data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Parker, David' _publ_contact_author_address ;Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE ; _publ_contact_author_email David.Parker@durham.ac.uk _publ_contact_author_phone '0191 334 2033' _publ_contact_author_fax '0191 384 4737' _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_year ? _ccdc_journal_depnumber ? _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_address A.L.Thompson ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; D.Parker ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; D.A.Fulton ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; J.A.K.Howard ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; S.Pandya ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; ; H.Puschmann ; ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; P.A.Stenson ;Department of Chemistry, University of Durham, South Rd., Durham, UK. DH1 3LE ; M.Botta ;Dipartimento di Scienzedell'Ambiente e della Vita, Universit\`a del Peimonte Orientale "Amadeo Avegadro", Via Bellini 25/G, 1-15100, Alesandria, Italy. ; S.Aime ;Dipartimento di Chimica IFM, Universit\`a degli Studi di Torino, 7 Via P Giuria, 10125 Torino, Italy. ; _publ_section_title ; On the Role of the Counter-ion in Defining Water Structure and dynamics: Order, Structure and Dynamics in Hydrophilic and Hydrophobic Gadolinium Salt Complexes. ; _publ_section_abstract ; The crystal structures of the hydrated salts of [Gd.DOTAM]^3+^] and it's more hydrophobic derivative ([Gd.2]^3+^], bearing 4 alpha-phenylethyl groups, Gd and Yb salts) are reported and compared. The nature of the anion determines the degree of ordering in the lattice and the extent of hydration. These effects are correlated with the results of ^17^O and ^1^H NMR measurements of water exchange dynamics in solution. With [Gd.DOTAM]^3+^, structural ordering in the hydrated lattice follows the sequence Cl^-^ > Br^-^>I^-^ and this order also defines the water exchange reate in solution: 7.5, 19.5, 33.3x10^4^ s^-1^ (298 K). For [Gd.2]^3+^ salts, the measured relaxivity is determined purely by the outer sphere term and the water exchange rate at 298 K is very similar (typically 1 x 10^4^ s^-1^) for chloride, bromide, iodide, acetate, triflate and nitrate salts, notwithstanding the different nature and extent of hydration found in the crystalline lattice. ; #============================================================================== data_[Gd.1]Cl3 _database_code_depnum_ccdc_archive 'CCDC 606215' #============================================================================== _chemical_name_systematic ; [Gd.DOTAM]Cl~3~.6H~2~O ; _chemical_name_common (Gd.DOTAM)Cl!3$.6H!2$O _chemical_melting_point 'not measured' _chemical_formula_moiety 'C16 H34 Gd N8 O5, 6(H2 O), 3Cl' _chemical_formula_sum 'C16 H46 Cl3 Gd N8 O11' _chemical_formula_weight 790.21 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' Gd Gd -0.1653 3.9035 '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 9.8684(4) _cell_length_b 12.3433(5) _cell_length_c 13.2434(5) _cell_angle_alpha 75.354(1) _cell_angle_beta 76.572(1) _cell_angle_gamma 83.254(1) _cell_volume 1515.12(10) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7004 _cell_measurement_theta_min 2.618 _cell_measurement_theta_max 29.883 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 802 _exptl_absorpt_coefficient_mu 2.516 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.908313 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 15766 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8138 _reflns_number_gt 7850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.6680P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8138 _refine_ls_number_parameters 397 _refine_ls_number_restraints 133 _refine_ls_R_factor_all 0.0179 _refine_ls_R_factor_gt 0.0169 _refine_ls_wR_factor_ref 0.0410 _refine_ls_wR_factor_gt 0.0407 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.792413(7) 0.730578(5) 0.654605(5) 0.00814(2) Uani 1 1 d . . . O1 O 0.94664(11) 0.58703(9) 0.59108(8) 0.0124(2) Uani 1 1 d . . . O2 O 0.62690(11) 0.64908(9) 0.59907(9) 0.0133(2) Uani 1 1 d . . . O3 O 0.66302(11) 0.90591(9) 0.60263(9) 0.0137(2) Uani 1 1 d . . . O4 O 0.99165(11) 0.83286(9) 0.59238(9) 0.0133(2) Uani 1 1 d . . . N1 N 0.97401(13) 0.63462(10) 0.77729(10) 0.0109(2) Uani 1 1 d . . . N2 N 0.71105(13) 0.53537(10) 0.78400(10) 0.0109(2) Uani 1 1 d . . . N3 N 0.55499(13) 0.75552(10) 0.79056(10) 0.0108(2) Uani 1 1 d . . . N4 N 0.81965(13) 0.85691(10) 0.78198(10) 0.0118(2) Uani 1 1 d . . . N5 N 1.13439(14) 0.46435(11) 0.58836(11) 0.0157(3) Uani 1 1 d . . . H5C H 1.1133 0.4392 0.5394 0.019 Uiso 1 1 calc R . . H5D H 1.2076 0.4369 0.6130 0.019 Uiso 1 1 calc R . . N6 N 0.47354(14) 0.52079(11) 0.61892(12) 0.0173(3) Uani 1 1 d . . . H6C H 0.4308 0.5653 0.5734 0.021 Uiso 1 1 calc R . . H6D H 0.4450 0.4548 0.6494 0.021 Uiso 1 1 calc R . . N7 N 0.47081(14) 1.02362(11) 0.62755(11) 0.0161(3) Uani 1 1 d . . . H7C H 0.5114 1.0790 0.5815 0.019 Uiso 1 1 calc R . . H7D H 0.3858 1.0328 0.6604 0.019 Uiso 1 1 calc R . . N8 N 1.12653(14) 0.96849(11) 0.58957(12) 0.0173(3) Uani 1 1 d . . . H8C H 1.1900 0.9492 0.5396 0.021 Uiso 1 1 calc R . . H8D H 1.1378 1.0236 0.6150 0.021 Uiso 1 1 calc R . . C1 C 0.91333(16) 0.53963(12) 0.86471(12) 0.0131(3) Uani 1 1 d . . . H1A H 0.8542 0.5696 0.9221 0.016 Uiso 1 1 calc R . . H1B H 0.9885 0.4928 0.8928 0.016 Uiso 1 1 calc R . . C2 C 0.82798(16) 0.46764(12) 0.82813(12) 0.0126(3) Uani 1 1 d . . . H2A H 0.8880 0.4335 0.7739 0.015 Uiso 1 1 calc R . . H2B H 0.7907 0.4079 0.8881 0.015 Uiso 1 1 calc R . . C3 C 0.59679(16) 0.55389(12) 0.87516(12) 0.0127(3) Uani 1 1 d . . . H3A H 0.6373 0.5724 0.9283 0.015 Uiso 1 1 calc R . . H3B H 0.5503 0.4847 0.9080 0.015 Uiso 1 1 calc R . . C4 C 0.48910(16) 0.64685(12) 0.84241(12) 0.0125(3) Uani 1 1 d . . . H4A H 0.4432 0.6264 0.7932 0.015 Uiso 1 1 calc R . . H4B H 0.4187 0.6555 0.9050 0.015 Uiso 1 1 calc R . . C5 C 0.57678(16) 0.80745(13) 0.87576(12) 0.0140(3) Uani 1 1 d . . . H5A H 0.6098 0.7491 0.9305 0.017 Uiso 1 1 calc R . . H5B H 0.4877 0.8390 0.9085 0.017 Uiso 1 1 calc R . . C6 C 0.68043(16) 0.89915(13) 0.83540(12) 0.0141(3) Uani 1 1 d . . . H6A H 0.6441 0.9609 0.7853 0.017 Uiso 1 1 calc R . . H6B H 0.6911 0.9273 0.8950 0.017 Uiso 1 1 calc R . . C7 C 0.89549(17) 0.79336(13) 0.86633(12) 0.0145(3) Uani 1 1 d . . . H7A H 0.8306 0.7476 0.9231 0.017 Uiso 1 1 calc R . . H7B H 0.9290 0.8463 0.8965 0.017 Uiso 1 1 calc R . . C8 C 1.01868(16) 0.71801(12) 0.82536(12) 0.0136(3) Uani 1 1 d . . . H8A H 1.0872 0.7639 0.7722 0.016 Uiso 1 1 calc R . . H8B H 1.0625 0.6787 0.8839 0.016 Uiso 1 1 calc R . . C9 C 1.09762(15) 0.59194(12) 0.70720(12) 0.0119(3) Uani 1 1 d . . . H9A H 1.1491 0.5338 0.7503 0.014 Uiso 1 1 calc R . . H9B H 1.1587 0.6524 0.6710 0.014 Uiso 1 1 calc R . . C10 C 1.05449(16) 0.54509(12) 0.62557(12) 0.0112(3) Uani 1 1 d . . . C11 C 0.65877(16) 0.47286(12) 0.71999(12) 0.0128(3) Uani 1 1 d . . . H11A H 0.5959 0.4177 0.7670 0.015 Uiso 1 1 calc R . . H11B H 0.7365 0.4336 0.6814 0.015 Uiso 1 1 calc R . . C12 C 0.58289(16) 0.55363(12) 0.64205(12) 0.0120(3) Uani 1 1 d . . . C13 C 0.46043(16) 0.82993(12) 0.72702(12) 0.0131(3) Uani 1 1 d . . . H13A H 0.3834 0.8604 0.7743 0.016 Uiso 1 1 calc R . . H13B H 0.4223 0.7870 0.6892 0.016 Uiso 1 1 calc R . . C14 C 0.53889(16) 0.92484(12) 0.64776(12) 0.0126(3) Uani 1 1 d . . . C15 C 0.90038(16) 0.95271(12) 0.71292(13) 0.0146(3) Uani 1 1 d . . . H15A H 0.9438 0.9852 0.7560 0.018 Uiso 1 1 calc R . . H15B H 0.8379 1.0101 0.6797 0.018 Uiso 1 1 calc R . . C16 C 1.01198(16) 0.91356(12) 0.62724(12) 0.0125(3) Uani 1 1 d . . . Cl1 Cl 0.69996(4) 0.60622(3) 0.11689(3) 0.01849(7) Uani 1 1 d . . . Cl2 Cl 0.34164(4) 0.76128(3) 0.49356(3) 0.01878(8) Uani 1 1 d . . . Cl3 Cl 0.81177(4) 0.96341(3) 0.18818(3) 0.02084(8) Uani 1 1 d . . . O1W O 0.83692(12) 0.78160(9) 0.45781(9) 0.0133(2) Uani 1 1 d D . . H1WA H 0.9191(13) 0.7686(17) 0.4270(15) 0.020 Uiso 1 1 d D . . H1WB H 0.7839(17) 0.7678(17) 0.4230(15) 0.020 Uiso 1 1 d D . . O2W O 1.10423(13) 0.74023(12) 0.36879(11) 0.0245(3) Uani 1 1 d D . . H2WA H 1.152(2) 0.752(2) 0.4097(15) 0.037 Uiso 1 1 d D . . H2WB H 1.150(2) 0.768(2) 0.3068(11) 0.037 Uiso 1 1 d D . . O3W O 0.64069(13) 0.70699(10) 0.36149(10) 0.0182(2) Uani 1 1 d D . . H3WA H 0.5648(17) 0.7119(18) 0.4065(13) 0.027 Uiso 1 1 d D . . H3WB H 0.624(2) 0.7452(17) 0.3028(11) 0.027 Uiso 1 1 d D . . O4W O 1.27565(15) 0.82735(14) 0.17579(11) 0.0316(3) Uani 1 1 d D . . H4WA H 1.3615(16) 0.831(2) 0.171(2) 0.047 Uiso 1 1 d D . . H4WB H 1.267(2) 0.823(2) 0.1152(14) 0.047 Uiso 1 1 d D . . O5W O 1.20169(15) 0.80593(12) -0.01021(12) 0.0287(3) Uani 1 1 d D . . H5WA H 1.188(2) 0.8694(14) -0.0517(17) 0.043 Uiso 1 1 d D . . H5WB H 1.1206(18) 0.790(2) 0.0256(18) 0.043 Uiso 1 1 d D . . O6W O 0.56973(16) 0.83483(13) 0.15907(14) 0.0344(3) Uani 1 1 d D . . H6WA H 0.614(3) 0.7801(16) 0.135(2) 0.052 Uiso 1 1 d D . . H6WB H 0.631(3) 0.880(3) 0.152(5) 0.052 Uiso 0.50 1 d PD A 1 H6WC H 0.551(6) 0.882(3) 0.105(2) 0.052 Uiso 0.50 1 d PD B 2 O7W O 0.95440(14) 0.73717(12) 0.12870(13) 0.0296(3) Uani 1 1 d D . . H7WA H 0.889(2) 0.7028(19) 0.122(2) 0.044 Uiso 1 1 d D . . H7WB H 0.915(2) 0.7948(16) 0.151(2) 0.044 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.00799(4) 0.00790(3) 0.00858(4) -0.00220(2) -0.00142(2) -0.00074(2) O1 0.0115(5) 0.0135(5) 0.0124(5) -0.0040(4) -0.0035(4) 0.0021(4) O2 0.0137(5) 0.0132(5) 0.0130(5) -0.0009(4) -0.0034(4) -0.0039(4) O3 0.0121(5) 0.0129(5) 0.0139(5) -0.0017(4) -0.0005(4) 0.0007(4) O4 0.0122(5) 0.0139(5) 0.0145(5) -0.0043(4) -0.0021(4) -0.0030(4) N1 0.0109(6) 0.0121(5) 0.0105(6) -0.0038(4) -0.0025(5) -0.0010(4) N2 0.0109(6) 0.0105(5) 0.0111(6) -0.0019(4) -0.0023(5) -0.0008(4) N3 0.0103(6) 0.0106(5) 0.0113(6) -0.0022(4) -0.0018(5) -0.0011(4) N4 0.0106(6) 0.0120(5) 0.0130(6) -0.0041(4) -0.0013(5) -0.0012(4) N5 0.0139(6) 0.0162(6) 0.0203(7) -0.0089(5) -0.0073(5) 0.0043(5) N6 0.0166(7) 0.0139(6) 0.0228(7) -0.0007(5) -0.0086(6) -0.0048(5) N7 0.0138(6) 0.0126(6) 0.0175(7) -0.0004(5) 0.0010(5) 0.0012(5) N8 0.0149(7) 0.0160(6) 0.0218(7) -0.0070(5) -0.0001(5) -0.0054(5) C1 0.0140(7) 0.0143(6) 0.0106(7) -0.0011(5) -0.0036(5) -0.0013(5) C2 0.0128(7) 0.0112(6) 0.0128(7) -0.0004(5) -0.0037(5) 0.0006(5) C3 0.0117(7) 0.0134(6) 0.0109(7) -0.0010(5) 0.0002(5) -0.0014(5) C4 0.0114(7) 0.0120(6) 0.0124(7) -0.0018(5) 0.0002(5) -0.0020(5) C5 0.0134(7) 0.0166(7) 0.0123(7) -0.0062(5) -0.0002(6) -0.0015(5) C6 0.0127(7) 0.0159(7) 0.0147(7) -0.0075(5) -0.0014(6) 0.0005(5) C7 0.0166(7) 0.0155(7) 0.0132(7) -0.0057(5) -0.0048(6) 0.0001(6) C8 0.0137(7) 0.0149(6) 0.0150(7) -0.0060(5) -0.0058(6) -0.0012(5) C9 0.0102(7) 0.0143(6) 0.0121(7) -0.0045(5) -0.0029(5) 0.0003(5) C10 0.0118(7) 0.0108(6) 0.0100(6) -0.0017(5) -0.0009(5) -0.0015(5) C11 0.0139(7) 0.0101(6) 0.0149(7) -0.0023(5) -0.0044(6) -0.0011(5) C12 0.0116(7) 0.0131(6) 0.0109(7) -0.0042(5) -0.0003(5) -0.0011(5) C13 0.0105(7) 0.0125(6) 0.0151(7) -0.0019(5) -0.0021(5) 0.0003(5) C14 0.0138(7) 0.0129(6) 0.0117(7) -0.0035(5) -0.0032(5) -0.0008(5) C15 0.0147(7) 0.0122(6) 0.0177(7) -0.0057(5) -0.0014(6) -0.0028(5) C16 0.0130(7) 0.0119(6) 0.0131(7) -0.0020(5) -0.0049(6) -0.0005(5) Cl1 0.01882(18) 0.02062(17) 0.01567(17) -0.00195(14) -0.00382(14) -0.00448(14) Cl2 0.01312(17) 0.01776(17) 0.02231(19) -0.00058(14) -0.00216(14) -0.00058(13) Cl3 0.01747(18) 0.02160(18) 0.0242(2) -0.00957(15) -0.00130(15) -0.00102(14) O1W 0.0123(5) 0.0162(5) 0.0123(5) -0.0046(4) -0.0028(4) -0.0010(4) O2W 0.0174(6) 0.0366(7) 0.0197(6) -0.0079(5) -0.0017(5) -0.0038(5) O3W 0.0171(6) 0.0205(6) 0.0151(6) -0.0029(4) -0.0022(5) 0.0016(4) O4W 0.0236(7) 0.0483(9) 0.0238(7) -0.0080(6) -0.0031(6) -0.0102(6) O5W 0.0245(7) 0.0312(7) 0.0284(7) -0.0044(6) -0.0048(6) -0.0010(6) O6W 0.0248(7) 0.0350(8) 0.0483(9) -0.0214(7) -0.0044(7) -0.0021(6) O7W 0.0196(7) 0.0238(7) 0.0480(9) -0.0134(6) -0.0084(6) 0.0019(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 Gd1 O4 2.3331(11) . ? Gd1 O2 2.3535(11) . ? Gd1 O1 2.3853(10) . ? Gd1 O3 2.4070(10) . ? Gd1 O1W 2.4668(11) . ? Gd1 N3 2.6415(13) . ? Gd1 N4 2.6436(13) . ? Gd1 N2 2.6673(12) . ? Gd1 N1 2.6711(12) . ? O1 C10 1.2595(18) . ? O2 C12 1.2518(18) . ? O3 C14 1.2552(19) . ? O4 C16 1.2524(18) . ? N1 C9 1.4824(19) . ? N1 C8 1.4925(19) . ? N1 C1 1.4934(19) . ? N2 C11 1.4857(19) . ? N2 C2 1.4871(18) . ? N2 C3 1.4927(19) . ? N3 C13 1.4816(18) . ? N3 C4 1.4917(19) . ? N3 C5 1.4969(19) . ? N4 C15 1.4852(19) . ? N4 C6 1.4922(19) . ? N4 C7 1.4935(19) . ? N5 C10 1.3195(19) . ? N5 H5C 0.8600 . ? N5 H5D 0.8600 . ? N6 C12 1.320(2) . ? N6 H6C 0.8600 . ? N6 H6D 0.8600 . ? N7 C14 1.3175(19) . ? N7 H7C 0.8600 . ? N7 H7D 0.8600 . ? N8 C16 1.317(2) . ? N8 H8C 0.8600 . ? N8 H8D 0.8600 . ? C1 C2 1.522(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.520(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.525(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.523(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.507(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.511(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C13 C14 1.512(2) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C15 C16 1.518(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? O1W H1WA 0.836(13) . ? O1W H1WB 0.829(13) . ? O2W H2WA 0.845(13) . ? O2W H2WB 0.847(13) . ? O3W H3WA 0.848(13) . ? O3W H3WB 0.843(13) . ? O4W H4WA 0.841(14) . ? O4W H4WB 0.841(14) . ? O5W H5WA 0.853(13) . ? O5W H5WB 0.847(13) . ? O6W H6WA 0.852(14) . ? O6W H6WB 0.850(15) . ? O6W H6WC 0.840(15) . ? O7W H7WA 0.844(14) . ? O7W H7WB 0.852(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Gd1 O2 143.23(4) . . ? O4 Gd1 O1 82.87(4) . . ? O2 Gd1 O1 83.06(4) . . ? O4 Gd1 O3 86.34(4) . . ? O2 Gd1 O3 85.93(4) . . ? O1 Gd1 O3 144.81(4) . . ? O4 Gd1 O1W 71.99(4) . . ? O2 Gd1 O1W 71.39(4) . . ? O1 Gd1 O1W 72.26(4) . . ? O3 Gd1 O1W 72.55(4) . . ? O4 Gd1 N3 132.92(4) . . ? O2 Gd1 N3 74.97(4) . . ? O1 Gd1 N3 140.50(4) . . ? O3 Gd1 N3 66.36(4) . . ? O1W Gd1 N3 127.87(4) . . ? O4 Gd1 N4 66.70(4) . . ? O2 Gd1 N4 143.23(4) . . ? O1 Gd1 N4 130.49(4) . . ? O3 Gd1 N4 73.44(4) . . ? O1W Gd1 N4 127.23(4) . . ? N3 Gd1 N4 68.99(4) . . ? O4 Gd1 N2 139.38(4) . . ? O2 Gd1 N2 66.22(4) . . ? O1 Gd1 N2 73.10(4) . . ? O3 Gd1 N2 131.26(4) . . ? O1W Gd1 N2 127.42(4) . . ? N3 Gd1 N2 68.11(4) . . ? N4 Gd1 N2 105.34(4) . . ? O4 Gd1 N1 72.77(4) . . ? O2 Gd1 N1 129.88(4) . . ? O1 Gd1 N1 65.69(4) . . ? O3 Gd1 N1 141.19(4) . . ? O1W Gd1 N1 127.39(4) . . ? N3 Gd1 N1 104.73(4) . . ? N4 Gd1 N1 68.35(4) . . ? N2 Gd1 N1 67.64(4) . . ? C10 O1 Gd1 124.41(9) . . ? C12 O2 Gd1 124.91(10) . . ? C14 O3 Gd1 122.36(9) . . ? C16 O4 Gd1 124.23(10) . . ? C9 N1 C8 108.89(12) . . ? C9 N1 C1 109.54(11) . . ? C8 N1 C1 108.96(12) . . ? C9 N1 Gd1 106.99(8) . . ? C8 N1 Gd1 110.93(8) . . ? C1 N1 Gd1 111.48(9) . . ? C11 N2 C2 109.34(11) . . ? C11 N2 C3 109.41(12) . . ? C2 N2 C3 108.27(11) . . ? C11 N2 Gd1 107.24(8) . . ? C2 N2 Gd1 111.81(9) . . ? C3 N2 Gd1 110.75(8) . . ? C13 N3 C4 108.55(11) . . ? C13 N3 C5 110.29(11) . . ? C4 N3 C5 108.68(11) . . ? C13 N3 Gd1 106.14(9) . . ? C4 N3 Gd1 112.22(8) . . ? C5 N3 Gd1 110.92(9) . . ? C15 N4 C6 109.87(11) . . ? C15 N4 C7 110.02(12) . . ? C6 N4 C7 108.34(12) . . ? C15 N4 Gd1 106.23(9) . . ? C6 N4 Gd1 110.93(9) . . ? C7 N4 Gd1 111.45(8) . . ? C10 N5 H5C 120.0 . . ? C10 N5 H5D 120.0 . . ? H5C N5 H5D 120.0 . . ? C12 N6 H6C 120.0 . . ? C12 N6 H6D 120.0 . . ? H6C N6 H6D 120.0 . . ? C14 N7 H7C 120.0 . . ? C14 N7 H7D 120.0 . . ? H7C N7 H7D 120.0 . . ? C16 N8 H8C 120.0 . . ? C16 N8 H8D 120.0 . . ? H8C N8 H8D 120.0 . . ? N1 C1 C2 113.00(12) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N2 C2 C1 111.32(12) . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N2 C3 C4 113.30(12) . . ? N2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N3 C4 C3 111.30(12) . . ? N3 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N3 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N3 C5 C6 113.92(12) . . ? N3 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N3 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 C5 111.74(12) . . ? N4 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N4 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? N4 C7 C8 113.45(12) . . ? N4 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N4 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C7 111.54(12) . . ? N1 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N1 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N1 C9 C10 110.92(12) . . ? N1 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.0 . . ? O1 C10 N5 121.51(14) . . ? O1 C10 C9 119.39(13) . . ? N5 C10 C9 119.03(13) . . ? N2 C11 C12 109.74(11) . . ? N2 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O2 C12 N6 121.50(14) . . ? O2 C12 C11 119.38(13) . . ? N6 C12 C11 119.10(13) . . ? N3 C13 C14 110.24(12) . . ? N3 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N3 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? O3 C14 N7 123.19(14) . . ? O3 C14 C13 119.27(13) . . ? N7 C14 C13 117.51(14) . . ? N4 C15 C16 110.24(12) . . ? N4 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? N4 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? O4 C16 N8 121.91(14) . . ? O4 C16 C15 119.76(14) . . ? N8 C16 C15 118.30(13) . . ? Gd1 O1W H1WA 115.2(14) . . ? Gd1 O1W H1WB 123.3(14) . . ? H1WA O1W H1WB 108.2(16) . . ? H2WA O2W H2WB 103.8(18) . . ? H3WA O3W H3WB 104.7(17) . . ? H4WA O4W H4WB 105.9(19) . . ? H5WA O5W H5WB 103.3(18) . . ? H6WA O6W H6WB 105(2) . . ? H6WA O6W H6WC 104(2) . . ? H6WB O6W H6WC 83(5) . . ? H7WA O7W H7WB 105.8(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Gd1 O1 C10 61.34(11) . . . . ? O2 Gd1 O1 C10 -152.72(12) . . . . ? O3 Gd1 O1 C10 134.54(11) . . . . ? O1W Gd1 O1 C10 134.65(12) . . . . ? N3 Gd1 O1 C10 -96.66(12) . . . . ? N4 Gd1 O1 C10 10.45(13) . . . . ? N2 Gd1 O1 C10 -85.52(12) . . . . ? N1 Gd1 O1 C10 -12.93(11) . . . . ? O4 Gd1 O2 C12 136.39(11) . . . . ? O1 Gd1 O2 C12 68.20(12) . . . . ? O3 Gd1 O2 C12 -145.28(12) . . . . ? O1W Gd1 O2 C12 141.77(12) . . . . ? N3 Gd1 O2 C12 -78.67(12) . . . . ? N4 Gd1 O2 C12 -90.21(13) . . . . ? N2 Gd1 O2 C12 -6.34(11) . . . . ? N1 Gd1 O2 C12 18.15(14) . . . . ? O4 Gd1 O3 C14 -152.22(12) . . . . ? O2 Gd1 O3 C14 63.75(12) . . . . ? O1 Gd1 O3 C14 135.63(11) . . . . ? O1W Gd1 O3 C14 135.52(12) . . . . ? N3 Gd1 O3 C14 -11.61(11) . . . . ? N4 Gd1 O3 C14 -85.45(12) . . . . ? N2 Gd1 O3 C14 10.65(14) . . . . ? N1 Gd1 O3 C14 -95.80(12) . . . . ? O2 Gd1 O4 C16 137.08(11) . . . . ? O1 Gd1 O4 C16 -154.68(12) . . . . ? O3 Gd1 O4 C16 58.88(11) . . . . ? O1W Gd1 O4 C16 131.72(12) . . . . ? N3 Gd1 O4 C16 6.34(13) . . . . ? N4 Gd1 O4 C16 -14.66(11) . . . . ? N2 Gd1 O4 C16 -101.24(12) . . . . ? N1 Gd1 O4 C16 -87.98(11) . . . . ? O4 Gd1 N1 C9 -63.40(9) . . . . ? O2 Gd1 N1 C9 83.08(10) . . . . ? O1 Gd1 N1 C9 26.45(8) . . . . ? O3 Gd1 N1 C9 -123.92(9) . . . . ? O1W Gd1 N1 C9 -13.54(10) . . . . ? N3 Gd1 N1 C9 165.62(8) . . . . ? N4 Gd1 N1 C9 -134.60(9) . . . . ? N2 Gd1 N1 C9 107.30(9) . . . . ? O4 Gd1 N1 C8 55.23(9) . . . . ? O2 Gd1 N1 C8 -158.28(9) . . . . ? O1 Gd1 N1 C8 145.09(10) . . . . ? O3 Gd1 N1 C8 -5.28(13) . . . . ? O1W Gd1 N1 C8 105.10(10) . . . . ? N3 Gd1 N1 C8 -75.74(10) . . . . ? N4 Gd1 N1 C8 -15.96(9) . . . . ? N2 Gd1 N1 C8 -134.06(10) . . . . ? O4 Gd1 N1 C1 176.86(10) . . . . ? O2 Gd1 N1 C1 -36.65(11) . . . . ? O1 Gd1 N1 C1 -93.28(9) . . . . ? O3 Gd1 N1 C1 116.35(9) . . . . ? O1W Gd1 N1 C1 -133.27(9) . . . . ? N3 Gd1 N1 C1 45.89(10) . . . . ? N4 Gd1 N1 C1 105.67(10) . . . . ? N2 Gd1 N1 C1 -12.43(9) . . . . ? O4 Gd1 N2 C11 -122.65(9) . . . . ? O2 Gd1 N2 C11 23.52(8) . . . . ? O1 Gd1 N2 C11 -66.25(9) . . . . ? O3 Gd1 N2 C11 84.18(10) . . . . ? O1W Gd1 N2 C11 -15.56(11) . . . . ? N3 Gd1 N2 C11 106.14(9) . . . . ? N4 Gd1 N2 C11 165.41(9) . . . . ? N1 Gd1 N2 C11 -136.36(10) . . . . ? O4 Gd1 N2 C2 -2.81(12) . . . . ? O2 Gd1 N2 C2 143.36(10) . . . . ? O1 Gd1 N2 C2 53.60(9) . . . . ? O3 Gd1 N2 C2 -155.97(8) . . . . ? O1W Gd1 N2 C2 104.29(9) . . . . ? N3 Gd1 N2 C2 -134.01(10) . . . . ? N4 Gd1 N2 C2 -74.74(10) . . . . ? N1 Gd1 N2 C2 -16.51(9) . . . . ? O4 Gd1 N2 C3 118.03(9) . . . . ? O2 Gd1 N2 C3 -95.80(9) . . . . ? O1 Gd1 N2 C3 174.43(10) . . . . ? O3 Gd1 N2 C3 -35.14(11) . . . . ? O1W Gd1 N2 C3 -134.88(9) . . . . ? N3 Gd1 N2 C3 -13.18(9) . . . . ? N4 Gd1 N2 C3 46.10(10) . . . . ? N1 Gd1 N2 C3 104.32(10) . . . . ? O4 Gd1 N3 C13 88.10(10) . . . . ? O2 Gd1 N3 C13 -63.89(9) . . . . ? O1 Gd1 N3 C13 -122.40(9) . . . . ? O3 Gd1 N3 C13 28.24(8) . . . . ? O1W Gd1 N3 C13 -12.75(11) . . . . ? N4 Gd1 N3 C13 108.74(9) . . . . ? N2 Gd1 N3 C13 -133.89(10) . . . . ? N1 Gd1 N3 C13 168.10(9) . . . . ? O4 Gd1 N3 C4 -153.49(8) . . . . ? O2 Gd1 N3 C4 54.52(9) . . . . ? O1 Gd1 N3 C4 -3.98(12) . . . . ? O3 Gd1 N3 C4 146.66(10) . . . . ? O1W Gd1 N3 C4 105.67(9) . . . . ? N4 Gd1 N3 C4 -132.84(10) . . . . ? N2 Gd1 N3 C4 -15.47(9) . . . . ? N1 Gd1 N3 C4 -73.49(9) . . . . ? O4 Gd1 N3 C5 -31.71(11) . . . . ? O2 Gd1 N3 C5 176.30(9) . . . . ? O1 Gd1 N3 C5 117.79(9) . . . . ? O3 Gd1 N3 C5 -91.57(9) . . . . ? O1W Gd1 N3 C5 -132.56(9) . . . . ? N4 Gd1 N3 C5 -11.07(8) . . . . ? N2 Gd1 N3 C5 106.30(9) . . . . ? N1 Gd1 N3 C5 48.29(9) . . . . ? O4 Gd1 N4 C15 27.40(8) . . . . ? O2 Gd1 N4 C15 -124.34(9) . . . . ? O1 Gd1 N4 C15 84.36(10) . . . . ? O3 Gd1 N4 C15 -65.78(9) . . . . ? O1W Gd1 N4 C15 -14.01(11) . . . . ? N3 Gd1 N4 C15 -136.28(9) . . . . ? N2 Gd1 N4 C15 165.02(8) . . . . ? N1 Gd1 N4 C15 107.26(9) . . . . ? O4 Gd1 N4 C6 146.76(10) . . . . ? O2 Gd1 N4 C6 -4.97(12) . . . . ? O1 Gd1 N4 C6 -156.28(8) . . . . ? O3 Gd1 N4 C6 53.58(9) . . . . ? O1W Gd1 N4 C6 105.36(9) . . . . ? N3 Gd1 N4 C6 -16.91(9) . . . . ? N2 Gd1 N4 C6 -75.61(9) . . . . ? N1 Gd1 N4 C6 -133.38(10) . . . . ? O4 Gd1 N4 C7 -92.43(10) . . . . ? O2 Gd1 N4 C7 115.83(10) . . . . ? O1 Gd1 N4 C7 -35.47(11) . . . . ? O3 Gd1 N4 C7 174.39(10) . . . . ? O1W Gd1 N4 C7 -133.83(9) . . . . ? N3 Gd1 N4 C7 103.89(10) . . . . ? N2 Gd1 N4 C7 45.19(10) . . . . ? N1 Gd1 N4 C7 -12.57(9) . . . . ? C9 N1 C1 C2 -77.39(15) . . . . ? C8 N1 C1 C2 163.59(12) . . . . ? Gd1 N1 C1 C2 40.83(14) . . . . ? C11 N2 C2 C1 162.67(12) . . . . ? C3 N2 C2 C1 -78.21(15) . . . . ? Gd1 N2 C2 C1 44.06(14) . . . . ? N1 C1 C2 N2 -58.59(16) . . . . ? C11 N2 C3 C4 -76.58(15) . . . . ? C2 N2 C3 C4 164.34(12) . . . . ? Gd1 N2 C3 C4 41.42(14) . . . . ? C13 N3 C4 C3 159.81(12) . . . . ? C5 N3 C4 C3 -80.22(14) . . . . ? Gd1 N3 C4 C3 42.82(14) . . . . ? N2 C3 C4 N3 -58.21(16) . . . . ? C13 N3 C5 C6 -78.39(15) . . . . ? C4 N3 C5 C6 162.73(12) . . . . ? Gd1 N3 C5 C6 38.91(14) . . . . ? C15 N4 C6 C5 160.73(13) . . . . ? C7 N4 C6 C5 -79.06(15) . . . . ? Gd1 N4 C6 C5 43.57(14) . . . . ? N3 C5 C6 N4 -57.43(17) . . . . ? C15 N4 C7 C8 -76.68(15) . . . . ? C6 N4 C7 C8 163.20(12) . . . . ? Gd1 N4 C7 C8 40.88(15) . . . . ? C9 N1 C8 C7 160.59(12) . . . . ? C1 N1 C8 C7 -79.98(15) . . . . ? Gd1 N1 C8 C7 43.11(14) . . . . ? N4 C7 C8 N1 -58.33(17) . . . . ? C8 N1 C9 C10 -157.78(12) . . . . ? C1 N1 C9 C10 83.15(14) . . . . ? Gd1 N1 C9 C10 -37.83(13) . . . . ? Gd1 O1 C10 N5 178.79(11) . . . . ? Gd1 O1 C10 C9 -4.34(19) . . . . ? N1 C9 C10 O1 31.57(18) . . . . ? N1 C9 C10 N5 -151.49(13) . . . . ? C2 N2 C11 C12 -158.24(12) . . . . ? C3 N2 C11 C12 83.34(14) . . . . ? Gd1 N2 C11 C12 -36.83(13) . . . . ? Gd1 O2 C12 N6 168.22(11) . . . . ? Gd1 O2 C12 C11 -13.46(19) . . . . ? N2 C11 C12 O2 36.37(19) . . . . ? N2 C11 C12 N6 -145.26(14) . . . . ? C4 N3 C13 C14 -162.83(12) . . . . ? C5 N3 C13 C14 78.21(15) . . . . ? Gd1 N3 C13 C14 -42.01(13) . . . . ? Gd1 O3 C14 N7 173.25(11) . . . . ? Gd1 O3 C14 C13 -8.63(19) . . . . ? N3 C13 C14 O3 37.32(19) . . . . ? N3 C13 C14 N7 -144.46(14) . . . . ? C6 N4 C15 C16 -157.63(12) . . . . ? C7 N4 C15 C16 83.18(14) . . . . ? Gd1 N4 C15 C16 -37.58(13) . . . . ? Gd1 O4 C16 N8 179.83(11) . . . . ? Gd1 O4 C16 C15 -2.20(18) . . . . ? N4 C15 C16 O4 30.42(19) . . . . ? N4 C15 C16 N8 -151.54(13) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.481 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.073 #============================================================================== data_[Gd.1]Br3 _database_code_depnum_ccdc_archive 'CCDC 606216' #============================================================================== _chemical_name_systematic ; [Gd.DOTAM]Cl~3~.6H~2~O ; _chemical_name_common (Gd.DOTAM)Cl!3$.6H!2$O _chemical_melting_point 'not measured' _chemical_formula_moiety 'C16 H34 Gd N8 O5, 6(H2 O), 3Br' _chemical_formula_sum 'C16 H46 Br3 Gd N8 O11' _chemical_formula_weight 923.59 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1223(7) _cell_length_b 12.4165(9) _cell_length_c 13.5247(8) _cell_angle_alpha 75.699(3) _cell_angle_beta 76.447(3) _cell_angle_gamma 83.308(3) _cell_volume 1598.18(19) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5925 _cell_measurement_theta_min 2.329 _cell_measurement_theta_max 30.016 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 910 _exptl_absorpt_coefficient_mu 5.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.576339 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 15538 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 30.02 _reflns_number_total 8344 _reflns_number_gt 7369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+13.8844P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8344 _refine_ls_number_parameters 392 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.79441(3) 0.72914(2) 0.653387(19) 0.01143(7) Uani 1 1 d . . . O1 O 0.9464(4) 0.5870(3) 0.5902(3) 0.0154(7) Uani 1 1 d . . . O2 O 0.6340(4) 0.6451(3) 0.5997(3) 0.0148(7) Uani 1 1 d . . . O3 O 0.6653(4) 0.9014(3) 0.6022(3) 0.0168(8) Uani 1 1 d . . . O4 O 0.9889(4) 0.8317(3) 0.5914(3) 0.0151(7) Uani 1 1 d . . . N1 N 0.9718(5) 0.6362(4) 0.7734(4) 0.0159(9) Uani 1 1 d . . . N2 N 0.7155(5) 0.5351(4) 0.7819(4) 0.0153(9) Uani 1 1 d . . . N3 N 0.5631(5) 0.7533(4) 0.7874(4) 0.0150(9) Uani 1 1 d . . . N4 N 0.8202(5) 0.8562(4) 0.7774(4) 0.0169(9) Uani 1 1 d . . . N5 N 1.1312(5) 0.4670(4) 0.5862(4) 0.0194(10) Uani 1 1 d . . . H5C H 1.1122 0.4429 0.5371 0.023 Uiso 1 1 calc R . . H5D H 1.2023 0.4400 0.6106 0.023 Uiso 1 1 calc R . . N6 N 0.4856(5) 0.5159(4) 0.6195(4) 0.0194(10) Uani 1 1 d . . . H6C H 0.4439 0.5590 0.5746 0.023 Uiso 1 1 calc R . . H6D H 0.4584 0.4504 0.6498 0.023 Uiso 1 1 calc R . . N7 N 0.4732(5) 1.0154(4) 0.6247(4) 0.0208(10) Uani 1 1 d . . . H7C H 0.5113 1.0701 0.5783 0.025 Uiso 1 1 calc R . . H7D H 0.3899 1.0236 0.6567 0.025 Uiso 1 1 calc R . . N8 N 1.1194(5) 0.9695(4) 0.5870(4) 0.0208(10) Uani 1 1 d . . . H8C H 1.1809 0.9507 0.5374 0.025 Uiso 1 1 calc R . . H8D H 1.1301 1.0248 0.6115 0.025 Uiso 1 1 calc R . . C1 C 0.9130(6) 0.5420(5) 0.8597(4) 0.0194(11) Uani 1 1 d . . . H1A H 0.8547 0.5722 0.9156 0.023 Uiso 1 1 calc R . . H1B H 0.9865 0.4965 0.8874 0.023 Uiso 1 1 calc R . . C2 C 0.8311(6) 0.4689(5) 0.8245(4) 0.0183(11) Uani 1 1 d . . . H2A H 0.8901 0.4352 0.7712 0.022 Uiso 1 1 calc R . . H2B H 0.7958 0.4096 0.8832 0.022 Uiso 1 1 calc R . . C3 C 0.6044(6) 0.5542(5) 0.8713(4) 0.0170(10) Uani 1 1 d . . . H3A H 0.6441 0.5737 0.9226 0.020 Uiso 1 1 calc R . . H3B H 0.5597 0.4853 0.9041 0.020 Uiso 1 1 calc R . . C4 C 0.4982(6) 0.6453(4) 0.8399(4) 0.0166(10) Uani 1 1 d . . . H4A H 0.4528 0.6238 0.7927 0.020 Uiso 1 1 calc R . . H4B H 0.4303 0.6548 0.9014 0.020 Uiso 1 1 calc R . . C5 C 0.5836(6) 0.8065(5) 0.8702(4) 0.0187(11) Uani 1 1 d . . . H5A H 0.6158 0.7495 0.9241 0.022 Uiso 1 1 calc R . . H5B H 0.4965 0.8381 0.9021 0.022 Uiso 1 1 calc R . . C6 C 0.6846(6) 0.8979(5) 0.8295(5) 0.0188(11) Uani 1 1 d . . . H6A H 0.6488 0.9583 0.7803 0.023 Uiso 1 1 calc R . . H6B H 0.6947 0.9271 0.8873 0.023 Uiso 1 1 calc R . . C7 C 0.8949(6) 0.7956(5) 0.8599(5) 0.0223(12) Uani 1 1 d . . . H7A H 0.8321 0.7511 0.9165 0.027 Uiso 1 1 calc R . . H7B H 0.9281 0.8496 0.8878 0.027 Uiso 1 1 calc R . . C8 C 1.0144(6) 0.7202(5) 0.8201(5) 0.0198(11) Uani 1 1 d . . . H8A H 1.0814 0.7653 0.7679 0.024 Uiso 1 1 calc R . . H8B H 1.0570 0.6819 0.8775 0.024 Uiso 1 1 calc R . . C9 C 1.0922(6) 0.5931(5) 0.7044(4) 0.0166(10) Uani 1 1 d . . . H9A H 1.1423 0.5357 0.7465 0.020 Uiso 1 1 calc R . . H9B H 1.1519 0.6530 0.6690 0.020 Uiso 1 1 calc R . . C10 C 1.0513(6) 0.5455(4) 0.6242(4) 0.0151(10) Uani 1 1 d . . . C11 C 0.6653(6) 0.4718(5) 0.7192(4) 0.0179(11) Uani 1 1 d . . . H11A H 0.6041 0.4172 0.7653 0.022 Uiso 1 1 calc R . . H11B H 0.7416 0.4325 0.6818 0.022 Uiso 1 1 calc R . . C12 C 0.5913(5) 0.5505(4) 0.6420(4) 0.0142(10) Uani 1 1 d . . . C13 C 0.4691(5) 0.8251(5) 0.7259(4) 0.0160(10) Uani 1 1 d . . . H13A H 0.3944 0.8556 0.7726 0.019 Uiso 1 1 calc R . . H13B H 0.4314 0.7808 0.6906 0.019 Uiso 1 1 calc R . . C14 C 0.5426(6) 0.9188(4) 0.6465(4) 0.0158(10) Uani 1 1 d . . . C15 C 0.8980(6) 0.9521(5) 0.7093(5) 0.0177(11) Uani 1 1 d . . . H15A H 0.9397 0.9856 0.7512 0.021 Uiso 1 1 calc R . . H15B H 0.8366 1.0081 0.6767 0.021 Uiso 1 1 calc R . . C16 C 1.0074(6) 0.9130(5) 0.6258(4) 0.0168(10) Uani 1 1 d . . . Br1 Br 0.69730(7) 0.60713(6) 0.11948(5) 0.02790(15) Uani 1 1 d . . . Br2 Br 0.34260(6) 0.75828(5) 0.49029(5) 0.02285(13) Uani 1 1 d . . . Br3 Br 0.81061(9) 0.96134(7) 0.18762(8) 0.02508(18) Uani 0.75 1 d P A 1 Br3A Br 1.1819(4) 0.8330(4) -0.0314(3) 0.0328(7) Uani 0.25 1 d P B 2 O1W O 0.8372(4) 0.7800(3) 0.4614(3) 0.0158(7) Uani 1 1 d D . . H1WA H 0.914(3) 0.756(6) 0.438(5) 0.024 Uiso 1 1 d D . . H1WB H 0.788(5) 0.758(6) 0.431(5) 0.024 Uiso 1 1 d D . . O2W O 1.0962(5) 0.7380(5) 0.3682(4) 0.0313(11) Uani 1 1 d D . . H2WA H 1.134(8) 0.781(6) 0.316(4) 0.047 Uiso 1 1 d D . . H2WB H 1.134(8) 0.744(7) 0.414(4) 0.047 Uiso 1 1 d D . . O3W O 0.6542(5) 0.7052(4) 0.3624(3) 0.0223(9) Uani 1 1 d D . . H3WA H 0.581(4) 0.721(6) 0.400(4) 0.034 Uiso 1 1 d D . . H3WB H 0.649(7) 0.737(6) 0.303(2) 0.034 Uiso 1 1 d D . . O4W O 1.2636(6) 0.8261(5) 0.1803(4) 0.0420(13) Uani 1 1 d D . . H4WA H 1.252(9) 0.819(9) 0.124(4) 0.063 Uiso 1 1 d D . . H4WB H 1.347(2) 0.822(9) 0.170(7) 0.063 Uiso 1 1 d D . . O5W O 1.2158(11) 0.7950(8) -0.0080(8) 0.048(3) Uani 0.75 1 d P C 1 O5WA O 0.804(2) 0.9526(18) 0.2342(19) 0.028(5) Uiso 0.25 1 d P D 2 O6WA O 0.5472(14) 0.8236(11) 0.1778(11) 0.043(3) Uiso 0.45 1 d P E 1 O6W O 0.5476(11) 0.8696(9) 0.1203(8) 0.040(2) Uiso 0.55 1 d P F 2 O7W O 0.597(2) 0.987(2) 0.0419(18) 0.044(5) Uiso 0.25 1 d P G 1 O7WA O 0.9649(7) 0.7353(6) 0.1200(7) 0.0418(18) Uani 0.75 1 d P H 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.00944(12) 0.01175(12) 0.01250(11) 0.00097(8) -0.00333(8) -0.00431(8) O1 0.0117(18) 0.0165(18) 0.0176(18) -0.0012(15) -0.0047(14) -0.0015(14) O2 0.0156(19) 0.0135(17) 0.0145(17) 0.0026(14) -0.0049(14) -0.0070(14) O3 0.0113(18) 0.0156(18) 0.0202(19) 0.0002(15) 0.0001(14) -0.0039(14) O4 0.0143(18) 0.0150(18) 0.0158(17) -0.0022(14) -0.0016(14) -0.0057(14) N1 0.017(2) 0.017(2) 0.014(2) -0.0010(17) -0.0060(17) -0.0047(17) N2 0.012(2) 0.014(2) 0.017(2) 0.0038(17) -0.0045(17) -0.0026(16) N3 0.014(2) 0.015(2) 0.015(2) 0.0033(17) -0.0049(17) -0.0071(17) N4 0.012(2) 0.018(2) 0.020(2) 0.0002(18) -0.0053(17) -0.0041(17) N5 0.016(2) 0.020(2) 0.025(2) -0.0057(19) -0.0101(19) 0.0001(18) N6 0.018(2) 0.015(2) 0.026(2) -0.0001(19) -0.0084(19) -0.0085(18) N7 0.015(2) 0.013(2) 0.027(2) 0.0051(19) -0.0008(19) -0.0024(18) N8 0.013(2) 0.019(2) 0.031(3) -0.008(2) -0.0013(19) -0.0090(18) C1 0.018(3) 0.021(3) 0.018(3) 0.005(2) -0.008(2) -0.005(2) C2 0.016(3) 0.019(3) 0.017(2) 0.007(2) -0.006(2) -0.007(2) C3 0.015(3) 0.017(3) 0.016(2) 0.005(2) -0.004(2) -0.005(2) C4 0.014(2) 0.016(2) 0.017(2) 0.005(2) -0.003(2) -0.008(2) C5 0.015(3) 0.022(3) 0.018(2) -0.001(2) -0.003(2) -0.007(2) C6 0.017(3) 0.018(3) 0.022(3) -0.002(2) -0.006(2) -0.006(2) C7 0.021(3) 0.027(3) 0.021(3) -0.004(2) -0.009(2) -0.004(2) C8 0.020(3) 0.020(3) 0.021(3) -0.002(2) -0.010(2) -0.003(2) C9 0.013(2) 0.018(3) 0.019(2) 0.000(2) -0.006(2) -0.0039(19) C10 0.013(2) 0.012(2) 0.020(2) 0.0007(19) -0.007(2) -0.0014(18) C11 0.016(3) 0.016(2) 0.021(3) 0.001(2) -0.005(2) -0.005(2) C12 0.013(2) 0.013(2) 0.017(2) -0.0027(19) -0.0040(19) -0.0008(18) C13 0.010(2) 0.017(2) 0.018(2) 0.000(2) -0.0018(19) -0.0017(19) C14 0.017(3) 0.015(2) 0.016(2) -0.001(2) -0.005(2) -0.004(2) C15 0.016(3) 0.014(2) 0.025(3) -0.005(2) -0.005(2) -0.007(2) C16 0.017(3) 0.015(2) 0.019(2) -0.001(2) -0.006(2) -0.007(2) Br1 0.0234(3) 0.0360(3) 0.0226(3) 0.0065(2) -0.0090(2) -0.0148(3) Br2 0.0153(3) 0.0193(3) 0.0310(3) 0.0012(2) -0.0055(2) -0.0030(2) Br3 0.0242(4) 0.0252(4) 0.0271(5) -0.0076(4) -0.0066(4) -0.0007(3) Br3A 0.0236(16) 0.053(2) 0.0215(15) -0.0037(15) -0.0035(11) -0.0134(15) O1W 0.0164(19) 0.0153(18) 0.0157(18) -0.0010(14) -0.0047(15) -0.0045(15) O2W 0.019(2) 0.045(3) 0.031(2) -0.007(2) -0.0059(19) -0.009(2) O3W 0.022(2) 0.026(2) 0.0174(19) 0.0008(17) -0.0059(16) -0.0028(17) O4W 0.034(3) 0.051(3) 0.041(3) -0.002(3) -0.010(2) -0.019(3) O5W 0.045(6) 0.043(6) 0.051(6) 0.015(4) -0.024(4) -0.007(4) O7WA 0.028(4) 0.024(3) 0.075(5) 0.002(3) -0.025(4) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O4 2.342(4) . ? Gd1 O2 2.361(4) . ? Gd1 O1 2.389(4) . ? Gd1 O3 2.409(4) . ? Gd1 O1W 2.461(4) . ? Gd1 N3 2.641(5) . ? Gd1 N4 2.642(5) . ? Gd1 N1 2.674(5) . ? Gd1 N2 2.682(4) . ? O1 C10 1.260(6) . ? O2 C12 1.251(6) . ? O3 C14 1.265(7) . ? O4 C16 1.259(6) . ? N1 C9 1.484(7) . ? N1 C8 1.494(7) . ? N1 C1 1.498(7) . ? N2 C11 1.490(7) . ? N2 C3 1.491(7) . ? N2 C2 1.495(7) . ? N3 C13 1.482(7) . ? N3 C5 1.497(7) . ? N3 C4 1.500(7) . ? N4 C6 1.487(8) . ? N4 C15 1.492(7) . ? N4 C7 1.493(7) . ? N5 C10 1.317(7) . ? N5 H5C 0.8600 . ? N5 H5D 0.8600 . ? N6 C12 1.321(7) . ? N6 H6C 0.8600 . ? N6 H6D 0.8600 . ? N7 C14 1.321(7) . ? N7 H7C 0.8600 . ? N7 H7D 0.8600 . ? N8 C16 1.334(7) . ? N8 H8C 0.8600 . ? N8 H8D 0.8600 . ? C1 C2 1.520(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.519(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.528(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.519(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.511(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.515(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C13 C14 1.506(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C15 C16 1.516(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? O1W H1WA 0.82(2) . ? O1W H1WB 0.816(19) . ? O2W H2WA 0.82(2) . ? O2W H2WB 0.82(2) . ? O3W H3WA 0.83(2) . ? O3W H3WB 0.82(2) . ? O4W H4WA 0.83(2) . ? O4W H4WB 0.82(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Gd1 O2 143.19(13) . . ? O4 Gd1 O1 82.61(13) . . ? O2 Gd1 O1 82.77(13) . . ? O4 Gd1 O3 86.91(13) . . ? O2 Gd1 O3 85.67(13) . . ? O1 Gd1 O3 144.40(13) . . ? O4 Gd1 O1W 71.68(13) . . ? O2 Gd1 O1W 71.74(13) . . ? O1 Gd1 O1W 72.48(13) . . ? O3 Gd1 O1W 71.92(13) . . ? O4 Gd1 N3 133.03(14) . . ? O2 Gd1 N3 75.23(14) . . ? O1 Gd1 N3 140.62(13) . . ? O3 Gd1 N3 66.37(13) . . ? O1W Gd1 N3 127.87(14) . . ? O4 Gd1 N4 66.75(14) . . ? O2 Gd1 N4 143.52(14) . . ? O1 Gd1 N4 130.49(14) . . ? O3 Gd1 N4 73.98(14) . . ? O1W Gd1 N4 126.71(13) . . ? N3 Gd1 N4 68.97(14) . . ? O4 Gd1 N1 72.80(14) . . ? O2 Gd1 N1 129.60(13) . . ? O1 Gd1 N1 65.99(14) . . ? O3 Gd1 N1 141.64(14) . . ? O1W Gd1 N1 127.73(14) . . ? N3 Gd1 N1 104.40(14) . . ? N4 Gd1 N1 68.19(14) . . ? O4 Gd1 N2 139.35(14) . . ? O2 Gd1 N2 66.14(13) . . ? O1 Gd1 N2 73.61(14) . . ? O3 Gd1 N2 130.74(14) . . ? O1W Gd1 N2 128.22(13) . . ? N3 Gd1 N2 67.73(14) . . ? N4 Gd1 N2 105.06(14) . . ? N1 Gd1 N2 67.56(14) . . ? C10 O1 Gd1 124.4(3) . . ? C12 O2 Gd1 125.3(3) . . ? C14 O3 Gd1 122.2(3) . . ? C16 O4 Gd1 123.8(4) . . ? C9 N1 C8 109.5(4) . . ? C9 N1 C1 109.4(4) . . ? C8 N1 C1 108.9(4) . . ? C9 N1 Gd1 106.6(3) . . ? C8 N1 Gd1 110.8(3) . . ? C1 N1 Gd1 111.6(3) . . ? C11 N2 C3 109.9(4) . . ? C11 N2 C2 109.3(4) . . ? C3 N2 C2 108.5(4) . . ? C11 N2 Gd1 106.9(3) . . ? C3 N2 Gd1 110.8(3) . . ? C2 N2 Gd1 111.5(3) . . ? C13 N3 C5 110.3(4) . . ? C13 N3 C4 107.8(4) . . ? C5 N3 C4 108.2(4) . . ? C13 N3 Gd1 106.4(3) . . ? C5 N3 Gd1 111.1(3) . . ? C4 N3 Gd1 113.0(3) . . ? C6 N4 C15 109.5(4) . . ? C6 N4 C7 108.3(4) . . ? C15 N4 C7 109.7(4) . . ? C6 N4 Gd1 110.8(3) . . ? C15 N4 Gd1 106.3(3) . . ? C7 N4 Gd1 112.1(3) . . ? C10 N5 H5C 120.0 . . ? C10 N5 H5D 120.0 . . ? H5C N5 H5D 120.0 . . ? C12 N6 H6C 120.0 . . ? C12 N6 H6D 120.0 . . ? H6C N6 H6D 120.0 . . ? C14 N7 H7C 120.0 . . ? C14 N7 H7D 120.0 . . ? H7C N7 H7D 120.0 . . ? C16 N8 H8C 120.0 . . ? C16 N8 H8D 120.0 . . ? H8C N8 H8D 120.0 . . ? N1 C1 C2 113.0(4) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N2 C2 C1 111.1(5) . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N2 C3 C4 113.6(4) . . ? N2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N3 C4 C3 110.7(4) . . ? N3 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 113.6(5) . . ? N3 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N3 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 C5 112.0(5) . . ? N4 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? N4 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N4 C7 C8 113.2(5) . . ? N4 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N4 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C7 112.2(5) . . ? N1 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N1 C9 C10 111.6(4) . . ? N1 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N1 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? O1 C10 N5 121.6(5) . . ? O1 C10 C9 119.1(5) . . ? N5 C10 C9 119.2(5) . . ? N2 C11 C12 110.2(4) . . ? N2 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? N2 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? O2 C12 N6 122.0(5) . . ? O2 C12 C11 119.1(5) . . ? N6 C12 C11 118.9(5) . . ? N3 C13 C14 110.7(4) . . ? N3 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O3 C14 N7 123.0(5) . . ? O3 C14 C13 119.4(5) . . ? N7 C14 C13 117.6(5) . . ? N4 C15 C16 110.0(4) . . ? N4 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? N4 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? O4 C16 N8 121.4(5) . . ? O4 C16 C15 120.0(5) . . ? N8 C16 C15 118.5(5) . . ? Gd1 O1W H1WA 109(5) . . ? Gd1 O1W H1WB 119(5) . . ? H1WA O1W H1WB 104(4) . . ? H2WA O2W H2WB 105(5) . . ? H3WA O3W H3WB 106(4) . . ? H4WA O4W H4WB 102(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Gd1 O1 C10 62.1(4) . . . . ? O2 Gd1 O1 C10 -151.8(4) . . . . ? O3 Gd1 O1 C10 136.1(4) . . . . ? O1W Gd1 O1 C10 135.1(4) . . . . ? N3 Gd1 O1 C10 -95.8(4) . . . . ? N4 Gd1 O1 C10 11.4(5) . . . . ? N1 Gd1 O1 C10 -12.3(4) . . . . ? N2 Gd1 O1 C10 -84.6(4) . . . . ? O4 Gd1 O2 C12 136.2(4) . . . . ? O1 Gd1 O2 C12 68.9(4) . . . . ? O3 Gd1 O2 C12 -144.9(4) . . . . ? O1W Gd1 O2 C12 142.7(5) . . . . ? N3 Gd1 O2 C12 -78.2(4) . . . . ? N4 Gd1 O2 C12 -89.5(5) . . . . ? N1 Gd1 O2 C12 18.4(5) . . . . ? N2 Gd1 O2 C12 -6.4(4) . . . . ? O4 Gd1 O3 C14 -152.9(4) . . . . ? O2 Gd1 O3 C14 63.2(4) . . . . ? O1 Gd1 O3 C14 134.4(4) . . . . ? O1W Gd1 O3 C14 135.4(4) . . . . ? N3 Gd1 O3 C14 -12.5(4) . . . . ? N4 Gd1 O3 C14 -86.2(4) . . . . ? N1 Gd1 O3 C14 -95.9(4) . . . . ? N2 Gd1 O3 C14 10.1(5) . . . . ? O2 Gd1 O4 C16 137.6(4) . . . . ? O1 Gd1 O4 C16 -155.0(4) . . . . ? O3 Gd1 O4 C16 59.1(4) . . . . ? O1W Gd1 O4 C16 131.1(4) . . . . ? N3 Gd1 O4 C16 5.9(5) . . . . ? N4 Gd1 O4 C16 -14.8(4) . . . . ? N1 Gd1 O4 C16 -87.9(4) . . . . ? N2 Gd1 O4 C16 -101.0(4) . . . . ? O4 Gd1 N1 C9 -63.7(3) . . . . ? O2 Gd1 N1 C9 82.6(3) . . . . ? O1 Gd1 N1 C9 25.8(3) . . . . ? O3 Gd1 N1 C9 -124.9(3) . . . . ? O1W Gd1 N1 C9 -14.7(4) . . . . ? N3 Gd1 N1 C9 165.2(3) . . . . ? N4 Gd1 N1 C9 -135.0(3) . . . . ? N2 Gd1 N1 C9 107.1(3) . . . . ? O4 Gd1 N1 C8 55.4(3) . . . . ? O2 Gd1 N1 C8 -158.3(3) . . . . ? O1 Gd1 N1 C8 144.9(4) . . . . ? O3 Gd1 N1 C8 -5.8(5) . . . . ? O1W Gd1 N1 C8 104.4(4) . . . . ? N3 Gd1 N1 C8 -75.7(4) . . . . ? N4 Gd1 N1 C8 -15.9(3) . . . . ? N2 Gd1 N1 C8 -133.8(4) . . . . ? O4 Gd1 N1 C1 176.9(4) . . . . ? O2 Gd1 N1 C1 -36.8(4) . . . . ? O1 Gd1 N1 C1 -93.6(4) . . . . ? O3 Gd1 N1 C1 115.7(4) . . . . ? O1W Gd1 N1 C1 -134.1(3) . . . . ? N3 Gd1 N1 C1 45.8(4) . . . . ? N4 Gd1 N1 C1 105.6(4) . . . . ? N2 Gd1 N1 C1 -12.3(3) . . . . ? O4 Gd1 N2 C11 -122.7(3) . . . . ? O2 Gd1 N2 C11 23.3(3) . . . . ? O1 Gd1 N2 C11 -65.9(3) . . . . ? O3 Gd1 N2 C11 84.0(4) . . . . ? O1W Gd1 N2 C11 -15.0(4) . . . . ? N3 Gd1 N2 C11 106.4(3) . . . . ? N4 Gd1 N2 C11 165.6(3) . . . . ? N1 Gd1 N2 C11 -136.2(4) . . . . ? O4 Gd1 N2 C3 117.7(3) . . . . ? O2 Gd1 N2 C3 -96.4(3) . . . . ? O1 Gd1 N2 C3 174.4(3) . . . . ? O3 Gd1 N2 C3 -35.7(4) . . . . ? O1W Gd1 N2 C3 -134.7(3) . . . . ? N3 Gd1 N2 C3 -13.3(3) . . . . ? N4 Gd1 N2 C3 46.0(3) . . . . ? N1 Gd1 N2 C3 104.1(3) . . . . ? O4 Gd1 N2 C2 -3.3(5) . . . . ? O2 Gd1 N2 C2 142.7(4) . . . . ? O1 Gd1 N2 C2 53.5(3) . . . . ? O3 Gd1 N2 C2 -156.6(3) . . . . ? O1W Gd1 N2 C2 104.3(4) . . . . ? N3 Gd1 N2 C2 -134.2(4) . . . . ? N4 Gd1 N2 C2 -75.0(4) . . . . ? N1 Gd1 N2 C2 -16.8(3) . . . . ? O4 Gd1 N3 C13 88.9(3) . . . . ? O2 Gd1 N3 C13 -63.5(3) . . . . ? O1 Gd1 N3 C13 -121.8(3) . . . . ? O3 Gd1 N3 C13 28.2(3) . . . . ? O1W Gd1 N3 C13 -11.5(4) . . . . ? N4 Gd1 N3 C13 109.3(3) . . . . ? N1 Gd1 N3 C13 168.7(3) . . . . ? N2 Gd1 N3 C13 -133.4(3) . . . . ? O4 Gd1 N3 C5 -31.2(4) . . . . ? O2 Gd1 N3 C5 176.4(4) . . . . ? O1 Gd1 N3 C5 118.1(3) . . . . ? O3 Gd1 N3 C5 -91.9(3) . . . . ? O1W Gd1 N3 C5 -131.6(3) . . . . ? N4 Gd1 N3 C5 -10.8(3) . . . . ? N1 Gd1 N3 C5 48.6(4) . . . . ? N2 Gd1 N3 C5 106.5(4) . . . . ? O4 Gd1 N3 C4 -153.0(3) . . . . ? O2 Gd1 N3 C4 54.5(3) . . . . ? O1 Gd1 N3 C4 -3.7(4) . . . . ? O3 Gd1 N3 C4 146.2(4) . . . . ? O1W Gd1 N3 C4 106.5(3) . . . . ? N4 Gd1 N3 C4 -132.6(4) . . . . ? N1 Gd1 N3 C4 -73.3(3) . . . . ? N2 Gd1 N3 C4 -15.4(3) . . . . ? O4 Gd1 N4 C6 146.7(4) . . . . ? O2 Gd1 N4 C6 -5.6(5) . . . . ? O1 Gd1 N4 C6 -156.8(3) . . . . ? O3 Gd1 N4 C6 53.1(3) . . . . ? O1W Gd1 N4 C6 105.0(3) . . . . ? N3 Gd1 N4 C6 -17.2(3) . . . . ? N1 Gd1 N4 C6 -133.4(4) . . . . ? N2 Gd1 N4 C6 -75.7(4) . . . . ? O4 Gd1 N4 C15 27.7(3) . . . . ? O2 Gd1 N4 C15 -124.5(3) . . . . ? O1 Gd1 N4 C15 84.3(4) . . . . ? O3 Gd1 N4 C15 -65.9(3) . . . . ? O1W Gd1 N4 C15 -13.9(4) . . . . ? N3 Gd1 N4 C15 -136.2(4) . . . . ? N1 Gd1 N4 C15 107.6(3) . . . . ? N2 Gd1 N4 C15 165.4(3) . . . . ? O4 Gd1 N4 C7 -92.1(4) . . . . ? O2 Gd1 N4 C7 115.7(4) . . . . ? O1 Gd1 N4 C7 -35.6(4) . . . . ? O3 Gd1 N4 C7 174.3(4) . . . . ? O1W Gd1 N4 C7 -133.8(3) . . . . ? N3 Gd1 N4 C7 104.0(4) . . . . ? N1 Gd1 N4 C7 -12.2(3) . . . . ? N2 Gd1 N4 C7 45.6(4) . . . . ? C9 N1 C1 C2 -76.6(6) . . . . ? C8 N1 C1 C2 163.8(5) . . . . ? Gd1 N1 C1 C2 41.1(6) . . . . ? C11 N2 C2 C1 162.5(5) . . . . ? C3 N2 C2 C1 -77.7(5) . . . . ? Gd1 N2 C2 C1 44.6(5) . . . . ? N1 C1 C2 N2 -59.2(6) . . . . ? C11 N2 C3 C4 -76.2(5) . . . . ? C2 N2 C3 C4 164.3(4) . . . . ? Gd1 N2 C3 C4 41.7(5) . . . . ? C13 N3 C4 C3 159.7(5) . . . . ? C5 N3 C4 C3 -81.0(6) . . . . ? Gd1 N3 C4 C3 42.5(5) . . . . ? N2 C3 C4 N3 -57.8(6) . . . . ? C13 N3 C5 C6 -79.3(6) . . . . ? C4 N3 C5 C6 163.0(5) . . . . ? Gd1 N3 C5 C6 38.4(5) . . . . ? C15 N4 C6 C5 161.0(4) . . . . ? C7 N4 C6 C5 -79.5(5) . . . . ? Gd1 N4 C6 C5 44.0(5) . . . . ? N3 C5 C6 N4 -57.4(6) . . . . ? C6 N4 C7 C8 162.6(5) . . . . ? C15 N4 C7 C8 -77.9(6) . . . . ? Gd1 N4 C7 C8 39.9(6) . . . . ? C9 N1 C8 C7 160.2(5) . . . . ? C1 N1 C8 C7 -80.2(6) . . . . ? Gd1 N1 C8 C7 42.9(5) . . . . ? N4 C7 C8 N1 -57.3(6) . . . . ? C8 N1 C9 C10 -157.3(4) . . . . ? C1 N1 C9 C10 83.4(5) . . . . ? Gd1 N1 C9 C10 -37.4(5) . . . . ? Gd1 O1 C10 N5 179.9(4) . . . . ? Gd1 O1 C10 C9 -4.8(7) . . . . ? N1 C9 C10 O1 31.6(7) . . . . ? N1 C9 C10 N5 -153.0(5) . . . . ? C3 N2 C11 C12 83.6(5) . . . . ? C2 N2 C11 C12 -157.5(4) . . . . ? Gd1 N2 C11 C12 -36.7(5) . . . . ? Gd1 O2 C12 N6 168.5(4) . . . . ? Gd1 O2 C12 C11 -13.2(7) . . . . ? N2 C11 C12 O2 36.2(7) . . . . ? N2 C11 C12 N6 -145.4(5) . . . . ? C5 N3 C13 C14 79.2(5) . . . . ? C4 N3 C13 C14 -162.8(4) . . . . ? Gd1 N3 C13 C14 -41.4(5) . . . . ? Gd1 O3 C14 N7 175.0(4) . . . . ? Gd1 O3 C14 C13 -6.8(6) . . . . ? N3 C13 C14 O3 35.6(7) . . . . ? N3 C13 C14 N7 -146.1(5) . . . . ? C6 N4 C15 C16 -157.8(4) . . . . ? C7 N4 C15 C16 83.4(5) . . . . ? Gd1 N4 C15 C16 -38.0(5) . . . . ? Gd1 O4 C16 N8 -179.2(4) . . . . ? Gd1 O4 C16 C15 -2.3(7) . . . . ? N4 C15 C16 O4 30.7(7) . . . . ? N4 C15 C16 N8 -152.