data_global _journal_name_full 'Sci.Rep.Res.Inst.Tohoku Univ.Series A' _journal_coden_cambridge 0117 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email rhhudson@uwo.ca _publ_contact_author_name 'Robert Hudson' loop_ _publ_author_name R.Hudson M.Milne K.Chicas A.Li R.Bartha data_b10070p-1 _database_code_depnum_ccdc_archive 'CCDC 814847' #TrackingRef '- Dy.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H42 Dy N8 O5, C3 H6 O, 4(H2 O), 2(Cl H), Cl' _chemical_formula_sum 'C31 H58 Cl3 Dy N8 O10' _chemical_formula_weight 971.70 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' Dy Dy -0.1892 4.4098 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8844(4) _cell_length_b 14.3626(6) _cell_length_c 15.4658(10) _cell_angle_alpha 113.395(3) _cell_angle_beta 103.121(3) _cell_angle_gamma 99.252(2) _cell_volume 2074.15(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9691 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.99 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 994 _exptl_absorpt_coefficient_mu 2.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8611 _exptl_absorpt_correction_T_max 0.9223 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 286221 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 30.03 _reflns_number_total 12145 _reflns_number_gt 11022 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+2.0704P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12145 _refine_ls_number_parameters 516 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _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 Dy1 Dy 0.382913(9) 0.370326(7) 0.265321(6) 0.01340(3) Uani 1 1 d . . . Cl1 Cl 0.96258(6) 0.36513(5) 0.54814(5) 0.03045(12) Uani 1 1 d . . . Cl2 Cl 0.02186(6) 0.66258(5) 0.12561(5) 0.03178(12) Uani 1 1 d D . . H2G H -0.049(3) 0.643(3) 0.164(2) 0.048 Uiso 1 1 d D . . Cl3 Cl 0.43811(7) 0.85228(5) 0.16404(5) 0.03767(14) Uani 1 1 d D . . H3G H 0.533(2) 0.831(3) 0.179(3) 0.057 Uiso 1 1 d D . . O7S O 0.2723(2) 0.82980(14) 0.30139(13) 0.0330(4) Uani 1 1 d D . . H7E H 0.319(3) 0.844(3) 0.270(2) 0.049 Uiso 1 1 d D . . H7F H 0.2030(18) 0.788(2) 0.2569(18) 0.049 Uiso 1 1 d D . . O1 O 0.33218(14) 0.32901(11) 0.38806(10) 0.0171(3) Uani 1 1 d . . . O4 O 0.50840(15) 0.24928(11) 0.25034(11) 0.0196(3) Uani 1 1 d . . . O8S O 0.81104(17) 0.42499(16) 0.38867(15) 0.0335(4) Uani 1 1 d D . . H8F H 0.852(3) 0.403(2) 0.425(2) 0.050 Uiso 1 1 d D . . H8E H 0.865(3) 0.4770(18) 0.395(3) 0.050 Uiso 1 1 d D . . N6 N 0.69344(19) 0.46398(15) 0.14639(14) 0.0237(4) Uani 1 1 d . . . H6 H 0.7149 0.4299 0.0932 0.028 Uiso 1 1 calc R . . O9S O 0.0603(3) 0.8688(2) 0.08986(18) 0.0521(6) Uani 1 1 d D . . H9E H 0.089(4) 0.820(3) 0.092(3) 0.078 Uiso 1 1 d D . . H9F H 0.022(4) 0.888(3) 0.132(3) 0.078 Uiso 1 1 d D . . O10S O 0.2200(3) 0.6463(2) 0.00906(19) 0.0615(7) Uani 1 1 d D . . H10E H 0.275(3) 0.702(2) 0.053(3) 0.092 Uiso 1 1 d D . . H10F H 0.157(3) 0.643(3) 0.030(3) 0.092 Uiso 1 1 d D . . O3 O 0.55405(15) 0.46033(11) 0.23418(11) 0.0191(3) Uani 1 1 d . . . O2 O 0.37256(14) 0.54332(11) 0.37135(10) 0.0174(3) Uani 1 1 d . . . N4 N 0.34924(18) 0.70445(14) 0.39299(13) 0.0194(3) Uani 1 1 d . . . H4 H 0.3324 0.7456 0.3649 0.023 Uiso 1 1 calc R . . O5 O 0.57545(15) 0.44957(12) 0.41283(11) 0.0189(3) Uani 1 1 d D . . H5F H 0.6422(18) 0.438(2) 0.4000(19) 0.028 Uiso 1 1 d D . . H5E H 0.574(3) 0.440(2) 0.4611(14) 0.028 Uiso 1 1 d D . . O6 O 0.9259(3) 0.9841(3) 0.2309(2) 0.0746(8) Uani 1 1 d . . . N1 N 0.20106(18) 0.31231(14) 0.47803(13) 0.0196(3) Uani 1 1 d . . . H1 H 0.1251 0.3152 0.4881 0.023 Uiso 1 1 calc R . . C4 C 0.2910(3) 0.0801(2) 0.4405(2) 0.0357(6) Uani 1 1 d . . . H4A H 0.2901 0.0084 0.4060 0.043 Uiso 1 1 calc R . . N2 N 0.13523(17) 0.35310(13) 0.25769(12) 0.0171(3) Uani 1 1 d . . . N3 N 0.27414(18) 0.46122(13) 0.16535(12) 0.0179(3) Uani 1 1 d . . . N5 N 0.37687(17) 0.27738(13) 0.07889(13) 0.0180(3) Uani 1 1 d . . . N7 N 0.24008(17) 0.17073(13) 0.17370(12) 0.0171(3) Uani 1 1 d . . . N8 N 0.53197(19) 0.08531(15) 0.20829(15) 0.0241(4) Uani 1 1 d . . . H8 H 0.4938 0.0184 0.1892 0.029 Uiso 1 1 calc R . . C10 C 0.3760(2) 0.74596(17) 0.50080(15) 0.0208(4) Uani 1 1 d . . . H10A H 0.3033 0.7089 0.5142 0.025 Uiso 1 1 calc R . . H10B H 0.4580 0.7330 0.5307 0.025 Uiso 1 1 calc R . . C1 C 0.2286(2) 0.33681(15) 0.40987(15) 0.0173(4) Uani 1 1 d . . . C2 C 0.2939(2) 0.28029(18) 0.53746(16) 0.0231(4) Uani 1 1 d . . . H2A H 0.2721 0.2906 0.5988 0.028 Uiso 1 1 calc R . . H2B H 0.3837 0.3263 0.5574 0.028 Uiso 1 1 calc R . . C3 C 0.2922(2) 0.16973(19) 0.48370(18) 0.0263(4) Uani 1 1 d . . . C5 C 0.1319(2) 0.37865(17) 0.35943(15) 0.0194(4) Uani 1 1 d . . . H5A H 0.0422 0.3472 0.3563 0.023 Uiso 1 1 calc R . . H5B H 0.1536 0.4563 0.3988 0.023 Uiso 1 1 calc R . . C6 C 0.0837(2) 0.42877(17) 0.22567(16) 0.0203(4) Uani 1 1 d . . . H6A H 0.1160 0.5004 0.2825 0.024 Uiso 1 1 calc R . . H6B H -0.0135 0.4073 0.2049 0.024 Uiso 1 1 calc R . . C7 C 0.1272(2) 0.43143(18) 0.14031(15) 0.0217(4) Uani 1 1 d . . . H7A H 0.0890 0.3609 0.0820 0.026 Uiso 1 1 calc R . . H7B H 0.0928 0.4829 0.1217 0.026 Uiso 1 1 calc R . . C13 C 0.3056(2) 0.43246(17) 0.07029(15) 0.0210(4) Uani 1 1 d . . . H13A H 0.3970 0.4723 0.0848 0.025 Uiso 1 1 calc R . . H13B H 0.2461 0.4524 0.0263 0.025 Uiso 1 1 calc R . . C14 C 0.2905(2) 0.31475(17) 0.01750(15) 0.0223(4) Uani 1 1 d . . . H14A H 0.1977 0.2756 -0.0003 0.027 Uiso 1 1 calc R . . H14B H 0.3115 0.2983 -0.0450 0.027 Uiso 1 1 calc R . . C20 C 0.3272(2) 0.15977(16) 0.03337(15) 0.0205(4) Uani 1 1 d . . . H20A H 0.3986 0.1310 0.0549 0.025 Uiso 1 1 calc R . . H20B H 0.3005 0.1303 -0.0400 0.025 Uiso 1 1 calc R . . C21 C 0.2111(2) 0.12598(16) 0.06336(15) 0.0208(4) Uani 1 1 d . . . H21A H 0.1369 0.1486 0.0355 0.025 Uiso 1 1 calc R . . H21B H 0.1831 0.0479 0.0339 0.025 Uiso 1 1 calc R . . C22 C 0.3184(2) 0.11226(16) 0.21263(16) 0.0197(4) Uani 1 1 d . . . H22A H 0.2857 0.0359 0.1660 0.024 Uiso 1 1 calc R . . H22B H 0.3093 0.1217 0.2776 0.024 Uiso 1 1 calc R . . C23 C 0.4612(2) 0.15315(16) 0.22472(15) 0.0186(4) Uani 1 1 d . . . C24 C 0.6720(2) 0.1180(2) 0.22089(19) 0.0287(5) Uani 1 1 d . . . H24A H 0.7151 0.0677 0.2353 0.034 Uiso 1 1 calc R . . H24B H 0.7132 0.1887 0.2784 0.034 Uiso 1 1 calc R . . C25 C 0.6930(2) 0.12161(18) 0.13155(19) 0.0277(5) Uani 1 1 d . . . C26 C 0.7093(3) 0.1257(2) 0.0597(2) 0.0342(5) Uani 1 1 d . . . H26 H 0.7223 0.1289 0.0022 0.041 Uiso 1 1 calc R . . C27 C 0.1127(2) 0.15853(16) 0.19397(16) 0.0209(4) Uani 1 1 d . . . H27A H 0.1275 0.1627 0.2611 0.025 Uiso 1 1 calc R . . H27B H 0.0522 0.0882 0.1450 0.025 Uiso 1 1 calc R . . C28 C 0.0505(2) 0.24384(17) 0.18776(17) 0.0221(4) Uani 1 1 d . . . H28A H 0.0301 0.2357 0.1190 0.027 Uiso 1 1 calc R . . H28B H -0.0334 0.2337 0.2021 0.027 Uiso 1 1 calc R . . C15 C 0.5141(2) 0.30658(17) 0.07946(16) 0.0226(4) Uani 1 1 d . . . H15A H 0.5134 0.3016 0.0136 0.027 Uiso 1 1 calc R . . H15B H 0.5592 0.2559 0.0909 0.027 Uiso 1 1 calc R . . C16 C 0.5891(2) 0.41683(17) 0.15874(16) 0.0199(4) Uani 1 1 d . . . C17 C 0.7749(2) 0.57121(19) 0.21833(18) 0.0270(5) Uani 1 1 d . . . H17A H 0.8556 0.5876 0.2016 0.032 Uiso 1 1 calc R . . H17B H 0.8011 0.5758 0.2859 0.032 Uiso 1 1 calc R . . C18 C 0.7017(3) 0.6482(2) 0.21692(19) 0.0326(5) Uani 1 1 d . . . C19 C 0.6414(3) 0.7104(2) 0.2152(2) 0.0421(7) Uani 1 1 d . . . H19 H 0.5935 0.7599 0.2138 0.051 Uiso 1 1 calc R . . C8 C 0.3289(2) 0.57718(16) 0.22812(15) 0.0208(4) Uani 1 1 d . . . H8A H 0.2681 0.6135 0.2058 0.025 Uiso 1 1 calc R . . H8B H 0.4140 0.6012 0.2197 0.025 Uiso 1 1 calc R . . C9 C 0.3496(2) 0.60748(16) 0.33707(15) 0.0179(4) Uani 1 1 d . . . C11 C 0.3893(2) 0.85960(19) 0.54593(17) 0.0271(5) Uani 1 1 d . . . C12 C 0.4027(3) 0.9517(2) 0.5824(2) 0.0426(7) Uani 1 1 d . . . H12 H 0.4135 1.0257 0.6117 0.051 Uiso 1 1 calc R . . C29 C 0.9640(4) 0.8908(3) 0.3273(3) 0.0643(10) Uani 1 1 d . . . H29A H 0.9648 0.8353 0.2650 0.096 Uiso 1 1 calc R . . H29B H 0.8945 0.8633 0.3488 0.096 Uiso 1 1 calc R . . H29C H 1.0492 0.9134 0.3787 0.096 Uiso 1 1 calc R . . C30 C 0.9385(3) 0.9836(3) 0.3112(3) 0.0539(8) Uani 1 1 d . . . C31 C 0.9308(4) 1.0740(3) 0.3974(3) 0.0771(14) Uani 1 1 d . . . H31A H 0.9438 1.1370 0.3865 0.116 Uiso 1 1 calc R . . H31B H 0.9992 1.0869 0.4576 0.116 Uiso 1 1 calc R . . H31C H 0.8442 1.0579 0.4053 0.116 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01320(5) 0.01382(4) 0.01257(4) 0.00440(3) 0.00538(3) 0.00459(3) Cl1 0.0236(3) 0.0367(3) 0.0363(3) 0.0162(2) 0.0166(2) 0.0125(2) Cl2 0.0300(3) 0.0352(3) 0.0305(3) 0.0151(2) 0.0108(2) 0.0078(2) Cl3 0.0513(4) 0.0240(3) 0.0328(3) 0.0109(2) 0.0111(3) 0.0066(3) O7S 0.0399(11) 0.0266(8) 0.0275(9) 0.0116(7) 0.0035(8) 0.0093(8) O1 0.0156(7) 0.0190(6) 0.0175(6) 0.0073(5) 0.0074(5) 0.0063(5) O4 0.0189(7) 0.0165(6) 0.0215(7) 0.0061(6) 0.0070(6) 0.0059(5) O8S 0.0194(8) 0.0387(10) 0.0383(10) 0.0145(8) 0.0075(7) 0.0080(7) N6 0.0245(9) 0.0256(9) 0.0228(9) 0.0089(7) 0.0145(7) 0.0068(7) O9S 0.0472(14) 0.0571(15) 0.0435(13) 0.0283(12) -0.0007(10) -0.0004(11) O10S 0.0572(15) 0.0479(13) 0.0508(14) -0.0047(11) 0.0348(12) -0.0120(11) O3 0.0214(7) 0.0206(7) 0.0173(7) 0.0080(6) 0.0105(6) 0.0066(6) O2 0.0176(7) 0.0173(6) 0.0179(6) 0.0075(5) 0.0057(5) 0.0070(5) N4 0.0231(9) 0.0180(8) 0.0165(8) 0.0067(6) 0.0063(7) 0.0074(7) O5 0.0163(7) 0.0226(7) 0.0168(7) 0.0077(6) 0.0054(6) 0.0059(6) O6 0.080(2) 0.084(2) 0.079(2) 0.0472(18) 0.0358(17) 0.0288(17) N1 0.0195(8) 0.0234(8) 0.0208(8) 0.0108(7) 0.0119(7) 0.0091(7) C4 0.0372(14) 0.0305(12) 0.0449(15) 0.0188(11) 0.0167(12) 0.0139(11) N2 0.0151(8) 0.0190(8) 0.0165(7) 0.0066(6) 0.0049(6) 0.0063(6) N3 0.0207(8) 