# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1568 data_global _publ_requested_journal 'J. Chem. Soc., Dalton Trans' _publ_contact_author_name 'Wai-Kwok Wong' _publ_contact_author_address ; Department of Chemistry Hong Kong Baptist University Kowloon, Hong Kong ; _publ_contact_author_email 'wkwong@sci.hkbu.edu.hk' _publ_section_title ; Synthesis, characterization and crystal structures of neutral mono- and dinuclear lanthanide(III) porphyrinate complexes ; #----------------------------------------------------------------------------- data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H50 Cl N4 O3 Y' _chemical_formula_weight 927.34 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 '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)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.276(1) _cell_length_b 28.313(2) _cell_length_c 13.846(1) _cell_angle_alpha 90.00 _cell_angle_beta 109.43(1) _cell_angle_gamma 90.00 _cell_volume 5647.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used '105 from 4 still frames' _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 1.120 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.934 _exptl_absorpt_correction_T_max 1.071 _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 ; Rigaku RU-200 rotating anode generator powered at 50kV / 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS IIc' _diffrn_measurement_method ; Data was collected to 0.82\%A with 80% completeness by taking 44 oscillation photos in the range of 0 - 180\%, \D\f = 6\% for \f = 0 - 84\% and 168 - 180\%, \D\f = 3\% for \f = 84 - 168\%. Crystal to detector distance is 78.086mm, background level -40. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8138 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.53 _reflns_number_total 8138 _reflns_number_gt 6262 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BioteX 1.0 (MSC, 1995)' _computing_cell_refinement 'BioteX 1.0 (MSC, 1995)' _computing_data_reduction 'BioteX 1.0 (MSC, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PC (Siemens, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1080P)^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 SHELXL _refine_ls_extinction_coef 0.0038(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8138 _refine_ls_number_parameters 569 _refine_ls_number_restraints 413 _refine_ls_R_factor_all 0.1177 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.2297 _refine_ls_wR_factor_gt 0.2098 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.058 _refine_ls_shift/su_mean 0.004 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.53805(3) 0.69736(2) 0.41782(3) 0.05137(15) Uani 1 1 d . . . Cl1 Cl 0.40739(11) 0.65620(7) 0.26205(11) 0.0781(5) Uani 1 1 d . . . N1 N 0.4209(3) 0.74139(16) 0.4542(3) 0.0538(11) Uani 1 1 d DU . . N2 N 0.6117(3) 0.77056(16) 0.4901(3) 0.0557(11) Uani 1 1 d DU . . N3 N 0.6736(3) 0.67708(16) 0.5614(3) 0.0525(10) Uani 1 1 d DU . . N4 N 0.4821(3) 0.64672(16) 0.5215(3) 0.0519(10) Uani 1 1 d DU . . C1 C 0.3353(4) 0.7216(2) 0.4417(4) 0.0607(13) Uani 1 1 d DU . . C2 C 0.2651(4) 0.7580(2) 0.4163(5) 0.0724(16) Uani 1 1 d DU . . H2 H 0.2016 0.7536 0.4011 0.087 Uiso 1 1 calc R . . C3 C 0.3092(4) 0.7994(2) 0.4188(5) 0.0733(16) Uani 1 1 d DU . . H3 H 0.2816 0.8291 0.4072 0.088 Uiso 1 1 calc R . . C4 C 0.4069(4) 0.7894(2) 0.4428(4) 0.0585(13) Uani 1 1 d DU . . C5 C 0.4758(4) 0.8244(2) 0.4517(4) 0.0590(13) Uani 1 1 d U . . C6 C 0.5710(4) 0.8146(2) 0.4749(4) 0.0600(14) Uani 1 1 d DU . . C7 C 0.6426(4) 0.8508(2) 0.4933(5) 0.0748(16) Uani 1 1 d DU . . H7 H 0.6333 0.8833 0.4887 0.090 Uiso 1 1 calc R . . C8 C 0.7252(4) 0.8281(2) 0.5182(5) 0.0713(16) Uani 1 1 d DU . . H8 H 0.7832 0.8421 0.5329 0.086 Uiso 1 1 calc R . . C9 C 0.7063(4) 0.7782(2) 0.5176(4) 0.0588(13) Uani 1 1 d DU . . C10 C 0.7749(4) 0.7435(2) 0.5494(4) 0.0609(13) Uani 1 1 d U . . C11 C 0.7601(4) 0.6969(2) 0.5745(4) 0.0621(14) Uani 1 1 d DU . . C12 C 0.8312(4) 0.6637(2) 0.6253(5) 0.0753(18) Uani 1 1 d DU . . H12 H 0.8947 0.6679 0.6405 0.090 Uiso 1 1 calc R . . C13 C 0.7896(4) 0.6254(3) 0.6469(5) 0.0794(18) Uani 1 1 d DU . . H13 H 0.8190 0.5985 0.6811 0.095 Uiso 1 1 calc R . . C14 C 0.6901(4) 0.6337(2) 0.6069(4) 0.0599(14) Uani 1 1 d DU . . C15 C 0.6235(4) 0.6023(2) 0.6204(4) 0.0598(13) Uani 1 1 d U . . C16 C 0.5264(4) 0.60859(19) 0.5789(4) 0.0549(13) Uani 1 1 d DU . . C17 C 0.4587(4) 0.5776(2) 0.5960(4) 0.0641(15) Uani 1 1 d DU . . H17 H 0.4706 0.5492 0.6321 0.077 Uiso 1 1 calc R . . C18 C 0.3751(4) 0.5971(2) 0.5502(4) 0.0651(15) Uani 1 1 d DU . . H18 H 0.3182 0.5847 0.5482 0.078 Uiso 1 1 calc R . . C19 C 0.3893(4) 0.6404(2) 0.5051(4) 0.0559(13) Uani 1 1 d DU . . C20 C 0.3193(4) 0.6742(2) 0.4614(4) 0.0622(13) Uani 1 1 d U . . C21 C 0.4456(4) 0.8742(2) 0.4401(4) 0.0654(14) Uani 1 1 d DU . . C22 C 0.4193(4) 0.8970(2) 0.5143(4) 0.0773(17) Uani 1 1 d DU . . H22 H 0.4200 0.8808 0.5729 0.093 Uiso 1 1 calc R . . C23 C 0.3920(4) 0.9439(2) 0.5022(5) 0.089(2) Uani 1 1 d DU . . H23 H 0.3740 0.9584 0.5529 0.106 Uiso 1 1 calc R . . C24 C 0.3906(5) 0.9695(2) 0.4186(5) 0.095(2) Uani 1 1 d DU . . C25 C 0.4170(6) 0.9470(2) 0.3443(6) 0.106(2) Uani 1 1 d DU . . H25 H 0.4155 0.9634 0.2855 0.127 Uiso 1 1 calc R . . C26 C 0.4454(5) 0.9008(2) 0.3560(5) 0.092(2) Uani 1 1 d DU . . H26 H 0.4651 0.8868 0.3059 0.110 Uiso 1 1 calc R . . C27 C 0.3577(7) 1.0217(3) 0.4041(8) 0.133(3) Uani 1 1 d DU . . H27A H 0.3622 1.0336 0.3410 0.200 Uiso 1 1 calc R . . H27B H 0.3963 1.0403 0.4601 0.200 Uiso 1 1 calc R . . H27C H 0.2945 1.0235 0.4023 0.200 Uiso 1 1 calc R . . C28 C 0.8727(4) 0.7580(2) 0.5667(4) 0.0669(16) Uani 1 1 d DU . . C29 C 0.9038(4) 0.7656(3) 0.4861(5) 0.104(3) Uani 1 1 d DU . . H29 H 0.8632 0.7615 0.4197 0.125 Uiso 1 1 calc R . . C30 C 0.9945(5) 0.7794(3) 0.5015(6) 0.123(3) Uani 1 1 d DU . . H30 H 1.0130 0.7844 0.4448 0.147 Uiso 1 1 calc R . . C31 C 1.0571(4) 0.7859(3) 0.5966(6) 0.114(3) Uani 1 1 d DU . . C32 C 1.0273(5) 0.7788(3) 0.6773(6) 0.112(3) Uani 1 1 d DU . . H32 H 1.0682 0.7833 0.7435 0.134 Uiso 1 1 calc R . . C33 C 0.9364(4) 0.7649(3) 0.6626(5) 0.095(2) Uani 1 1 d DU . . H33 H 0.9182 0.7602 0.7196 0.114 Uiso 1 1 calc R . . C34 C 1.1572(5) 0.8011(4) 0.6129(9) 0.159(4) Uani 1 1 d DU . . H34A H 1.1664 0.8036 0.5478 0.239 Uiso 1 1 calc R . . H34B H 1.1992 0.7781 0.6544 0.239 Uiso 1 1 calc R . . H34C H 1.1687 0.8312 0.6468 0.239 Uiso 1 1 calc R . . C35 C 0.6586(4) 0.5594(2) 0.6829(4) 0.0637(14) Uani 1 1 d DU . . C36 C 0.7041(4) 0.5632(2) 0.7872(4) 0.0836(19) Uani 1 1 d DU . . H36 H 0.7102 0.5928 0.8182 0.100 Uiso 1 1 calc R . . C37 C 0.7408(4) 0.5237(2) 0.8467(5) 0.086(2) Uani 1 1 d DU . . H37 H 0.7712 0.5273 0.9167 0.103 Uiso 1 1 calc R . . C38 C 0.7329(4) 0.4796(2) 0.8033(4) 0.0767(17) Uani 1 1 d DU . . C39 C 0.6860(5) 0.4748(2) 0.7026(5) 0.088(2) Uani 1 1 d DU . . H39 H 0.6776 0.4449 0.6730 0.106 Uiso 1 1 calc R . . C40 C 0.6498(4) 0.5144(2) 0.6421(5) 0.0793(18) Uani 1 1 d DU . . H40 H 0.6188 0.5103 0.5724 0.095 Uiso 1 1 calc R . . C41 C 0.7779(6) 0.4365(3) 0.8687(6) 0.108(3) Uani 1 1 d DU . . H41A H 0.8085 0.4463 0.9382 0.162 Uiso 1 1 calc R . . H41B H 0.8223 0.4225 0.8420 0.162 Uiso 1 1 calc R . . H41C H 0.7308 0.4137 0.8668 0.162 Uiso 1 1 calc R . . C42 C 0.2209(4) 0.6591(2) 0.4415(5) 0.0728(17) Uani 1 1 d DU . . C43 C 0.1775(4) 0.6306(3) 0.3597(5) 0.098(2) Uani 1 1 d DU . . H43 H 0.2099 0.6201 0.3176 0.117 Uiso 1 1 calc R . . C44 C 0.0861(5) 0.6170(3) 0.3391(7) 0.139(3) Uani 1 1 d DU . . H44 H 0.0587 0.5976 0.2831 0.167 Uiso 1 1 calc R . . C45 C 0.0353(5) 0.6309(4) 0.3967(8) 0.138(4) Uani 1 1 d DU . . C46 C 0.0795(5) 0.6572(4) 0.4803(8) 0.158(4) Uani 1 1 d DU . . H46 H 0.0478 0.6651 0.5248 0.189 Uiso 1 1 calc R . . C47 C 0.1699(4) 0.6731(3) 0.5025(6) 0.122(3) Uani 1 1 d DU . . H47 H 0.1962 0.6930 0.5580 0.147 Uiso 1 1 calc R . . C48 C -0.0672(5) 0.6171(5) 0.3748(12) 0.220(7) Uani 1 1 d DU . . H48A H -0.0893 0.6310 0.4256 0.329 Uiso 1 1 calc R . . H48B H -0.0723 0.5833 0.3770 0.329 Uiso 1 1 calc R . . H48C H -0.1038 0.6283 0.3082 0.329 Uiso 1 1 calc R . . C49 C 0.5586(6) 0.5712(3) 0.3545(6) 0.106(2) Uani 1 1 d DU . . H49A H 0.5173 0.5689 0.3936 0.160 Uiso 1 1 calc R . . H49B H 0.6024 0.5457 0.3723 0.160 Uiso 1 1 calc R . . H49C H 0.5234 0.5696 0.2828 0.160 Uiso 1 1 calc R . . O1 O 0.6073(3) 0.61539(18) 0.3764(3) 0.0870(13) Uani 1 1 d DU . . C50 C 0.6688(7) 0.6210(3) 0.3226(9) 0.164(4) Uani 1 1 d DU . . H50A H 0.7264 0.6056 0.3616 0.197 Uiso 1 1 calc R . . H50B H 0.6437 0.6038 0.2587 0.197 Uiso 1 1 calc R . . C51 C 0.6891(6) 0.6631(3) 0.3007(8) 0.148(3) Uani 1 1 d DU . . H51A H 0.6782 0.6633 0.2275 0.178 Uiso 1 1 calc R . . H51B H 0.7556 0.6666 0.3338 0.178 Uiso 1 1 calc R . . O2 O 0.6487(3) 0.70421(16) 0.3221(3) 0.0795(12) Uani 1 1 d DU . . C52 C 0.6281(6) 0.7361(4) 0.2406(7) 0.157(3) Uani 1 1 d DU . . H52A H 0.6838 0.7542 0.2481 0.189 Uiso 1 1 calc R . . H52B H 0.6148 0.7178 0.1780 0.189 Uiso 1 1 calc R . . C53 C 0.5608(6) 0.7655(4) 0.2280(7) 0.141(3) Uani 1 1 d DU . . H53A H 0.5278 0.7677 0.1550 0.169 Uiso 1 1 calc R . . H53B H 0.5883 0.7963 0.2498 0.169 Uiso 1 1 calc R . . O3 O 0.4949(3) 0.75831(16) 0.2752(3) 0.0738(12) Uani 1 1 d DU . . C54 C 0.4024(4) 0.7679(3) 0.2086(5) 0.095(2) Uani 1 1 d DU . . H54A H 0.3591 0.7606 0.2433 0.142 Uiso 1 1 calc R . . H54B H 0.3890 0.7489 0.1480 0.142 Uiso 1 1 calc R . . H54C H 0.3971 0.8007 0.1901 0.142 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 Y1 0.0561(3) 0.0496(3) 0.0493(2) -0.0025(2) 0.0187(2) -0.0012(3) Cl1 0.0766(9) 0.0873(13) 0.0642(8) -0.0172(8) 0.0152(7) -0.0108(9) N1 0.055(2) 0.052(3) 0.055(2) -0.003(2) 0.0210(19) 0.002(2) N2 0.065(2) 0.048(3) 0.053(2) 0.001(2) 0.019(2) 0.002(2) N3 0.055(2) 0.048(3) 0.053(2) -0.0016(19) 0.0166(19) -0.005(2) N4 0.057(2) 0.046(3) 0.054(2) -0.0022(19) 0.0200(19) -0.003(2) C1 0.065(3) 0.061(3) 0.059(3) 0.002(3) 0.025(3) 0.005(3) C2 0.060(3) 0.071(4) 0.084(4) 0.000(3) 0.021(3) 0.008(3) C3 0.070(3) 0.065(4) 0.085(4) 0.000(3) 0.027(3) 0.013(3) C4 0.066(3) 0.051(3) 0.062(3) 0.004(3) 0.026(3) 0.006(2) C5 0.070(3) 0.051(3) 0.059(3) 0.005(2) 0.025(3) 0.007(3) C6 0.070(3) 0.054(4) 0.058(3) 0.003(2) 0.024(3) 0.000(2) C7 0.086(4) 0.052(4) 0.090(4) -0.003(3) 0.033(3) -0.012(3) C8 0.073(3) 0.062(4) 0.081(4) 0.001(3) 0.029(3) -0.008(3) C9 0.059(3) 0.057(3) 0.059(3) -0.003(3) 0.018(2) -0.008(3) C10 0.065(3) 0.056(3) 0.061(3) 0.002(3) 0.020(2) -0.007(3) C11 0.058(3) 0.064(3) 0.063(3) 0.001(3) 0.018(3) -0.001(3) C12 0.055(3) 0.064(4) 0.099(4) 0.009(3) 0.016(3) 0.001(3) C13 0.065(3) 0.066(4) 0.099(4) 0.013(4) 0.016(3) 0.007(3) C14 0.063(3) 0.050(3) 0.064(3) 0.003(3) 0.018(3) 0.002(3) C15 0.069(3) 0.049(3) 0.062(3) -0.001(2) 0.022(3) -0.001(3) C16 0.067(3) 0.042(3) 0.057(3) 0.000(2) 0.022(2) -0.002(2) C17 0.071(3) 0.055(4) 0.068(3) 0.005(3) 0.025(3) -0.007(3) C18 0.069(3) 0.053(4) 0.077(3) -0.006(3) 0.029(3) -0.012(3) C19 0.062(3) 0.049(3) 0.062(3) -0.005(2) 0.027(2) -0.004(2) C20 0.065(3) 0.059(3) 0.070(3) -0.007(3) 0.032(3) -0.001(3) C21 0.081(4) 0.049(3) 0.073(3) 0.003(3) 0.035(3) 0.003(3) C22 0.107(4) 0.059(4) 0.079(3) 0.001(3) 0.048(3) 0.008(3) C23 0.116(5) 0.066(4) 0.101(4) 0.001(3) 0.058(4) 0.016(4) C24 0.125(5) 0.055(4) 0.117(5) 0.005(3) 0.057(4) 0.011(4) C25 0.159(6) 0.065(4) 0.121(5) 0.027(4) 0.083(5) 0.029(5) C26 0.148(6) 0.059(4) 0.087(4) 0.011(3) 0.064(4) 0.014(4) C27 0.175(8) 0.061(5) 0.189(8) 0.024(5) 0.095(7) 0.034(5) C28 0.059(3) 0.063(4) 0.076(3) 0.000(3) 0.018(3) -0.004(3) C29 0.098(4) 0.131(7) 0.096(4) -0.039(4) 0.050(3) -0.053(5) C30 0.093(4) 0.162(9) 0.136(5) -0.052(6) 0.068(4) -0.046(5) C31 0.071(4) 0.103(6) 0.173(6) -0.060(5) 0.050(4) -0.034(4) C32 0.073(4) 0.120(7) 0.120(5) -0.007(6) 0.003(4) -0.020(5) C33 0.074(4) 0.106(6) 0.095(4) -0.001(4) 0.014(3) -0.023(4) C34 0.075(4) 0.165(10) 0.253(11) -0.087(8) 0.074(5) -0.039(5) C35 0.067(3) 0.054(3) 0.067(3) 0.003(3) 0.018(3) 0.000(3) C36 0.108(5) 0.069(4) 0.067(3) 0.005(3) 0.020(3) 0.000(4) C37 0.111(5) 0.076(4) 0.070(3) 0.005(3) 0.027(4) 0.003(4) C38 0.076(4) 0.067(4) 0.087(4) 0.015(3) 0.027(3) 0.003(3) C39 0.107(5) 0.055(4) 0.090(4) -0.003(3) 0.016(4) 0.008(4) C40 0.090(4) 0.064(4) 0.077(3) -0.002(3) 0.018(3) 0.009(4) C41 0.115(6) 0.082(5) 0.118(5) 0.036(4) 0.025(5) 0.021(5) C42 0.059(3) 0.070(4) 0.093(4) -0.002(3) 0.030(3) 0.001(3) C43 0.070(4) 0.103(6) 0.113(5) -0.016(4) 0.020(4) -0.013(4) C44 0.073(4) 0.146(9) 0.180(8) -0.028(7) 0.017(5) -0.033(5) C45 0.060(4) 0.124(8) 0.224(9) 0.030(6) 0.037(5) 0.002(5) C46 0.103(4) 0.174(11) 0.239(9) -0.018(7) 0.113(5) -0.014(6) C47 0.087(4) 0.153(8) 0.153(6) -0.036(5) 0.076(4) -0.012(5) C48 0.072(5) 0.198(13) 0.384(18) 0.033(13) 0.071(7) -0.016(6) C49 0.153(7) 0.071(5) 0.104(5) -0.018(4) 0.053(5) -0.006(4) O1 0.086(3) 0.081(3) 0.093(3) -0.024(3) 0.028(2) -0.005(3) C50 0.165(6) 0.098(5) 0.292(10) -0.031(7) 0.158(6) 0.007(6) C51 0.171(6) 0.129(6) 0.204(8) 0.030(6) 0.142(6) 0.051(5) O2 0.079(2) 0.095(3) 0.078(2) 0.012(2) 0.044(2) 0.012(2) C52 0.159(6) 0.174(8) 0.186(7) 0.112(6) 0.122(5) 0.065(6) C53 0.132(5) 0.157(8) 0.167(6) 0.098(6) 0.094(5) 0.042(5) O3 0.083(2) 0.080(3) 0.058(2) 0.015(2) 0.0229(19) 0.001(2) C54 0.094(4) 0.113(7) 0.066(4) 0.014(4) 0.012(3) 0.025(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 N1 2.368(4) . ? Y1 N4 2.380(4) . ? Y1 N2 2.411(5) . ? Y1 N3 2.414(4) . ? Y1 O2 2.478(4) . ? Y1 O3 2.539(4) . ? Y1 Cl1 2.6702(16) . ? Y1 O1 2.690(5) . ? N1 C1 1.379(7) . ? N1 C4 1.378(7) . ? N2 C6 1.377(7) . ? N2 C9 1.384(7) . ? N3 C14 1.365(7) . ? N3 C11 1.391(7) . ? N4 C19 1.371(6) . ? N4 C16 1.377(7) . ? C1 C20 1.406(9) . ? C1 C2 1.443(8) . ? C2 C3 1.347(9) . ? C3 C4 1.445(8) . ? C4 C5 1.421(8) . ? C5 C6 1.409(8) . ? C5 C21 1.475(8) . ? C6 C7 1.458(8) . ? C7 C8 1.354(9) . ? C8 C9 1.441(9) . ? C9 C10 1.397(8) . ? C10 C11 1.401(8) . ? C10 C28 1.490(7) . ? C11 C12 1.433(8) . ? C12 C13 1.339(9) . ? C13 C14 1.453(8) . ? C14 C15 1.410(8) . ? C15 C16 1.411(8) . ? C15 C35 1.485(8) . ? C16 C17 1.435(7) . ? C17 C18 1.342(8) . ? C18 C19 1.423(8) . ? C19 C20 1.414(8) . ? C20 C42 1.498(8) . ? C21 C22 1.382(7) . ? C21 C26 1.385(7) . ? C22 C23 1.385(7) . ? C23 C24 1.359(8) . ? C24 C25 1.380(8) . ? C24 C27 1.552(8) . ? C25 C26 1.372(8) . ? C28 C29 1.366(7) . ? C28 C33 1.375(7) . ? C29 C30 1.387(8) . ? C30 C31 1.358(9) . ? C31 C32 1.355(9) . ? C31 C34 1.531(8) . ? C32 C33 1.391(8) . ? C35 C36 1.383(7) . ? C35 C40 1.384(7) . ? C36 C37 1.391(8) . ? C37 C38 1.375(8) . ? C38 C39 1.346(7) . ? C38 C41 1.539(8) . ? C39 C40 1.397(8) . ? C42 C43 1.369(8) . ? C42 C47 1.383(8) . ? C43 C44 1.382(8) . ? C44 C45 1.343(9) . ? C45 C46 1.353(10) . ? C45 C48 1.544(9) . ? C46 C47 1.385(8) . ? C49 O1 1.435(8) . ? O1 C50 1.388(9) . ? C50 C51 1.292(11) . ? C51 O2 1.396(9) . ? O2 C52 1.396(8) . ? C52 C53 1.290(10) . ? C53 O3 1.386(8) . ? O3 C54 1.433(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Y1 N4 74.95(15) . . ? N1 Y1 N2 74.96(15) . . ? N4 Y1 N2 118.61(14) . . ? N1 Y1 N3 116.83(14) . . ? N4 Y1 N3 75.01(14) . . ? N2 Y1 N3 73.06(15) . . ? N1 Y1 O2 140.40(15) . . ? N4 Y1 O2 144.64(15) . . ? N2 Y1 O2 81.25(15) . . ? N3 Y1 O2 84.77(14) . . ? N1 Y1 O3 77.80(14) . . ? N4 Y1 O3 145.71(14) . . ? N2 Y1 O3 72.75(14) . . ? N3 Y1 O3 137.05(14) . . ? O2 Y1 O3 65.02(13) . . ? N1 Y1 Cl1 89.26(11) . . ? N4 Y1 Cl1 84.40(10) . . ? N2 Y1 Cl1 146.18(11) . . ? N3 Y1 Cl1 140.09(12) . . ? O2 Y1 Cl1 93.52(11) . . ? O3 Y1 Cl1 74.77(10) . . ? N1 Y1 O1 151.40(15) . . ? N4 Y1 O1 81.63(14) . . ? N2 Y1 O1 131.88(14) . . ? N3 Y1 O1 71.33(14) . . ? O2 Y1 O1 64.34(15) . . ? O3 Y1 O1 116.07(14) . . ? Cl1 Y1 O1 72.11(10) . . ? C1 N1 C4 106.4(4) . . ? C1 N1 Y1 120.7(4) . . ? C4 N1 Y1 126.5(3) . . ? C6 N2 C9 106.1(5) . . ? C6 N2 Y1 126.1(3) . . ? C9 N2 Y1 123.3(4) . . ? C14 N3 C11 106.3(5) . . ? C14 N3 Y1 124.8(3) . . ? C11 N3 Y1 121.9(3) . . ? C19 N4 C16 106.0(4) . . ? C19 N4 Y1 122.6(3) . . ? C16 N4 Y1 127.9(3) . . ? N1 C1 C20 125.6(5) . . ? N1 C1 C2 109.7(5) . . ? C20 C1 C2 124.3(5) . . ? C3 C2 C1 106.9(5) . . ? C2 C3 C4 107.7(6) . . ? N1 C4 C5 126.6(5) . . ? N1 C4 C3 109.2(5) . . ? C5 C4 C3 124.2(6) . . ? C6 C5 C4 124.0(5) . . ? C6 C5 C21 118.4(5) . . ? C4 C5 C21 117.5(5) . . ? N2 C6 C5 126.4(5) . . ? N2 C6 C7 109.6(5) . . ? C5 C6 C7 123.9(6) . . ? C8 C7 C6 107.0(6) . . ? C7 C8 C9 107.2(6) . . ? N2 C9 C10 125.6(5) . . ? N2 C9 C8 110.1(5) . . ? C10 C9 C8 124.1(5) . . ? C11 C10 C9 125.0(5) . . ? C11 C10 C28 117.2(5) . . ? C9 C10 C28 117.6(5) . . ? N3 C11 C10 125.0(5) . . ? N3 C11 C12 109.3(5) . . ? C10 C11 C12 125.5(5) . . ? C13 C12 C11 107.7(5) . . ? C12 C13 C14 107.3(6) . . ? N3 C14 C15 126.6(5) . . ? N3 C14 C13 109.4(5) . . ? C15 C14 C13 123.9(6) . . ? C16 C15 C14 125.0(5) . . ? C16 C15 C35 117.9(5) . . ? C14 C15 C35 117.1(5) . . ? N4 C16 C15 125.6(5) . . ? N4 C16 C17 109.4(5) . . ? C15 C16 C17 124.9(5) . . ? C18 C17 C16 107.1(5) . . ? C17 C18 C19 107.6(5) . . ? N4 C19 C20 125.1(5) . . ? N4 C19 C18 109.9(5) . . ? C20 C19 C18 124.6(5) . . ? C1 C20 C19 125.0(5) . . ? C1 C20 C42 117.8(5) . . ? C19 C20 C42 117.0(5) . . ? C22 C21 C26 116.9(5) . . ? C22 C21 C5 121.5(5) . . ? C26 C21 C5 121.6(5) . . ? C21 C22 C23 120.5(6) . . ? C24 C23 C22 122.2(6) . . ? C23 C24 C25 117.6(6) . . ? C23 C24 C27 122.0(6) . . ? C25 C24 C27 120.3(6) . . ? C24 C25 C26 120.8(6) . . ? C21 C26 C25 121.9(6) . . ? C29 C28 C33 116.1(6) . . ? C29 C28 C10 121.0(5) . . ? C33 C28 C10 122.9(5) . . ? C28 C29 C30 121.4(6) . . ? C31 C30 C29 122.1(7) . . ? C32 C31 C30 117.3(6) . . ? C32 C31 C34 120.8(7) . . ? C30 C31 C34 121.8(8) . . ? C31 C32 C33 120.9(7) . . ? C28 C33 C32 122.2(7) . . ? C36 C35 C40 116.4(6) . . ? C36 C35 C15 120.2(5) . . ? C40 C35 C15 123.3(5) . . ? C35 C36 C37 121.3(6) . . ? C38 C37 C36 120.8(6) . . ? C39 C38 C37 118.9(6) . . ? C39 C38 C41 120.7(6) . . ? C37 C38 C41 120.4(6) . . ? C38 C39 C40 120.6(6) . . ? C35 C40 C39 121.9(6) . . ? C43 C42 C47 117.2(6) . . ? C43 C42 C20 120.1(5) . . ? C47 C42 C20 122.7(6) . . ? C42 C43 C44 120.8(7) . . ? C45 C44 C43 122.7(8) . . ? C44 C45 C46 116.5(7) . . ? C44 C45 C48 124.0(9) . . ? C46 C45 C48 119.5(9) . . ? C45 C46 C47 123.0(8) . . ? C42 C47 C46 119.6(7) . . ? C50 O1 C49 112.4(6) . . ? C50 O1 Y1 113.6(5) . . ? C49 O1 Y1 125.7(4) . . ? C51 C50 O1 119.3(8) . . ? C50 C51 O2 124.2(8) . . ? C51 O2 C52 111.4(7) . . ? C51 O2 Y1 118.5(4) . . ? C52 O2 Y1 118.2(4) . . ? C53 C52 O2 118.8(7) . . ? C52 C53 O3 120.8(7) . . ? C53 O3 C54 112.6(5) . . ? C53 O3 Y1 115.2(4) . . ? C54 O3 Y1 125.1(4) . . ? _diffrn_measured_fraction_theta_max 0.771 _diffrn_reflns_theta_full 25.53 _diffrn_measured_fraction_theta_full 0.771 _refine_diff_density_max 0.588 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.083 #----------------------------------------------------------------------------- data_2 _audit_creation_method Manual _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H87 Cl2 N8 O6.50 Y2' _chemical_formula_weight 1753.