Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Stefania Tanase-Grecea' _publ_contact_author_address ; Dr. S. Tanase Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University PO Box 9502 2300 RA Leiden The Netherlands ; _publ_contact_author_phone '031 071 5274451' _publ_contact_author_fax '031 024 5274451' _publ_contact_author_email s.grecea@chem.leidenuniv.nl _publ_requested_coeditor_name ? #============================================================================== # 3. AUTHOR LIST loop_ _publ_author_name _publ_author_address S.Tanase ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University PO Box 9502 2300 RA Leiden The Netherlands ; F.Prins ; Leiden Institute of Chemistry Gorlaeus Laboratories Leiden University PO Box 9502 2300 RA Leiden The Netherlands ; J.M.M.Smits ; Molecular Materials Department Institute for Molecules and Materials Radboud University Nijmegen Toernooiveld 1 6525 ED Nijmegen The Netherlands ; 'R.de Gelder' ; Molecular Materials Department Institute for Molecules and Materials Radboud University Nijmegen Toernooiveld 1 6525 ED Nijmegen The Netherlands ; #============================================================================== # 4. TEXT _publ_section_title ; Nanotubular three-dimensional Ln/W complexes with cyanido and carboxylato bridges ; _publ_section_references ; Beurskens, P. T., Beurskens, G., Bosman, W. P., Gelder, R. de, Garcia-Granda, S., Gould, R. O., Israel, R. & Smits, J. M. M. (1996). DIRDIF-96, A computer program system for crystal structure determination by Patterson methods and direct methods applied to difference structure factors. Crystallography Laboratory, University of Nijmegen, The Netherlands. Beurskens, P. T., Beurskens, G., Strumpel, M. & Nordman, C. E. (1987). In Patterson and Pattersons, pp. 356--367. Glusker, J. P., Patterson, B. K. & Rossi, M., Eds. Oxford, England: Clarendon Press. Duisenberg, A.J.M. (1998). Reflections on area detectors, PhD Thesis, Utrecht University, Utrecht, The Netherlands. International Tables for X-ray Crystallography (1974). Vol. IV, Birmingham, England: Kynoch Press. Nonius B.V. (1999). COLLECT, data collection software. Delft, The Netherlands. Sheldrick, G.M. (1996). SADABS. Program for Emperical Absorption Correction. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97, Program for the refinement of crystal structures. University of Gottingen, Germany. Spek, A. L. (2003). PLATON. A Multipurpose Crystallographic Tool. Utrecht University, Utrecht, The Netherlands. ; #============================================================================== data_LEID39 _database_code_depnum_ccdc_archive 'CCDC 606487' _audit_creation_method 'SHELXL, adapted and expanded' _audit_creation_date 2006-09-22 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H40 Eu2 N12 O18 W' _chemical_formula_weight 1248.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8755(5) _cell_length_b 19.129(2) _cell_length_c 19.3765(18) _cell_angle_alpha 90.00 _cell_angle_beta 98.745(5) _cell_angle_gamma 90.00 _cell_volume 3984.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 394 _cell_measurement_theta_min 2.130 _cell_measurement_theta_max 27.500 _exptl_crystal_description 'regular fragment' _exptl_crystal_colour 'translucent light red' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 6.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS multiscan (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 1.000 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'Nonius KappaCCD' _diffrn_measurement_method 'area detector \f and \w scan' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.000 _diffrn_reflns_number 60244 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8929 _reflns_number_gt 8109 _reflns_number_observed 8109 _reflns_threshold_expression >2sigma(I) _reflns_observed_criterion >2sigma(I) _computing_data_collection ; Nonius "Collect" program suite (Nonius, 1999) ; _computing_cell_refinement ? _computing_data_reduction ; Nonius "EvalCCD" program suite (Duisenberg, 1998) ; _computing_structure_solution ; DIRDIF (Beurskens et al., 1996), PATTY (Beurskens et al., 1987) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLATON (Spek, 2003) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0094P)^2^+16.9496P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8929 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0203 _refine_ls_R_factor_obs 0.0203 _refine_ls_wR_factor_ref 0.0450 _refine_ls_wR_factor_all 0.0450 _refine_ls_wR_factor_gt 0.0435 _refine_ls_wR_factor_obs 0.0435 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_goodness_of_fit_all 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.002 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_shift/esd_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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.585796(15) 0.374832(8) 0.857459(8) 0.00877(4) Uani 1 d . . . N10 N 0.7570(3) 0.46261(15) 0.91761(14) 0.0155(6) Uani 1 d . . . C11 C 0.7437(3) 0.50754(19) 0.96865(18) 0.0189(7) Uani 1 d . . . H11 H 0.6752 0.5025 0.9925 0.023 Uiso 1 calc R . . C12 C 0.8279(3) 0.56158(18) 0.98791(18) 0.0182(7) Uani 1 d . . . N13 N 0.9294(3) 0.56861(16) 0.95653(15) 0.0198(6) Uani 1 d . . . C14 C 0.9443(3) 0.52248(18) 0.90660(18) 0.0179(7) Uani 1 d . . . H14 H 1.0149 0.5259 0.8842 0.021 Uiso 1 calc R . . C15 C 0.8589(3) 0.46989(17) 0.88695(16) 0.0140(7) Uani 1 d . . . C16 C 0.8065(4) 0.6137(2) 1.0426(2) 0.0312(10) Uani 1 d . . . H16A H 0.8824 0.6195 1.0754 0.047 Uiso 1 calc R . . H16B H 0.7408 0.5970 1.0671 0.047 Uiso 1 calc R . . H16C H 0.7824 0.6582 1.0205 0.047 Uiso 1 calc R . . C17 C 0.8718(3) 0.41956(17) 0.82882(16) 0.0138(7) Uani 1 d . . . O18 O 0.9728(2) 0.41757(14) 0.80532(13) 0.0203(5) Uani 1 d . . . O19 O 0.7778(2) 0.38261(13) 0.80785(12) 0.0184(5) Uani 1 d . . . N20 N 0.4708(3) 0.25998(14) 0.88759(14) 0.0130(6) Uani 1 d . . . C21 C 0.5188(3) 0.20775(18) 0.92780(18) 0.0173(7) Uani 1 d . . . H21 H 0.6018 0.2109 0.9499 0.021 Uiso 1 calc R . . C22 C 0.4502(4) 0.14815(18) 0.93843(18) 0.0176(7) Uani 1 d . . . N23 N 0.3343(3) 0.14022(15) 0.90586(16) 0.0207(7) Uani 1 d . . . C24 C 0.2854(4) 0.19276(19) 0.86444(19) 0.0207(8) Uani 1 d . . . H24 H 0.2040 0.1884 0.8403 0.025 Uiso 1 calc R . . C25 C 0.3520(3) 0.25293(17) 0.85645(17) 0.0142(7) Uani 1 d . . . C26 C 0.5038(4) 0.0916(2) 0.9869(2) 0.0270(9) Uani 1 d . . . H26A H 0.4531 0.0858 1.0236 0.040 Uiso 1 calc R . . H26B H 0.5879 0.1041 1.0075 0.040 Uiso 1 calc R . . H26C H 0.5052 0.0482 0.9613 0.040 Uiso 1 calc R . . C27 C 0.2978(3) 0.31408(17) 0.81448(17) 0.0150(7) Uani 1 d . . . O28 O 0.1877(2) 0.30902(13) 0.78397(14) 0.0214(6) Uani 1 d . . . O29 O 0.3655(2) 0.36740(12) 0.81430(13) 0.0170(5) Uani 1 d . . . N31 N 0.4926(3) 0.49161(15) 0.87357(14) 0.0166(6) Uani 1 d . . . N32 N 0.5463(3) 0.37634(15) 0.98043(15) 0.0177(6) Uani 1 d . . . N33 N 0.5753(3) 0.28757(15) 0.76332(15) 0.0175(6) Uani 1 d . . . O41 O 0.7459(2) 0.29808(14) 0.92115(13) 0.0215(5) Uani 1 d . . . H41 H 0.7625 0.3113 0.9623 0.026 Uiso 1 calc R . . O42 O 0.5534(3) 0.44764(14) 0.74816(13) 0.0261(6) Uani 1 d . . . C42 C 0.5842(6) 0.4364(3) 0.6802(2) 0.0464(14) Uani 1 d . . . H42A H 0.6430 0.4717 0.6703 0.070 Uiso 1 calc R . . H42B H 0.5094 0.4393 0.6460 0.070 Uiso 1 calc R . . H42C H 0.6211 0.3904 0.6781 0.070 Uiso 1 calc R . . Eu2 Eu 0.048448(16) 0.128653(9) 0.202235(8) 0.01286(4) Uani 1 d . . . O51 O -0.0695(3) 0.14033(15) 0.08483(14) 0.0228(6) Uani 1 d . . . H51A H -0.016(6) 0.149(3) 0.054(3) 0.065(19) Uiso 1 d . . . H51B H -0.138(6) 0.159(3) 0.079(3) 0.060(19) Uiso 1 d . . . O52 O 0.1949(3) 0.03716(15) 0.25250(15) 0.0213(6) Uani 1 d . . . H52A H 0.256(5) 0.054(3) 0.272(2) 0.029(13) Uiso 1 d . . . H52B H 0.190(5) 0.003(3) 0.271(3) 0.052(18) Uiso 1 d . . . O53 O -0.1218(3) 0.20149(17) 0.22418(16) 0.0267(7) Uani 1 d . . . H53A H -0.170(5) 0.183(3) 0.247(3) 0.033(13) Uiso 1 d . . . H53B H -0.157(6) 0.225(3) 0.198(3) 0.06(2) Uiso 1 d . . . O54 O 0.2055(3) 0.11290(17) 0.13096(18) 0.0342(8) Uani 1 d . . . H54A H 0.231(5) 0.140(3) 0.112(3) 0.039(16) Uiso 1 d . . . H54B H 0.232(5) 0.070(3) 0.121(3) 0.038(14) Uiso 1 d . . . O55 O 0.0839(3) 0.24447(15) 0.15376(16) 0.0258(6) Uani 1 d . . . H55A H 0.143(5) 0.269(3) 0.166(3) 0.040(15) Uiso 1 d . . . H55B H 0.033(6) 0.258(3) 0.122(3) 0.06(2) Uiso 1 d . . . O56 O -0.0590(3) 0.02392(16) 0.16877(16) 0.0321(7) Uani 1 d . . . H56A H -0.061(5) -0.018(3) 0.192(3) 0.060(18) Uiso 1 d . . . H56B H -0.096(6) 0.016(3) 0.130(3) 0.062(19) Uiso 1 d . . . W1 W 0.536981(12) 0.162562(6) 0.645454(6) 0.00821(3) Uani 1 d . . . C31 C 0.4838(3) 0.55153(17) 0.86908(16) 0.0122(6) Uani 1 d . . . C32 C 0.5373(3) 0.36366(16) 1.03761(16) 0.0114(6) Uani 1 d . . . C33 C 0.5575(3) 0.24400(17) 0.72194(17) 0.0130(6) Uani 1 d . . . C34 C 0.3539(3) 0.14370(18) 0.67144(18) 0.0172(7) Uani 1 d . . . N34 N 0.2568(3) 0.13494(18) 0.68729(19) 0.0292(8) Uani 1 d . . . C35 C 0.7267(3) 0.12779(18) 0.66301(18) 0.0171(7) Uani 1 d . . . N35 N 0.8281(3) 0.1074(2) 0.67278(19) 0.0319(8) Uani 1 d . . . C36 C 0.5670(3) 0.11413(17) 0.74873(17) 0.0169(7) Uani 1 d . . . N36 N 0.5819(4) 0.08577(18) 0.80165(16) 0.0279(8) Uani 1 d . . . C37 C 0.6481(3) 0.24331(17) 0.60538(16) 0.0135(6) Uani 1 d . . . N37 N 0.7096(3) 0.28497(16) 0.58512(16) 0.0210(7) Uani 1 d . . . C38 C 0.4048(3) 0.23765(19) 0.59173(18) 0.0181(7) Uani 1 d . . . N38 N 0.3330(3) 0.27761(19) 0.56622(19) 0.0320(8) Uani 1 d . . . O61 O 0.2606(3) 0.98164(16) 0.09049(15) 0.0305(7) Uani 1 d . . . H61 H 0.3207 0.9687 0.1193 0.037 Uiso 1 calc R . . C61 C 0.1608(8) 0.9325(5) 0.0892(4) 0.088(2) Uani 1 d . . . H61A H 0.0914 0.9469 0.0546 0.132 Uiso 1 calc R . . H61B H 0.1346 0.9307 0.1348 0.132 Uiso 1 calc R . . H61C H 0.1889 0.8865 0.0772 0.132 Uiso 1 calc R . . O62 O 0.1840(3) 0.46348(18) 0.45086(18) 0.0324(7) Uani 1 d . . . H62A H 0.225(6) 0.439(3) 0.437(3) 0.052(19) Uiso 1 d . . . H62B H 0.215(6) 0.482(4) 0.487(4) 0.07(2) Uiso 1 d . . . O63 O 0.0633(3) 0.09717(18) 0.76436(17) 0.0332(7) Uani 1 d . . . H63A H 0.114(5) 0.103(3) 0.742(3) 0.030(14) Uiso 1 d . . . H63B H 0.000(5) 0.104(3) 0.740(3) 0.040(16) Uiso 1 d . . . O64 O 0.9139(3) 0.18388(17) 0.54670(19) 0.0314(7) Uani 1 d . . . H64A H 0.952(6) 0.157(3) 0.540(3) 0.045(18) Uiso 1 d . . . H64B H 0.880(6) 0.175(4) 0.576(4) 0.07(2) Uiso 1 d . . . O65 O 0.0874(4) 0.3274(2) 0.4852(2) 0.0570(10) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01092(8) 0.00777(7) 0.00768(7) -0.00107(5) 0.00157(5) -0.00073(6) N10 0.0146(16) 0.0163(14) 0.0156(14) -0.0022(11) 0.0023(11) -0.0008(11) C11 0.0160(19) 0.0233(18) 0.0177(17) -0.0058(14) 0.0038(13) 0.0003(14) C12 0.0175(19) 0.0178(17) 0.0178(17) -0.0033(13) -0.0020(13) 0.0011(14) N13 0.0194(17) 0.0188(15) 0.0198(15) -0.0014(12) -0.0011(12) -0.0040(12) C14 0.0159(19) 0.0184(17) 0.0193(17) -0.0007(13) 0.0024(13) -0.0034(14) C15 0.0164(18) 0.0129(15) 0.0123(15) 0.0014(12) 0.0014(12) -0.0003(13) C16 0.029(2) 0.032(2) 0.033(2) -0.0191(18) 0.0031(17) 0.0008(18) C17 0.0157(18) 0.0146(16) 0.0110(14) 0.0024(12) 0.0019(12) 0.0013(13) O18 0.0150(14) 0.0254(14) 0.0219(13) -0.0040(10) 0.0071(10) -0.0030(11) O19 0.0146(13) 0.0233(13) 0.0181(12) -0.0074(10) 0.0056(10) -0.0052(10) N20 0.0152(16) 0.0119(13) 0.0119(13) -0.0017(10) 0.0021(10) -0.0019(11) C21 0.0191(19) 0.0151(16) 0.0173(16) 0.0026(13) 0.0011(13) -0.0002(14) C22 0.024(2) 0.0131(16) 0.0163(16) -0.0002(13) 0.0044(14) -0.0002(14) N23 0.0226(18) 0.0148(14) 0.0240(16) 0.0017(12) 0.0021(13) -0.0051(12) C24 0.019(2) 0.0186(17) 0.0231(18) 0.0023(14) -0.0012(14) -0.0061(14) C25 0.0150(18) 0.0119(15) 0.0150(15) -0.0015(12) -0.0001(13) 0.0000(13) C26 0.032(2) 0.0185(18) 0.030(2) 0.0083(16) 0.0033(17) 0.0025(16) C27 0.0155(19) 0.0148(16) 0.0145(15) -0.0007(12) 0.0017(13) 0.0027(13) O28 0.0121(14) 0.0194(13) 0.0295(14) 0.0040(10) -0.0069(10) -0.0024(10) O29 0.0132(13) 0.0122(11) 0.0240(13) 0.0024(9) -0.0020(10) -0.0008(9) N31 0.0239(17) 0.0135(14) 0.0124(13) 0.0005(11) 0.0026(11) 0.0015(12) N32 0.0264(18) 0.0119(14) 0.0151(14) -0.0004(11) 0.0039(12) 0.0003(12) N33 0.0244(18) 0.0145(14) 0.0149(14) -0.0043(11) 0.0069(12) -0.0035(12) O41 0.0189(14) 0.0232(13) 0.0211(13) 