(9) 0.117(6) 0.109(5) -0.054(5) -0.114(6) 0.062(6) N13 0.082(4) 0.087(3) 0.046(3) 0.007(2) -0.034(3) 0.005(3) N15 0.061(3) 0.080(3) 0.048(3) -0.006(2) 0.013(2) -0.020(2) N23 0.057(3) 0.039(2) 0.047(2) 0.0012(17) -0.0285(19) -0.0114(18) N25 0.051(2) 0.050(2) 0.038(2) 0.0092(17) -0.0142(17) -0.0271(19) N33 0.0339(19) 0.042(2) 0.054(2) -0.0154(17) -0.0132(16) -0.0076(16) N35 0.048(2) 0.0271(18) 0.045(2) -0.0042(15) -0.0112(18) -0.0102(16) N61 0.093(4) 0.050(2) 0.060(3) -0.018(2) -0.034(3) 0.005(2) O17A 0.0336(15) 0.0505(17) 0.0313(14) -0.0011(12) -0.0115(12) -0.0059(13) O17B 0.0315(15) 0.0460(16) 0.0288(14) 0.0002(12) -0.0051(12) -0.0088(12) O27A 0.0440(16) 0.0359(15) 0.0473(16) 0.0114(12) -0.0188(13) -0.0214(13) O27B 0.0299(14) 0.0316(14) 0.0392(14) 0.0025(11) -0.0175(12) -0.0074(11) O37A 0.0340(14) 0.0248(14) 0.0394(14) -0.0030(11) -0.0111(12) -0.0066(11) O37B 0.0272(15) 0.0320(15) 0.069(2) -0.0059(13) -0.0152(13) -0.0077(12) O5 0.0427(16) 0.0432(16) 0.0596(18) -0.0153(14) -0.0145(14) -0.0095(13) O51 0.0512(18) 0.0471(17) 0.0416(16) -0.0137(13) -0.0144(14) 0.0045(14) O92 0.221(9) 0.175(7) 0.290(11) -0.027(7) -0.077(8) -0.052(7) O93 0.224(8) 0.172(6) 0.167(6) -0.053(5) -0.095(6) -0.006(6) O13A 0.119(4) 0.270(8) 0.078(3) -0.071(4) -0.042(3) 0.124(5) O13B 0.183(6) 0.155(5) 0.172(6) -0.059(5) -0.138(5) 0.053(4) O15A 0.051(3) 0.175(5) 0.084(3) -0.020(3) 0.012(2) -0.020(3) O15B 0.100(3) 0.143(4) 0.053(3) -0.029(3) 0.028(2) -0.022(3) O23A 0.106(3) 0.114(3) 0.040(2) 0.008(2) -0.032(2) -0.053(3) O23B 0.0380(19) 0.072(2) 0.084(2) -0.0209(19) -0.0280(18) -0.0068(16) O25A 0.093(3) 0.039(2) 0.087(3) 0.0013(17) -0.029(2) -0.0289(19) O25B 0.046(2) 0.079(2) 0.071(2) 0.0040(18) -0.0194(17) -0.0313(18) O33A 0.067(2) 0.059(2) 0.128(3) -0.038(2) -0.067(2) 0.0182(19) O33B 0.065(2) 0.0517(19) 0.069(2) -0.0211(17) -0.0261(17) -0.0173(16) O35A 0.084(3) 0.052(2) 0.048(2) 0.0059(16) 0.0052(19) -0.0089(18) O35B 0.055(2) 0.0502(19) 0.069(2) 0.0026(16) -0.0143(17) 0.0077(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 Pr1 O27A 2.405(3) 2_666 ? Pr1 O27B 2.414(2) . ? Pr1 O17B 2.424(2) . ? Pr1 O17A 2.468(2) 2_566 ? Pr1 O37A 2.488(2) 2_566 ? Pr1 O51 2.552(3) . ? Pr1 O37B 2.577(3) . ? Pr1 O5 2.617(3) . ? Pr1 O37A 2.730(2) . ? Pr1 C37 3.026(4) . ? Pr1 Pr1 4.1038(9) 2_566 ? C11 C16 1.374(5) . ? C11 C12 1.377(5) . ? C11 C17 1.500(5) . ? C12 C13 1.377(6) . ? C13 C14 1.379(6) . ? C13 N13 1.467(6) . ? C14 C15 1.387(6) . ? C14 C18 1.512(6) . ? C15 C16 1.385(6) . ? C15 N15 1.468(6) . ? C17 O17B 1.250(4) . ? C17 O17A 1.253(4) . ? C21 C26 1.380(5) . ? C21 C22 1.393(5) . ? C21 C27 1.500(5) . ? C22 C23 1.376(5) . ? C23 C24 1.388(5) . ? C23 