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 13.607(2) _cell_length_b 14.732(2) _cell_length_c 14.933(2) _cell_angle_alpha 63.95(2) _cell_angle_beta 87.14(2) _cell_angle_gamma 71.12(2) _cell_volume 2529.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used '91 from 4 still frames' _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 907 _exptl_absorpt_coefficient_mu 1.246 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.855 _exptl_absorpt_correction_T_max 1.149 _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 ; Rigaku RU-200 rotating-anode generator powered at 50kV / 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS IIc' _diffrn_measurement_method ; Data was collected to 0.82\%A and 80% completeness by taking 36 oscillation frames in the range of 0 - 180\%, \D\f = 5\%, 10 min. per frame. Crystal to detector distance is 77.766 mm, background level -30. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6225 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1100 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.59 _reflns_number_total 6255 _reflns_number_gt 3532 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'BioteX 1.0 (MSC, 1990)' _computing_cell_refinement 'BioteX 1.0 (MSC, 1990)' _computing_data_reduction 'BioteX 1.0 (MSC, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Siemens, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F against OBSERVED reflections. The weighted R-factor Rw and goodness of fit S are based on F. The threshold expression of F > 6sigma(F) is used for refinement. The structure was refined in two separate blocks, number of parameters and data-to-parameter ratio of each block is 516 (6.8:1) and 564 (6.3:1), respectively. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo) + 0.0050Fo^2^]' _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 0.025(13) _refine_ls_number_reflns 3532 _refine_ls_number_parameters 1071 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1361 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.1863 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.33 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max 0.063 _refine_ls_shift/su_mean 0.025 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.18640 0.10629 0.29971 0.0565(4) Uani 1 1 d D . . Cl1 Cl 0.0568(4) 0.0017(4) 0.4285(4) 0.151(1) Uani 1 1 d D . . O1W O 0.3149(5) -0.0554(5) 0.4214(5) 0.112(1) Uani 1 1 d D . . O4W O 0.1883(5) -0.1827(5) 0.7574(5) 0.161(1) Uani 1 1 d D . . N1 N 0.0428(4) 0.2359(4) 0.3093(4) 0.068(1) Uani 1 1 d D . . N2 N 0.1135(4) 0.2099(4) 0.1322(4) 0.062(1) Uani 1 1 d D . . N3 N 0.3279(4) 0.1378(4) 0.2192(4) 0.057(1) Uani 1 1 d D . . N4 N 0.2531(4) 0.1762(4) 0.3856(4) 0.047(1) Uani 1 1 d D . . C1 C 0.0236(5) 0.2580(5) 0.3899(4) 0.062(1) Uani 1 1 d D . . C2 C -0.0782(5) 0.3315(5) 0.3762(5) 0.074(1) Uani 1 1 d D . . H2 H -0.1075 0.3667 0.4172 0.080 Uiso 1 1 calc R . . C3 C -0.1324(5) 0.3423(5) 0.2815(4) 0.047(1) Uani 1 1 d D . . H3 H -0.2045 0.3766 0.2544 0.080 Uiso 1 1 calc R . . C4 C -0.0487(4) 0.2899(5) 0.2463(4) 0.063(1) Uani 1 1 d D . . C5 C -0.0647(5) 0.2983(5) 0.1484(5) 0.060(1) Uani 1 1 d D . . C6 C 0.0091(4) 0.2560(5) 0.0965(4) 0.051(1) Uani 1 1 d D . . C7 C -0.0112(5) 0.2681(5) 0.0030(5) 0.060(1) Uani 1 1 d D . . H7 H -0.0783 0.3028 -0.0358 0.080 Uiso 1 1 calc R . . C8 C 0.0826(5) 0.2216(5) -0.0269(5) 0.073(1) Uani 1 1 d D . . H8 H 0.0934 0.2140 -0.0877 0.080 Uiso 1 1 calc R . . C9 C 0.1651(5) 0.1856(5) 0.0598(4) 0.084(1) Uani 1 1 d D . . C10 C 0.2681(5) 0.1675(5) 0.0463(5) 0.063(1) Uani 1 1 d D . . C11 C 0.3397(5) 0.1472(5) 0.1240(4) 0.071(1) Uani 1 1 d D . . C12 C 0.4630(5) 0.1330(5) 0.1053(5) 0.074(1) Uani 1 1 d D . . H12 H 0.4963 0.1320 0.0474 0.080 Uiso 1 1 calc R . . C13 C 0.5058(5) 0.1234(5) 0.1878(5) 0.077(1) Uani 1 1 d D . . H13 H 0.5766 0.1179 0.1999 0.080 Uiso 1 1 calc R . . C14 C 0.4237(4) 0.1227(4) 0.2597(4) 0.045(1) Uani 1 1 d D . . C15 C 0.4440(5) 0.1138(4) 0.3525(4) 0.038(1) Uani 1 1 d D . . C16 C 0.3595(4) 0.1342(5) 0.4130(5) 0.066(1) Uani 1 1 d D . . C17 C 0.3801(5) 0.1364(5) 0.5165(5) 0.065(1) Uani 1 1 d D . . H17 H 0.4464 0.1135 0.5535 0.080 Uiso 1 1 calc R . . C18 C 0.2889(5) 0.1756(5) 0.5396(5) 0.066(1) Uani 1 1 d D . . H18 H 0.2747 0.1969 0.5924 0.080 Uiso 1 1 calc R . . C19 C 0.2074(4) 0.1823(5) 0.4687(4) 0.055(1) Uani 1 1 d D . . C20 C 0.1015(5) 0.2336(4) 0.4599(5) 0.051(1) Uani 1 1 d . . . C22 C -0.2049(4) 0.4494(4) 0.0135(4) 0.073(1) Uani 1 1 d G . . H22 H -0.1535 0.4832 -0.0140 0.080 Uiso 1 1 calc G . . C23 C -0.3077 0.4993 -0.0317 0.103(1) Uani 1 1 d G . . H23 H -0.3271 0.5674 -0.0902 0.080 Uiso 1 1 calc G . . C24 C -0.3823 0.4502 0.0082 0.111(1) Uani 1 1 d G . . H24 H -0.4531 0.4845 -0.0229 0.080 Uiso 1 1 calc G . . C25 C -0.3542 0.3512 0.0932 0.095(1) Uani 1 1 d G . . H25 H -0.4055 0.3175 0.1207 0.080 Uiso 1 1 calc G . . C26 C -0.2513 0.3014 0.1384 0.088(1) Uani 1 1 d G . . H26 H -0.2319 0.2333 0.1969 0.080 Uiso 1 1 calc G . . C21 C -0.1767 0.3505 0.0985 0.056(1) Uani 1 1 d G . . C28 C 0.2781(4) 0.2501(4) -0.1433(4) 0.089(1) Uani 1 1 d G . . H28 H 0.2303 0.3164 -0.1476 0.080 Uiso 1 1 calc G . . C29 C 0.3120 0.2426 -0.2304 0.071(1) Uani 1 1 d G . . H29 H 0.2875 0.3039 -0.2945 0.080 Uiso 1 1 calc G . . C30 C 0.3816 0.1462 -0.2241 0.072(1) Uani 1 1 d G . . H30 H 0.4049 0.1410 -0.2840 0.080 Uiso 1 1 calc G . . C31 C 0.4172 0.0571 -0.1309 0.088(1) Uani 1 1 d G . . H31 H 0.4651 -0.0093 -0.1266 0.080 Uiso 1 1 calc G . . C32 C 0.3833 0.0646 -0.0439 0.084(1) Uani 1 1 d G . . H32 H 0.4079 0.0033 0.0203 0.080 Uiso 1 1 calc G . . C27 C 0.3138 0.1610 -0.0501 0.060(1) Uani 1 1 d G . . C34 C 0.6191(4) -0.0021(4) 0.4309(4) 0.139(1) Uani 1 1 d G . . H34 H 0.5948 -0.0608 0.4444 0.080 Uiso 1 1 calc G . . C35 C 0.7227 -0.0221 0.4600 0.110(1) Uani 1 1 d G . . H35 H 0.7698 -0.0946 0.4937 0.080 Uiso 1 1 calc G . . C36 C 0.7580 0.0631 0.4403 0.087(1) Uani 1 1 d G . . H36 H 0.8293 0.0494 0.4604 0.080 Uiso 1 1 calc G . . C37 C 0.6895 0.1685 0.3914 0.086(1) Uani 1 1 d G . . H37 H 0.7138 0.2272 0.3779 0.080 Uiso 1 1 calc G . . C38 C 0.5858 0.1885 0.3623 0.084(1) Uani 1 1 d G . . H38 H 0.5387 0.2610 0.3287 0.080 Uiso 1 1 calc G . . C33 C 0.5506 0.1032 0.3820 0.073(1) Uani 1 1 d G . . C40 C 0.0833(4) 0.3170(4) 0.5822(4) 0.071(1) Uani 1 1 d G . . H40 H 0.1265 0.3574 0.5438 0.080 Uiso 1 1 calc G . . C41 C 0.0454 0.3268 0.6672 0.068(1) Uani 1 1 d G . . H41 H 0.0626 0.3738 0.6874 0.080 Uiso 1 1 calc G . . C42 C -0.0175 0.2681 0.7229 0.129(1) Uani 1 1 d G . . H42 H -0.0435 0.2748 0.7815 0.080 Uiso 1 1 calc G . . C43 C -0.0425 0.1997 0.6936 0.098(1) Uani 1 1 d G . . H43 H -0.0857 0.1594 0.7320 0.080 Uiso 1 1 calc G . . C44 C -0.0046 0.1900 0.6086 0.089(1) Uani 1 1 d G . . H44 H -0.0218 0.1430 0.5884 0.080 Uiso 1 1 calc G . . C39 C 0.0583 0.2486 0.5528 0.061(1) Uani 1 1 d D . . O1 O 0.2467(4) -0.0294(4) 0.2349(4) 0.074(1) Uani 1 1 d D . . C89 C 0.1768(4) -0.0524(4) 0.1868(4) 0.095(1) Uani 1 1 d D . . H89A H 0.1199 -0.0634 0.2261 0.150 Uiso 1 1 calc R . . H89B H 0.1498 0.0059 0.1213 0.150 Uiso 1 1 calc R . . C90 C 0.2377(4) -0.1527(4) 0.1785(5) 0.198(1) Uani 1 1 d D . . H90A H 0.2292 -0.1410 0.1104 0.150 Uiso 1 1 calc R . . H90B H 0.2138 -0.2104 0.2215 0.150 Uiso 1 1 calc R . . C91 C 0.3467(4) -0.1785(4) 0.2087(5) 0.138(1) Uani 1 1 d D . . H91A H 0.3742 -0.2504 0.2614 0.150 Uiso 1 1 calc R . . H91B H 0.3867 -0.1715 0.1527 0.150 Uiso 1 1 calc R . . C92 C 0.3502(4) -0.0998(4) 0.2452(5) 0.096(1) Uani 1 1 d D . . H92A H 0.3932 -0.0594 0.2061 0.150 Uiso 1 1 calc R . . H92B H 0.3784 -0.1373 0.3144 0.150 Uiso 1 1 calc R . . O5 O -0.2048(5) -0.0399(4) 0.8033(5) 0.259(1) Uani 0.5 1 d PD . . C105 C -0.2704(4) -0.0879(4) 0.7824(5) 0.123(1) Uani 0.5 1 d PD . . H10K H -0.2361 -0.1268 0.7457 0.150 Uiso 0.5 1 calc PR . . H10L H -0.2896 -0.1355 0.8433 0.150 Uiso 0.5 1 calc PR . . C106 C -0.3643(5) 0.0048(4) 0.7202(5) 0.112(1) Uani 0.5 1 d PD . . H10M H -0.4244 0.0027 0.7566 0.150 Uiso 0.5 1 calc PR . . H10N H -0.3770 0.0022 0.6589 0.150 Uiso 0.5 1 calc PR . . C107 C -0.3426(4) 0.1019(4) 0.6985(5) 0.185(1) Uani 0.5 1 d PD . . H10O H -0.3608 0.1510 0.6286 0.150 Uiso 0.5 1 calc PR . . H10P H -0.3812 0.1355 0.7378 0.150 Uiso 0.5 1 calc PR . . C108 C -0.2276(4) 0.0671(5) 0.7263(5) 0.256(1) Uani 0.5 1 d PD . . H10Q H -0.2117 0.1116 0.7508 0.150 Uiso 0.5 1 calc PR . . H10R H -0.1894 0.0686 0.6701 0.150 Uiso 0.5 1 calc PR . . Y2 Y 0.16485(14) -0.36460(14) 0.55454(14) 0.0618(4) Uani 1 1 d D . . Cl2 Cl 0.3070(3) -0.2815(3) 0.4994(3) 0.092(1) Uani 1 1 d D . . O2W O 0.0579(5) -0.2113(4) 0.4181(5) 0.093(1) Uani 1 1 d D . . O3W O 0.1525(5) -0.2326(5) 0.6052(5) 0.154(1) Uani 1 1 d D . . N5 N 0.0896(4) -0.4266(4) 0.4594(4) 0.074(1) Uani 1 1 d D . . N6 N 0.0161(4) -0.4025(4) 0.6443(4) 0.066(1) Uani 1 1 d D . . N7 N 0.2315(4) -0.4761(4) 0.7263(4) 0.063(1) Uani 1 1 d D . . N8 N 0.3091(4) -0.5136(4) 0.5536(4) 0.050(1) Uani 1 1 d D . . C45 C 0.1427(4) -0.4648(4) 0.3948(4) 0.060(1) Uani 1 1 d D . . C46 C 0.0725(5) -0.4388(5) 0.3213(5) 0.069(1) Uani 1 1 d D . . H46 H 0.0847 -0.4339 0.2558 0.080 Uiso 1 1 calc R . . C47 C -0.0245(5) -0.4196(5) 0.3617(5) 0.062(1) Uani 1 1 d D . . H47 H -0.0897 -0.4108 0.3314 0.080 Uiso 1 1 calc R . . C48 C -0.0131(4) -0.4161(4) 0.4436(4) 0.048(1) Uani 1 1 d D . . C49 C -0.0800(5) -0.4013(5) 0.5009(5) 0.067(1) Uani 1 1 d D . . C50 C -0.0747(4) -0.3939(5) 0.5994(4) 0.091(1) Uani 1 1 d D . . C51 C -0.1484(5) -0.3837(5) 0.6607(5) 0.072(1) Uani 1 1 d D . . H51 H -0.2215 -0.3689 0.6467 0.080 Uiso 1 1 calc R . . C52 C -0.1016(5) -0.3962(5) 0.7460(5) 0.086(1) Uani 1 1 d D . . H52 H -0.1360 -0.3964 0.8038 0.080 Uiso 1 1 calc R . . C53 C -0.0052(5) -0.4090(5) 0.7375(4) 0.057(1) Uani 1 1 d D . . C54 C 0.0722(5) -0.4238(5) 0.8053(5) 0.067(1) Uani 1 1 d D . . C55 C 0.1859(4) -0.4659(4) 0.8072(4) 0.043(1) Uani 1 1 d D . . C56 C 0.2596(5) -0.4965(5) 0.8809(5) 0.070(1) Uani 1 1 d D . . H56 H 0.2445 -0.5013 0.9460 0.080 Uiso 1 1 calc R . . C57 C 0.3498(5) -0.5180(5) 0.8549(5) 0.093(1) Uani 1 1 d D . . H57 H 0.4135 -0.5326 0.8917 0.080 Uiso 1 1 calc R . . C58 C 0.3379(4) -0.5153(5) 0.7509(5) 0.072(1) Uani 1 1 d D . . C59 C 0.4190(5) -0.5503(5) 0.7001(5) 0.060(1) Uani 1 1 d D . . C60 C 0.4028(4) -0.5577(5) 0.6129(4) 0.058(1) Uani 1 1 d D . . C61 C 0.4810(5) -0.6066(5) 0.5521(5) 0.074(1) Uani 1 1 d D . . H61 H 0.5526 -0.6510 0.5756 0.080 Uiso 1 1 calc R . . C62 C 0.4384(5) -0.5806(5) 0.4726(5) 0.060(1) Uani 1 1 d D . . H62 H 0.4725 -0.5911 0.4183 0.080 Uiso 1 1 calc R . . C63 C 0.3292(5) -0.5319(4) 0.4704(4) 0.053(1) Uani 1 1 d D . . C64 C 0.2523(5) -0.4950(5) 0.3822(5) 0.068(1) Uani 1 1 d . . . C66 C -0.2793(4) -0.2804(4) 0.4298(4) 0.075(1) Uani 1 1 d G . . H66 H -0.2674 -0.2155 0.4184 0.080 Uiso 1 1 calc G . . C67 C -0.3793 -0.2774 0.4085 0.108(1) Uani 1 1 d G . . H67 H -0.4363 -0.2105 0.3825 0.080 Uiso 1 1 calc G . . C68 C -0.3966 -0.3716 0.4251 0.094(1) Uani 1 1 d G . . H68 H -0.4654 -0.3695 0.4105 0.080 Uiso 1 1 calc G . . C69 C -0.3139 -0.4687 0.4629 0.115(1) Uani 1 1 d G . . H69 H -0.3258 -0.5336 0.4743 0.080 Uiso 1 1 calc G . . C70 C -0.2139 -0.4717 0.4841 0.087(1) Uani 1 1 d G . . H70 H -0.1570 -0.5386 0.5101 0.080 Uiso 1 1 calc G . . C65 C -0.1966 -0.3775 0.4675 0.072(1) Uani 1 1 d G . . C72 C 0.0637(4) -0.5022(4) 0.9919(4) 0.066(1) Uani 1 1 d G . . H72 H 0.1034 -0.5728 0.9999 0.080 Uiso 1 1 calc G . . C73 C 0.0286 -0.4869 1.0753 0.100(1) Uani 1 1 d G . . H73 H 0.0443 -0.5470 1.1407 0.080 Uiso 1 1 calc G . . C74 C -0.0291 -0.3843 1.0637 0.158(1) Uani 1 1 d G . . H74 H -0.0532 -0.3738 1.1211 0.080 Uiso 1 1 calc G . . C75 C -0.0518 -0.2970 0.9687 0.137(1) Uani 1 1 d G . . H75 H -0.0915 -0.2264 0.9608 0.080 Uiso 1 1 calc G . . C76 C -0.0167 -0.3123 0.8853 0.100(1) Uani 1 1 d G . . H76 H -0.0323 -0.2522 0.8200 0.080 Uiso 1 1 calc G . . C71 C 0.0410 -0.4149 0.8969 0.080(1) Uani 1 1 d G . . C78 C 0.5495(4) -0.7057(4) 0.8315(4) 0.121(1) Uani 1 1 d G . . H78 H 0.4954 -0.7370 0.8526 0.080 Uiso 1 1 calc G . . C79 C 0.6491 -0.7601 0.8839 0.118(1) Uani 1 1 d G . . H79 H 0.6637 -0.8289 0.9411 0.080 Uiso 1 1 calc G . . C80 C 0.7277 -0.7146 0.8533 0.087(1) Uani 1 1 d G . . H80 H 0.7963 -0.7520 0.8893 0.080 Uiso 1 1 calc G . . C81 C 0.7065 -0.6146 0.7702 0.110(1) Uani 1 1 d G . . H81 H 0.7605 -0.5833 0.7491 0.080 Uiso 1 1 calc G . . C82 C 0.6068 -0.5602 0.7178 0.084(1) Uani 1 1 d G . . H82 H 0.5922 -0.4915 0.6607 0.080 Uiso 1 1 calc G . . C77 C 0.5283 -0.6058 0.7485 0.096(1) Uani 1 1 d G . . C84 C 0.2621(4) -0.5862(4) 0.2776(4) 0.065(1) Uani 1 1 d G . . H84 H 0.2155 -0.6209 0.3173 0.080 Uiso 1 1 calc G . . C85 C 0.3003 -0.6062 0.1972 0.083(1) Uani 1 1 d G . . H85 H 0.2799 -0.6547 0.1816 0.080 Uiso 1 1 calc G . . C86 C 0.3680 -0.5558 0.1396 0.066(1) Uani 1 1 d G . . H86 H 0.3943 -0.5696 0.0842 0.080 Uiso 1 1 calc G . . C87 C 0.3976 -0.4854 0.1622 0.078(1) Uani 1 1 d G . . H87 H 0.4443 -0.4507 0.1225 0.080 Uiso 1 1 calc G . . C88 C 0.3595 -0.4654 0.2426 0.079(1) Uani 1 1 d G . . H88 H 0.3798 -0.4169 0.2582 0.080 Uiso 1 1 calc G . . C83 C 0.2917 -0.5158 0.3003 0.075(1) Uani 1 1 d G . . O2 O -0.0682(5) -0.1328(4) 0.2441(4) 0.061(1) Uani 0.5 1 d PD . . C93 C -0.1536(5) -0.0410(5) 0.2350(4) 0.107(1) Uani 0.5 1 d PD . . H93A H -0.2162 -0.0586 0.2523 0.150 Uiso 0.5 1 calc PR . . H93B H -0.1385 -0.0117 0.2766 0.150 Uiso 0.5 1 calc PR . . C94 C -0.1634(5) 0.0355(4) 0.1261(4) 0.087(1) Uani 0.5 1 d PD . . H94A H -0.1192 0.0779 0.1150 0.150 Uiso 0.5 1 calc PR . . H94B H -0.2345 0.0819 0.1026 0.150 Uiso 0.5 1 calc PR . . C95 C -0.1303(5) -0.0325(4) 0.0763(4) 0.102(1) Uani 0.5 1 d PD . . H95A H -0.1901 -0.0360 0.0481 0.150 Uiso 0.5 1 calc PR . . H95B H -0.0889 -0.0046 0.0239 0.150 Uiso 0.5 1 calc PR . . C96 C -0.0664(5) -0.1420(4) 0.1532(4) 0.127(1) Uani 0.5 1 d PD . . H96A H 0.0038 -0.1619 0.1365 0.150 Uiso 0.5 1 calc PR . . H96B H -0.0970 -0.1943 0.1586 0.150 Uiso 0.5 1 calc PR . . O3 O -0.2996(5) -0.3316(4) 0.1771(5) 0.126(1) Uani 0.5 1 d PD . . C97 C -0.3206(5) -0.2206(4) 0.1133(4) 0.128(1) Uani 0.5 1 d PD . . H97A H -0.3663 -0.1768 0.1410 0.150 Uiso 0.5 1 calc PR . . H97B H -0.2574 -0.2035 0.1004 0.150 Uiso 0.5 1 calc PR . . C98 C -0.3728(5) -0.2080(4) 0.0204(4) 0.265(1) Uani 0.5 1 d PD . . H98A H -0.3217 -0.2218 -0.0229 0.150 Uiso 0.5 1 calc PR . . H98B H -0.4219 -0.1367 -0.0147 0.150 Uiso 0.5 1 calc PR . . C99 C -0.4265(5) -0.2857(4) 0.0527(4) 0.110(1) Uani 0.5 1 d PD . . H99A H -0.4994 -0.2516 0.0541 0.150 Uiso 0.5 1 calc PR . . H99B H -0.4186 -0.3186 0.0085 0.150 Uiso 0.5 1 calc PR . . C100 C -0.3767(5) -0.3678(5) 0.1564(4) 0.123(1) Uani 0.5 1 d PD . . H10A H -0.3450 -0.4372 0.1583 0.150 Uiso 0.5 1 calc PR . . H10B H -0.4272 -0.3715 0.2039 0.150 Uiso 0.5 1 calc PR . . O4 O 0.4558(5) -0.1474(4) 0.5878(4) 0.088(1) Uani 0.5 1 d PD . . C101 C 0.4798(5) -0.1274(4) 0.6678(4) 0.145(1) Uani 0.5 1 d PD . . H10C H 0.5144 -0.0751 0.6454 0.150 Uiso 0.5 1 calc PR . . H10D H 0.4180 -0.1036 0.6967 0.150 Uiso 0.5 1 calc PR . . C102 C 0.5514(5) -0.2353(4) 0.7407(5) 0.104(1) Uani 0.5 1 d PD . . H10E H 0.5427 -0.2443 0.8080 0.150 Uiso 0.5 1 calc PR . . H10F H 0.6226 -0.2414 0.7282 0.150 Uiso 0.5 1 calc PR . . C103 C 0.5247(5) -0.3163(4) 0.7274(4) 0.110(1) Uani 0.5 1 d PD . . H10G H 0.5864 -0.3749 0.7344 0.150 Uiso 0.5 1 calc PR . . H10H H 0.4786 -0.3428 0.7750 0.150 Uiso 0.5 1 calc PR . . C104 C 0.4714(5) -0.2585(4) 0.6226(4) 0.145(1) Uani 0.5 1 d PD . . H10I H 0.4054 -0.2691 0.6223 0.150 Uiso 0.5 1 calc PR . . H10J H 0.5144 -0.2847 0.5803 0.150 Uiso 0.5 1 calc PR . . 