# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Loiseau, Thierry' _publ_contact_author_email thierry.loiseau@ensc-lille.fr _publ_section_title ; Lanthanide-based 0D and 2D molecular assemblies with pyridazine-3,6-dicarboxylate linker ; _publ_author_name T.Loiseau # Attachment '- 1_Prdcp.cif' data_770963 _database_code_depnum_ccdc_archive 'CCDC 770963' #TrackingRef '- 1_Prdcp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; '2(Pr 3+). 3(C6 N2 O4 H2 2-). 4(H2 O); 3.5(H2 O)' ; _chemical_formula_sum 'C18 H21 N6 O19.5 Pr2' _chemical_formula_weight 915.2 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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5283(8) _cell_length_b 13.4817(12) _cell_length_c 20.5006(18) _cell_angle_alpha 90.00 _cell_angle_beta 102.016(4) _cell_angle_gamma 90.00 _cell_volume 2846.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9952 _cell_measurement_theta_min 2.558 _cell_measurement_theta_max 28.556 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 3.480 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.368 _exptl_absorpt_correction_T_max 0.603 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006), based on the method developped by R. Blessing, Acta Cryst. A, 51, 33 (1995) ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95040 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 33.73 _reflns_number_total 11292 _reflns_number_gt 9751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _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^)+(0.0465P)^2^+2.4520P] 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 11292 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.448313(10) 0.352781(8) 0.240859(5) 0.01255(3) Uani 1 1 d . . . Pr2 Pr 0.308783(11) 0.230949(9) 0.416513(6) 0.01565(4) Uani 1 1 d . . . O1B O 0.67905(17) 0.36064(15) 0.24731(10) 0.0284(4) Uani 1 1 d . . . O2B O 0.88138(18) 0.3031(2) 0.28074(11) 0.0413(6) Uani 1 1 d . . . O3B O 0.47471(18) 0.17157(17) 0.50954(9) 0.0297(4) Uani 1 1 d . . . N1B N 0.60567(18) 0.28189(15) 0.35372(10) 0.0175(3) Uani 1 1 d . . . N2B N 0.56407(18) 0.24270(15) 0.40551(10) 0.0178(3) Uani 1 1 d . . . C2B C 0.7301(2) 0.27231(19) 0.34985(12) 0.0212(4) Uani 1 1 d . . . C3B C 0.8207(3) 0.2225(2) 0.39829(15) 0.0335(6) Uani 1 1 d . . . H3B H 0.9072 0.2173 0.3949 0.040 Uiso 1 1 calc R . . C4B C 0.7780(2) 0.1817(2) 0.45100(14) 0.0315(6) Uani 1 1 d . . . H4B H 0.8341 0.1473 0.4844 0.038 Uiso 1 1 calc R . . C1B C 0.7674(2) 0.3161(2) 0.28742(13) 0.0250(5) Uani 1 1 d . . . C5B C 0.6474(2) 0.19364(18) 0.45269(11) 0.0197(4) Uani 1 1 d . . . O1H O 0.39818(18) 0.39011(16) 0.12169(9) 0.0290(4) Uani 1 1 d . . . O1C O 0.5061(2) 0.53111(13) 0.24396(10) 0.0298(4) Uani 1 1 d . . . O1A O 0.24221(19) 0.43946(17) 0.22274(10) 0.0347(5) Uani 1 1 d . . . C2A C 0.0504(2) 0.5308(2) 0.20066(13) 0.0253(5) Uani 1 1 d . . . C1A C 0.1589(2) 0.4766(2) 0.17673(13) 0.0278(5) Uani 1 1 d . . . O2A O 0.1602(3) 0.4745(2) 0.11691(11) 0.0551(8) Uani 1 1 d . . . O3H O 0.10608(19) 0.33709(17) 0.37758(11) 0.0341(4) Uani 1 1 d . . . O3C O 0.2955(2) 0.34258(15) 0.50590(10) 0.0314(4) Uani 1 1 d . . . O2H O 0.1682(3) 0.1458(2) 0.47901(12) 0.0484(7) Uani 1 1 d . . . O2C O 0.4804(2) 0.68595(13) 0.27718(11) 0.0329(4) Uani 1 1 d . . . O4C O 0.2779(3) 0.4925(2) 0.55014(13) 0.0594(8) Uani 1 1 d . . . C6C C 0.3024(3) 0.4362(2) 0.50728(14) 0.0308(6) Uani 1 1 d . . . C5C C 0.3466(3) 0.48405(19) 0.44839(13) 0.0255(5) Uani 1 1 d . . . C2C C 0.4290(2) 0.55791(18) 0.34388(12) 0.0223(4) Uani 1 1 d . . . C1C C 0.4767(2) 0.59436(17) 0.28323(13) 0.0217(4) Uani 1 1 d . . . N2C N 0.37771(19) 0.42276(15) 0.40291(10) 0.0193(4) Uani 1 1 d . . . N1C N 0.41906(19) 0.45998(14) 0.35019(10) 0.0184(3) Uani 1 1 d . . . N1A N -0.0349(2) 0.57995(17) 0.15389(11) 0.0261(4) Uani 1 1 d . . . N2A N -0.1263(2) 0.63467(16) 0.17316(11) 0.0225(4) Uani 1 1 d . . . C5A C -0.1336(2) 0.63983(19) 0.23693(12) 0.0227(5) Uani 1 1 d . . . O4H O 0.3911(2) 0.06495(15) 0.38049(11) 0.0334(4) Uani 1 1 d . . . C3C C 0.3949(4) 0.6247(2) 0.38922(18) 0.0405(7) Uani 1 1 d . . . H3C H 0.3999 0.6928 0.3832 0.049 Uiso 1 1 calc R . . C4C C 0.3538(4) 0.5862(2) 0.44287(18) 0.0433(8) Uani 1 1 d . . . H4C H 0.3311 0.6275 0.4749 0.052 Uiso 1 1 calc R . . C3A C 0.0449(3) 0.5318(2) 0.26762(14) 0.0348(7) Uani 1 1 d . . . H3A H 0.1041 0.4958 0.2987 0.042 Uiso 1 1 calc R . . C4A C -0.0508(3) 0.5878(2) 0.28707(14) 0.0351(7) Uani 1 1 d . . . H4A H -0.0594 0.5905 0.3313 0.042 Uiso 1 1 calc R . . C6A C -0.2374(2) 0.70861(19) 0.25134(12) 0.0223(4) Uani 1 1 d . . . O3A O -0.2496(2) 0.72452(17) 0.30873(9) 0.0324(5) Uani 1 1 d . . . O4B O 0.6658(2) 0.1022(2) 0.55238(12) 0.0429(6) Uani 1 1 d . . . C6B C 0.5925(2) 0.15118(19) 0.50963(12) 0.0230(5) Uani 1 1 d . . . O4A O -0.31055(17) 0.75064(14) 0.20025(8) 0.0211(3) Uani 1 1 d . . . O7H O 0.0628(3) 0.2619(3) 0.56645(15) 0.0621(8) Uani 1 1 d . . . O6H O 0.9739(4) 0.4057(4) 0.4659(2) 0.1049(15) Uani 1 1 d . . . O5H O 0.0359(7) 0.9911(6) 0.4859(3) 0.072(2) Uani 0.50 1 d P . . O8H O 0.8924(3) 0.3125(3) 0.14210(15) 0.0802(11) 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 0.01313(5) 0.00979(6) 0.01572(6) 0.00169(4) 0.00531(4) 0.00107(3) Pr2 0.01475(5) 0.01766(6) 0.01530(6) 0.00131(4) 0.00491(4) -0.00228(4) O1B 0.0171(7) 0.0367(11) 0.0320(10) 0.0151(8) 0.0066(7) 0.0005(7) O2B 0.0170(8) 0.0765(17) 0.0327(10) 0.0155(11) 0.0106(7) 0.0081(10) O3B 0.0225(8) 0.0473(12) 0.0207(8) 0.0104(8) 0.0079(7) 0.0037(8) N1B 0.0150(7) 0.0197(9) 0.0191(8) 0.0034(7) 0.0065(6) 0.0004(6) N2B 0.0164(8) 0.0197(9) 0.0180(8) 0.0031(7) 0.0052(7) 0.0002(6) C2B 0.0157(9) 0.0267(12) 0.0222(10) 0.0030(9) 0.0063(8) 0.0029(8) C3B 0.0187(10) 0.0494(18) 0.0335(14) 0.0134(12) 0.0082(10) 0.0110(11) C4B 0.0202(10) 0.0444(16) 0.0297(13) 0.0136(12) 0.0051(9) 0.0101(11) C1B 0.0166(9) 0.0346(14) 0.0246(11) 0.0056(10) 0.0062(8) -0.0002(9) C5B 0.0185(9) 0.0204(11) 0.0204(10) 0.0036(8) 0.0045(8) 0.0011(8) O1H 0.0297(9) 0.0408(11) 0.0176(8) 0.0017(8) 0.0072(7) 0.0078(8) O1C 0.0468(11) 0.0142(8) 0.0333(10) 0.0001(7) 0.0192(9) -0.0028(8) O1A 0.0260(9) 0.0455(12) 0.0319(10) 0.0033(9) 0.0047(8) 0.0216(9) C2A 0.0220(10) 0.0284(12) 0.0252(11) 0.0021(9) 0.0044(9) 0.0126(9) C1A 0.0233(10) 0.0320(13) 0.0289(12) 0.0030(10) 0.0072(9) 0.0149(10) O2A 0.0530(14) 0.087(2) 0.0278(11) 0.0092(12) 0.0134(10) 0.0461(14) O3H 0.0229(9) 0.0391(11) 0.0390(11) 0.0028(9) 0.0036(8) 0.0071(8) O3C 0.0436(11) 0.0312(10) 0.0228(9) -0.0032(7) 0.0144(8) -0.0063(8) O2H 0.0446(13) 0.0692(18) 0.0358(12) 0.0107(11) 0.0184(10) -0.0186(12) O2C 0.0460(11) 0.0105(8) 0.0438(12) 0.0023(7) 0.0129(9) -0.0040(7) O4C 0.101(2) 0.0462(15) 0.0439(14) -0.0180(12) 0.0453(15) -0.0066(15) C6C 0.0355(13) 0.0339(14) 0.0258(12) -0.0068(11) 0.0128(10) -0.0043(11) C5C 0.0319(12) 0.0220(12) 0.0242(11) -0.0067(9) 0.0099(9) -0.0012(9) C2C 0.0273(11) 0.0140(10) 0.0272(11) -0.0010(8) 0.0091(9) -0.0018(8) C1C 0.0257(10) 0.0124(9) 0.0270(11) 0.0008(8) 0.0054(9) -0.0035(8) N2C 0.0216(8) 0.0179(9) 0.0195(8) -0.0019(7) 0.0070(7) -0.0020(7) N1C 0.0220(8) 0.0138(8) 0.0205(8) -0.0010(7) 0.0068(7) -0.0013(7) N1A 0.0224(9) 0.0315(12) 0.0250(10) 0.0025(8) 0.0068(8) 0.0154(8) N2A 0.0202(8) 0.0255(10) 0.0225(9) 0.0019(8) 0.0062(7) 0.0110(7) C5A 0.0209(10) 0.0269(12) 0.0206(10) 0.0015(9) 0.0046(8) 0.0119(8) O4H 0.0427(11) 0.0204(9) 0.0402(11) 0.0001(8) 0.0160(9) 0.0040(8) C3C 0.067(2) 0.0127(11) 0.0484(18) -0.0076(11) 0.0279(16) -0.0032(12) C4C 0.072(2) 0.0207(13) 0.0439(18) -0.0136(12) 0.0278(16) -0.0013(14) C3A 0.0343(13) 0.0428(17) 0.0273(12) 0.0085(11) 0.0063(11) 0.0237(12) C4A 0.0374(14) 0.0468(17) 0.0217(11) 0.0056(11) 0.0071(10) 0.0241(13) C6A 0.0209(10) 0.0250(11) 0.0208(10) -0.0007(9) 0.0037(8) 0.0070(8) O3A 0.0336(10) 0.0454(12) 0.0188(8) -0.0004(8) 0.0064(7) 0.0173(9) O4B 0.0312(10) 0.0584(15) 0.0379(12) 0.0293(11) 0.0045(9) 0.0057(10) C6B 0.0227(10) 0.0264(12) 0.0201(10) 0.0044(9) 0.0045(8) -0.0016(8) O4A 0.0213(7) 0.0249(8) 0.0173(7) -0.0012(6) 0.0045(6) 0.0092(6) O7H 0.0481(16) 0.091(2) 0.0457(16) 0.0016(15) 0.0071(13) -0.0133(15) O6H 0.087(3) 0.133(4) 0.103(3) -0.030(3) 0.038(2) 0.024(3) O5H 0.079(6) 0.069(4) 0.059(5) 0.010(4) -0.005(3) -0.013(4) O8H 0.069(2) 0.131(3) 0.0461(17) 0.0120(19) 0.0255(15) 0.035(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O1B 2.4075(18) . ? Pr1 O2C 2.4238(18) 2_645 ? Pr1 O1A 2.4241(17) . ? Pr1 O1H 2.4420(18) . ? Pr1 O1C 2.4774(18) . ? Pr1 O4A 2.4873(17) 2_545 ? Pr1 N1B 2.7231(19) . ? Pr1 N1C 2.738(2) . ? Pr1 O3A 2.7413(19) 2_545 ? Pr1 C6A 2.980(2) 2_545 ? Pr2 O3C 2.398(2) . ? Pr2 O4A 2.4122(17) 2_545 ? Pr2 O2H 2.437(2) . ? Pr2 O3B 2.4377(18) . ? Pr2 O3H 2.555(2) . ? Pr2 O4H 2.564(2) . ? Pr2 N2A 2.699(2) 2_545 ? Pr2 N2C 2.716(2) . ? Pr2 N2B 2.7482(19) . ? O1B C1B 1.259(3) . ? O2B C1B 1.248(3) . ? O3B C6B 1.270(3) . ? N1B N2B 1.339(3) . ? N1B C2B 1.335(3) . ? N2B C5B 1.337(3) . ? C2B C3B 1.397(3) . ? C2B C1B 1.533(3) . ? C3B C4B 1.370(4) . ? C3B H3B 0.9300 . ? C4B C5B 1.392(3) . ? C4B H4B 0.9300 . ? C5B C6B 1.518(3) . ? O1C C1C 1.255(3) . ? O1A C1A 1.251(3) . ? C2A N1A 1.344(3) . ? C2A C3A 1.386(4) . ? C2A C1A 1.520(3) . ? C1A O2A 1.230(3) . ? O3C C6C 1.264(4) . ? O2C C1C 1.242(3) . ? O2C Pr1 2.4238(18) 2_655 ? O4C C6C 1.229(4) . ? C6C C5C 1.525(4) . ? C5C N2C 1.337(3) . ? C5C C4C 1.385(4) . ? C2C N1C 1.333(3) . ? C2C C3C 1.394(4) . ? C2C C1C 1.516(4) . ? N2C N1C 1.344(3) . ? N1A N2A 1.336(3) . ? N2A C5A 1.327(3) . ? N2A Pr2 2.6988(19) 2 ? C5A C4A 1.391(3) . ? C5A C6A 1.509(3) . ? C3C C4C 1.366(5) . ? C3C H3C 0.9300 . ? C4C H4C 0.9300 . ? C3A C4A 1.383(4) . ? C3A H3A 0.9300 . ? C4A H4A 0.9300 . ? C6A O3A 1.229(3) . ? C6A O4A 1.294(3) . ? C6A Pr1 2.980(2) 2 ? O3A Pr1 2.7413(19) 2 ? O4B C6B 1.232(3) . ? O4A Pr2 2.4122(17) 2 ? O4A Pr1 2.4873(17) 2 ? O5H O5H 1.070(14) 3_576 ? 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 O1B Pr1 O2C 73.03(7) . 2_645 ? O1B Pr1 O1A 147.99(7) . . ? O2C Pr1 O1A 136.04(8) 2_645 . ? O1B Pr1 O1H 92.94(6) . . ? O2C Pr1 O1H 92.75(7) 2_645 . ? O1A Pr1 O1H 75.36(7) . . ? O1B Pr1 O1C 73.53(7) . . ? O2C Pr1 O1C 145.31(7) 2_645 . ? O1A Pr1 O1C 75.12(8) . . ? O1H Pr1 O1C 80.01(7) . . ? O1B Pr1 O4A 132.95(6) . 2_545 ? O2C Pr1 O4A 77.93(7) 2_645 2_545 ? O1A Pr1 O4A 75.37(7) . 2_545 ? O1H Pr1 O4A 124.98(6) . 2_545 ? O1C Pr1 O4A 133.60(6) . 2_545 ? O1B Pr1 N1B 62.63(6) . . ? O2C Pr1 N1B 69.57(7) 2_645 . ? O1A Pr1 N1B 131.78(6) . . ? O1H Pr1 N1B 152.73(6) . . ? O1C Pr1 N1B 102.48(7) . . ? O4A Pr1 N1B 72.92(6) 2_545 . ? O1B Pr1 N1C 102.47(7) . . ? O2C Pr1 N1C 134.91(7) 2_645 . ? O1A Pr1 N1C 67.75(6) . . ? O1H Pr1 N1C 132.27(6) . . ? O1C Pr1 N1C 62.33(6) . . ? O4A Pr1 N1C 73.65(6) 2_545 . ? N1B Pr1 N1C 69.02(6) . . ? O1B Pr1 O3A 137.02(7) . 2_545 ? O2C Pr1 O3A 66.10(7) 2_645 2_545 ? O1A Pr1 O3A 69.97(8) . 2_545 ? O1H Pr1 O3A 76.68(6) . 2_545 ? O1C Pr1 O3A 141.80(7) . 2_545 ? O4A Pr1 O3A 49.74(6) 2_545 2_545 ? N1B Pr1 O3A 112.09(6) . 2_545 ? N1C Pr1 O3A 115.43(6) . 2_545 ? O1B Pr1 C6A 141.29(7) . 2_545 ? O2C Pr1 C6A 70.19(7) 2_645 2_545 ? O1A Pr1 C6A 70.69(8) . 2_545 ? O1H Pr1 C6A 100.36(7) . 2_545 ? O1C Pr1 C6A 144.40(7) . 2_545 ? O4A Pr1 C6A 25.40(6) 2_545 2_545 ? N1B Pr1 C6A 93.09(6) . 2_545 ? N1C Pr1 C6A 95.06(6) . 2_545 ? O3A Pr1 C6A 24.34(6) 2_545 2_545 ? O3C Pr2 O4A 134.67(7) . 2_545 ? O3C Pr2 O2H 75.83(8) . . ? O4A Pr2 O2H 134.79(8) 2_545 . ? O3C Pr2 O3B 75.80(7) . . ? O4A Pr2 O3B 131.31(6) 2_545 . ? O2H Pr2 O3B 81.30(8) . . ? O3C Pr2 O3H 73.10(7) . . ? O4A Pr2 O3H 78.86(7) 2_545 . ? O2H Pr2 O3H 82.47(9) . . ? O3B Pr2 O3H 147.58(7) . . ? O3C Pr2 O4H 147.69(7) . . ? O4A Pr2 O4H 74.77(7) 2_545 . ? O2H Pr2 O4H 91.09(8) . . ? O3B Pr2 O4H 73.05(7) . . ? O3H Pr2 O4H 135.19(7) . . ? O3C Pr2 N2A 132.52(7) . 2_545 ? O4A Pr2 N2A 61.87(6) 2_545 2_545 ? O2H Pr2 N2A 73.00(8) . 2_545 ? O3B Pr2 N2A 131.87(7) . 2_545 ? O3H Pr2 N2A 68.09(7) . 2_545 ? O4H Pr2 N2A 67.63(7) . 2_545 ? O3C Pr2 N2C 62.63(6) . . ? O4A Pr2 N2C 74.69(6) 2_545 . ? O2H Pr2 N2C 134.99(8) . . ? O3B Pr2 N2C 103.28(7) . . ? O3H Pr2 N2C 70.02(7) . . ? O4H Pr2 N2C 133.47(6) . . ? N2A Pr2 N2C 123.75(6) 2_545 . ? O3C Pr2 N2B 103.91(7) . . ? O4A Pr2 N2B 72.69(6) 2_545 . ? O2H Pr2 N2B 141.41(8) . . ? O3B Pr2 N2B 61.92(6) . . ? O3H Pr2 N2B 135.20(7) . . ? O4H Pr2 N2B 68.38(6) . . ? N2A Pr2 N2B 122.78(6) 2_545 . ? N2C Pr2 N2B 69.51(6) . . ? C1B O1B Pr1 127.96(16) . . ? C6B O3B Pr2 127.79(16) . . ? N2B N1B C2B 119.73(19) . . ? N2B N1B Pr1 124.81(13) . . ? C2B N1B Pr1 114.49(15) . . ? N1B N2B C5B 119.68(19) . . ? N1B N2B Pr2 125.10(13) . . ? C5B N2B Pr2 114.67(15) . . ? N1B C2B C3B 122.5(2) . . ? N1B C2B C1B 115.9(2) . . ? C3B C2B C1B 121.5(2) . . ? C4B C3B C2B 117.8(2) . . ? C4B C3B H3B 121.1 . . ? C2B C3B H3B 121.1 . . ? C3B C4B C5B 117.5(2) . . ? C3B C4B H4B 121.3 . . ? C5B C4B H4B 121.3 . . ? O2B C1B O1B 126.3(2) . . ? O2B C1B C2B 117.2(2) . . ? O1B C1B C2B 116.5(2) . . ? N2B C5B C4B 122.8(2) . . ? N2B C5B C6B 116.4(2) . . ? C4B C5B C6B 120.8(2) . . ? C1C O1C Pr1 125.73(16) . . ? C1A O1A Pr1 140.64(18) . . ? N1A C2A C3A 122.8(2) . . ? N1A C2A C1A 116.2(2) . . ? C3A C2A C1A 120.9(2) . . ? O2A C1A O1A 126.2(2) . . ? O2A C1A C2A 119.8(2) . . ? O1A C1A C2A 113.9(2) . . ? C6C O3C Pr2 129.15(18) . . ? C1C O2C Pr1 162.65(19) . 2_655 ? O4C C6C O3C 127.8(3) . . ? O4C C6C C5C 116.6(3) . . ? O3C C6C C5C 115.5(2) . . ? N2C C5C C4C 122.2(3) . . ? N2C C5C C6C 116.7(2) . . ? C4C C5C C6C 121.1(2) . . ? N1C C2C C3C 122.6(2) . . ? N1C C2C C1C 116.5(2) . . ? C3C C2C C1C 120.9(2) . . ? O2C C1C O1C 126.5(2) . . ? O2C C1C C2C 115.2(2) . . ? O1C C1C C2C 118.3(2) . . ? C5C N2C N1C 119.8(2) . . ? C5C N2C Pr2 114.05(16) . . ? N1C N2C Pr2 125.20(14) . . ? C2C N1C N2C 119.6(2) . . ? C2C N1C Pr1 114.76(16) . . ? N2C N1C Pr1 124.89(14) . . ? N2A N1A C2A 118.5(2) . . ? C5A N2A N1A 120.8(2) . . ? C5A N2A Pr2 117.85(15) . 2 ? N1A N2A Pr2 121.24(15) . 2 ? N2A C5A C4A 123.1(2) . . ? N2A C5A C6A 114.7(2) . . ? C4A C5A C6A 122.2(2) . . ? C4C C3C C2C 117.4(3) . . ? C4C C3C H3C 121.3 . . ? C2C C3C H3C 121.3 . . ? C3C C4C C5C 118.4(3) . . ? C3C C4C H4C 120.8 . . ? C5C C4C H4C 120.8 . . ? C4A C3A C2A 118.3(2) . . ? C4A C3A H3A 120.8 . . ? C2A C3A H3A 120.8 . . ? C3A C4A C5A 116.4(3) . . ? C3A C4A H4A 121.8 . . ? C5A C4A H4A 121.8 . . ? O3A C6A O4A 122.3(2) . . ? O3A C6A C5A 121.3(2) . . ? O4A C6A C5A 116.4(2) . . ? O3A C6A Pr1 66.86(13) . 2 ? O4A C6A Pr1 55.49(12) . 2 ? C5A C6A Pr1 171.73(17) . 2 ? C6A O3A Pr1 88.79(14) . 2 ? O4B C6B O3B 125.7(2) . . ? O4B C6B C5B 117.8(2) . . ? O3B C6B C5B 116.4(2) . . ? C6A O4A Pr2 128.94(15) . 2 ? C6A O4A Pr1 99.12(14) . 2 ? Pr2 O4A Pr1 131.94(7) 2 2 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 33.73 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.865 _refine_diff_density_min -1.571 _refine_diff_density_rms 0.414 # Attachment '- 2_Nddcp.cif' data_770964 _database_code_depnum_ccdc_archive 'CCDC 770964' #TrackingRef '- 2_Nddcp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; '2(Nd 3+). 3(C6 N2 O4 H2 2-). 4(H2 O); 3.5(H2 O)' ; _chemical_formula_sum 'C18 H21 N6 Nd2 O19.5' _chemical_formula_weight 921.86 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4836(5) _cell_length_b 13.4043(8) _cell_length_c 20.4238(13) _cell_angle_alpha 90.00 _cell_angle_beta 102.163(3) _cell_angle_gamma 90.00 _cell_volume 2805.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5856 _cell_measurement_theta_min 2.544 _cell_measurement_theta_max 24.264 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 3.758 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4486 _exptl_absorpt_correction_T_max 0.8892 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006), based on the method developped by R. Blessing, Acta Cryst. A, 51, 33 (1995).' ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82298 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.14 _reflns_number_total 5570 _reflns_number_gt 4395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0494P)^2^+6.6638P] 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 5570 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Nd1 Nd 0.44825(3) 0.35263(2) 0.241029(14) 0.01500(10) Uani 1 1 d . . . Nd2 Nd 0.30934(3) 0.23064(2) 0.416094(15) 0.01803(11) Uani 1 1 d . . . O1B O 0.6782(4) 0.3609(3) 0.2467(2) 0.0302(10) Uani 1 1 d . . . O2B O 0.8809(4) 0.3032(4) 0.2802(2) 0.0418(12) Uani 1 1 d . . . O3B O 0.4740(4) 0.1711(3) 0.5092(2) 0.0300(10) Uani 1 1 d . . . N1B N 0.6050(4) 0.2824(3) 0.3531(2) 0.0199(11) Uani 1 1 d . . . N2B N 0.5634(4) 0.2434(4) 0.4053(2) 0.0207(11) Uani 1 1 d . . . C2B C 0.7300(5) 0.2727(4) 0.3493(3) 0.0220(13) Uani 1 1 d . . . C3B C 0.8211(6) 0.2230(5) 0.3981(3) 0.0341(16) Uani 1 1 d . . . H3B H 0.9079 0.2177 0.3947 0.041 Uiso 1 1 calc R . . C4B C 0.7787(6) 0.1826(5) 0.4507(3) 0.0329(15) Uani 1 1 d . . . H4B H 0.8356 0.1486 0.4845 0.039 Uiso 1 1 calc R . . C1B C 0.7665(6) 0.3155(5) 0.2867(3) 0.0290(14) Uani 1 1 d . . . C5B C 0.6473(5) 0.1936(4) 0.4525(3) 0.0202(12) Uani 1 1 d . . . O1H O 0.3989(4) 0.3893(3) 0.1220(2) 0.0309(10) Uani 1 1 d . . . O1C O 0.5069(4) 0.5313(3) 0.2438(2) 0.0309(10) Uani 1 1 d . . . O1A O 0.2431(4) 0.4397(4) 0.2230(2) 0.0371(11) Uani 1 1 d . . . C2A C 0.0506(6) 0.5310(5) 0.2004(3) 0.0278(14) Uani 1 1 d . . . C1A C 0.1587(6) 0.4763(5) 0.1765(3) 0.0293(15) Uani 1 1 d . . . O2A O 0.1608(5) 0.4742(4) 0.1164(2) 0.0553(15) Uani 1 1 d . . . O3H O 0.1062(4) 0.3363(3) 0.3773(2) 0.0349(11) Uani 1 1 d . . . O3C O 0.2957(4) 0.3415(3) 0.5055(2) 0.0314(10) Uani 1 1 d . . . O2H O 0.1705(5) 0.1445(4) 0.4786(2) 0.0476(13) Uani 1 1 d . . . O2C O 0.4809(4) 0.6864(3) 0.2771(2) 0.0337(10) Uani 1 1 d . . . O4C O 0.2786(6) 0.4913(4) 0.5500(3) 0.0588(16) Uani 1 1 d . . . C6C C 0.3038(6) 0.4354(5) 0.5074(3) 0.0327(15) Uani 1 1 d . . . C5C C 0.3462(6) 0.4835(4) 0.4481(3) 0.0260(14) Uani 1 1 d . . . C2C C 0.4289(5) 0.5587(4) 0.3436(3) 0.0232(13) Uani 1 1 d . . . C1C C 0.4763(5) 0.5945(5) 0.2827(3) 0.0243(13) Uani 1 1 d . . . N2C N 0.3774(4) 0.4218(3) 0.4032(2) 0.0196(10) Uani 1 1 d . . . N1C N 0.4194(4) 0.4595(3) 0.3501(2) 0.0198(10) Uani 1 1 d . . . N1A N -0.0346(5) 0.5803(4) 0.1539(2) 0.0277(12) Uani 1 1 d . . . N2A N -0.1268(5) 0.6345(4) 0.1732(3) 0.0250(12) Uani 1 1 d . . . C5A C -0.1333(6) 0.6407(4) 0.2374(3) 0.0248(14) Uani 1 1 d . . . O4H O 0.3919(4) 0.0648(3) 0.3811(2) 0.0325(10) Uani 1 1 d . . . C3C C 0.3952(7) 0.6241(5) 0.3895(4) 0.0423(18) Uani 1 1 d . . . H3C H 0.4012 0.6927 0.3839 0.051 Uiso 1 1 calc R . . C4C C 0.3534(8) 0.5862(5) 0.4426(4) 0.0471(19) Uani 1 1 d . . . H4C H 0.3300 0.6279 0.4746 0.057 Uiso 1 1 calc R . . C3A C 0.0446(6) 0.5321(5) 0.2677(3) 0.0380(17) Uani 1 1 d . . . H3A H 0.1041 0.4961 0.2990 0.046 Uiso 1 1 calc R . . C4A C -0.0505(6) 0.5872(5) 0.2868(3) 0.0350(16) Uani 1 1 d . . . H4A H -0.0594 0.5888 0.3311 0.042 Uiso 1 1 calc R . . C6A C -0.2379(5) 0.7089(4) 0.2511(3) 0.0241(14) Uani 1 1 d . . . O3A O -0.2495(4) 0.7250(3) 0.3089(2) 0.0331(11) Uani 1 1 d . . . O4B O 0.6657(4) 0.1022(4) 0.5524(2) 0.0442(13) Uani 1 1 d . . . C6B C 0.5916(6) 0.1511(4) 0.5098(3) 0.0250(14) Uani 1 1 d . . . O4A O -0.3109(4) 0.7514(3) 0.20022(19) 0.0217(9) Uani 1 1 d . . . O7H O 0.0639(5) 0.2615(5) 0.5655(3) 0.0634(16) Uani 1 1 d . . . O6H O 0.9733(7) 0.4069(7) 0.4651(4) 0.112(3) Uani 1 1 d . . . O5H O 0.0361(16) 0.9901(14) 0.4856(7) 0.087(5) Uani 0.50 1 d P . . O8H O 0.8940(6) 0.3123(6) 0.1420(3) 0.080(2) 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 Nd1 0.01589(16) 0.01224(17) 0.01785(19) 0.00168(12) 0.00575(12) 0.00097(11) Nd2 0.01723(17) 0.02004(19) 0.01745(19) 0.00148(13) 0.00510(13) -0.00224(12) O1B 0.019(2) 0.039(3) 0.032(3) 0.012(2) 0.0060(19) 0.0005(18) O2B 0.019(2) 0.074(4) 0.034(3) 0.012(3) 0.0094(19) 0.006(2) O3B 0.022(2) 0.050(3) 0.019(2) 0.007(2) 0.0064(17) 0.0020(19) N1B 0.017(2) 0.022(3) 0.022(3) 0.001(2) 0.007(2) 0.0007(19) N2B 0.021(2) 0.024(3) 0.018(3) 0.002(2) 0.006(2) -0.001(2) C2B 0.020(3) 0.022(3) 0.026(3) -0.002(3) 0.008(3) -0.003(2) C3B 0.023(3) 0.050(4) 0.033(4) 0.011(3) 0.015(3) 0.009(3) C4B 0.021(3) 0.043(4) 0.035(4) 0.013(3) 0.007(3) 0.011(3) C1B 0.021(3) 0.033(4) 0.032(4) 0.006(3) 0.004(3) -0.002(3) C5B 0.024(3) 0.019(3) 0.018(3) 0.002(2) 0.005(2) 0.001(2) O1H 0.033(2) 0.042(3) 0.019(2) 0.005(2) 0.0074(18) 0.005(2) O1C 0.044(3) 0.018(2) 0.037(3) -0.004(2) 0.022(2) -0.0103(19) O1A 0.029(2) 0.050(3) 0.031(3) 0.004(2) 0.004(2) 0.019(2) C2A 0.028(3) 0.030(4) 0.026(4) 0.002(3) 0.006(3) 0.012(3) C1A 0.027(3) 0.027(3) 0.034(4) 0.003(3) 0.006(3) 0.012(3) O2A 0.053(3) 0.086(4) 0.029(3) 0.009(3) 0.012(2) 0.045(3) O3H 0.024(2) 0.042(3) 0.038(3) 0.003(2) 0.0045(19) 0.0017(19) O3C 0.043(3) 0.032(3) 0.022(2) -0.0037(19) 0.015(2) -0.004(2) O2H 0.045(3) 0.064(4) 0.037(3) 0.012(2) 0.018(2) -0.015(2) O2C 0.046(3) 0.011(2) 0.045(3) 0.004(2) 0.012(2) -0.0025(19) O4C 0.097(5) 0.049(3) 0.043(3) -0.018(3) 0.042(3) -0.005(3) C6C 0.034(4) 0.037(4) 0.029(4) -0.005(3) 0.010(3) -0.003(3) C5C 0.027(3) 0.022(3) 0.029(4) -0.003(3) 0.008(3) -0.001(3) C2C 0.025(3) 0.017(3) 0.027(3) -0.004(3) 0.004(3) -0.002(2) C1C 0.021(3) 0.026(4) 0.026(3) -0.003(3) 0.005(2) -0.002(3) N2C 0.023(2) 0.018(3) 0.020(3) -0.003(2) 0.010(2) -0.0012(19) N1C 0.018(2) 0.017(3) 0.024(3) -0.002(2) 0.005(2) -0.0017(19) N1A 0.025(3) 0.035(3) 0.025(3) 0.001(2) 0.008(2) 0.013(2) N2A 0.020(3) 0.029(3) 0.027(3) 0.003(2) 0.007(2) 0.007(2) C5A 0.021(3) 0.028(3) 0.026(4) 0.003(3) 0.007(3) 0.006(2) O4H 0.042(3) 0.021(2) 0.038(3) -0.001(2) 0.016(2) 0.0003(19) C3C 0.061(5) 0.016(3) 0.055(5) -0.004(3) 0.024(4) 0.000(3) C4C 0.073(5) 0.032(4) 0.046(5) -0.015(4) 0.032(4) -0.001(4) C3A 0.035(4) 0.044(4) 0.036(4) 0.012(3) 0.010(3) 0.020(3) C4A 0.033(4) 0.047(4) 0.025(4) 0.005(3) 0.007(3) 0.019(3) C6A 0.021(3) 0.022(3) 0.029(4) -0.002(3) 0.005(3) 0.003(2) O3A 0.032(2) 0.044(3) 0.023(3) -0.005(2) 0.0060(19) 0.014(2) O4B 0.030(2) 0.059(3) 0.043(3) 0.030(3) 0.005(2) 0.006(2) C6B 0.026(3) 0.024(3) 0.025(3) 0.001(3) 0.005(3) -0.003(3) O4A 0.021(2) 0.027(2) 0.016(2) 0.0001(17) 0.0036(17) 0.0103(17) O7H 0.055(4) 0.088(5) 0.047(4) -0.001(3) 0.011(3) -0.012(3) O6H 0.082(5) 0.141(7) 0.122(7) -0.042(6) 0.041(5) 0.020(5) O5H 0.112(16) 0.090(11) 0.052(11) 0.004(9) 0.003(8) -0.029(11) O8H 0.072(4) 0.125(6) 0.050(4) 0.015(4) 0.030(3) 0.037(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1B 2.391(4) . ? Nd1 O2C 2.401(4) 2_645 ? Nd1 O1A 2.406(4) . ? Nd1 O1H 2.427(4) . ? Nd1 O4A 2.466(4) 2_545 ? Nd1 O1C 2.470(4) . ? Nd1 N1B 2.692(5) . ? Nd1 N1C 2.719(5) . ? Nd1 O3A 2.723(4) 2_545 ? Nd1 C6A 2.958(6) 2_545 ? Nd2 O3C 2.381(4) . ? Nd2 O4A 2.395(4) 2_545 ? Nd2 O3B 2.418(4) . ? Nd2 O2H 2.422(4) . ? Nd2 O3H 2.541(4) . ? Nd2 O4H 2.542(4) . ? Nd2 N2A 2.679(5) 2_545 ? Nd2 N2C 2.688(5) . ? Nd2 N2B 2.724(5) . ? O1B C1B 1.255(7) . ? O2B C1B 1.246(7) . ? O3B C6B 1.259(7) . ? N1B C2B 1.335(7) . ? N1B N2B 1.340(6) . ? N2B C5B 1.337(7) . ? C2B C3B 1.395(9) . ? C2B C1B 1.523(8) . ? C3B C4B 1.359(9) . ? C3B H3B 0.9300 . ? C4B C5B 1.393(8) . ? C4B H4B 0.9300 . ? C5B C6B 1.525(8) . ? O1C C1C 1.248(7) . ? O1A C1A 1.254(7) . ? C2A N1A 1.334(7) . ? C2A C3A 1.389(9) . ? C2A C1A 1.514(8) . ? C1A O2A 1.233(8) . ? O3C C6C 1.262(8) . ? O2C C1C 1.239(7) . ? O2C Nd1 2.402(4) 2_655 ? O4C C6C 1.218(8) . ? C6C C5C 1.518(9) . ? C5C N2C 1.327(7) . ? C5C C4C 1.384(9) . ? C2C N1C 1.343(7) . ? C2C C3C 1.382(9) . ? C2C C1C 1.511(8) . ? N2C N1C 1.350(6) . ? N1A N2A 1.333(6) . ? N2A C5A 1.330(8) . ? N2A Nd2 2.679(5) 2 ? C5A C4A 1.384(8) . ? C5A C6A 1.499(8) . ? C3C C4C 1.353(10) . ? C3C H3C 0.9300 . ? C4C H4C 0.9300 . ? C3A C4A 1.361(9) . ? C3A H3A 0.9300 . ? C4A H4A 0.9300 . ? C6A O3A 1.231(7) . ? C6A O4A 1.288(7) . ? C6A Nd1 2.958(6) 2 ? O3A Nd1 2.723(4) 2 ? O4B C6B 1.227(7) . ? O4A Nd2 2.395(4) 2 ? O4A Nd1 2.466(4) 2 ? O5H O5H 1.08(3) 3_576 ? 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 O1B Nd1 O2C 73.08(15) . 2_645 ? O1B Nd1 O1A 147.60(15) . . ? O2C Nd1 O1A 136.22(16) 2_645 . ? O1B Nd1 O1H 92.23(14) . . ? O2C Nd1 O1H 92.37(15) 2_645 . ? O1A Nd1 O1H 75.73(14) . . ? O1B Nd1 O4A 133.45(13) . 2_545 ? O2C Nd1 O4A 78.21(14) 2_645 2_545 ? O1A Nd1 O4A 75.33(15) . 2_545 ? O1H Nd1 O4A 125.17(13) . 2_545 ? O1B Nd1 O1C 73.19(14) . . ? O2C Nd1 O1C 145.04(15) 2_645 . ? O1A Nd1 O1C 75.12(15) . . ? O1H Nd1 O1C 80.00(14) . . ? O4A Nd1 O1C 133.62(13) 2_545 . ? O1B Nd1 N1B 63.02(13) . . ? O2C Nd1 N1B 69.70(15) 2_645 . ? O1A Nd1 N1B 131.75(14) . . ? O1H Nd1 N1B 152.38(14) . . ? O4A Nd1 N1B 73.02(13) 2_545 . ? O1C Nd1 N1B 102.42(14) . . ? O1B Nd1 N1C 102.77(14) . . ? O2C Nd1 N1C 134.93(14) 2_645 . ? O1A Nd1 N1C 67.64(14) . . ? O1H Nd1 N1C 132.63(14) . . ? O4A Nd1 N1C 73.37(13) 2_545 . ? O1C Nd1 N1C 62.63(13) . . ? N1B Nd1 N1C 68.94(13) . . ? O1B Nd1 O3A 136.97(14) . 2_545 ? O2C Nd1 O3A 66.20(14) 2_645 2_545 ? O1A Nd1 O3A 70.06(15) . 2_545 ? O1H Nd1 O3A 76.53(14) . 2_545 ? O4A Nd1 O3A 50.04(12) 2_545 2_545 ? O1C Nd1 O3A 141.72(14) . 2_545 ? N1B Nd1 O3A 112.39(13) . 2_545 ? N1C Nd1 O3A 115.45(13) . 2_545 ? O1B Nd1 C6A 141.53(15) . 2_545 ? O2C Nd1 C6A 70.27(15) 2_645 2_545 ? O1A Nd1 C6A 70.84(16) . 2_545 ? O1H Nd1 C6A 100.50(16) . 2_545 ? O4A Nd1 C6A 25.45(15) 2_545 2_545 ? O1C Nd1 C6A 144.58(15) . 2_545 ? N1B Nd1 C6A 93.13(15) . 2_545 ? N1C Nd1 C6A 94.92(15) . 2_545 ? O3A Nd1 C6A 24.59(14) 2_545 2_545 ? O3C Nd2 O4A 134.57(14) . 2_545 ? O3C Nd2 O3B 75.60(15) . . ? O4A Nd2 O3B 131.70(13) 2_545 . ? O3C Nd2 O2H 75.72(16) . . ? O4A Nd2 O2H 135.15(15) 2_545 . ? O3B Nd2 O2H 80.61(15) . . ? O3C Nd2 O3H 73.12(15) . . ? O4A Nd2 O3H 78.83(14) 2_545 . ? O3B Nd2 O3H 147.30(14) . . ? O2H Nd2 O3H 82.69(16) . . ? O3C Nd2 O4H 147.15(15) . . ? O4A Nd2 O4H 75.47(14) 2_545 . ? O3B Nd2 O4H 72.76(14) . . ? O2H Nd2 O4H 90.55(16) . . ? O3H Nd2 O4H 135.43(14) . . ? O3C Nd2 N2A 132.24(15) . 2_545 ? O4A Nd2 N2A 62.25(14) 2_545 2_545 ? O3B Nd2 N2A 131.73(15) . 2_545 ? O2H Nd2 N2A 72.96(16) . 2_545 ? O3H Nd2 N2A 67.93(15) . 2_545 ? O4H Nd2 N2A 67.97(14) . 2_545 ? O3C Nd2 N2C 62.64(14) . . ? O4A Nd2 N2C 74.58(13) 2_545 . ? O3B Nd2 N2C 103.39(14) . . ? O2H Nd2 N2C 135.04(16) . . ? O3H Nd2 N2C 70.15(14) . . ? O4H Nd2 N2C 133.86(13) . . ? N2A Nd2 N2C 123.92(14) 2_545 . ? O3C Nd2 N2B 103.91(14) . . ? O4A Nd2 N2B 72.63(13) 2_545 . ? O3B Nd2 N2B 62.36(13) . . ? O2H Nd2 N2B 141.17(16) . . ? O3H Nd2 N2B 135.19(14) . . ? O4H Nd2 N2B 68.61(14) . . ? N2A Nd2 N2B 123.08(14) 2_545 . ? N2C Nd2 N2B 69.39(14) . . ? C1B O1B Nd1 127.4(4) . . ? C6B O3B Nd2 127.8(4) . . ? C2B N1B N2B 119.7(5) . . ? C2B N1B Nd1 114.5(4) . . ? N2B N1B Nd1 124.8(3) . . ? C5B N2B N1B 119.5(5) . . ? C5B N2B Nd2 114.6(4) . . ? N1B N2B Nd2 125.2(3) . . ? N1B C2B C3B 122.5(5) . . ? N1B C2B C1B 115.8(5) . . ? C3B C2B C1B 121.7(5) . . ? C4B C3B C2B 117.8(6) . . ? C4B C3B H3B 121.1 . . ? C2B C3B H3B 121.1 . . ? C3B C4B C5B 117.9(6) . . ? C3B C4B H4B 121.1 . . ? C5B C4B H4B 121.1 . . ? O2B C1B O1B 126.1(6) . . ? O2B C1B C2B 117.2(5) . . ? O1B C1B C2B 116.6(5) . . ? N2B C5B C4B 122.6(5) . . ? N2B C5B C6B 116.0(5) . . ? C4B C5B C6B 121.4(5) . . ? C1C O1C Nd1 125.2(4) . . ? C1A O1A Nd1 140.5(4) . . ? N1A C2A C3A 122.4(5) . . ? N1A C2A C1A 116.3(5) . . ? C3A C2A C1A 121.2(5) . . ? O2A C1A O1A 126.0(6) . . ? O2A C1A C2A 120.3(5) . . ? O1A C1A C2A 113.6(6) . . ? C6C O3C Nd2 129.2(4) . . ? C1C O2C Nd1 162.9(4) . 2_655 ? O4C C6C O3C 127.8(6) . . ? O4C C6C C5C 116.9(6) . . ? O3C C6C C5C 115.3(5) . . ? N2C C5C C4C 122.5(6) . . ? N2C C5C C6C 116.4(5) . . ? C4C C5C C6C 121.1(6) . . ? N1C C2C C3C 121.8(6) . . ? N1C C2C C1C 116.1(5) . . ? C3C C2C C1C 122.1(5) . . ? O2C C1C O1C 126.5(6) . . ? O2C C1C C2C 114.7(5) . . ? O1C C1C C2C 118.7(5) . . ? C5C N2C N1C 119.5(5) . . ? C5C N2C Nd2 114.6(4) . . ? N1C N2C Nd2 125.0(3) . . ? C2C N1C N2C 119.6(5) . . ? C2C N1C Nd1 114.7(4) . . ? N2C N1C Nd1 124.9(3) . . ? N2A N1A C2A 118.6(5) . . ? C5A N2A N1A 121.1(5) . . ? C5A N2A Nd2 117.6(4) . 2 ? N1A N2A Nd2 121.3(4) . 2 ? N2A C5A C4A 122.1(5) . . ? N2A C5A C6A 114.5(5) . . ? C4A C5A C6A 123.4(6) . . ? C4C C3C C2C 118.5(6) . . ? C4C C3C H3C 120.7 . . ? C2C C3C H3C 120.7 . . ? C3C C4C C5C 118.1(6) . . ? C3C C4C H4C 121.0 . . ? C5C C4C H4C 121.0 . . ? C4A C3A C2A 118.6(6) . . ? C4A C3A H3A 120.7 . . ? C2A C3A H3A 120.7 . . ? C3A C4A C5A 117.2(6) . . ? C3A C4A H4A 121.4 . . ? C5A C4A H4A 121.4 . . ? O3A C6A O4A 122.3(5) . . ? O3A C6A C5A 120.7(5) . . ? O4A C6A C5A 116.9(5) . . ? O3A C6A Nd1 66.9(3) . 2 ? O4A C6A Nd1 55.4(3) . 2 ? C5A C6A Nd1 172.1(4) . 2 ? C6A O3A Nd1 88.5(3) . 2 ? O4B C6B O3B 126.4(6) . . ? O4B C6B C5B 117.1(5) . . ? O3B C6B C5B 116.5(5) . . ? C6A O4A Nd2 128.5(4) . 2 ? C6A O4A Nd1 99.2(3) . 2 ? Nd2 O4A Nd1 132.34(16) 2 2 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.14 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.134 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.252 # Attachment '- 3_Smdcp.cif' data_770965 _database_code_depnum_ccdc_archive 'CCDC 770965' #TrackingRef '- 3_Smdcp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; '2(Sm 3+). 3(C6 N2 O4 H2 2-). 4(H2 O); 3.5(H2 O)' ; _chemical_formula_sum 'C18 H21 N6 O19.5 Sm2' _chemical_formula_weight 934.08 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4555(19) _cell_length_b 13.333(3) _cell_length_c 20.372(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.245(10) _cell_angle_gamma 90.00 _cell_volume 2775.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 610 _cell_measurement_theta_min 2.511 _cell_measurement_theta_max 28.946 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 4.290 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3883 _exptl_absorpt_correction_T_max 0.8893 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006), based on the method developped by R. Blessing, Acta Cryst. A, 51, 33 (1995).' Rint is greater than 0.1, due to the high angle data collection, meaning that less defined intensities were taken into account for the space group choice. ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 194149 _diffrn_reflns_av_R_equivalents 0.1317 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 31.00 _reflns_number_total 8585 _reflns_number_gt 6130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _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^)+(0.0556P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8585 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Sm1 Sm 0.44814(2) 0.352418(17) 0.241400(11) 0.01552(7) Uani 1 1 d . . . Sm2 Sm 0.31028(2) 0.230183(18) 0.415185(12) 0.01841(7) Uani 1 1 d . . . O1B O 0.6755(3) 0.3611(3) 0.24530(18) 0.0301(8) Uani 1 1 d . . . O2B O 0.8802(4) 0.3053(4) 0.2796(2) 0.0425(11) Uani 1 1 d . . . O3B O 0.4724(4) 0.1727(3) 0.50866(17) 0.0312(9) Uani 1 1 d . . . N1B N 0.6042(4) 0.2828(3) 0.3521(2) 0.0210(8) Uani 1 1 d . . . N2B N 0.5624(4) 0.2433(3) 0.4043(2) 0.0215(8) Uani 1 1 d . . . C2B C 0.7299(5) 0.2732(4) 0.3489(2) 0.0237(10) Uani 1 1 d . . . C3B C 0.8206(6) 0.2243(5) 0.3972(3) 0.0349(13) Uani 1 1 d . . . H3B H 0.9076 0.2191 0.3937 0.042 Uiso 1 1 calc R . . C4B C 0.7782(5) 0.1837(5) 0.4503(3) 0.0345(13) Uani 1 1 d . . . H4B H 0.8354 0.1498 0.4843 0.041 Uiso 1 1 calc R . . C1B C 0.7658(5) 0.3173(4) 0.2861(3) 0.0261(10) Uani 1 1 d . . . C5B C 0.6469(5) 0.1947(4) 0.4519(2) 0.0218(10) Uani 1 1 d . . . O1H O 0.4008(4) 0.3870(3) 0.12359(17) 0.0292(8) Uani 1 1 d . . . O1C O 0.5058(4) 0.5306(3) 0.24334(18) 0.0317(9) Uani 1 1 d . . . O1A O 0.2451(4) 0.4394(3) 0.22334(19) 0.0348(9) Uani 1 1 d . . . C2A C 0.0526(5) 0.5308(4) 0.2012(3) 0.0275(11) Uani 1 1 d . . . C1A C 0.1608(5) 0.4761(4) 0.1773(3) 0.0289(11) Uani 1 1 d . . . O2A O 0.1623(5) 0.4746(4) 0.1169(2) 0.0570(14) Uani 1 1 d . . . O3H O 0.1081(4) 0.3353(3) 0.3771(2) 0.0337(9) Uani 1 1 d . . . O3C O 0.2950(4) 0.3393(3) 0.50482(18) 0.0317(9) Uani 1 1 d . . . O2H O 0.1735(4) 0.1441(4) 0.4773(2) 0.0463(12) Uani 1 1 d . . . O2C O 0.4834(4) 0.6866(3) 0.2775(2) 0.0344(9) Uani 1 1 d . . . O4C O 0.2783(6) 0.4898(4) 0.5504(2) 0.0576(14) Uani 1 1 d . . . C6C C 0.3028(6) 0.4330(4) 0.5073(3) 0.0321(12) Uani 1 1 d . . . C5C C 0.3483(5) 0.4824(4) 0.4484(3) 0.0267(11) Uani 1 1 d . . . C2C C 0.4303(5) 0.5576(4) 0.3435(3) 0.0245(10) Uani 1 1 d . . . C1C C 0.4774(5) 0.5939(4) 0.2829(3) 0.0224(10) Uani 1 1 d . . . N2C N 0.3783(4) 0.4204(3) 0.4027(2) 0.0218(8) Uani 1 1 d . . . N1C N 0.4202(4) 0.4586(3) 0.3496(2) 0.0207(8) Uani 1 1 d . . . N1A N -0.0352(4) 0.5793(3) 0.1539(2) 0.0286(10) Uani 1 1 d . . . N2A N -0.1273(4) 0.6343(3) 0.1734(2) 0.0258(9) Uani 1 1 d . . . C5A C -0.1336(5) 0.6403(4) 0.2374(3) 0.0251(10) Uani 1 1 d . . . O4H O 0.3916(4) 0.0658(3) 0.38101(19) 0.0321(9) Uani 1 1 d . . . C3C C 0.3965(7) 0.6245(4) 0.3889(3) 0.0427(16) Uani 1 1 d . . . H3C H 0.4024 0.6934 0.3830 0.051 Uiso 1 1 calc R . . C4C C 0.3536(7) 0.5855(4) 0.4433(3) 0.0438(16) Uani 1 1 d . . . H4C H 0.3292 0.6271 0.4752 0.053 Uiso 1 1 calc R . . C3A C 0.0466(6) 0.5329(5) 0.2691(3) 0.0387(14) Uani 1 1 d . . . H3A H 0.1069 0.4973 0.3007 0.046 Uiso 1 1 calc R . . C4A C -0.0485(5) 0.5876(5) 0.2880(3) 0.0349(13) Uani 1 1 d . . . H4A H -0.0568 0.5900 0.3325 0.042 Uiso 1 1 calc R . . C6A C -0.2382(5) 0.7095(4) 0.2514(3) 0.0231(10) Uani 1 1 d . . . O3A O -0.2500(4) 0.7253(3) 0.30909(18) 0.0338(9) Uani 1 1 d . . . O4B O 0.6651(4) 0.1030(4) 0.5526(2) 0.0441(11) Uani 1 1 d . . . C6B C 0.5906(5) 0.1517(4) 0.5097(3) 0.0266(11) Uani 1 1 d . . . O4A O -0.3124(3) 0.7515(3) 0.20020(17) 0.0225(7) Uani 1 1 d . . . O7H O 0.0645(5) 0.2622(5) 0.5640(3) 0.0635(15) Uani 1 1 d . . . O6H O 0.9750(7) 0.4100(6) 0.4635(4) 0.106(3) Uani 1 1 d . . . O5H O 0.0353(15) 0.9890(12) 0.4860(7) 0.080(5) Uani 0.50 1 d P . . O8H O 0.8945(6) 0.3106(6) 0.1411(3) 0.0797(19) 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 Sm1 0.01612(12) 0.01305(10) 0.01832(12) 0.00175(8) 0.00576(9) 0.00108(8) Sm2 0.01794(12) 0.02052(12) 0.01751(13) 0.00108(9) 0.00542(9) -0.00232(9) O1B 0.0196(18) 0.039(2) 0.032(2) 0.0138(16) 0.0062(15) -0.0012(15) O2B 0.022(2) 0.072(3) 0.037(2) 0.015(2) 0.0140(17) 0.008(2) O3B 0.025(2) 0.051(3) 0.0193(19) 0.0069(16) 0.0074(15) 0.0030(17) N1B 0.019(2) 0.025(2) 0.020(2) 0.0038(15) 0.0068(16) 0.0006(16) N2B 0.021(2) 0.024(2) 0.019(2) 0.0021(15) 0.0038(16) -0.0009(16) C2B 0.019(2) 0.030(3) 0.024(3) 0.001(2) 0.0078(19) -0.001(2) C3B 0.023(3) 0.047(4) 0.035(3) 0.010(3) 0.007(2) 0.006(2) C4B 0.019(3) 0.051(4) 0.033(3) 0.014(3) 0.006(2) 0.009(2) C1B 0.021(2) 0.032(3) 0.027(3) 0.004(2) 0.007(2) -0.002(2) C5B 0.020(2) 0.022(2) 0.023(3) 0.0023(18) 0.0053(19) 0.0023(19) O1H 0.030(2) 0.041(2) 0.0177(18) 0.0021(15) 0.0075(15) 0.0056(17) O1C 0.044(2) 0.0200(18) 0.037(2) 0.0001(15) 0.0207(18) -0.0055(16) O1A 0.029(2) 0.045(2) 0.030(2) 0.0028(17) 0.0061(16) 0.0189(18) C2A 0.024(3) 0.031(3) 0.028(3) 0.003(2) 0.006(2) 0.013(2) C1A 0.023(3) 0.032(3) 0.032(3) 0.002(2) 0.009(2) 0.012(2) O2A 0.053(3) 0.087(4) 0.034(3) 0.007(2) 0.015(2) 0.045(3) O3H 0.0219(19) 0.037(2) 0.042(2) 0.0023(17) 0.0066(17) 0.0066(16) O3C 0.042(2) 0.034(2) 0.0220(19) -0.0030(15) 0.0126(17) -0.0034(17) O2H 0.043(3) 0.066(3) 0.034(2) 0.011(2) 0.018(2) -0.014(2) O2C 0.044(2) 0.0158(17) 0.046(2) 0.0012(16) 0.0137(19) -0.0029(17) O4C 0.095(4) 0.047(3) 0.042(3) -0.018(2) 0.041(3) -0.008(3) C6C 0.037(3) 0.035(3) 0.027(3) -0.005(2) 0.012(2) -0.009(2) C5C 0.028(3) 0.024(3) 0.029(3) -0.005(2) 0.007(2) -0.003(2) C2C 0.026(3) 0.020(2) 0.029(3) -0.0047(19) 0.007(2) -0.003(2) C1C 0.018(2) 0.018(2) 0.031(3) 0.0004(18) 0.0050(19) -0.0054(18) N2C 0.026(2) 0.0167(19) 0.024(2) -0.0021(15) 0.0084(17) 0.0001(16) N1C 0.021(2) 0.0154(19) 0.026(2) -0.0013(15) 0.0054(17) -0.0012(15) N1A 0.025(2) 0.033(3) 0.028(2) 0.0009(18) 0.0070(18) 0.0127(19) N2A 0.024(2) 0.028(2) 0.026(2) 0.0026(17) 0.0066(18) 0.0085(17) C5A 0.023(3) 0.027(3) 0.025(3) 0.000(2) 0.005(2) 0.007(2) O4H 0.036(2) 0.0231(19) 0.039(2) -0.0009(16) 0.0119(18) 0.0015(16) C3C 0.071(5) 0.016(3) 0.049(4) -0.007(2) 0.030(3) -0.003(3) C4C 0.071(5) 0.025(3) 0.043(4) -0.016(2) 0.027(3) -0.003(3) C3A 0.038(3) 0.044(3) 0.034(3) 0.009(3) 0.009(3) 0.024(3) C4A 0.033(3) 0.045(4) 0.026(3) 0.003(2) 0.003(2) 0.020(3) C6A 0.019(2) 0.024(2) 0.025(3) -0.0006(18) 0.0037(19) 0.0043(19) O3A 0.033(2) 0.049(3) 0.0200(19) -0.0018(16) 0.0071(16) 0.0146(18) O4B 0.032(2) 0.060(3) 0.038(2) 0.029(2) 0.0025(18) 0.007(2) C6B 0.031(3) 0.028(3) 0.021(3) 0.003(2) 0.006(2) -0.002(2) O4A 0.0226(18) 0.0259(18) 0.0194(17) 0.0001(13) 0.0055(14) 0.0090(14) O7H 0.052(3) 0.089(4) 0.049(3) -0.005(3) 0.010(3) -0.015(3) O6H 0.088(5) 0.136(7) 0.101(6) -0.033(5) 0.038(4) 0.026(5) O5H 0.093(13) 0.082(9) 0.062(10) 0.007(7) 0.006(6) -0.029(9) O8H 0.069(4) 0.128(6) 0.049(3) 0.016(3) 0.028(3) 0.037(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1B 2.364(4) . ? Sm1 O1A 2.378(4) . ? Sm1 O2C 2.380(4) 2_645 ? Sm1 O1H 2.390(3) . ? Sm1 O4A 2.440(3) 2_545 ? Sm1 O1C 2.449(4) . ? Sm1 N1B 2.655(4) . ? Sm1 N1C 2.686(4) . ? Sm1 O3A 2.705(4) 2_545 ? Sm1 C6A 2.934(5) 2_545 ? Sm2 O3C 2.366(4) . ? Sm2 O4A 2.373(3) 2_545 ? Sm2 O3B 2.391(4) . ? Sm2 O2H 2.394(4) . ? Sm2 O4H 2.503(4) . ? Sm2 O3H 2.518(4) . ? Sm2 N2A 2.662(4) 2_545 ? Sm2 N2C 2.661(4) . ? Sm2 N2B 2.698(4) . ? O1B C1B 1.262(6) . ? O2B C1B 1.241(6) . ? O3B C6B 1.263(6) . ? N1B C2B 1.336(6) . ? N1B N2B 1.339(5) . ? N2B C5B 1.333(6) . ? C2B C3B 1.376(7) . ? C2B C1B 1.526(7) . ? C3B C4B 1.366(8) . ? C3B H3B 0.9300 . ? C4B C5B 1.388(7) . ? C4B H4B 0.9300 . ? C5B C6B 1.534(7) . ? O1C C1C 1.246(6) . ? O1A C1A 1.243(6) . ? C2A N1A 1.347(6) . ? C2A C3A 1.398(7) . ? C2A C1A 1.511(7) . ? C1A O2A 1.235(6) . ? O3C C6C 1.252(7) . ? O2C C1C 1.243(6) . ? O2C Sm1 2.380(4) 2_655 ? O4C C6C 1.227(6) . ? C6C C5C 1.531(7) . ? C5C N2C 1.331(6) . ? C5C C4C 1.380(8) . ? C2C N1C 1.331(6) . ? C2C C3C 1.385(7) . ? C2C C1C 1.503(7) . ? N2C N1C 1.351(5) . ? N1A N2A 1.336(6) . ? N2A C5A 1.323(6) . ? N2A Sm2 2.662(4) 2 ? C5A C4A 1.399(7) . ? C5A C6A 1.503(7) . ? C3C C4C 1.382(8) . ? C3C H3C 0.9300 . ? C4C H4C 0.9300 . ? C3A C4A 1.352(7) . ? C3A H3A 0.9300 . ? C4A H4A 0.9300 . ? C6A O3A 1.225(6) . ? C6A O4A 1.289(6) . ? C6A Sm1 2.934(5) 2 ? O3A Sm1 2.705(4) 2 ? O4B C6B 1.227(6) . ? O4A Sm2 2.373(3) 2 ? O4A Sm1 2.440(3) 2 ? O5H O5H 1.06(2) 3_576 ? 