N23 1.482(5) . ? C24 C25 1.396(5) . ? C24 C28 1.501(5) . ? C25 C26 1.380(5) . ? C25 N25 1.481(5) . ? C27 O27A 1.242(4) . ? C27 O27B 1.252(4) . ? C31 C36 1.377(5) . ? C31 C32 1.384(5) . ? C31 C37 1.499(5) . ? C32 C33 1.387(5) . ? C33 C34 1.384(5) . ? C33 N33 1.480(5) . ? C34 C35 1.395(5) . ? C34 C38 1.505(5) . ? C35 C36 1.370(5) . ? C35 N35 1.490(5) . ? C37 O37B 1.246(4) . ? C37 O37A 1.275(4) . ? C62 N61 1.316(7) . ? C62 C63 1.380(8) . ? C63 C64 1.376(9) . ? C64 C65 1.369(8) . ? C64 C67 1.527(7) . ? C65 C66 1.385(8) . ? C66 N61 1.315(7) . ? C67 C67 1.339(13) 2_567 ? N13 O13A 1.095(6) . ? N13 O13B 1.242(7) . ? N15 O15B 1.206(6) . ? N15 O15A 1.217(6) . ? N23 O23A 1.210(5) . ? N23 O23B 1.213(5) . ? N25 O25A 1.211(5) . ? N25 O25B 1.221(5) . ? N33 O33A 1.207(4) . ? N33 O33B 1.215(4) . ? N35 O35B 1.205(4) . ? N35 O35A 1.210(4) . ? O17A Pr1 2.468(2) 2_566 ? O27A Pr1 2.405(3) 2_666 ? O37A Pr1 2.488(2) 2_566 ? 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 O27A Pr1 O27B 85.34(9) 2_666 . ? O27A Pr1 O17B 134.54(9) 2_666 . ? O27B Pr1 O17B 87.78(8) . . ? O27A Pr1 O17A 72.67(9) 2_666 2_566 ? O27B Pr1 O17A 135.41(9) . 2_566 ? O17B Pr1 O17A 134.98(8) . 2_566 ? O27A Pr1 O37A 90.26(9) 2_666 2_566 ? O27B Pr1 O37A 148.49(8) . 2_566 ? O17B Pr1 O37A 73.30(8) . 2_566 ? O17A Pr1 O37A 71.54(8) 2_566 2_566 ? O27A Pr1 O51 80.27(10) 2_666 . ? O27B Pr1 O51 68.95(9) . . ? O17B Pr1 O51 137.47(9) . . ? O17A Pr1 O51 69.38(9) 2_566 . ? O37A Pr1 O51 140.86(8) 2_566 . ? O27A Pr1 O37B 148.87(10) 2_666 . ? O27B Pr1 O37B 73.80(8) . . ? O17B Pr1 O37B 68.59(9) . . ? O17A Pr1 O37B 106.44(9) 2_566 . ? O37A Pr1 O37B 119.51(8) 2_566 . ? O51 Pr1 O37B 70.86(9) . . ? O27A Pr1 O5 68.35(9) 2_666 . ? O27B Pr1 O5 71.52(9) . . ? O17B Pr1 O5 66.86(9) . . ? O17A Pr1 O5 129.58(9) 2_566 . ? O37A Pr1 O5 77.85(8) 2_566 . ? O51 Pr1 O5 130.78(9) . . ? O37B Pr1 O5 123.48(9) . . ? O27A Pr1 O37A 144.25(8) 2_666 . ? O27B Pr1 O37A 122.72(8) . . ? O17B Pr1 O37A 73.47(8) . . ? O17A Pr1 O37A 71.66(8) 2_566 . ? O37A Pr1 O37A 76.40(8) 2_566 . ? O51 Pr1 O37A 89.42(9) . . ? O37B Pr1 O37A 48.92(7) . . ? O5 Pr1 O37A 137.37(8) . . ? O27A Pr1 C37 157.29(10) 2_666 . ? O27B Pr1 C37 97.81(9) . . ? O17B Pr1 C37 68.16(9) . . ? O17A Pr1 C37 89.94(9) 2_566 . ? O37A Pr1 C37 98.11(9) 2_566 . ? O51 Pr1 C37 79.95(10) . . ? O37B Pr1 C37 24.03(9) . . ? O5 Pr1 C37 134.02(9) . . ? O37A Pr1 C37 24.92(8) . . ? O27A Pr1 Pr1 122.87(6) 2_666 2_566 ? O27B Pr1 Pr1 151.22(6) . 2_566 ? O17B Pr1 Pr1 68.68(6) . 2_566 ? O17A Pr1 Pr1 66.34(6) 2_566 2_566 ? O37A Pr1 Pr1 40.29(5) 2_566 2_566 ? O51 Pr1 Pr1 117.61(6) . 2_566 ? O37B Pr1 Pr1 82.03(6) . 2_566 ? O5 Pr1 Pr1 111.22(6) . 