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 2.848 _refine_diff_density_min -2.545 _refine_diff_density_rms 0.189 #============================================================================== data_[Gd.2]Cl3 _database_code_depnum_ccdc_archive 'CCDC 606217' #============================================================================== _chemical_name_systematic ; [Gd.DOTAPh]Cl~3~.8H~2~O ; _chemical_name_common '[Gd.2]Cl3' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C48 H66 Gd N8 O5, 8(H2 O), 3Cl' _chemical_formula_sum 'C48 H82 Cl3 Gd N8 O13' _chemical_formula_weight 1242.82 _chemical_absolute_configuration syn 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.2850(10) _cell_length_b 12.2650(8) _cell_length_c 15.5372(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.1380(10) _cell_angle_gamma 90.00 _cell_volume 2912.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7522 _cell_measurement_theta_min 2.129 _cell_measurement_theta_max 29.139 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1290 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5673 _exptl_absorpt_correction_T_max 0.6696 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.2000 -1.00 0.00 0.00 0.2000 0.00 1.00 0.00 0.1800 0.00 -1.00 0.00 0.2200 0.00 0.00 1.00 0.2000 0.00 0.00 -1.00 0.2500 1.00 0.00 1.00 0.1500 -1.00 0.00 -1.00 0.2500 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 33785 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 29.14 _reflns_number_total 15247 _reflns_number_gt 14912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+2.4599P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(5) _refine_ls_number_reflns 15247 _refine_ls_number_parameters 719 _refine_ls_number_restraints 190 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd -0.247399(6) -1.262418(11) -0.237467(6) 0.01089(3) Uani 1 1 d . . . N1 N -0.14298(15) -1.40862(18) -0.30852(15) 0.0133(4) Uani 1 1 d . . . N2 N -0.20088(15) -1.42014(18) -0.12616(15) 0.0133(4) Uani 1 1 d . . . N3 N -0.38431(15) -1.38270(18) -0.18659(15) 0.0128(4) Uani 1 1 d . . . N4 N -0.32755(15) -1.37151(18) -0.36775(15) 0.0135(4) Uani 1 1 d . . . N5 N -0.09194(17) -1.2245(2) -0.48028(17) 0.0174(5) Uani 1 1 d . . . H5C H -0.0559 -1.2694 -0.5061 0.021 Uiso 1 1 calc R . . N6 N -0.00235(14) -1.2740(3) -0.07210(14) 0.0154(4) Uani 1 1 d . . . H6C H 0.0135 -1.3108 -0.0258 0.019 Uiso 1 1 calc R . . N7 N -0.39489(16) -1.2215(2) 0.00815(16) 0.0162(5) Uani 1 1 d . . . H7C H -0.4461 -1.2434 0.0263 0.019 Uiso 1 1 calc R . . N8 N -0.48704(17) -1.1548(2) -0.38736(16) 0.0181(5) Uani 1 1 d . . . H8C H -0.5144 -1.1780 -0.4342 0.022 Uiso 1 1 calc R . . O1 O -0.17853(14) -1.19813(16) -0.36536(14) 0.0167(4) Uani 1 1 d . . . O2 O -0.10791(13) -1.23742(14) -0.17176(13) 0.0147(4) Uani 1 1 d . . . O3 O -0.29842(13) -1.21682(16) -0.09999(13) 0.0153(4) Uani 1 1 d . . . O4 O -0.37440(13) -1.17676(16) -0.29312(13) 0.0155(4) Uani 1 1 d . . . C1 C -0.09445(18) -1.4727(2) -0.24158(19) 0.0147(5) Uani 1 1 d . . . H1A H -0.0471 -1.4272 -0.2161 0.018 Uiso 1 1 calc R . . H1B H -0.0672 -1.5371 -0.2686 0.018 Uiso 1 1 calc R . . C2 C -0.15485(19) -1.5101(2) -0.17104(19) 0.0164(5) Uani 1 1 d . . . H2A H -0.1992 -1.5601 -0.1965 0.020 Uiso 1 1 calc R . . H2B H -0.1201 -1.5520 -0.1279 0.020 Uiso 1 1 calc R . . C3 C -0.27734(18) -1.4665(2) -0.08125(18) 0.0145(5) Uani 1 1 d . . . H3A H -0.2949 -1.4163 -0.0348 0.017 Uiso 1 1 calc R . . H3B H -0.2604 -1.5369 -0.0544 0.017 Uiso 1 1 calc R . . C4 C -0.35387(18) -1.4844(2) -0.14210(18) 0.0153(5) Uani 1 1 d . . . H4A H -0.3372 -1.5386 -0.1861 0.018 Uiso 1 1 calc R . . H4B H -0.4031 -1.5154 -0.1095 0.018 Uiso 1 1 calc R . . C5 C -0.44338(18) -1.4133(2) -0.25966(18) 0.0159(5) Uani 1 1 d . . . H5A H -0.4790 -1.3494 -0.2772 0.019 Uiso 1 1 calc R . . H5B H -0.4838 -1.4715 -0.2410 0.019 Uiso 1 1 calc R . . C6 C -0.39175(19) -1.4533(2) -0.33604(18) 0.0163(5) Uani 1 1 d . . . H6A H -0.3600 -1.5206 -0.3193 0.020 Uiso 1 1 calc R . . H6B H -0.4331 -1.4721 -0.3836 0.020 Uiso 1 1 calc R . . C7 C -0.26225(18) -1.4289(2) -0.42140(18) 0.0157(5) Uani 1 1 d . . . H7A H -0.2337 -1.3756 -0.4596 0.019 Uiso 1 1 calc R . . H7B H -0.2925 -1.4837 -0.4581 0.019 Uiso 1 1 calc R . . C8 C -0.19343(19) -1.4849(2) -0.36563(19) 0.0171(5) Uani 1 1 d . . . H8A H -0.2223 -1.5402 -0.3295 0.021 Uiso 1 1 calc R . . H8B H -0.1521 -1.5236 -0.4033 0.021 Uiso 1 1 calc R . . C9 C -0.07881(18) -1.3484(2) -0.35992(18) 0.0155(5) Uani 1 1 d . . . H9A H -0.0545 -1.3975 -0.4040 0.019 Uiso 1 1 calc R . . H9B H -0.0300 -1.3236 -0.3220 0.019 Uiso 1 1 calc R . . C10 C -0.12091(17) -1.2513(3) -0.40345(17) 0.0158(6) Uani 1 1 d . . . C11 C -0.14095(18) -1.3681(2) -0.06201(19) 0.0163(5) Uani 1 1 d . . . H11A H -0.1052 -1.4247 -0.0326 0.020 Uiso 1 1 calc R . . H11B H -0.1755 -1.3297 -0.0181 0.020 Uiso 1 1 calc R . . C12 C -0.08183(17) -1.28794(19) -0.10648(18) 0.0143(5) Uani 1 1 d . . . C13 C -0.43290(18) -1.3122(2) -0.12637(18) 0.0150(5) Uani 1 1 d . . . H13A H -0.4700 -1.3581 -0.0895 0.018 Uiso 1 1 calc R . . H13B H -0.4716 -1.2622 -0.1596 0.018 Uiso 1 1 calc R . . C14 C -0.37054(18) -1.2468(2) -0.07067(17) 0.0145(6) Uani 1 1 d . . . C15 C -0.37392(18) -1.2872(2) -0.41983(18) 0.0153(5) Uani 1 1 d . . . H15A H -0.4207 -1.3219 -0.4552 0.018 Uiso 1 1 calc R . . H15B H -0.3323 -1.2519 -0.4591 0.018 Uiso 1 1 calc R . . C16 C -0.41346(18) -1.2021(2) -0.36175(18) 0.0150(5) Uani 1 1 d . . . C17 C -0.11748(19) -1.1228(2) -0.52438(19) 0.0175(5) Uani 1 1 d . . . H17 H -0.1097 -1.0614 -0.4827 0.021 Uiso 1 1 calc R . . C18 C -0.21194(19) -1.1233(2) -0.55551(18) 0.0163(5) Uani 1 1 d . . . C19 C -0.2432(2) -1.1989(2) -0.6162(2) 0.0208(6) Uani 1 1 d . . . H19 H -0.2051 -1.2535 -0.6374 0.025 Uiso 1 1 calc R . . C20 C -0.3298(2) -1.1945(3) -0.6457(2) 0.0252(6) Uani 1 1 d . . . H20 H -0.3505 -1.2463 -0.6867 0.030 Uiso 1 1 calc R . . C21 C -0.3860(2) -1.1149(3) -0.6158(2) 0.0268(7) Uani 1 1 d . . . H21 H -0.4449 -1.1118 -0.6363 0.032 Uiso 1 1 calc R . . C22 C -0.3553(2) -1.0398(3) -0.5553(2) 0.0265(7) Uani 1 1 d . . . H22 H -0.3934 -0.9851 -0.5345 0.032 Uiso 1 1 calc R . . C23 C -0.2690(2) -1.0444(2) -0.5252(2) 0.0202(6) Uani 1 1 d . . . H23 H -0.2489 -0.9930 -0.4836 0.024 Uiso 1 1 calc R . . C24 C -0.0530(2) -1.1060(3) -0.5977(2) 0.0277(7) Uani 1 1 d . . . H24A H 0.0065 -1.0985 -0.5737 0.042 Uiso 1 1 calc R . . H24B H -0.0688 -1.0398 -0.6298 0.042 Uiso 1 1 calc R . . H24C H -0.0555 -1.1689 -0.6366 0.042 Uiso 1 1 calc R . . C25 C 0.05927(19) -1.1971(2) -0.1113(2) 0.0174(5) Uani 1 1 d . . . H25 H 0.0266 -1.1294 -0.1278 0.021 Uiso 1 1 calc R . . C26 C 0.09839(18) -1.2456(2) -0.19183(19) 0.0177(6) Uani 1 1 d . . . C27 C 0.1032(2) -1.1830(3) -0.2661(2) 0.0245(6) Uani 1 1 d . . . H27 H 0.0798 -1.1113 -0.2671 0.029 Uiso 1 1 calc R . . C28 C 0.1426(3) -1.2255(3) -0.3394(2) 0.0307(8) Uani 1 1 d . . . H28 H 0.1463 -1.1823 -0.3899 0.037 Uiso 1 1 calc R . . C29 C 0.1763(3) -1.3301(4) -0.3383(3) 0.0324(8) Uani 1 1 d . . . H29 H 0.2029 -1.3586 -0.3883 0.039 Uiso 1 1 calc R . . C30 C 0.1715(2) -1.3934(3) -0.2648(3) 0.0302(7) Uani 1 1 d . . . H30 H 0.1945 -1.4654 -0.2645 0.036 Uiso 1 1 calc R . . C31 C 0.1329(2) -1.3516(3) -0.1910(2) 0.0221(6) Uani 1 1 d . . . H31 H 0.1300 -1.3948 -0.1404 0.027 Uiso 1 1 calc R . . C32 C 0.1294(2) -1.1674(3) -0.0448(2) 0.0252(6) Uani 1 1 d . . . H32A H 0.1021 -1.1329 0.0048 0.038 Uiso 1 1 calc R . . H32B H 0.1711 -1.1166 -0.0703 0.038 Uiso 1 1 calc R . . H32C H 0.1603 -1.2335 -0.0260 0.038 Uiso 1 1 calc R . . C33 C -0.33765(19) -1.1573(2) 0.06568(19) 0.0163(5) Uani 1 1 d . . . H33 H -0.3046 -1.1043 0.0298 0.020 Uiso 1 1 calc R . . C34 C -0.2720(2) -1.2296(2) 0.1124(2) 0.0174(5) Uani 1 1 d . . . C35 C -0.1860(2) -1.1936(3) 0.1248(2) 0.0268(7) Uani 1 1 d . . . H35 H -0.1695 -1.1238 0.1043 0.032 Uiso 1 1 calc R . . C36 C -0.12441(19) -1.2587(5) 0.1666(2) 0.0341(7) Uani 1 1 d . . . H36 H -0.0662 -1.2330 0.1750 0.041 Uiso 1 1 calc R . . C37 C -0.1475(3) -1.3619(3) 0.1963(3) 0.0355(8) Uani 1 1 d . . . H37 H -0.1052 -1.4069 0.2245 0.043 Uiso 1 1 calc R . . C38 C -0.2326(3) -1.3979(3) 0.1844(2) 0.0313(7) Uani 1 1 d . . . H38 H -0.2488 -1.4681 0.2045 0.038 Uiso 1 1 calc R . . C39 C -0.2947(2) -1.3324(3) 0.1432(2) 0.0232(6) Uani 1 1 d . . . H39 H -0.3531 -1.3578 0.1360 0.028 Uiso 1 1 calc R . . C40 C -0.3939(2) -1.0924(3) 0.1279(2) 0.0228(6) Uani 1 1 d . . . H40A H -0.4337 -1.0446 0.0951 0.034 Uiso 1 1 calc R . . H40B H -0.3561 -1.0482 0.1657 0.034 Uiso 1 1 calc R . . H40C H -0.4281 -1.1429 0.1627 0.034 Uiso 1 1 calc R . . C41 C -0.5238(2) -1.0632(2) -0.33813(19) 0.0203(6) Uani 1 1 d . . . H41 H -0.4758 -1.0097 -0.3257 0.024 Uiso 1 1 calc R . . C42 C -0.56074(19) -1.1003(2) -0.2537(2) 0.0187(5) Uani 1 1 d . . . C43 C -0.5343(2) -1.0484(3) -0.1777(2) 0.0231(6) Uani 1 1 d . . . H43 H -0.4924 -0.9913 -0.1796 0.028 Uiso 1 1 calc R . . C44 C -0.5689(2) -1.0795(3) -0.0989(2) 0.0295(7) Uani 1 1 d . . . H44 H -0.5509 -1.0431 -0.0476 0.035 Uiso 1 1 calc R . . C45 C -0.6293(2) -1.1631(3) -0.0953(3) 0.0339(8) Uani 1 1 d . . . H45 H -0.6527 -1.1841 -0.0416 0.041 Uiso 1 1 calc R . . C46 C -0.6559(2) -1.2164(3) -0.1700(3) 0.0343(8) Uani 1 1 d . . . H46 H -0.6969 -1.2744 -0.1674 0.041 Uiso 1 1 calc R . . C47 C -0.6223(2) -1.1847(3) -0.2493(2) 0.0268(7) Uani 1 1 d . . . H47 H -0.6413 -1.2206 -0.3005 0.032 Uiso 1 1 calc R . . C48 C -0.5931(3) -1.0076(3) -0.3947(2) 0.0357(8) Uani 1 1 d . . . H48A H -0.5665 -0.9821 -0.4479 0.054 Uiso 1 1 calc R . . H48B H -0.6176 -0.9454 -0.3638 0.054 Uiso 1 1 calc R . . H48C H -0.6399 -1.0596 -0.4088 0.054 Uiso 1 1 calc R . . Cl1 Cl -0.25568(6) -0.92874(6) -0.04089(6) 0.02798(16) Uani 1 1 d . . . Cl2 Cl -0.44314(5) -0.75406(11) -0.26362(5) 0.03489(19) Uani 1 1 d . . . Cl3 Cl -0.21105(6) -0.75075(9) -0.44235(5) 0.03042(17) Uani 1 1 d . . . O1W O -0.22654(15) -1.06701(16) -0.21852(15) 0.0174(4) Uani 1 1 d D . . H1WA H -0.254(3) -1.027(4) -0.253(2) 0.051(18) Uiso 1 1 d D . . H1WB H -0.234(3) -1.042(3) -0.1696(14) 0.031(12) Uiso 1 1 d D . . O2W O -0.30581(17) -0.92771(19) -0.32663(17) 0.0263(5) Uani 1 1 d D . . H2WA H -0.272(3) -0.886(3) -0.351(3) 0.045(4) Uiso 1 1 d D . . H2WB H -0.343(2) -0.889(3) -0.304(3) 0.045(4) Uiso 1 1 d D . . O3W O -0.11562(18) -0.7504(3) -0.25860(18) 0.0343(6) Uani 1 1 d D . . H3WA H -0.1611(18) -0.751(5) -0.229(2) 0.045(4) Uiso 1 1 d D . . H3WB H -0.134(3) -0.740(4) -0.3091(13) 0.045(4) Uiso 1 1 d D . . O4W O -0.26340(19) -0.7291(2) -0.1599(2) 0.0318(6) Uani 1 1 d D . . H4WA H -0.306(2) -0.737(4) -0.193(2) 0.045(4) Uiso 1 1 d D . . H4WB H -0.263(3) -0.781(3) -0.125(2) 0.045(4) Uiso 1 1 d D . . O5W O -0.45375(17) -0.8296(2) -0.06883(17) 0.0303(5) Uani 1 1 d D . . H5WA H -0.449(3) -0.810(4) -0.1201(15) 0.045(4) Uiso 1 1 d D . . H5WB H -0.407(2) -0.860(4) -0.056(3) 0.045(4) Uiso 1 1 d D . . O6W O -0.04931(18) -0.9291(3) -0.05576(19) 0.0372(6) Uani 1 1 d D . . H6WA H -0.1020(15) -0.941(4) -0.049(3) 0.045(4) Uiso 1 1 d D . . H6WB H -0.042(3) -0.935(5) -0.1088(13) 0.045(4) Uiso 1 1 d D . . O7W O -0.05258(17) -0.9596(2) -0.2524(2) 0.0384(7) Uani 1 1 d D . . H7WA H -0.069(3) -0.8954(17) -0.248(4) 0.045(4) Uiso 1 1 d D . . H7WB H -0.096(2) -0.998(3) -0.244(4) 0.045(4) Uiso 1 1 d D . . O8W O -0.0287(2) -0.8767(2) -0.4424(2) 0.0365(6) Uani 1 1 d D . . H8WA H 0.002(3) -0.921(4) -0.414(3) 0.045(4) Uiso 1 1 d D . . H8WB H -0.0782(16) -0.877(4) -0.424(3) 0.045(4) Uiso 1 1 d D . . O9W O -0.42115(19) -0.7428(4) -0.46913(18) 0.0496(10) Uani 1 1 d D . . H9WA H -0.434(3) -0.738(4) -0.4181(14) 0.045(4) Uiso 1 1 d D . . H9WB H -0.3683(14) -0.754(5) -0.472(2) 0.045(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01153(5) 0.00897(5) 0.01221(5) 0.00000(7) 0.00113(3) -0.00028(5) N1 0.0143(10) 0.0109(10) 0.0148(11) 0.0014(8) 0.0017(8) -0.0005(8) N2 0.0140(10) 0.0120(10) 0.0139(10) 0.0000(8) 0.0035(8) -0.0004(8) N3 0.0122(10) 0.0125(10) 0.0138(10) 0.0001(8) 0.0013(8) 0.0019(8) N4 0.0145(10) 0.0123(10) 0.0139(10) 0.0004(8) 0.0021(8) 0.0007(8) N5 0.0177(11) 0.0154(9) 0.0194(12) 0.0031(8) 0.0036(9) 0.0006(8) N6 0.0146(9) 0.0164(12) 0.0152(9) -0.0002(10) -0.0023(7) -0.0026(10) N7 0.0146(11) 0.0176(10) 0.0164(12) -0.0026(8) 0.0032(9) -0.0002(8) N8 0.0185(11) 0.0194(11) 0.0163(11) -0.0001(9) -0.0015(9) 0.0035(9) O1 0.0175(10) 0.0134(9) 0.0194(10) 0.0015(7) 0.0043(7) 0.0013(7) O2 0.0132(8) 0.0146(11) 0.0162(9) 0.0014(6) -0.0014(7) -0.0007(6) O3 0.0155(9) 0.0145(8) 0.0162(9) -0.0020(7) 0.0031(7) 0.0008(7) O4 0.0160(9) 0.0139(9) 0.0164(10) -0.0002(7) -0.0009(7) 0.0011(7) C1 0.0147(12) 0.0108(11) 0.0186(12) 0.0015(9) 0.0031(9) 0.0026(9) C2 0.0183(13) 0.0130(11) 0.0180(13) 0.0015(9) 0.0041(10) 0.0023(9) C3 0.0123(11) 0.0166(12) 0.0147(12) 0.0022(9) 0.0028(9) 0.0001(9) C4 0.0148(12) 0.0125(11) 0.0185(13) 0.0035(9) -0.0007(10) -0.0010(9) C5 0.0141(12) 0.0165(12) 0.0171(13) 0.0004(10) 0.0022(10) -0.0034(9) C6 0.0171(13) 0.0160(12) 0.0160(12) -0.0019(9) 0.0016(10) -0.0055(9) C7 0.0165(12) 0.0155(12) 0.0150(12) -0.0031(9) 0.0008(10) 0.0003(9) C8 0.0189(13) 0.0151(12) 0.0173(13) -0.0044(10) 0.0001(10) 0.0014(10) C9 0.0151(12) 0.0159(12) 0.0156(12) 0.0035(9) 0.0032(9) 0.0020(9) C10 0.0139(10) 0.0179(17) 0.0156(10) 0.0016(12) 0.0023(8) -0.0010(12) C11 0.0138(12) 0.0175(12) 0.0176(13) -0.0005(10) 0.0028(10) -0.0006(9) C12 0.0122(11) 0.0128(14) 0.0180(12) -0.0026(8) 0.0019(9) 0.0011(8) C13 0.0130(12) 0.0162(12) 0.0159(12) -0.0010(10) 0.0022(9) 0.0013(9) C14 0.0153(10) 0.0123(18) 0.0159(11) 0.0002(9) 0.0024(8) 0.0023(9) C15 0.0163(11) 0.0157(15) 0.0138(11) 0.0003(8) 0.0000(9) 0.0000(8) C16 0.0154(12) 0.0133(12) 0.0165(12) 0.0027(9) 0.0012(9) 0.0004(9) C17 0.0166(13) 0.0150(12) 0.0210(13) 0.0031(10) 0.0029(10) -0.0017(9) C18 0.0177(13) 0.0147(12) 0.0164(13) 0.0041(9) 0.0026(10) -0.0025(10) C19 0.0254(15) 0.0181(13) 0.0191(14) -0.0015(10) 0.0035(11) 0.0001(11) C20 0.0300(17) 0.0248(14) 0.0209(15) 0.0013(11) -0.0014(12) -0.0063(12) C21 0.0218(15) 0.0267(15) 0.0318(17) 0.0065(13) -0.0023(12) -0.0005(12) C22 0.0227(15) 0.0206(14) 0.0363(18) 0.0026(12) 0.0037(13) 0.0042(11) C23 0.0227(14) 0.0145(12) 0.0236(14) -0.0035(10) 0.0025(11) -0.0012(10) C24 0.0253(16) 0.0294(16) 0.0288(17) 0.0157(13) 0.0114(13) 0.0017(12) C25 0.0148(12) 0.0159(12) 0.0215(14) -0.0036(10) 0.0018(10) -0.0013(9) C26 0.0150(11) 0.0187(17) 0.0196(12) -0.0053(10) 0.0011(8) -0.0026(10) C27 0.0269(16) 0.0244(15) 0.0225(15) -0.0021(12) 0.0030(12) -0.0026(12) C28 0.035(2) 0.0368(18) 0.0211(16) -0.0036(13) 0.0077(14) -0.0090(14) C29 0.0282(19) 0.042(2) 0.0276(18) -0.0148(15) 0.0064(15) -0.0025(16) C30 0.0264(16) 0.0265(16) 0.0377(19) -0.0132(14) 0.0018(14) 0.0021(13) C31 0.0200(14) 0.0208(14) 0.0255(15) -0.0056(11) 0.0012(11) 0.0000(11) C32 0.0222(15) 0.0302(16) 0.0232(15) -0.0093(12) -0.0013(12) -0.0072(12) C33 0.0167(12) 0.0146(11) 0.0178(13) -0.0024(10) 0.0039(10) -0.0004(9) C34 0.0180(13) 0.0198(13) 0.0145(12) -0.0041(9) 0.0024(10) 0.0025(9) C35 0.0203(15) 0.0289(16) 0.0314(17) -0.0073(13) 0.0025(12) -0.0014(12) C36 0.0208(12) 0.0443(18) 0.0369(16) -0.011(3) -0.0039(11) 0.000(2) C37 0.0348(19) 0.040(2) 0.0318(19) -0.0047(15) -0.0048(15) 0.0179(16) C38 0.040(2) 0.0241(16) 0.0296(17) 0.0006(13) -0.0012(14) 0.0098(14) C39 0.0246(15) 0.0209(14) 0.0241(15) -0.0005(12) 0.0013(12) 0.0018(12) C40 0.0229(14) 0.0228(14) 0.0227(15) -0.0051(11) 0.0046(11) 0.0052(11) C41 0.0248(14) 0.0187(13) 0.0176(13) 0.0003(10) 0.0005(11) 0.0072(11) C42 0.0145(12) 0.0186(13) 0.0229(14) -0.0005(10) 0.0005(10) 0.0070(10) C43 0.0249(15) 0.0195(13) 0.0249(15) -0.0015(11) -0.0007(12) 0.0057(11) C44 0.0353(18) 0.0294(16) 0.0239(16) -0.0022(13) 0.0043(13) 0.0136(14) C45 0.0297(18) 0.0401(19) 0.0322(19) 0.0091(15) 0.0127(14) 0.0142(15) C46 0.0180(16) 0.0385(18) 0.047(2) 0.0048(16) 0.0079(14) -0.0004(13) C47 0.0161(14) 0.0331(17) 0.0313(18) -0.0035(13) -0.0011(12) -0.0003(12) C48 0.040(2) 0.040(2) 0.0269(17) 0.0062(15) -0.0028(15) 0.0219(16) Cl1 0.0318(4) 0.0202(3) 0.0320(4) 0.0031(3) 0.0030(3) -0.0027(3) Cl2 0.0329(4) 0.0456(5) 0.0262(3) 0.0023(5) 0.0019(3) 0.0182(5) Cl3 0.0372(4) 0.0261(4) 0.0282(3) -0.0013(4) 0.0065(3) -0.0053(4) O1W 0.0220(10) 0.0112(9) 0.0191(10) -0.0008(7) 0.0012(8) 0.0001(7) O2W 0.0310(13) 0.0179(10) 0.0302(13) 0.0040(9) 0.0052(10) 0.0054(9) O3W 0.0386(12) 0.0272(14) 0.0374(12) -0.0053(13) 0.0058(10) -0.0027(12) O4W 0.0328(13) 0.0184(10) 0.0442(16) 0.0049(9) 0.0014(12) -0.0055(9) O5W 0.0222(12) 0.0420(15) 0.0269(12) -0.0044(10) 0.0055(9) 0.0039(10) O6W 0.0265(13) 0.0496(16) 0.0353(15) -0.0141(13) -0.0026(11) -0.0015(12) O7W 0.0194(12) 0.0224(12) 0.073(2) -0.0046(13) 0.0012(12) -0.0020(9) O8W 0.0331(14) 0.0331(14) 0.0440(17) -0.0044(11) 0.0163(12) -0.0060(11) O9W 0.0361(13) 0.089(3) 0.0240(12) 0.0142(16) -0.0019(10) 0.0193(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O3 2.356(2) . ? Gd1 O4 2.356(2) . ? Gd1 O2 2.365(2) . ? Gd1 O1 2.400(2) . ? Gd1 O1W 2.435(2) . ? Gd1 N1 2.655(2) . ? Gd1 N2 2.681(2) . ? Gd1 N3 2.692(2) . ? Gd1 N4 2.700(2) . ? N1 C9 1.475(3) . ? N1 C1 1.489(4) . ? N1 C8 1.494(4) . ? N2 C11 1.484(4) . ? N2 C3 1.486(3) . ? N2 C2 1.489(3) . ? N3 C13 1.484(3) . ? N3 C5 1.485(4) . ? N3 C4 1.496(3) . ? N4 C15 1.485(3) . ? N4 C7 1.490(3) . ? N4 C6 1.494(3) . ? N5 C10 1.323(4) . ? N5 C17 1.472(4) . ? N5 H5C 0.8800 . ? N6 C12 1.328(3) . ? N6 C25 1.473(4) . ? N6 H6C 0.8800 . ? N7 C14 1.324(3) . ? N7 C33 1.467(4) . ? N7 H7C 0.8800 . ? N8 C16 1.320(4) . ? N8 C41 1.476(4) . ? N8 H8C 0.8800 . ? O1 C10 1.254(4) . ? O2 C12 1.247(3) . ? O3 C14 1.256(3) . ? O4 C16 1.251(4) . ? C1 C2 1.518(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.506(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.519(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.515(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.508(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.512(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 C14 1.506(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.514(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C18 1.514(4) . ? C17 C24 1.536(4) . ? C17 H17 1.0000 . ? C18 C23 1.392(4) . ? C18 C19 1.399(4) . ? C19 C20 1.394(5) . ? C19 H19 0.9500 . ? C20 C21 1.386(5) . ? C20 H20 0.9500 . ? C21 C22 1.390(5) . ? C21 H21 0.9500 . ? C22 C23 1.391(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.518(4) . ? C25 C32 1.519(4) . ? C25 H25 1.0000 . ? C26 C27 1.389(4) . ? C26 C31 1.402(4) . ? C27 C28 1.399(5) . ? C27 H27 0.9500 . ? C28 C29 1.383(6) . ? C28 H28 0.9500 . ? C29 C30 1.384(6) . ? C29 H29 0.9500 . ? C30 C31 1.398(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.514(4) . ? C33 C40 1.530(4) . ? C33 H33 1.0000 . ? C34 C39 1.394(4) . ? C34 C35 1.397(4) . ? C35 C36 1.386(6) . ? C35 H35 0.9500 . ? C36 C37 1.394(7) . ? C36 H36 0.9500 . ? C37 C38 1.383(6) . ? C37 H37 0.9500 . ? C38 C39 1.389(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.509(4) . ? C41 C48 1.525(4) . ? C41 H41 1.0000 . ? C42 C43 1.394(4) . ? C42 C47 1.401(4) . ? C43 C44 1.397(5) . ? C43 H43 0.9500 . ? C44 C45 1.382(6) . ? C44 H44 0.9500 . ? C45 C46 1.385(6) . ? C45 H45 0.9500 . ? C46 C47 1.400(5) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? O1W H1WA 0.829(18) . ? O1W H1WB 0.829(18) . ? O2W H2WA 0.826(18) . ? O2W H2WB 0.826(18) . ? O3W H3WA 0.839(18) . ? O3W H3WB 0.841(18) . ? O4W H4WA 0.820(18) . ? O4W H4WB 0.832(18) . ? O5W H5WA 0.837(18) . ? O5W H5WB 0.830(18) . ? O6W H6WA 0.829(18) . ? O6W H6WB 0.836(18) . ? O7W H7WA 0.831(18) . ? O7W H7WB 0.823(18) . ? O8W H8WA 0.840(18) . ? O8W H8WB 0.814(18) . ? O9W H9WA 0.822(18) . ? O9W H9WB 0.822(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Gd1 O4 86.66(7) . . ? O3 Gd1 O2 83.67(7) . . ? O4 Gd1 O2 146.04(6) . . ? O3 Gd1 O1 146.22(7) . . ? O4 Gd1 O1 85.49(7) . . ? O2 Gd1 O1 84.74(7) . . ? O3 Gd1 O1W 72.64(7) . . ? O4 Gd1 O1W 73.17(7) . . ? O2 Gd1 O1W 72.87(7) . . ? O1 Gd1 O1W 73.63(7) . . ? O3 Gd1 N1 138.57(7) . . ? O4 Gd1 N1 130.24(7) . . ? O2 Gd1 N1 73.91(7) . . ? O1 Gd1 N1 66.46(7) . . ? O1W Gd1 N1 129.54(7) . . ? O3 Gd1 N2 71.02(7) . . ? O4 Gd1 N2 139.84(7) . . ? O2 Gd1 N2 65.79(7) . . ? O1 Gd1 N2 130.99(7) . . ? O1W Gd1 N2 126.85(8) . . ? N1 Gd1 N2 68.10(7) . . ? O3 Gd1 N3 65.83(7) . . ? O4 Gd1 N3 73.29(7) . . ? O2 Gd1 N3 130.06(7) . . ? O1 Gd1 N3 141.21(7) . . ? O1W Gd1 N3 127.20(7) . . ? N1 Gd1 N3 103.25(7) . . ? N2 Gd1 N3 67.23(7) . . ? O3 Gd1 N4 130.09(7) . . ? O4 Gd1 N4 65.65(7) . . ? O2 Gd1 N4 141.21(7) . . ? O1 Gd1 N4 75.05(7) . . ? O1W Gd1 N4 129.40(7) . . ? N1 Gd1 N4 67.74(7) . . ? N2 Gd1 N4 103.69(7) . . ? N3 Gd1 N4 66.72(7) . . ? C9 N1 C1 108.3(2) . . ? C9 N1 C8 109.4(2) . . ? C1 N1 C8 109.2(2) . . ? C9 N1 Gd1 107.39(15) . . ? C1 N1 Gd1 111.16(16) . . ? C8 N1 Gd1 111.26(16) . . ? C11 N2 C3 109.3(2) . . ? C11 N2 C2 110.0(2) . . ? C3 N2 C2 108.6(2) . . ? C11 N2 Gd1 105.98(16) . . ? C3 N2 Gd1 112.22(16) . . ? C2 N2 Gd1 110.74(16) . . ? C13 N3 C5 109.0(2) . . ? C13 N3 C4 110.5(2) . . ? C5 N3 C4 108.7(2) . . ? C13 N3 Gd1 105.53(16) . . ? C5 N3 Gd1 112.25(16) . . ? C4 N3 Gd1 110.87(16) . . ? C15 N4 C7 110.0(2) . . ? C15 N4 C6 109.8(2) . . ? C7 N4 C6 108.6(2) . . ? C15 N4 Gd1 105.55(15) . . ? C7 N4 Gd1 110.77(16) . . ? C6 N4 Gd1 112.14(16) . . ? C10 N5 C17 122.7(3) . . ? C10 N5 H5C 118.7 . . ? C17 N5 H5C 118.7 . . ? C12 N6 C25 120.2(2) . . ? C12 N6 H6C 119.9 . . ? C25 N6 H6C 119.9 . . ? C14 N7 C33 120.9(2) . . ? C14 N7 H7C 119.5 . . ? C33 N7 H7C 119.5 . . ? C16 N8 C41 120.6(3) . . ? C16 N8 H8C 119.7 . . ? C41 N8 H8C 119.7 . . ? C10 O1 Gd1 122.9(2) . . ? C12 O2 Gd1 123.88(17) . . ? C14 O3 Gd1 124.60(18) . . ? C16 O4 Gd1 125.31(18) . . ? N1 C1 C2 111.2(2) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 114.4(2) . . ? N2 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? N2 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N2 C3 C4 111.7(2) . . ? N2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C3 113.5(2) . . ? N3 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? N3 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? N3 C5 C6 111.2(2) . . ? N3 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N3 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N4 C6 C5 113.3(2) . . ? N4 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? N4 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N4 C7 C8 111.1(2) . . ? N4 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N4 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N1 C8 C7 113.6(2) . . ? N1 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N1 C9 C10 110.8(2) . . ? N1 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O1 C10 N5 123.2(3) . . ? O1 C10 C9 119.8(2) . . ? N5 C10 C9 116.9(3) . . ? N2 C11 C12 109.8(2) . . ? N2 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O2 C12 N6 122.6(2) . . ? O2 C12 C11 120.7(2) . . ? N6 C12 C11 116.7(2) . . ? N3 C13 C14 110.7(2) . . ? N3 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O3 C14 N7 122.1(3) . . ? O3 C14 C13 119.8(2) . . ? N7 C14 C13 118.1(2) . . ? N4 C15 C16 110.3(2) . . ? N4 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? N4 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? O4 C16 N8 122.5(3) . . ? O4 C16 C15 119.3(2) . . ? N8 C16 C15 118.1(3) . . ? N5 C17 C18 112.8(2) . . ? N5 C17 C24 106.9(2) . . ? C18 C17 C24 112.7(3) . . ? N5 C17 H17 108.1 . . ? C18 C17 H17 108.1 . . ? C24 C17 H17 108.1 . . ? C23 C18 C19 118.7(3) . . ? C23 C18 C17 119.3(3) . . ? C19 C18 C17 121.9(3) . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.4(3) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 120.7(3) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? C17 C24 H24A 109.5 . . ? C17 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C17 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C25 C26 110.8(2) . . ? N6 C25 C32 108.7(2) . . ? C26 C25 C32 111.7(2) . . ? N6 C25 H25 108.5 . . ? C26 C25 H25 108.5 . . ? C32 C25 H25 108.5 . . ? C27 C26 C31 119.6(3) . . ? C27 C26 C25 119.8(3) . . ? C31 C26 C25 120.6(3) . . ? C26 C27 C28 120.1(3) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 120.1(4) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.3(3) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C31 120.1(3) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C26 119.8(3) . . ? C30 C31 H31 120.1 . . ? C26 C31 H31 120.1 . . ? C25 C32 H32A 109.5 . . ? C25 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C25 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N7 C33 C34 111.0(2) . . ? N7 C33 C40 109.1(2) . . ? C34 C33 C40 112.2(3) . . ? N7 C33 H33 108.1 . . ? C34 C33 H33 108.1 . . ? C40 C33 H33 108.1 . . ? C39 C34 C35 118.5(3) . . ? C39 C34 C33 121.9(3) . . ? C35 C34 C33 119.6(3) . . ? C36 C35 C34 120.7(4) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 120.3(3) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C36 119.3(3) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C37 C38 C39 120.6(4) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C34 120.6(3) . . ? C38 C39 H39 119.7 . . ? C34 C39 H39 119.7 . . ? C33 C40 H40A 109.5 . . ? C33 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C33 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N8 C41 C42 112.0(2) . . ? N8 C41 C48 108.0(3) . . ? C42 C41 C48 111.6(3) . . ? N8 C41 H41 108.4 . . ? C42 C41 H41 108.4 . . ? C48 C41 H41 108.4 . . ? C43 C42 C47 118.7(3) . . ? C43 C42 C41 119.4(3) . . ? C47 C42 C41 121.9(3) . . ? C42 C43 C44 120.7(3) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C45 C44 C43 120.2(3) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.1(3) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C47 120.0(4) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C42 120.4(3) . . ? C46 C47 H47 119.8 . . ? C42 C47 H47 119.8 . . ? C41 C48 H48A 109.5 . . ? C41 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C41 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Gd1 O1W H1WA 116(4) . . ? Gd1 O1W H1WB 117(3) . . ? H1WA O1W H1WB 107(3) . . ? H2WA O2W H2WB 106(3) . . ? H3WA O3W H3WB 104(2) . . ? H4WA O4W H4WB 107(3) . . ? H5WA O5W H5WB 105(3) . . ? H6WA O6W H6WB 105(3) . . ? H7WA O7W H7WB 106(3) . . ? H8WA O8W H8WB 109(3) . . ? H9WA O9W H9WB 108(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Gd1 N1 C9 -127.42(17) . . . . ? O4 Gd1 N1 C9 85.04(19) . . . . ? O2 Gd1 N1 C9 -67.44(17) . . . . ? O1 Gd1 N1 C9 23.80(16) . . . . ? O1W Gd1 N1 C9 -16.9(2) . . . . ? N2 Gd1 N1 C9 -137.32(19) . . . . ? N3 Gd1 N1 C9 164.22(17) . . . . ? N4 Gd1 N1 C9 106.57(18) . . . . ? O3 Gd1 N1 C1 -9.1(2) . . . . ? O4 Gd1 N1 C1 -156.61(15) . . . . ? O2 Gd1 N1 C1 50.91(16) . . . . ? O1 Gd1 N1 C1 142.15(18) . . . . ? O1W Gd1 N1 C1 101.45(17) . . . . ? N2 Gd1 N1 C1 -18.97(16) . . . . ? N3 Gd1 N1 C1 -77.42(17) . . . . ? N4 Gd1 N1 C1 -135.07(18) . . . . ? O3 Gd1 N1 C8 112.83(18) . . . . ? O4 Gd1 N1 C8 -34.7(2) . . . . ? O2 Gd1 N1 C8 172.81(18) . . . . ? O1 Gd1 N1 C8 -95.95(18) . . . . ? O1W Gd1 N1 C8 -136.64(17) . . . . ? N2 Gd1 N1 C8 102.93(18) . . . . ? N3 Gd1 N1 C8 44.48(18) . . . . ? N4 Gd1 N1 C8 -13.17(16) . . . . ? O3 Gd1 N2 C11 -63.16(16) . . . . ? O4 Gd1 N2 C11 -122.96(16) . . . . ? O2 Gd1 N2 C11 28.37(15) . . . . ? O1 Gd1 N2 C11 86.78(17) . . . . ? O1W Gd1 N2 C11 -13.86(19) . . . . ? N1 Gd1 N2 C11 109.93(17) . . . . ? N3 Gd1 N2 C11 -134.18(17) . . . . ? N4 Gd1 N2 C11 168.73(15) . . . . ? O3 Gd1 N2 C3 56.01(17) . . . . ? O4 Gd1 N2 C3 -3.8(2) . . . . ? O2 Gd1 N2 C3 147.55(19) . . . . ? O1 Gd1 N2 C3 -154.04(16) . . . . ? O1W Gd1 N2 C3 105.32(18) . . . . ? N1 Gd1 N2 C3 -130.89(19) . . . . ? N3 Gd1 N2 C3 -15.01(16) . . . . ? N4 Gd1 N2 C3 -72.09(18) . . . . ? O3 Gd1 N2 C2 177.58(19) . . . . ? O4 Gd1 N2 C2 117.78(17) . . . . ? O2 Gd1 N2 C2 -90.89(18) . . . . ? O1 Gd1 N2 C2 -32.5(2) . . . . ? O1W Gd1 N2 C2 -133.12(17) . . . . ? N1 Gd1 N2 C2 -9.33(16) . . . . ? N3 Gd1 N2 C2 106.56(18) . . . . ? N4 Gd1 N2 C2 49.47(18) . . . . ? O3 Gd1 N3 C13 27.56(16) . . . . ? O4 Gd1 N3 C13 -66.34(16) . . . . ? O2 Gd1 N3 C13 85.19(18) . . . . ? O1 Gd1 N3 C13 -126.05(17) . . . . ? O1W Gd1 N3 C13 -13.7(2) . . . . ? N1 Gd1 N3 C13 165.18(16) . . . . ? N2 Gd1 N3 C13 106.13(17) . . . . ? N4 Gd1 N3 C13 -136.49(18) . . . . ? O3 Gd1 N3 C5 146.14(19) . . . . ? O4 Gd1 N3 C5 52.24(17) . . . . ? O2 Gd1 N3 C5 -156.23(15) . . . . ? O1 Gd1 N3 C5 -7.5(2) . . . . ? O1W Gd1 N3 C5 104.84(18) . . . . ? N1 Gd1 N3 C5 -76.24(18) . . . . ? N2 Gd1 N3 C5 -135.29(18) . . . . ? N4 Gd1 N3 C5 -17.91(16) . . . . ? O3 Gd1 N3 C4 -92.05(18) . . . . ? O4 Gd1 N3 C4 174.04(18) . . . . ? O2 Gd1 N3 C4 -34.4(2) . . . . ? O1 Gd1 N3 C4 114.34(18) . . . . ? O1W Gd1 N3 C4 -133.35(17) . . . . ? N1 Gd1 N3 C4 45.56(18) . . . . ? N2 Gd1 N3 C4 -13.49(16) . . . . ? N4 Gd1 N3 C4 103.89(18) . . . . ? O3 Gd1 N4 C15 89.47(17) . . . . ? O4 Gd1 N4 C15 27.15(15) . . . . ? O2 Gd1 N4 C15 -125.74(16) . . . . ? O1 Gd1 N4 C15 -64.65(16) . . . . ? O1W Gd1 N4 C15 -11.29(19) . . . . ? N1 Gd1 N4 C15 -134.93(17) . . . . ? N2 Gd1 N4 C15 166.02(15) . . . . ? N3 Gd1 N4 C15 108.60(17) . . . . ? O3 Gd1 N4 C7 -151.51(16) . . . . ? O4 Gd1 N4 C7 146.17(18) . . . . ? O2 Gd1 N4 C7 -6.7(2) . . . . ? O1 Gd1 N4 C7 54.36(17) . . . . ? O1W Gd1 N4 C7 107.72(17) . . . . ? N1 Gd1 N4 C7 -15.92(16) . . . . ? N2 Gd1 N4 C7 -74.96(17) . . . . ? N3 Gd1 N4 C7 -132.39(18) . . . . ? O3 Gd1 N4 C6 -30.0(2) . . . . ? O4 Gd1 N4 C6 -92.31(18) . . . . ? O2 Gd1 N4 C6 114.80(18) . . . . ? O1 Gd1 N4 C6 175.88(18) . . . . ? O1W Gd1 N4 C6 -130.76(17) . . . . ? N1 Gd1 N4 C6 105.60(18) . . . . ? N2 Gd1 N4 C6 46.56(18) . . . . ? N3 Gd1 N4 C6 -10.87(16) . . . . ? O3 Gd1 O1 C10 138.2(2) . . . . ? O4 Gd1 O1 C10 -144.7(2) . . . . ? O2 Gd1 O1 C10 67.9(2) . . . . ? O1W Gd1 O1 C10 141.5(2) . . . . ? N1 Gd1 O1 C10 -6.8(2) . . . . ? N2 Gd1 O1 C10 16.6(3) . . . . ? N3 Gd1 O1 C10 -88.6(2) . . . . ? N4 Gd1 O1 C10 -78.7(2) . . . . ? O3 Gd1 O2 C12 56.8(2) . . . . ? O4 Gd1 O2 C12 131.16(19) . . . . ? O1 Gd1 O2 C12 -155.0(2) . . . . ? O1W Gd1 O2 C12 130.5(2) . . . . ? N1 Gd1 O2 C12 -88.0(2) . . . . ? N2 Gd1 O2 C12 -15.21(19) . . . . ? N3 Gd1 O2 C12 6.0(2) . . . . ? N4 Gd1 O2 C12 -96.9(2) . . . . ? O4 Gd1 O3 C14 58.8(2) . . . . ? O2 Gd1 O3 C14 -153.8(2) . . . . ? O1 Gd1 O3 C14 135.6(2) . . . . ? O1W Gd1 O3 C14 132.2(2) . . . . ? N1 Gd1 O3 C14 -97.0(2) . . . . ? N2 Gd1 O3 C14 -87.3(2) . . . . ? N3 Gd1 O3 C14 -14.4(2) . . . . ? N4 Gd1 O3 C14 4.9(3) . . . . ? O3 Gd1 O4 C16 -149.9(2) . . . . ? O2 Gd1 O4 C16 136.7(2) . . . . ? O1 Gd1 O4 C16 63.0(2) . . . . ? O1W Gd1 O4 C16 137.3(2) . . . . ? N1 Gd1 O4 C16 9.3(3) . . . . ? N2 Gd1 O4 C16 -94.9(2) . . . . ? N3 Gd1 O4 C16 -84.1(2) . . . . ? N4 Gd1 O4 C16 -12.6(2) . . . . ? C9 N1 C1 C2 163.6(2) . . . . ? C8 N1 C1 C2 -77.3(3) . . . . ? Gd1 N1 C1 C2 45.8(2) . . . . ? C11 N2 C2 C1 -79.0(3) . . . . ? C3 N2 C2 C1 161.4(2) . . . . ? Gd1 N2 C2 C1 37.8(3) . . . . ? N1 C1 C2 N2 -58.2(3) . . . . ? C11 N2 C3 C4 159.9(2) . . . . ? C2 N2 C3 C4 -80.1(3) . . . . ? Gd1 N2 C3 C4 42.7(3) . . . . ? C13 N3 C4 C3 -74.6(3) . . . . ? C5 N3 C4 C3 165.9(2) . . . . ? Gd1 N3 C4 C3 42.0(3) . . . . ? N2 C3 C4 N3 -58.6(3) . . . . ? C13 N3 C5 C6 161.7(2) . . . . ? C4 N3 C5 C6 -77.8(3) . . . . ? Gd1 N3 C5 C6 45.2(2) . . . . ? C15 N4 C6 C5 -77.8(3) . . . . ? C7 N4 C6 C5 161.9(2) . . . . ? Gd1 N4 C6 C5 39.2(3) . . . . ? N3 C5 C6 N4 -58.0(3) . . . . ? C15 N4 C7 C8 160.0(2) . . . . ? C6 N4 C7 C8 -79.9(3) . . . . ? Gd1 N4 C7 C8 43.7(2) . . . . ? C9 N1 C8 C7 -76.1(3) . . . . ? C1 N1 C8 C7 165.5(2) . . . . ? Gd1 N1 C8 C7 42.5(3) . . . . ? N4 C7 C8 N1 -59.9(3) . . . . ? C1 N1 C9 C10 -157.6(2) . . . . ? C8 N1 C9 C10 83.5(3) . . . . ? Gd1 N1 C9 C10 -37.4(3) . . . . ? Gd1 O1 C10 N5 169.7(2) . . . . ? Gd1 O1 C10 C9 -12.7(4) . . . . ? C17 N5 C10 O1 7.0(5) . . . . ? C17 N5 C10 C9 -170.7(3) . . . . ? N1 C9 C10 O1 36.4(4) . . . . ? N1 C9 C10 N5 -145.9(3) . . . . ? C3 N2 C11 C12 -160.0(2) . . . . ? C2 N2 C11 C12 80.9(3) . . . . ? Gd1 N2 C11 C12 -38.9(2) . . . . ? Gd1 O2 C12 N6 178.4(2) . . . . ? Gd1 O2 C12 C11 -2.2(3) . . . . ? C25 N6 C12 O2 -0.4(4) . . . . ? C25 N6 C12 C11 -179.8(2) . . . . ? N2 C11 C12 O2 31.6(3) . . . . ? N2 C11 C12 N6 -149.0(2) . . . . ? C5 N3 C13 C14 -159.3(2) . . . . ? C4 N3 C13 C14 81.3(3) . . . . ? Gd1 N3 C13 C14 -38.6(2) . . . . ? Gd1 O3 C14 N7 178.0(2) . . . . ? Gd1 O3 C14 C13 -3.1(4) . . . . ? C33 N7 C14 O3 -0.6(4) . . . . ? C33 N7 C14 C13 -179.6(2) . . . . ? N3 C13 C14 O3 32.0(4) . . . . ? N3 C13 C14 N7 -148.9(3) . . . . ? C7 N4 C15 C16 -158.6(2) . . . . ? C6 N4 C15 C16 82.0(3) . . . . ? Gd1 N4 C15 C16 -39.1(2) . . . . ? Gd1 O4 C16 N8 176.3(2) . . . . ? Gd1 O4 C16 C15 -5.9(3) . . . . ? C41 N8 C16 O4 4.2(4) . . . . ? C41 N8 C16 C15 -173.5(2) . . . . ? N4 C15 C16 O4 34.1(3) . . . . ? N4 C15 C16 N8 -148.0(2) . . . . ? C10 N5 C17 C18 -70.7(4) . . . . ? C10 N5 C17 C24 164.8(3) . . . . ? N5 C17 C18 C23 120.2(3) . . . . ? C24 C17 C18 C23 -118.5(3) . . . . ? N5 C17 C18 C19 -61.9(4) . . . . ? C24 C17 C18 C19 59.3(4) . . . . ? C23 C18 C19 C20 0.2(4) . . . . ? C17 C18 C19 C20 -177.7(3) . . . . ? C18 C19 C20 C21 0.3(5) . . . . ? C19 C20 C21 C22 -0.4(5) . . . . ? C20 C21 C22 C23 0.0(5) . . . . ? C21 C22 C23 C18 0.6(5) . . . . ? C19 C18 C23 C22 -0.7(4) . . . . ? C17 C18 C23 C22 177.3(3) . . . . ? C12 N6 C25 C26 -76.5(3) . . . . ? C12 N6 C25 C32 160.3(3) . . . . ? N6 C25 C26 C27 134.2(3) . . . . ? C32 C25 C26 C27 -104.4(3) . . . . ? N6 C25 C26 C31 -48.3(4) . . . . ? C32 C25 C26 C31 73.1(3) . . . . ? C31 C26 C27 C28 -0.3(5) . . . . ? C25 C26 C27 C28 177.2(3) . . . . ? C26 C27 C28 C29 0.5(6) . . . . ? C27 C28 C29 C30 -0.2(6) . . . . ? C28 C29 C30 C31 -0.3(6) . . . . ? C29 C30 C31 C26 0.5(5) . . . . ? C27 C26 C31 C30 -0.2(5) . . . . ? C25 C26 C31 C30 -177.7(3) . . . . ? C14 N7 C33 C34 -84.7(3) . . . . ? C14 N7 C33 C40 151.2(3) . . . . ? N7 C33 C34 C39 -39.2(4) . . . . ? C40 C33 C34 C39 83.2(3) . . . . ? N7 C33 C34 C35 140.3(3) . . . . ? C40 C33 C34 C35 -97.3(3) . . . . ? C39 C34 C35 C36 0.1(5) . . . . ? C33 C34 C35 C36 -179.4(3) . . . . ? C34 C35 C36 C37 0.6(5) . . . . ? C35 C36 C37 C38 -0.7(6) . . . . ? C36 C37 C38 C39 0.0(6) . . . . ? C37 C38 C39 C34 0.7(5) . . . . ? C35 C34 C39 C38 -0.7(5) . . . . ? C33 C34 C39 C38 178.7(3) . . . . ? C16 N8 C41 C42 -71.5(4) . . . . ? C16 N8 C41 C48 165.3(3) . . . . ? N8 C41 C42 C43 127.9(3) . . . . ? C48 C41 C42 C43 -110.9(3) . . . . ? N8 C41 C42 C47 -53.2(4) . . . . ? C48 C41 C42 C47 68.0(4) . . . . ? C47 C42 C43 C44 -0.4(4) . . . . ? C41 C42 C43 C44 178.6(3) . . . . ? C42 C43 C44 C45 0.6(5) . . . . ? C43 C44 C45 C46 -0.1(5) . . . . ? C44 C45 C46 C47 -0.7(6) . . . . ? C45 C46 C47 C42 1.0(5) . . . . ? C43 C42 C47 C46 -0.4(5) . . . . ? C41 C42 C47 C46 -179.4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O2W 0.829(18) 1.84(2) 2.670(3) 174(6) . O1W H1WB Cl1 0.829(18) 2.46(2) 3.277(2) 167(4) . O2W H2WB Cl2 0.826(18) 2.35(2) 3.160(3) 168(4) . O2W H2WA Cl3 0.826(18) 2.38(2) 3.185(3) 164(5) . O3W H3WB Cl3 0.841(18) 2.36(2) 3.180(3) 164(4) . O3W H3WA O4W 0.839(18) 1.94(2) 2.767(4) 171(6) . O4W H4WB Cl1 0.832(18) 2.239(19) 3.069(3) 175(5) . O4W H4WA Cl2 0.820(18) 2.36(2) 3.172(3) 169(5) . O5W H5WB Cl1 0.830(18) 2.46(2) 3.284(3) 169(4) . O5W H5WA Cl2 0.837(18) 2.336(18) 3.172(3) 177(4) . O6W H6WA Cl1 0.829(18) 2.36(2) 3.167(3) 165(5) . O6W H6WB O7W 0.836(18) 2.25(2) 3.077(5) 168(4) . O7W H7WB O1W 0.823(18) 2.21(2) 3.023(3) 168(4) . O7W H7WA O3W 0.831(18) 1.92(2) 2.742(4) 170(6) . O8W H8WA O7W 0.840(18) 2.71(4) 3.150(5) 115(4) . O8W H8WB Cl3 0.814(18) 2.56(3) 3.187(3) 134(4) . O9W H9WA Cl2 0.822(18) 2.42(2) 3.220(3) 167(4) . O9W H9WB Cl3 0.822(18) 2.44(2) 3.232(3) 162(5) . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.219 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.074 #============================================================================== data_[Gd.2]Br3 _database_code_depnum_ccdc_archive 'CCDC 606218' #============================================================================== _chemical_name_systematic ; [Gd.DOTAPh]Br~3~ ; _chemical_name_common (Gd.DOTAPh)Br!3$ _chemical_melting_point 'not measured' _chemical_formula_moiety 'C48 H66 Gd N8 O5, 3Br' _chemical_formula_sum 'C48 H66 Br3 Gd N8 O5' _chemical_formula_weight 1232.07 _chemical_absolute_configuration syn 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 19.0018(11) _cell_length_b 19.0018(11) _cell_length_c 14.7698(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5332.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 5778 _cell_measurement_theta_min 2.143 _cell_measurement_theta_max 27.299 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2476 _exptl_absorpt_coefficient_mu 3.541 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1383 _exptl_absorpt_correction_T_max 0.7116 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.0700 -1.00 0.00 0.00 0.0700 0.00 0.00 1.00 0.0600 0.00 0.00 -1.00 0.6000 0.00 1.00 0.00 0.0500 0.00 -1.00 0.00 0.0500 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 61193 _diffrn_reflns_av_R_equivalents 0.1651 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6634 _reflns_number_gt 4674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+16.4803P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(2) _refine_ls_number_reflns 6634 _refine_ls_number_parameters 220 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.827032(12) 0.827032(12) 0.0000 0.02410(9) Uani 1 2 d S C . N1 N 0.8367(3) 0.6892(3) 0.0449(3) 0.0327(12) Uani 1 1 d . C . N2 N 0.7385(3) 0.7882(3) 0.1377(3) 0.0311(11) Uani 1 1 d . C . N3 N 1.0096(3) 0.6819(4) -0.0565(4) 0.0479(15) Uani 1 1 d . . . H3C H 1.0201 0.6397 -0.0404 0.057 Uiso 1 1 calc R A 1 N4 N 0.8807(3) 0.8279(3) 0.2958(4) 0.0445(14) Uani 1 1 d . . . H4C H 0.8589 0.8217 0.3462 0.053 Uiso 1 1 calc R B 1 O1 O 0.9310(2) 0.7703(2) -0.0502(3) 0.0392(11) Uani 1 1 d . . . O2 O 0.8775(2) 0.8268(3) 0.1446(3) 0.0362(10) Uani 1 1 d . . . C1 C 0.8064(5) 0.6761(5) 0.1372(5) 0.044(2) Uani 1 1 d . . . H1A H 0.8386 0.6937 0.1828 0.053 Uiso 1 1 calc R . . H1B H 0.8011 0.6258 0.1463 0.053 Uiso 1 1 calc R . . C2 C 0.7362(4) 0.7112(3) 0.1486(5) 0.043(2) Uani 1 1 d . . . H2A H 0.7036 0.6918 0.1045 0.052 Uiso 1 1 calc R . . H2B H 0.7180 0.7003 0.2083 0.052 Uiso 1 1 calc R . . C3 C 0.6657(4) 0.8137(4) 0.1201(5) 0.0363(18) Uani 1 1 d . . . H3A H 0.6631 0.8636 0.1335 0.044 Uiso 1 1 calc R . . H3B H 0.6333 0.7894 0.1601 0.044 Uiso 1 1 calc R . . C4 C 0.6433(3) 0.8015(4) 0.0225(4) 0.0458(19) Uani 1 1 d . . . H4A H 0.6432 0.7513 0.0105 0.055 Uiso 1 1 calc R . . H4B H 0.5955 0.8185 0.0148 0.055 Uiso 1 1 calc R . . C5 C 0.9122(4) 0.6728(4) 0.0474(5) 0.0430(16) Uani 1 1 d . . . H5A H 0.9188 0.6226 0.0398 0.052 Uiso 1 1 calc R C . H5B H 0.9312 0.6861 0.1059 0.052 Uiso 1 1 calc R . . C6 C 0.9509(4) 0.7111(4) -0.0256(4) 0.0383(16) Uani 1 1 d . C . C7 C 0.7667(3) 0.8221(4) 0.2209(4) 0.0399(15) Uani 1 1 d . . . H7A H 0.7518 0.7956 0.2737 0.048 Uiso 1 1 calc R C . H7B H 0.7480 0.8694 0.2260 0.048 Uiso 1 1 calc R . . C8 C 0.8452(3) 0.8249(3) 0.2176(4) 0.0344(18) Uani 1 1 d . C . C9 C 1.0565(4) 0.7200(5) -0.1171(5) 0.057(2) Uani 0.60 1 d P C 1 H9A H 1.0650 0.7684 -0.0971 0.068 Uiso 0.60 1 calc PR C 1 C10 C 1.0256(6) 0.7164(5) -0.2151(5) 0.0589(13) Uiso 0.60 1 d PG C 1 C11 C 1.0129(6) 0.7784(4) -0.2623(7) 0.0589(13) Uiso 0.60 1 d PG C 1 H11A H 1.0212 0.8216 -0.2348 0.071 Uiso 0.60 1 calc PR C 1 C12 C 0.9877(6) 0.7758(4) -0.3506(6) 0.0589(13) Uiso 0.60 1 d PG C 1 H12A H 0.9791 0.8172 -0.3822 0.071 Uiso 0.60 1 calc PR C 1 C13 C 0.9752(5) 0.7111(5) -0.3917(5) 0.0589(13) Uiso 0.60 1 d PG C 1 H13A H 0.9583 0.7094 -0.4507 0.071 Uiso 0.60 1 calc PR C 1 C14 C 0.9879(6) 0.6491(4) -0.3445(6) 0.0589(13) Uiso 0.60 1 d PG C 1 H14A H 0.9795 0.6059 -0.3720 0.071 Uiso 0.60 1 calc PR C 1 C15 C 1.0131(6) 0.6518(4) -0.2562(6) 0.0589(13) Uiso 0.60 1 d PG C 1 H15A H 1.0216 0.6103 -0.2246 0.071 Uiso 0.60 1 calc PR C 1 C16 C 1.1250(7) 0.6732(8) -0.1139(10) 0.052(3) Uiso 0.60 1 d P C 1 H16A H 1.1377 0.6644 -0.0520 0.078 Uiso 0.60 1 calc PR C 1 H16B H 1.1628 0.6974 -0.1438 0.078 Uiso 0.60 1 calc PR C 1 H16C H 1.1163 0.6292 -0.1439 0.078 Uiso 0.60 1 calc PR C 1 C9A C 1.0565(4) 0.7200(5) -0.1171(5) 0.057(2) Uani 0.40 1 d P C 2 H9B H 1.0546 0.7673 -0.0908 0.068 Uiso 0.40 1 calc PR C 2 C10A C 1.0301(8) 0.7334(7) -0.2064(8) 0.0589(13) Uiso 0.40 1 d PG C 2 C11A C 1.0247(8) 0.8007(6) -0.2425(9) 0.0589(13) Uiso 0.40 1 d PG C 2 H11B H 1.0391 0.8394 -0.2086 0.071 Uiso 0.40 1 calc PR C 2 C12A C 0.9979(8) 0.8102(6) -0.3292(9) 0.0589(13) Uiso 0.40 1 d PG C 2 H12B H 0.9943 0.8553 -0.3533 0.071 Uiso 0.40 1 calc PR C 2 C13A C 0.9764(7) 0.7524(7) -0.3798(7) 0.0589(13) Uiso 0.40 1 d PG C 2 H13B H 0.9584 0.7588 -0.4377 0.071 Uiso 0.40 1 calc PR C 2 C14A C 0.9818(8) 0.6850(6) -0.3437(9) 0.0589(13) Uiso 0.40 1 d PG C 2 H14B H 0.9675 0.6464 -0.3775 0.071 Uiso 0.40 1 calc PR C 2 C15A C 1.0087(8) 0.6755(6) -0.2570(9) 0.0589(13) Uiso 0.40 1 d PG C 2 H15B H 1.0123 0.6305 -0.2328 0.071 Uiso 0.40 1 calc PR C 2 C16A C 1.1318(11) 0.7066(12) -0.1156(15) 0.052(3) Uiso 0.40 1 d P C 2 H16D H 1.1490 0.7110 -0.0547 0.078 Uiso 0.40 1 calc PR C 2 H16E H 1.1553 0.7402 -0.1537 0.078 Uiso 0.40 1 calc PR C 2 H16F H 1.1409 0.6599 -0.1374 0.078 Uiso 0.40 1 calc PR C 2 C17 C 0.9572(4) 0.8416(4) 0.2958(5) 0.0485(19) Uani 0.60 1 d P D 1 H17A H 0.9659 0.8858 0.2635 0.058 Uiso 0.60 1 calc PR D 1 C18 C 1.0006(6) 0.7837(4) 0.2512(7) 0.0572(12) Uiso 0.60 1 d PG D 1 C19 C 1.0500(6) 0.8045(4) 0.1872(7) 0.0572(12) Uiso 0.60 1 d PG D 1 H19A H 1.0555 0.8519 0.1734 0.069 Uiso 0.60 1 calc PR D 1 C20 C 1.0911(5) 0.7543(5) 0.1437(6) 0.0572(12) Uiso 0.60 1 d PG D 1 H20A H 1.1242 0.7682 0.1009 0.069 Uiso 0.60 1 calc PR D 1 C21 C 1.0829(5) 0.6834(4) 0.1644(7) 0.0572(12) Uiso 0.60 1 d PG D 1 H21A H 1.1105 0.6499 0.1353 0.069 Uiso 0.60 1 calc PR D 1 C22 C 1.0335(5) 0.6627(4) 0.2284(7) 0.0572(12) Uiso 0.60 1 d PG D 1 H22A H 1.0280 0.6153 0.2422 0.069 Uiso 0.60 1 calc PR D 1 C23 C 0.9923(5) 0.7128(5) 0.2719(7) 0.0572(12) Uiso 0.60 1 d PG D 1 H23A H 0.9593 0.6990 0.3147 0.069 Uiso 0.60 1 calc PR D 1 C24 C 0.9834(9) 0.8495(8) 0.3923(11) 0.055(3) Uiso 0.60 1 d P D 1 H24A H 0.9596 0.8882 0.4208 0.083 Uiso 0.60 1 calc PR D 1 H24B H 1.0331 0.8582 0.3919 0.083 Uiso 0.60 1 calc PR D 1 H24C H 0.9739 0.8070 0.4254 0.083 Uiso 0.60 1 calc PR D 1 C17A C 0.9572(4) 0.8416(4) 0.2958(5) 0.0485(19) Uani 0.40 1 d P D 2 H17B H 0.9654 0.8778 0.2496 0.058 Uiso 0.40 1 calc PR D 2 C18A C 0.9957(8) 0.7775(6) 0.2647(10) 0.0572(12) Uiso 0.40 1 d PG D 2 C19A C 1.0425(8) 0.7818(6) 0.1926(10) 0.0572(12) Uiso 0.40 1 d PG D 2 H19B H 1.0534 0.8253 0.1675 0.069 Uiso 0.40 1 calc PR D 2 C20A C 1.0731(7) 0.7210(7) 0.1580(8) 0.0572(12) Uiso 0.40 1 d PG D 2 H20B H 1.1044 0.7239 0.1098 0.069 Uiso 0.40 1 calc PR D 2 C21A C 1.0568(7) 0.6559(6) 0.1956(9) 0.0572(12) Uiso 0.40 1 d PG D 2 H21B H 1.0773 0.6153 0.1725 0.069 Uiso 0.40 1 calc PR D 2 C22A C 1.0100(8) 0.6516(6) 0.2677(9) 0.0572(12) Uiso 0.40 1 d PG D 2 H22B H 0.9991 0.6081 0.2928 0.069 Uiso 0.40 1 calc PR D 2 C23A C 0.9794(7) 0.7124(7) 0.3022(9) 0.0572(12) Uiso 0.40 1 d PG D 2 H23B H 0.9481 0.7095 0.3505 0.069 Uiso 0.40 1 calc PR D 2 C24A C 0.9783(14) 0.8757(12) 0.3892(17) 0.055(3) Uiso 0.40 1 d P D 2 H24D H 0.9581 0.9219 0.3936 0.083 Uiso 0.40 1 calc PR D 2 H24E H 1.0286 0.8791 0.3930 0.083 Uiso 0.40 1 calc PR D 2 H24F H 0.9611 0.8469 0.4378 0.083 Uiso 0.40 1 calc PR D 2 O1W O 0.91559(19) 0.91559(19) 0.0000 0.0439(14) Uani 1 2 d SD . . H1W H 0.927(5) 0.941(4) 0.049(3) 0.07(3) Uiso 1 1 d D . . Br1 Br 1.0000 1.0000 0.16239(9) 0.1273(8) Uani 1 2 d S . . Br2 Br 0.80288(4) 0.80288(4) 0.5000 0.0601(3) Uani 1 2 d S . . Br3 Br 1.0000 0.5000 -0.03921(13) 0.0972(6) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02695(11) 0.02695(11) 0.01840(15) 0.0003(2) -0.0003(2) 0.00170(14) N1 0.042(3) 0.032(3) 0.024(3) 0.005(2) 0.003(2) 0.006(2) N2 0.030(3) 0.039(3) 0.024(3) 0.000(2) 0.000(2) -0.001(2) N3 0.046(3) 0.061(4) 0.037(3) 0.004(3) 0.002(3) 0.017(3) N4 0.048(3) 0.068(4) 0.017(3) -0.002(3) -0.006(2) -0.010(3) O1 0.038(3) 0.044(3) 0.035(3) 0.003(2) 0.008(2) 0.004(2) O2 0.035(2) 0.052(3) 0.022(2) 0.004(2) -0.0007(18) -0.004(2) C1 0.058(5) 0.037(4) 0.037(4) 0.010(4) 0.014(4) 0.002(4) C2 0.050(4) 0.042(4) 0.038(4) 0.006(3) 0.011(3) -0.010(4) C3 0.028(4) 0.052(5) 0.030(4) -0.007(3) 0.004(3) 0.003(4) C4 0.028(3) 0.070(5) 0.040(5) 0.001(3) -0.002(3) -0.009(3) C5 0.047(4) 0.045(4) 0.037(4) 0.008(3) 0.006(3) 0.021(4) C6 0.040(4) 0.046(4) 0.029(4) 0.002(3) -0.001(3) 0.012(3) C7 0.041(4) 0.058(4) 0.021(3) -0.004(3) 0.001(3) 0.008(3) C8 0.041(4) 0.040(4) 0.022(3) 0.005(3) -0.001(2) -0.001(3) C9 0.043(4) 0.086(6) 0.041(5) -0.007(4) 0.012(3) 0.013(4) C9A 0.043(4) 0.086(6) 0.041(5) -0.007(4) 0.012(3) 0.013(4) C17 0.047(4) 0.072(6) 0.026(4) 0.001(3) -0.004(3) -0.011(4) C17A 0.047(4) 0.072(6) 0.026(4) 0.001(3) -0.004(3) -0.011(4) O1W 0.051(2) 0.051(2) 0.029(3) 0.011(4) -0.011(4) -0.025(3) Br1 0.231(3) 0.0961(13) 0.0547(8) 0.000 0.000 -0.0995(13) Br2 0.0718(4) 0.0718(4) 0.0368(5) -0.0069(7) 0.0069(7) -0.0040(5) Br3 0.1254(14) 0.0594(9) 0.1066(13) 0.000 0.000 0.0253(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2 2.341(4) 7 ? Gd1 O2 2.341(4) . ? Gd1 O1 2.369(4) . ? Gd1 O1 2.369(4) 7 ? Gd1 O1W 2.380(5) . ? Gd1 N1 2.708(5) 7 ? Gd1 N1 2.708(5) . ? Gd1 N2 2.740(5) 7 ? Gd1 N2 2.740(5) . ? N1 C5 1.467(8) . ? N1 C4 1.483(8) 7 ? N1 C1 1.500(9) . ? N2 C2 1.472(8) . ? N2 C7 1.487(8) . ? N2 C3 1.490(9) . ? N3 C6 1.326(8) . ? N3 C9 1.455(10) . ? N3 H3C 0.8600 . ? N4 C8 1.340(8) . ? N4 C17 1.477(9) . ? N4 H4C 0.8600 . ? O1 C6 1.241(8) . ? O2 C8 1.240(7) . ? C1 C2 1.501(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.520(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N1 1.483(8) 7 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.494(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 C8 1.494(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.564(11) . ? C9 C16 1.578(16) . ? C9 H9A 0.9800 . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C10A C11A 1.3900 . ? C10A C15A 1.3900 . ? C11A C12A 1.3900 . ? C11A H11B 0.9300 . ? C12A C13A 1.3900 . ? C12A H12B 0.9300 . ? C13A C14A 1.3900 . ? C13A H13B 0.9300 . ? C14A C15A 1.3900 . ? C14A H14B 0.9300 . ? C15A H15B 0.9300 . ? C16A H16D 0.9600 . ? C16A H16E 0.9600 . ? C16A H16F 0.9600 . ? C17 C24 1.518(18) . ? C17 C18 1.523(10) . ? C17 H17A 0.9800 . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C19 H19A 0.9300 . ? C20 C21 1.3900 . ? C20 H20A 0.9300 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C18A C19A 1.3900 . ? C18A C23A 1.3900 . ? C19A C20A 1.3900 . ? C19A H19B 0.9300 . ? C20A C21A 1.3900 . ? C20A H20B 0.9300 . ? C21A C22A 1.3900 . ? C21A H21B 0.9300 . ? C22A C23A 1.3900 . ? C22A H22B 0.9300 . ? C23A H23B 0.9300 . ? C24A H24D 0.9600 . ? C24A H24E 0.9600 . ? C24A H24F 0.9600 . ? O1W H1W 0.898(10) . ? 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 O2 Gd1 O2 146.5(2) 7 . ? O2 Gd1 O1 84.43(16) 7 . ? O2 Gd1 O1 86.74(16) . . ? O2 Gd1 O1 86.74(16) 7 7 ? O2 Gd1 O1 84.43(16) . 7 ? O1 Gd1 O1 149.0(2) . 7 ? O2 Gd1 O1W 73.27(11) 7 . ? O2 Gd1 O1W 73.27(11) . . ? O1 Gd1 O1W 74.49(11) . . ? O1 Gd1 O1W 74.49(11) 7 . ? O2 Gd1 N1 75.32(16) 7 7 ? O2 Gd1 N1 128.28(15) . 7 ? O1 Gd1 N1 139.51(16) . 7 ? O1 Gd1 N1 65.14(15) 7 7 ? O1W Gd1 N1 129.48(11) . 7 ? O2 Gd1 N1 128.28(15) 7 . ? O2 Gd1 N1 75.32(16) . . ? O1 Gd1 N1 65.14(15) . . ? O1 Gd1 N1 139.51(16) 7 . ? O1W Gd1 N1 129.48(11) . . ? N1 Gd1 N1 101.0(2) 7 . ? O2 Gd1 N2 64.75(15) 7 7 ? O2 Gd1 N2 141.83(16) . 7 ? O1 Gd1 N2 73.33(16) . 7 ? O1 Gd1 N2 128.37(16) 7 7 ? O1W Gd1 N2 128.65(11) . 7 ? N1 Gd1 N2 66.37(15) 7 7 ? N1 Gd1 N2 66.84(15) . 7 ? O2 Gd1 N2 141.83(16) 7 . ? O2 Gd1 N2 64.75(15) . . ? O1 Gd1 N2 128.37(16) . . ? O1 Gd1 N2 73.33(16) 7 . ? O1W Gd1 N2 128.65(11) . . ? N1 Gd1 N2 66.84(15) 7 . ? N1 Gd1 N2 66.37(15) . . ? N2 Gd1 N2 102.7(2) 7 . ? C5 N1 C4 109.4(5) . 7 ? C5 N1 C1 108.5(5) . . ? C4 N1 C1 109.8(6) 7 . ? C5 N1 Gd1 106.1(4) . . ? C4 N1 Gd1 112.0(4) 7 . ? C1 N1 Gd1 110.9(4) . . ? C2 N2 C7 110.6(5) . . ? C2 N2 C3 108.3(5) . . ? C7 N2 C3 109.7(5) . . ? C2 N2 Gd1 111.6(4) . . ? C7 N2 Gd1 106.0(4) . . ? C3 N2 Gd1 110.7(4) . . ? C6 N3 C9 121.2(7) . . ? C6 N3 H3C 119.4 . . ? C9 N3 H3C 119.4 . . ? C8 N4 C17 120.2(6) . . ? C8 N4 H4C 119.9 . . ? C17 N4 H4C 119.9 . . ? C6 O1 Gd1 125.2(4) . . ? C8 O2 Gd1 126.2(4) . . ? N1 C1 C2 111.7(6) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 113.7(6) . . ? N2 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? N2 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? N2 C3 C4 112.1(6) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N1 C4 C3 113.8(6) 7 . ? N1 C4 H4A 108.8 7 . ? C3 C4 H4A 108.8 . . ? N1 C4 H4B 108.8 7 . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N1 C5 C6 111.1(5) . . ? N1 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N1 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? O1 C6 N3 122.4(7) . . ? O1 C6 C5 120.1(6) . . ? N3 C6 C5 117.4(6) . . ? N2 C7 C8 110.3(5) . . ? N2 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? O2 C8 N4 119.9(6) . . ? O2 C8 C7 121.6(5) . . ? N4 C8 C7 118.5(6) . . ? N3 C9 C10 108.6(7) . . ? N3 C9 C16 101.9(8) . . ? C10 C9 C16 108.2(8) . . ? N3 C9 H9A 112.5 . . ? C10 C9 H9A 112.5 . . ? C16 C9 H9A 112.5 . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 119.5(7) . . ? C15 C10 C9 120.5(7) . . ? C10 C11 C12 120.0 . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 H15A 120.0 . . ? C10 C15 H15A 120.0 . . ? C11A C10A C15A 120.0 . . ? C10A C11A C12A 120.0 . . ? C10A C11A H11B 120.0 . . ? C12A C11A H11B 120.0 . . ? C11A C12A C13A 120.0 . . ? C11A C12A H12B 120.0 . . ? C13A C12A H12B 120.0 . . ? C14A C13A C12A 120.0 . . ? C14A C13A H13B 120.0 . . ? C12A C13A H13B 120.0 . . ? C13A C14A C15A 120.0 . . ? C13A C14A H14B 120.0 . . ? C15A C14A H14B 120.0 . . ? C14A C15A C10A 120.0 . . ? C14A C15A H15B 120.0 . . ? C10A C15A H15B 120.0 . . ? H16D C16A H16E 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? N4 C17 C24 109.8(8) . . ? N4 C17 C18 113.9(8) . . ? C24 C17 C18 107.4(9) . . ? N4 C17 H17A 108.5 . . ? C24 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? C19 C18 C23 120.0 . . ? C19 C18 C17 117.0(7) . . ? C23 C18 C17 123.0(7) . . ? C18 C19 C20 120.0 . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 H23A 120.0 . . ? C18 C23 H23A 120.0 . . ? C19A C18A C23A 120.0 . . ? C20A C19A C18A 120.0 . . ? C20A C19A H19B 120.0 . . ? C18A C19A H19B 120.0 . . ? C19A C20A C21A 120.0 . . ? C19A C20A H20B 120.0 . . ? C21A C20A H20B 120.0 . . ? C22A C21A C20A 120.0 . . ? C22A C21A H21B 120.0 . . ? C20A C21A H21B 120.0 . . ? C21A C22A C23A 120.0 . . ? C21A C22A H22B 120.0 . . ? C23A C22A H22B 120.0 . . ? C22A C23A C18A 120.0 . . ? C22A C23A H23B 120.0 . . ? C18A C23A H23B 120.0 . . ? H24D C24A H24E 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? Gd1 O1W H1W 123(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Gd1 N1 C5 85.4(4) 7 . . . ? O2 Gd1 N1 C5 -67.7(4) . . . . ? O1 Gd1 N1 C5 25.5(4) . . . . ? O1 Gd1 N1 C5 -130.2(4) 7 . . . ? O1W Gd1 N1 C5 -14.7(4) . . . . ? N1 Gd1 N1 C5 165.3(4) 7 . . . ? N2 Gd1 N1 C5 107.2(4) 7 . . . ? N2 Gd1 N1 C5 -136.2(4) . . . . ? O2 Gd1 N1 C4 -33.9(5) 7 . . 7 ? O2 Gd1 N1 C4 173.0(4) . . . 7 ? O1 Gd1 N1 C4 -93.8(4) . . . 7 ? O1 Gd1 N1 C4 110.5(4) 7 . . 7 ? O1W Gd1 N1 C4 -134.0(4) . . . 7 ? N1 Gd1 N1 C4 46.0(4) 7 . . 7 ? N2 Gd1 N1 C4 -12.1(4) 7 . . 7 ? N2 Gd1 N1 C4 104.5(4) . . . 7 ? O2 Gd1 N1 C1 -156.9(5) 7 . . . ? O2 Gd1 N1 C1 50.0(5) . . . . ? O1 Gd1 N1 C1 143.2(5) . . . . ? O1 Gd1 N1 C1 -12.5(6) 7 . . . ? O1W Gd1 N1 C1 103.0(5) . . . . ? N1 Gd1 N1 C1 -77.0(5) 7 . . . ? N2 Gd1 N1 C1 -135.1(5) 7 . . . ? N2 Gd1 N1 C1 -18.5(5) . . . . ? O2 Gd1 N2 C2 112.2(4) 7 . . . ? O2 Gd1 N2 C2 -94.6(4) . . . . ? O1 Gd1 N2 C2 -31.6(5) . . . . ? O1 Gd1 N2 C2 173.7(4) 7 . . . ? O1W Gd1 N2 C2 -132.9(4) . . . . ? N1 Gd1 N2 C2 104.2(4) 7 . . . ? N1 Gd1 N2 C2 -10.3(4) . . . . ? N2 Gd1 N2 C2 47.1(4) 7 . . . ? O2 Gd1 N2 C7 -127.3(4) 7 . . . ? O2 Gd1 N2 C7 25.8(4) . . . . ? O1 Gd1 N2 C7 88.9(4) . . . . ? O1 Gd1 N2 C7 -65.8(4) 7 . . . ? O1W Gd1 N2 C7 -12.5(5) . . . . ? N1 Gd1 N2 C7 -135.4(4) 7 . . . ? N1 Gd1 N2 C7 110.1(4) . . . . ? N2 Gd1 N2 C7 167.5(5) 7 . . . ? O2 Gd1 N2 C3 -8.5(6) 7 . . . ? O2 Gd1 N2 C3 144.7(5) . . . . ? O1 Gd1 N2 C3 -152.2(4) . . . . ? O1 Gd1 N2 C3 53.1(4) 7 . . . ? O1W Gd1 N2 C3 106.4(4) . . . . ? N1 Gd1 N2 C3 -16.5(4) 7 . . . ? N1 Gd1 N2 C3 -131.0(5) . . . . ? N2 Gd1 N2 C3 -73.6(4) 7 . . . ? O2 Gd1 O1 C6 -148.6(5) 7 . . . ? O2 Gd1 O1 C6 63.8(5) . . . . ? O1 Gd1 O1 C6 137.3(5) 7 . . . ? O1W Gd1 O1 C6 137.3(5) . . . . ? N1 Gd1 O1 C6 -89.0(6) 7 . . . ? N1 Gd1 O1 C6 -11.6(5) . . . . ? N2 Gd1 O1 C6 -83.3(5) 7 . . . ? N2 Gd1 O1 C6 9.9(6) . . . . ? O2 Gd1 O2 C8 134.3(5) 7 . . . ? O1 Gd1 O2 C8 -150.9(5) . . . . ? O1 Gd1 O2 C8 58.8(5) 7 . . . ? O1W Gd1 O2 C8 134.3(5) . . . . ? N1 Gd1 O2 C8 6.8(6) 7 . . . ? N1 Gd1 O2 C8 -85.8(5) . . . . ? N2 Gd1 O2 C8 -93.4(6) 7 . . . ? N2 Gd1 O2 C8 -15.3(5) . . . . ? C5 N1 C1 C2 163.0(6) . . . . ? C4 N1 C1 C2 -77.5(8) 7 . . . ? Gd1 N1 C1 C2 46.7(7) . . . . ? C7 N2 C2 C1 -78.2(7) . . . . ? C3 N2 C2 C1 161.6(6) . . . . ? Gd1 N2 C2 C1 39.5(7) . . . . ? N1 C1 C2 N2 -60.0(9) . . . . ? C2 N2 C3 C4 -78.6(7) . . . . ? C7 N2 C3 C4 160.6(6) . . . . ? Gd1 N2 C3 C4 44.0(7) . . . . ? N2 C3 C4 N1 -59.2(9) . . . 7 ? C4 N1 C5 C6 83.8(7) 7 . . . ? C1 N1 C5 C6 -156.5(6) . . . . ? Gd1 N1 C5 C6 -37.2(6) . . . . ? Gd1 O1 C6 N3 179.7(5) . . . . ? Gd1 O1 C6 C5 -6.0(9) . . . . ? C9 N3 C6 O1 4.0(11) . . . . ? C9 N3 C6 C5 -170.5(7) . . . . ? N1 C5 C6 O1 32.8(9) . . . . ? N1 C5 C6 N3 -152.7(6) . . . . ? C2 N2 C7 C8 86.6(7) . . . . ? C3 N2 C7 C8 -154.0(6) . . . . ? Gd1 N2 C7 C8 -34.5(6) . . . . ? Gd1 O2 C8 N4 -177.3(5) . . . . ? Gd1 O2 C8 C7 0.4(9) . . . . ? C17 N4 C8 O2 7.1(10) . . . . ? C17 N4 C8 C7 -170.6(7) . . . . ? N2 C7 C8 O2 27.4(9) . . . . ? N2 C7 C8 N4 -154.9(6) . . . . ? C6 N3 C9 C10 -79.8(9) . . . . ? C6 N3 C9 C16 166.1(8) . . . . ? N3 C9 C10 C11 124.4(8) . . . . ? C16 C9 C10 C11 -125.7(9) . . . . ? N3 C9 C10 C15 -57.7(9) . . . . ? C16 C9 C10 C15 52.2(11) . . . . ? C15 C10 C11 C12 0.0 . . . . ? C9 C10 C11 C12 177.9(9) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? C9 C10 C15 C14 -177.9(10) . . . . ? C15A C10A C11A C12A 0.0 . . . . ? C10A C11A C12A C13A 0.0 . . . . ? C11A C12A C13A C14A 0.0 . . . . ? C12A C13A C14A C15A 0.0 . . . . ? C13A C14A C15A C10A 0.0 . . . . ? C11A C10A C15A C14A 0.0 . . . . ? C8 N4 C17 C24 174.5(8) . . . . ? C8 N4 C17 C18 -65.0(10) . . . . ? N4 C17 C18 C19 130.7(7) . . . . ? C24 C17 C18 C19 -107.4(9) . . . . ? N4 C17 C18 C23 -49.1(10) . . . . ? C24 C17 C18 C23 72.8(11) . . . . ? C23 C18 C19 C20 0.0 . . . . ? C17 C18 C19 C20 -179.8(10) . . . . ? C18 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C18 0.0 . . . . ? C19 C18 C23 C22 0.0 . . . . ? C17 C18 C23 C22 179.8(11) . . . . ? C23A C18A C19A C20A 0.0 . . . . ? C18A C19A C20A C21A 0.0 . . . . ? C19A C20A C21A C22A 0.0 . . . . ? C20A C21A C22A C23A 0.0 . . . . ? C21A C22A C23A C18A 0.0 . . . . ? C19A C18A C23A C22A 0.0 . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W Br1 0.898(10) 2.45(3) 3.301(4) 159(8) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.396 _refine_diff_density_min -1.348 _refine_diff_density_rms 0.123 #============================================================================== data_[Gd.2]I3 _database_code_depnum_ccdc_archive 'CCDC 606219' #============================================================================== _chemical_name_systematic ; [Gd.DOTAPh]Br~3~ ; _chemical_name_common (Gd.DOTAPh)Br!3$ _chemical_melting_point 'not measured' _chemical_formula_moiety 'C48 H66 Gd N8 O5, 3I' _chemical_formula_sum 'C48 H66 Gd I3 N8 O5' _chemical_formula_weight 1373.04 _chemical_absolute_configuration syn 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 19.3897(13) _cell_length_b 19.3897(13) _cell_length_c 14.8981(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5601.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 7761 _cell_measurement_theta_min 3.448 _cell_measurement_theta_max 26.730 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2692 _exptl_absorpt_coefficient_mu 2.885 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4883 _exptl_absorpt_correction_T_max 0.6247 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 1.00 0.00 0.0900 -1.00 -1.00 0.00 0.0900 1.00 1.00 0.00 0.0900 -1.00 -1.00 0.00 0.0900 -1.00 0.00 -1.00 0.1200 1.00 0.00 -1.00 0.1200 0.00 -1.00 -1.00 0.1200 0.00 1.00 -1.00 0.1200 0.00 0.00 1.00 0.1500 0.00 0.00 -1.00 0.1500 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 38190 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.03 _reflns_number_total 5882 _reflns_number_gt 4830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(15) _refine_ls_number_reflns 5882 _refine_ls_number_parameters 255 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.176606(8) 0.176606(8) 0.0000 0.03005(7) Uani 1 2 d S C . N1 N 0.31162(17) 0.16526(18) 0.0406(2) 0.0389(8) Uani 1 1 d . C . N2 N 0.21554(18) 0.26074(17) 0.1362(2) 0.0382(8) Uani 1 1 d . C . N3 N 0.3131(2) -0.0038(2) -0.0616(2) 0.0551(10) Uani 1 1 d . . . H3C H 0.3543 -0.0149 -0.0459 0.066 Uiso 1 1 calc R A 1 N4 N 0.1819(2) 0.1190(2) 0.2905(2) 0.0550(10) Uani 1 1 d . . . H4A H 0.1885 0.1404 0.3404 0.066 Uiso 1 1 calc R B 1 O1 O 0.22959(16) 0.07539(15) -0.05509(19) 0.0439(7) Uani 1 1 d . . . O2 O 0.17963(16) 0.12376(15) 0.14095(16) 0.0415(7) Uani 1 1 d . . . C1 C 0.3264(3) 0.1946(3) 0.1315(3) 0.0428(12) Uani 1 1 d . . . H1A H 0.3759 0.2000 0.1387 0.051 Uiso 1 1 calc R . . H1B H 0.3103 0.1628 0.1772 0.051 Uiso 1 1 calc R . . C2 C 0.2919(2) 0.2637(2) 0.1444(3) 0.0490(13) Uani 1 1 d . . . H2A H 0.3037 0.2813 0.2034 0.059 Uiso 1 1 calc R . . H2B H 0.3097 0.2958 0.1002 0.059 Uiso 1 1 calc R . . C3 C 0.1886(3) 0.3317(3) 0.1228(3) 0.0475(13) Uani 1 1 d . . . H3A H 0.2120 0.3630 0.1635 0.057 Uiso 1 1 calc R . . H3B H 0.1398 0.3326 0.1370 0.057 Uiso 1 1 calc R . . C4 C 0.1991(3) 0.3561(2) 0.0271(3) 0.0514(12) Uani 1 1 d . . . H4B H 0.1811 0.4026 0.0214 0.062 Uiso 1 1 calc R . . H4C H 0.2481 0.3578 0.0145 0.062 Uiso 1 1 calc R . . C5 C 0.3258(3) 0.0905(2) 0.0429(3) 0.0497(11) Uani 1 1 d . . . H5A H 0.3129 0.0721 0.1011 0.060 Uiso 1 1 calc R C . H5B H 0.3748 0.0827 0.0346 0.060 Uiso 1 1 calc R . . C6 C 0.2863(2) 0.0535(2) -0.0294(3) 0.0427(10) Uani 1 1 d . C . C7 C 0.1844(3) 0.2306(2) 0.2191(3) 0.0450(10) Uani 1 1 d . . . H7A H 0.2111 0.2449 0.2709 0.054 Uiso 1 1 calc R C . H7B H 0.1378 0.2481 0.2263 0.054 Uiso 1 1 calc R . . C8 C 0.1825(2) 0.1540(2) 0.2151(3) 0.0426(11) Uani 1 1 d . C . C9 C 0.2761(4) -0.0491(3) -0.1227(3) 0.0686(17) Uani 0.60 1 d PD C 1 H9A H 0.2272 -0.0471 -0.1063 0.082 Uiso 0.60 1 calc PR C 1 C10 C 0.2826(3) -0.0204(4) -0.2200(4) 0.052(2) Uiso 0.60 1 d PG C 1 C11 C 0.3470(3) -0.0120(4) -0.2596(4) 0.064(3) Uiso 0.60 1 d PG C 1 H11A H 0.3868 -0.0217 -0.2271 0.077 Uiso 0.60 1 calc PR C 1 C12 C 0.3519(3) 0.0108(4) -0.3478(4) 0.076(3) Uiso 0.60 1 d PG C 1 H12A H 0.3950 0.0163 -0.3743 0.092 Uiso 0.60 1 calc PR C 1 C13 C 0.2925(4) 0.0252(4) -0.3965(4) 0.092(3) Uiso 0.60 1 d PG C 1 H13A H 0.2958 0.0405 -0.4555 0.110 Uiso 0.60 1 calc PR C 1 C14 C 0.2281(3) 0.0169(4) -0.3569(5) 0.088(4) Uiso 0.60 1 d PG C 1 H14A H 0.1883 0.0266 -0.3894 0.106 Uiso 0.60 1 calc PR C 1 C15 C 0.2232(3) -0.0059(4) -0.2687(5) 0.077(3) Uiso 0.60 1 d PG C 1 H15A H 0.1801 -0.0115 -0.2422 0.092 Uiso 0.60 1 calc PR C 1 C16 C 0.2972(6) -0.1228(5) -0.1193(8) 0.073(3) Uiso 0.60 1 d PD C 1 H16A H 0.3068 -0.1356 -0.0583 0.110 Uiso 0.60 1 calc PR C 1 H16B H 0.3379 -0.1293 -0.1551 0.110 Uiso 0.60 1 calc PR C 1 H16C H 0.2606 -0.1511 -0.1423 0.110 Uiso 0.60 1 calc PR C 1 C9A C 0.2761(4) -0.0491(3) -0.1227(3) 0.0686(17) Uani 0.40 1 d PD C 2 H9B H 0.2337 -0.0643 -0.0929 0.082 Uiso 0.40 1 calc PR C 2 C10A C 0.2592(5) -0.0265(4) -0.2077(5) 0.043(3) Uiso 0.40 1 d PG C 2 C11A C 0.3131(4) -0.0028(5) -0.2609(6) 0.052(3) Uiso 0.40 1 d PG C 2 H11B H 0.3581 -0.0040 -0.2392 0.063 Uiso 0.40 1 calc PR C 2 C12A C 0.2998(6) 0.0227(6) -0.3463(6) 0.110(7) Uiso 0.40 1 d PG C 2 H12B H 0.3359 0.0386 -0.3819 0.132 Uiso 0.40 1 calc PR C 2 C13A C 0.2326(6) 0.0245(7) -0.3787(6) 0.125(10) Uiso 0.40 1 d PG C 2 H13B H 0.2237 0.0416 -0.4358 0.150 Uiso 0.40 1 calc PR C 2 C14A C 0.1787(5) 0.0008(7) -0.3255(7) 0.128(7) Uiso 0.40 1 d PG C 2 H14B H 0.1337 0.0020 -0.3471 0.153 Uiso 0.40 1 calc PR C 2 C15A C 0.1919(4) -0.0247(6) -0.2400(7) 0.098(6) Uiso 0.40 1 d PG C 2 H15B H 0.1559 -0.0405 -0.2045 0.118 Uiso 0.40 1 calc PR C 2 C16A C 0.3311(8) -0.1131(6) -0.1207(10) 0.057(3) Uiso 0.40 1 d PD C 2 H16D H 0.3469 -0.1202 -0.0604 0.085 Uiso 0.40 1 calc PR C 2 H16E H 0.3697 -0.1024 -0.1586 0.085 Uiso 0.40 1 calc PR C 2 H16F H 0.3090 -0.1542 -0.1420 0.085 Uiso 0.40 1 calc PR C 2 C17 C 0.1699(3) 0.0436(2) 0.2914(3) 0.0594(14) Uani 0.60 1 d PD D 1 H17A H 0.1278 0.0355 0.2566 0.071 Uiso 0.60 1 calc PR D 1 C18 C 0.2259(3) 0.0007(3) 0.2479(4) 0.055(4) Uiso 0.60 1 d PGD D 1 C19 C 0.2056(3) -0.0487(4) 0.1856(5) 0.066(3) Uiso 0.60 1 d PGD D 1 H19A H 0.1591 -0.0544 0.1722 0.079 Uiso 0.60 1 calc PR D 1 C20 C 0.2548(4) -0.0896(4) 0.1435(5) 0.086(3) Uiso 0.60 1 d PGD D 1 H20A H 0.2412 -0.1226 0.1019 0.103 Uiso 0.60 1 calc PR D 1 C21 C 0.3243(3) -0.0810(3) 0.1635(5) 0.068(2) Uiso 0.60 1 d PGD D 1 H21A H 0.3572 -0.1084 0.1353 0.082 Uiso 0.60 1 calc PR D 1 C22 C 0.3446(3) -0.0316(4) 0.2258(5) 0.067(3) Uiso 0.60 1 d PGD D 1 H22A H 0.3911 -0.0259 0.2392 0.080 Uiso 0.60 1 calc PR D 1 C23 C 0.2954(4) 0.0093(3) 0.2679(4) 0.057(2) Uiso 0.60 1 d PGD D 1 H23A H 0.3090 0.0423 0.3095 0.068 Uiso 0.60 1 calc PR D 1 C24 C 0.1536(5) 0.0217(3) 0.3893(4) 0.098(3) Uani 0.60 1 d P D 1 H24A H 0.1567 -0.0275 0.3944 0.147 Uiso 1 1 calc R D 1 H24B H 0.1078 0.0363 0.4048 0.147 Uiso 1 1 calc R D 1 H24C H 0.1862 0.0428 0.4294 0.147 Uiso 1 1 calc R D 1 C17A C 0.1699(3) 0.0436(2) 0.2914(3) 0.0594(14) Uani 0.40 1 d PD D 2 H17B H 0.1301 0.0329 0.2533 0.071 Uiso 0.40 1 calc PR D 2 C18A C 0.2313(5) 0.0074(4) 0.2561(6) 0.051(6) Uiso 0.40 1 d PGD D 2 C19A C 0.2252(4) -0.0394(5) 0.1858(6) 0.072(5) Uiso 0.40 1 d PGD D 2 H19B H 0.1822 -0.0483 0.1607 0.086 Uiso 0.40 1 calc PR D 2 C20A C 0.2834(5) -0.0728(5) 0.1532(6) 0.072(4) Uiso 0.40 1 d PGD D 2 H20B H 0.2794 -0.1042 0.1062 0.086 Uiso 0.40 1 calc PR D 2 C21A C 0.3477(5) -0.0595(6) 0.1907(7) 0.069(4) Uiso 0.40 1 d PGD D 2 H21B H 0.3866 -0.0819 0.1688 0.082 Uiso 0.40 1 calc PR D 2 C22A C 0.3537(5) -0.0127(6) 0.2609(7) 0.091(6) Uiso 0.40 1 d PGD D 2 H22B H 0.3967 -0.0037 0.2860 0.109 Uiso 0.40 1 calc PR D 2 C23A C 0.2955(6) 0.0208(5) 0.2936(6) 0.072(5) Uiso 0.40 1 d PGD D 2 H23B H 0.2996 0.0521 0.3406 0.086 Uiso 0.40 1 calc PR D 2 C24A C 0.1536(5) 0.0217(3) 0.3893(4) 0.098(3) Uani 0.40 1 d P D 2 O1W O 0.08977(13) 0.08977(13) 0.0000 0.0526(9) Uani 1 2 d SD . . H1W H 0.058(2) 0.076(3) 0.040(3) 0.079 Uiso 1 1 d D . . I1 I 0.0074(4) -0.0136(5) 0.16833(14) 0.103(3) Uani 0.35 1 d P . 1 I1A I -0.0138(9) 0.0321(11) 0.1657(7) 0.201(7) Uani 0.15 1 d P . 2 I2 I 0.0000 0.5000 0.04385(6) 0.1154(3) Uani 1 2 d S . . I3 I 0.292768(17) 0.707232(17) 0.0000 0.06440(13) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.03435(9) 0.03435(9) 0.02145(11) 0.00024(12) -0.00024(12) 0.00305(10) N1 0.0403(19) 0.050(2) 0.0267(15) -0.0042(15) -0.0075(15) 0.0110(16) N2 0.050(2) 0.0372(19) 0.0270(17) -0.0016(14) 0.0013(15) 0.0057(16) N3 0.075(3) 0.050(2) 0.0405(19) -0.0020(19) -0.0024(19) 0.027(2) N4 0.091(3) 0.054(2) 0.0198(16) 0.0032(16) -0.0001(19) -0.008(2) O1 0.0484(17) 0.0424(16) 0.0408(16) -0.0068(14) -0.0020(14) 0.0063(14) O2 0.0587(19) 0.0433(16) 0.0225(13) 0.0014(12) -0.0053(13) -0.0007(14) C1 0.036(2) 0.055(3) 0.037(2) -0.010(2) -0.009(2) 0.001(3) C2 0.053(3) 0.052(3) 0.041(2) -0.0131(19) -0.010(2) -0.009(2) C3 0.064(3) 0.041(3) 0.038(3) -0.010(2) 0.001(2) 0.008(3) C4 0.074(3) 0.031(2) 0.049(3) 0.0031(18) 0.004(2) -0.003(2) C5 0.058(3) 0.053(3) 0.038(2) -0.003(2) -0.007(2) 0.028(2) C6 0.048(3) 0.048(3) 0.032(2) 0.0012(17) 0.0022(17) 0.011(2) C7 0.059(3) 0.053(3) 0.0227(18) 0.0002(18) 0.0042(19) 0.008(2) C8 0.045(2) 0.052(2) 0.030(2) 0.0013(17) -0.0029(17) 0.001(2) C9 0.112(5) 0.045(3) 0.049(3) -0.015(2) 0.011(3) 0.004(3) C9A 0.112(5) 0.045(3) 0.049(3) -0.015(2) 0.011(3) 0.004(3) C17 0.091(4) 0.053(3) 0.034(2) 0.007(2) -0.006(3) -0.020(3) C24 0.176(8) 0.071(4) 0.046(3) 0.012(3) 0.016(4) -0.022(5) C17A 0.091(4) 0.053(3) 0.034(2) 0.007(2) -0.006(3) -0.020(3) C24A 0.176(8) 0.071(4) 0.046(3) 0.012(3) 0.016(4) -0.022(5) O1W 0.0590(15) 0.0590(15) 0.040(2) 0.006(3) -0.006(3) -0.0201(19) I1 0.064(3) 0.187(8) 0.0570(7) 0.0084(19) -0.0193(16) -0.070(4) I1A 0.213(12) 0.227(13) 0.164(6) -0.078(7) 0.078(7) -0.119(11) I2 0.1687(8) 0.0706(4) 0.1069(5) 0.000 0.000 0.0427(5) I3 0.07835(19) 0.07835(19) 0.03649(19) 0.0076(2) 0.0076(2) 0.0027(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2 2.337(3) . ? Gd1 O2 2.337(3) 7 ? Gd1 O1 2.362(3) . ? Gd1 O1 2.362(3) 7 ? Gd1 O1W 2.381(4) . ? Gd1 N1 2.696(3) . ? Gd1 N1 2.696(3) 7 ? Gd1 N2 2.711(3) . ? Gd1 N2 2.711(3) 7 ? N1 C5 1.476(6) . ? N1 C4 1.480(5) 7 ? N1 C1 1.497(5) . ? N2 C3 1.486(6) . ? N2 C2 1.486(5) . ? N2 C7 1.494(5) . ? N3 C6 1.317(6) . ? N3 C9 1.455(7) . ? N3 H3C 0.8600 . ? N4 C8 1.311(5) . ? N4 C17 1.481(6) . ? N4 H4A 0.8600 . ? O1 C6 1.240(5) . ? O2 C8 1.252(5) . ? C1 C2 1.509(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.516(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N1 1.480(5) 7 ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C6 1.504(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 C8 1.488(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C16 1.488(10) . ? C9 C10 1.558(7) . ? C9 H9A 0.9800 . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C10A C11A 1.3900 . ? C10A C15A 1.3900 . ? C11A C12A 1.3900 . ? C11A H11B 0.9300 . ? C12A C13A 1.3900 . ? C12A H12B 0.9300 . ? C13A C14A 1.3900 . ? C13A H13B 0.9300 . ? C14A C15A 1.3900 . ? C14A H14B 0.9300 . ? C15A H15B 0.9300 . ? C16A H16D 0.9600 . ? C16A H16E 0.9600 . ? C16A H16F 0.9600 . ? C17 C18 1.514(8) . ? C17 C24 1.552(7) . ? C17 H17A 0.9800 . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C19 H19A 0.9300 . ? C20 C21 1.3900 . ? C20 H20A 0.9300 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C18A C19A 1.3900 . ? C18A C23A 1.3900 . ? C19A C20A 1.3900 . ? C19A H19B 0.9300 . ? C20A C21A 1.3900 . ? C20A H20B 0.9300 . ? C21A C22A 1.3900 . ? C21A H21B 0.9300 . ? C22A C23A 1.3900 . ? C22A H22B 0.9300 . ? C23A H23B 0.9300 . ? O1W H1W 0.897(10) . ? I1 I1 0.600(19) 2 ? I1A I1A 1.36(5) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O2 146.01(14) . 7 ? O2 Gd1 O1 86.39(10) . . ? O2 Gd1 O1 84.22(10) 7 . ? O2 Gd1 O1 84.22(10) . 7 ? O2 Gd1 O1 86.39(10) 7 7 ? O1 Gd1 O1 147.49(15) . 7 ? O2 Gd1 O1W 73.01(7) . . ? O2 Gd1 O1W 73.01(7) 7 . ? O1 Gd1 O1W 73.74(7) . . ? O1 Gd1 O1W 73.74(7) 7 . ? O2 Gd1 N1 74.82(11) . . ? O2 Gd1 N1 129.01(10) 7 . ? O1 Gd1 N1 65.67(10) . . ? O1 Gd1 N1 139.84(10) 7 . ? O1W Gd1 N1 128.97(7) . . ? O2 Gd1 N1 129.01(10) . 7 ? O2 Gd1 N1 74.82(11) 7 7 ? O1 Gd1 N1 139.84(10) . 7 ? O1 Gd1 N1 65.67(10) 7 7 ? O1W Gd1 N1 128.97(7) . 7 ? N1 Gd1 N1 102.06(15) . 7 ? O2 Gd1 N2 65.44(10) . . ? O2 Gd1 N2 141.21(11) 7 . ? O1 Gd1 N2 129.71(10) . . ? O1 Gd1 N2 73.12(10) 7 . ? O1W Gd1 N2 128.50(7) . . ? N1 Gd1 N2 67.09(10) . . ? N1 Gd1 N2 66.82(10) 7 . ? O2 Gd1 N2 141.21(11) . 7 ? O2 Gd1 N2 65.44(10) 7 7 ? O1 Gd1 N2 73.12(10) . 7 ? O1 Gd1 N2 129.71(10) 7 7 ? O1W Gd1 N2 128.50(7) . 7 ? N1 Gd1 N2 66.82(10) . 7 ? N1 Gd1 N2 67.09(10) 7 7 ? N2 Gd1 N2 103.01(14) . 7 ? C5 N1 C4 110.0(4) . 7 ? C5 N1 C1 108.5(3) . . ? C4 N1 C1 109.6(4) 7 . ? C5 N1 Gd1 105.5(3) . . ? C4 N1 Gd1 112.1(2) 7 . ? C1 N1 Gd1 111.0(3) . . ? C3 N2 C2 109.0(4) . . ? C3 N2 C7 109.3(3) . . ? C2 N2 C7 110.4(3) . . ? C3 N2 Gd1 111.0(3) . . ? C2 N2 Gd1 111.2(2) . . ? C7 N2 Gd1 105.7(2) . . ? C6 N3 C9 122.9(4) . . ? C6 N3 H3C 118.6 . . ? C9 N3 H3C 118.6 . . ? C8 N4 C17 121.3(4) . . ? C8 N4 H4A 119.4 . . ? C17 N4 H4A 119.4 . . ? C6 O1 Gd1 124.3(3) . . ? C8 O2 Gd1 126.1(3) . . ? N1 C1 C2 111.6(4) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 113.5(4) . . ? N2 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? N2 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N2 C3 C4 111.6(4) . . ? N2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? N1 C4 C3 113.6(4) 7 . ? N1 C4 H4B 108.9 7 . ? C3 C4 H4B 108.9 . . ? N1 C4 H4C 108.9 7 . ? C3 C4 H4C 108.9 . . ? H4B C4 H4C 107.7 . . ? N1 C5 C6 110.9(4) . . ? N1 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.0 . . ? O1 C6 N3 121.8(4) . . ? O1 C6 C5 120.6(4) . . ? N3 C6 C5 117.6(4) . . ? C8 C7 N2 111.6(3) . . ? C8 C7 H7A 109.3 . . ? N2 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? N2 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? O2 C8 N4 121.0(4) . . ? O2 C8 C7 120.2(4) . . ? N4 C8 C7 118.8(4) . . ? N3 C9 C16 115.0(6) . . ? N3 C9 C10 109.0(5) . . ? C16 C9 C10 110.7(6) . . ? N3 C9 H9A 107.3 . . ? C16 C9 H9A 107.3 . . ? C10 C9 H9A 107.3 . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 120.6(5) . . ? C15 C10 C9 119.3(5) . . ? C10 C11 C12 120.0 . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 H15A 120.0 . . ? C10 C15 H15A 120.0 . . ? C11A C10A C15A 120.0 . . ? C12A C11A C10A 120.0 . . ? C12A C11A H11B 120.0 . . ? C10A C11A H11B 120.0 . . ? C13A C12A C11A 120.0 . . ? C13A C12A H12B 120.0 . . ? C11A C12A H12B 120.0 . . ? C14A C13A C12A 120.0 . . ? C14A C13A H13B 120.0 . . ? C12A C13A H13B 120.0 . . ? C13A C14A C15A 120.0 . . ? C13A C14A H14B 120.0 . . ? C15A C14A H14B 120.0 . . ? C14A C15A C10A 120.0 . . ? C14A C15A H15B 120.0 . . ? C10A C15A H15B 120.0 . . ? H16D C16A H16E 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? N4 C17 C18 115.2(4) . . ? N4 C17 C24 108.1(4) . . ? C18 C17 C24 113.5(4) . . ? N4 C17 H17A 106.5 . . ? C18 C17 H17A 106.5 . . ? C24 C17 H17A 106.5 . . ? C19 C18 C23 120.0 . . ? C19 C18 C17 117.5(5) . . ? C23 C18 C17 122.5(5) . . ? C18 C19 C20 120.0 . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 H23A 120.0 . . ? C18 C23 H23A 120.0 . . ? C19A C18A C23A 120.0 . . ? C20A C19A C18A 120.0 . . ? C20A C19A H19B 120.0 . . ? C18A C19A H19B 120.0 . . ? C19A C20A C21A 120.0 . . ? C19A C20A H20B 120.0 . . ? C21A C20A H20B 120.0 . . ? C20A C21A C22A 120.0 . . ? C20A C21A H21B 120.0 . . ? C22A C21A H21B 120.0 . . ? C23A C22A C21A 120.0 . . ? C23A C22A H22B 120.0 . . ? C21A C22A H22B 120.0 . . ? C22A C23A C18A 120.0 . . ? C22A C23A H23B 120.0 . . ? C18A C23A H23B 120.0 . . ? Gd1 O1W H1W 134(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Gd1 N1 C5 65.5(3) . . . . ? O2 Gd1 N1 C5 -86.9(3) 7 . . . ? O1 Gd1 N1 C5 -27.5(3) . . . . ? O1 Gd1 N1 C5 126.6(3) 7 . . . ? O1W Gd1 N1 C5 13.0(3) . . . . ? N1 Gd1 N1 C5 -167.0(3) 7 . . . ? N2 Gd1 N1 C5 134.8(3) . . . . ? N2 Gd1 N1 C5 -108.7(3) 7 . . . ? O2 Gd1 N1 C4 -174.8(3) . . . 7 ? O2 Gd1 N1 C4 32.8(3) 7 . . 7 ? O1 Gd1 N1 C4 92.2(3) . . . 7 ? O1 Gd1 N1 C4 -113.7(3) 7 . . 7 ? O1W Gd1 N1 C4 132.7(3) . . . 7 ? N1 Gd1 N1 C4 -47.3(3) 7 . . 7 ? N2 Gd1 N1 C4 -105.5(3) . . . 7 ? N2 Gd1 N1 C4 11.1(3) 7 . . 7 ? O2 Gd1 N1 C1 -51.8(3) . . . . ? O2 Gd1 N1 C1 155.8(3) 7 . . . ? O1 Gd1 N1 C1 -144.8(3) . . . . ? O1 Gd1 N1 C1 9.3(4) 7 . . . ? O1W Gd1 N1 C1 -104.3(3) . . . . ? N1 Gd1 N1 C1 75.7(3) 7 . . . ? N2 Gd1 N1 C1 17.5(3) . . . . ? N2 Gd1 N1 C1 134.0(3) 7 . . . ? O2 Gd1 N2 C3 -143.8(3) . . . . ? O2 Gd1 N2 C3 8.7(4) 7 . . . ? O1 Gd1 N2 C3 154.2(3) . . . . ? O1 Gd1 N2 C3 -52.5(3) 7 . . . ? O1W Gd1 N2 C3 -104.5(3) . . . . ? N1 Gd1 N2 C3 133.1(3) . . . . ? N1 Gd1 N2 C3 17.8(3) 7 . . . ? N2 Gd1 N2 C3 75.5(3) 7 . . . ? O2 Gd1 N2 C2 94.6(3) . . . . ? O2 Gd1 N2 C2 -112.9(3) 7 . . . ? O1 Gd1 N2 C2 32.6(3) . . . . ? O1 Gd1 N2 C2 -174.1(3) 7 . . . ? O1W Gd1 N2 C2 133.9(2) . . . . ? N1 Gd1 N2 C2 11.5(3) . . . . ? N1 Gd1 N2 C2 -103.9(3) 7 . . . ? N2 Gd1 N2 C2 -46.1(2) 7 . . . ? O2 Gd1 N2 C7 -25.3(2) . . . . ? O2 Gd1 N2 C7 127.2(3) 7 . . . ? O1 Gd1 N2 C7 -87.3(3) . . . . ? O1 Gd1 N2 C7 66.0(3) 7 . . . ? O1W Gd1 N2 C7 14.0(3) . . . . ? N1 Gd1 N2 C7 -108.4(3) . . . . ? N1 Gd1 N2 C7 136.2(3) 7 . . . ? N2 Gd1 N2 C7 -166.0(3) 7 . . . ? O2 Gd1 O1 C6 -59.8(3) . . . . ? O2 Gd1 O1 C6 152.9(3) 7 . . . ? O1 Gd1 O1 C6 -133.2(3) 7 . . . ? O1W Gd1 O1 C6 -133.2(3) . . . . ? N1 Gd1 O1 C6 15.2(3) . . . . ? N1 Gd1 O1 C6 94.8(4) 7 . . . ? N2 Gd1 O1 C6 -6.2(4) . . . . ? N2 Gd1 O1 C6 86.8(3) 7 . . . ? O2 Gd1 O2 C8 -133.7(4) 7 . . . ? O1 Gd1 O2 C8 152.2(4) . . . . ? O1 Gd1 O2 C8 -59.0(3) 7 . . . ? O1W Gd1 O2 C8 -133.7(3) . . . . ? N1 Gd1 O2 C8 86.4(3) . . . . ? N1 Gd1 O2 C8 -6.9(4) 7 . . . ? N2 Gd1 O2 C8 15.1(3) . . . . ? N2 Gd1 O2 C8 95.1(4) 7 . . . ? C5 N1 C1 C2 -161.1(4) . . . . ? C4 N1 C1 C2 78.8(5) 7 . . . ? Gd1 N1 C1 C2 -45.6(4) . . . . ? C3 N2 C2 C1 -163.3(3) . . . . ? C7 N2 C2 C1 76.5(5) . . . . ? Gd1 N2 C2 C1 -40.5(4) . . . . ? N1 C1 C2 N2 60.0(5) . . . . ? C2 N2 C3 C4 77.7(5) . . . . ? C7 N2 C3 C4 -161.5(4) . . . . ? Gd1 N2 C3 C4 -45.2(5) . . . . ? N2 C3 C4 N1 59.0(6) . . . 7 ? C4 N1 C5 C6 -83.3(4) 7 . . . ? C1 N1 C5 C6 156.8(4) . . . . ? Gd1 N1 C5 C6 37.8(4) . . . . ? Gd1 O1 C6 N3 179.2(3) . . . . ? Gd1 O1 C6 C5 1.5(6) . . . . ? C9 N3 C6 O1 -6.1(7) . . . . ? C9 N3 C6 C5 171.6(4) . . . . ? N1 C5 C6 O1 -30.7(6) . . . . ? N1 C5 C6 N3 151.6(4) . . . . ? C3 N2 C7 C8 154.1(4) . . . . ? C2 N2 C7 C8 -85.9(4) . . . . ? Gd1 N2 C7 C8 34.5(4) . . . . ? Gd1 O2 C8 N4 178.0(3) . . . . ? Gd1 O2 C8 C7 -0.1(6) . . . . ? C17 N4 C8 O2 -7.0(7) . . . . ? C17 N4 C8 C7 171.1(4) . . . . ? N2 C7 C8 O2 -27.2(6) . . . . ? N2 C7 C8 N4 154.6(4) . . . . ? C6 N3 C9 C16 -152.8(7) . . . . ? C6 N3 C9 C10 82.2(6) . . . . ? N3 C9 C10 C11 59.4(6) . . . . ? C16 C9 C10 C11 -68.1(8) . . . . ? N3 C9 C10 C15 -123.4(5) . . . . ? C16 C9 C10 C15 109.1(8) . . . . ? C15 C10 C11 C12 0.0 . . . . ? C9 C10 C11 C12 177.1(6) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? C9 C10 C15 C14 -177.2(6) . . . . ? C15A C10A C11A C12A 0.0 . . . . ? C10A C11A C12A C13A 0.0 . . . . ? C11A C12A C13A C14A 0.0 . . . . ? C12A C13A C14A C15A 0.0 . . . . ? C13A C14A C15A C10A 0.0 . . . . ? C11A C10A C15A C14A 0.0 . . . . ? C8 N4 C17 C18 66.3(6) . . . . ? C8 N4 C17 C24 -165.6(5) . . . . ? N4 C17 C18 C19 -130.6(4) . . . . ? C24 C17 C18 C19 104.0(5) . . . . ? N4 C17 C18 C23 49.4(5) . . . . ? C24 C17 C18 C23 -76.0(5) . . . . ? C23 C18 C19 C20 0.0 . . . . ? C17 C18 C19 C20 179.98(16) . . . . ? C18 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C18 0.0 . . . . ? C19 C18 C23 C22 0.0 . . . . ? C17 C18 C23 C22 -179.98(17) . . . . ? C23A C18A C19A C20A 0.0 . . . . ? C18A C19A C20A C21A 0.0 . . . . ? C19A C20A C21A C22A 0.0 . . . . ? C20A C21A C22A C23A 0.0 . . . . ? C21A C22A C23A C18A 0.0 . . . . ? C19A C18A C23A C22A 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.303 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.083 #============================================================================== data_[Yb.2]Cl3 _database_code_depnum_ccdc_archive 'CCDC 606220' #============================================================================== _chemical_name_systematic ; [Yb.DOTAPh]Cl~3~.7H~2~O ; _chemical_name_common (Yb.DOTAPh)Cl!3$.7H!2$O _chemical_melting_point 'not measured' _chemical_formula_moiety 'C48 H64 N8 O5 Yb, 7(H2 O), 3Cl' _chemical_formula_sum 'C48 H78 Cl3 N8 O12 Yb' _chemical_formula_weight 1238.60 _chemical_absolute_configuration syn 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 Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 22.0655(18) _cell_length_b 11.2776(9) _cell_length_c 33.982(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.113(1) _cell_angle_gamma 90.00 _cell_volume 8434.6(12) _cell_formula_units_Z 6 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8743 _cell_measurement_theta_min 2.796 _cell_measurement_theta_max 28.280 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3750 _exptl_absorpt_coefficient_mu 1.869 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6680 _exptl_absorpt_correction_T_max 0.7806 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.1100 -1.00 0.00 0.00 0.1100 0.00 1.00 0.00 0.1100 0.00 -1.00 0.00 0.1100 0.00 0.00 1.00 0.0700 0.00 0.00 -1.00 0.0700 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 94160 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 28.28 _reflns_number_total 41387 _reflns_number_gt 39368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+45.7088P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(5) _refine_ls_number_reflns 41387 _refine_ls_number_parameters 2002 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.747271(13) 0.77963(3) 0.993805(7) 0.01363(5) Uani 1 1 d . . . O11 O 0.77032(19) 0.7154(4) 0.93271(12) 0.0150(8) Uani 1 1 d . . . O12 O 0.65345(19) 0.7254(4) 0.96961(12) 0.0161(8) Uani 1 1 d . . . O13 O 0.7144(2) 0.7156(4) 1.05188(13) 0.0175(9) Uani 1 1 d . . . O14 O 0.8387(2) 0.7027(4) 1.01743(13) 0.0195(9) Uani 1 1 d . . . N11 N 0.8299(3) 0.9086(4) 0.96373(15) 0.0169(10) Uani 1 1 d . . . N12 N 0.6975(3) 0.9306(4) 0.94000(17) 0.0206(11) Uani 1 1 d . . . N13 N 0.6718(3) 0.9294(5) 1.02352(16) 0.0199(11) Uani 1 1 d . . . N14 N 0.8026(3) 0.9107(5) 1.04796(15) 0.0183(10) Uani 1 1 d . . . N15 N 0.8272(3) 0.7105(5) 0.88025(17) 0.0233(12) Uani 1 1 d . . . H15A H 0.8603 0.7335 0.8694 0.028 Uiso 1 1 calc R . . N16 N 0.5718(3) 0.7191(5) 0.92676(17) 0.0227(11) Uani 1 1 d . . . H16A H 0.5494 0.7524 0.9073 0.027 Uiso 1 1 calc R . . N17 N 0.6533(3) 0.7186(5) 1.10224(16) 0.0196(11) Uani 1 1 d . . . H17A H 0.6225 0.7518 1.1131 0.023 Uiso 1 1 calc R . . N18 N 0.9166(2) 0.6805(5) 1.06408(16) 0.0205(11) Uani 1 1 d . B . H18A H 0.9349 0.7071 1.0862 0.025 Uiso 1 1 calc R . . C101 C 0.8031(3) 1.0110(6) 0.94101(19) 0.0211(13) Uani 1 1 d . . . H10A H 0.8335 1.0421 0.9236 0.025 Uiso 1 1 calc R . . H10B H 0.7939 1.0749 0.9597 0.025 Uiso 1 1 calc R . . C102 C 0.7453(3) 0.9796(6) 0.9159(2) 0.0222(13) Uani 1 1 d . . . H10C H 0.7295 1.0515 0.9020 0.027 Uiso 1 1 calc R . . H10D H 0.7550 0.9205 0.8958 0.027 Uiso 1 1 calc R . . C103 C 0.6674(3) 1.0325(6) 0.9588(2) 0.0260(14) Uani 1 1 d . . . H10E H 0.6400 1.0732 0.9388 0.031 Uiso 1 1 calc R . . H10F H 0.6987 1.0901 0.9689 0.031 Uiso 1 1 calc R . . C104 C 0.6314(3) 0.9917(6) 0.9924(2) 0.0266(15) Uani 1 1 d . . . H10G H 0.6121 1.0610 1.0043 0.032 Uiso 1 1 calc R . . H10H H 0.5988 0.9371 0.9823 0.032 Uiso 1 1 calc R . . C105 C 0.7062(3) 1.0219(6) 1.0471(2) 0.0273(15) Uani 1 1 d . . . H10I H 0.6782 1.0626 1.0641 0.033 Uiso 1 1 calc R . . H10J H 0.7216 1.0816 1.0289 0.033 Uiso 1 1 calc R . . C106 C 0.7594(3) 0.9722(6) 1.0727(2) 0.0246(14) Uani 1 1 d . . . H10K H 0.7807 1.0375 1.0875 0.030 Uiso 1 1 calc R . . H10L H 0.7443 0.9158 1.0920 0.030 Uiso 1 1 calc R . . C107 C 0.8424(3) 1.0014(6) 1.0298(2) 0.0252(14) Uani 1 1 d . . . H10M H 0.8169 1.0699 1.0207 0.030 Uiso 1 1 calc R . . H10N H 0.8730 1.0304 1.0502 0.030 Uiso 1 1 calc R . . C108 C 0.8746(3) 0.9549(6) 0.99562(19) 0.0255(14) Uani 1 1 d . . . H10O H 0.9025 0.8904 1.0048 0.031 Uiso 1 1 calc R . . H10P H 0.8991 1.0191 0.9848 0.031 Uiso 1 1 calc R . . C109 C 0.8622(3) 0.8294(6) 0.93767(18) 0.0217(13) Uani 1 1 d . . . H10Q H 0.8928 0.7818 0.9535 0.026 Uiso 1 1 calc R . . H10R H 0.8836 0.8770 0.9185 0.026 Uiso 1 1 calc R . . C110 C 0.8164(3) 0.7484(6) 0.91608(18) 0.0191(12) Uani 1 1 d . . . C111 C 0.6517(3) 0.8627(6) 0.9156(2) 0.0222(13) Uani 1 1 d . . . H11A H 0.6708 0.8281 0.8928 0.027 Uiso 1 1 calc R . . H11B H 0.6190 0.9169 0.9054 0.027 Uiso 1 1 calc R . . C112 C 0.6249(3) 0.7657(6) 0.93877(16) 0.0184(12) Uani 1 1 d . . . C113 C 0.6338(3) 0.8604(6) 1.0492(2) 0.0225(13) Uani 1 1 d . . . H11C H 0.5982 0.8280 1.0334 0.027 Uiso 1 1 calc R . . H11D H 0.6188 0.9128 1.0698 0.027 Uiso 1 1 calc R . . C114 C 0.6698(3) 0.7610(6) 1.06834(18) 0.0190(12) Uani 1 1 d . . . C115 C 0.8412(3) 0.8305(6) 1.07390(17) 0.0208(13) Uani 1 1 d . . . H11E H 0.8166 0.7951 1.0941 0.025 Uiso 1 1 calc R . . H11F H 0.8747 0.8763 1.0876 0.025 Uiso 1 1 calc R . . C116 C 0.8671(3) 0.7332(6) 1.04936(18) 0.0181(12) Uani 1 1 d . . . C117 C 0.7841(3) 0.6301(6) 0.8585(2) 0.0254(14) Uani 1 1 d . . . H11G H 0.7662 0.5755 0.8778 0.031 Uiso 1 1 calc R . . C118 C 0.7326(3) 0.6998(8) 0.8367(2) 0.0317(17) Uani 1 1 d . . . C119 C 0.6733(4) 0.6586(9) 0.8372(3) 0.044(2) Uani 1 1 d . . . H11H H 0.6656 0.5876 0.8511 0.053 Uiso 1 1 calc R . . C120 C 0.6255(4) 0.7184(12) 0.8182(3) 0.061(3) Uani 1 1 d . . . H12A H 0.5851 0.6901 0.8193 0.073 Uiso 1 1 calc R . . C121 C 0.6369(5) 0.8209(13) 0.7972(3) 0.060(3) Uani 1 1 d . . . H12B H 0.6041 0.8621 0.7837 0.072 Uiso 1 1 calc R . . C122 C 0.6962(5) 0.8641(11) 0.7957(3) 0.057(3) Uani 1 1 d . . . H12C H 0.7040 0.9340 0.7812 0.068 Uiso 1 1 calc R . . C123 C 0.7434(4) 0.8021(8) 0.8158(2) 0.0337(18) Uani 1 1 d . . . H12D H 0.7838 0.8307 0.8153 0.040 Uiso 1 1 calc R . . C124 C 0.8188(4) 0.5563(8) 0.8300(3) 0.0372(18) Uani 1 1 d . . . H12E H 0.8498 0.5090 0.8449 0.056 Uiso 1 1 calc R . . H12F H 0.8384 0.6091 0.8118 0.056 Uiso 1 1 calc R . . H12R H 0.7905 0.5035 0.8149 0.056 Uiso 1 1 calc R . . C125 C 0.5502(3) 0.6126(6) 0.9456(2) 0.0241(13) Uani 1 1 d . . . H12G H 0.5847 0.5552 0.9488 0.029 Uiso 1 1 calc R . . C126 C 0.5284(3) 0.6378(6) 0.9864(2) 0.0248(14) Uani 1 1 d . . . C127 C 0.5478(4) 0.5621(7) 1.0176(2) 0.0348(17) Uani 1 1 d . . . H12H H 0.5755 0.4994 1.0136 0.042 Uiso 1 1 calc R . . C128 C 0.5255(5) 0.5808(8) 1.0550(3) 0.043(2) Uani 1 1 d . . . H12I H 0.5372 0.5283 1.0760 0.052 Uiso 1 1 calc R . . C129 C 0.4881(5) 0.6713(8) 1.0612(2) 0.044(2) Uani 1 1 d . . . H12J H 0.4746 0.6841 1.0868 0.053 Uiso 1 1 calc R . . C130 C 0.4690(4) 0.7464(8) 1.0306(2) 0.0372(17) Uani 1 1 d . . . H13A H 0.4421 0.8098 1.0352 0.045 Uiso 1 1 calc R . . C131 C 0.4891(3) 0.7296(7) 0.9929(2) 0.0321(16) Uani 1 1 d . . . H13B H 0.4758 0.7811 0.9719 0.039 Uiso 1 1 calc R . . C132 C 0.4995(4) 0.5557(8) 0.9184(2) 0.0329(17) Uani 1 1 d . . . H13C H 0.5139 0.5440 0.8921 0.049 Uiso 1 1 calc R . . H13D H 0.4639 0.6079 0.9165 0.049 Uiso 1 1 calc R . . H13E H 0.4883 0.4790 0.9293 0.049 Uiso 1 1 calc R . . C133 C 0.6845(3) 0.6175(6) 1.1225(2) 0.0215(13) Uani 1 1 d . . . H13F H 0.6928 0.5557 1.1025 0.026 Uiso 1 1 calc R . . C134 C 0.7444(3) 0.6580(6) 1.1426(2) 0.0224(13) Uani 1 1 d . . . C135 C 0.7956(3) 0.5886(7) 1.1397(2) 0.0280(15) Uani 1 1 d . . . H13G H 0.7938 0.5198 1.1236 0.034 Uiso 1 1 calc R . . C136 C 0.8502(4) 0.6199(8) 1.1606(2) 0.0360(17) Uani 1 1 d . . . H13H H 0.8851 0.5715 1.1590 0.043 Uiso 1 1 calc R . . C137 C 0.8533(4) 0.7188(7) 1.1831(2) 0.0325(17) Uani 1 1 d . . . H13I H 0.8907 0.7403 1.1969 0.039 Uiso 1 1 calc R . . C138 C 0.8018(3) 0.7898(8) 1.1860(2) 0.0321(15) Uani 1 1 d . . . H13J H 0.8043 0.8592 1.2019 0.039 Uiso 1 1 calc R . . C139 C 0.7472(3) 0.7593(6) 1.16589(19) 0.0239(13) Uani 1 1 d . . . H13K H 0.7121 0.8071 1.1680 0.029 Uiso 1 1 calc R . . C140 C 0.6419(3) 0.5651(6) 1.1516(2) 0.0249(14) Uani 1 1 d . . . H14A H 0.6051 0.5352 1.1371 0.037 Uiso 1 1 calc R . . H14B H 0.6310 0.6266 1.1702 0.037 Uiso 1 1 calc R . . H14C H 0.6625 0.4998 1.1662 0.037 Uiso 1 1 calc R . . C141 C 0.9422(3) 0.5784(7) 1.0445(2) 0.0290(15) Uani 1 1 d . . . H14D H 0.9097 0.5247 1.0327 0.035 Uiso 1 1 calc R A 1 C142 C 0.9824(4) 0.6350(9) 1.0108(3) 0.018(3) Uani 0.50 1 d PG B 1 C143 C 0.9726(5) 0.5918(9) 0.9726(3) 0.031(3) Uani 0.50 1 d PG B 1 H14E H 0.9420 0.5339 0.9667 0.037 Uiso 0.50 1 calc PR B 1 C144 C 1.0075(6) 0.6333(12) 0.9430(2) 0.047(7) Uani 0.50 1 d PG B 1 H14F H 1.0008 0.6037 0.9169 0.057 Uiso 0.50 1 calc PR B 1 C145 C 1.0522(6) 0.7180(11) 0.9517(3) 0.044(5) Uani 0.50 1 d PG B 1 H14G H 1.0760 0.7464 0.9315 0.052 Uiso 0.50 1 calc PR B 1 C146 C 1.0620(4) 0.7612(8) 0.9899(4) 0.040(4) Uani 0.50 1 d PG B 1 H14H H 1.0926 0.8191 0.9959 0.049 Uiso 0.50 1 calc PR B 1 C147 C 1.0271(5) 0.7197(9) 1.0195(3) 0.028(3) Uani 0.50 1 d PG B 1 H14I H 1.0338 0.7492 1.0456 0.033 Uiso 0.50 1 calc PR B 1 C42A C 0.9645(5) 0.5984(10) 1.0062(2) 0.021(3) Uani 0.50 1 d PG B 2 C43A C 0.9467(5) 0.5321(10) 0.9729(3) 0.032(3) Uani 0.50 1 d PG B 2 H43A H 0.9172 0.4712 0.9744 0.039 Uiso 0.50 1 calc PR B 2 C44A C 0.9721(6) 0.5548(11) 0.9374(2) 0.049(5) Uani 0.50 1 d PG B 2 H44A H 0.9599 0.5095 0.9146 0.059 Uiso 0.50 1 calc PR B 2 C45A C 1.0153(6) 0.6438(12) 0.9352(3) 0.036(5) Uani 0.50 1 d PG B 2 H45A H 1.0326 0.6593 0.9109 0.043 Uiso 0.50 1 calc PR B 2 C46A C 1.0331(5) 0.7102(9) 0.9685(4) 0.035(4) Uani 0.50 1 d PG B 2 H46A H 1.0626 0.7710 0.9670 0.042 Uiso 0.50 1 calc PR B 2 C47A C 1.0077(5) 0.6875(9) 1.0040(3) 0.030(3) Uani 0.50 1 d PG B 2 H47A H 1.0199 0.7328 1.0268 0.036 Uiso 0.50 1 calc PR B 2 C148 C 0.9857(3) 0.5130(7) 1.0741(2) 0.0290(15) Uani 1 1 d . B . H14J H 0.9657 0.4996 1.0986 0.043 Uiso 1 1 calc R . . H14K H 1.0223 0.5609 1.0798 0.043 Uiso 1 1 calc R . . H14L H 0.9969 0.4366 1.0630 0.043 Uiso 1 1 calc R . . Yb2 Yb 1.409993(11) 0.79615(2) 0.337171(7) 0.01290(6) Uani 1 1 d . . . O21 O 1.50648(19) 0.7295(4) 0.35161(13) 0.0178(8) Uani 1 1 d . . . O22 O 1.42570(19) 0.7589(4) 0.27297(12) 0.0236(10) Uani 1 1 d . . . O23 O 1.31377(18) 0.7296(4) 0.31797(14) 0.0191(9) Uani 1 1 d . . . O24 O 1.39598(19) 0.7040(4) 0.39490(14) 0.0187(9) Uani 1 1 d . . . N21 N 1.4708(2) 0.9256(4) 0.39096(15) 0.0161(10) Uani 1 1 d . . . N22 N 1.4799(2) 0.9525(5) 0.30595(15) 0.0184(10) Uani 1 1 d . . . N23 N 1.3465(2) 0.9488(5) 0.29336(17) 0.0185(11) Uani 1 1 d . . . N24 N 1.3371(2) 0.9139(5) 0.38023(17) 0.0213(11) Uani 1 1 d . . . N25 N 1.5952(2) 0.7112(5) 0.38786(18) 0.0216(11) Uani 1 1 d . . . H25A H 1.6206 0.7429 0.4061 0.026 Uiso 1 1 calc R . . N26 N 1.4815(3) 0.7596(6) 0.22046(17) 0.0293(13) Uani 1 1 d . . . H26A H 1.5132 0.7875 0.2092 0.035 Uiso 1 1 calc R . . N27 N 1.2321(2) 0.7145(5) 0.27474(18) 0.0230(12) Uani 1 1 d . . . H27A H 1.2092 0.7474 0.2555 0.028 Uiso 1 1 calc R . . N28 N 1.3526(2) 0.6829(5) 0.45315(17) 0.0215(11) Uani 1 1 d . . . H28A H 1.3245 0.7078 0.4683 0.026 Uiso 1 1 calc R . . C201 C 1.4956(3) 1.0313(6) 0.3734(2) 0.0234(14) Uani 1 1 d . . . H20A H 1.5260 1.0679 0.3925 0.028 Uiso 1 1 calc R . . H20B H 1.4626 1.0894 0.3676 0.028 Uiso 1 1 calc R . . C202 C 1.5256(3) 1.0033(6) 0.3354(2) 0.0211(13) Uani 1 1 d . . . H20C H 1.5429 1.0766 0.3248 0.025 Uiso 1 1 calc R . . H20D H 1.5591 0.9459 0.3409 0.025 Uiso 1 1 calc R . . C203 C 1.4447(3) 1.0531(6) 0.2871(2) 0.0277(15) Uani 1 1 d . . . H20E H 1.4694 1.0915 0.2675 0.033 Uiso 1 1 calc R . . H20F H 1.4369 1.1127 0.3075 0.033 Uiso 1 1 calc R . . C204 C 1.3847(3) 1.0141(6) 0.2668(2) 0.0235(14) Uani 1 1 d . . . H20G H 1.3622 1.0848 0.2564 0.028 Uiso 1 1 calc R . . H20H H 1.3926 0.9628 0.2441 0.028 Uiso 1 1 calc R . . C205 C 1.3177(3) 1.0349(6) 0.3203(2) 0.0250(14) Uani 1 1 d . . . H20I H 1.2858 1.0802 0.3048 0.030 Uiso 1 1 calc R . . H20J H 1.3490 1.0921 0.3307 0.030 Uiso 1 1 calc R . . C206 C 1.2898(3) 0.9755(6) 0.3547(2) 0.0250(14) Uani 1 1 d . . . H20K H 1.2695 1.0358 0.3704 0.030 Uiso 1 1 calc R . . H20L H 1.2587 0.9176 0.3446 0.030 Uiso 1 1 calc R . . C207 C 1.3704(3) 1.0031(6) 0.4068(2) 0.0251(14) Uani 1 1 d . . . H20M H 1.3757 1.0772 0.3919 0.030 Uiso 1 1 calc R . . H20N H 1.3455 1.0217 0.4291 0.030 Uiso 1 1 calc R . . C208 C 1.4313(3) 0.9601(6) 0.4228(2) 0.0246(14) Uani 1 1 d . . . H20O H 1.4516 1.0235 0.4390 0.030 Uiso 1 1 calc R . . H20P H 1.4259 0.8910 0.4402 0.030 Uiso 1 1 calc R . . C209 C 1.5213(3) 0.8518(6) 0.40916(18) 0.0181(12) Uani 1 1 d . . . H20Q H 1.5076 0.8116 0.4329 0.022 Uiso 1 1 calc R . . H20R H 1.5560 0.9036 0.4176 0.022 Uiso 1 1 calc R . . C210 C 1.5417(3) 0.7601(5) 0.38064(17) 0.0176(12) Uani 1 1 d . . . C211 C 1.5121(3) 0.8872(6) 0.27544(19) 0.0224(13) Uani 1 1 d . . . H21A H 1.5480 0.8459 0.2880 0.027 Uiso 1 1 calc R . . H21B H 1.5262 0.9439 0.2558 0.027 Uiso 1 1 calc R . . C212 C 1.4697(3) 0.7987(6) 0.2552(2) 0.0205(13) Uani 1 1 d . . . C213 C 1.2982(3) 0.8834(7) 0.2697(2) 0.0245(15) Uani 1 1 d . . . H21C H 1.3124 0.8660 0.2433 0.029 Uiso 1 1 calc R . . H21D H 1.2617 0.9341 0.2660 0.029 Uiso 1 1 calc R . . C214 C 1.2816(3) 0.7691(6) 0.28902(19) 0.0208(13) Uani 1 1 d . . . C215 C 1.3085(3) 0.8224(7) 0.4053(2) 0.0236(15) Uani 1 1 d . . . H21E H 1.2928 0.8607 0.4288 0.028 Uiso 1 1 calc R . . H21F H 1.2742 0.7836 0.3901 0.028 Uiso 1 1 calc R . . C216 C 1.3557(3) 0.7319(6) 0.41808(19) 0.0207(13) Uani 1 1 d . . . C217 C 1.6145(3) 0.6055(6) 0.3667(2) 0.0212(13) Uani 1 1 d . . . H21G H 1.5780 0.5540 0.3610 0.025 Uiso 1 1 calc R . . C218 C 1.6403(3) 0.6350(6) 0.3281(2) 0.0236(13) Uani 1 1 d . . . C219 C 1.6181(4) 0.5769(8) 0.2942(3) 0.0382(18) Uani 1 1 d . . . H21H H 1.5846 0.5242 0.2952 0.046 Uiso 1 1 calc R . . C220 C 1.6440(5) 0.5946(10) 0.2588(3) 0.052(2) Uani 1 1 d . . . H22A H 1.6291 0.5525 0.2359 0.062 Uiso 1 1 calc R . . C221 C 1.6913(5) 0.6732(10) 0.2567(3) 0.052(2) Uani 1 1 d . . . H22B H 1.7085 0.6862 0.2322 0.062 Uiso 1 1 calc R . . C222 C 1.7139(4) 0.7333(7) 0.2900(3) 0.0395(19) Uani 1 1 d . . . H22C H 1.7469 0.7867 0.2886 0.047 Uiso 1 1 calc R . . C223 C 1.6876(3) 0.7149(6) 0.3258(3) 0.0322(17) Uani 1 1 d . . . H22D H 1.7022 0.7575 0.3487 0.039 Uiso 1 1 calc R . . C224 C 1.6597(3) 0.5370(7) 0.3941(2) 0.0278(15) Uani 1 1 d . . . H22E H 1.6395 0.5099 0.4172 0.042 Uiso 1 1 calc R . . H22F H 1.6938 0.5888 0.4025 0.042 Uiso 1 1 calc R . . H22G H 1.6747 0.4683 0.3800 0.042 Uiso 1 1 calc R . . C225 C 1.4428(4) 0.6699(8) 0.1997(2) 0.0376(19) Uani 1 1 d . . . H22H H 1.4232 0.6210 0.2197 0.045 Uiso 1 1 calc R . . C226 C 1.3929(3) 0.7291(8) 0.1729(3) 0.040(2) Uani 1 1 d . . . C227 C 1.3319(4) 0.7017(9) 0.1778(4) 