# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Shu-Yun Niu' _publ_contact_author_email SYNIU@SOHU.COM loop_ _publ_author_name 'Niu Shuyun' 'Yu-Xian Chi' 'Jing Jin' 'Ye Li' 'Ru Wang' data_c70432 _database_code_depnum_ccdc_archive 'CCDC 714919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H43 Cd N2 Nd O10' _chemical_formula_weight 1112.52 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4169(15) _cell_length_b 15.0768(17) _cell_length_c 15.098(3) _cell_angle_alpha 114.712(2) _cell_angle_beta 99.311(2) _cell_angle_gamma 110.6320(10) _cell_volume 2418.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1114 _exptl_absorpt_coefficient_mu 1.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8596 _exptl_absorpt_correction_T_max 0.8596 _exptl_absorpt_process_details sadabs _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 'Smart Apex II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13153 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9274 _reflns_number_gt 6625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997a)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9274 _refine_ls_number_parameters 671 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.94687(2) 0.45754(2) 0.345109(17) 0.03945(9) Uani 1 1 d . . . Cd2 Cd 0.81980(3) 0.46363(3) 0.09497(2) 0.04659(11) Uani 1 1 d . . . N1 N 0.7794(3) 0.4646(3) -0.0617(3) 0.0467(9) Uani 1 1 d . . . N2 N 0.7052(3) 0.5550(3) 0.0940(3) 0.0534(10) Uani 1 1 d . . . O1 O 1.1192(3) 0.6346(3) 0.4568(2) 0.0527(8) Uani 1 1 d . . . O2 O 0.8713(3) 0.3128(3) 0.3787(3) 0.0598(9) Uani 1 1 d . . . O3 O 0.8883(3) 0.5345(3) 0.4833(2) 0.0556(9) Uani 1 1 d . . . O4 O 1.0997(3) 0.4050(3) 0.3530(2) 0.0619(9) Uani 1 1 d . . . O5 O 0.7479(3) 0.3711(3) 0.2400(3) 0.0675(10) Uani 1 1 d . . . O6 O 0.6662(3) 0.3260(3) 0.0766(3) 0.0675(10) Uani 1 1 d . . . O7 O 0.9073(3) 0.3674(3) 0.0262(2) 0.0601(9) Uani 1 1 d . . . O8 O 0.9432(3) 0.3675(3) 0.1733(2) 0.0590(9) Uani 1 1 d . . . O9 O 0.9147(3) 0.5813(3) 0.2906(2) 0.0557(9) Uani 1 1 d . . . O10 O 0.9768(3) 0.6423(3) 0.1922(3) 0.0651(10) Uani 1 1 d . . . C1 C 1.3160(5) 0.8379(5) 0.5316(5) 0.0692(17) Uani 1 1 d . . . H1A H 1.292(4) 0.781(4) 0.468(4) 0.075(18) Uiso 1 1 d . . . C2 C 1.4048(6) 0.9401(5) 0.5707(5) 0.096(2) Uani 1 1 d . . . H2A H 1.4447 0.9518 0.5283 0.115 Uiso 1 1 calc R . . C3 C 1.4379(5) 1.0267(5) 0.6703(5) 0.0759(17) Uani 1 1 d . . . C4 C 1.3782(5) 1.0056(5) 0.7309(5) 0.0738(17) Uani 1 1 d . . . H4A H 1.393(4) 1.059(4) 0.802(4) 0.085(19) Uiso 1 1 d . . . C5 C 1.2883(5) 0.9018(5) 0.6930(4) 0.0662(15) Uani 1 1 d . . . H5A H 1.243(5) 0.887(4) 0.741(4) 0.093(19) Uiso 1 1 d . . . C6 C 1.2568(4) 0.8163(4) 0.5930(4) 0.0489(12) Uani 1 1 d . . . C7 C 1.1619(4) 0.7049(4) 0.5534(4) 0.0491(12) Uani 1 1 d . . . C8 C 1.5359(6) 1.1393(5) 0.7124(6) 0.118(3) Uani 1 1 d . . . H8A H 1.5455 1.1878 0.7829 0.178 Uiso 1 1 calc R . . H8B H 1.5199 1.1686 0.6695 0.178 Uiso 1 1 calc R . . H8C H 1.6047 1.1334 0.7117 0.178 Uiso 1 1 calc R . . C9 C 0.7415(6) 0.6709(7) 0.6207(5) 0.107(3) Uani 1 1 d . . . H9A H 0.779(4) 0.691(4) 0.679(4) 0.051(14) Uiso 1 1 d . . . C10 C 0.6574(7) 0.7004(7) 0.6059(5) 0.137(4) Uani 1 1 d . . . H10A H 0.6425 0.7420 0.6629 0.164 Uiso 1 1 calc R . . C11 C 0.5943(7) 0.6680(7) 0.5053(6) 0.132(3) Uani 1 1 d . . . C12 C 0.6170(6) 0.6051(7) 0.4237(6) 0.108(3) Uani 1 1 d . . . H12A H 0.573(5) 0.576(5) 0.353(5) 0.10(2) Uiso 1 1 d . . . C13 C 0.7007(6) 0.5743(6) 0.4392(5) 0.080(2) Uani 1 1 d . . . H13A H 0.705(4) 0.526(4) 0.381(4) 0.080(19) Uiso 1 1 d . . . C14 C 0.7652(4) 0.6086(4) 0.5383(4) 0.0597(14) Uani 1 1 d . . . C15 C 0.8572(4) 0.5771(4) 0.5575(4) 0.0496(12) Uani 1 1 d . . . C16 C 0.4995(8) 0.6994(10) 0.4868(7) 0.214(6) Uani 1 1 d . . . H16A H 0.4648 0.6699 0.4132 0.322 Uiso 1 1 calc R . . H16B H 0.5315 0.7785 0.5235 0.322 Uiso 1 1 calc R . . H16C H 0.4428 0.6696 0.5120 0.322 Uiso 1 1 calc R . . C17 C 0.5511(5) 0.2091(5) 0.2240(5) 0.0697(16) Uani 1 1 d . . . H17A H 0.606(4) 0.267(4) 0.293(4) 0.069(16) Uiso 1 1 d . . . C18 C 0.4596(6) 0.1199(6) 0.2119(7) 0.094(2) Uani 1 1 d . . . H18A H 0.4505 0.1173 0.2707 0.113 Uiso 1 1 calc R . . C19 C 0.3827(6) 0.0361(7) 0.1155(9) 0.101(3) Uani 1 1 d . . . C20 C 0.3971(7) 0.0450(6) 0.0314(8) 0.109(3) Uani 1 1 d . . . H20A H 0.360(5) -0.003(4) -0.033(4) 0.067(18) Uiso 1 1 d . . . C21 C 0.4876(5) 0.1329(5) 0.0396(5) 0.0750(17) Uani 1 1 d . . . H21A H 0.512(5) 0.137(5) -0.027(4) 0.10(2) Uiso 1 1 d . . . C22 C 0.5671(4) 0.2171(4) 0.1394(4) 0.0512(12) Uani 1 1 d . . . C23 C 0.6685(4) 0.3125(4) 0.1534(4) 0.0524(12) Uani 1 1 d . . . C24 C 0.2805(6) -0.0646(7) 0.0982(9) 0.186(5) Uani 1 1 d . . . H24A H 0.2371 -0.1140 0.0246 0.279 Uiso 1 1 calc R . . H24B H 0.2330 -0.0410 0.1330 0.279 Uiso 1 1 calc R . . H24C H 0.3074 -0.1021 0.1262 0.279 Uiso 1 1 calc R . . C25 C 1.0378(5) 0.2227(5) 0.0966(4) 0.0624(15) Uani 1 1 d . . . H25A H 1.029(4) 0.240(4) 0.163(4) 0.072(16) Uiso 1 1 d . . . C26 C 1.0867(6) 0.1549(5) 0.0541(5) 0.0777(19) Uani 1 1 d . . . H26A H 1.099(4) 0.120(4) 0.091(4) 0.084(18) Uiso 1 1 d . . . C27 C 1.0993(5) 0.1305(5) -0.0397(5) 0.0760(17) Uani 1 1 d . . . C28 C 1.0625(6) 0.1750(5) -0.0922(5) 0.0715(18) Uani 1 1 d . . . H28A H 1.072(5) 0.165(5) -0.146(5) 0.10(2) Uiso 1 1 d . . . C29 C 1.0138(5) 0.2421(5) -0.0523(4) 0.0554(13) Uani 1 1 d . . . H29A H 0.995(4) 0.272(3) -0.087(3) 0.045(13) Uiso 1 1 d . . . C30 C 1.0015(4) 0.2666(4) 0.0423(3) 0.0443(11) Uani 1 1 d . . . C31 C 0.9480(4) 0.3391(4) 0.0838(3) 0.0454(11) Uani 1 1 d . . . C32 C 1.1519(6) 0.0552(6) -0.0858(6) 0.127(3) Uani 1 1 d . . . H32A H 1.1540 0.0479 -0.1516 0.190 Uiso 1 1 calc R . . H32B H 1.1065 -0.0163 -0.0962 0.190 Uiso 1 1 calc R . . H32C H 1.2282 0.0867 -0.0384 0.190 Uiso 1 1 calc R . . C33 C 1.1013(6) 0.8602(6) 0.3627(6) 0.089(2) Uani 1 1 d . . . H33A H 1.124(4) 0.838(3) 0.304(3) 0.037(13) Uiso 1 1 d . . . C34 C 1.1532(8) 0.9684(6) 0.4472(8) 0.129(4) Uani 1 1 d . . . H34A H 1.2034 1.0255 0.4420 0.155 Uiso 1 1 calc R . . C35 C 1.1314(9) 0.9916(7) 0.5369(8) 0.133(5) Uani 1 1 d . . . C36 C 1.0589(10) 0.9076(9) 0.5428(6) 0.119(4) Uani 1 1 d . . . H36A H 1.040(4) 0.917(4) 0.596(4) 0.058(17) Uiso 1 1 d . . . C37 C 1.0066(6) 0.7984(5) 0.4603(4) 0.0822(19) Uani 1 1 d . . . H37A H 0.9572 0.7419 0.4667 0.099 Uiso 1 1 calc R . . C38 C 1.0285(5) 0.7750(4) 0.3698(4) 0.0610(15) Uani 1 1 d . . . C39 C 0.9723(4) 0.6605(4) 0.2795(4) 0.0489(12) Uani 1 1 d . . . C40 C 1.1888(8) 1.1101(6) 0.6307(6) 0.187(5) Uani 1 1 d . . . H40A H 1.1631 1.1103 0.6865 0.280 Uiso 1 1 calc R . . H40B H 1.1691 1.1558 0.6101 0.280 Uiso 1 1 calc R . . H40C H 1.2703 1.1385 0.6542 0.280 Uiso 1 1 calc R . . C41 C 0.8166(4) 0.4215(4) -0.1367(4) 0.0567(13) Uani 1 1 d . . . H41A H 0.8555 0.3827 -0.1308 0.068 Uiso 1 1 calc R . . C42 C 0.7992(5) 0.4326(6) -0.2245(5) 0.0709(18) Uani 1 1 d . . . H42A H 0.825(4) 0.403(4) -0.270(4) 0.063(18) Uiso 1 1 d . . . C43 C 0.7451(5) 0.4882(6) -0.2347(5) 0.081(2) Uani 1 1 d . . . H43A H 0.733(4) 0.499(4) -0.292(4) 0.079(17) Uiso 1 1 d . . . C44 C 0.7021(4) 0.5335(5) -0.1590(5) 0.0665(16) Uani 1 1 d . . . C45 C 0.6405(5) 0.5940(6) -0.1617(6) 0.089(2) Uani 1 1 d . . . H45A H 0.6288 0.6057 -0.2175 0.107 Uiso 1 1 calc R . . C46 C 0.5998(5) 0.6337(5) -0.0891(6) 0.090(2) Uani 1 1 d . . . H46A H 0.5585 0.6703 -0.0957 0.108 Uiso 1 1 calc R . . C47 C 0.6186(5) 0.6211(4) 0.0000(5) 0.0687(16) Uani 1 1 d . . . C48 C 0.5777(6) 0.6600(5) 0.0803(7) 0.083(2) Uani 1 1 d . . . H48A H 0.536(5) 0.681(4) 0.065(4) 0.07(2) Uiso 1 1 d . . . C49 C 0.6001(5) 0.6476(5) 0.1628(5) 0.0793(18) Uani 1 1 d . . . H49A H 0.5720 0.6731 0.2154 0.095 Uiso 1 1 calc R . . C50 C 0.6660(5) 0.5959(5) 0.1677(5) 0.0688(16) Uani 1 1 d . . . H50A H 0.671(4) 0.577(4) 0.216(3) 0.042(14) Uiso 1 1 d . . . C51 C 0.6821(4) 0.5673(4) 0.0105(4) 0.0510(12) Uani 1 1 d . . . C52 C 0.7226(4) 0.5202(4) -0.0708(4) 0.0492(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.04261(16) 0.04682(16) 0.03079(13) 0.02294(12) 0.01428(11) 0.01877(13) Cd2 0.0535(2) 0.0528(2) 0.03384(19) 0.02146(17) 0.01330(16) 0.02749(19) N1 0.046(2) 0.055(3) 0.039(2) 0.0251(19) 0.0131(18) 0.023(2) N2 0.048(3) 0.051(3) 0.053(3) 0.020(2) 0.019(2) 0.023(2) O1 0.050(2) 0.053(2) 0.047(2) 0.0301(17) 0.0110(16) 0.0133(17) O2 0.070(2) 0.056(2) 0.056(2) 0.0378(18) 0.0262(19) 0.0200(19) O3 0.065(2) 0.070(2) 0.049(2) 0.0329(18) 0.0341(18) 0.039(2) O4 0.068(2) 0.090(3) 0.046(2) 0.0395(19) 0.0253(18) 0.048(2) O5 0.041(2) 0.073(3) 0.062(2) 0.034(2) 0.0062(18) 0.0078(19) O6 0.062(2) 0.076(3) 0.067(2) 0.047(2) 0.0184(19) 0.024(2) O7 0.087(3) 0.079(2) 0.049(2) 0.0423(19) 0.0333(19) 