Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Prof. David Parker' _publ_contact_author_address ;Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE ; _publ_contact_author_email David.Parker@durham.ac.uk _publ_contact_author_phone '0191 334 2033' _publ_contact_author_fax '0191 384 4737' _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_year ? _ccdc_journal_depnumber ? _publ_section_title_footnote ; . ; loop_ _publ_author_name _publ_author_address K.Senanayake ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; A.L.Thompson ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; J.A.K.Howard ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; M.Botta ;Dipartimento di Scienze dell'Ambiente e della Vita, Universit\`a del Piemonte Orientale "Amadeo Avogadro", Via Bellini 25/G, I-15100, Alessandria, Italy. ; D.Parker ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; _publ_section_title ; Synthesis and Characterisation of Dimeric Eight-coordinate Lanthanide(III) Complexes of a Macrocyclic Tribenzylphosphinate Ligand ; _publ_section_abstract ; The macrocyclic ligand 1,4,7,10-tetraazacyclododecane-1,4, 7-triyl(methylenebenzyl-phosphinic acid) H~3~L^3^, has been prepared and its complexes with Eu, Gd and Tb(III) studied by NMR, relaxometry, luminescence and single crystal X-ray crystallography. In solution and in the crystal, the complexes have eight-coordinate metal centres which form dimetallic dimers with bridging phosphinate groups linking the two twisted square antiprismatic coordination polyhedra. A single stereoisomer crystallises from solution with an RRR and SSS configuration at the P centres in each sub-unit. The relaxivity of [GdL~3~]~2~ is low (1.9 Mm^-1^ s^-1^, 298 K, 20 MHz), consistent with the absence of any proximate water molecules. The terbium dimer possesses a relatively long excited state lifetime (2.47 ms, 298 K). ; #============================================================================== data_[Gd.L^3^]~2~.10H~2~O _database_code_depnum_ccdc_archive 'CCDC 618886' #============================================================================== _chemical_name_systematic ; bis((\m~2~-1-4-7-10-tetra-azacyclododecane-1,4,7,10-tetrayl-methyl- (trimethylene-tris(phenylphosphinato)))-gadolinium(III)) decahydrate ; _chemical_name_common ; bis((mu!2$-1-4-7-10-tetra-azacyclododecane-1,4,7,10-tetrayl- methyl-(trimethylene-tris(phenylphosphinato)))-gadolinium(iii)) decahydrate ; _chemical_melting_point 'not measured' _chemical_formula_moiety 'C64 H88 Gd2 N8 O12 P6, 10(O H2)' _chemical_formula_sum 'C64 H108 Gd2 N8 O22 P6' _chemical_formula_weight 1841.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.6618(7) _cell_length_b 15.1330(6) _cell_length_c 30.2751(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.0290(10) _cell_angle_gamma 90.00 _cell_volume 7576.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9348 _cell_measurement_theta_min 2.361 _cell_measurement_theta_max 27.462 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3768 _exptl_absorpt_coefficient_mu 1.939 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.7693 _exptl_absorpt_correction_T_max 0.9621 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.0100 0.00 0.00 -1.00 0.0100 1.00 1.00 0.00 0.0700 -1.00 -1.00 0.00 0.0700 1.00 -1.00 0.00 0.0700 -1.00 1.00 0.00 0.0700 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 4 sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.44 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 31846 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8657 _reflns_number_gt 6503 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0148P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8657 _refine_ls_number_parameters 496 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0473 _refine_ls_wR_factor_gt 0.0418 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.006 _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 0.308915(8) 0.699684(9) 0.596277(4) 0.01212(4) Uani 1 1 d . . . P1 P 0.15553(4) 0.68422(4) 0.50965(2) 0.01303(15) Uani 1 1 d . . . P2 P 0.27689(4) 0.48045(5) 0.61870(2) 0.01542(16) Uani 1 1 d . . . P3 P 0.50467(4) 0.66970(5) 0.63977(3) 0.01646(16) Uani 1 1 d . . . N1 N 0.16387(13) 0.77711(13) 0.58893(7) 0.0142(5) Uani 1 1 d . . . N2 N 0.21608(13) 0.63192(14) 0.65165(7) 0.0149(5) Uani 1 1 d . . . N3 N 0.37263(13) 0.71872(14) 0.68019(7) 0.0144(5) Uani 1 1 d . . . N4 N 0.31662(13) 0.86154(14) 0.62161(7) 0.0149(5) Uani 1 1 d . . . H4C H 0.3591 0.8841 0.6090 0.018 Uiso 1 1 calc R . . C1 C 0.10633(16) 0.72255(17) 0.61096(9) 0.0162(6) Uani 1 1 d . . . H1A H 0.0884 0.6732 0.5918 0.019 Uiso 1 1 calc R . . H1B H 0.0593 0.7579 0.6151 0.019 Uiso 1 1 calc R . . C2 C 0.14381(16) 0.68758(18) 0.65570(9) 0.0176(6) Uani 1 1 d . . . H2A H 0.1593 0.7369 0.6754 0.021 Uiso 1 1 calc R . . H2B H 0.1040 0.6529 0.6689 0.021 Uiso 1 1 calc R . . C3 C 0.26233(17) 0.61805(18) 0.69670(9) 0.0180(6) Uani 1 1 d . . . H3A H 0.2962 0.5661 0.6959 0.022 Uiso 1 1 calc R . . H3B H 0.2245 0.6071 0.7180 0.022 Uiso 1 1 calc R . . C4 C 0.31495(16) 0.6963(2) 0.71223(8) 0.0188(6) Uani 1 1 d . . . H4A H 0.2808 0.7471 0.7159 0.023 Uiso 1 1 calc R . . H4B H 0.3449 0.6829 0.7410 0.023 Uiso 1 1 calc R . . C5 C 0.40115(16) 0.81085(18) 0.68833(9) 0.0176(6) Uani 1 1 d . . . H5A H 0.4502 0.8198 0.6746 0.021 Uiso 1 1 calc R . . H5B H 0.4141 0.8203 0.7201 0.021 Uiso 1 1 calc R . . C6 C 0.33804(17) 0.87745(18) 0.66976(9) 0.0174(6) Uani 1 1 d . . . H6A H 0.2902 0.8718 0.6849 0.021 Uiso 1 1 calc R . . H6B H 0.3591 0.9369 0.6746 0.021 Uiso 1 1 calc R . . C7 C 0.24628(16) 0.91411(18) 0.60173(9) 0.0181(6) Uani 1 1 d . . . H7A H 0.2488 0.9218 0.5701 0.022 Uiso 1 1 calc R . . H7B H 0.2475 0.9721 0.6155 0.022 Uiso 1 1 calc R . . C8 C 0.16879(16) 0.86705(17) 0.60886(9) 0.0160(6) Uani 1 1 d . . . H8A H 0.1655 0.8624 0.6405 0.019 Uiso 1 1 calc R . . H8B H 0.1230 0.9018 0.5957 0.019 Uiso 1 1 calc R . . C9 C 0.13517(16) 0.78431(16) 0.54068(8) 0.0144(6) Uani 1 1 d . . . H9A H 0.1615 0.8342 0.5284 0.017 Uiso 1 1 calc R . . H9B H 0.0774 0.7956 0.5368 0.017 Uiso 1 1 calc R . . C10 C 0.19023(16) 0.54330(17) 0.63394(9) 0.0171(6) Uani 1 1 d . . . H10A H 0.1504 0.5502 0.6080 0.021 Uiso 1 1 calc R . . H10B H 0.1652 0.5110 0.6563 0.021 Uiso 1 1 calc R . . C11 C 0.44334(16) 0.65823(19) 0.68582(9) 0.0184(6) Uani 1 1 d . . . H11A H 0.4246 0.5977 0.6871 0.022 Uiso 1 1 calc R . . H11B H 0.4764 0.6713 0.7137 0.022 Uiso 1 1 calc R . . C12 C 0.06354(16) 0.61870(18) 0.50083(9) 0.0200(7) Uani 1 1 d . . . H12A H 0.0613 0.5805 0.5264 0.024 Uiso 1 1 calc R . . H12B H 0.0174 0.6581 0.4991 0.024 Uiso 1 1 calc R . . C13 C 0.05668(16) 0.56249(18) 0.45931(9) 0.0179(6) Uani 1 1 d . . . C14 C 0.00563(17) 0.5877(2) 0.42154(10) 0.0256(7) Uani 1 1 d . . . H14 H -0.0251 0.6389 0.4221 0.031 Uiso 1 1 calc R . . C15 C 0.00022(19) 0.5374(2) 0.38319(11) 0.0340(9) Uani 1 1 d . . . H15 H -0.0340 0.5552 0.3582 0.041 Uiso 1 1 calc R . . C16 C 0.0449(2) 0.4611(2) 0.38155(11) 0.0378(9) Uani 1 1 d . . . H16 H 0.0411 0.4275 0.3557 0.045 Uiso 1 1 calc R . . C17 C 0.0952(2) 0.4354(2) 0.41868(11) 0.0325(8) Uani 1 1 d . . . H17 H 0.1253 0.3838 0.4180 0.039 Uiso 1 1 calc R . . C18 C 0.10157(18) 0.48582(19) 0.45725(10) 0.0224(7) Uani 1 1 d . . . H18 H 0.1364 0.4679 0.4820 0.027 Uiso 1 1 calc R . . C19 C 0.23855(17) 0.42565(18) 0.56707(9) 0.0199(7) Uani 1 1 d . . . H19A H 0.2075 0.3744 0.5740 0.024 Uiso 1 1 calc R . . H19B H 0.2020 0.4656 0.5495 0.024 Uiso 1 1 calc R . . C20 C 0.30273(17) 0.39612(19) 0.53925(9) 0.0183(6) Uani 1 1 d . . . C21 C 0.32484(17) 0.3087(2) 0.53701(10) 0.0283(7) Uani 1 1 d . . . H21 H 0.3005 0.2667 0.5534 0.034 Uiso 1 1 calc R . . C22 C 0.38285(19) 0.2822(2) 0.51064(11) 0.0350(9) Uani 1 1 d . . . H22 H 0.3961 0.2226 0.5092 0.042 Uiso 1 1 calc R . . C23 C 0.42099(18) 0.3429(2) 0.48663(10) 0.0281(8) Uani 1 1 d . . . H23 H 0.4599 0.3249 0.4689 0.034 Uiso 1 1 calc R . . C24 C 0.4006(2) 0.4310(2) 0.48924(10) 0.0327(8) Uani 1 1 d . . . H24 H 0.4265 0.4730 0.4736 0.039 Uiso 1 1 calc R . . C25 C 0.3417(2) 0.4572(2) 0.51507(10) 0.0291(8) Uani 1 1 d . . . H25 H 0.3281 0.5167 0.5162 0.035 Uiso 1 1 calc R . . C26 C 0.53229(17) 0.55862(17) 0.62597(9) 0.0176(6) Uani 1 1 d . . . H26A H 0.4853 0.5304 0.6098 0.021 Uiso 1 1 calc R . . H26B H 0.5736 0.5621 0.6061 0.021 Uiso 1 1 calc R . . C27 C 0.56333(17) 0.50017(18) 0.66482(9) 0.0184(6) Uani 1 1 d . . . C28 C 0.51958(18) 0.42518(19) 0.67402(10) 0.0217(7) Uani 1 1 d . . . H28 H 0.4694 0.4145 0.6578 0.026 Uiso 1 1 calc R . . C29 C 0.54975(19) 0.3666(2) 0.70690(10) 0.0276(8) Uani 1 1 d . . . H29 H 0.5204 0.3163 0.7122 0.033 Uiso 1 1 calc R . . C30 C 0.6234(2) 0.3826(2) 0.73188(10) 0.0280(8) Uani 1 1 d . . . H30 H 0.6436 0.3432 0.7541 0.034 Uiso 1 1 calc R . . C31 C 0.66690(19) 0.4575(2) 0.72372(10) 0.0260(7) Uani 1 1 d . . . H31 H 0.7162 0.4687 0.7407 0.031 Uiso 1 1 calc R . . C32 C 0.63724(18) 0.51592(19) 0.69037(9) 0.0209(7) Uani 1 1 d . . . H32 H 0.6669 0.5660 0.6850 0.025 Uiso 1 1 calc R . . O1 O 0.21956(11) 0.63317(11) 0.53904(6) 0.0151(4) Uani 1 1 d . . . O2 O 0.33708(11) 0.55117(11) 0.60882(6) 0.0152(4) Uani 1 1 d . . . O3 O 0.44748(10) 0.70494(13) 0.60072(6) 0.0165(4) Uani 1 1 d . . . O4 O 0.17627(10) 0.71301(11) 0.46481(6) 0.0146(4) Uani 1 1 d . . . O5 O 0.30431(11) 0.41358(12) 0.65385(6) 0.0207(5) Uani 1 1 d . . . O6 O 0.57963(11) 0.72353(12) 0.65346(6) 0.0223(5) Uani 1 1 d . . . O1W O 0.67163(14) 0.85527(15) 0.70176(8) 0.0294(5) Uani 1 1 d D . . H1WA H 0.6457(16) 0.8169(17) 0.6880(9) 0.044 Uiso 1 1 d D . . H1WB H 0.7114(13) 0.866(2) 0.6900(10) 0.044 Uiso 1 1 d D . . O2W O 0.70962(14) 0.6798(2) 0.60946(8) 0.0486(7) Uani 1 1 d D . . H2WA H 0.692(2) 0.672(3) 0.5835(5) 0.073 Uiso 1 1 d D . . H2WB H 0.6717(15) 0.697(3) 0.6221(10) 0.073 Uiso 1 1 d D . . O3W O 0.85725(14) 0.73815(15) 0.65698(9) 0.0390(6) Uani 1 1 d D . . H3WA H 0.8143(13) 0.7152(19) 0.6465(12) 0.058 Uiso 1 1 d D . . H3WB H 0.8475(19) 0.7912(9) 0.6573(12) 0.058 Uiso 1 1 d D . . O4W O 0.5744(2) 0.98629(18) 0.73341(10) 0.0613(9) Uani 1 1 d D . . H4WA H 0.604(2) 0.948(2) 0.7265(15) 0.092 Uiso 1 1 d D . . H4WB H 0.551(4) 0.969(4) 0.754(2) 0.092 Uiso 0.50 1 d PD A 1 H4WC H 0.593(4) 1.0341(17) 0.728(3) 0.092 Uiso 0.50 1 d PD B 2 O5W O 0.9170(2) 0.6583(2) 0.73708(9) 0.0731(10) Uani 1 1 d D . . H5WA H 0.890(2) 0.671(3) 0.7137(9) 0.110 Uiso 1 1 d D . . H5WB H 0.919(6) 0.6048(10) 0.739(2) 0.110 Uiso 0.50 1 d PD C 1 H5WC H 0.9637(14) 0.654(7) 0.7322(19) 0.110 Uiso 0.50 1 d PD D 2 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 0.01337(6) 0.01215(6) 0.01096(6) 0.00059(7) 0.00193(4) 0.00029(7) P1 0.0129(4) 0.0126(4) 0.0136(4) 0.0004(3) 0.0016(3) -0.0018(3) P2 0.0172(4) 0.0135(4) 0.0154(4) 0.0015(3) 0.0015(3) 0.0002(3) P3 0.0153(4) 0.0166(4) 0.0173(4) -0.0004(3) 0.0015(3) 0.0017(3) N1 0.0169(12) 0.0128(13) 0.0133(12) 0.0009(9) 0.0038(10) -0.0004(9) N2 0.0172(13) 0.0137(12) 0.0142(13) 0.0008(10) 0.0032(10) 0.0011(10) N3 0.0151(12) 0.0152(13) 0.0133(12) -0.0008(9) 0.0030(9) 0.0009(9) N4 0.0144(12) 0.0178(13) 0.0128(12) -0.0014(10) 0.0033(10) 0.0007(10) C1 0.0148(14) 0.0170(16) 0.0179(15) -0.0021(11) 0.0066(12) -0.0004(11) C2 0.0180(14) 0.0184(16) 0.0182(15) 0.0002(12) 0.0095(12) 0.0003(12) C3 0.0215(16) 0.0218(16) 0.0114(15) 0.0046(12) 0.0055(12) 0.0033(13) C4 0.0227(15) 0.0213(15) 0.0125(14) -0.0020(13) 0.0026(11) 0.0021(14) C5 0.0191(14) 0.0184(16) 0.0148(14) -0.0031(13) -0.0002(11) -0.0002(13) C6 0.0209(16) 0.0139(15) 0.0175(16) -0.0044(12) 0.0020(12) -0.0017(12) C7 