0.052(3) Uani 1 1 d . . . H22I H 1.3211 0.6495 0.1981 0.063 Uiso 1 1 calc R . . C228 C 1.2868(4) 0.7545(11) 0.1513(4) 0.063(3) Uani 1 1 d . . . H22K H 1.2452 0.7381 0.1546 0.076 Uiso 1 1 calc R . . C229 C 1.3007(6) 0.8254(13) 0.1224(5) 0.076(4) Uani 1 1 d . . . H22L H 1.2695 0.8571 0.1048 0.091 Uiso 1 1 calc R . . C230 C 1.3611(5) 0.8535(11) 0.1179(4) 0.064(3) Uani 1 1 d . . . H23A H 1.3713 0.9065 0.0977 0.077 Uiso 1 1 calc R . . C231 C 1.4072(4) 0.8034(10) 0.1434(3) 0.043(2) Uani 1 1 d . . . H23B H 1.4485 0.8216 0.1400 0.052 Uiso 1 1 calc R . . C232 C 1.4825(4) 0.5890(8) 0.1765(2) 0.0366(18) Uani 1 1 d . . . H23C H 1.5082 0.5405 0.1948 0.055 Uiso 1 1 calc R . . H23D H 1.5081 0.6372 0.1604 0.055 Uiso 1 1 calc R . . H23E H 1.4566 0.5373 0.1593 0.055 Uiso 1 1 calc R . . C233 C 1.2145(3) 0.5979(5) 0.29075(19) 0.0190(12) Uani 1 1 d . . . H23F H 1.2511 0.5454 0.2925 0.023 Uiso 1 1 calc R . . C234 C 1.1927(3) 0.6117(5) 0.3316(2) 0.0186(12) Uani 1 1 d . . . C235 C 1.2162(3) 0.5402(6) 0.3623(2) 0.0238(13) Uani 1 1 d . . . H23G H 1.2474 0.4850 0.3576 0.029 Uiso 1 1 calc R . . C236 C 1.1948(4) 0.5477(7) 0.3997(2) 0.0305(16) Uani 1 1 d . . . H23H H 1.2111 0.4981 0.4204 0.037 Uiso 1 1 calc R . . C237 C 1.1486(3) 0.6297(7) 0.4066(2) 0.0306(16) Uani 1 1 d . . . H23I H 1.1334 0.6357 0.4320 0.037 Uiso 1 1 calc R . . C238 C 1.1257(3) 0.7008(6) 0.3764(2) 0.0290(15) Uani 1 1 d . . . H23J H 1.0945 0.7560 0.3810 0.035 Uiso 1 1 calc R . . C239 C 1.1476(3) 0.6936(5) 0.3387(2) 0.0227(13) Uani 1 1 d . . . H23K H 1.1317 0.7443 0.3181 0.027 Uiso 1 1 calc R . . C240 C 1.1665(3) 0.5417(6) 0.2621(2) 0.0247(14) Uani 1 1 d . . . H24A H 1.1827 0.5334 0.2361 0.037 Uiso 1 1 calc R . . H24B H 1.1303 0.5922 0.2598 0.037 Uiso 1 1 calc R . . H24C H 1.1556 0.4633 0.2718 0.037 Uiso 1 1 calc R . . C241 C 1.3942(3) 0.5881(6) 0.46796(19) 0.0196(12) Uani 1 1 d . . . H24D H 1.4011 0.5338 0.4455 0.024 Uiso 1 1 calc R . . C242 C 1.4556(3) 0.6389(6) 0.48330(18) 0.0203(12) Uani 1 1 d . . . C243 C 1.5094(3) 0.5938(7) 0.4708(2) 0.0266(14) Uani 1 1 d . . . H24E H 1.5079 0.5342 0.4510 0.032 Uiso 1 1 calc R . . C244 C 1.5655(3) 0.6340(7) 0.4867(2) 0.0287(15) Uani 1 1 d . . . H24F H 1.6019 0.6024 0.4777 0.034 Uiso 1 1 calc R . . C245 C 1.5679(4) 0.7212(6) 0.5159(2) 0.0330(17) Uani 1 1 d . . . H24G H 1.6061 0.7486 0.5271 0.040 Uiso 1 1 calc R . . C246 C 1.5148(4) 0.7675(6) 0.5286(2) 0.0350(18) Uani 1 1 d . . . H24H H 1.5166 0.8278 0.5482 0.042 Uiso 1 1 calc R . . C247 C 1.4586(3) 0.7262(6) 0.5130(2) 0.0239(15) Uani 1 1 d . . . H24I H 1.4223 0.7570 0.5223 0.029 Uiso 1 1 calc R . . C248 C 1.3641(3) 0.5166(6) 0.4994(2) 0.0231(13) Uani 1 1 d . . . H24J H 1.3282 0.4759 0.4874 0.035 Uiso 1 1 calc R . . H24K H 1.3520 0.5701 0.5202 0.035 Uiso 1 1 calc R . . H24L H 1.3930 0.4579 0.5109 0.035 Uiso 1 1 calc R . . Yb3 Yb 1.090665(11) 0.753831(19) 0.667356(7) 0.01132(6) Uani 1 1 d . . . O31 O 1.12493(18) 0.6906(4) 0.60880(13) 0.0146(8) Uani 1 1 d . . . O32 O 0.99980(18) 0.6874(4) 0.64090(12) 0.0141(8) Uani 1 1 d . . . O33 O 1.05484(19) 0.6839(4) 0.72451(13) 0.0181(9) Uani 1 1 d . . . O34 O 1.18138(19) 0.6849(4) 0.69504(14) 0.0177(9) Uani 1 1 d . . . N31 N 1.1736(2) 0.8929(4) 0.64139(15) 0.0148(10) Uani 1 1 d . . . N32 N 1.0429(2) 0.8961(4) 0.61249(15) 0.0135(9) Uani 1 1 d . . . N33 N 1.0084(2) 0.8934(4) 0.69427(15) 0.0147(10) Uani 1 1 d . . . N34 N 1.1385(2) 0.8926(4) 0.72365(15) 0.0131(9) Uani 1 1 d . . . N35 N 1.1895(2) 0.6933(5) 0.56007(16) 0.0176(10) Uani 1 1 d . . . H35A H 1.2221 0.7248 0.5508 0.021 Uiso 1 1 calc R . . N36 N 0.9229(2) 0.6746(5) 0.59359(16) 0.0172(10) Uani 1 1 d . . . H36A H 0.9053 0.7036 0.5716 0.021 Uiso 1 1 calc R . . N37 N 0.9928(2) 0.6907(5) 0.77468(15) 0.0166(10) Uani 1 1 d . . . H37A H 0.9609 0.7238 0.7843 0.020 Uiso 1 1 calc R . . N38 N 1.2590(2) 0.6765(5) 0.74144(17) 0.0183(10) Uani 1 1 d . . . H38A H 1.2765 0.7060 0.7634 0.022 Uiso 1 1 calc R . . C301 C 1.1442(3) 0.9913(5) 0.61736(19) 0.0160(11) Uani 1 1 d . . . H30A H 1.1750 1.0286 0.6015 0.019 Uiso 1 1 calc R . . H30B H 1.1297 1.0523 0.6354 0.019 Uiso 1 1 calc R . . C302 C 1.0913(3) 0.9504(5) 0.58990(18) 0.0152(11) Uani 1 1 d . . . H30C H 1.0743 1.0189 0.5746 0.018 Uiso 1 1 calc R . . H30D H 1.1057 0.8916 0.5710 0.018 Uiso 1 1 calc R . . C303 C 1.0062(3) 0.9921(5) 0.62925(18) 0.0169(12) Uani 1 1 d . . . H30E H 0.9787 1.0267 0.6080 0.020 Uiso 1 1 calc R . . H30F H 1.0337 1.0557 0.6398 0.020 Uiso 1 1 calc R . . C304 C 0.9689(3) 0.9473(6) 0.66188(19) 0.0182(12) Uani 1 1 d . . . H30G H 0.9458 1.0140 0.6724 0.022 Uiso 1 1 calc R . . H30H H 0.9393 0.8875 0.6510 0.022 Uiso 1 1 calc R . . C305 C 1.0375(3) 0.9912(5) 0.71889(17) 0.0164(11) Uani 1 1 d . . . H30I H 1.0066 1.0274 0.7349 0.020 Uiso 1 1 calc R . . H30J H 1.0520 1.0533 0.7012 0.020 Uiso 1 1 calc R . . C306 C 1.0905(3) 0.9485(5) 0.74613(19) 0.0176(12) Uani 1 1 d . . . H30K H 1.1082 1.0166 0.7614 0.021 Uiso 1 1 calc R . . H30L H 1.0758 0.8903 0.7650 0.021 Uiso 1 1 calc R . . C307 C 1.1757(3) 0.9895(5) 0.70731(19) 0.0167(12) Uani 1 1 d . . . H30M H 1.2032 1.0229 0.7288 0.020 Uiso 1 1 calc R . . H30N H 1.1483 1.0538 0.6971 0.020 Uiso 1 1 calc R . . C308 C 1.2128(3) 0.9463(5) 0.67461(18) 0.0167(11) Uani 1 1 d . . . H30O H 1.2359 1.0136 0.6645 0.020 Uiso 1 1 calc R . . H30P H 1.2424 0.8864 0.6852 0.020 Uiso 1 1 calc R . . C309 C 1.2111(2) 0.8190(5) 0.61727(18) 0.0162(11) Uani 1 1 d . . . H30Q H 1.2422 0.7773 0.6345 0.019 Uiso 1 1 calc R . . H30R H 1.2322 0.8698 0.5988 0.019 Uiso 1 1 calc R . . C310 C 1.1725(3) 0.7304(5) 0.59446(17) 0.0121(11) Uani 1 1 d . . . C311 C 1.0029(3) 0.8191(6) 0.58586(18) 0.0179(12) Uani 1 1 d . . . H31A H 1.0273 0.7831 0.5656 0.022 Uiso 1 1 calc R . . H31B H 0.9708 0.8682 0.5721 0.022 Uiso 1 1 calc R . . C312 C 0.9740(3) 0.7223(5) 0.60867(19) 0.0141(11) Uani 1 1 d . . . C313 C 0.9709(3) 0.8180(6) 0.71867(17) 0.0175(12) Uani 1 1 d . . . H31C H 0.9386 0.7788 0.7016 0.021 Uiso 1 1 calc R . . H31D H 0.9513 0.8678 0.7381 0.021 Uiso 1 1 calc R . . C314 C 1.0103(3) 0.7256(6) 0.73988(18) 0.0159(12) Uani 1 1 d . . . C315 C 1.1776(3) 0.8158(5) 0.75000(18) 0.0175(12) Uani 1 1 d . . . H31E H 1.1528 0.7780 0.7697 0.021 Uiso 1 1 calc R . . H31F H 1.2093 0.8645 0.7644 0.021 Uiso 1 1 calc R . . C316 C 1.2070(3) 0.7221(5) 0.72675(18) 0.0141(12) Uani 1 1 d . . . C317 C 1.1566(3) 0.6027(6) 0.53685(18) 0.0183(12) Uani 1 1 d . . . H31G H 1.1435 0.5403 0.5553 0.022 Uiso 1 1 calc R . . C318 C 1.0994(3) 0.6548(6) 0.51475(19) 0.0191(12) Uani 1 1 d . . . C319 C 1.0452(3) 0.5920(6) 0.5137(2) 0.0250(14) Uani 1 1 d . . . H31H H 1.0436 0.5183 0.5272 0.030 Uiso 1 1 calc R . . C320 C 0.9932(3) 0.6357(7) 0.4931(2) 0.0311(16) Uani 1 1 d . . . H32A H 0.9563 0.5921 0.4926 0.037 Uiso 1 1 calc R . . C321 C 0.9954(3) 0.7443(8) 0.4732(2) 0.0333(17) Uani 1 1 d . . . H32B H 0.9601 0.7748 0.4591 0.040 Uiso 1 1 calc R . . C322 C 1.0490(3) 0.8057(7) 0.4745(2) 0.0277(15) Uani 1 1 d . . . H32C H 1.0507 0.8792 0.4609 0.033 Uiso 1 1 calc R . . C323 C 1.1005(3) 0.7628(6) 0.4950(2) 0.0253(14) Uani 1 1 d . . . H32D H 1.1371 0.8074 0.4958 0.030 Uiso 1 1 calc R . . C324 C 1.1988(3) 0.5456(6) 0.5091(2) 0.0241(14) Uani 1 1 d . . . H32E H 1.2331 0.5088 0.5245 0.036 Uiso 1 1 calc R . . H32F H 1.2140 0.6061 0.4916 0.036 Uiso 1 1 calc R . . H32G H 1.1766 0.4848 0.4933 0.036 Uiso 1 1 calc R . . C325 C 0.8947(3) 0.5736(5) 0.61296(18) 0.0145(11) Uani 1 1 d . . . H32H H 0.9268 0.5123 0.6192 0.017 Uiso 1 1 calc R . . C326 C 0.8689(2) 0.6102(5) 0.65104(18) 0.0148(11) Uani 1 1 d . . . C327 C 0.8304(3) 0.7089(5) 0.6527(2) 0.0199(13) Uani 1 1 d . . . H32I H 0.8201 0.7531 0.6293 0.024 Uiso 1 1 calc R . . C328 C 0.8069(3) 0.7433(6) 0.6880(2) 0.0224(12) Uani 1 1 d . . . H32J H 0.7813 0.8108 0.6887 0.027 Uiso 1 1 calc R . . C329 C 0.8213(3) 0.6778(6) 0.7223(2) 0.0227(13) Uani 1 1 d . . . H32K H 0.8056 0.7007 0.7465 0.027 Uiso 1 1 calc R . . C330 C 0.8590(3) 0.5781(6) 0.7208(2) 0.0248(14) Uani 1 1 d . . . H33A H 0.8685 0.5324 0.7439 0.030 Uiso 1 1 calc R . . C331 C 0.8825(3) 0.5463(6) 0.6855(2) 0.0206(12) Uani 1 1 d . . . H33B H 0.9085 0.4793 0.6848 0.025 Uiso 1 1 calc R . . C332 C 0.8461(3) 0.5195(6) 0.5836(2) 0.0208(13) Uani 1 1 d . . . H33C H 0.8650 0.4945 0.5597 0.031 Uiso 1 1 calc R . . H33D H 0.8147 0.5789 0.5766 0.031 Uiso 1 1 calc R . . H33E H 0.8276 0.4507 0.5956 0.031 Uiso 1 1 calc R . . C333 C 1.0263(3) 0.5972(6) 0.79727(18) 0.0184(12) Uani 1 1 d . . . H33F H 1.0386 0.5350 0.7784 0.022 Uiso 1 1 calc R . . C334 C 1.0831(3) 0.6463(6) 0.81918(18) 0.0203(12) Uani 1 1 d . . . C335 C 1.0818(3) 0.7481(6) 0.8421(2) 0.0232(13) Uani 1 1 d . . . H33G H 1.0447 0.7897 0.8438 0.028 Uiso 1 1 calc R . . C336 C 1.1350(3) 0.7899(8) 0.8627(2) 0.0322(15) Uani 1 1 d . . . H33H H 1.1339 0.8580 0.8791 0.039 Uiso 1 1 calc R . . C337 C 1.1902(4) 0.7291(8) 0.8588(2) 0.0354(19) Uani 1 1 d . . . H33I H 1.2268 0.7578 0.8719 0.043 Uiso 1 1 calc R . . C338 C 1.1911(4) 0.6280(7) 0.8359(2) 0.0341(17) Uani 1 1 d . . . H33J H 1.2282 0.5862 0.8338 0.041 Uiso 1 1 calc R . . C339 C 1.1377(3) 0.5869(7) 0.8157(2) 0.0262(14) Uani 1 1 d . . . H33K H 1.1388 0.5182 0.7996 0.031 Uiso 1 1 calc R . . C340 C 0.9835(3) 0.5413(6) 0.8253(2) 0.0241(14) Uani 1 1 d . . . H34A H 0.9492 0.5044 0.8099 0.036 Uiso 1 1 calc R . . H34B H 0.9683 0.6027 0.8424 0.036 Uiso 1 1 calc R . . H34C H 1.0054 0.4810 0.8414 0.036 Uiso 1 1 calc R . . C341 C 1.2882(3) 0.5777(5) 0.72186(19) 0.0184(12) Uani 1 1 d . . . H34D H 1.2563 0.5177 0.7137 0.022 Uiso 1 1 calc R . . C342 C 1.3167(3) 0.6207(6) 0.6853(2) 0.0219(13) Uani 1 1 d . . . C343 C 1.3048(3) 0.5603(6) 0.6496(2) 0.0254(14) Uani 1 1 d . . . H34E H 1.2800 0.4914 0.6486 0.030 Uiso 1 1 calc R . . C344 C 1.3292(4) 0.6014(8) 0.6159(3) 0.0367(18) Uani 1 1 d . . . H34F H 1.3206 0.5611 0.5915 0.044 Uiso 1 1 calc R . . C345 C 1.3657(4) 0.6998(7) 0.6172(3) 0.0363(18) Uani 1 1 d . . . H34G H 1.3819 0.7280 0.5938 0.044 Uiso 1 1 calc R . . C346 C 1.3792(3) 0.7583(7) 0.6526(2) 0.0322(16) Uani 1 1 d . . . H34H H 1.4057 0.8248 0.6536 0.039 Uiso 1 1 calc R . . C347 C 1.3544(3) 0.7202(6) 0.6863(2) 0.0258(14) Uani 1 1 d . . . H34I H 1.3629 0.7618 0.7103 0.031 Uiso 1 1 calc R . . C348 C 1.3347(3) 0.5193(6) 0.7514(2) 0.0250(14) Uani 1 1 d . . . H34J H 1.3148 0.4957 0.7750 0.038 Uiso 1 1 calc R . . H34K H 1.3674 0.5758 0.7587 0.038 Uiso 1 1 calc R . . H34L H 1.3518 0.4491 0.7393 0.038 Uiso 1 1 calc R . . Cl1 Cl 0.91629(8) 0.86549(15) 0.82812(5) 0.0278(3) Uani 1 1 d . . . Cl2 Cl 0.97561(9) 0.2956(2) 0.74476(6) 0.0395(4) Uani 1 1 d . . . Cl3 Cl 1.27259(7) 0.27051(17) 0.43745(5) 0.0332(4) Uani 1 1 d . . . Cl4 Cl 0.57658(9) 0.87244(17) 1.16127(6) 0.0326(4) Uani 1 1 d . . . Cl5 Cl 1.28801(8) 0.84328(15) 0.51574(5) 0.0289(4) Uani 1 1 d . . . Cl6 Cl 1.18514(9) 0.36823(17) 0.60906(6) 0.0337(4) Uani 1 1 d . . . Cl7 Cl 1.48121(9) 0.3829(2) 0.28750(7) 0.0429(5) Uani 1 1 d . . . Cl8 Cl 0.63702(15) 0.3150(2) 1.07810(11) 0.0210(6) Uani 0.50 1 d P . . Cl9 Cl 0.83270(16) 0.4317(3) 0.93962(11) 0.0263(7) Uani 0.50 1 d P . . Cl10 Cl 1.1397(2) 0.2936(5) 0.46717(15) 0.0557(11) Uani 0.50 1 d P . . Cl11 Cl 0.8550(3) 0.2974(6) 0.78548(16) 0.0640(13) Uani 0.50 1 d P . . O11W O 0.7431(2) 0.5663(3) 0.99272(13) 0.0159(8) Uani 1 1 d . . . O12W O 0.6613(4) 0.3811(7) 0.9888(3) 0.069(2) Uani 1 1 d . . . O13W O 0.7717(4) 0.4063(7) 1.0599(2) 0.067(2) Uani 1 1 d . . . O14W O 0.9994(3) 0.6030(6) 1.18747(18) 0.0416(14) Uani 1 1 d . . . O15W O 0.4825(3) 0.8215(7) 0.8704(2) 0.0544(18) Uani 1 1 d . . . O16W O 0.7726(4) 0.2573(9) 0.9917(3) 0.029(2) Uiso 0.50 1 d P . . O17W O 0.8900(5) 0.2992(11) 0.8721(3) 0.036(2) Uiso 0.50 1 d P . . O18W O 0.8785(5) 0.2856(13) 0.9112(4) 0.044(3) Uiso 0.50 1 d P . . O19W O 0.4840(6) 0.6007(11) 0.8112(4) 0.041(3) Uiso 0.50 1 d P . . O20W O 0.8084(3) 0.3080(7) 0.9822(2) 0.0130(15) Uiso 0.50 1 d P . . O21W O 0.6404(4) 0.2951(9) 1.0969(3) 0.0193(19) Uiso 0.50 1 d P . . O22W O 1.3362(3) 0.3968(5) 0.30405(18) 0.0354(12) Uani 1 1 d . . . O23W O 1.4737(3) 0.4247(6) 0.38124(19) 0.0443(15) Uani 1 1 d . . . O24W O 1.3669(3) 0.2856(6) 0.37351(19) 0.0466(14) Uani 1 1 d . . . O25W O 1.1537(4) 0.6034(9) 0.1550(2) 0.073(3) Uani 1 1 d . . . O26W O 1.7311(3) 0.6206(5) 0.48611(16) 0.0335(12) Uani 1 1 d . . . O27W O 1.5484(3) 0.3109(8) 0.2138(2) 0.065(2) Uani 1 1 d . . . O28W O 1.6912(2) 0.8113(5) 0.43699(16) 0.0336(12) Uani 1 1 d . . . O29W O 1.4130(2) 0.5868(4) 0.32697(14) 0.0202(9) Uani 1 1 d . . . O30W O 1.3287(3) 0.7868(7) 0.80271(19) 0.0483(15) Uani 1 1 d . . . O31W O 1.09402(19) 0.5370(4) 0.66480(13) 0.0151(8) Uani 1 1 d . . . O32W O 1.0016(2) 0.3624(5) 0.65577(19) 0.0380(13) Uani 1 1 d . . . O33W O 1.1126(3) 0.3873(5) 0.73344(17) 0.0398(14) Uani 1 1 d . . . O34W O 1.1099(3) 0.2332(5) 0.66842(19) 0.0413(14) Uani 1 1 d . . . O35W O 0.8449(3) 0.6820(5) 0.45987(17) 0.0365(13) Uani 1 1 d . . . O36W O 1.3421(4) 0.6033(9) 0.8587(2) 0.067(2) Uani 1 1 d . . . O37W O 1.0103(3) 0.2694(6) 0.87301(19) 0.0496(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01618(10) 0.01302(10) 0.01187(11) 0.00103(11) 0.00230(8) 0.00129(9) O11 0.019(2) 0.020(2) 0.0069(19) 0.0017(15) 0.0060(15) -0.0050(15) O12 0.020(2) 0.020(2) 0.0075(19) 0.0022(15) -0.0002(15) 0.0036(16) O13 0.023(2) 0.016(2) 0.014(2) 0.0043(15) 0.0027(17) 0.0081(16) O14 0.020(2) 0.026(2) 0.012(2) 0.0025(16) -0.0017(17) 0.0004(17) N11 0.029(3) 0.014(2) 0.008(2) 0.0042(17) -0.001(2) -0.005(2) N12 0.027(3) 0.013(2) 0.022(3) 0.004(2) 0.002(2) 0.003(2) N13 0.025(3) 0.017(2) 0.017(3) -0.001(2) 0.003(2) 0.006(2) N14 0.030(3) 0.017(2) 0.007(2) 0.0015(18) 0.003(2) -0.002(2) N15 0.022(3) 0.030(3) 0.019(3) 0.003(2) 0.007(2) -0.003(2) N16 0.022(3) 0.026(3) 0.019(3) 0.001(2) -0.003(2) 0.000(2) N17 0.026(3) 0.021(3) 0.013(2) 0.0003(19) 0.004(2) 0.004(2) N18 0.017(3) 0.030(3) 0.014(3) 0.000(2) -0.001(2) 0.000(2) C101 0.028(3) 0.019(3) 0.015(3) 0.005(2) -0.003(2) -0.006(2) C102 0.023(3) 0.020(3) 0.024(3) 0.009(2) 0.003(3) -0.003(2) C103 0.034(4) 0.018(3) 0.027(4) 0.009(3) 0.005(3) 0.010(3) C104 0.023(3) 0.028(3) 0.028(4) 0.005(3) 0.000(3) 0.014(3) C105 0.036(4) 0.020(3) 0.027(4) -0.003(3) 0.004(3) 0.012(3) C106 0.040(4) 0.018(3) 0.017(3) -0.005(2) 0.009(3) -0.002(3) C107 0.034(4) 0.022(3) 0.019(3) 0.001(2) 0.000(3) -0.009(3) C108 0.033(4) 0.030(3) 0.013(3) -0.004(2) 0.001(3) -0.012(3) C109 0.023(3) 0.035(3) 0.008(3) 0.003(2) 0.005(2) -0.004(3) C110 0.019(3) 0.026(3) 0.014(3) 0.007(2) 0.008(2) 0.005(3) C111 0.023(3) 0.025(3) 0.017(3) -0.001(2) -0.003(2) 0.001(3) C112 0.019(3) 0.026(4) 0.010(2) 0.001(2) 0.0002(19) 0.007(3) C113 0.025(3) 0.025(3) 0.018(3) 0.003(2) 0.006(3) 0.014(3) C114 0.018(3) 0.021(3) 0.018(3) -0.003(2) -0.002(2) 0.001(2) C115 0.026(3) 0.029(3) 0.006(3) -0.001(2) -0.006(2) -0.001(3) C116 0.018(3) 0.023(3) 0.014(3) 0.000(2) 0.000(2) -0.001(2) C117 0.021(3) 0.033(4) 0.023(3) -0.004(3) 0.009(3) -0.002(3) C118 0.022(3) 0.055(5) 0.019(3) -0.018(3) 0.005(3) -0.006(3) C119 0.031(4) 0.064(6) 0.039(5) -0.022(4) 0.007(4) -0.013(4) C120 0.018(4) 0.113(10) 0.051(6) -0.039(6) -0.001(4) 0.000(5) C121 0.041(5) 0.102(10) 0.033(5) -0.016(6) -0.010(4) 0.022(6) C122 0.056(6) 0.082(8) 0.032(5) -0.004(5) -0.009(4) 0.026(6) C123 0.034(4) 0.045(5) 0.021(3) 0.000(3) -0.007(3) 0.002(4) C124 0.036(4) 0.041(4) 0.036(5) -0.014(3) 0.014(3) 0.004(3) C125 0.018(3) 0.028(3) 0.026(4) -0.004(3) -0.001(3) 0.002(2) C126 0.029(4) 0.026(3) 0.020(3) -0.001(3) 0.005(3) -0.006(3) C127 0.044(5) 0.029(4) 0.030(4) -0.002(3) 0.000(3) -0.008(3) C128 0.058(6) 0.041(5) 0.029(4) 0.005(4) -0.002(4) -0.016(4) C129 0.067(6) 0.045(5) 0.021(4) -0.009(3) 0.013(4) -0.021(4) C130 0.034(4) 0.040(4) 0.039(4) -0.012(4) 0.012(3) -0.006(4) C131 0.031(4) 0.036(4) 0.030(4) -0.002(3) 0.006(3) -0.005(3) C132 0.027(4) 0.045(4) 0.026(4) -0.005(3) -0.001(3) -0.011(3) C133 0.024(3) 0.020(3) 0.021(3) 0.006(2) 0.005(3) 0.001(2) C134 0.029(3) 0.020(3) 0.018(3) 0.007(2) 0.000(3) -0.001(2) C135 0.029(4) 0.035(4) 0.019(3) 0.001(3) -0.002(3) 0.008(3) C136 0.029(4) 0.048(5) 0.030(4) 0.006(3) -0.002(3) 0.006(3) C137 0.031(4) 0.041(4) 0.025(4) 0.006(3) -0.004(3) -0.007(3) C138 0.039(4) 0.028(3) 0.029(3) 0.002(3) 0.003(3) -0.013(4) C139 0.027(3) 0.022(3) 0.023(3) 0.004(3) 0.003(2) -0.004(3) C140 0.030(4) 0.026(3) 0.019(3) 0.002(3) 0.006(3) -0.003(3) C141 0.027(4) 0.034(4) 0.025(4) -0.006(3) -0.009(3) 0.008(3) C142 0.016(8) 0.021(8) 0.015(6) -0.010(5) -0.007(5) -0.002(6) C143 0.031(8) 0.035(8) 0.024(8) -0.006(6) -0.009(6) 0.009(6) C144 0.061(16) 0.059(16) 0.023(9) -0.005(9) 0.016(10) 0.033(14) C145 0.043(11) 0.044(10) 0.045(12) 0.018(8) 0.017(9) 0.020(8) C146 0.037(8) 0.020(7) 0.066(11) 0.015(7) 0.013(8) 0.005(6) C147 0.012(6) 0.019(7) 0.050(10) -0.003(6) -0.006(6) -0.001(5) C42A 0.018(8) 0.033(9) 0.013(7) -0.002(6) 0.001(5) 0.001(6) C43A 0.049(10) 0.035(8) 0.013(7) -0.004(6) 0.007(6) 0.003(7) C44A 0.074(14) 0.059(12) 0.015(8) -0.003(7) 0.007(8) 0.003(11) C45A 0.036(11) 0.044(12) 0.030(9) 0.013(9) 0.020(9) 0.017(9) C46A 0.038(10) 0.027(8) 0.040(11) 0.008(7) 0.013(8) 0.016(7) C47A 0.013(7) 0.035(9) 0.039(10) 0.007(7) -0.006(6) -0.001(6) C148 0.025(4) 0.031(4) 0.030(4) 0.008(3) 0.001(3) 0.003(3) Yb2 0.01115(12) 0.01484(14) 0.01283(10) 0.00322(9) 0.00173(8) -0.00081(11) O21 0.0160(19) 0.023(2) 0.014(2) -0.0008(16) -0.0006(16) -0.0005(16) O22 0.0182(19) 0.038(3) 0.0154(19) -0.006(2) 0.0068(15) -0.0064(19) O23 0.0116(19) 0.021(2) 0.025(2) 0.0087(17) 0.0022(16) 0.0001(16) O24 0.012(2) 0.024(2) 0.021(2) 0.0014(17) 0.0049(17) -0.0002(16) N21 0.016(2) 0.017(2) 0.015(2) -0.0031(19) 0.0002(19) -0.0017(19) N22 0.015(2) 0.031(3) 0.010(2) 0.003(2) -0.0002(19) -0.002(2) N23 0.013(2) 0.018(2) 0.025(3) 0.013(2) 0.000(2) -0.0003(19) N24 0.016(3) 0.027(3) 0.021(3) 0.000(2) -0.002(2) 0.003(2) N25 0.012(2) 0.020(3) 0.032(3) -0.005(2) -0.003(2) 0.0008(19) N26 0.029(3) 0.039(4) 0.022(3) -0.009(3) 0.013(2) -0.009(3) N27 0.018(3) 0.024(3) 0.026(3) 0.011(2) -0.005(2) -0.005(2) N28 0.016(2) 0.031(3) 0.019(3) 0.002(2) 0.006(2) 0.005(2) C201 0.022(3) 0.017(3) 0.031(4) 0.002(3) -0.003(3) -0.009(2) C202 0.016(3) 0.026(3) 0.020(3) -0.001(2) 0.002(2) -0.009(2) C203 0.026(4) 0.025(3) 0.031(4) 0.012(3) 0.001(3) -0.005(3) C204 0.025(3) 0.020(3) 0.025(3) 0.013(3) 0.001(3) -0.006(2) C205 0.026(3) 0.023(3) 0.026(4) 0.008(3) 0.000(3) 0.003(3) C206 0.011(3) 0.035(4) 0.030(4) 0.003(3) 0.003(3) 0.007(2) C207 0.024(3) 0.026(3) 0.025(3) -0.010(3) 0.004(3) 0.004(3) C208 0.022(3) 0.025(3) 0.027(4) -0.011(3) 0.002(3) 0.003(3) C209 0.021(3) 0.024(3) 0.010(3) -0.007(2) -0.001(2) 0.005(2) C210 0.014(2) 0.022(3) 0.016(3) 0.002(2) -0.003(2) -0.007(2) C211 0.016(3) 0.036(4) 0.016(3) 0.001(3) 0.007(2) -0.011(3) C212 0.015(3) 0.023(3) 0.025(3) 0.000(3) 0.007(2) -0.001(3) C213 0.023(3) 0.027(4) 0.023(3) 0.010(3) -0.005(3) -0.009(3) C214 0.012(2) 0.022(3) 0.028(3) 0.005(3) -0.001(2) 0.000(2) C215 0.013(3) 0.037(4) 0.022(3) 0.003(3) 0.006(2) 0.005(3) C216 0.016(3) 0.031(3) 0.017(3) -0.001(2) 0.013(2) -0.002(2) C217 0.010(3) 0.025(3) 0.028(3) -0.003(3) -0.002(2) 0.004(2) C218 0.015(3) 0.024(3) 0.031(4) -0.001(3) -0.003(3) 0.007(2) C219 0.029(4) 0.054(5) 0.032(4) -0.005(4) -0.001(3) -0.008(3) C220 0.056(6) 0.073(7) 0.026(5) -0.005(4) 0.006(4) 0.003(5) C221 0.056(6) 0.062(6) 0.040(5) 0.012(5) 0.023(5) 0.010(5) C222 0.031(4) 0.031(4) 0.059(6) 0.012(4) 0.016(4) 0.007(3) C223 0.027(4) 0.027(4) 0.044(5) 0.000(3) 0.008(3) 0.006(3) C224 0.028(4) 0.030(4) 0.025(4) 0.004(3) 0.000(3) 0.007(3) C225 0.045(5) 0.040(4) 0.029(4) -0.015(3) 0.013(3) -0.015(4) C226 0.025(4) 0.055(5) 0.040(5) -0.032(4) 0.005(3) -0.002(3) C227 0.034(5) 0.057(6) 0.068(7) -0.025(5) 0.016(5) -0.010(4) C228 0.027(4) 0.057(6) 0.105(10) -0.023(7) 0.002(5) -0.006(4) C229 0.046(6) 0.074(9) 0.105(11) -0.039(8) -0.014(7) 0.016(6) C230 0.051(6) 0.070(7) 0.069(8) -0.016(6) -0.015(6) 0.024(5) C231 0.027(4) 0.062(6) 0.041(4) -0.008(5) 0.004(3) 0.001(4) C232 0.043(5) 0.042(4) 0.025(4) -0.008(3) 0.006(3) 0.005(4) C233 0.017(3) 0.020(3) 0.020(3) 0.005(2) 0.000(2) -0.001(2) C234 0.014(3) 0.018(3) 0.024(3) 0.005(2) 0.001(2) -0.007(2) C235 0.026(3) 0.022(3) 0.023(3) 0.002(3) 0.003(3) 0.002(3) C236 0.038(4) 0.026(4) 0.028(4) 0.003(3) 0.003(3) 0.004(3) C237 0.025(4) 0.039(4) 0.028(4) -0.011(3) 0.002(3) -0.006(3) C238 0.021(3) 0.027(3) 0.039(4) -0.006(3) 0.003(3) -0.001(3) C239 0.018(3) 0.016(3) 0.034(4) 0.003(2) -0.002(3) -0.002(2) C240 0.023(3) 0.029(3) 0.021(3) 0.004(3) -0.003(3) -0.007(3) C241 0.020(3) 0.022(3) 0.017(3) 0.003(2) 0.005(2) 0.000(2) C242 0.028(3) 0.020(3) 0.013(3) 0.002(2) -0.002(2) -0.004(2) C243 0.021(3) 0.033(4) 0.026(4) 0.002(3) -0.001(3) 0.000(3) C244 0.021(3) 0.042(4) 0.023(3) 0.008(3) 0.000(3) 0.000(3) C245 0.031(4) 0.029(4) 0.037(4) 0.013(3) -0.014(3) -0.013(3) C246 0.045(4) 0.020(4) 0.038(4) -0.001(3) -0.016(3) 0.001(3) C247 0.025(3) 0.025(4) 0.021(3) -0.005(3) 0.005(3) 0.001(3) C248 0.019(3) 0.027(3) 0.023(3) 0.002(3) 0.004(3) -0.001(2) Yb3 0.00702(11) 0.01649(15) 0.01093(10) 0.00076(9) 0.00407(8) -0.00010(10) O31 0.0081(18) 0.019(2) 0.017(2) -0.0032(16) 0.0058(15) -0.0011(15) O32 0.0145(19) 0.021(2) 0.0070(19) 0.0005(15) 0.0033(15) -0.0018(16) O33 0.015(2) 0.026(2) 0.015(2) -0.0036(17) 0.0077(16) -0.0024(17) O34 0.013(2) 0.017(2) 0.023(2) 0.0004(17) 0.0050(17) 0.0031(16) N31 0.013(2) 0.015(2) 0.017(3) 0.0000(18) 0.0078(19) 0.0007(18) N32 0.012(2) 0.016(2) 0.012(2) 0.0005(18) 0.0013(18) -0.0009(18) N33 0.013(2) 0.020(2) 0.012(2) 0.0003(18) 0.0055(18) -0.0050(18) N34 0.008(2) 0.019(2) 0.013(2) -0.0040(18) 0.0033(17) 0.0034(17) N35 0.012(2) 0.021(2) 0.021(3) -0.003(2) 0.008(2) 0.0001(19) N36 0.013(2) 0.023(2) 0.016(3) 0.006(2) 0.0010(19) -0.0030(19) N37 0.013(2) 0.023(3) 0.014(2) 0.0044(19) 0.0060(19) 0.0017(19) N38 0.014(2) 0.021(2) 0.021(3) 0.001(2) 0.000(2) 0.0051(19) C301 0.013(3) 0.013(3) 0.022(3) 0.001(2) 0.003(2) -0.003(2) C302 0.007(2) 0.024(3) 0.014(3) 0.005(2) 0.003(2) 0.002(2) C303 0.016(3) 0.021(3) 0.014(3) 0.007(2) 0.004(2) 0.008(2) C304 0.012(3) 0.023(3) 0.020(3) 0.001(2) -0.001(2) 0.005(2) C305 0.018(3) 0.021(3) 0.011(3) -0.001(2) 0.007(2) 0.003(2) C306 0.017(3) 0.018(3) 0.018(3) -0.008(2) 0.002(2) 0.002(2) C307 0.006(2) 0.019(3) 0.026(3) -0.003(2) 0.006(2) -0.002(2) C308 0.009(3) 0.022(3) 0.019(3) -0.007(2) 0.003(2) -0.003(2) C309 0.008(2) 0.023(3) 0.018(3) -0.001(2) 0.005(2) -0.001(2) C310 0.010(3) 0.016(3) 0.011(3) -0.002(2) 0.007(2) 0.001(2) C311 0.009(2) 0.030(3) 0.015(3) 0.001(2) 0.002(2) -0.004(2) C312 0.011(3) 0.016(3) 0.016(3) -0.004(2) 0.001(2) 0.001(2) C313 0.011(2) 0.030(3) 0.012(3) 0.004(2) 0.002(2) 0.000(2) C314 0.013(3) 0.021(3) 0.014(3) 0.001(2) 0.000(2) -0.007(2) C315 0.011(2) 0.025(3) 0.016(3) -0.001(2) -0.002(2) 0.005(2) C316 0.015(3) 0.012(3) 0.016(3) 0.002(2) 0.003(2) -0.001(2) C317 0.019(3) 0.022(3) 0.014(3) -0.001(2) 0.004(2) -0.002(2) C318 0.018(3) 0.022(3) 0.017(3) -0.007(2) 0.001(2) 0.000(2) C319 0.025(3) 0.030(3) 0.020(3) -0.002(3) 0.005(3) -0.009(3) C320 0.018(3) 0.040(4) 0.036(4) -0.005(3) 0.005(3) -0.008(3) C321 0.021(3) 0.045(5) 0.034(4) -0.004(4) 0.000(3) 0.005(3) C322 0.027(3) 0.025(4) 0.033(4) 0.004(3) 0.008(3) 0.004(3) C323 0.019(3) 0.022(3) 0.035(4) -0.004(3) 0.007(2) -0.003(3) C324 0.021(3) 0.024(3) 0.027(4) -0.008(3) 0.004(3) 0.005(2) C325 0.009(2) 0.018(3) 0.017(3) 0.000(2) 0.006(2) 0.001(2) C326 0.006(2) 0.020(3) 0.019(3) -0.004(2) 0.006(2) -0.004(2) C327 0.010(3) 0.020(3) 0.029(4) -0.003(2) 0.002(2) 0.002(2) C328 0.018(3) 0.021(3) 0.029(3) -0.009(3) 0.002(2) 0.000(3) C329 0.011(3) 0.030(3) 0.028(3) -0.008(3) 0.007(2) -0.006(2) C330 0.024(3) 0.030(3) 0.020(3) 0.003(3) 0.004(3) -0.007(3) C331 0.019(3) 0.021(3) 0.022(3) 0.000(2) 0.004(2) -0.001(2) C332 0.015(3) 0.023(3) 0.025(3) -0.003(2) 0.002(2) -0.002(2) C333 0.020(3) 0.021(3) 0.014(3) 0.001(2) 0.003(2) -0.002(2) C334 0.023(3) 0.026(3) 0.012(3) 0.006(2) 0.001(2) 0.000(2) C335 0.026(3) 0.019(3) 0.025(3) 0.003(3) 0.000(3) -0.001(3) C336 0.031(3) 0.033(4) 0.032(4) -0.001(3) -0.002(3) -0.006(3) C337 0.027(4) 0.046(5) 0.031(4) 0.007(3) -0.007(3) -0.007(3) C338 0.027(4) 0.042(4) 0.032(4) 0.013(3) -0.007(3) 0.008(3) C339 0.023(3) 0.034(4) 0.021(3) 0.004(3) -0.001(3) 0.010(3) C340 0.024(3) 0.025(3) 0.023(3) 0.009(3) 0.003(3) -0.006(3) C341 0.018(3) 0.015(3) 0.022(3) 0.001(2) 0.001(2) 0.006(2) C342 0.015(3) 0.020(3) 0.030(4) 0.003(3) -0.002(2) 0.008(2) C343 0.027(3) 0.023(3) 0.026(4) 0.001(3) -0.004(3) 0.008(3) C344 0.033(4) 0.042(4) 0.035(4) 0.000(3) 0.004(3) 0.019(3) C345 0.029(4) 0.044(4) 0.037(5) 0.012(3) 0.004(3) 0.016(3) C346 0.019(3) 0.030(4) 0.048(4) 0.013(3) 0.006(3) 0.005(3) C347 0.019(3) 0.027(3) 0.031(4) 0.004(3) 0.001(3) 0.002(2) C348 0.018(3) 0.021(3) 0.036(4) 0.004(3) 0.003(3) 0.011(2) Cl1 0.0314(9) 0.0284(8) 0.0249(9) 0.0021(6) 0.0113(7) 0.0014(7) Cl2 0.0443(10) 0.0367(9) 0.0388(9) 0.0004(9) 0.0114(8) -0.0016(9) Cl3 0.0246(7) 0.0416(10) 0.0326(8) 0.0027(8) -0.0027(6) -0.0003(7) Cl4 0.0360(10) 0.0337(9) 0.0290(9) -0.0040(7) 0.0081(8) 0.0063(7) Cl5 0.0334(9) 0.0242(8) 0.0310(9) -0.0029(6) 0.0155(7) -0.0045(6) Cl6 0.0319(9) 0.0378(9) 0.0318(9) 0.0034(7) 0.0058(7) 0.0020(7) Cl7 0.0283(9) 0.0485(12) 0.0525(13) -0.0174(10) 0.0067(9) 0.0015(8) Cl8 0.0302(16) 0.0113(13) 0.0229(16) 0.0023(11) 0.0111(12) 0.0002(10) Cl9 0.0256(16) 0.0258(15) 0.0284(17) 0.0010(12) 0.0069(13) 0.0028(12) Cl10 0.052(2) 0.056(3) 0.058(3) -0.007(3) -0.004(2) -0.001(2) Cl11 0.069(3) 0.064(3) 0.056(3) -0.010(3) -0.011(2) -0.010(3) O11W 0.020(2) 0.0100(18) 0.018(2) 0.0018(15) 0.0014(16) -0.0003(15) O12W 0.051(5) 0.061(5) 0.096(7) -0.006(4) 0.009(4) -0.021(4) O13W 0.096(7) 0.055(4) 0.048(4) 0.008(3) -0.015(4) 0.009(4) O14W 0.037(3) 0.055(4) 0.033(3) 0.002(3) 0.004(3) 0.014(3) O15W 0.038(3) 0.069(5) 0.054(4) 0.013(4) -0.013(3) 0.014(3) O22W 0.027(3) 0.038(3) 0.041(3) -0.006(2) 0.002(2) -0.001(2) O23W 0.043(4) 0.051(4) 0.037(3) 0.020(3) -0.011(3) -0.006(3) O24W 0.048(3) 0.041(3) 0.052(3) 0.001(3) 0.008(3) -0.007(3) O25W 0.062(5) 0.112(7) 0.045(4) 0.013(4) 0.005(4) -0.042(5) O26W 0.035(3) 0.039(3) 0.026(3) 0.002(2) -0.002(2) -0.007(2) O27W 0.058(4) 0.088(6) 0.051(4) 0.026(4) 0.019(3) 0.034(4) O28W 0.021(2) 0.046(3) 0.034(3) -0.017(2) 0.002(2) -0.003(2) O29W 0.018(2) 0.022(2) 0.021(2) -0.0007(17) 0.0028(18) 0.0011(17) O30W 0.044(3) 0.048(4) 0.052(4) -0.012(3) -0.003(3) -0.013(3) O31W 0.0114(19) 0.020(2) 0.015(2) 0.0014(16) 0.0055(15) 0.0006(15) O32W 0.025(3) 0.039(3) 0.049(4) 0.002(3) -0.004(2) -0.002(2) O33W 0.048(4) 0.041(3) 0.029(3) 0.010(2) -0.010(3) -0.003(3) O34W 0.041(3) 0.031(3) 0.053(4) 0.004(3) 0.015(3) 0.010(2) O35W 0.029(3) 0.051(3) 0.029(3) -0.009(2) 0.002(2) 0.004(2) O36W 0.048(4) 0.122(7) 0.029(4) -0.004(4) 0.003(3) 0.010(4) O37W 0.059(4) 0.035(4) 0.051(4) 0.011(3) -0.023(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O12 2.256(4) . ? Yb1 O13 2.269(4) . ? Yb1 O14 2.289(4) . ? Yb1 O11 2.290(4) . ? Yb1 O11W 2.408(4) . ? Yb1 N14 2.596(5) . ? Yb1 N11 2.598(5) . ? Yb1 N13 2.624(5) . ? Yb1 N12 2.676(5) . ? Yb1 C114 3.163(6) . ? Yb1 C110 3.163(6) . ? Yb1 C112 3.177(6) . ? O11 C110 1.255(7) . ? O12 C112 1.268(7) . ? O13 C114 1.275(7) . ? O14 C116 1.261(8) . ? N11 C109 1.478(8) . ? N11 C101 1.487(8) . ? N11 C108 1.505(8) . ? N12 C111 1.475(8) . ? N12 C102 1.486(8) . ? N12 C103 1.494(8) . ? N13 C113 1.476(9) . ? N13 C105 1.489(9) . ? N13 C104 1.507(8) . ? N14 C106 1.487(8) . ? N14 C115 1.488(8) . ? N14 C107 1.509(8) . ? N15 C110 1.328(8) . ? N15 C117 1.475(9) . ? N15 H15A 0.8800 . ? N16 C112 1.321(8) . ? N16 C125 1.458(9) . ? N16 H16A 0.8800 . ? N17 C114 1.322(8) . ? N17 C133 1.477(8) . ? N17 H17A 0.8800 . ? N18 C116 1.311(8) . ? N18 C141 1.464(9) . ? N18 H18A 0.8800 . ? C101 C102 1.525(9) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.510(10) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.518(10) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.498(10) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.513(10) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C111 C112 1.494(9) . ? C111 H11A 0.9900 . ? C111 H11B 0.9900 . ? C113 C114 1.494(8) . ? C113 H11C 0.9900 . ? C113 H11D 0.9900 . ? C115 C116 1.515(9) . ? C115 H11E 0.9900 . ? C115 H11F 0.9900 . ? C117 C124 1.524(10) . ? C117 C118 1.529(11) . ? C117 H11G 1.0000 . ? C118 C123 1.384(12) . ? C118 C119 1.390(11) . ? C119 C120 1.374(15) . ? C119 H11H 0.9500 . ? C120 C121 1.391(18) . ? C120 H12A 0.9500 . ? C121 C122 1.399(17) . ? C121 H12B 0.9500 . ? C122 C123 1.394(12) . ? C122 H12C 0.9500 . ? C123 H12D 0.9500 . ? C124 H12E 0.9800 . ? C124 H12F 0.9800 . ? C124 H12R 0.9800 . ? C125 C126 1.525(10) . ? C125 C132 1.539(10) . ? C125 H12G 1.0000 . ? C126 C131 1.379(11) . ? C126 C127 1.403(11) . ? C127 C128 1.412(13) . ? C127 H12H 0.9500 . ? C128 C129 1.339(14) . ? C128 H12I 0.9500 . ? C129 C130 1.384(13) . ? C129 H12J 0.9500 . ? C130 C131 1.399(11) . ? C130 H13A 0.9500 . ? C131 H13B 0.9500 . ? C132 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C133 C134 1.513(10) . ? C133 C140 1.531(9) . ? C133 H13F 1.0000 . ? C134 C135 1.385(10) . ? C134 C139 1.389(10) . ? C135 C136 1.398(11) . ? C135 H13G 0.9500 . ? C136 C137 1.350(12) . ? C136 H13H 0.9500 . ? C137 C138 1.400(12) . ? C137 H13I 0.9500 . ? C138 C139 1.386(10) . ? C138 H13J 0.9500 . ? C139 H13K 0.9500 . ? C140 H14A 0.9800 . ? C140 H14B 0.9800 . ? C140 H14C 0.9800 . ? C141 C42A 1.440(11) . ? C141 C148 1.530(10) . ? C141 C142 1.626(12) . ? C141 H14D 1.0000 . ? C142 C143 1.3900 . ? C142 C147 1.3900 . ? C143 C144 1.3900 . ? C143 H14E 0.9500 . ? C144 C145 1.3900 . ? C144 H14F 0.9500 . ? C145 C146 1.3900 . ? C145 H14G 0.9500 . ? C146 C147 1.3900 . ? C146 H14H 0.9500 . ? C147 H14I 0.9500 . ? C42A C43A 1.3900 . ? C42A C47A 1.3900 . ? C43A C44A 1.3900 . ? C43A H43A 0.9500 . ? C44A C45A 1.3900 . ? C44A H44A 0.9500 . ? C45A C46A 1.3900 . ? C45A H45A 0.9500 . ? C46A C47A 1.3900 . ? C46A H46A 0.9500 . ? C47A H47A 0.9500 . ? C148 H14J 0.9800 . ? C148 H14K 0.9800 . ? C148 H14L 0.9800 . ? Yb2 O24 2.261(5) . ? Yb2 O22 2.272(4) . ? Yb2 O21 2.278(4) . ? Yb2 O23 2.302(4) . ? Yb2 O29W 2.388(4) . ? Yb2 N24 2.614(6) . ? Yb2 N23 2.616(5) . ? Yb2 N22 2.617(5) . ? Yb2 N21 2.630(5) . ? Yb2 C216 3.161(6) . ? Yb2 C212 3.166(6) . ? Yb2 C214 3.184(6) . ? O21 C210 1.259(7) . ? O22 C212 1.262(8) . ? O23 C214 1.253(7) . ? O24 C216 1.268(7) . ? N21 C201 1.458(8) . ? N21 C209 1.489(8) . ? N21 C208 1.490(8) . ? N22 C202 1.483(8) . ? N22 C211 1.492(8) . ? N22 C203 1.494(8) . ? N23 C204 1.475(8) . ? N23 C213 1.484(9) . ? N23 C205 1.506(9) . ? N24 C206 1.481(8) . ? N24 C215 1.505(9) . ? N24 C207 1.508(9) . ? N25 C210 1.310(8) . ? N25 C217 1.470(8) . ? N25 H25A 0.8800 . ? N26 C212 1.303(8) . ? N26 C225 1.471(9) . ? N26 H26A 0.8800 . ? N27 C214 1.316(8) . ? N27 C233 1.485(8) . ? N27 H27A 0.8800 . ? N28 C216 1.320(9) . ? N28 C241 1.473(8) . ? N28 H28A 0.8800 . ? C201 C202 1.524(10) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.514(10) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.517(10) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.493(10) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.508(9) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C211 C212 1.500(9) . ? C211 H21A 0.9900 . ? C211 H21B 0.9900 . ? C213 C214 1.505(9) . ? C213 H21C 0.9900 . ? C213 H21D 0.9900 . ? C215 C216 1.499(10) . ? C215 H21E 0.9900 . ? C215 H21F 0.9900 . ? C217 C218 1.506(10) . ? C217 C224 1.523(9) . ? C217 H21G 1.0000 . ? C218 C223 1.384(10) . ? C218 C219 1.385(11) . ? C219 C220 1.382(13) . ? C219 H21H 0.9500 . ? C220 C221 1.375(16) . ? C220 H22A 0.9500 . ? C221 C222 1.380(15) . ? C221 H22B 0.9500 . ? C222 C223 1.402(12) . ? C222 H22C 0.9500 . ? C223 H22D 0.9500 . ? C224 H22E 0.9800 . ? C224 H22F 0.9800 . ? C224 H22G 0.9800 . ? C225 C232 1.522(11) . ? C225 C226 1.530(13) . ? C225 H22H 1.0000 . ? C226 C231 1.361(14) . ? C226 C227 1.402(12) . ? C227 C228 1.424(17) . ? C227 H22I 0.9500 . ? C228 C229 1.320(19) . ? C228 H22K 0.9500 . ? C229 C230 1.390(18) . ? C229 H22L 0.9500 . ? C230 C231 1.406(13) . ? C230 H23A 0.9500 . ? C231 H23B 0.9500 . ? C232 H23C 0.9800 . ? C232 H23D 0.9800 . ? C232 H23E 0.9800 . ? C233 C234 1.509(9) . ? C233 C240 1.525(9) . ? C233 H23F 1.0000 . ? C234 C235 1.389(9) . ? C234 C239 1.392(9) . ? C235 C236 1.391(10) . ? C235 H23G 0.9500 . ? C236 C237 1.407(11) . ? C236 H23H 0.9500 . ? C237 C238 1.370(11) . ? C237 H23I 0.9500 . ? C238 C239 1.403(11) . ? C238 H23J 0.9500 . ? C239 H23K 0.9500 . ? C240 H24A 0.9800 . ? C240 H24B 0.9800 . ? C240 H24C 0.9800 . ? C241 C248 1.528(9) . ? C241 C242 1.529(9) . ? C241 H24D 1.0000 . ? C242 C243 1.386(10) . ? C242 C247 1.407(9) . ? C243 C244 1.390(10) . ? C243 H24E 0.9500 . ? C244 C245 1.397(11) . ? C244 H24F 0.9500 . ? C245 C246 1.379(12) . ? C245 H24G 0.9500 . ? C246 C247 1.394(10) . ? C246 H24H 0.9500 . ? C247 H24I 0.9500 . ? C248 H24J 0.9800 . ? C248 H24K 0.9800 . ? C248 H24L 0.9800 . ? Yb3 O32 2.265(4) . ? Yb3 O34 2.286(4) . ? Yb3 O33 2.289(4) . ? Yb3 O31 2.293(4) . ? Yb3 O31W 2.448(4) . ? Yb3 N31 2.611(5) . ? Yb3 N33 2.616(5) . ? Yb3 N32 2.623(5) . ? Yb3 N34 2.633(5) . ? Yb3 C314 3.154(6) . ? Yb3 C312 3.162(6) . ? Yb3 C316 3.170(6) . ? O31 C310 1.271(7) . ? O32 C312 1.261(8) . ? O33 C314 1.238(8) . ? O34 C316 1.253(8) . ? N31 C309 1.465(7) . ? N31 C301 1.497(8) . ? N31 C308 1.499(8) . ? N32 C303 1.490(7) . ? N32 C302 1.490(7) . ? N32 C311 1.496(7) . ? N33 C313 1.481(7) . ? N33 C304 1.485(8) . ? N33 C305 1.501(8) . ? N34 C315 1.478(7) . ? N34 C306 1.489(7) . ? N34 C307 1.497(8) . ? N35 C310 1.321(8) . ? N35 C317 1.452(8) . ? N35 H35A 0.8800 . ? N36 C312 1.319(8) . ? N36 C325 1.475(7) . ? N36 H36A 0.8800 . ? N37 C314 1.330(8) . ? N37 C333 1.472(8) . ? N37 H37A 0.8800 . ? N38 C316 1.322(8) . ? N38 C341 1.471(8) . ? N38 H38A 0.8800 . ? C301 C302 1.514(8) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C303 C304 1.515(8) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C305 C306 1.517(9) . ? C305 H30I 0.9900 . ? C305 H30J 0.9900 . ? C306 H30K 0.9900 . ? C306 H30L 0.9900 . ? C307 C308 1.508(8) . ? C307 H30M 0.9900 . ? C307 H30N 0.9900 . ? C308 H30O 0.9900 . ? C308 H30P 0.9900 . ? C309 C310 1.492(8) . ? C309 H30Q 0.9900 . ? C309 H30R 0.9900 . ? C311 C312 1.507(8) . ? C311 H31A 0.9900 . ? C311 H31B 0.9900 . ? C313 C314 1.507(9) . ? C313 H31C 0.9900 . ? C313 H31D 0.9900 . ? C315 C316 1.495(8) . ? C315 H31E 0.9900 . ? C315 H31F 0.9900 . ? C317 C324 1.514(9) . ? C317 C318 1.539(9) . ? C317 H31G 1.0000 . ? C318 C319 1.389(9) . ? C318 C323 1.391(9) . ? C319 C320 1.390(11) . ? C319 H31H 0.9500 . ? C320 C321 1.401(12) . ? C320 H32A 0.9500 . ? C321 C322 1.369(11) . ? C321 H32B 0.9500 . ? C322 C323 1.380(10) . ? C322 H32C 0.9500 . ? C323 H32D 0.9500 . ? C324 H32E 0.9800 . ? C324 H32F 0.9800 . ? C324 H32G 0.9800 . ? C325 C326 1.509(8) . ? C325 C332 1.538(9) . ? C325 H32H 1.0000 . ? C326 C331 1.389(9) . ? C326 C327 1.404(8) . ? C327 C328 1.397(9) . ? C327 H32I 0.9500 . ? C328 C329 1.396(10) . ? C328 H32J 0.9500 . ? C329 C330 1.402(10) . ? C329 H32K 0.9500 . ? C330 C331 1.388(10) . ? C330 H33A 0.9500 . ? C331 H33B 0.9500 . ? C332 H33C 0.9800 . ? C332 H33D 0.9800 . ? C332 H33E 0.9800 . ? C333 C334 1.517(9) . ? C333 C340 1.524(9) . ? C333 H33F 1.0000 . ? C334 C335 1.388(10) . ? C334 C339 1.391(9) . ? C335 C336 1.406(10) . ? C335 H33G 0.9500 . ? C336 C337 1.412(12) . ? C336 H33H 0.9500 . ? C337 C338 1.382(13) . ? C337 H33I 0.9500 . ? C338 C339 1.399(11) . ? C338 H33J 0.9500 . ? C339 H33K 0.9500 . ? C340 H34A 0.9800 . ? C340 H34B 0.9800 . ? C340 H34C 0.9800 . ? C341 C342 1.511(9) . ? C341 C348 1.531(9) . ? C341 H34D 1.0000 . ? C342 C347 1.396(10) . ? C342 C343 1.400(10) . ? C343 C344 1.381(12) . ? C343 H34E 0.9500 . ? C344 C345 1.371(13) . ? C344 H34F 0.9500 . ? C345 C346 1.384(12) . ? C345 H34G 0.9500 . ? C346 C347 1.372(10) . ? C346 H34H 0.9500 . ? C347 H34I 0.9500 . ? C348 H34J 0.9800 . ? C348 H34K 0.9800 . ? C348 H34L 0.9800 . ? Cl8 O21W 0.676(9) . ? Cl9 O20W 2.106(8) . ? O16W O20W 1.045(12) . ? O17W O18W 1.378(16) . ? 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 O12 Yb1 O13 83.60(16) . . ? O12 Yb1 O14 142.00(16) . . ? O13 Yb1 O14 84.44(16) . . ? O12 Yb1 O11 80.89(15) . . ? O13 Yb1 O11 142.51(15) . . ? O14 Yb1 O11 87.16(16) . . ? O12 Yb1 O11W 71.96(15) . . ? O13 Yb1 O11W 71.39(15) . . ? O14 Yb1 O11W 70.05(15) . . ? O11 Yb1 O11W 71.39(15) . . ? O12 Yb1 N14 141.73(17) . . ? O13 Yb1 N14 74.22(16) . . ? O14 Yb1 N14 66.99(17) . . ? O11 Yb1 N14 134.34(16) . . ? O11W Yb1 N14 126.54(16) . . ? O12 Yb1 N11 131.27(15) . . ? O13 Yb1 N11 142.89(16) . . ? O14 Yb1 N11 74.00(17) . . ? O11 Yb1 N11 67.23(15) . . ? O11W Yb1 N11 125.52(16) . . ? N14 Yb1 N11 69.67(16) . . ? O12 Yb1 N13 73.97(17) . . ? O13 Yb1 N13 67.60(16) . . ? O14 Yb1 N13 132.59(17) . . ? O11 Yb1 N13 137.80(16) . . ? O11W Yb1 N13 128.63(16) . . ? N14 Yb1 N13 68.88(18) . . ? N11 Yb1 N13 105.85(17) . . ? O12 Yb1 N12 66.60(16) . . ? O13 Yb1 N12 130.99(16) . . ? O14 Yb1 N12 142.09(17) . . ? O11 Yb1 N12 71.87(16) . . ? O11W Yb1 N12 127.73(16) . . ? N14 Yb1 N12 105.72(17) . . ? N11 Yb1 N12 68.88(17) . . ? N13 Yb1 N12 67.23(17) . . ? O12 Yb1 C114 74.88(15) . . ? O13 Yb1 C114 19.52(15) . . ? O14 Yb1 C114 102.00(16) . . ? O11 Yb1 C114 150.79(16) . . ? O11W Yb1 C114 85.61(16) . . ? N14 Yb1 C114 73.98(16) . . ? N11 Yb1 C114 141.90(16) . . ? N13 Yb1 C114 48.71(17) . . ? N12 Yb1 C114 111.75(17) . . ? O12 Yb1 C110 98.66(16) . . ? O13 Yb1 C110 153.41(16) . . ? O14 Yb1 C110 77.56(16) . . ? O11 Yb1 C110 19.29(16) . . ? O11W Yb1 C110 84.05(16) . . ? N14 Yb1 C110 115.13(18) . . ? N11 Yb1 C110 48.70(17) . . ? N13 Yb1 C110 138.62(17) . . ? N12 Yb1 C110 72.49(17) . . ? C114 Yb1 C110 169.13(16) . . ? O12 Yb1 C112 18.75(15) . . ? O13 Yb1 C112 100.66(16) . . ? O14 Yb1 C112 151.51(16) . . ? O11 Yb1 C112 71.67(15) . . ? O11W Yb1 C112 84.92(16) . . ? N14 Yb1 C112 141.46(17) . . ? N11 Yb1 C112 112.76(16) . . ? N13 Yb1 C112 73.88(17) . . ? N12 Yb1 C112 48.66(17) . . ? C114 Yb1 C112 88.99(15) . . ? C110 Yb1 C112 86.77(15) . . ? C110 O11 Yb1 123.7(4) . . ? C112 O12 Yb1 126.4(4) . . ? C114 O13 Yb1 124.0(4) . . ? C116 O14 Yb1 124.7(4) . . ? C109 N11 C101 110.4(5) . . ? C109 N11 C108 108.7(5) . . ? C101 N11 C108 108.6(5) . . ? C109 N11 Yb1 106.3(4) . . ? C101 N11 Yb1 112.1(4) . . ? C108 N11 Yb1 110.7(4) . . ? C111 N12 C102 111.6(5) . . ? C111 N12 C103 109.4(5) . . ? C102 N12 C103 107.7(5) . . ? C111 N12 Yb1 106.5(4) . . ? C102 N12 Yb1 109.9(4) . . ? C103 N12 Yb1 111.7(4) . . ? C113 N13 C105 109.9(5) . . ? C113 N13 C104 109.1(5) . . ? C105 N13 C104 107.7(5) . . ? C113 N13 Yb1 107.0(4) . . ? C105 N13 Yb1 110.2(4) . . ? C104 N13 Yb1 113.0(4) . . ? C106 N14 C115 108.1(5) . . ? C106 N14 C107 109.3(5) . . ? C115 N14 C107 109.3(5) . . ? C106 N14 Yb1 112.3(4) . . ? C115 N14 Yb1 107.1(4) . . ? C107 N14 Yb1 110.7(4) . . ? C110 N15 C117 120.4(6) . . ? C110 N15 H15A 119.8 . . ? C117 N15 H15A 119.8 . . ? C112 N16 C125 120.2(5) . . ? C112 N16 H16A 119.9 . . ? C125 N16 H16A 119.9 . . ? C114 N17 C133 122.6(5) . . ? C114 N17 H17A 118.7 . . ? C133 N17 H17A 118.7 . . ? C116 N18 C141 121.4(6) . . ? C116 N18 H18A 119.3 . . ? C141 N18 H18A 119.3 . . ? N11 C101 C102 113.2(5) . . ? N11 C101 H10A 108.9 . . ? C102 C101 H10A 108.9 . . ? N11 C101 H10B 108.9 . . ? C102 C101 H10B 108.9 . . ? H10A C101 H10B 107.7 . . ? N12 C102 C101 112.1(6) . . ? N12 C102 H10C 109.2 . . ? C101 C102 H10C 109.2 . . ? N12 C102 H10D 109.2 . . ? C101 C102 H10D 109.2 . . ? H10C C102 H10D 107.9 . . ? N12 C103 C104 111.4(5) . . ? N12 C103 H10E 109.4 . . ? C104 C103 H10E 109.4 . . ? N12 C103 H10F 109.4 . . ? C104 C103 H10F 109.4 . . ? H10E C103 H10F 108.0 . . ? N13 C104 C103 110.8(6) . . ? N13 C104 H10G 109.5 . . ? C103 C104 H10G 109.5 . . ? N13 C104 H10H 109.5 . . ? C103 C104 H10H 109.5 . . ? H10G C104 H10H 108.1 . . ? N13 C105 C106 113.2(5) . . ? N13 C105 H10I 108.9 . . ? C106 C105 H10I 108.9 . . ? N13 C105 H10J 108.9 . . ? C106 C105 H10J 108.9 . . ? H10I C105 H10J 107.8 . . ? N14 C106 C105 110.4(5) . . ? N14 C106 H10K 109.6 . . ? C105 C106 H10K 109.6 . . ? N14 C106 H10L 109.6 . . ? C105 C106 H10L 109.6 . . ? H10K C106 H10L 108.1 . . ? C108 C107 N14 113.7(5) . . ? C108 C107 H10M 108.8 . . ? N14 C107 H10M 108.8 . . ? C108 C107 H10N 108.8 . . ? N14 C107 H10N 108.8 . . ? H10M C107 H10N 107.7 . . ? C107 C108 N11 110.9(6) . . ? C107 C108 H10O 109.5 . . ? N11 C108 H10O 109.5 . . ? C107 C108 H10P 109.5 . . ? N11 C108 H10P 109.5 . . ? H10O C108 H10P 108.1 . . ? N11 C109 C110 108.7(5) . . ? N11 C109 H10Q 109.9 . . ? C110 C109 H10Q 109.9 . . ? N11 C109 H10R 109.9 . . ? C110 C109 H10R 109.9 . . ? H10Q C109 H10R 108.3 . . ? O11 C110 N15 121.4(6) . . ? O11 C110 C109 119.7(5) . . ? N15 C110 C109 118.8(5) . . ? O11 C110 Yb1 37.1(3) . . ? N15 C110 Yb1 158.5(5) . . ? C109 C110 Yb1 82.7(3) . . ? N12 C111 C112 111.5(5) . . ? N12 C111 H11A 109.3 . . ? C112 C111 H11A 109.3 . . ? N12 C111 H11B 109.3 . . ? C112 C111 H11B 109.3 . . ? H11A C111 H11B 108.0 . . ? O12 C112 N16 119.3(6) . . ? O12 C112 C111 120.3(6) . . ? N16 C112 C111 120.3(5) . . ? O12 C112 Yb1 34.9(3) . . ? N16 C112 Yb1 154.0(4) . . ? C111 C112 Yb1 85.5(4) . . ? N13 C113 C114 110.2(5) . . ? N13 C113 H11C 109.6 . . ? C114 C113 H11C 109.6 . . ? N13 C113 H11D 109.6 . . ? C114 C113 H11D 109.6 . . ? H11C C113 H11D 108.1 . . ? O13 C114 N17 120.4(6) . . ? O13 C114 C113 120.9(5) . . ? N17 C114 C113 118.7(6) . . ? O13 C114 Yb1 36.5(3) . . ? N17 C114 Yb1 156.9(4) . . ? C113 C114 Yb1 84.4(4) . . ? N14 C115 C116 109.7(5) . . ? N14 C115 H11E 109.7 . . ? C116 C115 H11E 109.7 . . ? N14 C115 H11F 109.7 . . ? C116 C115 H11F 109.7 . . ? H11E C115 H11F 108.2 . . ? O14 C116 N18 123.6(6) . . ? O14 C116 C115 119.2(5) . . ? N18 C116 C115 117.1(6) . . ? O14 C116 Yb1 36.3(3) . . ? N18 C116 Yb1 159.4(5) . . ? C115 C116 Yb1 82.9(3) . . ? N15 C117 C124 108.6(6) . . ? N15 C117 C118 110.9(6) . . ? C124 C117 C118 111.2(6) . . ? N15 C117 H11G 108.7 . . ? C124 C117 H11G 108.7 . . ? C118 C117 H11G 108.7 . . ? C123 C118 C119 118.9(8) . . ? C123 C118 C117 121.9(7) . . ? C119 C118 C117 119.3(8) . . ? C120 C119 C118 121.4(10) . . ? C120 C119 H11H 119.3 . . ? C118 C119 H11H 119.3 . . ? C119 C120 C121 119.2(9) . . ? C119 C120 H12A 120.4 . . ? C121 C120 H12A 120.4 . . ? C120 C121 C122 120.9(10) . . ? C120 C121 H12B 119.6 . . ? C122 C121 H12B 119.6 . . ? C123 C122 C121 118.3(11) . . ? C123 C122 H12C 120.9 . . ? C121 C122 H12C 120.9 . . ? C118 C123 C122 121.3(9) . . ? C118 C123 H12D 119.3 . . ? C122 C123 H12D 119.3 . . ? C117 C124 H12E 109.5 . . ? C117 C124 H12F 109.5 . . ? H12E C124 H12F 109.5 . . ? C117 C124 H12R 109.5 . . ? H12E C124 H12R 109.5 . . ? H12F C124 H12R 109.5 . . ? N16 C125 C126 112.4(6) . . ? N16 C125 C132 109.0(6) . . ? C126 C125 C132 111.1(6) . . ? N16 C125 H12G 108.1 . . ? C126 C125 H12G 108.1 . . ? C132 C125 H12G 108.1 . . ? C131 C126 C127 119.8(7) . . ? C131 C126 C125 121.9(7) . . ? C127 C126 C125 118.3(7) . . ? C126 C127 C128 118.8(8) . . ? C126 C127 H12H 120.6 . . ? C128 C127 H12H 120.6 . . ? C129 C128 C127 121.1(8) . . ? C129 C128 H12I 119.5 . . ? C127 C128 H12I 119.5 . . ? C128 C129 C130 120.3(8) . . ? C128 C129 H12J 119.9 . . ? C130 C129 H12J 119.9 . . ? C129 C130 C131 120.5(8) . . ? C129 C130 H13A 119.8 . . ? C131 C130 H13A 119.8 . . ? C126 C131 C130 119.6(8) . . ? C126 C131 H13B 120.2 . . ? C130 C131 H13B 120.2 . . ? C125 C132 H13C 109.5 . . ? C125 C132 H13D 109.5 . . ? H13C C132 H13D 109.5 . . ? C125 C132 H13E 109.5 . . ? H13C C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? N17 C133 C134 109.9(5) . . ? N17 C133 C140 108.2(5) . . ? C134 C133 C140 112.4(6) . . ? N17 C133 H13F 108.7 . . ? C134 C133 H13F 108.7 . . ? C140 C133 H13F 108.7 . . ? C135 C134 C139 120.1(7) . . ? C135 C134 C133 119.3(6) . . ? C139 C134 C133 120.5(6) . . ? C134 C135 C136 120.0(7) . . ? C134 C135 H13G 120.0 . . ? C136 C135 H13G 120.0 . . ? C137 C136 C135 120.2(8) . . ? C137 C136 H13H 119.9 . . ? C135 C136 H13H 119.9 . . ? C136 C137 C138 120.3(7) . . ? C136 C137 H13I 119.9 . . ? C138 C137 H13I 119.9 . . ? C139 C138 C137 120.3(8) . . ? C139 C138 H13J 119.9 . . ? C137 C138 H13J 119.9 . . ? C138 C139 C134 119.2(7) . . ? C138 C139 H13K 120.4 . . ? C134 C139 H13K 120.4 . . ? C133 C140 H14A 109.5 . . ? C133 C140 H14B 109.5 . . ? H14A C140 H14B 109.5 . . ? C133 C140 H14C 109.5 . . ? H14A C140 H14C 109.5 . . ? H14B C140 H14C 109.5 . . ? C42A C141 N18 117.1(7) . . ? C42A C141 C148 115.5(7) . . ? N18 C141 C148 108.9(6) . . ? C42A C141 C142 20.8(4) . . ? N18 C141 C142 105.0(6) . . ? C148 C141 C142 107.7(6) . . ? C42A C141 H14D 91.0 . . ? N18 C141 H14D 111.6 . . ? C148 C141 H14D 111.6 . . ? C142 C141 H14D 111.6 . . ? C143 C142 C147 120.0 . . ? C143 C142 C141 117.6(7) . . ? C147 C142 C141 122.3(7) . . ? C144 C143 C142 