# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Dr Zhen-Feng Chen' _publ_contact_author_address ; The Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China) School of Chemistry and Chemical Engineering Guangxi Normal University Guilin 541004 China ; _publ_contact_author_email chenzfubc@yahoo.com _publ_contact_author_fax '86 773 2120958' _publ_contact_author_phone '86 773 2120998' #========================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; High cytotoxicity of dihalo-substituted 8-quinolinolato-lanthanides ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Zhen-Feng Chen' ? ; The Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China) School of Chemistry and Chemical Engineering Guangxi Normal University Guilin 541004 China ; 'Xiao-Yan Song' ? ; The Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China) School of Chemistry and Chemical Engineering Guangxi Normal University Guilin 541004 China ; 'Yan Peng' ? ; The Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China) School of Chemistry and Chemical Engineering Guangxi Normal University Guilin 541004 China ; 'Xue Hong' ? ; The Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China) School of Chemistry and Chemical Engineering Guangxi Normal University Guilin 541004 China ; 'Yan-Cheng Liu' ? ; The Key Laboratory of Medicinal Chemical Resources and Molecular Engineering of Medicinal Resources (Ministry of Education of China) School of Chemistry and Chemical Engineering Guangxi Normal University Guilin 541004 China ; ; Hong Liang ; ? ; The Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China) School of Chemistry and Chemical Engineering Guangxi Normal University Guilin 541004 China ; #========================================================================== data_shelxl-a _database_code_depnum_ccdc_archive 'CCDC 794955' #TrackingRef '- CCDC794955CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H16 Cl6 Dy N3 O5, C2 H6 O, 1/3(C2 H6 O), 1/3(H2 O)' _chemical_formula_sum 'C29.67 H24.67 Cl6 Dy N3 O6.67' _chemical_formula_weight 905.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3:H' _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 21.7675(14) _cell_length_b 21.7675(14) _cell_length_c 37.171(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 15252.8(18) _cell_formula_units_Z 18 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 21106 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8010 _exptl_absorpt_coefficient_mu 2.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.188 _exptl_absorpt_correction_T_max 0.336 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26016 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6297 _reflns_number_gt 5772 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+57.7554P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6297 _refine_ls_number_parameters 429 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.488913(14) 0.462929(14) 0.571908(7) 0.03961(12) Uani 1 1 d . . . Cl1 Cl 0.40335(9) 0.30646(10) 0.45171(4) 0.0648(5) Uani 1 1 d . . . Cl2 Cl 0.13684(10) 0.20146(13) 0.49976(7) 0.0992(8) Uani 1 1 d . . . Cl3 Cl 0.44832(9) 0.39261(8) 0.71182(4) 0.0561(4) Uani 1 1 d . . . Cl4 Cl 0.54492(11) 0.21417(10) 0.68189(6) 0.0761(5) Uani 1 1 d . . . Cl5 Cl 0.70709(9) 0.53089(10) 0.48470(4) 0.0595(4) Uani 1 1 d . . . Cl6 Cl 0.87913(9) 0.68782(11) 0.59241(7) 0.0808(6) Uani 1 1 d . . . O1 O 0.4439(2) 0.3890(2) 0.52164(10) 0.0451(9) Uani 1 1 d . . . O2 O 0.4675(2) 0.4241(2) 0.63182(10) 0.0429(9) Uani 1 1 d . . . O3 O 0.5894(2) 0.5043(2) 0.53659(10) 0.0460(9) Uani 1 1 d . . . O4 O 0.4655(2) 0.5328(2) 0.53035(10) 0.0468(9) Uani 1 1 d D . . H4A H 0.502(2) 0.560(3) 0.5192(15) 0.056 Uiso 1 1 d D . . H4B H 0.441(3) 0.515(3) 0.5126(11) 0.056 Uiso 1 1 d D . . O5 O 0.4585(3) 0.5399(3) 0.60191(12) 0.0624(12) Uani 1 1 d D . . H5A H 0.452(4) 0.546(4) 0.6229(7) 0.075 Uiso 1 1 d D . . H5B H 0.446(4) 0.560(4) 0.5876(16) 0.075 Uiso 1 1 d D . . N1 N 0.3560(3) 0.3823(3) 0.57250(12) 0.0472(12) Uani 1 1 d . . . N2 N 0.5162(2) 0.3672(3) 0.58432(12) 0.0427(11) Uani 1 1 d . . . N3 N 0.6054(3) 0.5474(3) 0.60430(13) 0.0473(11) Uani 1 1 d . . . C1 C 0.3763(3) 0.3454(3) 0.51632(15) 0.0426(13) Uani 1 1 d . . . C2 C 0.3470(3) 0.3036(3) 0.48601(16) 0.0480(14) Uani 1 1 d . . . C3 C 0.2745(4) 0.2594(3) 0.48096(19) 0.0583(17) Uani 1 1 d . . . H3 H 0.2574 0.2325 0.4598 0.070 Uiso 1 1 calc R . . C4 C 0.2282(3) 0.2555(4) 0.5069(2) 0.0627(18) Uani 1 1 d . . . C5 C 0.2531(3) 0.2955(3) 0.53891(18) 0.0535(15) Uani 1 1 d . . . C6 C 0.2090(4) 0.2946(4) 0.5670(2) 0.069(2) Uani 1 1 d . . . H6 H 0.1595 0.2651 0.5655 0.083 Uiso 1 1 calc R . . C7 C 0.2386(4) 0.3364(5) 0.5961(2) 0.077(2) Uani 1 1 d . . . H7 H 0.2099 0.3365 0.6150 0.092 Uiso 1 1 calc R . . C8 C 0.3127(4) 0.3798(4) 0.59779(18) 0.0652(19) Uani 1 1 d . . . H8 H 0.3323 0.4086 0.6182 0.078 Uiso 1 1 calc R . . C9 C 0.3267(3) 0.3406(3) 0.54298(15) 0.0455(13) Uani 1 1 d . . . C10 C 0.4834(3) 0.3779(3) 0.64393(15) 0.0392(12) Uani 1 1 d . . . C11 C 0.4781(3) 0.3561(3) 0.67929(15) 0.0450(13) Uani 1 1 d . . . C12 C 0.4964(3) 0.3051(3) 0.69081(17) 0.0522(15) Uani 1 1 d . . . H12 H 0.4918 0.2922 0.7152 0.063 Uiso 1 1 calc R . . C13 C 0.5206(3) 0.2750(3) 0.66696(18) 0.0517(15) Uani 1 1 d . . . C14 C 0.5281(3) 0.2942(3) 0.62975(17) 0.0473(14) Uani 1 1 d . . . C15 C 0.5531(3) 0.2665(3) 0.60285(19) 0.0541(16) Uani 1 1 d . . . H15 H 0.5660 0.2325 0.6088 0.065 Uiso 1 1 calc R . . C16 C 0.5586(3) 0.2890(3) 0.56864(19) 0.0555(16) Uani 1 1 d . . . H16 H 0.5754 0.2707 0.5506 0.067 Uiso 1 1 calc R . . C17 C 0.5394(3) 0.3391(3) 0.56004(17) 0.0517(15) Uani 1 1 d . . . H17 H 0.5430 0.3538 0.5360 0.062 Uiso 1 1 calc R . . C18 C 0.5096(3) 0.3449(3) 0.61909(15) 0.0407(12) Uani 1 1 d . . . C19 C 0.6548(3) 0.5456(3) 0.54790(16) 0.0419(13) Uani 1 1 d . . . C20 C 0.7153(3) 0.5656(3) 0.52793(16) 0.0480(14) Uani 1 1 d . . . C21 C 0.7840(3) 0.6096(4) 0.5414(2) 0.0566(16) Uani 1 1 d . . . H21 H 0.8236 0.6226 0.5266 0.068 Uiso 1 1 calc R . . C22 C 0.7932(3) 0.6334(3) 0.5757(2) 0.0566(17) Uani 1 1 d . . . C23 C 0.7338(3) 0.6143(3) 0.59873(18) 0.0490(14) Uani 1 1 d . . . C24 C 0.7381(4) 0.6347(4) 0.63493(19) 0.0596(17) Uani 1 1 d . . . H24 H 0.7827 0.6637 0.6456 0.072 Uiso 1 1 calc R . . C25 C 0.6783(4) 0.6129(4) 0.65451(19) 0.0621(18) Uani 1 1 d . . . H25 H 0.6807 0.6273 0.6785 0.074 Uiso 1 1 calc R . . C26 C 0.6125(4) 0.5681(4) 0.63807(17) 0.0588(17) Uani 1 1 d . . . H26 H 0.5712 0.5520 0.6520 0.071 Uiso 1 1 calc R . . C27 C 0.6657(3) 0.5708(3) 0.58423(16) 0.0430(13) Uani 1 1 d . . . O6 O 0.4342(4) 0.5166(3) 0.67043(18) 0.1022(19) Uiso 1 1 d D . . O7 O 0.3829(15) 0.5975(13) 0.5690(7) 0.061(5) Uiso 0.17 1 d PD . . O7' O 0.4257(14) 0.6258(15) 0.5592(7) 0.061(5) Uiso 0.17 1 d PD . . O8 O 0.6222(19) 0.353(2) 0.7674(9) 0.079(7) Uiso 0.17 1 d P . . O8' O 0.6227(16) 0.3037(19) 0.7711(9) 0.079(7) Uiso 0.17 1 d P . . C28 C 0.3855(16) 0.5098(18) 0.6988(8) 0.160(6) Uiso 0.50 1 d PD . . C28' C 0.3697(13) 0.5013(17) 0.6888(9) 0.160(6) Uiso 0.50 1 d PD . . C29 C 0.4034(18) 0.5774(17) 0.7202(8) 0.160(6) Uiso 0.50 1 d PD . . C29' C 0.3890(18) 0.5790(16) 0.6983(9) 0.160(6) Uiso 0.50 1 d PD . . C30 C 0.3852(16) 0.6522(18) 0.5459(9) 0.133(12) Uiso 0.33 1 d PD . . C31 C 0.3333 0.6667 0.5279(7) 0.167(10) Uiso 1 3 d SD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.04045(17) 0.05173(19) 0.02925(17) -0.00227(11) -0.00157(10) 0.02499(13) Cl1 0.0684(11) 0.0802(11) 0.0468(9) -0.0223(8) -0.0054(8) 0.0379(9) Cl2 0.0479(10) 0.1028(16) 0.1200(19) -0.0349(14) -0.0162(11) 0.0175(10) Cl3 0.0752(10) 