# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H234 Cd2 Ce4 Cl14 N66 O107' _chemical_formula_weight 5307.07 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' Cd Cd -0.8075 1.2024 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.278(2) _cell_length_b 17.861(2) _cell_length_c 18.092(2) _cell_angle_alpha 82.207(5) _cell_angle_beta 71.356(5) _cell_angle_gamma 66.625(4) _cell_volume 4855.7(10) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2694 _exptl_absorpt_coefficient_mu 1.447 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6239 _exptl_absorpt_correction_T_max 0.6790 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54307 _diffrn_reflns_av_R_equivalents 0.0863 _diffrn_reflns_av_sigmaI/netI 0.0954 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.10 _reflns_number_total 17141 _reflns_number_gt 10873 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1253P)^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 17141 _refine_ls_number_parameters 1103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.2087 _refine_ls_wR_factor_gt 0.1885 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.003 _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 Cl5 Cl 1.5125(6) -1.0531(5) -0.3373(3) 0.254(5) Uani 1 1 d . . . Cl6 Cl 1.0817(4) -0.0179(3) 0.1152(4) 0.166(2) Uani 1 1 d . . . Cl7 Cl 1.5308(5) -0.8827(4) -0.9469(4) 0.201(3) Uani 1 1 d . . . Cl1 Cl 1.92453(14) -1.31235(14) -0.49970(13) 0.0581(6) Uani 1 1 d . . . Cl2 Cl 1.74592(17) -1.11250(15) -0.5535(3) 0.1019(13) Uani 1 1 d . . . Cl3 Cl 1.89224(19) -1.0879(2) -0.43410(18) 0.0924(10) Uani 1 1 d . . . Cl4 Cl 1.9811(3) -1.1278(3) -0.65491(19) 0.1131(12) Uani 1 1 d . . . Cd1 Cd 1.89166(4) -1.16987(4) -0.53423(4) 0.0530(3) Uani 0.949(2) 1 d P A 1 Cd1' Cd 1.8392(7) -1.1629(8) -0.4594(8) 0.053(5) Uani 0.051(2) 1 d P A 2 O1W O 1.2281(5) -0.2968(4) -0.1621(3) 0.0636(13) Uani 1 1 d . . . O2W O 1.6369(5) -0.7350(5) -0.9221(3) 0.083(2) Uani 1 1 d . . . O3W O 1.5332(4) -0.8138(4) -0.7960(4) 0.0698(18) Uani 1 1 d . . . O4W O 1.5886(4) -0.6304(4) -0.6812(4) 0.0653(17) Uani 1 1 d . . . O5W O 1.7325(5) -0.8767(4) -0.8261(3) 0.0636(13) Uani 1 1 d . . . O6W O 1.7290(5) -0.8064(5) -0.2231(5) 0.087(2) Uani 1 1 d . . . O7W O 1.6538(4) -0.6474(4) -0.2981(4) 0.083(2) Uani 1 1 d . . . O8W O 1.4175(5) -0.7220(7) -0.1816(4) 0.107(3) Uani 1 1 d . . . O9W O 1.4934(6) -0.6057(6) -0.1882(6) 0.127(4) Uani 1 1 d . . . O10W O 1.5074(7) -0.6489(6) -0.3473(6) 0.119(3) Uani 1 1 d . . . O11W O 1.6082(7) -0.8941(6) -0.2067(5) 0.115(3) Uani 1 1 d . . . O12W O 1.5605(6) -0.7488(8) -0.1062(4) 0.128(4) Uani 1 1 d . . . Ce1 Ce 1.62368(3) -0.73644(3) -0.77835(2) 0.04148(15) Uani 1 1 d . . . Ce2 Ce 1.57790(3) -0.74859(3) -0.25202(3) 0.04872(17) Uani 1 1 d . . . N33 N 1.4885(4) -0.5766(4) -0.8123(4) 0.0407(16) Uani 1 1 d . . . O17 O 1.5720(5) -0.5849(5) -0.8342(4) 0.085(2) Uani 1 1 d . . . O18 O 1.4707(4) -0.6320(5) -0.7800(5) 0.082(2) Uani 1 1 d . . . O19 O 1.4373(5) -0.5081(5) -0.8259(6) 0.106(3) Uani 1 1 d . . . C1 C 1.7640(5) -0.8330(4) -0.6507(4) 0.0371(17) Uani 1 1 d . . . C2 C 1.8449(4) -0.8809(4) -0.5610(4) 0.0348(17) Uani 1 1 d . . . H2 H 1.9061 -0.9211 -0.5697 0.042 Uiso 1 1 calc R . . C3 C 1.7776(4) -0.9226(5) -0.5444(4) 0.0351(16) Uani 1 1 d . . . H3 H 1.8068 -0.9827 -0.5482 0.042 Uiso 1 1 calc R . . C4 C 1.7426(4) -0.8429(4) -0.4369(4) 0.0319(17) Uani 1 1 d . . . C5 C 1.6672(4) -0.9121(5) -0.6158(4) 0.0354(16) Uani 1 1 d . . . H5A H 1.6681 -0.9028 -0.6707 0.042 Uiso 1 1 calc R . . H5B H 1.6831 -0.9708 -0.6051 0.042 Uiso 1 1 calc R . . C6 C 1.6562(4) -0.9312(4) -0.4195(4) 0.0342(16) Uani 1 1 d . . . H6A H 1.6761 -0.9880 -0.4347 0.041 Uiso 1 1 calc R . . H6B H 1.6519 -0.9311 -0.3641 0.041 Uiso 1 1 calc R . . C7 C 1.5171(5) -0.8052(5) -0.5907(4) 0.0368(17) Uani 1 1 d . . . C8 C 1.5433(4) -0.9002(4) -0.4928(4) 0.0310(15) Uani 1 1 d . . . H8 H 1.5526 -0.9583 -0.4956 0.037 Uiso 1 1 calc R . . C9 C 1.4431(4) -0.8447(4) -0.4701(4) 0.0349(17) Uani 1 1 d . . . H9 H 1.4057 -0.8765 -0.4637 0.042 Uiso 1 1 calc R . . C10 C 1.5023(4) -0.8329(5) -0.3755(4) 0.0354(17) Uani 1 1 d . . . C11 C 1.3554(4) -0.7442(5) -0.5559(4) 0.0367(17) Uani 1 1 d . . . H11A H 1.3686 -0.7276 -0.6109 0.044 Uiso 1 1 calc R . . H11B H 1.3244 -0.7813 -0.5490 0.044 Uiso 1 1 calc R . . C12 C 1.3395(4) -0.7688(5) -0.3455(4) 0.0379(17) Uani 1 1 d . . . H12A H 1.3061 -0.8035 -0.3403 0.045 Uiso 1 1 calc R . . H12B H 1.3442 -0.7646 -0.2937 0.045 Uiso 1 1 calc R . . C13 C 1.2618(4) -0.6011(5) -0.5428(4) 0.0335(16) Uani 1 1 d . . . C14 C 1.2448(4) -0.6773(5) -0.4282(4) 0.0351(17) Uani 1 1 d . . . H14 H 1.2170 -0.7176 -0.4219 0.042 Uiso 1 1 calc R . . C15 C 1.1756(4) -0.5897(4) -0.4125(4) 0.0309(15) Uani 1 1 d . . . H15 H 1.1148 -0.5887 -0.3921 0.037 Uiso 1 1 calc R . . C16 C 1.2631(5) -0.6232(5) -0.3289(4) 0.0401(18) Uani 1 1 d . . . C17 C 1.1285(5) -0.4734(5) -0.5083(4) 0.0352(17) Uani 1 1 d . . . H17A H 1.1399 -0.4696 -0.5651 0.042 Uiso 1 1 calc R . . H17B H 1.0685 -0.4724 -0.4850 0.042 Uiso 1 1 calc R . . C18 C 1.1380(5) -0.4879(5) -0.3078(4) 0.0395(18) Uani 1 1 d . . . H18A H 1.0782 -0.4879 -0.2937 0.047 Uiso 1 1 calc R . . H18B H 1.1531 -0.4910 -0.2594 0.047 Uiso 1 1 calc R . . C19 C 1.1582(4) -0.3475(5) -0.5313(4) 0.0331(16) Uani 1 1 d . . . C20 C 1.0876(4) -0.3746(4) -0.4031(4) 0.0327(16) Uani 1 1 d . . . H20 H 1.0286 -0.3779 -0.3843 0.039 Uiso 1 1 calc R . . C21 C 1.0821(4) -0.2862(4) -0.4106(4) 0.0313(15) Uani 1 1 d . . . H21 H 1.0205 -0.2465 -0.4005 0.038 Uiso 1 1 calc R . . C22 C 1.1500(4) -0.3555(5) -0.3136(4) 0.0359(17) Uani 1 1 d . . . C23 C 1.8689(5) -0.7985(5) -0.4716(4) 0.0381(18) Uani 1 1 d . . . H23A H 1.9301 -0.8375 -0.4864 0.046 Uiso 1 1 calc R . . H23B H 1.8499 -0.7911 -0.4151 0.046 Uiso 1 1 calc R . . C24 C 1.8920(5) -0.7937(5) -0.6780(4) 0.0403(18) Uani 1 1 d . . . H24A H 1.9528 -0.8311 -0.6822 0.048 Uiso 1 1 calc R . . H24B H 1.8853 -0.7850 -0.7307 0.048 Uiso 1 1 calc R . . C25 C 1.1508(5) -0.2765(6) 0.0587(5) 0.054(2) Uani 1 1 d . . . C26 C 1.0260(5) -0.2017(6) 0.1557(4) 0.047(2) Uani 1 1 d . . . H26 H 1.0146 -0.1459 0.1700 0.056 Uiso 1 1 calc R . . C27 C 1.0910(4) -0.2658(5) 0.1935(5) 0.0425(19) Uani 1 1 d . . . H27 H 1.1096 -0.2406 0.2267 0.051 Uiso 1 1 calc R . . C28 C 0.9581(5) -0.2853(5) 0.2379(4) 0.0402(18) Uani 1 1 d . . . C29 C 1.2499(5) -0.3641(6) 0.1351(5) 0.057(2) Uani 1 1 d . . . H29A H 1.2953 -0.3655 0.0856 0.068 Uiso 1 1 calc R . . H29B H 1.2640 -0.3448 0.1754 0.068 Uiso 1 1 calc R . . C30 C 1.0726(5) -0.3710(5) 0.2995(4) 0.0418(18) Uani 1 1 d . . . H30A H 1.0209 -0.3754 0.3400 0.050 Uiso 1 1 calc R . . H30B H 1.1013 -0.3476 0.3234 0.050 Uiso 1 1 calc R . . C31 C 1.3022(5) -0.5104(6) 0.1060(4) 0.049(2) Uani 1 1 d . . . C32 C 1.2282(4) -0.4737(5) 0.2357(4) 0.0388(18) Uani 1 1 d . . . H32 H 1.2549 -0.4562 0.2677 0.047 Uiso 1 1 calc R . . C33 C 1.2640(4) -0.5654(5) 0.2298(4) 0.0382(18) Uani 1 1 d . . . H33 H 1.3089 -0.5918 0.2579 0.046 Uiso 1 1 calc R . . C34 C 1.1114(4) -0.5195(5) 0.2945(4) 0.0352(17) Uani 1 1 d . . . C35 C 1.3622(5) -0.6592(6) 0.1149(5) 0.053(2) Uani 1 1 d . . . H35A H 1.3994 -0.6870 0.1492 0.063 Uiso 1 1 calc R . . H35B H 1.4008 -0.6520 0.0637 0.063 Uiso 1 1 calc R . . C36 C 1.1924(5) -0.6682(5) 0.2881(4) 0.0366(17) Uani 1 1 d . . . H36A H 1.1385 -0.6658 0.3295 0.044 Uiso 1 1 calc R . . H36B H 1.2421 -0.6948 0.3098 0.044 Uiso 1 1 calc R . . C37 C 1.3287(4) -0.7365(5) 0.0361(4) 0.0393(18) Uani 1 1 d . . . C38 C 1.2883(5) -0.7610(5) 0.1710(4) 0.0432(19) Uani 1 1 d . . . H38 H 1.3338 -0.7913 0.1978 0.052 Uiso 1 1 calc R . . C39 C 1.2681(5) -0.8186(5) 0.1296(4) 0.0414(18) Uani 1 1 d . . . H39 H 1.3010 -0.8765 0.1402 0.050 Uiso 1 1 calc R . . C40 C 1.1379(5) -0.7401(5) 0.2201(4) 0.0401(18) Uani 1 1 d . . . C41 C 1.3148(5) -0.8527(6) -0.0132(5) 0.049(2) Uani 1 1 d . . . H41A H 1.3569 -0.8421 -0.0603 0.058 Uiso 1 1 calc R . . H41B H 1.3421 -0.9091 0.0035 0.058 Uiso 1 1 calc R . . C42 C 1.1305(6) -0.8464(6) 0.1548(4) 0.053(2) Uani 1 1 d . . . H42A H 1.0747 -0.8329 0.1968 0.064 Uiso 1 1 calc R . . H42B H 1.1668 -0.9036 0.1619 0.064 Uiso 1 1 calc R . . C43 C 1.2249(5) -0.8168(5) -0.1057(4) 0.0424(19) Uani 1 1 d . . . C44 C 1.1776(5) -0.8835(5) 0.0125(4) 0.0418(18) Uani 1 1 d . . . H44 H 1.2101 -0.9403 0.0268 0.050 Uiso 1 1 calc R . . C45 C 1.1241(5) -0.8807(5) -0.0412(4) 0.0395(17) Uani 1 1 d . . . H45 H 1.1345 -0.9361 -0.0557 0.047 Uiso 1 1 calc R . . C46 C 1.0281(5) -0.8190(5) 0.0760(4) 0.044(2) Uani 1 1 d . . . C47 C 0.8593(5) -0.1649(6) 0.1818(4) 0.051(2) Uani 1 1 d . . . H47A H 0.8145 -0.1793 0.2232 0.061 Uiso 1 1 calc R . . H47B H 0.8516 -0.1094 0.1916 0.061 Uiso 1 1 calc R . . C48 C 1.0400(6) -0.1563(6) 0.0147(5) 0.057(2) Uani 1 1 d . . . H48A H 1.0899 -0.1648 -0.0327 0.068 Uiso 1 1 calc R . . H48B H 1.0227 -0.1016 0.0339 0.068 Uiso 1 1 calc R . . N1 N 1.8324(4) -0.8320(4) -0.6300(3) 0.0360(14) Uani 1 1 d . . . N2 N 1.7329(3) -0.8873(4) -0.6037(3) 0.0357(14) Uani 1 1 d . . . N3 N 1.8146(4) -0.8323(4) -0.4907(3) 0.0345(14) Uani 1 1 d . . . N4 N 1.7224(3) -0.8966(4) -0.4662(3) 0.0329(13) Uani 1 1 d . . . N5 N 1.5786(3) -0.8691(4) -0.5673(3) 0.0364(14) Uani 1 1 d . . . N6 N 1.4380(3) -0.7880(4) -0.5372(3) 0.0357(14) Uani 1 1 d . . . N7 N 1.5709(3) -0.8865(4) -0.4297(3) 0.0334(14) Uani 1 1 d . . . N8 N 1.4279(3) -0.8079(4) -0.3979(3) 0.0335(13) Uani 1 1 d . . . N9 N 1.2976(3) -0.6726(4) -0.5089(3) 0.0320(13) Uani 1 1 d . . . N10 N 1.1909(4) -0.5507(4) -0.4883(3) 0.0349(14) Uani 1 1 d . . . N11 N 1.2919(3) -0.6899(4) -0.3706(3) 0.0329(13) Uani 1 1 d . . . N12 N 1.2004(4) -0.5610(4) -0.3552(3) 0.0347(14) Uani 1 1 d . . . N13 N 1.1341(4) -0.4042(4) -0.4819(3) 0.0327(13) Uani 1 1 d . . . N14 N 1.1349(4) -0.2797(4) -0.4895(4) 0.0378(14) Uani 1 1 d . . . N15 N 1.1388(4) -0.4122(4) -0.3485(3) 0.0320(13) Uani 1 1 d . . . N16 N 1.1221(4) -0.2829(4) -0.3513(3) 0.0349(14) Uani 1 1 d . . . N17 N 1.0677(4) -0.2153(5) 0.0725(3) 0.0471(17) Uani 1 1 d . . . N18 N 1.1638(4) -0.3067(5) 0.1278(4) 0.0518(18) Uani 1 1 d . . . N19 N 0.9466(4) -0.2209(4) 0.1862(3) 0.0438(16) Uani 1 1 d . . . N20 N 1.0434(4) -0.3165(4) 0.2395(3) 0.0403(15) Uani 1 1 d . . . N21 N 1.2515(4) -0.4460(4) 0.1552(4) 0.0487(17) Uani 1 1 d . . . N22 N 1.3023(4) -0.5802(4) 0.1465(3) 0.0440(16) Uani 1 1 d . . . N23 N 1.1328(3) -0.4516(4) 0.2724(3) 0.0386(15) Uani 1 1 d . . . N24 N 1.1866(4) -0.5871(4) 0.2649(4) 0.0391(15) Uani 1 1 d . . . N25 N 1.3183(4) -0.7108(5) 0.1064(4) 0.0481(17) Uani 1 1 d . . . N26 N 1.2971(4) -0.7981(4) 0.0474(4) 0.0451(16) Uani 1 1 d . . . N27 N 1.2039(4) -0.7175(4) 0.2249(3) 0.0402(15) Uani 1 1 d . . . N28 N 1.1742(4) -0.7970(4) 0.1619(4) 0.0463(17) Uani 1 1 d . . . N29 N 1.2370(4) -0.8438(4) -0.0317(4) 0.0419(15) Uani 1 1 d . . . N30 N 1.1555(4) -0.8345(4) -0.1090(3) 0.0407(15) Uani 1 1 d . . . N31 N 1.1118(4) -0.8378(4) 0.0798(4) 0.0459(17) Uani 1 1 d . . . N32 N 1.0335(4) -0.8389(5) 0.0047(4) 0.0474(17) Uani 1 1 d . . . O1 O 1.7372(4) -0.7949(3) -0.7049(3) 0.0445(13) Uani 1 1 d . . . O2 O 1.5311(3) -0.7698(3) -0.6553(3) 0.0429(13) Uani 1 1 d . . . O3 O 1.2873(3) -0.5827(3) -0.6122(3) 0.0442(13) Uani 1 1 d . . . O4 O 1.1942(3) -0.3564(3) -0.6017(3) 0.0425(13) Uani 1 1 d . . . O5 O 1.7066(3) -0.8123(3) -0.3723(3) 0.0383(12) Uani 1 1 d . . . O6 O 1.5085(3) -0.8116(4) -0.3173(3) 0.0476(14) Uani 1 1 d . . . O7 O 1.2877(4) -0.6171(4) -0.2729(3) 0.0539(15) Uani 1 1 d . . . O8 O 1.1803(4) -0.3671(4) -0.2598(3) 0.0515(14) Uani 1 1 d . . . O9 O 1.2024(4) -0.2982(5) -0.0064(3) 0.075(2) Uani 1 1 d . . . O10 O 1.3394(4) -0.5045(4) 0.0374(3) 0.0700(19) Uani 1 1 d . . . O11 O 1.3599(4) -0.7099(4) -0.0263(3) 0.0599(16) Uani 1 1 d . . . O12 O 1.2682(4) -0.7871(4) -0.1542(3) 0.0610(17) Uani 1 1 d . . . O13 O 0.9009(3) -0.3105(4) 0.2759(3) 0.0513(15) Uani 1 1 d . . . O14 O 1.0408(3) -0.5199(3) 0.3323(3) 0.0482(14) Uani 1 1 d . . . O15 O 1.0615(3) -0.7145(4) 0.2607(3) 0.0546(15) Uani 1 1 d . . . O16 O 0.9593(4) -0.7869(5) 0.1274(3) 0.0670(19) 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 Cl5 0.467(12) 0.313(9) 0.123(4) -0.011(5) -0.017(5) -0.339(10) Cl6 0.179(5) 0.147(4) 0.204(5) 0.050(4) -0.063(4) -0.105(4) Cl7 0.245(7) 0.190(6) 0.183(5) -0.042(4) -0.132(5) -0.029(5) Cl1 0.0592(12) 0.0492(14) 0.0561(13) 0.0002(10) -0.0261(10) -0.0035(10) Cl2 0.0659(15) 0.0372(15) 0.230(4) 0.0144(18) -0.086(2) -0.0190(12) Cl3 0.0828(18) 0.087(2) 0.090(2) -0.0351(17) -0.0430(16) 0.0108(15) Cl4 0.127(3) 0.164(4) 0.0669(19) -0.004(2) -0.0041(18) -0.091(3) Cd1 0.0410(4) 0.0523(5) 0.0634(5) -0.0018(3) -0.0218(3) -0.0099(3) Cd1' 0.036(6) 0.050(8) 0.072(10) 0.015(7) -0.030(6) -0.010(5) O1W 0.106(3) 0.067(3) 0.021(2) -0.0078(19) 0.001(2) -0.049(3) O2W 0.092(5) 0.132(7) 0.027(3) -0.003(4) -0.009(3) -0.051(5) O3W 0.074(4) 0.074(5) 0.068(4) -0.021(4) -0.013(3) -0.036(4) O4W 0.085(4) 0.049(4) 0.063(4) -0.001(3) -0.036(3) -0.016(3) O5W 0.106(3) 0.067(3) 0.021(2) -0.0078(19) 0.001(2) -0.049(3) O6W 0.077(4) 0.110(6) 0.089(5) 0.016(5) -0.046(4) -0.039(4) O7W 0.061(4) 0.076(5) 0.093(5) -0.014(4) 0.015(4) -0.032(4) O8W 0.088(5) 0.204(10) 0.060(4) -0.060(5) 0.015(4) -0.096(6) O9W 0.109(7) 0.134(8) 0.127(8) -0.064(7) 0.027(6) -0.064(6) O10W 0.136(8) 0.087(6) 0.148(9) 0.038(6) -0.074(7) -0.044(6) O11W 0.209(10) 0.125(8) 0.081(6) 0.045(5) -0.085(6) -0.116(8) O12W 0.115(7) 0.211(12) 0.043(4) -0.025(6) -0.012(4) -0.048(7) Ce1 0.0392(2) 0.0514(3) 0.0342(3) -0.0021(2) -0.00828(18) -0.0188(2) Ce2 0.0446(3) 0.0680(4) 0.0383(3) -0.0056(2) -0.0079(2) -0.0277(2) N33 0.031(3) 0.034(4) 0.058(4) 0.010(3) -0.029(3) -0.004(3) O17 0.077(5) 0.097(6) 0.088(5) 0.028(5) -0.029(4) -0.046(4) O18 0.062(4) 0.092(6) 0.093(6) 0.003(5) -0.029(4) -0.025(4) O19 0.091(5) 0.091(6) 0.162(9) 0.033(6) -0.065(6) -0.048(5) C1 0.040(4) 0.030(4) 0.037(4) -0.007(3) -0.009(3) -0.009(3) C2 0.031(3) 0.030(4) 0.037(4) 0.000(3) -0.005(3) -0.009(3) C3 0.032(3) 0.030(4) 0.042(4) -0.008(3) -0.008(3) -0.010(3) C4 0.024(3) 0.040(4) 0.027(4) 0.009(3) -0.011(3) -0.007(3) C5 0.033(3) 0.035(4) 0.038(4) -0.007(3) -0.006(3) -0.013(3) C6 0.029(3) 0.026(4) 0.047(4) 0.001(3) -0.013(3) -0.010(3) C7 0.042(4) 0.036(5) 0.037(4) -0.009(3) -0.007(3) -0.021(3) C8 0.029(3) 0.021(4) 0.039(4) -0.006(3) -0.006(3) -0.008(3) C9 0.027(3) 0.029(4) 0.051(5) -0.001(3) -0.011(3) -0.012(3) C10 0.038(4) 0.039(5) 0.030(4) 0.004(3) -0.007(3) -0.019(3) C11 0.036(4) 0.041(5) 0.029(4) -0.006(3) -0.012(3) -0.006(3) C12 0.032(3) 0.039(5) 0.035(4) -0.008(3) 0.000(3) -0.011(3) C13 0.031(3) 0.042(5) 0.031(4) 0.003(3) -0.009(3) -0.018(3) C14 0.030(3) 0.044(5) 0.036(4) -0.001(3) -0.007(3) -0.020(3) C15 0.028(3) 0.034(4) 0.030(4) 0.001(3) -0.007(3) -0.013(3) C16 0.042(4) 0.052(5) 0.032(4) 0.007(4) -0.013(3) -0.024(4) C17 0.044(4) 0.047(5) 0.019(3) 0.003(3) -0.014(3) -0.019(3) C18 0.052(4) 0.041(5) 0.021(4) 0.001(3) -0.006(3) -0.017(4) C19 0.032(3) 0.037(4) 0.031(4) 0.002(3) -0.014(3) -0.012(3) C20 0.028(3) 0.035(4) 0.033(4) -0.002(3) -0.008(3) -0.010(3) C21 0.033(3) 0.038(4) 0.028(4) -0.007(3) -0.009(3) -0.016(3) C22 0.034(3) 0.038(5) 0.039(4) -0.006(4) -0.012(3) -0.014(3) C23 0.037(4) 0.054(5) 0.034(4) -0.003(4) -0.013(3) -0.025(4) C24 0.053(4) 0.049(5) 0.022(4) 0.000(3) -0.003(3) -0.029(4) C25 0.046(4) 0.069(6) 0.053(6) 0.015(5) -0.017(4) -0.032(4) C26 0.047(4) 0.062(6) 0.035(4) 0.006(4) -0.012(3) -0.026(4) C27 0.035(4) 0.053(5) 0.042(4) -0.006(4) -0.004(3) -0.023(4) C28 0.035(4) 0.051(5) 0.034(4) -0.005(4) -0.012(3) -0.013(4) C29 0.031(4) 0.068(6) 0.055(5) 0.005(5) 0.005(4) -0.018(4) C30 0.038(4) 0.056(5) 0.033(4) -0.005(4) -0.009(3) -0.019(4) C31 0.040(4) 0.076(7) 0.032(4) 0.005(4) 0.001(3) -0.034(4) C32 0.025(3) 0.061(5) 0.029(4) -0.004(4) -0.004(3) -0.018(3) C33 0.023(3) 0.053(5) 0.032(4) -0.012(3) -0.002(3) -0.008(3) C34 0.033(4) 0.052(5) 0.021(3) 0.000(3) -0.008(3) -0.017(3) C35 0.038(4) 0.077(7) 0.044(5) -0.025(4) 0.007(3) -0.031(4) C36 0.047(4) 0.049(5) 0.014(3) -0.006(3) -0.004(3) -0.020(4) C37 0.035(4) 0.051(5) 0.027(4) -0.007(3) 0.002(3) -0.018(3) C38 0.033(4) 0.056(5) 0.034(4) 0.001(4) -0.004(3) -0.016(4) C39 0.049(4) 0.048(5) 0.023(4) -0.005(3) -0.005(3) -0.018(4) C40 0.040(4) 0.055(5) 0.032(4) 0.006(4) -0.015(3) -0.024(4) C41 0.039(4) 0.061(6) 0.037(4) -0.021(4) 0.002(3) -0.014(4) C42 0.068(5) 0.080(7) 0.019(4) 0.002(4) -0.003(3) -0.044(5) C43 0.045(4) 0.063(6) 0.010(3) -0.002(3) 0.000(3) -0.015(4) C44 0.052(4) 0.045(5) 0.032(4) 0.001(4) -0.008(3) -0.026(4) C45 0.045(4) 0.034(4) 0.046(5) -0.005(3) -0.017(3) -0.017(3) C46 0.057(5) 0.054(5) 0.026(4) 0.009(4) -0.007(4) -0.033(4) C47 0.046(4) 0.066(6) 0.028(4) 0.005(4) -0.010(3) -0.012(4) C48 0.060(5) 0.081(7) 0.034(4) 0.021(5) -0.011(4) -0.041(5) N1 0.045(3) 0.039(4) 0.030(3) 0.001(3) -0.008(3) -0.024(3) N2 0.029(3) 0.037(4) 0.041(3) 0.001(3) -0.013(2) -0.011(3) N3 0.035(3) 0.039(4) 0.032(3) 0.000(3) -0.007(2) -0.018(3) N4 0.029(3) 0.039(4) 0.034(3) -0.002(3) -0.005(2) -0.018(3) N5 0.031(3) 0.040(4) 0.031(3) -0.007(3) -0.008(2) -0.004(3) N6 0.031(3) 0.039(4) 0.034(3) -0.005(3) -0.009(2) -0.009(3) N7 0.030(3) 0.042(4) 0.029(3) -0.006(3) -0.007(2) -0.013(3) N8 0.033(3) 0.042(4) 0.027(3) -0.005(3) -0.010(2) -0.012(3) N9 0.031(3) 0.035(4) 0.021(3) -0.006(3) -0.001(2) -0.007(3) N10 0.036(3) 0.042(4) 0.025(3) -0.005(3) -0.008(2) -0.012(3) N11 0.029(3) 0.036(4) 0.027(3) -0.004(3) -0.010(2) -0.003(3) N12 0.037(3) 0.034(4) 0.032(3) -0.007(3) -0.013(3) -0.008(3) N13 0.037(3) 0.037(4) 0.025(3) -0.006(3) -0.009(2) -0.013(3) N14 0.041(3) 0.036(4) 0.039(4) -0.005(3) -0.010(3) -0.017(3) N15 0.039(3) 0.033(4) 0.021(3) 0.001(2) -0.009(2) -0.010(3) N16 0.043(3) 0.039(4) 0.031(3) -0.007(3) -0.007(3) -0.024(3) N17 0.045(4) 0.073(5) 0.024(3) 0.001(3) -0.006(3) -0.027(3) N18 0.034(3) 0.070(5) 0.043(4) 0.003(4) -0.001(3) -0.021(3) N19 0.037(3) 0.060(5) 0.026(3) 0.008(3) -0.007(3) -0.014(3) N20 0.037(3) 0.051(4) 0.033(3) 0.002(3) -0.009(3) -0.019(3) N21 0.036(3) 0.057(5) 0.042(4) -0.002(3) 0.006(3) -0.019(3) N22 0.038(3) 0.068(5) 0.028(3) -0.011(3) 0.000(3) -0.026(3) N23 0.028(3) 0.047(4) 0.032(3) -0.008(3) 0.003(2) -0.012(3) N24 0.029(3) 0.047(4) 0.040(4) -0.009(3) -0.004(3) -0.016(3) N25 0.045(3) 0.069(5) 0.030(4) -0.009(3) 0.005(3) -0.032(3) N26 0.039(3) 0.057(5) 0.036(4) -0.012(3) -0.007(3) -0.015(3) N27 0.039(3) 0.051(4) 0.028(3) -0.012(3) -0.004(3) -0.015(3) N28 0.046(3) 0.067(5) 0.034(4) -0.015(3) -0.004(3) -0.032(3) N29 0.045(3) 0.046(4) 0.041(4) -0.013(3) -0.007(3) -0.024(3) N30 0.044(3) 0.053(4) 0.022(3) 0.004(3) -0.010(3) -0.017(3) N31 0.043(3) 0.067(5) 0.030(3) 0.001(3) -0.005(3) -0.028(3) N32 0.047(4) 0.076(5) 0.029(3) 0.002(3) -0.011(3) -0.034(4) O1 0.062(3) 0.037(3) 0.039(3) 0.003(3) -0.022(3) -0.019(3) O2 0.034(2) 0.049(3) 0.036(3) 0.000(3) -0.002(2) -0.013(2) O3 0.044(3) 0.052(4) 0.031(3) 0.000(2) -0.009(2) -0.014(2) O4 0.047(3) 0.063(4) 0.021(3) -0.003(2) -0.003(2) -0.028(3) O5 0.039(3) 0.043(3) 0.031(3) 0.000(2) -0.005(2) -0.018(2) O6 0.036(3) 0.064(4) 0.042(3) -0.007(3) -0.014(2) -0.014(3) O7 0.065(3) 0.053(4) 0.043(3) -0.008(3) -0.036(3) -0.004(3) O8 0.068(4) 0.060(4) 0.040(3) 0.001(3) -0.028(3) -0.029(3) O9 0.065(4) 0.114(6) 0.032(3) -0.007(4) 0.012(3) -0.040(4) O10 0.064(4) 0.092(5) 0.037(3) -0.008(3) 0.008(3) -0.028(4) O11 0.070(4) 0.078(5) 0.037(3) -0.002(3) -0.004(3) -0.041(3) O12 0.071(4) 0.089(5) 0.033(3) 0.012(3) -0.009(3) -0.049(4) O13 0.039(3) 0.066(4) 0.044(3) 0.013(3) -0.006(2) -0.025(3) O14 0.029(2) 0.057(4) 0.050(3) -0.001(3) 0.000(2) -0.017(2) O15 0.039(3) 0.077(4) 0.043(3) -0.013(3) 0.003(2) -0.025(3) O16 0.056(3) 0.106(6) 0.030(3) -0.004(3) 0.000(3) -0.030(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 Cl1 Cd1 2.416(2) . ? Cl1 Cd1' 2.559(14) . ? Cl2 Cd1 2.435(2) . ? Cl2 Cd1' 2.548(12) . ? Cl3 Cd1' 2.062(14) . ? Cl3 Cd1 2.483(3) . ? Cl4 Cd1 2.457(3) . ? O1W Ce1 2.709(6) 2_844 ? O2W Ce1 2.535(6) . ? O3W Ce1 2.571(6) . ? O4W Ce1 2.520(7) . ? O5W Ce1 2.524(7) . ? O6W Ce2 2.596(7) . ? O7W Ce2 2.541(7) . ? O8W Ce2 2.528(7) . ? O9W Ce2 2.596(9) . ? O10W Ce2 2.533(8) . ? O11W Ce2 2.513(9) . ? O12W Ce2 2.557(8) . ? Ce1 O2 2.447(5) . ? Ce1 O1 2.523(5) . ? Ce1 O18 2.567(7) . ? Ce1 O17 2.658(7) . ? Ce1 O1W 2.709(6) 2_844 ? Ce1 N33 3.022(6) . ? Ce2 O6 2.536(6) . ? Ce2 O5 2.558(5) . ? N33 O18 1.177(9) . ? N33 O19 1.241(10) . ? N33 O17 1.320(9) . ? C1 O1 1.225(8) . ? C1 N1 1.355(9) . ? C1 N2 1.361(9) . ? C2 N1 1.448(9) . ? C2 N3 1.470(9) . ? C2 C3 1.547(9) . ? C2 H2 0.9900 . ? C3 N4 1.446(9) . ? C3 N2 1.452(9) . ? C3 H3 0.9900 . ? C4 O5 1.221(8) . ? C4 N4 1.357(10) . ? C4 N3 1.376(8) . ? C5 N5 1.448(8) . ? C5 N2 1.455(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.430(8) . ? C6 N4 1.485(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.251(8) . ? C7 N6 1.342(9) . ? C7 N5 1.344(9) . ? C8 N5 1.428(9) . ? C8 N7 1.452(9) . ? C8 C9 1.562(9) . ? C8 H8 0.9900 . ? C9 N8 1.443(9) . ? C9 N6 1.474(9) . ? C9 H9 0.9900 . ? C10 O6 1.216(9) . ? C10 N8 1.359(9) . ? C10 N7 1.377(9) . ? C11 N9 1.447(9) . ? C11 N6 1.453(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.419(9) . ? C12 N8 1.459(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.235(8) . ? C13 N9 1.340(9) . ? C13 N10 1.370(9) . ? C14 N9 1.465(8) . ? C14 N11 1.460(9) . ? C14 C15 1.542(10) . ? C14 H14 0.9900 . ? C15 N10 1.445(8) . ? C15 N12 1.458(9) . ? C15 H15 0.9900 . ? C16 O7 1.248(9) . ? C16 N11 1.330(10) . ? C16 N12 1.366(9) . ? C17 N13 1.432(9) . ? C17 N10 1.460(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.453(9) . ? C18 N12 1.482(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.226(8) . ? C19 N13 1.361(9) . ? C19 N14 1.368(9) . ? C20 N13 1.446(9) . ? C20 N15 1.455(8) . ? C20 C21 1.534(10) . ? C20 H20 0.9900 . ? C21 N14 1.446(9) . ? C21 N16 1.468(9) . ? C21 H21 0.9900 . ? C22 O8 1.205(8) . ? C22 N16 1.361(9) . ? C22 N15 1.366(10) . ? C23 N3 1.440(9) . ? C23 N14 1.463(10) 2_844 ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.436(10) 2_844 ? C24 N1 1.452(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O9 1.229(10) . ? C25 N18 1.343(10) . ? C25 N17 1.384(11) . ? C26 N17 1.453(10) . ? C26 N19 1.463(9) . ? C26 C27 1.515(11) . ? C26 H26 0.9900 . ? C27 N18 1.442(10) . ? C27 N20 1.462(9) . ? C27 H27 0.9900 . ? C28 O13 1.218(9) . ? C28 N20 1.361(9) . ? C28 N19 1.373(10) . ? C29 N21 1.449(11) . ? C29 N18 1.470(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.434(9) . ? C30 N23 1.439(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O10 1.214(9) . ? C31 N22 1.357(10) . ? C31 N21 1.364(11) . ? C32 N21 1.456(9) . ? C32 N23 1.472(8) . ? C32 C33 1.509(11) . ? C32 H32 0.9900 . ? C33 N22 1.453(9) . ? C33 N24 1.464(9) . ? C33 H33 0.9900 . ? C34 O14 1.196(8) . ? C34 N23 1.377(10) . ? C34 N24 1.385(9) . ? C35 N22 1.440(11) . ? C35 N25 1.455(10) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.425(10) . ? C36 N27 1.454(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O11 1.209(9) . ? C37 N25 1.344(10) . ? C37 N26 1.377(10) . ? C38 N27 1.442(9) . ? C38 N25 1.460(10) . ? C38 C39 1.549(12) . ? C38 H38 0.9900 . ? C39 N28 1.443(9) . ? C39 N26 1.454(9) . ? C39 H39 0.9900 . ? C40 O15 1.218(9) . ? C40 N27 1.381(9) . ? C40 N28 1.377(10) . ? C41 N29 1.432(10) . ? C41 N26 1.445(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N28 1.410(10) . ? C42 N31 1.467(10) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O12 1.175(9) . ? C43 N30 1.376(10) . ? C43 N29 1.411(9) . ? C44 N31 1.447(10) . ? C44 N29 1.447(9) . ? C44 C45 1.524(11) . ? C44 H44 0.9900 . ? C45 N32 1.452(10) . ? C45 N30 1.461(9) . ? C45 H45 0.9900 . ? C46 O16 1.226(9) . ? C46 N32 1.349(10) . ? C46 N31 1.370(10) . ? C47 N30 1.421(10) 2_745 ? C47 N19 1.463(9) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N17 1.434(10) . ? C48 N32 1.458(10) 2_745 ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? N14 C23 1.463(10) 2_844 ? N16 C24 1.436(10) 2_844 ? N30 C47 1.421(10) 2_745 ? N32 C48 1.458(10) 2_745 ? 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 Cd1 Cl1 Cd1' 31.5(3) . . ? Cd1 Cl2 Cd1' 31.5(3) . . ? Cd1' Cl3 Cd1 33.1(4) . . ? Cl1 Cd1 Cl2 108.24(8) . . ? Cl1 Cd1 Cl4 121.01(12) . . ? Cl2 Cd1 Cl4 101.93(14) . . ? Cl1 Cd1 Cl3 113.97(10) . . ? Cl2 Cd1 Cl3 108.23(11) . . ? Cl4 Cd1 Cl3 102.31(13) . . ? Cl3 Cd1' Cl2 119.3(5) . . ? Cl3 Cd1' Cl1 125.2(5) . . ? Cl2 Cd1' Cl1 100.6(5) . . ? O2 Ce1 O4W 73.1(2) . . ? O2 Ce1 O1 81.28(16) . . ? O4W Ce1 O1 73.26(19) . . ? O2 Ce1 O5W 101.16(17) . . ? O4W Ce1 O5W 141.6(2) . . ? O1 Ce1 O5W 68.31(19) . . ? O2 Ce1 O2W 136.9(2) . . ? O4W Ce1 O2W 135.1(2) . . ? O1 Ce1 O2W 131.9(2) . . ? O5W Ce1 O2W 75.0(2) . . ? O2 Ce1 O3W 66.39(19) . . ? O4W Ce1 O3W 131.6(2) . . ? O1 Ce1 O3W 123.1(2) . . ? O5W Ce1 O3W 73.6(2) . . ? O2W Ce1 O3W 71.6(2) . . ? O2 Ce1 O18 79.1(2) . . ? O4W Ce1 O18 75.6(2) . . ? O1 Ce1 O18 146.9(2) . . ? O5W Ce1 O18 141.8(2) . . ? O2W Ce1 O18 79.3(3) . . ? O3W Ce1 O18 71.7(2) . . ? O2 Ce1 O17 119.1(2) . . ? O4W Ce1 O17 66.7(2) . . ? O1 Ce1 O17 124.8(2) . . ? O5W Ce1 O17 138.4(2) . . ? O2W Ce1 O17 68.7(3) . . ? O3W Ce1 O17 111.8(2) . . ? O18 Ce1 O17 48.3(2) . . ? O2 Ce1 O1W 141.56(17) . 2_844 ? O4W Ce1 O1W 81.8(2) . 2_844 ? O1 Ce1 O1W 63.57(18) . 2_844 ? O5W Ce1 O1W 80.77(19) . 2_844 ? O2W Ce1 O1W 81.1(2) . 2_844 ? O3W Ce1 O1W 146.34(19) . 2_844 ? O18 Ce1 O1W 122.6(2) . 2_844 ? O17 Ce1 O1W 74.3(2) . 2_844 ? O2 Ce1 N33 98.01(17) . . ? O4W Ce1 N33 69.79(19) . . ? O1 Ce1 N33 141.44(18) . . ? O5W Ce1 N33 147.22(19) . . ? O2W Ce1 N33 72.8(2) . . ? O3W Ce1 N33 90.4(2) . . ? O18 Ce1 N33 22.47(19) . . ? O17 Ce1 N33 25.86(19) . . ? O1W Ce1 N33 100.12(19) 2_844 . ? O11W Ce2 O10W 139.7(3) . . ? O11W Ce2 O8W 86.4(4) . . ? O10W Ce2 O8W 80.4(3) . . ? O11W Ce2 O6 70.7(2) . . ? O10W Ce2 O6 69.1(3) . . ? O8W Ce2 O6 66.2(2) . . ? O11W Ce2 O7W 141.1(3) . . ? O10W Ce2 O7W 71.1(3) . . ? O8W Ce2 O7W 129.1(3) . . ? O6 Ce2 O7W 133.1(2) . . ? O11W Ce2 O12W 74.1(3) . . ? O10W Ce2 O12W 135.6(4) . . ? O8W Ce2 O12W 73.4(3) . . ? O6 Ce2 O12W 127.1(3) . . ? O7W Ce2 O12W 98.7(3) . . ? O11W Ce2 O5 84.0(3) . . ? O10W Ce2 O5 85.6(3) . . ? O8W Ce2 O5 145.15(19) . . ? O6 Ce2 O5 78.97(16) . . ? O7W Ce2 O5 74.24(19) . . ? O12W Ce2 O5 134.6(3) . . ? O11W Ce2 O6W 71.7(3) . . ? O10W Ce2 O6W 137.5(3) . . ? O8W Ce2 O6W 139.3(3) . . ? O6 Ce2 O6W 131.5(2) . . ? O7W Ce2 O6W 70.3(3) . . ? O12W Ce2 O6W 67.9(3) . . ? O5 Ce2 O6W 67.6(2) . . ? O11W Ce2 O9W 136.4(3) . . ? O10W Ce2 O9W 71.3(4) . . ? O8W Ce2 O9W 67.2(3) . . ? O6 Ce2 O9W 122.3(3) . . ? O7W Ce2 O9W 64.1(2) . . ? O12W Ce2 O9W 65.6(4) . . ? O5 Ce2 O9W 136.9(2) . . ? O6W Ce2 O9W 106.1(3) . . ? O18 N33 O19 127.8(7) . . ? O18 N33 O17 117.9(7) . . ? O19 N33 O17 114.2(7) . . ? O18 N33 Ce1 56.5(4) . . ? O19 N33 Ce1 175.1(6) . . ? O17 N33 Ce1 61.5(4) . . ? N33 O17 Ce1 92.7(5) . . ? N33 O18 Ce1 101.1(5) . . ? O1 C1 N1 126.2(7) . . ? O1 C1 N2 125.2(7) . . ? N1 C1 N2 108.5(6) . . ? N1 C2 N3 113.4(6) . . ? N1 C2 C3 103.1(6) . . ? N3 C2 C3 103.1(5) . . ? N1 C2 H2 112.2 . . ? N3 C2 H2 112.2 . . ? C3 C2 H2 112.2 . . ? N4 C3 N2 113.5(5) . . ? N4 C3 C2 103.4(6) . . ? N2 C3 C2 103.0(6) . . ? N4 C3 H3 112.1 . . ? N2 C3 H3 112.1 . . ? C2 C3 H3 112.1 . . ? O5 C4 N4 126.3(6) . . ? O5 C4 N3 125.1(7) . . ? N4 C4 N3 108.4(6) . . ? N5 C5 N2 113.5(6) . . ? N5 C5 H5A 108.9 . . ? N2 C5 H5A 108.9 . . ? N5 C5 H5B 108.9 . . ? N2 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 112.4(5) . . ? N7 C6 H6A 109.1 . . ? N4 C6 H6A 109.1 . . ? N7 C6 H6B 109.1 . . ? N4 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N6 124.9(7) . . ? O2 C7 N5 124.4(6) . . ? N6 C7 N5 110.5(6) . . ? N5 C8 N7 115.3(5) . . ? N5 C8 C9 103.6(5) . . ? N7 C8 C9 102.7(5) . . ? N5 C8 H8 111.5 . . ? N7 C8 H8 111.5 . . ? C9 C8 H8 111.5 . . ? N8 C9 N6 114.7(6) . . ? N8 C9 C8 104.0(5) . . ? N6 C9 C8 102.1(5) . . ? N8 C9 H9 111.8 . . ? N6 C9 H9 111.8 . . ? C8 C9 H9 111.8 . . ? O6 C10 N8 126.1(7) . . ? O6 C10 N7 124.8(7) . . ? N8 C10 N7 109.1(6) . . ? N9 C11 N6 114.1(6) . . ? N9 C11 H11A 108.7 . . ? N6 C11 H11A 108.7 . . ? N9 C11 H11B 108.7 . . ? N6 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N11 C12 N8 113.9(6) . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12B 108.8 . . ? N8 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 126.2(7) . . ? O3 C13 N10 124.7(7) . . ? N9 C13 N10 109.1(6) . . ? N9 C14 N11 114.1(5) . . ? N9 C14 C15 103.1(5) . . ? N11 C14 C15 103.6(6) . . ? N9 C14 H14 111.8 . . ? N11 C14 H14 111.8 . . ? C15 C14 H14 111.8 . . ? N10 C15 N12 114.6(6) . . ? N10 C15 C14 103.0(5) . . ? N12 C15 C14 102.5(5) . . ? N10 C15 H15 112.0 . . ? N12 C15 H15 112.0 . . ? C14 C15 H15 112.0 . . ? O7 C16 N11 126.0(7) . . ? O7 C16 N12 123.9(8) . . ? N11 C16 N12 110.1(6) . . ? N13 C17 N10 112.6(5) . . ? N13 C17 H17A 109.1 . . ? N10 C17 H17A 109.1 . . ? N13 C17 H17B 109.1 . . ? N10 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? N15 C18 N12 112.7(5) . . ? N15 C18 H18A 109.0 . . ? N12 C18 H18A 109.0 . . ? N15 C18 H18B 109.0 . . ? N12 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N13 125.1(7) . . ? O4 C19 N14 126.3(7) . . ? N13 C19 N14 108.6(6) . . ? N13 C20 N15 113.3(5) . . ? N13 C20 C21 102.6(5) . . ? N15 C20 C21 104.1(5) . . ? N13 C20 H20 112.1 . . ? N15 C20 H20 112.1 . . ? C21 C20 H20 112.1 . . ? N14 C21 N16 113.2(5) . . ? N14 C21 C20 104.5(6) . . ? N16 C21 C20 102.3(5) . . ? N14 C21 H21 112.1 . . ? N16 C21 H21 112.1 . . ? C20 C21 H21 112.1 . . ? O8 C22 N16 125.4(7) . . ? O8 C22 N15 126.6(7) . . ? N16 C22 N15 108.0(6) . . ? N3 C23 N14 113.3(6) . 2_844 ? N3 C23 H23A 108.9 . . ? N14 C23 H23A 108.9 2_844 . ? N3 C23 H23B 108.9 . . ? N14 C23 H23B 108.9 2_844 . ? H23A C23 H23B 107.7 . . ? N16 C24 N1 113.9(6) 2_844 . ? N16 C24 H24A 108.8 2_844 . ? N1 C24 H24A 108.8 . . ? N16 C24 H24B 108.8 2_844 . ? N1 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? O9 C25 N18 127.1(8) . . ? O9 C25 N17 124.7(8) . . ? N18 C25 N17 108.2(7) . . ? N17 C26 N19 113.9(7) . . ? N17 C26 C27 104.3(7) . . ? N19 C26 C27 103.6(6) . . ? N17 C26 H26 111.5 . . ? N19 C26 H26 111.5 . . ? C27 C26 H26 111.5 . . ? N18 C27 N20 114.2(7) . . ? N18 C27 C26 103.4(6) . . ? N20 C27 C26 104.5(6) . . ? N18 C27 H27 111.4 . . ? N20 C27 H27 111.4 . . ? C26 C27 H27 111.4 . . ? O13 C28 N20 125.8(7) . . ? O13 C28 N19 125.1(7) . . ? N20 C28 N19 109.1(6) . . ? N21 C29 N18 112.5(7) . . ? N21 C29 H29A 109.1 . . ? N18 C29 H29A 109.1 . . ? N21 C29 H29B 109.1 . . ? N18 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? N20 C30 N23 114.0(6) . . ? N20 C30 H30A 108.7 . . ? N23 C30 H30A 108.7 . . ? N20 C30 H30B 108.7 . . ? N23 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? O10 C31 N22 126.8(9) . . ? O10 C31 N21 124.5(8) . . ? N22 C31 N21 108.6(6) . . ? N21 C32 N23 114.1(6) . . ? N21 C32 C33 104.0(6) . . ? N23 C32 C33 104.0(6) . . ? N21 C32 H32 111.4 . . ? N23 C32 H32 111.4 . . ? C33 C32 H32 111.4 . . ? N22 C33 N24 114.0(6) . . ? N22 C33 C32 103.9(6) . . ? N24 C33 C32 104.4(5) . . ? N22 C33 H33 111.4 . . ? N24 C33 H33 111.4 . . ? C32 C33 H33 111.4 . . ? O14 C34 N23 126.2(7) . . ? O14 C34 N24 126.3(7) . . ? N23 C34 N24 107.6(5) . . ? N22 C35 N25 113.6(6) . . ? N22 C35 H35A 108.9 . . ? N25 C35 H35A 108.9 . . ? N22 C35 H35B 108.9 . . ? N25 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? N24 C36 N27 113.7(6) . . ? N24 C36 H36A 108.8 . . ? N27 C36 H36A 108.8 . . ? N24 C36 H36B 108.8 . . ? N27 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? O11 C37 N25 126.0(8) . . ? O11 C37 N26 125.8(7) . . ? N25 C37 N26 108.2(6) . . ? N27 C38 N25 114.0(7) . . ? N27 C38 C39 103.1(6) . . ? N25 C38 C39 102.4(6) . . ? N27 C38 H38 112.2 . . ? N25 C38 H38 112.2 . . ? C39 C38 H38 112.2 . . ? N28 C39 N26 114.9(6) . . ? N28 C39 C38 104.1(6) . . ? N26 C39 C38 103.5(6) . . ? N28 C39 H39 111.3 . . ? N26 C39 H39 111.3 . . ? C38 C39 H39 111.3 . . ? O15 C40 N27 125.8(8) . . ? O15 C40 N28 126.4(7) . . ? N27 C40 N28 107.8(6) . . ? N29 C41 N26 112.8(6) . . ? N29 C41 H41A 109.0 . . ? N26 C41 H41A 109.0 . . ? N29 C41 H41B 109.0 . . ? N26 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? N28 C42 N31 114.3(6) . . ? N28 C42 H42A 108.7 . . ? N31 C42 H42A 108.7 . . ? N28 C42 H42B 108.7 . . ? N31 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? O12 C43 N30 128.3(7) . . ? O12 C43 N29 125.3(7) . . ? N30 C43 N29 106.3(6) . . ? N31 C44 N29 113.3(7) . . ? N31 C44 C45 103.6(6) . . ? N29 C44 C45 104.6(6) . . ? N31 C44 H44 111.6 . . ? N29 C44 H44 111.6 . . ? C45 C44 H44 111.6 . . ? N32 C45 N30 114.4(6) . . ? N32 C45 C44 103.6(6) . . ? N30 C45 C44 103.4(6) . . ? N32 C45 H45 111.6 . . ? N30 C45 H45 111.6 . . ? C44 C45 H45 111.6 . . ? O16 C46 N32 125.1(7) . . ? O16 C46 N31 126.2(8) . . ? N32 C46 N31 108.6(7) . . ? N30 C47 N19 114.1(7) 2_745 . ? N30 C47 H47A 108.7 2_745 . ? N19 C47 H47A 108.7 . . ? N30 C47 H47B 108.7 2_745 . ? N19 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? N17 C48 N32 112.9(7) . 2_745 ? N17 C48 H48A 109.0 . . ? N32 C48 H48A 109.0 2_745 . ? N17 C48 H48B 109.0 . . ? N32 C48 H48B 109.0 2_745 . ? H48A C48 H48B 107.8 . . ? C1 N1 C2 112.6(6) . . ? C1 N1 C24 122.6(6) . . ? C2 N1 C24 124.4(6) . . ? C1 N2 C3 112.5(6) . . ? C1 N2 C5 123.5(6) . . ? C3 N2 C5 123.8(6) . . ? C4 N3 C23 123.4(6) . . ? C4 N3 C2 111.7(6) . . ? C23 N3 C2 122.5(5) . . ? C4 N4 C3 113.2(5) . . ? C4 N4 C6 123.1(6) . . ? C3 N4 C6 123.4(6) . . ? C7 N5 C8 112.5(5) . . ? C7 N5 C5 124.9(6) . . ? C8 N5 C5 121.7(6) . . ? C7 N6 C11 123.0(6) . . ? C7 N6 C9 111.2(6) . . ? C11 N6 C9 121.4(5) . . ? C10 N7 C6 123.4(6) . . ? C10 N7 C8 112.1(5) . . ? C6 N7 C8 124.0(6) . . ? C10 N8 C9 112.2(6) . . ? C10 N8 C12 123.4(6) . . ? C9 N8 C12 122.2(5) . . ? C13 N9 C11 120.3(6) . . ? C13 N9 C14 111.9(5) . . ? C11 N9 C14 122.7(6) . . ? C13 N10 C15 112.2(6) . . ? C13 N10 C17 123.1(6) . . ? C15 N10 C17 123.7(5) . . ? C16 N11 C12 122.8(6) . . ? C16 N11 C14 111.7(6) . . ? C12 N11 C14 122.4(6) . . ? C16 N12 C15 111.2(6) . . ? C16 N12 C18 122.5(6) . . ? C15 N12 C18 120.6(6) . . ? C19 N13 C17 122.9(6) . . ? C19 N13 C20 112.7(6) . . ? C17 N13 C20 121.4(6) . . ? C19 N14 C21 110.9(6) . . ? C19 N14 C23 121.1(6) . 2_844 ? C21 N14 C23 123.0(6) . 2_844 ? C22 N15 C18 120.0(6) . . ? C22 N15 C20 111.8(6) . . ? C18 N15 C20 121.5(6) . . ? C22 N16 C24 123.6(6) . 2_844 ? C22 N16 C21 112.8(6) . . ? C24 N16 C21 121.1(6) 2_844 . ? C25 N17 C48 123.3(6) . . ? C25 N17 C26 110.7(6) . . ? C48 N17 C26 122.8(7) . . ? C25 N18 C27 113.2(7) . . ? C25 N18 C29 122.6(7) . . ? C27 N18 C29 123.2(7) . . ? C28 N19 C26 111.3(6) . . ? C28 N19 C47 122.3(6) . . ? C26 N19 C47 123.8(7) . . ? C28 N20 C30 123.1(6) . . ? C28 N20 C27 111.0(6) . . ? C30 N20 C27 122.1(6) . . ? C31 N21 C32 111.0(7) . . ? C31 N21 C29 123.0(6) . . ? C32 N21 C29 122.1(7) . . ? C31 N22 C35 121.8(6) . . ? C31 N22 C33 111.4(7) . . ? C35 N22 C33 122.6(7) . . ? C34 N23 C30 122.6(5) . . ? C34 N23 C32 111.8(6) . . ? C30 N23 C32 123.9(6) . . ? C34 N24 C36 122.3(6) . . ? C34 N24 C33 111.7(6) . . ? C36 N24 C33 123.2(6) . . ? C37 N25 C35 121.5(6) . . ? C37 N25 C38 113.3(7) . . ? C35 N25 C38 121.6(7) . . ? C37 N26 C41 123.8(6) . . ? C37 N26 C39 112.1(6) . . ? C41 N26 C39 121.6(7) . . ? C40 N27 C38 112.8(6) . . ? C40 N27 C36 122.5(6) . . ? C38 N27 C36 123.6(6) . . ? C40 N28 C42 121.6(6) . . ? C40 N28 C39 112.1(6) . . ? C42 N28 C39 123.2(7) . . ? C43 N29 C41 122.4(6) . . ? C43 N29 C44 112.2(6) . . ? C41 N29 C44 123.0(7) . . ? C43 N30 C47 120.5(6) . 2_745 ? C43 N30 C45 113.2(5) . . ? C47 N30 C45 122.2(7) 2_745 . ? C46 N31 C44 111.4(6) . . ? C46 N31 C42 121.5(6) . . ? C44 N31 C42 120.9(7) . . ? C46 N32 C48 123.5(6) . 