# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- compound 1-12.cif' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Xiao-Ying Huang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. CHINA ; _publ_contact_author_email xyhuang@fjirsm.ac.cn _publ_contact_author_phone 86-59183793727 _publ_contact_author_fax 86-59183793727 loop_ _publ_author_name _publ_author_address 'Bin Tan' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; 'Zai-Lai Xie' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; 'Mei-Ling Feng' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; 'Bing Hu' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; 'Zhao-Feng Wu' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; 'Xiao-Ying Huang' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; _publ_section_title ; Ionothermal Syntheses, Crystal Structures and Properties of Three-Dimensional Rare Earth Metal Organic Frameworks with 1,4-naphthalenedicarboxylic acid ; data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 876521' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 La2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl La2 N2 O12' _chemical_formula_weight 1123.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.0824(2) _cell_length_b 14.75579(17) _cell_length_c 16.3179(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.2061(13) _cell_angle_gamma 90.00 _cell_volume 4328.43(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11442 _cell_measurement_theta_min 2.2477 _cell_measurement_theta_max 28.8278 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 2.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89433 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19860 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8989 _reflns_number_gt 6939 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0300P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8989 _refine_ls_number_parameters 607 _refine_ls_number_restraints 391 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.007 _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 La1 La 0.378838(9) 0.025318(10) -0.005352(10) 0.01585(5) Uani 1 1 d . . . La2 La 0.115031(9) 0.014143(11) -0.000741(10) 0.01589(5) Uani 1 1 d . . . Cl1 Cl 0.25217(4) -0.09004(5) 0.02433(6) 0.0337(2) Uani 1 1 d . . . O1 O 0.44780(13) 0.13339(16) -0.08086(17) 0.0418(7) Uani 1 1 d . . . O2 O 0.57030(13) 0.11322(15) -0.06261(17) 0.0426(7) Uani 1 1 d . . . O3 O 0.31770(13) 0.13733(17) 0.07618(17) 0.0468(7) Uani 1 1 d . . . O5 O 0.48169(15) 0.43149(17) -0.40321(16) 0.0518(8) Uani 1 1 d . . . O4 O 0.19758(13) 0.14042(15) 0.03068(16) 0.0381(6) Uani 1 1 d . . . O6 O 0.60354(15) 0.42808(18) -0.37698(16) 0.0513(7) Uani 1 1 d . . . O7 O 0.28163(12) 0.43156(16) 0.38925(14) 0.0382(6) Uani 1 1 d . . . O8 O 0.15934(12) 0.44684(15) 0.36510(13) 0.0316(5) Uani 1 1 d . . . O9 O 0.06178(14) 0.10471(16) 0.10817(16) 0.0435(7) Uani 1 1 d . . . O10 O -0.06244(13) 0.10751(16) 0.08897(16) 0.0444(7) Uani 1 1 d . . . O11 O 0.00262(13) 0.41673(15) 0.43167(15) 0.0351(6) Uani 1 1 d . . . O12 O -0.11360(13) 0.41230(18) 0.37657(17) 0.0507(8) Uani 1 1 d . . . C1 C 0.51267(18) 0.1520(2) -0.0946(2) 0.0288(8) Uani 1 1 d . . . C2 C 0.52136(17) 0.2244(2) -0.1583(2) 0.0256(7) Uani 1 1 d . . . C3 C 0.47261(18) 0.2232(2) -0.2282(2) 0.0347(9) Uani 1 1 d . . . H3A H 0.4350 0.1799 -0.2338 0.042 Uiso 1 1 calc R . . C4 C 0.47814(19) 0.2860(2) -0.2918(2) 0.0347(9) Uani 1 1 d . . . H4A H 0.4438 0.2843 -0.3386 0.042 Uiso 1 1 calc R . . C5 C 0.53323(18) 0.3496(2) -0.2861(2) 0.0277(8) Uani 1 1 d . . . C6 C 0.58374(17) 0.3563(2) -0.2124(2) 0.0243(7) Uani 1 1 d . . . C7 C 0.57830(17) 0.2918(2) -0.1479(2) 0.0248(7) Uani 1 1 d . . . C8 C 0.62894(19) 0.2986(2) -0.0758(2) 0.0354(9) Uani 1 1 d . . . H8A H 0.6271 0.2560 -0.0341 0.042 Uiso 1 1 calc R . . C9 C 0.6801(2) 0.3659(3) -0.0664(2) 0.0450(10) Uani 1 1 d . . . H9A H 0.7129 0.3690 -0.0185 0.054 Uiso 1 1 calc R . . C10 C 0.6839(2) 0.4306(3) -0.1282(2) 0.0432(10) Uani 1 1 d . . . H10A H 0.7186 0.4772 -0.1205 0.052 Uiso 1 1 calc R . . C11 C 0.63765(19) 0.4262(2) -0.1991(2) 0.0334(8) Uani 1 1 d . . . H11A H 0.6413 0.4697 -0.2398 0.040 Uiso 1 1 calc R . . C12 C 0.5397(2) 0.4080(2) -0.3600(2) 0.0350(9) Uani 1 1 d . . . C13 C 0.25316(19) 0.1681(2) 0.0772(2) 0.0307(8) Uani 1 1 d . . . C14 C 0.24180(18) 0.2395(2) 0.1398(2) 0.0278(8) Uani 1 1 d . . . C15 C 0.28540(19) 0.2339(2) 0.2136(2) 0.0394(9) Uani 1 1 d . . . H15A H 0.3217 0.1891 0.2204 0.047 Uiso 1 1 calc R . . C16 C 0.27769(19) 0.2925(2) 0.2787(2) 0.0371(9) Uani 1 1 d . . . H16A H 0.3093 0.2869 0.3273 0.045 Uiso 1 1 calc R . . C17 C 0.22391(16) 0.3587(2) 0.2722(2) 0.0237(7) Uani 1 1 d . . . C18 C 0.17720(16) 0.36899(19) 0.19663(19) 0.0213(7) Uani 1 1 d . . . C19 C 0.18696(17) 0.3099(2) 0.1282(2) 0.0235(7) Uani 1 1 d . . . C20 C 0.1438(2) 0.3255(2) 0.0527(2) 0.0345(8) Uani 1 1 d . . . H20A H 0.1503 0.2884 0.0079 0.041 Uiso 1 1 calc R . . C21 C 0.0926(2) 0.3938(2) 0.0436(2) 0.0398(9) Uani 1 1 d . . . H21A H 0.0650 0.4031 -0.0072 0.048 Uiso 1 1 calc R . . C22 C 0.0817(2) 0.4489(2) 0.1095(2) 0.0413(9) Uani 1 1 d . . . H22A H 0.0461 0.4945 0.1027 0.050 Uiso 1 1 calc R . . C23 C 0.12211(17) 0.4380(2) 0.1845(2) 0.0258(7) Uani 1 1 d . . . H23A H 0.1135 0.4759 0.2280 0.031 Uiso 1 1 calc R . . C24 C 0.22094(17) 0.4171(2) 0.34731(19) 0.0242(7) Uani 1 1 d . . . C25 C 0.0000(2) 0.1365(2) 0.1202(2) 0.0338(8) Uani 1 1 d . . . C26 C -0.00241(18) 0.2143(2) 0.1792(2) 0.0293(8) Uani 1 1 d . . . C27 C 0.0357(2) 0.2077(2) 0.2560(2) 0.0395(9) Uani 1 1 d . . . H27A H 0.0694 0.1606 0.2674 0.047 Uiso 1 1 calc R . . C28 C 0.0248(2) 0.2707(2) 0.3181(2) 0.0378(9) Uani 1 1 d . . . H28A H 0.0518 0.2653 0.3697 0.045 Uiso 1 1 calc R . . C29 C -0.02497(18) 0.3400(2) 0.3033(2) 0.0293(8) Uani 1 1 d . . . C30 C -0.06068(18) 0.3556(2) 0.2212(2) 0.0297(8) Uani 1 1 d . . . C31 C -0.04955(18) 0.2910(2) 0.1591(2) 0.0301(8) Uani 1 1 d . . . C32 C -0.0830(2) 0.3069(3) 0.0776(2) 0.0422(10) Uani 1 1 d . . . H32A H -0.0775 0.2649 0.0362 0.051 Uiso 1 1 calc R . . C33 C -0.1229(3) 0.3833(3) 0.0604(3) 0.0593(12) Uani 1 1 d . . . H33A H -0.1440 0.3935 0.0067 0.071 Uiso 1 1 calc R . . C34 C -0.1330(2) 0.4465(3) 0.1203(3) 0.0614(13) Uani 1 1 d . . . H34A H -0.1599 0.4989 0.1061 0.074 Uiso 1 1 calc R . . C35 C -0.1042(2) 0.4333(2) 0.2001(3) 0.0431(10) Uani 1 1 d . . . H35A H -0.1132 0.4753 0.2404 0.052 Uiso 1 1 calc R . . C36 C -0.04619(19) 0.3939(2) 0.3743(2) 0.0331(8) Uani 1 1 d . . . N1A N 0.2373(4) -0.2640(4) 0.2755(4) 0.0558(12) Uani 0.675(4) 1 d PDU A 1 N2A N 0.3115(5) -0.1512(5) 0.2701(4) 0.0702(14) Uani 0.675(4) 1 d PDU A 1 C37A C 0.2776(5) -0.2698(5) 0.3468(4) 0.0645(16) Uani 0.675(4) 1 d PDU A 1 H37A H 0.2752 -0.3113 0.3893 0.077 Uiso 0.675(4) 1 calc PR A 1 C38A C 0.3293(5) -0.1899(5) 0.3408(4) 0.0694(16) Uani 0.675(4) 1 d PDU A 1 H38A H 0.3670 -0.1719 0.3807 0.083 Uiso 0.675(4) 1 calc PR A 1 C39A C 0.2538(8) -0.1987(8) 0.2299(5) 0.0557(16) Uani 0.675(4) 1 d PDU A 1 H39A H 0.2303 -0.1855 0.1777 0.067 Uiso 0.675(4) 1 calc PR A 1 C40A C 0.1798(4) -0.3348(4) 0.2517(6) 0.080(2) Uani 0.675(4) 1 d PDU A 1 H40A H 0.1375 -0.3073 0.2208 0.120 Uiso 0.675(4) 1 calc PR A 1 H40B H 0.1648 -0.3626 0.3004 0.120 Uiso 0.675(4) 1 calc PR A 1 H40C H 0.2003 -0.3801 0.2184 0.120 Uiso 0.675(4) 1 calc PR A 1 C41A C 0.3423(6) -0.0701(6) 0.2338(6) 0.1050(19) Uani 0.675(4) 1 d PDU A 1 H41A H 0.3740 -0.0883 0.1924 0.126 Uiso 0.675(4) 1 calc PR A 1 H41B H 0.3020 -0.0337 0.2070 0.126 Uiso 0.675(4) 1 calc PR A 1 C43A C 0.3275(6) 0.0293(6) 0.3510(7) 0.151(2) Uani 0.675(4) 1 d PDU A 1 H43A H 0.2870 0.0585 0.3171 0.181 Uiso 0.675(4) 1 calc PR A 1 H43B H 0.3075 -0.0145 0.3871 0.181 Uiso 0.675(4) 1 calc PR A 1 C42A C 0.3853(6) -0.0160(6) 0.2967(6) 0.136(2) Uani 0.675(4) 1 d PDU A 1 H42A H 0.4133 0.0304 0.2712 0.163 Uiso 0.675(4) 1 calc PR A 1 H42B H 0.4200 -0.0540 0.3307 0.163 Uiso 0.675(4) 1 calc PR A 1 C44A C 0.3771(8) 0.0971(7) 0.3988(6) 0.173(2) Uani 0.675(4) 1 d PDU A 1 H44A H 0.4120 0.1172 0.3614 0.208 Uiso 0.675(4) 1 calc PR A 1 H44B H 0.3456 0.1488 0.4070 0.208 Uiso 0.675(4) 1 calc PR A 1 C45A C 0.4226(8) 0.0820(8) 0.4801(7) 0.193(3) Uani 0.675(4) 1 d PDU A 1 H45A H 0.4204 0.0184 0.4947 0.232 Uiso 0.675(4) 1 calc PR A 1 H45D H 0.4741 0.0968 0.4748 0.232 Uiso 0.675(4) 1 calc PR A 1 C46A C 0.3972(9) 0.1363(9) 0.5459(7) 0.212(4) Uani 0.675(4) 1 d PDU A 1 H46A H 0.4260 0.1217 0.5971 0.318 Uiso 0.675(4) 1 calc PR A 1 H46B H 0.3457 0.1236 0.5502 0.318 Uiso 0.675(4) 1 calc PR A 1 H46C H 0.4031 0.1994 0.5339 0.318 Uiso 0.675(4) 1 calc PR A 1 N2B N 0.3020(10) -0.1800(10) 0.2824(9) 0.0702(14) Uani 0.325(4) 1 d PDU A 2 N1B N 0.2116(7) -0.2771(8) 0.2334(7) 0.0558(12) Uani 0.325(4) 1 d PDU A 2 C40B C 0.1549(8) -0.3208(10) 0.1769(9) 0.080(2) Uani 0.325(4) 1 d PDU A 2 H40D H 0.1636 -0.3073 0.1212 0.120 Uiso 0.325(4) 1 calc PR A 2 H40E H 0.1068 -0.2987 0.1869 0.120 Uiso 0.325(4) 1 calc PR A 2 H40F H 0.1570 -0.3851 0.1854 0.120 Uiso 0.325(4) 1 calc PR A 2 C37B C 0.2311(9) -0.2975(10) 0.3099(8) 0.0645(16) Uani 0.325(4) 1 d PDU A 2 H37B H 0.2082 -0.3400 0.3409 0.077 Uiso 0.325(4) 1 calc PR A 2 C38B C 0.2981(10) -0.2393(11) 0.3401(9) 0.0694(16) Uani 0.325(4) 1 d PDU A 2 H38B H 0.3292 -0.2451 0.3890 0.083 Uiso 0.325(4) 1 calc PR A 2 C41B C 0.3486(10) -0.0976(10) 0.2665(12) 0.1050(19) Uani 0.325(4) 1 d PDU A 2 H41C H 0.3739 -0.1120 0.2187 0.126 Uiso 0.325(4) 1 calc PR A 2 H41D H 0.3868 -0.0934 0.3129 0.126 Uiso 0.325(4) 1 calc PR A 2 C42B C 0.3168(12) -0.0002(11) 0.2520(12) 0.136(2) Uani 0.325(4) 1 d PDU A 2 H42C H 0.3181 0.0216 0.1962 0.163 Uiso 0.325(4) 1 calc PR A 2 H42D H 0.2677 0.0078 0.2698 0.163 Uiso 0.325(4) 1 calc PR A 2 C39B C 0.2522(16) -0.2089(17) 0.2179(12) 0.0557(16) Uani 0.325(4) 1 d PDU A 2 H39B H 0.2482 -0.1809 0.1666 0.067 Uiso 0.325(4) 1 calc PR A 2 C44B C 0.3786(16) 0.0370(13) 0.4054(11) 0.173(2) Uani 0.325(4) 1 d PDU A 2 H44C H 0.4293 0.0234 0.4278 0.208 Uiso 0.325(4) 1 calc PR A 2 H44D H 0.3497 -0.0163 0.4160 0.208 Uiso 0.325(4) 1 calc PR A 2 C43B C 0.3807(13) 0.0372(15) 0.3141(12) 0.151(2) Uani 0.325(4) 1 d PDU A 2 H43C H 0.4253 0.0043 0.3038 0.181 Uiso 0.325(4) 1 calc PR A 2 H43D H 0.3884 0.0996 0.2985 0.181 Uiso 0.325(4) 1 calc PR A 2 C45B C 0.3521(13) 0.1117(18) 0.4647(16) 0.193(3) Uani 0.325(4) 1 d PDU A 2 H45B H 0.3242 0.1589 0.4336 0.232 Uiso 0.325(4) 1 calc PR A 2 H45C H 0.3210 0.0854 0.5034 0.232 Uiso 0.325(4) 1 calc PR A 2 C46B C 0.4256(17) 0.150(2) 0.5107(17) 0.212(4) Uani 0.325(4) 1 d PDU A 2 H46G H 0.4142 0.2010 0.5442 0.318 Uiso 0.325(4) 1 calc PR A 2 H46D H 0.4578 0.1699 0.4711 0.318 Uiso 0.325(4) 1 calc PR A 2 H46E H 0.4499 0.1041 0.5452 0.318 Uiso 0.325(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01587(9) 0.01791(9) 0.01410(9) 0.00020(7) 0.00314(7) 0.00092(7) La2 0.01533(9) 0.01773(9) 0.01505(9) -0.00046(7) 0.00365(7) -0.00175(7) Cl1 0.0204(4) 0.0307(4) 0.0513(6) 0.0142(4) 0.0101(4) 0.0033(3) O1 0.0260(13) 0.0445(14) 0.0557(18) 0.0250(13) 0.0072(13) -0.0044(11) O2 0.0293(14) 0.0370(14) 0.0608(19) 0.0260(13) 0.0021(13) 0.0039(11) O3 0.0307(14) 0.0523(16) 0.0583(19) -0.0320(14) 0.0092(14) 0.0069(12) O5 0.0512(17) 0.0534(17) 0.0454(17) 0.0224(14) -0.0186(14) -0.0006(13) O4 0.0329(14) 0.0360(13) 0.0470(17) -0.0209(12) 0.0119(13) -0.0132(11) O6 0.0466(17) 0.0683(19) 0.0397(16) 0.0303(14) 0.0080(14) -0.0135(14) O7 0.0254(13) 0.0584(16) 0.0303(14) -0.0226(12) 0.0005(11) -0.0020(11) O8 0.0273(12) 0.0470(14) 0.0214(12) -0.0092(11) 0.0070(10) 0.0072(11) O9 0.0330(14) 0.0518(16) 0.0487(17) -0.0302(13) 0.0181(13) -0.0075(12) O10 0.0325(14) 0.0488(15) 0.0542(18) -0.0330(13) 0.0157(13) -0.0165(12) O11 0.0327(14) 0.0407(14) 0.0320(14) -0.0169(11) 0.0045(11) -0.0114(11) O12 0.0234(14) 0.077(2) 0.0537(18) -0.0409(15) 0.0132(13) -0.0079(12) C1 0.0260(18) 0.0261(17) 0.034(2) 0.0119(15) 0.0031(16) 0.0003(14) C2 0.0203(16) 0.0244(16) 0.033(2) 0.0140(15) 0.0058(15) 0.0009(13) C3 0.0222(18) 0.0364(19) 0.044(2) 0.0155(17) -0.0014(17) -0.0083(15) C4 0.0247(18) 0.043(2) 0.034(2) 0.0133(17) -0.0054(16) -0.0050(15) C5 0.0224(17) 0.0333(18) 0.0273(19) 0.0120(15) 0.0021(15) 0.0013(14) C6 0.0196(16) 0.0261(16) 0.0278(19) 0.0080(14) 0.0048(14) 0.0013(13) C7 0.0193(16) 0.0294(17) 0.0257(18) 0.0078(14) 0.0031(14) 0.0011(13) C8 0.037(2) 0.043(2) 0.025(2) 0.0100(16) 0.0012(17) -0.0045(16) C9 0.042(2) 0.059(3) 0.032(2) 0.0030(19) -0.0050(19) -0.0148(19) C10 0.046(2) 0.045(2) 0.039(2) -0.0019(19) 0.0045(19) -0.0193(18) C11 0.035(2) 0.0327(18) 0.033(2) 0.0077(16) 0.0058(17) -0.0077(15) C12 0.041(2) 0.0345(19) 0.027(2) 0.0138(16) -0.0060(17) -0.0047(16) C13 0.0312(19) 0.0266(17) 0.036(2) -0.0130(15) 0.0122(17) -0.0080(14) C14 0.0214(17) 0.0315(18) 0.032(2) -0.0110(15) 0.0083(15) -0.0014(13) C15 0.030(2) 0.042(2) 0.046(2) -0.0182(18) -0.0019(18) 0.0153(16) C16 0.0286(19) 0.050(2) 0.030(2) -0.0144(18) -0.0056(16) 0.0134(16) C17 0.0183(16) 0.0292(16) 0.0233(18) -0.0082(14) 0.0010(14) 0.0003(13) C18 0.0161(15) 0.0263(16) 0.0221(17) -0.0019(13) 0.0048(13) -0.0058(12) C19 0.0197(16) 0.0281(16) 0.0235(18) -0.0064(14) 0.0055(14) -0.0058(13) C20 0.040(2) 0.039(2) 0.0233(19) -0.0067(16) 0.0013(16) -0.0041(16) C21 0.046(2) 0.049(2) 0.023(2) -0.0024(17) -0.0053(17) 0.0043(18) C22 0.040(2) 0.037(2) 0.047(2) 0.0050(18) 0.0023(19) 0.0123(17) C23 0.0256(17) 0.0280(16) 0.0245(18) -0.0029(14) 0.0053(14) 0.0013(13) C24 0.0244(17) 0.0321(17) 0.0165(16) -0.0049(14) 0.0035(14) -0.0021(13) C25 0.036(2) 0.0342(19) 0.034(2) -0.0153(16) 0.0153(17) -0.0115(16) C26 0.0256(18) 0.0362(19) 0.028(2) -0.0150(16) 0.0108(16) -0.0101(14) C27 0.029(2) 0.042(2) 0.046(2) -0.0182(18) 0.0033(18) 0.0084(16) C28 0.034(2) 0.051(2) 0.028(2) -0.0159(18) 0.0009(17) 0.0022(17) C29 0.0235(17) 0.0371(19) 0.028(2) -0.0134(16) 0.0069(15) -0.0066(14) C30 0.0278(18) 0.0307(17) 0.032(2) -0.0088(16) 0.0108(16) -0.0091(14) C31 0.0266(18) 0.0347(18) 0.030(2) -0.0086(16) 0.0092(16) -0.0120(15) C32 0.047(2) 0.053(2) 0.027(2) -0.0042(18) 0.0038(19) -0.0132(19) C33 0.062(3) 0.074(3) 0.041(3) 0.014(2) 0.000(2) -0.008(2) C34 0.053(3) 0.052(3) 0.079(4) 0.013(3) 0.008(3) 0.012(2) C35 0.048(2) 0.037(2) 0.047(3) -0.0014(19) 0.016(2) 0.0023(18) C36 0.0300(19) 0.0369(19) 0.034(2) -0.0194(16) 0.0124(17) -0.0104(15) N1A 0.075(3) 0.043(2) 0.055(3) 0.011(2) 0.031(2) 0.0191(19) N2A 0.107(3) 0.053(3) 0.056(3) 0.012(2) 0.030(3) -0.003(3) C37A 0.090(4) 0.052(3) 0.054(3) 0.015(3) 0.020(3) 0.016(3) C38A 0.101(4) 0.062(3) 0.047(3) 0.014(3) 0.017(3) 0.020(3) C39A 0.075(3) 0.048(3) 0.046(3) 0.004(3) 0.017(3) 0.004(2) C40A 0.074(4) 0.054(4) 0.121(6) -0.007(4) 0.047(5) 0.011(3) C41A 0.163(4) 0.069(4) 0.090(4) 0.021(3) 0.044(4) -0.038(3) C43A 0.243(5) 0.095(4) 0.128(4) 0.013(4) 0.080(4) -0.027(4) C42A 0.212(5) 0.086(4) 0.119(4) 0.009(4) 0.059(4) -0.026(4) C44A 0.276(5) 0.114(4) 0.139(5) 0.025(4) 0.064(5) -0.031(5) C45A 0.296(6) 0.129(5) 0.165(6) 0.023(5) 0.069(5) -0.027(5) C46A 0.348(10) 0.124(7) 0.186(9) -0.023(8) 0.132(9) -0.013(8) N2B 0.107(3) 0.053(3) 0.056(3) 0.012(2) 0.030(3) -0.003(3) N1B 0.075(3) 0.043(2) 0.055(3) 0.011(2) 0.031(2) 0.0191(19) C40B 0.074(4) 0.054(4) 0.121(6) -0.007(4) 0.047(5) 0.011(3) C37B 0.090(4) 0.052(3) 0.054(3) 0.015(3) 0.020(3) 0.016(3) C38B 0.101(4) 0.062(3) 0.047(3) 0.014(3) 0.017(3) 0.020(3) C41B 0.163(4) 0.069(4) 0.090(4) 0.021(3) 0.044(4) -0.038(3) C42B 0.212(5) 0.086(4) 0.119(4) 0.009(4) 0.059(4) -0.026(4) C39B 0.075(3) 0.048(3) 0.046(3) 0.004(3) 0.017(3) 0.004(2) C44B 0.276(5) 0.114(4) 0.139(5) 0.025(4) 0.064(5) -0.031(5) C43B 0.243(5) 0.095(4) 0.128(4) 0.013(4) 0.080(4) -0.027(4) C45B 0.296(6) 0.129(5) 0.165(6) 0.023(5) 0.069(5) -0.027(5) C46B 0.348(10) 0.124(7) 0.186(9) -0.023(8) 0.132(9) -0.013(8) _geom_special_details ; All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 La1 O7 2.408(2) 4_565 ? La1 O1 2.439(2) . ? La1 O5 2.444(2) 4_566 ? La1 O6 2.445(2) 2_644 ? La1 O2 2.456(2) 3_655 ? La1 O3 2.458(2) . ? La1 Cl1 2.9358(8) . ? La2 O4 2.408(2) . ? La2 O10 2.430(2) 3 ? La2 O11 2.430(2) 4_565 ? La2 O8 2.479(2) 4_565 ? La2 O9 2.498(2) . ? La2 O12 2.525(2) 2_545 ? La2 O11 2.895(2) 2_545 ? La2 Cl1 2.9087(8) . ? La2 C36 3.084(3) 2_545 ? La2 La2 4.1836(3) 3 ? O1 C1 1.248(4) . ? O2 C1 1.252(4) . ? O2 La1 2.456(2) 3_655 ? O3 C13 1.254(4) . ? O5 C12 1.248(4) . ? O5 La1 2.444(2) 4_565 ? O4 C13 1.260(4) . ? O6 C12 1.251(4) . ? O6 La1 2.445(2) 2_654 ? O7 C24 1.248(4) . ? O7 La1 2.408(2) 4_566 ? O8 C24 1.260(4) . ? O8 La2 2.479(2) 4_566 ? O9 C25 1.247(4) . ? O10 C25 1.261(4) . ? O10 La2 2.430(2) 3 ? O11 C36 1.261(4) . ? O11 La2 2.430(2) 4_566 ? O11 La2 2.895(2) 2 ? O12 C36 1.253(4) . ? O12 La2 2.525(2) 2 ? C1 C2 1.511(4) . ? C2 C3 1.364(4) . ? C2 C7 1.428(4) . ? C3 C4 1.404(5) . ? C3 H3A 0.9300 . ? C4 C5 1.364(4) . ? C4 H4A 0.9300 . ? C5 C6 1.432(4) . ? C5 C12 1.497(4) . ? C6 C11 1.420(4) . ? C6 C7 1.431(4) . ? C7 C8 1.413(4) . ? C8 C9 1.355(5) . ? C8 H8A 0.9300 . ? C9 C10 1.395(5) . ? C9 H9A 0.9300 . ? C10 C11 1.355(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.497(4) . ? C14 C15 1.369(5) . ? C14 C19 1.433(4) . ? C15 C16 1.388(5) . ? C15 H15A 0.9300 . ? C16 C17 1.374(4) . ? C16 H16A 0.9300 . ? C17 C18 1.425(4) . ? C17 C24 1.504(4) . ? C18 C23 1.423(4) . ? C18 C19 1.443(4) . ? C19 C20 1.403(4) . ? C20 C21 1.366(5) . ? C20 H20A 0.9300 . ? C21 C22 1.380(5) . ? C21 H21A 0.9300 . ? C22 C23 1.366(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.503(4) . ? C26 C27 1.367(5) . ? C26 C31 1.434(5) . ? C27 C28 1.403(5) . ? C27 H27A 0.9300 . ? C28 C29 1.366(5) . ? C28 H28A 0.9300 . ? C29 C30 1.442(5) . ? C29 C36 1.489(4) . ? C30 C35 1.413(5) . ? C30 C31 1.421(4) . ? C31 C32 1.420(5) . ? C32 C33 1.350(6) . ? C32 H32A 0.9300 . ? C33 C34 1.378(6) . ? C33 H33A 0.9300 . ? C34 C35 1.362(6) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 La2 3.084(3) 2 ? N1A C39A 1.273(6) . ? N1A C37A 1.306(6) . ? N1A C40A 1.495(8) . ? N2A C38A 1.298(6) . ? N2A C39A 1.365(7) . ? N2A C41A 1.471(7) . ? C37A C38A 1.514(10) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.457(8) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C44A 1.504(9) . ? C43A C42A 1.589(9) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.502(9) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.453(9) . ? C45A H45A 0.9700 . ? C45A H45D 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N2B C38B 1.292(8) . ? N2B C39B 1.376(10) . ? N2B C41B 1.517(10) . ? N1B C39B 1.288(8) . ? N1B C37B 1.296(8) . ? N1B C40B 1.453(11) . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C37B C38B 1.522(13) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C41B C42B 1.557(10) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.554(10) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C39B H39B 0.9300 . ? C44B C43B 1.494(10) . ? C44B C45B 1.576(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C45B C46B 1.562(11) . ? C45B H45B 0.9700 . ? C45B H45C 0.9700 . ? C46B H46G 0.9600 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? 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 O7 La1 O1 80.79(8) 4_565 . ? O7 La1 O5 149.44(9) 4_565 4_566 ? O1 La1 O5 77.36(9) . 4_566 ? O7 La1 O6 75.00(9) 4_565 2_644 ? O1 La1 O6 82.52(9) . 2_644 ? O5 La1 O6 122.30(9) 4_566 2_644 ? O7 La1 O2 138.69(9) 4_565 3_655 ? O1 La1 O2 125.82(8) . 3_655 ? O5 La1 O2 71.88(9) 4_566 3_655 ? O6 La1 O2 77.99(9) 2_644 3_655 ? O7 La1 O3 82.68(9) 4_565 . ? O1 La1 O3 96.79(9) . . ? O5 La1 O3 79.00(8) 4_566 . ? O6 La1 O3 157.51(9) 2_644 . ? O2 La1 O3 118.92(9) 3_655 . ? O7 La1 Cl1 75.45(6) 4_565 . ? O1 La1 Cl1 155.94(6) . . ? O5 La1 Cl1 126.05(7) 4_566 . ? O6 La1 Cl1 87.68(7) 2_644 . ? O2 La1 Cl1 72.76(6) 3_655 . ? O3 La1 Cl1 84.03(6) . . ? O4 La2 O10 153.10(8) . 3 ? O4 La2 O11 103.93(8) . 4_565 ? O10 La2 O11 77.67(9) 3 4_565 ? O4 La2 O8 75.89(8) . 4_565 ? O10 La2 O8 77.96(8) 3 4_565 ? O11 La2 O8 80.56(7) 4_565 4_565 ? O4 La2 O9 73.28(8) . . ? O10 La2 O9 131.34(8) 3 . ? O11 La2 O9 74.36(8) 4_565 . ? O8 La2 O9 133.64(8) 4_565 . ? O4 La2 O12 110.46(9) . 2_545 ? O10 La2 O12 89.91(9) 3 2_545 ? O11 La2 O12 122.24(8) 4_565 2_545 ? O8 La2 O12 151.54(8) 4_565 2_545 ? O9 La2 O12 73.11(9) . 2_545 ? O4 La2 O11 140.00(8) . 2_545 ? O10 La2 O11 66.85(8) 3 2_545 ? O11 La2 O11 76.78(7) 4_565 2_545 ? O8 La2 O11 141.30(7) 4_565 2_545 ? O9 La2 O11 68.45(7) . 2_545 ? O12 La2 O11 47.19(7) 2_545 2_545 ? O4 La2 Cl1 83.09(6) . . ? O10 La2 Cl1 88.05(6) 3 . ? O11 La2 Cl1 160.80(6) 4_565 . ? O8 La2 Cl1 83.97(5) 4_565 . ? O9 La2 Cl1 124.82(7) . . ? O12 La2 Cl1 69.82(6) 2_545 . ? O11 La2 Cl1 109.51(4) 2_545 . ? O4 La2 C36 126.05(9) . 2_545 ? O10 La2 C36 79.11(10) 3 2_545 ? O11 La2 C36 99.61(8) 4_565 2_545 ? O8 La2 C36 156.47(9) 4_565 2_545 ? O9 La2 C36 67.50(9) . 2_545 ? O12 La2 C36 23.19(8) 2_545 2_545 ? O11 La2 C36 24.09(7) 2_545 2_545 ? Cl1 La2 C36 90.08(6) . 2_545 ? O4 La2 La2 132.06(6) . 3 ? O10 La2 La2 66.67(6) 3 3 ? O11 La2 La2 42.35(5) 4_565 3 ? O8 La2 La2 116.41(5) 4_565 3 ? O9 La2 La2 65.75(5) . 3 ? O12 La2 La2 80.77(5) 2_545 3 ? O11 La2 La2 34.43(4) 2_545 3 ? Cl1 La2 La2 141.223(17) . 3 ? C36 La2 La2 57.67(6) 2_545 3 ? La2 Cl1 La1 109.80(3) . . ? C1 O1 La1 140.9(2) . . ? C1 O2 La1 145.3(2) . 3_655 ? C13 O3 La1 136.4(2) . . ? C12 O5 La1 171.4(3) . 4_565 ? C13 O4 La2 144.6(2) . . ? C12 O6 La1 121.0(2) . 2_654 ? C24 O7 La1 165.5(2) . 4_566 ? C24 O8 La2 131.5(2) . 4_566 ? C25 O9 La2 137.2(2) . . ? C25 O10 La2 139.9(2) . 3 ? C36 O11 La2 158.9(2) . 4_566 ? C36 O11 La2 86.39(19) . 2 ? La2 O11 La2 103.22(7) 4_566 2 ? C36 O12 La2 104.3(2) . 2 ? O1 C1 O2 125.5(3) . . ? O1 C1 C2 116.7(3) . . ? O2 C1 C2 117.8(3) . . ? C3 C2 C7 120.1(3) . . ? C3 C2 C1 117.4(3) . . ? C7 C2 C1 122.5(3) . . ? C2 C3 C4 121.2(3) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 C12 117.4(3) . . ? C6 C5 C12 122.6(3) . . ? C11 C6 C7 118.2(3) . . ? C11 C6 C5 122.9(3) . . ? C7 C6 C5 118.9(3) . . ? C8 C7 C2 122.9(3) . . ? C8 C7 C6 118.4(3) . . ? C2 C7 C6 118.8(3) . . ? C9 C8 C7 121.3(3) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C8 C9 C10 120.4(4) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 120.7(3) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C6 121.0(3) . . ? C10 C11 H11A 119.5 . . ? C6 C11 H11A 119.5 . . ? O5 C12 O6 123.2(3) . . ? O5 C12 C5 118.7(3) . . ? O6 C12 C5 118.0(3) . . ? O3 C13 O4 123.9(3) . . ? O3 C13 C14 117.4(3) . . ? O4 C13 C14 118.7(3) . . ? C15 C14 C19 119.0(3) . . ? C15 C14 C13 116.7(3) . . ? C19 C14 C13 124.3(3) . . ? C14 C15 C16 122.7(3) . . ? C14 C15 H15A 118.7 . . ? C16 C15 H15A 118.7 . . ? C17 C16 C15 120.8(3) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 119.4(3) . . ? C16 C17 C24 115.6(3) . . ? C18 C17 C24 125.0(3) . . ? C23 C18 C17 122.5(3) . . ? C23 C18 C19 117.9(3) . . ? C17 C18 C19 119.6(3) . . ? C20 C19 C14 123.1(3) . . ? C20 C19 C18 118.5(3) . . ? C14 C19 C18 118.4(3) . . ? C21 C20 C19 121.5(3) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 121.5(3) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C18 120.5(3) . . ? C22 C23 H23A 119.8 . . ? C18 C23 H23A 119.8 . . ? O7 C24 O8 124.1(3) . . ? O7 C24 C17 116.0(3) . . ? O8 C24 C17 119.9(3) . . ? O9 C25 O10 126.0(3) . . ? O9 C25 C26 118.4(3) . . ? O10 C25 C26 115.5(3) . . ? C27 C26 C31 119.6(3) . . ? C27 C26 C25 119.2(3) . . ? C31 C26 C25 121.0(3) . . ? C26 C27 C28 121.2(3) . . ? C26 C27 H27A 119.4 . . ? C28 C27 H27A 119.4 . . ? C29 C28 C27 120.6(3) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 120.2(3) . . ? C28 C29 C36 118.9(3) . . ? C30 C29 C36 120.7(3) . . ? C35 C30 C31 119.2(3) . . ? C35 C30 C29 122.6(3) . . ? C31 C30 C29 118.2(3) . . ? C32 C31 C30 118.6(3) . . ? C32 C31 C26 121.8(3) . . ? C30 C31 C26 119.5(3) . . ? C33 C32 C31 119.7(4) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C32 C33 C34 121.8(4) . . ? C32 C33 H33A 119.1 . . ? C34 C33 H33A 119.1 . . ? C35 C34 C33 121.0(4) . . ? C35 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? C34 C35 C30 119.6(4) . . ? C34 C35 H35A 120.2 . . ? C30 C35 H35A 120.2 . . ? O12 C36 O11 121.6(3) . . ? O12 C36 C29 118.2(3) . . ? O11 C36 C29 120.1(3) . . ? O12 C36 La2 52.49(16) . 2 ? O11 C36 La2 69.52(18) . 2 ? C29 C36 La2 169.8(3) . 2 ? C39A N1A C37A 115.2(7) . . ? C39A N1A C40A 125.2(7) . . ? C37A N1A C40A 119.5(6) . . ? C38A N2A C39A 107.7(6) . . ? C38A N2A C41A 130.4(7) . . ? C39A N2A C41A 121.9(6) . . ? N1A C37A C38A 100.5(6) . . ? N1A C37A H37A 129.8 . . ? C38A C37A H37A 129.8 . . ? N2A C38A C37A 107.8(7) . . ? N2A C38A H38A 126.1 . . ? C37A C38A H38A 126.1 . . ? N1A C39A N2A 108.9(6) . . ? N1A C39A H39A 125.6 . . ? N2A C39A H39A 125.6 . . ? C42A C41A N2A 111.1(8) . . ? C42A C41A H41A 109.4 . . ? N2A C41A H41A 109.4 . . ? C42A C41A H41B 109.4 . . ? N2A C41A H41B 109.4 . . ? H41A C41A H41B 108.0 . . ? C44A C43A C42A 100.2(8) . . ? C44A C43A H43A 111.7 . . ? C42A C43A H43A 111.7 . . ? C44A C43A H43B 111.7 . . ? C42A C43A H43B 111.7 . . ? H43A C43A H43B 109.5 . . ? C41A C42A C43A 106.8(9) . . ? C41A C42A H42A 110.4 . . ? C43A C42A H42A 110.4 . . ? C41A C42A H42B 110.4 . . ? C43A C42A H42B 110.4 . . ? H42A C42A H42B 108.6 . . ? C45A C44A C43A 126.8(10) . . ? C45A C44A H44A 105.6 . . ? C43A C44A H44A 105.6 . . ? C45A C44A H44B 105.6 . . ? C43A C44A H44B 105.6 . . ? H44A C44A H44B 106.1 . . ? C46A C45A C44A 112.6(10) . . ? C46A C45A H45A 109.1 . . ? C44A C45A H45A 109.1 . . ? C46A C45A H45D 109.1 . . ? C44A C45A H45D 109.1 . . ? H45A C45A H45D 107.8 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C38B N2B C39B 105.3(9) . . ? C38B N2B C41B 137.9(13) . . ? C39B N2B C41B 116.5(9) . . ? C39B N1B C37B 105.6(13) . . ? C39B N1B C40B 126.9(12) . . ? C37B N1B C40B 127.5(10) . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N1B C37B C38B 107.8(12) . . ? N1B C37B H37B 126.1 . . ? C38B C37B H37B 126.1 . . ? N2B C38B C37B 104.5(11) . . ? N2B C38B H38B 127.7 . . ? C37B C38B H38B 127.7 . . ? N2B C41B C42B 124.3(16) . . ? N2B C41B H41C 106.3 . . ? C42B C41B H41C 106.3 . . ? N2B C41B H41D 106.3 . . ? C42B C41B H41D 106.3 . . ? H41C C41B H41D 106.4 . . ? C43B C42B C41B 89.5(14) . . ? C43B C42B H42C 113.7 . . ? C41B C42B H42C 113.7 . . ? C43B C42B H42D 113.7 . . ? C41B C42B H42D 113.7 . . ? H42C C42B H42D 111.0 . . ? N1B C39B N2B 115.6(11) . . ? N1B C39B H39B 122.2 . . ? N2B C39B H39B 122.2 . . ? C43B C44B C45B 130.8(17) . . ? C43B C44B H44C 104.6 . . ? C45B C44B H44C 104.6 . . ? C43B C44B H44D 104.6 . . ? C45B C44B H44D 104.6 . . ? H44C C44B H44D 105.7 . . ? C44B C43B C42B 123.5(15) . . ? C44B C43B H43C 106.4 . . ? C42B C43B H43C 106.4 . . ? C44B C43B H43D 106.5 . . ? C42B C43B H43D 106.5 . . ? H43C C43B H43D 106.5 . . ? C46B C45B C44B 104.5(10) . . ? C46B C45B H45B 110.8 . . ? C44B C45B H45B 110.8 . . ? C46B C45B H45C 110.8 . . ? C44B C45B H45C 110.8 . . ? H45B C45B H45C 108.9 . . ? C45B C46B H46G 109.5 . . ? C45B C46B H46D 109.5 . . ? H46G C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46G C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 La2 Cl1 La1 -24.55(7) . . . . ? O10 La2 Cl1 La1 130.01(7) 3 . . . ? O11 La2 Cl1 La1 88.35(17) 4_565 . . . ? O8 La2 Cl1 La1 51.91(6) 4_565 . . . ? O9 La2 Cl1 La1 -88.61(7) . . . . ? O12 La2 Cl1 La1 -139.37(8) 2_545 . . . ? O11 La2 Cl1 La1 -165.42(5) 2_545 . . . ? C36 La2 Cl1 La1 -150.89(8) 2_545 . . . ? La2 La2 Cl1 La1 177.549(11) 3 . . . ? O7 La1 Cl1 La2 -39.73(7) 4_565 . . . ? O1 La1 Cl1 La2 -49.06(16) . . . . ? O5 La1 Cl1 La2 115.97(8) 4_566 . . . ? O6 La1 Cl1 La2 -114.84(7) 2_644 . . . ? O2 La1 Cl1 La2 167.02(8) 3_655 . . . ? O3 La1 Cl1 La2 44.23(7) . . . . ? O7 La1 O1 C1 -155.2(4) 4_565 . . . ? O5 La1 O1 C1 46.3(4) 4_566 . . . ? O6 La1 O1 C1 -79.3(4) 2_644 . . . ? O2 La1 O1 C1 -10.0(4) 3_655 . . . ? O3 La1 O1 C1 123.4(4) . . . . ? Cl1 La1 O1 C1 -146.1(3) . . . . ? O7 La1 O3 C13 28.2(4) 4_565 . . . ? O1 La1 O3 C13 108.0(4) . . . . ? O5 La1 O3 C13 -176.3(4) 4_566 . . . ? O6 La1 O3 C13 21.2(5) 2_644 . . . ? O2 La1 O3 C13 -114.3(4) 3_655 . . . ? Cl1 La1 O3 C13 -47.8(4) . . . . ? O10 La2 O4 C13 -113.7(4) 3 . . . ? O11 La2 O4 C13 156.2(4) 4_565 . . . ? O8 La2 O4 C13 -127.5(4) 4_565 . . . ? O9 La2 O4 C13 87.5(4) . . . . ? O12 La2 O4 C13 23.4(4) 2_545 . . . ? O11 La2 O4 C13 70.2(4) 2_545 . . . ? Cl1 La2 O4 C13 -42.0(4) . . . . ? C36 La2 O4 C13 43.0(4) 2_545 . . . ? La2 La2 O4 C13 119.5(4) 3 . . . ? O4 La2 O9 C25 131.6(4) . . . . ? O10 La2 O9 C25 -35.8(4) 3 . . . ? O11 La2 O9 C25 21.5(3) 4_565 . . . ? O8 La2 O9 C25 81.3(4) 4_565 . . . ? O12 La2 O9 C25 -110.1(4) 2_545 . . . ? O11 La2 O9 C25 -60.2(3) 2_545 . . . ? Cl1 La2 O9 C25 -159.6(3) . . . . ? C36 La2 O9 C25 -86.2(4) 2_545 . . . ? La2 La2 O9 C25 -22.8(3) 3 . . . ? La1 O1 C1 O2 -4.5(7) . . . . ? La1 O1 C1 C2 172.5(2) . . . . ? La1 O2 C1 O1 22.5(7) 3_655 . . . ? La1 O2 C1 C2 -154.5(3) 3_655 . . . ? O1 C1 C2 C3 -41.6(5) . . . . ? O2 C1 C2 C3 135.7(4) . . . . ? O1 C1 C2 C7 139.1(3) . . . . ? O2 C1 C2 C7 -43.7(5) . . . . ? C7 C2 C3 C4 1.5(5) . . . . ? C1 C2 C3 C4 -177.9(3) . . . . ? C2 C3 C4 C5 0.9(6) . . . . ? C3 C4 C5 C6 -3.7(5) . . . . ? C3 C4 C5 C12 174.0(3) . . . . ? C4 C5 C6 C11 -173.8(3) . . . . ? C12 C5 C6 C11 8.7(5) . . . . ? C4 C5 C6 C7 4.0(5) . . . . ? C12 C5 C6 C7 -173.6(3) . . . . ? C3 C2 C7 C8 177.8(3) . . . . ? C1 C2 C7 C8 -2.8(5) . . . . ? C3 C2 C7 C6 -1.1(5) . . . . ? C1 C2 C7 C6 178.3(3) . . . . ? C11 C6 C7 C8 -2.7(5) . . . . ? C5 C6 C7 C8 179.4(3) . . . . ? C11 C6 C7 C2 176.2(3) . . . . ? C5 C6 C7 C2 -1.6(5) . . . . ? C2 C7 C8 C9 -176.9(4) . . . . ? C6 C7 C8 C9 2.0(5) . . . . ? C7 C8 C9 C10 0.1(6) . . . . ? C8 C9 C10 C11 -1.4(6) . . . . ? C9 C10 C11 C6 0.5(6) . . . . ? C7 C6 C11 C10 1.5(5) . . . . ? C5 C6 C11 C10 179.3(3) . . . . ? La1 O5 C12 O6 34.7(19) 4_565 . . . ? La1 O5 C12 C5 -142.7(15) 4_565 . . . ? La1 O6 C12 O5 3.8(5) 2_654 . . . ? La1 O6 C12 C5 -178.8(2) 2_654 . . . ? C4 C5 C12 O5 35.8(5) . . . . ? C6 C5 C12 O5 -146.6(3) . . . . ? C4 C5 C12 O6 -141.8(4) . . . . ? C6 C5 C12 O6 35.9(5) . . . . ? La1 O3 C13 O4 3.2(6) . . . . ? La1 O3 C13 C14 -179.2(2) . . . . ? La2 O4 C13 O3 67.9(6) . . . . ? La2 O4 C13 C14 -109.7(4) . . . . ? O3 C13 C14 C15 -33.0(5) . . . . ? O4 C13 C14 C15 144.8(3) . . . . ? O3 C13 C14 C19 149.6(3) . . . . ? O4 C13 C14 C19 -32.6(5) . . . . ? C19 C14 C15 C16 1.4(6) . . . . ? C13 C14 C15 C16 -176.2(3) . . . . ? C14 C15 C16 C17 1.4(6) . . . . ? C15 C16 C17 C18 -2.1(5) . . . . ? C15 C16 C17 C24 179.5(3) . . . . ? C16 C17 C18 C23 -177.8(3) . . . . ? C24 C17 C18 C23 0.5(5) . . . . ? C16 C17 C18 C19 0.1(5) . . . . ? C24 C17 C18 C19 178.4(3) . . . . ? C15 C14 C19 C20 174.8(3) . . . . ? C13 C14 C19 C20 -7.8(5) . . . . ? C15 C14 C19 C18 -3.3(5) . . . . ? C13 C14 C19 C18 174.1(3) . . . . ? C23 C18 C19 C20 2.3(4) . . . . ? C17 C18 C19 C20 -175.6(3) . . . . ? C23 C18 C19 C14 -179.4(3) . . . . ? C17 C18 C19 C14 2.6(4) . . . . ? C14 C19 C20 C21 -179.3(3) . . . . ? C18 C19 C20 C21 -1.1(5) . . . . ? C19 C20 C21 C22 -0.6(6) . . . . ? C20 C21 C22 C23 1.0(6) . . . . ? C21 C22 C23 C18 0.3(5) . . . . ? C17 C18 C23 C22 175.9(3) . . . . ? C19 C18 C23 C22 -1.9(4) . . . . ? La1 O7 C24 O8 9.6(12) 4_566 . . . ? La1 O7 C24 C17 -169.3(8) 4_566 . . . ? La2 O8 C24 O7 -28.1(5) 4_566 . . . ? La2 O8 C24 C17 150.7(2) 4_566 . . . ? C16 C17 C24 O7 32.6(4) . . . . ? C18 C17 C24 O7 -145.8(3) . . . . ? C16 C17 C24 O8 -146.3(3) . . . . ? C18 C17 C24 O8 35.4(5) . . . . ? La2 O9 C25 O10 24.0(6) . . . . ? La2 O9 C25 C26 -158.4(2) . . . . ? La2 O10 C25 O9 3.3(7) 3 . . . ? La2 O10 C25 C26 -174.4(2) 3 . . . ? O9 C25 C26 C27 -50.7(5) . . . . ? O10 C25 C26 C27 127.1(4) . . . . ? O9 C25 C26 C31 135.4(4) . . . . ? O10 C25 C26 C31 -46.7(5) . . . . ? C31 C26 C27 C28 5.4(5) . . . . ? C25 C26 C27 C28 -168.6(3) . . . . ? C26 C27 C28 C29 0.8(6) . . . . ? C27 C28 C29 C30 -7.3(5) . . . . ? C27 C28 C29 C36 167.8(3) . . . . ? C28 C29 C30 C35 -170.7(3) . . . . ? C36 C29 C30 C35 14.3(5) . . . . ? C28 C29 C30 C31 7.4(5) . . . . ? C36 C29 C30 C31 -167.5(3) . . . . ? C35 C30 C31 C32 -0.2(5) . . . . ? C29 C30 C31 C32 -178.5(3) . . . . ? C35 C30 C31 C26 176.9(3) . . . . ? C29 C30 C31 C26 -1.3(5) . . . . ? C27 C26 C31 C32 172.1(3) . . . . ? C25 C26 C31 C32 -14.1(5) . . . . ? C27 C26 C31 C30 -5.0(5) . . . . ? C25 C26 C31 C30 168.9(3) . . . . ? C30 C31 C32 C33 1.6(5) . . . . ? C26 C31 C32 C33 -175.5(4) . . . . ? C31 C32 C33 C34 -0.8(6) . . . . ? C32 C33 C34 C35 -1.3(7) . . . . ? C33 C34 C35 C30 2.7(7) . . . . ? C31 C30 C35 C34 -1.9(5) . . . . ? C29 C30 C35 C34 176.3(4) . . . . ? La2 O12 C36 O11 7.7(4) 2 . . . ? La2 O12 C36 C29 -175.2(3) 2 . . . ? La2 O11 C36 O12 -124.7(5) 4_566 . . . ? La2 O11 C36 O12 -6.5(4) 2 . . . ? La2 O11 C36 C29 58.2(8) 4_566 . . . ? La2 O11 C36 C29 176.4(3) 2 . . . ? La2 O11 C36 La2 -118.3(6) 4_566 . . 2 ? C28 C29 C36 O12 -135.8(4) . . . . ? C30 C29 C36 O12 39.2(5) . . . . ? C28 C29 C36 O11 41.4(5) . . . . ? C30 C29 C36 O11 -143.6(3) . . . . ? C28 C29 C36 La2 -157.9(12) . . . 2 ? C30 C29 C36 La2 17.1(15) . . . 2 ? C39A N1A C37A C38A -0.3(12) . . . . ? C40A N1A C37A C38A 176.4(6) . . . . ? C39A N2A C38A C37A -0.4(12) . . . . ? C41A N2A C38A C37A 178.3(9) . . . . ? N1A C37A C38A N2A 0.4(8) . . . . ? C37A N1A C39A N2A 0.1(16) . . . . ? C40A N1A C39A N2A -176.4(8) . . . . ? C38A N2A C39A N1A 0.2(16) . . . . ? C41A N2A C39A N1A -178.6(10) . . . . ? C38A N2A C41A C42A -16.9(15) . . . . ? C39A N2A C41A C42A 161.7(12) . . . . ? N2A C41A C42A C43A -71.2(11) . . . . ? C44A C43A C42A C41A -167.9(8) . . . . ? C42A C43A C44A C45A -89.5(14) . . . . ? C43A C44A C45A C46A -114.0(15) . . . . ? C39B N1B C37B C38B -7(2) . . . . ? C40B N1B C37B C38B 174.1(15) . . . . ? C39B N2B C38B C37B -10(3) . . . . ? C41B N2B C38B C37B 176(2) . . . . ? N1B C37B C38B N2B 11(2) . . . . ? C38B N2B C41B C42B -119(3) . . . . ? C39B N2B C41B C42B 68(3) . . . . ? N2B C41B C42B C43B 133.2(17) . . . . ? C37B N1B C39B N2B 1(3) . . . . ? C40B N1B C39B N2B 180(2) . . . . ? C38B N2B C39B N1B 7(4) . . . . ? C41B N2B C39B N1B -178(2) . . . . ? C45B C44B C43B C42B -93(3) . . . . ? C41B C42B C43B C44B -83(2) . . . . ? C43B C44B C45B C46B -106(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.929 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.084 #===END data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 876522' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Ce2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Ce2 Cl N2 O12' _chemical_formula_weight 1125.47 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.0206(3) _cell_length_b 14.8154(2) _cell_length_c 16.1806(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.0266(14) _cell_angle_gamma 90.00 _cell_volume 4296.05(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12389 _cell_measurement_theta_min 2.4779 _cell_measurement_theta_max 28.8226 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 2.222 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85634 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18726 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8921 _reflns_number_gt 7218 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0301P)^2^+4.9529P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8921 _refine_ls_number_parameters 607 _refine_ls_number_restraints 379 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.058 _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 Ce1 Ce 0.378059(9) 0.025211(12) -0.005556(10) 0.01596(5) Uani 1 1 d . . . Ce2 Ce 0.114910(9) 0.013498(12) -0.001187(11) 0.01647(5) Uani 1 1 d . . . Cl1 Cl 0.25182(4) -0.08876(6) 0.02308(6) 0.0337(2) Uani 1 1 d . . . O1 O 0.44827(13) 0.13195(19) -0.07843(18) 0.0416(7) Uani 1 1 d . . . O2 O 0.57120(14) 0.11238(18) -0.06065(18) 0.0414(7) Uani 1 1 d . . . O3 O 0.31588(14) 0.1357(2) 0.07472(19) 0.0480(8) Uani 1 1 d . . . O5 O 0.47701(15) 0.4321(2) -0.40076(18) 0.0498(8) Uani 1 1 d . . . O4 O 0.19574(13) 0.13934(18) 0.02984(17) 0.0376(7) Uani 1 1 d . . . O6 O 0.59980(15) 0.4314(2) -0.37726(17) 0.0477(8) Uani 1 1 d . . . O7 O 0.28305(13) 0.43157(19) 0.38866(16) 0.0377(7) Uani 1 1 d . . . O8 O 0.16016(12) 0.44828(18) 0.36526(14) 0.0314(6) Uani 1 1 d . . . O9 O 0.06214(14) 0.10088(19) 0.10954(17) 0.0415(7) Uani 1 1 d . . . O10 O -0.06236(14) 0.10581(19) 0.08978(18) 0.0424(7) Uani 1 1 d . . . O11 O 0.00408(14) 0.41606(18) 0.43284(16) 0.0364(6) Uani 1 1 d . . . O12 O -0.11270(14) 0.4108(2) 0.37873(18) 0.0496(8) Uani 1 1 d . . . C1 C 0.51324(18) 0.1507(2) -0.0928(2) 0.0287(8) Uani 1 1 d . . . C2 C 0.52130(17) 0.2236(2) -0.1564(2) 0.0259(8) Uani 1 1 d . . . C3 C 0.47212(19) 0.2227(3) -0.2270(2) 0.0344(9) Uani 1 1 d . . . H3A H 0.4348 0.1792 -0.2326 0.041 Uiso 1 1 calc R . . C4 C 0.47662(19) 0.2857(3) -0.2906(2) 0.0335(9) Uani 1 1 d . . . H4A H 0.4420 0.2838 -0.3375 0.040 Uiso 1 1 calc R . . C5 C 0.53120(18) 0.3498(2) -0.2847(2) 0.0265(8) Uani 1 1 d . . . C6 C 0.58299(17) 0.3560(2) -0.2112(2) 0.0236(7) Uani 1 1 d . . . C7 C 0.57832(17) 0.2909(2) -0.1470(2) 0.0244(7) Uani 1 1 d . . . C8 C 0.6300(2) 0.2975(3) -0.0747(2) 0.0343(9) Uani 1 1 d . . . H8A H 0.6289 0.2546 -0.0329 0.041 Uiso 1 1 calc R . . C9 C 0.6809(2) 0.3650(3) -0.0654(3) 0.0440(10) Uani 1 1 d . . . H9A H 0.7141 0.3679 -0.0174 0.053 Uiso 1 1 calc R . . C10 C 0.6839(2) 0.4301(3) -0.1273(3) 0.0421(10) Uani 1 1 d . . . H10A H 0.7186 0.4767 -0.1198 0.051 Uiso 1 1 calc R . . C11 C 0.6368(2) 0.4261(3) -0.1983(2) 0.0334(9) Uani 1 1 d . . . H11A H 0.6397 0.4699 -0.2391 0.040 Uiso 1 1 calc R . . C12 C 0.5362(2) 0.4095(3) -0.3591(2) 0.0324(9) Uani 1 1 d . . . C13 C 0.25128(19) 0.1670(2) 0.0758(2) 0.0302(8) Uani 1 1 d . . . C14 C 0.24047(18) 0.2387(2) 0.1394(2) 0.0281(8) Uani 1 1 d . . . C15 C 0.2843(2) 0.2319(3) 0.2136(3) 0.0393(10) Uani 1 1 d . . . H15A H 0.3201 0.1865 0.2207 0.047 Uiso 1 1 calc R . . C16 C 0.2765(2) 0.2917(3) 0.2789(2) 0.0375(10) Uani 1 1 d . . . H16A H 0.3077 0.2860 0.3282 0.045 Uiso 1 1 calc R . . C17 C 0.22375(17) 0.3585(2) 0.2719(2) 0.0233(7) Uani 1 1 d . . . C18 C 0.17671(16) 0.3689(2) 0.1957(2) 0.0212(7) Uani 1 1 d . . . C19 C 0.18616(17) 0.3091(2) 0.1279(2) 0.0235(7) Uani 1 1 d . . . C20 C 0.1427(2) 0.3249(3) 0.0511(2) 0.0349(9) Uani 1 1 d . . . H20A H 0.1487 0.2875 0.0061 0.042 Uiso 1 1 calc R . . C21 C 0.0927(2) 0.3933(3) 0.0417(2) 0.0403(10) Uani 1 1 d . . . H21A H 0.0653 0.4027 -0.0096 0.048 Uiso 1 1 calc R . . C22 C 0.0819(2) 0.4496(3) 0.1083(3) 0.0403(10) Uani 1 1 d . . . H22A H 0.0467 0.4956 0.1013 0.048 Uiso 1 1 calc R . . C23 C 0.12217(18) 0.4384(2) 0.1834(2) 0.0270(8) Uani 1 1 d . . . H23A H 0.1140 0.4765 0.2272 0.032 Uiso 1 1 calc R . . C24 C 0.22129(17) 0.4179(2) 0.3472(2) 0.0239(7) Uani 1 1 d . . . C25 C 0.0004(2) 0.1337(3) 0.1218(2) 0.0324(9) Uani 1 1 d . . . C26 C -0.00218(18) 0.2117(2) 0.1799(2) 0.0281(8) Uani 1 1 d . . . C27 C 0.0364(2) 0.2058(3) 0.2568(3) 0.0391(10) Uani 1 1 d . . . H27A H 0.0705 0.1591 0.2681 0.047 Uiso 1 1 calc R . . C28 C 0.0257(2) 0.2689(3) 0.3194(2) 0.0375(9) Uani 1 1 d . . . H28A H 0.0525 0.2635 0.3714 0.045 Uiso 1 1 calc R . . C29 C -0.02417(19) 0.3383(3) 0.3042(2) 0.0298(8) Uani 1 1 d . . . C30 C -0.05941(19) 0.3531(2) 0.2220(2) 0.0279(8) Uani 1 1 d . . . C31 C -0.04859(19) 0.2884(3) 0.1593(2) 0.0299(8) Uani 1 1 d . . . C32 C -0.0818(2) 0.3040(3) 0.0774(2) 0.0417(10) Uani 1 1 d . . . H32A H -0.0762 0.2618 0.0359 0.050 Uiso 1 1 calc R . . C33 C -0.1217(3) 0.3804(4) 0.0592(3) 0.0576(13) Uani 1 1 d . . . H33A H -0.1425 0.3905 0.0049 0.069 Uiso 1 1 calc R . . C34 C -0.1319(3) 0.4433(4) 0.1200(3) 0.0590(13) Uani 1 1 d . . . H34A H -0.1592 0.4953 0.1056 0.071 Uiso 1 1 calc R . . C35 C -0.1031(2) 0.4310(3) 0.2003(3) 0.0432(10) Uani 1 1 d . . . H35A H -0.1118 0.4732 0.2407 0.052 Uiso 1 1 calc R . . C36 C -0.0454(2) 0.3928(3) 0.3749(2) 0.0326(9) Uani 1 1 d . . . N1A N 0.2377(7) -0.2679(8) 0.2812(6) 0.0617(15) Uani 0.562(6) 1 d PDU A 1 N2A N 0.3064(9) -0.1503(10) 0.2671(9) 0.0706(14) Uani 0.562(6) 1 d PDU A 1 C37A C 0.2889(6) -0.2642(8) 0.3476(7) 0.0628(18) Uani 0.562(6) 1 d PDU A 1 H37A H 0.2939 -0.3046 0.3918 0.075 Uiso 0.562(6) 1 calc PR A 1 C38A C 0.3335(8) -0.1878(9) 0.3378(8) 0.0739(18) Uani 0.562(6) 1 d PDU A 1 H38A H 0.3738 -0.1679 0.3738 0.089 Uiso 0.562(6) 1 calc PR A 1 C39A C 0.2531(11) -0.2056(12) 0.2279(10) 0.0563(14) Uani 0.562(6) 1 d PDU A 1 H39A H 0.2317 -0.2002 0.1733 0.068 Uiso 0.562(6) 1 calc PR A 1 C40A C 0.1830(7) -0.3370(9) 0.2628(8) 0.085(3) Uani 0.562(6) 1 d PDU A 1 H40A H 0.1497 -0.3196 0.2152 0.128 Uiso 0.562(6) 1 calc PR A 1 H40B H 0.1551 -0.3452 0.3097 0.128 Uiso 0.562(6) 1 calc PR A 1 H40C H 0.2074 -0.3925 0.2513 0.128 Uiso 0.562(6) 1 calc PR A 1 C41A C 0.3332(8) -0.0684(8) 0.2288(7) 0.0909(19) Uani 0.562(6) 1 d PDU A 1 H41A H 0.2915 -0.0313 0.2067 0.109 Uiso 0.562(6) 1 calc PR A 1 H41B H 0.3623 -0.0841 0.1837 0.109 Uiso 0.562(6) 1 calc PR A 1 C43A C 0.3265(8) 0.0294(9) 0.3517(9) 0.130(2) Uani 0.562(6) 1 d PDU A 1 H43A H 0.2844 0.0559 0.3180 0.156 Uiso 0.562(6) 1 calc PR A 1 H43B H 0.3077 -0.0138 0.3896 0.156 Uiso 0.562(6) 1 calc PR A 1 C42A C 0.3802(8) -0.0189(9) 0.2947(8) 0.117(2) Uani 0.562(6) 1 d PDU A 1 H42A H 0.4108 0.0254 0.2700 0.140 Uiso 0.562(6) 1 calc PR A 1 H42B H 0.4129 -0.0606 0.3273 0.140 Uiso 0.562(6) 1 calc PR A 1 C44A C 0.3720(10) 0.1030(9) 0.4005(8) 0.153(3) Uani 0.562(6) 1 d PDU A 1 H44A H 0.4028 0.1317 0.3624 0.183 Uiso 0.562(6) 1 calc PR A 1 H44B H 0.3369 0.1483 0.4157 0.183 Uiso 0.562(6) 1 calc PR A 1 C45A C 0.4229(9) 0.0797(11) 0.4794(9) 0.161(3) Uani 0.562(6) 1 d PDU A 1 H45A H 0.4190 0.0159 0.4913 0.193 Uiso 0.562(6) 1 calc PR A 1 H45D H 0.4743 0.0926 0.4709 0.193 Uiso 0.562(6) 1 calc PR A 1 C46A C 0.4010(11) 0.1346(13) 0.5528(8) 0.181(5) Uani 0.562(6) 1 d PDU A 1 H46A H 0.4316 0.1171 0.6024 0.272 Uiso 0.562(6) 1 calc PR A 1 H46B H 0.3495 0.1236 0.5598 0.272 Uiso 0.562(6) 1 calc PR A 1 H46C H 0.4081 0.1976 0.5425 0.272 Uiso 0.562(6) 1 calc PR A 1 N2B N 0.3122(12) -0.1641(13) 0.2743(12) 0.0706(14) Uani 0.438(6) 1 d PDU A 2 N1B N 0.2279(10) -0.2686(10) 0.2560(8) 0.0617(15) Uani 0.438(6) 1 d PDU A 2 C40B C 0.1711(9) -0.3233(12) 0.2146(10) 0.085(3) Uani 0.438(6) 1 d PDU A 2 H40D H 0.1608 -0.3034 0.1580 0.128 Uiso 0.438(6) 1 calc PR A 2 H40E H 0.1266 -0.3185 0.2422 0.128 Uiso 0.438(6) 1 calc PR A 2 H40F H 0.1874 -0.3850 0.2154 0.128 Uiso 0.438(6) 1 calc PR A 2 C37B C 0.2634(8) -0.2786(10) 0.3330(9) 0.0628(18) Uani 0.438(6) 1 d PDU A 2 H37B H 0.2531 -0.3218 0.3719 0.075 Uiso 0.438(6) 1 calc PR A 2 C38B C 0.3188(10) -0.2121(12) 0.3435(10) 0.0739(18) Uani 0.438(6) 1 d PDU A 2 H38B H 0.3532 -0.2035 0.3898 0.089 Uiso 0.438(6) 1 calc PR A 2 C41B C 0.3588(8) -0.0877(8) 0.2540(11) 0.0909(19) Uani 0.438(6) 1 d PDU A 2 H41C H 0.3745 -0.0964 0.1991 0.109 Uiso 0.438(6) 1 calc PR A 2 H41D H 0.4031 -0.0853 0.2935 0.109 Uiso 0.438(6) 1 calc PR A 2 C42B C 0.3160(9) 0.0023(10) 0.2564(10) 0.117(2) Uani 0.438(6) 1 d PDU A 2 H42C H 0.2696 -0.0010 0.2816 0.140 Uiso 0.438(6) 1 calc PR A 2 H42D H 0.3105 0.0354 0.2044 0.140 Uiso 0.438(6) 1 calc PR A 2 C39B C 0.2514(15) -0.1936(15) 0.2245(13) 0.0563(14) Uani 0.438(6) 1 d PDU A 2 H39B H 0.2303 -0.1653 0.1763 0.068 Uiso 0.438(6) 1 calc PR A 2 C44B C 0.3793(13) 0.0463(12) 0.4048(9) 0.153(3) Uani 0.438(6) 1 d PDU A 2 H44C H 0.4292 0.0304 0.4287 0.183 Uiso 0.438(6) 1 calc PR A 2 H44D H 0.3488 -0.0044 0.4185 0.183 Uiso 0.438(6) 1 calc PR A 2 C43B C 0.3854(10) 0.0281(13) 0.3166(10) 0.130(2) Uani 0.438(6) 1 d PDU A 2 H43C H 0.4215 -0.0203 0.3143 0.156 Uiso 0.438(6) 1 calc PR A 2 H43D H 0.4071 0.0814 0.2939 0.156 Uiso 0.438(6) 1 calc PR A 2 C45B C 0.3580(10) 0.1164(14) 0.4689(12) 0.161(3) Uani 0.438(6) 1 d PDU A 2 H45B H 0.3238 0.0899 0.5046 0.193 Uiso 0.438(6) 1 calc PR A 2 H45C H 0.3339 0.1680 0.4407 0.193 Uiso 0.438(6) 1 calc PR A 2 C46B C 0.4320(13) 0.1466(17) 0.5219(12) 0.181(5) Uani 0.438(6) 1 d PDU A 2 H46G H 0.4218 0.1974 0.5558 0.272 Uiso 0.438(6) 1 calc PR A 2 H46D H 0.4684 0.1632 0.4854 0.272 Uiso 0.438(6) 1 calc PR A 2 H46E H 0.4508 0.0976 0.5568 0.272 Uiso 0.438(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.01543(9) 0.01759(10) 0.01507(9) -0.00014(7) 0.00254(6) 0.00099(7) Ce2 0.01522(9) 0.01826(10) 0.01626(9) -0.00022(7) 0.00320(6) -0.00160(7) Cl1 0.0206(4) 0.0304(5) 0.0512(6) 0.0136(4) 0.0091(4) 0.0027(3) O1 0.0245(13) 0.0458(17) 0.0550(19) 0.0253(14) 0.0067(12) -0.0059(12) O2 0.0296(14) 0.0366(16) 0.0573(19) 0.0245(14) 0.0016(12) 0.0035(12) O3 0.0324(15) 0.0496(18) 0.062(2) -0.0328(16) 0.0056(13) 0.0091(13) O5 0.0487(17) 0.0518(19) 0.0438(18) 0.0228(15) -0.0200(14) -0.0010(14) O4 0.0321(14) 0.0350(15) 0.0470(17) -0.0224(13) 0.0095(12) -0.0120(12) O6 0.0474(17) 0.062(2) 0.0345(16) 0.0247(15) 0.0076(13) -0.0124(15) O7 0.0230(12) 0.0579(19) 0.0312(15) -0.0201(13) -0.0014(11) -0.0031(12) O8 0.0243(12) 0.0484(16) 0.0221(13) -0.0098(12) 0.0056(10) 0.0087(11) O9 0.0324(14) 0.0509(18) 0.0434(17) -0.0255(14) 0.0147(12) -0.0054(13) O10 0.0308(14) 0.0457(17) 0.0522(18) -0.0297(14) 0.0113(12) -0.0138(12) O11 0.0347(14) 0.0417(16) 0.0329(15) -0.0169(12) 0.0048(11) -0.0116(12) O12 0.0233(14) 0.073(2) 0.0548(19) -0.0405(17) 0.0143(12) -0.0090(13) C1 0.0248(18) 0.0257(19) 0.036(2) 0.0128(16) 0.0040(15) -0.0010(14) C2 0.0179(16) 0.0271(19) 0.033(2) 0.0116(15) 0.0033(14) 0.0004(13) C3 0.0224(18) 0.037(2) 0.043(2) 0.0139(18) -0.0023(16) -0.0089(16) C4 0.0228(18) 0.042(2) 0.034(2) 0.0125(17) -0.0067(15) -0.0061(16) C5 0.0210(16) 0.033(2) 0.0250(19) 0.0106(15) 0.0016(14) 0.0015(14) C6 0.0198(16) 0.0269(18) 0.0245(18) 0.0068(14) 0.0038(13) -0.0003(13) C7 0.0188(16) 0.0283(19) 0.0264(19) 0.0067(15) 0.0038(13) 0.0000(13) C8 0.036(2) 0.043(2) 0.023(2) 0.0094(17) -0.0010(15) -0.0047(17) C9 0.040(2) 0.058(3) 0.032(2) 0.001(2) -0.0093(18) -0.014(2) C10 0.039(2) 0.044(3) 0.043(2) -0.002(2) 0.0020(18) -0.0191(19) C11 0.034(2) 0.035(2) 0.031(2) 0.0079(17) 0.0048(16) -0.0083(16) C12 0.037(2) 0.033(2) 0.026(2) 0.0098(16) -0.0032(16) -0.0042(16) C13 0.0269(18) 0.0269(19) 0.038(2) -0.0135(16) 0.0103(16) -0.0050(15) C14 0.0220(17) 0.033(2) 0.031(2) -0.0133(16) 0.0060(14) -0.0013(14) C15 0.032(2) 0.042(2) 0.043(2) -0.0159(19) -0.0025(17) 0.0178(17) C16 0.031(2) 0.049(3) 0.031(2) -0.0128(18) -0.0060(16) 0.0127(17) C17 0.0179(16) 0.0287(19) 0.0232(18) -0.0092(14) 0.0013(13) 0.0010(13) C18 0.0169(15) 0.0238(17) 0.0231(18) -0.0038(14) 0.0033(13) -0.0028(13) C19 0.0196(16) 0.0278(18) 0.0232(18) -0.0072(14) 0.0024(13) -0.0050(13) C20 0.042(2) 0.041(2) 0.0211(19) -0.0078(17) -0.0007(16) -0.0049(18) C21 0.044(2) 0.049(3) 0.027(2) -0.0013(18) -0.0063(17) 0.0054(19) C22 0.038(2) 0.037(2) 0.044(2) 0.0032(19) -0.0028(18) 0.0126(18) C23 0.0268(17) 0.0265(19) 0.0279(19) -0.0037(15) 0.0035(14) 0.0026(14) C24 0.0221(16) 0.0317(19) 0.0181(17) -0.0047(14) 0.0024(13) 0.0000(14) C25 0.032(2) 0.036(2) 0.032(2) -0.0131(17) 0.0148(16) -0.0097(16) C26 0.0225(17) 0.033(2) 0.030(2) -0.0140(16) 0.0100(14) -0.0074(15) C27 0.031(2) 0.044(2) 0.042(2) -0.0154(19) 0.0018(17) 0.0076(17) C28 0.034(2) 0.048(3) 0.029(2) -0.0155(18) -0.0035(16) 0.0031(18) C29 0.0248(18) 0.035(2) 0.030(2) -0.0154(16) 0.0073(15) -0.0072(15) C30 0.0252(17) 0.0291(19) 0.030(2) -0.0078(15) 0.0078(15) -0.0058(15) C31 0.0272(18) 0.035(2) 0.028(2) -0.0080(16) 0.0085(15) -0.0106(16) C32 0.049(2) 0.048(3) 0.028(2) -0.0063(19) 0.0037(18) -0.013(2) C33 0.059(3) 0.074(4) 0.037(3) 0.013(3) -0.006(2) -0.006(3) C34 0.048(3) 0.055(3) 0.073(4) 0.018(3) 0.005(2) 0.008(2) C35 0.045(2) 0.038(2) 0.048(3) -0.002(2) 0.012(2) 0.0016(19) C36 0.0300(19) 0.038(2) 0.031(2) -0.0170(17) 0.0109(15) -0.0112(16) N1A 0.072(3) 0.053(2) 0.064(4) 0.009(3) 0.025(3) 0.021(2) N2A 0.095(3) 0.066(3) 0.051(3) 0.005(2) 0.013(2) 0.009(3) C37A 0.081(4) 0.054(3) 0.053(3) 0.014(3) 0.004(3) 0.013(3) C38A 0.096(4) 0.070(4) 0.056(3) 0.010(3) 0.009(3) 0.013(3) C39A 0.068(3) 0.052(4) 0.050(3) 0.013(2) 0.013(2) 0.009(3) C40A 0.083(5) 0.061(5) 0.121(9) -0.004(7) 0.056(7) 0.011(4) C41A 0.125(4) 0.071(4) 0.078(4) 0.007(3) 0.015(3) -0.017(3) C43A 0.191(5) 0.089(4) 0.117(5) 0.010(4) 0.045(4) -0.020(4) C42A 0.165(4) 0.083(4) 0.105(4) 0.002(4) 0.027(4) -0.016(4) C44A 0.228(5) 0.101(5) 0.131(5) 0.029(5) 0.034(5) -0.016(5) C45A 0.238(6) 0.105(5) 0.143(6) 0.023(5) 0.036(5) -0.018(5) C46A 0.280(10) 0.124(8) 0.153(9) -0.005(8) 0.087(9) -0.032(8) N2B 0.095(3) 0.066(3) 0.051(3) 0.005(2) 0.013(2) 0.009(3) N1B 0.072(3) 0.053(2) 0.064(4) 0.009(3) 0.025(3) 0.021(2) C40B 0.083(5) 0.061(5) 0.121(9) -0.004(7) 0.056(7) 0.011(4) C37B 0.081(4) 0.054(3) 0.053(3) 0.014(3) 0.004(3) 0.013(3) C38B 0.096(4) 0.070(4) 0.056(3) 0.010(3) 0.009(3) 0.013(3) C41B 0.125(4) 0.071(4) 0.078(4) 0.007(3) 0.015(3) -0.017(3) C42B 0.165(4) 0.083(4) 0.105(4) 0.002(4) 0.027(4) -0.016(4) C39B 0.068(3) 0.052(4) 0.050(3) 0.013(2) 0.013(2) 0.009(3) C44B 0.228(5) 0.101(5) 0.131(5) 0.029(5) 0.034(5) -0.016(5) C43B 0.191(5) 0.089(4) 0.117(5) 0.010(4) 0.045(4) -0.020(4) C45B 0.238(6) 0.105(5) 0.143(6) 0.023(5) 0.036(5) -0.018(5) C46B 0.280(10) 0.124(8) 0.153(9) -0.005(8) 0.087(9) -0.032(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O7 2.378(2) 4_565 ? Ce1 O1 2.409(2) . ? Ce1 O5 2.413(2) 4_566 ? Ce1 O6 2.418(3) 2_644 ? Ce1 O3 2.435(2) . ? Ce1 O2 2.436(2) 3_655 ? Ce1 Cl1 2.9091(8) . ? Ce2 O4 2.387(2) . ? Ce2 O11 2.402(2) 4_565 ? Ce2 O10 2.406(2) 3 ? Ce2 O8 2.455(2) 4_565 ? Ce2 O9 2.480(2) . ? Ce2 O12 2.502(3) 2_545 ? Ce2 Cl1 2.8867(8) . ? Ce2 O11 2.899(3) 2_545 ? Ce2 C36 3.079(4) 2_545 ? O1 C1 1.249(4) . ? O2 C1 1.253(4) . ? O2 Ce1 2.436(2) 3_655 ? O3 C13 1.255(4) . ? O5 C12 1.246(4) . ? O5 Ce1 2.413(2) 4_565 ? O4 C13 1.252(4) . ? O6 C12 1.256(4) . ? O6 Ce1 2.418(3) 2_654 ? O7 C24 1.254(4) . ? O7 Ce1 2.378(2) 4_566 ? O8 C24 1.253(4) . ? O8 Ce2 2.455(2) 4_566 ? O9 C25 1.249(4) . ? O10 C25 1.264(4) . ? O10 Ce2 2.406(2) 3 ? O11 C36 1.271(4) . ? O11 Ce2 2.402(2) 4_566 ? O11 Ce2 2.899(3) 2 ? O12 C36 1.250(4) . ? O12 Ce2 2.502(3) 2 ? C1 C2 1.509(5) . ? C2 C3 1.369(5) . ? C2 C7 1.428(5) . ? C3 C4 1.397(5) . ? C3 H3A 0.9300 . ? C4 C5 1.364(5) . ? C4 H4A 0.9300 . ? C5 C6 1.436(4) . ? C5 C12 1.504(5) . ? C6 C11 1.421(5) . ? C6 C7 1.426(5) . ? C7 C8 1.420(5) . ? C8 C9 1.355(5) . ? C8 H8A 0.9300 . ? C9 C10 1.396(6) . ? C9 H9A 0.9300 . ? C10 C11 1.357(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.506(5) . ? C14 C15 1.370(5) . ? C14 C19 1.429(5) . ? C15 C16 1.398(5) . ? C15 H15A 0.9300 . ? C16 C17 1.368(5) . ? C16 H16A 0.9300 . ? C17 C18 1.429(4) . ? C17 C24 1.508(4) . ? C18 C23 1.423(5) . ? C18 C19 1.434(4) . ? C19 C20 1.417(5) . ? C20 C21 1.354(5) . ? C20 H20A 0.9300 . ? C21 C22 1.394(5) . ? C21 H21A 0.9300 . ? C22 C23 1.358(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.493(5) . ? C26 C27 1.363(5) . ? C26 C31 1.430(5) . ? C27 C28 1.407(5) . ? C27 H27A 0.9300 . ? C28 C29 1.371(5) . ? C28 H28A 0.9300 . ? C29 C30 1.429(5) . ? C29 C36 1.483(5) . ? C30 C35 1.420(5) . ? C30 C31 1.424(5) . ? C31 C32 1.414(5) . ? C32 C33 1.357(6) . ? C32 H32A 0.9300 . ? C33 C34 1.381(7) . ? C33 H33A 0.9300 . ? C34 C35 1.361(6) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 Ce2 3.079(4) 2 ? N1A C39A 1.311(7) . ? N1A C37A 1.341(7) . ? N1A C40A 1.432(9) . ? N2A C38A 1.319(7) . ? N2A C39A 1.367(9) . ? N2A C41A 1.467(9) . ? C37A C38A 1.407(10) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.483(9) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C44A 1.533(9) . ? C43A C42A 1.578(9) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.532(9) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.524(10) . ? C45A H45A 0.9700 . ? C45A H45D 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N2B C38B 1.321(8) . ? N2B C39B 1.361(10) . ? N2B C41B 1.467(9) . ? N1B C39B 1.313(8) . ? N1B C37B 1.348(8) . ? N1B C40B 1.418(9) . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C37B C38B 1.400(11) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C41B C42B 1.542(10) . ? C41B C43B 2.02(2) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.551(10) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C39B H39B 0.9300 . ? C44B C43B 1.468(9) . ? C44B C45B 1.544(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C45B C46B 1.572(10) . ? C45B H45B 0.9700 . ? C45B H45C 0.9700 . ? C46B H46G 0.9600 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? 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 O7 Ce1 O1 81.17(9) 4_565 . ? O7 Ce1 O5 149.13(10) 4_565 4_566 ? O1 Ce1 O5 77.55(10) . 4_566 ? O7 Ce1 O6 75.88(10) 4_565 2_644 ? O1 Ce1 O6 81.68(11) . 2_644 ? O5 Ce1 O6 122.10(10) 4_566 2_644 ? O7 Ce1 O3 82.30(10) 4_565 . ? O1 Ce1 O3 96.57(11) . . ? O5 Ce1 O3 78.24(9) 4_566 . ? O6 Ce1 O3 158.13(10) 2_644 . ? O7 Ce1 O2 138.63(10) 4_565 3_655 ? O1 Ce1 O2 124.91(8) . 3_655 ? O5 Ce1 O2 72.23(10) 4_566 3_655 ? O6 Ce1 O2 77.20(10) 2_644 3_655 ? O3 Ce1 O2 120.04(11) . 3_655 ? O7 Ce1 Cl1 75.82(6) 4_565 . ? O1 Ce1 Cl1 156.71(7) . . ? O5 Ce1 Cl1 124.96(8) 4_566 . ? O6 Ce1 Cl1 89.27(8) 2_644 . ? O3 Ce1 Cl1 83.92(7) . . ? O2 Ce1 Cl1 73.02(6) 3_655 . ? O4 Ce2 O11 102.40(9) . 4_565 ? O4 Ce2 O10 153.17(9) . 3 ? O11 Ce2 O10 78.32(10) 4_565 3 ? O4 Ce2 O8 75.71(9) . 4_565 ? O11 Ce2 O8 81.15(8) 4_565 4_565 ? O10 Ce2 O8 77.96(9) 3 4_565 ? O4 Ce2 O9 73.27(8) . . ? O11 Ce2 O9 74.35(9) 4_565 . ? O10 Ce2 O9 131.08(8) 3 . ? O8 Ce2 O9 134.73(10) 4_565 . ? O4 Ce2 O12 111.63(10) . 2_545 ? O11 Ce2 O12 122.31(8) 4_565 2_545 ? O10 Ce2 O12 89.26(11) 3 2_545 ? O8 Ce2 O12 150.69(9) 4_565 2_545 ? O9 Ce2 O12 72.90(10) . 2_545 ? O4 Ce2 Cl1 83.53(7) . . ? O11 Ce2 Cl1 161.32(7) 4_565 . ? O10 Ce2 Cl1 88.44(7) 3 . ? O8 Ce2 Cl1 83.26(6) 4_565 . ? O9 Ce2 Cl1 124.26(7) . . ? O12 Ce2 Cl1 69.98(6) 2_545 . ? O4 Ce2 O11 140.21(8) . 2_545 ? O11 Ce2 O11 76.83(8) 4_565 2_545 ? O10 Ce2 O11 66.48(8) 3 2_545 ? O8 Ce2 O11 141.09(8) 4_565 2_545 ? O9 Ce2 O11 68.23(8) . 2_545 ? O12 Ce2 O11 47.24(7) 2_545 2_545 ? Cl1 Ce2 O11 110.04(5) . 2_545 ? O4 Ce2 C36 126.59(10) . 2_545 ? O11 Ce2 C36 99.77(9) 4_565 2_545 ? O10 Ce2 C36 78.85(10) 3 2_545 ? O8 Ce2 C36 156.09(10) 4_565 2_545 ? O9 Ce2 C36 67.04(10) . 2_545 ? O12 Ce2 C36 23.05(8) 2_545 2_545 ? Cl1 Ce2 C36 90.38(7) . 2_545 ? O11 Ce2 C36 24.31(8) 2_545 2_545 ? Ce2 Cl1 Ce1 110.19(3) . . ? C1 O1 Ce1 142.0(2) . . ? C1 O2 Ce1 145.1(2) . 3_655 ? C13 O3 Ce1 137.3(2) . . ? C12 O5 Ce1 168.0(3) . 4_565 ? C13 O4 Ce2 144.4(3) . . ? C12 O6 Ce1 124.2(2) . 2_654 ? C24 O7 Ce1 163.7(2) . 4_566 ? C24 O8 Ce2 132.1(2) . 4_566 ? C25 O9 Ce2 137.2(2) . . ? C25 O10 Ce2 139.8(2) . 3 ? C36 O11 Ce2 158.6(3) . 4_566 ? C36 O11 Ce2 85.8(2) . 2 ? Ce2 O11 Ce2 103.17(8) 4_566 2 ? C36 O12 Ce2 105.4(2) . 2 ? O1 C1 O2 125.4(3) . . ? O1 C1 C2 116.5(3) . . ? O2 C1 C2 118.1(3) . . ? C3 C2 C7 119.4(3) . . ? C3 C2 C1 117.5(3) . . ? C7 C2 C1 123.1(3) . . ? C2 C3 C4 121.7(3) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C5 C4 C3 120.7(3) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 C12 117.2(3) . . ? C6 C5 C12 122.5(3) . . ? C11 C6 C7 118.7(3) . . ? C11 C6 C5 122.8(3) . . ? C7 C6 C5 118.5(3) . . ? C8 C7 C6 118.0(3) . . ? C8 C7 C2 122.5(3) . . ? C6 C7 C2 119.4(3) . . ? C9 C8 C7 121.3(4) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C8 C9 C10 120.5(4) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 120.6(4) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C6 120.9(4) . . ? C10 C11 H11A 119.6 . . ? C6 C11 H11A 119.6 . . ? O5 C12 O6 123.7(3) . . ? O5 C12 C5 118.1(3) . . ? O6 C12 C5 118.1(3) . . ? O4 C13 O3 123.8(3) . . ? O4 C13 C14 119.0(3) . . ? O3 C13 C14 117.2(3) . . ? C15 C14 C19 119.5(3) . . ? C15 C14 C13 116.3(3) . . ? C19 C14 C13 124.2(3) . . ? C14 C15 C16 121.4(3) . . ? C14 C15 H15A 119.3 . . ? C16 C15 H15A 119.3 . . ? C17 C16 C15 121.4(3) . . ? C17 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C16 C17 C18 119.6(3) . . ? C16 C17 C24 115.7(3) . . ? C18 C17 C24 124.7(3) . . ? C23 C18 C17 122.5(3) . . ? C23 C18 C19 118.4(3) . . ? C17 C18 C19 119.1(3) . . ? C20 C19 C14 122.9(3) . . ? C20 C19 C18 118.1(3) . . ? C14 C19 C18 119.0(3) . . ? C21 C20 C19 121.5(4) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C20 C21 C22 120.4(4) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C23 C22 C21 121.0(4) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C18 120.6(3) . . ? C22 C23 H23A 119.7 . . ? C18 C23 H23A 119.7 . . ? O8 C24 O7 124.8(3) . . ? O8 C24 C17 120.0(3) . . ? O7 C24 C17 115.3(3) . . ? O9 C25 O10 125.5(3) . . ? O9 C25 C26 119.3(3) . . ? O10 C25 C26 115.2(3) . . ? C27 C26 C31 119.6(3) . . ? C27 C26 C25 118.5(4) . . ? C31 C26 C25 121.7(3) . . ? C26 C27 C28 121.3(4) . . ? C26 C27 H27A 119.4 . . ? C28 C27 H27A 119.4 . . ? C29 C28 C27 120.5(4) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C28 C29 C30 120.0(3) . . ? C28 C29 C36 119.2(3) . . ? C30 C29 C36 120.6(3) . . ? C35 C30 C31 119.0(4) . . ? C35 C30 C29 122.3(3) . . ? C31 C30 C29 118.7(3) . . ? C32 C31 C30 118.8(4) . . ? C32 C31 C26 121.8(4) . . ? C30 C31 C26 119.3(3) . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 121.0(4) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C35 C34 C33 121.6(5) . . ? C35 C34 H34A 119.2 . . ? C33 C34 H34A 119.2 . . ? C34 C35 C30 119.4(4) . . ? C34 C35 H35A 120.3 . . ? C30 C35 H35A 120.3 . . ? O12 C36 O11 121.0(3) . . ? O12 C36 C29 118.9(3) . . ? O11 C36 C29 119.9(3) . . ? O12 C36 Ce2 51.59(18) . 2 ? O11 C36 Ce2 69.89(19) . 2 ? C29 C36 Ce2 169.7(3) . 2 ? C39A N1A C37A 108.9(10) . . ? C39A N1A C40A 123.7(9) . . ? C37A N1A C40A 126.5(8) . . ? C38A N2A C39A 109.1(7) . . ? C38A N2A C41A 127.3(9) . . ? C39A N2A C41A 123.2(7) . . ? N1A C37A C38A 107.2(10) . . ? N1A C37A H37A 126.4 . . ? C38A C37A H37A 126.4 . . ? N2A C38A C37A 105.8(8) . . ? N2A C38A H38A 127.1 . . ? C37A C38A H38A 127.1 . . ? N1A C39A N2A 107.7(8) . . ? N1A C39A H39A 126.2 . . ? N2A C39A H39A 126.2 . . ? N2A C41A C42A 107.1(11) . . ? N2A C41A H41A 110.3 . . ? C42A C41A H41A 110.3 . . ? N2A C41A H41B 110.3 . . ? C42A C41A H41B 110.3 . . ? H41A C41A H41B 108.5 . . ? C44A C43A C42A 107.2(10) . . ? C44A C43A H43A 110.3 . . ? C42A C43A H43A 110.3 . . ? C44A C43A H43B 110.3 . . ? C42A C43A H43B 110.3 . . ? H43A C43A H43B 108.5 . . ? C41A C42A C43A 107.8(11) . . ? C41A C42A H42A 110.1 . . ? C43A C42A H42A 110.1 . . ? C41A C42A H42B 110.1 . . ? C43A C42A H42B 110.1 . . ? H42A C42A H42B 108.5 . . ? C45A C44A C43A 120.7(11) . . ? C45A C44A H44A 107.2 . . ? C43A C44A H44A 107.2 . . ? C45A C44A H44B 107.2 . . ? C43A C44A H44B 107.2 . . ? H44A C44A H44B 106.8 . . ? C46A C45A C44A 110.3(10) . . ? C46A C45A H45A 109.6 . . ? C44A C45A H45A 109.6 . . ? C46A C45A H45D 109.6 . . ? C44A C45A H45D 109.6 . . ? H45A C45A H45D 108.1 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C38B N2B C39B 109.0(8) . . ? C38B N2B C41B 127.0(11) . . ? C39B N2B C41B 123.9(9) . . ? C39B N1B C37B 108.1(13) . . ? C39B N1B C40B 123.2(12) . . ? C37B N1B C40B 128.6(10) . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N1B C37B C38B 107.3(13) . . ? N1B C37B H37B 126.3 . . ? C38B C37B H37B 126.3 . . ? N2B C38B C37B 106.0(10) . . ? N2B C38B H38B 127.0 . . ? C37B C38B H38B 127.0 . . ? N2B C41B C42B 111.3(15) . . ? N2B C41B C43B 130.8(14) . . ? C42B C41B C43B 49.3(7) . . ? N2B C41B H41C 109.4 . . ? C42B C41B H41C 109.4 . . ? C43B C41B H41C 119.6 . . ? N2B C41B H41D 109.4 . . ? C42B C41B H41D 109.4 . . ? C43B C41B H41D 60.3 . . ? H41C C41B H41D 108.0 . . ? C41B C42B C43B 81.8(11) . . ? C41B C42B H42C 115.0 . . ? C43B C42B H42C 115.0 . . ? C41B C42B H42D 115.0 . . ? C43B C42B H42D 115.0 . . ? H42C C42B H42D 112.0 . . ? N1B C39B N2B 108.3(11) . . ? N1B C39B H39B 125.9 . . ? N2B C39B H39B 125.9 . . ? C43B C44B C45B 145.7(17) . . ? C43B C44B H44C 100.4 . . ? C45B C44B H44C 100.4 . . ? C43B C44B H44D 100.4 . . ? C45B C44B H44D 100.4 . . ? H44C C44B H44D 104.3 . . ? C44B C43B C42B 121.2(13) . . ? C44B C43B C41B 127.2(14) . . ? C42B C43B C41B 48.9(6) . . ? C44B C43B H43C 107.0 . . ? C42B C43B H43C 107.0 . . ? C41B C43B H43C 58.7 . . ? C44B C43B H43D 107.0 . . ? C42B C43B H43D 107.0 . . ? C41B C43B H43D 125.8 . . ? H43C C43B H43D 106.8 . . ? C44B C45B C46B 107.5(10) . . ? C44B C45B H45B 110.2 . . ? C46B C45B H45B 110.2 . . ? C44B C45B H45C 110.2 . . ? C46B C45B H45C 110.2 . . ? H45B C45B H45C 108.5 . . ? C45B C46B H46G 109.5 . . ? C45B C46B H46D 109.5 . . ? H46G C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46G C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ce2 Cl1 Ce1 -24.10(7) . . . . ? O11 Ce2 Cl1 Ce1 85.7(2) 4_565 . . . ? O10 Ce2 Cl1 Ce1 130.26(8) 3 . . . ? O8 Ce2 Cl1 Ce1 52.20(7) 4_565 . . . ? O9 Ce2 Cl1 Ce1 -88.77(8) . . . . ? O12 Ce2 Cl1 Ce1 -139.95(9) 2_545 . . . ? O11 Ce2 Cl1 Ce1 -165.52(6) 2_545 . . . ? C36 Ce2 Cl1 Ce1 -150.91(8) 2_545 . . . ? O7 Ce1 Cl1 Ce2 -40.19(8) 4_565 . . . ? O1 Ce1 Cl1 Ce2 -49.11(19) . . . . ? O5 Ce1 Cl1 Ce2 114.44(9) 4_566 . . . ? O6 Ce1 Cl1 Ce2 -115.80(8) 2_644 . . . ? O3 Ce1 Cl1 Ce2 43.38(8) . . . . ? O2 Ce1 Cl1 Ce2 167.36(8) 3_655 . . . ? O7 Ce1 O1 C1 -153.7(5) 4_565 . . . ? O5 Ce1 O1 C1 48.8(4) 4_566 . . . ? O6 Ce1 O1 C1 -76.8(4) 2_644 . . . ? O3 Ce1 O1 C1 125.2(4) . . . . ? O2 Ce1 O1 C1 -8.8(5) 3_655 . . . ? Cl1 Ce1 O1 C1 -144.9(4) . . . . ? O7 Ce1 O3 C13 28.6(4) 4_565 . . . ? O1 Ce1 O3 C13 108.8(4) . . . . ? O5 Ce1 O3 C13 -175.5(4) 4_566 . . . ? O6 Ce1 O3 C13 24.7(6) 2_644 . . . ? O2 Ce1 O3 C13 -114.2(4) 3_655 . . . ? Cl1 Ce1 O3 C13 -47.8(4) . . . . ? O11 Ce2 O4 C13 156.9(4) 4_565 . . . ? O10 Ce2 O4 C13 -114.5(4) 3 . . . ? O8 Ce2 O4 C13 -125.8(4) 4_565 . . . ? O9 Ce2 O4 C13 87.6(4) . . . . ? O12 Ce2 O4 C13 24.4(4) 2_545 . . . ? Cl1 Ce2 O4 C13 -41.1(4) . . . . ? O11 Ce2 O4 C13 72.7(4) 2_545 . . . ? C36 Ce2 O4 C13 44.6(4) 2_545 . . . ? O4 Ce2 O9 C25 128.8(4) . . . . ? O11 Ce2 O9 C25 20.3(4) 4_565 . . . ? O10 Ce2 O9 C25 -38.1(4) 3 . . . ? O8 Ce2 O9 C25 80.1(4) 4_565 . . . ? O12 Ce2 O9 C25 -111.5(4) 2_545 . . . ? Cl1 Ce2 O9 C25 -161.5(4) . . . . ? O11 Ce2 O9 C25 -61.5(4) 2_545 . . . ? C36 Ce2 O9 C25 -87.8(4) 2_545 . . . ? Ce1 O1 C1 O2 -6.2(7) . . . . ? Ce1 O1 C1 C2 171.6(3) . . . . ? Ce1 O2 C1 O1 23.9(8) 3_655 . . . ? Ce1 O2 C1 C2 -153.9(3) 3_655 . . . ? O1 C1 C2 C3 -42.0(5) . . . . ? O2 C1 C2 C3 136.0(4) . . . . ? O1 C1 C2 C7 139.5(4) . . . . ? O2 C1 C2 C7 -42.5(5) . . . . ? C7 C2 C3 C4 0.6(6) . . . . ? C1 C2 C3 C4 -177.9(4) . . . . ? C2 C3 C4 C5 0.7(6) . . . . ? C3 C4 C5 C6 -2.7(6) . . . . ? C3 C4 C5 C12 174.6(4) . . . . ? C4 C5 C6 C11 -174.3(4) . . . . ? C12 C5 C6 C11 8.5(6) . . . . ? C4 C5 C6 C7 3.3(5) . . . . ? C12 C5 C6 C7 -173.9(3) . . . . ? C11 C6 C7 C8 -2.5(5) . . . . ? C5 C6 C7 C8 179.8(3) . . . . ? C11 C6 C7 C2 175.7(3) . . . . ? C5 C6 C7 C2 -2.0(5) . . . . ? C3 C2 C7 C8 178.3(4) . . . . ? C1 C2 C7 C8 -3.3(6) . . . . ? C3 C2 C7 C6 0.1(5) . . . . ? C1 C2 C7 C6 178.5(3) . . . . ? C6 C7 C8 C9 1.9(6) . . . . ? C2 C7 C8 C9 -176.3(4) . . . . ? C7 C8 C9 C10 -0.1(7) . . . . ? C8 C9 C10 C11 -1.1(7) . . . . ? C9 C10 C11 C6 0.4(6) . . . . ? C7 C6 C11 C10 1.4(6) . . . . ? C5 C6 C11 C10 179.0(4) . . . . ? Ce1 O5 C12 O6 30.8(16) 4_565 . . . ? Ce1 O5 C12 C5 -147.0(12) 4_565 . . . ? Ce1 O6 C12 O5 1.7(6) 2_654 . . . ? Ce1 O6 C12 C5 179.4(2) 2_654 . . . ? C4 C5 C12 O5 35.9(5) . . . . ? C6 C5 C12 O5 -146.8(4) . . . . ? C4 C5 C12 O6 -142.0(4) . . . . ? C6 C5 C12 O6 35.3(6) . . . . ? Ce2 O4 C13 O3 66.1(6) . . . . ? Ce2 O4 C13 C14 -110.8(4) . . . . ? Ce1 O3 C13 O4 4.0(7) . . . . ? Ce1 O3 C13 C14 -179.1(3) . . . . ? O4 C13 C14 C15 144.0(4) . . . . ? O3 C13 C14 C15 -33.2(5) . . . . ? O4 C13 C14 C19 -33.4(6) . . . . ? O3 C13 C14 C19 149.5(4) . . . . ? C19 C14 C15 C16 0.9(6) . . . . ? C13 C14 C15 C16 -176.5(4) . . . . ? C14 C15 C16 C17 1.2(7) . . . . ? C15 C16 C17 C18 -1.4(6) . . . . ? C15 C16 C17 C24 179.8(4) . . . . ? C16 C17 C18 C23 -178.2(3) . . . . ? C24 C17 C18 C23 0.4(5) . . . . ? C16 C17 C18 C19 -0.4(5) . . . . ? C24 C17 C18 C19 178.3(3) . . . . ? C15 C14 C19 C20 175.0(4) . . . . ? C13 C14 C19 C20 -7.7(6) . . . . ? C15 C14 C19 C18 -2.6(5) . . . . ? C13 C14 C19 C18 174.6(3) . . . . ? C23 C18 C19 C20 2.5(5) . . . . ? C17 C18 C19 C20 -175.4(3) . . . . ? C23 C18 C19 C14 -179.7(3) . . . . ? C17 C18 C19 C14 2.4(5) . . . . ? C14 C19 C20 C21 -178.7(4) . . . . ? C18 C19 C20 C21 -1.1(5) . . . . ? C19 C20 C21 C22 -0.8(6) . . . . ? C20 C21 C22 C23 1.2(7) . . . . ? C21 C22 C23 C18 0.3(6) . . . . ? C17 C18 C23 C22 175.6(4) . . . . ? C19 C18 C23 C22 -2.2(5) . . . . ? Ce2 O8 C24 O7 -29.3(6) 4_566 . . . ? Ce2 O8 C24 C17 149.1(3) 4_566 . . . ? Ce1 O7 C24 O8 9.3(12) 4_566 . . . ? Ce1 O7 C24 C17 -169.2(8) 4_566 . . . ? C16 C17 C24 O8 -145.5(4) . . . . ? C18 C17 C24 O8 35.8(5) . . . . ? C16 C17 C24 O7 33.0(5) . . . . ? C18 C17 C24 O7 -145.7(3) . . . . ? Ce2 O9 C25 O10 25.4(7) . . . . ? Ce2 O9 C25 C26 -155.6(3) . . . . ? Ce2 O10 C25 O9 3.7(7) 3 . . . ? Ce2 O10 C25 C26 -175.3(3) 3 . . . ? O9 C25 C26 C27 -50.2(5) . . . . ? O10 C25 C26 C27 128.9(4) . . . . ? O9 C25 C26 C31 135.0(4) . . . . ? O10 C25 C26 C31 -46.0(5) . . . . ? C31 C26 C27 C28 6.6(6) . . . . ? C25 C26 C27 C28 -168.3(4) . . . . ? C26 C27 C28 C29 -0.1(6) . . . . ? C27 C28 C29 C30 -7.0(6) . . . . ? C27 C28 C29 C36 168.1(4) . . . . ? C28 C29 C30 C35 -170.9(4) . . . . ? C36 C29 C30 C35 14.0(5) . . . . ? C28 C29 C30 C31 7.4(5) . . . . ? C36 C29 C30 C31 -167.7(3) . . . . ? C35 C30 C31 C32 0.0(5) . . . . ? C29 C30 C31 C32 -178.4(3) . . . . ? C35 C30 C31 C26 177.4(3) . . . . ? C29 C30 C31 C26 -0.9(5) . . . . ? C27 C26 C31 C32 171.3(4) . . . . ? C25 C26 C31 C32 -13.9(5) . . . . ? C27 C26 C31 C30 -6.0(5) . . . . ? C25 C26 C31 C30 168.8(3) . . . . ? C30 C31 C32 C33 1.4(6) . . . . ? C26 C31 C32 C33 -175.9(4) . . . . ? C31 C32 C33 C34 -1.2(7) . . . . ? C32 C33 C34 C35 -0.5(8) . . . . ? C33 C34 C35 C30 2.0(7) . . . . ? C31 C30 C35 C34 -1.7(6) . . . . ? C29 C30 C35 C34 176.6(4) . . . . ? Ce2 O12 C36 O11 8.8(5) 2 . . . ? Ce2 O12 C36 C29 -175.2(3) 2 . . . ? Ce2 O11 C36 O12 -123.4(6) 4_566 . . . ? Ce2 O11 C36 O12 -7.4(4) 2 . . . ? Ce2 O11 C36 C29 60.7(9) 4_566 . . . ? Ce2 O11 C36 C29 176.8(3) 2 . . . ? Ce2 O11 C36 Ce2 -116.0(7) 4_566 . . 2 ? C28 C29 C36 O12 -134.6(4) . . . . ? C30 C29 C36 O12 40.6(5) . . . . ? C28 C29 C36 O11 41.4(5) . . . . ? C30 C29 C36 O11 -143.5(4) . . . . ? C28 C29 C36 Ce2 -156.0(13) . . . 2 ? C30 C29 C36 Ce2 19.2(17) . . . 2 ? C39A N1A C37A C38A 7(2) . . . . ? C40A N1A C37A C38A 176.6(14) . . . . ? C39A N2A C38A C37A -7(2) . . . . ? C41A N2A C38A C37A 179.8(19) . . . . ? N1A C37A C38A N2A 0.4(18) . . . . ? C37A N1A C39A N2A -11(3) . . . . ? C40A N1A C39A N2A 178.5(18) . . . . ? C38A N2A C39A N1A 12(3) . . . . ? C41A N2A C39A N1A -175.0(18) . . . . ? C38A N2A C41A C42A -18(3) . . . . ? C39A N2A C41A C42A 170(2) . . . . ? N2A C41A C42A C43A -76.5(16) . . . . ? C44A C43A C42A C41A -162.1(11) . . . . ? C42A C43A C44A C45A -81.8(16) . . . . ? C43A C44A C45A C46A -122.6(16) . . . . ? C39B N1B C37B C38B -8(3) . . . . ? C40B N1B C37B C38B 175(2) . . . . ? C39B N2B C38B C37B 5(3) . . . . ? C41B N2B C38B C37B -178(2) . . . . ? N1B C37B C38B N2B 2(2) . . . . ? C38B N2B C41B C42B -108(3) . . . . ? C39B N2B C41B C42B 69(4) . . . . ? C38B N2B C41B C43B -54(3) . . . . ? C39B N2B C41B C43B 122(3) . . . . ? N2B C41B C42B C43B 126.2(14) . . . . ? C37B N1B C39B N2B 11(4) . . . . ? C40B N1B C39B N2B -172(2) . . . . ? C38B N2B C39B N1B -10(4) . . . . ? C41B N2B C39B N1B 173(2) . . . . ? C45B C44B C43B C42B -80(3) . . . . ? C45B C44B C43B C41B -140(3) . . . . ? C41B C42B C43B C44B -114.1(19) . . . . ? N2B C41B C43B C44B 18(3) . . . . ? C42B C41B C43B C44B 101.6(18) . . . . ? N2B C41B C43B C42B -83.6(18) . . . . ? C43B C44B C45B C46B -110(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.133 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.090 #===END data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 876523' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Pr2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl N2 O12 Pr2' _chemical_formula_weight 1127.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.9610(2) _cell_length_b 14.81098(16) _cell_length_c 16.1045(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.7691(11) _cell_angle_gamma 90.00 _cell_volume 4262.41(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12439 _cell_measurement_theta_min 2.4908 _cell_measurement_theta_max 28.8296 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 2.389 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76018 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19947 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8858 _reflns_number_gt 7167 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0399P)^2^+0.1609P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8858 _refine_ls_number_parameters 607 _refine_ls_number_restraints 368 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.092 _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 Pr1 Pr 0.377902(9) 0.025015(12) -0.005443(10) 0.01385(6) Uani 1 1 d . . . Pr2 Pr 0.115055(9) 0.012901(12) -0.001096(11) 0.01447(6) Uani 1 1 d . . . Cl1 Cl 0.25169(4) -0.08769(6) 0.02308(6) 0.0310(2) Uani 1 1 d . . . O1 O 0.44857(14) 0.13084(17) -0.07793(18) 0.0383(7) Uani 1 1 d . . . O2 O 0.57177(14) 0.11176(17) -0.06045(18) 0.0390(7) Uani 1 1 d . . . O3 O 0.31584(14) 0.13498(18) 0.07448(18) 0.0426(7) Uani 1 1 d . . . O5 O 0.47458(15) 0.43213(19) -0.39967(18) 0.0468(8) Uani 1 1 d . . . O4 O 0.19477(13) 0.13819(16) 0.02944(17) 0.0331(6) Uani 1 1 d . . . O6 O 0.59832(16) 0.4324(2) -0.37776(17) 0.0436(8) Uani 1 1 d . . . O7 O 0.28393(13) 0.43167(18) 0.38878(16) 0.0343(7) Uani 1 1 d . . . O8 O 0.16061(13) 0.44961(17) 0.36610(14) 0.0281(6) Uani 1 1 d . . . O9 O 0.06242(14) 0.09859(18) 0.10964(17) 0.0385(7) Uani 1 1 d . . . O10 O -0.06251(14) 0.10510(18) 0.08921(17) 0.0378(7) Uani 1 1 d . . . O11 O 0.00583(14) 0.41581(17) 0.43343(16) 0.0325(6) Uani 1 1 d . . . O12 O -0.11191(14) 0.4096(2) 0.38053(18) 0.0456(8) Uani 1 1 d . . . C1 C 0.5135(2) 0.1500(2) -0.0921(2) 0.0265(8) Uani 1 1 d . . . C2 C 0.52137(19) 0.2227(2) -0.1567(2) 0.0245(8) Uani 1 1 d . . . C3 C 0.4715(2) 0.2220(3) -0.2264(2) 0.0316(9) Uani 1 1 d . . . H3A H 0.4338 0.1787 -0.2318 0.038 Uiso 1 1 calc R . . C4 C 0.4763(2) 0.2857(3) -0.2901(2) 0.0310(9) Uani 1 1 d . . . H4A H 0.4416 0.2839 -0.3370 0.037 Uiso 1 1 calc R . . C5 C 0.53073(18) 0.3502(2) -0.2848(2) 0.0239(8) Uani 1 1 d . . . C6 C 0.58239(18) 0.3560(2) -0.2115(2) 0.0212(8) Uani 1 1 d . . . C7 C 0.57826(18) 0.2902(2) -0.1469(2) 0.0225(8) Uani 1 1 d . . . C8 C 0.6303(2) 0.2962(3) -0.0746(2) 0.0318(9) Uani 1 1 d . . . H8A H 0.6295 0.2531 -0.0327 0.038 Uiso 1 1 calc R . . C9 C 0.6813(2) 0.3642(3) -0.0659(3) 0.0404(10) Uani 1 1 d . . . H9A H 0.7149 0.3671 -0.0181 0.048 Uiso 1 1 calc R . . C10 C 0.6838(2) 0.4300(3) -0.1281(3) 0.0398(10) Uani 1 1 d . . . H10A H 0.7183 0.4769 -0.1208 0.048 Uiso 1 1 calc R . . C11 C 0.6363(2) 0.4260(3) -0.1987(2) 0.0314(9) Uani 1 1 d . . . H11A H 0.6391 0.4698 -0.2397 0.038 Uiso 1 1 calc R . . C12 C 0.5345(2) 0.4099(2) -0.3586(2) 0.0295(9) Uani 1 1 d . . . C13 C 0.2503(2) 0.1659(2) 0.0756(2) 0.0270(8) Uani 1 1 d . . . C14 C 0.24016(19) 0.2374(2) 0.1399(2) 0.0238(8) Uani 1 1 d . . . C15 C 0.2837(2) 0.2313(3) 0.2142(3) 0.0358(10) Uani 1 1 d . . . H15A H 0.3194 0.1858 0.2215 0.043 Uiso 1 1 calc R . . C16 C 0.2763(2) 0.2908(3) 0.2792(2) 0.0345(10) Uani 1 1 d . . . H16A H 0.3076 0.2849 0.3285 0.041 Uiso 1 1 calc R . . C17 C 0.22398(18) 0.3582(2) 0.2722(2) 0.0214(8) Uani 1 1 d . . . C18 C 0.17722(17) 0.3687(2) 0.1956(2) 0.0189(7) Uani 1 1 d . . . C19 C 0.18639(18) 0.3084(2) 0.1277(2) 0.0211(7) Uani 1 1 d . . . C20 C 0.1432(2) 0.3237(3) 0.0509(2) 0.0309(9) Uani 1 1 d . . . H20A H 0.1491 0.2860 0.0059 0.037 Uiso 1 1 calc R . . C21 C 0.0927(2) 0.3930(3) 0.0415(2) 0.0385(10) Uani 1 1 d . . . H21A H 0.0650 0.4021 -0.0098 0.046 Uiso 1 1 calc R . . C22 C 0.0824(2) 0.4504(3) 0.1082(3) 0.0371(10) Uani 1 1 d . . . H22A H 0.0474 0.4967 0.1015 0.044 Uiso 1 1 calc R . . C23 C 0.12332(19) 0.4386(2) 0.1829(2) 0.0252(8) Uani 1 1 d . . . H23A H 0.1158 0.4772 0.2268 0.030 Uiso 1 1 calc R . . C24 C 0.22213(18) 0.4184(2) 0.3474(2) 0.0217(7) Uani 1 1 d . . . C25 C 0.0006(2) 0.1322(2) 0.1214(2) 0.0299(9) Uani 1 1 d . . . C26 C -0.00171(19) 0.2106(2) 0.1802(2) 0.0253(8) Uani 1 1 d . . . C27 C 0.0370(2) 0.2039(3) 0.2582(3) 0.0356(10) Uani 1 1 d . . . H27A H 0.0705 0.1567 0.2698 0.043 Uiso 1 1 calc R . . C28 C 0.0265(2) 0.2677(3) 0.3202(2) 0.0353(10) Uani 1 1 d . . . H28A H 0.0536 0.2626 0.3723 0.042 Uiso 1 1 calc R . . C29 C -0.02306(19) 0.3371(3) 0.3051(2) 0.0274(9) Uani 1 1 d . . . C30 C -0.0584(2) 0.3517(2) 0.2227(2) 0.0265(8) Uani 1 1 d . . . C31 C -0.04777(19) 0.2872(2) 0.1598(2) 0.0260(8) Uani 1 1 d . . . C32 C -0.0814(2) 0.3032(3) 0.0771(3) 0.0384(10) Uani 1 1 d . . . H32A H -0.0756 0.2612 0.0352 0.046 Uiso 1 1 calc R . . C33 C -0.1214(3) 0.3787(3) 0.0594(3) 0.0545(13) Uani 1 1 d . . . H33A H -0.1428 0.3887 0.0052 0.065 Uiso 1 1 calc R . . C34 C -0.1311(3) 0.4424(3) 0.1211(3) 0.0574(13) Uani 1 1 d . . . H34A H -0.1587 0.4944 0.1071 0.069 Uiso 1 1 calc R . . C35 C -0.1014(2) 0.4304(3) 0.2013(3) 0.0401(10) Uani 1 1 d . . . H35A H -0.1090 0.4733 0.2418 0.048 Uiso 1 1 calc R . . C36 C -0.0437(2) 0.3922(2) 0.3762(2) 0.0292(9) Uani 1 1 d . . . N1A N 0.2369(6) -0.2681(7) 0.2801(5) 0.0569(15) Uani 0.591(5) 1 d PDU A 1 N2A N 0.3058(7) -0.1489(8) 0.2687(8) 0.0675(15) Uani 0.591(5) 1 d PDU A 1 C37A C 0.2885(6) -0.2648(7) 0.3476(6) 0.0564(17) Uani 0.591(5) 1 d PDU A 1 H37A H 0.2935 -0.3058 0.3915 0.068 Uiso 0.591(5) 1 calc PR A 1 C38A C 0.3331(7) -0.1879(8) 0.3389(7) 0.0704(18) Uani 0.591(5) 1 d PDU A 1 H38A H 0.3735 -0.1686 0.3752 0.085 Uiso 0.591(5) 1 calc PR A 1 C39A C 0.2539(9) -0.2048(9) 0.2276(9) 0.0535(16) Uani 0.591(5) 1 d PDU A 1 H39A H 0.2340 -0.1992 0.1723 0.064 Uiso 0.591(5) 1 calc PR A 1 C40A C 0.1820(6) -0.3371(7) 0.2607(7) 0.079(3) Uani 0.591(5) 1 d PDU A 1 H40A H 0.1371 -0.3106 0.2339 0.118 Uiso 0.591(5) 1 calc PR A 1 H40B H 0.1711 -0.3665 0.3113 0.118 Uiso 0.591(5) 1 calc PR A 1 H40C H 0.2011 -0.3806 0.2241 0.118 Uiso 0.591(5) 1 calc PR A 1 C41A C 0.3323(6) -0.0617(7) 0.2341(7) 0.088(2) Uani 0.591(5) 1 d PDU A 1 H41A H 0.2893 -0.0237 0.2177 0.106 Uiso 0.591(5) 1 calc PR A 1 H41B H 0.3569 -0.0744 0.1844 0.106 Uiso 0.591(5) 1 calc PR A 1 C43A C 0.3260(6) 0.0285(9) 0.3542(8) 0.122(2) Uani 0.591(5) 1 d PDU A 1 H43A H 0.2835 0.0565 0.3223 0.147 Uiso 0.591(5) 1 calc PR A 1 H43B H 0.3089 -0.0166 0.3916 0.147 Uiso 0.591(5) 1 calc PR A 1 C42A C 0.3862(6) -0.0106(8) 0.2962(7) 0.110(2) Uani 0.591(5) 1 d PDU A 1 H42A H 0.4123 0.0371 0.2697 0.131 Uiso 0.591(5) 1 calc PR A 1 H42B H 0.4221 -0.0504 0.3266 0.131 Uiso 0.591(5) 1 calc PR A 1 C44A C 0.3802(9) 0.0990(8) 0.4003(7) 0.146(3) Uani 0.591(5) 1 d PDU A 1 H44A H 0.4150 0.1184 0.3617 0.175 Uiso 0.591(5) 1 calc PR A 1 H44B H 0.3508 0.1514 0.4126 0.175 Uiso 0.591(5) 1 calc PR A 1 C45A C 0.4244(8) 0.0711(9) 0.4788(8) 0.160(3) Uani 0.591(5) 1 d PDU A 1 H45A H 0.4771 0.0709 0.4699 0.192 Uiso 0.591(5) 1 calc PR A 1 H45D H 0.4107 0.0098 0.4921 0.192 Uiso 0.591(5) 1 calc PR A 1 C46A C 0.4135(10) 0.1320(12) 0.5538(8) 0.183(5) Uani 0.591(5) 1 d PDU A 1 H46A H 0.4459 0.1122 0.6014 0.274 Uiso 0.591(5) 1 calc PR A 1 H46B H 0.3624 0.1286 0.5662 0.274 Uiso 0.591(5) 1 calc PR A 1 H46C H 0.4254 0.1932 0.5407 0.274 Uiso 0.591(5) 1 calc PR A 1 N2B N 0.3121(11) -0.1667(12) 0.2734(12) 0.0675(15) Uani 0.409(5) 1 d PDU A 2 N1B N 0.2257(10) -0.2710(10) 0.2539(8) 0.0569(15) Uani 0.409(5) 1 d PDU A 2 C40B C 0.1689(8) -0.3212(11) 0.2084(9) 0.079(3) Uani 0.409(5) 1 d PDU A 2 H40D H 0.1630 -0.3006 0.1516 0.118 Uiso 0.409(5) 1 calc PR A 2 H40E H 0.1227 -0.3133 0.2328 0.118 Uiso 0.409(5) 1 calc PR A 2 H40F H 0.1823 -0.3840 0.2097 0.118 Uiso 0.409(5) 1 calc PR A 2 C37B C 0.2615(9) -0.2801(10) 0.3313(9) 0.0564(17) Uani 0.409(5) 1 d PDU A 2 H37B H 0.2507 -0.3233 0.3703 0.068 Uiso 0.409(5) 1 calc PR A 2 C38B C 0.3172(10) -0.2144(11) 0.3436(10) 0.0704(18) Uani 0.409(5) 1 d PDU A 2 H38B H 0.3508 -0.2058 0.3908 0.085 Uiso 0.409(5) 1 calc PR A 2 C41B C 0.3594(8) -0.0881(8) 0.2491(12) 0.088(2) Uani 0.409(5) 1 d PDU A 2 H41C H 0.3596 -0.0883 0.1889 0.106 Uiso 0.409(5) 1 calc PR A 2 H41D H 0.4105 -0.0978 0.2732 0.106 Uiso 0.409(5) 1 calc PR A 2 C42B C 0.3340(11) 0.0054(10) 0.2760(10) 0.110(2) Uani 0.409(5) 1 d PDU A 2 H42C H 0.2802 0.0064 0.2775 0.131 Uiso 0.409(5) 1 calc PR A 2 H42D H 0.3474 0.0510 0.2369 0.131 Uiso 0.409(5) 1 calc PR A 2 C39B C 0.2484(13) -0.1935(14) 0.2257(13) 0.0535(16) Uani 0.409(5) 1 d PDU A 2 H39B H 0.2250 -0.1619 0.1805 0.064 Uiso 0.409(5) 1 calc PR A 2 C44B C 0.3329(9) 0.0879(13) 0.4215(11) 0.146(3) Uani 0.409(5) 1 d PDU A 2 H44C H 0.3120 0.1347 0.3841 0.175 Uiso 0.409(5) 1 calc PR A 2 H44D H 0.2908 0.0527 0.4366 0.175 Uiso 0.409(5) 1 calc PR A 2 C43B C 0.3753(10) 0.0253(13) 0.3673(11) 0.122(2) Uani 0.409(5) 1 d PDU A 2 H43C H 0.3839 -0.0317 0.3963 0.147 Uiso 0.409(5) 1 calc PR A 2 H43D H 0.4238 0.0518 0.3612 0.147 Uiso 0.409(5) 1 calc PR A 2 C45B C 0.3618(10) 0.1353(15) 0.4985(12) 0.160(3) Uani 0.409(5) 1 d PDU A 2 H45B H 0.3426 0.1054 0.5455 0.192 Uiso 0.409(5) 1 calc PR A 2 H45C H 0.3422 0.1963 0.4962 0.192 Uiso 0.409(5) 1 calc PR A 2 C46B C 0.4478(10) 0.1404(18) 0.5153(14) 0.183(5) Uani 0.409(5) 1 d PDU A 2 H46G H 0.4614 0.1894 0.5528 0.274 Uiso 0.409(5) 1 calc PR A 2 H46D H 0.4690 0.1502 0.4636 0.274 Uiso 0.409(5) 1 calc PR A 2 H46E H 0.4665 0.0848 0.5398 0.274 Uiso 0.409(5) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.01492(10) 0.01397(10) 0.01303(10) 0.00011(7) 0.00322(7) 0.00087(6) Pr2 0.01537(10) 0.01435(10) 0.01419(10) -0.00034(7) 0.00387(7) -0.00138(7) Cl1 0.0195(4) 0.0267(5) 0.0481(6) 0.0137(4) 0.0098(4) 0.0028(3) O1 0.0266(15) 0.0394(16) 0.0501(19) 0.0233(14) 0.0105(13) -0.0037(12) O2 0.0274(15) 0.0321(15) 0.057(2) 0.0229(14) 0.0003(13) 0.0027(12) O3 0.0303(15) 0.0431(17) 0.055(2) -0.0308(15) 0.0048(13) 0.0083(13) O5 0.0440(18) 0.0492(19) 0.0429(18) 0.0201(15) -0.0166(14) -0.0022(14) O4 0.0277(14) 0.0297(15) 0.0430(17) -0.0187(13) 0.0093(12) -0.0109(11) O6 0.0430(18) 0.0533(19) 0.0353(17) 0.0234(15) 0.0075(13) -0.0108(14) O7 0.0220(13) 0.0512(18) 0.0292(15) -0.0198(13) -0.0007(11) -0.0010(12) O8 0.0238(13) 0.0407(15) 0.0205(14) -0.0056(12) 0.0062(10) 0.0069(11) O9 0.0311(15) 0.0458(17) 0.0408(18) -0.0255(14) 0.0146(13) -0.0043(13) O10 0.0276(15) 0.0391(16) 0.0488(19) -0.0274(14) 0.0136(13) -0.0119(12) O11 0.0316(15) 0.0376(16) 0.0291(16) -0.0150(13) 0.0071(12) -0.0115(12) O12 0.0233(15) 0.065(2) 0.0505(19) -0.0366(16) 0.0151(13) -0.0080(13) C1 0.026(2) 0.0212(19) 0.031(2) 0.0097(16) 0.0008(16) -0.0009(15) C2 0.0219(18) 0.0217(18) 0.031(2) 0.0128(16) 0.0054(15) -0.0003(14) C3 0.024(2) 0.034(2) 0.036(2) 0.0126(19) -0.0031(17) -0.0104(16) C4 0.0236(19) 0.039(2) 0.029(2) 0.0125(18) -0.0064(16) -0.0042(16) C5 0.0191(17) 0.0264(19) 0.026(2) 0.0083(16) 0.0017(15) 0.0003(14) C6 0.0177(17) 0.0216(18) 0.025(2) 0.0066(15) 0.0041(14) 0.0002(13) C7 0.0186(17) 0.0270(19) 0.022(2) 0.0056(15) 0.0040(14) -0.0005(14) C8 0.033(2) 0.039(2) 0.022(2) 0.0091(17) -0.0015(16) -0.0024(17) C9 0.039(2) 0.052(3) 0.029(2) 0.002(2) -0.0035(18) -0.014(2) C10 0.040(2) 0.044(3) 0.036(2) -0.003(2) 0.0038(19) -0.019(2) C11 0.035(2) 0.030(2) 0.031(2) 0.0081(17) 0.0071(17) -0.0082(17) C12 0.037(2) 0.027(2) 0.023(2) 0.0088(17) 0.0003(17) -0.0031(17) C13 0.028(2) 0.0217(19) 0.033(2) -0.0101(16) 0.0107(17) -0.0044(15) C14 0.0220(18) 0.0245(19) 0.026(2) -0.0091(16) 0.0084(15) -0.0002(14) C15 0.029(2) 0.035(2) 0.042(3) -0.0158(19) -0.0020(18) 0.0154(17) C16 0.028(2) 0.046(2) 0.028(2) -0.0139(19) -0.0055(17) 0.0124(18) C17 0.0193(17) 0.0238(18) 0.0213(19) -0.0079(15) 0.0028(14) -0.0004(14) C18 0.0171(16) 0.0185(17) 0.0218(19) -0.0030(14) 0.0059(14) -0.0041(13) C19 0.0189(17) 0.0256(19) 0.0196(19) -0.0057(15) 0.0055(14) -0.0063(14) C20 0.038(2) 0.034(2) 0.020(2) -0.0083(17) 0.0000(16) -0.0018(17) C21 0.043(2) 0.048(3) 0.022(2) -0.0014(19) -0.0058(18) 0.006(2) C22 0.039(2) 0.031(2) 0.040(3) 0.004(2) 0.0027(19) 0.0131(18) C23 0.0269(19) 0.0226(19) 0.026(2) -0.0034(16) 0.0051(15) 0.0042(15) C24 0.0240(18) 0.0228(18) 0.0186(19) -0.0018(15) 0.0032(14) -0.0007(14) C25 0.035(2) 0.029(2) 0.028(2) -0.0122(17) 0.0116(17) -0.0094(17) C26 0.0241(19) 0.027(2) 0.026(2) -0.0140(17) 0.0095(15) -0.0067(15) C27 0.031(2) 0.037(2) 0.038(3) -0.0138(19) 0.0005(18) 0.0088(17) C28 0.034(2) 0.047(3) 0.024(2) -0.0150(19) -0.0031(17) 0.0033(18) C29 0.0232(19) 0.033(2) 0.027(2) -0.0139(17) 0.0088(16) -0.0062(16) C30 0.0255(19) 0.026(2) 0.030(2) -0.0069(17) 0.0104(16) -0.0071(15) C31 0.0250(19) 0.029(2) 0.025(2) -0.0058(16) 0.0072(15) -0.0101(15) C32 0.042(3) 0.045(3) 0.028(2) -0.004(2) 0.0050(19) -0.010(2) C33 0.057(3) 0.068(3) 0.036(3) 0.010(3) -0.007(2) -0.007(3) C34 0.045(3) 0.055(3) 0.072(4) 0.017(3) 0.007(3) 0.009(2) C35 0.044(3) 0.032(2) 0.046(3) -0.001(2) 0.015(2) 0.0001(19) C36 0.031(2) 0.028(2) 0.030(2) -0.0154(17) 0.0132(17) -0.0105(16) N1A 0.070(3) 0.047(2) 0.057(4) 0.007(3) 0.025(3) 0.021(2) N2A 0.090(3) 0.064(3) 0.051(2) 0.002(2) 0.017(2) 0.011(3) C37A 0.077(4) 0.043(3) 0.049(3) 0.010(3) 0.006(3) 0.011(3) C38A 0.092(4) 0.064(4) 0.055(3) 0.008(3) 0.007(3) 0.015(3) C39A 0.069(3) 0.047(3) 0.046(3) 0.009(2) 0.012(2) 0.008(3) C40A 0.078(5) 0.048(5) 0.121(8) 0.000(6) 0.064(6) 0.005(4) C41A 0.113(4) 0.073(4) 0.085(4) 0.003(3) 0.036(4) -0.015(4) C43A 0.158(5) 0.097(4) 0.121(4) 0.000(4) 0.059(4) -0.006(4) C42A 0.138(5) 0.091(4) 0.108(4) -0.003(4) 0.051(4) -0.003(4) C44A 0.178(5) 0.116(5) 0.149(5) 0.024(4) 0.045(5) -0.019(5) C45A 0.195(6) 0.123(6) 0.165(6) 0.022(5) 0.039(6) -0.023(5) C46A 0.232(10) 0.143(8) 0.184(9) -0.003(9) 0.074(8) -0.021(9) N2B 0.090(3) 0.064(3) 0.051(2) 0.002(2) 0.017(2) 0.011(3) N1B 0.070(3) 0.047(2) 0.057(4) 0.007(3) 0.025(3) 0.021(2) C40B 0.078(5) 0.048(5) 0.121(8) 0.000(6) 0.064(6) 0.005(4) C37B 0.077(4) 0.043(3) 0.049(3) 0.010(3) 0.006(3) 0.011(3) C38B 0.092(4) 0.064(4) 0.055(3) 0.008(3) 0.007(3) 0.015(3) C41B 0.113(4) 0.073(4) 0.085(4) 0.003(3) 0.036(4) -0.015(4) C42B 0.138(5) 0.091(4) 0.108(4) -0.003(4) 0.051(4) -0.003(4) C39B 0.069(3) 0.047(3) 0.046(3) 0.009(2) 0.012(2) 0.008(3) C44B 0.178(5) 0.116(5) 0.149(5) 0.024(4) 0.045(5) -0.019(5) C43B 0.158(5) 0.097(4) 0.121(4) 0.000(4) 0.059(4) -0.006(4) C45B 0.195(6) 0.123(6) 0.165(6) 0.022(5) 0.039(6) -0.023(5) C46B 0.232(10) 0.143(8) 0.184(9) -0.003(9) 0.074(8) -0.021(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O7 2.363(2) 4_565 ? Pr1 O5 2.393(3) 4_566 ? Pr1 O1 2.393(2) . ? Pr1 O6 2.401(3) 2_644 ? Pr1 O3 2.417(2) . ? Pr1 O2 2.419(2) 3_655 ? Pr1 Cl1 2.8889(8) . ? Pr2 O4 2.365(2) . ? Pr2 O11 2.379(2) 4_565 ? Pr2 O10 2.385(2) 3 ? Pr2 O8 2.430(2) 4_565 ? Pr2 O9 2.454(2) . ? Pr2 O12 2.477(3) 2_545 ? Pr2 Cl1 2.8639(8) . ? Pr2 O11 2.906(2) 2_545 ? Pr2 C36 3.066(3) 2_545 ? O1 C1 1.244(4) . ? O2 C1 1.253(4) . ? O2 Pr1 2.419(2) 3_655 ? O3 C13 1.264(4) . ? O5 C12 1.249(4) . ? O5 Pr1 2.393(3) 4_565 ? O4 C13 1.252(4) . ? O6 C12 1.262(4) . ? O6 Pr1 2.401(3) 2_654 ? O7 C24 1.251(4) . ? O7 Pr1 2.363(2) 4_566 ? O8 C24 1.262(4) . ? O8 Pr2 2.430(2) 4_566 ? O9 C25 1.249(4) . ? O10 C25 1.263(4) . ? O10 Pr2 2.385(2) 3 ? O11 C36 1.264(4) . ? O11 Pr2 2.379(2) 4_566 ? O11 Pr2 2.906(2) 2 ? O12 C36 1.261(4) . ? O12 Pr2 2.477(3) 2 ? C1 C2 1.514(5) . ? C2 C3 1.364(5) . ? C2 C7 1.427(5) . ? C3 C4 1.403(5) . ? C3 H3A 0.9300 . ? C4 C5 1.364(5) . ? C4 H4A 0.9300 . ? C5 C6 1.429(5) . ? C5 C12 1.488(5) . ? C6 C11 1.419(5) . ? C6 C7 1.432(5) . ? C7 C8 1.421(5) . ? C8 C9 1.358(5) . ? C8 H8A 0.9300 . ? C9 C10 1.402(5) . ? C9 H9A 0.9300 . ? C10 C11 1.352(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.505(5) . ? C14 C15 1.366(5) . ? C14 C19 1.428(5) . ? C15 C16 1.384(5) . ? C15 H15A 0.9300 . ? C16 C17 1.367(5) . ? C16 H16A 0.9300 . ? C17 C18 1.430(5) . ? C17 C24 1.507(5) . ? C18 C23 1.418(4) . ? C18 C19 1.434(4) . ? C19 C20 1.411(5) . ? C20 C21 1.368(5) . ? C20 H20A 0.9300 . ? C21 C22 1.397(5) . ? C21 H21A 0.9300 . ? C22 C23 1.356(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.501(5) . ? C26 C27 1.376(5) . ? C26 C31 1.423(5) . ? C27 C28 1.400(5) . ? C27 H27A 0.9300 . ? C28 C29 1.365(5) . ? C28 H28A 0.9300 . ? C29 C30 1.429(5) . ? C29 C36 1.483(5) . ? C30 C31 1.419(5) . ? C30 C35 1.422(5) . ? C31 C32 1.426(5) . ? C32 C33 1.345(6) . ? C32 H32A 0.9300 . ? C33 C34 1.394(7) . ? C33 H33A 0.9300 . ? C34 C35 1.358(6) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 Pr2 3.066(3) 2 ? N1A C39A 1.317(7) . ? N1A C37A 1.356(7) . ? N1A C40A 1.433(8) . ? N2A C38A 1.319(7) . ? N2A C39A 1.367(9) . ? N2A C41A 1.504(8) . ? C37A C38A 1.407(9) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.521(9) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C44A 1.564(9) . ? C43A C42A 1.607(9) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.483(9) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.535(9) . ? C45A H45A 0.9700 . ? C45A H45D 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N2B C38B 1.328(8) . ? N2B C39B 1.371(10) . ? N2B C41B 1.514(9) . ? N1B C39B 1.315(8) . ? N1B C37B 1.351(8) . ? N1B C40B 1.407(9) . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C37B C38B 1.397(11) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C41B C42B 1.535(10) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.606(10) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C39B H39B 0.9300 . ? C44B C45B 1.473(10) . ? C44B C43B 1.528(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C45B C46B 1.542(10) . ? C45B H45B 0.9700 . ? C45B H45C 0.9700 . ? C46B H46G 0.9600 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? 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 O7 Pr1 O5 148.85(10) 4_565 4_566 ? O7 Pr1 O1 81.14(9) 4_565 . ? O5 Pr1 O1 77.93(10) 4_566 . ? O7 Pr1 O6 76.16(10) 4_565 2_644 ? O5 Pr1 O6 122.40(10) 4_566 2_644 ? O1 Pr1 O6 81.21(10) . 2_644 ? O7 Pr1 O3 82.34(9) 4_565 . ? O5 Pr1 O3 77.45(9) 4_566 . ? O1 Pr1 O3 96.55(10) . . ? O6 Pr1 O3 158.48(10) 2_644 . ? O7 Pr1 O2 138.74(10) 4_565 3_655 ? O5 Pr1 O2 72.39(10) 4_566 3_655 ? O1 Pr1 O2 124.69(8) . 3_655 ? O6 Pr1 O2 77.13(10) 2_644 3_655 ? O3 Pr1 O2 120.18(10) . 3_655 ? O7 Pr1 Cl1 75.91(6) 4_565 . ? O5 Pr1 Cl1 124.41(8) 4_566 . ? O1 Pr1 Cl1 156.79(7) . . ? O6 Pr1 Cl1 89.92(7) 2_644 . ? O3 Pr1 Cl1 83.88(7) . . ? O2 Pr1 Cl1 73.20(6) 3_655 . ? O4 Pr2 O11 101.47(9) . 4_565 ? O4 Pr2 O10 153.33(9) . 3 ? O11 Pr2 O10 78.59(10) 4_565 3 ? O4 Pr2 O8 75.72(8) . 4_565 ? O11 Pr2 O8 81.03(8) 4_565 4_565 ? O10 Pr2 O8 77.99(9) 3 4_565 ? O4 Pr2 O9 73.29(8) . . ? O11 Pr2 O9 74.45(9) 4_565 . ? O10 Pr2 O9 130.76(8) 3 . ? O8 Pr2 O9 135.22(9) 4_565 . ? O4 Pr2 O12 112.49(10) . 2_545 ? O11 Pr2 O12 122.60(8) 4_565 2_545 ? O10 Pr2 O12 88.57(10) 3 2_545 ? O8 Pr2 O12 150.16(9) 4_565 2_545 ? O9 Pr2 O12 73.07(10) . 2_545 ? O4 Pr2 Cl1 83.53(6) . . ? O11 Pr2 Cl1 161.50(6) 4_565 . ? O10 Pr2 Cl1 88.98(7) 3 . ? O8 Pr2 Cl1 83.03(6) 4_565 . ? O9 Pr2 Cl1 123.89(7) . . ? O12 Pr2 Cl1 70.06(6) 2_545 . ? O4 Pr2 O11 140.33(8) . 2_545 ? O11 Pr2 O11 76.82(8) 4_565 2_545 ? O10 Pr2 O11 66.09(8) 3 2_545 ? O8 Pr2 O11 140.68(8) 4_565 2_545 ? O9 Pr2 O11 68.07(8) . 2_545 ? O12 Pr2 O11 47.44(8) 2_545 2_545 ? Cl1 Pr2 O11 110.73(5) . 2_545 ? O4 Pr2 C36 127.25(10) . 2_545 ? O11 Pr2 C36 99.73(9) 4_565 2_545 ? O10 Pr2 C36 78.27(10) 3 2_545 ? O8 Pr2 C36 155.59(10) 4_565 2_545 ? O9 Pr2 C36 66.91(9) . 2_545 ? O12 Pr2 C36 23.33(9) 2_545 2_545 ? Cl1 Pr2 C36 90.95(7) . 2_545 ? O11 Pr2 C36 24.25(8) 2_545 2_545 ? Pr2 Cl1 Pr1 110.68(3) . . ? C1 O1 Pr1 142.4(2) . . ? C1 O2 Pr1 144.8(2) . 3_655 ? C13 O3 Pr1 137.0(2) . . ? C12 O5 Pr1 166.3(3) . 4_565 ? C13 O4 Pr2 144.1(3) . . ? C12 O6 Pr1 125.4(2) . 2_654 ? C24 O7 Pr1 163.2(2) . 4_566 ? C24 O8 Pr2 132.4(2) . 4_566 ? C25 O9 Pr2 136.9(3) . . ? C25 O10 Pr2 139.6(2) . 3 ? C36 O11 Pr2 159.1(2) . 4_566 ? C36 O11 Pr2 85.0(2) . 2 ? Pr2 O11 Pr2 103.18(8) 4_566 2 ? C36 O12 Pr2 105.6(2) . 2 ? O1 C1 O2 125.6(3) . . ? O1 C1 C2 116.3(3) . . ? O2 C1 C2 118.0(3) . . ? C3 C2 C7 120.0(3) . . ? C3 C2 C1 117.4(3) . . ? C7 C2 C1 122.6(3) . . ? C2 C3 C4 120.9(3) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C5 C4 C3 121.5(3) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 C6 119.7(3) . . ? C4 C5 C12 117.1(3) . . ? C6 C5 C12 123.2(3) . . ? C11 C6 C5 122.7(3) . . ? C11 C6 C7 118.4(3) . . ? C5 C6 C7 118.8(3) . . ? C8 C7 C2 122.6(3) . . ? C8 C7 C6 118.3(3) . . ? C2 C7 C6 119.0(3) . . ? C9 C8 C7 120.8(4) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 120.7(4) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 120.5(4) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C6 121.2(4) . . ? C10 C11 H11A 119.4 . . ? C6 C11 H11A 119.4 . . ? O5 C12 O6 123.8(4) . . ? O5 C12 C5 118.3(3) . . ? O6 C12 C5 117.8(3) . . ? O4 C13 O3 124.1(3) . . ? O4 C13 C14 119.6(3) . . ? O3 C13 C14 116.2(3) . . ? C15 C14 C19 119.2(3) . . ? C15 C14 C13 117.3(3) . . ? C19 C14 C13 123.5(3) . . ? C14 C15 C16 122.0(3) . . ? C14 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? C17 C16 C15 121.3(4) . . ? C17 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C16 C17 C18 119.3(3) . . ? C16 C17 C24 115.9(3) . . ? C18 C17 C24 124.8(3) . . ? C23 C18 C17 122.5(3) . . ? C23 C18 C19 118.3(3) . . ? C17 C18 C19 119.2(3) . . ? C20 C19 C14 122.9(3) . . ? C20 C19 C18 118.2(3) . . ? C14 C19 C18 118.8(3) . . ? C21 C20 C19 121.2(4) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C22 120.5(4) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C22 C23 C18 121.5(3) . . ? C22 C23 H23A 119.2 . . ? C18 C23 H23A 119.2 . . ? O7 C24 O8 124.5(3) . . ? O7 C24 C17 115.5(3) . . ? O8 C24 C17 119.9(3) . . ? O9 C25 O10 125.9(3) . . ? O9 C25 C26 119.0(3) . . ? O10 C25 C26 115.1(3) . . ? C27 C26 C31 119.7(3) . . ? C27 C26 C25 118.5(4) . . ? C31 C26 C25 121.5(3) . . ? C26 C27 C28 120.7(4) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C29 C28 C27 120.9(4) . . ? C29 C28 H28A 119.6 . . ? C27 C28 H28A 119.6 . . ? C28 C29 C30 120.0(3) . . ? C28 C29 C36 119.1(4) . . ? C30 C29 C36 120.7(3) . . ? C31 C30 C35 119.2(4) . . ? C31 C30 C29 118.8(3) . . ? C35 C30 C29 122.0(4) . . ? C30 C31 C26 119.3(3) . . ? C30 C31 C32 118.7(4) . . ? C26 C31 C32 122.0(3) . . ? C33 C32 C31 120.2(4) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 121.0(4) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C35 C34 C33 121.5(5) . . ? C35 C34 H34A 119.2 . . ? C33 C34 H34A 119.2 . . ? C34 C35 C30 119.4(4) . . ? C34 C35 H35A 120.3 . . ? C30 C35 H35A 120.3 . . ? O12 C36 O11 121.3(3) . . ? O12 C36 C29 118.4(3) . . ? O11 C36 C29 120.2(3) . . ? O12 C36 Pr2 51.08(18) . 2 ? O11 C36 Pr2 70.76(19) . 2 ? C29 C36 Pr2 168.7(3) . 2 ? C39A N1A C37A 107.7(9) . . ? C39A N1A C40A 124.5(8) . . ? C37A N1A C40A 126.8(8) . . ? C38A N2A C39A 109.0(7) . . ? C38A N2A C41A 126.2(9) . . ? C39A N2A C41A 124.5(7) . . ? N1A C37A C38A 107.4(9) . . ? N1A C37A H37A 126.3 . . ? C38A C37A H37A 126.3 . . ? N2A C38A C37A 105.8(8) . . ? N2A C38A H38A 127.1 . . ? C37A C38A H38A 127.1 . . ? N1A C39A N2A 108.1(8) . . ? N1A C39A H39A 125.9 . . ? N2A C39A H39A 125.9 . . ? N2A C41A C42A 112.8(10) . . ? N2A C41A H41A 109.0 . . ? C42A C41A H41A 109.0 . . ? N2A C41A H41B 109.0 . . ? C42A C41A H41B 109.0 . . ? H41A C41A H41B 107.8 . . ? C44A C43A C42A 95.4(8) . . ? C44A C43A H43A 112.7 . . ? C42A C43A H43A 112.7 . . ? C44A C43A H43B 112.7 . . ? C42A C43A H43B 112.7 . . ? H43A C43A H43B 110.2 . . ? C41A C42A C43A 98.1(9) . . ? C41A C42A H42A 112.1 . . ? C43A C42A H42A 112.1 . . ? C41A C42A H42B 112.1 . . ? C43A C42A H42B 112.1 . . ? H42A C42A H42B 109.8 . . ? C45A C44A C43A 118.3(11) . . ? C45A C44A H44A 107.7 . . ? C43A C44A H44A 107.7 . . ? C45A C44A H44B 107.7 . . ? C43A C44A H44B 107.7 . . ? H44A C44A H44B 107.1 . . ? C44A C45A C46A 114.0(10) . . ? C44A C45A H45A 108.8 . . ? C46A C45A H45A 108.8 . . ? C44A C45A H45D 108.8 . . ? C46A C45A H45D 108.8 . . ? H45A C45A H45D 107.6 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C38B N2B C39B 107.8(9) . . ? C38B N2B C41B 129.5(12) . . ? C39B N2B C41B 122.4(9) . . ? C39B N1B C37B 105.7(13) . . ? C39B N1B C40B 121.0(12) . . ? C37B N1B C40B 132.9(10) . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N1B C37B C38B 109.2(13) . . ? N1B C37B H37B 125.4 . . ? C38B C37B H37B 125.4 . . ? N2B C38B C37B 105.3(11) . . ? N2B C38B H38B 127.4 . . ? C37B C38B H38B 127.4 . . ? N2B C41B C42B 115.5(15) . . ? N2B C41B H41C 108.4 . . ? C42B C41B H41C 108.4 . . ? N2B C41B H41D 108.4 . . ? C42B C41B H41D 108.4 . . ? H41C C41B H41D 107.5 . . ? C41B C42B C43B 107.5(14) . . ? C41B C42B H42C 110.2 . . ? C43B C42B H42C 110.2 . . ? C41B C42B H42D 110.2 . . ? C43B C42B H42D 110.2 . . ? H42C C42B H42D 108.5 . . ? N1B C39B N2B 109.3(12) . . ? N1B C39B H39B 125.4 . . ? N2B C39B H39B 125.4 . . ? C45B C44B C43B 128.1(12) . . ? C45B C44B H44C 105.3 . . ? C43B C44B H44C 105.3 . . ? C45B C44B H44D 105.3 . . ? C43B C44B H44D 105.3 . . ? H44C C44B H44D 106.0 . . ? C44B C43B C42B 115.1(12) . . ? C44B C43B H43C 108.5 . . ? C42B C43B H43C 108.5 . . ? C44B C43B H43D 108.5 . . ? C42B C43B H43D 108.5 . . ? H43C C43B H43D 107.5 . . ? C44B C45B C46B 115.6(11) . . ? C44B C45B H45B 108.4 . . ? C46B C45B H45B 108.4 . . ? C44B C45B H45C 108.4 . . ? C46B C45B H45C 108.4 . . ? H45B C45B H45C 107.4 . . ? C45B C46B H46G 109.5 . . ? C45B C46B H46D 109.5 . . ? H46G C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46G C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Pr2 Cl1 Pr1 -24.06(7) . . . . ? O11 Pr2 Cl1 Pr1 82.9(2) 4_565 . . . ? O10 Pr2 Cl1 Pr1 130.30(7) 3 . . . ? O8 Pr2 Cl1 Pr1 52.27(6) 4_565 . . . ? O9 Pr2 Cl1 Pr1 -88.93(8) . . . . ? O12 Pr2 Cl1 Pr1 -140.85(9) 2_545 . . . ? O11 Pr2 Cl1 Pr1 -165.82(6) 2_545 . . . ? C36 Pr2 Cl1 Pr1 -151.46(8) 2_545 . . . ? O7 Pr1 Cl1 Pr2 -40.17(7) 4_565 . . . ? O5 Pr1 Cl1 Pr2 113.67(9) 4_566 . . . ? O1 Pr1 Cl1 Pr2 -48.91(18) . . . . ? O6 Pr1 Cl1 Pr2 -115.90(8) 2_644 . . . ? O3 Pr1 Cl1 Pr2 43.44(8) . . . . ? O2 Pr1 Cl1 Pr2 167.53(8) 3_655 . . . ? O7 Pr1 O1 C1 -154.1(5) 4_565 . . . ? O5 Pr1 O1 C1 49.1(4) 4_566 . . . ? O6 Pr1 O1 C1 -76.9(4) 2_644 . . . ? O3 Pr1 O1 C1 124.7(4) . . . . ? O2 Pr1 O1 C1 -9.3(5) 3_655 . . . ? Cl1 Pr1 O1 C1 -145.5(4) . . . . ? O7 Pr1 O3 C13 29.4(4) 4_565 . . . ? O5 Pr1 O3 C13 -174.4(4) 4_566 . . . ? O1 Pr1 O3 C13 109.5(4) . . . . ? O6 Pr1 O3 C13 26.9(6) 2_644 . . . ? O2 Pr1 O3 C13 -113.6(4) 3_655 . . . ? Cl1 Pr1 O3 C13 -47.1(4) . . . . ? O11 Pr2 O4 C13 157.1(4) 4_565 . . . ? O10 Pr2 O4 C13 -115.5(4) 3 . . . ? O8 Pr2 O4 C13 -125.4(4) 4_565 . . . ? O9 Pr2 O4 C13 87.4(4) . . . . ? O12 Pr2 O4 C13 24.3(4) 2_545 . . . ? Cl1 Pr2 O4 C13 -40.9(4) . . . . ? O11 Pr2 O4 C13 74.0(4) 2_545 . . . ? C36 Pr2 O4 C13 45.3(4) 2_545 . . . ? O4 Pr2 O9 C25 127.0(4) . . . . ? O11 Pr2 O9 C25 19.6(4) 4_565 . . . ? O10 Pr2 O9 C25 -39.7(4) 3 . . . ? O8 Pr2 O9 C25 78.9(4) 4_565 . . . ? O12 Pr2 O9 C25 -112.4(4) 2_545 . . . ? Cl1 Pr2 O9 C25 -163.1(3) . . . . ? O11 Pr2 O9 C25 -62.2(4) 2_545 . . . ? C36 Pr2 O9 C25 -88.4(4) 2_545 . . . ? Pr1 O1 C1 O2 -5.3(7) . . . . ? Pr1 O1 C1 C2 171.4(3) . . . . ? Pr1 O2 C1 O1 22.8(8) 3_655 . . . ? Pr1 O2 C1 C2 -153.9(3) 3_655 . . . ? O1 C1 C2 C3 -40.6(5) . . . . ? O2 C1 C2 C3 136.4(4) . . . . ? O1 C1 C2 C7 139.6(4) . . . . ? O2 C1 C2 C7 -43.4(5) . . . . ? C7 C2 C3 C4 1.5(6) . . . . ? C1 C2 C3 C4 -178.3(3) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C3 C4 C5 C6 -2.7(6) . . . . ? C3 C4 C5 C12 175.3(4) . . . . ? C4 C5 C6 C11 -174.6(3) . . . . ? C12 C5 C6 C11 7.6(6) . . . . ? C4 C5 C6 C7 3.5(5) . . . . ? C12 C5 C6 C7 -174.4(3) . . . . ? C3 C2 C7 C8 178.0(4) . . . . ? C1 C2 C7 C8 -2.2(6) . . . . ? C3 C2 C7 C6 -0.6(5) . . . . ? C1 C2 C7 C6 179.2(3) . . . . ? C11 C6 C7 C8 -2.4(5) . . . . ? C5 C6 C7 C8 179.5(3) . . . . ? C11 C6 C7 C2 176.3(3) . . . . ? C5 C6 C7 C2 -1.9(5) . . . . ? C2 C7 C8 C9 -176.7(4) . . . . ? C6 C7 C8 C9 1.9(6) . . . . ? C7 C8 C9 C10 -0.1(6) . . . . ? C8 C9 C10 C11 -1.3(7) . . . . ? C9 C10 C11 C6 0.7(6) . . . . ? C5 C6 C11 C10 179.2(4) . . . . ? C7 C6 C11 C10 1.1(6) . . . . ? Pr1 O5 C12 O6 28.6(14) 4_565 . . . ? Pr1 O5 C12 C5 -148.8(10) 4_565 . . . ? Pr1 O6 C12 O5 1.3(6) 2_654 . . . ? Pr1 O6 C12 C5 178.7(2) 2_654 . . . ? C4 C5 C12 O5 35.5(5) . . . . ? C6 C5 C12 O5 -146.6(4) . . . . ? C4 C5 C12 O6 -142.0(4) . . . . ? C6 C5 C12 O6 35.9(5) . . . . ? Pr2 O4 C13 O3 66.2(6) . . . . ? Pr2 O4 C13 C14 -110.9(4) . . . . ? Pr1 O3 C13 O4 3.3(7) . . . . ? Pr1 O3 C13 C14 -179.5(2) . . . . ? O4 C13 C14 C15 143.9(4) . . . . ? O3 C13 C14 C15 -33.4(5) . . . . ? O4 C13 C14 C19 -34.1(5) . . . . ? O3 C13 C14 C19 148.5(4) . . . . ? C19 C14 C15 C16 1.4(6) . . . . ? C13 C14 C15 C16 -176.7(3) . . . . ? C14 C15 C16 C17 0.9(6) . . . . ? C15 C16 C17 C18 -1.6(6) . . . . ? C15 C16 C17 C24 -179.8(3) . . . . ? C16 C17 C18 C23 -178.1(3) . . . . ? C24 C17 C18 C23 0.0(5) . . . . ? C16 C17 C18 C19 -0.1(5) . . . . ? C24 C17 C18 C19 177.9(3) . . . . ? C15 C14 C19 C20 175.1(4) . . . . ? C13 C14 C19 C20 -6.9(5) . . . . ? C15 C14 C19 C18 -3.0(5) . . . . ? C13 C14 C19 C18 175.0(3) . . . . ? C23 C18 C19 C20 2.2(5) . . . . ? C17 C18 C19 C20 -175.8(3) . . . . ? C23 C18 C19 C14 -179.6(3) . . . . ? C17 C18 C19 C14 2.4(5) . . . . ? C14 C19 C20 C21 -179.4(3) . . . . ? C18 C19 C20 C21 -1.3(5) . . . . ? C19 C20 C21 C22 -0.3(6) . . . . ? C20 C21 C22 C23 1.0(6) . . . . ? C21 C22 C23 C18 0.1(6) . . . . ? C17 C18 C23 C22 176.3(4) . . . . ? C19 C18 C23 C22 -1.7(5) . . . . ? Pr1 O7 C24 O8 8.8(11) 4_566 . . . ? Pr1 O7 C24 C17 -169.2(7) 4_566 . . . ? Pr2 O8 C24 O7 -29.9(5) 4_566 . . . ? Pr2 O8 C24 C17 148.0(2) 4_566 . . . ? C16 C17 C24 O7 32.8(5) . . . . ? C18 C17 C24 O7 -145.3(3) . . . . ? C16 C17 C24 O8 -145.3(4) . . . . ? C18 C17 C24 O8 36.6(5) . . . . ? Pr2 O9 C25 O10 26.8(7) . . . . ? Pr2 O9 C25 C26 -154.9(3) . . . . ? Pr2 O10 C25 O9 3.3(7) 3 . . . ? Pr2 O10 C25 C26 -175.0(3) 3 . . . ? O9 C25 C26 C27 -49.6(5) . . . . ? O10 C25 C26 C27 128.8(4) . . . . ? O9 C25 C26 C31 135.8(4) . . . . ? O10 C25 C26 C31 -45.7(5) . . . . ? C31 C26 C27 C28 5.7(6) . . . . ? C25 C26 C27 C28 -168.9(4) . . . . ? C26 C27 C28 C29 0.9(6) . . . . ? C27 C28 C29 C30 -7.4(6) . . . . ? C27 C28 C29 C36 168.1(4) . . . . ? C28 C29 C30 C31 7.2(5) . . . . ? C36 C29 C30 C31 -168.2(3) . . . . ? C28 C29 C30 C35 -170.3(4) . . . . ? C36 C29 C30 C35 14.3(5) . . . . ? C35 C30 C31 C26 176.9(3) . . . . ? C29 C30 C31 C26 -0.6(5) . . . . ? C35 C30 C31 C32 -0.7(5) . . . . ? C29 C30 C31 C32 -178.3(3) . . . . ? C27 C26 C31 C30 -5.7(5) . . . . ? C25 C26 C31 C30 168.8(3) . . . . ? C27 C26 C31 C32 171.8(4) . . . . ? C25 C26 C31 C32 -13.7(5) . . . . ? C30 C31 C32 C33 1.0(6) . . . . ? C26 C31 C32 C33 -176.6(4) . . . . ? C31 C32 C33 C34 -0.3(7) . . . . ? C32 C33 C34 C35 -0.6(8) . . . . ? C33 C34 C35 C30 0.8(7) . . . . ? C31 C30 C35 C34 -0.2(6) . . . . ? C29 C30 C35 C34 177.3(4) . . . . ? Pr2 O12 C36 O11 9.4(5) 2 . . . ? Pr2 O12 C36 C29 -175.1(3) 2 . . . ? Pr2 O11 C36 O12 -122.1(6) 4_566 . . . ? Pr2 O11 C36 O12 -7.7(4) 2 . . . ? Pr2 O11 C36 C29 62.5(9) 4_566 . . . ? Pr2 O11 C36 C29 176.9(3) 2 . . . ? Pr2 O11 C36 Pr2 -114.4(7) 4_566 . . 