0.0184(8) 0.0138(7) 0.0061(6) 0.0056(6) 0.0065(6) N5 0.0195(8) 0.0172(7) 0.0162(7) 0.0051(6) 0.0076(6) 0.0065(6) N7 0.0157(8) 0.0180(7) 0.0161(7) 0.0058(6) 0.0052(6) 0.0056(6) N8 0.0234(9) 0.0210(8) 0.0289(9) 0.0101(7) 0.0093(8) 0.0103(7) C10 0.0218(10) 0.0213(9) 0.0173(9) 0.0065(8) 0.0070(8) 0.0059(8) C1 0.0169(9) 0.0155(8) 0.0162(8) 0.0040(7) 0.0058(7) 0.0043(7) C2 0.0264(11) 0.0269(10) 0.0196(9) 0.0114(8) 0.0094(8) 0.0110(9) C3 0.0248(11) 0.0301(11) 0.0303(11) 0.0170(10) 0.0119(9) 0.0107(9) C5 0.0179(9) 0.0232(9) 0.0202(9) 0.0095(8) 0.0101(8) 0.0091(8) C6 0.0166(9) 0.0235(9) 0.0210(9) 0.0092(8) 0.0054(8) 0.0096(8) C7 0.0206(10) 0.0265(10) 0.0178(9) 0.0100(8) 0.0036(8) 0.0094(8) C13 0.0285(11) 0.0232(9) 0.0149(9) 0.0097(8) 0.0086(8) 0.0107(8) C14 0.0310(12) 0.0223(10) 0.0138(9) 0.0067(8) 0.0080(8) 0.0108(9) C20 0.0254(11) 0.0173(9) 0.0152(9) 0.0033(7) 0.0071(8) 0.0070(8) C21 0.0214(10) 0.0178(9) 0.0174(9) 0.0040(7) 0.0043(8) 0.0035(8) C22 0.0207(10) 0.0181(9) 0.0211(9) 0.0084(8) 0.0081(8) 0.0067(8) C23 0.0217(10) 0.0179(9) 0.0159(8) 0.0065(7) 0.0067(7) 0.0067(8) C24 0.0216(11) 0.0322(12) 0.0316(12) 0.0119(10) 0.0077(9) 0.0137(9) C25 0.0188(10) 0.0242(10) 0.0357(12) 0.0096(9) 0.0069(9) 0.0082(8) C26 0.0326(13) 0.0331(13) 0.0361(13) 0.0122(11) 0.0130(11) 0.0133(11) C27 0.0160(9) 0.0189(9) 0.0224(10) 0.0053(8) 0.0063(8) 0.0017(7) C28 0.0133(9) 0.0213(9) 0.0246(10) 0.0055(8) 0.0035(8) 0.0026(7) C15 0.0262(11) 0.0216(9) 0.0223(10) 0.0073(8) 0.0146(9) 0.0093(8) C16 0.0208(10) 0.0224(9) 0.0201(9) 0.0105(8) 0.0093(8) 0.0092(8) C17 0.0246(11) 0.0289(11) 0.0251(11) 0.0102(9) 0.0113(9) 0.0017(9) C18 0.0389(14) 0.0324(12) 0.0257(11) 0.0137(10) 0.0125(10) 0.0033(11) C19 0.0532(18) 0.0432(15) 0.0383(15) 0.0246(13) 0.0181(13) 0.0134(14) C8 0.0283(11) 0.0170(9) 0.0178(9) 0.0073(7) 0.0079(8) 0.0086(8) C9 0.0151(9) 0.0183(9) 0.0182(9) 0.0060(7) 0.0053(7) 0.0048(7) C11 0.0322(12) 0.0254(11) 0.0184(10) 0.0051(8) 0.0072(9) 0.0085(9) C12 0.0586(19) 0.0271(12) 0.0295(13) 0.0040(10) 0.0076(13) 0.0128(12) C29 0.065(2) 0.0462(19) 0.076(3) 0.0238(19) 0.025(2) 0.0087(17) C30 0.0353(16) 0.054(2) 0.069(2) 0.0256(18) 0.0184(16) 0.0085(14) C31 0.045(2) 0.067(3) 0.080(3) 0.001(2) 0.008(2) 0.0197(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O3 2.3452(15) . ? Dy1 O1 2.3506(14) . ? Dy1 O4 2.3514(14) . ? Dy1 O2 2.4112(14) . ? Dy1 O5 2.4274(15) . ? Dy1 N3 2.6010(17) . ? Dy1 N5 2.6322(17) . ? Dy1 N2 2.6383(17) . ? Dy1 N7 2.6427(17) . ? Cl2 H2G 1.138(10) . ? Cl3 H3G 1.124(10) . ? O7S H7E 0.829(10) . ? O7S H7F 0.831(10) . ? O1 C1 1.257(2) . ? O4 C23 1.254(2) . ? O8S H8F 0.824(10) . ? O8S H8E 0.826(10) . ? N6 C16 1.319(3) . ? N6 C17 1.466(3) . ? N6 H6 0.8800 . ? O9S H9E 0.823(10) . ? O9S H9F 0.825(10) . ? O10S H10E 0.827(10) . ? O10S H10F 0.821(10) . ? O3 C16 1.264(2) . ? O2 C9 1.263(2) . ? N4 C9 1.317(3) . ? N4 C10 1.468(3) . ? N4 H4 0.8800 . ? O5 H5F 0.822(9) . ? O5 H5E 0.816(9) . ? O6 C30 1.220(5) . ? N1 C1 1.315(3) . ? N1 C2 1.463(3) . ? N1 H1 0.8800 . ? C4 C3 1.189(4) . ? C4 H4A 0.9500 . ? N2 C5 1.478(3) . ? N2 C28 1.489(3) . ? N2 C6 1.496(3) . ? N3 C8 1.485(3) . ? N3 C13 1.497(3) . ? N3 C7 1.503(3) . ? N5 C15 1.482(3) . ? N5 C20 1.493(3) . ? N5 C14 1.495(3) . ? N7 C22 1.481(3) . ? N7 C27 1.488(3) . ? N7 C21 1.498(3) . ? N8 C23 1.320(3) . ? N8 C24 1.464(3) . ? N8 H8 0.8800 . ? C10 C11 1.465(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C1 C5 1.510(3) . ? C2 C3 1.466(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.512(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C13 C14 1.518(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C20 C21 1.516(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.510(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C24 C25 1.470(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.186(4) . ? C26 H26 0.9500 . ? C27 C28 1.516(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C15 C16 1.505(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C18 1.467(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.195(4) . ? C19 H19 0.9500 . ? C8 C9 1.514(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C11 C12 1.182(4) . ? C12 H12 0.9500 . ? C29 C30 1.506(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.477(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 O3 Dy1 O1 142.41(5) . . ? O3 Dy1 O4 82.93(5) . . ? O1 Dy1 O4 85.31(5) . . ? O3 Dy1 O2 85.75(5) . . ? O1 Dy1 O2 83.13(5) . . ? O4 Dy1 O2 143.96(5) . . ? O3 Dy1 O5 71.45(5) . . ? O1 Dy1 O5 70.96(5) . . ? O4 Dy1 O5 71.90(5) . . ? O2 Dy1 O5 72.06(5) . . ? O3 Dy1 N3 74.31(5) . . ? O1 Dy1 N3 131.92(5) . . ? O4 Dy1 N3 139.87(5) . . ? O2 Dy1 N3 67.35(5) . . ? O5 Dy1 N3 127.93(5) . . ? O3 Dy1 N5 67.22(5) . . ? O1 Dy1 N5 140.52(5) . . ? O4 Dy1 N5 71.62(5) . . ? O2 Dy1 N5 133.53(5) . . ? O5 Dy1 N5 127.11(5) . . ? N3 Dy1 N5 69.21(5) . . ? O3 Dy1 N2 142.09(5) . . ? O1 Dy1 N2 66.85(5) . . ? O4 Dy1 N2 131.78(5) . . ? O2 Dy1 N2 73.13(5) . . ? O5 Dy1 N2 127.45(5) . . ? N3 Dy1 N2 68.63(5) . . ? N5 Dy1 N2 105.41(5) . . ? O3 Dy1 N7 131.78(5) . . ? O1 Dy1 N7 73.29(5) . . ? O4 Dy1 N7 66.28(5) . . ? O2 Dy1 N7 140.19(5) . . ? O5 Dy1 N7 126.18(5) . . ? N3 Dy1 N7 105.89(5) . . ? N5 Dy1 N7 68.24(5) . . ? N2 Dy1 N7 68.27(5) . . ? H7E O7S H7F 103(2) . . ? C1 O1 Dy1 123.29(13) . . ? C23 O4 Dy1 123.90(13) . . ? H8F O8S H8E 105(2) . . ? C16 N6 C17 122.15(18) . . ? C16 N6 H6 118.9 . . ? C17 N6 H6 118.9 . . ? H9E O9S H9F 109(2) . . ? H10E O10S H10F 104(2) . . ? C16 O3 Dy1 122.39(13) . . ? C9 O2 Dy1 120.99(13) . . ? C9 N4 C10 121.98(18) . . ? C9 N4 H4 119.0 . . ? C10 N4 H4 119.0 . . ? Dy1 O5 H5F 112.4(19) . . ? Dy1 O5 H5E 120(2) . . ? H5F O5 H5E 108(2) . . ? C1 N1 C2 121.48(18) . . ? C1 N1 H1 119.3 . . ? C2 N1 H1 119.3 . . ? C3 C4 H4A 180.0 . . ? C5 N2 C28 109.67(17) . . ? C5 N2 C6 109.32(15) . . ? C28 N2 C6 108.77(16) . . ? C5 N2 Dy1 106.59(12) . . ? C28 N2 Dy1 111.16(12) . . ? C6 N2 Dy1 111.30(12) . . ? C8 N3 C13 108.57(16) . . ? C8 N3 C7 109.56(16) . . ? C13 N3 C7 108.17(16) . . ? C8 N3 Dy1 107.29(12) . . ? C13 N3 Dy1 111.25(12) . . ? C7 N3 Dy1 111.94(12) . . ? C15 N5 C20 108.90(16) . . ? C15 N5 C14 110.40(17) . . ? C20 N5 C14 108.06(16) . . ? C15 N5 Dy1 106.44(12) . . ? C20 N5 Dy1 112.68(12) . . ? C14 N5 Dy1 110.35(11) . . ? C22 N7 C27 109.46(16) . . ? C22 N7 C21 109.85(16) . . ? C27 N7 C21 108.04(16) . . ? C22 N7 Dy1 106.49(12) . . ? C27 N7 Dy1 111.70(12) . . ? C21 N7 Dy1 111.29(12) . . ? C23 N8 C24 122.05(19) . . ? C23 N8 H8 119.0 . . ? C24 N8 H8 119.0 . . ? C11 C10 N4 110.18(18) . . ? C11 C10 H10A 109.6 . . ? N4 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? N4 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? O1 C1 N1 122.51(19) . . ? O1 C1 C5 120.16(18) . . ? N1 C1 C5 117.31(18) . . ? N1 C2 C3 112.67(19) . . ? N1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 179.7(3) . . ? N2 C5 C1 110.87(16) . . ? N2 C5 H5A 109.5 . . ? C1 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? C1 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? N2 C6 C7 111.08(17) . . ? N2 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N3 C7 C6 112.66(17) . . ? N3 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N3 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N3 C13 C14 110.93(17) . . ? N3 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.0 . . ? N5 C14 C13 113.14(17) . . ? N5 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? N5 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N5 C20 C21 111.28(16) . . ? N5 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? N5 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N7 C21 C20 113.42(17) . . ? N7 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? N7 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? N7 C22 C23 109.50(16) . . ? N7 C22 H22A 109.8 . . ? C23 C22 H22A 109.8 . . ? N7 C22 H22B 109.8 . . ? C23 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? O4 C23 N8 122.4(2) . . ? O4 C23 C22 119.55(18) . . ? N8 C23 C22 118.03(18) . . ? N8 C24 C25 111.7(2) . . ? N8 C24 H24A 109.3 . . ? C25 C24 H24A 109.3 . . ? N8 C24 H24B 109.3 . . ? C25 C24 H24B 109.3 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 179.1(3) . . ? C25 C26 H26 180.0 . . ? N7 C27 C28 110.95(17) . . ? N7 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? N7 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? N2 C28 C27 113.60(17) . . ? N2 C28 H28A 108.8 . . ? C27 C28 H28A 108.8 . . ? N2 C28 H28B 108.8 . . ? C27 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? N5 C15 C16 111.91(16) . . ? N5 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N5 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O3 C16 N6 122.3(2) . . ? O3 C16 C15 120.85(19) . . ? N6 C16 C15 116.88(18) . . ? N6 C17 C18 110.2(2) . . ? N6 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? N6 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C19 C18 C17 179.5(4) . . ? C18 C19 H19 180.0 . . ? N3 C8 C9 111.74(17) . . ? N3 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N3 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? O2 C9 N4 123.08(19) . . ? O2 C9 C8 120.36(17) . . ? N4 C9 C8 116.46(18) . . ? C12 C11 C10 178.6(3) . . ? C11 C12 H12 180.0 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O6 C30 C31 121.9(4) . . ? O6 C30 C29 121.4(4) . . ? C31 C30 C29 116.7(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? 