Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Richard Layfield' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email RAL34@CAM.AC.UK _publ_section_title ; A structural and magnetic study of organolanthanide(III) amides ; loop_ _publ_author_name 'Richard Layfield' 'Alan Bashall' 'M. McPartlin' 'J. Rawson' 'Dominic S. Wright' # Attachment '4.cif' data_mw0207 _database_code_depnum_ccdc_archive 'CCDC 286296' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 N6 Yb2' _chemical_formula_weight 1035.02 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.1200(2) _cell_length_b 13.6353(3) _cell_length_c 23.2134(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4152.76(13) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 35072 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour amber _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 4.515 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.5319 _exptl_absorpt_correction_T_max 0.6133 _exptl_absorpt_process_details psi-scans _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19094 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7202 _reflns_number_gt 6843 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0645P)^2^+9.7843P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(17) _refine_ls_number_reflns 7202 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.851 _refine_ls_shift/su_mean 0.051 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 Yb1 Yb 0.26888(2) 0.22176(3) 0.381815(13) 0.01993(10) Uani 1 1 d . . . Yb2 Yb 0.11203(3) 0.43133(3) 0.329126(14) 0.02125(11) Uani 1 1 d . . . N1 N 0.2195(6) 0.3867(5) 0.4083(3) 0.0251(15) Uani 1 1 d . . . H1 H 0.2745 0.4437 0.3983 0.030 Uiso 1 1 d . . . N2 N 0.2431(5) 0.3186(5) 0.2958(3) 0.0198(14) Uani 1 1 d . . . H2 H 0.3021 0.3552 0.2901 0.024 Uiso 1 1 calc R . . N16 N 0.2120(6) 0.4403(6) 0.5050(3) 0.0319(17) Uani 1 1 d . . . N12 N 0.2052(5) 0.2705(5) 0.4775(3) 0.0215(14) Uani 1 1 d . . . N26 N 0.2533(6) 0.2656(6) 0.1989(3) 0.0302(17) Uani 1 1 d . . . N22 N 0.1030(5) 0.3355(5) 0.2405(3) 0.0239(15) Uani 1 1 d . . . C11 C 0.2103(6) 0.3666(7) 0.4660(3) 0.0225(18) Uani 1 1 d . . . C13 C 0.2072(7) 0.4113(8) 0.5604(4) 0.035(2) Uani 1 1 d . . . C14 C 0.2024(7) 0.3148(9) 0.5762(4) 0.037(3) Uani 1 1 d . . . H14 H 0.1995 0.2969 0.6157 0.045 Uiso 1 1 calc R . . C15 C 0.2019(6) 0.2438(7) 0.5339(3) 0.030(2) Uani 1 1 d . . . C21 C 0.2005(6) 0.3036(6) 0.2432(4) 0.0245(18) Uani 1 1 d . . . C23 C 0.2029(7) 0.2555(7) 0.1484(4) 0.029(2) Uani 1 1 d . . . C24 C 0.1019(8) 0.2851(8) 0.1428(3) 0.034(2) Uani 1 1 d . . . H24 H 0.0666 0.2762 0.1075 0.040 Uiso 1 1 calc R . . C25 C 0.0535(7) 0.3281(7) 0.1898(3) 0.0248(18) Uani 1 1 d . . . C31 C 0.1061(7) 0.1361(6) 0.3386(4) 0.0298(19) Uani 1 1 d . . . H31 H 0.0553 0.1778 0.3227 0.036 Uiso 1 1 calc R . . C32 C 0.1117(7) 0.1042(7) 0.3955(4) 0.032(2) Uani 1 1 d . . . H32 H 0.0649 0.1206 0.4252 0.038 Uiso 1 1 calc R . . C33 C 0.1985(7) 0.0433(7) 0.4019(4) 0.032(2) Uani 1 1 d . . . H33 H 0.2212 0.0133 0.4366 0.039 Uiso 1 1 calc R . . C34 C 0.2446(7) 0.0356(6) 0.3474(4) 0.0284(19) Uani 1 1 d . . . H34 H 0.3026 -0.0033 0.3386 0.034 Uiso 1 1 calc R . . C35 C 0.1911(8) 0.0943(7) 0.3083(4) 0.034(2) Uani 1 1 d . . . H35 H 0.2080 0.1046 0.2690 0.041 Uiso 1 1 calc R . . C41 C 0.4615(8) 0.2284(14) 0.3482(5) 0.065(4) Uani 1 1 d . . . H41 H 0.4751 0.2302 0.3080 0.078 Uiso 1 1 calc R . . C42 C 0.4517(8) 0.3058(10) 0.3832(7) 0.054(3) Uani 1 1 d . . . H42 H 0.4556 0.3726 0.3719 0.065 Uiso 1 1 calc R . . C43 C 0.4347(7) 0.2719(10) 0.4393(5) 0.050(3) Uani 1 1 d . . . H43 H 0.4256 0.3120 0.4724 0.060 Uiso 1 1 calc R . . C44 C 0.4335(7) 0.1720(9) 0.4386(5) 0.043(3) Uani 1 1 d . . . H44 H 0.4243 0.1296 0.4707 0.051 Uiso 1 1 calc R . . C45 C 0.4482(7) 0.1444(9) 0.3818(6) 0.053(3) Uani 1 1 d . . . H45 H 0.4491 0.0789 0.3678 0.063 Uiso 1 1 calc R . . C51 C 0.1569(10) 0.6181(7) 0.3397(4) 0.045(3) Uani 1 1 d . . . H51 H 0.1425 0.6469 0.3761 0.054 Uiso 1 1 calc R . . C52 C 0.0901(9) 0.6127(8) 0.2916(4) 0.043(3) Uani 1 1 d . . . H52 H 0.0224 0.6372 0.2901 0.051 Uiso 1 1 calc R . . C53 C 0.1412(7) 0.5653(7) 0.2473(4) 0.032(2) Uani 1 1 d . . . H53 H 0.1141 0.5510 0.2103 0.038 Uiso 1 1 calc R . . C54 C 0.2383(8) 0.5425(7) 0.2663(4) 0.036(2) Uani 1 1 d . . . H54 H 0.2898 0.5113 0.2441 0.043 Uiso 1 1 calc R . . C55 C 0.2480(7) 0.5728(8) 0.3232(4) 0.041(2) Uani 1 1 d . . . H55 H 0.3065 0.5643 0.3469 0.049 Uiso 1 1 calc R . . C61 C -0.0570(7) 0.5009(7) 0.3788(4) 0.037(2) Uani 1 1 d . . . H61 H -0.0638 0.5698 0.3835 0.044 Uiso 1 1 calc R . . C62 C -0.0880(7) 0.4463(8) 0.3306(4) 0.037(2) Uani 1 1 d . . . H62 H -0.1180 0.4725 0.2967 0.045 Uiso 1 1 calc R . . C63 C -0.0675(6) 0.3464(8) 0.3408(4) 0.032(2) Uani 1 1 d . . . H63 H -0.0815 0.2932 0.3156 0.038 Uiso 1 1 calc R . . C64 C -0.0220(7) 0.3410(7) 0.3957(4) 0.031(2) Uani 1 1 d . . . H64 H -0.0001 0.2826 0.4142 0.037 Uiso 1 1 calc R . . C65 C -0.0145(7) 0.4359(8) 0.4185(4) 0.032(2) Uani 1 1 d . . . H65 H 0.0145 0.4529 0.4547 0.038 Uiso 1 1 calc R . . C131 C 0.2103(12) 0.4944(10) 0.6040(4) 0.064(4) Uani 1 1 d . . . H13A H 0.2766 0.5274 0.6019 0.096 Uiso 1 1 calc R . . H13B H 0.2002 0.4680 0.6428 0.096 Uiso 1 1 calc R . . H13C H 0.1560 0.5416 0.5953 0.096 Uiso 1 1 calc R . . C151 C 0.2020(8) 0.1363(7) 0.5475(4) 0.035(2) Uani 1 1 d . . . H15A H 0.1565 0.1019 0.5209 0.052 Uiso 1 1 calc R . . H15B H 0.1783 0.1264 0.5871 0.052 Uiso 1 1 calc R . . H15C H 0.2713 0.1104 0.5435 0.052 Uiso 1 1 calc R . . C231 C 0.2601(9) 0.2132(10) 0.0992(4) 0.050(3) Uani 1 1 d . . . H23A H 0.3320 0.2322 0.1020 0.076 Uiso 1 1 calc R . . H23B H 0.2315 0.2379 0.0630 0.076 Uiso 1 1 calc R . . H23C H 0.2546 0.1415 0.1002 0.076 Uiso 1 1 calc R . . C251 C -0.0530(8) 0.3662(8) 0.1856(4) 0.039(2) Uani 1 1 d . . . H25A H -0.0939 0.3394 0.2173 0.058 Uiso 1 1 calc R . . H25B H -0.0828 0.3462 0.1487 0.058 Uiso 1 1 calc R . . H25C H -0.0523 0.4379 0.1881 0.058 Uiso 1 1 calc R . . C1S C 0.5093(9) 0.4389(12) 0.2302(7) 0.068(4) Uani 1 1 d . . . H1S H 0.4569 0.4860 0.2242 0.081 Uiso 1 1 calc R . . C2S C 0.5109(14) 0.3578(17) 0.1980(7) 0.086(6) Uani 1 1 d . . . H2S H 0.4571 0.3475 0.1713 0.103 Uiso 1 1 calc R . . C3S C 0.5859(16) 0.2892(14) 0.2016(7) 0.082(5) Uani 1 1 d . . . H3S H 0.5863 0.2331 0.1774 0.098 Uiso 1 1 calc R . . C4S C 0.6587(14) 0.3037(12) 0.2406(7) 0.081(5) Uani 1 1 d . . . H4S H 0.7125 0.2573 0.2434 0.097 Uiso 1 1 calc R . . C5S C 0.6592(10) 0.3835(13) 0.2769(6) 0.066(4) Uani 1 1 d . . . H5S H 0.7114 0.3896 0.3050 0.079 Uiso 1 1 calc R . . C6S C 0.5832(12) 0.4564(9) 0.2729(5) 0.060(4) Uani 1 1 d . . . C7S C 0.579(2) 0.5462(14) 0.3083(11) 0.166(14) Uani 1 1 d . . . H7S1 H 0.5473 0.5310 0.3455 0.248 Uiso 1 1 calc R . . H7S2 H 0.5380 0.5959 0.2883 0.248 Uiso 1 1 calc R . . H7S3 H 0.6479 0.5712 0.3144 0.248 Uiso 1 1 calc R . . C1T C 0.6267(14) 0.2039(12) 0.0402(5) 0.073(4) Uani 1 1 d . . . H1T H 0.6805 0.1606 0.0503 0.088 Uiso 1 1 calc R . . C2T C 0.639(3) 0.3017(19) 0.0515(9) 0.150(12) Uani 1 1 d . . . H2T H 0.6993 0.3224 0.0701 0.180 Uiso 1 1 calc R . . C3T C 0.569(3) 0.3704(17) 0.0377(10) 0.133(10) Uani 1 1 d . . . H3T H 0.5762 0.4386 0.0449 0.160 Uiso 1 1 calc R . . C4T C 0.482(2) 0.326(2) 0.0103(9) 0.129(10) Uani 1 1 d . . . H4T H 0.4301 0.3710 -0.0003 0.155 Uiso 1 1 calc R . . C5T C 0.4597(15) 0.2353(19) -0.0026(7) 0.090(6) Uani 1 1 d . . . H5T H 0.3986 0.2155 -0.0212 0.108 Uiso 1 1 calc R . . C6T C 0.5428(13) 0.1659(13) 0.0154(6) 0.076(5) Uani 1 1 d . . . C7T C 0.5232(17) 0.0692(17) 0.0033(8) 0.119(8) Uani 1 1 d . . . H7T1 H 0.4876 0.0643 -0.0337 0.178 Uiso 1 1 calc R . . H7T2 H 0.4805 0.0412 0.0338 0.178 Uiso 1 1 calc R . . H7T3 H 0.5876 0.0329 0.0012 0.178 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01429(17) 0.02522(19) 0.02028(16) 0.00073(14) -0.00092(13) -0.00053(13) Yb2 0.01745(17) 0.02443(19) 0.02186(17) 0.00188(14) 0.00061(14) 0.00081(14) N1 0.028(4) 0.031(4) 0.016(3) 0.008(3) 0.000(3) -0.001(3) N2 0.013(3) 0.026(4) 0.020(3) 0.000(3) 0.002(3) 0.003(3) N16 0.033(4) 0.037(5) 0.026(3) -0.003(3) -0.004(3) 0.002(4) N12 0.014(3) 0.027(4) 0.023(3) 0.003(3) 0.005(3) 0.000(3) N26 0.026(4) 0.043(5) 0.021(3) -0.003(3) 0.004(3) 0.000(3) N22 0.020(4) 0.024(4) 0.028(3) 0.000(3) -0.003(3) 0.001(3) C11 0.011(4) 0.038(5) 0.018(4) -0.003(4) 0.000(3) -0.001(3) C13 0.031(5) 0.049(7) 0.025(4) -0.010(4) -0.002(4) 0.005(4) C14 0.020(5) 0.073(8) 0.019(4) 0.008(4) 0.005(3) 0.008(4) C15 0.017(4) 0.051(6) 0.022(4) -0.003(4) -0.001(3) 0.003(4) C21 0.019(4) 0.026(5) 0.028(4) 0.001(3) 0.001(3) -0.004(3) C23 0.030(5) 0.034(5) 0.024(4) 0.000(4) 0.005(4) -0.004(4) C24 0.035(5) 0.044(6) 0.023(4) 0.008(4) -0.009(4) -0.009(5) C25 0.028(5) 0.023(5) 0.024(4) 0.004(3) -0.007(3) -0.001(4) C31 0.033(5) 0.020(4) 0.037(5) 0.001(4) -0.011(4) -0.002(4) C32 0.025(4) 0.037(5) 0.034(5) -0.003(4) 0.005(4) 0.002(4) C33 0.020(4) 0.032(5) 0.045(5) 0.002(4) -0.007(4) -0.002(3) C34 0.020(4) 0.025(4) 0.041(5) -0.010(4) 0.000(4) 0.004(3) C35 0.036(5) 0.038(6) 0.030(4) -0.009(4) -0.003(4) -0.008(4) C41 0.019(5) 0.139(14) 0.037(5) 0.029(8) -0.001(4) -0.002(7) C42 0.021(5) 0.057(8) 0.083(9) 0.013(7) -0.003(6) -0.007(5) C43 0.019(5) 0.072(9) 0.058(7) -0.032(7) -0.003(5) -0.008(5) C44 0.014(4) 0.064(8) 0.050(6) 0.025(6) -0.008(4) -0.002(5) C45 0.015(4) 0.055(7) 0.089(9) -0.038(7) -0.007(6) 0.015(4) C51 0.070(7) 0.025(5) 0.039(5) 0.001(4) 0.007(5) -0.007(5) C52 0.050(7) 0.034(6) 0.044(6) 0.010(4) 0.002(5) 0.008(5) C53 0.033(5) 0.033(5) 0.029(4) 0.006(4) 0.003(4) -0.007(4) C54 0.037(5) 0.032(5) 0.039(5) 0.011(4) 0.006(4) -0.004(4) C55 0.033(5) 0.047(6) 0.044(5) 0.020(5) -0.003(4) -0.016(5) C61 0.025(5) 0.035(6) 0.051(5) 0.005(5) 0.018(5) 0.008(4) C62 0.019(4) 0.057(7) 0.035(5) 0.006(5) -0.004(4) 0.005(4) C63 0.013(4) 0.043(6) 0.040(5) 0.003(4) 0.002(4) -0.003(4) C64 0.027(5) 0.026(5) 0.039(5) 0.008(4) 0.007(4) 0.001(4) C65 0.026(5) 0.043(6) 0.027(4) 0.001(4) 0.005(3) 0.008(4) C131 0.092(10) 0.071(9) 0.030(5) -0.025(6) -0.006(6) 0.007(8) C151 0.039(5) 0.028(5) 0.037(5) 0.005(4) 0.006(4) -0.003(4) C231 0.045(6) 0.077(8) 0.029(4) -0.015(5) -0.001(4) 0.005(6) C251 0.034(5) 0.040(6) 0.041(5) 0.001(4) -0.022(4) 0.007(4) C1S 0.037(6) 0.072(10) 0.095(10) 0.040(9) 0.017(7) 0.020(7) C2S 0.073(11) 0.115(16) 0.070(9) 0.018(10) -0.021(8) -0.067(12) C3S 0.100(14) 0.070(11) 0.075(9) 0.000(9) 0.012(10) -0.026(11) C4S 0.092(12) 0.074(11) 0.075(10) 0.028(9) 0.047(9) 0.034(9) C5S 0.034(6) 0.113(13) 0.050(7) 0.033(8) 0.001(5) -0.020(7) C6S 0.080(10) 0.045(7) 0.056(7) 0.001(5) 0.036(7) -0.021(6) C7S 0.25(3) 0.072(13) 0.18(2) -0.052(13) 0.16(2) -0.078(17) C1T 0.096(12) 0.076(11) 0.047(6) 0.011(7) 0.005(7) -0.020(9) C2T 0.26(4) 0.102(19) 0.091(13) 0.001(13) 0.069(18) -0.03(2) C3T 0.24(3) 0.051(13) 0.111(16) 0.010(12) 0.023(19) -0.007(17) C4T 0.20(3) 0.12(2) 0.067(11) 0.005(13) 0.071(15) -0.02(2) C5T 0.079(11) 0.135(17) 0.055(8) 0.026(11) 0.041(8) 0.030(12) C6T 0.075(10) 0.097(12) 0.057(7) -0.001(8) 0.012(7) -0.046(9) C7T 0.128(17) 0.127(17) 0.101(13) -0.033(13) 0.044(12) -0.073(15) _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 Yb1 N2 