0.0033(10) -0.0015(10) 0.0024(11) O42 0.0428(18) 0.0231(14) 0.0148(12) 0.0054(10) 0.0121(11) 0.0086(12) C42 0.078(4) 0.050(3) 0.016(2) 0.0108(19) 0.022(2) 0.026(3) Eu2 0.01043(9) 0.01337(8) 0.01464(8) 0.00084(6) 0.00147(6) -0.00076(6) O51 0.0220(16) 0.0267(14) 0.0193(13) 0.0016(11) 0.0023(11) 0.0044(12) O52 0.0179(16) 0.0148(13) 0.0298(15) 0.0022(11) -0.0009(11) 0.0005(11) O53 0.0225(17) 0.0329(16) 0.0272(15) 0.0152(13) 0.0116(12) 0.0136(13) O54 0.036(2) 0.0219(16) 0.052(2) 0.0127(14) 0.0284(16) 0.0074(14) O55 0.0216(17) 0.0222(14) 0.0318(16) 0.0066(12) -0.0012(12) -0.0060(12) O56 0.044(2) 0.0242(15) 0.0237(15) 0.0049(12) -0.0090(13) -0.0187(14) W1 0.01024(7) 0.00704(6) 0.00752(6) -0.00108(4) 0.00193(4) -0.00010(5) C31 0.0153(18) 0.0112(15) 0.0105(14) -0.0003(11) 0.0028(12) 0.0003(12) C32 0.0165(18) 0.0073(14) 0.0108(15) -0.0006(11) 0.0030(12) 0.0004(12) C33 0.0126(18) 0.0124(15) 0.0149(15) 0.0008(12) 0.0044(12) -0.0014(12) C34 0.017(2) 0.0156(16) 0.0193(17) 0.0032(13) 0.0037(14) 0.0019(13) N34 0.021(2) 0.0305(19) 0.0375(19) 0.0057(15) 0.0098(15) 0.0000(14) C35 0.0147(19) 0.0181(17) 0.0181(16) 0.0032(13) 0.0014(13) -0.0021(14) N35 0.019(2) 0.038(2) 0.038(2) 0.0118(16) 0.0048(15) 0.0068(15) C36 0.023(2) 0.0133(16) 0.0149(16) -0.0027(13) 0.0038(13) 0.0015(14) N36 0.042(2) 0.0257(17) 0.0154(15) 0.0043(13) 0.0029(14) 0.0056(16) C37 0.0138(18) 0.0138(15) 0.0129(15) -0.0006(12) 0.0020(12) -0.0001(13) N37 0.0217(18) 0.0198(16) 0.0220(15) -0.0003(12) 0.0046(12) -0.0043(13) C38 0.019(2) 0.0201(17) 0.0176(16) 0.0047(13) 0.0091(14) 0.0048(14) N38 0.029(2) 0.035(2) 0.0339(19) 0.0152(16) 0.0134(15) 0.0152(16) O61 0.0326(18) 0.0330(16) 0.0257(15) 0.0037(12) 0.0033(12) 0.0026(13) C61 0.086(6) 0.113(7) 0.068(5) -0.004(4) 0.019(4) -0.010(5) O62 0.0336(19) 0.0348(18) 0.0273(16) -0.0070(13) 0.0001(13) 0.0143(15) O63 0.0214(18) 0.0439(19) 0.0336(17) 0.0150(14) 0.0021(15) -0.0099(14) O64 0.029(2) 0.0265(17) 0.0401(19) 0.0018(14) 0.0108(15) 0.0119(14) O65 0.057(3) 0.068(3) 0.047(2) -0.0069(19) 0.0118(18) -0.006(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 Eu1 O29 2.418(2) . Y Eu1 O19 2.432(2) . Y Eu1 O41 2.461(2) . Y Eu1 N33 2.462(3) . Y Eu1 N32 2.485(3) . Y Eu1 N31 2.492(3) . Y Eu1 O42 2.514(2) . Y Eu1 N20 2.637(3) . Y Eu1 N10 2.643(3) . Y N10 C11 1.334(4) . Y N10 C15 1.342(4) . Y C11 C12 1.393(5) . Y C11 H11 0.9400 . ? C12 N13 1.346(5) . Y C12 C16 1.498(5) . Y N13 C14 1.337(5) . Y C14 C15 1.383(5) . Y C14 H14 0.9400 . ? C15 C17 1.504(4) . Y C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 O18 1.252(4) . Y C17 O19 1.258(4) . Y O18 Eu2 2.439(2) 4_666 Y N20 C21 1.325(4) . Y N20 C25 1.347(4) . Y C21 C22 1.395(5) . Y C21 H21 0.9400 . ? C22 N23 1.330(5) . Y C22 C26 1.492(5) . Y N23 C24 1.344(5) . Y C24 C25 1.381(5) . Y C24 H24 0.9400 . ? C25 C27 1.494(5) . Y C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 O28 1.255(4) . Y C27 O29 1.259(4) . Y O28 Eu2 2.344(2) 4_566 Y N31 C31 1.152(4) . Y N32 C32 1.153(4) . Y N33 C33 1.152(4) . Y O41 H41 0.8300 . ? O42 C42 1.423(4) . Y C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? Eu2 O28 2.344(2) 4_565 Y Eu2 O56 2.360(3) . Y Eu2 O54 2.373(3) . Y Eu2 O53 2.406(3) . Y Eu2 O18 2.439(2) 4_465 Y Eu2 O51 2.446(3) . Y Eu2 O55 2.460(3) . Y Eu2 O52 2.465(3) . Y O51 H51A 0.91(6) . Y O51 H51B 0.82(6) . Y O52 H52A 0.79(5) . Y O52 H52B 0.75(6) . Y O53 H53A 0.82(5) . Y O53 H53B 0.74(6) . Y O54 H54A 0.72(5) . Y O54 H54B 0.91(5) . Y O55 H55A 0.80(6) . Y O55 H55B 0.80(6) . Y O56 H56A 0.91(6) . Y O56 H56B 0.82(6) . Y W1 C33 2.138(3) . Y W1 C35 2.146(4) . Y W1 C32 2.149(3) 4_565 Y W1 C31 2.150(3) 2_646 Y W1 C34 2.158(4) . Y W1 C37 2.176(3) . Y W1 C38 2.181(4) . Y W1 C36 2.184(3) . Y C31 W1 2.150(3) 2_656 Y C32 W1 2.150(3) 4_566 Y C34 N34 1.155(5) . Y C35 N35 1.157(5) . Y C36 N36 1.150(5) . Y C37 N37 1.147(4) . Y C38 N38 1.149(5) . Y O61 C61 1.433(8) . Y O61 H61 0.8300 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C61 H61C 0.9700 . ? O62 H62A 0.72(6) . Y O62 H62B 0.81(7) . Y O63 H63A 0.76(5) . Y O63 H63B 0.79(6) . Y O64 H64A 0.68(6) . Y O64 H64B 0.75(7) . Y 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 O29 Eu1 O19 137.02(8) . . Y O29 Eu1 O41 136.59(8) . . Y O19 Eu1 O41 69.52(9) . . Y O29 Eu1 N33 76.81(9) . . Y O19 Eu1 N33 72.23(9) . . Y O41 Eu1 N33 85.22(10) . . Y O29 Eu1 N32 91.46(10) . . Y O19 Eu1 N32 131.48(9) . . Y O41 Eu1 N32 74.85(9) . . Y N33 Eu1 N32 136.29(9) . . Y O29 Eu1 N31 72.29(9) . . Y O19 Eu1 N31 112.62(9) . . Y O41 Eu1 N31 137.91(9) . . Y N33 Eu1 N31 136.59(10) . . Y N32 Eu1 N31 74.72(9) . . Y O29 Eu1 O42 74.74(9) . . Y O19 Eu1 O42 69.63(9) . . Y O41 Eu1 O42 138.63(9) . . Y N33 Eu1 O42 76.51(9) . . Y N32 Eu1 O42 141.14(9) . . Y N31 Eu1 O42 66.52(9) . . Y O29 Eu1 N20 63.21(8) . . Y O19 Eu1 N20 127.09(8) . . Y O41 Eu1 N20 73.46(9) . . Y N33 Eu1 N20 68.22(9) . . Y N32 Eu1 N20 68.92(9) . . Y N31 Eu1 N20 120.23(9) . . Y O42 Eu1 N20 129.61(9) . . Y O29 Eu1 N10 141.65(8) . . Y O19 Eu1 N10 62.99(8) . . Y O41 Eu1 N10 76.14(9) . . Y N33 Eu1 N10 135.05(9) . . Y N32 Eu1 N10 77.46(9) . . Y N31 Eu1 N10 69.39(10) . . Y O42 Eu1 N10 91.06(9) . . Y N20 Eu1 N10 139.27(9) . . Y C11 N10 C15 116.8(3) . . Y C11 N10 Eu1 126.0(2) . . Y C15 N10 Eu1 116.4(2) . . Y N10 C11 C12 122.4(3) . . Y N10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? N13 C12 C11 120.2(3) . . Y N13 C12 C16 118.6(3) . . Y C11 C12 C16 121.1(3) . . Y C14 N13 C12 117.3(3) . . Y N13 C14 C15 121.9(3) . . Y N13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? N10 C15 C14 121.3(3) . . Y N10 C15 C17 116.3(3) . . Y C14 C15 C17 122.4(3) . . Y C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O18 C17 O19 125.5(3) . . Y O18 C17 C15 118.6(3) . . Y O19 C17 C15 115.9(3) . . Y C17 O18 Eu2 137.1(2) . 4_666 Y C17 O19 Eu1 127.6(2) . . Y C21 N20 C25 117.0(3) . . Y C21 N20 Eu1 126.9(2) . . Y C25 N20 Eu1 116.0(2) . . Y N20 C21 C22 122.1(3) . . Y N20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? N23 C22 C21 120.9(3) . . Y N23 C22 C26 117.9(3) . . Y C21 C22 C26 121.3(3) . . Y C22 N23 C24 117.2(3) . . Y N23 C24 C25 121.6(3) . . Y N23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? N20 C25 C24 121.1(3) . . Y N20 C25 C27 116.0(3) . . Y C24 C25 C27 122.9(3) . . Y C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O28 C27 O29 125.3(3) . . Y O28 C27 C25 117.7(3) . . Y O29 C27 C25 116.9(3) . . Y C27 O28 Eu2 138.7(2) . 