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 Y1 0.0491(4) 0.0689(4) 0.0591(4) -0.0152(4) 0.0020(4) -0.0380(4) Cl1 0.114(1) 0.104(1) 0.210(1) -0.048(1) 0.041(1) -0.044(1) O1W 0.115(1) 0.101(1) 0.102(1) -0.035(1) -0.001(1) -0.031(1) O4W 0.167(1) 0.168(1) 0.159(1) -0.055(1) 0.017(1) -0.084(1) N1 0.050(1) 0.073(1) 0.060(1) -0.007(1) -0.013(1) -0.019(1) N2 0.053(1) 0.085(1) 0.055(1) -0.021(1) -0.004(1) -0.039(1) N3 0.056(1) 0.058(1) 0.057(1) -0.010(1) 0.000(1) -0.033(1) N4 0.045(1) 0.060(1) 0.042(1) -0.015(1) -0.016(1) -0.028(1) C1 0.054(1) 0.084(1) 0.053(1) -0.016(1) -0.001(1) -0.041(1) C2 0.061(1) 0.083(1) 0.078(1) -0.026(1) -0.015(1) -0.032(1) C3 0.041(1) 0.075(1) 0.035(1) -0.014(1) 0.000(1) -0.036(1) C4 0.049(1) 0.069(1) 0.068(1) -0.028(1) -0.005(1) -0.020(1) C5 0.055(1) 0.070(1) 0.056(1) -0.023(1) 0.000(1) -0.028(1) C6 0.041(1) 0.050(1) 0.044(1) 0.008(1) -0.007(1) -0.021(1) C7 0.040(1) 0.086(1) 0.052(1) -0.012(1) -0.020(1) -0.033(1) C8 0.078(1) 0.092(1) 0.066(1) -0.028(1) -0.011(1) -0.048(1) C9 0.081(1) 0.096(1) 0.071(1) -0.016(1) -0.009(1) -0.042(1) C10 0.064(1) 0.064(1) 0.057(1) -0.015(1) 0.000(1) -0.029(1) C11 0.058(1) 0.075(1) 0.069(1) -0.007(1) 0.000(1) -0.032(1) C12 0.074(1) 0.094(1) 0.060(1) -0.017(1) -0.010(1) -0.046(1) C13 0.066(1) 0.095(1) 0.062(1) -0.020(1) 0.010(1) -0.035(1) C14 0.043(1) 0.056(1) 0.045(1) -0.021(1) 0.007(1) -0.027(1) C15 0.045(1) 0.028(1) 0.036(1) 0.000(1) -0.007(1) -0.017(1) C16 0.058(1) 0.063(1) 0.060(1) -0.018(1) -0.005(1) -0.013(1) C17 0.065(1) 0.087(1) 0.055(1) -0.019(1) -0.022(1) -0.042(1) C18 0.062(1) 0.094(1) 0.045(1) -0.018(1) -0.017(1) -0.038(1) C19 0.058(1) 0.055(1) 0.048(1) -0.022(1) 0.004(1) -0.018(1) C20 0.059(1) 0.057(1) 0.052(1) -0.026(1) -0.006(1) -0.030(1) C22 0.039(1) 0.085(1) 0.069(1) -0.014(1) -0.015(1) -0.014(1) C23 0.087(1) 0.108(1) 0.086(1) -0.020(1) -0.022(1) -0.025(1) C24 0.100(1) 0.129(1) 0.118(1) -0.043(1) -0.001(1) -0.063(1) C25 0.064(1) 0.125(1) 0.083(1) -0.035(1) -0.005(1) -0.031(1) C26 0.079(1) 0.090(1) 0.084(1) -0.036(1) 0.003(1) -0.024(1) C21 0.035(1) 0.069(1) 0.039(1) -0.005(1) -0.011(1) -0.009(1) C28 0.086(1) 0.090(1) 0.084(1) -0.014(1) 0.005(1) -0.043(1) C29 0.070(1) 0.095(1) 0.053(1) -0.031(1) -0.008(1) -0.033(1) C30 0.067(1) 0.111(1) 0.051(1) -0.025(1) -0.015(1) -0.051(1) C31 0.095(1) 0.099(1) 0.081(1) -0.014(1) 0.014(1) -0.062(1) C32 0.089(1) 0.096(1) 0.066(1) -0.015(1) 0.025(1) -0.048(1) C27 0.054(1) 0.070(1) 0.054(1) -0.011(1) 0.002(1) -0.033(1) C34 0.132(1) 0.151(1) 0.172(1) -0.072(1) -0.014(1) -0.085(1) C35 0.089(1) 0.118(1) 0.125(1) -0.031(1) -0.021(1) -0.056(1) C36 0.071(1) 0.096(1) 0.092(1) -0.020(1) 0.004(1) -0.045(1) C37 0.083(1) 0.099(1) 0.092(1) -0.043(1) -0.003(1) -0.046(1) C38 0.066(1) 0.097(1) 0.080(1) -0.020(1) 0.000(1) -0.036(1) C33 0.070(1) 0.076(1) 0.081(1) -0.031(1) -0.013(1) -0.036(1) C40 0.079(1) 0.072(1) 0.058(1) -0.015(1) -0.002(1) -0.030(1) C41 0.085(1) 0.072(1) 0.054(1) -0.020(1) -0.009(1) -0.038(1) C42 0.129(1) 0.147(1) 0.114(1) -0.035(1) 0.012(1) -0.069(1) C43 0.096(1) 0.110(1) 0.090(1) -0.054(1) 0.022(1) -0.035(1) C44 0.100(1) 0.081(1) 0.083(1) -0.031(1) 0.030(1) -0.034(1) C39 0.057(1) 0.084(1) 0.040(1) -0.014(1) 0.000(1) -0.032(1) O1 0.086(1) 0.068(1) 0.067(1) -0.010(1) 0.002(1) -0.040(1) C89 0.117(1) 0.080(1) 0.109(1) -0.032(1) 0.001(1) -0.058(1) C90 0.192(1) 0.181(1) 0.197(1) -0.033(1) 0.022(1) -0.084(1) C91 0.143(1) 0.138(1) 0.151(1) -0.056(1) 0.021(1) -0.074(1) C92 0.088(1) 0.095(1) 0.106(1) -0.030(1) -0.003(1) -0.045(1) O5 0.260(1) 0.263(1) 0.265(1) -0.089(1) 0.021(1) -0.125(1) C105 0.122(1) 0.113(1) 0.129(1) -0.036(1) 0.015(1) -0.052(1) C106 0.110(1) 0.111(1) 0.110(1) -0.039(1) 0.010(1) -0.045(1) C107 0.193(1) 0.188(1) 0.190(1) -0.069(1) 0.017(1) -0.096(1) C108 0.260(1) 0.256(1) 0.262(1) -0.094(1) 0.032(1) -0.120(1) Y2 0.0650(4) 0.0635(4) 0.0477(4) -0.0099(4) -0.0174(4) -0.0226(4) Cl2 0.077(1) 0.072(1) 0.112(1) -0.029(1) 0.015(1) -0.025(1) O2W 0.091(1) 0.094(1) 0.084(1) -0.034(1) -0.012(1) -0.027(1) O3W 0.173(1) 0.153(1) 0.159(1) -0.054(1) -0.002(1) -0.087(1) N5 0.067(1) 0.062(1) 0.071(1) 0.000(1) 0.016(1) -0.027(1) N6 0.058(1) 0.083(1) 0.063(1) -0.014(1) -0.012(1) -0.044(1) N7 0.047(1) 0.055(1) 0.066(1) -0.003(1) -0.003(1) -0.018(1) N8 0.067(1) 0.048(1) 0.041(1) -0.016(1) 0.005(1) -0.028(1) C45 0.083(1) 0.057(1) 0.050(1) -0.027(1) 0.007(1) -0.031(1) C46 0.072(1) 0.091(1) 0.062(1) -0.028(1) -0.005(1) -0.049(1) C47 0.054(1) 0.069(1) 0.052(1) -0.014(1) -0.001(1) -0.023(1) C48 0.048(1) 0.057(1) 0.056(1) -0.020(1) -0.001(1) -0.038(1) C49 0.071(1) 0.075(1) 0.065(1) -0.021(1) -0.014(1) -0.039(1) C50 0.081(1) 0.097(1) 0.082(1) -0.017(1) -0.006(1) -0.036(1) C51 0.055(1) 0.105(1) 0.061(1) -0.027(1) 0.006(1) -0.041(1) C52 0.065(1) 0.106(1) 0.067(1) -0.009(1) 0.004(1) -0.035(1) C53 0.052(1) 0.075(1) 0.048(1) -0.017(1) 0.013(1) -0.036(1) C54 0.052(1) 0.090(1) 0.042(1) -0.001(1) -0.005(1) -0.030(1) C55 0.058(1) 0.042(1) 0.024(1) -0.014(1) 0.001(1) -0.012(1) C56 0.072(1) 0.082(1) 0.065(1) -0.023(1) 0.003(1) -0.041(1) C57 0.091(1) 0.103(1) 0.079(1) -0.013(1) 0.002(1) -0.049(1) C58 0.067(1) 0.089(1) 0.070(1) -0.029(1) -0.001(1) -0.042(1) C59 0.048(1) 0.062(1) 0.048(1) -0.003(1) -0.018(1) -0.013(1) C60 0.052(1) 0.070(1) 0.051(1) -0.006(1) -0.006(1) -0.035(1) C61 0.068(1) 0.085(1) 0.071(1) -0.012(1) 0.003(1) -0.046(1) C62 0.057(1) 0.069(1) 0.062(1) -0.013(1) 0.011(1) -0.041(1) C63 0.059(1) 0.051(1) 0.042(1) -0.021(1) 0.005(1) -0.014(1) C64 0.070(1) 0.062(1) 0.050(1) -0.007(1) 0.010(1) -0.017(1) C66 0.039(1) 0.076(1) 0.091(1) -0.003(1) -0.029(1) -0.029(1) C67 0.094(1) 0.108(1) 0.117(1) -0.020(1) -0.006(1) -0.055(1) C68 0.093(1) 0.111(1) 0.086(1) -0.046(1) -0.006(1) -0.042(1) C69 0.118(1) 0.134(1) 0.115(1) -0.041(1) 0.019(1) -0.075(1) C70 0.084(1) 0.109(1) 0.092(1) -0.037(1) 0.006(1) -0.061(1) C65 0.062(1) 0.089(1) 0.066(1) -0.012(1) 0.003(1) -0.044(1) C72 0.052(1) 0.078(1) 0.068(1) -0.026(1) -0.008(1) -0.027(1) C73 0.103(1) 0.118(1) 0.090(1) -0.034(1) 0.006(1) -0.058(1) C74 0.155(1) 0.170(1) 0.148(1) -0.045(1) 0.039(1) -0.079(1) C75 0.132(1) 0.144(1) 0.125(1) -0.020(1) 0.010(1) -0.070(1) C76 0.102(1) 0.102(1) 0.080(1) -0.011(1) -0.010(1) -0.042(1) C71 0.069(1) 0.102(1) 0.061(1) -0.013(1) -0.009(1) -0.038(1) C78 0.108(1) 0.125(1) 0.122(1) -0.043(1) -0.005(1) -0.042(1) C79 0.090(1) 0.119(1) 0.104(1) -0.027(1) -0.014(1) -0.019(1) C80 0.062(1) 0.114(1) 0.078(1) -0.020(1) -0.002(1) -0.042(1) C81 0.102(1) 0.135(1) 0.119(1) -0.052(1) 0.012(1) -0.071(1) C82 0.074(1) 0.087(1) 0.089(1) -0.025(1) -0.001(1) -0.037(1) C77 0.103(1) 0.107(1) 0.101(1) -0.042(1) 0.011(1) -0.061(1) C84 0.069(1) 0.075(1) 0.058(1) -0.027(1) 0.009(1) -0.036(1) C85 0.071(1) 0.099(1) 0.080(1) -0.014(1) -0.010(1) -0.048(1) C86 0.067(1) 0.085(1) 0.042(1) -0.007(1) 0.008(1) -0.038(1) C87 0.089(1) 0.085(1) 0.077(1) -0.051(1) 0.034(1) -0.038(1) C88 0.098(1) 0.089(1) 0.080(1) -0.047(1) -0.006(1) -0.050(1) C83 0.074(1) 0.083(1) 0.058(1) -0.018(1) 0.005(1) -0.029(1) O2 0.069(1) 0.054(1) 0.048(1) -0.004(1) -0.012(1) -0.024(1) C93 0.114(1) 0.117(1) 0.097(1) -0.024(1) -0.002(1) -0.064(1) C94 0.081(1) 0.077(1) 0.071(1) -0.012(1) 0.013(1) -0.016(1) C95 0.104(1) 0.104(1) 0.103(1) -0.041(1) 0.008(1) -0.047(1) C96 0.127(1) 0.128(1) 0.134(1) -0.052(1) 0.011(1) -0.059(1) O3 0.116(1) 0.128(1) 0.120(1) -0.035(1) 0.012(1) -0.048(1) C97 0.126(1) 0.129(1) 0.135(1) -0.050(1) 0.007(1) -0.058(1) C98 0.265(1) 0.261(1) 0.263(1) -0.085(1) 0.030(1) -0.114(1) C99 0.104(1) 0.112(1) 0.107(1) -0.034(1) 0.001(1) -0.044(1) C100 0.121(1) 0.117(1) 0.117(1) -0.030(1) 0.014(1) -0.049(1) O4 0.095(1) 0.090(1) 0.079(1) -0.034(1) -0.002(1) -0.034(1) C101 0.139(1) 0.138(1) 0.142(1) -0.046(1) 0.013(1) -0.050(1) C102 0.104(1) 0.108(1) 0.106(1) -0.045(1) 0.002(1) -0.046(1) C103 0.097(1) 0.105(1) 0.095(1) -0.017(1) -0.001(1) -0.027(1) C104 0.153(1) 0.149(1) 0.141(1) -0.048(1) 0.008(1) -0.073(1) _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 Y1 Cl1 2.829(5) . ? Y1 O1W 2.419(5) . ? Y1 N1 2.299(5) . ? Y1 N2 2.342(5) . ? Y1 N3 2.286(6) . ? Y1 N4 2.326(7) . ? Y1 O1 2.483(7) . ? N1 C1 1.371(10) . ? N1 C4 1.374(7) . ? N2 C6 1.377(7) . ? N2 C9 1.375(9) . ? N3 C11 1.373(9) . ? N3 C14 1.374(9) . ? N4 C16 1.380(7) . ? N4 C19 1.386(9) . ? C1 C2 1.413(8) . ? C1 C20 1.371(9) . ? C2 C3 1.550(10) . ? C3 C4 1.377(9) . ? C4 C5 1.433(10) . ? C5 C6 1.392(9) . ? C5 C21 1.524(8) . ? C6 C7 1.360(10) . ? C7 C8 1.395(9) . ? C8 C9 1.541(9) . ? C9 C10 1.361(9) . ? C10 C11 1.416(10) . ? C10 C27 1.569(9) . ? C11 C12 1.647(9) . ? C12 C13 1.320(11) . ? C13 C14 1.509(9) . ? C14 C15 1.368(10) . ? C15 C16 1.463(9) . ? C15 C33 1.477(9) . ? C16 C17 1.600(11) . ? C17 C18 1.289(8) . ? C18 C19 1.521(10) . ? C19 C20 1.375(8) . ? C20 C39 1.557(9) . ? C22 C23 1.395 . ? C22 C21 1.395 . ? C23 C24 1.395 . ? C24 C25 1.395 . ? C25 C26 1.395 . ? C26 C21 1.395 . ? C28 C29 1.395 . ? C28 C27 1.395 . ? C29 C30 1.395 . ? C30 C31 1.395 . ? C31 C32 1.395 . ? C32 C27 1.395 . ? C34 C35 1.395 . ? C34 C33 1.395 . ? C35 C36 1.395 . ? C36 C37 1.395 . ? C37 C38 1.395 . ? C38 C33 1.395 . ? C40 C41 1.395 . ? C40 C39 1.395 . ? C41 C42 1.395 . ? C42 C43 1.395 . ? C43 C44 1.395 . ? C44 C39 1.395 . ? O1 C89 1.424(10) . ? O1 C92 1.420(7) . ? C89 C90 1.498(9) . ? C90 C91 1.449(8) . ? C91 C92 1.496(11) . ? O5 C105 1.424(11) . ? O5 C108 1.425(7) . ? C105 C106 1.496(7) . ? C106 C107 1.447(10) . ? C107 C108 1.498(8) . ? Y2 Cl2 2.531(5) . ? Y2 O2W 2.344(5) . ? Y2 O3W 2.334(9) . ? Y2 N5 2.407(8) . ? Y2 N6 2.452(6) . ? Y2 N7 2.381(5) . ? Y2 N8 2.431(6) . ? N5 C45 1.383(9) . ? N5 C48 1.376(8) . ? N6 C50 1.378(9) . ? N6 C53 1.375(9) . ? N7 C55 1.374(9) . ? N7 C58 1.376(7) . ? N8 C60 1.379(8) . ? N8 C63 1.379(9) . ? C45 C46 1.327(9) . ? C45 C64 1.440(8) . ? C46 C47 1.420(9) . ? C47 C48 1.265(11) . ? C48 C49 1.252(9) . ? C49 C50 1.529(11) . ? C49 C65 1.567(9) . ? C50 C51 1.341(9) . ? C51 C52 1.364(11) . ? C52 C53 1.270(9) . ? C53 C54 1.395(10) . ? C54 C55 1.465(8) . ? C54 C71 1.461(10) . ? C55 C56 1.342(9) . ? C56 C57 1.252(9) . ? C57 C58 1.552(11) . ? C58 C59 1.396(9) . ? C59 C60 1.387(11) . ? C59 C77 1.485(8) . ? C60 C61 1.567(9) . ? C61 C62 1.191(10) . ? C62 C63 1.420(8) . ? C63 C64 1.506(9) . ? C64 C83 1.427(10) . ? C66 C67 1.395 . ? C66 C65 1.395 . ? C67 C68 1.395 . ? C68 C69 1.395 . ? C69 C70 1.395 . ? C70 C65 1.395 . ? C72 C73 1.395 . ? C72 C71 1.395 . ? C73 C74 1.395 . ? C74 C75 1.395 . ? C75 C76 1.395 . ? C76 C71 1.395 . ? C78 C79 1.395 . ? C78 C77 1.395 . ? C79 C80 1.395 . ? C80 C81 1.395 . ? C81 C82 1.395 . ? C82 C77 1.395 . ? C84 C85 1.395 . ? C84 C83 1.395 . ? C85 C86 1.395 . ? C86 C87 1.395 . ? C87 C88 1.395 . ? C88 C83 1.395 . ? O2 C93 1.425(8) . ? O2 C96 1.421(10) . ? C93 C94 1.499(7) . ? C94 C95 1.445(10) . ? C95 C96 1.498(6) . ? O3 C97 1.421(7) . ? O3 C100 1.421(11) . ? C97 C98 1.500(10) . ? C98 C99 1.448(10) . ? C99 C100 1.500(7) . ? O4 C101 1.425(11) . ? O4 C104 1.426(8) . ? C101 C102 1.498(6) . ? C102 C103 1.447(11) . ? C103 C104 1.498(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 Cl1 Y1 O1W 78.7(2) . . ? Cl1 Y1 N1 72.3(2) . . ? O1W Y1 N1 134.6(2) . . ? Cl1 Y1 N2 113.9(2) . . ? O1W Y1 N2 147.2(2) . . ? N1 Y1 N2 77.7(2) . . ? Cl1 Y1 N3 162.1(1) . . ? O1W Y1 N3 84.3(2) . . ? N1 Y1 N3 124.8(2) . . ? N2 Y1 N3 78.0(2) . . ? Cl1 Y1 N4 105.7(2) . . ? O1W Y1 N4 79.5(2) . . ? N1 Y1 N4 75.8(2) . . ? N2 Y1 N4 121.7(2) . . ? N3 Y1 N4 76.4(2) . . ? Cl1 Y1 O1 93.0(2) . . ? O1W Y1 O1 69.7(2) . . ? N1 Y1 O1 144.2(2) . . ? N2 Y1 O1 79.2(2) . . ? N3 Y1 O1 75.6(2) . . ? N4 Y1 O1 140.0(2) . . ? Y1 N1 C1 125.9(3) . . ? Y1 N1 C4 126.7(5) . . ? C1 N1 C4 106.1(5) . . ? Y1 N2 C6 127.4(4) . . ? Y1 N2 C9 118.9(3) . . ? C6 N2 C9 106.2(6) . . ? Y1 N3 C11 122.5(5) . . ? Y1 N3 C14 128.5(4) . . ? C11 N3 C14 106.8(5) . . ? Y1 N4 C16 116.9(5) . . ? Y1 N4 C19 119.1(5) . . ? C16 N4 C19 105.9(5) . . ? N1 C1 C2 111.0(5) . . ? N1 C1 C20 122.7(5) . . ? C2 C1 C20 124.3(7) . . ? C1 C2 C3 105.1(6) . . ? C2 C3 C4 101.0(5) . . ? N1 C4 C3 115.6(6) . . ? N1 C4 C5 126.7(6) . . ? C3 C4 C5 117.6(5) . . ? C4 C5 C6 127.5(5) . . ? C4 C5 C21 116.9(5) . . ? C6 C5 C21 115.4(6) . . ? N2 C6 C5 121.0(7) . . ? N2 C6 C7 114.0(6) . . ? C5 C6 C7 124.4(5) . . ? C6 C7 C8 108.0(5) . . ? C7 C8 C9 104.1(6) . . ? N2 C9 C8 107.6(5) . . ? N2 C9 C10 127.9(7) . . ? C8 C9 C10 121.3(6) . . ? C9 C10 C11 119.7(6) . . ? C9 C10 C27 122.9(6) . . ? C11 C10 C27 117.3(5) . . ? N3 C11 C10 132.3(6) . . ? N3 C11 C12 107.9(5) . . ? C10 C11 C12 119.8(5) . . ? C11 C12 C13 104.6(6) . . ? C12 C13 C14 107.9(6) . . ? N3 C14 C13 112.7(6) . . ? N3 C14 C15 125.1(6) . . ? C13 C14 C15 122.1(6) . . ? C14 C15 C16 121.2(6) . . ? C14 C15 C33 117.8(5) . . ? C16 C15 C33 120.0(6) . . ? N4 C16 C15 128.6(6) . . ? N4 C16 C17 108.0(5) . . ? C15 C16 C17 122.0(5) . . ? C16 C17 C18 105.4(6) . . ? C17 C18 C19 108.2(7) . . ? N4 C19 C18 109.1(5) . . ? N4 C19 C20 119.1(5) . . ? C18 C19 C20 125.7(7) . . ? C1 C20 C19 130.5(7) . . ? C1 C20 C39 112.5(5) . . ? C19 C20 C39 116.0(5) . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C23 C24 C25 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? C5 C21 C22 119.4(3) . . ? C5 C21 C26 120.6(3) . . ? C22 C21 C26 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C31 120.0 . . ? C30 C31 C32 120.0 . . ? C31 C32 C27 120.0 . . ? C10 C27 C28 119.5(2) . . ? C10 C27 C32 120.3(2) . . ? C28 C27 C32 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C37 120.0 . . ? C36 C37 C38 120.0 . . ? C37 C38 C33 120.0 . . ? C15 C33 C34 114.8(3) . . ? C15 C33 C38 125.2(3) . . ? C34 C33 C38 120.0 . . ? C41 C40 C39 120.0 . . ? C40 C41 C42 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C44 120.0 . . ? C43 C44 C39 120.0 . . ? C20 C39 C40 121.4(4) . . ? C20 C39 C44 118.6(4) . . ? C40 C39 C44 120.0 . . ? Y1 O1 C89 122.6(4) . . ? Y1 O1 C92 127.3(5) . . ? C89 O1 C92 109.9(6) . . ? O1 C89 C90 107.0(5) . . ? C89 C90 C91 107.8(6) . . ? C90 C91 C92 106.2(5) . . ? O1 C92 C91 108.4(6) . . ? C105 O5 C108 109.1(5) . . ? O5 C105 C106 104.3(5) . . ? C105 C106 C107 107.3(6) . . ? C106 C107 C108 105.7(4) . . ? O5 C108 C107 102.8(5) . . ? Cl2 Y2 O2W 86.0(2) . . ? Cl2 Y2 O3W 66.4(2) . . ? O2W Y2 O3W 79.1(2) . . ? Cl2 Y2 N5 124.3(2) . . ? O2W Y2 N5 73.3(2) . . ? O3W Y2 N5 149.0(2) . . ? Cl2 Y2 N6 157.2(2) . . ? O2W Y2 N6 93.3(2) . . ? O3W Y2 N6 91.0(2) . . ? N5 Y2 N6 76.8(2) . . ? Cl2 Y2 N7 98.2(2) . . ? O2W Y2 N7 155.6(3) . . ? O3W Y2 N7 80.6(2) . . ? N5 Y2 N7 121.5(2) . . ? N6 Y2 N7 73.7(2) . . ? Cl2 Y2 N8 78.5(2) . . ? O2W Y2 N8 128.7(2) . . ? O3W Y2 N8 133.7(2) . . ? N5 Y2 N8 76.1(2) . . ? N6 Y2 N8 118.5(2) . . ? N7 Y2 N8 75.5(2) . . ? Y2 N5 C45 123.9(5) . . ? Y2 N5 C48 129.3(5) . . ? C45 N5 C48 106.1(7) . . ? Y2 N6 C50 124.1(4) . . ? Y2 N6 C53 127.8(5) . . ? C50 N6 C53 106.3(5) . . ? Y2 N7 C55 126.3(3) . . ? Y2 N7 C58 118.3(4) . . ? C55 N7 C58 107.3(6) . . ? Y2 N8 C60 123.1(5) . . ? Y2 N8 C63 123.6(3) . . ? C60 N8 C63 107.2(5) . . ? N5 C45 C46 106.8(5) . . ? N5 C45 C64 130.3(7) . . ? C46 C45 C64 120.0(6) . . ? C45 C46 C47 104.3(6) . . ? C46 C47 C48 110.5(6) . . ? N5 C48 C47 107.5(6) . . ? N5 C48 C49 123.3(7) . . ? C47 C48 C49 129.1(7) . . ? C48 C49 C50 133.1(6) . . ? C48 C49 C65 117.9(6) . . ? C50 C49 C65 108.8(5) . . ? N6 C50 C49 123.0(5) . . ? N6 C50 C51 106.5(6) . . ? C49 C50 C51 130.5(6) . . ? C50 C51 C52 108.0(6) . . ? C51 C52 C53 109.4(6) . . ? N6 C53 C52 109.4(6) . . ? N6 C53 C54 121.2(6) . . ? C52 C53 C54 129.4(6) . . ? C53 C54 C55 128.6(7) . . ? C53 C54 C71 118.1(5) . . ? C55 C54 C71 112.4(6) . . ? N7 C55 C54 121.5(6) . . ? N7 C55 C56 110.3(5) . . ? C54 C55 C56 128.1(6) . . ? C55 C56 C57 112.3(7) . . ? C56 C57 C58 106.1(6) . . ? N7 C58 C57 103.4(5) . . ? N7 C58 C59 130.3(7) . . ? C57 C58 C59 126.2(5) . . ? C58 C59 C60 123.4(6) . . ? C58 C59 C77 120.9(6) . . ? C60 C59 C77 114.3(6) . . ? N8 C60 C59 126.0(6) . . ? N8 C60 C61 102.5(6) . . ? C59 C60 C61 131.3(5) . . ? C60 C61 C62 110.0(5) . . ? C61 C62 C63 109.5(6) . . ? N8 C63 C62 109.8(6) . . ? N8 C63 C64 127.0(5) . . ? C62 C63 C64 122.8(6) . . ? C45 C64 C63 118.0(6) . . ? C45 C64 C83 122.7(6) . . ? C63 C64 C83 117.6(5) . . ? C67 C66 C65 120.0 . . ? C66 C67 C68 120.0 . . ? C67 C68 C69 120.0 . . ? C68 C69 C70 120.0 . . ? C69 C70 C65 120.0 . . ? C49 C65 C66 129.1(3) . . ? C49 C65 C70 110.9(3) . . ? C66 C65 C70 120.0 . . ? C73 C72 C71 120.0 . . ? C72 C73 C74 120.0 . . ? C73 C74 C75 120.0 . . ? C74 C75 C76 120.0 . . ? C75 C76 C71 120.0 . . ? C54 C71 C72 123.7(3) . . ? C54 C71 C76 116.3(3) . . ? C72 C71 C76 120.0 . . ? C79 C78 C77 120.0 . . ? C78 C79 C80 120.0 . . ? C79 C80 C81 120.0 . . ? C80 C81 C82 120.0 . . ? C81 C82 C77 120.0 . . ? C59 C77 C78 116.8(3) . . ? C59 C77 C82 123.1(3) . . ? C78 C77 C82 120.0 . . ? C85 C84 C83 120.0 . . ? C84 C85 C86 120.0 . . ? C85 C86 C87 120.0 . . ? C86 C87 C88 120.0 . . ? C87 C88 C83 120.0 . . ? C64 C83 C84 120.0(4) . . ? C64 C83 C88 120.0(4) . . ? C84 C83 C88 120.0 . . ? C93 O2 C96 109.7(5) . . ? O2 C93 C94 103.0(5) . . ? C93 C94 C95 104.5(5) . . ? C94 C95 C96 107.5(5) . . ? O2 C96 C95 104.6(5) . . ? C97 O3 C100 111.2(5) . . ? O3 C97 C98 101.2(6) . . ? C97 C98 C99 106.8(5) . . ? C98 C99 C100 106.0(6) . . ? O3 C100 C99 104.7(5) . . ? C101 O4 C104 110.6(5) . . ? O4 C101 C102 102.4(5) . . ? C101 C102 C103 108.1(6) . . ? C102 C103 C104 103.9(5) . . ? O4 C104 C103 107.3(6) . . ? _diffrn_measured_fraction_theta_max 0.808 _diffrn_reflns_theta_full 25.59 _diffrn_measured_fraction_theta_full 0.808 _refine_diff_density_max 1.06 _refine_diff_density_min -0.35 _refine_diff_density_rms 0.091 #----------------------------------------------------------------------------- data_3 _audit_creation_method Manual _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106.50 H88 N8 O11 Yb2' _chemical_formula_weight 2001.