120.0 . . ? C144 C143 H14E 120.0 . . ? C142 C143 H14E 120.0 . . ? C143 C144 C145 120.0 . . ? C143 C144 H14F 120.0 . . ? C145 C144 H14F 120.0 . . ? C144 C145 C146 120.0 . . ? C144 C145 H14G 120.0 . . ? C146 C145 H14G 120.0 . . ? C147 C146 C145 120.0 . . ? C147 C146 H14H 120.0 . . ? C145 C146 H14H 120.0 . . ? C146 C147 C142 120.0 . . ? C146 C147 H14I 120.0 . . ? C142 C147 H14I 120.0 . . ? C43A C42A C47A 120.0 . . ? C43A C42A C141 123.8(7) . . ? C47A C42A C141 116.2(7) . . ? C42A C43A C44A 120.0 . . ? C42A C43A H43A 120.0 . . ? C44A C43A H43A 120.0 . . ? C45A C44A C43A 120.0 . . ? C45A C44A H44A 120.0 . . ? C43A C44A H44A 120.0 . . ? C44A C45A C46A 120.0 . . ? C44A C45A H45A 120.0 . . ? C46A C45A H45A 120.0 . . ? C45A C46A C47A 120.0 . . ? C45A C46A H46A 120.0 . . ? C47A C46A H46A 120.0 . . ? C46A C47A C42A 120.0 . . ? C46A C47A H47A 120.0 . . ? C42A C47A H47A 120.0 . . ? C141 C148 H14J 109.5 . . ? C141 C148 H14K 109.5 . . ? H14J C148 H14K 109.5 . . ? C141 C148 H14L 109.5 . . ? H14J C148 H14L 109.5 . . ? H14K C148 H14L 109.5 . . ? O24 Yb2 O22 141.99(17) . . ? O24 Yb2 O21 81.11(15) . . ? O22 Yb2 O21 86.63(16) . . ? O24 Yb2 O23 85.14(16) . . ? O22 Yb2 O23 82.46(16) . . ? O21 Yb2 O23 141.49(15) . . ? O24 Yb2 O29W 71.25(16) . . ? O22 Yb2 O29W 70.75(17) . . ? O21 Yb2 O29W 70.71(15) . . ? O23 Yb2 O29W 70.81(15) . . ? O24 Yb2 N24 67.64(17) . . ? O22 Yb2 N24 140.69(17) . . ? O21 Yb2 N24 130.58(16) . . ? O23 Yb2 N24 74.44(17) . . ? O29W Yb2 N24 127.46(17) . . ? O24 Yb2 N23 134.04(16) . . ? O22 Yb2 N23 71.80(18) . . ? O21 Yb2 N23 142.55(16) . . ? O23 Yb2 N23 66.90(16) . . ? O29W Yb2 N23 125.97(17) . . ? N24 Yb2 N23 70.01(18) . . ? O24 Yb2 N22 141.52(16) . . ? O22 Yb2 N22 66.44(17) . . ? O21 Yb2 N22 74.97(16) . . ? O23 Yb2 N22 131.54(16) . . ? O29W Yb2 N22 125.73(17) . . ? N24 Yb2 N22 106.81(18) . . ? N23 Yb2 N22 68.47(16) . . ? O24 Yb2 N21 75.33(16) . . ? O22 Yb2 N21 131.63(16) . . ? O21 Yb2 N21 67.12(16) . . ? O23 Yb2 N21 142.36(16) . . ? O29W Yb2 N21 129.15(16) . . ? N24 Yb2 N21 68.46(17) . . ? N23 Yb2 N21 104.83(17) . . ? N22 Yb2 N21 67.79(16) . . ? O24 Yb2 C216 19.24(16) . . ? O22 Yb2 C216 152.40(17) . . ? O21 Yb2 C216 98.25(16) . . ? O23 Yb2 C216 76.86(16) . . ? O29W Yb2 C216 85.18(17) . . ? N24 Yb2 C216 48.89(18) . . ? N23 Yb2 C216 115.15(17) . . ? N22 Yb2 C216 141.09(17) . . ? N21 Yb2 C216 74.26(17) . . ? O24 Yb2 C212 149.21(17) . . ? O22 Yb2 C212 19.14(16) . . ? O21 Yb2 C212 75.56(16) . . ? O23 Yb2 C212 100.80(16) . . ? O29W Yb2 C212 82.15(17) . . ? N24 Yb2 C212 143.13(18) . . ? N23 Yb2 C212 74.54(17) . . ? N22 Yb2 C212 48.89(17) . . ? N21 Yb2 C212 112.50(17) . . ? C216 Yb2 C212 167.15(18) . . ? O24 Yb2 C214 103.28(16) . . ? O22 Yb2 C214 71.36(16) . . ? O21 Yb2 C214 149.63(16) . . ? O23 Yb2 C214 18.93(16) . . ? O29W Yb2 C214 82.16(16) . . ? N24 Yb2 C214 77.02(17) . . ? N23 Yb2 C214 49.46(16) . . ? N22 Yb2 C214 112.64(16) . . ? N21 Yb2 C214 143.24(16) . . ? C216 Yb2 C214 92.66(17) . . ? C212 Yb2 C214 87.72(16) . . ? C210 O21 Yb2 126.4(4) . . ? C212 O22 Yb2 124.7(4) . . ? C214 O23 Yb2 124.5(4) . . ? C216 O24 Yb2 124.8(4) . . ? C201 N21 C209 109.6(5) . . ? C201 N21 C208 109.9(5) . . ? C209 N21 C208 107.7(5) . . ? C201 N21 Yb2 110.9(4) . . ? C209 N21 Yb2 107.9(3) . . ? C208 N21 Yb2 110.8(4) . . ? C202 N22 C211 109.0(5) . . ? C202 N22 C203 107.7(5) . . ? C211 N22 C203 109.6(5) . . ? C202 N22 Yb2 112.2(4) . . ? C211 N22 Yb2 105.8(4) . . ? C203 N22 Yb2 112.5(4) . . ? C204 N23 C213 109.6(5) . . ? C204 N23 C205 109.5(5) . . ? C213 N23 C205 109.5(5) . . ? C204 N23 Yb2 111.7(4) . . ? C213 N23 Yb2 108.4(4) . . ? C205 N23 Yb2 108.1(4) . . ? C206 N24 C215 110.4(5) . . ? C206 N24 C207 109.3(5) . . ? C215 N24 C207 108.9(5) . . ? C206 N24 Yb2 110.3(4) . . ? C215 N24 Yb2 105.6(4) . . ? C207 N24 Yb2 112.4(4) . . ? C210 N25 C217 122.6(5) . . ? C210 N25 H25A 118.7 . . ? C217 N25 H25A 118.7 . . ? C212 N26 C225 121.4(6) . . ? C212 N26 H26A 119.3 . . ? C225 N26 H26A 119.3 . . ? C214 N27 C233 120.7(5) . . ? C214 N27 H27A 119.6 . . ? C233 N27 H27A 119.6 . . ? C216 N28 C241 122.7(5) . . ? C216 N28 H28A 118.7 . . ? C241 N28 H28A 118.7 . . ? N21 C201 C202 112.1(5) . . ? N21 C201 H20A 109.2 . . ? C202 C201 H20A 109.2 . . ? N21 C201 H20B 109.2 . . ? C202 C201 H20B 109.2 . . ? H20A C201 H20B 107.9 . . ? N22 C202 C201 109.7(5) . . ? N22 C202 H20C 109.7 . . ? C201 C202 H20C 109.7 . . ? N22 C202 H20D 109.7 . . ? C201 C202 H20D 109.7 . . ? H20C C202 H20D 108.2 . . ? N22 C203 C204 112.7(5) . . ? N22 C203 H20E 109.1 . . ? C204 C203 H20E 109.1 . . ? N22 C203 H20F 109.1 . . ? C204 C203 H20F 109.1 . . ? H20E C203 H20F 107.8 . . ? N23 C204 C203 112.7(6) . . ? N23 C204 H20G 109.1 . . ? C203 C204 H20G 109.1 . . ? N23 C204 H20H 109.1 . . ? C203 C204 H20H 109.1 . . ? H20G C204 H20H 107.8 . . ? N23 C205 C206 113.3(5) . . ? N23 C205 H20I 108.9 . . ? C206 C205 H20I 108.9 . . ? N23 C205 H20J 108.9 . . ? C206 C205 H20J 108.9 . . ? H20I C205 H20J 107.7 . . ? N24 C206 C205 110.5(5) . . ? N24 C206 H20K 109.6 . . ? C205 C206 H20K 109.6 . . ? N24 C206 H20L 109.6 . . ? C205 C206 H20L 109.6 . . ? H20K C206 H20L 108.1 . . ? C208 C207 N24 112.9(5) . . ? C208 C207 H20M 109.0 . . ? N24 C207 H20M 109.0 . . ? C208 C207 H20N 109.0 . . ? N24 C207 H20N 109.0 . . ? H20M C207 H20N 107.8 . . ? N21 C208 C207 112.2(6) . . ? N21 C208 H20O 109.2 . . ? C207 C208 H20O 109.2 . . ? N21 C208 H20P 109.2 . . ? C207 C208 H20P 109.2 . . ? H20O C208 H20P 107.9 . . ? N21 C209 C210 111.4(5) . . ? N21 C209 H20Q 109.3 . . ? C210 C209 H20Q 109.3 . . ? N21 C209 H20R 109.3 . . ? C210 C209 H20R 109.3 . . ? H20Q C209 H20R 108.0 . . ? O21 C210 N25 121.9(6) . . ? O21 C210 C209 119.7(5) . . ? N25 C210 C209 118.3(5) . . ? O21 C210 Yb2 35.1(3) . . ? N25 C210 Yb2 156.8(4) . . ? C209 C210 Yb2 84.6(3) . . ? N22 C211 C212 109.6(5) . . ? N22 C211 H21A 109.8 . . ? C212 C211 H21A 109.8 . . ? N22 C211 H21B 109.8 . . ? C212 C211 H21B 109.8 . . ? H21A C211 H21B 108.2 . . ? O22 C212 N26 121.5(6) . . ? O22 C212 C211 119.5(6) . . ? N26 C212 C211 118.8(6) . . ? O22 C212 Yb2 36.2(3) . . ? N26 C212 Yb2 156.4(5) . . ? C211 C212 Yb2 83.5(4) . . ? N23 C213 C214 112.1(5) . . ? N23 C213 H21C 109.2 . . ? C214 C213 H21C 109.2 . . ? N23 C213 H21D 109.2 . . ? C214 C213 H21D 109.2 . . ? H21C C213 H21D 107.9 . . ? O23 C214 N27 122.2(6) . . ? O23 C214 C213 120.3(5) . . ? N27 C214 C213 117.5(5) . . ? O23 C214 Yb2 36.6(3) . . ? N27 C214 Yb2 156.8(5) . . ? C213 C214 Yb2 84.6(3) . . ? C216 C215 N24 108.7(5) . . ? C216 C215 H21E 110.0 . . ? N24 C215 H21E 110.0 . . ? C216 C215 H21F 110.0 . . ? N24 C215 H21F 110.0 . . ? H21E C215 H21F 108.3 . . ? O24 C216 N28 122.8(6) . . ? O24 C216 C215 119.5(6) . . ? N28 C216 C215 117.7(5) . . ? O24 C216 Yb2 36.0(3) . . ? N28 C216 Yb2 158.3(5) . . ? C215 C216 Yb2 83.8(4) . . ? N25 C217 C218 112.8(6) . . ? N25 C217 C224 108.3(6) . . ? C218 C217 C224 111.9(5) . . ? N25 C217 H21G 107.9 . . ? C218 C217 H21G 107.9 . . ? C224 C217 H21G 107.9 . . ? C223 C218 C219 119.0(8) . . ? C223 C218 C217 121.7(7) . . ? C219 C218 C217 119.2(7) . . ? C220 C219 C218 120.7(8) . . ? C220 C219 H21H 119.6 . . ? C218 C219 H21H 119.6 . . ? C221 C220 C219 120.1(9) . . ? C221 C220 H22A 119.9 . . ? C219 C220 H22A 119.9 . . ? C220 C221 C222 120.3(9) . . ? C220 C221 H22B 119.9 . . ? C222 C221 H22B 119.9 . . ? C221 C222 C223 119.5(8) . . ? C221 C222 H22C 120.3 . . ? C223 C222 H22C 120.3 . . ? C218 C223 C222 120.3(8) . . ? C218 C223 H22D 119.8 . . ? C222 C223 H22D 119.8 . . ? C217 C224 H22E 109.5 . . ? C217 C224 H22F 109.5 . . ? H22E C224 H22F 109.5 . . ? C217 C224 H22G 109.5 . . ? H22E C224 H22G 109.5 . . ? H22F C224 H22G 109.5 . . ? N26 C225 C232 109.0(7) . . ? N26 C225 C226 110.7(7) . . ? C232 C225 C226 111.7(7) . . ? N26 C225 H22H 108.4 . . ? C232 C225 H22H 108.4 . . ? C226 C225 H22H 108.4 . . ? C231 C226 C227 119.8(9) . . ? C231 C226 C225 120.8(7) . . ? C227 C226 C225 119.3(9) . . ? C226 C227 C228 117.9(11) . . ? C226 C227 H22I 121.1 . . ? C228 C227 H22I 121.1 . . ? C229 C228 C227 122.2(10) . . ? C229 C228 H22K 118.9 . . ? C227 C228 H22K 118.9 . . ? C228 C229 C230 119.8(13) . . ? C228 C229 H22L 120.1 . . ? C230 C229 H22L 120.1 . . ? C229 C230 C231 119.9(13) . . ? C229 C230 H23A 120.1 . . ? C231 C230 H23A 120.1 . . ? C226 C231 C230 120.4(9) . . ? C226 C231 H23B 119.8 . . ? C230 C231 H23B 119.8 . . ? C225 C232 H23C 109.5 . . ? C225 C232 H23D 109.5 . . ? H23C C232 H23D 109.5 . . ? C225 C232 H23E 109.5 . . ? H23C C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? N27 C233 C234 110.8(5) . . ? N27 C233 C240 108.8(5) . . ? C234 C233 C240 112.2(5) . . ? N27 C233 H23F 108.3 . . ? C234 C233 H23F 108.3 . . ? C240 C233 H23F 108.3 . . ? C235 C234 C239 119.2(6) . . ? C235 C234 C233 120.4(6) . . ? C239 C234 C233 120.4(6) . . ? C234 C235 C236 121.3(7) . . ? C234 C235 H23G 119.4 . . ? C236 C235 H23G 119.4 . . ? C235 C236 C237 119.3(7) . . ? C235 C236 H23H 120.4 . . ? C237 C236 H23H 120.4 . . ? C238 C237 C236 119.5(7) . . ? C238 C237 H23I 120.2 . . ? C236 C237 H23I 120.2 . . ? C237 C238 C239 121.2(7) . . ? C237 C238 H23J 119.4 . . ? C239 C238 H23J 119.4 . . ? C234 C239 C238 119.6(6) . . ? C234 C239 H23K 120.2 . . ? C238 C239 H23K 120.2 . . ? C233 C240 H24A 109.5 . . ? C233 C240 H24B 109.5 . . ? H24A C240 H24B 109.5 . . ? C233 C240 H24C 109.5 . . ? H24A C240 H24C 109.5 . . ? H24B C240 H24C 109.5 . . ? N28 C241 C248 109.4(5) . . ? N28 C241 C242 111.1(5) . . ? C248 C241 C242 112.2(5) . . ? N28 C241 H24D 108.0 . . ? C248 C241 H24D 108.0 . . ? C242 C241 H24D 108.0 . . ? C243 C242 C247 118.7(6) . . ? C243 C242 C241 121.1(6) . . ? C247 C242 C241 120.1(6) . . ? C242 C243 C244 121.3(7) . . ? C242 C243 H24E 119.4 . . ? C244 C243 H24E 119.4 . . ? C243 C244 C245 119.6(7) . . ? C243 C244 H24F 120.2 . . ? C245 C244 H24F 120.2 . . ? C246 C245 C244 119.9(7) . . ? C246 C245 H24G 120.1 . . ? C244 C245 H24G 120.1 . . ? C245 C246 C247 120.5(7) . . ? C245 C246 H24H 119.8 . . ? C247 C246 H24H 119.8 . . ? C246 C247 C242 120.1(7) . . ? C246 C247 H24I 119.9 . . ? C242 C247 H24I 119.9 . . ? C241 C248 H24J 109.5 . . ? C241 C248 H24K 109.5 . . ? H24J C248 H24K 109.5 . . ? C241 C248 H24L 109.5 . . ? H24J C248 H24L 109.5 . . ? H24K C248 H24L 109.5 . . ? O32 Yb3 O34 140.77(15) . . ? O32 Yb3 O33 82.70(15) . . ? O34 Yb3 O33 83.05(16) . . ? O32 Yb3 O31 83.70(14) . . ? O34 Yb3 O31 85.29(15) . . ? O33 Yb3 O31 141.71(15) . . ? O32 Yb3 O31W 71.55(15) . . ? O34 Yb3 O31W 69.33(15) . . ? O33 Yb3 O31W 72.50(15) . . ? O31 Yb3 O31W 69.26(14) . . ? O32 Yb3 N31 133.35(16) . . ? O34 Yb3 N31 74.30(16) . . ? O33 Yb3 N31 141.88(16) . . ? O31 Yb3 N31 67.09(15) . . ? O31W Yb3 N31 124.35(14) . . ? O32 Yb3 N33 73.82(15) . . ? O34 Yb3 N33 132.04(16) . . ? O33 Yb3 N33 67.67(16) . . ? O31 Yb3 N33 140.42(15) . . ? O31W Yb3 N33 129.55(14) . . ? N31 Yb3 N33 106.10(15) . . ? O32 Yb3 N32 67.75(15) . . ? O34 Yb3 N32 142.74(16) . . ? O33 Yb3 N32 131.94(16) . . ? O31 Yb3 N32 73.38(15) . . ? O31W Yb3 N32 126.69(15) . . ? N31 Yb3 N32 69.38(16) . . ? N33 Yb3 N32 68.10(15) . . ? O32 Yb3 N34 141.47(15) . . ? O34 Yb3 N34 67.02(15) . . ? O33 Yb3 N34 74.52(15) . . ? O31 Yb3 N34 132.49(15) . . ? O31W Yb3 N34 127.43(15) . . ? N31 Yb3 N34 68.56(16) . . ? N33 Yb3 N34 68.94(15) . . ? N32 Yb3 N34 105.81(15) . . ? O32 Yb3 C314 75.25(15) . . ? O34 Yb3 C314 99.72(16) . . ? O33 Yb3 C314 18.98(16) . . ? O31 Yb3 C314 152.36(15) . . ? O31W Yb3 C314 86.97(15) . . ? N31 Yb3 C314 140.50(16) . . ? N33 Yb3 C314 49.04(16) . . ? N32 Yb3 C314 113.42(16) . . ? N34 Yb3 C314 73.19(15) . . ? O32 Yb3 C312 19.08(15) . . ? O34 Yb3 C312 150.53(16) . . ? O33 Yb3 C312 100.45(16) . . ? O31 Yb3 C312 73.85(15) . . ? O31W Yb3 C312 83.72(15) . . ? N31 Yb3 C312 114.40(16) . . ? N33 Yb3 C312 74.59(16) . . ? N32 Yb3 C312 49.69(15) . . ? N34 Yb3 C312 142.29(15) . . ? C314 Yb3 C312 90.21(16) . . ? O32 Yb3 C316 150.30(15) . . ? O34 Yb3 C316 18.99(16) . . ? O33 Yb3 C316 74.58(16) . . ? O31 Yb3 C316 102.42(15) . . ? O31W Yb3 C316 83.38(15) . . ? N31 Yb3 C316 74.21(16) . . ? N33 Yb3 C316 113.32(16) . . ? N32 Yb3 C316 141.94(15) . . ? N34 Yb3 C316 48.73(15) . . ? C314 Yb3 C316 88.06(16) . . ? C312 Yb3 C316 167.05(15) . . ? C310 O31 Yb3 123.8(4) . . ? C312 O32 Yb3 125.0(4) . . ? C314 O33 Yb3 124.0(4) . . ? C316 O34 Yb3 124.6(4) . . ? C309 N31 C301 110.9(5) . . ? C309 N31 C308 109.4(5) . . ? C301 N31 C308 108.5(5) . . ? C309 N31 Yb3 106.5(3) . . ? C301 N31 Yb3 110.0(3) . . ? C308 N31 Yb3 111.6(3) . . ? C303 N32 C302 109.1(5) . . ? C303 N32 C311 109.9(5) . . ? C302 N32 C311 109.9(5) . . ? C303 N32 Yb3 112.0(3) . . ? C302 N32 Yb3 110.6(3) . . ? C311 N32 Yb3 105.3(3) . . ? C313 N33 C304 109.1(5) . . ? C313 N33 C305 110.1(5) . . ? C304 N33 C305 108.5(5) . . ? C313 N33 Yb3 106.3(3) . . ? C304 N33 Yb3 111.9(4) . . ? C305 N33 Yb3 110.9(3) . . ? C315 N34 C306 110.0(5) . . ? C315 N34 C307 109.9(5) . . ? C306 N34 C307 108.0(4) . . ? C315 N34 Yb3 106.2(3) . . ? C306 N34 Yb3 111.2(3) . . ? C307 N34 Yb3 111.5(4) . . ? C310 N35 C317 122.8(5) . . ? C310 N35 H35A 118.6 . . ? C317 N35 H35A 118.6 . . ? C312 N36 C325 121.2(5) . . ? C312 N36 H36A 119.4 . . ? C325 N36 H36A 119.4 . . ? C314 N37 C333 120.6(5) . . ? C314 N37 H37A 119.7 . . ? C333 N37 H37A 119.7 . . ? C316 N38 C341 121.3(5) . . ? C316 N38 H38A 119.3 . . ? C341 N38 H38A 119.3 . . ? N31 C301 C302 113.3(5) . . ? N31 C301 H30A 108.9 . . ? C302 C301 H30A 108.9 . . ? N31 C301 H30B 108.9 . . ? C302 C301 H30B 108.9 . . ? H30A C301 H30B 107.7 . . ? N32 C302 C301 110.9(5) . . ? N32 C302 H30C 109.5 . . ? C301 C302 H30C 109.5 . . ? N32 C302 H30D 109.5 . . ? C301 C302 H30D 109.5 . . ? H30C C302 H30D 108.0 . . ? N32 C303 C304 112.1(5) . . ? N32 C303 H30E 109.2 . . ? C304 C303 H30E 109.2 . . ? N32 C303 H30F 109.2 . . ? C304 C303 H30F 109.2 . . ? H30E C303 H30F 107.9 . . ? N33 C304 C303 111.0(5) . . ? N33 C304 H30G 109.4 . . ? C303 C304 H30G 109.4 . . ? N33 C304 H30H 109.4 . . ? C303 C304 H30H 109.4 . . ? H30G C304 H30H 108.0 . . ? N33 C305 C306 112.8(5) . . ? N33 C305 H30I 109.0 . . ? C306 C305 H30I 109.0 . . ? N33 C305 H30J 109.0 . . ? C306 C305 H30J 109.0 . . ? H30I C305 H30J 107.8 . . ? N34 C306 C305 111.5(5) . . ? N34 C306 H30K 109.3 . . ? C305 C306 H30K 109.3 . . ? N34 C306 H30L 109.3 . . ? C305 C306 H30L 109.3 . . ? H30K C306 H30L 108.0 . . ? N34 C307 C308 112.2(5) . . ? N34 C307 H30M 109.2 . . ? C308 C307 H30M 109.2 . . ? N34 C307 H30N 109.2 . . ? C308 C307 H30N 109.2 . . ? H30M C307 H30N 107.9 . . ? N31 C308 C307 111.7(5) . . ? N31 C308 H30O 109.3 . . ? C307 C308 H30O 109.3 . . ? N31 C308 H30P 109.3 . . ? C307 C308 H30P 109.3 . . ? H30O C308 H30P 107.9 . . ? N31 C309 C310 110.4(5) . . ? N31 C309 H30Q 109.6 . . ? C310 C309 H30Q 109.6 . . ? N31 C309 H30R 109.6 . . ? C310 C309 H30R 109.6 . . ? H30Q C309 H30R 108.1 . . ? O31 C310 N35 121.4(6) . . ? O31 C310 C309 119.5(5) . . ? N35 C310 C309 119.0(5) . . ? O31 C310 Yb3 36.8(3) . . ? N35 C310 Yb3 158.2(4) . . ? C309 C310 Yb3 82.8(3) . . ? N32 C311 C312 111.3(5) . . ? N32 C311 H31A 109.4 . . ? C312 C311 H31A 109.4 . . ? N32 C311 H31B 109.4 . . ? C312 C311 H31B 109.4 . . ? H31A C311 H31B 108.0 . . ? O32 C312 N36 122.0(6) . . ? O32 C312 C311 119.4(5) . . ? N36 C312 C311 118.5(5) . . ? O32 C312 Yb3 36.0(3) . . ? N36 C312 Yb3 157.7(4) . . ? C311 C312 Yb3 83.5(3) . . ? N33 C313 C314 109.8(5) . . ? N33 C313 H31C 109.7 . . ? C314 C313 H31C 109.7 . . ? N33 C313 H31D 109.7 . . ? C314 C313 H31D 109.7 . . ? H31C C313 H31D 108.2 . . ? O33 C314 N37 123.5(6) . . ? O33 C314 C313 120.6(5) . . ? N37 C314 C313 115.8(5) . . ? O33 C314 Yb3 37.0(3) . . ? N37 C314 Yb3 160.1(4) . . ? C313 C314 Yb3 83.9(3) . . ? N34 C315 C316 110.5(5) . . ? N34 C315 H31E 109.5 . . ? C316 C315 H31E 109.5 . . ? N34 C315 H31F 109.5 . . ? C316 C315 H31F 109.5 . . ? H31E C315 H31F 108.1 . . ? O34 C316 N38 121.4(6) . . ? O34 C316 C315 120.3(5) . . ? N38 C316 C315 118.2(5) . . ? O34 C316 Yb3 36.4(3) . . ? N38 C316 Yb3 157.8(4) . . ? C315 C316 Yb3 83.9(3) . . ? N35 C317 C324 109.4(5) . . ? N35 C317 C318 110.9(5) . . ? C324 C317 C318 112.2(5) . . ? N35 C317 H31G 108.1 . . ? C324 C317 H31G 108.1 . . ? C318 C317 H31G 108.1 . . ? C319 C318 C323 118.6(6) . . ? C319 C318 C317 119.5(6) . . ? C323 C318 C317 121.8(6) . . ? C318 C319 C320 120.7(7) . . ? C318 C319 H31H 119.7 . . ? C320 C319 H31H 119.7 . . ? C319 C320 C321 119.8(7) . . ? C319 C320 H32A 120.1 . . ? C321 C320 H32A 120.1 . . ? C322 C321 C320 119.1(7) . . ? C322 C321 H32B 120.4 . . ? C320 C321 H32B 120.4 . . ? C321 C322 C323 121.1(7) . . ? C321 C322 H32C 119.4 . . ? C323 C322 H32C 119.4 . . ? C322 C323 C318 120.6(6) . . ? C322 C323 H32D 119.7 . . ? C318 C323 H32D 119.7 . . ? C317 C324 H32E 109.5 . . ? C317 C324 H32F 109.5 . . ? H32E C324 H32F 109.5 . . ? C317 C324 H32G 109.5 . . ? H32E C324 H32G 109.5 . . ? H32F C324 H32G 109.5 . . ? N36 C325 C326 111.6(5) . . ? N36 C325 C332 108.2(5) . . ? C326 C325 C332 112.2(5) . . ? N36 C325 H32H 108.2 . . ? C326 C325 H32H 108.2 . . ? C332 C325 H32H 108.2 . . ? C331 C326 C327 118.2(6) . . ? C331 C326 C325 120.5(5) . . ? C327 C326 C325 121.2(6) . . ? C328 C327 C326 121.1(6) . . ? C328 C327 H32I 119.4 . . ? C326 C327 H32I 119.4 . . ? C329 C328 C327 119.6(6) . . ? C329 C328 H32J 120.2 . . ? C327 C328 H32J 120.2 . . ? C328 C329 C330 119.6(6) . . ? C328 C329 H32K 120.2 . . ? C330 C329 H32K 120.2 . . ? C331 C330 C329 119.9(7) . . ? C331 C330 H33A 120.1 . . ? C329 C330 H33A 120.1 . . ? C330 C331 C326 121.5(6) . . ? C330 C331 H33B 119.3 . . ? C326 C331 H33B 119.3 . . ? C325 C332 H33C 109.5 . . ? C325 C332 H33D 109.5 . . ? H33C C332 H33D 109.5 . . ? C325 C332 H33E 109.5 . . ? H33C C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? N37 C333 C334 111.1(5) . . ? N37 C333 C340 108.2(5) . . ? C334 C333 C340 111.9(5) . . ? N37 C333 H33F 108.5 . . ? C334 C333 H33F 108.5 . . ? C340 C333 H33F 108.5 . . ? C335 C334 C339 119.9(7) . . ? C335 C334 C333 121.8(6) . . ? C339 C334 C333 118.3(6) . . ? C334 C335 C336 120.4(7) . . ? C334 C335 H33G 119.8 . . ? C336 C335 H33G 119.8 . . ? C335 C336 C337 119.0(8) . . ? C335 C336 H33H 120.5 . . ? C337 C336 H33H 120.5 . . ? C338 C337 C336 120.1(7) . . ? C338 C337 H33I 120.0 . . ? C336 C337 H33I 120.0 . . ? C337 C338 C339 120.2(7) . . ? C337 C338 H33J 119.9 . . ? C339 C338 H33J 119.9 . . ? C334 C339 C338 120.2(7) . . ? C334 C339 H33K 119.9 . . ? C338 C339 H33K 119.9 . . ? C333 C340 H34A 109.5 . . ? C333 C340 H34B 109.5 . . ? H34A C340 H34B 109.5 . . ? C333 C340 H34C 109.5 . . ? H34A C340 H34C 109.5 . . ? H34B C340 H34C 109.5 . . ? N38 C341 C342 110.5(5) . . ? N38 C341 C348 108.9(5) . . ? C342 C341 C348 112.1(5) . . ? N38 C341 H34D 108.4 . . ? C342 C341 H34D 108.4 . . ? C348 C341 H34D 108.4 . . ? C347 C342 C343 119.0(7) . . ? C347 C342 C341 121.5(6) . . ? C343 C342 C341 119.5(6) . . ? C344 C343 C342 119.8(7) . . ? C344 C343 H34E 120.1 . . ? C342 C343 H34E 120.1 . . ? C345 C344 C343 120.4(8) . . ? C345 C344 H34F 119.8 . . ? C343 C344 H34F 119.8 . . ? C344 C345 C346 120.3(8) . . ? C344 C345 H34G 119.8 . . ? C346 C345 H34G 119.8 . . ? C347 C346 C345 120.0(7) . . ? C347 C346 H34H 120.0 . . ? C345 C346 H34H 120.0 . . ? C346 C347 C342 120.4(7) . . ? C346 C347 H34I 119.8 . . ? C342 C347 H34I 119.8 . . ? C341 C348 H34J 109.5 . . ? C341 C348 H34K 109.5 . . ? H34J C348 H34K 109.5 . . ? C341 C348 H34L 109.5 . . ? H34J C348 H34L 109.5 . . ? H34K C348 H34L 109.5 . . ? O16W O20W Cl9 144.1(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 Yb1 O11 C110 156.9(5) . . . . ? O13 Yb1 O11 C110 -136.3(4) . . . . ? O14 Yb1 O11 C110 -59.2(5) . . . . ? O11W Yb1 O11 C110 -129.1(5) . . . . ? N14 Yb1 O11 C110 -5.8(6) . . . . ? N11 Yb1 O11 C110 14.6(5) . . . . ? N13 Yb1 O11 C110 103.3(5) . . . . ? N12 Yb1 O11 C110 88.7(5) . . . . ? C114 Yb1 O11 C110 -169.0(4) . . . . ? C112 Yb1 O11 C110 140.1(5) . . . . ? O13 Yb1 O12 C112 155.5(5) . . . . ? O14 Yb1 O12 C112 -132.1(5) . . . . ? O11 Yb1 O12 C112 -58.8(5) . . . . ? O11W Yb1 O12 C112 -132.1(5) . . . . ? N14 Yb1 O12 C112 101.2(5) . . . . ? N11 Yb1 O12 C112 -10.2(6) . . . . ? N13 Yb1 O12 C112 87.0(5) . . . . ? N12 Yb1 O12 C112 15.3(5) . . . . ? C114 Yb1 O12 C112 137.7(5) . . . . ? C110 Yb1 O12 C112 -51.3(5) . . . . ? O12 Yb1 O13 C114 -62.0(5) . . . . ? O14 Yb1 O13 C114 154.1(5) . . . . ? O11 Yb1 O13 C114 -127.9(5) . . . . ? O11W Yb1 O13 C114 -135.1(5) . . . . ? N14 Yb1 O13 C114 86.5(5) . . . . ? N11 Yb1 O13 C114 100.1(5) . . . . ? N13 Yb1 O13 C114 13.3(5) . . . . ? N12 Yb1 O13 C114 -10.8(6) . . . . ? C110 Yb1 O13 C114 -158.6(4) . . . . ? C112 Yb1 O13 C114 -54.2(5) . . . . ? O12 Yb1 O14 C116 -129.9(5) . . . . ? O13 Yb1 O14 C116 -57.8(5) . . . . ? O11 Yb1 O14 C116 158.8(5) . . . . ? O11W Yb1 O14 C116 -130.0(5) . . . . ? N14 Yb1 O14 C116 17.4(5) . . . . ? N11 Yb1 O14 C116 91.7(5) . . . . ? N13 Yb1 O14 C116 -5.3(6) . . . . ? N12 Yb1 O14 C116 103.6(5) . . . . ? C114 Yb1 O14 C116 -49.2(5) . . . . ? C110 Yb1 O14 C116 141.9(5) . . . . ? C112 Yb1 O14 C116 -159.9(4) . . . . ? O12 Yb1 N11 C109 -82.3(4) . . . . ? O13 Yb1 N11 C109 121.6(4) . . . . ? O14 Yb1 N11 C109 64.7(4) . . . . ? O11 Yb1 N11 C109 -29.0(4) . . . . ? O11W Yb1 N11 C109 14.6(4) . . . . ? N14 Yb1 N11 C109 135.6(4) . . . . ? N13 Yb1 N11 C109 -164.7(4) . . . . ? N12 Yb1 N11 C109 -107.4(4) . . . . ? C114 Yb1 N11 C109 153.9(3) . . . . ? C110 Yb1 N11 C109 -22.6(3) . . . . ? C112 Yb1 N11 C109 -85.9(4) . . . . ? O12 Yb1 N11 C101 38.4(5) . . . . ? O13 Yb1 N11 C101 -117.6(4) . . . . ? O14 Yb1 N11 C101 -174.6(4) . . . . ? O11 Yb1 N11 C101 91.7(4) . . . . ? O11W Yb1 N11 C101 135.3(4) . . . . ? N14 Yb1 N11 C101 -103.7(4) . . . . ? N13 Yb1 N11 C101 -44.0(4) . . . . ? N12 Yb1 N11 C101 13.3(4) . . . . ? C114 Yb1 N11 C101 -85.4(4) . . . . ? C110 Yb1 N11 C101 98.1(4) . . . . ? C112 Yb1 N11 C101 34.8(4) . . . . ? O12 Yb1 N11 C108 159.8(4) . . . . ? O13 Yb1 N11 C108 3.8(6) . . . . ? O14 Yb1 N11 C108 -53.1(4) . . . . ? O11 Yb1 N11 C108 -146.8(5) . . . . ? O11W Yb1 N11 C108 -103.3(4) . . . . ? N14 Yb1 N11 C108 17.8(4) . . . . ? N13 Yb1 N11 C108 77.5(4) . . . . ? N12 Yb1 N11 C108 134.7(5) . . . . ? C114 Yb1 N11 C108 36.0(5) . . . . ? C110 Yb1 N11 C108 -140.5(5) . . . . ? C112 Yb1 N11 C108 156.3(4) . . . . ? O12 Yb1 N12 C111 -23.5(4) . . . . ? O13 Yb1 N12 C111 -81.0(4) . . . . ? O14 Yb1 N12 C111 123.8(4) . . . . ? O11 Yb1 N12 C111 64.2(4) . . . . ? O11W Yb1 N12 C111 16.9(5) . . . . ? N14 Yb1 N12 C111 -163.6(4) . . . . ? N11 Yb1 N12 C111 136.1(4) . . . . ? N13 Yb1 N12 C111 -105.2(4) . . . . ? C114 Yb1 N12 C111 -84.9(4) . . . . ? C110 Yb1 N12 C111 84.5(4) . . . . ? C112 Yb1 N12 C111 -17.0(4) . . . . ? O12 Yb1 N12 C102 -144.6(4) . . . . ? O13 Yb1 N12 C102 157.9(4) . . . . ? O14 Yb1 N12 C102 2.7(6) . . . . ? O11 Yb1 N12 C102 -56.9(4) . . . . ? O11W Yb1 N12 C102 -104.2(4) . . . . ? N14 Yb1 N12 C102 75.3(4) . . . . ? N11 Yb1 N12 C102 15.0(4) . . . . ? N13 Yb1 N12 C102 133.7(5) . . . . ? C114 Yb1 N12 C102 154.0(4) . . . . ? C110 Yb1 N12 C102 -36.6(4) . . . . ? C112 Yb1 N12 C102 -138.1(5) . . . . ? O12 Yb1 N12 C103 95.9(5) . . . . ? O13 Yb1 N12 C103 38.3(5) . . . . ? O14 Yb1 N12 C103 -116.8(5) . . . . ? O11 Yb1 N12 C103 -176.4(5) . . . . ? O11W Yb1 N12 C103 136.3(4) . . . . ? N14 Yb1 N12 C103 -44.2(5) . . . . ? N11 Yb1 N12 C103 -104.5(5) . . . . ? N13 Yb1 N12 C103 14.2(4) . . . . ? C114 Yb1 N12 C103 34.5(5) . . . . ? C110 Yb1 N12 C103 -156.2(5) . . . . ? C112 Yb1 N12 C103 102.4(5) . . . . ? O12 Yb1 N13 C113 64.7(4) . . . . ? O13 Yb1 N13 C113 -24.9(4) . . . . ? O14 Yb1 N13 C113 -83.5(5) . . . . ? O11 Yb1 N13 C113 120.5(4) . . . . ? O11W Yb1 N13 C113 14.7(5) . . . . ? N14 Yb1 N13 C113 -105.9(4) . . . . ? N11 Yb1 N13 C113 -166.1(4) . . . . ? N12 Yb1 N13 C113 135.6(4) . . . . ? C114 Yb1 N13 C113 -19.0(4) . . . . ? C110 Yb1 N13 C113 149.6(4) . . . . ? C112 Yb1 N13 C113 84.2(4) . . . . ? O12 Yb1 N13 C105 -175.8(4) . . . . ? O13 Yb1 N13 C105 94.6(4) . . . . ? O14 Yb1 N13 C105 36.0(5) . . . . ? O11 Yb1 N13 C105 -120.0(4) . . . . ? O11W Yb1 N13 C105 134.1(4) . . . . ? N14 Yb1 N13 C105 13.6(4) . . . . ? N11 Yb1 N13 C105 -46.7(4) . . . . ? N12 Yb1 N13 C105 -105.0(4) . . . . ? C114 Yb1 N13 C105 100.4(5) . . . . ? C110 Yb1 N13 C105 -90.9(5) . . . . ? C112 Yb1 N13 C105 -156.3(4) . . . . ? O12 Yb1 N13 C104 -55.4(4) . . . . ? O13 Yb1 N13 C104 -145.0(5) . . . . ? O14 Yb1 N13 C104 156.4(4) . . . . ? O11 Yb1 N13 C104 0.4(6) . . . . ? O11W Yb1 N13 C104 -105.4(5) . . . . ? N14 Yb1 N13 C104 134.0(5) . . . . ? N11 Yb1 N13 C104 73.8(5) . . . . ? N12 Yb1 N13 C104 15.5(4) . . . . ? C114 Yb1 N13 C104 -139.1(5) . . . . ? C110 Yb1 N13 C104 29.5(6) . . . . ? C112 Yb1 N13 C104 -35.9(4) . . . . ? O12 Yb1 N14 C106 1.0(5) . . . . ? O13 Yb1 N14 C106 -56.0(4) . . . . ? O14 Yb1 N14 C106 -146.6(4) . . . . ? O11 Yb1 N14 C106 152.8(4) . . . . ? O11W Yb1 N14 C106 -107.5(4) . . . . ? N11 Yb1 N14 C106 132.7(4) . . . . ? N13 Yb1 N14 C106 15.6(4) . . . . ? N12 Yb1 N14 C106 72.9(4) . . . . ? C114 Yb1 N14 C106 -35.7(4) . . . . ? C110 Yb1 N14 C106 150.6(4) . . . . ? C112 Yb1 N14 C106 31.4(5) . . . . ? O12 Yb1 N14 C115 119.5(4) . . . . ? O13 Yb1 N14 C115 62.6(4) . . . . ? O14 Yb1 N14 C115 -28.0(4) . . . . ? O11 Yb1 N14 C115 -88.7(4) . . . . ? O11W Yb1 N14 C115 11.0(5) . . . . ? N11 Yb1 N14 C115 -108.7(4) . . . . ? N13 Yb1 N14 C115 134.2(4) . . . . ? N12 Yb1 N14 C115 -168.5(4) . . . . ? C114 Yb1 N14 C115 82.9(4) . . . . ? C110 Yb1 N14 C115 -90.8(4) . . . . ? C112 Yb1 N14 C115 149.9(4) . . . . ? O12 Yb1 N14 C107 -121.4(4) . . . . ? O13 Yb1 N14 C107 -178.4(5) . . . . ? O14 Yb1 N14 C107 91.0(4) . . . . ? O11 Yb1 N14 C107 30.3(5) . . . . ? O11W Yb1 N14 C107 130.1(4) . . . . ? N11 Yb1 N14 C107 10.3(4) . . . . ? N13 Yb1 N14 C107 -106.8(4) . . . . ? N12 Yb1 N14 C107 -49.5(5) . . . . ? C114 Yb1 N14 C107 -158.1(5) . . . . ? C110 Yb1 N14 C107 28.2(5) . . . . ? C112 Yb1 N14 C107 -91.0(5) . . . . ? C109 N11 C101 C102 77.1(7) . . . . ? C108 N11 C101 C102 -163.7(6) . . . . ? Yb1 N11 C101 C102 -41.1(6) . . . . ? C111 N12 C102 C101 -159.9(5) . . . . ? C103 N12 C102 C101 80.0(7) . . . . ? Yb1 N12 C102 C101 -41.9(6) . . . . ? N11 C101 C102 N12 57.9(7) . . . . ? C111 N12 C103 C104 74.7(7) . . . . ? C102 N12 C103 C104 -163.8(6) . . . . ? Yb1 N12 C103 C104 -43.0(7) . . . . ? C113 N13 C104 C103 -163.1(6) . . . . ? C105 N13 C104 C103 77.7(7) . . . . ? Yb1 N13 C104 C103 -44.2(7) . . . . ? N12 C103 C104 N13 59.1(8) . . . . ? C113 N13 C105 C106 75.3(7) . . . . ? C104 N13 C105 C106 -165.9(6) . . . . ? Yb1 N13 C105 C106 -42.3(7) . . . . ? C115 N14 C106 C105 -161.0(5) . . . . ? C107 N14 C106 C105 80.1(7) . . . . ? Yb1 N14 C106 C105 -43.1(6) . . . . ? N13 C105 C106 N14 58.9(8) . . . . ? C106 N14 C107 C108 -163.2(6) . . . . ? C115 N14 C107 C108 78.7(7) . . . . ? Yb1 N14 C107 C108 -39.1(7) . . . . ? N14 C107 C108 N11 58.0(8) . . . . ? C109 N11 C108 C107 -161.3(5) . . . . ? C101 N11 C108 C107 78.5(7) . . . . ? Yb1 N11 C108 C107 -44.9(6) . . . . ? C101 N11 C109 C110 -82.2(6) . . . . ? C108 N11 C109 C110 158.7(5) . . . . ? Yb1 N11 C109 C110 39.6(5) . . . . ? Yb1 O11 C110 N15 -178.6(4) . . . . ? Yb1 O11 C110 C109 3.8(8) . . . . ? C117 N15 C110 O11 1.5(10) . . . . ? C117 N15 C110 C109 179.1(6) . . . . ? C117 N15 C110 Yb1 -0.8(16) . . . . ? N11 C109 C110 O11 -32.7(8) . . . . ? N11 C109 C110 N15 149.6(6) . . . . ? N11 C109 C110 Yb1 -30.4(4) . . . . ? O12 Yb1 C110 O11 -23.0(5) . . . . ? O13 Yb1 C110 O11 70.0(6) . . . . ? O14 Yb1 C110 O11 118.5(5) . . . . ? O11W Yb1 C110 O11 47.7(5) . . . . ? N14 Yb1 C110 O11 175.4(4) . . . . ? N11 Yb1 C110 O11 -162.0(6) . . . . ? N13 Yb1 C110 O11 -98.6(5) . . . . ? N12 Yb1 C110 O11 -85.0(5) . . . . ? C114 Yb1 C110 O11 29.6(11) . . . . ? C112 Yb1 C110 O11 -37.6(5) . . . . ? O12 Yb1 C110 N15 -19.8(13) . . . . ? O13 Yb1 C110 N15 73.2(13) . . . . ? O14 Yb1 C110 N15 121.7(13) . . . . ? O11 Yb1 C110 N15 3.2(11) . . . . ? O11W Yb1 C110 N15 50.9(13) . . . . ? N14 Yb1 C110 N15 178.7(12) . . . . ? N11 Yb1 C110 N15 -158.7(13) . . . . ? N13 Yb1 C110 N15 -95.3(13) . . . . ? N12 Yb1 C110 N15 -81.8(13) . . . . ? C114 Yb1 C110 N15 32.9(18) . . . . ? C112 Yb1 C110 N15 -34.3(13) . . . . ? O12 Yb1 C110 C109 160.3(4) . . . . ? O13 Yb1 C110 C109 -106.7(5) . . . . ? O14 Yb1 C110 C109 -58.2(4) . . . . ? O11 Yb1 C110 C109 -176.7(7) . . . . ? O11W Yb1 C110 C109 -129.1(4) . . . . ? N14 Yb1 C110 C109 -1.3(4) . . . . ? N11 Yb1 C110 C109 21.3(3) . . . . ? N13 Yb1 C110 C109 84.7(4) . . . . ? N12 Yb1 C110 C109 98.3(4) . . . . ? C114 Yb1 C110 C109 -147.1(8) . . . . ? C112 Yb1 C110 C109 145.7(4) . . . . ? C102 N12 C111 C112 150.1(5) . . . . ? C103 N12 C111 C112 -90.7(6) . . . . ? Yb1 N12 C111 C112 30.1(6) . . . . ? Yb1 O12 C112 N16 175.2(4) . . . . ? Yb1 O12 C112 C111 -3.1(8) . . . . ? C125 N16 C112 O12 -8.1(9) . . . . ? C125 N16 C112 C111 170.3(6) . . . . ? C125 N16 C112 Yb1 -1.8(14) . . . . ? N12 C111 C112 O12 -22.2(8) . . . . ? N12 C111 C112 N16 159.4(6) . . . . ? N12 C111 C112 Yb1 -24.0(5) . . . . ? O13 Yb1 C112 O12 -24.8(5) . . . . ? O14 Yb1 C112 O12 73.2(6) . . . . ? O11 Yb1 C112 O12 117.2(5) . . . . ? O11W Yb1 C112 O12 45.1(5) . . . . ? N14 Yb1 C112 O12 -102.8(5) . . . . ? N11 Yb1 C112 O12 171.7(5) . . . . ? N13 Yb1 C112 O12 -87.6(5) . . . . ? N12 Yb1 C112 O12 -161.2(6) . . . . ? C114 Yb1 C112 O12 -40.5(5) . . . . ? C110 Yb1 C112 O12 129.4(5) . . . . ? O12 Yb1 C112 N16 -9.5(8) . . . . ? O13 Yb1 C112 N16 -34.3(10) . . . . ? O14 Yb1 C112 N16 63.7(11) . . . . ? O11 Yb1 C112 N16 107.7(10) . . . . ? O11W Yb1 C112 N16 35.6(10) . . . . ? N14 Yb1 C112 N16 -112.3(10) . . . . ? N11 Yb1 C112 N16 162.1(10) . . . . ? N13 Yb1 C112 N16 -97.1(10) . . . . ? N12 Yb1 C112 N16 -170.7(11) . . . . ? C114 Yb1 C112 N16 -50.1(10) . . . . ? C110 Yb1 C112 N16 119.9(10) . . . . ? O12 Yb1 C112 C111 177.3(7) . . . . ? O13 Yb1 C112 C111 152.5(3) . . . . ? O14 Yb1 C112 C111 -109.5(4) . . . . ? O11 Yb1 C112 C111 -65.5(4) . . . . ? O11W Yb1 C112 C111 -137.6(4) . . . . ? N14 Yb1 C112 C111 74.5(4) . . . . ? N11 Yb1 C112 C111 -11.1(4) . . . . ? N13 Yb1 C112 C111 89.7(4) . . . . ? N12 Yb1 C112 C111 16.1(3) . . . . ? C114 Yb1 C112 C111 136.7(4) . . . . ? C110 Yb1 C112 C111 -53.3(4) . . . . ? C105 N13 C113 C114 -86.1(6) . . . . ? C104 N13 C113 C114 156.1(5) . . . . ? Yb1 N13 C113 C114 33.5(6) . . . . ? Yb1 O13 C114 N17 179.9(4) . . . . ? Yb1 O13 C114 C113 1.9(8) . . . . ? C133 N17 C114 O13 -0.5(10) . . . . ? C133 N17 C114 C113 177.6(6) . . . . ? C133 N17 C114 Yb1 -0.4(15) . . . . ? N13 C113 C114 O13 -27.3(9) . . . . ? N13 C113 C114 N17 154.7(6) . . . . ? N13 C113 C114 Yb1 -26.1(5) . . . . ? O12 Yb1 C114 O13 114.6(5) . . . . ? O14 Yb1 C114 O13 -26.4(5) . . . . ? O11 Yb1 C114 O13 79.7(6) . . . . ? O11W Yb1 C114 O13 42.1(5) . . . . ? N14 Yb1 C114 O13 -87.9(5) . . . . ? N11 Yb1 C114 O13 -105.7(5) . . . . ? N13 Yb1 C114 O13 -163.6(6) . . . . ? N12 Yb1 C114 O13 171.2(5) . . . . ? C110 Yb1 C114 O13 60.1(10) . . . . ? C112 Yb1 C114 O13 127.1(5) . . . . ? O12 Yb1 C114 N17 114.5(12) . . . . ? O13 Yb1 C114 N17 -0.2(10) . . . . ? O14 Yb1 C114 N17 -26.5(12) . . . . ? O11 Yb1 C114 N17 79.5(12) . . . . ? O11W Yb1 C114 N17 42.0(12) . . . . ? N14 Yb1 C114 N17 -88.0(12) . . . . ? N11 Yb1 C114 N17 -105.8(12) . . . . ? N13 Yb1 C114 N17 -163.8(12) . . . . ? N12 Yb1 C114 N17 171.1(11) . . . . ? C110 Yb1 C114 N17 60.0(16) . . . . ? C112 Yb1 C114 N17 127.0(12) . . . . ? O12 Yb1 C114 C113 -63.7(4) . . . . ? O13 Yb1 C114 C113 -178.4(7) . . . . ? O14 Yb1 C114 C113 155.3(4) . . . . ? O11 Yb1 C114 C113 -98.7(5) . . . . ? O11W Yb1 C114 C113 -136.2(4) . . . . ? N14 Yb1 C114 C113 93.7(4) . . . . ? N11 Yb1 C114 C113 76.0(5) . . . . ? N13 Yb1 C114 C113 18.0(4) . . . . ? N12 Yb1 C114 C113 -7.2(4) . . . . ? C110 Yb1 C114 C113 -118.2(8) . . . . ? C112 Yb1 C114 C113 -51.2(4) . . . . ? C106 N14 C115 C116 157.5(5) . . . . ? C107 N14 C115 C116 -83.6(6) . . . . ? Yb1 N14 C115 C116 36.4(6) . . . . ? Yb1 O14 C116 N18 173.5(5) . . . . ? Yb1 O14 C116 C115 -2.2(8) . . . . ? C141 N18 C116 O14 -1.5(10) . . . . ? C141 N18 C116 C115 174.4(6) . . . . ? C141 N18 C116 Yb1 9.4(17) . . . . ? N14 C115 C116 O14 -26.4(8) . . . . ? N14 C115 C116 N18 157.5(6) . . . . ? N14 C115 C116 Yb1 -27.8(5) . . . . ? O12 Yb1 C116 O14 76.1(6) . . . . ? O13 Yb1 C116 O14 119.2(5) . . . . ? O11 Yb1 C116 O14 -21.9(5) . . . . ? O11W Yb1 C116 O14 46.6(5) . . . . ? N14 Yb1 C116 O14 -158.6(6) . . . . ? N11 Yb1 C116 O14 -83.1(5) . . . . ? N13 Yb1 C116 O14 175.7(5) . . . . ? N12 Yb1 C116 O14 -101.4(5) . . . . ? C114 Yb1 C116 O14 132.2(5) . . . . ? C110 Yb1 C116 O14 -37.1(5) . . . . ? C112 Yb1 C116 O14 50.1(10) . . . . ? O12 Yb1 C116 N18 60.7(14) . . . . ? O13 Yb1 C116 N18 103.8(13) . . . . ? O14 Yb1 C116 N18 -15.4(11) . . . . ? O11 Yb1 C116 N18 -37.4(13) . . . . ? O11W Yb1 C116 N18 31.1(13) . . . . ? N14 Yb1 C116 N18 -174.0(14) . . . . ? N11 Yb1 C116 N18 -98.5(13) . . . . ? N13 Yb1 C116 N18 160.3(13) . . . . ? N12 Yb1 C116 N18 -116.8(13) . . . . ? C114 Yb1 C116 N18 116.8(13) . . . . ? C110 Yb1 C116 N18 -52.5(13) . . . . ? C112 Yb1 C116 N18 34.7(18) . . . . ? O12 Yb1 C116 C115 -105.8(4) . . . . ? O13 Yb1 C116 C115 -62.8(4) . . . . ? O14 Yb1 C116 C115 178.0(7) . . . . ? O11 Yb1 C116 C115 156.1(3) . . . . ? O11W Yb1 C116 C115 -135.4(4) . . . . ? N14 Yb1 C116 C115 19.5(3) . . . . ? N11 Yb1 C116 C115 95.0(4) . . . . ? N13 Yb1 C116 C115 -6.2(4) . . . . ? N12 Yb1 C116 C115 76.6(4) . . . . ? C114 Yb1 C116 C115 -49.7(4) . . . . ? C110 Yb1 C116 C115 141.0(4) . . . . ? C112 Yb1 C116 C115 -131.9(7) . . . . ? C110 N15 C117 C124 -153.0(7) . . . . ? C110 N15 C117 C118 84.5(8) . . . . ? N15 C117 C118 C123 43.6(9) . . . . ? C124 C117 C118 C123 -77.3(9) . . . . ? N15 C117 C118 C119 -137.2(7) . . . . ? C124 C117 C118 C119 101.8(8) . . . . ? C123 C118 C119 C120 -1.1(12) . . . . ? C117 C118 C119 C120 179.8(8) . . . . ? C118 C119 C120 C121 1.4(14) . . . . ? C119 C120 C121 C122 -0.7(15) . . . . ? C120 C121 C122 C123 -0.3(15) . . . . ? C119 C118 C123 C122 0.1(12) . . . . ? C117 C118 C123 C122 179.2(8) . . . . ? C121 C122 C123 C118 0.6(14) . . . . ? C112 N16 C125 C126 74.3(8) . . . . ? C112 N16 C125 C132 -162.0(6) . . . . ? N16 C125 C126 C131 48.6(9) . . . . ? C132 C125 C126 C131 -73.9(9) . . . . ? N16 C125 C126 C127 -133.5(7) . . . . ? C132 C125 C126 C127 104.0(8) . . . . ? C131 C126 C127 C128 1.2(11) . . . . ? C125 C126 C127 C128 -176.8(7) . . . . ? C126 C127 C128 C129 -2.3(13) . . . . ? C127 C128 C129 C130 2.1(14) . . . . ? C128 C129 C130 C131 -0.8(13) . . . . ? C127 C126 C131 C130 0.1(11) . . . . ? C125 C126 C131 C130 177.9(7) . . . . ? C129 C130 C131 C126 -0.3(12) . . . . ? C114 N17 C133 C134 76.5(8) . . . . ? C114 N17 C133 C140 -160.4(6) . . . . ? N17 C133 C134 C135 -136.3(6) . . . . ? C140 C133 C134 C135 103.1(7) . . . . ? N17 C133 C134 C139 48.1(8) . . . . ? C140 C133 C134 C139 -72.6(8) . . . . ? C139 C134 C135 C136 0.7(11) . . . . ? C133 C134 C135 C136 -175.0(7) . . . . ? C134 C135 C136 C137 -1.2(12) . . . . ? C135 C136 C137 C138 0.9(12) . . . . ? C136 C137 C138 C139 -0.1(12) . . . . ? C137 C138 C139 C134 -0.3(11) . . . . ? C135 C134 C139 C138 0.1(10) . . . . ? C133 C134 C139 C138 175.7(6) . . . . ? C116 N18 C141 C42A 64.8(10) . . . . ? C116 N18 C141 C148 -161.8(6) . . . . ? C116 N18 C141 C142 83.0(8) . . . . ? C42A C141 C142 C143 -0.9(17) . . . . ? N18 C141 C142 C143 -129.3(7) . . . . ? C148 C141 C142 C143 114.8(7) . . . . ? C42A C141 C142 C147 -178(2) . . . . ? N18 C141 C142 C147 53.5(8) . . . . ? C148 C141 C142 C147 -62.4(8) . . . . ? C147 C142 C143 C144 0.0 . . . . ? C141 C142 C143 C144 -177.2(9) . . . . ? C142 C143 C144 C145 0.0 . . . . ? C143 C144 C145 C146 0.0 . . . . ? C144 C145 C146 C147 0.0 . . . . ? C145 C146 C147 C142 0.0 . . . . ? C143 C142 C147 C146 0.0 . . . . ? C141 C142 C147 C146 177.1(9) . . . . ? N18 C141 C42A C43A -127.0(8) . . . . ? C148 C141 C42A C43A 102.7(9) . . . . ? C142 C141 C42A C43A 175(2) . . . . ? N18 C141 C42A C47A 55.1(10) . . . . ? C148 C141 C42A C47A -75.2(9) . . . . ? C142 C141 C42A C47A -3.1(15) . . . . ? C47A C42A C43A C44A 0.0 . . . . ? C141 C42A C43A C44A -177.8(11) . . . . ? C42A C43A C44A C45A 0.0 . . . . ? C43A C44A C45A C46A 0.0 . . . . ? C44A C45A C46A C47A 0.0 . . . . ? C45A C46A C47A C42A 0.0 . . . . ? C43A C42A C47A C46A 0.0 . . . . ? C141 C42A C47A C46A 178.0(10) . . . . ? O24 Yb2 O21 C210 -64.1(5) . . . . ? O22 Yb2 O21 C210 152.0(5) . . . . ? O23 Yb2 O21 C210 -134.6(5) . . . . ? O29W Yb2 O21 C210 -137.2(5) . . . . ? N24 Yb2 O21 C210 -14.0(6) . . . . ? N23 Yb2 O21 C210 98.3(5) . . . . ? N22 Yb2 O21 C210 85.5(5) . . . . ? N21 Yb2 O21 C210 13.6(5) . . . . ? C216 Yb2 O21 C210 -55.3(5) . . . . ? C212 Yb2 O21 C210 136.2(5) . . . . ? C214 Yb2 O21 C210 -165.2(4) . . . . ? O24 Yb2 O22 C212 -124.6(5) . . . . ? O21 Yb2 O22 C212 -53.7(5) . . . . ? O23 Yb2 O22 C212 163.3(6) . . . . ? O29W Yb2 O22 C212 -124.4(6) . . . . ? N24 Yb2 O22 C212 109.4(5) . . . . ? N23 Yb2 O22 C212 95.2(5) . . . . ? N22 Yb2 O22 C212 21.4(5) . . . . ? N21 Yb2 O22 C212 1.3(6) . . . . ? C216 Yb2 O22 C212 -155.1(5) . . . . ? C214 Yb2 O22 C212 147.6(6) . . . . ? O24 Yb2 O23 C214 163.5(5) . . . . ? O22 Yb2 O23 C214 -52.5(5) . . . . ? O21 Yb2 O23 C214 -127.4(5) . . . . ? O29W Yb2 O23 C214 -124.7(5) . . . . ? N24 Yb2 O23 C214 95.3(5) . . . . ? N23 Yb2 O23 C214 20.8(5) . . . . ? N22 Yb2 O23 C214 -3.5(6) . . . . ? N21 Yb2 O23 C214 105.2(5) . . . . ? C216 Yb2 O23 C214 145.9(5) . . . . ? C212 Yb2 O23 C214 -47.0(5) . . . . ? O22 Yb2 O24 C216 -134.5(5) . . . . ? O21 Yb2 O24 C216 152.8(5) . . . . ? O23 Yb2 O24 C216 -63.3(5) . . . . ? O29W Yb2 O24 C216 -134.7(5) . . . . ? N24 Yb2 O24 C216 11.8(5) . . . . ? N23 Yb2 O24 C216 -12.4(6) . . . . ? N22 Yb2 O24 C216 101.0(5) . . . . ? N21 Yb2 O24 C216 84.2(5) . . . . ? C212 Yb2 O24 C216 -166.3(5) . . . . ? C214 Yb2 O24 C216 -57.9(5) . . . . ? O24 Yb2 N21 C201 -175.4(4) . . . . ? O22 Yb2 N21 C201 35.6(5) . . . . ? O21 Yb2 N21 C201 98.2(4) . . . . ? O23 Yb2 N21 C201 -114.3(4) . . . . ? O29W Yb2 N21 C201 134.5(4) . . . . ? N24 Yb2 N21 C201 -104.0(4) . . . . ? N23 Yb2 N21 C201 -43.0(4) . . . . ? N22 Yb2 N21 C201 15.8(4) . . . . ? C216 Yb2 N21 C201 -155.5(4) . . . . ? C212 Yb2 N21 C201 36.1(5) . . . . ? C214 Yb2 N21 C201 -82.7(5) . . . . ? O24 Yb2 N21 C209 64.6(4) . . . . ? O22 Yb2 N21 C209 -84.4(4) . . . . ? O21 Yb2 N21 C209 -21.8(4) . . . . ? O23 Yb2 N21 C209 125.8(4) . . . . ? O29W Yb2 N21 C209 14.5(5) . . . . ? N24 Yb2 N21 C209 136.0(4) . . . . ? N23 Yb2 N21 C209 -163.0(4) . . . . ? N22 Yb2 N21 C209 -104.2(4) . . . . ? C216 Yb2 N21 C209 84.5(4) . . . . ? C212 Yb2 N21 C209 -83.9(4) . . . . ? C214 Yb2 N21 C209 157.3(4) . . . . ? O24 Yb2 N21 C208 -53.0(4) . . . . ? O22 Yb2 N21 C208 158.0(4) . . . . ? O21 Yb2 N21 C208 -139.4(4) . . . . ? O23 Yb2 N21 C208 8.1(5) . . . . ? O29W Yb2 N21 C208 -103.1(4) . . . . ? N24 Yb2 N21 C208 18.4(4) . . . . ? N23 Yb2 N21 C208 79.4(4) . . . . ? N22 Yb2 N21 C208 138.2(4) . . . . ? C216 Yb2 N21 C208 -33.1(4) . . . . ? C212 Yb2 N21 C208 158.5(4) . . . . ? C214 Yb2 N21 C208 39.7(5) . . . . ? O24 Yb2 N22 C202 -2.6(6) . . . . ? O22 Yb2 N22 C202 -149.0(5) . . . . ? O21 Yb2 N22 C202 -56.1(4) . . . . ? O23 Yb2 N22 C202 156.3(4) . . . . ? O29W Yb2 N22 C202 -108.1(4) . . . . ? N24 Yb2 N22 C202 72.4(4) . . . . ? N23 Yb2 N22 C202 132.2(5) . . . . ? N21 Yb2 N22 C202 15.0(4) . . . . ? C216 Yb2 N22 C202 28.4(5) . . . . ? C212 Yb2 N22 C202 -139.8(5) . . . . ? C214 Yb2 N22 C202 155.1(4) . . . . ? O24 Yb2 N22 C211 116.2(4) . . . . ? O22 Yb2 N22 C211 -30.2(4) . . . . ? O21 Yb2 N22 C211 62.7(4) . . . . ? O23 Yb2 N22 C211 -84.9(4) . . . . ? O29W Yb2 N22 C211 10.6(4) . . . . ? N24 Yb2 N22 C211 -168.8(4) . . . . ? N23 Yb2 N22 C211 -109.0(4) . . . . ? N21 Yb2 N22 C211 133.7(4) . . . . ? C216 Yb2 N22 C211 147.2(4) . . . . ? C212 Yb2 N22 C211 -21.1(4) . . . . ? C214 Yb2 N22 C211 -86.2(4) . . . . ? O24 Yb2 N22 C203 -124.2(4) . . . . ? O22 Yb2 N22 C203 89.4(5) . . . . ? O21 Yb2 N22 C203 -177.7(5) . . . . ? O23 Yb2 N22 C203 34.7(5) . . . . ? O29W Yb2 N22 C203 130.3(4) . . . . ? N24 Yb2 N22 C203 -49.2(5) . . . . ? N23 Yb2 N22 C203 10.6(4) . . . . ? N21 Yb2 N22 C203 -106.6(5) . . . . ? C216 Yb2 N22 C203 -93.2(5) . . . . ? C212 Yb2 N22 C203 98.6(5) . . . . ? C214 Yb2 N22 C203 33.5(5) . . . . ? O24 Yb2 N23 C204 158.8(4) . . . . ? O22 Yb2 N23 C204 -54.5(4) . . . . ? O21 Yb2 N23 C204 3.5(6) . . . . ? O23 Yb2 N23 C204 -143.9(5) . . . . ? O29W Yb2 N23 C204 -102.6(4) . . . . ? N24 Yb2 N23 C204 135.0(5) . . . . ? N22 Yb2 N23 C204 16.7(4) . . . . ? N21 Yb2 N23 C204 75.1(5) . . . . ? C216 Yb2 N23 C204 154.4(4) . . . . ? C212 Yb2 N23 C204 -34.7(4) . . . . ? C214 Yb2 N23 C204 -135.2(5) . . . . ? O24 Yb2 N23 C213 -80.3(5) . . . . ? O22 Yb2 N23 C213 66.4(4) . . . . ? O21 Yb2 N23 C213 124.3(4) . . . . ? O23 Yb2 N23 C213 -23.0(4) . . . . ? O29W Yb2 N23 C213 18.3(5) . . . . ? N24 Yb2 N23 C213 -104.1(4) . . . . ? N22 Yb2 N23 C213 137.6(5) . . . . ? N21 Yb2 N23 C213 -164.1(4) . . . . ? C216 Yb2 N23 C213 -84.8(5) . . . . ? C212 Yb2 N23 C213 86.2(4) . . . . ? C214 Yb2 N23 C213 -14.3(4) . . . . ? O24 Yb2 N23 C205 38.3(5) . . . . ? O22 Yb2 N23 C205 -175.0(4) . . . . ? O21 Yb2 N23 C205 -117.1(4) . . . . ? O23 Yb2 N23 C205 95.5(4) . . . . ? O29W Yb2 N23 C205 136.8(4) . . . . ? N24 Yb2 N23 C205 14.5(4) . . . . ? N22 Yb2 N23 C205 -103.9(4) . . . . ? N21 Yb2 N23 C205 -45.5(4) . . . . ? C216 Yb2 N23 C205 33.8(4) . . . . ? C212 Yb2 N23 C205 -155.2(4) . . . . ? C214 Yb2 N23 C205 104.3(4) . . . . ? O24 Yb2 N24 C206 -146.2(5) . . . . ? O22 Yb2 N24 C206 1.2(6) . . . . ? O21 Yb2 N24 C206 158.7(4) . . . . ? O23 Yb2 N24 C206 -55.1(4) . . . . ? O29W Yb2 N24 C206 -105.1(4) . . . . ? N23 Yb2 N24 C206 15.5(4) . . . . ? N22 Yb2 N24 C206 74.3(4) . . . . ? N21 Yb2 N24 C206 131.4(5) . . . . ? C216 Yb2 N24 C206 -141.1(5) . . . . ? C212 Yb2 N24 C206 32.2(6) . . . . ? C214 Yb2 N24 C206 -35.8(4) . . . . ? O24 Yb2 N24 C215 -27.0(4) . . . . ? O22 Yb2 N24 C215 120.4(4) . . . . ? O21 Yb2 N24 C215 -82.1(4) . . . . ? O23 Yb2 N24 C215 64.1(4) . . . . ? O29W Yb2 N24 C215 14.1(5) . . . . ? N23 Yb2 N24 C215 134.7(4) . . . . ? N22 Yb2 N24 C215 -166.5(4) . . . . ? N21 Yb2 N24 C215 -109.4(4) . . . . ? C216 Yb2 N24 C215 -21.9(4) . . . . ? C212 Yb2 N24 C215 151.4(4) . . . . ? C214 Yb2 N24 C215 83.5(4) . . . . ? O24 Yb2 N24 C207 91.5(4) . . . . ? O22 Yb2 N24 C207 -121.1(4) . . . . ? O21 Yb2 N24 C207 36.4(5) . . . . ? O23 Yb2 N24 C207 -177.4(5) . . . . ? O29W Yb2 N24 C207 132.6(4) . . . . ? N23 Yb2 N24 C207 -106.8(5) . . . . ? N22 Yb2 N24 C207 -48.0(5) . . . . ? N21 Yb2 N24 C207 9.1(4) . . . . ? C216 Yb2 N24 C207 96.7(5) . . . . ? C212 Yb2 N24 C207 -90.1(5) . . . . ? C214 Yb2 N24 C207 -158.0(5) . . . . ? C209 N21 C201 C202 73.6(6) . . . . ? C208 N21 C201 C202 -168.3(5) . . . . ? Yb2 N21 C201 C202 -45.4(6) . . . . ? C211 N22 C202 C201 -160.1(5) . . . . ? C203 N22 C202 C201 81.0(6) . . . . ? Yb2 N22 C202 C201 -43.3(6) . . . . ? N21 C201 C202 N22 61.0(7) . . . . ? C202 N22 C203 C204 -161.2(6) . . . . ? C211 N22 C203 C204 80.4(7) . . . . ? Yb2 N22 C203 C204 -37.1(7) . . . . ? C213 N23 C204 C203 -163.3(6) . . . . ? C205 N23 C204 C203 76.6(7) . . . . ? Yb2 N23 C204 C203 -43.1(7) . . . . ? N22 C203 C204 N23 55.0(8) . . . . ? C204 N23 C205 C206 -166.6(6) . . . . ? C213 N23 C205 C206 73.2(7) . . . . ? Yb2 N23 C205 C206 -44.6(6) . . . . ? C215 N24 C206 C205 -160.5(6) . . . . ? C207 N24 C206 C205 79.8(7) . . . . ? Yb2 N24 C206 C205 -44.3(7) . . . . ? N23 C205 C206 N24 62.7(8) . . . . ? C206 N24 C207 C208 -159.5(6) . . . . ? C215 N24 C207 C208 79.9(7) . . . . ? Yb2 N24 C207 C208 -36.7(7) . . . . ? C201 N21 C208 C207 77.5(7) . . . . ? C209 N21 C208 C207 -163.2(6) . . . . ? Yb2 N21 C208 C207 -45.4(6) . . . . ? N24 C207 C208 N21 56.4(8) . . . . ? C201 N21 C209 C210 -92.4(6) . . . . ? C208 N21 C209 C210 148.1(5) . . . . ? Yb2 N21 C209 C210 28.5(6) . . . . ? Yb2 O21 C210 N25 175.6(4) . . . . ? Yb2 O21 C210 C209 -1.8(8) . . . . ? C217 N25 C210 O21 -9.8(10) . . . . ? C217 N25 C210 C209 167.6(6) . . . . ? C217 N25 C210 Yb2 -3.4(15) . . . . ? N21 C209 C210 O21 -21.1(8) . . . . ? N21 C209 C210 N25 161.5(6) . . . . ? N21 C209 C210 Yb2 -22.1(5) . . . . ? O24 Yb2 C210 O21 112.1(5) . . . . ? O22 Yb2 C210 O21 -28.8(5) . . . . ? O23 Yb2 C210 O21 69.5(6) . . . . ? O29W Yb2 C210 O21 40.1(5) . . . . ? N24 Yb2 C210 O21 168.6(5) . . . . ? N23 Yb2 C210 O21 -105.7(5) . . . . ? N22 Yb2 C210 O21 -89.4(5) . . . . ? N21 Yb2 C210 O21 -163.3(6) . . . . ? C216 Yb2 C210 O21 125.4(5) . . . . ? C212 Yb2 C210 O21 -42.1(5) . . . . ? C214 Yb2 C210 O21 34.3(10) . . . . ? O24 Yb2 C210 N25 102.6(11) . . . . ? O22 Yb2 C210 N25 -38.2(11) . . . . ? O21 Yb2 C210 N25 -9.4(10) . . . . ? O23 Yb2 C210 N25 60.1(12) . . . . ? O29W Yb2 C210 N25 30.6(11) . . . . ? N24 Yb2 C210 N25 159.1(11) . . . . ? N23 Yb2 C210 N25 -115.2(11) . . . . ? N22 Yb2 C210 N25 -98.8(11) . . . . ? N21 Yb2 C210 N25 -172.8(12) . . . . ? C216 