0.058(2) O8 0.076(2) 0.074(2) 0.0320(17) 0.0241(17) 0.0222(17) 0.043(2) O9 0.065(2) 0.051(2) 0.050(2) 0.0291(17) 0.0165(17) 0.0249(19) O10 0.077(3) 0.062(2) 0.050(2) 0.0310(19) 0.0228(19) 0.024(2) C1 0.068(4) 0.056(4) 0.056(4) 0.022(3) 0.026(3) 0.009(3) C2 0.089(5) 0.074(5) 0.084(5) 0.037(4) 0.042(4) -0.001(4) C3 0.062(4) 0.055(4) 0.079(4) 0.031(3) 0.015(3) 0.006(3) C4 0.078(5) 0.059(4) 0.051(4) 0.018(3) 0.012(3) 0.017(4) C5 0.076(4) 0.059(4) 0.057(4) 0.030(3) 0.027(3) 0.024(3) C6 0.046(3) 0.049(3) 0.047(3) 0.028(2) 0.011(2) 0.016(3) C7 0.046(3) 0.052(3) 0.050(3) 0.030(3) 0.011(2) 0.021(3) C8 0.095(5) 0.070(5) 0.128(7) 0.040(5) 0.029(5) -0.004(4) C9 0.116(6) 0.170(8) 0.046(4) 0.037(4) 0.018(4) 0.106(6) C10 0.144(7) 0.214(9) 0.066(5) 0.036(5) 0.025(4) 0.147(7) C11 0.139(7) 0.197(9) 0.070(5) 0.039(5) 0.019(5) 0.133(7) C12 0.106(6) 0.166(8) 0.059(4) 0.047(5) 0.014(4) 0.091(6) C13 0.087(5) 0.114(6) 0.046(3) 0.033(4) 0.022(3) 0.065(4) C14 0.058(3) 0.080(4) 0.042(3) 0.028(3) 0.020(3) 0.037(3) C15 0.047(3) 0.064(3) 0.046(3) 0.030(3) 0.022(2) 0.030(3) C16 0.220(11) 0.336(15) 0.122(8) 0.066(9) 0.026(7) 0.244(12) C17 0.056(4) 0.070(4) 0.075(4) 0.038(4) 0.021(3) 0.020(3) C18 0.068(5) 0.094(5) 0.133(7) 0.072(5) 0.046(5) 0.031(4) C19 0.053(4) 0.082(6) 0.171(9) 0.077(6) 0.029(5) 0.026(4) C20 0.062(5) 0.056(5) 0.123(8) 0.016(5) -0.031(5) 0.009(4) C21 0.061(4) 0.058(4) 0.074(4) 0.023(3) -0.001(3) 0.020(3) C22 0.042(3) 0.053(3) 0.059(3) 0.029(3) 0.012(3) 0.025(3) C23 0.044(3) 0.052(3) 0.060(3) 0.028(3) 0.017(3) 0.024(3) C24 0.071(5) 0.120(7) 0.340(15) 0.144(9) 0.039(7) 0.001(5) C25 0.074(4) 0.068(4) 0.053(3) 0.032(3) 0.019(3) 0.042(3) C26 0.089(5) 0.079(4) 0.089(5) 0.050(4) 0.027(4) 0.056(4) C27 0.076(4) 0.073(4) 0.090(5) 0.041(4) 0.037(4) 0.045(4) C28 0.087(5) 0.072(4) 0.074(4) 0.036(4) 0.051(4) 0.047(4) C29 0.071(4) 0.064(4) 0.052(3) 0.038(3) 0.034(3) 0.039(3) C30 0.043(3) 0.041(3) 0.042(3) 0.021(2) 0.012(2) 0.016(2) C31 0.046(3) 0.043(3) 0.038(3) 0.019(2) 0.013(2) 0.015(2) C32 0.132(7) 0.122(6) 0.168(8) 0.069(6) 0.075(6) 0.099(6) C33 0.091(5) 0.060(5) 0.081(5) 0.026(4) 0.007(4) 0.024(4) C34 0.120(7) 0.054(5) 0.127(7) 0.019(5) -0.024(6) 0.020(5) C35 0.133(8) 0.063(5) 0.114(8) -0.002(6) -0.048(7) 0.055(6) C36 0.160(9) 0.128(8) 0.051(5) 0.006(5) 0.008(5) 0.111(8) C37 0.103(5) 0.077(4) 0.052(4) 0.017(3) 0.007(3) 0.056(4) C38 0.070(4) 0.049(3) 0.051(3) 0.023(3) -0.001(3) 0.027(3) C39 0.048(3) 0.049(3) 0.048(3) 0.026(3) 0.010(2) 0.023(3) C40 0.198(10) 0.082(6) 0.128(7) -0.035(5) -0.068(7) 0.077(6) C41 0.063(3) 0.060(3) 0.046(3) 0.028(3) 0.021(3) 0.025(3) C42 0.065(4) 0.088(5) 0.049(3) 0.039(4) 0.023(3) 0.020(4) C43 0.066(4) 0.119(6) 0.068(4) 0.071(4) 0.018(3) 0.029(4) C44 0.048(3) 0.077(4) 0.074(4) 0.055(3) 0.010(3) 0.013(3) C45 0.070(5) 0.116(6) 0.114(6) 0.091(5) 0.020(4) 0.043(4) C46 0.059(4) 0.086(5) 0.137(7) 0.075(5) 0.013(4) 0.034(4) C47 0.050(3) 0.050(3) 0.093(5) 0.034(3) 0.011(3) 0.021(3) C48 0.055(4) 0.043(4) 0.117(7) 0.025(4) 0.009(4) 0.020(3) C49 0.064(4) 0.054(4) 0.082(5) 0.007(3) 0.021(4) 0.026(3) C50 0.062(4) 0.064(4) 0.064(4) 0.024(3) 0.016(3) 0.028(3) C51 0.033(3) 0.046(3) 0.063(3) 0.029(3) 0.008(2) 0.012(2) C52 0.034(3) 0.049(3) 0.054(3) 0.032(3) 0.005(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O3 2.338(3) . ? Nd1 O8 2.353(3) . ? Nd1 O2 2.362(3) . ? Nd1 O5 2.406(3) . ? Nd1 O1 2.437(3) . ? Nd1 O4 2.448(3) . ? Nd1 O9 2.467(3) . ? Cd2 O7 2.213(3) . ? Cd2 O6 2.225(3) . ? Cd2 N1 2.348(4) . ? Cd2 O10 2.354(3) . ? Cd2 N2 2.400(4) . ? Cd2 O9 2.511(3) . ? N1 C41 1.322(6) . ? N1 C52 1.348(6) . ? N2 C50 1.320(7) . ? N2 C51 1.353(6) . ? O1 C7 1.259(5) . ? O2 C7 1.270(5) 2_766 ? O3 C15 1.257(5) . ? O4 C15 1.250(5) 2_766 ? O5 C23 1.243(5) . ? O6 C23 1.256(6) . ? O7 C31 1.248(5) . ? O8 C31 1.257(5) . ? O9 C39 1.268(5) . ? O10 C39 1.245(5) . ? C1 C2 1.364(7) . ? C1 C6 1.381(7) . ? C2 C3 1.377(8) . ? C3 C4 1.371(8) . ? C3 C8 1.507(7) . ? C4 C5 1.389(8) . ? C5 C6 1.379(7) . ? C6 C7 1.485(6) . ? C7 O2 1.270(5) 2_766 ? C9 C10 1.370(9) . ? C9 C14 1.376(8) . ? C10 C11 1.390(9) . ? C11 C12 1.364(9) . ? C11 C16 1.530(9) . ? C12 C13 1.379(9) . ? C13 C14 1.370(7) . ? C14 C15 1.498(7) . ? C15 O4 1.250(5) 2_766 ? C17 C22 1.376(7) . ? C17 C18 1.381(8) . ? C18 C19 1.355(10) . ? C19 C20 1.368(11) . ? C19 C24 1.530(9) . ? C20 C21 1.388(10) . ? C21 C22 1.395(7) . ? C22 C23 1.496(7) . ? C25 C30 1.377(6) . ? C25 C26 1.396(8) . ? C26 C27 1.362(8) . ? C27 C28 1.369(8) . ? C27 C32 1.528(8) . ? C28 C29 1.378(8) . ? C29 C30 1.372(6) . ? C30 C31 1.493(6) . ? C33 C38 1.371(8) . ? C33 C34 1.395(10) . ? C34 C35 1.360(14) . ? C35 C36 1.345(14) . ? C35 C40 1.534(10) . ? C36 C37 1.394(10) . ? C37 C38 1.371(8) . ? C38 C39 1.479(7) . ? C41 C42 1.398(7) . ? C42 C43 1.324(9) . ? C43 C44 1.395(9) . ? C44 C52 1.425(6) . ? C44 C45 1.439(8) . ? C45 C46 1.316(9) . ? C46 C47 1.430(8) . ? C47 C48 1.401(10) . ? C47 C51 1.401(7) . ? C48 C49 1.338(9) . ? C49 C50 1.381(8) . ? C51 C52 1.437(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Nd1 O8 160.12(11) . . ? O3 Nd1 O2 77.45(12) . . ? O8 Nd1 O2 103.80(12) . . ? O3 Nd1 O5 83.78(12) . . ? O8 Nd1 O5 77.02(12) . . ? O2 Nd1 O5 79.72(12) . . ? O3 Nd1 O1 81.10(11) . . ? O8 Nd1 O1 111.75(11) . . ? O2 Nd1 O1 127.74(10) . . ? O5 Nd1 O1 143.94(12) . . ? O3 Nd1 O4 126.21(11) . . ? O8 Nd1 O4 72.83(11) . . ? O2 Nd1 O4 78.69(12) . . ? O5 Nd1 O4 137.12(12) . . ? O1 Nd1 O4 76.80(12) . . ? O3 Nd1 O9 87.10(11) . . ? O8 Nd1 O9 81.92(11) . . ? O2 Nd1 O9 148.41(12) . . ? O5 Nd1 O9 71.26(12) . . ? O1 Nd1 O9 75.43(10) . . ? O4 Nd1 O9 131.72(11) . . ? O7 Cd2 O6 97.97(14) . . ? O7 Cd2 N1 85.05(12) . . ? O6 Cd2 N1 106.77(13) . . ? O7 Cd2 O10 99.51(13) . . ? O6 Cd2 O10 153.10(13) . . ? N1 Cd2 O10 94.99(12) . . ? O7 Cd2 N2 154.88(13) . . ? O6 Cd2 N2 87.14(13) . . ? N1 Cd2 N2 69.97(14) . . ? O10 Cd2 N2 85.65(13) . . ? O7 Cd2 O9 111.29(11) . . ? O6 Cd2 O9 101.31(12) . . ? N1 Cd2 O9 145.14(12) . . ? O10 Cd2 O9 53.11(11) . . ? N2 Cd2 O9 91.56(12) . . ? C41 N1 C52 118.9(4) . . ? C41 N1 Cd2 123.8(3) . . ? C52 N1 Cd2 117.1(3) . . ? C50 N2 C51 117.8(5) . . ? C50 N2 Cd2 126.3(4) . . ? C51 N2 Cd2 115.9(3) . . ? C7 O1 Nd1 134.0(3) . . ? C7 O2 Nd1 140.5(3) 2_766 . ? C15 O3 Nd1 179.2(3) . . ? C15 O4 Nd1 110.6(3) 2_766 . ? C23 O5 Nd1 150.9(3) . . ? C23 O6 Cd2 117.3(3) . . ? C31 O7 Cd2 113.0(3) . . ? C31 O8 Nd1 168.0(3) . . ? C39 O9 Nd1 138.3(3) . . ? C39 O9 Cd2 88.3(3) . . ? Nd1 O9 Cd2 104.52(12) . . ? C39 O10 Cd2 96.1(3) . . ? C2 C1 C6 120.4(6) . . ? C1 C2 C3 122.7(6) . . ? C4 C3 C2 116.9(6) . . ? C4 C3 C8 120.9(6) . . ? C2 C3 C8 122.2(6) . . ? C3 C4 C5 121.3(6) . . ? C6 C5 C4 120.8(6) . . ? C5 C6 C1 117.8(5) . . ? C5 C6 C7 120.6(5) . . ? C1 C6 C7 121.5(5) . . ? O1 C7 O2 124.0(5) . 2_766 ? O1 C7 C6 119.5(4) . . ? O2 C7 C6 116.4(4) 2_766 . ? C10 C9 C14 121.8(6) . . ? C9 C10 C11 119.7(7) . . ? C12 C11 C10 118.3(6) . . ? C12 C11 C16 121.0(7) . . ? C10 C11 C16 120.7(7) . . ? C11 C12 C13 121.6(6) . . ? C14 C13 C12 120.3(6) . . ? C13 C14 C9 118.2(5) . . ? C13 C14 C15 121.5(5) . . ? C9 C14 C15 120.3(5) . . ? O4 C15 O3 122.7(4) 2_766 . ? O4 C15 C14 118.6(4) 2_766 . ? O3 C15 C14 118.7(4) . . ? C22 C17 C18 121.5(6) . . ? C19 C18 C17 121.0(7) . . ? C18 C19 C20 117.6(7) . . ? C18 C19 C24 122.8(9) . . ? C20 C19 C24 119.6(9) . . ? C19 C20 C21 123.6(7) . . ? C20 C21 C22 117.9(7) . . ? C17 C22 C21 118.4(6) . . ? C17 C22 C23 121.0(5) . . ? C21 C22 C23 120.6(5) . . ? O5 C23 O6 125.8(5) . . ? O5 C23 C22 117.1(5) . . ? O6 C23 C22 117.2(4) . . ? C30 C25 C26 119.1(6) . . ? C27 C26 C25 121.9(6) . . ? C26 C27 C28 117.9(6) . . ? C26 C27 C32 121.4(6) . . ? C28 C27 C32 120.7(6) . . ? C27 C28 C29 121.5(6) . . ? C30 C29 C28 120.4(5) . . ? C29 C30 C25 119.2(5) . . ? C29 C30 C31 119.4(4) . . ? C25 C30 C31 121.3(4) . . ? O7 C31 O8 122.4(5) . . ? O7 C31 C30 117.9(4) . . ? O8 C31 C30 119.6(4) . . ? C38 C33 C34 120.2(8) . . ? C35 C34 C33 120.9(10) . . ? C36 C35 C34 118.5(8) . . ? C36 C35 C40 120.2(12) . . ? C34 C35 C40 121.4(12) . . ? C35 C36 C37 122.1(9) . . ? C38 C37 C36 119.4(8) . . ? C33 C38 C37 118.9(6) . . ? C33 C38 C39 120.1(6) . . ? C37 C38 C39 121.0(5) . . ? O10 C39 O9 120.2(4) . . ? O10 C39 C38 120.4(5) . . ? O9 C39 C38 119.3(5) . . ? N1 C41 C42 121.8(6) . . ? C43 C42 C41 120.6(7) . . ? C42 C43 C44 119.9(6) . . ? C43 C44 C52 117.2(5) . . ? C43 C44 C45 125.4(6) . . ? C52 C44 C45 117.4(6) . . ? C46 C45 C44 123.2(6) . . ? C45 C46 C47 120.6(6) . . ? C48 C47 C51 116.1(6) . . ? C48 C47 C46 124.3(6) . . ? C51 C47 C46 119.6(6) . . ? C49 C48 C47 121.5(6) . . ? C48 C49 C50 118.2(7) . . ? N2 C50 C49 123.8(6) . . ? N2 C51 C47 122.6(5) . . ? N2 C51 C52 117.7(4) . . ? C47 C51 C52 119.7(5) . . ? N1 C52 C44 121.5(5) . . ? N1 C52 C51 119.1(4) . . ? C44 C52 C51 119.4(5) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.581 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.087 data_c70730 _database_code_depnum_ccdc_archive 'CCDC 714920' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H43 Cd N2 O10 Pr' _chemical_formula_weight 1109.19 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' Cd Cd -0.8075 1.2024 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.463(3) _cell_length_b 15.038(3) _cell_length_c 15.120(5) _cell_angle_alpha 114.833(4) _cell_angle_beta 99.215(4) _cell_angle_gamma 110.609(3) _cell_volume 2423.