2_745 ? C46 N32 C45 112.1(6) . . ? C48 N32 C45 121.4(7) 2_745 . ? C1 O1 Ce1 153.0(5) . . ? C7 O2 Ce1 154.8(5) . . ? C4 O5 Ce2 156.4(4) . . ? C10 O6 Ce2 150.9(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.587 _refine_diff_density_min -1.400 _refine_diff_density_rms 0.141 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.094 0.500 1.094 666 249 ' ' 2 0.395 -0.004 0.233 155 56 ' ' 3 0.111 0.969 0.761 30 10 ' ' 4 0.271 0.891 1.049 45 19 ' ' 5 0.602 0.004 0.767 150 63 ' ' 6 0.469 0.584 0.011 22 10 ' ' 7 0.534 0.408 0.988 19 8 ' ' 8 0.729 0.110 0.949 45 21 ' ' 9 0.884 0.031 0.236 27 14 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952098' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H240 Cd2 Cl14 N66 Nd4 O110' _chemical_formula_weight 5377.60 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.1436(6) _cell_length_b 18.0998(6) _cell_length_c 18.3169(6) _cell_angle_alpha 84.8960(10) _cell_angle_beta 65.7330(10) _cell_angle_gamma 71.5460(10) _cell_volume 4909.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2732 _exptl_absorpt_coefficient_mu 1.564 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6264 _exptl_absorpt_correction_T_max 0.6775 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48500 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17027 _reflns_number_gt 12318 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1218P)^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 17027 _refine_ls_number_parameters 1109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1934 _refine_ls_wR_factor_gt 0.1760 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Cl5 Cl 0.7225(2) 0.08596(16) 0.83866(19) 0.0807(8) Uani 1 1 d . . . Cl6 Cl 1.02497(17) 0.07504(16) 0.08270(18) 0.0763(7) Uani 1 1 d . . . Cl7 Cl 0.9288(3) -0.3303(2) 0.0252(2) 0.1004(11) Uani 1 1 d . . . N33 N 0.9961(4) -0.8149(4) 0.4214(4) 0.0448(15) Uani 1 1 d . . . O1W O 1.1246(6) -0.2218(4) 0.1143(5) 0.082(2) Uani 1 1 d . . . O2W O 1.2517(4) -0.2513(4) 0.1921(4) 0.0663(17) Uani 1 1 d . . . O3W O 0.9403(5) -0.1840(4) 0.2657(6) 0.111(3) Uani 1 1 d . . . O4W O 1.1615(4) -0.3017(4) 0.3537(4) 0.0687(18) Uani 1 1 d . . . O5W O 1.0918(5) -0.1264(4) 0.2609(4) 0.080(2) Uani 1 1 d . . . O6W O 0.9952(5) -0.1948(4) 0.3923(5) 0.090(2) Uani 1 1 d . . . O7W O 1.0181(6) -0.3529(5) 0.3464(4) 0.090(2) Uani 1 1 d . . . O8W O 1.0319(3) -0.8059(3) 0.1934(3) 0.0433(12) Uani 1 1 d . . . O9W O 1.1383(4) -0.9278(3) 0.2630(4) 0.0591(16) Uani 1 1 d . . . O10W O 1.2272(4) -0.8397(4) 0.1214(4) 0.0609(16) Uani 1 1 d . . . O11W O 1.0944(4) -0.6862(3) 0.3626(3) 0.0613(16) Uani 1 1 d . . . O12W O 1.2609(4) -0.8508(4) 0.2872(5) 0.077(2) Uani 1 1 d . . . O17 O 1.0809(4) -0.8381(4) 0.4058(4) 0.0684(18) Uani 1 1 d . . . O18 O 0.9752(4) -0.7772(5) 0.3673(4) 0.0695(19) Uani 1 1 d . . . O19 O 0.9410(4) -0.8248(4) 0.4912(4) 0.0625(16) Uani 1 1 d . . . Nd1 Nd 1.09318(3) -0.26346(2) 0.25283(3) 0.04502(15) Uani 1 1 d . . . Nd2 Nd 1.12820(2) -0.78659(2) 0.25757(2) 0.03135(13) Uani 1 1 d . . . Cl1 Cl 0.41433(14) 0.50917(12) 0.67837(13) 0.0538(5) Uani 1 1 d . . . Cl2 Cl 0.23901(14) 0.44949(17) 0.88464(13) 0.0672(7) Uani 1 1 d . . . Cl3 Cl 0.37440(16) 0.58858(16) 0.89342(17) 0.0758(7) Uani 1 1 d . . . Cl4 Cl 0.48846(18) 0.36455(15) 0.8442(2) 0.0802(8) Uani 1 1 d . . . Cd1 Cd 0.38008(4) 0.47835(4) 0.81741(4) 0.0455(3) Uani 0.965(2) 1 d P A 1 Cd1' Cd 0.3396(10) 0.5423(13) 0.8393(10) 0.049(7) Uani 0.035(2) 1 d P A 2 C1 C 1.2534(4) -0.4529(4) 0.1612(4) 0.0307(15) Uani 1 1 d . . . C2 C 1.3563(4) -0.5789(4) 0.1252(4) 0.0314(15) Uani 1 1 d . . . H2 H 1.4205 -0.5897 0.0888 0.038 Uiso 1 1 calc R . . C3 C 1.2952(4) -0.5624(4) 0.0784(4) 0.0311(14) Uani 1 1 d . . . H3 H 1.3304 -0.5691 0.0196 0.037 Uiso 1 1 calc R . . C4 C 1.2729(4) -0.6661(4) 0.1630(4) 0.0298(15) Uani 1 1 d . . . C5 C 1.1752(4) -0.4365(4) 0.0700(4) 0.0326(15) Uani 1 1 d . . . H5A H 1.1723 -0.3816 0.0712 0.039 Uiso 1 1 calc R . . H5B H 1.1973 -0.4537 0.0138 0.039 Uiso 1 1 calc R . . C6 C 1.1830(4) -0.6330(4) 0.0824(4) 0.0328(15) Uani 1 1 d . . . H6A H 1.2019 -0.6249 0.0248 0.039 Uiso 1 1 calc R . . H6B H 1.1821 -0.6870 0.0912 0.039 Uiso 1 1 calc R . . C7 C 1.0183(4) -0.3884(4) 0.1682(4) 0.0292(14) Uani 1 1 d . . . C8 C 1.0558(4) -0.5048(4) 0.0976(4) 0.0279(14) Uani 1 1 d . . . H8 H 1.0648 -0.5081 0.0409 0.034 Uiso 1 1 calc R . . C9 C 0.9547(4) -0.4803(4) 0.1559(4) 0.0312(15) Uani 1 1 d . . . H9 H 0.9149 -0.4722 0.1272 0.037 Uiso 1 1 calc R . . C10 C 1.0294(4) -0.6030(4) 0.1898(4) 0.0301(15) Uani 1 1 d . . . C11 C 0.8536(4) -0.3539(4) 0.2344(4) 0.0311(15) Uani 1 1 d . . . H11A H 0.8599 -0.3027 0.2387 0.037 Uiso 1 1 calc R . . H11B H 0.8205 -0.3492 0.2006 0.037 Uiso 1 1 calc R . . C12 C 0.8629(4) -0.5601(4) 0.2542(4) 0.0335(15) Uani 1 1 d . . . H12A H 0.8301 -0.5520 0.2197 0.040 Uiso 1 1 calc R . . H12B H 0.8745 -0.6147 0.2687 0.040 Uiso 1 1 calc R . . C13 C 0.7740(5) -0.3324(4) 0.3821(5) 0.0402(17) Uani 1 1 d . . . C14 C 0.7540(4) -0.4296(4) 0.3258(4) 0.0297(14) Uani 1 1 d . . . H14 H 0.7256 -0.4238 0.2873 0.036 Uiso 1 1 calc R . . C15 C 0.6828(4) -0.4121(4) 0.4116(4) 0.0277(14) Uani 1 1 d . . . H15 H 0.6211 -0.3902 0.4139 0.033 Uiso 1 1 calc R . . C16 C 0.7679(4) -0.5430(4) 0.3973(4) 0.0330(15) Uani 1 1 d . . . C17 C 0.6476(5) -0.3062(4) 0.5121(4) 0.0362(16) Uani 1 1 d . . . H17A H 0.5875 -0.2896 0.5117 0.043 Uiso 1 1 calc R . . H17B H 0.6658 -0.2595 0.5091 0.043 Uiso 1 1 calc R . . C18 C 0.6319(4) -0.5035(4) 0.5236(4) 0.0321(15) Uani 1 1 d . . . H18A H 0.5712 -0.4805 0.5250 0.039 Uiso 1 1 calc R . . H18B H 0.6439 -0.5601 0.5261 0.039 Uiso 1 1 calc R . . C19 C 0.6527(4) -0.3059(4) 0.6447(4) 0.0301(14) Uani 1 1 d . . . C20 C 0.5887(4) -0.3949(4) 0.6230(4) 0.0287(14) Uani 1 1 d . . . H20 H 0.5291 -0.3748 0.6203 0.034 Uiso 1 1 calc R . . C21 C 0.5805(4) -0.3982(4) 0.7102(4) 0.0288(14) Uani 1 1 d . . . H21 H 0.5171 -0.3859 0.7493 0.035 Uiso 1 1 calc R . . C22 C 0.6577(4) -0.5225(4) 0.6470(4) 0.0324(15) Uani 1 1 d . . . C23 C 0.6030(4) -0.3063(3) 0.7911(4) 0.0279(14) Uani 1 1 d . . . H23A H 0.5400 -0.2990 0.8271 0.033 Uiso 1 1 calc R . . H23B H 0.6119 -0.2548 0.7826 0.033 Uiso 1 1 calc R . . C24 C 0.6259(4) -0.5129(4) 0.7907(4) 0.0313(15) Uani 1 1 d . . . H24A H 0.5627 -0.4966 0.8286 0.038 Uiso 1 1 calc R . . H24B H 0.6455 -0.5697 0.7829 0.038 Uiso 1 1 calc R . . C25 C 0.7372(5) -0.1179(4) 0.1875(4) 0.0391(17) Uani 1 1 d . . . C26 C 0.6354(4) -0.0625(4) 0.1270(4) 0.0362(16) Uani 1 1 d . . . H26 H 0.6437 -0.0821 0.0748 0.043 Uiso 1 1 calc R . . C27 C 0.6946(4) -0.0073(4) 0.1173(4) 0.0321(15) Uani 1 1 d . . . H27 H 0.7304 -0.0004 0.0603 0.039 Uiso 1 1 calc R . . C28 C 0.5421(5) 0.0624(4) 0.1853(4) 0.0408(17) Uani 1 1 d . . . C29 C 0.8312(4) -0.0288(4) 0.1470(5) 0.0419(18) Uani 1 1 d . . . H29A H 0.8729 -0.0746 0.1586 0.050 Uiso 1 1 calc R . . H29B H 0.8607 -0.0174 0.0908 0.050 Uiso 1 1 calc R . . C30 C 0.6482(6) 0.1383(4) 0.1470(5) 0.048(2) Uani 1 1 d . . . H30A H 0.5928 0.1815 0.1571 0.057 Uiso 1 1 calc R . . H30B H 0.6893 0.1395 0.0910 0.057 Uiso 1 1 calc R . . C31 C 0.8442(4) 0.0288(4) 0.2558(5) 0.0380(17) Uani 1 1 d . . . C32 C 0.7867(4) 0.1162(4) 0.1770(4) 0.0339(15) Uani 1 1 d . . . H32 H 0.8226 0.1240 0.1203 0.041 Uiso 1 1 calc R . . C33 C 0.8009(4) 0.1616(4) 0.2353(4) 0.0373(16) Uani 1 1 d . . . H33 H 0.8460 0.1888 0.2060 0.045 Uiso 1 1 calc R . . C34 C 0.6499(5) 0.2089(4) 0.2542(5) 0.0387(17) Uani 1 1 d . . . C35 C 0.8738(4) 0.1125(4) 0.3332(5) 0.0381(17) Uani 1 1 d . . . H35A H 0.9102 0.1473 0.3077 0.046 Uiso 1 1 calc R . . H35B H 0.9145 0.0620 0.3380 0.046 Uiso 1 1 calc R . . C36 C 0.6990(5) 0.2824(4) 0.3283(4) 0.0365(16) Uani 1 1 d . . . H36A H 0.7505 0.3024 0.3034 0.044 Uiso 1 1 calc R . . H36B H 0.6452 0.3243 0.3304 0.044 Uiso 1 1 calc R . . C37 C 0.8075(5) 0.1084(4) 0.4803(5) 0.0390(17) Uani 1 1 d . . . C38 C 0.7686(4) 0.2289(4) 0.4272(4) 0.0309(15) Uani 1 1 d . . . H38 H 0.8133 0.2571 0.4014 0.037 Uiso 1 1 calc R . . C39 C 0.7278(4) 0.2388(4) 0.5210(4) 0.0375(16) Uani 1 1 d . . . H39 H 0.7534 0.2718 0.5390 0.045 Uiso 1 1 calc R . . C40 C 0.6126(4) 0.2912(4) 0.4758(4) 0.0341(15) Uani 1 1 d . . . C41 C 0.7470(4) 0.1409(5) 0.6247(5) 0.0466(19) Uani 1 1 d . . . H41A H 0.7921 0.0909 0.6230 0.056 Uiso 1 1 calc R . . H41B H 0.7607 0.1810 0.6455 0.056 Uiso 1 1 calc R . . C42 C 0.5682(4) 0.3052(4) 0.6210(4) 0.0356(16) Uani 1 1 d . . . H42A H 0.5956 0.3314 0.6439 0.043 Uiso 1 1 calc R . . H42B H 0.5159 0.3447 0.6170 0.043 Uiso 1 1 calc R . . C43 C 0.6440(5) 0.0685(4) 0.7088(5) 0.0414(18) Uani 1 1 d . . . C44 C 0.5861(4) 0.2032(4) 0.7219(5) 0.0360(16) Uani 1 1 d . . . H44 H 0.6055 0.2365 0.7466 0.043 Uiso 1 1 calc R . . C45 C 0.5167(4) 0.1699(4) 0.7854(4) 0.0348(15) Uani 1 1 d . . . H45 H 0.5046 0.1858 0.8404 0.042 Uiso 1 1 calc R . . C46 C 0.4493(5) 0.2491(4) 0.7066(5) 0.0391(17) Uani 1 1 d . . . C47 C 0.5331(5) 0.0291(4) 0.8268(5) 0.0424(18) Uani 1 1 d . . . H47A H 0.5186 0.0497 0.8801 0.051 Uiso 1 1 calc R . . H47B H 0.5836 -0.0191 0.8151 0.051 Uiso 1 1 calc R . . C48 C 0.6510(4) -0.1982(4) 0.1749(5) 0.0440(19) Uani 1 1 d . . . H48A H 0.6957 -0.2379 0.1895 0.053 Uiso 1 1 calc R . . H48B H 0.6602 -0.2125 0.1210 0.053 Uiso 1 1 calc R . . N1 N 1.3217(3) -0.5075(3) 0.1742(3) 0.0285(12) Uani 1 1 d . . . N2 N 1.2386(3) -0.4829(3) 0.1034(3) 0.0285(12) Uani 1 1 d . . . N3 N 1.3389(3) -0.6454(3) 0.1704(3) 0.0297(12) Uani 1 1 d . . . N4 N 1.2469(3) -0.6199(3) 0.1093(3) 0.0298(12) Uani 1 1 d . . . N5 N 1.0855(3) -0.4431(3) 0.1135(3) 0.0280(12) Uani 1 1 d . . . N6 N 0.9421(3) -0.4089(3) 0.1953(3) 0.0271(12) Uani 1 1 d . . . N7 N 1.0935(3) -0.5802(3) 0.1256(3) 0.0285(12) Uani 1 1 d . . . N8 N 0.9486(3) -0.5455(3) 0.2091(3) 0.0309(12) Uani 1 1 d . . . N9 N 0.8016(3) -0.3743(3) 0.3126(3) 0.0305(12) Uani 1 1 d . . . N10 N 0.7095(4) -0.3564(3) 0.4420(3) 0.0310(12) Uani 1 1 d . . . N11 N 0.8074(3) -0.5111(3) 0.3259(3) 0.0320(12) Uani 1 1 d . . . N12 N 0.6966(4) -0.4862(3) 0.4481(3) 0.0310(12) Uani 1 1 d . . . N13 N 0.6427(4) -0.3427(3) 0.5873(3) 0.0310(12) Uani 1 1 d . . . N14 N 0.6209(3) -0.3402(3) 0.7151(3) 0.0302(12) Uani 1 1 d . . . N15 N 0.6347(3) -0.4746(3) 0.5921(3) 0.0286(12) Uani 1 1 d . . . N16 N 0.6324(4) -0.4785(3) 0.7147(3) 0.0323(13) Uani 1 1 d . . . N17 N 0.6658(4) -0.1238(3) 0.1736(4) 0.0379(14) Uani 1 1 d . . . N18 N 0.7506(4) -0.0473(3) 0.1582(4) 0.0380(14) Uani 1 1 d . . . N19 N 0.5439(4) -0.0109(3) 0.1715(4) 0.0392(14) Uani 1 1 d . . . N20 N 0.6273(4) 0.0657(3) 0.1582(4) 0.0442(15) Uani 1 1 d . . . N21 N 0.8134(4) 0.0367(3) 0.1973(4) 0.0369(14) Uani 1 1 d . . . N22 N 0.8324(4) 0.1021(3) 0.2831(4) 0.0373(14) Uani 1 1 d . . . N23 N 0.6890(4) 0.1503(3) 0.1986(4) 0.0419(15) Uani 1 1 d . . . N24 N 0.7127(4) 0.2170(3) 0.2784(4) 0.0353(13) Uani 1 1 d . . . N25 N 0.8098(3) 0.1448(3) 0.4130(4) 0.0342(13) Uani 1 1 d . . . N26 N 0.7544(4) 0.1586(3) 0.5435(4) 0.0390(14) Uani 1 1 d . . . N27 N 0.6886(4) 0.2620(3) 0.4088(4) 0.0368(14) Uani 1 1 d . . . N28 N 0.6319(3) 0.2756(3) 0.5415(4) 0.0346(13) Uani 1 1 d . . . N29 N 0.6593(4) 0.1367(4) 0.6791(4) 0.0415(15) Uani 1 1 d . . . N30 N 0.5609(4) 0.0849(3) 0.7687(4) 0.0392(14) Uani 1 1 d . . . N31 N 0.5371(3) 0.2488(3) 0.6758(3) 0.0321(13) Uani 1 1 d . . . N32 N 0.4387(4) 0.1982(3) 0.7690(4) 0.0439(15) Uani 1 1 d . . . O1 O 1.2130(3) -0.3876(3) 0.1941(3) 0.0375(11) Uani 1 1 d . . . O2 O 1.0254(3) -0.3279(3) 0.1886(3) 0.0391(11) Uani 1 1 d . . . O3 O 0.8023(4) -0.2785(3) 0.3875(3) 0.0563(15) Uani 1 1 d . . . O4 O 0.6848(4) -0.2528(3) 0.6344(3) 0.0473(13) Uani 1 1 d . . . O5 O 1.2435(3) -0.7192(3) 0.1986(3) 0.0383(11) Uani 1 1 d . . . O6 O 1.0430(3) -0.6646(2) 0.2226(3) 0.0342(11) Uani 1 1 d . . . O7 O 0.7921(3) -0.6124(3) 0.4125(3) 0.0423(12) Uani 1 1 d . . . O8 O 0.6922(3) -0.5939(3) 0.6376(3) 0.0430(12) Uani 1 1 d . . . O9 O 0.7794(4) -0.1639(3) 0.2198(4) 0.0526(14) Uani 1 1 d . . . O10 O 0.8768(4) -0.0323(3) 0.2827(4) 0.0547(15) Uani 1 1 d . . . O11 O 0.8482(4) 0.0382(3) 0.4829(4) 0.0587(16) Uani 1 1 d . . . O12 O 0.6987(4) 0.0028(3) 0.6848(4) 0.0529(14) Uani 1 1 d . . . O13 O 0.4724(4) 0.1172(3) 0.2165(4) 0.0547(15) Uani 1 1 d . . . O14 O 0.5710(3) 0.2487(3) 0.2800(4) 0.0489(13) Uani 1 1 d . . . O15 O 0.5387(3) 0.3276(3) 0.4763(3) 0.0438(12) Uani 1 1 d . . . O16 O 0.3920(3) 0.2851(3) 0.6822(3) 0.0470(13) 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 Cl5 0.0927(18) 0.0670(16) 0.097(2) 0.0131(15) -0.0441(16) -0.0388(14) Cl6 0.0733(15) 0.0651(16) 0.0887(19) -0.0144(14) -0.0299(14) -0.0181(12) Cl7 0.150(3) 0.108(2) 0.106(2) 0.046(2) -0.090(2) -0.080(2) N33 0.039(3) 0.048(4) 0.049(4) 0.003(3) -0.017(3) -0.016(3) O1W 0.128(6) 0.066(5) 0.090(5) 0.037(4) -0.066(5) -0.058(4) O2W 0.060(4) 0.049(4) 0.089(5) 0.008(3) -0.024(3) -0.023(3) O3W 0.102(6) 0.045(4) 0.221(10) -0.032(5) -0.118(7) 0.012(4) O4W 0.063(4) 0.064(4) 0.056(4) -0.004(3) -0.025(3) 0.014(3) O5W 0.089(5) 0.054(4) 0.078(5) -0.014(4) -0.009(4) -0.028(4) O6W 0.071(4) 0.078(5) 0.099(6) -0.021(4) -0.018(4) -0.010(4) O7W 0.122(6) 0.096(6) 0.063(5) 0.022(4) -0.027(4) -0.065(5) O8W 0.044(3) 0.035(3) 0.053(3) -0.005(2) -0.021(2) -0.011(2) O9W 0.074(4) 0.026(3) 0.082(4) 0.006(3) -0.034(3) -0.019(3) O10W 0.050(3) 0.068(4) 0.055(4) -0.025(3) -0.004(3) -0.021(3) O11W 0.099(5) 0.047(4) 0.045(4) -0.001(3) -0.029(3) -0.032(3) O12W 0.055(3) 0.056(4) 0.145(7) 0.049(4) -0.064(4) -0.031(3) O17 0.060(4) 0.077(5) 0.077(5) 0.022(4) -0.038(3) -0.025(3) O18 0.045(3) 0.117(6) 0.044(4) -0.011(4) -0.017(3) -0.019(3) O19 0.046(3) 0.089(5) 0.050(4) 0.001(3) -0.009(3) -0.030(3) Nd1 0.0456(2) 0.0296(2) 0.0675(3) 0.0049(2) -0.0317(2) -0.01036(18) Nd2 0.02931(19) 0.0229(2) 0.0414(3) 0.00270(16) -0.01499(16) -0.00689(14) Cl1 0.0554(11) 0.0435(11) 0.0471(12) 0.0067(9) -0.0060(9) -0.0162(9) Cl2 0.0543(12) 0.130(2) 0.0372(12) 0.0190(12) -0.0209(10) -0.0554(14) Cl3 0.0568(13) 0.0789(17) 0.0795(18) -0.0307(14) -0.0073(12) -0.0233(12) Cl4 0.0746(16) 0.0531(15) 0.114(2) 0.0037(15) -0.0463(16) -0.0110(12) Cd1 0.0372(3) 0.0531(5) 0.0437(4) 0.0010(3) -0.0097(3) -0.0194(3) Cd1' 0.028(9) 0.069(17) 0.042(11) -0.010(9) 0.006(7) -0.027(10) C1 0.029(3) 0.032(4) 0.034(4) 0.008(3) -0.012(3) -0.015(3) C2 0.027(3) 0.037(4) 0.027(4) 0.010(3) -0.007(3) -0.014(3) C3 0.033(3) 0.035(4) 0.021(4) 0.009(3) -0.007(3) -0.013(3) C4 0.023(3) 0.026(4) 0.030(4) -0.006(3) -0.008(3) 0.004(3) C5 0.039(3) 0.035(4) 0.025(4) 0.018(3) -0.018(3) -0.011(3) C6 0.028(3) 0.035(4) 0.033(4) -0.009(3) -0.014(3) -0.001(3) C7 0.035(3) 0.026(4) 0.032(4) 0.005(3) -0.020(3) -0.009(3) C8 0.027(3) 0.036(4) 0.025(4) 0.002(3) -0.015(3) -0.009(3) C9 0.033(3) 0.023(3) 0.044(4) -0.001(3) -0.022(3) -0.006(3) C10 0.024(3) 0.023(4) 0.042(4) -0.011(3) -0.019(3) 0.004(3) C11 0.036(3) 0.015(3) 0.036(4) 0.001(3) -0.014(3) -0.001(3) C12 0.022(3) 0.026(4) 0.043(4) -0.006(3) -0.007(3) -0.001(3) C13 0.042(4) 0.037(4) 0.042(5) 0.007(4) -0.021(3) -0.008(3) C14 0.035(3) 0.022(3) 0.033(4) 0.005(3) -0.018(3) -0.005(3) C15 0.033(3) 0.024(3) 0.025(4) 0.004(3) -0.012(3) -0.008(3) C16 0.038(3) 0.025(4) 0.045(4) 0.010(3) -0.023(3) -0.016(3) C17 0.048(4) 0.022(4) 0.032(4) 0.002(3) -0.016(3) -0.001(3) C18 0.040(3) 0.031(4) 0.033(4) 0.004(3) -0.014(3) -0.023(3) C19 0.028(3) 0.021(3) 0.034(4) 0.000(3) -0.012(3) 0.001(3) C20 0.029(3) 0.026(3) 0.032(4) -0.003(3) -0.014(3) -0.005(3) C21 0.028(3) 0.031(4) 0.030(4) 0.004(3) -0.017(3) -0.007(3) C22 0.027(3) 0.034(4) 0.042(4) 0.013(3) -0.020(3) -0.012(3) C23 0.029(3) 0.010(3) 0.040(4) 0.000(3) -0.017(3) 0.003(2) C24 0.029(3) 0.029(4) 0.044(4) 0.015(3) -0.022(3) -0.014(3) C25 0.044(4) 0.030(4) 0.038(4) -0.011(3) -0.015(3) -0.003(3) C26 0.039(4) 0.026(4) 0.038(4) 0.000(3) -0.015(3) -0.003(3) C27 0.039(3) 0.023(3) 0.031(4) 0.001(3) -0.013(3) -0.007(3) C28 0.054(4) 0.025(4) 0.036(4) 0.001(3) -0.020(4) 0.000(3) C29 0.031(3) 0.040(4) 0.047(5) -0.010(4) -0.014(3) 0.001(3) C30 0.060(5) 0.028(4) 0.067(6) 0.008(4) -0.044(4) -0.006(3) C31 0.027(3) 0.029(4) 0.048(5) -0.007(3) -0.011(3) 0.002(3) C32 0.038(3) 0.022(3) 0.033(4) -0.003(3) -0.012(3) 0.000(3) C33 0.035(4) 0.033(4) 0.040(4) 0.002(3) -0.012(3) -0.009(3) C34 0.040(4) 0.023(4) 0.046(5) 0.006(3) -0.020(3) 0.001(3) C35 0.035(3) 0.017(3) 0.056(5) -0.004(3) -0.019(3) 0.003(3) C36 0.042(4) 0.030(4) 0.038(4) 0.007(3) -0.019(3) -0.010(3) C37 0.040(4) 0.021(4) 0.054(5) -0.001(3) -0.015(4) -0.013(3) C38 0.018(3) 0.022(3) 0.045(4) -0.006(3) -0.011(3) 0.003(2) C39 0.026(3) 0.038(4) 0.046(4) 0.003(3) -0.018(3) -0.003(3) C40 0.035(4) 0.030(4) 0.041(4) 0.007(3) -0.018(3) -0.012(3) C41 0.031(4) 0.051(5) 0.048(5) -0.005(4) -0.020(3) 0.008(3) C42 0.033(3) 0.018(3) 0.047(4) -0.001(3) -0.014(3) 0.002(3) C43 0.040(4) 0.025(4) 0.047(5) 0.009(3) -0.015(3) 0.001(3) C44 0.037(3) 0.015(3) 0.049(5) 0.000(3) -0.021(3) 0.008(3) C45 0.041(4) 0.020(3) 0.039(4) 0.007(3) -0.019(3) -0.002(3) C46 0.033(4) 0.036(4) 0.041(4) 0.004(3) -0.010(3) -0.007(3) C47 0.034(4) 0.036(4) 0.045(5) 0.016(4) -0.015(3) 0.000(3) C48 0.035(4) 0.011(3) 0.069(6) 0.003(3) -0.015(4) 0.005(3) N1 0.026(3) 0.032(3) 0.031(3) 0.006(2) -0.013(2) -0.013(2) N2 0.028(3) 0.029(3) 0.031(3) 0.005(2) -0.012(2) -0.012(2) N3 0.027(3) 0.034(3) 0.028(3) 0.008(2) -0.013(2) -0.008(2) N4 0.032(3) 0.027(3) 0.031(3) 0.004(2) -0.015(2) -0.008(2) N5 0.025(2) 0.023(3) 0.037(3) 0.003(2) -0.015(2) -0.004(2) N6 0.026(3) 0.015(3) 0.036(3) -0.003(2) -0.014(2) 0.002(2) N7 0.024(3) 0.022(3) 0.032(3) 0.000(2) -0.010(2) 0.002(2) N8 0.034(3) 0.023(3) 0.035(3) 0.005(2) -0.012(2) -0.011(2) N9 0.028(3) 0.029(3) 0.030(3) 0.006(2) -0.009(2) -0.008(2) N10 0.044(3) 0.013(3) 0.031(3) 0.002(2) -0.011(3) -0.008(2) N11 0.032(3) 0.018(3) 0.037(3) 0.003(2) -0.011(2) 0.000(2) N12 0.044(3) 0.020(3) 0.026(3) -0.001(2) -0.014(2) -0.004(2) N13 0.042(3) 0.026(3) 0.026(3) 0.010(2) -0.014(2) -0.015(2) N14 0.031(3) 0.034(3) 0.026(3) 0.003(2) -0.013(2) -0.011(2) N15 0.039(3) 0.020(3) 0.030(3) 0.000(2) -0.016(2) -0.010(2) N16 0.043(3) 0.022(3) 0.037(3) 0.009(3) -0.023(3) -0.010(2) N17 0.043(3) 0.018(3) 0.045(4) 0.005(3) -0.013(3) -0.006(2) N18 0.039(3) 0.026(3) 0.051(4) 0.004(3) -0.026(3) -0.003(2) N19 0.038(3) 0.031(3) 0.044(4) 0.005(3) -0.014(3) -0.010(3) N20 0.047(3) 0.024(3) 0.063(4) 0.002(3) -0.028(3) -0.004(3) N21 0.036(3) 0.020(3) 0.047(4) -0.006(3) -0.016(3) 0.003(2) N22 0.037(3) 0.023(3) 0.050(4) -0.002(3) -0.020(3) -0.001(2) N23 0.044(3) 0.027(3) 0.057(4) -0.007(3) -0.031(3) 0.000(3) N24 0.033(3) 0.025(3) 0.040(4) -0.001(3) -0.016(3) 0.002(2) N25 0.028(3) 0.018(3) 0.049(4) 0.000(3) -0.016(3) 0.004(2) N26 0.036(3) 0.032(3) 0.040(4) 0.003(3) -0.013(3) -0.001(2) N27 0.029(3) 0.039(3) 0.038(4) 0.003(3) -0.016(3) -0.003(2) N28 0.024(3) 0.026(3) 0.044(4) -0.001(3) -0.013(3) 0.005(2) N29 0.033(3) 0.036(4) 0.044(4) 0.012(3) -0.013(3) -0.003(3) N30 0.035(3) 0.023(3) 0.050(4) 0.007(3) -0.013(3) -0.004(2) N31 0.033(3) 0.022(3) 0.040(3) 0.013(2) -0.016(3) -0.009(2) N32 0.033(3) 0.034(3) 0.058(4) 0.014(3) -0.018(3) -0.006(3) O1 0.042(3) 0.023(3) 0.048(3) 0.002(2) -0.022(2) -0.005(2) O2 0.036(2) 0.039(3) 0.043(3) -0.003(2) -0.016(2) -0.011(2) O3 0.081(4) 0.041(3) 0.048(3) 0.002(3) -0.009(3) -0.044(3) O4 0.060(3) 0.053(3) 0.038(3) 0.008(3) -0.017(3) -0.034(3) O5 0.041(3) 0.035(3) 0.048(3) 0.015(2) -0.025(2) -0.019(2) O6 0.030(2) 0.011(2) 0.051(3) -0.004(2) -0.016(2) 0.0081(17) O7 0.055(3) 0.025(3) 0.050(3) 0.006(2) -0.027(3) -0.011(2) O8 0.051(3) 0.030(3) 0.052(3) 0.005(2) -0.025(3) -0.014(2) O9 0.067(3) 0.029(3) 0.061(4) 0.012(3) -0.037(3) -0.001(3) O10 0.068(4) 0.037(3) 0.064(4) 0.000(3) -0.040(3) -0.004(3) O11 0.057(3) 0.022(3) 0.068(4) 0.012(3) -0.012(3) 0.005(2) O12 0.051(3) 0.033(3) 0.059(4) 0.004(3) -0.019(3) 0.001(2) O13 0.056(3) 0.024(3) 0.071(4) -0.002(3) -0.024(3) 0.005(2) O14 0.040(3) 0.036(3) 0.066(4) -0.003(3) -0.026(3) 0.003(2) O15 0.029(2) 0.043(3) 0.052(3) 0.001(2) -0.019(2) 0.003(2) O16 0.040(3) 0.033(3) 0.070(4) 0.012(3) -0.029(3) -0.006(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 N33 O18 1.262(8) . ? N33 O19 1.278(8) . ? N33 O17 1.291(8) . ? O1W Nd1 2.469(7) . ? O2W Nd1 2.553(6) . ? O3W Nd1 2.482(6) . ? O4W Nd1 2.511(6) . ? O5W Nd1 2.491(6) . ? O6W Nd1 2.570(8) . ? O7W Nd1 2.495(7) . ? O8W Nd2 2.504(5) . ? O9W Nd2 2.503(5) . ? O10W Nd2 2.438(6) . ? O11W Nd2 2.524(5) . ? O12W Nd2 2.459(5) . ? O17 Nd2 2.668(6) . ? O18 Nd2 2.529(6) . ? Nd1 O1 2.473(5) . ? Nd1 O2 2.513(5) . ? Nd2 O6 2.428(4) . ? Nd2 O5 2.471(4) . ? Cl1 Cd1 2.422(2) . ? Cl1 Cd1' 2.723(18) . ? Cl2 Cd1 2.4239(19) . ? Cl2 Cd1' 2.626(16) . ? Cl3 Cd1' 1.729(17) . ? Cl3 Cd1 2.488(2) . ? Cl4 Cd1 2.467(3) . ? C1 O1 1.228(8) . ? C1 N1 1.365(8) . ? C1 N2 1.373(8) . ? C2 N3 1.437(8) . ? C2 N1 1.453(9) . ? C2 C3 1.554(9) . ? C2 H2 0.9900 . ? C3 N2 1.445(9) . ? C3 N4 1.464(8) . ? C3 H3 0.9900 . ? C4 O5 1.235(8) . ? C4 N3 1.358(8) . ? C4 N4 1.359(8) . ? C5 N5 1.451(8) . ? C5 N2 1.464(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.450(8) . ? C6 N4 1.459(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.245(8) . ? C7 N5 1.349(8) . ? C7 N6 1.353(8) . ? C8 N5 1.458(8) . ? C8 N7 1.461(8) . ? C8 C9 1.555(9) . ? C8 H8 0.9900 . ? C9 N6 1.448(8) . ? C9 N8 1.464(8) . ? C9 H9 0.9900 . ? C10 O6 1.219(8) . ? C10 N8 1.370(8) . ? C10 N7 1.378(9) . ? C11 N9 1.430(8) . ? C11 N6 1.444(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.437(8) . ? C12 N8 1.455(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.248(9) . ? C13 N10 1.355(9) . ? C13 N9 1.367(9) . ? C14 N9 1.428(8) . ? C14 N11 1.470(8) . ? C14 C15 1.526(9) . ? C14 H14 0.9900 . ? C15 N12 1.439(8) . ? C15 N10 1.461(8) . ? C15 H15 0.9900 . ? C16 O7 1.238(8) . ? C16 N12 1.362(9) . ? C16 N11 1.373(9) . ? C17 N10 1.441(8) . ? C17 N13 1.456(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.426(8) . ? C18 N12 1.456(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.216(8) . ? C19 N14 1.357(9) . ? C19 N13 1.387(8) . ? C20 N15 1.444(8) . ? C20 N13 1.457(8) . ? C20 C21 1.542(9) . ? C20 H20 0.9900 . ? C21 N14 1.457(8) . ? C21 N16 1.459(8) . ? C21 H21 0.9900 . ? C22 O8 1.233(8) . ? C22 N15 1.369(8) . ? C22 N16 1.369(9) . ? C23 N14 1.444(8) . ? C23 N3 1.474(8) 2_746 ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N1 1.443(8) 2_746 ? C24 N16 1.449(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O9 1.204(9) . ? C25 N17 1.387(9) . ? C25 N18 1.391(9) . ? C26 N17 1.435(9) . ? C26 N19 1.468(9) . ? C26 C27 1.588(9) . ? C26 H26 0.9900 . ? C27 N18 1.435(8) . ? C27 N20 1.462(9) . ? C27 H27 0.9900 . ? C28 O13 1.236(9) . ? C28 N20 1.354(10) . ? C28 N19 1.362(9) . ? C29 N21 1.442(9) . ? C29 N18 1.453(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.445(9) . ? C30 N23 1.451(9) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O10 1.232(9) . ? C31 N21 1.354(9) . ? C31 N22 1.385(9) . ? C32 N21 1.432(9) . ? C32 N23 1.478(8) . ? C32 C33 1.541(10) . ? C32 H32 0.9900 . ? C33 N22 1.440(9) . ? C33 N24 1.454(9) . ? C33 H33 0.9900 . ? C34 O14 1.220(8) . ? C34 N23 1.339(9) . ? C34 N24 1.371(9) . ? C35 N22 1.426(9) . ? C35 N25 1.453(9) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N27 1.439(9) . ? C36 N24 1.460(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O11 1.248(8) . ? C37 N25 1.336(9) . ? C37 N26 1.339(9) . ? C38 N25 1.456(8) . ? C38 N27 1.476(8) . ? C38 C39 1.568(10) . ? C38 H38 0.9900 . ? C39 N26 1.455(9) . ? C39 N28 1.460(8) . ? C39 H39 0.9900 . ? C40 O15 1.226(8) . ? C40 N28 1.358(9) . ? C40 N27 1.359(9) . ? C41 N29 1.444(9) . ? C41 N26 1.455(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N31 1.432(8) . ? C42 N28 1.436(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O12 1.237(8) . ? C43 N30 1.352(9) . ? C43 N29 1.363(9) . ? C44 N29 1.429(9) . ? C44 N31 1.456(8) . ? C44 C45 1.524(10) . ? C44 H44 0.9900 . ? C45 N32 1.419(9) . ? C45 N30 1.479(8) . ? C45 H45 0.9900 . ? C46 O16 1.222(8) . ? C46 N31 1.373(8) . ? C46 N32 1.390(9) . ? C47 N30 1.441(9) . ? C47 N19 1.446(9) 2_656 ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N17 1.442(9) . ? C48 N32 1.457(9) 2_656 ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? N1 C24 1.443(8) 2_746 ? N3 C23 1.474(8) 2_746 ? N19 C47 1.446(9) 2_656 ? N32 C48 1.457(9) 2_656 ? 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 O18 N33 O19 125.9(6) . . ? O18 N33 O17 115.2(6) . . ? O19 N33 O17 118.5(7) . . ? N33 O17 Nd2 94.1(4) . . ? N33 O18 Nd2 101.6(4) . . ? O1W Nd1 O1 87.1(2) . . ? O1W Nd1 O3W 79.0(3) . . ? O1 Nd1 O3W 142.90(19) . . ? O1W Nd1 O5W 76.8(2) . . ? O1 Nd1 O5W 134.0(2) . . ? O3W Nd1 O5W 75.9(2) . . ? O1W Nd1 O7W 138.9(2) . . ? O1 Nd1 O7W 82.2(2) . . ? O3W Nd1 O7W 86.1(3) . . ? O5W Nd1 O7W 136.0(2) . . ? O1W Nd1 O4W 143.0(2) . . ? O1 Nd1 O4W 76.69(18) . . ? O3W Nd1 O4W 132.1(3) . . ? O5W Nd1 O4W 90.9(2) . . ? O7W Nd1 O4W 72.0(3) . . ? O1W Nd1 O2 69.82(19) . . ? O1 Nd1 O2 76.66(15) . . ? O3W Nd1 O2 66.27(19) . . ? O5W Nd1 O2 133.1(2) . . ? O7W Nd1 O2 69.2(2) . . ? O4W Nd1 O2 135.1(2) . . ? O1W Nd1 O2W 72.1(2) . . ? O1 Nd1 O2W 66.11(17) . . ? O3W Nd1 O2W 137.7(3) . . ? O5W Nd1 O2W 68.0(2) . . ? O7W Nd1 O2W 135.5(3) . . ? O4W Nd1 O2W 70.9(2) . . ? O2 Nd1 O2W 127.18(19) . . ? O1W Nd1 O6W 134.3(3) . . ? O1 Nd1 O6W 137.9(2) . . ? O3W Nd1 O6W 67.6(3) . . ? O5W Nd1 O6W 65.8(2) . . ? O7W Nd1 O6W 70.2(3) . . ? O4W Nd1 O6W 65.1(2) . . ? O2 Nd1 O6W 119.1(2) . . ? O2W Nd1 O6W 113.6(2) . . ? O6 Nd2 O10W 97.3(2) . . ? O6 Nd2 O12W 144.52(17) . . ? O10W Nd2 O12W 84.6(2) . . ? O6 Nd2 O5 78.84(15) . . ? O10W Nd2 O5 70.90(18) . . ? O12W Nd2 O5 68.29(17) . . ? O6 Nd2 O9W 139.16(17) . . ? O10W Nd2 O9W 75.5(2) . . ? O12W Nd2 O9W 75.8(2) . . ? O5 Nd2 O9W 132.25(18) . . ? O6 Nd2 O8W 67.42(15) . . ? O10W Nd2 O8W 72.52(18) . . ? O12W Nd2 O8W 144.2(2) . . ? O5 Nd2 O8W 125.55(16) . . ? O9W Nd2 O8W 72.15(18) . . ? O6 Nd2 O11W 74.37(18) . . ? O10W Nd2 O11W 144.46(19) . . ? O12W Nd2 O11W 83.6(2) . . ? O5 Nd2 O11W 73.59(19) . . ? O9W Nd2 O11W 132.8(2) . . ? O8W Nd2 O11W 130.43(19) . . ? O6 Nd2 O18 81.8(2) . . ? O10W Nd2 O18 142.02(19) . . ? O12W Nd2 O18 117.7(2) . . ? O5 Nd2 O18 144.0(2) . . ? O9W Nd2 O18 80.7(2) . . ? O8W Nd2 O18 72.22(18) . . ? O11W Nd2 O18 72.1(2) . . ? O6 Nd2 O17 123.56(18) . . ? O10W Nd2 O17 137.7(2) . . ? O12W Nd2 O17 68.8(2) . . ? O5 Nd2 O17 123.31(17) . . ? O9W Nd2 O17 66.6(2) . . ? O8W Nd2 O17 110.95(18) . . ? O11W Nd2 O17 66.4(2) . . ? O18 Nd2 O17 48.9(2) . . ? Cd1 Cl1 Cd1' 25.0(5) . . ? Cd1 Cl2 Cd1' 26.0(4) . . ? Cd1' Cl3 Cd1 24.1(7) . . ? Cl1 Cd1 Cl2 113.74(7) . . ? Cl1 Cd1 Cl4 116.85(9) . . ? Cl2 Cd1 Cl4 102.95(10) . . ? Cl1 Cd1 Cl3 110.20(9) . . ? Cl2 Cd1 Cl3 108.20(9) . . ? Cl4 Cd1 Cl3 104.09(10) . . ? Cl3 Cd1' Cl2 130.9(9) . . ? Cl3 Cd1' Cl1 128.1(7) . . ? Cl2 Cd1' Cl1 98.7(6) . . ? O1 C1 N1 126.1(6) . . ? O1 C1 N2 125.7(6) . . ? N1 C1 N2 108.3(6) . . ? N3 C2 N1 113.8(5) . . ? N3 C2 C3 103.6(5) . . ? N1 C2 C3 102.8(5) . . ? N3 C2 H2 112.0 . . ? N1 C2 H2 112.0 . . ? C3 C2 H2 112.0 . . ? N2 C3 N4 113.5(5) . . ? N2 C3 C2 103.6(5) . . ? N4 C3 C2 102.2(5) . . ? N2 C3 H3 112.3 . . ? N4 C3 H3 112.3 . . ? C2 C3 H3 112.3 . . ? O5 C4 N3 124.9(6) . . ? O5 C4 N4 126.7(6) . . ? N3 C4 N4 108.4(6) . . ? N5 C5 N2 112.5(5) . . ? N5 C5 H5A 109.1 . . ? N2 C5 H5A 109.1 . . ? N5 C5 H5B 109.1 . . ? N2 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N7 C6 N4 110.5(5) . . ? N7 C6 H6A 109.5 . . ? N4 C6 H6A 109.5 . . ? N7 C6 H6B 109.5 . . ? N4 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? O2 C7 N5 124.9(6) . . ? O2 C7 N6 125.9(6) . . ? N5 C7 N6 109.1(5) . . ? N5 C8 N7 113.2(5) . . ? N5 C8 C9 102.4(5) . . ? N7 C8 C9 103.5(5) . . ? N5 C8 H8 112.3 . . ? N7 C8 H8 112.3 . . ? C9 C8 H8 112.3 . . ? N6 C9 N8 113.5(6) . . ? N6 C9 C8 103.3(5) . . ? N8 C9 C8 103.1(5) . . ? N6 C9 H9 112.1 . . ? N8 C9 H9 112.1 . . ? C8 C9 H9 112.1 . . ? O6 C10 N8 126.4(6) . . ? O6 C10 N7 125.2(5) . . ? N8 C10 N7 108.3(6) . . ? N9 C11 N6 114.4(5) . . ? N9 C11 H11A 108.6 . . ? N6 C11 H11A 108.6 . . ? N9 C11 H11B 108.6 . . ? N6 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N11 C12 N8 113.6(5) . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12B 108.8 . . ? N8 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 126.1(7) . . ? O3 C13 N9 124.1(7) . . ? N10 C13 N9 109.7(6) . . ? N9 C14 N11 114.7(5) . . ? N9 C14 C15 105.5(5) . . ? N11 C14 C15 103.8(5) . . ? N9 C14 H14 110.8 . . ? N11 C14 H14 110.8 . . ? C15 C14 H14 110.8 . . ? N12 C15 N10 112.9(5) . . ? N12 C15 C14 104.0(5) . . ? N10 C15 C14 102.1(5) . . ? N12 C15 H15 112.4 . . ? N10 C15 H15 112.4 . . ? C14 C15 H15 112.4 . . ? O7 C16 N12 125.4(6) . . ? O7 C16 N11 125.5(7) . . ? N12 C16 N11 109.1(5) . . ? N10 C17 N13 113.8(5) . . ? N10 C17 H17A 108.8 . . ? N13 C17 H17A 108.8 . . ? N10 C17 H17B 108.8 . . ? N13 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N15 C18 N12 113.1(5) . . ? N15 C18 H18A 109.0 . . ? N12 C18 H18A 109.0 . . ? N15 C18 H18B 109.0 . . ? N12 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N14 125.5(6) . . ? O4 C19 N13 126.7(6) . . ? N14 C19 N13 107.8(5) . . ? N15 C20 N13 113.6(5) . . ? N15 C20 C21 103.7(5) . . ? N13 C20 C21 103.1(5) . . ? N15 C20 H20 111.9 . . ? N13 C20 H20 111.9 . . ? C21 C20 H20 111.9 . . ? N14 C21 N16 114.2(5) . . ? N14 C21 C20 103.4(5) . . ? N16 C21 C20 103.2(5) . . ? N14 C21 H21 111.8 . . ? N16 C21 H21 111.8 . . ? C20 C21 H21 111.8 . . ? O8 C22 N15 125.1(7) . . ? O8 C22 N16 126.2(6) . . ? N15 C22 N16 108.7(6) . . ? N14 C23 N3 112.9(5) . 2_746 ? N14 C23 H23A 109.0 . . ? N3 C23 H23A 109.0 2_746 . ? N14 C23 H23B 109.0 . . ? N3 C23 H23B 109.0 2_746 . ? H23A C23 H23B 107.8 . . ? N1 C24 N16 114.6(5) 2_746 . ? N1 C24 H24A 108.6 2_746 . ? N16 C24 H24A 108.6 . . ? N1 C24 H24B 108.6 2_746 . ? N16 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? O9 C25 N17 127.2(7) . . ? O9 C25 N18 125.8(7) . . ? N17 C25 N18 107.0(6) . . ? N17 C26 N19 113.4(6) . . ? N17 C26 C27 103.0(5) . . ? N19 C26 C27 102.1(5) . . ? N17 C26 H26 112.5 . . ? N19 C26 H26 112.5 . . ? C27 C26 H26 112.5 . . ? N18 C27 N20 114.1(6) . . ? N18 C27 C26 102.9(5) . . ? N20 C27 C26 102.8(5) . . ? N18 C27 H27 112.1 . . ? N20 C27 H27 112.1 . . ? C26 C27 H27 112.1 . . ? O13 C28 N20 126.2(7) . . ? O13 C28 N19 124.1(7) . . ? N20 C28 N19 109.7(6) . . ? N21 C29 N18 113.3(6) . . ? N21 C29 H29A 108.9 . . ? N18 C29 H29A 108.9 . . ? N21 C29 H29B 108.9 . . ? N18 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N20 C30 N23 113.8(6) . . ? N20 C30 H30A 108.8 . . ? N23 C30 H30A 108.8 . . ? N20 C30 H30B 108.8 . . ? N23 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? O10 C31 N21 127.4(7) . . ? O10 C31 N22 123.6(7) . . ? N21 C31 N22 109.0(6) . . ? N21 C32 N23 114.2(6) . . ? N21 C32 C33 104.1(6) . . ? N23 C32 C33 102.0(5) . . ? N21 C32 H32 111.9 . . ? N23 C32 H32 111.9 . . ? C33 C32 H32 111.9 . . ? N22 C33 N24 115.0(6) . . ? N22 C33 C32 103.7(6) . . ? N24 C33 C32 104.2(5) . . ? N22 C33 H33 111.1 . . ? N24 C33 H33 111.1 . . ? C32 C33 H33 111.1 . . ? O14 C34 N23 125.9(7) . . ? O14 C34 N24 125.0(7) . . ? N23 C34 N24 109.0(6) . . ? N22 C35 N25 113.4(5) . . ? N22 C35 H35A 108.9 . . ? N25 C35 H35A 108.9 . . ? N22 C35 H35B 108.9 . . ? N25 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? N27 C36 N24 113.2(6) . . ? N27 C36 H36A 108.9 . . ? N24 C36 H36A 108.9 . . ? N27 C36 H36B 108.9 . . ? N24 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? O11 C37 N25 124.7(7) . . ? O11 C37 N26 125.9(7) . . ? N25 C37 N26 109.4(6) . . ? N25 C38 N27 115.3(5) . . ? N25 C38 C39 102.6(5) . . ? N27 C38 C39 102.6(5) . . ? N25 C38 H38 111.8 . . ? N27 C38 H38 111.8 . . ? C39 C38 H38 111.8 . . ? N26 C39 N28 116.3(6) . . ? N26 C39 C38 101.7(5) . . ? N28 C39 C38 103.0(5) . . ? N26 C39 H39 111.7 . . ? N28 C39 H39 111.7 . . ? C38 C39 H39 111.7 . . ? O15 C40 N28 125.5(6) . . ? O15 C40 N27 125.0(6) . . ? N28 C40 N27 109.6(5) . . ? N29 C41 N26 113.7(6) . . ? N29 C41 H41A 108.8 . . ? N26 C41 H41A 108.8 . . ? N29 C41 H41B 108.8 . . ? N26 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? N31 C42 N28 116.1(5) . . ? N31 C42 H42A 108.3 . . ? N28 C42 H42A 108.3 . . ? N31 C42 H42B 108.3 . . ? N28 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? O12 C43 N30 126.5(7) . . ? O12 C43 N29 124.8(7) . . ? N30 C43 N29 108.7(6) . . ? N29 C44 N31 114.8(6) . . ? N29 C44 C45 105.1(5) . . ? N31 C44 C45 102.8(5) . . ? N29 C44 H44 111.2 . . ? N31 C44 H44 111.2 . . ? C45 C44 H44 111.2 . . ? N32 C45 N30 113.4(6) . . ? N32 C45 C44 105.3(5) . . ? N30 C45 C44 102.1(5) . . ? N32 C45 H45 111.8 . . ? N30 C45 H45 111.8 . . ? C44 C45 H45 111.8 . . ? O16 C46 N31 126.5(7) . . ? O16 C46 N32 126.5(6) . . ? N31 C46 N32 107.0(6) . . ? N30 C47 N19 114.1(6) . 2_656 ? N30 C47 H47A 108.7 . . ? N19 C47 H47A 108.7 2_656 . ? N30 C47 H47B 108.7 . . ? N19 C47 H47B 108.7 2_656 . ? H47A C47 H47B 107.6 . . ? N17 C48 N32 113.1(6) . 2_656 ? N17 C48 H48A 109.0 . . ? N32 C48 H48A 109.0 2_656 . ? N17 C48 H48B 109.0 . . ? N32 C48 H48B 109.0 2_656 . ? H48A C48 H48B 107.8 . . ? C1 N1 C24 122.1(5) . 2_746 ? C1 N1 C2 112.8(5) . . ? C24 N1 C2 121.6(5) 2_746 . ? C1 N2 C3 112.3(5) . . ? C1 N2 C5 122.3(6) . . ? C3 N2 C5 125.3(5) . . ? C4 N3 C2 113.0(5) . . ? C4 N3 C23 123.2(5) . 2_746 ? C2 N3 C23 123.1(5) . 2_746 ? C4 N4 C6 121.5(5) . . ? C4 N4 C3 112.6(5) . . ? C6 N4 C3 125.7(5) . . ? C7 N5 C5 122.9(5) . . ? C7 N5 C8 112.7(5) . . ? C5 N5 C8 124.1(5) . . ? C7 N6 C11 122.9(5) . . ? C7 N6 C9 112.4(5) . . ? C11 N6 C9 120.9(5) . . ? C10 N7 C6 122.1(5) . . ? C10 N7 C8 112.4(5) . . ? C6 N7 C8 124.4(5) . . ? C10 N8 C12 122.4(5) . . ? C10 N8 C9 112.7(5) . . ? C12 N8 C9 120.9(5) . . ? C13 N9 C14 110.4(5) . . ? C13 N9 C11 124.9(6) . . ? C14 N9 C11 123.1(6) . . ? C13 N10 C17 120.5(6) . . ? C13 N10 C15 111.3(5) . . ? C17 N10 C15 121.4(5) . . ? C16 N11 C12 120.2(5) . . ? C16 N11 C14 110.4(5) . . ? C12 N11 C14 123.1(5) . . ? C16 N12 C15 112.3(5) . . ? C16 N12 C18 122.4(5) . . ? C15 N12 C18 124.1(5) . . ? C19 N13 C17 120.4(5) . . ? C19 N13 C20 111.8(5) . . ? C17 N13 C20 121.9(5) . . ? C19 N14 C23 122.6(5) . . ? C19 N14 C21 112.9(5) . . ? C23 N14 C21 121.8(5) . . ? C22 N15 C18 122.7(6) . . ? C22 N15 C20 112.2(5) . . ? C18 N15 C20 122.6(5) . . ? C22 N16 C24 122.3(5) . . ? C22 N16 C21 111.6(5) . . ? C24 N16 C21 121.8(6) . . ? C25 N17 C26 113.3(6) . . ? C25 N17 C48 120.8(6) . . ? C26 N17 C48 120.9(6) . . ? C25 N18 C27 113.4(5) . . ? C25 N18 C29 122.1(6) . . ? C27 N18 C29 121.7(6) . . ? C28 N19 C47 123.4(6) . 2_656 ? C28 N19 C26 112.6(6) . . ? C47 N19 C26 120.5(6) 2_656 . ? C28 N20 C30 122.9(6) . . ? C28 N20 C27 112.6(6) . . ? C30 N20 C27 121.6(6) . . ? C31 N21 C32 112.0(6) . . ? C31 N21 C29 122.0(6) . . ? C32 N21 C29 123.7(6) . . ? C31 N22 C35 121.8(6) . . ? C31 N22 C33 110.9(6) . . ? C35 N22 C33 124.4(6) . . ? C34 N23 C30 122.9(6) . . ? C34 N23 C32 112.9(5) . . ? C30 N23 C32 121.4(6) . . ? C34 N24 C33 111.7(6) . . ? C34 N24 C36 124.6(5) . . ? C33 N24 C36 122.5(5) . . ? C37 N25 C35 123.8(5) . . ? C37 N25 C38 112.3(6) . . ? C35 N25 C38 119.9(6) . . ? C37 N26 C39 113.0(6) . . ? C37 N26 C41 123.4(6) . . ? C39 N26 C41 120.9(6) . . ? C40 N27 C36 124.9(5) . . ? C40 N27 C38 112.0(5) . . ? C36 N27 C38 120.1(5) . . ? C40 N28 C42 123.4(5) . . ? C40 N28 C39 112.6(6) . . ? C42 N28 C39 123.0(6) . . ? C43 N29 C44 112.1(6) . . ? C43 N29 C41 122.8(6) . . ? C44 N29 C41 123.5(6) . . ? C43 N30 C47 122.5(6) . . ? C43 N30 C45 111.9(6) . . ? C47 N30 C45 122.0(6) . . ? C46 N31 C42 122.4(5) . . ? C46 N31 C44 112.5(6) . . ? C42 N31 C44 122.6(5) . . ? C46 N32 C45 112.1(6) . . ? C46 N32 C48 120.2(5) . 2_656 ? C45 N32 C48 124.5(6) . 