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 N6 H6 O10S 0.88 1.89 2.768(3) 171.9 2_665 O9S H9F O6 0.825(10) 2.210(15) 3.000(4) 160(4) 1_455 N4 H4 O7S 0.88 1.94 2.815(3) 172.7 . O5 H5F O8S 0.822(9) 1.915(11) 2.732(2) 172(3) . N8 H8 Cl3 0.88 2.21 3.079(2) 167.5 1_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.395 _refine_diff_density_min -1.146 _refine_diff_density_rms 0.090 # Attachment '- Nd.txt' data_b10109ap-1 _database_code_depnum_ccdc_archive 'CCDC 814848' #TrackingRef '- Nd.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H42 N8 Nd O5, C3 H6 O, 4(H2 O), 2(Cl H), Cl' _chemical_formula_sum 'C31 H58 Cl3 N8 Nd O10' _chemical_formula_weight 953.44 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' Nd Nd -0.1943 3.0179 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1524(6) _cell_length_b 13.9136(7) _cell_length_c 15.2106(12) _cell_angle_alpha 110.878(3) _cell_angle_beta 103.133(3) _cell_angle_gamma 100.034(2) _cell_volume 2061.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9791 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 23.15 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 982 _exptl_absorpt_coefficient_mu 1.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9254 _exptl_absorpt_correction_T_max 0.9660 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 220951 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.88 _reflns_number_total 9849 _reflns_number_gt 8659 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+2.4190P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9849 _refine_ls_number_parameters 516 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0647 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.005 _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 Nd1 Nd 0.604855(12) 0.622493(10) 0.729238(9) 0.01182(4) Uani 1 1 d . . . Cl1 Cl 0.36350(8) 0.21824(7) 0.76859(6) 0.04033(18) Uani 1 1 d D . . H1G H 0.271(2) 0.173(3) 0.771(3) 0.060 Uiso 1 1 d D . . Cl2 Cl 0.18117(6) 0.66726(5) 0.01134(5) 0.02609(14) Uani 1 1 d D . . H2G H 0.2824(13) 0.675(3) 0.050(2) 0.039 Uiso 1 1 d D . . Cl3 Cl 0.04365(6) 0.64520(6) 0.45621(5) 0.02951(15) Uani 1 1 d . . . N1 N 0.2916(2) 0.52590(17) 0.85229(16) 0.0193(4) Uani 1 1 d . . . H1 H 0.2735 0.5589 0.9067 0.023 Uiso 1 1 calc R . . O7S O 0.5897(2) 0.14514(16) 0.83776(16) 0.0324(5) Uani 1 1 d D . . H7F H 0.646(2) 0.1986(17) 0.881(2) 0.049 Uiso 1 1 d D . . H7E H 0.524(2) 0.167(2) 0.826(3) 0.049 Uiso 1 1 d D . . O1 O 0.43009(16) 0.52790(13) 0.76470(12) 0.0168(3) Uani 1 1 d . . . O8S O 0.81422(19) 0.43133(18) 0.39117(16) 0.0321(5) Uani 1 1 d D . . H8F H 0.872(2) 0.4839(19) 0.401(3) 0.048 Uiso 1 1 d D . . H8E H 0.851(3) 0.401(2) 0.422(2) 0.048 Uiso 1 1 d D . . N8 N 0.6457(2) 0.28127(16) 0.60301(15) 0.0174(4) Uani 1 1 d . . . H8 H 0.6638 0.2382 0.6314 0.021 Uiso 1 1 calc R . . O9S O 0.7125(2) 0.15334(18) 0.69962(16) 0.0340(5) Uani 1 1 d D . . H9F H 0.677(3) 0.149(3) 0.741(2) 0.051 Uiso 1 1 d D . . H9E H 0.7851(16) 0.147(3) 0.718(2) 0.051 Uiso 1 1 d D . . O10S O 0.9268(2) 0.13270(19) 0.93740(17) 0.0395(5) Uani 1 1 d D . . H10E H 0.898(4) 0.185(2) 0.939(3) 0.059 Uiso 1 1 d D . . H10F H 0.950(4) 0.121(3) 0.8866(19) 0.059 Uiso 1 1 d D . . O4 O 0.61689(16) 0.44395(13) 0.62267(12) 0.0158(3) Uani 1 1 d . . . O3 O 0.67121(15) 0.67246(13) 0.60763(12) 0.0156(3) Uani 1 1 d . . . O2 O 0.49105(16) 0.76074(13) 0.75010(13) 0.0180(3) Uani 1 1 d . . . O5 O 0.41412(16) 0.55229(14) 0.58048(13) 0.0173(3) Uani 1 1 d D . . H5E H 0.3442(16) 0.556(2) 0.589(2) 0.026 Uiso 1 1 d D . . H5F H 0.412(3) 0.558(2) 0.5281(13) 0.026 Uiso 1 1 d D . . O6 O -0.0645(3) 0.0879(2) 0.74539(19) 0.0524(6) Uani 1 1 d . . . N3 N 0.75645(18) 0.82631(16) 0.82950(15) 0.0156(4) Uani 1 1 d . . . N2 N 0.60961(19) 0.70749(16) 0.91966(15) 0.0165(4) Uani 1 1 d . . . N7 N 0.70676(19) 0.51837(16) 0.82902(15) 0.0157(4) Uani 1 1 d . . . C24 C 0.6228(2) 0.24449(19) 0.49601(18) 0.0183(5) Uani 1 1 d . . . H24A H 0.6907 0.2893 0.4837 0.022 Uiso 1 1 calc R . . H24B H 0.5393 0.2525 0.4646 0.022 Uiso 1 1 calc R . . N5 N 0.85496(19) 0.63869(16) 0.74121(14) 0.0153(4) Uani 1 1 d . . . N6 N 0.8042(2) 0.69050(16) 0.51947(15) 0.0176(4) Uani 1 1 d . . . H6 H 0.8796 0.6887 0.5114 0.021 Uiso 1 1 calc R . . N4 N 0.4860(2) 0.93307(17) 0.79879(16) 0.0192(4) Uani 1 1 d . . . H4 H 0.5306 1.0007 0.8232 0.023 Uiso 1 1 calc R . . C11 C 0.3114(2) 0.8919(2) 0.8622(2) 0.0233(5) Uani 1 1 d . . . C7 C 0.7813(2) 0.8618(2) 0.93836(18) 0.0189(5) Uani 1 1 d . . . H7A H 0.8134 0.9410 0.9708 0.023 Uiso 1 1 calc R . . H7B H 0.8498 0.8330 0.9642 0.023 Uiso 1 1 calc R . . C6 C 0.6647(2) 0.82669(19) 0.96683(18) 0.0173(5) Uani 1 1 d . . . H6A H 0.6892 0.8521 1.0398 0.021 Uiso 1 1 calc R . . H6B H 0.5984 0.8602 0.9462 0.021 Uiso 1 1 calc R . . C1 C 0.4747(2) 0.6814(2) 0.91903(19) 0.0189(5) Uani 1 1 d . . . H1A H 0.4351 0.7361 0.9078 0.023 Uiso 1 1 calc R . . H1B H 0.4731 0.6839 0.9846 0.023 Uiso 1 1 calc R . . C2 C 0.3966(2) 0.57138(19) 0.83924(18) 0.0162(5) Uani 1 1 d . . . C3 C 0.2046(2) 0.4219(2) 0.77848(19) 0.0222(5) Uani 1 1 d . . . H3A H 0.2540 0.3691 0.7613 0.027 Uiso 1 1 calc R . . H3B H 0.1623 0.4291 0.7174 0.027 Uiso 1 1 calc R . . C4 C 0.1072(2) 0.3841(2) 0.8185(2) 0.0223(5) Uani 1 1 d . . . C5 C 0.0301(3) 0.3556(2) 0.8521(2) 0.0284(6) Uani 1 1 d . . . H5 H -0.0322 0.3327 0.8793 0.034 Uiso 1 1 calc R . . C28 C 0.6873(3) 0.6603(2) 0.97829(18) 0.0210(5) Uani 1 1 d . . . H28A H 0.6627 0.6709 1.0389 0.025 Uiso 1 1 calc R . . H28B H 0.7791 0.6996 0.9992 0.025 Uiso 1 1 calc R . . C27 C 0.6710(2) 0.5417(2) 0.92214(18) 0.0186(5) Uani 1 1 d . . . H27A H 0.7252 0.5165 0.9655 0.022 Uiso 1 1 calc R . . H27B H 0.5805 0.5014 0.9051 0.022 Uiso 1 1 calc R . . C22 C 0.6538(2) 0.40182(19) 0.76552(18) 0.0182(5) Uani 1 1 d . . . H22A H 0.5689 0.3759 0.7716 0.022 Uiso 1 1 calc R . . H22B H 0.7113 0.3632 0.7890 0.022 Uiso 1 1 calc R . . C23 C 0.6398(2) 0.37686(19) 0.65791(18) 0.0152(5) Uani 1 1 d . . . C25 C 0.6224(3) 0.1318(2) 0.45142(19) 0.0230(5) Uani 1 1 d . . . C26 C 0.6217(3) 0.0410(2) 0.4136(2) 0.0308(6) Uani 1 1 d . . . H26 H 0.6212 -0.0318 0.3832 0.037 Uiso 1 1 calc R . . C21 C 0.8497(2) 0.5499(2) 0.85661(18) 0.0186(5) Uani 1 1 d . . . H21A H 0.8823 0.4969 0.8770 0.022 Uiso 1 1 calc R . . H21B H 0.8846 0.6203 0.9143 0.022 Uiso 1 1 calc R . . C20 C 0.8987(2) 0.5574(2) 0.77343(18) 0.0180(5) Uani 1 1 d . . . H20A H 0.9936 0.5774 0.7962 0.022 Uiso 1 1 calc R . . H20B H 0.8672 0.4865 0.7164 0.022 Uiso 1 1 calc R . . C14 C 0.9389(2) 0.74738(19) 0.81362(19) 0.0190(5) Uani 1 1 d . . . H14A H 1.0223 0.7589 0.8008 0.023 Uiso 1 1 calc R . . H14B H 0.9557 0.7502 0.8814 0.023 Uiso 1 1 calc R . . C13 C 0.8818(2) 0.83759(19) 0.80900(19) 0.0189(5) Uani 1 1 d . . . H13A H 0.9426 0.9071 0.8582 0.023 Uiso 1 1 calc R . . H13B H 0.8689 0.8375 0.7424 0.023 Uiso 1 1 calc R . . C15 C 0.8644(2) 0.6190(2) 0.64148(18) 0.0176(5) Uani 1 1 d . . . H15A H 0.8442 0.5409 0.6021 0.021 Uiso 1 1 calc R . . H15B H 0.9535 0.6524 0.6473 0.021 Uiso 1 1 calc R . . C16 C 0.7734(2) 0.66433(18) 0.58820(17) 0.0152(5) Uani 1 1 d . . . C17 C 0.7147(3) 0.7226(2) 0.45624(19) 0.0212(5) Uani 1 1 d . . . H17A H 0.6297 0.6690 0.4285 0.025 Uiso 1 1 calc R . . H17B H 0.7455 0.7229 0.4002 0.025 Uiso 1 1 calc R . . C18 C 0.7007(3) 0.8286(2) 0.50952(19) 0.0220(5) Uani 1 1 d . . . C19 C 0.6866(3) 0.9131(2) 0.5517(2) 0.0282(6) Uani 1 1 d . . . H19 H 0.6753 0.9812 0.5857 0.034 Uiso 1 1 calc R . . C8 C 0.6878(2) 0.89396(19) 0.79342(19) 0.0176(5) Uani 1 1 d . . . H8A H 0.6994 0.8886 0.7294 0.021 Uiso 1 1 calc R . . H8B H 0.7243 0.9698 0.8416 0.021 Uiso 1 1 calc R . . C9 C 0.5463(2) 0.85844(19) 0.78014(17) 0.0158(5) Uani 1 1 d . . . C10 C 0.3475(2) 0.9072(2) 0.7803(2) 0.0235(5) Uani 1 1 d . . . H10A H 0.3053 0.8410 0.7188 0.028 Uiso 1 1 calc R . . H10B H 0.3161 0.9659 0.7700 0.028 Uiso 1 1 calc R . . C12 C 0.2821(3) 0.8776(3) 0.9272(2) 0.0348(7) Uani 1 1 d . . . H12 H 0.2585 0.8660 0.9796 0.042 Uiso 1 1 calc R . . C31 C 0.0750(4) -0.0094(4) 0.6836(4) 0.0749(15) Uani 1 1 d . . . H31A H 0.0863 -0.0234 0.7433 0.112 Uiso 1 1 calc R . . H31B H 0.1591 0.0215 0.6805 0.112 Uiso 1 1 calc R . . H31C H 0.0315 -0.0768 0.6248 0.112 Uiso 1 1 calc R . . C30 C -0.0041(3) 0.0674(3) 0.6869(3) 0.0428(8) Uani 1 1 d . . . C29 C -0.0137(4) 0.1147(3) 0.6112(3) 0.0550(10) Uani 1 1 d . . . H29A H -0.0567 0.1714 0.6278 0.083 Uiso 1 1 calc R . . H29B H -0.0632 0.0585 0.5453 0.083 Uiso 1 1 calc R . . H29C H 0.0726 0.1449 0.6113 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01243(6) 0.01213(6) 0.01113(6) 0.00410(5) 0.00483(4) 0.00406(4) Cl1 0.0427(4) 0.0443(4) 0.0385(4) 0.0158(4) 0.0142(4) 0.0241(4) Cl2 0.0260(3) 0.0256(3) 0.0252(3) 0.0065(3) 0.0125(3) 0.0061(3) Cl3 0.0216(3) 0.0400(4) 0.0364(4) 0.0209(3) 0.0147(3) 0.0129(3) N1 0.0206(10) 0.0207(10) 0.0169(10) 0.0055(9) 0.0116(9) 0.0043(8) O7S 0.0328(11) 0.0208(10) 0.0368(12) 0.0101(9) 0.0036(9) 0.0051(8) O1 0.0175(8) 0.0185(8) 0.0159(8) 0.0064(7) 0.0087(7) 0.0055(7) O8S 0.0214(10) 0.0413(13) 0.0374(12) 0.0193(10) 0.0092(9) 0.0116(9) N8 0.0231(11) 0.0148(10) 0.0152(10) 0.0064(8) 0.0057(8) 0.0072(8) O9S 0.0488(14) 0.0317(11) 0.0321(12) 0.0171(10) 0.0170(10) 0.0223(10) O10S 0.0398(13) 0.0404(13) 0.0327(13) 0.0105(11) 0.0069(10) 0.0134(10) O4 0.0185(8) 0.0159(8) 0.0147(8) 0.0064(7) 0.0059(7) 0.0077(7) O3 0.0141(8) 0.0177(8) 0.0160(8) 0.0070(7) 0.0064(7) 0.0046(6) O2 0.0154(8) 0.0145(8) 0.0223(9) 0.0056(7) 0.0060(7) 0.0042(6) O5 0.0159(8) 0.0209(9) 0.0154(9) 0.0079(7) 0.0043(7) 0.0055(7) O6 0.0607(17) 0.0615(17) 0.0426(15) 0.0227(13) 0.0231(13) 0.0237(14) N3 0.0143(9) 0.0166(10) 0.0156(10) 0.0047(8) 0.0068(8) 0.0053(8) N2 0.0167(10) 0.0166(10) 0.0164(10) 0.0056(8) 0.0065(8) 0.0063(8) N7 0.0195(10) 0.0159(10) 0.0128(10) 0.0050(8) 0.0067(8) 0.0072(8) C24 0.0230(12) 0.0175(12) 0.0154(12) 0.0068(10) 0.0073(10) 0.0065(10) N5 0.0154(9) 