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 O1B Sm1 O1A 147.07(14) . . ? O1B Sm1 O2C 73.51(14) . 2_645 ? O1A Sm1 O2C 135.83(15) . 2_645 ? O1B Sm1 O1H 90.96(12) . . ? O1A Sm1 O1H 76.27(13) . . ? O2C Sm1 O1H 91.25(14) 2_645 . ? O1B Sm1 O4A 134.04(12) . 2_545 ? O1A Sm1 O4A 75.64(13) . 2_545 ? O2C Sm1 O4A 78.05(13) 2_645 2_545 ? O1H Sm1 O4A 125.30(12) . 2_545 ? O1B Sm1 O1C 73.10(13) . . ? O1A Sm1 O1C 74.83(14) . . ? O2C Sm1 O1C 145.27(14) 2_645 . ? O1H Sm1 O1C 80.05(13) . . ? O4A Sm1 O1C 133.91(12) 2_545 . ? O1B Sm1 N1B 63.66(12) . . ? O1A Sm1 N1B 132.03(12) . . ? O2C Sm1 N1B 70.18(13) 2_645 . ? O1H Sm1 N1B 151.57(12) . . ? O4A Sm1 N1B 73.09(12) 2_545 . ? O1C Sm1 N1B 102.74(13) . . ? O1B Sm1 N1C 103.29(13) . . ? O1A Sm1 N1C 67.74(13) . . ? O2C Sm1 N1C 135.32(13) 2_645 . ? O1H Sm1 N1C 133.36(12) . . ? O4A Sm1 N1C 73.44(12) 2_545 . ? O1C Sm1 N1C 62.92(12) . . ? N1B Sm1 N1C 69.00(12) . . ? O1B Sm1 O3A 136.63(13) . 2_545 ? O1A Sm1 O3A 70.14(14) . 2_545 ? O2C Sm1 O3A 65.74(14) 2_645 2_545 ? O1H Sm1 O3A 76.12(12) . 2_545 ? O4A Sm1 O3A 50.39(11) 2_545 2_545 ? O1C Sm1 O3A 141.26(13) . 2_545 ? N1B Sm1 O3A 112.77(12) . 2_545 ? N1C Sm1 O3A 115.75(12) . 2_545 ? O1B Sm1 C6A 141.97(14) . 2_545 ? O1A Sm1 C6A 70.84(15) . 2_545 ? O2C Sm1 C6A 70.04(14) 2_645 2_545 ? O1H Sm1 C6A 100.22(14) . 2_545 ? O4A Sm1 C6A 25.72(12) 2_545 2_545 ? O1C Sm1 C6A 144.45(14) . 2_545 ? N1B Sm1 C6A 93.55(13) . 2_545 ? N1C Sm1 C6A 95.11(13) . 2_545 ? O3A Sm1 C6A 24.67(12) 2_545 2_545 ? O3C Sm2 O4A 134.99(12) . 2_545 ? O3C Sm2 O3B 74.62(14) . . ? O4A Sm2 O3B 132.33(12) 2_545 . ? O3C Sm2 O2H 75.00(15) . . ? O4A Sm2 O2H 135.53(14) 2_545 . ? O3B Sm2 O2H 80.05(14) . . ? O3C Sm2 O4H 146.68(13) . . ? O4A Sm2 O4H 75.78(13) 2_545 . ? O3B Sm2 O4H 73.48(13) . . ? O2H Sm2 O4H 90.21(15) . . ? O3C Sm2 O3H 72.90(13) . . ? O4A Sm2 O3H 79.15(13) 2_545 . ? O3B Sm2 O3H 146.17(13) . . ? O2H Sm2 O3H 82.71(15) . . ? O4H Sm2 O3H 135.60(13) . . ? O3C Sm2 N2A 131.46(14) . 2_545 ? O4A Sm2 N2A 62.77(12) 2_545 2_545 ? O3B Sm2 N2A 132.24(14) . 2_545 ? O2H Sm2 N2A 72.81(14) . 2_545 ? O4H Sm2 N2A 68.19(13) . 2_545 ? O3H Sm2 N2A 67.84(14) . 2_545 ? O3C Sm2 N2C 63.30(12) . . ? O4A Sm2 N2C 74.46(12) 2_545 . ? O3B Sm2 N2C 102.87(13) . . ? O2H Sm2 N2C 135.16(15) . . ? O4H Sm2 N2C 134.01(12) . . ? O3H Sm2 N2C 70.35(13) . . ? N2A Sm2 N2C 124.14(13) 2_545 . ? O3C Sm2 N2B 104.50(13) . . ? O4A Sm2 N2B 72.30(12) 2_545 . ? O3B Sm2 N2B 63.02(12) . . ? O2H Sm2 N2B 141.10(14) . . ? O4H Sm2 N2B 68.80(13) . . ? O3H Sm2 N2B 135.21(13) . . ? N2A Sm2 N2B 123.34(13) 2_545 . ? N2C Sm2 N2B 69.19(13) . . ? C1B O1B Sm1 127.3(3) . . ? C6B O3B Sm2 127.6(3) . . ? C2B N1B N2B 119.4(4) . . ? C2B N1B Sm1 115.2(3) . . ? N2B N1B Sm1 124.5(3) . . ? C5B N2B N1B 119.4(4) . . ? C5B N2B Sm2 114.6(3) . . ? N1B N2B Sm2 125.4(3) . . ? N1B C2B C3B 123.1(5) . . ? N1B C2B C1B 115.1(4) . . ? C3B C2B C1B 121.8(5) . . ? C4B C3B C2B 117.6(5) . . ? C4B C3B H3B 121.2 . . ? C2B C3B H3B 121.2 . . ? C3B C4B C5B 117.7(5) . . ? C3B C4B H4B 121.1 . . ? C5B C4B H4B 121.1 . . ? O2B C1B O1B 126.4(5) . . ? O2B C1B C2B 117.0(5) . . ? O1B C1B C2B 116.6(4) . . ? N2B C5B C4B 122.7(5) . . ? N2B C5B C6B 115.9(4) . . ? C4B C5B C6B 121.4(5) . . ? C1C O1C Sm1 125.2(3) . . ? C1A O1A Sm1 140.9(3) . . ? N1A C2A C3A 122.1(5) . . ? N1A C2A C1A 116.4(4) . . ? C3A C2A C1A 121.5(5) . . ? O2A C1A O1A 126.1(5) . . ? O2A C1A C2A 119.8(5) . . ? O1A C1A C2A 114.0(5) . . ? C6C O3C Sm2 129.1(3) . . ? C1C O2C Sm1 163.7(4) . 2_655 ? O4C C6C O3C 128.6(5) . . ? O4C C6C C5C 116.2(5) . . ? O3C C6C C5C 115.2(5) . . ? N2C C5C C4C 123.1(5) . . ? N2C C5C C6C 116.1(5) . . ? C4C C5C C6C 120.8(5) . . ? N1C C2C C3C 122.7(5) . . ? N1C C2C C1C 116.3(4) . . ? C3C C2C C1C 121.0(5) . . ? O2C C1C O1C 126.4(5) . . ? O2C C1C C2C 115.1(4) . . ? O1C C1C C2C 118.5(4) . . ? C5C N2C N1C 119.4(4) . . ? C5C N2C Sm2 114.7(3) . . ? N1C N2C Sm2 125.1(3) . . ? C2C N1C N2C 119.6(4) . . ? C2C N1C Sm1 114.9(3) . . ? N2C N1C Sm1 124.7(3) . . ? N2A N1A C2A 118.4(4) . . ? C5A N2A N1A 121.1(4) . . ? C5A N2A Sm2 117.4(3) . 2 ? N1A N2A Sm2 121.4(3) . 2 ? N2A C5A C4A 122.5(5) . . ? N2A C5A C6A 114.5(4) . . ? C4A C5A C6A 123.0(5) . . ? C4C C3C C2C 117.7(5) . . ? C4C C3C H3C 121.1 . . ? C2C C3C H3C 121.1 . . ? C3C C4C C5C 117.4(5) . . ? C3C C4C H4C 121.3 . . ? C5C C4C H4C 121.3 . . ? C4A C3A C2A 118.8(5) . . ? C4A C3A H3A 120.6 . . ? C2A C3A H3A 120.6 . . ? C3A C4A C5A 117.0(5) . . ? C3A C4A H4A 121.5 . . ? C5A C4A H4A 121.5 . . ? O3A C6A O4A 122.4(5) . . ? O3A C6A C5A 120.8(4) . . ? O4A C6A C5A 116.8(4) . . ? O3A C6A Sm1 67.2(3) . 2 ? O4A C6A Sm1 55.2(2) . 2 ? C5A C6A Sm1 171.9(4) . 2 ? C6A O3A Sm1 88.2(3) . 2 ? O4B C6B O3B 126.9(5) . . ? O4B C6B C5B 117.1(5) . . ? O3B C6B C5B 116.0(4) . . ? C6A O4A Sm2 128.3(3) . 2 ? C6A O4A Sm1 99.1(3) . 2 ? Sm2 O4A Sm1 132.68(14) 2 2 ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.281 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.337 # Attachment '- 4_Eudcp.cif' data_770966 _database_code_depnum_ccdc_archive 'CCDC 770966' #TrackingRef '- 4_Eudcp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; '2(Eu 3+). 3(C6 N2 O4 H2 2-). 4(H2 O); 3(H2 O)' ; _chemical_formula_sum 'C18 H20 Eu2 N6 O19' _chemical_formula_weight 928.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4063(10) _cell_length_b 13.1997(13) _cell_length_c 20.244(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.695(5) _cell_angle_gamma 90.00 _cell_volume 2712.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 302(2) _cell_measurement_reflns_used 5602 _cell_measurement_theta_min 2.501 _cell_measurement_theta_max 23.567 _exptl_crystal_description platelet _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 4.682 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7058 _exptl_absorpt_correction_T_max 0.9547 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006), based on the method developped by R. Blessing, Acta Cryst. A, 51, 33 (1995).' ; _diffrn_ambient_temperature 302(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 53377 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.13 _reflns_number_total 4822 _reflns_number_gt 4230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker X8' _computing_cell_refinement 'Bruker X8/SAINT' _computing_data_reduction 'Bruker X8/SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0228P)^2^+13.0510P] 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 4822 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0546 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 Eu1 Eu 0.44814(2) 0.351010(16) 0.241549(11) 0.01719(7) Uani 1 1 d . . . Eu2 Eu 0.31183(2) 0.225661(17) 0.415004(11) 0.02017(7) Uani 1 1 d . . . O1B O 0.6762(3) 0.3602(3) 0.24508(17) 0.0319(8) Uani 1 1 d . . . O2B O 0.8815(3) 0.3014(3) 0.27867(18) 0.0461(10) Uani 1 1 d . . . O3B O 0.4748(3) 0.1676(3) 0.50856(16) 0.0329(8) Uani 1 1 d . . . N1B N 0.6049(4) 0.2797(3) 0.35198(19) 0.0228(8) Uani 1 1 d . . . N2B N 0.5640(4) 0.2403(3) 0.40470(18) 0.0224(8) Uani 1 1 d . . . C2B C 0.7309(4) 0.2694(4) 0.3485(2) 0.0253(10) Uani 1 1 d . . . C3B C 0.8218(5) 0.2178(4) 0.3971(3) 0.0377(13) Uani 1 1 d . . . H3B H 0.9090 0.2112 0.3934 0.045 Uiso 1 1 calc R . . C4B C 0.7801(5) 0.1772(4) 0.4501(3) 0.0363(13) Uani 1 1 d . . . H4B H 0.8375 0.1418 0.4840 0.044 Uiso 1 1 calc R . . C1B C 0.7656(5) 0.3150(4) 0.2852(3) 0.0296(11) Uani 1 1 d . . . C5B C 0.6490(5) 0.1904(4) 0.4521(2) 0.0253(10) Uani 1 1 d . . . O1H O 0.3999(3) 0.3861(3) 0.12382(16) 0.0332(8) Uani 1 1 d . . . O1C O 0.5067(4) 0.5286(2) 0.24427(17) 0.0336(8) Uani 1 1 d . . . O1A O 0.2459(3) 0.4368(3) 0.22230(18) 0.0406(9) Uani 1 1 d . . . C2A C 0.0500(5) 0.5263(4) 0.2002(3) 0.0317(11) Uani 1 1 d . . . C1A C 0.1600(5) 0.4719(4) 0.1762(3) 0.0345(12) Uani 1 1 d . . . O2A O 0.1580(4) 0.4703(4) 0.1150(2) 0.0614(13) Uani 1 1 d . . . O3H O 0.1088(3) 0.3292(3) 0.37725(19) 0.0393(9) Uani 1 1 d . . . O3C O 0.2954(4) 0.3325(3) 0.50546(17) 0.0355(8) Uani 1 1 d . . . O2H O 0.1756(4) 0.1294(3) 0.47442(18) 0.0429(9) Uani 1 1 d . . . O2C O 0.4815(4) 0.6860(2) 0.27889(18) 0.0361(8) Uani 1 1 d . . . O4C O 0.2775(5) 0.4834(3) 0.5521(2) 0.0625(13) Uani 1 1 d . . . C6C C 0.3022(5) 0.4276(4) 0.5078(3) 0.0351(12) Uani 1 1 d . . . C5C C 0.3453(5) 0.4788(4) 0.4489(3) 0.0316(11) Uani 1 1 d . . . C2C C 0.4289(5) 0.5552(3) 0.3445(2) 0.0261(10) Uani 1 1 d . . . C1C C 0.4775(5) 0.5930(3) 0.2837(2) 0.0262(11) Uani 1 1 d . . . N2C N 0.3774(4) 0.4165(3) 0.40313(18) 0.0234(8) Uani 1 1 d . . . N1C N 0.4196(4) 0.4554(3) 0.35063(19) 0.0225(8) Uani 1 1 d . . . N1A N -0.0399(4) 0.5737(3) 0.1531(2) 0.0337(10) Uani 1 1 d . . . N2A N -0.1311(4) 0.6295(3) 0.1731(2) 0.0273(9) Uani 1 1 d . . . C5A C -0.1342(5) 0.6370(4) 0.2382(2) 0.0280(11) Uani 1 1 d . . . O4H O 0.3943(3) 0.0628(2) 0.37979(18) 0.0343(8) Uani 1 1 d . . . C3C C 0.3924(6) 0.6227(4) 0.3901(3) 0.0440(15) Uani 1 1 d . . . H3C H 0.3972 0.6924 0.3842 0.053 Uiso 1 1 calc R . . C4C C 0.3496(6) 0.5828(4) 0.4436(3) 0.0448(15) Uani 1 1 d . . . H4C H 0.3240 0.6245 0.4754 0.054 Uiso 1 1 calc R . . C3A C 0.0465(5) 0.5287(4) 0.2687(3) 0.0419(14) Uani 1 1 d . . . H3A H 0.1073 0.4921 0.3003 0.050 Uiso 1 1 calc R . . C4A C -0.0483(5) 0.5860(4) 0.2884(3) 0.0381(13) Uani 1 1 d . . . H4A H -0.0541 0.5901 0.3335 0.046 Uiso 1 1 calc R . . C6A C -0.2385(5) 0.7075(4) 0.2520(2) 0.0260(10) Uani 1 1 d . . . O3A O -0.2490(3) 0.7246(3) 0.31004(17) 0.0364(9) Uani 1 1 d . . . O4B O 0.6698(4) 0.1023(3) 0.55497(19) 0.0458(10) Uani 1 1 d . . . C6B C 0.5945(5) 0.1485(4) 0.5102(2) 0.0273(11) Uani 1 1 d . . . O4A O -0.3133(3) 0.7491(2) 0.20019(15) 0.0239(7) Uani 1 1 d . . . O7H O 0.0644(5) 0.2575(4) 0.5599(2) 0.0754(15) Uani 1 1 d . . . O6H O 0.9744(6) 0.4105(6) 0.4610(4) 0.120(3) Uani 1 1 d . . . O8H O 0.8956(5) 0.3060(5) 0.1410(3) 0.0860(17) 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 Eu1 0.01938(12) 0.01297(11) 0.02054(12) 0.00179(9) 0.00723(9) 0.00124(9) Eu2 0.02056(12) 0.02105(13) 0.02005(12) 0.00085(9) 0.00693(9) -0.00221(9) O1B 0.0230(18) 0.036(2) 0.037(2) 0.0131(16) 0.0073(15) 0.0003(15) O2B 0.0227(19) 0.081(3) 0.038(2) 0.017(2) 0.0135(16) 0.0089(19) O3B 0.0267(19) 0.050(2) 0.0232(17) 0.0086(16) 0.0083(14) 0.0024(16) N1B 0.024(2) 0.021(2) 0.024(2) 0.0008(16) 0.0084(16) 0.0013(16) N2B 0.024(2) 0.023(2) 0.021(2) 0.0003(16) 0.0048(16) -0.0003(16) C2B 0.021(2) 0.028(3) 0.027(3) 0.001(2) 0.006(2) -0.001(2) C3B 0.027(3) 0.050(3) 0.039(3) 0.010(3) 0.012(2) 0.005(2) C4B 0.030(3) 0.048(3) 0.032(3) 0.015(2) 0.007(2) 0.010(2) C1B 0.022(3) 0.035(3) 0.032(3) 0.003(2) 0.008(2) -0.002(2) C5B 0.025(2) 0.025(2) 0.025(2) -0.001(2) 0.004(2) -0.001(2) O1H 0.0334(19) 0.043(2) 0.0233(17) 0.0041(15) 0.0072(15) 0.0061(17) O1C 0.053(2) 0.0173(17) 0.038(2) -0.0019(15) 0.0256(17) -0.0048(16) O1A 0.032(2) 0.048(2) 0.040(2) 0.0068(18) 0.0058(17) 0.0192(18) C2A 0.026(3) 0.034(3) 0.035(3) 0.002(2) 0.007(2) 0.010(2) C1A 0.037(3) 0.032(3) 0.037(3) 0.005(2) 0.013(2) 0.013(2) O2A 0.062(3) 0.085(3) 0.041(2) 0.012(2) 0.018(2) 0.044(3) O3H 0.031(2) 0.038(2) 0.049(2) 0.0036(17) 0.0091(17) 0.0069(17) O3C 0.049(2) 0.034(2) 0.0272(18) -0.0047(15) 0.0163(16) -0.0066(17) O2H 0.042(2) 0.053(2) 0.036(2) 0.0063(18) 0.0157(17) -0.0144(19) O2C 0.048(2) 0.0154(17) 0.047(2) 0.0040(16) 0.0141(18) -0.0044(16) O4C 0.103(4) 0.050(3) 0.048(3) -0.018(2) 0.045(3) -0.007(3) C6C 0.039(3) 0.038(3) 0.031(3) -0.006(2) 0.015(2) -0.004(2) C5C 0.034(3) 0.030(3) 0.032(3) -0.009(2) 0.012(2) -0.003(2) C2C 0.029(3) 0.017(2) 0.034(3) -0.004(2) 0.010(2) -0.004(2) C1C 0.026(3) 0.016(2) 0.036(3) 0.003(2) 0.004(2) -0.004(2) N2C 0.027(2) 0.022(2) 0.023(2) -0.0021(16) 0.0092(16) -0.0029(17) N1C 0.023(2) 0.019(2) 0.026(2) 0.0000(16) 0.0060(16) -0.0016(16) N1A 0.031(2) 0.036(2) 0.036(2) 0.004(2) 0.0105(19) 0.013(2) N2A 0.025(2) 0.025(2) 0.032(2) 0.0034(17) 0.0078(17) 0.0103(17) C5A 0.026(3) 0.029(3) 0.030(3) 0.000(2) 0.009(2) 0.004(2) O4H 0.042(2) 0.0218(17) 0.042(2) -0.0012(15) 0.0164(17) 0.0031(16) C3C 0.071(4) 0.016(3) 0.051(3) -0.008(2) 0.025(3) -0.005(3) C4C 0.066(4) 0.034(3) 0.042(3) -0.013(3) 0.029(3) 0.000(3) C3A 0.040(3) 0.050(4) 0.035(3) 0.012(3) 0.008(2) 0.025(3) C4A 0.040(3) 0.045(3) 0.029(3) 0.006(2) 0.007(2) 0.017(3) C6A 0.025(3) 0.026(3) 0.027(3) 0.001(2) 0.007(2) 0.007(2) O3A 0.038(2) 0.046(2) 0.0248(19) -0.0018(16) 0.0064(16) 0.0157(17) O4B 0.036(2) 0.059(3) 0.040(2) 0.029(2) 0.0045(17) 0.004(2) C6B 0.032(3) 0.026(3) 0.022(2) 0.000(2) 0.004(2) -0.005(2) O4A 0.0242(17) 0.0245(17) 0.0230(17) -0.0011(13) 0.0048(14) 0.0089(14) O7H 0.065(3) 0.103(4) 0.060(3) -0.004(3) 0.017(3) -0.018(3) O6H 0.086(4) 0.157(7) 0.123(5) -0.037(5) 0.034(4) 0.033(5) O8H 0.082(4) 0.124(5) 0.059(3) 0.018(3) 0.031(3) 0.035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O1A 2.346(3) . ? Eu1 O1B 2.362(3) . ? Eu1 O2C 2.363(3) 2_645 ? Eu1 O1H 2.371(3) . ? Eu1 O1C 2.419(3) . ? Eu1 O4A 2.428(3) 2_545 ? Eu1 N1B 2.635(4) . ? Eu1 N1C 2.674(4) . ? Eu1 O3A 2.687(3) 2_545 ? Eu1 C6A 2.914(5) 2_545 ? Eu1 C1B 3.261(5) . ? Eu1 Eu2 4.3897(4) . ? Eu2 O3C 2.347(3) . ? Eu2 O4A 2.356(3) 2_545 ? Eu2 O3B 2.374(3) . ? Eu2 O2H 2.413(3) . ? Eu2 O4H 2.477(3) . ? Eu2 O3H 2.491(3) . ? Eu2 N2A 2.618(4) 2_545 ? Eu2 N2C 2.635(4) . ? Eu2 N2B 2.684(4) . ? O1B C1B 1.244(6) . ? O2B C1B 1.255(6) . ? O3B C6B 1.265(6) . ? N1B C2B 1.335(6) . ? N1B N2B 1.339(5) . ? N2B C5B 1.329(6) . ? C2B C3B 1.386(7) . ? C2B C1B 1.528(6) . ? C3B C4B 1.354(7) . ? C3B H3B 0.9300 . ? C4B C5B 1.385(7) . ? C4B H4B 0.9300 . ? C5B C6B 1.516(6) . ? O1C C1C 1.249(6) . ? O1A C1A 1.233(6) . ? C2A N1A 1.337(6) . ? C2A C3A 1.394(7) . ? C2A C1A 1.519(7) . ? C1A O2A 1.234(6) . ? O3C C6C 1.258(6) . ? O2C C1C 1.232(6) . ? O2C Eu1 2.363(3) 2_655 ? O4C C6C 1.231(6) . ? C6C C5C 1.521(7) . ? C5C N2C 1.335(6) . ? C5C C4C 1.379(8) . ? C2C N1C 1.328(6) . ? C2C C3C 1.394(7) . ? C2C C1C 1.515(6) . ? N2C N1C 1.338(5) . ? N1A N2A 1.333(5) . ? N2A C5A 1.328(6) . ? N2A Eu2 2.618(4) 2 ? C5A C4A 1.374(7) . ? C5A C6A 1.502(6) . ? C3C C4C 1.364(8) . ? C3C H3C 0.9300 . ? C4C H4C 0.9300 . ? C3A C4A 1.370(7) . ? C3A H3A 0.9300 . ? C4A H4A 0.9300 . ? C6A O3A 1.225(6) . ? C6A O4A 1.284(6) . ? C6A Eu1 2.914(5) 2 ? O3A Eu1 2.687(3) 2 ? O4B C6B 1.223(6) . ? O4A Eu2 2.356(3) 2 ? O4A Eu1 2.428(3) 2 ? 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 O1A Eu1 O1B 147.04(13) . . ? O1A Eu1 O2C 135.80(13) . 2_645 ? O1B Eu1 O2C 72.84(12) . 2_645 ? O1A Eu1 O1H 75.80(12) . . ? O1B Eu1 O1H 90.56(11) . . ? O2C Eu1 O1H 90.53(12) 2_645 . ? O1A Eu1 O1C 75.43(13) . . ? O1B Eu1 O1C 72.72(12) . . ? O2C Eu1 O1C 144.18(12) 2_645 . ? O1H Eu1 O1C 80.23(12) . . ? O1A Eu1 O4A 75.83(12) . 2_545 ? O1B Eu1 O4A 134.25(11) . 2_545 ? O2C Eu1 O4A 78.96(12) 2_645 2_545 ? O1H Eu1 O4A 125.39(11) . 2_545 ? O1C Eu1 O4A 134.04(11) . 2_545 ? O1A Eu1 N1B 132.77(12) . . ? O1B Eu1 N1B 64.01(11) . . ? O2C Eu1 N1B 70.22(12) 2_645 . ? O1H Eu1 N1B 151.34(11) . . ? O1C Eu1 N1B 102.75(12) . . ? O4A Eu1 N1B 72.92(11) 2_545 . ? O1A Eu1 N1C 68.30(12) . . ? O1B Eu1 N1C 103.98(12) . . ? O2C Eu1 N1C 135.59(12) 2_645 . ? O1H Eu1 N1C 133.80(12) . . ? O1C Eu1 N1C 63.59(11) . . ? O4A Eu1 N1C 72.76(11) 2_545 . ? N1B Eu1 N1C 69.12(11) . . ? O1A Eu1 O3A 69.39(13) . 2_545 ? O1B Eu1 O3A 136.71(12) . 2_545 ? O2C Eu1 O3A 66.52(12) 2_645 2_545 ? O1H Eu1 O3A 75.86(11) . 2_545 ? O1C Eu1 O3A 141.21(12) . 2_545 ? O4A Eu1 O3A 50.66(10) 2_545 2_545 ? N1B Eu1 O3A 112.90(11) . 2_545 ? N1C Eu1 O3A 115.15(11) . 2_545 ? O1A Eu1 C6A 70.61(14) . 2_545 ? O1B Eu1 C6A 142.14(13) . 2_545 ? O2C Eu1 C6A 70.88(13) 2_645 2_545 ? O1H Eu1 C6A 100.19(13) . 2_545 ? O1C Eu1 C6A 144.69(13) . 2_545 ? O4A Eu1 C6A 25.82(12) 2_545 2_545 ? N1B Eu1 C6A 93.44(12) . 