2.417(6) . ? Yb1 N1 2.420(8) . ? Yb1 N12 2.466(6) . ? Yb1 C45 2.579(9) . ? Yb1 C44 2.620(9) . ? Yb1 C31 2.634(9) . ? Yb1 C32 2.631(10) . ? Yb1 C33 2.645(9) . ? Yb1 C41 2.647(10) . ? Yb1 C35 2.641(9) . ? Yb1 C42 2.659(10) . ? Yb1 C43 2.643(10) . ? Yb2 N1 2.395(7) . ? Yb2 N2 2.433(6) . ? Yb2 N22 2.441(7) . ? Yb2 C62 2.633(9) . ? Yb2 C52 2.637(10) . ? Yb2 C51 2.625(10) . ? Yb2 C63 2.639(9) . ? Yb2 C55 2.631(9) . ? Yb2 C65 2.658(8) . ? Yb2 C54 2.677(9) . ? Yb2 C61 2.674(9) . ? Yb2 C53 2.663(9) . ? N1 C11 1.373(10) . ? N2 C21 1.360(10) . ? N16 C13 1.346(12) . ? N16 C11 1.353(11) . ? N12 C11 1.339(12) . ? N12 C15 1.358(10) . ? N26 C23 1.352(11) . ? N26 C21 1.344(11) . ? N22 C25 1.348(10) . ? N22 C21 1.353(11) . ? C13 C14 1.367(15) . ? C13 C131 1.520(14) . ? C14 C15 1.379(14) . ? C15 C151 1.499(14) . ? C23 C24 1.392(14) . ? C23 C231 1.483(13) . ? C24 C25 1.392(13) . ? C25 C251 1.494(13) . ? C31 C32 1.393(13) . ? C31 C35 1.437(14) . ? C32 C33 1.417(14) . ? C33 C34 1.407(13) . ? C34 C35 1.399(14) . ? C41 C42 1.34(2) . ? C41 C45 1.396(19) . ? C42 C43 1.400(18) . ? C43 C44 1.363(16) . ? C44 C45 1.387(17) . ? C51 C55 1.398(16) . ? C51 C52 1.421(16) . ? C52 C53 1.386(14) . ? C53 C54 1.384(14) . ? C54 C55 1.391(14) . ? C61 C65 1.397(13) . ? C61 C62 1.403(14) . ? C62 C63 1.409(15) . ? C63 C64 1.408(13) . ? C64 C65 1.402(14) . ? C1S C2S 1.34(2) . ? C1S C6S 1.41(2) . ? C2S C3S 1.36(3) . ? C3S C4S 1.33(2) . ? C4S C5S 1.38(2) . ? C5S C6S 1.41(2) . ? C6S C7S 1.47(2) . ? C1T C6T 1.34(2) . ? C1T C2T 1.37(3) . ? C2T C3T 1.35(4) . ? C3T C4T 1.45(4) . ? C4T C5T 1.30(3) . ? C5T C6T 1.50(2) . ? C6T C7T 1.37(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Yb1 N1 70.4(2) . . ? N2 Yb1 N16 123.3(2) . . ? N1 Yb1 N16 55.2(2) . . ? N2 Yb1 C45 110.5(4) . . ? N1 Yb1 C45 128.7(3) . . ? N12 Yb1 C45 114.9(3) . . ? N2 Yb1 C44 132.3(3) . . ? N1 Yb1 C44 109.5(3) . . ? N12 Yb1 C44 84.0(3) . . ? C45 Yb1 C44 30.9(4) . . ? N2 Yb1 C31 79.3(2) . . ? N1 Yb1 C31 107.0(3) . . ? N12 Yb1 C31 100.8(3) . . ? C45 Yb1 C31 123.9(3) . . ? C44 Yb1 C31 138.2(3) . . ? N2 Yb1 C32 108.9(3) . . ? N1 Yb1 C32 109.0(3) . . ? N12 Yb1 C32 77.9(3) . . ? C45 Yb1 C32 117.8(4) . . ? C44 Yb1 C32 115.3(3) . . ? C31 Yb1 C32 30.7(3) . . ? N2 Yb1 C33 126.9(3) . . ? N1 Yb1 C33 135.8(3) . . ? N12 Yb1 C33 88.3(3) . . ? C45 Yb1 C33 86.7(4) . . ? C44 Yb1 C33 87.7(3) . . ? C31 Yb1 C33 51.4(3) . . ? C32 Yb1 C33 31.2(3) . . ? N2 Yb1 C41 82.6(3) . . ? N1 Yb1 C41 107.4(5) . . ? N12 Yb1 C41 125.5(3) . . ? C45 Yb1 C41 30.9(4) . . ? C44 Yb1 C41 50.9(3) . . ? C31 Yb1 C41 132.7(4) . . ? C32 Yb1 C41 143.6(5) . . ? C33 Yb1 C41 114.6(5) . . ? N2 Yb1 C35 76.8(3) . . ? N1 Yb1 C35 132.3(3) . . ? N12 Yb1 C35 129.0(3) . . ? C45 Yb1 C35 94.7(3) . . ? C44 Yb1 C35 118.2(4) . . ? C31 Yb1 C35 31.6(3) . . ? C32 Yb1 C35 51.3(3) . . ? C33 Yb1 C35 51.2(3) . . ? C41 Yb1 C35 101.6(4) . . ? N2 Yb1 C42 84.3(3) . . ? N1 Yb1 C42 80.7(4) . . ? N12 Yb1 C42 100.3(4) . . ? C45 Yb1 C42 49.7(4) . . ? C44 Yb1 C42 50.3(4) . . ? C31 Yb1 C42 158.1(4) . . ? C32 Yb1 C42 165.5(3) . . ? C33 Yb1 C42 135.2(3) . . ? C41 Yb1 C42 29.2(4) . . ? C35 Yb1 C42 129.8(4) . . ? N2 Yb1 C43 113.0(4) . . ? N1 Yb1 C43 81.5(3) . . ? N12 Yb1 C43 75.8(3) . . ? C45 Yb1 C43 49.8(4) . . ? C44 Yb1 C43 30.0(4) . . ? C31 Yb1 C43 167.2(4) . . ? C32 Yb1 C43 137.9(4) . . ? C33 Yb1 C43 115.9(4) . . ? C41 Yb1 C43 49.7(4) . . ? C35 Yb1 C43 144.6(3) . . ? C42 Yb1 C43 30.6(4) . . ? N1 Yb2 N2 70.5(2) . . ? N1 Yb2 N22 122.7(2) . . ? N2 Yb2 N22 55.1(2) . . ? N1 Yb2 C62 126.6(3) . . ? N2 Yb2 C62 139.3(3) . . ? N22 Yb2 C62 90.2(3) . . ? N1 Yb2 C52 123.8(3) . . ? N2 Yb2 C52 124.4(3) . . ? N22 Yb2 C52 102.6(3) . . ? C62 Yb2 C52 79.8(3) . . ? N1 Yb2 C51 92.4(3) . . ? N2 Yb2 C51 118.9(3) . . ? N22 Yb2 C51 127.5(3) . . ? C62 Yb2 C51 98.5(4) . . ? C52 Yb2 C51 31.3(4) . . ? N1 Yb2 C63 109.6(3) . . ? N2 Yb2 C63 112.7(3) . . ? N22 Yb2 C63 78.9(3) . . ? C62 Yb2 C63 31.0(3) . . ? C52 Yb2 C63 110.4(3) . . ? C51 Yb2 C63 128.1(4) . . ? N1 Yb2 C55 80.0(3) . . ? N2 Yb2 C55 88.1(3) . . ? N22 Yb2 C55 112.4(3) . . ? C62 Yb2 C55 128.3(3) . . ? C52 Yb2 C55 50.9(3) . . ? C51 Yb2 C55 30.9(4) . . ? C63 Yb2 C55 158.8(3) . . ? N1 Yb2 C65 77.0(3) . . ? N2 Yb2 C65 134.8(3) . . ? N22 Yb2 C65 129.8(3) . . ? C62 Yb2 C65 50.6(3) . . ? C52 Yb2 C65 99.7(3) . . ? C51 Yb2 C65 92.6(3) . . ? C63 Yb2 C65 51.1(3) . . ? C55 Yb2 C65 116.6(3) . . ? N1 Yb2 C54 101.4(3) . . ? N2 Yb2 C54 75.4(3) . . ? N22 Yb2 C54 82.8(3) . . ? C62 Yb2 C54 125.5(3) . . ? C52 Yb2 C54 50.0(3) . . ? C51 Yb2 C54 50.4(3) . . ? C63 Yb2 C54 149.0(3) . . ? C55 Yb2 C54 30.4(3) . . ? C65 Yb2 C54 143.0(3) . . ? N1 Yb2 C61 104.4(3) . . ? N2 Yb2 C61 161.4(3) . . ? N22 Yb2 C61 120.9(3) . . ? C62 Yb2 C61 30.6(3) . . ? C52 Yb2 C61 73.7(3) . . ? C51 Yb2 C61 78.6(3) . . ? C63 Yb2 C61 51.0(3) . . ? C55 Yb2 C61 109.0(3) . . ? C65 Yb2 C61 30.4(3) . . ? C54 Yb2 C61 123.2(3) . . ? N1 Yb2 C53 129.6(3) . . ? N2 Yb2 C53 96.1(3) . . ? N22 Yb2 C53 76.9(3) . . ? C62 Yb2 C53 95.7(3) . . ? C52 Yb2 C53 30.3(3) . . ? C51 Yb2 C53 50.9(3) . . ? C63 Yb2 C53 120.2(3) . . ? C55 Yb2 C53 50.4(3) . . ? C65 Yb2 C53 129.1(3) . . ? C54 Yb2 C53 30.0(3) . . ? C61 Yb2 C53 100.5(3) . . ? C11 N1 Yb2 138.4(6) . . ? C11 N1 Yb1 94.9(5) . . ? Yb2 N1 Yb1 101.5(3) . . ? C21 N2 Yb1 135.9(6) . . ? C21 N2 Yb2 95.1(5) . . ? Yb1 N2 Yb2 100.5(2) . . ? C13 N16 C11 114.9(8) . . ? C11 N12 C15 117.2(7) . . ? C11 N12 Yb1 93.8(4) . . ? C15 N12 Yb1 143.7(6) . . ? C23 N26 C21 116.8(7) . . ? C25 N22 C21 118.2(7) . . ? C25 N22 Yb2 143.1(6) . . ? C21 N22 Yb2 95.0(5) . . ? N12 C11 N12 126.3(7) . . ? N12 C11 N1 113.3(7) . . ? N16 C11 N1 120.3(8) . . ? N12 C11 Yb1 58.6(4) . . ? N16 C11 Yb1 163.4(6) . . ? N1 C11 Yb1 56.8(4) . . ? N16 C13 C14 122.7(9) . . ? N16 C13 C131 114.5(10) . . ? C14 C13 C131 122.8(9) . . ? C13 C14 C15 119.0(8) . . ? N12 C15 C14 119.8(9) . . ? N12 C15 C151 117.8(8) . . ? C14 C15 C151 122.4(8) . . ? N26 C21 N26 125.1(8) . . ? N26 C21 N2 122.3(7) . . ? N22 C21 N2 112.5(7) . . ? N26 C21 Yb2 165.3(6) . . ? N22 C21 Yb2 57.2(4) . . ? N2 C21 Yb2 56.9(4) . . ? N26 C23 C24 121.1(8) . . ? N26 C23 C231 117.4(8) . . ? C24 C23 C231 121.5(8) . . ? C25 C24 C23 118.9(8) . . ? N22 C25 C24 119.7(8) . . ? N22 C25 C251 118.8(8) . . ? C24 C25 C251 121.5(8) . . ? C32 C31 C35 107.4(8) . . ? C32 C31 Yb1 74.6(5) . . ? C35 C31 Yb1 74.5(5) . . ? C31 C32 C33 109.0(8) . . ? C31 C32 Yb1 74.7(5) . . ? C33 C32 Yb1 75.0(5) . . ? C34 C33 C32 107.1(8) . . ? C34 C33 Yb1 76.1(5) . . ? C32 C33 Yb1 73.9(5) . . ? C33 C34 C35 109.0(8) . . ? C33 C34 Yb1 73.3(5) . . ? C35 C34 Yb1 73.2(5) . . ? C34 C35 C31 107.4(8) . . ? C34 C35 Yb1 76.3(5) . . ? C31 C35 Yb1 73.9(5) . . ? C42 C41 C45 107.3(10) . . ? C42 C41 Yb1 75.9(7) . . ? C45 C41 Yb1 71.8(6) . . ? C41 C42 C43 108.6(12) . . ? C41 C42 Yb1 74.9(7) . . ? C43 C42 Yb1 74.1(6) . . ? C44 C43 C42 108.7(11) . . ? C44 C43 Yb1 74.1(6) . . ? C42 C43 Yb1 75.3(6) . . ? C43 C44 C45 106.3(10) . . ? C43 C44 Yb1 75.9(6) . . ? C45 C44 Yb1 72.9(6) . . ? C41 C45 C44 109.0(11) . . ? C41 C45 Yb1 77.2(6) . . ? C44 C45 Yb1 76.2(5) . . ? C55 C51 C52 106.8(9) . . ? C55 C51 Yb2 74.8(6) . . ? C52 C51 Yb2 74.8(6) . . ? C53 C52 C51 108.0(10) . . ? C53 C52 Yb2 75.8(6) . . ? C51 C52 Yb2 73.8(6) . . ? C54 C53 C52 108.3(9) . . ? C54 C53 Yb2 75.6(5) . . ? C52 C53 Yb2 73.8(5) . . ? C53 C54 C55 108.7(9) . . ? C53 C54 Yb2 74.4(5) . . ? C55 C54 Yb2 73.0(5) . . ? C51 C55 C54 108.2(9) . . ? C51 C55 Yb2 74.3(6) . . ? C54 C55 Yb2 76.6(6) . . ? C65 C61 C62 107.8(9) . . ? C65 C61 Yb2 74.2(5) . . ? C62 C61 Yb2 73.1(5) . . ? C63 C62 C61 108.9(9) . . ? C63 C62 Yb2 74.7(5) . . ? C61 C62 Yb2 76.3(5) . . ? C62 C63 C64 106.5(9) . . ? C62 C63 Yb2 74.3(5) . . ? C64 C63 Yb2 74.8(5) . . ? C65 C64 C63 108.9(8) . . ? C65 C64 Yb2 75.2(5) . . ? C63 C64 Yb2 74.3(5) . . ? C61 C65 C64 107.9(8) . . ? C61 C65 Yb2 75.4(5) . . ? C64 C65 Yb2 74.2(5) . . ? C2S C1S C6S 121.6(14) . . ? C1S C2S C3S 123.1(15) . . ? C4S C3S C2S 117.4(16) . . ? C3S C4S C5S 122.5(16) . . ? C6S C5S C4S 121.0(13) . . ? C5S C6S C1S 114.4(12) . . ? C5S C6S C7S 125(2) . . ? C1S C6S C7S 120.3(19) . . ? C6T C1T C2T 123(2) . . ? C3T C2T C1T 124(3) . . ? C2T C3T C4T 110(2) . . ? C5T C4T C3T 133(3) . . ? C4T C5T C6T 112(2) . . ? C1T C6T C7T 128(2) . . ? C1T C6T C5T 118.0(17) . . ? C7T C6T C5T 114.3(19) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.576 _refine_diff_density_min -1.604 _refine_diff_density_rms 0.187 # Attachment '2.cif' data_m _database_code_depnum_ccdc_archive 'CCDC 286297' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 Gd2 N6' _chemical_formula_weight 819.17 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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0619(2) _cell_length_b 16.6647(3) _cell_length_c 16.0128(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.5960(10) _cell_angle_gamma 90.00 _cell_volume 3050.65(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 16763 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 4.341 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4351 _exptl_absorpt_correction_T_max 0.6707 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26648 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6972 _reflns_number_gt 6083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0256P)^2^+3.8200P] 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 6972 _refine_ls_number_parameters 384 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Gd1 Gd 0.129260(12) 0.233546(9) 0.441220(10) 0.01837(5) Uani 1 1 d . . . Gd2 Gd 0.275342(13) 0.342442(10) 0.294859(10) 0.01947(5) Uani 1 1 d . . . N1 N 0.0765(2) 0.32767(17) 0.30896(17) 0.0208(6) Uani 1 1 d . . . H1N H 0.0354 0.3222 0.2400 0.029(10) Uiso 1 1 d . . . N2 N 0.2590(2) 0.20478(17) 0.35409(18) 0.0225(6) Uani 1 1 d . . . H2N H 0.2030 0.1631 0.3227 0.040(11) Uiso 1 1 d . . . N12 N 0.0141(2) 0.36081(16) 0.42505(17) 0.0208(6) Uani 1 1 d . . . N16 N -0.0793(2) 0.42032(17) 0.28357(17) 0.0246(6) Uani 1 1 d . . . N22 N 0.4424(2) 0.25328(17) 0.37745(19) 0.0247(6) Uani 1 1 d . . . N26 N 0.4131(2) 0.11055(17) 0.38188(18) 0.0250(6) Uani 1 1 d . . . C11 C 0.0018(3) 0.37230(19) 0.3383(2) 0.0188(6) Uani 1 1 d . . . C13 C -0.0615(3) 0.3989(2) 0.4582(2) 0.0216(7) Uani 1 1 d . . . C14 C -0.1466(3) 0.4487(2) 0.4052(2) 0.0253(7) Uani 1 1 d . . . H14 H -0.1994 0.4762 0.4283 0.030 Uiso 1 1 calc R . . C15 C -0.1533(3) 0.4577(2) 0.3173(2) 0.0271(7) Uani 1 1 d . . . C21 C 0.3741(3) 0.1871(2) 0.3724(2) 0.0219(7) Uani 1 1 d . . . C23 C 0.5580(3) 0.2405(2) 0.3921(3) 0.0318(8) Uani 1 1 d . . . C24 C 0.6021(3) 0.1641(2) 0.4012(3) 0.0337(9) Uani 1 1 d . . . H24 H 0.6829 0.1552 0.4106 0.040 Uiso 1 1 calc R . . C25 C 0.5274(3) 0.1001(2) 0.3965(2) 0.0282(8) Uani 1 1 d . . . C31 C 0.2518(4) 0.3149(3) 0.5888(2) 0.0412(10) Uani 1 1 d . . . C32 C 0.1950(4) 0.2519(3) 0.6191(3) 0.0461(11) Uani 1 1 d . . . C33 C 0.2490(4) 0.1804(3) 0.6063(3) 0.0481(11) Uani 1 1 d . . . H33 H 0.2303 0.1283 0.6219 0.058 Uiso 1 1 calc R . . C34 C 0.3343(3) 0.1978(3) 0.5672(3) 0.0407(10) Uani 1 1 d . . . C35 C 0.3364(3) 0.2810(3) 0.5566(2) 0.0357(9) Uani 1 1 d . . . C41 C -0.0138(4) 0.1328(3) 0.3228(3) 0.0542(14) Uani 1 1 d . . . C42 C 0.0478(4) 0.0848(3) 0.3934(4) 0.0554(14) Uani 1 1 d . . . C43 C 0.0111(4) 0.1039(3) 0.4643(3) 0.0522(12) Uani 1 1 d . . . C44 C -0.0729(3) 0.1633(3) 0.4394(3) 0.0419(10) Uani 1 1 d . . . C45 C -0.0889(3) 0.1819(3) 0.3512(3) 0.0443(11) Uani 1 1 d . . . C51 C 0.2214(3) 0.4936(2) 0.3305(3) 0.0355(9) Uani 1 1 d . . . C52 C 0.2779(4) 0.4578(2) 0.4131(3) 0.0388(9) Uani 1 1 d . . . C53 C 0.3965(4) 0.4473(2) 0.4204(3) 0.0445(10) Uani 1 1 d . . . C54 C 0.4124(4) 0.4755(2) 0.3429(3) 0.0461(11) Uani 1 1 d . . . C55 C 0.3043(4) 0.5047(2) 0.2874(3) 0.0432(10) Uani 1 1 d . . . C61 C 0.3385(7) 0.3585(4) 0.1506(4) 0.0758(18) Uani 1 1 d . . . C62 C 0.2265(8) 0.3735(4) 0.1252(3) 0.084(2) Uani 1 1 d . . . H62 H 0.1936 0.4251 0.1082 0.101 Uiso 1 1 calc R . . C63 C 0.1611(4) 0.3055(6) 0.1261(3) 0.094(3) Uani 1 1 d . . . C64 C 0.2521(7) 0.2431(3) 0.1549(3) 0.0700(19) Uani 1 1 d . . . H64 H 0.2414 0.1876 0.1633 0.084 Uiso 1 1 calc R . . C65 C 0.3552(4) 0.2828(4) 0.1669(3) 0.0581(14) Uani 1 1 d . . . C131 C -0.0526(3) 0.3827(2) 0.5517(2) 0.0323(8) Uani 1 1 d . . . H13A H -0.0609 0.3249 0.5598 0.048 Uiso 1 1 calc R . . H13B H -0.1149 0.4116 0.5662 0.048 Uiso 1 1 calc R . . H13C H 0.0237 0.4008 0.5906 0.048 Uiso 1 1 calc R . . C151 C -0.2440(4) 0.5105(3) 0.2565(3) 0.0496(12) Uani 1 1 d . . . H15A H -0.2058 0.5568 0.2396 0.074 Uiso 1 1 calc R . . H15B H -0.2985 0.5291 0.2865 0.074 Uiso 1 1 calc R . . H15C H -0.2869 0.4801 0.2037 0.074 Uiso 1 1 calc R . . C231 C 0.6327(3) 0.3133(3) 0.3978(4) 0.0570(14) Uani 1 1 d . . . H23A H 0.6040 0.3439 0.3428 0.086 Uiso 1 1 calc R . . H23B H 0.7138 0.2968 0.4071 0.086 Uiso 1 1 calc R . . H23C H 0.6293 0.3469 0.4471 0.086 Uiso 1 1 calc R . . C251 C 0.5718(3) 0.0153(2) 0.4089(3) 0.0376(9) Uani 1 1 d . . . H25A H 0.5438 -0.0115 0.4528 0.056 Uiso 1 1 calc R . . H25B H 0.6576 0.0155 0.4292 0.056 Uiso 1 1 calc R . . H25C H 0.5431 -0.0136 0.3528 0.056 Uiso 1 1 calc R . . H31 H 0.2272 0.3795 0.5828 0.078(17) Uiso 1 1 d . . . H32 H 0.1286 0.2578 0.6625 0.072(16) Uiso 1 1 d . . . H34 H 0.4052 0.1643 0.5577 0.089(19) Uiso 1 1 d . . . H35 H 0.3978 0.3179 0.5377 0.068(15) Uiso 1 1 d . . . H41 H -0.0046 0.1316 0.2600 0.074(16) Uiso 1 1 d . . . H42 H 0.0981 0.0339 0.3819 0.093(19) Uiso 1 1 d . . . H43 H 0.0283 0.0710 0.5200 0.070(15) Uiso 1 1 d . . . H44 H -0.1213 0.1841 0.4776 0.058(14) Uiso 1 1 d . . . H45 H -0.1480 0.2289 0.3174 0.11(2) Uiso 1 1 d . . . H51 H 0.1351 0.5080 0.3225 0.082(17) Uiso 1 1 d . . . H52 H 0.2396 0.4339 0.4572 0.067(15) Uiso 1 1 d . . . H53 H 0.4546 0.4205 0.4800 0.080(17) Uiso 1 1 d . . . H54 H 0.4821 0.4784 0.3200 0.081(17) Uiso 1 1 d . . . H55 H 0.2930 0.5284 0.2173 0.088(18) Uiso 1 1 d . . . H61 H 0.4147 0.4056 0.1379 0.36(8) Uiso 1 1 d . . . H63 H 0.0683 0.3083 0.1007 0.17(3) Uiso 1 1 d . . . H65 H 0.4502 0.2496 0.2000 0.13(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01711(8) 0.01519(9) 0.02270(9) 0.00201(6) 0.00618(6) 0.00029(6) Gd2 0.02103(9) 0.01701(9) 0.02201(9) 0.00031(6) 0.00918(7) 0.00096(6) N1 0.0207(13) 0.0207(15) 0.0216(13) -0.0007(11) 0.0074(11) 0.0039(11) N2 0.0170(12) 0.0192(14) 0.0313(15) -0.0060(12) 0.0076(11) -0.0008(11) N12 0.0223(13) 0.0188(14) 0.0224(13) -0.0008(11) 0.0090(11) -0.0009(11) N16 0.0246(14) 0.0236(16) 0.0233(13) -0.0004(12) 0.0046(11) 0.0064(12) N22 0.0187(13) 0.0236(15) 0.0324(15) -0.0007(12) 0.0087(12) -0.0019(11) N26 0.0250(14) 0.0218(15) 0.0301(14) -0.0012(12) 0.0115(12) 0.0041(11) C11 0.0208(14) 0.0137(16) 0.0224(15) -0.0013(13) 0.0078(12) -0.0022(12) C13 0.0238(15) 0.0183(17) 0.0256(16) -0.0050(13) 0.0121(13) -0.0043(13) C14 0.0256(16) 0.0191(17) 0.0342(18) -0.0051(14) 0.0136(14) 0.0033(13) C15 0.0260(16) 0.0208(18) 0.0320(17) -0.0044(15) 0.0057(14) 0.0042(14) C21 0.0224(15) 0.0226(18) 0.0216(15) -0.0016(13) 0.0085(13) 0.0027(13) C23 0.0201(16) 0.035(2) 0.038(2) 0.0032(17) 0.0051(15) -0.0017(15) C24 0.0206(17) 0.041(2) 0.039(2) 0.0035(17) 0.0095(15) 0.0068(15) C25 0.0289(17) 0.034(2) 0.0231(16) -0.0009(15) 0.0102(14) 0.0083(15) C31 0.047(2) 0.039(2) 0.0257(18) -0.0089(17) -0.0045(17) 0.0080(19) C32 0.040(2) 0.071(3) 0.0239(19) 0.008(2) 0.0058(17) 0.007(2) C33 0.047(2) 0.047(3) 0.040(2) 0.021(2) -0.0011(19) -0.001(2) C34 0.0314(19) 0.043(3) 0.039(2) 0.0095(19) -0.0022(17) 0.0106(18) C35 0.0287(18) 0.043(2) 0.0274(18) -0.0010(17) -0.0025(15) -0.0077(17) C41 0.057(3) 0.067(3) 0.048(3) -0.031(2) 0.029(2) -0.049(3) C42 0.039(2) 0.025(2) 0.107(4) -0.019(3) 0.029(3) -0.0100(18) C43 0.046(2) 0.040(3) 0.065(3) 0.019(2) 0.010(2) -0.018(2) C44 0.029(2) 0.046(3) 0.056(3) -0.013(2) 0.0216(19) -0.0173(18) C45 0.0243(18) 0.035(2) 0.063(3) -0.002(2) -0.0009(19) -0.0114(17) C51 0.042(2) 0.0174(19) 0.051(2) -0.0057(17) 0.0207(19) 0.0005(16) C52 0.057(2) 0.024(2) 0.039(2) -0.0136(17) 0.0204(19) -0.0114(18) C53 0.052(2) 0.024(2) 0.047(2) -0.0074(18) 0.000(2) -0.0096(18) C54 0.044(2) 0.024(2) 0.076(3) -0.004(2) 0.027(2) -0.0098(18) C55 0.059(3) 0.019(2) 0.058(3) 0.0061(18) 0.028(2) -0.0025(18) C61 0.117(5) 0.079(5) 0.054(3) -0.012(3) 0.058(4) -0.016(4) C62 0.140(6) 0.083(5) 0.024(2) 0.014(3) 0.019(3) 0.049(5) C63 0.027(2) 0.230(9) 0.026(2) -0.046(4) 0.0101(19) -0.015(4) C64 0.148(6) 0.038(3) 0.032(2) -0.017(2) 0.040(3) -0.027(3) C65 0.051(3) 0.085(4) 0.041(2) -0.024(3) 0.020(2) 0.013(3) C131 0.041(2) 0.030(2) 0.0338(19) 0.0033(16) 0.0234(17) 0.0028(17) C151 0.053(3) 0.052(3) 0.037(2) -0.003(2) 0.0046(19) 0.032(2) C231 0.0238(19) 0.047(3) 0.097(4) 0.014(3) 0.014(2) -0.0067(19) C251 0.041(2) 0.033(2) 0.041(2) 0.0003(17) 0.0171(18) 0.0167(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N2 2.453(3) . ? Gd1 N12 2.503(3) . ? Gd1 N1 2.548(3) . ? Gd1 C44 2.696(4) . ? Gd1 C43 2.678(4) . ? Gd1 C42 2.686(4) . ? Gd1 C45 2.706(4) . ? Gd1 C32 2.720(4) . ? Gd1 C41 2.703(4) . ? Gd1 C33 2.724(4) . ? Gd1 C31 2.717(4) . ? Gd1 C35 2.709(3) . ? Gd2 N1 2.492(3) . ? Gd2 N2 2.514(3) . ? Gd2 N22 2.513(3) . ? Gd2 C62 2.640(5) . ? Gd2 C61 2.667(5) . ? Gd2 C65 2.715(4) . ? Gd2 C52 2.692(4) . ? Gd2 C63 2.684(4) . ? Gd2 C53 2.712(4) . ? Gd2 C55 2.735(4) . ? Gd2 C51 2.708(4) . ? Gd2 C54 2.725(4) . ? N1 C11 1.362(4) . ? N2 C21 1.357(4) . ? N12 C13 1.350(4) . ? N12 C11 1.363(4) . ? N16 C11 1.349(4) . ? N16 C15 1.336(4) . ? N22 C21 1.363(4) . ? N22 C23 1.356(4) . ? N26 C25 1.335(4) . ? N26 C21 1.351(4) . ? C13 C14 1.380(5) . ? C13 C131 1.492(5) . ? C14 C15 1.391(5) . ? C15 C151 1.495(5) . ? C23 C24 1.369(5) . ? C23 C231 1.497(5) . ? C24 C25 1.382(5) . ? C25 C251 1.502(5) . ? C31 C35 1.400(6) . ? C31 C32 1.421(7) . ? C32 C33 1.403(7) . ? C33 C34 1.394(6) . ? C34 C35 1.399(6) . ? C41 C42 1.390(7) . ? C41 C45 1.399(7) . ? C42 C43 1.381(7) . ? C43 C44 1.381(6) . ? C44 C45 1.399(6) . ? C51 C55 1.397(6) . ? C51 C52 1.413(6) . ? C52 C53 1.409(6) . ? C53 C54 1.396(6) . ? C54 C55 1.410(6) . ? C61 C62 1.305(9) . ? C61 C65 1.291(8) . ? C62 C63 1.382(10) . ? C63 C64 1.475(10) . ? C64 C65 1.366(8) . ? 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 N2 Gd1 N12 122.71(9) . . ? N2 Gd1 N1 71.53(9) . . ? N12 Gd1 N1 53.78(8) . . ? N2 Gd1 C44 130.37(11) . . ? N12 Gd1 C44 84.06(11) . . ? N1 Gd1 C44 105.85(12) . . ? N2 Gd1 C43 112.64(14) . . ? N12 Gd1 C43 113.30(13) . . ? N1 Gd1 C43 127.48(11) . . ? C44 Gd1 C43 29.78(14) . . ? N2 Gd1 C42 84.21(13) . . ? N12 Gd1 C42 127.72(11) . . ? N1 Gd1 C42 111.06(15) . . ? C44 Gd1 C42 49.39(13) . . ? C43 Gd1 C42 29.84(15) . . ? N2 Gd1 C45 108.84(12) . . ? N12 Gd1 C45 78.53(11) . . ? N1 Gd1 C45 79.06(11) . . ? C44 Gd1 C45 30.01(14) . . ? C43 Gd1 C45 49.24(13) . . ? C42 Gd1 C45 49.42(14) . . ? N2 Gd1 C32 126.28(11) . . ? N12 Gd1 C32 88.87(12) . . ? N1 Gd1 C32 135.54(13) . . ? C44 Gd1 C32 91.18(14) . . ? C43 Gd1 C32 86.35(15) . . ? C42 Gd1 C32 111.12(17) . . ? C45 Gd1 C32 120.21(14) . . ? N2 Gd1 C41 81.95(11) . . ? N12 Gd1 C41 104.17(15) . . ? N1 Gd1 C41 82.25(13) . . ? C44 Gd1 C41 49.46(13) . . ? C43 Gd1 C41 49.21(15) . . ? C42 Gd1 C41 29.89(16) . . ? C45 Gd1 C41 29.99(14) . . ? C32 Gd1 C41 135.41(15) . . ? N2 Gd1 C33 104.56(12) . . ? N12 Gd1 C33 118.73(12) . . ? N1 Gd1 C33 157.10(12) . . ? C44 Gd1 C33 93.84(14) . . ? C43 Gd1 C33 75.21(14) . . ? C42 Gd1 C33 90.54(17) . . ? C45 Gd1 C33 122.56(14) . . ? C32 Gd1 C33 29.86(14) . . ? C41 Gd1 C33 120.07(16) . . ? N2 Gd1 C31 108.87(11) . . ? N12 Gd1 C31 78.31(10) . . ? N1 Gd1 C31 109.78(11) . . ? C44 Gd1 C31 117.72(14) . . ? C43 Gd1 C31 116.64(15) . . ? C42 Gd1 C31 139.17(16) . . ? C45 Gd1 C31 142.11(14) . . ? C32 Gd1 C31 30.31(14) . . ? C41 Gd1 C31 165.65(14) . . ? C33 Gd1 C31 49.08(14) . . ? N2 Gd1 C35 80.11(11) . . ? N12 Gd1 C35 100.59(11) . . ? N1 Gd1 C35 108.59(11) . . ? C44 Gd1 C35 140.19(13) . . ? C43 Gd1 C35 123.86(13) . . ? C42 Gd1 C35 129.65(14) . . ? C45 Gd1 C35 170.03(14) . . ? C32 Gd1 C35 49.85(13) . . ? C41 Gd1 C35 154.63(16) . . ? C33 Gd1 C35 49.07(13) . . ? C31 Gd1 C35 29.91(13) . . ? N1 Gd2 N2 71.47(9) . . ? N1 Gd2 N22 121.81(9) . . ? N2 Gd2 N22 53.71(8) . . ? N1 Gd2 C62 101.9(2) . . ? N2 Gd2 C62 123.25(18) . . ? N22 Gd2 C62 122.40(17) . . ? N1 Gd2 C61 129.61(18) . . ? N2 Gd2 C61 119.79(17) . . ? N22 Gd2 C61 96.47(19) . . ? C62 Gd2 C61 28.5(2) . . ? N1 Gd2 C65 127.99(13) . . ? N2 Gd2 C65 92.30(16) . . ? N22 Gd2 C65 76.30(14) . . ? C62 Gd2 C65 46.52(18) . . ? C61 Gd2 C65 27.73(18) . . ? N1 Gd2 C52 78.59(11) . . ? N2 Gd2 C52 111.77(11) . . ? N22 Gd2 C52 102.98(11) . . ? C62 Gd2 C52 122.17(17) . . ? C61 Gd2 C52 126.55(17) . . ? C65 Gd2 C52 149.89(16) . . ? N1 Gd2 C63 82.46(12) . . ? N2 Gd2 C63 95.4(2) . . ? N22 Gd2 C63 117.5(2) . . ? C62 Gd2 C63 30.1(2) . . ? C61 Gd2 C63 49.27(19) . . ? C65 Gd2 C63 49.31(15) . . ? C52 Gd2 C63 139.4(2) . . ? N1 Gd2 C53 107.65(12) . . ? N2 Gd2 C53 113.37(11) . . ? N22 Gd2 C53 80.72(11) . . ? C62 Gd2 C53 121.8(2) . . ? C61 Gd2 C53 110.01(18) . . ? C65 Gd2 C53 123.93(16) . . ? C52 Gd2 C53 30.22(13) . . ? C63 Gd2 C53 151.2(2) . . ? N1 Gd2 C55 103.98(11) . . ? N2 Gd2 C55 161.00(11) . . ? N22 Gd2 C55 121.04(11) . . ? C62 Gd2 C55 75.57(19) . . ? C61 Gd2 C55 77.71(18) . . ? C65 Gd2 C55 104.35(18) . . ? C52 Gd2 C55 49.57(13) . . ? C63 Gd2 C55 102.4(3) . . ? C53 Gd2 C55 49.40(13) . . ? N1 Gd2 C51 76.69(10) . . ? N2 Gd2 C51 135.76(11) . . ? N22 Gd2 C51 130.19(11) . . ? C62 Gd2 C51 92.56(17) . . ? C61 Gd2 C51 104.09(19) . . ? C65 Gd2 C51 131.79(17) . . ? C52 Gd2 C51 30.34(12) . . ? C63 Gd2 C51 110.2(2) . . ? C53 Gd2 C51 49.71(13) . . ? C55 Gd2 C51 29.74(12) . . ? N1 Gd2 C54 124.72(11) . . ? N2 Gd2 C54 138.53(12) . . ? N22 Gd2 C54 91.15(11) . . ? C62 Gd2 C54 92.7(2) . . ? C61 Gd2 C54 81.24(18) . . ? C65 Gd2 C54 100.45(17) . . ? C52 Gd2 C54 49.52(13) . . ? C63 Gd2 C54 122.7(2) . . ? C53 Gd2 C54 29.76(14) . . ? C55 Gd2 C54 29.94(13) . . ? C51 Gd2 C54 49.36(12) . . ? C11 N1 Gd2 137.6(2) . . ? C11 N1 Gd1 93.82(19) . . ? Gd2 N1 Gd1 98.26(9) . . ? C21 N2 Gd1 135.6(2) . . ? C21 N2 Gd2 94.7(2) . . ? Gd1 N2 Gd2 100.20(10) . . ? C13 N12 C11 117.8(3) . . ? C13 N12 Gd1 141.2(2) . . ? C11 N12 Gd1 95.79(19) . . ? C11 N16 C15 117.0(3) . . ? C21 N22 C23 116.8(3) . . ? C21 N22 Gd2 94.55(19) . . ? C23 N22 Gd2 142.4(2) . . ? C25 N26 C21 116.5(3) . . ? N16 C11 N12 124.5(3) . . ? N16 C11 N1 121.5(3) . . ? N12 