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.807(2) _cell_length_b 18.212(2) _cell_length_c 18.864(2) _cell_angle_alpha 70.26(2) _cell_angle_beta 72.93(2) _cell_angle_gamma 68.06(2) _cell_volume 4653.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used '135 from 4 still frames' _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2022 _exptl_absorpt_coefficient_mu 2.063 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.929 _exptl_absorpt_correction_T_max 1.095 _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 ; Rigaku RU-200 rotating-anode generator powered at 50kV / 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS IIc' _diffrn_measurement_method ; Data was collected to 0.82\%A and 80% completeness by taking 45 oscillation frames in the range of 0 - 180\%, \D\f = 4\%, 8 min. per frame. Crystal to detector distance is 78.035 mm, background level -80. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13644 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0914 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.53 _reflns_number_total 13644 _reflns_number_gt 9883 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'BioteX 1.0 (MSC, 1995)' _computing_cell_refinement 'BioteX 1.0 (MSC, 1995)' _computing_data_reduction 'BioteX 1.0 (MSC, 1995)' _computing_structure_solution 'XS in SHELXTL-PC (Siemens, 1990)' _computing_structure_refinement 'XLS in SHELXTL-PC (Siemens, 1990)' _computing_molecular_graphics 'XP in SHELXTL-PC (Siemens, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F against OBSERVED reflections. The weighted R-factor Rw and goodness of fit S are based on F. The threshold expression of F > 6sigma(F) is used for all refinement. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo) + 0.0005Fo^2^]' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method -0.00020(2) _refine_ls_extinction_coef ? _refine_ls_number_reflns 9883 _refine_ls_number_parameters 1173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.80 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max 0.062 _refine_ls_shift/su_mean 0.008 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.04160(3) 0.07818(3) -0.08203(2) 0.0490(2) Uani 1 1 d D . . N1 N 0.1154(4) 0.1546(4) -0.0559(4) 0.054(1) Uani 1 1 d D . . N2 N 0.1489(4) 0.1108(4) -0.1965(3) 0.055(1) Uani 1 1 d D . . N3 N -0.0463(4) 0.1377(4) -0.1791(3) 0.052(1) Uani 1 1 d D . . N4 N -0.0827(4) 0.1751(5) -0.0364(3) 0.072(1) Uani 1 1 d D . . C1 C 0.0838(5) 0.1839(5) 0.0101(4) 0.055(1) Uani 1 1 d D . . C2 C 0.1610(5) 0.1933(5) 0.0293(4) 0.066(1) Uani 1 1 d D . . H2A H 0.1576 0.2131 0.0716 0.100 Uiso 1 1 calc R . . C3 C 0.2371(5) 0.1677(5) -0.0213(4) 0.064(1) Uani 1 1 d D . . H3A H 0.2984 0.1683 -0.0240 0.100 Uiso 1 1 calc R . . C4 C 0.2094(4) 0.1430(4) -0.0745(4) 0.054(1) Uani 1 1 d D . . C5 C 0.2670(4) 0.1192(5) -0.1396(4) 0.052(1) Uani 1 1 d D . . C6 C 0.2389(4) 0.1055(4) -0.1976(4) 0.051(1) Uani 1 1 d D . . C7 C 0.2989(5) 0.0882(5) -0.2683(4) 0.061(1) Uani 1 1 d D . . H7A H 0.3639 0.0833 -0.2832 0.100 Uiso 1 1 calc R . . C8 C 0.2455(5) 0.0820(5) -0.3090(4) 0.063(1) Uani 1 1 d D . . H8A H 0.2657 0.0712 -0.3587 0.100 Uiso 1 1 calc R . . C9 C 0.1499(5) 0.0945(4) -0.2628(4) 0.052(1) Uani 1 1 d D . . C10 C 0.0758(4) 0.0926(5) -0.2858(4) 0.060(1) Uani 1 1 d D . . C11 C -0.0162(4) 0.1128(5) -0.2457(4) 0.053(1) Uani 1 1 d D . . C12 C -0.0948(5) 0.1140(5) -0.2715(4) 0.067(1) Uani 1 1 d D . . H12A H -0.0915 0.0984 -0.3163 0.100 Uiso 1 1 calc R . . C13 C -0.1723(5) 0.1396(5) -0.2208(4) 0.063(1) Uani 1 1 d D . . H13A H -0.2349 0.1461 -0.2226 0.100 Uiso 1 1 calc R . . C14 C -0.1428(4) 0.1568(5) -0.1628(4) 0.057(1) Uani 1 1 d D . . C15 C -0.2020(4) 0.1892(5) -0.1030(4) 0.052(1) Uani 1 1 d D . . C16 C -0.1725(5) 0.2033(5) -0.0465(4) 0.055(1) Uani 1 1 d D . . C17 C -0.2350(5) 0.2453(5) 0.0087(4) 0.070(1) Uani 1 1 d D . . H17A H -0.3014 0.2650 0.0143 0.100 Uiso 1 1 calc R . . C18 C -0.1818(5) 0.2526(5) 0.0525(4) 0.066(1) Uani 1 1 d D . . H18A H -0.2041 0.2792 0.0935 0.100 Uiso 1 1 calc R . . C19 C -0.0849(4) 0.2114(4) 0.0236(4) 0.052(1) Uani 1 1 d D . . C20 C 0.0078(5) 0.2072(5) 0.0487(4) 0.060(1) Uani 1 1 d D . . C21 C 0.3702(5) 0.1041(5) -0.1476(4) 0.058(1) Uani 1 1 d D . . C22 C 0.4175(5) 0.1556(5) -0.2034(4) 0.062(1) Uani 1 1 d D . . H22A H 0.3839 0.2016 -0.2385 0.100 Uiso 1 1 calc R . . C23 C 0.5126(5) 0.1411(5) -0.2108(4) 0.066(1) Uani 1 1 d D . . H23A H 0.5430 0.1796 -0.2469 0.100 Uiso 1 1 calc R . . C24 C 0.5608(5) 0.0734(5) -0.1646(4) 0.065(1) Uani 1 1 d D . . C25 C 0.5181(5) 0.0195(5) -0.1082(4) 0.074(1) Uani 1 1 d D . . H25A H 0.5542 -0.0294 -0.0775 0.100 Uiso 1 1 calc R . . C26 C 0.4230(5) 0.0361(5) -0.0989(4) 0.076(1) Uani 1 1 d D . . H26A H 0.3916 0.0019 -0.0574 0.100 Uiso 1 1 calc R . . C27 C 0.7074(5) 0.0039(5) -0.1318(5) 0.131(1) Uani 1 1 d D . . H27A H 0.7715 -0.0054 -0.1474 0.150 Uiso 1 1 calc R . . H27B H 0.6849 0.0015 -0.0801 0.150 Uiso 1 1 calc R . . H27C H 0.7020 -0.0536 -0.1344 0.150 Uiso 1 1 calc R . . C28 C 0.0932(5) 0.0698(5) -0.3598(4) 0.060(1) Uani 1 1 d D . . C29 C 0.1453(5) 0.0085(5) -0.3643(5) 0.084(1) Uani 1 1 d D . . H29A H 0.1718 -0.0450 -0.3207 0.100 Uiso 1 1 calc R . . C30 C 0.1606(5) -0.0361(5) -0.4266(5) 0.106(1) Uani 1 1 d D . . H30A H 0.1942 -0.0919 -0.4282 0.100 Uiso 1 1 calc R . . C31 C 0.1256(5) 0.0190(5) -0.4893(4) 0.092(1) Uani 1 1 d D . . C32 C 0.0710(5) 0.1015(5) -0.4885(5) 0.086(1) Uani 1 1 d D . . H32A H 0.0458 0.1384 -0.5327 0.100 Uiso 1 1 calc R . . C33 C 0.0584(5) 0.1235(5) -0.4210(4) 0.079(1) Uani 1 1 d D . . H33A H 0.0241 0.1790 -0.4187 0.100 Uiso 1 1 calc R . . C34 C 0.1033(5) 0.0442(5) -0.6226(5) 0.161(1) Uani 1 1 d D . . H34A H 0.1200 0.0155 -0.6614 0.150 Uiso 1 1 calc R . . H34B H 0.0369 0.0644 -0.6090 0.150 Uiso 1 1 calc R . . H34C H 0.1284 0.0893 -0.6419 0.150 Uiso 1 1 calc R . . C35 C -0.3039(4) 0.2118(4) -0.0982(4) 0.052(1) Uani 1 1 d D . . C36 C -0.3573(5) 0.1701(5) -0.0366(4) 0.065(1) Uani 1 1 d D . . H36A H -0.3275 0.1293 0.0039 0.100 Uiso 1 1 calc R . . C37 C -0.4510(5) 0.1890(5) -0.0315(4) 0.074(1) Uani 1 1 d D . . H37A H -0.4867 0.1592 0.0109 0.100 Uiso 1 1 calc R . . C38 C -0.4931(5) 0.2488(5) -0.0896(4) 0.067(1) Uani 1 1 d D . . C39 C -0.4432(5) 0.2905(5) -0.1497(4) 0.070(1) Uani 1 1 d D . . H39A H -0.4735 0.3342 -0.1883 0.100 Uiso 1 1 calc R . . C40 C -0.3492(5) 0.2704(5) -0.1543(4) 0.069(1) Uani 1 1 d D . . H40A H -0.3119 0.2961 -0.1988 0.100 Uiso 1 1 calc R . . C41 C -0.6370(5) 0.3273(5) -0.1364(5) 0.089(1) Uani 1 1 d D . . H41A H -0.7024 0.3342 -0.1238 0.150 Uiso 1 1 calc R . . H41B H -0.6272 0.3782 -0.1423 0.150 Uiso 1 1 calc R . . H41C H -0.6107 0.3110 -0.1836 0.150 Uiso 1 1 calc R . . C42 C -0.0273(4) 0.2282(5) 0.1220(4) 0.058(1) Uani 1 1 d D . . C43 C -0.0579(5) 0.1804(5) 0.1895(4) 0.094(1) Uani 1 1 d D . . H43A H -0.0681 0.1313 0.1906 0.100 Uiso 1 1 calc R . . C44 C -0.0741(5) 0.2009(5) 0.2597(5) 0.112(1) Uani 1 1 d D . . H44A H -0.0965 0.1672 0.3078 0.100 Uiso 1 1 calc R . . C45 C -0.0576(5) 0.2703(5) 0.2599(4) 0.097(1) Uani 1 1 d D . . C46 C -0.0269(5) 0.3163(5) 0.1934(5) 0.102(1) Uani 1 1 d D . . H46A H -0.0137 0.3641 0.1922 0.100 Uiso 1 1 calc R . . C47 C -0.0127(5) 0.2954(5) 0.1252(4) 0.083(1) Uani 1 1 d D . . H47A H 0.0076 0.3305 0.0773 0.100 Uiso 1 1 calc R . . C48 C -0.1174(6) 0.2727(6) 0.3885(5) 0.249(1) Uani 1 1 d D . . H48A H -0.1113 0.2968 0.4241 0.150 Uiso 1 1 calc R . . H48B H -0.1804 0.2938 0.3808 0.150 Uiso 1 1 calc R . . H48C H -0.1012 0.2143 0.4086 0.150 Uiso 1 1 calc R . . O1 O 0.6536(4) 0.0640(4) -0.1811(4) 0.095(1) Uani 1 1 d D . . O2 O 0.1425(5) 0.0086(5) -0.5562(4) 0.126(1) Uani 1 1 d D . . O3 O -0.5888(4) 0.2645(4) -0.0767(4) 0.085(1) Uani 1 1 d D . . O4 O -0.0710(5) 0.2933(5) 0.3259(4) 0.161(1) Uani 1 1 d D . . O9 O 0.0485(4) 0.0043(4) 0.0402(3) 0.057(1) Uani 1 1 d D . . O10 O 0.1566(4) -0.0458(4) -0.1045(4) 0.119(1) Uani 1 1 d D . . Yb2 Yb -0.50051(3) 0.56438(3) 0.40687(2) 0.0524(2) Uani 1 1 d D . . N5 N -0.4249(4) 0.6617(4) 0.3678(4) 0.059(1) Uani 1 1 d D . . N6 N -0.6233(4) 0.6833(4) 0.3932(4) 0.057(1) Uani 1 1 d D . . N7 N -0.5801(4) 0.5453(4) 0.3313(3) 0.060(1) Uani 1 1 d D . . N8 N -0.3813(4) 0.5232(4) 0.3123(4) 0.058(1) Uani 1 1 d D . . C49 C -0.3288(5) 0.6469(5) 0.3466(4) 0.060(1) Uani 1 1 d D . . C50 C -0.3053(5) 0.7024(5) 0.3684(4) 0.070(1) Uani 1 1 d D . . H50A H -0.2427 0.7019 0.3624 0.100 Uiso 1 1 calc R . . C51 C -0.3860(5) 0.7584(5) 0.3982(4) 0.063(1) Uani 1 1 d D . . H51A H -0.3908 0.8027 0.4173 0.100 Uiso 1 1 calc R . . C52 C -0.4599(5) 0.7324(5) 0.3970(4) 0.063(1) Uani 1 1 d D . . C53 C -0.5564(5) 0.7755(5) 0.4165(4) 0.057(1) Uani 1 1 d D . . C54 C -0.6290(5) 0.7529(5) 0.4122(4) 0.056(1) Uani 1 1 d D . . C55 C -0.7246(5) 0.8025(5) 0.4265(4) 0.065(1) Uani 1 1 d D . . H55A H -0.7482 0.8529 0.4417 0.100 Uiso 1 1 calc R . . C56 C -0.7741(5) 0.7605(5) 0.4163(4) 0.069(1) Uani 1 1 d D . . H56A H -0.8406 0.7767 0.4234 0.100 Uiso 1 1 calc R . . C57 C -0.7115(4) 0.6868(5) 0.3934(4) 0.062(1) Uani 1 1 d D . . C58 C -0.7363(5) 0.6288(5) 0.3770(4) 0.056(1) Uani 1 1 d D . . C59 C -0.6779(5) 0.5657(5) 0.3464(4) 0.064(1) Uani 1 1 d D . . C60 C -0.7034(5) 0.5090(5) 0.3264(4) 0.079(1) Uani 1 1 d D . . H60A H -0.7655 0.5088 0.3313 0.100 Uiso 1 1 calc R . . C61 C -0.6247(5) 0.4556(5) 0.3011(5) 0.080(1) Uani 1 1 d D . . H61A H -0.6201 0.4106 0.2830 0.100 Uiso 1 1 calc R . . C62 C -0.5457(5) 0.4758(5) 0.3021(4) 0.061(1) Uani 1 1 d D . . C63 C -0.4489(5) 0.4363(5) 0.2766(4) 0.069(1) Uani 1 1 d D . . C64 C -0.3771(5) 0.4629(5) 0.2752(4) 0.063(1) Uani 1 1 d D . . C65 C -0.2827(5) 0.4383(5) 0.2316(4) 0.073(1) Uani 1 1 d D . . H65A H -0.2588 0.3972 0.2036 0.100 Uiso 1 1 calc R . . C66 C -0.2354(5) 0.4814(5) 0.2404(4) 0.072(1) Uani 1 1 d D . . H66A H -0.1717 0.4782 0.2172 0.100 Uiso 1 1 calc R . . C67 C -0.2954(5) 0.5334(5) 0.2889(4) 0.062(1) Uani 1 1 d D . . C68 C -0.2688(5) 0.5861(5) 0.3093(4) 0.058(1) Uani 1 1 d D . . C69 C -0.5767(5) 0.8521(5) 0.4406(4) 0.058(1) Uani 1 1 d D . . C70 C -0.5727(5) 0.8502(5) 0.5131(4) 0.081(1) Uani 1 1 d D . . H70A H -0.5565 0.7977 0.5492 0.100 Uiso 1 1 calc R . . C71 C -0.5886(5) 0.9181(5) 0.5342(5) 0.097(1) Uani 1 1 d D . . H71A H -0.5836 0.9145 0.5848 0.100 Uiso 1 1 calc R . . C72 C -0.6156(5) 0.9911(5) 0.4848(5) 0.082(1) Uani 1 1 d D . . C73 C -0.6196(5) 0.9957(5) 0.4120(5) 0.100(1) Uani 1 1 d D . . H73A H -0.6321 1.0473 0.3743 0.100 Uiso 1 1 calc R . . C74 C -0.5989(5) 0.9231(5) 0.3927(5) 0.107(1) Uani 1 1 d D . . H74A H -0.6034 0.9250 0.3425 0.100 Uiso 1 1 calc R . . C75 C -0.6725(5) 1.1413(5) 0.4664(5) 0.184(1) Uani 1 1 d D . . H75A H -0.6798 1.1795 0.4942 0.150 Uiso 1 1 calc R . . H75B H -0.6324 1.1528 0.4175 0.150 Uiso 1 1 calc R . . H75C H -0.7321 1.1464 0.4589 0.150 Uiso 1 1 calc R . . C76 C -0.8363(5) 0.6369(5) 0.3957(4) 0.062(1) Uani 1 1 d D . . C77 C -0.8925(5) 0.6782(5) 0.3432(5) 0.073(1) Uani 1 1 d D . . H77A H -0.8661 0.7024 0.2918 0.100 Uiso 1 1 calc R . . C78 C -0.9883(5) 0.6844(5) 0.3623(5) 0.077(1) Uani 1 1 d D . . H78A H -1.0262 0.7107 0.3237 0.100 Uiso 1 1 calc R . . C79 C -1.0276(5) 0.6497(5) 0.4365(5) 0.082(1) Uani 1 1 d D . . C80 C -0.9739(5) 0.6109(5) 0.4872(5) 0.133(1) Uani 1 1 d D . . H80A H -1.0005 0.5907 0.5399 0.100 Uiso 1 1 calc R . . C81 C -0.8781(5) 0.6026(5) 0.4670(5) 0.124(1) Uani 1 1 d D . . H81A H -0.8395 0.5663 0.5035 0.100 Uiso 1 1 calc R . . C82 C -1.1634(5) 0.6290(6) 0.5198(5) 0.201(1) Uani 1 1 d D . . H82A H -1.2280 0.6393 0.5216 0.150 Uiso 1 1 calc R . . H82B H -1.1326 0.5711 0.5311 0.150 Uiso 1 1 calc R . . H82C H -1.1572 0.6511 0.5569 0.150 Uiso 1 1 calc R . . C83 C -0.4243(5) 0.3609(5) 0.2512(4) 0.071(1) Uani 1 1 d D . . C84 C -0.4587(5) 0.3571(5) 0.1940(4) 0.084(1) Uani 1 1 d D . . H84A H -0.5002 0.4056 0.1675 0.100 Uiso 1 1 calc R . . C85 C -0.4322(5) 0.2834(5) 0.1740(5) 0.088(1) Uani 1 1 d D . . H85A H -0.4542 0.2817 0.1324 0.100 Uiso 1 1 calc R . . C86 C -0.3775(5) 0.2154(5) 0.2119(5) 0.084(1) Uani 1 1 d D . . C87 C -0.3457(5) 0.2160(5) 0.2711(5) 0.098(1) Uani 1 1 d D . . H87A H -0.3063 0.1663 0.2982 0.100 Uiso 1 1 calc R . . C88 C -0.3677(5) 0.2902(5) 0.2888(5) 0.091(1) Uani 1 1 d D . . H88A H -0.3434 0.2920 0.3290 0.100 Uiso 1 1 calc R . . C89 C -0.4179(5) 0.1210(5) 0.1803(5) 0.141(1) Uani 1 1 d D . . H89A H -0.3922 0.0675 0.1712 0.150 Uiso 1 1 calc R . . H89B H -0.4694 0.1216 0.2228 0.150 Uiso 1 1 calc R . . H89C H -0.4388 0.1605 0.1353 0.150 Uiso 1 1 calc R . . C90 C -0.1701(5) 0.5840(5) 0.2844(4) 0.062(1) Uani 1 1 d D . . C91 C -0.1406(5) 0.6480(5) 0.2319(4) 0.070(1) Uani 1 1 d D . . H91A H -0.1866 0.6963 0.2104 0.100 Uiso 1 1 calc R . . C92 C -0.0501(5) 0.6448(5) 0.2071(4) 0.073(1) Uani 1 1 d D . . H92A H -0.0324 0.6905 0.1703 0.100 Uiso 1 1 calc R . . C93 C 0.0174(5) 0.5775(5) 0.2378(5) 0.078(1) Uani 1 1 d D . . C94 C -0.0100(5) 0.5104(5) 0.2921(5) 0.083(1) Uani 1 1 d D . . H94A H 0.0358 0.4627 0.3146 0.100 Uiso 1 1 calc R . . C95 C -0.1047(5) 0.5171(5) 0.3126(4) 0.080(1) Uani 1 1 d D . . H95A H -0.1236 0.4715 0.3483 0.100 Uiso 1 1 calc R . . C96 C 0.1447(5) 0.6250(5) 0.1652(5) 0.103(1) Uani 1 1 d D . . H96A H 0.2114 0.6077 0.1566 0.150 Uiso 1 1 calc R . . H96B H 0.1251 0.6381 0.1176 0.150 Uiso 1 1 calc R . . H96C H 0.1203 0.6726 0.1849 0.150 Uiso 1 1 calc R . . O5 O -0.6353(5) 1.0624(4) 0.5108(4) 0.118(1) Uani 1 1 d D . . O6 O -1.1214(4) 0.6596(5) 0.4485(4) 0.110(1) Uani 1 1 d D . . O7 O -0.3515(5) 0.1394(4) 0.1951(4) 0.118(1) Uani 1 1 d D . . O8 O 0.1126(4) 0.5620(4) 0.2193(4) 0.095(1) Uani 1 1 d D . . O11 O -0.6054(5) 0.5111(5) 0.5124(5) 0.094(1) Uani 0.5 1 d P . . O12 O -0.5278(6) 0.5814(5) 0.5333(5) 0.112(1) Uani 0.5 1 d P . . C101 C -0.7677(5) 0.2719(5) 0.2546(4) 0.171(1) Uani 0.5 1 d PGD . . C102 C -0.7372 0.2153 0.2107 0.178(1) Uani 0.5 1 d PGD . . C103 C -0.6798 0.2297 0.1388 0.133(1) Uani 0.5 1 d PG . . C104 C -0.6529 0.3007 0.1108 0.132(1) Uani 0.5 1 d PG . . C105 C -0.6834 0.3572 0.1546 0.145(1) Uani 0.5 1 d PG . . C106 C -0.7408 0.3428 0.2265 0.133(1) Uani 0.5 1 d PGD . . C107 C -0.8432(5) 0.2646(5) 0.3244(5) 0.339(1) Uani 0.5 1 d PD . . C108 C 0.0962(5) 0.4581(6) -0.0159(5) 0.204(1) Uani 0.5 1 d PD . . C109 C 0.0328(5) 0.4656(5) -0.0570(5) 0.136(1) Uani 0.5 1 d PD . . C110 C -0.0607(4) 0.5062(6) -0.0390(5) 0.182(1) Uani 0.5 1 d PD . . C111 C -0.5824(4) 0.5483(5) 0.0316(5) 0.145(1) Uani 0.5 1 d PD . . C112 C -0.4943(5) 0.5465(5) 0.0314(5) 0.131(1) Uani 0.5 1 d PD . . C113 C -0.4155(5) 0.4898(5) 0.0042(6) 0.171(1) Uani 0.5 1 d PD . . 