4_566 Y C27 O29 Eu1 126.6(2) . . Y C31 N31 Eu1 155.9(3) . . Y C32 N32 Eu1 166.3(3) . . Y C33 N33 Eu1 171.8(3) . . Y Eu1 O41 H41 109.5 . . ? C42 O42 Eu1 132.3(2) . . Y O42 C42 H42A 109.5 . . ? O42 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O42 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O28 Eu2 O56 149.27(10) 4_565 . Y O28 Eu2 O54 90.54(11) 4_565 . Y O56 Eu2 O54 95.88(12) . . Y O28 Eu2 O53 91.24(10) 4_565 . Y O56 Eu2 O53 100.25(12) . . Y O54 Eu2 O53 144.84(11) . . Y O28 Eu2 O18 83.97(9) 4_565 4_465 Y O56 Eu2 O18 72.70(10) . 4_465 Y O54 Eu2 O18 142.45(10) . 4_465 Y O53 Eu2 O18 72.59(9) . 4_465 Y O28 Eu2 O51 140.85(9) 4_565 . Y O56 Eu2 O51 69.77(10) . . Y O54 Eu2 O51 78.01(12) . . Y O53 Eu2 O51 78.63(10) . . Y O18 Eu2 O51 126.90(10) 4_465 . Y O28 Eu2 O55 71.16(10) 4_565 . Y O56 Eu2 O55 139.43(11) . . Y O54 Eu2 O55 73.96(11) . . Y O53 Eu2 O55 73.46(11) . . Y O18 Eu2 O55 137.00(10) 4_465 . Y O51 Eu2 O55 69.70(10) . . Y O28 Eu2 O52 77.40(9) 4_565 . Y O56 Eu2 O52 76.65(11) . . Y O54 Eu2 O52 70.18(11) . . Y O53 Eu2 O52 144.05(10) . . Y O18 Eu2 O52 72.36(9) 4_465 . Y O51 Eu2 O52 130.41(10) . . Y O55 Eu2 O52 131.39(11) . . Y Eu2 O51 H51A 109(4) . . Y Eu2 O51 H51B 121(4) . . Y H51A O51 H51B 119(6) . . Y Eu2 O52 H52A 110(3) . . Y Eu2 O52 H52B 136(4) . . Y H52A O52 H52B 104(5) . . Y Eu2 O53 H53A 114(3) . . Y Eu2 O53 H53B 125(5) . . Y H53A O53 H53B 110(6) . . Y Eu2 O54 H54A 126(4) . . Y Eu2 O54 H54B 121(3) . . Y H54A O54 H54B 113(5) . . Y Eu2 O55 H55A 125(4) . . Y Eu2 O55 H55B 117(4) . . Y H55A O55 H55B 119(6) . . Y Eu2 O56 H56A 131(4) . . Y Eu2 O56 H56B 124(4) . . Y H56A O56 H56B 105(5) . . Y C33 W1 C35 96.87(13) . . Y C33 W1 C32 145.93(12) . 4_565 Y C35 W1 C32 86.45(13) . 4_565 Y C33 W1 C31 143.93(12) . 2_646 Y C35 W1 C31 78.11(13) . 2_646 Y C32 W1 C31 69.99(11) 4_565 2_646 Y C33 W1 C34 87.86(13) . . Y C35 W1 C34 144.18(13) . . Y C32 W1 C34 109.01(13) 4_565 . Y C31 W1 C34 77.47(13) 2_646 . Y C33 W1 C37 74.05(12) . . Y C35 W1 C37 72.76(13) . . Y C32 W1 C37 74.68(12) 4_565 . Y C31 W1 C37 135.03(12) 2_646 . Y C34 W1 C37 141.67(13) . . Y C33 W1 C38 80.95(13) . . Y C35 W1 C38 145.89(13) . . Y C32 W1 C38 77.76(12) 4_565 . Y C31 W1 C38 122.65(13) 2_646 . Y C34 W1 C38 69.93(13) . . Y C37 W1 C38 73.96(13) . . Y C33 W1 C36 71.87(12) . . Y C35 W1 C36 73.57(13) . . Y C32 W1 C36 140.31(12) 4_565 . Y C31 W1 C36 72.49(12) 2_646 . Y C34 W1 C36 74.33(13) . . Y C37 W1 C36 127.90(13) . . Y C38 W1 C36 135.43(13) . . Y N31 C31 W1 176.7(3) . 2_656 Y N32 C32 W1 175.1(3) . 4_566 Y N33 C33 W1 176.4(3) . . Y N34 C34 W1 177.7(3) . . Y N35 C35 W1 178.3(3) . . Y N36 C36 W1 176.9(3) . . Y N37 C37 W1 178.1(3) . . Y N38 C38 W1 176.9(3) . . Y C61 O61 H61 109.5 . . ? O61 C61 H61A 109.5 . . ? O61 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O61 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? H62A O62 H62B 114(6) . . Y H63A O63 H63B 106(5) . . Y H64A O64 H64B 111(7) . . Y 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 O62 H62B O61 0.81(7) 2.11(7) 2.904(4) 166(7) 4_576 O54 H54B O61 0.91(5) 1.83(5) 2.724(4) 170(5) 1_545 O56 H56B O62 0.82(6) 1.98(6) 2.757(4) 159(6) 2_545 O64 H64A N13 0.68(6) 2.13(6) 2.793(5) 166(6) 2_746 O56 H56A O63 0.91(6) 1.74(6) 2.658(4) 179(6) 3_556 O62 H62A N23 0.72(6) 2.07(6) 2.793(5) 173(6) 4_565 O63 H63A N34 0.76(5) 2.10(5) 2.852(5) 171(5) . O41 H41 O64 0.83 2.14 2.833(4) 141.0 4_566 O55 H55A N34 0.80(6) 2.22(6) 2.985(5) 159(5) 4_565 O55 H55B O64 0.80(6) 2.12(7) 2.904(5) 167(6) 4_465 O64 H64B N35 0.75(7) 2.41(7) 3.110(5) 157(7) . O52 H52B N35 0.75(6) 2.40(6) 3.149(5) 178(6) 3_656 O51 H51A O65 0.91(6) 1.93(7) 2.832(5) 175(6) 4_565 O63 H63B N35 0.79(6) 2.11(6) 2.890(5) 171(5) 1_455 O61 H61 N36 0.83 2.02 2.806(4) 159.1 3_666 O51 H51B N37 0.82(6) 1.99(6) 2.797(4) 167(6) 4_465 O53 H53B N37 0.74(6) 2.45(6) 3.031(4) 137(6) 4_465 O54 H54A N38 0.72(5) 2.19(6) 2.901(5) 171(6) 4_565 O52 H52A O29 0.79(5) 2.00(5) 2.745(4) 156(5) 4_565 O53 H53A O19 0.82(5) 1.86(5) 2.636(4) 157(5) 4_465 _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 3.013 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.115 _publ_section_experimental ; Crystal colour: translucent light red, crystal shape: regular fragment. Special experimental condition: measurements were performed at -65 degrees C. Least-squares refinement using calculated weights: w=1/[\s^2^(Fo^2^)+(0.0094P)^2^+16.9496P] where P=(Fo^2^+2Fc^2^)/3 All nonhydrogen atoms were refined with anisotropic temperature factors. Where possible, hydrogen atoms were placed at calculated positions. If not, hydrogen positions were, as many as possible, found from a difference fourier map. All hydrogen atoms were refined isotropically in riding mode. The least squares refinement, and especially the refinement of the lighter atoms, was troublesome because of the considerable difference in scattering power of Eu and W vs. C, N, and O. On Eu1 there is, among others, an OH group (O41) and an OCH~3~ group (O42, C42). There is some rather diffuse electron density in the difference fourier map near O41 which makes it virtually impossible to determine with sufficient certainty whether the OH group is correct or should also be an OCH~3~ group. On the other hand, the thermal displacement parameters of C42 are rather large, which enlarges the uncertainty. There are at least 4 water molecules present in the structure, but PLATON (Spek, 2003) showed a void of 33 \%A^3^ with 8 electrons. It is assumed that 5 water molecules are present in the structure and the fifth water molecule was accounted for by using the SQUEEZE procedure of PLATON. For one of the water molecules, O65, no reliable indications for the location of the hydrogen atoms could be found in the fourier difference map. All calculated physical properties take into account these atoms which are missing from