# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'H. Xu' _publ_contact_author_email HAIBINGXU@FJIRSM.AC.CN _publ_section_title ; Syntheses, Structures and Photophysical Properties of Heterotrinuclear Zn2Ln Clusters (Ln = Nd, Eu, Tb, Er, Yb) ; loop_ _publ_author_name 'H. Xu' 'Xiao-Ming Chen' 'Zhong-Ning Chen' 'Wei-Xiong Zhang' 'Ye-Teng Zhong' # Attachment 'Zn2Nd-752291.cif' data_nd _database_code_depnum_ccdc_archive 'CCDC 752291' #TrackingRef 'Zn2Nd-752291.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H33.50 Cl F12 N4 Nd O10 Zn2' _chemical_formula_weight 1388.74 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' 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' F F 0.0171 0.0103 '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' Zn Zn 0.2839 1.4301 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.7227(18) _cell_length_b 18.4700(10) _cell_length_c 24.1252(13) _cell_angle_alpha 90.00 _cell_angle_beta 125.0233(8) _cell_angle_gamma 90.00 _cell_volume 12670.4(12) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8877 _cell_measurement_theta_min 2.383 _cell_measurement_theta_max 24.334 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5492 _exptl_absorpt_coefficient_mu 1.687 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.7860 _exptl_absorpt_correction_T_max 0.8630 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 CCD _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32525 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12444 _reflns_number_gt 8827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the weak interaction between the solvent molecules and the clusters, the solvent molecules are in severe disordered and with large Uiso values. Therefore, the non-H atoms of solvent molecules were refined in isotropic model with restrained thermal factors, and their occupancies are fixed to 0.5 according to the element analysis results. The total solvent accessible voids is 36 A**3 per independent unit in this structure. It is not verylarge, and no significant residual electron peaks was found in these sites. Therefore, no new solvent molecules were identified to further reduce the solvent accessible voids. the following restrains is used in the refinement 1) The CF3 groups are in disorder. Therefore, the ADPs of the related non-H atoms are restrained by using EADP and DELU commands, and their occupancies are refined by PART instructions. The related C-C, C-F bonds and the F...F distances are restrained to 1.49(1), 1.33(1) and 2.15(2) A respectively by DFIX command. 2) The solvent molecules are in severe disordered, so their non-H atoms ADPs are refined in isotropic model and restrained by EADP commands. The related C-C, C-Cl bonds and the C...C and Cl...Cl distances are fixed to 1.50(1), 1.74(1), 2.50(2) and 2.90(2) A respectively by DFIX command. 3) A disordered methyl group is refined in two parts with equal ADPs by PART instruction and EADP command. The related C-C bond is fixed to 1.49(1) A by DFIX command. After checking cif, some alert level_B were found: PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C104 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C107 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C109 Answer: These atoms are bonding with the C atoms of disorderd methyl groups, which have larger Ueq value. The highest residual electron densities are located in the position very close to the lanthanide atoms. This phenomenon is usually found in the lanthanide compounds caused by the series termination errors of heavy atoms. ; _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^)+(0.1190P)^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 12444 _refine_ls_number_parameters 719 _refine_ls_number_restraints 104 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1777 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.031 _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 Nd1 Nd 0.141683(8) 0.683226(15) 0.588419(13) 0.05893(13) Uani 1 1 d . . . Zn1 Zn 0.166444(19) 0.58367(3) 0.49632(3) 0.06472(18) Uani 1 1 d . . . Zn2 Zn 0.057869(18) 0.62783(3) 0.42977(3) 0.05812(17) Uani 1 1 d . . . N1 N 0.21859(18) 0.5062(3) 0.5477(3) 0.0863(14) Uani 1 1 d . . . N2 N 0.19533(14) 0.6465(2) 0.4559(2) 0.0664(11) Uani 1 1 d . . . N3 N 0.02175(12) 0.5371(2) 0.43014(18) 0.0557(9) Uani 1 1 d . . . N4 N 0.00314(15) 0.6976(2) 0.3670(2) 0.0691(11) Uani 1 1 d . . . O1 O 0.20596(10) 0.62557(19) 0.59784(17) 0.0678(9) Uani 1 1 d . . . O2 O 0.12961(11) 0.68364(16) 0.47569(17) 0.0600(8) Uani 1 1 d . . . O3 O 0.11253(10) 0.57120(17) 0.51944(16) 0.0593(8) Uani 1 1 d . . . O4 O 0.06013(11) 0.69668(18) 0.50218(16) 0.0589(8) Uani 1 1 d . . . O5 O 0.06158(13) 0.5898(2) 0.35357(17) 0.0776(10) Uani 1 1 d . C . O6 O 0.12666(14) 0.5224(2) 0.4122(2) 0.0823(11) Uani 1 1 d . C . O7 O 0.13603(15) 0.8130(2) 0.5691(2) 0.0822(12) Uani 1 1 d . . . O8 O 0.20749(13) 0.7461(2) 0.6860(2) 0.0927(13) Uani 1 1 d . . . O9 O 0.11148(14) 0.7212(2) 0.6539(2) 0.0825(10) Uani 1 1 d . B . O10 O 0.16601(13) 0.5982(2) 0.6813(2) 0.0815(11) Uani 1 1 d . B . C101 C 0.1301(3) 0.9368(4) 0.5710(4) 0.136(3) Uani 1 1 d D . . F1 F 0.1575(4) 0.9939(5) 0.5955(6) 0.162(3) Uani 0.543(6) 1 d PD A 1 F2 F 0.1036(5) 0.9352(6) 0.5040(5) 0.162(3) Uani 0.543(6) 1 d PD A 1 F3 F 0.0983(4) 0.9530(5) 0.5856(5) 0.162(3) Uani 0.543(6) 1 d PD A 1 F1B F 0.1356(5) 0.9953(6) 0.6052(7) 0.162(3) Uani 0.457(6) 1 d PD A 2 F2B F 0.1530(4) 0.9566(6) 0.5412(6) 0.162(3) Uani 0.457(6) 1 d PD A 2 F3B F 0.0851(4) 0.9335(8) 0.5181(7) 0.162(3) Uani 0.457(6) 1 d PD A 2 C15A C 0.2562(4) 0.8175(7) 0.7802(5) 0.163(3) Uani 0.573(8) 1 d PDU A 1 F4 F 0.2686(5) 0.8863(6) 0.7964(6) 0.159(2) Uani 0.573(8) 1 d PDU A 1 F5 F 0.2943(3) 0.7793(7) 0.7974(5) 0.159(2) Uani 0.573(8) 1 d PDU A 1 F6 F 0.2440(4) 0.7922(7) 0.8201(4) 0.159(2) Uani 0.573(8) 1 d PDU A 1 C15B C 0.2611(4) 0.8158(10) 0.7766(6) 0.163(3) Uani 0.427(8) 1 d PD A 2 F4B F 0.2676(7) 0.8735(9) 0.8143(8) 0.159(2) Uani 0.427(8) 1 d PD A 2 F5B F 0.2967(5) 0.8141(9) 0.7698(7) 0.159(2) Uani 0.427(8) 1 d PD A 2 F6B F 0.2701(6) 0.7609(8) 0.8190(6) 0.159(2) Uani 0.427(8) 1 d PD A 2 C16A C 0.1019(5) 0.7593(8) 0.7369(7) 0.163(3) Uani 0.491(9) 1 d PD B 1 F7 F 0.0904(6) 0.8262(8) 0.7106(7) 0.162(2) Uani 0.491(9) 1 d PD B 1 F8 F 0.0632(5) 0.7310(8) 0.7274(9) 0.162(2) Uani 0.491(9) 1 d PD B 1 F9 F 0.1319(5) 0.7716(8) 0.8035(6) 0.162(2) Uani 0.491(9) 1 d PD B 1 C16B C 0.0991(5) 0.7618(7) 0.7305(7) 0.163(3) Uani 0.509(9) 1 d PDU B 2 F7B F 0.1155(5) 0.8280(7) 0.7313(8) 0.162(2) Uani 0.509(9) 1 d PDU B 2 F8B F 0.0526(4) 0.7649(8) 0.6875(7) 0.162(2) Uani 0.509(9) 1 d PDU B 2 F9B F 0.1069(5) 0.7524(7) 0.7908(7) 0.162(2) Uani 0.509(9) 1 d PDU B 2 C11A C 0.2009(6) 0.5429(9) 0.7841(10) 0.179(4) Uani 0.284(7) 1 d PD B 1 F10 F 0.2100(9) 0.4837(11) 0.7607(10) 0.169(2) Uani 0.284(7) 1 d PD B 1 F11 F 0.2429(7) 0.5756(11) 0.8253(10) 0.169(2) Uani 0.284(7) 1 d PD B 1 F12 F 0.1888(8) 0.5163(13) 0.8236(13) 0.169(2) Uani 0.284(7) 1 d PD B 1 C11B C 0.1965(4) 0.5405(6) 0.7834(5) 0.179(4) Uani 0.716(7) 1 d PDU B 2 F10B F 0.1714(3) 0.4800(5) 0.7594(4) 0.169(2) Uani 0.716(7) 1 d PDU B 2 F11B F 0.2374(3) 0.5273(6) 0.7907(5) 0.169(2) Uani 0.716(7) 1 d PDU B 2 F12B F 0.2069(3) 0.5507(5) 0.8453(4) 0.169(2) Uani 0.716(7) 1 d PDU B 2 C1 C 0.2232(3) 0.4480(5) 0.5191(5) 0.130(3) Uani 1 1 d . . . H1A H 0.2000 0.4352 0.4743 0.156 Uiso 1 1 d R . . C2 C 0.2653(4) 0.4050(6) 0.5596(7) 0.170(5) Uani 1 1 d . . . H2A H 0.2689 0.3629 0.5414 0.203 Uiso 1 1 d R . . C3 C 0.2975(4) 0.4224(7) 0.6220(6) 0.159(4) Uani 1 1 d . . . H3A H 0.3256 0.3963 0.6467 0.191 Uiso 1 1 d R . . C4 C 0.2938(3) 0.4825(5) 0.6535(4) 0.108(2) Uani 1 1 d . . . C5 C 0.3260(3) 0.5032(6) 0.7227(5) 0.126(3) Uani 1 1 d . . . H5A H 0.3535 0.4765 0.7499 0.151 Uiso 1 1 d R . . C6 C 0.3173(2) 0.5600(5) 0.7456(4) 0.102(2) Uani 1 1 d . . . H6A H 0.3392 0.5724 0.7910 0.123 Uiso 1 1 d R . . C7 C 0.27720(19) 0.6029(4) 0.7064(3) 0.0878(19) Uani 1 1 d . . . H7A H 0.2725 0.6424 0.7262 0.105 Uiso 1 1 d R . . C8 C 0.24382(17) 0.5860(3) 0.6392(3) 0.0742(16) Uani 1 1 d . . . C9 C 0.2519(2) 0.5236(4) 0.6125(4) 0.0849(17) Uani 1 1 d . . . C10 C 0.2285(2) 0.6268(3) 0.4467(3) 0.0807(16) Uani 1 1 d . . . H10A H 0.2419 0.5807 0.4607 0.097 Uiso 1 1 d R . . C11 C 0.2432(3) 0.6732(4) 0.4169(4) 0.097(2) Uani 1 1 d . . . H11A H 0.2660 0.6578 0.4107 0.116 Uiso 1 1 d R . . C12 C 0.2249(2) 0.7389(4) 0.3973(3) 0.0870(18) Uani 1 1 d . . . H12A H 0.2350 0.7698 0.3773 0.104 Uiso 1 1 d R . . C13 C 0.18985(19) 0.7630(3) 0.4055(3) 0.0708(14) Uani 1 1 d . . . C14 C 0.1674(2) 0.8315(4) 0.3844(3) 0.0839(18) Uani 1 1 d . . . H14A H 0.1762 0.8650 0.3646 0.101 Uiso 1 1 d R . . C15 C 0.1343(2) 0.8493(3) 0.3954(3) 0.0830(17) Uani 1 1 d . . . H15A H 0.1201 0.8948 0.3815 0.100 Uiso 1 1 d R . . C16 C 0.1201(2) 0.7995(3) 0.4264(3) 0.0728(14) Uani 1 1 d . . . H16A H 0.0972 0.8129 0.4332 0.087 Uiso 1 1 d R . . C17 C 0.14070(16) 0.7328(3) 0.4463(2) 0.0597(12) Uani 1 1 d . . . C18 C 0.17603(16) 0.7136(3) 0.4357(2) 0.0598(12) Uani 1 1 d . . . C19 C -0.02310(17) 0.5217(3) 0.3860(2) 0.0667(13) Uani 1 1 d . . . H19A H -0.0425 0.5564 0.3536 0.080 Uiso 1 1 d R . . C20 C -0.04327(19) 0.4560(3) 0.3868(3) 0.0794(16) Uani 1 1 d . . . H20A H -0.0751 0.4473 0.3552 0.095 Uiso 1 1 d R . . C21 C -0.01566(19) 0.4053(3) 0.4333(3) 0.0733(15) Uani 1 1 d . . . H21A H -0.0286 0.3608 0.4330 0.088 Uiso 1 1 d R . . C22 C 0.03271(18) 0.4194(3) 0.4821(3) 0.0670(13) Uani 1 1 d . . . C23 C 0.0638(2) 0.3712(3) 0.5350(3) 0.0805(16) Uani 1 1 d . . . H23A H 0.0531 0.3259 0.5381 0.097 Uiso 1 1 d R . . C24 C 0.1095(2) 0.3912(3) 0.5789(3) 0.0822(17) Uani 1 1 d . . . H24A H 0.1298 0.3583 0.6129 0.099 Uiso 1 1 d R . . C25 C 0.12637(18) 0.4569(3) 0.5750(3) 0.0785(16) Uani 1 1 d . . . H25A H 0.1579 0.4680 0.6071 0.094 Uiso 1 1 d R . . C26 C 0.09793(15) 0.5056(3) 0.5253(2) 0.0572(11) Uani 1 1 d . . . C27 C 0.05026(15) 0.4875(3) 0.4786(2) 0.0551(11) Uani 1 1 d . . . C28 C -0.0248(2) 0.6960(4) 0.3003(3) 0.095(2) Uani 1 1 d . . . H28A H -0.0199 0.6611 0.2768 0.114 Uiso 1 1 d R . . C29 C -0.0635(3) 0.7426(5) 0.2632(4) 0.127(3) Uani 1 1 d . . . H29A H -0.0836 0.7394 0.2160 0.153 Uiso 1 1 d R . . C30 C -0.0718(3) 0.7921(5) 0.2962(4) 0.139(3) Uani 1 1 d . . . H30A H -0.0965 0.8249 0.2720 0.166 Uiso 1 1 d R . . C31 C -0.0428(3) 0.7965(5) 0.3671(4) 0.113(2) Uani 1 1 d . . . C32 C -0.0481(3) 0.8478(5) 0.4052(4) 0.136(3) Uani 1 1 d . . . H32A H -0.0728 0.8811 0.3842 0.163 Uiso 1 1 d R . . C33 C -0.0182(3) 0.8461(5) 0.4734(5) 0.129(3) Uani 1 1 d . . . H33A H -0.0214 0.8806 0.4989 0.154 Uiso 1 1 d R . . C34 C 0.0195(2) 0.7959(4) 0.5087(3) 0.0857(17) Uani 1 1 d . . . H34A H 0.0396 0.7961 0.5560 0.103 Uiso 1 1 d R . . C35 C 0.02624(17) 0.7467(3) 0.4730(3) 0.0652(13) Uani 1 1 d . . . C36 C -0.00451(19) 0.7473(3) 0.4019(3) 0.0704(14) Uani 1 1 d . . . C51 C 0.0884(2) 0.5403(4) 0.3577(3) 0.0802(15) Uani 1 1 d DU . . C52A C 0.0798(11) 0.515(2) 0.2923(8) 0.115(5) Uani 0.51(4) 1 d PDU C 1 H52A H 0.0854 0.5540 0.2716 0.173 Uiso 0.51(4) 1 calc PR C 1 H52B H 0.0478 0.4988 0.2623 0.173 Uiso 0.51(4) 1 calc PR C 1 H52C H 0.1007 0.4755 0.3012 0.173 Uiso 0.51(4) 1 calc PR C 1 C52B C 0.0697(10) 0.4878(17) 0.2993(12) 0.115(5) Uani 0.49(4) 1 d PDU C 2 H52D H 0.0623 0.4425 0.3107 0.173 Uiso 0.49(4) 1 calc PR C 2 H52E H 0.0931 0.4801 0.2906 0.173 Uiso 0.49(4) 1 calc PR C 2 H52F H 0.0418 0.5074 0.2596 0.173 Uiso 0.49(4) 1 calc PR C 2 C102 C 0.1532(2) 0.8680(3) 0.6053(3) 0.0877(17) Uani 1 1 d D A . C103 C 0.1904(2) 0.8713(4) 0.6717(4) 0.096(2) Uani 1 1 d . . . H10B H 0.1994 0.9162 0.6937 0.115 Uiso 1 1 d R A . C104 C 0.2160(2) 0.8098(4) 0.7067(3) 0.091(2) Uani 1 1 d D A . C107 C 0.1228(2) 0.7094(4) 0.7125(3) 0.0872(18) Uani 1 1 d D . . C108 C 0.1515(3) 0.6534(5) 0.7552(3) 0.0948(19) Uani 