0.0207(16) 0.0129(15) 0.0206(16) -0.0008(12) 0.0018(12) 0.0015(12) C8 0.0204(16) 0.0128(14) 0.0150(15) -0.0018(12) 0.0030(12) 0.0053(12) C9 0.0133(14) 0.0140(15) 0.0155(14) -0.0005(11) -0.0002(11) 0.0014(11) C10 0.0192(16) 0.0169(15) 0.0161(15) 0.0013(12) 0.0060(12) -0.0034(12) C11 0.0197(16) 0.0214(16) 0.0135(15) -0.0019(12) -0.0006(12) 0.0014(13) C12 0.0146(15) 0.0202(16) 0.0258(17) -0.0021(13) 0.0041(13) -0.0042(12) C13 0.0151(15) 0.0179(15) 0.0208(16) 0.0031(12) 0.0029(12) -0.0088(12) C14 0.0149(16) 0.0272(18) 0.0336(19) 0.0095(15) -0.0009(14) -0.0069(13) C15 0.0269(19) 0.050(2) 0.0219(18) 0.0101(17) -0.0080(15) -0.0228(17) C16 0.047(2) 0.045(2) 0.0231(19) -0.0113(17) 0.0099(17) -0.0310(19) C17 0.039(2) 0.0215(18) 0.040(2) -0.0054(16) 0.0165(17) -0.0090(15) C18 0.0233(17) 0.0217(16) 0.0224(17) 0.0035(13) 0.0037(13) -0.0038(13) C19 0.0205(16) 0.0179(15) 0.0204(16) -0.0007(13) -0.0007(13) 0.0007(12) C20 0.0171(15) 0.0204(16) 0.0162(16) -0.0001(12) -0.0032(12) 0.0003(12) C21 0.0287(17) 0.0216(17) 0.0369(19) 0.0052(16) 0.0125(14) 0.0041(15) C22 0.037(2) 0.025(2) 0.046(2) 0.0051(16) 0.0151(17) 0.0142(15) C23 0.0213(17) 0.043(2) 0.0204(17) 0.0018(15) 0.0043(13) 0.0058(15) C24 0.043(2) 0.035(2) 0.0223(18) 0.0011(15) 0.0100(16) -0.0100(16) C25 0.046(2) 0.0208(17) 0.0217(18) -0.0022(14) 0.0093(15) -0.0006(15) C26 0.0186(15) 0.0174(15) 0.0168(15) -0.0015(12) 0.0027(12) 0.0026(12) C27 0.0201(16) 0.0193(16) 0.0168(15) -0.0034(12) 0.0064(12) 0.0070(12) C28 0.0194(16) 0.0228(16) 0.0246(17) 0.0002(13) 0.0094(13) 0.0035(13) C29 0.0290(19) 0.0278(18) 0.0290(19) 0.0037(15) 0.0152(15) 0.0032(14) C30 0.040(2) 0.0285(18) 0.0163(17) 0.0031(14) 0.0072(15) 0.0128(16) C31 0.0302(19) 0.0297(18) 0.0168(16) -0.0094(14) -0.0024(14) 0.0098(15) C32 0.0232(17) 0.0181(15) 0.0209(17) -0.0060(13) 0.0012(13) 0.0038(13) O1 0.0175(10) 0.0139(10) 0.0136(10) 0.0010(8) 0.0013(8) 0.0008(8) O2 0.0153(10) 0.0156(10) 0.0148(10) 0.0023(8) 0.0027(8) 0.0014(8) O3 0.0166(10) 0.0167(10) 0.0165(10) 0.0015(9) 0.0031(8) 0.0002(9) O4 0.0159(10) 0.0133(10) 0.0145(10) 0.0013(8) 0.0012(8) -0.0023(8) O5 0.0229(11) 0.0169(11) 0.0217(11) 0.0051(9) 0.0004(9) 0.0014(9) O6 0.0169(11) 0.0227(12) 0.0265(12) -0.0034(9) -0.0002(9) -0.0012(8) O1W 0.0308(14) 0.0282(14) 0.0308(14) -0.0048(10) 0.0094(11) -0.0097(10) O2W 0.0314(14) 0.071(2) 0.0445(16) -0.0130(15) 0.0099(12) -0.0097(14) O3W 0.0393(15) 0.0256(13) 0.0489(17) 0.0010(12) -0.0072(13) 0.0035(11) O4W 0.091(3) 0.0524(18) 0.0433(19) 0.0076(16) 0.0194(16) 0.0375(18) O5W 0.108(3) 0.070(2) 0.0386(18) -0.0005(16) -0.0026(17) 0.048(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 Gd1 O3 2.2976(17) . ? Gd1 O4 2.3105(17) 7_566 ? Gd1 O2 2.3177(17) . ? Gd1 O1 2.3668(18) . ? Gd1 N4 2.565(2) . ? Gd1 N2 2.625(2) . ? Gd1 N3 2.647(2) . ? Gd1 N1 2.671(2) . ? P1 O4 1.5058(18) . ? P1 O1 1.5147(18) . ? P1 C12 1.817(3) . ? P1 C9 1.836(3) . ? P2 O5 1.4988(19) . ? P2 O2 1.5211(19) . ? P2 C19 1.815(3) . ? P2 C10 1.835(3) . ? P3 O6 1.5063(19) . ? P3 O3 1.5212(18) . ? P3 C26 1.805(3) . ? P3 C11 1.835(3) . ? N1 C1 1.484(3) . ? N1 C9 1.484(3) . ? N1 C8 1.487(3) . ? N2 C2 1.487(3) . ? N2 C10 1.488(3) . ? N2 C3 1.497(3) . ? N3 C5 1.484(3) . ? N3 C11 1.485(3) . ? N3 C4 1.486(3) . ? N4 C6 1.477(3) . ? N4 C7 1.482(3) . ? N4 H4C 0.9100 . ? C1 C2 1.516(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.514(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.514(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.513(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.511(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.386(4) . ? C13 C14 1.392(4) . ? C14 C15 1.382(4) . ? C14 H14 0.9300 . ? C15 C16 1.377(5) . ? C15 H15 0.9300 . ? C16 C17 1.374(4) . ? C16 H16 0.9300 . ? C17 C18 1.388(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.507(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.378(4) . ? C20 C25 1.389(4) . ? C21 C22 1.386(4) . ? C21 H21 0.9300 . ? C22 C23 1.374(4) . ? C22 H22 0.9300 . ? C23 C24 1.381(4) . ? C23 H23 0.9300 . ? C24 C25 1.385(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.511(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C32 1.392(4) . ? C27 C28 1.395(4) . ? C28 C29 1.381(4) . ? C28 H28 0.9300 . ? C29 C30 1.382(4) . ? C29 H29 0.9300 . ? C30 C31 1.385(4) . ? C30 H30 0.9300 . ? C31 C32 1.386(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? O4 Gd1 2.3105(17) 7_566 ? O1W H1WA 0.808(13) . ? O1W H1WB 0.808(13) . ? O2W H2WA 0.814(13) . ? O2W H2WB 0.819(13) . ? O3W H3WA 0.824(13) . ? O3W H3WB 0.819(13) . ? O4W H4WA 0.805(13) . ? O4W H4WB 0.809(13) . ? O4W H4WC 0.806(14) . ? O5W H5WA 0.814(13) . ? O5W H5WB 0.811(14) . ? O5W H5WC 0.813(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Gd1 O4 79.75(6) . 7_566 ? O3 Gd1 O2 80.91(6) . . ? O4 Gd1 O2 130.26(6) 7_566 . ? O3 Gd1 O1 126.53(6) . . ? O4 Gd1 O1 77.08(6) 7_566 . ? O2 Gd1 O1 78.70(6) . . ? O3 Gd1 N4 86.35(7) . . ? O4 Gd1 N4 71.76(7) 7_566 . ? O2 Gd1 N4 151.07(6) . . ? O1 Gd1 N4 128.98(6) . . ? O3 Gd1 N2 129.99(7) . . ? O4 Gd1 N2 149.73(6) 7_566 . ? O2 Gd1 N2 68.89(6) . . ? O1 Gd1 N2 86.24(6) . . ? N4 Gd1 N2 101.18(7) . . ? O3 Gd1 N3 69.99(6) . . ? O4 Gd1 N3 129.53(6) 7_566 . ? O2 Gd1 N3 84.20(6) . . ? O1 Gd1 N3 153.08(6) . . ? N4 Gd1 N3 67.01(7) . . ? N2 Gd1 N3 68.15(7) . . ? O3 Gd1 N1 151.93(7) . . ? O4 Gd1 N1 82.34(6) 7_566 . ? O2 Gd1 N1 127.02(6) . . ? O1 Gd1 N1 69.14(6) . . ? N4 Gd1 N1 67.52(7) . . ? N2 Gd1 N1 68.07(7) . . ? N3 Gd1 N1 106.54(7) . . ? O4 P1 O1 117.02(10) . . ? O4 P1 C12 107.93(12) . . ? O1 P1 C12 109.19(12) . . ? O4 P1 C9 107.45(11) . . ? O1 P1 C9 106.34(11) . . ? C12 P1 C9 108.66(13) . . ? O5 P2 O2 117.63(11) . . ? O5 P2 C19 110.34(12) . . ? O2 P2 C19 108.85(12) . . ? O5 P2 C10 110.63(12) . . ? O2 P2 C10 104.05(11) . . ? C19 P2 C10 104.39(13) . . ? O6 P3 O3 116.34(11) . . ? O6 P3 C26 109.94(12) . . ? O3 P3 C26 107.45(12) . . ? O6 P3 C11 111.24(12) . . ? O3 P3 C11 105.64(11) . . ? C26 P3 C11 105.62(13) . . ? C1 N1 C9 109.6(2) . . ? C1 N1 C8 109.5(2) . . ? C9 N1 C8 109.10(19) . . ? C1 N1 Gd1 110.26(15) . . ? C9 N1 Gd1 107.06(15) . . ? C8 N1 Gd1 111.31(15) . . ? C2 N2 C10 109.8(2) . . ? C2 N2 C3 109.6(2) . . ? C10 N2 C3 107.2(2) . . ? C2 N2 Gd1 112.20(15) . . ? C10 N2 Gd1 106.80(15) . . ? C3 N2 Gd1 111.02(15) . . ? C5 N3 C11 109.1(2) . . ? C5 N3 C4 109.0(2) . . ? C11 N3 C4 110.6(2) . . ? C5 N3 Gd1 110.14(15) . . ? C11 N3 Gd1 105.21(15) . . ? C4 N3 Gd1 112.73(15) . . ? C6 N4 C7 113.4(2) . . ? C6 N4 Gd1 116.60(16) . . ? C7 N4 Gd1 112.52(16) . . ? C6 N4 H4C 104.2 . . ? C7 N4 H4C 104.2 . . ? Gd1 N4 H4C 104.2 . . ? N1 C1 C2 112.2(2) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 111.9(2) . . ? N2 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? N2 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N2 C3 C4 112.8(2) . . ? N2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? N2 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N3 C4 C3 111.8(2) . . ? N3 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N3 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? N3 C5 C6 111.7(2) . . ? N3 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N3 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? N4 C6 C5 109.3(2) . . ? N4 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N4 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N4 C7 C8 109.6(2) . . ? N4 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N4 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N1 C8 C7 112.3(2) . . ? N1 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N1 C9 P1 112.68(17) . . ? N1 C9 H9A 109.1 . . ? P1 C9 H9A 109.1 . . ? N1 C9 H9B 109.1 . . ? P1 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? N2 C10 P2 110.84(18) . . ? N2 C10 H10A 109.5 . . ? P2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? N3 C11 P3 111.24(18) . . ? N3 C11 H11A 109.4 . . ? P3 C11 H11A 109.4 . . ? N3 C11 H11B 109.4 . . ? P3 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 P1 113.96(19) . . ? C13 C12 H12A 108.8 . . ? P1 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? P1 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C18 C13 C14 118.1(3) . . ? C18 C13 C12 121.5(3) . . ? C14 C13 C12 120.4(3) . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 120.8(3) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 119.1(3) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 120.6(3) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C13 C18 C17 120.8(3) . . ? C13 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 P2 114.67(19) . . ? C20 C19 H19A 108.6 . . ? P2 C19 H19A 108.6 . . ? C20 C19 H19B 108.6 . . ? P2 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C21 C20 C25 117.9(3) . . ? C21 C20 C19 121.6(3) . . ? C25 C20 C19 120.4(3) . . ? C20 C21 C22 121.0(3) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C23 C22 C21 120.8(3) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 118.8(3) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C23 C24 C25 120.4(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C20 121.1(3) . . ? C24 C25 H25 119.5 . . ? C20 C25 H25 119.5 . . ? C27 C26 P3 115.95(19) . . ? C27 C26 H26A 108.3 . . ? P3 C26 H26A 108.3 . . ? C27 C26 H26B 108.3 . . ? P3 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C32 C27 C28 118.5(3) . . ? C32 C27 C26 121.8(3) . . ? C28 C27 C26 119.6(3) . . ? C29 C28 C27 120.9(3) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.2(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C31 119.6(3) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C30 C31 C32 120.3(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C27 120.5(3) . . ? C31 C32 H32 119.7 . . ? C27 C32 H32 119.7 . . ? P1 O1 Gd1 123.22(10) . . ? P2 O2 Gd1 126.11(10) . . ? P3 O3 Gd1 124.24(10) . . ? P1 O4 Gd1 161.07(11) . 7_566 ? H1WA O1W H1WB 110(2) . . ? H2WA O2W H2WB 107(2) . . ? H3WA O3W H3WB 105(2) . . ? H4WA O4W H4WB 109(3) . . ? H4WA O4W H4WC 110(3) . . ? H4WB O4W H4WC 131(7) . . ? H5WA O5W H5WB 108(3) . . ? H5WA O5W H5WC 107(3) . . ? H5WB O5W H5WC 84(9) . . ? 