2_656 ? C1 O1 Nd1 161.8(4) . . ? C7 O2 Nd1 149.6(4) . . ? C4 O5 Nd2 154.3(4) . . ? C10 O6 Nd2 158.1(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.718 _refine_diff_density_min -1.633 _refine_diff_density_rms 0.149 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.500 0.331 1.000 461 181 ' ' 2 0.129 0.371 0.500 672 238 ' ' 3 0.040 0.986 0.411 19 10 ' ' 4 0.130 0.914 0.039 24 9 ' ' 5 0.175 0.159 -0.006 11 10 ' ' 6 0.870 0.086 0.961 23 10 ' ' 7 0.825 0.841 0.006 11 11 ' ' 8 0.960 0.014 0.590 20 10 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952099' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H250 Cd2 Cl14 N66 O115 Sm4' _chemical_formula_weight 5492.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.0632(10) _cell_length_b 18.0202(10) _cell_length_c 18.2840(10) _cell_angle_alpha 84.728(2) _cell_angle_beta 65.772(2) _cell_angle_gamma 71.667(2) _cell_volume 4862.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2790 _exptl_absorpt_coefficient_mu 1.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6350 _exptl_absorpt_correction_T_max 0.6928 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51346 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.10 _reflns_number_total 17129 _reflns_number_gt 12192 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+9.5761P] 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 17129 _refine_ls_number_parameters 1082 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.2254 _refine_ls_wR_factor_gt 0.2066 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl5 Cl 0.4757(2) -0.57454(17) 1.41612(19) 0.0726(8) Uani 1 1 d . . . Cl6 Cl 0.7749(3) -0.58539(19) 0.6615(2) 0.0905(10) Uani 1 1 d . . . Cl7 Cl 0.5698(3) -0.1688(2) 1.4753(2) 0.0971(12) Uani 1 1 d . . . O1W O 0.4676(5) 0.3067(4) 1.3027(4) 0.0574(17) Uani 1 1 d . . . O2W O 0.2749(6) 0.3403(5) 1.3744(5) 0.0867(15) Uani 1 1 d . . . O3W O 0.2415(6) 0.3512(5) 1.2120(7) 0.098(3) Uani 1 1 d . . . O4W O 0.3624(9) 0.4238(5) 1.2388(7) 0.113(2) Uani 1 1 d . . . O5W O 0.3991(10) 0.1939(7) 1.1467(8) 0.140(3) Uani 1 1 d . . . O6W O 0.2491(6) -0.2477(5) 1.3074(5) 0.0867(15) Uani 1 1 d . . . O7W O 0.3396(6) -0.1994(5) 1.1498(5) 0.0867(15) Uani 1 1 d . . . O8W O 0.4078(9) -0.3629(6) 1.2317(7) 0.113(2) Uani 1 1 d . . . O9W O 0.3760(9) -0.2781(5) 1.3845(7) 0.113(2) Uani 1 1 d . . . O10W O 0.5588(10) -0.3134(7) 1.2279(8) 0.140(3) Uani 1 1 d . . . O11W O 0.4742(10) -0.1510(7) 1.1574(8) 0.140(3) Uani 1 1 d . . . O12W O 0.5014(11) -0.3026(10) 1.1073(12) 0.225(9) Uani 1 1 d . . . O17 O 0.5231(5) 0.2778(6) 1.1347(5) 0.078(2) Uani 1 1 d . . . O18 O 0.4190(6) 0.3375(5) 1.0953(5) 0.081(2) Uani 1 1 d . . . O19 O 0.5579(6) 0.3228(5) 1.0108(5) 0.081(2) Uani 1 1 d . . . N33 N 0.5046(5) 0.3118(4) 1.0825(5) 0.0425(17) Uani 1 1 d . . . Sm1 Sm 0.37184(3) 0.28587(2) 1.24308(3) 0.03458(15) Uani 1 1 d . . . Sm2 Sm 0.4082(3) -0.2362(3) 1.2442(4) 0.0361(9) Uani 0.63(4) 1 d P A 1 Sm2' Sm 0.3917(14) -0.2331(5) 1.2687(18) 0.054(3) Uani 0.37(4) 1 d P A 2 Cl1 Cl 0.91467(18) -0.99069(14) 1.17935(15) 0.0577(6) Uani 1 1 d . . . Cl2 Cl 0.8750(2) -0.91117(18) 1.3953(2) 0.0774(9) Uani 1 1 d . . . Cl3 Cl 0.73908(19) -1.0514(2) 1.38414(14) 0.0704(8) Uani 1 1 d . . . Cl4 Cl 0.9874(2) -1.13612(16) 1.3467(2) 0.0823(9) Uani 1 1 d . . . Cd1 Cd 0.88043(5) -1.02178(5) 1.31809(4) 0.0454(2) Uani 0.95 1 d P B 1 Cd1' Cd 0.8424(10) -0.9584(12) 1.3380(8) 0.059(4) Uani 0.05 1 d P B 2 C23 C 0.1260(6) -0.0138(4) 1.2913(5) 0.0344(18) Uani 1 1 d . . . H23A H 0.0625 0.0012 1.3291 0.041 Uiso 1 1 calc R . . H23B H 0.1470 -0.0707 1.2826 0.041 Uiso 1 1 calc R . . C24 C 0.8975(5) -0.1928(4) 0.7083(5) 0.0308(17) Uani 1 1 d . . . H24A H 0.8904 -0.2453 0.7155 0.037 Uiso 1 1 calc R . . H24B H 0.9605 -0.1983 0.6727 0.037 Uiso 1 1 calc R . . C47 C 1.1489(6) -0.6998(5) 0.6735(6) 0.048(2) Uani 1 1 d . . . H47A H 1.1579 -0.7132 0.6193 0.057 Uiso 1 1 calc R . . H47B H 1.1936 -0.7404 0.6878 0.057 Uiso 1 1 calc R . . C48 C 0.9645(7) -0.5298(5) 0.6724(6) 0.050(2) Uani 1 1 d . . . H48A H 0.9137 -0.4815 0.6841 0.060 Uiso 1 1 calc R . . H48B H 0.9783 -0.5509 0.6195 0.060 Uiso 1 1 calc R . . C1 C 0.2276(5) 0.1658(4) 1.3372(4) 0.0319(17) Uani 1 1 d . . . C2 C 0.1423(5) 0.0796(4) 1.3771(5) 0.0301(16) Uani 1 1 d . . . H2 H 0.0777 0.0906 1.4134 0.036 Uiso 1 1 calc R . . C3 C 0.2029(5) 0.0622(4) 1.4231(4) 0.0293(16) Uani 1 1 d . . . H3 H 0.1678 0.0682 1.4819 0.035 Uiso 1 1 calc R . . C4 C 0.2456(5) -0.0462(4) 1.3403(5) 0.0341(18) Uani 1 1 d . A . C5 C 0.3184(5) 0.1308(5) 1.4168(5) 0.0365(18) Uani 1 1 d . . . H5A H 0.3000 0.1219 1.4743 0.044 Uiso 1 1 calc R . . H5B H 0.3190 0.1852 1.4089 0.044 Uiso 1 1 calc R . . C6 C 0.3260(5) -0.0637(4) 1.4309(5) 0.0327(17) Uani 1 1 d . . . H6A H 0.3038 -0.0461 1.4869 0.039 Uiso 1 1 calc R . . H6B H 0.3291 -0.1189 1.4303 0.039 Uiso 1 1 calc R . . C7 C 0.4701(5) 0.1012(4) 1.3124(5) 0.0300(17) Uani 1 1 d . . . C8 C 0.4434(5) 0.0036(4) 1.4017(4) 0.0319(17) Uani 1 1 d . . . H8 H 0.4351 0.0068 1.4583 0.038 Uiso 1 1 calc R . . C9 C 0.5447(5) -0.0206(4) 1.3447(4) 0.0299(16) Uani 1 1 d . . . H9 H 0.5841 -0.0289 1.3740 0.036 Uiso 1 1 calc R . . C10 C 0.4805(6) -0.1112(4) 1.3318(5) 0.0337(18) Uani 1 1 d . A . C11 C 0.6369(5) 0.0607(4) 1.2442(5) 0.0341(18) Uani 1 1 d . . . H11A H 0.6242 0.1152 1.2283 0.041 Uiso 1 1 calc R . . H11B H 0.6711 0.0544 1.2775 0.041 Uiso 1 1 calc R . . C12 C 0.6450(6) -0.1468(4) 1.2656(5) 0.0345(18) Uani 1 1 d . . . H12A H 0.6379 -0.1980 1.2615 0.041 Uiso 1 1 calc R . . H12B H 0.6784 -0.1520 1.2994 0.041 Uiso 1 1 calc R . . C13 C 0.7319(6) 0.0434(4) 1.1003(5) 0.0343(18) Uani 1 1 d . . . C14 C 0.7454(5) -0.0704(4) 1.1743(4) 0.0284(16) Uani 1 1 d . . . H14 H 0.7745 -0.0762 1.2124 0.034 Uiso 1 1 calc R . . C15 C 0.8154(5) -0.0898(4) 1.0874(4) 0.0307(16) Uani 1 1 d . . . H15 H 0.8774 -0.1115 1.0851 0.037 Uiso 1 1 calc R . . C16 C 0.7266(6) -0.1709(4) 1.1194(5) 0.0346(18) Uani 1 1 d . . . C17 C 0.8673(6) 0.0025(5) 0.9764(5) 0.0391(19) Uani 1 1 d . . . H17A H 0.9279 -0.0213 0.9756 0.047 Uiso 1 1 calc R . . H17B H 0.8565 0.0591 0.9731 0.047 Uiso 1 1 calc R . . C18 C 0.8517(6) -0.1954(4) 0.9876(5) 0.039(2) Uani 1 1 d . . . H18A H 0.8326 -0.2419 0.9906 0.047 Uiso 1 1 calc R . . H18B H 0.9123 -0.2129 0.9875 0.047 Uiso 1 1 calc R . . C19 C 0.8418(5) 0.0223(4) 0.8521(5) 0.0331(17) Uani 1 1 d . . . C20 C 0.9100(5) -0.1059(4) 0.8755(4) 0.0286(16) Uani 1 1 d . . . H20 H 0.9695 -0.1258 0.8788 0.034 Uiso 1 1 calc R . . C21 C 0.9203(5) -0.1033(4) 0.7892(4) 0.0311(17) Uani 1 1 d . . . H21 H 0.9842 -0.1160 0.7507 0.037 Uiso 1 1 calc R . . C22 C 0.8455(5) -0.1939(4) 0.8545(4) 0.0321(17) Uani 1 1 d . . . C25 C 0.8519(6) -0.5689(4) 0.7918(5) 0.039(2) Uani 1 1 d . . . C26 C 0.9814(6) -0.6701(4) 0.7132(5) 0.0383(19) Uani 1 1 d . . . H26 H 0.9918 -0.6849 0.6584 0.046 Uiso 1 1 calc R . . C27 C 0.9119(6) -0.7048(5) 0.7781(5) 0.040(2) Uani 1 1 d . . . H27 H 0.8924 -0.7389 0.7541 0.048 Uiso 1 1 calc R . . C28 C 1.0484(6) -0.7482(5) 0.7945(5) 0.040(2) Uani 1 1 d . . . C29 C 0.7495(6) -0.6404(5) 0.8745(5) 0.044(2) Uani 1 1 d . . . H29A H 0.7352 -0.6807 0.8542 0.053 Uiso 1 1 calc R . . H29B H 0.7043 -0.5901 0.8765 0.053 Uiso 1 1 calc R . . C30 C 0.9292(5) -0.8056(4) 0.8800(5) 0.0331(17) Uani 1 1 d . . . H30A H 0.9008 -0.8318 0.8579 0.040 Uiso 1 1 calc R . . H30B H 0.9816 -0.8454 0.8841 0.040 Uiso 1 1 calc R . . C31 C 0.6916(6) -0.6077(4) 1.0204(5) 0.041(2) Uani 1 1 d . . . C32 C 0.7697(5) -0.7388(4) 0.9809(5) 0.0342(18) Uani 1 1 d . . . H32 H 0.7436 -0.7724 0.9637 0.041 Uiso 1 1 calc R . . C33 C 0.7298(5) -0.7279(4) 1.0732(5) 0.0316(17) Uani 1 1 d . . . H33 H 0.6850 -0.7564 1.0996 0.038 Uiso 1 1 calc R . . C34 C 0.8865(5) -0.7901(4) 1.0250(5) 0.0334(17) Uani 1 1 d . . . C35 C 0.6243(6) -0.6092(5) 1.1665(5) 0.044(2) Uani 1 1 d . . . H35A H 0.5853 -0.5582 1.1603 0.053 Uiso 1 1 calc R . . H35B H 0.5860 -0.6427 1.1931 0.053 Uiso 1 1 calc R . . C36 C 0.8026(6) -0.7810(4) 1.1721(5) 0.0371(19) Uani 1 1 d . . . H36A H 0.7527 -0.8034 1.1982 0.045 Uiso 1 1 calc R . . H36B H 0.8583 -0.8215 1.1684 0.045 Uiso 1 1 calc R . . C37 C 0.6565(5) -0.5268(4) 1.2421(5) 0.0375(19) Uani 1 1 d . . . C38 C 0.6982(6) -0.6604(5) 1.2643(5) 0.040(2) Uani 1 1 d . . . H38 H 0.6530 -0.6879 1.2933 0.048 Uiso 1 1 calc R . . C39 C 0.7131(6) -0.6153(4) 1.3235(6) 0.041(2) Uani 1 1 d . . . H39 H 0.6773 -0.6230 1.3804 0.050 Uiso 1 1 calc R . . C40 C 0.8501(6) -0.7079(4) 1.2461(5) 0.041(2) Uani 1 1 d . . . C41 C 0.6706(6) -0.4686(5) 1.3508(6) 0.047(2) Uani 1 1 d . . . H41A H 0.6312 -0.4221 1.3372 0.056 Uiso 1 1 calc R . . H41B H 0.6382 -0.4789 1.4070 0.056 Uiso 1 1 calc R . . C42 C 0.8537(7) -0.6394(5) 1.3526(6) 0.052(2) Uani 1 1 d . . . H42A H 0.9099 -0.6825 1.3402 0.062 Uiso 1 1 calc R . . H42B H 0.8139 -0.6427 1.4088 0.062 Uiso 1 1 calc R . . C43 C 0.7645(6) -0.3820(5) 1.3128(5) 0.044(2) Uani 1 1 d . . . C44 C 0.8070(6) -0.4920(4) 1.3833(5) 0.043(2) Uani 1 1 d . . . H44 H 0.7716 -0.4996 1.4403 0.051 Uiso 1 1 calc R . . C45 C 0.8654(5) -0.4388(4) 1.3748(5) 0.0334(17) Uani 1 1 d . . . H45 H 0.8572 -0.4199 1.4274 0.040 Uiso 1 1 calc R . . C46 C 0.9580(7) -0.5616(5) 1.3170(5) 0.045(2) Uani 1 1 d . . . N1 N 0.1608(4) 0.1455(3) 1.3308(4) 0.0294(14) Uani 1 1 d . . . N2 N 0.2533(4) 0.1205(3) 1.3927(4) 0.0302(14) Uani 1 1 d . . . N3 N 0.1773(4) 0.0075(3) 1.3267(4) 0.0295(14) Uani 1 1 d . . . N4 N 0.2614(4) -0.0179(3) 1.3972(4) 0.0305(14) Uani 1 1 d . . . N5 N 0.4076(4) 0.0804(3) 1.3747(4) 0.0302(14) Uani 1 1 d . . . N6 N 0.5505(4) 0.0449(3) 1.2927(4) 0.0302(14) Uani 1 1 d . . . N7 N 0.4133(4) -0.0573(4) 1.3889(4) 0.0312(14) Uani 1 1 d . . . N8 N 0.5577(4) -0.0920(3) 1.3042(4) 0.0264(13) Uani 1 1 d . . . N9 N 0.6916(4) 0.0104(3) 1.1734(4) 0.0344(15) Uani 1 1 d . . . N10 N 0.8024(4) -0.0135(3) 1.0509(4) 0.0318(14) Uani 1 1 d . . . N11 N 0.6975(5) -0.1263(4) 1.1868(4) 0.0328(15) Uani 1 1 d . . . N12 N 0.7908(5) -0.1455(3) 1.0580(4) 0.0318(14) Uani 1 1 d . . . N13 N 0.8644(5) -0.0267(3) 0.9072(4) 0.0330(15) Uani 1 1 d . . . N14 N 0.8677(5) -0.0219(4) 0.7837(4) 0.0334(15) Uani 1 1 d . . . N15 N 0.8564(5) -0.1580(4) 0.9126(4) 0.0337(15) Uani 1 1 d . . . N16 N 0.8786(5) -0.1608(4) 0.7842(4) 0.0330(15) Uani 1 1 d . . . N17 N 0.9389(5) -0.5846(4) 0.7309(4) 0.0440(18) Uani 1 1 d . . . N18 N 0.8379(5) -0.6363(4) 0.8199(4) 0.0411(17) Uani 1 1 d . . . N19 N 1.0608(5) -0.7008(4) 0.7281(5) 0.050(2) Uani 1 1 d . . . N20 N 0.9600(5) -0.7486(4) 0.8249(4) 0.0373(16) Uani 1 1 d . . . N21 N 0.7445(5) -0.6585(4) 0.9553(4) 0.0391(16) Uani 1 1 d . . . N22 N 0.6881(4) -0.6439(3) 1.0872(4) 0.0350(15) Uani 1 1 d . . . N23 N 0.8670(4) -0.7748(4) 0.9580(4) 0.0346(15) Uani 1 1 d . . . N24 N 0.8092(4) -0.7604(3) 1.0921(4) 0.0346(15) Uani 1 1 d . . . N25 N 0.6664(5) -0.5991(4) 1.2169(4) 0.0389(16) Uani 1 1 d . . . N26 N 0.6865(5) -0.5340(4) 1.3014(4) 0.0412(17) Uani 1 1 d . . . N27 N 0.7878(5) -0.7158(4) 1.2212(4) 0.0375(16) Uani 1 1 d . . . N28 N 0.8106(5) -0.6480(4) 1.3012(4) 0.0412(17) Uani 1 1 d . . . N29 N 0.7495(5) -0.4516(3) 1.3435(4) 0.0384(16) Uani 1 1 d . . . N30 N 0.8343(5) -0.3749(3) 1.3276(4) 0.0412(17) Uani 1 1 d . . . N31 N 0.8739(5) -0.5648(4) 1.3425(4) 0.0434(18) Uani 1 1 d . . . N32 N 0.9561(5) -0.4891(4) 1.3303(4) 0.0422(17) Uani 1 1 d . . . O1 O 0.2580(4) 0.2179(3) 1.3009(3) 0.0386(13) Uani 1 1 d . . . O2 O 0.4575(4) 0.1642(3) 1.2775(3) 0.0359(13) Uani 1 1 d . . . O3 O 0.7076(4) 0.1119(3) 1.0861(4) 0.0462(15) Uani 1 1 d . . . O4 O 0.8056(4) 0.0936(3) 0.8618(4) 0.0436(14) Uani 1 1 d . . . O5 O 0.2852(4) -0.1128(3) 1.3091(4) 0.0448(15) Uani 1 1 d . . . O6 O 0.4720(4) -0.1713(3) 1.3113(3) 0.0405(13) Uani 1 1 d . . . O7 O 0.6977(5) -0.2229(4) 1.1123(4) 0.0563(18) Uani 1 1 d . . . O8 O 0.8121(5) -0.2465(4) 0.8660(4) 0.0520(17) Uani 1 1 d . . . O9 O 0.8007(5) -0.5041(4) 0.8154(4) 0.0584(18) Uani 1 1 d . . . O10 O 0.6522(5) -0.5369(3) 1.0157(4) 0.0556(18) Uani 1 1 d . . . O11 O 0.6251(5) -0.4648(3) 1.2149(4) 0.0568(18) Uani 1 1 d . . . O12 O 0.7231(5) -0.3349(4) 1.2798(4) 0.0541(17) Uani 1 1 d . . . O13 O 1.1050(4) -0.7842(3) 0.8176(4) 0.0463(15) Uani 1 1 d . . . O14 O 0.9597(4) -0.8261(3) 1.0245(4) 0.0453(14) Uani 1 1 d . . . O15 O 0.9290(4) -0.7492(3) 1.2200(4) 0.0495(16) Uani 1 1 d . . . O16 O 1.0277(5) -0.6176(3) 1.2851(4) 0.0613(19) 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 Cl5 0.0702(19) 0.0674(17) 0.0795(19) -0.0106(14) -0.0276(16) -0.0198(14) Cl6 0.111(3) 0.0706(19) 0.112(3) 0.0119(18) -0.057(2) -0.0423(19) Cl7 0.139(3) 0.112(3) 0.100(2) 0.048(2) -0.083(3) -0.082(3) O1W 0.055(4) 0.051(4) 0.078(5) 0.008(3) -0.041(4) -0.015(3) O2W 0.076(3) 0.086(3) 0.074(3) -0.007(3) -0.013(3) -0.014(3) O3W 0.064(5) 0.068(5) 0.189(10) 0.071(6) -0.079(6) -0.036(4) O4W 0.162(6) 0.070(3) 0.132(5) 0.016(3) -0.066(5) -0.062(4) O5W 0.180(8) 0.107(5) 0.159(7) -0.009(5) -0.074(6) -0.067(5) O6W 0.076(3) 0.086(3) 0.074(3) -0.007(3) -0.013(3) -0.014(3) O7W 0.076(3) 0.086(3) 0.074(3) -0.007(3) -0.013(3) -0.014(3) O8W 0.162(6) 0.070(3) 0.132(5) 0.016(3) -0.066(5) -0.062(4) O9W 0.162(6) 0.070(3) 0.132(5) 0.016(3) -0.066(5) -0.062(4) O10W 0.180(8) 0.107(5) 0.159(7) -0.009(5) -0.074(6) -0.067(5) O11W 0.180(8) 0.107(5) 0.159(7) -0.009(5) -0.074(6) -0.067(5) O12W 0.119(12) 0.162(14) 0.24(2) -0.022(13) 0.019(12) 0.039(10) O17 0.036(4) 0.133(7) 0.058(5) -0.014(5) -0.019(4) -0.012(4) O18 0.069(6) 0.083(6) 0.097(6) 0.037(5) -0.038(5) -0.036(5) O19 0.067(5) 0.105(6) 0.058(5) 0.012(4) -0.007(4) -0.036(5) N33 0.029(4) 0.051(4) 0.045(5) 0.004(3) -0.010(4) -0.015(3) Sm1 0.0322(3) 0.0251(2) 0.0479(3) 0.00512(17) -0.0180(2) -0.00935(17) Sm2 0.0370(11) 0.0289(9) 0.0462(17) 0.0076(8) -0.0205(11) -0.0116(7) Sm2' 0.060(4) 0.0326(10) 0.084(7) -0.005(2) -0.046(5) -0.0066(17) Cl1 0.0585(15) 0.0493(13) 0.0470(13) 0.0058(10) -0.0016(11) -0.0201(11) Cl2 0.0568(17) 0.0721(17) 0.088(2) -0.0309(16) -0.0073(15) -0.0194(14) Cl3 0.0562(16) 0.142(3) 0.0344(12) 0.0235(14) -0.0193(11) -0.0623(18) Cl4 0.073(2) 0.0516(15) 0.126(3) -0.0014(16) -0.050(2) -0.0086(13) Cd1 0.0335(4) 0.0519(4) 0.0463(4) 0.0018(3) -0.0071(3) -0.0196(3) Cd1' 0.040(8) 0.105(14) 0.029(7) 0.020(8) 0.004(6) -0.049(9) C23 0.040(5) 0.035(4) 0.035(4) 0.013(3) -0.022(4) -0.013(3) C24 0.026(4) 0.025(3) 0.037(4) 0.001(3) -0.013(3) -0.003(3) C47 0.040(5) 0.030(4) 0.060(6) 0.016(4) -0.008(4) -0.016(4) C48 0.061(6) 0.026(4) 0.052(6) 0.015(4) -0.025(5) 0.000(4) C1 0.030(4) 0.028(4) 0.028(4) -0.007(3) -0.004(3) -0.005(3) C2 0.021(4) 0.031(4) 0.035(4) 0.010(3) -0.010(3) -0.009(3) C3 0.032(4) 0.035(4) 0.015(3) 0.008(3) -0.002(3) -0.013(3) C4 0.027(4) 0.036(4) 0.040(5) 0.015(3) -0.012(4) -0.016(3) C5 0.031(4) 0.045(4) 0.032(4) -0.006(3) -0.012(4) -0.009(4) C6 0.030(4) 0.031(4) 0.034(4) 0.016(3) -0.011(3) -0.011(3) C7 0.032(4) 0.029(4) 0.035(4) 0.001(3) -0.017(4) -0.012(3) C8 0.042(5) 0.031(4) 0.026(4) 0.001(3) -0.020(4) -0.006(3) C9 0.028(4) 0.029(4) 0.032(4) 0.006(3) -0.011(3) -0.010(3) C10 0.043(5) 0.026(4) 0.037(4) 0.006(3) -0.025(4) -0.006(3) C11 0.028(4) 0.029(4) 0.041(5) -0.002(3) -0.006(4) -0.014(3) C12 0.041(5) 0.029(4) 0.030(4) 0.005(3) -0.009(4) -0.013(3) C13 0.045(5) 0.027(4) 0.044(5) 0.010(3) -0.027(4) -0.018(3) C14 0.029(4) 0.023(3) 0.030(4) 0.002(3) -0.013(3) -0.004(3) C15 0.026(4) 0.033(4) 0.031(4) 0.003(3) -0.012(3) -0.006(3) C16 0.036(5) 0.029(4) 0.035(4) 0.002(3) -0.012(4) -0.009(3) C17 0.049(5) 0.044(4) 0.041(5) 0.010(4) -0.023(4) -0.032(4) C18 0.050(5) 0.026(4) 0.034(4) 0.007(3) -0.017(4) -0.005(4) C19 0.031(4) 0.032(4) 0.039(4) 0.007(3) -0.012(4) -0.018(3) C20 0.028(4) 0.027(3) 0.031(4) 0.002(3) -0.017(3) -0.002(3) C21 0.028(4) 0.034(4) 0.030(4) 0.006(3) -0.011(3) -0.010(3) C22 0.036(5) 0.031(4) 0.029(4) 0.000(3) -0.017(4) -0.004(3) C25 0.035(5) 0.028(4) 0.046(5) 0.007(3) -0.018(4) 0.002(3) C26 0.034(5) 0.032(4) 0.044(5) 0.007(3) -0.021(4) 0.001(3) C27 0.043(5) 0.033(4) 0.047(5) 0.003(4) -0.023(4) -0.009(4) C28 0.041(5) 0.036(4) 0.047(5) 0.009(4) -0.017(4) -0.019(4) C29 0.035(5) 0.039(4) 0.050(5) 0.002(4) -0.020(4) 0.003(4) C30 0.033(4) 0.021(3) 0.038(4) 0.005(3) -0.007(4) -0.009(3) C31 0.032(5) 0.028(4) 0.055(6) 0.001(4) -0.008(4) -0.012(3) C32 0.023(4) 0.025(4) 0.049(5) 0.009(3) -0.015(4) -0.002(3) C33 0.023(4) 0.024(3) 0.038(4) -0.003(3) -0.006(3) -0.001(3) C34 0.029(5) 0.028(4) 0.042(5) 0.010(3) -0.012(4) -0.012(3) C35 0.023(4) 0.039(4) 0.057(6) -0.004(4) -0.011(4) 0.006(3) C36 0.038(5) 0.021(3) 0.046(5) 0.002(3) -0.014(4) -0.005(3) C37 0.024(4) 0.033(4) 0.035(4) -0.002(3) -0.004(3) 0.008(3) C38 0.032(5) 0.035(4) 0.037(5) -0.007(3) -0.002(4) -0.003(3) C39 0.035(5) 0.025(4) 0.060(6) 0.002(4) -0.018(4) -0.005(3) C40 0.046(6) 0.028(4) 0.053(5) 0.016(4) -0.025(4) -0.011(4) C41 0.039(5) 0.031(4) 0.057(6) -0.005(4) -0.014(4) 0.001(4) C42 0.066(7) 0.029(4) 0.070(6) 0.005(4) -0.045(6) -0.005(4) C43 0.041(5) 0.031(4) 0.045(5) -0.002(4) -0.010(4) -0.001(4) C44 0.055(6) 0.029(4) 0.031(4) -0.001(3) -0.007(4) -0.010(4) C45 0.036(5) 0.024(4) 0.043(5) 0.010(3) -0.021(4) -0.009(3) C46 0.062(7) 0.036(5) 0.040(5) 0.014(4) -0.018(5) -0.024(4) N1 0.032(4) 0.030(3) 0.033(3) 0.008(3) -0.018(3) -0.013(3) N2 0.038(4) 0.029(3) 0.026(3) 0.004(2) -0.015(3) -0.012(3) N3 0.024(3) 0.029(3) 0.035(4) 0.011(3) -0.011(3) -0.012(3) N4 0.032(4) 0.033(3) 0.031(3) 0.012(3) -0.015(3) -0.016(3) N5 0.023(3) 0.029(3) 0.033(4) 0.004(3) -0.011(3) -0.001(3) N6 0.020(3) 0.022(3) 0.046(4) 0.009(3) -0.014(3) -0.005(2) N7 0.022(3) 0.033(3) 0.038(4) 0.002(3) -0.011(3) -0.008(3) N8 0.021(3) 0.023(3) 0.038(4) 0.008(2) -0.015(3) -0.009(2) N9 0.034(4) 0.023(3) 0.040(4) 0.006(3) -0.011(3) -0.007(3) N10 0.037(4) 0.027(3) 0.032(3) 0.011(3) -0.012(3) -0.015(3) N11 0.037(4) 0.034(3) 0.029(3) 0.010(3) -0.009(3) -0.020(3) N12 0.040(4) 0.029(3) 0.027(3) 0.009(3) -0.011(3) -0.016(3) N13 0.041(4) 0.028(3) 0.032(3) 0.006(3) -0.016(3) -0.013(3) N14 0.038(4) 0.031(3) 0.038(4) 0.011(3) -0.020(3) -0.014(3) N15 0.041(4) 0.035(3) 0.031(3) 0.007(3) -0.016(3) -0.018(3) N16 0.035(4) 0.037(3) 0.032(4) 0.005(3) -0.013(3) -0.018(3) N17 0.032(4) 0.041(4) 0.047(4) 0.014(3) -0.010(3) -0.006(3) N18 0.029(4) 0.036(4) 0.040(4) 0.013(3) -0.007(3) 0.001(3) N19 0.036(4) 0.032(4) 0.077(6) 0.021(3) -0.025(4) -0.007(3) N20 0.031(4) 0.030(3) 0.049(4) 0.012(3) -0.017(3) -0.007(3) N21 0.041(4) 0.028(3) 0.039(4) 0.007(3) -0.015(3) -0.002(3) N22 0.030(4) 0.023(3) 0.044(4) -0.002(3) -0.014(3) 0.002(3) N23 0.029(4) 0.032(3) 0.034(4) 0.005(3) -0.009(3) -0.004(3) N24 0.032(4) 0.027(3) 0.038(4) 0.001(3) -0.013(3) -0.001(3) N25 0.039(4) 0.031(3) 0.039(4) -0.005(3) -0.012(3) -0.005(3) N26 0.049(5) 0.025(3) 0.043(4) -0.004(3) -0.017(4) -0.003(3) N27 0.034(4) 0.031(3) 0.037(4) -0.002(3) -0.011(3) -0.001(3) N28 0.035(4) 0.033(3) 0.052(4) -0.004(3) -0.022(3) 0.003(3) N29 0.052(5) 0.025(3) 0.044(4) 0.006(3) -0.022(4) -0.016(3) N30 0.038(4) 0.020(3) 0.051(4) 0.006(3) -0.012(3) 0.001(3) N31 0.045(5) 0.025(3) 0.050(4) 0.007(3) -0.015(4) -0.006(3) N32 0.036(4) 0.032(3) 0.051(4) 0.009(3) -0.016(3) -0.005(3) O1 0.046(4) 0.029(3) 0.050(3) 0.017(2) -0.020(3) -0.027(3) O2 0.032(3) 0.026(3) 0.042(3) 0.003(2) -0.010(3) -0.005(2) O3 0.058(4) 0.033(3) 0.046(4) 0.011(2) -0.022(3) -0.013(3) O4 0.048(4) 0.030(3) 0.054(4) 0.004(2) -0.028(3) -0.004(3) O5 0.059(4) 0.028(3) 0.061(4) 0.006(3) -0.038(3) -0.015(3) O6 0.040(3) 0.034(3) 0.050(3) 0.002(2) -0.015(3) -0.019(3) O7 0.074(5) 0.055(4) 0.042(4) 0.002(3) -0.009(3) -0.042(4) O8 0.084(5) 0.047(3) 0.040(3) 0.009(3) -0.025(3) -0.043(4) O9 0.049(4) 0.037(3) 0.070(5) 0.011(3) -0.014(4) -0.004(3) O10 0.056(4) 0.030(3) 0.056(4) 0.006(3) -0.014(3) 0.006(3) O11 0.064(5) 0.034(3) 0.071(5) 0.002(3) -0.037(4) 0.000(3) O12 0.063(4) 0.043(3) 0.058(4) 0.019(3) -0.034(4) -0.010(3) O13 0.036(3) 0.031(3) 0.068(4) 0.017(3) -0.027(3) -0.002(2) O14 0.031(3) 0.044(3) 0.055(4) 0.007(3) -0.018(3) -0.005(3) O15 0.038(4) 0.042(3) 0.059(4) -0.009(3) -0.016(3) -0.002(3) O16 0.051(4) 0.029(3) 0.079(5) 0.000(3) -0.011(4) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W Sm1 2.433(6) . ? O2W Sm1 2.369(8) . ? O3W Sm1 2.434(7) . ? O4W Sm1 2.435(9) . ? O5W Sm1 2.334(11) . ? O6W Sm2' 2.33(2) . ? O6W Sm2 2.547(10) . ? O7W Sm2 2.398(11) . ? O7W Sm2' 2.62(2) . ? O8W Sm2 2.319(11) . ? O8W Sm2' 2.396(12) . ? O9W Sm2' 2.14(3) . ? O9W Sm2 2.490(13) . ? O10W Sm2 2.413(16) . ? O10W Sm2' 2.58(2) . ? O11W Sm2 2.305(14) . ? O11W Sm2' 2.59(3) . ? O12W Sm2 2.51(2) . ? O12W Sm2' 2.91(3) . ? O17 N33 1.186(10) . ? O17 Sm1 2.496(8) . ? O18 N33 1.309(11) . ? O18 Sm1 2.653(8) . ? O19 N33 1.293(10) . ? N33 Sm1 2.987(8) . ? Sm1 O2 2.413(5) . ? Sm1 O1 2.442(5) . ? Sm2 O6 2.494(9) . ? Sm2 O5 2.502(9) . ? Sm2' O5 2.293(14) . ? Sm2' O6 2.392(10) . ? Cl1 Cd1 2.412(3) . ? Cl1 Cd1' 2.683(15) . ? Cl2 Cd1' 1.751(17) . ? Cl2 Cd1 2.503(3) . ? Cl3 Cd1 2.421(3) . ? Cl3 Cd1' 2.647(15) . ? Cl4 Cd1 2.464(3) . ? C23 N3 1.433(10) . ? C23 N14 1.437(10) 2_657 ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.424(10) . ? C24 N1 1.471(9) 2_657 ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C47 N19 1.428(11) . ? C47 N30 1.458(10) 2_747 ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N17 1.416(11) . ? C48 N32 1.478(13) 2_747 ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C1 O1 1.225(9) . ? C1 N1 1.351(10) . ? C1 N2 1.369(10) . ? C2 N1 1.435(9) . ? C2 N3 1.475(9) . ? C2 C3 1.528(10) . ? C2 H2 0.9900 . ? C3 N4 1.461(9) . ? C3 N2 1.490(10) . ? C3 H3 0.9900 . ? C4 O5 1.234(9) . ? C4 N4 1.354(10) . ? C4 N3 1.357(10) . ? C5 N2 1.418(10) . ? C5 N5 1.426(10) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.404(10) . ? C6 N4 1.472(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.253(9) . ? C7 N5 1.324(10) . ? C7 N6 1.352(10) . ? C8 N7 1.422(10) . ? C8 N5 1.457(9) . ? C8 C9 1.547(11) . ? C8 H8 0.9900 . ? C9 N6 1.447(9) . ? C9 N8 1.453(9) . ? C9 H9 0.9900 . ? C10 O6 1.244(9) . ? C10 N8 1.350(10) . ? C10 N7 1.361(10) . ? C11 N9 1.435(10) . ? C11 N6 1.478(10) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.425(10) . ? C12 N11 1.437(10) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.213(9) . ? C13 N10 1.348(10) . ? C13 N9 1.402(10) . ? C14 N11 1.436(10) . ? C14 N9 1.460(9) . ? C14 C15 1.535(10) . ? C14 H14 0.9900 . ? C15 N12 1.421(10) . ? C15 N10 1.465(9) . ? C15 H15 0.9900 . ? C16 O7 1.225(10) . ? C16 N11 1.357(10) . ? C16 N12 1.372(10) . ? C17 N10 1.434(10) . ? C17 N13 1.439(10) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.440(10) . ? C18 N15 1.455(10) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.231(9) . ? C19 N13 1.374(10) . ? C19 N14 1.379(10) . ? C20 N13 1.435(9) . ? C20 N15 1.447(10) . ? C20 C21 1.513(10) . ? C20 H20 0.9900 . ? C21 N16 1.456(10) . ? C21 N14 1.479(9) . ? C21 H21 0.9900 . ? C22 O8 1.213(10) . ? C22 N16 1.342(10) . ? C22 N15 1.394(9) . ? C25 O9 1.205(10) . ? C25 N18 1.329(11) . ? C25 N17 1.400(11) . ? C26 N19 1.422(11) . ? C26 N17 1.483(10) . ? C26 C27 1.543(12) . ? C26 H26 0.9900 . ? C27 N20 1.440(11) . ? C27 N18 1.451(10) . ? C27 H27 0.9900 . ? C28 O13 1.193(10) . ? C28 N20 1.378(11) . ? C28 N19 1.400(11) . ? C29 N18 1.448(11) . ? C29 N21 1.456(11) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.415(10) . ? C30 N20 1.436(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O10 1.255(10) . ? C31 N22 1.319(11) . ? C31 N21 1.367(10) . ? C32 N21 1.465(9) . ? C32 N23 1.469(10) . ? C32 C33 1.545(11) . ? C32 H32 0.9900 . ? C33 N22 1.452(9) . ? C33 N24 1.465(10) . ? C33 H33 0.9900 . ? C34 O14 1.210(10) . ? C34 N24 1.371(10) . ? C34 N23 1.378(10) . ? C35 N25 1.434(11) . ? C35 N22 1.456(10) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N27 1.441(10) . ? C36 N24 1.441(10) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O11 1.234(10) . ? C37 N26 1.357(11) . ? C37 N25 1.358(10) . ? C38 N25 1.448(11) . ? C38 N27 1.466(10) . ? C38 C39 1.554(12) . ? C38 H38 0.9900 . ? C39 N26 1.463(10) . ? C39 N28 1.466(11) . ? C39 H39 0.9900 . ? C40 O15 1.225(11) . ? C40 N28 1.349(11) . ? C40 N27 1.365(11) . ? C41 N29 1.424(12) . ? C41 N26 1.439(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N28 1.455(11) . ? C42 N31 1.467(11) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O12 1.209(11) . ? C43 N30 1.371(12) . ? C43 N29 1.380(11) . ? C44 N29 1.436(11) . ? C44 N31 1.456(10) . ? C44 C45 1.542(12) . ? C44 H44 0.9900 . ? C45 N32 1.450(10) . ? C45 N30 1.469(10) . ? C45 H45 0.9900 . ? C46 O16 1.249(11) . ? C46 N31 1.334(12) . ? C46 N32 1.339(11) . ? N1 C24 1.471(9) 2_657 ? N14 C23 1.437(10) 2_657 ? N30 C47 1.458(10) 2_747 ? N32 C48 1.478(13) 2_747 ? 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 Sm2' O6W Sm2 8.4(5) . . ? Sm2 O7W Sm2' 8.0(5) . . ? Sm2 O8W Sm2' 10.0(6) . . ? Sm2' O9W Sm2 5.5(4) . . ? Sm2 O10W Sm2' 8.8(5) . . ? Sm2 O11W Sm2' 7.1(3) . . ? Sm2 O12W Sm2' 2.9(4) . . ? N33 O17 Sm1 102.6(6) . . ? N33 O18 Sm1 91.4(6) . . ? O17 N33 O19 128.9(8) . . ? O17 N33 O18 117.2(8) . . ? O19 N33 O18 113.7(8) . . ? O17 N33 Sm1 54.6(5) . . ? O19 N33 Sm1 175.8(6) . . ? O18 N33 Sm1 62.6(5) . . ? O5W Sm1 O2W 144.3(4) . . ? O5W Sm1 O2 75.1(4) . . ? O2W Sm1 O2 98.9(3) . . ? O5W Sm1 O1W 131.7(4) . . ? O2W Sm1 O1W 73.4(3) . . ? O2 Sm1 O1W 68.3(2) . . ? O5W Sm1 O3W 82.5(5) . . ? O2W Sm1 O3W 84.3(4) . . ? O2 Sm1 O3W 145.6(2) . . ? O1W Sm1 O3W 143.3(3) . . ? O5W Sm1 O4W 133.3(4) . . ? O2W Sm1 O4W 73.8(4) . . ? O2 Sm1 O4W 138.6(3) . . ? O1W Sm1 O4W 70.7(3) . . ? O3W Sm1 O4W 75.3(4) . . ? O5W Sm1 O1 72.2(4) . . ? O2W Sm1 O1 72.1(3) . . ? O2 Sm1 O1 78.89(19) . . ? O1W Sm1 O1 127.1(2) . . ? O3W Sm1 O1 69.5(2) . . ? O4W Sm1 O1 132.6(3) . . ? O5W Sm1 O17 73.6(4) . . ? O2W Sm1 O17 141.3(3) . . ? O2 Sm1 O17 81.7(3) . . ? O1W Sm1 O17 71.0(2) . . ? O3W Sm1 O17 116.7(3) . . ? O4W Sm1 O17 80.5(4) . . ? O1 Sm1 O17 144.0(3) . . ? O5W Sm1 O18 66.5(4) . . ? O2W Sm1 O18 136.4(3) . . ? O2 Sm1 O18 123.2(2) . . ? O1W Sm1 O18 109.5(3) . . ? O3W Sm1 O18 67.9(3) . . ? O4W Sm1 O18 67.2(3) . . ? O1 Sm1 O18 123.1(2) . . ? O17 Sm1 O18 48.8(3) . . ? O5W Sm1 N33 68.9(4) . . ? O2W Sm1 N33 145.3(3) . . ? O2 Sm1 N33 101.7(2) . . ? O1W Sm1 N33 88.6(2) . . ? O3W Sm1 N33 93.9(3) . . ? O4W Sm1 N33 72.2(3) . . ? O1 Sm1 N33 139.4(2) . . ? O17 Sm1 N33 22.8(2) . . ? O18 Sm1 N33 26.0(2) . . ? O11W Sm2 O8W 134.7(6) . . ? O11W Sm2 O7W 71.7(4) . . ? O8W Sm2 O7W 88.0(4) . . ? O11W Sm2 O10W 86.6(5) . . ? O8W Sm2 O10W 77.2(4) . . ? O7W Sm2 O10W 131.6(5) . . ? O11W Sm2 O9W 139.6(5) . . ? O8W Sm2 O9W 79.4(4) . . ? O7W Sm2 O9W 141.7(4) . . ? O10W Sm2 O9W 80.8(5) . . ? O11W Sm2 O6 71.0(4) . . ? O8W Sm2 O6 135.6(4) . . ? O7W Sm2 O6 135.9(3) . . ? O10W Sm2 O6 68.1(3) . . ? O9W Sm2 O6 68.6(3) . . ? O11W Sm2 O5 83.1(4) . . ? O8W Sm2 O5 132.6(4) . . ? O7W Sm2 O5 77.8(3) . . ? O10W Sm2 O5 143.2(4) . . ? O9W Sm2 O5 84.5(4) . . ? O6 Sm2 O5 75.1(3) . . ? O11W Sm2 O12W 70.8(6) . . ? O8W Sm2 O12W 63.9(6) . . ? O7W Sm2 O12W 64.9(5) . . ? O10W Sm2 O12W 67.2(6) . . ? O9W Sm2 O12W 135.1(5) . . ? O6 Sm2 O12W 121.7(5) . . ? O5 Sm2 O12W 139.4(5) . . ? O11W Sm2 O6W 134.2(5) . . ? O8W Sm2 O6W 68.2(4) . . ? O7W Sm2 O6W 70.6(3) . . ? O10W Sm2 O6W 138.5(4) . . ? O9W Sm2 O6W 71.1(4) . . ? O6 Sm2 O6W 124.5(4) . . ? O5 Sm2 O6W 64.5(3) . . ? O12W Sm2 O6W 113.7(6) . . ? O9W Sm2' O5 98.4(12) . . ? O9W Sm2' O6W 81.8(11) . . ? O5 Sm2' O6W 71.2(6) . . ? O9W Sm2' O6 76.4(6) . . ? O5 Sm2' O6 81.0(4) . . ? O6W Sm2' O6 141.5(13) . . ? O9W Sm2' O8W 85.2(7) . . ? O5 Sm2' O8W 140.7(7) . . ? O6W Sm2' O8W 70.6(5) . . ? O6 Sm2' O8W 137.1(5) . . ? O9W Sm2' O10W 84.2(6) . . ? O5 Sm2' O10W 146.5(6) . . ? O6W Sm2' O10W 141.6(5) . . ? O6 Sm2' O10W 67.1(4) . . ? O8W Sm2' O10W 72.8(5) . . ? O9W Sm2' O11W 144.1(5) . . ? O5 Sm2' O11W 81.3(6) . . ? O6W Sm2' O11W 130.4(7) . . ? O6 Sm2' O11W 68.0(6) . . ? O8W Sm2' O11W 117.6(12) . . ? O10W Sm2' O11W 77.6(9) . . ? O9W Sm2' O7W 151.6(10) . . ? O5 Sm2' O7W 77.2(4) . . ? O6W Sm2' O7W 70.2(4) . . ? O6 Sm2' O7W 129.2(10) . . ? O8W Sm2' O7W 81.4(6) . . ? O10W Sm2' O7W 115.1(12) . . ? O11W Sm2' O7W 63.8(7) . . ? O9W Sm2' O12W 132.3(6) . . ? O5 Sm2' O12W 129.1(10) . . ? O6W Sm2' O12W 107.4(7) . . ? O6 Sm2' O12W 110.8(11) . . ? O8W Sm2' O12W 56.8(7) . . ? O10W Sm2' O12W 59.3(7) . . ? O11W Sm2' O12W 60.8(8) . . ? O7W Sm2' O12W 56.7(7) . . ? Cd1 Cl1 Cd1' 24.9(4) . . ? Cd1' Cl2 Cd1 23.2(7) . . ? Cd1 Cl3 Cd1' 25.3(4) . . ? Cl1 Cd1 Cl3 113.28(9) . . ? Cl1 Cd1 Cl4 117.44(11) . . ? Cl3 Cd1 Cl4 102.42(12) . . ? Cl1 Cd1 Cl2 110.60(11) . . ? Cl3 Cd1 Cl2 108.48(10) . . ? Cl4 Cd1 Cl2 103.78(11) . . ? Cl2 Cd1' Cl3 129.5(7) . . ? Cl2 Cd1' Cl1 130.2(6) . . ? Cl3 Cd1' Cl1 98.5(6) . . ? N3 C23 N14 113.9(6) . 2_657 ? N3 C23 H23A 108.8 . . ? N14 C23 H23A 108.8 2_657 . ? N3 C23 H23B 108.8 . . ? N14 C23 H23B 108.8 2_657 . ? H23A C23 H23B 107.7 . . ? N16 C24 N1 113.8(6) . 2_657 ? N16 C24 H24A 108.8 . . ? N1 C24 H24A 108.8 2_657 . ? N16 C24 H24B 108.8 . . ? N1 C24 H24B 108.8 2_657 . ? H24A C24 H24B 107.7 . . ? N19 C47 N30 114.4(7) . 2_747 ? N19 C47 H47A 108.7 . . ? N30 C47 H47A 108.7 2_747 . ? N19 C47 H47B 108.7 . . ? N30 C47 H47B 108.7 2_747 . ? H47A C47 H47B 107.6 . . ? N17 C48 N32 112.7(7) . 2_747 ? N17 C48 H48A 109.1 . . ? N32 C48 H48A 109.1 2_747 . ? N17 C48 H48B 109.1 . . ? N32 C48 H48B 109.1 2_747 . ? H48A C48 H48B 107.8 . . ? O1 C1 N1 125.3(7) . . ? O1 C1 N2 125.8(7) . . ? N1 C1 N2 108.9(7) . . ? N1 C2 N3 112.4(6) . . ? N1 C2 C3 104.2(6) . . ? N3 C2 C3 102.6(5) . . ? N1 C2 H2 112.3 . . ? N3 C2 H2 112.3 . . ? C3 C2 H2 112.3 . . ? N4 C3 N2 112.2(6) . . ? N4 C3 C2 104.7(6) . . ? N2 C3 C2 102.9(6) . . ? N4 C3 H3 112.2 . . ? N2 C3 H3 112.2 . . ? C2 C3 H3 112.2 . . ? O5 C4 N4 124.0(7) . . ? O5 C4 N3 125.9(7) . . ? N4 C4 N3 110.0(7) . . ? N2 C5 N5 114.3(6) . . ? N2 C5 H5A 108.7 . . ? N5 C5 H5A 108.7 . . ? N2 C5 H5B 108.7 . . ? N5 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 113.4(6) . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6B 108.9 . . ? N4 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N5 125.4(7) . . ? O2 C7 N6 124.8(7) . . ? N5 C7 N6 109.8(7) . . ? N7 C8 N5 116.4(6) . . ? N7 C8 C9 103.8(6) . . ? N5 C8 C9 103.0(6) . . ? N7 C8 H8 111.0 . . ? N5 C8 H8 111.0 . . ? C9 C8 H8 111.0 . . ? N6 C9 N8 113.4(6) . . ? N6 C9 C8 102.5(6) . . ? N8 C9 C8 103.3(6) . . ? N6 C9 H9 112.3 . . ? N8 C9 H9 112.3 . . ? C8 C9 H9 112.3 . . ? O6 C10 N8 125.5(7) . . ? O6 C10 N7 124.3(8) . . ? N8 C10 N7 110.2(6) . . ? N9 C11 N6 113.5(6) . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11B 108.9 . . ? N6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 114.4(6) . . ? N8 C12 H12A 108.7 . . ? N11 C12 H12A 108.7 . . ? N8 C12 H12B 108.7 . . ? N11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N10 126.8(8) . . ? O3 C13 N9 124.9(8) . . ? N10 C13 N9 108.3(6) . . ? N11 C14 N9 114.0(6) . . ? N11 C14 C15 102.8(6) . . ? N9 C14 C15 104.3(6) . . ? N11 C14 H14 111.7 . . ? N9 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N12 C15 N10 115.1(6) . . ? N12 C15 C14 104.5(6) . . ? N10 C15 C14 102.7(6) . . ? N12 C15 H15 111.3 . . ? N10 C15 H15 111.3 . . ? C14 C15 H15 111.3 . . ? O7 C16 N11 126.3(8) . . ? O7 C16 N12 124.8(7) . . ? N11 C16 N12 108.8(6) . . ? N10 C17 N13 113.2(6) . . ? N10 C17 H17A 108.9 . . ? N13 C17 H17A 108.9 . . ? N10 C17 H17B 108.9 . . ? N13 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N12 C18 N15 113.8(6) . . ? N12 C18 H18A 108.8 . . ? N15 C18 H18A 108.8 . . ? N12 C18 H18B 108.8 . . ? N15 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N13 125.9(7) . . ? O4 C19 N14 125.9(7) . . ? N13 C19 N14 108.2(6) . . ? N13 C20 N15 113.0(6) . . ? N13 C20 C21 105.4(6) . . ? N15 C20 C21 104.8(6) . . ? N13 C20 H20 111.1 . . ? N15 C20 H20 111.1 . . ? C21 C20 H20 111.1 . . ? N16 C21 N14 113.2(6) . . ? N16 C21 C20 103.3(6) . . ? N14 C21 C20 102.8(6) . . ? N16 C21 H21 112.3 . . ? N14 C21 H21 112.3 . . ? C20 C21 H21 112.3 . . ? O8 C22 N16 126.1(7) . . ? O8 C22 N15 125.4(7) . . ? N16 C22 N15 108.6(7) . . ? O9 C25 N18 126.9(8) . . ? O9 C25 N17 124.4(8) . . ? N18 C25 N17 108.7(6) . . ? N19 C26 N17 113.6(7) . . ? N19 C26 C27 104.3(7) . . ? N17 C26 C27 103.0(6) . . ? N19 C26 H26 111.8 . . ? N17 C26 H26 111.8 . . ? C27 C26 H26 111.8 . . ? N20 C27 N18 114.6(7) . . ? N20 C27 C26 103.5(7) . . ? N18 C27 C26 103.5(6) . . ? N20 C27 H27 111.5 . . ? N18 C27 H27 111.5 . . ? C26 C27 H27 111.5 . . ? O13 C28 N20 126.8(8) . . ? O13 C28 N19 126.1(8) . . ? N20 C28 N19 107.0(7) . . ? N18 C29 N21 112.1(7) . . ? N18 C29 H29A 109.2 . . ? N21 C29 H29A 109.2 . . ? N18 C29 H29B 109.2 . . ? N21 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? N23 C30 N20 114.5(6) . . ? N23 C30 H30A 108.6 . . ? N20 C30 H30A 108.6 . . ? N23 C30 H30B 108.6 . . ? N20 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? O10 C31 N22 125.8(8) . . ? O10 C31 N21 123.8(8) . . ? N22 C31 N21 110.4(7) . . ? N21 C32 N23 114.2(7) . . ? N21 C32 C33 102.8(6) . . ? N23 C32 C33 104.3(6) . . ? N21 C32 H32 111.7 . . ? N23 C32 H32 111.7 . . ? C33 C32 H32 111.7 . . ? N22 C33 N24 115.4(6) . . ? N22 C33 C32 103.4(6) . . ? N24 C33 C32 103.1(6) . . ? N22 C33 H33 111.4 . . ? N24 C33 H33 111.4 . . ? C32 C33 H33 111.4 . . ? O14 C34 N24 125.5(8) . . ? O14 C34 N23 125.2(8) . . ? N24 C34 N23 109.2(7) . . ? N25 C35 N22 113.7(7) . . ? N25 C35 H35A 108.8 . . ? N22 C35 H35A 108.8 . . ? N25 C35 H35B 108.8 . . ? N22 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N27 C36 N24 113.4(6) . . ? N27 C36 H36A 108.9 . . ? N24 C36 H36A 108.9 . . ? N27 C36 H36B 108.9 . . ? N24 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? O11 C37 N26 125.9(8) . . ? O11 C37 N25 124.9(8) . . ? N26 C37 N25 109.2(7) . . ? N25 C38 N27 115.6(7) . . ? N25 C38 C39 103.2(6) . . ? N27 C38 C39 103.4(7) . . ? N25 C38 H38 111.3 . . ? N27 C38 H38 111.3 . . ? C39 C38 H38 111.3 . . ? N26 C39 N28 113.0(7) . . ? N26 C39 C38 103.0(7) . . ? N28 C39 C38 102.3(6) . . ? N26 C39 H39 112.6 . . ? N28 C39 H39 112.6 . . ? C38 C39 H39 112.6 . . ? O15 C40 N28 127.4(8) . . ? O15 C40 N27 123.7(8) . . ? N28 C40 N27 108.9(7) . . ? N29 C41 N26 115.2(7) . . ? N29 C41 H41A 108.5 . . ? N26 C41 H41A 108.5 . . ? N29 C41 H41B 108.5 . . ? N26 C41 H41B 108.5 . . ? H41A C41 H41B 107.5 . . ? N28 C42 N31 112.2(7) . . ? N28 C42 H42A 109.2 . . ? N31 C42 H42A 109.2 . . ? N28 C42 H42B 109.2 . . ? N31 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? O12 C43 N30 125.7(8) . . ? O12 C43 N29 126.7(9) . . ? N30 C43 N29 107.6(7) . . ? N29 C44 N31 114.6(7) . . ? N29 C44 C45 104.2(6) . . ? N31 C44 C45 102.8(7) . . ? N29 C44 H44 111.6 . . ? N31 C44 H44 111.6 . . ? C45 C44 H44 111.6 . . ? N32 C45 N30 113.1(7) . . ? N32 C45 C44 102.7(6) . . ? N30 C45 C44 102.8(6) . . ? N32 C45 H45 112.5 . . ? N30 C45 H45 112.5 . . ? C44 C45 H45 112.5 . . ? O16 C46 N31 125.1(8) . . ? O16 C46 N32 125.3(9) . . ? N31 C46 N32 109.7(8) . . ? C1 N1 C2 113.1(6) . . ? C1 N1 C24 124.0(6) . 2_657 ? C2 N1 C24 122.2(6) . 2_657 ? C1 N2 C5 122.8(7) . . ? C1 N2 C3 110.7(6) . . ? C5 N2 C3 126.5(6) . . ? C4 N3 C23 122.1(6) . . ? C4 N3 C2 111.7(6) . . ? C23 N3 C2 122.7(6) . . ? C4 N4 C3 111.0(6) . . ? C4 N4 C6 123.9(6) . . ? C3 N4 C6 125.0(6) . . ? C7 N5 C5 123.9(7) . . ? C7 N5 C8 112.3(6) . . ? C5 N5 C8 123.4(7) . . ? C7 N6 C9 112.3(6) . . ? C7 N6 C11 122.0(6) . . ? C9 N6 C11 122.5(6) . . ? C10 N7 C6 123.0(7) . . ? C10 N7 C8 111.8(7) . . ? C6 N7 C8 125.2(6) . . ? C10 N8 C12 123.5(6) . . ? C10 N8 C9 110.9(6) . . ? C12 N8 C9 121.7(6) . . ? C13 N9 C11 119.0(6) . . ? C13 N9 C14 110.5(6) . . ? C11 N9 C14 123.5(6) . . ? C13 N10 C17 122.7(6) . . ? C13 N10 C15 113.2(6) . . ? C17 N10 C15 123.2(6) . . ? C16 N11 C14 112.0(6) . . ? C16 N11 C12 123.4(6) . . ? C14 N11 C12 122.3(6) . . ? C16 N12 C15 110.8(6) . . ? C16 N12 C18 120.1(6) . . ? C15 N12 C18 122.7(7) . . ? C19 N13 C20 111.9(6) . . ? C19 N13 C17 121.9(6) . . ? C20 N13 C17 123.5(6) . . ? C19 N14 C23 121.5(6) . 