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour Green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6397 _exptl_absorpt_correction_T_max 0.9580 _exptl_absorpt_process_details sadabs _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 'Smart Apex II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13206 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9306 _reflns_number_gt 7033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997a)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9306 _refine_ls_number_parameters 659 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 0.946694(19) 0.456919(18) 0.344923(15) 0.04111(8) Uani 1 1 d . . . Cd1 Cd 0.81965(3) 0.46311(2) 0.09455(2) 0.04761(10) Uani 1 1 d . . . N1 N 0.7801(3) 0.4641(3) -0.0621(2) 0.0480(8) Uani 1 1 d . . . N2 N 0.7060(3) 0.5549(3) 0.0940(3) 0.0539(9) Uani 1 1 d . . . O1 O 0.9437(3) 0.3666(2) 0.1724(2) 0.0626(8) Uani 1 1 d . . . O2 O 0.9075(3) 0.3665(3) 0.0256(2) 0.0628(9) Uani 1 1 d . . . O3 O 0.6666(3) 0.3252(3) 0.0764(2) 0.0702(9) Uani 1 1 d . . . O4 O 0.7479(3) 0.3709(3) 0.2394(2) 0.0699(9) Uani 1 1 d . . . O5 O 0.9754(3) 0.6422(2) 0.1912(2) 0.0650(9) Uani 1 1 d . . . O6 O 0.9142(3) 0.5817(2) 0.2904(2) 0.0578(8) Uani 1 1 d . . . O7 O 0.8704(3) 0.3117(2) 0.3798(2) 0.0633(9) Uani 1 1 d . . . O8 O 1.1203(2) 0.6351(2) 0.4562(2) 0.0545(7) Uani 1 1 d . . . O9 O 1.0999(3) 0.4026(3) 0.3521(2) 0.0669(9) Uani 1 1 d . . . O10 O 0.8890(3) 0.5354(2) 0.4844(2) 0.0590(8) Uani 1 1 d . . . C1 C 1.0146(4) 0.2412(4) -0.0529(4) 0.0560(12) Uani 1 1 d . . . H1A H 0.989(3) 0.269(3) -0.091(3) 0.040(11) Uiso 1 1 d . . . C2 C 1.0638(5) 0.1742(5) -0.0919(5) 0.0754(17) Uani 1 1 d . . . H2A H 1.069(4) 0.161(4) -0.146(4) 0.071(17) Uiso 1 1 d . . . C3 C 1.0995(5) 0.1289(4) -0.0406(5) 0.0798(16) Uani 1 1 d . . . C4 C 1.0862(5) 0.1536(5) 0.0540(5) 0.0833(18) Uani 1 1 d . . . H4A H 1.112(5) 0.125(4) 0.090(4) 0.098(19) Uiso 1 1 d . . . C5 C 1.0387(5) 0.2212(4) 0.0944(4) 0.0636(13) Uani 1 1 d . . . H5A H 1.033(4) 0.241(3) 0.158(3) 0.055(13) Uiso 1 1 d . . . C6 C 1.0019(4) 0.2659(3) 0.0419(3) 0.0461(10) Uani 1 1 d . . . C7 C 0.9474(4) 0.3380(3) 0.0824(3) 0.0448(10) Uani 1 1 d . . . C8 C 1.1517(6) 0.0544(6) -0.0876(6) 0.128(3) Uani 1 1 d . . . H8B H 1.1714 0.0291 -0.0421 0.192 Uiso 1 1 calc R . . H8C H 1.2189 0.0952 -0.0960 0.192 Uiso 1 1 calc R . . H8D H 1.0977 -0.0082 -0.1546 0.192 Uiso 1 1 calc R . . C9 C 0.4870(5) 0.1321(4) 0.0410(5) 0.0793(17) Uani 1 1 d . . . H9A H 0.497(4) 0.138(3) -0.014(3) 0.054(14) Uiso 1 1 d . . . C10 C 0.3974(6) 0.0435(5) 0.0298(8) 0.112(3) Uani 1 1 d . . . H10A H 0.349(5) -0.003(5) -0.035(4) 0.10(2) Uiso 1 1 d . . . C11 C 0.3816(5) 0.0362(6) 0.1138(8) 0.105(2) Uani 1 1 d . . . C12 C 0.4594(6) 0.1193(5) 0.2102(6) 0.0957(19) Uani 1 1 d . . . H12A H 0.4507 0.1162 0.2688 0.115 Uiso 1 1 calc R . . C13 C 0.5511(5) 0.2080(5) 0.2225(5) 0.0739(15) Uani 1 1 d . . . H13A H 0.607(5) 0.266(4) 0.285(4) 0.10(2) Uiso 1 1 d . . . C14 C 0.5664(4) 0.2164(3) 0.1386(3) 0.0513(11) Uani 1 1 d . . . C15 C 0.6674(4) 0.3112(4) 0.1527(3) 0.0525(11) Uani 1 1 d . . . C16 C 0.2803(6) -0.0637(6) 0.0975(8) 0.184(4) Uani 1 1 d . . . H16A H 0.2352 -0.1124 0.0243 0.276 Uiso 1 1 calc R . . H16B H 0.2347 -0.0393 0.1346 0.276 Uiso 1 1 calc R . . H16C H 0.3071 -0.1026 0.1235 0.276 Uiso 1 1 calc R . . C17 C 1.0071(5) 0.7991(5) 0.4600(4) 0.0837(18) Uani 1 1 d . . . H17A H 0.9576 0.7418 0.4653 0.100 Uiso 1 1 calc R . . C18 C 1.0584(7) 0.9075(6) 0.5430(5) 0.117(3) Uani 1 1 d . . . H18A H 1.0423 0.9228 0.6037 0.141 Uiso 1 1 calc R . . C19 C 1.1315(8) 0.9911(6) 0.5365(7) 0.130(4) Uani 1 1 d . . . C20 C 1.1525(7) 0.9703(5) 0.4469(7) 0.125(3) Uani 1 1 d . . . H20A H 1.2002 1.0287 0.4418 0.150 Uiso 1 1 calc R . . C21 C 1.1023(6) 0.8604(4) 0.3612(5) 0.097(2) Uani 1 1 d . . . H21A H 1.1186 0.8458 0.3006 0.117 Uiso 1 1 calc R . . C22 C 1.0299(4) 0.7764(4) 0.3687(3) 0.0627(13) Uani 1 1 d . . . C23 C 0.9720(4) 0.6604(3) 0.2786(3) 0.0501(10) Uani 1 1 d . . . C24 C 1.1910(8) 1.1116(6) 0.6297(6) 0.210(6) Uani 1 1 d . . . H24A H 1.2400 1.1596 0.6116 0.315 Uiso 1 1 calc R . . H24B H 1.2353 1.1160 0.6893 0.315 Uiso 1 1 calc R . . H24C H 1.1347 1.1340 0.6463 0.315 Uiso 1 1 calc R . . C25 C 0.7092(5) 0.0972(4) 0.3071(4) 0.0711(15) Uani 1 1 d . . . H25A H 0.752(5) 0.113(4) 0.263(4) 0.098(19) Uiso 1 1 d . . . C26 C 0.6203(5) -0.0061(5) 0.2696(4) 0.0850(17) Uani 1 1 d . . . H26A H 0.6005 -0.0626 0.2019 0.102 Uiso 1 1 calc R . . C27 C 0.5606(5) -0.0273(4) 0.3296(5) 0.0802(16) Uani 1 1 d . . . C28 C 0.5954(5) 0.0586(5) 0.4300(5) 0.100(2) Uani 1 1 d . . . H28A H 0.5573 0.0464 0.4732 0.120 Uiso 1 1 calc R . . C29 C 0.6837(5) 0.1607(5) 0.4684(4) 0.0753(17) Uani 1 1 d . . . H29A H 0.711(5) 0.208(4) 0.532(4) 0.088(19) Uiso 1 1 d . . . C30 C 0.7420(4) 0.1829(3) 0.4080(3) 0.0506(11) Uani 1 1 d . . . C31 C 0.8375(4) 0.2945(4) 0.4471(3) 0.0489(10) Uani 1 1 d . . . C32 C 0.4621(6) -0.1403(5) 0.2882(5) 0.126(3) Uani 1 1 d . . . H32A H 0.4504 -0.1889 0.2170 0.189 Uiso 1 1 calc R . . H32B H 0.3944 -0.1334 0.2914 0.189 Uiso 1 1 calc R . . H32C H 0.4792 -0.1703 0.3300 0.189 Uiso 1 1 calc R . . C33 C 1.2984(5) 0.4248(6) 0.5607(4) 0.0839(18) Uani 1 1 d . . . H33A H 1.291(4) 0.470(4) 0.614(4) 0.076(17) Uiso 1 1 d . . . C34 C 1.3827(6) 0.3949(7) 0.5763(5) 0.114(3) Uani 1 1 d . . . H34A H 1.430(5) 0.421(4) 0.641(4) 0.095(18) Uiso 1 1 d . . . C35 C 1.4056(7) 0.3323(7) 0.4953(5) 0.133(3) Uani 1 1 d . . . C36 C 1.3440(7) 0.3015(7) 0.3955(5) 0.141(3) Uani 1 1 d . . . H36A H 1.3614 0.2629 0.3390 0.169 Uiso 1 1 calc R . . C37 C 1.2579(6) 0.3276(6) 0.3795(4) 0.102(2) Uani 1 1 d . . . H37A H 1.217(4) 0.307(4) 0.318(4) 0.079(16) Uiso 1 1 d . . . C38 C 1.2341(4) 0.3909(4) 0.4612(3) 0.0625(13) Uani 1 1 d . . . C39 C 1.1421(4) 0.4204(4) 0.4410(3) 0.0557(11) Uani 1 1 d . . . C40 C 1.5026(9) 0.3026(9) 0.5130(6) 0.227(6) Uani 1 1 d . . . H40A H 1.5329 0.3260 0.5854 0.341 Uiso 1 1 calc R . . H40B H 1.5617 0.3396 0.4940 0.341 Uiso 1 1 calc R . . H40C H 1.4735 0.2239 0.4708 0.341 Uiso 1 1 calc R . . C41 C 0.6662(5) 0.5952(4) 0.1674(4) 0.0680(14) Uani 1 1 d . . . H41A H 0.676(4) 0.577(4) 0.223(4) 0.077(16) Uiso 1 1 d . . . C42 C 0.5994(5) 0.6472(5) 0.1618(6) 0.0842(19) Uani 1 1 d . . . H42A H 0.569(4) 0.663(4) 0.208(4) 0.078(18) Uiso 1 1 d . . . C43 C 0.5766(5) 0.6599(4) 0.0800(5) 0.0823(18) Uani 1 1 d . . . H43A H 0.5321 0.6943 0.0756 0.099 Uiso 1 1 calc R . . C44 C 0.6193(4) 0.6220(4) 0.0004(4) 0.0669(14) Uani 1 1 d . . . C45 C 0.6008(6) 0.6348(5) -0.0877(6) 0.092(2) Uani 1 1 d . . . H45A H 0.556(5) 0.672(5) -0.092(4) 0.11(2) Uiso 1 1 d . . . C46 C 0.6411(5) 0.5936(5) -0.1621(6) 0.094(2) Uani 1 1 d . . . H46A H 0.6288 0.6040 -0.2185 0.112 Uiso 1 1 calc R . . C47 C 0.7026(4) 0.5339(4) -0.1573(4) 0.0664(14) Uani 1 1 d . . . C48 C 0.7446(4) 0.4879(5) -0.2342(4) 0.0805(17) Uani 1 1 d . . . H48A H 0.7333 0.4958 -0.2923 0.097 Uiso 1 1 calc R . . C49 C 0.8018(4) 0.4320(4) -0.2246(3) 0.0687(14) Uani 1 1 d . . . H49A H 0.8301 0.4015 -0.2754 0.082 Uiso 1 1 calc R . . C50 C 0.8170(4) 0.4212(4) -0.1370(4) 0.0588(12) Uani 1 1 d . . . H50A H 0.853(3) 0.388(3) -0.130(3) 0.032(11) Uiso 1 1 d . . . C51 C 0.7232(4) 0.5196(3) -0.0716(3) 0.0512(11) Uani 1 1 d . . . C52 C 0.6821(4) 0.5665(3) 0.0099(3) 0.0529(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.04521(15) 0.04898(14) 0.03025(12) 0.02335(10) 0.01532(10) 0.01884(11) Cd1 0.0552(2) 0.05289(19) 0.03336(16) 0.02075(14) 0.01365(14) 0.02683(16) N1 0.051(2) 0.051(2) 0.0404(18) 0.0263(16) 0.0141(16) 0.0203(18) N2 0.053(2) 0.050(2) 0.049(2) 0.0186(17) 0.0162(18) 0.0238(19) O1 0.079(2) 0.074(2) 0.0338(15) 0.0234(15) 0.0235(15) 0.0397(19) O2 0.092(3) 0.081(2) 0.0485(17) 0.0431(17) 0.0335(17) 0.059(2) O3 0.069(2) 0.076(2) 0.067(2) 0.0462(18) 0.0186(17) 0.0265(19) O4 0.044(2) 0.074(2) 0.062(2) 0.0322(17) 0.0068(16) 0.0067(17) O5 0.080(2) 0.0579(19) 0.0470(17) 0.0275(15) 0.0223(16) 0.0221(17) O6 