1 1 d . B . H10C H 0.1585 0.6513 0.7989 0.114 Uiso 1 1 d R . . C109 C 0.1704(2) 0.6028(4) 0.7364(3) 0.0839(17) Uani 1 1 d D . . C1A C -0.0170(17) 0.0149(12) 0.3632(19) 0.48(2) Uiso 0.50 1 d PD . . H1AA H 0.0023 0.0149 0.4118 0.719 Uiso 0.50 1 calc PR . . H1AB H -0.0365 -0.0275 0.3469 0.719 Uiso 0.50 1 calc PR . . H1AC H -0.0365 0.0573 0.3469 0.719 Uiso 0.50 1 calc PR . . C2A C 0.0135(11) 0.0149(12) 0.3382(9) 0.48(2) Uiso 0.50 1 d PD . . H2AA H 0.0335 -0.0276 0.3553 0.576 Uiso 0.50 1 calc PR . . H2AB H 0.0335 0.0574 0.3552 0.576 Uiso 0.50 1 calc PR . . C3A C -0.0153(6) 0.0149(12) 0.2626(9) 0.48(2) Uiso 0.50 1 d PD . . H3AA H -0.0354 0.0574 0.2455 0.576 Uiso 0.50 1 calc PR . . H3AB H -0.0353 -0.0276 0.2456 0.576 Uiso 0.50 1 calc PR . . C4A C 0.1401(12) 0.273(4) 0.460(5) 0.717(18) Uiso 0.50 1 d PD . . H4AA H 0.1569 0.2654 0.4390 0.860 Uiso 0.50 1 calc PR . . H4AB H 0.1590 0.3036 0.4989 0.860 Uiso 0.50 1 calc PR . . Cl1 Cl 0.0859(15) 0.3137(16) 0.402(2) 0.717(18) Uiso 0.50 1 d PD . . Cl2 Cl 0.1308(13) 0.1897(19) 0.4844(18) 0.717(18) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.04307(17) 0.0728(2) 0.04890(18) -0.00031(11) 0.01938(13) -0.01237(11) Zn1 0.0512(3) 0.0726(4) 0.0647(4) 0.0082(3) 0.0300(3) -0.0013(3) Zn2 0.0490(3) 0.0670(4) 0.0488(3) 0.0046(2) 0.0225(3) -0.0016(2) N1 0.070(3) 0.084(3) 0.090(4) 0.015(3) 0.037(3) 0.010(3) N2 0.052(2) 0.079(3) 0.065(3) 0.001(2) 0.032(2) -0.011(2) N3 0.045(2) 0.071(2) 0.047(2) 0.0031(18) 0.0241(17) -0.0047(17) N4 0.062(3) 0.082(3) 0.052(2) 0.014(2) 0.027(2) 0.010(2) O1 0.0382(16) 0.087(2) 0.061(2) 0.0104(17) 0.0188(15) -0.0028(15) O2 0.0520(18) 0.071(2) 0.0561(19) 0.0087(15) 0.0303(16) -0.0069(14) O3 0.0437(16) 0.0651(19) 0.0581(19) 0.0052(15) 0.0227(15) -0.0082(14) O4 0.0461(17) 0.070(2) 0.0534(19) 0.0034(15) 0.0244(15) -0.0019(15) O5 0.070(2) 0.106(3) 0.052(2) -0.0008(19) 0.0322(19) 0.004(2) O6 0.067(2) 0.088(3) 0.080(3) -0.007(2) 0.035(2) -0.003(2) O7 0.086(3) 0.081(3) 0.063(2) -0.0086(19) 0.033(2) -0.020(2) O8 0.059(2) 0.104(3) 0.076(3) -0.009(2) 0.016(2) -0.017(2) O9 0.071(2) 0.103(3) 0.066(2) -0.005(2) 0.036(2) -0.007(2) O10 0.064(2) 0.101(3) 0.074(3) 0.008(2) 0.037(2) -0.008(2) C101 0.188(10) 0.089(6) 0.154(9) -0.005(6) 0.111(8) -0.010(6) F1 0.193(6) 0.101(3) 0.144(4) -0.007(2) 0.069(4) 0.013(3) F2 0.193(6) 0.101(3) 0.144(4) -0.007(2) 0.069(4) 0.013(3) F3 0.193(6) 0.101(3) 0.144(4) -0.007(2) 0.069(4) 0.013(3) F1B 0.193(6) 0.101(3) 0.144(4) -0.007(2) 0.069(4) 0.013(3) F2B 0.193(6) 0.101(3) 0.144(4) -0.007(2) 0.069(4) 0.013(3) F3B 0.193(6) 0.101(3) 0.144(4) -0.007(2) 0.069(4) 0.013(3) C15A 0.084(5) 0.178(7) 0.138(8) -0.026(8) 0.012(6) -0.041(5) F4 0.108(3) 0.185(5) 0.092(4) -0.037(3) 0.003(3) -0.021(3) F5 0.108(3) 0.185(5) 0.092(4) -0.037(3) 0.003(3) -0.021(3) F6 0.108(3) 0.185(5) 0.092(4) -0.037(3) 0.003(3) -0.021(3) C15B 0.084(5) 0.178(7) 0.138(8) -0.026(8) 0.012(6) -0.041(5) F4B 0.108(3) 0.185(5) 0.092(4) -0.037(3) 0.003(3) -0.021(3) F5B 0.108(3) 0.185(5) 0.092(4) -0.037(3) 0.003(3) -0.021(3) F6B 0.108(3) 0.185(5) 0.092(4) -0.037(3) 0.003(3) -0.021(3) C16A 0.163(6) 0.212(9) 0.153(7) -0.078(9) 0.113(7) -0.057(9) F7 0.158(5) 0.198(4) 0.175(5) -0.045(4) 0.122(5) -0.012(4) F8 0.158(5) 0.198(4) 0.175(5) -0.045(4) 0.122(5) -0.012(4) F9 0.158(5) 0.198(4) 0.175(5) -0.045(4) 0.122(5) -0.012(4) C16B 0.163(6) 0.212(9) 0.153(7) -0.078(9) 0.113(7) -0.057(9) F7B 0.158(5) 0.198(4) 0.175(5) -0.045(4) 0.122(5) -0.012(4) F8B 0.158(5) 0.198(4) 0.175(5) -0.045(4) 0.122(5) -0.012(4) F9B 0.158(5) 0.198(4) 0.175(5) -0.045(4) 0.122(5) -0.012(4) C11A 0.121(7) 0.287(13) 0.108(6) 0.069(7) 0.053(7) -0.023(8) F10 0.167(5) 0.193(6) 0.133(4) 0.076(4) 0.078(4) 0.038(4) F11 0.167(5) 0.193(6) 0.133(4) 0.076(4) 0.078(4) 0.038(4) F12 0.167(5) 0.193(6) 0.133(4) 0.076(4) 0.078(4) 0.038(4) C11B 0.121(7) 0.287(13) 0.108(6) 0.069(7) 0.053(7) -0.023(8) F10B 0.167(5) 0.193(6) 0.133(4) 0.076(4) 0.078(4) 0.038(4) F11B 0.167(5) 0.193(6) 0.133(4) 0.076(4) 0.078(4) 0.038(4) F12B 0.167(5) 0.193(6) 0.133(4) 0.076(4) 0.078(4) 0.038(4) C1 0.154(8) 0.105(6) 0.118(7) 0.025(5) 0.071(6) 0.050(6) C2 0.164(10) 0.132(8) 0.187(12) 0.036(8) 0.086(9) 0.082(8) C3 0.117(8) 0.169(10) 0.140(9) 0.047(8) 0.044(7) 0.071(7) C4 0.081(5) 0.112(6) 0.117(6) 0.045(5) 0.048(5) 0.033(4) C5 0.073(5) 0.152(8) 0.111(7) 0.059(6) 0.029(5) 0.030(5) C6 0.062(4) 0.131(6) 0.082(5) 0.032(4) 0.023(3) -0.004(4) C7 0.053(3) 0.120(5) 0.064(3) 0.027(3) 0.018(3) -0.013(3) C8 0.045(3) 0.094(4) 0.071(3) 0.020(3) 0.026(3) -0.014(3) C9 0.069(4) 0.089(4) 0.092(5) 0.030(4) 0.043(4) 0.005(3) C10 0.069(3) 0.092(4) 0.087(4) 0.007(3) 0.048(3) 0.001(3) C11 0.081(4) 0.128(6) 0.099(5) -0.004(4) 0.062(4) -0.014(4) C12 0.074(4) 0.118(5) 0.082(4) 0.005(4) 0.052(3) -0.023(4) C13 0.062(3) 0.089(4) 0.057(3) 0.000(3) 0.031(3) -0.023(3) C14 0.082(4) 0.091(4) 0.070(4) 0.006(3) 0.040(3) -0.030(3) C15 0.089(4) 0.074(4) 0.075(4) 0.007(3) 0.041(3) -0.013(3) C16 0.069(3) 0.076(4) 0.069(3) 0.008(3) 0.037(3) -0.004(3) C17 0.053(3) 0.072(3) 0.041(2) 0.003(2) 0.020(2) -0.014(2) C18 0.051(3) 0.073(3) 0.048(3) -0.001(2) 0.023(2) -0.014(2) C19 0.050(3) 0.088(4) 0.048(3) 0.000(2) 0.020(2) -0.006(2) C20 0.050(3) 0.111(5) 0.060(3) -0.006(3) 0.022(3) -0.025(3) C21 0.062(3) 0.086(4) 0.066(3) -0.008(3) 0.033(3) -0.031(3) C22 0.056(3) 0.075(3) 0.066(3) 0.001(3) 0.033(3) -0.014(2) C23 0.067(3) 0.078(4) 0.089(4) 0.017(3) 0.040(3) -0.011(3) C24 0.068(4) 0.079(4) 0.085(4) 0.028(3) 0.035(3) 0.007(3) C25 0.045(3) 0.086(4) 0.077(4) 0.020(3) 0.019(2) 0.000(3) C26 0.042(2) 0.067(3) 0.054(3) 0.007(2) 0.023(2) -0.009(2) C27 0.049(2) 0.068(3) 0.050(3) 0.003(2) 0.030(2) -0.007(2) C28 0.089(4) 0.113(5) 0.055(3) 0.013(3) 0.025(3) 0.028(4) C29 0.121(6) 0.163(8) 0.060(4) 0.033(5) 0.030(4) 0.064(6) C30 0.118(7) 0.158(7) 0.083(5) 0.035(5) 0.023(5) 0.073(6) C31 0.101(5) 0.121(6) 0.093(5) 0.012(4) 0.040(4) 0.046(5) C32 0.117(6) 0.149(7) 0.087(5) 0.003(5) 0.026(5) 0.068(6) C33 0.133(7) 0.125(6) 0.123(7) -0.006(5) 0.071(6) 0.054(6) C34 0.065(4) 0.106(4) 0.072(4) 0.001(3) 0.031(3) 0.009(3) C35 0.053(3) 0.068(3) 0.068(3) 0.005(3) 0.030(3) 0.000(2) C36 0.062(3) 0.080(3) 0.060(3) 0.012(3) 0.029(3) 0.014(3) C51 0.069(4) 0.097(4) 0.076(4) -0.011(3) 0.042(3) -0.003(3) C52A 0.123(8) 0.135(10) 0.094(6) -0.010(7) 0.066(5) 0.017(8) C52B 0.123(8) 0.135(10) 0.094(6) -0.010(7) 0.066(5) 0.017(8) C102 0.094(4) 0.078(4) 0.087(4) -0.015(3) 0.050(4) -0.021(3) C103 0.086(4) 0.089(5) 0.087(5) -0.026(4) 0.035(4) -0.020(4) C104 0.065(4) 0.108(5) 0.081(4) -0.038(4) 0.031(3) -0.030(4) C107 0.084(4) 0.114(5) 0.070(4) -0.018(4) 0.047(4) -0.029(4) C108 0.088(4) 0.133(6) 0.058(4) -0.005(4) 0.039(3) -0.017(4) C109 0.067(3) 0.113(5) 0.052(3) 0.015(3) 0.023(3) -0.011(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 Nd1 O1 2.363(3) . ? Nd1 O4 2.376(3) . ? Nd1 O7 2.429(4) . ? Nd1 O8 2.436(4) . ? Nd1 O9 2.448(4) . ? Nd1 O10 2.455(4) . ? Nd1 O3 2.478(3) . ? Nd1 O2 2.503(3) . ? Nd1 Zn1 3.3540(7) . ? Nd1 Zn2 3.3735(6) . ? Zn1 O6 2.022(4) . ? Zn1 N1 2.071(5) . ? Zn1 N2 2.104(4) . ? Zn1 O2 2.136(3) . ? Zn1 O1 2.150(4) . ? Zn1 O3 2.251(3) . ? Zn2 O5 2.040(4) . ? Zn2 N4 2.065(4) . ? Zn2 N3 2.096(4) . ? Zn2 O4 2.125(3) . ? Zn2 O3 2.159(3) . ? Zn2 O2 2.308(3) . ? N1 C1 1.336(9) . ? N1 C9 1.346(8) . ? N2 C10 1.343(7) . ? N2 C18 1.359(7) . ? N3 C19 1.318(6) . ? N3 C27 1.363(6) . ? N4 C28 1.318(7) . ? N4 C36 1.371(7) . ? O1 C8 1.324(6) . ? O2 C17 1.337(5) . ? O3 C26 1.352(5) . ? O4 C35 1.335(6) . ? O5 C51 1.266(7) . ? O6 C51 1.265(7) . ? O7 C102 1.246(7) . ? O8 C104 1.246(7) . ? O9 C107 1.249(7) . ? O10 C109 1.252(7) . ? C101 F1B 1.306(9) . ? C101 F1 1.314(8) . ? C101 F2 1.325(8) . ? C101 F3B 1.336(9) . ? C101 F3 1.369(8) . ? C101 F2B 1.395(9) . ? C101 C102 1.475(7) . ? C15A F4 1.327(9) . ? C15A F5 1.337(9) . ? C15A F6 1.340(9) . ? C15A C104 1.508(9) . ? C15B F4B 1.333(9) . ? C15B F5B 1.339(9) . ? C15B F6B 1.344(9) . ? C15B C104 1.509(9) . ? C16A F8 1.331(9) . ? C16A F9 1.340(9) . ? C16A F7 1.340(9) . ? C16A C107 1.489(9) . ? C16B F8B 1.329(9) . ? C16B F9B 1.329(9) . ? C16B F7B 1.343(9) . ? C16B C107 1.487(9) . ? C11A F12 1.338(10) . ? C11A F11 1.348(10) . ? C11A F10 1.349(10) . ? C11A C109 1.507(9) . ? C11B F10B 1.327(9) . ? C11B F12B 1.332(8) . ? C11B F11B 1.348(9) . ? C11B C109 1.501(9) . ? C1 C2 1.442(12) . ? C1 H1A 0.9345 . ? C2 C3 1.299(14) . ? C2 H2A 0.9367 . ? C3 C4 1.393(13) . ? C3 H3A 0.9316 . ? C4 C9 1.421(9) . ? C4 C5 1.428(12) . ? C5 C6 1.300(12) . ? C5 H5A 0.9317 . ? C6 C7 1.395(9) . ? C6 H6A 0.9351 . ? C7 C8 1.383(8) . ? C7 H7A 0.9365 . ? C8 C9 1.425(9) . ? C10 C11 1.389(9) . ? C10 H10A 0.9353 . ? C11 C12 1.325(9) . ? C11 H11A 0.9316 . ? C12 C13 1.413(9) . ? C12 H12A 0.9359 . ? C13 C18 1.412(7) . ? C13 C14 1.419(9) . ? C14 C15 1.358(9) . ? C14 H14A 0.9351 . ? C15 C16 1.440(8) . ? C15 H15A 0.9351 . ? C16 C17 1.366(7) . ? C16 H16A 0.9314 . ? C17 C18 1.434(7) . ? C19 C20 1.406(7) . ? C19 H19A 0.9348 . ? C20 C21 1.350(8) . ? C20 H20A 0.9297 . ? C21 C22 1.416(7) . ? C21 H21A 0.9350 . ? C22 C23 1.416(7) . ? C22 C27 1.421(7) . ? C23 C24 1.360(8) . ? C23 H23A 0.9357 . ? C24 C25 1.374(8) . ? C24 H24A 0.9349 . ? C25 C26 1.364(7) . ? C25 H25A 0.9302 . ? C26 C27 1.407(6) . ? C28 C29 1.404(9) . ? C28 H28A 0.9365 . ? C29 C30 1.347(11) . ? C29 H29A 0.9356 . ? C30 C31 1.403(11) . ? C30 H30A 0.9323 . ? C31 C32 1.402(11) . ? C31 C36 1.422(8) . ? C32 C33 1.351(11) . ? C32 H32A 0.9325 . ? C33 C34 1.421(9) . ? C33 H33A 0.9366 . ? C34 C35 1.361(8) . ? C34 H34A 0.9358 . ? C35 C36 1.406(7) . ? C51 C52A 1.503(9) . ? C51 C52B 1.516(9) . ? C52A H52A 0.9600 . ? C52A H52B 0.9600 . ? C52A H52C 0.9600 . ? C52B H52D 0.9600 . ? C52B H52E 0.9600 . ? C52B H52F 0.9600 . ? C102 C103 1.365(9) . ? C103 C104 1.390(9) . ? C103 H10B 0.9364 . ? C107 C108 1.394(10) . ? C108 C109 1.360(10) . ? C108 H10C 0.9369 . ? C1A C2A 1.489(10) . ? C1A H1AA 0.9600 . ? C1A H1AB 0.9600 . ? C1A H1AC 0.9600 . ? C2A C3A 1.495(10) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A C3A 1.496(10) 2 ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C4A Cl2 1.739(10) . ? C4A Cl1 1.747(10) . ? C4A H4AA 0.9700 . ? C4A H4AB 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nd1 O4 135.76(12) . . ? O1 Nd1 O7 115.53(14) . . ? O4 Nd1 O7 78.71(13) . . ? O1 Nd1 O8 79.12(14) . . ? O4 Nd1 O8 141.42(13) . . ? O7 Nd1 O8 69.07(14) . . ? O1 Nd1 O9 142.93(13) . . ? O4 Nd1 O9 78.38(12) . . ? O7 Nd1 O9 79.84(15) . . ? O8 Nd1 O9 75.61(15) . . ? O1 Nd1 O10 79.19(12) . . ? O4 Nd1 O10 118.62(12) . . ? O7 Nd1 O10 138.97(14) . . ? O8 Nd1 O10 77.43(14) . . ? O9 Nd1 O10 69.20(14) . . ? O1 Nd1 O3 71.80(11) . . ? O4 Nd1 O3 71.16(11) . . ? O7 Nd1 O3 137.60(12) . . ? O8 Nd1 O3 147.32(13) . . ? O9 Nd1 O3 120.77(12) . . ? O10 Nd1 O3 82.68(12) . . ? O1 Nd1 O2 70.48(11) . . ? O4 Nd1 O2 71.09(11) . . ? O7 Nd1 O2 81.01(12) . . ? O8 Nd1 O2 121.85(13) . . ? O9 Nd1 O2 146.52(12) . . ? O10 Nd1 O2 138.49(13) . . ? O3 Nd1 O2 61.56(10) . . ? O1 Nd1 Zn1 39.62(8) . . ? O4 Nd1 Zn1 96.14(8) . . ? O7 Nd1 Zn1 115.93(11) . . ? O8 Nd1 Zn1 116.51(12) . . ? O9 Nd1 Zn1 162.27(10) . . ? O10 Nd1 Zn1 99.72(10) . . ? O3 Nd1 Zn1 42.16(7) . . ? O2 Nd1 Zn1 39.52(7) . . ? O1 Nd1 Zn2 97.16(8) . . ? O4 Nd1 Zn2 38.72(8) . . ? O7 Nd1 Zn2 99.18(10) . . ? O8 Nd1 Zn2 163.89(11) . . ? O9 Nd1 Zn2 114.15(9) . . ? O10 Nd1 Zn2 117.53(10) . . ? O3 Nd1 Zn2 39.73(7) . . ? O2 Nd1 Zn2 43.16(7) . . ? Zn1 Nd1 Zn2 57.612(15) . . ? O6 Zn1 N1 94.2(2) . . ? O6 Zn1 N2 94.38(17) . . ? N1 Zn1 N2 99.94(19) . . ? O6 Zn1 O2 106.08(15) . . ? N1 Zn1 O2 159.74(19) . . ? N2 Zn1 O2 78.24(15) . . ? O6 Zn1 O1 165.09(15) . . ? N1 Zn1 O1 78.48(19) . . ? N2 Zn1 O1 99.62(15) . . ? O2 Zn1 O1 81.93(13) . . ? O6 Zn1 O3 90.28(14) . . ? N1 Zn1 O3 110.32(17) . . ? N2 Zn1 O3 148.96(15) . . ? O2 Zn1 O3 70.99(11) . . ? O1 Zn1 O3 80.35(12) . . ? O6 Zn1 Nd1 133.17(12) . . ? N1 Zn1 Nd1 