2_657 ? C19 N14 C21 111.0(6) . . ? C23 N14 C21 123.1(6) 2_657 . ? C22 N15 C20 110.2(6) . . ? C22 N15 C18 120.7(6) . . ? C20 N15 C18 123.3(6) . . ? C22 N16 C24 124.4(6) . . ? C22 N16 C21 112.5(6) . . ? C24 N16 C21 120.4(6) . . ? C25 N17 C48 122.3(7) . . ? C25 N17 C26 110.5(7) . . ? C48 N17 C26 121.6(7) . . ? C25 N18 C29 121.8(7) . . ? C25 N18 C27 114.0(7) . . ? C29 N18 C27 122.8(7) . . ? C28 N19 C26 112.4(7) . . ? C28 N19 C47 121.2(7) . . ? C26 N19 C47 125.1(8) . . ? C28 N20 C30 122.2(7) . . ? C28 N20 C27 112.7(7) . . ? C30 N20 C27 122.3(7) . . ? C31 N21 C29 123.6(7) . . ? C31 N21 C32 110.6(7) . . ? C29 N21 C32 122.8(7) . . ? C31 N22 C33 112.2(6) . . ? C31 N22 C35 122.9(6) . . ? C33 N22 C35 121.7(7) . . ? C34 N23 C30 123.6(7) . . ? C34 N23 C32 110.9(6) . . ? C30 N23 C32 124.0(7) . . ? C34 N24 C36 122.5(6) . . ? C34 N24 C33 112.2(6) . . ? C36 N24 C33 122.6(7) . . ? C37 N25 C35 121.4(7) . . ? C37 N25 C38 112.4(7) . . ? C35 N25 C38 123.6(7) . . ? C37 N26 C41 123.0(7) . . ? C37 N26 C39 111.9(6) . . ? C41 N26 C39 123.0(7) . . ? C40 N27 C36 123.8(7) . . ? C40 N27 C38 112.0(7) . . ? C36 N27 C38 122.8(7) . . ? C40 N28 C42 120.2(7) . . ? C40 N28 C39 113.1(7) . . ? C42 N28 C39 122.8(7) . . ? C43 N29 C41 120.7(7) . . ? C43 N29 C44 112.9(7) . . ? C41 N29 C44 124.7(7) . . ? C43 N30 C47 122.7(7) . 2_747 ? C43 N30 C45 112.5(7) . . ? C47 N30 C45 120.6(7) 2_747 . ? C46 N31 C44 112.1(7) . . ? C46 N31 C42 122.0(7) . . ? C44 N31 C42 122.8(8) . . ? C46 N32 C45 112.4(7) . . ? C46 N32 C48 123.1(7) . 2_747 ? C45 N32 C48 121.0(7) . 2_747 ? C1 O1 Sm1 155.1(5) . . ? C7 O2 Sm1 156.9(5) . . ? C4 O5 Sm2' 160.6(6) . . ? C4 O5 Sm2 161.3(6) . . ? Sm2' O5 Sm2 8.6(7) . . ? C10 O6 Sm2' 150.2(6) . . ? C10 O6 Sm2 150.7(5) . . ? Sm2' O6 Sm2 9.5(7) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.311 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.162 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.018 0.500 621 229 ' ' 2 0.028 0.471 1.000 760 261 ' ' 3 0.441 0.517 0.172 53 24 ' ' 4 0.561 0.482 0.822 52 15 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952100' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H284 Cd2 Cl14 Eu4 N66 O132' _chemical_formula_weight 5804.83 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.0389(17) _cell_length_b 17.9558(17) _cell_length_c 18.3397(19) _cell_angle_alpha 84.823(4) _cell_angle_beta 65.727(4) _cell_angle_gamma 71.616(4) _cell_volume 4848.9(8) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2964 _exptl_absorpt_coefficient_mu 1.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7010 _exptl_absorpt_correction_T_max 0.7718 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52076 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16888 _reflns_number_gt 11851 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 16888 _refine_ls_number_parameters 1069 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1313 _refine_ls_R_factor_gt 0.1102 _refine_ls_wR_factor_ref 0.3432 _refine_ls_wR_factor_gt 0.3205 _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_restrained_S_all 1.251 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl5 Cl 0.5250(3) 0.0744(3) -0.4171(3) 0.0713(11) Uani 1 1 d . . . Cl6 Cl 0.4320(4) 0.6680(3) 0.5238(3) 0.0919(17) Uani 1 1 d . . . Cl7 Cl 0.2242(4) 0.0874(3) 0.3389(4) 0.0925(16) Uani 1 1 d . . . N33 N 0.5030(7) 0.8129(6) 0.0862(8) 0.049(3) Uani 1 1 d . . . O1W O 0.3416(11) 0.2993(8) 0.1503(8) 0.091(3) Uani 1 1 d . . . O2W O 0.2455(8) 0.2543(7) 0.3094(8) 0.080(4) Uani 1 1 d . . . O3W O 0.4077(10) 0.1355(8) 0.2271(13) 0.120(5) Uani 1 1 d . . . O4W O 0.4774(14) 0.3524(13) 0.1520(12) 0.139(5) Uani 1 1 d . . . O5W O 0.3855(10) 0.2154(8) 0.3777(8) 0.091(3) Uani 1 1 d . . . O6W O 0.5628(10) 0.1884(8) 0.2137(12) 0.120(5) Uani 1 1 d . . . O7W O 0.5021(14) 0.2019(13) 0.1046(12) 0.139(5) Uani 1 1 d . . . O8W O 0.4691(6) 0.8064(5) 0.3029(5) 0.044(2) Uani 1 1 d . . . O9W O 0.2757(7) 0.8398(6) 0.3772(6) 0.060(3) Uani 1 1 d . . . O10W O 0.3663(8) 0.9228(6) 0.2325(7) 0.068(3) Uani 1 1 d . . . O11W O 0.2418(8) 0.8520(6) 0.2146(9) 0.081(4) Uani 1 1 d . . . O12W O 0.3985(10) 0.6893(7) 0.1439(6) 0.077(4) Uani 1 1 d . . . O17 O 0.5580(8) 0.8193(9) 0.0079(8) 0.086(4) Uani 1 1 d . . . O18 O 0.4165(8) 0.8372(9) 0.0974(9) 0.093(3) Uani 1 1 d . . . O19 O 0.5212(8) 0.7732(10) 0.1382(9) 0.093(3) Uani 1 1 d . . . Eu1 Eu 0.40022(6) 0.26667(4) 0.25424(6) 0.0603(3) Uani 1 1 d . . . Eu2 Eu 0.37166(4) 0.78557(3) 0.24451(4) 0.0362(2) Uani 1 1 d . . . Cl1 Cl -0.2617(3) 0.4489(3) 0.3842(2) 0.0712(13) Uani 1 1 d . . . Cl2 Cl -0.0861(3) 0.5095(2) 0.1779(2) 0.0567(9) Uani 1 1 d . . . Cl3 Cl -0.0119(3) 0.3655(3) 0.3450(3) 0.0775(12) Uani 1 1 d . . . Cl4 Cl -0.1261(3) 0.5905(3) 0.3926(3) 0.0701(11) Uani 1 1 d . . . Cd1 Cd -0.12013(6) 0.47883(6) 0.31653(6) 0.0469(3) Uani 1 1 d . . . C1 C 0.4780(7) 0.3880(7) 0.3321(7) 0.030(2) Uani 1 1 d . . . C2 C 0.5434(7) 0.4790(6) 0.3440(7) 0.031(2) Uani 1 1 d . . . H2 H 0.5843 0.4702 0.3718 0.038 Uiso 1 1 calc R . . C3 C 0.4441(7) 0.5033(6) 0.4036(7) 0.032(2) Uani 1 1 d . . . H3 H 0.4375 0.5056 0.4596 0.038 Uiso 1 1 calc R . . C4 C 0.4693(8) 0.6029(6) 0.3126(7) 0.031(3) Uani 1 1 d . . . C5 C 0.3209(8) 0.4397(8) 0.4330(7) 0.037(3) Uani 1 1 d . . . H5A H 0.2994 0.4592 0.4882 0.044 Uiso 1 1 calc R . . H5B H 0.3226 0.3845 0.4347 0.044 Uiso 1 1 calc R . . C6 C 0.3152(8) 0.6334(8) 0.4183(6) 0.036(3) Uani 1 1 d . . . H6A H 0.2955 0.6264 0.4760 0.043 Uiso 1 1 calc R . . H6B H 0.3160 0.6878 0.4086 0.043 Uiso 1 1 calc R . . C7 C 0.2433(8) 0.4541(7) 0.3404(8) 0.041(3) Uani 1 1 d . . . C8 C 0.2034(7) 0.5639(6) 0.4221(6) 0.025(2) Uani 1 1 d . . . H8 H 0.1677 0.5714 0.4807 0.030 Uiso 1 1 calc R . . C9 C 0.1409(7) 0.5810(7) 0.3757(7) 0.035(3) Uani 1 1 d . . . H9 H 0.0760 0.5925 0.4117 0.042 Uiso 1 1 calc R . . C10 C 0.2251(8) 0.6680(6) 0.3387(7) 0.030(2) Uani 1 1 d . . . C11 C 0.1255(8) 0.4870(7) 0.2889(7) 0.037(3) Uani 1 1 d . . . H11A H 0.1471 0.4298 0.2796 0.044 Uiso 1 1 calc R . . H11B H 0.0616 0.5017 0.3260 0.044 Uiso 1 1 calc R . . C12 C 0.1034(7) 0.6962(7) 0.2900(6) 0.033(2) Uani 1 1 d . . . H12A H 0.0399 0.7040 0.3259 0.039 Uiso 1 1 calc R . . H12B H 0.1132 0.7477 0.2812 0.039 Uiso 1 1 calc R . . C13 C 0.1584(8) 0.4786(7) 0.1467(8) 0.039(3) Uani 1 1 d . . . C14 C 0.0807(7) 0.6029(6) 0.2098(7) 0.029(2) Uani 1 1 d . . . H14 H 0.0169 0.6154 0.2488 0.035 Uiso 1 1 calc R . . C15 C 0.0893(8) 0.6070(7) 0.1216(6) 0.033(2) Uani 1 1 d . . . H15 H 0.0299 0.6263 0.1180 0.039 Uiso 1 1 calc R . . C16 C 0.1547(9) 0.6941(8) 0.1426(7) 0.041(3) Uani 1 1 d . . . C17 C 0.1327(10) 0.4980(8) 0.0224(8) 0.046(3) Uani 1 1 d . . . H17A H 0.1417 0.4414 0.0253 0.055 Uiso 1 1 calc R . . H17B H 0.0726 0.5237 0.0225 0.055 Uiso 1 1 calc R . . C18 C 0.1483(9) 0.6982(6) 0.0121(6) 0.037(3) Uani 1 1 d . . . H18A H 0.0876 0.7161 0.0122 0.044 Uiso 1 1 calc R . . H18B H 0.1678 0.7446 0.0095 0.044 Uiso 1 1 calc R . . C19 C 0.2713(9) 0.4572(8) -0.1022(8) 0.041(3) Uani 1 1 d . . . C20 C 0.1846(8) 0.5902(6) -0.0871(6) 0.033(2) Uani 1 1 d . . . H20 H 0.1222 0.6117 -0.0842 0.039 Uiso 1 1 calc R . . C21 C 0.2560(6) 0.5711(6) -0.1755(6) 0.025(2) Uani 1 1 d . . . H21 H 0.2275 0.5772 -0.2140 0.030 Uiso 1 1 calc R . . C22 C 0.2753(9) 0.6710(7) -0.1183(8) 0.038(3) Uani 1 1 d . . . C23 C 0.3633(7) 0.4401(6) -0.2438(7) 0.031(2) Uani 1 1 d . . . H23A H 0.3290 0.4479 -0.2771 0.038 Uiso 1 1 calc R . . H23B H 0.3750 0.3852 -0.2287 0.038 Uiso 1 1 calc R . . C24 C 0.6439(7) 0.3520(6) 0.2642(7) 0.030(2) Uani 1 1 d . . . H24A H 0.6785 0.3439 0.2972 0.036 Uiso 1 1 calc R . . H24B H 0.6344 0.3020 0.2591 0.036 Uiso 1 1 calc R . . C25 C -0.2342(9) 0.1186(7) 0.3152(8) 0.044(3) Uani 1 1 d . . . C26 C -0.1934(9) 0.0081(7) 0.3841(8) 0.039(3) Uani 1 1 d . . . H26 H -0.2300 0.0016 0.4409 0.047 Uiso 1 1 calc R . . C27 C -0.1336(9) 0.0637(7) 0.3743(7) 0.040(3) Uani 1 1 d . . . H27 H -0.1419 0.0837 0.4264 0.048 Uiso 1 1 calc R . . C28 C -0.0406(10) -0.0620(7) 0.3153(8) 0.044(3) Uani 1 1 d . . . C29 C -0.1494(9) 0.2015(7) 0.3271(9) 0.048(3) Uani 1 1 d . . . H29A H -0.1947 0.2427 0.3141 0.057 Uiso 1 1 calc R . . H29B H -0.1579 0.2137 0.3814 0.057 Uiso 1 1 calc R . . C30 C 0.0349(8) 0.0321(7) 0.3287(8) 0.039(3) Uani 1 1 d . . . H30A H 0.0197 0.0556 0.3809 0.046 Uiso 1 1 calc R . . H30B H 0.0853 -0.0164 0.3195 0.046 Uiso 1 1 calc R . . C31 C -0.0488(9) 0.2514(7) 0.2052(8) 0.040(3) Uani 1 1 d . . . C32 C 0.0223(9) 0.1688(7) 0.2834(7) 0.038(3) Uani 1 1 d . . . H32 H 0.0135 0.1838 0.3376 0.045 Uiso 1 1 calc R . . C33 C 0.0884(8) 0.2077(7) 0.2190(7) 0.038(3) Uani 1 1 d . . . H33 H 0.1083 0.2419 0.2426 0.046 Uiso 1 1 calc R . . C34 C 0.1475(9) 0.0690(8) 0.2090(8) 0.044(3) Uani 1 1 d . . . C35 C 0.0703(8) 0.3071(6) 0.1212(7) 0.033(2) Uani 1 1 d . . . H35A H 0.1011 0.3311 0.1428 0.039 Uiso 1 1 calc R . . H35B H 0.0183 0.3488 0.1184 0.039 Uiso 1 1 calc R . . C36 C 0.2508(8) 0.1412(7) 0.1236(8) 0.044(3) Uani 1 1 d . . . H36A H 0.2641 0.1819 0.1446 0.053 Uiso 1 1 calc R . . H36B H 0.2970 0.0911 0.1211 0.053 Uiso 1 1 calc R . . C37 C 0.1127(8) 0.2907(7) -0.0234(7) 0.036(3) Uani 1 1 d . . . C38 C 0.2299(6) 0.2393(6) 0.0201(6) 0.029(2) Uani 1 1 d . . . H38 H 0.2547 0.2737 0.0378 0.035 Uiso 1 1 calc R . . C39 C 0.2708(8) 0.2280(8) -0.0737(8) 0.041(3) Uani 1 1 d . . . H39 H 0.3164 0.2557 -0.1009 0.049 Uiso 1 1 calc R . . C40 C 0.3076(8) 0.1060(7) -0.0212(9) 0.044(3) Uani 1 1 d . . . C41 C 0.1983(9) 0.2790(7) -0.1714(7) 0.037(3) Uani 1 1 d . . . H41A H 0.2490 0.3006 -0.1973 0.045 Uiso 1 1 calc R . . H41B H 0.1432 0.3201 -0.1686 0.045 Uiso 1 1 calc R . . C42 C 0.3742(9) 0.1084(7) -0.1650(8) 0.043(3) Uani 1 1 d . . . H42A H 0.4119 0.1426 -0.1909 0.052 Uiso 1 1 calc R . . H42B H 0.4138 0.0574 -0.1589 0.052 Uiso 1 1 calc R . . C43 C 0.1503(8) 0.2049(6) -0.2468(7) 0.034(3) Uani 1 1 d . . . C44 C 0.3013(8) 0.1582(7) -0.2628(8) 0.039(3) Uani 1 1 d . . . H44 H 0.3467 0.1855 -0.2925 0.046 Uiso 1 1 calc R . . C45 C 0.2852(8) 0.1128(7) -0.3208(7) 0.037(3) Uani 1 1 d . . . H45 H 0.3208 0.1211 -0.3774 0.044 Uiso 1 1 calc R . . C46 C 0.3435(9) 0.0261(8) -0.2415(8) 0.043(3) Uani 1 1 d . . . C47 C 0.1483(9) 0.1355(7) -0.3516(9) 0.046(3) Uani 1 1 d . . . H47A H 0.0923 0.1792 -0.3395 0.055 Uiso 1 1 calc R . . H47B H 0.1889 0.1395 -0.4072 0.055 Uiso 1 1 calc R . . C48 C -0.3322(9) 0.0340(7) 0.3531(9) 0.048(3) Uani 1 1 d . . . H48A H -0.3734 0.0806 0.3414 0.058 Uiso 1 1 calc R . . H48B H -0.3621 0.0225 0.4093 0.058 Uiso 1 1 calc R . . N1 N 0.5567(6) 0.4099(5) 0.3048(5) 0.0267(19) Uani 1 1 d . . . N2 N 0.4107(6) 0.4436(5) 0.3895(5) 0.0291(19) Uani 1 1 d . . . N3 N 0.5505(6) 0.5455(6) 0.2910(6) 0.037(2) Uani 1 1 d . . . N4 N 0.4056(6) 0.5809(6) 0.3772(6) 0.035(2) Uani 1 1 d . . . N5 N 0.2560(6) 0.4845(6) 0.3997(6) 0.033(2) Uani 1 1 d . . . N6 N 0.1766(6) 0.5088(5) 0.3262(6) 0.031(2) Uani 1 1 d . . . N7 N 0.2509(6) 0.6202(6) 0.3925(5) 0.033(2) Uani 1 1 d . . . N8 N 0.1612(6) 0.6469(6) 0.3282(6) 0.033(2) Uani 1 1 d . . . N9 N 0.1329(6) 0.5230(6) 0.2149(6) 0.033(2) Uani 1 1 d . . . N10 N 0.1363(7) 0.5268(6) 0.0936(6) 0.038(2) Uani 1 1 d . . . N11 N 0.1219(6) 0.6614(5) 0.2143(6) 0.031(2) Uani 1 1 d . . . N12 N 0.1440(7) 0.6596(6) 0.0863(6) 0.037(2) Uani 1 1 d . . . N13 N 0.1992(6) 0.5130(5) -0.0501(5) 0.0293(19) Uani 1 1 d . . . N14 N 0.3099(7) 0.4892(5) -0.1736(6) 0.034(2) Uani 1 1 d . . . N15 N 0.2100(7) 0.6469(5) -0.0584(5) 0.032(2) Uani 1 1 d . . . N16 N 0.3038(6) 0.6267(5) -0.1860(6) 0.032(2) Uani 1 1 d . . . N17 N -0.2498(8) 0.0503(6) 0.3411(7) 0.044(3) Uani 1 1 d . . . N18 N -0.1652(7) 0.1270(6) 0.3263(7) 0.044(3) Uani 1 1 d . . . N19 N -0.1276(7) -0.0634(6) 0.3450(7) 0.045(3) Uani 1 1 d . . . N20 N -0.0438(7) 0.0124(6) 0.3313(7) 0.045(3) Uani 1 1 d . . . N21 N -0.0610(7) 0.2029(6) 0.2722(7) 0.043(3) Uani 1 1 d . . . N22 N 0.0379(7) 0.2498(6) 0.1757(6) 0.034(2) Uani 1 1 d . . . N23 N 0.0634(7) 0.0847(6) 0.2686(7) 0.045(3) Uani 1 1 d . . . N24 N 0.1620(7) 0.1356(6) 0.1782(6) 0.037(2) Uani 1 1 d . . . N25 N 0.1330(6) 0.2746(6) 0.0393(6) 0.034(2) Uani 1 1 d . . . N26 N 0.1902(7) 0.2596(6) -0.0926(6) 0.042(2) Uani 1 1 d . . . N27 N 0.2556(7) 0.1597(6) 0.0442(6) 0.041(2) Uani 1 1 d . . . N28 N 0.3097(6) 0.1424(5) -0.0864(6) 0.037(2) Uani 1 1 d . . . N29 N 0.2128(7) 0.2138(6) -0.2194(6) 0.041(2) Uani 1 1 d . . . N30 N 0.1897(7) 0.1444(6) -0.3002(6) 0.043(3) Uani 1 1 d . . . N31 N 0.3336(7) 0.0974(6) -0.2164(6) 0.042(2) Uani 1 1 d . . . N32 N 0.3139(7) 0.0329(6) -0.3016(7) 0.044(3) Uani 1 1 d . . . O1 O 0.4710(6) 0.3281(4) 0.3121(5) 0.0379(14) Uani 1 1 d . . . O2 O 0.2819(7) 0.3894(5) 0.3097(6) 0.051(2) Uani 1 1 d . . . O3 O 0.1949(6) 0.4076(5) 0.1358(6) 0.045(2) Uani 1 1 d . . . O4 O 0.2940(7) 0.3883(5) -0.0862(6) 0.049(2) Uani 1 1 d . . . O5 O 0.4548(5) 0.6651(4) 0.2799(5) 0.0359(18) Uani 1 1 d . . . O6 O 0.2562(6) 0.7212(4) 0.3027(5) 0.0379(14) Uani 1 1 d . . . O7 O 0.1913(6) 0.7465(5) 0.1320(5) 0.046(2) Uani 1 1 d . . . O8 O 0.3030(7) 0.7248(6) -0.1138(6) 0.053(2) Uani 1 1 d . . . O9 O -0.2758(8) 0.1679(6) 0.2776(6) 0.061(3) Uani 1 1 d . . . O10 O -0.1073(6) 0.2870(5) 0.1837(6) 0.050(2) Uani 1 1 d . . . O11 O 0.0389(5) 0.3256(5) -0.0238(5) 0.044(2) Uani 1 1 d . . . O12 O 0.0699(7) 0.2482(6) -0.2203(6) 0.053(2) Uani 1 1 d . . . O13 O 0.0289(7) -0.1156(5) 0.2832(6) 0.060(3) Uani 1 1 d . . . O14 O 0.2022(6) 0.0034(5) 0.1848(6) 0.055(3) Uani 1 1 d . . . O15 O 0.3458(7) 0.0365(5) -0.0158(6) 0.059(3) Uani 1 1 d . . . O16 O 0.3784(7) -0.0378(6) -0.2169(6) 0.056(3) 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 Cl5 0.075(3) 0.062(3) 0.077(3) -0.012(2) -0.028(2) -0.021(2) Cl6 0.134(4) 0.109(4) 0.088(3) 0.042(3) -0.076(3) -0.076(4) Cl7 0.113(4) 0.071(3) 0.120(4) 0.020(3) -0.065(4) -0.044(3) N33 0.031(5) 0.027(6) 0.076(8) 0.001(5) -0.002(6) -0.014(4) O1W 0.111(8) 0.076(6) 0.083(6) 0.007(5) -0.044(6) -0.019(6) O2W 0.064(7) 0.052(7) 0.093(9) 0.009(6) -0.007(6) -0.013(6) O3W 0.079(6) 0.057(6) 0.217(14) -0.052(7) -0.050(8) -0.010(5) O4W 0.131(11) 0.160(13) 0.120(10) 0.017(9) -0.039(9) -0.055(10) O5W 0.111(8) 0.076(6) 0.083(6) 0.007(5) -0.044(6) -0.019(6) O6W 0.079(6) 0.057(6) 0.217(14) -0.052(7) -0.050(8) -0.010(5) O7W 0.131(11) 0.160(13) 0.120(10) 0.017(9) -0.039(9) -0.055(10) O8W 0.043(5) 0.034(5) 0.054(5) -0.009(4) -0.014(4) -0.017(4) O9W 0.050(6) 0.060(7) 0.060(6) -0.021(5) -0.005(5) -0.021(5) O10W 0.073(7) 0.037(6) 0.089(8) 0.019(5) -0.030(6) -0.019(5) O11W 0.068(7) 0.052(7) 0.156(12) 0.054(7) -0.080(8) -0.027(6) O12W 0.137(11) 0.066(8) 0.056(6) 0.017(5) -0.042(7) -0.069(8) O17 0.056(7) 0.114(11) 0.083(9) 0.024(8) -0.019(7) -0.036(7) O18 0.045(5) 0.125(9) 0.105(7) -0.001(6) -0.031(5) -0.018(5) O19 0.045(5) 0.125(9) 0.105(7) -0.001(6) -0.031(5) -0.018(5) Eu1 0.0628(5) 0.0296(4) 0.1129(7) 0.0056(4) -0.0604(5) -0.0128(3) Eu2 0.0343(4) 0.0239(3) 0.0542(4) 0.0020(3) -0.0215(3) -0.0090(3) Cl1 0.051(2) 0.149(4) 0.0359(17) 0.017(2) -0.0168(15) -0.064(3) Cl2 0.060(2) 0.052(2) 0.0452(18) 0.0063(15) -0.0048(16) -0.0239(17) Cl3 0.067(3) 0.053(2) 0.114(4) -0.001(2) -0.040(3) -0.013(2) Cl4 0.058(2) 0.060(2) 0.077(3) -0.024(2) -0.009(2) -0.0174(19) Cd1 0.0359(5) 0.0521(6) 0.0502(6) 0.0010(4) -0.0094(4) -0.0208(5) C1 0.028(6) 0.033(6) 0.034(6) 0.012(5) -0.016(5) -0.014(5) C2 0.028(6) 0.021(5) 0.051(7) -0.002(5) -0.027(5) 0.001(4) C3 0.029(6) 0.026(6) 0.038(6) 0.004(5) -0.015(5) -0.003(5) C4 0.036(6) 0.016(5) 0.055(7) -0.006(5) -0.029(6) -0.008(5) C5 0.034(6) 0.055(8) 0.027(6) 0.009(5) -0.010(5) -0.026(6) C6 0.035(6) 0.047(7) 0.023(5) -0.010(5) -0.010(5) -0.009(5) C7 0.033(6) 0.034(7) 0.059(8) 0.015(6) -0.023(6) -0.012(5) C8 0.022(5) 0.026(6) 0.022(5) 0.005(4) -0.006(4) -0.004(4) C9 0.022(5) 0.025(6) 0.047(7) 0.013(5) -0.006(5) -0.007(5) C10 0.037(6) 0.019(5) 0.038(6) 0.003(4) -0.014(5) -0.016(5) C11 0.027(6) 0.037(7) 0.048(7) -0.004(5) -0.017(5) -0.007(5) C12 0.027(5) 0.039(7) 0.028(6) 0.000(5) -0.012(5) -0.002(5) C13 0.033(6) 0.035(7) 0.051(7) 0.008(5) -0.021(6) -0.010(5) C14 0.020(5) 0.027(6) 0.034(6) 0.008(4) -0.007(4) -0.006(4) C15 0.036(6) 0.040(7) 0.024(5) -0.005(5) -0.013(5) -0.012(5) C16 0.042(7) 0.042(7) 0.034(6) -0.002(5) -0.004(5) -0.022(6) C17 0.061(8) 0.038(7) 0.056(8) 0.003(6) -0.034(7) -0.026(6) C18 0.048(7) 0.018(5) 0.029(6) -0.006(4) -0.006(5) -0.002(5) C19 0.044(7) 0.043(8) 0.046(7) 0.009(6) -0.025(6) -0.020(6) C20 0.043(7) 0.022(6) 0.031(6) 0.000(4) -0.015(5) -0.007(5) C21 0.018(5) 0.023(5) 0.035(6) 0.004(4) -0.014(4) -0.004(4) C22 0.045(7) 0.020(6) 0.050(7) 0.009(5) -0.022(6) -0.007(5) C23 0.025(5) 0.020(5) 0.044(6) 0.000(4) -0.003(5) -0.014(4) C24 0.022(5) 0.013(5) 0.052(7) 0.006(4) -0.015(5) -0.003(4) C25 0.056(8) 0.021(6) 0.046(7) -0.003(5) -0.021(6) 0.001(6) C26 0.042(7) 0.030(6) 0.042(7) 0.006(5) -0.012(6) -0.014(5) C27 0.048(7) 0.033(7) 0.038(6) 0.004(5) -0.014(6) -0.015(6) C28 0.056(8) 0.030(7) 0.046(7) 0.010(5) -0.024(7) -0.011(6) C29 0.052(8) 0.029(7) 0.057(8) 0.014(6) -0.015(7) -0.019(6) C30 0.029(6) 0.024(6) 0.056(7) 0.012(5) -0.023(6) 0.004(5) C31 0.041(7) 0.032(7) 0.045(7) 0.011(5) -0.015(6) -0.013(6) C32 0.051(7) 0.037(7) 0.029(6) 0.013(5) -0.018(6) -0.018(6) C33 0.040(7) 0.038(7) 0.033(6) -0.001(5) -0.014(5) -0.008(5) C34 0.051(8) 0.042(8) 0.043(7) 0.000(6) -0.015(6) -0.023(7) C35 0.031(6) 0.015(5) 0.045(7) 0.001(4) -0.010(5) -0.005(4) C36 0.040(7) 0.031(7) 0.062(8) 0.011(6) -0.030(7) -0.003(5) C37 0.041(7) 0.024(6) 0.043(7) 0.007(5) -0.021(6) -0.008(5) C38 0.016(5) 0.021(5) 0.038(6) -0.006(4) -0.009(4) 0.011(4) C39 0.032(6) 0.041(7) 0.051(7) -0.006(6) -0.013(6) -0.018(5) C40 0.029(6) 0.022(6) 0.068(9) -0.006(6) -0.015(6) 0.005(5) C41 0.052(7) 0.029(6) 0.044(7) 0.010(5) -0.034(6) -0.013(5) C42 0.049(7) 0.021(6) 0.056(8) -0.005(5) -0.027(6) 0.002(5) C43 0.043(7) 0.017(5) 0.033(6) 0.005(4) -0.009(5) -0.007(5) C44 0.031(6) 0.032(7) 0.046(7) -0.004(5) -0.011(5) -0.006(5) C45 0.033(6) 0.039(7) 0.038(6) -0.005(5) -0.007(5) -0.018(5) C46 0.039(7) 0.047(8) 0.042(7) -0.006(6) -0.020(6) -0.003(6) C47 0.056(8) 0.024(6) 0.068(9) 0.004(6) -0.046(7) 0.002(6) C48 0.041(7) 0.029(7) 0.074(9) -0.002(6) -0.027(7) -0.003(5) N1 0.023(4) 0.014(4) 0.044(5) 0.012(4) -0.017(4) -0.005(3) N2 0.018(4) 0.034(5) 0.029(5) -0.007(4) -0.005(4) -0.005(4) N3 0.028(5) 0.029(5) 0.052(6) -0.004(4) -0.019(5) -0.001(4) N4 0.029(5) 0.041(6) 0.044(6) 0.003(4) -0.023(5) -0.011(4) N5 0.030(5) 0.032(5) 0.044(5) 0.015(4) -0.021(4) -0.014(4) N6 0.027(5) 0.024(5) 0.051(6) 0.009(4) -0.023(4) -0.011(4) N7 0.034(5) 0.034(5) 0.034(5) 0.004(4) -0.017(4) -0.010(4) N8 0.032(5) 0.032(5) 0.040(5) 0.013(4) -0.018(4) -0.017(4) N9 0.037(5) 0.031(5) 0.048(6) 0.012(4) -0.030(5) -0.017(4) N10 0.051(6) 0.045(6) 0.038(5) 0.018(4) -0.025(5) -0.035(5) N11 0.038(5) 0.020(5) 0.043(5) 0.009(4) -0.023(5) -0.013(4) N12 0.045(6) 0.030(5) 0.036(5) 0.012(4) -0.016(5) -0.017(4) N13 0.037(5) 0.024(5) 0.028(5) 0.001(4) -0.011(4) -0.014(4) N14 0.043(6) 0.025(5) 0.036(5) 0.005(4) -0.016(5) -0.011(4) N15 0.045(6) 0.018(5) 0.030(5) 0.000(4) -0.011(4) -0.013(4) N16 0.033(5) 0.021(5) 0.047(6) 0.003(4) -0.022(5) -0.008(4) N17 0.054(7) 0.027(6) 0.053(6) 0.000(5) -0.028(6) -0.007(5) N18 0.041(6) 0.022(5) 0.065(7) 0.009(5) -0.017(5) -0.014(4) N19 0.041(6) 0.018(5) 0.066(7) 0.002(5) -0.019(5) 0.001(4) N20 0.039(6) 0.039(6) 0.051(6) 0.013(5) -0.011(5) -0.017(5) N21 0.033(5) 0.024(5) 0.061(7) 0.015(5) -0.014(5) -0.005(4) N22 0.038(5) 0.028(5) 0.039(5) 0.002(4) -0.018(5) -0.009(4) N23 0.038(6) 0.033(6) 0.062(7) 0.016(5) -0.021(5) -0.012(5) N24 0.035(5) 0.025(5) 0.042(6) 0.006(4) -0.015(5) -0.001(4) N25 0.028(5) 0.032(5) 0.037(5) -0.007(4) -0.009(4) -0.007(4) N26 0.027(5) 0.041(6) 0.051(6) -0.004(5) -0.012(5) -0.003(4) N27 0.045(6) 0.023(5) 0.043(6) 0.001(4) -0.009(5) -0.007(4) N28 0.031(5) 0.010(4) 0.061(7) -0.004(4) -0.019(5) 0.008(4) N29 0.040(6) 0.028(5) 0.042(6) -0.009(4) -0.013(5) 0.004(4) N30 0.041(6) 0.043(6) 0.046(6) -0.002(5) -0.025(5) -0.002(5) N31 0.038(6) 0.042(6) 0.040(6) -0.004(5) -0.010(5) -0.008(5) N32 0.048(6) 0.018(5) 0.055(6) -0.007(4) -0.017(5) 0.001(4) O1 0.041(3) 0.021(3) 0.063(4) 0.008(3) -0.026(3) -0.018(3) O2 0.058(6) 0.024(5) 0.079(7) -0.003(4) -0.042(5) -0.001(4) O3 0.060(6) 0.026(5) 0.062(6) 0.003(4) -0.035(5) -0.017(4) O4 0.069(6) 0.023(5) 0.060(6) 0.011(4) -0.025(5) -0.023(4) O5 0.037(4) 0.020(4) 0.040(4) 0.000(3) -0.012(4) 0.002(3) O6 0.041(3) 0.021(3) 0.063(4) 0.008(3) -0.026(3) -0.018(3) O7 0.054(5) 0.036(5) 0.047(5) 0.004(4) -0.017(4) -0.020(4) O8 0.064(6) 0.049(6) 0.056(6) 0.007(4) -0.021(5) -0.035(5) O9 0.077(7) 0.032(5) 0.063(6) 0.003(4) -0.032(6) 0.003(5) O10 0.041(5) 0.033(5) 0.076(7) 0.018(4) -0.030(5) -0.008(4) O11 0.025(4) 0.049(5) 0.045(5) 0.000(4) -0.014(4) 0.003(4) O12 0.057(6) 0.038(5) 0.054(6) -0.013(4) -0.019(5) 0.000(5) O13 0.058(6) 0.029(5) 0.069(6) 0.006(4) -0.016(5) 0.005(5) O14 0.045(5) 0.027(5) 0.065(6) 0.011(4) -0.015(5) 0.011(4) O15 0.051(6) 0.033(5) 0.070(7) 0.002(4) -0.017(5) 0.006(4) O16 0.066(6) 0.038(5) 0.072(7) 0.006(5) -0.042(6) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N33 O19 1.221(18) . ? N33 O18 1.330(16) . ? N33 O17 1.374(17) . ? N33 Eu2 2.962(12) . ? O1W Eu1 2.443(13) . ? O2W Eu1 2.481(12) . ? O3W Eu1 2.404(13) . ? O4W Eu1 2.52(2) . ? O5W Eu1 2.311(13) . ? O6W Eu1 2.498(14) . ? O7W Eu1 2.70(2) . ? O8W Eu2 2.443(8) . ? O9W Eu2 2.386(10) . ? O10W Eu2 2.431(10) . ? O11W Eu2 2.416(9) . ? O12W Eu2 2.446(11) . ? O18 Eu2 2.650(15) . ? O19 Eu2 2.445(13) . ? Eu1 O2 2.424(9) . ? Eu1 O1 2.429(8) . ? Eu2 O5 2.383(7) . ? Eu2 O6 2.415(8) . ? Cl1 Cd1 2.426(3) . ? Cl2 Cd1 2.417(4) . ? Cl3 Cd1 2.458(4) . ? Cl4 Cd1 2.496(4) . ? C1 O1 1.222(14) . ? C1 N2 1.376(15) . ? C1 N1 1.396(14) . ? C2 N1 1.400(14) . ? C2 N3 1.473(15) . ? C2 C3 1.531(16) . ? C2 H2 0.9900 . ? C3 N2 1.448(15) . ? C3 N4 1.472(14) . ? C3 H3 0.9900 . ? C4 O5 1.221(13) . ? C4 N3 1.364(14) . ? C4 N4 1.367(16) . ? C5 N2 1.427(14) . ? C5 N5 1.467(14) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.445(14) . ? C6 N4 1.445(15) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.195(16) . ? C7 N6 1.348(14) . ? C7 N5 1.379(17) . ? C8 N5 1.415(14) . ? C8 N7 1.422(14) . ? C8 C9 1.564(15) . ? C8 H8 0.9900 . ? C9 N8 1.450(13) . ? C9 N6 1.462(15) . ? C9 H9 0.9900 . ? C10 O6 1.243(13) . ? C10 N8 1.346(14) . ? C10 N7 1.369(14) . ? C11 N9 1.425(15) . ? C11 N6 1.461(14) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.446(14) . ? C12 N8 1.465(13) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.223(15) . ? C13 N10 1.335(15) . ? C13 N9 1.379(16) . ? C14 N9 1.449(14) . ? C14 N11 1.459(15) . ? C14 C15 1.561(15) . ? C14 H14 0.9900 . ? C15 N10 1.430(16) . ? C15 N12 1.459(15) . ? C15 H15 0.9900 . ? C16 O7 1.243(15) . ? C16 N12 1.352(16) . ? C16 N11 1.361(16) . ? C17 N13 1.419(17) . ? C17 N10 1.478(15) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.454(14) . ? C18 N12 1.454(15) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.222(15) . ? C19 N13 1.363(16) . ? C19 N14 1.368(16) . ? C20 N15 1.436(14) . ? C20 N13 1.482(14) . ? C20 C21 1.563(15) . ? C20 H20 0.9900 . ? C21 N16 1.429(14) . ? C21 N14 1.474(13) . ? C21 H21 0.9900 . ? C22 O8 1.221(15) . ? C22 N15 1.358(16) . ? C22 N16 1.362(16) . ? C23 N14 1.413(15) . ? C23 N3 1.459(15) 2_665 ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.436(15) 2_665 ? C24 N1 1.448(13) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O9 1.287(15) . ? C25 N18 1.327(18) . ? C25 N17 1.342(17) . ? C26 N19 1.420(16) . ? C26 N17 1.476(16) . ? C26 C27 1.590(18) . ? C26 H26 0.9900 . ? C27 N20 1.436(17) . ? C27 N18 1.476(16) . ? C27 H27 0.9900 . ? C28 O13 1.220(16) . ? C28 N19 1.362(18) . ? C28 N20 1.373(17) . ? C29 N21 1.434(17) . ? C29 N18 1.447(17) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.416(15) . ? C30 N20 1.473(16) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O10 1.196(15) . ? C31 N22 1.341(16) . ? C31 N21 1.422(15) . ? C32 N23 1.447(16) . ? C32 N21 1.451(16) . ? C32 C33 1.550(17) . ? C32 H32 0.9900 . ? C33 N22 1.408(15) . ? C33 N24 1.480(15) . ? C33 H33 0.9900 . ? C34 O14 1.231(16) . ? C34 N24 1.327(16) . ? C34 N23 1.357(17) . ? C35 N22 1.443(14) . ? C35 N25 1.477(15) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N27 1.439(16) . ? C36 N24 1.460(17) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O11 1.218(14) . ? C37 N25 1.315(15) . ? C37 N26 1.397(16) . ? C38 N27 1.442(14) . ? C38 N25 1.467(13) . ? C38 C39 1.573(17) . ? C38 H38 0.9900 . ? C39 N28 1.467(15) . ? C39 N26 1.480(15) . ? C39 H39 0.9900 . ? C40 O15 1.228(15) . ? C40 N28 1.303(17) . ? C40 N27 1.396(16) . ? C41 N26 1.415(15) . ? C41 N29 1.426(15) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N31 1.435(16) . ? C42 N28 1.447(16) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O12 1.252(15) . ? C43 N30 1.336(15) . ? C43 N29 1.404(16) . ? C44 N31 1.434(16) . ? C44 N29 1.453(15) . ? C44 C45 1.552(16) . ? C44 H44 0.9900 . ? C45 N32 1.424(16) . ? C45 N30 1.437(15) . ? C45 H45 0.9900 . ? C46 O16 1.252(16) . ? C46 N31 1.336(17) . ? C46 N32 1.372(16) . ? C47 N19 1.428(17) 2 ? C47 N30 1.433(15) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N17 1.449(17) . ? C48 N32 1.469(17) 2 ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? N3 C23 1.459(15) 2_665 ? N16 C24 1.436(15) 2_665 ? N19 C47 1.428(17) 2 ? N32 C48 1.469(17) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O19 N33 O18 116.5(13) . . ? O19 N33 O17 129.8(12) . . ? O18 N33 O17 111.0(13) . . ? O19 N33 Eu2 53.7(7) . . ? O18 N33 Eu2 63.5(8) . . ? O17 N33 Eu2 170.9(9) . . ? N33 O18 Eu2 89.8(9) . . ? N33 O19 Eu2 102.6(8) . . ? O5W Eu1 O3W 80.8(6) . . ? O5W Eu1 O2 94.4(4) . . ? O3W Eu1 O2 136.4(4) . . ? O5W Eu1 O1 71.3(4) . . ? O3W Eu1 O1 137.2(5) . . ? O2 Eu1 O1 78.7(3) . . ? O5W Eu1 O1W 148.5(5) . . ? O3W Eu1 O1W 83.3(6) . . ? O2 Eu1 O1W 78.9(4) . . ? O1 Eu1 O1W 135.3(4) . . ? O5W Eu1 O2W 77.4(5) . . ? O3W Eu1 O2W 70.2(5) . . ? O2 Eu1 O2W 66.4(4) . . ? O1 Eu1 O2W 130.6(4) . . ? O1W Eu1 O2W 71.7(5) . . ? O5W Eu1 O6W 83.5(6) . . ? O3W Eu1 O6W 75.2(5) . . ? O2 Eu1 O6W 147.8(4) . . ? O1 Eu1 O6W 70.1(4) . . ? O1W Eu1 O6W 118.2(6) . . ? O2W Eu1 O6W 142.6(4) . . ? O5W Eu1 O4W 142.3(6) . . ? O3W Eu1 O4W 125.1(7) . . ? O2 Eu1 O4W 84.0(6) . . ? O1 Eu1 O4W 71.5(5) . . ? O1W Eu1 O4W 68.1(6) . . ? O2W Eu1 O4W 133.7(6) . . ? O6W Eu1 O4W 78.7(7) . . ? O5W Eu1 O7W 131.1(6) . . ? O3W Eu1 O7W 61.2(7) . . ? O2 Eu1 O7W 134.2(5) . . ? O1 Eu1 O7W 116.5(5) . . ? O1W Eu1 O7W 59.7(6) . . ? O2W Eu1 O7W 112.9(6) . . ? O6W Eu1 O7W 59.0(6) . . ? O4W Eu1 O7W 63.9(7) . . ? O5 Eu2 O9W 97.4(3) . . ? O5 Eu2 O6 79.5(3) . . ? O9W Eu2 O6 71.4(3) . . ? O5 Eu2 O11W 145.8(3) . . ? O9W Eu2 O11W 84.8(5) . . ? O6 Eu2 O11W 68.9(3) . . ? O5 Eu2 O10W 139.5(3) . . ? O9W Eu2 O10W 77.1(4) . . ? O6 Eu2 O10W 133.0(3) . . ? O11W Eu2 O10W 74.4(4) . . ? O5 Eu2 O8W 68.3(3) . . ? O9W Eu2 O8W 73.2(3) . . ? O6 Eu2 O8W 127.7(3) . . ? O11W Eu2 O8W 142.9(4) . . ? O10W Eu2 O8W 71.8(3) . . ? O5 Eu2 O19 81.1(4) . . ? O9W Eu2 O19 141.9(4) . . ? O6 Eu2 O19 143.6(4) . . ? O11W Eu2 O19 117.4(5) . . ? O10W Eu2 O19 79.8(5) . . ? O8W Eu2 O19 71.0(4) . . ? O5 Eu2 O12W 76.0(4) . . ? O9W Eu2 O12W 144.2(4) . . ? O6 Eu2 O12W 72.7(4) . . ? O11W Eu2 O12W 82.4(5) . . ? O10W Eu2 O12W 130.2(4) . . ? O8W Eu2 O12W 132.0(4) . . ? O19 Eu2 O12W 72.8(5) . . ? O5 Eu2 O18 124.4(4) . . ? O9W Eu2 O18 136.8(4) . . ? O6 Eu2 O18 122.3(4) . . ? O11W Eu2 O18 67.2(4) . . ? O10W Eu2 O18 64.4(5) . . ? O8W Eu2 O18 109.9(4) . . ? O19 Eu2 O18 50.2(4) . . ? O12W Eu2 O18 66.1(4) . . ? O5 Eu2 N33 102.9(3) . . ? O9W Eu2 N33 144.7(3) . . ? O6 Eu2 N33 140.4(3) . . ? O11W Eu2 N33 93.8(4) . . ? O10W Eu2 N33 68.7(4) . . ? O8W Eu2 N33 87.9(3) . . ? O19 Eu2 N33 23.7(4) . . ? O12W Eu2 N33 69.7(3) . . ? O18 Eu2 N33 26.7(3) . . ? Cl2 Cd1 Cl1 113.77(13) . . ? Cl2 Cd1 Cl3 117.45(16) . . ? Cl1 Cd1 Cl3 102.61(17) . . ? Cl2 Cd1 Cl4 110.42(15) . . ? Cl1 Cd1 Cl4 108.16(15) . . ? Cl3 Cd1 Cl4 103.53(16) . . ? O1 C1 N2 125.9(10) . . ? O1 C1 N1 126.3(11) . . ? N2 C1 N1 107.7(9) . . ? N1 C2 N3 113.2(9) . . ? N1 C2 C3 105.3(9) . . ? N3 C2 C3 104.3(8) . . ? N1 C2 H2 111.2 . . ? N3 C2 H2 111.2 . . ? C3 C2 H2 111.2 . . ? N2 C3 N4 112.8(8) . . ? N2 C3 C2 103.4(9) . . ? N4 C3 C2 103.2(9) . . ? N2 C3 H3 112.2 . . ? N4 C3 H3 112.2 . . ? C2 C3 H3 112.2 . . ? O5 C4 N3 125.7(12) . . ? O5 C4 N4 124.6(10) . . ? N3 C4 N4 109.7(10) . . ? N2 C5 N5 114.5(9) . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5B 108.6 . . ? N5 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 112.6(9) . . ? N7 C6 H6A 109.1 . . ? N4 C6 H6A 109.1 . . ? N7 C6 H6B 109.1 . . ? N4 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N6 126.2(12) . . ? O2 C7 N5 126.0(10) . . ? N6 C7 N5 107.8(11) . . ? N5 C8 N7 115.8(9) . . ? N5 C8 C9 103.3(8) . . ? N7 C8 C9 102.7(8) . . ? N5 C8 H8 111.5 . . ? N7 C8 H8 111.5 . . ? C9 C8 H8 111.5 . . ? N8 C9 N6 111.9(9) . . ? N8 C9 C8 103.2(9) . . ? N6 C9 C8 102.1(8) . . ? N8 C9 H9 112.9 . . ? N6 C9 H9 112.9 . . ? C8 C9 H9 112.9 . . ? O6 C10 N8 124.3(10) . . ? O6 C10 N7 126.7(10) . . ? N8 C10 N7 108.9(9) . . ? N9 C11 N6 113.6(10) . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11B 108.9 . . ? N6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 112.0(9) . . ? N11 C12 H12A 109.2 . . ? N8 C12 H12A 109.2 . . ? N11 C12 H12B 109.2 . . ? N8 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? O3 C13 N10 125.3(12) . . ? O3 C13 N9 126.7(11) . . ? N10 C13 N9 108.0(10) . . ? N9 C14 N11 113.5(8) . . ? N9 C14 C15 104.0(9) . . ? N11 C14 C15 102.8(9) . . ? N9 C14 H14 112.0 . . ? N11 C14 H14 112.0 . . ? C15 C14 H14 112.0 . . ? N10 C15 N12 113.6(10) . . ? N10 C15 C14 101.3(9) . . ? N12 C15 C14 103.1(9) . . ? N10 C15 H15 112.6 . . ? N12 C15 H15 112.6 . . ? C14 C15 H15 112.6 . . ? O7 C16 N12 126.4(11) . . ? O7 C16 N11 123.6(11) . . ? N12 C16 N11 109.9(10) . . ? N13 C17 N10 112.3(10) . . ? N13 C17 H17A 109.1 . . ? N10 C17 H17A 109.1 . . ? N13 C17 H17B 109.1 . . ? N10 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? N15 C18 N12 112.6(9) . . ? N15 C18 H18A 109.1 . . ? N12 C18 H18A 109.1 . . ? N15 C18 H18B 109.1 . . ? N12 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N13 123.1(12) . . ? O4 C19 N14 126.5(13) . . ? N13 C19 N14 110.3(10) . . ? N15 C20 N13 114.6(9) . . ? N15 C20 C21 103.5(9) . . ? N13 C20 C21 103.1(8) . . ? N15 C20 H20 111.7 . . ? N13 C20 H20 111.7 . . ? C21 C20 H20 111.7 . . ? N16 C21 N14 113.7(8) . . ? N16 C21 C20 102.3(9) . . ? N14 C21 C20 103.1(8) . . ? N16 C21 H21 112.3 . . ? N14 C21 H21 112.3 . . ? C20 C21 H21 112.3 . . ? O8 C22 N15 126.6(12) . . ? O8 C22 N16 124.9(12) . . ? N15 C22 N16 108.5(10) . . ? N14 C23 N3 113.6(9) . 2_665 ? N14 C23 H23A 108.8 . . ? N3 C23 H23A 108.8 2_665 . ? N14 C23 H23B 108.8 . . ? N3 C23 H23B 108.8 2_665 . ? H23A C23 H23B 107.7 . . ? N16 C24 N1 113.9(8) 2_665 . ? N16 C24 H24A 108.8 2_665 . ? N1 C24 H24A 108.8 . . ? N16 C24 H24B 108.8 2_665 . ? N1 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? O9 C25 N18 123.1(13) . . ? O9 C25 N17 124.2(13) . . ? N18 C25 N17 112.4(11) . . ? N19 C26 N17 114.4(10) . . ? N19 C26 C27 102.8(10) . . ? N17 C26 C27 101.9(9) . . ? N19 C26 H26 112.3 . . ? N17 C26 H26 112.3 . . ? C27 C26 H26 112.3 . . ? N20 C27 N18 113.9(10) . . ? N20 C27 C26 101.8(10) . . ? N18 C27 C26 102.7(9) . . ? N20 C27 H27 112.5 . . ? N18 C27 H27 112.5 . . ? C26 C27 H27 112.5 . . ? O13 C28 N19 128.5(13) . . ? O13 C28 N20 124.5(14) . . ? N19 C28 N20 107.0(11) . . ? N21 C29 N18 113.8(11) . . ? N21 C29 H29A 108.8 . . ? N18 C29 H29A 108.8 . . ? N21 C29 H29B 108.8 . . ? N18 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N23 C30 N20 113.5(9) . . ? N23 C30 H30A 108.9 . . ? N20 C30 H30A 108.9 . . ? N23 C30 H30B 108.9 . . ? N20 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? O10 C31 N22 129.4(11) . . ? O10 C31 N21 124.8(12) . . ? N22 C31 N21 105.7(10) . . ? N23 C32 N21 116.6(10) . . ? N23 C32 C33 106.8(10) . . ? N21 C32 C33 102.9(9) . . ? N23 C32 H32 110.0 . . ? N21 C32 H32 110.0 . . ? C33 C32 H32 110.0 . . ? N22 C33 N24 116.1(9) . . ? N22 C33 C32 103.2(10) . . ? N24 C33 C32 98.6(9) . . ? N22 C33 H33 112.6 . . ? N24 C33 H33 112.6 . . ? C32 C33 H33 112.6 . . ? O14 C34 N24 124.2(12) . . ? O14 C34 N23 126.1(12) . . ? N24 C34 N23 109.7(11) . . ? N22 C35 N25 114.0(9) . . ? N22 C35 H35A 108.7 . . ? N25 C35 H35A 108.7 . . ? N22 C35 H35B 108.7 . . ? N25 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N27 C36 N24 112.2(10) . . ? N27 C36 H36A 109.2 . . ? N24 C36 H36A 109.2 . . ? N27 C36 H36B 109.2 . . ? N24 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? O11 C37 N25 127.3(12) . . ? O11 C37 N26 123.4(11) . . ? N25 C37 N26 109.2(10) . . ? N27 C38 N25 115.2(10) . . ? N27 C38 C39 102.2(9) . . ? N25 C38 C39 102.0(8) . . ? N27 C38 H38 112.2 . . ? N25 C38 H38 112.2 . . ? C39 C38 H38 112.2 . . ? N28 C39 N26 112.9(10) . . ? N28 C39 C38 102.5(10) . . ? N26 C39 C38 103.1(9) . . ? N28 C39 H39 112.5 . . ? N26 C39 H39 112.5 . . ? C38 C39 H39 112.5 . . ? O15 C40 N28 127.3(13) . . ? O15 C40 N27 123.9(13) . . ? N28 C40 N27 108.8(10) . . ? N26 C41 N29 113.4(10) . . ? N26 C41 H41A 108.9 . . ? N29 C41 H41A 108.9 . . ? N26 C41 H41B 108.9 . . ? N29 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? N31 C42 N28 114.1(10) . . ? N31 C42 H42A 108.7 . . ? N28 C42 H42A 108.7 . . ? N31 C42 H42B 108.7 . . ? N28 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? O12 C43 N30 128.2(12) . . ? O12 C43 N29 121.9(10) . . ? N30 C43 N29 109.9(10) . . ? N31 C44 N29 115.6(10) . . ? N31 C44 C45 103.2(10) . . ? N29 C44 C45 103.6(9) . . ? N31 C44 H44 111.3 . . ? N29 C44 H44 111.3 . . ? C45 C44 H44 111.3 . . ? N32 C45 N30 114.3(10) . . ? N32 C45 C44 103.5(10) . . ? N30 C45 C44 104.0(9) . . ? N32 C45 H45 111.5 . . ? N30 C45 H45 111.5 . . ? C44 C45 H45 111.5 . . ? O16 C46 N31 125.7(11) . . ? O16 C46 N32 124.6(12) . . ? N31 C46 N32 109.6(11) . . ? N19 C47 N30 114.7(10) 2 . ? N19 C47 H47A 108.6 2 . ? N30 C47 H47A 108.6 . . ? N19 C47 H47B 108.6 2 . ? N30 C47 H47B 108.6 . . ? H47A C47 H47B 107.6 . . ? N17 C48 N32 111.5(11) . 2 ? N17 C48 H48A 109.3 . . ? N32 C48 H48A 109.3 2 . ? N17 C48 H48B 109.3 . . ? N32 C48 H48B 109.3 2 . ? H48A C48 H48B 108.0 . . ? C1 N1 C2 112.0(9) . . ? C1 N1 C24 119.8(9) . . ? C2 N1 C24 124.6(9) . . ? C1 N2 C5 123.9(10) . . ? C1 N2 C3 111.5(9) . . ? C5 N2 C3 124.5(9) . . ? C4 N3 C23 123.0(10) . 2_665 ? C4 N3 C2 111.1(10) . . ? C23 N3 C2 122.2(9) 2_665 . ? C4 N4 C6 122.0(10) . . ? C4 N4 C3 111.8(9) . . ? C6 N4 C3 125.8(10) . . ? C7 N5 C8 113.4(8) . . ? C7 N5 C5 122.9(10) . . ? C8 N5 C5 123.6(9) . . ? C7 N6 C11 121.0(10) . . ? C7 N6 C9 112.9(10) . . ? C11 N6 C9 122.5(9) . . ? C10 N7 C8 113.1(8) . . ? C10 N7 C6 120.2(10) . . ? C8 N7 C6 126.5(9) . . ? C10 N8 C9 112.1(9) . . ? C10 N8 C12 123.4(9) . . ? C9 N8 C12 122.9(9) . . ? C13 N9 C11 121.0(10) . . ? C13 N9 C14 110.8(9) . . ? C11 N9 C14 123.2(10) . . ? C13 N10 C15 115.2(10) . . ? C13 N10 C17 122.6(11) . . ? C15 N10 C17 119.4(9) . . ? C16 N11 C12 123.7(10) . . ? C16 N11 C14 111.8(9) . . ? C12 N11 C14 121.7(9) . . ? C16 N12 C18 120.2(10) . . ? C16 N12 C15 111.5(9) . . ? C18 N12 C15 122.2(10) . . ? C19 N13 C17 125.4(10) . . ? C19 N13 C20 111.3(9) . . ? C17 N13 C20 121.7(10) . . ? C19 N14 C23 119.7(10) . . ? C19 N14 C21 111.4(10) . . ? C23 N14 C21 122.1(9) . . ? C22 N15 C20 111.9(9) . . ? C22 N15 C18 120.0(10) . . ? C20 N15 C18 122.3(10) . . ? C22 N16 C21 113.1(10) . . ? C22 N16 C24 122.9(10) . 2_665 ? C21 N16 C24 121.7(9) . 