0.0532(9) 0.0349(8) 0.0004(6) 0.0067(7) 0.0285(8) Cl4 0.0838(13) 0.0698(11) 0.0914(14) 0.0177(10) -0.0017(11) 0.0510(11) Cl5 0.0565(9) 0.0816(11) 0.0488(9) 0.0060(8) 0.0111(7) 0.0408(9) Cl6 0.0384(9) 0.0882(14) 0.1014(16) -0.0208(11) -0.0104(9) 0.0209(9) O1 0.042(2) 0.058(2) 0.036(2) -0.0053(18) -0.0032(17) 0.0247(19) O2 0.048(2) 0.052(2) 0.035(2) -0.0009(17) -0.0026(17) 0.0299(19) O3 0.040(2) 0.061(2) 0.037(2) -0.0009(18) 0.0002(17) 0.026(2) O4 0.051(3) 0.060(3) 0.032(2) -0.0002(19) 0.0020(18) 0.030(2) O5 0.091(3) 0.080(3) 0.038(2) -0.005(2) 0.000(2) 0.059(3) N1 0.048(3) 0.063(3) 0.032(2) 0.000(2) 0.000(2) 0.028(3) N2 0.040(3) 0.055(3) 0.035(2) -0.006(2) -0.002(2) 0.025(2) N3 0.048(3) 0.059(3) 0.037(3) -0.006(2) -0.004(2) 0.029(2) C1 0.050(3) 0.046(3) 0.036(3) 0.003(2) -0.002(3) 0.028(3) C2 0.054(4) 0.049(3) 0.044(3) -0.008(3) -0.006(3) 0.028(3) C3 0.062(4) 0.053(4) 0.060(4) -0.016(3) -0.015(3) 0.029(3) C4 0.045(4) 0.056(4) 0.075(5) -0.012(4) -0.012(3) 0.016(3) C5 0.045(3) 0.058(4) 0.053(4) 0.004(3) -0.001(3) 0.022(3) C6 0.042(4) 0.089(5) 0.066(5) 0.002(4) 0.003(3) 0.025(4) C7 0.054(4) 0.116(7) 0.053(4) -0.003(4) 0.010(3) 0.037(4) C8 0.060(4) 0.088(5) 0.044(4) -0.005(3) 0.003(3) 0.034(4) C9 0.048(3) 0.052(3) 0.042(3) 0.002(3) -0.002(3) 0.029(3) C10 0.032(3) 0.041(3) 0.040(3) 0.000(2) -0.002(2) 0.015(2) C11 0.043(3) 0.045(3) 0.042(3) 0.004(3) 0.001(3) 0.018(3) C12 0.057(4) 0.048(3) 0.044(3) 0.011(3) 0.002(3) 0.021(3) C13 0.050(4) 0.044(3) 0.063(4) 0.002(3) -0.006(3) 0.025(3) C14 0.037(3) 0.045(3) 0.057(4) -0.008(3) -0.010(3) 0.018(3) C15 0.041(3) 0.046(3) 0.076(5) -0.009(3) -0.004(3) 0.022(3) C16 0.047(3) 0.060(4) 0.065(4) -0.021(3) -0.008(3) 0.031(3) C17 0.049(3) 0.062(4) 0.045(3) -0.011(3) -0.003(3) 0.028(3) C18 0.040(3) 0.042(3) 0.040(3) -0.003(2) -0.004(2) 0.020(3) C19 0.041(3) 0.043(3) 0.048(3) 0.004(3) -0.002(3) 0.026(3) C20 0.046(3) 0.060(4) 0.049(3) 0.007(3) 0.001(3) 0.034(3) C21 0.039(3) 0.057(4) 0.072(5) 0.008(3) 0.006(3) 0.022(3) C22 0.036(3) 0.058(4) 0.075(5) -0.004(3) -0.003(3) 0.023(3) C23 0.041(3) 0.048(3) 0.059(4) -0.004(3) -0.012(3) 0.023(3) C24 0.051(4) 0.059(4) 0.067(4) -0.013(3) -0.018(3) 0.026(3) C25 0.065(4) 0.072(4) 0.049(4) -0.013(3) -0.014(3) 0.034(4) C26 0.055(4) 0.079(5) 0.044(4) -0.009(3) -0.005(3) 0.035(4) C27 0.042(3) 0.043(3) 0.048(3) 0.002(3) 0.003(3) 0.024(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 Dy1 O3 2.312(4) . ? Dy1 O1 2.338(4) . ? Dy1 O2 2.344(4) . ? Dy1 O5 2.366(5) . ? Dy1 O4 2.395(4) . ? Dy1 N2 2.479(5) . ? Dy1 N1 2.525(5) . ? Dy1 N3 2.569(5) . ? Cl1 C2 1.748(6) . ? Cl2 C4 1.752(7) . ? Cl3 C11 1.740(6) . ? Cl4 C13 1.745(6) . ? Cl5 C20 1.746(6) . ? Cl6 C22 1.753(6) . ? O1 C1 1.308(7) . ? O2 C10 1.298(6) . ? O3 C19 1.317(7) . ? O4 H4A 0.83(6) . ? O4 H4B 0.81(5) . ? O5 H5A 0.82(3) . ? O5 H5B 0.82(8) . ? N1 C8 1.313(8) . ? N1 C9 1.362(7) . ? N2 C17 1.323(7) . ? N2 C18 1.363(7) . ? N3 C26 1.316(8) . ? N3 C27 1.368(7) . ? C1 C2 1.387(8) . ? C1 C9 1.431(8) . ? C2 C3 1.390(9) . ? C3 C4 1.368(10) . ? C3 H3 0.9400 . ? C4 C5 1.412(9) . ? C5 C9 1.407(8) . ? C5 C6 1.410(9) . ? C6 C7 1.353(10) . ? C6 H6 0.9400 . ? C7 C8 1.404(10) . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? C10 C11 1.382(8) . ? C10 C18 1.450(8) . ? C11 C12 1.420(8) . ? C12 C13 1.356(9) . ? C12 H12 0.9400 . ? C13 C14 1.430(9) . ? C14 C18 1.408(8) . ? C14 C15 1.409(9) . ? C15 C16 1.346(9) . ? C15 H15 0.9400 . ? C16 C17 1.388(9) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C19 C20 1.378(8) . ? C19 C27 1.432(8) . ? C20 C21 1.405(9) . ? C21 C22 1.353(10) . ? C21 H21 0.9400 . ? C22 C23 1.427(9) . ? C23 C24 1.406(9) . ? C23 C27 1.407(8) . ? C24 C25 1.353(10) . ? C24 H24 0.9400 . ? C25 C26 1.408(9) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? O6 C28' 1.442(18) . ? O6 C28 1.451(18) . ? O7 C30 1.449(18) . ? O7' C30 1.363(18) . ? O8 O8' 1.09(4) . ? O8 O8' 1.12(4) 3_665 ? O8' O8 1.12(4) 2_655 ? O8' O8' 1.47(5) 2_655 ? O8' O8' 1.47(5) 3_665 ? C28 C29 1.540(18) . ? C28' C29' 1.566(19) . ? C30 C31 1.475(16) . ? C31 C30 1.475(17) 2_665 ? C31 C30 1.475(17) 3_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Dy1 O1 78.64(13) . . ? O3 Dy1 O2 131.19(13) . . ? O1 Dy1 O2 124.88(14) . . ? O3 Dy1 O5 122.49(17) . . ? O1 Dy1 O5 134.04(15) . . ? O2 Dy1 O5 74.43(14) . . ? O3 Dy1 O4 81.20(14) . . ? O1 Dy1 O4 76.89(14) . . ? O2 Dy1 O4 140.73(13) . . ? O5 Dy1 O4 68.30(15) . . ? O3 Dy1 N2 81.68(14) . . ? O1 Dy1 N2 76.34(14) . . ? O2 Dy1 N2 66.95(14) . . ? O5 Dy1 N2 140.98(15) . . ? O4 Dy1 N2 150.53(14) . . ? O3 Dy1 N1 143.85(14) . . ? O1 Dy1 N1 65.71(14) . . ? O2 Dy1 N1 77.82(14) . . ? O5 Dy1 N1 81.87(18) . . ? O4 Dy1 N1 85.01(15) . . ? N2 Dy1 N1 95.01(16) . . ? O3 Dy1 N3 65.46(14) . . ? O1 Dy1 N3 142.30(14) . . ? O2 Dy1 N3 76.11(14) . . ? O5 Dy1 N3 78.33(17) . . ? O4 Dy1 N3 107.15(15) . . ? N2 Dy1 N3 87.07(15) . . ? N1 Dy1 N3 150.63(15) . . ? C1 O1 Dy1 123.5(3) . . ? C10 O2 Dy1 121.8(3) . . ? C19 O3 Dy1 125.0(3) . . ? Dy1 O4 H4A 110(5) . . ? Dy1 O4 H4B 122(5) . . ? H4A O4 H4B 96(6) . . ? Dy1 O5 H5A 135(5) . . ? Dy1 O5 H5B 111(5) . . ? H5A O5 H5B 114(7) . . ? C8 N1 C9 117.5(5) . . ? C8 N1 Dy1 125.8(4) . . ? C9 N1 Dy1 116.6(4) . . ? C17 N2 C18 118.6(5) . . ? C17 N2 Dy1 124.6(4) . . ? C18 N2 Dy1 116.7(3) . . ? C26 N3 C27 117.8(5) . . ? C26 N3 Dy1 126.6(4) . . ? C27 N3 Dy1 115.5(4) . . ? O1 C1 C2 125.5(5) . . ? O1 C1 C9 118.9(5) . . ? C2 C1 C9 115.6(5) . . ? C1 C2 C3 123.6(6) . . ? C1 C2 Cl1 119.0(5) . . ? C3 C2 Cl1 117.4(5) . . ? C4 C3 C2 119.7(6) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.8(6) . . ? C3 C4 Cl2 119.2(5) . . ? C5 C4 Cl2 119.9(5) . . ? C9 C5 C6 117.3(6) . . ? C9 C5 C4 118.2(6) . . ? C6 C5 C4 124.4(6) . . ? C7 C6 C5 119.4(6) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 119.3(7) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? N1 C8 C7 123.7(7) . . ? N1 C8 H8 118.2 . . ? C7 C8 H8 118.2 . . ? N1 C9 C5 122.8(6) . . ? N1 C9 C1 115.1(5) . . ? C5 C9 C1 122.1(6) . . ? O2 C10 C11 125.9(5) . . ? O2 C10 C18 119.1(5) . . ? C11 C10 C18 114.9(5) . . ? C10 C11 C12 123.2(5) . . ? C10 C11 Cl3 119.4(4) . . ? C12 C11 Cl3 117.5(4) . . ? C13 C12 C11 120.6(6) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.5(5) . . ? C12 C13 Cl4 119.8(5) . . ? C14 C13 Cl4 119.7(5) . . ? C18 C14 C15 117.3(6) . . ? C18 C14 C13 117.7(5) . . ? C15 C14 C13 125.0(6) . . ? C16 C15 C14 119.9(6) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 119.7(6) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? N2 C17 C16 122.8(6) . . ? N2 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? N2 C18 C14 121.7(5) . . ? N2 C18 C10 115.1(5) . . ? C14 C18 C10 123.1(5) . . ? O3 C19 C20 125.4(5) . . ? O3 C19 C27 118.6(5) . . ? C20 C19 C27 116.0(5) . . ? C19 C20 C21 123.1(6) . . ? C19 C20 Cl5 119.0(5) . . ? C21 C20 Cl5 117.8(5) . . ? C22 C21 C20 120.0(6) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 121.0(6) . . ? C21 C22 Cl6 119.7(5) . . ? C23 C22 Cl6 119.3(6) . . ? C24 C23 C27 117.4(6) . . ? C24 C23 C22 125.1(6) . . ? C27 C23 C22 117.5(6) . . ? C25 C24 C23 120.2(6) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 118.5(6) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? N3 C26 C25 123.7(6) . . ? N3 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? N3 C27 C23 122.2(5) . . ? N3 C27 C19 115.3(5) . . ? C23 C27 C19 122.4(5) . . ? O8' O8 O8' 83(4) . 3_665 ? O8 O8' O8 152(5) . 2_655 ? O8 O8' O8' 109(3) . 2_655 ? O8 O8' O8' 48(3) 2_655 2_655 ? O8 O8' O8' 50(3) . 