the parameter list. There is one more solvent molecule in the structure and a CH~3~OH molecule (C61, O61) comes closest to the electron density, but the refinement and the thermal displacement parameters are unreliable and this solvent molecule should be mistrusted. Near C61 a peak of 3 e/\%A^3^ is found in the difference fourier map and PLATON reports a void of 32 \%A^3^, but also a net electron count of 0 electrons in this void. It proved to be impossible to refine any disorder model for this electron density without getting physically meaningless results. For all hydrogen atoms that could not be placed on calculated positions the bond distances and angles deviate to some extend from expected values. Rather than using constraints to enforce near-theoretical values we choose to report observed values to enable a critical evaluation of the results. ; #===END # Attachment 'CCDC_606488.cif' data_LEID41 _database_code_depnum_ccdc_archive 'CCDC 606488' _audit_creation_method 'SHELXL, adapted and expanded' _audit_creation_date 2006-09-25 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H44 N12 Nd2 O17 W' _chemical_formula_weight 1257.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9221(5) _cell_length_b 19.266(2) _cell_length_c 19.4537(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.385(5) _cell_angle_gamma 90.00 _cell_volume 4049.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 438 _cell_measurement_theta_min 2.110 _cell_measurement_theta_max 27.500 _exptl_crystal_description 'regular fragment' _exptl_crystal_colour 'translucent light red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 5.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS multiscan (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 1.000 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'Nonius KappaCCD' _diffrn_measurement_method 'area detector \f and \w scan' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.000 _diffrn_reflns_number 55238 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8869 _reflns_number_gt 7705 _reflns_number_observed 7705 _reflns_threshold_expression >2sigma(I) _reflns_observed_criterion >2sigma(I) _computing_data_collection ; Nonius "Collect" program suite (Nonius, 1999) ; _computing_cell_refinement ? _computing_data_reduction ; Nonius "EvalCCD" program suite (Duisenberg, 1998) ; _computing_structure_solution ; DIRDIF (Beurskens et al., 1996), PATTY (Beurskens et al., 1987) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLATON (Spek, 2003) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+20.7661P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8869 _refine_ls_number_parameters 579 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0254 _refine_ls_R_factor_obs 0.0254 _refine_ls_wR_factor_ref 0.0585 _refine_ls_wR_factor_all 0.0585 _refine_ls_wR_factor_gt 0.0555 _refine_ls_wR_factor_obs 0.0555 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_goodness_of_fit_all 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.002 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_shift/esd_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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.58499(2) 0.374858(11) 0.857841(11) 0.01186(5) Uani 1 d . . . N10 N 0.7571(3) 0.46377(19) 0.91766(19) 0.0187(8) Uani 1 d . . . C11 C 0.7443(4) 0.5092(2) 0.9683(2) 0.0232(10) Uani 1 d . . . H11 H 0.6756 0.5049 0.9920 0.028 Uiso 1 calc R . . C12 C 0.8286(4) 0.5624(2) 0.9872(2) 0.0227(10) Uani 1 d . . . N13 N 0.9299(4) 0.5684(2) 0.9560(2) 0.0241(9) Uani 1 d . . . C14 C 0.9458(4) 0.5225(2) 0.9063(2) 0.0210(10) Uani 1 d . . . H14 H 1.0165 0.5256 0.8841 0.025 Uiso 1 calc R . . C15 C 0.8595(4) 0.4704(2) 0.8869(2) 0.0173(9) Uani 1 d . . . C16 C 0.8074(5) 0.6147(3) 1.0411(3) 0.0351(13) Uani 1 d . . . H16A H 0.8711 0.6100 1.0811 0.053 Uiso 1 calc R . . H16B H 0.7269 0.6069 1.0551 0.053 Uiso 1 calc R . . H16C H 0.8104 0.6610 1.0219 0.053 Uiso 1 calc R . . C17 C 0.8723(4) 0.4201(2) 0.8294(2) 0.0180(9) Uani 1 d . . . O18 O 0.9733(3) 0.41804(18) 0.80584(17) 0.0265(8) Uani 1 d . . . O19 O 0.7794(3) 0.38367(17) 0.80802(17) 0.0235(7) Uani 1 d . . . N20 N 0.4680(3) 0.25919(18) 0.88886(18) 0.0163(8) Uani 1 d . . . C21 C 0.5155(4) 0.2078(2) 0.9291(2) 0.0207(10) Uani 1 d . . . H21 H 0.5976 0.2115 0.9513 0.025 Uiso 1 calc R . . C22 C 0.4477(5) 0.1480(2) 0.9398(2) 0.0217(10) Uani 1 d . . . N23 N 0.3331(4) 0.1399(2) 0.9067(2) 0.0270(9) Uani 1 d . . . C24 C 0.2846(5) 0.1920(2) 0.8659(3) 0.0252(11) Uani 1 d . . . H24 H 0.2035 0.1877 0.8423 0.030 Uiso 1 calc R . . C25 C 0.3510(4) 0.2521(2) 0.8575(2) 0.0172(9) Uani 1 d . . . C26 C 0.5012(5) 0.0924(3) 0.9883(3) 0.0315(12) Uani 1 d . . . H26A H 0.4476 0.0846 1.0232 0.047 Uiso 1 calc R . . H26B H 0.5825 0.1065 1.0109 0.047 Uiso 1 calc R . . H26C H 0.5085 0.0498 0.9626 0.047 Uiso 1 calc R . . C27 C 0.2968(4) 0.3122(2) 0.8150(2) 0.0187(9) Uani 1 d . . . O28 O 0.1881(3) 0.30659(17) 0.78336(19) 0.0278(8) Uani 1 d . . . O29 O 0.3637(3) 0.36547(16) 0.81437(17) 0.0218(7) Uani 1 d . . . N31 N 0.4887(4) 0.49207(19) 0.87334(19) 0.0202(8) Uani 1 d . . . N32 N 0.5448(4) 0.37689(19) 0.9820(2) 0.0219(8) Uani 1 d . . . N33 N 0.5766(4) 0.2865(2) 0.7631(2) 0.0238(9) Uani 1 d . . . O41 O 0.7470(3) 0.29703(18) 0.92242(18) 0.0266(8) Uani 1 d . . . C41 C 0.811(2) 0.2476(17) 0.8902(18) 0.50(3) Uiso 1 d D . . H41A H 0.8378 0.2206 0.9325 0.596 Uiso 1 calc R A 1 H41B H 0.8826 0.2772 0.8864 0.596 Uiso 1 calc R A 1 C42A C 0.8447(11) 0.1910(6) 0.8392(6) 0.040(3) Uani 0.50 d PD B 1 H42A H 0.7702 0.1666 0.8193 0.060 Uiso 0.50 calc PR B 1 H42B H 0.9026 0.1584 0.8642 0.060 Uiso 0.50 calc PR B 1 H42C H 0.8823 0.2127 0.8025 0.060 Uiso 0.50 calc PR B 1 C42B C 0.9508(13) 0.2468(9) 0.8755(8) 0.063(4) Uani 0.50 d PD B 2 H42D H 0.9769 0.2938 0.8673 0.094 Uiso 0.50 calc PR B 2 H42E H 0.9569 0.2186 0.8348 0.094 Uiso 0.50 calc PR B 2 H42F H 1.0037 0.2276 0.9153 0.094 Uiso 0.50 calc PR B 2 O43 O 0.5519(4) 0.44814(18) 0.74683(17) 0.0317(8) Uani 1 d . . . C43 C 0.5836(7) 0.4364(4) 0.6793(3) 0.057(2) Uani 1 d . . . H43A H 0.6459 0.4697 0.6702 