2 ? C28 C29 C36 O12 -133.9(4) . . . . ? C30 C29 C36 O12 41.5(5) . . . . ? C28 C29 C36 O11 41.6(5) . . . . ? C30 C29 C36 O11 -142.9(4) . . . . ? C28 C29 C36 Pr2 -153.5(11) . . . 2 ? C30 C29 C36 Pr2 21.9(15) . . . 2 ? C39A N1A C37A C38A 7.5(17) . . . . ? C40A N1A C37A C38A 176.9(12) . . . . ? C39A N2A C38A C37A -9(2) . . . . ? C41A N2A C38A C37A 177.0(14) . . . . ? N1A C37A C38A N2A 1.0(15) . . . . ? C37A N1A C39A N2A -13(2) . . . . ? C40A N1A C39A N2A 177.3(15) . . . . ? C38A N2A C39A N1A 14(2) . . . . ? C41A N2A C39A N1A -171.9(14) . . . . ? C38A N2A C41A C42A -11(2) . . . . ? C39A N2A C41A C42A 176.0(19) . . . . ? N2A C41A C42A C43A -76.2(14) . . . . ? C44A C43A C42A C41A -165.9(10) . . . . ? C42A C43A C44A C45A -91.1(14) . . . . ? C43A C44A C45A C46A -124.0(15) . . . . ? C39B N1B C37B C38B -11(3) . . . . ? C40B N1B C37B C38B 176(2) . . . . ? C39B N2B C38B C37B 9(3) . . . . ? C41B N2B C38B C37B -178(2) . . . . ? N1B C37B C38B N2B 1(2) . . . . ? C38B N2B C41B C42B -87(3) . . . . ? C39B N2B C41B C42B 85(3) . . . . ? N2B C41B C42B C43B 89.6(19) . . . . ? C37B N1B C39B N2B 17(3) . . . . ? C40B N1B C39B N2B -169(2) . . . . ? C38B N2B C39B N1B -17(4) . . . . ? C41B N2B C39B N1B 170(2) . . . . ? C45B C44B C43B C42B -165(2) . . . . ? C41B C42B C43B C44B -151.7(16) . . . . ? C43B C44B C45B C46B 15(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.871 _refine_diff_density_min -1.366 _refine_diff_density_rms 0.119 #===END data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 876524' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Nd2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl N2 Nd2 O12' _chemical_formula_weight 1133.71 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.9082(4) _cell_length_b 14.8189(3) _cell_length_c 16.0623(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.729(2) _cell_angle_gamma 90.00 _cell_volume 4241.34(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12458 _cell_measurement_theta_min 2.4986 _cell_measurement_theta_max 28.8360 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 2.552 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83176 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19250 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8812 _reflns_number_gt 7086 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8812 _refine_ls_number_parameters 607 _refine_ls_number_restraints 374 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.102 _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 Nd1 Nd 0.377983(9) 0.024920(11) -0.005390(9) 0.01466(6) Uani 1 1 d . . . Nd2 Nd 0.115198(9) 0.012618(11) -0.001139(9) 0.01530(6) Uani 1 1 d . . . Cl1 Cl 0.25183(4) -0.08647(6) 0.02321(6) 0.0315(2) Uani 1 1 d . . . O1 O 0.44890(14) 0.12933(17) -0.07751(16) 0.0402(7) Uani 1 1 d . . . O2 O 0.57262(14) 0.11102(16) -0.06093(16) 0.0392(7) Uani 1 1 d . . . O3 O 0.31539(14) 0.13322(17) 0.07478(16) 0.0426(7) Uani 1 1 d . . . O5 O 0.47380(15) 0.43190(18) -0.39989(15) 0.0451(7) Uani 1 1 d . . . O4 O 0.19436(13) 0.13749(15) 0.02984(15) 0.0333(6) Uani 1 1 d . . . O6 O 0.59749(15) 0.43247(18) -0.37888(15) 0.0420(7) Uani 1 1 d . . . O7 O 0.28491(13) 0.43100(17) 0.38873(14) 0.0344(6) Uani 1 1 d . . . O8 O 0.16141(13) 0.45046(16) 0.36640(13) 0.0289(6) Uani 1 1 d . . . O9 O 0.06233(14) 0.09641(17) 0.11002(15) 0.0373(6) Uani 1 1 d . . . O10 O -0.06261(14) 0.10420(17) 0.08936(15) 0.0375(6) Uani 1 1 d . . . O11 O 0.00765(13) 0.41510(17) 0.43403(14) 0.0341(6) Uani 1 1 d . . . O12 O -0.11028(14) 0.40830(19) 0.38273(16) 0.0445(7) Uani 1 1 d . . . C1 C 0.51406(19) 0.1489(2) -0.0924(2) 0.0267(8) Uani 1 1 d . . . C2 C 0.52157(18) 0.2217(2) -0.1567(2) 0.0234(7) Uani 1 1 d . . . C3 C 0.47162(19) 0.2209(2) -0.2267(2) 0.0324(9) Uani 1 1 d . . . H3A H 0.4342 0.1772 -0.2324 0.039 Uiso 1 1 calc R . . C4 C 0.4759(2) 0.2853(2) -0.2900(2) 0.0320(9) Uani 1 1 d . . . H4A H 0.4407 0.2838 -0.3367 0.038 Uiso 1 1 calc R . . C5 C 0.53015(18) 0.3497(2) -0.2849(2) 0.0250(8) Uani 1 1 d . . . C6 C 0.58201(18) 0.3556(2) -0.2115(2) 0.0228(7) Uani 1 1 d . . . C7 C 0.57819(18) 0.2897(2) -0.14731(19) 0.0234(7) Uani 1 1 d . . . C8 C 0.6305(2) 0.2959(2) -0.0745(2) 0.0316(9) Uani 1 1 d . . . H8A H 0.6297 0.2528 -0.0325 0.038 Uiso 1 1 calc R . . C9 C 0.6813(2) 0.3640(3) -0.0659(2) 0.0410(10) Uani 1 1 d . . . H9A H 0.7152 0.3668 -0.0183 0.049 Uiso 1 1 calc R . . C10 C 0.6832(2) 0.4303(3) -0.1279(2) 0.0402(10) Uani 1 1 d . . . H10A H 0.7176 0.4773 -0.1204 0.048 Uiso 1 1 calc R . . C11 C 0.6356(2) 0.4262(2) -0.1987(2) 0.0304(8) Uani 1 1 d . . . H11A H 0.6379 0.4703 -0.2396 0.037 Uiso 1 1 calc R . . C12 C 0.5337(2) 0.4100(2) -0.3595(2) 0.0298(8) Uani 1 1 d . . . C13 C 0.25031(19) 0.1650(2) 0.0761(2) 0.0269(8) Uani 1 1 d . . . C14 C 0.23957(18) 0.2363(2) 0.1396(2) 0.0251(7) Uani 1 1 d . . . C15 C 0.2833(2) 0.2297(3) 0.2148(2) 0.0372(10) Uani 1 1 d . . . H15A H 0.3186 0.1837 0.2223 0.045 Uiso 1 1 calc R . . C16 C 0.2761(2) 0.2902(2) 0.2798(2) 0.0334(9) Uani 1 1 d . . . H16A H 0.3074 0.2843 0.3292 0.040 Uiso 1 1 calc R . . C17 C 0.22434(17) 0.3576(2) 0.27271(19) 0.0215(7) Uani 1 1 d . . . C18 C 0.17729(17) 0.3686(2) 0.19583(19) 0.0199(7) Uani 1 1 d . . . C19 C 0.18651(18) 0.3075(2) 0.12819(19) 0.0218(7) Uani 1 1 d . . . C20 C 0.1434(2) 0.3236(2) 0.0506(2) 0.0319(9) Uani 1 1 d . . . H20A H 0.1496 0.2861 0.0054 0.038 Uiso 1 1 calc R . . C21 C 0.0932(2) 0.3930(3) 0.0410(2) 0.0386(10) Uani 1 1 d . . . H21A H 0.0654 0.4022 -0.0104 0.046 Uiso 1 1 calc R . . C22 C 0.0833(2) 0.4505(2) 0.1085(2) 0.0372(9) Uani 1 1 d . . . H22A H 0.0486 0.4973 0.1016 0.045 Uiso 1 1 calc R . . C23 C 0.12359(19) 0.4385(2) 0.1832(2) 0.0269(8) Uani 1 1 d . . . H23A H 0.1159 0.4770 0.2273 0.032 Uiso 1 1 calc R . . C24 C 0.22248(18) 0.4183(2) 0.34792(18) 0.0232(7) Uani 1 1 d . . . C25 C 0.0009(2) 0.1311(2) 0.1217(2) 0.0286(8) Uani 1 1 d . . . C26 C -0.00128(18) 0.2088(2) 0.1801(2) 0.0249(8) Uani 1 1 d . . . C27 C 0.0375(2) 0.2025(3) 0.2583(2) 0.0346(9) Uani 1 1 d . . . H27A H 0.0709 0.1551 0.2700 0.042 Uiso 1 1 calc R . . C28 C 0.0275(2) 0.2664(3) 0.3207(2) 0.0357(9) Uani 1 1 d . . . H28A H 0.0551 0.2612 0.3727 0.043 Uiso 1 1 calc R . . C29 C -0.02197(19) 0.3360(2) 0.3064(2) 0.0280(8) Uani 1 1 d . . . C30 C -0.05744(19) 0.3509(2) 0.2232(2) 0.0272(8) Uani 1 1 d . . . C31 C -0.04746(19) 0.2860(2) 0.1610(2) 0.0268(8) Uani 1 1 d . . . C32 C -0.0808(2) 0.3024(3) 0.0775(2) 0.0389(10) Uani 1 1 d . . . H32A H -0.0746 0.2608 0.0353 0.047 Uiso 1 1 calc R . . C33 C -0.1212(3) 0.3784(3) 0.0602(3) 0.0548(12) Uani 1 1 d . . . H33A H -0.1433 0.3883 0.0060 0.066 Uiso 1 1 calc R . . C34 C -0.1303(2) 0.4420(3) 0.1219(3) 0.0556(12) Uani 1 1 d . . . H34A H -0.1573 0.4944 0.1079 0.067 Uiso 1 1 calc R . . C35 C -0.1006(2) 0.4293(3) 0.2028(3) 0.0404(10) Uani 1 1 d . . . H35A H -0.1085 0.4716 0.2438 0.048 Uiso 1 1 calc R . . C36 C -0.0423(2) 0.3908(2) 0.3775(2) 0.0297(8) Uani 1 1 d . . . N1A N 0.2368(6) -0.2684(7) 0.2784(5) 0.0614(15) Uani 0.609(5) 1 d PDU A 1 N2A N 0.3061(8) -0.1490(8) 0.2687(8) 0.0714(15) Uani 0.609(5) 1 d PDU A 1 C37A C 0.2877(5) -0.2658(6) 0.3468(6) 0.0589(17) Uani 0.609(5) 1 d PDU A 1 H37A H 0.2925 -0.3074 0.3903 0.071 Uiso 0.609(5) 1 calc PR A 1 C38A C 0.3328(7) -0.1868(7) 0.3394(7) 0.0733(18) Uani 0.609(5) 1 d PDU A 1 H38A H 0.3723 -0.1666 0.3766 0.088 Uiso 0.609(5) 1 calc PR A 1 C39A C 0.2491(8) -0.1981(9) 0.2315(7) 0.0548(18) Uani 0.609(5) 1 d PDU A 1 H39A H 0.2224 -0.1846 0.1804 0.066 Uiso 0.609(5) 1 calc PR A 1 C40A C 0.1822(6) -0.3371(7) 0.2595(7) 0.083(3) Uani 0.609(5) 1 d PDU A 1 H40A H 0.1449 -0.3160 0.2168 0.125 Uiso 0.609(5) 1 calc PR A 1 H40B H 0.1587 -0.3518 0.3089 0.125 Uiso 0.609(5) 1 calc PR A 1 H40C H 0.2061 -0.3899 0.2399 0.125 Uiso 0.609(5) 1 calc PR A 1 C41A C 0.3317(6) -0.0600(6) 0.2375(7) 0.096(2) Uani 0.609(5) 1 d PDU A 1 H41A H 0.2882 -0.0214 0.2258 0.115 Uiso 0.609(5) 1 calc PR A 1 H41B H 0.3531 -0.0700 0.1850 0.115 Uiso 0.609(5) 1 calc PR A 1 C43A C 0.3294(6) 0.0279(8) 0.3564(8) 0.128(2) Uani 0.609(5) 1 d PDU A 1 H43A H 0.2857 0.0538 0.3247 0.154 Uiso 0.609(5) 1 calc PR A 1 H43B H 0.3140 -0.0176 0.3946 0.154 Uiso 0.609(5) 1 calc PR A 1 C42A C 0.3895(6) -0.0102(8) 0.2971(7) 0.113(2) Uani 0.609(5) 1 d PDU A 1 H42A H 0.4149 0.0375 0.2696 0.135 Uiso 0.609(5) 1 calc PR A 1 H42B H 0.4259 -0.0504 0.3263 0.135 Uiso 0.609(5) 1 calc PR A 1 C44A C 0.3811(8) 0.1016(8) 0.4024(7) 0.149(3) Uani 0.609(5) 1 d PDU A 1 H44A H 0.4166 0.1218 0.3646 0.179 Uiso 0.609(5) 1 calc PR A 1 H44B H 0.3502 0.1529 0.4139 0.179 Uiso 0.609(5) 1 calc PR A 1 C45A C 0.4232(8) 0.0730(9) 0.4812(7) 0.160(3) Uani 0.609(5) 1 d PDU A 1 H45A H 0.4762 0.0711 0.4734 0.192 Uiso 0.609(5) 1 calc PR A 1 H45D H 0.4079 0.0122 0.4942 0.192 Uiso 0.609(5) 1 calc PR A 1 C46A C 0.4124(10) 0.1342(11) 0.5558(8) 0.188(5) Uani 0.609(5) 1 d PDU A 1 H46A H 0.4444 0.1143 0.6037 0.282 Uiso 0.609(5) 1 calc PR A 1 H46B H 0.3610 0.1315 0.5679 0.282 Uiso 0.609(5) 1 calc PR A 1 H46C H 0.4249 0.1951 0.5425 0.282 Uiso 0.609(5) 1 calc PR A 1 N2B N 0.3101(13) -0.1663(13) 0.2733(12) 0.0714(15) Uani 0.391(5) 1 d PDU A 2 N1B N 0.2243(10) -0.2721(11) 0.2525(8) 0.0614(15) Uani 0.391(5) 1 d PDU A 2 C40B C 0.1676(9) -0.3216(11) 0.2079(10) 0.083(3) Uani 0.391(5) 1 d PDU A 2 H40D H 0.1648 -0.3055 0.1498 0.125 Uiso 0.391(5) 1 calc PR A 2 H40E H 0.1205 -0.3087 0.2292 0.125 Uiso 0.391(5) 1 calc PR A 2 H40F H 0.1784 -0.3849 0.2141 0.125 Uiso 0.391(5) 1 calc PR A 2 C37B C 0.2594(9) -0.2819(10) 0.3307(9) 0.0589(17) Uani 0.391(5) 1 d PDU A 2 H37B H 0.2477 -0.3244 0.3700 0.071 Uiso 0.391(5) 1 calc PR A 2 C38B C 0.3171(11) -0.2159(11) 0.3421(10) 0.0733(18) Uani 0.391(5) 1 d PDU A 2 H38B H 0.3523 -0.2090 0.3883 0.088 Uiso 0.391(5) 1 calc PR A 2 C41B C 0.3590(9) -0.0892(9) 0.2494(12) 0.096(2) Uani 0.391(5) 1 d PDU A 2 H41C H 0.3587 -0.0880 0.1890 0.115 Uiso 0.391(5) 1 calc PR A 2 H41D H 0.4102 -0.1003 0.2730 0.115 Uiso 0.391(5) 1 calc PR A 2 C42B C 0.3340(11) 0.0034(11) 0.2793(10) 0.113(2) Uani 0.391(5) 1 d PDU A 2 H42C H 0.2808 0.0024 0.2863 0.135 Uiso 0.391(5) 1 calc PR A 2 H42D H 0.3427 0.0493 0.2383 0.135 Uiso 0.391(5) 1 calc PR A 2 C39B C 0.2555(13) -0.2023(14) 0.2193(11) 0.0548(18) Uani 0.391(5) 1 d PDU A 2 H39B H 0.2418 -0.1805 0.1657 0.066 Uiso 0.391(5) 1 calc PR A 2 C44B C 0.3381(10) 0.0812(14) 0.4266(11) 0.149(3) Uani 0.391(5) 1 d PDU A 2 H44C H 0.3074 0.1213 0.3897 0.179 Uiso 0.391(5) 1 calc PR A 2 H44D H 0.3034 0.0382 0.4472 0.179 Uiso 0.391(5) 1 calc PR A 2 C43B C 0.3819(10) 0.0262(14) 0.3679(11) 0.128(2) Uani 0.391(5) 1 d PDU A 2 H43C H 0.3978 -0.0300 0.3953 0.154 Uiso 0.391(5) 1 calc PR A 2 H43D H 0.4267 0.0593 0.3572 0.154 Uiso 0.391(5) 1 calc PR A 2 C45B C 0.3623(10) 0.1372(14) 0.4997(12) 0.160(3) Uani 0.391(5) 1 d PDU A 2 H45B H 0.3405 0.1130 0.5479 0.192 Uiso 0.391(5) 1 calc PR A 2 H45C H 0.3426 0.1977 0.4899 0.192 Uiso 0.391(5) 1 calc PR A 2 C46B C 0.4485(10) 0.1431(18) 0.5205(15) 0.188(5) Uani 0.391(5) 1 d PDU A 2 H46G H 0.4605 0.1927 0.5579 0.282 Uiso 0.391(5) 1 calc PR A 2 H46D H 0.4718 0.1524 0.4698 0.282 Uiso 0.391(5) 1 calc PR A 2 H46E H 0.4667 0.0880 0.5465 0.282 Uiso 0.391(5) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01551(9) 0.01643(9) 0.01206(9) -0.00004(6) 0.00151(6) 0.00096(6) Nd2 0.01592(9) 0.01694(10) 0.01312(9) -0.00025(7) 0.00187(6) -0.00118(7) Cl1 0.0203(4) 0.0284(5) 0.0467(5) 0.0137(4) 0.0080(4) 0.0030(3) O1 0.0267(15) 0.0417(16) 0.0526(16) 0.0260(14) 0.0063(12) -0.0047(12) O2 0.0290(15) 0.0358(15) 0.0518(16) 0.0223(13) -0.0014(12) 0.0033(12) O3 0.0310(15) 0.0452(16) 0.0515(16) -0.0295(14) 0.0031(12) 0.0079(12) O5 0.0446(17) 0.0501(17) 0.0360(14) 0.0206(14) -0.0181(13) -0.0034(14) O4 0.0268(14) 0.0333(14) 0.0405(14) -0.0177(12) 0.0065(11) -0.0093(11) O6 0.0427(17) 0.0529(18) 0.0307(14) 0.0220(13) 0.0046(12) -0.0110(14) O7 0.0223(13) 0.0540(16) 0.0261(12) -0.0197(12) -0.0020(10) 0.0003(12) O8 0.0273(14) 0.0427(15) 0.0171(11) -0.0071(11) 0.0041(9) 0.0077(11) O9 0.0312(15) 0.0464(16) 0.0358(14) -0.0209(13) 0.0112(11) -0.0026(12) O10 0.0300(15) 0.0402(15) 0.0439(15) -0.0234(13) 0.0109(12) -0.0116(12) O11 0.0341(15) 0.0411(15) 0.0272(13) -0.0148(12) 0.0036(11) -0.0139(12) O12 0.0258(15) 0.0599(19) 0.0494(16) -0.0339(15) 0.0126(12) -0.0072(13) C1 0.0234(19) 0.0240(18) 0.0321(19) 0.0114(16) 0.0000(15) -0.0020(14) C2 0.0199(17) 0.0213(17) 0.0291(18) 0.0109(15) 0.0026(14) 0.0000(13) C3 0.0208(19) 0.037(2) 0.038(2) 0.0141(18) -0.0039(15) -0.0083(16) C4 0.028(2) 0.039(2) 0.0274(19) 0.0135(17) -0.0069(15) -0.0061(16) C5 0.0212(18) 0.0303(19) 0.0235(17) 0.0069(15) 0.0020(14) 0.0022(14) C6 0.0192(17) 0.0254(17) 0.0239(17) 0.0092(15) 0.0028(13) 0.0002(14) C7 0.0195(17) 0.0287(18) 0.0222(16) 0.0069(15) 0.0032(13) -0.0007(14) C8 0.036(2) 0.039(2) 0.0193(17) 0.0098(16) -0.0022(15) -0.0037(17) C9 0.041(2) 0.053(3) 0.0266(19) 0.0013(19) -0.0082(17) -0.011(2) C10 0.042(2) 0.046(2) 0.032(2) -0.0026(19) 0.0023(17) -0.0194(19) C11 0.035(2) 0.0284(19) 0.0285(18) 0.0063(16) 0.0059(15) -0.0070(16) C12 0.036(2) 0.0291(19) 0.0236(18) 0.0051(16) -0.0028(16) -0.0018(16) C13 0.0235(19) 0.0262(18) 0.0321(19) -0.0106(16) 0.0084(15) -0.0040(15) C14 0.0210(18) 0.0283(18) 0.0262(17) -0.0098(15) 0.0039(14) -0.0005(14) C15 0.030(2) 0.038(2) 0.041(2) -0.0164(19) -0.0031(17) 0.0149(17) C16 0.030(2) 0.043(2) 0.0250(18) -0.0100(17) -0.0074(15) 0.0105(17) C17 0.0191(17) 0.0270(18) 0.0186(16) -0.0084(14) 0.0024(13) -0.0009(14) C18 0.0177(17) 0.0220(16) 0.0201(16) -0.0040(14) 0.0026(13) -0.0044(13) C19 0.0214(17) 0.0265(17) 0.0177(15) -0.0082(14) 0.0032(13) -0.0027(14) C20 0.038(2) 0.037(2) 0.0202(17) -0.0069(16) -0.0007(15) -0.0019(17) C21 0.043(2) 0.048(2) 0.0232(18) -0.0023(18) -0.0076(16) 0.0086(19) C22 0.039(2) 0.035(2) 0.037(2) 0.0009(18) -0.0012(17) 0.0109(17) C23 0.030(2) 0.0262(18) 0.0253(17) -0.0018(15) 0.0035(14) 0.0042(15) C24 0.0239(18) 0.0292(18) 0.0165(15) -0.0027(14) 0.0017(13) -0.0004(14) C25 0.032(2) 0.032(2) 0.0235(17) -0.0087(16) 0.0115(15) -0.0087(16) C26 0.0207(18) 0.0303(19) 0.0243(17) -0.0112(15) 0.0065(13) -0.0069(14) C27 0.031(2) 0.037(2) 0.035(2) -0.0144(18) -0.0020(16) 0.0077(17) C28 0.036(2) 0.048(2) 0.0216(18) -0.0145(17) -0.0039(15) 0.0020(18) C29 0.0232(19) 0.033(2) 0.0286(18) -0.0143(16) 0.0057(14) -0.0061(15) C30 0.0252(19) 0.0304(19) 0.0266(18) -0.0075(16) 0.0060(14) -0.0069(15) C31 0.0252(19) 0.0308(19) 0.0248(17) -0.0071(16) 0.0040(14) -0.0097(15) C32 0.045(3) 0.047(2) 0.0236(19) -0.0024(18) -0.0005(17) -0.011(2) C33 0.061(3) 0.065(3) 0.037(2) 0.011(2) -0.004(2) -0.005(3) C34 0.047(3) 0.054(3) 0.065(3) 0.018(3) 0.002(2) 0.008(2) C35 0.043(2) 0.034(2) 0.046(2) -0.0033(19) 0.0134(19) -0.0001(18) C36 0.032(2) 0.030(2) 0.0282(18) -0.0127(16) 0.0092(15) -0.0111(16) N1A 0.070(3) 0.058(2) 0.060(4) 0.006(3) 0.024(3) 0.021(2) N2A 0.090(3) 0.076(3) 0.050(2) -0.002(2) 0.016(2) 0.011(3) C37A 0.074(4) 0.054(3) 0.047(3) 0.007(3) 0.003(3) 0.012(3) C38A 0.090(4) 0.077(4) 0.053(3) 0.006(3) 0.006(3) 0.021(3) C39A 0.066(3) 0.058(3) 0.042(3) 0.005(3) 0.016(3) 0.003(2) C40A 0.082(5) 0.052(5) 0.126(8) -0.003(6) 0.059(6) 0.008(4) C41A 0.120(4) 0.084(4) 0.091(3) 0.002(3) 0.043(3) -0.020(4) C43A 0.158(5) 0.108(4) 0.126(4) -0.010(4) 0.050(4) -0.028(4) C42A 0.137(4) 0.103(4) 0.105(4) -0.016(3) 0.042(4) -0.025(4) C44A 0.177(5) 0.123(5) 0.153(5) 0.016(4) 0.038(5) -0.037(5) C45A 0.187(6) 0.129(5) 0.167(6) 0.019(5) 0.033(5) -0.034(5) C46A 0.227(9) 0.151(7) 0.197(9) 0.000(8) 0.075(8) -0.031(8) N2B 0.090(3) 0.076(3) 0.050(2) -0.002(2) 0.016(2) 0.011(3) N1B 0.070(3) 0.058(2) 0.060(4) 0.006(3) 0.024(3) 0.021(2) C40B 0.082(5) 0.052(5) 0.126(8) -0.003(6) 0.059(6) 0.008(4) C37B 0.074(4) 0.054(3) 0.047(3) 0.007(3) 0.003(3) 0.012(3) C38B 0.090(4) 0.077(4) 0.053(3) 0.006(3) 0.006(3) 0.021(3) C41B 0.120(4) 0.084(4) 0.091(3) 0.002(3) 0.043(3) -0.020(4) C42B 0.137(4) 0.103(4) 0.105(4) -0.016(3) 0.042(4) -0.025(4) C39B 0.066(3) 0.058(3) 0.042(3) 0.005(3) 0.016(3) 0.003(2) C44B 0.177(5) 0.123(5) 0.153(5) 0.016(4) 0.038(5) -0.037(5) C43B 0.158(5) 0.108(4) 0.126(4) -0.010(4) 0.050(4) -0.028(4) C45B 0.187(6) 0.129(5) 0.167(6) 0.019(5) 0.033(5) -0.034(5) C46B 0.227(9) 0.151(7) 0.197(9) 0.000(8) 0.075(8) -0.031(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O7 2.352(2) 4_565 ? Nd1 O1 2.375(2) . ? Nd1 O5 2.376(2) 4_566 ? Nd1 O6 2.385(2) 2_644 ? Nd1 O3 2.404(2) . ? Nd1 O2 2.406(2) 3_655 ? Nd1 Cl1 2.8717(9) . ? Nd2 O11 2.354(2) 4_565 ? Nd2 O4 2.354(2) . ? Nd2 O10 2.372(2) 3 ? Nd2 O8 2.421(2) 4_565 ? Nd2 O9 2.442(2) . ? Nd2 O12 2.459(2) 2_545 ? Nd2 Cl1 2.8470(8) . ? Nd2 O11 2.926(3) 2_545 ? Nd2 C36 3.071(4) 2_545 ? O1 C1 1.249(4) . ? O2 C1 1.251(4) . ? O2 Nd1 2.406(2) 3_655 ? O3 C13 1.259(4) . ? O5 C12 1.240(4) . ? O5 Nd1 2.376(2) 4_565 ? O4 C13 1.254(4) . ? O6 C12 1.258(4) . ? O6 Nd1 2.385(2) 2_654 ? O7 C24 1.253(4) . ? O7 Nd1 2.352(2) 4_566 ? O8 C24 1.255(4) . ? O8 Nd2 2.421(2) 4_566 ? O9 C25 1.246(4) . ? O10 C25 1.267(4) . ? O10 Nd2 2.372(2) 3 ? O11 C36 1.262(4) . ? O11 Nd2 2.354(2) 4_566 ? O11 Nd2 2.926(3) 2 ? O12 C36 1.256(4) . ? O12 Nd2 2.459(2) 2 ? C1 C2 1.508(4) . ? C2 C3 1.365(4) . ? C2 C7 1.427(4) . ? C3 C4 1.402(5) . ? C3 H3A 0.9300 . ? C4 C5 1.359(4) . ? C4 H4A 0.9300 . ? C5 C6 1.429(4) . ? C5 C12 1.501(4) . ? C6 C11 1.421(4) . ? C6 C7 1.427(4) . ? C7 C8 1.426(4) . ? C8 C9 1.356(5) . ? C8 H8A 0.9300 . ? C9 C10 1.402(5) . ? C9 H9A 0.9300 . ? C10 C11 1.353(4) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.495(4) . ? C14 C15 1.375(4) . ? C14 C19 1.420(4) . ? C15 C16 1.391(5) . ? C15 H15A 0.9300 . ? C16 C17 1.360(4) . ? C16 H16A 0.9300 . ? C17 C18 1.433(4) . ? C17 C24 1.509(4) . ? C18 C23 1.414(4) . ? C18 C19 1.436(4) . ? C19 C20 1.419(4) . ? C20 C21 1.365(5) . ? C20 H20A 0.9300 . ? C21 C22 1.404(5) . ? C21 H21A 0.9300 . ? C22 C23 1.349(4) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.488(4) . ? C26 C27 1.376(4) . ? C26 C31 1.428(5) . ? C27 C28 1.403(5) . ? C27 H27A 0.9300 . ? C28 C29 1.364(5) . ? C28 H28A 0.9300 . ? C29 C30 1.437(4) . ? C29 C36 1.476(5) . ? C30 C31 1.411(5) . ? C30 C35 1.416(5) . ? C31 C32 1.433(4) . ? C32 C33 1.354(6) . ? C32 H32A 0.9300 . ? C33 C34 1.390(6) . ? C33 H33A 0.9300 . ? C34 C35 1.366(5) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 Nd2 3.071(4) 2 ? N1A C39A 1.316(7) . ? N1A C37A 1.356(6) . ? N1A C40A 1.423(8) . ? N2A C38A 1.312(6) . ? N2A C39A 1.345(7) . ? N2A C41A 1.498(8) . ? C37A C38A 1.433(9) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.528(9) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C44A 1.567(9) . ? C43A C42A 1.609(9) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.470(9) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.530(9) . ? C45A H45A 0.9700 . ? C45A H45D 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N2B C38B 1.324(8) . ? N2B C39B 1.350(9) . ? N2B C41B 1.511(9) . ? N1B C39B 1.314(8) . ? N1B C37B 1.356(8) . ? N1B C40B 1.391(9) . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C37B C38B 1.421(11) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C41B C42B 1.536(10) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.622(10) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C39B H39B 0.9300 . ? C44B C45B 1.467(10) . ? C44B C43B 1.523(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C45B C46B 1.550(10) . ? C45B H45B 0.9700 . ? C45B H45C 0.9700 . ? C46B H46G 0.9600 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? 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 O7 Nd1 O1 80.87(8) 4_565 . ? O7 Nd1 O5 148.23(10) 4_565 4_566 ? O1 Nd1 O5 77.83(9) . 4_566 ? O7 Nd1 O6 76.60(9) 4_565 2_644 ? O1 Nd1 O6 81.09(10) . 2_644 ? O5 Nd1 O6 122.31(9) 4_566 2_644 ? O7 Nd1 O3 82.37(9) 4_565 . ? O1 Nd1 O3 97.30(10) . . ? O5 Nd1 O3 77.31(9) 4_566 . ? O6 Nd1 O3 158.91(9) 2_644 . ? O7 Nd1 O2 139.07(9) 4_565 3_655 ? O1 Nd1 O2 124.78(9) . 3_655 ? O5 Nd1 O2 72.68(9) 4_566 3_655 ? O6 Nd1 O2 77.05(9) 2_644 3_655 ? O3 Nd1 O2 119.50(9) . 3_655 ? O7 Nd1 Cl1 76.31(6) 4_565 . ? O1 Nd1 Cl1 156.91(6) . . ? O5 Nd1 Cl1 124.36(7) 4_566 . ? O6 Nd1 Cl1 90.20(7) 2_644 . ? O3 Nd1 Cl1 83.21(7) . . ? O2 Nd1 Cl1 73.04(6) 3_655 . ? O11 Nd2 O4 100.64(8) 4_565 . ? O11 Nd2 O10 79.01(9) 4_565 3 ? O4 Nd2 O10 153.50(9) . 3 ? O11 Nd2 O8 81.07(8) 4_565 4_565 ? O4 Nd2 O8 75.92(8) . 4_565 ? O10 Nd2 O8 77.88(8) 3 4_565 ? O11 Nd2 O9 74.47(8) 4_565 . ? O4 Nd2 O9 73.44(8) . . ? O10 Nd2 O9 130.40(8) 3 . ? O8 Nd2 O9 135.98(8) 4_565 . ? O11 Nd2 O12 122.50(8) 4_565 2_545 ? O4 Nd2 O12 113.45(9) . 2_545 ? O10 Nd2 O12 87.74(9) 3 2_545 ? O8 Nd2 O12 149.70(9) 4_565 2_545 ? O9 Nd2 O12 73.01(9) . 2_545 ? O11 Nd2 Cl1 161.72(6) 4_565 . ? O4 Nd2 Cl1 83.41(6) . . ? O10 Nd2 Cl1 89.44(6) 3 . ? O8 Nd2 Cl1 82.69(6) 4_565 . ? O9 Nd2 Cl1 123.54(6) . . ? O12 Nd2 Cl1 70.50(6) 2_545 . ? O11 Nd2 O11 77.04(8) 4_565 2_545 ? O4 Nd2 O11 140.30(8) . 2_545 ? O10 Nd2 O11 65.88(8) 3 2_545 ? O8 Nd2 O11 140.42(7) 4_565 2_545 ? O9 Nd2 O11 67.74(8) . 2_545 ? O12 Nd2 O11 47.04(7) 2_545 2_545 ? Cl1 Nd2 O11 111.23(5) . 2_545 ? O11 Nd2 C36 99.89(9) 4_565 2_545 ? O4 Nd2 C36 127.71(9) . 2_545 ? O10 Nd2 C36 77.76(9) 3 2_545 ? O8 Nd2 C36 154.96(9) 4_565 2_545 ? O9 Nd2 C36 66.75(9) . 2_545 ? O12 Nd2 C36 23.03(8) 2_545 2_545 ? Cl1 Nd2 C36 91.32(7) . 2_545 ? O11 Nd2 C36 24.14(7) 2_545 2_545 ? Nd2 Cl1 Nd1 111.14(3) . . ? C1 O1 Nd1 143.2(2) . . ? C1 O2 Nd1 144.2(2) . 3_655 ? C13 O3 Nd1 137.8(2) . . ? C12 O5 Nd1 165.7(3) . 4_565 ? C13 O4 Nd2 144.0(2) . . ? C12 O6 Nd1 125.9(2) . 2_654 ? C24 O7 Nd1 162.0(2) . 4_566 ? C24 O8 Nd2 132.51(19) . 4_566 ? C25 O9 Nd2 137.1(2) . . ? C25 O10 Nd2 139.6(2) . 3 ? C36 O11 Nd2 159.7(2) . 4_566 ? C36 O11 Nd2 84.4(2) . 2 ? Nd2 O11 Nd2 102.96(8) 4_566 2 ? C36 O12 Nd2 107.0(2) . 2 ? O1 C1 O2 125.4(3) . . ? O1 C1 C2 116.5(3) . . ? O2 C1 C2 118.0(3) . . ? C3 C2 C7 119.6(3) . . ? C3 C2 C1 117.5(3) . . ? C7 C2 C1 122.9(3) . . ? C2 C3 C4 120.9(3) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C5 C4 C3 121.6(3) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 119.6(3) . . ? C4 C5 C12 117.2(3) . . ? C6 C5 C12 123.1(3) . . ? C11 C6 C7 118.6(3) . . ? C11 C6 C5 122.6(3) . . ? C7 C6 C5 118.7(3) . . ? C8 C7 C6 118.3(3) . . ? C8 C7 C2 122.3(3) . . ? C6 C7 C2 119.4(3) . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.9(3) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C6 121.0(3) . . ? C10 C11 H11A 119.5 . . ? C6 C11 H11A 119.5 . . ? O5 C12 O6 124.1(3) . . ? O5 C12 C5 118.0(3) . . ? O6 C12 C5 117.8(3) . . ? O4 C13 O3 123.7(3) . . ? O4 C13 C14 119.0(3) . . ? O3 C13 C14 117.3(3) . . ? C15 C14 C19 118.7(3) . . ? C15 C14 C13 116.7(3) . . ? C19 C14 C13 124.6(3) . . ? C14 C15 C16 121.7(3) . . ? C14 C15 H15A 119.1 . . ? C16 C15 H15A 119.1 . . ? C17 C16 C15 121.6(3) . . ? C17 C16 H16A 119.2 . . ? C15 C16 H16A 119.2 . . ? C16 C17 C18 119.5(3) . . ? C16 C17 C24 116.1(3) . . ? C18 C17 C24 124.3(3) . . ? C23 C18 C17 122.7(3) . . ? C23 C18 C19 118.8(3) . . ? C17 C18 C19 118.6(3) . . ? C20 C19 C14 122.4(3) . . ? C20 C19 C18 117.7(3) . . ? C14 C19 C18 119.8(3) . . ? C21 C20 C19 121.3(3) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 120.6(3) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C18 121.3(3) . . ? C22 C23 H23A 119.3 . . ? C18 C23 H23A 119.3 . . ? O7 C24 O8 124.9(3) . . ? O7 C24 C17 114.7(3) . . ? O8 C24 C17 120.3(3) . . ? O9 C25 O10 125.3(3) . . ? O9 C25 C26 119.6(3) . . ? O10 C25 C26 115.1(3) . . ? C27 C26 C31 118.6(3) . . ? C27 C26 C25 118.8(3) . . ? C31 C26 C25 122.4(3) . . ? C26 C27 C28 121.2(3) . . ? C26 C27 H27A 119.4 . . ? C28 C27 H27A 119.4 . . ? C29 C28 C27 121.1(3) . . ? C29 C28 H28A 119.5 . . ? C27 C28 H28A 119.5 . . ? C28 C29 C30 119.5(3) . . ? C28 C29 C36 119.4(3) . . ? C30 C29 C36 120.9(3) . . ? C31 C30 C35 120.0(3) . . ? C31 C30 C29 118.5(3) . . ? C35 C30 C29 121.5(3) . . ? C30 C31 C26 120.4(3) . . ? C30 C31 C32 118.5(3) . . ? C26 C31 C32 121.0(3) . . ? C33 C32 C31 119.8(4) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C32 C33 C34 121.1(4) . . ? C32 C33 H33A 119.4 . . ? C34 C33 H33A 119.4 . . ? C35 C34 C33 121.5(4) . . ? C35 C34 H34A 119.3 . . ? C33 C34 H34A 119.3 . . ? C34 C35 C30 119.1(4) . . ? C34 C35 H35A 120.5 . . ? C30 C35 H35A 120.5 . . ? O12 C36 O11 121.0(3) . . ? O12 C36 C29 118.8(3) . . ? O11 C36 C29 120.2(3) . . ? O12 C36 Nd2 50.00(17) . 2 ? O11 C36 Nd2 71.51(19) . 2 ? C29 C36 Nd2 167.8(2) . 2 ? C39A N1A C37A 107.7(8) . . ? C39A N1A C40A 126.4(8) . . ? C37A N1A C40A 125.8(7) . . ? C38A N2A C39A 110.3(7) . . ? C38A N2A C41A 124.6(8) . . ? C39A N2A C41A 124.9(7) . . ? N1A C37A C38A 107.2(8) . . ? N1A C37A H37A 126.4 . . ? C38A C37A H37A 126.4 . . ? N2A C38A C37A 105.1(7) . . ? N2A C38A H38A 127.4 . . ? C37A C38A H38A 127.4 . . ? N1A C39A N2A 109.7(7) . . ? N1A C39A H39A 125.1 . . ? N2A C39A H39A 125.1 . . ? N2A C41A C42A 115.2(9) . . ? N2A C41A H41A 108.5 . . ? C42A C41A H41A 108.5 . . ? N2A C41A H41B 108.5 . . ? C42A C41A H41B 108.5 . . ? H41A C41A H41B 107.5 . . ? C44A C43A C42A 97.2(8) . . ? C44A C43A H43A 112.3 . . ? C42A C43A H43A 112.3 . . ? C44A C43A H43B 112.3 . . ? C42A C43A H43B 112.3 . . ? H43A C43A H43B 109.9 . . ? C41A C42A C43A 95.2(9) . . ? C41A C42A H42A 112.7 . . ? C43A C42A H42A 112.7 . . ? C41A C42A H42B 112.7 . . ? C43A C42A H42B 112.7 . . ? H42A C42A H42B 110.2 . . ? C45A C44A C43A 115.7(10) . . ? C45A C44A H44A 108.4 . . ? C43A C44A H44A 108.4 . . ? C45A C44A H44B 108.4 . . ? C43A C44A H44B 108.4 . . ? H44A C44A H44B 107.4 . . ? C44A C45A C46A 114.1(10) . . ? C44A C45A H45A 108.7 . . ? C46A C45A H45A 108.7 . . ? C44A C45A H45D 108.7 . . ? C46A C45A H45D 108.7 . . ? H45A C45A H45D 107.6 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C38B N2B C39B 108.5(8) . . ? C38B N2B C41B 128.5(12) . . ? C39B N2B C41B 122.5(9) . . ? C39B N1B C37B 106.5(13) . . ? C39B N1B C40B 121.7(12) . . ? C37B N1B C40B 131.8(10) . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N1B C37B C38B 108.0(13) . . ? N1B C37B H37B 126.0 . . ? C38B C37B H37B 126.0 . . ? N2B C38B C37B 105.6(10) . . ? N2B C38B H38B 127.2 . . ? C37B C38B H38B 127.2 . . ? N2B C41B C42B 113.7(16) . . ? N2B C41B H41C 108.8 . . ? C42B C41B H41C 108.8 . . ? N2B C41B H41D 108.8 . . ? C42B C41B H41D 108.8 . . ? H41C C41B H41D 107.7 . . ? C41B C42B C43B 108.3(14) . . ? C41B C42B H42C 110.0 . . ? C43B C42B H42C 110.0 . . ? C41B C42B H42D 110.0 . . ? C43B C42B H42D 110.0 . . ? H42C C42B H42D 108.4 . . ? N1B C39B N2B 111.2(10) . . ? N1B C39B H39B 124.4 . . ? N2B C39B H39B 124.4 . . ? C45B C44B C43B 132.0(13) . . ? C45B C44B H44C 104.2 . . ? C43B C44B H44C 104.2 . . ? C45B C44B H44D 104.2 . . ? C43B C44B H44D 104.2 . . ? H44C C44B H44D 105.6 . . ? C44B C43B C42B 113.2(12) . . ? C44B C43B H43C 108.9 . . ? C42B C43B H43C 108.9 . . ? C44B C43B H43D 108.9 . . ? C42B C43B H43D 108.9 . . ? H43C C43B H43D 107.8 . . ? C44B C45B C46B 114.4(11) . . ? C44B C45B H45B 108.7 . . ? C46B C45B H45B 108.7 . . ? C44B C45B H45C 108.7 . . ? C46B C45B H45C 108.7 . . ? H45B C45B H45C 107.6 . . ? C45B C46B H46G 109.5 . . ? C45B C46B H46D 109.5 . . ? H46G C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46G C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Nd2 Cl1 Nd1 79.6(2) 4_565 . . . ? O4 Nd2 Cl1 Nd1 -24.45(7) . . . . ? O10 Nd2 Cl1 Nd1 129.98(7) 3 . . . ? O8 Nd2 Cl1 Nd1 52.13(6) 4_565 . . . ? O9 Nd2 Cl1 Nd1 -89.56(8) . . . . ? O12 Nd2 Cl1 Nd1 -142.22(8) 2_545 . . . ? O11 Nd2 Cl1 Nd1 -166.26(5) 2_545 . . . ? C36 Nd2 Cl1 Nd1 -152.27(7) 2_545 . . . ? O7 Nd1 Cl1 Nd2 -39.96(7) 4_565 . . . ? O1 Nd1 Cl1 Nd2 -48.87(18) . . . . ? O5 Nd1 Cl1 Nd2 113.35(8) 4_566 . . . ? O6 Nd1 Cl1 Nd2 -116.12(7) 2_644 . . . ? O3 Nd1 Cl1 Nd2 43.80(7) . . . . ? O2 Nd1 Cl1 Nd2 167.50(8) 3_655 . . . ? O7 Nd1 O1 C1 -154.0(4) 4_565 . . . ? O5 Nd1 O1 C1 49.7(4) 4_566 . . . ? O6 Nd1 O1 C1 -76.3(4) 2_644 . . . ? O3 Nd1 O1 C1 125.0(4) . . . . ? O2 Nd1 O1 C1 -8.9(5) 3_655 . . . ? Cl1 Nd1 O1 C1 -145.2(3) . . . . ? O7 Nd1 O3 C13 28.8(4) 4_565 . . . ? O1 Nd1 O3 C13 108.5(4) . . . . ? O5 Nd1 O3 C13 -175.8(4) 4_566 . . . ? O6 Nd1 O3 C13 24.3(6) 2_644 . . . ? O2 Nd1 O3 C13 -114.4(4) 3_655 . . . ? Cl1 Nd1 O3 C13 -48.3(4) . . . . ? O11 Nd2 O4 C13 157.8(4) 4_565 . . . ? O10 Nd2 O4 C13 -115.5(4) 3 . . . ? O8 Nd2 O4 C13 -124.3(4) 4_565 . . . ? O9 Nd2 O4 C13 87.7(4) . . . . ? O12 Nd2 O4 C13 25.2(4) 2_545 . . . ? Cl1 Nd2 O4 C13 -40.2(4) . . . . ? O11 Nd2 O4 C13 75.4(4) 2_545 . . . ? C36 Nd2 O4 C13 46.4(4) 2_545 . . . ? O11 Nd2 O9 C25 18.7(3) 4_565 . . . ? O4 Nd2 O9 C25 125.1(4) . . . . ? O10 Nd2 O9 C25 -41.6(4) 3 . . . ? O8 Nd2 O9 C25 77.4(4) 4_565 . . . ? O12 Nd2 O9 C25 -113.2(4) 2_545 . . . ? Cl1 Nd2 O9 C25 -164.8(3) . . . . ? O11 Nd2 O9 C25 -63.4(3) 2_545 . . . ? C36 Nd2 O9 C25 -89.6(4) 2_545 . . . ? Nd1 O1 C1 O2 -5.6(7) . . . . ? Nd1 O1 C1 C2 171.7(3) . . . . ? Nd1 O2 C1 O1 22.4(7) 3_655 . . . ? Nd1 O2 C1 C2 -154.8(3) 3_655 . . . ? O1 C1 C2 C3 -41.1(5) . . . . ? O2 C1 C2 C3 136.4(4) . . . . ? O1 C1 C2 C7 139.2(4) . . . . ? O2 C1 C2 C7 -43.3(5) . . . . ? C7 C2 C3 C4 1.0(6) . . . . ? C1 C2 C3 C4 -178.7(3) . . . . ? C2 C3 C4 C5 1.0(6) . . . . ? C3 C4 C5 C6 -3.4(6) . . . . ? C3 C4 C5 C12 174.7(3) . . . . ? C4 C5 C6 C11 -174.0(4) . . . . ? C12 C5 C6 C11 8.0(5) . . . . ? C4 C5 C6 C7 3.8(5) . . . . ? C12 C5 C6 C7 -174.2(3) . . . . ? C11 C6 C7 C8 -2.5(5) . . . . ? C5 C6 C7 C8 179.7(3) . . . . ? C11 C6 C7 C2 176.0(3) . . . . ? C5 C6 C7 C2 -1.9(5) . . . . ? C3 C2 C7 C8 177.9(3) . . . . ? C1 C2 C7 C8 -2.4(5) . . . . ? C3 C2 C7 C6 -0.5(5) . . . . ? C1 C2 C7 C6 179.2(3) . . . . ? C6 C7 C8 C9 1.6(5) . . . . ? C2 C7 C8 C9 -176.8(4) . . . . ? C7 C8 C9 C10 0.5(6) . . . . ? C8 C9 C10 C11 -1.7(6) . . . . ? C9 C10 C11 C6 0.7(6) . . . . ? C7 C6 C11 C10 1.4(5) . . . . ? C5 C6 C11 C10 179.2(4) . . . . ? Nd1 O5 C12 O6 27.2(13) 4_565 . . . ? Nd1 O5 C12 C5 -150.1(8) 4_565 . . . ? Nd1 O6 C12 O5 1.6(5) 2_654 . . . ? Nd1 O6 C12 C5 178.9(2) 2_654 . . . ? C4 C5 C12 O5 35.5(5) . . . . ? C6 C5 C12 O5 -146.4(4) . . . . ? C4 C5 C12 O6 -141.9(4) . . . . ? C6 C5 C12 O6 36.1(5) . . . . ? Nd2 O4 C13 O3 64.9(6) . . . . ? Nd2 O4 C13 C14 -112.0(4) . . . . ? Nd1 O3 C13 O4 4.8(6) . . . . ? Nd1 O3 C13 C14 -178.3(2) . . . . ? O4 C13 C14 C15 143.8(4) . . . . ? O3 C13 C14 C15 -33.3(5) . . . . ? O4 C13 C14 C19 -34.4(5) . . . . ? O3 C13 C14 C19 148.6(4) . . . . ? C19 C14 C15 C16 0.8(6) . . . . ? C13 C14 C15 C16 -177.4(3) . . . . ? C14 C15 C16 C17 1.4(6) . . . . ? C15 C16 C17 C18 -1.7(6) . . . . ? C15 C16 C17 C24 179.9(3) . . . . ? C16 C17 C18 C23 -178.4(3) . . . . ? C24 C17 C18 C23 -0.2(5) . . . . ? C16 C17 C18 C19 -0.1(5) . . . . ? C24 C17 C18 C19 178.1(3) . . . . ? C15 C14 C19 C20 174.9(3) . . . . ? C13 C14 C19 C20 -7.0(5) . . . . ? C15 C14 C19 C18 -2.6(5) . . . . ? C13 C14 C19 C18 175.5(3) . . . . ? C23 C18 C19 C20 3.0(5) . . . . ? C17 C18 C19 C20 -175.4(3) . . . . ? C23 C18 C19 C14 -179.4(3) . . . . ? C17 C18 C19 C14 2.2(5) . . . . ? C14 C19 C20 C21 -179.5(4) . . . . ? C18 C19 C20 C21 -2.0(5) . . . . ? C19 C20 C21 C22 0.2(6) . . . . ? C20 C21 C22 C23 0.6(6) . . . . ? C21 C22 C23 C18 0.5(6) . . . . ? C17 C18 C23 C22 175.9(3) . . . . ? C19 C18 C23 C22 -2.4(5) . . . . ? Nd1 O7 C24 O8 8.8(10) 4_566 . . . ? Nd1 O7 C24 C17 -169.9(6) 4_566 . . . ? Nd2 O8 C24 O7 -31.6(5) 4_566 . . . ? Nd2 O8 C24 C17 147.0(2) 4_566 . . . ? C16 C17 C24 O7 33.1(4) . . . . ? C18 C17 C24 O7 -145.1(3) . . . . ? C16 C17 C24 O8 -145.6(3) . . . . ? C18 C17 C24 O8 36.2(5) . . . . ? Nd2 O9 C25 O10 28.8(6) . . . . ? Nd2 O9 C25 C26 -153.4(2) . . . . ? Nd2 O10 C25 O9 2.6(6) 3 . . . ? Nd2 O10 C25 C26 -175.3(2) 3 . . . ? O9 C25 C26 C27 -49.0(5) . . . . ? O10 C25 C26 C27 129.0(4) . . . . ? O9 C25 C26 C31 136.8(4) . . . . ? O10 C25 C26 C31 -45.1(5) . . . . ? C31 C26 C27 C28 5.3(6) . . . . ? C25 C26 C27 C28 -169.1(4) . . . . ? C26 C27 C28 C29 1.1(6) . . . . ? C27 C28 C29 C30 -7.9(6) . . . . ? C27 C28 C29 C36 167.8(4) . . . . ? C28 C29 C30 C31 8.1(5) . . . . ? C36 C29 C30 C31 -167.5(3) . . . . ? C28 C29 C30 C35 -170.8(4) . . . . ? C36 C29 C30 C35 13.6(5) . . . . ? C35 C30 C31 C26 177.1(3) . . . . ? C29 C30 C31 C26 -1.8(5) . . . . ? C35 C30 C31 C32 1.0(5) . . . . ? C29 C30 C31 C32 -178.0(3) . . . . ? C27 C26 C31 C30 -4.8(5) . . . . ? C25 C26 C31 C30 169.4(3) . . . . ? C27 C26 C31 C32 171.3(3) . . . . ? C25 C26 C31 C32 -14.6(5) . . . . ? C30 C31 C32 C33 -0.5(6) . . . . ? C26 C31 C32 C33 -176.7(4) . . . . ? C31 C32 C33 C34 0.9(7) . . . . ? C32 C33 C34 C35 -1.7(7) . . . . ? C33 C34 C35 C30 2.1(7) . . . . ? C31 C30 C35 C34 -1.7(6) . . . . ? C29 C30 C35 C34 177.2(4) . . . . ? Nd2 O12 C36 O11 9.5(4) 2 . . . ? Nd2 O12 C36 C29 -174.3(3) 2 . . . ? Nd2 O11 C36 O12 -120.2(6) 4_566 . . . ? Nd2 O11 C36 O12 -7.7(3) 2 . . . ? Nd2 O11 C36 C29 63.7(8) 4_566 . . . ? Nd2 O11 C36 C29 176.2(3) 2 . . . ? Nd2 O11 C36 Nd2 -112.5(7) 4_566 . . 2 ? C28 C29 C36 O12 -133.6(4) . . . . ? C30 C29 C36 O12 42.1(5) . . . . ? C28 C29 C36 O11 42.6(5) . . . . ? C30 C29 C36 O11 -141.7(3) . . . . ? C28 C29 C36 Nd2 -154.7(10) . . . 2 ? C30 C29 C36 Nd2 21.0(14) . . . 2 ? C39A N1A C37A C38A 0.8(14) . . . . ? C40A N1A C37A C38A 178.2(12) . . . . ? C39A N2A C38A C37A -0.6(17) . . . . ? C41A N2A C38A C37A 175.0(14) . . . . ? N1A C37A C38A N2A -0.1(14) . . . . ? C37A N1A C39A N2A -1.1(18) . . . . ? C40A N1A C39A N2A -178.6(14) . . . . ? C38A N2A C39A N1A 1(2) . . . . ? C41A N2A C39A N1A -174.5(15) . . . . ? C38A N2A C41A C42A -4(2) . . . . ? C39A N2A C41A C42A 171.1(16) . . . . ? N2A C41A C42A C43A -78.9(14) . . . . ? C44A C43A C42A C41A -164.4(9) . . . . ? C42A C43A C44A C45A -92.5(13) . . . . ? C43A C44A C45A C46A -126.5(14) . . . . ? C39B N1B C37B C38B -3(2) . . . . ? C40B N1B C37B C38B 176(2) . . . . ? C39B N2B C38B C37B -4(3) . . . . ? C41B N2B C38B C37B -177(2) . . . . ? N1B C37B C38B N2B 4(2) . . . . ? C38B N2B C41B C42B -89(3) . . . . ? C39B N2B C41B C42B 99(3) . . . . ? N2B C41B C42B C43B 95.2(18) . . . . ? C37B N1B C39B N2B 0(3) . . . . ? C40B N1B C39B N2B -179(2) . . . . ? C38B N2B C39B N1B 3(3) . . . . ? C41B N2B C39B N1B 176(2) . . . . ? C45B C44B C43B C42B -161(2) . . . . ? C41B C42B C43B C44B -147.2(17) . . . . ? C43B C44B C45B C46B 1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.998 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.099 #===END data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 876525' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Sm2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl N2 O12 Sm2' _chemical_formula_weight 1145.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.8177(4) _cell_length_b 14.8107(3) _cell_length_c 15.9935(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.176(2) _cell_angle_gamma 90.00 _cell_volume 4203.38(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12327 _cell_measurement_theta_min 2.5199 _cell_measurement_theta_max 28.8748 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 2.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80679 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17852 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8726 _reflns_number_gt 7079 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0336P)^2^+22.9541P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8726 _refine_ls_number_parameters 607 _refine_ls_number_restraints 373 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.033 _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 Sm1 Sm 0.378008(12) 0.024810(15) -0.005075(13) 0.01329(7) Uani 1 1 d . . . Sm2 Sm 0.115786(12) 0.012169(15) -0.001149(14) 0.01425(7) Uani 1 1 d . . . Cl1 Cl 0.25198(7) -0.08503(9) 0.02344(9) 0.0296(3) Uani 1 1 d . . . O1 O 0.4492(2) 0.1269(3) -0.0775(3) 0.0378(10) Uani 1 1 d . . . O2 O 0.5735(2) 0.1085(3) -0.0627(3) 0.0382(10) Uani 1 1 d . . . O3 O 0.3152(2) 0.1309(3) 0.0739(3) 0.0399(11) Uani 1 1 d . . . O5 O 0.4718(2) 0.4309(3) -0.4002(3) 0.0406(11) Uani 1 1 d . . . O4 O 0.1936(2) 0.1358(2) 0.0303(2) 0.0298(9) Uani 1 1 d . . . O6 O 0.5957(2) 0.4321(3) -0.3811(2) 0.0390(10) Uani 1 1 d . . . O7 O 0.2867(2) 0.4302(3) 0.3891(2) 0.0314(9) Uani 1 1 d . . . O8 O 0.1629(2) 0.4519(3) 0.3674(2) 0.0264(8) Uani 1 1 d . . . O9 O 0.0621(2) 0.0927(3) 0.1102(2) 0.0325(9) Uani 1 1 d . . . O10 O -0.0628(2) 0.1028(3) 0.0880(2) 0.0333(9) Uani 1 1 d . . . O11 O 0.0115(2) 0.4133(3) 0.4347(2) 0.0332(9) Uani 1 1 d . . . O12 O -0.1077(2) 0.4065(3) 0.3866(3) 0.0403(11) Uani 1 1 d . . . C1 C 0.5143(3) 0.1462(3) -0.0929(3) 0.0257(11) Uani 1 1 d . . . C2 C 0.5221(3) 0.2198(3) -0.1575(3) 0.0226(11) Uani 1 1 d . . . C3 C 0.4715(3) 0.2181(4) -0.2269(4) 0.0313(13) Uani 1 1 d . . . H3A H 0.4340 0.1742 -0.2318 0.038 Uiso 1 1 calc R . . C4 C 0.4759(3) 0.2826(4) -0.2915(3) 0.0306(13) Uani 1 1 d . . . H4A H 0.4414 0.2801 -0.3387 0.037 Uiso 1 1 calc R . . C5 C 0.5294(3) 0.3481(3) -0.2861(3) 0.0224(11) Uani 1 1 d . . . C6 C 0.5817(3) 0.3545(3) -0.2123(3) 0.0212(10) Uani 1 1 d . . . C7 C 0.5782(3) 0.2884(3) -0.1484(3) 0.0211(10) Uani 1 1 d . . . C8 C 0.6300(3) 0.2952(4) -0.0758(3) 0.0302(12) Uani 1 1 d . . . H8A H 0.6293 0.2518 -0.0339 0.036 Uiso 1 1 calc R . . C9 C 0.6808(3) 0.3640(4) -0.0664(4) 0.0391(15) Uani 1 1 d . . . H9A H 0.7143 0.3673 -0.0184 0.047 Uiso 1 1 calc R . . C10 C 0.6824(3) 0.4304(4) -0.1295(4) 0.0386(14) Uani 1 1 d . . . H10A H 0.7167 0.4777 -0.1225 0.046 Uiso 1 1 calc R . . C11 C 0.6345(3) 0.4259(4) -0.2004(3) 0.0299(12) Uani 1 1 d . . . H11A H 0.6363 0.4702 -0.2414 0.036 Uiso 1 1 calc R . . C12 C 0.5328(3) 0.4085(4) -0.3610(3) 0.0273(12) Uani 1 1 d . . . C13 C 0.2500(3) 0.1629(4) 0.0760(3) 0.0260(11) Uani 1 1 d . . . C14 C 0.2396(3) 0.2347(4) 0.1406(3) 0.0245(11) Uani 1 1 d . . . C15 C 0.2827(3) 0.2278(4) 0.2155(4) 0.0353(14) Uani 1 1 d . . . H15A H 0.3174 0.1809 0.2229 0.042 Uiso 1 1 calc R . . C16 C 0.2765(3) 0.2887(4) 0.2814(4) 0.0350(14) Uani 1 1 d . . . H16A H 0.3075 0.2823 0.3310 0.042 Uiso 1 1 calc R . . C17 C 0.2254(3) 0.3573(3) 0.2736(3) 0.0217(10) Uani 1 1 d . . . C18 C 0.1779(3) 0.3681(3) 0.1972(3) 0.0192(10) Uani 1 1 d . . . C19 C 0.1866(3) 0.3068(3) 0.1284(3) 0.0208(10) Uani 1 1 d . . . C20 C 0.1434(3) 0.3228(4) 0.0516(3) 0.0310(13) Uani 1 1 d . . . H20A H 0.1489 0.2847 0.0064 0.037 Uiso 1 1 calc R . . C21 C 0.0938(4) 0.3926(4) 0.0421(4) 0.0382(14) Uani 1 1 d . . . H21A H 0.0661 0.4015 -0.0094 0.046 Uiso 1 1 calc R . . C22 C 0.0841(3) 0.4508(4) 0.1088(4) 0.0341(13) Uani 1 1 d . . . H22A H 0.0500 0.4983 0.1016 0.041 Uiso 1 1 calc R . . C23 C 0.1243(3) 0.4387(3) 0.1843(3) 0.0256(11) Uani 1 1 d . . . H23A H 0.1165 0.4775 0.2284 0.031 Uiso 1 1 calc R . . C24 C 0.2243(3) 0.4186(3) 0.3495(3) 0.0211(10) Uani 1 1 d . . . C25 C 0.0001(3) 0.1284(4) 0.1216(3) 0.0276(12) Uani 1 1 d . . . C26 C -0.0006(3) 0.2068(4) 0.1807(3) 0.0255(11) Uani 1 1 d . . . C27 C 0.0385(3) 0.1997(4) 0.2574(4) 0.0336(13) Uani 1 1 d . . . H27A H 0.0721 0.1521 0.2680 0.040 Uiso 1 1 calc R . . C28 C 0.0288(3) 0.2635(4) 0.3216(3) 0.0340(13) Uani 1 1 d . . . H28A H 0.0562 0.2577 0.3736 0.041 Uiso 1 1 calc R . . C29 C -0.0200(3) 0.3327(4) 0.3073(3) 0.0259(11) Uani 1 1 d . . . C30 C -0.0560(3) 0.3486(4) 0.2253(3) 0.0250(11) Uani 1 1 d . . . C31 C -0.0469(3) 0.2840(4) 0.1604(3) 0.0256(11) Uani 1 1 d . . . C32 C -0.0811(4) 0.3007(4) 0.0790(4) 0.0373(14) Uani 1 1 d . . . H32A H -0.0767 0.2582 0.0369 0.045 Uiso 1 1 calc R . . C33 C -0.1204(4) 0.3777(5) 0.0611(4) 0.0490(17) Uani 1 1 d . . . H33A H -0.1414 0.3885 0.0067 0.059 Uiso 1 1 calc R . . C34 C -0.1295(4) 0.4411(5) 0.1243(5) 0.0495(17) Uani 1 1 d . . . H34A H -0.1569 0.4934 0.1113 0.059 Uiso 1 1 calc R . . C35 C -0.0992(4) 0.4275(4) 0.2043(4) 0.0394(14) Uani 1 1 d . . . H35A H -0.1066 0.4701 0.2456 0.047 Uiso 1 1 calc R . . C36 C -0.0398(3) 0.3887(4) 0.3803(3) 0.0283(12) Uani 1 1 d . . . N1A N 0.2364(8) -0.2677(8) 0.2794(7) 0.0592(18) Uani 0.603(8) 1 d PDU A 1 N2A N 0.3046(10) -0.1470(10) 0.2685(10) 0.0675(17) Uani 0.603(8) 1 d PDU A 1 C37A C 0.2867(8) -0.2662(9) 0.3464(8) 0.057(2) Uani 0.603(8) 1 d PDU A 1 H37A H 0.2912 -0.3077 0.3903 0.068 Uiso 0.603(8) 1 calc PR A 1 C38A C 0.3326(9) -0.1881(10) 0.3373(8) 0.066(2) Uani 0.603(8) 1 d PDU A 1 H38A H 0.3739 -0.1699 0.3729 0.079 Uiso 0.603(8) 1 calc PR A 1 C39A C 0.2525(12) -0.2034(12) 0.2276(12) 0.0576(18) Uani 0.603(8) 1 d PDU A 1 H39A H 0.2320 -0.1971 0.1723 0.069 Uiso 0.603(8) 1 calc PR A 1 C40A C 0.1810(8) -0.3377(9) 0.2564(10) 0.077(3) Uani 0.603(8) 1 d PDU A 1 H40A H 0.1376 -0.3112 0.2259 0.116 Uiso 0.603(8) 1 calc PR A 1 H40B H 0.1663 -0.3662 0.3062 0.116 Uiso 0.603(8) 1 calc PR A 1 H40C H 0.2026 -0.3819 0.2218 0.116 Uiso 0.603(8) 1 calc PR A 1 C41A C 0.3274(10) -0.0583(10) 0.2352(10) 0.091(2) Uani 0.603(8) 1 d PDU A 1 H41A H 0.2842 -0.0183 0.2282 0.109 Uiso 0.603(8) 1 calc PR A 1 H41B H 0.3467 -0.0664 0.1809 0.109 Uiso 0.603(8) 1 calc PR A 1 C43A C 0.3316(10) 0.0268(13) 0.3556(12) 0.123(3) Uani 0.603(8) 1 d PDU A 1 H43A H 0.2874 0.0487 0.3217 0.148 Uiso 0.603(8) 1 calc PR A 1 H43B H 0.3156 -0.0177 0.3948 0.148 Uiso 0.603(8) 1 calc PR A 1 C42A C 0.3888(10) -0.0169(13) 0.2977(11) 0.111(2) Uani 0.603(8) 1 d PDU A 1 H42A H 0.4193 0.0276 0.2720 0.133 Uiso 0.603(8) 1 calc PR A 1 H42B H 0.4207 -0.0622 0.3267 0.133 Uiso 0.603(8) 1 calc PR A 1 C44A C 0.3727(13) 0.1069(11) 0.4042(10) 0.137(3) Uani 0.603(8) 1 d PDU A 1 H44A H 0.4006 0.1405 0.3652 0.165 Uiso 0.603(8) 1 calc PR A 1 H44B H 0.3348 0.1471 0.4233 0.165 Uiso 0.603(8) 1 calc PR A 1 C45A C 0.4271(11) 0.0808(15) 0.4801(12) 0.145(3) Uani 0.603(8) 1 d PDU A 1 H45A H 0.4781 0.0922 0.4663 0.174 Uiso 0.603(8) 1 calc PR A 1 H45D H 0.4226 0.0164 0.4894 0.174 Uiso 0.603(8) 1 calc PR A 1 C46A C 0.4153(17) 0.1302(18) 0.5628(11) 0.168(5) Uani 0.603(8) 1 d PDU A 1 H46A H 0.4494 0.1062 0.6072 0.251 Uiso 0.603(8) 1 calc PR A 1 H46B H 0.3643 0.1215 0.5762 0.251 Uiso 0.603(8) 1 calc PR A 1 H46C H 0.4248 0.1935 0.5564 0.251 Uiso 0.603(8) 1 calc PR A 1 N2B N 0.3090(15) -0.1655(15) 0.2736(15) 0.0675(17) Uani 0.397(8) 1 d PDU A 2 N1B N 0.2256(12) -0.2714(12) 0.2512(11) 0.0592(18) Uani 0.397(8) 1 d PDU A 2 C40B C 0.1680(12) -0.3193(15) 0.2003(13) 0.077(3) Uani 0.397(8) 1 d PDU A 2 H40D H 0.1606 -0.2913 0.1460 0.116 Uiso 0.397(8) 1 calc PR A 2 H40E H 0.1218 -0.3176 0.2268 0.116 Uiso 0.397(8) 1 calc PR A 2 H40F H 0.1833 -0.3809 0.1940 0.116 Uiso 0.397(8) 1 calc PR A 2 C37B C 0.2572(13) -0.2854(13) 0.3285(12) 0.057(2) Uani 0.397(8) 1 d PDU A 2 H37B H 0.2455 -0.3302 0.3659 0.068 Uiso 0.397(8) 1 calc PR A 2 C38B C 0.3133(14) -0.2163(15) 0.3415(12) 0.066(2) Uani 0.397(8) 1 d PDU A 2 H38B H 0.3466 -0.2086 0.3892 0.079 Uiso 0.397(8) 1 calc PR A 2 C41B C 0.3559(13) -0.0866(13) 0.2521(17) 0.091(2) Uani 0.397(8) 1 d PDU A 2 H41C H 0.3481 -0.0806 0.1916 0.109 Uiso 0.397(8) 1 calc PR A 2 H41D H 0.4078 -0.1057 0.2644 0.109 Uiso 0.397(8) 1 calc PR A 2 C42B C 0.352(2) 0.0102(16) 0.2870(14) 0.111(2) Uani 0.397(8) 1 d PDU A 2 H42C H 0.2997 0.0277 0.2837 0.133 Uiso 0.397(8) 1 calc PR A 2 H42D H 0.3768 0.0497 0.2494 0.133 Uiso 0.397(8) 1 calc PR A 2 C39B C 0.2466(19) -0.1932(18) 0.2234(18) 0.0576(18) Uani 0.397(8) 1 d PDU A 2 H39B H 0.2233 -0.1618 0.1778 0.069 Uiso 0.397(8) 1 calc PR A 2 C44B C 0.3345(14) 0.077(2) 0.4377(16) 0.137(3) Uani 0.397(8) 1 d PDU A 2 H44C H 0.2936 0.1051 0.4027 0.165 Uiso 0.397(8) 1 calc PR A 2 H44D H 0.3124 0.0302 0.4700 0.165 Uiso 0.397(8) 1 calc PR A 2 C43B C 0.3873(15) 0.030(2) 0.3784(15) 0.123(3) Uani 0.397(8) 1 d PDU A 2 H43C H 0.4044 -0.0263 0.4040 0.148 Uiso 0.397(8) 1 calc PR A 2 H43D H 0.4313 0.0682 0.3750 0.148 Uiso 0.397(8) 1 calc PR A 2 C45B C 0.3677(17) 0.149(2) 0.500(2) 0.145(3) Uani 0.397(8) 1 d PDU A 2 H45B H 0.3444 0.1421 0.5519 0.174 Uiso 0.397(8) 1 calc PR A 2 H45C H 0.3541 0.2079 0.4772 0.174 Uiso 0.397(8) 1 calc PR A 2 C46B C 0.4545(17) 0.146(3) 0.520(2) 0.168(5) Uani 0.397(8) 1 d PDU A 2 H46G H 0.4701 0.1940 0.5572 0.251 Uiso 0.397(8) 1 calc PR A 2 H46D H 0.4784 0.1519 0.4686 0.251 Uiso 0.397(8) 1 calc PR A 2 H46E H 0.4686 0.0889 0.5457 0.251 Uiso 0.397(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01295(12) 0.01429(12) 0.01251(12) 0.00033(8) 0.00057(8) 0.00057(9) Sm2 0.01368(12) 0.01538(12) 0.01360(12) -0.00032(9) 0.00075(8) -0.00104(9) Cl1 0.0163(6) 0.0263(6) 0.0466(8) 0.0136(6) 0.0048(5) 0.0025(5) O1 0.026(2) 0.039(2) 0.048(3) 0.022(2) 0.0041(18) -0.0045(18) O2 0.026(2) 0.031(2) 0.058(3) 0.024(2) -0.0016(18) 0.0051(17) O3 0.024(2) 0.040(2) 0.055(3) -0.030(2) 0.0037(18) 0.0065(18) O5 0.035(2) 0.049(3) 0.034(2) 0.0197(19) -0.0144(18) -0.001(2) O4 0.024(2) 0.0253(19) 0.040(2) -0.0171(16) 0.0015(16) -0.0072(15) O6 0.036(2) 0.051(3) 0.030(2) 0.0205(19) 0.0037(17) -0.010(2) O7 0.0197(19) 0.049(2) 0.0253(19) -0.0178(17) -0.0020(15) -0.0017(17) O8 0.0234(19) 0.038(2) 0.0176(17) -0.0065(15) 0.0011(14) 0.0080(16) O9 0.025(2) 0.041(2) 0.033(2) -0.0183(18) 0.0089(16) -0.0023(17) O10 0.025(2) 0.037(2) 0.039(2) -0.0211(18) 0.0082(16) -0.0106(17) O11 0.032(2) 0.040(2) 0.027(2) -0.0130(17) 0.0005(16) -0.0171(18) O12 0.022(2) 0.058(3) 0.042(2) -0.028(2) 0.0119(17) -0.0069(19) C1 0.023(3) 0.024(3) 0.030(3) 0.010(2) 0.003(2) -0.002(2) C2 0.017(2) 0.022(3) 0.029(3) 0.013(2) 0.000(2) 0.000(2) C3 0.019(3) 0.035(3) 0.038(3) 0.011(2) -0.006(2) -0.008(2) C4 0.025(3) 0.035(3) 0.030(3) 0.016(2) -0.009(2) -0.005(2) C5 0.019(2) 0.028(3) 0.020(2) 0.012(2) 0.0018(19) 0.000(2) C6 0.016(2) 0.024(3) 0.023(3) 0.007(2) 0.0015(19) -0.0002(19) C7 0.015(2) 0.027(3) 0.022(2) 0.005(2) 0.0003(18) 0.000(2) C8 0.025(3) 0.037(3) 0.027(3) 0.013(2) -0.004(2) -0.004(2) C9 0.038(3) 0.052(4) 0.025(3) 0.001(3) -0.010(2) -0.011(3) C10 0.038(3) 0.041(3) 0.037(3) -0.003(3) -0.003(3) -0.019(3) C11 0.034(3) 0.029(3) 0.027(3) 0.006(2) 0.004(2) -0.008(2) C12 0.031(3) 0.027(3) 0.024(3) 0.011(2) -0.003(2) -0.003(2) C13 0.021(3) 0.027(3) 0.030(3) -0.007(2) 0.003(2) -0.004(2) C14 0.018(3) 0.028(3) 0.028(3) -0.009(2) 0.005(2) -0.002(2) C15 0.026(3) 0.035(3) 0.043(3) -0.019(3) -0.005(2) 0.015(2) C16 0.029(3) 0.041(3) 0.032(3) -0.013(3) -0.010(2) 0.013(3) C17 0.016(2) 0.027(3) 0.022(3) -0.008(2) -0.0005(19) 0.000(2) C18 0.016(2) 0.021(2) 0.020(2) -0.0040(19) 0.0015(18) -0.0017(19) C19 0.017(2) 0.022(2) 0.023(2) -0.008(2) 0.0011(19) -0.0033(19) C20 0.040(3) 0.034(3) 0.018(3) -0.008(2) -0.003(2) 0.000(3) C21 0.043(4) 0.044(4) 0.025(3) -0.001(3) -0.012(2) 0.007(3) C22 0.037(3) 0.031(3) 0.033(3) 0.001(2) -0.004(2) 0.011(3) C23 0.026(3) 0.024(3) 0.027(3) -0.004(2) 0.002(2) 0.005(2) C24 0.018(2) 0.027(3) 0.018(2) -0.0034(19) -0.0011(18) 0.000(2) C25 0.031(3) 0.031(3) 0.022(3) -0.006(2) 0.007(2) -0.009(2) C26 0.020(3) 0.029(3) 0.028(3) -0.010(2) 0.006(2) -0.006(2) C27 0.032(3) 0.036(3) 0.031(3) -0.014(2) -0.001(2) 0.006(3) C28 0.032(3) 0.044(3) 0.024(3) -0.015(2) -0.007(2) 0.002(3) C29 0.021(3) 0.029(3) 0.028(3) -0.012(2) 0.006(2) -0.007(2) C30 0.025(3) 0.025(3) 0.026(3) -0.007(2) 0.007(2) -0.005(2) C31 0.023(3) 0.029(3) 0.025(3) -0.008(2) 0.003(2) -0.010(2) C32 0.042(4) 0.041(3) 0.028(3) -0.003(3) -0.001(3) -0.009(3) C33 0.052(4) 0.057(4) 0.036(4) 0.008(3) -0.007(3) -0.005(3) C34 0.046(4) 0.045(4) 0.057(4) 0.014(3) 0.003(3) 0.010(3) C35 0.040(4) 0.031(3) 0.049(4) -0.002(3) 0.010(3) 0.001(3) C36 0.029(3) 0.027(3) 0.030(3) -0.012(2) 0.007(2) -0.012(2) N1A 0.070(4) 0.052(3) 0.058(4) 0.014(3) 0.023(3) 0.019(3) N2A 0.086(3) 0.065(4) 0.054(3) 0.007(3) 0.017(3) 0.008(3) C37A 0.074(4) 0.050(4) 0.048(4) 0.016(3) 0.012(4) 0.019(4) C38A 0.084(4) 0.063(4) 0.052(3) 0.012(4) 0.013(3) 0.014(4) C39A 0.070(4) 0.054(4) 0.051(3) 0.014(3) 0.015(3) 0.009(3) C40A 0.074(6) 0.054(6) 0.112(8) 0.008(7) 0.055(7) 0.014(5) C41A 0.113(4) 0.079(4) 0.084(4) 0.012(4) 0.022(4) -0.007(4) C43A 0.155(5) 0.106(5) 0.113(5) 0.017(4) 0.035(5) -0.006(5) C42A 0.139(5) 0.095(4) 0.103(4) 0.014(4) 0.031(4) -0.001(4) C44A 0.169(5) 0.116(5) 0.130(5) 0.023(5) 0.032(5) -0.012(5) C45A 0.177(6) 0.122(6) 0.139(6) 0.020(6) 0.030(6) -0.016(6) C46A 0.204(10) 0.143(9) 0.161(10) 0.005(9) 0.046(9) -0.019(9) N2B 0.086(3) 0.065(4) 0.054(3) 0.007(3) 0.017(3) 0.008(3) N1B 0.070(4) 0.052(3) 0.058(4) 0.014(3) 0.023(3) 0.019(3) C40B 0.074(6) 0.054(6) 0.112(8) 0.008(7) 0.055(7) 0.014(5) C37B 0.074(4) 0.050(4) 0.048(4) 0.016(3) 0.012(4) 0.019(4) C38B 0.084(4) 0.063(4) 0.052(3) 0.012(4) 0.013(3) 0.014(4) C41B 0.113(4) 0.079(4) 0.084(4) 0.012(4) 0.022(4) -0.007(4) C42B 0.139(5) 0.095(4) 0.103(4) 0.014(4) 0.031(4) -0.001(4) C39B 0.070(4) 0.054(4) 0.051(3) 0.014(3) 0.015(3) 0.009(3) C44B 0.169(5) 0.116(5) 0.130(5) 0.023(5) 0.032(5) -0.012(5) C43B 0.155(5) 0.106(5) 0.113(5) 0.017(4) 0.035(5) -0.006(5) C45B 0.177(6) 0.122(6) 0.139(6) 0.020(6) 0.030(6) -0.016(6) C46B 0.204(10) 0.143(9) 0.161(10) 0.005(9) 0.046(9) -0.019(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O7 2.336(3) 4_565 ? Sm1 O1 2.347(4) . ? Sm1 O5 2.351(4) 4_566 ? Sm1 O3 2.361(4) . ? Sm1 O6 2.361(4) 2_644 ? Sm1 O2 2.377(4) 3_655 ? Sm1 Cl1 2.8428(13) . ? Sm2 O11 2.320(3) 4_565 ? Sm2 O4 2.324(3) . ? Sm2 O10 2.342(3) 3 ? Sm2 O8 2.394(3) 4_565 ? Sm2 O9 2.412(4) . ? Sm2 O12 2.424(4) 2_545 ? Sm2 Cl1 2.8185(12) . ? Sm2 C36 3.064(5) 2_545 ? O1 C1 1.240(6) . ? O2 C1 1.252(6) . ? O2 Sm1 2.377(4) 3_655 ? O3 C13 1.258(6) . ? O5 C12 1.251(6) . ? O5 Sm1 2.351(4) 4_565 ? O4 C13 1.255(6) . ? O6 C12 1.243(6) . ? O6 Sm1 2.361(4) 2_654 ? O7 C24 1.241(6) . ? O7 Sm1 2.336(3) 4_566 ? O8 C24 1.256(6) . ? O8 Sm2 2.394(3) 4_566 ? O9 C25 1.253(7) . ? O10 C25 1.256(6) . ? O10 Sm2 2.342(3) 3 ? O11 C36 1.257(6) . ? O11 Sm2 2.320(3) 4_566 ? O12 C36 1.253(7) . ? O12 Sm2 2.424(4) 2 ? C1 C2 1.516(7) . ? C2 C3 1.366(7) . ? C2 C7 1.424(7) . ? C3 C4 1.414(7) . ? C3 H3A 0.9300 . ? C4 C5 1.357(7) . ? C4 H4A 0.9300 . ? C5 C6 1.440(7) . ? C5 C12 1.500(6) . ? C6 C11 1.417(7) . ? C6 C7 1.420(7) . ? C7 C8 1.420(7) . ? C8 C9 1.362(8) . ? C8 H8A 0.9300 . ? C9 C10 1.411(8) . ? C9 H9A 0.9300 . ? C10 C11 1.358(8) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.507(7) . ? C14 C15 1.366(7) . ? C14 C19 1.427(7) . ? C15 C16 1.399(8) . ? C15 H15A 0.9300 . ? C16 C17 1.362(7) . ? C16 H16A 0.9300 . ? C17 C18 1.431(6) . ? C17 C24 1.517(6) . ? C18 C23 1.419(7) . ? C18 C19 1.446(6) . ? C19 C20 1.410(7) . ? C20 C21 1.360(8) . ? C20 H20A 0.9300 . ? C21 C22 1.396(8) . ? C21 H21A 0.9300 . ? C22 C23 1.358(7) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.498(7) . ? C26 C27 1.359(8) . ? C26 C31 1.431(8) . ? C27 C28 1.417(7) . ? C27 H27A 0.9300 . ? C28 C29 1.351(8) . ? C28 H28A 0.9300 . ? C29 C30 1.426(7) . ? C29 C36 1.499(7) . ? C30 C35 1.424(8) . ? C30 C31 1.431(7) . ? C31 C32 1.408(8) . ? C32 C33 1.356(9) . ? C32 H32A 0.9300 . ? C33 C34 1.399(10) . ? C33 H33A 0.9300 . ? C34 C35 1.359(9) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 Sm2 3.064(5) 2 ? N1A C39A 1.311(9) . ? N1A C37A 1.334(8) . ? N1A C40A 1.456(13) . ? N2A C38A 1.315(8) . ? N2A C39A 1.370(12) . ? N2A C41A 1.488(13) . ? C37A C38A 1.432(15) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.541(10) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C44A 1.564(10) . ? C43A C42A 1.575(10) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.533(10) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.542(10) . ? C45A H45A 0.9700 . ? C45A H45D 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N2B C38B 1.317(9) . ? N2B C39B 1.374(13) . ? N2B C41B 1.495(14) . ? N1B C39B 1.308(9) . ? N1B C37B 1.327(9) . ? N1B C40B 1.438(13) . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C37B C38B 1.433(16) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C41B C42B 1.542(10) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.566(10) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C39B H39B 0.9300 . ? C44B C45B 1.536(10) . ? C44B C43B 1.557(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C45B C46B 1.550(10) . ? C45B H45B 0.9700 . ? C45B H45C 0.9700 . ? C46B H46G 0.9600 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? 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 O7 Sm1 O1 80.28(13) 4_565 . ? O7 Sm1 O5 147.22(15) 4_565 4_566 ? O1 Sm1 O5 77.96(15) . 4_566 ? O7 Sm1 O3 82.24(14) 4_565 . ? O1 Sm1 O3 97.98(16) . . ? O5 Sm1 O3 76.88(14) 4_566 . ? O7 Sm1 O6 77.35(14) 4_565 2_644 ? O1 Sm1 O6 80.80(16) . 2_644 ? O5 Sm1 O6 122.33(14) 4_566 2_644 ? O3 Sm1 O6 159.47(14) . 2_644 ? O7 Sm1 O2 140.15(15) 4_565 3_655 ? O1 Sm1 O2 124.75(14) . 3_655 ? O5 Sm1 O2 72.60(15) 4_566 3_655 ? O3 Sm1 O2 118.64(16) . 3_655 ? O6 Sm1 O2 77.26(15) 2_644 3_655 ? O7 Sm1 Cl1 76.73(9) 4_565 . ? O1 Sm1 Cl1 156.68(10) . . ? O5 Sm1 Cl1 124.46(12) 4_566 . ? O3 Sm1 Cl1 82.87(11) . . ? O6 Sm1 Cl1 90.32(11) 2_644 . ? O2 Sm1 Cl1 73.22(10) 3_655 . ? O11 Sm2 O4 99.17(14) 4_565 . ? O11 Sm2 O10 79.59(15) 4_565 3 ? O4 Sm2 O10 154.42(14) . 3 ? O11 Sm2 O8 80.58(13) 4_565 4_565 ? O4 Sm2 O8 76.42(13) . 4_565 ? O10 Sm2 O8 78.19(13) 3 4_565 ? O11 Sm2 O9 74.70(13) 4_565 . ? O4 Sm2 O9 73.68(13) . . ? O10 Sm2 O9 129.20(13) 3 . ? O8 Sm2 O9 137.12(14) 4_565 . ? O11 Sm2 O12 122.82(13) 4_565 2_545 ? O4 Sm2 O12 114.84(15) . 2_545 ? O10 Sm2 O12 86.01(15) 3 2_545 ? O8 Sm2 O12 148.98(14) 4_565 2_545 ? O9 Sm2 O12 72.95(15) . 2_545 ? O11 Sm2 Cl1 161.83(10) 4_565 . ? O4 Sm2 Cl1 83.28(10) . . ? O10 Sm2 Cl1 90.43(10) 3 . ? O8 Sm2 Cl1 82.54(9) 4_565 . ? O9 Sm2 Cl1 122.91(10) . . ? O12 Sm2 Cl1 70.94(9) 2_545 . ? O11 Sm2 C36 100.42(14) 4_565 2_545 ? O4 Sm2 C36 128.51(15) . 2_545 ? O10 Sm2 C36 76.27(15) 3 2_545 ? O8 Sm2 C36 153.78(14) 4_565 2_545 ? O9 Sm2 C36 66.54(14) . 2_545 ? O12 Sm2 C36 22.79(13) 2_545 2_545 ? Cl1 Sm2 C36 91.79(10) . 2_545 ? Sm2 Cl1 Sm1 111.59(4) . . ? C1 O1 Sm1 143.5(3) . . ? C1 O2 Sm1 143.7(4) . 3_655 ? C13 O3 Sm1 138.4(3) . . ? C12 O5 Sm1 164.1(4) . 4_565 ? C13 O4 Sm2 144.0(4) . . ? C12 O6 Sm1 127.5(3) . 2_654 ? C24 O7 Sm1 160.6(3) . 4_566 ? C24 O8 Sm2 132.0(3) . 4_566 ? C25 O9 Sm2 136.8(3) . . ? C25 O10 Sm2 140.3(4) . 3 ? C36 O11 Sm2 161.3(4) . 4_566 ? C36 O12 Sm2 108.7(3) . 2 ? O1 C1 O2 126.2(5) . . ? O1 C1 C2 116.5(4) . . ? O2 C1 C2 117.2(5) . . ? C3 C2 C7 120.1(4) . . ? C3 C2 C1 116.5(5) . . ? C7 C2 C1 123.4(4) . . ? C2 C3 C4 120.4(5) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 121.4(5) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 C6 119.8(4) . . ? C4 C5 C12 117.1(4) . . ? C6 C5 C12 123.0(4) . . ? C11 C6 C7 119.2(4) . . ? C11 C6 C5 122.2(4) . . ? C7 C6 C5 118.5(4) . . ? C8 C7 C6 118.2(5) . . ? C8 C7 C2 122.2(4) . . ? C6 C7 C2 119.6(4) . . ? C9 C8 C7 121.3(5) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C8 C9 C10 119.9(5) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 120.7(5) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C6 120.6(5) . . ? C10 C11 H11A 119.7 . . ? C6 C11 H11A 119.7 . . ? O6 C12 O5 124.0(5) . . ? O6 C12 C5 118.5(5) . . ? O5 C12 C5 117.5(5) . . ? O4 C13 O3 123.9(5) . . ? O4 C13 C14 118.9(5) . . ? O3 C13 C14 117.1(4) . . ? C15 C14 C19 119.3(5) . . ? C15 C14 C13 117.0(5) . . ? C19 C14 C13 123.7(5) . . ? C14 C15 C16 122.3(5) . . ? C14 C15 H15A 118.8 . . ? C16 C15 H15A 118.8 . . ? C17 C16 C15 120.7(5) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C16 C17 C18 120.0(5) . . ? C16 C17 C24 115.5(4) . . ? C18 C17 C24 124.5(4) . . ? C23 C18 C17 123.1(4) . . ? C23 C18 C19 118.0(4) . . ? C17 C18 C19 118.9(4) . . ? C20 C19 C14 123.2(5) . . ? C20 C19 C18 118.0(5) . . ? C14 C19 C18 118.7(4) . . ? C21 C20 C19 121.6(5) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C20 C21 C22 120.5(5) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C23 C22 C21 120.4(5) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C18 121.4(5) . . ? C22 C23 H23A 119.3 . . ? C18 C23 H23A 119.3 . . ? O7 C24 O8 126.0(5) . . ? O7 C24 C17 114.6(4) . . ? O8 C24 C17 119.4(4) . . ? O9 C25 O10 125.1(5) . . ? O9 C25 C26 118.4(5) . . ? O10 C25 C26 116.4(5) . . ? C27 C26 C31 120.3(5) . . ? C27 C26 C25 118.5(5) . . ? C31 C26 C25 121.0(5) . . ? C26 C27 C28 121.1(5) . . ? C26 C27 H27A 119.4 . . ? C28 C27 H27A 119.4 . . ? C29 C28 C27 120.2(5) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C28 C29 C30 120.6(5) . . ? C28 C29 C36 118.8(5) . . ? C30 C29 C36 120.4(5) . . ? C35 C30 C29 122.7(5) . . ? C35 C30 C31 118.1(5) . . ? C29 C30 C31 119.1(5) . . ? C32 C31 C26 122.8(5) . . ? C32 C31 C30 119.1(5) . . ? C26 C31 C30 118.0(5) . . ? C33 C32 C31 121.0(6) . . ? C33 C32 H32A 119.5 . . ? C31 C32 H32A 119.5 . . ? C32 C33 C34 120.2(6) . . ? C32 C33 H33A 119.9 . . ? C34 C33 H33A 119.9 . . ? C35 C34 C33 121.3(6) . . ? C35 C34 H34A 119.4 . . ? C33 C34 H34A 119.4 . . ? C34 C35 C30 120.3(6) . . ? C34 C35 H35A 119.9 . . ? C30 C35 H35A 119.9 . . ? O12 C36 O11 122.0(5) . . ? O12 C36 C29 118.4(5) . . ? O11 C36 C29 119.5(5) . . ? O12 C36 Sm2 48.5(3) . 2 ? O11 C36 Sm2 74.0(3) . 2 ? C29 C36 Sm2 165.8(4) . 2 ? C39A N1A C37A 109.1(11) . . ? C39A N1A C40A 122.6(11) . . ? C37A N1A C40A 127.3(10) . . ? C38A N2A C39A 107.9(10) . . ? C38A N2A C41A 127.8(12) . . ? C39A N2A C41A 124.2(9) . . ? N1A C37A C38A 106.2(11) . . ? N1A C37A H37A 126.9 . . ? C38A C37A H37A 126.9 . . ? N2A C38A C37A 106.4(11) . . ? N2A C38A H38A 126.8 . . ? C37A C38A H38A 126.8 . . ? N1A C39A N2A 108.5(10) . . ? N1A C39A H39A 125.7 . . ? N2A C39A H39A 125.7 . . ? N2A C41A C42A 108.6(14) . . ? N2A C41A H41A 110.0 . . ? C42A C41A H41A 110.0 . . ? N2A C41A H41B 110.0 . . ? C42A C41A H41B 110.0 . . ? H41A C41A H41B 108.3 . . ? C44A C43A C42A 107.8(11) . . ? C44A C43A H43A 110.2 . . ? C42A C43A H43A 110.2 . . ? C44A C43A H43B 110.2 . . ? C42A C43A H43B 110.2 . . ? H43A C43A H43B 108.5 . . ? C41A C42A C43A 94.9(14) . . ? C41A C42A H42A 112.8 . . ? C43A C42A H42A 112.8 . . ? C41A C42A H42B 112.8 . . ? C43A C42A H42B 112.8 . . ? H42A C42A H42B 110.2 . . ? C45A C44A C43A 115.9(13) . . ? C45A C44A H44A 108.3 . . ? C43A C44A H44A 108.3 . . ? C45A C44A H44B 108.3 . . ? C43A C44A H44B 108.3 . . ? H44A C44A H44B 107.4 . . ? C44A C45A C46A 115.7(12) . . ? C44A C45A H45A 108.4 . . ? C46A C45A H45A 108.4 . . ? C44A C45A H45D 108.4 . . ? C46A C45A H45D 108.4 . . ? H45A C45A H45D 107.4 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C38B N2B C39B 107.2(11) . . ? C38B N2B C41B 130.0(15) . . ? C39B N2B C41B 122.6(11) . . ? C39B N1B C37B 110.1(17) . . ? C39B N1B C40B 117.1(16) . . ? C37B N1B C40B 132.2(13) . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N1B C37B C38B 104.9(16) . . ? N1B C37B H37B 127.6 . . ? C38B C37B H37B 127.6 . . ? N2B C38B C37B 107.4(13) . . ? N2B C38B H38B 126.3 . . ? C37B C38B H38B 126.3 . . ? N2B C41B C42B 127(2) . . ? N2B C41B H41C 105.6 . . ? C42B C41B H41C 105.6 . . ? N2B C41B H41D 105.6 . . ? C42B C41B H41D 105.6 . . ? H41C C41B H41D 106.1 . . ? C41B C42B C43B 119(2) . . ? C41B C42B H42C 107.5 . . ? C43B C42B H42C 107.5 . . ? C41B C42B H42D 107.5 . . ? C43B C42B H42D 107.5 . . ? H42C C42B H42D 107.0 . . ? N1B C39B N2B 107.9(14) . . ? N1B C39B H39B 126.1 . . ? N2B C39B H39B 126.1 . . ? C45B C44B C43B 118.8(14) . . ? C45B C44B H44C 107.6 . . ? C43B C44B H44C 107.6 . . ? C45B C44B H44D 107.6 . . ? C43B C44B H44D 107.6 . . ? H44C C44B H44D 107.0 . . ? C44B C43B C42B 116.2(15) . . ? C44B C43B H43C 108.2 . . ? C42B C43B H43C 108.2 . . ? C44B C43B H43D 108.2 . . ? C42B C43B H43D 108.2 . . ? H43C C43B H43D 107.4 . . ? C44B C45B C46B 115.6(12) . . ? C44B C45B H45B 108.4 . . ? C46B C45B H45B 108.4 . . ? C44B C45B H45C 108.4 . . ? C46B C45B H45C 108.4 . . ? H45B C45B H45C 107.5 . . ? C45B C46B H46G 109.5 . . ? C45B C46B H46D 109.5 . . ? H46G C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46G C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Sm2 Cl1 Sm1 74.0(3) 4_565 . . . ? O4 Sm2 Cl1 Sm1 -24.93(11) . . . . ? O10 Sm2 Cl1 Sm1 130.22(11) 3 . . . ? O8 Sm2 Cl1 Sm1 52.19(10) 4_565 . . . ? O9 Sm2 Cl1 Sm1 -90.52(12) . . . . ? O12 Sm2 Cl1 Sm1 -144.15(13) 2_545 . . . ? C36 Sm2 Cl1 Sm1 -153.51(12) 2_545 . . . ? O7 Sm1 Cl1 Sm2 -39.63(11) 4_565 . . . ? O1 Sm1 Cl1 Sm2 -49.6(3) . . . . ? O5 Sm1 Cl1 Sm2 112.73(13) 4_566 . . . ? O3 Sm1 Cl1 Sm2 44.04(12) . . . . ? O6 Sm1 Cl1 Sm2 -116.54(11) 2_644 . . . ? O2 Sm1 Cl1 Sm2 166.87(13) 3_655 . . . ? O7 Sm1 O1 C1 -154.4(7) 4_565 . . . ? O5 Sm1 O1 C1 50.3(7) 4_566 . . . ? O3 Sm1 O1 C1 125.0(7) . . . . ? O6 Sm1 O1 C1 -75.7(7) 2_644 . . . ? O2 Sm1 O1 C1 -8.3(7) 3_655 . . . ? Cl1 Sm1 O1 C1 -144.5(5) . . . . ? O7 Sm1 O3 C13 29.5(6) 4_565 . . . ? O1 Sm1 O3 C13 108.5(6) . . . . ? O5 Sm1 O3 C13 -175.9(6) 4_566 . . . ? O6 Sm1 O3 C13 23.4(9) 2_644 . . . ? O2 Sm1 O3 C13 -114.4(6) 3_655 . . . ? Cl1 Sm1 O3 C13 -48.0(6) . . . . ? O11 Sm2 O4 C13 159.9(6) 4_565 . . . ? O10 Sm2 O4 C13 -115.1(6) 3 . . . ? O8 Sm2 O4 C13 -122.2(6) 4_565 . . . ? O9 Sm2 O4 C13 88.9(6) . . . . ? O12 Sm2 O4 C13 27.1(6) 2_545 . . . ? Cl1 Sm2 O4 C13 -38.3(6) . . . . ? C36 Sm2 O4 C13 48.7(6) 2_545 . . . ? O11 Sm2 O9 C25 18.4(5) 4_565 . . . ? O4 Sm2 O9 C25 123.0(6) . . . . ? O10 Sm2 O9 C25 -43.9(6) 3 . . . ? O8 Sm2 O9 C25 75.5(6) 4_565 . . . ? O12 Sm2 O9 C25 -113.8(5) 2_545 . . . ? Cl1 Sm2 O9 C25 -166.5(5) . . . . ? C36 Sm2 O9 C25 -90.4(5) 2_545 . . . ? Sm1 O1 C1 O2 -4.6(11) . . . . ? Sm1 O1 C1 C2 172.5(4) . . . . ? Sm1 O2 C1 O1 19.6(11) 3_655 . . . ? Sm1 O2 C1 C2 -157.6(5) 3_655 . . . ? O1 C1 C2 C3 -41.4(8) . . . . ? O2 C1 C2 C3 136.0(6) . . . . ? O1 C1 C2 C7 138.5(6) . . . . ? O2 C1 C2 C7 -44.1(8) . . . . ? C7 C2 C3 C4 1.9(9) . . . . ? C1 C2 C3 C4 -178.2(5) . . . . ? C2 C3 C4 C5 -0.7(9) . . . . ? C3 C4 C5 C6 -1.9(9) . . . . ? C3 C4 C5 C12 175.2(5) . . . . ? C4 C5 C6 C11 -174.6(5) . . . . ? C12 C5 C6 C11 8.5(8) . . . . ? C4 C5 C6 C7 3.2(8) . . . . ? C12 C5 C6 C7 -173.8(5) . . . . ? C11 C6 C7 C8 -2.1(8) . . . . ? C5 C6 C7 C8 -179.9(5) . . . . ? C11 C6 C7 C2 175.9(5) . . . . ? C5 C6 C7 C2 -2.0(7) . . . . ? C3 C2 C7 C8 177.4(5) . . . . ? C1 C2 C7 C8 -2.5(8) . . . . ? C3 C2 C7 C6 -0.5(8) . . . . ? C1 C2 C7 C6 179.6(5) . . . . ? C6 C7 C8 C9 1.4(9) . . . . ? C2 C7 C8 C9 -176.5(6) . . . . ? C7 C8 C9 C10 0.1(10) . . . . ? C8 C9 C10 C11 -0.9(10) . . . . ? C9 C10 C11 C6 0.1(10) . . . . ? C7 C6 C11 C10 1.4(8) . . . . ? C5 C6 C11 C10 179.2(6) . . . . ? Sm1 O6 C12 O5 0.4(9) 2_654 . . . ? Sm1 O6 C12 C5 179.4(4) 2_654 . . . ? Sm1 O5 C12 O6 27.5(19) 4_565 . . . ? Sm1 O5 C12 C5 -151.5(12) 4_565 . . . ? C4 C5 C12 O6 -141.4(6) . . . . ? C6 C5 C12 O6 35.6(8) . . . . ? C4 C5 C12 O5 37.7(8) . . . . ? C6 C5 C12 O5 -145.3(5) . . . . ? Sm2 O4 C13 O3 63.2(9) . . . . ? Sm2 O4 C13 C14 -113.5(6) . . . . ? Sm1 O3 C13 O4 5.0(10) . . . . ? Sm1 O3 C13 C14 -178.3(4) . . . . ? O4 C13 C14 C15 143.1(6) . . . . ? O3 C13 C14 C15 -33.8(8) . . . . ? O4 C13 C14 C19 -35.2(8) . . . . ? O3 C13 C14 C19 147.8(5) . . . . ? C19 C14 C15 C16 0.4(9) . . . . ? C13 C14 C15 C16 -178.0(6) . . . . ? C14 C15 C16 C17 1.2(10) . . . . ? C15 C16 C17 C18 -0.5(9) . . . . ? C15 C16 C17 C24 -180.0(5) . . . . ? C16 C17 C18 C23 -179.0(5) . . . . ? C24 C17 C18 C23 0.4(8) . . . . ? C16 C17 C18 C19 -1.7(8) . . . . ? C24 C17 C18 C19 177.7(5) . . . . ? C15 C14 C19 C20 175.7(6) . . . . ? C13 C14 C19 C20 -6.0(8) . . . . ? C15 C14 C19 C18 -2.6(8) . . . . ? C13 C14 C19 C18 175.7(5) . . . . ? C23 C18 C19 C20 2.3(7) . . . . ? C17 C18 C19 C20 -175.2(5) . . . . ? C23 C18 C19 C14 -179.3(5) . . . . ? C17 C18 C19 C14 3.3(7) . . . . ? C14 C19 C20 C21 -179.5(6) . . . . ? C18 C19 C20 C21 -1.1(8) . . . . ? C19 C20 C21 C22 -0.1(10) . . . . ? C20 C21 C22 C23 0.1(10) . . . . ? C21 C22 C23 C18 1.1(9) . . . . ? C17 C18 C23 C22 175.0(5) . . . . ? C19 C18 C23 C22 -2.3(8) . . . . ? Sm1 O7 C24 O8 8.2(15) 4_566 . . . ? Sm1 O7 C24 C17 -171.1(9) 4_566 . . . ? Sm2 O8 C24 O7 -33.1(8) 4_566 . . . ? Sm2 O8 C24 C17 146.2(4) 4_566 . . . ? C16 C17 C24 O7 33.7(7) . . . . ? C18 C17 C24 O7 -145.7(5) . . . . ? C16 C17 C24 O8 -145.6(5) . . . . ? C18 C17 C24 O8 35.0(8) . . . . ? Sm2 O9 C25 O10 29.6(9) . . . . ? Sm2 O9 C25 C26 -151.5(4) . . . . ? Sm2 O10 C25 O9 4.6(10) 3 . . . ? Sm2 O10 C25 C26 -174.3(4) 3 . . . ? O9 C25 C26 C27 -48.1(7) . . . . ? O10 C25 C26 C27 130.8(6) . . . . ? O9 C25 C26 C31 137.7(5) . . . . ? O10 C25 C26 C31 -43.3(7) . . . . ? C31 C26 C27 C28 6.2(9) . . . . ? C25 C26 C27 C28 -168.0(5) . . . . ? C26 C27 C28 C29 0.3(9) . . . . ? C27 C28 C29 C30 -7.2(9) . . . . ? C27 C28 C29 C36 168.7(5) . . . . ? C28 C29 C30 C35 -170.7(6) . . . . ? C36 C29 C30 C35 13.5(8) . . . . ? C28 C29 C30 C31 7.5(8) . . . . ? C36 C29 C30 C31 -168.3(5) . . . . ? C27 C26 C31 C32 171.8(6) . . . . ? C25 C26 C31 C32 -14.2(8) . . . . ? C27 C26 C31 C30 -5.5(8) . . . . ? C25 C26 C31 C30 168.5(5) . . . . ? C35 C30 C31 C32 -0.3(8) . . . . ? C29 C30 C31 C32 -178.6(5) . . . . ? C35 C30 C31 C26 177.1(5) . . . . ? C29 C30 C31 C26 -1.2(7) . . . . ? C26 C31 C32 C33 -175.5(6) . . . . ? C30 C31 C32 C33 1.8(9) . . . . ? C31 C32 C33 C34 -1.9(10) . . . . ? C32 C33 C34 C35 0.5(11) . . . . ? C33 C34 C35 C30 1.1(10) . . . . ? C29 C30 C35 C34 177.1(6) . . . . ? C31 C30 C35 C34 -1.1(9) . . . . ? Sm2 O12 C36 O11 9.7(7) 2 . . . ? Sm2 O12 C36 C29 -173.2(4) 2 . . . ? Sm2 O11 C36 O12 -112.6(11) 4_566 . . . ? Sm2 O11 C36 C29 70.3(14) 4_566 . . . ? Sm2 O11 C36 Sm2 -105.0(12) 4_566 . . 2 ? C28 C29 C36 O12 -133.4(6) . . . . ? C30 C29 C36 O12 42.5(8) . . . . ? C28 C29 C36 O11 43.8(8) . . . . ? C30 C29 C36 O11 -140.3(5) . . . . ? C28 C29 C36 Sm2 -154.7(13) . . . 2 ? C30 C29 C36 Sm2 21.2(18) . . . 2 ? C39A N1A C37A C38A 6(2) . . . . ? C40A N1A C37A C38A 174.8(15) . . . . ? C39A N2A C38A C37A -10(3) . . . . ? C41A N2A C38A C37A 174(2) . . . . ? N1A C37A C38A N2A 2.7(19) . . . . ? C37A N1A C39A N2A -13(3) . . . . ? C40A N1A C39A N2A 178.1(19) . . . . ? C38A N2A C39A N1A 14(3) . . . . ? C41A N2A C39A N1A -170(2) . . . . ? C38A N2A C41A C42A -3(3) . . . . ? C39A N2A C41A C42A -178(2) . . . . ? N2A C41A C42A C43A -85(2) . . . . ? C44A C43A C42A C41A -156.7(14) . . . . ? C42A C43A C44A C45A -79(2) . . . . ? C43A C44A C45A C46A -128(2) . . . . ? C39B N1B C37B C38B -12(3) . . . . ? C40B N1B C37B C38B 177(3) . . . . ? C39B N2B C38B C37B 7(4) . . . . ? C41B N2B C38B C37B -177(3) . . . . ? N1B C37B C38B N2B 2(3) . . . . ? C38B N2B C41B C42B -76(4) . . . . ? C39B N2B C41B C42B 99(4) . . . . ? N2B C41B C42B C43B 75(4) . . . . ? C37B N1B C39B N2B 17(4) . . . . ? C40B N1B C39B N2B -171(3) . . . . ? C38B N2B C39B N1B -15(5) . . . . ? C41B N2B C39B N1B 170(3) . . . . ? C45B C44B C43B C42B -142(3) . . . . ? C41B C42B C43B C44B -126(3) . . . . ? C43B C44B C45B C46B -20(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.368 _refine_diff_density_min -1.892 _refine_diff_density_rms 0.131 #===END data_compound-6 _database_code_depnum_ccdc_archive 'CCDC 876526' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Eu2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl Eu2 N2 O12' _chemical_formula_weight 1149.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.7876(2) _cell_length_b 14.81893(16) _cell_length_c 15.94964(19) _cell_angle_alpha 90.00 _cell_angle_beta 94.9429(11) _cell_angle_gamma 90.00 _cell_volume 4188.59(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12260 _cell_measurement_theta_min 2.5284 _cell_measurement_theta_max 28.8208 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 3.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85153 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18560 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8700 _reflns_number_gt 7166 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0390P)^2^+1.2643P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8700 _refine_ls_number_parameters 607 _refine_ls_number_restraints 931 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.114 _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 Eu1 Eu 0.378106(9) 0.024720(11) -0.004786(9) 0.01319(6) Uani 1 1 d . . . Eu2 Eu 0.116139(9) 0.011984(11) -0.001158(9) 0.01399(6) Uani 1 1 d . . . Cl1 Cl 0.25207(5) -0.08439(7) 0.02369(6) 0.0297(2) Uani 1 1 d . . . O1 O 0.44934(15) 0.1257(2) -0.07738(18) 0.0373(7) Uani 1 1 d . . . O2 O 0.57390(15) 0.10769(19) -0.06305(18) 0.0371(7) Uani 1 1 d . . . O3 O 0.31539(15) 0.1308(2) 0.07393(18) 0.0397(7) Uani 1 1 d . . . O5 O 0.47146(16) 0.4303(2) -0.40133(17) 0.0433(8) Uani 1 1 d . . . O4 O 0.19324(14) 0.13517(17) 0.03079(16) 0.0303(6) Uani 1 1 d . . . O6 O 0.59570(16) 0.4324(2) -0.38252(16) 0.0391(7) Uani 1 1 d . . . O7 O 0.28800(14) 0.43033(19) 0.38978(15) 0.0323(7) Uani 1 1 d . . . O8 O 0.16426(14) 0.45323(18) 0.36853(14) 0.0255(6) Uani 1 1 d . . . O9 O 0.06173(15) 0.09084(19) 0.11054(16) 0.0324(7) Uani 1 1 d . . . O10 O -0.06367(15) 0.10238(18) 0.08794(16) 0.0324(7) Uani 1 1 d . . . O11 O 0.01392(15) 0.41254(19) 0.43511(15) 0.0329(7) Uani 1 1 d . . . O12 O -0.10616(15) 0.4048(2) 0.38914(18) 0.0400(8) Uani 1 1 d . . . C1 C 0.5145(2) 0.1456(3) -0.0933(2) 0.0261(8) Uani 1 1 d . . . C2 C 0.5217(2) 0.2189(2) -0.1580(2) 0.0227(8) Uani 1 1 d . . . C3 C 0.4715(2) 0.2175(3) -0.2283(2) 0.0317(10) Uani 1 1 d . . . H3A H 0.4344 0.1732 -0.2337 0.038 Uiso 1 1 calc R . . C4 C 0.4753(2) 0.2818(3) -0.2919(2) 0.0309(9) Uani 1 1 d . . . H4A H 0.4403 0.2797 -0.3387 0.037 Uiso 1 1 calc R . . C5 C 0.5293(2) 0.3476(3) -0.2868(2) 0.0233(8) Uani 1 1 d . . . C6 C 0.58146(19) 0.3541(2) -0.2135(2) 0.0203(8) Uani 1 1 d . . . C7 C 0.5782(2) 0.2878(3) -0.1489(2) 0.0224(8) Uani 1 1 d . . . C8 C 0.6298(2) 0.2947(3) -0.0762(2) 0.0299(9) Uani 1 1 d . . . H8A H 0.6293 0.2515 -0.0340 0.036 Uiso 1 1 calc R . . C9 C 0.6803(2) 0.3642(3) -0.0678(2) 0.0390(11) Uani 1 1 d . . . H9A H 0.7141 0.3676 -0.0200 0.047 Uiso 1 1 calc R . . C10 C 0.6816(2) 0.4304(3) -0.1304(2) 0.0356(10) Uani 1 1 d . . . H10A H 0.7157 0.4779 -0.1232 0.043 Uiso 1 1 calc R . . C11 C 0.6343(2) 0.4260(3) -0.2008(2) 0.0300(9) Uani 1 1 d . . . H11A H 0.6361 0.4706 -0.2416 0.036 Uiso 1 1 calc R . . C12 C 0.5325(2) 0.4084(3) -0.3619(2) 0.0271(9) Uani 1 1 d . . . C13 C 0.2498(2) 0.1625(3) 0.0762(2) 0.0255(8) Uani 1 1 d . . . C14 C 0.2394(2) 0.2343(2) 0.1408(2) 0.0235(8) Uani 1 1 d . . . C15 C 0.2831(2) 0.2272(3) 0.2156(2) 0.0340(10) Uani 1 1 d . . . H15A H 0.3179 0.1803 0.2228 0.041 Uiso 1 1 calc R . . C16 C 0.2770(2) 0.2879(3) 0.2810(2) 0.0338(10) Uani 1 1 d . . . H16A H 0.3082 0.2813 0.3306 0.041 Uiso 1 1 calc R . . C17 C 0.22584(19) 0.3576(2) 0.2740(2) 0.0199(7) Uani 1 1 d . . . C18 C 0.17865(18) 0.3679(2) 0.19734(19) 0.0173(7) Uani 1 1 d . . . C19 C 0.1867(2) 0.3067(2) 0.1288(2) 0.0217(8) Uani 1 1 d . . . C20 C 0.1434(2) 0.3227(3) 0.0521(2) 0.0298(9) Uani 1 1 d . . . H20A H 0.1487 0.2844 0.0068 0.036 Uiso 1 1 calc R . . C21 C 0.0940(2) 0.3931(3) 0.0427(2) 0.0354(10) Uani 1 1 d . . . H21A H 0.0664 0.4025 -0.0088 0.043 Uiso 1 1 calc R . . C22 C 0.0850(2) 0.4507(3) 0.1097(2) 0.0342(10) Uani 1 1 d . . . H22A H 0.0506 0.4980 0.1030 0.041 Uiso 1 1 calc R . . C23 C 0.1256(2) 0.4391(2) 0.1848(2) 0.0252(8) Uani 1 1 d . . . H23A H 0.1186 0.4785 0.2288 0.030 Uiso 1 1 calc R . . C24 C 0.2252(2) 0.4194(2) 0.3494(2) 0.0210(8) Uani 1 1 d . . . C25 C 0.0002(2) 0.1273(3) 0.1208(2) 0.0249(8) Uani 1 1 d . . . C26 C -0.0009(2) 0.2053(3) 0.1806(2) 0.0239(8) Uani 1 1 d . . . C27 C 0.0387(2) 0.1979(3) 0.2578(2) 0.0320(9) Uani 1 1 d . . . H27A H 0.0716 0.1497 0.2684 0.038 Uiso 1 1 calc R . . C28 C 0.0304(2) 0.2618(3) 0.3215(2) 0.0338(10) Uani 1 1 d . . . H28A H 0.0588 0.2562 0.3731 0.041 Uiso 1 1 calc R . . C29 C -0.0189(2) 0.3323(3) 0.3083(2) 0.0234(8) Uani 1 1 d . . . C30 C -0.0559(2) 0.3478(3) 0.2254(2) 0.0248(8) Uani 1 1 d . . . C31 C -0.0462(2) 0.2832(3) 0.1621(2) 0.0246(8) Uani 1 1 d . . . C32 C -0.0810(2) 0.3005(3) 0.0793(2) 0.0363(10) Uani 1 1 d . . . H32A H -0.0766 0.2585 0.0366 0.044 Uiso 1 1 calc R . . C33 C -0.1201(3) 0.3774(3) 0.0631(3) 0.0487(12) Uani 1 1 d . . . H33A H -0.1416 0.3883 0.0089 0.058 Uiso 1 1 calc R . . C34 C -0.1288(3) 0.4403(3) 0.1257(3) 0.0505(13) Uani 1 1 d . . . H34A H -0.1560 0.4929 0.1129 0.061 Uiso 1 1 calc R . . C35 C -0.0983(2) 0.4261(3) 0.2052(3) 0.0373(10) Uani 1 1 d . . . H35A H -0.1054 0.4685 0.2468 0.045 Uiso 1 1 calc R . . C36 C -0.0381(2) 0.3876(3) 0.3813(2) 0.0276(9) Uani 1 1 d . . . N1A N 0.2340(4) -0.2665(4) 0.2716(4) 0.0577(11) Uani 0.667(3) 1 d PDU A 1 N2A N 0.3051(4) -0.1519(5) 0.2692(4) 0.0665(11) Uani 0.667(3) 1 d PDU A 1 C37A C 0.2780(9) -0.2692(11) 0.3425(9) 0.0668(13) Uani 0.667(3) 1 d PDU A 1 H37A H 0.2765 -0.3118 0.3851 0.080 Uiso 0.667(3) 1 calc PR A 1 C38A C 0.3286(5) -0.1938(6) 0.3412(5) 0.0672(12) Uani 0.667(3) 1 d PDU A 1 H38A H 0.3680 -0.1779 0.3806 0.081 Uiso 0.667(3) 1 calc PR A 1 C39A C 0.2504(13) -0.1962(12) 0.2275(10) 0.0625(11) Uani 0.667(3) 1 d PDU A 1 H39A H 0.2272 -0.1803 0.1751 0.075 Uiso 0.667(3) 1 calc PR A 1 C40A C 0.1772(5) -0.3373(6) 0.2491(6) 0.0720(18) Uani 0.667(3) 1 d PDU A 1 H40A H 0.1377 -0.3128 0.2111 0.108 Uiso 0.667(3) 1 calc PR A 1 H40B H 0.1564 -0.3583 0.2991 0.108 Uiso 0.667(3) 1 calc PR A 1 H40C H 0.2008 -0.3867 0.2226 0.108 Uiso 0.667(3) 1 calc PR A 1 C41A C 0.3372(5) -0.0660(6) 0.2397(5) 0.0793(12) Uani 0.667(3) 1 d PDU A 1 H41A H 0.2950 -0.0276 0.2207 0.095 Uiso 0.667(3) 1 calc PR A 1 H41B H 0.3633 -0.0804 0.1904 0.095 Uiso 0.667(3) 1 calc PR A 1 C42A C 0.3906(5) -0.0094(7) 0.2970(6) 0.0899(14) Uani 0.667(3) 1 d PDU A 1 H42A H 0.4144 0.0379 0.2665 0.108 Uiso 0.667(3) 1 calc PR A 1 H42B H 0.4290 -0.0458 0.3278 0.108 Uiso 0.667(3) 1 calc PR A 1 C43A C 0.3302(5) 0.0304(7) 0.3574(6) 0.0957(14) Uani 0.667(3) 1 d PDU A 1 H43A H 0.2868 0.0578 0.3264 0.115 Uiso 0.667(3) 1 calc PR A 1 H43B H 0.3141 -0.0139 0.3969 0.115 Uiso 0.667(3) 1 calc PR A 1 C44A C 0.3860(7) 0.1006(7) 0.3991(5) 0.1079(16) Uani 0.667(3) 1 d PDU A 1 H44A H 0.4230 0.1142 0.3596 0.129 Uiso 0.667(3) 1 calc PR A 1 H44B H 0.3580 0.1557 0.4070 0.129 Uiso 0.667(3) 1 calc PR A 1 C45A C 0.4279(7) 0.0769(8) 0.4816(6) 0.1162(19) Uani 0.667(3) 1 d PDU A 1 H45A H 0.4815 0.0865 0.4786 0.139 Uiso 0.667(3) 1 calc PR A 1 H45D H 0.4199 0.0137 0.4942 0.139 Uiso 0.667(3) 1 calc PR A 1 C46A C 0.3996(9) 0.1357(9) 0.5507(7) 0.140(3) Uani 0.667(3) 1 d PDU A 1 H46A H 0.4281 0.1226 0.6031 0.210 Uiso 0.667(3) 1 calc PR A 1 H46B H 0.3472 0.1233 0.5556 0.210 Uiso 0.667(3) 1 calc PR A 1 H46C H 0.4058 0.1981 0.5368 0.210 Uiso 0.667(3) 1 calc PR A 1 N1B N 0.2090(8) -0.2819(8) 0.2287(8) 0.0577(11) Uani 0.333(3) 1 d PDU A 2 N2B N 0.2952(8) -0.2002(9) 0.2936(8) 0.0665(11) Uani 0.333(3) 1 d PDU A 2 C37B C 0.2207(9) -0.3158(11) 0.3054(8) 0.0668(13) Uani 0.333(3) 1 d PDU A 2 H37B H 0.1925 -0.3601 0.3297 0.080 Uiso 0.333(3) 1 calc PR A 2 C38B C 0.2867(19) -0.270(2) 0.3439(18) 0.0672(12) Uani 0.333(3) 1 d PDU A 2 H38B H 0.3162 -0.2851 0.3927 0.081 Uiso 0.333(3) 1 calc PR A 2 C39B C 0.247(3) -0.206(2) 0.226(2) 0.0625(11) Uani 0.333(3) 1 d PDU A 2 H39B H 0.2405 -0.1630 0.1831 0.075 Uiso 0.333(3) 1 calc PR A 2 C40B C 0.1547(9) -0.3222(11) 0.1639(9) 0.0720(18) Uani 0.333(3) 1 d PDU A 2 H40D H 0.1499 -0.2839 0.1151 0.108 Uiso 0.333(3) 1 calc PR A 2 H40E H 0.1064 -0.3283 0.1859 0.108 Uiso 0.333(3) 1 calc PR A 2 H40F H 0.1724 -0.3806 0.1485 0.108 Uiso 0.333(3) 1 calc PR A 2 C41B C 0.3496(9) -0.1215(10) 0.3010(11) 0.0793(12) Uani 0.333(3) 1 d PDU A 2 H41C H 0.3875 -0.1373 0.2633 0.095 Uiso 0.333(3) 1 calc PR A 2 H41D H 0.3745 -0.1275 0.3573 0.095 Uiso 0.333(3) 1 calc PR A 2 C42B C 0.3398(12) -0.0162(11) 0.2890(10) 0.0899(14) Uani 0.333(3) 1 d PDU A 2 H42C H 0.2870 0.0012 0.2833 0.108 Uiso 0.333(3) 1 calc PR A 2 H42D H 0.3643 0.0055 0.2408 0.108 Uiso 0.333(3) 1 calc PR A 2 C44B C 0.3380(10) 0.0807(14) 0.4329(12) 0.1079(16) Uani 0.333(3) 1 d PDU A 2 H44C H 0.2997 0.1097 0.3951 0.129 Uiso 0.333(3) 1 calc PR A 2 H44D H 0.3112 0.0398 0.4672 0.129 Uiso 0.333(3) 1 calc PR A 2 C43B C 0.3818(11) 0.0192(14) 0.3761(11) 0.0957(14) Uani 0.333(3) 1 d PDU A 2 H43C H 0.3986 -0.0333 0.4089 0.115 Uiso 0.333(3) 1 calc PR A 2 H43D H 0.4267 0.0515 0.3628 0.115 Uiso 0.333(3) 1 calc PR A 2 C45B C 0.3672(11) 0.1532(14) 0.4914(14) 0.1162(19) Uani 0.333(3) 1 d PDU A 2 H45B H 0.3375 0.1546 0.5396 0.139 Uiso 0.333(3) 1 calc PR A 2 H45C H 0.3615 0.2110 0.4631 0.139 Uiso 0.333(3) 1 calc PR A 2 C46B C 0.4512(11) 0.1386(19) 0.5221(16) 0.140(3) Uani 0.333(3) 1 d PDU A 2 H46D H 0.4678 0.1862 0.5602 0.210 Uiso 0.333(3) 1 calc PR A 2 H46E H 0.4810 0.1390 0.4747 0.210 Uiso 0.333(3) 1 calc PR A 2 H46F H 0.4570 0.0816 0.5505 0.210 Uiso 0.333(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01267(9) 0.01414(9) 0.01296(9) -0.00013(6) 0.00220(6) 0.00079(7) Eu2 0.01354(10) 0.01483(9) 0.01377(9) -0.00032(6) 0.00220(6) -0.00092(7) Cl1 0.0165(4) 0.0269(5) 0.0465(5) 0.0137(4) 0.0074(4) 0.0025(4) O1 0.0217(15) 0.0424(18) 0.0487(17) 0.0229(14) 0.0080(12) -0.0053(14) O2 0.0251(15) 0.0328(16) 0.0524(18) 0.0237(14) -0.0024(13) 0.0019(13) O3 0.0243(16) 0.0414(17) 0.0532(18) -0.0280(15) 0.0024(13) 0.0076(14) O5 0.0368(18) 0.0499(19) 0.0400(16) 0.0221(15) -0.0163(13) -0.0024(15) O4 0.0227(14) 0.0275(14) 0.0411(16) -0.0149(12) 0.0056(12) -0.0054(12) O6 0.0366(17) 0.0506(19) 0.0307(15) 0.0209(14) 0.0061(12) -0.0104(15) O7 0.0202(14) 0.0477(18) 0.0282(14) -0.0180(13) -0.0022(11) -0.0001(13) O8 0.0214(14) 0.0359(15) 0.0195(12) -0.0079(11) 0.0031(10) 0.0066(12) O9 0.0270(15) 0.0401(17) 0.0314(14) -0.0167(13) 0.0096(12) -0.0005(13) O10 0.0255(15) 0.0355(16) 0.0373(15) -0.0202(13) 0.0091(12) -0.0115(13) O11 0.0331(16) 0.0400(17) 0.0261(14) -0.0120(12) 0.0051(12) -0.0159(14) O12 0.0247(16) 0.0488(19) 0.0485(17) -0.0272(15) 0.0149(13) -0.0099(14) C1 0.025(2) 0.0224(19) 0.031(2) 0.0095(16) 0.0018(16) -0.0018(17) C2 0.0167(19) 0.0219(19) 0.0294(19) 0.0103(16) 0.0022(15) -0.0001(16) C3 0.019(2) 0.033(2) 0.043(2) 0.0145(19) -0.0032(17) -0.0074(18) C4 0.024(2) 0.038(2) 0.030(2) 0.0154(18) -0.0053(16) -0.0040(19) C5 0.0175(19) 0.028(2) 0.0245(19) 0.0092(16) 0.0007(14) 0.0013(16) C6 0.0165(18) 0.0213(18) 0.0233(18) 0.0068(15) 0.0024(14) -0.0001(15) C7 0.0185(19) 0.0257(19) 0.0233(18) 0.0072(15) 0.0036(14) 0.0026(16) C8 0.030(2) 0.036(2) 0.0227(19) 0.0109(17) -0.0030(16) -0.0033(19) C9 0.034(2) 0.053(3) 0.028(2) 0.004(2) -0.0049(18) -0.012(2) C10 0.034(2) 0.038(2) 0.035(2) -0.0011(19) 0.0039(18) -0.013(2) C11 0.033(2) 0.030(2) 0.028(2) 0.0049(17) 0.0048(17) -0.0079(19) C12 0.029(2) 0.028(2) 0.0239(19) 0.0083(16) -0.0027(16) -0.0032(18) C13 0.021(2) 0.0245(19) 0.032(2) -0.0094(16) 0.0085(16) -0.0022(17) C14 0.0192(19) 0.0253(19) 0.0268(19) -0.0111(16) 0.0054(15) 0.0030(16) C15 0.025(2) 0.033(2) 0.043(2) -0.0158(19) -0.0035(18) 0.0145(19) C16 0.028(2) 0.045(3) 0.026(2) -0.0099(18) -0.0105(16) 0.014(2) C17 0.0158(18) 0.0240(19) 0.0200(17) -0.0062(15) 0.0014(14) -0.0001(15) C18 0.0145(17) 0.0221(18) 0.0153(16) -0.0033(14) 0.0019(13) -0.0036(15) C19 0.0192(19) 0.0234(19) 0.0228(18) -0.0066(15) 0.0037(14) -0.0030(16) C20 0.034(2) 0.032(2) 0.0227(19) -0.0068(16) -0.0006(16) -0.0026(19) C21 0.039(2) 0.040(2) 0.026(2) -0.0031(18) -0.0068(18) 0.004(2) C22 0.032(2) 0.036(2) 0.034(2) 0.0008(19) -0.0013(17) 0.010(2) C23 0.028(2) 0.0230(19) 0.0242(18) -0.0055(16) 0.0014(15) 0.0043(17) C24 0.0197(19) 0.0258(19) 0.0175(17) -0.0035(15) 0.0022(14) 0.0001(16) C25 0.026(2) 0.027(2) 0.0240(19) -0.0087(16) 0.0104(15) -0.0064(17) C26 0.022(2) 0.029(2) 0.0216(18) -0.0117(16) 0.0096(15) -0.0073(17) C27 0.025(2) 0.035(2) 0.034(2) -0.0110(18) -0.0020(17) 0.0107(19) C28 0.031(2) 0.047(3) 0.0223(19) -0.0125(18) -0.0056(16) 0.004(2) C29 0.0206(19) 0.026(2) 0.0241(18) -0.0110(16) 0.0060(15) -0.0051(16) C30 0.021(2) 0.028(2) 0.0266(19) -0.0086(16) 0.0049(15) -0.0071(17) C31 0.022(2) 0.026(2) 0.0258(19) -0.0047(16) 0.0047(15) -0.0059(17) C32 0.044(3) 0.045(3) 0.0197(19) -0.0023(18) -0.0005(17) -0.011(2) C33 0.048(3) 0.062(3) 0.034(2) 0.009(2) -0.009(2) 0.001(3) C34 0.045(3) 0.049(3) 0.058(3) 0.016(3) 0.006(2) 0.013(3) C35 0.039(3) 0.032(2) 0.042(2) -0.0036(19) 0.011(2) 0.001(2) C36 0.028(2) 0.029(2) 0.0275(19) -0.0119(17) 0.0118(16) -0.0104(18) N1A 0.071(3) 0.052(2) 0.054(2) 0.006(2) 0.030(2) 0.010(2) N2A 0.083(2) 0.064(2) 0.056(2) 0.003(2) 0.0246(19) -0.001(2) C37A 0.083(3) 0.064(2) 0.056(2) 0.007(2) 0.023(2) 0.014(2) C38A 0.084(3) 0.067(2) 0.053(2) 0.005(2) 0.019(2) 0.011(2) C39A 0.075(2) 0.062(2) 0.053(2) 0.008(2) 0.0190(19) 0.003(2) C40A 0.073(4) 0.061(4) 0.085(4) -0.006(4) 0.029(3) 0.000(3) C41A 0.094(2) 0.077(2) 0.070(2) 0.003(2) 0.025(2) -0.005(2) C42A 0.104(3) 0.089(3) 0.080(2) 0.007(2) 0.028(2) -0.004(3) C43A 0.111(3) 0.090(3) 0.088(3) 0.002(2) 0.023(3) -0.003(3) C44A 0.122(3) 0.104(3) 0.100(3) 0.009(3) 0.020(3) -0.008(3) C45A 0.128(4) 0.110(3) 0.112(3) 0.007(3) 0.014(3) -0.007(3) C46A 0.159(6) 0.130(5) 0.136(6) -0.009(5) 0.034(5) -0.004(6) N1B 0.071(3) 0.052(2) 0.054(2) 0.006(2) 0.030(2) 0.010(2) N2B 0.083(2) 0.064(2) 0.056(2) 0.003(2) 0.0246(19) -0.001(2) C37B 0.083(3) 0.064(2) 0.056(2) 0.007(2) 0.023(2) 0.014(2) C38B 0.084(3) 0.067(2) 0.053(2) 0.005(2) 0.019(2) 0.011(2) C39B 0.075(2) 0.062(2) 0.053(2) 0.008(2) 0.0190(19) 0.003(2) C40B 0.073(4) 0.061(4) 0.085(4) -0.006(4) 0.029(3) 0.000(3) C41B 0.094(2) 0.077(2) 0.070(2) 0.003(2) 0.025(2) -0.005(2) C42B 0.104(3) 0.089(3) 0.080(2) 0.007(2) 0.028(2) -0.004(3) C44B 0.122(3) 0.104(3) 0.100(3) 0.009(3) 0.020(3) -0.008(3) C43B 0.111(3) 0.090(3) 0.088(3) 0.002(2) 0.023(3) -0.003(3) C45B 0.128(4) 0.110(3) 0.112(3) 0.007(3) 0.014(3) -0.007(3) C46B 0.159(6) 0.130(5) 0.136(6) -0.009(5) 0.034(5) -0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O7 2.319(2) 4_565 ? Eu1 O1 2.332(3) . ? Eu1 O5 2.335(3) 4_566 ? Eu1 O6 2.338(2) 2_644 ? Eu1 O3 2.353(3) . ? Eu1 O2 2.364(3) 3_655 ? Eu1 Cl1 2.8323(9) . ? Eu1 C12 3.257(4) 2_644 ? Eu1 Eu1 4.3875(3) 3_655 ? Eu2 O11 2.296(3) 4_565 ? Eu2 O4 2.314(2) . ? Eu2 O10 2.332(2) 3 ? Eu2 O8 2.372(2) 4_565 ? Eu2 O9 2.403(2) . ? Eu2 O12 2.408(3) 2_545 ? Eu2 Cl1 2.8067(9) . ? Eu2 O11 3.009(3) 2_545 ? Eu2 C36 3.072(4) 2_545 ? Eu2 Eu2 4.1503(3) 3 ? O1 C1 1.243(4) . ? O2 C1 1.256(4) . ? O2 Eu1 2.364(3) 3_655 ? O3 C13 1.261(4) . ? O5 C12 1.250(4) . ? O5 Eu1 2.335(3) 4_565 ? O4 C13 1.256(4) . ? O6 C12 1.250(4) . ? O6 Eu1 2.338(2) 2_654 ? O7 C24 1.250(4) . ? O7 Eu1 2.319(2) 4_566 ? O8 C24 1.256(4) . ? O8 Eu2 2.372(2) 4_566 ? O9 C25 1.243(4) . ? O10 C25 1.265(4) . ? O10 Eu2 2.332(2) 3 ? O11 C36 1.261(4) . ? O11 Eu2 2.296(3) 4_566 ? O11 Eu2 3.009(3) 2 ? O12 C36 1.255(5) . ? O12 Eu2 2.408(3) 2 ? C1 C2 1.511(5) . ? C2 C3 1.373(5) . ? C2 C7 1.431(5) . ? C3 C4 1.397(5) . ? C3 H3A 0.9300 . ? C4 C5 1.366(5) . ? C4 H4A 0.9300 . ? C5 C6 1.432(5) . ? C5 C12 1.504(5) . ? C6 C11 1.423(5) . ? C6 C7 1.429(5) . ? C7 C8 1.419(5) . ? C8 C9 1.365(5) . ? C8 H8A 0.9300 . ? C9 C10 1.401(6) . ? C9 H9A 0.9300 . ? C10 C11 1.345(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 Eu1 3.257(4) 2_654 ? C13 C14 1.504(5) . ? C14 C15 1.371(5) . ? C14 C19 1.426(5) . ? C15 C16 1.389(5) . ? C15 H15A 0.9300 . ? C16 C17 1.375(5) . ? C16 H16A 0.9300 . ? C17 C18 1.431(4) . ? C17 C24 1.512(5) . ? C18 C23 1.418(5) . ? C18 C19 1.436(4) . ? C19 C20 1.408(5) . ? C20 C21 1.364(5) . ? C20 H20A 0.9300 . ? C21 C22 1.389(5) . ? C21 H21A 0.9300 . ? C22 C23 1.356(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.499(5) . ? C26 C27 1.370(5) . ? C26 C31 1.425(5) . ? C27 C28 1.406(5) . ? C27 H27A 0.9300 . ? C28 C29 1.369(5) . ? C28 H28A 0.9300 . ? C29 C30 1.443(5) . ? C29 C36 1.487(5) . ? C30 C35 1.407(6) . ? C30 C31 1.413(5) . ? C31 C32 1.432(5) . ? C32 C33 1.348(6) . ? C32 H32A 0.9300 . ? C33 C34 1.385(7) . ? C33 H33A 0.9300 . ? C34 C35 1.353(6) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 Eu2 3.072(4) 2 ? N1A C39A 1.304(7) . ? N1A C37A 1.319(8) . ? N1A C40A 1.478(10) . ? N2A C39A 1.307(9) . ? N2A C38A 1.339(7) . ? N2A C41A 1.489(9) . ? C37A C38A 1.437(14) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.514(8) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C42A C43A 1.616(8) . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C43A C44A 1.548(8) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C44A C45A 1.497(8) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.523(9) . ? C45A H45A 0.9700 . ? C45A H45D 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N1B C39B 1.315(9) . ? N1B C37B 1.323(9) . ? N1B C40B 1.479(12) . ? N2B C38B 1.321(10) . ? N2B C39B 1.327(11) . ? N2B C41B 1.514(12) . ? C37B C38B 1.449(17) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C39B H39B 0.9300 . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C41B C42B 1.580(10) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.607(10) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C44B C45B 1.487(10) . ? C44B C43B 1.543(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C45B C46B 1.548(10) . ? C45B H45B 0.9700 . ? C45B H45C 0.9700 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? C46B H46F 0.9600 . ? 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 O7 Eu1 O1 80.02(9) 4_565 . ? O7 Eu1 O5 146.68(11) 4_565 4_566 ? O1 Eu1 O5 77.52(11) . 4_566 ? O7 Eu1 O6 77.39(10) 4_565 2_644 ? O1 Eu1 O6 80.86(11) . 2_644 ? O5 Eu1 O6 122.26(10) 4_566 2_644 ? O7 Eu1 O3 82.25(10) 4_565 . ? O1 Eu1 O3 97.98(11) . . ? O5 Eu1 O3 76.88(10) 4_566 . ? O6 Eu1 O3 159.50(10) 2_644 . ? O7 Eu1 O2 140.36(10) 4_565 3_655 ? O1 Eu1 O2 124.72(9) . 3_655 ? O5 Eu1 O2 72.95(11) 4_566 3_655 ? O6 Eu1 O2 77.18(10) 2_644 3_655 ? O3 Eu1 O2 118.66(11) . 3_655 ? O7 Eu1 Cl1 76.88(7) 4_565 . ? O1 Eu1 Cl1 156.55(7) . . ? O5 Eu1 Cl1 125.04(8) 4_566 . ? O6 Eu1 Cl1 90.12(8) 2_644 . ? O3 Eu1 Cl1 82.98(7) . . ? O2 Eu1 Cl1 73.29(7) 3_655 . ? O7 Eu1 C12 91.41(9) 4_565 2_644 ? O1 Eu1 C12 72.48(10) . 2_644 ? O5 Eu1 C12 104.77(10) 4_566 2_644 ? O6 Eu1 C12 17.67(9) 2_644 2_644 ? O3 Eu1 C12 169.42(10) . 2_644 ? O2 Eu1 C12 71.46(10) 3_655 2_644 ? Cl1 Eu1 C12 103.90(7) . 2_644 ? O7 Eu1 Eu1 133.84(6) 4_565 3_655 ? O1 Eu1 Eu1 63.05(7) . 3_655 ? O5 Eu1 Eu1 51.87(7) 4_566 3_655 ? O6 Eu1 Eu1 70.56(7) 2_644 3_655 ? O3 Eu1 Eu1 127.28(7) . 3_655 ? O2 Eu1 Eu1 61.88(7) 3_655 3_655 ? Cl1 Eu1 Eu1 133.84(2) . 3_655 ? C12 Eu1 Eu1 52.95(6) 2_644 3_655 ? O11 Eu2 O4 98.33(10) 4_565 . ? O11 Eu2 O10 80.21(10) 4_565 3 ? O4 Eu2 O10 154.64(9) . 3 ? O11 Eu2 O8 80.67(9) 4_565 4_565 ? O4 Eu2 O8 76.68(9) . 4_565 ? O10 Eu2 O8 78.11(9) 3 4_565 ? O11 Eu2 O9 74.76(9) 4_565 . ? O4 Eu2 O9 73.86(9) . . ? O10 Eu2 O9 128.86(9) 3 . ? O8 Eu2 O9 137.98(9) 4_565 . ? O11 Eu2 O12 122.92(9) 4_565 2_545 ? O4 Eu2 O12 115.92(10) . 2_545 ? O10 Eu2 O12 84.83(10) 3 2_545 ? O8 Eu2 O12 148.07(10) 4_565 2_545 ? O9 Eu2 O12 73.16(10) . 2_545 ? O11 Eu2 Cl1 161.82(7) 4_565 . ? O4 Eu2 Cl1 83.30(7) . . ? O10 Eu2 Cl1 90.57(7) 3 . ? O8 Eu2 Cl1 82.11(6) 4_565 . ? O9 Eu2 Cl1 122.68(7) . . ? O12 Eu2 Cl1 71.18(7) 2_545 . ? O11 Eu2 O11 77.89(9) 4_565 2_545 ? O4 Eu2 O11 140.21(8) . 2_545 ? O10 Eu2 O11 64.62(8) 3 2_545 ? O8 Eu2 O11 139.44(8) 4_565 2_545 ? O9 Eu2 O11 66.90(8) . 2_545 ? O12 Eu2 O11 46.31(8) 2_545 2_545 ? Cl1 Eu2 O11 112.36(5) . 2_545 ? O11 Eu2 C36 100.63(10) 4_565 2_545 ? O4 Eu2 C36 128.87(10) . 2_545 ? O10 Eu2 C36 75.76(10) 3 2_545 ? O8 Eu2 C36 153.17(10) 4_565 2_545 ? O9 Eu2 C36 66.28(10) . 2_545 ? O12 Eu2 C36 22.57(9) 2_545 2_545 ? Cl1 Eu2 C36 92.12(7) . 2_545 ? O11 Eu2 C36 23.91(8) 2_545 2_545 ? O11 Eu2 Eu2 45.14(7) 4_565 3 ? O4 Eu2 Eu2 129.59(6) . 3 ? O10 Eu2 Eu2 66.12(6) 3 3 ? O8 Eu2 Eu2 117.46(6) 4_565 3 ? O9 Eu2 Eu2 64.54(6) . 3 ? O12 Eu2 Eu2 78.46(6) 2_545 3 ? Cl1 Eu2 Eu2 143.26(2) . 3 ? O11 Eu2 Eu2 32.74(5) 2_545 3 ? C36 Eu2 Eu2 55.90(7) 2_545 3 ? Eu2 Cl1 Eu1 111.78(3) . . ? C1 O1 Eu1 144.0(2) . . ? C1 O2 Eu1 143.7(2) . 3_655 ? C13 O3 Eu1 138.3(2) . . ? C12 O5 Eu1 164.5(3) . 4_565 ? C13 O4 Eu2 144.3(3) . . ? C12 O6 Eu1 127.7(2) . 2_654 ? C24 O7 Eu1 160.3(2) . 4_566 ? C24 O8 Eu2 133.1(2) . 4_566 ? C25 O9 Eu2 136.4(2) . . ? C25 O10 Eu2 139.3(2) . 3 ? C36 O11 Eu2 161.8(3) . 4_566 ? C36 O11 Eu2 80.8(2) . 2 ? Eu2 O11 Eu2 102.11(9) 4_566 2 ? C36 O12 Eu2 110.0(2) . 2 ? O1 C1 O2 125.7(3) . . ? O1 C1 C2 116.4(3) . . ? O2 C1 C2 117.7(3) . . ? C3 C2 C7 119.7(3) . . ? C3 C2 C1 117.4(3) . . ? C7 C2 C1 123.0(3) . . ? C2 C3 C4 120.9(4) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C5 C4 C3 121.4(3) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 C12 117.1(3) . . ? C6 C5 C12 122.9(3) . . ? C11 C6 C7 118.6(3) . . ? C11 C6 C5 122.8(3) . . ? C7 C6 C5 118.6(3) . . ? C8 C7 C6 118.4(3) . . ? C8 C7 C2 122.2(3) . . ? C6 C7 C2 119.3(3) . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.6(4) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C11 C10 C9 120.9(4) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C6 120.9(4) . . ? C10 C11 H11A 119.6 . . ? C6 C11 H11A 119.6 . . ? O5 C12 O6 123.8(3) . . ? O5 C12 C5 117.8(3) . . ? O6 C12 C5 118.5(3) . . ? O5 C12 Eu1 89.2(2) . 2_654 ? O6 C12 Eu1 34.58(17) . 2_654 ? C5 C12 Eu1 153.0(2) . 2_654 ? O4 C13 O3 124.1(3) . . ? O4 C13 C14 118.9(3) . . ? O3 C13 C14 116.9(3) . . ? C15 C14 C19 119.4(3) . . ? C15 C14 C13 116.5(3) . . ? C19 C14 C13 124.0(3) . . ? C14 C15 C16 121.9(4) . . ? C14 C15 H15A 119.1 . . ? C16 C15 H15A 119.1 . . ? C17 C16 C15 121.3(3) . . ? C17 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C16 C17 C18 119.0(3) . . ? C16 C17 C24 116.1(3) . . ? C18 C17 C24 124.9(3) . . ? C23 C18 C17 122.3(3) . . ? C23 C18 C19 118.1(3) . . ? C17 C18 C19 119.6(3) . . ? C20 C19 C14 123.1(3) . . ? C20 C19 C18 118.2(3) . . ? C14 C19 C18 118.7(3) . . ? C21 C20 C19 121.6(4) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C20 C21 C22 120.1(4) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C18 121.1(3) . . ? C22 C23 H23A 119.4 . . ? C18 C23 H23A 119.4 . . ? O7 C24 O8 125.1(3) . . ? O7 C24 C17 114.9(3) . . ? O8 C24 C17 120.0(3) . . ? O9 C25 O10 126.0(3) . . ? O9 C25 C26 118.6(3) . . ? O10 C25 C26 115.3(3) . . ? C27 C26 C31 119.2(3) . . ? C27 C26 C25 118.5(4) . . ? C31 C26 C25 122.1(3) . . ? C26 C27 C28 121.3(4) . . ? C26 C27 H27A 119.3 . . ? C28 C27 H27A 119.3 . . ? C29 C28 C27 120.5(3) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 119.9(3) . . ? C28 C29 C36 119.1(3) . . ? C30 C29 C36 120.8(3) . . ? C35 C30 C31 119.4(4) . . ? C35 C30 C29 122.3(3) . . ? C31 C30 C29 118.3(4) . . ? C30 C31 C26 120.2(3) . . ? C30 C31 C32 118.0(4) . . ? C26 C31 C32 121.8(3) . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 121.4(4) . . ? C32 C33 H33A 119.3 . . ? C34 C33 H33A 119.3 . . ? C35 C34 C33 120.6(4) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C30 120.5(4) . . ? C34 C35 H35A 119.7 . . ? C30 C35 H35A 119.7 . . ? O12 C36 O11 122.0(3) . . ? O12 C36 C29 118.6(3) . . ? O11 C36 C29 119.3(3) . . ? O12 C36 Eu2 47.46(18) . 2 ? O11 C36 Eu2 75.2(2) . 2 ? C29 C36 Eu2 164.6(3) . 2 ? C39A N1A C37A 110.0(8) . . ? C39A N1A C40A 128.0(8) . . ? C37A N1A C40A 121.9(7) . . ? C39A N2A C38A 111.6(8) . . ? C39A N2A C41A 123.9(7) . . ? C38A N2A C41A 124.5(8) . . ? N1A C37A C38A 106.9(9) . . ? N1A C37A H37A 126.5 . . ? C38A C37A H37A 126.5 . . ? N2A C38A C37A 102.8(9) . . ? N2A C38A H38A 128.6 . . ? C37A C38A H38A 128.6 . . ? N1A C39A N2A 108.5(7) . . ? N1A C39A H39A 125.7 . . ? N2A C39A H39A 125.7 . . ? N2A C41A C42A 121.4(8) . . ? N2A C41A H41A 107.0 . . ? C42A C41A H41A 107.0 . . ? N2A C41A H41B 107.0 . . ? C42A C41A H41B 107.0 . . ? H41A C41A H41B 106.7 . . ? C41A C42A C43A 98.5(7) . . ? C41A C42A H42A 112.1 . . ? C43A C42A H42A 112.1 . . ? C41A C42A H42B 112.1 . . ? C43A C42A H42B 112.1 . . ? H42A C42A H42B 109.7 . . ? C44A C43A C42A 93.9(7) . . ? C44A C43A H43A 112.9 . . ? C42A C43A H43A 112.9 . . ? C44A C43A H43B 112.9 . . ? C42A C43A H43B 112.9 . . ? H43A C43A H43B 110.4 . . ? C45A C44A C43A 118.1(9) . . ? C45A C44A H44A 107.8 . . ? C43A C44A H44A 107.8 . . ? C45A C44A H44B 107.8 . . ? C43A C44A H44B 107.8 . . ? H44A C44A H44B 107.1 . . ? C44A C45A C46A 109.3(8) . . ? C44A C45A H45A 109.8 . . ? C46A C45A H45A 109.8 . . ? C44A C45A H45D 109.8 . . ? C46A C45A H45D 109.8 . . ? H45A C45A H45D 108.3 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C39B N1B C37B 108.6(15) . . ? C39B N1B C40B 128.8(13) . . ? C37B N1B C40B 122.3(10) . . ? C38B N2B C39B 110.2(10) . . ? C38B N2B C41B 131.2(12) . . ? C39B N2B C41B 118.6(10) . . ? N1B C37B C38B 105.6(15) . . ? N1B C37B H37B 127.2 . . ? C38B C37B H37B 127.2 . . ? N2B C38B C37B 104.0(13) . . ? N2B C38B H38B 128.0 . . ? C37B C38B H38B 128.0 . . ? N1B C39B N2B 108.8(11) . . ? N1B C39B H39B 125.6 . . ? N2B C39B H39B 125.6 . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N2B C41B C42B 133.5(15) . . ? N2B C41B H41C 103.8 . . ? C42B C41B H41C 103.8 . . ? N2B C41B H41D 103.8 . . ? C42B C41B H41D 103.8 . . ? H41C C41B H41D 105.4 . . ? C41B C42B C43B 100.3(13) . . ? C41B C42B H42C 111.7 . . ? C43B C42B H42C 111.7 . . ? C41B C42B H42D 111.7 . . ? C43B C42B H42D 111.7 . . ? H42C C42B H42D 109.5 . . ? C45B C44B C43B 129.0(13) . . ? C45B C44B H44C 105.1 . . ? C43B C44B H44C 105.1 . . ? C45B C44B H44D 105.1 . . ? C43B C44B H44D 105.1 . . ? H44C C44B H44D 105.9 . . ? C44B C43B C42B 118.6(13) . . ? C44B C43B H43C 107.7 . . ? C42B C43B H43C 107.7 . . ? C44B C43B H43D 107.7 . . ? C42B C43B H43D 107.7 . . ? H43C C43B H43D 107.1 . . ? C44B C45B C46B 111.9(10) . . ? C44B C45B H45B 109.2 . . ? C46B C45B H45B 109.2 . . ? C44B C45B H45C 109.2 . . ? C46B C45B H45C 109.2 . . ? H45B C45B H45C 107.9 . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C45B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Eu2 Cl1 Eu1 71.1(2) 4_565 . . . ? O4 Eu2 Cl1 Eu1 -25.24(7) . . . . ? O10 Eu2 Cl1 Eu1 130.09(7) 3 . . . ? O8 Eu2 Cl1 Eu1 52.17(7) 4_565 . . . ? O9 Eu2 Cl1 Eu1 -91.17(9) . . . . ? O12 Eu2 Cl1 Eu1 -145.57(9) 2_545 . . . ? O11 Eu2 Cl1 Eu1 -167.27(6) 2_545 . . . ? C36 Eu2 Cl1 Eu1 -154.14(8) 2_545 . . . ? Eu2 Eu2 Cl1 Eu1 178.519(11) 3 . . . ? O7 Eu1 Cl1 Eu2 -39.52(8) 4_565 . . . ? O1 Eu1 Cl1 Eu2 -49.8(2) . . . . ? O5 Eu1 Cl1 Eu2 112.67(9) 4_566 . . . ? O6 Eu1 Cl1 Eu2 -116.53(8) 2_644 . . . ? O3 Eu1 Cl1 Eu2 44.11(8) . . . . ? O2 Eu1 Cl1 Eu2 166.90(8) 3_655 . . . ? C12 Eu1 Cl1 Eu2 -127.70(7) 2_644 . . . ? Eu1 Eu1 Cl1 Eu2 -179.179(14) 3_655 . . . ? O7 Eu1 O1 C1 -154.6(5) 4_565 . . . ? O5 Eu1 O1 C1 50.2(5) 4_566 . . . ? O6 Eu1 O1 C1 -75.9(5) 2_644 . . . ? O3 Eu1 O1 C1 124.8(5) . . . . ? O2 Eu1 O1 C1 -8.5(5) 3_655 . . . ? Cl1 Eu1 O1 C1 -144.5(4) . . . . ? C12 Eu1 O1 C1 -59.9(5) 2_644 . . . ? Eu1 Eu1 O1 C1 -3.1(4) 3_655 . . . ? O7 Eu1 O3 C13 30.4(4) 4_565 . . . ? O1 Eu1 O3 C13 109.1(4) . . . . ? O5 Eu1 O3 C13 -175.8(4) 4_566 . . . ? O6 Eu1 O3 C13 23.8(6) 2_644 . . . ? O2 Eu1 O3 C13 -113.9(4) 3_655 . . . ? Cl1 Eu1 O3 C13 -47.3(4) . . . . ? C12 Eu1 O3 C13 83.9(7) 2_644 . . . ? Eu1 Eu1 O3 C13 171.1(4) 3_655 . . . ? O11 Eu2 O4 C13 160.9(4) 4_565 . . . ? O10 Eu2 O4 C13 -114.4(4) 3 . . . ? O8 Eu2 O4 C13 -120.8(4) 4_565 . . . ? O9 Eu2 O4 C13 89.5(4) . . . . ? O12 Eu2 O4 C13 27.9(4) 2_545 . . . ? Cl1 Eu2 O4 C13 -37.4(4) . . . . ? O11 Eu2 O4 C13 79.9(4) 2_545 . . . ? C36 Eu2 O4 C13 50.0(4) 2_545 . . . ? Eu2 Eu2 O4 C13 124.4(4) 3 . . . ? O11 Eu2 O9 C25 17.4(4) 4_565 . . . ? O4 Eu2 O9 C25 121.0(4) . . . . ? O10 Eu2 O9 C25 -46.1(4) 3 . . . ? O8 Eu2 O9 C25 73.8(4) 4_565 . . . ? O12 Eu2 O9 C25 -114.8(4) 2_545 . . . ? Cl1 Eu2 O9 C25 -168.3(3) . . . . ? O11 Eu2 O9 C25 -65.7(4) 2_545 . . . ? C36 Eu2 O9 C25 -91.8(4) 2_545 . . . ? Eu2 Eu2 O9 C25 -29.8(3) 3 . . . ? Eu1 O1 C1 O2 -4.2(8) . . . . ? Eu1 O1 C1 C2 172.7(3) . . . . ? Eu1 O2 C1 O1 19.1(8) 3_655 . . . ? Eu1 O2 C1 C2 -157.7(3) 3_655 . . . ? O1 C1 C2 C3 -41.7(5) . . . . ? O2 C1 C2 C3 135.5(4) . . . . ? O1 C1 C2 C7 138.7(4) . . . . ? O2 C1 C2 C7 -44.2(5) . . . . ? C7 C2 C3 C4 1.0(6) . . . . ? C1 C2 C3 C4 -178.7(4) . . . . ? C2 C3 C4 C5 0.6(7) . . . . ? C3 C4 C5 C6 -2.8(6) . . . . ? C3 C4 C5 C12 174.9(4) . . . . ? C4 C5 C6 C11 -173.9(4) . . . . ? C12 C5 C6 C11 8.6(6) . . . . ? C4 C5 C6 C7 3.4(6) . . . . ? C12 C5 C6 C7 -174.1(3) . . . . ? C11 C6 C7 C8 -2.4(5) . . . . ? C5 C6 C7 C8 -179.8(3) . . . . ? C11 C6 C7 C2 175.5(3) . . . . ? C5 C6 C7 C2 -1.9(5) . . . . ? C3 C2 C7 C8 177.6(4) . . . . ? C1 C2 C7 C8 -2.8(6) . . . . ? C3 C2 C7 C6 -0.2(6) . . . . ? C1 C2 C7 C6 179.4(3) . . . . ? C6 C7 C8 C9 1.3(6) . . . . ? C2 C7 C8 C9 -176.5(4) . . . . ? C7 C8 C9 C10 0.5(7) . . . . ? C8 C9 C10 C11 -1.2(7) . . . . ? C9 C10 C11 C6 0.1(7) . . . . ? C7 C6 C11 C10 1.8(6) . . . . ? C5 C6 C11 C10 179.0(4) . . . . ? Eu1 O5 C12 O6 24.6(14) 4_565 . . . ? Eu1 O5 C12 C5 -153.7(9) 4_565 . . . ? Eu1 O5 C12 Eu1 25.2(11) 4_565 . . 