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 0.0381(2) 0.0532(3) 0.0545(2) -0.0180(2) -0.0102(2) -0.0068(2) N1 0.039(1) 0.061(1) 0.064(1) -0.022(1) -0.003(1) -0.018(1) N2 0.039(1) 0.063(1) 0.062(1) -0.018(1) -0.011(1) -0.013(1) N3 0.038(1) 0.055(1) 0.057(1) -0.016(1) -0.008(1) -0.007(1) N4 0.015(1) 0.137(1) 0.043(1) -0.007(1) -0.007(1) -0.015(1) C1 0.050(1) 0.055(1) 0.063(1) -0.022(1) -0.015(1) -0.008(1) C2 0.053(1) 0.074(1) 0.068(1) -0.023(1) -0.007(1) -0.016(1) C3 0.047(1) 0.083(1) 0.068(1) -0.011(1) -0.015(1) -0.031(1) C4 0.042(1) 0.057(1) 0.074(1) -0.019(1) -0.012(1) -0.024(1) C5 0.037(1) 0.067(1) 0.050(1) -0.020(1) -0.010(1) -0.009(1) C6 0.039(1) 0.056(1) 0.052(1) -0.020(1) -0.002(1) -0.004(1) C7 0.051(1) 0.060(1) 0.073(1) -0.029(1) 0.002(1) -0.018(1) C8 0.053(1) 0.067(1) 0.069(1) -0.019(1) -0.013(1) -0.017(1) C9 0.057(1) 0.054(1) 0.043(1) -0.029(1) -0.006(1) 0.000(1) C10 0.042(1) 0.074(1) 0.064(1) -0.024(1) -0.014(1) -0.007(1) C11 0.042(1) 0.057(1) 0.061(1) -0.011(1) -0.016(1) -0.015(1) C12 0.059(1) 0.086(1) 0.067(1) -0.032(1) -0.015(1) -0.020(1) C13 0.050(1) 0.070(1) 0.072(1) -0.030(1) -0.013(1) -0.008(1) C14 0.039(1) 0.059(1) 0.068(1) -0.017(1) -0.029(1) 0.009(1) C15 0.039(1) 0.054(1) 0.050(1) -0.009(1) -0.009(1) -0.004(1) C16 0.052(1) 0.051(1) 0.048(1) -0.021(1) 0.000(1) 0.003(1) C17 0.060(1) 0.075(1) 0.075(1) -0.031(1) -0.014(1) -0.010(1) C18 0.056(1) 0.064(1) 0.072(1) -0.023(1) -0.008(1) -0.009(1) C19 0.039(1) 0.041(1) 0.068(1) -0.007(1) -0.015(1) -0.007(1) C20 0.057(1) 0.060(1) 0.063(1) -0.018(1) -0.016(1) -0.013(1) C21 0.048(1) 0.059(1) 0.070(1) -0.026(1) -0.005(1) -0.015(1) C22 0.051(1) 0.073(1) 0.070(1) -0.023(1) -0.018(1) -0.020(1) C23 0.046(1) 0.082(1) 0.074(1) -0.034(1) -0.004(1) -0.017(1) C24 0.036(1) 0.070(1) 0.086(1) -0.015(1) -0.020(1) -0.009(1) C25 0.055(1) 0.069(1) 0.093(1) -0.024(1) -0.018(1) -0.005(1) C26 0.053(1) 0.082(1) 0.085(1) -0.027(1) -0.021(1) 0.001(1) C27 0.044(1) 0.124(1) 0.174(1) -0.026(1) -0.022(1) 0.027(1) C28 0.047(1) 0.070(1) 0.064(1) -0.014(1) -0.009(1) -0.026(1) C29 0.086(1) 0.093(1) 0.081(1) -0.037(1) -0.016(1) -0.021(1) C30 0.113(1) 0.089(1) 0.108(1) 0.002(1) -0.030(1) -0.045(1) C31 0.070(1) 0.132(1) 0.093(1) -0.020(1) -0.010(1) -0.068(1) C32 0.104(1) 0.075(1) 0.088(1) -0.027(1) -0.028(1) -0.024(1) C33 0.101(1) 0.062(1) 0.084(1) -0.012(1) -0.039(1) -0.025(1) C34 0.249(1) 0.163(1) 0.101(1) -0.063(1) -0.062(1) -0.047(1) C35 0.036(1) 0.054(1) 0.067(1) -0.020(1) -0.012(1) -0.006(1) C36 0.052(1) 0.060(1) 0.074(1) -0.016(1) -0.025(1) 0.005(1) C37 0.038(1) 0.083(1) 0.084(1) -0.019(1) -0.011(1) -0.002(1) C38 0.047(1) 0.073(1) 0.078(1) -0.019(1) -0.014(1) -0.014(1) C39 0.054(1) 0.076(1) 0.064(1) -0.018(1) -0.015(1) 0.004(1) C40 0.057(1) 0.063(1) 0.071(1) -0.021(1) -0.014(1) 0.006(1) C41 0.050(1) 0.099(1) 0.111(1) -0.015(1) -0.041(1) -0.005(1) C42 0.046(1) 0.077(1) 0.053(1) -0.025(1) -0.003(1) -0.016(1) C43 0.128(1) 0.120(1) 0.069(1) -0.067(1) -0.019(1) -0.034(1) C44 0.117(1) 0.154(1) 0.079(1) -0.074(1) -0.019(1) -0.009(1) C45 0.087(1) 0.160(1) 0.080(1) -0.051(1) -0.001(1) -0.072(1) C46 0.103(1) 0.126(1) 0.097(1) -0.038(1) -0.007(1) -0.058(1) C47 0.094(1) 0.083(1) 0.072(1) -0.030(1) -0.009(1) -0.021(1) C48 0.331(1) 0.231(1) 0.208(1) -0.122(1) -0.098(1) -0.005(1) O1 0.044(1) 0.118(1) 0.107(1) -0.021(1) -0.015(1) -0.012(1) O2 0.116(1) 0.147(1) 0.141(1) -0.029(1) -0.017(1) -0.085(1) O3 0.045(1) 0.097(1) 0.101(1) -0.021(1) -0.021(1) -0.008(1) O4 0.145(1) 0.272(1) 0.094(1) -0.093(1) 0.027(1) -0.090(1) O9 0.049(1) 0.060(1) 0.061(1) -0.028(1) -0.020(1) 0.003(1) O10 0.080(1) 0.060(1) 0.147(1) 0.004(1) 0.025(1) -0.008(1) Yb2 0.0432(2) 0.0550(3) 0.0564(2) -0.0168(2) -0.0112(2) -0.0076(2) N5 0.045(1) 0.066(1) 0.067(1) -0.022(1) -0.013(1) -0.009(1) N6 0.037(1) 0.066(1) 0.071(1) -0.011(1) -0.014(1) -0.021(1) N7 0.052(1) 0.075(1) 0.053(1) -0.022(1) -0.006(1) -0.016(1) N8 0.020(1) 0.040(1) 0.108(1) -0.011(1) 0.003(1) -0.023(1) C49 0.051(1) 0.055(1) 0.077(1) -0.028(1) -0.015(1) -0.007(1) C50 0.041(1) 0.097(1) 0.075(1) -0.027(1) -0.014(1) -0.019(1) C51 0.058(1) 0.074(1) 0.068(1) -0.035(1) -0.006(1) -0.019(1) C52 0.063(1) 0.066(1) 0.061(1) -0.023(1) -0.009(1) -0.014(1) C53 0.056(1) 0.045(1) 0.061(1) -0.012(1) -0.012(1) -0.006(1) C54 0.051(1) 0.052(1) 0.065(1) -0.018(1) -0.012(1) -0.013(1) C55 0.061(1) 0.067(1) 0.075(1) -0.018(1) -0.016(1) -0.028(1) C56 0.057(1) 0.067(1) 0.070(1) -0.010(1) -0.013(1) -0.009(1) C57 0.029(1) 0.067(1) 0.065(1) 0.001(1) -0.008(1) -0.007(1) C58 0.050(1) 0.065(1) 0.057(1) -0.023(1) -0.007(1) -0.018(1) C59 0.040(1) 0.076(1) 0.069(1) -0.018(1) -0.007(1) -0.014(1) C60 0.055(1) 0.098(1) 0.103(1) -0.029(1) -0.019(1) -0.042(1) C61 0.067(1) 0.077(1) 0.120(1) -0.031(1) -0.018(1) -0.043(1) C62 0.055(1) 0.070(1) 0.066(1) -0.026(1) -0.009(1) -0.021(1) C63 0.062(1) 0.080(1) 0.065(1) -0.025(1) -0.001(1) -0.026(1) C64 0.053(1) 0.067(1) 0.071(1) -0.030(1) -0.005(1) -0.013(1) C65 0.062(1) 0.060(1) 0.085(1) -0.008(1) -0.013(1) -0.018(1) C66 0.047(1) 0.075(1) 0.084(1) -0.013(1) -0.010(1) -0.017(1) C67 0.045(1) 0.082(1) 0.052(1) -0.023(1) 0.003(1) -0.016(1) C68 0.057(1) 0.043(1) 0.063(1) -0.021(1) -0.008(1) 0.004(1) C69 0.054(1) 0.063(1) 0.059(1) -0.023(1) -0.016(1) -0.008(1) C70 0.091(1) 0.080(1) 0.084(1) -0.029(1) -0.011(1) -0.036(1) C71 0.110(1) 0.101(1) 0.097(1) -0.032(1) -0.015(1) -0.048(1) C72 0.071(1) 0.096(1) 0.102(1) -0.037(1) 0.002(1) -0.053(1) C73 0.124(1) 0.075(1) 0.098(1) -0.018(1) -0.028(1) -0.027(1) C74 0.157(1) 0.085(1) 0.091(1) -0.017(1) -0.036(1) -0.049(1) C75 0.268(1) 0.056(1) 0.278(1) -0.015(1) -0.166(1) -0.045(1) C76 0.053(1) 0.073(1) 0.069(1) -0.026(1) -0.019(1) -0.014(1) C77 0.061(1) 0.074(1) 0.085(1) -0.032(1) -0.009(1) -0.015(1) C78 0.060(1) 0.077(1) 0.104(1) -0.031(1) -0.028(1) -0.013(1) C79 0.062(1) 0.097(1) 0.099(1) -0.037(1) -0.023(1) -0.019(1) C80 0.072(1) 0.228(1) 0.073(1) -0.054(1) 0.001(1) -0.012(1) C81 0.064(1) 0.212(1) 0.080(1) -0.059(1) -0.024(1) 0.009(1) C82 0.081(1) 0.293(1) 0.151(1) -0.063(1) 0.017(1) 0.010(1) C83 0.068(1) 0.066(1) 0.081(1) -0.026(1) -0.004(1) -0.023(1) C84 0.089(1) 0.065(1) 0.096(1) 0.000(1) -0.029(1) -0.034(1) C85 0.084(1) 0.089(1) 0.096(1) -0.020(1) -0.028(1) -0.028(1) C86 0.082(1) 0.079(1) 0.096(1) -0.021(1) -0.005(1) -0.044(1) C87 0.117(1) 0.067(1) 0.108(1) -0.010(1) -0.042(1) -0.024(1) C88 0.100(1) 0.072(1) 0.096(1) -0.009(1) -0.032(1) -0.025(1) C89 0.147(1) 0.106(1) 0.209(1) -0.024(1) -0.074(1) -0.069(1) C90 0.046(1) 0.059(1) 0.074(1) -0.015(1) -0.014(1) -0.009(1) C91 0.052(1) 0.058(1) 0.073(1) -0.006(1) -0.016(1) 0.008(1) C92 0.062(1) 0.063(1) 0.087(1) -0.015(1) -0.022(1) -0.010(1) C93 0.058(1) 0.083(1) 0.092(1) -0.040(1) 0.000(1) -0.014(1) C94 0.047(1) 0.075(1) 0.106(1) -0.015(1) -0.021(1) 0.004(1) C95 0.058(1) 0.082(1) 0.086(1) -0.037(1) -0.004(1) 0.005(1) C96 0.085(1) 0.087(1) 0.133(1) -0.056(1) -0.005(1) -0.003(1) O5 0.110(1) 0.134(1) 0.152(1) -0.047(1) -0.007(1) -0.091(1) O6 0.036(1) 0.162(1) 0.125(1) -0.024(1) -0.011(1) -0.039(1) O7 0.107(1) 0.079(1) 0.167(1) -0.025(1) -0.004(1) -0.055(1) O8 0.049(1) 0.085(1) 0.123(1) -0.028(1) -0.003(1) 0.007(1) O11 0.070(1) 0.124(1) 0.038(1) -0.025(1) -0.022(1) 0.044(1) O12 0.202(1) 0.106(1) 0.031(1) -0.080(1) -0.026(1) 0.018(1) C101 0.103(1) 0.215(1) 0.139(1) -0.022(1) 0.003(1) -0.032(1) C102 0.127(1) 0.222(1) 0.169(1) -0.014(1) -0.040(1) -0.064(1) C103 0.087(1) 0.184(1) 0.138(1) -0.047(1) -0.032(1) -0.039(1) C104 0.124(1) 0.178(1) 0.122(1) -0.043(1) -0.037(1) -0.064(1) C105 0.084(1) 0.195(1) 0.145(1) -0.017(1) -0.043(1) -0.039(1) C106 0.098(1) 0.178(1) 0.146(1) -0.060(1) -0.046(1) -0.029(1) C107 0.289(1) 0.303(1) 0.259(1) 0.106(1) -0.156(1) -0.002(1) C108 0.354(1) 0.120(1) 0.141(1) -0.169(1) 0.093(1) -0.050(1) C109 0.308(1) 0.105(1) 0.038(1) -0.149(1) 0.023(1) -0.023(1) C110 0.342(1) 0.132(1) 0.100(1) -0.168(1) -0.007(1) 0.014(1) C111 0.172(1) 0.046(1) 0.093(1) 0.043(1) 0.021(1) 0.008(1) C112 0.207(1) 0.049(1) 0.105(1) -0.070(1) 0.017(1) 0.013(1) C113 0.230(1) 0.122(1) 0.107(1) -0.086(1) -0.008(1) 0.052(1) _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 N1 2.357(9) . ? Yb1 N2 2.373(6) . ? Yb1 N3 2.343(7) . ? Yb1 N4 2.271(6) . ? Yb1 O9 2.255(5) . ? Yb1 O10 2.389(6) . ? Yb1 Yb1 3.724(1) 2 ? Yb1 O9 2.247(7) 2 ? N1 C1 1.403(11) . ? N1 C4 1.372(9) . ? N2 C6 1.385(10) . ? N2 C9 1.374(12) . ? N3 C11 1.372(11) . ? N3 C14 1.393(9) . ? N4 C16 1.366(9) . ? N4 C19 1.477(13) . ? C1 C2 1.452(13) . ? C1 C20 1.392(9) . ? C2 C3 1.335(9) . ? C3 C4 1.454(14) . ? C4 C5 1.390(10) . ? C5 C6 1.417(13) . ? C5 C21 1.519(10) . ? C6 C7 1.447(10) . ? C7 C8 1.351(14) . ? C8 C9 1.484(9) . ? C9 C10 1.378(12) . ? C10 C11 1.401(9) . ? C10 C28 1.510(12) . ? C11 C12 1.452(12) . ? C12 C13 1.349(9) . ? C13 C14 1.469(14) . ? C14 C15 1.382(10) . ? C15 C16 1.407(13) . ? C15 C35 1.489(10) . ? C16 C17 1.421(10) . ? C17 C18 1.404(14) . ? C18 C19 1.460(8) . ? C19 C20 1.400(12) . ? C20 C42 1.473(12) . ? C21 C22 1.394(10) . ? C21 C26 1.409(9) . ? C22 C23 1.398(10) . ? C23 C24 1.350(9) . ? C24 C25 1.385(10) . ? C24 O1 1.363(9) . ? C25 C26 1.386(10) . ? C27 O1 1.421(9) . ? C28 C29 1.371(11) . ? C28 C33 1.341(10) . ? C29 C30 1.355(14) . ? C30 C31 1.370(11) . ? C31 C32 1.429(11) . ? C31 O2 1.430(13) . ? C32 C33 1.401(13) . ? C34 O2 1.440(11) . ? C35 C36 1.396(10) . ? C35 C40 1.372(9) . ? C36 C37 1.372(10) . ? C37 C38 1.381(10) . ? C38 C39 1.351(10) . ? C38 O3 1.392(9) . ? C39 C40 1.374(10) . ? C41 O3 1.464(9) . ? C42 C43 1.347(9) . ? C42 C47 1.351(14) . ? C43 C44 1.423(13) . ? C44 C45 1.382(15) . ? C45 C46 1.321(10) . ? C45 O4 1.379(13) . ? C46 C47 1.396(14) . ? C48 O4 1.213(10) . ? O9 Yb1 2.247(7) 2 ? Yb2 N5 2.301(8) . ? Yb2 N6 2.302(6) . ? Yb2 N7 2.335(9) . ? Yb2 N8 2.274(6) . ? Yb2 O11 2.370(8) . ? Yb2 O12 2.401(9) . ? Yb2 Yb2 3.505(1) 2_466 ? Yb2 O11 2.318(8) 2_466 ? Yb2 O12 2.430(9) 2_466 ? N5 C49 1.397(9) . ? N5 C52 1.427(12) . ? N6 C54 1.395(13) . ? N6 C57 1.371(10) . ? N7 C59 1.412(9) . ? N7 C62 1.407(12) . ? N8 C64 1.463(13) . ? N8 C67 1.362(10) . ? C49 C50 1.406(14) . ? C49 C68 1.405(11) . ? C50 C51 1.406(9) . ? C51 C52 1.423(13) . ? C52 C53 1.432(9) . ? C53 C54 1.387(13) . ? C53 C69 1.504(13) . ? C54 C55 1.442(9) . ? C55 C56 1.368(14) . ? C56 C57 1.454(11) . ? C57 C58 1.401(14) . ? C58 C59 1.360(11) . ? C58 C76 1.476(10) . ? C59 C60 1.427(15) . ? C60 C61 1.335(9) . ? C61 C62 1.433(13) . ? C62 C63 1.439(9) . ? C63 C64 1.382(13) . ? C63 C83 1.483(13) . ? C64 C65 1.461(9) . ? C65 C66 1.342(14) . ? C66 C67 1.429(11) . ? C67 C68 1.375(14) . ? C68 C90 1.480(10) . ? C69 C70 1.376(12) . ? C69 C74 1.291(10) . ? C70 C71 1.339(14) . ? C71 C72 1.338(10) . ? C72 C73 1.367(13) . ? C72 O5 1.435(13) . ? C73 C74 1.385(14) . ? C75 O5 1.399(10) . ? C76 C77 1.360(11) . ? C76 C81 1.361(10) . ? C77 C78 1.420(11) . ? C78 C79 1.389(10) . ? C79 C80 1.307(12) . ? C79 O6 1.382(10) . ? C80 C81 1.412(11) . ? C82 O6 1.344(10) . ? C83 C84 1.374(14) . ? C83 C88 1.362(9) . ? C84 C85 1.397(13) . ? C85 C86 1.325(10) . ? C86 C87 1.358(14) . ? C86 O7 1.406(13) . ? C87 C88 1.393(14) . ? C89 O7 1.337(14) . ? C90 C91 1.383(11) . ? C90 C95 1.334(9) . ? C91 C92 1.353(10) . ? C92 C93 1.373(9) . ? C93 C94 1.421(11) . ? C93 O8 1.382(9) . ? C94 C95 1.400(10) . ? C96 O8 1.398(10) . ? O11 Yb2 2.318(8) 2_466 ? O12 Yb2 2.430(9) 2_466 ? C101 C107 1.501(10) . ? C108 C109 1.381(14) . ? C108 C110 1.283(15) 2_565 ? C109 C110 1.380(9) . ? C110 C108 1.283(15) 2_565 ? C111 C112 1.379(12) . ? C111 C113 1.135(17) 2_465 ? C112 C113 1.380(10) . ? C113 C111 1.135(17) 2_465 ? 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 N1 Yb1 N2 74.8(3) . . ? N1 Yb1 N3 120.2(2) . . ? N2 Yb1 N3 75.0(2) . . ? N1 Yb1 N4 78.7(3) . . ? N2 Yb1 N4 122.6(2) . . ? N3 Yb1 N4 76.1(2) . . ? N1 Yb1 O9 84.3(2) . . ? N2 Yb1 O9 136.8(2) . . ? N3 Yb1 O9 146.7(2) . . ? N4 Yb1 O9 88.5(2) . . ? N1 Yb1 O10 107.8(3) . . ? N2 Yb1 O10 71.2(2) . . ? N3 Yb1 O10 109.3(3) . . ? N4 Yb1 O10 166.2(2) . . ? O9 Yb1 O10 80.3(2) . . ? N1 Yb1 Yb1 117.5(1) . 2 ? N2 Yb1 Yb1 149.7(2) . 2 ? N3 Yb1 Yb1 114.7(2) . 2 ? N4 Yb1 Yb1 87.7(2) . 2 ? O9 Yb1 Yb1 34.1(2) . 2 ? O10 Yb1 Yb1 78.6(2) . 2 ? N1 Yb1 O9 149.8(2) . 2 ? N2 Yb1 O9 134.4(3) . 2 ? N3 Yb1 O9 81.5(2) . 2 ? N4 Yb1 O9 87.7(2) . 2 ? O9 Yb1 O9 68.3(3) . 2 ? O10 Yb1 O9 80.8(2) . 2 ? Yb1 Yb1 O9 34.2(2) 2 2 ? Yb1 N1 C1 122.4(5) . . ? Yb1 N1 C4 124.7(6) . . ? C1 N1 C4 105.5(7) . . ? Yb1 N2 C6 123.4(5) . . ? Yb1 N2 C9 121.5(6) . . ? C6 N2 C9 107.2(6) . . ? Yb1 N3 C11 121.0(4) . . ? Yb1 N3 C14 121.9(4) . . ? C11 N3 C14 106.4(7) . . ? Yb1 N4 C16 130.3(7) . . ? Yb1 N4 C19 124.6(4) . . ? C16 N4 C19 104.4(6) . . ? N1 C1 C2 109.3(6) . . ? N1 C1 C20 126.5(8) . . ? C2 C1 C20 123.9(8) . . ? C1 C2 C3 107.4(8) . . ? C2 C3 C4 107.6(7) . . ? N1 C4 C3 110.1(6) . . ? N1 C4 C5 124.2(8) . . ? C3 C4 C5 125.4(7) . . ? C4 C5 C6 126.3(7) . . ? C4 C5 C21 116.4(8) . . ? C6 C5 C21 117.3(6) . . ? N2 C6 C5 124.8(6) . . ? N2 C6 C7 110.1(8) . . ? C5 C6 C7 125.1(7) . . ? C6 C7 C8 106.9(6) . . ? C7 C8 C9 107.6(7) . . ? N2 C9 C8 108.2(7) . . ? N2 C9 C10 127.4(6) . . ? C8 C9 C10 124.4(7) . . ? C9 C10 C11 124.1(8) . . ? C9 C10 C28 118.6(6) . . ? C11 C10 C28 117.2(8) . . ? N3 C11 C10 125.8(8) . . ? N3 C11 C12 109.9(6) . . ? C10 C11 C12 124.2(8) . . ? C11 C12 C13 107.8(8) . . ? C12 C13 C14 106.7(7) . . ? N3 C14 C13 109.1(6) . . ? N3 C14 C15 125.8(9) . . ? C13 C14 C15 125.1(7) . . ? C14 C15 C16 124.5(7) . . ? C14 C15 C35 118.1(8) . . ? C16 C15 C35 117.5(6) . . ? N4 C16 C15 124.2(6) . . ? N4 C16 C17 112.8(8) . . ? C15 C16 C17 122.9(7) . . ? C16 C17 C18 107.5(6) . . ? C17 C18 C19 106.5(7) . . ? N4 C19 C18 108.2(7) . . ? N4 C19 C20 126.2(6) . . ? C18 C19 C20 125.6(8) . . ? C1 C20 C19 124.7(8) . . ? C1 C20 C42 119.1(8) . . ? C19 C20 C42 116.2(6) . . ? C5 C21 C22 122.2(6) . . ? C5 C21 C26 121.1(6) . . ? C22 C21 C26 116.7(6) . . ? C21 C22 C23 122.0(6) . . ? C22 C23 C24 119.0(7) . . ? C23 C24 C25 121.9(7) . . ? C23 C24 O1 112.9(6) . . ? C25 C24 O1 125.1(6) . . ? C24 C25 C26 118.8(6) . . ? C21 C26 C25 121.5(7) . . ? C10 C28 C29 119.0(6) . . ? C10 C28 C33 121.9(7) . . ? C29 C28 C33 119.1(8) . . ? C28 C29 C30 123.5(7) . . ? C29 C30 C31 117.3(8) . . ? C30 C31 C32 122.0(9) . . ? C30 C31 O2 118.3(7) . . ? C32 C31 O2 119.7(7) . . ? C31 C32 C33 116.0(7) . . ? C28 C33 C32 122.0(7) . . ? C15 C35 C36 120.2(6) . . ? C15 C35 C40 123.0(6) . . ? C36 C35 C40 116.7(6) . . ? C35 C36 C37 121.3(6) . . ? C36 C37 C38 119.5(6) . . ? C37 C38 C39 120.5(7) . . ? C37 C38 O3 114.1(6) . . ? C39 C38 O3 125.2(6) . . ? C38 C39 C40 119.3(6) . . ? C35 C40 C39 122.6(6) . . ? C20 C42 C43 122.1(9) . . ? C20 C42 C47 121.5(6) . . ? C43 C42 C47 116.4(8) . . ? C42 C43 C44 121.1(9) . . ? C43 C44 C45 120.2(7) . . ? C44 C45 C46 118.2(9) . . ? C44 C45 O4 123.2(7) . . ? C46 C45 O4 118.6(10) . . ? C45 C46 C47 120.5(10) . . ? C42 C47 C46 123.6(7) . . ? C24 O1 C27 115.6(6) . . ? C31 O2 C34 121.6(7) . . ? C38 O3 C41 116.5(6) . . ? C45 O4 C48 129.0(11) . . ? Yb1 O9 Yb1 111.7(3) . 2 ? N5 Yb2 N6 78.8(2) . . ? N5 Yb2 N7 124.6(2) . . ? N6 Yb2 N7 77.3(3) . . ? N5 Yb2 N8 76.3(3) . . ? N6 Yb2 N8 126.6(2) . . ? N7 Yb2 N8 79.3(2) . . ? N5 Yb2 O11 140.5(3) . . ? N6 Yb2 O11 84.8(2) . . ? N7 Yb2 O11 85.4(3) . . ? N8 Yb2 O11 139.8(3) . . ? N5 Yb2 O12 85.7(3) . . ? N6 Yb2 O12 82.6(3) . . ? N7 Yb2 O12 138.3(3) . . ? N8 Yb2 O12 140.4(3) . . ? O11 Yb2 O12 56.5(4) . . ? N5 Yb2 Yb2 118.5(2) . 2_466 ? N6 Yb2 Yb2 116.0(1) . 2_466 ? N7 Yb2 Yb2 116.9(2) . 2_466 ? N8 Yb2 Yb2 117.5(1) . 2_466 ? O11 Yb2 Yb2 41.1(2) . 2_466 ? O12 Yb2 Yb2 43.8(2) . 2_466 ? N5 Yb2 O11 86.1(3) . 2_466 ? N6 Yb2 O11 139.0(3) . 2_466 ? N7 Yb2 O11 140.1(3) . 2_466 ? N8 Yb2 O11 85.2(2) . 2_466 ? O11 Yb2 O11 83.2(3) . 2_466 ? O12 Yb2 O11 58.2(3) . 2_466 ? Yb2 Yb2 O11 42.2(2) 2_466 2_466 ? N5 Yb2 O12 139.5(3) . 2_466 ? N6 Yb2 O12 139.3(3) . 2_466 ? N7 Yb2 O12 85.1(3) . 2_466 ? N8 Yb2 O12 84.5(2) . 2_466 ? O11 Yb2 O12 57.2(3) . 2_466 ? O12 Yb2 O12 87.0(4) . 2_466 ? Yb2 Yb2 O12 43.2(2) 2_466 2_466 ? O11 Yb2 O12 56.7(4) 2_466 2_466 ? Yb2 N5 C49 125.8(5) . . ? Yb2 N5 C52 122.2(4) . . ? C49 N5 C52 105.5(8) . . ? Yb2 N6 C54 123.9(5) . . ? Yb2 N6 C57 124.1(6) . . ? C54 N6 C57 108.0(6) . . ? Yb2 N7 C59 122.3(6) . . ? Yb2 N7 C62 121.5(5) . . ? C59 N7 C62 106.3(8) . . ? Yb2 N8 C64 123.2(5) . . ? Yb2 N8 C67 130.3(7) . . ? C64 N8 C67 105.3(6) . . ? N5 C49 C50 108.7(7) . . ? N5 C49 C68 123.6(9) . . ? C50 C49 C68 127.7(7) . . ? C49 C50 C51 110.4(7) . . ? C50 C51 C52 104.2(8) . . ? N5 C52 C51 110.9(6) . . ? N5 C52 C53 124.6(8) . . ? C51 C52 C53 124.3(8) . . ? C52 C53 C54 124.9(8) . . ? C52 C53 C69 115.2(8) . . ? C54 C53 C69 119.9(6) . . ? N6 C54 C53 127.6(6) . . ? N6 C54 C55 110.1(8) . . ? C53 C54 C55 122.2(8) . . ? C54 C55 C56 104.7(7) . . ? C55 C56 C57 110.2(6) . . ? N6 C57 C56 106.9(8) . . ? N6 C57 C58 126.3(6) . . ? C56 C57 C58 126.8(7) . . ? C57 C58 C59 126.8(7) . . ? C57 C58 C76 116.4(6) . . ? C59 C58 C76 116.8(9) . . ? N7 C59 C58 124.0(9) . . ? N7 C59 C60 109.1(7) . . ? C58 C59 C60 126.9(7) . . ? C59 C60 C61 107.1(8) . . ? C60 C61 C62 110.5(9) . . ? N7 C62 C61 107.0(6) . . ? N7 C62 C63 124.7(8) . . ? C61 C62 C63 128.3(8) . . ? C62 C63 C64 124.6(8) . . ? C62 C63 C83 117.8(8) . . ? C64 C63 C83 117.6(6) . . ? N8 C64 C63 127.5(6) . . ? N8 C64 C65 107.1(7) . . ? C63 C64 C65 125.2(9) . . ? C64 C65 C66 107.6(8) . . ? C65 C66 C67 109.0(7) . . ? N8 C67 C66 111.0(8) . . ? N8 C67 C68 125.1(7) . . ? C66 C67 C68 123.9(7) . . ? C49 C68 C67 125.4(7) . . ? C49 C68 C90 116.4(8) . . ? C67 C68 C90 117.9(7) . . ? C53 C69 C70 122.4(6) . . ? C53 C69 C74 120.2(8) . . ? C70 C69 C74 117.4(9) . . ? C69 C70 C71 122.5(7) . . ? C70 C71 C72 119.0(9) . . ? C71 C72 C73 120.1(9) . . ? C71 C72 O5 117.1(8) . . ? C73 C72 O5 122.7(7) . . ? C72 C73 C74 118.0(7) . . ? C69 C74 C73 122.8(9) . . ? C58 C76 C77 122.6(6) . . ? C58 C76 C81 121.8(7) . . ? C77 C76 C81 115.6(7) . . ? C76 C77 C78 121.6(6) . . ? C77 C78 C79 120.2(7) . . ? C78 C79 C80 118.2(7) . . ? C78 C79 O6 115.2(7) . . ? C80 C79 O6 126.5(7) . . ? C79 C80 C81 121.1(7) . . ? C76 C81 C80 123.2(7) . . ? C63 C83 C84 123.8(6) . . ? C63 C83 C88 118.6(9) . . ? C84 C83 C88 117.6(9) . . ? C83 C84 C85 120.0(7) . . ? C84 C85 C86 121.0(9) . . ? C85 C86 C87 120.5(9) . . ? C85 C86 O7 122.8(9) . . ? C87 C86 O7 116.6(7) . . ? C86 C87 C88 118.8(7) . . ? C83 C88 C87 121.9(9) . . ? C68 C90 C91 123.5(6) . . ? C68 C90 C95 119.5(7) . . ? C91 C90 C95 117.0(7) . . ? C90 C91 C92 123.5(6) . . ? C91 C92 C93 119.9(7) . . ? C92 C93 C94 118.3(7) . . ? C92 C93 O8 128.6(7) . . ? C94 C93 O8 112.9(6) . . ? C93 C94 C95 118.3(6) . . ? C90 C95 C94 122.9(7) . . ? C72 O5 C75 121.5(8) . . ? C79 O6 C82 117.6(7) . . ? C86 O7 C89 116.6(6) . . ? C93 O8 C96 116.0(6) . . ? Yb2 O11 Yb2 96.8(3) . 