0.085 Uiso 1 calc R . . H43B H 0.5104 0.4418 0.6449 0.085 Uiso 1 calc R . . H43C H 0.6159 0.3897 0.6767 0.085 Uiso 1 calc R . . Nd2 Nd 0.04936(2) 0.129125(12) 0.201135(13) 0.01707(6) Uani 1 d . . . O51 O -0.0742(4) 0.1403(2) 0.0841(2) 0.0305(10) Uani 1 d . . . H51A H -0.146(6) 0.158(3) 0.078(3) 0.046 Uiso 1 d . . . H51B H -0.044(8) 0.144(4) 0.066(4) 0.046 Uiso 1 d . . . O52 O 0.1996(3) 0.03801(19) 0.2522(2) 0.0263(8) Uani 1 d . . . H52A H 0.251(6) 0.059(3) 0.276(3) 0.040 Uiso 1 d . . . H52B H 0.182(6) 0.005(3) 0.270(3) 0.040 Uiso 1 d . . . O53 O -0.1234(4) 0.2022(2) 0.2245(2) 0.0335(10) Uani 1 d . . . H53A H -0.154(7) 0.186(4) 0.239(4) 0.050 Uiso 1 d . . . H53B H -0.158(6) 0.232(4) 0.201(3) 0.050 Uiso 1 d . . . O54 O 0.2053(4) 0.1141(2) 0.1262(3) 0.0444(12) Uani 1 d . . . H54A H 0.236(7) 0.146(4) 0.110(4) 0.067 Uiso 1 d . . . H54B H 0.228(7) 0.075(4) 0.119(4) 0.067 Uiso 1 d . . . O55 O 0.0835(4) 0.2462(2) 0.1517(2) 0.0306(9) Uani 1 d . . . H55A H 0.134(6) 0.269(4) 0.165(3) 0.046 Uiso 1 d . . . H55B H 0.038(7) 0.248(4) 0.127(4) 0.046 Uiso 1 d . . . O56 O -0.0562(5) 0.0221(2) 0.1684(2) 0.0468(12) Uani 1 d . . . H56A H -0.049(7) -0.016(4) 0.195(4) 0.070 Uiso 1 d . . . H56B H -0.099(7) 0.010(4) 0.129(4) 0.070 Uiso 1 d . . . W1 W 0.538409(15) 0.161783(8) 0.646691(8) 0.01125(4) Uani 1 d . . . C31 C 0.4806(4) 0.5516(2) 0.8680(2) 0.0155(9) Uani 1 d . . . C32 C 0.5367(4) 0.3641(2) 1.0393(2) 0.0157(9) Uani 1 d . . . C33 C 0.5589(4) 0.2428(2) 0.7225(2) 0.0182(9) Uani 1 d . . . C34 C 0.3548(4) 0.1429(2) 0.6720(2) 0.0203(10) Uani 1 d . . . N34 N 0.2577(4) 0.1344(2) 0.6876(3) 0.0341(11) Uani 1 d . . . C35 C 0.7276(4) 0.1273(2) 0.6635(2) 0.0205(10) Uani 1 d . . . N35 N 0.8290(4) 0.1078(3) 0.6733(3) 0.0366(11) Uani 1 d . . . C36 C 0.5688(4) 0.1138(2) 0.7496(2) 0.0188(9) Uani 1 d . . . N36 N 0.5852(5) 0.0860(2) 0.8024(2) 0.0343(11) Uani 1 d . . . C37 C 0.6494(4) 0.2420(2) 0.6060(2) 0.0187(9) Uani 1 d . . . N37 N 0.7100(4) 0.2828(2) 0.5851(2) 0.0249(9) Uani 1 d . . . C38 C 0.4085(5) 0.2372(2) 0.5943(2) 0.0232(10) Uani 1 d . . . N38 N 0.3387(4) 0.2779(3) 0.5690(3) 0.0383(12) Uani 1 d . . . O61 O 0.2590(4) 0.9820(2) 0.0889(2) 0.0382(9) Uani 1 d . . . H61 H 0.3199 0.9657 0.1143 0.057 Uiso 1 calc R . . C61 C 0.1675(15) 0.9404(11) 0.0873(9) 0.198(8) Uani 1 d . . . H61A H 0.1327 0.9593 0.1270 0.238 Uiso 1 calc R . . H61B H 0.2136 0.8994 0.1064 0.238 Uiso 1 calc R . . C62 C 0.0415(9) 0.8999(6) 0.0488(5) 0.092(3) Uani 1 d . . . H62A H 0.0105 0.8692 0.0818 0.138 Uiso 1 calc R . . H62B H 0.0619 0.8730 0.0099 0.138 Uiso 1 calc R . . H62C H -0.0214 0.9339 0.0322 0.138 Uiso 1 calc R . . O63 O 0.9122(4) 0.1829(2) 0.5444(2) 0.0362(10) Uani 1 d . . . H63A H 0.867(6) 0.168(4) 0.579(4) 0.054 Uiso 1 d . . . H63B H 0.950(7) 0.156(4) 0.546(4) 0.054 Uiso 1 d . . . O64 O 0.1838(4) 0.4650(2) 0.4494(2) 0.0408(10) Uani 1 d . . . H64A H 0.239(7) 0.445(4) 0.437(4) 0.061 Uiso 1 d . . . H64B H 0.227(6) 0.489(4) 0.490(4) 0.061 Uiso 1 d . . . O65 O 0.0623(4) 0.0970(2) 0.7632(2) 0.0369(10) Uani 1 d . . . H65A H 0.115(7) 0.107(4) 0.741(4) 0.055 Uiso 1 d . . . H65B H -0.004(7) 0.107(4) 0.735(4) 0.055 Uiso 1 d . . . O66 O 0.0890(8) 0.3261(5) 0.4862(4) 0.127(3) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01493(12) 0.01023(10) 0.01033(11) -0.00136(8) 0.00155(8) -0.00081(8) N10 0.020(2) 0.0190(19) 0.0169(19) -0.0035(15) 0.0026(16) -0.0022(15) C11 0.022(3) 0.026(3) 0.022(3) -0.0093(19) 0.005(2) -0.0026(19) C12 0.023(3) 0.022(2) 0.022(3) -0.0057(18) -0.002(2) 0.0001(18) N13 0.026(2) 0.022(2) 0.023(2) -0.0041(16) -0.0028(17) -0.0034(16) C14 0.022(2) 0.022(2) 0.019(2) 0.0002(18) 0.0006(19) -0.0062(18) C15 0.018(2) 0.016(2) 0.017(2) -0.0015(16) 0.0004(18) -0.0012(17) C16 0.036(3) 0.033(3) 0.036(3) -0.021(2) 0.004(2) -0.004(2) C17 0.017(2) 0.019(2) 0.017(2) 0.0010(17) -0.0003(18) 0.0002(17) O18 0.0184(18) 0.035(2) 0.0267(19) -0.0110(15) 0.0065(14) -0.0066(14) O19 0.0195(17) 0.0299(18) 0.0222(18) -0.0101(14) 0.0061(14) -0.0046(14) N20 0.020(2) 0.0143(18) 0.0139(19) -0.0027(14) -0.0006(15) -0.0015(14) C21 0.021(2) 0.021(2) 0.019(2) 0.0013(18) -0.0015(19) 0.0003(18) C22 0.030(3) 0.016(2) 0.019(2) -0.0008(17) 0.003(2) 0.0015(18) N23 0.032(2) 0.019(2) 0.029(2) 0.0041(16) -0.0002(19) -0.0062(17) C24 0.023(3) 0.022(2) 0.028(3) 0.002(2) -0.005(2) -0.0058(19) C25 0.020(2) 0.018(2) 0.014(2) -0.0005(16) -0.0007(18) -0.0034(17) C26 0.041(3) 0.019(2) 0.033(3) 0.008(2) 0.001(2) 0.002(2) C27 0.020(2) 0.015(2) 0.020(2) -0.0020(17) 0.0021(19) 0.0015(17) O28 0.0182(18) 0.0227(18) 0.039(2) 0.0030(15) -0.0093(15) -0.0048(13) O29 0.0178(17) 0.0169(16) 0.0288(19) 0.0031(13) -0.0027(14) -0.0025(12) N31 0.031(2) 0.0155(19) 0.0147(19) 0.0013(14) 0.0051(16) 0.0024(16) N32 0.037(2) 0.0134(18) 0.016(2) -0.0003(15) 0.0058(17) -0.0007(16) N33 0.035(2) 0.018(2) 0.020(2) -0.0052(16) 0.0081(18) -0.0049(17) O41 0.0224(18) 0.0244(18) 0.032(2) 0.0056(15) 0.0002(15) 0.0030(14) C42A 0.042(7) 0.046(7) 0.031(6) -0.005(5) 0.001(5) 0.003(5) C42B 0.057(9) 0.083(11) 0.050(8) 0.028(8) 0.015(7) 0.036(8) O43 0.051(2) 0.0290(19) 0.0176(18) 0.0061(14) 0.0131(16) 0.0117(17) C43 0.096(6) 0.056(4) 0.022(3) 0.012(3) 0.021(3) 0.031(4) Nd2 0.01404(12) 0.01739(12) 0.01952(13) 0.00130(9) 0.00157(9) -0.00108(9) O51 0.032(3) 0.035(2) 0.023(2) 0.0003(16) 0.0017(17) 0.0091(18) O52 0.0224(19) 0.0195(18) 0.036(2) 0.0022(15) -0.0010(15) -0.0009(14) O53 0.032(2) 0.037(2) 0.034(2) 0.0183(17) 0.0139(17) 0.0145(18) O54 0.045(3) 0.028(2) 0.070(3) 0.014(2) 0.041(2) 0.0075(19) O55 0.026(2) 0.0244(19) 0.040(3) 0.0056(17) -0.0016(17) -0.0073(16) O56 0.068(3) 0.034(2) 0.032(2) 0.0084(18) -0.014(2) -0.024(2) W1 0.01386(9) 0.00972(7) 0.01032(8) -0.00147(6) 0.00228(6) -0.00025(6) C31 0.021(2) 0.016(2) 0.009(2) -0.0017(15) 0.0028(17) 0.0008(17) C32 0.023(2) 0.0093(19) 0.015(2) -0.0016(15) 0.0021(18) -0.0001(16) C33 0.020(2) 0.018(2) 0.017(2) -0.0007(17) 0.0057(18) -0.0007(17) C34 0.024(3) 0.014(2) 0.023(2) 0.0020(17) 0.004(2) 0.0003(17) N34 0.023(2) 0.037(3) 0.043(3) 0.004(2) 0.011(2) -0.0002(19) C35 0.022(3) 0.019(2) 0.021(2) 0.0029(18) 0.0047(19) -0.0014(18) N35 0.025(3) 0.043(3) 