# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Xiaoping Yang' R.A.Jones M.M.Oye M.Wiester R.J.Lai _publ_contact_author_name 'Richard Jones' _publ_contact_author_email rajones@mail.utexas.edu data_complex-1 _database_code_depnum_ccdc_archive 'CCDC 777193' #TrackingRef '- Complex-1 revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H46 Br2 Cl6 N4 O8 Tb2' _chemical_formula_sum 'C36 H46 Br2 Cl6 N4 O8 Tb2' _chemical_formula_weight 1353.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.302(2) _cell_length_b 11.513(3) _cell_length_c 11.737(2) _cell_angle_alpha 66.37(3) _cell_angle_beta 64.29(4) _cell_angle_gamma 87.93(3) _cell_volume 1133.1(7) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4211 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 5.264 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.3905 _exptl_absorpt_correction_T_max 0.4508 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6439 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3973 _reflns_number_gt 3587 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0220P)^2^+3.8116P] 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 3973 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.74236(3) 0.06751(2) 0.86678(3) 0.01796(10) Uani 1 1 d U . . Br1 Br 1.32094(6) 0.48140(6) 0.12209(6) 0.02648(15) Uani 1 1 d U . . Cl1 Cl 0.97847(14) 0.16302(12) 0.87942(13) 0.0175(3) Uani 1 1 d U . . Cl2 Cl 0.69047(15) -0.07020(14) 0.74702(15) 0.0245(3) Uani 1 1 d U . . Cl3 Cl 0.52998(13) -0.13320(12) 1.11583(13) 0.0157(3) Uani 1 1 d U . . O1 O 0.9873(4) 0.1214(3) 0.6255(4) 0.0163(8) Uani 1 1 d U . . O2 O 0.7914(4) 0.2589(3) 0.6790(4) 0.0140(8) Uani 1 1 d U . . H2A H 0.7198 0.3103 0.6944 0.017 Uiso 1 1 calc R . . O3 O 0.6343(4) 0.1627(4) 1.0361(4) 0.0237(9) Uani 1 1 d U . . H3B H 0.5690 0.0998 1.0864 0.028 Uiso 1 1 calc R . . O4 O 0.8748(4) -0.1106(3) 0.9283(4) 0.0157(8) Uani 1 1 d U . . H4A H 0.8974 -0.0980 0.9818 0.019 Uiso 1 1 calc R . . N1 N 0.7861(5) 0.6117(4) 0.3951(5) 0.0148(9) Uani 1 1 d U . . H1A H 0.8532 0.6591 0.3123 0.018 Uiso 1 1 calc R . . N2 N 0.6711(5) 0.4527(4) 0.6003(4) 0.0146(9) Uani 1 1 d U . . C1 C 1.0970(7) 0.0439(6) 0.5983(6) 0.0326(16) Uani 1 1 d U . . H1B H 1.1137 0.0343 0.5157 0.049 Uiso 1 1 calc R . . H1C H 1.0655 -0.0391 0.6764 0.049 Uiso 1 1 calc R . . H1D H 1.1859 0.0842 0.5845 0.049 Uiso 1 1 calc R . . C2 C 1.0146(6) 0.2396(5) 0.5190(5) 0.0137(11) Uani 1 1 d U . . C3 C 1.1374(6) 0.2888(5) 0.3927(5) 0.0154(11) Uani 1 1 d U . . H3A H 1.2119 0.2410 0.3728 0.019 Uiso 1 1 calc R . . C4 C 1.1488(6) 0.4120(5) 0.2941(5) 0.0155(11) Uani 1 1 d U . . C5 C 1.0406(6) 0.4819(5) 0.3194(5) 0.0156(11) Uani 1 1 d U . . H5A H 1.0487 0.5630 0.2517 0.019 Uiso 1 1 calc R . . C6 C 0.9145(5) 0.4296(5) 0.4509(5) 0.0121(10) Uani 1 1 d U . . C7 C 0.9013(5) 0.3094(5) 0.5541(5) 0.0120(10) Uani 1 1 d U . . C8 C 0.7950(6) 0.4977(5) 0.4814(5) 