Yb2 C210 N25 116.0(11) . . . . ? C212 Yb2 C210 N25 -51.6(11) . . . . ? C214 Yb2 C210 N25 24.8(16) . . . . ? O24 Yb2 C210 C209 -69.5(4) . . . . ? O22 Yb2 C210 C209 149.7(4) . . . . ? O21 Yb2 C210 C209 178.5(7) . . . . ? O23 Yb2 C210 C209 -112.0(4) . . . . ? O29W Yb2 C210 C209 -141.5(4) . . . . ? N24 Yb2 C210 C209 -13.0(4) . . . . ? N23 Yb2 C210 C209 72.7(4) . . . . ? N22 Yb2 C210 C209 89.1(4) . . . . ? N21 Yb2 C210 C209 15.2(3) . . . . ? C216 Yb2 C210 C209 -56.1(4) . . . . ? C212 Yb2 C210 C209 136.3(4) . . . . ? C214 Yb2 C210 C209 -147.3(6) . . . . ? C202 N22 C211 C212 158.3(5) . . . . ? C203 N22 C211 C212 -84.1(6) . . . . ? Yb2 N22 C211 C212 37.4(6) . . . . ? Yb2 O22 C212 N26 169.1(5) . . . . ? Yb2 O22 C212 C211 -6.9(9) . . . . ? C225 N26 C212 O22 1.9(11) . . . . ? C225 N26 C212 C211 178.0(7) . . . . ? C225 N26 C212 Yb2 18.1(17) . . . . ? N22 C211 C212 O22 -25.0(9) . . . . ? N22 C211 C212 N26 158.9(6) . . . . ? N22 C211 C212 Yb2 -29.1(5) . . . . ? O24 Yb2 C212 O22 81.9(6) . . . . ? O21 Yb2 C212 O22 123.8(6) . . . . ? O23 Yb2 C212 O22 -16.8(6) . . . . ? O29W Yb2 C212 O22 51.8(5) . . . . ? N24 Yb2 C212 O22 -95.2(6) . . . . ? N23 Yb2 C212 O22 -79.0(5) . . . . ? N22 Yb2 C212 O22 -153.7(6) . . . . ? N21 Yb2 C212 O22 -178.9(5) . . . . ? C216 Yb2 C212 O22 61.4(10) . . . . ? C214 Yb2 C212 O22 -30.6(5) . . . . ? O24 Yb2 C212 N26 58.2(13) . . . . ? O22 Yb2 C212 N26 -23.7(11) . . . . ? O21 Yb2 C212 N26 100.2(12) . . . . ? O23 Yb2 C212 N26 -40.5(13) . . . . ? O29W Yb2 C212 N26 28.2(12) . . . . ? N24 Yb2 C212 N26 -118.9(12) . . . . ? N23 Yb2 C212 N26 -102.6(12) . . . . ? N22 Yb2 C212 N26 -177.3(13) . . . . ? N21 Yb2 C212 N26 157.4(12) . . . . ? C216 Yb2 C212 N26 37.7(17) . . . . ? C214 Yb2 C212 N26 -54.2(12) . . . . ? O24 Yb2 C212 C211 -104.1(5) . . . . ? O22 Yb2 C212 C211 173.9(8) . . . . ? O21 Yb2 C212 C211 -62.2(4) . . . . ? O23 Yb2 C212 C211 157.1(4) . . . . ? O29W Yb2 C212 C211 -134.2(4) . . . . ? N24 Yb2 C212 C211 78.7(5) . . . . ? N23 Yb2 C212 C211 95.0(4) . . . . ? N22 Yb2 C212 C211 20.3(4) . . . . ? N21 Yb2 C212 C211 -5.0(4) . . . . ? C216 Yb2 C212 C211 -124.7(7) . . . . ? C214 Yb2 C212 C211 143.4(4) . . . . ? C204 N23 C213 C214 147.6(6) . . . . ? C205 N23 C213 C214 -92.3(7) . . . . ? Yb2 N23 C213 C214 25.4(7) . . . . ? Yb2 O23 C214 N27 167.0(5) . . . . ? Yb2 O23 C214 C213 -13.9(8) . . . . ? C233 N27 C214 O23 -4.4(10) . . . . ? C233 N27 C214 C213 176.6(6) . . . . ? C233 N27 C214 Yb2 15.4(16) . . . . ? N23 C213 C214 O23 -11.3(9) . . . . ? N23 C213 C214 N27 167.7(6) . . . . ? N23 C213 C214 Yb2 -19.6(5) . . . . ? O24 Yb2 C214 O23 -16.9(5) . . . . ? O22 Yb2 C214 O23 123.8(5) . . . . ? O21 Yb2 C214 O23 78.2(6) . . . . ? O29W Yb2 C214 O23 51.6(5) . . . . ? N24 Yb2 C214 O23 -79.8(5) . . . . ? N23 Yb2 C214 O23 -154.5(6) . . . . ? N22 Yb2 C214 O23 177.1(5) . . . . ? N21 Yb2 C214 O23 -100.1(5) . . . . ? C216 Yb2 C214 O23 -33.2(5) . . . . ? C212 Yb2 C214 O23 134.0(5) . . . . ? O24 Yb2 C214 N27 -45.8(12) . . . . ? O22 Yb2 C214 N27 95.0(12) . . . . ? O21 Yb2 C214 N27 49.3(13) . . . . ? O23 Yb2 C214 N27 -28.8(10) . . . . ? O29W Yb2 C214 N27 22.8(12) . . . . ? N24 Yb2 C214 N27 -108.7(12) . . . . ? N23 Yb2 C214 N27 176.7(13) . . . . ? N22 Yb2 C214 N27 148.3(12) . . . . ? N21 Yb2 C214 N27 -128.9(12) . . . . ? C216 Yb2 C214 N27 -62.0(12) . . . . ? C212 Yb2 C214 N27 105.2(12) . . . . ? O24 Yb2 C214 C213 151.0(4) . . . . ? O22 Yb2 C214 C213 -68.2(4) . . . . ? O21 Yb2 C214 C213 -113.9(5) . . . . ? O23 Yb2 C214 C213 167.9(7) . . . . ? O29W Yb2 C214 C213 -140.5(4) . . . . ? N24 Yb2 C214 C213 88.1(4) . . . . ? N23 Yb2 C214 C213 13.4(4) . . . . ? N22 Yb2 C214 C213 -14.9(4) . . . . ? N21 Yb2 C214 C213 67.8(5) . . . . ? C216 Yb2 C214 C213 134.8(4) . . . . ? C212 Yb2 C214 C213 -58.1(4) . . . . ? C206 N24 C215 C216 157.8(6) . . . . ? C207 N24 C215 C216 -82.2(7) . . . . ? Yb2 N24 C215 C216 38.7(6) . . . . ? Yb2 O24 C216 N28 -173.7(5) . . . . ? Yb2 O24 C216 C215 7.6(9) . . . . ? C241 N28 C216 O24 -2.3(10) . . . . ? C241 N28 C216 C215 176.4(6) . . . . ? C241 N28 C216 Yb2 -12.3(17) . . . . ? N24 C215 C216 O24 -34.5(9) . . . . ? N24 C215 C216 N28 146.7(6) . . . . ? N24 C215 C216 Yb2 -30.0(5) . . . . ? O22 Yb2 C216 O24 71.4(6) . . . . ? O21 Yb2 C216 O24 -27.2(5) . . . . ? O23 Yb2 C216 O24 113.9(5) . . . . ? O29W Yb2 C216 O24 42.5(5) . . . . ? N24 Yb2 C216 O24 -165.4(6) . . . . ? N23 Yb2 C216 O24 170.2(5) . . . . ? N22 Yb2 C216 O24 -103.5(5) . . . . ? N21 Yb2 C216 O24 -90.5(5) . . . . ? C212 Yb2 C216 O24 33.0(10) . . . . ? C214 Yb2 C216 O24 124.4(5) . . . . ? O24 Yb2 C216 N28 14.4(11) . . . . ? O22 Yb2 C216 N28 85.8(14) . . . . ? O21 Yb2 C216 N28 -12.7(13) . . . . ? O23 Yb2 C216 N28 128.3(13) . . . . ? O29W Yb2 C216 N28 56.9(13) . . . . ? N24 Yb2 C216 N28 -151.0(14) . . . . ? N23 Yb2 C216 N28 -175.4(13) . . . . ? N22 Yb2 C216 N28 -89.0(14) . . . . ? N21 Yb2 C216 N28 -76.1(13) . . . . ? C212 Yb2 C216 N28 47.4(18) . . . . ? C214 Yb2 C216 N28 138.8(13) . . . . ? O24 Yb2 C216 C215 -173.3(8) . . . . ? O22 Yb2 C216 C215 -101.9(5) . . . . ? O21 Yb2 C216 C215 159.5(4) . . . . ? O23 Yb2 C216 C215 -59.4(4) . . . . ? O29W Yb2 C216 C215 -130.8(4) . . . . ? N24 Yb2 C216 C215 21.3(4) . . . . ? N23 Yb2 C216 C215 -3.1(5) . . . . ? N22 Yb2 C216 C215 83.2(5) . . . . ? N21 Yb2 C216 C215 96.2(4) . . . . ? C212 Yb2 C216 C215 -140.3(7) . . . . ? C214 Yb2 C216 C215 -48.9(4) . . . . ? C210 N25 C217 C218 84.6(7) . . . . ? C210 N25 C217 C224 -151.1(6) . . . . ? N25 C217 C218 C223 54.2(8) . . . . ? C224 C217 C218 C223 -68.1(8) . . . . ? N25 C217 C218 C219 -128.7(7) . . . . ? C224 C217 C218 C219 109.0(8) . . . . ? C223 C218 C219 C220 2.4(12) . . . . ? C217 C218 C219 C220 -174.7(8) . . . . ? C218 C219 C220 C221 -1.9(15) . . . . ? C219 C220 C221 C222 1.1(16) . . . . ? C220 C221 C222 C223 -1.0(14) . . . . ? C219 C218 C223 C222 -2.3(11) . . . . ? C217 C218 C223 C222 174.8(6) . . . . ? C221 C222 C223 C218 1.6(12) . . . . ? C212 N26 C225 C232 -145.0(7) . . . . ? C212 N26 C225 C226 91.8(9) . . . . ? N26 C225 C226 C231 59.5(10) . . . . ? C232 C225 C226 C231 -62.2(11) . . . . ? N26 C225 C226 C227 -123.5(8) . . . . ? C232 C225 C226 C227 114.8(9) . . . . ? C231 C226 C227 C228 -0.4(13) . . . . ? C225 C226 C227 C228 -177.4(8) . . . . ? C226 C227 C228 C229 1.3(16) . . . . ? C227 C228 C229 C230 -2.1(18) . . . . ? C228 C229 C230 C231 2.0(18) . . . . ? C227 C226 C231 C230 0.4(14) . . . . ? C225 C226 C231 C230 177.3(8) . . . . ? C229 C230 C231 C226 -1.1(16) . . . . ? C214 N27 C233 C234 71.2(8) . . . . ? C214 N27 C233 C240 -165.0(6) . . . . ? N27 C233 C234 C235 -129.8(6) . . . . ? C240 C233 C234 C235 108.4(7) . . . . ? N27 C233 C234 C239 52.1(8) . . . . ? C240 C233 C234 C239 -69.6(7) . . . . ? C239 C234 C235 C236 1.0(10) . . . . ? C233 C234 C235 C236 -177.1(6) . . . . ? C234 C235 C236 C237 -0.2(11) . . . . ? C235 C236 C237 C238 -0.2(11) . . . . ? C236 C237 C238 C239 -0.2(11) . . . . ? C235 C234 C239 C238 -1.3(9) . . . . ? C233 C234 C239 C238 176.7(6) . . . . ? C237 C238 C239 C234 1.0(10) . . . . ? C216 N28 C241 C248 -156.4(6) . . . . ? C216 N28 C241 C242 79.2(8) . . . . ? N28 C241 C242 C243 -128.9(6) . . . . ? C248 C241 C242 C243 108.3(7) . . . . ? N28 C241 C242 C247 56.4(8) . . . . ? C248 C241 C242 C247 -66.4(8) . . . . ? C247 C242 C243 C244 -0.7(10) . . . . ? C241 C242 C243 C244 -175.5(6) . . . . ? C242 C243 C244 C245 0.3(11) . . . . ? C243 C244 C245 C246 -0.6(11) . . . . ? C244 C245 C246 C247 1.2(11) . . . . ? C245 C246 C247 C242 -1.6(11) . . . . ? C243 C242 C247 C246 1.3(10) . . . . ? C241 C242 C247 C246 176.2(6) . . . . ? O32 Yb3 O31 C310 156.6(5) . . . . ? O34 Yb3 O31 C310 -61.2(5) . . . . ? O33 Yb3 O31 C310 -133.7(4) . . . . ? O31W Yb3 O31 C310 -130.8(5) . . . . ? N31 Yb3 O31 C310 13.8(4) . . . . ? N33 Yb3 O31 C310 101.6(5) . . . . ? N32 Yb3 O31 C310 87.9(5) . . . . ? N34 Yb3 O31 C310 -8.5(5) . . . . ? C314 Yb3 O31 C310 -163.1(4) . . . . ? C312 Yb3 O31 C310 139.9(5) . . . . ? C316 Yb3 O31 C310 -52.9(5) . . . . ? O34 Yb3 O32 C312 -132.1(5) . . . . ? O33 Yb3 O32 C312 158.4(5) . . . . ? O31 Yb3 O32 C312 -57.5(5) . . . . ? O31W Yb3 O32 C312 -127.7(5) . . . . ? N31 Yb3 O32 C312 -7.5(5) . . . . ? N33 Yb3 O32 C312 89.6(5) . . . . ? N32 Yb3 O32 C312 17.1(4) . . . . ? N34 Yb3 O32 C312 104.7(5) . . . . ? C314 Yb3 O32 C312 140.6(5) . . . . ? C316 Yb3 O32 C312 -161.6(4) . . . . ? O32 Yb3 O33 C314 -65.4(5) . . . . ? O34 Yb3 O33 C314 151.3(5) . . . . ? O31 Yb3 O33 C314 -135.5(4) . . . . ? O31W Yb3 O33 C314 -138.3(5) . . . . ? N31 Yb3 O33 C314 97.9(5) . . . . ? N33 Yb3 O33 C314 10.1(5) . . . . ? N32 Yb3 O33 C314 -14.3(6) . . . . ? N34 Yb3 O33 C314 83.3(5) . . . . ? C312 Yb3 O33 C314 -58.3(5) . . . . ? C316 Yb3 O33 C314 133.9(5) . . . . ? O32 Yb3 O34 C316 -131.4(5) . . . . ? O33 Yb3 O34 C316 -62.0(5) . . . . ? O31 Yb3 O34 C316 154.5(5) . . . . ? O31W Yb3 O34 C316 -135.9(5) . . . . ? N31 Yb3 O34 C316 87.0(5) . . . . ? N33 Yb3 O34 C316 -10.7(6) . . . . ? N32 Yb3 O34 C316 100.2(5) . . . . ? N34 Yb3 O34 C316 14.1(5) . . . . ? C314 Yb3 O34 C316 -52.9(5) . . . . ? C312 Yb3 O34 C316 -161.0(4) . . . . ? O32 Yb3 N31 C309 -82.9(4) . . . . ? O34 Yb3 N31 C309 64.4(4) . . . . ? O33 Yb3 N31 C309 120.2(4) . . . . ? O31 Yb3 N31 C309 -27.1(3) . . . . ? O31W Yb3 N31 C309 13.9(4) . . . . ? N33 Yb3 N31 C309 -165.6(3) . . . . ? N32 Yb3 N31 C309 -107.2(4) . . . . ? N34 Yb3 N31 C309 135.4(4) . . . . ? C314 Yb3 N31 C309 150.7(3) . . . . ? C312 Yb3 N31 C309 -85.5(4) . . . . ? C316 Yb3 N31 C309 84.1(4) . . . . ? O32 Yb3 N31 C301 37.4(4) . . . . ? O34 Yb3 N31 C301 -175.4(4) . . . . ? O33 Yb3 N31 C301 -119.5(4) . . . . ? O31 Yb3 N31 C301 93.1(4) . . . . ? O31W Yb3 N31 C301 134.2(3) . . . . ? N33 Yb3 N31 C301 -45.4(4) . . . . ? N32 Yb3 N31 C301 13.1(3) . . . . ? N34 Yb3 N31 C301 -104.3(4) . . . . ? C314 Yb3 N31 C301 -89.1(4) . . . . ? C312 Yb3 N31 C301 34.7(4) . . . . ? C316 Yb3 N31 C301 -155.6(4) . . . . ? O32 Yb3 N31 C308 157.8(3) . . . . ? O34 Yb3 N31 C308 -54.9(4) . . . . ? O33 Yb3 N31 C308 0.9(5) . . . . ? O31 Yb3 N31 C308 -146.4(4) . . . . ? O31W Yb3 N31 C308 -105.4(4) . . . . ? N33 Yb3 N31 C308 75.1(4) . . . . ? N32 Yb3 N31 C308 133.6(4) . . . . ? N34 Yb3 N31 C308 16.1(3) . . . . ? C314 Yb3 N31 C308 31.4(5) . . . . ? C312 Yb3 N31 C308 155.2(3) . . . . ? C316 Yb3 N31 C308 -35.2(4) . . . . ? O32 Yb3 N32 C303 92.9(4) . . . . ? O34 Yb3 N32 C303 -119.4(4) . . . . ? O33 Yb3 N32 C303 36.4(5) . . . . ? O31 Yb3 N32 C303 -177.2(4) . . . . ? O31W Yb3 N32 C303 135.9(4) . . . . ? N31 Yb3 N32 C303 -105.9(4) . . . . ? N33 Yb3 N32 C303 12.1(4) . . . . ? N34 Yb3 N32 C303 -46.8(4) . . . . ? C314 Yb3 N32 C303 31.4(4) . . . . ? C312 Yb3 N32 C303 100.2(4) . . . . ? C316 Yb3 N32 C303 -88.1(4) . . . . ? O32 Yb3 N32 C302 -145.1(4) . . . . ? O34 Yb3 N32 C302 2.5(5) . . . . ? O33 Yb3 N32 C302 158.4(3) . . . . ? O31 Yb3 N32 C302 -55.2(4) . . . . ? O31W Yb3 N32 C302 -102.1(4) . . . . ? N31 Yb3 N32 C302 16.0(4) . . . . ? N33 Yb3 N32 C302 134.1(4) . . . . ? N34 Yb3 N32 C302 75.2(4) . . . . ? C314 Yb3 N32 C302 153.4(4) . . . . ? C312 Yb3 N32 C302 -137.9(4) . . . . ? C316 Yb3 N32 C302 33.8(5) . . . . ? O32 Yb3 N32 C311 -26.5(3) . . . . ? O34 Yb3 N32 C311 121.1(4) . . . . ? O33 Yb3 N32 C311 -83.0(4) . . . . ? O31 Yb3 N32 C311 63.4(3) . . . . ? O31W Yb3 N32 C311 16.5(4) . . . . ? N31 Yb3 N32 C311 134.7(4) . . . . ? N33 Yb3 N32 C311 -107.3(4) . . . . ? N34 Yb3 N32 C311 -166.2(3) . . . . ? C314 Yb3 N32 C311 -88.0(4) . . . . ? C312 Yb3 N32 C311 -19.3(3) . . . . ? C316 Yb3 N32 C311 152.4(3) . . . . ? O32 Yb3 N33 C313 64.0(3) . . . . ? O34 Yb3 N33 C313 -81.5(4) . . . . ? O33 Yb3 N33 C313 -24.6(3) . . . . ? O31 Yb3 N33 C313 122.0(4) . . . . ? O31W Yb3 N33 C313 15.9(4) . . . . ? N31 Yb3 N33 C313 -164.7(3) . . . . ? N32 Yb3 N33 C313 136.1(4) . . . . ? N34 Yb3 N33 C313 -105.9(4) . . . . ? C314 Yb3 N33 C313 -20.3(3) . . . . ? C312 Yb3 N33 C313 83.8(4) . . . . ? C316 Yb3 N33 C313 -85.3(4) . . . . ? O32 Yb3 N33 C304 -55.0(4) . . . . ? O34 Yb3 N33 C304 159.5(3) . . . . ? O33 Yb3 N33 C304 -143.7(4) . . . . ? O31 Yb3 N33 C304 3.0(5) . . . . ? O31W Yb3 N33 C304 -103.2(4) . . . . ? N31 Yb3 N33 C304 76.3(4) . . . . ? N32 Yb3 N33 C304 17.0(4) . . . . ? N34 Yb3 N33 C304 135.0(4) . . . . ? C314 Yb3 N33 C304 -139.3(4) . . . . ? C312 Yb3 N33 C304 -35.2(4) . . . . ? C316 Yb3 N33 C304 155.7(4) . . . . ? O32 Yb3 N33 C305 -176.3(4) . . . . ? O34 Yb3 N33 C305 38.1(4) . . . . ? O33 Yb3 N33 C305 95.0(4) . . . . ? O31 Yb3 N33 C305 -118.4(4) . . . . ? O31W Yb3 N33 C305 135.5(3) . . . . ? N31 Yb3 N33 C305 -45.0(4) . . . . ? N32 Yb3 N33 C305 -104.3(4) . . . . ? N34 Yb3 N33 C305 13.7(3) . . . . ? C314 Yb3 N33 C305 99.4(4) . . . . ? C312 Yb3 N33 C305 -156.5(4) . . . . ? C316 Yb3 N33 C305 34.4(4) . . . . ? O32 Yb3 N34 C315 119.0(4) . . . . ? O34 Yb3 N34 C315 -25.9(3) . . . . ? O33 Yb3 N34 C315 63.1(3) . . . . ? O31 Yb3 N34 C315 -85.2(4) . . . . ? O31W Yb3 N34 C315 10.3(4) . . . . ? N31 Yb3 N34 C315 -107.3(4) . . . . ? N33 Yb3 N34 C315 134.6(4) . . . . ? N32 Yb3 N34 C315 -167.0(3) . . . . ? C314 Yb3 N34 C315 82.8(4) . . . . ? C312 Yb3 N34 C315 150.2(3) . . . . ? C316 Yb3 N34 C315 -19.8(3) . . . . ? O32 Yb3 N34 C306 -0.6(5) . . . . ? O34 Yb3 N34 C306 -145.6(4) . . . . ? O33 Yb3 N34 C306 -56.6(4) . . . . ? O31 Yb3 N34 C306 155.1(3) . . . . ? O31W Yb3 N34 C306 -109.4(4) . . . . ? N31 Yb3 N34 C306 133.0(4) . . . . ? N33 Yb3 N34 C306 15.0(4) . . . . ? N32 Yb3 N34 C306 73.3(4) . . . . ? C314 Yb3 N34 C306 -36.9(4) . . . . ? C312 Yb3 N34 C306 30.5(5) . . . . ? C316 Yb3 N34 C306 -139.5(5) . . . . ? O32 Yb3 N34 C307 -121.3(4) . . . . ? O34 Yb3 N34 C307 93.8(4) . . . . ? O33 Yb3 N34 C307 -177.2(4) . . . . ? O31 Yb3 N34 C307 34.5(4) . . . . ? O31W Yb3 N34 C307 130.0(3) . . . . ? N31 Yb3 N34 C307 12.4(3) . . . . ? N33 Yb3 N34 C307 -105.6(4) . . . . ? N32 Yb3 N34 C307 -47.3(4) . . . . ? C314 Yb3 N34 C307 -157.5(4) . . . . ? C312 Yb3 N34 C307 -90.1(4) . . . . ? C316 Yb3 N34 C307 99.9(4) . . . . ? C309 N31 C301 C302 75.3(6) . . . . ? C308 N31 C301 C302 -164.6(5) . . . . ? Yb3 N31 C301 C302 -42.2(6) . . . . ? C303 N32 C302 C301 79.8(6) . . . . ? C311 N32 C302 C301 -159.7(5) . . . . ? Yb3 N32 C302 C301 -43.9(5) . . . . ? N31 C301 C302 N32 60.0(6) . . . . ? C302 N32 C303 C304 -163.2(5) . . . . ? C311 N32 C303 C304 76.3(6) . . . . ? Yb3 N32 C303 C304 -40.4(6) . . . . ? C313 N33 C304 C303 -162.0(5) . . . . ? C305 N33 C304 C303 78.0(6) . . . . ? Yb3 N33 C304 C303 -44.7(6) . . . . ? N32 C303 C304 N33 58.2(7) . . . . ? C313 N33 C305 C306 75.3(6) . . . . ? C304 N33 C305 C306 -165.3(5) . . . . ? Yb3 N33 C305 C306 -42.0(5) . . . . ? C315 N34 C306 C305 -159.9(5) . . . . ? C307 N34 C306 C305 80.1(6) . . . . ? Yb3 N34 C306 C305 -42.5(6) . . . . ? N33 C305 C306 N34 58.5(6) . . . . ? C315 N34 C307 C308 77.0(6) . . . . ? C306 N34 C307 C308 -163.0(5) . . . . ? Yb3 N34 C307 C308 -40.5(6) . . . . ? C309 N31 C308 C307 -161.5(5) . . . . ? C301 N31 C308 C307 77.4(6) . . . . ? Yb3 N31 C308 C307 -43.9(6) . . . . ? N34 C307 C308 N31 58.0(7) . . . . ? C301 N31 C309 C310 -82.2(6) . . . . ? C308 N31 C309 C310 158.3(5) . . . . ? Yb3 N31 C309 C310 37.5(5) . . . . ? Yb3 O31 C310 N35 -178.2(4) . . . . ? Yb3 O31 C310 C309 3.2(8) . . . . ? C317 N35 C310 O31 -2.0(9) . . . . ? C317 N35 C310 C309 176.6(5) . . . . ? C317 N35 C310 Yb3 -4.9(16) . . . . ? N31 C309 C310 O31 -30.9(8) . . . . ? N31 C309 C310 N35 150.5(6) . . . . ? N31 C309 C310 Yb3 -28.9(4) . . . . ? O32 Yb3 C310 O31 -23.8(5) . . . . ? O34 Yb3 C310 O31 116.0(5) . . . . ? O33 Yb3 C310 O31 72.3(6) . . . . ? O31W Yb3 C310 O31 45.6(5) . . . . ? N31 Yb3 C310 O31 -162.9(5) . . . . ? N33 Yb3 C310 O31 -102.3(5) . . . . ? N32 Yb3 C310 O31 -86.3(5) . . . . ? N34 Yb3 C310 O31 173.2(4) . . . . ? C314 Yb3 C310 O31 47.2(11) . . . . ? C312 Yb3 C310 O31 -38.2(5) . . . . ? C316 Yb3 C310 O31 128.8(5) . . . . ? O32 Yb3 C310 N35 -19.6(12) . . . . ? O34 Yb3 C310 N35 120.2(12) . . . . ? O33 Yb3 C310 N35 76.5(13) . . . . ? O31 Yb3 C310 N35 4.2(10) . . . . ? O31W Yb3 C310 N35 49.7(12) . . . . ? N31 Yb3 C310 N35 -158.7(13) . . . . ? N33 Yb3 C310 N35 -98.1(12) . . . . ? N32 Yb3 C310 N35 -82.1(12) . . . . ? N34 Yb3 C310 N35 177.4(12) . . . . ? C314 Yb3 C310 N35 51.4(17) . . . . ? C312 Yb3 C310 N35 -34.1(12) . . . . ? C316 Yb3 C310 N35 133.0(12) . . . . ? O32 Yb3 C310 C309 159.0(3) . . . . ? O34 Yb3 C310 C309 -61.1(3) . . . . ? O33 Yb3 C310 C309 -104.9(4) . . . . ? O31 Yb3 C310 C309 -177.2(7) . . . . ? O31W Yb3 C310 C309 -131.6(4) . . . . ? N31 Yb3 C310 C309 19.9(3) . . . . ? N33 Yb3 C310 C309 80.6(4) . . . . ? N32 Yb3 C310 C309 96.6(4) . . . . ? N34 Yb3 C310 C309 -4.0(4) . . . . ? C314 Yb3 C310 C309 -129.9(8) . . . . ? C312 Yb3 C310 C309 144.6(3) . . . . ? C316 Yb3 C310 C309 -48.3(3) . . . . ? C303 N32 C311 C312 -86.3(6) . . . . ? C302 N32 C311 C312 153.6(5) . . . . ? Yb3 N32 C311 C312 34.5(5) . . . . ? Yb3 O32 C312 N36 175.6(4) . . . . ? Yb3 O32 C312 C311 -2.7(8) . . . . ? C325 N36 C312 O32 -2.9(9) . . . . ? C325 N36 C312 C311 175.4(5) . . . . ? C325 N36 C312 Yb3 4.0(15) . . . . ? N32 C311 C312 O32 -25.5(8) . . . . ? N32 C311 C312 N36 156.2(5) . . . . ? N32 C311 C312 Yb3 -27.1(4) . . . . ? O34 Yb3 C312 O32 72.5(6) . . . . ? O33 Yb3 C312 O32 -21.8(5) . . . . ? O31 Yb3 C312 O32 119.2(5) . . . . ? O31W Yb3 C312 O32 49.0(5) . . . . ? N31 Yb3 C312 O32 174.0(4) . . . . ? N33 Yb3 C312 O32 -85.0(5) . . . . ? N32 Yb3 C312 O32 -159.1(5) . . . . ? N34 Yb3 C312 O32 -100.0(5) . . . . ? C314 Yb3 C312 O32 -37.9(5) . . . . ? C316 Yb3 C312 O32 44.3(10) . . . . ? O32 Yb3 C312 N36 -10.0(10) . . . . ? O34 Yb3 C312 N36 62.5(13) . . . . ? O33 Yb3 C312 N36 -31.8(12) . . . . ? O31 Yb3 C312 N36 109.2(12) . . . . ? O31W Yb3 C312 N36 39.0(12) . . . . ? N31 Yb3 C312 N36 164.0(11) . . . . ? N33 Yb3 C312 N36 -95.0(12) . . . . ? N32 Yb3 C312 N36 -169.1(12) . . . . ? N34 Yb3 C312 N36 -110.0(11) . . . . ? C314 Yb3 C312 N36 -47.9(12) . . . . ? C316 Yb3 C312 N36 34.3(16) . . . . ? O32 Yb3 C312 C311 177.6(7) . . . . ? O34 Yb3 C312 C311 -109.8(4) . . . . ? O33 Yb3 C312 C311 155.8(3) . . . . ? O31 Yb3 C312 C311 -63.2(3) . . . . ? O31W Yb3 C312 C311 -133.3(3) . . . . ? N31 Yb3 C312 C311 -8.3(4) . . . . ? N33 Yb3 C312 C311 92.7(3) . . . . ? N32 Yb3 C312 C311 18.5(3) . . . . ? N34 Yb3 C312 C311 77.7(4) . . . . ? C314 Yb3 C312 C311 139.7(3) . . . . ? C316 Yb3 C312 C311 -138.1(6) . . . . ? C304 N33 C313 C314 156.4(5) . . . . ? C305 N33 C313 C314 -84.6(6) . . . . ? Yb3 N33 C313 C314 35.6(5) . . . . ? Yb3 O33 C314 N37 -174.4(4) . . . . ? Yb3 O33 C314 C313 7.9(8) . . . . ? C333 N37 C314 O33 -0.4(9) . . . . ? C333 N37 C314 C313 177.4(5) . . . . ? C333 N37 C314 Yb3 -10.4(16) . . . . ? N33 C313 C314 O33 -32.6(8) . . . . ? N33 C313 C314 N37 149.5(5) . . . . ? N33 C313 C314 Yb3 -27.8(4) . . . . ? O32 Yb3 C314 O33 111.2(5) . . . . ? O34 Yb3 C314 O33 -29.0(5) . . . . ? O31 Yb3 C314 O33 69.5(6) . . . . ? O31W Yb3 C314 O33 39.5(5) . . . . ? N31 Yb3 C314 O33 -106.0(5) . . . . ? N33 Yb3 C314 O33 -167.6(6) . . . . ? N32 Yb3 C314 O33 168.5(5) . . . . ? N34 Yb3 C314 O33 -91.2(5) . . . . ? C312 Yb3 C314 O33 123.2(5) . . . . ? C316 Yb3 C314 O33 -44.0(5) . . . . ? O32 Yb3 C314 N37 125.0(13) . . . . ? O34 Yb3 C314 N37 -15.1(13) . . . . ? O33 Yb3 C314 N37 13.9(11) . . . . ? O31 Yb3 C314 N37 83.4(13) . . . . ? O31W Yb3 C314 N37 53.3(13) . . . . ? N31 Yb3 C314 N37 -92.2(13) . . . . ? N33 Yb3 C314 N37 -153.8(14) . . . . ? N32 Yb3 C314 N37 -177.7(13) . . . . ? N34 Yb3 C314 N37 -77.4(13) . . . . ? C312 Yb3 C314 N37 137.0(13) . . . . ? C316 Yb3 C314 N37 -30.1(13) . . . . ? O32 Yb3 C314 C313 -62.0(3) . . . . ? O34 Yb3 C314 C313 157.9(3) . . . . ? O33 Yb3 C314 C313 -173.2(7) . . . . ? O31 Yb3 C314 C313 -103.6(4) . . . . ? O31W Yb3 C314 C313 -133.7(4) . . . . ? N31 Yb3 C314 C313 80.8(4) . . . . ? N33 Yb3 C314 C313 19.2(3) . . . . ? N32 Yb3 C314 C313 -4.7(4) . . . . ? N34 Yb3 C314 C313 95.6(4) . . . . ? C312 Yb3 C314 C313 -50.0(4) . . . . ? C316 Yb3 C314 C313 142.8(4) . . . . ? C306 N34 C315 C316 155.7(5) . . . . ? C307 N34 C315 C316 -85.5(6) . . . . ? Yb3 N34 C315 C316 35.2(5) . . . . ? Yb3 O34 C316 N38 178.7(4) . . . . ? Yb3 O34 C316 C315 1.8(8) . . . . ? C341 N38 C316 O34 -1.8(9) . . . . ? C341 N38 C316 C315 175.1(5) . . . . ? C341 N38 C316 Yb3 0.2(15) . . . . ? N34 C315 C316 O34 -28.6(8) . . . . ? N34 C315 C316 N38 154.3(5) . . . . ? N34 C315 C316 Yb3 -27.6(4) . . . . ? O32 Yb3 C316 O34 73.1(6) . . . . ? O33 Yb3 C316 O34 114.6(5) . . . . ? O31 Yb3 C316 O34 -26.0(5) . . . . ? O31W Yb3 C316 O34 41.0(5) . . . . ? N31 Yb3 C316 O34 -87.6(5) . . . . ? N33 Yb3 C316 O34 171.4(5) . . . . ? N32 Yb3 C316 O34 -104.8(5) . . . . ? N34 Yb3 C316 O34 -162.7(6) . . . . ? C314 Yb3 C316 O34 128.2(5) . . . . ? C312 Yb3 C316 O34 45.7(10) . . . . ? O32 Yb3 C316 N38 70.3(12) . . . . ? O34 Yb3 C316 N38 -2.9(10) . . . . ? O33 Yb3 C316 N38 111.7(12) . . . . ? O31 Yb3 C316 N38 -28.9(12) . . . . ? O31W Yb3 C316 N38 38.1(12) . . . . ? N31 Yb3 C316 N38 -90.5(12) . . . . ? N33 Yb3 C316 N38 168.5(11) . . . . ? N32 Yb3 C316 N38 -107.7(11) . . . . ? N34 Yb3 C316 N38 -165.5(12) . . . . ? C314 Yb3 C316 N38 125.3(12) . . . . ? C312 Yb3 C316 N38 42.8(16) . . . . ? O32 Yb3 C316 C315 -105.3(4) . . . . ? O34 Yb3 C316 C315 -178.4(7) . . . . ? O33 Yb3 C316 C315 -63.9(4) . . . . ? O31 Yb3 C316 C315 155.5(3) . . . . ? O31W Yb3 C316 C315 -137.5(4) . . . . ? N31 Yb3 C316 C315 94.0(4) . . . . ? N33 Yb3 C316 C315 -7.1(4) . . . . ? N32 Yb3 C316 C315 76.7(4) . . . . ? N34 Yb3 C316 C315 18.9(3) . . . . ? C314 Yb3 C316 C315 -50.3(4) . . . . ? C312 Yb3 C316 C315 -132.7(7) . . . . ? C310 N35 C317 C324 -157.2(6) . . . . ? C310 N35 C317 C318 78.5(7) . . . . ? N35 C317 C318 C319 -136.8(6) . . . . ? C324 C317 C318 C319 100.5(7) . . . . ? N35 C317 C318 C323 44.4(8) . . . . ? C324 C317 C318 C323 -78.3(8) . . . . ? C323 C318 C319 C320 0.4(10) . . . . ? C317 C318 C319 C320 -178.4(6) . . . . ? C318 C319 C320 C321 0.0(11) . . . . ? C319 C320 C321 C322 -0.1(12) . . . . ? C320 C321 C322 C323 -0.3(12) . . . . ? C321 C322 C323 C318 0.8(11) . . . . ? C319 C318 C323 C322 -0.8(10) . . . . ? C317 C318 C323 C322 178.0(6) . . . . ? C312 N36 C325 C326 70.1(7) . . . . ? C312 N36 C325 C332 -166.0(6) . . . . ? N36 C325 C326 C331 -130.2(6) . . . . ? C332 C325 C326 C331 108.1(6) . . . . ? N36 C325 C326 C327 50.2(7) . . . . ? C332 C325 C326 C327 -71.5(7) . . . . ? C331 C326 C327 C328 0.8(9) . . . . ? C325 C326 C327 C328 -179.5(6) . . . . ? C326 C327 C328 C329 -0.7(9) . . . . ? C327 C328 C329 C330 -0.2(9) . . . . ? C328 C329 C330 C331 1.0(10) . . . . ? C329 C330 C331 C326 -0.9(10) . . . . ? C327 C326 C331 C330 0.0(9) . . . . ? C325 C326 C331 C330 -179.7(6) . . . . ? C314 N37 C333 C334 80.1(7) . . . . ? C314 N37 C333 C340 -156.7(6) . . . . ? N37 C333 C334 C335 49.0(8) . . . . ? C340 C333 C334 C335 -72.0(8) . . . . ? N37 C333 C334 C339 -130.7(6) . . . . ? C340 C333 C334 C339 108.3(7) . . . . ? C339 C334 C335 C336 -1.8(10) . . . . ? C333 C334 C335 C336 178.5(6) . . . . ? C334 C335 C336 C337 2.1(11) . . . . ? C335 C336 C337 C338 -2.0(12) . . . . ? C336 C337 C338 C339 1.6(12) . . . . ? C335 C334 C339 C338 1.3(10) . . . . ? C333 C334 C339 C338 -179.0(6) . . . . ? C337 C338 C339 C334 -1.2(12) . . . . ? C316 N38 C341 C342 74.3(7) . . . . ? C316 N38 C341 C348 -162.1(6) . . . . ? N38 C341 C342 C347 49.2(8) . . . . ? C348 C341 C342 C347 -72.6(8) . . . . ? N38 C341 C342 C343 -130.3(6) . . . . ? C348 C341 C342 C343 108.0(7) . . . . ? C347 C342 C343 C344 -1.5(10) . . . . ? C341 C342 C343 C344 178.0(6) . . . . ? C342 C343 C344 C345 0.9(11) . . . . ? C343 C344 C345 C346 0.9(11) . . . . ? C344 C345 C346 C347 -2.2(11) . . . . ? C345 C346 C347 C342 1.6(10) . . . . ? C343 C342 C347 C346 0.2(10) . . . . ? C341 C342 C347 C346 -179.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.942 _refine_diff_density_min -2.851 _refine_diff_density_rms 0.144 #============================================================================== data_[Yb.2]Br3 _database_code_depnum_ccdc_archive 'CCDC 606221' #============================================================================== _chemical_name_systematic ; [Yb.DOTAPh]Br~3~.7H~2~O ; _chemical_name_common (Yb.DOTAPh)Br!3$.7H!2$O _chemical_melting_point 'not measured' _chemical_formula_moiety 'C48 H64 N8 O5 Yb, 7(H2 O), 3Br' _chemical_formula_sum 'C48 H78 Br3 N8 O12 Yb' _chemical_formula_weight 1371.95 _chemical_absolute_configuration syn 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' Br Br -0.2901 2.4595 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.9399(11) _cell_length_b 22.6800(18) _cell_length_c 18.0276(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.699(1) _cell_angle_gamma 90.00 _cell_volume 5687.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9937 _cell_measurement_theta_min 3.174 _cell_measurement_theta_max 26.563 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2716 _exptl_absorpt_coefficient_mu 3.814 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1850 _exptl_absorpt_correction_T_max 0.5176 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.2000 -1.00 0.00 0.00 0.2000 0.00 1.00 0.00 0.1600 0.00 -1.00 0.00 0.1600 1.00 0.00 -1.00 0.1000 -1.00 0.00 1.00 0.1000 0.00 1.00 -1.00 0.1800 0.00 -1.00 1.00 0.1800 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 42251 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.65 _reflns_number_total 21040 _reflns_number_gt 17292 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+12.9358P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(8) _refine_ls_number_reflns 21040 _refine_ls_number_parameters 1297 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.00974(2) 1.004501(14) -0.00079(3) 0.01380(10) Uani 1 1 d . . . O11 O -0.0339(3) 0.9662(2) -0.1151(3) 0.0181(11) Uani 1 1 d . . . O12 O -0.1316(3) 0.9653(2) 0.0307(3) 0.0189(11) Uani 1 1 d . . . O13 O 0.0564(3) 0.9759(2) 0.1159(3) 0.0187(11) Uani 1 1 d . . . O14 O 0.1610(3) 0.9758(2) -0.0287(3) 0.0215(11) Uani 1 1 d . . . N11 N 0.0567(4) 1.0724(3) -0.1093(3) 0.0181(13) Uani 1 1 d . . . N12 N -0.1364(4) 1.0675(3) -0.0516(3) 0.0167(12) Uani 1 1 d . . . N13 N -0.0498(4) 1.0764(2) 0.1030(3) 0.0165(12) Uani 1 1 d . . . N14 N 0.1428(4) 1.0795(3) 0.0452(3) 0.0181(13) Uani 1 1 d . . . N15 N -0.0310(4) 0.9610(3) -0.2407(4) 0.0217(14) Uani 1 1 d . . . H15A H -0.0109 0.9771 -0.2814 0.026 Uiso 1 1 calc R . . N16 N -0.2942(4) 0.9637(3) 0.0302(4) 0.0219(14) Uani 1 1 d . . . H16A H -0.3495 0.9773 0.0109 0.026 Uiso 1 1 calc R . . N17 N 0.0512(4) 0.9720(3) 0.2411(4) 0.0246(15) Uani 1 1 d . . . H17A H 0.0309 0.9879 0.2817 0.030 Uiso 1 1 calc R . . N18 N 0.3231(4) 0.9794(3) -0.0200(4) 0.0227(14) Uani 1 1 d . . . H18A H 0.3755 0.9957 0.0008 0.027 Uiso 1 1 calc R . . C101 C -0.0181(5) 1.1174(3) -0.1264(5) 0.0241(17) Uani 1 1 d . . . H10A H -0.0089 1.1343 -0.1761 0.029 Uiso 1 1 calc R . . H10B H -0.0102 1.1497 -0.0896 0.029 Uiso 1 1 calc R . . C102 C -0.1194(5) 1.0933(3) -0.1255(4) 0.0238(17) Uani 1 1 d . . . H10C H -0.1661 1.1254 -0.1369 0.029 Uiso 1 1 calc R . . H10D H -0.1293 1.0626 -0.1643 0.029 Uiso 1 1 calc R . . C103 C -0.1575(6) 1.1161(3) 0.0005(4) 0.0235(17) Uani 1 1 d . . . H10E H -0.2239 1.1303 -0.0114 0.028 Uiso 1 1 calc R . . H10F H -0.1133 1.1493 -0.0073 0.028 Uiso 1 1 calc R . . C104 C -0.1476(5) 1.0984(3) 0.0815(4) 0.0211(16) Uani 1 1 d . . . H10G H -0.1618 1.1328 0.1128 0.025 Uiso 1 1 calc R . . H10H H -0.1951 1.0672 0.0907 0.025 Uiso 1 1 calc R . . C105 C 0.0174(6) 1.1280(3) 0.1138(5) 0.0248(17) Uani 1 1 d . . . H10I H 0.0052 1.1481 0.1610 0.030 Uiso 1 1 calc R . . H10J H 0.0043 1.1566 0.0728 0.030 Uiso 1 1 calc R . . C106 C 0.1215(5) 1.1094(3) 0.1155(4) 0.0226(16) Uani 1 1 d . . . H10K H 0.1632 1.1445 0.1228 0.027 Uiso 1 1 calc R . . H10L H 0.1357 1.0823 0.1578 0.027 Uiso 1 1 calc R . . C107 C 0.1563(6) 1.1261(3) -0.0130(4) 0.0228(17) Uani 1 1 d . . . H10M H 0.1064 1.1568 -0.0090 0.027 Uiso 1 1 calc R . . H10N H 0.2197 1.1450 -0.0026 0.027 Uiso 1 1 calc R . . C108 C 0.1507(5) 1.1028(3) -0.0908(4) 0.0205(16) Uani 1 1 d . . . H10O H 0.2040 1.0746 -0.0966 0.025 Uiso 1 1 calc R . . H10P H 0.1581 1.1357 -0.1260 0.025 Uiso 1 1 calc R . . C109 C 0.0671(6) 1.0342(3) -0.1741(4) 0.0209(16) Uani 1 1 d . . . H10Q H 0.1331 1.0180 -0.1725 0.025 Uiso 1 1 calc R . . H10R H 0.0566 1.0577 -0.2202 0.025 Uiso 1 1 calc R . . C110 C -0.0041(5) 0.9847(3) -0.1747(4) 0.0170(15) Uani 1 1 d . . . C111 C -0.2200(5) 1.0260(3) -0.0585(4) 0.0195(16) Uani 1 1 d . . . H11A H -0.2809 1.0484 -0.0583 0.023 Uiso 1 1 calc R . . H11B H -0.2196 1.0041 -0.1060 0.023 Uiso 1 1 calc R . . C112 C -0.2136(5) 0.9838(3) 0.0047(4) 0.0183(15) Uani 1 1 d . . . C113 C -0.0499(5) 1.0427(3) 0.1720(4) 0.0214(16) Uani 1 1 d . . . H11C H -0.1144 1.0252 0.1764 0.026 Uiso 1 1 calc R . . H11D H -0.0370 1.0697 0.2147 0.026 Uiso 1 1 calc R . . C114 C 0.0240(5) 0.9944(3) 0.1756(4) 0.0191(16) Uani 1 1 d . . . C115 C 0.2335(5) 1.0449(3) 0.0573(4) 0.0213(17) Uani 1 1 d . . . H11E H 0.2361 1.0263 0.1071 0.026 Uiso 1 1 calc R . . H11F H 0.2896 1.0714 0.0551 0.026 Uiso 1 1 calc R . . C116 C 0.2373(5) 0.9981(3) -0.0012(4) 0.0193(16) Uani 1 1 d . . . C117 C -0.0935(6) 0.9086(3) -0.2470(4) 0.0231(17) Uani 1 1 d . . . H11G H -0.0690 0.8793 -0.2089 0.028 Uiso 1 1 calc R . . C118 C -0.1961(5) 0.9244(3) -0.2308(4) 0.0226(17) Uani 1 1 d . . . C119 C -0.2445(6) 0.9709(3) -0.2664(4) 0.0266(18) Uani 1 1 d . . . H11H H -0.2114 0.9952 -0.2993 0.032 Uiso 1 1 calc R . . C120 C -0.3390(6) 0.9827(4) -0.2551(5) 0.0305(19) Uani 1 1 d . . . H12A H -0.3705 1.0146 -0.2806 0.037 Uiso 1 1 calc R . . C121 C -0.3897(6) 0.9480(4) -0.2060(5) 0.033(2) Uani 1 1 d . . . H12B H -0.4552 0.9561 -0.1984 0.039 Uiso 1 1 calc R . . C122 C -0.3420(6) 0.9015(3) -0.1689(5) 0.0308(19) Uani 1 1 d . . . H12C H -0.3753 0.8777 -0.1356 0.037 Uiso 1 1 calc R . . C123 C -0.2481(6) 0.8899(3) -0.1800(5) 0.0272(18) Uani 1 1 d . . . H12D H -0.2164 0.8584 -0.1536 0.033 Uiso 1 1 calc R . . C124 C -0.0885(6) 0.8811(4) -0.3219(5) 0.031(2) Uani 1 1 d . . . H12E H -0.0216 0.8710 -0.3300 0.046 Uiso 1 1 calc R . . H12F H -0.1126 0.9091 -0.3601 0.046 Uiso 1 1 calc R . . H12G H -0.1279 0.8453 -0.3247 0.046 Uiso 1 1 calc R . . C125 C -0.2945(5) 0.9195(3) 0.0898(4) 0.0221(16) Uani 1 1 d . . . H12H H -0.2431 0.8898 0.0819 0.026 Uiso 1 1 calc R . . C126 C -0.2739(6) 0.9480(3) 0.1655(5) 0.0262(17) Uani 1 1 d . . . C127 C -0.3269(6) 0.9958(3) 0.1874(5) 0.0296(19) Uani 1 1 d . . . H12I H -0.3747 1.0129 0.1542 0.035 Uiso 1 1 calc R . . C128 C -0.3092(6) 1.0188(4) 0.2598(5) 0.037(2) Uani 1 1 d . . . H12J H -0.3434 1.0526 0.2747 0.045 Uiso 1 1 calc R . . C129 C -0.2444(7) 0.9933(4) 0.3076(5) 0.037(2) Uani 1 1 d . . . H12K H -0.2361 1.0081 0.3569 0.045 Uiso 1 1 calc R . . C130 C -0.1891(7) 0.9457(4) 0.2870(5) 0.040(2) Uani 1 1 d . . . H13A H -0.1421 0.9287 0.3210 0.048 Uiso 1 1 calc R . . C131 C -0.2045(6) 0.9237(4) 0.2149(5) 0.0309(19) Uani 1 1 d . . . H13B H -0.1668 0.8915 0.1994 0.037 Uiso 1 1 calc R . . C132 C -0.3910(6) 0.8883(4) 0.0845(5) 0.038(2) Uani 1 1 d . . . H13C H -0.4016 0.8702 0.0353 0.057 Uiso 1 1 calc R . . H13D H -0.4422 0.9170 0.0919 0.057 Uiso 1 1 calc R . . H13E H -0.3917 0.8577 0.1229 0.057 Uiso 1 1 calc R . . C133 C 0.1155(6) 0.9204(3) 0.2464(4) 0.0247(17) Uani 1 1 d . . . H13F H 0.0933 0.8925 0.2060 0.030 Uiso 1 1 calc R . . C134 C 0.2176(6) 0.9367(3) 0.2338(4) 0.0235(17) Uani 1 1 d . . . C135 C 0.2647(6) 0.9804(4) 0.2745(5) 0.0285(18) Uani 1 1 d . . . H13G H 0.2317 1.0013 0.3107 0.034 Uiso 1 1 calc R . . C136 C 0.3593(6) 0.9945(4) 0.2637(5) 0.034(2) Uani 1 1 d . . . H13H H 0.3905 1.0252 0.2917 0.041 Uiso 1 1 calc R . . C137 C 0.4081(6) 0.9635(4) 0.2116(5) 0.038(2) Uani 1 1 d . . . H13I H 0.4730 0.9730 0.2038 0.045 Uiso 1 1 calc R . . C138 C 0.3625(7) 0.9187(4) 0.1711(5) 0.039(2) Uani 1 1 d . . . H13J H 0.3969 0.8971 0.1363 0.047 Uiso 1 1 calc R . . C139 C 0.2689(6) 0.9053(4) 0.1802(5) 0.0313(19) Uani 1 1 d . . . H13K H 0.2378 0.8751 0.1510 0.038 Uiso 1 1 calc R . . C140 C 0.1054(6) 0.8893(4) 0.3194(5) 0.033(2) Uani 1 1 d . . . H14A H 0.0376 0.8798 0.3247 0.050 Uiso 1 1 calc R . . H14B H 0.1289 0.9150 0.3603 0.050 Uiso 1 1 calc R . . H14C H 0.1432 0.8528 0.3206 0.050 Uiso 1 1 calc R . . C141 C 0.3314(5) 0.9326(3) -0.0742(5) 0.0271(18) Uani 1 1 d . . . H14D H 0.2796 0.9031 -0.0668 0.033 Uiso 1 1 calc R . . C142 C 0.3179(5) 0.9558(3) -0.1528(5) 0.0257(17) Uani 1 1 d . . . C143 C 0.3706(5) 1.0038(4) -0.1748(5) 0.0303(19) Uani 1 1 d . . . H14E H 0.4127 1.0238 -0.1397 0.036 Uiso 1 1 calc R . . C144 C 0.3617(8) 1.0230(4) -0.2494(5) 0.047(3) Uani 1 1 d . . . H14F H 0.3999 1.0547 -0.2654 0.057 Uiso 1 1 calc R . . C145 C 0.2970(7) 0.9952(4) -0.2989(5) 0.039(2) Uani 1 1 d . . . H14G H 0.2884 1.0093 -0.3485 0.047 Uiso 1 1 calc R . . C146 C 0.2465(8) 0.9490(5) -0.2779(6) 0.051(3) Uani 1 1 d . . . H14H H 0.2035 0.9298 -0.3132 0.061 Uiso 1 1 calc R . . C147 C 0.2557(6) 0.9281(4) -0.2046(5) 0.036(2) Uani 1 1 d . . . H14I H 0.2193 0.8950 -0.1906 0.043 Uiso 1 1 calc R . . C148 C 0.4275(6) 0.9022(4) -0.0594(5) 0.0305(19) Uani 1 1 d . . . H14J H 0.4330 0.8875 -0.0082 0.046 Uiso 1 1 calc R . . H14K H 0.4795 0.9304 -0.0666 0.046 Uiso 1 1 calc R . . H14L H 0.4324 0.8691 -0.0939 0.046 Uiso 1 1 calc R . . Yb2 Yb 0.50345(5) 0.756960(13) -0.504947(16) 0.01213(10) Uani 1 1 d . . . O21 O 0.5504(3) 0.7282(2) -0.3879(3) 0.0211(11) Uani 1 1 d . . . O22 O 0.6527(3) 0.7249(2) -0.5316(3) 0.0150(10) Uani 1 1 d . . . O23 O 0.4583(3) 0.7184(2) -0.6196(3) 0.0186(11) Uani 1 1 d . . . O24 O 0.3592(3) 0.7207(2) -0.4717(3) 0.0154(10) Uani 1 1 d . . . N21 N 0.4477(4) 0.8303(2) -0.4017(3) 0.0164(12) Uani 1 1 d . . . N22 N 0.6422(4) 0.8305(3) -0.4610(3) 0.0178(13) Uani 1 1 d . . . N23 N 0.5539(4) 0.8238(2) -0.6145(3) 0.0166(12) Uani 1 1 d . . . N24 N 0.3603(4) 0.8210(2) -0.5561(3) 0.0190(13) Uani 1 1 d . . . N25 N 0.5415(4) 0.7226(3) -0.2645(3) 0.0209(14) Uani 1 1 d . . . H25A H 0.5216 0.7384 -0.2237 0.025 Uiso 1 1 calc R . . N26 N 0.8127(4) 0.7249(3) -0.5223(4) 0.0209(14) Uani 1 1 d . . . H26A H 0.8660 0.7404 -0.5019 0.025 Uiso 1 1 calc R . . N27 N 0.4585(4) 0.7135(3) -0.7439(3) 0.0199(13) Uani 1 1 d . . . H27A H 0.4771 0.7292 -0.7853 0.024 Uiso 1 1 calc R . . N28 N 0.1986(4) 0.7205(3) -0.4750(4) 0.0207(14) Uani 1 1 d . . . H28A H 0.1445 0.7345 -0.4957 0.025 Uiso 1 1 calc R . . C201 C 0.5161(5) 0.8800(3) -0.3912(4) 0.0205(16) Uani 1 1 d . . . H20A H 0.5050 0.9003 -0.3439 0.025 Uiso 1 1 calc R . . H20B H 0.5040 0.9088 -0.4321 0.025 Uiso 1 1 calc R . . C202 C 0.6203(5) 0.8597(3) -0.3898(4) 0.0233(17) Uani 1 1 d . . . H20C H 0.6632 0.8942 -0.3813 0.028 Uiso 1 1 calc R . . H20D H 0.6331 0.8318 -0.3482 0.028 Uiso 1 1 calc R . . C203 C 0.6559(6) 0.8767(3) -0.5173(4) 0.0241(17) Uani 1 1 d . . . H20E H 0.7196 0.8953 -0.5070 0.029 Uiso 1 1 calc R . . H20F H 0.6063 0.9075 -0.5131 0.029 Uiso 1 1 calc R . . C204 C 0.6495(5) 0.8523(3) -0.5962(4) 0.0195(16) Uani 1 1 d . . . H20G H 0.6591 0.8847 -0.6318 0.023 Uiso 1 1 calc R . . H20H H 0.7012 0.8229 -0.6013 0.023 Uiso 1 1 calc R . . C205 C 0.4806(5) 0.8700(3) -0.6312(4) 0.0202(16) Uani 1 1 d . . . H20I H 0.4899 0.8869 -0.6809 0.024 Uiso 1 1 calc R . . H20J H 0.4895 0.9021 -0.5942 0.024 Uiso 1 1 calc R . . C206 C 0.3778(5) 0.8456(3) -0.6299(4) 0.0203(16) Uani 1 1 d . . . H20K H 0.3311 0.8775 -0.6421 0.024 Uiso 1 1 calc R . . H20L H 0.3681 0.8144 -0.6680 0.024 Uiso 1 1 calc R . . C207 C 0.3410(5) 0.8706(3) -0.5058(4) 0.0187(15) Uani 1 1 d . . . H20M H 0.2754 0.8858 -0.5186 0.022 Uiso 1 1 calc R . . H20N H 0.3870 0.9028 -0.5141 0.022 Uiso 1 1 calc R . . C208 C 0.3493(5) 0.8535(3) -0.4239(4) 0.0190(16) Uani 1 1 d . . . H20O H 0.3360 0.8883 -0.3932 0.023 Uiso 1 1 calc R . . H20P H 0.3008 0.8229 -0.4146 0.023 Uiso 1 1 calc R . . C209 C 0.4446(5) 0.7962(3) -0.3316(4) 0.0206(16) Uani 1 1 d . . . H20Q H 0.3794 0.7796 -0.3278 0.025 Uiso 1 1 calc R . . H20R H 0.4582 0.8229 -0.2887 0.025 Uiso 1 1 calc R . . C210 C 0.5172(5) 0.7469(3) -0.3287(4) 0.0180(16) Uani 1 1 d . . . C211 C 0.7292(5) 0.7939(3) -0.4477(5) 0.0236(18) Uani 1 1 d . . . H21A H 0.7302 0.7765 -0.3973 0.028 Uiso 1 1 calc R . . H21B H 0.7871 0.8189 -0.4504 0.028 Uiso 1 1 calc R . . C212 C 0.7306(5) 0.7453(3) -0.5049(4) 0.0171(16) Uani 1 1 d . . . C213 C 0.5618(5) 0.7850(3) -0.6804(4) 0.0192(16) Uani 1 1 d . . . H21C H 0.6271 0.7677 -0.6794 0.023 Uiso 1 1 calc R . . H21D H 0.5517 0.8087 -0.7264 0.023 Uiso 1 1 calc R . . C214 C 0.4886(5) 0.7366(3) -0.6806(4) 0.0158(15) Uani 1 1 d . . . C215 C 0.2762(5) 0.7813(3) -0.5638(4) 0.0207(17) Uani 1 1 d . . . H21E H 0.2767 0.7594 -0.6113 0.025 Uiso 1 1 calc R . . H21F H 0.2163 0.8048 -0.5646 0.025 Uiso 1 1 calc R . . C216 C 0.2786(5) 0.7378(3) -0.4990(4) 0.0182(15) Uani 1 1 d . . . C217 C 0.6024(5) 0.6685(3) -0.2593(4) 0.0208(16) Uani 1 1 d . . . H21G H 0.5766 0.6397 -0.2976 0.025 Uiso 1 1 calc R . . C218 C 0.7057(5) 0.6821(3) -0.2743(4) 0.0205(16) Uani 1 1 d . . . C219 C 0.7569(6) 0.7261(3) -0.2353(5) 0.0278(18) Uani 1 1 d . . . H21H H 0.7262 0.7495 -0.2001 0.033 Uiso 1 1 calc R . . C220 C 0.8534(6) 0.7359(4) -0.2477(5) 0.0278(18) Uani 1 1 d . . . H22A H 0.8882 0.7660 -0.2211 0.033 Uiso 1 1 calc R . . C221 C 0.8979(6) 0.7023(4) -0.2982(5) 0.035(2) Uani 1 1 d . . . H22B H 0.9635 0.7094 -0.3065 0.042 Uiso 1 1 calc R . . C222 C 0.8486(6) 0.6578(4) -0.3375(5) 0.033(2) Uani 1 1 d . . . H22C H 0.8798 0.6343 -0.3723 0.040 Uiso 1 1 calc R . . C223 C 0.7506(6) 0.6484(3) -0.3246(5) 0.0263(18) Uani 1 1 d . . . H22D H 0.7157 0.6183 -0.3511 0.032 Uiso 1 1 calc R . . C224 C 0.5940(6) 0.6412(3) -0.1825(4) 0.0246(17) Uani 1 1 d . . . H22E H 0.5263 0.6331 -0.1749 0.037 Uiso 1 1 calc R . . H22F H 0.6198 0.6686 -0.1443 0.037 Uiso 1 1 calc R . . H22G H 0.6305 0.6042 -0.1792 0.037 Uiso 1 1 calc R . . C225 C 0.8187(5) 0.6756(3) -0.5764(4) 0.0226(16) Uani 1 1 d . . . H22H H 0.7696 0.6454 -0.5647 0.027 Uiso 1 1 calc R . . C226 C 0.7957(6) 0.6966(3) -0.6545(5) 0.0279(18) Uani 1 1 d . . . C227 C 0.8419(7) 0.7453(3) -0.6824(5) 0.032(2) Uani 1 1 d . . . H22I H 0.8872 0.7670 -0.6516 0.039 Uiso 1 1 calc R . . C228 C 0.8214(7) 0.7618(4) -0.7553(5) 0.038(2) Uani 1 1 d . . . H22J H 0.8524 0.7953 -0.7744 0.046 Uiso 1 1 calc R . . C229 C 0.7574(7) 0.7310(4) -0.8004(6) 0.042(2) Uani 1 1 d . . . H22K H 0.7454 0.7425 -0.8508 0.051 Uiso 1 1 calc R . . C230 C 0.7106(6) 0.6837(4) -0.7737(5) 0.035(2) Uani 1 1 d . . . H23A H 0.6646 0.6629 -0.8050 0.042 Uiso 1 1 calc R . . C231 C 0.7303(6) 0.6658(4) -0.7001(5) 0.0306(19) Uani 1 1 d . . . H23B H 0.6986 0.6323 -0.6815 0.037 Uiso 1 1 calc R . . C232 C 0.9173(5) 0.6470(4) -0.5657(5) 0.0288(19) Uani 1 1 d . . . H23C H 0.9281 0.6338 -0.5141 0.043 Uiso 1 1 calc R . . H23D H 0.9668 0.6758 -0.5769 0.043 Uiso 1 1 calc R . . H23E H 0.9206 0.6132 -0.5992 0.043 Uiso 1 1 calc R . . C233 C 0.3934(5) 0.6611(3) -0.7486(4) 0.0187(15) Uani 1 1 d . . . H23F H 0.4157 0.6322 -0.7093 0.022 Uiso 1 1 calc R . . C234 C 0.2910(5) 0.6790(3) -0.7358(4) 0.0213(17) Uani 1 1 d . . . C235 C 0.2469(6) 0.7259(4) -0.7752(5) 0.0304(19) Uani 1 1 d . . . H23G H 0.2816 0.7478 -0.8096 0.036 Uiso 1 1 calc R . . C236 C 0.1512(6) 0.7405(4) -0.7637(5) 0.034(2) Uani 1 1 d . . . H23H H 0.1203 0.7718 -0.7909 0.041 Uiso 1 1 calc R . . C237 C 0.1034(6) 0.7095(4) -0.7137(6) 0.039(2) Uani 1 1 d . . . H23I H 0.0393 0.7205 -0.7050 0.047 Uiso 1 1 calc R . . C238 C 0.1447(6) 0.6626(4) -0.6748(5) 0.034(2) Uani 1 1 d . . . H23J H 0.1093 0.6406 -0.6411 0.041 Uiso 1 1 calc R . . C239 C 0.2409(6) 0.6484(3) -0.6868(4) 0.0259(18) Uani 1 1 d . . . H23K H 0.2711 0.6167 -0.6599 0.031 Uiso 1 1 calc R . . C240 C 0.4016(5) 0.6326(3) -0.8247(4) 0.0213(16) Uani 1 1 d . . . H24A H 0.3594 0.5981 -0.8292 0.032 Uiso 1 1 calc R . . H24B H 0.4682 0.6203 -0.8299 0.032 Uiso 1 1 calc R . . H24C H 0.3825 0.6611 -0.8637 0.032 Uiso 1 1 calc R . . C241 C 0.1951(5) 0.6773(3) -0.4129(5) 0.0256(18) Uani 1 1 d . . . H24D H 0.2491 0.6486 -0.4164 0.031 Uiso 1 1 calc R . . C242 C 0.2070(6) 0.7083(4) -0.3384(5) 0.0294(19) Uani 1 1 d . . . C243 C 0.1511(6) 0.7553(4) -0.3213(5) 0.0318(19) Uani 1 1 d . . . H24E H 0.1066 0.7715 -0.3579 0.038 Uiso 1 1 calc R . . C244 C 0.1597(8) 0.7795(5) -0.2495(6) 0.049(3) Uani 1 1 d . . . H24F H 0.1224 0.8130 -0.2382 0.059 Uiso 1 1 calc R . . C245 C 0.2213(8) 0.7553(5) -0.1953(6) 0.053(3) Uani 1 1 d . . . H24G H 0.2237 0.7703 -0.1460 0.064 Uiso 1 1 calc R . . C246 C 0.2813(8) 0.7077(5) -0.2136(6) 0.050(3) Uani 1 1 d . . . H24H H 0.3275 0.6923 -0.1777 0.060 Uiso 1 1 calc R . . C247 C 0.2718(7) 0.6844(4) -0.2835(6) 0.044(2) Uani 1 1 d . . . H24I H 0.3097 0.6513 -0.2953 0.052 Uiso 1 1 calc R . . C248 C 0.1003(6) 0.6438(4) -0.4221(5) 0.032(2) Uani 1 1 d . . . H24J H 0.0952 0.6245 -0.4708 0.048 Uiso 1 1 calc R . . H24K H 0.0467 0.6714 -0.4185 0.048 Uiso 1 1 calc R . . H24L H 0.0981 0.6140 -0.3829 0.048 Uiso 1 1 calc R . . Br1 Br -0.26113(7) 0.77628(4) -0.02880(6) 0.0362(2) Uani 1 1 d . . . Br2 Br 0.24901(8) 0.79592(5) 0.02805(6) 0.0452(3) Uani 1 1 d . . . Br3 Br 0.47767(7) 0.56365(4) -0.01065(6) 0.0330(2) Uani 1 1 d . . . Br4 Br 0.23530(7) 0.53026(5) -0.53384(5) 0.0377(2) Uani 1 1 d . . . Br5 Br 0.74984(8) 0.53568(6) -0.47795(5) 0.0417(2) Uani 1 1 d . . . Br6 Br 0.99205(9) 0.31327(4) -0.49471(6) 0.0309(2) Uani 1 1 d . . . O1W O 0.0257(4) 0.8972(2) 0.0038(3) 0.0213(11) Uani 1 1 d . . . O2W O 0.5143(3) 0.6497(2) -0.4998(2) 0.0193(11) Uani 1 1 d . . . O3W O -0.0467(4) 0.8087(3) -0.0926(3) 0.0387(15) Uani 1 1 d . . . O4W O -0.0803(5) 0.8208(3) 0.0955(3) 0.0419(15) Uani 1 1 d . . . O5W O -0.4022(5) 0.6854(3) 0.0571(4) 0.0517(19) Uani 1 1 d . . . O6W O -0.4839(5) 0.7723(3) -0.1232(3) 0.0339(14) Uani 1 1 d . . . O7W O 0.0388(5) 0.7408(3) 0.0245(4) 0.0465(17) Uani 1 1 d . . . O8W O 0.3923(5) 0.7018(3) -0.0499(4) 0.0522(19) Uani 1 1 d . . . O9W O 0.4778(5) 0.7695(3) 0.1184(4) 0.0425(17) Uani 1 1 d . . . O10W O 0.4481(4) 0.5619(3) -0.5972(3) 0.0374(14) Uani 1 1 d . . . O11W O 0.4101(5) 0.5769(3) -0.4053(3) 0.0438(16) Uani 1 1 d . . . O12W O 0.0839(6) 0.4444(4) -0.4510(4) 0.059(2) Uani 1 1 d . . . O13W O 0.0080(5) 0.5175(3) -0.6255(4) 0.0460(18) Uani 1 1 d . . . O14W O 0.5269(5) 0.4949(2) -0.4752(4) 0.0416(16) Uani 1 1 d . . . O15W O 0.8828(5) 0.4390(4) -0.5632(4) 0.055(2) Uani 1 1 d . . . O16W O 0.9678(5) 0.5234(3) -0.3809(3) 0.0369(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01529(18) 0.0156(2) 0.01004(18) 0.00029(12) -0.00291(14) -0.00091(18) O11 0.025(3) 0.018(3) 0.011(3) 0.000(2) 0.001(2) -0.004(2) O12 0.023(3) 0.014(2) 0.019(3) 0.002(2) 0.003(2) 0.0022(19) O13 0.022(2) 0.026(3) 0.009(3) 0.000(2) 0.004(2) 0.007(2) O14 0.023(3) 0.021(3) 0.020(3) 0.000(2) -0.001(2) 0.000(2) N11 0.023(3) 0.017(3) 0.013(3) 0.002(2) -0.002(2) -0.003(2) N12 0.016(3) 0.018(3) 0.016(3) 0.003(3) -0.001(2) 0.007(2) N13 0.025(3) 0.015(3) 0.009(3) -0.003(2) 0.004(2) 0.002(2) N14 0.023(3) 0.020(3) 0.011(3) -0.003(2) -0.003(2) 0.003(2) N15 0.027(3) 0.020(3) 0.017(3) 0.001(3) -0.004(3) -0.006(3) N16 0.020(3) 0.025(3) 0.020(4) 0.001(3) -0.003(3) -0.001(3) N17 0.028(3) 0.029(4) 0.016(4) -0.001(3) -0.002(3) 0.009(3) N18 0.018(3) 0.027(3) 0.023(4) -0.001(3) 0.001(3) 0.002(3) C101 0.032(4) 0.018(4) 0.021(4) 0.009(3) -0.005(3) 0.004(3) C102 0.027(4) 0.024(4) 0.019(4) 0.003(3) -0.007(3) 0.003(3) C103 0.023(4) 0.023(4) 0.024(4) 0.002(3) 0.000(3) 0.007(3) C104 0.015(3) 0.024(4) 0.024(4) -0.006(3) 0.000(3) 0.001(3) C105 0.031(4) 0.019(4) 0.024(4) -0.008(3) 0.001(3) 0.000(3) C106 0.025(4) 0.022(4) 0.021(4) -0.005(3) -0.001(3) -0.005(3) C107 0.027(4) 0.019(4) 0.023(4) 0.000(3) 0.006(3) -0.003(3) C108 0.023(4) 0.019(4) 0.019(4) -0.003(3) 0.000(3) -0.008(3) C109 0.034(4) 0.020(4) 0.008(4) 0.002(3) 0.003(3) -0.004(3) C110 0.020(4) 0.018(4) 0.013(4) -0.003(3) -0.004(3) 0.006(3) C111 0.017(3) 0.024(4) 0.017(4) -0.001(3) -0.005(3) -0.001(3) C112 0.015(3) 0.020(4) 0.019(4) -0.004(3) -0.005(3) 0.002(3) C113 0.023(4) 0.029(4) 0.012(4) 0.003(3) 0.003(3) 0.005(3) C114 0.025(4) 0.019(4) 0.013(4) 0.008(3) 0.002(3) 0.000(3) C115 0.016(3) 0.033(4) 0.014(4) -0.005(3) -0.008(3) 0.000(3) C116 0.020(3) 0.018(4) 0.020(4) 0.001(3) 0.002(3) 0.001(3) C117 0.030(4) 0.020(4) 0.019(4) 0.004(3) -0.007(3) 0.000(3) C118 0.025(4) 0.028(4) 0.015(4) -0.003(3) -0.004(3) -0.002(3) C119 0.047(5) 0.020(4) 0.012(4) -0.003(3) -0.002(4) 0.002(3) C120 0.041(5) 0.025(4) 0.024(5) 0.001(3) -0.011(4) 0.006(4) C121 0.027(4) 0.042(5) 0.029(5) -0.009(4) 0.001(4) 0.007(4) C122 0.041(5) 0.023(4) 0.029(5) 0.003(3) 0.009(4) 0.001(4) C123 0.035(4) 0.019(4) 0.028(5) 0.007(3) 0.003(4) 0.004(3) C124 0.036(5) 0.025(4) 0.031(5) -0.008(4) -0.007(4) -0.004(3) C125 0.019(4) 0.022(4) 0.025(4) -0.001(3) 0.000(3) 0.003(3) C126 0.030(4) 0.025(4) 0.024(4) 0.001(3) 0.011(3) -0.003(3) C127 0.027(4) 0.020(4) 0.043(6) 0.000(4) 