116.84(17) . . ? N2 Zn1 Nd1 112.11(13) . . ? O2 Zn1 Nd1 48.21(9) . . ? O1 Zn1 Nd1 44.50(9) . . ? O3 Zn1 Nd1 47.64(8) . . ? O5 Zn2 N4 93.55(17) . . ? O5 Zn2 N3 94.35(15) . . ? N4 Zn2 N3 101.59(17) . . ? O5 Zn2 O4 162.76(15) . . ? N4 Zn2 O4 79.24(16) . . ? N3 Zn2 O4 102.40(14) . . ? O5 Zn2 O3 105.20(15) . . ? N4 Zn2 O3 161.24(16) . . ? N3 Zn2 O3 78.02(13) . . ? O4 Zn2 O3 82.52(12) . . ? O5 Zn2 O2 88.71(14) . . ? N4 Zn2 O2 111.03(15) . . ? N3 Zn2 O2 146.99(13) . . ? O4 Zn2 O2 79.50(12) . . ? O3 Zn2 O2 69.49(11) . . ? O5 Zn2 Nd1 131.86(11) . . ? N4 Zn2 Nd1 118.31(13) . . ? N3 Zn2 Nd1 111.49(10) . . ? O4 Zn2 Nd1 44.37(8) . . ? O3 Zn2 Nd1 47.19(8) . . ? O2 Zn2 Nd1 47.88(8) . . ? C1 N1 C9 121.0(6) . . ? C1 N1 Zn1 124.8(5) . . ? C9 N1 Zn1 113.7(4) . . ? C10 N2 C18 118.7(5) . . ? C10 N2 Zn1 127.6(4) . . ? C18 N2 Zn1 113.6(3) . . ? C19 N3 C27 119.2(4) . . ? C19 N3 Zn2 127.0(3) . . ? C27 N3 Zn2 113.6(3) . . ? C28 N4 C36 119.9(5) . . ? C28 N4 Zn2 127.1(4) . . ? C36 N4 Zn2 112.9(3) . . ? C8 O1 Zn1 111.6(4) . . ? C8 O1 Nd1 142.7(3) . . ? Zn1 O1 Nd1 95.88(11) . . ? C17 O2 Zn1 113.2(3) . . ? C17 O2 Zn2 127.5(3) . . ? Zn1 O2 Zn2 93.59(11) . . ? C17 O2 Nd1 131.2(3) . . ? Zn1 O2 Nd1 92.27(11) . . ? Zn2 O2 Nd1 88.95(11) . . ? C26 O3 Zn2 111.9(2) . . ? C26 O3 Zn1 122.2(3) . . ? Zn2 O3 Zn1 94.59(12) . . ? C26 O3 Nd1 135.3(3) . . ? Zn2 O3 Nd1 93.08(11) . . ? Zn1 O3 Nd1 90.21(10) . . ? C35 O4 Zn2 112.0(3) . . ? C35 O4 Nd1 141.3(3) . . ? Zn2 O4 Nd1 96.92(13) . . ? C51 O5 Zn2 126.9(4) . . ? C51 O6 Zn1 127.1(4) . . ? C102 O7 Nd1 135.8(4) . . ? C104 O8 Nd1 135.4(4) . . ? C107 O9 Nd1 135.0(4) . . ? C109 O10 Nd1 134.0(4) . . ? F1B C101 F1 40.8(8) . . ? F1B C101 F2 122.5(10) . . ? F1 C101 F2 112.5(9) . . ? F1B C101 F3B 108.0(9) . . ? F1 C101 F3B 127.9(10) . . ? F2 C101 F3B 38.8(8) . . ? F1B C101 F3 60.3(8) . . ? F1 C101 F3 101.0(8) . . ? F2 C101 F3 102.8(9) . . ? F3B C101 F3 65.4(8) . . ? F1B C101 F2B 100.8(9) . . ? F1 C101 F2B 62.6(7) . . ? F2 C101 F2B 65.0(8) . . ? F3B C101 F2B 102.7(10) . . ? F3 C101 F2B 149.1(8) . . ? F1B C101 C102 121.5(9) . . ? F1 C101 C102 114.7(8) . . ? F2 C101 C102 116.0(8) . . ? F3B C101 C102 117.3(9) . . ? F3 C101 C102 107.7(7) . . ? F2B C101 C102 103.1(8) . . ? F4 C15A F5 108.6(10) . . ? F4 C15A F6 107.7(11) . . ? F5 C15A F6 104.9(10) . . ? F4 C15A C104 111.3(10) . . ? F5 C15A C104 113.6(9) . . ? F6 C15A C104 110.5(9) . . ? F4B C15B F5B 107.2(12) . . ? F4B C15B F6B 102.2(11) . . ? F5B C15B F6B 104.3(12) . . ? F4B C15B C104 118.9(13) . . ? F5B C15B C104 107.5(11) . . ? F6B C15B C104 115.7(12) . . ? F8 C16A F9 106.7(11) . . ? F8 C16A F7 106.5(11) . . ? F9 C16A F7 103.1(11) . . ? F8 C16A C107 111.1(10) . . ? F9 C16A C107 111.0(11) . . ? F7 C16A C107 117.6(12) . . ? F8B C16B F9B 104.7(10) . . ? F8B C16B F7B 106.7(11) . . ? F9B C16B F7B 106.5(11) . . ? F8B C16B C107 115.3(11) . . ? F9B C16B C107 115.8(11) . . ? F7B C16B C107 107.3(11) . . ? F12 C11A F11 106.8(14) . . ? F12 C11A F10 104.2(12) . . ? F11 C11A F10 105.0(13) . . ? F12 C11A C109 116.2(16) . . ? F11 C11A C109 103.0(14) . . ? F10 C11A C109 120.5(16) . . ? F10B C11B F12B 107.3(9) . . ? F10B C11B F11B 106.5(10) . . ? F12B C11B F11B 106.9(9) . . ? F10B C11B C109 110.8(8) . . ? F12B C11B C109 113.3(9) . . ? F11B C11B C109 111.8(8) . . ? N1 C1 C2 117.9(9) . . ? N1 C1 H1A 121.3 . . ? C2 C1 H1A 120.8 . . ? C3 C2 C1 120.9(10) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.6 . . ? C2 C3 C4 122.7(9) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 117.0 . . ? C3 C4 C9 115.2(8) . . ? C3 C4 C5 126.5(8) . . ? C9 C4 C5 118.2(8) . . ? C6 C5 C4 119.7(7) . . ? C6 C5 H5A 121.5 . . ? C4 C5 H5A 118.7 . . ? C5 C6 C7 123.7(8) . . ? C5 C6 H6A 117.6 . . ? C7 C6 H6A 118.7 . . ? C8 C7 C6 120.3(8) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 119.6 . . ? O1 C8 C7 124.1(6) . . ? O1 C8 C9 118.3(5) . . ? C7 C8 C9 117.6(6) . . ? N1 C9 C4 122.3(7) . . ? N1 C9 C8 117.3(5) . . ? C4 C9 C8 120.4(7) . . ? N2 C10 C11 121.5(6) . . ? N2 C10 H10A 118.8 . . ? C11 C10 H10A 119.6 . . ? C12 C11 C10 120.4(6) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 120.9(6) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.3 . . ? C18 C13 C12 116.4(6) . . ? C18 C13 C14 118.8(5) . . ? C12 C13 C14 124.8(5) . . ? C15 C14 C13 119.9(5) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 121.8(6) . . ? C14 C15 H15A 118.8 . . ? C16 C15 H15A 119.4 . . ? C17 C16 C15 119.5(6) . . ? C17 C16 H16A 120.3 . . ? C15 C16 H16A 120.2 . . ? O2 C17 C16 123.1(5) . . ? O2 C17 C18 117.6(4) . . ? C16 C17 C18 119.3(5) . . ? N2 C18 C13 122.0(5) . . ? N2 C18 C17 117.2(4) . . ? C13 C18 C17 120.8(5) . . ? N3 C19 C20 122.8(5) . . ? N3 C19 H19A 118.6 . . ? C20 C19 H19A 118.5 . . ? C21 C20 C19 119.2(5) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.5 . . ? C20 C21 C22 120.1(5) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 120.2 . . ? C21 C22 C23 124.2(5) . . ? C21 C22 C27 117.2(5) . . ? C23 C22 C27 118.6(4) . . ? C24 C23 C22 118.5(5) . . ? C24 C23 H23A 121.4 . . ? C22 C23 H23A 120.1 . . ? C23 C24 C25 122.6(5) . . ? C23 C24 H24A 117.4 . . ? C25 C24 H24A 119.9 . . ? C26 C25 C24 121.4(5) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 118.7 . . ? O3 C26 C25 123.8(4) . . ? O3 C26 C27 117.9(4) . . ? C25 C26 C27 118.2(4) . . ? N3 C27 C26 117.9(4) . . ? N3 C27 C22 121.4(4) . . ? C26 C27 C22 120.7(4) . . ? N4 C28 C29 121.9(7) . . ? N4 C28 H28A 119.6 . . ? C29 C28 H28A 118.3 . . ? C30 C29 C28 119.3(7) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.7 . . ? C29 C30 C31 120.9(7) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 119.0 . . ? C32 C31 C30 124.5(7) . . ? C32 C31 C36 118.3(7) . . ? C30 C31 C36 117.1(7) . . ? C33 C32 C31 118.9(7) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.9 . . ? C32 C33 C34 123.0(7) . . ? C32 C33 H33A 119.1 . . ? C34 C33 H33A 117.8 . . ? C35 C34 C33 119.3(6) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 120.9 . . ? O4 C35 C34 123.2(5) . . ? O4 C35 C36 118.1(5) . . ? C34 C35 C36 118.7(5) . . ? N4 C36 C35 117.7(5) . . ? N4 C36 C31 120.7(6) . . ? C35 C36 C31 121.6(6) . . ? O6 C51 O5 123.8(5) . . ? O6 C51 C52A 117.8(11) . . ? O5 C51 C52A 116.7(12) . . ? O6 C51 C52B 115.7(12) . . ? O5 C51 C52B 119.1(11) . . ? C52A C51 C52B 26.3(12) . . ? C51 C52A H52A 109.5 . . ? C51 C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C51 C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C51 C52B H52D 109.5 . . ? C51 C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C51 C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? O7 C102 C103 127.4(6) . . ? O7 C102 C101 114.9(6) . . ? C103 C102 C101 117.6(6) . . ? C102 C103 C104 121.4(6) . . ? C102 C103 H10B 119.2 . . ? C104 C103 H10B 119.3 . . ? O8 C104 C103 127.4(6) . . ? O8 C104 C15A 114.0(8) . . ? C103 C104 C15A 118.3(7) . . ? O8 C104 C15B 111.9(9) . . ? C103 C104 C15B 120.6(9) . . ? C15A C104 C15B 8.8(9) . . ? O9 C107 C108 126.4(6) . . ? O9 C107 C16B 110.4(8) . . ? C108 C107 C16B 123.2(8) . . ? O9 C107 C16A 115.5(8) . . ? C108 C107 C16A 118.1(8) . . ? C16B C107 C16A 5.2(9) . . ? C109 C108 C107 122.7(6) . . ? C109 C108 H10C 118.9 . . ? C107 C108 H10C 118.4 . . ? O10 C109 C108 127.8(6) . . ? O10 C109 C11B 113.8(7) . . ? C108 C109 C11B 118.2(7) . . ? O10 C109 C11A 111.4(10) . . ? C108 C109 C11A 120.9(11) . . ? C11B C109 C11A 5.8(10) . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C1A C2A C3A 111.1(16) . . ? C1A C2A H2AA 109.4 . . ? C3A C2A H2AA 109.4 . . ? C1A C2A H2AB 109.4 . . ? C3A C2A H2AB 109.4 . . ? H2AA C2A H2AB 108.0 . . ? C2A C3A C3A 111.2(16) . 2 ? C2A C3A H3AA 109.4 . . ? C3A C3A H3AA 109.4 2 . ? C2A C3A H3AB 109.4 . . ? C3A C3A H3AB 109.4 2 . ? H3AA C3A H3AB 108.0 . . ? Cl2 C4A Cl1 109.2(13) . . ? Cl2 C4A H4AA 109.8 . . ? Cl1 C4A H4AA 109.8 . . ? Cl2 C4A H4AB 109.9 . . ? Cl1 C4A H4AB 109.9 . . ? H4AA C4A H4AB 108.3 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.042 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.171 # Attachment 'Zm2Eu-752292.cif' data_eu _database_code_depnum_ccdc_archive 'CCDC 752292' #TrackingRef 'Zm2Eu-752292.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H33.50 Cl Eu F12 N4 O10 Zn2' _chemical_formula_weight 1396.46 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' 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' F F 0.0171 0.0103 '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' Zn Zn 0.2839 1.4301 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.7248(15) _cell_length_b 18.3371(8) _cell_length_c 23.9455(11) _cell_angle_alpha 90.00 _cell_angle_beta 124.9360(10) _cell_angle_gamma 90.00 _cell_volume 12499.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8565 _cell_measurement_theta_min 2.331 _cell_measurement_theta_max 26.013 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5516 _exptl_absorpt_coefficient_mu 1.883 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.7654 _exptl_absorpt_correction_T_max 0.8488 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 CCD _diffrn_measurement_method '/w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33696 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12279 _reflns_number_gt 8513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the weak interaction between the solvent molecules and the clusters, the solvent molecules are in severe disordered and with large Uiso values. Therefore, the non-H atoms of solvent molecules were refined in isotropic model with restrained thermal factors, and their occupancies are fixed to 0.5 according to the element analysis results. The total solvent accessible voids is 81 A**3 per independent in this structure. It is not verylarge, and no significant residual electron peaks was found in these sites. Therefore, no new solvent molecules were identified to further reduce the solvent accessible voids. the following restrains is used in the refinement 1) The CF3 groups are in disorder. Therefore, the ADPs of the related non-H atoms are restrained by using EADP and DELU commands, and their occupancies are refined by PART instructions. The related C-C, C-F bonds and the F...F distances are restrained to 1.49(1), 1.33(1) and 2.15(2) A respectively by DFIX command. 2) The solvent molecules are in severe disordered, so their non-H atoms ADPs are refined in isotropic model and restrained by EADP commands. The related C-C, C-Cl bonds and the C...C and Cl...Cl distances are fixed to 1.50(1), 1.74(1), 2.50(2) and 2.90(2) A respectively by DFIX command. 