2_545 ? N1C Eu1 C6A 94.46(12) . 2_545 ? O3A Eu1 C6A 24.85(11) 2_545 2_545 ? O1A Eu1 C1B 159.02(13) . . ? O1B Eu1 C1B 17.83(12) . . ? O2C Eu1 C1B 65.09(13) 2_645 . ? O1H Eu1 C1B 106.19(12) . . ? O1C Eu1 C1B 84.26(13) . . ? O4A Eu1 C1B 116.52(11) 2_545 . ? N1B Eu1 C1B 46.88(12) . . ? N1C Eu1 C1B 98.10(12) . . ? O3A Eu1 C1B 131.58(12) 2_545 . ? C6A Eu1 C1B 128.09(13) 2_545 . ? O1A Eu1 Eu2 83.05(9) . . ? O1B Eu1 Eu2 119.63(8) . . ? O2C Eu1 Eu2 87.68(9) 2_645 . ? O1H Eu1 Eu2 147.51(8) . . ? O1C Eu1 Eu2 118.10(8) . . ? O4A Eu1 Eu2 23.06(7) 2_545 . ? N1B Eu1 Eu2 55.63(8) . . ? N1C Eu1 Eu2 54.53(8) . . ? O3A Eu1 Eu2 73.72(7) 2_545 . ? C6A Eu1 Eu2 48.87(9) 2_545 . ? C1B Eu1 Eu2 102.38(9) . . ? O3C Eu2 O4A 135.30(11) . 2_545 ? O3C Eu2 O3B 74.53(12) . . ? O4A Eu2 O3B 132.31(11) 2_545 . ? O3C Eu2 O2H 77.07(13) . . ? O4A Eu2 O2H 134.02(12) 2_545 . ? O3B Eu2 O2H 80.06(12) . . ? O3C Eu2 O4H 146.65(12) . . ? O4A Eu2 O4H 75.58(11) 2_545 . ? O3B Eu2 O4H 73.60(12) . . ? O2H Eu2 O4H 87.99(13) . . ? O3C Eu2 O3H 72.99(13) . . ? O4A Eu2 O3H 79.27(12) 2_545 . ? O3B Eu2 O3H 146.16(12) . . ? O2H Eu2 O3H 83.69(13) . . ? O4H Eu2 O3H 135.39(12) . . ? O3C Eu2 N2A 131.19(12) . 2_545 ? O4A Eu2 N2A 63.19(11) 2_545 2_545 ? O3B Eu2 N2A 131.85(13) . 2_545 ? O2H Eu2 N2A 70.83(12) . 2_545 ? O4H Eu2 N2A 68.01(12) . 2_545 ? O3H Eu2 N2A 67.86(12) . 2_545 ? O3C Eu2 N2C 63.98(11) . . ? O4A Eu2 N2C 74.10(11) 2_545 . ? O3B Eu2 N2C 103.14(12) . . ? O2H Eu2 N2C 137.86(12) . . ? O4H Eu2 N2C 133.67(11) . . ? O3H Eu2 N2C 70.54(12) . . ? N2A Eu2 N2C 124.26(12) 2_545 . ? O3C Eu2 N2B 104.91(12) . . ? O4A Eu2 N2B 72.21(11) 2_545 . ? O3B Eu2 N2B 63.02(11) . . ? O2H Eu2 N2B 140.18(12) . . ? O4H Eu2 N2B 68.50(11) . . ? O3H Eu2 N2B 135.59(12) . . ? N2A Eu2 N2B 123.35(12) 2_545 . ? N2C Eu2 N2B 69.33(11) . . ? O3C Eu2 Eu1 119.29(8) . . ? O4A Eu2 Eu1 23.81(7) 2_545 . ? O3B Eu2 Eu1 117.39(8) . . ? O2H Eu2 Eu1 157.80(9) . . ? O4H Eu2 Eu1 84.47(8) . . ? O3H Eu2 Eu1 87.09(9) . . ? N2A Eu2 Eu1 86.99(8) 2_545 . ? N2C Eu2 Eu1 55.31(8) . . ? N2B Eu2 Eu1 54.38(8) . . ? C1B O1B Eu1 126.6(3) . . ? C6B O3B Eu2 127.7(3) . . ? C2B N1B N2B 119.4(4) . . ? C2B N1B Eu1 115.0(3) . . ? N2B N1B Eu1 124.7(3) . . ? C5B N2B N1B 119.4(4) . . ? C5B N2B Eu2 114.5(3) . . ? N1B N2B Eu2 125.3(3) . . ? N1B C2B C3B 122.5(4) . . ? N1B C2B C1B 114.8(4) . . ? C3B C2B C1B 122.6(4) . . ? C4B C3B C2B 118.0(5) . . ? C4B C3B H3B 121.0 . . ? C2B C3B H3B 121.0 . . ? C3B C4B C5B 117.6(5) . . ? C3B C4B H4B 121.2 . . ? C5B C4B H4B 121.2 . . ? O1B C1B O2B 126.7(5) . . ? O1B C1B C2B 117.1(4) . . ? O2B C1B C2B 116.2(4) . . ? O1B C1B Eu1 35.5(2) . . ? O2B C1B Eu1 158.8(4) . . ? C2B C1B Eu1 82.7(3) . . ? N2B C5B C4B 123.0(4) . . ? N2B C5B C6B 116.0(4) . . ? C4B C5B C6B 121.0(4) . . ? C1C O1C Eu1 125.4(3) . . ? C1A O1A Eu1 141.5(3) . . ? N1A C2A C3A 122.1(4) . . ? N1A C2A C1A 116.8(4) . . ? C3A C2A C1A 121.0(4) . . ? O2A C1A O1A 127.1(5) . . ? O2A C1A C2A 118.8(5) . . ? O1A C1A C2A 114.0(4) . . ? C6C O3C Eu2 128.0(3) . . ? C1C O2C Eu1 161.6(3) . 2_655 ? O4C C6C O3C 127.2(5) . . ? O4C C6C C5C 116.8(5) . . ? O3C C6C C5C 115.9(4) . . ? N2C C5C C4C 122.8(5) . . ? N2C C5C C6C 115.6(4) . . ? C4C C5C C6C 121.6(5) . . ? N1C C2C C3C 122.4(5) . . ? N1C C2C C1C 116.6(4) . . ? C3C C2C C1C 121.0(4) . . ? O2C C1C O1C 127.6(5) . . ? O2C C1C C2C 114.6(4) . . ? O1C C1C C2C 117.8(4) . . ? C5C N2C N1C 119.4(4) . . ? C5C N2C Eu2 114.6(3) . . ? N1C N2C Eu2 125.2(3) . . ? C2C N1C N2C 119.9(4) . . ? C2C N1C Eu1 114.2(3) . . ? N2C N1C Eu1 125.0(3) . . ? N2A N1A C2A 118.3(4) . . ? C5A N2A N1A 121.1(4) . . ? C5A N2A Eu2 118.0(3) . 2 ? N1A N2A Eu2 120.9(3) . 2 ? N2A C5A C4A 122.9(4) . . ? N2A C5A C6A 114.0(4) . . ? C4A C5A C6A 123.1(4) . . ? C4C C3C C2C 117.6(5) . . ? C4C C3C H3C 121.2 . . ? C2C C3C H3C 121.2 . . ? C3C C4C C5C 117.9(5) . . ? C3C C4C H4C 121.1 . . ? C5C C4C H4C 121.1 . . ? C4A C3A C2A 118.7(5) . . ? C4A C3A H3A 120.6 . . ? C2A C3A H3A 120.6 . . ? C3A C4A C5A 116.6(5) . . ? C3A C4A H4A 121.7 . . ? C5A C4A H4A 121.7 . . ? O3A C6A O4A 122.6(4) . . ? O3A C6A C5A 120.9(4) . . ? O4A C6A C5A 116.5(4) . . ? O3A C6A Eu1 67.1(3) . 2 ? O4A C6A Eu1 55.5(2) . 2 ? C5A C6A Eu1 171.9(3) . 2 ? C6A O3A Eu1 88.0(3) . 2 ? O4B C6B O3B 125.8(5) . . ? O4B C6B C5B 118.0(4) . . ? O3B C6B C5B 116.2(4) . . ? C6A O4A Eu2 128.1(3) . 2 ? C6A O4A Eu1 98.7(3) . 2 ? Eu2 O4A Eu1 133.13(13) 2 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A Eu1 Eu2 O3C -68.47(14) . . . . ? O1B Eu1 Eu2 O3C 86.10(15) . . . . ? O2C Eu1 Eu2 O3C 154.83(14) 2_645 . . . ? O1H Eu1 Eu2 O3C -117.83(19) . . . . ? O1C Eu1 Eu2 O3C 0.90(15) . . . . ? O4A Eu1 Eu2 O3C -138.4(2) 2_545 . . . ? N1B Eu1 Eu2 O3C 87.33(14) . . . . ? N1C Eu1 Eu2 O3C -0.22(14) . . . . ? O3A Eu1 Eu2 O3C -138.97(13) 2_545 . . . ? C6A Eu1 Eu2 O3C -138.73(16) 2_545 . . . ? C1B Eu1 Eu2 O3C 90.96(14) . . . . ? O1A Eu1 Eu2 O4A 69.9(2) . . . 2_545 ? O1B Eu1 Eu2 O4A -135.5(2) . . . 2_545 ? O2C Eu1 Eu2 O4A -66.8(2) 2_645 . . 2_545 ? O1H Eu1 Eu2 O4A 20.5(2) . . . 2_545 ? O1C Eu1 Eu2 O4A 139.3(2) . . . 2_545 ? N1B Eu1 Eu2 O4A -134.3(2) . . . 2_545 ? N1C Eu1 Eu2 O4A 138.1(2) . . . 2_545 ? O3A Eu1 Eu2 O4A -0.6(2) 2_545 . . 2_545 ? C6A Eu1 Eu2 O4A -0.4(2) 2_545 . . 2_545 ? C1B Eu1 Eu2 O4A -130.7(2) . . . 2_545 ? O1A Eu1 Eu2 O3B -155.38(14) . . . . ? O1B Eu1 Eu2 O3B -0.81(14) . . . . ? O2C Eu1 Eu2 O3B 67.92(13) 2_645 . . . ? O1H Eu1 Eu2 O3B 155.26(19) . . . . ? O1C Eu1 Eu2 O3B -86.01(14) . . . . ? O4A Eu1 Eu2 O3B 134.7(2) 2_545 . . . ? N1B Eu1 Eu2 O3B 0.42(14) . . . . ? N1C Eu1 Eu2 O3B -87.13(14) . . . . ? O3A Eu1 Eu2 O3B 134.12(13) 2_545 . . . ? C6A Eu1 Eu2 O3B 134.35(16) 2_545 . . . ? C1B Eu1 Eu2 O3B 4.05(14) . . . . ? O1A Eu1 Eu2 O2H 65.6(3) . . . . ? O1B Eu1 Eu2 O2H -139.8(3) . . . . ? O2C Eu1 Eu2 O2H -71.1(3) 2_645 . . . ? O1H Eu1 Eu2 O2H 16.3(3) . . . . ? O1C Eu1 Eu2 O2H 135.0(3) . . . . ? O4A Eu1 Eu2 O2H -4.3(3) 2_545 . . . ? N1B Eu1 Eu2 O2H -138.6(3) . . . . ? N1C Eu1 Eu2 O2H 133.9(3) . . . . ? O3A Eu1 Eu2 O2H -4.9(3) 2_545 . . . ? C6A Eu1 Eu2 O2H -4.7(3) 2_545 . . . ? C1B Eu1 Eu2 O2H -135.0(3) . . . . ? O1A Eu1 Eu2 O4H 136.31(13) . . . . ? O1B Eu1 Eu2 O4H -69.11(13) . . . . ? O2C Eu1 Eu2 O4H -0.38(12) 2_645 . . . ? O1H Eu1 Eu2 O4H 86.96(18) . . . . ? O1C Eu1 Eu2 O4H -154.32(13) . . . . ? O4A Eu1 Eu2 O4H 66.4(2) 2_545 . . . ? N1B Eu1 Eu2 O4H -67.89(13) . . . . ? N1C Eu1 Eu2 O4H -155.44(13) . . . . ? O3A Eu1 Eu2 O4H 65.82(12) 2_545 . . . ? C6A Eu1 Eu2 O4H 66.05(15) 2_545 . . . ? C1B Eu1 Eu2 O4H -64.25(13) . . . . ? O1A Eu1 Eu2 O3H 0.17(13) . . . . ? O1B Eu1 Eu2 O3H 154.74(13) . . . . ? O2C Eu1 Eu2 O3H -136.53(13) 2_645 . . . ? O1H Eu1 Eu2 O3H -49.19(18) . . . . ? O1C Eu1 Eu2 O3H 69.53(13) . . . . ? O4A Eu1 Eu2 O3H -69.7(2) 2_545 . . . ? N1B Eu1 Eu2 O3H 155.97(13) . . . . ? N1C Eu1 Eu2 O3H 68.41(13) . . . . ? O3A Eu1 Eu2 O3H -70.33(12) 2_545 . . . ? C6A Eu1 Eu2 O3H -70.10(15) 2_545 . . . ? C1B Eu1 Eu2 O3H 159.60(13) . . . . ? O1A Eu1 Eu2 N2A 68.13(13) . . . 2_545 ? O1B Eu1 Eu2 N2A -137.30(13) . . . 2_545 ? O2C Eu1 Eu2 N2A -68.56(13) 2_645 . . 2_545 ? O1H Eu1 Eu2 N2A 18.78(18) . . . 2_545 ? O1C Eu1 Eu2 N2A 137.50(13) . . . 2_545 ? O4A Eu1 Eu2 N2A -1.8(2) 2_545 . . 2_545 ? N1B Eu1 Eu2 N2A -136.07(13) . . . 2_545 ? N1C Eu1 Eu2 N2A 136.38(13) . . . 2_545 ? O3A Eu1 Eu2 N2A -2.37(12) 2_545 . . 2_545 ? C6A Eu1 Eu2 N2A -2.13(15) 2_545 . . 2_545 ? C1B Eu1 Eu2 N2A -132.43(13) . . . 2_545 ? O1A Eu1 Eu2 N2C -68.09(14) . . . . ? O1B Eu1 Eu2 N2C 86.48(14) . . . . ? O2C Eu1 Eu2 N2C 155.22(14) 2_645 . . . ? O1H Eu1 Eu2 N2C -117.44(19) . . . . ? O1C Eu1 Eu2 N2C 1.28(14) . . . . ? O4A Eu1 Eu2 N2C -138.0(2) 2_545 . . . ? N1B Eu1 Eu2 N2C 87.71(14) . . . . ? N1C Eu1 Eu2 N2C 0.16(14) . . . . ? O3A Eu1 Eu2 N2C -138.59(13) 2_545 . . . ? C6A Eu1 Eu2 N2C -138.35(16) 2_545 . . . ? C1B Eu1 Eu2 N2C 91.35(14) . . . . ? O1A Eu1 Eu2 N2B -156.24(14) . . . . ? O1B Eu1 Eu2 N2B -1.67(14) . . . . ? O2C Eu1 Eu2 N2B 67.07(13) 2_645 . . . ? O1H Eu1 Eu2 N2B 154.41(19) . . . . ? O1C Eu1 Eu2 N2B -86.87(14) . . . . ? O4A Eu1 Eu2 N2B 133.9(2) 2_545 . . . ? N1B Eu1 Eu2 N2B -0.44(14) . . . . ? N1C Eu1 Eu2 N2B -87.99(14) . . . . ? O3A Eu1 Eu2 N2B 133.26(13) 2_545 . . . ? C6A Eu1 Eu2 N2B 133.50(16) 2_545 . . . ? C1B Eu1 Eu2 N2B 3.20(13) . . . . ? O1A Eu1 O1B C1B 144.1(4) . . . . ? O2C Eu1 O1B C1B -61.3(4) 2_645 . . . ? O1H Eu1 O1B C1B -151.7(4) . . . . ? O1C Eu1 O1B C1B 128.7(4) . . . . ? O4A Eu1 O1B C1B -6.8(5) 2_545 . . . ? N1B Eu1 O1B C1B 14.6(4) . . . . ? N1C Eu1 O1B C1B 72.6(4) . . . . ? O3A Eu1 O1B C1B -82.0(4) 2_545 . . . ? C6A Eu1 O1B C1B -44.2(5) 2_545 . . . ? Eu2 Eu1 O1B C1B 15.7(4) . . . . ? O3C Eu2 O3B C6B -131.3(4) . . . . ? O4A Eu2 O3B C6B 6.9(5) 2_545 . . . ? O2H Eu2 O3B C6B 149.5(4) . . . . ? O4H Eu2 O3B C6B 58.7(4) . . . . ? O3H Eu2 O3B C6B -148.0(4) . . . . ? N2A Eu2 O3B C6B 96.7(4) 2_545 . . . ? N2C Eu2 O3B C6B -73.4(4) . . . . ? N2B Eu2 O3B C6B -15.1(4) . . . . ? Eu1 Eu2 O3B C6B -15.9(4) . . . . ? O1A Eu1 N1B C2B -156.2(3) . . . . ? O1B Eu1 N1B C2B -11.0(3) . . . . ? O2C Eu1 N1B C2B 69.0(3) 2_645 . . . ? O1H Eu1 N1B C2B 18.6(5) . . . . ? O1C Eu1 N1B C2B -74.3(3) . . . . ? O4A Eu1 N1B C2B 153.1(3) 2_545 . . . ? N1C Eu1 N1B C2B -129.3(3) . . . . ? O3A Eu1 N1B C2B 121.3(3) 2_545 . . . ? C6A Eu1 N1B C2B 137.3(3) 2_545 . . . ? C1B Eu1 N1B C2B -5.0(3) . . . . ? Eu2 Eu1 N1B C2B 170.2(4) . . . . ? O1A Eu1 N1B N2B 34.5(4) . . . . ? O1B Eu1 N1B N2B 179.7(4) . . . . ? O2C Eu1 N1B N2B -100.3(3) 2_645 . . . ? O1H Eu1 N1B N2B -150.7(3) . . . . ? O1C Eu1 N1B N2B 116.4(3) . . . . ? O4A Eu1 N1B N2B -16.2(3) 2_545 . . . ? N1C Eu1 N1B N2B 61.4(3) . . . . ? O3A Eu1 N1B N2B -48.0(3) 2_545 . . . ? C6A Eu1 N1B N2B -32.0(3) 2_545 . . . ? C1B Eu1 N1B N2B -174.3(4) . . . . ? Eu2 Eu1 N1B N2B 0.9(3) . . . . ? C2B N1B N2B C5B -0.9(6) . . . . ? Eu1 N1B N2B C5B 168.0(3) . . . . ? C2B N1B N2B Eu2 -170.3(3) . . . . ? Eu1 N1B N2B Eu2 -1.4(5) . . . . ? O3C Eu2 N2B C5B 75.4(3) . . . . ? O4A Eu2 N2B C5B -151.2(3) 2_545 . . . ? O3B Eu2 N2B C5B 11.8(3) . . . . ? O2H Eu2 N2B C5B -12.2(4) . . . . ? O4H Eu2 N2B C5B -70.1(3) . . . . ? O3H Eu2 N2B C5B 156.1(3) . . . . ? N2A Eu2 N2B C5B -112.3(3) 2_545 . . . ? N2C Eu2 N2B C5B 129.5(3) . . . . ? Eu1 Eu2 N2B C5B -169.0(3) . . . . ? O3C Eu2 N2B N1B -114.7(3) . . . . ? O4A Eu2 N2B N1B 18.7(3) 2_545 . . . ? O3B Eu2 N2B N1B -178.3(4) . . . . ? O2H Eu2 N2B N1B 157.7(3) . . . . ? O4H Eu2 N2B N1B 99.8(3) . . . . ? O3H Eu2 N2B N1B -34.0(4) . . . . ? N2A Eu2 N2B N1B 57.6(4) 2_545 . . . ? N2C Eu2 N2B N1B -60.6(3) . . . . ? Eu1 Eu2 N2B N1B 0.9(3) . . . . ? N2B N1B C2B C3B 0.9(7) . . . . ? Eu1 N1B C2B C3B -169.0(4) . . . . ? N2B N1B C2B C1B 178.4(4) . . . . ? Eu1 N1B C2B C1B 8.5(5) . . . . ? N1B C2B C3B C4B -0.4(8) . . . . ? C1B C2B C3B C4B -177.7(5) . . . . ? C2B C3B C4B C5B -0.1(8) . . . . ? Eu1 O1B C1B O2B 163.1(4) . . . . ? Eu1 O1B C1B C2B -15.7(6) . . . . ? N1B C2B C1B O1B 2.9(7) . . . . ? C3B C2B C1B O1B -179.6(5) . . . . ? N1B C2B C1B O2B -176.1(5) . . . . ? C3B C2B C1B O2B 1.4(7) . . . . ? N1B C2B C1B Eu1 -6.3(4) . . . . ? C3B C2B C1B Eu1 171.2(5) . . . . ? O1A Eu1 C1B O1B -63.0(6) . . . . ? O2C Eu1 C1B O1B 112.4(4) 2_645 . . . ? O1H Eu1 C1B O1B 29.5(4) . . . . ? O1C Eu1 C1B O1B -48.5(4) . . . . ? O4A Eu1 C1B O1B 174.5(4) 2_545 . . . ? N1B Eu1 C1B O1B -162.0(5) . . . . ? N1C Eu1 C1B O1B -110.8(4) . . . . ? O3A Eu1 C1B O1B 114.8(4) 2_545 . . . ? C6A Eu1 C1B O1B 147.0(4) 2_545 . . . ? Eu2 Eu1 C1B O1B -166.1(4) . . . . ? O1A Eu1 C1B O2B -103.0(11) . . . . ? O1B Eu1 C1B O2B -40.0(9) . . . . ? O2C Eu1 C1B O2B 72.4(11) 2_645 . . . ? O1H Eu1 C1B O2B -10.5(11) . . . . ? O1C Eu1 C1B O2B -88.6(11) . . . . ? O4A Eu1 C1B O2B 134.5(10) 2_545 . . . ? N1B Eu1 C1B O2B 158.0(11) . . . . ? N1C Eu1 C1B O2B -150.8(10) . . . . ? O3A Eu1 C1B O2B 74.8(11) 2_545 . . . ? C6A Eu1 C1B O2B 107.0(10) 2_545 . . . ? Eu2 Eu1 C1B O2B 153.9(10) . . . . ? O1A Eu1 C1B C2B 102.9(4) . . . . ? O1B Eu1 C1B C2B 165.9(6) . . . . ? O2C Eu1 C1B C2B -81.7(3) 2_645 . . . ? O1H Eu1 C1B C2B -164.5(3) . . . . ? O1C Eu1 C1B C2B 117.4(3) . . . . ? O4A Eu1 C1B C2B -19.5(3) 2_545 . . . ? N1B Eu1 C1B C2B 4.0(2) . . . . ? N1C Eu1 C1B C2B 55.2(3) . . . . ? O3A Eu1 C1B C2B -79.3(3) 2_545 . . . ? C6A Eu1 C1B C2B -47.0(3) 2_545 . . . ? Eu2 Eu1 C1B C2B -0.2(3) . . . . ? N1B N2B C5B C4B 0.3(7) . . . . ? Eu2 N2B C5B C4B 170.9(4) . . . . ? N1B N2B C5B C6B 179.8(4) . . . . ? Eu2 N2B C5B C6B -9.7(5) . . . . ? C3B C4B C5B N2B 0.2(8) . . . . ? C3B C4B C5B C6B -179.3(5) . . . . ? O1A Eu1 O1C C1C 58.5(4) . . . . ? O1B Eu1 O1C C1C -130.1(4) . . . . ? O2C Eu1 O1C C1C -146.6(4) 2_645 . . . ? O1H Eu1 O1C C1C 136.2(4) . . . . ? O4A Eu1 O1C C1C 5.6(5) 2_545 . . . ? N1B Eu1 O1C C1C -72.8(4) . . . . ? N1C Eu1 O1C C1C -14.2(4) . . . . ? O3A Eu1 O1C C1C 83.8(4) 2_545 . . . ? C6A Eu1 O1C C1C 42.4(5) 2_545 . . . ? C1B Eu1 O1C C1C -116.2(4) . . . . ? Eu2 Eu1 O1C C1C -15.2(4) . . . . ? O1B Eu1 O1A C1A 73.5(7) . . . . ? O2C Eu1 O1A C1A -70.4(6) 2_645 . . . ? O1H Eu1 O1A C1A 5.3(6) . . . . ? O1C Eu1 O1A C1A 88.7(6) . . . . ? O4A Eu1 O1A C1A -127.5(6) 2_545 . . . ? N1B Eu1 O1A C1A -177.3(5) . . . . ? N1C Eu1 O1A C1A 155.7(6) . . . . ? O3A Eu1 O1A C1A -74.6(6) 2_545 . . . ? C6A Eu1 O1A C1A -101.1(6) 2_545 . . . ? C1B Eu1 O1A C1A 103.6(6) . . . . ? Eu2 Eu1 O1A C1A -149.8(6) . . . . ? Eu1 O1A C1A O2A 0.3(11) . . . . ? Eu1 O1A C1A C2A -176.9(4) . . . . ? N1A C2A C1A O2A -3.2(8) . . . . ? C3A C2A C1A O2A 178.8(6) . . . . ? N1A C2A C1A O1A 174.3(5) . . . . ? C3A C2A C1A O1A -3.8(8) . . . . ? O4A Eu2 O3C C6C -10.8(5) 2_545 . . . ? O3B Eu2 O3C C6C 124.7(5) . . . . ? O2H Eu2 O3C C6C -152.2(5) . . . . ? O4H Eu2 O3C C6C 142.3(4) . . . . ? O3H Eu2 O3C C6C -64.9(4) . . . . ? N2A Eu2 O3C C6C -102.6(4) 2_545 . . . ? N2C Eu2 O3C C6C 11.3(4) . . . . ? N2B Eu2 O3C C6C 68.8(5) . . . . ? Eu1 Eu2 O3C C6C 11.6(5) . . . . ? Eu2 O3C C6C O4C 170.3(5) . . . . ? Eu2 O3C C6C C5C -9.5(7) . . . . ? O4C C6C C5C N2C 177.0(5) . . . . ? O3C C6C C5C N2C -3.2(7) . . . . ? O4C C6C C5C C4C -3.5(8) . . . . ? O3C C6C C5C C4C 176.3(5) . . . . ? Eu1 O2C C1C O1C -40.1(14) 2_655 . . . ? Eu1 O2C C1C C2C 141.0(9) 2_655 . . . ? Eu1 O1C C1C O2C -164.4(4) . . . . ? Eu1 O1C C1C C2C 14.4(6) . . . . ? N1C C2C C1C O2C 178.2(4) . . . . ? C3C C2C C1C O2C 0.1(7) . . . . ? N1C C2C C1C O1C -0.8(7) . . . . ? C3C C2C C1C O1C -178.9(5) . . . . ? C4C C5C N2C N1C 2.2(8) . . . . ? C6C C5C N2C N1C -178.3(4) . . . . ? C4C C5C N2C Eu2 -167.9(4) . . . . ? C6C C5C N2C Eu2 11.6(5) . . . . ? O3C Eu2 N2C C5C -11.3(3) . . . . ? O4A Eu2 N2C C5C 152.7(4) 2_545 . . . ? O3B Eu2 N2C C5C -76.5(3) . . . . ? O2H Eu2 N2C C5C 13.1(4) . . . . ? O4H Eu2 N2C C5C -156.3(3) . . . . ? O3H Eu2 N2C C5C 68.7(3) . . . . ? N2A Eu2 N2C C5C 112.3(3) 2_545 . . . ? N2B Eu2 N2C C5C -130.7(4) . . . . ? Eu1 Eu2 N2C C5C 169.1(4) . . . . ? O3C Eu2 N2C N1C 179.3(4) . . . . ? O4A Eu2 N2C N1C -16.6(3) 2_545 . . . ? O3B Eu2 N2C N1C 114.1(3) . . . . ? O2H Eu2 N2C N1C -156.3(3) . . . . ? O4H Eu2 N2C N1C 34.3(4) . . . . ? O3H Eu2 N2C N1C -100.6(3) . . . . ? N2A Eu2 N2C N1C -57.0(4) 2_545 . . . ? N2B Eu2 N2C N1C 60.0(3) . . . . ? Eu1 Eu2 N2C N1C -0.3(3) . . . . ? C3C C2C N1C N2C -1.9(7) . . . . ? C1C C2C N1C N2C 180.0(4) . . . . ? C3C C2C N1C Eu1 167.5(4) . . . . ? C1C C2C N1C Eu1 -10.6(5) . . . . ? C5C N2C N1C C2C -0.1(6) . . . . ? Eu2 N2C N1C C2C 168.8(3) . . . . ? C5C N2C N1C Eu1 -168.4(3) . . . . ? Eu2 N2C N1C Eu1 0.5(5) . . . . ? O1A Eu1 N1C C2C -72.0(3) . . . . ? O1B Eu1 N1C C2C 74.2(3) . . . . ? O2C Eu1 N1C C2C 153.8(3) 2_645 . . . ? O1H Eu1 N1C C2C -30.4(4) . . . . ? O1C Eu1 N1C C2C 12.0(3) . . . . ? O4A Eu1 N1C C2C -153.3(3) 2_545 . . . ? N1B Eu1 N1C C2C 128.9(3) . . . . ? O3A Eu1 N1C C2C -124.8(3) 2_545 . . . ? C6A Eu1 N1C C2C -139.1(3) 2_545 . . . ? C1B Eu1 N1C C2C 91.4(3) . . . . ? Eu2 Eu1 N1C C2C -169.1(4) . . . . ? O1A Eu1 N1C N2C 96.8(3) . . . . ? O1B Eu1 N1C N2C -116.9(3) . . . . ? O2C Eu1 N1C N2C -37.3(4) 2_645 . . . ? O1H Eu1 N1C N2C 138.4(3) . . . . ? O1C Eu1 N1C N2C -179.2(4) . . . . ? O4A Eu1 N1C N2C 15.6(3) 2_545 . . . ? N1B Eu1 N1C N2C -62.3(3) . . . . ? O3A Eu1 N1C N2C 44.1(4) 2_545 . . . ? C6A Eu1 N1C N2C 29.7(3) 2_545 . . . ? C1B Eu1 N1C N2C -99.8(3) . . . . ? Eu2 Eu1 N1C N2C -0.3(3) . . . . ? C3A C2A N1A N2A 3.8(8) . . . . ? C1A C2A N1A N2A -174.2(4) . . . . ? C2A N1A N2A C5A -0.8(7) . . . . ? C2A N1A N2A Eu2 180.0(4) . . . 2 ? N1A N2A C5A C4A -2.4(8) . . . . ? Eu2 N2A C5A C4A 176.8(4) 2 . . . ? N1A N2A C5A C6A 176.7(4) . . . . ? Eu2 N2A C5A C6A -4.1(5) 2 . . . ? N1C C2C C3C C4C 1.9(9) . . . . ? C1C C2C C3C C4C 180.0(5) . . . . ? C2C C3C C4C C5C 0.0(9) . . . . ? N2C C5C C4C C3C -2.1(9) . . . . ? C6C C5C C4C C3C 178.5(5) . . . . ? N1A C2A C3A C4A -3.5(9) . . . . ? C1A C2A C3A C4A 174.4(5) . . . . ? C2A C3A C4A C5A 0.3(9) . . . . ? N2A C5A C4A C3A 2.6(8) . . . . ? C6A C5A C4A C3A -176.4(5) . . . . ? N2A C5A C6A O3A -177.2(5) . . . . ? C4A C5A C6A O3A 1.9(8) . . . . ? N2A C5A C6A O4A 1.9(6) . . . . ? C4A C5A C6A O4A -179.0(5) . . . . ? N2A C5A C6A Eu1 -5(3) . . . 2 ? C4A C5A C6A Eu1 174(2) . . . 2 ? O4A C6A O3A Eu1 -0.2(5) . . . 2 ? C5A C6A O3A Eu1 178.8(4) . . . 2 ? Eu2 O3B C6B O4B -166.3(4) . . . . ? Eu2 O3B C6B C5B 16.0(6) . . . . ? N2B C5B C6B O4B -179.8(4) . . . . ? C4B C5B C6B O4B -0.4(7) . . . . ? N2B C5B C6B O3B -1.9(6) . . . . ? C4B C5B C6B O3B 177.6(5) . . . . ? O3A C6A O4A Eu2 -179.2(3) . . . 2 ? C5A C6A O4A Eu2 1.8(6) . . . 2 ? Eu1 C6A O4A Eu2 -179.4(4) 2 . . 2 ? O3A C6A O4A Eu1 0.2(5) . . . 2 ? C5A C6A O4A Eu1 -178.8(4) . . . 2 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.651 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.108 # Attachment '- 5_Gddcp.cif' data_770967 _database_code_depnum_ccdc_archive 'CCDC 770967' #TrackingRef '- 5_Gddcp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; '2(Gd 3+). 3(C6 N2 O4 H2 2-). 