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 O3 Gd1 N1 C1 -151.29(15) . . . . ? O4 Gd1 N1 C1 158.03(16) 7_566 . . . ? O2 Gd1 N1 C1 22.36(18) . . . . ? O1 Gd1 N1 C1 78.99(16) . . . . ? N4 Gd1 N1 C1 -128.60(17) . . . . ? N2 Gd1 N1 C1 -15.47(15) . . . . ? N3 Gd1 N1 C1 -72.92(16) . . . . ? O3 Gd1 N1 C9 89.57(19) . . . . ? O4 Gd1 N1 C9 38.89(15) 7_566 . . . ? O2 Gd1 N1 C9 -96.78(15) . . . . ? O1 Gd1 N1 C9 -40.14(14) . . . . ? N4 Gd1 N1 C9 112.27(16) . . . . ? N2 Gd1 N1 C9 -134.60(16) . . . . ? N3 Gd1 N1 C9 167.95(14) . . . . ? O3 Gd1 N1 C8 -29.6(2) . . . . ? O4 Gd1 N1 C8 -80.25(16) 7_566 . . . ? O2 Gd1 N1 C8 144.08(15) . . . . ? O1 Gd1 N1 C8 -159.29(17) . . . . ? N4 Gd1 N1 C8 -6.88(15) . . . . ? N2 Gd1 N1 C8 106.25(17) . . . . ? N3 Gd1 N1 C8 48.80(17) . . . . ? O3 Gd1 N2 C2 140.95(15) . . . . ? O4 Gd1 N2 C2 -26.6(2) 7_566 . . . ? O2 Gd1 N2 C2 -162.05(18) . . . . ? O1 Gd1 N2 C2 -82.71(16) . . . . ? N4 Gd1 N2 C2 46.31(17) . . . . ? N3 Gd1 N2 C2 105.77(17) . . . . ? N1 Gd1 N2 C2 -13.71(16) . . . . ? O3 Gd1 N2 C10 -98.70(17) . . . . ? O4 Gd1 N2 C10 93.77(19) 7_566 . . . ? O2 Gd1 N2 C10 -41.70(15) . . . . ? O1 Gd1 N2 C10 37.63(16) . . . . ? N4 Gd1 N2 C10 166.65(15) . . . . ? N3 Gd1 N2 C10 -133.88(17) . . . . ? N1 Gd1 N2 C10 106.64(17) . . . . ? O3 Gd1 N2 C3 17.87(19) . . . . ? O4 Gd1 N2 C3 -149.66(15) 7_566 . . . ? O2 Gd1 N2 C3 74.87(16) . . . . ? O1 Gd1 N2 C3 154.20(16) . . . . ? N4 Gd1 N2 C3 -76.78(17) . . . . ? N3 Gd1 N2 C3 -17.31(15) . . . . ? N1 Gd1 N2 C3 -136.79(17) . . . . ? O3 Gd1 N3 C5 75.32(16) . . . . ? O4 Gd1 N3 C5 18.41(19) 7_566 . . . ? O2 Gd1 N3 C5 157.74(16) . . . . ? O1 Gd1 N3 C5 -151.68(15) . . . . ? N4 Gd1 N3 C5 -19.32(15) . . . . ? N2 Gd1 N3 C5 -132.70(17) . . . . ? N1 Gd1 N3 C5 -75.31(16) . . . . ? O3 Gd1 N3 C11 -42.08(15) . . . . ? O4 Gd1 N3 C11 -98.99(16) 7_566 . . . ? O2 Gd1 N3 C11 40.34(15) . . . . ? O1 Gd1 N3 C11 90.9(2) . . . . ? N4 Gd1 N3 C11 -136.72(17) . . . . ? N2 Gd1 N3 C11 109.89(16) . . . . ? N1 Gd1 N3 C11 167.29(15) . . . . ? O3 Gd1 N3 C4 -162.71(18) . . . . ? O4 Gd1 N3 C4 140.38(16) 7_566 . . . ? O2 Gd1 N3 C4 -80.29(17) . . . . ? O1 Gd1 N3 C4 -29.7(2) . . . . ? N4 Gd1 N3 C4 102.65(18) . . . . ? N2 Gd1 N3 C4 -10.73(16) . . . . ? N1 Gd1 N3 C4 46.66(18) . . . . ? O3 Gd1 N4 C6 -80.02(18) . . . . ? O4 Gd1 N4 C6 -160.43(19) 7_566 . . . ? O2 Gd1 N4 C6 -16.3(3) . . . . ? O1 Gd1 N4 C6 144.29(16) . . . . ? N2 Gd1 N4 C6 50.05(18) . . . . ? N3 Gd1 N4 C6 -10.22(17) . . . . ? N1 Gd1 N4 C6 110.46(19) . . . . ? O3 Gd1 N4 C7 146.49(17) . . . . ? O4 Gd1 N4 C7 66.09(17) 7_566 . . . ? O2 Gd1 N4 C7 -149.77(16) . . . . ? O1 Gd1 N4 C7 10.8(2) . . . . ? N2 Gd1 N4 C7 -83.43(17) . . . . ? N3 Gd1 N4 C7 -143.71(18) . . . . ? N1 Gd1 N4 C7 -23.02(16) . . . . ? C9 N1 C1 C2 161.3(2) . . . . ? C8 N1 C1 C2 -79.1(3) . . . . ? Gd1 N1 C1 C2 43.7(2) . . . . ? C10 N2 C2 C1 -76.5(3) . . . . ? C3 N2 C2 C1 165.9(2) . . . . ? Gd1 N2 C2 C1 42.1(2) . . . . ? N1 C1 C2 N2 -59.4(3) . . . . ? C2 N2 C3 C4 -79.7(3) . . . . ? C10 N2 C3 C4 161.1(2) . . . . ? Gd1 N2 C3 C4 44.8(2) . . . . ? C5 N3 C4 C3 160.5(2) . . . . ? C11 N3 C4 C3 -79.6(3) . . . . ? Gd1 N3 C4 C3 37.9(3) . . . . ? N2 C3 C4 N3 -56.8(3) . . . . ? C11 N3 C5 C6 162.4(2) . . . . ? C4 N3 C5 C6 -76.7(3) . . . . ? Gd1 N3 C5 C6 47.4(2) . . . . ? C7 N4 C6 C5 171.0(2) . . . . ? Gd1 N4 C6 C5 37.9(3) . . . . ? N3 C5 C6 N4 -57.3(3) . . . . ? C6 N4 C7 C8 -84.0(3) . . . . ? Gd1 N4 C7 C8 51.0(2) . . . . ? C1 N1 C8 C7 158.0(2) . . . . ? C9 N1 C8 C7 -82.0(3) . . . . ? Gd1 N1 C8 C7 35.9(3) . . . . ? N4 C7 C8 N1 -58.8(3) . . . . ? C1 N1 C9 P1 -77.5(2) . . . . ? C8 N1 C9 P1 162.65(17) . . . . ? Gd1 N1 C9 P1 42.09(19) . . . . ? O4 P1 C9 N1 -143.89(17) . . . . ? O1 P1 C9 N1 -17.8(2) . . . . ? C12 P1 C9 N1 99.6(2) . . . . ? C2 N2 C10 P2 169.38(17) . . . . ? C3 N2 C10 P2 -71.6(2) . . . . ? Gd1 N2 C10 P2 47.50(19) . . . . ? O5 P2 C10 N2 101.71(19) . . . . ? O2 P2 C10 N2 -25.5(2) . . . . ? C19 P2 C10 N2 -139.61(19) . . . . ? C5 N3 C11 P3 -71.6(2) . . . . ? C4 N3 C11 P3 168.53(18) . . . . ? Gd1 N3 C11 P3 46.52(19) . . . . ? O6 P3 C11 N3 102.38(19) . . . . ? O3 P3 C11 N3 -24.7(2) . . . . ? C26 P3 C11 N3 -138.37(19) . . . . ? O4 P1 C12 C13 35.2(2) . . . . ? O1 P1 C12 C13 -92.9(2) . . . . ? C9 P1 C12 C13 151.5(2) . . . . ? P1 C12 C13 C18 75.2(3) . . . . ? P1 C12 C13 C14 -103.6(3) . . . . ? C18 C13 C14 C15 0.0(4) . . . . ? C12 C13 C14 C15 178.8(3) . . . . ? C13 C14 C15 C16 0.2(4) . . . . ? C14 C15 C16 C17 0.1(5) . . . . ? C15 C16 C17 C18 -0.6(5) . . . . ? C14 C13 C18 C17 -0.5(4) . . . . ? C12 C13 C18 C17 -179.3(3) . . . . ? C16 C17 C18 C13 0.8(5) . . . . ? O5 P2 C19 C20 -81.6(2) . . . . ? O2 P2 C19 C20 48.8(2) . . . . ? C10 P2 C19 C20 159.5(2) . . . . ? P2 C19 C20 C21 104.6(3) . . . . ? P2 C19 C20 C25 -75.2(3) . . . . ? C25 C20 C21 C22 -1.4(5) . . . . ? C19 C20 C21 C22 178.8(3) . . . . ? C20 C21 C22 C23 1.2(5) . . . . ? C21 C22 C23 C24 0.1(5) . . . . ? C22 C23 C24 C25 -1.0(5) . . . . ? C23 C24 C25 C20 0.8(5) . . . . ? C21 C20 C25 C24 0.5(5) . . . . ? C19 C20 C25 C24 -179.8(3) . . . . ? O6 P3 C26 C27 73.5(2) . . . . ? O3 P3 C26 C27 -159.0(2) . . . . ? C11 P3 C26 C27 -46.6(2) . . . . ? P3 C26 C27 C32 -68.1(3) . . . . ? P3 C26 C27 C28 115.8(3) . . . . ? C32 C27 C28 C29 -1.7(4) . . . . ? C26 C27 C28 C29 174.5(3) . . . . ? C27 C28 C29 C30 1.3(4) . . . . ? C28 C29 C30 C31 -0.1(4) . . . . ? C29 C30 C31 C32 -0.6(4) . . . . ? C30 C31 C32 C27 0.2(4) . . . . ? C28 C27 C32 C31 0.9(4) . . . . ? C26 C27 C32 C31 -175.2(3) . . . . ? O4 P1 O1 Gd1 97.32(13) . . . . ? C12 P1 O1 Gd1 -139.76(12) . . . . ? C9 P1 O1 Gd1 -22.69(15) . . . . ? O3 Gd1 O1 P1 -118.54(12) . . . . ? O4 Gd1 O1 P1 -51.94(12) 7_566 . . . ? O2 Gd1 O1 P1 171.85(13) . . . . ? N4 Gd1 O1 P1 1.29(16) . . . . ? N2 Gd1 O1 P1 102.63(12) . . . . ? N3 Gd1 O1 P1 120.24(14) . . . . ? N1 Gd1 O1 P1 34.69(11) . . . . ? O5 P2 O2 Gd1 -138.46(12) . . . . ? C19 P2 O2 Gd1 95.16(14) . . . . ? C10 P2 O2 Gd1 -15.71(16) . . . . ? O3 Gd1 O2 P2 170.93(13) . . . . ? O4 Gd1 O2 P2 -120.88(12) 7_566 . . . ? O1 Gd1 O2 P2 -58.78(12) . . . . ? N4 Gd1 O2 P2 105.93(16) . . . . ? N2 Gd1 O2 P2 31.53(12) . . . . ? N3 Gd1 O2 P2 100.32(13) . . . . ? N1 Gd1 O2 P2 -6.05(16) . . . . ? O6 P3 O3 Gd1 -141.36(12) . . . . ? C26 P3 O3 Gd1 94.97(14) . . . . ? C11 P3 O3 Gd1 -17.42(16) . . . . ? O4 Gd1 O3 P3 171.50(14) 7_566 . . . ? O2 Gd1 O3 P3 -54.55(13) . . . . ? O1 Gd1 O3 P3 -123.13(12) . . . . ? N4 Gd1 O3 P3 99.39(13) . . . . ? N2 Gd1 O3 P3 -2.15(17) . . . . ? N3 Gd1 O3 P3 32.54(12) . . . . ? N1 Gd1 O3 P3 120.32(15) . . . . ? O1 P1 O4 Gd1 -132.6(3) . . . 7_566 ? C12 P1 O4 Gd1 103.9(3) . . . 7_566 ? C9 P1 O4 Gd1 -13.2(4) . . . 7_566 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O6 0.808(13) 2.005(13) 2.813(3) 179(4) . O1W H1WB O5 0.808(13) 2.125(14) 2.925(3) 170(3) 3 O2W H2WB O6 0.819(13) 1.944(14) 2.759(3) 173(4) . O3W H3WA O2W 0.824(13) 2.027(16) 2.835(3) 167(4) . O3W H3WB O5 0.819(13) 1.986(15) 2.796(3) 170(3) 3 O4W H4WA O1W 0.805(13) 2.002(14) 2.803(3) 173(5) . O4W H4WB O4W 0.809(13) 2.19(5) 2.785(6) 131(6) 2_656 O4W H4WC O5W 0.806(14) 2.16(6) 2.750(5) 130(6) 4_656 O5W H5WA O3W 0.814(13) 2.01(2) 2.782(4) 159(5) . O5W H5WB O4W 0.811(14) 1.98(3) 2.750(5) 158(8) 4_646 O5W H5WC O5W 0.813(14) 2.09(4) 2.781(8) 143(6) 2_756 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.767 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.115 #============================================================================== data_[Eu.L^3^]~2~.10H~2~O _database_code_depnum_ccdc_archive 'CCDC 618887' #============================================================================== _chemical_name_systematic ; bis((\m~2~-1-4-7-10-tetra-azacyclododecane-1,4,7,10-tetrayl-methyl- (trimethylene-tris(phenylphosphinato)))-europium(III)) decahydrate ; _chemical_name_common ; bis((mu!2$-1-4-7-10-tetra-azacyclododecane-1,4,7,10-tetrayl- methyl-(trimethylene-tris(phenylphosphinato)))-europium(iii)) decahydrate ; _chemical_melting_point 'not measured' _chemical_formula_moiety 'C64 H88 Eu2 N8 O12 P6, 10(O H2)' _chemical_formula_sum 'C64 H108 Eu2 N8 O22 P6' _chemical_formula_weight 1831.32 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' P P 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.6586(8) _cell_length_b 15.1326(7) _cell_length_c 30.2862(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.0140(10) _cell_angle_gamma 90.00 _cell_volume 7577.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7729 _cell_measurement_theta_min 2.361 _cell_measurement_theta_max 26.084 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3760 _exptl_absorpt_coefficient_mu 1.844 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.6675 _exptl_absorpt_correction_T_max 0.9820 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.0050 0.00 0.00 -1.00 0.0050 1.00 -1.00 1.00 0.0600 -1.00 1.00 -1.00 0.0600 1.00 1.00 -1.00 0.1200 -1.00 -1.00 1.00 0.1200 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 4 sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.44 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 35450 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7442 _reflns_number_gt 6499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+88.0228P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7442 _refine_ls_number_parameters 496 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.420 _refine_ls_restrained_S_all 1.411 _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 0.309638(19) 0.69866(2) 0.596130(11) 0.01028(9) Uani 1 1 d . . . P1 P 0.15526(10) 0.68353(10) 0.50970(5) 0.0104(3) Uani 1 1 d . . . P2 P 0.27703(10) 0.47917(11) 0.61871(6) 0.0130(3) Uani 1 1 d . . . P3 P 0.50565(10) 0.66891(11) 0.64018(6) 0.0137(4) Uani 1 1 d . . . N1 N 0.1641(3) 0.7761(3) 0.58899(17) 0.0120(11) Uani 1 1 d . . . N2 N 0.2165(3) 0.6304(3) 0.65192(17) 0.0112(11) Uani 1 1 d . . . N3 N 0.3735(3) 0.7182(3) 0.68041(17) 0.0117(11) Uani 1 1 d . . . N4 N 0.3171(3) 0.8611(3) 0.62181(17) 0.0123(11) Uani 1 1 d . . . H4C H 0.3596 0.8839 0.6093 0.015 Uiso 1 1 calc R . . C1 C 0.1066(4) 0.7214(4) 0.6113(2) 0.0152(14) Uani 1 1 d . . . H1A H 0.0884 0.6721 0.5921 0.018 Uiso 1 1 calc R . . H1B H 0.0597 0.7568 0.6156 0.018 Uiso 1 1 calc R . . C2 C 0.1443(4) 0.6861(4) 0.6558(2) 0.0159(14) Uani 1 1 d . . . H2A H 0.1598 0.7354 0.6755 0.019 Uiso 1 1 calc R . . H2B H 0.1044 0.6514 0.6690 0.019 Uiso 1 1 calc R . . C3 C 0.2629(4) 0.6162(4) 0.6967(2) 0.0153(14) Uani 1 1 d . . . H3A H 0.2971 0.5646 0.6957 0.018 Uiso 1 1 calc R . . H3B H 0.2252 0.6046 0.7181 0.018 Uiso 1 1 calc R . . C4 C 0.3153(4) 0.6954(5) 0.7124(2) 0.0170(13) Uani 1 1 d . . . H4A H 0.2807 0.7459 0.7158 0.020 Uiso 1 1 calc R . . H4B H 0.3450 0.6823 0.7412 0.020 Uiso 1 1 calc R . . C5 C 0.4019(4) 0.8108(4) 0.6887(2) 0.0165(14) Uani 1 1 d . . . H5A H 0.4511 0.8202 0.6752 0.020 Uiso 1 1 calc R . . H5B H 0.4141 0.8205 0.7205 0.020 Uiso 1 1 calc R . . C6 C 0.3382(4) 0.8759(4) 0.6697(2) 0.0138(14) Uani 1 1 d . . . H6A H 0.2903 0.8693 0.6847 0.017 Uiso 1 1 calc R . . H6B H 0.3583 0.9356 0.6747 0.017 Uiso 1 1 calc R . . C7 C 0.2469(4) 0.9131(4) 0.6020(2) 0.0151(14) Uani 1 1 d . . . H7A H 0.2493 0.9203 0.5704 0.018 Uiso 1 1 calc R . . H7B H 0.2483 0.9712 0.6155 0.018 Uiso 1 1 calc R . . C8 C 0.1685(4) 0.8663(4) 0.6093(2) 0.0144(14) Uani 1 1 d . . . H8A H 0.1652 0.8614 0.6410 0.017 Uiso 1 1 calc R . . H8B H 0.1228 0.9011 0.5962 0.017 Uiso 1 1 calc R . . C9 C 0.1347(4) 0.7832(4) 0.5412(2) 0.0131(13) Uani 1 1 d . . . H9A H 0.1604 0.8335 0.5289 0.016 Uiso 1 1 calc R . . H9B H 0.0769 0.7939 0.5378 0.016 Uiso 1 1 calc R . . C10 C 0.1898(4) 0.5419(4) 0.6341(2) 0.0148(14) Uani 1 1 d . . . H10A H 0.1500 0.5491 0.6082 0.018 Uiso 1 1 calc R . . H10B H 0.1648 0.5095 0.6565 0.018 Uiso 1 1 calc R . . C11 C 0.4431(4) 0.6564(4) 0.6862(2) 0.0163(14) Uani 1 1 d . . . H11A H 0.4234 0.5962 0.6869 0.020 Uiso 1 1 calc R . . H11B H 0.4758 0.6683 0.7143 0.020 Uiso 1 1 calc R . . C12 C 0.0631(4) 0.6185(5) 0.5011(2) 0.0195(15) Uani 1 1 d . . . H12A H 0.0608 0.5802 0.5266 0.023 Uiso 1 1 calc R . . H12B H 0.0169 0.6580 0.4993 0.023 Uiso 1 1 calc R . . C13 C 0.0567(4) 0.5626(4) 0.4595(2) 0.0174(14) Uani 1 1 d . . . C14 C 0.0052(4) 0.5883(5) 0.4222(2) 0.0241(17) Uani 1 1 d . . . H14 H -0.0259 0.6391 0.4231 0.029 Uiso 1 1 calc R . . C15 C 0.0000(5) 0.5380(6) 0.3832(3) 0.032(2) Uani 1 1 d . . . H15 H -0.0343 0.5562 0.3584 0.039 Uiso 1 1 calc R . . C16 C 0.0447(5) 0.4622(5) 0.3810(3) 0.034(2) Uani 1 1 d . . . H16 H 0.0408 0.4292 0.3549 0.041 Uiso 1 1 calc R . . C17 C 0.0960(5) 0.4358(5) 0.4186(3) 0.0256(17) Uani 1 1 d . . . H17 H 0.1263 0.3844 0.4177 0.031 Uiso 1 1 calc R . . C18 C 0.1019(4) 0.4855(5) 0.4569(2) 0.0215(15) Uani 1 1 d . . . H18 H 0.1367 0.4673 0.4816 0.026 Uiso 1 1 calc R . . C19 C 0.2376(4) 0.4250(4) 0.5672(2) 0.0167(14) Uani 1 1 d . . . H19A H 0.2068 0.3735 0.5741 0.020 Uiso 1 1 calc R . . H19B H 0.2009 0.4650 0.5498 0.020 Uiso 1 1 calc R . . C20 C 0.3028(4) 0.3961(4) 0.5392(2) 0.0172(15) Uani 1 1 d . . . C21 C 0.3249(4) 0.3087(5) 0.5373(2) 0.0255(16) Uani 1 1 