2_566 ? O37A Pr1 Pr1 36.10(5) . 2_566 ? C37 Pr1 Pr1 58.81(7) . 2_566 ? C16 C11 C12 118.6(3) . . ? C16 C11 C17 120.9(3) . . ? C12 C11 C17 120.4(3) . . ? C11 C12 C13 119.2(4) . . ? C12 C13 C14 124.8(4) . . ? C12 C13 N13 115.0(4) . . ? C14 C13 N13 120.2(4) . . ? C13 C14 C15 113.9(4) . . ? C13 C14 C18 122.4(4) . . ? C15 C14 C18 123.7(5) . . ? C16 C15 C14 123.3(4) . . ? C16 C15 N15 115.7(4) . . ? C14 C15 N15 121.0(4) . . ? C11 C16 C15 120.2(4) . . ? O17B C17 O17A 126.3(3) . . ? O17B C17 C11 117.0(3) . . ? O17A C17 C11 116.7(3) . . ? C26 C21 C22 119.2(3) . . ? C26 C21 C27 121.4(3) . . ? C22 C21 C27 119.3(3) . . ? C23 C22 C21 118.9(3) . . ? C22 C23 C24 125.1(3) . . ? C22 C23 N23 115.0(3) . . ? C24 C23 N23 119.9(3) . . ? C23 C24 C25 112.8(3) . . ? C23 C24 C28 123.4(3) . . ? C25 C24 C28 123.8(4) . . ? C26 C25 C24 125.2(3) . . ? C26 C25 N25 115.9(3) . . ? C24 C25 N25 118.9(3) . . ? C21 C26 C25 118.7(3) . . ? O27A C27 O27B 124.9(3) . . ? O27A C27 C21 117.0(3) . . ? O27B C27 C21 118.0(3) . . ? C36 C31 C32 118.7(3) . . ? C36 C31 C37 119.6(3) . . ? C32 C31 C37 121.7(3) . . ? C31 C32 C33 119.2(3) . . ? C34 C33 C32 124.4(3) . . ? C34 C33 N33 119.9(3) . . ? C32 C33 N33 115.7(3) . . ? C33 C34 C35 113.0(3) . . ? C33 C34 C38 124.5(3) . . ? C35 C34 C38 122.5(3) . . ? C36 C35 C34 124.8(3) . . ? C36 C35 N35 116.4(3) . . ? C34 C35 N35 118.8(3) . . ? C35 C36 C31 119.6(3) . . ? O37B C37 O37A 121.6(3) . . ? O37B C37 C31 118.6(3) . . ? O37A C37 C31 119.7(3) . . ? O37B C37 Pr1 57.31(18) . . ? O37A C37 Pr1 64.44(18) . . ? C31 C37 Pr1 174.5(2) . . ? N61 C62 C63 123.6(6) . . ? C64 C63 C62 119.6(6) . . ? C65 C64 C63 117.0(5) . . ? C65 C64 C67 121.8(7) . . ? C63 C64 C67 121.2(7) . . ? C64 C65 C66 119.1(6) . . ? N61 C66 C65 124.1(6) . . ? C67 C67 C64 117.6(8) 2_567 . ? O13A N13 O13B 122.8(6) . . ? O13A N13 C13 122.7(5) . . ? O13B N13 C13 114.4(5) . . ? O15B N15 O15A 123.7(5) . . ? O15B N15 C15 118.7(5) . . ? O15A N15 C15 117.5(4) . . ? O23A N23 O23B 124.5(4) . . ? O23A N23 C23 118.1(4) . . ? O23B N23 C23 117.5(4) . . ? O25A N25 O25B 124.9(4) . . ? O25A N25 C25 118.4(4) . . ? O25B N25 C25 116.7(4) . . ? O33A N33 O33B 124.1(3) . . ? O33A N33 C33 117.4(3) . . ? O33B N33 C33 118.4(3) . . ? O35B N35 O35A 124.7(4) . . ? O35B N35 C35 117.1(3) . . ? O35A N35 C35 118.2(3) . . ? C66 N61 C62 116.6(5) . . ? C17 O17A Pr1 140.3(2) . 2_566 ? C17 O17B Pr1 138.0(2) . . ? C27 O27A Pr1 154.3(2) . 2_666 ? C27 O27B Pr1 147.9(2) . . ? C37 O37A Pr1 147.0(2) . 2_566 ? C37 O37A Pr1 90.6(2) . . ? Pr1 O37A Pr1 103.60(8) 2_566 . ? C37 O37B Pr1 98.7(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.743 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.078