0.0135(11) Uani 1 1 d U . . C9 C 0.6516(6) 0.6406(5) 0.4609(6) 0.0167(11) Uani 1 1 d U . . C10 C 0.5872(6) 0.7436(5) 0.4140(6) 0.0224(12) Uani 1 1 d U . . H10A H 0.6362 0.8115 0.3257 0.027 Uiso 1 1 calc R . . C11 C 0.4473(7) 0.7402(6) 0.5047(7) 0.0258(13) Uani 1 1 d U . . H11A H 0.3983 0.8067 0.4766 0.031 Uiso 1 1 calc R . . C12 C 0.3745(7) 0.6394(6) 0.6394(7) 0.0269(14) Uani 1 1 d U . . H12A H 0.2800 0.6425 0.6988 0.032 Uiso 1 1 calc R . . C13 C 0.4382(6) 0.5377(6) 0.6853(6) 0.0227(12) Uani 1 1 d U . . H13A H 0.3904 0.4708 0.7744 0.027 Uiso 1 1 calc R . . C14 C 0.5779(6) 0.5397(5) 0.5918(6) 0.0161(11) Uani 1 1 d U . . C15 C 0.6770(8) 0.0946(6) 1.2367(7) 0.0337(15) Uani 1 1 d U . . H15A H 0.6978 0.1260 1.2925 0.050 Uiso 1 1 calc R . . H15B H 0.7532 0.0498 1.2001 0.050 Uiso 1 1 calc R . . H15C H 0.5853 0.0369 1.2935 0.050 Uiso 1 1 calc R . . C16 C 0.6688(6) 0.2032(5) 1.1206(6) 0.0210(12) Uani 1 1 d U . . H16B H 0.5950 0.2506 1.1580 0.025 Uiso 1 1 calc R . . H16A H 0.7619 0.2609 1.0631 0.025 Uiso 1 1 calc R . . C17 C 0.9512(7) -0.3067(6) 0.9135(8) 0.0368(17) Uani 1 1 d U . . H17A H 0.9175 -0.3969 0.9509 0.055 Uiso 1 1 calc R . . H17B H 1.0302 -0.2947 0.9325 0.055 Uiso 1 1 calc R . . H17C H 0.9845 -0.2680 0.8143 0.055 Uiso 1 1 calc R . . C18 C 0.8300(6) -0.2456(5) 0.9797(7) 0.0233(13) Uani 1 1 d U . . H18A H 0.7499 -0.2586 0.9611 0.028 Uiso 1 1 calc R . . H18B H 0.7949 -0.2864 1.0802 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01573(15) 0.01708(15) 0.01426(15) -0.00366(11) -0.00387(11) 0.00143(10) Br1 0.0159(3) 0.0242(3) 0.0160(3) -0.0014(2) 0.0061(2) -0.0023(2) Cl1 0.0136(6) 0.0144(6) 0.0160(6) -0.0002(5) -0.0050(5) -0.0030(5) Cl2 0.0173(7) 0.0359(8) 0.0216(7) -0.0202(7) -0.0028(6) 0.0031(6) Cl3 0.0113(6) 0.0156(6) 0.0107(6) 0.0007(5) -0.0027(5) 0.0020(5) O1 0.0166(19) 0.0125(18) 0.0101(18) -0.0015(15) -0.0012(16) 0.0063(15) O2 0.0087(17) 0.0131(17) 0.0113(18) -0.0012(15) -0.0009(15) 0.0047(14) O3 0.017(2) 0.031(2) 0.025(2) -0.0169(19) -0.0066(18) -0.0006(17) O4 0.0150(19) 0.0123(18) 0.0173(19) -0.0034(15) -0.0080(16) 0.0006(15) N1 0.016(2) 0.012(2) 0.012(2) -0.0017(18) -0.0058(19) 0.0010(17) N2 0.013(2) 0.013(2) 0.011(2) -0.0036(18) -0.0021(19) 0.0012(17) C1 0.030(4) 0.026(3) 0.016(3) -0.001(3) 0.003(3) 0.018(3) C2 0.015(3) 0.013(2) 0.011(2) -0.005(2) -0.004(2) 0.000(2) C3 0.015(3) 0.016(3) 0.018(3) -0.010(2) -0.007(2) 0.004(2) C4 0.015(3) 0.015(3) 0.010(2) -0.004(2) 0.000(2) -0.003(2) C5 0.019(3) 0.011(2) 0.011(3) -0.001(2) -0.005(2) -0.001(2) C6 0.010(2) 0.010(2) 0.013(2) -0.004(2) -0.003(2) -0.0010(19) C7 0.011(2) 0.014(2) 0.011(2) -0.006(2) -0.004(2) 0.002(2) C8 0.014(3) 0.009(2) 0.012(3) -0.001(2) -0.004(2) -0.003(2) C9 0.019(3) 0.013(2) 0.020(3) -0.006(2) -0.011(2) 0.001(2) C10 0.025(3) 0.016(3) 0.027(3) -0.007(2) -0.014(3) 0.005(2) C11 0.027(3) 0.021(3) 0.037(3) -0.014(3) -0.020(3) 0.012(2) C12 0.018(3) 0.027(3) 