C11 N1 114.0(3) . . ? N12 C13 C14 120.3(3) . . ? N12 C13 C131 117.9(3) . . ? C14 C13 C131 121.8(3) . . ? C15 C14 C13 118.6(3) . . ? N16 C15 C14 121.8(3) . . ? N16 C15 C151 117.1(3) . . ? C14 C15 C151 121.1(3) . . ? N2 C21 N22 113.2(3) . . ? N2 C21 N26 121.7(3) . . ? N22 C21 N26 125.1(3) . . ? N22 C23 C24 120.5(3) . . ? N22 C23 C231 116.7(3) . . ? C24 C23 C231 122.8(3) . . ? C23 C24 C25 119.2(3) . . ? N26 C25 C24 121.8(3) . . ? N26 C25 C251 116.8(3) . . ? C24 C25 C251 121.4(3) . . ? C35 C31 C32 108.3(4) . . ? C35 C31 Gd1 74.7(2) . . ? C32 C31 Gd1 75.0(2) . . ? C31 C32 C33 106.3(4) . . ? C31 C32 Gd1 74.7(2) . . ? C33 C32 Gd1 75.3(2) . . ? C34 C33 C32 109.4(4) . . ? C34 C33 Gd1 74.7(2) . . ? C32 C33 Gd1 74.9(2) . . ? C33 C34 C35 107.7(4) . . ? C33 C34 Gd1 75.6(2) . . ? C35 C34 Gd1 74.9(2) . . ? C31 C35 C34 108.1(4) . . ? C31 C35 Gd1 75.4(2) . . ? C34 C35 Gd1 75.2(2) . . ? C42 C41 C45 107.8(4) . . ? C42 C41 Gd1 74.4(2) . . ? C45 C41 Gd1 75.1(2) . . ? C43 C42 C41 107.9(4) . . ? C43 C42 Gd1 74.8(3) . . ? C41 C42 Gd1 75.7(2) . . ? C42 C43 C44 109.0(4) . . ? C42 C43 Gd1 75.4(2) . . ? C44 C43 Gd1 75.8(2) . . ? C45 C44 C43 107.6(4) . . ? C45 C44 Gd1 75.4(2) . . ? C43 C44 Gd1 74.4(2) . . ? C44 C45 C41 107.6(4) . . ? C44 C45 Gd1 74.6(2) . . ? C41 C45 Gd1 74.9(2) . . ? C55 C51 C52 108.2(4) . . ? C55 C51 Gd2 76.2(2) . . ? C52 C51 Gd2 74.2(2) . . ? C51 C52 C53 107.7(4) . . ? C51 C52 Gd2 75.5(2) . . ? C53 C52 Gd2 75.7(2) . . ? C54 C53 C52 108.0(4) . . ? C54 C53 Gd2 75.6(2) . . ? C52 C53 Gd2 74.1(2) . . ? C53 C54 C55 108.4(4) . . ? C53 C54 Gd2 74.6(2) . . ? C55 C54 Gd2 75.4(2) . . ? C51 C55 C54 107.8(4) . . ? C51 C55 Gd2 74.1(2) . . ? C54 C55 Gd2 74.7(2) . . ? C62 C61 C65 109.2(6) . . ? C62 C61 Gd2 74.6(3) . . ? C65 C61 Gd2 78.2(3) . . ? C61 C62 C63 112.1(6) . . ? C61 C62 Gd2 76.9(3) . . ? C63 C62 Gd2 76.7(3) . . ? C62 C63 C64 102.2(5) . . ? C62 C63 Gd2 73.2(3) . . ? C64 C63 Gd2 75.8(2) . . ? C65 C64 C63 104.8(5) . . ? C65 C64 Gd2 75.0(3) . . ? C63 C64 Gd2 72.6(3) . . ? C61 C65 C64 111.6(6) . . ? C61 C65 Gd2 74.1(3) . . ? C64 C65 Gd2 75.9(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.821 _refine_diff_density_min -1.156 _refine_diff_density_rms 0.164 data_nx486 _database_code_depnum_ccdc_archive 'CCDC 286298' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 N6 Nd2' _chemical_formula_weight 793.15 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.155(3) _cell_length_b 16.870(5) _cell_length_c 16.225(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.30(2) _cell_angle_gamma 90.00 _cell_volume 3158.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour blue _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 3.281 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5529 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.00 _reflns_number_total 4396 _reflns_number_gt 3462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0218P)^2^+3.6380P] 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 4396 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.573 _refine_ls_shift/su_mean 0.018 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.22318(3) 0.843307(19) 0.70540(2) 0.02639(11) Uani 1 1 d . . . Nd2 Nd 0.37112(3) 0.734705(19) 0.55644(2) 0.02503(10) Uani 1 1 d . . . N1 N 0.2400(4) 0.7048(3) 0.6461(4) 0.0302(13) Uani 1 1 d . . . H1N H 0.282(5) 0.670(3) 0.666(4) 0.026(19) Uiso 1 1 d . . . C11 C 0.1267(5) 0.6856(4) 0.6284(4) 0.0292(15) Uani 1 1 d . . . N12 N 0.0564(4) 0.7502(3) 0.6219(3) 0.0314(12) Uani 1 1 d . . . C13 C -0.0579(5) 0.7360(4) 0.6072(4) 0.0384(17) Uani 1 1 d . . . C14 C -0.0989(6) 0.6597(4) 0.5997(4) 0.0444(18) Uani 1 1 d . . . H14 H -0.1771 0.6499 0.5908 0.053 Uiso 1 1 calc R . . C15 C -0.0232(6) 0.5981(4) 0.6056(4) 0.0348(16) Uani 1 1 d . . . N16 N 0.0903(4) 0.6091(3) 0.6204(3) 0.0344(13) Uani 1 1 d . . . C131 C -0.1336(6) 0.8072(4) 0.6006(6) 0.067(2) Uani 1 1 d . . . H13A H -0.1198 0.8442 0.5601 0.100 Uiso 1 1 calc R . . H13B H -0.1163 0.8318 0.6566 0.100 Uiso 1 1 calc R . . H13C H -0.2135 0.7912 0.5811 0.100 Uiso 1 1 calc R . . C151 C -0.0662(6) 0.5129(4) 0.5946(5) 0.051(2) Uani 1 1 d . . . H15A H -0.0584 0.4905 0.6506 0.076 Uiso 1 1 calc R . . H15B H -0.0212 0.4826 0.5668 0.076 Uiso 1 1 calc R . . H15C H -0.1462 0.5120 0.5596 0.076 Uiso 1 1 calc R . . N2 N 0.4256(5) 0.8298(3) 0.6892(4) 0.0285(13) Uani 1 1 d . . . H2N H 0.449(5) 0.823(3) 0.735(3) 0.022(19) Uiso 1 1 d . . . C21 C 0.5011(5) 0.8734(3) 0.6615(4) 0.0225(13) Uani 1 1 d . . . N22 N 0.4872(4) 0.8635(3) 0.5748(3) 0.0276(12) Uani 1 1 d . . . C23 C 0.5639(5) 0.9005(3) 0.5426(4) 0.0281(14) Uani 1 1 d . . . C24 C 0.6502(5) 0.9470(4) 0.5955(4) 0.0346(16) Uani 1 1 d . . . H24 H 0.7030 0.9723 0.5736 0.041 Uiso 1 1 calc R . . C25 C 0.6577(5) 0.9559(4) 0.6827(4) 0.0346(16) Uani 1 1 d . . . N26 N 0.5842(4) 0.9189(3) 0.7161(3) 0.0303(12) Uani 1 1 d . . . C231 C 0.5530(6) 0.8860(4) 0.4500(4) 0.0450(18) Uani 1 1 d . . . H23A H 0.4809 0.9073 0.4137 0.068 Uiso 1 1 calc R . . H23B H 0.5552 0.8300 0.4401 0.068 Uiso 1 1 calc R . . H23C H 0.6160 0.9113 0.4365 0.068 Uiso 1 1 calc R . . C251 C 0.7500(7) 1.0060(5) 0.7446(5) 0.066(3) Uani 1 1 d . . . H25A H 0.8250 0.9887 0.7440 0.098 Uiso 1 1 calc R . . H25B H 0.7449 1.0006 0.8022 0.098 Uiso 1 1 calc R . . H25C H 0.7389 1.0605 0.7270 0.098 Uiso 1 1 calc R . . C31 C 0.1047(8) 0.9495(4) 0.5799(5) 0.061(2) Uani 1 1 d . . . C32 C 0.0854(7) 0.9777(4) 0.6546(6) 0.059(2) Uani 1 1 d . . . C33 C 0.1911(7) 1.0072(4) 0.7104(5) 0.054(2) Uani 1 1 d . . . C34 C 0.2745(6) 0.9968(4) 0.6693(5) 0.0467(19) Uani 1 1 d . . . C35 C 0.2209(7) 0.9615(4) 0.5890(5) 0.050(2) Uani 1 1 d . . . C41 C 0.3340(7) 0.8099(10) 0.8773(5) 0.091(4) Uani 1 1 d . . . C42 C 0.2653(13) 0.8740(8) 0.8761(5) 0.084(3) Uani 1 1 d . . . C43 C 0.1563(12) 0.8557(9) 0.8496(7) 0.097(4) Uani 1 1 d . . . C44 C 0.1456(10) 0.7797(9) 0.8342(6) 0.081(3) Uani 1 1 d . . . C45 C 0.2500(14) 0.7447(5) 0.8479(5) 0.081(3) Uani 1 1 d . . . C51 C 0.1659(7) 0.6998(5) 0.4295(5) 0.055(2) Uani 1 1 d . . . C52 C 0.1608(6) 0.7807(5) 0.4400(4) 0.049(2) Uani 1 1 d . . . C53 C 0.2432(8) 0.8153(5) 0.4094(5) 0.059(2) Uani 1 1 d . . . C54 C 0.2980(7) 0.7540(7) 0.3775(5) 0.071(3) Uani 1 1 d . . . C55 C 0.2463(8) 0.6835(6) 0.3909(5) 0.067(3) Uani 1 1 d . . . C61 C 0.5747(6) 0.6616(5) 0.5589(5) 0.0491(19) Uani 1 1 d . . . C62 C 0.4920(7) 0.6036(5) 0.5326(5) 0.057(2) Uani 1 1 d . . . C63 C 0.4556(7) 0.5851(4) 0.6034(7) 0.069(3) Uani 1 1 d . . . C64 C 0.5173(8) 0.6322(6) 0.6728(5) 0.065(3) Uani 1 1 d . . . C65 C 0.5909(6) 0.6800(5) 0.6441(5) 0.054(2) Uani 1 1 d . . . H31 H 0.0429 0.9292 0.5414 0.04(2) Uiso 1 1 d . . . H32 H 0.0082 0.9812 0.6800 0.07(2) Uiso 1 1 d . . . H33 H 0.2056 1.0177 0.7822 0.19(5) Uiso 1 1 d . . . H34 H 0.3756 1.0015 0.6980 0.06(2) Uiso 1 1 d . . . H35 H 0.2459 0.9450 0.5375 0.07(2) Uiso 1 1 d . . . H41 H 0.4021 0.8005 0.8982 0.11(4) Uiso 1 1 d . . . H42 H 0.2831 0.9169 0.8777 0.10(4) Uiso 1 1 d . . . H43 H 0.1062 0.8790 0.8424 0.118 Uiso 1 1 d . . . H44 H 0.0857 0.7562 0.8219 0.09(4) Uiso 1 1 d . . . H45 H 0.2866 0.7018 0.8378 0.09(3) Uiso 1 1 d . . . H51 H 0.1223 0.6681 0.4419 0.06(3) Uiso 1 1 d . . . H52 H 0.1068 0.8061 0.4620 0.06(2) Uiso 1 1 d . . . H53 H 0.2589 0.8645 0.4025 0.07(3) Uiso 1 1 d . . . H54 H 0.3528 0.7622 0.3580 0.06(2) Uiso 1 1 d . . . H55 H 0.2579 0.6331 0.3776 0.14(4) Uiso 1 1 d . . . H61 H 0.6111 0.6843 0.5219 0.04(2) Uiso 1 1 d . . . H62 H 0.4619 0.5711 0.4794 0.10(3) Uiso 1 1 d . . . H63 H 0.4074 0.5418 0.5981 0.08(3) Uiso 1 1 d . . . H64 H 0.5059 0.6313 0.7200 0.07(3) Uiso 1 1 d . . . H65 H 0.6459 0.7168 0.6821 0.06(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0271(2) 0.02576(19) 0.02896(19) 0.00045(15) 0.01259(15) -0.00119(15) Nd2 0.02193(19) 0.02288(18) 0.0304(2) -0.00290(15) 0.00848(15) -0.00067(15) N1 0.020(3) 0.023(3) 0.049(4) 0.004(3) 0.013(3) 0.002(3) C11 0.028(4) 0.036(4) 0.024(3) -0.001(3) 0.009(3) 0.001(3) N12 0.026(3) 0.028(3) 0.039(3) 0.001(2) 0.008(3) 0.003(2) C13 0.017(4) 0.055(4) 0.043(4) 0.000(4) 0.008(3) 0.004(3) C14 0.020(4) 0.059(5) 0.054(5) -0.007(4) 0.012(3) -0.011(4) C15 0.035(4) 0.040(4) 0.031(4) 0.001(3) 0.012(3) -0.006(3) N16 0.033(3) 0.031(3) 0.040(3) 0.001(3) 0.014(3) -0.007(3) C131 0.027(4) 0.057(5) 0.113(7) -0.015(5) 0.016(5) 0.009(4) C151 0.049(5) 0.047(4) 0.057(5) 0.007(4) 0.017(4) -0.019(4) N2 0.031(3) 0.026(3) 0.030(3) 0.002(3) 0.011(3) -0.004(2) C21 0.021(3) 0.017(3) 0.032(4) 0.003(3) 0.012(3) 0.003(3) N22 0.032(3) 0.025(3) 0.029(3) -0.003(2) 0.014(2) -0.001(2) C23 0.027(3) 0.027(3) 0.033(4) 0.005(3) 0.013(3) 0.006(3) C24 0.028(4) 0.034(4) 0.046(4) 0.004(3) 0.017(3) -0.005(3) C25 0.031(4) 0.026(3) 0.040(4) 0.011(3) 0.002(3) -0.005(3) N26 0.030(3) 0.029(3) 0.029(3) 0.002(2) 0.005(2) -0.012(3) C231 0.063(5) 0.041(4) 0.040(4) 0.001(3) 0.029(4) -0.010(4) C251 0.068(6) 0.068(5) 0.049(5) 0.001(4) 0.001(4) -0.047(5) C31 0.065(6) 0.030(4) 0.067(6) 0.013(4) -0.011(5) 0.012(4) C32 0.066(6) 0.029(4) 0.093(7) 0.007(4) 0.041(5) 0.021(4) C33 0.074(6) 0.028(4) 0.074(6) -0.006(4) 0.042(5) -0.003(4) C34 0.048(5) 0.032(4) 0.061(5) 0.004(4) 0.017(4) -0.008(4) C35 0.075(6) 0.034(4) 0.050(5) 0.021(4) 0.032(5) 0.008(4) C41 0.031(5) 0.212(14) 0.028(5) 0.046(7) 0.007(4) 0.033(8) C42 0.113(11) 0.107(10) 0.034(5) -0.010(5) 0.027(6) -0.034(9) C43 0.116(11) 0.128(11) 0.081(8) 0.023(8) 0.080(8) 0.021(9) C44 0.074(8) 0.127(10) 0.047(5) 0.031(6) 0.024(5) -0.044(8) C45 0.164(12) 0.054(6) 0.033(5) 0.019(4) 0.042(7) 0.031(8) C51 0.034(4) 0.069(6) 0.055(5) -0.008(4) 0.004(4) -0.019(5) C52 0.040(5) 0.062(5) 0.036(4) -0.003(4) 0.000(4) 0.010(4) C53 0.077(6) 0.049(5) 0.032(4) 0.018(4) -0.010(4) -0.014(5) C54 0.047(5) 0.136(10) 0.025(4) -0.008(5) 0.005(4) -0.010(6) C55 0.075(7) 0.067(6) 0.043(5) -0.030(4) -0.006(5) -0.004(5) C61 0.032(4) 0.056(5) 0.070(6) 0.007(4) 0.031(4) 0.013(4) C62 0.058(5) 0.044(5) 0.072(6) -0.017(5) 0.026(5) 0.018(4) C63 0.047(5) 0.028(4) 0.131(9) 0.013(5) 0.025(6) 0.011(4) C64 0.060(6) 0.095(7) 0.051(5) 0.043(5) 0.032(5) 0.063(6) C65 0.036(4) 0.054(5) 0.067(6) -0.004(4) 0.006(4) 0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N2 2.565(5) . ? Nd1 N1 2.560(5) . ? Nd1 N12 2.586(5) . ? Nd1 C42 2.703(8) . ? Nd1 C43 2.715(9) . ? Nd1 C35 2.740(6) . ? Nd1 C41 2.748(8) . ? Nd1 C31 2.755(7) . ? Nd1 C34 2.769(7) . ? Nd1 C44 2.765(8) . ? Nd1 C45 2.783(8) . ? Nd1 C32 2.786(7) . ? Nd2 N1 2.522(5) . ? Nd2 N22 2.557(5) . ? Nd2 N2 2.599(6) . ? Nd2 C63 2.741(7) . ? Nd2 C62 2.750(7) . ? Nd2 C61 2.754(6) . ? Nd2 C51 2.754(7) . ? Nd2 C53 2.761(7) . ? Nd2 C64 2.758(7) . ? Nd2 C65 2.762(7) . ? Nd2 C52 2.769(7) . ? Nd2 C55 2.776(7) . ? N1 C11 1.356(8) . ? C11 N16 1.356(7) . ? C11 N12 1.369(7) . ? N12 C13 1.356(8) . ? C13 C14 1.372(9) . ? C13 C131 1.496(9) . ? C14 C15 1.372(9) . ? C15 N16 1.336(8) . ? C15 C151 1.520(9) . ? N2 C21 1.359(7) . ? C21 N26 1.353(7) . ? C21 N22 1.373(7) . ? N22 C23 1.356(7) . ? C23 C24 1.374(8) . ? C23 C231 1.485(8) . ? C24 C25 1.396(8) . ? C25 N26 1.337(7) . ? C25 C251 1.508(8) . ? C31 C32 1.389(11) . ? C31 C35 1.388(11) . ? C32 C33 1.409(11) . ? C33 C34 1.389(10) . ? C34 C35 1.393(10) . ? C41 C42 1.363(15) . ? C41 C45 1.474(14) . ? C42 C43 1.295(14) . ? C43 C44 1.304(15) . ? C44 C45 1.354(14) . ? C51 C55 1.345(11) . ? C51 C52 1.380(11) . ? C52 C53 1.379(11) . ? C53 C54 1.414(12) . ? C54 C55 1.394(12) . ? C61 C65 1.370(10) . ? C61 C62 1.371(10) . ? C62 C63 1.390(11) . ? C63 C64 1.390(12) . ? C64 C65 1.389(11) . ? 