3) A disordered methyl group is refined in two parts with equal ADPs by PART instruction and EADP command. The related C-C bond is fixed to 1.49(1) A by DFIX command. After checking cif, some alert level_B were found: PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C107 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C109 Answer: These atoms are bonding with the C atoms of disorderd methyl groups, which have larger Ueq value. Cl2 is positioned too close to H2AB. But the occupancies of Cl2 and H2AB are 0.5, so both sites would not be occupied at the same time. The highest residual electron densities are located in the position very close to the lanthanide atoms. This phenomenon is usually found in the lanthanide compounds caused by the series termination errors of heavy atoms. ; _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^)+(0.0981P)^2^+1.2424P] 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 12279 _refine_ls_number_parameters 719 _refine_ls_number_restraints 110 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.142021(8) 0.681500(15) 0.588753(13) 0.05550(12) Uani 1 1 d . . . Zn1 Zn 0.16660(2) 0.58231(4) 0.49672(3) 0.06163(19) Uani 1 1 d . . . Zn2 Zn 0.05847(2) 0.62737(3) 0.43078(3) 0.05682(18) Uani 1 1 d . . . N1 N 0.21855(19) 0.5046(3) 0.5480(3) 0.0805(15) Uani 1 1 d . . . N2 N 0.19557(15) 0.6454(3) 0.4558(2) 0.0636(12) Uani 1 1 d . . . N3 N 0.02205(14) 0.5361(2) 0.4310(2) 0.0554(10) Uani 1 1 d . . . N4 N 0.00419(17) 0.6986(3) 0.3681(2) 0.0657(12) Uani 1 1 d . . . O1 O 0.20561(11) 0.6246(2) 0.59853(18) 0.0638(10) Uani 1 1 d . . . O2 O 0.13018(12) 0.68347(18) 0.47715(18) 0.0580(9) Uani 1 1 d . . . O3 O 0.11272(11) 0.57060(18) 0.52088(17) 0.0562(9) Uani 1 1 d . . . O4 O 0.06166(11) 0.69685(19) 0.50415(18) 0.0560(9) Uani 1 1 d . . . O5 O 0.06203(15) 0.5882(3) 0.35392(19) 0.0760(11) Uani 1 1 d . C . O6 O 0.12656(14) 0.5198(2) 0.4125(2) 0.0781(11) Uani 1 1 d . C . O7 O 0.13688(16) 0.8102(2) 0.5692(2) 0.0793(12) Uani 1 1 d . . . O8 O 0.20696(13) 0.7417(3) 0.6871(2) 0.0826(13) Uani 1 1 d . . . O9 O 0.11238(14) 0.7200(2) 0.6535(2) 0.0763(11) Uani 1 1 d . B . O10 O 0.16584(14) 0.5957(2) 0.6800(2) 0.0752(11) Uani 1 1 d . B . C101 C 0.1320(3) 0.9356(4) 0.5713(4) 0.124(3) Uani 1 1 d D . . F1 F 0.1603(4) 0.9915(5) 0.5943(6) 0.148(2) Uani 0.564(6) 1 d PD A 1 F2 F 0.1040(4) 0.9333(6) 0.5037(5) 0.148(2) Uani 0.564(6) 1 d PD A 1 F3 F 0.1022(4) 0.9556(5) 0.5896(5) 0.148(2) Uani 0.564(6) 1 d PD A 1 F1B F 0.1381(5) 0.9941(7) 0.6062(6) 0.148(2) Uani 0.436(6) 1 d PD A 2 F2B F 0.1555(4) 0.9560(6) 0.5419(6) 0.148(2) Uani 0.436(6) 1 d PD A 2 F3B F 0.0872(4) 0.9331(8) 0.5164(7) 0.148(2) Uani 0.436(6) 1 d PD A 2 C15A C 0.2549(4) 0.8117(8) 0.7830(5) 0.144(3) Uani 0.540(8) 1 d PDU A 1 F4 F 0.2678(6) 0.8813(7) 0.7992(7) 0.145(2) Uani 0.540(8) 1 d PDU A 1 F5 F 0.2929(4) 0.7719(7) 0.8028(6) 0.145(2) Uani 0.540(8) 1 d PDU A 1 F6 F 0.2415(4) 0.7887(7) 0.8227(5) 0.145(2) Uani 0.540(8) 1 d PDU A 1 C15B C 0.2601(4) 0.8109(9) 0.7793(5) 0.144(3) Uani 0.460(8) 1 d PD A 2 F4B F 0.2676(7) 0.8712(9) 0.8157(8) 0.145(2) Uani 0.460(8) 1 d PD A 2 F5B F 0.2960(4) 0.8047(8) 0.7734(7) 0.145(2) Uani 0.460(8) 1 d PD A 2 F6B F 0.2662(5) 0.7569(8) 0.8216(6) 0.145(2) Uani 0.460(8) 1 d PD A 2 C16A C 0.1020(5) 0.7565(7) 0.7368(7) 0.152(3) Uani 0.494(9) 1 d PDU B 1 F7 F 0.0903(5) 0.8220(7) 0.7064(7) 0.1446(18) Uani 0.494(9) 1 d PDU B 1 F8 F 0.0629(5) 0.7290(7) 0.7264(8) 0.1446(18) Uani 0.494(9) 1 d PDU B 1 F9 F 0.1303(4) 0.7705(8) 0.8033(6) 0.1446(18) Uani 0.494(9) 1 d PDU B 1 C16B C 0.0996(5) 0.7576(7) 0.7323(7) 0.152(3) Uani 0.506(9) 1 d PDU B 2 F7B F 0.1140(5) 0.8261(7) 0.7341(7) 0.1446(18) Uani 0.506(9) 1 d PDU B 2 F8B F 0.0528(4) 0.7593(8) 0.6875(6) 0.1446(18) Uani 0.506(9) 1 d PDU B 2 F9B F 0.1059(5) 0.7449(7) 0.7915(6) 0.1446(18) Uani 0.506(9) 1 d PDU B 2 C11A C 0.2008(6) 0.5399(8) 0.7846(9) 0.163(4) Uani 0.341(6) 1 d PD B 1 F10 F 0.2075(8) 0.4792(9) 0.7596(8) 0.156(2) Uani 0.341(6) 1 d PD B 1 F11 F 0.2436(6) 0.5702(9) 0.8255(9) 0.156(2) Uani 0.341(6) 1 d PD B 1 F12 F 0.1886(7) 0.5153(11) 0.8250(11) 0.156(2) Uani 0.341(6) 1 d PD B 1 C11B C 0.1965(4) 0.5369(6) 0.7826(6) 0.163(4) Uani 0.659(6) 1 d PDU B 2 F10B F 0.1702(3) 0.4773(5) 0.7604(4) 0.156(2) Uani 0.659(6) 1 d PDU B 2 F11B F 0.2357(3) 0.5203(6) 0.7864(5) 0.156(2) Uani 0.659(6) 1 d PDU B 2 F12B F 0.2088(4) 0.5470(6) 0.8459(5) 0.156(2) Uani 0.659(6) 1 d PDU B 2 C1 C 0.2243(3) 0.4475(5) 0.5205(5) 0.120(3) Uani 1 1 d . . . H1A H 0.2010 0.4348 0.4757 0.144 Uiso 1 1 d R . . C2 C 0.2655(4) 0.4022(6) 0.5581(7) 0.162(5) Uani 1 1 d . . . H2A H 0.2691 0.3601 0.5399 0.195 Uiso 1 1 d R . . C3 C 0.2986(4) 0.4227(6) 0.6220(6) 0.143(4) Uani 1 1 d . . . H3A H 0.3266 0.3966 0.6467 0.172 Uiso 1 1 d R . . C4 C 0.2944(3) 0.4827(4) 0.6544(5) 0.098(2) Uani 1 1 d . . . C5 C 0.3269(3) 0.5038(6) 0.7233(5) 0.117(3) Uani 1 1 d . . . H5A H 0.3544 0.4771 0.7505 0.140 Uiso 1 1 d R . . C6 C 0.3176(2) 0.5612(5) 0.7472(4) 0.098(3) Uani 1 1 d . . . H6A H 0.3395 0.5735 0.7926 0.117 Uiso 1 1 d R . . C7 C 0.27699(19) 0.6036(4) 0.7078(3) 0.0806(19) Uani 1 1 d . . . H7A H 0.2723 0.6431 0.7276 0.097 Uiso 1 1 d R . . C8 C 0.24374(18) 0.5856(3) 0.6406(3) 0.0666(16) Uani 1 1 d . . . C9 C 0.2519(2) 0.5228(4) 0.6133(4) 0.0808(19) Uani 1 1 d . . . C10 C 0.2280(2) 0.6262(4) 0.4461(3) 0.0771(17) Uani 1 1 d . . . H10A H 0.2414 0.5801 0.4601 0.093 Uiso 1 1 d R . . C11 C 0.2434(3) 0.6720(5) 0.4163(4) 0.093(2) Uani 1 1 d . . . H11A H 0.2662 0.6565 0.4100 0.111 Uiso 1 1 d R . . C12 C 0.2242(2) 0.7392(5) 0.3964(4) 0.088(2) Uani 1 1 d . . . H12A H 0.2343 0.7700 0.3763 0.106 Uiso 1 1 d R . . C13 C 0.1894(2) 0.7633(4) 0.4045(3) 0.0678(15) Uani 1 1 d . . . C14 C 0.1677(2) 0.8320(4) 0.3842(3) 0.0807(19) Uani 1 1 d . . . H14A H 0.1765 0.8655 0.3644 0.097 Uiso 1 1 d R . . C15 C 0.1344(2) 0.8501(4) 0.3950(3) 0.0772(18) Uani 1 1 d . . . H15A H 0.1202 0.8957 0.3811 0.093 Uiso 1 1 d R . . C16 C 0.1205(2) 0.7997(3) 0.4266(3) 0.0686(15) Uani 1 1 d . . . H16A H 0.0976 0.8131 0.4334 0.082 Uiso 1 1 d R . . C17 C 0.14082(18) 0.7325(3) 0.4465(2) 0.0569(13) Uani 1 1 d . . . C18 C 0.17587(18) 0.7134(3) 0.4355(3) 0.0577(13) Uani 1 1 d . . . C19 C -0.02279(19) 0.5212(3) 0.3867(3) 0.0677(15) Uani 1 1 d . . . H19A H -0.0422 0.5559 0.3543 0.081 Uiso 1 1 d R . . C20 C -0.0420(2) 0.4537(4) 0.3876(3) 0.0770(18) Uani 1 1 d . . . H20A H -0.0739 0.4450 0.3560 0.092 Uiso 1 1 d R . . C21 C -0.0153(2) 0.4032(4) 0.4331(3) 0.0722(16) Uani 1 1 d . . . H21A H -0.0282 0.3586 0.4327 0.087 Uiso 1 1 d R . . C22 C 0.03297(19) 0.4168(3) 0.4821(3) 0.0648(14) Uani 1 1 d . . . C23 C 0.0638(2) 0.3685(3) 0.5336(3) 0.0781(18) Uani 1 1 d . . . H23A H 0.0530 0.3233 0.5368 0.094 Uiso 1 1 d R . . C24 C 0.1090(2) 0.3870(3) 0.5788(3) 0.085(2) Uani 1 1 d . . . H24A H 0.1293 0.3541 0.6128 0.102 Uiso 1 1 d R . . C25 C 0.1262(2) 0.4550(3) 0.5760(3) 0.0731(17) Uani 1 1 d . . . H25A H 0.1577 0.4661 0.6080 0.088 Uiso 1 1 d R . . C26 C 0.09817(16) 0.5042(3) 0.5268(3) 0.0542(12) Uani 1 1 d . . . C27 C 0.05011(16) 0.4859(3) 0.4790(3) 0.0529(12) Uani 1 1 d . . . C28 C -0.0241(3) 0.6967(4) 0.3016(3) 0.093(2) Uani 1 1 d . . . H28A H -0.0192 0.6618 0.2780 0.112 Uiso 1 1 d R . . C29 C -0.0624(3) 0.7464(5) 0.2646(4) 0.123(3) Uani 1 1 d . . . H29A H -0.0825 0.7431 0.2174 0.148 Uiso 1 1 d R . . C30 C -0.0696(3) 0.7963(6) 0.2979(5) 0.131(4) Uani 1 1 d . . . H30A H -0.0943 0.8290 0.2737 0.157 Uiso 1 1 d R . . C31 C -0.0394(3) 0.8017(5) 0.3697(4) 0.103(3) Uani 1 1 d . . . C32 C -0.0444(3) 0.8514(5) 0.4092(5) 0.127(3) Uani 1 1 d . . . H32A H -0.0690 0.8847 0.3882 0.153 Uiso 1 1 d R . . C33 C -0.0137(3) 0.8509(5) 0.4780(4) 0.114(3) Uani 1 1 d . . . H33A H -0.0169 0.8854 0.5035 0.136 Uiso 1 1 d R . . C34 C 0.0225(2) 0.7995(4) 0.5115(4) 0.0802(18) Uani 1 1 d . . . H34A H 0.0426 0.7997 0.5589 0.096 Uiso 1 1 d R . . C35 C 0.02870(18) 0.7485(3) 0.4758(3) 0.0631(14) Uani 1 1 d . . . C36 C -0.00228(19) 0.7495(3) 0.4033(3) 0.0674(15) Uani 1 1 d . . . C51 C 0.0879(2) 0.5379(4) 0.3578(3) 0.0783(17) Uani 1 1 d DU . . C52A C 0.0785(9) 0.5109(19) 0.2919(8) 0.109(5) Uani 0.50(3) 1 d PDU C 1 H52A H 0.0841 0.5497 0.2703 0.163 Uiso 0.50(3) 1 calc PR C 1 H52B H 0.0465 0.4951 0.2624 0.163 Uiso 0.50(3) 1 calc PR C 1 H52C H 0.0991 0.4709 0.3007 0.163 Uiso 0.50(3) 1 calc PR C 1 C52B C 0.0688(9) 0.4811(14) 0.3019(11) 0.109(5) Uani 0.50(3) 1 d PDU C 2 H52D H 0.0620 0.4370 0.3162 0.163 Uiso 0.50(3) 1 calc PR C 2 H52E H 0.0918 0.4712 0.2927 0.163 Uiso 0.50(3) 1 calc PR C 2 H52F H 0.0407 0.4991 0.2613 0.163 Uiso 0.50(3) 1 calc PR C 2 C102 C 0.1542(2) 0.8652(4) 0.6066(4) 0.0823(18) Uani 1 1 d D A . C103 C 0.1909(2) 0.8680(4) 0.6735(4) 0.089(2) Uani 1 1 d . . . H10B H 0.1999 0.9129 0.6956 0.106 Uiso 1 1 d R A . C104 C 0.2155(2) 0.8059(4) 0.7089(3) 0.086(2) Uani 1 1 d D A . C107 C 0.1233(2) 0.7065(4) 0.7122(4) 0.0803(18) Uani 1 1 d D . . C108 C 0.1517(2) 0.6508(5) 0.7552(3) 0.087(2) Uani 1 1 d . B . H10C H 0.1587 0.6487 0.7989 0.104 Uiso 1 1 d R . . C109 C 0.1707(2) 0.5995(4) 0.7357(3) 0.0769(18) Uani 1 1 d D . . C1A C -0.0157(19) 0.0131(13) 0.365(2) 0.56(3) Uiso 0.50 1 d PD D 1 H1AA H 0.0040 0.0132 0.4143 0.835 Uiso 0.50 1 calc PR D 1 H1AB H -0.0352 -0.0296 0.3495 0.835 Uiso 0.50 1 calc PR D 1 H1AC H -0.0352 0.0559 0.3495 0.835 Uiso 0.50 1 calc PR D 1 C2A C 0.0141(12) 0.0131(13) 0.3389(10) 0.56(3) Uiso 0.50 1 d PD D 1 H2AA H 0.0341 0.0559 0.3556 0.668 Uiso 0.50 1 calc PR D 1 H2AB H 0.0341 -0.0296 0.3556 0.668 Uiso 0.50 1 calc PR D 1 C3A C -0.0153(6) 0.0131(13) 0.2628(9) 0.56(3) Uiso 0.50 1 d PD . 1 H3AA H -0.0353 0.0560 0.2459 0.668 Uiso 0.50 1 calc PR . 1 H3AB H -0.0353 -0.0297 0.2459 0.668 Uiso 0.50 1 calc PR . 1 C4A C 0.110(3) 0.176(4) 0.468(2) 0.81(2) Uiso 0.50 1 d PD E 1 H4AA H 0.1058 0.1784 0.5040 0.977 Uiso 0.50 1 calc PR E 1 H4AB H 0.1401 0.1513 0.4857 0.977 Uiso 0.50 1 calc PR E 1 Cl1 Cl 0.1135(14) 0.264(2) 0.4436(18) 0.81(2) Uiso 0.50 1 d PD E 1 Cl2 Cl 0.0650(16) 0.125(2) 0.400(2) 0.81(2) Uiso 0.50 1 d PD E 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.04203(16) 0.0673(2) 0.04662(17) 0.00006(12) 0.01917(13) -0.01028(11) Zn1 0.0517(3) 0.0671(4) 0.0615(4) 0.0062(3) 0.0297(3) -0.0016(3) Zn2 0.0493(3) 0.0642(4) 0.0471(3) 0.0041(3) 0.0219(3) -0.0014(3) N1 0.075(3) 0.074(3) 0.085(4) 0.012(3) 0.041(3) 0.007(3) N2 0.059(3) 0.075(3) 0.062(3) -0.004(2) 0.038(2) -0.011(2) N3 0.045(2) 0.069(3) 0.048(2) 0.005(2) 0.024(2) -0.002(2) N4 0.062(3) 0.080(3) 0.047(3) 0.011(2) 0.027(2) 0.010(2) O1 0.0407(18) 0.081(3) 0.056(2) 0.0097(19) 0.0201(17) -0.0044(17) O2 0.054(2) 0.067(2) 0.056(2) 0.0075(17) 0.0328(18) -0.0050(16) O3 0.0434(17) 0.059(2) 0.054(2) 0.0057(16) 0.0212(16) -0.0070(15) O4 0.0432(18) 0.064(2) 0.050(2) 0.0035(16) 0.0205(16) -0.0008(15) O5 0.069(2) 0.105(3) 0.052(2) 0.001(2) 0.033(2) 0.006(2) O6 0.069(3) 0.080(3) 0.078(3) -0.010(2) 0.038(2) -0.003(2) O7 0.087(3) 0.078(3) 0.063(3) -0.009(2) 0.037(2) -0.021(2) O8 0.050(2) 0.104(3) 0.065(3) -0.008(2) 0.016(2) -0.015(2) O9 0.069(2) 0.093(3) 0.060(3) -0.002(2) 0.033(2) -0.005(2) O10 0.067(2) 0.091(3) 0.067(3) 0.012(2) 0.038(2) -0.004(2) C101 0.163(9) 0.092(6) 0.139(9) 0.001(6) 0.099(8) -0.004(6) F1 0.184(6) 0.091(3) 0.132(4) -0.001(2) 0.069(4) 0.012(3) F2 0.184(6) 0.091(3) 0.132(4) -0.001(2) 0.069(4) 0.012(3) F3 0.184(6) 0.091(3) 0.132(4) -0.001(2) 0.069(4) 0.012(3) F1B 0.184(6) 0.091(3) 0.132(4) -0.001(2) 0.069(4) 0.012(3) F2B 0.184(6) 0.091(3) 0.132(4) -0.001(2) 0.069(4) 0.012(3) F3B 0.184(6) 0.091(3) 0.132(4) -0.001(2) 0.069(4) 0.012(3) C15A 0.089(6) 0.170(7) 0.122(8) -0.050(7) 0.029(6) -0.035(5) F4 0.104(3) 0.171(4) 0.084(4) -0.030(3) 0.010(3) -0.016(3) F5 0.104(3) 0.171(4) 0.084(4) -0.030(3) 0.010(3) -0.016(3) F6 0.104(3) 0.171(4) 0.084(4) -0.030(3) 0.010(3) -0.016(3) C15B 0.089(6) 0.170(7) 0.122(8) -0.050(7) 0.029(6) -0.035(5) F4B 0.104(3) 0.171(4) 0.084(4) -0.030(3) 0.010(3) -0.016(3) F5B 0.104(3) 0.171(4) 0.084(4) -0.030(3) 0.010(3) -0.016(3) F6B 0.104(3) 0.171(4) 0.084(4) -0.030(3) 0.010(3) -0.016(3) C16A 0.144(6) 0.202(7) 0.117(5) -0.020(6) 0.080(6) -0.028(6) F7 0.138(4) 0.188(4) 0.128(4) -0.035(4) 0.088(4) -0.003(4) F8 0.138(4) 0.188(4) 0.128(4) -0.035(4) 0.088(4) -0.003(4) F9 0.138(4) 0.188(4) 0.128(4) -0.035(4) 0.088(4) -0.003(4) C16B 0.144(6) 0.202(7) 0.117(5) -0.020(6) 0.080(6) -0.028(6) F7B 0.138(4) 0.188(4) 0.128(4) -0.035(4) 0.088(4) -0.003(4) F8B 0.138(4) 0.188(4) 0.128(4) -0.035(4) 0.088(4) -0.003(4) F9B 0.138(4) 0.188(4) 0.128(4) -0.035(4) 0.088(4) -0.003(4) C11A 0.125(8) 0.238(12) 0.112(6) 0.065(7) 0.059(7) -0.008(7) F10 0.161(5) 0.165(6) 0.129(4) 0.065(4) 0.076(4) 0.031(4) F11 0.161(5) 0.165(6) 0.129(4) 0.065(4) 0.076(4) 0.031(4) F12 0.161(5) 0.165(6) 0.129(4) 0.065(4) 0.076(4) 0.031(4) C11B 0.125(8) 0.238(12) 0.112(6) 0.065(7) 0.059(7) -0.008(7) F10B 0.161(5) 0.165(6) 0.129(4) 0.065(4) 0.076(4) 0.031(4) F11B 0.161(5) 0.165(6) 0.129(4) 0.065(4) 0.076(4) 0.031(4) F12B 0.161(5) 0.165(6) 0.129(4) 0.065(4) 0.076(4) 0.031(4) C1 0.121(7) 0.095(6) 0.114(7) 0.013(5) 0.049(6) 0.027(5) C2 0.147(9) 0.123(8) 0.161(11) 0.016(8) 0.056(9) 0.064(7) C3 0.112(7) 0.147(9) 0.144(10) 0.047(8) 0.058(7) 0.057(7) C4 0.076(4) 0.094(5) 0.107(6) 0.040(5) 0.043(5) 