6(H2 O); 3(H2 O)' ; _chemical_formula_sum 'C18 H24 Gd2 N6 O21' _chemical_formula_weight 974.91 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8519(2) _cell_length_b 19.6425(3) _cell_length_c 14.9977(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.5080(10) _cell_angle_gamma 90.00 _cell_volume 3408.61(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9946 _cell_measurement_theta_min 2.497 _cell_measurement_theta_max 28.052 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1794 _exptl_absorpt_coefficient_mu 3.944 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7463 _exptl_absorpt_correction_T_max 0.9333 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006), based on the method developped by R. Blessing, Acta Cryst. A, 51, 33 (1995).' ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 103337 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 30.54 _reflns_number_total 10419 _reflns_number_gt 8386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _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. O7H and O8H have been refined with an 50% occupancy factor due to the observed low Fourier peak density and in order to get reasonable thermal parameters. Some solvent accessible voids are observed, due to the unaccurate location of the crystallization water molecules. ; _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^)+(0.0862P)^2^+9.5627P] 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 10419 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Gd1 Gd 0.79029(2) 0.015840(11) 0.806234(16) 0.02196(7) Uani 1 1 d . . . Gd2 Gd 0.67014(2) 0.224391(11) 0.744765(16) 0.02348(7) Uani 1 1 d . . . O5H O 0.9220(4) 0.0553(2) 0.9396(3) 0.0396(9) Uani 1 1 d . . . O6H O 0.8136(3) -0.08885(18) 0.8799(3) 0.0298(7) Uani 1 1 d . . . O4H O 0.5883(3) -0.0217(2) 0.7616(3) 0.0340(8) Uani 1 1 d . . . O3A O 0.9796(4) -0.0129(2) 0.7885(3) 0.0393(10) Uani 1 1 d . . . N2A N 0.9131(4) 0.1138(2) 0.7486(3) 0.0265(8) Uani 1 1 d . . . N1A N 0.8795(4) 0.1791(2) 0.7370(3) 0.0255(8) Uani 1 1 d . . . O1C O 0.6975(3) 0.11913(17) 0.8271(2) 0.0268(7) Uani 1 1 d . . . N1B N 0.6631(4) 0.1270(2) 0.6202(3) 0.0288(9) Uani 1 1 d . . . O2C O 0.6058(4) 0.19415(19) 0.8947(3) 0.0360(9) Uani 1 1 d . . . O1H O 0.4751(4) 0.1830(2) 0.7128(3) 0.0449(11) Uani 1 1 d . . . O3H O 0.8062(4) 0.2655(2) 0.8834(3) 0.0439(10) Uani 1 1 d . . . O1B O 0.5875(4) 0.2543(2) 0.5916(3) 0.0359(9) Uani 1 1 d . . . O1A O 0.7963(4) 0.3021(2) 0.6970(3) 0.0404(10) Uani 1 1 d . . . O2H O 0.5856(4) 0.32695(19) 0.7790(3) 0.0378(9) Uani 1 1 d . . . N2B N 0.6949(4) 0.0621(2) 0.6395(3) 0.0285(9) Uani 1 1 d . . . O2A O 0.9727(4) 0.3446(2) 0.7100(4) 0.0502(12) Uani 1 1 d . . . C1A C 0.9051(5) 0.2972(3) 0.7075(4) 0.0347(11) Uani 1 1 d . . . C2A C 0.9508(5) 0.2252(3) 0.7163(4) 0.0287(10) Uani 1 1 d . . . C5A C 1.0156(5) 0.0960(3) 0.7345(4) 0.0304(10) Uani 1 1 d . . . O2B O 0.5463(4) 0.2391(2) 0.4411(3) 0.0450(11) Uani 1 1 d . . . O3B O 0.7747(4) -0.0619(2) 0.6826(3) 0.0344(8) Uani 1 1 d . . . C1B C 0.5806(5) 0.2190(3) 0.5215(4) 0.0328(11) Uani 1 1 d . . . C2B C 0.6152(5) 0.1448(3) 0.5345(4) 0.0334(11) Uani 1 1 d . . . C5B C 0.6775(6) 0.0160(3) 0.5736(4) 0.0349(12) Uani 1 1 d . . . C3A C 1.0606(5) 0.2091(3) 0.7029(5) 0.0419(14) Uani 1 1 d . . . H3A H 1.1103 0.2426 0.6900 0.050 Uiso 1 1 calc R . . C4A C 1.0916(5) 0.1426(3) 0.7095(5) 0.0403(14) Uani 1 1 d . . . H4A H 1.1618 0.1284 0.6976 0.048 Uiso 1 1 calc R . . C6A C 1.0466(5) 0.0216(3) 0.7510(4) 0.0328(11) Uani 1 1 d . . . O4A O 1.1343(4) 0.0004(3) 0.7288(5) 0.0582(15) Uani 1 1 d . . . C6B C 0.7155(6) -0.0561(3) 0.6030(4) 0.0385(13) Uani 1 1 d . . . O4B O 0.6846(6) -0.1022(2) 0.5487(4) 0.0653(16) Uani 1 1 d . . . C3B C 0.5981(7) 0.0991(3) 0.4624(4) 0.0497(17) Uani 1 1 d . . . H3B H 0.5670 0.1130 0.4029 0.060 Uiso 1 1 calc R . . C4B C 0.6291(7) 0.0318(4) 0.4824(5) 0.0517(18) Uani 1 1 d . . . H4B H 0.6182 -0.0014 0.4371 0.062 Uiso 1 1 calc R . . C1C C 0.6497(4) 0.1376(2) 0.8932(3) 0.0261(9) Uani 1 1 d . . . C2C C 0.6491(4) 0.0874(2) 0.9676(3) 0.0254(9) Uani 1 1 d . . . C3C C 0.6089(5) 0.1037(3) 1.0450(4) 0.0339(11) Uani 1 1 d . . . H3C H 0.5823 0.1472 1.0540 0.041 Uiso 1 1 calc R . . N1C N 0.6911(4) 0.0260(2) 0.9522(3) 0.0270(8) Uani 1 1 d . . . N2C N 0.6880(4) -0.0247(2) 1.0126(3) 0.0286(9) Uani 1 1 d . . . C4C C 0.6101(5) 0.0529(3) 1.1077(4) 0.0345(11) Uani 1 1 d . . . H4C H 0.5881 0.0610 1.1626 0.041 Uiso 1 1 calc R . . C5C C 0.6461(4) -0.0126(2) 1.0855(4) 0.0275(10) Uani 1 1 d . . . C6C C 0.6370(4) -0.0738(3) 1.1473(4) 0.0297(10) Uani 1 1 d . . . O3C O 0.6929(4) -0.1256(2) 1.1361(3) 0.0463(11) Uani 1 1 d . . . O4C O 0.5720(4) -0.0670(2) 1.2017(3) 0.0399(10) Uani 1 1 d . . . O7H O 0.2829(8) 0.2353(9) 0.6005(10) 0.107(7) Uani 0.50 1 d P . . O8H O 0.3615(8) 0.3594(5) 0.7525(9) 0.062(3) Uani 0.50 1 d P . . O9H O 0.6221(4) 0.3754(2) 0.4419(3) 0.0375(9) Uani 1 1 d . . . O10H O 0.4096(7) 0.3630(5) 0.5794(6) 0.116(4) 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 Gd1 0.02470(12) 0.01454(11) 0.02704(12) 0.00176(7) 0.00647(9) 0.00113(7) Gd2 0.02418(12) 0.01572(11) 0.03064(13) 0.00586(8) 0.00616(9) 0.00122(8) O5H 0.036(2) 0.040(2) 0.040(2) -0.0043(18) 0.0033(17) -0.0062(18) O6H 0.042(2) 0.0171(15) 0.0298(17) 0.0026(13) 0.0071(15) -0.0002(14) O4H 0.0302(19) 0.031(2) 0.042(2) -0.0021(16) 0.0109(16) -0.0016(15) O3A 0.034(2) 0.0235(19) 0.066(3) 0.0045(18) 0.021(2) 0.0034(15) N2A 0.027(2) 0.0211(19) 0.032(2) 0.0026(16) 0.0082(16) 0.0005(15) N1A 0.0265(19) 0.0208(19) 0.031(2) 0.0026(15) 0.0096(16) -0.0005(15) O1C 0.0362(19) 0.0172(15) 0.0308(17) 0.0064(13) 0.0156(15) 0.0056(13) N1B 0.032(2) 0.025(2) 0.027(2) 0.0043(16) 0.0014(17) 0.0001(17) O2C 0.050(2) 0.0180(16) 0.045(2) 0.0042(15) 0.0204(18) 0.0088(16) O1H 0.032(2) 0.041(2) 0.060(3) 0.019(2) 0.0060(19) -0.0095(18) O3H 0.038(2) 0.038(2) 0.052(3) -0.0071(19) 0.0008(19) 0.0008(18) O1B 0.045(2) 0.0268(19) 0.035(2) 0.0100(16) 0.0067(17) 0.0020(16) O1A 0.032(2) 0.0274(19) 0.064(3) 0.0176(19) 0.0155(19) 0.0047(16) O2H 0.039(2) 0.0198(17) 0.057(3) 0.0038(17) 0.0162(19) 0.0045(15) N2B 0.033(2) 0.023(2) 0.028(2) 0.0039(16) 0.0027(17) 0.0003(16) O2A 0.039(2) 0.026(2) 0.090(4) 0.012(2) 0.024(2) -0.0031(17) C1A 0.033(3) 0.026(2) 0.049(3) 0.007(2) 0.016(2) 0.000(2) C2A 0.026(2) 0.024(2) 0.036(3) 0.0075(19) 0.009(2) -0.0007(18) C5A 0.029(2) 0.027(2) 0.038(3) 0.005(2) 0.012(2) 0.0004(19) O2B 0.058(3) 0.034(2) 0.034(2) 0.0127(17) -0.0088(19) -0.005(2) O3B 0.043(2) 0.0261(18) 0.0326(19) -0.0025(15) 0.0049(16) 0.0072(16) C1B 0.033(3) 0.027(3) 0.034(3) 0.010(2) 0.000(2) -0.003(2) C2B 0.040(3) 0.028(2) 0.030(2) 0.007(2) 0.001(2) -0.001(2) C5B 0.044(3) 0.025(3) 0.033(3) 0.0012(19) 0.002(2) 0.000(2) C3A 0.033(3) 0.033(3) 0.065(4) 0.017(3) 0.022(3) 0.002(2) C4A 0.029(3) 0.035(3) 0.063(4) 0.015(3) 0.022(3) 0.008(2) C6A 0.030(3) 0.023(2) 0.047(3) 0.002(2) 0.012(2) 0.0047(19) O4A 0.047(3) 0.035(2) 0.106(4) 0.008(3) 0.044(3) 0.011(2) C6B 0.052(4) 0.023(2) 0.038(3) -0.003(2) 0.005(3) 0.003(2) O4B 0.106(5) 0.031(2) 0.046(3) -0.005(2) -0.011(3) 0.005(3) C3B 0.074(5) 0.034(3) 0.032(3) 0.005(2) -0.010(3) 0.004(3) C4B 0.077(5) 0.034(3) 0.035(3) 0.000(3) -0.008(3) 0.005(3) C1C 0.027(2) 0.020(2) 0.032(2) 0.0043(18) 0.0073(18) 0.0022(17) C2C 0.028(2) 0.0161(19) 0.033(2) 0.0008(17) 0.0093(18) 0.0006(17) C3C 0.045(3) 0.022(2) 0.041(3) 0.002(2) 0.024(2) 0.004(2) N1C 0.031(2) 0.0189(18) 0.033(2) 0.0026(15) 0.0093(17) 0.0026(15) N2C 0.034(2) 0.0206(19) 0.033(2) 0.0051(16) 0.0127(18) 0.0014(16) C4C 0.045(3) 0.028(3) 0.036(3) 0.001(2) 0.022(2) 0.003(2) C5C 0.027(2) 0.021(2) 0.036(3) 0.0067(18) 0.011(2) 0.0005(17) C6C 0.026(2) 0.028(2) 0.037(3) 0.011(2) 0.0119(19) -0.0004(19) O3C 0.058(3) 0.028(2) 0.061(3) 0.0147(19) 0.030(2) 0.0111(19) O4C 0.045(2) 0.033(2) 0.049(2) 0.0159(18) 0.0253(19) 0.0044(17) O7H 0.022(4) 0.201(17) 0.101(10) 0.116(11) 0.022(5) 0.034(7) O8H 0.027(4) 0.027(4) 0.131(10) -0.012(5) 0.021(5) 0.003(3) O9H 0.038(2) 0.035(2) 0.041(2) 0.0028(17) 0.0131(17) 0.0002(17) O10H 0.094(5) 0.159(8) 0.112(6) 0.094(6) 0.059(5) 0.069(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O6H 2.322(3) . ? Gd1 O1C 2.361(3) . ? Gd1 O3B 2.378(4) . ? Gd1 O3A 2.384(4) . ? Gd1 O5H 2.385(4) . ? Gd1 O4H 2.456(4) . ? Gd1 N2A 2.666(4) . ? Gd1 N2B 2.670(4) . ? Gd1 N1C 2.707(4) . ? Gd2 O1A 2.354(4) . ? Gd2 O2H 2.356(4) . ? Gd2 O1B 2.368(4) . ? Gd2 O1C 2.394(3) . ? Gd2 O1H 2.399(4) . ? Gd2 O3H 2.474(5) . ? Gd2 O2C 2.595(4) . ? Gd2 N1A 2.662(4) . ? Gd2 N1B 2.662(4) . ? Gd2 C1C 2.856(5) . ? O3A C6A 1.264(7) . ? N2A C5A 1.324(7) . ? N2A N1A 1.344(6) . ? N1A C2A 1.320(6) . ? O1C C1C 1.296(6) . ? N1B C2B 1.335(7) . ? N1B N2B 1.343(6) . ? O2C C1C 1.230(6) . ? O1B C1B 1.248(7) . ? O1A C1A 1.269(7) . ? N2B C5B 1.323(7) . ? O2A C1A 1.223(7) . ? C1A C2A 1.509(7) . ? C2A C3A 1.396(8) . ? C5A C4A 1.392(7) . ? C5A C6A 1.514(7) . ? O2B C1B 1.250(7) . ? O3B C6B 1.253(7) . ? C1B C2B 1.516(8) . ? C2B C3B 1.387(9) . ? C5B C4B 1.400(9) . ? C5B C6B 1.522(8) . ? C3A C4A 1.356(8) . ? C3A H3A 0.9300 . ? C4A H4A 0.9300 . ? C6A O4A 1.230(7) . ? C6B O4B 1.221(7) . ? C3B C4B 1.386(9) . ? C3B H3B 0.9300 . ? C4B H4B 0.9300 . ? C1C C2C 1.490(7) . ? C2C N1C 1.344(6) . ? C2C C3C 1.384(7) . ? C3C C4C 1.369(7) . ? C3C H3C 0.9300 . ? N1C N2C 1.351(6) . ? N2C C5C 1.317(7) . ? C4C C5C 1.417(7) . ? C4C H4C 0.9300 . ? C5C C6C 1.536(7) . ? C6C O3C 1.245(7) . ? C6C O4C 1.245(6) . ? 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 O6H Gd1 O1C 135.14(13) . . ? O6H Gd1 O3B 77.48(13) . . ? O1C Gd1 O3B 134.06(13) . . ? O6H Gd1 O3A 79.95(14) . . ? O1C Gd1 O3A 134.04(13) . . ? O3B Gd1 O3A 71.15(15) . . ? O6H Gd1 O5H 84.28(14) . . ? O1C Gd1 O5H 81.30(15) . . ? O3B Gd1 O5H 142.08(15) . . ? O3A Gd1 O5H 73.11(16) . . ? O6H Gd1 O4H 82.67(14) . . ? O1C Gd1 O4H 80.75(13) . . ? O3B Gd1 O4H 71.83(14) . . ? O3A Gd1 O4H 141.65(15) . . ? O5H Gd1 O4H 138.50(15) . . ? O6H Gd1 N2A 140.89(14) . . ? O1C Gd1 N2A 74.08(12) . . ? O3B Gd1 N2A 99.56(14) . . ? O3A Gd1 N2A 62.72(13) . . ? O5H Gd1 N2A 74.53(14) . . ? O4H Gd1 N2A 134.14(14) . . ? O6H Gd1 N2B 136.82(13) . . ? O1C Gd1 N2B 73.54(13) . . ? O3B Gd1 N2B 62.81(13) . . ? O3A Gd1 N2B 101.19(15) . . ? O5H Gd1 N2B 137.91(15) . . ? O4H Gd1 N2B 69.92(14) . . ? N2A Gd1 N2B 66.49(13) . . ? O6H Gd1 N1C 73.03(13) . . ? O1C Gd1 N1C 62.18(12) . . ? O3B Gd1 N1C 134.72(14) . . ? O3A Gd1 N1C 133.77(15) . . ? O5H Gd1 N1C 67.54(14) . . ? O4H Gd1 N1C 70.98(14) . . ? N2A Gd1 N1C 124.92(13) . . ? N2B Gd1 N1C 124.21(14) . . ? O1A Gd2 O2H 80.81(14) . . ? O1A Gd2 O1B 72.55(15) . . ? O2H Gd2 O1B 83.87(15) . . ? O1A Gd2 O1C 133.87(13) . . ? O2H Gd2 O1C 129.98(14) . . ? O1B Gd2 O1C 134.11(14) . . ? O1A Gd2 O1H 143.80(15) . . ? O2H Gd2 O1H 84.03(16) . . ? O1B Gd2 O1H 73.28(15) . . ? O1C Gd2 O1H 80.05(14) . . ? O1A Gd2 O3H 72.73(17) . . ? O2H Gd2 O3H 76.61(15) . . ? O1B Gd2 O3H 142.33(16) . . ? O1C Gd2 O3H 81.81(15) . . ? O1H Gd2 O3H 134.64(17) . . ? O1A Gd2 O2C 137.51(16) . . ? O2H Gd2 O2C 77.76(13) . . ? O1B Gd2 O2C 139.47(14) . . ? O1C Gd2 O2C 52.25(11) . . ? O1H Gd2 O2C 69.15(15) . . ? O3H Gd2 O2C 66.84(16) . . ? O1A Gd2 N1A 62.85(13) . . ? O2H Gd2 N1A 137.72(14) . . ? O1B Gd2 N1A 103.53(14) . . ? O1C Gd2 N1A 73.19(12) . . ? O1H Gd2 N1A 138.18(16) . . ? O3H Gd2 N1A 72.65(14) . . ? O2C Gd2 N1A 114.40(13) . . ? O1A Gd2 N1B 100.24(15) . . ? O2H Gd2 N1B 144.82(14) . . ? O1B Gd2 N1B 63.54(14) . . ? O1C Gd2 N1B 73.81(12) . . ? O1H Gd2 N1B 74.58(16) . . ? O3H Gd2 N1B 137.69(14) . . ? O2C Gd2 N1B 118.23(13) . . ? N1A Gd2 N1B 67.49(13) . . ? O1A Gd2 C1C 142.27(15) . . ? O2H Gd2 C1C 103.22(15) . . ? O1B Gd2 C1C 144.84(15) . . ? O1C Gd2 C1C 26.77(13) . . ? O1H Gd2 C1C 73.31(15) . . ? O3H Gd2 C1C 71.90(16) . . ? O2C Gd2 C1C 25.50(12) . . ? N1A Gd2 C1C 94.12(13) . . ? N1B Gd2 C1C 97.05(14) . . ? C6A O3A Gd1 128.3(3) . . ? C5A N2A N1A 119.2(4) . . ? C5A N2A Gd1 116.4(3) . . ? N1A N2A Gd1 124.3(3) . . ? C2A N1A N2A 119.9(4) . . ? C2A N1A Gd2 115.6(3) . . ? N2A N1A Gd2 124.5(3) . . ? C1C O1C Gd1 129.4(3) . . ? C1C O1C Gd2 96.9(3) . . ? Gd1 O1C Gd2 133.55(15) . . ? C2B N1B N2B 119.9(5) . . ? C2B N1B Gd2 115.4(4) . . ? N2B N1B Gd2 124.5(3) . . ? C1C O2C Gd2 89.2(3) . . ? C1B O1B Gd2 128.2(3) . . ? C1A O1A Gd2 127.5(3) . . ? C5B N2B N1B 119.8(4) . . ? C5B N2B Gd1 115.7(3) . . ? N1B N2B Gd1 124.5(3) . . ? O2A C1A O1A 126.0(5) . . ? O2A C1A C2A 119.4(5) . . ? O1A C1A C2A 114.7(5) . . ? N1A C2A C3A 122.9(5) . . ? N1A C2A C1A 115.3(5) . . ? C3A C2A C1A 121.8(5) . . ? N2A C5A C4A 122.6(5) . . ? N2A C5A C6A 115.3(5) . . ? C4A C5A C6A 122.0(5) . . ? C6B O3B Gd1 128.1(4) . . ? O1B C1B O2B 125.9(5) . . ? O1B C1B C2B 117.3(5) . . ? O2B C1B C2B 116.8(5) . . ? N1B C2B C3B 122.7(5) . . ? N1B C2B C1B 115.1(5) . . ? C3B C2B C1B 122.2(5) . . ? N2B C5B C4B 123.0(5) . . ? N2B C5B C6B 115.6(5) . . ? C4B C5B C6B 121.5(5) . . ? C4A C3A C2A 116.9(5) . . ? C4A C3A H3A 121.5 . . ? C2A C3A H3A 121.5 . . ? C3A C4A C5A 118.3(5) . . ? C3A C4A H4A 120.9 . . ? C5A C4A H4A 120.9 . . ? O4A C6A O3A 126.0(5) . . ? O4A C6A C5A 118.1(5) . . ? O3A C6A C5A 115.8(5) . . ? O4B C6B O3B 126.3(6) . . ? O4B C6B C5B 118.1(6) . . ? O3B C6B C5B 115.5(5) . . ? C4B C3B C2B 117.6(6) . . ? C4B C3B H3B 121.2 . . ? C2B C3B H3B 121.2 . . ? C3B C4B C5B 117.1(6) . . ? C3B C4B H4B 121.5 . . ? C5B C4B H4B 121.5 . . ? O2C C1C O1C 121.6(5) . . ? O2C C1C C2C 120.9(5) . . ? O1C C1C C2C 117.5(4) . . ? O2C C1C Gd2 65.3(3) . . ? O1C C1C Gd2 56.3(2) . . ? C2C C1C Gd2 173.6(3) . . ? N1C C2C C3C 124.0(5) . . ? N1C C2C C1C 113.8(4) . . ? C3C C2C C1C 122.2(4) . . ? C4C C3C C2C 116.9(5) . . ? C4C C3C H3C 121.5 . . ? C2C C3C H3C 121.5 . . ? C2C N1C N2C 118.8(4) . . ? C2C N1C Gd1 116.5(3) . . ? N2C N1C Gd1 124.5(3) . . ? C5C N2C N1C 119.6(4) . . ? C3C C4C C5C 117.3(5) . . ? C3C C4C H4C 121.3 . . ? C5C C4C H4C 121.3 . . ? N2C C5C C4C 123.1(5) . . ? N2C C5C C6C 116.6(4) . . ? C4C C5C C6C 120.3(5) . . ? O3C C6C O4C 126.8(5) . . ? O3C C6C C5C 116.7(5) . . ? O4C C6C C5C 116.5(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.714 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.373 # Attachment '- 6_Tbdcp.cif' data_770968 _database_code_depnum_ccdc_archive 'CCDC 770968' #TrackingRef '- 6_Tbdcp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; '2(Tb 3+). 3(C6 N2 O4 H2 2-). 6(H2 O); 3(H2 O)' ; _chemical_formula_sum 'C18 H24 N6 O21 Tb2' _chemical_formula_weight 978.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8076(6) _cell_length_b 19.6020(10) _cell_length_c 14.9743(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.750(2) _cell_angle_gamma 90.00 _cell_volume 3380.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9695 _cell_measurement_theta_min 2.502 _cell_measurement_theta_max 31.412 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.381 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.090 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 4.237 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6006 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006), based on the method developped by R. Blessing, Acta Cryst. A, 51, 33 (1995).' ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 115552 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 30.51 _reflns_number_total 10305 _reflns_number_gt 8618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. O7H and O8H have been refined with an 50% occupancy factor due to the observed low Fourier peak density and in order to get reasonable thermal parameters. Some solvent accessible voids are observed, due to the unaccurate location of the crystallization water molecules. There is still some relatively high residual electron density in our calculations. This comes from the difficulty to reasonably locate the free crystallization water molecules and to refine them accurately. ; _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^)+(0.0816P)^2^+10.1305P] 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 10305 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.1359 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Tb1 Tb 0.790002(19) 0.015469(10) 0.806350(15) 0.02657(7) Uani 1 1 d . . . Tb2 Tb 0.669600(18) 0.223388(10) 0.744419(16) 0.02770(7) Uani 1 1 d . . . O5H O 0.9220(4) 0.0550(2) 0.9397(3) 0.0425(9) Uani 1 1 d . . . O6H O 0.8135(3) -0.08847(17) 0.8806(3) 0.0349(7) Uani 1 1 d . . . O4H O 0.5885(3) -0.02188(19) 0.7625(3) 0.0387(8) Uani 1 1 d . . . O3A O 0.9786(4) -0.01380(18) 0.7890(3) 0.0436(10) Uani 1 1 d . . . N2A N 0.9120(4) 0.1130(2) 0.7493(3) 0.0312(8) Uani 1 1 d . . . N1A N 0.8784(4) 0.1784(2) 0.7382(3) 0.0307(8) Uani 1 1 d . . . O1C O 0.6966(3) 0.11858(17) 0.8262(2) 0.0316(7) Uani 1 1 d . . . N1B N 0.6617(4) 0.1268(2) 0.6206(3) 0.0333(8) Uani 1 1 d . . . O2C O 0.6039(4) 0.19424(19) 0.8935(3) 0.0424(9) Uani 1 1 d . . . O1H O 0.4744(4) 0.1821(2) 0.7109(3) 0.0509(11) Uani 1 1 d . . . O3H O 0.8045(4) 0.2640(2) 0.8835(3) 0.0479(10) Uani 1 1 d . . . O1B O 0.5875(4) 0.25387(19) 0.5920(3) 0.0408(8) Uani 1 1 d . . . O1A O 0.7949(3) 0.3017(2) 0.6982(3) 0.0442(9) Uani 1 1 d . . . O2H O 0.5851(4) 0.32549(19) 0.7772(3) 0.0434(9) Uani 1 1 d . . . N2B N 0.6939(4) 0.0615(2) 0.6402(3) 0.0337(9) Uani 1 1 d . . . O2A O 0.9720(4) 0.3443(2) 0.7105(4) 0.0578(13) Uani 1 1 d . . . C1A C 0.9041(4) 0.2967(3) 0.7090(4) 0.0376(11) Uani 1 1 d . . . C2A C 0.9497(4) 0.2247(2) 0.7170(4) 0.0353(11) Uani 1 1 d . . . C5A C 1.0146(4) 0.0951(3) 0.7348(4) 0.0355(10) Uani 1 1 d . . . O2B O 0.5448(5) 0.2386(2) 0.4409(3) 0.0516(11) Uani 1 1 d . . . O3B O 0.7743(4) -0.06285(19) 0.6842(3) 0.0397(8) Uani 1 1 d . . . C1B C 0.5791(5) 0.2187(3) 0.5217(4) 0.0380(12) Uani 1 1 d . . . C2B C 0.6149(5) 0.1448(3) 0.5352(4) 0.0391(11) Uani 1 1 d . . . C5B C 0.6778(6) 0.0152(3) 0.5742(4) 0.0418(13) Uani 1 1 d . . . C3A C 1.0602(5) 0.2086(3) 0.7030(5) 0.0476(14) Uani 1 1 d . . . H3A H 1.1102 0.2421 0.6905 0.057 Uiso 1 1 calc R . . C4A C 1.0905(5) 0.1417(3) 0.7086(5) 0.0474(14) Uani 1 1 d . . . H4A H 1.1600 0.1273 0.6954 0.057 Uiso 1 1 calc R . . C6A C 1.0453(5) 0.0203(3) 0.7507(5) 