0.014(4) 0.003(3) C128 0.039(5) 0.035(5) 0.038(6) -0.017(4) 0.013(4) -0.003(4) C129 0.048(5) 0.043(6) 0.022(5) -0.002(4) 0.017(4) -0.010(4) C130 0.044(5) 0.045(5) 0.033(5) 0.006(4) 0.006(4) -0.005(4) C131 0.037(5) 0.025(4) 0.031(5) 0.004(4) 0.003(4) 0.001(3) C132 0.025(4) 0.038(5) 0.051(6) -0.007(4) 0.010(4) -0.013(4) C133 0.029(4) 0.023(4) 0.021(4) -0.001(3) -0.006(3) 0.010(3) C134 0.034(4) 0.024(4) 0.013(4) 0.006(3) 0.001(3) 0.010(3) C135 0.040(5) 0.025(4) 0.021(4) 0.005(3) -0.001(4) 0.005(3) C136 0.040(4) 0.027(5) 0.035(5) 0.011(4) 0.000(4) -0.001(4) C137 0.028(4) 0.049(6) 0.037(6) 0.025(4) 0.007(4) 0.004(4) C138 0.039(5) 0.051(6) 0.029(5) 0.010(4) 0.013(4) 0.010(4) C139 0.034(5) 0.035(5) 0.026(5) 0.003(4) 0.007(4) 0.008(4) C140 0.028(4) 0.040(5) 0.031(5) 0.016(4) 0.002(4) 0.010(4) C141 0.022(4) 0.026(4) 0.033(5) -0.005(3) 0.001(3) 0.004(3) C142 0.027(4) 0.023(4) 0.027(4) -0.004(3) 0.002(3) 0.017(3) C143 0.031(4) 0.039(5) 0.021(4) 0.002(4) -0.002(3) 0.015(4) C144 0.066(6) 0.045(6) 0.032(6) 0.015(5) 0.013(5) 0.021(5) C145 0.057(5) 0.043(6) 0.018(5) 0.006(4) -0.004(4) 0.022(5) C146 0.058(6) 0.060(7) 0.033(6) -0.028(5) -0.017(5) 0.021(6) C147 0.039(5) 0.043(5) 0.024(5) -0.010(4) -0.001(4) 0.006(4) C148 0.033(4) 0.031(4) 0.027(5) 0.007(4) 0.004(4) 0.013(3) Yb2 0.01038(16) 0.0151(2) 0.01065(17) -0.00049(14) -0.00130(13) -0.00039(11) O21 0.011(2) 0.028(3) 0.024(3) -0.004(2) -0.001(2) 0.004(2) O22 0.014(2) 0.026(3) 0.006(2) 0.000(2) 0.0087(18) -0.0040(19) O23 0.014(2) 0.022(3) 0.019(3) -0.002(2) -0.001(2) -0.0026(19) O24 0.017(2) 0.021(3) 0.009(2) 0.001(2) 0.0054(19) 0.0034(19) N21 0.025(3) 0.014(3) 0.011(3) -0.005(2) 0.004(2) 0.003(2) N22 0.022(3) 0.018(3) 0.013(3) 0.001(2) -0.001(2) 0.002(2) N23 0.022(3) 0.015(3) 0.013(3) 0.000(2) 0.001(2) -0.003(2) N24 0.021(3) 0.014(3) 0.021(3) 0.004(3) -0.004(2) -0.001(2) N25 0.029(3) 0.026(3) 0.008(3) 0.004(3) 0.002(3) 0.004(3) N26 0.015(3) 0.025(3) 0.023(4) 0.001(3) 0.001(3) -0.004(2) N27 0.027(3) 0.024(3) 0.009(3) -0.003(3) -0.001(3) -0.005(3) N28 0.010(3) 0.029(3) 0.024(4) -0.003(3) 0.003(3) 0.000(2) C201 0.022(4) 0.016(3) 0.023(4) -0.008(3) 0.000(3) 0.002(3) C202 0.027(4) 0.029(4) 0.013(4) -0.009(3) 0.002(3) -0.004(3) C203 0.030(4) 0.020(4) 0.022(4) -0.003(3) 0.002(3) -0.008(3) C204 0.017(3) 0.022(4) 0.020(4) -0.003(3) 0.000(3) -0.001(3) C205 0.019(4) 0.025(4) 0.016(4) 0.005(3) 0.001(3) 0.006(3) C206 0.022(4) 0.022(4) 0.017(4) 0.002(3) 0.001(3) -0.003(3) C207 0.026(4) 0.013(3) 0.016(4) 0.001(3) 0.000(3) 0.004(3) C208 0.016(3) 0.016(3) 0.026(4) 0.005(3) 0.003(3) 0.006(3) C209 0.025(4) 0.023(4) 0.014(4) 0.002(3) 0.003(3) 0.005(3) C210 0.020(4) 0.014(4) 0.020(4) -0.004(3) 0.000(3) 0.003(3) C211 0.010(3) 0.027(4) 0.033(5) -0.003(3) -0.005(3) -0.003(3) C212 0.009(3) 0.026(4) 0.016(4) 0.003(3) 0.001(3) -0.001(3) C213 0.021(4) 0.026(4) 0.012(4) -0.002(3) 0.009(3) -0.007(3) C214 0.015(3) 0.017(3) 0.015(4) 0.003(3) 0.000(3) -0.001(3) C215 0.009(3) 0.028(4) 0.024(4) -0.002(3) -0.001(3) 0.001(3) C216 0.019(4) 0.020(4) 0.016(4) -0.006(3) 0.000(3) 0.000(3) C217 0.028(4) 0.024(4) 0.010(4) -0.001(3) 0.001(3) 0.003(3) C218 0.023(4) 0.020(4) 0.018(4) 0.005(3) -0.002(3) 0.000(3) C219 0.042(5) 0.020(4) 0.020(4) 0.000(3) -0.003(4) 0.002(3) C220 0.032(4) 0.026(4) 0.024(4) 0.005(3) -0.006(4) -0.004(3) C221 0.028(4) 0.036(5) 0.039(6) 0.001(4) -0.003(4) 0.000(4) C222 0.037(5) 0.031(4) 0.034(5) 0.001(4) 0.012(4) 0.001(4) C223 0.029(4) 0.024(4) 0.026(5) -0.001(3) -0.003(3) 0.002(3) C224 0.030(4) 0.028(4) 0.015(4) 0.004(3) 0.002(3) 0.008(3) C225 0.023(4) 0.017(4) 0.028(5) -0.003(3) 0.002(3) 0.001(3) C226 0.027(4) 0.026(4) 0.032(5) -0.004(4) 0.010(4) 0.008(3) C227 0.036(5) 0.021(5) 0.039(5) 0.000(4) 0.003(4) 0.004(3) C228 0.053(6) 0.035(5) 0.028(5) -0.005(4) 0.012(4) 0.007(4) C229 0.061(6) 0.035(5) 0.031(5) 0.000(4) 0.005(5) 0.028(5) C230 0.034(5) 0.047(6) 0.024(5) -0.012(4) 0.000(4) 0.005(4) C231 0.039(5) 0.029(4) 0.024(5) -0.008(4) 0.004(4) 0.005(4) C232 0.020(4) 0.031(4) 0.036(5) 0.004(4) 0.006(3) 0.008(3) C233 0.025(4) 0.018(3) 0.013(4) -0.004(3) 0.001(3) -0.006(3) C234 0.020(4) 0.022(4) 0.021(4) -0.008(3) -0.007(3) -0.001(3) C235 0.032(4) 0.026(4) 0.032(5) -0.007(4) -0.005(4) 0.001(3) C236 0.035(5) 0.029(5) 0.038(5) -0.002(4) -0.010(4) 0.007(4) C237 0.025(4) 0.040(5) 0.051(6) -0.014(5) -0.003(4) 0.002(4) C238 0.027(4) 0.044(5) 0.031(5) -0.006(4) 0.008(4) -0.008(4) C239 0.034(4) 0.027(4) 0.017(4) -0.004(3) -0.002(3) -0.003(3) C240 0.026(4) 0.024(4) 0.014(4) -0.004(3) 0.000(3) -0.003(3) C241 0.015(4) 0.028(4) 0.034(5) 0.005(4) 0.003(3) -0.002(3) C242 0.028(4) 0.032(4) 0.029(5) 0.004(4) 0.008(4) -0.013(3) C243 0.034(5) 0.033(5) 0.028(4) -0.003(4) -0.002(4) -0.014(4) C244 0.068(7) 0.044(6) 0.037(6) -0.006(5) 0.005(5) -0.016(5) C245 0.072(8) 0.061(7) 0.027(5) 0.000(6) 0.000(5) -0.031(6) C246 0.060(7) 0.052(6) 0.036(6) 0.014(5) -0.003(5) -0.016(5) C247 0.052(6) 0.042(5) 0.035(6) 0.019(4) -0.008(5) -0.010(4) C248 0.025(4) 0.037(5) 0.035(5) -0.005(4) 0.013(4) -0.012(3) Br1 0.0458(5) 0.0263(4) 0.0360(5) 0.0018(4) 0.0002(4) 0.0007(4) Br2 0.0548(6) 0.0512(7) 0.0302(5) -0.0046(5) 0.0071(5) -0.0079(5) Br3 0.0308(5) 0.0279(4) 0.0404(5) -0.0017(4) 0.0033(4) -0.0043(4) Br4 0.0424(5) 0.0366(5) 0.0349(5) 0.0023(4) 0.0078(4) -0.0028(4) Br5 0.0499(6) 0.0429(5) 0.0329(5) -0.0041(5) 0.0061(4) -0.0122(4) Br6 0.0232(5) 0.0269(4) 0.0433(6) -0.0005(3) 0.0061(4) -0.0005(3) O1W 0.032(3) 0.018(3) 0.014(3) 0.0016(19) 0.000(2) 0.001(2) O2W 0.027(3) 0.017(3) 0.015(3) 0.0028(18) 0.003(2) -0.004(2) O3W 0.046(4) 0.037(3) 0.032(4) -0.004(3) -0.003(3) -0.003(3) O4W 0.054(4) 0.040(4) 0.034(4) 0.008(3) 0.015(3) 0.002(3) O5W 0.058(5) 0.067(5) 0.030(4) -0.006(3) 0.000(3) -0.011(4) O6W 0.049(4) 0.031(3) 0.022(3) -0.001(3) 0.005(3) 0.007(3) O7W 0.059(4) 0.024(3) 0.055(4) -0.003(3) -0.006(4) 0.011(3) O8W 0.055(4) 0.067(5) 0.036(4) 0.020(4) 0.015(3) 0.011(4) O9W 0.060(4) 0.042(4) 0.026(4) 0.000(3) 0.005(3) -0.019(3) O10W 0.047(3) 0.039(3) 0.026(3) -0.003(3) 0.002(3) -0.004(3) O11W 0.060(4) 0.036(3) 0.037(4) 0.005(3) 0.014(3) -0.001(3) O12W 0.061(5) 0.070(5) 0.049(5) -0.011(4) 0.018(4) -0.015(4) O13W 0.078(5) 0.037(4) 0.022(4) -0.004(3) -0.001(3) 0.017(3) O14W 0.048(3) 0.023(3) 0.052(4) -0.003(3) -0.002(3) 0.005(3) O15W 0.058(5) 0.073(5) 0.032(4) -0.004(4) -0.010(3) 0.002(4) O16W 0.055(4) 0.035(4) 0.021(3) -0.004(3) 0.005(3) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O13 2.257(5) . ? Yb1 O12 2.267(5) . ? Yb1 O11 2.282(5) . ? Yb1 O14 2.294(5) . ? Yb1 O1W 2.445(5) . ? Yb1 N11 2.605(6) . ? Yb1 N12 2.606(5) . ? Yb1 N14 2.613(6) . ? Yb1 N13 2.655(6) . ? Yb1 C112 3.156(7) . ? Yb1 C110 3.161(7) . ? Yb1 C116 3.177(7) . ? O11 C110 1.250(9) . ? O12 C112 1.278(8) . ? O13 C114 1.265(9) . ? O14 C116 1.252(8) . ? N11 C109 1.469(9) . ? N11 C101 1.478(9) . ? N11 C108 1.499(9) . ? N12 C102 1.488(10) . ? N12 C103 1.489(9) . ? N12 C111 1.498(9) . ? N13 C113 1.460(9) . ? N13 C104 1.481(9) . ? N13 C105 1.504(9) . ? N14 C106 1.484(10) . ? N14 C115 1.493(9) . ? N14 C107 1.508(9) . ? N15 C110 1.337(9) . ? N15 C117 1.475(9) . ? N15 H15A 0.8800 . ? N16 C112 1.323(9) . ? N16 C125 1.471(10) . ? N16 H16A 0.8800 . ? N17 C114 1.318(9) . ? N17 C133 1.474(9) . ? N17 H17A 0.8800 . ? N18 C116 1.332(9) . ? N18 C141 1.453(10) . ? N18 H18A 0.8800 . ? C101 C102 1.515(11) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.512(11) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.510(10) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.497(11) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.497(10) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C111 C112 1.486(10) . ? C111 H11A 0.9900 . ? C111 H11B 0.9900 . ? C113 C114 1.503(10) . ? C113 H11C 0.9900 . ? C113 H11D 0.9900 . ? C115 C116 1.499(10) . ? C115 H11E 0.9900 . ? C115 H11F 0.9900 . ? C117 C124 1.492(11) . ? C117 C118 1.521(11) . ? C117 H11G 1.0000 . ? C118 C119 1.387(11) . ? C118 C123 1.437(11) . ? C119 C120 1.373(12) . ? C119 H11H 0.9500 . ? C120 C121 1.408(13) . ? C120 H12A 0.9500 . ? C121 C122 1.394(12) . ? C121 H12B 0.9500 . ? C122 C123 1.363(12) . ? C122 H12C 0.9500 . ? C123 H12D 0.9500 . ? C124 H12E 0.9800 . ? C124 H12F 0.9800 . ? C124 H12G 0.9800 . ? C125 C132 1.517(10) . ? C125 C126 1.521(11) . ? C125 H12H 1.0000 . ? C126 C127 1.382(11) . ? C126 C131 1.387(11) . ? C127 C128 1.413(13) . ? C127 H12I 0.9500 . ? C128 C129 1.338(13) . ? C128 H12J 0.9500 . ? C129 C130 1.391(13) . ? C129 H12K 0.9500 . ? C130 C131 1.396(12) . ? C130 H13A 0.9500 . ? C131 H13B 0.9500 . ? C132 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C133 C134 1.501(11) . ? C133 C140 1.508(11) . ? C133 H13F 1.0000 . ? C134 C135 1.374(11) . ? C134 C139 1.429(11) . ? C135 C136 1.382(12) . ? C135 H13G 0.9500 . ? C136 C137 1.386(13) . ? C136 H13H 0.9500 . ? C137 C138 1.382(14) . ? C137 H13I 0.9500 . ? C138 C139 1.360(12) . ? C138 H13J 0.9500 . ? C139 H13K 0.9500 . ? C140 H14A 0.9800 . ? C140 H14B 0.9800 . ? C140 H14C 0.9800 . ? C141 C142 1.512(11) . ? C141 C148 1.515(10) . ? C141 H14D 1.0000 . ? C142 C147 1.384(11) . ? C142 C143 1.385(12) . ? C143 C144 1.411(12) . ? C143 H14E 0.9500 . ? C144 C145 1.379(14) . ? C144 H14F 0.9500 . ? C145 C146 1.332(15) . ? C145 H14G 0.9500 . ? C146 C147 1.401(14) . ? C146 H14H 0.9500 . ? C147 H14I 0.9500 . ? C148 H14J 0.9800 . ? C148 H14K 0.9800 . ? C148 H14L 0.9800 . ? Yb2 O21 2.265(5) . ? Yb2 O22 2.284(5) . ? Yb2 O24 2.288(5) . ? Yb2 O23 2.295(5) . ? Yb2 O2W 2.440(5) . ? Yb2 N24 2.590(6) . ? Yb2 N23 2.622(6) . ? Yb2 N22 2.636(6) . ? Yb2 N21 2.649(6) . ? Yb2 C216 3.173(7) . ? Yb2 C212 3.177(7) . ? Yb2 C210 3.179(7) . ? O21 C210 1.262(9) . ? O22 C212 1.249(8) . ? O23 C214 1.271(9) . ? O24 C216 1.259(8) . ? N21 C201 1.482(9) . ? N21 C209 1.486(9) . ? N21 C208 1.499(8) . ? N22 C211 1.476(9) . ? N22 C203 1.480(9) . ? N22 C202 1.493(9) . ? N23 C205 1.481(9) . ? N23 C213 1.487(9) . ? N23 C204 1.499(9) . ? N24 C206 1.477(9) . ? N24 C215 1.477(9) . ? N24 C207 1.480(9) . ? N25 C210 1.307(9) . ? N25 C217 1.492(9) . ? N25 H25A 0.8800 . ? N26 C212 1.292(9) . ? N26 C225 1.490(10) . ? N26 H26A 0.8800 . ? N27 C214 1.301(9) . ? N27 C233 1.496(9) . ? N27 H27A 0.8800 . ? N28 C216 1.283(9) . ? N28 C241 1.491(10) . ? N28 H28A 0.8800 . ? C201 C202 1.522(10) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.525(10) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.539(10) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.524(10) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.507(9) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C211 C212 1.511(10) . ? C211 H21A 0.9900 . ? C211 H21B 0.9900 . ? C213 C214 1.498(9) . ? C213 H21C 0.9900 . ? C213 H21D 0.9900 . ? C215 C216 1.527(11) . ? C215 H21E 0.9900 . ? C215 H21F 0.9900 . ? C217 C218 1.513(11) . ? C217 C224 1.528(10) . ? C217 H21G 1.0000 . ? C218 C223 1.369(11) . ? C218 C219 1.390(11) . ? C219 C220 1.396(12) . ? C219 H21H 0.9500 . ? C220 C221 1.366(13) . ? C220 H22A 0.9500 . ? C221 C222 1.388(12) . ? C221 H22B 0.9500 . ? C222 C223 1.417(12) . ? C222 H22C 0.9500 . ? C223 H22D 0.9500 . ? C224 H22E 0.9800 . ? C224 H22F 0.9800 . ? C224 H22G 0.9800 . ? C225 C226 1.502(12) . ? C225 C232 1.520(10) . ? C225 H22H 1.0000 . ? C226 C231 1.378(12) . ? C226 C227 1.389(12) . ? C227 C228 1.379(13) . ? C227 H22I 0.9500 . ? C228 C229 1.360(14) . ? C228 H22J 0.9500 . ? C229 C230 1.358(14) . ? C229 H22K 0.9500 . ? C230 C231 1.399(12) . ? C230 H23A 0.9500 . ? C231 H23B 0.9500 . ? C232 H23C 0.9800 . ? C232 H23D 0.9800 . ? C232 H23E 0.9800 . ? C233 C234 1.516(10) . ? C233 C240 1.527(10) . ? C233 H23F 1.0000 . ? C234 C239 1.354(12) . ? C234 C235 1.398(11) . ? C235 C236 1.402(12) . ? C235 H23G 0.9500 . ? C236 C237 1.353(14) . ? C236 H23H 0.9500 . ? C237 C238 1.379(13) . ? C237 H23I 0.9500 . ? C238 C239 1.409(12) . ? C238 H23J 0.9500 . ? C239 H23K 0.9500 . ? C240 H24A 0.9800 . ? C240 H24B 0.9800 . ? C240 H24C 0.9800 . ? C241 C242 1.515(12) . ? C241 C248 1.524(10) . ? C241 H24D 1.0000 . ? C242 C243 1.366(13) . ? C242 C247 1.406(12) . ? C243 C244 1.404(13) . ? C243 H24E 0.9500 . ? C244 C245 1.373(15) . ? C244 H24F 0.9500 . ? C245 C246 1.417(16) . ? C245 H24G 0.9500 . ? C246 C247 1.367(14) . ? C246 H24H 0.9500 . ? C247 H24I 0.9500 . ? C248 H24J 0.9800 . ? C248 H24K 0.9800 . ? C248 H24L 0.9800 . ? 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 O13 Yb1 O12 81.72(18) . . ? O13 Yb1 O11 140.89(18) . . ? O12 Yb1 O11 83.77(18) . . ? O13 Yb1 O14 84.80(18) . . ? O12 Yb1 O14 140.30(17) . . ? O11 Yb1 O14 83.63(18) . . ? O13 Yb1 O1W 70.23(17) . . ? O12 Yb1 O1W 71.29(17) . . ? O11 Yb1 O1W 70.73(16) . . ? O14 Yb1 O1W 69.01(18) . . ? O13 Yb1 N11 142.99(18) . . ? O12 Yb1 N11 133.20(17) . . ? O11 Yb1 N11 67.20(17) . . ? O14 Yb1 N11 73.98(18) . . ? O1W Yb1 N11 125.94(17) . . ? O13 Yb1 N12 131.07(18) . . ? O12 Yb1 N12 68.36(18) . . ? O11 Yb1 N12 74.61(18) . . ? O14 Yb1 N12 141.95(19) . . ? O1W Yb1 N12 128.70(18) . . ? N11 Yb1 N12 68.94(19) . . ? O13 Yb1 N14 74.69(18) . . ? O12 Yb1 N14 141.89(18) . . ? O11 Yb1 N14 132.60(18) . . ? O14 Yb1 N14 67.10(18) . . ? O1W Yb1 N14 125.22(17) . . ? N11 Yb1 N14 69.24(18) . . ? N12 Yb1 N14 106.08(19) . . ? O13 Yb1 N13 66.68(17) . . ? O12 Yb1 N13 75.43(18) . . ? O11 Yb1 N13 142.45(17) . . ? O14 Yb1 N13 131.51(18) . . ? O1W Yb1 N13 128.27(17) . . ? N11 Yb1 N13 105.7(2) . . ? N12 Yb1 N13 68.79(18) . . ? N14 Yb1 N13 67.91(18) . . ? O13 Yb1 C112 98.81(19) . . ? O12 Yb1 C112 19.77(18) . . ? O11 Yb1 C112 76.44(18) . . ? O14 Yb1 C112 152.51(18) . . ? O1W Yb1 C112 86.46(18) . . ? N11 Yb1 C112 114.06(18) . . ? N12 Yb1 C112 48.89(19) . . ? N14 Yb1 C112 140.23(18) . . ? N13 Yb1 C112 73.49(18) . . ? O13 Yb1 C110 151.56(18) . . ? O12 Yb1 C110 101.22(18) . . ? O11 Yb1 C110 19.06(18) . . ? O14 Yb1 C110 74.93(18) . . ? O1W Yb1 C110 83.80(17) . . ? N11 Yb1 C110 48.81(18) . . ? N12 Yb1 C110 74.51(18) . . ? N14 Yb1 C110 113.81(19) . . ? N13 Yb1 C110 141.66(17) . . ? C112 Yb1 C110 90.73(19) . . ? O13 Yb1 C116 76.21(19) . . ? O12 Yb1 C116 150.09(18) . . ? O11 Yb1 C116 100.88(19) . . ? O14 Yb1 C116 18.93(18) . . ? O1W Yb1 C116 82.30(18) . . ? N11 Yb1 C116 74.09(18) . . ? N12 Yb1 C116 141.49(19) . . ? N14 Yb1 C116 48.83(18) . . ? N13 Yb1 C116 112.79(19) . . ? C112 Yb1 C116 168.69(18) . . ? C110 Yb1 C116 89.32(19) . . ? C110 O11 Yb1 124.3(4) . . ? C112 O12 Yb1 123.4(5) . . ? C114 O13 Yb1 126.9(4) . . ? C116 O14 Yb1 124.6(5) . . ? C109 N11 C101 110.2(6) . . ? C109 N11 C108 108.5(6) . . ? C101 N11 C108 108.9(6) . . ? C109 N11 Yb1 107.0(4) . . ? C101 N11 Yb1 110.9(4) . . ? C108 N11 Yb1 111.3(4) . . ? C102 N12 C103 108.9(6) . . ? C102 N12 C111 110.0(5) . . ? C103 N12 C111 109.5(6) . . ? C102 N12 Yb1 111.3(4) . . ? C103 N12 Yb1 111.4(4) . . ? C111 N12 Yb1 105.7(4) . . ? C113 N13 C104 110.3(6) . . ? C113 N13 C105 109.4(6) . . ? C104 N13 C105 109.1(5) . . ? C113 N13 Yb1 107.3(4) . . ? C104 N13 Yb1 110.3(4) . . ? C105 N13 Yb1 110.4(4) . . ? C106 N14 C115 109.2(5) . . ? C106 N14 C107 108.4(5) . . ? C115 N14 C107 109.2(6) . . ? C106 N14 Yb1 113.0(4) . . ? C115 N14 Yb1 106.3(4) . . ? C107 N14 Yb1 110.7(4) . . ? C110 N15 C117 121.5(7) . . ? C110 N15 H15A 119.2 . . ? C117 N15 H15A 119.2 . . ? C112 N16 C125 122.1(6) . . ? C112 N16 H16A 118.9 . . ? C125 N16 H16A 118.9 . . ? C114 N17 C133 120.2(7) . . ? C114 N17 H17A 119.9 . . ? C133 N17 H17A 119.9 . . ? C116 N18 C141 121.0(6) . . ? C116 N18 H18A 119.5 . . ? C141 N18 H18A 119.5 . . ? N11 C101 C102 113.2(6) . . ? N11 C101 H10A 108.9 . . ? C102 C101 H10A 108.9 . . ? N11 C101 H10B 108.9 . . ? C102 C101 H10B 108.9 . . ? H10A C101 H10B 107.8 . . ? N12 C102 C101 110.7(6) . . ? N12 C102 H10C 109.5 . . ? C101 C102 H10C 109.5 . . ? N12 C102 H10D 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 108.1 . . ? N12 C103 C104 113.8(6) . . ? N12 C103 H10E 108.8 . . ? C104 C103 H10E 108.8 . . ? N12 C103 H10F 108.8 . . ? C104 C103 H10F 108.8 . . ? H10E C103 H10F 107.7 . . ? N13 C104 C103 111.5(6) . . ? N13 C104 H10G 109.3 . . ? C103 C104 H10G 109.3 . . ? N13 C104 H10H 109.3 . . ? C103 C104 H10H 109.3 . . ? H10G C104 H10H 108.0 . . ? N13 C105 C106 112.0(6) . . ? N13 C105 H10I 109.2 . . ? C106 C105 H10I 109.2 . . ? N13 C105 H10J 109.2 . . ? C106 C105 H10J 109.2 . . ? H10I C105 H10J 107.9 . . ? N14 C106 C105 110.8(6) . . ? N14 C106 H10K 109.5 . . ? C105 C106 H10K 109.5 . . ? N14 C106 H10L 109.5 . . ? C105 C106 H10L 109.5 . . ? H10K C106 H10L 108.1 . . ? C108 C107 N14 113.8(6) . . ? C108 C107 H10M 108.8 . . ? N14 C107 H10M 108.8 . . ? C108 C107 H10N 108.8 . . ? N14 C107 H10N 108.8 . . ? H10M C107 H10N 107.7 . . ? C107 C108 N11 111.3(6) . . ? C107 C108 H10O 109.4 . . ? N11 C108 H10O 109.4 . . ? C107 C108 H10P 109.4 . . ? N11 C108 H10P 109.4 . . ? H10O C108 H10P 108.0 . . ? N11 C109 C110 110.4(6) . . ? N11 C109 H10Q 109.6 . . ? C110 C109 H10Q 109.6 . . ? N11 C109 H10R 109.6 . . ? C110 C109 H10R 109.6 . . ? H10Q C109 H10R 108.1 . . ? O11 C110 N15 122.7(7) . . ? O11 C110 C109 120.2(6) . . ? N15 C110 C109 117.1(7) . . ? O11 C110 Yb1 36.6(3) . . ? N15 C110 Yb1 159.3(5) . . ? C109 C110 Yb1 83.6(4) . . ? C112 C111 N12 109.5(5) . . ? C112 C111 H11A 109.8 . . ? N12 C111 H11A 109.8 . . ? C112 C111 H11B 109.8 . . ? N12 C111 H11B 109.8 . . ? H11A C111 H11B 108.2 . . ? O12 C112 N16 121.3(7) . . ? O12 C112 C111 120.1(6) . . ? N16 C112 C111 118.5(6) . . ? O12 C112 Yb1 36.9(3) . . ? N16 C112 Yb1 157.6(5) . . ? C111 C112 Yb1 83.7(4) . . ? N13 C113 C114 112.3(6) . . ? N13 C113 H11C 109.2 . . ? C114 C113 H11C 109.2 . . ? N13 C113 H11D 109.1 . . ? C114 C113 H11D 109.1 . . ? H11C C113 H11D 107.9 . . ? O13 C114 N17 122.4(7) . . ? O13 C114 C113 119.2(6) . . ? N17 C114 C113 118.4(7) . . ? O13 C114 Yb1 34.6(3) . . ? N17 C114 Yb1 156.8(5) . . ? C113 C114 Yb1 84.6(4) . . ? N14 C115 C116 109.7(5) . . ? N14 C115 H11E 109.7 . . ? C116 C115 H11E 109.7 . . ? N14 C115 H11F 109.7 . . ? C116 C115 H11F 109.7 . . ? H11E C115 H11F 108.2 . . ? O14 C116 N18 121.6(7) . . ? O14 C116 C115 119.8(7) . . ? N18 C116 C115 118.5(6) . . ? O14 C116 Yb1 36.5(3) . . ? N18 C116 Yb1 158.1(5) . . ? C115 C116 Yb1 83.4(4) . . ? N15 C117 C124 110.1(7) . . ? N15 C117 C118 110.7(6) . . ? C124 C117 C118 111.8(6) . . ? N15 C117 H11G 108.1 . . ? C124 C117 H11G 108.1 . . ? C118 C117 H11G 108.1 . . ? C119 C118 C123 117.3(7) . . ? C119 C118 C117 121.8(7) . . ? C123 C118 C117 120.9(7) . . ? C120 C119 C118 121.5(8) . . ? C120 C119 H11H 119.3 . . ? C118 C119 H11H 119.3 . . ? C119 C120 C121 120.7(7) . . ? C119 C120 H12A 119.6 . . ? C121 C120 H12A 119.6 . . ? C122 C121 C120 118.7(8) . . ? C122 C121 H12B 120.6 . . ? C120 C121 H12B 120.6 . . ? C123 C122 C121 120.6(8) . . ? C123 C122 H12C 119.7 . . ? C121 C122 H12C 119.7 . . ? C122 C123 C118 121.2(7) . . ? C122 C123 H12D 119.4 . . ? C118 C123 H12D 119.4 . . ? C117 C124 H12E 109.5 . . ? C117 C124 H12F 109.5 . . ? H12E C124 H12F 109.5 . . ? C117 C124 H12G 109.5 . . ? H12E C124 H12G 109.5 . . ? H12F C124 H12G 109.5 . . ? N16 C125 C132 108.4(6) . . ? N16 C125 C126 110.8(6) . . ? C132 C125 C126 111.8(7) . . ? N16 C125 H12H 108.6 . . ? C132 C125 H12H 108.6 . . ? C126 C125 H12H 108.6 . . ? C127 C126 C131 119.5(8) . . ? C127 C126 C125 121.1(7) . . ? C131 C126 C125 119.3(7) . . ? C126 C127 C128 119.2(8) . . ? C126 C127 H12I 120.4 . . ? C128 C127 H12I 120.4 . . ? C129 C128 C127 120.4(8) . . ? C129 C128 H12J 119.8 . . ? C127 C128 H12J 119.8 . . ? C128 C129 C130 121.7(9) . . ? C128 C129 H12K 119.2 . . ? C130 C129 H12K 119.2 . . ? C129 C130 C131 118.2(9) . . ? C129 C130 H13A 120.9 . . ? C131 C130 H13A 120.9 . . ? C126 C131 C130 120.9(8) . . ? C126 C131 H13B 119.6 . . ? C130 C131 H13B 119.6 . . ? C125 C132 H13C 109.5 . . ? C125 C132 H13D 109.5 . . ? H13C C132 H13D 109.5 . . ? C125 C132 H13E 109.5 . . ? H13C C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? N17 C133 C134 112.0(6) . . ? N17 C133 C140 109.7(7) . . ? C134 C133 C140 112.9(6) . . ? N17 C133 H13F 107.3 . . ? C134 C133 H13F 107.3 . . ? C140 C133 H13F 107.3 . . ? C135 C134 C139 118.5(8) . . ? C135 C134 C133 121.4(7) . . ? C139 C134 C133 120.0(7) . . ? C134 C135 C136 121.3(8) . . ? C134 C135 H13G 119.4 . . ? C136 C135 H13G 119.4 . . ? C135 C136 C137 119.5(8) . . ? C135 C136 H13H 120.3 . . ? C137 C136 H13H 120.3 . . ? C138 C137 C136 120.1(8) . . ? C138 C137 H13I 119.9 . . ? C136 C137 H13I 119.9 . . ? C139 C138 C137 120.9(9) . . ? C139 C138 H13J 119.6 . . ? C137 C138 H13J 119.6 . . ? C138 C139 C134 119.7(8) . . ? C138 C139 H13K 120.2 . . ? C134 C139 H13K 120.2 . . ? C133 C140 H14A 109.5 . . ? C133 C140 H14B 109.5 . . ? H14A C140 H14B 109.5 . . ? C133 C140 H14C 109.5 . . ? H14A C140 H14C 109.5 . . ? H14B C140 H14C 109.5 . . ? N18 C141 C142 111.4(6) . . ? N18 C141 C148 108.8(6) . . ? C142 C141 C148 112.2(7) . . ? N18 C141 H14D 108.1 . . ? C142 C141 H14D 108.1 . . ? C148 C141 H14D 108.1 . . ? C147 C142 C143 118.9(8) . . ? C147 C142 C141 120.6(8) . . ? C143 C142 C141 120.4(7) . . ? C142 C143 C144 120.0(9) . . ? C142 C143 H14E 120.0 . . ? C144 C143 H14E 120.0 . . ? C145 C144 C143 119.3(10) . . ? C145 C144 H14F 120.4 . . ? C143 C144 H14F 120.4 . . ? C146 C145 C144 120.8(9) . . ? C146 C145 H14G 119.6 . . ? C144 C145 H14G 119.6 . . ? C145 C146 C147 121.0(9) . . ? C145 C146 H14H 119.5 . . ? C147 C146 H14H 119.5 . . ? C142 C147 C146 120.0(9) . . ? C142 C147 H14I 120.0 . . ? C146 C147 H14I 120.0 . . ? C141 C148 H14J 109.5 . . ? C141 C148 H14K 109.5 . . ? H14J C148 H14K 109.5 . . ? C141 C148 H14L 109.5 . . ? H14J C148 H14L 109.5 . . ? H14K C148 H14L 109.5 . . ? O21 Yb2 O22 83.79(17) . . ? O21 Yb2 O24 81.84(17) . . ? O22 Yb2 O24 140.18(18) . . ? O21 Yb2 O23 140.9(2) . . ? O22 Yb2 O23 83.66(17) . . ? O24 Yb2 O23 84.53(17) . . ? O21 Yb2 O2W 70.34(16) . . ? O22 Yb2 O2W 68.60(16) . . ? O24 Yb2 O2W 71.60(16) . . ? O23 Yb2 O2W 70.57(16) . . ? O21 Yb2 N24 131.53(19) . . ? O22 Yb2 N24 142.71(18) . . ? O24 Yb2 N24 67.96(18) . . ? O23 Yb2 N24 74.49(18) . . ? O2W Yb2 N24 128.12(17) . . ? O21 Yb2 N23 142.51(17) . . ? O22 Yb2 N23 74.57(17) . . ? O24 Yb2 N23 133.49(17) . . ? O23 Yb2 N23 67.19(17) . . ? O2W Yb2 N23 125.91(17) . . ? N24 Yb2 N23 69.23(19) . . ? O21 Yb2 N22 74.92(18) . . ? O22 Yb2 N22 66.69(17) . . ? O24 Yb2 N22 142.07(18) . . ? O23 Yb2 N22 131.67(18) . . ? O2W Yb2 N22 125.23(16) . . ? N24 Yb2 N22 106.63(19) . . ? N23 Yb2 N22 68.53(18) . . ? O21 Yb2 N21 66.82(18) . . ? O22 Yb2 N21 131.31(17) . . ? O24 Yb2 N21 74.88(17) . . ? O23 Yb2 N21 142.77(17) . . ? O2W Yb2 N21 128.27(16) . . ? N24 Yb2 N21 69.14(19) . . ? N23 Yb2 N21 105.76(19) . . ? N22 Yb2 N21 68.57(18) . . ? O21 Yb2 C216 98.95(18) . . ? O22 Yb2 C216 151.46(17) . . ? O24 Yb2 C216 19.13(18) . . ? O23 Yb2 C216 76.37(17) . . ? O2W Yb2 C216 85.46(17) . . ? N24 Yb2 C216 49.34(19) . . ? N23 Yb2 C216 114.71(18) . . ? N22 Yb2 C216 141.59(18) . . ? N21 Yb2 C216 74.16(18) . . ? O21 Yb2 C212 75.41(18) . . ? O22 Yb2 C212 18.63(18) . . ? O24 Yb2 C212 149.62(17) . . ? O23 Yb2 C212 100.58(18) . . ? O2W Yb2 C212 81.83(17) . . ? N24 Yb2 C212 142.36(18) . . ? N23 Yb2 C212 74.48(18) . . ? N22 Yb2 C212 48.75(18) . . ? N21 Yb2 C212 112.93(18) . . ? C216 Yb2 C212 167.22(19) . . ? O21 Yb2 C210 18.69(17) . . ? O22 Yb2 C210 100.95(17) . . ? O24 Yb2 C210 73.13(18) . . ? O23 Yb2 C210 150.29(18) . . ? O2W Yb2 C210 83.71(16) . . ? N24 Yb2 C210 113.06(19) . . ? N23 Yb2 C210 142.46(17) . . ? N22 Yb2 C210 75.46(18) . . ? N21 Yb2 C210 49.04(17) . . ? C216 Yb2 C210 87.28(19) . . ? C212 Yb2 C210 89.89(18) . . ? C210 O21 Yb2 126.2(4) . . ? C212 O22 Yb2 125.6(5) . . ? C214 O23 Yb2 124.6(4) . . ? C216 O24 Yb2 124.3(5) . . ? C201 N21 C209 109.9(6) . . ? C201 N21 C208 109.7(5) . . ? C209 N21 C208 109.5(6) . . ? C201 N21 Yb2 110.6(4) . . ? C209 N21 Yb2 107.3(4) . . ? C208 N21 Yb2 109.7(4) . . ? C211 N22 C203 111.6(6) . . ? C211 N22 C202 108.8(6) . . ? C203 N22 C202 108.4(6) . . ? C211 N22 Yb2 105.9(4) . . ? C203 N22 Yb2 111.5(4) . . ? C202 N22 Yb2 110.7(4) . . ? C205 N23 C213 110.0(6) . . ? C205 N23 C204 109.3(5) . . ? C213 N23 C204 108.6(5) . . ? C205 N23 Yb2 110.4(4) . . ? C213 N23 Yb2 107.3(4) . . ? C204 N23 Yb2 111.2(4) . . ? C206 N24 C215 108.8(6) . . ? C206 N24 C207 108.1(5) . . ? C215 N24 C207 110.3(6) . . ? C206 N24 Yb2 111.3(4) . . ? C215 N24 Yb2 106.3(4) . . ? C207 N24 Yb2 112.0(4) . . ? C210 N25 C217 121.1(6) . . ? C210 N25 H25A 119.5 . . ? C217 N25 H25A 119.5 . . ? C212 N26 C225 121.0(6) . . ? C212 N26 H26A 119.5 . . ? C225 N26 H26A 119.5 . . ? C214 N27 C233 122.0(6) . . ? C214 N27 H27A 119.0 . . ? C233 N27 H27A 119.0 . . ? C216 N28 C241 121.7(6) . . ? C216 N28 H28A 119.1 . . ? C241 N28 H28A 119.1 . . ? N21 C201 C202 112.2(6) . . ? N21 C201 H20A 109.2 . . ? C202 C201 H20A 109.2 . . ? N21 C201 H20B 109.2 . . ? C202 C201 H20B 109.2 . . ? H20A C201 H20B 107.9 . . ? N22 C202 C201 111.6(6) . . ? N22 C202 H20C 109.3 . . ? C201 C202 H20C 109.3 . . ? N22 C202 H20D 109.3 . . ? C201 C202 H20D 109.3 . . ? H20C C202 H20D 108.0 . . ? N22 C203 C204 112.3(6) . . ? N22 C203 H20E 109.1 . . ? C204 C203 H20E 109.1 . . ? N22 C203 H20F 109.1 . . ? C204 C203 H20F 109.1 . . ? H20E C203 H20F 107.9 . . ? N23 C204 C203 111.1(6) . . ? N23 C204 H20G 109.4 . . ? C203 C204 H20G 109.4 . . ? N23 C204 H20H 109.4 . . ? C203 C204 H20H 109.4 . . ? H20G C204 H20H 108.0 . . ? N23 C205 C206 111.8(6) . . ? N23 C205 H20I 109.3 . . ? C206 C205 H20I 109.3 . . ? N23 C205 H20J 109.3 . . ? C206 C205 H20J 109.3 . . ? H20I C205 H20J 107.9 . . ? N24 C206 C205 111.1(6) . . ? N24 C206 H20K 109.4 . . ? C205 C206 H20K 109.4 . . ? N24 C206 H20L 109.4 . . ? C205 C206 H20L 109.4 . . ? H20K C206 H20L 108.0 . . ? N24 C207 C208 113.2(6) . . ? N24 C207 H20M 108.9 . . ? C208 C207 H20M 108.9 . . ? N24 C207 H20N 108.9 . . ? C208 C207 H20N 108.9 . . ? H20M C207 H20N 107.8 . . ? N21 C208 C207 111.0(6) . . ? N21 C208 H20O 109.4 . . ? C207 C208 H20O 109.4 . . ? N21 C208 H20P 109.4 . . ? C207 C208 H20P 109.4 . . ? H20O C208 H20P 108.0 . . ? N21 C209 C210 111.0(6) . . ? N21 C209 H20Q 109.4 . . ? C210 C209 H20Q 109.4 . . ? N21 C209 H20R 109.4 . . ? C210 C209 H20R 109.4 . . ? H20Q C209 H20R 108.0 . . ? O21 C210 N25 121.2(6) . . ? O21 C210 C209 120.2(6) . . ? N25 C210 C209 118.6(7) . . ? O21 C210 Yb2 35.1(3) . . ? N25 C210 Yb2 155.6(5) . . ? C209 C210 Yb2 85.2(4) . . ? N22 C211 C212 110.2(6) . . ? N22 C211 H21A 109.6 . . ? C212 C211 H21A 109.6 . . ? N22 C211 H21B 109.6 . . ? C212 C211 H21B 109.6 . . ? H21A C211 H21B 108.1 . . ? O22 C212 N26 122.4(7) . . ? O22 C212 C211 119.0(6) . . ? N26 C212 C211 118.5(6) . . ? O22 C212 Yb2 35.7(3) . . ? N26 C212 Yb2 158.2(5) . . ? C211 C212 Yb2 83.3(4) . . ? N23 C213 C214 110.4(6) . . ? N23 C213 H21C 109.6 . . ? C214 C213 H21C 109.6 . . ? N23 C213 H21D 109.6 . . ? C214 C213 H21D 109.6 . . ? H21C C213 H21D 108.1 . . ? O23 C214 N27 121.4(6) . . ? O23 C214 C213 120.0(6) . . ? N27 C214 C213 118.5(7) . . ? O23 C214 Yb2 36.3(3) . . ? N27 C214 Yb2 157.7(5) . . ? C213 C214 Yb2 83.8(4) . . ? N24 C215 C216 110.1(6) . . ? N24 C215 H21E 109.6 . . ? C216 C215 H21E 109.6 . . ? N24 C215 H21F 109.6 . . ? C216 C215 H21F 109.6 . . ? H21E C215 H21F 108.2 . . ? O24 C216 N28 123.1(7) . . ? O24 C216 C215 118.3(6) . . ? N28 C216 C215 118.6(6) . . ? O24 C216 Yb2 36.6(3) . . ? N28 C216 Yb2 159.2(5) . . ? C215 C216 Yb2 81.9(4) . . ? N25 C217 C218 111.4(6) . . ? N25 C217 C224 108.3(6) . . ? C218 C217 C224 111.9(6) . . ? N25 C217 H21G 108.4 . . ? C218 C217 H21G 108.4 . . ? C224 C217 H21G 108.4 . . ? C223 C218 C219 119.6(7) . . ? C223 C218 C217 119.0(7) . . ? C219 C218 C217 121.4(7) . . ? C218 C219 C220 120.2(8) . . ? C218 C219 H21H 119.9 . . ? C220 C219 H21H 119.9 . . ? C221 C220 C219 120.1(8) . . ? C221 C220 H22A 120.0 . . ? C219 C220 H22A 120.0 . . ? C220 C221 C222 121.0(8) . . ? C220 C221 H22B 119.5 . . ? C222 C221 H22B 119.5 . . ? C221 C222 C223 118.4(8) . . ? C221 C222 H22C 120.8 . . ? C223 C222 H22C 120.8 . . ? C218 C223 C222 120.8(7) . . ? C218 C223 H22D 119.6 . . ? C222 C223 H22D 119.6 . . ? C217 C224 H22E 109.5 . . ? C217 C224 H22F 109.5 . . ? H22E C224 H22F 109.5 . . ? C217 C224 H22G 109.5 . . ? H22E C224 H22G 109.5 . . ? H22F C224 H22G 109.5 . . ? N26 C225 C226 110.9(6) . . ? N26 C225 C232 109.0(6) . . ? C226 C225 C232 113.0(7) . . ? N26 C225 H22H 107.9 . . ? C226 C225 H22H 107.9 . . ? C232 C225 H22H 107.9 . . ? C231 C226 C227 119.5(8) . . ? C231 C226 C225 119.4(8) . . ? C227 C226 C225 121.1(8) . . ? C228 C227 C226 119.2(9) . . ? C228 C227 H22I 120.4 . . ? C226 C227 H22I 120.4 . . ? C229 C228 C227 121.2(9) . . ? C229 C228 H22J 119.4 . . ? C227 C228 H22J 119.4 . . ? C230 C229 C228 120.4(9) . . ? C230 C229 H22K 119.8 . . ? C228 C229 H22K 119.8 . . ? C229 C230 C231 119.7(8) . . ? C229 C230 H23A 120.2 . . ? C231 C230 H23A 120.2 . . ? C226 C231 C230 120.0(8) . . ? C226 C231 H23B 120.0 . . ? C230 C231 H23B 120.0 . . ? C225 C232 H23C 109.5 . . ? C225 C232 H23D 109.5 . . ? H23C C232 H23D 109.5 . . ? C225 C232 H23E 109.5 . . ? H23C C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? N27 C233 C234 110.6(6) . . ? N27 C233 C240 107.8(6) . . ? C234 C233 C240 112.1(6) . . ? N27 C233 H23F 108.7 . . ? C234 C233 H23F 108.7 . . ? C240 C233 H23F 108.7 . . ? C239 C234 C235 119.6(7) . . ? C239 C234 C233 119.4(7) . . ? C235 C234 C233 121.0(7) . . ? C234 C235 C236 119.7(9) . . ? C234 C235 H23G 120.1 . . ? C236 C235 H23G 120.1 . . ? C237 C236 C235 119.3(8) . . ? C237 C236 H23H 120.3 . . ? C235 C236 H23H 120.3 . . ? C236 C237 C238 122.1(8) . . ? C236 C237 H23I 118.9 . . ? C238 C237 H23I 118.9 . . ? C237 C238 C239 118.0(8) . . ? C237 C238 H23J 121.0 . . ? C239 C238 H23J 121.0 . . ? C234 C239 C238 121.2(8) . . ? C234 C239 H23K 119.4 . . ? C238 C239 H23K 119.4 . . ? C233 C240 H24A 109.5 . . ? C233 C240 H24B 109.5 . . ? H24A C240 H24B 109.5 . . ? C233 C240 H24C 109.5 . . ? H24A C240 H24C 109.5 . . ? H24B C240 H24C 109.5 . . ? N28 C241 C242 110.7(6) . . ? N28 C241 C248 108.4(6) . . ? C242 C241 C248 111.9(7) . . ? N28 C241 H24D 108.6 . . ? C242 C241 H24D 108.6 . . ? C248 C241 H24D 108.6 . . ? C243 C242 C247 119.5(9) . . ? C243 C242 C241 122.1(8) . . ? C247 C242 C241 118.2(8) . . ? C242 C243 C244 119.8(9) . . ? C242 C243 H24E 120.1 . . ? C244 C243 H24E 120.1 . . ? C245 C244 C243 120.8(11) . . ? C245 C244 H24F 119.6 . . ? C243 C244 H24F 119.6 . . ? C244 C245 C246 119.4(10) . . ? C244 C245 H24G 120.3 . . ? C246 C245 H24G 120.3 . . ? C247 C246 C245 119.1(10) . . ? C247 C246 H24H 120.5 . . ? C245 C246 H24H 120.5 . . ? C246 C247 C242 121.3(10) . . ? C246 C247 H24I 119.4 . . ? C242 C247 H24I 119.4 . . ? C241 C248 H24J 109.5 . . ? C241 C248 H24K 109.5 . . ? H24J C248 H24K 109.5 . . ? C241 C248 H24L 109.5 . . ? H24J C248 H24L 109.5 . . ? H24K C248 H24L 109.5 . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 26.65 _diffrn_measured_fraction_theta_full 0.914 _refine_diff_density_max 1.418 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.129 #============================================================================== data_[Yb.2]I3 _database_code_depnum_ccdc_archive 'CCDC 606222' #============================================================================== _chemical_name_systematic ; [Yb.DOTAPh]I~3~ ; _chemical_name_common (Yb.DOTAPh)I!3$ _chemical_melting_point 'not measured' _chemical_formula_moiety 'C48 H66 N8 O5 Yb, 3I' _chemical_formula_sum 'C48 H66 I3 N8 O5 Yb' _chemical_formula_weight 1388.83 _chemical_absolute_configuration syn 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 19.6170(13) _cell_length_b 19.7668(14) _cell_length_c 14.5591(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5645.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7962 _cell_measurement_theta_min 2.307 _cell_measurement_theta_max 27.461 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2716 _exptl_absorpt_coefficient_mu 3.344 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5484 _exptl_absorpt_correction_T_max 0.6909 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.0600 -1.00 0.00 0.00 0.0600 0.00 1.00 0.00 0.0800 0.00 -1.00 -1.00 0.0800 0.00 -1.00 1.00 0.1000 0.00 -1.00 0.00 0.1200 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of sets of \w scans each set at different \f and/or 2\q angles and each scan covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 48273 _diffrn_reflns_av_R_equivalents 0.1100 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9938 _reflns_number_gt 8000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+139.0219P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 9938 _refine_ls_number_parameters 300 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1942 _refine_ls_wR_factor_gt 0.1668 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.29993(4) 0.69792(5) 0.75272(6) 0.02067(17) Uani 1 1 d D . . N1 N 0.2154(10) 0.7287(10) 0.8896(12) 0.025(4) Uiso 1 1 d . . . N2 N 0.1703(9) 0.6794(9) 0.7069(11) 0.022(4) Uiso 1 1 d . . . N3 N 0.2630(9) 0.7779(9) 0.6153(11) 0.022(4) Uiso 1 1 d . . . N4 N 0.3083(9) 0.8226(8) 0.7997(11) 0.019(4) Uiso 1 1 d . . . N5 N 0.3578(9) 0.6986(10) 1.0457(13) 0.028(4) Uiso 1 1 d . . . H5A H 0.3366 0.7135 1.0950 0.034 Uiso 1 1 calc R . . N6 N 0.1811(11) 0.5133(12) 0.8062(14) 0.041(6) Uiso 1 1 d . . . H6A H 0.1423 0.4971 0.7851 0.049 Uiso 1 1 calc R . . N7 N 0.3166(10) 0.6429(11) 0.4599(15) 0.038(5) Uiso 1 1 d . . . H7A H 0.3186 0.6657 0.4080 0.046 Uiso 1 1 calc R . . N8 N 0.4785(10) 0.8268(11) 0.6921(13) 0.034(5) Uiso 1 1 d . . . H8A H 0.4900 0.8676 0.7109 0.040 Uiso 1 1 calc R . . O1 O 0.3531(7) 0.6969(8) 0.8924(9) 0.022(3) Uiso 1 1 d . . . O2 O 0.2578(8) 0.5978(8) 0.8038(9) 0.020(3) Uiso 1 1 d . . . O3 O 0.3043(9) 0.6469(8) 0.6147(10) 0.028(4) Uiso 1 1 d . . . O4 O 0.3940(9) 0.7449(9) 0.6983(11) 0.032(4) Uiso 1 1 d . . . O1W O 0.3907(7) 0.6168(7) 0.7573(11) 0.030(3) Uiso 1 1 d D . . H1WB H 0.434(3) 0.627(8) 0.741(13) 0.03(6) Uiso 1 1 d D . . H1WA H 0.400(8) 0.573(2) 0.771(10) 0.04(7) Uiso 1 1 d D . . C1 C 0.1476(14) 0.7009(17) 0.8743(18) 0.040(7) Uiso 1 1 d . . . H1A H 0.1142 0.7251 0.9132 0.048 Uiso 1 1 calc R . . H1B H 0.1471 0.6525 0.8921 0.048 Uiso 1 1 calc R . . C2 C 0.1272(11) 0.7079(11) 0.7721(14) 0.025(5) Uiso 1 1 d . . . H2A H 0.0815 0.6875 0.7644 0.029 Uiso 1 1 calc R . . H2B H 0.1229 0.7567 0.7582 0.029 Uiso 1 1 calc R . . C3 C 0.1540(14) 0.7064(16) 0.6170(18) 0.037(7) Uiso 1 1 d . . . H3A H 0.1039 0.7107 0.6111 0.045 Uiso 1 1 calc R . . H3B H 0.1699 0.6745 0.5692 0.045 Uiso 1 1 calc R . . C4 C 0.1894(14) 0.7805(14) 0.6002(18) 0.039(6) Uiso 1 1 d . . . H4A H 0.1802 0.7955 0.5365 0.047 Uiso 1 1 calc R . . H4B H 0.1689 0.8139 0.6426 0.047 Uiso 1 1 calc R . . C5 C 0.2852(13) 0.8500(13) 0.6326(16) 0.029(6) Uiso 1 1 d . . . H5B H 0.3339 0.8551 0.6157 0.035 Uiso 1 1 calc R . . H5C H 0.2583 0.8809 0.5932 0.035 Uiso 1 1 calc R . . C6 C 0.2758(10) 0.8695(10) 0.7311(13) 0.023(5) Uiso 1 1 d . . . H6B H 0.2263 0.8719 0.7442 0.027 Uiso 1 1 calc R . . H6C H 0.2948 0.9154 0.7402 0.027 Uiso 1 1 calc R . . C7 C 0.2803(11) 0.8387(11) 0.8876(14) 0.019(5) Uiso 1 1 d . . . H7B H 0.2738 0.8883 0.8925 0.023 Uiso 1 1 calc R . . H7C H 0.3123 0.8245 0.9364 0.023 Uiso 1 1 calc R . . C8 C 0.2119(13) 0.8031(14) 0.9010(15) 0.035(5) Uiso 1 1 d . . . H8B H 0.1947 0.8133 0.9634 0.042 Uiso 1 1 calc R . . H8C H 0.1788 0.8215 0.8563 0.042 Uiso 1 1 calc R . . C9 C 0.2444(13) 0.6999(15) 0.9755(16) 0.036(6) Uiso 1 1 d . . . H9A H 0.2260 0.6538 0.9854 0.043 Uiso 1 1 calc R . . H9B H 0.2307 0.7283 1.0285 0.043 Uiso 1 1 calc R . . C10 C 0.3269(11) 0.6968(13) 0.9693(13) 0.021(5) Uiso 1 1 d . . . C11 C 0.1632(16) 0.6082(15) 0.7050(19) 0.046(7) Uiso 1 1 d . . . H11A H 0.1792 0.5911 0.6448 0.055 Uiso 1 1 calc R . . H11B H 0.1143 0.5965 0.7109 0.055 Uiso 1 1 calc R . . C12 C 0.2028(14) 0.5727(13) 0.7810(17) 0.039(6) Uiso 1 1 d . . . C13 C 0.2979(14) 0.7502(13) 0.5333(16) 0.035(6) Uiso 1 1 d . . . H13A H 0.2716 0.7624 0.4777 0.042 Uiso 1 1 calc R . . H13B H 0.3436 0.7710 0.5279 0.042 Uiso 1 1 calc R . . C14 C 0.3051(15) 0.6778(14) 0.5375(16) 0.038(6) Uiso 1 1 d . . . C15 C 0.3841(11) 0.8421(12) 0.7994(14) 0.023(5) Uiso 1 1 d . . . H15A H 0.3891 0.8911 0.7874 0.028 Uiso 1 1 calc R . . H15B H 0.4048 0.8320 0.8599 0.028 Uiso 1 1 calc R . . C16 C 0.4196(13) 0.8016(14) 0.7246(18) 0.040(6) Uiso 1 1 d . . . C17 C 0.4308(13) 0.6753(11) 1.0521(18) 0.049(8) Uiso 1 1 d D . . H17A H 0.4386 0.6305 1.0219 0.059 Uiso 1 1 calc R . . C18 C 0.4709(10) 0.7323(8) 1.0075(12) 0.050(8) Uiso 1 1 d G . . C19 C 0.4619(11) 0.7979(9) 1.0396(13) 0.063(8) Uiso 1 1 d GD . . H19A H 0.4305 0.8067 1.0878 0.075 Uiso 1 1 calc R . . C20 C 0.4988(13) 0.8508(8) 1.0010(16) 0.091(13) Uiso 1 1 d G . . H20A H 0.4927 0.8956 1.0229 0.109 Uiso 1 1 calc R . . C21 C 0.5448(13) 0.8380(10) 0.9304(16) 0.086(12) Uiso 1 1 d G . . H21A H 0.5700 0.8741 0.9040 0.103 Uiso 1 1 calc R . . C22 C 0.5537(10) 0.7723(11) 0.8983(13) 0.079(11) Uiso 1 1 d G . . H22A H 0.5851 0.7636 0.8501 0.095 Uiso 1 1 calc R . . C23 C 0.5168(10) 0.7195(8) 0.9369(12) 0.045(7) Uiso 1 1 d GD . . H23A H 0.5229 0.6746 0.9150 0.054 Uiso 1 1 calc R . . C24 C 0.4518(16) 0.6759(17) 1.154(2) 0.059(8) Uiso 1 1 d . . . H24A H 0.4994 0.6614 1.1594 0.089 Uiso 1 1 calc R . . H24B H 0.4225 0.6449 1.1884 0.089 Uiso 1 1 calc R . . H24C H 0.4470 0.7218 1.1784 0.089 Uiso 1 1 calc R . . C25 C 0.2216(10) 0.4753(12) 0.8689(12) 0.031(5) Uiso 1 1 d D . . H25A H 0.2697 0.4752 0.8461 0.037 Uiso 1 1 calc R . . C26 C 0.2220(7) 0.4967(10) 0.9702(9) 0.041(6) Uiso 1 1 d G . . C27 C 0.1604(6) 0.5063(10) 1.0156(10) 0.036(6) Uiso 1 1 d GD . . H27A H 0.1187 0.4968 0.9852 0.044 Uiso 1 1 calc R . . C28 C 0.1599(7) 0.5299(10) 1.1056(10) 0.055(7) Uiso 1 1 d G . . H28A H 0.1179 0.5365 1.1366 0.065 Uiso 1 1 calc R . . C29 C 0.2210(9) 0.5438(10) 1.1502(9) 0.065(9) Uiso 1 1 d G . . H29A H 0.2207 0.5599 1.2116 0.078 Uiso 1 1 calc R . . C30 C 0.2826(7) 0.5342(11) 1.1048(11) 0.052(7) Uiso 1 1 d G . . H30A H 0.3243 0.5437 1.1352 0.062 Uiso 1 1 calc R . . C31 C 0.2831(6) 0.5106(11) 1.0148(11) 0.072(10) Uiso 1 1 d GD . . H31A H 0.3252 0.5041 0.9838 0.087 Uiso 1 1 calc R . . C32 C 0.1932(17) 0.4002(16) 0.864(2) 0.052(8) Uiso 1 1 d . . . H32A H 0.1982 0.3827 0.8018 0.078 Uiso 1 1 calc R . . H32B H 0.1448 0.4000 0.8815 0.078 Uiso 1 1 calc R . . H32C H 0.2188 0.3716 0.9071 0.078 Uiso 1 1 calc R . . C33 C 0.3258(10) 0.5719(11) 0.4564(16) 0.036(6) Uiso 1 1 d D . . H33A H 0.3663 0.5653 0.4971 0.043 Uiso 1 1 calc R . . C34 C 0.2733(7) 0.5230(8) 0.4994(11) 0.037(6) Uiso 1 1 d G . . C35 C 0.2047(8) 0.5253(9) 0.4757(12) 0.062(8) Uiso 1 1 d GD . . H35A H 0.1893 0.5567 0.4309 0.074 Uiso 1 1 calc R . . C36 C 0.1587(7) 0.4817(10) 0.5175(14) 0.060(8) Uiso 1 1 d G . . H36A H 0.1118 0.4832 0.5013 0.072 Uiso 1 1 calc R . . C37 C 0.1812(8) 0.4357(9) 0.5831(14) 0.056(8) Uiso 1 1 d G . . H37A H 0.1498 0.4059 0.6117 0.067 Uiso 1 1 calc R . . C38 C 0.2498(9) 0.4334(9) 0.6068(12) 0.073(10) Uiso 1 1 d G . . H38A H 0.2653 0.4020 0.6516 0.088 Uiso 1 1 calc R . . C39 C 0.2959(7) 0.4771(9) 0.5649(11) 0.042(6) Uiso 1 1 d GD . . H39A H 0.3428 0.4755 0.5811 0.050 Uiso 1 1 calc R . . C40 C 0.3557(16) 0.5527(16) 0.358(2) 0.058(8) Uiso 1 1 d . . . H40A H 0.3865 0.5886 0.3375 0.086 Uiso 1 1 calc R . . H40B H 0.3182 0.5477 0.3144 0.086 Uiso 1 1 calc R . . H40C H 0.3808 0.5100 0.3627 0.086 Uiso 1 1 calc R . . C41 C 0.5207(17) 0.7968(15) 0.6348(14) 0.067(9) Uiso 1 1 d D . . H41A H 0.5147 0.7474 0.6472 0.080 Uiso 1 1 calc R . . C42 C 0.5002(11) 0.8054(9) 0.5343(10) 0.047(6) Uiso 1 1 d G . . C43 C 0.4796(13) 0.7489(8) 0.4847(13) 0.073(10) Uiso 1 1 d GD . . H43A H 0.4782 0.7058 0.5135 0.087 Uiso 1 1 calc R . . C44 C 0.4609(13) 0.7555(11) 0.3930(13) 0.132(19) Uiso 1 1 d G . . H44A H 0.4469 0.7169 0.3591 0.158 Uiso 1 1 calc R . . C45 C 0.4629(12) 0.8186(13) 0.3509(10) 0.061(8) Uiso 1 1 d G . . H45A H 0.4502 0.8231 0.2883 0.074 Uiso 1 1 calc R . . C46 C 0.4835(14) 0.8751(10) 0.4005(13) 0.110(15) Uiso 1 1 d G . . H46A H 0.4849 0.9182 0.3717 0.132 Uiso 1 1 calc R . . C47 C 0.5021(13) 0.8685(8) 0.4922(13) 0.078(10) Uiso 1 1 d GD . . H47A H 0.5162 0.9071 0.5261 0.094 Uiso 1 1 calc R . . C48 C 0.595(2) 0.808(2) 0.639(3) 0.084(12) Uiso 1 1 d . . . H48A H 0.6050 0.8457 0.6796 0.126 Uiso 1 1 calc R . . H48B H 0.6120 0.8179 0.5768 0.126 Uiso 1 1 calc R . . H48C H 0.6173 0.7668 0.6617 0.126 Uiso 1 1 calc R . . I1 I 0.5000 1.0000 0.72084(18) 0.0787(11) Uani 1 2 d S . . I2 I 0.2621(3) 0.7333(3) 0.2574(3) 0.0356(10) Uani 0.75 1 d P . . I3 I 0.0022(2) 0.47562(17) 0.8192(2) 0.0445(9) Uani 0.50 1 d P . . I4 I 0.2713(9) 0.7294(8) 0.2475(14) 0.071(5) Uani 0.25 1 d P . . I5 I 0.5383(4) 0.6015(4) 0.4713(6) 0.054(2) Uani 0.25 1 d P . . I6 I 0.5000 0.5000 0.0556(9) 0.048(2) Uani 0.25 2 d SP . . I7 I 0.5000 0.5000 0.1128(7) 0.0367(19) Uani 0.25 2 d SP . . I8 I 0.5165(10) 0.5794(11) 0.5741(14) 0.075(5) Uiso 0.13 1 d P . . I9 I 0.5967(15) 0.6067(15) 0.264(2) 0.053(7) Uiso 0.06 1 d P . . I10 I 0.5410(19) 0.5113(19) -0.105(2) 0.059(9) Uiso 0.06 1 d P . . I11 I 0.2632(11) 0.6623(11) 0.2686(16) 0.032(5) Uiso 0.06 1 d P . . I12 I 0.6183(18) 0.6535(19) 0.735(3) 0.085(12) Uiso 0.06 1 d P . . I13 I 0.5271(18) 0.5897(18) 0.387(3) 0.062(9) Uiso 0.06 1 d P . . I14 I 0.523(2) 0.541(3) 0.612(3) 0.026(10) Uiso 0.03 1 d P . . I15 I 0.5000 0.5000 -0.068(3) 0.068(11) Uiso 0.06 2 d SP . . 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 0.0244(5) 0.0294(5) 0.0082(3) 0.0020(5) -0.0039(5) -0.0090(3) I1 0.141(3) 0.0485(17) 0.0472(15) 0.000 0.000 -0.049(2) I2 0.0419(17) 0.056(2) 0.0092(16) 0.0084(15) 0.0008(14) 0.0227(13) I3 0.0360(17) 0.066(3) 0.0320(13) -0.0093(13) -0.0012(16) -0.006(3) I4 0.092(11) 0.091(11) 0.029(5) -0.023(6) 0.006(6) -0.069(6) I5 0.036(4) 0.044(4) 0.082(6) 0.004(4) 0.011(4) -0.007(3) I6 0.019(5) 0.057(7) 0.068(7) 0.000 0.000 0.029(4) I7 0.036(6) 0.036(6) 0.038(5) 0.000 0.000 -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O4 2.213(17) . ? Yb1 O3 2.249(15) . ? Yb1 O2 2.270(15) . ? Yb1 O1 2.286(14) . ? Yb1 O1W 2.398(10) . ? Yb1 N4 2.562(17) . ? Yb1 N3 2.651(17) . ? Yb1 N2 2.655(18) . ? Yb1 N1 2.664(18) . ? Yb1 C16 3.14(3) . ? Yb1 C12 3.15(3) . ? Yb1 C14 3.16(2) . ? N1 C1 1.46(3) . ? N1 C8 1.48(3) . ? N1 C9 1.49(3) . ? N2 C2 1.39(3) . ? N2 C11 1.41(3) . ? N2 C3 1.45(3) . ? N3 C4 1.46(3) . ? N3 C13 1.48(3) . ? N3 C5 1.51(3) . ? N4 C7 1.43(3) . ? N4 C6 1.51(3) . ? N4 C15 1.54(3) . ? N5 C10 1.27(3) . ? N5 C17 1.51(3) . ? N5 H5A 0.8800 . ? N6 C12 1.30(3) . ? N6 C25 1.43(3) . ? N6 H6A 0.8800 . ? N7 C14 1.34(3) . ? N7 C33 1.42(3) . ? N7 H7A 0.8800 . ? N8 C41 1.32(4) . ? N8 C16 1.34(3) . ? N8 H8A 0.8800 . ? O1 C10 1.23(2) . ? O2 C12 1.23(3) . ? O3 C14 1.28(3) . ? O4 C16 1.29(3) . ? O1W H1WB 0.899(10) . ? O1W H1WA 0.900(10) . ? C1 C2 1.55(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.64(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.50(3) . ? C5 H5B 0.9900 . ? C5 H5C 0.9900 . ? C6 H6B 0.9900 . ? C6 H6C 0.9900 . ? C7 C8 1.53(3) . ? C7 H7B 0.9900 . ? C7 H7C 0.9900 . ? C8 H8B 0.9900 . ? C8 H8C 0.9900 . ? C9 C10 1.62(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.52(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 C14 1.44(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.52(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C18 1.519(16) . ? C17 C24 1.54(4) . ? C17 H17A 1.0000 . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C19 H19A 0.9500 . ? C20 C21 1.3900 . ? C20 H20A 0.9500 . ? C21 C22 1.3900 . ? C21 H21A 0.9500 . ? C22 C23 1.3900 . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.534(15) . ? C25 C32 1.59(4) . ? C25 H25A 1.0000 . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C27 H27A 0.9500 . ? C28 C29 1.3900 . ? C28 H28A 0.9500 . ? C29 C30 1.3900 . ? C29 H29A 0.9500 . ? C30 C31 1.3900 . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.543(15) . ? C33 C40 1.59(4) . ? C33 H33A 1.0000 . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C35 H35A 0.9500 . ? C36 C37 1.3900 . ? C36 H36A 0.9500 . ? C37 C38 1.3900 . ? C37 H37A 0.9500 . ? C38 C39 1.3900 . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C48 1.47(5) . ? C41 C42 1.527(16) . ? C41 H41A 1.0000 . ? C42 C43 1.3900 . ? C42 C47 1.3900 . ? C43 C44 1.3900 . ? C43 H43A 0.9500 . ? C44 C45 1.3900 . ? C44 H44A 0.9500 . ? C45 C46 1.3900 . ? C45 H45A 0.9500 . ? C46 C47 1.3900 . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? I2 I11 1.41(2) . ? I3 I3 0.968(7) 2_565 ? I4 I11 1.37(3) . ? I5 I13 1.27(4) . ? I5 I8 1.62(2) . ? I5 I14 2.38(4) . ? I6 I7 0.833(10) . ? I6 I15 1.80(5) . ? I6 I10 2.48(4) 2_665 ? I6 I10 2.48(4) . ? I7 I15 2.63(5) . ? I8 I14 0.93(5) . ? I8 I14 2.57(6) 2_665 ? I8 I13 2.74(4) . ? I9 I13 2.27(5) . ? I10 I15 0.99(4) . ? I10 I10 1.67(8) 2_665 ? I14 I14 1.86(9) 2_665 ? I14 I8 2.57(6) 2_665 ? I15 I10 0.99(4) 2_665 ? 