0.031(4) C5 0.078(5) 0.136(8) 0.110(7) 0.055(6) 0.038(5) 0.031(5) C6 0.057(4) 0.130(7) 0.075(5) 0.035(5) 0.020(4) -0.009(4) C7 0.051(3) 0.110(5) 0.061(4) 0.022(3) 0.020(3) -0.009(3) C8 0.046(3) 0.080(4) 0.070(4) 0.021(3) 0.031(3) -0.005(3) C9 0.066(4) 0.082(4) 0.088(5) 0.033(4) 0.040(4) 0.005(3) C10 0.069(4) 0.092(5) 0.078(4) 0.000(3) 0.046(4) 0.000(3) C11 0.076(4) 0.121(6) 0.099(6) -0.002(5) 0.061(4) -0.013(4) C12 0.076(4) 0.116(6) 0.082(5) -0.001(4) 0.052(4) -0.032(4) C13 0.061(3) 0.085(4) 0.056(3) 0.000(3) 0.033(3) -0.019(3) C14 0.084(4) 0.086(5) 0.065(4) 0.006(3) 0.039(4) -0.025(4) C15 0.084(4) 0.069(4) 0.063(4) 0.008(3) 0.033(3) -0.013(3) C16 0.066(3) 0.072(4) 0.061(4) 0.006(3) 0.033(3) 0.000(3) C17 0.055(3) 0.068(3) 0.041(3) 0.006(2) 0.023(2) -0.010(3) C18 0.052(3) 0.065(3) 0.051(3) -0.002(2) 0.026(2) -0.010(3) C19 0.053(3) 0.092(4) 0.045(3) 0.002(3) 0.020(3) -0.008(3) C20 0.053(3) 0.108(5) 0.059(4) -0.015(4) 0.025(3) -0.030(3) C21 0.058(3) 0.090(4) 0.060(4) -0.006(3) 0.028(3) -0.024(3) C22 0.058(3) 0.070(4) 0.068(4) 0.003(3) 0.036(3) -0.013(3) C23 0.070(4) 0.067(4) 0.088(5) 0.012(3) 0.040(4) -0.016(3) C24 0.071(4) 0.073(4) 0.087(5) 0.029(3) 0.031(4) 0.004(3) C25 0.048(3) 0.082(4) 0.068(4) 0.016(3) 0.020(3) 0.001(3) C26 0.045(3) 0.061(3) 0.053(3) 0.002(2) 0.026(2) -0.006(2) C27 0.045(2) 0.064(3) 0.052(3) 0.000(2) 0.029(2) -0.004(2) C28 0.090(5) 0.112(5) 0.058(4) 0.011(4) 0.031(4) 0.026(4) C29 0.108(6) 0.158(8) 0.059(4) 0.033(5) 0.022(4) 0.054(6) C30 0.117(7) 0.146(8) 0.081(6) 0.026(5) 0.028(5) 0.071(6) C31 0.091(5) 0.110(6) 0.086(5) 0.017(4) 0.039(5) 0.043(4) C32 0.108(6) 0.134(7) 0.100(6) 0.001(6) 0.035(5) 0.055(6) C33 0.112(6) 0.126(6) 0.083(5) -0.007(5) 0.044(5) 0.048(5) C34 0.066(4) 0.087(4) 0.071(4) -0.007(3) 0.029(3) 0.008(3) C35 0.051(3) 0.069(4) 0.066(4) 0.004(3) 0.031(3) -0.002(3) C36 0.057(3) 0.076(4) 0.055(3) 0.014(3) 0.024(3) 0.013(3) C51 0.064(4) 0.100(5) 0.071(4) -0.010(3) 0.038(3) -0.009(3) C52A 0.111(8) 0.140(10) 0.085(6) -0.012(7) 0.062(5) 0.007(8) C52B 0.111(8) 0.140(10) 0.085(6) -0.012(7) 0.062(5) 0.007(8) C102 0.086(4) 0.074(4) 0.088(5) -0.009(4) 0.051(4) -0.014(4) C103 0.073(4) 0.093(5) 0.080(5) -0.031(4) 0.033(4) -0.019(4) C104 0.063(4) 0.100(5) 0.080(5) -0.033(4) 0.032(4) -0.029(4) C107 0.074(4) 0.111(5) 0.065(4) -0.023(4) 0.045(4) -0.024(4) C108 0.074(4) 0.127(6) 0.052(4) 0.006(4) 0.032(3) -0.013(4) C109 0.059(3) 0.109(5) 0.051(3) 0.014(3) 0.025(3) -0.011(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 Eu1 O1 2.330(4) . ? Eu1 O4 2.344(3) . ? Eu1 O7 2.392(4) . ? Eu1 O8 2.402(4) . ? Eu1 O9 2.407(5) . ? Eu1 O10 2.421(4) . ? Eu1 O3 2.433(3) . ? Eu1 O2 2.460(4) . ? Eu1 Zn1 3.3238(8) . ? Eu1 Zn2 3.3379(6) . ? Zn1 O6 2.025(4) . ? Zn1 N1 2.063(5) . ? Zn1 N2 2.107(5) . ? Zn1 O2 2.140(4) . ? Zn1 O1 2.144(4) . ? Zn1 O3 2.263(4) . ? Zn2 O5 2.044(4) . ? Zn2 N4 2.067(4) . ? Zn2 N3 2.099(4) . ? Zn2 O4 2.121(4) . ? Zn2 O3 2.152(3) . ? Zn2 O2 2.308(3) . ? N1 C1 1.311(10) . ? N1 C9 1.350(8) . ? N2 C10 1.322(7) . ? N2 C18 1.370(7) . ? N3 C19 1.316(6) . ? N3 C27 1.355(6) . ? N4 C28 1.309(8) . ? N4 C36 1.358(8) . ? O1 C8 1.324(6) . ? O2 C17 1.339(6) . ? O3 C26 1.356(6) . ? O4 C35 1.334(6) . ? O5 C51 1.254(7) . ? O6 C51 1.270(7) . ? O7 C102 1.251(8) . ? O8 C104 1.252(8) . ? O9 C107 1.252(8) . ? O10 C109 1.247(7) . ? C101 F1B 1.301(9) . ? C101 F1 1.303(8) . ? C101 F2 1.327(8) . ? C101 F3B 1.344(9) . ? C101 F3 1.385(8) . ? C101 F2B 1.400(9) . ? C101 C102 1.493(7) . ? C15A F4 1.334(9) . ? C15A F5 1.336(9) . ? C15A F6 1.343(9) . ? C15A C104 1.500(9) . ? C15B F4B 1.337(9) . ? C15B F5B 1.340(9) . ? C15B F6B 1.343(9) . ? C15B C104 1.502(9) . ? C16A F8 1.330(9) . ? C16A F9 1.332(9) . ? C16A F7 1.342(9) . ? C16A C107 1.494(9) . ? C16B F9B 1.327(9) . ? C16B F8B 1.338(9) . ? C16B F7B 1.344(9) . ? C16B C107 1.497(9) . ? C11A F12 1.336(10) . ? C11A F10 1.346(10) . ? C11A F11 1.346(10) . ? C11A C109 1.502(9) . ? C11B F10B 1.326(9) . ? C11B F12B 1.330(9) . ? C11B F11B 1.346(9) . ? C11B C109 1.493(9) . ? C1 C2 1.439(12) . ? C1 H1A 0.9298 . ? C2 C3 1.338(14) . ? C2 H2A 0.9302 . ? C3 C4 1.401(13) . ? C3 H3A 0.9302 . ? C4 C5 1.418(12) . ? C4 C9 1.423(9) . ? C5 C6 1.324(12) . ? C5 H5A 0.9302 . ? C6 C7 1.399(9) . ? C6 H6A 0.9298 . ? C7 C8 1.380(8) . ? C7 H7A 0.9297 . ? C8 C9 1.430(9) . ? C10 C11 1.391(9) . ? C10 H10A 0.9296 . ? C11 C12 1.350(10) . ? C11 H11A 0.9302 . ? C12 C13 1.403(10) . ? C12 H12A 0.9306 . ? C13 C14 1.403(9) . ? C13 C18 1.418(8) . ? C14 C15 1.360(10) . ? C14 H14A 0.9296 . ? C15 C16 1.443(9) . ? C15 H15A 0.9299 . ? C16 C17 1.364(8) . ? C16 H16A 0.9295 . ? C17 C18 1.428(8) . ? C19 C20 1.411(8) . ? C19 H19A 0.9298 . ? C20 C21 1.323(9) . ? C20 H20A 0.9298 . ? C21 C22 1.412(8) . ? C21 H21A 0.9299 . ? C22 C23 1.393(8) . ? C22 C27 1.419(7) . ? C23 C24 1.344(8) . ? C23 H23A 0.9303 . ? C24 C25 1.402(8) . ? C24 H24A 0.9300 . ? C25 C26 1.355(7) . ? C25 H25A 0.9300 . ? C26 C27 1.422(6) . ? C28 C29 1.426(10) . ? C28 H28A 0.9302 . ? C29 C30 1.328(12) . ? C29 H29A 0.9298 . ? C30 C31 1.413(11) . ? C30 H30A 0.9297 . ? C31 C32 1.395(12) . ? C31 C36 1.427(8) . ? C32 C33 1.357(11) . ? C32 H32A 0.9301 . ? C33 C34 1.398(9) . ? C33 H33A 0.9300 . ? C34 C35 1.366(9) . ? C34 H34A 0.9302 . ? C35 C36 1.425(8) . ? C51 C52A 1.502(9) . ? C51 C52B 1.517(9) . ? C52A H52A 0.9600 . ? C52A H52B 0.9600 . ? C52A H52C 0.9600 . ? C52B H52D 0.9600 . ? C52B H52E 0.9600 . ? C52B H52F 0.9600 . ? C102 C103 1.362(9) . ? C103 C104 1.384(10) . ? C103 H10B 0.9299 . ? C107 C108 1.383(10) . ? C108 C109 1.376(10) . ? C108 H10C 0.9293 . ? C1A C2A 1.495(10) . ? C1A H1AA 0.9600 . ? C1A H1AB 0.9600 . ? C1A H1AC 0.9600 . ? C2A C3A 1.494(10) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A C3A 1.497(10) 2 ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C4A Cl1 1.738(10) . ? C4A Cl2 1.746(10) . ? C4A H4AA 0.9700 . ? C4A H4AB 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Eu1 O4 137.00(13) . . ? O1 Eu1 O7 114.94(15) . . ? O4 Eu1 O7 78.11(14) . . ? O1 Eu1 O8 78.68(15) . . ? O4 Eu1 O8 140.96(14) . . ? O7 Eu1 O8 70.20(15) . . ? O1 Eu1 O9 142.85(13) . . ? O4 Eu1 O9 77.59(13) . . ? O7 Eu1 O9 79.96(16) . . ? O8 Eu1 O9 75.00(15) . . ? O1 Eu1 O10 78.68(13) . . ? O4 Eu1 O10 118.71(13) . . ? O7 Eu1 O10 140.02(15) . . ? O8 Eu1 O10 76.73(15) . . ? O9 Eu1 O10 70.13(15) . . ? O1 Eu1 O3 72.69(12) . . ? O4 Eu1 O3 71.80(12) . . ? O7 Eu1 O3 137.55(13) . . ? O8 Eu1 O3 146.94(13) . . ? O9 Eu1 O3 120.40(13) . . ? O10 Eu1 O3 81.70(13) . . ? O1 Eu1 O2 71.03(12) . . ? O4 Eu1 O2 71.56(12) . . ? O7 Eu1 O2 79.95(14) . . ? O8 Eu1 O2 122.50(14) . . ? O9 Eu1 O2 145.96(13) . . ? O10 Eu1 O2 138.40(14) . . ? O3 Eu1 O2 62.67(11) . . ? O1 Eu1 Zn1 39.92(9) . . ? O4 Eu1 Zn1 97.08(9) . . ? O7 Eu1 Zn1 115.38(12) . . ? O8 Eu1 Zn1 116.64(11) . . ? O9 Eu1 Zn1 162.70(11) . . ? O10 Eu1 Zn1 99.08(11) . . ? O3 Eu1 Zn1 42.90(8) . . ? O2 Eu1 Zn1 40.05(8) . . ? O1 Eu1 Zn2 98.02(9) . . ? O4 Eu1 Zn2 39.13(9) . . ? O7 Eu1 Zn2 98.77(10) . . ? O8 Eu1 Zn2 165.15(11) . . ? O9 Eu1 Zn2 113.74(10) . . ? O10 Eu1 Zn2 117.09(10) . . ? O3 Eu1 Zn2 40.07(8) . . ? O2 Eu1 Zn2 43.73(8) . . ? Zn1 Eu1 Zn2 58.163(16) . . ? O6 Zn1 N1 94.0(2) . . ? O6 Zn1 N2 94.94(18) . . ? N1 Zn1 N2 99.7(2) . . ? O6 Zn1 O2 106.85(16) . . ? N1 Zn1 O2 159.2(2) . . ? N2 Zn1 O2 78.58(17) . . ? O6 Zn1 O1 164.40(16) . . ? N1 Zn1 O1 78.8(2) . . ? N2 Zn1 O1 99.86(15) . . ? O2 Zn1 O1 81.07(14) . . ? O6 Zn1 O3 90.23(15) . . ? N1 Zn1 O3 110.58(18) . . ? N2 Zn1 O3 148.86(16) . . ? O2 Zn1 O3 70.54(12) . . ? O1 Zn1 O3 79.64(13) . . ? O6 Zn1 Eu1 132.78(12) . . ? N1 Zn1 Eu1 116.91(18) . . ? N2 Zn1 Eu1 112.35(13) . . ? O2 Zn1 Eu1 47.70(10) . . ? O1 Zn1 Eu1 44.20(10) . . ? O3 Zn1 Eu1 47.05(9) . . ? O5 Zn2 N4 93.94(18) . . ? O5 Zn2 N3 93.95(17) . . ? N4 Zn2 N3 101.86(18) . . ? O5 Zn2 O4 162.81(16) . . ? N4 Zn2 O4 79.33(17) . . ? N3 Zn2 O4 102.89(15) . . ? O5 Zn2 O3 105.24(16) . . ? N4 Zn2 O3 160.79(18) . . ? N3 Zn2 O3 78.17(14) . . ? O4 Zn2 O3 81.94(13) . . ? O5 Zn2 O2 89.13(15) . . ? N4 Zn2 O2 110.58(16) . . ? N3 Zn2 O2 147.12(14) . . ? O4 Zn2 O2 78.67(13) . . ? O3 Zn2 O2 69.47(12) . . ? O5 Zn2 Eu1 131.55(12) . . ? N4 Zn2 Eu1 118.30(14) . . ? N3 Zn2 Eu1 111.62(11) . . ? O4 Zn2 Eu1 44.23(9) . . ? O3 Zn2 Eu1 46.69(9) . . ? O2 Zn2 Eu1 47.47(9) . . ? C1 N1 C9 120.2(6) . . ? C1 N1 Zn1 125.8(5) . . ? C9 N1 Zn1 113.3(5) . . ? C10 N2 C18 118.9(5) . . ? C10 N2 Zn1 128.2(4) . . ? C18 N2 Zn1 112.9(3) . . ? C19 N3 C27 119.0(5) . . ? C19 N3 Zn2 126.9(4) . . ? C27 N3 Zn2 113.7(3) . . ? C28 N4 C36 119.9(5) . . ? C28 N4 Zn2 127.1(5) . . ? C36 N4 Zn2 112.9(3) . . ? C8 O1 Zn1 112.0(4) . . ? C8 O1 Eu1 142.8(4) . . ? Zn1 O1 Eu1 95.88(12) . . ? C17 O2 Zn1 112.8(3) . . ? C17 O2 Zn2 126.6(3) . . ? Zn1 O2 Zn2 93.35(12) . . ? C17 O2 Eu1 132.7(3) . . ? Zn1 O2 Eu1 92.25(12) . . ? Zn2 O2 Eu1 88.80(12) . . ? C26 O3 Zn2 112.0(3) . . ? C26 O3 Zn1 121.6(3) . . ? Zn2 O3 Zn1 94.31(13) . . ? C26 O3 Eu1 135.9(3) . . ? Zn2 O3 Eu1 93.24(12) . . ? Zn1 O3 Eu1 90.05(11) . . ? C35 O4 Zn2 112.5(3) . . ? C35 O4 Eu1 140.8(3) . . ? Zn2 O4 Eu1 96.63(14) . . ? C51 O5 Zn2 127.0(4) . . ? C51 O6 Zn1 126.6(4) . . ? C102 O7 Eu1 134.7(4) . . ? C104 O8 Eu1 135.0(4) . . ? C107 O9 Eu1 134.3(4) . . ? C109 O10 Eu1 134.1(4) . . ? F1B C101 F1 43.4(8) . . ? F1B C101 F2 123.0(10) . . ? F1 C101 F2 112.9(9) . . ? F1B C101 F3B 109.1(10) . . ? F1 C101 F3B 127.6(10) . . ? F2 C101 F3B 34.7(8) . . ? F1B C101 F3 56.9(8) . . ? F1 C101 F3 100.1(8) . . ? F2 C101 F3 103.7(9) . . ? F3B C101 F3 70.3(8) . . ? F1B C101 F2B 100.1(10) . . ? F1 C101 F2B 59.2(7) . . ? F2 C101 F2B 68.1(8) . . ? F3B C101 F2B 101.5(10) . . ? F3 C101 F2B 147.7(8) . . ? F1B C101 C102 120.5(9) . . ? F1 C101 C102 114.8(8) . . ? F2 C101 C102 116.3(8) . . ? F3B C101 C102 117.3(9) . . ? F3 C101 C102 106.7(7) . . ? F2B C101 C102 104.7(8) . . ? F4 C15A F5 108.7(11) . . ? F4 C15A F6 106.8(11) . . ? F5 C15A F6 104.6(10) . . ? F4 C15A C104 109.7(11) . . ? F5 C15A C104 115.3(10) . . ? F6 C15A C104 111.3(10) . . ? F4B C15B F5B 107.0(12) . . ? F4B C15B F6B 103.4(11) . . ? F5B C15B F6B 105.2(12) . . ? F4B C15B C104 118.2(13) . . ? F5B C15B C104 107.4(11) . . ? F6B C15B C104 114.7(11) . . ? F8 C16A F9 105.8(10) . . ? F8 C16A F7 106.1(11) . . ? F9 C16A F7 105.2(11) . . ? F8 C16A C107 112.1(10) . . ? F9 C16A C107 113.4(11) . . ? F7 C16A C107 113.6(12) . . ? F9B C16B F8B 104.0(10) . . ? F9B C16B F7B 107.3(11) . . ? F8B C16B F7B 105.3(11) . . ? F9B C16B C107 116.7(11) . . ? F8B C16B C107 113.3(11) . . ? F7B C16B C107 109.4(11) . . ? F12 C11A F10 104.5(12) . . ? F12 C11A F11 106.6(13) . . ? F10 C11A F11 105.3(12) . . ? F12 C11A C109 116.3(14) . . ? F10 C11A C109 118.4(14) . . ? F11 C11A C109 104.6(12) . . ? F10B C11B F12B 105.7(9) . . ? F10B C11B F11B 106.1(10) . . ? F12B C11B F11B 107.6(10) . . ? F10B C11B C109 110.6(9) . . ? F12B C11B C109 114.5(9) . . ? F11B C11B C109 111.8(9) . . ? N1 C1 C2 121.9(9) . . ? N1 C1 H1A 119.8 . . ? C2 C1 H1A 118.2 . . ? C3 C2 C1 116.7(10) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 122.6 . . ? C2 C3 C4 124.0(9) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 117.0 . . ? C3 C4 C5 126.3(8) . . ? C3 C4 C9 114.7(8) . . ? C5 C4 C9 118.9(8) . . ? C6 C5 C4 119.4(7) . . ? C6 C5 H5A 121.5 . . ? C4 C5 H5A 119.0 . . ? C5 C6 C7 123.4(8) . . ? C5 C6 H6A 117.4 . . ? C7 C6 H6A 119.2 . . ? C8 C7 C6 120.1(8) . . ? C8 C7 H7A 120.5 . . ? C6 C7 H7A 119.4 . . ? O1 C8 C7 124.2(6) . . ? O1 C8 C9 117.5(6) . . ? C7 C8 C9 118.2(6) . . ? N1 C9 C4 122.4(8) . . ? N1 C9 C8 117.7(6) . . ? C4 C9 C8 119.9(7) . . ? N2 C10 C11 123.0(7) . . ? N2 C10 H10A 118.6 . . ? C11 C10 H10A 118.4 . . ? C12 C11 C10 118.4(7) . . ? C12 C11 H11A 120.9 . . ? C10 C11 H11A 120.6 . . ? C11 C12 C13 121.9(6) . . ? C11 C12 H12A 118.8 . . ? C13 C12 H12A 119.3 . . ? C14 C13 C12 124.7(6) . . ? C14 C13 C18 119.2(6) . . ? C12 C13 C18 116.1(6) . . ? C15 C14 C13 