d . . . H21 H 0.3006 0.2671 0.5540 0.031 Uiso 1 1 calc R . . C22 C 0.3831(5) 0.2811(5) 0.5106(3) 0.034(2) Uani 1 1 d . . . H22 H 0.3964 0.2216 0.5093 0.041 Uiso 1 1 calc R . . C23 C 0.4208(5) 0.3419(5) 0.4863(2) 0.0276(18) Uani 1 1 d . . . H23 H 0.4594 0.3241 0.4684 0.033 Uiso 1 1 calc R . . C24 C 0.4000(5) 0.4297(5) 0.4891(2) 0.0309(19) Uani 1 1 d . . . H24 H 0.4258 0.4716 0.4732 0.037 Uiso 1 1 calc R . . C25 C 0.3416(5) 0.4568(5) 0.5150(2) 0.0272(18) Uani 1 1 d . . . H25 H 0.3282 0.5163 0.5161 0.033 Uiso 1 1 calc R . . C26 C 0.5328(4) 0.5577(4) 0.6265(2) 0.0191(15) Uani 1 1 d . . . H26A H 0.4857 0.5296 0.6103 0.023 Uiso 1 1 calc R . . H26B H 0.5740 0.5609 0.6065 0.023 Uiso 1 1 calc R . . C27 C 0.5636(4) 0.4996(4) 0.6650(2) 0.0164(14) Uani 1 1 d . . . C28 C 0.5195(4) 0.4244(4) 0.6740(2) 0.0218(16) Uani 1 1 d . . . H28 H 0.4695 0.4138 0.6577 0.026 Uiso 1 1 calc R . . C29 C 0.5495(5) 0.3655(5) 0.7071(3) 0.0260(18) Uani 1 1 d . . . H29 H 0.5199 0.3155 0.7126 0.031 Uiso 1 1 calc R . . C30 C 0.6239(5) 0.3814(5) 0.7321(2) 0.0266(17) Uani 1 1 d . . . H30 H 0.6443 0.3417 0.7540 0.032 Uiso 1 1 calc R . . C31 C 0.6673(5) 0.4561(5) 0.7242(2) 0.0227(16) Uani 1 1 d . . . H31 H 0.7165 0.4674 0.7413 0.027 Uiso 1 1 calc R . . C32 C 0.6379(4) 0.5144(5) 0.6907(2) 0.0210(15) Uani 1 1 d . . . H32 H 0.6680 0.5641 0.6853 0.025 Uiso 1 1 calc R . . O1 O 0.2192(3) 0.6324(3) 0.53867(14) 0.0128(9) Uani 1 1 d . . . O2 O 0.3376(3) 0.5495(3) 0.60892(14) 0.0131(9) Uani 1 1 d . . . O3 O 0.4490(3) 0.7047(3) 0.60113(13) 0.0150(9) Uani 1 1 d . . . O4 O 0.1752(3) 0.7135(3) 0.46490(14) 0.0125(9) Uani 1 1 d . . . O5 O 0.3042(3) 0.4124(3) 0.65366(16) 0.0202(11) Uani 1 1 d . . . O6 O 0.5807(3) 0.7223(3) 0.65415(16) 0.0209(11) Uani 1 1 d . . . O1W O 0.6718(3) 0.8548(3) 0.70195(18) 0.0271(12) Uani 1 1 d D . . H1WA H 0.646(4) 0.817(4) 0.687(2) 0.041 Uiso 1 1 d D . . H1WB H 0.711(4) 0.866(5) 0.688(2) 0.041 Uiso 1 1 d D . . O2W O 0.7103(4) 0.6775(5) 0.6096(2) 0.0468(17) Uani 1 1 d D . . H2WA H 0.691(5) 0.675(7) 0.5831(13) 0.070 Uiso 1 1 d D . . H2WB H 0.673(4) 0.695(7) 0.623(3) 0.070 Uiso 1 1 d D . . O3W O 0.8578(4) 0.7370(4) 0.6571(2) 0.0370(14) Uani 1 1 d D . . H3WA H 0.813(3) 0.719(5) 0.645(3) 0.055 Uiso 1 1 d D . . H3WB H 0.854(5) 0.792(2) 0.656(3) 0.055 Uiso 1 1 d D . . O4W O 0.5748(5) 0.9863(5) 0.7334(2) 0.059(2) Uani 1 1 d D . . H4WA H 0.606(6) 0.947(6) 0.727(4) 0.088 Uiso 1 1 d D . . H4WB H 0.558(12) 0.968(10) 0.756(5) 0.088 Uiso 0.50 1 d PD A 1 H4WC H 0.544(11) 0.996(13) 0.710(3) 0.088 Uiso 0.50 1 d PD B 2 O5W O 0.9167(6) 0.6569(6) 0.7372(2) 0.073(3) Uani 1 1 d D . . H5WA H 0.891(7) 0.676(8) 0.714(3) 0.109 Uiso 1 1 d D . . H5WB H 0.903(15) 0.604(6) 0.738(7) 0.109 Uiso 0.50 1 d PD C 1 H5WC H 0.965(3) 0.659(18) 0.732(6) 0.109 Uiso 0.50 1 d PD D 2 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 0.01129(15) 0.01040(14) 0.00951(15) 0.00056(14) 0.00268(10) 0.00044(14) P1 0.0113(8) 0.0082(8) 0.0120(8) 0.0004(6) 0.0028(6) 0.0000(6) P2 0.0141(9) 0.0115(8) 0.0135(9) 0.0011(6) 0.0022(7) 0.0011(6) P3 0.0132(9) 0.0136(8) 0.0143(9) 0.0000(6) 0.0018(7) 0.0021(6) N1 0.016(3) 0.009(3) 0.012(3) 0.002(2) 0.005(2) -0.001(2) N2 0.008(3) 0.014(3) 0.013(3) 0.000(2) 0.004(2) 0.000(2) N3 0.009(3) 0.013(3) 0.013(3) 0.000(2) 0.001(2) 0.004(2) N4 0.015(3) 0.015(3) 0.008(3) 0.000(2) 0.005(2) -0.001(2) C1 0.013(3) 0.014(3) 0.020(4) -0.001(3) 0.006(3) 0.001(2) C2 0.016(3) 0.016(3) 0.018(3) -0.002(3) 0.011(3) -0.002(3) C3 0.025(4) 0.018(3) 0.004(3) 0.002(3) 0.005(3) -0.002(3) C4 0.019(3) 0.021(3) 0.011(3) -0.003(3) 0.002(3) -0.002(3) C5 0.016(3) 0.020(3) 0.012(3) -0.001(3) -0.004(3) 0.004(3) C6 0.011(3) 0.015(3) 0.016(3) -0.004(3) 0.002(3) 0.003(3) C7 0.020(4) 0.010(3) 0.014(3) -0.002(3) 0.000(3) -0.001(3) C8 0.019(4) 0.010(3) 0.015(3) -0.004(3) 0.004(3) 0.002(3) C9 0.016(3) 0.008(3) 0.014(3) 0.000(2) 0.000(3) 0.001(2) C10 0.020(4) 0.016(3) 0.009(3) 0.000(3) 0.007(3) -0.004(3) C11 0.014(4) 0.021(3) 0.014(4) 0.001(3) 0.003(3) -0.006(3) C12 0.013(4) 0.023(4) 0.023(4) -0.001(3) 0.006(3) -0.004(3) C13 0.014(4) 0.017(3) 0.020(4) 0.002(3) 0.001(3) -0.009(3) C14 0.018(4) 0.024(4) 0.029(4) 0.009(3) -0.003(3) -0.010(3) C15 0.025(4) 0.052(5) 0.019(4) 0.011(4) -0.004(3) -0.025(4) C16 0.042(5) 0.036(5) 0.026(5) -0.011(4) 0.012(4) -0.029(4) C17 0.030(4) 0.018(4) 0.032(5) -0.006(3) 0.018(4) -0.010(3) C18 0.023(4) 0.022(4) 0.020(4) 0.001(3) 0.003(3) -0.001(3) C19 0.019(4) 0.018(3) 0.012(3) 0.001(3) -0.001(3) 0.003(3) C20 0.020(4) 0.016(3) 0.015(4) -0.002(3) -0.001(3) -0.001(3) C21 0.027(4) 0.021(4) 0.031(4) 0.005(3) 0.012(3) 0.008(3) C22 0.038(5) 0.020(4) 0.046(5) 0.004(3) 0.013(4) 0.015(3) C23 0.019(4) 0.047(5) 0.017(4) -0.002(3) 0.004(3) 0.004(3) C24 0.049(5) 0.030(4) 0.015(4) 0.004(3) 0.010(4) -0.009(4) C25 0.045(5) 0.020(4) 0.019(4) -0.001(3) 0.011(4) 0.001(3) C26 0.025(4) 0.017(3) 0.016(4) -0.004(3) 0.005(3) 0.002(3) C27 0.018(4) 0.017(3) 0.015(4) -0.004(3) 0.004(3) 0.006(3) C28 0.018(4) 0.022(4) 0.027(4) -0.004(3) 0.008(3) 0.004(3) C29 0.029(5) 0.019(4) 0.034(5) 0.004(3) 0.019(4) 0.002(3) C30 0.039(5) 0.026(4) 0.015(4) 0.004(3) 0.007(3) 0.011(3) C31 0.027(4) 0.026(4) 0.015(4) -0.006(3) -0.001(3) 0.010(3) C32 0.019(4) 0.020(4) 0.024(4) -0.010(3) -0.002(3) 0.003(3) O1 0.011(2) 0.015(2) 0.012(2) 0.0008(18) 0.0008(18) 0.0028(17) O2 0.015(2) 0.013(2) 0.012(2) 0.0035(17) 0.0036(18) 0.0014(18) O3 0.016(2) 0.016(2) 0.012(2) 0.0007(19) 0.0005(18) 0.000(2) O4 0.016(2) 0.010(2) 0.012(2) -0.0007(17) 0.0018(18) -0.0026(17) O5 0.026(3) 0.015(2) 0.020(3) 0.005(2) 0.004(2) 0.002(2) O6 0.015(3) 0.022(3) 0.025(3) -0.001(2) 0.001(2) 0.0003(19) O1W 0.033(3) 0.021(3) 0.028(3) -0.005(2) 0.006(3) -0.008(2) O2W 0.031(3) 0.064(5) 0.048(4) -0.012(4) 0.012(3) -0.011(3) O3W 0.040(4) 0.022(3) 0.046(4) 0.002(3) -0.006(3) 0.002(3) O4W 0.087(6) 0.053(4) 0.038(4) 0.009(3) 0.016(4) 0.037(4) O5W 0.111(7) 0.067(5) 0.040(4) 0.002(4) 0.006(4) 0.048(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 Eu1 O3 2.309(4) . ? Eu1 O4 2.316(4) 7_566 ? Eu1 O2 2.327(4) . ? Eu1 O1 2.379(4) . ? Eu1 N4 2.577(5) . ? Eu1 N2 2.640(5) . ? Eu1 N3 2.659(5) . ? Eu1 N1 2.677(5) . ? Eu1 P3 3.4031(18) . ? Eu1 P1 3.4460(17) . ? Eu1 P2 3.4474(16) . ? P1 O4 1.506(4) . ? P1 O1 1.508(4) . ? P1 C12 1.816(7) . ? P1 C9 1.839(6) . ? P2 O5 1.493(5) . ? P2 O2 1.520(5) . ? P2 C19 1.814(7) . ? P2 C10 1.843(7) . ? P3 O6 1.505(5) . ? P3 O3 1.520(4) . ? P3 C26 1.805(7) . ? P3 C11 1.850(7) . ? N1 C9 1.473(8) . ? N1 C1 1.490(8) . ? N1 C8 1.495(8) . ? N2 C2 1.485(8) . ? N2 C10 1.491(8) . ? N2 C3 1.492(8) . ? N3 C11 1.482(8) . ? N3 C5 1.490(8) . ? N3 C4 1.492(8) . ? N4 C6 1.467(8) . ? N4 C7 1.474(8) . ? N4 H4C 0.9100 . ? C1 C2 1.512(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.524(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.510(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.526(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.511(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.388(10) . ? C13 C18 1.396(10) . ? C14 C15 1.397(11) . ? C14 H14 0.9300 . ? C15 C16 1.373(12) . ? C15 H15 0.9300 . ? C16 C17 1.396(12) . ? C16 H16 0.9300 . ? C17 C18 1.377(10) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.521(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.377(10) . ? C20 C25 1.383(10) . ? C21 C22 1.400(10) . ? C21 H21 0.9300 . ? C22 C23 1.376(11) . ? C22 H22 0.9300 . ? C23 C24 1.377(11) . ? C23 H23 0.9300 . ? C24 C25 1.386(11) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.501(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C32 1.398(10) . ? C27 C28 1.398(10) . ? C28 C29 1.389(10) . ? C28 H28 0.9300 . ? C29 C30 1.391(11) . ? C29 H29 0.9300 . ? C30 C31 1.378(11) . ? C30 H30 0.9300 . ? C31 C32 1.387(10) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? O4 Eu1 2.316(4) 7_566 ? O1W H1WA 0.83(3) . ? O1W H1WB 0.83(3) . ? O2W H2WA 0.83(3) . ? O2W H2WB 0.83(3) . ? O3W H3WA 0.83(3) . ? O3W H3WB 0.83(3) . ? O4W H4WA 0.83(3) . ? O4W H4WB 0.83(3) . ? O4W H4WC 0.83(3) . ? O5W H5WA 0.83(3) . ? O5W H5WB 0.83(3) . ? O5W H5WC 0.83(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Eu1 O4 79.82(15) . 7_566 ? O3 Eu1 O2 81.27(16) . . ? O4 Eu1 O2 130.60(15) 7_566 . ? O3 Eu1 O1 127.29(15) . . ? O4 Eu1 O1 77.22(14) 7_566 . ? O2 Eu1 O1 79.00(15) . . ? O3 Eu1 N4 86.10(16) . . ? O4 Eu1 N4 71.77(15) 7_566 . ? O2 Eu1 N4 150.89(16) . . ? O1 Eu1 N4 128.71(16) . . ? O3 Eu1 N2 129.63(15) . . ? O4 Eu1 N2 149.93(16) 7_566 . ? O2 Eu1 N2 68.60(15) . . ? O1 Eu1 N2 86.25(15) . . ? N4 Eu1 N2 100.98(16) . . ? O3 Eu1 N3 69.60(15) . . ? O4 Eu1 N3 129.23(15) 7_566 . ? O2 Eu1 N3 84.25(15) . . ? O1 Eu1 N3 153.17(15) . . ? N4 Eu1 N3 66.75(16) . . ? N2 Eu1 N3 68.08(16) . . ? O3 Eu1 N1 151.75(16) . . ? O4 Eu1 N1 82.51(15) 7_566 . ? O2 Eu1 N1 126.78(15) . . ? O1 Eu1 N1 68.86(15) . . ? N4 Eu1 N1 67.44(16) . . ? N2 Eu1 N1 68.05(15) . . ? N3 Eu1 N1 106.32(15) . . ? O3 Eu1 P3 21.70(11) . . ? O4 Eu1 P3 101.31(11) 7_566 . ? O2 Eu1 P3 69.12(11) . . ? O1 Eu1 P3 136.25(10) . . ? N4 Eu1 P3 89.97(13) . . ? N2 Eu1 P3 107.94(12) . . ? N3 Eu1 P3 52.13(11) . . ? N1 Eu1 P3 154.89(11) . . ? O3 Eu1 P1 134.70(10) . . ? O4 Eu1 P1 64.89(11) 7_566 . ? O2 Eu1 P1 100.23(11) . . ? O1 Eu1 P1 21.46(10) . . ? N4 Eu1 P1 107.25(12) . . ? N2 Eu1 P1 91.03(12) . . ? N3 Eu1 P1 155.59(11) . . ? N1 Eu1 P1 51.93(11) . . ? P3 Eu1 P1 151.69(4) . . ? O3 Eu1 P2 101.91(12) . . ? O4 Eu1 P2 138.31(10) 7_566 . ? O2 Eu1 P2 20.91(11) . . ? O1 Eu1 P2 68.80(10) . . ? N4 Eu1 P2 149.56(12) . . ? N2 Eu1 P2 51.46(11) . . ? N3 Eu1 P2 88.35(11) . . ? N1 Eu1 P2 105.95(11) . . ? P3 Eu1 P2 87.81(4) . . ? P1 Eu1 P2 88.03(4) . . ? O4 P1 O1 117.4(2) . . ? O4 P1 C12 108.1(3) . . ? O1 P1 C12 109.3(3) . . ? O4 P1 C9 107.3(3) . . ? O1 P1 C9 106.3(3) . . ? C12 P1 C9 108.1(3) . . ? O4 P1 Eu1 115.97(18) . . ? O1 P1 Eu1 35.25(17) . . ? C12 P1 Eu1 133.2(2) . . ? C9 P1 Eu1 73.7(2) . . ? O5 P2 O2 117.5(3) . . ? O5 P2 C19 110.5(3) . . ? O2 P2 C19 109.2(3) . . ? O5 P2 C10 110.4(3) . . ? O2 P2 C10 104.5(3) . . ? C19 P2 C10 103.7(3) . . ? O5 P2 Eu1 138.7(2) . . ? O2 P2 Eu1 33.11(16) . . ? C19 P2 Eu1 108.3(2) . . ? C10 P2 Eu1 72.7(2) . . ? O6 P3 O3 116.3(3) . . ? O6 P3 C26 110.0(3) . . ? O3 P3 C26 107.6(3) . . ? O6 P3 C11 111.6(3) . . ? O3 P3 C11 105.6(3) . . ? C26 P3 C11 105.0(3) . . ? O6 P3 Eu1 139.79(19) . . ? O3 P3 Eu1 34.17(17) . . ? C26 P3 Eu1 106.8(2) . . ? C11 P3 Eu1 72.9(2) . . ? C9 N1 C1 109.3(5) . . ? C9 N1 C8 109.4(5) . . ? C1 N1 C8 108.8(5) . . ? C9 N1 Eu1 107.5(4) . . ? C1 N1 Eu1 110.2(3) . . ? C8 N1 Eu1 111.6(4) . . ? C2 N2 C10 109.2(5) . . ? C2 N2 C3 110.1(5) . . ? C10 N2 C3 107.3(5) . . ? C2 N2 Eu1 111.9(4) . . ? C10 N2 Eu1 107.0(3) . . ? C3 N2 Eu1 111.0(4) . . ? C11 N3 C5 110.2(5) . . ? C11 N3 C4 109.8(5) . . ? C5 N3 C4 109.0(5) . . ? C11 N3 Eu1 105.0(4) . . ? C5 N3 Eu1 110.4(3) . . ? C4 N3 Eu1 112.4(4) . . ? C6 N4 C7 113.8(5) . . ? C6 N4 Eu1 116.2(4) . . ? C7 N4 Eu1 112.3(4) . . ? C6 N4 H4C 104.3 . . ? C7 N4 H4C 104.3 . . ? Eu1 N4 H4C 104.3 . . ? N1 C1 C2 112.4(5) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 112.5(5) . . ? N2 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? N2 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N2 C3 C4 112.5(5) . . ? N2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N3 C4 C3 111.9(5) . . ? N3 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? N3 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N3 C5 C6 110.8(5) . . ? N3 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? N4 C6 C5 110.5(5) . . ? N4 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N4 C7 