0.068(2) 0.0567(18) 0.0498(17) 0.0324(15) 0.0169(15) 0.0264(17) O7 0.081(2) 0.0583(19) 0.0543(18) 0.0371(16) 0.0297(17) 0.0240(17) O8 0.0533(19) 0.0520(17) 0.0494(17) 0.0299(15) 0.0147(14) 0.0129(15) O9 0.077(2) 0.103(3) 0.0468(17) 0.0432(18) 0.0294(16) 0.058(2) O10 0.069(2) 0.071(2) 0.0512(17) 0.0340(16) 0.0349(16) 0.0387(18) C1 0.065(3) 0.065(3) 0.053(3) 0.035(2) 0.030(2) 0.036(3) C2 0.086(4) 0.085(4) 0.070(4) 0.038(3) 0.051(3) 0.048(3) C3 0.080(4) 0.075(4) 0.095(4) 0.039(3) 0.038(3) 0.049(3) C4 0.094(5) 0.086(4) 0.089(4) 0.050(4) 0.029(4) 0.057(4) C5 0.077(4) 0.064(3) 0.049(3) 0.027(2) 0.018(3) 0.037(3) C6 0.047(3) 0.042(2) 0.040(2) 0.0196(18) 0.0127(19) 0.014(2) C7 0.048(3) 0.042(2) 0.037(2) 0.0186(19) 0.0150(19) 0.017(2) C8 0.138(7) 0.129(6) 0.169(7) 0.074(5) 0.079(6) 0.109(6) C9 0.071(4) 0.059(3) 0.075(4) 0.027(3) -0.003(3) 0.020(3) C10 0.064(5) 0.058(4) 0.140(7) 0.032(4) -0.023(5) 0.007(3) C11 0.049(4) 0.085(5) 0.180(8) 0.082(6) 0.028(5) 0.020(3) C12 0.077(5) 0.101(5) 0.136(6) 0.081(5) 0.056(4) 0.036(4) C13 0.062(4) 0.070(4) 0.081(4) 0.040(3) 0.026(3) 0.021(3) C14 0.040(3) 0.052(3) 0.062(3) 0.032(2) 0.009(2) 0.022(2) C15 0.049(3) 0.059(3) 0.059(3) 0.036(2) 0.019(2) 0.027(2) C16 0.082(6) 0.115(6) 0.325(13) 0.132(8) 0.049(7) 0.005(5) C17 0.106(5) 0.080(4) 0.051(3) 0.015(3) 0.010(3) 0.061(4) C18 0.147(7) 0.106(5) 0.062(4) 0.006(4) 0.000(4) 0.085(6) C19 0.132(7) 0.067(4) 0.104(6) 0.000(5) -0.045(5) 0.052(5) C20 0.115(6) 0.057(4) 0.135(7) 0.035(5) -0.020(5) 0.018(4) C21 0.103(5) 0.056(3) 0.089(4) 0.031(3) -0.003(4) 0.018(3) C22 0.072(3) 0.047(3) 0.047(3) 0.014(2) -0.004(2) 0.029(3) C23 0.053(3) 0.053(3) 0.047(2) 0.028(2) 0.014(2) 0.026(2) C24 0.209(10) 0.085(5) 0.150(7) -0.045(5) -0.090(7) 0.081(6) C25 0.078(4) 0.067(3) 0.050(3) 0.028(3) 0.021(3) 0.019(3) C26 0.092(5) 0.062(3) 0.057(3) 0.015(3) 0.010(3) 0.018(3) C27 0.067(4) 0.063(3) 0.082(4) 0.033(3) 0.018(3) 0.012(3) C28 0.105(5) 0.079(4) 0.086(4) 0.041(4) 0.052(4) 0.009(4) C29 0.077(4) 0.063(3) 0.056(3) 0.023(3) 0.032(3) 0.009(3) C30 0.050(3) 0.050(2) 0.045(2) 0.025(2) 0.011(2) 0.017(2) C31 0.044(3) 0.056(3) 0.052(3) 0.034(2) 0.016(2) 0.023(2) C32 0.104(6) 0.061(4) 0.139(6) 0.028(4) 0.028(5) 0.002(4) C33 0.090(5) 0.116(5) 0.044(3) 0.032(3) 0.019(3) 0.061(4) C34 0.108(6) 0.182(8) 0.059(4) 0.047(4) 0.014(4) 0.100(6) C35 0.132(6) 0.208(8) 0.077(4) 0.049(5) 0.017(4) 0.136(7) C36 0.143(7) 0.224(9) 0.072(4) 0.042(5) 0.032(4) 0.149(7) C37 0.118(6) 0.163(6) 0.048(3) 0.040(4) 0.024(3) 0.109(5) C38 0.071(3) 0.083(3) 0.039(2) 0.028(2) 0.021(2) 0.045(3) C39 0.061(3) 0.065(3) 0.051(3) 0.032(2) 0.027(2) 0.034(3) C40 0.239(12) 0.347(14) 0.128(7) 0.068(8) 0.022(7) 0.255(12) C41 0.062(3) 0.065(3) 0.058(3) 0.017(3) 0.021(3) 0.030(3) C42 0.069(4) 0.066(4) 0.079(4) 0.009(3) 0.027(4) 0.029(3) C43 0.053(3) 0.046(3) 0.114(5) 0.020(3) 0.016(3) 0.021(3) C44 0.046(3) 0.048(3) 0.090(4) 0.035(3) 0.007(3) 0.015(2) C45 0.074(4) 0.083(4) 0.128(6) 0.069(4) 0.015(4) 0.036(4) C46 0.079(4) 0.110(5) 0.110(5) 0.086(4) 0.014(4) 0.036(4) C47 0.048(3) 0.079(3) 0.068(3) 0.051(3) 0.008(2) 0.014(3) C48 0.060(4) 0.107(4) 0.071(3) 0.065(3) 0.013(3) 0.018(3) C49 0.059(3) 0.086(4) 0.046(3) 0.035(3) 0.020(2) 0.018(3) C50 0.058(3) 0.067(3) 0.049(3) 0.030(2) 0.023(2) 0.025(3) C51 0.042(3) 0.051(2) 0.051(2) 0.031(2) 0.007(2) 0.011(2) C52 0.043(3) 0.045(2) 0.059(3) 0.027(2) 0.008(2) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O10 2.350(3) . ? Pr1 O1 2.367(3) . ? Pr1 O7 2.379(3) . ? Pr1 O4 2.417(3) . ? Pr1 O8 2.453(3) . ? Pr1 O9 2.475(3) . ? Pr1 O6 2.481(3) . ? Cd1 O2 2.220(3) . ? Cd1 O3 2.227(3) . ? Cd1 O5 2.350(3) . ? Cd1 N1 2.350(3) . ? Cd1 N2 2.396(4) . ? Cd1 O6 2.515(3) . ? N1 C50 1.318(6) . ? N1 C51 1.349(5) . ? N2 C41 1.319(6) . ? N2 C52 1.358(5) . ? O1 C7 1.258(4) . ? O2 C7 1.238(4) . ? O3 C15 1.256(5) . ? O4 C15 1.253(5) . ? O5 C23 1.243(5) . ? O6 C23 1.269(5) . ? O7 C31 1.260(5) . ? O8 C31 1.262(5) 2_766 ? O9 C39 1.244(5) . ? O10 C39 1.269(5) 2_766 ? C1 C2 1.377(7) . ? C1 C6 1.378(5) . ? C2 C3 1.361(8) . ? C3 C4 1.378(8) . ? C3 C8 1.516(7) . ? C4 C5 1.369(7) . ? C5 C6 1.373(6) . ? C6 C7 1.494(6) . ? C9 C10 1.367(9) . ? C9 C14 1.377(6) . ? C10 C11 1.363(11) . ? C11 C12 1.357(9) . ? C11 C16 1.523(9) . ? C12 C13 1.378(7) . ? C13 C14 1.366(7) . ? C14 C15 1.488(6) . ? C17 C18 1.386(8) . ? C17 C22 1.389(7) . ? C18 C19 1.350(12) . ? C19 C20 1.357(12) . ? C19 C24 1.543(8) . ? C20 C21 1.415(9) . ? C21 C22 1.359(8) . ? C22 C23 1.488(6) . ? C25 C26 1.378(7) . ? C25 C30 1.384(6) . ? C26 C27 1.366(8) . ? C27 C28 1.375(7) . ? C27 C32 1.514(7) . ? C28 C29 1.361(7) . ? C29 C30 1.366(6) . ? C30 C31 1.491(6) . ? C31 O8 1.262(5) 2_766 ? C33 C38 1.378(6) . ? C33 C34 1.382(8) . ? C34 C35 1.356(9) . ? C35 C36 1.386(8) . ? C35 C40 1.540(9) . ? C36 C37 1.366(8) . ? C37 C38 1.373(7) . ? C38 C39 1.485(6) . ? C39 O10 1.269(5) 2_766 ? C41 C42 1.398(8) . ? C42 C43 1.334(8) . ? C43 C44 1.408(8) . ? C44 C52 1.410(6) . ? C44 C45 1.420(8) . ? C45 C46 1.337(9) . ? C46 C47 1.433(8) . ? C47 C48 1.400(7) . ? C47 C51 1.402(6) . ? C48 C49 1.357(7) . ? C49 C50 1.392(6) . ? C51 C52 1.444(6) . ? 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 O10 Pr1 O1 160.44(11) . . ? O10 Pr1 O7 77.13(10) . . ? O1 Pr1 O7 104.47(11) . . ? O10 Pr1 O4 84.07(11) . . ? O1 Pr1 O4 77.12(11) . . ? O7 Pr1 O4 80.05(11) . . ? O10 Pr1 O8 81.34(11) . . ? O1 Pr1 O8 111.02(11) . . ? O7 Pr1 O8 127.73(10) . . ? O4 Pr1 O8 143.86(10) . . ? O10 Pr1 O9 126.18(10) . . ? O1 Pr1 O9 72.64(10) . . ? O7 Pr1 O9 78.87(11) . . ? O4 Pr1 O9 137.09(11) . . ? O8 Pr1 O9 76.68(11) . . ? O10 Pr1 O6 87.01(10) . . ? O1 Pr1 O6 81.81(10) . . ? O7 Pr1 O6 148.08(11) . . ? O4 Pr1 O6 70.79(11) . . ? O8 Pr1 O6 75.57(10) . . ? O9 Pr1 O6 131.92(11) . . ? O2 Cd1 O3 98.11(13) . . ? O2 Cd1 O5 99.49(12) . . ? O3 Cd1 O5 153.10(11) . . ? O2 Cd1 N1 84.93(11) . . ? O3 Cd1 N1 106.98(11) . . ? O5 Cd1 N1 94.72(11) . . ? O2 Cd1 N2 154.94(11) . . ? O3 Cd1 N2 87.23(13) . . ? O5 Cd1 N2 85.39(12) . . ? N1 Cd1 N2 70.13(12) . . ? O2 Cd1 O6 111.26(10) . . ? O3 Cd1 O6 101.26(11) . . ? O5 Cd1 O6 53.20(10) . . ? N1 Cd1 O6 145.04(10) . . ? N2 Cd1 O6 91.43(11) . . ? C50 N1 C51 118.3(4) . . ? C50 N1 Cd1 124.3(3) . . ? C51 N1 Cd1 117.2(3) . . ? C41 N2 C52 118.0(4) . . ? C41 N2 Cd1 126.1(3) . . ? C52 N2 Cd1 115.9(3) . . ? C7 O1 Pr1 168.0(3) . . ? C7 O2 Cd1 113.1(3) . . ? C15 O3 Cd1 118.0(3) . . ? C15 O4 Pr1 151.5(3) . . ? C23 O5 Cd1 96.3(3) . . ? C23 O6 Pr1 137.9(3) . . ? C23 O6 Cd1 87.9(2) . . ? Pr1 O6 Cd1 104.45(10) . . ? C31 O7 Pr1 140.7(3) . . ? C31 O8 Pr1 133.3(3) 2_766 . ? C39 O9 Pr1 110.2(3) . . ? C39 O10 Pr1 178.5(3) 2_766 . ? C2 C1 C6 120.1(5) . . ? C3 C2 C1 122.2(5) . . ? C2 C3 C4 117.4(5) . . ? C2 C3 C8 120.1(6) . . ? C4 C3 C8 122.4(6) . . ? C5 C4 C3 121.0(5) . . ? C4 C5 C6 121.4(5) . . ? C5 C6 C1 117.9(4) . . ? C5 C6 C7 122.9(4) . . ? C1 C6 C7 119.2(4) . . ? O2 C7 O1 122.9(4) . . ? O2 C7 C6 118.5(3) . . ? O1 C7 C6 118.6(4) . . ? C10 C9 C14 120.6(7) . . ? C11 C10 C9 121.8(7) . . ? C12 C11 C10 117.8(6) . . ? C12 C11 C16 122.2(9) . . ? C10 C11 C16 120.0(8) . . ? C11 C12 C13 121.0(6) . . ? C14 C13 C12 121.4(6) . . ? C13 C14 C9 117.4(5) . . ? C13 C14 C15 120.9(4) . . ? C9 C14 C15 121.7(5) . . ? O4 C15 O3 124.5(4) . . ? O4 C15 C14 117.9(4) . . ? O3 C15 C14 117.6(4) . . ? C18 C17 C22 119.7(7) . . ? C19 C18 C17 120.7(8) . . ? C18 C19 C20 120.2(7) . . ? C18 C19 C24 120.8(10) . . ? C20 C19 C24 119.0(10) . . ? C19 C20 C21 120.5(8) . . ? C22 C21 C20 119.0(7) . . ? C21 C22 C17 119.9(5) . . ? C21 C22 C23 120.5(5) . . ? C17 C22 C23 119.6(5) . . ? O5 C23 O6 120.7(4) . . ? O5 C23 C22 119.7(4) . . ? O6 C23 C22 119.5(4) . . ? C26 C25 C30 120.8(5) . . ? C27 C26 C25 121.6(5) . . ? C26 C27 C28 116.8(5) . . ? C26 C27 C32 121.7(6) . . ? C28 C27 C32 121.6(6) . . ? C29 C28 C27 122.3(5) . . ? C28 C29 C30 121.1(5) . . ? C29 C30 C25 117.4(5) . . ? C29 C30 C31 122.3(4) . . ? C25 C30 C31 120.3(4) . . ? O7 C31 O8 124.4(4) . 2_766 ? O7 C31 C30 116.7(4) . . ? O8 C31 C30 118.9(4) 2_766 . ? C38 C33 C34 120.6(6) . . ? C35 C34 C33 121.6(6) . . ? C34 C35 C36 117.9(6) . . ? C34 C35 C40 121.6(6) . . ? C36 C35 C40 120.4(7) . . ? C37 C36 C35 120.5(6) . . ? C36 C37 C38 121.8(5) . . ? C37 C38 C33 117.5(5) . . ? C37 C38 C39 120.3(4) . . ? C33 C38 C39 122.2(5) . . ? O9 C39 O10 122.6(4) . 