2_654 ? Eu1 O6 C12 O5 1.2(6) 2_654 . . . ? Eu1 O6 C12 C5 179.5(2) 2_654 . . . ? C4 C5 C12 O5 36.7(6) . . . . ? C6 C5 C12 O5 -145.7(4) . . . . ? C4 C5 C12 O6 -141.7(4) . . . . ? C6 C5 C12 O6 35.9(6) . . . . ? C4 C5 C12 Eu1 -141.1(5) . . . 2_654 ? C6 C5 C12 Eu1 36.6(8) . . . 2_654 ? Eu2 O4 C13 O3 62.4(6) . . . . ? Eu2 O4 C13 C14 -114.4(4) . . . . ? Eu1 O3 C13 O4 4.6(7) . . . . ? Eu1 O3 C13 C14 -178.6(3) . . . . ? O4 C13 C14 C15 143.3(4) . . . . ? O3 C13 C14 C15 -33.8(5) . . . . ? O4 C13 C14 C19 -35.7(6) . . . . ? O3 C13 C14 C19 147.2(4) . . . . ? C19 C14 C15 C16 0.9(6) . . . . ? C13 C14 C15 C16 -178.1(4) . . . . ? C14 C15 C16 C17 0.9(7) . . . . ? C15 C16 C17 C18 -0.6(6) . . . . ? C15 C16 C17 C24 -179.6(4) . . . . ? C16 C17 C18 C23 -178.7(4) . . . . ? C24 C17 C18 C23 0.1(6) . . . . ? C16 C17 C18 C19 -1.4(5) . . . . ? C24 C17 C18 C19 177.5(3) . . . . ? C15 C14 C19 C20 175.4(4) . . . . ? C13 C14 C19 C20 -5.6(6) . . . . ? C15 C14 C19 C18 -2.8(6) . . . . ? C13 C14 C19 C18 176.1(3) . . . . ? C23 C18 C19 C20 2.2(5) . . . . ? C17 C18 C19 C20 -175.3(3) . . . . ? C23 C18 C19 C14 -179.5(3) . . . . ? C17 C18 C19 C14 3.1(5) . . . . ? C14 C19 C20 C21 -179.4(4) . . . . ? C18 C19 C20 C21 -1.2(6) . . . . ? C19 C20 C21 C22 -0.5(6) . . . . ? C20 C21 C22 C23 1.0(7) . . . . ? C21 C22 C23 C18 0.1(6) . . . . ? C17 C18 C23 C22 175.7(4) . . . . ? C19 C18 C23 C22 -1.7(6) . . . . ? Eu1 O7 C24 O8 6.1(11) 4_566 . . . ? Eu1 O7 C24 C17 -171.9(6) 4_566 . . . ? Eu2 O8 C24 O7 -33.3(6) 4_566 . . . ? Eu2 O8 C24 C17 144.5(3) 4_566 . . . ? C16 C17 C24 O7 32.7(5) . . . . ? C18 C17 C24 O7 -146.1(4) . . . . ? C16 C17 C24 O8 -145.3(4) . . . . ? C18 C17 C24 O8 35.8(5) . . . . ? Eu2 O9 C25 O10 32.6(6) . . . . ? Eu2 O9 C25 C26 -150.7(3) . . . . ? Eu2 O10 C25 O9 2.6(7) 3 . . . ? Eu2 O10 C25 C26 -174.2(3) 3 . . . ? O9 C25 C26 C27 -46.3(5) . . . . ? O10 C25 C26 C27 130.8(4) . . . . ? O9 C25 C26 C31 138.7(4) . . . . ? O10 C25 C26 C31 -44.2(5) . . . . ? C31 C26 C27 C28 5.4(6) . . . . ? C25 C26 C27 C28 -169.7(4) . . . . ? C26 C27 C28 C29 1.5(7) . . . . ? C27 C28 C29 C30 -7.7(6) . . . . ? C27 C28 C29 C36 167.6(4) . . . . ? C28 C29 C30 C35 -170.5(4) . . . . ? C36 C29 C30 C35 14.3(6) . . . . ? C28 C29 C30 C31 6.9(6) . . . . ? C36 C29 C30 C31 -168.3(3) . . . . ? C35 C30 C31 C26 177.4(4) . . . . ? C29 C30 C31 C26 0.0(5) . . . . ? C35 C30 C31 C32 -0.4(6) . . . . ? C29 C30 C31 C32 -177.9(3) . . . . ? C27 C26 C31 C30 -6.0(6) . . . . ? C25 C26 C31 C30 168.9(3) . . . . ? C27 C26 C31 C32 171.8(4) . . . . ? C25 C26 C31 C32 -13.3(6) . . . . ? C30 C31 C32 C33 1.5(6) . . . . ? C26 C31 C32 C33 -176.3(4) . . . . ? C31 C32 C33 C34 -1.2(7) . . . . ? C32 C33 C34 C35 -0.1(8) . . . . ? C33 C34 C35 C30 1.2(7) . . . . ? C31 C30 C35 C34 -0.9(6) . . . . ? C29 C30 C35 C34 176.5(4) . . . . ? Eu2 O12 C36 O11 11.0(5) 2 . . . ? Eu2 O12 C36 C29 -172.0(3) 2 . . . ? Eu2 O11 C36 O12 -109.3(8) 4_566 . . . ? Eu2 O11 C36 O12 -8.4(4) 2 . . . ? Eu2 O11 C36 C29 73.6(10) 4_566 . . . ? Eu2 O11 C36 C29 174.6(4) 2 . . . ? Eu2 O11 C36 Eu2 -101.0(8) 4_566 . . 2 ? C28 C29 C36 O12 -132.5(4) . . . . ? C30 C29 C36 O12 42.6(5) . . . . ? C28 C29 C36 O11 44.6(5) . . . . ? C30 C29 C36 O11 -140.2(4) . . . . ? C28 C29 C36 Eu2 -155.4(8) . . . 2 ? C30 C29 C36 Eu2 19.8(12) . . . 2 ? C39A N1A C37A C38A -2(2) . . . . ? C40A N1A C37A C38A 176.5(9) . . . . ? C39A N2A C38A C37A -3(2) . . . . ? C41A N2A C38A C37A 177.1(12) . . . . ? N1A C37A C38A N2A 3.0(18) . . . . ? C37A N1A C39A N2A 0(3) . . . . ? C40A N1A C39A N2A -178.5(12) . . . . ? C38A N2A C39A N1A 3(3) . . . . ? C41A N2A C39A N1A -177.9(12) . . . . ? C39A N2A C41A C42A 169.2(19) . . . . ? C38A N2A C41A C42A -11.3(14) . . . . ? N2A C41A C42A C43A -73.0(11) . . . . ? C41A C42A C43A C44A -168.7(8) . . . . ? C42A C43A C44A C45A -96.6(11) . . . . ? C43A C44A C45A C46A -111.2(13) . . . . ? C39B N1B C37B C38B -17(4) . . . . ? C40B N1B C37B C38B 169(2) . . . . ? C39B N2B C38B C37B -6(5) . . . . ? C41B N2B C38B C37B 174.7(18) . . . . ? N1B C37B C38B N2B 14(3) . . . . ? C37B N1B C39B N2B 13(5) . . . . ? C40B N1B C39B N2B -173(2) . . . . ? C38B N2B C39B N1B -4(6) . . . . ? C41B N2B C39B N1B 175(3) . . . . ? C38B N2B C41B C42B -133(3) . . . . ? C39B N2B C41B C42B 48(4) . . . . ? N2B C41B C42B C43B 128.3(19) . . . . ? C45B C44B C43B C42B -150(2) . . . . ? C41B C42B C43B C44B -124.0(19) . . . . ? C43B C44B C45B C46B -25(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.305 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.120 #===END data_compound-7 _database_code_depnum_ccdc_archive 'CCDC 876527' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Gd2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl Gd2 N2 O12' _chemical_formula_weight 1159.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.7374(3) _cell_length_b 14.7992(3) _cell_length_c 15.9201(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.7447(17) _cell_angle_gamma 90.00 _cell_volume 4164.69(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13652 _cell_measurement_theta_min 2.5383 _cell_measurement_theta_max 28.8671 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 3.290 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.87621 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18150 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8650 _reflns_number_gt 7374 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0364P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8650 _refine_ls_number_parameters 605 _refine_ls_number_restraints 951 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.378316(8) 0.024717(10) -0.004639(9) 0.01385(5) Uani 1 1 d . . . Gd2 Gd 0.116458(8) 0.011929(11) -0.001180(9) 0.01454(5) Uani 1 1 d . . . Cl1 Cl 0.25214(5) -0.08359(6) 0.02419(6) 0.0302(2) Uani 1 1 d . . . O1 O 0.44968(15) 0.1243(2) -0.07737(18) 0.0377(7) Uani 1 1 d . . . O2 O 0.57452(15) 0.1066(2) -0.06429(19) 0.0386(7) Uani 1 1 d . . . O3 O 0.31538(15) 0.1297(2) 0.07397(18) 0.0395(7) Uani 1 1 d . . . O5 O 0.47129(16) 0.4292(2) -0.40174(18) 0.0434(8) Uani 1 1 d . . . O4 O 0.19317(14) 0.13442(18) 0.03118(17) 0.0313(6) Uani 1 1 d . . . O6 O 0.59588(16) 0.4314(2) -0.38331(17) 0.0398(7) Uani 1 1 d . . . O7 O 0.28888(14) 0.4299(2) 0.39017(15) 0.0320(6) Uani 1 1 d . . . O8 O 0.16506(13) 0.45361(19) 0.36867(14) 0.0267(6) Uani 1 1 d . . . O9 O 0.06179(14) 0.08915(19) 0.11054(16) 0.0324(6) Uani 1 1 d . . . O10 O -0.06371(15) 0.10142(19) 0.08769(16) 0.0328(6) Uani 1 1 d . . . O11 O 0.01549(15) 0.4114(2) 0.43510(16) 0.0336(6) Uani 1 1 d . . . O12 O -0.10481(15) 0.4039(2) 0.39108(18) 0.0391(7) Uani 1 1 d . . . C1 C 0.5148(2) 0.1440(3) -0.0942(2) 0.0258(8) Uani 1 1 d . . . C2 C 0.52216(19) 0.2176(2) -0.1585(2) 0.0234(7) Uani 1 1 d . . . C3 C 0.4713(2) 0.2159(3) -0.2290(2) 0.0313(9) Uani 1 1 d . . . H3A H 0.4338 0.1718 -0.2340 0.038 Uiso 1 1 calc R . . C4 C 0.4757(2) 0.2801(3) -0.2932(2) 0.0313(9) Uani 1 1 d . . . H4A H 0.4414 0.2773 -0.3406 0.038 Uiso 1 1 calc R . . C5 C 0.52903(19) 0.3465(3) -0.2877(2) 0.0240(8) Uani 1 1 d . . . C6 C 0.58104(18) 0.3534(2) -0.2143(2) 0.0223(7) Uani 1 1 d . . . C7 C 0.57807(19) 0.2870(3) -0.1495(2) 0.0225(7) Uani 1 1 d . . . C8 C 0.6299(2) 0.2941(3) -0.0766(2) 0.0327(9) Uani 1 1 d . . . H8A H 0.6301 0.2503 -0.0347 0.039 Uiso 1 1 calc R . . C9 C 0.6792(2) 0.3648(3) -0.0679(3) 0.0401(10) Uani 1 1 d . . . H9A H 0.7122 0.3691 -0.0196 0.048 Uiso 1 1 calc R . . C10 C 0.6812(2) 0.4304(3) -0.1299(3) 0.0372(10) Uani 1 1 d . . . H10A H 0.7152 0.4781 -0.1224 0.045 Uiso 1 1 calc R . . C11 C 0.6337(2) 0.4258(3) -0.2019(2) 0.0306(8) Uani 1 1 d . . . H11A H 0.6358 0.4701 -0.2430 0.037 Uiso 1 1 calc R . . C12 C 0.5322(2) 0.4075(3) -0.3630(2) 0.0281(8) Uani 1 1 d . . . C13 C 0.2499(2) 0.1618(3) 0.0769(2) 0.0263(8) Uani 1 1 d . . . C14 C 0.23958(19) 0.2336(3) 0.1410(2) 0.0256(8) Uani 1 1 d . . . C15 C 0.2830(2) 0.2261(3) 0.2164(2) 0.0349(10) Uani 1 1 d . . . H15A H 0.3175 0.1788 0.2238 0.042 Uiso 1 1 calc R . . C16 C 0.2767(2) 0.2870(3) 0.2815(2) 0.0338(9) Uani 1 1 d . . . H16A H 0.3077 0.2802 0.3312 0.041 Uiso 1 1 calc R . . C17 C 0.22597(18) 0.3569(2) 0.2747(2) 0.0216(7) Uani 1 1 d . . . C18 C 0.17894(18) 0.3679(2) 0.1971(2) 0.0186(7) Uani 1 1 d . . . C19 C 0.18690(18) 0.3064(2) 0.1297(2) 0.0212(7) Uani 1 1 d . . . C20 C 0.1434(2) 0.3220(3) 0.0516(2) 0.0317(9) Uani 1 1 d . . . H20A H 0.1488 0.2836 0.0062 0.038 Uiso 1 1 calc R . . C21 C 0.0943(2) 0.3922(3) 0.0428(2) 0.0361(10) Uani 1 1 d . . . H21A H 0.0662 0.4012 -0.0085 0.043 Uiso 1 1 calc R . . C22 C 0.0853(2) 0.4509(3) 0.1094(2) 0.0341(9) Uani 1 1 d . . . H22A H 0.0513 0.4986 0.1022 0.041 Uiso 1 1 calc R . . C23 C 0.1258(2) 0.4392(3) 0.1851(2) 0.0257(8) Uani 1 1 d . . . H23A H 0.1185 0.4784 0.2294 0.031 Uiso 1 1 calc R . . C24 C 0.22604(19) 0.4189(2) 0.3501(2) 0.0216(7) Uani 1 1 d . . . C25 C 0.0003(2) 0.1263(3) 0.1211(2) 0.0253(8) Uani 1 1 d . . . C26 C -0.0009(2) 0.2044(3) 0.1809(2) 0.0250(8) Uani 1 1 d . . . C27 C 0.0393(2) 0.1970(3) 0.2574(2) 0.0326(9) Uani 1 1 d . . . H27A H 0.0730 0.1492 0.2673 0.039 Uiso 1 1 calc R . . C28 C 0.0308(2) 0.2603(3) 0.3215(2) 0.0333(9) Uani 1 1 d . . . H28A H 0.0589 0.2541 0.3731 0.040 Uiso 1 1 calc R . . C29 C -0.0185(2) 0.3311(3) 0.3088(2) 0.0261(8) Uani 1 1 d . . . C30 C -0.0553(2) 0.3467(3) 0.2268(2) 0.0260(8) Uani 1 1 d . . . C31 C -0.04630(19) 0.2821(3) 0.1623(2) 0.0242(7) Uani 1 1 d . . . C32 C -0.0810(2) 0.2994(3) 0.0799(2) 0.0371(10) Uani 1 1 d . . . H32A H -0.0765 0.2576 0.0371 0.045 Uiso 1 1 calc R . . C33 C -0.1207(3) 0.3773(4) 0.0639(3) 0.0494(12) Uani 1 1 d . . . H33A H -0.1427 0.3882 0.0098 0.059 Uiso 1 1 calc R . . C34 C -0.1288(3) 0.4406(3) 0.1267(3) 0.0478(11) Uani 1 1 d . . . H34A H -0.1554 0.4936 0.1139 0.057 Uiso 1 1 calc R . . C35 C -0.0982(2) 0.4262(3) 0.2072(3) 0.0381(10) Uani 1 1 d . . . H35A H -0.1054 0.4684 0.2491 0.046 Uiso 1 1 calc R . . C36 C -0.0366(2) 0.3866(3) 0.3825(2) 0.0281(8) Uani 1 1 d . . . N1A N 0.2345(4) -0.2684(4) 0.2711(4) 0.0580(11) Uani 0.644(4) 1 d PDU A 1 N2A N 0.3025(4) -0.1495(5) 0.2698(4) 0.0638(11) Uani 0.644(4) 1 d PDU A 1 C37A C 0.2845(4) -0.2683(7) 0.3408(5) 0.0652(12) Uani 0.644(4) 1 d PDU A 1 H37A H 0.2882 -0.3129 0.3822 0.078 Uiso 0.644(4) 1 calc PR A 1 C38A C 0.3246(5) -0.1986(6) 0.3404(5) 0.0672(12) Uani 0.644(4) 1 d PDU A 1 H38A H 0.3629 -0.1830 0.3812 0.081 Uiso 0.644(4) 1 calc PR A 1 C39A C 0.2469(4) -0.1940(5) 0.2280(4) 0.0614(11) Uani 0.644(4) 1 d PDU A 1 H39A H 0.2210 -0.1763 0.1775 0.074 Uiso 0.644(4) 1 calc PR A 1 C40A C 0.1794(5) -0.3376(6) 0.2499(6) 0.0730(18) Uani 0.644(4) 1 d PDU A 1 H40A H 0.1516 -0.3228 0.1974 0.109 Uiso 0.644(4) 1 calc PR A 1 H40B H 0.1453 -0.3418 0.2934 0.109 Uiso 0.644(4) 1 calc PR A 1 H40C H 0.2046 -0.3945 0.2446 0.109 Uiso 0.644(4) 1 calc PR A 1 C41A C 0.3310(5) -0.0613(6) 0.2391(6) 0.0764(12) Uani 0.644(4) 1 d PDU A 1 H41A H 0.2873 -0.0230 0.2252 0.092 Uiso 0.644(4) 1 calc PR A 1 H41B H 0.3538 -0.0731 0.1868 0.092 Uiso 0.644(4) 1 calc PR A 1 C43A C 0.3426(6) 0.0374(8) 0.3685(7) 0.0920(14) Uani 0.644(4) 1 d PDU A 1 H43A H 0.3039 0.0800 0.3476 0.110 Uiso 0.644(4) 1 calc PR A 1 H43B H 0.3216 -0.0069 0.4050 0.110 Uiso 0.644(4) 1 calc PR A 1 C42A C 0.3871(6) -0.0073(7) 0.2951(6) 0.0830(13) Uani 0.644(4) 1 d PDU A 1 H42A H 0.4097 0.0395 0.2626 0.100 Uiso 0.644(4) 1 calc PR A 1 H42B H 0.4271 -0.0464 0.3193 0.100 Uiso 0.644(4) 1 calc PR A 1 C44A C 0.4169(6) 0.0850(8) 0.4104(6) 0.1018(15) Uani 0.644(4) 1 d PDU A 1 H44A H 0.4595 0.0497 0.3943 0.122 Uiso 0.644(4) 1 calc PR A 1 H44B H 0.4202 0.1435 0.3835 0.122 Uiso 0.644(4) 1 calc PR A 1 C45A C 0.4298(7) 0.1012(9) 0.5072(6) 0.1108(19) Uani 0.644(4) 1 d PDU A 1 H45A H 0.4364 0.0440 0.5367 0.133 Uiso 0.644(4) 1 calc PR A 1 H45B H 0.4747 0.1377 0.5201 0.133 Uiso 0.644(4) 1 calc PR A 1 C46A C 0.3599(8) 0.1501(10) 0.5338(9) 0.139(3) Uani 0.644(4) 1 d PDU A 1 H46A H 0.3673 0.1654 0.5925 0.208 Uiso 0.644(4) 1 calc PR A 1 H46B H 0.3166 0.1114 0.5245 0.208 Uiso 0.644(4) 1 calc PR A 1 H46C H 0.3519 0.2043 0.5011 0.208 Uiso 0.644(4) 1 calc PR A 1 N1B N 0.2072(6) -0.2812(6) 0.2286(7) 0.0580(11) Uani 0.356(4) 1 d PDU A 2 N2B N 0.2902(6) -0.2075(7) 0.2941(7) 0.0638(11) Uani 0.356(4) 1 d PDU A 2 C37B C 0.2173(8) -0.3202(10) 0.3061(7) 0.0652(12) Uani 0.356(4) 1 d PDU A 2 H37B H 0.1921 -0.3700 0.3259 0.078 Uiso 0.356(4) 1 calc PR A 2 C38B C 0.2681(8) -0.2740(10) 0.3448(10) 0.0672(12) Uani 0.356(4) 1 d PDU A 2 H38B H 0.2876 -0.2839 0.4000 0.081 Uiso 0.356(4) 1 calc PR A 2 C39B C 0.2534(6) -0.2098(8) 0.2215(7) 0.0614(11) Uani 0.356(4) 1 d PDU A 2 H39B H 0.2574 -0.1718 0.1756 0.074 Uiso 0.356(4) 1 calc PR A 2 C40B C 0.1525(8) -0.3148(11) 0.1630(8) 0.0730(18) Uani 0.356(4) 1 d PDU A 2 H40D H 0.1537 -0.2777 0.1137 0.109 Uiso 0.356(4) 1 calc PR A 2 H40E H 0.1028 -0.3128 0.1826 0.109 Uiso 0.356(4) 1 calc PR A 2 H40F H 0.1648 -0.3759 0.1495 0.109 Uiso 0.356(4) 1 calc PR A 2 C41B C 0.3495(7) -0.1462(9) 0.3280(9) 0.0764(12) Uani 0.356(4) 1 d PDU A 2 H41C H 0.3958 -0.1785 0.3452 0.092 Uiso 0.356(4) 1 calc PR A 2 H41D H 0.3337 -0.1119 0.3754 0.092 Uiso 0.356(4) 1 calc PR A 2 C42B C 0.3592(12) -0.0859(10) 0.2528(9) 0.0830(13) Uani 0.356(4) 1 d PDU A 2 H42C H 0.3262 -0.1025 0.2036 0.100 Uiso 0.356(4) 1 calc PR A 2 H42D H 0.4112 -0.0822 0.2387 0.100 Uiso 0.356(4) 1 calc PR A 2 C43B C 0.3328(11) -0.0005(12) 0.2968(11) 0.0920(14) Uani 0.356(4) 1 d PDU A 2 H43C H 0.2806 -0.0088 0.3092 0.110 Uiso 0.356(4) 1 calc PR A 2 H43D H 0.3342 0.0500 0.2581 0.110 Uiso 0.356(4) 1 calc PR A 2 C44B C 0.3820(12) 0.0245(14) 0.3819(12) 0.1018(15) Uani 0.356(4) 1 d PDU A 2 H44C H 0.3873 -0.0291 0.4170 0.122 Uiso 0.356(4) 1 calc PR A 2 H44D H 0.4322 0.0422 0.3683 0.122 Uiso 0.356(4) 1 calc PR A 2 C45B C 0.3483(11) 0.1008(14) 0.4323(12) 0.1108(19) Uani 0.356(4) 1 d PDU A 2 H45C H 0.3223 0.1428 0.3932 0.133 Uiso 0.356(4) 1 calc PR A 2 H45D H 0.3110 0.0751 0.4667 0.133 Uiso 0.356(4) 1 calc PR A 2 C46B C 0.4055(15) 0.1522(16) 0.4885(15) 0.139(3) Uani 0.356(4) 1 d PDU A 2 H46D H 0.4436 0.1764 0.4554 0.208 Uiso 0.356(4) 1 calc PR A 2 H46E H 0.4287 0.1123 0.5307 0.208 Uiso 0.356(4) 1 calc PR A 2 H46F H 0.3808 0.2007 0.5154 0.208 Uiso 0.356(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01288(8) 0.01497(9) 0.01362(8) -0.00024(6) 0.00053(6) 0.00065(6) Gd2 0.01359(8) 0.01561(9) 0.01431(8) 0.00002(6) 0.00050(6) -0.00088(6) Cl1 0.0166(4) 0.0267(5) 0.0477(5) 0.0134(4) 0.0051(4) 0.0020(3) O1 0.0241(14) 0.0396(17) 0.0498(17) 0.0218(14) 0.0053(12) -0.0051(12) O2 0.0238(14) 0.0354(17) 0.0556(18) 0.0242(14) -0.0035(12) 0.0019(12) O3 0.0239(14) 0.0417(18) 0.0524(17) -0.0276(14) -0.0003(12) 0.0077(12) O5 0.0368(16) 0.0494(19) 0.0403(16) 0.0232(15) -0.0181(13) -0.0038(14) O4 0.0215(13) 0.0297(15) 0.0425(15) -0.0166(12) 0.0016(11) -0.0058(11) O6 0.0351(16) 0.051(2) 0.0329(15) 0.0245(14) -0.0003(12) -0.0093(14) O7 0.0189(13) 0.0492(18) 0.0271(13) -0.0178(12) -0.0038(10) -0.0001(12) O8 0.0218(13) 0.0386(15) 0.0195(11) -0.0082(11) 0.0016(9) 0.0076(11) O9 0.0263(14) 0.0397(17) 0.0318(14) -0.0171(12) 0.0066(11) -0.0007(12) O10 0.0261(14) 0.0359(16) 0.0371(15) -0.0192(12) 0.0073(11) -0.0110(12) O11 0.0339(15) 0.0393(17) 0.0277(14) -0.0141(12) 0.0031(11) -0.0158(13) O12 0.0257(15) 0.0489(19) 0.0443(16) -0.0257(14) 0.0124(12) -0.0076(13) C1 0.0212(18) 0.0226(18) 0.0333(19) 0.0107(16) -0.0005(14) -0.0021(14) C2 0.0180(17) 0.0241(19) 0.0280(18) 0.0105(15) 0.0009(14) 0.0002(14) C3 0.0197(18) 0.033(2) 0.040(2) 0.0134(18) -0.0069(15) -0.0083(16) C4 0.0223(19) 0.038(2) 0.032(2) 0.0146(17) -0.0091(15) -0.0041(16) C5 0.0189(17) 0.029(2) 0.0241(17) 0.0127(15) 0.0011(13) 0.0011(14) C6 0.0156(16) 0.0246(19) 0.0267(17) 0.0066(15) 0.0019(13) -0.0019(14) C7 0.0177(16) 0.0271(19) 0.0225(17) 0.0075(14) 0.0003(13) 0.0011(14) C8 0.032(2) 0.040(2) 0.0247(18) 0.0108(17) -0.0054(16) -0.0049(18) C9 0.037(2) 0.052(3) 0.030(2) 0.0008(19) -0.0080(17) -0.012(2) C10 0.036(2) 0.039(2) 0.036(2) -0.0033(18) 0.0003(17) -0.0158(19) C11 0.030(2) 0.030(2) 0.0320(19) 0.0064(16) 0.0018(16) -0.0070(16) C12 0.031(2) 0.028(2) 0.0243(18) 0.0098(15) -0.0021(15) -0.0023(16) C13 0.0211(18) 0.0249(19) 0.0331(19) -0.0100(16) 0.0039(15) -0.0027(15) C14 0.0199(17) 0.029(2) 0.0281(18) -0.0127(15) 0.0022(14) 0.0001(15) C15 0.028(2) 0.035(2) 0.040(2) -0.0140(18) -0.0085(17) 0.0146(17) C16 0.026(2) 0.045(2) 0.0286(19) -0.0125(18) -0.0099(15) 0.0128(18) C17 0.0180(16) 0.0262(19) 0.0198(16) -0.0058(14) -0.0023(13) 0.0014(14) C18 0.0148(15) 0.0230(18) 0.0181(15) -0.0038(13) 0.0019(12) -0.0021(13) C19 0.0176(16) 0.0237(18) 0.0221(16) -0.0059(14) 0.0001(13) -0.0021(14) C20 0.038(2) 0.035(2) 0.0219(17) -0.0089(16) -0.0042(16) -0.0020(17) C21 0.036(2) 0.046(3) 0.0247(19) 0.0002(18) -0.0093(16) 0.0070(19) C22 0.035(2) 0.032(2) 0.034(2) 0.0034(18) -0.0045(17) 0.0121(18) C23 0.0248(18) 0.0246(19) 0.0274(18) -0.0048(15) 0.0012(14) 0.0029(15) C24 0.0213(17) 0.0251(19) 0.0182(16) -0.0029(14) 0.0014(13) 0.0004(14) C25 0.0258(19) 0.029(2) 0.0226(17) -0.0087(15) 0.0080(14) -0.0068(15) C26 0.0227(18) 0.030(2) 0.0234(17) -0.0100(15) 0.0069(14) -0.0067(15) C27 0.027(2) 0.035(2) 0.035(2) -0.0115(18) -0.0040(16) 0.0077(17) C28 0.031(2) 0.043(2) 0.0249(19) -0.0119(17) -0.0076(15) 0.0049(18) C29 0.0214(18) 0.033(2) 0.0245(18) -0.0119(16) 0.0052(14) -0.0076(15) C30 0.0222(18) 0.028(2) 0.0288(18) -0.0073(15) 0.0050(14) -0.0059(15) C31 0.0215(17) 0.0266(19) 0.0247(17) -0.0071(15) 0.0038(14) -0.0077(15) C32 0.043(2) 0.042(3) 0.0253(19) -0.0017(18) -0.0007(17) -0.007(2) C33 0.048(3) 0.058(3) 0.039(2) 0.014(2) -0.010(2) -0.003(2) C34 0.045(3) 0.044(3) 0.055(3) 0.010(2) 0.003(2) 0.010(2) C35 0.041(2) 0.030(2) 0.044(2) -0.0025(19) 0.0097(19) -0.0006(18) C36 0.028(2) 0.027(2) 0.0300(19) -0.0123(16) 0.0098(15) -0.0083(16) N1A 0.064(2) 0.053(2) 0.060(2) 0.012(2) 0.023(2) 0.012(2) N2A 0.074(2) 0.062(2) 0.057(2) 0.0099(19) 0.0165(19) 0.008(2) C37A 0.076(3) 0.062(2) 0.060(2) 0.015(2) 0.019(2) 0.016(2) C38A 0.076(2) 0.064(2) 0.062(2) 0.011(2) 0.015(2) 0.013(2) C39A 0.069(2) 0.059(2) 0.057(2) 0.0121(19) 0.0171(19) 0.012(2) C40A 0.068(4) 0.062(4) 0.092(4) -0.002(4) 0.023(3) 0.006(3) C41A 0.084(2) 0.072(2) 0.075(2) 0.009(2) 0.017(2) 0.008(2) C43A 0.102(3) 0.087(3) 0.089(3) 0.010(2) 0.019(2) 0.008(3) C42A 0.091(3) 0.079(2) 0.082(2) 0.012(2) 0.019(2) 0.009(2) C44A 0.110(3) 0.095(3) 0.101(3) 0.011(3) 0.017(3) 0.003(3) C45A 0.118(4) 0.101(4) 0.115(3) 0.023(3) 0.020(3) 0.010(3) C46A 0.150(6) 0.119(6) 0.152(6) 0.017(6) 0.038(6) 0.013(6) N1B 0.064(2) 0.053(2) 0.060(2) 0.012(2) 0.023(2) 0.012(2) N2B 0.074(2) 0.062(2) 0.057(2) 0.0099(19) 0.0165(19) 0.008(2) C37B 0.076(3) 0.062(2) 0.060(2) 0.015(2) 0.019(2) 0.016(2) C38B 0.076(2) 0.064(2) 0.062(2) 0.011(2) 0.015(2) 0.013(2) C39B 0.069(2) 0.059(2) 0.057(2) 0.0121(19) 0.0171(19) 0.012(2) C40B 0.068(4) 0.062(4) 0.092(4) -0.002(4) 0.023(3) 0.006(3) C41B 0.084(2) 0.072(2) 0.075(2) 0.009(2) 0.017(2) 0.008(2) C42B 0.091(3) 0.079(2) 0.082(2) 0.012(2) 0.019(2) 0.009(2) C43B 0.102(3) 0.087(3) 0.089(3) 0.010(2) 0.019(2) 0.008(3) C44B 0.110(3) 0.095(3) 0.101(3) 0.011(3) 0.017(3) 0.003(3) C45B 0.118(4) 0.101(4) 0.115(3) 0.023(3) 0.020(3) 0.010(3) C46B 0.150(6) 0.119(6) 0.152(6) 0.017(6) 0.038(6) 0.013(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O7 2.309(2) 4_565 ? Gd1 O1 2.315(3) . ? Gd1 O5 2.328(2) 4_566 ? Gd1 O6 2.331(3) 2_644 ? Gd1 O3 2.336(3) . ? Gd1 O2 2.351(3) 3_655 ? Gd1 Cl1 2.8211(9) . ? Gd2 O11 2.286(2) 4_565 ? Gd2 O4 2.299(2) . ? Gd2 O10 2.318(2) 3 ? Gd2 O8 2.365(2) 4_565 ? Gd2 O9 2.386(2) . ? Gd2 O12 2.394(3) 2_545 ? Gd2 Cl1 2.7914(9) . ? O1 C1 1.242(4) . ? O2 C1 1.253(4) . ? O2 Gd1 2.351(3) 3_655 ? O3 C13 1.260(4) . ? O5 C12 1.241(4) . ? O5 Gd1 2.328(2) 4_565 ? O4 C13 1.259(4) . ? O6 C12 1.251(5) . ? O6 Gd1 2.331(3) 2_654 ? O7 C24 1.248(4) . ? O7 Gd1 2.309(2) 4_566 ? O8 C24 1.255(4) . ? O8 Gd2 2.365(2) 4_566 ? O9 C25 1.245(4) . ? O10 C25 1.267(4) . ? O10 Gd2 2.318(2) 3 ? O11 C36 1.250(4) . ? O11 Gd2 2.286(2) 4_566 ? O12 C36 1.255(4) . ? O12 Gd2 2.394(3) 2 ? C1 C2 1.506(5) . ? C2 C3 1.382(5) . ? C2 C7 1.427(5) . ? C3 C4 1.402(5) . ? C3 H3A 0.9300 . ? C4 C5 1.361(5) . ? C4 H4A 0.9300 . ? C5 C6 1.432(5) . ? C5 C12 1.505(5) . ? C6 C11 1.425(5) . ? C6 C7 1.428(5) . ? C7 C8 1.423(5) . ? C8 C9 1.364(6) . ? C8 H8A 0.9300 . ? C9 C10 1.386(6) . ? C9 H9A 0.9300 . ? C10 C11 1.367(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.495(5) . ? C14 C15 1.376(5) . ? C14 C19 1.428(5) . ? C15 C16 1.386(5) . ? C15 H15A 0.9300 . ? C16 C17 1.370(5) . ? C16 H16A 0.9300 . ? C17 C18 1.441(4) . ? C17 C24 1.510(5) . ? C18 C23 1.416(5) . ? C18 C19 1.424(4) . ? C19 C20 1.427(5) . ? C20 C21 1.355(6) . ? C20 H20A 0.9300 . ? C21 C22 1.390(6) . ? C21 H21A 0.9300 . ? C22 C23 1.363(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.499(5) . ? C26 C27 1.365(5) . ? C26 C31 1.421(5) . ? C27 C28 1.402(5) . ? C27 H27A 0.9300 . ? C28 C29 1.370(5) . ? C28 H28A 0.9300 . ? C29 C30 1.428(5) . ? C29 C36 1.490(5) . ? C30 C31 1.421(5) . ? C30 C35 1.423(6) . ? C31 C32 1.426(5) . ? C32 C33 1.364(6) . ? C32 H32A 0.9300 . ? C33 C34 1.386(7) . ? C33 H33A 0.9300 . ? C34 C35 1.366(6) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? N1A C39A 1.326(7) . ? N1A C37A 1.362(8) . ? N1A C40A 1.437(10) . ? N2A C39A 1.319(9) . ? N2A C38A 1.370(7) . ? N2A C41A 1.495(10) . ? C37A C38A 1.254(13) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.511(8) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C44A 1.591(9) . ? C43A C42A 1.607(9) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.558(9) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.525(9) . ? C45A H45A 0.9700 . ? C45A H45B 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N1B C39B 1.347(9) . ? N1B C37B 1.360(9) . ? N1B C40B 1.453(12) . ? N2B C39B 1.280(10) . ? N2B C38B 1.352(9) . ? N2B C41B 1.459(12) . ? C37B C38B 1.252(16) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C39B H39B 0.9300 . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C41B C42B 1.513(10) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.536(10) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C43B C44B 1.593(10) . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C44B C45B 1.535(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C45B C46B 1.503(10) . ? C45B H45C 0.9700 . ? C45B H45D 0.9700 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? C46B H46F 0.9600 . ? 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 O7 Gd1 O1 79.82(9) 4_565 . ? O7 Gd1 O5 146.01(11) 4_565 4_566 ? O1 Gd1 O5 77.33(11) . 4_566 ? O7 Gd1 O6 77.52(10) 4_565 2_644 ? O1 Gd1 O6 81.05(11) . 2_644 ? O5 Gd1 O6 122.64(10) 4_566 2_644 ? O7 Gd1 O3 82.24(10) 4_565 . ? O1 Gd1 O3 98.61(12) . . ? O5 Gd1 O3 76.73(10) 4_566 . ? O6 Gd1 O3 159.51(10) 2_644 . ? O7 Gd1 O2 140.84(10) 4_565 3_655 ? O1 Gd1 O2 124.86(10) . 3_655 ? O5 Gd1 O2 73.12(11) 4_566 3_655 ? O6 Gd1 O2 77.45(11) 2_644 3_655 ? O3 Gd1 O2 117.84(11) . 3_655 ? O7 Gd1 Cl1 77.09(7) 4_565 . ? O1 Gd1 Cl1 156.52(7) . . ? O5 Gd1 Cl1 125.25(9) 4_566 . ? O6 Gd1 Cl1 89.80(8) 2_644 . ? O3 Gd1 Cl1 82.53(8) . . ? O2 Gd1 Cl1 73.20(7) 3_655 . ? O11 Gd2 O4 97.78(10) 4_565 . ? O11 Gd2 O10 80.36(10) 4_565 3 ? O4 Gd2 O10 154.95(10) . 3 ? O11 Gd2 O8 80.39(9) 4_565 4_565 ? O4 Gd2 O8 76.96(9) . 4_565 ? O10 Gd2 O8 78.11(9) 3 4_565 ? O11 Gd2 O9 75.01(9) 4_565 . ? O4 Gd2 O9 74.03(9) . . ? O10 Gd2 O9 128.35(9) 3 . ? O8 Gd2 O9 138.57(10) 4_565 . ? O11 Gd2 O12 123.00(9) 4_565 2_545 ? O4 Gd2 O12 116.60(10) . 2_545 ? O10 Gd2 O12 84.07(11) 3 2_545 ? O8 Gd2 O12 147.71(10) 4_565 2_545 ? O9 Gd2 O12 73.09(10) . 2_545 ? O11 Gd2 Cl1 161.84(7) 4_565 . ? O4 Gd2 Cl1 83.09(7) . . ? O10 Gd2 Cl1 91.16(7) 3 . ? O8 Gd2 Cl1 82.16(7) 4_565 . ? O9 Gd2 Cl1 122.23(7) . . ? O12 Gd2 Cl1 71.42(7) 2_545 . ? Gd2 Cl1 Gd1 112.01(3) . . ? C1 O1 Gd1 144.5(2) . . ? C1 O2 Gd1 143.1(2) . 3_655 ? C13 O3 Gd1 138.9(2) . . ? C12 O5 Gd1 164.2(3) . 4_565 ? C13 O4 Gd2 144.4(3) . . ? C12 O6 Gd1 127.1(2) . 2_654 ? C24 O7 Gd1 160.0(2) . 4_566 ? C24 O8 Gd2 132.7(2) . 4_566 ? C25 O9 Gd2 136.6(2) . . ? C25 O10 Gd2 139.7(2) . 3 ? C36 O11 Gd2 162.2(3) . 4_566 ? C36 O12 Gd2 111.0(2) . 2 ? O1 C1 O2 125.9(3) . . ? O1 C1 C2 116.8(3) . . ? O2 C1 C2 117.4(3) . . ? C3 C2 C7 119.7(3) . . ? C3 C2 C1 116.9(3) . . ? C7 C2 C1 123.4(3) . . ? C2 C3 C4 120.5(3) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 121.5(3) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 C12 117.0(3) . . ? C6 C5 C12 122.9(3) . . ? C11 C6 C7 118.7(3) . . ? C11 C6 C5 122.5(3) . . ? C7 C6 C5 118.8(3) . . ? C8 C7 C6 118.6(3) . . ? C8 C7 C2 122.1(3) . . ? C6 C7 C2 119.3(3) . . ? C9 C8 C7 120.3(4) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 121.2(4) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C6 120.3(4) . . ? C10 C11 H11A 119.8 . . ? C6 C11 H11A 119.8 . . ? O5 C12 O6 124.5(3) . . ? O5 C12 C5 117.6(3) . . ? O6 C12 C5 118.0(3) . . ? O3 C13 O4 123.5(3) . . ? O3 C13 C14 117.3(3) . . ? O4 C13 C14 119.1(3) . . ? C15 C14 C19 119.0(3) . . ? C15 C14 C13 116.5(3) . . ? C19 C14 C13 124.5(3) . . ? C14 C15 C16 121.7(4) . . ? C14 C15 H15A 119.1 . . ? C16 C15 H15A 119.1 . . ? C17 C16 C15 121.7(3) . . ? C17 C16 H16A 119.1 . . ? C15 C16 H16A 119.1 . . ? C16 C17 C18 118.9(3) . . ? C16 C17 C24 116.0(3) . . ? C18 C17 C24 125.1(3) . . ? C23 C18 C19 118.7(3) . . ? C23 C18 C17 122.1(3) . . ? C19 C18 C17 119.2(3) . . ? C18 C19 C14 119.5(3) . . ? C18 C19 C20 118.3(3) . . ? C14 C19 C20 122.2(3) . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 120.9(3) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? C23 C22 C21 120.7(4) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C18 120.7(3) . . ? C22 C23 H23A 119.7 . . ? C18 C23 H23A 119.7 . . ? O7 C24 O8 125.2(3) . . ? O7 C24 C17 115.3(3) . . ? O8 C24 C17 119.5(3) . . ? O9 C25 O10 125.5(3) . . ? O9 C25 C26 119.0(3) . . ? O10 C25 C26 115.5(3) . . ? C27 C26 C31 119.7(3) . . ? C27 C26 C25 118.2(4) . . ? C31 C26 C25 122.0(3) . . ? C26 C27 C28 121.1(4) . . ? C26 C27 H27A 119.4 . . ? C28 C27 H27A 119.4 . . ? C29 C28 C27 120.6(3) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 119.8(3) . . ? C28 C29 C36 118.8(3) . . ? C30 C29 C36 121.3(4) . . ? C31 C30 C35 119.2(3) . . ? C31 C30 C29 118.8(3) . . ? C35 C30 C29 122.0(3) . . ? C30 C31 C26 119.4(3) . . ? C30 C31 C32 118.6(4) . . ? C26 C31 C32 122.0(3) . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 C34 121.2(4) . . ? C32 C33 H33A 119.4 . . ? C34 C33 H33A 119.4 . . ? C35 C34 C33 121.0(4) . . ? C35 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? C34 C35 C30 119.9(4) . . ? C34 C35 H35A 120.1 . . ? C30 C35 H35A 120.1 . . ? O11 C36 O12 122.3(3) . . ? O11 C36 C29 119.6(3) . . ? O12 C36 C29 118.1(3) . . ? C39A N1A C37A 107.3(8) . . ? C39A N1A C40A 127.5(8) . . ? C37A N1A C40A 125.2(7) . . ? C39A N2A C38A 107.5(8) . . ? C39A N2A C41A 122.0(6) . . ? C38A N2A C41A 130.6(8) . . ? C38A C37A N1A 109.1(9) . . ? C38A C37A H37A 125.4 . . ? N1A C37A H37A 125.4 . . ? C37A C38A N2A 108.5(9) . . ? C37A C38A H38A 125.8 . . ? N2A C38A H38A 125.8 . . ? N2A C39A N1A 107.6(7) . . ? N2A C39A H39A 126.2 . . ? N1A C39A H39A 126.2 . . ? N1A C40A H40A 109.5 . . ? N1A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? N1A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? N2A C41A C42A 119.5(8) . . ? N2A C41A H41A 107.4 . . ? C42A C41A H41A 107.4 . . ? N2A C41A H41B 107.4 . . ? C42A C41A H41B 107.4 . . ? H41A C41A H41B 107.0 . . ? C44A C43A C42A 92.6(7) . . ? C44A C43A H43A 113.2 . . ? C42A C43A H43A 113.2 . . ? C44A C43A H43B 113.2 . . ? C42A C43A H43B 113.2 . . ? H43A C43A H43B 110.5 . . ? C41A C42A C43A 107.9(8) . . ? C41A C42A H42A 110.1 . . ? C43A C42A H42A 110.1 . . ? C41A C42A H42B 110.1 . . ? C43A C42A H42B 110.1 . . ? H42A C42A H42B 108.4 . . ? C45A C44A C43A 122.1(9) . . ? C45A C44A H44A 106.8 . . ? C43A C44A H44A 106.8 . . ? C45A C44A H44B 106.8 . . ? C43A C44A H44B 106.8 . . ? H44A C44A H44B 106.7 . . ? C46A C45A C44A 107.0(8) . . ? C46A C45A H45A 110.3 . . ? C44A C45A H45A 110.3 . . ? C46A C45A H45B 110.3 . . ? C44A C45A H45B 110.3 . . ? H45A C45A H45B 108.6 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C39B N1B C37B 111.9(13) . . ? C39B N1B C40B 125.6(12) . . ? C37B N1B C40B 122.5(10) . . ? C39B N2B C38B 111.6(10) . . ? C39B N2B C41B 130.5(10) . . ? C38B N2B C41B 117.9(11) . . ? C38B C37B N1B 104.5(14) . . ? C38B C37B H37B 127.8 . . ? N1B C37B H37B 127.8 . . ? C37B C38B N2B 109.7(14) . . ? C37B C38B H38B 125.2 . . ? N2B C38B H38B 125.2 . . ? N2B C39B N1B 102.4(10) . . ? N2B C39B H39B 128.8 . . ? N1B C39B H39B 128.8 . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N2B C41B C42B 101.5(12) . . ? N2B C41B H41C 111.5 . . ? C42B C41B H41C 111.5 . . ? N2B C41B H41D 111.5 . . ? C42B C41B H41D 111.5 . . ? H41C C41B H41D 109.3 . . ? C41B C42B C43B 93.8(12) . . ? C41B C42B H42C 113.0 . . ? C43B C42B H42C 113.0 . . ? C41B C42B H42D 113.0 . . ? C43B C42B H42D 113.0 . . ? H42C C42B H42D 110.4 . . ? C42B C43B C44B 114.3(12) . . ? C42B C43B H43C 108.7 . . ? C44B C43B H43C 108.7 . . ? C42B C43B H43D 108.7 . . ? C44B C43B H43D 108.7 . . ? H43C C43B H43D 107.6 . . ? C45B C44B C43B 114.0(12) . . ? C45B C44B H44C 108.8 . . ? C43B C44B H44C 108.8 . . ? C45B C44B H44D 108.8 . . ? C43B C44B H44D 108.8 . . ? H44C C44B H44D 107.7 . . ? C46B C45B C44B 114.3(11) . . ? C46B C45B H45C 108.7 . . ? C44B C45B H45C 108.7 . . ? C46B C45B H45D 108.7 . . ? C44B C45B H45D 108.7 . . ? H45C C45B H45D 107.6 . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C45B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Gd2 Cl1 Gd1 68.2(3) 4_565 . . . ? O4 Gd2 Cl1 Gd1 -25.73(7) . . . . ? O10 Gd2 Cl1 Gd1 129.82(8) 3 . . . ? O8 Gd2 Cl1 Gd1 51.99(7) 4_565 . . . ? O9 Gd2 Cl1 Gd1 -91.90(9) . . . . ? O12 Gd2 Cl1 Gd1 -146.83(9) 2_545 . . . ? O7 Gd1 Cl1 Gd2 -39.15(8) 4_565 . . . ? O1 Gd1 Cl1 Gd2 -49.9(2) . . . . ? O5 Gd1 Cl1 Gd2 112.46(10) 4_566 . . . ? O6 Gd1 Cl1 Gd2 -116.39(8) 2_644 . . . ? O3 Gd1 Cl1 Gd2 44.56(8) . . . . ? O2 Gd1 Cl1 Gd2 166.67(9) 3_655 . . . ? O7 Gd1 O1 C1 -154.3(5) 4_565 . . . ? O5 Gd1 O1 C1 51.1(5) 4_566 . . . ? O6 Gd1 O1 C1 -75.5(5) 2_644 . . . ? O3 Gd1 O1 C1 125.3(5) . . . . ? O2 Gd1 O1 C1 -7.7(5) 3_655 . . . ? Cl1 Gd1 O1 C1 -143.6(4) . . . . ? O7 Gd1 O3 C13 30.4(4) 4_565 . . . ? O1 Gd1 O3 C13 108.8(4) . . . . ? O5 Gd1 O3 C13 -176.5(5) 4_566 . . . ? O6 Gd1 O3 C13 21.4(7) 2_644 . . . ? O2 Gd1 O3 C13 -114.0(4) 3_655 . . . ? Cl1 Gd1 O3 C13 -47.5(4) . . . . ? O11 Gd2 O4 C13 161.2(4) 4_565 . . . ? O10 Gd2 O4 C13 -114.9(4) 3 . . . ? O8 Gd2 O4 C13 -120.6(4) 4_565 . . . ? O9 Gd2 O4 C13 89.3(4) . . . . ? O12 Gd2 O4 C13 28.1(4) 2_545 . . . ? Cl1 Gd2 O4 C13 -37.1(4) . . . . ? O11 Gd2 O9 C25 17.2(4) 4_565 . . . ? O4 Gd2 O9 C25 120.0(4) . . . . ? O10 Gd2 O9 C25 -47.2(4) 3 . . . ? O8 Gd2 O9 C25 72.8(4) 4_565 . . . ? O12 Gd2 O9 C25 -115.0(4) 2_545 . . . ? Cl1 Gd2 O9 C25 -169.1(3) . . . . ? Gd1 O1 C1 O2 -4.8(8) . . . . ? Gd1 O1 C1 C2 173.1(3) . . . . ? Gd1 O2 C1 O1 18.6(8) 3_655 . . . ? Gd1 O2 C1 C2 -159.3(3) 3_655 . . . ? O1 C1 C2 C3 -42.3(5) . . . . ? O2 C1 C2 C3 135.7(4) . . . . ? O1 C1 C2 C7 137.6(4) . . . . ? O2 C1 C2 C7 -44.3(6) . . . . ? C7 C2 C3 C4 2.1(6) . . . . ? C1 C2 C3 C4 -177.9(4) . . . . ? C2 C3 C4 C5 -0.9(6) . . . . ? C3 C4 C5 C6 -1.7(6) . . . . ? C3 C4 C5 C12 175.7(4) . . . . ? C4 C5 C6 C11 -174.5(4) . . . . ? C12 C5 C6 C11 8.3(6) . . . . ? C4 C5 C6 C7 3.1(6) . . . . ? C12 C5 C6 C7 -174.1(3) . . . . ? C11 C6 C7 C8 -2.4(5) . . . . ? C5 C6 C7 C8 179.9(3) . . . . ? C11 C6 C7 C2 175.8(3) . . . . ? C5 C6 C7 C2 -1.9(5) . . . . ? C3 C2 C7 C8 177.5(4) . . . . ? C1 C2 C7 C8 -2.5(6) . . . . ? C3 C2 C7 C6 -0.6(6) . . . . ? C1 C2 C7 C6 179.4(3) . . . . ? C6 C7 C8 C9 2.4(6) . . . . ? C2 C7 C8 C9 -175.7(4) . . . . ? C7 C8 C9 C10 -1.1(7) . . . . ? C8 C9 C10 C11 -0.3(7) . . . . ? C9 C10 C11 C6 0.3(7) . . . . ? C7 C6 C11 C10 1.1(6) . . . . ? C5 C6 C11 C10 178.7(4) . . . . ? Gd1 O5 C12 O6 22.9(14) 4_565 . . . ? Gd1 O5 C12 C5 -155.5(9) 4_565 . . . ? Gd1 O6 C12 O5 1.6(6) 2_654 . . . ? Gd1 O6 C12 C5 179.9(3) 2_654 . . . ? C4 C5 C12 O5 37.5(6) . . . . ? C6 C5 C12 O5 -145.3(4) . . . . ? C4 C5 C12 O6 -141.0(4) . . . . ? C6 C5 C12 O6 36.3(6) . . . . ? Gd1 O3 C13 O4 4.7(7) . . . . ? Gd1 O3 C13 C14 -177.9(3) . . . . ? Gd2 O4 C13 O3 62.5(6) . . . . ? Gd2 O4 C13 C14 -114.9(4) . . . . ? O3 C13 C14 C15 -34.6(5) . . . . ? O4 C13 C14 C15 143.0(4) . . . . ? O3 C13 C14 C19 147.3(4) . . . . ? O4 C13 C14 C19 -35.2(6) . . . . ? C19 C14 C15 C16 0.3(6) . . . . ? C13 C14 C15 C16 -178.0(4) . . . . ? C14 C15 C16 C17 1.1(7) . . . . ? C15 C16 C17 C18 -1.0(6) . . . . ? C15 C16 C17 C24 -179.1(4) . . . . ? C16 C17 C18 C23 -179.3(4) . . . . ? C24 C17 C18 C23 -1.3(5) . . . . ? C16 C17 C18 C19 -0.6(5) . . . . ? C24 C17 C18 C19 177.4(3) . . . . ? C23 C18 C19 C14 -179.3(3) . . . . ? C17 C18 C19 C14 1.9(5) . . . . ? C23 C18 C19 C20 2.8(5) . . . . ? C17 C18 C19 C20 -175.9(3) . . . . ? C15 C14 C19 C18 -1.8(5) . . . . ? C13 C14 C19 C18 176.3(3) . . . . ? C15 C14 C19 C20 176.0(4) . . . . ? C13 C14 C19 C20 -5.9(6) . . . . ? C18 C19 C20 C21 -1.7(6) . . . . ? C14 C19 C20 C21 -179.5(4) . . . . ? C19 C20 C21 C22 0.3(7) . . . . ? C20 C21 C22 C23 0.1(7) . . . . ? C21 C22 C23 C18 1.1(6) . . . . ? C19 C18 C23 C22 -2.6(5) . . . . ? C17 C18 C23 C22 176.1(4) . . . . ? Gd1 O7 C24 O8 7.1(11) 4_566 . . . ? Gd1 O7 C24 C17 -171.7(6) 4_566 . . . ? Gd2 O8 C24 O7 -34.8(6) 4_566 . . . ? Gd2 O8 C24 C17 144.0(3) 4_566 . . . ? C16 C17 C24 O7 32.9(5) . . . . ? C18 C17 C24 O7 -145.1(4) . . . . ? C16 C17 C24 O8 -146.0(4) . . . . ? C18 C17 C24 O8 36.0(5) . . . . ? Gd2 O9 C25 O10 33.4(6) . . . . ? Gd2 O9 C25 C26 -149.6(3) . . . . ? Gd2 O10 C25 O9 2.9(7) 3 . . . ? Gd2 O10 C25 C26 -174.2(3) 3 . . . ? O9 C25 C26 C27 -45.3(5) . . . . ? O10 C25 C26 C27 132.0(4) . . . . ? O9 C25 C26 C31 139.0(4) . . . . ? O10 C25 C26 C31 -43.7(5) . . . . ? C31 C26 C27 C28 6.6(6) . . . . ? C25 C26 C27 C28 -169.2(4) . . . . ? C26 C27 C28 C29 0.2(7) . . . . ? C27 C28 C29 C30 -7.0(6) . . . . ? C27 C28 C29 C36 168.7(4) . . . . ? C28 C29 C30 C31 7.0(5) . . . . ? C36 C29 C30 C31 -168.7(3) . . . . ? C28 C29 C30 C35 -170.7(4) . . . . ? C36 C29 C30 C35 13.7(6) . . . . ? C35 C30 C31 C26 177.4(3) . . . . ? C29 C30 C31 C26 -0.3(5) . . . . ? C35 C30 C31 C32 -0.2(5) . . . . ? C29 C30 C31 C32 -177.9(3) . . . . ? C27 C26 C31 C30 -6.5(5) . . . . ? C25 C26 C31 C30 169.2(3) . . . . ? C27 C26 C31 C32 171.1(4) . . . . ? C25 C26 C31 C32 -13.3(5) . . . . ? C30 C31 C32 C33 1.1(6) . . . . ? C26 C31 C32 C33 -176.4(4) . . . . ? C31 C32 C33 C34 -0.5(7) . . . . ? C32 C33 C34 C35 -1.0(8) . . . . ? C33 C34 C35 C30 2.0(7) . . . . ? C31 C30 C35 C34 -1.4(6) . . . . ? C29 C30 C35 C34 176.3(4) . . . . ? Gd2 O11 C36 O12 -105.5(8) 4_566 . . . ? Gd2 O11 C36 C29 77.2(10) 4_566 . . . ? Gd2 O12 C36 O11 11.5(5) 2 . . . ? Gd2 O12 C36 C29 -171.2(3) 2 . . . ? C28 C29 C36 O11 44.8(5) . . . . ? C30 C29 C36 O11 -139.5(4) . . . . ? C28 C29 C36 O12 -132.5(4) . . . . ? C30 C29 C36 O12 43.2(5) . . . . ? C39A N1A C37A C38A 0.0(3) . . . . ? C40A N1A C37A C38A 179.9(3) . . . . ? N1A C37A C38A N2A 0.0(3) . . . . ? C39A N2A C38A C37A -0.1(3) . . . . ? C41A N2A C38A C37A 179.6(2) . . . . ? C38A N2A C39A N1A 0.1(3) . . . . ? C41A N2A C39A N1A -179.6(2) . . . . ? C37A N1A C39A N2A -0.1(3) . . . . ? C40A N1A C39A N2A -179.9(2) . . . . ? C39A N2A C41A C42A 171.7(7) . . . . ? C38A N2A C41A C42A -8.0(7) . . . . ? N2A C41A C42A C43A -73.8(10) . . . . ? C44A C43A C42A C41A -180.0(9) . . . . ? C42A C43A C44A C45A -148.0(11) . . . . ? C43A C44A C45A C46A -52.5(16) . . . . ? C39B N1B C37B C38B -0.1(3) . . . . ? C40B N1B C37B C38B 179.9(3) . . . . ? N1B C37B C38B N2B -0.1(3) . . . . ? C39B N2B C38B C37B 0.3(4) . . . . ? C41B N2B C38B C37B -179.8(2) . . . . ? C38B N2B C39B N1B -0.4(3) . . . . ? C41B N2B C39B N1B 179.8(2) . . . . ? C37B N1B C39B N2B 0.3(3) . . . . ? C40B N1B C39B N2B -179.8(2) . . . . ? C39B N2B C41B C42B -2.0(11) . . . . ? C38B N2B C41B C42B 178.2(11) . . . . ? N2B C41B C42B C43B 116.1(11) . . . . ? C41B C42B C43B C44B 59(2) . . . . ? C42B C43B C44B C45B -171.0(18) . . . . ? C43B C44B C45B C46B -155(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.447 _refine_diff_density_min -1.180 _refine_diff_density_rms 0.102 #===END data_compound-8 _database_code_depnum_ccdc_archive 'CCDC 876528' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Tb2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl N2 O12 Tb2' _chemical_formula_weight 1163.07 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.6908(5) _cell_length_b 14.8181(5) _cell_length_c 15.8924(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.582(3) _cell_angle_gamma 90.00 _cell_volume 4152.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11376 _cell_measurement_theta_min 2.3052 _cell_measurement_theta_max 28.4205 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 3.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68295 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17571 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 26.05 _reflns_number_total 8185 _reflns_number_gt 6540 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0364P)^2^+10.2027P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8185 _refine_ls_number_parameters 605 _refine_ls_number_restraints 945 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.051 _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 0.378340(11) 0.024710(14) -0.004440(12) 0.01434(7) Uani 1 1 d . . . Tb2 Tb 0.117106(11) 0.011779(14) -0.001262(12) 0.01502(7) Uani 1 1 d . . . Cl1 Cl 0.25211(7) -0.08281(8) 0.02495(8) 0.0309(3) Uani 1 1 d . . . O1 O 0.4500(2) 0.1229(3) -0.0777(2) 0.0376(9) Uani 1 1 d . . . O2 O 0.5753(2) 0.1053(2) -0.0652(2) 0.0372(9) Uani 1 1 d . . . O3 O 0.3153(2) 0.1289(3) 0.0736(2) 0.0399(10) Uani 1 1 d . . . O5 O 0.4701(2) 0.4287(3) -0.4026(2) 0.0411(10) Uani 1 1 d . . . O4 O 0.19270(19) 0.1337(2) 0.0315(2) 0.0298(8) Uani 1 1 d . . . O6 O 0.5951(2) 0.4313(3) -0.3846(2) 0.0399(10) Uani 1 1 d . . . O7 O 0.29041(19) 0.4298(2) 0.3902(2) 0.0311(8) Uani 1 1 d . . . O8 O 0.16653(18) 0.4547(2) 0.36966(19) 0.0265(8) Uani 1 1 d . . . O9 O 0.06161(19) 0.0866(2) 0.1104(2) 0.0320(8) Uani 1 1 d . . . O10 O -0.06361(19) 0.1003(2) 0.0871(2) 0.0326(9) Uani 1 1 d . . . O11 O 0.0187(2) 0.4098(3) 0.4353(2) 0.0348(9) Uani 1 1 d . . . O12 O -0.1025(2) 0.4030(3) 0.3933(2) 0.0367(9) Uani 1 1 d . . . C1 C 0.5153(3) 0.1425(3) -0.0949(3) 0.0254(11) Uani 1 1 d . . . C2 C 0.5225(3) 0.2165(3) -0.1592(3) 0.0240(11) Uani 1 1 d . . . C3 C 0.4719(3) 0.2144(4) -0.2287(3) 0.0304(12) Uani 1 1 d . . . H3A H 0.4347 0.1699 -0.2333 0.036 Uiso 1 1 calc R . . C4 C 0.4752(3) 0.2786(4) -0.2935(3) 0.0298(12) Uani 1 1 d . . . H4A H 0.4405 0.2757 -0.3405 0.036 Uiso 1 1 calc R . . C5 C 0.5290(3) 0.3454(3) -0.2885(3) 0.0230(10) Uani 1 1 d . . . C6 C 0.5805(3) 0.3534(3) -0.2147(3) 0.0224(10) Uani 1 1 d . . . C7 C 0.5779(3) 0.2866(3) -0.1504(3) 0.0221(10) Uani 1 1 d . . . C8 C 0.6295(3) 0.2938(4) -0.0778(3) 0.0321(12) Uani 1 1 d . . . H8A H 0.6298 0.2500 -0.0359 0.039 Uiso 1 1 calc R . . C9 C 0.6786(3) 0.3647(4) -0.0690(3) 0.0386(14) Uani 1 1 d . . . H9A H 0.7117 0.3688 -0.0207 0.046 Uiso 1 1 calc R . . C10 C 0.6801(3) 0.4309(4) -0.1308(3) 0.0384(14) Uani 1 1 d . . . H10A H 0.7137 0.4790 -0.1230 0.046 Uiso 1 1 calc R . . C11 C 0.6327(3) 0.4259(4) -0.2029(3) 0.0306(12) Uani 1 1 d . . . H11A H 0.6346 0.4700 -0.2443 0.037 Uiso 1 1 calc R . . C12 C 0.5314(3) 0.4072(3) -0.3633(3) 0.0267(11) Uani 1 1 d . . . C13 C 0.2497(3) 0.1611(3) 0.0771(3) 0.0269(11) Uani 1 1 d . . . C14 C 0.2400(3) 0.2329(3) 0.1416(3) 0.0246(11) Uani 1 1 d . . . C15 C 0.2832(3) 0.2255(4) 0.2164(3) 0.0361(13) Uani 1 1 d . . . H15A H 0.3178 0.1782 0.2236 0.043 Uiso 1 1 calc R . . C16 C 0.2773(3) 0.2862(4) 0.2823(3) 0.0337(13) Uani 1 1 d . . . H16A H 0.3080 0.2788 0.3321 0.040 Uiso 1 1 calc R . . C17 C 0.2267(2) 0.3574(3) 0.2752(3) 0.0209(10) Uani 1 1 d . . . C18 C 0.1794(2) 0.3680(3) 0.1981(3) 0.0177(9) Uani 1 1 d . . . C19 C 0.1875(3) 0.3066(3) 0.1302(3) 0.0223(10) Uani 1 1 d . . . C20 C 0.1437(3) 0.3217(4) 0.0528(3) 0.0341(13) Uani 1 1 d . . . H20A H 0.1483 0.2824 0.0079 0.041 Uiso 1 1 calc R . . C21 C 0.0947(3) 0.3930(4) 0.0432(3) 0.0357(13) Uani 1 1 d . . . H21A H 0.0671 0.4025 -0.0083 0.043 Uiso 1 1 calc R . . C22 C 0.0861(3) 0.4516(4) 0.1105(3) 0.0355(13) Uani 1 1 d . . . H22A H 0.0522 0.4995 0.1036 0.043 Uiso 1 1 calc R . . C23 C 0.1262(3) 0.4396(3) 0.1854(3) 0.0272(11) Uani 1 1 d . . . H23A H 0.1190 0.4790 0.2297 0.033 Uiso 1 1 calc R . . C24 C 0.2277(3) 0.4195(3) 0.3508(3) 0.0214(10) Uani 1 1 d . . . C25 C 0.0000(3) 0.1246(3) 0.1207(3) 0.0254(11) Uani 1 1 d . . . C26 C -0.0008(3) 0.2028(3) 0.1807(3) 0.0233(10) Uani 1 1 d . . . C27 C 0.0397(3) 0.1949(4) 0.2577(3) 0.0326(12) Uani 1 1 d . . . H27A H 0.0730 0.1468 0.2673 0.039 Uiso 1 1 calc R . . C28 C 0.0316(3) 0.2581(4) 0.3223(3) 0.0326(13) Uani 1 1 d . . . H28A H 0.0599 0.2517 0.3738 0.039 Uiso 1 1 calc R . . C29 C -0.0176(3) 0.3293(3) 0.3098(3) 0.0253(11) Uani 1 1 d . . . C30 C -0.0547(3) 0.3456(3) 0.2279(3) 0.0258(11) Uani 1 1 d . . . C31 C -0.0462(3) 0.2810(3) 0.1628(3) 0.0239(10) Uani 1 1 d . . . C32 C -0.0811(3) 0.2988(4) 0.0805(3) 0.0369(13) Uani 1 1 d . . . H32A H -0.0771 0.2569 0.0375 0.044 Uiso 1 1 calc R . . C33 C -0.1204(4) 0.3771(4) 0.0647(4) 0.0501(17) Uani 1 1 d . . . H33A H -0.1424 0.3884 0.0106 0.060 Uiso 1 1 calc R . . C34 C -0.1280(3) 0.4405(4) 0.1287(4) 0.0465(15) Uani 1 1 d . . . H34A H -0.1546 0.4938 0.1165 0.056 Uiso 1 1 calc R . . C35 C -0.0971(3) 0.4251(4) 0.2083(4) 0.0387(14) Uani 1 1 d . . . H35A H -0.1039 0.4671 0.2505 0.046 Uiso 1 1 calc R . . C36 C -0.0347(3) 0.3854(3) 0.3842(3) 0.0250(11) Uani 1 1 d . . . N1A N 0.2341(5) -0.2679(6) 0.2708(6) 0.0658(13) Uani 0.614(4) 1 d PDU A 1 N2A N 0.3010(5) -0.1480(6) 0.2706(6) 0.0705(13) Uani 0.614(4) 1 d PDU A 1 C37A C 0.2826(6) -0.2699(10) 0.3402(7) 0.0690(14) Uani 0.614(4) 1 d PDU A 1 H37A H 0.2863 -0.3152 0.3808 0.083 Uiso 0.614(4) 1 calc PR A 1 C38A C 0.3233(7) -0.1973(8) 0.3402(6) 0.0716(13) Uani 0.614(4) 1 d PDU A 1 H38A H 0.3615 -0.1814 0.3811 0.086 Uiso 0.614(4) 1 calc PR A 1 C39A C 0.2459(6) -0.1930(6) 0.2284(6) 0.0675(13) Uani 0.614(4) 1 d PDU A 1 H39A H 0.2200 -0.1753 0.1779 0.081 Uiso 0.614(4) 1 calc PR A 1 C40A C 0.1781(6) -0.3378(8) 0.2471(8) 0.072(2) Uani 0.614(4) 1 d PDU A 1 H40A H 0.1508 -0.3219 0.1946 0.109 Uiso 0.614(4) 1 calc PR A 1 H40B H 0.1433 -0.3429 0.2902 0.109 Uiso 0.614(4) 1 calc PR A 1 H40C H 0.2034 -0.3945 0.2411 0.109 Uiso 0.614(4) 1 calc PR A 1 C41A C 0.3290(6) -0.0590(8) 0.2409(7) 0.0780(13) Uani 0.614(4) 1 d PDU A 1 H41A H 0.2853 -0.0200 0.2308 0.094 Uiso 0.614(4) 1 calc PR A 1 H41B H 0.3492 -0.0692 0.1867 0.094 Uiso 0.614(4) 1 calc PR A 1 C43A C 0.3496(7) 0.0406(10) 0.3713(8) 0.0889(15) Uani 0.614(4) 1 d PDU A 1 H43A H 0.3257 -0.0025 0.4067 0.107 Uiso 0.614(4) 1 calc PR A 1 H43B H 0.3135 0.0869 0.3520 0.107 Uiso 0.614(4) 1 calc PR A 1 C42A C 0.3886(7) -0.0067(9) 0.2954(7) 0.0807(14) Uani 0.614(4) 1 d PDU A 1 H42A H 0.4114 0.0388 0.2616 0.097 Uiso 0.614(4) 1 calc PR A 1 H42B H 0.4282 -0.0473 0.3178 0.097 Uiso 0.614(4) 1 calc PR A 1 C44A C 0.4264(7) 0.0817(10) 0.4161(7) 0.0946(16) Uani 0.614(4) 1 d PDU A 1 H44A H 0.4672 0.0396 0.4079 0.114 Uiso 0.614(4) 1 calc PR A 1 H44B H 0.4377 0.1370 0.3871 0.114 Uiso 0.614(4) 1 calc PR A 1 C45A C 0.4278(8) 0.1029(11) 0.5126(7) 0.101(2) Uani 0.614(4) 1 d PDU A 1 H45A H 0.4315 0.0471 0.5447 0.122 Uiso 0.614(4) 1 calc PR A 1 H45B H 0.4717 0.1397 0.5298 0.122 Uiso 0.614(4) 1 calc PR A 1 C46A C 0.3540(9) 0.1539(12) 0.5308(10) 0.124(3) Uani 0.614(4) 1 d PDU A 1 H46A H 0.3568 0.1719 0.5890 0.187 Uiso 0.614(4) 1 calc PR A 1 H46B H 0.3111 0.1150 0.5191 0.187 Uiso 0.614(4) 1 calc PR A 1 H46C H 0.3485 0.2065 0.4956 0.187 Uiso 0.614(4) 1 calc PR A 1 N1B N 0.2071(7) -0.2818(7) 0.2287(9) 0.0658(13) Uani 0.386(4) 1 d PDU A 2 N2B N 0.2909(7) -0.2072(9) 0.2968(9) 0.0705(13) Uani 0.386(4) 1 d PDU A 2 C37B C 0.2163(9) -0.3218(11) 0.3052(9) 0.0690(14) Uani 0.386(4) 1 d PDU A 2 H37B H 0.1910 -0.3719 0.3242 0.083 Uiso 0.386(4) 1 calc PR A 2 C38B C 0.2686(10) -0.2739(11) 0.3459(12) 0.0716(13) Uani 0.386(4) 1 d PDU A 2 H38B H 0.2879 -0.2844 0.4012 0.086 Uiso 0.386(4) 1 calc PR A 2 C39B C 0.2533(7) -0.2106(9) 0.2234(9) 0.0675(13) Uani 0.386(4) 1 d PDU A 2 H39B H 0.2573 -0.1724 0.1776 0.081 Uiso 0.386(4) 1 calc PR A 2 C40B C 0.1522(9) -0.3150(12) 0.1612(10) 0.072(2) Uani 0.386(4) 1 d PDU A 2 H40D H 0.1540 -0.2774 0.1122 0.109 Uiso 0.386(4) 1 calc PR A 2 H40E H 0.1020 -0.3134 0.1803 0.109 Uiso 0.386(4) 1 calc PR A 2 H40F H 0.1646 -0.3759 0.1471 0.109 Uiso 0.386(4) 1 calc PR A 2 C41B C 0.3500(9) -0.1418(11) 0.3262(10) 0.0780(13) Uani 0.386(4) 1 d PDU A 2 H41C H 0.3971 -0.1723 0.3440 0.094 Uiso 0.386(4) 1 calc PR A 2 H41D H 0.3340 -0.1064 0.3730 0.094 Uiso 0.386(4) 1 calc PR A 2 C42B C 0.3591(13) -0.0822(11) 0.2489(10) 0.0807(14) Uani 0.386(4) 1 d PDU A 2 H42C H 0.4108 -0.0776 0.2331 0.097 Uiso 0.386(4) 1 calc PR A 2 H42D H 0.3242 -0.0964 0.2005 0.097 Uiso 0.386(4) 1 calc PR A 2 C43B C 0.3341(12) -0.0029(14) 0.3020(12) 0.0889(15) Uani 0.386(4) 1 d PDU A 2 H43C H 0.2835 -0.0161 0.3182 0.107 Uiso 0.386(4) 1 calc PR A 2 H43D H 0.3301 0.0500 0.2659 0.107 Uiso 0.386(4) 1 calc PR A 2 C44B C 0.3849(13) 0.0232(14) 0.3847(13) 0.0946(16) Uani 0.386(4) 1 d PDU A 2 H44C H 0.3877 -0.0282 0.4227 0.114 Uiso 0.386(4) 1 calc PR A 2 H44D H 0.4360 0.0359 0.3698 0.114 Uiso 0.386(4) 1 calc PR A 2 C45B C 0.3551(11) 0.1060(14) 0.4319(13) 0.101(2) Uani 0.386(4) 1 d PDU A 2 H45C H 0.3351 0.1496 0.3904 0.122 Uiso 0.386(4) 1 calc PR A 2 H45D H 0.3134 0.0866 0.4636 0.122 Uiso 0.386(4) 1 calc PR A 2 C46B C 0.4141(15) 0.1530(16) 0.4924(16) 0.124(3) Uani 0.386(4) 1 d PDU A 2 H46D H 0.4532 0.1780 0.4609 0.187 Uiso 0.386(4) 1 calc PR A 2 H46E H 0.4360 0.1099 0.5324 0.187 Uiso 0.386(4) 1 calc PR A 2 H46F H 0.3902 0.2004 0.5217 0.187 Uiso 0.386(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01540(11) 0.01414(12) 0.01370(11) -0.00009(8) 0.00266(8) 0.00073(8) Tb2 0.01686(12) 0.01531(12) 0.01307(11) 0.00001(8) 0.00238(8) -0.00095(8) Cl1 0.0184(6) 0.0262(6) 0.0487(8) 0.0132(6) 0.0071(5) 0.0027(5) O1 0.026(2) 0.040(2) 0.047(2) 0.0234(18) 0.0065(17) -0.0071(17) O2 0.030(2) 0.033(2) 0.047(2) 0.0223(18) -0.0007(17) 0.0032(16) O3 0.024(2) 0.043(2) 0.053(3) -0.0298(19) 0.0014(17) 0.0056(17) O5 0.037(2) 0.045(2) 0.038(2) 0.0204(18) -0.0129(17) -0.0036(18) O4 0.0240(19) 0.029(2) 0.036(2) -0.0139(16) 0.0019(15) -0.0055(15) O6 0.037(2) 0.049(3) 0.033(2) 0.0222(18) 0.0031(17) -0.0088(18) O7 0.0227(19) 0.043(2) 0.0274(19) -0.0150(16) -0.0008(14) 0.0009(16) O8 0.0258(18) 0.037(2) 0.0175(17) -0.0067(15) 0.0040(13) 0.0064(15) O9 0.028(2) 0.036(2) 0.033(2) -0.0130(16) 0.0082(15) 0.0023(16) O10 0.026(2) 0.036(2) 0.037(2) -0.0179(17) 0.0087(15) -0.0090(16) O11 0.036(2) 0.041(2) 0.027(2) -0.0157(16) 0.0053(16) -0.0165(17) O12 0.031(2) 0.042(2) 0.038(2) -0.0210(17) 0.0128(16) -0.0068(17) C1 0.022(3) 0.025(3) 0.030(3) 0.009(2) 0.003(2) 0.000(2) C2 0.019(2) 0.025(3) 0.028(3) 0.009(2) 0.0032(19) 0.0010(19) C3 0.020(3) 0.033(3) 0.038(3) 0.012(2) -0.002(2) -0.008(2) C4 0.026(3) 0.037(3) 0.025(3) 0.012(2) -0.006(2) -0.005(2) C5 0.023(3) 0.026(3) 0.020(2) 0.009(2) 0.0011(19) 0.002(2) C6 0.021(2) 0.026(3) 0.021(2) 0.0023(19) 0.0045(19) -0.0016(19) C7 0.017(2) 0.026(3) 0.023(3) 0.007(2) 0.0036(19) 0.0014(19) C8 0.031(3) 0.038(3) 0.026(3) 0.011(2) 0.000(2) -0.004(2) C9 0.034(3) 0.052(4) 0.029(3) 0.001(3) -0.006(2) -0.006(3) C10 0.037(3) 0.039(3) 0.039(3) -0.001(3) 0.003(2) -0.017(3) C11 0.033(3) 0.033(3) 0.026(3) 0.007(2) 0.003(2) -0.006(2) C12 0.029(3) 0.027(3) 0.024(3) 0.008(2) 0.000(2) -0.003(2) C13 0.024(3) 0.023(3) 0.034(3) -0.007(2) 0.006(2) -0.003(2) C14 0.021(3) 0.028(3) 0.026(3) -0.011(2) 0.005(2) -0.001(2) C15 0.031(3) 0.034(3) 0.042(3) -0.015(2) -0.004(2) 0.014(2) C16 0.031(3) 0.040(3) 0.029(3) -0.010(2) -0.006(2) 0.013(2) C17 0.016(2) 0.023(3) 0.023(3) -0.0059(19) 0.0031(18) 0.0015(18) C18 0.017(2) 0.018(2) 0.019(2) -0.0024(18) 0.0041(17) -0.0007(18) C19 0.021(2) 0.024(3) 0.023(3) -0.0093(19) 0.0026(19) -0.0011(19) C20 0.046(3) 0.035(3) 0.021(3) -0.009(2) -0.003(2) 0.000(2) C21 0.040(3) 0.045(3) 0.021(3) -0.002(2) -0.008(2) 0.008(3) C22 0.044(3) 0.028(3) 0.034(3) 0.003(2) -0.002(2) 0.012(2) C23 0.025(3) 0.025(3) 0.031(3) -0.006(2) 0.004(2) 0.005(2) C24 0.021(2) 0.025(3) 0.019(2) -0.0004(19) 0.0021(18) -0.0016(19) C25 0.030(3) 0.028(3) 0.019(2) -0.006(2) 0.007(2) -0.008(2) C26 0.022(3) 0.029(3) 0.020(3) -0.008(2) 0.0077(19) -0.006(2) C27 0.029(3) 0.036(3) 0.033(3) -0.012(2) -0.003(2) 0.008(2) C28 0.035(3) 0.043(3) 0.019(3) -0.011(2) -0.004(2) 0.007(2) C29 0.023(3) 0.029(3) 0.025(3) -0.014(2) 0.007(2) -0.008(2) C30 0.025(3) 0.025(3) 0.029(3) -0.005(2) 0.006(2) -0.003(2) C31 0.020(2) 0.026(3) 0.026(3) -0.005(2) 0.0055(19) -0.006(2) C32 0.047(4) 0.041(3) 0.023(3) -0.002(2) 0.002(2) -0.007(3) C33 0.054(4) 0.055(4) 0.039(4) 0.016(3) -0.007(3) -0.005(3) C34 0.048(4) 0.041(4) 0.051(4) 0.011(3) 0.004(3) 0.010(3) C35 0.039(3) 0.028(3) 0.050(4) -0.003(3) 0.009(3) 0.000(2) C36 0.031(3) 0.022(3) 0.023(3) -0.008(2) 0.011(2) -0.007(2) N1A 0.077(3) 0.056(3) 0.068(3) 0.011(2) 0.027(2) 0.013(2) N2A 0.083(3) 0.063(2) 0.069(3) 0.009(2) 0.024(2) 0.011(2) C37A 0.081(3) 0.061(3) 0.067(3) 0.012(2) 0.025(2) 0.015(2) C38A 0.083(3) 0.063(3) 0.071(3) 0.010(2) 0.022(2) 0.015(2) C39A 0.079(3) 0.060(3) 0.067(3) 0.010(2) 0.024(2) 0.013(2) C40A 0.076(4) 0.062(4) 0.083(4) -0.001(4) 0.027(4) 0.009(4) C41A 0.088(3) 0.069(3) 0.079(3) 0.009(2) 0.024(2) 0.010(2) C43A 0.100(3) 0.080(3) 0.089(3) 0.010(2) 0.021(3) 0.011(3) C42A 0.091(3) 0.073(3) 0.081(3) 0.010(2) 0.025(2) 0.011(2) C44A 0.105(3) 0.085(3) 0.096(3) 0.010(3) 0.020(3) 0.007(3) C45A 0.111(4) 0.090(4) 0.104(4) 0.020(3) 0.020(4) 0.011(4) C46A 0.136(6) 0.106(6) 0.134(6) 0.017(6) 0.028(6) 0.007(6) N1B 0.077(3) 0.056(3) 0.068(3) 0.011(2) 0.027(2) 0.013(2) N2B 0.083(3) 0.063(2) 0.069(3) 0.009(2) 0.024(2) 0.011(2) C37B 0.081(3) 0.061(3) 0.067(3) 0.012(2) 0.025(2) 0.015(2) C38B 0.083(3) 0.063(3) 0.071(3) 0.010(2) 0.022(2) 0.015(2) C39B 0.079(3) 0.060(3) 0.067(3) 0.010(2) 0.024(2) 0.013(2) C40B 0.076(4) 0.062(4) 0.083(4) -0.001(4) 0.027(4) 0.009(4) C41B 0.088(3) 0.069(3) 0.079(3) 0.009(2) 0.024(2) 0.010(2) C42B 0.091(3) 0.073(3) 0.081(3) 0.010(2) 0.025(2) 0.011(2) C43B 0.100(3) 0.080(3) 0.089(3) 0.010(2) 0.021(3) 0.011(3) C44B 0.105(3) 0.085(3) 0.096(3) 0.010(3) 0.020(3) 0.007(3) C45B 0.111(4) 0.090(4) 0.104(4) 0.020(3) 0.020(4) 0.011(4) C46B 0.136(6) 0.106(6) 0.134(6) 0.017(6) 0.028(6) 0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O7 2.294(3) 4_565 ? Tb1 O1 2.305(3) . ? Tb1 O5 2.305(3) 4_566 ? Tb1 O6 2.320(3) 2_644 ? Tb1 O3 2.320(3) . ? Tb1 O2 2.338(3) 3_655 ? Tb1 Cl1 2.8125(12) . ? Tb2 O11 2.263(3) 4_565 ? Tb2 O4 2.283(3) . ? Tb2 O10 2.305(3) 3 ? Tb2 O8 2.346(3) 4_565 ? Tb2 O9 2.371(3) . ? Tb2 O12 2.384(3) 2_545 ? Tb2 Cl1 2.7718(12) . ? O1 C1 1.244(6) . ? O2 C1 1.254(6) . ? O2 Tb1 2.338(3) 3_655 ? O3 C13 1.261(6) . ? O5 C12 1.248(6) . ? O5 Tb1 2.305(3) 4_565 ? O4 C13 1.261(6) . ? O6 C12 1.255(6) . ? O6 Tb1 2.320(3) 2_654 ? O7 C24 1.239(5) . ? O7 Tb1 2.294(3) 4_566 ? O8 C24 1.259(5) . ? O8 Tb2 2.346(3) 4_566 ? O9 C25 1.248(6) . ? O10 C25 1.259(6) . ? O10 Tb2 2.305(3) 3 ? O11 C36 1.249(6) . ? O11 Tb2 2.263(3) 4_566 ? O12 C36 1.246(6) . ? O12 Tb2 2.384(3) 2 ? C1 C2 1.510(6) . ? C2 C3 1.366(7) . ? C2 C7 1.428(7) . ? C3 C4 1.407(7) . ? C3 H3A 0.9300 . ? C4 C5 1.370(7) . ? C4 H4A 0.9300 . ? C5 C6 1.431(6) . ? C5 C12 1.503(6) . ? C6 C11 1.419(7) . ? C6 C7 1.427(6) . ? C7 C8 1.416(6) . ? C8 C9 1.362(7) . ? C8 H8A 0.9300 . ? C9 C10 1.389(8) . ? C9 H9A 0.9300 . ? C10 C11 1.368(7) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.496(6) . ? C14 C15 1.367(7) . ? C14 C19 1.436(7) . ? C15 C16 1.391(7) . ? C15 H15A 0.9300 . ? C16 C17 1.382(7) . ? C16 H16A 0.9300 . ? C17 C18 1.436(6) . ? C17 C24 1.512(6) . ? C18 C19 1.427(6) . ? C18 C23 1.422(6) . ? C19 C20 1.417(7) . ? C20 C21 1.367(7) . ? C20 H20A 0.9300 . ? C21 C22 1.395(7) . ? C21 H21A 0.9300 . ? C22 C23 1.349(7) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.503(6) . ? C26 C27 1.372(7) . ? C26 C31 1.425(7) . ? C27 C28 1.406(7) . ? C27 H27A 0.9300 . ? C28 C29 1.372(7) . ? C28 H28A 0.9300 . ? C29 C30 1.432(7) . ? C29 C36 1.495(6) . ? C30 C35 1.418(7) . ? C30 C31 1.426(7) . ? C31 C32 1.426(7) . ? C32 C33 1.365(8) . ? C32 H32A 0.9300 . ? C33 C34 1.400(9) . ? C33 H33A 0.9300 . ? C34 C35 1.358(8) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? N1A C39A 1.323(9) . ? N1A C37A 1.343(9) . ? N1A C40A 1.462(13) . ? N2A C39A 1.318(12) . ? N2A C38A 1.357(9) . ? N2A C41A 1.499(13) . ? C37A C38A 1.295(18) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.521(9) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C42A 1.598(9) . ? C43A C44A 1.604(9) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.564(9) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.557(9) . ? C45A H45A 0.9700 . ? C45A H45B 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N1B C39B 1.341(10) . ? N1B C37B 1.350(10) . ? N1B C40B 1.473(15) . ? N2B C39B 1.297(13) . ? N2B C38B 1.339(10) . ? N2B C41B 1.473(14) . ? C37B C38B 1.30(2) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C39B H39B 0.9300 . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C41B C42B 1.533(10) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.533(10) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C43B C44B 1.580(10) . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C44B C45B 1.553(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C45B C46B 1.529(10) . ? C45B H45C 0.9700 . ? C45B H45D 0.9700 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? C46B H46F 0.9600 . ? 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 O7 Tb1 O1 79.29(12) 4_565 . ? O7 Tb1 O5 145.42(14) 4_565 4_566 ? O1 Tb1 O5 77.33(14) . 4_566 ? O7 Tb1 O6 77.68(13) 4_565 2_644 ? O1 Tb1 O6 80.79(15) . 2_644 ? O5 Tb1 O6 122.60(13) 4_566 2_644 ? O7 Tb1 O3 82.42(13) 4_565 . ? O1 Tb1 O3 99.01(15) . . ? O5 Tb1 O3 76.53(13) 4_566 . ? O6 Tb1 O3 159.79(13) 2_644 . ? O7 Tb1 O2 141.21(13) 4_565 3_655 ? O1 Tb1 O2 124.95(13) . 3_655 ? O5 Tb1 O2 73.35(14) 4_566 3_655 ? O6 Tb1 O2 77.48(14) 2_644 3_655 ? O3 Tb1 O2 117.45(14) . 3_655 ? O7 Tb1 Cl1 77.67(9) 4_565 . ? O1 Tb1 Cl1 156.53(9) . . ? O5 Tb1 Cl1 125.25(11) 4_566 . ? O6 Tb1 Cl1 89.98(11) 2_644 . ? O3 Tb1 Cl1 82.33(10) . . ? O2 Tb1 Cl1 73.01(9) 3_655 . ? O11 Tb2 O4 96.36(13) 4_565 . ? O11 Tb2 O10 80.88(14) 4_565 3 ? O4 Tb2 O10 155.60(13) . 3 ? O11 Tb2 O8 80.15(12) 4_565 4_565 ? O4 Tb2 O8 77.24(12) . 4_565 ? O10 Tb2 O8 78.40(12) 3 4_565 ? O11 Tb2 O9 75.11(12) 4_565 . ? O4 Tb2 O9 74.29(12) . . ? O10 Tb2 O9 127.26(12) 3 . ? O8 Tb2 O9 139.52(13) 4_565 . ? O11 Tb2 O12 122.98(13) 4_565 2_545 ? O4 Tb2 O12 117.82(13) . 2_545 ? O10 Tb2 O12 82.86(13) 3 2_545 ? O8 Tb2 O12 147.35(13) 4_565 2_545 ? O9 Tb2 O12 72.69(13) . 2_545 ? O11 Tb2 Cl1 161.79(9) 4_565 . ? O4 Tb2 Cl1 83.34(9) . . ? O10 Tb2 Cl1 91.87(9) 3 . ? O8 Tb2 Cl1 82.05(9) 4_565 . ? O9 Tb2 Cl1 121.84(9) . . ? O12 Tb2 Cl1 72.04(9) 2_545 . ? Tb2 Cl1 Tb1 112.00(4) . . ? C1 O1 Tb1 144.8(3) . . ? C1 O2 Tb1 142.7(3) . 3_655 ? C13 O3 Tb1 139.4(3) . . ? C12 O5 Tb1 164.3(4) . 4_565 ? C13 O4 Tb2 144.3(3) . . ? C12 O6 Tb1 128.0(3) . 2_654 ? C24 O7 Tb1 158.9(3) . 4_566 ? C24 O8 Tb2 133.1(3) . 4_566 ? C25 O9 Tb2 136.6(3) . . ? C25 O10 Tb2 140.1(3) . 3 ? C36 O11 Tb2 162.5(4) . 4_566 ? C36 O12 Tb2 112.7(3) . 2 ? O1 C1 O2 126.0(5) . . ? O1 C1 C2 116.7(4) . . ? O2 C1 C2 117.4(4) . . ? C3 C2 C7 119.8(4) . . ? C3 C2 C1 116.5(4) . . ? C7 C2 C1 123.8(4) . . ? C2 C3 C4 120.9(5) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C5 C4 C3 121.0(4) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 120.1(4) . . ? C4 C5 C12 117.2(4) . . ? C6 C5 C12 122.8(4) . . ? C11 C6 C7 119.2(4) . . ? C11 C6 C5 122.4(4) . . ? C7 C6 C5 118.4(4) . . ? C8 C7 C6 118.4(4) . . ? C8 C7 C2 121.9(4) . . ? C6 C7 C2 119.7(4) . . ? C9 C8 C7 120.4(5) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 121.4(5) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C11 C10 C9 120.5(5) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C6 120.1(5) . . ? C10 C11 H11A 120.0 . . ? C6 C11 H11A 120.0 . . ? O5 C12 O6 123.7(5) . . ? O5 C12 C5 118.3(4) . . ? O6 C12 C5 118.0(4) . . ? O3 C13 O4 123.3(5) . . ? O3 C13 C14 117.1(4) . . ? O4 C13 C14 119.5(4) . . ? C15 C14 C19 118.9(4) . . ? C15 C14 C13 116.8(5) . . ? C19 C14 C13 124.3(4) . . ? C14 C15 C16 122.2(5) . . ? C14 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? C15 C16 C17 121.4(5) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C16 C17 C18 118.8(4) . . ? C16 C17 C24 115.7(4) . . ? C18 C17 C24 125.5(4) . . ? C19 C18 C23 118.3(4) . . ? C19 C18 C17 119.3(4) . . ? C23 C18 C17 122.4(4) . . ? C20 C19 C18 118.4(4) . . ? C20 C19 C14 122.2(4) . . ? C18 C19 C14 119.5(4) . . ? C21 C20 C19 121.1(5) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C20 C21 C22 120.2(5) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 120.8(5) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C18 121.3(5) . . ? C22 C23 H23A 119.4 . . ? C18 C23 H23A 119.4 . . ? O7 C24 O8 125.5(4) . . ? O7 C24 C17 115.5(4) . . ? O8 C24 C17 119.1(4) . . ? O9 C25 O10 125.2(5) . . ? O9 C25 C26 118.9(4) . . ? O10 C25 C26 115.8(5) . . ? C27 C26 C31 119.6(4) . . ? C27 C26 C25 118.0(5) . . ? C31 C26 C25 122.3(4) . . ? C26 C27 C28 121.2(5) . . ? C26 C27 H27A 119.4 . . ? C28 C27 H27A 119.4 . . ? C29 C28 C27 120.5(5) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.8 . . ? C28 C29 C30 120.0(4) . . ? C28 C29 C36 118.7(5) . . ? C30 C29 C36 121.2(5) . . ? C35 C30 C31 118.9(5) . . ? C35 C30 C29 122.4(5) . . ? C31 C30 C29 118.6(5) . . ? C32 C31 C30 118.5(5) . . ? C32 C31 C26 122.0(5) . . ? C30 C31 C26 119.4(4) . . ? C33 C32 C31 120.2(5) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 120.9(6) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C35 C34 C33 120.6(6) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C30 120.8(5) . . ? C34 C35 H35A 119.6 . . ? C30 C35 H35A 119.6 . . ? O11 C36 O12 123.3(4) . . ? O11 C36 C29 118.9(5) . . ? O12 C36 C29 117.7(4) . . ? C39A N1A C37A 108.8(12) . . ? C39A N1A C40A 126.5(11) . . ? C37A N1A C40A 124.8(9) . . ? C39A N2A C38A 107.3(10) . . ? C39A N2A C41A 122.3(8) . . ? C38A N2A C41A 130.3(11) . . ? C38A C37A N1A 107.4(13) . . ? C38A C37A H37A 126.3 . . ? N1A C37A H37A 126.3 . . ? C37A C38A N2A 108.8(13) . . ? C37A C38A H38A 125.6 . . ? N2A C38A H38A 125.6 . . ? N2A C39A N1A 107.7(10) . . ? N2A C39A H39A 126.1 . . ? N1A C39A H39A 126.1 . . ? N1A C40A H40A 109.5 . . ? N1A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? N1A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? N2A C41A C42A 120.1(11) . . ? N2A C41A H41A 107.3 . . ? C42A C41A H41A 107.3 . . ? N2A C41A H41B 107.3 . . ? C42A C41A H41B 107.3 . . ? H41A C41A H41B 106.9 . . ? C42A C43A C44A 95.7(8) . . ? C42A C43A H43A 112.6 . . ? C44A C43A H43A 112.6 . . ? C42A C43A H43B 112.6 . . ? C44A C43A H43B 112.6 . . ? H43A C43A H43B 110.1 . . ? C41A C42A C43A 109.4(10) . . ? C41A C42A H42A 109.8 . . ? C43A C42A H42A 109.8 . . ? C41A C42A H42B 109.8 . . ? C43A C42A H42B 109.8 . . ? H42A C42A H42B 108.2 . . ? C45A C44A C43A 117.3(9) . . ? C45A C44A H44A 108.0 . . ? C43A C44A H44A 108.0 . . ? C45A C44A H44B 108.0 . . ? C43A C44A H44B 108.0 . . ? H44A C44A H44B 107.2 . . ? C46A C45A C44A 109.4(9) . . ? C46A C45A H45A 109.8 . . ? C44A C45A H45A 109.8 . . ? C46A C45A H45B 109.8 . . ? C44A C45A H45B 109.8 . . ? H45A C45A H45B 108.2 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C39B N1B C37B 111.8(16) . . ? C39B N1B C40B 125.9(14) . . ? C37B N1B C40B 122.3(11) . . ? C39B N2B C38B 110.0(12) . . ? C39B N2B C41B 127.7(12) . . ? C38B N2B C41B 122.3(13) . . ? C38B C37B N1B 103.9(16) . . ? C38B C37B H37B 128.1 . . ? N1B C37B H37B 128.1 . . ? C37B C38B N2B 110.1(16) . . ? C37B C38B H38B 124.9 . . ? N2B C38B H38B 124.9 . . ? N2B C39B N1B 104.2(12) . . ? N2B C39B H39B 127.9 . . ? N1B C39B H39B 127.9 . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N2B C41B C42B 104.0(13) . . ? N2B C41B H41C 111.0 . . ? C42B C41B H41C 111.0 . . ? N2B C41B H41D 111.0 . . ? C42B C41B H41D 111.0 . . ? H41C C41B H41D 109.0 . . ? C43B C42B C41B 86.9(13) . . ? C43B C42B H42C 114.2 . . ? C41B C42B H42C 114.2 . . ? C43B C42B H42D 114.2 . . ? C41B C42B H42D 114.2 . . ? H42C C42B H42D 111.3 . . ? C42B C43B C44B 118.4(13) . . ? C42B C43B H43C 107.7 . . ? C44B C43B H43C 107.7 . . ? C42B C43B H43D 107.7 . . ? C44B C43B H43D 107.7 . . ? H43C C43B H43D 107.1 . . ? C45B C44B C43B 113.7(12) . . ? C45B C44B H44C 108.8 . . ? C43B C44B H44C 108.8 . . ? C45B C44B H44D 108.8 . . ? C43B C44B H44D 108.8 . . ? H44C C44B H44D 107.7 . . ? C46B C45B C44B 114.9(11) . . ? C46B C45B H45C 108.5 . . ? C44B C45B H45C 108.5 . . ? C46B C45B H45D 108.5 . . ? C44B C45B H45D 108.5 . . ? H45C C45B H45D 107.5 . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C45B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Tb2 Cl1 Tb1 63.8(3) 4_565 . . . ? O4 Tb2 Cl1 Tb1 -26.32(10) . . . . ? O10 Tb2 Cl1 Tb1 129.68(10) 3 . . . ? O8 Tb2 Cl1 Tb1 51.67(9) 4_565 . . . ? O9 Tb2 Cl1 Tb1 -93.15(11) . . . . ? O12 Tb2 Cl1 Tb1 -148.44(11) 2_545 . . . ? O7 Tb1 Cl1 Tb2 -38.98(10) 4_565 . . . ? O1 Tb1 Cl1 Tb2 -50.1(3) . . . . ? O5 Tb1 Cl1 Tb2 112.37(12) 4_566 . . . ? O6 Tb1 Cl1 Tb2 -116.37(10) 2_644 . . . ? O3 Tb1 Cl1 Tb2 44.88(11) . . . . ? O2 Tb1 Cl1 Tb2 166.72(12) 3_655 . . . ? O7 Tb1 O1 C1 -154.3(6) 4_565 . . . ? O5 Tb1 O1 C1 51.4(6) 4_566 . . . ? O6 Tb1 O1 C1 -75.2(6) 2_644 . . . ? O3 Tb1 O1 C1 125.3(6) . . . . ? O2 Tb1 O1 C1 -7.6(7) 3_655 . . . ? Cl1 Tb1 O1 C1 -143.2(5) . . . . ? O7 Tb1 O3 C13 31.3(6) 4_565 . . . ? O1 Tb1 O3 C13 109.1(6) . . . . ? O5 Tb1 O3 C13 -176.3(6) 4_566 . . . ? O6 Tb1 O3 C13 21.3(9) 2_644 . . . ? O2 Tb1 O3 C13 -113.5(6) 3_655 . . . ? Cl1 Tb1 O3 C13 -47.2(6) . . . . ? O11 Tb2 O4 C13 162.4(6) 4_565 . . . ? O10 Tb2 O4 C13 -115.7(6) 3 . . . ? O8 Tb2 O4 C13 -119.2(6) 4_565 . . . ? O9 Tb2 O4 C13 89.8(6) . . . . ? O12 Tb2 O4 C13 29.7(6) 2_545 . . . ? Cl1 Tb2 O4 C13 -35.9(6) . . . . ? O11 Tb2 O9 C25 17.0(5) 4_565 . . . ? O4 Tb2 O9 C25 118.2(5) . . . . ? O10 Tb2 O9 C25 -48.9(5) 3 . . . ? O8 Tb2 O9 C25 71.2(5) 4_565 . . . ? O12 Tb2 O9 C25 -115.3(5) 2_545 . . . ? Cl1 Tb2 O9 C25 -170.3(4) . . . . ? Tb1 O1 C1 O2 -4.6(10) . . . . ? Tb1 O1 C1 C2 173.9(4) . . . . ? Tb1 O2 C1 O1 18.0(10) 3_655 . . . ? Tb1 O2 C1 C2 -160.4(4) 3_655 . . . ? O1 C1 C2 C3 -42.8(7) . . . . ? O2 C1 C2 C3 135.8(5) . . . . ? O1 C1 C2 C7 137.0(5) . . . . ? O2 C1 C2 C7 -44.4(7) . . . . ? C7 C2 C3 C4 2.2(8) . . . . ? C1 C2 C3 C4 -178.0(5) . . . . ? C2 C3 C4 C5 -0.5(9) . . . . ? C3 C4 C5 C6 -3.0(8) . . . . ? C3 C4 C5 C12 176.1(5) . . . . ? C4 C5 C6 C11 -174.3(5) . . . . ? C12 C5 C6 C11 6.7(8) . . . . ? C4 C5 C6 C7 4.6(7) . . . . ? C12 C5 C6 C7 -174.5(5) . . . . ? C11 C6 C7 C8 -1.8(7) . . . . ? C5 C6 C7 C8 179.3(5) . . . . ? C11 C6 C7 C2 176.1(5) . . . . ? C5 C6 C7 C2 -2.8(7) . . . . ? C3 C2 C7 C8 177.3(5) . . . . ? C1 C2 C7 C8 -2.5(8) . . . . ? C3 C2 C7 C6 -0.5(8) . . . . ? C1 C2 C7 C6 179.7(5) . . . . ? C6 C7 C8 C9 2.0(8) . . . . ? C2 C7 C8 C9 -175.9(5) . . . . ? C7 C8 C9 C10 -0.7(9) . . . . ? C8 C9 C10 C11 -0.8(9) . . . . ? C9 C10 C11 C6 0.9(9) . . . . ? C7 C6 C11 C10 0.4(8) . . . . ? C5 C6 C11 C10 179.3(5) . . . . ? Tb1 O5 C12 O6 20.4(18) 4_565 . . . ? Tb1 O5 C12 C5 -156.8(11) 4_565 . . . ? Tb1 O6 C12 O5 2.7(8) 2_654 . . . ? Tb1 O6 C12 C5 179.8(3) 2_654 . . . ? C4 C5 C12 O5 36.4(7) . . . . ? C6 C5 C12 O5 -144.5(5) . . . . ? C4 C5 C12 O6 -140.9(5) . . . . ? C6 C5 C12 O6 38.2(7) . . . . ? Tb1 O3 C13 O4 4.2(9) . . . . ? Tb1 O3 C13 C14 -178.0(4) . . . . ? Tb2 O4 C13 O3 61.8(8) . . . . ? Tb2 O4 C13 C14 -115.9(5) . . . . ? O3 C13 C14 C15 -35.0(7) . . . . ? O4 C13 C14 C15 142.9(5) . . . . ? O3 C13 C14 C19 146.6(5) . . . . ? O4 C13 C14 C19 -35.6(8) . . . . ? C19 C14 C15 C16 0.9(9) . . . . ? C13 C14 C15 C16 -177.6(5) . . . . ? C14 C15 C16 C17 0.3(9) . . . . ? C15 C16 C17 C18 0.2(8) . . . . ? C15 C16 C17 C24 -178.5(5) . . . . ? C16 C17 C18 C19 -1.9(7) . . . . ? C24 C17 C18 C19 176.7(4) . . . . ? C16 C17 C18 C23 -179.6(5) . . . . ? C24 C17 C18 C23 -1.1(7) . . . . ? C23 C18 C19 C20 1.7(7) . . . . ? C17 C18 C19 C20 -176.1(4) . . . . ? C23 C18 C19 C14 -179.2(4) . . . . ? C17 C18 C19 C14 3.0(7) . . . . ? C15 C14 C19 C20 176.5(5) . . . . ? C13 C14 C19 C20 -5.1(8) . . . . ? C15 C14 C19 C18 -2.5(7) . . . . ? C13 C14 C19 C18 175.9(4) . . . . ? C18 C19 C20 C21 -0.1(8) . . . . ? C14 C19 C20 C21 -179.2(5) . . . . ? C19 C20 C21 C22 -1.2(9) . . . . ? C20 C21 C22 C23 0.8(9) . . . . ? C21 C22 C23 C18 0.9(8) . . . . ? C19 C18 C23 C22 -2.2(7) . . . . ? C17 C18 C23 C22 175.6(5) . . . . ? Tb1 O7 C24 O8 7.0(13) 4_566 . . . ? Tb1 O7 C24 C17 -171.6(7) 4_566 . . . ? Tb2 O8 C24 O7 -35.6(7) 4_566 . . . ? Tb2 O8 C24 C17 143.0(3) 4_566 . . . ? C16 C17 C24 O7 33.2(7) . . . . ? C18 C17 C24 O7 -145.4(5) . . . . ? C16 C17 C24 O8 -145.5(5) . . . . ? C18 C17 C24 O8 35.9(7) . . . . ? Tb2 O9 C25 O10 35.1(8) . . . . ? Tb2 O9 C25 C26 -148.1(4) . . . . ? Tb2 O10 C25 O9 3.0(9) 3 . . . ? Tb2 O10 C25 C26 -173.9(3) 3 . . . ? O9 C25 C26 C27 -44.9(7) . . . . ? O10 C25 C26 C27 132.2(5) . . . . ? O9 C25 C26 C31 139.8(5) . . . . ? O10 C25 C26 C31 -43.1(7) . . . . ? C31 C26 C27 C28 6.3(8) . . . . ? C25 C26 C27 C28 -169.2(5) . . . . ? C26 C27 C28 C29 0.4(9) . . . . ? C27 C28 C29 C30 -7.2(8) . . . . ? C27 C28 C29 C36 169.3(5) . . . . ? C28 C29 C30 C35 -170.5(5) . . . . ? C36 C29 C30 C35 13.1(7) . . . . ? C28 C29 C30 C31 7.0(7) . . . . ? C36 C29 C30 C31 -169.4(4) . . . . ? C35 C30 C31 C32 -0.4(7) . . . . ? C29 C30 C31 C32 -178.0(4) . . . . ? C35 C30 C31 C26 177.2(5) . . . . ? C29 C30 C31 C26 -0.4(7) . . . . ? C27 C26 C31 C32 171.3(5) . . . . ? C25 C26 C31 C32 -13.4(7) . . . . ? C27 C26 C31 C30 -6.1(7) . . . . ? C25 C26 C31 C30 169.1(4) . . . . ? C30 C31 C32 C33 1.4(8) . . . . ? C26 C31 C32 C33 -176.1(5) . . . . ? C31 C32 C33 C34 -0.9(9) . . . . ? C32 C33 C34 C35 -0.7(10) . . . . ? C33 C34 C35 C30 1.7(9) . . . . ? C31 C30 C35 C34 -1.2(8) . . . . ? C29 C30 C35 C34 176.3(5) . . . . ? Tb2 O11 C36 O12 -97.0(12) 4_566 . . . ? Tb2 O11 C36 C29 85.4(12) 4_566 . . . ? Tb2 O12 C36 O11 11.7(6) 2 . . . ? Tb2 O12 C36 C29 -170.7(3) 2 . . . ? C28 C29 C36 O11 45.1(7) . . . . ? C30 C29 C36 O11 -138.5(5) . . . . ? C28 C29 C36 O12 -132.6(5) . . . . ? C30 C29 C36 O12 43.8(7) . . . . ? C39A N1A C37A C38A 0.1(2) . . . . ? C40A N1A C37A C38A 180.0(2) . . . . ? N1A C37A C38A N2A 0.1(3) . . . . ? C39A N2A C38A C37A -0.2(3) . . . . ? C41A N2A C38A C37A 179.7(2) . . . . ? C38A N2A C39A N1A 0.2(3) . . . . ? C41A N2A C39A N1A -179.6(2) . . . . ? C37A N1A C39A N2A -0.2(3) . . . . ? C40A N1A C39A N2A 179.9(2) . . . . ? C39A N2A C41A C42A 175.3(8) . . . . ? C38A N2A C41A C42A -4.5(9) . . . . ? N2A C41A C42A C43A -76.4(13) . . . . ? C44A C43A C42A C41A 176.6(11) . . . . ? C42A C43A C44A C45A -156.1(12) . . . . ? C43A C44A C45A C46A -46.3(19) . . . . ? C39B N1B C37B C38B -0.1(2) . . . . ? C40B N1B C37B C38B 179.9(2) . . . . ? N1B C37B C38B N2B 0.0(3) . . . . ? C39B N2B C38B C37B 0.1(3) . . . . ? C41B N2B C38B C37B -179.9(2) . . . . ? C38B N2B C39B N1B -0.2(3) . . . . ? C41B N2B C39B N1B 179.9(2) . . . . ? C37B N1B C39B N2B 0.2(3) . . . . ? C40B N1B C39B N2B -179.8(2) . . . . ? C39B N2B C41B C42B -2.7(12) . . . . ? C38B N2B C41B C42B 177.4(12) . . . . ? N2B C41B C42B C43B 118.6(11) . . . . ? C41B C42B C43B C44B 62(2) . . . . ? C42B C43B C44B C45B 178(2) . . . . ? C43B C44B C45B C46B -160(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.448 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.127 #===END data_compound-9 _database_code_depnum_ccdc_archive 'CCDC 876529' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Dy2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl Dy2 N2 O12' _chemical_formula_weight 1170.23 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.66597(18) _cell_length_b 14.78124(14) _cell_length_c 15.84149(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.3097(9) _cell_angle_gamma 90.00 _cell_volume 4124.91(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10636 _cell_measurement_theta_min 2.2585 _cell_measurement_theta_max 28.9062 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 3.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80934 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17185 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8551 _reflns_number_gt 6748 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8551 _refine_ls_number_parameters 605 _refine_ls_number_restraints 943 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.056 _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 Dy1 Dy 0.378438(9) 0.024605(10) -0.004156(9) 0.01254(5) Uani 1 1 d . . . Dy2 Dy 0.117500(9) 0.011639(11) -0.001260(9) 0.01324(5) Uani 1 1 d . . . Cl1 Cl 0.25226(5) -0.08217(6) 0.02562(6) 0.0283(2) Uani 1 1 d . . . O1 O 0.45051(16) 0.12171(18) -0.07760(18) 0.0344(7) Uani 1 1 d . . . O2 O 0.57552(15) 0.10445(18) -0.06563(17) 0.0346(7) Uani 1 1 d . . . O3 O 0.31561(16) 0.12857(19) 0.07354(18) 0.0371(7) Uani 1 1 d . . . O5 O 0.46946(16) 0.4280(2) -0.40278(18) 0.0398(8) Uani 1 1 d . . . O4 O 0.19261(15) 0.13352(17) 0.03156(16) 0.0281(6) Uani 1 1 d . . . O6 O 0.59467(16) 0.43058(19) -0.38618(17) 0.0364(7) Uani 1 1 d . . . O7 O 0.29141(15) 0.42965(19) 0.39060(16) 0.0299(7) Uani 1 1 d . . . O8 O 0.16738(14) 0.45585(17) 0.37016(14) 0.0239(6) Uani 1 1 d . . . O9 O 0.06125(15) 0.08535(18) 0.11076(16) 0.0281(6) Uani 1 1 d . . . O10 O -0.06410(15) 0.09984(18) 0.08676(16) 0.0294(7) Uani 1 1 d . . . O11 O 0.02046(16) 0.40846(18) 0.43551(16) 0.0313(7) Uani 1 1 d . . . O12 O -0.10127(16) 0.40216(18) 0.39529(17) 0.0329(7) Uani 1 1 d . . . C1 C 0.5157(2) 0.1416(2) -0.0949(2) 0.0241(9) Uani 1 1 d . . . C2 C 0.5225(2) 0.2155(2) -0.1598(2) 0.0215(8) Uani 1 1 d . . . C3 C 0.4715(2) 0.2133(3) -0.2299(3) 0.0296(10) Uani 1 1 d . . . H3A H 0.4343 0.1687 -0.2347 0.036 Uiso 1 1 calc R . . C4 C 0.4754(2) 0.2780(3) -0.2942(2) 0.0285(10) Uani 1 1 d . . . H4A H 0.4409 0.2750 -0.3415 0.034 Uiso 1 1 calc R . . C5 C 0.5284(2) 0.3451(3) -0.2892(2) 0.0222(8) Uani 1 1 d . . . C6 C 0.5804(2) 0.3526(2) -0.2160(2) 0.0205(8) Uani 1 1 d . . . C7 C 0.5777(2) 0.2857(2) -0.1509(2) 0.0214(8) Uani 1 1 d . . . C8 C 0.6293(2) 0.2936(3) -0.0786(2) 0.0305(10) Uani 1 1 d . . . H8A H 0.6298 0.2494 -0.0368 0.037 Uiso 1 1 calc R . . C9 C 0.6784(2) 0.3649(3) -0.0690(3) 0.0366(11) Uani 1 1 d . . . H9A H 0.7114 0.3690 -0.0206 0.044 Uiso 1 1 calc R . . C10 C 0.6793(2) 0.4311(3) -0.1310(3) 0.0346(10) Uani 1 1 d . . . H10A H 0.7125 0.4798 -0.1233 0.041 Uiso 1 1 calc R . . C11 C 0.6320(2) 0.4258(3) -0.2037(2) 0.0293(9) Uani 1 1 d . . . H11A H 0.6338 0.4703 -0.2450 0.035 Uiso 1 1 calc R . . C12 C 0.5311(2) 0.4065(3) -0.3644(2) 0.0254(9) Uani 1 1 d . . . C13 C 0.2496(2) 0.1605(2) 0.0768(2) 0.0246(9) Uani 1 1 d . . . C14 C 0.2398(2) 0.2324(2) 0.1418(2) 0.0220(8) Uani 1 1 d . . . C15 C 0.2832(2) 0.2251(3) 0.2165(3) 0.0339(10) Uani 1 1 d . . . H15A H 0.3173 0.1773 0.2237 0.041 Uiso 1 1 calc R . . C16 C 0.2781(2) 0.2863(3) 0.2821(2) 0.0327(10) Uani 1 1 d . . . H16A H 0.3095 0.2795 0.3315 0.039 Uiso 1 1 calc R . . C17 C 0.2270(2) 0.3573(2) 0.2751(2) 0.0197(8) Uani 1 1 d . . . C18 C 0.1799(2) 0.3677(2) 0.1984(2) 0.0171(8) Uani 1 1 d . . . C19 C 0.1878(2) 0.3061(2) 0.1306(2) 0.0206(8) Uani 1 1 d . . . C20 C 0.1441(2) 0.3219(3) 0.0529(2) 0.0305(10) Uani 1 1 d . . . H20A H 0.1490 0.2829 0.0076 0.037 Uiso 1 1 calc R . . C21 C 0.0954(2) 0.3930(3) 0.0437(2) 0.0342(10) Uani 1 1 d . . . H21A H 0.0676 0.4023 -0.0078 0.041 Uiso 1 1 calc R . . C22 C 0.0869(2) 0.4520(3) 0.1108(2) 0.0319(10) Uani 1 1 d . . . H22A H 0.0530 0.5001 0.1040 0.038 Uiso 1 1 calc R . . C23 C 0.1271(2) 0.4400(2) 0.1857(2) 0.0251(9) Uani 1 1 d . . . H23A H 0.1203 0.4798 0.2299 0.030 Uiso 1 1 calc R . . C24 C 0.2281(2) 0.4199(2) 0.3514(2) 0.0198(8) Uani 1 1 d . . . C25 C 0.0002(2) 0.1230(2) 0.1204(2) 0.0225(8) Uani 1 1 d . . . C26 C -0.0003(2) 0.2014(3) 0.1812(2) 0.0223(9) Uani 1 1 d . . . C27 C 0.0403(2) 0.1931(3) 0.2576(2) 0.0311(10) Uani 1 1 d . . . H27A H 0.0735 0.1447 0.2670 0.037 Uiso 1 1 calc R . . C28 C 0.0327(2) 0.2567(3) 0.3223(2) 0.0306(10) Uani 1 1 d . . . H28A H 0.0611 0.2504 0.3737 0.037 Uiso 1 1 calc R . . C29 C -0.0166(2) 0.3283(3) 0.3100(2) 0.0232(9) Uani 1 1 d . . . C30 C -0.0538(2) 0.3447(3) 0.2283(2) 0.0238(9) Uani 1 1 d . . . C31 C -0.0456(2) 0.2799(2) 0.1637(2) 0.0215(8) Uani 1 1 d . . . C32 C -0.0807(2) 0.2977(3) 0.0813(3) 0.0338(10) Uani 1 1 d . . . H32A H -0.0768 0.2559 0.0380 0.041 Uiso 1 1 calc R . . C33 C -0.1200(3) 0.3764(3) 0.0662(3) 0.0466(13) Uani 1 1 d . . . H33A H -0.1422 0.3878 0.0121 0.056 Uiso 1 1 calc R . . C34 C -0.1277(3) 0.4400(3) 0.1300(3) 0.0440(12) Uani 1 1 d . . . H34A H -0.1541 0.4934 0.1179 0.053 Uiso 1 1 calc R . . C35 C -0.0969(2) 0.4245(3) 0.2097(3) 0.0347(10) Uani 1 1 d . . . H35A H -0.1040 0.4661 0.2524 0.042 Uiso 1 1 calc R . . C36 C -0.0329(2) 0.3843(2) 0.3852(2) 0.0238(9) Uani 1 1 d . . . N1A N 0.2330(5) -0.2682(5) 0.2703(5) 0.0603(12) Uani 0.592(3) 1 d PDU A 1 N2A N 0.3025(5) -0.1493(5) 0.2706(5) 0.0662(12) Uani 0.592(3) 1 d PDU A 1 C37A C 0.2817(8) -0.2690(12) 0.3411(8) 0.0649(13) Uani 0.592(3) 1 d PDU A 1 H37A H 0.2843 -0.3136 0.3826 0.078 Uiso 0.592(3) 1 calc PR A 1 C38A C 0.3228(6) -0.1991(7) 0.3410(6) 0.0687(12) Uani 0.592(3) 1 d PDU A 1 H38A H 0.3609 -0.1841 0.3823 0.082 Uiso 0.592(3) 1 calc PR A 1 C39A C 0.2498(15) -0.1955(13) 0.2266(11) 0.0647(12) Uani 0.592(3) 1 d PDU A 1 H39A H 0.2280 -0.1797 0.1734 0.078 Uiso 0.592(3) 1 calc PR A 1 C40A C 0.1791(6) -0.3380(6) 0.2470(7) 0.0727(19) Uani 0.592(3) 1 d PDU A 1 H40A H 0.1517 -0.3224 0.1944 0.109 Uiso 0.592(3) 1 calc PR A 1 H40B H 0.1442 -0.3442 0.2902 0.109 Uiso 0.592(3) 1 calc PR A 1 H40C H 0.2054 -0.3942 0.2406 0.109 Uiso 0.592(3) 1 calc PR A 1 C41A C 0.3233(6) -0.0537(6) 0.2472(7) 0.0779(12) Uani 0.592(3) 1 d PDU A 1 H41A H 0.2785 -0.0165 0.2509 0.094 Uiso 0.592(3) 1 calc PR A 1 H41B H 0.3346 -0.0543 0.1882 0.094 Uiso 0.592(3) 1 calc PR A 1 C43A C 0.3474(6) 0.0413(8) 0.3743(7) 0.0924(14) Uani 0.592(3) 1 d PDU A 1 H43A H 0.3100 0.0860 0.3544 0.111 Uiso 0.592(3) 1 calc PR A 1 H43B H 0.3249 -0.0026 0.4104 0.111 Uiso 0.592(3) 1 calc PR A 1 C42A C 0.3903(6) -0.0051(7) 0.2979(6) 0.0802(13) Uani 0.592(3) 1 d PDU A 1 H42A H 0.4135 0.0400 0.2637 0.096 Uiso 0.592(3) 1 calc PR A 1 H42B H 0.4287 -0.0479 0.3195 0.096 Uiso 0.592(3) 1 calc PR A 1 C44A C 0.4240(6) 0.0860(8) 0.4179(6) 0.1001(15) Uani 0.592(3) 1 d PDU A 1 H44A H 0.4657 0.0463 0.4064 0.120 Uiso 0.592(3) 1 calc PR A 1 H44B H 0.4321 0.1424 0.3886 0.120 Uiso 0.592(3) 1 calc PR A 1 C45A C 0.4316(6) 0.1070(9) 0.5150(6) 0.1060(19) Uani 0.592(3) 1 d PDU A 1 H45A H 0.4392 0.0519 0.5478 0.127 Uiso 0.592(3) 1 calc PR A 1 H45B H 0.4736 0.1478 0.5291 0.127 Uiso 0.592(3) 1 calc PR A 1 C46A C 0.3554(7) 0.1518(9) 0.5315(8) 0.134(3) Uani 0.592(3) 1 d PDU A 1 H46A H 0.3565 0.1707 0.5896 0.201 Uiso 0.592(3) 1 calc PR A 1 H46B H 0.3149 0.1092 0.5200 0.201 Uiso 0.592(3) 1 calc PR A 1 H46C H 0.3473 0.2035 0.4953 0.201 Uiso 0.592(3) 1 calc PR A 1 N1B N 0.2071(7) -0.2817(7) 0.2278(7) 0.0603(12) Uani 0.408(3) 1 d PDU A 2 N2B N 0.2901(7) -0.2066(8) 0.2962(7) 0.0662(12) Uani 0.408(3) 1 d PDU A 2 C37B C 0.2183(8) -0.3210(9) 0.3056(7) 0.0649(13) Uani 0.408(3) 1 d PDU A 2 H37B H 0.1934 -0.3714 0.3253 0.078 Uiso 0.408(3) 1 calc PR A 2 C38B C 0.2693(13) -0.2752(15) 0.3454(12) 0.0687(12) Uani 0.408(3) 1 d PDU A 2 H38B H 0.2895 -0.2868 0.4003 0.082 Uiso 0.408(3) 1 calc PR A 2 C39B C 0.248(2) -0.2058(19) 0.2266(16) 0.0647(12) Uani 0.408(3) 1 d PDU A 2 H39B H 0.2468 -0.1620 0.1843 0.078 Uiso 0.408(3) 1 calc PR A 2 C40B C 0.1552(8) -0.3174(9) 0.1611(8) 0.0727(19) Uani 0.408(3) 1 d PDU A 2 H40D H 0.1566 -0.2802 0.1116 0.109 Uiso 0.408(3) 1 calc PR A 2 H40E H 0.1047 -0.3178 0.1795 0.109 Uiso 0.408(3) 1 calc PR A 2 H40F H 0.1699 -0.3780 0.1479 0.109 Uiso 0.408(3) 1 calc PR A 2 C41B C 0.3518(8) -0.1450(9) 0.3256(8) 0.0779(12) Uani 0.408(3) 1 d PDU A 2 H41C H 0.3989 -0.1780 0.3376 0.094 Uiso 0.408(3) 1 calc PR A 2 H41D H 0.3395 -0.1131 0.3763 0.094 Uiso 0.408(3) 1 calc PR A 2 C42B C 0.3583(10) -0.0794(9) 0.2521(8) 0.0802(13) Uani 0.408(3) 1 d PDU A 2 H42C H 0.4093 -0.0735 0.2340 0.096 Uiso 0.408(3) 1 calc PR A 2 H42D H 0.3219 -0.0903 0.2042 0.096 Uiso 0.408(3) 1 calc PR A 2 C43B C 0.3356(9) -0.0043(10) 0.3105(9) 0.0924(14) Uani 0.408(3) 1 d PDU A 2 H43C H 0.2892 -0.0233 0.3345 0.111 Uiso 0.408(3) 1 calc PR A 2 H43D H 0.3229 0.0482 0.2756 0.111 Uiso 0.408(3) 1 calc PR A 2 C44B C 0.3924(9) 0.0279(11) 0.3861(10) 0.1001(15) Uani 0.408(3) 1 d PDU A 2 H44C H 0.4043 -0.0222 0.4244 0.120 Uiso 0.408(3) 1 calc PR A 2 H44D H 0.4393 0.0488 0.3645 0.120 Uiso 0.408(3) 1 calc PR A 2 C45B C 0.3554(9) 0.1061(11) 0.4343(10) 0.1060(19) Uani 0.408(3) 1 d PDU A 2 H45C H 0.3339 0.1500 0.3937 0.127 Uiso 0.408(3) 1 calc PR A 2 H45D H 0.3143 0.0819 0.4649 0.127 Uiso 0.408(3) 1 calc PR A 2 C46B C 0.4120(12) 0.1524(12) 0.4955(12) 0.134(3) Uani 0.408(3) 1 d PDU A 2 H46D H 0.4518 0.1781 0.4651 0.201 Uiso 0.408(3) 1 calc PR A 2 H46E H 0.4333 0.1091 0.5358 0.201 Uiso 0.408(3) 1 calc PR A 2 H46F H 0.3871 0.1995 0.5247 0.201 Uiso 0.408(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01283(9) 0.01317(9) 0.01185(9) -0.00023(6) 0.00258(6) 0.00077(6) Dy2 0.01389(9) 0.01371(9) 0.01234(9) -0.00030(6) 0.00243(6) -0.00074(7) Cl1 0.0165(5) 0.0247(5) 0.0446(6) 0.0132(4) 0.0072(4) 0.0024(4) O1 0.0243(16) 0.0362(17) 0.0435(18) 0.0205(14) 0.0072(13) -0.0064(13) O2 0.0243(16) 0.0328(16) 0.0464(18) 0.0234(14) 0.0001(14) 0.0021(13) O3 0.0220(16) 0.0413(18) 0.0479(18) -0.0235(15) 0.0013(14) 0.0072(13) O5 0.0327(18) 0.0457(19) 0.0384(17) 0.0224(15) -0.0137(14) -0.0047(14) O4 0.0240(15) 0.0255(15) 0.0348(16) -0.0135(12) 0.0023(12) -0.0060(12) O6 0.0326(18) 0.0467(19) 0.0302(16) 0.0211(14) 0.0057(13) -0.0063(14) O7 0.0188(15) 0.0449(18) 0.0257(15) -0.0164(13) -0.0005(12) -0.0011(13) O8 0.0218(14) 0.0350(15) 0.0153(13) -0.0048(12) 0.0041(11) 0.0091(12) O9 0.0251(16) 0.0326(16) 0.0277(15) -0.0118(12) 0.0087(12) 0.0002(13) O10 0.0265(16) 0.0329(16) 0.0299(15) -0.0164(13) 0.0086(12) -0.0105(13) O11 0.0336(17) 0.0376(17) 0.0227(15) -0.0121(13) 0.0022(13) -0.0136(14) O12 0.0270(17) 0.0364(17) 0.0369(17) -0.0174(13) 0.0119(13) -0.0050(13) C1 0.019(2) 0.022(2) 0.031(2) 0.0103(17) 0.0019(17) -0.0019(16) C2 0.019(2) 0.022(2) 0.024(2) 0.0102(16) 0.0027(16) 0.0014(16) C3 0.019(2) 0.031(2) 0.038(2) 0.0123(19) -0.0035(18) -0.0080(18) C4 0.022(2) 0.036(2) 0.026(2) 0.0115(18) -0.0073(17) -0.0041(18) C5 0.020(2) 0.027(2) 0.0197(19) 0.0108(16) 0.0024(16) 0.0010(16) C6 0.017(2) 0.022(2) 0.0223(19) 0.0028(16) 0.0019(15) -0.0010(16) C7 0.019(2) 0.026(2) 0.0193(19) 0.0088(16) 0.0029(16) 0.0005(16) C8 0.034(3) 0.035(2) 0.021(2) 0.0092(18) -0.0019(18) -0.0019(19) C9 0.034(3) 0.048(3) 0.026(2) 0.001(2) -0.0045(19) -0.010(2) C10 0.033(3) 0.037(2) 0.035(2) -0.0031(19) 0.0035(19) -0.019(2) C11 0.031(2) 0.028(2) 0.030(2) 0.0078(18) 0.0067(18) -0.0066(18) C12 0.029(2) 0.025(2) 0.022(2) 0.0079(17) 0.0008(17) -0.0003(18) C13 0.020(2) 0.023(2) 0.032(2) -0.0077(17) 0.0083(17) -0.0033(17) C14 0.017(2) 0.024(2) 0.025(2) -0.0106(16) 0.0046(16) -0.0001(16) C15 0.030(3) 0.031(2) 0.040(3) -0.014(2) -0.002(2) 0.0132(19) C16 0.029(2) 0.041(3) 0.026(2) -0.0137(19) -0.0086(18) 0.013(2) C17 0.016(2) 0.025(2) 0.0185(19) -0.0059(15) 0.0037(15) 0.0014(16) C18 0.0164(19) 0.0177(18) 0.0172(18) -0.0022(14) 0.0017(15) -0.0005(15) C19 0.020(2) 0.0218(19) 0.0207(19) -0.0084(15) 0.0053(16) -0.0010(16) C20 0.040(3) 0.032(2) 0.019(2) -0.0073(17) -0.0021(18) -0.001(2) C21 0.037(3) 0.044(3) 0.020(2) 0.0019(19) -0.0077(18) 0.004(2) C22 0.039(3) 0.026(2) 0.030(2) 0.0008(18) -0.0028(19) 0.014(2) C23 0.023(2) 0.025(2) 0.027(2) -0.0059(17) 0.0039(17) 0.0052(17) C24 0.021(2) 0.0218(19) 0.0167(18) -0.0015(15) 0.0026(15) -0.0004(16) C25 0.026(2) 0.023(2) 0.0192(19) -0.0064(16) 0.0077(16) -0.0068(17) C26 0.023(2) 0.025(2) 0.020(2) -0.0087(16) 0.0074(16) -0.0064(17) C27 0.030(2) 0.030(2) 0.032(2) -0.0112(18) -0.0045(19) 0.0106(19) C28 0.028(2) 0.040(3) 0.022(2) -0.0133(18) -0.0062(18) 0.0084(19) C29 0.022(2) 0.025(2) 0.023(2) -0.0129(16) 0.0073(16) -0.0055(17) C30 0.023(2) 0.024(2) 0.026(2) -0.0046(17) 0.0074(17) -0.0067(17) C31 0.021(2) 0.022(2) 0.022(2) -0.0042(16) 0.0038(16) -0.0040(16) C32 0.042(3) 0.033(2) 0.025(2) -0.0008(18) -0.001(2) -0.005(2) C33 0.057(3) 0.048(3) 0.033(3) 0.013(2) -0.008(2) 0.000(3) C34 0.048(3) 0.038(3) 0.047(3) 0.011(2) 0.008(2) 0.014(2) C35 0.039(3) 0.029(2) 0.036(2) -0.0046(19) 0.005(2) 0.001(2) C36 0.029(2) 0.020(2) 0.024(2) -0.0057(16) 0.0093(17) -0.0074(17) N1A 0.069(3) 0.053(2) 0.063(3) 0.008(2) 0.028(2) 0.010(2) N2A 0.077(3) 0.063(2) 0.062(2) 0.005(2) 0.025(2) 0.006(2) C37A 0.076(3) 0.061(2) 0.061(2) 0.011(2) 0.025(2) 0.014(2) C38A 0.079(3) 0.064(2) 0.066(2) 0.007(2) 0.022(2) 0.011(2) C39A 0.073(2) 0.063(2) 0.061(2) 0.010(2) 0.022(2) 0.008(2) C40A 0.071(4) 0.064(4) 0.087(4) -0.008(4) 0.027(4) 0.010(3) C41A 0.085(3) 0.073(2) 0.079(2) 0.003(2) 0.025(2) 0.007(2) C43A 0.100(3) 0.087(3) 0.092(3) 0.002(2) 0.020(3) 0.006(3) C42A 0.087(3) 0.076(3) 0.081(2) 0.004(2) 0.028(2) 0.006(2) C44A 0.106(3) 0.092(3) 0.104(3) 0.001(3) 0.022(3) -0.001(3) C45A 0.111(4) 0.096(3) 0.114(3) 0.015(3) 0.023(3) 0.010(3) C46A 0.141(6) 0.111(6) 0.155(6) 0.000(5) 0.040(6) 0.007(6) N1B 0.069(3) 0.053(2) 0.063(3) 0.008(2) 0.028(2) 0.010(2) N2B 0.077(3) 0.063(2) 0.062(2) 0.005(2) 0.025(2) 0.006(2) C37B 0.076(3) 0.061(2) 0.061(2) 0.011(2) 0.025(2) 0.014(2) C38B 0.079(3) 0.064(2) 0.066(2) 0.007(2) 0.022(2) 0.011(2) C39B 0.073(2) 0.063(2) 0.061(2) 0.010(2) 0.022(2) 0.008(2) C40B 0.071(4) 0.064(4) 0.087(4) -0.008(4) 0.027(4) 0.010(3) C41B 0.085(3) 0.073(2) 0.079(2) 0.003(2) 0.025(2) 0.007(2) C42B 0.087(3) 0.076(3) 0.081(2) 0.004(2) 0.028(2) 0.006(2) C43B 0.100(3) 0.087(3) 0.092(3) 0.002(2) 0.020(3) 0.006(3) C44B 0.106(3) 0.092(3) 0.104(3) 0.001(3) 0.022(3) -0.001(3) C45B 0.111(4) 0.096(3) 0.114(3) 0.015(3) 0.023(3) 0.010(3) C46B 0.141(6) 0.111(6) 0.155(6) 0.000(5) 0.040(6) 0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O7 2.284(2) 4_565 ? Dy1 O1 2.293(3) . ? Dy1 O5 2.295(3) 4_566 ? Dy1 O6 2.302(3) 2_644 ? Dy1 O3 2.305(3) . ? Dy1 O2 2.321(2) 3_655 ? Dy1 Cl1 2.8000(9) . ? Dy2 O11 2.254(2) 4_565 ? Dy2 O4 2.274(2) . ? Dy2 O10 2.291(2) 3 ? Dy2 O8 2.329(2) 4_565 ? Dy2 O9 2.364(2) . ? Dy2 O12 2.365(2) 2_545 ? Dy2 Cl1 2.7603(9) . ? O1 C1 1.238(4) . ? O2 C1 1.249(4) . ? O2 Dy1 2.321(2) 3_655 ? O3 C13 1.262(4) . ? O5 C12 1.247(4) . ? O5 Dy1 2.295(3) 4_565 ? O4 C13 1.256(4) . ? O6 C12 1.251(5) . ? O6 Dy1 2.302(3) 2_654 ? O7 C24 1.246(4) . ? O7 Dy1 2.284(2) 4_566 ? O8 C24 1.253(4) . ? O8 Dy2 2.329(2) 4_566 ? O9 C25 1.234(4) . ? O10 C25 1.265(4) . ? O10 Dy2 2.291(2) 3 ? O11 C36 1.240(4) . ? O11 Dy2 2.254(2) 4_566 ? O12 C36 1.258(5) . ? O12 Dy2 2.365(2) 2 ? C1 C2 1.511(5) . ? C2 C3 1.378(5) . ? C2 C7 1.423(5) . ? C3 C4 1.402(5) . ? C3 H3A 0.9300 . ? C4 C5 1.362(5) . ? C4 H4A 0.9300 . ? C5 C6 1.429(5) . ? C5 C12 1.501(5) . ? C6 C11 1.419(5) . ? C6 C7 1.432(5) . ? C7 C8 1.413(5) . ? C8 C9 1.365(5) . ? C8 H8A 0.9300 . ? C9 C10 1.388(5) . ? C9 H9A 0.9300 . ? C10 C11 1.374(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.499(5) . ? C14 C15 1.366(5) . ? C14 C19 1.427(5) . ? C15 C16 1.385(5) . ? C15 H15A 0.9300 . ? C16 C17 1.383(5) . ? C16 H16A 0.9300 . ? C17 C18 1.428(5) . ? C17 C24 1.521(5) . ? C18 C23 1.422(5) . ? C18 C19 1.424(4) . ? C19 C20 1.421(5) . ? C20 C21 1.360(5) . ? C20 H20A 0.9300 . ? C21 C22 1.392(5) . ? C21 H21A 0.9300 . ? C22 C23 1.348(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.507(5) . ? C26 C27 1.365(5) . ? C26 C31 1.425(5) . ? C27 C28 1.404(5) . ? C27 H27A 0.9300 . ? C28 C29 1.374(5) . ? C28 H28A 0.9300 . ? C29 C30 1.427(5) . ? C29 C36 1.497(5) . ? C30 C31 1.418(5) . ? C30 C35 1.422(5) . ? C31 C32 1.427(5) . ? C32 C33 1.367(6) . ? C32 H32A 0.9300 . ? C33 C34 1.395(6) . ? C33 H33A 0.9300 . ? C34 C35 1.356(6) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? N1A C39A 1.326(7) . ? N1A C37A 1.361(8) . ? N1A C40A 1.433(10) . ? N2A C39A 1.311(9) . ? N2A C38A 1.361(7) . ? N2A C41A 1.513(10) . ? C37A C38A 1.263(14) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.555(8) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C44A 1.613(9) . ? C43A C42A 1.627(9) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.565(8) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.540(9) . ? C45A H45A 0.9700 . ? C45A H45B 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N1B C39B 1.338(8) . ? N1B C37B 1.364(9) . ? N1B C40B 1.445(12) . ? N2B C39B 1.282(10) . ? N2B C38B 1.347(9) . ? N2B C41B 1.468(11) . ? C37B C38B 1.258(17) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C39B H39B 0.9300 . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C41B C42B 1.527(10) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.519(9) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C43B C44B 1.578(10) . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C44B C45B 1.556(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C45B C46B 1.505(10) . ? C45B H45C 0.9700 . ? C45B H45D 0.9700 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? C46B H46F 0.9600 . ? 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 O7 Dy1 O1 79.24(9) 4_565 . ? O7 Dy1 O5 144.91(11) 4_565 4_566 ? O1 Dy1 O5 77.14(11) . 4_566 ? O7 Dy1 O6 78.09(10) 4_565 2_644 ? O1 Dy1 O6 80.85(11) . 2_644 ? O5 Dy1 O6 122.61(10) 4_566 2_644 ? O7 Dy1 O3 82.40(10) 4_565 . ? O1 Dy1 O3 99.30(11) . . ? O5 Dy1 O3 76.29(10) 4_566 . ? O6 Dy1 O3 160.12(10) 2_644 . ? O7 Dy1 O2 141.60(10) 4_565 3_655 ? O1 Dy1 O2 124.61(10) . 3_655 ? O5 Dy1 O2 73.48(10) 4_566 3_655 ? O6 Dy1 O2 77.20(10) 2_644 3_655 ? O3 Dy1 O2 117.33(11) . 3_655 ? O7 Dy1 Cl1 77.83(7) 4_565 . ? O1 Dy1 Cl1 156.60(7) . . ? O5 Dy1 Cl1 125.37(8) 4_566 . ? O6 Dy1 Cl1 89.94(8) 2_644 . ? O3 Dy1 Cl1 82.21(8) . . ? O2 Dy1 Cl1 73.23(7) 3_655 . ? O11 Dy2 O4 95.61(10) 4_565 . ? O11 Dy2 O10 81.28(10) 4_565 3 ? O4 Dy2 O10 155.81(10) . 3 ? O11 Dy2 O8 80.12(9) 4_565 4_565 ? O4 Dy2 O8 77.52(9) . 4_565 ? O10 Dy2 O8 78.31(9) 3 4_565 ? O11 Dy2 O9 75.14(9) 4_565 . ? O4 Dy2 O9 74.59(9) . . ? O10 Dy2 O9 126.71(9) 3 . ? O8 Dy2 O9 140.29(9) 4_565 . ? O11 Dy2 O12 123.05(10) 4_565 2_545 ? O4 Dy2 O12 118.66(10) . 2_545 ? O10 Dy2 O12 82.01(10) 3 2_545 ? O8 Dy2 O12 146.72(10) 4_565 2_545 ? O9 Dy2 O12 72.68(9) . 2_545 ? O11 Dy2 Cl1 161.85(7) 4_565 . ? O4 Dy2 Cl1 83.17(7) . . ? O10 Dy2 Cl1 92.41(7) 3 . ? O8 Dy2 Cl1 81.95(7) 4_565 . ? O9 Dy2 Cl1 121.47(7) . . ? O12 Dy2 Cl1 72.30(7) 2_545 . ? Dy2 Cl1 Dy1 112.28(3) . . ? C1 O1 Dy1 145.2(2) . . ? C1 O2 Dy1 142.6(3) . 3_655 ? C13 O3 Dy1 139.0(2) . . ? C12 O5 Dy1 163.4(3) . 4_565 ? C13 O4 Dy2 144.2(3) . . ? C12 O6 Dy1 128.3(2) . 2_654 ? C24 O7 Dy1 158.1(3) . 4_566 ? C24 O8 Dy2 133.0(2) . 4_566 ? C25 O9 Dy2 136.2(2) . . ? C25 O10 Dy2 139.5(3) . 3 ? C36 O11 Dy2 162.2(3) . 4_566 ? C36 O12 Dy2 113.7(2) . 2 ? O1 C1 O2 126.1(3) . . ? O1 C1 C2 116.4(3) . . ? O2 C1 C2 117.4(3) . . ? C3 C2 C7 119.9(3) . . ? C3 C2 C1 116.8(3) . . ? C7 C2 C1 123.3(3) . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 121.7(3) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 C12 117.2(3) . . ? C6 C5 C12 122.8(3) . . ? C11 C6 C5 122.5(3) . . ? C11 C6 C7 118.9(3) . . ? C5 C6 C7 118.5(3) . . ? C8 C7 C2 122.4(3) . . ? C8 C7 C6 118.1(3) . . ? C2 C7 C6 119.4(3) . . ? C9 C8 C7 121.4(4) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C8 C9 C10 120.4(4) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 120.9(4) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C10 C11 C6 120.2(4) . . ? C10 C11 H11A 119.9 . . ? C6 C11 H11A 119.9 . . ? O5 C12 O6 124.2(4) . . ? O5 C12 C5 117.5(4) . . ? O6 C12 C5 118.2(3) . . ? O4 C13 O3 124.1(3) . . ? O4 C13 C14 119.2(3) . . ? O3 C13 C14 116.6(3) . . ? C15 C14 C19 118.9(3) . . ? C15 C14 C13 116.9(3) . . ? C19 C14 C13 124.2(3) . . ? C14 C15 C16 122.3(4) . . ? C14 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? C17 C16 C15 121.0(4) . . ? C17 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? C16 C17 C18 119.0(3) . . ? C16 C17 C24 115.4(3) . . ? C18 C17 C24 125.6(3) . . ? C23 C18 C19 118.2(3) . . ? C23 C18 C17 122.4(3) . . ? C19 C18 C17 119.3(3) . . ? C20 C19 C18 118.1(3) . . ? C20 C19 C14 122.4(3) . . ? C18 C19 C14 119.5(3) . . ? C21 C20 C19 121.3(4) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C22 120.4(4) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C18 121.4(4) . . ? C22 C23 H23A 119.3 . . ? C18 C23 H23A 119.3 . . ? O7 C24 O8 125.8(3) . . ? O7 C24 C17 115.1(3) . . ? O8 C24 C17 119.1(3) . . ? O9 C25 O10 126.2(3) . . ? O9 C25 C26 118.3(3) . . ? O10 C25 C26 115.4(3) . . ? C27 C26 C31 119.7(3) . . ? C27 C26 C25 118.0(4) . . ? C31 C26 C25 122.1(3) . . ? C26 C27 C28 120.9(4) . . ? C26 C27 H27A 119.6 . . ? C28 C27 H27A 119.6 . . ? C29 C28 C27 120.5(4) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C28 C29 C30 120.2(3) . . ? C28 C29 C36 118.1(3) . . ? C30 C29 C36 121.6(4) . . ? C31 C30 C35 119.5(4) . . ? C31 C30 C29 118.3(3) . . ? C35 C30 C29 122.1(4) . . ? C30 C31 C26 119.8(3) . . ? C30 C31 C32 118.3(4) . . ? C26 C31 C32 121.8(3) . . ? C33 C32 C31 119.9(4) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C32 C33 C34 121.4(4) . . ? C32 C33 H33A 119.3 . . ? C34 C33 H33A 119.3 . . ? C35 C34 C33 120.5(4) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C30 120.3(4) . . ? C34 C35 H35A 119.9 . . ? C30 C35 H35A 119.9 . . ? O11 C36 O12 123.3(3) . . ? O11 C36 C29 119.2(4) . . ? O12 C36 C29 117.5(3) . . ? C39A N1A C37A 106.5(10) . . ? C39A N1A C40A 128.3(9) . . ? C37A N1A C40A 125.0(8) . . ? C39A N2A C38A 106.7(8) . . ? C39A N2A C41A 122.1(7) . . ? C38A N2A C41A 130.7(9) . . ? C38A C37A N1A 108.7(11) . . ? C38A C37A H37A 125.7 . . ? N1A C37A H37A 125.7 . . ? C37A C38A N2A 109.1(11) . . ? C37A C38A H38A 125.4 . . ? N2A C38A H38A 125.4 . . ? N2A C39A N1A 108.8(7) . . ? N2A C39A H39A 125.6 . . ? N1A C39A H39A 125.6 . . ? N1A C40A H40A 109.5 . . ? N1A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? N1A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? N2A C41A C42A 119.6(8) . . ? N2A C41A H41A 107.4 . . ? C42A C41A H41A 107.4 . . ? N2A C41A H41B 107.4 . . ? C42A C41A H41B 107.4 . . ? H41A C41A H41B 106.9 . . ? C44A C43A C42A 94.0(7) . . ? C44A C43A H43A 112.9 . . ? C42A C43A H43A 112.9 . . ? C44A C43A H43B 112.9 . . ? C42A C43A H43B 112.9 . . ? H43A C43A H43B 110.3 . . ? C41A C42A C43A 101.6(8) . . ? C41A C42A H42A 111.5 . . ? C43A C42A H42A 111.5 . . ? C41A C42A H42B 111.5 . . ? C43A C42A H42B 111.5 . . ? H42A C42A H42B 109.3 . . ? C45A C44A C43A 120.6(9) . . ? C45A C44A H44A 107.2 . . ? C43A C44A H44A 107.2 . . ? C45A C44A H44B 107.2 . . ? C43A C44A H44B 107.2 . . ? H44A C44A H44B 106.8 . . ? C46A C45A C44A 104.0(8) . . ? C46A C45A H45A 111.0 . . ? C44A C45A H45A 111.0 . . ? C46A C45A H45B 111.0 . . ? C44A C45A H45B 111.0 . . ? H45A C45A H45B 109.0 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C39B N1B C37B 109.1(13) . . ? C39B N1B C40B 127.7(11) . . ? C37B N1B C40B 123.1(9) . . ? C39B N2B C38B 109.9(10) . . ? C39B N2B C41B 129.4(10) . . ? C38B N2B C41B 120.8(10) . . ? C38B C37B N1B 105.9(13) . . ? C38B C37B H37B 127.1 . . ? N1B C37B H37B 127.1 . . ? C37B C38B N2B 109.4(13) . . ? C37B C38B H38B 125.3 . . ? N2B C38B H38B 125.3 . . ? N2B C39B N1B 105.0(10) . . ? N2B C39B H39B 127.5 . . ? N1B C39B H39B 127.5 . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N2B C41B C42B 104.4(10) . . ? N2B C41B H41C 110.9 . . ? C42B C41B H41C 110.9 . . ? N2B C41B H41D 110.9 . . ? C42B C41B H41D 110.9 . . ? H41C C41B H41D 108.9 . . ? C43B C42B C41B 87.8(11) . . ? C43B C42B H42C 114.0 . . ? C41B C42B H42C 114.0 . . ? C43B C42B H42D 114.0 . . ? C41B C42B H42D 114.0 . . ? H42C C42B H42D 111.2 . . ? C42B C43B C44B 120.1(12) . . ? C42B C43B H43C 107.3 . . ? C44B C43B H43C 107.3 . . ? C42B C43B H43D 107.3 . . ? C44B C43B H43D 107.3 . . ? H43C C43B H43D 106.9 . . ? C45B C44B C43B 109.2(10) . . ? C45B C44B H44C 109.8 . . ? C43B C44B H44C 109.8 . . ? C45B C44B H44D 109.8 . . ? C43B C44B H44D 109.8 . . ? H44C C44B H44D 108.3 . . ? C46B C45B C44B 111.7(10) . . ? C46B C45B H45C 109.3 . . ? C44B C45B H45C 109.3 . . ? C46B C45B H45D 109.3 . . ? C44B C45B H45D 109.3 . . ? H45C C45B H45D 107.9 . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C45B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Dy2 Cl1 Dy1 60.5(2) 4_565 . . . ? O4 Dy2 Cl1 Dy1 -26.67(7) . . . . ? O10 Dy2 Cl1 Dy1 129.46(7) 3 . . . ? O8 Dy2 Cl1 Dy1 51.63(7) 4_565 . . . ? O9 Dy2 Cl1 Dy1 -93.90(8) . . . . ? O12 Dy2 Cl1 Dy1 -149.72(8) 2_545 . . . ? O7 Dy1 Cl1 Dy2 -38.60(8) 4_565 . . . ? O1 Dy1 Cl1 Dy2 -50.2(2) . . . . ? O5 Dy1 Cl1 Dy2 112.27(9) 4_566 . . . ? O6 Dy1 Cl1 Dy2 -116.42(8) 2_644 . . . ? O3 Dy1 Cl1 Dy2 45.25(8) . . . . ? O2 Dy1 Cl1 Dy2 166.94(9) 3_655 . . . ? O7 Dy1 O1 C1 -155.0(5) 4_565 . . . ? O5 Dy1 O1 C1 51.1(5) 4_566 . . . ? O6 Dy1 O1 C1 -75.5(5) 2_644 . . . ? O3 Dy1 O1 C1 124.6(5) . . . . ? O2 Dy1 O1 C1 -8.1(5) 3_655 . . . ? Cl1 Dy1 O1 C1 -143.5(4) . . . . ? O7 Dy1 O3 C13 31.6(4) 4_565 . . . ? O1 Dy1 O3 C13 109.3(4) . . . . ? O5 Dy1 O3 C13 -176.5(4) 4_566 . . . ? O6 Dy1 O3 C13 20.5(6) 2_644 . . . ? O2 Dy1 O3 C13 -113.6(4) 3_655 . . . ? Cl1 Dy1 O3 C13 -47.1(4) . . . . ? O11 Dy2 O4 C13 163.4(4) 4_565 . . . ? O10 Dy2 O4 C13 -115.4(4) 3 . . . ? O8 Dy2 O4 C13 -118.0(4) 4_565 . . . ? O9 Dy2 O4 C13 90.5(4) . . . . ? O12 Dy2 O4 C13 30.7(5) 2_545 . . . ? Cl1 Dy2 O4 C13 -34.8(4) . . . . ? O11 Dy2 O9 C25 17.1(4) 4_565 . . . ? O4 Dy2 O9 C25 117.4(4) . . . . ? O10 Dy2 O9 C25 -49.7(4) 3 . . . ? O8 Dy2 O9 C25 70.4(4) 4_565 . . . ? O12 Dy2 O9 C25 -115.3(4) 2_545 . . . ? Cl1 Dy2 O9 C25 -170.9(3) . . . . ? Dy1 O1 C1 O2 -3.6(8) . . . . ? Dy1 O1 C1 C2 174.1(3) . . . . ? Dy1 O2 C1 O1 16.9(8) 3_655 . . . ? Dy1 O2 C1 C2 -160.7(3) 3_655 . . . ? O1 C1 C2 C3 -42.3(5) . . . . ? O2 C1 C2 C3 135.5(4) . . . . ? O1 C1 C2 C7 137.0(4) . . . . ? O2 C1 C2 C7 -45.2(6) . . . . ? C7 C2 C3 C4 2.4(6) . . . . ? C1 C2 C3 C4 -178.3(4) . . . . ? C2 C3 C4 C5 -0.9(6) . . . . ? C3 C4 C5 C6 -1.9(6) . . . . ? C3 C4 C5 C12 175.6(4) . . . . ? C4 C5 C6 C11 -174.0(4) . . . . ? C12 C5 C6 C11 8.7(6) . . . . ? C4 C5 C6 C7 3.0(6) . . . . ? C12 C5 C6 C7 -174.3(4) . . . . ? C3 C2 C7 C8 177.2(4) . . . . ? C1 C2 C7 C8 -2.1(6) . . . . ? C3 C2 C7 C6 -1.2(6) . . . . ? C1 C2 C7 C6 179.5(4) . . . . ? C11 C6 C7 C8 -2.8(6) . . . . ? C5 C6 C7 C8 -179.9(4) . . . . ? C11 C6 C7 C2 175.6(4) . . . . ? C5 C6 C7 C2 -1.5(6) . . . . ? C2 C7 C8 C9 -175.7(4) . . . . ? C6 C7 C8 C9 2.7(6) . . . . ? C7 C8 C9 C10 -0.8(7) . . . . ? C8 C9 C10 C11 -1.0(7) . . . . ? C9 C10 C11 C6 0.8(7) . . . . ? C5 C6 C11 C10 178.1(4) . . . . ? C7 C6 C11 C10 1.1(6) . . . . ? Dy1 O5 C12 O6 19.6(13) 4_565 . . . ? Dy1 O5 C12 C5 -158.2(8) 4_565 . . . ? Dy1 O6 C12 O5 3.1(6) 2_654 . . . ? Dy1 O6 C12 C5 -179.2(2) 2_654 . . . ? C4 C5 C12 O5 37.7(6) . . . . ? C6 C5 C12 O5 -144.9(4) . . . . ? C4 C5 C12 O6 -140.2(4) . . . . ? C6 C5 C12 O6 37.2(6) . . . . ? Dy2 O4 C13 O3 60.9(7) . . . . ? Dy2 O4 C13 C14 -116.5(4) . . . . ? Dy1 O3 C13 O4 4.2(7) . . . . ? Dy1 O3 C13 C14 -178.4(3) . . . . ? O4 C13 C14 C15 143.0(4) . . . . ? O3 C13 C14 C15 -34.5(5) . . . . ? O4 C13 C14 C19 -36.0(6) . . . . ? O3 C13 C14 C19 146.5(4) . . . . ? C19 C14 C15 C16 0.4(7) . . . . ? C13 C14 C15 C16 -178.7(4) . . . . ? C14 C15 C16 C17 1.4(7) . . . . ? C15 C16 C17 C18 -0.9(6) . . . . ? C15 C16 C17 C24 -179.3(4) . . . . ? C16 C17 C18 C23 -178.7(4) . . . . ? C24 C17 C18 C23 -0.4(6) . . . . ? C16 C17 C18 C19 -1.3(5) . . . . ? C24 C17 C18 C19 177.0(3) . . . . ? C23 C18 C19 C20 2.0(5) . . . . ? C17 C18 C19 C20 -175.5(3) . . . . ? C23 C18 C19 C14 -179.5(3) . . . . ? C17 C18 C19 C14 3.0(5) . . . . ? C15 C14 C19 C20 175.9(4) . . . . ? C13 C14 C19 C20 -5.1(6) . . . . ? C15 C14 C19 C18 -2.6(6) . . . . ? C13 C14 C19 C18 176.4(3) . . . . ? C18 C19 C20 C21 -1.0(6) . . . . ? C14 C19 C20 C21 -179.5(4) . . . . ? C19 C20 C21 C22 -0.3(7) . . . . ? C20 C21 C22 C23 0.5(7) . . . . ? C21 C22 C23 C18 0.6(7) . . . . ? C19 C18 C23 C22 -1.8(6) . . . . ? C17 C18 C23 C22 175.6(4) . . . . ? Dy1 O7 C24 O8 7.1(10) 4_566 . . . ? Dy1 O7 C24 C17 -172.2(5) 4_566 . . . ? Dy2 O8 C24 O7 -37.0(6) 4_566 . . . ? Dy2 O8 C24 C17 142.3(3) 4_566 . . . ? C16 C17 C24 O7 32.6(5) . . . . ? C18 C17 C24 O7 -145.7(4) . . . . ? C16 C17 C24 O8 -146.7(4) . . . . ? C18 C17 C24 O8 35.0(5) . . . . ? Dy2 O9 C25 O10 35.7(6) . . . . ? Dy2 O9 C25 C26 -147.7(3) . . . . ? Dy2 O10 C25 O9 3.3(7) 3 . . . ? Dy2 O10 C25 C26 -173.4(2) 3 . . . ? O9 C25 C26 C27 -44.0(5) . . . . ? O10 C25 C26 C27 133.0(4) . . . . ? O9 C25 C26 C31 140.4(4) . . . . ? O10 C25 C26 C31 -42.6(5) . . . . ? C31 C26 C27 C28 6.0(6) . . . . ? C25 C26 C27 C28 -169.7(4) . . . . ? C26 C27 C28 C29 0.6(7) . . . . ? C27 C28 C29 C30 -7.3(6) . . . . ? C27 C28 C29 C36 169.2(4) . . . . ? C28 C29 C30 C31 7.3(6) . . . . ? C36 C29 C30 C31 -169.1(3) . . . . ? C28 C29 C30 C35 -171.3(4) . . . . ? C36 C29 C30 C35 12.3(6) . . . . ? C35 C30 C31 C26 177.8(4) . . . . ? C29 C30 C31 C26 -0.8(6) . . . . ? C35 C30 C31 C32 0.7(6) . . . . ? C29 C30 C31 C32 -177.9(4) . . . . ? C27 C26 C31 C30 -5.8(6) . . . . ? C25 C26 C31 C30 169.7(3) . . . . ? C27 C26 C31 C32 171.2(4) . . . . ? C25 C26 C31 C32 -13.3(6) . . . . ? C30 C31 C32 C33 0.9(6) . . . . ? C26 C31 C32 C33 -176.2(4) . . . . ? C31 C32 C33 C34 -0.8(7) . . . . ? C32 C33 C34 C35 -1.0(8) . . . . ? C33 C34 C35 C30 2.6(7) . . . . ? C31 C30 C35 C34 -2.4(6) . . . . ? C29 C30 C35 C34 176.1(4) . . . . ? Dy2 O11 C36 O12 -93.7(9) 4_566 . . . ? Dy2 O11 C36 C29 88.6(9) 4_566 . . . ? Dy2 O12 C36 O11 12.6(5) 2 . . . ? Dy2 O12 C36 C29 -169.6(2) 2 . . . ? C28 C29 C36 O11 45.3(5) . . . . ? C30 C29 C36 O11 -138.2(4) . . . . ? C28 C29 C36 O12 -132.6(4) . . . . ? C30 C29 C36 O12 44.0(5) . . . . ? C39A N1A C37A C38A 2(2) . . . . ? C40A N1A C37A C38A 177.8(11) . . . . ? N1A C37A C38A N2A 0.4(19) . . . . ? C39A N2A C38A C37A -3(2) . . . . ? C41A N2A C38A C37A 168.2(13) . . . . ? C38A N2A C39A N1A 5(3) . . . . ? C41A N2A C39A N1A -167.5(14) . . . . ? C37A N1A C39A N2A -5(3) . . . . ? C40A N1A C39A N2A -179.7(14) . . . . ? C39A N2A C41A C42A -175(2) . . . . ? C38A N2A C41A C42A 14.2(16) . . . . ? N2A C41A C42A C43A -88.4(11) . . . . ? C44A C43A C42A C41A 179.7(9) . . . . ? C42A C43A C44A C45A -153.6(11) . . . . ? C43A C44A C45A C46A -45.1(15) . . . . ? C39B N1B C37B C38B -6(3) . . . . ? C40B N1B C37B C38B 176.8(19) . . . . ? N1B C37B C38B N2B 1(3) . . . . ? C39B N2B C38B C37B 4(4) . . . . ? C41B N2B C38B C37B -176.8(17) . . . . ? C38B N2B C39B N1B -8(4) . . . . ? C41B N2B C39B N1B 173.4(18) . . . . ? C37B N1B C39B N2B 8(4) . . . . ? C40B N1B C39B N2B -174.5(18) . . . . ? C39B N2B C41B C42B -2(3) . . . . ? C38B N2B C41B C42B 179.0(19) . . . . ? N2B C41B C42B C43B 116.5(12) . . . . ? C41B C42B C43B C44B 70.6(18) . . . . ? C42B C43B C44B C45B 179.0(15) . . . . ? C43B C44B C45B C46B -168.4(16) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.273 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.103 #===END data_compound-10 _database_code_depnum_ccdc_archive 'CCDC 876530' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Ho2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl Ho2 N2 O12' _chemical_formula_weight 1175.09 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.6148(5) _cell_length_b 14.7818(5) _cell_length_c 15.8066(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.043(3) _cell_angle_gamma 90.00 _cell_volume 4105.