0.0165(10) 0.0123(10) 0.0038(8) 0.0041(8) 0.0052(8) N6 0.0182(10) 0.0190(10) 0.0197(11) 0.0094(9) 0.0105(8) 0.0060(8) N4 0.0211(10) 0.0165(10) 0.0233(11) 0.0090(9) 0.0098(9) 0.0081(8) C11 0.0208(12) 0.0223(13) 0.0286(15) 0.0104(11) 0.0096(11) 0.0085(10) C7 0.0187(12) 0.0190(12) 0.0138(12) 0.0023(10) 0.0039(9) 0.0039(9) C6 0.0218(12) 0.0154(11) 0.0120(11) 0.0021(9) 0.0054(9) 0.0061(9) C1 0.0203(12) 0.0191(12) 0.0185(12) 0.0054(10) 0.0111(10) 0.0069(10) C2 0.0182(11) 0.0185(12) 0.0162(12) 0.0097(10) 0.0069(9) 0.0075(9) C3 0.0229(13) 0.0222(13) 0.0209(13) 0.0068(11) 0.0109(11) 0.0042(10) C4 0.0215(13) 0.0202(12) 0.0215(13) 0.0062(11) 0.0049(10) 0.0046(10) C5 0.0260(14) 0.0260(14) 0.0354(16) 0.0140(12) 0.0141(12) 0.0040(11) C28 0.0286(13) 0.0239(13) 0.0119(12) 0.0070(10) 0.0063(10) 0.0115(11) C27 0.0255(13) 0.0217(12) 0.0141(12) 0.0098(10) 0.0089(10) 0.0110(10) C22 0.0251(13) 0.0157(11) 0.0166(12) 0.0080(10) 0.0078(10) 0.0076(10) C23 0.0135(11) 0.0151(11) 0.0166(12) 0.0065(9) 0.0052(9) 0.0029(9) C25 0.0310(14) 0.0224(13) 0.0150(12) 0.0070(10) 0.0065(11) 0.0085(11) C26 0.0491(18) 0.0245(14) 0.0211(14) 0.0092(12) 0.0113(13) 0.0159(13) C21 0.0187(12) 0.0219(12) 0.0153(12) 0.0075(10) 0.0032(10) 0.0092(10) C20 0.0152(11) 0.0209(12) 0.0175(12) 0.0067(10) 0.0048(9) 0.0077(9) C14 0.0121(11) 0.0195(12) 0.0196(13) 0.0034(10) 0.0027(9) 0.0035(9) C13 0.0123(11) 0.0181(12) 0.0207(13) 0.0035(10) 0.0051(9) 0.0003(9) C15 0.0160(11) 0.0213(12) 0.0172(12) 0.0073(10) 0.0078(9) 0.0071(9) C16 0.0159(11) 0.0128(11) 0.0145(11) 0.0033(9) 0.0052(9) 0.0025(9) C17 0.0258(13) 0.0233(13) 0.0165(12) 0.0089(10) 0.0083(10) 0.0080(10) C18 0.0242(13) 0.0241(13) 0.0214(13) 0.0135(11) 0.0073(11) 0.0064(10) C19 0.0376(16) 0.0228(14) 0.0272(15) 0.0115(12) 0.0115(13) 0.0112(12) C8 0.0175(11) 0.0150(11) 0.0206(12) 0.0069(10) 0.0079(10) 0.0042(9) C9 0.0181(11) 0.0177(11) 0.0127(11) 0.0062(9) 0.0061(9) 0.0065(9) C10 0.0195(12) 0.0299(14) 0.0273(14) 0.0149(12) 0.0096(11) 0.0123(11) C12 0.0335(16) 0.0381(17) 0.0383(18) 0.0180(14) 0.0177(14) 0.0101(13) C31 0.051(2) 0.106(4) 0.117(4) 0.081(4) 0.043(3) 0.043(3) C30 0.0410(19) 0.0400(19) 0.047(2) 0.0173(16) 0.0165(16) 0.0088(15) C29 0.068(3) 0.049(2) 0.050(2) 0.0231(19) 0.022(2) 0.011(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 Nd1 O3 2.4108(16) . ? Nd1 O1 2.4315(16) . ? Nd1 O2 2.4516(16) . ? Nd1 O5 2.4722(17) . ? Nd1 O4 2.4823(16) . ? Nd1 N7 2.655(2) . ? Nd1 N2 2.694(2) . ? Nd1 N3 2.702(2) . ? Nd1 N5 2.718(2) . ? Cl1 H1G 1.129(10) . ? Cl2 H2G 1.113(10) . ? N1 C2 1.322(3) . ? N1 C3 1.468(3) . ? N1 H1 0.8800 . ? O7S H7F 0.824(10) . ? O7S H7E 0.847(10) . ? O1 C2 1.254(3) . ? O8S H8F 0.828(10) . ? O8S H8E 0.827(10) . ? N8 C23 1.317(3) . ? N8 C24 1.466(3) . ? N8 H8 0.8800 . ? O9S H9F 0.825(10) . ? O9S H9E 0.825(10) . ? O10S H10E 0.834(10) . ? O10S H10F 0.839(10) . ? O4 C23 1.266(3) . ? O3 C16 1.254(3) . ? O2 C9 1.255(3) . ? O5 H5E 0.825(10) . ? O5 H5F 0.820(10) . ? O6 C30 1.218(4) . ? N3 C8 1.484(3) . ? N3 C7 1.491(3) . ? N3 C13 1.494(3) . ? N2 C1 1.481(3) . ? N2 C6 1.496(3) . ? N2 C28 1.497(3) . ? N7 C22 1.484(3) . ? N7 C21 1.494(3) . ? N7 C27 1.498(3) . ? C24 C25 1.469(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? N5 C15 1.474(3) . ? N5 C14 1.493(3) . ? N5 C20 1.495(3) . ? N6 C16 1.317(3) . ? N6 C17 1.464(3) . ? N6 H6 0.8800 . ? N4 C9 1.316(3) . ? N4 C10 1.460(3) . ? N4 H4 0.8800 . ? C11 C12 1.177(4) . ? C11 C10 1.466(4) . ? C7 C6 1.518(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C1 C2 1.519(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.468(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.176(4) . ? C5 H5 0.9500 . ? C28 C27 1.518(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C22 C23 1.511(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C25 C26 1.185(4) . ? C26 H26 0.9500 . ? C21 C20 1.516(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C14 C13 1.519(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.516(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C18 1.465(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.179(4) . ? C19 H19 0.9500 . ? C8 C9 1.512(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C12 H12 0.9500 . ? C31 C30 1.495(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C30 C29 1.511(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 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 O3 Nd1 O1 146.02(6) . . ? O3 Nd1 O2 86.90(6) . . ? O1 Nd1 O2 84.70(6) . . ? O3 Nd1 O5 73.24(6) . . ? O1 Nd1 O5 72.81(6) . . ? O2 Nd1 O5 73.10(6) . . ? O3 Nd1 O4 82.63(5) . . ? O1 Nd1 O4 87.12(5) . . ? O2 Nd1 O4 147.68(6) . . ? O5 Nd1 O4 74.61(6) . . ? O3 Nd1 N7 129.05(6) . . ? O1 Nd1 N7 73.79(6) . . ? O2 Nd1 N7 139.76(6) . . ? O5 Nd1 N7 128.67(6) . . ? O4 Nd1 N7 65.86(6) . . ? O3 Nd1 N2 141.15(6) . . ? O1 Nd1 N2 65.43(6) . . ? O2 Nd1 N2 71.62(6) . . ? O5 Nd1 N2 126.75(6) . . ? O4 Nd1 N2 131.74(6) . . ? N7 Nd1 N2 68.59(6) . . ? O3 Nd1 N3 74.17(6) . . ? O1 Nd1 N3 129.92(6) . . ? O2 Nd1 N3 64.95(6) . . ? O5 Nd1 N3 127.37(6) . . ? O4 Nd1 N3 138.97(6) . . ? N7 Nd1 N3 103.96(6) . . ? N2 Nd1 N3 67.51(6) . . ? O3 Nd1 N5 65.06(6) . . ? O1 Nd1 N5 141.04(6) . . ? O2 Nd1 N5 129.45(6) . . ? O5 Nd1 N5 129.13(6) . . ? O4 Nd1 N5 72.44(6) . . ? N7 Nd1 N5 67.66(6) . . ? N2 Nd1 N5 104.09(6) . . ? N3 Nd1 N5 67.21(6) . . ? C2 N1 C3 121.8(2) . . ? C2 N1 H1 119.1 . . ? C3 N1 H1 119.1 . . ? H7F O7S H7E 105(2) . . ? C2 O1 Nd1 122.22(15) . . ? H8F O8S H8E 104(2) . . ? C23 N8 C24 122.0(2) . . ? C23 N8 H8 119.0 . . ? C24 N8 H8 119.0 . . ? H9F O9S H9E 107(2) . . ? H10E O10S H10F 100(2) . . ? C23 O4 Nd1 121.26(15) . . ? C16 O3 Nd1 124.57(15) . . ? C9 O2 Nd1 123.37(15) . . ? Nd1 O5 H5E 117.9(19) . . ? Nd1 O5 H5F 126(2) . . ? H5E O5 H5F 106(2) . . ? C8 N3 C7 110.43(18) . . ? C8 N3 C13 108.53(19) . . ? C7 N3 C13 108.93(18) . . ? C8 N3 Nd1 106.78(14) . . ? C7 N3 Nd1 110.91(14) . . ? C13 N3 Nd1 111.22(13) . . ? C1 N2 C6 108.79(18) . . ? C1 N2 C28 110.35(19) . . ? C6 N2 C28 108.80(19) . . ? C1 N2 Nd1 106.67(14) . . ? C6 N2 Nd1 111.89(14) . . ? C28 N2 Nd1 110.32(14) . . ? C22 N7 C21 110.13(18) . . ? C22 N7 C27 108.51(18) . . ? C21 N7 C27 108.34(19) . . ? C22 N7 Nd1 107.98(14) . . ? C21 N7 Nd1 111.42(14) . . ? C27 N7 Nd1 110.42(13) . . ? N8 C24 C25 110.8(2) . . ? N8 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? N8 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C15 N5 C14 109.86(19) . . ? C15 N5 C20 109.78(18) . . ? C14 N5 C20 108.39(18) . . ? C15 N5 Nd1 107.15(13) . . ? C14 N5 Nd1 111.07(13) . . ? C20 N5 Nd1 110.58(14) . . ? C16 N6 C17 120.9(2) . . ? C16 N6 H6 119.5 . . ? C17 N6 H6 119.5 . . ? C9 N4 C10 122.1(2) . . ? C9 N4 H4 119.0 . . ? C10 N4 H4 119.0 . . ? C12 C11 C10 178.8(3) . . ? N3 C7 C6 114.1(2) . . ? N3 C7 H7A 108.7 . . ? C6 C7 H7A 108.7 . . ? N3 C7 H7B 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? N2 C6 C7 111.96(19) . . ? N2 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N2 C1 C2 111.99(19) . . ? N2 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N2 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? O1 C2 N1 122.6(2) . . ? O1 C2 C1 121.1(2) . . ? N1 C2 C1 116.3(2) . . ? N1 C3 C4 109.8(2) . . ? N1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C3 178.7(3) . . ? C4 C5 H5 180.0 . . ? N2 C28 C27 113.9(2) . . ? N2 C28 H28A 108.8 . . ? C27 C28 H28A 108.8 . . ? N2 C28 H28B 108.8 . . ? C27 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? N7 C27 C28 112.3(2) . . ? N7 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? N7 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? N7 C22 C23 111.93(19) . . ? N7 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? N7 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? O4 C23 N8 122.6(2) . . ? O4 C23 C22 120.4(2) . . ? N8 C23 C22 116.9(2) . . ? C26 C25 C24 178.6(3) . . ? C25 C26 H26 180.0 . . ? N7 C21 C20 113.52(19) . . ? N7 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? N7 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? N5 C20 C21 111.25(19) . . ? N5 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? N5 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N5 C14 C13 113.56(19) . . ? N5 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? N5 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? N3 C13 C14 111.7(2) . . ? N3 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N3 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? N5 C15 C16 111.55(19) . . ? N5 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? N5 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? O3 C16 N6 122.4(2) . . ? O3 C16 C15 120.3(2) . . ? N6 C16 C15 117.3(2) . . ? N6 C17 C18 112.8(2) . . ? N6 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? N6 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C19 C18 C17 178.6(3) . . ? C18 C19 H19 180.0 . . ? N3 C8 C9 110.51(19) . . ? N3 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O2 C9 N4 123.0(2) . . ? O2 C9 C8 119.7(2) . . ? N4 C9 C8 117.3(2) . . ? N4 C10 C11 112.4(2) . . ? N4 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? N4 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C11 C12 H12 180.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O6 C30 C31 121.6(4) . . ? O6 C30 C29 120.3(3) . . ? C31 C30 C29 118.0(3) . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 O7S H7E Cl1 0.847(10) 2.156(12) 2.992(2) 169(3) . O7S H7F Cl2 0.824(10) 2.240(10) 3.058(2) 172(3) 2_666 N8 H8 O9S 0.88 1.90 2.777(3) 176.0 . O9S H9F O7S 0.825(10) 1.956(10) 2.780(3) 176(4) . O9S H9E O6 0.825(10) 2.020(15) 2.821(3) 164(4) 1_655 O10S H10F O6 0.839(10) 1.992(18) 2.789(3) 159(4) 1_655 O5 H5E O8S 0.825(10) 1.887(10) 2.712(3) 179(3) 2_666 O5 H5F O4 0.820(10) 2.234(11) 3.051(2) 173(3) 2_666 N4 H4 O7S 0.88 1.92 2.766(3) 161.3 1_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.143 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.101 # Attachment '- Tb.txt' data_b10069ap-1 _database_code_depnum_ccdc_archive 'CCDC 814849' #TrackingRef '- Tb.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H42 N8 O5 Tb, C3 H6 O, 3(H2 O), 2(Cl H), H O, Cl' _chemical_formula_sum 'C31 H57 Cl3 N8 O10 Tb' _chemical_formula_weight 967.12 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' Tb Tb -0.1723 4.1537 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8916(5) _cell_length_b 14.3620(6) _cell_length_c 15.4604(10) _cell_angle_alpha 113.338(2) _cell_angle_beta 103.205(3) _cell_angle_gamma 99.220(2) _cell_volume 2075.04(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9943 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.67 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 990 _exptl_absorpt_coefficient_mu 1.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8179 _exptl_absorpt_correction_T_max 0.9436 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 246235 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.70 _reflns_number_total 10723 _reflns_number_gt 9933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+2.5533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10723 _refine_ls_number_parameters 513 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Tb1 Tb 0.383711(9) 0.370486(7) 0.266009(7) 0.01312(3) Uani 1 1 d . . . Cl1 Cl 0.96212(6) 0.36492(5) 0.54814(5) 0.03005(12) Uani 1 1 d . . . Cl2 Cl 1.02168(6) 0.66259(5) 0.12544(5) 0.03165(12) Uani 1 1 d D . . Cl3 Cl 0.43733(7) 0.85166(5) 0.16382(5) 0.03766(14) Uani 1 1 d D . . O6S O 0.2720(2) 0.82990(15) 0.30128(14) 0.0326(4) Uani 1 1 d D . . H6E H 0.2019(18) 0.791(2) 0.2569(18) 0.049 Uiso 1 1 d D . . H6D H 0.320(3) 0.844(3) 0.271(2) 0.049 Uiso 1 1 d D . . O1 O 0.50924(14) 0.24826(12) 0.25050(11) 0.0193(3) Uani 1 1 d . . . O2 O 0.33170(14) 0.32826(11) 0.38863(11) 0.0169(3) Uani 1 1 d . . . O9S O 0.81152(17) 0.42543(16) 0.38904(15) 0.0336(4) Uani 1 1 d D . . H9E H 0.864(3) 0.4765(19) 0.394(3) 0.050 Uiso 1 1 d D . . H9D H 0.853(3) 0.404(3) 0.425(2) 0.050 Uiso 1 1 d D . . O7S O 0.0594(2) 0.8695(2) 0.09065(18) 0.0530(6) Uani 1 1 d D . . O4 O 0.55506(15) 0.46085(12) 0.23424(11) 0.0188(3) Uani 1 1 d . . . O3 O 0.37274(14) 0.54417(11) 0.37200(11) 0.0174(3) Uani 1 1 d . . . O8S O 0.2188(3) 0.6464(2) 0.00866(19) 0.0603(7) Uani 1 1 d D . . N6 N 0.34903(18) 0.70490(14) 0.39337(13) 0.0186(3) Uani 1 1 d . . . H6 H 0.3316 0.7458 0.3651 0.022 Uiso 1 1 calc R . . O6 O 0.57710(14) 0.44941(12) 0.41409(11) 0.0183(3) Uani 1 1 d D . . H6F H 0.6471(17) 0.442(2) 0.405(2) 0.028 Uiso 1 1 d D . . H6G H 0.572(3) 0.439(2) 0.4616(15) 0.028 Uiso 1 1 d D . . O5 O 0.9262(3) 0.9843(3) 0.2310(3) 0.0754(8) Uani 1 1 d . . . N1 N 0.53180(19) 0.08412(15) 0.20764(15) 0.0236(4) Uani 1 1 d . . . H1 H 0.4934 0.0172 0.1884 0.028 Uiso 1 1 calc R . . N2 N 0.24058(17) 0.17026(14) 0.17342(13) 0.0171(3) Uani 1 1 d . . . N3 N 0.13532(17) 0.35286(14) 0.25772(13) 0.0166(3) Uani 1 1 d . . . N4 N 0.20028(18) 0.31156(14) 0.47822(14) 0.0192(3) Uani 1 1 d . . . H4 H 0.1243 0.3146 0.4882 0.023 Uiso 1 1 calc R . . N5 N 0.27396(17) 0.46188(14) 0.16592(13) 0.0178(3) Uani 1 1 d . . . N7 N 0.37752(17) 0.27808(14) 0.07920(13) 0.0179(3) Uani 1 1 d . . . N8 N 0.69405(19) 0.46449(15) 0.14628(14) 0.0235(4) Uani 1 1 d . . . H8 H 0.7151 0.4304 0.0929 0.028 Uiso 1 1 calc R . . C26 C 0.3764(2) 0.74659(17) 0.50125(16) 0.0204(4) Uani 1 1 d . . . H26A H 0.3040 0.7096 0.5149 0.025 Uiso 1 1 calc R . . H26B H 0.4585 0.7336 0.5310 0.025 Uiso 1 1 calc R . . C1 C 0.4616(2) 0.15218(17) 0.22440(15) 0.0184(4) Uani 1 1 d . . . C2 C 0.6718(2) 0.1164(2) 0.22011(19) 0.0282(5) Uani 1 1 d . . . H2A H 0.7145 0.0656 0.2339 0.034 Uiso 1 1 calc R . . H2B H 0.7134 0.1867 0.2781 0.034 Uiso 1 1 calc R . . C3 C 0.6932(2) 0.12103(19) 0.13138(19) 0.0275(5) Uani 1 1 d . . . C4 C 0.7093(3) 0.1256(2) 0.0599(2) 0.0340(6) Uani 1 1 d . . . H4A H 0.7222 0.1293 0.0025 0.041 Uiso 1 1 calc R . . C5 C 0.3187(2) 0.11173(17) 0.21241(16) 0.0194(4) Uani 1 1 d . . . H5A H 0.2857 0.0354 0.1659 0.023 Uiso 1 1 calc R . . H5B H 0.3097 0.1213 0.2775 0.023 Uiso 1 1 calc R . . C6 C 0.1132(2) 0.15833(17) 0.19391(17) 0.0207(4) Uani 1 1 d . . . H6A H 0.1282 0.1626 0.2612 0.025 Uiso 1 1 calc R . . H6B H 0.0526 0.0880 0.1451 0.025 Uiso 1 1 calc R . . C7 C 0.0506(2) 0.24354(17) 0.18761(17) 0.0222(4) Uani 1 1 d . . . H7A H 0.0300 0.2355 0.1188 0.027 Uiso 1 1 calc R . . H7B H -0.0333 0.2333 0.2019 0.027 Uiso 1 1 calc R . . C8 C 0.1315(2) 0.37807(17) 0.35932(16) 0.0191(4) Uani 1 1 d . . . H8C H 0.0416 0.3465 0.3559 0.023 Uiso 1 1 calc R . . H8D H 0.1532 0.4556 0.3989 0.023 Uiso 1 1 calc R . . C9 C 0.2279(2) 0.33599(16) 0.40989(15) 0.0166(4) Uani 1 1 d . . . C10 C 0.2930(2) 0.27955(19) 0.53795(17) 0.0238(4) Uani 1 1 d . . . H10A H 0.3827 0.3258 0.5584 0.029 Uiso 1 1 calc R . . H10B H 0.2706 0.2894 0.5990 0.029 Uiso 1 1 calc R . . C11 C 0.2919(2) 0.16941(19) 0.48418(18) 0.0258(5) Uani 1 1 d . . . C12 C 0.2907(3) 0.0799(2) 0.4407(2) 0.0352(6) Uani 1 1 d . . . H12 H 0.2898 0.0083 0.4060 0.042 Uiso 1 1 calc R . . C13 C 0.0838(2) 0.42852(17) 0.22594(16) 0.0199(4) Uani 1 1 d . . . H13A H 0.1158 0.5000 0.2829 0.024 Uiso 1 1 calc R . . H13B H -0.0134 0.4069 0.2049 0.024 Uiso 1 1 calc R . . C14 C 0.1275(2) 0.43176(18) 0.14067(16) 0.0210(4) Uani 1 1 d . . . H14A H 0.0897 0.3614 0.0823 0.025 Uiso 1 1 calc R . . H14B H 0.0929 0.4832 0.1220 0.025 Uiso 1 1 calc R . . C15 C 0.3057(2) 0.43306(17) 0.07100(16) 0.0209(4) Uani 1 1 d . . . H15A H 0.3970 0.4730 0.0858 0.025 Uiso 1 1 calc R . . H15B H 0.2463 0.4531 0.0269 0.025 Uiso 1 1 calc R . . C16 C 0.2909(2) 0.31561(17) 0.01806(16) 0.0218(4) Uani 1 1 d . . . H16A H 0.1982 0.2763 0.0002 0.026 Uiso 1 1 calc R . . H16B H 0.3117 0.2994 -0.0445 0.026 Uiso 1 1 calc R . . C17 C 0.5146(2) 0.30727(17) 0.07988(17) 0.0221(4) Uani 1 1 d . . . H17A H 0.5139 0.3021 0.0140 0.027 Uiso 1 1 calc R . . H17B H 0.5597 0.2566 0.0914 0.027 Uiso 1 1 calc R . . C18 C 0.5901(2) 0.41770(17) 0.15915(16) 0.0195(4) Uani 1 1 d . . . C19 C 0.7755(2) 0.57136(19) 0.21807(18) 0.0262(5) Uani 1 1 d . . . H19A H 0.8560 0.5878 0.2012 0.031 Uiso 1 1 calc R . . H19B H 0.8021 0.5759 0.2856 0.031 Uiso 1 1 calc R . . C20 C 0.7018(3) 0.6483(2) 0.21664(19) 0.0328(5) Uani 1 1 d . . . C21 C 0.6414(3) 0.7107(3) 0.2151(2) 0.0423(7) Uani 1 1 d . . . H21 H 0.5935 0.7602 0.2139 0.051 Uiso 1 1 calc R . . C22 C 0.3280(2) 0.16047(17) 0.03349(16) 0.0205(4) Uani 1 1 d . . . H22A H 0.3995 0.1318 0.0551 0.025 Uiso 1 1 calc R . . H22B H 0.3014 0.1312 -0.0399 0.025 Uiso 1 1 calc R . . C23 C 0.2115(2) 0.12623(17) 0.06326(16) 0.0208(4) Uani 1 1 d . . . H23A H 0.1374 0.1491 0.0357 0.025 Uiso 1 1 calc R . . H23B H 0.1835 0.0481 0.0334 0.025 Uiso 1 1 calc R . . C24 C 0.3288(2) 0.57754(17) 0.22848(16) 0.0204(4) Uani 1 1 d . . . H24A H 0.2680 0.6139 0.2061 0.024 Uiso 1 1 calc R . . H24B H 0.4137 0.6014 0.2199 0.024 Uiso 1 1 calc R . . C25 C 0.34973(19) 0.60810(16) 0.33765(15) 0.0172(4) Uani 1 1 d . . . C27 C 0.3898(2) 0.86000(19) 0.54629(17) 0.0267(5) Uani 1 1 d . . . C28 C 0.4029(3) 0.9518(2) 0.5828(2) 0.0417(7) Uani 1 1 d . . . H28 H 0.4134 1.0257 0.6121 0.050 Uiso 1 1 calc R . . C29 C 0.9306(4) 1.0732(4) 0.3974(3) 0.0760(13) Uani 1 1 d . . . H29A H 0.9401 1.1358 0.3855 0.114 Uiso 1 1 calc R . . H29B H 1.0012 1.0878 0.4572 0.114 Uiso 1 1 calc R . . H29C H 0.8454 1.0558 0.4067 0.114 Uiso 1 1 calc R . . C31 C 0.9384(3) 0.9835(3) 0.3112(3) 0.0534(8) Uani 1 1 d . . . C30 C 0.9648(4) 0.8905(3) 0.3271(3) 0.0641(10) Uani 1 1 d . . . H30A H 0.9665 0.8355 0.2648 0.096 Uiso 1 1 calc R . . H30B H 0.8952 0.8621 0.3479 0.096 Uiso 1 1 calc R . . H30C H 1.0497 0.9134 0.3788 0.096 Uiso 1 1 calc R . . H7D H 0.091(5) 0.821(3) 0.091(4) 0.096 Uiso 1 1 d D . . H8E H 0.159(3) 0.648(4) 0.032(3) 0.096 Uiso 1 1 d D . . H8F H 0.278(3) 0.701(2) 0.050(3) 0.096 Uiso 1 1 d D . . H3G H 0.529(3) 0.827(4) 0.182(4) 0.096 Uiso 1 1 d D . . H2G H 0.949(4) 0.642(4) 0.162(3) 0.096 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 Tb1 0.01326(5) 0.01356(5) 0.01161(5) 0.00381(3) 0.00517(3) 0.00462(3) Cl1 0.0234(3) 0.0369(3) 0.0346(3) 0.0156(3) 0.0163(2) 0.0123(2) Cl2 0.0303(3) 0.0350(3) 0.0300(3) 0.0149(3) 0.0108(2) 0.0077(2) Cl3 0.0515(4) 0.0244(3) 0.0323(3) 0.0108(3) 0.0113(3) 0.0066(3) O6S 0.0390(10) 0.0280(9) 0.0260(9) 0.0115(8) 0.0030(8) 0.0095(8) O1 0.0175(7) 0.0167(7) 0.0204(7) 0.0050(6) 0.0060(6) 0.0054(6) O2 0.0147(6) 0.0196(7) 0.0169(7) 0.0072(6) 0.0072(5) 0.0057(5) O9S 0.0211(8) 0.0396(11) 0.0372(10) 0.0150(9) 0.0081(8) 0.0089(7) O7S 0.0482(13) 0.0552(15) 0.0456(13) 0.0302(12) -0.0042(10) -0.0029(11) O4 0.0204(7) 0.0202(7) 0.0166(7) 0.0069(6) 0.0098(6) 0.0057(6) O3 0.0184(7) 0.0169(7) 0.0162(7) 0.0066(6) 0.0047(6) 0.0069(6) O8S 0.0568(15) 0.0471(14) 0.0486(14) -0.0049(11) 0.0338(12) -0.0127(11) N6 0.0232(9) 0.0163(8) 0.0160(8) 0.0065(7) 0.0061(7) 0.0073(7) O6 0.0156(7) 0.0227(7) 0.0154(7) 0.0073(6) 0.0047(6) 0.0055(6) O5 0.079(2) 0.084(2) 0.082(2) 0.0490(19) 0.0357(17) 0.0304(17) N1 0.0234(9) 0.0206(9) 0.0280(10) 0.0100(8) 0.0096(8) 0.0103(7) N2 0.0155(8) 0.0166(8) 0.0167(8) 0.0049(7) 0.0055(6) 0.0042(6) N3 0.0158(8) 0.0181(8) 0.0143(8) 0.0054(7) 0.0049(6) 0.0059(6) N4 0.0197(8) 0.0221(9) 0.0202(9) 0.0098(7) 0.0115(7) 0.0092(7) N5 0.0206(8) 0.0188(8) 0.0131(8) 0.0054(7) 0.0058(7) 0.0070(7) N7 0.0201(8) 0.0179(8) 0.0149(8) 0.0049(7) 0.0071(7) 