2_665 ? C25 N17 C48 123.4(11) . . ? C25 N17 C26 111.3(10) . . ? C48 N17 C26 121.4(11) . . ? C25 N18 C29 124.4(11) . . ? C25 N18 C27 111.1(10) . . ? C29 N18 C27 118.7(11) . . ? C28 N19 C26 114.4(11) . . ? C28 N19 C47 121.4(10) . 2 ? C26 N19 C47 122.7(11) . 2 ? C28 N20 C27 114.0(11) . . ? C28 N20 C30 123.3(11) . . ? C27 N20 C30 120.0(11) . . ? C31 N21 C29 121.3(10) . . ? C31 N21 C32 111.6(10) . . ? C29 N21 C32 126.3(10) . . ? C31 N22 C33 116.0(10) . . ? C31 N22 C35 121.9(9) . . ? C33 N22 C35 118.9(10) . . ? C34 N23 C30 124.4(10) . . ? C34 N23 C32 109.7(10) . . ? C30 N23 C32 120.9(11) . . ? C34 N24 C36 123.6(10) . . ? C34 N24 C33 114.8(10) . . ? C36 N24 C33 119.6(10) . . ? C37 N25 C38 114.6(9) . . ? C37 N25 C35 123.8(9) . . ? C38 N25 C35 119.8(9) . . ? C37 N26 C41 124.5(10) . . ? C37 N26 C39 110.7(10) . . ? C41 N26 C39 121.4(10) . . ? C40 N27 C36 122.7(10) . . ? C40 N27 C38 112.3(10) . . ? C36 N27 C38 122.7(10) . . ? C40 N28 C42 122.2(9) . . ? C40 N28 C39 113.5(10) . . ? C42 N28 C39 119.9(10) . . ? C43 N29 C41 125.0(9) . . ? C43 N29 C44 109.9(9) . . ? C41 N29 C44 123.5(11) . . ? C43 N30 C47 120.2(10) . . ? C43 N30 C45 112.2(10) . . ? C47 N30 C45 123.1(11) . . ? C46 N31 C44 112.2(10) . . ? C46 N31 C42 122.1(10) . . ? C44 N31 C42 123.6(11) . . ? C46 N32 C45 111.4(10) . . ? C46 N32 C48 123.2(10) . 2 ? C45 N32 C48 123.5(11) . 2 ? C1 O1 Eu1 149.0(7) . . ? C7 O2 Eu1 161.0(9) . . ? C4 O5 Eu2 159.0(8) . . ? C10 O6 Eu2 154.5(7) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.314 _refine_diff_density_min -2.431 _refine_diff_density_rms 0.246 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.024 0.024 0.000 666 359 ' ' 2 0.000 0.021 0.500 448 269 ' ' 3 0.320 0.837 0.508 13 12 ' ' 4 0.370 0.087 0.464 20 13 ' ' 5 0.465 0.010 0.077 21 11 ' ' 6 0.539 -0.012 0.913 17 11 ' ' 7 0.630 0.913 0.536 22 14 ' ' 8 0.680 0.163 0.492 13 14 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952101' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H229 Cl4 Gd N64 O98' _chemical_formula_weight 4147.48 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' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 28.3249(19) _cell_length_b 28.3249(19) _cell_length_c 21.949(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17609(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8676 _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9058 _exptl_absorpt_correction_T_max 0.9409 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61360 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8607 _reflns_number_gt 5493 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1704P)^2^+21.5407P] 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 8607 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1250 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.2925 _refine_ls_wR_factor_gt 0.2683 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.5000 0.7500 -0.27958(17) 0.170(3) Uani 0.80 2 d SP . . Cl2 Cl 0.53477(14) 0.75255(17) -0.36872(14) 0.1132(14) Uani 0.60 1 d P . . Gd1 Gd 0.46009(5) 0.79039(5) 0.10064(7) 0.0488(5) Uani 0.1702(6) 1 d P . 1 Gd2 Gd 0.5000 0.7500 0.05173(9) 0.0391(7) Uani 0.1596(13) 2 d SP . 2 O1W O 0.4528(6) 0.7124(7) 0.0342(10) 0.219(10) Uani 0.50 1 d P . . O2W O 0.4942(4) 0.8387(12) 0.1096(11) 0.36(2) Uani 0.50 1 d P . . C1 C 0.36906(17) 0.87150(16) 0.1259(2) 0.0473(11) Uani 1 1 d . . . C2 C 0.30533(14) 0.92332(14) 0.13060(19) 0.0370(9) Uani 1 1 d . . . H2 H 0.2791 0.9199 0.1600 0.044 Uiso 1 1 calc R . . C3 C 0.29908(16) 0.89008(14) 0.07494(18) 0.0401(9) Uani 1 1 d . . . H3 H 0.2700 0.8708 0.0778 0.048 Uiso 1 1 calc R . . C4 C 0.30022(13) 0.96866(14) 0.04173(19) 0.0358(9) Uani 1 1 d . . . C5 C 0.3469(2) 0.81903(16) 0.0409(2) 0.0597(14) Uani 1 1 d . . . H5A H 0.3163 0.8031 0.0381 0.072 Uiso 1 1 calc R . . H5B H 0.3688 0.7975 0.0616 0.072 Uiso 1 1 calc R . . C6 C 0.28217(14) 0.90898(15) -0.03637(19) 0.0397(9) Uani 1 1 d . . . H6A H 0.2566 0.8858 -0.0326 0.048 Uiso 1 1 calc R . . H6B H 0.2693 0.9368 -0.0571 0.048 Uiso 1 1 calc R . . C7 C 0.40853(19) 0.81668(16) -0.0386(2) 0.0526(12) Uani 1 1 d . . . C8 C 0.33330(17) 0.84051(14) -0.07042(19) 0.0432(10) Uani 1 1 d . . . H8 H 0.3058 0.8190 -0.0726 0.052 Uiso 1 1 calc R . . C9 C 0.36619(14) 0.83467(15) -0.12635(19) 0.0406(9) Uani 1 1 d . . . H9 H 0.3549 0.8093 -0.1538 0.049 Uiso 1 1 calc R . . C10 C 0.33463(14) 0.91149(14) -0.12549(19) 0.0385(9) Uani 1 1 d . . . C11 C 0.44834(17) 0.80063(16) -0.1360(2) 0.0532(12) Uani 1 1 d . . . H11A H 0.4335 0.7792 -0.1654 0.064 Uiso 1 1 calc R . . H11B H 0.4684 0.7817 -0.1090 0.064 Uiso 1 1 calc R . . C12 C 0.38124(15) 0.88992(16) -0.21653(19) 0.0430(10) Uani 1 1 d . . . H12A H 0.3716 0.8640 -0.2434 0.052 Uiso 1 1 calc R . . H12B H 0.3663 0.9189 -0.2315 0.052 Uiso 1 1 calc R . . C13 C 0.52505(16) 0.83738(16) -0.1599(2) 0.0494(11) Uani 1 1 d . . . C14 C 0.46321(15) 0.85484(16) -0.2261(2) 0.0434(10) Uani 1 1 d . . . H14 H 0.4501 0.8306 -0.2538 0.052 Uiso 1 1 calc R . . C15 C 0.50880(15) 0.87702(16) -0.2519(2) 0.0435(10) Uani 1 1 d . . . H15 H 0.5167 0.8639 -0.2924 0.052 Uiso 1 1 calc R . . C16 C 0.45281(15) 0.93599(16) -0.23989(18) 0.0416(10) Uani 1 1 d . . . C17 C 0.59393(15) 0.86801(15) -0.2168(2) 0.0467(11) Uani 1 1 d . . . H17A H 0.6006 0.8581 -0.2587 0.056 Uiso 1 1 calc R . . H17B H 0.6103 0.8462 -0.1894 0.056 Uiso 1 1 calc R . . C18 C 0.52669(15) 0.96035(17) -0.2896(2) 0.0480(11) Uani 1 1 d . . . H18A H 0.5375 0.9453 -0.3273 0.058 Uiso 1 1 calc R . . H18B H 0.5068 0.9873 -0.3009 0.058 Uiso 1 1 calc R . . C19 C 0.64241(15) 0.92692(15) -0.1606(2) 0.0428(10) Uani 1 1 d . . . C20 C 0.61112(14) 0.95235(16) -0.25316(19) 0.0414(10) Uani 1 1 d . . . H20 H 0.6210 0.9403 -0.2935 0.050 Uiso 1 1 calc R . . C21 C 0.64605(14) 0.99005(15) -0.22868(19) 0.0396(9) Uani 1 1 d . . . H21 H 0.6730 0.9951 -0.2566 0.048 Uiso 1 1 calc R . . C22 C 0.57109(15) 1.02352(15) -0.24118(19) 0.0415(10) Uani 1 1 d . . . C23 C 0.29736(14) 1.01261(15) 0.1393(2) 0.0409(10) Uani 1 1 d . . . H23A H 0.2855 1.0374 0.1121 0.049 Uiso 1 1 calc R . . H23B H 0.2727 1.0060 0.1695 0.049 Uiso 1 1 calc R . . C24 C 0.36417(16) 0.92091(15) 0.2178(2) 0.0447(10) Uani 1 1 d . . . H24A H 0.3880 0.8983 0.2318 0.054 Uiso 1 1 calc R . . H24B H 0.3367 0.9180 0.2447 0.054 Uiso 1 1 calc R . . N1 N 0.35015(12) 0.90852(12) 0.15682(16) 0.0410(8) Uani 1 1 d . . . N2 N 0.34165(15) 0.86134(13) 0.07738(17) 0.0505(10) Uani 1 1 d . . . N3 N 0.30620(12) 0.96986(11) 0.10368(15) 0.0382(8) Uani 1 1 d . . . N4 N 0.29775(12) 0.92260(12) 0.02416(15) 0.0387(8) Uani 1 1 d . . . N5 N 0.36449(15) 0.82833(13) -0.02075(17) 0.0506(10) Uani 1 1 d . . . N6 N 0.41203(14) 0.82337(13) -0.10036(18) 0.0487(9) Uani 1 1 d . . . N7 N 0.31932(13) 0.88904(12) -0.07332(16) 0.0431(8) Uani 1 1 d . . . N8 N 0.36396(12) 0.88036(12) -0.15546(16) 0.0406(8) Uani 1 1 d . . . N9 N 0.47790(13) 0.83484(13) -0.16898(18) 0.0474(9) Uani 1 1 d . . . N10 N 0.54465(13) 0.86450(13) -0.20633(17) 0.0450(9) Uani 1 1 d . . . N11 N 0.43180(12) 0.89523(12) -0.22030(16) 0.0405(8) Uani 1 1 d . . . N12 N 0.49821(12) 0.92647(13) -0.25521(17) 0.0431(8) Uani 1 1 d . . . N13 N 0.61277(12) 0.91580(12) -0.20753(17) 0.0419(8) Uani 1 1 d . . . N14 N 0.66085(12) 0.97011(12) -0.17058(16) 0.0402(8) Uani 1 1 d . . . N15 N 0.56664(13) 0.97721(13) -0.25674(18) 0.0467(9) Uani 1 1 d . . . N16 N 0.61658(12) 1.03138(13) -0.22369(17) 0.0452(9) Uani 1 1 d . . . O1 O 0.40538(13) 0.85025(13) 0.14071(17) 0.0674(10) Uani 1 1 d . . . O2 O 0.44035(14) 0.80209(15) -0.00647(18) 0.0749(11) Uani 1 1 d . . . O3 O 0.54706(12) 0.81969(12) -0.11799(17) 0.0610(9) Uani 1 1 d . . . O4 O 0.65067(13) 0.90128(11) -0.11639(15) 0.0571(9) Uani 1 1 d . . . O5 O 0.29625(12) 1.00328(10) 0.00890(14) 0.0499(8) Uani 1 1 d . . . O6 O 0.32357(11) 0.95046(11) -0.14298(14) 0.0489(8) Uani 1 1 d . . . O7 O 0.43352(11) 0.97473(11) -0.24324(15) 0.0522(8) Uani 1 1 d . . . O8 O 0.54024(11) 1.05332(12) -0.24404(17) 0.0577(9) 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 Cl1 0.340(8) 0.089(2) 0.081(2) 0.000 0.000 0.127(4) Cl2 0.161(3) 0.118(2) 0.0602(16) -0.0145(17) 0.065(2) -0.022(3) Gd1 0.0443(8) 0.0505(8) 0.0516(8) -0.0011(6) -0.0081(6) 0.0016(6) Gd2 0.0322(10) 0.0304(10) 0.0545(13) 0.000 0.000 -0.0004(7) O1W 0.157(14) 0.232(18) 0.27(2) 0.178(17) 0.017(13) -0.055(12) O2W 0.038(6) 0.71(5) 0.34(3) -0.39(3) 0.030(10) -0.057(14) C1 0.052(3) 0.042(2) 0.047(3) 0.011(2) 0.012(2) 0.007(2) C2 0.034(2) 0.038(2) 0.039(2) 0.0062(17) 0.0046(17) -0.0019(16) C3 0.049(2) 0.036(2) 0.035(2) 0.0075(17) 0.0056(18) 0.0041(18) C4 0.0281(19) 0.036(2) 0.043(2) 0.0033(18) 0.0024(16) 0.0009(16) C5 0.102(4) 0.034(2) 0.043(3) 0.0022(19) 0.014(3) 0.016(2) C6 0.038(2) 0.042(2) 0.039(2) 0.0025(18) 0.0004(17) 0.0005(18) C7 0.067(3) 0.040(2) 0.051(3) 0.007(2) -0.010(2) -0.001(2) C8 0.057(3) 0.033(2) 0.040(2) 0.0043(18) 0.008(2) -0.0024(19) C9 0.037(2) 0.044(2) 0.042(2) -0.0030(19) 0.0021(18) 0.0030(18) C10 0.038(2) 0.038(2) 0.039(2) 0.0012(18) 0.0004(18) -0.0077(18) C11 0.048(3) 0.043(3) 0.068(3) 0.014(2) 0.009(2) 0.009(2) C12 0.041(2) 0.051(3) 0.038(2) 0.0024(19) -0.0014(18) -0.0006(19) C13 0.045(3) 0.038(2) 0.065(3) 0.001(2) 0.003(2) 0.005(2) C14 0.038(2) 0.047(2) 0.045(2) -0.001(2) -0.0010(19) 0.0057(18) C15 0.039(2) 0.050(3) 0.042(2) -0.0109(19) 0.0005(18) 0.0028(19) C16 0.042(2) 0.051(3) 0.032(2) 0.0010(18) -0.0065(17) 0.002(2) C17 0.042(2) 0.038(2) 0.061(3) -0.002(2) -0.002(2) 0.0081(18) C18 0.040(2) 0.058(3) 0.046(2) 0.016(2) -0.0059(19) -0.005(2) C19 0.043(2) 0.042(2) 0.043(2) 0.0010(19) 0.0068(19) 0.0130(19) C20 0.034(2) 0.051(3) 0.039(2) -0.0016(19) 0.0039(17) 0.0012(18) C21 0.033(2) 0.046(2) 0.040(2) 0.0063(18) 0.0036(17) 0.0019(17) C22 0.039(2) 0.044(2) 0.042(2) 0.0128(19) 0.0021(18) 0.0063(19) C23 0.035(2) 0.038(2) 0.049(2) -0.0045(18) -0.0049(18) 0.0069(17) C24 0.046(2) 0.037(2) 0.051(3) 0.0085(19) -0.008(2) 0.0031(19) N1 0.0411(19) 0.0400(19) 0.042(2) 0.0066(15) -0.0003(15) 0.0070(15) N2 0.070(3) 0.041(2) 0.041(2) 0.0001(16) 0.0017(19) 0.0211(18) N3 0.0395(19) 0.0343(18) 0.0406(19) 0.0038(15) -0.0024(15) -0.0004(14) N4 0.0423(19) 0.0387(19) 0.0353(18) 0.0080(14) 0.0037(15) 0.0053(15) N5 0.073(3) 0.041(2) 0.038(2) 0.0006(16) 0.0043(18) 0.0126(19) N6 0.050(2) 0.046(2) 0.050(2) 0.0085(17) 0.0019(17) 0.0012(17) N7 0.052(2) 0.0346(18) 0.043(2) 0.0030(15) 0.0076(17) 0.0017(15) N8 0.0420(19) 0.0392(19) 0.0405(19) 0.0035(15) 0.0067(15) 0.0042(15) N9 0.042(2) 0.043(2) 0.057(2) 0.0113(17) 0.0000(17) 0.0039(16) N10 0.043(2) 0.043(2) 0.049(2) 0.0052(17) -0.0018(16) 0.0023(16) N11 0.0369(18) 0.0398(19) 0.045(2) 0.0005(15) 0.0032(15) 0.0040(15) N12 0.0364(19) 0.042(2) 0.051(2) 0.0069(16) 0.0031(16) 0.0019(15) N13 0.0372(19) 0.0389(19) 0.050(2) 0.0027(16) -0.0052(16) 0.0014(15) N14 0.0398(19) 0.0358(19) 0.045(2) 0.0047(15) -0.0035(15) 0.0014(15) N15 0.040(2) 0.044(2) 0.056(2) 0.0037(18) -0.0041(17) 0.0009(16) N16 0.039(2) 0.043(2) 0.054(2) 0.0039(17) -0.0046(16) 0.0004(16) O1 0.069(2) 0.066(2) 0.067(2) 0.0111(18) 0.0013(18) 0.0324(19) O2 0.075(3) 0.079(3) 0.071(3) 0.023(2) -0.018(2) 0.011(2) O3 0.053(2) 0.058(2) 0.073(2) 0.0200(18) -0.0116(17) 0.0114(16) O4 0.068(2) 0.0497(19) 0.054(2) 0.0114(16) -0.0086(16) -0.0004(16) O5 0.065(2) 0.0369(16) 0.0480(18) 0.0089(14) -0.0054(15) 0.0036(14) O6 0.0547(19) 0.0444(18) 0.0477(18) 0.0096(14) 0.0054(14) 0.0054(14) O7 0.0496(18) 0.0434(18) 0.063(2) 0.0089(15) 0.0001(15) 0.0128(14) O8 0.0439(18) 0.053(2) 0.076(2) 0.0129(17) 0.0014(16) 0.0064(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Cl2 2.192(4) 6_564 ? Cl1 Cl2 2.192(4) . ? Cl1 Cl2 2.441(5) 15_564 ? Cl1 Cl2 2.441(5) 12_765 ? Cl2 Cl2 1.424(6) 15_564 ? Cl2 Cl2 1.424(6) 12_765 ? Cl2 Cl2 1.975(8) 6_564 ? Cl2 Cl1 2.441(5) 15_564 ? Gd1 O2W 1.69(2) . ? Gd1 O2W 2.09(3) 12_766 ? Gd1 O2 2.439(4) . ? Gd1 O1 2.460(4) . ? Gd1 Gd1 2.513(2) 15_565 ? Gd1 Gd1 2.513(2) 12_766 ? Gd1 O1W 2.54(2) 15_565 ? Gd1 O1W 2.66(3) . ? Gd1 O1W 2.866(18) 6_564 ? Gd1 Gd1 3.217(3) 6_564 ? Gd2 O1W 1.752(18) . ? Gd2 O1W 1.752(18) 6_564 ? Gd2 O2 2.581(4) . ? Gd2 O2 2.581(4) 6_564 ? Gd2 O2W 2.82(2) . ? Gd2 O2W 2.82(2) 6_564 ? Gd2 Gd2 3.216(4) 15_565 ? O1W Gd1 2.54(2) 12_766 ? O1W Gd1 2.866(18) 6_564 ? O2W Gd1 2.09(3) 15_565 ? C1 O1 1.236(6) . ? C1 N2 1.349(6) . ? C1 N1 1.359(6) . ? C2 N3 1.445(5) . ? C2 N1 1.456(5) . ? C2 C3 1.552(6) . ? C2 H2 0.9900 . ? C3 N4 1.446(5) . ? C3 N2 1.456(6) . ? C3 H3 0.9900 . ? C4 O5 1.222(5) . ? C4 N4 1.362(5) . ? C4 N3 1.371(5) . ? C5 N2 1.449(6) . ? C5 N5 1.466(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.444(5) . ? C6 N4 1.452(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.217(6) . ? C7 N5 1.348(7) . ? C7 N6 1.372(6) . ? C8 N7 1.432(5) . ? C8 N5 1.445(6) . ? C8 C9 1.550(6) . ? C8 H8 0.9900 . ? C9 N8 1.445(5) . ? C9 N6 1.454(6) . ? C9 H9 0.9900 . ? C10 O6 1.210(5) . ? C10 N8 1.379(5) . ? C10 N7 1.380(5) . ? C11 N6 1.444(6) . ? C11 N9 1.471(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.442(5) . ? C12 N8 1.452(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.219(6) . ? C13 N9 1.352(6) . ? C13 N10 1.391(6) . ? C14 N9 1.437(6) . ? C14 N11 1.455(5) . ? C14 C15 1.544(6) . ? C14 H14 0.9900 . ? C15 N12 1.434(6) . ? C15 N10 1.468(6) . ? C15 H15 0.9900 . ? C16 O7 1.228(5) . ? C16 N12 1.356(6) . ? C16 N11 1.368(6) . ? C17 N10 1.418(6) . ? C17 N13 1.469(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.425(6) . ? C18 N12 1.463(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.234(5) . ? C19 N14 1.348(6) . ? C19 N13 1.366(6) . ? C20 N13 1.441(6) . ? C20 N15 1.445(5) . ? C20 C21 1.552(6) . ? C20 H20 0.9900 . ? C21 N16 1.442(6) . ? C21 N14 1.456(5) . ? C21 H21 0.9900 . ? C22 O8 1.217(5) . ? C22 N15 1.361(6) . ? C22 N16 1.363(6) . ? C23 N14 1.453(5) 9_675 ? C23 N3 1.463(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N1 1.440(6) . ? C24 N16 1.463(6) 9_675 ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? N14 C23 1.453(5) 9_675 ? N16 C24 1.463(6) 9_675 ? 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 Cl2 Cl1 Cl2 53.6(2) 6_564 . ? Cl2 Cl1 Cl2 35.28(13) 6_564 15_564 ? Cl2 Cl1 Cl2 35.28(13) . 15_564 ? Cl2 Cl1 Cl2 35.28(13) 6_564 12_765 ? Cl2 Cl1 Cl2 35.28(13) . 12_765 ? Cl2 Cl1 Cl2 47.73(16) 15_564 12_765 ? Cl2 Cl2 Cl2 87.85(9) 15_564 12_765 ? Cl2 Cl2 Cl2 46.08(4) 15_564 6_564 ? Cl2 Cl2 Cl2 46.08(4) 12_765 6_564 ? Cl2 Cl2 Cl1 81.97(18) 15_564 . ? Cl2 Cl2 Cl1 81.97(18) 12_765 . ? Cl2 Cl2 Cl1 63.22(12) 6_564 . ? Cl2 Cl2 Cl1 62.8(2) 15_564 15_564 ? Cl2 Cl2 Cl1 62.8(2) 12_765 15_564 ? Cl2 Cl2 Cl1 66.13(8) 6_564 15_564 ? Cl1 Cl2 Cl1 129.35(19) . 15_564 ? O2W Gd1 O2W 146.77(19) . 12_766 ? O2W Gd1 O2 97.6(10) . . ? O2W Gd1 O2 109.6(4) 12_766 . ? O2W Gd1 O1 76.1(6) . . ? O2W Gd1 O1 82.2(6) 12_766 . ? O2 Gd1 O1 96.12(14) . . ? O2W Gd1 Gd1 55.7(10) . 15_565 ? O2W Gd1 Gd1 114.6(4) 12_766 15_565 ? O2 Gd1 Gd1 128.19(13) . 15_565 ? O1 Gd1 Gd1 114.94(12) . 15_565 ? O2W Gd1 Gd1 133.5(11) . 12_766 ? O2W Gd1 Gd1 41.7(6) 12_766 12_766 ? O2 Gd1 Gd1 122.13(13) . 12_766 ? O1 Gd1 Gd1 117.92(12) . 12_766 ? Gd1 Gd1 Gd1 79.57(5) 15_565 12_766 ? O2W Gd1 O1W 78.9(10) . 15_565 ? O2W Gd1 O1W 69.4(6) 12_766 15_565 ? O2 Gd1 O1W 163.0(4) . 15_565 ? O1 Gd1 O1W 66.9(4) . 15_565 ? Gd1 Gd1 O1W 63.5(5) 15_565 15_565 ? Gd1 Gd1 O1W 69.2(4) 12_766 15_565 ? O2W Gd1 O1W 141.6(6) . . ? O2W Gd1 O1W 70.0(6) 12_766 . ? O2 Gd1 O1W 64.3(3) . . ? O1 Gd1 O1W 136.2(4) . . ? Gd1 Gd1 O1W 107.4(4) 15_565 . ? Gd1 Gd1 O1W 58.7(3) 12_766 . ? O1W Gd1 O1W 127.7(5) 15_565 . ? O2W Gd1 O1W 65.7(5) . 6_564 ? O2W Gd1 O1W 139.8(7) 12_766 6_564 ? O2 Gd1 O1W 73.2(4) . 6_564 ? O1 Gd1 O1W 138.0(4) . 6_564 ? Gd1 Gd1 O1W 55.8(4) 15_565 6_564 ? Gd1 Gd1 O1W 101.3(5) 12_766 6_564 ? O1W Gd1 O1W 119.2(8) 15_565 6_564 ? O1W Gd1 O1W 76.4(4) . 6_564 ? O2W Gd1 Gd1 100.0(8) . 6_564 ? O2W Gd1 Gd1 91.2(6) 12_766 6_564 ? O2 Gd1 Gd1 104.94(10) . 6_564 ? O1 Gd1 Gd1 158.93(9) . 6_564 ? Gd1 Gd1 Gd1 50.22(2) 15_565 6_564 ? Gd1 Gd1 Gd1 50.22(2) 12_766 6_564 ? O1W Gd1 Gd1 92.1(4) 15_565 6_564 ? O1W Gd1 Gd1 57.5(4) . 6_564 ? O1W Gd1 Gd1 51.4(5) 6_564 6_564 ? O1W Gd2 O1W 154.7(12) . 6_564 ? O1W Gd2 O2 74.9(5) . . ? O1W Gd2 O2 92.5(8) 6_564 . ? O1W Gd2 O2 92.5(8) . 6_564 ? O1W Gd2 O2 74.9(5) 6_564 6_564 ? O2 Gd2 O2 120.7(2) . 6_564 ? O1W Gd2 O2W 126.6(8) . . ? O1W Gd2 O2W 66.5(6) 6_564 . ? O2 Gd2 O2W 71.1(6) . . ? O2 Gd2 O2W 140.3(3) 6_564 . ? O1W Gd2 O2W 66.5(6) . 6_564 ? O1W Gd2 O2W 126.6(8) 6_564 6_564 ? O2 Gd2 O2W 140.3(3) . 6_564 ? O2 Gd2 O2W 71.1(6) 6_564 6_564 ? O2W Gd2 O2W 126.5(14) . 6_564 ? O1W Gd2 Gd2 102.7(6) . 15_565 ? O1W Gd2 Gd2 102.7(6) 6_564 15_565 ? O2 Gd2 Gd2 119.66(10) . 15_565 ? O2 Gd2 Gd2 119.66(10) 6_564 15_565 ? O2W Gd2 Gd2 63.3(7) . 15_565 ? O2W Gd2 Gd2 63.3(7) 6_564 15_565 ? Gd2 O1W Gd1 74.9(8) . 12_766 ? Gd2 O1W Gd1 46.7(6) . . ? Gd1 O1W Gd1 57.9(5) 12_766 . ? Gd2 O1W Gd1 41.3(4) . 6_564 ? Gd1 O1W Gd1 55.1(4) 12_766 6_564 ? Gd1 O1W Gd1 71.2(5) . 6_564 ? Gd1 O2W Gd1 82.6(15) . 15_565 ? Gd1 O2W Gd2 42.1(5) . . ? Gd1 O2W Gd2 64.1(8) 15_565 . ? O1 C1 N2 125.7(4) . . ? O1 C1 N1 124.9(5) . . ? N2 C1 N1 109.4(4) . . ? N3 C2 N1 114.2(3) . . ? N3 C2 C3 103.5(3) . . ? N1 C2 C3 103.7(3) . . ? N3 C2 H2 111.6 . . ? N1 C2 H2 111.6 . . ? C3 C2 H2 111.6 . . ? N4 C3 N2 113.9(3) . . ? N4 C3 C2 102.9(3) . . ? N2 C3 C2 102.5(3) . . ? N4 C3 H3 112.3 . . ? N2 C3 H3 112.3 . . ? C2 C3 H3 112.3 . . ? O5 C4 N4 126.6(4) . . ? O5 C4 N3 125.2(4) . . ? N4 C4 N3 108.1(3) . . ? N2 C5 N5 113.4(4) . . ? N2 C5 H5A 108.9 . . ? N5 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? N5 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 113.3(3) . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6B 108.9 . . ? N4 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N5 126.9(5) . . ? O2 C7 N6 124.5(5) . . ? N5 C7 N6 108.7(4) . . ? N7 C8 N5 115.6(4) . . ? N7 C8 C9 103.5(3) . . ? N5 C8 C9 101.8(4) . . ? N7 C8 H8 111.7 . . ? N5 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N8 C9 N6 114.2(4) . . ? N8 C9 C8 103.2(3) . . ? N6 C9 C8 104.4(3) . . ? N8 C9 H9 111.5 . . ? N6 C9 H9 111.5 . . ? C8 C9 H9 111.5 . . ? O6 C10 N8 126.0(4) . . ? O6 C10 N7 127.0(4) . . ? N8 C10 N7 106.9(3) . . ? N6 C11 N9 112.2(4) . . ? N6 C11 H11A 109.2 . . ? N9 C11 H11A 109.2 . . ? N6 C11 H11B 109.2 . . ? N9 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N11 C12 N8 114.0(3) . . ? N11 C12 H12A 108.7 . . ? N8 C12 H12A 108.7 . . ? N11 C12 H12B 108.7 . . ? N8 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N9 126.5(4) . . ? O3 C13 N10 125.1(4) . . ? N9 C13 N10 108.4(4) . . ? N9 C14 N11 114.3(4) . . ? N9 C14 C15 103.8(3) . . ? N11 C14 C15 102.9(3) . . ? N9 C14 H14 111.7 . . ? N11 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N12 C15 N10 114.5(4) . . ? N12 C15 C14 104.0(3) . . ? N10 C15 C14 103.3(3) . . ? N12 C15 H15 111.5 . . ? N10 C15 H15 111.5 . . ? C14 C15 H15 111.5 . . ? O7 C16 N12 125.8(4) . . ? O7 C16 N11 125.4(4) . . ? N12 C16 N11 108.8(4) . . ? N10 C17 N13 113.6(3) . . ? N10 C17 H17A 108.9 . . ? N13 C17 H17A 108.9 . . ? N10 C17 H17B 108.9 . . ? N13 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N15 C18 N12 113.3(4) . . ? N15 C18 H18A 108.9 . . ? N12 C18 H18A 108.9 . . ? N15 C18 H18B 108.9 . . ? N12 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N14 126.0(4) . . ? O4 C19 N13 125.0(4) . . ? N14 C19 N13 109.0(4) . . ? N13 C20 N15 114.6(3) . . ? N13 C20 C21 103.5(3) . . ? N15 C20 C21 103.9(3) . . ? N13 C20 H20 111.5 . . ? N15 C20 H20 111.5 . . ? C21 C20 H20 111.5 . . ? N16 C21 N14 114.5(3) . . ? N16 C21 C20 102.5(3) . . ? N14 C21 C20 102.7(3) . . ? N16 C21 H21 112.1 . . ? N14 C21 H21 112.1 . . ? C20 C21 H21 112.1 . . ? O8 C22 N15 126.1(4) . . ? O8 C22 N16 125.5(4) . . ? N15 C22 N16 108.4(4) . . ? N14 C23 N3 113.1(3) 9_675 . ? N14 C23 H23A 109.0 9_675 . ? N3 C23 H23A 109.0 . . ? N14 C23 H23B 109.0 9_675 . ? N3 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N1 C24 N16 114.2(4) . 9_675 ? N1 C24 H24A 108.7 . . ? N16 C24 H24A 108.7 9_675 . ? N1 C24 H24B 108.7 . . ? N16 C24 H24B 108.7 9_675 . ? H24A C24 H24B 107.6 . . ? C1 N1 C24 122.9(4) . . ? C1 N1 C2 111.6(4) . . ? C24 N1 C2 122.6(3) . . ? C1 N2 C5 123.6(4) . . ? C1 N2 C3 112.7(4) . . ? C5 N2 C3 121.9(4) . . ? C4 N3 C2 112.4(3) . . ? C4 N3 C23 122.0(3) . . ? C2 N3 C23 122.2(3) . . ? C4 N4 C3 113.0(3) . . ? C4 N4 C6 121.9(3) . . ? C3 N4 C6 122.9(3) . . ? C7 N5 C8 113.9(4) . . ? C7 N5 C5 122.5(4) . . ? C8 N5 C5 122.2(4) . . ? C7 N6 C11 121.7(4) . . ? C7 N6 C9 110.7(4) . . ? C11 N6 C9 121.5(4) . . ? C10 N7 C8 113.1(3) . . ? C10 N7 C6 121.0(3) . . ? C8 N7 C6 123.5(3) . . ? C10 N8 C9 112.9(3) . . ? C10 N8 C12 121.6(3) . . ? C9 N8 C12 124.1(3) . . ? C13 N9 C14 113.2(4) . . ? C13 N9 C11 121.7(4) . . ? C14 N9 C11 121.6(4) . . ? C13 N10 C17 123.4(4) . . ? C13 N10 C15 110.8(4) . . ? C17 N10 C15 123.6(4) . . ? C16 N11 C12 122.5(4) . . ? C16 N11 C14 111.7(3) . . ? C12 N11 C14 122.0(4) . . ? C16 N12 C15 112.3(3) . . ? C16 N12 C18 121.3(4) . . ? C15 N12 C18 123.5(4) . . ? C19 N13 C20 112.2(3) . . ? C19 N13 C17 122.7(4) . . ? C20 N13 C17 123.6(4) . . ? C19 N14 C23 123.0(4) . 9_675 ? C19 N14 C21 112.5(3) . . ? C23 N14 C21 121.1(3) 9_675 . ? C22 N15 C18 121.6(4) . . ? C22 N15 C20 112.0(3) . . ? C18 N15 C20 123.8(4) . . ? C22 N16 C21 113.2(4) . . ? C22 N16 C24 121.9(4) . 9_675 ? C21 N16 C24 122.7(3) . 9_675 ? C1 O1 Gd1 140.0(3) . . ? C7 O2 Gd1 140.8(4) . . ? C7 O2 Gd2 165.0(4) . . ? Gd1 O2 Gd2 45.20(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.917 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.084 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.008 -0.003 -0.002 4410 1653 ' ' 2 0.000 0.000 0.500 358 104 ' ' 3 0.000 0.500 0.500 358 104 ' ' 4 0.250 0.250 0.750 358 105 ' ' 5 0.250 0.750 0.250 358 105 ' ' 6 0.500 0.500 0.000 358 104 ' ' 7 0.500 1.000 1.000 358 104 ' ' 8 0.750 0.250 0.750 358 105 ' ' 9 0.750 0.750 0.250 358 105 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952102' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H235 Cl4 N64 O101 Tb' _chemical_formula_weight 4203.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 28.3123(19) _cell_length_b 28.3123(19) _cell_length_c 21.934(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17582(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8800 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8863 _exptl_absorpt_correction_T_max 0.9273 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57536 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 24.99 _reflns_number_total 7734 _reflns_number_gt 4921 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1538P)^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 7734 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1109 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2506 _refine_ls_wR_factor_gt 0.2312 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 1.0000 1.2500 -0.27927(15) 0.162(2) Uani 0.80 2 d SP . . Cl2 Cl 0.99648(14) 1.21522(11) -0.38105(12) 0.1054(12) Uani 0.60 1 d P . . Tb1 Tb 0.95977(4) 1.20967(4) 0.10094(6) 0.0510(4) Uani 0.1880(6) 1 d P . 1 Tb2 Tb 1.0000 1.2500 0.05227(11) 0.0443(9) Uani 0.1240(12) 2 d SP . 2 O1W O 0.9524(5) 1.2835(6) 0.0386(9) 0.211(8) Uani 0.50 1 d P . . O2W O 0.9943(5) 1.1449(5) 0.0983(8) 0.189(6) Uani 0.50 1 d P . . C1 C 1.02548(15) 1.16244(14) -0.1596(2) 0.0482(10) Uani 1 1 d . . . C2 C 1.00884(13) 1.12339(14) -0.25205(19) 0.0440(10) Uani 1 1 d . . . H2 H 1.0167 1.1366 -0.2926 0.053 Uiso 1 1 calc R . . C3 C 0.96316(13) 1.14542(15) -0.22593(18) 0.0428(9) Uani 1 1 d . . . H3 H 0.9498 1.1697 -0.2534 0.051 Uiso 1 1 calc R . . C4 C 0.95265(14) 1.06403(14) -0.23991(17) 0.0416(9) Uani 1 1 d . . . C5 C 0.94856(16) 1.19905(15) -0.1348(2) 0.0531(11) Uani 1 1 d . . . H5A H 0.9686 1.2177 -0.1075 0.064 Uiso 1 1 calc R . . H5B H 0.9339 1.2208 -0.1639 0.064 Uiso 1 1 calc R . . C6 C 0.88120(13) 1.11017(15) -0.21653(17) 0.0404(9) Uani 1 1 d . . . H6A H 0.8716 1.1361 -0.2433 0.048 Uiso 1 1 calc R . . H6B H 0.8664 1.0812 -0.2318 0.048 Uiso 1 1 calc R . . C7 C 0.90838(17) 1.18323(15) -0.0387(2) 0.0530(11) Uani 1 1 d . . . C8 C 0.86578(14) 1.16532(13) -0.12600(18) 0.0405(9) Uani 1 1 d . . . H8 H 0.8548 1.1908 -0.1535 0.049 Uiso 1 1 calc R . . C9 C 0.83347(15) 1.15995(13) -0.07087(17) 0.0436(9) Uani 1 1 d . . . H9 H 0.8060 1.1816 -0.0730 0.052 Uiso 1 1 calc R . . C10 C 0.83444(13) 1.08880(14) -0.12565(17) 0.0378(9) Uani 1 1 d . . . C11 C 0.8461(2) 1.18146(14) 0.04135(19) 0.0573(12) Uani 1 1 d . . . H11A H 0.8675 1.2033 0.0622 0.069 Uiso 1 1 calc R . . H11B H 0.8152 1.1969 0.0378 0.069 Uiso 1 1 calc R . . C12 C 0.78222(13) 1.09119(13) -0.03589(17) 0.0391(9) Uani 1 1 d . . . H12A H 0.7693 1.0634 -0.0566 0.047 Uiso 1 1 calc R . . H12B H 0.7567 1.1144 -0.0319 0.047 Uiso 1 1 calc R . . C13 C 0.86863(15) 1.12870(14) 0.1260(2) 0.0478(11) Uani 1 1 d . . . C14 C 0.79863(14) 1.10993(13) 0.07509(16) 0.0385(9) Uani 1 1 d . . . H14 H 0.7695 1.1292 0.0777 0.046 Uiso 1 1 calc R . . C15 C 0.80489(13) 1.07688(13) 0.13101(19) 0.0395(9) Uani 1 1 d . . . H15 H 0.7786 1.0803 0.1605 0.047 Uiso 1 1 calc R . . C16 C 0.79985(12) 1.03085(13) 0.04207(18) 0.0363(9) Uani 1 1 d . . . C17 C 0.86419(15) 1.07908(13) 0.21808(19) 0.0453(10) Uani 1 1 d . . . H17A H 0.8368 1.0820 0.2451 0.054 Uiso 1 1 calc R . . H17B H 0.8881 1.1017 0.2320 0.054 Uiso 1 1 calc R . . C18 C 0.79743(14) 0.98752(14) 0.13889(19) 0.0447(10) Uani 1 1 d . . . H18A H 0.7725 0.9938 0.1688 0.054 Uiso 1 1 calc R . . H18B H 0.7860 0.9628 0.1114 0.054 Uiso 1 1 calc R . . C19 C 0.92854(14) 1.02329(14) 0.24130(18) 0.0419(9) Uani 1 1 d . . . C20 C 0.85382(14) 0.98973(14) 0.22897(18) 0.0419(9) Uani 1 1 d . . . H20 H 0.8268 0.9950 0.2569 0.050 Uiso 1 1 calc R . . C21 C 0.88814(13) 0.95224(14) 0.25353(19) 0.0426(9) Uani 1 1 d . . . H21 H 0.8782 0.9403 0.2940 0.051 Uiso 1 1 calc R . . C22 C 0.85754(13) 0.92637(14) 0.16044(19) 0.0428(9) Uani 1 1 d . . . C23 C 1.02670(14) 1.04022(16) -0.2897(2) 0.0515(11) Uani 1 1 d . . . H23A H 1.0068 1.0134 -0.3014 0.062 Uiso 1 1 calc R . . H23B H 1.0377 1.0554 -0.3272 0.062 Uiso 1 1 calc R . . C24 C 1.09430(13) 1.13188(14) -0.2170(2) 0.0460(10) Uani 1 1 d . . . H24A H 1.1108 1.1538 -0.1898 0.055 Uiso 1 1 calc R . . H24B H 1.1010 1.1416 -0.2590 0.055 Uiso 1 1 calc R . . N1 N 1.04457(11) 1.13578(11) -0.20634(16) 0.0450(8) Uani 1 1 d . . . N2 N 0.97820(11) 1.16532(12) -0.16831(16) 0.0468(8) Uani 1 1 d . . . N3 N 0.99809(11) 1.07382(11) -0.25567(15) 0.0425(8) Uani 1 1 d . . . N4 N 0.93231(11) 1.10487(11) -0.21993(15) 0.0406(8) Uani 1 1 d . . . N5 N 0.91207(12) 1.17637(12) -0.09958(16) 0.0479(9) Uani 1 1 d . . . N6 N 0.86457(13) 1.17150(12) -0.02047(15) 0.0501(9) Uani 1 1 d . . . N7 N 0.86385(12) 1.11955(12) -0.15553(15) 0.0440(8) Uani 1 1 d . . . N8 N 0.81922(11) 1.11107(10) -0.07314(14) 0.0413(8) Uani 1 1 d . . . N9 N 0.84111(14) 1.13852(12) 0.07801(15) 0.0511(9) Uani 1 1 d . . . N10 N 0.85010(11) 1.09138(11) 0.15730(15) 0.0422(8) Uani 1 1 d . . . N11 N 0.79784(11) 1.07758(11) 0.02429(14) 0.0379(7) Uani 1 1 d . . . N12 N 0.80595(11) 1.03017(10) 0.10381(14) 0.0387(7) Uani 1 1 d . . . N13 N 0.88340(11) 1.03128(11) 0.22368(16) 0.0446(8) Uani 1 1 d . . . N14 N 0.93316(11) 0.97717(12) 0.25686(16) 0.0449(8) Uani 1 1 d . . . N15 N 0.83880(11) 0.97042(11) 0.17057(15) 0.0409(8) Uani 1 1 d . . . N16 N 0.88699(11) 0.91533(11) 0.20763(15) 0.0426(8) Uani 1 1 d . . . O1 O 1.04727(11) 1.18002(11) -0.11778(15) 0.0597(8) Uani 1 1 d . . . O2 O 0.94071(13) 1.19762(13) -0.00619(16) 0.0748(10) Uani 1 1 d . . . O3 O 0.90536(12) 1.14945(11) 0.14038(15) 0.0658(9) Uani 1 1 d . . . O4 O 0.96017(10) 1.05311(10) 0.24427(15) 0.0571(8) Uani 1 1 d . . . O5 O 0.93334(10) 1.02520(10) -0.24302(14) 0.0553(8) Uani 1 1 d . . . O6 O 0.82357(10) 1.04960(10) -0.14327(13) 0.0483(7) Uani 1 1 d . . . O7 O 0.79644(11) 0.99689(10) 0.00909(13) 0.0514(7) Uani 1 1 d . . . O8 O 0.84889(11) 0.90104(10) 0.11670(14) 0.0558(8) 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 Cl1 0.322(6) 0.084(2) 0.081(2) 0.000 0.000 -0.119(3) Cl2 0.1176(19) 0.142(3) 0.0567(14) 0.0580(19) -0.0202(14) -0.033(3) Tb1 0.0464(7) 0.0536(7) 0.0531(8) 0.0019(5) -0.0072(5) 0.0024(5) Tb2 0.0403(14) 0.0335(13) 0.0591(17) 0.000 0.000 0.0012(9) O1W 0.164(12) 0.218(15) 0.252(18) -0.140(14) 0.010(12) 0.061(11) O2W 0.132(10) 0.169(12) 0.265(18) 0.042(12) 0.006(11) 0.047(9) C1 0.046(2) 0.039(2) 0.060(3) -0.004(2) -0.001(2) -0.0063(18) C2 0.041(2) 0.046(2) 0.045(2) 0.0100(18) 0.0006(18) -0.0025(17) C3 0.035(2) 0.053(2) 0.041(2) 0.0055(19) 0.0008(17) -0.0037(17) C4 0.042(2) 0.049(2) 0.034(2) 0.0010(18) -0.0039(17) 0.0035(19) C5 0.054(3) 0.043(2) 0.062(3) -0.014(2) 0.009(2) -0.017(2) C6 0.035(2) 0.051(2) 0.035(2) -0.0015(17) -0.0013(16) 0.0022(17) C7 0.066(3) 0.046(2) 0.047(3) -0.009(2) -0.004(2) 0.002(2) C8 0.044(2) 0.036(2) 0.041(2) 0.0036(17) 0.0019(17) -0.0026(17) C9 0.057(2) 0.036(2) 0.037(2) -0.0078(17) 0.0086(19) -0.0002(18) C10 0.035(2) 0.042(2) 0.036(2) 0.0017(17) -0.0004(16) 0.0043(17) C11 0.101(4) 0.033(2) 0.038(2) -0.0016(18) 0.012(2) -0.014(2) C12 0.037(2) 0.041(2) 0.039(2) -0.0026(17) -0.0033(17) -0.0011(16) C13 0.052(3) 0.042(2) 0.050(3) -0.0150(19) 0.015(2) -0.0101(19) C14 0.046(2) 0.038(2) 0.031(2) -0.0054(16) 0.0064(17) 0.0006(17) C15 0.037(2) 0.036(2) 0.045(2) -0.0044(17) 0.0076(17) -0.0022(16) C16 0.0274(18) 0.037(2) 0.045(2) -0.0039(18) 0.0008(16) -0.0030(15) C17 0.053(2) 0.032(2) 0.051(3) -0.0071(18) -0.0049(19) -0.0051(18) C18 0.042(2) 0.046(2) 0.046(2) 0.0006(18) -0.0018(18) -0.0066(18) C19 0.038(2) 0.049(2) 0.039(2) -0.0101(18) 0.0006(17) -0.0027(18) C20 0.039(2) 0.045(2) 0.042(2) -0.0083(18) 0.0027(17) -0.0029(17) C21 0.037(2) 0.048(2) 0.042(2) -0.0041(18) 0.0047(17) 0.0020(17) C22 0.039(2) 0.048(2) 0.042(2) 0.0000(19) 0.0042(18) -0.0101(18) C23 0.044(2) 0.063(3) 0.048(3) -0.015(2) -0.0054(19) 0.002(2) C24 0.038(2) 0.035(2) 0.064(3) 0.0004(19) -0.0016(19) -0.0037(17) N1 0.0409(18) 0.0439(19) 0.050(2) -0.0079(16) -0.0033(15) -0.0053(15) N2 0.0400(19) 0.0452(19) 0.055(2) -0.0164(16) 0.0005(16) -0.0030(15) N3 0.0370(18) 0.0431(19) 0.047(2) -0.0077(15) 0.0044(15) -0.0027(14) N4 0.0364(17) 0.0409(18) 0.0444(19) -0.0026(15) 0.0030(14) -0.0047(14) N5 0.047(2) 0.048(2) 0.049(2) -0.0073(16) -0.0032(16) -0.0017(15) N6 0.070(2) 0.0447(19) 0.0359(19) -0.0039(15) 0.0043(17) -0.0159(17) N7 0.0473(19) 0.0465(19) 0.0382(19) -0.0045(15) 0.0037(15) -0.0018(15) N8 0.052(2) 0.0330(17) 0.0385(19) -0.0037(14) 0.0070(15) -0.0018(14) N9 0.072(2) 0.044(2) 0.037(2) -0.0019(15) -0.0020(18) -0.0211(17) N10 0.0421(18) 0.0446(19) 0.0399(19) -0.0042(15) 0.0001(14) -0.0097(15) N11 0.0415(18) 0.0418(18) 0.0305(17) -0.0038(14) 0.0030(13) -0.0049(14) N12 0.0436(18) 0.0365(17) 0.0359(18) -0.0036(14) -0.0006(14) -0.0011(14) N13 0.0388(18) 0.0440(19) 0.051(2) -0.0018(15) -0.0092(15) -0.0038(14) N14 0.0357(18) 0.046(2) 0.052(2) -0.0026(16) -0.0065(15) -0.0034(15) N15 0.0438(18) 0.0376(18) 0.0412(19) -0.0015(14) -0.0063(15) 0.0011(14) N16 0.0373(17) 0.0438(18) 0.047(2) -0.0020(15) -0.0032(15) -0.0008(14) O1 0.0551(18) 0.0575(19) 0.066(2) -0.0184(16) -0.0110(16) -0.0072(14) O2 0.079(2) 0.081(2) 0.064(2) -0.0191(18) -0.0208(19) -0.0112(19) O3 0.071(2) 0.064(2) 0.062(2) -0.0089(16) 0.0017(17) -0.0295(17) O4 0.0445(17) 0.0546(18) 0.072(2) -0.0110(15) 0.0017(14) -0.0103(14) O5 0.0470(16) 0.0485(17) 0.070(2) -0.0122(15) 0.0008(15) -0.0120(14) O6 0.0530(17) 0.0413(16) 0.0505(17) -0.0076(13) 0.0052(13) -0.0029(13) O7 0.0665(19) 0.0386(16) 0.0490(18) -0.0097(13) -0.0042(14) -0.0011(13) O8 0.066(2) 0.0510(18) 0.0505(19) -0.0128(14) -0.0082(15) 0.0016(14) _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 Cl1 Cl2 2.202(4) 15_574 ? Cl1 Cl2 2.202(4) 12_865 ? Cl1 Cl2 2.442(4) . ? Cl1 Cl2 2.442(4) 6_674 ? Cl2 Cl2 1.425(5) 12_865 ? Cl2 Cl2 1.425(5) 15_574 ? Cl2 Cl2 1.980(6) 6_674 ? Cl2 Cl1 2.202(4) 15_574 ? Tb1 O2W 2.079(13) . ? Tb1 O2 2.435(4) . ? Tb1 O1W 2.440(18) 12_866 ? Tb1 O3 2.455(3) . ? Tb1 O1W 2.51(2) . ? Tb1 Tb1 2.5133(18) 12_866 ? Tb1 Tb1 2.5133(18) 15_575 ? Tb1 O2W 2.513(17) 15_575 ? Tb1 O1W 2.846(16) 6_674 ? Tb1 Tb1 3.226(2) 6_674 ? Tb2 O1W 1.676(15) 6_674 ? Tb2 O1W 1.676(15) . ? Tb2 O2 2.581(4) . ? Tb2 O2 2.581(4) 6_674 ? Tb2 Tb2 3.191(5) 15_575 ? O1W Tb1 2.440(18) 15_575 ? O1W Tb1 2.846(16) 6_674 ? O2W Tb1 2.513(17) 12_866 ? C1 O1 1.213(5) . ? C1 N2 1.355(5) . ? C1 N1 1.383(5) . ? C2 N3 1.438(5) . ? C2 N1 1.467(5) . ? C2 C3 1.546(6) . ? C2 H2 0.9900 . ? C3 N2 1.448(5) . ? C3 N4 1.448(5) . ? C3 H3 0.9900 . ? C4 O5 1.230(5) . ? C4 N3 1.361(5) . ? C4 N4 1.364(5) . ? C5 N5 1.441(5) . ? C5 N2 1.468(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.450(5) . ? C6 N4 1.457(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.230(5) . ? C7 N6 1.345(6) . ? C7 N5 1.353(6) . ? C8 N7 1.450(5) . ? C8 N5 1.467(5) . ? C8 C9 1.524(5) . ? C8 H8 0.9900 . ? C9 N8 1.442(5) . ? C9 N6 1.451(5) . ? C9 H9 0.9900 . ? C10 O6 1.215(4) . ? C10 N7 1.371(5) . ? C10 N8 1.382(5) . ? C11 N9 1.464(5) . ? C11 N6 1.480(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.443(5) . ? C12 N11 1.444(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.235(5) . ? C13 N9 1.339(6) . ? C13 N10 1.365(5) . ? C14 N11 1.442(5) . ? C14 N9 1.451(5) . ? C14 C15 1.553(6) . ? C14 H14 0.9900 . ? C15 N12 1.451(5) . ? C15 N10 1.463(5) . ? C15 H15 0.9900 . ? C16 O7 1.207(4) . ? C16 N12 1.365(5) . ? C16 N11 1.381(5) . ? C17 N10 1.434(5) . ? C17 N13 1.464(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.445(5) . ? C18 N12 1.452(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.232(5) . ? C19 N13 1.354(5) . ? C19 N14 1.356(5) . ? C20 N13 1.449(5) . ? C20 N15 1.456(5) . ? C20 C21 1.537(6) . ? C20 H20 0.9900 . ? C21 N16 1.451(5) . ? C21 N14 1.459(5) . ? C21 H21 0.9900 . ? C22 O8 1.223(5) . ? C22 N16 1.365(5) . ? C22 N15 1.373(5) . ? C23 N14 1.433(5) 9_775 ? C23 N3 1.455(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N1 1.431(5) . ? C24 N16 1.452(5) 9_775 ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? N14 C23 1.433(5) 9_775 ? N16 C24 1.452(5) 9_775 ? 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 Cl2 Cl1 Cl2 53.42(19) 15_574 12_865 ? Cl2 Cl1 Cl2 35.25(11) 15_574 . ? Cl2 Cl1 Cl2 35.25(11) 12_865 . ? Cl2 Cl1 Cl2 35.25(11) 15_574 6_674 ? Cl2 Cl1 Cl2 35.25(11) 12_865 6_674 ? Cl2 Cl1 Cl2 47.82(13) . 6_674 ? Cl2 Cl2 Cl2 88.01(7) 12_865 15_574 ? Cl2 Cl2 Cl2 46.00(4) 12_865 6_674 ? Cl2 Cl2 Cl2 46.00(4) 15_574 6_674 ? Cl2 Cl2 Cl1 81.62(16) 12_865 15_574 ? Cl2 Cl2 Cl1 81.62(16) 15_574 15_574 ? Cl2 Cl2 Cl1 63.29(10) 6_674 15_574 ? Cl2 Cl2 Cl1 63.13(19) 12_865 . ? Cl2 Cl2 Cl1 63.13(18) 15_574 . ? Cl2 Cl2 Cl1 66.09(7) 6_674 . ? Cl1 Cl2 Cl1 129.38(16) 15_574 . ? O2W Tb1 O2 87.3(5) . . ? O2W Tb1 O1W 85.2(7) . 12_866 ? O2 Tb1 O1W 164.6(3) . 12_866 ? O2W Tb1 O3 72.1(4) . . ? O2 Tb1 O3 95.96(12) . . ? O1W Tb1 O3 68.9(3) 12_866 . ? O2W Tb1 O1W 139.4(6) . . ? O2 Tb1 O1W 64.6(3) . . ? O1W Tb1 O1W 128.3(5) 12_866 . ? O3 Tb1 O1W 135.9(4) . . ? O2W Tb1 Tb1 65.6(5) . 12_866 ? O2 Tb1 Tb1 127.35(11) . 12_866 ? O1W Tb1 Tb1 60.8(4) 12_866 12_866 ? O3 Tb1 Tb1 114.98(11) . 12_866 ? O1W Tb1 Tb1 107.7(4) . 12_866 ? O2W Tb1 Tb1 144.4(5) . 15_575 ? O2 Tb1 Tb1 122.15(11) . 15_575 ? O1W Tb1 Tb1 70.1(4) 12_866 15_575 ? O3 Tb1 Tb1 118.77(10) . 15_575 ? O1W Tb1 Tb1 58.2(3) . 15_575 ? Tb1 Tb1 Tb1 79.84(4) 12_866 15_575 ? O2W Tb1 O2W 144.5(2) . 15_575 ? O2 Tb1 O2W 109.8(4) . 15_575 ? O1W Tb1 O2W 70.2(6) 12_866 15_575 ? O3 Tb1 O2W 75.3(3) . 15_575 ? O1W Tb1 O2W 75.4(5) . 15_575 ? Tb1 Tb1 O2W 118.5(3) 12_866 15_575 ? Tb1 Tb1 O2W 48.9(3) 15_575 15_575 ? O2W Tb1 O1W 68.6(5) . 6_674 ? O2 Tb1 O1W 74.9(4) . 