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 N2 Nd1 N1 71.79(16) . . ? N2 Nd1 N12 120.75(16) . . ? N1 Nd1 N12 52.45(16) . . ? N2 Nd1 C42 104.1(4) . . ? N1 Nd1 C42 123.3(3) . . ? N12 Nd1 C42 121.2(3) . . ? N2 Nd1 C43 130.6(3) . . ? N1 Nd1 C43 118.4(3) . . ? N12 Nd1 C43 95.8(4) . . ? C42 Nd1 C43 27.7(3) . . ? N2 Nd1 C35 78.3(2) . . ? N1 Nd1 C35 112.9(2) . . ? N12 Nd1 C35 104.1(2) . . ? C42 Nd1 C35 121.6(3) . . ? C43 Nd1 C35 126.7(3) . . ? N2 Nd1 C41 84.6(2) . . ? N1 Nd1 C41 97.1(4) . . ? N12 Nd1 C41 117.5(3) . . ? C42 Nd1 C41 28.9(3) . . ? C43 Nd1 C41 47.6(3) . . ? C35 Nd1 C41 138.1(4) . . ? N2 Nd1 C31 106.1(2) . . ? N1 Nd1 C31 113.6(2) . . ? N12 Nd1 C31 82.3(2) . . ? C42 Nd1 C31 121.3(4) . . ? C43 Nd1 C31 111.0(3) . . ? C35 Nd1 C31 29.3(2) . . ? C41 Nd1 C31 149.3(4) . . ? N2 Nd1 C34 76.97(19) . . ? N1 Nd1 C34 136.4(2) . . ? N12 Nd1 C34 130.44(19) . . ? C42 Nd1 C34 93.1(3) . . ? C43 Nd1 C34 105.0(4) . . ? C35 Nd1 C34 29.3(2) . . ? C41 Nd1 C34 109.6(4) . . ? C31 Nd1 C34 48.4(2) . . ? N2 Nd1 C44 127.5(3) . . ? N1 Nd1 C44 91.0(4) . . ? N12 Nd1 C44 76.3(3) . . ? C42 Nd1 C44 45.6(3) . . ? C43 Nd1 C44 27.5(3) . . ? C35 Nd1 C44 150.6(4) . . ? C41 Nd1 C44 47.8(3) . . ? C31 Nd1 C44 126.0(4) . . ? C34 Nd1 C44 132.5(4) . . ? N2 Nd1 C45 99.6(3) . . ? N1 Nd1 C45 76.4(2) . . ? N12 Nd1 C45 86.6(3) . . ? C42 Nd1 C45 47.8(3) . . ? C43 Nd1 C45 47.1(3) . . ? C35 Nd1 C45 168.7(3) . . ? C41 Nd1 C45 30.9(3) . . ? C31 Nd1 C45 154.2(4) . . ? C34 Nd1 C45 139.4(3) . . ? C44 Nd1 C45 28.2(3) . . ? N2 Nd1 C32 123.3(2) . . ? N1 Nd1 C32 138.0(2) . . ? N12 Nd1 C32 92.3(2) . . ? C42 Nd1 C32 92.9(4) . . ? C43 Nd1 C32 83.0(3) . . ? C35 Nd1 C32 47.8(2) . . ? C41 Nd1 C32 121.7(4) . . ? C31 Nd1 C32 29.0(2) . . ? C34 Nd1 C32 48.0(2) . . ? C44 Nd1 C32 102.9(4) . . ? C45 Nd1 C32 129.4(3) . . ? N1 Nd2 N22 121.87(16) . . ? N1 Nd2 N2 71.83(17) . . ? N22 Nd2 N2 52.51(16) . . ? N1 Nd2 C63 84.6(2) . . ? N22 Nd2 C63 127.3(2) . . ? N2 Nd2 C63 111.2(3) . . ? N1 Nd2 C62 112.5(2) . . ? N22 Nd2 C62 113.6(2) . . ? N2 Nd2 C62 127.2(2) . . ? C63 Nd2 C62 29.3(2) . . ? N1 Nd2 C61 129.0(2) . . ? N22 Nd2 C61 85.3(2) . . ? N2 Nd2 C61 105.7(2) . . ? C63 Nd2 C61 47.7(2) . . ? C62 Nd2 C61 28.9(2) . . ? N1 Nd2 C51 78.5(2) . . ? N22 Nd2 C51 127.3(2) . . ? N2 Nd2 C51 133.4(2) . . ? C63 Nd2 C51 100.5(3) . . ? C62 Nd2 C51 97.0(3) . . ? C61 Nd2 C51 120.9(3) . . ? N1 Nd2 C53 108.1(2) . . ? N22 Nd2 C53 79.8(2) . . ? N2 Nd2 C53 109.9(2) . . ? C63 Nd2 C53 138.9(3) . . ? C62 Nd2 C53 117.1(3) . . ? C61 Nd2 C53 119.5(3) . . ? C51 Nd2 C53 47.7(2) . . ? N1 Nd2 C64 82.4(2) . . ? N22 Nd2 C64 103.9(3) . . ? N2 Nd2 C64 83.0(3) . . ? C63 Nd2 C64 29.3(2) . . ? C62 Nd2 C64 48.2(2) . . ? C61 Nd2 C64 47.7(2) . . ? C51 Nd2 C64 128.0(3) . . ? C53 Nd2 C64 165.2(3) . . ? N1 Nd2 C65 108.7(2) . . ? N22 Nd2 C65 79.3(2) . . ? N2 Nd2 C65 80.0(2) . . ? C63 Nd2 C65 48.1(2) . . ? C62 Nd2 C65 47.9(2) . . ? C61 Nd2 C65 28.8(2) . . ? C51 Nd2 C65 144.7(3) . . ? C53 Nd2 C65 143.2(3) . . ? C64 Nd2 C65 29.1(2) . . ? N1 Nd2 C52 80.5(2) . . ? N22 Nd2 C52 101.5(2) . . ? N2 Nd2 C52 109.4(2) . . ? C63 Nd2 C52 129.2(3) . . ? C62 Nd2 C52 123.3(2) . . ? C61 Nd2 C52 140.2(2) . . ? C51 Nd2 C52 28.9(2) . . ? C53 Nd2 C52 28.9(2) . . ? C64 Nd2 C52 154.3(3) . . ? C65 Nd2 C52 168.9(2) . . ? N1 Nd2 C55 104.1(3) . . ? N22 Nd2 C55 119.4(2) . . ? N2 Nd2 C55 156.0(2) . . ? C63 Nd2 C55 91.4(3) . . ? C62 Nd2 C55 76.5(3) . . ? C61 Nd2 C55 95.2(3) . . ? C51 Nd2 C55 28.2(2) . . ? C53 Nd2 C55 47.8(3) . . ? C64 Nd2 C55 120.4(3) . . ? C65 Nd2 C55 122.7(3) . . ? C52 Nd2 C55 47.2(2) . . ? C11 N1 Nd2 135.3(4) . . ? C11 N1 Nd1 95.9(4) . . ? Nd2 N1 Nd1 100.02(17) . . ? N16 C11 N1 121.8(6) . . ? N16 C11 N12 125.0(5) . . ? N1 C11 N12 113.1(5) . . ? C13 N12 C11 116.9(5) . . ? C13 N12 Nd1 142.3(4) . . ? C11 N12 Nd1 94.4(4) . . ? N12 C13 C14 120.3(6) . . ? N12 C13 C131 116.4(6) . . ? C14 C13 C131 123.3(6) . . ? C15 C14 C13 119.2(6) . . ? N16 C15 C14 122.6(6) . . ? N16 C15 C151 116.8(6) . . ? C14 C15 C151 120.6(6) . . ? C15 N16 C11 115.9(6) . . ? C21 N2 Nd1 139.0(4) . . ? C21 N2 Nd2 94.8(4) . . ? Nd1 N2 Nd2 97.88(18) . . ? N26 C21 N2 122.2(5) . . ? N26 C21 N22 124.5(5) . . ? N2 C21 N22 113.2(5) . . ? C23 N22 C21 117.4(5) . . ? C23 N22 Nd2 140.1(4) . . ? C21 N22 Nd2 96.3(3) . . ? N22 C23 C24 120.3(5) . . ? N22 C23 C231 117.4(5) . . ? C24 C23 C231 122.3(6) . . ? C23 C24 C25 119.3(6) . . ? N26 C25 C24 121.4(6) . . ? N26 C25 C251 116.4(6) . . ? C24 C25 C251 122.2(6) . . ? C25 N26 C21 117.1(5) . . ? C32 C31 C35 107.6(7) . . ? C32 C31 Nd1 76.7(4) . . ? C35 C31 Nd1 74.8(4) . . ? C31 C32 C33 108.2(7) . . ? C31 C32 Nd1 74.3(4) . . ? C33 C32 Nd1 75.8(4) . . ? C34 C33 C32 107.6(7) . . ? C34 C33 Nd1 74.5(4) . . ? C32 C33 Nd1 74.9(4) . . ? C33 C34 C35 107.8(7) . . ? C33 C34 Nd1 76.6(4) . . ? C35 C34 Nd1 74.2(4) . . ? C31 C35 C34 108.9(7) . . ? C31 C35 Nd1 76.0(4) . . ? C34 C35 Nd1 76.5(4) . . ? C42 C41 C45 103.2(9) . . ? C42 C41 Nd1 73.7(5) . . ? C45 C41 Nd1 75.9(4) . . ? C43 C42 C41 111.9(12) . . ? C43 C42 Nd1 76.7(6) . . ? C41 C42 Nd1 77.4(5) . . ? C42 C43 C44 109.2(12) . . ? C42 C43 Nd1 75.7(6) . . ? C44 C43 Nd1 78.4(6) . . ? C43 C44 C45 111.4(11) . . ? C43 C44 Nd1 74.1(5) . . ? C45 C44 Nd1 76.6(5) . . ? C44 C45 C41 104.2(9) . . ? C44 C45 Nd1 75.1(5) . . ? C41 C45 Nd1 73.2(4) . . ? C55 C51 C52 109.1(8) . . ? C55 C51 Nd2 76.8(4) . . ? C52 C51 Nd2 76.1(4) . . ? C51 C52 C53 108.0(7) . . ? C51 C52 Nd2 74.9(4) . . ? C53 C52 Nd2 75.2(4) . . ? C52 C53 C54 107.6(7) . . ? C52 C53 Nd2 75.9(4) . . ? C54 C53 Nd2 75.8(4) . . ? C55 C54 C53 106.2(8) . . ? C55 C54 Nd2 75.4(5) . . ? C53 C54 Nd2 74.6(4) . . ? C51 C55 C54 109.1(8) . . ? C51 C55 Nd2 75.0(4) . . ? C54 C55 Nd2 75.5(4) . . ? C65 C61 C62 109.6(7) . . ? C65 C61 Nd2 76.0(4) . . ? C62 C61 Nd2 75.4(4) . . ? C61 C62 C63 107.2(7) . . ? C61 C62 Nd2 75.7(4) . . ? C63 C62 Nd2 75.0(4) . . ? C62 C63 C64 108.1(8) . . ? C62 C63 Nd2 75.7(4) . . ? C64 C63 Nd2 76.0(4) . . ? C65 C64 C63 107.5(7) . . ? C65 C64 Nd2 75.6(4) . . ? C63 C64 Nd2 74.7(4) . . ? C61 C65 C64 107.6(7) . . ? C61 C65 Nd2 75.3(4) . . ? C64 C65 Nd2 75.3(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.492 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.114 # Attachment '3.cif' data_m_3 _database_code_depnum_ccdc_archive 'CCDC 286299' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 Dy2 N6' _chemical_formula_weight 1013.94 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.274(2) _cell_length_b 13.766(2) _cell_length_c 23.426(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4280.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour amber _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 3.502 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.08869 _exptl_absorpt_correction_T_max 0.11776 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4225 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.00 _reflns_number_total 4011 _reflns_number_gt 3715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0837P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 4011 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.147 _refine_ls_shift/su_mean 0.010 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.73033(3) 0.27928(3) 0.118455(19) 0.02676(15) Uani 1 1 d . . . N1 N 0.7808(7) 0.1103(6) 0.0909(3) 0.033(2) Uani 1 1 d . . . H1 H 0.7244 0.0735 0.0950 0.040 Uiso 1 1 calc R . . C11 C 0.7874(8) 0.1304(8) 0.0344(4) 0.031(2) Uani 1 1 d . . . N16 N 0.7840(7) 0.0593(7) -0.0049(4) 0.039(2) Uani 1 1 d . . . C13 C 0.7881(10) 0.0880(10) -0.0595(5) 0.050(3) Uani 1 1 d . . . C14 C 0.7960(9) 0.1850(9) -0.0753(5) 0.046(3) Uani 1 1 d . . . H14 H 0.8011 0.2024 -0.1135 0.055 Uiso 1 1 calc R . . C15 C 0.7963(9) 0.2549(9) -0.0332(5) 0.043(3) Uani 1 1 d . . . N12 N 0.7942(6) 0.2279(6) 0.0227(3) 0.0299(19) Uani 1 1 d . . . C131 C 0.7868(14) 0.0084(11) -0.1033(5) 0.077(5) Uani 1 1 d . . . H13A H 0.8486 -0.0277 -0.1012 0.115 Uiso 1 1 calc R . . H13B H 0.7801 0.0363 -0.1407 0.115 Uiso 1 1 calc R . . H13C H 0.7310 -0.0342 -0.0961 0.115 Uiso 1 1 calc R . . C151 C 0.8001(10) 0.3613(8) -0.0476(5) 0.043(3) Uani 1 1 d . . . H15A H 0.7394 0.3922 -0.0347 0.064 Uiso 1 1 calc R . . H15B H 0.8061 0.3690 -0.0882 0.064 Uiso 1 1 calc R . . H15C H 0.8571 0.3905 -0.0292 0.064 Uiso 1 1 calc R . . Dy2 Dy 0.88844(4) 0.06847(3) 0.17131(2) 0.02831(15) Uani 1 1 d . . . N2 N 0.7555(6) 0.1827(6) 0.2062(3) 0.0264(19) Uani 1 1 d . . . H2 H 0.6986 0.1471 0.2117 0.032 Uiso 1 1 calc R . . C21 C 0.7981(8) 0.1961(7) 0.2580(4) 0.029(2) Uani 1 1 d . . . N26 N 0.7462(7) 0.2354(7) 0.3015(4) 0.039(2) Uani 1 1 d . . . C23 C 0.7966(9) 0.2449(9) 0.3522(5) 0.040(3) Uani 1 1 d . . . C24 C 0.8965(9) 0.2140(8) 0.3568(5) 0.040(3) Uani 1 1 d . . . H24 H 0.9306 0.2213 0.3912 0.048 Uiso 1 1 calc R . . C25 C 0.9439(9) 0.1738(8) 0.3116(5) 0.036(3) Uani 1 1 d . . . N22 N 0.8953(7) 0.1660(6) 0.2603(4) 0.033(2) Uani 1 1 d . . . C231 C 0.7389(11) 0.2882(12) 0.4006(5) 0.071(4) Uani 1 1 d . . . H23A H 0.7277 0.3560 0.3933 0.106 Uiso 1 1 calc R . . H23B H 0.7767 0.2809 0.4353 0.106 Uiso 1 1 calc R . . H23C H 0.6753 0.2556 0.4043 0.106 Uiso 1 1 calc R . . C251 C 1.0509(10) 0.1350(9) 0.3147(5) 0.047(3) Uani 1 1 d . . . H25A H 1.0498 0.0655 0.3115 0.070 Uiso 1 1 calc R . . H25B H 1.0806 0.1532 0.3505 0.070 Uiso 1 1 calc R . . H25C H 1.0899 0.1618 0.2840 0.070 Uiso 1 1 calc R . . C31 C 0.8105(10) 0.4085(8) 0.1920(5) 0.044(3) Uani 1 1 d . . . H31 H 0.7950 0.3983 0.2303 0.053 Uiso 1 1 calc R . . C32 C 0.7582(11) 0.4655(7) 0.1536(5) 0.044(3) Uani 1 1 d . . . H32 H 0.7015 0.5025 0.1620 0.053 Uiso 1 1 calc R . . C33 C 0.8044(9) 0.4583(7) 0.1001(5) 0.040(3) Uani 1 1 d . . . H33 H 0.7826 0.4877 0.0665 0.047 Uiso 1 1 calc R . . C34 C 0.8891(10) 0.3990(8) 0.1061(5) 0.046(3) Uani 1 1 d . . . H34 H 0.9345 0.3835 0.0773 0.055 Uiso 1 1 calc R . . C35 C 0.8942(9) 0.3679(8) 0.1607(5) 0.040(3) Uani 1 1 d . . . H35 H 0.9434 0.3272 0.1757 0.048 Uiso 1 1 calc R . . C41 C 0.5647(10) 0.3336(14) 0.0650(8) 0.073(6) Uani 1 1 d . . . H41 H 0.5755 0.3770 0.0352 0.087 Uiso 1 1 calc R . . C42 C 0.5477(10) 0.3572(12) 0.1186(8) 0.066(4) Uani 1 1 d . . . H42 H 0.5423 0.4203 0.1324 0.079 Uiso 1 1 calc R . . C43 C 0.5391(9) 0.2733(19) 0.1517(6) 0.087(7) Uani 1 1 d . . . H43 H 0.5299 0.2702 0.1910 0.105 Uiso 1 1 calc R . . C44 C 0.5467(10) 0.1973(12) 0.1152(9) 0.069(4) Uani 1 1 d . . . H44 H 0.5413 0.1322 0.1254 0.082 Uiso 1 1 calc R . . C45 C 0.5638(10) 0.2314(14) 0.0606(7) 0.067(5) Uani 1 1 d . . . H45 H 0.5729 0.1946 0.0277 0.080 Uiso 1 1 calc R . . C51 C 1.0235(9) 0.1605(9) 0.1045(5) 0.044(3) Uani 1 1 d . . . H51 H 1.0023 0.2178 0.0873 0.052 Uiso 1 1 calc R . . C52 C 1.0692(9) 0.1528(10) 0.1577(6) 0.051(3) Uani 1 1 d . . . H52 H 1.0843 0.2044 0.1818 0.061 Uiso 1 1 calc R . . C53 C 1.0891(9) 0.0525(10) 0.1692(6) 0.050(3) Uani 1 