0.0413(12) Uani 1 1 d . . . O4A O 1.1333(5) -0.0007(3) 0.7292(5) 0.0675(16) Uani 1 1 d . . . C6B C 0.7164(6) -0.0569(3) 0.6043(4) 0.0428(12) Uani 1 1 d . . . O4B O 0.6855(6) -0.1033(2) 0.5488(4) 0.0713(17) Uani 1 1 d . . . C3B C 0.5981(7) 0.0981(3) 0.4623(4) 0.0565(18) Uani 1 1 d . . . H3B H 0.5675 0.1119 0.4024 0.068 Uiso 1 1 calc R . . C4B C 0.6289(8) 0.0309(3) 0.4830(5) 0.0578(18) Uani 1 1 d . . . H4B H 0.6174 -0.0025 0.4378 0.069 Uiso 1 1 calc R . . C1C C 0.6494(4) 0.1372(2) 0.8930(4) 0.0325(9) Uani 1 1 d . . . C2C C 0.6487(4) 0.0869(2) 0.9670(3) 0.0316(9) Uani 1 1 d . . . C3C C 0.6084(5) 0.1039(3) 1.0447(4) 0.0415(12) Uani 1 1 d . . . H3C H 0.5815 0.1475 1.0532 0.050 Uiso 1 1 calc R . . N1C N 0.6919(4) 0.0262(2) 0.9524(3) 0.0325(8) Uani 1 1 d . . . N2C N 0.6886(4) -0.0244(2) 1.0135(3) 0.0361(9) Uani 1 1 d . . . C4C C 0.6104(5) 0.0534(3) 1.1079(4) 0.0421(12) Uani 1 1 d . . . H4C H 0.5884 0.0618 1.1629 0.050 Uiso 1 1 calc R . . C5C C 0.6470(5) -0.0121(2) 1.0869(4) 0.0338(10) Uani 1 1 d . . . C6C C 0.6380(5) -0.0735(3) 1.1486(4) 0.0383(11) Uani 1 1 d . . . O3C O 0.6949(4) -0.1252(2) 1.1384(4) 0.0571(12) Uani 1 1 d . . . O4C O 0.5741(4) -0.0666(2) 1.2028(3) 0.0468(10) Uani 1 1 d . . . O7H O 0.2833(8) 0.2368(10) 0.5997(9) 0.112(7) Uani 0.50 1 d P . . O8H O 0.3613(8) 0.3584(5) 0.7535(11) 0.077(4) Uani 0.50 1 d P . . O9H O 0.6210(4) 0.3751(2) 0.4415(3) 0.0442(9) Uani 1 1 d . . . O10H O 0.4094(7) 0.3637(5) 0.5792(6) 0.116(3) 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 Tb1 0.03012(12) 0.01520(10) 0.03419(13) 0.00230(7) 0.00667(9) 0.00130(7) Tb2 0.02849(12) 0.01682(11) 0.03779(13) 0.00676(7) 0.00733(9) 0.00127(7) O5H 0.0387(19) 0.041(2) 0.045(2) -0.0057(17) 0.0036(16) -0.0049(16) O6H 0.047(2) 0.0180(14) 0.0397(18) 0.0018(13) 0.0097(15) 0.0005(13) O4H 0.0339(18) 0.0323(18) 0.050(2) 0.0007(16) 0.0101(16) -0.0011(14) O3A 0.040(2) 0.0234(17) 0.073(3) 0.0051(16) 0.024(2) 0.0054(14) N2A 0.0307(19) 0.0225(17) 0.042(2) 0.0022(15) 0.0113(16) 0.0014(14) N1A 0.0331(19) 0.0205(17) 0.039(2) 0.0047(15) 0.0095(16) -0.0006(14) O1C 0.0380(17) 0.0208(14) 0.0390(17) 0.0069(13) 0.0149(14) 0.0044(12) N1B 0.037(2) 0.0260(18) 0.035(2) 0.0067(16) 0.0020(16) -0.0001(15) O2C 0.056(2) 0.0236(16) 0.053(2) 0.0035(15) 0.0230(19) 0.0064(16) O1H 0.037(2) 0.046(2) 0.067(3) 0.021(2) 0.0062(19) -0.0099(17) O3H 0.043(2) 0.041(2) 0.055(3) -0.0068(19) 0.0012(19) 0.0006(17) O1B 0.051(2) 0.0268(17) 0.042(2) 0.0110(15) 0.0054(17) 0.0010(15) O1A 0.0368(19) 0.0280(18) 0.069(3) 0.0150(18) 0.0146(18) 0.0016(15) O2H 0.045(2) 0.0209(16) 0.067(3) 0.0037(16) 0.0185(19) 0.0039(14) N2B 0.041(2) 0.0234(18) 0.034(2) 0.0079(15) 0.0036(17) -0.0023(16) O2A 0.044(2) 0.0257(18) 0.110(4) 0.012(2) 0.030(3) -0.0045(16) C1A 0.033(2) 0.026(2) 0.057(3) 0.007(2) 0.016(2) 0.0010(18) C2A 0.031(2) 0.026(2) 0.051(3) 0.010(2) 0.015(2) 0.0009(17) C5A 0.035(2) 0.027(2) 0.046(3) 0.004(2) 0.015(2) 0.0033(18) O2B 0.068(3) 0.037(2) 0.041(2) 0.0143(17) -0.007(2) -0.005(2) O3B 0.053(2) 0.0292(17) 0.0356(18) -0.0017(14) 0.0065(16) 0.0080(16) C1B 0.038(3) 0.027(2) 0.044(3) 0.014(2) -0.003(2) -0.0062(18) C2B 0.047(3) 0.030(2) 0.036(2) 0.0063(19) 0.000(2) -0.003(2) C5B 0.059(3) 0.026(2) 0.035(3) 0.0004(18) -0.001(2) -0.002(2) C3A 0.036(3) 0.037(3) 0.075(4) 0.019(3) 0.024(3) 0.003(2) C4A 0.035(3) 0.043(3) 0.069(4) 0.014(3) 0.022(3) 0.006(2) C6A 0.039(3) 0.025(2) 0.062(4) 0.001(2) 0.016(3) 0.0046(19) O4A 0.055(3) 0.038(2) 0.125(5) 0.009(3) 0.053(3) 0.012(2) C6B 0.059(3) 0.025(2) 0.043(3) -0.003(2) 0.007(2) 0.001(2) O4B 0.118(5) 0.031(2) 0.051(3) -0.0050(19) -0.012(3) 0.004(3) C3B 0.083(5) 0.035(3) 0.039(3) 0.006(2) -0.012(3) -0.002(3) C4B 0.088(5) 0.037(3) 0.040(3) -0.002(2) -0.005(3) 0.004(3) C1C 0.037(2) 0.024(2) 0.039(2) 0.0040(18) 0.0129(19) 0.0018(17) C2C 0.034(2) 0.0226(19) 0.038(2) 0.0035(17) 0.0085(18) -0.0003(16) C3C 0.050(3) 0.027(2) 0.054(3) 0.002(2) 0.027(3) 0.003(2) N1C 0.037(2) 0.0234(17) 0.039(2) 0.0006(15) 0.0127(17) 0.0016(15) N2C 0.042(2) 0.0265(19) 0.042(2) 0.0060(17) 0.0138(19) 0.0019(16) C4C 0.052(3) 0.031(2) 0.049(3) 0.003(2) 0.024(3) 0.003(2) C5C 0.034(2) 0.026(2) 0.044(3) 0.0056(18) 0.015(2) 0.0007(17) C6C 0.033(2) 0.033(2) 0.050(3) 0.013(2) 0.011(2) 0.0002(19) O3C 0.070(3) 0.032(2) 0.079(3) 0.019(2) 0.039(3) 0.015(2) O4C 0.049(2) 0.038(2) 0.060(3) 0.0169(19) 0.025(2) 0.0058(17) O7H 0.027(4) 0.213(17) 0.097(9) 0.113(11) 0.018(5) 0.031(7) O8H 0.036(4) 0.028(4) 0.170(13) -0.010(6) 0.029(6) 0.006(3) O9H 0.047(2) 0.036(2) 0.051(2) 0.0027(17) 0.0133(18) 0.0002(17) O10H 0.091(5) 0.158(8) 0.114(6) 0.087(6) 0.053(4) 0.062(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O6H 2.308(3) . ? Tb1 O1C 2.352(3) . ? Tb1 O3B 2.364(4) . ? Tb1 O3A 2.369(4) . ? Tb1 O5H 2.375(4) . ? Tb1 O4H 2.437(4) . ? Tb1 N2A 2.646(4) . ? Tb1 N2B 2.655(4) . ? Tb1 N1C 2.699(4) . ? Tb2 O2H 2.336(4) . ? Tb2 O1A 2.339(4) . ? Tb2 O1B 2.351(4) . ? Tb2 O1C 2.377(3) . ? Tb2 O1H 2.389(4) . ? Tb2 O3H 2.459(4) . ? Tb2 O2C 2.584(4) . ? Tb2 N1B 2.637(4) . ? Tb2 N1A 2.640(4) . ? Tb2 C1C 2.846(5) . ? O3A C6A 1.263(7) . ? N2A C5A 1.323(6) . ? N2A N1A 1.342(5) . ? N1A C2A 1.323(6) . ? O1C C1C 1.300(6) . ? N1B C2B 1.323(7) . ? N1B N2B 1.349(6) . ? O2C C1C 1.242(6) . ? O1B C1B 1.245(7) . ? O1A C1A 1.267(6) . ? N2B C5B 1.325(7) . ? O2A C1A 1.227(6) . ? C1A C2A 1.507(7) . ? C2A C3A 1.401(7) . ? C5A C4A 1.395(8) . ? C5A C6A 1.516(7) . ? O2B C1B 1.250(7) . ? O3B C6B 1.245(7) . ? C1B C2B 1.511(7) . ? C2B C3B 1.404(9) . ? C5B C4B 1.395(8) . ? C5B C6B 1.521(8) . ? C3A C4A 1.358(8) . ? C6A O4A 1.226(7) . ? C6B O4B 1.233(7) . ? C3B C4B 1.382(9) . ? C1C C2C 1.483(7) . ? C2C N1C 1.330(6) . ? C2C C3C 1.391(7) . ? C3C C4C 1.367(8) . ? N1C N2C 1.358(6) . ? N2C C5C 1.320(7) . ? C4C C5C 1.411(7) . ? C5C C6C 1.536(7) . ? C6C O4C 1.232(7) . ? C6C O3C 1.244(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 O6H Tb1 O1C 135.01(13) . . ? O6H Tb1 O3B 77.31(13) . . ? O1C Tb1 O3B 134.18(13) . . ? O6H Tb1 O3A 79.81(13) . . ? O1C Tb1 O3A 134.44(13) . . ? O3B Tb1 O3A 70.91(15) . . ? O6H Tb1 O5H 84.02(14) . . ? O1C Tb1 O5H 81.52(14) . . ? O3B Tb1 O5H 141.92(14) . . ? O3A Tb1 O5H 73.31(16) . . ? O6H Tb1 O4H 82.60(13) . . ? O1C Tb1 O4H 80.52(13) . . ? O3B Tb1 O4H 72.00(14) . . ? O3A Tb1 O4H 141.55(15) . . ? O5H Tb1 O4H 138.16(14) . . ? O6H Tb1 N2A 140.97(13) . . ? O1C Tb1 N2A 73.98(12) . . ? O3B Tb1 N2A 100.06(14) . . ? O3A Tb1 N2A 63.09(12) . . ? O5H Tb1 N2A 74.50(14) . . ? O4H Tb1 N2A 134.34(13) . . ? O6H Tb1 N2B 137.13(13) . . ? O1C Tb1 N2B 73.21(13) . . ? O3B Tb1 N2B 63.33(13) . . ? O3A Tb1 N2B 101.36(16) . . ? O5H Tb1 N2B 137.94(14) . . ? O4H Tb1 N2B 70.11(14) . . ? N2A Tb1 N2B 66.57(13) . . ? O6H Tb1 N1C 72.92(13) . . ? O1C Tb1 N1C 62.18(12) . . ? O3B Tb1 N1C 134.68(14) . . ? O3A Tb1 N1C 133.63(15) . . ? O5H Tb1 N1C 67.24(14) . . ? O4H Tb1 N1C 70.95(14) . . ? N2A Tb1 N1C 124.52(13) . . ? N2B Tb1 N1C 124.16(14) . . ? O2H Tb2 O1A 80.06(14) . . ? O2H Tb2 O1B 83.25(15) . . ? O1A Tb2 O1B 72.47(15) . . ? O2H Tb2 O1C 130.33(14) . . ? O1A Tb2 O1C 134.21(13) . . ? O1B Tb2 O1C 134.39(13) . . ? O2H Tb2 O1H 84.11(16) . . ? O1A Tb2 O1H 143.48(15) . . ? O1B Tb2 O1H 73.14(15) . . ? O1C Tb2 O1H 80.17(14) . . ? O2H Tb2 O3H 76.78(15) . . ? O1A Tb2 O3H 72.80(17) . . ? O1B Tb2 O3H 142.30(15) . . ? O1C Tb2 O3H 81.67(14) . . ? O1H Tb2 O3H 134.61(17) . . ? O2H Tb2 O2C 77.55(13) . . ? O1A Tb2 O2C 136.92(16) . . ? O1B Tb2 O2C 139.17(15) . . ? O1C Tb2 O2C 52.80(12) . . ? O1H Tb2 O2C 69.34(16) . . ? O3H Tb2 O2C 66.52(16) . . ? O2H Tb2 N1B 144.32(15) . . ? O1A Tb2 N1B 100.92(15) . . ? O1B Tb2 N1B 63.71(13) . . ? O1C Tb2 N1B 73.85(12) . . ? O1H Tb2 N1B 74.12(16) . . ? O3H Tb2 N1B 138.07(14) . . ? O2C Tb2 N1B 118.56(13) . . ? O2H Tb2 N1A 137.65(14) . . ? O1A Tb2 N1A 63.38(13) . . ? O1B Tb2 N1A 103.84(14) . . ? O1C Tb2 N1A 73.09(12) . . ? O1H Tb2 N1A 138.15(15) . . ? O3H Tb2 N1A 72.69(14) . . ? O2C Tb2 N1A 114.67(13) . . ? N1B Tb2 N1A 67.90(13) . . ? O2H Tb2 C1C 103.37(15) . . ? O1A Tb2 C1C 142.01(15) . . ? O1B Tb2 C1C 145.29(15) . . ? O1C Tb2 C1C 26.96(13) . . ? O1H Tb2 C1C 73.74(15) . . ? O3H Tb2 C1C 71.36(16) . . ? O2C Tb2 C1C 25.87(12) . . ? N1B Tb2 C1C 97.32(13) . . ? N1A Tb2 C1C 93.96(13) . . ? C6A O3A Tb1 128.1(3) . . ? C5A N2A N1A 119.2(4) . . ? C5A N2A Tb1 116.4(3) . . ? N1A N2A Tb1 124.3(3) . . ? C2A N1A N2A 119.9(4) . . ? C2A N1A Tb2 115.4(3) . . ? N2A N1A Tb2 124.6(3) . . ? C1C O1C Tb1 129.1(3) . . ? C1C O1C Tb2 97.1(3) . . ? Tb1 O1C Tb2 133.69(15) . . ? C2B N1B N2B 120.0(4) . . ? C2B N1B Tb2 115.5(3) . . ? N2B N1B Tb2 124.3(3) . . ? C1C O2C Tb2 88.9(3) . . ? C1B O1B Tb2 128.3(3) . . ? C1A O1A Tb2 127.2(3) . . ? C5B N2B N1B 120.1(4) . . ? C5B N2B Tb1 115.3(3) . . ? N1B N2B Tb1 124.6(3) . . ? O2A C1A O1A 125.9(5) . . ? O2A C1A C2A 119.4(5) . . ? O1A C1A C2A 114.7(4) . . ? N1A C2A C3A 123.0(5) . . ? N1A C2A C1A 115.2(4) . . ? C3A C2A C1A 121.8(5) . . ? N2A C5A C4A 122.8(5) . . ? N2A C5A C6A 115.2(5) . . ? C4A C5A C6A 122.0(5) . . ? C6B O3B Tb1 127.9(3) . . ? O1B C1B O2B 126.5(5) . . ? O1B C1B C2B 116.7(5) . . ? O2B C1B C2B 116.7(5) . . ? N1B C2B C3B 122.3(5) . . ? N1B C2B C1B 115.4(5) . . ? C3B C2B C1B 122.2(5) . . ? N2B C5B C4B 122.6(5) . . ? N2B C5B C6B 115.5(5) . . ? C4B C5B C6B 121.9(5) . . ? C4A C3A C2A 116.7(5) . . ? C3A C4A C5A 118.2(5) . . ? O4A C6A O3A 126.2(5) . . ? O4A C6A C5A 118.1(5) . . ? O3A C6A C5A 115.6(5) . . ? O4B C6B O3B 126.6(5) . . ? O4B C6B C5B 117.4(5) . . ? O3B C6B C5B 115.9(5) . . ? C4B C3B C2B 117.5(6) . . ? C3B C4B C5B 117.5(6) . . ? O2C C1C O1C 121.1(4) . . ? O2C C1C C2C 121.3(5) . . ? O1C C1C C2C 117.5(4) . . ? O2C C1C Tb2 65.2(3) . . ? O1C C1C Tb2 56.0(2) . . ? C2C C1C Tb2 173.3(3) . . ? N1C C2C C3C 124.4(5) . . ? N1C C2C C1C 113.9(4) . . ? C3C C2C C1C 121.6(4) . . ? C4C C3C C2C 116.7(5) . . ? C2C N1C N2C 118.3(4) . . ? C2C N1C Tb1 116.8(3) . . ? N2C N1C Tb1 124.8(3) . . ? C5C N2C N1C 119.9(4) . . ? C3C C4C C5C 117.6(5) . . ? N2C C5C C4C 122.8(5) . . ? N2C C5C C6C 116.4(4) . . ? C4C C5C C6C 120.9(5) . . ? O4C C6C O3C 126.6(5) . . ? O4C C6C C5C 116.4(5) . . ? O3C C6C C5C 117.0(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.338 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.374 # Attachment '- 7_Dydcp.cif' data_770969 _database_code_depnum_ccdc_archive 'CCDC 770969' #TrackingRef '- 7_Dydcp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; '2(Dy 3+). 3(C6 N2 O4 H2 2-). 6(H2 O); 3(H2 O)' ; _chemical_formula_sum 'C18 H24 Dy2 N6 O21' _chemical_formula_weight 985.41 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8365(3) _cell_length_b 19.5914(5) _cell_length_c 15.0554(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.6320(10) _cell_angle_gamma 90.00 _cell_volume 3406.74(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9869 _cell_measurement_theta_min 2.499 _cell_measurement_theta_max 27.089 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.889 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1845 _exptl_absorpt_coefficient_mu 4.960 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1993 _exptl_absorpt_correction_T_max 0.6265 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006), based on the method developped by R. Blessing, Acta Cryst. A, 51, 33 (1995).' ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 138135 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 36.28 _reflns_number_total 16270 _reflns_number_gt 12175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _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. O7H and O8H have been refined with an 50% occupancy factor due to the observed low Fourier peak density and in order to get reasonable thermal parameters. Some solvent accessible voids are observed, due to the unaccurate location of the crystallization water molecules. ; _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^)+(0.0818P)^2^+5.4059P] 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 16270 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Dy1 Dy 0.789943(14) 0.017095(7) 0.806984(11) 0.02346(5) Uani 1 1 d . . . Dy2 Dy 0.670524(14) 0.224690(8) 0.746242(12) 0.02440(5) Uani 1 1 d . . . O5H O 0.9200(3) 0.05517(17) 0.9392(2) 0.0392(7) Uani 1 1 d . . . O6H O 0.8130(3) -0.08703(13) 0.87887(19) 0.0307(5) Uani 1 1 d . . . O4H O 0.5901(3) -0.01984(15) 0.7628(2) 0.0351(6) Uani 1 1 d . . . O3A O 0.9786(3) -0.01277(14) 0.7908(3) 0.0390(7) Uani 1 1 d . . . N2A N 0.9115(3) 0.11471(15) 0.7515(2) 0.0267(5) Uani 1 1 d . . . N1A N 0.8777(3) 0.18008(15) 0.7394(2) 0.0268(5) Uani 1 1 d . . . O1C O 0.6977(2) 0.12003(13) 0.82741(19) 0.0281(5) Uani 1 1 d . . . N1B N 0.6625(3) 0.12850(16) 0.6234(2) 0.0298(6) Uani 1 1 d . . . O2C O 0.6046(3) 0.19524(14) 0.8940(2) 0.0375(6) Uani 1 1 d . . . O1H O 0.4776(3) 0.18373(18) 0.7145(3) 0.0469(8) Uani 1 1 d . . . O3H O 0.8047(3) 0.26509(18) 0.8836(3) 0.0423(7) Uani 1 1 d . . . O1B O 0.5879(3) 0.25580(15) 0.5956(2) 0.0379(6) Uani 1 1 d . . . O1A O 0.7936(3) 0.30330(15) 0.7002(3) 0.0401(7) Uani 1 1 d . . . O2H O 0.5866(3) 0.32652(14) 0.7797(3) 0.0388(7) Uani 1 1 d . . . N2B N 0.6954(3) 0.06373(16) 0.6429(2) 0.0301(6) Uani 1 1 d . . . O2A O 0.9713(3) 0.34632(16) 0.7124(3) 0.0531(10) Uani 1 1 d . . . C1A C 0.9034(4) 0.2982(2) 0.7101(3) 0.0355(8) Uani 1 1 d . . . C2A C 0.9498(3) 0.22665(18) 0.7197(3) 0.0308(7) Uani 1 1 d . . . C5A C 1.0152(3) 0.09672(19) 0.7375(3) 0.0315(7) Uani 1 1 d . . . O2B O 0.5439(3) 0.24089(18) 0.4450(2) 0.0461(8) Uani 1 1 d . . . O3B O 0.7749(3) -0.06070(14) 0.6856(2) 0.0345(6) Uani 1 1 d . . . C1B C 0.5796(4) 0.2205(2) 0.5248(3) 0.0342(8) Uani 1 1 d . . . C2B C 0.6150(4) 0.1465(2) 0.5378(3) 0.0339(8) Uani 1 1 d . . . C5B C 0.6780(4) 0.01740(19) 0.5768(3) 0.0360(8) Uani 1 1 d . . . C3A C 1.0602(4) 0.2106(2) 0.7069(4) 0.0428(10) Uani 1 1 d . . . H3A H 1.1099 0.2442 0.6942 0.051 Uiso 1 1 calc R . . C4A C 1.0918(4) 0.1437(2) 0.7136(4) 0.0425(10) Uani 1 1 d . . . H4A H 1.1625 0.1298 0.7026 0.051 Uiso 1 1 calc R . . C6A C 1.0460(4) 0.0218(2) 0.7536(3) 0.0364(9) Uani 1 1 d . . . O4A O 1.1339(3) 0.0008(2) 0.7321(4) 0.0598(11) Uani 1 1 d . . . C6B C 0.7157(4) -0.0548(2) 0.6059(3) 0.0368(8) Uani 1 1 d . . . O4B O 0.6850(5) -0.10138(18) 0.5523(3) 0.0622(12) Uani 1 1 d . . . C3B C 0.5972(5) 0.1003(3) 0.4656(3) 0.0481(12) Uani 1 1 d . . . H3B H 0.5657 0.1141 0.4063 0.058 Uiso 1 1 calc R . . C4B C 0.6283(6) 0.0334(3) 0.4858(3) 0.0503(13) Uani 1 1 d . . . H4B H 0.6167 0.0001 0.4407 0.060 Uiso 1 1 calc R . . C1C C 0.6499(3) 0.13850(18) 0.8939(3) 0.0287(6) Uani 1 1 d . . . C2C C 0.6484(3) 0.08764(17) 0.9672(3) 0.0268(6) Uani 1 1 d . . . C3C C 0.6066(4) 0.1036(2) 1.0442(3) 0.0366(8) Uani 1 1 d . . . H3C H 0.5786 0.1469 1.0527 0.044 Uiso 1 1 calc R . . N1C N 0.6915(3) 0.02675(16) 0.9527(2) 0.0292(6) Uani 1 1 d . . . N2C N 0.6880(3) -0.02435(16) 1.0117(2) 0.0315(6) Uani 1 1 d . . . C4C C 0.6086(4) 0.0531(2) 1.1068(3) 0.0377(9) Uani 1 1 d . . . H4C H 0.5868 0.0614 1.1615 0.045 Uiso 1 1 calc R . . C5C C 0.6451(3) -0.01246(18) 1.0854(3) 0.0288(7) Uani 1 1 d . . . C6C C 0.6371(3) -0.0743(2) 1.1456(3) 0.0328(7) Uani 1 1 d . . . O3C O 0.6917(3) -0.12606(17) 1.1339(3) 0.0501(9) Uani 1 1 d . . . O4C O 0.5718(3) -0.06771(17) 1.2005(2) 0.0420(7) Uani 1 1 d . . . O7H O 0.2851(7) 0.2384(8) 0.6054(9) 0.122(6) Uani 0.50 1 d P . . O8H O 0.3630(7) 0.3590(4) 0.7578(9) 0.075(3) Uani 0.50 1 d P . . O9H O 0.6217(3) 0.37630(16) 0.4438(2) 0.0382(6) Uani 1 1 d . . . O10H O 0.4130(5) 0.3662(4) 0.5830(4) 0.103(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02561(8) 0.01395(7) 0.03073(8) 0.00210(5) 0.00599(6) 0.00119(5) Dy2 0.02444(8) 0.01516(7) 0.03374(9) 0.00624(5) 0.00664(6) 0.00132(5) O5H 0.0339(14) 0.0405(16) 0.0403(16) -0.0060(13) 0.0022(12) -0.0042(12) O6H 0.0423(15) 0.0157(10) 0.0335(13) 0.0014(9) 0.0070(11) 0.0002(10) O4H 0.0303(13) 0.0278(13) 0.0477(17) -0.0002(11) 0.0098(12) -0.0005(10) O3A 0.0336(14) 0.0199(12) 0.067(2) 0.0049(12) 0.0184(14) 0.0036(10) N2A 0.0256(13) 0.0181(12) 0.0375(15) 0.0016(10) 0.0091(11) 0.0011(10) N1A 0.0271(13) 0.0188(12) 0.0354(15) 0.0030(10) 0.0091(11) -0.0005(10) O1C 0.0350(13) 0.0174(10) 0.0354(13) 0.0056(9) 0.0157(10) 0.0037(9) N1B 0.0321(15) 0.0230(13) 0.0320(14) 0.0053(11) 0.0019(12) -0.0011(11) O2C 0.0484(17) 0.0211(12) 0.0480(17) 0.0044(11) 0.0214(14) 0.0087(11) O1H 0.0342(15) 0.0416(18) 0.062(2) 0.0214(16) 0.0043(14) -0.0089(13) O3H 0.0364(16) 0.0385(16) 0.0485(18) -0.0082(14) 0.0017(13) 0.0007(13) O1B 0.0475(17) 0.0260(13) 0.0383(15) 0.0099(11) 0.0056(13) 0.0020(12) O1A 0.0288(13) 0.0275(13) 0.066(2) 0.0173(13) 0.0138(13) 0.0022(11) O2H 0.0375(15) 0.0183(11) 0.063(2) 0.0043(12) 0.0153(14) 0.0035(10) N2B 0.0355(16) 0.0211(13) 0.0316(14) 0.0032(11) 0.0028(12) -0.0013(11) O2A 0.0391(17) 0.0235(14) 0.102(3) 0.0119(17) 0.0265(19) -0.0036(12) C1A 0.0325(18) 0.0225(16) 0.053(2) 0.0096(15) 0.0131(16) -0.0009(13) C2A 0.0271(16) 0.0216(15) 0.045(2) 0.0082(13) 0.0121(15) -0.0001(12) C5A 0.0294(16) 0.0240(15) 0.044(2) 0.0041(14) 0.0135(15) 0.0031(12) O2B 0.057(2) 0.0358(16) 0.0376(16) 0.0134(13) -0.0070(14) -0.0051(14) O3B 0.0429(16) 0.0248(12) 0.0346(14) -0.0016(10) 0.0057(12) 0.0065(11) C1B 0.0330(18) 0.0253(16) 0.040(2) 0.0103(14) -0.0009(15) -0.0046(13) C2B 0.040(2) 0.0250(16) 0.0332(17) 0.0072(13) -0.0007(15) -0.0017(14) C5B 0.048(2) 0.0228(16) 0.0336(18) 0.0014(13) 0.0015(16) 0.0003(15) C3A 0.0325(19) 0.0322(19) 0.068(3) 0.016(2) 0.021(2) 0.0019(15) C4A 0.0325(19) 0.034(2) 0.067(3) 0.017(2) 0.024(2) 0.0084(16) C6A 0.0342(19) 0.0242(16) 0.054(2) 0.0030(15) 0.0159(17) 0.0067(13) O4A 0.048(2) 0.0361(17) 0.108(4) 0.009(2) 0.044(2) 0.0130(16) C6B 0.048(2) 0.0235(16) 0.0369(19) -0.0008(14) 0.0058(17) 0.0014(15) O4B 0.097(3) 0.0284(16) 0.049(2) -0.0073(14) -0.010(2) 0.0032(19) C3B 0.066(3) 0.033(2) 0.037(2) 0.0055(17) -0.006(2) 0.002(2) C4B 0.076(4) 0.033(2) 0.034(2) -0.0004(17) -0.003(2) 0.004(2) C1C 0.0328(17) 0.0192(13) 0.0349(17) 0.0039(12) 0.0092(13) 0.0021(12) C2C 0.0302(16) 