6_674 ? O1W Tb1 O1W 114.5(7) 12_866 6_674 ? O3 Tb1 O1W 139.9(4) . 6_674 ? O1W Tb1 O1W 75.8(4) . 6_674 ? Tb1 Tb1 O1W 53.7(4) 12_866 6_674 ? Tb1 Tb1 O1W 98.1(4) 15_575 6_674 ? O2W Tb1 O1W 144.8(5) 15_575 6_674 ? O2W Tb1 Tb1 107.0(4) . 6_674 ? O2 Tb1 Tb1 104.81(9) . 6_674 ? O1W Tb1 Tb1 90.3(3) 12_866 6_674 ? O3 Tb1 Tb1 159.18(8) . 6_674 ? O1W Tb1 Tb1 57.9(4) . 6_674 ? Tb1 Tb1 Tb1 50.08(2) 12_866 6_674 ? Tb1 Tb1 Tb1 50.08(2) 15_575 6_674 ? O2W Tb1 Tb1 98.6(3) 15_575 6_674 ? O1W Tb1 Tb1 48.3(4) 6_674 6_674 ? O1W Tb2 O1W 159.4(12) 6_674 . ? O1W Tb2 O2 96.3(7) 6_674 . ? O1W Tb2 O2 73.3(5) . . ? O1W Tb2 O2 73.3(5) 6_674 6_674 ? O1W Tb2 O2 96.3(7) . 6_674 ? O2 Tb2 O2 120.4(2) . 6_674 ? O1W Tb2 Tb2 100.3(6) 6_674 15_575 ? O1W Tb2 Tb2 100.3(6) . 15_575 ? O2 Tb2 Tb2 119.79(10) . 15_575 ? O2 Tb2 Tb2 119.79(10) 6_674 15_575 ? Tb2 O1W Tb1 78.3(7) . 15_575 ? Tb2 O1W Tb1 50.4(6) . . ? Tb1 O1W Tb1 61.1(5) 15_575 . ? Tb2 O1W Tb1 41.3(4) . 6_674 ? Tb1 O1W Tb1 56.2(4) 15_575 6_674 ? Tb1 O1W Tb1 73.8(5) . 6_674 ? Tb1 O2W Tb1 65.6(5) . 12_866 ? O1 C1 N2 125.8(4) . . ? O1 C1 N1 125.9(4) . . ? N2 C1 N1 108.3(4) . . ? N3 C2 N1 114.6(3) . . ? N3 C2 C3 103.7(3) . . ? N1 C2 C3 103.1(3) . . ? N3 C2 H2 111.6 . . ? N1 C2 H2 111.6 . . ? C3 C2 H2 111.6 . . ? N2 C3 N4 114.0(3) . . ? N2 C3 C2 103.6(3) . . ? N4 C3 C2 102.6(3) . . ? N2 C3 H3 112.0 . . ? N4 C3 H3 112.0 . . ? C2 C3 H3 112.0 . . ? O5 C4 N3 126.0(4) . . ? O5 C4 N4 126.0(4) . . ? N3 C4 N4 107.9(3) . . ? N5 C5 N2 112.8(3) . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? N2 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N7 C6 N4 113.8(3) . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6B 108.8 . . ? N4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 126.5(4) . . ? O2 C7 N5 124.2(4) . . ? N6 C7 N5 109.2(4) . . ? N7 C8 N5 113.6(3) . . ? N7 C8 C9 104.0(3) . . ? N5 C8 C9 104.1(3) . . ? N7 C8 H8 111.5 . . ? N5 C8 H8 111.5 . . ? C9 C8 H8 111.5 . . ? N8 C9 N6 114.4(3) . . ? N8 C9 C8 103.7(3) . . ? N6 C9 C8 102.6(3) . . ? N8 C9 H9 111.9 . . ? N6 C9 H9 111.9 . . ? C8 C9 H9 111.9 . . ? O6 C10 N7 125.6(4) . . ? O6 C10 N8 127.1(4) . . ? N7 C10 N8 107.3(3) . . ? N9 C11 N6 112.3(3) . . ? N9 C11 H11A 109.2 . . ? N6 C11 H11A 109.2 . . ? N9 C11 H11B 109.2 . . ? N6 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N8 C12 N11 113.5(3) . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12B 108.9 . . ? N11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 126.3(4) . . ? O3 C13 N10 124.3(4) . . ? N9 C13 N10 109.4(4) . . ? N11 C14 N9 113.6(3) . . ? N11 C14 C15 103.3(3) . . ? N9 C14 C15 101.9(3) . . ? N11 C14 H14 112.4 . . ? N9 C14 H14 112.4 . . ? C15 C14 H14 112.4 . . ? N12 C15 N10 113.6(3) . . ? N12 C15 C14 103.1(3) . . ? N10 C15 C14 104.0(3) . . ? N12 C15 H15 111.8 . . ? N10 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? O7 C16 N12 126.4(4) . . ? O7 C16 N11 126.2(4) . . ? N12 C16 N11 107.4(3) . . ? N10 C17 N13 113.9(3) . . ? N10 C17 H17A 108.8 . . ? N13 C17 H17A 108.8 . . ? N10 C17 H17B 108.8 . . ? N13 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N15 C18 N12 113.5(3) . . ? N15 C18 H18A 108.9 . . ? N12 C18 H18A 108.9 . . ? N15 C18 H18B 108.9 . . ? N12 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N13 125.9(4) . . ? O4 C19 N14 125.2(4) . . ? N13 C19 N14 108.9(3) . . ? N13 C20 N15 113.8(3) . . ? N13 C20 C21 102.9(3) . . ? N15 C20 C21 103.5(3) . . ? N13 C20 H20 112.0 . . ? N15 C20 H20 112.0 . . ? C21 C20 H20 112.0 . . ? N16 C21 N14 113.7(3) . . ? N16 C21 C20 103.9(3) . . ? N14 C21 C20 103.6(3) . . ? N16 C21 H21 111.7 . . ? N14 C21 H21 111.7 . . ? C20 C21 H21 111.7 . . ? O8 C22 N16 125.7(4) . . ? O8 C22 N15 125.6(4) . . ? N16 C22 N15 108.7(3) . . ? N14 C23 N3 114.1(3) 9_775 . ? N14 C23 H23A 108.7 9_775 . ? N3 C23 H23A 108.7 . . ? N14 C23 H23B 108.7 9_775 . ? N3 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N1 C24 N16 114.0(3) . 9_775 ? N1 C24 H24A 108.8 . . ? N16 C24 H24A 108.8 9_775 . ? N1 C24 H24B 108.8 . . ? N16 C24 H24B 108.8 9_775 . ? H24A C24 H24B 107.7 . . ? C1 N1 C24 123.2(3) . . ? C1 N1 C2 111.6(3) . . ? C24 N1 C2 123.2(3) . . ? C1 N2 C3 113.0(3) . . ? C1 N2 C5 122.2(3) . . ? C3 N2 C5 121.4(3) . . ? C4 N3 C2 112.6(3) . . ? C4 N3 C23 121.6(3) . . ? C2 N3 C23 123.3(3) . . ? C4 N4 C3 112.8(3) . . ? C4 N4 C6 121.5(3) . . ? C3 N4 C6 121.5(3) . . ? C7 N5 C5 121.4(4) . . ? C7 N5 C8 110.6(3) . . ? C5 N5 C8 121.6(3) . . ? C7 N6 C9 112.9(3) . . ? C7 N6 C11 123.5(4) . . ? C9 N6 C11 121.8(4) . . ? C10 N7 C8 112.1(3) . . ? C10 N7 C6 122.0(3) . . ? C8 N7 C6 124.3(3) . . ? C10 N8 C9 112.3(3) . . ? C10 N8 C12 121.4(3) . . ? C9 N8 C12 123.9(3) . . ? C13 N9 C14 113.7(3) . . ? C13 N9 C11 123.2(4) . . ? C14 N9 C11 121.2(4) . . ? C13 N10 C17 123.3(3) . . ? C13 N10 C15 110.8(3) . . ? C17 N10 C15 122.8(3) . . ? C16 N11 C14 112.9(3) . . ? C16 N11 C12 121.8(3) . . ? C14 N11 C12 122.8(3) . . ? C16 N12 C15 113.1(3) . . ? C16 N12 C18 121.1(3) . . ? C15 N12 C18 122.5(3) . . ? C19 N13 C20 112.8(3) . . ? C19 N13 C17 121.9(3) . . ? C20 N13 C17 122.9(3) . . ? C19 N14 C23 122.3(3) . 9_775 ? C19 N14 C21 111.7(3) . . ? C23 N14 C21 123.5(3) 9_775 . ? C22 N15 C18 122.7(3) . . ? C22 N15 C20 111.7(3) . . ? C18 N15 C20 122.3(3) . . ? C22 N16 C21 112.0(3) . . ? C22 N16 C24 122.7(3) . 9_775 ? C21 N16 C24 123.8(3) . 9_775 ? C7 O2 Tb1 140.5(3) . . ? C7 O2 Tb2 164.3(3) . . ? Tb1 O2 Tb2 45.25(8) . . ? C13 O3 Tb1 140.2(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.045 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.077 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 358 107 ' ' 2 -0.003 -0.035 0.460 4382 1735 ' ' 3 0.000 0.500 1.000 358 107 ' ' 4 0.250 0.250 0.250 358 108 ' ' 5 0.250 0.750 0.750 358 108 ' ' 6 0.500 0.000 0.500 358 107 ' ' 7 0.500 0.500 0.500 358 107 ' ' 8 0.750 0.250 0.250 358 108 ' ' 9 0.750 0.750 0.750 358 108 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952103' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H239 Cl4 Ho N64 O103' _chemical_formula_weight 4245.24 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' Ho Ho -0.2175 4.6783 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 28.464(4) _cell_length_b 28.464(4) _cell_length_c 21.992(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17817(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8888 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8791 _exptl_absorpt_correction_T_max 0.9226 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62083 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8723 _reflns_number_gt 5167 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1627P)^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 8723 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.2562 _refine_ls_wR_factor_gt 0.2333 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 Cl1 Cl 0.49690(13) 0.71327(13) -0.38314(13) 0.1265(15) Uani 0.60 1 d P . . Cl2 Cl 0.5000 0.7500 -0.27903(16) 0.174(2) Uani 0.80 2 d SP . . Ho1 Ho 0.45845(3) 0.70927(3) 0.10180(5) 0.0490(4) Uani 0.1997(5) 1 d P . 1 Ho2 Ho 0.5000 0.7500 0.04869(14) 0.0518(11) Uani 0.1006(11) 2 d SP . 2 O1W O 0.4956(3) 0.6404(3) 0.0940(5) 0.108(3) Uani 0.50 1 d P . . O2W O 0.4516(4) 0.7803(3) 0.0437(4) 0.128(4) Uani 0.50 1 d P . . C1 C 0.52539(14) 0.66142(13) -0.16000(19) 0.0446(9) Uani 1 1 d . . . C2 C 0.50855(13) 0.62221(14) -0.25255(17) 0.0429(9) Uani 1 1 d . . . H2 H 0.5161 0.6351 -0.2932 0.051 Uiso 1 1 calc R . . C3 C 0.46308(12) 0.64404(13) -0.22553(17) 0.0409(9) Uani 1 1 d . . . H3 H 0.4498 0.6682 -0.2530 0.049 Uiso 1 1 calc R . . C4 C 0.45210(13) 0.56364(13) -0.23887(17) 0.0410(9) Uani 1 1 d . . . C5 C 0.44934(14) 0.69808(13) -0.1349(2) 0.0506(10) Uani 1 1 d . . . H5A H 0.4351 0.7204 -0.1634 0.061 Uiso 1 1 calc R . . H5B H 0.4697 0.7158 -0.1072 0.061 Uiso 1 1 calc R . . C6 C 0.38107(12) 0.60997(14) -0.21625(17) 0.0429(9) Uani 1 1 d . . . H6A H 0.3716 0.6361 -0.2425 0.052 Uiso 1 1 calc R . . H6B H 0.3661 0.5814 -0.2317 0.052 Uiso 1 1 calc R . . C7 C 0.40870(16) 0.68208(14) -0.03876(19) 0.0502(10) Uani 1 1 d . . . C8 C 0.36640(13) 0.66452(12) -0.12559(17) 0.0405(9) Uani 1 1 d . . . H8 H 0.3555 0.6900 -0.1528 0.049 Uiso 1 1 calc R . . C9 C 0.33451(13) 0.65900(12) -0.07018(16) 0.0388(8) Uani 1 1 d . . . H9 H 0.3073 0.6806 -0.0723 0.047 Uiso 1 1 calc R . . C10 C 0.33541(13) 0.58848(12) -0.12494(16) 0.0378(8) Uani 1 1 d . . . C11 C 0.3466(2) 0.68016(13) 0.04109(19) 0.0622(13) Uani 1 1 d . . . H11A H 0.3681 0.7018 0.0618 0.075 Uiso 1 1 calc R . . H11B H 0.3160 0.6957 0.0378 0.075 Uiso 1 1 calc R . . C12 C 0.28299(12) 0.59075(13) -0.03518(16) 0.0391(8) Uani 1 1 d . . . H12A H 0.2577 0.6139 -0.0310 0.047 Uiso 1 1 calc R . . H12B H 0.2699 0.5631 -0.0556 0.047 Uiso 1 1 calc R . . C13 C 0.37003(14) 0.62833(12) 0.12624(19) 0.0445(10) Uani 1 1 d . . . C14 C 0.29996(13) 0.60953(12) 0.07522(16) 0.0390(8) Uani 1 1 d . . . H14 H 0.2709 0.6286 0.0777 0.047 Uiso 1 1 calc R . . C15 C 0.30559(12) 0.57652(12) 0.13120(18) 0.0378(8) Uani 1 1 d . . . H15 H 0.2794 0.5801 0.1605 0.045 Uiso 1 1 calc R . . C16 C 0.30074(11) 0.53094(12) 0.04299(18) 0.0374(8) Uani 1 1 d . . . C17 C 0.36458(14) 0.57914(13) 0.21734(19) 0.0470(10) Uani 1 1 d . . . H17A H 0.3372 0.5819 0.2441 0.056 Uiso 1 1 calc R . . H17B H 0.3881 0.6019 0.2313 0.056 Uiso 1 1 calc R . . C18 C 0.29813(13) 0.48784(13) 0.14003(19) 0.0426(9) Uani 1 1 d . . . H18A H 0.2865 0.4632 0.1128 0.051 Uiso 1 1 calc R . . H18B H 0.2736 0.4943 0.1701 0.051 Uiso 1 1 calc R . . C19 C 0.42893(13) 0.52357(14) 0.24083(17) 0.0425(9) Uani 1 1 d . . . C20 C 0.35516(13) 0.49036(13) 0.22953(17) 0.0401(9) Uani 1 1 d . . . H20 H 0.3285 0.4954 0.2577 0.048 Uiso 1 1 calc R . . C21 C 0.38932(12) 0.45266(13) 0.25327(18) 0.0416(9) Uani 1 1 d . . . H21 H 0.3797 0.4408 0.2937 0.050 Uiso 1 1 calc R . . C22 C 0.35824(12) 0.42714(13) 0.16135(17) 0.0393(8) Uani 1 1 d . . . C23 C 0.47426(14) 0.46005(15) 0.28929(19) 0.0495(10) Uani 1 1 d . . . H23A H 0.4942 0.4865 0.3016 0.059 Uiso 1 1 calc R . . H23B H 0.4632 0.4445 0.3264 0.059 Uiso 1 1 calc R . . C24 C 0.59396(13) 0.63093(13) -0.21769(19) 0.0450(9) Uani 1 1 d . . . H24A H 0.6107 0.6527 -0.1908 0.054 Uiso 1 1 calc R . . H24B H 0.6005 0.6403 -0.2597 0.054 Uiso 1 1 calc R . . N1 N 0.54414(11) 0.63501(11) -0.20654(15) 0.0442(8) Uani 1 1 d . . . N2 N 0.47767(11) 0.66440(11) -0.16862(16) 0.0470(8) Uani 1 1 d . . . N3 N 0.49746(10) 0.57301(11) -0.25484(14) 0.0411(7) Uani 1 1 d . . . N4 N 0.43198(10) 0.60440(10) -0.21996(14) 0.0404(7) Uani 1 1 d . . . N5 N 0.41191(11) 0.67489(11) -0.09952(15) 0.0456(8) Uani 1 1 d . . . N6 N 0.36475(13) 0.67054(11) -0.02068(15) 0.0516(9) Uani 1 1 d . . . N7 N 0.36430(11) 0.61887(10) -0.15521(15) 0.0417(7) Uani 1 1 d . . . N8 N 0.31979(11) 0.61052(10) -0.07291(14) 0.0418(7) Uani 1 1 d . . . N9 N 0.34157(13) 0.63828(11) 0.07744(15) 0.0501(9) Uani 1 1 d . . . N10 N 0.35091(10) 0.59116(10) 0.15756(14) 0.0403(7) Uani 1 1 d . . . N11 N 0.29893(10) 0.57727(10) 0.02454(13) 0.0385(7) Uani 1 1 d . . . N12 N 0.30677(10) 0.53008(10) 0.10482(13) 0.0368(7) Uani 1 1 d . . . N13 N 0.38407(10) 0.53188(11) 0.22370(15) 0.0430(8) Uani 1 1 d . . . N14 N 0.43394(10) 0.47817(11) 0.25633(15) 0.0458(8) Uani 1 1 d . . . N15 N 0.33984(10) 0.47073(10) 0.17135(14) 0.0400(7) Uani 1 1 d . . . N16 N 0.38792(10) 0.41619(10) 0.20793(14) 0.0406(7) Uani 1 1 d . . . O1 O 0.54705(10) 0.67934(10) -0.11835(15) 0.0616(8) Uani 1 1 d . . . O2 O 0.44106(13) 0.69605(13) -0.00681(15) 0.0769(10) Uani 1 1 d . . . O3 O 0.40598(11) 0.64872(11) 0.14039(14) 0.0646(9) Uani 1 1 d . . . O4 O 0.46065(9) 0.55376(10) 0.24303(14) 0.0562(8) Uani 1 1 d . . . O5 O 0.43296(9) 0.52492(9) -0.24177(13) 0.0517(7) Uani 1 1 d . . . O6 O 0.32405(9) 0.54906(9) -0.14235(12) 0.0466(7) Uani 1 1 d . . . O7 O 0.29765(10) 0.49667(9) 0.00977(13) 0.0515(7) Uani 1 1 d . . . O8 O 0.34956(10) 0.40192(10) 0.11741(13) 0.0545(7) 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 Cl1 0.1109(19) 0.195(3) 0.0740(18) 0.090(2) -0.0233(16) -0.045(3) Cl2 0.336(6) 0.099(2) 0.088(2) 0.000 0.000 -0.137(3) Ho1 0.0455(6) 0.0491(6) 0.0524(7) 0.0008(4) -0.0084(4) 0.0016(4) Ho2 0.0528(18) 0.0450(17) 0.058(2) 0.000 0.000 -0.0017(12) O1W 0.059(4) 0.115(7) 0.151(8) 0.034(6) -0.006(5) 0.020(4) O2W 0.179(10) 0.109(7) 0.095(7) -0.042(5) 0.013(6) 0.083(6) C1 0.049(2) 0.037(2) 0.047(3) -0.0001(18) -0.0035(19) -0.0046(17) C2 0.043(2) 0.049(2) 0.037(2) 0.0043(17) -0.0036(16) -0.0051(17) C3 0.0376(19) 0.047(2) 0.038(2) 0.0049(17) -0.0023(16) -0.0014(16) C4 0.041(2) 0.047(2) 0.036(2) 0.0010(17) -0.0082(16) -0.0003(17) C5 0.052(2) 0.041(2) 0.059(3) -0.0098(19) 0.014(2) -0.0146(17) C6 0.0361(19) 0.055(2) 0.038(2) -0.0018(18) -0.0005(16) 0.0006(16) C7 0.069(3) 0.041(2) 0.041(2) -0.0062(18) -0.004(2) 0.0036(19) C8 0.046(2) 0.0345(19) 0.041(2) 0.0024(16) 0.0004(17) -0.0004(15) C9 0.050(2) 0.0353(19) 0.031(2) -0.0041(15) 0.0019(16) 0.0043(16) C10 0.043(2) 0.039(2) 0.032(2) -0.0010(16) -0.0036(16) 0.0010(16) C11 0.110(4) 0.034(2) 0.042(3) -0.0013(18) 0.012(2) -0.018(2) C12 0.0374(19) 0.047(2) 0.033(2) -0.0031(16) 0.0015(15) 0.0007(16) C13 0.051(2) 0.0343(19) 0.048(3) -0.0146(17) 0.0138(19) -0.0113(17) C14 0.045(2) 0.041(2) 0.031(2) -0.0005(15) 0.0031(16) 0.0061(16) C15 0.0316(18) 0.0350(18) 0.047(2) -0.0012(16) 0.0065(15) 0.0028(14) C16 0.0262(17) 0.0351(19) 0.051(2) 0.0010(17) 0.0015(15) -0.0008(14) C17 0.048(2) 0.039(2) 0.053(3) -0.0054(18) -0.0102(19) -0.0072(17) C18 0.0369(19) 0.039(2) 0.052(3) 0.0025(17) -0.0031(17) -0.0078(15) C19 0.043(2) 0.050(2) 0.034(2) -0.0078(17) 0.0068(16) -0.0026(17) C20 0.0387(19) 0.045(2) 0.037(2) -0.0039(16) 0.0058(16) -0.0026(15) C21 0.0339(19) 0.052(2) 0.038(2) 0.0020(17) 0.0018(16) -0.0001(16) C22 0.038(2) 0.042(2) 0.037(2) -0.0041(17) 0.0048(16) -0.0089(16) C23 0.045(2) 0.060(2) 0.044(2) -0.0151(19) -0.0102(18) 0.0059(18) C24 0.039(2) 0.043(2) 0.053(3) 0.0003(18) -0.0007(18) -0.0087(16) N1 0.0413(17) 0.0438(17) 0.048(2) -0.0052(15) -0.0094(14) -0.0014(14) N2 0.0413(18) 0.0435(18) 0.056(2) -0.0101(15) -0.0019(15) -0.0029(14) N3 0.0409(17) 0.0425(17) 0.0398(19) -0.0082(14) -0.0009(14) -0.0031(13) N4 0.0357(16) 0.0399(17) 0.0456(19) -0.0027(14) 0.0033(14) -0.0044(13) N5 0.0444(18) 0.0468(18) 0.046(2) -0.0069(15) 0.0005(15) -0.0030(14) N6 0.078(3) 0.0429(18) 0.0341(19) -0.0046(14) 0.0032(17) -0.0144(17) N7 0.0428(17) 0.0419(17) 0.0405(19) -0.0077(14) -0.0012(14) -0.0044(13) N8 0.0518(19) 0.0387(17) 0.0349(18) -0.0005(13) 0.0062(14) -0.0019(14) N9 0.076(2) 0.0384(17) 0.0355(19) -0.0034(14) 0.0010(17) -0.0175(16) N10 0.0439(17) 0.0404(17) 0.0368(19) -0.0042(13) -0.0007(14) -0.0074(13) N11 0.0420(17) 0.0433(17) 0.0302(17) -0.0055(13) 0.0039(13) -0.0038(13) N12 0.0459(17) 0.0354(15) 0.0292(17) -0.0021(12) -0.0010(13) -0.0009(13) N13 0.0375(17) 0.0448(18) 0.047(2) -0.0029(14) -0.0054(14) -0.0065(13) N14 0.0367(17) 0.0452(19) 0.056(2) -0.0059(15) -0.0069(15) -0.0011(14) N15 0.0411(17) 0.0369(16) 0.0420(19) -0.0026(13) -0.0072(14) 0.0000(13) N16 0.0407(17) 0.0377(16) 0.0434(19) -0.0046(14) -0.0057(14) 0.0012(13) O1 0.0538(17) 0.0588(18) 0.072(2) -0.0207(16) -0.0132(15) -0.0077(14) O2 0.080(2) 0.089(2) 0.062(2) -0.0228(18) -0.0222(18) -0.0112(19) O3 0.072(2) 0.0630(19) 0.059(2) -0.0097(15) 0.0044(16) -0.0251(16) O4 0.0418(15) 0.0505(16) 0.076(2) -0.0120(15) 0.0025(14) -0.0113(13) O5 0.0468(15) 0.0461(16) 0.062(2) -0.0095(13) 0.0004(13) -0.0115(12) O6 0.0526(16) 0.0419(15) 0.0454(16) -0.0065(12) 0.0022(12) -0.0059(12) O7 0.0705(19) 0.0376(15) 0.0463(17) -0.0114(12) -0.0057(14) -0.0020(13) O8 0.0651(18) 0.0491(16) 0.0493(18) -0.0104(13) -0.0082(14) 0.0008(13) _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 Cl1 Cl1 1.526(6) 15_564 ? Cl1 Cl1 1.526(6) 12_765 ? Cl1 Cl1 2.098(7) 6_564 ? Cl1 Cl2 2.198(4) 15_564 ? Cl2 Cl1 2.198(4) 15_564 ? Cl2 Cl1 2.198(4) 12_765 ? Ho1 O1W 2.236(8) . ? Ho1 O2W 2.330(9) 12_766 ? Ho1 O2W 2.398(10) . ? Ho1 O3 2.433(3) . ? Ho1 O2 2.468(3) . ? Ho1 Ho1 2.5548(15) 15_565 ? Ho1 Ho1 2.5548(15) 12_766 ? Ho1 O1W 2.613(10) 15_565 ? Ho1 O2W 2.876(11) 6_564 ? Ho1 Ho1 3.312(2) 6_564 ? Ho2 O2W 1.627(9) . ? Ho2 O2W 1.627(9) 6_564 ? Ho2 O2 2.581(4) . ? Ho2 O2 2.581(4) 6_564 ? Ho2 Ho2 3.357(6) 15_565 ? O1W Ho1 2.613(10) 12_766 ? O2W Ho1 2.330(9) 15_565 ? O2W Ho1 2.876(11) 6_564 ? C1 O1 1.216(5) . ? C1 N2 1.374(5) . ? C1 N1 1.377(5) . ? C2 N3 1.437(5) . ? C2 N1 1.477(5) . ? C2 C3 1.554(5) . ? C2 H2 0.9900 . ? C3 N4 1.439(5) . ? C3 N2 1.440(5) . ? C3 H3 0.9900 . ? C4 O5 1.231(4) . ? C4 N4 1.359(5) . ? C4 N3 1.364(5) . ? C5 N2 1.456(5) . ? C5 N5 1.475(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.447(5) . ? C6 N4 1.460(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.225(5) . ? C7 N6 1.353(6) . ? C7 N5 1.355(5) . ? C8 N5 1.447(5) . ? C8 N7 1.455(5) . ? C8 C9 1.528(5) . ? C8 H8 0.9900 . ? C9 N6 1.426(5) . ? C9 N8 1.443(5) . ? C9 H9 0.9900 . ? C10 O6 1.229(4) . ? C10 N7 1.367(5) . ? C10 N8 1.379(5) . ? C11 N9 1.443(5) . ? C11 N6 1.478(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.442(5) . ? C12 N8 1.450(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.217(5) . ? C13 N9 1.374(5) . ? C13 N10 1.375(5) . ? C14 N9 1.440(5) . ? C14 N11 1.444(5) . ? C14 C15 1.557(5) . ? C14 H14 0.9900 . ? C15 N12 1.444(4) . ? C15 N10 1.474(5) . ? C15 H15 0.9900 . ? C16 O7 1.222(4) . ? C16 N12 1.371(5) . ? C16 N11 1.381(5) . ? C17 N10 1.413(5) . ? C17 N13 1.462(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.451(5) . ? C18 N15 1.456(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.247(4) . ? C19 N14 1.344(5) . ? C19 N13 1.352(5) . ? C20 N13 1.446(5) . ? C20 N15 1.463(5) . ? C20 C21 1.539(5) . ? C20 H20 0.9900 . ? C21 N16 1.440(5) . ? C21 N14 1.465(5) . ? C21 H21 0.9900 . ? C22 O8 1.229(4) . ? C22 N16 1.364(5) . ? C22 N15 1.365(5) . ? C23 N3 1.452(5) 9_665 ? C23 N14 1.452(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N1 1.444(5) . ? C24 N16 1.453(5) 9_665 ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? N3 C23 1.452(5) 9_665 ? N16 C24 1.453(5) 9_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Cl1 Cl1 86.84(9) 15_564 12_765 ? Cl1 Cl1 Cl1 46.58(4) 15_564 6_564 ? Cl1 Cl1 Cl1 46.58(4) 12_765 6_564 ? Cl1 Cl1 Cl2 83.00(15) 15_564 15_564 ? Cl1 Cl1 Cl2 83.00(15) 12_765 15_564 ? Cl1 Cl1 Cl2 61.49(11) 6_564 15_564 ? Cl1 Cl2 Cl1 57.0(2) 15_564 12_765 ? O1W Ho1 O2W 85.9(4) . 12_766 ? O1W Ho1 O2W 137.4(3) . . ? O2W Ho1 O2W 127.9(4) 12_766 . ? O1W Ho1 O3 72.3(2) . . ? O2W Ho1 O3 71.0(2) 12_766 . ? O2W Ho1 O3 137.1(3) . . ? O1W Ho1 O2 83.5(3) . . ? O2W Ho1 O2 165.4(3) 12_766 . ? O2W Ho1 O2 66.2(2) . . ? O3 Ho1 O2 96.11(12) . . ? O1W Ho1 Ho1 146.2(2) . 15_565 ? O2W Ho1 Ho1 72.0(3) 12_766 15_565 ? O2W Ho1 Ho1 56.0(2) . 15_565 ? O3 Ho1 Ho1 121.05(9) . 15_565 ? O2 Ho1 Ho1 121.88(10) . 15_565 ? O1W Ho1 Ho1 65.7(2) . 12_766 ? O2W Ho1 Ho1 58.6(2) 12_766 12_766 ? O2W Ho1 Ho1 107.1(3) . 12_766 ? O3 Ho1 Ho1 114.64(10) . 12_766 ? O2 Ho1 Ho1 124.67(10) . 12_766 ? Ho1 Ho1 Ho1 80.82(3) 15_565 12_766 ? O1W Ho1 O1W 144.83(15) . 15_565 ? O2W Ho1 O1W 72.4(4) 12_766 15_565 ? O2W Ho1 O1W 76.7(3) . 15_565 ? O3 Ho1 O1W 74.54(18) . 15_565 ? O2 Ho1 O1W 111.6(2) . 15_565 ? Ho1 Ho1 O1W 51.26(16) 15_565 15_565 ? Ho1 Ho1 O1W 120.15(19) 12_766 15_565 ? O1W Ho1 O2W 68.6(3) . 6_564 ? O2W Ho1 O2W 109.0(4) 12_766 6_564 ? O2W Ho1 O2W 75.4(3) . 6_564 ? O3 Ho1 O2W 140.76(19) . 6_564 ? O2 Ho1 O2W 76.4(2) . 6_564 ? Ho1 Ho1 O2W 94.3(2) 15_565 6_564 ? Ho1 Ho1 O2W 50.39(18) 12_766 6_564 ? O1W Ho1 O2W 144.3(3) 15_565 6_564 ? O1W Ho1 Ho1 106.0(2) . 6_564 ? O2W Ho1 Ho1 88.09(19) 12_766 6_564 ? O2W Ho1 Ho1 57.9(3) . 6_564 ? O3 Ho1 Ho1 159.09(8) . 6_564 ? O2 Ho1 Ho1 104.47(9) . 6_564 ? Ho1 Ho1 Ho1 49.588(17) 15_565 6_564 ? Ho1 Ho1 Ho1 49.588(17) 12_766 6_564 ? O1W Ho1 Ho1 100.72(16) 15_565 6_564 ? O2W Ho1 Ho1 44.9(2) 6_564 6_564 ? O2W Ho2 O2W 172.3(7) . 6_564 ? O2W Ho2 O2 74.5(4) . . ? O2W Ho2 O2 101.7(4) 6_564 . ? O2W Ho2 O2 101.7(4) . 6_564 ? O2W Ho2 O2 74.5(4) 6_564 6_564 ? O2 Ho2 O2 123.6(2) . 6_564 ? O2W Ho2 Ho2 93.9(3) . 15_565 ? O2W Ho2 Ho2 93.9(3) 6_564 15_565 ? O2 Ho2 Ho2 118.22(10) . 15_565 ? O2 Ho2 Ho2 118.22(10) 6_564 15_565 ? Ho1 O1W Ho1 63.0(2) . 12_766 ? Ho2 O2W Ho1 85.9(4) . 15_565 ? Ho2 O2W Ho1 56.6(3) . . ? Ho1 O2W Ho1 65.4(3) 15_565 . ? Ho2 O2W Ho1 43.3(3) . 6_564 ? Ho1 O2W Ho1 57.6(2) 15_565 6_564 ? Ho1 O2W Ho1 77.2(3) . 6_564 ? O1 C1 N2 125.4(4) . . ? O1 C1 N1 126.3(4) . . ? N2 C1 N1 108.3(3) . . ? N3 C2 N1 114.5(3) . . ? N3 C2 C3 102.7(3) . . ? N1 C2 C3 102.2(3) . . ? N3 C2 H2 112.2 . . ? N1 C2 H2 112.2 . . ? C3 C2 H2 112.2 . . ? N4 C3 N2 114.7(3) . . ? N4 C3 C2 103.4(3) . . ? N2 C3 C2 104.7(3) . . ? N4 C3 H3 111.2 . . ? N2 C3 H3 111.2 . . ? C2 C3 H3 111.2 . . ? O5 C4 N4 126.4(3) . . ? O5 C4 N3 125.5(3) . . ? N4 C4 N3 108.1(3) . . ? N2 C5 N5 112.0(3) . . ? N2 C5 H5A 109.2 . . ? N5 C5 H5A 109.2 . . ? N2 C5 H5B 109.2 . . ? N5 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N7 C6 N4 113.5(3) . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6B 108.9 . . ? N4 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 127.3(4) . . ? O2 C7 N5 124.3(4) . . ? N6 C7 N5 108.4(4) . . ? N5 C8 N7 113.4(3) . . ? N5 C8 C9 103.7(3) . . ? N7 C8 C9 103.9(3) . . ? N5 C8 H8 111.8 . . ? N7 C8 H8 111.8 . . ? C9 C8 H8 111.8 . . ? N6 C9 N8 115.3(3) . . ? N6 C9 C8 103.1(3) . . ? N8 C9 C8 103.7(3) . . ? N6 C9 H9 111.4 . . ? N8 C9 H9 111.4 . . ? C8 C9 H9 111.4 . . ? O6 C10 N7 125.8(3) . . ? O6 C10 N8 126.1(3) . . ? N7 C10 N8 108.1(3) . . ? N9 C11 N6 113.0(3) . . ? N9 C11 H11A 109.0 . . ? N6 C11 H11A 109.0 . . ? N9 C11 H11B 109.0 . . ? N6 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N11 C12 N8 113.4(3) . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? N8 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 126.7(4) . . ? O3 C13 N10 124.9(4) . . ? N9 C13 N10 108.4(3) . . ? N9 C14 N11 113.8(3) . . ? N9 C14 C15 103.4(3) . . ? N11 C14 C15 103.2(3) . . ? N9 C14 H14 111.9 . . ? N11 C14 H14 111.9 . . ? C15 C14 H14 111.9 . . ? N12 C15 N10 113.4(3) . . ? N12 C15 C14 103.7(3) . . ? N10 C15 C14 103.3(3) . . ? N12 C15 H15 111.9 . . ? N10 C15 H15 111.9 . . ? C14 C15 H15 111.9 . . ? O7 C16 N12 126.0(3) . . ? O7 C16 N11 125.7(4) . . ? N12 C16 N11 108.3(3) . . ? N10 C17 N13 114.6(3) . . ? N10 C17 H17A 108.6 . . ? N13 C17 H17A 108.6 . . ? N10 C17 H17B 108.6 . . ? N13 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? N12 C18 N15 113.0(3) . . ? N12 C18 H18A 109.0 . . ? N15 C18 H18A 109.0 . . ? N12 C18 H18B 109.0 . . ? N15 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N14 125.2(4) . . ? O4 C19 N13 125.0(4) . . ? N14 C19 N13 109.8(3) . . ? N13 C20 N15 113.8(3) . . ? N13 C20 C21 103.9(3) . . ? N15 C20 C21 102.6(3) . . ? N13 C20 H20 111.9 . . ? N15 C20 H20 111.9 . . ? C21 C20 H20 111.9 . . ? N16 C21 N14 114.4(3) . . ? N16 C21 C20 104.5(3) . . ? N14 C21 C20 102.6(3) . . ? N16 C21 H21 111.6 . . ? N14 C21 H21 111.6 . . ? C20 C21 H21 111.6 . . ? O8 C22 N16 125.6(3) . . ? O8 C22 N15 125.5(4) . . ? N16 C22 N15 108.9(3) . . ? N3 C23 N14 114.1(3) 9_665 . ? N3 C23 H23A 108.7 9_665 . ? N14 C23 H23A 108.7 . . ? N3 C23 H23B 108.7 9_665 . ? N14 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N1 C24 N16 113.5(3) . 9_665 ? N1 C24 H24A 108.9 . . ? N16 C24 H24A 108.9 9_665 . ? N1 C24 H24B 108.9 . . ? N16 C24 H24B 108.9 9_665 . ? H24A C24 H24B 107.7 . . ? C1 N1 C24 123.4(3) . . ? C1 N1 C2 112.2(3) . . ? C24 N1 C2 122.5(3) . . ? C1 N2 C3 112.3(3) . . ? C1 N2 C5 121.2(3) . . ? C3 N2 C5 123.2(3) . . ? C4 N3 C2 112.9(3) . . ? C4 N3 C23 122.2(3) . 9_665 ? C2 N3 C23 121.9(3) . 9_665 ? C4 N4 C3 112.6(3) . . ? C4 N4 C6 121.9(3) . . ? C3 N4 C6 122.0(3) . . ? C7 N5 C8 111.2(3) . . ? C7 N5 C5 120.1(3) . . ? C8 N5 C5 122.0(3) . . ? C7 N6 C9 112.9(3) . . ? C7 N6 C11 123.2(4) . . ? C9 N6 C11 122.3(4) . . ? C10 N7 C6 122.7(3) . . ? C10 N7 C8 111.8(3) . . ? C6 N7 C8 123.9(3) . . ? C10 N8 C9 112.1(3) . . ? C10 N8 C12 122.1(3) . . ? C9 N8 C12 123.9(3) . . ? C13 N9 C14 113.2(3) . . ? C13 N9 C11 123.0(3) . . ? C14 N9 C11 122.2(4) . . ? C13 N10 C17 122.9(3) . . ? C13 N10 C15 111.5(3) . . ? C17 N10 C15 122.6(3) . . ? C16 N11 C12 122.3(3) . . ? C16 N11 C14 112.3(3) . . ? C12 N11 C14 122.7(3) . . ? C16 N12 C15 112.3(3) . . ? C16 N12 C18 121.5(3) . . ? C15 N12 C18 122.7(3) . . ? C19 N13 C20 111.7(3) . . ? C19 N13 C17 123.1(3) . . ? C20 N13 C17 123.0(3) . . ? C19 N14 C23 123.5(3) . . ? C19 N14 C21 111.9(3) . . ? C23 N14 C21 122.1(3) . . ? C22 N15 C18 122.7(3) . . ? C22 N15 C20 112.0(3) . . ? C18 N15 C20 121.9(3) . . ? C22 N16 C21 111.9(3) . . ? C22 N16 C24 122.8(3) . 9_665 ? C21 N16 C24 123.6(3) . 9_665 ? C7 O2 Ho1 139.1(3) . . ? C7 O2 Ho2 162.4(3) . . ? Ho1 O2 Ho2 47.26(9) . . ? C13 O3 Ho1 139.9(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.002 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.085 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.008 -0.002 -0.004 4499 1855 ' ' 2 0.000 0.000 0.500 340 102 ' ' 3 0.000 0.500 0.500 340 102 ' ' 4 0.250 0.250 0.750 340 106 ' ' 5 0.250 0.750 0.250 340 106 ' ' 6 0.500 0.000 0.000 340 102 ' ' 7 0.500 0.500 1.000 340 102 ' ' 8 0.750 0.250 0.750 340 106 ' ' 9 0.750 0.750 0.250 340 106 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952104' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H241 Cl4 Er N64 O104' _chemical_formula_weight 4265.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 28.440(3) _cell_length_b 28.440(3) _cell_length_c 22.010(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17803(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8932 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8741 _exptl_absorpt_correction_T_max 0.9193 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62053 _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8683 _reflns_number_gt 4206 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1327P)^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 8683 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1363 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2323 _refine_ls_wR_factor_gt 0.2098 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 Cl1 Cl 0.0000 0.7500 -0.02880(15) 0.168(2) Uani 0.70 2 d SP . . Cl2 Cl 0.03625(10) 0.75098(17) -0.13235(11) 0.1326(12) Uani 0.65 1 d P . . Er1 Er 0.04207(4) 0.79015(4) 0.34855(5) 0.0726(4) Uani 0.2047(5) 1 d P . 1 Er2 Er 0.0000 0.7500 0.29930(15) 0.0633(14) Uani 0.0905(11) 2 d SP . 2 O1W O -0.0302(3) 0.7977(4) 0.2948(5) 0.146(4) Uani 0.50 1 d P . . O2W O 0.0986(6) 0.7548(4) 0.3466(11) 0.298(11) Uani 0.50 1 d P . . C1 C 0.22585(16) 0.82049(14) 0.49030(17) 0.0505(10) Uani 1 1 d . . . C2 C 0.29696(14) 0.85968(13) 0.50212(16) 0.0478(9) Uani 1 1 d . . . H2 H 0.3088 0.8690 0.5427 0.057 Uiso 1 1 calc R . . C3 C 0.25923(14) 0.89457(13) 0.47828(16) 0.0472(9) Uani 1 1 d . . . H3 H 0.2541 0.9211 0.5066 0.057 Uiso 1 1 calc R . . C4 C 0.32267(14) 0.89112(14) 0.41125(17) 0.0483(9) Uani 1 1 d . . . C5 C 0.17092(13) 0.88505(15) 0.46653(18) 0.0539(10) Uani 1 1 d . . . H5A H 0.1480 0.8616 0.4804 0.065 Uiso 1 1 calc R . . H5B H 0.1684 0.9124 0.4934 0.065 Uiso 1 1 calc R . . C6 C 0.26250(14) 0.95178(13) 0.39037(18) 0.0506(10) Uani 1 1 d . . . H6A H 0.2873 0.9637 0.3636 0.061 Uiso 1 1 calc R . . H6B H 0.2558 0.9761 0.4207 0.061 Uiso 1 1 calc R . . C7 C 0.12157(14) 0.88037(16) 0.37479(19) 0.0555(11) Uani 1 1 d . . . C8 C 0.17361(13) 0.94429(13) 0.38156(16) 0.0456(9) Uani 1 1 d . . . H8 H 0.1701 0.9705 0.4109 0.055 Uiso 1 1 calc R . . C9 C 0.13999(13) 0.94983(14) 0.32461(15) 0.0469(9) Uani 1 1 d . . . H9 H 0.1207 0.9788 0.3269 0.056 Uiso 1 1 calc R . . C10 C 0.21964(13) 0.94950(12) 0.29281(17) 0.0440(9) Uani 1 1 d . . . C11 C 0.07003(14) 0.90310(19) 0.29141(17) 0.0677(13) Uani 1 1 d . . . H11A H 0.0544 0.9337 0.2885 0.081 Uiso 1 1 calc R . . H11B H 0.0485 0.8814 0.3120 0.081 Uiso 1 1 calc R . . C12 C 0.15964(14) 0.96695(13) 0.21455(16) 0.0494(10) Uani 1 1 d . . . H12A H 0.1875 0.9797 0.1942 0.059 Uiso 1 1 calc R . . H12B H 0.1367 0.9925 0.2185 0.059 Uiso 1 1 calc R . . C13 C 0.06826(14) 0.84176(17) 0.21132(18) 0.0563(11) Uani 1 1 d . . . C14 C 0.09110(13) 0.91603(15) 0.18007(15) 0.0495(10) Uani 1 1 d . . . H14 H 0.0696 0.9433 0.1778 0.059 Uiso 1 1 calc R . . C15 C 0.08595(13) 0.88361(13) 0.12455(16) 0.0457(9) Uani 1 1 d . . . H15 H 0.0608 0.8948 0.0970 0.055 Uiso 1 1 calc R . . C16 C 0.16175(14) 0.91490(14) 0.12585(16) 0.0453(9) Uani 1 1 d . . . C17 C 0.05180(14) 0.80214(15) 0.1144(2) 0.0606(12) Uani 1 1 d . . . H17A H 0.0304 0.8170 0.0853 0.073 Uiso 1 1 calc R . . H17B H 0.0330 0.7822 0.1414 0.073 Uiso 1 1 calc R . . C18 C 0.14004(15) 0.86997(13) 0.03452(16) 0.0529(10) Uani 1 1 d . . . H18A H 0.1686 0.8852 0.0193 0.064 Uiso 1 1 calc R . . H18B H 0.1138 0.8796 0.0084 0.064 Uiso 1 1 calc R . . C19 C 0.08898(14) 0.72544(16) 0.0904(2) 0.0561(11) Uani 1 1 d . . . C20 C 0.10564(15) 0.78726(13) 0.02471(17) 0.0513(10) Uani 1 1 d . . . H20 H 0.0815 0.8000 -0.0033 0.062 Uiso 1 1 calc R . . C21 C 0.12853(14) 0.74238(14) -0.00054(17) 0.0524(10) Uani 1 1 d . . . H21 H 0.1159 0.7344 -0.0412 0.063 Uiso 1 1 calc R . . C22 C 0.18627(15) 0.79832(15) 0.01232(16) 0.0501(10) Uani 1 1 d . . . C23 C 0.11904(14) 0.65659(14) 0.0336(2) 0.0558(11) Uani 1 1 d . . . H23A H 0.1097 0.6499 -0.0084 0.067 Uiso 1 1 calc R . . H23B H 0.0970 0.6402 0.0605 0.067 Uiso 1 1 calc R . . C24 C 0.21083(16) 0.72505(15) -0.03743(19) 0.0626(12) Uani 1 1 d . . . H24A H 0.1959 0.7141 -0.0750 0.075 Uiso 1 1 calc R . . H24B H 0.2375 0.7451 -0.0488 0.075 Uiso 1 1 calc R . . N1 N 0.27168(12) 0.81522(11) 0.50436(14) 0.0536(8) Uani 1 1 d . . . N2 N 0.21813(11) 0.86523(11) 0.47250(14) 0.0493(8) Uani 1 1 d . . . N3 N 0.33370(11) 0.86180(11) 0.45627(14) 0.0509(8) Uani 1 1 d . . . N4 N 0.27918(11) 0.90993(11) 0.42085(13) 0.0495(8) Uani 1 1 d . . . N5 N 0.15901(11) 0.89892(11) 0.40732(13) 0.0492(8) Uani 1 1 d . . . N6 N 0.11181(11) 0.90812(13) 0.32756(14) 0.0562(9) Uani 1 1 d . . . N7 N 0.21985(10) 0.94298(11) 0.35433(13) 0.0440(8) Uani 1 1 d . . . N8 N 0.17292(11) 0.95119(11) 0.27475(12) 0.0462(8) Uani 1 1 d . . . N9 N 0.07917(12) 0.88535(13) 0.22926(14) 0.0578(9) Uani 1 1 d . . . N10 N 0.07460(11) 0.83842(11) 0.15019(14) 0.0516(8) Uani 1 1 d . . . N11 N 0.13959(11) 0.93028(11) 0.17679(13) 0.0473(8) Uani 1 1 d . . . N12 N 0.13114(11) 0.88589(11) 0.09583(13) 0.0490(8) Uani 1 1 d . . . N13 N 0.08559(11) 0.77263(12) 0.08126(15) 0.0550(9) Uani 1 1 d . . . N14 N 0.11566(11) 0.70683(11) 0.04434(14) 0.0527(8) Uani 1 1 d . . . N15 N 0.14576(11) 0.81873(10) 0.03038(13) 0.0465(8) Uani 1 1 d . . . N16 N 0.17721(11) 0.75295(11) -0.00347(13) 0.0470(8) Uani 1 1 d . . . O1 O 0.19593(11) 0.78938(10) 0.49275(14) 0.0700(9) Uani 1 1 d . . . O2 O 0.10123(11) 0.84347(11) 0.38903(14) 0.0755(9) Uani 1 1 d . . . O3 O 0.05420(13) 0.80909(12) 0.24311(14) 0.0849(10) Uani 1 1 d . . . O4 O 0.07107(11) 0.70369(11) 0.13229(14) 0.0731(9) Uani 1 1 d . . . O5 O 0.34826(10) 0.90078(11) 0.36732(13) 0.0668(8) Uani 1 1 d . . . O6 O 0.25323(10) 0.95288(11) 0.26009(12) 0.0628(8) Uani 1 1 d . . . O7 O 0.20081(10) 0.92563(10) 0.10821(12) 0.0585(7) Uani 1 1 d . . . O8 O 0.22502(11) 0.81794(10) 0.00946(13) 0.0637(8) 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 Cl1 0.096(2) 0.313(6) 0.094(2) 0.000 0.000 -0.120(3) Cl2 0.183(2) 0.136(2) 0.0791(15) 0.0005(17) -0.064(2) 0.011(4) Er1 0.0766(8) 0.0612(7) 0.0800(8) 0.0170(5) -0.0047(6) -0.0031(6) Er2 0.052(2) 0.070(3) 0.067(2) 0.000 0.000 -0.0007(17) O1W 0.115(7) 0.166(9) 0.156(8) 0.012(7) 0.038(6) 0.065(7) O2W 0.289(19) 0.102(9) 0.50(3) -0.026(12) -0.18(2) 0.043(10) C1 0.060(3) 0.043(3) 0.048(2) -0.0067(18) 0.0129(19) -0.005(2) C2 0.055(2) 0.045(2) 0.044(2) -0.0060(17) 0.0002(18) 0.000(2) C3 0.057(3) 0.038(2) 0.047(2) -0.0003(16) 0.0053(18) -0.0008(19) C4 0.050(3) 0.045(2) 0.050(2) -0.0015(19) 0.0017(19) -0.004(2) C5 0.042(2) 0.057(3) 0.063(3) 0.010(2) 0.0106(19) -0.002(2) C6 0.049(2) 0.044(2) 0.059(2) 0.0052(18) -0.0025(19) -0.0061(19) C7 0.047(3) 0.061(3) 0.058(3) -0.008(2) 0.016(2) -0.010(2) C8 0.049(2) 0.042(2) 0.046(2) -0.0046(16) 0.0012(17) -0.0031(19) C9 0.048(2) 0.046(2) 0.047(2) -0.0029(17) 0.0057(17) -0.0009(19) C10 0.040(2) 0.036(2) 0.056(2) -0.0050(17) -0.0008(19) 0.0010(17) C11 0.041(2) 0.115(4) 0.047(2) -0.018(2) 0.0062(18) -0.021(2) C12 0.056(3) 0.044(2) 0.048(2) -0.0016(17) 0.0011(18) -0.002(2) C13 0.037(2) 0.080(3) 0.052(2) 0.006(2) 0.0057(18) -0.001(2) C14 0.042(2) 0.066(3) 0.040(2) -0.0027(19) -0.0011(17) 0.000(2) C15 0.043(2) 0.050(2) 0.044(2) -0.0031(17) -0.0024(17) -0.0033(18) C16 0.043(2) 0.049(2) 0.044(2) 0.0070(17) 0.0005(18) 0.003(2) C17 0.047(3) 0.057(3) 0.077(3) -0.019(2) 0.017(2) -0.010(2) C18 0.071(3) 0.047(2) 0.041(2) -0.0025(17) 0.0010(19) 0.001(2) C19 0.043(2) 0.054(3) 0.071(3) 0.000(2) -0.002(2) -0.006(2) C20 0.062(3) 0.039(2) 0.053(2) -0.0039(17) -0.0060(19) 0.001(2) C21 0.053(3) 0.055(3) 0.050(2) -0.0032(19) -0.0098(18) 0.001(2) C22 0.052(3) 0.052(3) 0.047(2) 0.0122(18) 0.0000(19) 0.000(2) C23 0.045(3) 0.048(3) 0.074(3) -0.005(2) -0.004(2) -0.002(2) C24 0.077(3) 0.055(3) 0.056(2) 0.014(2) 0.014(2) 0.013(2) N1 0.054(2) 0.039(2) 0.068(2) 0.0079(15) 0.0048(17) 0.0015(17) N2 0.051(2) 0.040(2) 0.0568(19) 0.0075(15) 0.0029(15) -0.0037(16) N3 0.0412(19) 0.051(2) 0.060(2) 0.0038(16) 0.0053(15) -0.0018(16) N4 0.046(2) 0.054(2) 0.0486(18) 0.0067(15) 0.0013(14) -0.0022(17) N5 0.045(2) 0.055(2) 0.0480(18) 0.0064(15) 0.0048(15) -0.0070(16) N6 0.045(2) 0.079(3) 0.0444(18) -0.0014(17) 0.0009(15) -0.0208(18) N7 0.0336(18) 0.054(2) 0.0442(17) 0.0022(14) 0.0039(13) -0.0038(15) N8 0.050(2) 0.0496(19) 0.0386(16) -0.0030(13) 0.0057(14) 0.0017(16) N9 0.049(2) 0.076(3) 0.0487(19) -0.0058(18) 0.0023(15) -0.0162(19) N10 0.052(2) 0.047(2) 0.0552(19) -0.0020(15) 0.0126(16) -0.0026(16) N11 0.0413(19) 0.057(2) 0.0437(17) -0.0087(15) 0.0007(14) -0.0026(16) N12 0.049(2) 0.050(2) 0.0474(18) -0.0048(15) 0.0038(15) -0.0045(16) N13 0.052(2) 0.046(2) 0.067(2) 0.0019(16) 0.0106(16) -0.0025(17) N14 0.046(2) 0.052(2) 0.060(2) 0.0066(16) 0.0071(16) 0.0020(16) N15 0.053(2) 0.0351(18) 0.0516(18) -0.0061(14) 0.0065(15) -0.0056(16) N16 0.044(2) 0.043(2) 0.0534(19) -0.0024(14) 0.0052(15) -0.0048(16) O1 0.065(2) 0.0487(18) 0.097(2) 0.0009(15) 0.0202(16) -0.0133(16) O2 0.071(2) 0.079(2) 0.077(2) -0.0020(17) 0.0145(16) -0.0305(18) O3 0.097(3) 0.085(2) 0.072(2) 0.0143(18) 0.0232(18) -0.006(2) O4 0.070(2) 0.062(2) 0.087(2) 0.0155(16) 0.0245(17) -0.0110(16) O5 0.0587(19) 0.078(2) 0.0633(18) 0.0061(15) 0.0122(15) 0.0009(16) O6 0.0468(17) 0.085(2) 0.0568(16) 0.0073(14) 0.0194(14) -0.0038(15) O7 0.0536(19) 0.0656(19) 0.0564(16) -0.0041(13) 0.0112(13) -0.0048(15) O8 0.059(2) 0.0504(18) 0.082(2) 0.0040(14) 0.0118(15) -0.0118(16) _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 Cl1 Cl2 2.211(4) 11_565 ? Cl1 Cl2 2.211(4) 16_665 ? Cl2 Cl2 1.494(5) 11_565 ? Cl2 Cl2 1.494(5) 16_665 ? Cl2 Cl2 2.062(6) 6_464 ? Cl2 Cl1 2.211(4) 11_565 ? Er1 O2W 1.896(16) . ? Er1 O1W 2.370(10) 11_566 ? Er1 O1W 2.381(10) . ? Er1 O3 2.407(3) . ? Er1 O2 2.434(3) . ? Er1 O2W 2.45(2) 16_666 ? Er1 Er1 2.6129(17) 11_566 ? Er1 Er1 2.6129(17) 16_666 ? Er1 O1W 2.785(11) 6_464 ? Er1 Er1 3.308(2) 6_464 ? Er2 O1W 1.608(9) . ? Er2 O1W 1.608(9) 6_464 ? Er2 O3 2.594(4) 6_464 ? Er2 O3 2.594(4) . ? Er2 Er2 3.332(6) 11_566 ? O1W Er1 2.370(10) 16_666 ? O1W Er1 2.785(11) 6_464 ? O2W Er1 2.45(2) 11_566 ? C1 O1 1.229(5) . ? C1 N1 1.348(5) . ? C1 N2 1.349(5) . ? C2 N3 1.454(5) . ? C2 N1 1.455(5) . ? C2 C3 1.553(5) . ? C2 H2 0.9900 . ? C3 N2 1.442(5) . ? C3 N4 1.453(4) . ? C3 H3 0.9900 . ? C4 O5 1.241(4) . ? C4 N3 1.332(5) . ? C4 N4 1.364(5) . ? C5 N5 1.403(5) . ? C5 N2 1.462(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.446(5) . ? C6 N7 1.471(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.239(5) . ? C7 N6 1.334(5) . ? C7 N5 1.387(5) . ? C8 N7 1.446(5) . ? C8 N5 1.469(5) . ? C8 C9 1.584(5) . ? C8 H8 0.9900 . ? C9 N6 1.433(5) . ? C9 N8 1.443(4) . ? C9 H9 0.9900 . ? C10 O6 1.200(4) . ? C10 N7 1.367(5) . ? C10 N8 1.388(5) . ? C11 N6 1.437(5) . ? C11 N9 1.481(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.449(5) . ? C12 N11 1.450(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.230(5) . ? C13 N9 1.337(5) . ? C13 N10 1.361(5) . ? C14 N9 1.431(5) . ? C14 N11 1.439(5) . ? C14 C15 1.538(5) . ? C14 H14 0.9900 . ? C15 N12 1.433(5) . ? C15 N10 1.441(5) . ? C15 H15 0.9900 . ? C16 O7 1.216(4) . ? C16 N11 1.359(5) . ? C16 N12 1.369(5) . ? C17 N10 1.450(5) . ? C17 N13 1.470(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.446(5) . ? C18 N15 1.469(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.221(5) . ? C19 N13 1.361(5) . ? C19 N14 1.373(5) . ? C20 N13 1.431(5) . ? C20 N15 1.455(5) . ? C20 C21 1.537(5) . ? C20 H20 0.9900 . ? C21 N16 1.418(5) . ? C21 N14 1.460(5) . ? C21 H21 0.9900 . ? C22 O8 1.237(5) . ? C22 N15 1.350(5) . ? C22 N16 1.361(5) . ? C23 N14 1.452(5) . ? C23 N3 1.459(5) 13_565 ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N1 1.445(5) 13_565 ? C24 N16 1.450(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? N1 C24 1.445(5) 13_565 ? N3 C23 1.459(5) 13_565 ? 