1 d . . . H53 H 1.1184 0.0272 0.2020 0.060 Uiso 1 1 calc R . . C54 C 1.0571(9) 0.0012(9) 0.1228(7) 0.057(4) Uani 1 1 d . . . H54 H 1.0620 -0.0658 0.1189 0.068 Uiso 1 1 calc R . . C55 C 1.0149(9) 0.0650(10) 0.0809(5) 0.047(3) Uani 1 1 d . . . H55 H 0.9875 0.0479 0.0458 0.056 Uiso 1 1 calc R . . C61 C 0.8433(13) -0.1199(8) 0.1625(5) 0.058(4) Uani 1 1 d . . . H61 H 0.8579 -0.1479 0.1273 0.070 Uiso 1 1 calc R . . C62 C 0.7520(10) -0.0773(9) 0.1776(6) 0.054(3) Uani 1 1 d . . . H62 H 0.6955 -0.0712 0.1545 0.065 Uiso 1 1 calc R . . C63 C 0.7608(10) -0.0454(9) 0.2342(5) 0.049(3) Uani 1 1 d . . . H63 H 0.7111 -0.0149 0.2557 0.059 Uiso 1 1 calc R . . C64 C 0.8593(9) -0.0682(9) 0.2526(5) 0.046(3) Uani 1 1 d . . . H64 H 0.8864 -0.0547 0.2883 0.055 Uiso 1 1 calc R . . C65 C 0.9083(10) -0.1140(8) 0.2080(5) 0.048(3) Uani 1 1 d . . . H65 H 0.9742 -0.1369 0.2087 0.057 Uiso 1 1 calc R . . C1T C 0.4919(13) 0.0600(15) 0.2680(9) 0.077(6) Uani 1 1 d . . . H1T H 0.5429 0.0145 0.2733 0.093 Uiso 1 1 calc R . . C2T C 0.4931(19) 0.138(3) 0.2987(12) 0.142(15) Uani 1 1 d . . . H2T H 0.5466 0.1487 0.3235 0.170 Uiso 1 1 calc R . . C3T C 0.417(3) 0.2039(19) 0.2953(9) 0.129(12) Uani 1 1 d . . . H3T H 0.4172 0.2577 0.3193 0.155 Uiso 1 1 calc R . . C4T C 0.3451(17) 0.1923(12) 0.2587(9) 0.088(6) Uani 1 1 d . . . H4T H 0.2938 0.2382 0.2565 0.105 Uiso 1 1 calc R . . C5T C 0.3436(11) 0.1130(15) 0.2232(7) 0.075(5) Uani 1 1 d . . . H5T H 0.2930 0.1064 0.1960 0.090 Uiso 1 1 calc R . . C6T C 0.4198(15) 0.0410(11) 0.2282(7) 0.072(5) Uani 1 1 d . . . C7T C 0.425(3) -0.0456(16) 0.1913(12) 0.193(17) Uani 1 1 d . . . H7T1 H 0.3584 -0.0610 0.1777 0.290 Uiso 1 1 calc R . . H7T2 H 0.4508 -0.0994 0.2128 0.290 Uiso 1 1 calc R . . H7T3 H 0.4681 -0.0327 0.1594 0.290 Uiso 1 1 calc R . . C1S C 0.882(2) 0.208(3) 0.5385(9) 0.129(10) Uani 1 1 d . . . H1S H 0.8273 0.1686 0.5478 0.155 Uiso 1 1 calc R . . C2S C 0.868(4) 0.314(4) 0.5522(13) 0.25(3) Uani 1 1 d . . . H2S H 0.8127 0.3404 0.5706 0.299 Uiso 1 1 calc R . . C3S C 0.955(6) 0.369(2) 0.532(2) 0.26(4) Uani 1 1 d . . . H3S H 0.9670 0.4349 0.5357 0.307 Uiso 1 1 calc R . . C4S C 1.008(7) 0.309(5) 0.511(2) 0.38(7) Uani 1 1 d . . . H4S H 1.0553 0.3505 0.4948 0.456 Uiso 1 1 calc R . . C5S C 1.0451(19) 0.228(3) 0.4957(8) 0.141(13) Uani 1 1 d . . . H5S H 1.1056 0.2118 0.4779 0.170 Uiso 1 1 calc R . . C6S C 0.957(2) 0.164(2) 0.5159(11) 0.125(9) Uani 1 1 d . . . C7S C 0.978(3) 0.0734(19) 0.5033(11) 0.182(16) Uani 1 1 d . . . H7S1 H 1.0115 0.0433 0.5350 0.272 Uiso 1 1 calc R . . H7S2 H 1.0205 0.0711 0.4703 0.272 Uiso 1 1 calc R . . H7S3 H 0.9162 0.0393 0.4955 0.272 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0263(2) 0.0251(2) 0.0289(2) 0.0011(2) -0.0019(2) -0.0007(2) N1 0.042(5) 0.035(5) 0.021(4) -0.004(4) 0.001(4) 0.004(5) C11 0.025(6) 0.041(6) 0.027(5) 0.001(5) -0.006(4) -0.005(5) N16 0.048(5) 0.037(5) 0.034(5) -0.011(4) -0.002(4) 0.010(5) C13 0.048(7) 0.063(9) 0.038(6) -0.014(6) -0.004(6) 0.009(7) C14 0.050(7) 0.059(8) 0.028(6) -0.003(6) 0.007(5) 0.009(7) C15 0.033(6) 0.049(7) 0.046(7) 0.010(6) 0.005(5) 0.003(6) N12 0.036(5) 0.031(5) 0.022(4) 0.001(4) -0.002(4) 0.002(4) C131 0.111(13) 0.080(10) 0.039(7) -0.028(7) 0.002(8) 0.012(11) C151 0.054(7) 0.039(6) 0.035(6) 0.012(5) 0.008(6) 0.008(6) Dy2 0.0305(3) 0.0246(3) 0.0299(2) 0.0020(2) 0.0006(2) 0.0009(2) N2 0.024(4) 0.032(4) 0.023(4) 0.003(4) -0.007(4) -0.010(4) C21 0.031(6) 0.021(5) 0.034(6) -0.003(4) 0.013(5) 0.003(5) N26 0.040(5) 0.046(5) 0.032(4) -0.002(4) -0.003(4) -0.004(5) C23 0.039(6) 0.045(7) 0.035(6) 0.001(5) 0.001(5) 0.001(6) C24 0.052(7) 0.033(6) 0.035(5) 0.001(5) -0.011(6) -0.004(7) C25 0.051(7) 0.020(5) 0.038(6) 0.008(5) -0.012(5) -0.002(5) N22 0.029(5) 0.030(5) 0.040(5) 0.006(4) -0.006(4) 0.000(4) C231 0.065(8) 0.110(12) 0.038(6) -0.019(8) 0.000(6) -0.004(11) C251 0.054(7) 0.031(6) 0.055(8) -0.007(6) -0.020(6) 0.009(6) C31 0.054(7) 0.039(7) 0.039(6) 0.002(5) -0.001(6) -0.021(6) C32 0.058(8) 0.024(5) 0.051(7) -0.007(5) -0.001(6) -0.004(6) C33 0.049(7) 0.016(5) 0.053(7) -0.003(5) -0.005(6) -0.007(5) C34 0.045(7) 0.026(6) 0.068(8) -0.005(6) 0.004(7) -0.016(6) C35 0.042(6) 0.025(6) 0.053(7) 0.016(5) -0.014(6) -0.005(6) C41 0.024(7) 0.108(14) 0.086(12) 0.074(12) -0.006(8) -0.005(8) C42 0.042(7) 0.067(9) 0.088(12) -0.031(10) -0.030(9) 0.015(7) C43 0.016(6) 0.19(2) 0.054(9) 0.054(13) 0.005(6) 0.022(11) C44 0.028(7) 0.072(10) 0.106(13) 0.025(11) 0.002(9) -0.011(7) C45 0.031(7) 0.099(13) 0.071(10) -0.031(10) -0.021(7) 0.001(9) C51 0.040(7) 0.033(6) 0.058(8) 0.019(6) 0.017(6) 0.010(6) C52 0.034(6) 0.056(8) 0.064(9) 0.005(7) 0.003(6) -0.008(6) C53 0.038(6) 0.063(8) 0.050(7) 0.023(8) 0.003(6) 0.015(6) C54 0.043(7) 0.039(7) 0.089(10) -0.004(8) 0.005(8) 0.011(6) C55 0.037(6) 0.056(7) 0.047(7) -0.001(7) 0.012(5) 0.005(7) C61 0.110(12) 0.020(6) 0.045(7) -0.007(5) 0.006(8) -0.022(7) C62 0.057(8) 0.048(7) 0.057(8) 0.021(7) -0.008(7) -0.026(7) C63 0.049(7) 0.047(7) 0.050(7) 0.016(6) 0.013(6) -0.002(7) C64 0.067(8) 0.036(6) 0.035(6) -0.003(6) -0.005(6) -0.007(7) C65 0.056(8) 0.023(6) 0.063(8) 0.014(6) 0.008(7) -0.001(6) C1T 0.054(9) 0.072(12) 0.107(16) 0.044(12) 0.010(11) 0.002(10) C2T 0.078(15) 0.24(4) 0.11(2) 0.08(3) -0.037(15) -0.07(2) C3T 0.21(3) 0.115(19) 0.062(12) -0.027(13) 0.023(17) -0.10(2) C4T 0.118(16) 0.048(9) 0.097(14) 0.015(10) 0.053(13) 0.027(11) C5T 0.044(8) 0.120(15) 0.062(9) 0.037(10) -0.009(7) -0.039(10) C6T 0.095(13) 0.050(9) 0.072(10) -0.010(8) 0.040(10) -0.017(9) C7T 0.31(4) 0.084(16) 0.19(3) -0.040(17) 0.14(3) -0.08(2) C1S 0.114(17) 0.20(3) 0.078(13) 0.036(17) 0.003(13) 0.08(2) C2S 0.33(6) 0.32(6) 0.09(2) -0.07(3) -0.05(3) 0.24(6) C3S 0.50(11) 0.10(2) 0.17(4) 0.06(2) -0.14(5) -0.11(5) C4S 0.70(18) 0.28(7) 0.16(4) -0.05(4) -0.29(8) 0.23(9) C5S 0.101(15) 0.27(4) 0.052(11) 0.060(19) -0.038(10) -0.07(2) C6S 0.14(2) 0.14(2) 0.101(16) 0.015(16) -0.033(16) 0.06(2) C7S 0.29(4) 0.126(19) 0.13(2) -0.042(18) -0.08(2) 0.12(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 N2 2.471(7) . ? Dy1 N1 2.505(8) . ? Dy1 N12 2.501(8) . ? Dy1 C41 2.638(13) . ? Dy1 C42 2.651(13) . ? Dy1 C43 2.657(12) . ? Dy1 C44 2.687(13) . ? Dy1 C45 2.675(12) . ? Dy1 C33 2.688(10) . ? Dy1 C31 2.695(11) . ? Dy1 C35 2.683(11) . ? Dy1 C32 2.717(10) . ? N1 C11 1.354(13) . ? N1 Dy2 2.434(8) . ? C11 N16 1.344(13) . ? C11 N12 1.374(14) . ? N12 C13 1.339(15) . ? C13 C14 1.390(19) . ? C13 C131 1.502(18) . ? C14 C15 1.377(17) . ? C15 N12 1.360(13) . ? C15 C151 1.504(16) . ? Dy2 N22 2.481(9) . ? Dy2 N2 2.500(8) . ? Dy2 C65 2.667(11) . ? Dy2 C55 2.702(11) . ? Dy2 C53 2.673(12) . ? Dy2 C51 2.696(11) . ? Dy2 C61 2.670(11) . ? Dy2 C54 2.675(12) . ? Dy2 C64 2.704(12) . ? Dy2 C52 2.684(12) . ? Dy2 C62 2.707(11) . ? N2 C21 1.351(13) . ? C21 N22 1.357(13) . ? C21 N26 1.343(13) . ? N26 C23 1.370(14) . ? C23 C24 1.396(17) . ? C23 C231 1.491(17) . ? C24 C25 1.351(16) . ? C25 N22 1.369(13) . ? C25 C251 1.519(17) . ? C31 C32 1.381(17) . ? C31 C35 1.442(17) . ? C32 C33 1.401(17) . ? C33 C34 1.395(17) . ? C34 C35 1.351(17) . ? C41 C42 1.32(2) . ? C41 C45 1.41(2) . ? C42 C43 1.39(3) . ? C43 C44 1.35(2) . ? C44 C45 1.38(2) . ? C51 C55 1.431(18) . ? C51 C52 1.388(18) . ? C52 C53 1.431(19) . ? C53 C54 1.364(18) . ? C54 C55 1.430(18) . ? C61 C65 1.374(19) . ? C61 C62 1.39(2) . ? C62 C63 1.402(18) . ? C63 C64 1.411(18) . ? C64 C65 1.382(17) . ? C1T C2T 1.29(4) . ? C1T C6T 1.36(2) . ? C2T C3T 1.36(4) . ? C3T C4T 1.29(3) . ? C4T C5T 1.37(3) . ? C5T C6T 1.42(2) . ? C6T C7T 1.47(3) . ? C1S C6S 1.29(3) . ? C1S C2S 1.50(6) . ? C2S C3S 1.46(7) . ? C3S C4S 1.18(10) . ? C4S C5S 1.28(5) . ? C5S C6S 1.53(4) . ? C6S C7S 1.31(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 N2 Dy1 N1 71.3(3) . . ? N2 Dy1 N12 123.3(3) . . ? N1 Dy1 N12 54.2(3) . . ? N2 Dy1 C41 131.3(3) . . ? N1 Dy1 C41 111.3(5) . . ? N12 Dy1 C41 86.4(5) . . ? N2 Dy1 C42 109.9(5) . . ? N1 Dy1 C42 128.4(4) . . ? N12 Dy1 C42 115.2(4) . . ? C41 Dy1 C42 28.8(5) . . ? N2 Dy1 C43 82.5(4) . . ? N1 Dy1 C43 107.6(6) . . ? N12 Dy1 C43 125.3(5) . . ? C41 Dy1 C43 49.6(4) . . ? C42 Dy1 C43 30.5(6) . . ? N2 Dy1 C44 85.4(4) . . ? N1 Dy1 C44 81.1(5) . . ? N12 Dy1 C44 99.4(5) . . ? C41 Dy1 C44 49.4(5) . . ? C42 Dy1 C44 48.7(5) . . ? C43 Dy1 C44 29.4(5) . . ? N2 Dy1 C45 113.6(5) . . ? N1 Dy1 C45 82.1(4) . . ? N12 Dy1 C45 75.9(4) . . ? C41 Dy1 C45 30.8(5) . . ? C42 Dy1 C45 49.1(5) . . ? C43 Dy1 C45 49.6(5) . . ? C44 Dy1 C45 29.9(5) . . ? N2 Dy1 C33 125.3(3) . . ? N1 Dy1 C33 135.4(3) . . ? N12 Dy1 C33 89.5(3) . . ? C41 Dy1 C33 88.2(5) . . ? C42 Dy1 C33 87.9(5) . . ? C43 Dy1 C33 115.1(6) . . ? C44 Dy1 C33 135.4(4) . . ? C45 Dy1 C33 116.5(5) . . ? N2 Dy1 C31 76.7(3) . . ? N1 Dy1 C31 132.2(3) . . ? N12 Dy1 C31 128.8(3) . . ? C41 Dy1 C31 116.4(6) . . ? C42 Dy1 C31 95.4(4) . . ? C43 Dy1 C31 102.1(6) . . ? C44 Dy1 C31 130.8(6) . . ? C45 Dy1 C31 144.4(5) . . ? C33 Dy1 C31 49.7(4) . . ? N2 Dy1 C35 80.1(3) . . ? N1 Dy1 C35 107.5(3) . . ? N12 Dy1 C35 100.7(3) . . ? C41 Dy1 C35 136.2(5) . . ? C42 Dy1 C35 123.8(4) . . ? C43 Dy1 C35 132.9(6) . . ? C44 Dy1 C35 159.5(5) . . ? C45 Dy1 C35 165.6(5) . . ? C33 Dy1 C35 49.1(3) . . ? C31 Dy1 C35 31.1(4) . . ? N2 Dy1 C32 103.7(3) . . ? N1 Dy1 C32 156.6(4) . . ? N12 Dy1 C32 119.5(3) . . ? C41 Dy1 C32 89.4(5) . . ? C42 Dy1 C32 75.1(4) . . ? C43 Dy1 C32 94.0(6) . . ? C44 Dy1 C32 121.9(5) . . ? C45 Dy1 C32 119.9(5) . . ? C33 Dy1 C32 30.0(4) . . ? C31 Dy1 C32 29.6(4) . . ? C35 Dy1 C32 49.4(4) . . ? C11 N1 Dy2 140.1(7) . . ? C11 N1 Dy1 94.6(6) . . ? Dy2 N1 Dy1 100.2(3) . . ? N12 C11 N16 125.1(9) . . ? N16 C11 N1 121.3(10) . . ? N12 C11 N1 113.6(9) . . ? C11 N12 C13 116.0(10) . . ? N16 C13 C14 122.7(11) . . ? N16 C13 C131 116.0(12) . . ? C14 C13 C131 121.3(12) . . ? C13 C14 C15 118.8(11) . . ? N12 C15 C14 119.9(11) . . ? N12 C15 C151 118.8(11) . . ? C14 C15 C151 121.3(11) . . ? C15 N12 C11 117.4(9) . . ? C15 N12 Dy1 142.5(7) . . ? C11 N12 Dy1 94.2(6) . . ? N1 Dy2 N22 122.9(3) . . ? N1 Dy2 N2 71.9(3) . . ? N22 Dy2 N2 53.9(3) . . ? N1 Dy2 C65 122.0(4) . . ? N22 Dy2 C65 103.6(3) . . ? N2 Dy2 C65 123.8(3) . . ? N1 Dy2 C55 76.2(3) . . ? N22 Dy2 C55 130.1(4) . . ? N2 Dy2 C55 134.9(3) . . ? C65 Dy2 C55 100.1(4) . . ? N1 Dy2 C53 126.2(3) . . ? N22 Dy2 C53 91.3(4) . . ? N2 Dy2 C53 139.5(4) . . ? C65 Dy2 C53 80.2(4) . . ? C55 Dy2 C53 50.6(4) . . ? N1 Dy2 C51 80.2(3) . . ? N22 Dy2 C51 102.0(3) . . ? N2 Dy2 C51 111.3(3) . . ? C65 Dy2 C51 124.3(4) . . ? C55 Dy2 C51 30.8(4) . . ? C53 Dy2 C51 50.6(4) . . ? N1 Dy2 C61 92.2(4) . . ? N22 Dy2 C61 126.8(3) . . ? N2 Dy2 C61 118.5(4) . . ? C65 Dy2 C61 29.8(4) . . ? C55 Dy2 C61 93.5(4) . . ? C53 Dy2 C61 98.2(5) . . ? C51 Dy2 C61 124.1(4) . . ? N1 Dy2 C54 104.1(4) . . ? N22 Dy2 C54 120.9(4) . . ? N2 Dy2 C54 161.2(3) . . ? C65 Dy2 C54 74.3(4) . . ? C55 Dy2 C54 30.8(4) . . ? C53 Dy2 C54 29.5(4) . . ? C51 Dy2 C54 50.2(4) . . ? C61 Dy2 C54 79.6(5) . . ? N1 Dy2 C64 128.7(3) . . ? N22 Dy2 C64 77.9(3) . . ? N2 Dy2 C64 96.1(3) . . ? C65 Dy2 C64 29.8(4) . . ? C55 Dy2 C64 128.9(4) . . ? C53 Dy2 C64 95.7(4) . . ? C51 Dy2 C64 146.2(4) . . ? C61 Dy2 C64 49.2(4) . . ? C54 Dy2 C64 100.3(4) . . ? N1 Dy2 C52 109.3(4) . . ? N22 Dy2 C52 80.4(4) . . ? N2 