0.0075(7) N8 0.0254(9) 0.0252(10) 0.0211(9) 0.0076(8) 0.0148(8) 0.0068(8) C26 0.0233(10) 0.0197(10) 0.0157(10) 0.0050(8) 0.0071(8) 0.0060(8) C1 0.0205(10) 0.0202(10) 0.0142(9) 0.0064(8) 0.0064(8) 0.0080(8) C2 0.0218(11) 0.0319(12) 0.0301(12) 0.0112(10) 0.0074(9) 0.0141(9) C3 0.0198(10) 0.0242(11) 0.0327(13) 0.0076(10) 0.0062(9) 0.0083(9) C4 0.0317(13) 0.0337(14) 0.0357(14) 0.0121(11) 0.0132(11) 0.0125(11) C5 0.0201(10) 0.0174(9) 0.0210(10) 0.0082(8) 0.0076(8) 0.0061(8) C6 0.0171(9) 0.0177(10) 0.0227(10) 0.0051(8) 0.0076(8) 0.0018(8) C7 0.0143(9) 0.0211(10) 0.0233(11) 0.0048(9) 0.0030(8) 0.0030(8) C8 0.0186(9) 0.0226(10) 0.0186(10) 0.0082(8) 0.0098(8) 0.0096(8) C9 0.0168(9) 0.0139(9) 0.0152(9) 0.0029(7) 0.0057(7) 0.0032(7) C10 0.0272(11) 0.0288(12) 0.0190(10) 0.0117(9) 0.0097(9) 0.0113(9) C11 0.0252(11) 0.0297(12) 0.0283(12) 0.0170(10) 0.0107(9) 0.0098(9) C12 0.0378(14) 0.0301(13) 0.0430(15) 0.0182(12) 0.0156(12) 0.0143(11) C13 0.0174(9) 0.0231(10) 0.0198(10) 0.0086(8) 0.0058(8) 0.0104(8) C14 0.0192(10) 0.0254(11) 0.0177(10) 0.0092(9) 0.0039(8) 0.0089(8) C15 0.0290(11) 0.0226(10) 0.0150(9) 0.0093(8) 0.0093(8) 0.0114(9) C16 0.0298(11) 0.0217(10) 0.0126(9) 0.0056(8) 0.0067(8) 0.0098(9) C17 0.0247(10) 0.0211(10) 0.0209(10) 0.0063(9) 0.0128(9) 0.0076(8) C18 0.0215(10) 0.0226(10) 0.0177(10) 0.0094(8) 0.0093(8) 0.0094(8) C19 0.0241(11) 0.0277(12) 0.0236(11) 0.0090(10) 0.0105(9) 0.0017(9) C20 0.0395(14) 0.0327(13) 0.0262(12) 0.0138(11) 0.0136(11) 0.0042(11) C21 0.0517(18) 0.0464(17) 0.0379(16) 0.0249(14) 0.0185(14) 0.0153(14) C22 0.0265(10) 0.0164(9) 0.0140(9) 0.0024(8) 0.0065(8) 0.0061(8) C23 0.0216(10) 0.0184(10) 0.0157(10) 0.0034(8) 0.0039(8) 0.0033(8) C24 0.0281(11) 0.0168(10) 0.0156(10) 0.0061(8) 0.0068(8) 0.0082(8) C25 0.0137(8) 0.0195(10) 0.0166(9) 0.0061(8) 0.0051(7) 0.0051(7) C27 0.0321(12) 0.0254(12) 0.0175(10) 0.0054(9) 0.0067(9) 0.0085(9) C28 0.0578(19) 0.0265(13) 0.0293(14) 0.0045(11) 0.0079(13) 0.0126(13) C29 0.046(2) 0.067(3) 0.078(3) 0.002(2) 0.007(2) 0.0175(19) C31 0.0356(16) 0.053(2) 0.068(2) 0.0250(18) 0.0186(16) 0.0074(14) C30 0.061(2) 0.048(2) 0.076(3) 0.022(2) 0.025(2) 0.0085(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O4 2.3572(15) . ? Tb1 O2 2.3609(14) . ? Tb1 O1 2.3650(15) . ? Tb1 O3 2.4224(14) . ? Tb1 O6 2.4369(15) . ? Tb1 N5 2.6102(18) . ? Tb1 N7 2.6368(17) . ? Tb1 N3 2.6450(17) . ? Tb1 N2 2.6516(17) . ? Cl2 H2G 1.139(10) . ? Cl3 H3G 1.125(10) . ? O6S H6E 0.828(10) . ? O6S H6D 0.828(10) . ? O1 C1 1.253(3) . ? O2 C9 1.257(2) . ? O9S H9E 0.823(10) . ? O9S H9D 0.823(10) . ? O7S H7D 0.821(10) . ? O4 C18 1.259(3) . ? O3 C25 1.260(3) . ? O8S H8E 0.818(10) . ? O8S H8F 0.826(10) . ? N6 C25 1.316(3) . ? N6 C26 1.468(3) . ? N6 H6 0.8800 . ? O6 H6F 0.822(10) . ? O6 H6G 0.819(9) . ? O5 C31 1.222(5) . ? N1 C1 1.318(3) . ? N1 C2 1.465(3) . ? N1 H1 0.8800 . ? N2 C5 1.480(3) . ? N2 C6 1.491(3) . ? N2 C23 1.496(3) . ? N3 C8 1.478(3) . ? N3 C7 1.491(3) . ? N3 C13 1.493(3) . ? N4 C9 1.317(3) . ? N4 C10 1.464(3) . ? N4 H4 0.8800 . ? N5 C24 1.482(3) . ? N5 C15 1.497(3) . ? N5 C14 1.498(3) . ? N7 C17 1.481(3) . ? N7 C22 1.494(3) . ? N7 C16 1.494(3) . ? N8 C18 1.319(3) . ? N8 C19 1.462(3) . ? N8 H8 0.8800 . ? C26 C27 1.462(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C1 C5 1.512(3) . ? C2 C3 1.468(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.183(4) . ? C4 H4A 0.9500 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.518(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.511(3) . ? C8 H8C 0.9900 . ? C8 H8D 0.9900 . ? C10 C11 1.463(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.188(4) . ? C12 H12 0.9500 . ? C13 C14 1.515(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.517(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.508(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.470(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.198(4) . ? C21 H21 0.9500 . ? C22 C23 1.520(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.516(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C27 C28 1.179(4) . ? C28 H28 0.9500 . ? C29 C31 1.473(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C30 1.509(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 O4 Tb1 O2 142.94(5) . . ? O4 Tb1 O1 83.10(5) . . ? O2 Tb1 O1 85.42(5) . . ? O4 Tb1 O3 85.79(5) . . ? O2 Tb1 O3 83.37(5) . . ? O1 Tb1 O3 144.37(5) . . ? O4 Tb1 O6 71.69(5) . . ? O2 Tb1 O6 71.24(5) . . ? O1 Tb1 O6 71.95(5) . . ? O3 Tb1 O6 72.42(5) . . ? O4 Tb1 N5 74.30(5) . . ? O2 Tb1 N5 131.57(5) . . ? O1 Tb1 N5 139.94(5) . . ? O3 Tb1 N5 67.04(5) . . ? O6 Tb1 N5 128.10(5) . . ? O4 Tb1 N7 66.97(5) . . ? O2 Tb1 N7 140.46(5) . . ? O1 Tb1 N7 71.63(5) . . ? O3 Tb1 N7 133.19(5) . . ? O6 Tb1 N7 127.07(5) . . ? N5 Tb1 N7 69.20(5) . . ? O4 Tb1 N3 141.93(5) . . ? O2 Tb1 N3 66.68(5) . . ? O1 Tb1 N3 131.57(5) . . ? O3 Tb1 N3 73.14(5) . . ? O6 Tb1 N3 127.66(5) . . ? N5 Tb1 N3 68.41(5) . . ? N7 Tb1 N3 105.24(5) . . ? O4 Tb1 N2 131.51(5) . . ? O2 Tb1 N2 73.23(5) . . ? O1 Tb1 N2 66.07(5) . . ? O3 Tb1 N2 140.25(5) . . ? O6 Tb1 N2 126.15(5) . . ? N5 Tb1 N2 105.75(6) . . ? N7 Tb1 N2 68.17(5) . . ? N3 Tb1 N2 68.25(5) . . ? H6E O6S H6D 104(2) . . ? C1 O1 Tb1 123.89(13) . . ? C9 O2 Tb1 123.19(13) . . ? H9E O9S H9D 106(2) . . ? C18 O4 Tb1 122.57(14) . . ? C25 O3 Tb1 121.08(13) . . ? H8E O8S H8F 104(2) . . ? C25 N6 C26 121.96(18) . . ? C25 N6 H6 119.0 . . ? C26 N6 H6 119.0 . . ? Tb1 O6 H6F 116.6(19) . . ? Tb1 O6 H6G 118(2) . . ? H6F O6 H6G 109(2) . . ? C1 N1 C2 122.0(2) . . ? C1 N1 H1 119.0 . . ? C2 N1 H1 119.0 . . ? C5 N2 C6 109.41(16) . . ? C5 N2 C23 110.15(16) . . ? C6 N2 C23 108.14(16) . . ? C5 N2 Tb1 106.47(12) . . ? C6 N2 Tb1 111.41(12) . . ? C23 N2 Tb1 111.25(12) . . ? C8 N3 C7 109.52(17) . . ? C8 N3 C13 109.14(16) . . ? C7 N3 C13 108.80(16) . . ? C8 N3 Tb1 106.68(12) . . ? C7 N3 Tb1 111.26(12) . . ? C13 N3 Tb1 111.40(12) . . ? C9 N4 C10 121.54(18) . . ? C9 N4 H4 119.2 . . ? C10 N4 H4 119.2 . . ? C24 N5 C15 108.52(16) . . ? C24 N5 C14 109.87(17) . . ? C15 N5 C14 108.21(16) . . ? C24 N5 Tb1 107.33(12) . . ? C15 N5 Tb1 110.89(12) . . ? C14 N5 Tb1 111.97(12) . . ? C17 N7 C22 108.82(16) . . ? C17 N7 C16 110.61(17) . . ? C22 N7 C16 108.08(16) . . ? C17 N7 Tb1 106.43(12) . . ? C22 N7 Tb1 112.62(12) . . ? C16 N7 Tb1 110.28(12) . . ? C18 N8 C19 121.93(19) . . ? C18 N8 H8 119.0 . . ? C19 N8 H8 119.0 . . ? C27 C26 N6 110.29(18) . . ? C27 C26 H26A 109.6 . . ? N6 C26 H26A 109.6 . . ? C27 C26 H26B 109.6 . . ? N6 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? O1 C1 N1 122.5(2) . . ? O1 C1 C5 119.45(18) . . ? N1 C1 C5 118.06(19) . . ? N1 C2 C3 111.9(2) . . ? N1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? N1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C2 179.1(3) . . ? C3 C4 H4A 180.0 . . ? N2 C5 C1 109.60(17) . . ? N2 C5 H5A 109.7 . . ? C1 C5 H5A 109.7 . . ? N2 C5 H5B 109.7 . . ? C1 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N2 C6 C7 111.17(17) . . ? N2 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N3 C7 C6 113.49(17) . . ? N3 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N3 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N3 C8 C9 110.84(16) . . ? N3 C8 H8C 109.5 . . ? C9 C8 H8C 109.5 . . ? N3 C8 H8D 109.5 . . ? C9 C8 H8D 109.5 . . ? H8C C8 H8D 108.1 . . ? O2 C9 N4 122.32(19) . . ? O2 C9 C8 120.31(18) . . ? N4 C9 C8 117.34(18) . . ? C11 C10 N4 112.63(19) . . ? C11 C10 H10A 109.1 . . ? N4 C10 H10A 109.1 . . ? C11 C10 H10B 109.1 . . ? N4 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C12 C11 C10 179.7(3) . . ? C11 C12 H12 180.0 . . ? N3 C13 C14 111.05(17) . . ? N3 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? N3 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N5 C14 C13 112.74(17) . . ? N5 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? N5 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N5 C15 C16 111.22(17) . . ? N5 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N5 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N7 C16 C15 113.20(17) . . ? N7 C16 H16A 108.9 . . ? C15 C16 H16A 108.9 . . ? N7 C16 H16B 108.9 . . ? C15 C16 H16B 108.9 . . ? H16A C16 H16B 107.8 . . ? N7 C17 C18 112.09(17) . . ? N7 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? N7 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? O4 C18 N8 122.6(2) . . ? O4 C18 C17 120.58(19) . . ? N8 C18 C17 116.76(19) . . ? N8 C19 C20 110.0(2) . . ? N8 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? N8 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C21 C20 C19 179.7(4) . . ? C20 C21 H21 180.0 . . ? N7 C22 C23 111.33(17) . . ? N7 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? N7 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? N2 C23 C22 113.36(17) . . ? N2 C23 H23A 108.9 . . ? C22 C23 H23A 108.9 . . ? N2 C23 H23B 108.9 . . ? C22 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N5 C24 C25 111.83(17) . . ? N5 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? N5 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? O3 C25 N6 123.09(19) . . ? O3 C25 C24 120.30(18) . . ? N6 C25 C24 116.52(18) . . ? C28 C27 C26 178.8(3) . . ? C27 C28 H28 180.0 . . ? C31 C29 H29A 109.5 . . ? C31 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C31 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O5 C31 C29 122.0(4) . . ? O5 C31 C30 121.3(4) . . ? C29 C31 C30 116.7(4) . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 N6 H6 O6S 0.88 1.94 2.813(3) 173.3 . O6 H6F O9S 0.822(10) 1.901(10) 2.723(2) 178(3) . N1 H1 Cl3 0.88 2.21 3.074(2) 167.2 1_545 N8 H8 O8S 0.88 1.90 2.771(3) 171.1 2_665 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.591 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.084 # Attachment '- Yb.txt' data_b10110ap-1 _database_code_depnum_ccdc_archive 'CCDC 814850' #TrackingRef '- Yb.