2_766 ? O9 C39 C38 118.8(4) . . ? O10 C39 C38 118.6(4) 2_766 . ? N2 C41 C42 123.2(6) . . ? C43 C42 C41 119.1(6) . . ? C42 C43 C44 120.7(6) . . ? C43 C44 C52 116.6(5) . . ? C43 C44 C45 123.9(6) . . ? C52 C44 C45 119.5(6) . . ? C46 C45 C44 120.6(6) . . ? C45 C46 C47 121.9(6) . . ? C48 C47 C51 116.8(5) . . ? C48 C47 C46 123.8(5) . . ? C51 C47 C46 119.4(5) . . ? C49 C48 C47 120.6(5) . . ? C48 C49 C50 118.4(5) . . ? N1 C50 C49 123.3(5) . . ? N1 C51 C47 122.7(4) . . ? N1 C51 C52 118.8(4) . . ? C47 C51 C52 118.6(4) . . ? N2 C52 C44 122.4(5) . . ? N2 C52 C51 117.8(4) . . ? C44 C52 C51 119.9(4) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.586 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.079 data_w0445 _database_code_depnum_ccdc_archive 'CCDC 714921' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H43 Cd N2 O10 Sm' _chemical_formula_weight 1118.63 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' Cd Cd -0.8075 1.2024 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.407(3) _cell_length_b 15.041(3) _cell_length_c 15.050(3) _cell_angle_alpha 114.42(3) _cell_angle_beta 99.53(3) _cell_angle_gamma 110.75(3) _cell_volume 2404.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1118 _exptl_absorpt_coefficient_mu 1.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8475 _exptl_absorpt_correction_T_max 0.8475 _exptl_absorpt_process_details sadabs _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 'Smart Apex II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21904 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.46 _reflns_number_total 10425 _reflns_number_gt 7941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997a)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^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 geog _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10425 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.110 _refine_ls_shift/su_mean 0.016 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 0.446774(17) 0.958100(17) 0.344939(14) 0.03644(7) Uani 1 1 d . . . Cd1 Cd 0.32023(3) 0.96458(3) 0.09520(2) 0.04433(9) Uani 1 1 d . . . N1 N 0.2799(3) 0.9649(3) -0.0624(3) 0.0454(8) Uani 1 1 d . . . N2 N 0.2060(3) 1.0561(3) 0.0941(3) 0.0519(9) Uani 1 1 d . . . O1 O 0.2502(3) 0.8723(3) 0.2419(2) 0.0631(9) Uani 1 1 d . . . O2 O 0.1677(3) 0.8272(3) 0.0782(3) 0.0643(9) Uani 1 1 d . . . O3 O 0.4160(3) 1.0807(2) 0.2901(2) 0.0509(7) Uani 1 1 d . . . O4 O 0.4772(3) 1.1433(3) 0.1922(2) 0.0631(9) Uani 1 1 d . . . O5 O 0.4440(3) 0.8686(3) 0.1755(2) 0.0590(8) Uani 1 1 d . . . O6 O 0.4092(3) 0.8691(3) 0.0278(2) 0.0561(8) Uani 1 1 d . . . O7 O 0.3868(3) 1.0332(3) 0.4794(2) 0.0545(8) Uani 1 1 d . . . O8 O 0.6001(3) 0.9090(3) 0.3566(2) 0.0563(8) Uani 1 1 d . . . O9 O 0.6175(2) 1.1332(2) 0.4566(2) 0.0486(7) Uani 1 1 d . . . O10 O 0.3735(3) 0.8149(3) 0.3791(2) 0.0554(8) Uani 1 1 d . . . C1 C 0.1692(4) 0.8131(4) 0.1549(4) 0.0476(10) Uani 1 1 d . . . C2 C 0.0674(3) 0.7179(3) 0.1416(3) 0.0471(10) Uani 1 1 d . . . C3 C -0.0119(4) 0.6336(4) 0.0420(4) 0.0718(15) Uani 1 1 d . . . H3A H -0.0038 0.6380 -0.0165 0.086 Uiso 1 1 calc R . . C4 C -0.1017(5) 0.5443(5) 0.0299(7) 0.103(3) Uani 1 1 d . . . H4A H -0.1528 0.4872 -0.0373 0.123 Uiso 1 1 calc R . . C5 C -0.1187(5) 0.5366(6) 0.1162(8) 0.098(2) Uani 1 1 d . . . C6 C -0.0406(5) 0.6197(6) 0.2125(6) 0.091(2) Uani 1 1 d . . . H6A H -0.0494 0.6163 0.2712 0.109 Uiso 1 1 calc R . . C7 C 0.0516(4) 0.7093(5) 0.2257(4) 0.0673(14) Uani 1 1 d . . . H7B H 0.1040 0.7648 0.2929 0.081 Uiso 1 1 calc R . . C8 C -0.2184(6) 0.4368(7) 0.1030(10) 0.178(5) Uani 1 1 d . . . H8A H -0.2152 0.4461 0.1706 0.266 Uiso 1 1 calc R . . H8B H -0.2135 0.3709 0.0619 0.266 Uiso 1 1 calc R . . H8C H -0.2895 0.4304 0.0680 0.266 Uiso 1 1 calc R . . C9 C 0.4732(4) 1.1611(4) 0.2796(3) 0.0447(9) Uani 1 1 d . . . C10 C 0.5299(4) 1.2757(4) 0.3707(4) 0.0582(13) Uani 1 1 d . . . C11 C 0.6034(5) 1.3617(5) 0.3653(5) 0.089(2) Uani 1 1 d . . . H11A H 0.6203 1.3482 0.3050 0.107 Uiso 1 1 calc R . . C12 C 0.6534(7) 1.4699(5) 0.4500(7) 0.118(3) Uani 1 1 d . . . H12A H 0.7033 1.5281 0.4457 0.141 Uiso 1 1 calc R . . C13 C 0.6298(8) 1.4905(6) 0.5376(7) 0.121(4) Uani 1 1 d . . . C14 C 0.5567(8) 1.4062(7) 0.5436(5) 0.113(3) Uani 1 1 d . . . H14A H 0.5402 1.4211 0.6043 0.136 Uiso 1 1 calc R . . C15 C 0.5050(5) 1.2965(5) 0.4601(4) 0.0771(17) Uani 1 1 d . . . H15A H 0.4549 1.2389 0.4651 0.093 Uiso 1 1 calc R . . C16 C 0.6856(9) 1.6086(6) 0.6296(7) 0.195(6) Uani 1 1 d . . . H16A H 0.6604 1.6090 0.6857 0.292 Uiso 1 1 calc R . . H16B H 0.6643 1.6530 0.6077 0.292 Uiso 1 1 calc R . . H16C H 0.7675 1.6383 0.6532 0.292 Uiso 1 1 calc R . . C17 C 0.4482(3) 0.8399(3) 0.0854(3) 0.0416(9) Uani 1 1 d . . . C18 C 0.5026(3) 0.7686(3) 0.0452(3) 0.0433(9) Uani 1 1 d . . . C19 C 0.5392(4) 0.7244(4) 0.0998(4) 0.0620(13) Uani 1 1 d . . . H19A H 0.5319 0.7403 0.1643 0.074 Uiso 1 1 calc R . . C20 C 0.5867(5) 0.6561(5) 0.0579(5) 0.0793(17) Uani 1 1 d . . . H20A H 0.6105 0.6260 0.0946 0.095 Uiso 1 1 calc R . . C21 C 0.5996(5) 0.6317(5) -0.0382(5) 0.0726(15) Uani 1 1 d . . . C22 C 0.5629(5) 0.6775(4) -0.0900(4) 0.0674(14) Uani 1 1 d . . . H22A H 0.5713 0.6629 -0.1539 0.081 Uiso 1 1 calc R . . C23 C 0.5149(4) 0.7434(4) -0.0511(4) 0.0522(11) Uani 1 1 d . . . H23A H 0.4900 0.7721 -0.0890 0.063 Uiso 1 1 calc R . . C24 C 0.6545(7) 0.5596(7) -0.0828(7) 0.120(3) Uani 1 1 d . . . H24A H 0.6746 0.5350 -0.0362 0.181 Uiso 1 1 calc R . . H24B H 0.7223 0.6015 -0.0902 0.181 Uiso 1 1 calc R . . H24C H 0.6014 0.4965 -0.1501 0.181 Uiso 1 1 calc R . . C25 C 0.6427(4) 0.9238(4) 0.4449(3) 0.0489(10) Uani 1 1 d . . . C26 C 0.7343(4) 0.8922(4) 0.4629(3) 0.0562(12) Uani 1 1 d . . . C27 C 0.7559(5) 0.8299(6) 0.3799(4) 0.089(2) Uani 1 1 d . . . H27A H 0.7135 0.8080 0.3123 0.106 Uiso 1 1 calc R . . C28 C 0.8396(7) 0.7994(8) 0.3949(5) 0.132(4) Uani 1 1 d . . . H28A H 0.8539 0.7577 0.3377 0.159 Uiso 1 1 calc R . . C29 C 0.9030(7) 0.8304(8) 0.4951(5) 0.123(3) Uani 1 1 d . . . C30 C 0.8819(6) 0.8929(7) 0.5762(5) 0.107(3) Uani 1 1 d . . . H30A H 0.9249 0.9155 0.6439 0.128 Uiso 1 1 calc R . . C31 C 0.7988(5) 0.9242(5) 0.5623(4) 0.0775(17) Uani 1 1 d . . . H31A H 0.7860 0.9671 0.6200 0.093 Uiso 1 1 calc R . . C32 C 0.9917(9) 0.7908(11) 0.5106(7) 0.221(7) Uani 1 1 d . . . H32A H 1.0263 0.8179 0.5839 0.331 Uiso 1 1 calc R . . H32B H 1.0497 0.8183 0.4853 0.331 Uiso 1 1 calc R . . H32C H 0.9546 0.7114 0.4725 0.331 Uiso 1 1 calc R . . C33 C 0.6589(4) 1.2031(4) 0.5535(3) 0.0455(10) Uani 1 1 d . . . C34 C 0.7557(4) 1.3157(4) 0.5928(3) 0.0457(10) Uani 1 1 d . . . C35 C 0.8150(4) 1.3368(4) 0.5317(4) 0.0645(14) Uani 1 1 d . . . H35A H 0.7943 1.2810 0.4635 0.077 Uiso 1 1 calc R . . C36 C 0.9041(5) 1.4393(4) 0.5704(5) 0.0834(19) Uani 1 1 d . . . H36A H 0.9440 1.4511 0.5280 0.100 Uiso 1 1 calc R . . C37 C 0.9367(5) 1.5252(4) 0.6695(5) 0.0734(15) Uani 1 1 d . . . C38 C 0.8761(5) 1.5047(4) 0.7297(4) 0.0744(15) Uani 1 1 d . . . H38A H 0.8956 1.5618 0.7970 0.089 Uiso 1 1 calc R . . C39 C 0.7868(5) 1.4017(4) 0.6931(4) 0.0646(13) Uani 1 1 d . . . H39A H 0.7474 1.3898 0.7359 0.077 Uiso 1 1 calc R . . C40 C 1.0348(6) 1.6387(5) 0.7108(6) 0.109(3) Uani 1 1 d . . . H40A H 1.0441 1.6878 0.7809 0.164 Uiso 1 1 calc R . . H40B H 1.0185 1.6669 0.6666 0.164 Uiso 1 1 calc R . . H40C H 1.1041 1.6333 0.7111 0.164 Uiso 1 1 calc R . . C41 C 0.3155(4) 0.9212(4) -0.1379(3) 0.0531(11) Uani 1 1 d . . . H41A H 0.3539 0.8822 -0.1312 0.064 Uiso 1 1 calc R . . C42 C 0.2989(4) 0.9301(5) -0.2269(4) 0.0660(14) Uani 1 1 d . . . H42A H 0.3261 0.8985 -0.2780 0.079 Uiso 1 1 calc R . . C43 C 0.2422(5) 0.9860(5) -0.2373(4) 0.0747(17) Uani 1 1 d . . . H43A H 0.2303 0.9930 -0.2962 0.090 Uiso 1 1 calc R . . C44 C 0.2014(4) 1.0332(5) -0.1601(4) 0.0649(14) Uani 1 1 d . . . C45 C 0.1401(5) 1.0918(6) -0.1658(6) 0.088(2) Uani 1 1 d . . . H45A H 0.1278 1.1025 -0.2224 0.106 Uiso 1 1 calc R . . C46 C 0.0991(5) 1.1322(5) -0.0908(6) 0.0838(19) Uani 1 1 d . . . H46A H 0.0576 1.1686 -0.0978 0.101 Uiso 1 1 calc R . . C47 C 0.1179(4) 1.1207(4) -0.0015(5) 0.0624(14) Uani 1 1 d . . . C48 C 0.0761(5) 1.1598(4) 0.0792(6) 0.0790(18) Uani 1 1 d . . . H48A H 0.0309 1.1935 0.0741 0.095 Uiso 1 1 calc R . . C49 C 0.1009(5) 1.1488(4) 0.1631(5) 0.0761(16) Uani 1 1 d . . . H49A H 0.0741 1.1753 0.2165 0.091 Uiso 1 1 calc R . . C50 C 0.1672(4) 1.0971(4) 0.1682(4) 0.0650(13) Uani 1 1 d . . . H50A H 0.1854 1.0909 0.2271 0.078 Uiso 1 1 calc R . . C51 C 0.1815(3) 1.0666(3) 0.0092(4) 0.0494(11) Uani 1 1 d . . . C52 C 0.2228(3) 1.0210(4) -0.0719(3) 0.0485(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.04053(12) 0.04330(12) 0.02833(10) 0.02203(9) 0.01396(8) 0.01751(9) Cd1 0.05176(18) 0.05015(18) 0.03272(15) 0.02127(14) 0.01309(14) 0.02659(16) N1 0.0470(19) 0.050(2) 0.0379(17) 0.0248(16) 0.0130(16) 0.0198(17) N2 0.050(2) 0.048(2) 0.051(2) 0.0215(18) 0.0142(18) 0.0236(18) O1 0.0410(17) 0.068(2) 0.0541(19) 0.0275(18) 0.0044(16) 0.0094(16) O2 