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9574 _cell_measurement_theta_min 2.2587 _cell_measurement_theta_max 28.8697 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 3.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88428 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17461 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 26.54 _reflns_number_total 8502 _reflns_number_gt 6320 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0650P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8502 _refine_ls_number_parameters 605 _refine_ls_number_restraints 939 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.009 _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 Ho1 Ho 0.378560(14) 0.024631(18) -0.004114(16) 0.01277(9) Uani 1 1 d . . . Ho2 Ho 0.117714(14) 0.011582(18) -0.001410(16) 0.01341(9) Uani 1 1 d . . . Cl1 Cl 0.25239(8) -0.08141(11) 0.02619(11) 0.0291(4) Uani 1 1 d . . . O1 O 0.4507(3) 0.1208(3) -0.0771(3) 0.0363(13) Uani 1 1 d . . . O2 O 0.5765(2) 0.1038(3) -0.0660(3) 0.0357(13) Uani 1 1 d . . . O3 O 0.3152(3) 0.1278(4) 0.0731(3) 0.0381(13) Uani 1 1 d . . . O5 O 0.4683(3) 0.4273(4) -0.4032(3) 0.0392(13) Uani 1 1 d . . . O4 O 0.1921(2) 0.1325(3) 0.0320(3) 0.0280(11) Uani 1 1 d . . . O6 O 0.5944(3) 0.4307(4) -0.3875(3) 0.0358(12) Uani 1 1 d . . . O7 O 0.2924(2) 0.4292(3) 0.3906(3) 0.0299(11) Uani 1 1 d . . . O8 O 0.1683(2) 0.4569(3) 0.3708(2) 0.0217(10) Uani 1 1 d . . . O9 O 0.0616(2) 0.0837(3) 0.1105(3) 0.0285(11) Uani 1 1 d . . . O10 O -0.0641(2) 0.0991(3) 0.0870(3) 0.0282(11) Uani 1 1 d . . . O11 O 0.0219(3) 0.4077(3) 0.4355(3) 0.0324(12) Uani 1 1 d . . . O12 O -0.1001(3) 0.4013(3) 0.3966(3) 0.0323(12) Uani 1 1 d . . . C1 C 0.5159(4) 0.1406(4) -0.0951(4) 0.0240(14) Uani 1 1 d . . . C2 C 0.5224(3) 0.2145(4) -0.1594(4) 0.0224(14) Uani 1 1 d . . . C3 C 0.4721(4) 0.2124(5) -0.2299(4) 0.0275(16) Uani 1 1 d . . . H3A H 0.4352 0.1673 -0.2347 0.033 Uiso 1 1 calc R . . C4 C 0.4754(4) 0.2774(5) -0.2951(4) 0.0268(16) Uani 1 1 d . . . H4A H 0.4409 0.2743 -0.3424 0.032 Uiso 1 1 calc R . . C5 C 0.5287(3) 0.3449(5) -0.2897(4) 0.0224(14) Uani 1 1 d . . . C6 C 0.5803(3) 0.3523(4) -0.2161(4) 0.0197(13) Uani 1 1 d . . . C7 C 0.5784(3) 0.2854(4) -0.1513(4) 0.0208(14) Uani 1 1 d . . . C8 C 0.6295(4) 0.2931(5) -0.0781(4) 0.0297(16) Uani 1 1 d . . . H8A H 0.6300 0.2489 -0.0362 0.036 Uiso 1 1 calc R . . C9 C 0.6780(4) 0.3654(5) -0.0690(5) 0.0372(19) Uani 1 1 d . . . H9A H 0.7105 0.3705 -0.0202 0.045 Uiso 1 1 calc R . . C10 C 0.6792(4) 0.4308(5) -0.1313(5) 0.0371(18) Uani 1 1 d . . . H10A H 0.7128 0.4791 -0.1239 0.044 Uiso 1 1 calc R . . C11 C 0.6315(4) 0.4258(5) -0.2042(4) 0.0295(16) Uani 1 1 d . . . H11A H 0.6329 0.4706 -0.2454 0.035 Uiso 1 1 calc R . . C12 C 0.5305(4) 0.4068(5) -0.3650(4) 0.0243(15) Uani 1 1 d . . . C13 C 0.2489(3) 0.1595(5) 0.0771(4) 0.0253(15) Uani 1 1 d . . . C14 C 0.2402(3) 0.2323(4) 0.1414(4) 0.0238(14) Uani 1 1 d . . . C15 C 0.2830(4) 0.2235(5) 0.2168(5) 0.0344(18) Uani 1 1 d . . . H15A H 0.3161 0.1748 0.2243 0.041 Uiso 1 1 calc R . . C16 C 0.2782(4) 0.2855(5) 0.2824(4) 0.0295(17) Uani 1 1 d . . . H16A H 0.3096 0.2786 0.3318 0.035 Uiso 1 1 calc R . . C17 C 0.2276(3) 0.3575(4) 0.2757(4) 0.0195(13) Uani 1 1 d . . . C18 C 0.1806(3) 0.3680(4) 0.1986(4) 0.0149(12) Uani 1 1 d . . . C19 C 0.1877(3) 0.3059(4) 0.1309(4) 0.0179(13) Uani 1 1 d . . . C20 C 0.1441(4) 0.3215(5) 0.0528(4) 0.0296(16) Uani 1 1 d . . . H20A H 0.1489 0.2823 0.0074 0.035 Uiso 1 1 calc R . . C21 C 0.0956(4) 0.3927(5) 0.0438(4) 0.0340(17) Uani 1 1 d . . . H21A H 0.0675 0.4019 -0.0075 0.041 Uiso 1 1 calc R . . C22 C 0.0880(4) 0.4518(5) 0.1108(4) 0.0316(16) Uani 1 1 d . . . H22A H 0.0549 0.5006 0.1037 0.038 Uiso 1 1 calc R . . C23 C 0.1273(3) 0.4400(4) 0.1857(4) 0.0236(14) Uani 1 1 d . . . H23A H 0.1197 0.4796 0.2300 0.028 Uiso 1 1 calc R . . C24 C 0.2285(3) 0.4196(4) 0.3521(4) 0.0186(13) Uani 1 1 d . . . C25 C -0.0005(4) 0.1224(5) 0.1201(4) 0.0229(14) Uani 1 1 d . . . C26 C -0.0004(3) 0.2007(4) 0.1803(4) 0.0210(14) Uani 1 1 d . . . C27 C 0.0403(4) 0.1917(5) 0.2579(4) 0.0315(17) Uani 1 1 d . . . H27A H 0.0727 0.1425 0.2675 0.038 Uiso 1 1 calc R . . C28 C 0.0333(4) 0.2558(5) 0.3220(4) 0.0301(17) Uani 1 1 d . . . H28A H 0.0623 0.2496 0.3732 0.036 Uiso 1 1 calc R . . C29 C -0.0157(3) 0.3278(4) 0.3104(4) 0.0203(14) Uani 1 1 d . . . C30 C -0.0534(3) 0.3437(4) 0.2291(4) 0.0219(14) Uani 1 1 d . . . C31 C -0.0455(3) 0.2794(4) 0.1636(4) 0.0206(14) Uani 1 1 d . . . C32 C -0.0809(4) 0.2971(5) 0.0815(4) 0.0324(17) Uani 1 1 d . . . H32A H -0.0772 0.2553 0.0380 0.039 Uiso 1 1 calc R . . C33 C -0.1205(5) 0.3759(6) 0.0671(5) 0.046(2) Uani 1 1 d . . . H33A H -0.1429 0.3873 0.0132 0.055 Uiso 1 1 calc R . . C34 C -0.1281(4) 0.4393(6) 0.1309(5) 0.042(2) Uani 1 1 d . . . H34A H -0.1551 0.4924 0.1192 0.050 Uiso 1 1 calc R . . C35 C -0.0958(4) 0.4234(5) 0.2107(5) 0.0341(17) Uani 1 1 d . . . H35A H -0.1019 0.4655 0.2534 0.041 Uiso 1 1 calc R . . C36 C -0.0314(4) 0.3833(4) 0.3855(4) 0.0237(14) Uani 1 1 d . . . N1A N 0.2334(8) -0.2687(9) 0.2704(8) 0.0712(15) Uani 0.572(5) 1 d PDU A 1 N2A N 0.2996(7) -0.1469(9) 0.2714(8) 0.0748(15) Uani 0.572(5) 1 d PDU A 1 C37A C 0.2824(9) -0.2710(14) 0.3403(10) 0.0730(16) Uani 0.572(5) 1 d PDU A 1 H37A H 0.2868 -0.3168 0.3807 0.088 Uiso 0.572(5) 1 calc PR A 1 C38A C 0.3210(10) -0.1989(11) 0.3401(9) 0.0751(15) Uani 0.572(5) 1 d PDU A 1 H38A H 0.3590 -0.1835 0.3813 0.090 Uiso 0.572(5) 1 calc PR A 1 C39A C 0.2443(8) -0.1920(8) 0.2280(8) 0.0728(15) Uani 0.572(5) 1 d PDU A 1 H39A H 0.2182 -0.1736 0.1777 0.087 Uiso 0.572(5) 1 calc PR A 1 C40A C 0.1793(9) -0.3398(11) 0.2482(11) 0.074(2) Uani 0.572(5) 1 d PDU A 1 H40A H 0.1514 -0.3250 0.1957 0.111 Uiso 0.572(5) 1 calc PR A 1 H40B H 0.1446 -0.3457 0.2921 0.111 Uiso 0.572(5) 1 calc PR A 1 H40C H 0.2059 -0.3958 0.2422 0.111 Uiso 0.572(5) 1 calc PR A 1 C41A C 0.3279(8) -0.0593(10) 0.2456(10) 0.0779(15) Uani 0.572(5) 1 d PDU A 1 H41A H 0.2836 -0.0204 0.2377 0.093 Uiso 0.572(5) 1 calc PR A 1 H41B H 0.3463 -0.0682 0.1899 0.093 Uiso 0.572(5) 1 calc PR A 1 C43A C 0.3591(9) 0.0538(14) 0.3708(10) 0.0861(16) Uani 0.572(5) 1 d PDU A 1 H43A H 0.3305 0.1062 0.3496 0.103 Uiso 0.572(5) 1 calc PR A 1 H43B H 0.3273 0.0177 0.4054 0.103 Uiso 0.572(5) 1 calc PR A 1 C42A C 0.3889(10) -0.0037(12) 0.2959(10) 0.0806(15) Uani 0.572(5) 1 d PDU A 1 H42A H 0.4122 0.0370 0.2571 0.097 Uiso 0.572(5) 1 calc PR A 1 H42B H 0.4282 -0.0444 0.3190 0.097 Uiso 0.572(5) 1 calc PR A 1 C44A C 0.4355(9) 0.0826(13) 0.4219(9) 0.0900(17) Uani 0.572(5) 1 d PDU A 1 H44A H 0.4712 0.0329 0.4197 0.108 Uiso 0.572(5) 1 calc PR A 1 H44B H 0.4567 0.1335 0.3929 0.108 Uiso 0.572(5) 1 calc PR A 1 C45A C 0.4302(9) 0.1093(15) 0.5165(9) 0.093(2) Uani 0.572(5) 1 d PDU A 1 H45A H 0.4725 0.1487 0.5339 0.112 Uiso 0.572(5) 1 calc PR A 1 H45B H 0.4344 0.0552 0.5513 0.112 Uiso 0.572(5) 1 calc PR A 1 C46A C 0.3543(10) 0.1584(15) 0.5319(12) 0.109(3) Uani 0.572(5) 1 d PDU A 1 H46A H 0.3550 0.1776 0.5900 0.163 Uiso 0.572(5) 1 calc PR A 1 H46B H 0.3124 0.1176 0.5199 0.163 Uiso 0.572(5) 1 calc PR A 1 H46C H 0.3485 0.2101 0.4954 0.163 Uiso 0.572(5) 1 calc PR A 1 N1B N 0.2092(8) -0.2813(9) 0.2307(12) 0.0712(15) Uani 0.428(5) 1 d PDU A 2 N2B N 0.2929(9) -0.2065(11) 0.2984(12) 0.0748(15) Uani 0.428(5) 1 d PDU A 2 C37B C 0.2174(12) -0.3222(14) 0.3077(11) 0.0730(16) Uani 0.428(5) 1 d PDU A 2 H37B H 0.1920 -0.3723 0.3271 0.088 Uiso 0.428(5) 1 calc PR A 2 C38B C 0.2684(12) -0.2747(14) 0.3461(15) 0.0751(15) Uani 0.428(5) 1 d PDU A 2 H38B H 0.2871 -0.2857 0.4016 0.090 Uiso 0.428(5) 1 calc PR A 2 C39B C 0.2554(9) -0.2094(11) 0.2238(11) 0.0728(15) Uani 0.428(5) 1 d PDU A 2 H39B H 0.2597 -0.1712 0.1776 0.087 Uiso 0.428(5) 1 calc PR A 2 C40B C 0.1553(11) -0.3134(15) 0.1636(12) 0.074(2) Uani 0.428(5) 1 d PDU A 2 H40D H 0.1576 -0.2752 0.1147 0.111 Uiso 0.428(5) 1 calc PR A 2 H40E H 0.1048 -0.3119 0.1828 0.111 Uiso 0.428(5) 1 calc PR A 2 H40F H 0.1679 -0.3743 0.1489 0.111 Uiso 0.428(5) 1 calc PR A 2 C41B C 0.3509(10) -0.1431(13) 0.3279(12) 0.0779(15) Uani 0.428(5) 1 d PDU A 2 H41C H 0.3982 -0.1737 0.3451 0.093 Uiso 0.428(5) 1 calc PR A 2 H41D H 0.3348 -0.1077 0.3751 0.093 Uiso 0.428(5) 1 calc PR A 2 C42B C 0.3595(15) -0.0837(13) 0.2500(11) 0.0806(15) Uani 0.428(5) 1 d PDU A 2 H42C H 0.4116 -0.0752 0.2351 0.097 Uiso 0.428(5) 1 calc PR A 2 H42D H 0.3258 -0.0991 0.2009 0.097 Uiso 0.428(5) 1 calc PR A 2 C43B C 0.3296(13) -0.0093(16) 0.3068(13) 0.0861(16) Uani 0.428(5) 1 d PDU A 2 H43C H 0.2802 -0.0287 0.3237 0.103 Uiso 0.428(5) 1 calc PR A 2 H43D H 0.3211 0.0444 0.2721 0.103 Uiso 0.428(5) 1 calc PR A 2 C44B C 0.3782(14) 0.0194(15) 0.3889(14) 0.0900(17) Uani 0.428(5) 1 d PDU A 2 H44C H 0.3821 -0.0322 0.4268 0.108 Uiso 0.428(5) 1 calc PR A 2 H44D H 0.4292 0.0334 0.3733 0.108 Uiso 0.428(5) 1 calc PR A 2 C45B C 0.3489(12) 0.1009(15) 0.4386(15) 0.093(2) Uani 0.428(5) 1 d PDU A 2 H45C H 0.3196 0.1396 0.3989 0.112 Uiso 0.428(5) 1 calc PR A 2 H45D H 0.3144 0.0783 0.4788 0.112 Uiso 0.428(5) 1 calc PR A 2 C46B C 0.4091(16) 0.1590(17) 0.4869(18) 0.109(3) Uani 0.428(5) 1 d PDU A 2 H46D H 0.4450 0.1803 0.4485 0.163 Uiso 0.428(5) 1 calc PR A 2 H46E H 0.4351 0.1235 0.5308 0.163 Uiso 0.428(5) 1 calc PR A 2 H46F H 0.3850 0.2097 0.5118 0.163 Uiso 0.428(5) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01162(14) 0.01364(15) 0.01307(15) -0.00023(11) 0.00103(10) 0.00021(10) Ho2 0.01263(14) 0.01419(16) 0.01339(15) -0.00003(11) 0.00072(10) -0.00090(10) Cl1 0.0150(7) 0.0250(9) 0.0477(10) 0.0142(8) 0.0040(7) 0.0014(6) O1 0.020(2) 0.036(3) 0.054(3) 0.021(3) 0.006(2) -0.005(2) O2 0.021(2) 0.033(3) 0.053(3) 0.022(3) 0.000(2) 0.002(2) O3 0.020(2) 0.044(3) 0.051(3) -0.024(3) 0.000(2) 0.004(2) O5 0.029(3) 0.045(3) 0.041(3) 0.021(3) -0.015(2) -0.005(2) O4 0.018(2) 0.023(2) 0.043(3) -0.014(2) 0.001(2) -0.0049(19) O6 0.029(3) 0.044(3) 0.035(3) 0.019(3) 0.001(2) -0.006(2) O7 0.019(2) 0.041(3) 0.029(3) -0.017(2) -0.0035(19) 0.005(2) O8 0.020(2) 0.033(3) 0.013(2) -0.005(2) 0.0066(16) 0.0068(19) O9 0.025(3) 0.033(3) 0.027(3) -0.015(2) 0.003(2) 0.002(2) O10 0.022(2) 0.031(3) 0.033(3) -0.014(2) 0.008(2) -0.009(2) O11 0.030(3) 0.035(3) 0.033(3) -0.012(2) 0.006(2) -0.014(2) O12 0.026(3) 0.036(3) 0.036(3) -0.015(2) 0.011(2) -0.004(2) C1 0.022(3) 0.021(3) 0.029(4) 0.008(3) 0.002(3) -0.006(3) C2 0.015(3) 0.024(4) 0.029(4) 0.014(3) 0.000(3) 0.002(3) C3 0.022(3) 0.029(4) 0.030(4) 0.010(3) -0.006(3) -0.007(3) C4 0.022(3) 0.033(4) 0.025(4) 0.016(3) -0.007(3) -0.008(3) C5 0.016(3) 0.029(4) 0.022(3) 0.009(3) 0.000(3) 0.002(3) C6 0.014(3) 0.023(3) 0.023(3) 0.006(3) 0.003(2) -0.002(2) C7 0.016(3) 0.025(3) 0.021(3) 0.008(3) 0.001(2) 0.002(3) C8 0.030(4) 0.033(4) 0.025(4) 0.011(3) -0.006(3) -0.004(3) C9 0.034(4) 0.047(5) 0.029(4) 0.002(4) -0.010(3) -0.010(3) C10 0.033(4) 0.042(5) 0.037(4) 0.001(4) 0.003(3) -0.020(3) C11 0.029(4) 0.026(4) 0.034(4) 0.008(3) 0.003(3) -0.007(3) C12 0.030(4) 0.023(4) 0.019(3) 0.010(3) -0.003(3) -0.002(3) C13 0.016(3) 0.030(4) 0.031(4) -0.008(3) 0.005(3) -0.001(3) C14 0.016(3) 0.024(4) 0.032(4) -0.007(3) 0.005(3) -0.002(3) C15 0.032(4) 0.025(4) 0.044(4) -0.017(3) -0.009(3) 0.018(3) C16 0.028(4) 0.040(4) 0.019(3) -0.011(3) -0.008(3) 0.013(3) C17 0.017(3) 0.020(3) 0.021(3) -0.011(3) -0.001(2) 0.001(2) C18 0.013(3) 0.017(3) 0.015(3) -0.003(3) 0.004(2) -0.004(2) C19 0.012(3) 0.021(3) 0.021(3) -0.009(3) 0.001(2) 0.000(2) C20 0.044(4) 0.027(4) 0.016(3) -0.007(3) -0.003(3) -0.002(3) C21 0.031(4) 0.046(5) 0.023(4) 0.004(3) -0.008(3) 0.002(3) C22 0.040(4) 0.019(3) 0.035(4) 0.002(3) 0.001(3) 0.013(3) C23 0.022(3) 0.018(3) 0.030(4) -0.008(3) 0.000(3) 0.005(3) C24 0.017(3) 0.024(3) 0.015(3) -0.005(3) 0.000(2) -0.001(2) C25 0.027(4) 0.024(4) 0.017(3) -0.002(3) 0.002(3) -0.005(3) C26 0.021(3) 0.022(3) 0.021(3) -0.009(3) 0.007(3) -0.004(3) C27 0.027(4) 0.029(4) 0.037(4) -0.013(3) -0.007(3) 0.010(3) C28 0.031(4) 0.039(4) 0.019(3) -0.006(3) -0.005(3) 0.007(3) C29 0.016(3) 0.025(4) 0.021(3) -0.011(3) 0.006(2) -0.001(3) C30 0.017(3) 0.022(3) 0.027(4) -0.004(3) 0.007(3) -0.004(3) C31 0.020(3) 0.020(3) 0.022(3) -0.003(3) 0.005(3) -0.006(3) C32 0.042(4) 0.034(4) 0.021(4) -0.003(3) -0.001(3) -0.005(3) C33 0.048(5) 0.047(5) 0.040(5) 0.014(4) -0.010(4) 0.000(4) C34 0.037(4) 0.045(5) 0.043(5) 0.005(4) 0.007(4) 0.013(4) C35 0.040(4) 0.026(4) 0.037(4) -0.001(3) 0.009(3) 0.001(3) C36 0.026(4) 0.021(3) 0.024(3) -0.010(3) 0.005(3) -0.009(3) N1A 0.081(3) 0.059(3) 0.077(3) 0.014(3) 0.032(3) 0.018(3) N2A 0.086(3) 0.063(3) 0.079(3) 0.012(3) 0.031(3) 0.017(3) C37A 0.084(3) 0.062(3) 0.076(3) 0.013(3) 0.031(3) 0.018(3) C38A 0.086(3) 0.063(3) 0.079(3) 0.013(3) 0.030(3) 0.018(3) C39A 0.083(3) 0.061(3) 0.077(3) 0.013(3) 0.030(3) 0.018(3) C40A 0.077(5) 0.064(5) 0.084(5) 0.009(4) 0.032(4) 0.015(4) C41A 0.088(3) 0.066(3) 0.083(3) 0.011(3) 0.030(3) 0.017(3) C43A 0.098(3) 0.073(3) 0.090(3) 0.014(3) 0.026(3) 0.016(3) C42A 0.091(3) 0.069(3) 0.085(3) 0.012(3) 0.030(3) 0.017(3) C44A 0.101(3) 0.076(3) 0.095(3) 0.014(3) 0.025(3) 0.013(3) C45A 0.106(4) 0.079(4) 0.098(4) 0.018(4) 0.024(4) 0.016(4) C46A 0.120(6) 0.091(6) 0.118(6) 0.015(6) 0.026(6) 0.008(6) N1B 0.081(3) 0.059(3) 0.077(3) 0.014(3) 0.032(3) 0.018(3) N2B 0.086(3) 0.063(3) 0.079(3) 0.012(3) 0.031(3) 0.017(3) C37B 0.084(3) 0.062(3) 0.076(3) 0.013(3) 0.031(3) 0.018(3) C38B 0.086(3) 0.063(3) 0.079(3) 0.013(3) 0.030(3) 0.018(3) C39B 0.083(3) 0.061(3) 0.077(3) 0.013(3) 0.030(3) 0.018(3) C40B 0.077(5) 0.064(5) 0.084(5) 0.009(4) 0.032(4) 0.015(4) C41B 0.088(3) 0.066(3) 0.083(3) 0.011(3) 0.030(3) 0.017(3) C42B 0.091(3) 0.069(3) 0.085(3) 0.012(3) 0.030(3) 0.017(3) C43B 0.098(3) 0.073(3) 0.090(3) 0.014(3) 0.026(3) 0.016(3) C44B 0.101(3) 0.076(3) 0.095(3) 0.014(3) 0.025(3) 0.013(3) C45B 0.106(4) 0.079(4) 0.098(4) 0.018(4) 0.024(4) 0.016(4) C46B 0.120(6) 0.091(6) 0.118(6) 0.015(6) 0.026(6) 0.008(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O1 2.275(4) . ? Ho1 O7 2.277(4) 4_565 ? Ho1 O5 2.278(4) 4_566 ? Ho1 O6 2.282(5) 2_644 ? Ho1 O3 2.292(5) . ? Ho1 O2 2.310(5) 3_655 ? Ho1 Cl1 2.7885(16) . ? Ho2 O11 2.243(4) 4_565 ? Ho2 O4 2.257(4) . ? Ho2 O10 2.285(4) 3 ? Ho2 O8 2.312(4) 4_565 ? Ho2 O9 2.343(4) . ? Ho2 O12 2.360(4) 2_545 ? Ho2 Cl1 2.7499(15) . ? O1 C1 1.238(7) . ? O2 C1 1.255(7) . ? O2 Ho1 2.310(5) 3_655 ? O3 C13 1.263(7) . ? O5 C12 1.251(7) . ? O5 Ho1 2.278(4) 4_565 ? O4 C13 1.253(7) . ? O6 C12 1.255(8) . ? O6 Ho1 2.282(5) 2_654 ? O7 C24 1.249(7) . ? O7 Ho1 2.277(4) 4_566 ? O8 C24 1.249(7) . ? O8 Ho2 2.312(4) 4_566 ? O9 C25 1.252(8) . ? O10 C25 1.251(7) . ? O10 Ho2 2.285(4) 3 ? O11 C36 1.237(7) . ? O11 Ho2 2.243(4) 4_566 ? O12 C36 1.263(7) . ? O12 Ho2 2.360(4) 2 ? C1 C2 1.502(9) . ? C2 C3 1.374(8) . ? C2 C7 1.438(9) . ? C3 C4 1.415(9) . ? C3 H3A 0.9300 . ? C4 C5 1.368(9) . ? C4 H4A 0.9300 . ? C5 C6 1.430(8) . ? C5 C12 1.503(8) . ? C6 C11 1.415(9) . ? C6 C7 1.426(8) . ? C7 C8 1.420(8) . ? C8 C9 1.369(9) . ? C8 H8A 0.9300 . ? C9 C10 1.381(10) . ? C9 H9A 0.9300 . ? C10 C11 1.380(9) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.495(9) . ? C14 C15 1.371(9) . ? C14 C19 1.430(8) . ? C15 C16 1.391(9) . ? C15 H15A 0.9300 . ? C16 C17 1.388(8) . ? C16 H16A 0.9300 . ? C17 C18 1.433(8) . ? C17 C24 1.515(8) . ? C18 C23 1.424(8) . ? C18 C19 1.421(8) . ? C19 C20 1.427(8) . ? C20 C21 1.356(10) . ? C20 H20A 0.9300 . ? C21 C22 1.388(10) . ? C21 H21A 0.9300 . ? C22 C23 1.339(9) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.498(9) . ? C26 C27 1.382(9) . ? C26 C31 1.423(9) . ? C27 C28 1.399(9) . ? C27 H27A 0.9300 . ? C28 C29 1.374(9) . ? C28 H28A 0.9300 . ? C29 C30 1.423(8) . ? C29 C36 1.485(8) . ? C30 C35 1.414(9) . ? C30 C31 1.420(9) . ? C31 C32 1.424(9) . ? C32 C33 1.368(10) . ? C32 H32A 0.9300 . ? C33 C34 1.389(11) . ? C33 H33A 0.9300 . ? C34 C35 1.367(10) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? N1A C39A 1.338(10) . ? N1A C37A 1.354(11) . ? N1A C40A 1.445(17) . ? N2A C39A 1.330(16) . ? N2A C38A 1.361(11) . ? N2A C41A 1.456(17) . ? C37A C38A 1.26(2) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.531(9) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C44A 1.579(9) . ? C43A C42A 1.577(9) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.555(9) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.556(9) . ? C45A H45A 0.9700 . ? C45A H45B 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N1B C39B 1.348(11) . ? N1B C37B 1.357(11) . ? N1B C40B 1.452(18) . ? N2B C39B 1.311(16) . ? N2B C38B 1.348(12) . ? N2B C41B 1.440(17) . ? C37B C38B 1.26(3) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C39B H39B 0.9300 . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C41B C42B 1.529(10) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.536(9) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C43B C44B 1.562(10) . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C44B C45B 1.547(9) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C45B C46B 1.526(10) . ? C45B H45C 0.9700 . ? C45B H45D 0.9700 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? C46B H46F 0.9600 . ? 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 Ho1 O7 79.01(16) . 4_565 ? O1 Ho1 O5 77.00(19) . 4_566 ? O7 Ho1 O5 144.28(19) 4_565 4_566 ? O1 Ho1 O6 81.14(19) . 2_644 ? O7 Ho1 O6 78.29(18) 4_565 2_644 ? O5 Ho1 O6 122.98(17) 4_566 2_644 ? O1 Ho1 O3 99.47(19) . . ? O7 Ho1 O3 82.24(18) 4_565 . ? O5 Ho1 O3 76.10(17) 4_566 . ? O6 Ho1 O3 160.04(17) 2_644 . ? O1 Ho1 O2 124.90(16) . 3_655 ? O7 Ho1 O2 141.78(18) 4_565 3_655 ? O5 Ho1 O2 73.92(19) 4_566 3_655 ? O6 Ho1 O2 77.17(19) 2_644 3_655 ? O3 Ho1 O2 117.04(19) . 3_655 ? O1 Ho1 Cl1 156.79(13) . . ? O7 Ho1 Cl1 78.22(11) 4_565 . ? O5 Ho1 Cl1 125.25(14) 4_566 . ? O6 Ho1 Cl1 89.88(13) 2_644 . ? O3 Ho1 Cl1 81.87(13) . . ? O2 Ho1 Cl1 72.90(11) 3_655 . ? O11 Ho2 O4 95.10(18) 4_565 . ? O11 Ho2 O10 81.45(18) 4_565 3 ? O4 Ho2 O10 156.17(17) . 3 ? O11 Ho2 O8 80.14(16) 4_565 4_565 ? O4 Ho2 O8 77.98(16) . 4_565 ? O10 Ho2 O8 78.20(15) 3 4_565 ? O11 Ho2 O9 75.47(16) 4_565 . ? O4 Ho2 O9 74.46(16) . . ? O10 Ho2 O9 126.45(15) 3 . ? O8 Ho2 O9 141.01(17) 4_565 . ? O11 Ho2 O12 123.21(16) 4_565 2_545 ? O4 Ho2 O12 119.05(17) . 2_545 ? O10 Ho2 O12 81.48(17) 3 2_545 ? O8 Ho2 O12 146.12(17) 4_565 2_545 ? O9 Ho2 O12 72.59(17) . 2_545 ? O11 Ho2 Cl1 161.85(12) 4_565 . ? O4 Ho2 Cl1 83.03(12) . . ? O10 Ho2 Cl1 92.96(12) 3 . ? O8 Ho2 Cl1 81.82(11) 4_565 . ? O9 Ho2 Cl1 120.87(12) . . ? O12 Ho2 Cl1 72.43(11) 2_545 . ? Ho2 Cl1 Ho1 112.39(6) . . ? C1 O1 Ho1 145.6(4) . . ? C1 O2 Ho1 141.8(4) . 3_655 ? C13 O3 Ho1 139.5(4) . . ? C12 O5 Ho1 162.7(5) . 4_565 ? C13 O4 Ho2 144.4(5) . . ? C12 O6 Ho1 128.5(4) . 2_654 ? C24 O7 Ho1 157.1(4) . 4_566 ? C24 O8 Ho2 133.0(4) . 4_566 ? C25 O9 Ho2 135.9(4) . . ? C25 O10 Ho2 139.9(4) . 3 ? C36 O11 Ho2 162.2(5) . 4_566 ? C36 O12 Ho2 114.7(4) . 2 ? O1 C1 O2 126.3(6) . . ? O1 C1 C2 116.3(6) . . ? O2 C1 C2 117.3(5) . . ? C3 C2 C7 119.2(6) . . ? C3 C2 C1 117.2(6) . . ? C7 C2 C1 123.7(5) . . ? C2 C3 C4 121.2(6) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 120.8(6) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 120.1(6) . . ? C4 C5 C12 116.5(6) . . ? C6 C5 C12 123.4(6) . . ? C11 C6 C7 119.0(6) . . ? C11 C6 C5 122.0(6) . . ? C7 C6 C5 119.0(6) . . ? C8 C7 C6 118.9(6) . . ? C8 C7 C2 121.5(6) . . ? C6 C7 C2 119.5(5) . . ? C9 C8 C7 120.2(6) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C10 120.8(6) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 121.3(7) . . ? C11 C10 H10A 119.4 . . ? C9 C10 H10A 119.4 . . ? C10 C11 C6 119.8(6) . . ? C10 C11 H11A 120.1 . . ? C6 C11 H11A 120.1 . . ? O5 C12 O6 124.6(6) . . ? O5 C12 C5 117.6(6) . . ? O6 C12 C5 117.7(5) . . ? O4 C13 O3 123.9(6) . . ? O4 C13 C14 120.0(6) . . ? O3 C13 C14 116.1(6) . . ? C15 C14 C19 118.9(6) . . ? C15 C14 C13 116.5(6) . . ? C19 C14 C13 124.5(6) . . ? C14 C15 C16 121.9(6) . . ? C14 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? C17 C16 C15 121.4(6) . . ? C17 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C16 C17 C18 118.5(5) . . ? C16 C17 C24 115.6(5) . . ? C18 C17 C24 125.8(5) . . ? C23 C18 C19 117.9(5) . . ? C23 C18 C17 122.5(5) . . ? C19 C18 C17 119.6(5) . . ? C18 C19 C20 118.4(6) . . ? C18 C19 C14 119.7(5) . . ? C20 C19 C14 121.8(6) . . ? C21 C20 C19 120.8(6) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 120.2(6) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 121.4(6) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C18 121.2(6) . . ? C22 C23 H23A 119.4 . . ? C18 C23 H23A 119.4 . . ? O8 C24 O7 125.8(6) . . ? O8 C24 C17 119.6(5) . . ? O7 C24 C17 114.6(5) . . ? O10 C25 O9 126.0(6) . . ? O10 C25 C26 116.0(6) . . ? O9 C25 C26 117.9(5) . . ? C27 C26 C31 119.4(6) . . ? C27 C26 C25 117.8(6) . . ? C31 C26 C25 122.5(6) . . ? C26 C27 C28 120.7(6) . . ? C26 C27 H27A 119.6 . . ? C28 C27 H27A 119.6 . . ? C29 C28 C27 120.9(6) . . ? C29 C28 H28A 119.5 . . ? C27 C28 H28A 119.5 . . ? C28 C29 C30 119.8(6) . . ? C28 C29 C36 118.2(6) . . ? C30 C29 C36 121.9(6) . . ? C35 C30 C31 119.0(6) . . ? C35 C30 C29 122.0(6) . . ? C31 C30 C29 118.9(6) . . ? C30 C31 C32 118.9(6) . . ? C30 C31 C26 119.6(6) . . ? C32 C31 C26 121.5(6) . . ? C33 C32 C31 119.5(7) . . ? C33 C32 H32A 120.2 . . ? C31 C32 H32A 120.2 . . ? C32 C33 C34 121.9(7) . . ? C32 C33 H33A 119.1 . . ? C34 C33 H33A 119.1 . . ? C35 C34 C33 119.9(7) . . ? C35 C34 H34A 120.1 . . ? C33 C34 H34A 120.1 . . ? C34 C35 C30 120.9(7) . . ? C34 C35 H35A 119.6 . . ? C30 C35 H35A 119.6 . . ? O11 C36 O12 122.8(6) . . ? O11 C36 C29 119.7(6) . . ? O12 C36 C29 117.5(5) . . ? C39A N1A C37A 108.9(17) . . ? C39A N1A C40A 127.6(16) . . ? C37A N1A C40A 123.5(12) . . ? C39A N2A C38A 106.3(14) . . ? C39A N2A C41A 123.6(12) . . ? C38A N2A C41A 130.1(15) . . ? C38A C37A N1A 106.8(18) . . ? C38A C37A H37A 126.6 . . ? N1A C37A H37A 126.6 . . ? C37A C38A N2A 111.1(18) . . ? C37A C38A H38A 124.5 . . ? N2A C38A H38A 124.5 . . ? N2A C39A N1A 106.9(13) . . ? N2A C39A H39A 126.5 . . ? N1A C39A H39A 126.5 . . ? N1A C40A H40A 109.5 . . ? N1A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? N1A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? N2A C41A C42A 125.1(15) . . ? N2A C41A H41A 106.1 . . ? C42A C41A H41A 106.1 . . ? N2A C41A H41B 106.1 . . ? C42A C41A H41B 106.1 . . ? H41A C41A H41B 106.3 . . ? C44A C43A C42A 102.3(9) . . ? C44A C43A H43A 111.3 . . ? C42A C43A H43A 111.3 . . ? C44A C43A H43B 111.3 . . ? C42A C43A H43B 111.3 . . ? H43A C43A H43B 109.2 . . ? C41A C42A C43A 114.8(13) . . ? C41A C42A H42A 108.6 . . ? C43A C42A H42A 108.6 . . ? C41A C42A H42B 108.6 . . ? C43A C42A H42B 108.6 . . ? H42A C42A H42B 107.5 . . ? C45A C44A C43A 117.0(10) . . ? C45A C44A H44A 108.0 . . ? C43A C44A H44A 108.0 . . ? C45A C44A H44B 108.0 . . ? C43A C44A H44B 108.0 . . ? H44A C44A H44B 107.3 . . ? C44A C45A C46A 112.3(9) . . ? C44A C45A H45A 109.2 . . ? C46A C45A H45A 109.2 . . ? C44A C45A H45B 109.1 . . ? C46A C45A H45B 109.2 . . ? H45A C45A H45B 107.9 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C39B N1B C37B 113.3(19) . . ? C39B N1B C40B 124.5(18) . . ? C37B N1B C40B 122.2(13) . . ? C39B N2B C38B 108.5(15) . . ? C39B N2B C41B 127.8(14) . . ? C38B N2B C41B 123.7(16) . . ? C38B C37B N1B 102(2) . . ? C38B C37B H37B 128.9 . . ? N1B C37B H37B 128.9 . . ? C37B C38B N2B 113(2) . . ? C37B C38B H38B 123.5 . . ? N2B C38B H38B 123.5 . . ? N2B C39B N1B 102.8(15) . . ? N2B C39B H39B 128.6 . . ? N1B C39B H39B 128.6 . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N2B C41B C42B 102.8(16) . . ? N2B C41B H41C 111.2 . . ? C42B C41B H41C 111.2 . . ? N2B C41B H41D 111.2 . . ? C42B C41B H41D 111.2 . . ? H41C C41B H41D 109.1 . . ? C43B C42B C41B 83.2(14) . . ? C43B C42B H42C 114.8 . . ? C41B C42B H42C 114.8 . . ? C43B C42B H42D 114.8 . . ? C41B C42B H42D 114.8 . . ? H42C C42B H42D 111.8 . . ? C42B C43B C44B 119.3(14) . . ? C42B C43B H43C 107.5 . . ? C44B C43B H43C 107.5 . . ? C42B C43B H43D 107.5 . . ? C44B C43B H43D 107.5 . . ? H43C C43B H43D 107.0 . . ? C45B C44B C43B 116.8(13) . . ? C45B C44B H44C 108.1 . . ? C43B C44B H44C 108.1 . . ? C45B C44B H44D 108.1 . . ? C43B C44B H44D 108.1 . . ? H44C C44B H44D 107.3 . . ? C46B C45B C44B 116.6(12) . . ? C46B C45B H45C 108.1 . . ? C44B C45B H45C 108.1 . . ? C46B C45B H45D 108.1 . . ? C44B C45B H45D 108.1 . . ? H45C C45B H45D 107.3 . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C45B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Ho2 Cl1 Ho1 57.8(5) 4_565 . . . ? O4 Ho2 Cl1 Ho1 -27.32(13) . . . . ? O10 Ho2 Cl1 Ho1 129.09(13) 3 . . . ? O8 Ho2 Cl1 Ho1 51.46(12) 4_565 . . . ? O9 Ho2 Cl1 Ho1 -94.52(15) . . . . ? O12 Ho2 Cl1 Ho1 -150.81(15) 2_545 . . . ? O1 Ho1 Cl1 Ho2 -49.6(4) . . . . ? O7 Ho1 Cl1 Ho2 -38.19(14) 4_565 . . . ? O5 Ho1 Cl1 Ho2 112.06(16) 4_566 . . . ? O6 Ho1 Cl1 Ho2 -116.25(14) 2_644 . . . ? O3 Ho1 Cl1 Ho2 45.51(14) . . . . ? O2 Ho1 Cl1 Ho2 167.14(16) 3_655 . . . ? O7 Ho1 O1 C1 -154.3(9) 4_565 . . . ? O5 Ho1 O1 C1 52.3(9) 4_566 . . . ? O6 Ho1 O1 C1 -74.7(9) 2_644 . . . ? O3 Ho1 O1 C1 125.6(9) . . . . ? O2 Ho1 O1 C1 -7.2(10) 3_655 . . . ? Cl1 Ho1 O1 C1 -143.0(7) . . . . ? O1 Ho1 O3 C13 110.1(8) . . . . ? O7 Ho1 O3 C13 32.7(8) 4_565 . . . ? O5 Ho1 O3 C13 -175.9(8) 4_566 . . . ? O6 Ho1 O3 C13 20.0(11) 2_644 . . . ? O2 Ho1 O3 C13 -112.5(8) 3_655 . . . ? Cl1 Ho1 O3 C13 -46.5(7) . . . . ? O11 Ho2 O4 C13 164.0(7) 4_565 . . . ? O10 Ho2 O4 C13 -115.6(8) 3 . . . ? O8 Ho2 O4 C13 -117.2(8) 4_565 . . . ? O9 Ho2 O4 C13 90.6(8) . . . . ? O12 Ho2 O4 C13 31.3(8) 2_545 . . . ? Cl1 Ho2 O4 C13 -34.2(7) . . . . ? O11 Ho2 O9 C25 16.9(6) 4_565 . . . ? O4 Ho2 O9 C25 116.5(7) . . . . ? O10 Ho2 O9 C25 -50.6(7) 3 . . . ? O8 Ho2 O9 C25 69.9(7) 4_565 . . . ? O12 Ho2 O9 C25 -115.5(6) 2_545 . . . ? Cl1 Ho2 O9 C25 -171.7(6) . . . . ? Ho1 O1 C1 O2 -4.5(14) . . . . ? Ho1 O1 C1 C2 174.1(6) . . . . ? Ho1 O2 C1 O1 16.9(13) 3_655 . . . ? Ho1 O2 C1 C2 -161.6(5) 3_655 . . . ? O1 C1 C2 C3 -43.6(9) . . . . ? O2 C1 C2 C3 135.1(7) . . . . ? O1 C1 C2 C7 137.2(7) . . . . ? O2 C1 C2 C7 -44.1(10) . . . . ? C7 C2 C3 C4 1.2(11) . . . . ? C1 C2 C3 C4 -178.0(6) . . . . ? C2 C3 C4 C5 -0.4(11) . . . . ? C3 C4 C5 C6 -2.1(10) . . . . ? C3 C4 C5 C12 176.2(6) . . . . ? C4 C5 C6 C11 -174.0(6) . . . . ? C12 C5 C6 C11 7.8(10) . . . . ? C4 C5 C6 C7 3.8(10) . . . . ? C12 C5 C6 C7 -174.4(6) . . . . ? C11 C6 C7 C8 -1.9(9) . . . . ? C5 C6 C7 C8 -179.7(6) . . . . ? C11 C6 C7 C2 174.9(6) . . . . ? C5 C6 C7 C2 -2.9(9) . . . . ? C3 C2 C7 C8 177.1(6) . . . . ? C1 C2 C7 C8 -3.7(10) . . . . ? C3 C2 C7 C6 0.5(10) . . . . ? C1 C2 C7 C6 179.6(6) . . . . ? C6 C7 C8 C9 2.1(10) . . . . ? C2 C7 C8 C9 -174.6(7) . . . . ? C7 C8 C9 C10 -1.3(12) . . . . ? C8 C9 C10 C11 0.4(12) . . . . ? C9 C10 C11 C6 -0.3(11) . . . . ? C7 C6 C11 C10 1.0(10) . . . . ? C5 C6 C11 C10 178.8(6) . . . . ? Ho1 O5 C12 O6 15(2) 4_565 . . . ? Ho1 O5 C12 C5 -161.0(14) 4_565 . . . ? Ho1 O6 C12 O5 4.7(11) 2_654 . . . ? Ho1 O6 C12 C5 -179.0(4) 2_654 . . . ? C4 C5 C12 O5 36.8(9) . . . . ? C6 C5 C12 O5 -144.9(7) . . . . ? C4 C5 C12 O6 -139.8(7) . . . . ? C6 C5 C12 O6 38.5(10) . . . . ? Ho2 O4 C13 O3 60.9(11) . . . . ? Ho2 O4 C13 C14 -118.0(7) . . . . ? Ho1 O3 C13 O4 3.4(13) . . . . ? Ho1 O3 C13 C14 -177.6(5) . . . . ? O4 C13 C14 C15 141.9(7) . . . . ? O3 C13 C14 C15 -37.1(9) . . . . ? O4 C13 C14 C19 -34.2(10) . . . . ? O3 C13 C14 C19 146.8(7) . . . . ? C19 C14 C15 C16 -1.8(11) . . . . ? C13 C14 C15 C16 -178.1(7) . . . . ? C14 C15 C16 C17 2.5(12) . . . . ? C15 C16 C17 C18 -1.1(10) . . . . ? C15 C16 C17 C24 180.0(6) . . . . ? C16 C17 C18 C23 -179.6(6) . . . . ? C24 C17 C18 C23 -0.8(10) . . . . ? C16 C17 C18 C19 -0.9(9) . . . . ? C24 C17 C18 C19 177.9(6) . . . . ? C23 C18 C19 C20 3.0(9) . . . . ? C17 C18 C19 C20 -175.8(6) . . . . ? C23 C18 C19 C14 -179.7(6) . . . . ? C17 C18 C19 C14 1.6(9) . . . . ? C15 C14 C19 C18 -0.2(9) . . . . ? C13 C14 C19 C18 175.8(6) . . . . ? C15 C14 C19 C20 177.0(7) . . . . ? C13 C14 C19 C20 -7.0(10) . . . . ? C18 C19 C20 C21 -1.5(10) . . . . ? C14 C19 C20 C21 -178.8(7) . . . . ? C19 C20 C21 C22 0.2(11) . . . . ? C20 C21 C22 C23 -0.5(11) . . . . ? C21 C22 C23 C18 2.1(11) . . . . ? C19 C18 C23 C22 -3.4(9) . . . . ? C17 C18 C23 C22 175.3(6) . . . . ? Ho2 O8 C24 O7 -39.5(10) 4_566 . . . ? Ho2 O8 C24 C17 141.5(5) 4_566 . . . ? Ho1 O7 C24 O8 8.6(17) 4_566 . . . ? Ho1 O7 C24 C17 -172.3(9) 4_566 . . . ? C16 C17 C24 O8 -147.2(6) . . . . ? C18 C17 C24 O8 34.0(9) . . . . ? C16 C17 C24 O7 33.6(9) . . . . ? C18 C17 C24 O7 -145.2(6) . . . . ? Ho2 O10 C25 O9 2.1(12) 3 . . . ? Ho2 O10 C25 C26 -174.2(4) 3 . . . ? Ho2 O9 C25 O10 37.2(11) . . . . ? Ho2 O9 C25 C26 -146.6(5) . . . . ? O10 C25 C26 C27 132.1(7) . . . . ? O9 C25 C26 C27 -44.5(9) . . . . ? O10 C25 C26 C31 -42.3(9) . . . . ? O9 C25 C26 C31 141.1(6) . . . . ? C31 C26 C27 C28 4.6(10) . . . . ? C25 C26 C27 C28 -169.9(6) . . . . ? C26 C27 C28 C29 1.9(11) . . . . ? C27 C28 C29 C30 -7.4(10) . . . . ? C27 C28 C29 C36 168.7(6) . . . . ? C28 C29 C30 C35 -171.0(6) . . . . ? C36 C29 C30 C35 13.0(10) . . . . ? C28 C29 C30 C31 6.5(9) . . . . ? C36 C29 C30 C31 -169.5(6) . . . . ? C35 C30 C31 C32 -0.2(9) . . . . ? C29 C30 C31 C32 -177.7(6) . . . . ? C35 C30 C31 C26 177.5(6) . . . . ? C29 C30 C31 C26 -0.1(9) . . . . ? C27 C26 C31 C30 -5.4(9) . . . . ? C25 C26 C31 C30 168.9(6) . . . . ? C27 C26 C31 C32 172.2(6) . . . . ? C25 C26 C31 C32 -13.5(10) . . . . ? C30 C31 C32 C33 1.0(10) . . . . ? C26 C31 C32 C33 -176.6(7) . . . . ? C31 C32 C33 C34 -0.8(12) . . . . ? C32 C33 C34 C35 -0.3(13) . . . . ? C33 C34 C35 C30 1.2(12) . . . . ? C31 C30 C35 C34 -1.0(10) . . . . ? C29 C30 C35 C34 176.5(7) . . . . ? Ho2 O11 C36 O12 -92.0(16) 4_566 . . . ? Ho2 O11 C36 C29 90.3(16) 4_566 . . . ? Ho2 O12 C36 O11 13.2(9) 2 . . . ? Ho2 O12 C36 C29 -169.0(4) 2 . . . ? C28 C29 C36 O11 45.7(9) . . . . ? C30 C29 C36 O11 -138.3(7) . . . . ? C28 C29 C36 O12 -132.2(7) . . . . ? C30 C29 C36 O12 43.8(9) . . . . ? C39A N1A C37A C38A 0.0(2) . . . . ? C40A N1A C37A C38A 180.0(2) . . . . ? N1A C37A C38A N2A 0.1(3) . . . . ? C39A N2A C38A C37A -0.1(3) . . . . ? C41A N2A C38A C37A 179.8(2) . . . . ? C38A N2A C39A N1A 0.1(3) . . . . ? C41A N2A C39A N1A -179.8(2) . . . . ? C37A N1A C39A N2A -0.1(3) . . . . ? C40A N1A C39A N2A 180.0(2) . . . . ? C39A N2A C41A C42A 177.2(12) . . . . ? C38A N2A C41A C42A -2.7(12) . . . . ? N2A C41A C42A C43A -81.4(18) . . . . ? C44A C43A C42A C41A 166.8(16) . . . . ? C42A C43A C44A C45A -158.0(17) . . . . ? C43A C44A C45A C46A -35(3) . . . . ? C39B N1B C37B C38B -0.1(2) . . . . ? C40B N1B C37B C38B 179.9(2) . . . . ? N1B C37B C38B N2B 0.0(3) . . . . ? C39B N2B C38B C37B 0.1(3) . . . . ? C41B N2B C38B C37B -179.9(2) . . . . ? C38B N2B C39B N1B -0.2(3) . . . . ? C41B N2B C39B N1B 179.9(2) . . . . ? C37B N1B C39B N2B 0.2(3) . . . . ? C40B N1B C39B N2B -179.9(2) . . . . ? C39B N2B C41B C42B -2.3(14) . . . . ? C38B N2B C41B C42B 177.7(14) . . . . ? N2B C41B C42B C43B 115.5(12) . . . . ? C41B C42B C43B C44B 64(3) . . . . ? C42B C43B C44B C45B 174(2) . . . . ? C43B C44B C45B C46B -149(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.54 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.779 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.158 #===END data_compound-11 _database_code_depnum_ccdc_archive 'CCDC 876531' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Er2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl Er2 N2 O12' _chemical_formula_weight 1179.75 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.6322(6) _cell_length_b 14.7719(4) _cell_length_c 15.7947(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.131(3) _cell_angle_gamma 90.00 _cell_volume 4103.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11909 _cell_measurement_theta_min 2.5651 _cell_measurement_theta_max 28.7847 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 4.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73725 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18406 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8485 _reflns_number_gt 6653 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8485 _refine_ls_number_parameters 605 _refine_ls_number_restraints 951 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.051 _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 Er1 Er 0.378632(9) 0.024556(11) -0.003879(9) 0.01206(6) Uani 1 1 d . . . Er2 Er 0.118025(9) 0.011599(11) -0.001425(9) 0.01248(6) Uani 1 1 d . . . Cl1 Cl 0.25229(6) -0.08079(7) 0.02652(7) 0.0274(2) Uani 1 1 d . . . O1 O 0.45074(17) 0.1194(2) -0.0770(2) 0.0347(8) Uani 1 1 d . . . O2 O 0.57653(17) 0.1029(2) -0.06734(19) 0.0349(8) Uani 1 1 d . . . O3 O 0.31528(17) 0.1271(2) 0.07309(19) 0.0365(8) Uani 1 1 d . . . O5 O 0.46857(18) 0.4276(2) -0.40309(19) 0.0400(9) Uani 1 1 d . . . O4 O 0.19216(16) 0.13220(19) 0.03231(18) 0.0278(7) Uani 1 1 d . . . O6 O 0.59420(18) 0.4302(2) -0.38807(18) 0.0356(8) Uani 1 1 d . . . O7 O 0.29287(16) 0.4295(2) 0.39110(17) 0.0277(7) Uani 1 1 d . . . O8 O 0.16894(15) 0.45797(19) 0.37083(15) 0.0227(6) Uani 1 1 d . . . O9 O 0.06152(17) 0.08290(19) 0.11017(17) 0.0279(7) Uani 1 1 d . . . O10 O -0.06427(16) 0.09812(19) 0.08619(17) 0.0266(7) Uani 1 1 d . . . O11 O 0.02362(16) 0.4073(2) 0.43571(17) 0.0281(7) Uani 1 1 d . . . O12 O -0.09886(17) 0.4017(2) 0.39822(18) 0.0294(7) Uani 1 1 d . . . C1 C 0.5168(2) 0.1395(3) -0.0958(3) 0.0228(9) Uani 1 1 d . . . C2 C 0.5231(2) 0.2136(3) -0.1605(2) 0.0207(9) Uani 1 1 d . . . C3 C 0.4721(2) 0.2115(3) -0.2310(3) 0.0281(10) Uani 1 1 d . . . H3A H 0.4355 0.1662 -0.2359 0.034 Uiso 1 1 calc R . . C4 C 0.4747(2) 0.2764(3) -0.2952(3) 0.0295(11) Uani 1 1 d . . . H4A H 0.4394 0.2737 -0.3419 0.035 Uiso 1 1 calc R . . C5 C 0.5282(2) 0.3440(3) -0.2907(2) 0.0214(9) Uani 1 1 d . . . C6 C 0.5801(2) 0.3524(3) -0.2169(2) 0.0199(9) Uani 1 1 d . . . C7 C 0.5777(2) 0.2853(3) -0.1517(2) 0.0213(9) Uani 1 1 d . . . C8 C 0.6288(2) 0.2928(3) -0.0788(2) 0.0292(10) Uani 1 1 d . . . H8A H 0.6295 0.2485 -0.0369 0.035 Uiso 1 1 calc R . . C9 C 0.6772(3) 0.3652(3) -0.0698(3) 0.0397(12) Uani 1 1 d . . . H9A H 0.7102 0.3697 -0.0213 0.048 Uiso 1 1 calc R . . C10 C 0.6779(3) 0.4327(3) -0.1325(3) 0.0353(12) Uani 1 1 d . . . H10A H 0.7102 0.4822 -0.1248 0.042 Uiso 1 1 calc R . . C11 C 0.6309(2) 0.4254(3) -0.2049(3) 0.0274(10) Uani 1 1 d . . . H11A H 0.6326 0.4694 -0.2469 0.033 Uiso 1 1 calc R . . C12 C 0.5306(2) 0.4059(3) -0.3656(3) 0.0243(9) Uani 1 1 d . . . C13 C 0.2490(2) 0.1595(3) 0.0773(3) 0.0238(9) Uani 1 1 d . . . C14 C 0.2396(2) 0.2312(3) 0.1423(3) 0.0225(9) Uani 1 1 d . . . C15 C 0.2831(3) 0.2230(3) 0.2176(3) 0.0336(11) Uani 1 1 d . . . H15A H 0.3168 0.1747 0.2251 0.040 Uiso 1 1 calc R . . C16 C 0.2778(3) 0.2854(3) 0.2829(3) 0.0326(11) Uani 1 1 d . . . H16A H 0.3089 0.2785 0.3326 0.039 Uiso 1 1 calc R . . C17 C 0.2278(2) 0.3573(3) 0.2759(2) 0.0192(9) Uani 1 1 d . . . C18 C 0.1806(2) 0.3677(3) 0.1989(2) 0.0166(8) Uani 1 1 d . . . C19 C 0.1877(2) 0.3057(3) 0.1312(2) 0.0197(9) Uani 1 1 d . . . C20 C 0.1444(3) 0.3213(3) 0.0530(3) 0.0303(11) Uani 1 1 d . . . H20A H 0.1494 0.2822 0.0076 0.036 Uiso 1 1 calc R . . C21 C 0.0956(3) 0.3932(3) 0.0440(3) 0.0352(12) Uani 1 1 d . . . H21A H 0.0673 0.4023 -0.0073 0.042 Uiso 1 1 calc R . . C22 C 0.0878(3) 0.4527(3) 0.1112(3) 0.0301(10) Uani 1 1 d . . . H22A H 0.0544 0.5014 0.1044 0.036 Uiso 1 1 calc R . . C23 C 0.1285(2) 0.4405(3) 0.1866(3) 0.0242(9) Uani 1 1 d . . . H23A H 0.1222 0.4806 0.2309 0.029 Uiso 1 1 calc R . . C24 C 0.2293(2) 0.4205(3) 0.3517(2) 0.0194(9) Uani 1 1 d . . . C25 C -0.0006(2) 0.1215(3) 0.1200(2) 0.0201(9) Uani 1 1 d . . . C26 C -0.0010(2) 0.1995(3) 0.1811(2) 0.0211(9) Uani 1 1 d . . . C27 C 0.0407(2) 0.1906(3) 0.2580(3) 0.0280(10) Uani 1 1 d . . . H27A H 0.0734 0.1416 0.2671 0.034 Uiso 1 1 calc R . . C28 C 0.0340(3) 0.2548(3) 0.3223(3) 0.0301(11) Uani 1 1 d . . . H28A H 0.0635 0.2487 0.3732 0.036 Uiso 1 1 calc R . . C29 C -0.0155(2) 0.3268(3) 0.3114(2) 0.0216(9) Uani 1 1 d . . . C30 C -0.0533(2) 0.3433(3) 0.2301(3) 0.0223(9) Uani 1 1 d . . . C31 C -0.0455(2) 0.2782(3) 0.1647(2) 0.0204(9) Uani 1 1 d . . . C32 C -0.0810(3) 0.2965(3) 0.0823(3) 0.0323(11) Uani 1 1 d . . . H32A H -0.0780 0.2544 0.0389 0.039 Uiso 1 1 calc R . . C33 C -0.1191(3) 0.3757(3) 0.0673(3) 0.0441(13) Uani 1 1 d . . . H33A H -0.1401 0.3880 0.0128 0.053 Uiso 1 1 calc R . . C34 C -0.1276(3) 0.4390(3) 0.1318(3) 0.0417(13) Uani 1 1 d . . . H34A H -0.1551 0.4919 0.1204 0.050 Uiso 1 1 calc R . . C35 C -0.0954(3) 0.4231(3) 0.2115(3) 0.0335(11) Uani 1 1 d . . . H35A H -0.1013 0.4653 0.2542 0.040 Uiso 1 1 calc R . . C36 C -0.0309(2) 0.3828(3) 0.3866(2) 0.0215(9) Uani 1 1 d . . . N1A N 0.2322(5) -0.2684(5) 0.2681(5) 0.0614(12) Uani 0.555(4) 1 d PDU A 1 N2A N 0.2987(5) -0.1464(6) 0.2728(5) 0.0679(12) Uani 0.555(4) 1 d PDU A 1 C37A C 0.2808(6) -0.2722(9) 0.3389(6) 0.0654(13) Uani 0.555(4) 1 d PDU A 1 H37A H 0.2848 -0.3189 0.3785 0.078 Uiso 0.555(4) 1 calc PR A 1 C38A C 0.3208(6) -0.1978(7) 0.3407(6) 0.0698(13) Uani 0.555(4) 1 d PDU A 1 H38A H 0.3586 -0.1826 0.3824 0.084 Uiso 0.555(4) 1 calc PR A 1 C39A C 0.2444(5) -0.1917(6) 0.2291(5) 0.0629(12) Uani 0.555(4) 1 d PDU A 1 H39A H 0.2189 -0.1723 0.1788 0.076 Uiso 0.555(4) 1 calc PR A 1 C40A C 0.1780(6) -0.3404(7) 0.2446(7) 0.073(2) Uani 0.555(4) 1 d PDU A 1 H40A H 0.1502 -0.3253 0.1920 0.110 Uiso 0.555(4) 1 calc PR A 1 H40B H 0.1432 -0.3471 0.2883 0.110 Uiso 0.555(4) 1 calc PR A 1 H40C H 0.2048 -0.3962 0.2382 0.110 Uiso 0.555(4) 1 calc PR A 1 C41A C 0.3276(5) -0.0562(7) 0.2487(7) 0.0751(12) Uani 0.555(4) 1 d PDU A 1 H41A H 0.2840 -0.0159 0.2451 0.090 Uiso 0.555(4) 1 calc PR A 1 H41B H 0.3434 -0.0623 0.1914 0.090 Uiso 0.555(4) 1 calc PR A 1 C43A C 0.3534(6) 0.0443(9) 0.3770(7) 0.0896(14) Uani 0.555(4) 1 d PDU A 1 H43A H 0.3175 0.0909 0.3577 0.107 Uiso 0.555(4) 1 calc PR A 1 H43B H 0.3294 0.0017 0.4135 0.107 Uiso 0.555(4) 1 calc PR A 1 C42A C 0.3922(6) -0.0050(8) 0.2996(7) 0.0795(13) Uani 0.555(4) 1 d PDU A 1 H42A H 0.4150 0.0394 0.2639 0.095 Uiso 0.555(4) 1 calc PR A 1 H42B H 0.4314 -0.0468 0.3211 0.095 Uiso 0.555(4) 1 calc PR A 1 C44A C 0.4311(7) 0.0851(9) 0.4205(7) 0.0955(16) Uani 0.555(4) 1 d PDU A 1 H44A H 0.4715 0.0421 0.4126 0.115 Uiso 0.555(4) 1 calc PR A 1 H44B H 0.4429 0.1400 0.3905 0.115 Uiso 0.555(4) 1 calc PR A 1 C45A C 0.4314(7) 0.1075(10) 0.5166(7) 0.1008(19) Uani 0.555(4) 1 d PDU A 1 H45A H 0.4730 0.1481 0.5336 0.121 Uiso 0.555(4) 1 calc PR A 1 H45B H 0.4367 0.0528 0.5504 0.121 Uiso 0.555(4) 1 calc PR A 1 C46A C 0.3533(7) 0.1540(10) 0.5280(9) 0.121(3) Uani 0.555(4) 1 d PDU A 1 H46A H 0.3518 0.1744 0.5856 0.182 Uiso 0.555(4) 1 calc PR A 1 H46B H 0.3130 0.1113 0.5152 0.182 Uiso 0.555(4) 1 calc PR A 1 H46C H 0.3472 0.2048 0.4902 0.182 Uiso 0.555(4) 1 calc PR A 1 N1B N 0.2079(5) -0.2815(6) 0.2272(7) 0.0614(12) Uani 0.445(4) 1 d PDU A 2 N2B N 0.2908(5) -0.2062(7) 0.2969(7) 0.0679(12) Uani 0.445(4) 1 d PDU A 2 C37B C 0.2161(7) -0.3221(8) 0.3048(6) 0.0654(13) Uani 0.445(4) 1 d PDU A 2 H37B H 0.1907 -0.3726 0.3236 0.078 Uiso 0.445(4) 1 calc PR A 2 C38B C 0.2682(8) -0.2733(9) 0.3465(9) 0.0698(13) Uani 0.445(4) 1 d PDU A 2 H38B H 0.2868 -0.2835 0.4023 0.084 Uiso 0.445(4) 1 calc PR A 2 C39B C 0.2537(5) -0.2109(7) 0.2234(7) 0.0629(12) Uani 0.445(4) 1 d PDU A 2 H39B H 0.2582 -0.1725 0.1774 0.076 Uiso 0.445(4) 1 calc PR A 2 C40B C 0.1544(7) -0.3146(9) 0.1589(7) 0.073(2) Uani 0.445(4) 1 d PDU A 2 H40D H 0.1567 -0.2764 0.1100 0.110 Uiso 0.445(4) 1 calc PR A 2 H40E H 0.1038 -0.3138 0.1776 0.110 Uiso 0.445(4) 1 calc PR A 2 H40F H 0.1676 -0.3755 0.1444 0.110 Uiso 0.445(4) 1 calc PR A 2 C41B C 0.3488(7) -0.1425(8) 0.3289(8) 0.0751(12) Uani 0.445(4) 1 d PDU A 2 H41C H 0.3960 -0.1735 0.3456 0.090 Uiso 0.445(4) 1 calc PR A 2 H41D H 0.3323 -0.1093 0.3773 0.090 Uiso 0.445(4) 1 calc PR A 2 C42B C 0.3584(10) -0.0798(8) 0.2544(8) 0.0795(13) Uani 0.445(4) 1 d PDU A 2 H42C H 0.4102 -0.0757 0.2378 0.095 Uiso 0.445(4) 1 calc PR A 2 H42D H 0.3228 -0.0909 0.2058 0.095 Uiso 0.445(4) 1 calc PR A 2 C43B C 0.3358(9) -0.0039(10) 0.3102(9) 0.0896(14) Uani 0.445(4) 1 d PDU A 2 H43C H 0.2887 -0.0211 0.3341 0.107 Uiso 0.445(4) 1 calc PR A 2 H43D H 0.3248 0.0485 0.2743 0.107 Uiso 0.445(4) 1 calc PR A 2 C44B C 0.3937(9) 0.0265(11) 0.3856(10) 0.0955(16) Uani 0.445(4) 1 d PDU A 2 H44C H 0.4067 -0.0246 0.4224 0.115 Uiso 0.445(4) 1 calc PR A 2 H44D H 0.4400 0.0493 0.3636 0.115 Uiso 0.445(4) 1 calc PR A 2 C45B C 0.3551(8) 0.1023(10) 0.4362(10) 0.1008(19) Uani 0.445(4) 1 d PDU A 2 H45C H 0.3296 0.1446 0.3967 0.121 Uiso 0.445(4) 1 calc PR A 2 H45D H 0.3170 0.0754 0.4698 0.121 Uiso 0.445(4) 1 calc PR A 2 C46B C 0.4126(11) 0.1525(11) 0.4939(11) 0.121(3) Uani 0.445(4) 1 d PDU A 2 H46D H 0.4515 0.1768 0.4610 0.182 Uiso 0.445(4) 1 calc PR A 2 H46E H 0.4350 0.1116 0.5358 0.182 Uiso 0.445(4) 1 calc PR A 2 H46F H 0.3878 0.2009 0.5215 0.182 Uiso 0.445(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01122(10) 0.01258(9) 0.01224(10) -0.00054(6) -0.00010(7) 0.00067(6) Er2 0.01199(10) 0.01289(9) 0.01243(10) 0.00006(7) -0.00014(7) -0.00068(7) Cl1 0.0149(5) 0.0244(5) 0.0429(6) 0.0131(5) 0.0016(5) 0.0015(4) O1 0.0203(17) 0.0378(18) 0.0461(19) 0.0218(16) 0.0015(14) -0.0059(15) O2 0.0197(17) 0.0333(18) 0.051(2) 0.0237(16) -0.0037(15) 0.0016(14) O3 0.0240(18) 0.0373(18) 0.048(2) -0.0249(16) -0.0023(15) 0.0058(15) O5 0.033(2) 0.046(2) 0.0382(19) 0.0214(16) -0.0172(15) -0.0048(16) O4 0.0194(16) 0.0259(15) 0.0376(17) -0.0135(14) -0.0007(13) -0.0044(13) O6 0.0312(19) 0.0428(19) 0.0326(17) 0.0206(15) 0.0009(14) -0.0084(16) O7 0.0171(16) 0.0402(18) 0.0248(15) -0.0139(14) -0.0043(12) -0.0005(14) O8 0.0182(15) 0.0336(16) 0.0162(13) -0.0040(13) 0.0013(11) 0.0090(13) O9 0.0283(18) 0.0316(17) 0.0239(15) -0.0112(13) 0.0031(13) 0.0013(14) O10 0.0203(16) 0.0287(16) 0.0312(16) -0.0136(14) 0.0053(13) -0.0065(13) O11 0.0259(17) 0.0343(17) 0.0237(15) -0.0100(14) -0.0015(13) -0.0100(14) O12 0.0227(18) 0.0311(17) 0.0352(17) -0.0136(14) 0.0080(14) -0.0057(14) C1 0.018(2) 0.021(2) 0.029(2) 0.0108(18) 0.0003(18) -0.0030(18) C2 0.015(2) 0.022(2) 0.025(2) 0.0111(18) 0.0016(17) 0.0003(17) C3 0.014(2) 0.031(2) 0.038(3) 0.014(2) -0.0061(19) -0.0086(19) C4 0.023(3) 0.034(2) 0.030(2) 0.014(2) -0.0101(19) -0.005(2) C5 0.016(2) 0.026(2) 0.022(2) 0.0095(18) 0.0003(17) 0.0005(18) C6 0.016(2) 0.019(2) 0.024(2) 0.0043(17) -0.0028(17) 0.0005(17) C7 0.016(2) 0.026(2) 0.022(2) 0.0079(18) -0.0011(17) -0.0015(17) C8 0.032(3) 0.033(2) 0.022(2) 0.0083(19) -0.0080(19) -0.005(2) C9 0.037(3) 0.052(3) 0.029(2) 0.003(2) -0.011(2) -0.011(3) C10 0.035(3) 0.037(3) 0.033(2) -0.001(2) -0.002(2) -0.019(2) C11 0.028(3) 0.026(2) 0.029(2) 0.0079(19) 0.0035(19) -0.0056(19) C12 0.025(2) 0.025(2) 0.022(2) 0.0086(18) -0.0031(18) -0.0041(19) C13 0.021(2) 0.021(2) 0.029(2) -0.0103(18) 0.0016(18) -0.0042(18) C14 0.015(2) 0.025(2) 0.027(2) -0.0103(18) -0.0003(17) 0.0005(18) C15 0.028(3) 0.028(2) 0.042(3) -0.014(2) -0.011(2) 0.015(2) C16 0.031(3) 0.038(3) 0.026(2) -0.009(2) -0.012(2) 0.015(2) C17 0.015(2) 0.023(2) 0.020(2) -0.0056(17) 0.0019(16) 0.0012(17) C18 0.013(2) 0.021(2) 0.0165(19) -0.0013(16) 0.0023(15) -0.0013(16) C19 0.013(2) 0.023(2) 0.023(2) -0.0082(17) -0.0007(16) -0.0006(17) C20 0.039(3) 0.029(2) 0.021(2) -0.0083(19) -0.005(2) 0.003(2) C21 0.044(3) 0.042(3) 0.018(2) 0.003(2) -0.012(2) 0.009(2) C22 0.034(3) 0.023(2) 0.032(2) 0.003(2) -0.007(2) 0.016(2) C23 0.025(2) 0.021(2) 0.027(2) -0.0074(18) -0.0007(18) 0.0048(18) C24 0.019(2) 0.021(2) 0.0183(19) -0.0006(17) 0.0000(16) -0.0018(17) C25 0.023(2) 0.021(2) 0.0172(19) -0.0043(17) 0.0061(17) -0.0059(18) C26 0.021(2) 0.023(2) 0.020(2) -0.0073(18) 0.0054(17) -0.0046(18) C27 0.026(3) 0.027(2) 0.030(2) -0.0106(19) -0.0055(19) 0.012(2) C28 0.030(3) 0.039(3) 0.020(2) -0.009(2) -0.0077(19) 0.009(2) C29 0.018(2) 0.023(2) 0.024(2) -0.0105(18) 0.0033(17) -0.0025(18) C30 0.023(2) 0.021(2) 0.023(2) -0.0059(18) 0.0024(18) -0.0053(18) C31 0.021(2) 0.020(2) 0.021(2) -0.0028(17) 0.0031(17) -0.0043(18) C32 0.037(3) 0.033(3) 0.026(2) -0.003(2) -0.007(2) -0.005(2) C33 0.046(3) 0.046(3) 0.038(3) 0.009(3) -0.012(2) -0.001(3) C34 0.042(3) 0.037(3) 0.046(3) 0.008(2) 0.002(2) 0.007(2) C35 0.038(3) 0.027(2) 0.035(3) -0.005(2) 0.002(2) 0.001(2) C36 0.022(2) 0.020(2) 0.023(2) -0.0068(17) 0.0048(18) -0.0065(18) N1A 0.069(3) 0.053(2) 0.065(3) 0.009(2) 0.021(2) 0.019(2) N2A 0.078(3) 0.061(2) 0.067(2) 0.006(2) 0.017(2) 0.017(2) C37A 0.075(3) 0.060(2) 0.063(3) 0.011(2) 0.020(2) 0.022(2) C38A 0.079(3) 0.064(2) 0.068(2) 0.006(2) 0.016(2) 0.021(2) C39A 0.072(3) 0.058(2) 0.061(2) 0.008(2) 0.018(2) 0.020(2) C40A 0.072(4) 0.065(4) 0.084(4) -0.004(4) 0.018(4) 0.015(4) C41A 0.082(3) 0.067(2) 0.078(2) 0.005(2) 0.019(2) 0.019(2) C43A 0.098(3) 0.081(3) 0.090(3) 0.006(2) 0.011(3) 0.018(3) C42A 0.086(3) 0.073(3) 0.081(3) 0.006(2) 0.019(2) 0.018(2) C44A 0.102(3) 0.086(3) 0.100(3) 0.004(3) 0.012(3) 0.011(3) C45A 0.109(4) 0.088(3) 0.106(3) 0.012(3) 0.011(3) 0.018(3) C46A 0.130(6) 0.098(5) 0.137(6) 0.006(5) 0.021(6) 0.008(6) N1B 0.069(3) 0.053(2) 0.065(3) 0.009(2) 0.021(2) 0.019(2) N2B 0.078(3) 0.061(2) 0.067(2) 0.006(2) 0.017(2) 0.017(2) C37B 0.075(3) 0.060(2) 0.063(3) 0.011(2) 0.020(2) 0.022(2) C38B 0.079(3) 0.064(2) 0.068(2) 0.006(2) 0.016(2) 0.021(2) C39B 0.072(3) 0.058(2) 0.061(2) 0.008(2) 0.018(2) 0.020(2) C40B 0.072(4) 0.065(4) 0.084(4) -0.004(4) 0.018(4) 0.015(4) C41B 0.082(3) 0.067(2) 0.078(2) 0.005(2) 0.019(2) 0.019(2) C42B 0.086(3) 0.073(3) 0.081(3) 0.006(2) 0.019(2) 0.018(2) C43B 0.098(3) 0.081(3) 0.090(3) 0.006(2) 0.011(3) 0.018(3) C44B 0.102(3) 0.086(3) 0.100(3) 0.004(3) 0.012(3) 0.011(3) C45B 0.109(4) 0.088(3) 0.106(3) 0.012(3) 0.011(3) 0.018(3) C46B 0.130(6) 0.098(5) 0.137(6) 0.006(5) 0.021(6) 0.008(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.264(3) . ? Er1 O7 2.267(3) 4_565 ? Er1 O5 2.277(3) 4_566 ? Er1 O6 2.281(3) 2_644 ? Er1 O3 2.284(3) . ? Er1 O2 2.303(3) 3_655 ? Er1 Cl1 2.7872(10) . ? Er2 O11 2.226(3) 4_565 ? Er2 O4 2.251(3) . ? Er2 O10 2.266(3) 3 ? Er2 O8 2.311(2) 4_565 ? Er2 O9 2.337(3) . ? Er2 O12 2.343(3) 2_545 ? Er2 Cl1 2.7407(10) . ? O1 C1 1.258(5) . ? O2 C1 1.239(5) . ? O2 Er1 2.303(3) 3_655 ? O3 C13 1.268(5) . ? O5 C12 1.247(5) . ? O5 Er1 2.277(3) 4_565 ? O4 C13 1.253(5) . ? O6 C12 1.253(5) . ? O6 Er1 2.281(3) 2_654 ? O7 C24 1.250(4) . ? O7 Er1 2.267(3) 4_566 ? O8 C24 1.255(4) . ? O8 Er2 2.311(2) 4_566 ? O9 C25 1.254(5) . ? O10 C25 1.256(5) . ? O10 Er2 2.266(3) 3 ? O11 C36 1.245(5) . ? O11 Er2 2.226(3) 4_566 ? O12 C36 1.256(5) . ? O12 Er2 2.343(3) 2 ? C1 C2 1.506(5) . ? C2 C3 1.380(5) . ? C2 C7 1.431(5) . ? C3 C4 1.399(5) . ? C3 H3A 0.9300 . ? C4 C5 1.373(6) . ? C4 H4A 0.9300 . ? C5 C6 1.435(5) . ? C5 C12 1.498(5) . ? C6 C11 1.406(5) . ? C6 C7 1.431(5) . ? C7 C8 1.415(5) . ? C8 C9 1.369(6) . ? C8 H8A 0.9300 . ? C9 C10 1.407(6) . ? C9 H9A 0.9300 . ? C10 C11 1.367(6) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.492(5) . ? C14 C15 1.373(5) . ? C14 C19 1.434(5) . ? C15 C16 1.392(6) . ? C15 H15A 0.9300 . ? C16 C17 1.380(5) . ? C16 H16A 0.9300 . ? C17 C18 1.432(5) . ? C17 C24 1.516(5) . ? C18 C23 1.419(5) . ? C18 C19 1.420(5) . ? C19 C20 1.422(5) . ? C20 C21 1.368(6) . ? C20 H20A 0.9300 . ? C21 C22 1.393(6) . ? C21 H21A 0.9300 . ? C22 C23 1.357(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.505(5) . ? C26 C27 1.379(5) . ? C26 C31 1.417(6) . ? C27 C28 1.401(5) . ? C27 H27A 0.9300 . ? C28 C29 1.380(6) . ? C28 H28A 0.9300 . ? C29 C30 1.424(5) . ? C29 C36 1.488(5) . ? C30 C35 1.413(6) . ? C30 C31 1.425(5) . ? C31 C32 1.428(5) . ? C32 C33 1.361(6) . ? C32 H32A 0.9300 . ? C33 C34 1.399(7) . ? C33 H33A 0.9300 . ? C34 C35 1.363(6) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? N1A C39A 1.315(8) . ? N1A C37A 1.361(8) . ? N1A C40A 1.460(11) . ? N2A C39A 1.320(10) . ? N2A C38A 1.349(8) . ? N2A C41A 1.486(11) . ? C37A C38A 1.305(16) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.545(9) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C44A 1.604(9) . ? C43A C42A 1.617(9) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.554(9) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.560(9) . ? C45A H45A 0.9700 . ? C45A H45B 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N1B C39B 1.323(9) . ? N1B C37B 1.362(9) . ? N1B C40B 1.465(12) . ? N2B C39B 1.292(10) . ? N2B C38B 1.342(9) . ? N2B C41B 1.453(12) . ? C37B C38B 1.308(17) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C39B H39B 0.9300 . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C41B C42B 1.517(9) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.496(9) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C43B C44B 1.577(9) . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C44B C45B 1.561(9) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C45B C46B 1.508(10) . ? C45B H45C 0.9700 . ? C45B H45D 0.9700 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? C46B H46F 0.9600 . ? 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 Er1 O7 79.10(10) . 4_565 ? O1 Er1 O5 77.06(12) . 4_566 ? O7 Er1 O5 144.39(12) 4_565 4_566 ? O1 Er1 O6 80.83(12) . 2_644 ? O7 Er1 O6 78.49(11) 4_565 2_644 ? O5 Er1 O6 122.65(11) 4_566 2_644 ? O1 Er1 O3 100.08(12) . . ? O7 Er1 O3 82.23(11) 4_565 . ? O5 Er1 O3 76.38(11) 4_566 . ? O6 Er1 O3 160.17(11) 2_644 . ? O1 Er1 O2 124.71(11) . 3_655 ? O7 Er1 O2 142.14(11) 4_565 3_655 ? O5 Er1 O2 73.44(11) 4_566 3_655 ? O6 Er1 O2 77.46(11) 2_644 3_655 ? O3 Er1 O2 116.49(12) . 3_655 ? O1 Er1 Cl1 156.72(8) . . ? O7 Er1 Cl1 78.10(7) 4_565 . ? O5 Er1 Cl1 125.30(9) 4_566 . ? O6 Er1 Cl1 90.07(9) 2_644 . ? O3 Er1 Cl1 81.44(8) . . ? O2 Er1 Cl1 73.15(8) 3_655 . ? O11 Er2 O4 94.75(11) 4_565 . ? O11 Er2 O10 81.58(11) 4_565 3 ? O4 Er2 O10 156.50(10) . 3 ? O11 Er2 O8 80.26(10) 4_565 4_565 ? O4 Er2 O8 78.30(10) . 4_565 ? O10 Er2 O8 78.20(10) 3 4_565 ? O11 Er2 O9 75.42(10) 4_565 . ? O4 Er2 O9 74.73(10) . . ? O10 Er2 O9 125.81(10) 3 . ? O8 Er2 O9 141.66(10) 4_565 . ? O11 Er2 O12 122.87(10) 4_565 2_545 ? O4 Er2 O12 119.63(10) . 2_545 ? O10 Er2 O12 80.80(10) 3 2_545 ? O8 Er2 O12 145.79(10) 4_565 2_545 ? O9 Er2 O12 72.36(10) . 2_545 ? O11 Er2 Cl1 161.70(7) 4_565 . ? O4 Er2 Cl1 82.86(8) . . ? O10 Er2 Cl1 93.36(8) 3 . ? O8 Er2 Cl1 81.49(7) 4_565 . ? O9 Er2 Cl1 120.88(7) . . ? O12 Er2 Cl1 73.08(7) 2_545 . ? Er2 Cl1 Er1 112.71(3) . . ? C1 O1 Er1 146.1(3) . . ? C1 O2 Er1 141.9(3) . 3_655 ? C13 O3 Er1 140.0(3) . . ? C12 O5 Er1 162.6(3) . 4_565 ? C13 O4 Er2 144.7(3) . . ? C12 O6 Er1 128.8(3) . 2_654 ? C24 O7 Er1 157.5(3) . 4_566 ? C24 O8 Er2 133.3(2) . 4_566 ? C25 O9 Er2 136.2(3) . . ? C25 O10 Er2 140.4(3) . 3 ? C36 O11 Er2 162.5(3) . 4_566 ? C36 O12 Er2 116.3(2) . 2 ? O2 C1 O1 126.1(4) . . ? O2 C1 C2 117.5(4) . . ? O1 C1 C2 116.4(4) . . ? C3 C2 C7 119.2(4) . . ? C3 C2 C1 117.1(4) . . ? C7 C2 C1 123.6(4) . . ? C2 C3 C4 121.1(4) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 121.3(4) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 120.0(4) . . ? C4 C5 C12 117.5(4) . . ? C6 C5 C12 122.5(4) . . ? C11 C6 C7 119.1(4) . . ? C11 C6 C5 122.5(4) . . ? C7 C6 C5 118.3(4) . . ? C8 C7 C6 118.7(4) . . ? C8 C7 C2 121.4(4) . . ? C6 C7 C2 119.9(4) . . ? C9 C8 C7 120.1(4) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C10 121.1(4) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C11 C10 C9 119.9(4) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C6 120.9(4) . . ? C10 C11 H11A 119.5 . . ? C6 C11 H11A 119.5 . . ? O5 C12 O6 124.4(4) . . ? O5 C12 C5 117.3(4) . . ? O6 C12 C5 118.3(4) . . ? O4 C13 O3 123.4(4) . . ? O4 C13 C14 119.6(4) . . ? O3 C13 C14 116.9(4) . . ? C15 C14 C19 119.1(4) . . ? C15 C14 C13 116.7(4) . . ? C19 C14 C13 124.2(4) . . ? C14 C15 C16 121.3(4) . . ? C14 C15 H15A 119.3 . . ? C16 C15 H15A 119.3 . . ? C17 C16 C15 121.8(4) . . ? C17 C16 H16A 119.1 . . ? C15 C16 H16A 119.1 . . ? C16 C17 C18 118.6(4) . . ? C16 C17 C24 115.8(3) . . ? C18 C17 C24 125.5(3) . . ? C23 C18 C19 118.5(3) . . ? C23 C18 C17 121.9(3) . . ? C19 C18 C17 119.6(3) . . ? C18 C19 C20 118.6(4) . . ? C18 C19 C14 119.5(3) . . ? C20 C19 C14 121.9(4) . . ? C21 C20 C19 120.7(4) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 120.4(4) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C23 C22 C21 120.7(4) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C18 121.1(4) . . ? C22 C23 H23A 119.4 . . ? C18 C23 H23A 119.4 . . ? O7 C24 O8 125.4(4) . . ? O7 C24 C17 115.0(3) . . ? O8 C24 C17 119.6(3) . . ? O9 C25 O10 125.8(4) . . ? O9 C25 C26 118.1(4) . . ? O10 C25 C26 116.0(4) . . ? C27 C26 C31 119.6(4) . . ? C27 C26 C25 117.7(4) . . ? C31 C26 C25 122.6(4) . . ? C26 C27 C28 120.4(4) . . ? C26 C27 H27A 119.8 . . ? C28 C27 H27A 119.8 . . ? C29 C28 C27 121.1(4) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C28 C29 C30 119.7(4) . . ? C28 C29 C36 118.6(4) . . ? C30 C29 C36 121.6(4) . . ? C35 C30 C29 122.3(4) . . ? C35 C30 C31 119.3(4) . . ? C29 C30 C31 118.4(4) . . ? C26 C31 C30 120.1(4) . . ? C26 C31 C32 121.6(4) . . ? C30 C31 C32 118.3(4) . . ? C33 C32 C31 120.0(4) . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 C34 121.7(4) . . ? C32 C33 H33A 119.2 . . ? C34 C33 H33A 119.2 . . ? C35 C34 C33 119.9(5) . . ? C35 C34 H34A 120.1 . . ? C33 C34 H34A 120.1 . . ? C34 C35 C30 120.9(4) . . ? C34 C35 H35A 119.6 . . ? C30 C35 H35A 119.6 . . ? O11 C36 O12 123.1(4) . . ? O11 C36 C29 118.8(4) . . ? O12 C36 C29 118.1(4) . . ? C39A N1A C37A 107.7(11) . . ? C39A N1A C40A 129.5(10) . . ? C37A N1A C40A 122.8(8) . . ? C39A N2A C38A 106.7(9) . . ? C39A N2A C41A 124.7(8) . . ? C38A N2A C41A 128.6(10) . . ? C38A C37A N1A 106.9(12) . . ? C38A C37A H37A 126.6 . . ? N1A C37A H37A 126.6 . . ? C37A C38A N2A 109.4(12) . . ? C37A C38A H38A 125.3 . . ? N2A C38A H38A 125.3 . . ? N1A C39A N2A 109.3(8) . . ? N1A C39A H39A 125.4 . . ? N2A C39A H39A 125.4 . . ? N1A C40A H40A 109.5 . . ? N1A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? N1A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? N2A C41A C42A 124.0(10) . . ? N2A C41A H41A 106.3 . . ? C42A C41A H41A 106.3 . . ? N2A C41A H41B 106.3 . . ? C42A C41A H41B 106.3 . . ? H41A C41A H41B 106.4 . . ? C44A C43A C42A 95.6(7) . . ? C44A C43A H43A 112.6 . . ? C42A C43A H43A 112.6 . . ? C44A C43A H43B 112.6 . . ? C42A C43A H43B 112.6 . . ? H43A C43A H43B 110.1 . . ? C41A C42A C43A 106.1(9) . . ? C41A C42A H42A 110.5 . . ? C43A C42A H42A 110.5 . . ? C41A C42A H42B 110.5 . . ? C43A C42A H42B 110.5 . . ? H42A C42A H42B 108.7 . . ? C45A C44A C43A 116.2(9) . . ? C45A C44A H44A 108.2 . . ? C43A C44A H44A 108.2 . . ? C45A C44A H44B 108.2 . . ? C43A C44A H44B 108.2 . . ? H44A C44A H44B 107.4 . . ? C44A C45A C46A 105.4(8) . . ? C44A C45A H45A 110.7 . . ? C46A C45A H45A 110.7 . . ? C44A C45A H45B 110.7 . . ? C46A C45A H45B 110.7 . . ? H45A C45A H45B 108.8 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C39B N1B C37B 111.2(12) . . ? C39B N1B C40B 126.3(11) . . ? C37B N1B C40B 122.4(9) . . ? C39B N2B C38B 109.4(10) . . ? C39B N2B C41B 130.2(10) . . ? C38B N2B C41B 120.4(10) . . ? C38B C37B N1B 103.6(13) . . ? C38B C37B H37B 128.2 . . ? N1B C37B H37B 128.2 . . ? C37B C38B N2B 109.9(13) . . ? C37B C38B H38B 125.0 . . ? N2B C38B H38B 125.0 . . ? N2B C39B N1B 105.8(10) . . ? N2B C39B H39B 127.1 . . ? N1B C39B H39B 127.1 . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N2B C41B C42B 103.9(10) . . ? N2B C41B H41C 111.0 . . ? C42B C41B H41C 111.0 . . ? N2B C41B H41D 111.0 . . ? C42B C41B H41D 111.0 . . ? H41C C41B H41D 109.0 . . ? C43B C42B C41B 87.3(10) . . ? C43B C42B H42C 114.1 . . ? C41B C42B H42C 114.1 . . ? C43B C42B H42D 114.1 . . ? C41B C42B H42D 114.1 . . ? H42C C42B H42D 111.3 . . ? C42B C43B C44B 118.2(11) . . ? C42B C43B H43C 107.8 . . ? C44B C43B H43C 107.8 . . ? C42B C43B H43D 107.8 . . ? C44B C43B H43D 107.8 . . ? H43C C43B H43D 107.1 . . ? C45B C44B C43B 108.0(10) . . ? C45B C44B H44C 110.1 . . ? C43B C44B H44C 110.1 . . ? C45B C44B H44D 110.1 . . ? C43B C44B H44D 110.1 . . ? H44C C44B H44D 108.4 . . ? C46B C45B C44B 111.3(10) . . ? C46B C45B H45C 109.4 . . ? C44B C45B H45C 109.4 . . ? C46B C45B H45D 109.4 . . ? C44B C45B H45D 109.4 . . ? H45C C45B H45D 108.0 . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C45B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Er2 Cl1 Er1 55.9(3) 4_565 . . . ? O4 Er2 Cl1 Er1 -27.63(8) . . . . ? O10 Er2 Cl1 Er1 129.07(8) 3 . . . ? O8 Er2 Cl1 Er1 51.54(7) 4_565 . . . ? O9 Er2 Cl1 Er1 -95.04(9) . . . . ? O12 Er2 Cl1 Er1 -151.61(9) 2_545 . . . ? O1 Er1 Cl1 Er2 -49.9(2) . . . . ? O7 Er1 Cl1 Er2 -38.10(8) 4_565 . . . ? O5 Er1 Cl1 Er2 112.23(10) 4_566 . . . ? O6 Er1 Cl1 Er2 -116.31(9) 2_644 . . . ? O3 Er1 Cl1 Er2 45.70(9) . . . . ? O2 Er1 Cl1 Er2 166.82(10) 3_655 . . . ? O7 Er1 O1 C1 -154.4(5) 4_565 . . . ? O5 Er1 O1 C1 52.3(5) 4_566 . . . ? O6 Er1 O1 C1 -74.4(5) 2_644 . . . ? O3 Er1 O1 C1 125.7(5) . . . . ? O2 Er1 O1 C1 -6.7(6) 3_655 . . . ? Cl1 Er1 O1 C1 -142.6(4) . . . . ? O1 Er1 O3 C13 109.6(5) . . . . ? O7 Er1 O3 C13 32.2(5) 4_565 . . . ? O5 Er1 O3 C13 -176.5(5) 4_566 . . . ? O6 Er1 O3 C13 18.7(7) 2_644 . . . ? O2 Er1 O3 C13 -113.1(5) 3_655 . . . ? Cl1 Er1 O3 C13 -46.9(5) . . . . ? O11 Er2 O4 C13 164.4(5) 4_565 . . . ? O10 Er2 O4 C13 -115.8(5) 3 . . . ? O8 Er2 O4 C13 -116.5(5) 4_565 . . . ? O9 Er2 O4 C13 91.0(5) . . . . ? O12 Er2 O4 C13 32.1(5) 2_545 . . . ? Cl1 Er2 O4 C13 -33.8(5) . . . . ? O11 Er2 O9 C25 17.4(4) 4_565 . . . ? O4 Er2 O9 C25 116.6(4) . . . . ? O10 Er2 O9 C25 -50.6(4) 3 . . . ? O8 Er2 O9 C25 69.7(4) 4_565 . . . ? O12 Er2 O9 C25 -114.8(4) 2_545 . . . ? Cl1 Er2 O9 C25 -171.7(3) . . . . ? Er1 O2 C1 O1 15.8(8) 3_655 . . . ? Er1 O2 C1 C2 -162.6(3) 3_655 . . . ? Er1 O1 C1 O2 -4.2(9) . . . . ? Er1 O1 C1 C2 174.3(3) . . . . ? O2 C1 C2 C3 135.1(4) . . . . ? O1 C1 C2 C3 -43.5(6) . . . . ? O2 C1 C2 C7 -45.8(6) . . . . ? O1 C1 C2 C7 135.6(4) . . . . ? C7 C2 C3 C4 2.2(7) . . . . ? C1 C2 C3 C4 -178.6(4) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? C3 C4 C5 C6 -3.7(7) . . . . ? C3 C4 C5 C12 175.2(4) . . . . ? C4 C5 C6 C11 -173.4(4) . . . . ? C12 C5 C6 C11 7.7(6) . . . . ? C4 C5 C6 C7 4.2(6) . . . . ? C12 C5 C6 C7 -174.7(4) . . . . ? C11 C6 C7 C8 -2.5(6) . . . . ? C5 C6 C7 C8 179.8(4) . . . . ? C11 C6 C7 C2 176.1(4) . . . . ? C5 C6 C7 C2 -1.6(6) . . . . ? C3 C2 C7 C8 177.0(4) . . . . ? C1 C2 C7 C8 -2.1(7) . . . . ? C3 C2 C7 C6 -1.6(6) . . . . ? C1 C2 C7 C6 179.3(4) . . . . ? C6 C7 C8 C9 2.7(7) . . . . ? C2 C7 C8 C9 -176.0(4) . . . . ? C7 C8 C9 C10 -0.6(7) . . . . ? C8 C9 C10 C11 -1.6(8) . . . . ? C9 C10 C11 C6 1.8(7) . . . . ? C7 C6 C11 C10 0.3(7) . . . . ? C5 C6 C11 C10 177.9(4) . . . . ? Er1 O5 C12 O6 19.6(14) 4_565 . . . ? Er1 O5 C12 C5 -158.1(8) 4_565 . . . ? Er1 O6 C12 O5 3.4(7) 2_654 . . . ? Er1 O6 C12 C5 -178.9(3) 2_654 . . . ? C4 C5 C12 O5 37.5(6) . . . . ? C6 C5 C12 O5 -143.6(4) . . . . ? C4 C5 C12 O6 -140.3(4) . . . . ? C6 C5 C12 O6 38.6(6) . . . . ? Er2 O4 C13 O3 60.2(7) . . . . ? Er2 O4 C13 C14 -117.2(4) . . . . ? Er1 O3 C13 O4 4.3(8) . . . . ? Er1 O3 C13 C14 -178.2(3) . . . . ? O4 C13 C14 C15 142.3(4) . . . . ? O3 C13 C14 C15 -35.3(6) . . . . ? O4 C13 C14 C19 -36.5(6) . . . . ? O3 C13 C14 C19 145.9(4) . . . . ? C19 C14 C15 C16 -0.1(7) . . . . ? C13 C14 C15 C16 -179.0(4) . . . . ? C14 C15 C16 C17 1.3(8) . . . . ? C15 C16 C17 C18 -0.5(7) . . . . ? C15 C16 C17 C24 -179.1(4) . . . . ? C16 C17 C18 C23 -179.2(4) . . . . ? C24 C17 C18 C23 -0.8(6) . . . . ? C16 C17 C18 C19 -1.5(6) . . . . ? C24 C17 C18 C19 176.9(4) . . . . ? C23 C18 C19 C20 2.4(6) . . . . ? C17 C18 C19 C20 -175.4(4) . . . . ? C23 C18 C19 C14 -179.6(4) . . . . ? C17 C18 C19 C14 2.7(6) . . . . ? C15 C14 C19 C18 -1.9(6) . . . . ? C13 C14 C19 C18 176.9(4) . . . . ? C15 C14 C19 C20 176.1(4) . . . . ? C13 C14 C19 C20 -5.1(7) . . . . ? C18 C19 C20 C21 -1.7(7) . . . . ? C14 C19 C20 C21 -179.7(4) . . . . ? C19 C20 C21 C22 0.5(7) . . . . ? C20 C21 C22 C23 0.0(8) . . . . ? C21 C22 C23 C18 0.8(7) . . . . ? C19 C18 C23 C22 -2.0(6) . . . . ? C17 C18 C23 C22 175.7(4) . . . . ? Er1 O7 C24 O8 6.4(10) 4_566 . . . ? Er1 O7 C24 C17 -172.6(5) 4_566 . . . ? Er2 O8 C24 O7 -39.1(6) 4_566 . . . ? Er2 O8 C24 C17 139.9(3) 4_566 . . . ? C16 C17 C24 O7 32.5(5) . . . . ? C18 C17 C24 O7 -146.0(4) . . . . ? C16 C17 C24 O8 -146.5(4) . . . . ? C18 C17 C24 O8 35.0(6) . . . . ? Er2 O9 C25 O10 36.8(6) . . . . ? Er2 O9 C25 C26 -146.8(3) . . . . ? Er2 O10 C25 O9 3.3(7) 3 . . . ? Er2 O10 C25 C26 -173.1(3) 3 . . . ? O9 C25 C26 C27 -43.2(5) . . . . ? O10 C25 C26 C27 133.4(4) . . . . ? O9 C25 C26 C31 140.5(4) . . . . ? O10 C25 C26 C31 -42.8(6) . . . . ? C31 C26 C27 C28 5.6(7) . . . . ? C25 C26 C27 C28 -170.7(4) . . . . ? C26 C27 C28 C29 1.7(7) . . . . ? C27 C28 C29 C30 -8.3(7) . . . . ? C27 C28 C29 C36 168.8(4) . . . . ? C28 C29 C30 C35 -170.2(4) . . . . ? C36 C29 C30 C35 12.9(7) . . . . ? C28 C29 C30 C31 7.3(6) . . . . ? C36 C29 C30 C31 -169.6(4) . . . . ? C27 C26 C31 C30 -6.4(6) . . . . ? C25 C26 C31 C30 169.8(4) . . . . ? C27 C26 C31 C32 171.1(4) . . . . ? C25 C26 C31 C32 -12.7(6) . . . . ? C35 C30 C31 C26 177.5(4) . . . . ? C29 C30 C31 C26 -0.1(6) . . . . ? C35 C30 C31 C32 -0.1(6) . . . . ? C29 C30 C31 C32 -177.6(4) . . . . ? C26 C31 C32 C33 -175.6(4) . . . . ? C30 C31 C32 C33 1.9(7) . . . . ? C31 C32 C33 C34 -2.8(8) . . . . ? C32 C33 C34 C35 1.8(8) . . . . ? C33 C34 C35 C30 0.1(8) . . . . ? C29 C30 C35 C34 176.5(4) . . . . ? C31 C30 C35 C34 -0.9(7) . . . . ? Er2 O11 C36 O12 -86.7(10) 4_566 . . . ? Er2 O11 C36 C29 94.7(10) 4_566 . . . ? Er2 O12 C36 O11 12.6(5) 2 . . . ? Er2 O12 C36 C29 -168.8(3) 2 . . . ? C28 C29 C36 O11 45.6(6) . . . . ? C30 C29 C36 O11 -137.4(4) . . . . ? C28 C29 C36 O12 -133.1(4) . . . . ? C30 C29 C36 O12 43.9(6) . . . . ? C39A N1A C37A C38A 0.1(2) . . . . ? C40A N1A C37A C38A 180.0(2) . . . . ? N1A C37A C38A N2A 0.1(3) . . . . ? C39A N2A C38A C37A -0.3(3) . . . . ? C41A N2A C38A C37A 179.5(2) . . . . ? C37A N1A C39A N2A -0.3(3) . . . . ? C40A N1A C39A N2A 179.8(2) . . . . ? C38A N2A C39A N1A 0.4(3) . . . . ? C41A N2A C39A N1A -179.4(2) . . . . ? C39A N2A C41A C42A -178.8(8) . . . . ? C38A N2A C41A C42A 1.4(8) . . . . ? N2A C41A C42A C43A -81.6(11) . . . . ? C44A C43A C42A C41A 176.7(10) . . . . ? C42A C43A C44A C45A -156.7(11) . . . . ? C43A C44A C45A C46A -42.7(16) . . . . ? C39B N1B C37B C38B -0.1(2) . . . . ? C40B N1B C37B C38B 179.9(2) . . . . ? N1B C37B C38B N2B -0.1(3) . . . . ? C39B N2B C38B C37B 0.2(3) . . . . ? C41B N2B C38B C37B -179.8(2) . . . . ? C38B N2B C39B N1B -0.3(3) . . . . ? C41B N2B C39B N1B 179.8(2) . . . . ? C37B N1B C39B N2B 0.2(3) . . . . ? C40B N1B C39B N2B -179.8(2) . . . . ? C39B N2B C41B C42B -0.7(9) . . . . ? C38B N2B C41B C42B 179.3(9) . . . . ? N2B C41B C42B C43B 120.4(9) . . . . ? C41B C42B C43B C44B 71.0(18) . . . . ? C42B C43B C44B C45B -177.0(14) . . . . ? C43B C44B C45B C46B -164.6(16) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.603 _refine_diff_density_min -1.223 _refine_diff_density_rms 0.134 #===END data_compound-12 _database_code_depnum_ccdc_archive 'CCDC 876532' #TrackingRef '- compound 1-12.cif' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Cl O12 Y2, C10 H19 N2' _chemical_formula_sum 'C46 H37 Cl N2 O12 Y2' _chemical_formula_weight 1023.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.6892(3) _cell_length_b 14.7676(4) _cell_length_c 15.8400(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.1242(19) _cell_angle_gamma 90.00 _cell_volume 4127.12(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7017 _cell_measurement_theta_min 2.5570 _cell_measurement_theta_max 28.8111 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 2.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73489 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17701 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8504 _reflns_number_gt 5175 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0320P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8504 _refine_ls_number_parameters 607 _refine_ls_number_restraints 384 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.111 _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 Y1 Y 0.37866(2) 0.02467(3) -0.00389(3) 0.01513(11) Uani 1 1 d . . . Y2 Y 0.11774(2) 0.01193(3) -0.00136(3) 0.01568(11) Uani 1 1 d . . . Cl1 Cl 0.25234(5) -0.08147(8) 0.02692(8) 0.0315(3) Uani 1 1 d . . . O1 O 0.45068(15) 0.1202(2) -0.0777(2) 0.0379(9) Uani 1 1 d . . . O2 O 0.57641(15) 0.1030(2) -0.0672(2) 0.0381(9) Uani 1 1 d . . . O3 O 0.31568(15) 0.1278(2) 0.0734(2) 0.0399(10) Uani 1 1 d . . . O5 O 0.46850(17) 0.4266(3) -0.4040(2) 0.0437(10) Uani 1 1 d . . . O4 O 0.19248(15) 0.1324(2) 0.0329(2) 0.0327(9) Uani 1 1 d . . . O6 O 0.59417(16) 0.4301(3) -0.3882(2) 0.0393(10) Uani 1 1 d . . . O7 O 0.29285(14) 0.4291(2) 0.39158(19) 0.0329(9) Uani 1 1 d . . . O8 O 0.16853(14) 0.4564(2) 0.37114(18) 0.0263(8) Uani 1 1 d . . . O9 O 0.06125(15) 0.0839(2) 0.10973(19) 0.0303(8) Uani 1 1 d . . . O10 O -0.06494(15) 0.0994(2) 0.08571(19) 0.0290(8) Uani 1 1 d . . . O11 O 0.02303(16) 0.4071(2) 0.4353(2) 0.0338(9) Uani 1 1 d . . . O12 O -0.09926(15) 0.4023(2) 0.3970(2) 0.0343(9) Uani 1 1 d . . . C1 C 0.5161(2) 0.1411(3) -0.0962(3) 0.0256(11) Uani 1 1 d . . . C2 C 0.5222(2) 0.2144(3) -0.1608(3) 0.0234(11) Uani 1 1 d . . . C3 C 0.4722(2) 0.2123(3) -0.2306(3) 0.0310(13) Uani 1 1 d . . . H3A H 0.4352 0.1675 -0.2350 0.037 Uiso 1 1 calc R . . C4 C 0.4754(2) 0.2759(4) -0.2955(3) 0.0330(13) Uani 1 1 d . . . H4A H 0.4411 0.2721 -0.3428 0.040 Uiso 1 1 calc R . . C5 C 0.5284(2) 0.3438(3) -0.2905(3) 0.0230(11) Uani 1 1 d . . . C6 C 0.5798(2) 0.3511(3) -0.2177(3) 0.0191(10) Uani 1 1 d . . . C7 C 0.5776(2) 0.2848(3) -0.1523(3) 0.0215(11) Uani 1 1 d . . . C8 C 0.6282(2) 0.2940(4) -0.0793(3) 0.0327(12) Uani 1 1 d . . . H8A H 0.6282 0.2507 -0.0367 0.039 Uiso 1 1 calc R . . C9 C 0.6768(3) 0.3656(4) -0.0707(3) 0.0413(14) Uani 1 1 d . . . H9A H 0.7100 0.3702 -0.0226 0.050 Uiso 1 1 calc R . . C10 C 0.6774(2) 0.4320(4) -0.1332(3) 0.0369(13) Uani 1 1 d . . . H10A H 0.7098 0.4814 -0.1257 0.044 Uiso 1 1 calc R . . C11 C 0.6312(2) 0.4254(3) -0.2047(3) 0.0313(12) Uani 1 1 d . . . H11A H 0.6330 0.4698 -0.2462 0.038 Uiso 1 1 calc R . . C12 C 0.5309(2) 0.4051(3) -0.3660(3) 0.0276(12) Uani 1 1 d . . . C13 C 0.2498(2) 0.1598(3) 0.0777(3) 0.0274(11) Uani 1 1 d . . . C14 C 0.2405(2) 0.2324(3) 0.1419(3) 0.0258(11) Uani 1 1 d . . . C15 C 0.2832(2) 0.2244(4) 0.2174(3) 0.0351(13) Uani 1 1 d . . . H15A H 0.3168 0.1761 0.2249 0.042 Uiso 1 1 calc R . . C16 C 0.2781(2) 0.2861(3) 0.2828(3) 0.0327(13) Uani 1 1 d . . . H16A H 0.3090 0.2791 0.3323 0.039 Uiso 1 1 calc R . . C17 C 0.2279(2) 0.3576(3) 0.2757(3) 0.0212(10) Uani 1 1 d . . . C18 C 0.1807(2) 0.3675(3) 0.1997(3) 0.0179(10) Uani 1 1 d . . . C19 C 0.1874(2) 0.3060(3) 0.1317(3) 0.0222(11) Uani 1 1 d . . . C20 C 0.1446(2) 0.3212(3) 0.0540(3) 0.0323(12) Uani 1 1 d . . . H20A H 0.1498 0.2825 0.0085 0.039 Uiso 1 1 calc R . . C21 C 0.0957(2) 0.3929(4) 0.0457(3) 0.0355(13) Uani 1 1 d . . . H21A H 0.0678 0.4022 -0.0056 0.043 Uiso 1 1 calc R . . C22 C 0.0868(2) 0.4521(4) 0.1126(3) 0.0346(13) Uani 1 1 d . . . H22A H 0.0529 0.5001 0.1057 0.042 Uiso 1 1 calc R . . C23 C 0.1274(2) 0.4403(3) 0.1879(3) 0.0256(11) Uani 1 1 d . . . H23A H 0.1205 0.4800 0.2323 0.031 Uiso 1 1 calc R . . C24 C 0.2293(2) 0.4193(3) 0.3515(3) 0.0213(10) Uani 1 1 d . . . C25 C -0.0002(2) 0.1230(3) 0.1204(3) 0.0239(11) Uani 1 1 d . . . C26 C -0.0009(2) 0.2009(3) 0.1812(3) 0.0220(11) Uani 1 1 d . . . C27 C 0.0400(2) 0.1927(4) 0.2572(3) 0.0333(13) Uani 1 1 d . . . H27A H 0.0733 0.1443 0.2662 0.040 Uiso 1 1 calc R . . C28 C 0.0329(2) 0.2558(3) 0.3216(3) 0.0314(13) Uani 1 1 d . . . H28A H 0.0617 0.2493 0.3727 0.038 Uiso 1 1 calc R . . C29 C -0.0163(2) 0.3273(3) 0.3101(3) 0.0235(11) Uani 1 1 d . . . C30 C -0.0536(2) 0.3437(3) 0.2291(3) 0.0226(11) Uani 1 1 d . . . C31 C -0.0463(2) 0.2793(3) 0.1641(3) 0.0231(11) Uani 1 1 d . . . C32 C -0.0814(3) 0.2986(4) 0.0826(3) 0.0354(13) Uani 1 1 d . . . H32A H -0.0781 0.2570 0.0389 0.042 Uiso 1 1 calc R . . C33 C -0.1200(3) 0.3774(4) 0.0679(4) 0.0451(15) Uani 1 1 d . . . H33A H -0.1417 0.3894 0.0139 0.054 Uiso 1 1 calc R . . C34 C -0.1274(3) 0.4400(4) 0.1318(4) 0.0435(14) Uani 1 1 d . . . H34A H -0.1543 0.4933 0.1205 0.052 Uiso 1 1 calc R . . C35 C -0.0956(2) 0.4238(4) 0.2114(3) 0.0345(12) Uani 1 1 d . . . H35A H -0.1015 0.4657 0.2542 0.041 Uiso 1 1 calc R . . C36 C -0.0312(2) 0.3833(3) 0.3857(3) 0.0259(11) Uani 1 1 d . . . N1A N 0.2332(6) -0.2669(7) 0.2720(6) 0.0532(15) Uani 0.515(4) 1 d PDU A 1 N2A N 0.3024(6) -0.1508(7) 0.2705(6) 0.0636(15) Uani 0.515(4) 1 d PDU A 1 C37A C 0.2722(10) -0.2664(11) 0.3454(9) 0.0629(19) Uani 0.515(4) 1 d PDU A 1 H37A H 0.2670 -0.3056 0.3905 0.075 Uiso 0.515(4) 1 calc PR A 1 C38A C 0.3237(7) -0.1942(9) 0.3418(7) 0.0657(19) Uani 0.515(4) 1 d PDU A 1 H38A H 0.3638 -0.1799 0.3807 0.079 Uiso 0.515(4) 1 calc PR A 1 C39A C 0.2472(15) -0.1967(14) 0.2262(12) 0.0534(18) Uani 0.515(4) 1 d PDU A 1 H39A H 0.2239 -0.1814 0.1737 0.064 Uiso 0.515(4) 1 calc PR A 1 C40A C 0.1800(6) -0.3388(8) 0.2445(9) 0.069(3) Uani 0.515(4) 1 d PDU A 1 H40A H 0.1468 -0.3174 0.1982 0.103 Uiso 0.515(4) 1 calc PR A 1 H40B H 0.1507 -0.3557 0.2907 0.103 Uiso 0.515(4) 1 calc PR A 1 H40C H 0.2077 -0.3904 0.2266 0.103 Uiso 0.515(4) 1 calc PR A 1 C41A C 0.3367(9) -0.0715(10) 0.2386(9) 0.091(2) Uani 0.515(4) 1 d PDU A 1 H41A H 0.2974 -0.0327 0.2125 0.109 Uiso 0.515(4) 1 calc PR A 1 H41B H 0.3698 -0.0890 0.1951 0.109 Uiso 0.515(4) 1 calc PR A 1 C43A C 0.3451(9) 0.0369(12) 0.3750(10) 0.131(2) Uani 0.515(4) 1 d PDU A 1 H43A H 0.3303 -0.0014 0.4208 0.157 Uiso 0.515(4) 1 calc PR A 1 H43B H 0.3012 0.0704 0.3519 0.157 Uiso 0.515(4) 1 calc PR A 1 C42A C 0.3810(10) -0.0201(12) 0.3050(10) 0.112(2) Uani 0.515(4) 1 d PDU A 1 H42A H 0.4129 0.0212 0.2758 0.134 Uiso 0.515(4) 1 calc PR A 1 H42B H 0.4148 -0.0633 0.3344 0.134 Uiso 0.515(4) 1 calc PR A 1 C44A C 0.4123(11) 0.1036(12) 0.4065(9) 0.145(3) Uani 0.515(4) 1 d PDU A 1 H44A H 0.4571 0.0873 0.3780 0.174 Uiso 0.515(4) 1 calc PR A 1 H44B H 0.3983 0.1647 0.3893 0.174 Uiso 0.515(4) 1 calc PR A 1 C45A C 0.4333(9) 0.1035(14) 0.5046(9) 0.147(3) Uani 0.515(4) 1 d PDU A 1 H45A H 0.4422 0.0423 0.5254 0.176 Uiso 0.515(4) 1 calc PR A 1 H45D H 0.4783 0.1396 0.5187 0.176 Uiso 0.515(4) 1 calc PR A 1 C46A C 0.3636(11) 0.1453(14) 0.5423(12) 0.173(5) Uani 0.515(4) 1 d PDU A 1 H46A H 0.3719 0.1476 0.6028 0.259 Uiso 0.515(4) 1 calc PR A 1 H46B H 0.3198 0.1090 0.5270 0.259 Uiso 0.515(4) 1 calc PR A 1 H46C H 0.3557 0.2055 0.5206 0.259 Uiso 0.515(4) 1 calc PR A 1 N2B N 0.2913(6) -0.2057(8) 0.2988(7) 0.0636(15) Uani 0.485(4) 1 d PDU A 2 N1B N 0.2079(6) -0.2808(7) 0.2281(7) 0.0532(15) Uani 0.485(4) 1 d PDU A 2 C40B C 0.1557(6) -0.3140(9) 0.1595(8) 0.069(3) Uani 0.485(4) 1 d PDU A 2 H40D H 0.1575 -0.2748 0.1114 0.103 Uiso 0.485(4) 1 calc PR A 2 H40E H 0.1052 -0.3150 0.1779 0.103 Uiso 0.485(4) 1 calc PR A 2 H40F H 0.1702 -0.3742 0.1442 0.103 Uiso 0.485(4) 1 calc PR A 2 C37B C 0.2182(7) -0.3218(9) 0.3025(7) 0.0629(19) Uani 0.485(4) 1 d PDU A 2 H37B H 0.1900 -0.3692 0.3228 0.075 Uiso 0.485(4) 1 calc PR A 2 C38B C 0.2812(11) -0.2780(11) 0.3441(11) 0.0657(19) Uani 0.485(4) 1 d PDU A 2 H38B H 0.3093 -0.2965 0.3930 0.079 Uiso 0.485(4) 1 calc PR A 2 C41B C 0.3468(8) -0.1395(9) 0.3225(10) 0.091(2) Uani 0.485(4) 1 d PDU A 2 H41C H 0.3963 -0.1615 0.3092 0.109 Uiso 0.485(4) 1 calc PR A 2 H41D H 0.3481 -0.1297 0.3832 0.109 Uiso 0.485(4) 1 calc PR A 2 C42B C 0.3301(11) -0.0481(11) 0.2759(11) 0.112(2) Uani 0.485(4) 1 d PDU A 2 H42C H 0.3259 -0.0566 0.2150 0.134 Uiso 0.485(4) 1 calc PR A 2 H42D H 0.2836 -0.0212 0.2930 0.134 Uiso 0.485(4) 1 calc PR A 2 C39B C 0.2501(16) -0.2082(15) 0.2247(13) 0.0534(18) Uani 0.485(4) 1 d PDU A 2 H39B H 0.2511 -0.1671 0.1803 0.064 Uiso 0.485(4) 1 calc PR A 2 C44B C 0.4068(11) 0.0315(12) 0.4001(10) 0.145(3) Uani 0.485(4) 1 d PDU A 2 H44C H 0.4585 0.0506 0.4147 0.174 Uiso 0.485(4) 1 calc PR A 2 H44D H 0.3996 -0.0253 0.4292 0.174 Uiso 0.485(4) 1 calc PR A 2 C43B C 0.3995(11) 0.0115(14) 0.3037(11) 0.131(2) Uani 0.485(4) 1 d PDU A 2 H43C H 0.3956 0.0685 0.2731 0.157 Uiso 0.485(4) 1 calc PR A 2 H43D H 0.4452 -0.0187 0.2883 0.157 Uiso 0.485(4) 1 calc PR A 2 C45B C 0.3537(9) 0.1024(14) 0.4376(12) 0.147(3) Uani 0.485(4) 1 d PDU A 2 H45B H 0.3304 0.1404 0.3930 0.176 Uiso 0.485(4) 1 calc PR A 2 H45C H 0.3140 0.0724 0.4663 0.176 Uiso 0.485(4) 1 calc PR A 2 C46B C 0.4039(13) 0.1597(14) 0.5006(13) 0.173(5) Uani 0.485(4) 1 d PDU A 2 H46G H 0.3734 0.2045 0.5259 0.259 Uiso 0.485(4) 1 calc PR A 2 H46D H 0.4427 0.1892 0.4712 0.259 Uiso 0.485(4) 1 calc PR A 2 H46E H 0.4270 0.1212 0.5439 0.259 Uiso 0.485(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.00972(18) 0.0165(3) 0.0191(2) -0.0004(2) 0.00059(15) 0.00064(19) Y2 0.01061(18) 0.0170(3) 0.0194(2) 0.0003(2) 0.00041(15) -0.00067(19) Cl1 0.0125(4) 0.0272(7) 0.0548(9) 0.0138(6) 0.0033(5) 0.0014(5) O1 0.0142(15) 0.045(2) 0.056(2) 0.0230(19) 0.0068(15) -0.0035(15) O2 0.0172(15) 0.037(2) 0.059(3) 0.0243(19) -0.0031(15) 0.0025(15) O3 0.0132(14) 0.047(3) 0.059(2) -0.029(2) 0.0008(15) 0.0063(15) O5 0.0274(17) 0.055(3) 0.046(2) 0.026(2) -0.0149(16) -0.0049(18) O4 0.0145(14) 0.031(2) 0.052(2) -0.0151(17) -0.0019(14) -0.0042(14) O6 0.0270(17) 0.055(3) 0.036(2) 0.0225(19) 0.0037(15) -0.0089(17) O7 0.0120(14) 0.049(2) 0.037(2) -0.0168(18) -0.0045(13) 0.0016(15) O8 0.0155(13) 0.038(2) 0.0251(18) -0.0094(16) 0.0017(12) 0.0079(14) O9 0.0184(15) 0.040(2) 0.033(2) -0.0120(17) 0.0043(13) 0.0017(15) O10 0.0200(15) 0.035(2) 0.032(2) -0.0177(17) 0.0035(13) -0.0082(15) O11 0.0257(16) 0.040(2) 0.035(2) -0.0149(18) 0.0001(14) -0.0123(16) O12 0.0176(15) 0.043(2) 0.043(2) -0.0144(18) 0.0077(14) -0.0008(15) C1 0.019(2) 0.024(3) 0.034(3) 0.008(2) 0.002(2) -0.003(2) C2 0.013(2) 0.025(3) 0.032(3) 0.010(2) 0.0011(19) 0.002(2) C3 0.018(2) 0.031(3) 0.043(3) 0.015(3) -0.005(2) -0.009(2) C4 0.020(2) 0.043(4) 0.034(3) 0.009(3) -0.008(2) -0.006(2) C5 0.014(2) 0.021(3) 0.034(3) 0.008(2) 0.0004(19) -0.0004(19) C6 0.0115(19) 0.021(3) 0.025(3) 0.003(2) 0.0045(17) -0.0003(19) C7 0.0122(19) 0.025(3) 0.027(3) 0.004(2) 0.0006(18) 0.0012(19) C8 0.030(2) 0.038(3) 0.030(3) 0.009(2) -0.002(2) -0.004(2) C9 0.035(3) 0.052(4) 0.035(3) 0.003(3) -0.007(2) -0.007(3) C10 0.027(2) 0.042(4) 0.042(3) 0.001(3) 0.000(2) -0.017(2) C11 0.029(2) 0.028(3) 0.038(3) 0.005(2) 0.004(2) -0.003(2) C12 0.026(2) 0.029(3) 0.027(3) 0.006(2) -0.004(2) -0.005(2) C13 0.021(2) 0.024(3) 0.037(3) -0.009(2) 0.003(2) -0.003(2) C14 0.016(2) 0.025(3) 0.037(3) -0.009(2) 0.0060(19) -0.001(2) C15 0.025(2) 0.035(3) 0.044(3) -0.012(3) -0.009(2) 0.016(2) C16 0.021(2) 0.036(3) 0.039(3) -0.013(3) -0.012(2) 0.011(2) C17 0.015(2) 0.024(3) 0.025(3) -0.005(2) 0.0013(18) -0.0004(19) C18 0.0132(19) 0.018(3) 0.023(3) -0.002(2) 0.0021(17) -0.0022(18) C19 0.0131(19) 0.025(3) 0.028(3) -0.004(2) -0.0004(18) -0.0005(19) C20 0.033(3) 0.035(3) 0.029(3) -0.011(2) -0.003(2) 0.002(2) C21 0.033(3) 0.042(3) 0.030(3) 0.002(3) -0.011(2) 0.006(2) C22 0.030(2) 0.034(3) 0.038(3) 0.001(3) -0.004(2) 0.009(2) C23 0.022(2) 0.022(3) 0.033(3) -0.008(2) 0.0020(19) 0.003(2) C24 0.020(2) 0.022(3) 0.021(3) 0.000(2) 0.0024(18) -0.002(2) C25 0.025(2) 0.025(3) 0.023(3) -0.004(2) 0.0059(19) -0.006(2) C26 0.015(2) 0.023(3) 0.029(3) -0.008(2) 0.0056(19) -0.0035(19) C27 0.020(2) 0.039(3) 0.041(3) -0.017(3) -0.002(2) 0.010(2) C28 0.026(2) 0.037(3) 0.030(3) -0.013(3) -0.007(2) 0.008(2) C29 0.015(2) 0.026(3) 0.030(3) -0.012(2) 0.0031(19) -0.004(2) C30 0.014(2) 0.023(3) 0.031(3) -0.003(2) 0.0028(19) -0.0027(19) C31 0.017(2) 0.027(3) 0.027(3) -0.002(2) 0.0044(19) -0.007(2) C32 0.038(3) 0.037(3) 0.030(3) -0.006(3) -0.003(2) -0.005(3) C33 0.041(3) 0.054(4) 0.039(4) 0.011(3) -0.009(2) -0.003(3) C34 0.037(3) 0.035(4) 0.058(4) 0.009(3) -0.001(3) 0.010(3) C35 0.034(3) 0.032(3) 0.038(3) -0.002(3) 0.008(2) -0.003(2) C36 0.024(2) 0.023(3) 0.031(3) -0.006(2) 0.005(2) -0.007(2) N1A 0.057(3) 0.048(3) 0.057(3) 0.009(3) 0.017(3) 0.015(3) N2A 0.071(3) 0.061(3) 0.061(3) 0.007(3) 0.014(3) -0.001(3) C37A 0.074(4) 0.059(4) 0.058(4) 0.016(3) 0.014(3) 0.025(3) C38A 0.075(4) 0.065(4) 0.058(3) 0.012(3) 0.009(3) 0.019(3) C39A 0.057(3) 0.055(4) 0.050(3) 0.007(3) 0.011(2) 0.003(3) C40A 0.054(5) 0.059(6) 0.094(6) -0.020(6) 0.011(5) 0.007(4) C41A 0.101(4) 0.083(4) 0.092(4) 0.008(4) 0.024(4) -0.016(4) C43A 0.173(5) 0.100(5) 0.125(5) 0.013(4) 0.049(4) -0.013(5) C42A 0.135(4) 0.095(4) 0.108(4) 0.014(4) 0.027(4) -0.023(4) C44A 0.195(6) 0.106(5) 0.141(5) 0.013(5) 0.060(5) -0.013(5) C45A 0.193(7) 0.108(6) 0.148(6) 0.018(6) 0.067(6) -0.002(6) C46A 0.234(10) 0.107(9) 0.192(10) -0.026(9) 0.112(9) -0.018(9) N2B 0.071(3) 0.061(3) 0.061(3) 0.007(3) 0.014(3) -0.001(3) N1B 0.057(3) 0.048(3) 0.057(3) 0.009(3) 0.017(3) 0.015(3) C40B 0.054(5) 0.059(6) 0.094(6) -0.020(6) 0.011(5) 0.007(4) C37B 0.074(4) 0.059(4) 0.058(4) 0.016(3) 0.014(3) 0.025(3) C38B 0.075(4) 0.065(4) 0.058(3) 0.012(3) 0.009(3) 0.019(3) C41B 0.101(4) 0.083(4) 0.092(4) 0.008(4) 0.024(4) -0.016(4) C42B 0.135(4) 0.095(4) 0.108(4) 0.014(4) 0.027(4) -0.023(4) C39B 0.057(3) 0.055(4) 0.050(3) 0.007(3) 0.011(2) 0.003(3) C44B 0.195(6) 0.106(5) 0.141(5) 0.013(5) 0.060(5) -0.013(5) C43B 0.173(5) 0.100(5) 0.125(5) 0.013(4) 0.049(4) -0.013(5) C45B 0.193(7) 0.108(6) 0.148(6) 0.018(6) 0.067(6) -0.002(6) C46B 0.234(10) 0.107(9) 0.192(10) -0.026(9) 0.112(9) -0.018(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O7 2.269(3) 4_565 ? Y1 O5 2.277(3) 4_566 ? Y1 O1 2.279(3) . ? Y1 O6 2.285(3) 2_644 ? Y1 O3 2.292(3) . ? Y1 O2 2.307(3) 3_655 ? Y1 Cl1 2.8009(11) . ? Y2 O11 2.236(3) 4_565 ? Y2 O4 2.259(3) . ? Y2 O10 2.276(3) 3 ? Y2 O8 2.316(3) 4_565 ? Y2 O9 2.340(3) . ? Y2 O12 2.353(3) 2_545 ? Y2 Cl1 2.7602(11) . ? O1 C1 1.253(5) . ? O2 C1 1.263(5) . ? O2 Y1 2.307(3) 3_655 ? O3 C13 1.264(5) . ? O5 C12 1.260(5) . ? O5 Y1 2.277(3) 4_565 ? O4 C13 1.262(5) . ? O6 C12 1.253(5) . ? O6 Y1 2.285(3) 2_654 ? O7 C24 1.259(4) . ? O7 Y1 2.269(3) 4_566 ? O8 C24 1.266(5) . ? O8 Y2 2.316(3) 4_566 ? O9 C25 1.253(5) . ? O10 C25 1.282(5) . ? O10 Y2 2.276(3) 3 ? O11 C36 1.247(5) . ? O11 Y2 2.236(3) 4_566 ? O12 C36 1.261(5) . ? O12 Y2 2.353(3) 2 ? C1 C2 1.500(6) . ? C2 C3 1.366(6) . ? C2 C7 1.429(6) . ? C3 C4 1.397(6) . ? C3 H3A 0.9300 . ? C4 C5 1.371(6) . ? C4 H4A 0.9300 . ? C5 C6 1.420(6) . ? C5 C12 1.502(6) . ? C6 C7 1.428(6) . ? C6 C11 1.431(6) . ? C7 C8 1.416(6) . ? C8 C9 1.364(7) . ? C8 H8A 0.9300 . ? C9 C10 1.395(7) . ? C9 H9A 0.9300 . ? C10 C11 1.351(6) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.495(6) . ? C14 C15 1.373(6) . ? C14 C19 1.437(6) . ? C15 C16 1.387(6) . ? C15 H15A 0.9300 . ? C16 C17 1.379(6) . ? C16 H16A 0.9300 . ? C17 C18 1.423(5) . ? C17 C24 1.506(6) . ? C18 C19 1.421(6) . ? C18 C23 1.433(6) . ? C19 C20 1.416(6) . ? C20 C21 1.368(6) . ? C20 H20A 0.9300 . ? C21 C22 1.390(7) . ? C21 H21A 0.9300 . ? C22 C23 1.359(6) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.501(6) . ? C26 C27 1.365(6) . ? C26 C31 1.425(6) . ? C27 C28 1.393(6) . ? C27 H27A 0.9300 . ? C28 C29 1.372(6) . ? C28 H28A 0.9300 . ? C29 C30 1.422(6) . ? C29 C36 1.494(6) . ? C30 C31 1.414(6) . ? C30 C35 1.414(6) . ? C31 C32 1.421(6) . ? C32 C33 1.360(7) . ? C32 H32A 0.9300 . ? C33 C34 1.385(7) . ? C33 H33A 0.9300 . ? C34 C35 1.364(7) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? N1A C39A 1.298(8) . ? N1A C37A 1.308(9) . ? N1A C40A 1.464(12) . ? N2A C38A 1.328(8) . ? N2A C39A 1.344(9) . ? N2A C41A 1.428(12) . ? C37A C38A 1.406(19) . ? C37A H37A 0.9300 . ? C38A H38A 0.9300 . ? C39A H39A 0.9300 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.476(9) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A C42A 1.563(10) . ? C43A C44A 1.596(10) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C44A C45A 1.572(10) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.537(10) . ? C45A H45A 0.9700 . ? C45A H45D 0.9700 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? N2B C38B 1.307(10) . ? N2B C39B 1.337(10) . ? N2B C41B 1.417(12) . ? N1B C39B 1.309(8) . ? N1B C37B 1.326(9) . ? N1B C40B 1.459(12) . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C37B C38B 1.411(19) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C41B C42B 1.557(10) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.550(10) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C39B H39B 0.9300 . ? C44B C43B 1.551(10) . ? C44B C45B 1.552(10) . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C45B C46B 1.541(10) . ? C45B H45B 0.9700 . ? C45B H45C 0.9700 . ? C46B H46G 0.9600 . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? 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 O7 Y1 O5 143.98(13) 4_565 4_566 ? O7 Y1 O1 78.98(11) 4_565 . ? O5 Y1 O1 76.88(13) 4_566 . ? O7 Y1 O6 78.67(12) 4_565 2_644 ? O5 Y1 O6 122.62(11) 4_566 2_644 ? O1 Y1 O6 80.73(13) . 2_644 ? O7 Y1 O3 82.22(12) 4_565 . ? O5 Y1 O3 76.16(11) 4_566 . ? O1 Y1 O3 100.02(13) . . ? O6 Y1 O3 160.37(11) 2_644 . ? O7 Y1 O2 142.22(12) 4_565 3_655 ? O5 Y1 O2 73.77(13) 4_566 3_655 ? O1 Y1 O2 124.77(10) . 3_655 ? O6 Y1 O2 77.40(13) 2_644 3_655 ? O3 Y1 O2 116.48(13) . 3_655 ? O7 Y1 Cl1 78.18(8) 4_565 . ? O5 Y1 Cl1 125.56(10) 4_566 . ? O1 Y1 Cl1 156.65(8) . . ? O6 Y1 Cl1 90.09(9) 2_644 . ? O3 Y1 Cl1 81.62(9) . . ? O2 Y1 Cl1 73.08(7) 3_655 . ? O11 Y2 O4 95.38(12) 4_565 . ? O11 Y2 O10 81.96(12) 4_565 3 ? O4 Y2 O10 156.65(12) . 3 ? O11 Y2 O8 79.99(11) 4_565 4_565 ? O4 Y2 O8 78.09(11) . 4_565 ? O10 Y2 O8 78.61(11) 3 4_565 ? O11 Y2 O9 75.40(11) 4_565 . ? O4 Y2 O9 74.68(11) . . ? O10 Y2 O9 126.16(10) 3 . ? O8 Y2 O9 141.00(12) 4_565 . ? O11 Y2 O12 123.05(11) 4_565 2_545 ? O4 Y2 O12 118.77(12) . 2_545 ? O10 Y2 O12 81.00(12) 3 2_545 ? O8 Y2 O12 146.46(12) 4_565 2_545 ? O9 Y2 O12 72.30(12) . 2_545 ? O11 Y2 Cl1 161.74(9) 4_565 . ? O4 Y2 Cl1 82.61(8) . . ? O10 Y2 Cl1 92.70(8) 3 . ? O8 Y2 Cl1 81.85(7) 4_565 . ? O9 Y2 Cl1 120.99(8) . . ? O12 Y2 Cl1 72.78(7) 2_545 . ? Y2 Cl1 Y1 112.44(4) . . ? C1 O1 Y1 146.3(3) . . ? C1 O2 Y1 142.5(3) . 3_655 ? C13 O3 Y1 139.7(3) . . ? C12 O5 Y1 162.9(3) . 4_565 ? C13 O4 Y2 145.2(3) . . ? C12 O6 Y1 129.1(3) . 2_654 ? C24 O7 Y1 158.3(3) . 4_566 ? C24 O8 Y2 133.8(3) . 4_566 ? C25 O9 Y2 137.1(3) . . ? C25 O10 Y2 139.8(3) . 3 ? C36 O11 Y2 162.1(3) . 4_566 ? C36 O12 Y2 115.8(3) . 2 ? O1 C1 O2 125.2(4) . . ? O1 C1 C2 116.7(4) . . ? O2 C1 C2 118.1(4) . . ? C3 C2 C7 119.5(4) . . ? C3 C2 C1 117.5(4) . . ? C7 C2 C1 122.9(4) . . ? C2 C3 C4 121.5(4) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 119.9(4) . . ? C4 C5 C12 117.0(4) . . ? C6 C5 C12 123.1(4) . . ? C5 C6 C7 119.2(4) . . ? C5 C6 C11 122.6(4) . . ? C7 C6 C11 118.1(4) . . ? C8 C7 C6 118.6(4) . . ? C8 C7 C2 122.4(4) . . ? C6 C7 C2 119.0(4) . . ? C9 C8 C7 120.9(5) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 120.7(5) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C11 C10 C9 120.7(5) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C6 121.1(5) . . ? C10 C11 H11A 119.5 . . ? C6 C11 H11A 119.5 . . ? O6 C12 O5 124.1(4) . . ? O6 C12 C5 118.7(4) . . ? O5 C12 C5 117.2(4) . . ? O4 C13 O3 123.8(4) . . ? O4 C13 C14 119.3(4) . . ? O3 C13 C14 116.9(4) . . ? C15 C14 C19 118.5(4) . . ? C15 C14 C13 116.8(4) . . ? C19 C14 C13 124.6(4) . . ? C14 C15 C16 122.2(4) . . ? C14 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? C17 C16 C15 121.2(4) . . ? C17 C16 H16A 119.4 . . ? C15 C16 H16A 119.4 . . ? C16 C17 C18 118.9(4) . . ? C16 C17 C24 115.1(4) . . ? C18 C17 C24 126.0(4) . . ? C19 C18 C17 119.9(4) . . ? C19 C18 C23 118.2(4) . . ? C17 C18 C23 121.9(4) . . ? C20 C19 C18 119.2(4) . . ? C20 C19 C14 121.5(4) . . ? C18 C19 C14 119.2(4) . . ? C21 C20 C19 120.1(5) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C20 C21 C22 121.2(4) . . ? C20 C21 H21A 119.4 . . ? C22 C21 H21A 119.4 . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C18 120.7(4) . . ? C22 C23 H23A 119.6 . . ? C18 C23 H23A 119.6 . . ? O7 C24 O8 124.7(4) . . ? O7 C24 C17 115.8(4) . . ? O8 C24 C17 119.5(3) . . ? O9 C25 O10 125.0(4) . . ? O9 C25 C26 119.1(4) . . ? O10 C25 C26 115.8(4) . . ? C27 C26 C31 119.7(4) . . ? C27 C26 C25 118.1(4) . . ? C31 C26 C25 122.1(4) . . ? C26 C27 C28 121.1(5) . . ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 . . ? C29 C28 C27 120.5(4) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 119.9(4) . . ? C28 C29 C36 117.9(4) . . ? C30 C29 C36 122.1(4) . . ? C31 C30 C35 119.5(4) . . ? C31 C30 C29 118.8(4) . . ? C35 C30 C29 121.6(4) . . ? C30 C31 C32 118.0(4) . . ? C30 C31 C26 119.2(4) . . ? C32 C31 C26 122.7(4) . . ? C33 C32 C31 120.5(5) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C32 C33 C34 121.4(5) . . ? C32 C33 H33A 119.3 . . ? C34 C33 H33A 119.3 . . ? C35 C34 C33 120.2(5) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C30 120.4(5) . . ? C34 C35 H35A 119.8 . . ? C30 C35 H35A 119.8 . . ? O11 C36 O12 123.1(4) . . ? O11 C36 C29 119.3(4) . . ? O12 C36 C29 117.6(4) . . ? C39A N1A C37A 112.4(12) . . ? C39A N1A C40A 123.9(11) . . ? C37A N1A C40A 123.7(10) . . ? C38A N2A C39A 110.6(11) . . ? C38A N2A C41A 126.5(11) . . ? C39A N2A C41A 122.7(9) . . ? N1A C37A C38A 105.7(13) . . ? N1A C37A H37A 127.2 . . ? C38A C37A H37A 127.2 . . ? N2A C38A C37A 104.7(12) . . ? N2A C38A H38A 127.6 . . ? C37A C38A H38A 127.6 . . ? N1A C39A N2A 105.8(9) . . ? N1A C39A H39A 127.1 . . ? N2A C39A H39A 127.1 . . ? N2A C41A C42A 112.8(12) . . ? N2A C41A H41A 109.0 . . ? C42A C41A H41A 109.0 . . ? N2A C41A H41B 109.0 . . ? C42A C41A H41B 109.0 . . ? H41A C41A H41B 107.8 . . ? C42A C43A C44A 102.9(10) . . ? C42A C43A H43A 111.2 . . ? C44A C43A H43A 111.2 . . ? C42A C43A H43B 111.2 . . ? C44A C43A H43B 111.2 . . ? H43A C43A H43B 109.1 . . ? C41A C42A C43A 124.1(15) . . ? C41A C42A H42A 106.3 . . ? C43A C42A H42A 106.3 . . ? C41A C42A H42B 106.3 . . ? C43A C42A H42B 106.3 . . ? H42A C42A H42B 106.4 . . ? C45A C44A C43A 115.2(12) . . ? C45A C44A H44A 108.5 . . ? C43A C44A H44A 108.5 . . ? C45A C44A H44B 108.5 . . ? C43A C44A H44B 108.5 . . ? H44A C44A H44B 107.5 . . ? C46A C45A C44A 104.1(9) . . ? C46A C45A H45A 110.9 . . ? C44A C45A H45A 110.9 . . ? C46A C45A H45D 110.9 . . ? C44A C45A H45D 110.9 . . ? H45A C45A H45D 108.9 . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C38B N2B C39B 111.8(10) . . ? C38B N2B C41B 122.5(11) . . ? C39B N2B C41B 125.2(11) . . ? C39B N1B C37B 111.6(12) . . ? C39B N1B C40B 125.2(11) . . ? C37B N1B C40B 123.1(10) . . ? N1B C40B H40D 109.5 . . ? N1B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? N1B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N1B C37B C38B 105.0(13) . . ? N1B C37B H37B 127.5 . . ? C38B C37B H37B 127.5 . . ? N2B C38B C37B 104.6(12) . . ? N2B C38B H38B 127.7 . . ? C37B C38B H38B 127.7 . . ? N2B C41B C42B 111.5(11) . . ? N2B C41B H41C 109.3 . . ? C42B C41B H41C 109.3 . . ? N2B C41B H41D 109.3 . . ? C42B C41B H41D 109.3 . . ? H41C C41B H41D 108.0 . . ? C43B C42B C41B 103.8(13) . . ? C43B C42B H42C 111.0 . . ? C41B C42B H42C 111.0 . . ? C43B C42B H42D 111.0 . . ? C41B C42B H42D 111.0 . . ? H42C C42B H42D 109.0 . . ? N1B C39B N2B 105.3(10) . . ? N1B C39B H39B 127.4 . . ? N2B C39B H39B 127.4 . . ? C43B C44B C45B 119.7(14) . . ? C43B C44B H44C 107.4 . . ? C45B C44B H44C 107.4 . . ? C43B C44B H44D 107.4 . . ? C45B C44B H44D 107.4 . . ? H44C C44B H44D 106.9 . . ? C42B C43B C44B 113.3(12) . . ? C42B C43B H43C 108.9 . . ? C44B C43B H43C 108.9 . . ? C42B C43B H43D 108.9 . . ? C44B C43B H43D 108.9 . . ? H43C C43B H43D 107.7 . . ? C46B C45B C44B 106.4(10) . . ? C46B C45B H45B 110.5 . . ? C44B C45B H45B 110.5 . . ? C46B C45B H45C 110.5 . . ? C44B C45B H45C 110.5 . . ? H45B C45B H45C 108.6 . . ? C45B C46B H46G 109.5 . . ? C45B C46B H46D 109.5 . . ? H46G C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46G C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Y2 Cl1 Y1 56.8(3) 4_565 . . . ? O4 Y2 Cl1 Y1 -27.89(10) . . . . ? O10 Y2 Cl1 Y1 129.14(9) 3 . . . ? O8 Y2 Cl1 Y1 51.06(9) 4_565 . . . ? O9 Y2 Cl1 Y1 -95.03(11) . . . . ? O12 Y2 Cl1 Y1 -151.15(10) 2_545 . . . ? O7 Y1 Cl1 Y2 -37.85(10) 4_565 . . . ? O5 Y1 Cl1 Y2 112.16(11) 4_566 . . . ? O1 Y1 Cl1 Y2 -50.0(3) . . . . ? O6 Y1 Cl1 Y2 -116.26(9) 2_644 . . . ? O3 Y1 Cl1 Y2 45.89(10) . . . . ? O2 Y1 Cl1 Y2 166.95(11) 3_655 . . . ? O7 Y1 O1 C1 -155.6(6) 4_565 . . . ? O5 Y1 O1 C1 51.3(6) 4_566 . . . ? O6 Y1 O1 C1 -75.5(6) 2_644 . . . ? O3 Y1 O1 C1 124.4(6) . . . . ? O2 Y1 O1 C1 -8.0(7) 3_655 . . . ? Cl1 Y1 O1 C1 -143.5(5) . . . . ? O7 Y1 O3 C13 32.5(5) 4_565 . . . ? O5 Y1 O3 C13 -176.6(5) 4_566 . . . ? O1 Y1 O3 C13 109.7(5) . . . . ? O6 Y1 O3 C13 19.2(8) 2_644 . . . ? O2 Y1 O3 C13 -113.0(5) 3_655 . . . ? Cl1 Y1 O3 C13 -46.7(5) . . . . ? O11 Y2 O4 C13 165.1(5) 4_565 . . . ? O10 Y2 O4 C13 -112.8(6) 3 . . . ? O8 Y2 O4 C13 -116.4(5) 4_565 . . . ? O9 Y2 O4 C13 91.8(5) . . . . ? O12 Y2 O4 C13 32.5(6) 2_545 . . . ? Cl1 Y2 O4 C13 -33.2(5) . . . . ? O11 Y2 O9 C25 17.0(4) 4_565 . . . ? O4 Y2 O9 C25 116.8(5) . . . . ? O10 Y2 O9 C25 -51.4(5) 3 . . . ? O8 Y2 O9 C25 69.6(5) 4_565 . . . ? O12 Y2 O9 C25 -115.5(5) 2_545 . . . ? Cl1 Y2 O9 C25 -171.8(4) . . . . ? Y1 O1 C1 O2 -2.4(10) . . . . ? Y1 O1 C1 C2 174.6(4) . . . . ? Y1 O2 C1 O1 14.9(9) 3_655 . . . ? Y1 O2 C1 C2 -162.2(4) 3_655 . . . ? O1 C1 C2 C3 -42.9(7) . . . . ? O2 C1 C2 C3 134.4(5) . . . . ? O1 C1 C2 C7 137.5(5) . . . . ? O2 C1 C2 C7 -45.2(7) . . . . ? C7 C2 C3 C4 2.0(7) . . . . ? C1 C2 C3 C4 -177.6(5) . . . . ? C2 C3 C4 C5 -1.1(8) . . . . ? C3 C4 C5 C6 -1.3(7) . . . . ? C3 C4 C5 C12 175.9(4) . . . . ? C4 C5 C6 C7 2.8(7) . . . . ? C12 C5 C6 C7 -174.3(4) . . . . ? C4 C5 C6 C11 -173.6(4) . . . . ? C12 C5 C6 C11 9.3(7) . . . . ? C5 C6 C7 C8 -178.7(4) . . . . ? C11 C6 C7 C8 -2.2(6) . . . . ? C5 C6 C7 C2 -1.9(6) . . . . ? C11 C6 C7 C2 174.6(4) . . . . ? C3 C2 C7 C8 176.2(5) . . . . ? C1 C2 C7 C8 -4.2(7) . . . . ? C3 C2 C7 C6 -0.5(7) . . . . ? C1 C2 C7 C6 179.1(4) . . . . ? C6 C7 C8 C9 1.4(7) . . . . ? C2 C7 C8 C9 -175.3(5) . . . . ? C7 C8 C9 C10 0.7(8) . . . . ? C8 C9 C10 C11 -1.9(8) . . . . ? C9 C10 C11 C6 1.1(8) . . . . ? C5 C6 C11 C10 177.4(5) . . . . ? C7 C6 C11 C10 1.0(7) . . . . ? Y1 O6 C12 O5 3.1(8) 2_654 . . . ? Y1 O6 C12 C5 -178.3(3) 2_654 . . . ? Y1 O5 C12 O6 17.8(16) 4_565 . . . ? Y1 O5 C12 C5 -160.8(10) 4_565 . . . ? C4 C5 C12 O6 -140.4(5) . . . . ? C6 C5 C12 O6 36.8(7) . . . . ? C4 C5 C12 O5 38.2(7) . . . . ? C6 C5 C12 O5 -144.6(5) . . . . ? Y2 O4 C13 O3 59.9(8) . . . . ? Y2 O4 C13 C14 -118.2(5) . . . . ? Y1 O3 C13 O4 4.2(9) . . . . ? Y1 O3 C13 C14 -177.7(3) . . . . ? O4 C13 C14 C15 141.8(5) . . . . ? O3 C13 C14 C15 -36.4(7) . . . . ? O4 C13 C14 C19 -34.6(7) . . . . ? O3 C13 C14 C19 147.2(5) . . . . ? C19 C14 C15 C16 -1.6(7) . . . . ? C13 C14 C15 C16 -178.2(5) . . . . ? C14 C15 C16 C17 1.7(8) . . . . ? C15 C16 C17 C18 0.1(7) . . . . ? C15 C16 C17 C24 -179.4(4) . . . . ? C16 C17 C18 C19 -1.9(6) . . . . ? C24 C17 C18 C19 177.5(4) . . . . ? C16 C17 C18 C23 -179.8(4) . . . . ? C24 C17 C18 C23 -0.4(7) . . . . ? C17 C18 C19 C20 -174.8(4) . . . . ? C23 C18 C19 C20 3.2(6) . . . . ? C17 C18 C19 C14 2.0(6) . . . . ? C23 C18 C19 C14 180.0(4) . . . . ? C15 C14 C19 C20 176.4(5) . . . . ? C13 C14 C19 C20 -7.3(7) . . . . ? C15 C14 C19 C18 -0.3(6) . . . . ? C13 C14 C19 C18 176.0(4) . . . . ? C18 C19 C20 C21 -2.0(7) . . . . ? C14 C19 C20 C21 -178.7(4) . . . . ? C19 C20 C21 C22 0.1(8) . . . . ? C20 C21 C22 C23 0.5(8) . . . . ? C21 C22 C23 C18 0.7(7) . . . . ? C19 C18 C23 C22 -2.6(6) . . . . ? C17 C18 C23 C22 175.3(4) . . . . ? Y1 O7 C24 O8 6.0(12) 4_566 . . . ? Y1 O7 C24 C17 -173.3(6) 4_566 . . . ? Y2 O8 C24 O7 -37.9(7) 4_566 . . . ? Y2 O8 C24 C17 141.4(3) 4_566 . . . ? C16 C17 C24 O7 33.0(6) . . . . ? C18 C17 C24 O7 -146.5(4) . . . . ? C16 C17 C24 O8 -146.4(4) . . . . ? C18 C17 C24 O8 34.2(7) . . . . ? Y2 O9 C25 O10 36.4(7) . . . . ? Y2 O9 C25 C26 -146.8(4) . . . . ? Y2 O10 C25 O9 4.5(8) 3 . . . ? Y2 O10 C25 C26 -172.4(3) 3 . . . ? O9 C25 C26 C27 -43.3(6) . . . . ? O10 C25 C26 C27 133.8(5) . . . . ? O9 C25 C26 C31 140.8(4) . . . . ? O10 C25 C26 C31 -42.2(6) . . . . ? C31 C26 C27 C28 6.0(7) . . . . ? C25 C26 C27 C28 -170.0(4) . . . . ? C26 C27 C28 C29 0.6(8) . . . . ? C27 C28 C29 C30 -7.5(7) . . . . ? C27 C28 C29 C36 169.8(4) . . . . ? C28 C29 C30 C31 7.5(6) . . . . ? C36 C29 C30 C31 -169.6(4) . . . . ? C28 C29 C30 C35 -170.4(4) . . . . ? C36 C29 C30 C35 12.5(7) . . . . ? C35 C30 C31 C32 0.5(6) . . . . ? C29 C30 C31 C32 -177.5(4) . . . . ? C35 C30 C31 C26 177.0(4) . . . . ? C29 C30 C31 C26 -1.0(6) . . . . ? C27 C26 C31 C30 -5.7(6) . . . . ? C25 C26 C31 C30 170.2(4) . . . . ? C27 C26 C31 C32 170.6(4) . . . . ? C25 C26 C31 C32 -13.5(7) . . . . ? C30 C31 C32 C33 0.9(7) . . . . ? C26 C31 C32 C33 -175.5(5) . . . . ? C31 C32 C33 C34 -1.3(8) . . . . ? C32 C33 C34 C35 0.3(8) . . . . ? C33 C34 C35 C30 1.1(8) . . . . ? C31 C30 C35 C34 -1.5(7) . . . . ? C29 C30 C35 C34 176.4(4) . . . . ? Y2 O11 C36 O12 -87.5(11) 4_566 . . . ? Y2 O11 C36 C29 94.3(11) 4_566 . . . ? Y2 O12 C36 O11 12.7(6) 2 . . . ? Y2 O12 C36 C29 -169.1(3) 2 . . . ? C28 C29 C36 O11 44.9(6) . . . . ? C30 C29 C36 O11 -137.9(5) . . . . ? C28 C29 C36 O12 -133.4(5) . . . . ? C30 C29 C36 O12 43.8(6) . . . . ? C39A N1A C37A C38A -8(3) . . . . ? C40A N1A C37A C38A 171.6(12) . . . . ? C39A N2A C38A C37A -7(2) . . . . ? C41A N2A C38A C37A 179.4(15) . . . . ? N1A C37A C38A N2A 8.7(18) . . . . ? C37A N1A C39A N2A 4(3) . . . . ? C40A N1A C39A N2A -175.6(14) . . . . ? C38A N2A C39A N1A 2(3) . . . . ? C41A N2A C39A N1A 176.2(16) . . . . ? C38A N2A C41A C42A -21(2) . . . . ? C39A N2A C41A C42A 165(2) . . . . ? N2A C41A C42A C43A -72(2) . . . . ? C44A C43A C42A C41A -160.5(16) . . . . ? C42A C43A C44A C45A -126.7(16) . . . . ? C43A C44A C45A C46A -68(2) . . . . ? C39B N1B C37B C38B -10(2) . . . . ? C40B N1B C37B C38B 170.3(14) . . . . ? C39B N2B C38B C37B -12(3) . . . . ? C41B N2B C38B C37B 176.0(14) . . . . ? N1B C37B C38B N2B 13(2) . . . . ? C38B N2B C41B C42B -161.4(18) . . . . ? C39B N2B C41B C42B 27(3) . . . . ? N2B C41B C42B C43B -175.3(13) . . . . ? C37B N1B C39B N2B 3(3) . . . . ? C40B N1B C39B N2B -177.0(15) . . . . ? C38B N2B C39B N1B 6(3) . . . . ? C41B N2B C39B N1B 178.2(16) . . . . ? C41B C42B C43B C44B -64(2) . . . . ? C45B C44B C43B C42B -76(2) . . . . ? C43B C44B C45B C46B -136.6(18) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.174 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.108 #===END