Dy2 C52 113.4(3) . . ? C65 Dy2 C52 110.9(4) . . ? C55 Dy2 C52 50.2(4) . . ? C53 Dy2 C52 31.0(4) . . ? C51 Dy2 C52 29.9(4) . . ? C61 Dy2 C52 127.7(5) . . ? C54 Dy2 C52 49.6(4) . . ? C64 Dy2 C52 120.8(4) . . ? N1 Dy2 C62 79.9(3) . . ? N26 Dy2 C62 112.3(4) . . ? N2 Dy2 C62 88.6(4) . . ? C65 Dy2 C62 49.5(4) . . ? C55 Dy2 C62 116.4(4) . . ? C53 Dy2 C62 127.3(4) . . ? C51 Dy2 C62 145.6(4) . . ? C61 Dy2 C62 30.0(4) . . ? C54 Dy2 C62 109.0(4) . . ? C64 Dy2 C62 49.5(4) . . ? C52 Dy2 C62 157.7(4) . . ? C21 N2 Dy1 136.9(6) . . ? C21 N2 Dy2 94.9(6) . . ? Dy1 N2 Dy2 99.3(3) . . ? N2 C21 N22 113.0(8) . . ? N2 C21 N26 121.4(9) . . ? N22 C21 N26 125.5(10) . . ? C21 N26 C23 116.5(9) . . ? N26 C23 C24 120.1(10) . . ? N26 C23 C231 116.5(10) . . ? C24 C23 C231 123.4(11) . . ? C25 C24 C23 120.5(10) . . ? N22 C25 C24 120.1(10) . . ? N22 C25 C251 117.0(10) . . ? C24 C25 C251 122.9(10) . . ? C21 N22 C25 117.3(9) . . ? C21 N22 Dy2 95.6(6) . . ? C25 N22 Dy2 142.9(7) . . ? C32 C31 C35 106.1(10) . . ? C32 C31 Dy1 76.1(6) . . ? C35 C31 Dy1 74.0(6) . . ? C31 C32 C33 108.8(11) . . ? C31 C32 Dy1 74.3(6) . . ? C33 C32 Dy1 73.8(6) . . ? C32 C33 C34 107.7(11) . . ? C32 C33 Dy1 76.2(6) . . ? C34 C33 Dy1 75.1(6) . . ? C35 C34 C33 108.8(12) . . ? C35 C34 Dy1 75.1(7) . . ? C33 C34 Dy1 74.8(6) . . ? C34 C35 C31 108.7(10) . . ? C34 C35 Dy1 75.8(7) . . ? C31 C35 Dy1 74.9(6) . . ? C42 C41 C45 108.3(14) . . ? C42 C41 Dy1 76.1(8) . . ? C45 C41 Dy1 76.1(8) . . ? C41 C42 C43 109.9(16) . . ? C41 C42 Dy1 75.0(8) . . ? C43 C42 Dy1 75.0(8) . . ? C44 C43 C42 106.4(12) . . ? C44 C43 Dy1 76.5(8) . . ? C42 C43 Dy1 74.5(8) . . ? C43 C44 C45 109.5(15) . . ? C43 C44 Dy1 74.1(8) . . ? C45 C44 Dy1 74.6(7) . . ? C41 C45 C44 105.8(15) . . ? C41 C45 Dy1 73.1(8) . . ? C44 C45 Dy1 75.5(8) . . ? C55 C51 C52 108.1(11) . . ? C55 C51 Dy2 74.8(6) . . ? C52 C51 Dy2 74.6(7) . . ? C53 C52 C51 108.9(12) . . ? C53 C52 Dy2 74.1(7) . . ? C51 C52 Dy2 75.5(7) . . ? C52 C53 C54 106.9(11) . . ? C52 C53 Dy2 74.9(7) . . ? C54 C53 Dy2 75.3(7) . . ? C55 C54 C53 110.5(11) . . ? C55 C54 Dy2 75.6(7) . . ? C53 C54 Dy2 75.1(7) . . ? C51 C55 C54 105.5(11) . . ? C51 C55 Dy2 74.4(6) . . ? C54 C55 Dy2 73.6(7) . . ? C65 C61 C62 108.9(11) . . ? C65 C61 Dy2 75.0(6) . . ? C62 C61 Dy2 76.5(6) . . ? C63 C62 C61 107.5(12) . . ? C63 C62 Dy2 76.3(7) . . ? C61 C62 Dy2 73.5(6) . . ? C62 C63 C64 107.2(12) . . ? C62 C63 Dy2 73.9(7) . . ? C64 C63 Dy2 73.6(7) . . ? C65 C64 C63 107.9(11) . . ? C65 C64 Dy2 73.6(7) . . ? C63 C64 Dy2 76.3(7) . . ? C61 C65 C64 108.5(12) . . ? C61 C65 Dy2 75.2(7) . . ? C64 C65 Dy2 76.6(7) . . ? C2T C1T C6T 123(2) . . ? C3T C2T C1T 121(2) . . ? C4T C3T C2T 120(2) . . ? C3T C4T C5T 121(2) . . ? C4T C5T C6T 119.6(15) . . ? C5T C6T C7T 123(2) . . ? C5T C6T C1T 115.0(15) . . ? C7T C6T C1T 122(2) . . ? C6S C1S C2S 129(4) . . ? C1S C2S C3S 110(4) . . ? C4S C3S C2S 104(5) . . ? C3S C4S C5S 162(10) . . ? C4S C5S C6S 97(5) . . ? C1S C6S C7S 134(4) . . ? C1S C6S C5S 117(3) . . ? C7S C6S C5S 108(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.005 _refine_diff_density_min -1.467 _refine_diff_density_rms 0.134 # Attachment '5.cif' data_ix476 _database_code_depnum_ccdc_archive 'CCDC 286300' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H41 N6 O3 Yb3' _chemical_formula_weight 1136.88 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.383(5) _cell_length_b 17.295(8) _cell_length_c 18.602(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3662(3) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour amber _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2156 _exptl_absorpt_coefficient_mu 7.642 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details psi-scans _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 P4' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2922 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 21.00 _reflns_number_total 2735 _reflns_number_gt 2145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(7) _refine_ls_number_reflns 2735 _refine_ls_number_parameters 401 _refine_ls_number_restraints 276 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1908 _refine_ls_wR_factor_gt 0.1761 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 0.965 _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 Yb1 Yb -0.20299(12) -0.06074(8) 0.41753(7) 0.0276(4) Uani 1 1 d . . . Yb2 Yb 0.01640(11) -0.01892(9) 0.54509(7) 0.0279(4) Uani 1 1 d . . . Yb3 Yb -0.04282(14) 0.10174(9) 0.36561(7) 0.0357(4) Uani 1 1 d . . . O1 O -0.0610(17) 0.0140(11) 0.4473(10) 0.030(4) Uani 1 1 d U . . N1 N -0.234(2) 0.0494(15) 0.3382(13) 0.042(8) Uani 1 1 d . . . H1 H -0.2472 0.0376 0.2902 0.050 Uiso 1 1 calc R . . C11 C -0.331(3) 0.0759(17) 0.3767(16) 0.028(7) Uani 1 1 d U . . N12 N -0.411(2) 0.1181(16) 0.3410(12) 0.037(8) Uani 1 1 d . . . C13 C -0.497(3) 0.1432(19) 0.3826(18) 0.038(7) Uani 1 1 d U . . C14 C -0.513(3) 0.1248(18) 0.4562(17) 0.041(7) Uani 1 1 d U . . H14 H -0.5771 0.1447 0.4835 0.050 Uiso 1 1 calc R . . C15 C -0.431(3) 0.076(2) 0.4853(18) 0.045(8) Uani 1 1 d U . . N16 N -0.345(3) 0.0466(18) 0.4478(17) 0.063(7) Uani 1 1 d U . . O131 O -0.591(2) 0.1892(13) 0.3580(10) 0.042(7) Uani 1 1 d . . . C132 C -0.577(4) 0.210(2) 0.2877(18) 0.056(8) Uani 1 1 d U . . H13A H -0.4927 0.2136 0.2765 0.084 Uiso 1 1 calc R . . H13B H -0.6134 0.2609 0.2798 0.084 Uiso 1 1 calc R . . H13C H -0.6138 0.1718 0.2565 0.084 Uiso 1 1 calc R . . C151 C -0.432(3) 0.058(2) 0.5593(16) 0.051(8) Uani 1 1 d U . . H15A H -0.3793 0.0144 0.5683 0.076 Uiso 1 1 calc R . . H15B H -0.5124 0.0437 0.5737 0.076 Uiso 1 1 calc R . . H15C H -0.4066 0.1029 0.5872 0.076 Uiso 1 1 calc R . . N2 N -0.095(2) -0.1328(15) 0.5141(13) 0.037(6) Uani 1 1 d U . . H2 H -0.0469 -0.1707 0.4945 0.044 Uiso 1 1 calc R . . C21 C -0.190(2) -0.1644(15) 0.5461(15) 0.020(6) Uani 1 1 d U . . N22 N -0.188(2) -0.2182(14) 0.5976(13) 0.033(6) Uani 1 1 d U . . C23 C -0.302(3) -0.2454(18) 0.6154(16) 0.030(7) Uani 1 1 d U . . C24 C -0.400(3) -0.2152(16) 0.5855(18) 0.037(10) Uani 1 1 d . . . H24 H -0.4744 -0.2350 0.5998 0.045 Uiso 1 1 calc R . . C25 C -0.397(3) -0.162(2) 0.5398(19) 0.040(7) Uani 1 1 d U . . N26 N -0.297(2) -0.1287(15) 0.5162(14) 0.037(6) Uani 1 1 d U . . O231 O -0.309(3) -0.3002(14) 0.6654(13) 0.061(8) Uani 1 1 d . . . C232 C -0.194(3) -0.328(2) 0.6957(19) 0.051(8) Uani 1 1 d U . . H23A H -0.1562 -0.3624 0.6612 0.077 Uiso 1 1 calc R . . H23B H -0.2089 -0.3557 0.7407 0.077 Uiso 1 1 calc R . . H23C H -0.1433 -0.2834 0.7052 0.077 Uiso 1 1 calc R . . C251 C -0.510(4) -0.129(2) 0.512(2) 0.072(9) Uani 1 1 d U . . H25A H -0.5726 -0.1681 0.5162 0.108 Uiso 1 1 calc R . . H25B H -0.5010 -0.1143 0.4616 0.108 Uiso 1 1 calc R . . H25C H -0.5317 -0.0835 0.5405 0.108 Uiso 1 1 calc R . . C31 C -0.3264(15) -0.1818(11) 0.3656(9) 0.035(7) Uani 1 1 d GU . . H31 H -0.3915 -0.2011 0.3920 0.042 Uiso 1 1 calc R . . C32 C -0.2078(16) -0.2058(11) 0.3732(10) 0.022(6) Uani 1 1 d GU . . H32 H -0.1796 -0.2440 0.4056 0.026 Uiso 1 1 calc R . . C33 C -0.1386(15) -0.1626(14) 0.3240(12) 0.030(7) Uani 1 1 d GU . . H33 H -0.0561 -0.1669 0.3176 0.036 Uiso 1 1 calc R . . C34 C -0.215(2) -0.1119(13) 0.2859(11) 0.065(9) Uani 1 1 d GU . . H34 H -0.1917 -0.0764 0.2496 0.078 Uiso 1 1 calc R . . C35 C -0.3306(18) -0.1238(12) 0.3116(11) 0.040(7) Uani 1 1 d GU . . H35 H -0.3991 -0.0975 0.2956 0.048 Uiso 1 1 calc R . . C41 C 0.160(2) 0.0507(16) 0.3056(12) 0.062(7) Uani 1 1 d GU . . H41 H 0.2240 0.0390 0.3365 0.074 Uiso 1 1 calc R . . C42 C 0.135(3) 0.1241(14) 0.2752(16) 0.072(7) Uani 1 1 d GU . . H42 H 0.1785 0.1701 0.2822 0.087 Uiso 1 1 calc R . . C43 C 0.032(3) 0.1165(18) 0.2325(16) 0.093(7) Uani 1 1 d GU . . H43 H -0.0051 0.1567 0.2059 0.112 Uiso 1 1 calc R . . C44 C -0.006(2) 0.038(2) 0.2366(15) 0.081(7) Uani 1 1 d GU . . H44 H -0.0731 0.0172 0.2131 0.097 Uiso 1 1 calc R . . C45 C 0.073(3) -0.0022(14) 0.2818(16) 0.084(7) Uani 1 1 d GU . . H45 H 0.0685 -0.0555 0.2939 0.101 Uiso 1 1 calc R . . C51 C -0.1174(17) 0.0787(10) 0.6149(10) 0.026(7) Uani 1 1 d GU . . H51 H -0.1589 0.1151 0.5863 0.031 Uiso 1 1 calc R . . C52 C -0.1579(18) 0.0040(11) 0.6348(12) 0.050(8) Uani 1 1 d GU . . H52 H -0.2313 -0.0182 0.6219 0.061 Uiso 1 1 calc R . . C53 C -0.070(2) -0.0315(11) 0.6773(13) 0.043(7) Uani 1 1 d GU . . H53 H -0.0734 -0.0817 0.6979 0.051 Uiso 1 1 calc R . . C54 C 0.026(2) 0.0211(15) 0.6837(13) 0.069(8) Uani 1 1 d GU . . H54 H 0.0966 0.0123 0.7093 0.083 Uiso 1 1 calc R . . C55 C -0.0040(18) 0.0892(12) 0.6451(12) 0.048(8) Uani 1 1 d GU . . H55 H 0.0438 0.1340 0.6403 0.058 Uiso 1 1 calc R . . C61 C 0.1882(15) -0.1179(9) 0.5274(10) 0.037(7) Uani 1 1 d GU . . H61 H 0.1657 -0.1708 0.5256 0.044 Uiso 1 1 calc R . . C62 C 0.221(2) -0.0765(12) 0.5901(9) 0.047(8) Uani 1 1 d GU . . H62 H 0.2251 -0.0968 0.6376 0.057 Uiso 1 1 calc R . . C63 C 0.248(2) 0.0005(11) 0.5695(12) 0.065(9) Uani 1 1 d GU . . H63 H 0.2732 0.0408 0.6007 0.078 Uiso 1 1 calc R . . C64 C 0.232(2) 0.0067(10) 0.4941(12) 0.043(7) Uani 1 1 d GU . . H64 H 0.2436 0.0519 0.4659 0.052 Uiso 1 1 calc R . . C65 C 0.195(2) -0.0665(11) 0.4681(9) 0.026(6) Uani 1 1 d GU . . H65 H 0.1771 -0.0789 0.4195 0.031 Uiso 1 1 calc R . . C71 C -0.010(3) 0.2022(13) 0.4664(13) 0.086(9) Uani 1 1 d GU . . H71 H 0.0284 0.1830 0.5081 0.104 Uiso 1 1 calc R . . C72 C 0.047(3) 0.2322(17) 0.4042(16) 0.063(8) Uani 1 1 d GU . . H72 H 0.1289 0.2366 0.3971 0.076 Uiso 1 1 calc R . . C73 C -0.042(4) 0.2544(16) 0.3545(13) 0.107(10) Uani 1 1 d GU . . H73 H -0.0292 0.2763 0.3083 0.128 Uiso 1 1 calc R . . C74 C -0.153(3) 0.2382(19) 0.3860(18) 0.098(10) Uani 1 1 d GU . . H74 H -0.2274 0.2473 0.3645 0.117 Uiso 1 1 calc R . . C75 C -0.133(2) 0.2059(17) 0.4551(16) 0.077(9) Uani 1 1 d GU . . H75 H -0.1918 0.1896 0.4880 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.0250(8) 0.0334(7) 0.0243(7) 0.0035(8) -0.0065(7) 0.0035(8) Yb2 0.0203(7) 0.0435(8) 0.0198(7) -0.0003(7) -0.0007(6) -0.0003(7) Yb3 0.0376(9) 0.0428(9) 0.0266(8) 0.0079(8) 0.0028(8) -0.0046(9) O1 0.032(5) 0.028(5) 0.030(5) 0.003(4) 0.000(4) 0.004(4) N1 0.052(18) 0.043(17) 0.030(14) -0.029(14) -0.014(15) -0.003(16) C11 0.027(9) 0.028(10) 0.028(10) -0.004(8) -0.006(8) -0.002(7) N12 0.044(17) 0.054(18) 0.012(12) 0.018(14) -0.010(14) -0.021(16) C13 0.035(10) 0.038(10) 0.042(10) -0.001(8) -0.001(8) -0.007(8) C14 0.040(10) 0.044(10) 0.040(10) -0.002(8) -0.005(8) 0.003(8) C15 0.044(10) 0.046(10) 0.045(10) 0.001(8) -0.002(8) 0.002(8) N16 0.064(10) 0.060(10) 0.066(10) 0.005(8) 0.001(8) 0.001(8) O131 0.039(14) 0.068(16) 0.019(11) -0.015(12) -0.013(11) 0.022(14) C132 0.057(11) 0.057(11) 0.054(11) -0.002(8) -0.006(8) 0.001(8) C151 0.050(10) 0.054(10) 0.048(10) -0.003(8) -0.005(8) 0.006(8) N2 0.029(9) 0.040(9) 0.040(9) -0.010(7) -0.001(7) -0.004(7) C21 0.017(9) 0.018(9) 0.025(9) 0.005(7) -0.005(8) -0.005(7) N22 0.032(9) 0.036(9) 0.031(9) 0.001(7) 0.001(7) -0.003(7) C23 0.038(10) 0.030(9) 0.023(9) 0.000(7) 0.002(8) -0.005(8) C24 0.05(2) 0.019(17) 0.040(19) -0.019(18) -0.02(2) 0.008(17) C25 0.038(10) 0.043(10) 0.039(10) 0.001(8) -0.002(8) -0.002(8) N26 0.030(9) 0.041(9) 0.039(9) -0.001(7) 0.002(7) 0.000(7) O231 0.069(19) 0.065(17) 