0.061(2) 0.069(2) 0.062(2) 0.0430(19) 0.0144(17) 0.0218(18) O3 0.0578(18) 0.0458(16) 0.0441(16) 0.0246(14) 0.0109(14) 0.0209(15) O4 0.079(2) 0.0577(19) 0.0456(17) 0.0293(16) 0.0225(17) 0.0217(18) O5 0.074(2) 0.075(2) 0.0336(15) 0.0265(15) 0.0225(15) 0.0404(19) O6 0.081(2) 0.070(2) 0.0448(16) 0.0361(16) 0.0305(16) 0.0526(19) O7 0.0601(19) 0.066(2) 0.0466(16) 0.0295(16) 0.0291(15) 0.0340(17) O8 0.0613(19) 0.082(2) 0.0445(16) 0.0378(17) 0.0242(15) 0.0441(18) O9 0.0479(16) 0.0485(17) 0.0468(16) 0.0295(15) 0.0133(14) 0.0159(14) O10 0.068(2) 0.0528(18) 0.0542(17) 0.0363(16) 0.0270(16) 0.0238(16) C1 0.040(2) 0.048(2) 0.057(3) 0.028(2) 0.017(2) 0.022(2) C2 0.036(2) 0.043(2) 0.055(2) 0.023(2) 0.007(2) 0.0178(19) C3 0.059(3) 0.055(3) 0.068(3) 0.023(3) -0.003(3) 0.016(3) C4 0.055(3) 0.049(3) 0.124(6) 0.017(4) -0.026(4) 0.006(3) C5 0.051(3) 0.077(4) 0.166(8) 0.075(5) 0.026(4) 0.020(3) C6 0.071(4) 0.094(5) 0.131(6) 0.077(5) 0.048(4) 0.034(4) C7 0.051(3) 0.070(3) 0.072(3) 0.039(3) 0.018(3) 0.018(3) C8 0.077(5) 0.108(6) 0.319(15) 0.127(9) 0.048(7) 0.006(5) C9 0.049(2) 0.048(2) 0.045(2) 0.028(2) 0.014(2) 0.028(2) C10 0.065(3) 0.039(2) 0.050(3) 0.015(2) -0.003(2) 0.024(2) C11 0.088(4) 0.057(3) 0.093(4) 0.035(3) 0.004(4) 0.021(3) C12 0.109(6) 0.044(4) 0.120(6) 0.021(4) -0.022(5) 0.012(4) C13 0.124(7) 0.057(4) 0.102(6) 0.002(4) -0.039(5) 0.048(5) C14 0.154(7) 0.121(6) 0.052(3) 0.011(4) 0.006(4) 0.106(6) C15 0.099(4) 0.077(4) 0.050(3) 0.019(3) 0.011(3) 0.060(4) C16 0.204(10) 0.075(5) 0.139(7) -0.039(5) -0.082(7) 0.078(6) C17 0.043(2) 0.040(2) 0.0321(19) 0.0153(17) 0.0130(18) 0.0149(19) C18 0.044(2) 0.042(2) 0.042(2) 0.0199(18) 0.0137(19) 0.0202(19) C19 0.074(3) 0.067(3) 0.051(3) 0.033(2) 0.017(3) 0.038(3) C20 0.094(4) 0.081(4) 0.086(4) 0.047(3) 0.027(4) 0.063(4) C21 0.069(3) 0.064(3) 0.086(4) 0.029(3) 0.035(3) 0.040(3) C22 0.082(4) 0.066(3) 0.069(3) 0.035(3) 0.045(3) 0.041(3) C23 0.063(3) 0.057(3) 0.053(2) 0.033(2) 0.032(2) 0.036(2) C24 0.131(6) 0.122(6) 0.170(8) 0.081(6) 0.085(6) 0.101(6) C25 0.052(2) 0.062(3) 0.041(2) 0.029(2) 0.023(2) 0.029(2) C26 0.063(3) 0.080(3) 0.041(2) 0.031(2) 0.023(2) 0.048(3) C27 0.099(4) 0.132(6) 0.045(3) 0.030(3) 0.020(3) 0.085(4) C28 0.140(6) 0.210(9) 0.062(4) 0.037(5) 0.026(4) 0.143(7) C29 0.121(6) 0.185(8) 0.075(4) 0.043(5) 0.016(4) 0.122(6) C30 0.108(5) 0.175(8) 0.055(3) 0.045(4) 0.021(3) 0.105(6) C31 0.086(4) 0.114(5) 0.043(3) 0.033(3) 0.023(3) 0.067(4) C32 0.226(11) 0.337(16) 0.113(7) 0.048(9) 0.013(7) 0.248(13) C33 0.047(2) 0.051(2) 0.043(2) 0.030(2) 0.015(2) 0.021(2) C34 0.047(2) 0.046(2) 0.045(2) 0.026(2) 0.012(2) 0.021(2) C35 0.064(3) 0.053(3) 0.053(3) 0.023(2) 0.025(2) 0.007(2) C36 0.079(4) 0.062(3) 0.074(4) 0.032(3) 0.036(3) -0.001(3) C37 0.058(3) 0.051(3) 0.077(4) 0.028(3) 0.014(3) 0.003(3) C38 0.079(4) 0.051(3) 0.055(3) 0.016(2) 0.009(3) 0.013(3) C39 0.073(3) 0.063(3) 0.051(3) 0.029(2) 0.025(3) 0.025(3) C40 0.089(5) 0.059(4) 0.120(6) 0.032(4) 0.024(4) -0.003(3) C41 0.058(3) 0.057(3) 0.044(2) 0.026(2) 0.021(2) 0.025(2) C42 0.057(3) 0.077(3) 0.045(3) 0.032(3) 0.016(2) 0.012(3) C43 0.065(3) 0.099(4) 0.056(3) 0.056(3) 0.015(3) 0.020(3) C44 0.049(3) 0.079(4) 0.074(3) 0.059(3) 0.014(3) 0.020(3) C45 0.071(4) 0.117(5) 0.113(5) 0.094(5) 0.025(4) 0.042(4) C46 0.059(3) 0.070(4) 0.126(5) 0.064(4) 0.010(4) 0.027(3) C47 0.042(2) 0.041(2) 0.089(4) 0.030(3) 0.008(3) 0.015(2) C48 0.056(3) 0.049(3) 0.117(5) 0.031(3) 0.022(3) 0.028(3) C49 0.067(3) 0.058(3) 0.083(4) 0.016(3) 0.029(3) 0.031(3) C50 0.064(3) 0.061(3) 0.057(3) 0.017(2) 0.023(3) 0.033(3) C51 0.037(2) 0.039(2) 0.059(3) 0.024(2) 0.007(2) 0.0112(19) C52 0.038(2) 0.043(2) 0.052(2) 0.028(2) 0.003(2) 0.0077(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O7 2.304(3) . ? Sm1 O5 2.326(3) . ? Sm1 O10 2.335(3) . ? Sm1 O1 2.366(3) . ? Sm1 O9 2.407(3) . ? Sm1 O8 2.422(3) . ? Sm1 O3 2.436(3) . ? Cd1 O2 2.217(3) . ? Cd1 O6 2.219(3) . ? Cd1 O4 2.348(4) . ? Cd1 N1 2.347(3) . ? Cd1 N2 2.396(4) . ? Cd1 O3 2.497(3) . ? N1 C41 1.317(6) . ? N1 C52 1.356(6) . ? N2 C50 1.322(6) . ? N2 C51 1.354(6) . ? O1 C1 1.251(5) . ? O2 C1 1.255(5) . ? O3 C9 1.272(5) . ? O4 C9 1.244(5) . ? O5 C17 1.261(5) . ? O6 C17 1.243(5) . ? O7 C25 1.262(5) 2_676 ? O8 C25 1.248(5) . ? O9 C33 1.262(5) . ? O10 C33 1.258(5) 2_676 ? C1 C2 1.498(6) . ? C2 C7 1.366(7) . ? C2 C3 1.389(7) . ? C3 C4 1.367(9) . ? C4 C5 1.399(11) . ? C5 C6 1.353(10) . ? C5 C8 1.524(9) . ? C6 C7 1.379(7) . ? C9 C10 1.484(6) . ? C10 C11 1.364(8) . ? C10 C15 1.376(8) . ? C11 C12 1.398(9) . ? C12 C13 1.344(13) . ? C13 C14 1.348(12) . ? C13 C16 1.521(9) . ? C14 C15 1.404(9) . ? C17 C18 1.487(6) . ? C18 C19 1.380(6) . ? C18 C23 1.394(6) . ? C19 C20 1.385(7) . ? C20 C21 1.394(8) . ? C21 C22 1.371(8) . ? C21 C24 1.516(8) . ? C22 C23 1.355(7) . ? C25 O7 1.262(5) 2_676 ? C25 C26 1.490(6) . ? C26 C27 1.367(7) . ? C26 C31 1.377(6) . ? C27 C28 1.375(8) . ? C28 C29 1.388(8) . ? C29 C30 1.345(9) . ? C29 C32 1.532(9) . ? C30 C31 1.373(8) . ? C33 O10 1.258(5) 2_676 ? C33 C34 1.503(6) . ? C34 C35 1.372(6) . ? C34 C39 1.386(6) . ? C35 C36 1.365(7) . ? C36 C37 1.369(8) . ? C37 C38 1.369(8) . ? C37 C40 1.513(7) . ? C38 C39 1.378(7) . ? C41 C42 1.390(6) . ? C42 C43 1.353(8) . ? C43 C44 1.400(8) . ? C44 C52 1.410(6) . ? C44 C45 1.419(8) . ? C45 C46 1.349(9) . ? C46 C47 1.419(8) . ? C47 C51 1.403(6) . ? C47 C48 1.415(8) . ? C48 C49 1.343(8) . ? C49 C50 1.384(8) . ? C51 C52 1.437(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Sm1 O5 159.78(12) . . ? O7 Sm1 O10 77.80(12) . . ? O5 Sm1 O10 103.48(12) . . ? O7 Sm1 O1 82.73(12) . . ? O5 Sm1 O1 77.72(12) . . ? O10 Sm1 O1 79.82(12) . . ? O7 Sm1 O9 81.31(11) . . ? O5 Sm1 O9 112.04(12) . . ? O10 Sm1 O9 126.98(10) . . ? O1 Sm1 O9 144.27(12) . . ? O7 Sm1 O8 126.15(11) . . ? O5 Sm1 O8 73.20(11) . . ? O10 Sm1 O8 78.36(12) . . ? O1 Sm1 O8 138.06(12) . . ? O9 Sm1 O8 75.94(11) . . ? O7 Sm1 O3 86.90(11) . . ? O5 Sm1 O3 82.19(11) . . ? O10 Sm1 O3 149.27(11) . . ? O1 Sm1 O3 71.84(11) . . ? O9 Sm1 O3 75.55(10) . . ? O8 Sm1 O3 131.35(11) . . ? O2 Cd1 O6 98.09(14) . . ? O2 Cd1 O4 152.76(12) . . ? O6 Cd1 O4 99.24(13) . . ? O2 Cd1 N1 107.25(12) . . ? O6 Cd1 N1 85.05(12) . . ? O4 Cd1 N1 95.07(12) . . ? O2 Cd1 N2 87.54(13) . . ? O6 Cd1 N2 155.34(12) . . ? O4 Cd1 N2 85.42(13) . . ? N1 Cd1 N2 70.38(13) . . ? O2 Cd1 O3 100.85(12) . . ? O6 Cd1 O3 110.35(11) . . ? O4 Cd1 O3 53.24(11) . . ? N1 Cd1 O3 145.69(11) . . ? N2 Cd1 O3 91.92(12) . . ? C41 N1 C52 118.6(4) . . ? C41 N1 Cd1 124.4(3) . . ? C52 N1 Cd1 116.8(3) . . ? C50 N2 C51 118.4(4) . . ? C50 N2 Cd1 126.1(3) . . ? C51 N2 Cd1 115.4(3) . . ? C1 O1 Sm1 151.1(3) . . ? C1 O2 Cd1 118.2(3) . . ? C9 O3 Sm1 139.3(3) . . ? C9 O3 Cd1 88.5(2) . . ? Sm1 O3 Cd1 105.05(11) . . ? C9 O4 Cd1 96.1(3) . . ? C17 O5 Sm1 167.7(3) . . ? C17 O6 Cd1 112.9(3) . . ? C25 O7 Sm1 178.2(3) 2_676 . ? C25 O8 Sm1 112.4(3) . . ? C33 O9 Sm1 133.6(3) . . ? C33 O10 Sm1 140.6(3) 2_676 . ? O1 C1 O2 124.9(4) . . ? O1 C1 C2 117.2(4) . . ? O2 C1 C2 117.9(4) . . ? C7 C2 C3 118.3(4) . . ? C7 C2 C1 121.5(4) . . ? C3 C2 C1 120.2(5) . . ? C4 C3 C2 120.0(6) . . ? C3 C4 C5 121.6(6) . . ? C6 C5 C4 117.4(6) . . ? C6 C5 C8 120.9(9) . . ? C4 C5 C8 121.7(8) . . ? C5 C6 C7 121.6(7) . . ? C2 C7 C6 121.1(6) . . ? O4 C9 O3 119.7(4) . . ? O4 C9 C10 120.7(4) . . ? O3 C9 C10 119.5(4) . . ? C11 C10 C15 119.5(5) . . ? C11 C10 C9 120.5(5) . . ? C15 C10 C9 119.9(5) . . ? C10 C11 C12 120.2(8) . . ? C13 C12 C11 120.5(8) . . ? C14 C13 C12 119.8(7) . . ? C14 C13 C16 120.4(11) . . ? C12 C13 C16 119.9(11) . . ? C13 C14 C15 121.3(8) . . ? C10 C15 C14 118.7(7) . . ? O6 C17 O5 122.9(4) . . ? O6 C17 C18 117.8(3) . . ? O5 C17 C18 119.3(4) . . ? C19 C18 C23 118.8(4) . . ? C19 C18 C17 121.8(4) . . ? C23 C18 C17 119.4(4) . . ? C18 C19 C20 119.6(5) . . ? C19 C20 C21 121.4(5) . . ? C22 C21 C20 117.4(5) . . ? C22 C21 C24 121.1(6) . . ? C20 C21 C24 121.5(6) . . ? C23 C22 C21 122.2(5) . . ? C22 C23 C18 120.5(5) . . ? O8 C25 O7 122.7(4) . 