3_665 ? O8 O8' O8' 107(3) 2_655 3_665 ? O8' O8' O8' 60.00(2) 2_655 3_665 ? O6 C28 C29 117(2) . . ? O6 C28' C29' 99(2) . . ? O7' C30 C31 168(3) . . ? O7 C30 C31 137(3) . . ? C30 C31 C30 101(2) 2_665 3_565 ? C30 C31 C30 101(2) 2_665 . ? C30 C31 C30 101(2) 3_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Dy1 O1 C1 -171.3(4) . . . . ? O2 Dy1 O1 C1 56.0(4) . . . . ? O5 Dy1 O1 C1 -46.7(5) . . . . ? O4 Dy1 O1 C1 -87.8(4) . . . . ? N2 Dy1 O1 C1 104.6(4) . . . . ? N1 Dy1 O1 C1 2.6(4) . . . . ? N3 Dy1 O1 C1 171.0(4) . . . . ? O3 Dy1 O2 C10 -49.5(4) . . . . ? O1 Dy1 O2 C10 57.4(4) . . . . ? O5 Dy1 O2 C10 -169.3(4) . . . . ? O4 Dy1 O2 C10 172.0(3) . . . . ? N2 Dy1 O2 C10 5.0(4) . . . . ? N1 Dy1 O2 C10 105.8(4) . . . . ? N3 Dy1 O2 C10 -87.8(4) . . . . ? O1 Dy1 O3 C19 -165.2(4) . . . . ? O2 Dy1 O3 C19 -38.4(5) . . . . ? O5 Dy1 O3 C19 59.4(4) . . . . ? O4 Dy1 O3 C19 116.5(4) . . . . ? N2 Dy1 O3 C19 -87.5(4) . . . . ? N1 Dy1 O3 C19 -174.6(4) . . . . ? N3 Dy1 O3 C19 3.0(4) . . . . ? O3 Dy1 N1 C8 -169.3(5) . . . . ? O1 Dy1 N1 C8 -179.5(6) . . . . ? O2 Dy1 N1 C8 42.9(5) . . . . ? O5 Dy1 N1 C8 -32.9(5) . . . . ? O4 Dy1 N1 C8 -101.6(6) . . . . ? N2 Dy1 N1 C8 108.0(6) . . . . ? N3 Dy1 N1 C8 15.0(7) . . . . ? O3 Dy1 N1 C9 7.1(5) . . . . ? O1 Dy1 N1 C9 -3.1(4) . . . . ? O2 Dy1 N1 C9 -140.8(4) . . . . ? O5 Dy1 N1 C9 143.5(4) . . . . ? O4 Dy1 N1 C9 74.7(4) . . . . ? N2 Dy1 N1 C9 -75.7(4) . . . . ? N3 Dy1 N1 C9 -168.6(4) . . . . ? O3 Dy1 N2 C17 -39.3(4) . . . . ? O1 Dy1 N2 C17 41.0(4) . . . . ? O2 Dy1 N2 C17 178.9(5) . . . . ? O5 Dy1 N2 C17 -172.3(4) . . . . ? O4 Dy1 N2 C17 15.7(6) . . . . ? N1 Dy1 N2 C17 104.4(5) . . . . ? N3 Dy1 N2 C17 -104.9(5) . . . . ? O3 Dy1 N2 C18 137.6(4) . . . . ? O1 Dy1 N2 C18 -142.1(4) . . . . ? O2 Dy1 N2 C18 -4.2(4) . . . . ? O5 Dy1 N2 C18 4.6(5) . . . . ? O4 Dy1 N2 C18 -167.4(3) . . . . ? N1 Dy1 N2 C18 -78.6(4) . . . . ? N3 Dy1 N2 C18 72.0(4) . . . . ? O3 Dy1 N3 C26 -179.6(6) . . . . ? O1 Dy1 N3 C26 -160.5(5) . . . . ? O2 Dy1 N3 C26 -30.5(5) . . . . ? O5 Dy1 N3 C26 46.2(5) . . . . ? O4 Dy1 N3 C26 108.9(5) . . . . ? N2 Dy1 N3 C26 -97.4(5) . . . . ? N1 Dy1 N3 C26 -2.4(7) . . . . ? O3 Dy1 N3 C27 -2.0(4) . . . . ? O1 Dy1 N3 C27 17.1(5) . . . . ? O2 Dy1 N3 C27 147.2(4) . . . . ? O5 Dy1 N3 C27 -136.2(4) . . . . ? O4 Dy1 N3 C27 -73.5(4) . . . . ? N2 Dy1 N3 C27 80.2(4) . . . . ? N1 Dy1 N3 C27 175.2(4) . . . . ? Dy1 O1 C1 C2 176.1(4) . . . . ? Dy1 O1 C1 C9 -1.9(7) . . . . ? O1 C1 C2 C3 -178.0(6) . . . . ? C9 C1 C2 C3 0.0(9) . . . . ? O1 C1 C2 Cl1 1.3(8) . . . . ? C9 C1 C2 Cl1 179.4(4) . . . . ? C1 C2 C3 C4 -0.5(10) . . . . ? Cl1 C2 C3 C4 -179.8(5) . . . . ? C2 C3 C4 C5 -0.2(11) . . . . ? C2 C3 C4 Cl2 178.3(5) . . . . ? C3 C4 C5 C9 1.2(10) . . . . ? Cl2 C4 C5 C9 -177.3(5) . . . . ? C3 C4 C5 C6 179.9(7) . . . . ? Cl2 C4 C5 C6 1.5(10) . . . . ? C9 C5 C6 C7 0.2(11) . . . . ? C4 C5 C6 C7 -178.5(8) . . . . ? C5 C6 C7 C8 -0.2(13) . . . . ? C9 N1 C8 C7 0.5(11) . . . . ? Dy1 N1 C8 C7 176.8(6) . . . . ? C6 C7 C8 N1 -0.1(13) . . . . ? C8 N1 C9 C5 -0.4(9) . . . . ? Dy1 N1 C9 C5 -177.1(5) . . . . ? C8 N1 C9 C1 -179.9(6) . . . . ? Dy1 N1 C9 C1 3.5(6) . . . . ? C6 C5 C9 N1 0.1(9) . . . . ? C4 C5 C9 N1 178.9(6) . . . . ? C6 C5 C9 C1 179.5(6) . . . . ? C4 C5 C9 C1 -1.7(9) . . . . ? O1 C1 C9 N1 -1.3(8) . . . . ? C2 C1 C9 N1 -179.5(5) . . . . ? O1 C1 C9 C5 179.2(5) . . . . ? C2 C1 C9 C5 1.1(8) . . . . ? Dy1 O2 C10 C11 174.5(4) . . . . ? Dy1 O2 C10 C18 -5.3(6) . . . . ? O2 C10 C11 C12 180.0(5) . . . . ? C18 C10 C11 C12 -0.2(8) . . . . ? O2 C10 C11 Cl3 -0.6(8) . . . . ? C18 C10 C11 Cl3 179.3(4) . . . . ? C10 C11 C12 C13 0.0(9) . . . . ? Cl3 C11 C12 C13 -179.4(5) . . . . ? C11 C12 C13 C14 0.1(9) . . . . ? C11 C12 C13 Cl4 178.4(5) . . . . ? C12 C13 C14 C18 0.0(9) . . . . ? Cl4 C13 C14 C18 -178.3(4) . . . . ? C12 C13 C14 C15 179.5(6) . . . . ? Cl4 C13 C14 C15 1.2(8) . . . . ? C18 C14 C15 C16 0.1(8) . . . . ? C13 C14 C15 C16 -179.4(6) . . . . ? C14 C15 C16 C17 -0.2(9) . . . . ? C18 N2 C17 C16 -1.3(9) . . . . ? Dy1 N2 C17 C16 175.5(4) . . . . ? C15 C16 C17 N2 0.8(10) . . . . ? C17 N2 C18 C14 1.3(8) . . . . ? Dy1 N2 C18 C14 -175.8(4) . . . . ? C17 N2 C18 C10 -179.6(5) . . . . ? Dy1 N2 C18 C10 3.3(6) . . . . ? C15 C14 C18 N2 -0.7(8) . . . . ? C13 C14 C18 N2 178.9(5) . . . . ? C15 C14 C18 C10 -179.7(5) . . . . ? C13 C14 C18 C10 -0.2(8) . . . . ? O2 C10 C18 N2 1.0(7) . . . . ? C11 C10 C18 N2 -178.8(5) . . . . ? O2 C10 C18 C14 -179.9(5) . . . . ? C11 C10 C18 C14 0.2(8) . . . . ? Dy1 O3 C19 C20 174.2(4) . . . . ? Dy1 O3 C19 C27 -3.7(7) . . . . ? O3 C19 C20 C21 -179.7(6) . . . . ? C27 C19 C20 C21 -1.8(9) . . . . ? O3 C19 C20 Cl5 -3.5(8) . . . . ? C27 C19 C20 Cl5 174.4(4) . . . . ? C19 C20 C21 C22 1.3(10) . . . . ? Cl5 C20 C21 C22 -175.0(5) . . . . ? C20 C21 C22 C23 0.2(10) . . . . ? C20 C21 C22 Cl6 179.5(5) . . . . ? C21 C22 C23 C24 178.2(6) . . . . ? Cl6 C22 C23 C24 -1.2(9) . . . . ? C21 C22 C23 C27 -0.9(9) . . . . ? Cl6 C22 C23 C27 179.8(4) . . . . ? C27 C23 C24 C25 -0.2(10) . . . . ? C22 C23 C24 C25 -179.2(6) . . . . ? C23 C24 C25 C26 1.6(11) . . . . ? C27 N3 C26 C25 0.3(10) . . . . ? Dy1 N3 C26 C25 177.9(5) . . . . ? C24 C25 C26 N3 -1.8(11) . . . . ? C26 N3 C27 C23 1.2(9) . . . . ? Dy1 N3 C27 C23 -176.6(4) . . . . ? C26 N3 C27 C19 178.9(5) . . . . ? Dy1 N3 C27 C19 1.1(6) . . . . ? C24 C23 C27 N3 -1.3(9) . . . . ? C22 C23 C27 N3 177.8(5) . . . . ? C24 C23 C27 C19 -178.8(5) . . . . ? C22 C23 C27 C19 0.3(9) . . . . ? O3 C19 C27 N3 1.4(7) . . . . ? C20 C19 C27 N3 -176.7(5) . . . . ? O3 C19 C27 C23 179.1(5) . . . . ? C20 C19 C27 C23 1.0(8) . . . . ? O8' O8 O8' O8 -38(12) 3_665 . . 2_655 ? O8' O8 O8' O8' -9(3) 3_665 . . 2_655 ? C28' O6 C28 C29 -123(9) . . . . ? C28 O6 C28' C29' 68(7) . . . . ? O7' C30 C31 C30 169(16) . . . 2_665 ? O7 C30 C31 C30 116(3) . . . 2_665 ? O7' C30 C31 C30 65(19) . . . 3_565 ? O7 C30 C31 C30 13(6) . . . 3_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.934 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.102 #========================================================================== data_Er _database_code_depnum_ccdc_archive 'CCDC 794956' #TrackingRef 'Er.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H16 Cl6 Er N3 O5, C2 H6 O, 1/3(C2 H6 O), 1/3(H2 O)' _chemical_formula_sum 'C29.67 H24.67 Cl6 Er N3 O6.67' _chemical_formula_weight 909.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3:H' _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 21.7263(14) _cell_length_b 21.7263(14) _cell_length_c 37.099(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 15165.9(17) _cell_formula_units_Z 18 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9051 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8046 _exptl_absorpt_coefficient_mu 3.