C8 110.1(5) . . ? N4 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N4 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? N1 C8 C7 111.3(5) . . ? N1 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N1 C9 P1 112.9(4) . . ? N1 C9 H9A 109.0 . . ? P1 C9 H9A 109.0 . . ? N1 C9 H9B 109.0 . . ? P1 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N2 C10 P2 110.2(4) . . ? N2 C10 H10A 109.6 . . ? P2 C10 H10A 109.6 . . ? N2 C10 H10B 109.6 . . ? P2 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? N3 C11 P3 110.5(4) . . ? N3 C11 H11A 109.5 . . ? P3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? P3 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C13 C12 P1 113.2(5) . . ? C13 C12 H12A 108.9 . . ? P1 C12 H12A 108.9 . . ? C13 C12 H12B 108.9 . . ? P1 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C18 118.2(7) . . ? C14 C13 C12 119.8(6) . . ? C18 C13 C12 122.1(6) . . ? C13 C14 C15 120.2(7) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 121.2(7) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 118.7(7) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C18 C17 C16 120.4(7) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C13 121.3(7) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? C20 C19 P2 113.6(5) . . ? C20 C19 H19A 108.8 . . ? P2 C19 H19A 108.8 . . ? C20 C19 H19B 108.8 . . ? P2 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C21 C20 C25 118.1(7) . . ? C21 C20 C19 120.8(6) . . ? C25 C20 C19 121.1(6) . . ? C20 C21 C22 121.2(7) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 120.2(7) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 118.6(7) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C23 C24 C25 121.2(7) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C20 C25 C24 120.7(7) . . ? C20 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 P3 116.0(5) . . ? C27 C26 H26A 108.3 . . ? P3 C26 H26A 108.3 . . ? C27 C26 H26B 108.3 . . ? P3 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C32 C27 C28 118.2(6) . . ? C32 C27 C26 122.3(6) . . ? C28 C27 C26 119.4(6) . . ? C29 C28 C27 120.8(7) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 119.9(7) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0(7) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.1(7) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C27 121.0(7) . . ? C31 C32 H32 119.5 . . ? C27 C32 H32 119.5 . . ? P1 O1 Eu1 123.3(2) . . ? P2 O2 Eu1 126.0(2) . . ? P3 O3 Eu1 124.1(2) . . ? P1 O4 Eu1 161.7(3) . 7_566 ? H1WA O1W H1WB 105(5) . . ? H2WA O2W H2WB 105(5) . . ? H3WA O3W H3WB 104(5) . . ? H4WA O4W H4WB 105(5) . . ? H4WA O4W H4WC 105(5) . . ? H4WB O4W H4WC 121(10) . . ? H5WA O5W H5WB 105(5) . . ? H5WA O5W H5WC 105(5) . . ? H5WB O5W H5WC 108(10) . . ? 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 O3 Eu1 P1 O4 -22.2(3) . . . . ? O4 Eu1 P1 O4 20.2(3) 7_566 . . . ? O2 Eu1 P1 O4 -110.0(2) . . . . ? O1 Eu1 P1 O4 -101.4(3) . . . . ? N4 Eu1 P1 O4 79.8(2) . . . . ? N2 Eu1 P1 O4 -178.4(2) . . . . ? N3 Eu1 P1 O4 151.3(3) . . . . ? N1 Eu1 P1 O4 120.9(2) . . . . ? P3 Eu1 P1 O4 -45.4(2) . . . . ? P2 Eu1 P1 O4 -127.04(19) . . . . ? O3 Eu1 P1 O1 79.2(3) . . . . ? O4 Eu1 P1 O1 121.6(3) 7_566 . . . ? O2 Eu1 P1 O1 -8.6(3) . . . . ? N4 Eu1 P1 O1 -178.9(3) . . . . ? N2 Eu1 P1 O1 -77.0(3) . . . . ? N3 Eu1 P1 O1 -107.3(4) . . . . ? N1 Eu1 P1 O1 -137.8(3) . . . . ? P3 Eu1 P1 O1 56.0(3) . . . . ? P2 Eu1 P1 O1 -25.7(3) . . . . ? O3 Eu1 P1 C12 136.4(3) . . . . ? O4 Eu1 P1 C12 178.8(3) 7_566 . . . ? O2 Eu1 P1 C12 48.6(3) . . . . ? O1 Eu1 P1 C12 57.2(4) . . . . ? N4 Eu1 P1 C12 -121.7(3) . . . . ? N2 Eu1 P1 C12 -19.9(3) . . . . ? N3 Eu1 P1 C12 -50.1(4) . . . . ? N1 Eu1 P1 C12 -80.6(3) . . . . ? P3 Eu1 P1 C12 113.2(3) . . . . ? P2 Eu1 P1 C12 31.5(3) . . . . ? O3 Eu1 P1 C9 -123.8(3) . . . . ? O4 Eu1 P1 C9 -81.4(2) 7_566 . . . ? O2 Eu1 P1 C9 148.4(2) . . . . ? O1 Eu1 P1 C9 157.0(4) . . . . ? N4 Eu1 P1 C9 -21.9(2) . . . . ? N2 Eu1 P1 C9 79.9(2) . . . . ? N3 Eu1 P1 C9 49.7(3) . . . . ? N1 Eu1 P1 C9 19.2(2) . . . . ? P3 Eu1 P1 C9 -147.0(2) . . . . ? P2 Eu1 P1 C9 131.3(2) . . . . ? O3 Eu1 P2 O5 52.9(3) . . . . ? O4 Eu1 P2 O5 140.9(3) 7_566 . . . ? O2 Eu1 P2 O5 62.2(4) . . . . ? O1 Eu1 P2 O5 178.5(3) . . . . ? N4 Eu1 P2 O5 -49.9(4) . . . . ? N2 Eu1 P2 O5 -78.9(3) . . . . ? N3 Eu1 P2 O5 -15.9(3) . . . . ? N1 Eu1 P2 O5 -122.4(3) . . . . ? P3 Eu1 P2 O5 36.3(3) . . . . ? P1 Eu1 P2 O5 -171.7(3) . . . . ? O3 Eu1 P2 O2 -9.4(3) . . . . ? O4 Eu1 P2 O2 78.6(3) 7_566 . . . ? O1 Eu1 P2 O2 116.2(3) . . . . ? N4 Eu1 P2 O2 -112.2(4) . . . . ? N2 Eu1 P2 O2 -141.1(3) . . . . ? N3 Eu1 P2 O2 -78.1(3) . . . . ? N1 Eu1 P2 O2 175.4(3) . . . . ? P3 Eu1 P2 O2 -26.0(3) . . . . ? P1 Eu1 P2 O2 126.0(3) . . . . ? O3 Eu1 P2 C19 -106.6(3) . . . . ? O4 Eu1 P2 C19 -18.5(3) 7_566 . . . ? O2 Eu1 P2 C19 -97.2(4) . . . . ? O1 Eu1 P2 C19 19.1(3) . . . . ? N4 Eu1 P2 C19 150.6(3) . . . . ? N2 Eu1 P2 C19 121.7(3) . . . . ? N3 Eu1 P2 C19 -175.3(3) . . . . ? N1 Eu1 P2 C19 78.2(3) . . . . ? P3 Eu1 P2 C19 -123.2(2) . . . . ? P1 Eu1 P2 C19 28.8(2) . . . . ? O3 Eu1 P2 C10 154.3(2) . . . . ? O4 Eu1 P2 C10 -117.7(3) 7_566 . . . ? O2 Eu1 P2 C10 163.7(4) . . . . ? O1 Eu1 P2 C10 -80.1(2) . . . . ? N4 Eu1 P2 C10 51.5(3) . . . . ? N2 Eu1 P2 C10 22.6(3) . . . . ? N3 Eu1 P2 C10 85.6(2) . . . . ? N1 Eu1 P2 C10 -20.9(3) . . . . ? P3 Eu1 P2 C10 137.7(2) . . . . ? P1 Eu1 P2 C10 -70.3(2) . . . . ? O3 Eu1 P3 O6 58.8(4) . . . . ? O4 Eu1 P3 O6 50.7(3) 7_566 . . . ? O2 Eu1 P3 O6 -180.0(3) . . . . ? O1 Eu1 P3 O6 134.0(3) . . . . ? N4 Eu1 P3 O6 -20.7(3) . . . . ? N2 Eu1 P3 O6 -122.2(3) . . . . ? N3 Eu1 P3 O6 -80.7(3) . . . . ? N1 Eu1 P3 O6 -45.8(4) . . . . ? P1 Eu1 P3 O6 107.9(3) . . . . ? P2 Eu1 P3 O6 -170.3(3) . . . . ? O4 Eu1 P3 O3 -8.1(3) 7_566 . . . ? O2 Eu1 P3 O3 121.3(3) . . . . ? O1 Eu1 P3 O3 75.2(3) . . . . ? N4 Eu1 P3 O3 -79.5(3) . . . . ? N2 Eu1 P3 O3 179.0(3) . . . . ? N3 Eu1 P3 O3 -139.5(3) . . . . ? N1 Eu1 P3 O3 -104.6(4) . . . . ? P1 Eu1 P3 O3 49.2(3) . . . . ? P2 Eu1 P3 O3 130.9(3) . . . . ? O3 Eu1 P3 C26 -96.8(4) . . . . ? O4 Eu1 P3 C26 -104.8(3) 7_566 . . . ? O2 Eu1 P3 C26 24.5(3) . . . . ? O1 Eu1 P3 C26 -21.6(3) . . . . ? N4 Eu1 P3 C26 -176.2(3) . . . . ? N2 Eu1 P3 C26 82.2(3) . . . . ? N3 Eu1 P3 C26 123.7(3) . . . . ? N1 Eu1 P3 C26 158.6(3) . . . . ? P1 Eu1 P3 C26 -47.6(3) . . . . ? P2 Eu1 P3 C26 34.1(2) . . . . ? O3 Eu1 P3 C11 162.3(4) . . . . ? O4 Eu1 P3 C11 154.2(2) 7_566 . . . ? O2 Eu1 P3 C11 -76.5(2) . . . . ? O1 Eu1 P3 C11 -122.5(3) . . . . ? N4 Eu1 P3 C11 82.8(2) . . . . ? N2 Eu1 P3 C11 -18.7(3) . . . . ? N3 Eu1 P3 C11 22.8(3) . . . . ? N1 Eu1 P3 C11 57.7(3) . . . . ? P1 Eu1 P3 C11 -148.6(2) . . . . ? P2 Eu1 P3 C11 -66.8(2) . . . . ? O3 Eu1 N1 C9 91.0(4) . . . . ? O4 Eu1 N1 C9 39.4(3) 7_566 . . . ? O2 Eu1 N1 C9 -96.7(4) . . . . ? O1 Eu1 N1 C9 -39.7(3) . . . . ? N4 Eu1 N1 C9 112.7(4) . . . . ? N2 Eu1 N1 C9 -134.3(4) . . . . ? N3 Eu1 N1 C9 168.2(3) . . . . ? P3 Eu1 N1 C9 140.1(3) . . . . ? P1 Eu1 N1 C9 -24.4(3) . . . . ? P2 Eu1 N1 C9 -98.8(3) . . . . ? O3 Eu1 N1 C1 -150.0(4) . . . . ? O4 Eu1 N1 C1 158.4(4) 7_566 . . . ? O2 Eu1 N1 C1 22.3(4) . . . . ? O1 Eu1 N1 C1 79.3(4) . . . . ? N4 Eu1 N1 C1 -128.2(4) . . . . ? N2 Eu1 N1 C1 -15.3(4) . . . . ? N3 Eu1 N1 C1 -72.8(4) . . . . ? P3 Eu1 N1 C1 -100.8(4) . . . . ? P1 Eu1 N1 C1 94.6(4) . . . . ? P2 Eu1 N1 C1 20.2(4) . . . . ? O3 Eu1 N1 C8 -28.9(6) . . . . ? O4 Eu1 N1 C8 -80.5(4) 7_566 . . . ? O2 Eu1 N1 C8 143.3(4) . . . . ? O1 Eu1 N1 C8 -159.7(4) . . . . ? N4 Eu1 N1 C8 -7.2(4) . . . . ? N2 Eu1 N1 C8 105.7(4) . . . . ? N3 Eu1 N1 C8 48.2(4) . . . . ? P3 Eu1 N1 C8 20.2(5) . . . . ? P1 Eu1 N1 C8 -144.4(4) . . . . ? P2 Eu1 N1 C8 141.3(4) . . . . ? O3 Eu1 N2 C2 140.6(4) . . . . ? O4 Eu1 N2 C2 -26.0(6) 7_566 . . . ? O2 Eu1 N2 C2 -161.8(4) . . . . ? O1 Eu1 N2 C2 -82.2(4) . . . . ? N4 Eu1 N2 C2 46.5(4) . . . . ? N3 Eu1 N2 C2 105.8(4) . . . . ? N1 Eu1 N2 C2 -13.5(4) . . . . ? P3 Eu1 N2 C2 140.1(4) . . . . ? P1 Eu1 N2 C2 -61.3(4) . . . . ? P2 Eu1 N2 C2 -147.9(4) . . . . ? O3 Eu1 N2 C10 -99.8(4) . . . . ? O4 Eu1 N2 C10 93.7(5) 7_566 . . . ? O2 Eu1 N2 C10 -42.2(4) . . . . ? O1 Eu1 N2 C10 37.4(4) . . . . ? N4 Eu1 N2 C10 166.2(4) . . . . ? N3 Eu1 N2 C10 -134.6(4) . . . . ? N1 Eu1 N2 C10 106.1(4) . . . . ? P3 Eu1 N2 C10 -100.3(4) . . . . ? P1 Eu1 N2 C10 58.4(4) . . . . ? P2 Eu1 N2 C10 -28.3(3) . . . . ? O3 Eu1 N2 C3 17.0(5) . . . . ? O4 Eu1 N2 C3 -149.5(4) 7_566 . . . ? O2 Eu1 N2 C3 74.6(4) . . . . ? O1 Eu1 N2 C3 154.3(4) . . . . ? N4 Eu1 N2 C3 -77.0(4) . . . . ? N3 Eu1 N2 C3 -17.8(4) . . . . ? N1 Eu1 N2 C3 -137.0(4) . . . . ? P3 Eu1 N2 C3 16.6(4) . . . . ? P1 Eu1 N2 C3 175.2(4) . . . . ? P2 Eu1 N2 C3 88.5(4) . . . . ? O3 Eu1 N3 C11 -43.4(3) . . . . ? O4 Eu1 N3 C11 -100.3(4) 7_566 . . . ? O2 Eu1 N3 C11 39.4(4) . . . . ? O1 Eu1 N3 C11 90.8(5) . . . . ? N4 Eu1 N3 C11 -138.1(4) . . . . ? N2 Eu1 N3 C11 108.6(4) . . . . ? N1 Eu1 N3 C11 166.1(3) . . . . ? P3 Eu1 N3 C11 -28.6(3) . . . . ? P1 Eu1 N3 C11 141.5(3) . . . . ? P2 Eu1 N3 C11 59.9(3) . . . . ? O3 Eu1 N3 C5 75.4(4) . . . . ? O4 Eu1 N3 C5 18.5(4) 7_566 . . . ? O2 Eu1 N3 C5 158.2(4) . . . . ? O1 Eu1 N3 C5 -150.5(4) . . . . ? N4 Eu1 N3 C5 -19.3(4) . . . . ? N2 Eu1 N3 C5 -132.6(4) . . . . ? N1 Eu1 N3 C5 -75.1(4) . . . . ? P3 Eu1 N3 C5 90.2(4) . . . . ? P1 Eu1 N3 C5 -99.7(4) . . . . ? P2 Eu1 N3 C5 178.7(4) . . . . ? O3 Eu1 N3 C4 -162.7(4) . . . . ? O4 Eu1 N3 C4 140.5(4) 7_566 . . . ? O2 Eu1 N3 C4 -79.9(4) . . . . ? O1 Eu1 N3 C4 -28.5(6) . . . . ? N4 Eu1 N3 C4 102.7(4) . . . . ? N2 Eu1 N3 C4 -10.7(4) . . . . ? N1 Eu1 N3 C4 46.8(4) . . . . ? P3 Eu1 N3 C4 -147.9(4) . . . . ? P1 Eu1 N3 C4 22.2(6) . . . . ? P2 Eu1 N3 C4 -59.4(4) . . . . ? O3 Eu1 N4 C6 -79.8(4) . . . . ? O4 Eu1 N4 C6 -160.3(5) 7_566 . . . ? O2 Eu1 N4 C6 -15.6(6) . . . . ? O1 Eu1 N4 C6 143.9(4) . . . . ? N2 Eu1 N4 C6 49.9(4) . . . . ? N3 Eu1 N4 C6 -10.3(4) . . . . ? N1 Eu1 N4 C6 110.3(4) . . . . ? P3 Eu1 N4 C6 -58.4(4) . . . . ? P1 Eu1 N4 C6 144.4(4) . . . . ? P2 Eu1 N4 C6 27.2(6) . . . . ? O3 Eu1 N4 C7 146.8(4) . . . . ? O4 Eu1 N4 C7 66.2(4) 7_566 . . . ? O2 Eu1 N4 C7 -149.0(4) . . . . ? O1 Eu1 N4 C7 10.4(5) . . . . ? N2 Eu1 N4 C7 -83.6(4) . . . . ? N3 Eu1 N4 C7 -143.8(4) . . . . ? N1 Eu1 N4 C7 -23.1(4) . . . . ? P3 Eu1 N4 C7 168.1(4) . . . . ? P1 Eu1 N4 C7 11.0(4) . . . . ? P2 Eu1 N4 C7 -106.2(4) . . . . ? C9 N1 C1 C2 161.3(5) . . . . ? C8 N1 C1 C2 -79.4(6) . . . . ? Eu1 N1 C1 C2 43.3(6) . . . . ? C10 N2 C2 C1 -76.5(6) . . . . ? C3 N2 C2 C1 165.9(5) . . . . ? Eu1 N2 C2 C1 41.8(6) . . . . ? N1 C1 C2 N2 -59.2(7) . . . . ? C2 N2 C3 C4 -79.1(6) . . . . ? C10 N2 C3 C4 162.1(5) . . . . ? Eu1 N2 C3 C4 45.4(6) . . . . ? C11 N3 C4 C3 -78.4(6) . . . . ? C5 N3 C4 C3 160.8(5) . . . . ? Eu1 N3 C4 C3 38.1(6) . . . . ? N2 C3 C4 N3 -57.5(7) . . . . ? C11 N3 C5 C6 162.5(5) . . . . ? C4 N3 C5 C6 -76.9(6) . . . . ? Eu1 N3 C5 C6 47.0(6) . . . . ? C7 N4 C6 C5 171.4(5) . . . . ? Eu1 N4 C6 C5 38.7(6) . . . . ? N3 C5 C6 N4 -57.7(7) . . . . ? C6 N4 C7 C8 -83.0(6) . . . . ? Eu1 N4 C7 C8 51.6(6) . . . . ? C9 N1 C8 C7 -82.9(6) . . . . ? C1 N1 C8 C7 157.8(5) . . . . ? Eu1 N1 C8 C7 35.9(6) . . . . ? N4 C7 C8 N1 -59.2(7) . . . . ? C1 N1 C9 P1 -78.1(5) . . . . ? C8 N1 C9 P1 162.9(4) . . . . ? Eu1 N1 C9 P1 41.5(5) . . . . ? O4 P1 C9 N1 -143.5(4) . . . . ? O1 P1 C9 N1 -17.1(5) . . . . ? C12 P1 C9 N1 100.1(5) . . . . ? Eu1 P1 C9 N1 -30.8(4) . . . . ? C2 N2 C10 P2 169.0(4) . . . . ? C3 N2 C10 P2 -71.6(5) . . . . ? Eu1 N2 C10 P2 47.7(4) . . . . ? O5 P2 C10 N2 101.8(4) . . . . ? O2 P2 C10 N2 -25.4(5) . . . . ? C19 P2 C10 N2 -139.8(4) . . . . ? Eu1 P2 C10 N2 -34.5(4) . . . . ? C5 N3 C11 P3 -71.0(6) . . . . ? C4 N3 C11 P3 168.9(4) . . . . ? Eu1 N3 C11 P3 47.9(4) . . . . ? O6 P3 C11 N3 101.7(5) . . . . ? O3 P3 C11 N3 -25.6(5) . . . . ? C26 P3 C11 N3 -139.2(5) . . . . ? Eu1 P3 C11 N3 -35.9(4) . . . . ? O4 P1 C12 C13 36.2(6) . . . . ? O1 P1 C12 C13 -92.7(5) . . . . ? C9 P1 C12 C13 152.0(5) . . . . ? Eu1 P1 C12 C13 -123.6(4) . . . . ? P1 C12 C13 C14 -104.3(7) . . . . ? P1 C12 C13 C18 75.1(7) . . . . ? C18 C13 C14 C15 -0.6(10) . . . . ? C12 C13 C14 C15 178.8(6) . . . . ? C13 C14 C15 C16 0.6(11) . . . . ? C14 C15 C16 C17 0.0(11) . . . . ? C15 C16 C17 C18 -0.5(11) . . . . ? C16 C17 C18 C13 0.5(11) . . . . ? C14 C13 C18 C17 0.0(10) . . . . ? C12 C13 C18 C17 -179.4(6) . . . . ? O5 P2 C19 C20 -82.3(5) . . . . ? O2 P2 C19 C20 48.3(5) . . . . ? C10 P2 C19 C20 159.3(5) . . . . ? Eu1 P2 C19 C20 83.3(5) . . . . ? P2 C19 C20 C21 104.4(7) . . . . ? P2 C19 C20 C25 -75.7(8) . . . . ? C25 C20 C21 C22 -1.8(11) . . . . ? C19 C20 C21 C22 178.1(7) . . . . ? C20 C21 C22 C23 1.3(12) . . . . ? C21 C22 C23 C24 0.3(12) . . . . ? C22 C23 C24 C25 -1.2(12) . . . . ? C21 C20 C25 C24 0.9(11) . . . . ? C19 C20 C25 C24 -179.0(7) . . . . ? C23 C24 C25 C20 0.7(12) . . . . ? O6 P3 C26 C27 72.9(6) . . . . ? O3 P3 C26 C27 -159.4(5) . . . . ? C11 P3 C26 C27 -47.3(6) . . . . ? Eu1 P3 C26 C27 -123.6(5) . . . . ? P3 C26 C27 C32 -68.2(8) . . . . ? P3 C26 C27 C28 116.2(6) . . . . ? C32 C27 C28 C29 -1.1(10) . . . . ? C26 C27 C28 C29 174.7(6) . . . . ? C27 C28 C29 C30 0.6(10) . . . . ? C28 C29 C30 C31 0.7(11) . . . . ? C29 C30 C31 C32 -1.5(10) . . . . ? C30 C31 C32 C27 1.1(10) . . . . ? C28 C27 C32 C31 0.2(10) . . . . ? C26 C27 C32 C31 -175.4(6) . . . . ? O4 P1 O1 Eu1 97.0(3) . . . . ? C12 P1 O1 Eu1 -139.5(3) . . . . ? C9 P1 O1 Eu1 -23.0(4) . . . . ? O3 Eu1 O1 P1 -118.6(3) . . . . ? O4 Eu1 O1 P1 -52.2(3) 7_566 . . . ? O2 Eu1 O1 P1 171.4(3) . . . . ? N4 Eu1 O1 P1 1.4(4) . . . . ? N2 Eu1 O1 P1 102.5(3) . . . . ? N3 Eu1 O1 P1 119.0(3) . . . . ? N1 Eu1 O1 P1 34.6(3) . . . . ? P3 Eu1 O1 P1 -145.3(2) . . . . ? P2 Eu1 O1 P1 152.4(3) . . . . ? O5 P2 O2 Eu1 -138.8(3) . . . . ? C19 P2 O2 Eu1 94.4(3) . . . . ? C10 P2 O2 Eu1 -16.1(4) . . . . ? O3 Eu1 O2 P2 170.7(3) . . . . ? O4 Eu1 O2 P2 -120.8(3) 7_566 . . . ? O1 Eu1 O2 P2 -58.4(3) . . . . ? N4 Eu1 O2 P2 105.4(4) . . . . ? N2 Eu1 O2 P2 31.8(3) . . . . ? N3 Eu1 O2 P2 100.5(3) . . . . ? N1 Eu1 O2 P2 -5.6(4) . . . . ? P3 Eu1 O2 P2 152.1(3) . . . . ? P1 Eu1 O2 P2 -55.2(3) . . . . ? O6 P3 O3 Eu1 -142.0(3) . . . . ? C26 P3 O3 Eu1 94.1(4) . . . . ? C11 P3 O3 Eu1 -17.6(4) . . . . ? O4 Eu1 O3 P3 172.0(3) 7_566 . . . ? O2 Eu1 O3 P3 -53.9(3) . . . . ? O1 Eu1 O3 P3 -122.8(3) . . . . ? N4 Eu1 O3 P3 99.8(3) . . . . ? N2 Eu1 O3 P3 -1.2(4) . . . . ? N3 Eu1 O3 P3 33.2(3) . . . . ? N1 Eu1 O3 P3 119.8(4) . . . . ? P1 Eu1 O3 P3 -149.7(2) . . . . ? P2 Eu1 O3 P3 -50.5(3) . . . . ? O1 P1 O4 Eu1 -131.3(8) . . . 7_566 ? C12 P1 O4 Eu1 104.6(9) . . . 7_566 ? C9 P1 O4 Eu1 -11.8(9) . . . 7_566 ? Eu1 P1 O4 Eu1 -91.7(8) . . . 7_566 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O6 0.83(3) 1.98(3) 2.807(7) 176(8) . O1W H1WB O5 0.83(3) 2.10(3) 2.924(7) 173(8) 3 O2W H2WB O6 0.83(3) 1.94(3) 2.765(8) 173(11) . O3W H3WA O2W 0.83(3) 2.01(3) 2.838(8) 173(10) . O3W H3WB O5 0.83(3) 2.00(4) 2.798(7) 160(8) 3 O4W H4WA O1W 0.83(3) 1.98(4) 2.802(8) 172(12) . O4W H4WB O4W 0.83(3) 2.28(16) 2.800(17) 121(16) 2_656 O5W H5WA O3W 0.83(3) 1.97(5) 2.781(9) 164(13) . O5W H5WB O4W 0.83(3) 1.99(9) 2.729(11) 147(15) 4_646 O5W H5WC O5W 0.83(3) 2.08(9) 2.79(2) 144(15) 2_756 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.862 _refine_diff_density_min -2.580 _refine_diff_density_rms 0.146 #============================================================================== data_[Eu.L^3^]~2~.13H~2~O _database_code_depnum_ccdc_archive 'CCDC 618888' #============================================================================== _chemical_name_systematic ; bis((\m~2~-1-4-7-10-tetra-azacyclododecane-1,4,7,10-tetrayl-methyl- (trimethylene-tris(phenylphosphinato)))-europium(III)) tridecahydrate ; _chemical_name_common ; bis((mu!2$-1-4-7-10-tetra-azacyclododecane-1,4,7,10-tetrayl- methyl-(trimethylene-tris(phenylphosphinato)))-europium(iii)) tridecahydrate ; _chemical_melting_point 'not measured' _chemical_formula_moiety 'C64 H88 Eu2 N8 O12 P6, 13(O H2)' _chemical_formula_sum 'C64 H114 Eu2 N8 O25 P6' _chemical_formula_weight 1885.37 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' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2286(12) _cell_length_b 11.2774(12) _cell_length_c 16.8782(17) _cell_angle_alpha 98.094(2) _cell_angle_beta 107.307(2) _cell_angle_gamma 97.237(2) _cell_volume 1988.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3703 _cell_measurement_theta_min 2.428 _cell_measurement_theta_max 22.861 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 970 _exptl_absorpt_coefficient_mu 1.762 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.7084 _exptl_absorpt_correction_T_max 0.9665 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.1000 -1.00 0.00 0.00 0.1000 0.00 1.00 0.00 0.0300 0.00 -1.00 0.00 0.0300 0.00 0.00 1.00 0.0100 0.00 0.00 -1.00 0.0100 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 4 sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.44 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 19177 _diffrn_reflns_av_R_equivalents 0.1245 _diffrn_reflns_av_sigmaI/netI 0.1491 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7774 _reflns_number_gt 5288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0397P)^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 7774 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1149 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.32138(4) 0.44916(4) 0.31749(2) 0.01130(11) Uani 1 1 d . . . P1 P 0.51579(17) 0.33201(17) 0.47560(11) 0.0122(4) Uani 1 1 d . . . P2 P 0.10749(18) 0.18162(19) 0.27377(12) 0.0174(4) Uani 1 1 d . . . P3 P 0.07333(18) 0.59110(19) 0.23944(12) 0.0176(4) Uani 1 1 d . . . N1 N 0.5446(5) 0.3821(5) 0.3261(4) 0.0160(14) Uani 1 1 d . . . N2 N 0.2952(5) 0.2488(5) 0.2062(3) 0.0152(13) Uani 1 1 d . . . N3 N 0.2218(5) 0.4796(6) 0.1592(4) 0.0152(13) Uani 1 1 d . . . N4 N 0.4665(5) 0.6029(6) 0.2714(4) 0.0162(14) Uani 1 1 d . . . H4C H 0.4594 0.6769 0.2973 0.019 Uiso 1 1 calc R . . C1 C 0.5232(7) 0.2554(7) 0.2808(4) 0.0179(17) Uani 1 1 d . . . H1A H 0.5019 0.2007 0.3160 0.022 Uiso 1 1 calc R . . H1B H 0.6013 0.2388 0.2718 0.022 Uiso 1 1 calc R . . C2 C 0.4202(7) 0.2290(7) 0.1975(5) 0.0189(17) Uani 1 1 d . . . H2A H 0.4426 0.2812 0.1612 0.023 Uiso 1 1 calc R . . H2B H 0.4127 0.1453 0.1707 0.023 Uiso 1 1 calc R . . C3 C 0.2047(7) 0.2575(7) 0.1240(4) 0.0219(19) Uani 1 1 d . . . H3A H 0.1196 0.2458 0.1279 0.026 Uiso 1 1 calc R . . H3B H 0.2079 0.1921 0.0811 0.026 Uiso 1 1 calc R . . C4 C 0.2299(7) 0.3766(7) 0.0965(5) 0.0197(17) Uani 1 1 d . . . H4A H 0.3137 0.3879 0.0905 0.024 Uiso 1 1 calc R . . H4B H 0.1684 0.3754 0.0419 0.024 Uiso 1 1 calc R . . C5 C 0.2863(7) 0.5957(7) 0.1463(5) 0.0209(18) Uani 1 1 d . . . H5A H 0.2591 0.6636 0.1740 0.025 Uiso 1 1 calc R . . H5B H 0.2614 0.5976 0.0863 0.025 Uiso 1 1 calc R . . C6 C 0.4288(7) 0.6101(7) 0.1809(4) 0.0176(16) Uani 1 1 d . . . H6A H 0.4575 0.5463 0.1503 0.021 Uiso 1 1 calc R . . H6B H 0.4677 0.6879 0.1738 0.021 Uiso 1 1 calc R . . C7 C 0.6022(7) 0.5956(7) 0.3083(5) 0.0188(17) Uani 1 1 d . . . H7A H 0.6299 0.6246 0.3689 0.023 Uiso 1 1 calc R . . H7B H 0.6529 0.6468 0.2843 0.023 Uiso 1 1 calc R . . C8 C 0.6208(7) 0.4646(6) 0.2897(5) 0.0169(16) Uani 1 1 d . . . H8A H 0.5956 0.4370 0.2290 0.020 Uiso 1 1 calc R . . H8B H 0.7098 0.4605 0.3133 0.020 Uiso 1 1 calc R . . C9 C 0.6153(6) 0.3922(7) 0.4170(5) 0.0190(17) Uani 1 1 d . . . H9A H 0.6504 0.4771 0.4418 0.023 Uiso 1 1 calc R . . H9B H 0.6854 0.3483 0.4224 0.023 Uiso 1 1 calc R . . C10 C 0.2393(7) 0.1444(6) 0.2373(4) 0.0164(16) Uani 1 1 d . . . H10A H 0.3042 0.1245 0.2834 0.020 Uiso 1 1 calc R . . H10B H 0.2090 0.0736 0.1921 0.020 Uiso 1 1 calc R . . C11 C 0.0872(6) 0.4875(7) 0.1486(4) 0.0164(16) Uani 1 1 d . . . H11A H 0.0401 0.4071 0.1437 0.020 Uiso 1 1 calc R . . H11B H 0.0507 0.5170 0.0970 0.020 Uiso 1 1 calc R . . C12 C 0.5411(7) 0.1792(7) 0.4872(4) 0.0196(17) Uani 1 1 d . . . H12C H 0.4807 0.1224 0.4393 0.023 Uiso 1 1 calc R . . H12D H 0.6253 0.1717 0.4852 0.023 Uiso 1 1 calc R . . C13 C 0.5283(8) 0.1430(7) 0.5672(5) 0.0221(18) Uani 1 1 d . . . C14 C 0.6361(8) 0.1383(7) 0.6348(5) 0.0251(19) Uani 1 1 d . . . H14 H 0.7164 0.1563 0.6298 0.030 Uiso 1 1 calc R . . C15 C 0.6233(9) 0.1074(7) 0.7078(5) 0.032(2) Uani 1 1 d . . . H15 H 0.6956 0.1062 0.7522 0.039 Uiso 1 1 calc R . . C16 C 0.5065(10) 0.0782(8) 0.7171(5) 0.041(3) Uani 1 1 d . . . H16 H 0.4997 0.0545 0.7664 0.049 Uiso 1 1 calc R . . C17 C 0.3976(9) 0.0843(7) 0.6516(5) 0.032(2) Uani 1 1 d . . . H17 H 0.3179 0.0669 0.6576 0.038 Uiso 1 1 calc R . . C18 C 0.4097(8) 0.1169(7) 0.5766(5) 0.0227(18) Uani 1 1 d . . . H18 H 0.3376 0.1211 0.5329 0.027 Uiso 1 1 calc R . . C19 C 0.1328(7) 0.1252(7) 0.3713(5) 0.0191(17) Uani 1 1 d . . . H19A H 0.1100 0.0371 0.3582 0.023 Uiso 1 1 calc R . . H19B H 0.2223 0.1459 0.4036 0.023 Uiso 1 1 calc R . . C20 C 0.0586(7) 0.1743(7) 0.4250(5) 0.0202(17) Uani 1 1 d . . . C21 C -0.0450(7) 0.1018(7) 0.4328(5) 0.0259(19) Uani 1 1 d . . . H21 H -0.0707 0.0221 0.4030 0.031 Uiso 1 1 calc R . . C22 C -0.1105(8) 0.1474(9) 0.4846(5) 0.034(2) Uani 1 1 d . . . H22 H -0.1770 0.0962 0.4914 0.041 Uiso 1 1 calc R . . C23 C -0.0792(8) 0.2675(8) 0.5266(5) 0.031(2) Uani 1 1 d . . . H23 H -0.1265 0.2993 0.5585 0.037 Uiso 1 1 calc R . . C24 C 0.0253(8) 0.3381(8) 0.5190(5) 0.029(2) Uani 1 1 d . . . H24 H 0.0508 0.4181 0.5482 0.035 Uiso 1 1 calc R . . C25 C 0.0914(8) 0.2930(8) 0.4699(5) 0.033(2) Uani 1 1 d . . . H25 H 0.1611 0.3433 0.4661 0.039 Uiso 1 1 calc R . . C26 C -0.0617(7) 0.5166(8) 0.2617(5) 0.0238(19) Uani 1 1 d . . . H26A H -0.0358 0.4533 0.2931 0.029 Uiso 1 1 calc R . . H26B H -0.0883 0.5754 0.2975 0.029 Uiso 1 1 calc R . . C27 C -0.1733(7) 0.4605(9) 0.1845(5) 0.027(2) Uani 1 1 d . . . C28 C -0.2108(8) 0.3364(9) 0.1629(5) 0.037(2) Uani 1 1 d . . . H28 H -0.1640 0.2868 0.1945 0.044 Uiso 1 1 calc R . . C29 C -0.3198(9) 0.2830(11) 0.0932(7) 0.059(4) Uani 1 1 d . . . H29 H -0.3460 0.1990 0.0795 0.071 Uiso 1 1 calc R . . C30 C -0.3862(9) 0.3577(14) 0.0459(6) 0.061(4) Uani 1 1 d . . . H30 H -0.4577 0.3240 -0.0003 0.074 Uiso 1 1 calc R . . C31 C -0.3471(8) 0.4824(12) 0.0667(6) 0.050(3) Uani 1 1 d . . . H31 H -0.3931 0.5319 0.0346 0.060 Uiso 1 1 calc R . . C32 C -0.2412(7) 0.5341(10) 0.1343(5) 0.034(2) Uani 1 1 d . . . H32 H -0.2146 0.6180 0.1467 0.041 Uiso 1 1 calc R . . O1 O 0.3805(4) 0.3267(4) 0.4216(3) 0.0131(11) Uani 1 1 d . . . O2 O 0.1304(4) 0.3203(4) 0.2934(3) 0.0164(11) Uani 1 1 d . . . O3 O 0.1920(4) 0.5921(4) 0.3131(3) 0.0145(11) Uani 1 1 d . . . O4 O 0.5583(4) 0.4098(4) 0.5626(3) 0.0176(11) Uani 1 1 d . . . O5 O -0.0182(5) 0.1185(5) 0.2130(3) 0.0280(14) Uani 1 1 d . . . O6 O 0.0507(5) 0.7132(5) 0.2185(3) 0.0278(13) Uani 1 1 d . . . O1W O 0.0342(6) 0.7879(6) 0.0695(4) 0.0468(17) Uani 1 1 d . . . O2W O 0.5132(7) 0.9606(7) 0.0765(4) 0.054(2) Uani 1 1 d . . . O3W O 0.8856(7) 0.9717(6) 0.0584(4) 0.060(2) Uani 1 1 d . . . O4W O 0.2595(7) 0.9247(7) 0.0682(4) 0.055(2) Uani 1 1 d . . . O5W O 0.6892(7) 0.8139(9) 0.0872(7) 0.095(3) Uani 1 1 d . . . O6W O 0.8903(8) 0.8712(10) 0.2499(6) 0.053(3) Uani 0.75 1 d P A 1 O7W O 0.7466(14) 0.0591(14) 0.2303(9) 0.059(4) Uiso 0.50 1 d P B 2 O8W O 0.826(2) 