120.0(6) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 121.3(6) . . ? C14 C15 H15A 119.3 . . ? C16 C15 H15A 119.5 . . ? C17 C16 C15 120.0(6) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? O2 C17 C16 123.3(5) . . ? O2 C17 C18 117.9(5) . . ? C16 C17 C18 118.8(5) . . ? N2 C18 C13 121.7(5) . . ? N2 C18 C17 117.6(5) . . ? C13 C18 C17 120.7(5) . . ? N3 C19 C20 121.5(5) . . ? N3 C19 H19A 119.2 . . ? C20 C19 H19A 119.3 . . ? C21 C20 C19 120.7(5) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.5 . . ? C20 C21 C22 120.0(6) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 124.6(5) . . ? C23 C22 C27 118.8(5) . . ? C21 C22 C27 116.6(5) . . ? C24 C23 C22 120.2(5) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 121.3(6) . . ? C23 C24 H24A 119.4 . . ? C25 C24 H24A 119.4 . . ? C26 C25 C24 121.4(5) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.1 . . ? C25 C26 O3 124.3(5) . . ? C25 C26 C27 118.1(5) . . ? O3 C26 C27 117.7(4) . . ? N3 C27 C22 122.1(4) . . ? N3 C27 C26 117.7(4) . . ? C22 C27 C26 120.2(5) . . ? N4 C28 C29 121.4(7) . . ? N4 C28 H28A 119.2 . . ? C29 C28 H28A 119.4 . . ? C30 C29 C28 119.7(7) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 121.0(7) . . ? C29 C30 H30A 119.5 . . ? C31 C30 H30A 119.4 . . ? C32 C31 C30 125.2(7) . . ? C32 C31 C36 118.6(7) . . ? C30 C31 C36 116.2(7) . . ? C33 C32 C31 120.2(7) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C34 121.7(7) . . ? C32 C33 H33A 119.2 . . ? C34 C33 H33A 119.2 . . ? C35 C34 C33 120.9(7) . . ? C35 C34 H34A 119.3 . . ? C33 C34 H34A 119.8 . . ? O4 C35 C34 124.3(6) . . ? O4 C35 C36 117.3(5) . . ? C34 C35 C36 118.4(5) . . ? N4 C36 C35 118.0(5) . . ? N4 C36 C31 121.8(6) . . ? C35 C36 C31 120.2(6) . . ? O5 C51 O6 123.9(6) . . ? O5 C51 C52A 116.7(11) . . ? O6 C51 C52A 117.6(11) . . ? O5 C51 C52B 120.5(11) . . ? O6 C51 C52B 113.6(11) . . ? C52A C51 C52B 28.8(11) . . ? C51 C52A H52A 109.5 . . ? C51 C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C51 C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C51 C52B H52D 109.5 . . ? C51 C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C51 C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? O7 C102 C103 128.0(7) . . ? O7 C102 C101 114.2(6) . . ? C103 C102 C101 117.8(7) . . ? C102 C103 C104 121.5(6) . . ? C102 C103 H10B 119.0 . . ? C104 C103 H10B 119.4 . . ? O8 C104 C103 127.0(6) . . ? O8 C104 C15A 113.4(8) . . ? C103 C104 C15A 119.4(8) . . ? O8 C104 C15B 111.8(9) . . ? C103 C104 C15B 121.0(9) . . ? C15A C104 C15B 9.2(9) . . ? O9 C107 C108 127.6(7) . . ? O9 C107 C16A 114.9(8) . . ? C108 C107 C16A 117.5(8) . . ? O9 C107 C16B 111.6(8) . . ? C108 C107 C16B 120.8(8) . . ? C16A C107 C16B 3.6(9) . . ? C109 C108 C107 121.9(6) . . ? C109 C108 H10C 119.1 . . ? C107 C108 H10C 119.0 . . ? O10 C109 C108 127.2(6) . . ? O10 C109 C11B 114.7(8) . . ? C108 C109 C11B 117.8(7) . . ? O10 C109 C11A 113.7(10) . . ? C108 C109 C11A 119.2(10) . . ? C11B C109 C11A 5.3(9) . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C3A C2A C1A 111.3(16) . . ? C3A C2A H2AA 109.4 . . ? C1A C2A H2AA 109.4 . . ? C3A C2A H2AB 109.4 . . ? C1A C2A H2AB 109.4 . . ? H2AA C2A H2AB 108.0 . . ? C2A C3A C3A 110.5(16) . 2 ? C2A C3A H3AA 109.6 . . ? C3A C3A H3AA 109.6 2 . ? C2A C3A H3AB 109.6 . . ? C3A C3A H3AB 109.6 2 . ? H3AA C3A H3AB 108.1 . . ? Cl1 C4A Cl2 112.4(14) . . ? Cl1 C4A H4AA 109.1 . . ? Cl2 C4A H4AA 109.1 . . ? Cl1 C4A H4AB 109.1 . . ? Cl2 C4A H4AB 109.1 . . ? H4AA C4A H4AB 107.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.602 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.210 # Attachment 'Zn2Tb-752293.cif' data_tb _database_code_depnum_ccdc_archive 'CCDC 752293' #TrackingRef 'Zn2Tb-752293.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H33.50 Cl F12 N4 O10 Tb Zn2' _chemical_formula_weight 1403.42 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' 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' F F 0.0171 0.0103 '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' Zn Zn 0.2839 1.4301 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.716(10) _cell_length_b 18.480(4) _cell_length_c 24.147(13) _cell_angle_alpha 90.00 _cell_angle_beta 125.291(2) _cell_angle_gamma 90.00 _cell_volume 12645(8) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 14073 _cell_measurement_theta_min 3.0219 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5532 _exptl_absorpt_coefficient_mu 1.988 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.7548 _exptl_absorpt_correction_T_max 0.8414 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'RIGAKU MERCURY CCD/AFC' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43449 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12353 _reflns_number_gt 10138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the weak interaction between the solvent molecules and the clusters, the solvent molecules are in severe disordered and with large Uiso values. Therefore, the non-H atoms of solvent molecules were refined in isotropic model with restrained thermal factors, and their occupancies are fixed to 0.5 according to the element analysis results. The total solvent accessible voids is 48 A**3 per independent in this structure, It is not very large, and no significant residual electron peaks was found in these sites. Therefore, no new solvent molecules were identified to further reduce the solvent accessible voids. the following restrains is used in the refinement 1) The CF3 groups are in disorder. Therefore, the ADPs of the related non-H atoms are restrained by using EADP and DELU commands, and their occupancies are refined by PART instructions. The related C-C, C-F bonds and the F...F distances are restrained to 1.49(1), 1.33(1) and 2.15(2) A respectively by DFIX command. 2) The solvent molecules are in severe disordered, so their non-H atoms ADPs are refined in isotropic model and restrained by EADP commands. The related C-C, C-Cl bonds and the C...C and Cl...Cl distances are fixed to 1.50(1), 1.74(1), 2.50(2) and 2.90(2) A respectively by DFIX command. 3) A disordered methyl group is refined in two parts with equal ADPs by PART instruction and EADP command. The related C-C bond is fixed to 1.49(1) A by DFIX command. After checking cif, some alert level_B were found: PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C107 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C109 Answer: These atoms are bonding with the C atoms of disorderd methyl groups, which have larger Ueq value. The highest residual electron densities are located in the position very close to the lanthanide atoms. This phenomenon is usually found in the lanthanide compounds caused by the series termination errors of heavy atoms. ; _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^)+(0.1061P)^2^+20.8094P] 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 12353 _refine_ls_number_parameters 719 _refine_ls_number_restraints 135 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1500 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.151 _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 Tb1 Tb 0.142121(5) 0.681712(9) 0.587269(7) 0.05337(5) Uani 1 1 d . . . Zn1 Zn 0.167369(13) 0.58330(2) 0.49762(2) 0.06071(11) Uani 1 1 d . . . Zn2 Zn 0.058899(12) 0.62718(2) 0.430668(18) 0.05392(10) Uani 1 1 d . . . N1 N 0.21930(12) 0.5057(2) 0.5505(2) 0.0841(12) Uani 1 1 d . . . N2 N 0.19619(9) 0.64593(19) 0.45659(15) 0.0645(8) Uani 1 1 d . . . N3 N 0.02243(8) 0.53696(16) 0.43091(13) 0.0529(7) Uani 1 1 d . . . N4 N 0.00400(11) 0.69751(19) 0.36811(15) 0.0647(9) Uani 1 1 d . . . O1 O 0.20617(7) 0.62655(15) 0.59866(12) 0.0645(7) Uani 1 1 d . . . O2 O 0.13041(8) 0.68338(12) 0.47734(12) 0.0564(6) Uani 1 1 d . . . O3 O 0.11352(7) 0.57169(12) 0.52137(11) 0.0547(6) Uani 1 1 d . . . O4 O 0.06222(7) 0.69582(13) 0.50399(12) 0.0555(6) Uani 1 1 d . . . O5 O 0.06268(9) 0.58893(18) 0.35421(12) 0.0744(8) Uani 1 1 d . C . O6 O 0.12731(10) 0.52111(17) 0.41370(15) 0.0788(9) Uani 1 1 d . C . O7 O 0.13630(10) 0.80815(15) 0.56756(14) 0.0726(8) Uani 1 1 d . . . O8 O 0.20661(9) 0.74074(17) 0.68433(15) 0.0817(10) Uani 1 1 d . . . O9 O 0.11252(9) 0.72027(17) 0.65031(13) 0.0738(8) Uani 1 1 d . B . O10 O 0.16594(9) 0.59744(16) 0.67616(13) 0.0706(8) Uani 1 1 d . B . C101 C 0.13056(14) 0.9330(2) 0.5697(2) 0.1355(16) Uani 1 1 d DU . . F1 F 0.1582(2) 0.9897(3) 0.5933(3) 0.1429(14) Uani 0.548(4) 1 d PDU A 1 F2 F 0.1025(3) 0.9307(4) 0.5028(3) 0.1429(14) Uani 0.548(4) 1 d PDU A 1 F3 F 0.10048(19) 0.9514(4) 0.5874(3) 0.1429(14) Uani 0.548(4) 1 d PDU A 1 F1B F 0.1343(3) 0.9893(4) 0.6048(4) 0.1429(14) Uani 0.452(4) 1 d PDU A 2 F2B F 0.1546(2) 0.9543(4) 0.5424(4) 0.1429(14) Uani 0.452(4) 1 d PDU A 2 F3B F 0.0864(2) 0.9285(5) 0.5138(4) 0.1429(14) Uani 0.452(4) 1 d PDU A 2 C15A C 0.25482(19) 0.8118(3) 0.7800(3) 0.1484(7) Uani 0.548(5) 1 d PDU A 1 F4 F 0.2669(3) 0.8810(3) 0.7979(3) 0.1473(8) Uani 0.548(5) 1 d PDU A 1 F5 F 0.29348(19) 0.7746(4) 0.7985(3) 0.1473(8) Uani 0.548(5) 1 d PDU A 1 F6 F 0.2421(2) 0.7872(4) 0.8196(3) 0.1473(8) Uani 0.548(5) 1 d PDU A 1 C15B C 0.2602(2) 0.8106(4) 0.7758(3) 0.1484(7) Uani 0.452(5) 1 d PDU A 2 F4B F 0.2676(3) 0.8707(4) 0.8118(4) 0.1473(8) Uani 0.452(5) 1 d PDU A 2 F5B F 0.2963(2) 0.8058(5) 0.7702(4) 0.1473(8) Uani 0.452(5) 1 d PDU A 2 F6B F 0.2684(3) 0.7560(4) 0.8179(3) 0.1473(8) Uani 0.452(5) 1 d PDU A 2 C16A C 0.1032(2) 0.7552(4) 0.7359(3) 0.1495(16) Uani 0.389(4) 1 d PDU B 1 F7 F 0.0853(3) 0.8175(4) 0.7018(4) 0.1497(11) Uani 0.389(4) 1 d PDU B 1 F8 F 0.0684(2) 0.7237(5) 0.7353(4) 0.1497(11) Uani 0.389(4) 1 d PDU B 1 F9 F 0.1356(3) 0.7732(6) 0.8008(3) 0.1497(11) Uani 0.389(4) 1 d PDU B 1 C16B C 0.10057(18) 0.7591(3) 0.7291(3) 0.1495(16) Uani 0.611(4) 1 d PDU B 2 F7B F 0.1112(2) 0.8279(3) 0.7242(3) 0.1497(11) Uani 0.611(4) 1 d PDU B 2 F8B F 0.05358(16) 0.7543(4) 0.6885(3) 0.1497(11) Uani 0.611(4) 1 d PDU B 2 F9B F 0.1133(2) 0.7541(4) 0.7924(2) 0.1497(11) Uani 0.611(4) 1 d PDU B 2 C11A C 0.19767(19) 0.5388(3) 0.7796(3) 0.1523(15) Uani 0.526(4) 1 d PDU B 1 F10 F 0.1821(3) 0.4734(4) 0.7507(3) 0.1568(12) Uani 0.474(4) 1 d PDU B 1 F11 F 0.24239(18) 0.5431(5) 0.8017(3) 0.1568(12) Uani 0.526(4) 1 d PDU B 1 F12 F 0.1957(2) 0.5329(5) 0.8333(3) 0.1568(12) Uani 0.526(4) 1 d PDU B 1 C11B C 0.1965(2) 0.5362(3) 0.7771(3) 0.1523(15) Uani 0.474(4) 1 d PDU B 2 F10B F 0.1648(2) 0.4838(4) 0.7631(4) 0.1568(12) Uani 0.526(4) 1 d PDU B 2 F11B F 0.2261(2) 0.5011(5) 0.7683(3) 0.1568(12) Uani 0.474(4) 1 d PDU B 2 F12B F 0.2162(3) 0.5495(5) 0.8427(3) 0.1568(12) Uani 0.474(4) 1 d PDU B 2 C1 C 0.2247(2) 0.4478(3) 0.5234(4) 0.135(3) Uani 1 1 d . . . H1A H 0.2018 0.4362 0.4782 0.162 Uiso 1 1 calc R . . C2 C 0.2657(3) 0.4026(4) 0.5630(5) 0.174(4) Uani 1 1 d . . . H2A H 0.2697 0.3616 0.5446 0.209 Uiso 1 1 calc R . . C3 C 0.2990(3) 0.4225(4) 0.6299(4) 0.159(4) Uani 1 1 d . . . H3A H 0.3255 0.3936 0.6565 0.191 Uiso 1 1 calc R . . C4 C 0.29434(18) 0.4836(3) 0.6585(3) 0.105(2) Uani 1 1 d . . . C5 C 0.32640(19) 0.5050(4) 0.7264(3) 0.119(2) Uani 1 1 d . . . H5A H 0.3538 0.4783 0.7551 0.143 Uiso 1 1 calc R . . C6 C 0.31773(16) 0.5627(3) 0.7492(3) 0.1008(19) Uani 1 1 d . . . H6A H 0.3393 0.5760 0.7943 0.121 Uiso 1 1 calc R . . C7 C 0.27728(13) 0.6049(3) 0.7083(2) 0.0809(14) Uani 1 1 d . . . H7A H 0.2728 0.6455 0.7267 0.097 Uiso 1 1 calc R . . C8 C 0.24414(11) 0.5880(2) 0.64160(19) 0.0686(11) Uani 1 1 d . . . C9 C 0.25248(13) 0.5242(2) 0.6158(2) 0.0788(13) Uani 1 1 d . . . C10 C 0.22870(14) 0.6268(3) 0.4470(2) 0.0803(13) Uani 1 1 d . . . H10A H 0.2420 0.5809 0.4605 0.096 Uiso 1 1 calc R . . C11 C 0.24375(15) 0.6727(3) 0.4174(3) 0.0930(16) Uani 1 1 d . . . H11A H 0.2670 0.6578 0.4120 0.112 Uiso 1 1 calc R . . C12 C 0.22446(14) 0.7388(3) 0.3967(2) 0.0896(14) Uani 1 1 d . . . H12A H 0.2342 0.7694 0.3765 0.107 Uiso 1 1 