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 Cl2 Cl1 Cl2 55.61(18) 11_565 16_665 ? Cl2 Cl2 Cl2 87.31(8) 11_565 16_665 ? Cl2 Cl2 Cl2 46.34(4) 11_565 6_464 ? Cl2 Cl2 Cl2 46.34(4) 16_665 6_464 ? Cl2 Cl2 Cl1 82.51(15) 11_565 11_565 ? Cl2 Cl2 Cl1 82.51(15) 16_665 11_565 ? Cl2 Cl2 Cl1 62.20(9) 6_464 11_565 ? O2W Er1 O1W 84.4(8) . 11_566 ? O2W Er1 O1W 140.2(6) . . ? O1W Er1 O1W 124.1(4) 11_566 . ? O2W Er1 O3 88.6(7) . . ? O1W Er1 O3 166.4(2) 11_566 . ? O1W Er1 O3 67.9(2) . . ? O2W Er1 O2 75.7(4) . . ? O1W Er1 O2 70.4(2) 11_566 . ? O1W Er1 O2 136.3(3) . . ? O3 Er1 O2 96.57(12) . . ? O2W Er1 O2W 146.3(2) . 16_666 ? O1W Er1 O2W 68.3(5) 11_566 16_666 ? O1W Er1 O2W 73.4(5) . 16_666 ? O3 Er1 O2W 113.7(4) . 16_666 ? O2 Er1 O2W 76.9(4) . 16_666 ? O2W Er1 Er1 63.4(6) . 11_566 ? O1W Er1 Er1 56.8(2) 11_566 11_566 ? O1W Er1 Er1 106.5(3) . 11_566 ? O3 Er1 Er1 129.26(11) . 11_566 ? O2 Er1 Er1 114.14(10) . 11_566 ? O2W Er1 Er1 112.1(4) 16_666 11_566 ? O2W Er1 Er1 141.2(7) . 16_666 ? O1W Er1 Er1 67.8(3) 11_566 16_666 ? O1W Er1 Er1 56.4(2) . 16_666 ? O3 Er1 Er1 123.58(11) . 16_666 ? O2 Er1 Er1 116.27(10) . 16_666 ? O2W Er1 Er1 43.9(3) 16_666 16_666 ? Er1 Er1 Er1 78.55(4) 11_566 16_666 ? O2W Er1 O1W 67.5(5) . 6_464 ? O1W Er1 O1W 108.8(4) 11_566 6_464 ? O1W Er1 O1W 76.4(3) . 6_464 ? O3 Er1 O1W 79.0(2) . 6_464 ? O2 Er1 O1W 143.0(2) . 6_464 ? O2W Er1 O1W 138.8(4) 16_666 6_464 ? Er1 Er1 O1W 52.0(2) 11_566 6_464 ? Er1 Er1 O1W 95.7(2) 16_666 6_464 ? O2W Er1 Er1 104.3(5) . 6_464 ? O1W Er1 Er1 88.1(2) 11_566 6_464 ? O1W Er1 Er1 55.8(3) . 6_464 ? O3 Er1 Er1 104.96(9) . 6_464 ? O2 Er1 Er1 158.47(7) . 6_464 ? O2W Er1 Er1 94.3(3) 16_666 6_464 ? Er1 Er1 Er1 50.73(2) 11_566 6_464 ? Er1 Er1 Er1 50.73(2) 16_666 6_464 ? O1W Er1 Er1 45.0(2) 6_464 6_464 ? O1W Er2 O1W 172.9(7) . 6_464 ? O1W Er2 O3 101.5(4) . 6_464 ? O1W Er2 O3 75.0(4) 6_464 6_464 ? O1W Er2 O3 75.0(4) . . ? O1W Er2 O3 101.5(4) 6_464 . ? O3 Er2 O3 123.06(19) 6_464 . ? O1W Er2 Er2 93.5(4) . 11_566 ? O1W Er2 Er2 93.5(4) 6_464 11_566 ? O3 Er2 Er2 118.47(10) 6_464 11_566 ? O3 Er2 Er2 118.47(10) . 11_566 ? Er2 O1W Er1 86.9(4) . 16_666 ? Er2 O1W Er1 55.4(3) . . ? Er1 O1W Er1 66.7(3) 16_666 . ? Er2 O1W Er1 44.1(3) . 6_464 ? Er1 O1W Er1 60.3(2) 16_666 6_464 ? Er1 O1W Er1 79.2(3) . 6_464 ? Er1 O2W Er1 72.7(7) . 11_566 ? O1 C1 N1 125.4(4) . . ? O1 C1 N2 125.4(4) . . ? N1 C1 N2 109.2(3) . . ? N3 C2 N1 114.5(3) . . ? N3 C2 C3 103.6(3) . . ? N1 C2 C3 103.0(3) . . ? N3 C2 H2 111.7 . . ? N1 C2 H2 111.7 . . ? C3 C2 H2 111.7 . . ? N2 C3 N4 114.5(3) . . ? N2 C3 C2 102.7(3) . . ? N4 C3 C2 102.5(3) . . ? N2 C3 H3 112.1 . . ? N4 C3 H3 112.1 . . ? C2 C3 H3 112.1 . . ? O5 C4 N3 125.4(4) . . ? O5 C4 N4 124.5(4) . . ? N3 C4 N4 110.1(3) . . ? N5 C5 N2 114.4(3) . . ? N5 C5 H5A 108.7 . . ? N2 C5 H5A 108.7 . . ? N5 C5 H5B 108.7 . . ? N2 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N7 112.4(3) . . ? N4 C6 H6A 109.1 . . ? N7 C6 H6A 109.1 . . ? N4 C6 H6B 109.1 . . ? N7 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? O2 C7 N6 127.0(4) . . ? O2 C7 N5 123.4(4) . . ? N6 C7 N5 109.7(4) . . ? N7 C8 N5 113.2(3) . . ? N7 C8 C9 102.9(3) . . ? N5 C8 C9 102.8(3) . . ? N7 C8 H8 112.4 . . ? N5 C8 H8 112.4 . . ? C9 C8 H8 112.4 . . ? N6 C9 N8 114.8(3) . . ? N6 C9 C8 102.7(3) . . ? N8 C9 C8 102.3(3) . . ? N6 C9 H9 112.1 . . ? N8 C9 H9 112.1 . . ? C8 C9 H9 112.1 . . ? O6 C10 N7 127.0(3) . . ? O6 C10 N8 126.0(3) . . ? N7 C10 N8 107.0(3) . . ? N6 C11 N9 113.6(3) . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11B 108.8 . . ? N9 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 113.8(3) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 127.4(4) . . ? O3 C13 N10 123.5(4) . . ? N9 C13 N10 109.0(4) . . ? N9 C14 N11 115.9(3) . . ? N9 C14 C15 102.3(3) . . ? N11 C14 C15 102.7(3) . . ? N9 C14 H14 111.7 . . ? N11 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N12 C15 N10 114.5(3) . . ? N12 C15 C14 103.8(3) . . ? N10 C15 C14 104.2(3) . . ? N12 C15 H15 111.3 . . ? N10 C15 H15 111.3 . . ? C14 C15 H15 111.3 . . ? O7 C16 N11 127.3(4) . . ? O7 C16 N12 125.3(3) . . ? N11 C16 N12 107.3(3) . . ? N10 C17 N13 112.6(3) . . ? N10 C17 H17A 109.1 . . ? N13 C17 H17A 109.1 . . ? N10 C17 H17B 109.1 . . ? N13 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? N12 C18 N15 112.8(3) . . ? N12 C18 H18A 109.0 . . ? N15 C18 H18A 109.0 . . ? N12 C18 H18B 109.0 . . ? N15 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N13 125.6(4) . . ? O4 C19 N14 126.4(4) . . ? N13 C19 N14 108.1(4) . . ? N13 C20 N15 114.6(3) . . ? N13 C20 C21 104.0(3) . . ? N15 C20 C21 102.1(3) . . ? N13 C20 H20 111.8 . . ? N15 C20 H20 111.8 . . ? C21 C20 H20 111.8 . . ? N16 C21 N14 115.0(3) . . ? N16 C21 C20 104.7(3) . . ? N14 C21 C20 103.0(3) . . ? N16 C21 H21 111.2 . . ? N14 C21 H21 111.2 . . ? C20 C21 H21 111.2 . . ? O8 C22 N15 125.6(4) . . ? O8 C22 N16 125.7(4) . . ? N15 C22 N16 108.8(3) . . ? N14 C23 N3 112.9(3) . 13_565 ? N14 C23 H23A 109.0 . . ? N3 C23 H23A 109.0 13_565 . ? N14 C23 H23B 109.0 . . ? N3 C23 H23B 109.0 13_565 . ? H23A C23 H23B 107.8 . . ? N1 C24 N16 113.6(3) 13_565 . ? N1 C24 H24A 108.8 13_565 . ? N16 C24 H24A 108.8 . . ? N1 C24 H24B 108.8 13_565 . ? N16 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C1 N1 C24 122.4(4) . 13_565 ? C1 N1 C2 111.9(3) . . ? C24 N1 C2 122.4(3) 13_565 . ? C1 N2 C3 112.8(3) . . ? C1 N2 C5 122.6(3) . . ? C3 N2 C5 122.0(3) . . ? C4 N3 C2 111.9(3) . . ? C4 N3 C23 123.7(3) . 13_565 ? C2 N3 C23 122.7(3) . 13_565 ? C4 N4 C6 123.2(3) . . ? C4 N4 C3 111.8(3) . . ? C6 N4 C3 121.5(3) . . ? C7 N5 C5 123.9(3) . . ? C7 N5 C8 110.6(3) . . ? C5 N5 C8 122.5(3) . . ? C7 N6 C9 114.1(3) . . ? C7 N6 C11 123.0(4) . . ? C9 N6 C11 121.3(4) . . ? C10 N7 C8 113.8(3) . . ? C10 N7 C6 121.0(3) . . ? C8 N7 C6 121.5(3) . . ? C10 N8 C9 113.7(3) . . ? C10 N8 C12 121.5(3) . . ? C9 N8 C12 122.3(3) . . ? C13 N9 C14 113.4(3) . . ? C13 N9 C11 123.2(4) . . ? C14 N9 C11 122.2(4) . . ? C13 N10 C15 110.8(3) . . ? C13 N10 C17 121.8(3) . . ? C15 N10 C17 121.5(3) . . ? C16 N11 C14 113.3(3) . . ? C16 N11 C12 121.5(3) . . ? C14 N11 C12 123.4(3) . . ? C16 N12 C15 112.6(3) . . ? C16 N12 C18 121.8(3) . . ? C15 N12 C18 123.7(3) . . ? C19 N13 C20 112.8(3) . . ? C19 N13 C17 122.4(3) . . ? C20 N13 C17 121.8(3) . . ? C19 N14 C23 122.5(3) . . ? C19 N14 C21 111.8(3) . . ? C23 N14 C21 123.7(3) . . ? C22 N15 C20 112.3(3) . . ? C22 N15 C18 122.6(3) . . ? C20 N15 C18 121.9(3) . . ? C22 N16 C21 112.0(3) . . ? C22 N16 C24 121.7(3) . . ? C21 N16 C24 123.4(3) . . ? C7 O2 Er1 139.3(3) . . ? C13 O3 Er1 139.8(3) . . ? C13 O3 Er2 162.5(3) . . ? Er1 O3 Er2 46.40(9) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.644 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.068 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.008 -0.004 -0.001 4520 1886 ' ' 2 0.000 0.000 0.500 358 107 ' ' 3 0.000 0.500 0.500 358 107 ' ' 4 0.250 0.250 0.750 358 105 ' ' 5 0.250 0.750 0.250 358 105 ' ' 6 0.500 0.000 0.000 358 107 ' ' 7 0.500 0.500 0.000 358 107 ' ' 8 0.750 0.250 0.750 358 105 ' ' 9 0.750 0.750 0.250 358 105 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952105' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H247 Cl4 N64 O107 Tm' _chemical_formula_weight 4321.31 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' Tm Tm -0.3139 5.2483 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 28.4011(18) _cell_length_b 28.4011(18) _cell_length_c 21.939(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17696(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9056 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8798 _exptl_absorpt_correction_T_max 0.9278 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64026 _diffrn_reflns_av_R_equivalents 0.1117 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8627 _reflns_number_gt 4408 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1603P)^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 8627 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.2711 _refine_ls_wR_factor_gt 0.2448 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.5000 0.7500 -0.27797(10) 0.1610(9) Uani 0.80 2 d SP . . Cl2 Cl 0.49719(7) 0.71175(6) -0.38449(7) 0.1227(6) Uani 0.60 1 d P . . Tm1 Tm 0.45827(2) 0.70945(2) 0.10204(3) 0.04831(17) Uani 0.22 1 d P . 1 Tm1' Tm 0.5000 0.7500 0.1902(7) 0.238(6) Uani 0.06 2 d SP . 2 O1W O 0.4714(2) 0.7012(3) 0.2015(3) 0.146(3) Uani 0.50 1 d P . . O2W O 0.4960(3) 0.6444(2) 0.0935(4) 0.154(3) Uani 0.50 1 d P . . C1 C 0.52497(9) 0.66119(9) -0.15882(13) 0.0445(8) Uani 1 1 d . . . C2 C 0.50823(9) 0.62283(9) -0.25197(12) 0.0429(7) Uani 1 1 d . . . H2 H 0.5159 0.6357 -0.2927 0.051 Uiso 1 1 calc R . . C3 C 0.46316(9) 0.64548(9) -0.22503(12) 0.0415(7) Uani 1 1 d . . . H3 H 0.4500 0.6699 -0.2523 0.050 Uiso 1 1 calc R . . C4 C 0.45209(9) 0.56394(9) -0.23943(11) 0.0383(7) Uani 1 1 d . . . C5 C 0.44898(10) 0.69802(9) -0.13382(14) 0.0526(9) Uani 1 1 d . . . H5A H 0.4694 0.7160 -0.1064 0.063 Uiso 1 1 calc R . . H5B H 0.4343 0.7202 -0.1622 0.063 Uiso 1 1 calc R . . C6 C 0.38083(8) 0.61025(10) -0.21505(12) 0.0402(7) Uani 1 1 d . . . H6A H 0.3714 0.6363 -0.2417 0.048 Uiso 1 1 calc R . . H6B H 0.3656 0.5816 -0.2302 0.048 Uiso 1 1 calc R . . C7 C 0.40879(11) 0.68168(9) -0.03746(13) 0.0512(8) Uani 1 1 d . . . C8 C 0.36659(8) 0.66422(9) -0.12595(12) 0.0366(7) Uani 1 1 d . . . H8 H 0.3559 0.6899 -0.1531 0.044 Uiso 1 1 calc R . . C9 C 0.33397(10) 0.65875(9) -0.06953(11) 0.0407(7) Uani 1 1 d . . . H9 H 0.3067 0.6804 -0.0719 0.049 Uiso 1 1 calc R . . C10 C 0.33488(9) 0.58953(9) -0.12465(12) 0.0414(7) Uani 1 1 d . . . C11 C 0.34673(12) 0.68111(9) 0.04223(12) 0.0566(9) Uani 1 1 d . . . H11A H 0.3689 0.7024 0.0627 0.068 Uiso 1 1 calc R . . H11B H 0.3163 0.6973 0.0391 0.068 Uiso 1 1 calc R . . C12 C 0.28251(8) 0.59070(9) -0.03477(11) 0.0365(7) Uani 1 1 d . . . H12A H 0.2571 0.6138 -0.0304 0.044 Uiso 1 1 calc R . . H12B H 0.2695 0.5629 -0.0551 0.044 Uiso 1 1 calc R . . C13 C 0.36938(10) 0.62841(9) 0.12671(13) 0.0462(8) Uani 1 1 d . . . C14 C 0.29972(9) 0.60887(9) 0.07576(11) 0.0389(7) Uani 1 1 d . . . H14 H 0.2704 0.6276 0.0782 0.047 Uiso 1 1 calc R . . C15 C 0.30540(9) 0.57628(8) 0.13154(12) 0.0362(7) Uani 1 1 d . . . H15 H 0.2791 0.5799 0.1607 0.043 Uiso 1 1 calc R . . C16 C 0.29982(8) 0.53052(9) 0.04349(13) 0.0401(7) Uani 1 1 d . . . C17 C 0.36500(10) 0.57858(9) 0.21943(13) 0.0475(8) Uani 1 1 d . . . H17A H 0.3889 0.6010 0.2335 0.057 Uiso 1 1 calc R . . H17B H 0.3377 0.5814 0.2465 0.057 Uiso 1 1 calc R . . C18 C 0.29763(9) 0.48800(9) 0.14187(12) 0.0435(8) Uani 1 1 d . . . H18A H 0.2739 0.4953 0.1729 0.052 Uiso 1 1 calc R . . H18B H 0.2848 0.4633 0.1155 0.052 Uiso 1 1 calc R . . C19 C 0.42908(9) 0.52316(10) 0.24197(11) 0.0425(7) Uani 1 1 d . . . C20 C 0.35459(9) 0.49006(9) 0.23069(11) 0.0415(7) Uani 1 1 d . . . H20 H 0.3278 0.4952 0.2588 0.050 Uiso 1 1 calc R . . C21 C 0.38900(9) 0.45234(9) 0.25408(12) 0.0398(7) Uani 1 1 d . . . H21 H 0.3795 0.4401 0.2945 0.048 Uiso 1 1 calc R . . C22 C 0.35843(9) 0.42664(9) 0.16124(12) 0.0394(7) Uani 1 1 d . . . C23 C 0.52605(9) 0.53989(10) -0.29020(14) 0.0489(8) Uani 1 1 d . . . H23A H 0.5061 0.5133 -0.3024 0.059 Uiso 1 1 calc R . . H23B H 0.5371 0.5555 -0.3274 0.059 Uiso 1 1 calc R . . C24 C 0.59342(9) 0.63088(9) -0.21696(14) 0.0459(8) Uani 1 1 d . . . H24A H 0.6099 0.6528 -0.1898 0.055 Uiso 1 1 calc R . . H24B H 0.6001 0.6405 -0.2590 0.055 Uiso 1 1 calc R . . N1 N 0.54398(7) 0.63520(7) -0.20646(10) 0.0418(6) Uani 1 1 d . . . N2 N 0.47768(7) 0.66448(8) -0.16837(10) 0.0467(7) Uani 1 1 d . . . N3 N 0.49765(7) 0.57336(7) -0.25452(9) 0.0392(6) Uani 1 1 d . . . N4 N 0.43143(7) 0.60439(7) -0.21933(10) 0.0380(6) Uani 1 1 d . . . N5 N 0.41238(7) 0.67495(8) -0.09812(10) 0.0427(6) Uani 1 1 d . . . N6 N 0.36418(9) 0.67058(7) -0.01922(10) 0.0480(7) Uani 1 1 d . . . N7 N 0.36415(7) 0.61952(7) -0.15534(9) 0.0368(6) Uani 1 1 d . . . N8 N 0.31920(7) 0.61067(7) -0.07279(9) 0.0379(6) Uani 1 1 d . . . N9 N 0.34113(9) 0.63875(7) 0.07862(10) 0.0506(7) Uani 1 1 d . . . N10 N 0.35076(7) 0.59142(7) 0.15819(9) 0.0412(6) Uani 1 1 d . . . N11 N 0.29898(7) 0.57734(7) 0.02531(9) 0.0387(6) Uani 1 1 d . . . N12 N 0.30648(7) 0.53024(7) 0.10518(9) 0.0351(6) Uani 1 1 d . . . N13 N 0.38389(7) 0.53142(7) 0.22447(10) 0.0410(6) Uani 1 1 d . . . N14 N 0.43409(7) 0.47767(8) 0.25703(10) 0.0419(6) Uani 1 1 d . . . N15 N 0.33954(7) 0.47054(7) 0.17160(9) 0.0379(6) Uani 1 1 d . . . N16 N 0.38769(7) 0.41570(7) 0.20764(10) 0.0420(6) Uani 1 1 d . . . O1 O 0.54743(7) 0.67874(7) -0.11754(10) 0.0599(6) Uani 1 1 d . . . O2 O 0.44077(8) 0.69610(8) -0.00544(10) 0.0724(7) Uani 1 1 d . . . O3 O 0.40599(7) 0.64901(7) 0.14143(10) 0.0619(6) Uani 1 1 d . . . O4 O 0.46095(7) 0.55339(7) 0.24333(9) 0.0577(6) Uani 1 1 d . . . O5 O 0.43329(6) 0.52519(6) -0.24220(9) 0.0506(6) Uani 1 1 d . . . O6 O 0.32331(6) 0.54945(6) -0.14273(8) 0.0467(5) Uani 1 1 d . . . O7 O 0.29744(7) 0.49656(6) 0.01044(8) 0.0515(6) Uani 1 1 d . . . O8 O 0.34944(7) 0.40165(6) 0.11769(9) 0.0527(6) 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 Cl1 0.298(2) 0.0942(10) 0.0910(14) 0.000 0.000 -0.1255(13) Cl2 0.1050(11) 0.1857(13) 0.0775(8) 0.0994(9) -0.0210(8) -0.0322(13) Tm1 0.0492(3) 0.0505(3) 0.0452(3) 0.0010(3) -0.0058(3) 0.0029(3) Tm1' 0.130(6) 0.261(11) 0.323(14) 0.000 0.000 -0.029(7) O1W 0.119(4) 0.195(6) 0.126(5) -0.024(5) 0.002(4) -0.095(4) O2W 0.144(5) 0.078(4) 0.241(8) -0.017(5) 0.031(6) 0.030(4) C1 0.0399(14) 0.0428(14) 0.0509(16) 0.0016(13) -0.0068(13) -0.0041(12) C2 0.0490(15) 0.0408(14) 0.0388(15) 0.0049(12) 0.0014(12) -0.0067(13) C3 0.0335(13) 0.0513(15) 0.0398(15) 0.0071(13) 0.0002(12) 0.0017(12) C4 0.0427(14) 0.0415(14) 0.0306(13) 0.0011(11) -0.0100(11) 0.0007(12) C5 0.0542(16) 0.0430(15) 0.0605(18) -0.0162(14) 0.0072(14) -0.0106(13) C6 0.0345(13) 0.0501(15) 0.0360(14) -0.0057(12) -0.0042(11) -0.0013(12) C7 0.0725(19) 0.0380(14) 0.0431(16) -0.0097(13) -0.0078(15) 0.0013(14) C8 0.0363(13) 0.0328(13) 0.0406(14) 0.0013(11) -0.0029(11) -0.0036(11) C9 0.0514(15) 0.0397(14) 0.0310(14) -0.0027(11) -0.0006(12) 0.0055(13) C10 0.0412(14) 0.0482(15) 0.0350(14) -0.0067(12) -0.0057(12) 0.0031(13) C11 0.095(2) 0.0395(15) 0.0358(15) 0.0001(12) 0.0150(15) -0.0141(15) C12 0.0337(13) 0.0403(13) 0.0356(14) -0.0014(11) 0.0013(11) -0.0029(11) C13 0.0482(15) 0.0351(14) 0.0554(17) -0.0074(13) 0.0076(13) -0.0031(12) C14 0.0485(14) 0.0374(13) 0.0309(14) -0.0007(11) 0.0051(12) 0.0073(12) C15 0.0360(13) 0.0367(13) 0.0358(14) -0.0016(11) 0.0045(11) -0.0007(11) C16 0.0229(11) 0.0436(14) 0.0537(16) -0.0041(13) 0.0053(12) -0.0012(11) C17 0.0498(15) 0.0436(15) 0.0490(16) -0.0103(13) -0.0007(13) -0.0038(13) C18 0.0377(14) 0.0485(15) 0.0444(16) -0.0014(13) 0.0012(12) -0.0065(12) C19 0.0438(14) 0.0515(15) 0.0322(14) -0.0136(12) 0.0071(12) -0.0006(13) C20 0.0418(14) 0.0493(15) 0.0334(14) -0.0094(12) 0.0022(12) 0.0021(12) C21 0.0383(13) 0.0498(15) 0.0315(14) 0.0031(12) 0.0039(11) 0.0015(12) C22 0.0371(13) 0.0428(14) 0.0383(14) -0.0009(12) 0.0002(12) -0.0094(12) C23 0.0329(13) 0.0602(17) 0.0536(17) -0.0157(14) -0.0035(13) 0.0000(13) C24 0.0454(15) 0.0357(14) 0.0565(17) -0.0060(13) -0.0023(13) -0.0072(12) N1 0.0401(11) 0.0397(11) 0.0457(13) -0.0020(10) -0.0080(10) 0.0010(10) N2 0.0404(12) 0.0460(12) 0.0538(14) -0.0168(11) -0.0028(11) 0.0004(10) N3 0.0391(11) 0.0400(11) 0.0386(12) -0.0085(10) 0.0016(10) -0.0076(10) N4 0.0298(10) 0.0394(11) 0.0447(12) -0.0019(10) 0.0000(10) -0.0052(9) N5 0.0416(12) 0.0444(12) 0.0423(13) -0.0055(10) 0.0035(10) -0.0045(10) N6 0.0723(15) 0.0382(11) 0.0334(12) -0.0038(10) 0.0020(11) -0.0200(11) N7 0.0351(11) 0.0451(12) 0.0301(11) -0.0073(10) 0.0008(9) -0.0082(10) N8 0.0511(12) 0.0309(10) 0.0318(11) -0.0026(9) 0.0053(10) -0.0043(10) N9 0.0787(15) 0.0382(12) 0.0348(12) -0.0014(10) 0.0056(12) -0.0214(11) N10 0.0443(12) 0.0456(12) 0.0337(12) -0.0006(10) 0.0000(10) -0.0136(10) N11 0.0421(11) 0.0378(11) 0.0362(12) -0.0064(10) 0.0015(10) -0.0042(10) N12 0.0379(11) 0.0416(11) 0.0257(10) 0.0032(9) -0.0031(9) 0.0020(9) N13 0.0393(11) 0.0346(11) 0.0490(13) -0.0002(10) -0.0114(10) -0.0038(10) N14 0.0392(11) 0.0438(12) 0.0425(13) -0.0063(10) -0.0066(10) -0.0040(10) N15 0.0464(12) 0.0357(11) 0.0316(11) -0.0016(9) -0.0035(10) 0.0031(10) N16 0.0420(12) 0.0385(11) 0.0456(13) 0.0025(10) -0.0051(10) -0.0025(10) O1 0.0546(11) 0.0589(12) 0.0662(13) -0.0181(10) -0.0133(10) -0.0128(10) O2 0.0756(14) 0.0872(15) 0.0543(13) -0.0190(11) -0.0161(11) -0.0136(12) O3 0.0615(12) 0.0593(12) 0.0650(14) -0.0078(11) -0.0011(11) -0.0249(10) O4 0.0497(11) 0.0483(11) 0.0749(14) -0.0113(10) 0.0059(10) -0.0079(10) O5 0.0491(10) 0.0432(10) 0.0595(12) -0.0132(9) 0.0023(9) -0.0138(9) O6 0.0523(10) 0.0412(10) 0.0467(11) -0.0102(8) 0.0054(9) -0.0104(9) O7 0.0724(12) 0.0435(10) 0.0386(10) -0.0160(9) -0.0005(9) -0.0082(10) O8 0.0643(12) 0.0445(10) 0.0493(11) -0.0115(9) -0.0083(10) 0.0056(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 Cl1 Cl2 2.208(3) 15_564 ? Cl1 Cl2 2.208(3) 12_765 ? Cl2 Cl2 1.596(3) 15_564 ? Cl2 Cl2 1.596(3) 12_765 ? Cl2 Cl2 2.178(4) 6_564 ? Cl2 Cl1 2.208(3) 15_564 ? Tm1 O2W 2.142(6) . ? Tm1 O1W 2.226(7) . ? Tm1 O1W 2.298(6) 15_565 ? Tm1 O3 2.429(2) . ? Tm1 O2 2.440(2) . ? Tm1 O2W 2.513(7) 15_565 ? Tm1 Tm1 2.5450(9) 15_565 ? Tm1 Tm1 2.5450(9) 12_766 ? Tm1 O1W 2.846(8) 12_766 ? Tm1 Tm1 3.3051(12) 6_564 ? Tm1' O1W 1.625(7) 6_564 ? Tm1' O1W 1.625(7) . ? Tm1' O2 2.687(8) 15_565 ? Tm1' O2 2.687(8) 12_766 ? Tm1' Tm1' 2.86(3) 15_565 ? O1W Tm1 2.298(6) 12_766 ? O1W Tm1 2.846(8) 15_565 ? O2W Tm1 2.513(7) 12_766 ? C1 O1 1.215(3) . ? C1 N2 1.363(3) . ? C1 N1 1.389(3) . ? C2 N3 1.438(3) . ? C2 N1 1.467(3) . ? C2 C3 1.550(4) . ? C2 H2 0.9900 . ? C3 N2 1.417(3) . ? C3 N4 1.480(3) . ? C3 H3 0.9900 . ? C4 O5 1.225(3) . ? C4 N3 1.362(3) . ? C4 N4 1.363(3) . ? C5 N5 1.457(4) . ? C5 N2 1.465(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.418(3) . ? C6 N4 1.450(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.219(4) . ? C7 N5 1.348(4) . ? C7 N6 1.366(4) . ? C8 N7 1.425(3) . ? C8 N5 1.469(3) . ? C8 C9 1.554(4) . ? C8 H8 0.9900 . ? C9 N8 1.430(3) . ? C9 N6 1.438(3) . ? C9 H9 0.9900 . ? C10 O6 1.249(3) . ? C10 N8 1.361(3) . ? C10 N7 1.368(3) . ? C11 N9 1.452(3) . ? C11 N6 1.467(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.449(3) . ? C12 N8 1.450(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.236(3) . ? C13 N9 1.358(4) . ? C13 N10 1.364(3) . ? C14 N11 1.424(3) . ? C14 N9 1.452(3) . ? C14 C15 1.543(3) . ? C14 H14 0.9900 . ? C15 N12 1.430(3) . ? C15 N10 1.479(3) . ? C15 H15 0.9900 . ? C16 O7 1.208(3) . ? C16 N12 1.367(3) . ? C16 N11 1.389(3) . ? C17 N13 1.447(3) . ? C17 N10 1.450(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.445(3) . ? C18 N12 1.467(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.248(3) . ? C19 N14 1.341(3) . ? C19 N13 1.360(3) . ? C20 N13 1.446(3) . ? C20 N15 1.473(3) . ? C20 C21 1.538(4) . ? C20 H20 0.9900 . ? C21 N16 1.457(3) . ? C21 N14 1.470(3) . ? C21 H21 0.9900 . ? C22 O8 1.217(3) . ? C22 N16 1.350(3) . ? C22 N15 1.376(3) . ? C23 N14 1.435(3) 9_665 ? C23 N3 1.472(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N1 1.428(3) . ? C24 N16 1.442(3) 9_665 ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? N14 C23 1.435(3) 9_665 ? N16 C24 1.442(3) 9_665 ? O2 Tm1' 2.687(8) 15_565 ? 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 Cl2 Cl1 Cl2 59.12(11) 15_564 12_765 ? Cl2 Cl2 Cl2 86.10(5) 15_564 12_765 ? Cl2 Cl2 Cl2 46.95(3) 15_564 6_564 ? Cl2 Cl2 Cl2 46.95(3) 12_765 6_564 ? Cl2 Cl2 Cl1 83.69(10) 15_564 15_564 ? Cl2 Cl2 Cl1 83.69(10) 12_765 15_564 ? Cl2 Cl2 Cl1 60.44(6) 6_564 15_564 ? O2W Tm1 O1W 84.9(3) . . ? O2W Tm1 O1W 137.4(3) . 15_565 ? O1W Tm1 O1W 127.3(3) . 15_565 ? O2W Tm1 O3 74.2(2) . . ? O1W Tm1 O3 71.29(17) . . ? O1W Tm1 O3 137.1(2) 15_565 . ? O2W Tm1 O2 83.3(3) . . ? O1W Tm1 O2 164.9(2) . . ? O1W Tm1 O2 67.72(18) 15_565 . ? O3 Tm1 O2 96.29(8) . . ? O2W Tm1 O2W 146.73(12) . 15_565 ? O1W Tm1 O2W 73.0(3) . 15_565 ? O1W Tm1 O2W 75.5(3) 15_565 15_565 ? O3 Tm1 O2W 75.28(16) . 15_565 ? O2 Tm1 O2W 113.0(2) . 15_565 ? O2W Tm1 Tm1 145.0(2) . 15_565 ? O1W Tm1 Tm1 72.90(19) . 15_565 ? O1W Tm1 Tm1 54.45(17) 15_565 15_565 ? O3 Tm1 Tm1 121.07(6) . 15_565 ? O2 Tm1 Tm1 121.87(7) . 15_565 ? O2W Tm1 Tm1 50.11(16) 15_565 15_565 ? O2W Tm1 Tm1 64.2(2) . 12_766 ? O1W Tm1 Tm1 57.11(16) . 12_766 ? O1W Tm1 Tm1 107.08(19) 15_565 12_766 ? O3 Tm1 Tm1 114.28(6) . 12_766 ? O2 Tm1 Tm1 124.59(6) . 12_766 ? O2W Tm1 Tm1 118.74(19) 15_565 12_766 ? Tm1 Tm1 Tm1 80.983(19) 15_565 12_766 ? O2W Tm1 O1W 67.4(2) . 12_766 ? O1W Tm1 O1W 105.4(2) . 12_766 ? O1W Tm1 O1W 76.5(3) 15_565 12_766 ? O3 Tm1 O1W 141.55(13) . 12_766 ? O2 Tm1 O1W 78.67(15) . 12_766 ? O2W Tm1 O1W 142.0(2) 15_565 12_766 ? Tm1 Tm1 O1W 92.42(13) 15_565 12_766 ? Tm1 Tm1 O1W 48.38(14) 12_766 12_766 ? O2W Tm1 Tm1 104.02(19) . 6_564 ? O1W Tm1 Tm1 87.32(16) . 6_564 ? O1W Tm1 Tm1 57.77(19) 15_565 6_564 ? O3 Tm1 Tm1 158.60(5) . 6_564 ? O2 Tm1 Tm1 104.74(6) . 6_564 ? O2W Tm1 Tm1 99.56(15) 15_565 6_564 ? Tm1 Tm1 Tm1 49.508(10) 15_565 6_564 ? Tm1 Tm1 Tm1 49.508(10) 12_766 6_564 ? O1W Tm1 Tm1 43.07(13) 12_766 6_564 ? O1W Tm1' O1W 162.4(11) 6_564 . ? O1W Tm1' O2 70.7(4) 6_564 15_565 ? O1W Tm1' O2 99.6(5) . 15_565 ? O1W Tm1' O2 99.6(5) 6_564 12_766 ? O1W Tm1' O2 70.7(4) . 12_766 ? O2 Tm1' O2 115.6(5) 15_565 12_766 ? O1W Tm1' Tm1' 98.8(6) 6_564 15_565 ? O1W Tm1' Tm1' 98.8(6) . 15_565 ? O2 Tm1' Tm1' 122.2(3) 15_565 15_565 ? O2 Tm1' Tm1' 122.2(3) 12_766 15_565 ? Tm1' O1W Tm1 81.1(6) . . ? Tm1' O1W Tm1 54.6(3) . 12_766 ? Tm1 O1W Tm1 68.4(2) . 12_766 ? Tm1' O1W Tm1 39.4(3) . 15_565 ? Tm1 O1W Tm1 58.71(17) . 15_565 ? Tm1 O1W Tm1 79.2(2) 12_766 15_565 ? Tm1 O2W Tm1 65.71(18) . 12_766 ? O1 C1 N2 127.2(3) . . ? O1 C1 N1 125.1(2) . . ? N2 C1 N1 107.7(2) . . ? N3 C2 N1 113.9(2) . . ? N3 C2 C3 104.3(2) . . ? N1 C2 C3 102.3(2) . . ? N3 C2 H2 111.9 . . ? N1 C2 H2 111.9 . . ? C3 C2 H2 111.9 . . ? N2 C3 N4 113.8(2) . . ? N2 C3 C2 104.6(2) . . ? N4 C3 C2 102.0(2) . . ? N2 C3 H3 111.9 . . ? N4 C3 H3 111.9 . . ? C2 C3 H3 111.9 . . ? O5 C4 N3 125.4(2) . . ? O5 C4 N4 125.9(2) . . ? N3 C4 N4 108.8(2) . . ? N5 C5 N2 112.5(2) . . ? N5 C5 H5A 109.1 . . ? N2 C5 H5A 109.1 . . ? N5 C5 H5B 109.1 . . ? N2 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N7 C6 N4 114.4(2) . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6B 108.7 . . ? N4 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 124.1(3) . . ? O2 C7 N6 126.9(3) . . ? N5 C7 N6 109.1(2) . . ? N7 C8 N5 114.6(2) . . ? N7 C8 C9 104.02(19) . . ? N5 C8 C9 102.6(2) . . ? N7 C8 H8 111.7 . . ? N5 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N8 C9 N6 115.9(2) . . ? N8 C9 C8 103.33(19) . . ? N6 C9 C8 103.4(2) . . ? N8 C9 H9 111.2 . . ? N6 C9 H9 111.2 . . ? C8 C9 H9 111.2 . . ? O6 C10 N8 125.5(2) . . ? O6 C10 N7 124.8(2) . . ? N8 C10 N7 109.6(2) . . ? N9 C11 N6 111.9(2) . . ? N9 C11 H11A 109.2 . . ? N6 C11 H11A 109.2 . . ? N9 C11 H11B 109.2 . . ? N6 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N11 C12 N8 113.17(19) . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? N8 C12 H12B 108.9 . . ? H12A C12 H12B 107.8 . . ? O3 C13 N9 126.7(3) . . ? O3 C13 N10 123.9(3) . . ? N9 C13 N10 109.3(2) . . ? N11 C14 N9 114.4(2) . . ? N11 C14 C15 103.93(19) . . ? N9 C14 C15 103.4(2) . . ? N11 C14 H14 111.5 . . ? N9 C14 H14 111.5 . . ? C15 C14 H14 111.5 . . ? N12 C15 N10 114.0(2) . . ? N12 C15 C14 103.29(19) . . ? N10 C15 C14 103.31(19) . . ? N12 C15 H15 111.9 . . ? N10 C15 H15 111.9 . . ? C14 C15 H15 111.9 . . ? O7 C16 N12 126.7(2) . . ? O7 C16 N11 126.2(2) . . ? N12 C16 N11 107.0(2) . . ? N13 C17 N10 114.0(2) . . ? N13 C17 H17A 108.7 . . ? N10 C17 H17A 108.7 . . ? N13 C17 H17B 108.7 . . ? N10 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N15 C18 N12 112.8(2) . . ? N15 C18 H18A 109.0 . . ? N12 C18 H18A 109.0 . . ? N15 C18 H18B 109.0 . . ? N12 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N14 125.5(2) . . ? O4 C19 N13 124.9(2) . . ? N14 C19 N13 109.6(2) . . ? N13 C20 N15 112.9(2) . . ? N13 C20 C21 103.4(2) . . ? N15 C20 C21 102.5(2) . . ? N13 C20 H20 112.4 . . ? N15 C20 H20 112.4 . . ? C21 C20 H20 112.4 . . ? N16 C21 N14 113.7(2) . . ? N16 C21 C20 104.4(2) . . ? N14 C21 C20 103.1(2) . . ? N16 C21 H21 111.7 . . ? N14 C21 H21 111.7 . . ? C20 C21 H21 111.7 . . ? O8 C22 N16 125.9(2) . . ? O8 C22 N15 125.2(2) . . ? N16 C22 N15 108.9(2) . . ? N14 C23 N3 112.8(2) 9_665 . ? N14 C23 H23A 109.0 9_665 . ? N3 C23 H23A 109.0 . . ? N14 C23 H23B 109.0 9_665 . ? N3 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N1 C24 N16 115.0(2) . 9_665 ? N1 C24 H24A 108.5 . . ? N16 C24 H24A 108.5 9_665 . ? N1 C24 H24B 108.5 . . ? N16 C24 H24B 108.5 9_665 . ? H24A C24 H24B 107.5 . . ? C1 N1 C24 123.3(2) . . ? C1 N1 C2 111.7(2) . . ? C24 N1 C2 123.4(2) . . ? C1 N2 C3 113.3(2) . . ? C1 N2 C5 120.9(2) . . ? C3 N2 C5 122.7(2) . . ? C4 N3 C2 112.4(2) . . ? C4 N3 C23 121.5(2) . . ? C2 N3 C23 122.5(2) . . ? C4 N4 C6 123.0(2) . . ? C4 N4 C3 112.04(19) . . ? C6 N4 C3 121.2(2) . . ? C7 N5 C5 121.4(2) . . ? C7 N5 C8 111.9(2) . . ? C5 N5 C8 120.1(2) . . ? C7 N6 C9 112.5(2) . . ? C7 N6 C11 122.4(2) . . ? C9 N6 C11 123.5(2) . . ? C10 N7 C6 122.8(2) . . ? C10 N7 C8 111.2(2) . . ? C6 N7 C8 124.5(2) . . ? C10 N8 C9 111.5(2) . . ? C10 N8 C12 122.9(2) . . ? C9 N8 C12 123.7(2) . . ? C13 N9 C14 112.7(2) . . ? C13 N9 C11 122.8(2) . . ? C14 N9 C11 123.3(2) . . ? C13 N10 C17 123.7(2) . . ? C13 N10 C15 111.2(2) . . ? C17 N10 C15 122.4(2) . . ? C16 N11 C14 112.3(2) . . ? C16 N11 C12 121.2(2) . . ? C14 N11 C12 123.2(2) . . ? C16 N12 C15 113.1(2) . . ? C16 N12 C18 121.6(2) . . ? C15 N12 C18 121.5(2) . . ? C19 N13 C20 112.1(2) . . ? C19 N13 C17 122.1(2) . . ? C20 N13 C17 123.1(2) . . ? C19 N14 C23 122.9(2) . 9_665 ? C19 N14 C21 111.6(2) . . ? C23 N14 C21 122.6(2) 9_665 . ? C22 N15 C18 123.9(2) . . ? C22 N15 C20 111.9(2) . . ? C18 N15 C20 120.5(2) . . ? C22 N16 C24 123.1(2) . 9_665 ? C22 N16 C21 112.3(2) . . ? C24 N16 C21 123.1(2) 9_665 . ? C7 O2 Tm1 139.6(2) . . ? C7 O2 Tm1' 164.7(2) . 15_565 ? Tm1 O2 Tm1' 43.0(3) . 15_565 ? C13 O3 Tm1 139.10(19) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.979 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.088 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.008 -0.003 -0.004 4451 1881 ' ' 2 0.000 0.000 0.500 361 117 ' ' 3 0.000 0.500 0.500 361 116 ' ' 4 0.043 0.343 0.760 9 2 ' ' 5 0.043 0.843 0.240 9 2 ' ' 6 0.093 0.208 0.490 9 2 ' ' 7 0.093 0.708 0.510 9 2 ' ' 8 0.250 0.250 0.750 361 116 ' ' 9 0.250 0.750 0.250 361 116 ' ' 10 0.500 0.000 0.000 361 116 ' ' 11 0.500 0.500 1.000 361 117 ' ' 12 0.406 0.292 0.010 9 3 ' ' 13 0.406 0.792 0.990 9 3 ' ' 14 0.458 0.157 0.740 9 3 ' ' 15 0.458 0.657 0.260 9 3 ' ' 16 0.543 0.343 0.740 9 2 ' ' 17 0.543 0.843 0.260 9 2 ' ' 18 0.593 0.208 0.010 9 2 ' ' 19 0.593 0.708 0.990 9 2 ' ' 20 0.750 0.250 0.750 361 116 ' ' 21 0.750 0.750 0.250 361 116 ' ' 22 0.906 0.292 0.490 9 3 ' ' 23 0.906 0.792 0.510 9 3 ' ' 24 0.958 0.157 0.760 9 3 ' ' 25 0.958 0.657 0.240 9 3 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952106' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H237 Cl4 N64 O102 Yb' _chemical_formula_weight 4235.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 28.388(3) _cell_length_b 28.388(3) _cell_length_c 22.036(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17758(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8860 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8590 _exptl_absorpt_correction_T_max 0.9131 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64779 _diffrn_reflns_av_R_equivalents 0.1019 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8683 _reflns_number_gt 4065 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1769P)^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 8683 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1579 _refine_ls_R_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.2945 _refine_ls_wR_factor_gt 0.2612 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _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 Cl1 Cl 1.0000 0.2500 -0.27900(19) 0.191(3) Uani 0.80 2 d SP . . Cl2 Cl 0.99926(19) 0.28590(13) -0.38227(14) 0.1216(14) Uani 0.60 1 d P . . Yb1 Yb 0.95967(5) 0.29148(5) 0.09938(6) 0.0701(4) Uani 0.20 1 d P . . Yb1' Yb 1.0000 0.2500 0.0528(7) 0.250(5) Uani 0.10 2 d SP . . O1W O 0.9676(6) 0.2978(6) 0.2048(9) 0.219(8) Uani 0.50 1 d P . . O2W O 0.9949(6) 0.3550(7) 0.0914(10) 0.231(8) Uani 0.50 1 d P . . C1 C 0.92920(18) 0.47659(19) 0.2409(2) 0.0529(13) Uani 1 1 d . . . C2 C 0.88968(17) 0.54740(17) 0.2527(2) 0.0519(12) Uani 1 1 d . . . H2 H 0.8800 0.5593 0.2930 0.062 Uiso 1 1 calc R . . C3 C 0.85526(17) 0.50974(17) 0.2288(2) 0.0515(12) Uani 1 1 d . . . H3 H 0.8285 0.5046 0.2568 0.062 Uiso 1 1 calc R . . C4 C 0.85842(17) 0.57352(17) 0.1611(2) 0.0473(11) Uani 1 1 d . . . C5 C 0.86519(18) 0.42035(17) 0.2177(2) 0.0563(13) Uani 1 1 d . . . H5A H 0.8890 0.3976 0.2311 0.068 Uiso 1 1 calc R . . H5B H 0.8380 0.4175 0.2449 0.068 Uiso 1 1 calc R . . C6 C 0.79760(17) 0.51202(17) 0.1417(2) 0.0558(13) Uani 1 1 d . . . H6A H 0.7848 0.5369 0.1156 0.067 Uiso 1 1 calc R . . H6B H 0.7740 0.5047 0.1727 0.067 Uiso 1 1 calc R . . C7 C 0.86902(19) 0.37144(17) 0.1261(2) 0.0548(13) Uani 1 1 d . . . C8 C 0.80587(15) 0.42345(15) 0.13107(19) 0.0420(11) Uani 1 1 d . . . H8 H 0.7797 0.4199 0.1604 0.050 Uiso 1 1 calc R . . C9 C 0.79953(17) 0.39060(15) 0.07523(19) 0.0458(11) Uani 1 1 d . . . H9 H 0.7703 0.3716 0.0781 0.055 Uiso 1 1 calc R . . C10 C 0.79977(15) 0.46946(17) 0.0426(2) 0.0458(11) Uani 1 1 d . . . C11 C 0.8472(2) 0.31930(17) 0.0416(2) 0.0657(15) Uani 1 1 d . . . H11A H 0.8167 0.3032 0.0392 0.079 Uiso 1 1 calc R . . H11B H 0.8693 0.2980 0.0618 0.079 Uiso 1 1 calc R . . C12 C 0.78268(16) 0.40943(16) -0.0345(2) 0.0477(11) Uani 1 1 d . . . H12A H 0.7697 0.4373 -0.0547 0.057 Uiso 1 1 calc R . . H12B H 0.7573 0.3862 -0.0309 0.057 Uiso 1 1 calc R . . C13 C 0.9089(2) 0.31782(17) -0.0386(2) 0.0553(13) Uani 1 1 d . . . C14 C 0.83342(18) 0.34067(16) -0.0701(2) 0.0497(12) Uani 1 1 d . . . H14 H 0.8059 0.3193 -0.0723 0.060 Uiso 1 1 calc R . . C15 C 0.86590(16) 0.33551(16) -0.1255(2) 0.0468(11) Uani 1 1 d . . . H15 H 0.8549 0.3101 -0.1529 0.056 Uiso 1 1 calc R . . C16 C 0.83518(17) 0.41095(17) -0.1241(2) 0.0481(11) Uani 1 1 d . . . C17 C 0.94797(18) 0.30150(17) -0.1351(2) 0.0596(14) Uani 1 1 d . . . H17A H 0.9330 0.2800 -0.1640 0.072 Uiso 1 1 calc R . . H17B H 0.9682 0.2828 -0.1084 0.072 Uiso 1 1 calc R . . C18 C 0.87986(16) 0.38951(18) -0.2148(2) 0.0504(12) Uani 1 1 d . . . H18A H 0.8646 0.4182 -0.2298 0.060 Uiso 1 1 calc R . . H18B H 0.8701 0.3633 -0.2409 0.060 Uiso 1 1 calc R . . C19 C 1.02502(19) 0.33897(18) -0.1590(3) 0.0604(14) Uani 1 1 d . . . C20 C 0.96324(16) 0.35449(17) -0.2255(2) 0.0495(12) Uani 1 1 d . . . H20 H 0.9504 0.3301 -0.2531 0.059 Uiso 1 1 calc R . . C21 C 1.00771(18) 0.37715(18) -0.2510(2) 0.0559(13) Uani 1 1 d . . . H21 H 1.0156 0.3643 -0.2916 0.067 Uiso 1 1 calc R . . C22 C 0.95239(17) 0.43592(17) -0.2389(2) 0.0470(12) Uani 1 1 d . . . C23 C 1.09337(16) 0.36898(16) -0.2177(3) 0.0552(13) Uani 1 1 d . . . H23A H 1.0994 0.3605 -0.2601 0.066 Uiso 1 1 calc R . . H23B H 1.1102 0.3463 -0.1921 0.066 Uiso 1 1 calc R . . C24 C 1.02525(17) 0.4607(2) -0.2884(3) 0.0656(15) Uani 1 1 d . . . H24A H 1.0360 0.4458 -0.3261 0.079 Uiso 1 1 calc R . . H24B H 1.0052 0.4875 -0.2995 0.079 Uiso 1 1 calc R . . N1 N 0.93418(14) 0.52200(15) 0.25571(18) 0.0530(10) Uani 1 1 d . . . N2 N 0.88466(13) 0.46807(13) 0.22289(18) 0.0501(10) Uani 1 1 d . . . N3 N 0.88750(13) 0.58424(13) 0.20666(18) 0.0521(10) Uani 1 1 d . . . N4 N 0.84008(14) 0.52883(13) 0.17065(16) 0.0497(10) Uani 1 1 d . . . N5 N 0.85073(13) 0.40864(14) 0.15704(17) 0.0501(10) Uani 1 1 d . . . N6 N 0.84198(16) 0.36101(14) 0.07767(18) 0.0606(12) Uani 1 1 d . . . N7 N 0.80678(13) 0.46960(12) 0.10494(16) 0.0444(9) Uani 1 1 d . . . N8 N 0.79816(13) 0.42254(13) 0.02541(16) 0.0481(10) Uani 1 1 d . . . N9 N 0.86423(16) 0.32888(14) -0.02036(17) 0.0562(11) Uani 1 1 d . . . N10 N 0.91155(13) 0.32420(14) -0.09869(18) 0.0513(10) Uani 1 1 d . . . N11 N 0.81969(13) 0.38982(13) -0.07220(16) 0.0487(10) Uani 1 1 d . . . N12 N 0.86407(14) 0.38059(14) -0.15451(17) 0.0499(10) Uani 1 1 d . . . N13 N 0.97711(14) 0.33525(15) -0.16858(19) 0.0595(11) Uani 1 1 d . . . N14 N 1.04340(14) 0.36460(13) -0.20594(18) 0.0538(10) Uani 1 1 d . . . N15 N 0.93119(13) 0.39524(13) -0.21949(17) 0.0479(9) Uani 1 1 d . . . N16 N 0.99685(13) 0.42654(14) -0.25410(17) 0.0494(10) Uani 1 1 d . . . O1 O 0.96085(13) 0.44619(13) 0.24313(18) 0.0707(11) Uani 1 1 d . . . O2 O 0.90648(14) 0.35066(13) 0.13981(18) 0.0773(12) Uani 1 1 d . . . O3 O 0.94110(15) 0.30349(16) -0.00630(19) 0.0874(13) Uani 1 1 d . . . O4 O 1.04722(13) 0.32100(13) -0.11783(18) 0.0719(11) Uani 1 1 d . . . O5 O 0.84902(13) 0.59879(12) 0.11753(17) 0.0688(10) Uani 1 1 d . . . O6 O 0.79680(14) 0.50321(11) 0.01081(15) 0.0630(10) Uani 1 1 d . . . O7 O 0.82408(13) 0.45044(12) -0.14183(16) 0.0629(9) Uani 1 1 d . . . O8 O 0.93248(12) 0.47472(13) -0.24084(16) 0.0651(10) 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 Cl1 0.362(8) 0.110(3) 0.102(3) 0.000 0.000 0.138(4) Cl2 0.123(2) 0.177(3) 0.0651(17) -0.059(2) 0.0007(19) -0.017(4) Yb1 0.0615(8) 0.0755(9) 0.0734(8) -0.0052(7) -0.0125(6) -0.0013(7) Yb1' 0.269(14) 0.160(8) 0.321(16) 0.000 0.000 0.017(9) O1W 0.202(15) 0.203(15) 0.251(19) -0.010(13) -0.079(14) 0.134(13) O2W 0.160(14) 0.208(17) 0.33(2) -0.028(16) -0.016(14) -0.078(13) C1 0.049(3) 0.059(4) 0.051(3) 0.014(2) 0.011(2) -0.006(3) C2 0.052(3) 0.059(3) 0.045(3) 0.008(2) 0.013(2) 0.001(2) C3 0.050(3) 0.056(3) 0.049(3) 0.008(2) -0.001(2) -0.001(2) C4 0.047(3) 0.042(3) 0.053(3) 0.003(2) 0.005(2) 0.009(2) C5 0.051(3) 0.048(3) 0.070(3) 0.007(2) -0.002(2) 0.000(2) C6 0.050(3) 0.053(3) 0.065(3) 0.006(2) -0.007(2) 0.003(2) C7 0.059(3) 0.050(3) 0.055(3) 0.011(2) 0.007(3) 0.007(3) C8 0.045(3) 0.043(3) 0.038(2) 0.0021(19) 0.0013(19) -0.002(2) C9 0.048(3) 0.042(3) 0.047(3) 0.005(2) -0.001(2) -0.005(2) C10 0.032(2) 0.049(3) 0.057(3) 0.005(2) 0.004(2) 0.007(2) C11 0.105(4) 0.041(3) 0.052(3) 0.001(2) 0.015(3) 0.016(3) C12 0.052(3) 0.042(3) 0.049(3) 0.004(2) -0.001(2) 0.005(2) C13 0.066(4) 0.041(3) 0.059(3) 0.011(2) -0.008(3) -0.002(2) C14 0.058(3) 0.040(3) 0.051(3) 0.008(2) 0.008(2) 0.001(2) C15 0.054(3) 0.034(2) 0.053(3) 0.001(2) 0.001(2) 0.002(2) C16 0.052(3) 0.044(3) 0.048(3) 0.004(2) -0.011(2) 0.006(2) C17 0.059(3) 0.050(3) 0.070(3) 0.017(3) 0.009(3) 0.007(3) C18 0.045(3) 0.063(3) 0.043(3) 0.002(2) 0.002(2) -0.001(2) C19 0.055(3) 0.051(3) 0.075(4) 0.009(3) -0.010(3) 0.003(3) C20 0.040(3) 0.061(3) 0.047(3) -0.008(2) 0.002(2) -0.002(2) C21 0.059(3) 0.051(3) 0.057(3) -0.009(2) 0.007(2) 0.007(3) C22 0.051(3) 0.038(3) 0.052(3) -0.004(2) -0.012(2) 0.005(2) C23 0.044(3) 0.040(3) 0.081(4) 0.004(2) 0.006(2) 0.003(2) C24 0.044(3) 0.082(4) 0.070(3) 0.022(3) -0.011(3) -0.006(3) N1 0.046(2) 0.051(3) 0.063(3) 0.011(2) -0.0038(19) 0.004(2) N2 0.041(2) 0.049(2) 0.061(2) 0.0015(19) -0.0084(18) 0.0018(19) N3 0.046(2) 0.047(2) 0.063(3) 0.000(2) -0.001(2) 0.0003(19) N4 0.055(3) 0.051(3) 0.042(2) 0.0048(17) -0.0059(18) -0.001(2) N5 0.050(2) 0.053(3) 0.048(2) 0.0037(19) -0.0009(18) 0.0087(19) N6 0.081(3) 0.051(3) 0.049(2) 0.004(2) 0.004(2) 0.020(2) N7 0.045(2) 0.041(2) 0.047(2) -0.0034(17) 0.0004(17) 0.0036(17) N8 0.053(2) 0.048(2) 0.043(2) 0.0051(18) 0.0035(17) 0.0038(19) N9 0.083(3) 0.043(2) 0.043(2) 0.0057(18) 0.001(2) 0.010(2) N10 0.045(2) 0.051(2) 0.057(2) 0.0065(19) -0.0038(19) 0.0000(19) N11 0.055(2) 0.047(2) 0.045(2) 0.0058(18) 0.0048(18) 0.0081(19) N12 0.051(2) 0.053(2) 0.045(2) 0.0050(18) 0.0064(18) 0.0047(19) N13 0.046(3) 0.057(3) 0.076(3) 0.016(2) -0.003(2) -0.001(2) N14 0.050(2) 0.044(2) 0.067(3) 0.010(2) -0.010(2) 0.0024(19) N15 0.046(2) 0.043(2) 0.055(2) 0.0050(18) 0.0012(18) 0.0075(18) N16 0.038(2) 0.049(2) 0.061(2) 0.0086(19) 0.0004(18) 0.0043(18) O1 0.057(2) 0.060(2) 0.095(3) 0.014(2) -0.0008(19) 0.0121(19) O2 0.080(3) 0.068(3) 0.084(3) 0.014(2) -0.001(2) 0.030(2) O3 0.080(3) 0.099(3) 0.082(3) 0.021(2) -0.016(2) 0.006(2) O4 0.064(2) 0.061(2) 0.090(3) 0.020(2) -0.013(2) 0.0090(19) O5 0.080(3) 0.054(2) 0.072(2) 0.0217(19) -0.006(2) -0.0057(19) O6 0.095(3) 0.043(2) 0.0507(19) 0.0171(16) -0.0053(18) 0.0078(18) O7 0.070(2) 0.051(2) 0.067(2) 0.0129(17) 0.0108(18) 0.0047(18) O8 0.055(2) 0.063(2) 0.077(3) 0.0124(19) 0.0007(18) 0.0090(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 Cl1 Cl2 2.205(5) 12_755 ? Cl1 Cl2 2.205(5) 15_664 ? Cl2 Cl2 1.477(6) 15_664 ? Cl2 Cl2 1.477(6) 12_755 ? Cl2 Cl2 2.039(7) 6_654 ? Cl2 Cl1 2.205(5) 15_664 ? Yb1 Yb1' 1.936(9) . ? Yb1 O2W 2.070(16) . ? Yb1 O1W 2.341(19) . ? Yb1 O3 2.412(4) . ? Yb1 O1W 2.42(2) 12_756 ? Yb1 O2 2.428(4) . ? Yb1 Yb1 2.583(2) 15_665 ? Yb1 Yb1 2.583(2) 12_756 ? Yb1 O2W 2.61(2) 12_756 ? Yb1 Yb1' 2.710(13) 15_665 ? Yb1 O1W 2.784(18) 15_665 ? Yb1 Yb1 3.285(3) 6_654 ? Yb1' O1W 1.648(14) 12_756 ? Yb1' O1W 1.648(14) 15_665 ? Yb1' Yb1 1.936(9) 6_654 ? Yb1' O3 2.608(9) 6_654 ? Yb1' O3 2.608(9) . ? Yb1' Yb1 2.710(13) 15_665 ? Yb1' Yb1 2.710(13) 12_756 ? Yb1' Yb1' 3.18(3) 15_665 ? O1W Yb1' 1.648(14) 15_665 ? O1W Yb1 2.42(2) 15_665 ? O1W Yb1 2.784(18) 12_756 ? O2W Yb1 2.61(2) 15_665 ? C1 O1 1.247(6) . ? C1 N1 1.337(6) . ? C1 N2 1.348(6) . ? C2 N1 1.456(6) . ? C2 N3 1.458(6) . ? C2 C3 1.541(7) . ? C2 H2 0.9900 . ? C3 N2 1.454(6) . ? C3 N4 1.456(6) . ? C3 H3 0.9900 . ? C4 O5 1.227(5) . ? C4 N3 1.336(6) . ? C4 N4 1.387(6) . ? C5 N5 1.438(6) . ? C5 N2 1.467(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.446(6) . ? C6 N7 1.474(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.253(6) . ? C7 N6 1.347(7) . ? C7 N5 1.360(6) . ? C8 N7 1.431(5) . ? C8 N5 1.458(5) . ? C8 C9 1.554(6) . ? C8 H8 0.9900 . ? C9 N8 1.425(5) . ? C9 N6 1.470(6) . ? C9 H9 0.9900 . ? C10 O6 1.190(5) . ? C10 N8 1.386(6) . ? C10 N7 1.388(6) . ? C11 N6 1.433(6) . ? C11 N9 1.474(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.441(6) . ? C12 N11 1.450(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.227(6) . ? C13 N10 1.338(6) . ? C13 N9 1.368(7) . ? C14 N9 1.441(6) . ? C14 N11 1.449(6) . ? C14 C15 1.537(6) . ? C14 H14 0.9900 . ? C15 N12 1.432(6) . ? C15 N10 1.460(6) . ? C15 H15 0.9900 . ? C16 O7 1.228(5) . ? C16 N11 1.364(6) . ? C16 N12 1.365(6) . ? C17 N10 1.459(6) . ? C17 N13 1.465(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.424(6) . ? C18 N15 1.470(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.216(6) . ? C19 N14 1.368(6) . ? C19 N13 1.381(7) . ? C20 N13 1.424(6) . ? C20 N15 1.478(6) . ? C20 C21 1.524(7) . ? C20 H20 0.9900 . ? C21 N16 1.437(6) . ? C21 N14 1.464(6) . ? C21 H21 0.9900 . ? C22 O8 1.239(5) . ? C22 N16 1.333(6) . ? C22 N15 1.371(6) . ? C23 N14 1.447(6) . ? C23 N3 1.455(6) 9_765 ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N1 1.445(6) 9_765 ? C24 N16 1.470(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? N1 C24 1.445(6) 9_765 ? N3 C23 1.455(6) 9_765 ? 