0.0186(13) 0.0330(16) 0.0020(11) 0.0099(13) 0.0004(11) C3C 0.049(2) 0.0213(15) 0.046(2) 0.0024(14) 0.0249(18) 0.0026(15) N1C 0.0315(15) 0.0222(13) 0.0350(15) 0.0009(11) 0.0097(12) 0.0021(11) N2C 0.0387(17) 0.0220(13) 0.0358(16) 0.0064(11) 0.0129(13) 0.0031(11) C4C 0.048(2) 0.0267(17) 0.045(2) 0.0028(15) 0.0251(19) 0.0044(16) C5C 0.0284(16) 0.0237(15) 0.0358(17) 0.0046(12) 0.0102(13) 0.0005(12) C6C 0.0273(16) 0.0300(17) 0.043(2) 0.0128(15) 0.0119(14) 0.0010(13) O3C 0.060(2) 0.0286(15) 0.070(2) 0.0171(15) 0.0335(19) 0.0132(14) O4C 0.0451(17) 0.0342(15) 0.0535(19) 0.0145(14) 0.0256(15) 0.0061(13) O7H 0.024(3) 0.218(14) 0.129(9) 0.139(10) 0.024(5) 0.029(6) O8H 0.034(3) 0.029(3) 0.166(10) -0.011(5) 0.032(5) 0.003(3) O9H 0.0421(16) 0.0321(14) 0.0420(15) 0.0006(12) 0.0130(13) -0.0008(12) O10H 0.090(4) 0.131(5) 0.101(4) 0.071(4) 0.050(3) 0.060(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O6H 2.297(3) . ? Dy1 O1C 2.345(3) . ? Dy1 O5H 2.356(3) . ? Dy1 O3B 2.356(3) . ? Dy1 O3A 2.371(3) . ? Dy1 O4H 2.424(3) . ? Dy1 N2A 2.637(3) . ? Dy1 N2B 2.642(3) . ? Dy1 N1C 2.707(3) . ? Dy2 O1A 2.327(3) . ? Dy2 O2H 2.332(3) . ? Dy2 O1B 2.346(3) . ? Dy2 O1H 2.369(3) . ? Dy2 O1C 2.373(2) . ? Dy2 O3H 2.447(3) . ? Dy2 O2C 2.579(3) . ? Dy2 N1B 2.627(3) . ? Dy2 N1A 2.626(3) . ? Dy2 C1C 2.844(4) . ? O3A C6A 1.267(5) . ? N2A C5A 1.337(5) . ? N2A N1A 1.342(4) . ? N1A C2A 1.327(5) . ? O1C C1C 1.304(4) . ? N1B C2B 1.336(5) . ? N1B N2B 1.341(4) . ? O2C C1C 1.234(4) . ? O1B C1B 1.255(6) . ? O1A C1A 1.279(5) . ? N2B C5B 1.329(5) . ? O2A C1A 1.234(5) . ? C1A C2A 1.501(5) . ? C2A C3A 1.399(6) . ? C5A C4A 1.394(6) . ? C5A C6A 1.519(5) . ? O2B C1B 1.250(5) . ? O3B C6B 1.256(5) . ? C1B C2B 1.510(6) . ? C2B C3B 1.394(7) . ? C5B C4B 1.404(6) . ? C5B C6B 1.519(6) . ? C3A C4A 1.360(6) . ? C3A H3A 0.9300 . ? C4A H4A 0.9300 . ? C6A O4A 1.227(5) . ? C6B O4B 1.219(5) . ? C3B C4B 1.377(7) . ? C3B H3B 0.9300 . ? C4B H4B 0.9300 . ? C1C C2C 1.490(5) . ? C2C N1C 1.334(5) . ? C2C C3C 1.392(5) . ? C3C C4C 1.363(6) . ? C3C H3C 0.9300 . ? N1C N2C 1.345(4) . ? N2C C5C 1.337(5) . ? C4C C5C 1.414(5) . ? C4C H4C 0.9300 . ? C5C C6C 1.529(5) . ? C6C O3C 1.235(5) . ? C6C O4C 1.255(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6H Dy1 O1C 135.44(10) . . ? O6H Dy1 O5H 83.96(11) . . ? O1C Dy1 O5H 81.59(11) . . ? O6H Dy1 O3B 76.82(10) . . ? O1C Dy1 O3B 134.40(10) . . ? O5H Dy1 O3B 141.69(11) . . ? O6H Dy1 O3A 79.15(10) . . ? O1C Dy1 O3A 134.53(10) . . ? O5H Dy1 O3A 73.07(12) . . ? O3B Dy1 O3A 70.96(12) . . ? O6H Dy1 O4H 82.66(10) . . ? O1C Dy1 O4H 80.70(10) . . ? O5H Dy1 O4H 138.12(12) . . ? O3B Dy1 O4H 71.98(11) . . ? O3A Dy1 O4H 141.50(11) . . ? O6H Dy1 N2A 140.94(10) . . ? O1C Dy1 N2A 73.73(9) . . ? O5H Dy1 N2A 74.75(11) . . ? O3B Dy1 N2A 100.21(11) . . ? O3A Dy1 N2A 63.59(9) . . ? O4H Dy1 N2A 134.21(10) . . ? O6H Dy1 N2B 136.88(10) . . ? O1C Dy1 N2B 73.21(10) . . ? O5H Dy1 N2B 138.21(11) . . ? O3B Dy1 N2B 63.51(10) . . ? O3A Dy1 N2B 101.84(12) . . ? O4H Dy1 N2B 70.03(11) . . ? N2A Dy1 N2B 66.54(10) . . ? O6H Dy1 N1C 73.02(10) . . ? O1C Dy1 N1C 62.51(9) . . ? O5H Dy1 N1C 67.08(11) . . ? O3B Dy1 N1C 134.51(11) . . ? O3A Dy1 N1C 133.02(12) . . ? O4H Dy1 N1C 71.08(11) . . ? N2A Dy1 N1C 124.59(10) . . ? N2B Dy1 N1C 124.36(11) . . ? O1A Dy2 O2H 79.74(11) . . ? O1A Dy2 O1B 72.27(12) . . ? O2H Dy2 O1B 83.07(12) . . ? O1A Dy2 O1H 143.38(11) . . ? O2H Dy2 O1H 84.04(13) . . ? O1B Dy2 O1H 73.33(12) . . ? O1A Dy2 O1C 134.60(10) . . ? O2H Dy2 O1C 130.13(11) . . ? O1B Dy2 O1C 134.71(10) . . ? O1H Dy2 O1C 80.07(11) . . ? O1A Dy2 O3H 72.84(13) . . ? O2H Dy2 O3H 76.65(12) . . ? O1B Dy2 O3H 142.12(12) . . ? O1H Dy2 O3H 134.36(13) . . ? O1C Dy2 O3H 81.63(11) . . ? O1A Dy2 O2C 137.09(12) . . ? O2H Dy2 O2C 77.40(10) . . ? O1B Dy2 O2C 138.73(12) . . ? O1H Dy2 O2C 68.78(12) . . ? O1C Dy2 O2C 52.76(9) . . ? O3H Dy2 O2C 66.82(12) . . ? O1A Dy2 N1B 101.17(12) . . ? O2H Dy2 N1B 144.48(11) . . ? O1B Dy2 N1B 64.05(10) . . ? O1H Dy2 N1B 74.32(13) . . ? O1C Dy2 N1B 73.89(9) . . ? O3H Dy2 N1B 138.05(11) . . ? O2C Dy2 N1B 118.38(10) . . ? O1A Dy2 N1A 63.77(10) . . ? O2H Dy2 N1A 137.59(10) . . ? O1B Dy2 N1A 104.12(11) . . ? O1H Dy2 N1A 138.30(12) . . ? O1C Dy2 N1A 73.13(9) . . ? O3H Dy2 N1A 72.64(11) . . ? O2C Dy2 N1A 114.87(10) . . ? N1B Dy2 N1A 67.94(10) . . ? O1A Dy2 C1C 142.39(12) . . ? O2H Dy2 C1C 103.05(11) . . ? O1B Dy2 C1C 145.19(11) . . ? O1H Dy2 C1C 73.31(11) . . ? O1C Dy2 C1C 27.07(10) . . ? O3H Dy2 C1C 71.49(12) . . ? O2C Dy2 C1C 25.71(9) . . ? N1B Dy2 C1C 97.36(10) . . ? N1A Dy2 C1C 94.22(10) . . ? C6A O3A Dy1 127.7(3) . . ? C5A N2A N1A 119.2(3) . . ? C5A N2A Dy1 116.2(2) . . ? N1A N2A Dy1 124.6(2) . . ? C2A N1A N2A 119.9(3) . . ? C2A N1A Dy2 115.6(2) . . ? N2A N1A Dy2 124.5(2) . . ? C1C O1C Dy1 129.2(2) . . ? C1C O1C Dy2 97.0(2) . . ? Dy1 O1C Dy2 133.65(12) . . ? C2B N1B N2B 120.1(3) . . ? C2B N1B Dy2 115.6(3) . . ? N2B N1B Dy2 124.1(2) . . ? C1C O2C Dy2 89.2(2) . . ? C1B O1B Dy2 128.0(3) . . ? C1A O1A Dy2 126.9(2) . . ? C5B N2B N1B 119.5(3) . . ? C5B N2B Dy1 115.4(2) . . ? N1B N2B Dy1 125.1(2) . . ? O2A C1A O1A 125.6(4) . . ? O2A C1A C2A 119.2(4) . . ? O1A C1A C2A 115.1(3) . . ? N1A C2A C3A 122.9(4) . . ? N1A C2A C1A 115.1(3) . . ? C3A C2A C1A 122.0(3) . . ? N2A C5A C4A 122.5(4) . . ? N2A C5A C6A 115.2(3) . . ? C4A C5A C6A 122.2(4) . . ? C6B O3B Dy1 127.8(3) . . ? O2B C1B O1B 126.0(4) . . ? O2B C1B C2B 117.2(4) . . ? O1B C1B C2B 116.8(4) . . ? N1B C2B C3B 122.7(4) . . ? N1B C2B C1B 115.1(4) . . ? C3B C2B C1B 122.2(4) . . ? N2B C5B C4B 122.8(4) . . ? N2B C5B C6B 115.7(4) . . ? C4B C5B C6B 121.5(4) . . ? C4A C3A C2A 117.1(4) . . ? C4A C3A H3A 121.4 . . ? C2A C3A H3A 121.4 . . ? C3A C4A C5A 118.2(4) . . ? C3A C4A H4A 120.9 . . ? C5A C4A H4A 120.9 . . ? O4A C6A O3A 126.2(4) . . ? O4A C6A C5A 118.0(4) . . ? O3A C6A C5A 115.8(3) . . ? O4B C6B O3B 125.9(4) . . ? O4B C6B C5B 118.7(4) . . ? O3B C6B C5B 115.4(4) . . ? C4B C3B C2B 117.3(4) . . ? C4B C3B H3B 121.3 . . ? C2B C3B H3B 121.3 . . ? C3B C4B C5B 117.5(4) . . ? C3B C4B H4B 121.2 . . ? C5B C4B H4B 121.2 . . ? O2C C1C O1C 120.8(3) . . ? O2C C1C C2C 121.7(3) . . ? O1C C1C C2C 117.4(3) . . ? O2C C1C Dy2 65.0(2) . . ? O1C C1C Dy2 55.88(17) . . ? C2C C1C Dy2 173.2(3) . . ? N1C C2C C3C 123.7(3) . . ? N1C C2C C1C 114.2(3) . . ? C3C C2C C1C 122.1(3) . . ? C4C C3C C2C 117.2(4) . . ? C4C C3C H3C 121.4 . . ? C2C C3C H3C 121.4 . . ? C2C N1C N2C 119.3(3) . . ? C2C N1C Dy1 116.3(2) . . ? N2C N1C Dy1 124.4(2) . . ? C5C N2C N1C 119.4(3) . . ? C3C C4C C5C 117.5(4) . . ? C3C C4C H4C 121.3 . . ? C5C C4C H4C 121.3 . . ? N2C C5C C4C 122.5(3) . . ? N2C C5C C6C 115.9(3) . . ? C4C C5C C6C 121.5(4) . . ? O3C C6C O4C 126.5(4) . . ? O3C C6C C5C 117.6(4) . . ? O4C C6C C5C 115.8(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 36.28 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.784 _refine_diff_density_min -1.396 _refine_diff_density_rms 0.389 # Attachment '- 8_Erdcp.cif' data_770970 _database_code_depnum_ccdc_archive 'CCDC 770970' #TrackingRef '- 8_Erdcp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; '2(Er 3+). 3(C6 N2 O4 H2 2-). 6(H2 O); 3(H2 O)' ; _chemical_formula_sum 'C18 H24 Er2 N6 O21' _chemical_formula_weight 994.93 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8162(8) _cell_length_b 19.4943(13) _cell_length_c 15.0763(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.854(3) _cell_angle_gamma 90.00 _cell_volume 3385.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9612 _cell_measurement_theta_min 2.502 _cell_measurement_theta_max 33.343 _exptl_crystal_description platelet _exptl_crystal_colour pink _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 5.010 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_T_max 0.6858 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006), based on the method developped by R. Blessing, Acta Cryst. A, 51, 33 (1995).' ; _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 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62837 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 33.32 _reflns_number_total 12985 _reflns_number_gt 9587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _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. O7H and O8H have been refined with an 50% occupancy factor due to the observed low Fourier peak density and in order to get reasonable thermal parameters. Some solvent accessible voids are observed, due to the unaccurate location of the crystallization water molecules. ; _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^)+(0.0760P)^2^+9.1810P] 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 12985 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1451 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Er1 Er 0.789407(19) 0.017616(10) 0.807443(16) 0.02761(7) Uani 1 1 d . . . Er2 Er 0.670569(19) 0.224561(10) 0.747414(16) 0.02726(7) Uani 1 1 d . . . O5H O 0.9192(4) 0.0550(2) 0.9384(3) 0.0425(9) Uani 1 1 d . . . O6H O 0.8108(4) -0.08583(18) 0.8788(3) 0.0342(8) Uani 1 1 d . . . O4H O 0.5907(4) -0.01868(19) 0.7639(3) 0.0378(9) Uani 1 1 d . . . O3A O 0.9761(4) -0.01283(19) 0.7925(4) 0.0427(10) Uani 1 1 d . . . N2A N 0.9103(4) 0.1145(2) 0.7534(3) 0.0301(8) Uani 1 1 d . . . N1A N 0.8765(4) 0.1805(2) 0.7419(3) 0.0300(8) Uani 1 1 d . . . O1C O 0.6980(3) 0.12011(17) 0.8274(3) 0.0304(7) Uani 1 1 d . . . N1B N 0.6626(4) 0.1293(2) 0.6264(3) 0.0324(9) Uani 1 1 d . . . O2C O 0.6034(4) 0.1964(2) 0.8928(3) 0.0431(10) Uani 1 1 d . . . O1H O 0.4781(4) 0.1840(2) 0.7152(4) 0.0514(12) Uani 1 1 d . . . O3H O 0.8036(4) 0.2644(2) 0.8844(3) 0.0430(10) Uani 1 1 d . . . O1B O 0.5878(4) 0.2569(2) 0.5989(3) 0.0402(9) Uani 1 1 d . . . O1A O 0.7926(4) 0.3038(2) 0.7033(3) 0.0426(10) Uani 1 1 d . . . O2H O 0.5875(4) 0.32583(19) 0.7790(3) 0.0411(9) Uani 1 1 d . . . N2B N 0.6951(4) 0.0643(2) 0.6451(3) 0.0327(9) Uani 1 1 d . . . O2A O 0.9705(4) 0.3470(2) 0.7155(4) 0.0575(14) Uani 1 1 d . . . C1A C 0.9019(5) 0.2991(3) 0.7130(5) 0.0380(12) Uani 1 1 d . . . C2A C 0.9493(5) 0.2272(3) 0.7227(4) 0.0342(11) Uani 1 1 d . . . C5A C 1.0143(5) 0.0971(3) 0.7400(4) 0.0353(11) Uani 1 1 d . . . O2B O 0.5425(5) 0.2419(2) 0.4481(3) 0.0483(11) Uani 1 1 d . . . O3B O 0.7750(4) -0.0607(2) 0.6879(3) 0.0381(9) Uani 1 1 d . . . C1B C 0.5790(5) 0.2216(3) 0.5276(4) 0.0366(12) Uani 1 1 d . . . C2B C 0.6146(5) 0.1472(3) 0.5403(4) 0.0375(12) Uani 1 1 d . . . C5B C 0.6774(6) 0.0180(3) 0.5796(4) 0.0396(13) Uani 1 1 d . . . C3A C 1.0592(6) 0.2110(3) 0.7102(5) 0.0464(15) Uani 1 1 d . . . H3A H 1.1091 0.2448 0.6979 0.056 Uiso 1 1 calc R . . C4A C 1.0911(5) 0.1443(3) 0.7165(5) 0.0461(15) Uani 1 1 d . . . H4A H 1.1620 0.1303 0.7055 0.055 Uiso 1 1 calc R . . C6A C 1.0446(5) 0.0214(3) 0.7546(5) 0.0400(13) Uani 1 1 d . . . O4A O 1.1332(5) 0.0006(3) 0.7348(5) 0.0635(15) Uani 1 1 d . . . C6B C 0.7154(6) -0.0547(3) 0.6086(4) 0.0392(12) Uani 1 1 d . . . O4B O 0.6853(6) -0.1014(2) 0.5548(4) 0.0627(15) Uani 1 1 d . . . C3B C 0.5966(7) 0.1010(3) 0.4693(5) 0.0486(16) Uani 1 1 d . . . H3B H 0.5651 0.1150 0.4100 0.058 Uiso 1 1 calc R . . C4B C 0.6268(7) 0.0336(3) 0.4889(5) 0.0519(17) Uani 1 1 d . . . H4B H 0.6141 0.0000 0.4440 0.062 Uiso 1 1 calc R . . C1C C 0.6492(5) 0.1386(3) 0.8934(4) 0.0339(10) Uani 1 1 d . . . C2C C 0.6478(5) 0.0883(3) 0.9667(4) 0.0340(11) Uani 1 1 d . . . C3C C 0.6057(6) 0.1047(3) 1.0432(4) 0.0425(13) Uani 1 1 d . . . H3C H 0.5772 0.1482 1.0511 0.051 Uiso 1 1 calc R . . N1C N 0.6918(4) 0.0280(2) 0.9511(3) 0.0360(10) Uani 1 1 d . . . N2C N 0.6871(5) -0.0240(2) 1.0117(4) 0.0370(10) Uani 1 1 d . . . C4C C 0.6079(6) 0.0539(3) 1.1064(5) 0.0455(14) Uani 1 1 d . . . H4C H 0.5862 0.0624 1.1610 0.055 Uiso 1 1 calc R . . C5C C 0.6445(5) -0.0121(3) 1.0852(4) 0.0361(11) Uani 1 1 d . . . O3C O 0.6929(5) -0.1257(2) 1.1341(4) 0.0593(14) Uani 1 1 d . . . O4C O 0.5726(4) -0.0677(2) 1.2003(3) 0.0485(11) Uani 1 1 d . . . O7H O 0.2857(8) 0.2414(9) 0.6069(11) 0.113(7) Uani 0.50 1 d P . . O8H O 0.3640(9) 0.3577(5) 0.7588(11) 0.075(4) Uani 0.50 1 d P . . O9H O 0.6225(4) 0.3771(2) 0.4443(3) 0.0436(9) Uani 1 1 d . . . O10H O 0.4137(7) 0.3668(4) 0.5819(5) 0.099(3) Uani 1 1 d . . . C6C C 0.6370(5) -0.0739(3) 1.1455(4) 0.0395(12) 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 Er1 0.02925(11) 0.01514(10) 0.03747(12) 0.00262(7) 0.00533(9) 0.00129(7) Er2 0.02685(11) 0.01678(10) 0.03818(12) 0.00677(7) 0.00731(9) 0.00143(7) O5H 0.035(2) 0.040(2) 0.049(2) -0.0032(18) 0.0030(18) -0.0032(17) O6H 0.046(2) 0.0159(15) 0.0408(19) 0.0025(14) 0.0102(17) 0.0031(14) O4H 0.0322(19) 0.0270(19) 0.053(2) -0.0005(16) 0.0067(17) -0.0024(14) O3A 0.036(2) 0.0224(18) 0.073(3) 0.0034(18) 0.019(2) 0.0026(15) N2A 0.029(2) 0.0213(18) 0.041(2) -0.0004(16) 0.0102(17) 0.0011(15) N1A 0.030(2) 0.0235(19) 0.037(2) 0.0035(16) 0.0102(17) -0.0011(16) O1C 0.0367(19) 0.0173(14) 0.0405(18) 0.0065(13) 0.0155(16) 0.0060(13) N1B 0.035(2) 0.0220(19) 0.038(2) 0.0062(17) 0.0027(18) -0.0007(16) O2C 0.056(3) 0.0233(18) 0.057(3) 0.0001(17) 0.027(2) 0.0038(17) O1H 0.035(2) 0.048(3) 0.068(3) 0.025(2) 0.005(2) -0.0091(19) O3H 0.038(2) 0.038(2) 0.050(2) -0.0084(18) 0.0026(19) 0.0014(17) O1B 0.048(2) 0.0260(18) 0.044(2) 0.0112(16) 0.0048(19) -0.0013(17) O1A 0.034(2) 0.0254(19) 0.070(3) 0.0136(19) 0.014(2) 0.0020(15) O2H 0.042(2) 0.0194(17) 0.063(3) 0.0047(17) 0.015(2) 0.0048(15) N2B 0.038(2) 0.024(2) 0.035(2) 0.0052(16) 0.0037(18) 0.0002(17) O2A 0.042(2) 0.025(2) 0.109(4) 0.010(2) 0.024(3) -0.0055(17) C1A 0.033(3) 0.024(2) 0.058(3) 0.012(2) 0.014(2) -0.001(2) C2A 0.029(2) 0.026(2) 0.050(3) 0.008(2) 0.013(2) 0.0029(18) C5A 0.036(3) 0.026(2) 0.046(3) 0.003(2) 0.014(2) 0.005(2) O2B 0.059(3) 0.035(2) 0.044(2) 0.0122(18) -0.005(2) -0.006(2) O3B 0.047(2) 0.0272(18) 0.040(2) -0.0006(15) 0.0091(18) 0.0069(16) C1B 0.036(3) 0.025(2) 0.045(3) 0.013(2) 0.000(2) -0.0028(19) C2B 0.044(3) 0.026(2) 0.039(3) 0.008(2) 0.001(2) -0.002(2) C5B 0.050(3) 0.026(3) 0.039(3) 0.002(2) 0.003(3) -0.004(2) C3A 0.036(3) 0.031(3) 0.078(5) 0.017(3) 0.026(3) 0.002(2) C4A 0.036(3) 0.038(3) 0.069(4) 0.019(3) 0.022(3) 0.007(2) C6A 0.040(3) 0.022(2) 0.060(4) 0.002(2) 0.016(3) 0.005(2) O4A 0.053(3) 0.038(2) 0.113(5) 0.006(3) 0.047(3) 0.014(2) C6B 0.048(3) 0.025(2) 0.044(3) 0.000(2) 0.008(3) 0.002(2) O4B 0.099(4) 0.028(2) 0.052(3) -0.005(2) -0.002(3) 0.003(3) C3B 0.064(4) 0.035(3) 0.040(3) 0.006(2) -0.003(3) 0.000(3) C4B 0.078(5) 0.032(3) 0.041(3) -0.001(2) 0.003(3) 0.005(3) C1C 0.034(3) 0.029(2) 0.039(3) 0.003(2) 0.009(2) 0.000(2) C2C 0.034(3) 0.026(2) 0.043(3) 0.004(2) 0.010(2) 0.0006(19) C3C 0.054(4) 0.027(3) 0.054(3) 0.001(2) 0.027(3) 0.001(2) N1C 0.034(2) 0.031(2) 0.044(3) -0.0055(19) 0.011(2) 0.0031(18) N2C 0.042(3) 0.026(2) 0.044(3) 0.0051(18) 0.012(2) 0.0024(18) C4C 0.059(4) 0.035(3) 0.051(3) 0.003(3) 0.028(3) 0.004(3) C5C 0.035(3) 0.027(2) 0.047(3) 0.006(2) 0.012(2) 0.001(2) O3C 0.070(3) 0.034(2) 0.082(4) 0.020(2) 0.034(3) 0.018(2) O4C 0.048(3) 0.041(2) 0.063(3) 0.017(2) 0.026(2) 0.0069(19) O7H 0.022(4) 0.196(16) 0.123(11) 0.128(12) 0.021(6) 0.025(7) O8H 0.034(5) 0.030(5) 0.164(13) -0.008(6) 0.029(6) 0.003(4) O9H 0.048(2) 0.036(2) 0.047(2) 0.0004(18) 0.0107(19) -0.0007(18) O10H 0.096(5) 0.121(6) 0.093(5) 0.062(5) 0.047(4) 0.056(5) C6C 0.031(3) 0.034(3) 0.055(3) 0.015(2) 0.013(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O6H 2.273(4) . ? Er1 O1C 2.322(3) . ? Er1 O5H 2.331(4) . ? Er1 O3B 2.339(4) . ? Er1 O3A 2.343(4) . ? Er1 O4H 2.399(4) . ? Er1 N2A 2.606(4) . ? Er1 N2B 2.617(4) . ? Er1 N1C 2.678(5) . ? Er2 O2H 2.301(4) . ? Er2 O1A 2.310(4) . ? Er2 O1B 2.323(4) . ? Er2 O1C 2.352(3) . ? Er2 O1H 2.354(4) . ? Er2 O3H 2.428(4) . ? Er2 O2C 2.552(4) . ? Er2 N1B 2.590(5) . ? Er2 N1A 2.599(4) . ? Er2 C1C 2.822(5) . ? O3A C6A 1.279(7) . ? N2A C5A 1.332(7) . ? N2A N1A 1.347(6) . ? N1A C2A 1.328(7) . ? O1C C1C 1.308(6) . ? N1B N2B 1.336(6) . ? N1B C2B 1.341(7) . ? O2C C1C 1.249(7) . ? O1B C1B 1.261(8) . ? O1A C1A 1.270(7) . ? N2B C5B 1.320(7) . ? O2A C1A 1.232(7) . ? C1A C2A 1.504(7) . ? C2A C3A 1.390(8) . ? C5A C4A 1.393(8) . ? C5A C6A 1.522(7) . ? O2B C1B 1.245(7) . ? O3B C6B 1.250(7) . ? C1B C2B 1.511(8) . ? C2B C3B 1.378(9) . ? C5B C4B 1.398(9) . ? C5B C6B 1.521(8) . ? C3A C4A 1.351(8) . ? C3A H3A 0.9300 . ? C4A H4A 0.9300 . ? C6A O4A 1.219(7) . ? C6B O4B 1.218(7) . ? C3B C4B 1.378(9) . ? C3B H3B 0.9300 . ? C4B H4B 0.9300 . ? C1C C2C 1.480(8) . ? C2C N1C 1.327(7) . ? C2C C3C 1.390(8) . ? C3C C4C 1.371(9) . ? C3C H3C 0.9300 . ? N1C N2C 1.375(7) . ? N2C C5C 1.336(8) . ? C4C C5C 1.416(8) . ? C4C H4C 0.9300 . ? C5C C6C 1.523(8) . ? O3C C6C 1.238(8) . ? O4C C6C 1.248(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 O6H Er1 O1C 135.09(14) . . ? O6H Er1 O5H 83.89(15) . . ? O1C Er1 O5H 81.87(15) . . ? O6H Er1 O3B 76.53(14) . . ? O1C Er1 O3B 134.82(14) . . ? O5H Er1 O3B 141.10(15) . . ? O6H Er1 O3A 79.19(15) . . ? O1C Er1 O3A 134.84(13) . . ? O5H Er1 O3A 72.81(17) . . ? O3B Er1 O3A 70.71(16) . . ? O6H Er1 O4H 82.35(14) . . ? O1C Er1 O4H 80.46(14) . . ? O5H Er1 O4H 137.99(16) . . ? O3B Er1 O4H 72.41(15) . . ? O3A Er1 O4H 141.62(15) . . ? O6H Er1 N2A 141.25(14) . . ? O1C Er1 N2A 73.73(13) . . ? O5H Er1 N2A 74.62(15) . . ? O3B Er1 N2A 100.57(15) . . ? O3A Er1 N2A 63.91(13) . . ? O4H Er1 N2A 134.39(14) . . ? O6H Er1 N2B 136.95(14) . . ? O1C Er1 N2B 73.03(14) . . ? O5H Er1 N2B 138.27(15) . . ? O3B Er1 N2B 64.12(14) . . ? O3A Er1 N2B 102.27(16) . . ? O4H Er1 N2B 70.12(15) . . ? N2A Er1 N2B 66.70(14) . . ? O6H Er1 N1C 72.98(14) . . ? O1C Er1 N1C 62.22(13) . . ? O5H Er1 N1C 67.15(15) . . ? O3B Er1 N1C 134.59(15) . . ? O3A Er1 N1C 132.89(17) . . ? O4H Er1 N1C 70.87(15) . . ? N2A Er1 N1C 124.22(14) . . ? N2B Er1 N1C 124.04(15) . . ? O2H Er2 O1A 78.95(15) . . ? O2H Er2 O1B 81.88(16) . . ? O1A Er2 O1B 72.35(16) . . ? O2H Er2 O1C 130.80(15) . . ? O1A Er2 O1C 134.66(14) . . ? O1B Er2 O1C 135.21(14) . . ? O2H Er2 O1H 83.89(17) . . ? O1A Er2 O1H 143.27(16) . . ? O1B Er2 