2_676 ? O8 C25 C26 118.8(4) . . ? O7 C25 C26 118.5(4) 2_676 . ? C27 C26 C31 118.5(5) . . ? C27 C26 C25 120.0(4) . . ? C31 C26 C25 121.5(4) . . ? C28 C27 C26 120.8(5) . . ? C27 C28 C29 120.4(6) . . ? C30 C29 C28 118.2(6) . . ? C30 C29 C32 121.8(6) . . ? C28 C29 C32 120.0(7) . . ? C29 C30 C31 122.0(5) . . ? C30 C31 C26 120.1(5) . . ? O10 C33 O9 124.7(4) 2_676 . ? O10 C33 C34 116.9(4) 2_676 . ? O9 C33 C34 118.4(4) . . ? C35 C34 C39 118.2(4) . . ? C35 C34 C33 121.8(4) . . ? C39 C34 C33 120.0(4) . . ? C36 C35 C34 120.5(5) . . ? C35 C36 C37 122.3(5) . . ? C38 C37 C36 117.2(5) . . ? C38 C37 C40 121.1(6) . . ? C36 C37 C40 121.7(6) . . ? C37 C38 C39 121.7(5) . . ? C38 C39 C34 120.1(5) . . ? N1 C41 C42 123.6(5) . . ? C43 C42 C41 118.4(5) . . ? C42 C43 C44 120.4(5) . . ? C43 C44 C52 117.5(5) . . ? C43 C44 C45 123.8(5) . . ? C52 C44 C45 118.7(6) . . ? C46 C45 C44 121.3(5) . . ? C45 C46 C47 121.7(5) . . ? C51 C47 C48 116.6(5) . . ? C51 C47 C46 118.9(6) . . ? C48 C47 C46 124.5(5) . . ? C49 C48 C47 120.9(5) . . ? C48 C49 C50 118.4(6) . . ? N2 C50 C49 123.6(6) . . ? N2 C51 C47 122.0(5) . . ? N2 C51 C52 118.4(4) . . ? C47 C51 C52 119.6(5) . . ? N1 C52 C44 121.4(5) . . ? N1 C52 C51 118.7(4) . . ? C44 C52 C51 119.8(4) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.730 _refine_diff_density_min -1.318 _refine_diff_density_rms 0.285 data_ly07077 _database_code_depnum_ccdc_archive 'CCDC 714922' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H28 Cd Cl5 Ho N2 O10' _chemical_formula_weight 1235.29 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' Cd Cd -0.8075 1.2024 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2996(14) _cell_length_b 14.9188(16) _cell_length_c 14.980(3) _cell_angle_alpha 115.232(2) _cell_angle_beta 98.313(2) _cell_angle_gamma 110.4570(10) _cell_volume 2363.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 2.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7914 _exptl_absorpt_correction_T_max 0.7914 _exptl_absorpt_process_details sadabs _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 'Smart Apex II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12837 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9082 _reflns_number_gt 7576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997a)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.5138P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9082 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.052850(17) 0.043394(16) 0.155622(14) 0.03557(8) Uani 1 1 d . . . Cd1 Cd 0.18346(3) 0.03766(3) 0.40402(2) 0.04727(11) Uani 1 1 d . . . N1 N 0.2230(3) 0.0400(3) 0.5621(3) 0.0490(10) Uani 1 1 d . . . N2 N 0.2979(4) -0.0548(3) 0.4034(3) 0.0513(10) Uani 1 1 d . . . O1 O 0.3317(3) 0.1715(3) 0.4121(3) 0.0701(11) Uani 1 1 d . . . O2 O 0.2451(3) 0.1342(3) 0.2529(3) 0.0624(10) Uani 1 1 d . . . O3 O 0.0507(3) 0.1327(3) 0.3199(2) 0.0594(9) Uani 1 1 d . . . O4 O 0.0871(3) 0.1296(3) 0.4661(3) 0.0600(10) Uani 1 1 d . . . O5 O -0.1097(3) -0.1286(2) 0.0464(2) 0.0446(7) Uani 1 1 d . . . O6 O 0.1184(3) 0.1832(3) 0.1205(2) 0.0507(8) Uani 1 1 d . . . O7 O 0.0299(3) -0.1435(3) 0.3060(3) 0.0638(10) Uani 1 1 d . . . O8 O 0.0859(3) -0.0760(3) 0.2079(2) 0.0490(8) Uani 1 1 d . . . O9 O -0.1005(3) 0.0885(3) 0.1410(2) 0.0510(8) Uani 1 1 d . . . O10 O 0.1160(3) -0.0295(3) 0.0252(2) 0.0496(8) Uani 1 1 d . . . Cl1 Cl 0.7315(2) 0.5679(3) 0.3822(4) 0.232(2) Uani 1 1 d . . . Cl2 Cl -0.1580(3) 0.4607(2) 0.6026(2) 0.1483(11) Uani 1 1 d . . . Cl3 Cl -0.53524(17) -0.65165(15) -0.20971(19) 0.1125(7) Uani 1 1 d . . . Cl4 Cl -0.1828(2) -0.61913(16) -0.15506(18) 0.1355(10) Uani 1 1 d . . . Cl5 Cl -0.5143(4) 0.2024(4) -0.0085(2) 0.256(3) Uani 1 1 d . . . C1 C 0.1841(5) 0.0848(5) 0.6381(4) 0.0616(14) Uani 1 1 d . . . H1A H 0.1442 0.1232 0.6316 0.074 Uiso 1 1 calc R . . C2 C 0.2018(5) 0.0753(6) 0.7277(4) 0.0693(17) Uani 1 1 d . . . H2A H 0.163(4) 0.106(4) 0.771(4) 0.053(15) Uiso 1 1 d . . . C3 C 0.2581(5) 0.0191(6) 0.7373(5) 0.077(2) Uani 1 1 d . . . H3A H 0.2687 0.0118 0.7961 0.093 Uiso 1 1 calc R . . C4 C 0.3015(5) -0.0294(5) 0.6588(5) 0.0673(17) Uani 1 1 d . . . C5 C 0.3615(6) -0.0915(7) 0.6625(7) 0.089(2) Uani 1 1 d . . . H5A H 0.3719 -0.1031 0.7187 0.107 Uiso 1 1 calc R . . C6 C 0.4026(6) -0.1330(6) 0.5875(7) 0.089(2) Uani 1 1 d . . . H6A H 0.4447 -0.1695 0.5945 0.107 Uiso 1 1 calc R . . C7 C 0.3841(5) -0.1233(5) 0.4962(5) 0.0680(17) Uani 1 1 d . . . C8 C 0.4259(6) -0.1640(5) 0.4159(7) 0.080(2) Uani 1 1 d . . . H8A H 0.475(6) -0.182(6) 0.429(5) 0.09(2) Uiso 1 1 d . . . C9 C 0.4024(5) -0.1528(5) 0.3321(6) 0.0792(19) Uani 1 1 d . . . H9A H 0.4289 -0.1812 0.2775 0.095 Uiso 1 1 calc R . . C10 C 0.3379(5) -0.0981(5) 0.3285(4) 0.0647(15) Uani 1 1 d . . . H10A H 0.3216 -0.0915 0.2698 0.078 Uiso 1 1 calc R . . C11 C 0.3213(4) -0.0655(4) 0.4887(4) 0.0500(12) Uani 1 1 d . . . C12 C 0.2803(4) -0.0165(4) 0.5715(4) 0.0485(12) Uani 1 1 d . . . C13 C 0.3278(4) 0.1901(4) 0.3378(4) 0.0473(11) Uani 1 1 d . . . C14 C 0.4301(4) 0.2841(4) 0.3488(4) 0.0569(13) Uani 1 1 d . . . C15 C 0.5106(6) 0.3656(6) 0.4466(6) 0.093(2) Uani 1 1 d . . . H15A H 0.5025 0.3621 0.5058 0.111 Uiso 1 1 calc R . . C16 C 0.6043(7) 0.4537(7) 0.4564(9) 0.130(4) Uani 1 1 d . . . H16A H 0.6591 0.5096 0.5222 0.156 Uiso 1 1 calc R . . C17 C 0.6149(6) 0.4571(7) 0.3682(10) 0.116(4) Uani 1 1 d . . . C18 C 0.5368(6) 0.3765(6) 0.2716(7) 0.090(2) Uani 1 1 d . . . H18A H 0.5461 0.3792 0.2123 0.108 Uiso 1 1 calc R . . C19 C 0.4434(5) 0.2903(5) 0.2624(5) 0.0653(15) Uani 1 1 d . . . H19A H 0.3884 0.2355 0.1963 0.078 Uiso 1 1 calc R . . C20 C 0.0472(4) 0.1598(4) 0.4107(3) 0.0442(11) Uani 1 1 d . . . C21 C -0.0056(4) 0.2337(4) 0.4554(3) 0.0421(10) Uani 1 1 d . . . C22 C -0.0404(5) 0.2821(5) 0.4051(5) 0.0633(15) Uani 1 1 d . . . H22A H -0.025(5) 0.272(5) 0.350(5) 0.07(2) Uiso 1 1 d . . . C23 C -0.0887(6) 0.3511(6) 0.4489(6) 0.0807(19) Uani 1 1 d . . . H23A H -0.107(5) 0.392(5) 0.412(5) 0.09(2) Uiso 1 1 d . . . C24 C -0.1007(6) 0.3704(5) 0.5443(5) 0.0775(18) Uani 1 1 d . . . C25 C -0.0675(5) 0.3244(5) 0.5946(5) 0.0675(16) Uani 1 1 d . . . H25A H -0.0770 0.3386 0.6588 0.081 Uiso 1 1 calc R . . C26 C -0.0198(5) 0.2568(5) 0.5511(4) 0.0532(13) Uani 1 1 d . . . H26A H 0.007(4) 0.231(4) 0.584(4) 0.053(16) Uiso 1 1 d . . . C27 C -0.1512(4) -0.1995(4) -0.0515(4) 0.0420(10) Uani 1 1 d . . . C28 C -0.2778(5) -0.3979(5) -0.1907(4) 0.0570(14) Uani 1 1 d . . . H28A H -0.240(4) -0.389(4) -0.230(4) 0.052(15) Uiso 1 1 d . . . C29 C -0.3657(5) -0.5034(5) -0.2287(4) 0.0658(15) Uani 1 1 d . . . H29A H -0.3854 -0.5612 -0.2966 0.079 Uiso 1 1 calc R . . C30 C -0.4233(5) -0.5203(5) -0.1636(5) 0.0670(16) Uani 1 1 d . . . C31 C -0.3938(5) -0.4355(5) -0.0630(5) 0.0754(18) Uani 1 1 d . . . H31A H -0.4336 -0.4481 -0.0199 0.091 Uiso 1 1 calc R . . C32 C -0.3056(4) -0.3322(4) -0.0262(4) 0.0570(13) Uani 1 1 d . . . H32A H -0.2851 -0.2752 0.0424 0.068 Uiso 1 1 calc R . . C33 C -0.2469(4) -0.3119(4) -0.0899(4) 0.0412(10) Uani 1 1 d . . . C34 C 0.0313(4) -0.1582(4) 0.2185(4) 0.0460(11) Uani 1 1 d . . . C35 C -0.0233(5) -0.2729(4) 0.1247(4) 0.0546(13) Uani 1 1 d . . . C36 C 0.0047(5) -0.2927(5) 0.0355(4) 0.0638(15) Uani 1 1 d . . . H36A H 0.0561 -0.2331 0.0332 0.077 Uiso 1 1 calc R . . C37 C -0.0423(6) -0.3993(6) -0.0508(5) 0.082(2) Uani 1 1 d . . . H37A H -0.0218 -0.4129 -0.1103 0.098 Uiso 1 1 calc R . . C38 C -0.1193(7) -0.4834(6) -0.0458(6) 0.083(2) Uani 1 1 d . . . C39 C -0.1493(6) -0.4705(6) 0.0395(7) 0.092(2) Uani 1 1 d . . . H39A H -0.2010 -0.5311 0.0401 0.110 Uiso 1 1 calc R . . C40 C -0.0986(6) -0.3596(5) 0.1292(6) 0.0741(17) Uani 1 1 d . . . H40A H -0.129(4) -0.348(4) 0.184(4) 0.041(13) Uiso 1 1 d . . . C41 C -0.1447(4) 0.0728(4) 0.0531(4) 0.0464(11) Uani 1 1 d . . . C42 C -0.2367(5) 0.1048(5) 0.0370(4) 0.0564(13) Uani 1 1 d . . . C43 C -0.2581(7) 0.1688(7) 0.1226(5) 0.106(3) Uani 1 1 d . . . H43A H -0.2132 0.1937 0.1900 0.127 Uiso 1 1 calc R . . C44 C -0.3466(9) 0.1968(10) 0.1091(6) 0.159(5) Uani 1 1 d . . . H44A H -0.3652 0.2352 0.1663 0.190 Uiso 1 1 calc R . . C45 C -0.4058(9) 0.1661(9) 0.0092(6) 0.147(5) Uani 1 1 d . . . C46 C -0.3870(6) 0.1004(7) -0.0762(5) 0.102(3) Uani 1 1 d . . . H46A H -0.4303 0.0771 -0.1436 0.123 Uiso 1 1 calc R . . C47 C -0.3040(5) 0.0694(6) -0.0618(4) 0.0748(18) Uani 1 1 d . . . H47A H -0.2926 0.0230 -0.1203 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.04117(12) 0.04220(13) 0.02637(11) 0.01814(9) 0.01416(8) 0.02059(9) Cd1 0.0554(2) 0.0571(2) 0.03152(18) 0.01988(16) 0.01331(15) 0.03232(18) N1 0.049(2) 0.058(3) 0.041(2) 0.027(2) 0.0128(18) 0.025(2) N2 0.052(2) 0.047(2) 0.043(2) 0.0151(19) 0.0134(19) 0.023(2) O1 0.072(2) 0.076(3) 0.060(2) 0.042(2) 0.009(2) 0.029(2) O2 0.0435(19) 0.074(3) 0.052(2) 0.0308(19) 0.0071(16) 0.0147(18) O3 0.077(2) 0.076(3) 0.0295(17) 0.0219(17) 0.0216(16) 0.045(2) O4 0.088(3) 0.078(3) 0.045(2) 0.0355(19) 0.0308(19) 0.060(2) O5 0.0493(18) 0.0414(18) 0.0385(18) 0.0201(15) 0.0127(14) 0.0175(15) O6 0.061(2) 0.0481(19) 0.0417(18) 0.0259(16) 0.0203(16) 0.0197(16) O7 0.076(2) 0.064(2) 0.040(2) 0.0269(18) 0.0172(18) 0.021(2) O8 0.060(2) 0.049(2) 0.0439(18) 0.0276(16) 0.0156(16) 0.0280(17) O9 0.057(2) 0.075(2) 0.0383(18) 0.0308(17) 0.0218(15) 0.0438(19) O10 0.060(2) 0.062(2) 0.0389(17) 0.0248(16) 0.0272(16) 0.0384(18) Cl1 0.1007(19) 0.174(3) 0.341(5) 