calc R . . C13 C 0.18951(12) 0.7625(2) 0.40531(18) 0.0674(10) Uani 1 1 d . . . C14 C 0.16717(15) 0.8306(2) 0.3842(2) 0.0780(13) Uani 1 1 d . . . H14A H 0.1749 0.8633 0.3628 0.094 Uiso 1 1 calc R . . C15 C 0.13437(15) 0.8481(2) 0.3954(2) 0.0771(13) Uani 1 1 d . . . H15A H 0.1204 0.8936 0.3823 0.092 Uiso 1 1 calc R . . C16 C 0.12037(13) 0.7991(2) 0.42673(19) 0.0675(11) Uani 1 1 d . . . H16A H 0.0974 0.8124 0.4333 0.081 Uiso 1 1 calc R . . C17 C 0.14129(11) 0.73227(19) 0.44689(16) 0.0564(9) Uani 1 1 d . . . C18 C 0.17610(11) 0.7127(2) 0.43570(16) 0.0587(9) Uani 1 1 d . . . C19 C -0.02228(11) 0.5213(2) 0.38707(17) 0.0628(10) Uani 1 1 d . . . H19A H -0.0417 0.5555 0.3541 0.075 Uiso 1 1 calc R . . C20 C -0.04233(12) 0.4556(3) 0.3874(2) 0.0747(12) Uani 1 1 d U . . H20A H -0.0743 0.4468 0.3553 0.090 Uiso 1 1 calc R . . C21 C -0.01501(12) 0.4057(2) 0.43423(19) 0.0709(11) Uani 1 1 d U . . H21A H -0.0280 0.3617 0.4342 0.085 Uiso 1 1 calc R . . C22 C 0.03365(11) 0.4195(2) 0.48394(18) 0.0601(9) Uani 1 1 d . . . C23 C 0.06472(14) 0.3720(2) 0.5369(2) 0.0739(12) Uani 1 1 d . . . H23A H 0.0539 0.3277 0.5410 0.089 Uiso 1 1 calc R . . C24 C 0.11006(15) 0.3909(2) 0.5814(2) 0.0796(13) Uani 1 1 d . . . H24A H 0.1305 0.3585 0.6156 0.096 Uiso 1 1 calc R . . C25 C 0.12773(13) 0.4577(2) 0.5780(2) 0.0731(13) Uani 1 1 d . . . H25A H 0.1592 0.4693 0.6103 0.088 Uiso 1 1 calc R . . C26 C 0.09888(10) 0.50600(18) 0.52769(16) 0.0528(8) Uani 1 1 d . . . C27 C 0.05094(10) 0.48716(18) 0.48001(15) 0.0499(8) Uani 1 1 d . . . C28 C -0.02490(17) 0.6952(3) 0.3010(2) 0.0860(15) Uani 1 1 d . . . H28A H -0.0195 0.6615 0.2776 0.103 Uiso 1 1 calc R . . C29 C -0.0632(2) 0.7422(4) 0.2646(2) 0.119(2) Uani 1 1 d . . . H29A H -0.0836 0.7391 0.2176 0.143 Uiso 1 1 calc R . . C30 C -0.0705(2) 0.7923(4) 0.2985(3) 0.135(3) Uani 1 1 d . . . H30A H -0.0955 0.8245 0.2743 0.162 Uiso 1 1 calc R . . C31 C -0.04090(19) 0.7964(3) 0.3691(3) 0.1028(18) Uani 1 1 d . . . C32 C -0.0466(2) 0.8469(4) 0.4082(3) 0.133(3) Uani 1 1 d . . . H32A H -0.0711 0.8805 0.3872 0.160 Uiso 1 1 calc R . . C33 C -0.0155(2) 0.8452(3) 0.4773(3) 0.113(2) Uani 1 1 d . . . H33A H -0.0193 0.8786 0.5027 0.136 Uiso 1 1 calc R . . C34 C 0.02195(14) 0.7952(3) 0.5118(2) 0.0790(13) Uani 1 1 d . . . H34A H 0.0421 0.7957 0.5590 0.095 Uiso 1 1 calc R . . C35 C 0.02859(11) 0.7456(2) 0.47565(18) 0.0599(9) Uani 1 1 d . . . C36 C -0.00308(13) 0.7471(2) 0.40339(19) 0.0663(11) Uani 1 1 d . . . C51 C 0.08897(13) 0.5389(3) 0.35906(17) 0.0746(12) Uani 1 1 d DU . . C52A C 0.0801(4) 0.5140(7) 0.2934(3) 0.111(3) Uani 0.524(13) 1 d PDU C 1 H52A H 0.0858 0.5533 0.2730 0.167 Uiso 0.524(13) 1 calc PR C 1 H52B H 0.0479 0.4983 0.2633 0.167 Uiso 0.524(13) 1 calc PR C 1 H52C H 0.1009 0.4746 0.3021 0.167 Uiso 0.524(13) 1 calc PR C 1 C52B C 0.0711(5) 0.4873(6) 0.3005(4) 0.111(3) Uani 0.476(13) 1 d PDU C 2 H52D H 0.0633 0.4418 0.3109 0.167 Uiso 0.476(13) 1 calc PR C 2 H52E H 0.0951 0.4801 0.2929 0.167 Uiso 0.476(13) 1 calc PR C 2 H52F H 0.0434 0.5072 0.2603 0.167 Uiso 0.476(13) 1 calc PR C 2 C102 C 0.15272(15) 0.8630(2) 0.6042(2) 0.0801(13) Uani 1 1 d D A . C103 C 0.18975(16) 0.8667(3) 0.6702(2) 0.0886(16) Uani 1 1 d . . . H10B H 0.1987 0.9112 0.6921 0.106 Uiso 1 1 calc R A . C104 C 0.21476(14) 0.8046(3) 0.7059(2) 0.0863(15) Uani 1 1 d D A . C107 C 0.12356(13) 0.7073(3) 0.7090(2) 0.0807(13) Uani 1 1 d D . . C108 C 0.15231(16) 0.6511(3) 0.7522(2) 0.0870(15) Uani 1 1 d . B . H10C H 0.1592 0.6481 0.7955 0.104 Uiso 1 1 calc R . . C109 C 0.17071(13) 0.5999(2) 0.73165(19) 0.0772(13) Uani 1 1 d D . . C1A C -0.0341(3) 0.00902(7) 0.3440(5) 0.485(19) Uiso 0.50 1 d PD . . H1AA H -0.0195 0.0090 0.3920 0.728 Uiso 0.50 1 calc PR . . H1AB H -0.0534 -0.0334 0.3241 0.728 Uiso 0.50 1 calc PR . . H1AC H -0.0534 0.0514 0.3241 0.728 Uiso 0.50 1 calc PR . . C2A C 0.0033(3) 0.00904(12) 0.3311(3) 0.485(19) Uiso 0.50 1 d PD . . H2AA H 0.0230 0.0515 0.3518 0.583 Uiso 0.50 1 calc PR . . H2AB H 0.0230 -0.0334 0.3518 0.583 Uiso 0.50 1 calc PR . . C3A C -0.01861(12) 0.00902(9) 0.2565(2) 0.485(19) Uiso 0.50 1 d PD . . H3AA H -0.0384 -0.0335 0.2359 0.583 Uiso 0.50 1 calc PR . . H3AB H -0.0384 0.0515 0.2359 0.583 Uiso 0.50 1 calc PR . . C4A C 0.1412(4) 0.2707(5) 0.4694(14) 0.743(17) Uiso 0.50 1 d PD . . H4AA H 0.1620 0.2736 0.4548 0.891 Uiso 0.50 1 calc PR . . H4AB H 0.1562 0.2959 0.5124 0.891 Uiso 0.50 1 calc PR . . Cl1 Cl 0.0877(5) 0.3123(9) 0.4094(13) 0.743(17) Uiso 0.50 1 d PD . . Cl2 Cl 0.1327(8) 0.1805(6) 0.4801(13) 0.743(17) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.03879(7) 0.06332(10) 0.04691(8) 0.00136(6) 0.01836(6) -0.01078(6) Zn1 0.04828(15) 0.0658(2) 0.06443(19) 0.00818(16) 0.03045(14) -0.00120(16) Zn2 0.04540(15) 0.0609(2) 0.04717(16) 0.00505(14) 0.02194(12) -0.00188(15) N1 0.0689(17) 0.076(2) 0.093(2) 0.0189(17) 0.0383(15) 0.0112(16) N2 0.0529(11) 0.080(2) 0.0626(13) -0.0003(13) 0.0345(10) -0.0097(13) N3 0.0447(10) 0.0637(15) 0.0462(11) 0.0043(10) 0.0239(9) -0.0033(11) N4 0.0599(14) 0.0769(18) 0.0509(13) 0.0127(12) 0.0283(11) 0.0094(14) O1 0.0386(9) 0.0817(16) 0.0614(12) 0.0118(11) 0.0220(8) -0.0033(10) O2 0.0510(9) 0.0625(13) 0.0546(10) 0.0081(9) 0.0298(8) -0.0063(9) O3 0.0411(8) 0.0559(12) 0.0557(10) 0.0042(9) 0.0213(8) -0.0104(8) O4 0.0402(9) 0.0635(13) 0.0539(10) 0.0029(9) 0.0221(8) 0.0007(9) O5 0.0666(12) 0.100(2) 0.0555(11) 0.0014(12) 0.0344(9) 0.0047(13) O6 0.0667(13) 0.0840(18) 0.0767(15) -0.0060(13) 0.0363(11) -0.0042(13) O7 0.0800(14) 0.0657(15) 0.0622(12) -0.0055(11) 0.0354(11) -0.0205(12) O8 0.0541(13) 0.0883(18) 0.0722(16) -0.0121(14) 0.0188(12) -0.0201(13) O9 0.0606(12) 0.0937(19) 0.0626(12) -0.0073(12) 0.0330(10) -0.0069(13) O10 0.0649(11) 0.0798(16) 0.0623(12) 0.0107(11) 0.0340(9) -0.0059(12) C101 0.172(2) 0.082(3) 0.138(2) 0.016(2) 0.0807(17) 0.008(2) F1 0.171(2) 0.0930(15) 0.1464(19) 0.0106(14) 0.0810(17) 0.0104(16) F2 0.171(2) 0.0930(15) 0.1464(19) 0.0106(14) 0.0810(17) 0.0104(16) F3 0.171(2) 0.0930(15) 0.1464(19) 0.0106(14) 0.0810(17) 0.0104(16) F1B 0.171(2) 0.0930(15) 0.1464(19) 0.0106(14) 0.0810(17) 0.0104(16) F2B 0.171(2) 0.0930(15) 0.1464(19) 0.0106(14) 0.0810(17) 0.0104(16) F3B 0.171(2) 0.0930(15) 0.1464(19) 0.0106(14) 0.0810(17) 0.0104(16) C15A 0.0902(7) 0.1735(9) 0.0993(9) -0.0333(12) 0.0074(8) -0.0348(9) F4 0.1017(11) 0.1727(11) 0.0866(12) -0.0353(11) 0.0078(9) -0.0259(10) F5 0.1017(11) 0.1727(11) 0.0866(12) -0.0353(11) 0.0078(9) -0.0259(10) F6 0.1017(11) 0.1727(11) 0.0866(12) -0.0353(11) 0.0078(9) -0.0259(10) C15B 0.0902(7) 0.1735(9) 0.0993(9) -0.0333(12) 0.0074(8) -0.0348(9) F4B 0.1017(11) 0.1727(11) 0.0866(12) -0.0353(11) 0.0078(9) -0.0259(10) F5B 0.1017(11) 0.1727(11) 0.0866(12) -0.0353(11) 0.0078(9) -0.0259(10) F6B 0.1017(11) 0.1727(11) 0.0866(12) -0.0353(11) 0.0078(9) -0.0259(10) C16A 0.150(2) 0.199(3) 0.140(2) -0.041(3) 0.1076(19) -0.024(3) F7 0.1413(15) 0.197(2) 0.1516(14) -0.0438(16) 0.1083(12) -0.0106(18) F8 0.1413(15) 0.197(2) 0.1516(14) -0.0438(16) 0.1083(12) -0.0106(18) F9 0.1413(15) 0.197(2) 0.1516(14) -0.0438(16) 0.1083(12) -0.0106(18) C16B 0.150(2) 0.199(3) 0.140(2) -0.041(3) 0.1076(19) -0.024(3) F7B 0.1413(15) 0.197(2) 0.1516(14) -0.0438(16) 0.1083(12) -0.0106(18) F8B 0.1413(15) 0.197(2) 0.1516(14) -0.0438(16) 0.1083(12) -0.0106(18) F9B 0.1413(15) 0.197(2) 0.1516(14) -0.0438(16) 0.1083(12) -0.0106(18) C11A 0.1389(19) 0.189(3) 0.1384(19) 0.090(2) 0.0856(18) 0.028(2) F10 0.1425(17) 0.186(2) 0.1480(15) 0.0860(15) 0.0875(14) 0.0346(18) F11 0.1425(17) 0.186(2) 0.1480(15) 0.0860(15) 0.0875(14) 0.0346(18) F12 0.1425(17) 0.186(2) 0.1480(15) 0.0860(15) 0.0875(14) 0.0346(18) C11B 0.1389(19) 0.189(3) 0.1384(19) 0.090(2) 0.0856(18) 0.028(2) F10B 0.1425(17) 0.186(2) 0.1480(15) 0.0860(15) 0.0875(14) 0.0346(18) F11B 0.1425(17) 0.186(2) 0.1480(15) 0.0860(15) 0.0875(14) 0.0346(18) F12B 0.1425(17) 0.186(2) 0.1480(15) 0.0860(15) 0.0875(14) 0.0346(18) C1 0.131(4) 0.103(4) 0.138(5) 0.015(3) 0.058(4) 0.053(3) C2 0.187(6) 0.134(5) 0.179(7) 0.030(5) 0.093(5) 0.085(5) C3 0.118(4) 0.137(5) 0.160(6) 0.034(5) 0.045(5) 0.057(4) C4 0.073(2) 0.102(3) 0.113(3) 0.040(3) 0.039(2) 0.025(2) C5 0.074(3) 0.138(4) 0.108(3) 0.062(3) 0.031(3) 0.031(3) C6 0.055(2) 0.126(4) 0.082(3) 0.040(3) 0.017(2) -0.002(2) C7 0.0474(16) 0.106(3) 0.065(2) 0.024(2) 0.0185(15) -0.0094(19) C8 0.0368(12) 0.086(2) 0.0707(17) 0.0263(16) 0.0241(12) -0.0080(14) C9 0.0548(16) 0.081(2) 0.090(2) 0.0292(19) 0.0361(16) 0.0075(17) C10 0.0624(17) 0.095(3) 0.086(2) 0.004(2) 0.0447(15) -0.0022(19) C11 0.0715(17) 0.132(4) 0.098(2) -0.005(2) 0.0624(15) -0.011(2) C12 0.0793(17) 0.120(3) 0.084(2) 0.003(2) 0.0555(15) -0.030(2) C13 0.0627(15) 0.083(2) 0.0549(15) 0.0002(15) 0.0327(12) -0.0250(16) C14 0.0803(19) 0.076(2) 0.0706(19) 0.0049(17) 0.0397(16) -0.0278(18) C15 0.083(2) 0.066(2) 0.070(2) 0.0090(17) 0.0371(17) -0.0099(19) C16 0.0689(17) 0.071(2) 0.0633(17) 0.0047(15) 0.0384(14) -0.0059(17) C17 0.0471(13) 0.0647(19) 0.0456(14) 0.0047(13) 0.0200(11) -0.0136(13) C18 0.0492(14) 0.070(2) 0.0469(14) 0.0001(14) 0.0221(11) -0.0118(14) C19 0.0464(14) 0.085(2) 0.0468(15) 0.0028(15) 0.0209(12) -0.0067(15) C20 0.0470(15) 0.102(3) 0.0606(18) -0.0077(17) 0.0228(13) -0.0245(17) C21 0.0620(15) 0.077(2) 0.0698(18) -0.0047(15) 0.0356(13) -0.0254(15) C22 0.0531(13) 0.0651(19) 0.0624(15) -0.0022(14) 0.0335(11) -0.0148(14) C23 0.0670(17) 0.065(2) 0.080(2) 0.0109(17) 0.0370(15) -0.0134(16) C24 0.071(2) 0.068(2) 0.086(2) 0.0239(18) 0.0370(17) 0.0015(18) C25 0.0446(15) 0.073(2) 0.078(2) 0.0203(18) 0.0213(15) -0.0011(16) C26 0.0409(11) 0.0577(17) 0.0565(14) 0.0043(12) 0.0263(10) -0.0053(12) C27 0.0415(11) 0.0588(17) 0.0489(12) 0.0023(12) 0.0259(9) -0.0060(12) C28 0.078(2) 0.105(3) 0.0521(19) 0.015(2) 0.0248(18) 0.020(2) C29 0.105(3) 0.155(5) 0.051(2) 0.024(3) 0.018(2) 0.061(3) C30 0.116(4) 0.158(5) 0.080(3) 0.032(3) 0.026(3) 0.077(4) C31 0.095(3) 0.113(3) 0.082(3) 0.021(3) 0.041(2) 0.046(3) C32 0.107(3) 0.147(4) 0.089(3) -0.005(3) 0.024(3) 0.065(3) C33 0.116(3) 0.107(3) 0.109(3) 0.004(3) 0.061(3) 0.047(3) C34 0.0628(19) 0.090(3) 0.068(2) -0.006(2) 0.0285(16) 0.009(2) C35 0.0474(13) 0.068(2) 0.0627(16) 0.0021(14) 0.0308(11) -0.0009(14) C36 0.0569(16) 0.073(2) 0.0586(17) 0.0144(16) 0.0276(13) 0.0102(16) C51 0.0686(17) 0.094(3) 0.0618(17) -0.0026(17) 0.0381(14) -0.0046(19) C52A 0.114(4) 0.129(5) 0.079(3) -0.014(3) 0.049(3) 0.017(4) C52B 0.114(4) 0.129(5) 0.079(3) -0.014(3) 0.049(3) 0.017(4) C102 0.082(2) 0.073(2) 0.082(2) -0.0082(18) 0.0453(17) -0.0169(19) C103 0.076(2) 0.082(3) 0.086(3) -0.025(2) 0.034(2) -0.024(2) C104 0.0585(19) 0.107(3) 0.076(2) -0.022(2) 0.0286(17) -0.030(2) C107 0.0755(19) 0.106(3) 0.0628(18) -0.0188(19) 0.0414(15) -0.029(2) C108 0.083(2) 0.115(3) 0.0542(18) -0.002(2) 0.0345(16) -0.021(2) C109 0.0592(17) 0.103(3) 0.0559(18) 0.0116(18) 0.0254(14) -0.0159(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 Tb1 O1 2.314(3) . ? Tb1 O4 2.315(2) . ? Tb1 O7 2.370(3) . ? Tb1 O8 2.373(3) . ? Tb1 O10 2.380(3) . ? Tb1 O9 2.385(3) . ? Tb1 O3 2.414(2) . ? Tb1 O2 2.442(3) . ? Tb1 Zn1 3.3099(11) . ? Tb1 Zn2 3.3224(14) . ? Zn1 O6 2.026(3) . ? Zn1 N1 2.068(4) . ? Zn1 N2 2.114(4) . ? Zn1 O2 2.140(2) . ? Zn1 O1 2.147(3) . ? Zn1 O3 2.260(3) . ? Zn2 O5 2.051(3) . ? Zn2 N4 2.068(3) . ? Zn2 N3 2.096(3) . ? Zn2 O4 2.126(3) . ? Zn2 O3 2.155(2) . ? Zn2 O2 2.298(2) . ? N1 C1 1.325(8) . ? N1 C9 1.352(6) . ? N2 C10 1.325(6) . ? N2 C18 1.362(5) . ? N3 C19 1.310(4) . ? N3 C27 1.370(4) . ? N4 C28 1.326(5) . ? N4 C36 1.367(6) . ? O1 C8 1.319(4) . ? O2 C17 1.349(4) . ? O3 C26 1.358(4) . ? O4 C35 1.325(4) . ? O5 C51 1.256(5) . ? O6 C51 1.262(4) . ? O7 C102 1.246(5) . ? O8 C104 1.255(6) . ? O9 C107 1.260(5) . ? O10 C109 1.252(5) . ? C101 F1B 1.300(7) . ? C101 F1 1.308(6) . ? C101 F2 1.320(6) . ? C101 F3B 1.338(6) . ? C101 F3 1.381(7) . ? C101 F2B 1.385(7) . ? C101 C102 1.489(5) . ? C15A F5 