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.333 _exptl_absorpt_correction_T_max 0.502 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12475 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6233 _reflns_number_gt 5016 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6233 _refine_ls_number_parameters 428 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1322 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.462450(18) 0.488647(17) 0.428169(7) 0.04292(14) Uani 1 1 d . . . Cl1 Cl 0.30574(13) 0.40357(13) 0.54781(5) 0.0727(6) Uani 1 1 d . . . Cl2 Cl 0.20119(18) 0.13760(14) 0.50008(9) 0.1095(10) Uani 1 1 d . . . Cl3 Cl 0.53056(13) 0.70632(11) 0.51518(5) 0.0647(6) Uani 1 1 d . . . Cl4 Cl 0.68667(15) 0.87808(12) 0.40736(8) 0.0882(8) Uani 1 1 d . . . Cl5 Cl 0.39282(11) 0.44792(12) 0.28857(4) 0.0622(5) Uani 1 1 d . . . Cl6 Cl 0.21506(14) 0.54504(15) 0.31827(7) 0.0839(7) Uani 1 1 d . . . O1 O 0.3889(3) 0.4447(3) 0.47833(11) 0.0481(12) Uani 1 1 d . . . O2 O 0.5037(3) 0.5879(3) 0.46345(11) 0.0489(12) Uani 1 1 d . . . O3 O 0.4246(3) 0.4668(3) 0.36832(11) 0.0468(12) Uani 1 1 d . . . O4 O 0.5317(3) 0.4662(3) 0.46935(11) 0.0500(12) Uani 1 1 d D . . H4A H 0.555(4) 0.500(3) 0.4830(17) 0.060 Uiso 1 1 d D . . H4B H 0.520(4) 0.436(3) 0.4852(15) 0.060 Uiso 1 1 d D . . O5 O 0.5401(4) 0.4592(4) 0.39859(12) 0.0658(16) Uani 1 1 d D . . H5A H 0.538(5) 0.456(5) 0.3766(4) 0.079 Uiso 1 1 d D . . H5B H 0.546(5) 0.435(4) 0.4139(17) 0.079 Uiso 1 1 d D . . N1 N 0.3835(3) 0.3569(3) 0.42753(14) 0.0521(16) Uani 1 1 d . . . N2 N 0.5470(3) 0.6045(3) 0.39582(14) 0.0473(14) Uani 1 1 d . . . N3 N 0.3685(3) 0.5173(3) 0.41619(13) 0.0468(14) Uani 1 1 d . . . C1 C 0.3449(4) 0.3761(4) 0.48342(16) 0.0429(16) Uani 1 1 d . . . C2 C 0.3028(4) 0.3475(4) 0.51332(18) 0.0523(18) Uani 1 1 d . . . C3 C 0.2593(4) 0.2748(5) 0.5186(2) 0.061(2) Uani 1 1 d . . . H3 H 0.2332 0.2578 0.5401 0.074 Uiso 1 1 calc R . . C4 C 0.2546(5) 0.2289(4) 0.4932(2) 0.068(2) Uani 1 1 d . . . C5 C 0.2964(5) 0.2541(4) 0.4611(2) 0.059(2) Uani 1 1 d . . . C6 C 0.2947(5) 0.2096(5) 0.4331(2) 0.072(3) Uani 1 1 d . . . H6 H 0.2645 0.1601 0.4346 0.086 Uiso 1 1 calc R . . C7 C 0.3374(5) 0.2392(5) 0.4037(2) 0.075(3) Uani 1 1 d . . . H7 H 0.3373 0.2105 0.3847 0.090 Uiso 1 1 calc R . . C8 C 0.3819(5) 0.3142(5) 0.4026(2) 0.071(2) Uani 1 1 d . . . H8 H 0.4121 0.3342 0.3826 0.086 Uiso 1 1 calc R . . C9 C 0.3413(4) 0.3267(4) 0.45680(17) 0.0451(17) Uani 1 1 d . . . C10 C 0.5442(4) 0.6536(4) 0.45210(18) 0.0483(17) Uani 1 1 d . . . C11 C 0.5654(4) 0.7153(4) 0.47219(18) 0.0516(18) Uani 1 1 d . . . C12 C 0.6091(4) 0.7832(4) 0.4588(2) 0.0563(19) Uani 1 1 d . . . H12 H 0.6221 0.8230 0.4736 0.068 Uiso 1 1 calc R . . C13 C 0.6333(4) 0.7921(4) 0.4242(2) 0.060(2) Uani 1 1 d . . . C14 C 0.6140(4) 0.7331(4) 0.40136(19) 0.0529(18) Uani 1 1 d . . . C15 C 0.6339(5) 0.7372(5) 0.3645(2) 0.065(2) Uani 1 1 d . . . H15 H 0.6622 0.7817 0.3536 0.079 Uiso 1 1 calc R . . C16 C 0.6126(5) 0.6781(5) 0.3456(2) 0.067(2) Uani 1 1 d . . . H16 H 0.6270 0.6807 0.3214 0.081 Uiso 1 1 calc R . . C17 C 0.5689(5) 0.6124(5) 0.36148(19) 0.063(2) Uani 1 1 d . . . H17 H 0.5538 0.5713 0.3474 0.075 Uiso 1 1 calc R . . C18 C 0.5707(4) 0.6655(4) 0.41553(18) 0.0466(17) Uani 1 1 d . . . C19 C 0.3776(4) 0.4830(4) 0.35652(16) 0.0413(15) Uani 1 1 d . . . C20 C 0.3560(4) 0.4775(4) 0.32074(18) 0.0488(17) Uani 1 1 d . . . C21 C 0.3059(4) 0.4961(4) 0.3094(2) 0.057(2) Uani 1 1 d . . . H21 H 0.2930 0.4914 0.2850 0.068 Uiso 1 1 calc R . . C22 C 0.2757(4) 0.5205(4) 0.3329(2) 0.060(2) Uani 1 1 d . . . C23 C 0.2949(4) 0.5279(4) 0.37091(19) 0.0528(18) Uani 1 1 d . . . C24 C 0.2672(4) 0.5535(4) 0.3976(2) 0.060(2) Uani 1 1 d . . . H24 H 0.2333 0.5666 0.3915 0.073 Uiso 1 1 calc R . . C25 C 0.2895(4) 0.5589(4) 0.4318(2) 0.058(2) Uani 1 1 d . . . H25 H 0.2709 0.5751 0.4500 0.069 Uiso 1 1 calc R . . C26 C 0.3403(4) 0.5403(4) 0.43984(19) 0.056(2) Uani 1 1 d . . . H26 H 0.3555 0.5446 0.4639 0.067 Uiso 1 1 calc R . . C27 C 0.3448(4) 0.5094(4) 0.38110(17) 0.0432(16) Uani 1 1 d . . . O6 O 0.5163(4) 0.4333(4) 0.32984(19) 0.097(2) Uiso 1 1 d D . . O7 O 0.3823(19) 0.7861(17) 0.5710(8) 0.063(6) Uiso 0.17 1 d PD . . O7' O 0.4202(17) 0.7970(15) 0.5564(9) 0.063(6) Uiso 0.17 1 d PD . . O8 O 0.358(3) 0.626(3) 0.2338(13) 0.107(11) Uiso 0.17 1 d P . . O8' O 0.310(4) 0.628(2) 0.2323(12) 0.107(11) Uiso 0.17 1 d P . . C28 C 0.512(2) 0.3850(18) 0.3013(9) 0.167(7) Uiso 0.50 1 d PD A 1 C28' C 0.4968(19) 0.3665(14) 0.3130(10) 0.167(7) Uiso 0.50 1 d PD A 2 C29 C 0.578(2) 0.400(2) 0.2804(10) 0.167(7) Uiso 0.50 1 d PD A 1 C29' C 0.5739(19) 0.386(2) 0.3032(10) 0.167(7) Uiso 0.50 1 d PD A 2 C30 C 0.377(3) 0.7235(15) 0.5539(11) 0.184(12) Uiso 0.33 1 d PD . . C31 C 0.3333 0.6667 0.5280(9) 0.184(12) Uiso 1 3 d SD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0563(2) 0.0443(2) 0.03080(18) 0.00117(12) 0.00198(13) 0.02713(17) Cl1 0.0876(16) 0.0767(15) 0.0551(11) 0.0051(10) 0.0233(11) 0.0423(13) Cl2 0.113(2) 0.0541(15) 0.133(2) 0.0166(15) 0.0406(19) 0.0211(15) Cl3 0.0883(16) 0.0628(13) 0.0513(9) -0.0109(9) -0.0052(10) 0.0439(12) Cl4 0.0966(19) 0.0448(12) 0.1070(19) 0.0111(12) 0.0215(15) 0.0232(12) Cl5 0.0601(12) 0.0834(15) 0.0383(8) -0.0074(9) -0.0005(8) 0.0323(11) Cl6 0.0773(16) 0.0949(18) 0.0966(16) 0.0026(14) -0.0212(14) 0.0559(15) O1 0.061(3) 0.046(3) 0.036(2) 0.006(2) 0.009(2) 0.026(3) O2 0.064(3) 0.041(3) 0.041(2) -0.003(2) -0.002(2) 0.026(3) O3 0.054(3) 0.055(3) 0.035(2) -0.001(2) 0.001(2) 0.030(3) O4 0.071(4) 0.049(3) 0.036(2) 0.002(2) 0.001(2) 0.034(3) O5 0.087(4) 0.092(5) 0.038(3) -0.001(3) 0.005(3) 0.059(4) N1 0.068(4) 0.056(4) 0.036(3) -0.006(3) 0.000(3) 0.033(3) N2 0.058(4) 0.044(3) 0.042(3) 0.003(3) 0.004(3) 0.027(3) N3 0.054(4) 0.053(4) 0.036(3) -0.002(3) 0.003(3) 0.029(3) C1 0.046(4) 0.052(4) 0.034(3) 0.004(3) -0.005(3) 0.028(4) C2 0.050(4) 0.060(5) 0.050(4) 0.005(4) 0.007(3) 0.029(4) C3 0.055(5) 0.068(6) 0.060(4) 0.014(4) 0.014(4) 0.029(5) C4 0.055(5) 0.051(5) 0.086(6) 0.018(5) 0.014(5) 0.017(4) C5 0.069(5) 0.047(5) 0.055(4) 0.002(4) -0.002(4) 0.025(4) C6 0.091(7) 0.046(5) 0.065(5) 0.002(4) 0.005(5) 0.024(5) C7 0.097(7) 0.052(5) 0.067(5) -0.007(4) 0.000(5) 0.030(5) C8 0.098(7) 0.061(6) 0.054(4) 0.002(4) 0.006(5) 0.039(5) C9 0.051(4) 0.048(4) 0.041(3) 0.006(3) -0.002(3) 0.028(4) C10 0.049(4) 0.052(5) 0.050(4) -0.001(3) -0.009(3) 0.029(4) C11 0.064(5) 0.056(5) 0.046(4) -0.005(3) -0.008(4) 0.038(4) C12 0.068(5) 0.038(4) 0.065(5) -0.009(4) -0.007(4) 0.028(4) C13 0.056(5) 0.045(5) 0.079(6) 0.003(4) 0.001(4) 0.025(4) C14 0.054(5) 0.050(5) 0.059(4) 0.007(4) 0.002(4) 0.029(4) C15 0.073(6) 0.056(5) 0.067(5) 0.018(4) 0.018(4) 0.031(5) C16 0.077(6) 0.070(6) 0.052(4) 0.017(4) 0.017(4) 0.034(5) C17 0.079(6) 0.065(5) 0.049(4) 0.000(4) 0.006(4) 0.040(5) C18 0.049(4) 0.042(4) 0.050(4) 0.002(3) -0.004(3) 0.024(4) C19 0.040(4) 0.039(4) 0.039(3) 0.004(3) 0.005(3) 0.015(3) C20 0.044(4) 0.047(4) 0.044(4) 0.001(3) -0.004(3) 0.015(4) C21 0.051(5) 0.066(5) 0.050(4) -0.001(4) -0.013(4) 0.027(4) C22 0.044(4) 0.058(5) 0.076(5) 0.000(4) -0.007(4) 0.024(4) C23 0.054(5) 0.046(4) 0.054(4) 0.005(4) 0.010(4) 0.022(4) C24 0.051(5) 0.046(4) 0.082(6) 0.008(4) 0.010(4) 0.023(4) C25 0.057(5) 0.053(5) 0.064(5) 0.003(4) 0.016(4) 0.029(4) C26 0.069(5) 0.052(5) 0.050(4) 0.005(4) 0.018(4) 0.033(4) C27 0.041(4) 0.043(4) 0.045(3) 0.010(3) 0.005(3) 0.021(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 Er1 O2 2.288(4) . ? Er1 O1 2.325(4) . ? Er1 O3 2.333(4) . ? Er1 O5 2.354(6) . ? Er1 O4 2.360(5) . ? Er1 N3 2.453(6) . ? Er1 N1 2.496(6) . ? Er1 N2 2.555(6) . ? Cl1 C2 1.746(8) . ? Cl2 C4 1.745(9) . ? Cl3 C11 1.734(7) . ? Cl4 C13 1.748(8) . ? Cl5 C20 1.730(7) . ? Cl6 C22 1.738(8) . ? O1 C1 1.321(8) . ? O2 C10 1.317(8) . ? O3 C19 1.309(8) . ? O4 H4A 0.83(6) . ? O4 H4B 0.82(6) . ? O5 H5A 0.817(10) . ? O5 H5B 0.83(9) . ? N1 C8 1.298(10) . ? N1 C9 1.359(9) . ? N2 C17 1.340(9) . ? N2 C18 1.368(9) . ? N3 C26 1.306(9) . ? N3 C27 1.379(8) . ? C1 C2 1.374(9) . ? C1 C9 1.431(10) . ? C2 C3 1.390(11) . ? C3 C4 1.339(12) . ? C3 H3 0.9400 . ? C4 C5 1.430(11) . ? C5 C9 1.389(10) . ? C5 C6 1.408(11) . ? C6 C7 1.365(12) . ? C6 H6 0.9400 . ? C7 C8 1.421(12) . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? C10 C11 1.396(10) . ? C10 C18 1.446(9) . ? C11 C12 1.385(11) . ? C12 C13 1.367(12) . ? C12 H12 0.9400 . ? C13 C14 1.414(11) . ? C14 C18 1.391(10) . ? C14 C15 1.423(10) . ? C15 C16 1.328(12) . ? C15 H15 0.9400 . ? C16 C17 1.390(11) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C19 C20 1.394(9) . ? C19 C27 1.442(9) . ? C20 C21 1.401(10) . ? C21 C22 1.349(11) . ? C21 H21 0.9400 . ? C22 C23 1.454(10) . ? C23 C27 1.385(10) . ? C23 C24 1.409(10) . ? C24 C25 1.342(10) . ? C24 H24 0.9400 . ? C25 C26 1.384(11) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? O6 C28' 1.437(18) . ? O6 C28 1.457(18) . ? O7 O7' 0.91(4) . ? O7 C30 1.447(19) . ? O7' C30 1.393(19) . ? O8 O8' 1.07(7) . ? O8 O8' 1.09(7) 2_665 ? O8' O8 1.09(7) 3_565 ? O8' O8' 1.28(7) 2_665 ? O8' O8' 1.28(7) 3_565 ? C28 C29 1.533(19) . ? C28' C29' 1.553(19) . ? C30 C31 1.473(18) . ? C30 C30 1.93(6) 2_665 ? C30 C30 1.93(6) 3_565 ? C31 C30 1.473(18) 2_665 ? C31 C30 1.473(18) 3_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Er1 O1 78.10(16) . . ? O2 Er1 O3 131.95(16) . . ? O1 Er1 O3 125.32(17) . . ? O2 Er1 O5 121.8(2) . . ? O1 Er1 O5 134.50(19) . . ? O3 Er1 O5 74.26(17) . . ? O2 Er1 O4 80.47(17) . . ? O1 Er1 O4 77.04(17) . . ? O3 Er1 O4 140.42(16) . . ? O5 Er1 O4 68.16(17) . . ? O2 Er1 N3 81.26(18) . . ? O1 Er1 N3 76.14(17) . . ? O3 Er1 N3 68.02(17) . . ? O5 Er1 N3 141.69(17) . . ? O4 Er1 N3 150.09(17) . . ? O2 Er1 N1 143.83(17) . . ? O1 Er1 N1 66.39(17) . . ? O3 Er1 N1 77.72(17) . . ? O5 Er1 N1 81.9(2) . . ? O4 Er1 N1 85.01(19) . . ? N3 Er1 N1 96.2(2) . . ? O2 Er1 N2 65.80(17) . . ? O1 Er1 N2 142.04(17) . . ? O3 Er1 N2 76.12(17) . . ? O5 Er1 N2 77.8(2) . . ? O4 Er1 N2 106.80(19) . . ? N3 Er1 N2 86.80(19) . . ? N1 Er1 N2 150.36(17) . . ? C1 O1 Er1 122.6(4) . . ? C10 O2 Er1 125.0(4) . . ? C19 O3 Er1 120.4(4) . . ? Er1 O4 H4A 114(6) . . ? Er1 O4 H4B 130(6) . . ? H4A O4 H4B 94(7) . . ? Er1 O5 H5A 117(7) . . ? Er1 O5 H5B 102(6) . . ? H5A O5 H5B 132(9) . . ? C8 N1 C9 117.1(7) . . ? C8 N1 Er1 125.7(6) . . ? C9 N1 Er1 117.1(4) . . ? C17 N2 C18 116.6(6) . . ? C17 N2 Er1 127.3(5) . . ? C18 N2 Er1 116.1(4) . . ? C26 N3 C27 117.6(6) . . ? C26 N3 Er1 125.8(5) . . ? C27 N3 Er1 116.5(4) . . ? O1 C1 C2 124.7(6) . . ? O1 C1 C9 119.0(6) . . ? C2 C1 C9 116.3(7) . . ? C1 C2 C3 123.3(7) . . ? C1 C2 Cl1 119.4(6) . . ? C3 C2 Cl1 117.2(6) . . ? C4 C3 C2 120.1(7) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.2(8) . . ? C3 C4 Cl2 120.2(7) . . ? C5 C4 Cl2 119.4(7) . . ? C9 C5 C6 117.3(7) . . ? C9 C5 C4 118.8(7) . . ? C6 C5 C4 123.9(8) . . ? C7 C6 C5 119.2(8) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 118.5(8) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? N1 C8 C7 123.9(8) . . ? N1 C8 H8 118.1 . . ? C7 C8 H8 118.1 . . ? N1 C9 C5 124.1(7) . . ? N1 C9 C1 114.8(6) . . ? C5 C9 C1 121.1(7) . . ? O2 C10 C11 126.3(6) . . ? O2 C10 C18 119.0(6) . . ? C11 C10 C18 114.8(7) . . ? C12 C11 C10 123.6(7) . . ? C12 C11 Cl3 118.5(6) . . ? C10 C11 Cl3 117.8(6) . . ? C13 C12 C11 119.9(7) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 121.0(7) . . ? C12 C13 Cl4 119.4(6) . . ? C14 C13 Cl4 119.6(7) . . ? C18 C14 C13 118.0(7) . . ? C18 C14 C15 116.9(7) . . ? C13 C14 C15 125.1(7) . . ? C16 C15 C14 120.0(8) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 119.8(7) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? N2 C17 C16 123.4(8) . . ? N2 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? N2 C18 C14 123.2(6) . . ? N2 C18 C10 113.9(6) . . ? C14 C18 C10 122.8(7) . . ? O3 C19 C20 124.8(6) . . ? O3 C19 C27 120.2(6) . . ? C20 C19 C27 115.0(6) . . ? C19 C20 C21 122.6(7) . . ? C19 C20 Cl5 119.3(6) . . ? C21 C20 Cl5 118.1(5) . . ? C22 C21 C20 121.3(7) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 120.1(7) . . ? C21 C22 Cl6 120.7(6) . . ? C23 C22 Cl6 119.2(6) . . ? C27 C23 C24 118.2(7) . . ? C27 C23 C22 117.0(7) . . ? C24 C23 C22 124.8(8) . . ? C25 C24 C23 119.6(8) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 118.9(7) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? N3 C26 C25 124.3(7) . . ? N3 C26 H26 117.8 . . ? C25 C26 H26 117.8 . . ? N3 C27 C23 121.4(6) . . ? N3 C27 C19 114.7(6) . . ? C23 C27 C19 123.9(6) . . ? O7' O7 C30 68.1(17) . . ? O7 O7' C30 74.5(19) . . ? O8' O8 O8' 73(6) . 2_665 ? O8 O8' O8 166(7) . 3_565 ? O8 O8' O8' 54(5) . 2_665 ? O8 O8' O8' 113(5) 3_565 2_665 ? O8 O8' O8' 114(5) . 3_565 ? O8 O8' O8' 53(5) 3_565 3_565 ? O8' O8' O8' 60.000(11) 2_665 3_565 ? O6 C28 C29 120(3) . . ? O6 C28' C29' 96(2) . . ? O7' C30 C31 142(4) . . ? O7 C30 C31 142(4) . . ? O7' C30 C30 139(5) . 2_665 ? O7 C30 C30 106(5) . 2_665 ? C31 C30 C30 49.0(14) . 2_665 ? O7' C30 C30 160(5) . 3_565 ? O7 C30 C30 152(3) . 3_565 ? C31 C30 C30 49.0(14) . 3_565 ? C30 C30 C30 60.000(6) 2_665 3_565 ? C30 C31 C30 82(3) 2_665 . ? C30 C31 C30 82(3) 2_665 3_565 ? C30 C31 C30 82(3) . 3_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Er1 O1 C1 -170.8(5) . . . . ? O3 Er1 O1 C1 55.8(5) . . . . ? O5 Er1 O1 C1 -47.5(6) . . . . ? O4 Er1 O1 C1 -88.0(5) . . . . ? N3 Er1 O1 C1 105.4(5) . . . . ? N1 Er1 O1 C1 2.2(5) . . . . ? N2 Er1 O1 C1 171.2(4) . . . . ? O1 Er1 O2 C10 -163.6(6) . . . . ? O3 Er1 O2 C10 -36.3(6) . . . . ? O5 Er1 O2 C10 61.0(6) . . . . ? O4 Er1 O2 C10 117.8(6) . . . . ? N3 Er1 O2 C10 -86.0(5) . . . . ? N1 Er1 O2 C10 -174.5(5) . . . . ? N2 Er1 O2 C10 4.4(5) . . . . ? O2 Er1 O3 C19 -50.3(6) . . . . ? O1 Er1 O3 C19 57.0(5) . . . . ? O5 Er1 O3 C19 -169.2(5) . . . . ? O4 Er1 O3 C19 172.2(4) . . . . ? N3 Er1 O3 C19 4.0(5) . . . . ? N1 Er1 O3 C19 105.9(5) . . . . ? N2 Er1 O3 C19 -88.1(5) . . . . ? O2 Er1 N1 C8 -167.5(6) . . . . ? O1 Er1 N1 C8 -179.2(8) . . . . ? O3 Er1 N1 C8 43.0(7) . . . . ? O5 Er1 N1 C8 -32.6(7) . . . . ? O4 Er1 N1 C8 -101.2(7) . . . . ? N3 Er1 N1 C8 108.9(7) . . . . ? N2 Er1 N1 C8 14.5(9) . . . . ? O2 Er1 N1 C9 8.6(7) . . . . ? O1 Er1 N1 C9 -3.1(5) . . . . ? O3 Er1 N1 C9 -140.9(5) . . . . ? O5 Er1 N1 C9 143.5(5) . . . . ? O4 Er1 N1 C9 74.9(5) . . . . ? N3 Er1 N1 C9 -75.1(5) . . . . ? N2 Er1 N1 C9 -169.4(4) . . . . ? O2 Er1 N2 C17 179.7(7) . . . . ? O1 Er1 N2 C17 -160.9(6) . . . . ? O3 Er1 N2 C17 -30.3(6) . . . . ? O5 Er1 N2 C17 46.3(6) . . . . ? O4 Er1 N2 C17 108.7(6) . . . . ? N3 Er1 N2 C17 -98.4(7) . . . . ? N1 Er1 N2 C17 -1.6(9) . . . . ? O2 Er1 N2 C18 -2.5(5) . . . . ? O1 Er1 N2 C18 16.8(7) . . . . ? O3 Er1 N2 C18 147.5(5) . . . . ? O5 Er1 N2 C18 -136.0(5) . . . . ? O4 Er1 N2 C18 -73.6(5) . . . . ? N3 Er1 N2 C18 79.3(5) . . . . ? N1 Er1 N2 C18 176.2(5) . . . . ? O2 Er1 N3 C26 -39.4(6) . . . . ? O1 Er1 N3 C26 40.4(6) . . . . ? O3 Er1 N3 C26 178.3(7) . . . . ? O5 Er1 N3 C26 -171.1(6) . . . . ? O4 Er1 N3 C26 13.5(9) . . . . ? N1 Er1 N3 C26 104.2(6) . . . . ? N2 Er1 N3 C26 -105.4(6) . . . . ? O2 Er1 N3 C27 139.3(5) . . . . ? O1 Er1 N3 C27 -140.9(5) . . . . ? O3 Er1 N3 C27 -3.0(5) . . . . ? O5 Er1 N3 C27 7.6(7) . . . . ? O4 Er1 N3 C27 -167.8(4) . . . . ? N1 Er1 N3 C27 -77.1(5) . . . . ? N2 Er1 N3 C27 73.3(5) . . . . ? Er1 O1 C1 C2 177.0(5) . . . . ? Er1 O1 C1 C9 -1.2(8) . . . . ? O1 C1 C2 C3 -177.1(7) . . . . ? C9 C1 C2 C3 1.1(11) . . . . ? O1 C1 C2 Cl1 -0.1(10) . . . . ? C9 C1 C2 Cl1 178.1(5) . . . . ? C1 C2 C3 C4 -3.0(13) . . . . ? Cl1 C2 C3 C4 179.9(7) . . . . ? C2 C3 C4 C5 2.5(13) . . . . ? C2 C3 C4 Cl2 179.0(6) . . . . ? C3 C4 C5 C9 -0.3(13) . . . . ? Cl2 C4 C5 C9 -176.8(6) . . . . ? C3 C4 C5 C6 -180.0(9) . . . . ? Cl2 C4 C5 C6 3.4(13) . . . . ? C9 C5 C6 C7 1.0(13) . . . . ? C4 C5 C6 C7 -179.2(9) . . . . ? C5 C6 C7 C8 -0.2(15) . . . . ? C9 N1 C8 C7 2.2(13) . . . . ? Er1 N1 C8 C7 178.3(7) . . . . ? C6 C7 C8 N1 -1.6(15) . . . . ? C8 N1 C9 C5 -1.3(11) . . . . ? Er1 N1 C9 C5 -177.7(6) . . . . ? C8 N1 C9 C1 -179.9(7) . . . . ? Er1 N1 C9 C1 3.7(8) . . . . ? C6 C5 C9 N1 -0.3(12) . . . . ? C4 C5 C9 N1 179.9(7) . . . . ? C6 C5 C9 C1 178.2(7) . . . . ? C4 C5 C9 C1 -1.6(11) . . . . ? O1 C1 C9 N1 -1.8(9) . . . . ? C2 C1 C9 N1 179.8(6) . . . . ? O1 C1 C9 C5 179.5(6) . . . . ? C2 C1 C9 C5 1.2(10) . . . . ? Er1 O2 C10 C11 