0.804(2) 0.2422(15) 0.028(6) Uiso 0.25 1 d P C 3 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 0.00976(18) 0.01193(19) 0.00915(17) -0.00100(13) 0.00019(13) 0.00118(13) P1 0.0119(10) 0.0113(10) 0.0114(9) 0.0003(8) 0.0016(8) 0.0019(8) P2 0.0160(10) 0.0181(11) 0.0148(10) -0.0008(8) 0.0036(8) -0.0012(8) P3 0.0147(10) 0.0223(11) 0.0152(10) 0.0034(9) 0.0029(8) 0.0059(8) N1 0.019(3) 0.012(3) 0.015(3) -0.002(3) 0.003(3) 0.004(3) N2 0.019(3) 0.015(3) 0.010(3) 0.001(2) 0.004(3) -0.001(3) N3 0.013(3) 0.021(3) 0.014(3) 0.008(3) 0.005(3) 0.003(3) N4 0.010(3) 0.022(4) 0.013(3) -0.001(3) 0.001(2) 0.000(3) C1 0.018(4) 0.019(4) 0.020(4) 0.010(3) 0.008(3) 0.003(3) C2 0.023(4) 0.016(4) 0.021(4) -0.004(3) 0.014(3) 0.008(3) C3 0.017(4) 0.030(5) 0.010(4) -0.001(3) -0.003(3) -0.002(4) C4 0.022(4) 0.020(4) 0.015(4) -0.002(3) 0.003(3) 0.006(3) C5 0.024(4) 0.022(4) 0.015(4) 0.001(3) 0.006(3) -0.001(3) C6 0.022(4) 0.016(4) 0.018(4) 0.008(3) 0.008(3) 0.002(3) C7 0.018(4) 0.021(4) 0.017(4) 0.001(3) 0.007(3) 0.000(3) C8 0.022(4) 0.012(4) 0.018(4) 0.005(3) 0.006(3) 0.004(3) C9 0.007(4) 0.016(4) 0.031(4) 0.003(3) 0.002(3) 0.001(3) C10 0.019(4) 0.010(4) 0.013(4) -0.007(3) 0.000(3) -0.001(3) C11 0.012(4) 0.023(4) 0.011(4) -0.001(3) -0.001(3) 0.007(3) C12 0.020(4) 0.018(4) 0.018(4) -0.004(3) 0.007(3) -0.001(3) C13 0.035(5) 0.009(4) 0.020(4) 0.002(3) 0.008(4) -0.002(3) C14 0.038(5) 0.009(4) 0.027(5) 0.000(3) 0.006(4) 0.012(4) C15 0.049(6) 0.016(5) 0.020(4) 0.000(4) -0.004(4) 0.004(4) C16 0.082(8) 0.015(5) 0.024(5) 0.011(4) 0.015(5) -0.001(5) C17 0.044(5) 0.018(5) 0.031(5) 0.006(4) 0.010(4) -0.004(4) C18 0.026(4) 0.022(4) 0.022(4) 0.002(3) 0.012(4) -0.002(3) C19 0.014(4) 0.016(4) 0.027(4) 0.005(3) 0.007(3) -0.003(3) C20 0.015(4) 0.026(5) 0.017(4) 0.012(3) -0.001(3) 0.001(3) C21 0.019(4) 0.020(4) 0.036(5) -0.003(4) 0.008(4) 0.006(3) C22 0.021(4) 0.047(6) 0.029(5) -0.002(4) 0.007(4) -0.006(4) C23 0.032(5) 0.043(6) 0.017(4) 0.005(4) 0.005(4) 0.012(4) C24 0.047(6) 0.026(5) 0.016(4) 0.001(4) 0.010(4) 0.010(4) C25 0.041(5) 0.031(5) 0.023(4) 0.007(4) 0.009(4) -0.007(4) C26 0.016(4) 0.038(5) 0.015(4) 0.003(4) 0.003(3) 0.003(4) C27 0.013(4) 0.053(6) 0.016(4) -0.001(4) 0.008(3) 0.007(4) C28 0.021(5) 0.050(6) 0.032(5) -0.013(4) 0.006(4) 0.010(4) C29 0.027(5) 0.080(9) 0.051(7) -0.042(6) 0.012(5) 0.002(6) C30 0.022(5) 0.123(12) 0.022(5) -0.025(6) 0.000(4) 0.010(7) C31 0.020(5) 0.109(11) 0.023(5) 0.015(6) 0.008(4) 0.015(6) C32 0.008(4) 0.073(7) 0.024(5) 0.022(5) 0.004(3) 0.002(4) O1 0.012(2) 0.014(3) 0.011(2) 0.003(2) -0.001(2) 0.003(2) O2 0.014(3) 0.020(3) 0.013(3) 0.000(2) 0.006(2) -0.002(2) O3 0.013(2) 0.014(3) 0.017(3) 0.005(2) 0.004(2) 0.004(2) O4 0.019(3) 0.019(3) 0.010(2) 0.003(2) -0.002(2) 0.003(2) O5 0.023(3) 0.028(3) 0.022(3) -0.008(2) 0.000(2) -0.004(2) O6 0.029(3) 0.028(3) 0.027(3) 0.010(3) 0.005(3) 0.015(3) O1W 0.055(4) 0.048(4) 0.038(4) 0.009(3) 0.017(3) 0.009(3) O2W 0.065(5) 0.059(5) 0.031(4) 0.012(3) 0.011(4) -0.010(4) O3W 0.087(6) 0.043(4) 0.030(4) 0.000(3) -0.013(4) 0.020(4) O4W 0.049(4) 0.077(6) 0.046(4) 0.022(4) 0.017(4) 0.020(4) O5W 0.042(5) 0.093(7) 0.136(9) 0.063(6) -0.010(5) 0.008(5) O6W 0.032(5) 0.064(7) 0.059(6) 0.006(5) 0.008(5) 0.013(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 Eu1 O3 2.297(5) . ? Eu1 O4 2.319(5) 2_666 ? Eu1 O2 2.325(5) . ? Eu1 O1 2.379(5) . ? Eu1 N4 2.586(6) . ? Eu1 N2 2.651(6) . ? Eu1 N3 2.661(6) . ? Eu1 N1 2.677(6) . ? Eu1 P3 3.404(2) . ? Eu1 P1 3.4476(19) . ? Eu1 P2 3.451(2) . ? P1 O4 1.506(5) . ? P1 O1 1.510(5) . ? P1 C12 1.809(8) . ? P1 C9 1.828(8) . ? P2 O5 1.494(5) . ? P2 O2 1.525(5) . ? P2 C19 1.805(8) . ? P2 C10 1.836(7) . ? P3 O6 1.503(6) . ? P3 O3 1.525(5) . ? P3 C26 1.803(8) . ? P3 C11 1.850(7) . ? N1 C1 1.476(9) . ? N1 C9 1.484(9) . ? N1 C8 1.500(9) . ? N2 C3 1.480(9) . ? N2 C2 1.494(9) . ? N2 C10 1.497(9) . ? N3 C11 1.484(9) . ? N3 C4 1.488(9) . ? N3 C5 1.492(9) . ? N4 C6 1.475(9) . ? N4 C7 1.483(9) . ? N4 H4C 0.9100 . ? C1 C2 1.494(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.503(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.510(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.520(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.507(10) . ? C12 H12C 0.9700 . ? C12 H12D 0.9700 . ? C13 C18 1.388(11) . ? C13 C14 1.407(11) . ? C14 C15 1.369(12) . ? C14 H14 0.9300 . ? C15 C16 1.372(13) . ? C15 H15 0.9300 . ? C16 C17 1.400(13) . ? C16 H16 0.9300 . ? C17 C18 1.405(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.498(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.386(11) . ? C20 C25 1.387(11) . ? C21 C22 1.387(11) . ? C21 H21 0.9300 . ? C22 C23 1.387(12) . ? C22 H22 0.9300 . ? C23 C24 1.382(12) . ? C23 H23 0.9300 . ? C24 C25 1.357(12) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.505(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.373(12) . ? C27 C32 1.400(12) . ? C28 C29 1.415(12) . ? C28 H28 0.9300 . ? C29 C30 1.377(17) . ? C29 H29 0.9300 . ? C30 C31 1.381(16) . ? C30 H30 0.9300 . ? C31 C32 1.373(12) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? O4 Eu1 2.319(4) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Eu1 O4 79.96(17) . 2_666 ? O3 Eu1 O2 81.09(17) . . ? O4 Eu1 O2 129.00(17) 2_666 . ? O3 Eu1 O1 127.79(16) . . ? O4 Eu1 O1 76.85(16) 2_666 . ? O2 Eu1 O1 78.51(16) . . ? O3 Eu1 N4 86.47(18) . . ? O4 Eu1 N4 72.80(18) 2_666 . ? O2 Eu1 N4 151.63(17) . . ? O1 Eu1 N4 128.40(17) . . ? O3 Eu1 N2 129.15(17) . . ? O4 Eu1 N2 150.54(18) 2_666 . ? O2 Eu1 N2 68.46(17) . . ? O1 Eu1 N2 85.65(17) . . ? N4 Eu1 N2 101.37(18) . . ? O3 Eu1 N3 69.93(17) . . ? O4 Eu1 N3 129.93(18) 2_666 . ? O2 Eu1 N3 85.31(17) . . ? O1 Eu1 N3 152.74(17) . . ? N4 Eu1 N3 66.45(17) . . ? N2 Eu1 N3 67.94(18) . . ? O3 Eu1 N1 152.27(17) . . ? O4 Eu1 N1 83.36(17) 2_666 . ? O2 Eu1 N1 126.44(18) . . ? O1 Eu1 N1 68.45(17) . . ? N4 Eu1 N1 67.43(19) . . ? N2 Eu1 N1 68.11(17) . . ? N3 Eu1 N1 105.61(18) . . ? O3 Eu1 P3 21.61(12) . . ? O4 Eu1 P3 101.34(13) 2_666 . ? O2 Eu1 P3 69.68(13) . . ? O1 Eu1 P3 137.06(12) . . ? N4 Eu1 P3 89.79(14) . . ? N2 Eu1 P3 107.57(13) . . ? N3 Eu1 P3 52.28(13) . . ? N1 Eu1 P3 154.48(14) . . ? O3 Eu1 P1 135.05(12) . . ? O4 Eu1 P1 64.60(13) 2_666 . ? O2 Eu1 P1 99.80(13) . . ? O1 Eu1 P1 21.47(11) . . ? N4 Eu1 P1 106.95(13) . . ? N2 Eu1 P1 90.90(13) . . ? N3 Eu1 P1 154.87(13) . . ? N1 Eu1 P1 51.77(13) . . ? P3 Eu1 P1 152.33(5) . . ? O3 Eu1 P2 101.79(12) . . ? O4 Eu1 P2 136.18(13) 2_666 . ? O2 Eu1 P2 20.91(13) . . ? O1 Eu1 P2 67.69(11) . . ? N4 Eu1 P2 150.59(13) . . ? N2 Eu1 P2 51.68(13) . . ? N3 Eu1 P2 89.70(13) . . ? N1 Eu1 P2 105.58(13) . . ? P3 Eu1 P2 88.48(5) . . ? P1 Eu1 P2 87.17(5) . . ? O4 P1 O1 116.8(3) . . ? O4 P1 C12 107.9(3) . . ? O1 P1 C12 109.0(3) . . ? O4 P1 C9 108.0(3) . . ? O1 P1 C9 106.1(3) . . ? C12 P1 C9 108.8(3) . . ? O4 P1 Eu1 115.7(2) . . ? O1 P1 Eu1 35.21(18) . . ? C12 P1 Eu1 133.2(2) . . ? C9 P1 Eu1 73.6(2) . . ? O5 P2 O2 117.2(3) . . ? O5 P2 C19 108.9(3) . . ? O2 P2 C19 109.0(3) . . ? O5 P2 C10 112.0(3) . . ? O2 P2 C10 104.5(3) . . ? C19 P2 C10 104.4(3) . . ? O5 P2 Eu1 140.7(3) . . ? O2 P2 Eu1 32.97(18) . . ? C19 P2 Eu1 106.9(2) . . ? C10 P2 Eu1 73.3(2) . . ? O6 P3 O3 115.8(3) . . ? O6 P3 C26 109.8(4) . . ? O3 P3 C26 108.3(3) . . ? O6 P3 C11 111.8(3) . . ? O3 P3 C11 105.6(3) . . ? C26 P3 C11 105.0(4) . . ? O6 P3 Eu1 138.9(2) . . ? O3 P3 Eu1 33.69(19) . . ? C26 P3 Eu1 107.7(3) . . ? C11 P3 Eu1 73.3(2) . . ? C1 N1 C9 110.6(6) . . ? C1 N1 C8 109.9(5) . . ? C9 N1 C8 108.3(5) . . ? C1 N1 Eu1 109.6(4) . . ? C9 N1 Eu1 106.8(4) . . ? C8 N1 Eu1 111.6(4) . . ? C3 N2 C2 111.1(5) . . ? C3 N2 C10 108.0(5) . . ? C2 N2 C10 109.9(6) . . ? C3 N2 Eu1 109.2(4) . . ? C2 N2 Eu1 111.1(4) . . ? C10 N2 Eu1 107.4(4) . . ? C11 N3 C4 110.2(5) . . ? C11 N3 C5 109.0(6) . . ? C4 N3 C5 109.5(6) . . ? C11 N3 Eu1 105.5(4) . . ? C4 N3 Eu1 112.2(4) . . ? C5 N3 Eu1 110.4(4) . . ? C6 N4 C7 113.6(6) . . ? C6 N4 Eu1 117.1(4) . . ? C7 N4 Eu1 111.9(4) . . ? C6 N4 H4C 104.2 . . ? C7 N4 H4C 104.2 . . ? Eu1 N4 H4C 104.2 . . ? N1 C1 C2 113.6(6) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N2 C2 C1 112.2(6) . . ? N2 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? N2 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N2 C3 C4 113.9(6) . . ? N2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? N3 C4 C3 110.7(6) . . ? N3 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 111.9(6) . . ? N3 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? N3 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N4 C6 C5 109.3(6) . . ? N4 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N4 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N4 C7 C8 109.7(6) . . ? N4 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N4 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N1 C8 C7 111.5(6) . . ? N1 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N1 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N1 C9 P1 112.6(5) . . ? N1 C9 H9A 109.1 . . ? P1 C9 H9A 109.1 . . ? N1 C9 H9B 109.1 . . ? P1 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? N2 C10 P2 111.1(5) . . ? N2 C10 H10A 109.4 . . ? P2 C10 H10A 109.4 . . ? N2 C10 H10B 109.4 . . ? P2 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N3 C11 P3 111.0(5) . . ? N3 C11 H11A 109.4 . . ? P3 C11 H11A 109.4 . . ? N3 C11 H11B 109.4 . . ? P3 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 P1 114.8(5) . . ? C13 C12 H12C 108.6 . . ? P1 C12 H12C 108.6 . . ? C13 C12 H12D 108.6 . . ? P1 C12 H12D 108.6 . . ? H12C C12 H12D 107.5 . . ? C18 C13 C14 118.7(7) . . ? C18 C13 C12 120.4(7) . . ? C14 C13 C12 120.9(7) . . ? C15 C14 C13 120.3(8) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 121.7(8) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C17 119.3(8) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 119.5(8) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 120.5(8) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 P2 114.0(5) . . ? C20 C19 H19A 108.8 . . ? P2 C19 H19A 108.8 . . ? C20 C19 H19B 108.8 . . ? P2 C19 H19B 108.8 . . ? H19A C19 H19B 107.6 . . ? C21 C20 C25 117.2(8) . . ? C21 C20 C19 121.0(7) . . ? C25 C20 C19 121.8(7) . . ? C20 C21 C22 120.4(8) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 121.5(8) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C24 C23 C22 117.2(8) . . ? C24 C23 H23 121.4 . . ? C22 C23 H23 121.4 . . ? C25 C24 C23 121.3(8) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C20 122.2(8) . . ? C24 C25 H25 118.9 . . ? C20 C25 H25 118.9 . . ? C27 C26 P3 114.4(5) . . ? C27 C26 H26A 108.7 . . ? P3 C26 H26A 108.7 . . ? C27 C26 H26B 108.7 . . ? P3 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C32 119.1(8) . . ? C28 C27 C26 120.4(8) . . ? C32 C27 C26 120.5(8) . . ? C27 C28 C29 120.9(10) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 118.7(11) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C31 120.4(9) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C32 C31 C30 120.8(11) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C27 120.0(10) . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? P1 O1 Eu1 123.3(3) . . ? P2 O2 Eu1 126.1(3) . . ? P3 O3 Eu1 124.7(3) . . ? P1 O4 Eu1 161.5(3) . 2_666 ? 