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 Cl2 Cl1 Cl2 55.1(2) 12_755 15_664 ? Cl2 Cl2 Cl2 87.30(9) 15_664 12_755 ? Cl2 Cl2 Cl2 46.35(5) 15_664 6_654 ? Cl2 Cl2 Cl2 46.35(5) 12_755 6_654 ? Cl2 Cl2 Cl1 82.71(19) 15_664 15_664 ? Cl2 Cl2 Cl1 82.71(19) 12_755 15_664 ? Cl2 Cl2 Cl1 62.46(11) 6_654 15_664 ? Yb1' Yb1 O2W 101.5(6) . . ? Yb1' Yb1 O1W 121.0(5) . . ? O2W Yb1 O1W 88.3(8) . . ? Yb1' Yb1 O3 72.8(4) . . ? O2W Yb1 O3 84.3(6) . . ? O1W Yb1 O3 165.5(4) . . ? Yb1' Yb1 O1W 42.6(4) . 12_756 ? O2W Yb1 O1W 139.0(7) . 12_756 ? O1W Yb1 O1W 124.3(6) . 12_756 ? O3 Yb1 O1W 68.1(4) . 12_756 ? Yb1' Yb1 O2 169.3(4) . . ? O2W Yb1 O2 74.3(6) . . ? O1W Yb1 O2 69.1(3) . . ? O3 Yb1 O2 96.92(15) . . ? O1W Yb1 O2 136.5(5) 12_756 . ? Yb1' Yb1 Yb1 72.1(3) . 15_665 ? O2W Yb1 Yb1 67.2(6) . 15_665 ? O1W Yb1 Yb1 58.7(4) . 15_665 ? O3 Yb1 Yb1 128.36(13) . 15_665 ? O1W Yb1 Yb1 106.5(5) 12_756 15_665 ? O2 Yb1 Yb1 114.05(12) . 15_665 ? Yb1' Yb1 Yb1 72.1(3) . 12_756 ? O2W Yb1 Yb1 145.7(6) . 12_756 ? O1W Yb1 Yb1 68.7(4) . 12_756 ? O3 Yb1 Yb1 123.13(13) . 12_756 ? O1W Yb1 Yb1 55.7(4) 12_756 12_756 ? O2 Yb1 Yb1 116.99(12) . 12_756 ? Yb1 Yb1 Yb1 78.98(5) 15_665 12_756 ? Yb1' Yb1 O2W 111.9(4) . 12_756 ? O2W Yb1 O2W 145.4(3) . 12_756 ? O1W Yb1 O2W 67.1(7) . 12_756 ? O3 Yb1 O2W 113.6(5) . 12_756 ? O1W Yb1 O2W 75.3(6) 12_756 12_756 ? O2 Yb1 O2W 74.3(4) . 12_756 ? Yb1 Yb1 O2W 114.0(4) 15_665 12_756 ? Yb1 Yb1 O2W 47.0(3) 12_756 12_756 ? Yb1' Yb1 Yb1' 84.7(6) . 15_665 ? O2W Yb1 Yb1' 104.0(6) . 15_665 ? O1W Yb1 Yb1' 37.2(4) . 15_665 ? O3 Yb1 Yb1' 157.2(2) . 15_665 ? O1W Yb1 Yb1' 93.0(5) 12_756 15_665 ? O2 Yb1 Yb1' 105.8(2) . 15_665 ? Yb1 Yb1 Yb1' 42.84(8) 15_665 15_665 ? Yb1 Yb1 Yb1' 42.84(8) 12_756 15_665 ? O2W Yb1 Yb1' 71.3(4) 12_756 15_665 ? Yb1' Yb1 O1W 35.4(3) . 15_665 ? O2W Yb1 O1W 67.0(7) . 15_665 ? O1W Yb1 O1W 110.3(7) . 15_665 ? O3 Yb1 O1W 78.2(4) . 15_665 ? O1W Yb1 O1W 77.7(5) 12_756 15_665 ? O2 Yb1 O1W 141.3(4) . 15_665 ? Yb1 Yb1 O1W 51.6(4) 15_665 15_665 ? Yb1 Yb1 O1W 96.6(4) 12_756 15_665 ? O2W Yb1 O1W 143.1(5) 12_756 15_665 ? Yb1' Yb1 O1W 85.5(5) 15_665 15_665 ? Yb1' Yb1 Yb1 32.0(4) . 6_654 ? O2W Yb1 Yb1 106.7(6) . 6_654 ? O1W Yb1 Yb1 89.3(3) . 6_654 ? O3 Yb1 Yb1 104.70(11) . 6_654 ? O1W Yb1 Yb1 56.0(5) 12_756 6_654 ? O2 Yb1 Yb1 158.36(10) . 6_654 ? Yb1 Yb1 Yb1 50.51(2) 15_665 6_654 ? Yb1 Yb1 Yb1 50.51(2) 12_756 6_654 ? O2W Yb1 Yb1 97.3(3) 12_756 6_654 ? Yb1' Yb1 Yb1 52.7(2) 15_665 6_654 ? O1W Yb1 Yb1 46.1(4) 15_665 6_654 ? O1W Yb1' O1W 168.3(17) 12_756 15_665 ? O1W Yb1' Yb1 101.6(7) 12_756 6_654 ? O1W Yb1' Yb1 84.6(8) 15_665 6_654 ? O1W Yb1' Yb1 84.6(8) 12_756 . ? O1W Yb1' Yb1 101.6(7) 15_665 . ? Yb1 Yb1' Yb1 116.0(8) 6_654 . ? O1W Yb1' O3 98.7(9) 12_756 6_654 ? O1W Yb1' O3 75.3(7) 15_665 6_654 ? Yb1 Yb1' O3 62.06(14) 6_654 6_654 ? Yb1 Yb1' O3 176.3(4) . 6_654 ? O1W Yb1' O3 75.3(7) 12_756 . ? O1W Yb1' O3 98.7(9) 15_665 . ? Yb1 Yb1' O3 176.3(4) 6_654 . ? Yb1 Yb1' O3 62.06(14) . . ? O3 Yb1' O3 120.1(6) 6_654 . ? O1W Yb1' Yb1 132.4(10) 12_756 15_665 ? O1W Yb1' Yb1 59.2(7) 15_665 15_665 ? Yb1 Yb1' Yb1 65.1(4) 6_654 15_665 ? Yb1 Yb1' Yb1 65.1(4) . 15_665 ? O3 Yb1' Yb1 111.39(18) 6_654 15_665 ? O3 Yb1' Yb1 115.5(2) . 15_665 ? O1W Yb1' Yb1 59.2(7) 12_756 12_756 ? O1W Yb1' Yb1 132.4(10) 15_665 12_756 ? Yb1 Yb1' Yb1 65.1(4) 6_654 12_756 ? Yb1 Yb1' Yb1 65.1(4) . 12_756 ? O3 Yb1' Yb1 115.5(2) 6_654 12_756 ? O3 Yb1' Yb1 111.39(18) . 12_756 ? Yb1 Yb1' Yb1 74.6(4) 15_665 12_756 ? O1W Yb1' Yb1' 95.9(8) 12_756 15_665 ? O1W Yb1' Yb1' 95.9(8) 15_665 15_665 ? Yb1 Yb1' Yb1' 58.0(4) 6_654 15_665 ? Yb1 Yb1' Yb1' 58.0(4) . 15_665 ? O3 Yb1' Yb1' 120.0(3) 6_654 15_665 ? O3 Yb1' Yb1' 120.0(3) . 15_665 ? Yb1 Yb1' Yb1' 37.3(2) 15_665 15_665 ? Yb1 Yb1' Yb1' 37.3(2) 12_756 15_665 ? Yb1' O1W Yb1 83.6(9) 15_665 . ? Yb1' O1W Yb1 52.7(6) 15_665 15_665 ? Yb1 O1W Yb1 65.6(5) . 15_665 ? Yb1' O1W Yb1 42.9(5) 15_665 12_756 ? Yb1 O1W Yb1 59.8(4) . 12_756 ? Yb1 O1W Yb1 77.9(5) 15_665 12_756 ? Yb1 O2W Yb1 65.8(6) . 15_665 ? O1 C1 N1 125.6(5) . . ? O1 C1 N2 124.3(5) . . ? N1 C1 N2 110.1(4) . . ? N1 C2 N3 115.1(4) . . ? N1 C2 C3 102.9(4) . . ? N3 C2 C3 103.5(4) . . ? N1 C2 H2 111.6 . . ? N3 C2 H2 111.6 . . ? C3 C2 H2 111.6 . . ? N2 C3 N4 113.2(4) . . ? N2 C3 C2 103.3(4) . . ? N4 C3 C2 103.3(4) . . ? N2 C3 H3 112.1 . . ? N4 C3 H3 112.1 . . ? C2 C3 H3 112.1 . . ? O5 C4 N3 126.1(5) . . ? O5 C4 N4 124.9(5) . . ? N3 C4 N4 109.0(4) . . ? N5 C5 N2 113.1(4) . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? N2 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 111.4(4) . . ? N4 C6 H6A 109.4 . . ? N7 C6 H6A 109.4 . . ? N4 C6 H6B 109.4 . . ? N7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? O2 C7 N6 124.8(5) . . ? O2 C7 N5 124.7(5) . . ? N6 C7 N5 110.5(4) . . ? N7 C8 N5 114.0(4) . . ? N7 C8 C9 103.5(3) . . ? N5 C8 C9 103.8(3) . . ? N7 C8 H8 111.7 . . ? N5 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N8 C9 N6 114.5(4) . . ? N8 C9 C8 103.4(3) . . ? N6 C9 C8 102.6(4) . . ? N8 C9 H9 111.9 . . ? N6 C9 H9 111.9 . . ? C8 C9 H9 111.9 . . ? O6 C10 N8 127.6(4) . . ? O6 C10 N7 126.2(4) . . ? N8 C10 N7 106.2(4) . . ? N6 C11 N9 113.3(4) . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11B 108.9 . . ? N9 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 113.8(4) . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12B 108.8 . . ? N11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 125.3(5) . . ? O3 C13 N9 126.5(5) . . ? N10 C13 N9 108.1(4) . . ? N9 C14 N11 114.3(4) . . ? N9 C14 C15 102.6(4) . . ? N11 C14 C15 103.2(3) . . ? N9 C14 H14 112.0 . . ? N11 C14 H14 112.0 . . ? C15 C14 H14 112.0 . . ? N12 C15 N10 114.2(4) . . ? N12 C15 C14 104.4(4) . . ? N10 C15 C14 103.4(4) . . ? N12 C15 H15 111.5 . . ? N10 C15 H15 111.5 . . ? C14 C15 H15 111.5 . . ? O7 C16 N11 125.8(4) . . ? O7 C16 N12 125.0(4) . . ? N11 C16 N12 109.1(4) . . ? N10 C17 N13 112.8(4) . . ? N10 C17 H17A 109.0 . . ? N13 C17 H17A 109.0 . . ? N10 C17 H17B 109.0 . . ? N13 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N12 C18 N15 113.4(4) . . ? N12 C18 H18A 108.9 . . ? N15 C18 H18A 108.9 . . ? N12 C18 H18B 108.9 . . ? N15 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N14 126.1(5) . . ? O4 C19 N13 126.3(5) . . ? N14 C19 N13 107.5(4) . . ? N13 C20 N15 113.0(4) . . ? N13 C20 C21 104.9(4) . . ? N15 C20 C21 102.3(4) . . ? N13 C20 H20 112.0 . . ? N15 C20 H20 112.0 . . ? C21 C20 H20 112.0 . . ? N16 C21 N14 114.7(4) . . ? N16 C21 C20 104.6(4) . . ? N14 C21 C20 102.7(4) . . ? N16 C21 H21 111.4 . . ? N14 C21 H21 111.4 . . ? C20 C21 H21 111.4 . . ? O8 C22 N16 126.9(5) . . ? O8 C22 N15 124.1(4) . . ? N16 C22 N15 109.0(4) . . ? N14 C23 N3 114.5(4) . 9_765 ? N14 C23 H23A 108.6 . . ? N3 C23 H23A 108.6 9_765 . ? N14 C23 H23B 108.6 . . ? N3 C23 H23B 108.6 9_765 . ? H23A C23 H23B 107.6 . . ? N1 C24 N16 113.8(4) 9_765 . ? N1 C24 H24A 108.8 9_765 . ? N16 C24 H24A 108.8 . . ? N1 C24 H24B 108.8 9_765 . ? N16 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C1 N1 C24 122.3(4) . 9_765 ? C1 N1 C2 112.0(4) . . ? C24 N1 C2 123.1(4) 9_765 . ? C1 N2 C3 111.5(4) . . ? C1 N2 C5 122.8(4) . . ? C3 N2 C5 122.8(4) . . ? C4 N3 C23 124.4(4) . 9_765 ? C4 N3 C2 112.7(4) . . ? C23 N3 C2 121.5(4) 9_765 . ? C4 N4 C6 123.2(4) . . ? C4 N4 C3 111.3(4) . . ? C6 N4 C3 120.9(4) . . ? C7 N5 C5 122.5(4) . . ? C7 N5 C8 111.1(4) . . ? C5 N5 C8 123.2(4) . . ? C7 N6 C11 124.2(4) . . ? C7 N6 C9 111.7(4) . . ? C11 N6 C9 122.4(4) . . ? C10 N7 C8 113.1(4) . . ? C10 N7 C6 121.3(4) . . ? C8 N7 C6 121.6(4) . . ? C10 N8 C9 113.6(4) . . ? C10 N8 C12 120.6(4) . . ? C9 N8 C12 123.4(4) . . ? C13 N9 C14 113.1(4) . . ? C13 N9 C11 122.3(4) . . ? C14 N9 C11 123.2(4) . . ? C13 N10 C17 121.6(4) . . ? C13 N10 C15 112.4(4) . . ? C17 N10 C15 120.3(4) . . ? C16 N11 C14 111.3(4) . . ? C16 N11 C12 123.0(4) . . ? C14 N11 C12 123.1(4) . . ? C16 N12 C18 122.3(4) . . ? C16 N12 C15 111.5(4) . . ? C18 N12 C15 124.3(4) . . ? C19 N13 C20 112.2(4) . . ? C19 N13 C17 121.9(4) . . ? C20 N13 C17 122.6(4) . . ? C19 N14 C23 123.7(4) . . ? C19 N14 C21 112.3(4) . . ? C23 N14 C21 122.4(4) . . ? C22 N15 C18 123.4(4) . . ? C22 N15 C20 111.2(4) . . ? C18 N15 C20 122.0(4) . . ? C22 N16 C21 112.7(4) . . ? C22 N16 C24 121.1(4) . . ? C21 N16 C24 123.3(4) . . ? C7 O2 Yb1 139.9(4) . . ? C13 O3 Yb1 140.3(4) . . ? C13 O3 Yb1' 163.7(4) . . ? Yb1 O3 Yb1' 45.2(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.900 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.085 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 352 107 ' ' 2 -0.013 -0.042 0.454 4506 1778 ' ' 3 0.000 0.500 1.000 352 107 ' ' 4 0.250 0.250 0.250 352 108 ' ' 5 0.250 0.750 0.750 352 108 ' ' 6 0.500 0.500 0.500 352 107 ' ' 7 0.500 1.000 0.500 352 107 ' ' 8 0.750 0.250 0.250 352 108 ' ' 9 0.750 0.750 0.750 352 108 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952107' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H241 Cl3.50 Lu N64 O104' _chemical_formula_weight 4255.57 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' Lu Lu -0.4720 5.8584 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 28.3363(19) _cell_length_b 28.3363(19) _cell_length_c 21.928(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17607(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8910 _exptl_absorpt_coefficient_mu 0.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8420 _exptl_absorpt_correction_T_max 0.8719 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60112 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8619 _reflns_number_gt 4903 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1458P)^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 8619 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2475 _refine_ls_wR_factor_gt 0.2289 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.010 _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 Cl1 Cl 1.0000 1.2500 -0.27804(15) 0.147(2) Uani 0.70 2 d SP . . Cl2 Cl 0.99768(13) 1.21350(10) -0.38216(11) 0.1134(10) Uani 0.65 1 d P . . Lu1 Lu 0.95837(3) 1.20950(3) 0.10219(4) 0.0385(3) Uani 0.18 1 d P . . Lu1' Lu 1.0000 1.2500 0.202(3) 1.22(8) Uani 0.14 2 d SP . . O1W O 0.9950(4) 1.1435(3) 0.0928(6) 0.152(4) Uani 0.50 1 d P . . O2W O 0.9711(4) 1.2011(5) 0.2017(5) 0.168(6) Uani 0.50 1 d P . . C1 C 1.02519(14) 1.16157(14) -0.15926(19) 0.0465(10) Uani 1 1 d . . . C2 C 1.00894(14) 1.12337(14) -0.25178(18) 0.0447(9) Uani 1 1 d . . . H2 H 1.0168 1.1367 -0.2923 0.054 Uiso 1 1 calc R . . C3 C 0.96316(13) 1.14566(14) -0.22514(18) 0.0441(9) Uani 1 1 d . . . H3 H 0.9500 1.1703 -0.2523 0.053 Uiso 1 1 calc R . . C4 C 0.95244(14) 1.06413(13) -0.24006(17) 0.0427(9) Uani 1 1 d . . . C5 C 0.94941(15) 1.19817(15) -0.1343(2) 0.0538(11) Uani 1 1 d . . . H5A H 0.9347 1.2201 -0.1631 0.065 Uiso 1 1 calc R . . H5B H 0.9697 1.2165 -0.1070 0.065 Uiso 1 1 calc R . . C6 C 0.88040(12) 1.11061(14) -0.21520(17) 0.0428(9) Uani 1 1 d . . . H6A H 0.8708 1.1369 -0.2415 0.051 Uiso 1 1 calc R . . H6B H 0.8652 1.0819 -0.2306 0.051 Uiso 1 1 calc R . . C7 C 0.90913(17) 1.18179(15) -0.0375(2) 0.0537(11) Uani 1 1 d . . . C8 C 0.86630(13) 1.16479(13) -0.12553(18) 0.0423(9) Uani 1 1 d . . . H8 H 0.8557 1.1905 -0.1529 0.051 Uiso 1 1 calc R . . C9 C 0.83375(14) 1.15954(13) -0.06940(17) 0.0439(9) Uani 1 1 d . . . H9 H 0.8065 1.1813 -0.0716 0.053 Uiso 1 1 calc R . . C10 C 0.83460(13) 1.08910(14) -0.12460(18) 0.0424(9) Uani 1 1 d . . . C11 C 0.84678(18) 1.18140(14) 0.04262(18) 0.0566(12) Uani 1 1 d . . . H11A H 0.8690 1.2026 0.0632 0.068 Uiso 1 1 calc R . . H11B H 0.8164 1.1977 0.0397 0.068 Uiso 1 1 calc R . . C12 C 0.78217(13) 1.09079(13) -0.03429(17) 0.0424(9) Uani 1 1 d . . . H12A H 0.7567 1.1139 -0.0301 0.051 Uiso 1 1 calc R . . H12B H 0.7691 1.0628 -0.0545 0.051 Uiso 1 1 calc R . . C13 C 0.86913(14) 1.12850(13) 0.1268(2) 0.0470(10) Uani 1 1 d . . . C14 C 0.79942(14) 1.10913(13) 0.07630(16) 0.0400(9) Uani 1 1 d . . . H14 H 0.7700 1.1279 0.0789 0.048 Uiso 1 1 calc R . . C15 C 0.80556(12) 1.07656(12) 0.13232(17) 0.0375(9) Uani 1 1 d . . . H15 H 0.7794 1.0803 0.1619 0.045 Uiso 1 1 calc R . . C16 C 0.79984(12) 1.03070(13) 0.04345(18) 0.0403(9) Uani 1 1 d . . . C17 C 0.86494(15) 1.07887(14) 0.21952(19) 0.0509(10) Uani 1 1 d . . . H17A H 0.8374 1.0816 0.2464 0.061 Uiso 1 1 calc R . . H17B H 0.8887 1.1014 0.2338 0.061 Uiso 1 1 calc R . . C18 C 0.79758(13) 0.98779(13) 0.14136(19) 0.0452(9) Uani 1 1 d . . . H18A H 0.7732 0.9944 0.1719 0.054 Uiso 1 1 calc R . . H18B H 0.7855 0.9632 0.1141 0.054 Uiso 1 1 calc R . . C19 C 0.92886(14) 1.02284(15) 0.24277(18) 0.0459(10) Uani 1 1 d . . . C20 C 0.85472(13) 0.98965(14) 0.23051(17) 0.0427(9) Uani 1 1 d . . . H20 H 0.8279 0.9948 0.2588 0.051 Uiso 1 1 calc R . . C21 C 0.88892(13) 0.95177(14) 0.25420(18) 0.0439(9) Uani 1 1 d . . . H21 H 0.8791 0.9397 0.2946 0.053 Uiso 1 1 calc R . . C22 C 0.85791(13) 0.92673(13) 0.16204(17) 0.0405(9) Uani 1 1 d . . . C23 C 0.97384(14) 0.95934(15) 0.2906(2) 0.0515(10) Uani 1 1 d . . . H23A H 0.9626 0.9436 0.3277 0.062 Uiso 1 1 calc R . . H23B H 0.9938 0.9859 0.3031 0.062 Uiso 1 1 calc R . . C24 C 0.90634(13) 0.86869(14) 0.2174(2) 0.0493(10) Uani 1 1 d . . . H24A H 0.8897 0.8467 0.1904 0.059 Uiso 1 1 calc R . . H24B H 0.8998 0.8591 0.2595 0.059 Uiso 1 1 calc R . . N1 N 1.04394(11) 1.13568(11) -0.20663(15) 0.0453(8) Uani 1 1 d . . . N2 N 0.97811(11) 1.16481(12) -0.16775(16) 0.0490(8) Uani 1 1 d . . . N3 N 0.99769(10) 1.07392(11) -0.25551(14) 0.0426(8) Uani 1 1 d . . . N4 N 0.93106(10) 1.10494(10) -0.21916(14) 0.0398(7) Uani 1 1 d . . . N5 N 0.91228(11) 1.17519(11) -0.09807(16) 0.0466(8) Uani 1 1 d . . . N6 N 0.86429(13) 1.17108(12) -0.01948(15) 0.0513(9) Uani 1 1 d . . . N7 N 0.86399(11) 1.11947(11) -0.15479(14) 0.0418(8) Uani 1 1 d . . . N8 N 0.81904(11) 1.11078(11) -0.07275(14) 0.0426(8) Uani 1 1 d . . . N9 N 0.84100(13) 1.13893(11) 0.07889(15) 0.0512(9) Uani 1 1 d . . . N10 N 0.85096(11) 1.09155(11) 0.15813(14) 0.0456(8) Uani 1 1 d . . . N11 N 0.79857(11) 1.07753(10) 0.02605(14) 0.0419(8) Uani 1 1 d . . . N12 N 0.80613(10) 1.03031(10) 0.10604(13) 0.0385(7) Uani 1 1 d . . . N13 N 0.88404(11) 1.03158(11) 0.22458(15) 0.0443(8) Uani 1 1 d . . . N14 N 0.93375(11) 0.97743(12) 0.25764(15) 0.0460(8) Uani 1 1 d . . . N15 N 0.83922(11) 0.97038(11) 0.17198(14) 0.0421(8) Uani 1 1 d . . . N16 N 0.88748(11) 0.91509(11) 0.20810(15) 0.0444(8) Uani 1 1 d . . . O1 O 1.04786(11) 1.17908(11) -0.11739(15) 0.0638(8) Uani 1 1 d . . . O2 O 0.94048(13) 1.19630(13) -0.00476(16) 0.0823(11) Uani 1 1 d . . . O3 O 0.90581(11) 1.14933(11) 0.14073(15) 0.0656(9) Uani 1 1 d . . . O4 O 0.96105(10) 1.05313(10) 0.24454(14) 0.0588(8) Uani 1 1 d . . . O5 O 0.93312(10) 1.02522(10) -0.24250(13) 0.0537(7) Uani 1 1 d . . . O6 O 0.82345(10) 1.04956(9) -0.14258(13) 0.0508(7) Uani 1 1 d . . . O7 O 0.79685(11) 0.99652(9) 0.01077(13) 0.0538(7) Uani 1 1 d . . . O8 O 0.84903(10) 0.90144(10) 0.11780(14) 0.0585(8) 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 Cl1 0.286(6) 0.079(2) 0.076(2) 0.000 0.000 -0.116(3) Cl2 0.1217(18) 0.150(2) 0.0685(14) 0.0662(18) -0.0156(14) -0.016(3) Lu1 0.0381(5) 0.0388(5) 0.0386(5) 0.0004(4) -0.0043(4) 0.0030(4) Lu1' 0.174(17) 1.49(12) 2.0(2) 0.000 0.000 0.09(3) O1W 0.147(9) 0.087(6) 0.222(13) -0.031(7) 0.003(9) 0.038(6) O2W 0.099(8) 0.273(15) 0.132(9) -0.020(9) 0.012(6) -0.105(9) C1 0.045(2) 0.042(2) 0.053(3) -0.0044(19) -0.007(2) -0.0069(18) C2 0.046(2) 0.045(2) 0.043(2) 0.0065(18) 0.0057(18) -0.0032(18) C3 0.041(2) 0.046(2) 0.045(2) 0.0048(18) -0.0014(18) 0.0001(17) C4 0.048(2) 0.039(2) 0.041(2) 0.0016(17) -0.0054(18) -0.0006(18) C5 0.054(3) 0.051(2) 0.056(3) -0.017(2) 0.008(2) -0.011(2) C6 0.036(2) 0.053(2) 0.039(2) -0.0030(18) -0.0019(17) -0.0020(17) C7 0.066(3) 0.045(2) 0.050(3) -0.012(2) -0.012(2) 0.003(2) C8 0.050(2) 0.035(2) 0.042(2) 0.0020(17) -0.0074(18) -0.0031(17) C9 0.053(2) 0.039(2) 0.040(2) -0.0034(17) -0.0001(18) 0.0029(18) C10 0.039(2) 0.044(2) 0.044(2) -0.0021(18) -0.0021(18) -0.0001(17) C11 0.095(3) 0.036(2) 0.039(2) -0.0047(18) 0.010(2) -0.013(2) C12 0.039(2) 0.045(2) 0.043(2) 0.0014(18) 0.0034(17) -0.0035(17) C13 0.046(2) 0.039(2) 0.056(3) -0.0081(19) 0.005(2) -0.0106(18) C14 0.050(2) 0.039(2) 0.030(2) -0.0007(16) 0.0050(17) 0.0021(17) C15 0.036(2) 0.038(2) 0.038(2) -0.0024(16) 0.0031(16) -0.0002(16) C16 0.0288(18) 0.041(2) 0.051(2) 0.0009(19) 0.0020(17) -0.0014(15) C17 0.053(2) 0.046(2) 0.054(3) -0.007(2) -0.007(2) -0.0048(19) C18 0.040(2) 0.043(2) 0.052(2) -0.0036(18) -0.0021(18) -0.0073(17) C19 0.043(2) 0.055(3) 0.040(2) -0.0129(19) 0.0039(18) 0.000(2) C20 0.041(2) 0.048(2) 0.039(2) -0.0059(17) -0.0002(17) 0.0002(17) C21 0.041(2) 0.051(2) 0.040(2) 0.0017(18) 0.0022(17) 0.0008(18) C22 0.041(2) 0.040(2) 0.040(2) -0.0046(18) 0.0031(17) -0.0081(17) C23 0.040(2) 0.061(3) 0.053(3) -0.012(2) -0.0008(19) 0.0001(19) C24 0.042(2) 0.041(2) 0.065(3) -0.002(2) -0.002(2) -0.0060(18) N1 0.0409(18) 0.0417(18) 0.053(2) -0.0058(16) -0.0027(16) -0.0011(14) N2 0.0428(19) 0.049(2) 0.055(2) -0.0165(16) -0.0023(16) -0.0041(15) N3 0.0370(18) 0.0445(19) 0.0464(19) -0.0092(15) 0.0021(14) -0.0070(14) N4 0.0327(16) 0.0393(17) 0.0474(19) -0.0009(14) 0.0000(14) -0.0046(13) N5 0.0412(18) 0.0452(19) 0.053(2) -0.0088(16) 0.0022(16) -0.0054(14) N6 0.065(2) 0.047(2) 0.042(2) -0.0047(15) 0.0003(17) -0.0132(17) N7 0.0424(18) 0.0481(19) 0.0348(17) -0.0037(14) 0.0043(14) -0.0031(14) N8 0.0494(19) 0.0408(18) 0.0377(18) -0.0052(14) 0.0084(15) -0.0044(14) N9 0.069(2) 0.0422(19) 0.042(2) 0.0004(15) 0.0000(17) -0.0155(16) N10 0.0471(19) 0.051(2) 0.0391(19) -0.0029(15) -0.0023(15) -0.0067(15) N11 0.0463(18) 0.0398(18) 0.0395(19) -0.0036(14) 0.0022(14) -0.0017(14) N12 0.0435(18) 0.0377(17) 0.0343(17) -0.0005(13) -0.0028(14) 0.0005(13) N13 0.0406(18) 0.0392(18) 0.053(2) 0.0006(15) -0.0057(15) -0.0074(14) N14 0.0381(18) 0.047(2) 0.053(2) -0.0038(16) -0.0051(15) -0.0031(15) N15 0.0451(18) 0.0397(18) 0.0415(19) -0.0044(14) -0.0009(14) 0.0002(14) N16 0.0425(18) 0.0379(17) 0.053(2) 0.0000(15) -0.0062(16) -0.0018(14) O1 0.0610(19) 0.0589(19) 0.072(2) -0.0205(16) -0.0127(16) -0.0127(15) O2 0.083(2) 0.097(3) 0.067(2) -0.0257(19) -0.0207(19) -0.014(2) O3 0.065(2) 0.0595(19) 0.072(2) -0.0104(16) 0.0004(16) -0.0176(16) O4 0.0487(17) 0.0524(18) 0.075(2) -0.0111(15) 0.0034(15) -0.0133(14) O5 0.0511(17) 0.0469(17) 0.0631(19) -0.0132(14) -0.0006(14) -0.0089(13) O6 0.0568(17) 0.0406(16) 0.0550(18) -0.0105(13) 0.0048(14) -0.0107(13) O7 0.073(2) 0.0389(15) 0.0498(17) -0.0148(13) -0.0030(14) -0.0095(13) O8 0.0663(19) 0.0523(18) 0.0570(19) -0.0104(15) -0.0098(15) 0.0049(14) _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 Cl1 Cl2 2.225(4) 15_574 ? Cl1 Cl2 2.225(4) 12_865 ? Cl2 Cl2 1.499(5) 12_865 ? Cl2 Cl2 1.499(5) 15_574 ? Cl2 Cl2 2.073(6) 6_674 ? Cl2 Cl1 2.225(4) 15_574 ? Lu1 Lu1' 2.03(4) 15_575 ? Lu1 O1W 2.148(9) . ? Lu1 O2W 2.224(12) . ? Lu1 O2W 2.303(11) 15_575 ? Lu1 O3 2.417(3) . ? Lu1 O2 2.428(3) . ? Lu1 Lu1 2.5333(14) 12_866 ? Lu1 Lu1 2.5333(14) 15_575 ? Lu1 O1W 2.550(12) 15_575 ? Lu1 Lu1' 2.74(6) . ? Lu1 O2W 2.843(16) 12_866 ? Lu1 Lu1 3.2914(18) 6_674 ? Lu1' O2W 1.610(11) 6_674 ? Lu1' O2W 1.610(11) . ? Lu1' Lu1 2.03(4) 12_866 ? Lu1' Lu1 2.03(4) 15_575 ? Lu1' O2 2.55(3) 15_575 ? Lu1' O2 2.55(3) 12_866 ? Lu1' Lu1 2.74(6) 6_674 ? Lu1' Lu1' 3.39(14) 15_575 ? O1W Lu1 2.550(11) 12_866 ? O2W Lu1 2.303(11) 12_866 ? O2W Lu1 2.843(16) 15_575 ? C1 O1 1.225(5) . ? C1 N2 1.350(5) . ? C1 N1 1.378(5) . ? C2 N3 1.439(5) . ? C2 N1 1.444(5) . ? C2 C3 1.557(5) . ? C2 H2 0.9900 . ? C3 N2 1.434(5) . ? C3 N4 1.475(5) . ? C3 H3 0.9900 . ? C4 O5 1.232(4) . ? C4 N3 1.355(5) . ? C4 N4 1.384(5) . ? C5 N2 1.447(5) . ? C5 N5 1.470(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.426(5) . ? C6 N4 1.447(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.213(5) . ? C7 N5 1.345(5) . ? C7 N6 1.365(6) . ? C8 N7 1.437(5) . ? C8 N5 1.465(5) . ? C8 C9 1.545(5) . ? C8 H8 0.9900 . ? C9 N6 1.433(5) . ? C9 N8 1.445(5) . ? C9 H9 0.9900 . ? C10 O6 1.229(4) . ? C10 N8 1.366(5) . ? C10 N7 1.369(5) . ? C11 N9 1.452(5) . ? C11 N6 1.478(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.452(5) . ? C12 N8 1.457(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.234(5) . ? C13 N9 1.351(5) . ? C13 N10 1.354(5) . ? C14 N11 1.420(5) . ? C14 N9 1.451(5) . ? C14 C15 1.546(5) . ? C14 H14 0.9900 . ? C15 N12 1.432(5) . ? C15 N10 1.468(5) . ? C15 H15 0.9900 . ? C16 O7 1.208(4) . ? C16 N11 1.381(5) . ? C16 N12 1.384(5) . ? C17 N10 1.449(5) . ? C17 N13 1.449(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.445(5) . ? C18 N12 1.452(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.253(5) . ? C19 N14 1.335(5) . ? C19 N13 1.354(5) . ? C20 N13 1.456(5) . ? C20 N15 1.462(5) . ? C20 C21 1.537(5) . ? C20 H20 0.9900 . ? C21 N16 1.451(5) . ? C21 N14 1.466(5) . ? C21 H21 0.9900 . ? C22 O8 1.232(4) . ? C22 N16 1.353(5) . ? C22 N15 1.363(5) . ? C23 N14 1.441(5) . ? C23 N3 1.460(5) 9_775 ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.434(5) . ? C24 N1 1.434(5) 9_775 ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? N1 C24 1.434(5) 9_775 ? N3 C23 1.460(5) 9_775 ? O2 Lu1' 2.55(3) 15_575 ? 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 Cl2 Cl1 Cl2 55.52(19) 15_574 12_865 ? Cl2 Cl2 Cl2 87.49(7) 12_865 15_574 ? Cl2 Cl2 Cl2 46.26(4) 12_865 6_674 ? Cl2 Cl2 Cl2 46.26(4) 15_574 6_674 ? Cl2 Cl2 Cl1 82.14(14) 12_865 15_574 ? Cl2 Cl2 Cl1 82.14(14) 15_574 15_574 ? Cl2 Cl2 Cl1 62.24(9) 6_674 15_574 ? Lu1' Lu1 O1W 98.9(5) 15_575 . ? Lu1' Lu1 O2W 122.8(16) 15_575 . ? O1W Lu1 O2W 85.6(6) . . ? Lu1' Lu1 O2W 43.0(4) 15_575 15_575 ? O1W Lu1 O2W 137.5(5) . 15_575 ? O2W Lu1 O2W 127.5(6) . 15_575 ? Lu1' Lu1 O3 164.0(15) 15_575 . ? O1W Lu1 O3 73.5(3) . . ? O2W Lu1 O3 71.4(3) . . ? O2W Lu1 O3 136.6(4) 15_575 . ? Lu1' Lu1 O2 69.0(16) 15_575 . ? O1W Lu1 O2 82.7(4) . . ? O2W Lu1 O2 164.7(4) . . ? O2W Lu1 O2 67.5(3) 15_575 . ? O3 Lu1 O2 95.76(12) . . ? Lu1' Lu1 Lu1 72.9(12) 15_575 12_866 ? O1W Lu1 Lu1 65.4(3) . 12_866 ? O2W Lu1 Lu1 57.5(3) . 12_866 ? O2W Lu1 Lu1 107.2(4) 15_575 12_866 ? O3 Lu1 Lu1 114.78(9) . 12_866 ? O2 Lu1 Lu1 124.83(10) . 12_866 ? Lu1' Lu1 Lu1 72.9(12) 15_575 15_575 ? O1W Lu1 Lu1 146.3(3) . 15_575 ? O2W Lu1 Lu1 73.1(4) . 15_575 ? O2W Lu1 Lu1 54.5(3) 15_575 15_575 ? O3 Lu1 Lu1 121.19(9) . 15_575 ? O2 Lu1 Lu1 121.70(10) . 15_575 ? Lu1 Lu1 Lu1 81.03(3) 12_866 15_575 ? Lu1' Lu1 O1W 114.2(6) 15_575 15_575 ? O1W Lu1 O1W 146.52(19) . 15_575 ? O2W Lu1 O1W 72.9(5) . 15_575 ? O2W Lu1 O1W 75.3(4) 15_575 15_575 ? O3 Lu1 O1W 75.4(2) . 15_575 ? O2 Lu1 O1W 112.6(3) . 15_575 ? Lu1 Lu1 O1W 118.8(3) 12_866 15_575 ? Lu1 Lu1 O1W 50.0(2) 15_575 15_575 ? Lu1' Lu1 Lu1' 89(2) 15_575 . ? O1W Lu1 Lu1' 103.5(4) . . ? O2W Lu1 Lu1' 35.9(9) . . ? O2W Lu1 Lu1' 95.2(8) 15_575 . ? O3 Lu1 Lu1' 106.3(9) . . ? O2 Lu1 Lu1' 157.9(9) . . ? Lu1 Lu1 Lu1' 45.1(4) 12_866 . ? Lu1 Lu1 Lu1' 45.1(4) 15_575 . ? O1W Lu1 Lu1' 73.7(5) 15_575 . ? Lu1' Lu1 O2W 33.6(3) 15_575 12_866 ? O1W Lu1 O2W 68.0(4) . 12_866 ? O2W Lu1 O2W 105.9(4) . 12_866 ? O2W Lu1 O2W 76.7(4) 15_575 12_866 ? O3 Lu1 O2W 141.5(2) . 12_866 ? O2 Lu1 O2W 78.8(3) . 12_866 ? Lu1 Lu1 O2W 48.4(2) 12_866 12_866 ? Lu1 Lu1 O2W 92.7(2) 15_575 12_866 ? O1W Lu1 O2W 142.1(3) 15_575 12_866 ? Lu1' Lu1 O2W 84.0(8) . 12_866 ? Lu1' Lu1 Lu1 35.9(16) 15_575 6_674 ? O1W Lu1 Lu1 105.1(3) . 6_674 ? O2W Lu1 Lu1 87.6(2) . 6_674 ? O2W Lu1 Lu1 57.9(4) 15_575 6_674 ? O3 Lu1 Lu1 159.03(8) . 6_674 ? O2 Lu1 Lu1 104.89(9) . 6_674 ? Lu1 Lu1 Lu1 49.486(15) 12_866 6_674 ? Lu1 Lu1 Lu1 49.486(15) 15_575 6_674 ? O1W Lu1 Lu1 99.4(2) 15_575 6_674 ? Lu1' Lu1 Lu1 53.1(9) . 6_674 ? O2W Lu1 Lu1 43.3(2) 12_866 6_674 ? O2W Lu1' O2W 179(5) 6_674 . ? O2W Lu1' Lu1 102.0(18) 6_674 12_866 ? O2W Lu1' Lu1 77.5(14) . 12_866 ? O2W Lu1' Lu1 77.5(14) 6_674 15_575 ? O2W Lu1' Lu1 102.0(18) . 15_575 ? Lu1 Lu1' Lu1 108(3) 12_866 15_575 ? O2W Lu1' O2 74.8(11) 6_674 15_575 ? O2W Lu1' O2 105.6(15) . 15_575 ? Lu1 Lu1' O2 171(3) 12_866 15_575 ? Lu1 Lu1' O2 62.9(2) 15_575 15_575 ? O2W Lu1' O2 105.6(15) 6_674 12_866 ? O2W Lu1' O2 74.8(11) . 12_866 ? Lu1 Lu1' O2 62.9(2) 12_866 12_866 ? Lu1 Lu1' O2 171(3) 15_575 12_866 ? O2 Lu1' O2 126(3) 15_575 12_866 ? O2W Lu1' Lu1 125(3) 6_674 . ? O2W Lu1' Lu1 54.2(17) . . ? Lu1 Lu1' Lu1 62.0(15) 12_866 . ? Lu1 Lu1' Lu1 62.0(15) 15_575 . ? O2 Lu1' Lu1 112.5(8) 15_575 . ? O2 Lu1' Lu1 110.0(8) 12_866 . ? O2W Lu1' Lu1 54.2(17) 6_674 6_674 ? O2W Lu1' Lu1 125(3) . 6_674 ? Lu1 Lu1' Lu1 62.0(15) 12_866 6_674 ? Lu1 Lu1' Lu1 62.0(15) 15_575 6_674 ? O2 Lu1' Lu1 110.0(8) 15_575 6_674 ? O2 Lu1' Lu1 112.5(8) 12_866 6_674 ? Lu1 Lu1' Lu1 73.8(18) . 6_674 ? O2W Lu1' Lu1' 90(3) 6_674 15_575 ? O2W Lu1' Lu1' 90(3) . 15_575 ? Lu1 Lu1' Lu1' 54.1(16) 12_866 15_575 ? Lu1 Lu1' Lu1' 54.1(16) 15_575 15_575 ? O2 Lu1' Lu1' 116.9(14) 15_575 15_575 ? O2 Lu1' Lu1' 116.9(14) 12_866 15_575 ? Lu1 Lu1' Lu1' 36.9(9) . 15_575 ? Lu1 Lu1' Lu1' 36.9(9) 6_674 15_575 ? Lu1 O1W Lu1 64.6(3) . 12_866 ? Lu1' O2W Lu1 90(2) . . ? Lu1' O2W Lu1 59.5(15) . 12_866 ? Lu1 O2W Lu1 68.0(3) . 12_866 ? Lu1' O2W Lu1 44.4(15) . 15_575 ? Lu1 O2W Lu1 58.5(3) . 15_575 ? Lu1 O2W Lu1 78.8(3) 12_866 15_575 ? O1 C1 N2 126.4(4) . . ? O1 C1 N1 125.3(4) . . ? N2 C1 N1 108.2(3) . . ? N3 C2 N1 115.2(3) . . ? N3 C2 C3 103.4(3) . . ? N1 C2 C3 102.5(3) . . ? N3 C2 H2 111.7 . . ? N1 C2 H2 111.7 . . ? C3 C2 H2 111.7 . . ? N2 C3 N4 113.6(3) . . ? N2 C3 C2 103.7(3) . . ? N4 C3 C2 103.3(3) . . ? N2 C3 H3 111.9 . . ? N4 C3 H3 111.9 . . ? C2 C3 H3 111.9 . . ? O5 C4 N3 126.4(4) . . ? O5 C4 N4 124.6(4) . . ? N3 C4 N4 109.0(3) . . ? N2 C5 N5 112.8(3) . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5B 109.0 . . ? N5 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N7 C6 N4 113.5(3) . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6B 108.9 . . ? N4 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N5 125.6(5) . . ? O2 C7 N6 125.9(4) . . ? N5 C7 N6 108.4(4) . . ? N7 C8 N5 113.8(3) . . ? N7 C8 C9 104.0(3) . . ? N5 C8 C9 102.9(3) . . ? N7 C8 H8 111.8 . . ? N5 C8 H8 111.8 . . ? C9 C8 H8 111.8 . . ? N6 C9 N8 115.5(3) . . ? N6 C9 C8 103.1(3) . . ? N8 C9 C8 102.9(3) . . ? N6 C9 H9 111.5 . . ? N8 C9 H9 111.5 . . ? C8 C9 H9 111.5 . . ? O6 C10 N8 126.5(4) . . ? O6 C10 N7 125.1(4) . . ? N8 C10 N7 108.4(3) . . ? N9 C11 N6 112.2(3) . . ? N9 C11 H11A 109.2 . . ? N6 C11 H11A 109.2 . . ? N9 C11 H11B 109.2 . . ? N6 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N11 C12 N8 113.5(3) . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? N8 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 125.8(4) . . ? O3 C13 N10 124.4(4) . . ? N9 C13 N10 109.8(3) . . ? N11 C14 N9 114.3(3) . . ? N11 C14 C15 104.0(3) . . ? N9 C14 C15 103.0(3) . . ? N11 C14 H14 111.7 . . ? N9 C14 H14 111.7 . . ? C15 C14 H14 111.7 . . ? N12 C15 N10 114.2(3) . . ? N12 C15 C14 103.2(3) . . ? N10 C15 C14 103.4(3) . . ? N12 C15 H15 111.8 . . ? N10 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? O7 C16 N11 127.2(4) . . ? O7 C16 N12 126.2(4) . . ? N11 C16 N12 106.6(3) . . ? N10 C17 N13 113.7(3) . . ? N10 C17 H17A 108.8 . . ? N13 C17 H17A 108.8 . . ? N10 C17 H17B 108.8 . . ? N13 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N15 C18 N12 113.3(3) . . ? N15 C18 H18A 108.9 . . ? N12 C18 H18A 108.9 . . ? N15 C18 H18B 108.9 . . ? N12 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N14 125.2(4) . . ? O4 C19 N13 124.5(4) . . ? N14 C19 N13 110.2(3) . . ? N13 C20 N15 113.4(3) . . ? N13 C20 C21 103.9(3) . . ? N15 C20 C21 103.0(3) . . ? N13 C20 H20 111.9 . . ? N15 C20 H20 111.9 . . ? C21 C20 H20 111.9 . . ? N16 C21 N14 114.6(3) . . ? N16 C21 C20 104.3(3) . . ? N14 C21 C20 102.6(3) . . ? N16 C21 H21 111.6 . . ? N14 C21 H21 111.6 . . ? C20 C21 H21 111.6 . . ? O8 C22 N16 124.9(4) . . ? O8 C22 N15 125.1(4) . . ? N16 C22 N15 110.0(3) . . ? N14 C23 N3 113.6(3) . 9_775 ? N14 C23 H23A 108.8 . . ? N3 C23 H23A 108.8 9_775 . ? N14 C23 H23B 108.8 . . ? N3 C23 H23B 108.8 9_775 . ? H23A C23 H23B 107.7 . . ? N16 C24 N1 115.0(3) . 9_775 ? N16 C24 H24A 108.5 . . ? N1 C24 H24A 108.5 9_775 . ? N16 C24 H24B 108.5 . . ? N1 C24 H24B 108.5 9_775 . ? H24A C24 H24B 107.5 . . ? C1 N1 C24 123.3(3) . 9_775 ? C1 N1 C2 112.4(3) . . ? C24 N1 C2 122.7(3) 9_775 . ? C1 N2 C3 112.8(3) . . ? C1 N2 C5 122.0(3) . . ? C3 N2 C5 121.7(3) . . ? C4 N3 C2 113.2(3) . . ? C4 N3 C23 121.5(3) . 9_775 ? C2 N3 C23 122.4(3) . 9_775 ? C4 N4 C6 123.2(3) . . ? C4 N4 C3 110.7(3) . . ? C6 N4 C3 122.0(3) . . ? C7 N5 C8 112.0(3) . . ? C7 N5 C5 121.3(3) . . ? C8 N5 C5 120.2(3) . . ? C7 N6 C9 113.1(3) . . ? C7 N6 C11 122.3(3) . . ? C9 N6 C11 123.1(4) . . ? C10 N7 C6 122.5(3) . . ? C10 N7 C8 112.0(3) . . ? C6 N7 C8 123.9(3) . . ? C10 N8 C9 112.3(3) . . ? C10 N8 C12 122.6(3) . . ? C9 N8 C12 123.3(3) . . ? C13 N9 C14 112.5(3) . . ? C13 N9 C11 122.7(3) . . ? C14 N9 C11 123.5(4) . . ? C13 N10 C17 124.0(3) . . ? C13 N10 C15 111.2(3) . . ? C17 N10 C15 121.7(3) . . ? C16 N11 C14 113.0(3) . . ? C16 N11 C12 120.6(3) . . ? C14 N11 C12 123.3(3) . . ? C16 N12 C15 113.0(3) . . ? C16 N12 C18 120.9(3) . . ? C15 N12 C18 122.9(3) . . ? C19 N13 C17 122.8(3) . . ? C19 N13 C20 111.1(3) . . ? C17 N13 C20 123.3(3) . . ? C19 N14 C23 123.2(3) . . ? C19 N14 C21 112.1(3) . . ? C23 N14 C21 122.2(3) . . ? C22 N15 C18 123.6(3) . . ? C22 N15 C20 111.2(3) . . ? C18 N15 C20 121.7(3) . . ? C22 N16 C24 124.1(3) . . ? C22 N16 C21 111.3(3) . . ? C24 N16 C21 123.2(3) . . ? C7 O2 Lu1 140.9(3) . . ? C7 O2 Lu1' 162.7(9) . 15_575 ? Lu1 O2 Lu1' 48.2(14) . 15_575 ? C13 O3 Lu1 140.4(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.281 _refine_diff_density_min -0.936 _refine_diff_density_rms 0.078 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 359 111 ' ' 2 -0.003 -0.036 0.459 4406 1786 ' ' 3 0.000 0.500 1.000 359 111 ' ' 4 0.042 0.343 0.261 9 2 ' ' 5 0.042 0.843 0.739 9 2 ' ' 6 0.094 0.209 0.989 9 3 ' ' 7 0.094 0.709 0.011 9 2 ' ' 8 0.250 0.250 0.250 359 110 ' ' 9 0.250 0.750 0.750 359 110 ' ' 10 0.500 0.000 0.500 359 111 ' ' 11 0.500 0.500 0.500 359 111 ' ' 12 0.406 0.291 0.511 9 3 ' ' 13 0.406 0.791 0.489 9 3 ' ' 14 0.459 0.156 0.239 9 3 ' ' 15 0.459 0.656 0.761 9 3 ' ' 16 0.542 0.343 0.239 9 2 ' ' 17 0.542 0.843 0.761 9 2 ' ' 18 0.594 0.209 0.511 9 2 ' ' 19 0.594 0.709 0.489 9 3 ' ' 20 0.750 0.250 0.250 359 110 ' ' 21 0.750 0.750 0.750 359 110 ' ' 22 0.906 0.291 0.989 9 3 ' ' 23 0.906 0.791 0.011 9 3 ' ' 24 0.959 0.156 0.261 9 3 ' ' 25 0.959 0.656 0.739 9 3 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 952108'