174.5(6) . . . . ? Er1 O2 C10 C18 -5.8(9) . . . . ? O2 C10 C11 C12 178.9(7) . . . . ? C18 C10 C11 C12 -0.7(11) . . . . ? O2 C10 C11 Cl3 -5.2(10) . . . . ? C18 C10 C11 Cl3 175.1(5) . . . . ? C10 C11 C12 C13 0.5(13) . . . . ? Cl3 C11 C12 C13 -175.4(6) . . . . ? C11 C12 C13 C14 0.6(13) . . . . ? C11 C12 C13 Cl4 178.4(6) . . . . ? C12 C13 C14 C18 -1.3(12) . . . . ? Cl4 C13 C14 C18 -179.1(6) . . . . ? C12 C13 C14 C15 177.2(8) . . . . ? Cl4 C13 C14 C15 -0.7(12) . . . . ? C18 C14 C15 C16 -1.5(13) . . . . ? C13 C14 C15 C16 -179.9(9) . . . . ? C14 C15 C16 C17 2.1(14) . . . . ? C18 N2 C17 C16 -0.8(12) . . . . ? Er1 N2 C17 C16 176.9(6) . . . . ? C15 C16 C17 N2 -0.9(14) . . . . ? C17 N2 C18 C14 1.4(11) . . . . ? Er1 N2 C18 C14 -176.6(6) . . . . ? C17 N2 C18 C10 178.9(7) . . . . ? Er1 N2 C18 C10 0.9(8) . . . . ? C13 C14 C18 N2 178.3(7) . . . . ? C15 C14 C18 N2 -0.3(11) . . . . ? C13 C14 C18 C10 1.0(11) . . . . ? C15 C14 C18 C10 -177.6(7) . . . . ? O2 C10 C18 N2 2.8(10) . . . . ? C11 C10 C18 N2 -177.5(6) . . . . ? O2 C10 C18 C14 -179.7(7) . . . . ? C11 C10 C18 C14 0.0(11) . . . . ? Er1 O3 C19 C20 174.4(5) . . . . ? Er1 O3 C19 C27 -4.7(8) . . . . ? O3 C19 C20 C21 -179.5(7) . . . . ? C27 C19 C20 C21 -0.3(10) . . . . ? O3 C19 C20 Cl5 -0.3(10) . . . . ? C27 C19 C20 Cl5 178.9(5) . . . . ? C19 C20 C21 C22 0.1(12) . . . . ? Cl5 C20 C21 C22 -179.1(7) . . . . ? C20 C21 C22 C23 -0.1(13) . . . . ? C20 C21 C22 Cl6 178.6(6) . . . . ? C21 C22 C23 C27 0.5(12) . . . . ? Cl6 C22 C23 C27 -178.3(6) . . . . ? C21 C22 C23 C24 179.3(8) . . . . ? Cl6 C22 C23 C24 0.6(11) . . . . ? C27 C23 C24 C25 -0.2(12) . . . . ? C22 C23 C24 C25 -179.1(8) . . . . ? C23 C24 C25 C26 1.1(12) . . . . ? C27 N3 C26 C25 -1.6(12) . . . . ? Er1 N3 C26 C25 177.1(6) . . . . ? C24 C25 C26 N3 -0.2(13) . . . . ? C26 N3 C27 C23 2.4(10) . . . . ? Er1 N3 C27 C23 -176.3(5) . . . . ? C26 N3 C27 C19 -179.3(7) . . . . ? Er1 N3 C27 C19 2.0(8) . . . . ? C24 C23 C27 N3 -1.6(11) . . . . ? C22 C23 C27 N3 177.4(7) . . . . ? C24 C23 C27 C19 -179.7(7) . . . . ? C22 C23 C27 C19 -0.7(11) . . . . ? O3 C19 C27 N3 1.6(10) . . . . ? C20 C19 C27 N3 -177.6(6) . . . . ? O3 C19 C27 C23 179.9(6) . . . . ? C20 C19 C27 C23 0.7(10) . . . . ? O8' O8 O8' O8 -28(35) 2_665 . . 3_565 ? O8' O8 O8' O8' -4(5) 2_665 . . 3_565 ? C28' O6 C28 C29 -131(9) . . . . ? C28 O6 C28' C29' 57(6) . . . . ? O7 O7' C30 C31 117(7) . . . . ? O7 O7' C30 C30 35(4) . . . 2_665 ? O7 O7' C30 C30 -130(7) . . . 3_565 ? O7' O7 C30 C31 -115(7) . . . . ? O7' O7 C30 C30 -157(4) . . . 2_665 ? O7' O7 C30 C30 147(10) . . . 3_565 ? O7' C30 C31 C30 -121(9) . . . 2_665 ? O7 C30 C31 C30 -58(8) . . . 2_665 ? C30 C30 C31 C30 83(2) 3_565 . . 2_665 ? O7' C30 C31 C30 156(8) . . . 3_565 ? O7 C30 C31 C30 -141(6) . . . 3_565 ? C30 C30 C31 C30 -83(2) 2_665 . . 3_565 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.796 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.107 #========================================================================== data_Gd _database_code_depnum_ccdc_archive 'CCDC 794957' #TrackingRef 'Gd.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H16 Br6 Gd N3 O5, C2 H6 O, 1/3(C2 H6 O), 1/3(H2 O)' _chemical_formula_sum 'C29.67 H24.67 Br6 Gd N3 O6.67' _chemical_formula_weight 1166.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3:H' _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 22.246(2) _cell_length_b 22.246(2) _cell_length_c 37.488(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16066(3) _cell_formula_units_Z 18 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 23639 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9918 _exptl_absorpt_coefficient_mu 8.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.183 _exptl_absorpt_correction_T_max 0.315 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15731 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0919 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6586 _reflns_number_gt 4320 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+66.6823P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6586 _refine_ls_number_parameters 431 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1260 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.1958 _refine_ls_wR_factor_gt 0.1710 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.46298(3) 0.49071(3) 0.428623(18) 0.0476(2) Uani 1 1 d . . . Br1 Br 0.30639(9) 0.40410(8) 0.55039(5) 0.0732(5) Uani 1 1 d . . . Br2 Br 0.20677(12) 0.13377(9) 0.49965(7) 0.1159(8) Uani 1 1 d . . . Br3 Br 0.52438(8) 0.70593(8) 0.51787(4) 0.0698(4) Uani 1 1 d . . . Br4 Br 0.68704(9) 0.88112(8) 0.40652(6) 0.0899(6) Uani 1 1 d . . . Br5 Br 0.39394(7) 0.44943(8) 0.28721(4) 0.0648(4) Uani 1 1 d . . . Br6 Br 0.20967(9) 0.54496(9) 0.31921(6) 0.0891(6) Uani 1 1 d . . . O1 O 0.3889(4) 0.4437(4) 0.4788(2) 0.050(2) Uani 1 1 d . . . O2 O 0.5039(4) 0.5903(4) 0.4640(2) 0.051(2) Uani 1 1 d . . . O3 O 0.4244(4) 0.4709(4) 0.3688(2) 0.050(2) Uani 1 1 d . . . O4 O 0.5327(5) 0.4668(5) 0.4702(3) 0.053(2) Uani 1 1 d D . . H4A H 0.558(5) 0.500(4) 0.483(3) 0.04(4) Uiso 1 1 d D . . H4B H 0.506(5) 0.433(4) 0.482(3) 0.06(4) Uiso 1 1 d D . . O5 O 0.5383(6) 0.4593(6) 0.3983(3) 0.069(3) Uani 1 1 d D . . H5A H 0.532(8) 0.454(8) 0.3767(8) 0.083 Uiso 1 1 d D . . H5B H 0.564(6) 0.443(7) 0.399(5) 0.083 Uiso 1 1 d D . . N1 N 0.3836(5) 0.3585(5) 0.4276(3) 0.051(3) Uani 1 1 d . . . N2 N 0.5478(5) 0.6064(5) 0.3964(3) 0.054(3) Uani 1 1 d . . . N3 N 0.3677(5) 0.5180(5) 0.4163(3) 0.052(3) Uani 1 1 d . . . C1 C 0.3473(6) 0.3763(6) 0.4836(4) 0.049(3) Uani 1 1 d . . . C2 C 0.3052(7) 0.3468(6) 0.5124(4) 0.061(4) Uani 1 1 d . . . C3 C 0.2649(7) 0.2756(7) 0.5165(4) 0.064(4) Uani 1 1 d . . . H3 H 0.2379 0.2582 0.5372 0.076 Uiso 1 1 calc R . . C4 C 0.2629(8) 0.2312(7) 0.4924(5) 0.067(4) Uani 1 1 d . . . C5 C 0.2996(7) 0.2559(6) 0.4599(4) 0.061(4) Uani 1 1 d . . . C6 C 0.3006(9) 0.2154(9) 0.4316(5) 0.078(5) Uani 1 1 d . . . H6 H 0.2739 0.1667 0.4328 0.093 Uiso 1 1 calc R . . C7 C 0.3391(10) 0.2456(8) 0.4031(5) 0.088(5) Uani 1 1 d . . . H7 H 0.3381 0.2179 0.3840 0.106 Uiso 1 1 calc R . . C8 C 0.3819(8) 0.3189(7) 0.4007(5) 0.067(4) Uani 1 1 d . . . H8 H 0.4088 0.3391 0.3802 0.081 Uiso 1 1 calc R . . C9 C 0.3430(7) 0.3286(6) 0.4567(4) 0.056(3) Uani 1 1 d . . . C10 C 0.5441(6) 0.6549(7) 0.4522(4) 0.053(3) Uani 1 1 d . . . C11 C 0.5615(7) 0.7144(7) 0.4725(4) 0.059(4) Uani 1 1 d . . . C12 C 0.6047(7) 0.7804(7) 0.4581(5) 0.067(4) Uani 1 1 d . . . H12 H 0.6167 0.8195 0.4723 0.080 Uiso 1 1 calc R . . C13 C 0.6297(7) 0.7898(6) 0.4243(4) 0.056(3) Uani 1 1 d . . . C14 C 0.6123(7) 0.7329(6) 0.4021(4) 0.053(3) Uani 1 1 d . . . C15 C 0.6323(7) 0.7341(8) 0.3663(5) 0.069(4) Uani 1 1 d . . . H15 H 0.6614 0.7774 0.3556 0.083 Uiso 1 1 calc R . . C16 C 0.6122(8) 0.6777(8) 0.3474(5) 0.077(5) Uani 1 1 d . . . H16 H 0.6267 0.6806 0.3236 0.093 Uiso 1 1 calc R . . C17 C 0.5679(7) 0.6116(8) 0.3635(4) 0.063(4) Uani 1 1 d . . . H17 H 0.5530 0.5711 0.3500 0.075 Uiso 1 1 calc R . . C18 C 0.5692(6) 0.6647(7) 0.4163(4) 0.053(3) Uani 1 1 d . . . C19 C 0.3772(6) 0.4855(6) 0.3570(4) 0.047(3) Uani 1 1 d . . . C20 C 0.3550(6) 0.4802(6) 0.3231(4) 0.052(3) Uani 1 1 d . . . C21 C 0.3027(6) 0.4956(6) 0.3118(4) 0.054(3) Uani 1 1 d . . . H21 H 0.2878 0.4889 0.2879 0.065 Uiso 1 1 calc R . . C22 C 0.2754(6) 0.5196(6) 0.3356(4) 0.055(4) Uani 1 1 d . . . C23 C 0.2941(6) 0.5286(6) 0.3727(4) 0.049(3) Uani 1 1 d . . . C24 C 0.2689(6) 0.5537(6) 0.3991(5) 0.055(4) Uani 1 1 d . . . H24 H 0.2356 0.5663 0.3933 0.067 Uiso 1 1 calc R . . C25 C 0.2913(7) 0.5603(7) 0.4325(5) 0.066(4) Uani 1 1 d . . . H25 H 0.2739 0.5774 