0.169(4) 0.007(3) -0.036(2) Cl2 0.193(3) 0.159(2) 0.177(2) 0.084(2) 0.113(2) 0.151(2) Cl3 0.0854(12) 0.0557(10) 0.1382(18) 0.0269(11) 0.0383(12) 0.0027(9) Cl4 0.1423(19) 0.0668(12) 0.1096(16) -0.0099(11) -0.0260(14) 0.0565(12) Cl5 0.294(4) 0.411(6) 0.113(2) 0.064(3) 0.023(2) 0.320(5) C1 0.062(3) 0.077(4) 0.040(3) 0.027(3) 0.020(2) 0.030(3) C2 0.061(4) 0.093(5) 0.044(3) 0.034(3) 0.023(3) 0.026(3) C3 0.062(4) 0.107(5) 0.058(4) 0.057(4) 0.012(3) 0.019(4) C4 0.049(3) 0.089(4) 0.065(4) 0.055(3) 0.009(3) 0.018(3) C5 0.069(4) 0.113(6) 0.117(6) 0.094(5) 0.018(4) 0.036(4) C6 0.070(4) 0.082(5) 0.132(7) 0.072(5) 0.017(4) 0.037(4) C7 0.043(3) 0.052(3) 0.101(5) 0.041(3) 0.010(3) 0.019(3) C8 0.051(4) 0.047(3) 0.116(6) 0.021(4) 0.015(4) 0.028(3) C9 0.057(4) 0.060(4) 0.083(5) 0.011(3) 0.020(3) 0.025(3) C10 0.061(3) 0.061(4) 0.055(3) 0.015(3) 0.020(3) 0.029(3) C11 0.037(2) 0.040(3) 0.055(3) 0.020(2) 0.005(2) 0.010(2) C12 0.037(2) 0.050(3) 0.050(3) 0.028(2) 0.007(2) 0.010(2) C13 0.047(3) 0.053(3) 0.047(3) 0.026(2) 0.016(2) 0.028(2) C14 0.045(3) 0.058(3) 0.070(4) 0.035(3) 0.008(3) 0.029(3) C15 0.081(5) 0.072(5) 0.074(4) 0.030(4) -0.015(4) 0.011(4) C16 0.078(5) 0.085(6) 0.139(9) 0.040(6) -0.039(5) 0.002(5) C17 0.048(4) 0.097(6) 0.190(10) 0.092(7) 0.008(5) 0.009(4) C18 0.066(4) 0.098(5) 0.131(7) 0.079(5) 0.045(4) 0.034(4) C19 0.050(3) 0.067(4) 0.076(4) 0.036(3) 0.017(3) 0.025(3) C20 0.048(3) 0.046(3) 0.031(2) 0.015(2) 0.013(2) 0.021(2) C21 0.044(2) 0.039(3) 0.035(2) 0.013(2) 0.0119(19) 0.019(2) C22 0.077(4) 0.076(4) 0.050(3) 0.032(3) 0.023(3) 0.048(3) C23 0.096(5) 0.077(5) 0.087(5) 0.044(4) 0.025(4) 0.060(4) C24 0.083(4) 0.079(4) 0.080(4) 0.030(4) 0.038(4) 0.056(4) C25 0.083(4) 0.070(4) 0.059(3) 0.028(3) 0.044(3) 0.044(3) C26 0.060(3) 0.060(3) 0.044(3) 0.027(3) 0.025(2) 0.030(3) C27 0.046(3) 0.047(3) 0.042(3) 0.025(2) 0.017(2) 0.026(2) C28 0.063(3) 0.053(3) 0.050(3) 0.024(3) 0.022(3) 0.024(3) C29 0.066(4) 0.054(3) 0.053(3) 0.014(3) 0.019(3) 0.022(3) C30 0.055(3) 0.047(3) 0.084(4) 0.029(3) 0.020(3) 0.015(3) C31 0.066(4) 0.066(4) 0.080(4) 0.034(3) 0.042(3) 0.013(3) C32 0.060(3) 0.052(3) 0.047(3) 0.021(2) 0.020(2) 0.018(3) C33 0.042(2) 0.044(3) 0.043(3) 0.024(2) 0.014(2) 0.022(2) C34 0.048(3) 0.050(3) 0.041(3) 0.022(2) 0.010(2) 0.026(2) C35 0.062(3) 0.046(3) 0.052(3) 0.022(2) 0.007(2) 0.029(3) C36 0.078(4) 0.065(4) 0.046(3) 0.022(3) 0.012(3) 0.043(3) C37 0.101(5) 0.076(5) 0.054(4) 0.015(3) 0.008(3) 0.056(4) C38 0.089(5) 0.055(4) 0.075(5) 0.012(3) -0.006(4) 0.042(4) C39 0.085(5) 0.059(4) 0.107(6) 0.037(4) 0.010(5) 0.026(4) C40 0.073(4) 0.061(4) 0.075(4) 0.030(3) 0.015(4) 0.028(3) C41 0.052(3) 0.054(3) 0.037(3) 0.023(2) 0.020(2) 0.028(2) C42 0.065(3) 0.080(4) 0.041(3) 0.031(3) 0.023(2) 0.049(3) C43 0.131(6) 0.166(8) 0.049(4) 0.033(4) 0.026(4) 0.125(6) C44 0.182(9) 0.266(12) 0.053(4) 0.035(6) 0.027(5) 0.193(10) C45 0.162(8) 0.235(11) 0.072(5) 0.045(6) 0.015(5) 0.175(9) C46 0.101(5) 0.172(8) 0.050(4) 0.046(5) 0.023(4) 0.094(6) C47 0.084(4) 0.112(5) 0.039(3) 0.032(3) 0.021(3) 0.064(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O10 2.238(3) . ? Ho1 O3 2.255(3) . ? Ho1 O6 2.277(3) . ? Ho1 O2 2.305(3) . ? Ho1 O5 2.336(3) . ? Ho1 O9 2.369(3) . ? Ho1 O8 2.370(3) . ? Cd1 O1 2.205(4) . ? Cd1 O4 2.208(3) . ? Cd1 N1 2.334(4) . ? Cd1 O7 2.350(4) . ? Cd1 N2 2.384(4) . ? Cd1 O8 2.510(3) . ? N1 C1 1.332(7) . ? N1 C12 1.352(6) . ? N2 C10 1.323(7) . ? N2 C11 1.359(6) . ? O1 C13 1.255(6) . ? O2 C13 1.254(5) . ? O3 C20 1.257(5) . ? O4 C20 1.237(5) . ? O5 C27 1.269(5) . ? O6 C27 1.259(5) 2 ? O7 C34 1.237(6) . ? O8 C34 1.279(6) . ? O9 C41 1.246(5) . ? O10 C41 1.262(5) 2 ? Cl1 C17 1.732(7) . ? Cl2 C24 1.752(6) . ? Cl3 C30 1.744(5) . ? Cl4 C38 1.753(7) . ? Cl5 C45 1.735(7) . ? C1 C2 1.405(8) . ? C2 C3 1.340(10) . ? C3 C4 1.415(10) . ? C4 C12 1.404(7) . ? C4 C5 1.430(10) . ? C5 C6 1.330(11) . ? C6 C7 1.431(10) . ? C7 C8 1.389(10) . ? C7 C11 1.419(8) . ? C8 C9 1.343(10) . ? C9 C10 1.385(9) . ? C11 C12 1.440(7) . ? C13 C14 1.499(7) . ? C14 C19 1.369(8) . ? C14 C15 1.374(8) . ? C15 C16 1.393(11) . ? C16 C17 1.369(13) . ? C17 C18 1.351(12) . ? C18 C19 1.378(8) . ? C20 C21 1.485(7) . ? C21 C22 1.378(7) . ? C21 C26 1.384(7) . ? C22 C23 1.382(9) . ? C23 C24 1.378(9) . ? C24 C25 1.337(9) . ? C25 C26 1.360(8) . ? C27 O6 1.259(5) 2 ? C27 C33 1.495(6) . ? C28 C33 1.377(7) . ? C28 C29 1.387(8) . ? C29 C30 1.376(8) . ? C30 C31 1.371(8) . ? C31 C32 1.372(7) . ? C32 C33 1.382(7) . ? C34 C35 1.489(7) . ? C35 C40 1.367(8) . ? C35 C36 1.377(8) . ? C36 C37 1.383(8) . ? C37 C38 1.354(10) . ? C38 C39 1.349(11) . ? C39 C40 1.435(10) . ? C41 O10 1.262(5) 2 ? C41 C42 1.483(7) . ? C42 C43 1.373(8) . ? C42 C47 1.375(7) . ? C43 C44 1.397(9) . ? C44 C45 1.375(10) . ? C45 C46 1.361(10) . ? C46 C47 1.361(9) . ? 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 O10 Ho1 O3 159.97(13) . . ? O10 Ho1 O6 78.50(12) . . ? O3 Ho1 O6 102.67(13) . . ? O10 Ho1 O2 81.64(13) . . ? O3 Ho1 O2 79.04(14) . . ? O6 Ho1 O2 78.68(13) . . ? O10 Ho1 O5 81.25(12) . . ? O3 Ho1 O5 112.54(12) . . ? O6 Ho1 O5 125.63(11) . . ? O2 Ho1 O5 146.15(13) . . ? O10 Ho1 O9 125.50(11) . . ? O3 Ho1 O9 73.51(12) . . ? O6 Ho1 O9 76.72(12) . . ? O2 Ho1 O9 137.68(13) . . ? O5 Ho1 O9 75.36(12) . . ? O10 Ho1 O8 85.96(12) . . ? O3 Ho1 O8 83.68(12) . . ? O6 Ho1 O8 150.20(13) . . ? O2 Ho1 O8 73.97(13) . . ? O5 Ho1 O8 75.87(11) . . ? O9 Ho1 O8 132.38(12) . . ? O1 Cd1 O4 99.80(16) . . ? O1 Cd1 N1 109.30(13) . . ? O4 Cd1 N1 86.59(14) . . ? O1 Cd1 O7 149.61(14) . . ? O4 Cd1 O7 98.36(15) . . ? N1 Cd1 O7 95.89(13) . . ? O1 Cd1 N2 87.95(15) . . ? O4 Cd1 N2 157.29(13) . . ? N1 Cd1 N2 70.70(15) . . ? O7 Cd1 N2 84.55(14) . . ? O1 Cd1 O8 98.08(12) . . ? O4 Cd1 O8 105.82(12) . . ? N1 Cd1 O8 147.65(13) . . ? O7 Cd1 O8 53.35(11) . . ? N2 Cd1 O8 94.03(12) . . ? C1 N1 C12 119.1(4) . . ? C1 N1 Cd1 123.8(4) . . ? C12 N1 Cd1 116.9(3) . . ? C10 N2 C11 117.7(5) . . ? C10 N2 Cd1 126.9(4) . . ? C11 N2 Cd1 115.3(3) . . ? C13 O1 Cd1 120.7(3) . . ? C13 O2 Ho1 153.0(3) . . ? C20 O3 Ho1 165.1(3) . . ? C20 O4 Cd1 116.3(3) . . ? C27 O5 Ho1 134.6(3) . . ? C27 O6 Ho1 139.3(3) 2 . ? C34 O7 Cd1 96.1(3) . . ? C34 O8 Ho1 140.2(3) . . ? C34 O8 Cd1 87.7(3) . . ? Ho1 O8 Cd1 106.90(13) . . ? C41 O9 Ho1 115.1(3) . . ? C41 O10 Ho1 175.8(3) 2 . ? N1 C1 C2 121.5(6) . . ? C3 C2 C1 119.7(6) . . ? C2 C3 C4 120.7(5) . . ? C12 C4 C3 116.2(6) . . ? C12 C4 C5 119.5(6) . . ? C3 C4 C5 124.2(6) . . ? C6 C5 C4 121.5(6) . . ? C5 C6 C7 122.0(7) . . ? C8 C7 C11 117.8(6) . . ? C8 C7 C6 124.5(7) . . ? C11 C7 C6 117.6(7) . . ? C9 C8 C7 120.4(7) . . ? C8 C9 C10 118.7(7) . . ? N2 C10 C9 124.1(6) . . ? N2 C11 C7 121.2(5) . . ? N2 C11 C12 118.1(5) . . ? C7 C11 C12 120.7(5) . . ? N1 C12 C4 122.7(5) . . ? N1 C12 C11 118.7(4) . . ? C4 C12 C11 118.5(5) . . ? O2 C13 O1 124.9(5) . . ? O2 C13 C14 116.8(4) . . ? O1 C13 C14 118.4(4) . . ? C19 C14 C15 119.6(6) . . ? C19 C14 C13 120.6(5) . . ? C15 C14 C13 119.9(6) . . ? C14 C15 C16 119.5(8) . . ? C17 C16 C15 119.3(7) . . ? C18 C17 C16 121.5(7) . . ? C18 C17 Cl1 119.9(9) . . ? C16 C17 Cl1 118.6(8) . . ? C17 C18 C19 119.0(7) . . ? C14 C19 C18 121.0(6) . . ? O4 C20 O3 123.6(5) . . ? O4 C20 C21 117.9(4) . . ? O3 C20 C21 118.6(4) . . ? C22 C21 C26 118.0(5) . . ? C22 C21 C20 122.2(4) . . ? C26 C21 C20 119.8(4) . . ? C21 C22 C23 120.9(6) . . ? C24 C23 C22 118.1(6) . . ? C25 C24 C23 122.1(6) . . ? C25 C24 Cl2 119.2(5) . . ? C23 C24 Cl2 118.7(5) . . ? C24 C25 C26 119.4(6) . . ? C25 C26 C21 121.4(6) . . ? O6 C27 O5 125.3(4) 2 . ? O6 C27 C33 116.4(4) 2 . ? O5 C27 C33 118.4(4) . . ? C33 C28 C29 121.5(5) . . ? C30 C29 C28 118.4(5) . . ? C31 C30 C29 121.0(5) . . ? C31 C30 Cl3 119.6(5) . . ? C29 C30 Cl3 119.4(5) . . ? C30 C31 C32 119.9(5) . . ? C31 C32 C33 120.7(5) . . ? C28 C33 C32 118.6(5) . . ? C28 C33 C27 119.9(4) . . ? C32 C33 C27 121.5(4) . . ? O7 C34 O8 120.7(4) . . ? O7 C34 C35 120.6(5) . . ? O8 C34 C35 118.5(4) . . ? C40 C35 C36 120.0(6) . . ? C40 C35 C34 119.3(5) . . ? C36 C35 C34 120.6(5) . . ? C35 C36 C37 121.2(6) . . ? C38 C37 C36 117.7(7) . . ? C39 C38 C37 124.3(7) . . ? C39 C38 Cl4 116.9(7) . . ? C37 C38 Cl4 118.8(7) . . ? C38 C39 C40 117.5(7) . . ? C35 C40 C39 119.3(7) . . ? O9 C41 O10 123.2(5) . 2 ? O9 C41 C42 119.6(4) . . ? O10 C41 C42 117.2(4) 2 . ? C43 C42 C47 118.6(5) . . ? C43 C42 C41 119.6(5) . . ? C47 C42 C41 121.8(5) . . ? C42 C43 C44 120.5(6) . . ? C45 C44 C43 118.3(7) . . ? C46 C45 C44 121.3(7) . . ? C46 C45 Cl5 119.6(6) . . ? C44 C45 Cl5 118.9(6) . . ? C47 C46 C45 119.2(6) . . ? C46 C47 C42 121.7(6) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.064 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.098