0.042(3) 0.013(2) 0.005(2) 0.007(2) C36 0.026(3) 0.016(2) 0.014(2) -0.0037(17) 0.0018(19) 0.0002(18) N36 0.051(3) 0.030(2) 0.022(2) 0.0043(19) 0.006(2) 0.007(2) C37 0.021(2) 0.016(2) 0.018(2) -0.0023(17) 0.0003(19) 0.0005(17) N37 0.024(2) 0.025(2) 0.026(2) 0.0008(17) 0.0050(18) -0.0057(17) C38 0.025(3) 0.024(2) 0.023(3) 0.0064(19) 0.012(2) 0.0044(19) N38 0.035(3) 0.039(3) 0.045(3) 0.021(2) 0.018(2) 0.017(2) O61 0.042(2) 0.038(2) 0.034(2) 0.0020(17) 0.0031(19) 0.0017(18) C61 0.151(15) 0.27(2) 0.155(15) -0.026(15) -0.024(12) -0.015(16) C62 0.096(8) 0.098(8) 0.082(7) -0.005(6) 0.014(6) 0.016(6) O63 0.032(2) 0.031(2) 0.047(3) 0.0013(18) 0.0088(19) 0.0103(16) O64 0.039(2) 0.048(3) 0.033(2) -0.0075(19) 0.0001(19) 0.0188(19) O65 0.029(2) 0.045(2) 0.036(2) 0.0117(18) 0.0004(17) -0.0117(18) O66 0.134(7) 0.146(8) 0.101(6) -0.015(5) 0.021(5) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O29 2.448(3) . Y Nd1 O19 2.465(3) . Y Nd1 N33 2.501(4) . Y Nd1 O41 2.512(3) . Y Nd1 N32 2.518(4) . Y Nd1 N31 2.527(4) . Y Nd1 O43 2.561(3) . Y Nd1 N10 2.680(4) . Y Nd1 N20 2.681(4) . Y N10 C11 1.339(6) . Y N10 C15 1.350(6) . Y C11 C12 1.392(6) . Y C11 H11 0.9400 . ? C12 N13 1.343(6) . Y C12 C16 1.495(6) . Y N13 C14 1.339(6) . Y C14 C15 1.391(6) . Y C14 H14 0.9400 . ? C15 C17 1.500(6) . Y C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 O19 1.254(5) . Y C17 O18 1.256(5) . Y O18 Nd2 2.482(3) 4_666 Y N20 C21 1.320(6) . Y N20 C25 1.341(6) . Y C21 C22 1.402(6) . Y C21 H21 0.9400 . ? C22 N23 1.331(6) . Y C22 C26 1.490(6) . Y N23 C24 1.340(6) . Y C24 C25 1.389(6) . Y C24 H24 0.9400 . ? C25 C27 1.494(6) . Y C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 O28 1.259(6) . Y C27 O29 1.261(5) . Y O28 Nd2 2.384(3) 4_566 Y N31 C31 1.154(5) . Y N32 C32 1.157(6) . Y N33 C33 1.151(6) . Y O41 C41 1.38(2) . Y C41 C42A 1.553(18) . Y C41 C42B 1.594(18) . Y C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C42A H42C 0.9700 . ? C42B H42D 0.9700 . ? C42B H42E 0.9700 . ? C42B H42F 0.9700 . ? O43 C43 1.425(6) . Y C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? Nd2 O28 2.384(3) 4_565 Y Nd2 O56 2.403(4) . Y Nd2 O54 2.416(4) . Y Nd2 O53 2.449(4) . Y Nd2 O51 2.481(4) . Y Nd2 O18 2.482(3) 4_465 Y Nd2 O55 2.502(4) . Y Nd2 O52 2.507(4) . Y O51 H51A 0.85(7) . Y O51 H51B 0.52(7) . Y O52 H52A 0.79(6) . Y O52 H52B 0.76(6) . Y O53 H53A 0.56(7) . Y O53 H53B 0.80(7) . Y O54 H54A 0.80(8) . Y O54 H54B 0.81(8) . Y O55 H55A 0.73(7) . Y O55 H55B 0.64(7) . Y O56 H56A 0.89(8) . Y O56 H56B 0.87(8) . Y W1 C33 2.136(4) . Y W1 C32 2.145(4) 4_565 Y W1 C31 2.148(4) 2_646 Y W1 C35 2.150(5) . Y W1 C34 2.165(5) . Y W1 C38 2.178(5) . Y W1 C37 2.182(5) . Y W1 C36 2.186(4) . Y C31 W1 2.148(4) 2_656 Y C32 W1 2.145(4) 4_566 Y C34 N34 1.156(6) . Y C35 N35 1.159(6) . Y C36 N36 1.151(6) . Y C37 N37 1.141(6) . Y C38 N38 1.153(6) . Y O61 C61 1.278(18) . Y O61 H61 0.8300 . ? C61 C62 1.662(18) . Y C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C62 H62C 0.9700 . ? O63 H63A 0.93(7) . Y O63 H63B 0.67(7) . Y O64 H64A 0.79(7) . Y O64 H64B 0.97(7) . Y O65 H65A 0.80(7) . Y O65 H65B 0.87(7) . Y 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 O29 Nd1 O19 137.13(11) . . Y O29 Nd1 N33 76.52(12) . . Y O19 Nd1 N33 72.44(12) . . Y O29 Nd1 O41 135.78(11) . . Y O19 Nd1 O41 69.73(11) . . Y N33 Nd1 O41 84.82(13) . . Y O29 Nd1 N32 91.77(12) . . Y O19 Nd1 N32 131.07(12) . . Y N33 Nd1 N32 136.46(12) . . Y O41 Nd1 N32 74.82(12) . . Y O29 Nd1 N31 72.56(12) . . Y O19 Nd1 N31 112.49(12) . . Y N33 Nd1 N31 136.47(13) . . Y O41 Nd1 N31 138.47(12) . . Y N32 Nd1 N31 74.80(12) . . Y O29 Nd1 O43 74.86(12) . . Y O19 Nd1 O43 69.76(12) . . Y N33 Nd1 O43 76.60(12) . . Y O41 Nd1 O43 138.87(11) . . Y N32 Nd1 O43 141.03(12) . . Y N31 Nd1 O43 66.31(11) . . Y O29 Nd1 N10 142.34(11) . . Y O19 Nd1 N10 62.42(11) . . Y N33 Nd1 N10 134.68(12) . . Y O41 Nd1 N10 76.48(11) . . Y N32 Nd1 N10 77.46(12) . . Y N31 Nd1 N10 69.80(12) . . Y O43 Nd1 N10 91.00(12) . . Y O29 Nd1 N20 62.44(11) . . Y O19 Nd1 N20 127.73(11) . . Y N33 Nd1 N20 68.45(12) . . Y O41 Nd1 N20 73.46(11) . . Y N32 Nd1 N20 68.99(11) . . Y N31 Nd1 N20 119.70(12) . . Y O43 Nd1 N20 129.40(12) . . Y N10 Nd1 N20 139.52(11) . . Y C11 N10 C15 116.5(4) . . Y C11 N10 Nd1 126.5(3) . . Y C15 N10 Nd1 116.2(3) . . Y N10 C11 C12 122.7(4) . . Y N10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? N13 C12 C11 120.0(4) . . Y N13 C12 C16 118.8(4) . . Y C11 C12 C16 121.2(4) . . Y C14 N13 C12 118.1(4) . . Y N13 C14 C15 121.3(4) . . Y N13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? N10 C15 C14 121.3(4) . . Y N10 C15 C17 116.3(4) . . Y C14 C15 C17 122.4(4) . . Y C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O19 C17 O18 124.9(4) . . Y O19 C17 C15 116.8(4) . . Y O18 C17 C15 118.4(4) . . Y C17 O18 Nd2 136.8(3) . 4_666 Y C17 O19 Nd1 127.5(3) . . Y C21 N20 C25 117.4(4) . . Y C21 N20 Nd1 126.7(3) . . Y C25 N20 Nd1 115.9(3) . . Y N20 C21 C22 122.3(4) . . Y N20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? N23 C22 C21 120.3(4) . . Y N23 C22 C26 118.4(4) . . Y C21 C22 C26 121.3(4) . . Y C22 N23 C24 117.5(4) . . Y N23 C24 C25 121.8(4) . . Y N23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? N20 C25 C24 120.7(4) . . Y N20 C25 C27 116.6(4) . . Y C24 C25 C27 122.7(4) . . Y C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O28 C27 O29 124.9(4) . . Y O28 C27 C25 118.2(4) . . Y O29 C27 C25 116.9(4) . . Y C27 O28 Nd2 138.1(3) . 4_566 Y C27 O29 Nd1 127.0(3) . . Y C31 N31 Nd1 154.8(3) . . Y C32 N32 Nd1 165.7(3) . . Y C33 N33 Nd1 171.1(4) . . Y C41 O41 Nd1 123.4(16) . . Y O41 C41 C42A 162(2) . . Y O41 C41 C42B 130(2) . . Y C42A C41 C42B 63.7(11) . . Y O41 C41 H41A 95.4 . . ? C42A C41 H41A 95.4 . . ? C42B C41 H41A 88.3 . . ? O41 C41 H41B 95.4 . . ? C42A C41 H41B 95.4 . . ? C42B C41 H41B 36.5 . . ? H41A C41 H41B 103.3 . . ? C41 C42A H42A 109.5 . . ? C41 C42A H42B 109.5 . . ? C41 C42A H42C 109.5 . . ? C41 C42B H42D 109.5 . . ? C41 C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41 C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C43 O43 Nd1 131.8(3) . . Y O43 C43 H43A 109.5 . . ? O43 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O43 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O28 Nd2 O56 149.02(13) 4_565 . Y O28 Nd2 O54 91.84(15) 4_565 . Y O56 Nd2 O54 95.18(17) . . Y O28 Nd2 O53 90.49(14) 4_565 . Y O56 Nd2 O53 100.94(17) . . Y O54 Nd2 O53 144.20(14) . . Y O28 Nd2 O51 141.10(14) 4_565 . Y O56 Nd2 O51 69.84(15) . . Y O54 Nd2 O51 78.08(15) . . Y O53 Nd2 O51 77.87(14) . . Y O28 Nd2 O18 84.01(12) 4_565 4_465 Y O56 Nd2 O18 72.45(14) . 