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 O3 Eu1 P1 O4 -21.0(3) . . . . ? O4 Eu1 P1 O4 20.5(3) 2_666 . . . ? O2 Eu1 P1 O4 -108.1(3) . . . . ? O1 Eu1 P1 O4 -100.8(4) . . . . ? N4 Eu1 P1 O4 81.4(3) . . . . ? N2 Eu1 P1 O4 -176.4(3) . . . . ? N3 Eu1 P1 O4 151.9(4) . . . . ? N1 Eu1 P1 O4 122.7(3) . . . . ? P3 Eu1 P1 O4 -43.6(3) . . . . ? P2 Eu1 P1 O4 -124.9(2) . . . . ? O3 Eu1 P1 O1 79.8(4) . . . . ? O4 Eu1 P1 O1 121.3(3) 2_666 . . . ? O2 Eu1 P1 O1 -7.4(3) . . . . ? N4 Eu1 P1 O1 -177.8(3) . . . . ? N2 Eu1 P1 O1 -75.7(3) . . . . ? N3 Eu1 P1 O1 -107.4(4) . . . . ? N1 Eu1 P1 O1 -136.5(4) . . . . ? P3 Eu1 P1 O1 57.2(3) . . . . ? P2 Eu1 P1 O1 -24.1(3) . . . . ? O3 Eu1 P1 C12 135.9(4) . . . . ? O4 Eu1 P1 C12 177.4(4) 2_666 . . . ? O2 Eu1 P1 C12 48.7(4) . . . . ? O1 Eu1 P1 C12 56.1(5) . . . . ? N4 Eu1 P1 C12 -121.7(4) . . . . ? N2 Eu1 P1 C12 -19.6(4) . . . . ? N3 Eu1 P1 C12 -51.2(5) . . . . ? N1 Eu1 P1 C12 -80.4(4) . . . . ? P3 Eu1 P1 C12 113.3(3) . . . . ? P2 Eu1 P1 C12 32.0(3) . . . . ? O3 Eu1 P1 C9 -123.4(3) . . . . ? O4 Eu1 P1 C9 -81.9(3) 2_666 . . . ? O2 Eu1 P1 C9 149.4(3) . . . . ? O1 Eu1 P1 C9 156.8(4) . . . . ? N4 Eu1 P1 C9 -21.1(3) . . . . ? N2 Eu1 P1 C9 81.1(3) . . . . ? N3 Eu1 P1 C9 49.4(4) . . . . ? N1 Eu1 P1 C9 20.2(3) . . . . ? P3 Eu1 P1 C9 -146.0(3) . . . . ? P2 Eu1 P1 C9 132.7(3) . . . . ? O3 Eu1 P2 O5 47.8(4) . . . . ? O4 Eu1 P2 O5 135.5(4) 2_666 . . . ? O2 Eu1 P2 O5 55.9(5) . . . . ? O1 Eu1 P2 O5 174.0(4) . . . . ? N4 Eu1 P2 O5 -56.3(5) . . . . ? N2 Eu1 P2 O5 -83.3(4) . . . . ? N3 Eu1 P2 O5 -21.7(4) . . . . ? N1 Eu1 P2 O5 -127.8(4) . . . . ? P3 Eu1 P2 O5 30.6(4) . . . . ? P1 Eu1 P2 O5 -176.7(4) . . . . ? O3 Eu1 P2 O2 -8.2(4) . . . . ? O4 Eu1 P2 O2 79.6(4) 2_666 . . . ? O1 Eu1 P2 O2 118.1(4) . . . . ? N4 Eu1 P2 O2 -112.2(4) . . . . ? N2 Eu1 P2 O2 -139.2(4) . . . . ? N3 Eu1 P2 O2 -77.6(4) . . . . ? N1 Eu1 P2 O2 176.3(4) . . . . ? P3 Eu1 P2 O2 -25.3(3) . . . . ? P1 Eu1 P2 O2 127.4(3) . . . . ? O3 Eu1 P2 C19 -107.2(3) . . . . ? O4 Eu1 P2 C19 -19.5(3) 2_666 . . . ? O2 Eu1 P2 C19 -99.1(4) . . . . ? O1 Eu1 P2 C19 19.0(3) . . . . ? N4 Eu1 P2 C19 148.7(4) . . . . ? N2 Eu1 P2 C19 121.7(3) . . . . ? N3 Eu1 P2 C19 -176.7(3) . . . . ? N1 Eu1 P2 C19 77.2(3) . . . . ? P3 Eu1 P2 C19 -124.4(3) . . . . ? P1 Eu1 P2 C19 28.3(3) . . . . ? O3 Eu1 P2 C10 152.4(3) . . . . ? O4 Eu1 P2 C10 -119.9(3) 2_666 . . . ? O2 Eu1 P2 C10 160.5(4) . . . . ? O1 Eu1 P2 C10 -81.4(3) . . . . ? N4 Eu1 P2 C10 48.4(4) . . . . ? N2 Eu1 P2 C10 21.3(3) . . . . ? N3 Eu1 P2 C10 83.0(3) . . . . ? N1 Eu1 P2 C10 -23.2(3) . . . . ? P3 Eu1 P2 C10 135.2(2) . . . . ? P1 Eu1 P2 C10 -72.1(2) . . . . ? O3 Eu1 P3 O6 58.5(5) . . . . ? O4 Eu1 P3 O6 50.0(4) 2_666 . . . ? O2 Eu1 P3 O6 177.6(4) . . . . ? O1 Eu1 P3 O6 132.8(4) . . . . ? N4 Eu1 P3 O6 -22.4(4) . . . . ? N2 Eu1 P3 O6 -124.3(4) . . . . ? N3 Eu1 P3 O6 -82.3(4) . . . . ? N1 Eu1 P3 O6 -48.5(5) . . . . ? P1 Eu1 P3 O6 105.9(4) . . . . ? P2 Eu1 P3 O6 -173.1(4) . . . . ? O4 Eu1 P3 O3 -8.5(3) 2_666 . . . ? O2 Eu1 P3 O3 119.1(4) . . . . ? O1 Eu1 P3 O3 74.3(4) . . . . ? N4 Eu1 P3 O3 -80.9(4) . . . . ? N2 Eu1 P3 O3 177.2(4) . . . . ? N3 Eu1 P3 O3 -140.7(4) . . . . ? N1 Eu1 P3 O3 -106.9(4) . . . . ? P1 Eu1 P3 O3 47.5(4) . . . . ? P2 Eu1 P3 O3 128.5(3) . . . . ? O3 Eu1 P3 C26 -96.5(4) . . . . ? O4 Eu1 P3 C26 -105.0(3) 2_666 . . . ? O2 Eu1 P3 C26 22.6(3) . . . . ? O1 Eu1 P3 C26 -22.2(3) . . . . ? N4 Eu1 P3 C26 -177.4(3) . . . . ? N2 Eu1 P3 C26 80.7(3) . . . . ? N3 Eu1 P3 C26 122.8(3) . . . . ? N1 Eu1 P3 C26 156.6(4) . . . . ? P1 Eu1 P3 C26 -49.0(3) . . . . ? P2 Eu1 P3 C26 32.0(3) . . . . ? O3 Eu1 P3 C11 162.7(4) . . . . ? O4 Eu1 P3 C11 154.2(3) 2_666 . . . ? O2 Eu1 P3 C11 -78.2(3) . . . . ? O1 Eu1 P3 C11 -123.0(3) . . . . ? N4 Eu1 P3 C11 81.8(3) . . . . ? N2 Eu1 P3 C11 -20.1(3) . . . . ? N3 Eu1 P3 C11 21.9(3) . . . . ? N1 Eu1 P3 C11 55.8(4) . . . . ? P1 Eu1 P3 C11 -149.9(3) . . . . ? P2 Eu1 P3 C11 -68.9(3) . . . . ? O3 Eu1 N1 C1 -149.5(4) . . . . ? O4 Eu1 N1 C1 157.3(5) 2_666 . . . ? O2 Eu1 N1 C1 22.7(5) . . . . ? O1 Eu1 N1 C1 78.8(4) . . . . ? N4 Eu1 N1 C1 -128.6(5) . . . . ? N2 Eu1 N1 C1 -15.2(4) . . . . ? N3 Eu1 N1 C1 -73.0(5) . . . . ? P3 Eu1 N1 C1 -100.3(5) . . . . ? P1 Eu1 N1 C1 94.5(4) . . . . ? P2 Eu1 N1 C1 21.1(4) . . . . ? O3 Eu1 N1 C9 90.7(5) . . . . ? O4 Eu1 N1 C9 37.4(4) 2_666 . . . ? O2 Eu1 N1 C9 -97.1(4) . . . . ? O1 Eu1 N1 C9 -41.0(4) . . . . ? N4 Eu1 N1 C9 111.5(4) . . . . ? N2 Eu1 N1 C9 -135.1(5) . . . . ? N3 Eu1 N1 C9 167.1(4) . . . . ? P3 Eu1 N1 C9 139.9(4) . . . . ? P1 Eu1 N1 C9 -25.3(4) . . . . ? P2 Eu1 N1 C9 -98.7(4) . . . . ? O3 Eu1 N1 C8 -27.5(6) . . . . ? O4 Eu1 N1 C8 -80.7(4) 2_666 . . . ? O2 Eu1 N1 C8 144.7(4) . . . . ? O1 Eu1 N1 C8 -159.2(4) . . . . ? N4 Eu1 N1 C8 -6.6(4) . . . . ? N2 Eu1 N1 C8 106.8(4) . . . . ? N3 Eu1 N1 C8 48.9(4) . . . . ? P3 Eu1 N1 C8 21.7(6) . . . . ? P1 Eu1 N1 C8 -143.5(5) . . . . ? P2 Eu1 N1 C8 143.1(4) . . . . ? O3 Eu1 N2 C3 18.3(5) . . . . ? O4 Eu1 N2 C3 -151.6(4) 2_666 . . . ? O2 Eu1 N2 C3 75.8(4) . . . . ? O1 Eu1 N2 C3 155.2(4) . . . . ? N4 Eu1 N2 C3 -76.5(4) . . . . ? N3 Eu1 N2 C3 -17.9(4) . . . . ? N1 Eu1 N2 C3 -136.3(5) . . . . ? P3 Eu1 N2 C3 16.9(4) . . . . ? P1 Eu1 N2 C3 176.0(4) . . . . ? P2 Eu1 N2 C3 90.3(4) . . . . ? O3 Eu1 N2 C2 141.2(4) . . . . ? O4 Eu1 N2 C2 -28.6(6) 2_666 . . . ? O2 Eu1 N2 C2 -161.2(5) . . . . ? O1 Eu1 N2 C2 -81.9(4) . . . . ? N4 Eu1 N2 C2 46.4(5) . . . . ? N3 Eu1 N2 C2 105.0(5) . . . . ? N1 Eu1 N2 C2 -13.4(4) . . . . ? P3 Eu1 N2 C2 139.9(4) . . . . ? P1 Eu1 N2 C2 -61.0(4) . . . . ? P2 Eu1 N2 C2 -146.7(5) . . . . ? O3 Eu1 N2 C10 -98.6(4) . . . . ? O4 Eu1 N2 C10 91.5(5) 2_666 . . . ? O2 Eu1 N2 C10 -41.1(4) . . . . ? O1 Eu1 N2 C10 38.3(4) . . . . ? N4 Eu1 N2 C10 166.6(4) . . . . ? N3 Eu1 N2 C10 -134.8(5) . . . . ? N1 Eu1 N2 C10 106.8(4) . . . . ? P3 Eu1 N2 C10 -99.9(4) . . . . ? P1 Eu1 N2 C10 59.1(4) . . . . ? P2 Eu1 N2 C10 -26.5(4) . . . . ? O3 Eu1 N3 C11 -41.9(4) . . . . ? O4 Eu1 N3 C11 -98.7(4) 2_666 . . . ? O2 Eu1 N3 C11 40.3(4) . . . . ? O1 Eu1 N3 C11 93.7(5) . . . . ? N4 Eu1 N3 C11 -137.0(5) . . . . ? N2 Eu1 N3 C11 108.9(4) . . . . ? N1 Eu1 N3 C11 166.9(4) . . . . ? P3 Eu1 N3 C11 -27.6(4) . . . . ? P1 Eu1 N3 C11 143.4(4) . . . . ? P2 Eu1 N3 C11 60.7(4) . . . . ? O3 Eu1 N3 C4 -161.9(5) . . . . ? O4 Eu1 N3 C4 141.3(4) 2_666 . . . ? O2 Eu1 N3 C4 -79.7(5) . . . . ? O1 Eu1 N3 C4 -26.2(7) . . . . ? N4 Eu1 N3 C4 103.1(5) . . . . ? N2 Eu1 N3 C4 -11.1(4) . . . . ? N1 Eu1 N3 C4 46.9(5) . . . . ? P3 Eu1 N3 C4 -147.5(5) . . . . ? P1 Eu1 N3 C4 23.4(6) . . . . ? P2 Eu1 N3 C4 -59.2(4) . . . . ? O3 Eu1 N3 C5 75.7(5) . . . . ? O4 Eu1 N3 C5 18.9(5) 2_666 . . . ? O2 Eu1 N3 C5 157.9(5) . . . . ? O1 Eu1 N3 C5 -148.6(4) . . . . ? N4 Eu1 N3 C5 -19.3(4) . . . . ? N2 Eu1 N3 C5 -133.4(5) . . . . ? N1 Eu1 N3 C5 -75.5(5) . . . . ? P3 Eu1 N3 C5 90.1(5) . . . . ? P1 Eu1 N3 C5 -98.9(5) . . . . ? P2 Eu1 N3 C5 178.4(4) . . . . ? O3 Eu1 N4 C6 -79.6(5) . . . . ? O4 Eu1 N4 C6 -160.2(5) 2_666 . . . ? O2 Eu1 N4 C6 -15.8(7) . . . . ? O1 Eu1 N4 C6 143.1(4) . . . . ? N2 Eu1 N4 C6 49.6(5) . . . . ? N3 Eu1 N4 C6 -10.0(5) . . . . ? N1 Eu1 N4 C6 110.0(5) . . . . ? P3 Eu1 N4 C6 -58.2(5) . . . . ? P1 Eu1 N4 C6 144.1(5) . . . . ? P2 Eu1 N4 C6 28.3(7) . . . . ? O3 Eu1 N4 C7 146.7(4) . . . . ? O4 Eu1 N4 C7 66.1(4) 2_666 . . . ? O2 Eu1 N4 C7 -149.5(4) . . . . ? O1 Eu1 N4 C7 9.4(5) . . . . ? N2 Eu1 N4 C7 -84.0(4) . . . . ? N3 Eu1 N4 C7 -143.7(5) . . . . ? N1 Eu1 N4 C7 -23.7(4) . . . . ? P3 Eu1 N4 C7 168.1(4) . . . . ? P1 Eu1 N4 C7 10.5(5) . . . . ? P2 Eu1 N4 C7 -105.4(4) . . . . ? C9 N1 C1 C2 161.7(6) . . . . ? C8 N1 C1 C2 -78.7(7) . . . . ? Eu1 N1 C1 C2 44.2(7) . . . . ? C3 N2 C2 C1 163.5(6) . . . . ? C10 N2 C2 C1 -77.0(7) . . . . ? Eu1 N2 C2 C1 41.7(7) . . . . ? N1 C1 C2 N2 -60.3(8) . . . . ? C2 N2 C3 C4 -75.3(8) . . . . ? C10 N2 C3 C4 164.1(6) . . . . ? Eu1 N2 C3 C4 47.6(7) . . . . ? C11 N3 C4 C3 -78.3(7) . . . . ? C5 N3 C4 C3 161.9(6) . . . . ? Eu1 N3 C4 C3 39.0(7) . . . . ? N2 C3 C4 N3 -60.3(8) . . . . ? C11 N3 C5 C6 162.9(6) . . . . ? C4 N3 C5 C6 -76.5(7) . . . . ? Eu1 N3 C5 C6 47.4(7) . . . . ? C7 N4 C6 C5 170.5(6) . . . . ? Eu1 N4 C6 C5 37.6(7) . . . . ? N3 C5 C6 N4 -56.9(8) . . . . ? C6 N4 C7 C8 -83.0(7) . . . . ? Eu1 N4 C7 C8 52.3(6) . . . . ? C1 N1 C8 C7 157.7(6) . . . . ? C9 N1 C8 C7 -81.4(7) . . . . ? Eu1 N1 C8 C7 35.9(6) . . . . ? N4 C7 C8 N1 -59.7(7) . . . . ? C1 N1 C9 P1 -75.9(6) . . . . ? C8 N1 C9 P1 163.6(5) . . . . ? Eu1 N1 C9 P1 43.3(5) . . . . ? O4 P1 C9 N1 -144.4(5) . . . . ? O1 P1 C9 N1 -18.4(6) . . . . ? C12 P1 C9 N1 98.7(5) . . . . ? Eu1 P1 C9 N1 -32.1(4) . . . . ? C3 N2 C10 P2 -72.7(6) . . . . ? C2 N2 C10 P2 165.9(4) . . . . ? Eu1 N2 C10 P2 45.0(5) . . . . ? O5 P2 C10 N2 105.9(5) . . . . ? O2 P2 C10 N2 -21.9(5) . . . . ? C19 P2 C10 N2 -136.4(5) . . . . ? Eu1 P2 C10 N2 -32.7(4) . . . . ? C4 N3 C11 P3 167.5(5) . . . . ? C5 N3 C11 P3 -72.4(6) . . . . ? Eu1 N3 C11 P3 46.2(5) . . . . ? O6 P3 C11 N3 102.1(5) . . . . ? O3 P3 C11 N3 -24.7(6) . . . . ? C26 P3 C11 N3 -139.0(5) . . . . ? Eu1 P3 C11 N3 -34.5(4) . . . . ? O4 P1 C12 C13 31.1(6) . . . . ? O1 P1 C12 C13 -96.7(6) . . . . ? C9 P1 C12 C13 148.1(5) . . . . ? Eu1 P1 C12 C13 -127.1(5) . . . . ? P1 C12 C13 C18 74.0(8) . . . . ? P1 C12 C13 C14 -104.1(8) . . . . ? C18 C13 C14 C15 0.6(11) . . . . ? C12 C13 C14 C15 178.8(7) . . . . ? C13 C14 C15 C16 1.2(12) . . . . ? C14 C15 C16 C17 -2.4(13) . . . . ? C15 C16 C17 C18 1.8(13) . . . . ? C14 C13 C18 C17 -1.2(12) . . . . ? C12 C13 C18 C17 -179.3(7) . . . . ? C16 C17 C18 C13 0.0(12) . . . . ? O5 P2 C19 C20 -76.0(6) . . . . ? O2 P2 C19 C20 52.9(6) . . . . ? C10 P2 C19 C20 164.1(5) . . . . ? Eu1 P2 C19 C20 87.5(5) . . . . ? P2 C19 C20 C21 107.2(7) . . . . ? P2 C19 C20 C25 -73.8(8) . . . . ? C25 C20 C21 C22 -0.9(12) . . . . ? C19 C20 C21 C22 178.1(8) . . . . ? C20 C21 C22 C23 3.3(13) . . . . ? C21 C22 C23 C24 -4.0(13) . . . . ? C22 C23 C24 C25 2.5(13) . . . . ? C23 C24 C25 C20 -0.2(13) . . . . ? C21 C20 C25 C24 -0.6(12) . . . . ? C19 C20 C25 C24 -179.6(8) . . . . ? O6 P3 C26 C27 77.7(7) . . . . ? O3 P3 C26 C27 -155.0(6) . . . . ? C11 P3 C26 C27 -42.6(7) . . . . ? Eu1 P3 C26 C27 -119.5(6) . . . . ? P3 C26 C27 C28 113.1(8) . . . . ? P3 C26 C27 C32 -67.7(9) . . . . ? C32 C27 C28 C29 -2.7(12) . . . . ? C26 C27 C28 C29 176.5(8) . . . . ? C27 C28 C29 C30 1.5(14) . . . . ? C28 C29 C30 C31 -0.3(15) . . . . ? C29 C30 C31 C32 0.5(14) . . . . ? C30 C31 C32 C27 -1.7(13) . . . . ? C28 C27 C32 C31 2.9(12) . . . . ? C26 C27 C32 C31 -176.4(7) . . . . ? O4 P1 O1 Eu1 97.2(4) . . . . ? C12 P1 O1 Eu1 -140.2(3) . . . . ? C9 P1 O1 Eu1 -23.2(4) . . . . ? O3 Eu1 O1 P1 -118.4(3) . . . . ? O4 Eu1 O1 P1 -52.4(3) 2_666 . . . ? O2 Eu1 O1 P1 172.6(3) . . . . ? N4 Eu1 O1 P1 2.6(4) . . . . ? N2 Eu1 O1 P1 103.7(3) . . . . ? N3 Eu1 O1 P1 117.8(4) . . . . ? N1 Eu1 O1 P1 35.5(3) . . . . ? P3 Eu1 O1 P1 -145.0(2) . . . . ? P2 Eu1 O1 P1 153.8(3) . . . . ? O5 P2 O2 Eu1 -143.9(3) . . . . ? C19 P2 O2 Eu1 91.9(4) . . . . ? C10 P2 O2 Eu1 -19.3(4) . . . . ? O3 Eu1 O2 P2 171.9(3) . . . . ? O4 Eu1 O2 P2 -118.8(3) 2_666 . . . ? O1 Eu1 O2 P2 -56.4(3) . . . . ? N4 Eu1 O2 P2 106.9(5) . . . . ? N2 Eu1 O2 P2 33.4(3) . . . . ? N3 Eu1 O2 P2 101.5(3) . . . . ? N1 Eu1 O2 P2 -4.4(4) . . . . ? P3 Eu1 O2 P2 152.9(3) . . . . ? P1 Eu1 O2 P2 -53.7(3) . . . . ? O6 P3 O3 Eu1 -141.5(3) . . . . ? C26 P3 O3 Eu1 94.8(4) . . . . ? C11 P3 O3 Eu1 -17.2(4) . . . . ? O4 Eu1 O3 P3 171.5(3) 2_666 . . . ? O2 Eu1 O3 P3 -56.0(3) . . . . ? O1 Eu1 O3 P3 -123.9(3) . . . . ? N4 Eu1 O3 P3 98.4(3) . . . . ? N2 Eu1 O3 P3 -3.4(4) . . . . ? N3 Eu1 O3 P3 32.2(3) . . . . ? N1 Eu1 O3 P3 117.7(4) . . . . ? P1 Eu1 O3 P3 -151.0(2) . . . . ? P2 Eu1 O3 P3 -53.1(3) . . . . ? O1 P1 O4 Eu1 -133.0(9) . . . 2_666 ? C12 P1 O4 Eu1 103.9(10) . . . 2_666 ? C9 P1 O4 Eu1 -13.6(11) . . . 2_666 ? Eu1 P1 O4 Eu1 -93.6(10) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.825 _refine_diff_density_min -1.516 _refine_diff_density_rms 0.187