0.050(15) -0.014(15) 0.006(16) -0.020(17) C232 0.051(10) 0.052(10) 0.051(11) 0.004(8) -0.003(8) -0.004(8) C251 0.069(11) 0.074(11) 0.074(12) 0.002(8) -0.005(8) 0.001(8) C31 0.035(10) 0.039(10) 0.033(10) -0.007(8) -0.009(8) -0.003(8) C32 0.021(9) 0.023(9) 0.022(9) -0.002(7) -0.003(8) -0.004(7) C33 0.034(10) 0.031(10) 0.024(9) 0.005(7) -0.005(8) 0.002(8) C34 0.064(11) 0.063(11) 0.068(11) -0.004(8) 0.001(8) -0.001(8) C35 0.042(10) 0.039(10) 0.039(10) -0.008(8) -0.010(8) -0.003(8) C41 0.061(8) 0.065(8) 0.058(9) 0.000(6) 0.003(6) 0.000(6) C42 0.071(8) 0.072(9) 0.073(9) -0.001(6) 0.001(6) -0.001(6) C43 0.096(9) 0.095(9) 0.089(9) 0.003(6) 0.003(6) 0.001(6) C44 0.080(9) 0.084(9) 0.079(9) -0.005(6) 0.000(6) -0.002(6) C45 0.085(9) 0.084(9) 0.082(9) 0.002(6) 0.004(6) -0.001(6) C51 0.026(9) 0.026(10) 0.025(9) -0.007(7) 0.004(7) 0.006(7) C52 0.050(10) 0.053(11) 0.048(11) -0.004(8) 0.000(8) 0.002(8) C53 0.045(10) 0.043(10) 0.040(10) -0.005(8) 0.012(8) 0.002(8) C54 0.066(11) 0.073(11) 0.067(11) -0.008(8) -0.002(8) 0.003(8) C55 0.052(10) 0.046(10) 0.046(10) -0.002(8) 0.004(8) 0.000(8) C61 0.031(10) 0.037(10) 0.042(10) -0.009(8) 0.005(8) 0.003(8) C62 0.044(10) 0.052(10) 0.045(10) 0.001(8) -0.003(8) 0.006(8) C63 0.063(11) 0.070(11) 0.063(11) -0.004(8) -0.004(8) -0.002(8) C64 0.044(10) 0.050(10) 0.036(10) -0.001(8) 0.004(8) 0.003(8) C65 0.025(9) 0.029(9) 0.024(9) -0.003(8) 0.000(7) 0.003(8) C71 0.089(12) 0.083(12) 0.087(12) 0.000(8) -0.002(8) 0.005(8) C72 0.066(11) 0.059(11) 0.064(11) -0.004(8) 0.003(8) -0.008(8) C73 0.106(12) 0.105(12) 0.109(13) 0.004(8) 0.005(8) -0.002(8) C74 0.096(12) 0.097(12) 0.101(13) -0.001(8) -0.002(8) 0.003(8) C75 0.080(11) 0.077(11) 0.075(12) 0.002(8) 0.004(8) -0.001(8) _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 Yb1 O1 2.143(19) . ? Yb1 N1 2.43(3) . ? Yb1 N26 2.43(3) . ? Yb1 N16 2.53(3) . ? Yb1 N2 2.51(3) . ? Yb1 C33 2.58(2) . ? Yb1 C34 2.61(2) . ? Yb1 C32 2.64(2) . ? Yb1 C35 2.68(2) . ? Yb1 C31 2.700(18) . ? Yb2 O1 2.100(19) . ? Yb2 N2 2.41(3) . ? Yb2 C65 2.62(2) . ? Yb2 C52 2.62(2) . ? Yb2 C61 2.620(17) . ? Yb2 C51 2.618(19) . ? Yb2 C53 2.66(2) . ? Yb2 C64 2.67(2) . ? Yb2 C55 2.65(2) . ? Yb2 C54 2.67(3) . ? Yb2 C62 2.67(2) . ? Yb2 C63 2.70(2) . ? Yb3 O1 2.157(19) . ? Yb3 N1 2.41(3) . ? Yb3 C72 2.58(3) . ? Yb3 C71 2.58(2) . ? Yb3 C73 2.65(3) . ? Yb3 C75 2.66(3) . ? Yb3 C43 2.63(3) . ? Yb3 C74 2.70(3) . ? Yb3 C42 2.66(3) . ? Yb3 C44 2.67(3) . ? Yb3 C41 2.71(2) . ? Yb3 C45 2.72(3) . ? N1 C11 1.40(4) . ? C11 N12 1.34(4) . ? C11 N16 1.43(4) . ? N12 C13 1.32(4) . ? C13 O131 1.41(4) . ? C13 C14 1.42(4) . ? C14 C15 1.37(4) . ? C15 N16 1.31(4) . ? C15 C151 1.41(4) . ? O131 C132 1.37(4) . ? N2 C21 1.35(4) . ? C21 N22 1.34(4) . ? C21 N26 1.47(4) . ? N22 C23 1.42(4) . ? C23 C24 1.35(5) . ? C23 O231 1.33(4) . ? C24 C25 1.25(4) . ? C25 N26 1.35(4) . ? C25 C251 1.51(5) . ? O231 C232 1.50(4) . ? C31 C32 1.4200 . ? C31 C35 1.4200 . ? C32 C33 1.4200 . ? C33 C34 1.4200 . ? C34 C35 1.4200 . ? C41 C42 1.4200 . ? C41 C45 1.4200 . ? C42 C43 1.4200 . ? C43 C44 1.4200 . ? C44 C45 1.4200 . ? C51 C52 1.4200 . ? C51 C55 1.4200 . ? C52 C53 1.4200 . ? C53 C54 1.4200 . ? C54 C55 1.4200 . ? C61 C62 1.4200 . ? C61 C65 1.4200 . ? C62 C63 1.4200 . ? C63 C64 1.4200 . ? C64 C65 1.4200 . ? C71 C75 1.4200 . ? C71 C72 1.4200 . ? C72 C73 1.4200 . ? C73 C74 1.4200 . ? C74 C75 1.4200 . ? 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 O1 Yb1 N1 78.0(8) . . ? O1 Yb1 N26 115.4(8) . . ? N1 Yb1 N26 140.8(9) . . ? O1 Yb1 N16 89.0(9) . . ? N1 Yb1 N16 57.9(9) . . ? N26 Yb1 N16 84.6(9) . . ? O1 Yb1 N2 75.3(8) . . ? N1 Yb1 N2 153.3(8) . . ? N26 Yb1 N2 55.4(8) . . ? N16 Yb1 N2 121.3(9) . . ? O1 Yb1 C33 111.8(6) . . ? N1 Yb1 C33 99.6(8) . . ? N26 Yb1 C33 107.7(8) . . ? N16 Yb1 C33 146.4(9) . . ? N2 Yb1 C33 90.3(8) . . ? O1 Yb1 C34 119.1(7) . . ? N1 Yb1 C34 71.9(7) . . ? N26 Yb1 C34 121.6(7) . . ? N16 Yb1 C34 115.2(9) . . ? N2 Yb1 C34 121.9(8) . . ? C33 Yb1 C34 31.8(3) . . ? O1 Yb1 C32 132.0(6) . . ? N1 Yb1 C32 123.4(7) . . ? N26 Yb1 C32 76.5(7) . . ? N16 Yb1 C32 138.9(8) . . ? N2 Yb1 C32 76.2(7) . . ? C33 Yb1 C32 31.5(2) . . ? C34 Yb1 C32 51.9(3) . . ? O1 Yb1 C35 147.6(7) . . ? N1 Yb1 C35 78.2(7) . . ? N26 Yb1 C35 96.9(8) . . ? N16 Yb1 C35 96.6(8) . . ? N2 Yb1 C35 126.2(7) . . ? C33 Yb1 C35 51.7(3) . . ? C34 Yb1 C35 31.1(2) . . ? C32 Yb1 C35 51.2(3) . . ? O1 Yb1 C31 162.4(6) . . ? N1 Yb1 C31 108.4(7) . . ? N26 Yb1 C31 70.5(7) . . ? N16 Yb1 C31 108.4(8) . . ? N2 Yb1 C31 97.2(7) . . ? C33 Yb1 C31 51.5(3) . . ? C34 Yb1 C31 51.3(3) . . ? C32 Yb1 C31 30.81(19) . . ? C35 Yb1 C31 30.6(2) . . ? O1 Yb2 N2 78.1(8) . . ? O1 Yb2 C65 86.4(6) . . ? N2 Yb2 C65 91.2(7) . . ? O1 Yb2 C52 101.1(7) . . ? N2 Yb2 C52 83.0(7) . . ? C65 Yb2 C52 169.3(6) . . ? O1 Yb2 C61 112.5(7) . . ? N2 Yb2 C61 80.2(7) . . ? C65 Yb2 C61 31.5(2) . . ? C52 Yb2 C61 138.0(6) . . ? O1 Yb2 C51 90.6(6) . . ? N2 Yb2 C51 109.8(8) . . ? C65 Yb2 C51 157.7(6) . . ? C52 Yb2 C51 31.4(2) . . ? C61 Yb2 C51 156.6(6) . . ? O1 Yb2 C53 132.1(8) . . ? N2 Yb2 C53 87.7(8) . . ? C65 Yb2 C53 140.1(6) . . ? C52 Yb2 C53 31.2(3) . . ? C61 Yb2 C53 109.7(6) . . ? C51 Yb2 C53 51.6(3) . . ? O1 Yb2 C64 91.9(7) . . ? N2 Yb2 C64 122.3(8) . . ? C65 Yb2 C64 31.2(2) . . ? C52 Yb2 C64 153.8(6) . . ? C61 Yb2 C64 51.5(3) . . ? C51 Yb2 C64 127.2(6) . . ? C53 Yb2 C64 133.0(8) . . ? O1 Yb2 C55 112.3(7) . . ? N2 Yb2 C55 134.3(7) . . ? C65 Yb2 C55 132.4(6) . . ? C52 Yb2 C55 51.7(3) . . ? C61 Yb2 C55 127.9(6) . . ? C51 Yb2 C55 31.3(2) . . ? C53 Yb2 C55 51.3(4) . . ? C64 Yb2 C55 102.3(6) . . ? O1 Yb2 C54 141.4(7) . . ? N2 Yb2 C54 117.6(8) . . ? C65 Yb2 C54 125.4(6) . . ? C52 Yb2 C54 51.4(3) . . ? C61 Yb2 C54 105.1(6) . . ? C51 Yb2 C54 51.5(3) . . ? C53 Yb2 C54 30.9(3) . . ? C64 Yb2 C54 105.3(7) . . ? C55 Yb2 C54 31.0(3) . . ? O1 Yb2 C62 137.7(7) . . ? N2 Yb2 C62 103.3(8) . . ? C65 Yb2 C62 51.5(3) . . ? C52 Yb2 C62 121.2(6) . . ? C61 Yb2 C62 31.1(2) . . ? C51 Yb2 C62 126.4(6) . . ? C53 Yb2 C62 90.0(7) . . ? C64 Yb2 C62 51.0(3) . . ? C55 Yb2 C62 96.9(6) . . ? C54 Yb2 C62 76.1(6) . . ? O1 Yb2 C63 121.5(7) . . ? N2 Yb2 C63 131.0(7) . . ? C65 Yb2 C63 51.2(3) . . ? C52 Yb2 C63 127.9(6) . . ? C61 Yb2 C63 51.1(3) . . ? C51 Yb2 C63 113.9(6) . . ? C53 Yb2 C63 102.4(8) . . ? C64 Yb2 C63 30.7(2) . . ? C55 Yb2 C63 83.1(6) . . ? C54 Yb2 C63 76.5(7) . . ? C62 Yb2 C63 30.6(3) . . ? O1 Yb3 N1 78.3(8) . . ? O1 Yb3 C72 117.2(8) . . ? N1 Yb3 C72 138.1(9) . . ? O1 Yb3 C71 88.6(7) . . ? N1 Yb3 C71 122.5(9) . . ? C72 Yb3 C71 31.9(3) . . ? O1 Yb3 C73 139.1(7) . . ? N1 Yb3 C73 111.2(11) . . ? C72 Yb3 C73 31.5(3) . . ? C71 Yb3 C73 52.1(4) . . ? O1 Yb3 C75 89.9(8) . . ? N1 Yb3 C75 92.2(9) . . ? C72 Yb3 C75 52.0(3) . . ? C71 Yb3 C75 31.4(3) . . ? C73 Yb3 C75 51.3(4) . . ? O1 Yb3 C43 139.7(8) . . ? N1 Yb3 C43 97.4(9) . . ? C72 Yb3 C43 92.8(10) . . ? C71 Yb3 C43 124.8(10) . . ? C73 Yb3 C43 80.1(9) . . ? C75 Yb3 C43 130.4(9) . . ? O1 Yb3 C74 118.1(9) . . ? N1 Yb3 C74 86.5(9) . . ? C72 Yb3 C74 51.6(4) . . ? C71 Yb3 C74 51.5(4) . . ? C73 Yb3 C74 30.8(3) . . ? C75 Yb3 C74 30.7(3) . . ? C43 Yb3 C74 101.4(10) . . ? O1 Yb3 C42 128.4(8) . . ? N1 Yb3 C42 127.3(9) . . ? C72 Yb3 C42 75.5(8) . . ? C71 Yb3 C42 104.5(9) . . ? C73 Yb3 C42 78.6(10) . . ? C75 Yb3 C42 126.3(8) . . ? C43 Yb3 C42 31.2(3) . . ? C74 Yb3 C42 108.3(10) . . ? O1 Yb3 C44 111.1(9) . . ? N1 Yb3 C44 78.2(8) . . ? C72 Yb3 C44 123.2(9) . . ? C71 Yb3 C44 154.8(9) . . ? C73 Yb3 C44 109.7(9) . . ? C75 Yb3 C44 154.2(10) . . ? C43 Yb3 C44 31.1(3) . . ? C74 Yb3 C44 123.8(10) . . ? C42 Yb3 C44 51.1(4) . . ? O1 Yb3 C41 98.2(8) . . ? N1 Yb3 C41 123.9(8) . . ? C72 Yb3 C41 93.7(9) . . ? C71 Yb3 C41 113.2(9) . . ? C73 Yb3 C41 106.8(10) . . ? C75 Yb3 C41 143.8(8) . . ? C43 Yb3 C41 50.9(4) . . ? C74 Yb3 C41 137.6(10) . . ? C42 Yb3 C41 30.7(3) . . ? C44 Yb3 C41 50.5(4) . . ? O1 Yb3 C45 89.2(8) . . ? N1 Yb3 C45 93.8(8) . . ? C72 Yb3 C45 123.2(8) . . ? C71 Yb3 C45 142.2(9) . . ? C73 Yb3 C45 127.8(9) . . ? C75 Yb3 C45 173.5(9) . . ? C43 Yb3 C45 50.8(4) . . ? C74 Yb3 C45 152.0(10) . . ? C42 Yb3 C45 50.6(4) . . ? C44 Yb3 C45 30.5(3) . . ? C41 Yb3 C45 30.3(3) . . ? Yb2 O1 Yb1 112.1(8) . . ? Yb2 O1 Yb3 139.5(10) . . ? Yb1 O1 Yb3 108.4(8) . . ? C11 N1 Yb3 118.9(18) . . ? C11 N1 Yb1 93.5(18) . . ? Yb3 N1 Yb1 92.1(9) . . ? N12 C11 N1 118(3) . . ? N12 C11 N16 125(3) . . ? N1 C11 N16 117(3) . . ? C11 N12 C13 113(3) . . ? N12 C13 O131 124(3) . . ? N12 C13 C14 126(3) . . ? O131 C13 C14 110(3) . . ? C15 C14 C13 115(3) . . ? N16 C15 C14 123(3) . . ? N16 C15 C151 116(3) . . ? C14 C15 C151 121(3) . . ? C15 N16 C11 116(3) . . ? C15 N16 Yb1 153(3) . . ? C11 N16 Yb1 89(2) . . ? C13 O131 C132 112(3) . . ? C21 N2 Yb2 130(2) . . ? C21 N2 Yb1 97.1(17) . . ? Yb2 N2 Yb1 91.4(9) . . ? N22 C21 N2 125(3) . . ? N22 C21 N26 126(3) . . ? N2 C21 N26 109(2) . . ? C21 N22 C23 112(3) . . ? C24 C23 O231 121(3) . . ? C24 C23 N22 122(3) . . ? O231 C23 N22 117(3) . . ? C25 C24 C23 122(4) . . ? C24 C25 N26 124(3) . . ? C24 C25 C251 119(3) . . ? N26 C25 C251 117(3) . . ? C25 N26 C21 113(2) . . ? C25 N26 Yb1 145(2) . . ? C21 N26 Yb1 97.3(17) . . ? C23 O231 C232 116(3) . . ? C32 C31 C35 108.0 . . ? C32 C31 Yb1 72.3(7) . . ? C35 C31 Yb1 73.9(7) . . ? C31 C32 C33 108.0 . . ? C31 C32 Yb1 76.9(7) . . ? C33 C32 Yb1 72.0(7) . . ? C34 C33 C32 108.0 . . ? C34 C33 Yb1 75.1(8) . . ? C32 C33 Yb1 76.5(7) . . ? C33 C34 C35 108.0 . . ? C33 C34 Yb1 73.2(8) . . ? C35 C34 Yb1 77.3(7) . . ? C34 C35 C31 108.0 . . ? C34 C35 Yb1 71.6(7) . . ? C31 C35 Yb1 75.5(7) . . ? C42 C41 C45 108.0 . . ? C42 C41 Yb3 72.5(11) . . ? C45 C41 Yb3 75.2(10) . . ? C43 C42 C41 108.0 . . ? C43 C42 Yb3 73.4(9) . . ? C41 C42 Yb3 76.9(11) . . ? C42 C43 C44 108.0 . . ? C42 C43 Yb3 75.4(9) . . ? C44 C43 Yb3 76.1(11) . . ? C43 C44 C45 108.0 . . ? C43 C44 Yb3 72.9(11) . . ? C45 C44 Yb3 76.7(10) . . ? C44 C45 C41 108.0 . . ? C44 C45 Yb3 72.8(9) . . ? C41 C45 Yb3 74.5(10) . . ? C52 C51 C55 108.0 . . ? C52 C51 Yb2 74.5(8) . . ? C55 C51 Yb2 75.5(9) . . ? C53 C52 C51 108.0 . . ? C53 C52 Yb2 75.7(8) . . ? C51 C52 Yb2 74.1(7) . . ? C52 C53 C54 108.0 . . ? C52 C53 Yb2 73.1(8) . . ? C54 C53 Yb2 75.1(8) . . ? C55 C54 C53 108.0 . . ? C55 C54 Yb2 73.6(7) . . ? C53 C54 Yb2 74.0(8) . . ? C54 C55 C51 108.0 . . ? C54 C55 Yb2 75.4(8) . . ? C51 C55 Yb2 73.2(8) . . ? C62 C61 C65 108.0 . . ? C62 C61 Yb2 76.5(9) . . ? C65 C61 Yb2 74.1(8) . . ? C61 C62 C63 108.0 . . ? C61 C62 Yb2 72.4(8) . . ? C63 C62 Yb2 75.8(7) . . ? C64 C63 C62 108.0 . . ? C64 C63 Yb2 73.3(8) . . ? C62 C63 Yb2 73.6(7) . . ? C65 C64 C63 108.0 . . ? C65 C64 Yb2 72.5(7) . . ? C63 C64 Yb2 76.0(9) . . ? C64 C65 C61 108.0 . . ? C64 C65 Yb2 76.4(7) . . ? C61 C65 Yb2 74.4(8) . . ? C75 C71 C72 108.0 . . ? C75 C71 Yb3 77.2(12) . . ? C72 C71 Yb3 73.8(10) . . ? C73 C72 C71 108.0 . . ? C73 C72 Yb3 77.0(11) . . ? C71 C72 Yb3 74.3(10) . . ? C72 C73 C74 108.0 . . ? C72 C73 Yb3 71.5(10) . . ? C74 C73 Yb3 76.5(12) . . ? C75 C74 C73 108.0 . . ? C75 C74 Yb3 73.1(9) . . ? C73 C74 Yb3 72.7(11) . . ? C74 C75 C71 108.0 . . ? C74 C75 Yb3 76.2(9) . . ? C71 C75 Yb3 71.4(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.766 _refine_diff_density_min -2.436 _refine_diff_density_rms 0.331