1.335(7) . ? C15A F4 1.336(7) . ? C15A F6 1.343(8) . ? C15A C104 1.510(6) . ? C15B F6B 1.339(8) . ? C15B F4B 1.340(7) . ? C15B F5B 1.340(8) . ? C15B C104 1.508(6) . ? C16A F8 1.334(8) . ? C16A F9 1.340(7) . ? C16A F7 1.341(7) . ? C16A C107 1.494(7) . ? C16B F9B 1.327(7) . ? C16B F8B 1.335(6) . ? C16B F7B 1.349(7) . ? C16B C107 1.494(7) . ? C11A F11 1.321(7) . ? C11A F12 1.343(8) . ? C11A F10 1.343(7) . ? C11A C109 1.496(6) . ? C11B F11B 1.332(8) . ? C11B F12B 1.336(7) . ? C11B F10B 1.355(7) . ? C11B C109 1.501(6) . ? C1 C2 1.436(9) . ? C1 H1A 0.9300 . ? C2 C3 1.386(11) . ? C2 H2A 0.9300 . ? C3 C4 1.380(11) . ? C3 H3A 0.9300 . ? C4 C5 1.404(8) . ? C4 C9 1.418(6) . ? C5 C6 1.315(9) . ? C5 H5A 0.9300 . ? C6 C7 1.398(6) . ? C6 H6A 0.9300 . ? C7 C8 1.368(5) . ? C7 H7A 0.9300 . ? C8 C9 1.439(7) . ? C10 C11 1.391(8) . ? C10 H10A 0.9300 . ? C11 C12 1.343(8) . ? C11 H11A 0.9300 . ? C12 C13 1.414(7) . ? C12 H12A 0.9300 . ? C13 C14 1.410(6) . ? C13 C18 1.414(6) . ? C14 C15 1.353(8) . ? C14 H14A 0.9300 . ? C15 C16 1.433(7) . ? C15 H15A 0.9300 . ? C16 C17 1.372(5) . ? C16 H16A 0.9300 . ? C17 C18 1.429(6) . ? C19 C20 1.402(6) . ? C19 H19A 0.9300 . ? C20 C21 1.338(6) . ? C20 H20A 0.9300 . ? C21 C22 1.420(5) . ? C21 H21A 0.9300 . ? C22 C23 1.406(5) . ? C22 C27 1.414(5) . ? C23 C24 1.342(5) . ? C23 H23A 0.9300 . ? C24 C25 1.403(6) . ? C24 H24A 0.9300 . ? C25 C26 1.367(5) . ? C25 H25A 0.9300 . ? C26 C27 1.415(4) . ? C28 C29 1.395(7) . ? C28 H28A 0.9300 . ? C29 C30 1.352(10) . ? C29 H29A 0.9300 . ? C30 C31 1.394(8) . ? C30 H30A 0.9300 . ? C31 C36 1.409(6) . ? C31 C32 1.420(10) . ? C32 C33 1.367(8) . ? C32 H32A 0.9300 . ? C33 C34 1.410(7) . ? C33 H33A 0.9300 . ? C34 C35 1.374(7) . ? C34 H34A 0.9300 . ? C35 C36 1.427(5) . ? C51 C52A 1.501(8) . ? C51 C52B 1.511(8) . ? C52A H52A 0.9600 . ? C52A H52B 0.9600 . ? C52A H52C 0.9600 . ? C52B H52D 0.9600 . ? C52B H52E 0.9600 . ? C52B H52F 0.9600 . ? C102 C103 1.353(6) . ? C103 C104 1.396(7) . ? C103 H10B 0.9300 . ? C107 C108 1.401(7) . ? C108 C109 1.384(8) . ? C108 H10C 0.9300 . ? C1A C2A 1.498(9) . ? C1A H1AA 0.9600 . ? C1A H1AB 0.9600 . ? C1A H1AC 0.9600 . ? C2A C3A 1.498(7) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A C3A 1.496(8) 2 ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C4A Cl2 1.739(9) . ? C4A Cl1 1.742(9) . ? C4A H4AA 0.9700 . ? C4A H4AB 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O4 137.71(9) . . ? O1 Tb1 O7 115.02(11) . . ? O4 Tb1 O7 78.12(9) . . ? O1 Tb1 O8 77.97(11) . . ? O4 Tb1 O8 141.19(10) . . ? O7 Tb1 O8 70.58(10) . . ? O1 Tb1 O10 78.18(10) . . ? O4 Tb1 O10 118.33(9) . . ? O7 Tb1 O10 140.45(10) . . ? O8 Tb1 O10 76.83(11) . . ? O1 Tb1 O9 142.62(9) . . ? O4 Tb1 O9 77.23(10) . . ? O7 Tb1 O9 79.36(12) . . ? O8 Tb1 O9 74.98(12) . . ? O10 Tb1 O9 70.93(11) . . ? O1 Tb1 O3 73.04(8) . . ? O4 Tb1 O3 72.07(8) . . ? O7 Tb1 O3 138.01(9) . . ? O8 Tb1 O3 146.33(9) . . ? O10 Tb1 O3 80.77(9) . . ? O9 Tb1 O3 120.51(10) . . ? O1 Tb1 O2 71.33(8) . . ? O4 Tb1 O2 72.00(9) . . ? O7 Tb1 O2 80.10(10) . . ? O8 Tb1 O2 122.50(11) . . ? O10 Tb1 O2 137.84(10) . . ? O9 Tb1 O2 145.83(8) . . ? O3 Tb1 O2 63.09(8) . . ? O1 Tb1 Zn1 40.19(6) . . ? O4 Tb1 Zn1 97.52(8) . . ? O7 Tb1 Zn1 115.76(9) . . ? O8 Tb1 Zn1 116.31(9) . . ? O10 Tb1 Zn1 98.34(9) . . ? O9 Tb1 Zn1 162.98(8) . . ? O3 Tb1 Zn1 43.07(6) . . ? O2 Tb1 Zn1 40.25(6) . . ? O1 Tb1 Zn2 98.38(7) . . ? O4 Tb1 Zn2 39.46(7) . . ? O7 Tb1 Zn2 98.82(7) . . ? O8 Tb1 Zn2 165.31(9) . . ? O10 Tb1 Zn2 116.65(7) . . ? O9 Tb1 Zn2 113.90(7) . . ? O3 Tb1 Zn2 40.37(5) . . ? O2 Tb1 Zn2 43.74(6) . . ? Zn1 Tb1 Zn2 58.24(3) . . ? O6 Zn1 N1 94.25(14) . . ? O6 Zn1 N2 94.54(14) . . ? N1 Zn1 N2 100.93(16) . . ? O6 Zn1 O2 106.68(10) . . ? N1 Zn1 O2 159.05(13) . . ? N2 Zn1 O2 78.64(12) . . ? O6 Zn1 O1 164.87(13) . . ? N1 Zn1 O1 78.78(14) . . ? N2 Zn1 O1 99.94(12) . . ? O2 Zn1 O1 80.67(9) . . ? O6 Zn1 O3 90.55(12) . . ? N1 Zn1 O3 109.33(15) . . ? N2 Zn1 O3 148.85(11) . . ? O2 Zn1 O3 70.47(9) . . ? O1 Zn1 O3 79.33(10) . . ? O6 Zn1 Tb1 132.67(10) . . ? N1 Zn1 Tb1 116.28(13) . . ? N2 Zn1 Tb1 112.43(10) . . ? O2 Zn1 Tb1 47.51(7) . . ? O1 Zn1 Tb1 44.06(7) . . ? O3 Zn1 Tb1 46.83(6) . . ? O5 Zn2 N4 94.03(13) . . ? O5 Zn2 N3 94.66(12) . . ? N4 Zn2 N3 101.47(12) . . ? O5 Zn2 O4 162.63(12) . . ? N4 Zn2 O4 79.46(12) . . ? N3 Zn2 O4 102.39(11) . . ? O5 Zn2 O3 105.93(11) . . ? N4 Zn2 O3 160.01(13) . . ? N3 Zn2 O3 78.28(9) . . ? O4 Zn2 O3 81.09(10) . . ? O5 Zn2 O2 89.10(11) . . ? N4 Zn2 O2 110.66(11) . . ? N3 Zn2 O2 147.31(9) . . ? O4 Zn2 O2 78.37(10) . . ? O3 Zn2 O2 69.49(8) . . ? O5 Zn2 Tb1 131.55(8) . . ? N4 Zn2 Tb1 117.98(9) . . ? N3 Zn2 Tb1 111.57(7) . . ? O4 Zn2 Tb1 43.79(6) . . ? O3 Zn2 Tb1 46.51(6) . . ? O2 Zn2 Tb1 47.31(7) . . ? C1 N1 C9 120.8(4) . . ? C1 N1 Zn1 125.2(4) . . ? C9 N1 Zn1 113.3(3) . . ? C10 N2 C18 118.9(4) . . ? C10 N2 Zn1 128.1(3) . . ? C18 N2 Zn1 112.9(3) . . ? C19 N3 C27 118.6(3) . . ? C19 N3 Zn2 127.5(2) . . ? C27 N3 Zn2 113.67(19) . . ? C28 N4 C36 120.1(4) . . ? C28 N4 Zn2 126.9(3) . . ? C36 N4 Zn2 112.8(2) . . ? C8 O1 Zn1 112.2(3) . . ? C8 O1 Tb1 141.9(3) . . ? Zn1 O1 Tb1 95.74(8) . . ? C17 O2 Zn1 112.6(2) . . ? C17 O2 Zn2 126.77(17) . . ? Zn1 O2 Zn2 93.25(9) . . ? C17 O2 Tb1 132.6(2) . . ? Zn1 O2 Tb1 92.24(8) . . ? Zn2 O2 Tb1 88.95(9) . . ? C26 O3 Zn2 111.89(16) . . ? C26 O3 Zn1 122.1(2) . . ? Zn2 O3 Zn1 93.90(10) . . ? C26 O3 Tb1 135.8(2) . . ? Zn2 O3 Tb1 93.12(9) . . ? Zn1 O3 Tb1 90.10(8) . . ? C35 O4 Zn2 112.1(2) . . ? C35 O4 Tb1 141.5(2) . . ? Zn2 O4 Tb1 96.75(10) . . ? C51 O5 Zn2 126.2(2) . . ? C51 O6 Zn1 126.7(3) . . ? C102 O7 Tb1 135.2(3) . . ? C104 O8 Tb1 134.4(3) . . ? C107 O9 Tb1 134.3(3) . . ? C109 O10 Tb1 134.7(3) . . ? F1B C101 F1 45.8(6) . . ? F1B C101 F2 123.3(5) . . ? F1 C101 F2 113.4(6) . . ? F1B C101 F3B 109.4(6) . . ? F1 C101 F3B 127.9(6) . . ? F2 C101 F3B 32.6(6) . . ? F1B C101 F3 53.8(5) . . ? F1 C101 F3 99.4(5) . . ? F2 C101 F3 103.4(5) . . ? F3B C101 F3 72.4(6) . . ? F1B C101 F2B 102.8(6) . . ? F1 C101 F2B 59.2(5) . . ? F2 C101 F2B 69.5(5) . . ? F3B C101 F2B 101.1(6) . . ? F3 C101 F2B 148.1(5) . . ? F1B C101 C102 120.4(5) . . ? F1 C101 C102 116.1(4) . . ? F2 C101 C102 115.7(5) . . ? F3B C101 C102 115.5(5) . . ? F3 C101 C102 106.2(5) . . ? F2B C101 C102 104.7(5) . . ? F5 C15A F4 108.6(6) . . ? F5 C15A F6 105.6(6) . . ? F4 C15A F6 105.4(7) . . ? F5 C15A C104 114.2(6) . . ? F4 C15A C104 111.7(5) . . ? F6 C15A C104 110.9(5) . . ? F6B C15B F4B 104.9(7) . . ? F6B C15B F5B 103.0(7) . . ? F4B C15B F5B 106.2(7) . . ? F6B C15B C104 114.9(6) . . ? F4B C15B C104 118.1(6) . . ? F5B C15B C104 108.4(6) . . ? F8 C16A F9 105.4(7) . . ? F8 C16A F7 105.8(7) . . ? F9 C16A F7 106.4(7) . . ? F8 C16A C107 112.9(7) . . ? F9 C16A C107 111.5(6) . . ? F7 C16A C107 114.2(7) . . ? F9B C16B F8B 107.1(6) . . ? F9B C16B F7B 103.9(6) . . ? F8B C16B F7B 106.2(6) . . ? F9B C16B C107 116.4(5) . . ? F8B C16B C107 112.0(5) . . ? F7B C16B C107 110.5(6) . . ? F11 C11A F12 108.6(6) . . ? F11 C11A F10 106.8(7) . . ? F12 C11A F10 101.5(7) . . ? F11 C11A C109 109.4(6) . . ? F12 C11A C109 116.7(6) . . ? F10 C11A C109 113.2(5) . . ? F11B C11B F12B 111.3(6) . . ? F11B C11B F10B 101.7(6) . . ? F12B C11B F10B 102.3(7) . . ? F11B C11B C109 117.0(6) . . ? F12B C11B C109 113.8(6) . . ? F10B C11B C109 108.9(5) . . ? N1 C1 C2 120.6(6) . . ? N1 C1 H1A 119.7 . . ? C2 C1 H1A 119.7 . . ? C3 C2 C1 117.4(8) . . ? C3 C2 H2A 121.3 . . ? C1 C2 H2A 121.3 . . ? C4 C3 C2 122.7(6) . . ? C4 C3 H3A 118.6 . . ? C2 C3 H3A 118.6 . . ? C3 C4 C5 124.9(5) . . ? C3 C4 C9 115.8(5) . . ? C5 C4 C9 119.3(6) . . ? C6 C5 C4 120.0(5) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C7 122.4(5) . . ? C5 C6 H6A 118.8 . . ? C7 C6 H6A 118.8 . . ? C8 C7 C6 121.6(5) . . ? C8 C7 H7A 119.2 . . ? C6 C7 H7A 119.2 . . ? O1 C8 C7 125.5(4) . . ? O1 C8 C9 117.5(3) . . ? C7 C8 C9 117.0(4) . . ? N1 C9 C4 122.6(5) . . ? N1 C9 C8 117.6(3) . . ? C4 C9 C8 119.8(4) . . ? N2 C10 C11 122.5(5) . . ? N2 C10 H10A 118.7 . . ? C11 C10 H10A 118.7 . . ? C12 C11 C10 119.4(5) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C11 C12 C13 120.9(5) . . ? C11 C12 H12A 119.5 . . ? C13 C12 H12A 119.5 . . ? C14 C13 C18 119.5(4) . . ? C14 C13 C12 124.3(4) . . ? C18 C13 C12 116.2(4) . . ? C15 C14 C13 119.4(4) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 122.4(4) . . ? C14 C15 H15A 118.8 . . ? C16 C15 H15A 118.8 . . ? C17 C16 C15 119.0(4) . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? O2 C17 C16 122.6(4) . . ? O2 C17 C18 117.8(3) . . ? C16 C17 C18 119.5(4) . . ? N2 C18 C13 122.1(4) . . ? N2 C18 C17 117.9(3) . . ? C13 C18 C17 120.1(4) . . ? N3 C19 C20 123.2(3) . . ? N3 C19 H19A 118.4 . . ? C20 C19 H19A 118.4 . . ? C21 C20 C19 119.3(3) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C20 C21 C22 120.5(4) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C23 C22 C27 118.8(3) . . ? C23 C22 C21 124.8(4) . . ? C27 C22 C21 116.4(3) . . ? C24 C23 C22 119.7(4) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C23 C24 C25 122.2(4) . . ? C23 C24 H24A 118.9 . . ? C25 C24 H24A 118.9 . . ? C26 C25 C24 120.4(3) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? O3 C26 C25 123.6(3) . . ? O3 C26 C27 118.0(3) . . ? C25 C26 C27 118.4(3) . . ? N3 C27 C22 122.0(3) . . ? N3 C27 C26 117.4(3) . . ? C22 C27 C26 120.6(3) . . ? N4 C28 C29 121.5(5) . . ? N4 C28 H28A 119.2 . . ? C29 C28 H28A 119.2 . . ? C30 C29 C28 119.2(5) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? C29 C30 C31 121.0(5) . . ? C29 C30 H30A 119.5 . . ? C31 C30 H30A 119.5 . . ? C30 C31 C36 117.5(6) . . ? C30 C31 C32 124.2(5) . . ? C36 C31 C32 118.3(5) . . ? C33 C32 C31 118.8(5) . . ? C33 C32 H32A 120.6 . . ? C31 C32 H32A 120.6 . . ? C32 C33 C34 123.0(6) . . ? C32 C33 H33A 118.5 . . ? C34 C33 H33A 118.5 . . ? C35 C34 C33 119.8(4) . . ? C35 C34 H34A 120.1 . . ? C33 C34 H34A 120.1 . . ? O4 C35 C34 123.8(3) . . ? O4 C35 C36 118.1(4) . . ? C34 C35 C36 118.1(3) . . ? N4 C36 C31 120.6(4) . . ? N4 C36 C35 117.4(3) . . ? C31 C36 C35 122.0(4) . . ? O5 C51 O6 124.1(4) . . ? O5 C51 C52A 115.6(5) . . ? O6 C51 C52A 118.2(5) . . ? O5 C51 C52B 119.6(6) . . ? O6 C51 C52B 115.4(6) . . ? C52A C51 C52B 25.2(8) . . ? C51 C52A H52A 109.5 . . ? C51 C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C51 C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C51 C52B H52D 109.5 . . ? C51 C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C51 C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? O7 C102 C103 127.6(4) . . ? O7 C102 C101 115.7(4) . . ? C103 C102 C101 116.6(4) . . ? C102 C103 C104 121.0(4) . . ? C102 C103 H10B 119.5 . . ? C104 C103 H10B 119.5 . . ? O8 C104 C103 127.3(4) . . ? O8 C104 C15B 111.9(4) . . ? C103 C104 C15B 120.4(5) . . ? O8 C104 C15A 114.1(4) . . ? C103 C104 C15A 118.5(5) . . ? C15B C104 C15A 9.8(4) . . ? O9 C107 C108 127.0(4) . . ? O9 C107 C16A 117.6(4) . . ? C108 C107 C16A 115.4(4) . . ? O9 C107 C16B 111.8(4) . . ? C108 C107 C16B 121.2(5) . . ? C16A C107 C16B 5.8(3) . . ? C109 C108 C107 121.2(4) . . ? C109 C108 H10C 119.4 . . ? C107 C108 H10C 119.4 . . ? O10 C109 C108 127.3(4) . . ? O10 C109 C11A 115.9(5) . . ? C108 C109 C11A 116.8(5) . . ? O10 C109 C11B 114.1(5) . . ? C108 C109 C11B 118.5(5) . . ? C11A C109 C11B 2.6(3) . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C3A C2A C1A 110.6(7) . . ? C3A C2A H2AA 109.5 . . ? C1A C2A H2AA 109.5 . . ? C3A C2A H2AB 109.5 . . ? C1A C2A H2AB 109.5 . . ? H2AA C2A H2AB 108.1 . . ? C3A C3A C2A 110.7(5) 2 . ? C3A C3A H3AA 109.5 2 . ? C2A C3A H3AA 109.5 . . ? C3A C3A H3AB 109.5 2 . ? C2A C3A H3AB 109.5 . . ? H3AA C3A H3AB 108.1 . . ? Cl2 C4A Cl1 110.8(9) . . ? Cl2 C4A H4AA 109.5 . . ? Cl1 C4A H4AA 109.5 . . ? Cl2 C4A H4AB 109.5 . . ? Cl1 C4A H4AB 109.5 . . ? H4AA C4A H4AB 108.1 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.980 _refine_diff_density_min -1.488 _refine_diff_density_rms 0.245