2_464 ? Yb2 O12 Yb2 93.0(4) . 2_464 ? C102 C101 C107 119.7(6) . . ? C106 C101 C107 119.2(5) . . ? C109 C108 C110 114.1(7) . 2_565 ? C108 C109 C110 122.5(9) . . ? C109 C110 C108 123.4(10) . 2_565 ? C112 C111 C113 114.5(8) . 2_465 ? C111 C112 C113 122.2(10) . . ? C112 C113 C111 121.8(9) . 2_465 ? _diffrn_measured_fraction_theta_max 0.785 _diffrn_reflns_theta_full 25.53 _diffrn_measured_fraction_theta_full 0.785 _refine_diff_density_max 3.88 _refine_diff_density_min -0.78 _refine_diff_density_rms 0.175 #----------------------------------------------------------------------------- data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H82.50 N8 O3.25 Yb2' _chemical_formula_weight 1794.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Yb' 'Yb' -0.3850 5.5486 '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 16.758(1) _cell_length_b 27.758(1) _cell_length_c 20.303(1) _cell_angle_alpha 90.00 _cell_angle_beta 108.09(1) _cell_angle_gamma 90.00 _cell_volume 8977.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used '132 from 4 still photos' _cell_measurement_theta_min 26 _cell_measurement_theta_max 2 _exptl_crystal_description plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3618 _exptl_absorpt_coefficient_mu 2.124 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 1.194 _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 ; Rigaku RU-200 rotating-anode generator powered at 50kV/90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS IIc' _diffrn_measurement_method ; Data was collected at 0.82\%A and 88% completeness by taking 60 oscillation frames in the range of 0 - 180\%, \D\f = 3\%, 8 min. per frame. Crystal to detector distance is 77.865mm, background level -80. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12384 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 24.00 _reflns_number_total 12384 _reflns_number_gt 11177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BioteX 1.0 (MSC, 1995)' _computing_cell_refinement 'BioteX 1.0 (MSC, 1995)' _computing_data_reduction 'BioteX 1.0 (MSC, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PC (Siemens, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+79.9221P] 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 SHELXL _refine_ls_extinction_coef 0.00000(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12384 _refine_ls_number_parameters 1055 _refine_ls_number_restraints 1159 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0888 _refine_ls_wR_factor_ref 0.1872 _refine_ls_wR_factor_gt 0.1809 _refine_ls_goodness_of_fit_ref 1.235 _refine_ls_restrained_S_all 1.189 _refine_ls_shift/su_max 0.145 _refine_ls_shift/su_mean 0.002 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.027939(19) 0.803936(12) 0.944727(17) 0.04913(9) Uani 1 1 d . . . N1 N -0.0087(3) 0.8540(2) 1.0235(3) 0.0546(16) Uani 1 1 d DU . . N2 N 0.1589(3) 0.8276(2) 1.0185(3) 0.0531(16) Uani 1 1 d DU . . N3 N 0.0986(3) 0.7312(2) 0.9765(3) 0.0514(16) Uani 1 1 d DU . . N4 N -0.0651(3) 0.7584(2) 0.9850(3) 0.0520(15) Uani 1 1 d DU . . C1 C -0.0889(4) 0.8590(3) 1.0268(4) 0.061(2) Uani 1 1 d DU . . C2 C -0.0966(5) 0.9048(3) 1.0594(4) 0.069(2) Uani 1 1 d DU . . H2 H -0.1449 0.9171 1.0666 0.083 Uiso 1 1 calc R . . C3 C -0.0202(5) 0.9260(3) 1.0771(5) 0.074(2) Uani 1 1 d DU . . H3 H -0.0059 0.9556 1.0991 0.088 Uiso 1 1 calc R . . C4 C 0.0355(5) 0.8940(3) 1.0554(4) 0.0559(19) Uani 1 1 d DU . . C5 C 0.1212(5) 0.9029(3) 1.0647(4) 0.0612(19) Uani 1 1 d U . . C6 C 0.1763(4) 0.8729(3) 1.0469(4) 0.0552(19) Uani 1 1 d DU . . C7 C 0.2649(5) 0.8822(3) 1.0590(4) 0.067(2) Uani 1 1 d DU . . H7 H 0.2937 0.9100 1.0784 0.080 Uiso 1 1 calc R . . C8 C 0.2988(4) 0.8426(3) 1.0366(4) 0.062(2) Uani 1 1 d DU . . H8 H 0.3539 0.8389 1.0364 0.074 Uiso 1 1 calc R . . C9 C 0.2325(4) 0.8083(3) 1.0139(4) 0.0529(18) Uani 1 1 d DU . . C10 C 0.2437(4) 0.7619(3) 0.9952(4) 0.0555(18) Uani 1 1 d U . . C11 C 0.1819(4) 0.7247(3) 0.9824(4) 0.056(2) Uani 1 1 d DU . . C12 C 0.1994(5) 0.6744(3) 0.9791(4) 0.065(2) Uani 1 1 d DU . . H12 H 0.2504 0.6605 0.9804 0.078 Uiso 1 1 calc R . . C13 C 0.1264(5) 0.6510(3) 0.9736(4) 0.069(2) Uani 1 1 d DU . . H13 H 0.1183 0.6179 0.9713 0.083 Uiso 1 1 calc R . . C14 C 0.0653(5) 0.6862(3) 0.9719(4) 0.057(2) Uani 1 1 d DU . . C15 C -0.0185(5) 0.6758(3) 0.9702(4) 0.0576(17) Uani 1 1 d U . . C16 C -0.0806(4) 0.7107(3) 0.9721(3) 0.0533(17) Uani 1 1 d DU . . C17 C -0.1668(5) 0.6984(3) 0.9655(4) 0.066(2) Uani 1 1 d DU . . H17 H -0.1913 0.6681 0.9567 0.079 Uiso 1 1 calc R . . C18 C -0.2042(5) 0.7394(3) 0.9745(4) 0.063(2) Uani 1 1 d DU . . H18 H -0.2600 0.7429 0.9730 0.076 Uiso 1 1 calc R . . C19 C -0.1402(4) 0.7778(3) 0.9874(4) 0.0553(19) Uani 1 1 d DU . . C20 C -0.1523(4) 0.8241(3) 1.0050(4) 0.0584(18) Uani 1 1 d U . . C21 C 0.1599(4) 0.9478(2) 1.1039(3) 0.0615(19) Uani 1 1 d DU . . C22 C 0.1776(4) 0.9510(2) 1.1751(3) 0.077(2) Uani 1 1 d DU . . H22 H 0.1575 0.9274 1.1983 0.092 Uiso 1 1 calc R . . C23 C 0.2246(4) 0.9888(2) 1.2123(4) 0.082(3) Uani 1 1 d DU . . H23 H 0.2369 0.9898 1.2602 0.099 Uiso 1 1 calc R . . C24 C 0.2527(5) 1.0243(3) 1.1792(3) 0.089(3) Uani 1 1 d DU . . C25 C 0.2334(5) 1.0222(3) 1.1087(3) 0.091(3) Uani 1 1 d DU . . H25 H 0.2520 1.0467 1.0857 0.109 Uiso 1 1 calc R . . C26 C 0.1870(5) 0.9848(2) 1.0707(4) 0.081(3) Uani 1 1 d DU . . H26 H 0.1739 0.9844 1.0227 0.098 Uiso 1 1 calc R . . C27 C 0.3094(6) 1.0646(3) 1.2195(6) 0.135(4) Uani 1 1 d DU . . H27A H 0.3238 1.0858 1.1876 0.202 Uiso 1 1 calc R . . H27B H 0.3597 1.0508 1.2504 0.202 Uiso 1 1 calc R . . H27C H 0.2804 1.0823 1.2456 0.202 Uiso 1 1 calc R . . C28 C 0.3293(4) 0.7473(2) 0.9904(3) 0.0558(19) Uani 1 1 d DU . . C29 C 0.3989(3) 0.7479(2) 1.0479(3) 0.070(2) Uani 1 1 d DU . . H29 H 0.3930 0.7568 1.0903 0.083 Uiso 1 1 calc R . . C30 C 0.4773(4) 0.7358(3) 1.0448(3) 0.086(3) Uani 1 1 d DU . . H30 H 0.5238 0.7363 1.0845 0.104 Uiso 1 1 calc R . . C31 C 0.4851(3) 0.7231(4) 0.9825(3) 0.076(3) Uani 1 1 d DU . . C32 C 0.4167(4) 0.7214(4) 0.9242(4) 0.094(3) Uani 1 1 d DU . . H32 H 0.4229 0.7120 0.8821 0.112 Uiso 1 1 calc R . . C33 C 0.3374(4) 0.7338(3) 0.9279(3) 0.080(3) Uani 1 1 d DU . . H33 H 0.2907 0.7329 0.8885 0.096 Uiso 1 1 calc R . . C34 C 0.5718(4) 0.7098(5) 0.9765(6) 0.144(5) Uani 1 1 d DU . . H34A H 0.5664 0.7021 0.9293 0.216 Uiso 1 1 calc R . . H34B H 0.5937 0.6824 1.0054 0.216 Uiso 1 1 calc R . . H34C H 0.6094 0.7366 0.9913 0.216 Uiso 1 1 calc R . . C35 C -0.0450(4) 0.6242(2) 0.9640(3) 0.067(2) Uani 1 1 d DU . . C36 C -0.0661(4) 0.6010(2) 1.0163(4) 0.091(3) Uani 1 1 d DU . . H36 H -0.0628 0.6174 1.0570 0.109 Uiso 1 1 calc R . . C37 C -0.0924(5) 0.5533(2) 1.0082(4) 0.103(3) Uani 1 1 d DU . . H37 H -0.1058 0.5383 1.0444 0.124 Uiso 1 1 calc R . . C38 C -0.0994(5) 0.5276(2) 0.9502(4) 0.090(3) Uani 1 1 d DU . . C39 C -0.0767(6) 0.5498(2) 0.8994(4) 0.101(3) Uani 1 1 d DU . . H39 H -0.0798 0.5330 0.8590 0.121 Uiso 1 1 calc R . . C40 C -0.0488(6) 0.5972(2) 0.9065(4) 0.087(3) Uani 1 1 d DU . . H40 H -0.0321 0.6111 0.8711 0.105 Uiso 1 1 calc R . . C41 C -0.1300(7) 0.4756(3) 0.9418(7) 0.139(5) Uani 1 1 d DU . . H41A H -0.1310 0.4639 0.8971 0.209 Uiso 1 1 calc R . . H41B H -0.1856 0.4741 0.9458 0.209 Uiso 1 1 calc R . . H41C H -0.0928 0.4561 0.9773 0.209 Uiso 1 1 calc R . . C42 C -0.2395(4) 0.8381(3) 1.0044(3) 0.065(2) Uani 1 1 d DU . . C43 C -0.2985(4) 0.8534(2) 0.9443(4) 0.088(3) Uani 1 1 d DU . . H43 H -0.2835 0.8569 0.9041 0.105 Uiso 1 1 calc R . . C44 C -0.3805(4) 0.8635(3) 0.9428(4) 0.110(4) Uani 1 1 d DU . . H44 H -0.4194 0.8735 0.9016 0.132 Uiso 1 1 calc R . . C45 C -0.4045(4) 0.8591(4) 1.0009(3) 0.101(3) Uani 1 1 d DU . . C46 C -0.3466(4) 0.8443(4) 1.0594(4) 0.111(4) Uani 1 1 d DU . . H46 H -0.3617 0.8417 1.0996 0.133 Uiso 1 1 calc R . . C47 C -0.2655(4) 0.8326(4) 1.0621(4) 0.113(4) Uani 1 1 d DU . . H47 H -0.2282 0.8210 1.1031 0.135 Uiso 1 1 calc R . . C48 C -0.4949(4) 0.8688(6) 1.0003(7) 0.169(7) Uani 1 1 d DU . . H48A H -0.5282 0.8783 0.9545 0.253 Uiso 1 1 calc R . . H48B H -0.4950 0.8941 1.0324 0.253 Uiso 1 1 calc R . . H48C H -0.5179 0.8400 1.0134 0.253 Uiso 1 1 calc R . . Yb2 Yb 0.002110(19) 0.776198(12) 0.764768(18) 0.05051(9) Uani 1 1 d . . . N1' N 0.0492(4) 0.8265(2) 0.6932(3) 0.0549(16) Uani 1 1 d DU . . N2' N 0.0964(3) 0.7273(2) 0.7352(3) 0.0551(16) Uani 1 1 d DU . . N3' N -0.0728(3) 0.7064(2) 0.7284(3) 0.0536(16) Uani 1 1 d DU . . N4' N -0.1197(4) 0.8069(2) 0.6911(3) 0.0587(17) Uani 1 1 d DU . . C1' C 0.0130(5) 0.8682(3) 0.6643(4) 0.062(2) Uani 1 1 d DU . . C2' C 0.0758(5) 0.8969(3) 0.6479(4) 0.077(3) Uani 1 1 d DU . . H2' H 0.0674 0.9274 0.6278 0.093 Uiso 1 1 calc R . . C3' C 0.1478(5) 0.8727(3) 0.6662(5) 0.076(2) Uani 1 1 d DU . . H3' H 0.1986 0.8829 0.6615 0.091 Uiso 1 1 calc R . . C4' C 0.1318(4) 0.8284(3) 0.6946(4) 0.060(2) Uani 1 1 d DU . . C5' C 0.1906(4) 0.7898(3) 0.7160(4) 0.0602(19) Uani 1 1 d U . . C6' C 0.1741(4) 0.7428(3) 0.7321(3) 0.0558(17) Uani 1 1 d DU . . C7' C 0.2283(5) 0.7031(3) 0.7406(4) 0.064(2) Uani 1 1 d DU . . H7' H 0.2837 0.7045 0.7405 0.077 Uiso 1 1 calc R . . C8' C 0.1884(5) 0.6634(3) 0.7489(4) 0.068(2) Uani 1 1 d DU . . H8' H 0.2107 0.6325 0.7566 0.082 Uiso 1 1 calc R . . C9' C 0.1030(5) 0.6777(3) 0.7436(4) 0.0572(19) Uani 1 1 d DU . . C10' C 0.0403(5) 0.6460(3) 0.7453(4) 0.0596(18) Uani 1 1 d U . . C11' C -0.0453(5) 0.6601(3) 0.7360(4) 0.059(2) Uani 1 1 d DU . . C12' C -0.1116(5) 0.6268(3) 0.7345(4) 0.068(2) Uani 1 1 d DU . . H12' H -0.1087 0.5934 0.7385 0.081 Uiso 1 1 calc R . . C13' C -0.1795(5) 0.6557(3) 0.7259(4) 0.067(2) Uani 1 1 d DU . . H13' H -0.2329 0.6446 0.7226 0.080 Uiso 1 1 calc R . . C14' C -0.1586(4) 0.7048(3) 0.7225(4) 0.0550(18) Uani 1 1 d DU . . C15' C -0.2136(4) 0.7439(3) 0.7102(4) 0.0588(18) Uani 1 1 d U . . C16' C -0.1987(4) 0.7908(3) 0.6930(4) 0.062(2) Uani 1 1 d DU . . C17' C -0.2579(5) 0.8279(3) 0.6686(4) 0.075(3) Uani 1 1 d DU . . H17' H -0.3145 0.8263 0.6652 0.089 Uiso 1 1 calc R . . C18' C -0.2195(5) 0.8655(4) 0.6511(4) 0.075(2) Uani 1 1 d DU . . H18' H -0.2440 0.8946 0.6328 0.089 Uiso 1 1 calc R . . C19' C -0.1330(5) 0.8524(3) 0.6661(4) 0.065(2) Uani 1 1 d DU . . C20' C -0.0717(5) 0.8824(3) 0.6516(5) 0.068(2) Uani 1 1 d U . . C21' C 0.2782(3) 0.8002(2) 0.7160(3) 0.0566(19) Uani 1 1 d DU . . C22' C 0.3028(3) 0.7979(2) 0.6582(3) 0.079(3) Uani 1 1 d DU . . H22' H 0.2633 0.7898 0.6162 0.094 Uiso 1 1 calc R . . C23' C 0.3858(4) 0.8072(3) 0.6597(4) 0.087(3) Uani 1 1 d DU . . H23' H 0.4006 0.8047 0.6194 0.105 Uiso 1 1 calc R . . C24' C 0.4443(3) 0.8198(3) 0.7204(3) 0.087(3) Uani 1 1 d DU . . C25' C 0.4205(4) 0.8210(4) 0.7791(4) 0.086(3) Uani 1 1 d DU . . H25' H 0.4603 0.8287 0.8210 0.104 Uiso 1 1 calc R . . C26' C 0.3387(4) 0.8112(3) 0.7780(4) 0.079(3) Uani 1 1 d DU . . H26' H 0.3248 0.8119 0.8189 0.095 Uiso 1 1 calc R . . C27' C 0.5344(4) 0.8299(4) 0.7222(6) 0.122(4) Uani 1 1 d DU . . H27D H 0.5676 0.8379 0.7686 0.183 Uiso 1 1 calc R . . H27E H 0.5351 0.8564 0.6919 0.183 Uiso 1 1 calc R . . H27F H 0.5573 0.8018 0.7071 0.183 Uiso 1 1 calc R . . C28' C 0.0590(4) 0.5939(2) 0.7552(3) 0.071(2) Uani 1 1 d DU . . C29' C 0.1146(4) 0.5767(2) 0.8153(4) 0.091(3) Uani 1 1 d DU . . H29' H 0.1400 0.5982 0.8506 0.109 Uiso 1 1 calc R . . C30' C 0.1342(5) 0.5280(2) 0.8251(4) 0.117(3) Uani 1 1 d DU . . H30' H 0.1727 0.5177 0.8664 0.140 Uiso 1 1 calc R . . C31' C 0.0976(6) 0.4955(2) 0.7749(4) 0.141(4) Uani 1 1 d DU . . C32' C 0.0432(6) 0.5119(2) 0.7152(5) 0.130(4) Uani 1 1 d DU . . H32' H 0.0176 0.4900 0.6804 0.156 Uiso 1 1 calc R . . C33' C 0.0245(6) 0.5606(2) 0.7041(4) 0.105(3) Uani 1 1 d DU . . H33' H -0.0117 0.5708 0.6617 0.127 Uiso 1 1 calc R . . C34' C 0.1186(10) 0.4421(3) 0.7854(9) 0.234(7) Uani 1 1 d DU . . H34D H 0.1590 0.4372 0.8302 0.350 Uiso 1 1 calc R . . H34E H 0.1415 0.4311 0.7502 0.350 Uiso 1 1 calc R . . H34F H 0.0685 0.4242 0.7824 0.350 Uiso 1 1 calc R . . C35' C -0.2989(4) 0.7315(3) 0.7159(3) 0.062(2) Uani 1 1 d DU . . C36' C -0.3698(3) 0.7279(2) 0.6584(3) 0.062(2) Uani 1 1 d DU . . H36' H -0.3666 0.7355 0.6147 0.075 Uiso 1 1 calc R . . C37' C -0.4454(4) 0.7130(3) 0.6661(3) 0.086(3) Uani 1 1 d DU . . H37' H -0.4924 0.7110 0.6270 0.103 Uiso 1 1 calc R . . C38' C -0.4530(4) 0.7012(3) 0.7287(3) 0.092(3) Uani 1 1 d DU . . C39' C -0.3840(4) 0.7055(4) 0.7854(4) 0.109(4) Uani 1 1 d DU . . H39' H -0.3884 0.6988 0.8291 0.130 Uiso 1 1 calc R . . C40' C -0.3075(4) 0.7198(4) 0.7793(3) 0.095(4) Uani 1 1 d DU . . H40' H -0.2609 0.7216 0.8188 0.114 Uiso 1 1 calc R . . C41' C -0.5364(4) 0.6844(4) 0.7356(5) 0.116(4) Uani 1 1 d DU . . H41D H -0.5300 0.6779 0.7834 0.173 Uiso 1 1 calc R . . H41E H -0.5541 0.6556 0.7089 0.173 Uiso 1 1 calc R . . H41F H -0.5778 0.7091 0.7188 0.173 Uiso 1 1 calc R . . C42' C -0.0975(4) 0.9307(3) 0.6195(3) 0.083(2) Uani 1 1 d DU . . C43' C -0.1050(4) 0.9695(2) 0.6584(4) 0.124(3) Uani 1 1 d DU . . H43' H -0.0947 0.9660 0.7059 0.149 Uiso 1 1 calc R . . C44' C -0.1281(5) 1.0142(3) 0.6278(4) 0.172(4) Uani 1 1 d DU . . H44' H -0.1330 1.0401 0.6553 0.206 Uiso 1 1 calc R . . C45' C -0.1436(8) 1.0209(3) 0.5586(4) 0.197(4) Uani 1 1 d DU . . C46' C -0.1361(9) 0.9827(3) 0.5192(5) 0.197(5) Uani 1 1 d DU . . H46' H -0.1453 0.9867 0.4720 0.236 Uiso 1 1 calc R . . C47' C -0.1148(7) 0.9379(3) 0.5493(4) 0.137(4) Uani 1 1 d DU . . H47' H -0.1121 0.9118 0.5213 0.165 Uiso 1 1 calc R . . C48' C -0.1675(10) 1.0705(3) 0.5265(8) 0.317(7) Uani 1 1 d DU . . H48D H -0.1731 1.0925 0.5613 0.476 Uiso 1 1 calc R . . H48E H -0.2198 1.0684 0.4899 0.476 Uiso 1 1 calc R . . H48F H -0.1246 1.0819 0.5082 0.476 Uiso 1 1 calc R . . O1 O 0.0883(3) 0.81093(18) 0.8561(3) 0.0527(14) Uani 1 1 d U . . C49 C 0.1276(5) 0.8569(3) 0.8578(4) 0.067(2) Uani 1 1 d U . . H49A H 0.1538 0.8586 0.8214 0.080 Uiso 1 1 calc R . . H49B H 0.1708 0.8613 0.9020 0.080 Uiso 1 1 calc R . . C50 C 0.0619(6) 0.8964(3) 0.8473(5) 0.088(2) Uani 1 1 d U . . H50A H 0.0884 0.9278 0.8570 0.106 Uiso 1 1 calc R . . H50B H 0.0244 0.8962 0.8000 0.106 Uiso 1 1 calc R . . O2 O 0.0169(4) 0.8858(2) 0.8948(3) 0.0741(17) Uani 1 1 d U . . C51 C -0.0529(7) 0.9189(4) 0.8822(6) 0.124(4) Uani 1 1 d U . . H51A H -0.0845 0.9118 0.9132 0.186 Uiso 1 1 calc R . . H51B H -0.0885 0.9156 0.8352 0.186 Uiso 1 1 calc R . . H51C H -0.0321 0.9513 0.8898 0.186 Uiso 1 1 calc R . . O3 O -0.0576(3) 0.7777(2) 0.8469(3) 0.0656(17) Uani 1 1 d . . . H3A H -0.1127 0.7683 0.8408 0.079 Uiso 1 1 calc R . . O4 O -0.2047(5) 0.9869(4) 1.2094(2) 0.157(5) Uani 0.25 1 d PDU . . C52 C -0.1347(6) 0.9575(4) 1.2451(3) 0.160(7) Uiso 0.25 1 d PD . . H52A H -0.0828 0.9742 1.2479 0.192 Uiso 0.25 1 calc PR . . H52B H -0.1361 0.9277 1.2199 0.192 Uiso 0.25 1 calc PR . . C53 C -0.1379(12) 0.9467(6) 1.3170(4) 0.173(12) Uiso 0.25 1 d PD . . H53A H -0.0964 0.9228 1.3382 0.260 Uiso 0.25 1 calc PR . . H53B H -0.1926 0.9347 1.3143 0.260 Uiso 0.25 1 calc PR . . H53C H -0.1268 0.9756 1.3443 0.260 Uiso 0.25 1 calc PR . . C54 C -0.2178(5) 0.9856(6) 1.1369(3) 0.141(6) Uiso 0.25 1 d PD . . H54A H -0.2115 0.9529 1.1226 0.169 Uiso 0.25 1 calc PR . . H54B H -0.1760 1.0055 1.1258 0.169 Uiso 0.25 1 calc PR . . C55 C -0.3043(6) 1.0038(9) 1.0981(6) 0.171(11) Uiso 0.25 1 d PD . . H55A H -0.3121 1.0031 1.0492 0.256 Uiso 0.25 1 calc PR . . H55B H -0.3104 1.0363 1.1121 0.256 Uiso 0.25 1 calc PR . . H55C H -0.3456 0.9837 1.1082 0.256 Uiso 0.25 1 calc PR . . 