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 O4 Yb1 O3 80.6(6) . . ? O4 Yb1 O2 141.9(4) . . ? O3 Yb1 O2 85.1(5) . . ? O4 Yb1 O1 86.7(6) . . ? O3 Yb1 O1 140.6(4) . . ? O2 Yb1 O1 82.4(5) . . ? O4 Yb1 O1W 70.8(6) . . ? O3 Yb1 O1W 72.3(6) . . ? O2 Yb1 O1W 71.2(6) . . ? O1 Yb1 O1W 68.3(6) . . ? O4 Yb1 N4 68.8(6) . . ? O3 Yb1 N4 131.8(5) . . ? O2 Yb1 N4 140.7(5) . . ? O1 Yb1 N4 75.0(6) . . ? O1W Yb1 N4 126.0(6) . . ? O4 Yb1 N3 73.0(6) . . ? O3 Yb1 N3 66.7(6) . . ? O2 Yb1 N3 131.9(5) . . ? O1 Yb1 N3 143.3(6) . . ? O1W Yb1 N3 128.5(6) . . ? N4 Yb1 N3 69.2(5) . . ? O4 Yb1 N2 140.1(6) . . ? O3 Yb1 N2 75.5(6) . . ? O2 Yb1 N2 67.2(5) . . ? O1 Yb1 N2 131.3(5) . . ? O1W Yb1 N2 128.8(6) . . ? N4 Yb1 N2 105.2(5) . . ? N3 Yb1 N2 68.3(5) . . ? O4 Yb1 N1 133.8(6) . . ? O3 Yb1 N1 142.6(6) . . ? O2 Yb1 N1 74.2(5) . . ? O1 Yb1 N1 67.7(5) . . ? O1W Yb1 N1 126.5(6) . . ? N4 Yb1 N1 67.7(5) . . ? N3 Yb1 N1 105.0(4) . . ? N2 Yb1 N1 67.9(5) . . ? O4 Yb1 C16 19.4(6) . . ? O3 Yb1 C16 98.5(6) . . ? O2 Yb1 C16 152.0(6) . . ? O1 Yb1 C16 77.3(6) . . ? O1W Yb1 C16 83.4(7) . . ? N4 Yb1 C16 50.2(6) . . ? N3 Yb1 C16 73.6(6) . . ? N2 Yb1 C16 140.6(6) . . ? N1 Yb1 C16 114.4(6) . . ? O4 Yb1 C12 151.7(7) . . ? O3 Yb1 C12 77.7(6) . . ? O2 Yb1 C12 18.6(6) . . ? O1 Yb1 C12 98.8(6) . . ? O1W Yb1 C12 85.4(7) . . ? N4 Yb1 C12 139.4(6) . . ? N3 Yb1 C12 113.7(6) . . ? N2 Yb1 C12 49.1(6) . . ? N1 Yb1 C12 72.9(6) . . ? C16 Yb1 C12 168.8(6) . . ? O4 Yb1 C14 70.8(7) . . ? O3 Yb1 C14 19.4(6) . . ? O2 Yb1 C14 103.1(6) . . ? O1 Yb1 C14 150.1(6) . . ? O1W Yb1 C14 85.4(6) . . ? N4 Yb1 C14 112.6(6) . . ? N3 Yb1 C14 48.3(6) . . ? N2 Yb1 C14 76.3(7) . . ? N1 Yb1 C14 142.2(7) . . ? C16 Yb1 C14 85.9(7) . . ? C12 Yb1 C14 92.9(7) . . ? C1 N1 C8 111(2) . . ? C1 N1 C9 109.5(19) . . ? C8 N1 C9 107.6(18) . . ? C1 N1 Yb1 111.6(14) . . ? C8 N1 Yb1 109.8(13) . . ? C9 N1 Yb1 107.7(14) . . ? C2 N2 C11 111(2) . . ? C2 N2 C3 109.5(19) . . ? C11 N2 C3 109(2) . . ? C2 N2 Yb1 110.7(12) . . ? C11 N2 Yb1 103.6(16) . . ? C3 N2 Yb1 112.8(15) . . ? C4 N3 C13 110.4(19) . . ? C4 N3 C5 106.1(18) . . ? C13 N3 C5 110.4(18) . . ? C4 N3 Yb1 113.8(14) . . ? C13 N3 Yb1 105.2(14) . . ? C5 N3 Yb1 111.0(13) . . ? C7 N4 C6 107.0(16) . . ? C7 N4 C15 108.6(16) . . ? C6 N4 C15 104.7(15) . . ? C7 N4 Yb1 115.4(12) . . ? C6 N4 Yb1 112.9(11) . . ? C15 N4 Yb1 107.7(12) . . ? C10 N5 C17 120(2) . . ? C10 N5 H5A 120.0 . . ? C17 N5 H5A 120.0 . . ? C12 N6 C25 118(2) . . ? C12 N6 H6A 120.9 . . ? C25 N6 H6A 120.9 . . ? C14 N7 C33 124(2) . . ? C14 N7 H7A 117.9 . . ? C33 N7 H7A 117.9 . . ? C41 N8 C16 127(2) . . ? C41 N8 H8A 116.7 . . ? C16 N8 H8A 116.7 . . ? C10 O1 Yb1 128.2(14) . . ? C12 O2 Yb1 125.5(16) . . ? C14 O3 Yb1 124.9(15) . . ? C16 O4 Yb1 125.8(16) . . ? Yb1 O1W H1WB 122(10) . . ? Yb1 O1W H1WA 142(10) . . ? H1WB O1W H1WA 95.3(14) . . ? N1 C1 C2 110(2) . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N2 C2 C1 117.6(19) . . ? N2 C2 H2A 107.9 . . ? C1 C2 H2A 107.9 . . ? N2 C2 H2B 107.9 . . ? C1 C2 H2B 107.9 . . ? H2A C2 H2B 107.2 . . ? N2 C3 C4 112(2) . . ? N2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C3 111(2) . . ? N3 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N3 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C6 C5 N3 111.5(19) . . ? C6 C5 H5B 109.3 . . ? N3 C5 H5B 109.3 . . ? C6 C5 H5C 109.3 . . ? N3 C5 H5C 109.3 . . ? H5B C5 H5C 108.0 . . ? C5 C6 N4 115.1(17) . . ? C5 C6 H6B 108.5 . . ? N4 C6 H6B 108.5 . . ? C5 C6 H6C 108.5 . . ? N4 C6 H6C 108.5 . . ? H6B C6 H6C 107.5 . . ? N4 C7 C8 110.4(18) . . ? N4 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? N4 C7 H7C 109.6 . . ? C8 C7 H7C 109.6 . . ? H7B C7 H7C 108.1 . . ? N1 C8 C7 114(2) . . ? N1 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? N1 C8 H8C 108.8 . . ? C7 C8 H8C 108.8 . . ? H8B C8 H8C 107.7 . . ? N1 C9 C10 110.5(19) . . ? N1 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? N1 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? O1 C10 N5 127(2) . . ? O1 C10 C9 117.8(18) . . ? N5 C10 C9 115.3(18) . . ? O1 C10 Yb1 34.2(10) . . ? N5 C10 Yb1 160.8(16) . . ? C9 C10 Yb1 83.7(11) . . ? N2 C11 C12 113(2) . . ? N2 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? N2 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? O2 C12 N6 125(2) . . ? O2 C12 C11 117(2) . . ? N6 C12 C11 117(3) . . ? O2 C12 Yb1 35.9(11) . . ? N6 C12 Yb1 161(2) . . ? C11 C12 Yb1 81.5(16) . . ? C14 C13 N3 112(2) . . ? C14 C13 H13A 109.2 . . ? N3 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? N3 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? O3 C14 N7 120(2) . . ? O3 C14 C13 121(2) . . ? N7 C14 C13 119(2) . . ? O3 C14 Yb1 35.7(11) . . ? N7 C14 Yb1 154.7(18) . . ? C13 C14 Yb1 85.1(14) . . ? C16 C15 N4 108.2(18) . . ? C16 C15 H15A 110.1 . . ? N4 C15 H15A 110.1 . . ? C16 C15 H15B 110.1 . . ? N4 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? O4 C16 N8 124(2) . . ? O4 C16 C15 120(2) . . ? N8 C16 C15 117(2) . . ? O4 C16 Yb1 34.8(11) . . ? N8 C16 Yb1 158.4(19) . . ? C15 C16 Yb1 84.7(14) . . ? N5 C17 C18 103.8(18) . . ? N5 C17 C24 108(2) . . ? C18 C17 C24 105(2) . . ? N5 C17 H17A 112.9 . . ? C18 C17 H17A 112.9 . . ? C24 C17 H17A 112.9 . . ? C19 C18 C23 120.0 . . ? C19 C18 C17 118.9(7) . . ? C23 C18 C17 121.1(7) . . ? C18 C19 C20 120.0 . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 H23A 120.0 . . ? C18 C23 H23A 120.0 . . ? C17 C24 H24A 109.5 . . ? C17 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C17 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C25 C26 118.3(17) . . ? N6 C25 C32 105.7(19) . . ? C26 C25 C32 107.4(18) . . ? N6 C25 H25A 108.4 . . ? C26 C25 H25A 108.4 . . ? C32 C25 H25A 108.4 . . ? C27 C26 C31 120.0 . . ? C27 C26 C25 119.4(7) . . ? C31 C26 C25 120.5(7) . . ? C28 C27 C26 120.0 . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 H31A 120.0 . . ? C26 C31 H31A 120.0 . . ? C25 C32 H32A 109.5 . . ? C25 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C25 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N7 C33 C34 121.4(19) . . ? N7 C33 C40 108.4(19) . . ? C34 C33 C40 117(2) . . ? N7 C33 H33A 102.0 . . ? C34 C33 H33A 102.0 . . ? C40 C33 H33A 102.0 . . ? C35 C34 C39 120.0 . . ? C35 C34 C33 121.6(7) . . ? C39 C34 C33 118.3(7) . . ? C36 C35 C34 120.0 . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 H37A 120.0 . . ? C38 C37 H37A 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C38 C39 C34 120.0 . . ? C38 C39 H39A 120.0 . . ? C34 C39 H39A 120.0 . . ? C33 C40 H40A 109.5 . . ? C33 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C33 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N8 C41 C48 122(3) . . ? N8 C41 C42 113(2) . . ? C48 C41 C42 106(3) . . ? N8 C41 H41A 104.6 . . ? C48 C41 H41A 104.6 . . ? C42 C41 H41A 104.6 . . ? C43 C42 C47 120.0 . . ? C43 C42 C41 119.0(7) . . ? C47 C42 C41 121.0(7) . . ? C44 C43 C42 120.0 . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45A 120.0 . . ? C44 C45 H45A 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46A 120.0 . . ? C47 C46 H46A 120.0 . . ? C46 C47 C42 120.0 . . ? C46 C47 H47A 120.0 . . ? C42 C47 H47A 120.0 . . ? C41 C48 H48A 109.5 . . ? C41 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C41 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? I13 I5 I8 143.1(18) . . ? I13 I5 I14 136(2) . . ? I8 I5 I14 15.7(13) . . ? I7 I6 I15 180.000(12) . . ? I7 I6 I10 160.4(9) . 2_665 ? I15 I6 I10 19.6(9) . 2_665 ? I7 I6 I10 160.4(9) . . ? I15 I6 I10 19.6(9) . . ? I10 I6 I10 39.3(17) 2_665 . ? I6 I7 I15 0.000(6) . . ? I14 I8 I5 136(3) . . ? I14 I8 I14 34(3) . 2_665 ? I5 I8 I14 121.8(15) . 2_665 ? I14 I8 I13 129(3) . . ? I5 I8 I13 16.1(9) . . ? I14 I8 I13 107.7(15) 2_665 . ? I15 I10 I10 33(3) . 2_665 ? I15 I10 I6 38(3) . . ? I10 I10 I6 70.4(9) 2_665 . ? I4 I11 I2 9.9(9) . . ? I5 I13 I9 129(2) . . ? I5 I13 I8 20.7(11) . . ? I9 I13 I8 147.0(18) . . ? I8 I14 I14 130(4) . 2_665 ? I8 I14 I5 28(2) . . ? I14 I14 I5 120.0(12) 2_665 . ? I8 I14 I8 126(4) . 2_665 ? I14 I14 I8 16.1(15) 2_665 2_665 ? I5 I14 I8 108.6(17) . 2_665 ? I10 I15 I10 114(6) 2_665 . ? I10 I15 I6 123(3) 2_665 . ? I10 I15 I6 123(3) . . ? I10 I15 I7 123(3) 2_665 . ? I10 I15 I7 123(3) . . ? I6 I15 I7 0.000(1) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Yb1 N1 C1 155.5(16) . . . . ? O3 Yb1 N1 C1 4(2) . . . . ? O2 Yb1 N1 C1 -55.1(16) . . . . ? O1 Yb1 N1 C1 -143.2(18) . . . . ? O1W Yb1 N1 C1 -106.4(17) . . . . ? N4 Yb1 N1 C1 134.5(18) . . . . ? N3 Yb1 N1 C1 74.9(17) . . . . ? N2 Yb1 N1 C1 16.3(16) . . . . ? C16 Yb1 N1 C1 153.3(16) . . . . ? C12 Yb1 N1 C1 -35.8(17) . . . . ? C14 Yb1 N1 C1 36(2) . . . . ? O4 Yb1 N1 C8 32.5(17) . . . . ? O3 Yb1 N1 C8 -119.1(15) . . . . ? O2 Yb1 N1 C8 -178.0(15) . . . . ? O1 Yb1 N1 C8 93.9(15) . . . . ? O1W Yb1 N1 C8 130.7(14) . . . . ? N4 Yb1 N1 C8 11.5(13) . . . . ? N3 Yb1 N1 C8 -48.1(15) . . . . ? N2 Yb1 N1 C8 -106.6(15) . . . . ? C16 Yb1 N1 C8 30.4(16) . . . . ? C12 Yb1 N1 C8 -158.7(15) . . . . ? C14 Yb1 N1 C8 -87.0(17) . . . . ? O4 Yb1 N1 C9 -84.4(17) . . . . ? O3 Yb1 N1 C9 124.0(15) . . . . ? O2 Yb1 N1 C9 65.1(15) . . . . ? O1 Yb1 N1 C9 -23.1(15) . . . . ? O1W Yb1 N1 C9 13.8(17) . . . . ? N4 Yb1 N1 C9 -105.4(16) . . . . ? N3 Yb1 N1 C9 -165.0(14) . . . . ? N2 Yb1 N1 C9 136.4(16) . . . . ? C16 Yb1 N1 C9 -86.5(16) . . . . ? C12 Yb1 N1 C9 84.4(16) . . . . ? C14 Yb1 N1 C9 156.1(15) . . . . ? O4 Yb1 N2 C2 -121.0(14) . . . . ? O3 Yb1 N2 C2 -176.2(14) . . . . ? O2 Yb1 N2 C2 93.1(14) . . . . ? O1 Yb1 N2 C2 37.1(16) . . . . ? O1W Yb1 N2 C2 131.4(13) . . . . ? N4 Yb1 N2 C2 -46.1(14) . . . . ? N3 Yb1 N2 C2 -105.9(14) . . . . ? N1 Yb1 N2 C2 11.6(13) . . . . ? C16 Yb1 N2 C2 -90.4(16) . . . . ? C12 Yb1 N2 C2 97.7(15) . . . . ? C14 Yb1 N2 C2 -156.2(15) . . . . ? O4 Yb1 N2 C11 120.0(16) . . . . ? O3 Yb1 N2 C11 64.8(15) . . . . ? O2 Yb1 N2 C11 -26.0(15) . . . . ? O1 Yb1 N2 C11 -81.9(16) . . . . ? O1W Yb1 N2 C11 12.4(17) . . . . ? N4 Yb1 N2 C11 -165.1(14) . . . . ? N3 Yb1 N2 C11 135.1(16) . . . . ? N1 Yb1 N2 C11 -107.4(16) . . . . ? C16 Yb1 N2 C11 150.6(15) . . . . ? C12 Yb1 N2 C11 -21.3(15) . . . . ? C14 Yb1 N2 C11 84.8(16) . . . . ? O4 Yb1 N2 C3 2(2) . . . . ? O3 Yb1 N2 C3 -53.1(16) . . . . ? O2 Yb1 N2 C3 -143.9(17) . . . . ? O1 Yb1 N2 C3 160.2(16) . . . . ? O1W Yb1 N2 C3 -105.6(17) . . . . ? N4 Yb1 N2 C3 77.0(17) . . . . ? N3 Yb1 N2 C3 17.1(16) . . . . ? N1 Yb1 N2 C3 134.6(17) . . . . ? C16 Yb1 N2 C3 33(2) . . . . ? C12 Yb1 N2 C3 -139.3(19) . . . . ? C14 Yb1 N2 C3 -33.1(17) . . . . ? O4 Yb1 N3 C4 -177.7(16) . . . . ? O3 Yb1 N3 C4 95.4(16) . . . . ? O2 Yb1 N3 C4 36.1(18) . . . . ? O1 Yb1 N3 C4 -118.5(15) . . . . ? O1W Yb1 N3 C4 135.4(15) . . . . ? N4 Yb1 N3 C4 -104.4(16) . . . . ? N2 Yb1 N3 C4 12.4(15) . . . . ? N1 Yb1 N3 C4 -45.9(17) . . . . ? C16 Yb1 N3 C4 -157.4(17) . . . . ? C12 Yb1 N3 C4 31.7(17) . . . . ? C14 Yb1 N3 C4 103.1(17) . . . . ? O4 Yb1 N3 C13 61.4(14) . . . . ? O3 Yb1 N3 C13 -25.5(14) . . . . ? O2 Yb1 N3 C13 -84.8(15) . . . . ? O1 Yb1 N3 C13 120.5(15) . . . . ? O1W Yb1 N3 C13 14.5(17) . . . . ? N4 Yb1 N3 C13 134.6(15) . . . . ? N2 Yb1 N3 C13 -108.6(15) . . . . ? N1 Yb1 N3 C13 -166.8(13) . . . . ? C16 Yb1 N3 C13 81.6(15) . . . . ? C12 Yb1 N3 C13 -89.3(15) . . . . ? C14 Yb1 N3 C13 -17.8(15) . . . . ? O4 Yb1 N3 C5 -58.1(14) . . . . ? O3 Yb1 N3 C5 -145.0(15) . . . . ? O2 Yb1 N3 C5 155.7(13) . . . . ? O1 Yb1 N3 C5 1.1(18) . . . . ? O1W Yb1 N3 C5 -105.0(15) . . . . ? N4 Yb1 N3 C5 15.1(13) . . . . ? N2 Yb1 N3 C5 132.0(15) . . . . ? N1 Yb1 N3 C5 73.7(15) . . . . ? C16 Yb1 N3 C5 -37.8(14) . . . . ? C12 Yb1 N3 C5 151.2(14) . . . . ? C14 Yb1 N3 C5 -137.3(17) . . . . ? O4 Yb1 N4 C7 -146.6(15) . . . . ? O3 Yb1 N4 C7 159.0(13) . . . . ? O2 Yb1 N4 C7 2.6(18) . . . . ? O1 Yb1 N4 C7 -54.4(14) . . . . ? O1W Yb1 N4 C7 -102.5(14) . . . . ? N3 Yb1 N4 C7 134.3(15) . . . . ? N2 Yb1 N4 C7 75.0(14) . . . . ? N1 Yb1 N4 C7 17.3(13) . . . . ? C16 Yb1 N4 C7 -140.2(17) . . . . ? C12 Yb1 N4 C7 31.7(18) . . . . ? C14 Yb1 N4 C7 156.3(14) . . . . ? O4 Yb1 N4 C6 89.8(12) . . . . ? O3 Yb1 N4 C6 35.5(15) . . . . ? O2 Yb1 N4 C6 -120.9(12) . . . . ? O1 Yb1 N4 C6 -177.9(13) . . . . ? O1W Yb1 N4 C6 133.9(12) . . . . ? N3 Yb1 N4 C6 10.7(11) . . . . ? N2 Yb1 N4 C6 -48.5(13) . . . . ? N1 Yb1 N4 C6 -106.3(13) . . . . ? C16 Yb1 N4 C6 96.2(13) . . . . ? C12 Yb1 N4 C6 -91.9(14) . . . . ? C14 Yb1 N4 C6 32.7(14) . . . . ? O4 Yb1 N4 C15 -25.2(12) . . . . ? O3 Yb1 N4 C15 -79.5(14) . . . . ? O2 Yb1 N4 C15 124.1(12) . . . . ? O1 Yb1 N4 C15 67.0(12) . . . . ? O1W Yb1 N4 C15 18.9(14) . . . . ? N3 Yb1 N4 C15 -104.3(12) . . . . ? N2 Yb1 N4 C15 -163.5(11) . . . . ? N1 Yb1 N4 C15 138.7(13) . . . . ? C16 Yb1 N4 C15 -18.8(11) . . . . ? C12 Yb1 N4 C15 153.1(12) . . . . ? C14 Yb1 N4 C15 -82.3(13) . . . . ? O4 Yb1 O1 C10 155(2) . . . . ? O3 Yb1 O1 C10 -134.4(18) . . . . ? O2 Yb1 O1 C10 -62(2) . . . . ? O1W Yb1 O1 C10 -135(2) . . . . ? N4 Yb1 O1 C10 86(2) . . . . ? N3 Yb1 O1 C10 100(2) . . . . ? N2 Yb1 O1 C10 -11(2) . . . . ? N1 Yb1 O1 C10 14.2(19) . . . . ? C16 Yb1 O1 C10 138(2) . . . . ? C12 Yb1 O1 C10 -53(2) . . . . ? C14 Yb1 O1 C10 -165(2) . . . . ? O4 Yb1 O2 C12 -133.3(18) . . . . ? O3 Yb1 O2 C12 -65.3(19) . . . . ? O1 Yb1 O2 C12 152.1(19) . . . . ? O1W Yb1 O2 C12 -138.3(19) . . . . ? N4 Yb1 O2 C12 97(2) . . . . ? N3 Yb1 O2 C12 -13(2) . . . . ? N2 Yb1 O2 C12 11.0(18) . . . . ? N1 Yb1 O2 C12 83.2(19) . . . . ? C16 Yb1 O2 C12 -164(2) . . . . ? C14 Yb1 O2 C12 -58(2) . . . . ? O4 Yb1 O3 C14 -58(2) . . . . ? O2 Yb1 O3 C14 158(2) . . . . ? O1 Yb1 O3 C14 -131(2) . . . . ? O1W Yb1 O3 C14 -131(2) . . . . ? N4 Yb1 O3 C14 -8(2) . . . . ? N3 Yb1 O3 C14 18(2) . . . . ? N2 Yb1 O3 C14 90(2) . . . . ? N1 Yb1 O3 C14 102(2) . . . . ? C16 Yb1 O3 C14 -50(2) . . . . ? C12 Yb1 O3 C14 140(2) . . . . ? O3 Yb1 O4 C16 157(2) . . . . ? O2 Yb1 O4 C16 -133.4(18) . . . . ? O1 Yb1 O4 C16 -60(2) . . . . ? O1W Yb1 O4 C16 -128(2) . . . . ? N4 Yb1 O4 C16 15.0(19) . . . . ? N3 Yb1 O4 C16 89(2) . . . . ? N2 Yb1 O4 C16 103(2) . . . . ? N1 Yb1 O4 C16 -6(2) . . . . ? C12 Yb1 O4 C16 -163(2) . . . . ? C14 Yb1 O4 C16 140(2) . . . . ? C8 N1 C1 C2 82(2) . . . . ? C9 N1 C1 C2 -159(2) . . . . ? Yb1 N1 C1 C2 -40(3) . . . . ? C11 N2 C2 C1 75(3) . . . . ? C3 N2 C2 C1 -164.3(19) . . . . ? Yb1 N2 C2 C1 -39(2) . . . . ? N1 C1 C2 N2 57(3) . . . . ? C2 N2 C3 C4 82(2) . . . . ? C11 N2 C3 C4 -157(2) . . . . ? Yb1 N2 C3 C4 -42(2) . . . . ? C13 N3 C4 C3 81(2) . . . . ? C5 N3 C4 C3 -159.6(19) . . . . ? Yb1 N3 C4 C3 -37(2) . . . . ? N2 C3 C4 N3 54(3) . . . . ? C4 N3 C5 C6 84(2) . . . . ? C13 N3 C5 C6 -156.1(19) . . . . ? Yb1 N3 C5 C6 -40(2) . . . . ? N3 C5 C6 N4 53(2) . . . . ? C7 N4 C6 C5 -165.7(17) . . . . ? C15 N4 C6 C5 79(2) . . . . ? Yb1 N4 C6 C5 -38(2) . . . . ? C6 N4 C7 C8 83(2) . . . . ? C15 N4 C7 C8 -164.2(18) . . . . ? Yb1 N4 C7 C8 -43(2) . . . . ? C1 N1 C8 C7 -162.0(18) . . . . ? C9 N1 C8 C7 78(2) . . . . ? Yb1 N1 C8 C7 -38(2) . . . . ? N4 C7 C8 N1 56(2) . . . . ? C1 N1 C9 C10 151(2) . . . . ? C8 N1 C9 C10 -89(2) . . . . ? Yb1 N1 C9 C10 29(2) . . . . ? Yb1 O1 C10 N5 -177.3(19) . . . . ? Yb1 O1 C10 C9 -2(3) . . . . ? C17 N5 C10 O1 -23(4) . . . . ? C17 N5 C10 C9 162(2) . . . . ? C17 N5 C10 Yb1 -28(7) . . . . ? N1 C9 C10 O1 -22(3) . . . . ? N1 C9 C10 N5 154(2) . . . . ? N1 C9 C10 Yb1 -23.0(18) . . . . ? O4 Yb1 C10 O1 -26(2) . . . . ? O3 Yb1 C10 O1 67(2) . . . . ? O2 Yb1 C10 O1 115(2) . . . . ? O1W Yb1 C10 O1 42(2) . . . . ? N4 Yb1 C10 O1 -89(2) . . . . ? N3 Yb1 C10 O1 -104(2) . . . . ? N2 Yb1 C10 O1 170.7(19) . . . . ? N1 Yb1 C10 O1 -163(2) . . . . ? C16 Yb1 C10 O1 -41(2) . . . . ? C12 Yb1 C10 O1 128(2) . . . . ? C14 Yb1 C10 O1 34(5) . . . . ? O4 Yb1 C10 N5 -19(6) . . . . ? O3 Yb1 C10 N5 74(6) . . . . ? O2 Yb1 C10 N5 122(6) . . . . ? O1 Yb1 C10 N5 7(5) . . . . ? O1W Yb1 C10 N5 49(6) . . . . ? N4 Yb1 C10 N5 -83(6) . . . . ? N3 Yb1 C10 N5 -97(5) . . . . ? N2 Yb1 C10 N5 177(5) . . . . ? N1 Yb1 C10 N5 -156(6) . . . . ? C16 Yb1 C10 N5 -34(6) . . . . ? C12 Yb1 C10 N5 134(6) . . . . ? C14 Yb1 C10 N5 40(8) . . . . ? O4 Yb1 C10 C9 152.4(14) . . . . ? O3 Yb1 C10 C9 -114.4(16) . . . . ? O2 Yb1 C10 C9 -66.8(14) . . . . ? O1 Yb1 C10 C9 178(3) . . . . ? O1W Yb1 C10 C9 -139.6(15) . . . . ? N4 Yb1 C10 C9 89.0(14) . . . . ? N3 Yb1 C10 C9 74.1(17) . . . . ? N2 Yb1 C10 C9 -11.1(16) . . . . ? N1 Yb1 C10 C9 15.3(13) . . . . ? C16 Yb1 C10 C9 137.1(14) . . . . ? C12 Yb1 C10 C9 -54.0(15) . . . . ? C14 Yb1 C10 C9 -148(3) . . . . ? C2 N2 C11 C12 -81(3) . . . . ? C3 N2 C11 C12 159(2) . . . . ? Yb1 N2 C11 C12 38(2) . . . . ? Yb1 O2 C12 N6 175.5(19) . . . . ? Yb1 O2 C12 C11 7(3) . . . . ? C25 N6 C12 O2 4(4) . . . . ? C25 N6 C12 C11 172(2) . . . . ? C25 N6 C12 Yb1 12(7) . . . . ? N2 C11 C12 O2 -35(3) . . . . ? N2 C11 C12 N6 155(2) . . . . ? N2 C11 C12 Yb1 -31(2) . . . . ? O4 Yb1 C12 O2 71(2) . . . . ? O3 Yb1 C12 O2 112.1(19) . . . . ? O1 Yb1 C12 O2 -28.0(19) . . . . ? O1W Yb1 C12 O2 39.2(18) . . . . ? N4 Yb1 C12 O2 -105.2(19) . . . . ? N3 Yb1 C12 O2 169.5(17) . . . . ? N2 Yb1 C12 O2 -167(2) . . . . ? N1 Yb1 C12 O2 -91.3(19) . . . . ? C16 Yb1 C12 O2 41(5) . . . . ? C14 Yb1 C12 O2 124.3(19) . . . . ? O4 Yb1 C12 N6 60(6) . . . . ? O3 Yb1 C12 N6 101(6) . . . . ? O2 Yb1 C12 N6 -11(5) . . . . ? O1 Yb1 C12 N6 -39(6) . . . . ? O1W Yb1 C12 N6 28(6) . . . . ? N4 Yb1 C12 N6 -116(5) . . . . ? N3 Yb1 C12 N6 158(5) . . . . ? N2 Yb1 C12 N6 -178(6) . . . . ? N1 Yb1 C12 N6 -102(6) . . . . ? C16 Yb1 C12 N6 30(9) . . . . ? C14 Yb1 C12 N6 113(6) . . . . ? O4 Yb1 C12 C11 -102.6(18) . . . . ? O3 Yb1 C12 C11 -62.0(15) . . . . ? O2 Yb1 C12 C11 -174(3) . . . . ? O1 Yb1 C12 C11 158.0(15) . . . . ? O1W Yb1 C12 C11 -134.9(15) . . . . ? N4 Yb1 C12 C11 80.7(17) . . . . ? N3 Yb1 C12 C11 -4.5(16) . . . . ? N2 Yb1 C12 C11 19.4(14) . . . . ? N1 Yb1 C12 C11 94.7(15) . . . . ? C16 Yb1 C12 C11 -133(4) . . . . ? C14 Yb1 C12 C11 -49.7(15) . . . . ? C4 N3 C13 C14 -90(3) . . . . ? C5 N3 C13 C14 153(2) . . . . ? Yb1 N3 C13 C14 33(2) . . . . ? Yb1 O3 C14 N7 171.4(18) . . . . ? Yb1 O3 C14 C13 -5(4) . . . . ? C33 N7 C14 O3 3(4) . . . . ? C33 N7 C14 C13 179(2) . . . . ? C33 N7 C14 Yb1 14(6) . . . . ? N3 C13 C14 O3 -23(4) . . . . ? N3 C13 C14 N7 161(2) . . . . ? N3 C13 C14 Yb1 -26(2) . . . . ? O4 Yb1 C14 O3 118(2) . . . . ? O2 Yb1 C14 O3 -23(2) . . . . ? O1 Yb1 C14 O3 75(2) . . . . ? O1W Yb1 C14 O3 47(2) . . . . ? N4 Yb1 C14 O3 173.8(19) . . . . ? N3 Yb1 C14 O3 -158(2) . . . . ? N2 Yb1 C14 O3 -85(2) . . . . ? N1 Yb1 C14 O3 -104(2) . . . . ? C16 Yb1 C14 O3 130(2) . . . . ? C12 Yb1 C14 O3 -39(2) . . . . ? O4 Yb1 C14 N7 100(5) . . . . ? O3 Yb1 C14 N7 -18(4) . . . . ? O2 Yb1 C14 N7 -41(5) . . . . ? O1 Yb1 C14 N7 57(5) . . . . ? O1W Yb1 C14 N7 29(5) . . . . ? N4 Yb1 C14 N7 156(4) . . . . ? N3 Yb1 C14 N7 -176(5) . . . . ? N2 Yb1 C14 N7 -103(5) . . . . ? N1 Yb1 C14 N7 -122(4) . . . . ? C16 Yb1 C14 N7 113(5) . . . . ? C12 Yb1 C14 N7 -56(5) . . . . ? O4 Yb1 C14 C13 -66.2(17) . . . . ? O3 Yb1 C14 C13 176(3) . . . . ? O2 Yb1 C14 C13 153.0(16) . . . . ? O1 Yb1 C14 C13 -109.5(18) . . . . ? O1W Yb1 C14 C13 -137.5(18) . . . . ? N4 Yb1 C14 C13 -10.2(19) . . . . ? N3 Yb1 C14 C13 17.7(15) . . . . ? N2 Yb1 C14 C13 90.8(17) . . . . ? N1 Yb1 C14 C13 72(2) . . . . ? C16 Yb1 C14 C13 -53.8(17) . . . . ? C12 Yb1 C14 C13 137.4(17) . . . . ? C7 N4 C15 C16 158.2(19) . . . . ? C6 N4 C15 C16 -88(2) . . . . ? Yb1 N4 C15 C16 32.6(19) . . . . ? Yb1 O4 C16 N8 177.2(17) . . . . ? Yb1 O4 C16 C15 0(3) . . . . ? C41 N8 C16 O4 -5(4) . . . . ? C41 N8 C16 C15 172(2) . . . . ? C41 N8 C16 Yb1 -1(6) . . . . ? N4 C15 C16 O4 -25(3) . . . . ? N4 C15 C16 N8 158(2) . . . . ? N4 C15 C16 Yb1 -24.8(15) . . . . ? O3 Yb1 C16 O4 -23(2) . . . . ? O2 Yb1 C16 O4 73(2) . . . . ? O1 Yb1 C16 O4 117(2) . . . . ? O1W Yb1 C16 O4 48.1(19) . . . . ? N4 Yb1 C16 O4 -162(2) . . . . ? N3 Yb1 C16 O4 -85.3(19) . . . . ? N2 Yb1 C16 O4 -100(2) . . . . ? N1 Yb1 C16 O4 175.4(18) . . . . ? C12 Yb1 C16 O4 47(5) . . . . ? C14 Yb1 C16 O4 -38(2) . . . . ? O4 Yb1 C16 N8 -6(4) . . . . ? O3 Yb1 C16 N8 -29(5) . . . . ? O2 Yb1 C16 N8 67(5) . . . . ? O1 Yb1 C16 N8 111(5) . . . . ? O1W Yb1 C16 N8 42(5) . . . . ? N4 Yb1 C16 N8 -168(5) . . . . ? N3 Yb1 C16 N8 -92(5) . . . . ? N2 Yb1 C16 N8 -107(5) . . . . ? N1 Yb1 C16 N8 169(5) . . . . ? C12 Yb1 C16 N8 40(8) . . . . ? C14 Yb1 C16 N8 -44(5) . . . . ? O4 Yb1 C16 C15 180(3) . . . . ? O3 Yb1 C16 C15 157.0(13) . . . . ? O2 Yb1 C16 C15 -107.3(16) . . . . ? O1 Yb1 C16 C15 -62.8(13) . . . . ? O1W Yb1 C16 C15 -132.0(14) . . . . ? N4 Yb1 C16 C15 18.1(11) . . . . ? N3 Yb1 C16 C15 94.5(14) . . . . ? N2 Yb1 C16 C15 79.5(16) . . . . ? N1 Yb1 C16 C15 -4.8(15) . . . . ? C12 Yb1 C16 C15 -134(4) . . . . ? C14 Yb1 C16 C15 142.2(14) . . . . ? C10 N5 C17 C18 74(2) . . . . ? C10 N5 C17 C24 -174(2) . . . . ? N5 C17 C18 C19 54(2) . . . . ? C24 C17 C18 C19 -60(2) . . . . ? N5 C17 C18 C23 -127.1(16) . . . . ? C24 C17 C18 C23 119(2) . . . . ? C23 C18 C19 C20 0.0 . . . . ? C17 C18 C19 C20 179(2) . . . . ? C18 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C18 0.0 . . . . ? C19 C18 C23 C22 0.0 . . . . ? C17 C18 C23 C22 -179(2) . . . . ? C12 N6 C25 C26 75(3) . . . . ? C12 N6 C25 C32 -165(2) . . . . ? N6 C25 C26 C27 51(2) . . . . ? C32 C25 C26 C27 -69(2) . . . . ? N6 C25 C26 C31 -125.0(17) . . . . ? C32 C25 C26 C31 115.6(18) . . . . ? C31 C26 C27 C28 0.0 . . . . ? C25 C26 C27 C28 -175.9(19) . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C26 0.0 . . . . ? C27 C26 C31 C30 0.0 . . . . ? C25 C26 C31 C30 176(2) . . . . ? C14 N7 C33 C34 53(3) . . . . ? C14 N7 C33 C40 -166(2) . . . . ? N7 C33 C34 C35 55(3) . . . . ? C40 C33 C34 C35 -82(2) . . . . ? N7 C33 C34 C39 -123.6(19) . . . . ? C40 C33 C34 C39 99(2) . . . . ? C39 C34 C35 C36 0.0 . . . . ? C33 C34 C35 C36 -178(2) . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C34 0.0 . . . . ? C35 C34 C39 C38 0.0 . . . . ? C33 C34 C39 C38 178.5(19) . . . . ? C16 N8 C41 C48 -147(3) . . . . ? C16 N8 C41 C42 84(3) . . . . ? N8 C41 C42 C43 -113(2) . . . . ? C48 C41 C42 C43 110(3) . . . . ? N8 C41 C42 C47 67(3) . . . . ? C48 C41 C42 C47 -70(3) . . . . ? C47 C42 C43 C44 0.0 . . . . ? C41 C42 C43 C44 -180(2) . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C42 0.0 . . . . ? C43 C42 C47 C46 0.0 . . . . ? C41 C42 C47 C46 180(2) . . . . ? I10 I6 I7 I15 0(100) 2_665 . . . ? I10 I6 I7 I15 0(99) . . . . ? I13 I5 I8 I14 71(6) . . . . ? I13 I5 I8 I14 31(4) . . . 2_665 ? I14 I5 I8 I14 -40(5) . . . 2_665 ? I14 I5 I8 I13 -71(6) . . . . ? I7 I6 I10 I15 180.000(2) . . . . ? I10 I6 I10 I15 0.000(5) 2_665 . . . ? I7 I6 I10 I10 180.000(3) . . . 2_665 ? I15 I6 I10 I10 0.000(5) . . . 2_665 ? I8 I5 I13 I9 -155(2) . . . . ? I14 I5 I13 I9 -134(3) . . . . ? I14 I5 I13 I8 21(2) . . . . ? I14 I8 I13 I5 -123(5) . . . . ? I14 I8 I13 I5 -153(3) 2_665 . . . ? I14 I8 I13 I9 -86(5) . . . . ? I5 I8 I13 I9 37(3) . . . . ? I14 I8 I13 I9 -116(3) 2_665 . . . ? I5 I8 I14 I14 -79(7) . . . 2_665 ? I13 I8 I14 I14 -59(7) . . . 2_665 ? I14 I8 I14 I5 79(7) 2_665 . . . ? I13 I8 I14 I5 19.7(18) . . . . ? I5 I8 I14 I8 -59(6) . . . 2_665 ? I14 I8 I14 I8 20(2) 2_665 . . 2_665 ? I13 I8 I14 I8 -39(6) . . . 2_665 ? I13 I5 I14 I8 -126(5) . . . . ? I13 I5 I14 I14 -6(6) . . . 2_665 ? I8 I5 I14 I14 120(7) . . . 2_665 ? I13 I5 I14 I8 7(4) . . . 2_665 ? I8 I5 I14 I8 133(5) . . . 2_665 ? I6 I10 I15 I10 180.000(4) . . . 2_665 ? I10 I10 I15 I6 180.000(5) 2_665 . . . ? I10 I10 I15 I7 180.000(5) 2_665 . . . ? I6 I10 I15 I7 0.000(1) . . . . ? I7 I6 I15 I10 0(100) . . . 2_665 ? I10 I6 I15 I10 180.000(5) . . . 2_665 ? I7 I6 I15 I10 0(100) . . . . ? I10 I6 I15 I10 180.000(4) 2_665 . . . ? I10 I6 I15 I7 0(100) 2_665 . . . ? I10 I6 I15 I7 0(100) . . . . ? I6 I7 I15 I10 0(100) . . . 2_665 ? I6 I7 I15 I10 0(100) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.713 _refine_diff_density_min -1.566 _refine_diff_density_rms 0.260 #============================================================================== data_[Gd.1]I3 _database_code_depnum_ccdc_archive 'CCDC 615718' #============================================================================== _chemical_name_systematic ; [Gd.DOTAM]Cl~3~.6H~2~O ; _chemical_name_common '[Gd.1]Cl3' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C16 H34 Gd N8 O5, 3(H2 O), 3I' _chemical_formula_sum 'C16 H40 Gd I3 N8 O8' _chemical_formula_weight 1010.51 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3654(5) _cell_length_b 12.5940(5) _cell_length_c 11.9080(5) _cell_angle_alpha 77.660(1) _cell_angle_beta 77.559(1) _cell_angle_gamma 78.109(1) _cell_volume 1602.95(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9825 _cell_measurement_theta_min 2.220 _cell_measurement_theta_max 26.129 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 958 _exptl_absorpt_coefficient_mu 5.005 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6596 _exptl_absorpt_correction_T_max 0.7319 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.0400 -1.00 0.00 0.00 0.0400 0.00 1.00 0.00 0.0400 0.00 -1.00 0.00 0.0400 0.00 0.00 1.00 0.0400 0.00 0.00 -1.00 0.0400 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 4 sets of \w scans each set at different \f and/or 2\q angles and each scan (18s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 19048 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 29.13 _reflns_number_total 8424 _reflns_number_gt 6971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+4.3357P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8424 _refine_ls_number_parameters 349 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.784312(18) 0.747153(17) 0.658614(18) 0.01127(5) Uani 1 1 d . . . O1 O 0.9333(3) 0.5909(2) 0.6015(3) 0.0166(6) Uani 1 1 d . . . O2 O 0.6530(3) 0.6807(3) 0.5716(3) 0.0174(6) Uani 1 1 d . . . O3 O 0.6753(3) 0.9226(3) 0.5943(3) 0.0181(6) Uani 1 1 d . . . O4 O 0.9526(3) 0.8389(3) 0.6190(3) 0.0187(6) Uani 1 1 d . . . N1 N 0.9257(3) 0.6468(3) 0.8137(3) 0.0134(7) Uani 1 1 d . . . N2 N 0.7090(3) 0.5634(3) 0.7807(3) 0.0151(7) Uani 1 1 d . . . N3 N 0.5631(3) 0.7888(3) 0.7848(3) 0.0152(7) Uani 1 1 d . . . N4 N 0.7802(3) 0.8710(3) 0.8167(3) 0.0144(7) Uani 1 1 d . . . N5 N 1.0998(3) 0.4623(3) 0.6213(3) 0.0196(8) Uani 1 1 d . . . H5C H 1.0914 0.4331 0.5633 0.024 Uiso 1 1 calc R . . H5D H 1.1609 0.4342 0.6590 0.024 Uiso 1 1 calc R . . N6 N 0.6136(3) 0.5364(3) 0.5126(3) 0.0205(8) Uani 1 1 d . . . H6C H 0.5935 0.5780 0.4479 0.025 Uiso 1 1 calc R . . H6D H 0.6108 0.4654 0.5266 0.025 Uiso 1 1 calc R . . N7 N 0.5119(3) 1.0585(3) 0.6107(3) 0.0197(8) Uani 1 1 d . . . H7C H 0.5541 1.1082 0.5663 0.024 Uiso 1 1 calc R . . H7D H 0.4343 1.0781 0.6398 0.024 Uiso 1 1 calc R . . N8 N 1.0568(4) 0.9622(3) 0.6454(4) 0.0258(9) Uani 1 1 d . . . H8C H 1.1209 0.9396 0.5946 0.031 Uiso 1 1 calc R . . H8D H 1.0583 1.0161 0.6812 0.031 Uiso 1 1 calc R . . C1 C 0.8634(4) 0.5617(4) 0.8999(4) 0.0184(9) Uani 1 1 d . . . H1A H 0.8001 0.5990 0.9565 0.022 Uiso 1 1 calc R . . H1B H 0.9241 0.5120 0.9438 0.022 Uiso 1 1 calc R . . C2 C 0.8040(4) 0.4930(4) 0.8453(4) 0.0176(9) Uani 1 1 d . . . H2A H 0.8671 0.4529 0.7909 0.021 Uiso 1 1 calc R . . H2B H 0.7661 0.4378 0.9073 0.021 Uiso 1 1 calc R . . C3 C 0.5951(4) 0.5885(4) 0.8666(4) 0.0166(9) Uani 1 1 d . . . H3A H 0.6174 0.6023 0.9375 0.020 Uiso 1 1 calc R . . H3B H 0.5539 0.5231 0.8897 0.020 Uiso 1 1 calc R . . C4 C 0.5065(4) 0.6870(4) 0.8205(4) 0.0164(8) Uani 1 1 d . . . H4A H 0.4799 0.6719 0.7524 0.020 Uiso 1 1 calc R . . H4B H 0.4333 0.6989 0.8817 0.020 Uiso 1 1 calc R . . C5 C 0.5687(4) 0.8331(4) 0.8896(4) 0.0197(9) Uani 1 1 d . . . H5A H 0.5977 0.7713 0.9493 0.024 Uiso 1 1 calc R . . H5B H 0.4852 0.8667 0.9228 0.024 Uiso 1 1 calc R . . C6 C 0.6517(4) 0.9184(4) 0.8638(4) 0.0179(9) Uani 1 1 d . . . H6A H 0.6216 0.9818 0.8062 0.022 Uiso 1 1 calc R . . H6B H 0.6498 0.9456 0.9364 0.022 Uiso 1 1 calc R . . C7 C 0.8393(4) 0.8071(4) 0.9151(4) 0.0195(9) Uani 1 1 d . . . H7A H 0.7794 0.7665 0.9720 0.023 Uiso 1 1 calc R . . H7B H 0.8622 0.8590 0.9552 0.023 Uiso 1 1 calc R . . C8 C 0.9518(4) 0.7259(4) 0.8787(4) 0.0179(9) Uani 1 1 d . . . H8A H 1.0154 0.7668 0.8285 0.021 Uiso 1 1 calc R . . H8B H 0.9843 0.6842 0.9491 0.021 Uiso 1 1 calc R . . C9 C 1.0417(4) 0.5957(4) 0.7493(4) 0.0166(8) Uani 1 1 d . . . H9A H 1.0837 0.5368 0.8038 0.020 Uiso 1 1 calc R . . H9B H 1.0953 0.6519 0.7170 0.020 Uiso 1 1 calc R . . C10 C 1.0216(4) 0.5475(4) 0.6515(4) 0.0154(8) Uani 1 1 d . . . C11 C 0.6857(4) 0.5033(4) 0.6946(4) 0.0172(9) Uani 1 1 d . . . H11A H 0.6206 0.4591 0.7326 0.021 Uiso 1 1 calc R . . H11B H 0.7609 0.4518 0.6700 0.021 Uiso 1 1 calc R . . C12 C 0.6480(4) 0.5804(4) 0.5885(4) 0.0162(8) Uani 1 1 d . . . C13 C 0.4890(4) 0.8723(4) 0.7089(4) 0.0176(9) Uani 1 1 d . . . H13A H 0.4182 0.9108 0.7577 0.021 Uiso 1 1 calc R . . H13B H 0.4575 0.8355 0.6586 0.021 Uiso 1 1 calc R . . C14 C 0.5650(4) 0.9547(4) 0.6336(4) 0.0171(9) Uani 1 1 d . . . C15 C 0.8485(4) 0.9597(4) 0.7514(4) 0.0194(9) Uani 1 1 d . . . H15A H 0.8754 0.9937 0.8071 0.023 Uiso 1 1 calc R . . H15B H 0.7941 1.0174 0.7071 0.023 Uiso 1 1 calc R . . C16 C 0.9588(4) 0.9155(4) 0.6676(4) 0.0181(9) Uani 1 1 d . . . I1 I 0.64593(3) 0.61593(3) 0.19674(3) 0.02225(7) Uani 1 1 d . . . I2 I 0.70494(3) 0.25433(3) 0.47553(3) 0.02693(8) Uani 1 1 d . . . I3 I 1.19429(3) 0.82333(3) 0.02542(3) 0.02789(8) Uani 1 1 d . . . O1W O 0.8509(3) 0.7807(3) 0.4521(3) 0.0200(7) Uani 1 1 d D . . H1WA H 0.918(2) 0.771(5) 0.423(4) 0.030 Uiso 1 1 d D . . H1WB H 0.807(4) 0.801(5) 0.409(4) 0.030 Uiso 1 1 d D . . O2W O 1.0883(4) 0.7461(4) 0.3405(4) 0.0435(11) Uani 1 1 d D . . H2WA H 1.127(6) 0.758(7) 0.381(5) 0.065 Uiso 1 1 d D . . H2WB H 1.117(6) 0.763(7) 0.276(3) 0.065 Uiso 1 1 d D . . O3W O 0.7172(3) 0.8430(3) 0.2758(3) 0.0241(7) Uani 1 1 d D . . H3WA H 0.704(5) 0.793(4) 0.257(5) 0.036 Uiso 1 1 d D . . H3WB H 0.771(4) 0.866(5) 0.234(4) 0.036 Uiso 1 1 d D . . O4W O 0.9087(3) 0.9399(3) 0.1601(3) 0.0273(8) Uani 1 1 d D . . H4WA H 0.888(5) 0.995(3) 0.120(5) 0.041 Uiso 1 1 d D . . H4WB H 0.974(3) 0.916(5) 0.133(5) 0.041 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01136(9) 0.01192(10) 0.01197(10) -0.00415(7) -0.00151(7) -0.00366(7) O1 0.0170(15) 0.0166(15) 0.0185(15) -0.0067(12) -0.0032(12) -0.0038(12) O2 0.0181(15) 0.0177(16) 0.0190(16) -0.0043(12) -0.0058(13) -0.0053(12) O3 0.0169(15) 0.0173(16) 0.0200(16) -0.0048(13) -0.0013(12) -0.0029(12) O4 0.0173(15) 0.0214(16) 0.0199(16) -0.0087(13) 0.0002(13) -0.0069(13) N1 0.0129(16) 0.0161(17) 0.0131(17) -0.0050(14) -0.0025(14) -0.0043(13) N2 0.0124(16) 0.0180(18) 0.0172(18) -0.0052(15) -0.0028(14) -0.0051(14) N3 0.0134(16) 0.0169(18) 0.0161(18) -0.0054(14) 0.0008(14) -0.0057(14) N4 0.0137(16) 0.0140(17) 0.0176(18) -0.0055(14) -0.0021(14) -0.0048(13) N5 0.0138(17) 0.025(2) 0.022(2) -0.0110(16) -0.0054(15) 0.0014(15) N6 0.0214(19) 0.021(2) 0.024(2) -0.0086(16) -0.0059(16) -0.0072(15) N7 0.0169(18) 0.0176(19) 0.0214(19) -0.0006(15) -0.0004(15) -0.0020(15) N8 0.022(2) 0.026(2) 0.033(2) -0.0144(19) 0.0026(18) -0.0111(17) C1 0.021(2) 0.022(2) 0.014(2) -0.0013(17) -0.0060(17) -0.0078(18) C2 0.019(2) 0.015(2) 0.020(2) 0.0006(17) -0.0043(18) -0.0070(17) C3 0.016(2) 0.019(2) 0.016(2) -0.0027(17) -0.0009(17) -0.0095(17) C4 0.0114(18) 0.018(2) 0.019(2) -0.0037(17) 0.0039(16) -0.0071(16) C5 0.017(2) 0.021(2) 0.021(2) -0.0111(18) 0.0051(18) -0.0029(17) C6 0.016(2) 0.020(2) 0.020(2) -0.0134(18) -0.0019(17) -0.0002(17) C7 0.020(2) 0.024(2) 0.019(2) -0.0133(19) -0.0044(18) -0.0035(18) C8 0.020(2) 0.022(2) 0.016(2) -0.0082(18) -0.0065(17) -0.0050(17) C9 0.0128(19) 0.018(2) 0.020(2) -0.0076(17) -0.0021(17) -0.0020(16) C10 0.0144(19) 0.018(2) 0.017(2) -0.0040(17) -0.0037(16) -0.0064(16) C11 0.019(2) 0.015(2) 0.021(2) -0.0052(17) -0.0024(17) -0.0096(17) C12 0.0101(18) 0.022(2) 0.020(2) -0.0075(18) -0.0009(16) -0.0061(16) C13 0.016(2) 0.017(2) 0.021(2) -0.0043(18) -0.0027(17) -0.0058(16) C14 0.016(2) 0.018(2) 0.020(2) -0.0057(17) -0.0051(17) -0.0052(17) C15 0.019(2) 0.014(2) 0.027(2) -0.0101(18) -0.0009(19) -0.0050(17) C16 0.016(2) 0.014(2) 0.025(2) -0.0067(18) -0.0044(18) -0.0013(16) I1 0.02217(15) 0.03050(17) 0.01557(14) -0.00437(12) -0.00289(11) -0.00796(12) I2 0.02038(15) 0.02200(16) 0.03953(19) -0.01012(14) 0.00075(13) -0.00767(12) I3 0.02634(16) 0.02213(16) 0.03212(18) -0.00807(13) 0.00300(13) -0.00232(12) O1W 0.0142(15) 0.0307(19) 0.0140(15) -0.0036(14) -0.0018(12) -0.0027(14) O2W 0.025(2) 0.075(3) 0.030(2) -0.011(2) 0.0008(17) -0.009(2) O3W 0.0194(17) 0.0273(19) 0.0281(19) -0.0093(15) -0.0030(14) -0.0059(14) O4W 0.0240(18) 0.030(2) 0.029(2) -0.0096(16) -0.0013(15) -0.0048(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O4 2.346(3) . ? Gd1 O2 2.356(3) . ? Gd1 O3 2.358(3) . ? Gd1 O1W 2.385(3) . ? Gd1 O1 2.430(3) . ? Gd1 N3 2.649(4) . ? Gd1 N1 2.652(3) . ? Gd1 N2 2.654(4) . ? Gd1 N4 2.676(4) . ? O1 C10 1.247(5) . ? O2 C12 1.247(5) . ? O3 C14 1.254(5) . ? O4 C16 1.247(5) . ? N1 C9 1.472(5) . ? N1 C1 1.494(6) . ? N1 C8 1.494(5) . ? N2 C2 1.488(5) . ? N2 C3 1.490(6) . ? N2 C11 1.493(5) . ? N3 C13 1.480(6) . ? N3 C5 1.489(6) . ? N3 C4 1.493(5) . ? N4 C15 1.476(6) . ? N4 C7 1.478(6) . ? N4 C6 1.495(5) . ? N5 C10 1.305(6) . ? N5 H5C 0.8800 . ? N5 H5D 0.8800 . ? N6 C12 1.315(5) . ? N6 H6C 0.8800 . ? N6 H6D 0.8800 . ? N7 C14 1.320(6) . ? N7 H7C 0.8800 . ? N7 H7D 0.8800 . ? N8 C16 1.317(6) . ? N8 H8C 0.8800 . ? N8 H8D 0.8800 . ? C1 C2 1.516(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.512(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.514(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.510(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.500(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.504(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 C14 1.505(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.512(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O1W H1WA 0.77(2) . ? O1W H1WB 0.76(2) . ? O2W H2WA 0.77(3) . ? O2W H2WB 0.77(3) . ? O3W H3WA 0.77(2) . ? O3W H3WB 0.77(2) . ? O4W H4WA 0.78(2) . ? O4W H4WB 0.77(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Gd1 O2 143.85(11) . . ? O4 Gd1 O3 84.60(11) . . ? O2 Gd1 O3 84.87(11) . . ? O4 Gd1 O1W 72.30(11) . . ? O2 Gd1 O1W 71.59(11) . . ? O3 Gd1 O1W 75.39(11) . . ? O4 Gd1 O1 85.06(10) . . ? O2 Gd1 O1 84.63(10) . . ? O3 Gd1 O1 145.96(11) . . ? O1W Gd1 O1 70.57(11) . . ? O4 Gd1 N3 131.39(11) . . ? O2 Gd1 N3 74.02(11) . . ? O3 Gd1 N3 66.62(11) . . ? O1W Gd1 N3 130.19(11) . . ? O1 Gd1 N3 139.56(11) . . ? O4 Gd1 N1 73.11(11) . . ? O2 Gd1 N1 131.55(11) . . ? O3 Gd1 N1 140.45(11) . . ? O1W Gd1 N1 125.11(11) . . ? O1 Gd1 N1 65.18(10) . . ? N3 Gd1 N1 104.65(11) . . ? O4 Gd1 N2 140.92(11) . . ? O2 Gd1 N2 66.03(11) . . ? O3 Gd1 N2 131.51(11) . . ? O1W Gd1 N2 124.67(12) . . ? O1 Gd1 N2 71.61(11) . . ? N3 Gd1 N2 68.42(11) . . ? N1 Gd1 N2 68.77(10) . . ? O4 Gd1 N4 66.37(11) . . ? O2 Gd1 N4 141.48(11) . . ? O3 Gd1 N4 73.60(11) . . ? O1W Gd1 N4 129.79(12) . . ? O1 Gd1 N4 130.10(10) . . ? N3 Gd1 N4 68.24(11) . . ? N1 Gd1 N4 67.66(11) . . ? N2 Gd1 N4 105.45(11) . . ? C10 O1 Gd1 123.5(3) . . ? C12 O2 Gd1 121.2(3) . . ? C14 O3 Gd1 123.9(3) . . ? C16 O4 Gd1 124.3(3) . . ? C9 N1 C1 110.9(3) . . ? C9 N1 C8 108.8(3) . . ? C1 N1 C8 108.4(3) . . ? C9 N1 Gd1 107.5(2) . . ? C1 N1 Gd1 109.4(2) . . ? C8 N1 Gd1 111.8(3) . . ? C2 N2 C3 108.5(3) . . ? C2 N2 C11 109.3(3) . . ? C3 N2 C11 110.2(3) . . ? C2 N2 Gd1 111.2(2) . . ? C3 N2 Gd1 111.1(3) . . ? C11 N2 Gd1 106.5(2) . . ? C13 N3 C5 109.7(3) . . ? C13 N3 C4 108.9(3) . . ? C5 N3 C4 110.4(3) . . ? C13 N3 Gd1 106.7(3) . . ? C5 N3 Gd1 110.7(2) . . ? C4 N3 Gd1 110.4(2) . . ? C15 N4 C7 110.6(3) . . ? C15 N4 C6 110.4(3) . . ? C7 N4 C6 108.8(3) . . ? C15 N4 Gd1 104.6(3) . . ? C7 N4 Gd1 111.8(3) . . ? C6 N4 Gd1 110.6(2) . . ? C10 N5 H5C 120.0 . . ? C10 N5 H5D 120.0 . . ? H5C N5 H5D 120.0 . . ? C12 N6 H6C 120.0 . . ? C12 N6 H6D 120.0 . . ? H6C N6 H6D 120.0 . . ? C14 N7 H7C 120.0 . . ? C14 N7 H7D 120.0 . . ? H7C N7 H7D 120.0 . . ? C16 N8 H8C 120.0 . . ? C16 N8 H8D 120.0 . . ? H8C N8 H8D 120.0 . . ? N1 C1 C2 114.0(3) . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N2 C2 C1 111.1(4) . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N2 C3 C4 113.6(4) . . ? N2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? N3 C4 C3 111.5(3) . . ? N3 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N3 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N3 C5 C6 113.5(4) . . ? N3 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N3 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N4 C6 C5 111.1(4) . . ? N4 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N4 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N4 C7 C8 113.7(4) . . ? N4 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N4 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C7 112.2(3) . . ? N1 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N1 C9 C10 111.6(3) . . ? N1 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N1 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? O1 C10 N5 122.9(4) . . ? O1 C10 C9 119.2(4) . . ? N5 C10 C9 117.8(4) . . ? N2 C11 C12 112.1(4) . . ? N2 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N2 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? O2 C12 N6 121.7(4) . . ? O2 C12 C11 121.4(4) . . ? N6 C12 C11 116.8(4) . . ? N3 C13 C14 110.3(3) . . ? N3 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N3 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? O3 C14 N7 122.5(4) . . ? O3 C14 C13 119.3(4) . . ? N7 C14 C13 118.2(4) . . ? N4 C15 C16 111.1(4) . . ? N4 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N4 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? O4 C16 N8 122.2(4) . . ? O4 C16 C15 119.1(4) . . ? N8 C16 C15 118.6(4) . . ? Gd1 O1W H1WA 123(4) . . ? Gd1 O1W H1WB 123(4) . . ? H1WA O1W H1WB 113(4) . . ? H2WA O2W H2WB 111(5) . . ? H3WA O3W H3WB 111(4) . . ? H4WA O4W H4WB 108(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Gd1 O1 C10 59.4(3) . . . . ? O2 Gd1 O1 C10 -155.3(3) . . . . ? O3 Gd1 O1 C10 132.1(3) . . . . ? O1W Gd1 O1 C10 132.4(3) . . . . ? N3 Gd1 O1 C10 -97.8(3) . . . . ? N1 Gd1 O1 C10 -14.3(3) . . . . ? N2 Gd1 O1 C10 -88.8(3) . . . . ? N4 Gd1 O1 C10 6.2(4) . . . . ? O4 Gd1 O2 C12 117.6(3) . . . . ? O3 Gd1 O2 C12 -168.8(3) . . . . ? O1W Gd1 O2 C12 114.9(3) . . . . ? O1 Gd1 O2 C12 43.6(3) . . . . ? N3 Gd1 O2 C12 -101.7(3) . . . . ? N1 Gd1 O2 C12 -6.1(4) . . . . ? N2 Gd1 O2 C12 -28.6(3) . . . . ? N4 Gd1 O2 C12 -113.4(3) . . . . ? O4 Gd1 O3 C14 -147.5(3) . . . . ? O2 Gd1 O3 C14 67.2(3) . . . . ? O1W Gd1 O3 C14 139.4(3) . . . . ? O1 Gd1 O3 C14 139.6(3) . . . . ? N3 Gd1 O3 C14 -7.6(3) . . . . ? N1 Gd1 O3 C14 -92.4(4) . . . . ? N2 Gd1 O3 C14 15.8(4) . . . . ? N4 Gd1 O3 C14 -80.6(3) . . . . ? O2 Gd1 O4 C16 134.4(3) . . . . ? O3 Gd1 O4 C16 60.8(4) . . . . ? O1W Gd1 O4 C16 137.1(4) . . . . ? O1 Gd1 O4 C16 -151.7(4) . . . . ? N3 Gd1 O4 C16 8.7(4) . . . . ? N1 Gd1 O4 C16 -86.2(4) . . . . ? N2 Gd1 O4 C16 -99.2(4) . . . . ? N4 Gd1 O4 C16 -13.7(3) . . . . ? O4 Gd1 N1 C9 -65.1(3) . . . . ? O2 Gd1 N1 C9 84.0(3) . . . . ? O3 Gd1 N1 C9 -123.7(3) . . . . ? O1W Gd1 N1 C9 -12.2(3) . . . . ? O1 Gd1 N1 C9 27.2(2) . . . . ? N3 Gd1 N1 C9 165.4(2) . . . . ? N2 Gd1 N1 C9 106.1(3) . . . . ? N4 Gd1 N1 C9 -136.0(3) . . . . ? O4 Gd1 N1 C1 174.3(3) . . . . ? O2 Gd1 N1 C1 -36.5(3) . . . . ? O3 Gd1 N1 C1 115.8(3) . . . . ? O1W Gd1 N1 C1 -132.7(3) . . . . ? O1 Gd1 N1 C1 -93.3(3) . . . . ? N3 Gd1 N1 C1 44.9(3) . . . . ? N2 Gd1 N1 C1 -14.4(3) . . . . ? N4 Gd1 N1 C1 103.5(3) . . . . ? O4 Gd1 N1 C8 54.2(3) . . . . ? O2 Gd1 N1 C8 -156.6(2) . . . . ? O3 Gd1 N1 C8 -4.3(4) . . . . ? O1W Gd1 N1 C8 107.2(3) . . . . ? O1 Gd1 N1 C8 146.6(3) . . . . ? N3 Gd1 N1 C8 -75.2(3) . . . . ? N2 Gd1 N1 C8 -134.6(3) . . . . ? N4 Gd1 N1 C8 -16.6(3) . . . . ? O4 Gd1 N2 C2 -1.0(4) . . . . ? O2 Gd1 N2 C2 147.6(3) . . . . ? O3 Gd1 N2 C2 -154.0(3) . . . . ? O1W Gd1 N2 C2 104.3(3) . . . . ? O1 Gd1 N2 C2 55.4(3) . . . . ? N3 Gd1 N2 C2 -130.9(3) . . . . ? N1 Gd1 N2 C2 -14.4(3) . . . . ? N4 Gd1 N2 C2 -72.4(3) . . . . ? O4 Gd1 N2 C3 119.9(3) . . . . ? O2 Gd1 N2 C3 -91.4(3) . . . . ? O3 Gd1 N2 C3 -33.0(3) . . . . ? O1W Gd1 N2 C3 -134.7(2) . . . . ? O1 Gd1 N2 C3 176.3(3) . . . . ? N3 Gd1 N2 C3 -9.9(2) . . . . ? N1 Gd1 N2 C3 106.5(3) . . . . ? N4 Gd1 N2 C3 48.5(3) . . . . ? O4 Gd1 N2 C11 -120.0(3) . . . . ? O2 Gd1 N2 C11 28.6(2) . . . . ? O3 Gd1 N2 C11 87.0(3) . . . . ? O1W Gd1 N2 C11 -14.6(3) . . . . ? O1 Gd1 N2 C11 -63.6(2) . . . . ? N3 Gd1 N2 C11 110.1(3) . . . . ? N1 Gd1 N2 C11 -133.4(3) . . . . ? N4 Gd1 N2 C11 168.6(2) . . . . ? O4 Gd1 N3 C13 83.4(3) . . . . ? O2 Gd1 N3 C13 -66.7(3) . . . . ? O3 Gd1 N3 C13 24.6(2) . . . . ? O1W Gd1 N3 C13 -19.0(3) . . . . ? O1 Gd1 N3 C13 -127.6(2) . . . . ? N1 Gd1 N3 C13 163.6(2) . . . . ? N2 Gd1 N3 C13 -136.8(3) . . . . ? N4 Gd1 N3 C13 105.4(3) . . . . ? O4 Gd1 N3 C5 -35.9(3) . . . . ? O2 Gd1 N3 C5 174.0(3) . . . . ? O3 Gd1 N3 C5 -94.8(3) . . . . ? O1W Gd1 N3 C5 -138.3(3) . . . . ? O1 Gd1 N3 C5 113.1(3) . . . . ? N1 Gd1 N3 C5 44.3(3) . . . . ? N2 Gd1 N3 C5 103.9(3) . . . . ? N4 Gd1 N3 C5 -13.9(3) . . . . ? O4 Gd1 N3 C4 -158.5(2) . . . . ? O2 Gd1 N3 C4 51.4(3) . . . . ? O3 Gd1 N3 C4 142.7(3) . . . . ? O1W Gd1 N3 C4 99.2(3) . . . . ? O1 Gd1 N3 C4 -9.5(3) . . . . ? N1 Gd1 N3 C4 -78.2(3) . . . . ? N2 Gd1 N3 C4 -18.6(2) . . . . ? N4 Gd1 N3 C4 -136.4(3) . . . . ? O4 Gd1 N4 C15 28.0(2) . . . . ? O2 Gd1 N4 C15 -122.0(3) . . . . ? O3 Gd1 N4 C15 -63.3(3) . . . . ? O1W Gd1 N4 C15 -9.3(3) . . . . ? O1 Gd1 N4 C15 88.5(3) . . . . ? N3 Gd1 N4 C15 -134.1(3) . . . . ? N1 Gd1 N4 C15 108.6(3) . . . . ? N2 Gd1 N4 C15 167.3(2) . . . . ? O4 Gd1 N4 C7 -91.7(3) . . . . ? O2 Gd1 N4 C7 118.4(3) . . . . ? O3 Gd1 N4 C7 177.1(3) . . . . ? O1W Gd1 N4 C7 -128.9(3) . . . . ? O1 Gd1 N4 C7 -31.1(3) . . . . ? N3 Gd1 N4 C7 106.2(3) . . . . ? N1 Gd1 N4 C7 -11.1(3) . . . . ? N2 Gd1 N4 C7 47.6(3) . . . . ? O4 Gd1 N4 C6 146.8(3) . . . . ? O2 Gd1 N4 C6 -3.1(4) . . . . ? O3 Gd1 N4 C6 55.6(3) . . . . ? O1W Gd1 N4 C6 109.6(3) . . . . ? O1 Gd1 N4 C6 -152.6(3) . . . . ? N3 Gd1 N4 C6 -15.3(3) . . . . ? N1 Gd1 N4 C6 -132.5(3) . . . . ? N2 Gd1 N4 C6 -73.9(3) . . . . ? C9 N1 C1 C2 -74.7(4) . . . . ? C8 N1 C1 C2 165.8(4) . . . . ? Gd1 N1 C1 C2 43.7(4) . . . . ? C3 N2 C2 C1 -80.4(4) . . . . ? C11 N2 C2 C1 159.4(4) . . . . ? Gd1 N2 C2 C1 42.1(4) . . . . ? N1 C1 C2 N2 -60.1(5) . . . . ? C2 N2 C3 C4 161.1(3) . . . . ? C11 N2 C3 C4 -79.3(4) . . . . ? Gd1 N2 C3 C4 38.6(4) . . . . ? C13 N3 C4 C3 162.9(4) . . . . ? C5 N3 C4 C3 -76.6(4) . . . . ? Gd1 N3 C4 C3 46.1(4) . . . . ? N2 C3 C4 N3 -59.0(5) . . . . ? C13 N3 C5 C6 -74.2(4) . . . . ? C4 N3 C5 C6 165.7(4) . . . . ? Gd1 N3 C5 C6 43.3(4) . . . . ? C15 N4 C6 C5 158.5(4) . . . . ? C7 N4 C6 C5 -80.0(4) . . . . ? Gd1 N4 C6 C5 43.2(4) . . . . ? N3 C5 C6 N4 -60.3(5) . . . . ? C15 N4 C7 C8 -77.5(5) . . . . ? C6 N4 C7 C8 161.1(4) . . . . ? Gd1 N4 C7 C8 38.5(4) . . . . ? C9 N1 C8 C7 161.9(4) . . . . ? C1 N1 C8 C7 -77.4(4) . . . . ? Gd1 N1 C8 C7 43.3(4) . . . . ? N4 C7 C8 N1 -56.6(5) . . . . ? C1 N1 C9 C10 80.8(4) . . . . ? C8 N1 C9 C10 -160.0(4) . . . . ? Gd1 N1 C9 C10 -38.8(4) . . . . ? Gd1 O1 C10 N5 178.8(3) . . . . ? Gd1 O1 C10 C9 -2.6(5) . . . . ? N1 C9 C10 O1 30.8(6) . . . . ? N1 C9 C10 N5 -150.5(4) . . . . ? C2 N2 C11 C12 -149.7(4) . . . . ? C3 N2 C11 C12 91.2(4) . . . . ? Gd1 N2 C11 C12 -29.4(4) . . . . ? Gd1 O2 C12 N6 -154.6(3) . . . . ? Gd1 O2 C12 C11 22.9(5) . . . . ? N2 C11 C12 O2 8.9(6) . . . . ? N2 C11 C12 N6 -173.4(4) . . . . ? C5 N3 C13 C14 81.8(4) . . . . ? C4 N3 C13 C14 -157.2(4) . . . . ? Gd1 N3 C13 C14 -38.1(4) . . . . ? Gd1 O3 C14 N7 168.4(3) . . . . ? Gd1 O3 C14 C13 -12.2(5) . . . . ? N3 C13 C14 O3 36.6(6) . . . . ? N3 C13 C14 N7 -143.9(4) . . . . ? C7 N4 C15 C16 80.5(4) . . . . ? C6 N4 C15 C16 -159.1(4) . . . . ? Gd1 N4 C15 C16 -40.0(4) . . . . ? Gd1 O4 C16 N8 177.8(3) . . . . ? Gd1 O4 C16 C15 -4.8(6) . . . . ? N4 C15 C16 O4 34.4(6) . . . . ? N4 C15 C16 N8 -148.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5C O1 0.88 2.13 2.988(5) 163.9 2_766 N5 H5D I1 0.88 2.96 3.825(4) 168.0 2_766 N6 H6C I1 0.88 2.88 3.638(4) 145.9 . N6 H6D I2 0.88 2.80 3.585(4) 149.8 . N7 H7C I2 0.88 2.67 3.535(4) 166.7 1_565 N7 H7D O3W 0.88 1.98 2.831(5) 160.9 2_676 N8 H8C I2 0.88 2.96 3.714(4) 145.2 2_766 N8 H8D O4W 0.88 2.20 2.975(6) 146.0 2_776 O1W H1WA O2W 0.77(2) 1.96(3) 2.730(5) 177(6) . O1W H1WB O3W 0.76(2) 1.99(3) 2.741(5) 170(6) . O2W H2WA I2 0.77(3) 2.79(3) 3.540(4) 166(8) 2_766 O2W H2WB I3 0.77(3) 2.90(3) 3.668(4) 173(6) . O3W H3WA I1 0.77(2) 2.72(3) 3.486(3) 177(6) . O3W H3WB O4W 0.77(2) 1.93(3) 2.685(5) 166(6) . O4W H4WA I3 0.78(2) 2.69(3) 3.464(4) 175(6) 2_775 O4W H4WB I3 0.77(3) 2.70(3) 3.473(4) 174(6) . _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.567 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.165