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H41 N8 O5 Yb, C3 H6 O, H2 O, Cl H, 3(H O), 2(Cl)' _chemical_formula_sum 'C31 H53 Cl3 N8 O10 Yb' _chemical_formula_weight 977.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8858(5) _cell_length_b 14.3185(6) _cell_length_c 15.4483(7) _cell_angle_alpha 113.484(2) _cell_angle_beta 102.767(2) _cell_angle_gamma 99.404(2) _cell_volume 2067.00(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9780 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 20.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 2.516 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8909 _exptl_absorpt_correction_T_max 0.9514 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 278130 _diffrn_reflns_av_R_equivalents 0.1154 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10268 _reflns_number_gt 8829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+5.1339P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10268 _refine_ls_number_parameters 501 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.379954(13) 0.370491(11) 0.262747(10) 0.01217(4) Uani 1 1 d . . . Cl1 Cl 0.96424(9) 0.36553(8) 0.54806(7) 0.0286(2) Uani 1 1 d . . . Cl2 Cl 0.02183(9) 0.66335(8) 0.12685(7) 0.0301(2) Uani 1 1 d D . . H2G H -0.049(3) 0.641(3) 0.164(3) 0.045 Uiso 1 1 d D . . Cl3 Cl 0.43906(11) 0.85410(7) 0.16410(7) 0.0344(2) Uani 1 1 d . . . O7S O 0.2714(3) 0.8297(2) 0.30116(19) 0.0295(6) Uani 1 1 d D . . H7E H 0.313(4) 0.845(4) 0.268(3) 0.044 Uiso 1 1 d D . . O1 O 0.5497(2) 0.45915(17) 0.23323(16) 0.0164(5) Uani 1 1 d . . . O8S O 0.8097(2) 0.4224(2) 0.3881(2) 0.0308(6) Uani 1 1 d D . . H8E H 0.865(4) 0.475(2) 0.398(4) 0.046 Uiso 1 1 d D . . O2 O 0.5046(2) 0.25283(17) 0.24948(16) 0.0165(5) Uani 1 1 d . . . O3 O 0.3328(2) 0.33141(17) 0.38497(16) 0.0147(4) Uani 1 1 d . . . O9S O 0.9395(3) 0.1297(3) 0.9089(3) 0.0509(9) Uani 1 1 d D . . H9E H 0.918(6) 0.181(3) 0.905(5) 0.076 Uiso 1 1 d D . . O10S O 0.2200(4) 0.6474(3) 0.0087(3) 0.0549(10) Uani 1 1 d D . . H10E H 0.157(4) 0.640(4) 0.029(4) 0.082 Uiso 1 1 d D . . H10F H 0.270(4) 0.706(2) 0.050(3) 0.082 Uiso 1 1 d D . . N7 N 0.3501(3) 0.7035(2) 0.39181(19) 0.0166(5) Uani 1 1 d . . . H7 H 0.3341 0.7451 0.3641 0.020 Uiso 1 1 calc R . . O4 O 0.3720(2) 0.54099(17) 0.36776(16) 0.0158(4) Uani 1 1 d . . . O5 O 0.5706(2) 0.45031(18) 0.40968(17) 0.0175(5) Uani 1 1 d D . . H5E H 0.640(2) 0.438(3) 0.404(3) 0.026 Uiso 1 1 d D . . O6 O 0.9238(5) 0.9827(4) 0.2300(4) 0.0799(13) Uani 1 1 d . . . N1 N 0.3750(3) 0.2763(2) 0.0781(2) 0.0166(5) Uani 1 1 d . . . N2 N 0.2384(3) 0.1717(2) 0.17354(19) 0.0156(5) Uani 1 1 d . . . N3 N 0.5321(3) 0.0897(2) 0.2108(2) 0.0216(6) Uani 1 1 d . . . H3 H 0.4951 0.0225 0.1927 0.026 Uiso 1 1 calc R . . N4 N 0.1358(3) 0.3550(2) 0.25669(19) 0.0145(5) Uani 1 1 d . . . N5 N 0.2040(3) 0.3152(2) 0.4775(2) 0.0179(6) Uani 1 1 d . . . H5 H 0.1285 0.3184 0.4886 0.022 Uiso 1 1 calc R . . N6 N 0.2747(3) 0.4607(2) 0.1637(2) 0.0168(5) Uani 1 1 d . . . C28 C 0.3303(3) 0.5769(3) 0.2262(2) 0.0180(7) Uani 1 1 d . . . H28A H 0.2700 0.6138 0.2043 0.022 Uiso 1 1 calc R . . H28B H 0.4153 0.6006 0.2174 0.022 Uiso 1 1 calc R . . N8 N 0.6924(3) 0.4639(2) 0.1472(2) 0.0216(6) Uani 1 1 d . . . H8 H 0.7149 0.4300 0.0942 0.026 Uiso 1 1 calc R . . C1 C 0.5867(3) 0.4161(3) 0.1584(2) 0.0172(6) Uani 1 1 d . . . C2 C 0.5127(3) 0.3058(3) 0.0791(3) 0.0206(7) Uani 1 1 d . . . H2A H 0.5130 0.3009 0.0134 0.025 Uiso 1 1 calc R . . H2B H 0.5574 0.2549 0.0905 0.025 Uiso 1 1 calc R . . C3 C 0.3256(3) 0.1585(3) 0.0333(2) 0.0195(7) Uani 1 1 d . . . H3A H 0.3967 0.1300 0.0554 0.023 Uiso 1 1 calc R . . H3B H 0.2998 0.1283 -0.0401 0.023 Uiso 1 1 calc R . . C4 C 0.2090(3) 0.1250(3) 0.0631(2) 0.0187(7) Uani 1 1 d . . . H4A H 0.1350 0.1473 0.0349 0.022 Uiso 1 1 calc R . . H4B H 0.1813 0.0467 0.0345 0.022 Uiso 1 1 calc R . . C5 C 0.3172(3) 0.1143(3) 0.2138(2) 0.0175(6) Uani 1 1 d . . . H5A H 0.2857 0.0374 0.1679 0.021 Uiso 1 1 calc R . . H5B H 0.3077 0.1246 0.2790 0.021 Uiso 1 1 calc R . . C6 C 0.4594(3) 0.1565(3) 0.2258(2) 0.0163(6) Uani 1 1 d . . . C7 C 0.6715(3) 0.1232(3) 0.2233(3) 0.0254(8) Uani 1 1 d . . . H7C H 0.7157 0.0745 0.2398 0.030 Uiso 1 1 calc R . . H7D H 0.7114 0.1953 0.2794 0.030 Uiso 1 1 calc R . . C8 C 0.6928(3) 0.1239(3) 0.1326(3) 0.0253(8) Uani 1 1 d . . . C9 C 0.7095(4) 0.1261(3) 0.0603(3) 0.0328(9) Uani 1 1 d . . . H9 H 0.7228 0.1278 0.0022 0.039 Uiso 1 1 calc R . . C10 C 0.1111(3) 0.1599(3) 0.1945(2) 0.0189(7) Uani 1 1 d . . . H10A H 0.1258 0.1649 0.2620 0.023 Uiso 1 1 calc R . . H10B H 0.0505 0.0892 0.1460 0.023 Uiso 1 1 calc R . . C11 C 0.0495(3) 0.2452(3) 0.1877(3) 0.0204(7) Uani 1 1 d . . . H11A H 0.0286 0.2360 0.1186 0.024 Uiso 1 1 calc R . . H11B H -0.0340 0.2362 0.2031 0.024 Uiso 1 1 calc R . . C12 C 0.1333(3) 0.3815(3) 0.3592(2) 0.0175(7) Uani 1 1 d . . . H12A H 0.0439 0.3502 0.3570 0.021 Uiso 1 1 calc R . . H12B H 0.1555 0.4594 0.3984 0.021 Uiso 1 1 calc R . . C13 C 0.2300(3) 0.3394(2) 0.4087(2) 0.0142(6) Uani 1 1 d . . . C14 C 0.2973(3) 0.2832(3) 0.5364(3) 0.0218(7) Uani 1 1 d . . . H14A H 0.2768 0.2948 0.5986 0.026 Uiso 1 1 calc R . . H14B H 0.3870 0.3286 0.5548 0.026 Uiso 1 1 calc R . . C15 C 0.2941(3) 0.1717(3) 0.4831(3) 0.0239(7) Uani 1 1 d . . . C16 C 0.2916(4) 0.0815(3) 0.4402(3) 0.0322(9) Uani 1 1 d . . . H16 H 0.2896 0.0093 0.4058 0.039 Uiso 1 1 calc R . . C17 C 0.0842(3) 0.4307(3) 0.2251(2) 0.0184(7) Uani 1 1 d . . . H17A H 0.1171 0.5029 0.2816 0.022 Uiso 1 1 calc R . . H17B H -0.0128 0.4095 0.2050 0.022 Uiso 1 1 calc R . . C18 C 0.1277(3) 0.4316(3) 0.1385(2) 0.0194(7) Uani 1 1 d . . . H18A H 0.0891 0.3606 0.0807 0.023 Uiso 1 1 calc R . . H18B H 0.0942 0.4832 0.1194 0.023 Uiso 1 1 calc R . . C19 C 0.3505(3) 0.6065(3) 0.3352(2) 0.0151(6) Uani 1 1 d . . . C20 C 0.3752(3) 0.7449(3) 0.4995(2) 0.0189(7) Uani 1 1 d . . . H20A H 0.3022 0.7072 0.5125 0.023 Uiso 1 1 calc R . . H20B H 0.4570 0.7321 0.5296 0.023 Uiso 1 1 calc R . . C21 C 0.3878(4) 0.8588(3) 0.5451(3) 0.0242(8) Uani 1 1 d . . . C22 C 0.4003(5) 0.9505(3) 0.5814(3) 0.0394(10) Uani 1 1 d . . . H22 H 0.4104 1.0247 0.6108 0.047 Uiso 1 1 calc R . . C23 C 0.3058(3) 0.4313(3) 0.0684(2) 0.0194(7) Uani 1 1 d . . . H23A H 0.3972 0.4708 0.0824 0.023 Uiso 1 1 calc R . . H23B H 0.2466 0.4515 0.0246 0.023 Uiso 1 1 calc R . . C24 C 0.2897(4) 0.3134(3) 0.0159(2) 0.0207(7) Uani 1 1 d . . . H24A H 0.1968 0.2745 -0.0020 0.025 Uiso 1 1 calc R . . H24B H 0.3116 0.2964 -0.0466 0.025 Uiso 1 1 calc R . . C25 C 0.7735(3) 0.5713(3) 0.2196(3) 0.0241(7) Uani 1 1 d . . . H25A H 0.8549 0.5878 0.2034 0.029 Uiso 1 1 calc R . . H25B H 0.7985 0.5754 0.2870 0.029 Uiso 1 1 calc R . . C26 C 0.7012(4) 0.6495(3) 0.2186(3) 0.0285(8) Uani 1 1 d . . . C27 C 0.6423(4) 0.7136(4) 0.2179(3) 0.0392(10) Uani 1 1 d . . . H27 H 0.5958 0.7641 0.2173 0.047 Uiso 1 1 calc R . . C31 C 0.9329(5) 1.0777(5) 0.3967(5) 0.080(2) Uani 1 1 d . . . H31A H 0.9442 1.1393 0.3831 0.120 Uiso 1 1 calc R . . H31B H 1.0034 1.0927 0.4564 0.120 Uiso 1 1 calc R . . H31C H 0.8479 1.0629 0.4074 0.120 Uiso 1 1 calc R . . C29 C 0.9379(5) 0.9846(4) 0.3112(5) 0.0547(13) Uani 1 1 d . . . C30 C 0.9649(6) 0.8922(4) 0.3293(5) 0.0680(16) Uani 1 1 d . . . H30A H 0.9610 0.8341 0.2666 0.102 Uiso 1 1 calc R . . H30B H 0.8988 0.8677 0.3553 0.102 Uiso 1 1 calc R . . H30C H 1.0523 0.9151 0.3777 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01272(6) 0.01197(7) 0.01132(6) 0.00363(5) 0.00515(5) 0.00465(5) Cl1 0.0224(4) 0.0346(5) 0.0330(5) 0.0144(4) 0.0153(4) 0.0117(4) Cl2 0.0277(5) 0.0339(5) 0.0289(5) 0.0145(4) 0.0098(4) 0.0071(4) Cl3 0.0481(6) 0.0215(5) 0.0291(5) 0.0097(4) 0.0098(4) 0.0062(4) O7S 0.0395(16) 0.0235(14) 0.0233(14) 0.0102(11) 0.0063(12) 0.0096(12) O1 0.0197(11) 0.0152(11) 0.0150(11) 0.0057(9) 0.0084(9) 0.0054(9) O8S 0.0160(12) 0.0349(16) 0.0347(15) 0.0114(13) 0.0061(11) 0.0043(11) O2 0.0171(11) 0.0129(11) 0.0181(11) 0.0047(9) 0.0062(9) 0.0059(9) O3 0.0138(10) 0.0170(11) 0.0153(11) 0.0071(9) 0.0072(9) 0.0059(9) O9S 0.0441(19) 0.050(2) 0.0457(19) 0.0270(17) -0.0082(15) -0.0042(16) O10S 0.050(2) 0.042(2) 0.045(2) -0.0061(16) 0.0301(17) -0.0115(16) N7 0.0226(14) 0.0133(13) 0.0140(13) 0.0053(11) 0.0065(11) 0.0067(11) O4 0.0180(11) 0.0145(11) 0.0152(11) 0.0055(9) 0.0059(9) 0.0079(9) O5 0.0138(11) 0.0186(12) 0.0185(12) 0.0059(10) 0.0057(9) 0.0063(9) O6 0.085(3) 0.094(3) 0.082(3) 0.053(3) 0.037(3) 0.028(3) N1 0.0209(14) 0.0152(14) 0.0135(13) 0.0049(11) 0.0072(11) 0.0061(11) N2 0.0152(13) 0.0158(14) 0.0148(13) 0.0047(11) 0.0064(11) 0.0054(11) N3 0.0227(15) 0.0163(14) 0.0258(16) 0.0079(13) 0.0088(12) 0.0085(12) N4 0.0147(12) 0.0147(13) 0.0122(13) 0.0039(11) 0.0043(10) 0.0049(10) N5 0.0159(13) 0.0227(15) 0.0188(14) 0.0097(12) 0.0100(11) 0.0076(11) N6 0.0189(13) 0.0171(14) 0.0144(13) 0.0060(11) 0.0063(11) 0.0066(11) C28 0.0255(17) 0.0144(16) 0.0148(16) 0.0064(13) 0.0068(13) 0.0073(13) N8 0.0256(15) 0.0212(15) 0.0191(15) 0.0063(12) 0.0140(12) 0.0070(12) C1 0.0206(16) 0.0209(17) 0.0147(15) 0.0099(14) 0.0073(13) 0.0104(13) C2 0.0241(17) 0.0202(17) 0.0211(17) 0.0081(14) 0.0142(14) 0.0088(14) C3 0.0268(18) 0.0149(16) 0.0143(16) 0.0026(13) 0.0078(14) 0.0080(14) C4 0.0203(16) 0.0151(16) 0.0127(15) 0.0009(13) 0.0014(13) 0.0038(13) C5 0.0201(16) 0.0135(16) 0.0179(16) 0.0058(13) 0.0065(13) 0.0049(13) C6 0.0208(16) 0.0155(16) 0.0104(15) 0.0039(13) 0.0038(12) 0.0067(13) C7 0.0196(17) 0.029(2) 0.0271(19) 0.0106(16) 0.0061(15) 0.0123(15) C8 