4_465 Y O54 Nd2 O18 143.27(13) . 4_465 Y O53 Nd2 O18 72.47(12) . 4_465 Y O51 Nd2 O18 125.64(12) . 4_465 Y O28 Nd2 O55 70.93(13) 4_565 . Y O56 Nd2 O55 139.90(14) . . Y O54 Nd2 O55 73.65(14) . . Y O53 Nd2 O55 73.44(13) . . Y O51 Nd2 O55 70.18(14) . . Y O18 Nd2 O55 137.06(13) 4_465 . Y O28 Nd2 O52 77.43(12) 4_565 . Y O56 Nd2 O52 76.41(14) . . Y O54 Nd2 O52 71.17(14) . . Y O53 Nd2 O52 143.71(13) . . Y O51 Nd2 O52 131.42(13) . . Y O18 Nd2 O52 72.31(12) 4_465 . Y O55 Nd2 O52 131.16(13) . . Y Nd2 O51 H51A 122(4) . . Y Nd2 O51 H51B 108(10) . . Y H51A O51 H51B 122(10) . . Y Nd2 O52 H52A 104(5) . . Y Nd2 O52 H52B 125(5) . . Y H52A O52 H52B 112(6) . . Y Nd2 O53 H53A 107(8) . . Y Nd2 O53 H53B 129(5) . . Y H53A O53 H53B 116(9) . . Y Nd2 O54 H54A 122(6) . . Y Nd2 O54 H54B 118(5) . . Y H54A O54 H54B 120(7) . . Y Nd2 O55 H55A 124(5) . . Y Nd2 O55 H55B 101(7) . . Y H55A O55 H55B 134(9) . . Y Nd2 O56 H56A 123(5) . . Y Nd2 O56 H56B 129(5) . . Y H56A O56 H56B 107(7) . . Y C33 W1 C32 145.79(16) . 4_565 Y C33 W1 C31 144.30(16) . 2_646 Y C32 W1 C31 69.77(15) 4_565 2_646 Y C33 W1 C35 96.86(18) . . Y C32 W1 C35 87.01(17) 4_565 . Y C31 W1 C35 77.70(17) 2_646 . Y C33 W1 C34 88.46(17) . . Y C32 W1 C34 107.80(17) 4_565 . Y C31 W1 C34 77.82(16) 2_646 . Y C35 W1 C34 144.63(17) . . Y C33 W1 C38 80.26(18) . . Y C32 W1 C38 77.68(17) 4_565 . Y C31 W1 C38 123.62(18) 2_646 . Y C35 W1 C38 145.44(17) . . Y C34 W1 C38 69.92(17) . . Y C33 W1 C37 74.03(16) . . Y C32 W1 C37 74.82(16) 4_565 . Y C31 W1 C37 134.41(16) 2_646 . Y C35 W1 C37 72.61(17) . . Y C34 W1 C37 141.61(16) . . Y C38 W1 C37 73.53(17) . . Y C33 W1 C36 71.96(16) . . Y C32 W1 C36 140.56(16) 4_565 . Y C31 W1 C36 72.69(16) 2_646 . Y C35 W1 C36 73.50(17) . . Y C34 W1 C36 75.07(17) . . Y C38 W1 C36 135.43(17) . . Y C37 W1 C36 127.80(17) . . Y N31 C31 W1 177.5(4) . 2_656 Y N32 C32 W1 175.0(4) . 4_566 Y N33 C33 W1 176.4(4) . . Y N34 C34 W1 177.6(4) . . Y N35 C35 W1 178.7(4) . . Y N36 C36 W1 177.2(4) . . Y N37 C37 W1 178.3(4) . . Y N38 C38 W1 177.4(4) . . Y C61 O61 H61 109.5 . . ? O61 C61 C62 153.9(14) . . Y O61 C61 H61A 98.0 . . ? C62 C61 H61A 98.0 . . ? O61 C61 H61B 98.0 . . ? C62 C61 H61B 98.0 . . ? H61A C61 H61B 103.7 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? H63A O63 H63B 95(7) . . Y H64A O64 H64B 100(7) . . Y H65A O65 H65B 101(7) . . Y 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 O51 H51A N37 0.85(7) 1.96(7) 2.786(6) 163(6) 4_465 O51 H51B O66 0.52(7) 2.35(7) 2.865(9) 174(12) 4_565 O52 H52A O29 0.79(6) 1.97(7) 2.739(5) 163(6) 4_565 O52 H52B N35 0.76(6) 2.45(7) 3.195(6) 168(6) 3_656 O53 H53A O19 0.56(7) 2.10(7) 2.647(5) 165(10) 4_465 O53 H53A O18 0.56(7) 2.66(8) 2.915(5) 112(9) 4_465 O53 H53B N37 0.80(7) 2.51(7) 3.052(6) 127(6) 4_465 O54 H54A N38 0.80(8) 2.06(8) 2.856(6) 172(8) 4_565 O54 H54B O61 0.81(8) 1.93(8) 2.734(6) 170(8) 1_545 O55 H55A N34 0.73(7) 2.30(7) 3.001(6) 163(7) 4_565 O55 H55B O51 0.64(7) 2.50(7) 2.865(6) 119(8) . O55 H55B O63 0.64(7) 2.36(7) 2.930(6) 149(8) 4_465 O56 H56A O65 0.89(8) 1.78(8) 2.657(6) 168(7) 3_556 O56 H56B O64 0.87(8) 1.88(8) 2.733(6) 167(7) 2_545 O61 H61 N36 0.83 2.05 2.834(6) 157.4 3_666 O63 H63A N35 0.93(7) 2.26(7) 3.143(6) 157(6) . O63 H63B N13 0.67(7) 2.14(7) 2.801(5) 175(9) 2_746 O64 H64A N23 0.79(7) 2.06(8) 2.797(6) 157(8) 4_565 O64 H64B O61 0.97(7) 1.99(7) 2.904(6) 156(6) 4_576 O65 H65A N34 0.80(7) 2.05(7) 2.856(6) 177(7) . O65 H65B N35 0.87(7) 2.03(7) 2.880(6) 166(7) 1_455 _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.267 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.133 _publ_section_experimental ; Crystal colour: translucent light red, crystal shape: regular fragment. Special remarks: CCD sg139. Special experimental condition: measurements were performed at -65 degrees C. Least-squares refinement using calculated weights: w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+20.7661P] where P=(Fo^2^+2Fc^2^)/3 The least squares refinement, and especially the refinement of the lighter atoms, was troublesome because of the considerable difference in scattering power of Nd and W vs. C, N, and O. On Nd1 there is, among others, an OC~2~H~5~ group (O41, C41, C42) and an OCH~3~ group (O43, C43). Both groups are rather disordered, and only C42 could be split up into two partially occupied positions. This makes it virtually impossible to determine with sufficient certainty the exact chemical nature of these groups. Of course any intermolecular and intramolecular contacts and angles should be mistrusted. There are 4 water molecules present in the structure, but for one of them, O66, no reliable indications for the location of the hydrogen atoms could be found in the fourier difference map. All calculated physical properties take into account these atoms which are missing from the parameter list. There is one more solvent molecule in the structure and a C~2~H~5~OH molecule (C61, C62, O63) comes closest to the electron density, but the refinement and the thermal displacement parameters are unreliable and this solvent molecule should be mistrusted. It proved to be impossible to refine any disorder model for this electron density without getting physically meaningless results. Unfortunately, also for this moiety any intermolecular and intramolecular contacts and angles should be mistrusted. For all hydrogen atoms that could not be placed on calculated positions the bond distances and angles deviate to some extend from expected values. Rather than using constraints to enforce near-theoretical values we choose to report observed values to enable a critical assessment of the results. ; #===END