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 0.04183(15) 0.05618(18) 0.05780(17) -0.00227(15) 0.02773(13) -0.00445(14) N1 0.047(2) 0.062(3) 0.063(3) 0.002(3) 0.029(2) -0.004(2) N2 0.042(2) 0.071(3) 0.049(3) -0.011(3) 0.018(2) -0.005(2) N3 0.046(2) 0.052(3) 0.065(3) -0.001(3) 0.028(3) 0.000(2) N4 0.049(2) 0.065(3) 0.055(3) 0.003(3) 0.035(2) -0.003(2) C1 0.037(3) 0.075(4) 0.076(5) 0.003(4) 0.023(3) 0.002(3) C2 0.046(3) 0.074(4) 0.097(6) -0.006(4) 0.036(4) 0.002(3) C3 0.057(3) 0.079(4) 0.094(6) -0.019(4) 0.037(4) -0.006(3) C4 0.052(2) 0.064(4) 0.057(4) -0.003(3) 0.025(3) -0.003(3) C5 0.055(3) 0.058(3) 0.077(4) -0.005(3) 0.030(3) -0.004(3) C6 0.048(3) 0.061(3) 0.061(4) -0.004(3) 0.023(3) -0.004(3) C7 0.056(3) 0.066(4) 0.088(5) -0.015(4) 0.036(4) -0.013(3) C8 0.045(3) 0.074(4) 0.082(5) -0.011(4) 0.044(3) -0.017(3) C9 0.040(3) 0.065(3) 0.060(4) -0.008(3) 0.026(3) -0.008(2) C10 0.039(3) 0.066(3) 0.065(4) -0.002(3) 0.021(3) -0.005(2) C11 0.045(3) 0.057(3) 0.068(5) 0.006(4) 0.021(3) 0.002(3) C12 0.050(3) 0.065(3) 0.080(5) -0.007(4) 0.022(4) 0.008(3) C13 0.067(3) 0.050(3) 0.092(6) 0.000(4) 0.030(4) -0.002(3) C14 0.046(2) 0.061(4) 0.058(4) 0.013(4) 0.008(3) -0.003(2) C15 0.062(3) 0.064(3) 0.054(4) -0.006(3) 0.029(3) -0.011(3) C16 0.060(3) 0.066(3) 0.047(3) 0.005(3) 0.034(3) -0.008(3) C17 0.058(3) 0.075(4) 0.071(5) 0.001(4) 0.030(4) -0.014(3) C18 0.046(3) 0.085(4) 0.067(4) 0.005(4) 0.029(3) -0.011(3) C19 0.034(3) 0.074(3) 0.057(4) 0.003(3) 0.013(3) -0.003(2) C20 0.046(3) 0.085(3) 0.055(4) -0.008(3) 0.032(3) -0.002(3) C21 0.041(3) 0.069(4) 0.082(4) -0.013(3) 0.029(3) 0.001(3) C22 0.080(5) 0.068(4) 0.085(4) -0.011(4) 0.029(4) 0.003(4) C23 0.080(5) 0.088(5) 0.078(4) -0.021(3) 0.022(4) 0.005(4) C24 0.087(6) 0.075(5) 0.102(4) -0.029(4) 0.026(5) -0.008(4) C25 0.107(6) 0.071(5) 0.102(4) -0.017(4) 0.043(5) -0.020(4) C26 0.101(6) 0.055(4) 0.089(4) -0.008(3) 0.030(4) -0.007(4) C27 0.141(9) 0.110(6) 0.154(8) -0.072(6) 0.048(7) -0.039(5) C28 0.044(3) 0.060(4) 0.071(4) 0.003(3) 0.028(3) 0.000(3) C29 0.051(3) 0.094(6) 0.068(4) 0.005(4) 0.025(3) 0.011(4) C30 0.060(3) 0.134(8) 0.063(4) 0.016(5) 0.016(3) 0.028(5) C31 0.046(3) 0.109(7) 0.084(4) 0.004(5) 0.036(3) 0.010(4) C32 0.065(3) 0.155(10) 0.070(4) 0.000(6) 0.033(3) 0.019(5) C33 0.050(3) 0.119(8) 0.073(4) -0.013(5) 0.022(3) 0.008(5) C34 0.062(4) 0.210(14) 0.176(9) -0.030(10) 0.057(5) 0.024(7) C35 0.063(4) 0.060(3) 0.082(4) 0.000(3) 0.028(4) -0.011(3) C36 0.113(6) 0.077(4) 0.102(4) 0.004(4) 0.062(4) -0.014(5) C37 0.123(7) 0.072(4) 0.134(4) 0.023(4) 0.069(5) -0.007(5) C38 0.070(5) 0.056(4) 0.150(5) 0.010(3) 0.042(5) -0.005(4) C39 0.126(8) 0.074(4) 0.101(5) -0.013(4) 0.031(5) -0.026(5) C40 0.118(7) 0.068(4) 0.079(4) -0.001(3) 0.036(5) -0.020(5) C41 0.106(8) 0.060(4) 0.248(13) 0.002(5) 0.050(9) -0.017(5) C42 0.042(3) 0.080(5) 0.079(4) -0.009(4) 0.030(3) -0.007(3) C43 0.049(3) 0.127(8) 0.096(4) 0.020(5) 0.036(3) -0.002(4) C44 0.046(3) 0.157(11) 0.129(4) 0.016(7) 0.029(3) 0.006(5) C45 0.060(3) 0.116(8) 0.138(5) -0.008(6) 0.048(3) 0.016(5) C46 0.067(3) 0.167(11) 0.119(5) 0.006(6) 0.060(3) 0.016(5) C47 0.075(3) 0.179(11) 0.107(4) 0.036(6) 0.062(3) 0.038(6) C48 0.069(4) 0.269(19) 0.186(10) 0.011(12) 0.065(5) 0.037(8) Yb2 0.04252(15) 0.05890(19) 0.05847(17) 0.00011(15) 0.02783(13) -0.00313(14) N1' 0.051(2) 0.062(3) 0.060(3) 0.007(3) 0.030(3) -0.002(2) N2' 0.050(2) 0.058(3) 0.071(4) -0.008(3) 0.039(3) -0.009(2) N3' 0.047(2) 0.056(3) 0.066(3) -0.004(3) 0.030(3) -0.013(2) N4' 0.041(2) 0.072(3) 0.068(4) 0.013(3) 0.024(3) 0.003(2) C1' 0.060(3) 0.065(4) 0.077(4) 0.019(4) 0.042(3) 0.003(3) C2' 0.067(3) 0.070(4) 0.107(6) 0.026(4) 0.043(4) -0.004(3) C3' 0.058(3) 0.069(4) 0.113(6) 0.011(4) 0.046(4) -0.008(3) C4' 0.047(3) 0.070(3) 0.073(5) 0.008(4) 0.032(3) -0.002(3) C5' 0.039(2) 0.070(3) 0.084(5) 0.000(4) 0.038(3) -0.006(2) C6' 0.054(3) 0.074(3) 0.058(4) 0.007(3) 0.042(3) -0.004(3) C7' 0.049(3) 0.084(4) 0.072(5) -0.005(4) 0.038(3) 0.002(3) C8' 0.060(3) 0.069(4) 0.085(5) -0.003(4) 0.034(4) 0.007(3) C9' 0.059(3) 0.061(3) 0.063(4) -0.001(3) 0.035(3) -0.002(3) C10' 0.065(3) 0.063(3) 0.062(4) -0.006(3) 0.036(3) -0.008(3) C11' 0.055(3) 0.052(3) 0.069(5) -0.002(4) 0.018(4) -0.012(2) C12' 0.061(3) 0.069(4) 0.079(5) -0.001(4) 0.030(4) -0.018(3) C13' 0.061(3) 0.071(3) 0.072(5) -0.003(4) 0.026(4) -0.016(3) C14' 0.043(3) 0.070(3) 0.061(4) -0.016(4) 0.030(3) -0.015(3) C15' 0.046(3) 0.080(3) 0.058(4) 0.006(4) 0.026(3) -0.004(3) C16' 0.041(3) 0.085(3) 0.067(5) 0.012(4) 0.026(3) 0.002(3) C17' 0.042(3) 0.089(4) 0.099(6) 0.006(4) 0.030(4) 0.012(3) C18' 0.052(3) 0.096(4) 0.079(5) 0.024(4) 0.026(4) 0.020(3) C19' 0.043(3) 0.082(4) 0.072(5) 0.026(4) 0.021(3) 0.011(3) C20' 0.052(3) 0.073(3) 0.081(5) 0.019(3) 0.025(3) 0.004(3) C21' 0.043(2) 0.072(5) 0.068(3) 0.004(4) 0.036(2) -0.007(3) C22' 0.054(3) 0.120(8) 0.079(3) -0.010(5) 0.047(3) 0.000(4) C23' 0.072(3) 0.114(8) 0.103(4) -0.004(5) 0.066(3) -0.012(5) C24' 0.049(3) 0.077(6) 0.150(5) -0.009(5) 0.056(3) -0.012(4) C25' 0.049(3) 0.104(7) 0.105(4) -0.024(6) 0.023(3) -0.020(4) C26' 0.060(3) 0.106(7) 0.081(4) -0.025(5) 0.036(3) -0.027(4) C27' 0.061(3) 0.100(7) 0.230(9) -0.025(8) 0.084(4) -0.029(5) C28' 0.069(4) 0.066(3) 0.098(5) 0.004(3) 0.054(3) -0.008(3) C29' 0.101(6) 0.076(4) 0.110(5) 0.016(4) 0.056(4) 0.005(5) C30' 0.102(6) 0.095(4) 0.183(7) 0.047(4) 0.088(5) 0.036(5) C31' 0.169(8) 0.062(4) 0.241(8) 0.019(4) 0.136(6) 0.024(5) C32' 0.146(8) 0.079(4) 0.204(7) -0.043(5) 0.110(5) 0.003(5) C33' 0.122(8) 0.078(4) 0.127(6) -0.020(4) 0.055(5) -0.010(5) C34' 0.327(16) 0.070(4) 0.397(18) 0.057(6) 0.248(11) 0.047(8) C35' 0.040(3) 0.091(6) 0.062(3) 0.006(4) 0.024(3) 0.000(3) C36' 0.044(3) 0.088(6) 0.061(3) -0.007(4) 0.027(3) 0.000(4) C37' 0.046(3) 0.116(7) 0.108(4) -0.035(5) 0.043(3) -0.017(4) C38' 0.062(3) 0.095(7) 0.137(5) 0.013(5) 0.059(3) -0.012(4) C39' 0.081(4) 0.153(10) 0.111(5) 0.011(6) 0.058(3) -0.029(6) C40' 0.062(4) 0.170(10) 0.062(3) 0.013(5) 0.031(3) -0.014(5) C41' 0.072(4) 0.152(11) 0.147(7) -0.005(7) 0.070(4) -0.029(5) C42' 0.055(4) 0.088(3) 0.116(4) 0.039(3) 0.039(4) 0.008(3) C43' 0.141(8) 0.080(4) 0.185(5) 0.031(3) 0.101(6) 0.015(6) C44' 0.142(9) 0.093(5) 0.321(4) 0.066(4) 0.130(8) 0.035(6) C45' 0.133(10) 0.140(4) 0.333(6) 0.151(4) 0.096(9) 0.050(7) C46' 0.170(14) 0.211(5) 0.201(6) 0.142(4) 0.046(9) 0.045(9) C47' 0.136(10) 0.152(5) 0.116(4) 0.063(4) 0.027(7) 0.021(8) C48' 0.164(13) 0.194(5) 0.597(12) 0.275(7) 0.122(15) 0.077(9) O1 0.047(2) 0.058(3) 0.063(3) 0.002(2) 0.032(2) -0.008(2) C49 0.077(4) 0.058(4) 0.074(5) -0.006(4) 0.038(4) -0.014(3) C50 0.124(4) 0.062(4) 0.106(5) 0.011(4) 0.075(4) 0.002(4) O2 0.087(3) 0.067(3) 0.084(3) 0.012(3) 0.048(3) 0.010(3) C51 0.141(5) 0.118(8) 0.140(8) 0.047(7) 0.082(5) 0.062(5) O3 0.043(2) 0.106(4) 0.060(3) -0.012(3) 0.033(2) -0.016(3) O4 0.159(18) 0.14(3) 0.30(3) -0.03(2) 0.178(19) -0.067(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O3 2.182(5) . ? Yb1 N3 2.327(6) . ? Yb1 O1 2.330(5) . ? Yb1 N2 2.334(5) . ? Yb1 N1 2.340(6) . ? Yb1 N4 2.344(6) . ? Yb1 O2 2.472(6) . ? Yb1 Yb2 3.6260(5) . ? N1 C1 1.373(10) . ? N1 C4 1.379(10) . ? N2 C6 1.376(10) . ? N2 C9 1.375(9) . ? N3 C14 1.359(10) . ? N3 C11 1.375(9) . ? N4 C16 1.358(10) . ? N4 C19 1.384(9) . ? C1 C20 1.404(11) . ? C1 C2 1.457(12) . ? C2 C3 1.353(11) . ? C3 C4 1.452(12) . ? C4 C5 1.412(11) . ? C5 C6 1.373(11) . ? C5 C21 1.513(10) . ? C6 C7 1.451(10) . ? C7 C8 1.377(12) . ? C8 C9 1.425(10) . ? C9 C10 1.373(11) . ? C10 C11 1.426(10) . ? C10 C28 1.522(10) . ? C11 C12 1.435(11) . ? C12 C13 1.357(11) . ? C13 C14 1.408(11) . ? C14 C15 1.425(11) . ? C15 C16 1.429(11) . ? C15 C35 1.494(10) . ? C16 C17 1.450(11) . ? C17 C18 1.338(12) . ? C18 C19 1.478(11) . ? C19 C20 1.366(12) . ? C20 C42 1.508(10) . ? C21 C26 1.378(9) . ? C21 C22 1.385(8) . ? C22 C23 1.385(8) . ? C23 C24 1.356(9) . ? C24 C25 1.368(8) . ? C24 C27 1.529(9) . ? C25 C26 1.382(8) . ? C28 C33 1.368(8) . ? C28 C29 1.371(7) . ? C29 C30 1.376(8) . ? C30 C31 1.358(8) . ? C31 C32 1.370(7) . ? C31 C34 1.540(9) . ? C32 C33 1.397(8) . ? C35 C40 1.372(8) . ? C35 C36 1.379(8) . ? C36 C37 1.391(8) . ? C37 C38 1.349(8) . ? C38 C39 1.355(9) . ? C38 C41 1.522(9) . ? C39 C40 1.390(8) . ? C42 C47 1.379(9) . ? C42 C43 1.378(7) . ? C43 C44 1.393(8) . ? C44 C45 1.365(9) . ? C45 C46 1.344(8) . ? C45 C48 1.534(9) . ? C46 C47 1.380(8) . ? Yb2 O1 2.189(5) . ? Yb2 O3 2.195(5) . ? Yb2 N4' 2.288(6) . ? Yb2 N2' 2.300(6) . ? Yb2 N3' 2.303(6) . ? Yb2 N1' 2.324(6) . ? N1' C1' 1.353(10) . ? N1' C4' 1.377(10) . ? N2' C9' 1.388(10) . ? N2' C6' 1.393(9) . ? N3' C11' 1.356(10) . ? N3' C14' 1.405(9) . ? N4' C19' 1.354(11) . ? N4' C16' 1.410(10) . ? C1' C20' 1.418(11) . ? C1' C2' 1.438(12) . ? C2' C3' 1.328(12) . ? C3' C4' 1.418(12) . ? C4' C5' 1.427(11) . ? C5' C6' 1.394(11) . ? C5' C21' 1.498(9) . ? C6' C7' 1.403(11) . ? C7' C8' 1.327(12) . ? C8' C9' 1.457(11) . ? C9' C10' 1.379(11) . ? C10' C11' 1.442(11) . ? C10' C28' 1.478(10) . ? C11' C12' 1.439(11) . ? C12' C13' 1.357(12) . ? C13' C14' 1.415(11) . ? C14' C15' 1.395(11) . ? C15' C16' 1.390(12) . ? C15' C35' 1.508(10) . ? C16' C17' 1.408(11) . ? C17' C18' 1.332(13) . ? C18' C19' 1.433(11) . ? C19' C20' 1.422(12) . ? C20' C42' 1.494(11) . ? C21' C22' 1.361(8) . ? C21' C26' 1.383(7) . ? C22' C23' 1.404(8) . ? C23' C24' 1.360(8) . ? C24' C25' 1.369(9) . ? C24' C27' 1.526(8) . ? C25' C26' 1.390(8) . ? C28' C29' 1.371(8) . ? C28' C33' 1.377(8) . ? C29' C30' 1.390(8) . ? C30' C31' 1.358(9) . ? C31' C32' 1.351(9) . ? C31' C34' 1.523(9) . ? C32' C33' 1.389(8) . ? C35' C40' 1.379(8) . ? C35' C36' 1.386(7) . ? C36' C37' 1.387(8) . ? C37' C38' 1.357(8) . ? C38' C39' 1.361(8) . ? C38' C41' 1.519(9) . ? C39' C40' 1.385(9) . ? C42' C43' 1.366(9) . ? C42' C47' 1.379(9) . ? C43' C44' 1.387(9) . ? C44' C45' 1.361(9) . ? C45' C46' 1.357(10) . ? C45' C48' 1.523(10) . ? C46' C47' 1.383(9) . ? O1 C49 1.433(9) . ? C49 C50 1.521(12) . ? C50 O2 1.428(12) . ? O2 C51 1.446(12) . ? O4 C54 1.420(7) . ? O4 C52 1.427(8) . ? C52 C53 1.509(8) . ? C54 C55 1.506(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 O3 Yb1 N3 95.5(2) . . ? O3 Yb1 O1 69.20(18) . . ? N3 Yb1 O1 88.9(2) . . ? O3 Yb1 N2 154.0(2) . . ? N3 Yb1 N2 76.7(2) . . ? O1 Yb1 N2 85.72(19) . . ? O3 Yb1 N1 125.6(2) . . ? N3 Yb1 N1 123.0(2) . . ? O1 Yb1 N1 138.3(2) . . ? N2 Yb1 N1 77.8(2) . . ? O3 Yb1 N4 79.5(2) . . ? N3 Yb1 N4 76.8(2) . . ? O1 Yb1 N4 144.09(19) . . ? N2 Yb1 N4 121.5(2) . . ? N1 Yb1 N4 74.8(2) . . ? O3 Yb1 O2 89.4(2) . . ? N3 Yb1 O2 151.4(2) . . ? O1 Yb1 O2 66.56(19) . . ? N2 Yb1 O2 86.6(2) . . ? N1 Yb1 O2 74.4(2) . . ? N4 Yb1 O2 131.8(2) . . ? O3 Yb1 Yb2 34.19(14) . . ? N3 Yb1 Yb2 89.20(15) . . ? O1 Yb1 Yb2 35.33(11) . . ? N2 Yb1 Yb2 120.05(15) . . ? N1 Yb1 Yb2 147.13(14) . . ? N4 Yb1 Yb2 110.66(14) . . ? O2 Yb1 Yb2 79.17(14) . . ? C1 N1 C4 106.7(7) . . ? C1 N1 Yb1 124.2(5) . . ? C4 N1 Yb1 125.7(5) . . ? C6 N2 C9 107.8(6) . . ? C6 N2 Yb1 124.1(5) . . ? C9 N2 Yb1 122.1(5) . . ? C14 N3 C11 105.6(6) . . ? C14 N3 Yb1 127.9(5) . . ? C11 N3 Yb1 123.6(5) . . ? C16 N4 C19 105.5(6) . . ? C16 N4 Yb1 124.4(5) . . ? C19 N4 Yb1 120.8(5) . . ? N1 C1 C20 124.9(8) . . ? N1 C1 C2 109.6(7) . . ? C20 C1 C2 125.4(7) . . ? C3 C2 C1 106.9(7) . . ? C2 C3 C4 107.3(8) . . ? N1 C4 C5 125.4(7) . . ? N1 C4 C3 109.5(7) . . ? C5 C4 C3 125.1(7) . . ? C6 C5 C4 126.7(7) . . ? C6 C5 C21 115.2(6) . . ? C4 C5 C21 117.8(7) . . ? C5 C6 N2 126.3(7) . . ? C5 C6 C7 125.7(7) . . ? N2 C6 C7 107.9(7) . . ? C8 C7 C6 107.8(7) . . ? C7 C8 C9 106.3(7) . . ? N2 C9 C10 125.9(7) . . ? N2 C9 C8 110.1(7) . . ? C10 C9 C8 123.8(7) . . ? C9 C10 C11 125.1(7) . . ? C9 C10 C28 118.6(6) . . ? C11 C10 C28 116.2(7) . . ? N3 C11 C10 125.5(7) . . ? N3 C11 C12 109.9(7) . . ? C10 C11 C12 124.4(7) . . ? C13 C12 C11 106.1(7) . . ? C12 C13 C14 107.5(7) . . ? N3 C14 C13 110.9(7) . . ? N3 C14 C15 124.7(7) . . ? C13 C14 C15 124.3(7) . . ? C14 C15 C16 125.6(7) . . ? C14 C15 C35 117.5(7) . . ? C16 C15 C35 116.9(7) . . ? N4 C16 C15 124.7(7) . . ? N4 C16 C17 111.8(7) . . ? C15 C16 C17 123.4(7) . . ? C18 C17 C16 106.5(7) . . ? C17 C18 C19 107.0(7) . . ? C20 C19 N4 125.9(7) . . ? C20 C19 C18 124.6(7) . . ? N4 C19 C18 109.2(7) . . ? C19 C20 C1 124.9(7) . . ? C19 C20 C42 117.5(7) . . ? C1 C20 C42 117.5(7) . . ? C26 C21 C22 117.8(6) . . ? C26 C21 C5 120.5(6) . . ? C22 C21 C5 121.3(6) . . ? C23 C22 C21 121.2(7) . . ? C24 C23 C22 120.4(7) . . ? C23 C24 C25 118.8(6) . . ? C23 C24 C27 121.4(7) . . ? C25 C24 C27 119.7(7) . . ? C24 C25 C26 121.6(7) . . ? C21 C26 C25 120.0(7) . . ? C33 C28 C29 119.3(6) . . ? C33 C28 C10 119.9(5) . . ? C29 C28 C10 120.8(6) . . ? C28 C29 C30 122.1(6) . . ? C31 C30 C29 118.4(5) . . ? C30 C31 C32 121.1(6) . . ? C30 C31 C34 120.1(6) . . ? C32 C31 C34 118.8(7) . . ? C31 C32 C33 120.0(7) . . ? C28 C33 C32 119.2(6) . . ? C40 C35 C36 116.5(6) . . ? C40 C35 C15 122.0(6) . . ? C36 C35 C15 121.5(6) . . ? C35 C36 C37 120.1(7) . . ? C38 C37 C36 123.1(7) . . ? C37 C38 C39 117.0(6) . . ? C37 C38 C41 122.2(8) . . ? C39 C38 C41 120.7(8) . . ? C38 C39 C40 121.2(7) . . ? C35 C40 C39 122.0(7) . . ? C47 C42 C43 117.3(6) . . ? C47 C42 C20 121.7(6) . . ? C43 C42 C20 120.8(6) . . ? C42 C43 C44 120.8(7) . . ? C45 C44 C43 121.1(6) . . ? C46 C45 C44 117.7(6) . . ? C46 C45 C48 120.1(8) . . ? C44 C45 C48 122.1(7) . . ? C45 C46 C47 122.6(7) . . ? C42 C47 C46 120.4(7) . . ? O1 Yb2 O3 71.61(18) . . ? O1 Yb2 N4' 127.6(2) . . ? O3 Yb2 N4' 88.0(2) . . ? O1 Yb2 N2' 98.93(19) . . ? O3 Yb2 N2' 136.2(2) . . ? N4' Yb2 N2' 126.5(2) . . ? O1 Yb2 N3' 142.5(2) . . ? O3 Yb2 N3' 85.9(2) . . ? N4' Yb2 N3' 79.4(2) . . ? N2' Yb2 N3' 76.7(2) . . ? O1 Yb2 N1' 90.12(19) . . ? O3 Yb2 N1' 141.9(2) . . ? N4' Yb2 N1' 77.0(2) . . ? N2' Yb2 N1' 78.3(2) . . ? N3' Yb2 N1' 124.3(2) . . ? O1 Yb2 Yb1 37.99(13) . . ? O3 Yb2 Yb1 33.95(12) . . ? N4' Yb2 Yb1 112.52(17) . . ? N2' Yb2 Yb1 120.77(14) . . ? N3' Yb2 Yb1 112.61(16) . . ? N1' Yb2 Yb1 123.03(15) . . ? C1' N1' C4' 106.8(7) . . ? C1' N1' Yb2 126.3(5) . . ? C4' N1' Yb2 123.0(5) . . ? C9' N2' C6' 105.8(6) . . ? C9' N2' Yb2 126.1(5) . . ? C6' N2' Yb2 123.9(5) . . ? C11' N3' C14' 106.5(6) . . ? C11' N3' Yb2 128.9(5) . . ? C14' N3' Yb2 119.6(5) . . ? C19' N4' C16' 105.0(6) . . ? C19' N4' Yb2 127.0(5) . . ? C16' N4' Yb2 121.3(5) . . ? N1' C1' C20' 127.1(7) . . ? N1' C1' C2' 108.2(7) . . ? C20' C1' C2' 124.6(7) . . ? C3' C2' C1' 108.7(8) . . ? C2' C3' C4' 106.5(8) . . ? N1' C4' C3' 109.8(7) . . ? N1' C4' C5' 124.8(7) . . ? C3' C4' C5' 125.1(7) . . ? C6' C5' C4' 127.3(7) . . ? C6' C5' C21' 116.4(7) . . ? C4' C5' C21' 116.1(7) . . ? N2' C6' C5' 123.8(7) . . ? N2' C6' C7' 109.2(7) . . ? C5' C6' C7' 126.7(7) . . ? C8' C7' C6' 109.7(7) . . ? C7' C8' C9' 106.6(8) . . ? C10' C9' N2' 127.1(7) . . ? C10' C9' C8' 124.3(8) . . ? N2' C9' C8' 108.6(7) . . ? C9' C10' C11' 123.8(7) . . ? C9' C10' C28' 119.7(7) . . ? C11' C10' C28' 116.4(7) . . ? N3' C11' C12' 111.9(7) . . ? N3' C11' C10' 124.2(7) . . ? C12' C11' C10' 123.9(7) . . ? C13' C12' C11' 103.5(8) . . ? C12' C13' C14' 111.4(8) . . ? C15' C14' N3' 126.4(7) . . ? C15' C14' C13' 126.7(7) . . ? N3' C14' C13' 106.7(7) . . ? C16' C15' C14' 127.8(7) . . ? C16' C15' C35' 118.7(7) . . ? C14' C15' C35' 113.5(7) . . ? C15' C16' C17' 127.7(7) . . ? C15' C16' N4' 123.2(7) . . ? C17' C16' N4' 108.9(7) . . ? C18' C17' C16' 108.7(7) . . ? C17' C18' C19' 106.5(8) . . ? N4' C19' C20' 125.3(7) . . ? N4' C19' C18' 110.8(7) . . ? C20' C19' C18' 123.8(8) . . ? C1' C20' C19' 123.2(8) . . ? C1' C20' C42' 117.7(7) . . ? C19' C20' C42' 119.1(7) . . ? C22' C21' C26' 117.6(6) . . ? C22' C21' C5' 123.5(5) . . ? C26' C21' C5' 118.9(6) . . ? C21' C22' C23' 122.3(6) . . ? C24' C23' C22' 119.9(6) . . ? C23' C24' C25' 118.1(6) . . ? C23' C24' C27' 119.9(7) . . ? C25' C24' C27' 121.9(6) . . ? C24' C25' C26' 122.2(6) . . ? C21' C26' C25' 119.8(7) . . ? C29' C28' C33' 116.5(6) . . ? C29' C28' C10' 121.3(6) . . ? C33' C28' C10' 122.2(6) . . ? C28' C29' C30' 122.2(6) . . ? C31' C30' C29' 120.4(7) . . ? C32' C31' C30' 118.1(6) . . ? C32' C31' C34' 121.1(8) . . ? C30' C31' C34' 120.8(8) . . ? C31' C32' C33' 122.0(7) . . ? C28' C33' C32' 120.7(7) . . ? C40' C35' C36' 117.3(6) . . ? C40' C35' C15' 120.0(5) . . ? C36' C35' C15' 122.5(6) . . ? C35' C36' C37' 120.1(6) . . ? C38' C37' C36' 122.2(6) . . ? C37' C38' C39' 118.0(6) . . ? C37' C38' C41' 121.1(6) . . ? C39' C38' C41' 120.9(7) . . ? C38' C39' C40' 121.1(7) . . ? C35' C40' C39' 121.3(6) . . ? C43' C42' C47' 117.1(7) . . ? C43' C42' C20' 121.5(7) . . ? C47' C42' C20' 121.4(7) . . ? C42' C43' C44' 120.7(8) . . ? C45' C44' C43' 121.5(8) . . ? C46' C45' C44' 118.6(7) . . ? C46' C45' C48' 121.0(9) . . ? C44' C45' C48' 120.4(9) . . ? C45' C46' C47' 120.1(8) . . ? C42' C47' C46' 122.0(8) . . ? C49 O1 Yb2 126.2(4) . . ? C49 O1 Yb1 111.3(5) . . ? Yb2 O1 Yb1 106.68(19) . . ? O1 C49 C50 109.4(7) . . ? O2 C50 C49 105.6(7) . . ? C50 O2 C51 108.5(7) . . ? C50 O2 Yb1 118.6(5) . . ? C51 O2 Yb1 127.6(6) . . ? Yb1 O3 Yb2 111.9(2) . . ? C54 O4 C52 110.5(7) . . ? O4 C52 C53 109.6(8) . . ? O4 C54 C55 110.3(7) . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 0.708 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.118 #----------------------------------------------------------------------------- data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54.50 H52 Cl N4 O4 Yb' _chemical_formula_weight 1035.49 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.680(1) _cell_length_b 14.740(2) _cell_length_c 14.969(1) _cell_angle_alpha 64.59(1) _cell_angle_beta 87.25(1) _cell_angle_gamma 70.34(1) _cell_volume 2550.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used '202 from 4 still frames' _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 1.932 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 1.122 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV / 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS IIc' _diffrn_measurement_method ; Data was collected to 0.82\%A and 85% completeness by taking 27 oscillation frames in the range of 0 - 162\%, \D\f = 6\%, 8 min. per frame. Crystal to detector distance is 78.150mm, background level -100. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8136 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.51 _reflns_number_total 8136 _reflns_number_gt 7802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BioteX 1.0 (MSC, 1995)' _computing_cell_refinement 'BioteX 1.0 (MSC, 1995)' _computing_data_reduction 'BioteX 1.0 (MSC, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PC (Siemens, 1990)' _computing_publication_material 'Siemens 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^)+(0.1131P)^2^+1.2659P] 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 SHELXL _refine_ls_extinction_coef 0.0159(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8136 _refine_ls_number_parameters 615 _refine_ls_number_restraints 398 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1539 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 1.203 _refine_ls_shift/su_mean 0.021 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.512609(15) 1.239496(15) 1.368846(14) 0.05515(9) Uani 1 1 d . . . Cl1 Cl 0.37177(14) 1.14704(14) 1.43359(16) 0.0907(5) Uani 1 1 d . . . N1 N 0.5801(3) 1.3014(4) 1.4614(3) 0.0593(10) Uani 1 1 d D . . N2 N 0.6560(3) 1.2723(3) 1.2864(3) 0.0560(10) Uani 1 1 d D . . N3 N 0.4419(3) 1.3443(3) 1.2021(3) 0.0576(10) Uani 1 1 d D . . N4 N 0.3689(3) 1.3770(3) 1.3749(3) 0.0579(10) Uani 1 1 d D . . C1 C 0.5308(4) 1.3229(4) 1.5366(4) 0.0614(13) Uani 1 1 d D . . C2 C 0.6085(5) 1.3070(5) 1.6088(5) 0.0741(16) Uani 1 1 d D . . H2 H 0.5964 1.3143 1.6675 0.089 Uiso 1 1 calc R . . C3 C 0.7023(5) 1.2795(5) 1.5753(4) 0.0718(15) Uani 1 1 d D . . H3 H 0.7667 1.2652 1.6062 0.086 Uiso 1 1 calc R . . C4 C 0.6843(4) 1.2765(4) 1.4840(4) 0.0616(13) Uani 1 1 d D . . C5 C 0.7632(4) 1.2561(4) 1.4237(4) 0.0625(13) Uani 1 1 d . . . C6 C 0.7481(4) 1.2576(4) 1.3310(4) 0.0614(12) Uani 1 1 d D . . C7 C 0.8267(5) 1.2547(6) 1.2637(5) 0.0781(17) Uani 1 1 d D . . H7 H 0.8961 1.2451 1.2767 0.094 Uiso 1 1 calc R . . C8 C 0.7826(5) 1.2680(5) 1.1797(5) 0.0756(16) Uani 1 1 d D . . H8 H 0.8151 1.2699 1.1232 0.091 Uiso 1 1 calc R . . C9 C 0.6736(4) 1.2790(5) 1.1927(4) 0.0633(13) Uani 1 1 d D . . C10 C 0.5997(4) 1.2990(4) 1.1190(4) 0.0614(13) Uani 1 1 d . . . C11 C 0.4919(4) 1.3280(4) 1.1250(4) 0.0618(13) Uani 1 1 d D . . C12 C 0.4138(5) 1.3561(5) 1.0462(4) 0.0728(16) Uani 1 1 d D . . H12 H 0.4263 1.3518 0.9863 0.087 Uiso 1 1 calc R . . C13 C 0.3204(5) 1.3895(5) 1.0763(4) 0.0748(16) Uani 1 1 d D . . H13 H 0.2559 1.4119 1.0410 0.090 Uiso 1 1 calc R . . C14 C 0.3368(4) 1.3847(4) 1.1723(4) 0.0612(13) Uani 1 1 d D . . C15 C 0.2584(4) 1.4238(5) 1.2251(4) 0.0626(13) Uani 1 1 d . . . C16 C 0.2751(4) 1.4221(4) 1.3170(4) 0.0613(13) Uani 1 1 d D . . C17 C 0.1950(5) 1.4729(5) 1.3635(5) 0.0705(15) Uani 1 1 d D . . H17 H 0.1250 1.5105 1.3384 0.085 Uiso 1 1 calc R . . C18 C 0.2398(5) 1.4561(5) 1.4496(5) 0.0713(15) Uani 1 1 d D . . H18 H 0.2062 1.4798 1.4952 0.086 Uiso 1 1 calc R . . C19 C 0.3501(4) 1.3944(4) 1.4590(4) 0.0599(12) Uani 1 1 d D . . C20 C 0.4216(4) 1.3662(4) 1.5356(4) 0.0617(13) Uani 1 1 d . . . C21 C 0.8712(4) 1.2412(5) 1.4571(4) 0.0711(14) Uani 1 1 d D . . C22 C 0.9000(5) 1.3292(6) 1.4373(5) 0.095(2) Uani 1 1 d D . . H22 H 0.8499 1.3976 1.4071 0.114 Uiso 1 1 calc R . . C23 C 1.0017(6) 1.3177(8) 1.4614(6) 0.126(3) Uani 1 1 d D . . H23 H 1.0197 1.3773 1.4480 0.151 Uiso 1 1 calc R . . C24 C 1.0737(6) 1.2180(8) 1.5045(7) 0.137(4) Uani 1 1 d D . . H24 H 1.1421 1.2091 1.5207 0.165 Uiso 1 1 calc R . . C25 C 1.0482(6) 1.1311(9) 1.5244(8) 0.137(4) Uani 1 1 d D . . H25 H 1.0995 1.0633 1.5537 0.165 Uiso 1 1 calc R . . C26 C 0.9468(5) 1.1406(6) 1.5020(7) 0.111(3) Uani 1 1 d D . . H26 H 0.9301 1.0798 1.5171 0.133 Uiso 1 1 calc R . . C27 C 0.6372(4) 1.2925(4) 1.0252(4) 0.0667(14) Uani 1 1 d D . . C28 C 0.7064(5) 1.1974(5) 1.0283(5) 0.088(2) Uani 1 1 d D . . H28 H 0.7296 1.1369 1.0891 0.105 Uiso 1 1 calc R . . C29 C 0.7417(6) 1.1915(6) 0.9416(5) 0.100(2) Uani 1 1 d D . . H29 H 0.7903 1.1278 0.9455 0.120 Uiso 1 1 calc R . . C30 C 0.7064(5) 1.2768(6) 0.8522(5) 0.095(2) Uani 1 1 d D . . H30 H 0.7284 1.2715 0.7943 0.114 Uiso 1 1 calc R . . C31 C 0.6377(5) 1.3715(6) 0.8475(4) 0.0789(18) Uani 1 1 d D . . H31 H 0.6132 1.4305 0.7859 0.095 Uiso 1 1 calc R . . C32 C 0.6043(5) 1.3808(5) 0.9325(4) 0.0729(15) Uani 1 1 d D . . H32 H 0.5596 1.4465 0.9280 0.087 Uiso 1 1 calc R . . C33 C 0.1487(4) 1.4775(5) 1.1734(4) 0.0683(14) Uani 1 1 d D . . C34 C 0.1228(5) 1.5744(6) 1.0907(5) 0.087(2) Uani 1 1 d D . . H34 H 0.1733 1.6055 1.0665 0.104 Uiso 1 1 calc R . . C35 C 0.0214(5) 1.6266(7) 1.0428(6) 0.101(3) Uani 1 1 d D . . H35 H 0.0037 1.6925 0.9871 0.121 Uiso 1 1 calc R . . C36 C -0.0508(6) 1.5803(7) 1.0781(6) 0.104(3) Uani 1 1 d D . . H36 H -0.1183 1.6148 1.0455 0.124 Uiso 1 1 calc R . . C37 C -0.0277(5) 1.4848(7) 1.1598(6) 0.103(2) Uani 1 1 d D . . H37 H -0.0790 1.4548 1.1835 0.123 Uiso 1 1 calc R . . C38 C 0.0729(5) 1.4327(6) 1.2074(5) 0.0859(19) Uani 1 1 d D . . H38 H 0.0896 1.3668 1.2631 0.103 Uiso 1 1 calc R . . C39 C 0.3821(4) 1.3835(4) 1.6247(4) 0.0629(13) Uani 1 1 d D . . C40 C 0.4082(4) 1.4508(4) 1.6527(4) 0.0687(14) Uani 1 1 d D . . H40 H 0.4517 1.4865 1.6159 0.082 Uiso 1 1 calc R . . C41 C 0.3711(5) 1.4665(5) 1.7342(5) 0.0789(17) Uani 1 1 d D . . H41 H 0.3893 1.5125 1.7520 0.095 Uiso 1 1 calc R . . C42 C 0.3083(5) 1.4146(6) 1.7880(5) 0.085(2) Uani 1 1 d D . . H42 H 0.2839 1.4246 1.8434 0.102 Uiso 1 1 calc R . . C43 C 0.2799(6) 1.3478(6) 1.7627(5) 0.088(2) Uani 1 1 d D . . H43 H 0.2362 1.3129 1.8004 0.106 Uiso 1 1 calc R . . C44 C 0.3162(5) 1.3321(5) 1.6808(5) 0.0807(17) Uani 1 1 d D . . H44 H 0.2965 1.2869 1.6632 0.097 Uiso 1 1 calc R . . O1W O 0.6173(4) 1.0851(3) 1.5033(3) 0.0793(12) Uani 1 1 d . . . O1 O 0.5704(3) 1.1020(3) 1.3101(3) 0.0739(11) Uani 1 1 d D . . C45 C 0.5051(6) 1.0758(6) 1.2603(6) 0.099(2) Uani 1 1 d D . . H45A H 0.4958 1.1206 1.1891 0.119 Uiso 1 1 calc R . . H45B H 0.4371 1.0862 1.2845 0.119 Uiso 1 1 calc R . . C46 C 0.5591(8) 0.9621(7) 1.2827(9) 0.135(4) Uani 1 1 d D . . H46A H 0.5381 0.9158 1.3429 0.162 Uiso 1 1 calc R . . H46B H 0.5438 0.9481 1.2282 0.162 Uiso 1 1 calc R . . C47 C 0.6690(8) 0.9452(7) 1.2957(9) 0.133(3) Uani 1 1 d D . . H47A H 0.6999 0.9513 1.2346 0.160 Uiso 1 1 calc R . . H47B H 0.7057 0.8744 1.3482 0.160 Uiso 1 1 calc R . . C48 C 0.6755(5) 1.0288(5) 1.3223(6) 0.0836(19) Uani 1 1 d D . . H48A H 0.7064 0.9968 1.3906 0.100 Uiso 1 1 calc R . . H48B H 0.7183 1.0663 1.2792 0.100 Uiso 1 1 calc R . . O2 O 0.7556(6) 1.0014(5) 1.6718(5) 0.146(3) Uani 1 1 d DU . . C49 C 0.8254(10) 0.8955(9) 1.6924(8) 0.169(5) Uani 1 1 d DU . . H49A H 0.7901 0.8583 1.6734 0.203 Uiso 1 1 calc R . . H49B H 0.8852 0.8991 1.6552 0.203 Uiso 1 1 calc R . . C50 C 0.8582(14) 0.8409(11) 1.7959(9) 0.229(8) Uani 1 1 d DU . . H50A H 0.8393 0.7771 1.8254 0.275 Uiso 1 1 calc R . . H50B H 0.9335 0.8191 1.8074 0.275 Uiso 1 1 calc R . . C51 C 0.8098(14) 0.9093(11) 1.8390(8) 0.212(7) Uani 1 1 d DU . . H51A H 0.8620 0.9195 1.8717 0.255 Uiso 1 1 calc R . . H51B H 0.7671 0.8787 1.8884 0.255 Uiso 1 1 calc R . . C52 C 0.7453(12) 1.0110(9) 1.7611(8) 0.168(5) Uani 1 1 d DU . . H52A H 0.6729 1.0275 1.7745 0.202 Uiso 1 1 calc R . . H52B H 0.7681 1.0680 1.7572 0.202 Uiso 1 1 calc R . . O3 O -0.1008(16) 1.9449(13) 1.1262(19) 0.211(9) Uani 0.50 1 d PDU . . C53 C -0.0963(19) 1.8480(16) 1.1256(16) 0.188(8) Uani 0.50 1 d PDU . . H53A H -0.0565 1.8366 1.0736 0.226 Uiso 0.50 1 calc PR . . H53B H -0.1658 1.8480 1.1156 0.226 Uiso 0.50 1 calc PR . . C54 C -0.0446(17) 1.7667(14) 1.2229(16) 0.161(7) Uani 0.50 1 d PDU . . H54A H -0.0944 1.7584 1.2715 0.193 Uiso 0.50 1 calc PR . . H54B H -0.0095 1.6982 1.2215 0.193 Uiso 0.50 1 calc PR . . C55 C 0.0285(15) 1.8049(16) 1.2456(16) 0.163(7) Uani 0.50 1 d PDU . . H55A H 0.0965 1.7741 1.2277 0.196 Uiso 0.50 1 calc PR . . H55B H 0.0351 1.7858 1.3162 0.196 Uiso 0.50 1 calc PR . . C56 C -0.011(2) 1.9198(16) 1.188(2) 0.193(8) Uani 0.50 1 d PDU . . H56A H -0.0297 1.9546 1.2320 0.232 Uiso 0.50 1 calc PR . . H56B H 0.0411 1.9437 1.1483 0.232 Uiso 0.50 1 calc PR . . O4 O 0.4171(18) 1.009(3) 2.022(2) 0.265(12) Uani 0.50 1 d PDU A -1 H4 H 0.3971 1.0070 2.0754 0.398 Uiso 0.50 1 calc PR A -1 C57 C 0.463(3) 1.089(2) 1.980(2) 0.228(14) Uani 0.50 1 d PDU A -1 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 0.05537(15) 0.05347(13) 0.05419(13) -0.02612(10) 0.00339(9) -0.01251(10) Cl1 0.0760(9) 0.0704(9) 0.1245(14) -0.0391(9) 0.0237(9) -0.0309(8) N1 0.057(2) 0.068(2) 0.057(2) -0.0357(19) 0.0033(17) -0.016(2) N2 0.051(2) 0.062(2) 0.054(2) -0.0283(18) 0.0083(16) -0.0154(19) N3 0.054(2) 0.054(2) 0.051(2) -0.0230(17) -0.0020(17) -0.0025(19) N4 0.051(2) 0.055(2) 0.059(2) -0.0282(18) -0.0002(17) -0.0034(18) C1 0.061(3) 0.068(3) 0.059(3) -0.038(2) 0.005(2) -0.014(2) C2 0.067(3) 0.088(4) 0.070(3) -0.048(3) 0.000(3) -0.011(3) C3 0.059(3) 0.086(4) 0.068(3) -0.039(3) -0.002(2) -0.015(3) C4 0.061(3) 0.065(3) 0.061(3) -0.032(2) 0.007(2) -0.019(2) C5 0.056(3) 0.063(3) 0.065(3) -0.032(2) 0.002(2) -0.012(2) C6 0.053(3) 0.065(3) 0.070(3) -0.037(2) 0.009(2) -0.017(2) C7 0.056(3) 0.105(4) 0.081(4) -0.052(3) 0.012(3) -0.023(3) C8 0.062(3) 0.095(4) 0.071(3) -0.044(3) 0.014(2) -0.019(3) C9 0.059(3) 0.069(3) 0.059(3) -0.032(2) 0.011(2) -0.013(2) C10 0.065(3) 0.057(3) 0.057(3) -0.028(2) 0.002(2) -0.012(2) C11 0.060(3) 0.073(3) 0.057(3) -0.032(2) 0.009(2) -0.025(2) C12 0.066(3) 0.088(4) 0.062(3) -0.038(3) 0.004(2) -0.017(3) C13 0.073(4) 0.085(4) 0.067(3) -0.041(3) 0.000(3) -0.017(3) C14 0.059(3) 0.061(3) 0.055(3) -0.025(2) 0.002(2) -0.011(2) C15 0.058(3) 0.063(3) 0.061(3) -0.025(2) 0.007(2) -0.018(2) C16 0.060(3) 0.063(3) 0.061(3) -0.030(2) 0.008(2) -0.016(2) C17 0.058(3) 0.078(3) 0.075(3) -0.042(3) 0.007(2) -0.012(3) C18 0.061(3) 0.081(4) 0.071(3) -0.043(3) 0.009(2) -0.011(3) C19 0.056(3) 0.060(3) 0.064(3) -0.035(2) 0.007(2) -0.010(2) C20 0.067(3) 0.062(3) 0.061(3) -0.035(2) 0.010(2) -0.019(2) C21 0.061(3) 0.089(4) 0.074(3) -0.044(3) 0.009(2) -0.027(3) C22 0.078(4) 0.120(5) 0.101(5) -0.060(4) 0.006(4) -0.036(4) C23 0.103(5) 0.197(9) 0.115(6) -0.073(6) 0.017(5) -0.089(6) C24 0.065(4) 0.238(11) 0.133(7) -0.110(8) 0.006(4) -0.044(6) C25 0.069(5) 0.185(10) 0.160(8) -0.108(8) -0.016(5) 0.000(6) C26 0.078(4) 0.109(5) 0.137(7) -0.071(5) -0.026(4) 0.005(4) C27 0.065(3) 0.068(3) 0.062(3) -0.033(2) 0.006(2) -0.011(3) C28 0.094(5) 0.084(4) 0.071(4) -0.043(3) 0.006(3) -0.004(4) C29 0.094(5) 0.106(5) 0.103(5) -0.068(4) 0.021(4) -0.012(4) C30 0.084(4) 0.145(6) 0.071(4) -0.064(4) 0.018(3) -0.036(4) C31 0.077(4) 0.104(5) 0.059(3) -0.033(3) 0.009(3) -0.039(4) C32 0.075(4) 0.080(4) 0.068(3) -0.035(3) 0.011(3) -0.029(3) C33 0.055(3) 0.079(3) 0.070(3) -0.038(3) 0.003(2) -0.015(3) C34 0.069(4) 0.099(5) 0.072(4) -0.025(3) -0.002(3) -0.021(4) C35 0.072(4) 0.110(6) 0.086(5) -0.028(4) -0.012(3) -0.009(4) C36 0.065(4) 0.122(6) 0.100(5) -0.047(5) -0.016(4) -0.003(4) C37 0.065(4) 0.129(6) 0.132(6) -0.074(5) 0.015(4) -0.034(4) C38 0.066(4) 0.096(5) 0.088(4) -0.039(4) 0.004(3) -0.022(4) C39 0.061(3) 0.060(3) 0.062(3) -0.033(2) 0.007(2) -0.007(2) C40 0.072(3) 0.067(3) 0.070(3) -0.036(3) 0.008(3) -0.021(3) C41 0.075(4) 0.077(4) 0.087(4) -0.050(3) -0.004(3) -0.007(3) C42 0.068(4) 0.115(5) 0.070(4) -0.052(3) 0.005(3) -0.014(4) C43 0.087(4) 0.114(5) 0.076(4) -0.046(4) 0.029(3) -0.047(4) C44 0.087(4) 0.085(4) 0.085(4) -0.046(3) 0.023(3) -0.038(3) O1W 0.090(3) 0.058(2) 0.070(2) -0.0156(19) -0.018(2) -0.016(2) O1 0.088(3) 0.055(2) 0.071(2) -0.0313(18) 0.0005(19) -0.0091(19) C45 0.108(5) 0.099(5) 0.104(5) -0.057(4) -0.005(4) -0.032(4) C46 0.154(9) 0.111(6) 0.162(9) -0.081(6) 0.000(7) -0.044(6) C47 0.127(7) 0.114(6) 0.181(9) -0.100(6) 0.038(6) -0.026(6) C48 0.079(4) 0.068(4) 0.094(4) -0.036(3) 0.019(3) -0.015(3) O2 0.172(6) 0.112(4) 0.117(4) -0.033(4) -0.057(4) -0.019(4) C49 0.149(10) 0.166(8) 0.142(7) -0.073(6) -0.027(7) 0.018(8) C50 0.253(15) 0.161(9) 0.140(8) -0.039(7) -0.037(10) 0.055(10) C51 0.250(15) 0.176(11) 0.104(6) -0.035(6) -0.019(9) 0.022(10) C52 0.215(12) 0.122(7) 0.130(7) -0.051(6) -0.025(8) -0.013(7) O3 0.182(14) 0.151(8) 0.230(18) -0.057(10) -0.033(12) -0.001(13) C53 0.155(14) 0.187(12) 0.188(14) -0.092(12) -0.062(12) 0.004(14) C54 0.153(14) 0.149(9) 0.160(14) -0.081(10) -0.013(12) -0.006(11) C55 0.096(11) 0.235(12) 0.135(13) -0.088(12) 0.004(8) -0.019(11) C56 0.199(18) 0.217(12) 0.202(19) -0.121(14) 0.029(14) -0.080(14) O4 0.169(15) 0.37(2) 0.29(3) -0.16(2) 0.057(17) -0.115(17) C57 0.34(3) 0.135(19) 0.19(2) -0.062(17) -0.10(2) -0.061(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N1 2.320(4) . ? Yb1 O1W 2.331(4) . ? Yb1 N4 2.333(4) . ? Yb1 N3 2.339(4) . ? Yb1 N2 2.344(4) . ? Yb1 O1 2.428(4) . ? Yb1 Cl1 2.6388(18) . ? N1 C4 1.367(7) . ? N1 C1 1.382(7) . ? N2 C6 1.362(7) . ? N2 C9 1.379(7) . ? N3 C14 1.370(7) . ? N3 C11 1.382(7) . ? N4 C16 1.370(7) . ? N4 C19 1.386(7) . ? C1 C20 1.411(8) . ? C1 C2 1.443(8) . ? C2 C3 1.351(9) . ? C3 C4 1.422(8) . ? C4 C5 1.410(8) . ? C5 C6 1.402(8) . ? C5 C21 1.497(8) . ? C6 C7 1.440(8) . ? C7 C8 1.328(9) . ? C8 C9 1.457(8) . ? C9 C10 1.397(8) . ? C10 C11 1.400(8) . ? C10 C27 1.503(8) . ? C11 C12 1.451(8) . ? C12 C13 1.337(9) . ? C13 C14 1.433(8) . ? C14 C15 1.415(8) . ? C15 C16 1.395(8) . ? C15 C33 1.504(7) . ? C16 C17 1.437(8) . ? C17 C18 1.341(9) . ? C18 C19 1.452(8) . ? C19 C20 1.366(8) . ? C20 C39 1.505(7) . ? C21 C26 1.378(8) . ? C21 C22 1.388(8) . ? C22 C23 1.390(9) . ? C23 C24 1.348(10) . ? C24 C25 1.348(11) . ? C25 C26 1.388(9) . ? C27 C28 1.385(7) . ? C27 C32 1.391(7) . ? C28 C29 1.391(8) . ? C29 C30 1.347(8) . ? C30 C31 1.369(8) . ? C31 C32 1.378(8) . ? C33 C34 1.372(8) . ? C33 C38 1.376(8) . ? C34 C35 1.390(8) . ? C35 C36 1.346(9) . ? C36 C37 1.356(9) . ? C37 C38 1.380(8) . ? C39 C40 1.378(7) . ? C39 C44 1.391(8) . ? C40 C41 1.380(8) . ? C41 C42 1.349(8) . ? C42 C43 1.363(9) . ? C43 C44 1.382(8) . ? O1 C45 1.430(8) . ? O1 C48 1.441(7) . ? C45 C46 1.474(10) . ? C46 C47 1.447(12) . ? C47 C48 1.478(10) . ? O2 C52 1.399(10) . ? O2 C49 1.433(11) . ? C49 C50 1.415(12) . ? C50 C51 1.394(15) . ? C51 C52 1.447(12) . ? O3 C53 1.413(15) . ? O3 C56 1.419(15) . ? C53 C54 1.444(15) . ? C54 C55 1.417(18) . ? C55 C56 1.442(15) . ? O4 C57 1.419(19) . ? 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 N1 Yb1 O1W 75.13(16) . . ? N1 Yb1 N4 76.09(15) . . ? O1W Yb1 N4 127.17(17) . . ? N1 Yb1 N3 123.48(16) . . ? O1W Yb1 N3 154.82(18) . . ? N4 Yb1 N3 76.79(15) . . ? N1 Yb1 N2 77.52(16) . . ? O1W Yb1 N2 93.33(17) . . ? N4 Yb1 N2 122.00(16) . . ? N3 Yb1 N2 76.52(15) . . ? N1 Yb1 O1 139.19(15) . . ? O1W Yb1 O1 74.46(16) . . ? N4 Yb1 O1 144.68(16) . . ? N3 Yb1 O1 80.84(14) . . ? N2 Yb1 O1 77.75(16) . . ? N1 Yb1 Cl1 121.64(12) . . ? O1W Yb1 Cl1 81.89(13) . . ? N4 Yb1 Cl1 76.94(12) . . ? N3 Yb1 Cl1 98.67(13) . . ? N2 Yb1 Cl1 157.57(13) . . ? O1 Yb1 Cl1 79.86(12) . . ? C4 N1 C1 106.3(4) . . ? C4 N1 Yb1 124.5(3) . . ? C1 N1 Yb1 123.1(4) . . ? C6 N2 C9 107.0(4) . . ? C6 N2 Yb1 125.4(3) . . ? C9 N2 Yb1 125.3(4) . . ? C14 N3 C11 106.6(4) . . ? C14 N3 Yb1 123.0(3) . . ? C11 N3 Yb1 122.7(3) . . ? C16 N4 C19 107.2(4) . . ? C16 N4 Yb1 124.8(3) . . ? C19 N4 Yb1 123.4(3) . . ? N1 C1 C20 124.9(5) . . ? N1 C1 C2 108.9(5) . . ? C20 C1 C2 125.8(5) . . ? C3 C2 C1 107.1(5) . . ? C2 C3 C4 107.3(5) . . ? N1 C4 C5 125.6(5) . . ? N1 C4 C3 110.3(5) . . ? C5 C4 C3 124.0(5) . . ? C6 C5 C4 125.9(5) . . ? C6 C5 C21 116.7(5) . . ? C4 C5 C21 117.1(5) . . ? N2 C6 C5 125.9(5) . . ? N2 C6 C7 109.3(5) . . ? C5 C6 C7 124.5(5) . . ? C8 C7 C6 108.1(6) . . ? C7 C8 C9 107.1(5) . . ? N2 C9 C10 126.8(5) . . ? N2 C9 C8 108.5(5) . . ? C10 C9 C8 124.6(5) . . ? C11 C10 C9 124.5(5) . . ? C11 C10 C27 117.2(5) . . ? C9 C10 C27 118.2(5) . . ? N3 C11 C10 125.9(5) . . ? N3 C11 C12 108.9(5) . . ? C10 C11 C12 125.0(5) . . ? C13 C12 C11 106.9(5) . . ? C12 C13 C14 108.2(6) . . ? N3 C14 C15 124.6(5) . . ? N3 C14 C13 109.4(5) . . ? C15 C14 C13 125.9(5) . . ? C16 C15 C14 125.7(5) . . ? C16 C15 C33 118.0(5) . . ? C14 C15 C33 116.2(5) . . ? N4 C16 C15 126.3(5) . . ? N4 C16 C17 109.4(5) . . ? C15 C16 C17 124.2(5) . . ? C18 C17 C16 107.5(5) . . ? C17 C18 C19 107.9(5) . . ? C20 C19 N4 127.4(5) . . ? C20 C19 C18 124.5(5) . . ? N4 C19 C18 108.0(5) . . ? C19 C20 C1 124.5(5) . . ? C19 C20 C39 118.2(5) . . ? C1 C20 C39 117.3(5) . . ? C26 C21 C22 118.1(6) . . ? C26 C21 C5 121.2(6) . . ? C22 C21 C5 120.6(5) . . ? C21 C22 C23 121.7(7) . . ? C24 C23 C22 118.5(8) . . ? C23 C24 C25 121.1(8) . . ? C24 C25 C26 121.3(8) . . ? C25 C26 C21 119.2(8) . . ? C28 C27 C32 117.6(5) . . ? C28 C27 C10 120.7(5) . . ? C32 C27 C10 121.8(5) . . ? C27 C28 C29 120.7(6) . . ? C30 C29 C28 120.9(6) . . ? C29 C30 C31 119.2(6) . . ? C30 C31 C32 121.1(6) . . ? C31 C32 C27 120.4(6) . . ? C34 C33 C38 118.8(6) . . ? C34 C33 C15 119.5(5) . . ? C38 C33 C15 121.8(5) . . ? C33 C34 C35 120.5(7) . . ? C36 C35 C34 119.2(7) . . ? C35 C36 C37 121.8(7) . . ? C36 C37 C38 119.2(7) . . ? C33 C38 C37 120.6(7) . . ? C40 C39 C44 117.9(5) . . ? C40 C39 C20 121.9(5) . . ? C44 C39 C20 120.2(5) . . ? C41 C40 C39 121.4(6) . . ? C42 C41 C40 119.4(6) . . ? C41 C42 C43 121.2(6) . . ? C42 C43 C44 119.8(6) . . ? C43 C44 C39 120.3(6) . . ? C45 O1 C48 107.2(5) . . ? C45 O1 Yb1 126.0(4) . . ? C48 O1 Yb1 126.7(4) . . ? O1 C45 C46 106.1(6) . . ? C47 C46 C45 104.7(7) . . ? C46 C47 C48 106.5(6) . . ? O1 C48 C47 107.0(6) . . ? C52 O2 C49 108.7(7) . . ? C50 C49 O2 107.3(9) . . ? C51 C50 C49 108.8(9) . . ? C50 C51 C52 108.1(9) . . ? O2 C52 C51 107.1(9) . . ? C53 O3 C56 106.4(14) . . ? O3 C53 C54 104.0(14) . . ? C55 C54 C53 104.6(13) . . ? C54 C55 C56 106.4(12) . . ? O3 C56 C55 106.6(13) . . ? _diffrn_measured_fraction_theta_max 0.855 _diffrn_reflns_theta_full 25.51 _diffrn_measured_fraction_theta_full 0.855 _refine_diff_density_max 1.610 _refine_diff_density_min -1.600 _refine_diff_density_rms 0.127 #===End