O1H 73.25(16) . . ? O1C Er2 O1H 80.33(15) . . ? O2H Er2 O3H 77.01(16) . . ? O1A Er2 O3H 72.78(17) . . ? O1B Er2 O3H 141.97(16) . . ? O1C Er2 O3H 81.44(15) . . ? O1H Er2 O3H 134.08(18) . . ? O2H Er2 O2C 77.21(14) . . ? O1A Er2 O2C 136.47(16) . . ? O1B Er2 O2C 137.90(16) . . ? O1C Er2 O2C 53.63(12) . . ? O1H Er2 O2C 68.54(17) . . ? O3H Er2 O2C 66.68(16) . . ? O2H Er2 N1B 144.12(15) . . ? O1A Er2 N1B 101.74(16) . . ? O1B Er2 N1B 64.78(14) . . ? O1C Er2 N1B 73.72(13) . . ? O1H Er2 N1B 74.45(18) . . ? O3H Er2 N1B 138.04(15) . . ? O2C Er2 N1B 118.77(14) . . ? O2H Er2 N1A 137.36(15) . . ? O1A Er2 N1A 64.07(14) . . ? O1B Er2 N1A 104.81(15) . . ? O1C Er2 N1A 72.95(13) . . ? O1H Er2 N1A 138.68(17) . . ? O3H Er2 N1A 72.49(15) . . ? O2C Er2 N1A 115.37(14) . . ? N1B Er2 N1A 68.19(14) . . ? O2H Er2 C1C 103.41(16) . . ? O1A Er2 C1C 142.35(16) . . ? O1B Er2 C1C 145.25(16) . . ? O1C Er2 C1C 27.40(14) . . ? O1H Er2 C1C 73.24(16) . . ? O3H Er2 C1C 71.31(16) . . ? O2C Er2 C1C 26.26(14) . . ? N1B Er2 C1C 97.37(15) . . ? N1A Er2 C1C 94.33(15) . . ? C6A O3A Er1 127.9(4) . . ? C5A N2A N1A 118.8(4) . . ? C5A N2A Er1 116.8(3) . . ? N1A N2A Er1 124.4(3) . . ? C2A N1A N2A 119.7(4) . . ? C2A N1A Er2 115.9(3) . . ? N2A N1A Er2 124.4(3) . . ? C1C O1C Er1 129.2(3) . . ? C1C O1C Er2 96.8(3) . . ? Er1 O1C Er2 133.93(16) . . ? N2B N1B C2B 119.3(5) . . ? N2B N1B Er2 124.6(3) . . ? C2B N1B Er2 115.9(4) . . ? C1C O2C Er2 89.0(3) . . ? C1B O1B Er2 127.6(3) . . ? C1A O1A Er2 127.1(3) . . ? C5B N2B N1B 120.1(5) . . ? C5B N2B Er1 115.1(3) . . ? N1B N2B Er1 124.7(3) . . ? O2A C1A O1A 126.5(5) . . ? O2A C1A C2A 118.3(5) . . ? O1A C1A C2A 115.2(5) . . ? N1A C2A C3A 122.9(5) . . ? N1A C2A C1A 114.5(5) . . ? C3A C2A C1A 122.6(5) . . ? N2A C5A C4A 123.1(5) . . ? N2A C5A C6A 114.9(5) . . ? C4A C5A C6A 122.0(5) . . ? C6B O3B Er1 127.2(4) . . ? O2B C1B O1B 126.3(5) . . ? O2B C1B C2B 117.1(6) . . ? O1B C1B C2B 116.7(5) . . ? N1B C2B C3B 122.8(5) . . ? N1B C2B C1B 114.7(5) . . ? C3B C2B C1B 122.5(5) . . ? N2B C5B C4B 123.0(5) . . ? N2B C5B C6B 115.8(5) . . ? C4B C5B C6B 121.2(5) . . ? C4A C3A C2A 117.7(5) . . ? C4A C3A H3A 121.2 . . ? C2A C3A H3A 121.2 . . ? C3A C4A C5A 117.7(6) . . ? C3A C4A H4A 121.1 . . ? C5A C4A H4A 121.1 . . ? O4A C6A O3A 126.8(5) . . ? O4A C6A C5A 118.3(6) . . ? O3A C6A C5A 114.7(5) . . ? O4B C6B O3B 125.8(6) . . ? O4B C6B C5B 118.7(6) . . ? O3B C6B C5B 115.4(5) . . ? C2B C3B C4B 117.9(6) . . ? C2B C3B H3B 121.0 . . ? C4B C3B H3B 121.0 . . ? C3B C4B C5B 116.8(6) . . ? C3B C4B H4B 121.6 . . ? C5B C4B H4B 121.6 . . ? O2C C1C O1C 120.5(5) . . ? O2C C1C C2C 121.7(5) . . ? O1C C1C C2C 117.8(5) . . ? O2C C1C Er2 64.7(3) . . ? O1C C1C Er2 55.8(2) . . ? C2C C1C Er2 173.4(4) . . ? N1C C2C C3C 125.3(5) . . ? N1C C2C C1C 112.6(5) . . ? C3C C2C C1C 122.2(5) . . ? C4C C3C C2C 117.1(5) . . ? C4C C3C H3C 121.4 . . ? C2C C3C H3C 121.4 . . ? C2C N1C N2C 117.4(5) . . ? C2C N1C Er1 117.9(4) . . ? N2C N1C Er1 124.7(3) . . ? C5C N2C N1C 120.1(5) . . ? C3C C4C C5C 117.3(6) . . ? C3C C4C H4C 121.4 . . ? C5C C4C H4C 121.4 . . ? N2C C5C C4C 122.4(5) . . ? N2C C5C C6C 116.1(5) . . ? C4C C5C C6C 121.5(5) . . ? O3C C6C O4C 126.5(5) . . ? O3C C6C C5C 117.2(5) . . ? O4C C6C C5C 116.3(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 33.32 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.990 _refine_diff_density_min -2.130 _refine_diff_density_rms 0.238 # Attachment '- 9_Ludcp.cif' data_770971 _database_code_depnum_ccdc_archive 'CCDC 770971' #TrackingRef '- 9_Ludcp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; '2(Lu 3+). 3(C6 N2 O4 H2 2-). 6(H2 O); 3(H2 O)' ; _chemical_formula_sum 'C18 H24 Lu2 N6 O21' _chemical_formula_weight 1010.35 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' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7980(7) _cell_length_b 19.4168(12) _cell_length_c 14.8932(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.041(3) _cell_angle_gamma 90.00 _cell_volume 3323.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9569 _cell_measurement_theta_min 2.255 _cell_measurement_theta_max 29.554 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2290 _exptl_absorpt_coefficient_mu 5.996 _exptl_absorpt_correction_type 'empirical (SADABS)' _exptl_absorpt_correction_T_min 0.1137 _exptl_absorpt_correction_T_max 0.5339 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006), based on the method developped by R. Blessing, Acta Cryst. A, 51, 33 (1995).' ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 122645 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 30.51 _reflns_number_total 10139 _reflns_number_gt 8908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _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. O7H and O8H have been refined with an 50% occupancy factor due to the observed low Fourier peak density and in order to get reasonable thermal parameters. Some solvent accessible voids are observed, due to the unaccurate location of the crystallization water molecules. ; _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^)+(0.0688P)^2^+12.1299P] 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 SHELXL _refine_ls_extinction_coef 0.00170(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10139 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 Lu1 Lu 0.789080(16) 0.016114(9) 0.805557(13) 0.02459(7) Uani 1 1 d . . . Lu2 Lu 0.671339(16) 0.222099(9) 0.742938(14) 0.02486(7) Uani 1 1 d . . . O5H O 0.9183(3) 0.0537(2) 0.9358(3) 0.0373(8) Uani 1 1 d . . . O6H O 0.8129(3) -0.08530(17) 0.8792(2) 0.0300(7) Uani 1 1 d . . . O4H O 0.5930(3) -0.02006(19) 0.7641(3) 0.0340(8) Uani 1 1 d . . . O3A O 0.9737(4) -0.01551(19) 0.7894(3) 0.0402(9) Uani 1 1 d . . . N2A N 0.9086(4) 0.1120(2) 0.7495(3) 0.0288(8) Uani 1 1 d . . . N1A N 0.8745(4) 0.1781(2) 0.7370(3) 0.0281(8) Uani 1 1 d . . . O1C O 0.6989(3) 0.11847(17) 0.8237(2) 0.0263(6) Uani 1 1 d . . . N1B N 0.6622(4) 0.1270(2) 0.6220(3) 0.0305(8) Uani 1 1 d . . . O2C O 0.6051(4) 0.1954(2) 0.8899(3) 0.0385(8) Uani 1 1 d . . . O1H O 0.4810(3) 0.1822(2) 0.7101(3) 0.0434(10) Uani 1 1 d . . . O3H O 0.8041(4) 0.2610(2) 0.8804(3) 0.0417(9) Uani 1 1 d . . . O1B O 0.5894(4) 0.2547(2) 0.5938(3) 0.0373(8) Uani 1 1 d . . . O1A O 0.7903(3) 0.3015(2) 0.6980(3) 0.0405(9) Uani 1 1 d . . . O2H O 0.5888(4) 0.32190(19) 0.7744(3) 0.0384(8) Uani 1 1 d . . . N2B N 0.6954(4) 0.0612(2) 0.6424(3) 0.0306(8) Uani 1 1 d . . . O2A O 0.9674(4) 0.3450(2) 0.7086(4) 0.0552(13) Uani 1 1 d . . . C1A C 0.8995(5) 0.2969(3) 0.7072(4) 0.0356(11) Uani 1 1 d . . . C2A C 0.9464(5) 0.2245(3) 0.7164(4) 0.0332(10) Uani 1 1 d . . . C5A C 1.0109(5) 0.0940(3) 0.7346(4) 0.0324(10) Uani 1 1 d . . . O2B O 0.5438(4) 0.2402(2) 0.4415(3) 0.0467(10) Uani 1 1 d . . . O3B O 0.7728(4) -0.0634(2) 0.6882(3) 0.0372(8) Uani 1 1 d . . . C1B C 0.5794(5) 0.2194(3) 0.5226(4) 0.0327(10) Uani 1 1 d . . . C2B C 0.6150(5) 0.1447(3) 0.5358(4) 0.0352(10) Uani 1 1 d . . . C5B C 0.6780(6) 0.0145(3) 0.5754(4) 0.0372(12) Uani 1 1 d . . . C3A C 1.0570(5) 0.2082(3) 0.7021(5) 0.0448(15) Uani 1 1 d . . . H3A H 1.1066 0.2420 0.6887 0.054 Uiso 1 1 calc R . . C4A C 1.0881(5) 0.1404(3) 0.7087(5) 0.0430(13) Uani 1 1 d . . . H4A H 1.1581 0.1256 0.6965 0.052 Uiso 1 1 calc R . . C6A C 1.0417(5) 0.0187(3) 0.7517(5) 0.0386(12) Uani 1 1 d . . . O4A O 1.1303(5) -0.0030(3) 0.7310(5) 0.0627(16) Uani 1 1 d . . . C6B C 0.7156(6) -0.0581(3) 0.6066(4) 0.0384(11) Uani 1 1 d . . . O4B O 0.6868(6) -0.1055(2) 0.5514(3) 0.0645(16) Uani 1 1 d . . . C3B C 0.5971(7) 0.0978(3) 0.4624(4) 0.0489(16) Uani 1 1 d . . . H3B H 0.5652 0.1117 0.4023 0.059 Uiso 1 1 calc R . . C4B C 0.6287(8) 0.0302(3) 0.4832(4) 0.0527(17) Uani 1 1 d . . . H4B H 0.6177 -0.0035 0.4377 0.063 Uiso 1 1 calc R . . C1C C 0.6506(4) 0.1378(2) 0.8906(4) 0.0293(9) Uani 1 1 d . . . C2C C 0.6496(4) 0.0873(2) 0.9654(4) 0.0295(9) Uani 1 1 d . . . C3C C 0.6076(5) 0.1047(3) 1.0426(4) 0.0381(11) Uani 1 1 d . . . H3C H 0.5797 0.1487 1.0502 0.046 Uiso 1 1 calc R . . N1C N 0.6932(4) 0.0260(2) 0.9510(3) 0.0305(8) Uani 1 1 d . . . N2C N 0.6893(4) -0.0251(2) 1.0127(3) 0.0340(9) Uani 1 1 d . . . C4C C 0.6094(6) 0.0539(3) 1.1071(4) 0.0400(12) Uani 1 1 d . . . H4C H 0.5875 0.0626 1.1622 0.048 Uiso 1 1 calc R . . C5C C 0.6461(5) -0.0122(3) 1.0858(4) 0.0315(10) Uani 1 1 d . . . O3C O 0.6942(5) -0.1263(2) 1.1375(4) 0.0528(12) Uani 1 1 d . . . O4C O 0.5729(4) -0.0671(2) 1.2027(3) 0.0444(10) Uani 1 1 d . . . O7H O 0.2862(8) 0.2393(10) 0.6035(10) 0.103(7) Uani 0.50 1 d P . . O8H O 0.3635(8) 0.3541(5) 0.7554(11) 0.071(4) Uani 0.50 1 d P . . O9H O 0.6195(4) 0.3770(2) 0.4412(3) 0.0409(9) Uani 1 1 d . . . O10H O 0.4140(6) 0.3664(5) 0.5797(5) 0.097(3) Uani 1 1 d . . . C6C C 0.6377(5) -0.0742(3) 1.1485(4) 0.0356(11) 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 Lu1 0.02652(11) 0.01488(10) 0.03177(11) 0.00207(6) 0.00534(7) 0.00134(6) Lu2 0.02467(11) 0.01618(10) 0.03371(12) 0.00569(6) 0.00654(7) 0.00131(6) O5H 0.0319(18) 0.037(2) 0.041(2) -0.0057(16) 0.0023(15) -0.0033(15) O6H 0.0404(19) 0.0166(14) 0.0333(17) 0.0006(12) 0.0084(14) 0.0004(13) O4H 0.0292(17) 0.0283(18) 0.045(2) 0.0008(15) 0.0093(15) -0.0010(13) O3A 0.0343(19) 0.0232(17) 0.067(3) 0.0057(16) 0.0199(19) 0.0056(14) N2A 0.0275(18) 0.0216(18) 0.038(2) 0.0019(15) 0.0091(16) 0.0004(14) N1A 0.0265(18) 0.0199(17) 0.039(2) 0.0036(15) 0.0087(15) -0.0001(14) O1C 0.0310(16) 0.0182(14) 0.0322(16) 0.0045(12) 0.0123(13) 0.0036(12) N1B 0.033(2) 0.0229(18) 0.034(2) 0.0047(15) 0.0029(16) 0.0014(15) O2C 0.048(2) 0.0239(17) 0.048(2) 0.0027(15) 0.0181(18) 0.0058(15) O1H 0.0300(18) 0.040(2) 0.059(3) 0.0202(19) 0.0062(17) -0.0058(16) O3H 0.040(2) 0.034(2) 0.048(2) -0.0062(17) 0.0026(17) 0.0007(17) O1B 0.046(2) 0.0262(17) 0.0388(19) 0.0104(15) 0.0072(16) 0.0026(15) O1A 0.0315(18) 0.0263(18) 0.064(3) 0.0125(17) 0.0122(18) 0.0001(14) O2H 0.0372(19) 0.0209(16) 0.060(2) 0.0057(16) 0.0179(18) 0.0044(14) N2B 0.034(2) 0.0230(18) 0.033(2) 0.0030(15) 0.0032(16) -0.0006(15) O2A 0.040(2) 0.0241(19) 0.107(4) 0.011(2) 0.027(2) -0.0032(16) C1A 0.032(2) 0.023(2) 0.055(3) 0.009(2) 0.016(2) 0.0003(18) C2A 0.028(2) 0.025(2) 0.049(3) 0.0082(19) 0.013(2) 0.0003(17) C5A 0.031(2) 0.026(2) 0.042(3) 0.0041(19) 0.0121(19) 0.0023(18) O2B 0.057(3) 0.036(2) 0.038(2) 0.0144(17) -0.0071(19) -0.0039(19) O3B 0.050(2) 0.0264(17) 0.0329(18) 0.0003(14) 0.0056(16) 0.0090(16) C1B 0.033(2) 0.025(2) 0.036(2) 0.0091(18) -0.0014(19) -0.0044(17) C2B 0.040(3) 0.026(2) 0.036(2) 0.0061(19) 0.002(2) -0.0040(19) C5B 0.050(3) 0.023(2) 0.033(2) 0.0012(18) -0.001(2) 0.000(2) C3A 0.032(3) 0.032(3) 0.076(4) 0.020(3) 0.024(3) 0.004(2) C4A 0.032(3) 0.038(3) 0.064(4) 0.016(3) 0.022(3) 0.008(2) C6A 0.034(3) 0.025(2) 0.058(3) 0.003(2) 0.014(2) 0.0051(19) O4A 0.052(3) 0.037(2) 0.113(5) 0.013(3) 0.049(3) 0.015(2) C6B 0.049(3) 0.025(2) 0.039(3) -0.0014(19) 0.006(2) 0.002(2) O4B 0.107(4) 0.028(2) 0.044(2) -0.0048(18) -0.012(3) 0.002(2) C3B 0.068(4) 0.033(3) 0.036(3) 0.005(2) -0.009(3) -0.001(3) C4B 0.080(5) 0.035(3) 0.035(3) -0.001(2) -0.005(3) 0.002(3) C1C 0.030(2) 0.022(2) 0.037(2) 0.0011(17) 0.0105(18) 0.0012(17) C2C 0.031(2) 0.022(2) 0.037(2) 0.0028(17) 0.0100(18) -0.0011(16) C3C 0.050(3) 0.025(2) 0.046(3) 0.002(2) 0.025(2) 0.003(2) N1C 0.031(2) 0.0252(18) 0.036(2) 0.0021(16) 0.0087(16) 0.0017(15) N2C 0.041(2) 0.0233(18) 0.040(2) 0.0051(16) 0.0139(19) 0.0041(16) C4C 0.051(3) 0.030(2) 0.046(3) 0.003(2) 0.025(3) 0.003(2) C5C 0.031(2) 0.025(2) 0.040(3) 0.0057(18) 0.0110(19) -0.0011(17) O3C 0.063(3) 0.034(2) 0.071(3) 0.018(2) 0.034(3) 0.016(2) O4C 0.047(2) 0.036(2) 0.057(3) 0.0168(19) 0.025(2) 0.0055(17) O7H 0.023(4) 0.185(16) 0.105(10) 0.107(11) 0.020(5) 0.027(7) O8H 0.032(4) 0.033(5) 0.150(12) -0.018(6) 0.024(6) 0.005(4) O9H 0.042(2) 0.036(2) 0.046(2) 0.0021(17) 0.0128(17) -0.0010(17) O10H 0.077(4) 0.128(7) 0.096(5) 0.066(5) 0.039(4) 0.050(4) C6C 0.032(2) 0.030(2) 0.045(3) 0.013(2) 0.010(2) -0.0001(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 Lu1 O6H 2.240(3) . ? Lu1 O1C 2.299(3) . ? Lu1 O5H 2.299(4) . ? Lu1 O3B 2.307(4) . ? Lu1 O3A 2.328(4) . ? Lu1 O4H 2.362(4) . ? Lu1 N2B 2.585(4) . ? Lu1 N2A 2.586(4) . ? Lu1 N1C 2.668(4) . ? Lu2 O2H 2.265(4) . ? Lu2 O1A 2.284(4) . ? Lu2 O1B 2.302(4) . ? Lu2 O1H 2.320(4) . ? Lu2 O1C 2.329(3) . ? Lu2 O3H 2.402(4) . ? Lu2 O2C 2.538(4) . ? Lu2 N1B 2.566(4) . ? Lu2 N1A 2.565(4) . ? Lu2 C1C 2.797(5) . ? O3A C6A 1.266(7) . ? N2A C5A 1.322(6) . ? N2A N1A 1.345(5) . ? N1A C2A 1.321(6) . ? O1C C1C 1.311(6) . ? N1B C2B 1.324(7) . ? N1B N2B 1.349(6) . ? O2C C1C 1.239(6) . ? O1B C1B 1.246(7) . ? O1A C1A 1.268(7) . ? N2B C5B 1.330(7) . ? O2A C1A 1.227(7) . ? C1A C2A 1.506(7) . ? C2A C3A 1.404(7) . ? C5A C4A 1.395(7) . ? C5A C6A 1.514(7) . ? O2B C1B 1.253(6) . ? O3B C6B 1.255(7) . ? C1B C2B 1.511(7) . ? C2B C3B 1.401(8) . ? C5B C4B 1.399(8) . ? C5B C6B 1.519(7) . ? C3A C4A 1.365(8) . ? C3A H3A 0.9300 . ? C4A H4A 0.9300 . ? C6A O4A 1.231(7) . ? C6B O4B 1.229(7) . ? C3B C4B 1.381(9) . ? C3B H3B 0.9300 . ? C4B H4B 0.9300 . ? C1C C2C 1.485(7) . ? C2C N1C 1.333(6) . ? C2C C3C 1.393(7) . ? C3C C4C 1.373(8) . ? C3C H3C 0.9300 . ? N1C N2C 1.360(6) . ? N2C C5C 1.326(7) . ? C4C C5C 1.414(8) . ? C4C H4C 0.9300 . ? C5C C6C 1.540(7) . ? O3C C6C 1.243(7) . ? O4C C6C 1.239(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 O6H Lu1 O1C 135.46(13) . . ? O6H Lu1 O5H 83.10(14) . . ? O1C Lu1 O5H 82.13(14) . . ? O6H Lu1 O3B 76.23(13) . . ? O1C Lu1 O3B 134.92(13) . . ? O5H Lu1 O3B 141.01(15) . . ? O6H Lu1 O3A 78.57(14) . . ? O1C Lu1 O3A 135.15(13) . . ? O5H Lu1 O3A 73.31(16) . . ? O3B Lu1 O3A 70.43(16) . . ? O6H Lu1 O4H 82.73(14) . . ? O1C Lu1 O4H 80.56(13) . . ? O5H Lu1 O4H 137.60(15) . . ? O3B Lu1 O4H 72.19(15) . . ? O3A Lu1 O4H 141.15(15) . . ? O6H Lu1 N2B 137.53(13) . . ? O1C Lu1 N2B 72.93(13) . . ? O5H Lu1 N2B 138.36(15) . . ? O3B Lu1 N2B 64.54(13) . . ? O3A Lu1 N2B 101.76(16) . . ? O4H Lu1 N2B 70.71(14) . . ? O6H Lu1 N2A 140.70(14) . . ? O1C Lu1 N2A 73.48(12) . . ? O5H Lu1 N2A 74.80(15) . . ? O3B Lu1 N2A 101.30(15) . . ? O3A Lu1 N2A 64.22(13) . . ? O4H Lu1 N2A 134.69(14) . . ? N2B Lu1 N2A 66.49(14) . . ? O6H Lu1 N1C 72.26(13) . . ? O1C Lu1 N1C 63.26(12) . . ? O5H Lu1 N1C 67.28(14) . . ? O3B Lu1 N1C 133.25(15) . . ? O3A Lu1 N1C 132.94(16) . . ? O4H Lu1 N1C 70.35(14) . . ? N2B Lu1 N1C 124.71(14) . . ? N2A Lu1 N1C 124.92(13) . . ? O2H Lu2 O1A 78.70(14) . . ? O2H Lu2 O1B 81.80(16) . . ? O1A Lu2 O1B 71.58(16) . . ? O2H Lu2 O1H 83.59(16) . . ? O1A Lu2 O1H 142.44(15) . . ? O1B Lu2 O1H 73.29(15) . . ? O2H Lu2 O1C 130.48(14) . . ? O1A Lu2 O1C 135.31(13) . . ? O1B Lu2 O1C 135.65(13) . . ? O1H Lu2 O1C 80.58(13) . . ? O2H Lu2 O3H 77.43(16) . . ? O1A Lu2 O3H 73.25(17) . . ? O1B Lu2 O3H 141.91(15) . . ? O1H Lu2 O3H 134.30(17) . . ? O1C Lu2 O3H 81.00(14) . . ? O2H Lu2 O2C 76.50(14) . . ? O1A Lu2 O2C 136.02(16) . . ? O1B Lu2 O2C 138.09(15) . . ? O1H Lu2 O2C 69.03(15) . . ? O1C Lu2 O2C 54.01(12) . . ? O3H Lu2 O2C 66.27(15) . . ? O2H Lu2 N1B 144.04(15) . . ? O1A Lu2 N1B 102.22(16) . . ? O1B Lu2 N1B 65.08(14) . . ? O1H Lu2 N1B 74.13(16) . . ? O1C Lu2 N1B 73.70(12) . . ? O3H Lu2 N1B 137.84(14) . . ? O2C Lu2 N1B 119.07(13) . . ? O2H Lu2 N1A 137.82(14) . . ? O1A Lu2 N1A 64.81(13) . . ? O1B Lu2 N1A 104.53(15) . . ? O1H Lu2 N1A 138.49(16) . . ? O1C Lu2 N1A 72.96(12) . . ? O3H Lu2 N1A 72.53(15) . . ? O2C Lu2 N1A 115.67(13) . . ? N1B Lu2 N1A 68.12(14) . . ? O2H Lu2 C1C 102.73(15) . . ? O1A Lu2 C1C 142.57(16) . . ? O1B Lu2 C1C 145.84(15) . . ? O1H Lu2 C1C 73.62(15) . . ? O1C Lu2 C1C 27.75(13) . . ? O3H Lu2 C1C 70.72(15) . . ? O2C Lu2 C1C 26.28(13) . . ? N1B Lu2 C1C 97.67(14) . . ? N1A Lu2 C1C 94.61(14) . . ? C6A O3A Lu1 127.5(3) . . ? C5A N2A N1A 119.0(4) . . ? C5A N2A Lu1 116.7(3) . . ? N1A N2A Lu1 124.3(3) . . ? C2A N1A N2A 119.7(4) . . ? C2A N1A Lu2 115.8(3) . . ? N2A N1A Lu2 124.5(3) . . ? C1C O1C Lu1 129.0(3) . . ? C1C O1C Lu2 96.4(3) . . ? Lu1 O1C Lu2 134.50(15) . . ? C2B N1B N2B 120.1(4) . . ? C2B N1B Lu2 115.8(3) . . ? N2B N1B Lu2 124.0(3) . . ? C1C O2C Lu2 88.6(3) . . ? C1B O1B Lu2 127.5(3) . . ? C1A O1A Lu2 126.7(3) . . ? C5B N2B N1B 119.3(4) . . ? C5B N2B Lu1 115.8(3) . . ? N1B N2B Lu1 125.0(3) . . ? O2A C1A O1A 126.3(5) . . ? O2A C1A C2A 118.9(5) . . ? O1A C1A C2A 114.8(5) . . ? N1A C2A C3A 123.3(5) . . ? N1A C2A C1A 114.6(4) . . ? C3A C2A C1A 122.1(5) . . ? N2A C5A C4A 123.6(5) . . ? N2A C5A C6A 114.9(5) . . ? C4A C5A C6A 121.5(5) . . ? C6B O3B Lu1 127.8(3) . . ? O1B C1B O2B 126.2(5) . . ? O1B C1B C2B 116.6(5) . . ? O2B C1B C2B 117.2(5) . . ? N1B C2B C3B 122.9(5) . . ? N1B C2B C1B 114.8(5) . . ? C3B C2B C1B 122.2(5) . . ? N2B C5B C4B 123.2(5) . . ? N2B C5B C6B 114.8(5) . . ? C4B C5B C6B 122.1(5) . . ? C4A C3A C2A 116.8(5) . . ? C4A C3A H3A 121.6 . . ? C2A C3A H3A 121.6 . . ? C3A C4A C5A 117.4(5) . . ? C3A C4A H4A 121.3 . . ? C5A C4A H4A 121.3 . . ? O4A C6A O3A 126.2(5) . . ? O4A C6A C5A 118.3(5) . . ? O3A C6A C5A 115.5(5) . . ? O4B C6B O3B 126.4(5) . . ? O4B C6B C5B 118.2(5) . . ? O3B C6B C5B 115.4(5) . . ? C4B C3B C2B 117.2(5) . . ? C4B C3B H3B 121.4 . . ? C2B C3B H3B 121.4 . . ? C3B C4B C5B 117.3(6) . . ? C3B C4B H4B 121.4 . . ? C5B C4B H4B 121.4 . . ? O2C C1C O1C 120.8(5) . . ? O2C C1C C2C 121.7(5) . . ? O1C C1C C2C 117.4(4) . . ? O2C C1C Lu2 65.1(3) . . ? O1C C1C Lu2 55.8(2) . . ? C2C C1C Lu2 173.1(3) . . ? N1C C2C C3C 124.9(5) . . ? N1C C2C C1C 113.6(4) . . ? C3C C2C C1C 121.6(4) . . ? C4C C3C C2C 116.8(5) . . ? C4C C3C H3C 121.6 . . ? C2C C3C H3C 121.6 . . ? C2C N1C N2C 118.0(4) . . ? C2C N1C Lu1 116.4(3) . . ? N2C N1C Lu1 125.5(3) . . ? C5C N2C N1C 119.6(4) . . ? C3C C4C C5C 116.9(5) . . ? C3C C4C H4C 121.5 . . ? C5C C4C H4C 121.5 . . ? N2C C5C C4C 123.3(5) . . ? N2C C5C C6C 116.1(5) . . ? C4C C5C C6C 120.6(5) . . ? O4C C6C O3C 127.1(5) . . ? O4C C6C C5C 116.3(5) . . ? O3C C6C C5C 116.6(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.413 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.432