0.4503 0.079 Uiso 1 1 calc R . . C26 C 0.3421(7) 0.5412(6) 0.4410(4) 0.059(4) Uani 1 1 d . . . H26 H 0.3576 0.5453 0.4646 0.071 Uiso 1 1 calc R . . C27 C 0.3451(6) 0.5108(6) 0.3825(4) 0.049(3) Uani 1 1 d . . . O6 O 0.5134(12) 0.4260(11) 0.3272(7) 0.192(8) Uiso 1 1 d D . . O7 O 0.386(3) 0.786(2) 0.5765(14) 0.049(9) Uiso 0.17 1 d PD . . O7' O 0.424(2) 0.8024(19) 0.5617(15) 0.049(9) Uiso 0.17 1 d PD . . O8 O 0.348(8) 0.631(7) 0.228(3) 0.14(4) Uiso 0.17 1 d P . . O8' O 0.306(6) 0.634(4) 0.233(3) 0.10(3) Uiso 0.17 1 d P . . C28 C 0.497(4) 0.368(3) 0.3037(18) 0.222(17) Uiso 0.50 1 d PD A 1 C28' C 0.5877(18) 0.451(4) 0.320(2) 0.222(17) Uiso 0.50 1 d PD A 2 C29 C 0.565(4) 0.382(4) 0.288(2) 0.222(17) Uiso 0.50 1 d PD A 1 C29' C 0.607(4) 0.420(4) 0.289(2) 0.222(17) Uiso 0.50 1 d PD A 2 C30 C 0.383(3) 0.730(2) 0.555(2) 0.159(15) Uiso 0.33 1 d PD . . C31 C 0.3333 0.6667 0.5346(14) 0.159(15) Uiso 1 3 d SD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0646(4) 0.0485(4) 0.0336(4) 0.0024(3) 0.0031(3) 0.0311(3) Br1 0.0898(10) 0.0744(10) 0.0569(11) 0.0100(8) 0.0228(8) 0.0423(8) Br2 0.1261(16) 0.0584(10) 0.135(2) 0.0171(11) 0.0372(15) 0.0246(10) Br3 0.0968(11) 0.0683(9) 0.0514(10) -0.0088(7) -0.0015(8) 0.0466(8) Br4 0.0979(12) 0.0517(9) 0.1043(17) 0.0110(9) 0.0192(11) 0.0255(8) Br5 0.0656(8) 0.0859(10) 0.0427(9) -0.0082(7) 0.0017(7) 0.0376(8) Br6 0.0822(11) 0.0994(12) 0.1065(18) -0.0056(11) -0.0197(10) 0.0609(10) O1 0.078(6) 0.038(4) 0.036(5) 0.004(4) 0.001(4) 0.029(4) O2 0.060(5) 0.046(5) 0.046(6) 0.008(4) 0.007(4) 0.025(4) O3 0.063(5) 0.057(5) 0.041(5) 0.000(4) 0.006(4) 0.038(4) O4 0.075(6) 0.049(6) 0.036(6) 0.003(5) 0.009(5) 0.032(5) O5 0.094(7) 0.097(7) 0.045(7) -0.012(6) -0.002(6) 0.069(6) N1 0.068(7) 0.054(6) 0.034(6) -0.007(5) -0.009(5) 0.033(5) N2 0.065(7) 0.054(6) 0.050(8) 0.007(6) 0.008(6) 0.035(5) N3 0.067(7) 0.049(6) 0.040(7) 0.002(5) 0.013(5) 0.030(5) C1 0.044(7) 0.055(8) 0.052(9) 0.012(7) 0.004(6) 0.027(6) C2 0.064(8) 0.049(8) 0.078(12) 0.014(7) 0.015(8) 0.033(7) C3 0.072(9) 0.076(10) 0.048(9) 0.010(8) 0.010(7) 0.040(8) C4 0.079(10) 0.052(8) 0.068(12) 0.014(8) 0.015(8) 0.032(7) C5 0.074(9) 0.044(7) 0.056(10) 0.004(7) -0.001(8) 0.023(7) C6 0.100(12) 0.071(10) 0.047(11) 0.003(8) -0.011(9) 0.032(9) C7 0.127(15) 0.064(10) 0.075(14) -0.025(9) -0.023(12) 0.049(10) C8 0.081(10) 0.065(9) 0.063(11) 0.003(8) 0.008(8) 0.041(8) C9 0.068(8) 0.043(7) 0.057(10) 0.001(7) -0.003(7) 0.028(6) C10 0.050(7) 0.069(9) 0.044(9) 0.006(7) 0.002(6) 0.032(7) C11 0.066(8) 0.048(7) 0.069(11) -0.008(7) 0.002(7) 0.032(7) C12 0.065(9) 0.067(9) 0.082(13) 0.004(8) -0.003(8) 0.043(8) C13 0.061(8) 0.039(7) 0.064(11) 0.000(7) -0.007(7) 0.021(6) C14 0.065(8) 0.050(7) 0.041(8) 0.012(6) -0.001(7) 0.027(6) C15 0.055(8) 0.067(9) 0.086(14) 0.014(9) 0.004(8) 0.030(7) C16 0.077(10) 0.068(10) 0.073(13) 0.027(9) 0.033(9) 0.026(8) C17 0.082(10) 0.080(10) 0.032(8) -0.001(7) 0.002(7) 0.045(8) C18 0.054(7) 0.061(8) 0.052(9) 0.008(7) 0.003(7) 0.035(7) C19 0.054(7) 0.046(7) 0.034(8) -0.003(6) 0.001(6) 0.020(6) C20 0.056(7) 0.051(7) 0.033(7) -0.009(6) 0.007(6) 0.015(6) C21 0.054(7) 0.054(7) 0.058(10) -0.011(7) -0.021(7) 0.030(6) C22 0.056(8) 0.044(7) 0.071(11) -0.009(7) -0.013(7) 0.029(6) C23 0.052(7) 0.052(7) 0.047(9) 0.007(6) 0.008(6) 0.029(6) C24 0.050(7) 0.047(7) 0.075(12) 0.003(7) 0.016(7) 0.028(6) C25 0.073(10) 0.056(8) 0.077(13) 0.014(8) 0.023(9) 0.039(7) C26 0.075(9) 0.051(7) 0.045(9) 0.008(6) 0.021(7) 0.026(7) C27 0.062(8) 0.038(6) 0.046(9) 0.007(6) 0.016(7) 0.026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2 2.342(8) . ? Gd1 O3 2.364(9) . ? Gd1 O1 2.371(9) . ? Gd1 O5 2.399(10) . ? Gd1 O4 2.437(10) . ? Gd1 N3 2.522(10) . ? Gd1 N1 2.565(10) . ? Gd1 N2 2.605(11) . ? Br1 C2 1.904(15) . ? Br2 C4 1.905(13) . ? Br3 C11 1.861(16) . ? Br4 C13 1.898(13) . ? Br5 C20 1.904(12) . ? Br6 C22 1.914(12) . ? O1 C1 1.324(14) . ? O2 C10 1.332(15) . ? O3 C19 1.320(14) . ? O4 H4A 0.82(10) . ? O4 H4B 0.82(9) . ? O5 H5A 0.82(3) . ? O5 H5B 0.82(15) . ? N1 C8 1.326(17) . ? N1 C9 1.358(17) . ? N2 C17 1.296(17) . ? N2 C18 1.360(16) . ? N3 C26 1.320(16) . ? N3 C27 1.343(17) . ? C1 C2 1.362(19) . ? C1 C9 1.431(19) . ? C2 C3 1.383(18) . ? C3 C4 1.32(2) . ? C3 H3 0.9400 . ? C4 C5 1.41(2) . ? C5 C6 1.40(2) . ? C5 C9 1.415(17) . ? C6 C7 1.32(2) . ? C6 H6 0.9400 . ? C7 C8 1.42(2) . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? C10 C11 1.402(18) . ? C10 C18 1.432(18) . ? C11 C12 1.400(19) . ? C12 C13 1.36(2) . ? C12 H12 0.9400 . ? C13 C14 1.398(19) . ? C14 C15 1.41(2) . ? C14 C18 1.432(17) . ? C15 C16 1.31(2) . ? C15 H15 0.9400 . ? C16 C17 1.432(19) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C19 C20 1.347(18) . ? C19 C27 1.462(17) . ? C20 C21 1.432(17) . ? C21 C22 1.330(19) . ? C21 H21 0.9400 . ? C22 C23 1.44(2) . ? C23 C24 1.386(18) . ? C23 C27 1.424(17) . ? C24 C25 1.33(2) . ? C24 H24 0.9400 . ? C25 C26 1.428(19) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? O6 C28 1.45(2) . ? O6 C28' 1.48(2) . ? O7 O7' 0.91(6) . ? O7 C30 1.45(2) . ? O7' C30 1.42(2) . ? O8 O8' 0.83(12) 2_665 ? O8 O8' 0.98(11) . ? O8 O8' 1.68(9) 3_565 ? O8 O8 1.73(19) 3_565 ? O8 O8 1.73(19) 2_665 ? O8' O8 0.83(12) 3_565 ? O8' O8' 1.17(11) 2_665 ? O8' O8' 1.17(11) 3_565 ? O8' O8 1.68(9) 2_665 ? C28 C29 1.50(2) . ? C28' C29' 1.52(2) . ? C30 C31 1.496(19) . ? C31 C30 1.496(19) 2_665 ? C31 C30 1.496(19) 3_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O3 130.4(3) . . ? O2 Gd1 O1 79.8(3) . . ? O3 Gd1 O1 124.3(3) . . ? O2 Gd1 O5 123.1(3) . . ? O3 Gd1 O5 74.8(3) . . ? O1 Gd1 O5 132.8(3) . . ? O2 Gd1 O4 81.7(3) . . ? O3 Gd1 O4 141.1(3) . . ? O1 Gd1 O4 77.0(3) . . ? O5 Gd1 O4 68.1(3) . . ? O2 Gd1 N3 81.5(3) . . ? O3 Gd1 N3 66.4(3) . . ? O1 Gd1 N3 76.6(3) . . ? O5 Gd1 N3 141.0(4) . . ? O4 Gd1 N3 150.7(3) . . ? O2 Gd1 N1 144.3(3) . . ? O3 Gd1 N1 78.1(3) . . ? O1 Gd1 N1 65.0(3) . . ? O5 Gd1 N1 80.8(4) . . ? O4 Gd1 N1 84.7(3) . . ? N3 Gd1 N1 95.3(3) . . ? O2 Gd1 N2 65.3(3) . . ? O3 Gd1 N2 76.1(3) . . ? O1 Gd1 N2 143.5(3) . . ? O5 Gd1 N2 78.5(4) . . ? O4 Gd1 N2 106.6(3) . . ? N3 Gd1 N2 87.6(3) . . ? N1 Gd1 N2 150.4(4) . . ? C1 O1 Gd1 123.1(8) . . ? C10 O2 Gd1 124.4(8) . . ? C19 O3 Gd1 122.0(7) . . ? Gd1 O4 H4A 113(8) . . ? Gd1 O4 H4B 107(9) . . ? H4A O4 H4B 111(10) . . ? Gd1 O5 H5A 114(10) . . ? Gd1 O5 H5B 148(10) . . ? H5A O5 H5B 96(10) . . ? C8 N1 C9 119.6(12) . . ? C8 N1 Gd1 123.2(10) . . ? C9 N1 Gd1 117.2(8) . . ? C17 N2 C18 119.6(12) . . ? C17 N2 Gd1 125.2(10) . . ? C18 N2 Gd1 115.1(9) . . ? C26 N3 C27 119.9(12) . . ? C26 N3 Gd1 123.1(10) . . ? C27 N3 Gd1 117.0(8) . . ? O1 C1 C2 125.2(13) . . ? O1 C1 C9 119.5(12) . . ? C2 C1 C9 115.2(12) . . ? C1 C2 C3 122.4(14) . . ? C1 C2 Br1 119.6(10) . . ? C3 C2 Br1 117.9(12) . . ? C4 C3 C2 122.6(15) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 120.0(13) . . ? C3 C4 Br2 120.7(12) . . ? C5 C4 Br2 119.2(11) . . ? C6 C5 C4 126.4(13) . . ? C6 C5 C9 116.7(15) . . ? C4 C5 C9 116.7(14) . . ? C7 C6 C5 119.9(15) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 121.8(17) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? N1 C8 C7 119.6(15) . . ? N1 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? N1 C9 C5 122.3(13) . . ? N1 C9 C1 115.0(11) . . ? C5 C9 C1 122.7(14) . . ? O2 C10 C11 123.8(13) . . ? O2 C10 C18 118.6(12) . . ? C11 C10 C18 117.5(12) . . ? C12 C11 C10 120.1(15) . . ? C12 C11 Br3 119.7(11) . . ? C10 C11 Br3 120.1(10) . . ? C13 C12 C11 122.4(14) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 120.6(13) . . ? C12 C13 Br4 119.8(11) . . ? C14 C13 Br4 119.6(12) . . ? C13 C14 C15 127.4(13) . . ? C13 C14 C18 118.3(13) . . ? C15 