0.0202(17) 0.0190(18) 0.031(2) 0.0060(16) 0.0052(15) 0.0079(14) C9 0.032(2) 0.029(2) 0.033(2) 0.0092(18) 0.0116(18) 0.0100(17) C10 0.0168(15) 0.0157(16) 0.0177(16) 0.0026(13) 0.0054(13) 0.0007(13) C11 0.0113(15) 0.0204(17) 0.0216(17) 0.0047(14) 0.0018(13) 0.0018(13) C12 0.0158(15) 0.0210(17) 0.0176(16) 0.0074(14) 0.0078(13) 0.0096(13) C13 0.0152(15) 0.0123(15) 0.0117(14) 0.0024(12) 0.0040(12) 0.0033(12) C14 0.0238(17) 0.0267(19) 0.0188(17) 0.0114(15) 0.0098(14) 0.0105(15) C15 0.0223(17) 0.031(2) 0.0276(19) 0.0182(17) 0.0113(15) 0.0124(15) C16 0.034(2) 0.028(2) 0.040(2) 0.0178(19) 0.0141(18) 0.0130(17) C17 0.0160(15) 0.0197(17) 0.0205(17) 0.0082(14) 0.0064(13) 0.0093(13) C18 0.0189(16) 0.0217(17) 0.0159(16) 0.0074(14) 0.0028(13) 0.0079(14) C19 0.0131(14) 0.0164(16) 0.0153(15) 0.0057(13) 0.0049(12) 0.0056(12) C20 0.0194(16) 0.0197(17) 0.0164(16) 0.0067(14) 0.0056(13) 0.0061(13) C21 0.0279(19) 0.0236(19) 0.0140(16) 0.0030(15) 0.0039(14) 0.0074(15) C22 0.057(3) 0.025(2) 0.026(2) 0.0028(18) 0.009(2) 0.016(2) C23 0.0260(17) 0.0209(17) 0.0169(16) 0.0105(14) 0.0097(14) 0.0117(14) C24 0.0311(19) 0.0195(17) 0.0117(15) 0.0060(14) 0.0073(14) 0.0093(15) C25 0.0216(17) 0.0258(19) 0.0239(18) 0.0111(16) 0.0092(14) 0.0020(14) C26 0.033(2) 0.031(2) 0.0218(19) 0.0138(17) 0.0113(16) 0.0028(17) C27 0.044(3) 0.048(3) 0.035(2) 0.026(2) 0.016(2) 0.012(2) C31 0.039(3) 0.071(4) 0.081(4) -0.007(3) 0.008(3) 0.017(3) C29 0.032(2) 0.056(3) 0.074(4) 0.028(3) 0.017(3) 0.010(2) C30 0.064(4) 0.053(3) 0.083(4) 0.027(3) 0.028(3) 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 Yb1 O1 2.303(2) . ? Yb1 O2 2.306(2) . ? Yb1 O3 2.306(2) . ? Yb1 O4 2.361(2) . ? Yb1 O5 2.417(2) . ? Yb1 N6 2.570(3) . ? Yb1 N1 2.608(3) . ? Yb1 N4 2.609(3) . ? Yb1 N2 2.622(3) . ? Yb1 C1 3.171(3) . ? Yb1 C13 3.183(3) . ? Yb1 C6 3.186(3) . ? Cl2 H2G 1.131(10) . ? O7S H7E 0.821(10) . ? O1 C1 1.264(4) . ? O8S H8E 0.822(10) . ? O2 C6 1.255(4) . ? O3 C13 1.260(4) . ? O9S H9E 0.823(10) . ? O10S H10E 0.823(10) . ? O10S H10F 0.826(10) . ? N7 C19 1.315(4) . ? N7 C20 1.468(4) . ? N7 H7 0.8800 . ? O4 C19 1.258(4) . ? O5 H5E 0.818(10) . ? O6 C29 1.218(7) . ? N1 C2 1.485(4) . ? N1 C3 1.491(4) . ? N1 C24 1.497(4) . ? N2 C5 1.484(4) . ? N2 C10 1.490(4) . ? N2 C4 1.496(4) . ? N3 C6 1.322(4) . ? N3 C7 1.459(4) . ? N3 H3 0.8800 . ? N4 C12 1.481(4) . ? N4 C17 1.493(4) . ? N4 C11 1.493(4) . ? N5 C13 1.314(4) . ? N5 C14 1.464(4) . ? N5 H5 0.8800 . ? N6 C28 1.484(4) . ? N6 C23 1.495(4) . ? N6 C18 1.504(4) . ? C28 C19 1.517(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? N8 C1 1.322(4) . ? N8 C25 1.464(4) . ? N8 H8 0.8800 . ? C1 C2 1.500(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.513(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.508(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 C8 1.473(5) . ? C7 H7C 0.9900 . ? C7 H7D 0.9900 . ? C8 C9 1.182(6) . ? C9 H9 0.9500 . ? C10 C11 1.513(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.508(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C15 1.466(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.185(5) . ? C16 H16 0.9500 . ? C17 C18 1.517(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C20 C21 1.464(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.174(5) . ? C22 H22 0.9500 . ? C23 C24 1.513(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.473(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.204(6) . ? C27 H27 0.9500 . ? C31 C29 1.476(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C29 C30 1.517(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 O1 Yb1 O2 82.33(8) . . ? O1 Yb1 O3 140.96(8) . . ? O2 Yb1 O3 84.89(8) . . ? O1 Yb1 O4 85.45(8) . . ? O2 Yb1 O4 142.70(8) . . ? O3 Yb1 O4 82.79(8) . . ? O1 Yb1 O5 70.94(8) . . ? O2 Yb1 O5 71.43(8) . . ? O3 Yb1 O5 70.03(8) . . ? O4 Yb1 O5 71.27(7) . . ? O1 Yb1 N6 74.48(8) . . ? O2 Yb1 N6 139.92(8) . . ? O3 Yb1 N6 132.80(8) . . ? O4 Yb1 N6 67.92(8) . . ? O5 Yb1 N6 127.66(8) . . ? O1 Yb1 N1 67.84(8) . . ? O2 Yb1 N1 71.64(8) . . ? O3 Yb1 N1 140.56(8) . . ? O4 Yb1 N1 134.30(8) . . ? O5 Yb1 N1 127.16(8) . . ? N6 Yb1 N1 69.48(8) . . ? O1 Yb1 N4 142.35(8) . . ? O2 Yb1 N4 132.59(8) . . ? O3 Yb1 N4 67.58(8) . . ? O4 Yb1 N4 73.19(8) . . ? O5 Yb1 N4 126.97(8) . . ? N6 Yb1 N4 68.89(8) . . ? N1 Yb1 N4 105.83(8) . . ? O1 Yb1 N2 132.32(8) . . ? O2 Yb1 N2 66.83(8) . . ? O3 Yb1 N2 73.45(8) . . ? O4 Yb1 N2 140.38(8) . . ? O5 Yb1 N2 125.93(8) . . ? N6 Yb1 N2 106.41(8) . . ? N1 Yb1 N2 68.34(8) . . ? N4 Yb1 N2 68.61(8) . . ? O1 Yb1 C1 19.58(8) . . ? O2 Yb1 C1 71.53(8) . . ? O3 Yb1 C1 149.15(8) . . ? O4 Yb1 C1 103.89(8) . . ? O5 Yb1 C1 83.48(8) . . ? N6 Yb1 C1 76.10(8) . . ? N1 Yb1 C1 49.47(9) . . ? N4 Yb1 C1 143.28(8) . . ? N2 Yb1 C1 112.83(8) . . ? O1 Yb1 C13 151.53(8) . . ? O2 Yb1 C13 102.20(8) . . ? O3 Yb1 C13 19.23(8) . . ? O4 Yb1 C13 73.93(8) . . ? O5 Yb1 C13 83.76(8) . . ? N6 Yb1 C13 113.81(8) . . ? N1 Yb1 C13 140.46(8) . . ? N4 Yb1 C13 49.00(8) . . ? N2 Yb1 C13 73.38(8) . . ? C1 Yb1 C13 167.05(8) . . ? O1 Yb1 C6 99.67(8) . . ? O2 Yb1 C6 18.99(8) . . ? O3 Yb1 C6 76.09(8) . . ? O4 Yb1 C6 152.21(8) . . ? O5 Yb1 C6 84.53(8) . . ? N6 Yb1 C6 139.82(8) . . ? N1 Yb1 C6 71.58(8) . . ? N4 Yb1 C6 113.76(8) . . ? N2 Yb1 C6 48.43(8) . . ? C1 Yb1 C6 86.18(8) . . ? C13 Yb1 C6 90.43(8) . . ? C1 O1 Yb1 122.8(2) . . ? C6 O2 Yb1 124.3(2) . . ? C13 O3 Yb1 123.70(19) . . ? H10E O10S H10F 106(2) . . ? C19 N7 C20 122.5(3) . . ? C19 N7 H7 118.8 . . ? C20 N7 H7 118.8 . . ? C19 O4 Yb1 121.6(2) . . ? Yb1 O5 H5E 119(3) . . ? C2 N1 C3 109.0(2) . . ? C2 N1 C24 110.2(3) . . ? C3 N1 C24 108.2(3) . . ? C2 N1 Yb1 106.11(19) . . ? C3 N1 Yb1 112.82(18) . . ? C24 N1 Yb1 110.53(18) . . ? C5 N2 C10 109.4(2) . . ? C5 N2 C4 110.1(2) . . ? C10 N2 C4 107.9(2) . . ? C5 N2 Yb1 106.11(18) . . ? C10 N2 Yb1 111.74(18) . . ? C4 N2 Yb1 111.70(19) . . ? C6 N3 C7 122.4(3) . . ? C6 N3 H3 118.8 . . ? C7 N3 H3 118.8 . . ? C12 N4 C17 109.1(2) . . ? C12 N4 C11 109.3(3) . . ? C17 N4 C11 108.7(2) . . ? C12 N4 Yb1 106.33(18) . . ? C17 N4 Yb1 111.79(18) . . ? C11 N4 Yb1 111.52(18) . . ? C13 N5 C14 121.8(3) . . ? C13 N5 H5 119.1 . . ? C14 N5 H5 119.1 . . ? C28 N6 C23 108.5(2) . . ? C28 N6 C18 109.6(3) . . ? C23 N6 C18 107.7(2) . . ? C28 N6 Yb1 107.27(18) . . ? C23 N6 Yb1 111.61(18) . . ? C18 N6 Yb1 112.19(19) . . ? N6 C28 C19 111.0(3) . . ? N6 C28 H28A 109.4 . . ? C19 C28 H28A 109.4 . . ? N6 C28 H28B 109.4 . . ? C19 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C1 N8 C25 122.4(3) . . ? C1 N8 H8 118.8 . . ? C25 N8 H8 118.8 . . ? O1 C1 N8 122.4(3) . . ? O1 C1 C2 120.5(3) . . ? N8 C1 C2 117.1(3) . . ? O1 C1 Yb1 37.62(15) . . ? N8 C1 Yb1 159.3(2) . . ? C2 C1 Yb1 83.04(18) . . ? N1 C2 C1 111.8(3) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? N1 C3 C4 111.3(3) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C3 112.6(3) . . ? N2 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? N2 C5 C6 109.1(3) . . ? N2 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? N2 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? O2 C6 N3 122.4(3) . . ? O2 C6 C5 119.5(3) . . ? N3 C6 C5 118.1(3) . . ? O2 C6 Yb1 36.73(14) . . ? N3 C6 Yb1 158.7(2) . . ? C5 C6 Yb1 82.91(18) . . ? N3 C7 C8 111.7(3) . . ? N3 C7 H7C 109.3 . . ? C8 C7 H7C 109.3 . . ? N3 C7 H7D 109.3 . . ? C8 C7 H7D 109.3 . . ? H7C C7 H7D 107.9 . . ? C9 C8 C7 178.9(4) . . ? C8 C9 H9 180.0 . . ? N2 C10 C11 110.7(3) . . ? N2 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? N4 C11 C10 113.2(3) . . ? N4 C11 H11A 108.9 . . ? C10 C11 H11A 108.9 . . ? N4 C11 H11B 108.9 . . ? C10 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N4 C12 C13 110.6(2) . . ? N4 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? O3 C13 N5 122.8(3) . . ? O3 C13 C12 119.6(3) . . ? N5 C13 C12 117.6(3) . . ? O3 C13 Yb1 37.07(14) . . ? N5 C13 Yb1 159.8(2) . . ? C12 C13 Yb1 82.62(17) . . ? N5 C14 C15 112.7(3) . . ? N5 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? N5 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C14 179.8(4) . . ? C15 C16 H16 180.0 . . ? N4 C17 C18 110.3(3) . . ? N4 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? N4 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N6 C18 C17 112.1(3) . . ? N6 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N6 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? O4 C19 N7 123.5(3) . . ? O4 C19 C28 120.0(3) . . ? N7 C19 C28 116.5(3) . . ? O4 C19 Yb1 38.86(14) . . ? N7 C19 Yb1 162.3(2) . . ? C28 C19 Yb1 81.09(17) . . ? C21 C20 N7 110.4(3) . . ? C21 C20 H20A 109.6 . . ? N7 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? N7 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C22 C21 C20 178.7(4) . . ? C21 C22 H22 180.0 . . ? N6 C23 C24 110.8(3) . . ? N6 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? N6 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? N1 C24 C23 112.7(3) . . ? N1 C24 H24A 109.1 . . ? C23 C24 H24A 109.1 . . ? N1 C24 H24B 109.1 . . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? N8 C25 C26 110.4(3) . . ? N8 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? N8 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 179.9(7) . . ? C26 C27 H27 180.0 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O6 C29 C31 121.6(6) . . ? O6 C29 C30 121.3(6) . . ? C31 C29 C30 117.1(6) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 N7 H7 O7S 0.88 1.95 2.820(4) 171.4 . O5 H5E O8S 0.818(10) 1.953(12) 2.767(3) 173(4) . N8 H8 O10S 0.88 1.90 2.775(4) 172.3 2_665 N3 H3 Cl3 0.88 2.22 3.090(3) 168.9 1_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.333 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.126