C14 C18 114.3(13) . . ? C16 C15 C14 123.0(15) . . ? C16 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C15 C16 C17 118.9(16) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? N2 C17 C16 121.6(14) . . ? N2 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? N2 C18 C14 122.5(13) . . ? N2 C18 C10 116.4(12) . . ? C14 C18 C10 121.0(13) . . ? O3 C19 C20 126.5(12) . . ? O3 C19 C27 118.5(12) . . ? C20 C19 C27 114.9(12) . . ? C19 C20 C21 124.4(12) . . ? C19 C20 Br5 119.0(10) . . ? C21 C20 Br5 116.6(10) . . ? C22 C21 C20 119.0(13) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C23 123.2(12) . . ? C21 C22 Br6 118.2(12) . . ? C23 C22 Br6 118.6(10) . . ? C24 C23 C27 117.8(14) . . ? C24 C23 C22 126.9(13) . . ? C27 C23 C22 115.2(11) . . ? C25 C24 C23 120.9(13) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.1(14) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? N3 C26 C25 121.5(15) . . ? N3 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? N3 C27 C23 120.9(11) . . ? N3 C27 C19 115.9(11) . . ? C23 C27 C19 123.2(13) . . ? C28 O6 C28' 88(4) . . ? O7' O7 C30 70(2) . . ? O7 O7' C30 73(2) . . ? O8' O8 O8' 80(10) 2_665 . ? O8' O8 O8 73(9) 2_665 3_565 ? O8' O8 O8 71(7) . 2_665 ? O8 O8 O8 60.00(4) 3_565 2_665 ? O8 O8' O8' 114(10) 3_565 2_665 ? O8 O8' O8' 56(10) 3_565 3_565 ? O8 O8' O8' 102(9) . 3_565 ? O8' O8' O8' 60.00(4) 2_665 3_565 ? O8 O8' O8 79(9) 3_565 2_665 ? O8 O8' O8 76(8) . 2_665 ? O6 C28 C29 106(5) . . ? O6 C28' C29' 119(6) . . ? O7' C30 C31 155(6) . . ? O7 C30 C31 143(6) . . ? C30 C31 C30 95(5) 2_665 . ? C30 C31 C30 95(5) 2_665 3_565 ? C30 C31 C30 95(5) . 3_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Gd1 O1 C1 -170.1(9) . . . . ? O3 Gd1 O1 C1 57.6(9) . . . . ? O5 Gd1 O1 C1 -43.9(10) . . . . ? O4 Gd1 O1 C1 -86.4(9) . . . . ? N3 Gd1 O1 C1 106.3(9) . . . . ? N1 Gd1 O1 C1 3.8(8) . . . . ? N2 Gd1 O1 C1 173.2(8) . . . . ? O3 Gd1 O2 C10 -38.0(10) . . . . ? O1 Gd1 O2 C10 -164.7(9) . . . . ? O5 Gd1 O2 C10 60.3(10) . . . . ? O4 Gd1 O2 C10 117.1(9) . . . . ? N3 Gd1 O2 C10 -86.9(9) . . . . ? N1 Gd1 O2 C10 -174.2(8) . . . . ? N2 Gd1 O2 C10 4.4(8) . . . . ? O2 Gd1 O3 C19 -51.0(9) . . . . ? O1 Gd1 O3 C19 56.3(9) . . . . ? O5 Gd1 O3 C19 -171.8(9) . . . . ? O4 Gd1 O3 C19 170.4(8) . . . . ? N3 Gd1 O3 C19 3.3(8) . . . . ? N1 Gd1 O3 C19 104.6(8) . . . . ? N2 Gd1 O3 C19 -90.2(8) . . . . ? O2 Gd1 N1 C8 -171.7(9) . . . . ? O3 Gd1 N1 C8 40.9(10) . . . . ? O1 Gd1 N1 C8 178.0(11) . . . . ? O5 Gd1 N1 C8 -35.4(10) . . . . ? O4 Gd1 N1 C8 -104.0(10) . . . . ? N3 Gd1 N1 C8 105.4(10) . . . . ? N2 Gd1 N1 C8 10.8(14) . . . . ? O2 Gd1 N1 C9 6.5(12) . . . . ? O3 Gd1 N1 C9 -140.8(9) . . . . ? O1 Gd1 N1 C9 -3.7(8) . . . . ? O5 Gd1 N1 C9 142.9(9) . . . . ? O4 Gd1 N1 C9 74.3(9) . . . . ? N3 Gd1 N1 C9 -76.3(9) . . . . ? N2 Gd1 N1 C9 -170.9(8) . . . . ? O2 Gd1 N2 C17 179.7(12) . . . . ? O3 Gd1 N2 C17 -32.2(11) . . . . ? O1 Gd1 N2 C17 -162.1(9) . . . . ? O5 Gd1 N2 C17 44.7(11) . . . . ? O4 Gd1 N2 C17 107.4(11) . . . . ? N3 Gd1 N2 C17 -98.5(11) . . . . ? N1 Gd1 N2 C17 -1.9(15) . . . . ? O2 Gd1 N2 C18 -3.0(8) . . . . ? O3 Gd1 N2 C18 145.0(9) . . . . ? O1 Gd1 N2 C18 15.1(11) . . . . ? O5 Gd1 N2 C18 -138.0(9) . . . . ? O4 Gd1 N2 C18 -75.3(9) . . . . ? N3 Gd1 N2 C18 78.7(8) . . . . ? N1 Gd1 N2 C18 175.3(8) . . . . ? O2 Gd1 N3 C26 -38.6(9) . . . . ? O3 Gd1 N3 C26 -179.8(10) . . . . ? O1 Gd1 N3 C26 42.9(9) . . . . ? O5 Gd1 N3 C26 -172.4(9) . . . . ? O4 Gd1 N3 C26 16.9(13) . . . . ? N1 Gd1 N3 C26 105.6(9) . . . . ? N2 Gd1 N3 C26 -103.9(10) . . . . ? O2 Gd1 N3 C27 138.4(9) . . . . ? O3 Gd1 N3 C27 -2.8(8) . . . . ? O1 Gd1 N3 C27 -140.1(9) . . . . ? O5 Gd1 N3 C27 4.6(11) . . . . ? O4 Gd1 N3 C27 -166.1(8) . . . . ? N1 Gd1 N3 C27 -77.3(9) . . . . ? N2 Gd1 N3 C27 73.1(9) . . . . ? Gd1 O1 C1 C2 178.2(10) . . . . ? Gd1 O1 C1 C9 -3.7(15) . . . . ? O1 C1 C2 C3 -177.4(12) . . . . ? C9 C1 C2 C3 4(2) . . . . ? O1 C1 C2 Br1 -2.5(19) . . . . ? C9 C1 C2 Br1 179.4(9) . . . . ? C1 C2 C3 C4 -2(2) . . . . ? Br1 C2 C3 C4 -177.0(12) . . . . ? C2 C3 C4 C5 -4(2) . . . . ? C2 C3 C4 Br2 179.6(11) . . . . ? C3 C4 C5 C6 -177.9(15) . . . . ? Br2 C4 C5 C6 -1(2) . . . . ? C3 C4 C5 C9 6(2) . . . . ? Br2 C4 C5 C9 -177.0(10) . . . . ? C4 C5 C6 C7 -178.0(16) . . . . ? C9 C5 C6 C7 -2(2) . . . . ? C5 C6 C7 C8 2(3) . . . . ? C9 N1 C8 C7 -2(2) . . . . ? Gd1 N1 C8 C7 176.6(11) . . . . ? C6 C7 C8 N1 0(3) . . . . ? C8 N1 C9 C5 1(2) . . . . ? Gd1 N1 C9 C5 -177.0(10) . . . . ? C8 N1 C9 C1 -178.2(12) . . . . ? Gd1 N1 C9 C1 3.5(14) . . . . ? C6 C5 C9 N1 1(2) . . . . ? C4 C5 C9 N1 176.7(13) . . . . ? C6 C5 C9 C1 -179.9(13) . . . . ? C4 C5 C9 C1 -4(2) . . . . ? O1 C1 C9 N1 -0.2(17) . . . . ? C2 C1 C9 N1 178.1(12) . . . . ? O1 C1 C9 C5 -179.7(12) . . . . ? C2 C1 C9 C5 -1.5(19) . . . . ? Gd1 O2 C10 C11 172.2(9) . . . . ? Gd1 O2 C10 C18 -5.4(15) . . . . ? O2 C10 C11 C12 179.4(12) . . . . ? C18 C10 C11 C12 -2.9(19) . . . . ? O2 C10 C11 Br3 -3.2(18) . . . . ? C18 C10 C11 Br3 174.4(9) . . . . ? C10 C11 C12 C13 2(2) . . . . ? Br3 C11 C12 C13 -175.8(11) . . . . ? C11 C12 C13 C14 1(2) . . . . ? C11 C12 C13 Br4 179.2(10) . . . . ? C12 C13 C14 C15 178.0(14) . . . . ? Br4 C13 C14 C15 -0.3(19) . . . . ? C12 C13 C14 C18 -1.8(19) . . . . ? Br4 C13 C14 C18 179.9(9) . . . . ? C13 C14 C15 C16 -178.7(14) . . . . ? C18 C14 C15 C16 1(2) . . . . ? C14 C15 C16 C17 0(2) . . . . ? C18 N2 C17 C16 0(2) . . . . ? Gd1 N2 C17 C16 177.0(10) . . . . ? C15 C16 C17 N2 -1(2) . . . . ? C17 N2 C18 C14 1.4(19) . . . . ? Gd1 N2 C18 C14 -176.0(9) . . . . ? C17 N2 C18 C10 179.2(12) . . . . ? Gd1 N2 C18 C10 1.7(14) . . . . ? C13 C14 C18 N2 178.0(11) . . . . ? C15 C14 C18 N2 -1.8(18) . . . . ? C13 C14 C18 C10 0.3(19) . . . . ? C15 C14 C18 C10 -179.5(12) . . . . ? O2 C10 C18 N2 1.9(17) . . . . ? C11 C10 C18 N2 -175.8(11) . . . . ? O2 C10 C18 C14 179.8(11) . . . . ? C11 C10 C18 C14 2.0(18) . . . . ? Gd1 O3 C19 C20 175.6(10) . . . . ? Gd1 O3 C19 C27 -3.6(14) . . . . ? O3 C19 C20 C21 178.9(11) . . . . ? C27 C19 C20 C21 -1.8(18) . . . . ? O3 C19 C20 Br5 -0.4(17) . . . . ? C27 C19 C20 Br5 178.9(8) . . . . ? C19 C20 C21 C22 3.0(19) . . . . ? Br5 C20 C21 C22 -177.7(10) . . . . ? C20 C21 C22 C23 -2.4(19) . . . . ? C20 C21 C22 Br6 176.4(9) . . . . ? C21 C22 C23 C24 179.3(12) . . . . ? Br6 C22 C23 C24 0.6(18) . . . . ? C21 C22 C23 C27 0.8(18) . . . . ? Br6 C22 C23 C27 -177.9(8) . . . . ? C27 C23 C24 C25 -0.6(18) . . . . ? C22 C23 C24 C25 -179.1(13) . . . . ? C23 C24 C25 C26 0.1(19) . . . . ? C27 N3 C26 C25 -1.1(18) . . . . ? Gd1 N3 C26 C25 175.9(9) . . . . ? C24 C25 C26 N3 0.8(19) . . . . ? C26 N3 C27 C23 0.5(17) . . . . ? Gd1 N3 C27 C23 -176.6(8) . . . . ? C26 N3 C27 C19 179.3(11) . . . . ? Gd1 N3 C27 C19 2.1(13) . . . . ? C24 C23 C27 N3 0.3(17) . . . . ? C22 C23 C27 N3 179.0(11) . . . . ? C24 C23 C27 C19 -178.3(11) . . . . ? C22 C23 C27 C19 0.3(17) . . . . ? O3 C19 C27 N3 0.8(16) . . . . ? C20 C19 C27 N3 -178.6(11) . . . . ? O3 C19 C27 C23 179.5(10) . . . . ? C20 C19 C27 C23 0.2(17) . . . . ? O8' O8 O8' O8' -16(14) 3_565 . . 2_665 ? O8 O8 O8' O8' -17(15) 2_665 . . 2_665 ? O8' O8 O8' O8' 16(14) 2_665 . . 3_565 ? O8 O8 O8' O8' -2(2) 2_665 . . 3_565 ? O8' O8 O8' O8 17(15) 2_665 . . 2_665 ? O8' O8 O8' O8 2(2) 3_565 . . 2_665 ? C28' O6 C28 C29 -6(7) . . . . ? C28 O6 C28' C29' 15(8) . . . . ? O7 O7' C30 C31 106(15) . . . . ? O7' O7 C30 C31 -138(11) . . . . ? O7' C30 C31 C30 -99(17) . . . 2_665 ? O7 C30 C31 C30 -27(13) . . . 2_665 ? O7' C30 C31 C30 165(14) . . . 3_565 ? O7 C30 C31 C30 -123(7) . . . 3_565 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.938 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.161