0.037(3) -0.018(3) -0.009(3) 0.006(2) C13 0.020(3) 0.021(3) 0.022(3) -0.009(2) -0.006(2) 0.001(2) C14 0.017(3) 0.014(3) 0.019(3) -0.006(2) -0.010(2) 0.000(2) C15 0.041(4) 0.032(4) 0.030(4) -0.013(3) -0.018(3) 0.009(3) C16 0.022(3) 0.021(3) 0.024(3) -0.014(2) -0.010(2) 0.003(2) C17 0.029(4) 0.031(4) 0.066(5) -0.031(4) -0.026(4) 0.011(3) C18 0.019(3) 0.013(3) 0.033(3) -0.006(2) -0.012(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O2 2.278(4) . ? Tb1 O4 2.461(4) . ? Tb1 O3 2.476(4) . ? Tb1 Cl2 2.6973(15) . ? Tb1 O1 2.698(4) . ? Tb1 Cl1 2.7901(14) . ? Tb1 Cl3 2.8212(14) 2_657 ? Tb1 Cl3 2.841(2) . ? Br1 C4 1.887(5) . ? Cl3 Tb1 2.8212(14) 2_657 ? O1 C2 1.360(6) . ? O1 C1 1.420(7) . ? O2 C7 1.301(6) . ? O2 H2A 0.9300 . ? O3 C16 1.420(7) . ? O3 H3B 0.8200 . ? O4 C18 1.431(6) . ? O4 H4A 0.8200 . ? N1 C8 1.328(7) . ? N1 C9 1.368(7) . ? N1 H1A 0.8600 . ? N2 C8 1.329(7) . ? N2 C14 1.367(7) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.368(8) . ? C2 C7 1.400(7) . ? C3 C4 1.393(7) . ? C3 H3A 0.9300 . ? C4 C5 1.348(8) . ? C5 C6 1.416(7) . ? C5 H5A 0.9300 . ? C6 C7 1.388(7) . ? C6 C8 1.426(7) . ? C9 C10 1.374(8) . ? C9 C14 1.381(8) . ? C10 C11 1.361(9) . ? C10 H10A 0.9300 . ? C11 C12 1.404(9) . ? C11 H11A 0.9300 . ? C12 C13 1.355(8) . ? C12 H12A 0.9300 . ? C13 C14 1.374(8) . ? C13 H13A 0.9300 . ? C15 C16 1.468(8) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16B 0.9700 . ? C16 H16A 0.9700 . ? C17 C18 1.480(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9700 . ? C18 H18B 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 O2 Tb1 O4 136.22(12) . . ? O2 Tb1 O3 93.15(13) . . ? O4 Tb1 O3 116.15(13) . . ? O2 Tb1 Cl2 93.50(10) . . ? O4 Tb1 Cl2 79.87(9) . . ? O3 Tb1 Cl2 146.31(10) . . ? O2 Tb1 O1 60.64(12) . . ? O4 Tb1 O1 76.13(12) . . ? O3 Tb1 O1 137.07(12) . . ? Cl2 Tb1 O1 73.55(9) . . ? O2 Tb1 Cl1 86.34(10) . . ? O4 Tb1 Cl1 72.28(9) . . ? O3 Tb1 Cl1 74.81(10) . . ? Cl2 Tb1 Cl1 138.59(5) . . ? O1 Tb1 Cl1 70.46(9) . . ? O2 Tb1 Cl3 73.46(10) . 2_657 ? O4 Tb1 Cl3 145.10(9) . 2_657 ? O3 Tb1 Cl3 69.98(10) . 2_657 ? Cl2 Tb1 Cl3 80.41(5) . 2_657 ? O1 Tb1 Cl3 124.59(8) . 2_657 ? Cl1 Tb1 Cl3 137.87(4) . 2_657 ? O2 Tb1 Cl3 148.19(9) . . ? O4 Tb1 Cl3 74.35(9) . . ? O3 Tb1 Cl3 74.62(10) . . ? Cl2 Tb1 Cl3 82.54(5) . . ? O1 Tb1 Cl3 144.69(8) . . ? Cl1 Tb1 Cl3 117.21(5) . . ? Cl3 Tb1 Cl3 74.76(6) 2_657 . ? Tb1 Cl3 Tb1 105.24(6) 2_657 . ? C2 O1 C1 115.4(4) . . ? C2 O1 Tb1 116.8(3) . . ? C1 O1 Tb1 127.7(3) . . ? C7 O2 Tb1 131.7(3) . . ? C7 O2 H2A 114.1 . . ? Tb1 O2 H2A 114.1 . . ? C16 O3 Tb1 140.6(3) . . ? C16 O3 H3B 109.5 . . ? Tb1 O3 H3B 88.6 . . ? C18 O4 Tb1 129.0(3) . . ? C18 O4 H4A 109.5 . . ? Tb1 O4 H4A 102.4 . . ? C8 N1 C9 108.1(4) . . ? C8 N1 H1A 126.0 . . ? C9 N1 H1A 126.0 . . ? C8 N2 C14 109.1(4) . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O1 C2 C3 125.8(5) . . ? O1 C2 C7 111.8(4) . . ? C3 C2 C7 122.4(5) . . ? C2 C3 C4 118.9(5) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 121.5(5) . . ? C5 C4 Br1 119.8(4) . . ? C3 C4 Br1 118.7(4) . . ? C4 C5 C6 118.9(5) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C7 C6 C5 121.4(5) . . ? C7 C6 C8 117.5(5) . . ? C5 C6 C8 121.1(5) . . ? O2 C7 C6 124.3(5) . . ? O2 C7 C2 118.9(4) . . ? C6 C7 C2 116.8(5) . . ? N1 C8 N2 109.4(5) . . ? N1 C8 C6 126.1(5) . . ? N2 C8 C6 124.5(5) . . ? N1 C9 C10 130.6(5) . . ? N1 C9 C14 107.5(5) . . ? C10 C9 C14 121.8(5) . . ? C11 C10 C9 115.8(6) . . ? C11 C10 H10A 122.1 . . ? C9 C10 H10A 122.1 . . ? C10 C11 C12 122.1(5) . . ? C10 C11 H11A 118.9 . . ? C12 C11 H11A 118.9 . . ? C13 C12 C11 121.9(6) . . ? C13 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? C12 C13 C14 115.8(6) . . ? C12 C13 H13A 122.1 . . ? C14 C13 H13A 122.1 . . ? N2 C14 C13 131.5(5) . . ? N2 C14 C9 105.9(5) . . ? C13 C14 C9 122.6(5) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O3 C16 C15 112.2(5) . . ? O3 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? O3 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? H16B C16 H16A 107.9 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 C17 111.8(5) . . ? O4 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? O4 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.965 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.146 # Attachment '- Complex-2.CIF' data_complex-2 _database_code_depnum_ccdc_archive 'CCDC 777194' #TrackingRef '- Complex-2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H46 Br2 Cl6 Er2 N4 O8' _chemical_formula_sum 'C36 H46 Br2 Cl6 Er2 N4 O8' _chemical_formula_weight 1369.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.201(2) _cell_length_b 11.683(3) _cell_length_c 11.701(2) _cell_angle_alpha 64.80(3) _cell_angle_beta 64.79(4) _cell_angle_gamma 86.63(3) _cell_volume 1128.8(7) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4586 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _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 2.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 662 _exptl_absorpt_coefficient_mu 5.869 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.4181 _exptl_absorpt_correction_T_max 0.5914 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7225 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3949 _reflns_number_gt 3174 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0421P)^2^+4.4376P] 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 3949 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 0.74266(4) 0.06292(3) 0.86465(3) 0.04005(14) Uani 1 1 d U . . Br1 Br 1.31570(9) 0.48052(8) 0.12402(8) 0.0606(3) Uani 1 1 d U . . Cl1 Cl 0.98619(18) 0.15870(15) 0.86767(18) 0.0396(4) Uani 1 1 d U . . Cl2 Cl 0.6822(2) -0.0665(2) 0.74764(19) 0.0490(5) Uani 1 1 d U . . Cl3 Cl 0.53381(18) -0.13539(16) 1.11237(17) 0.0403(4) Uani 1 1 d U . . O1 O 0.9847(5) 0.1135(5) 0.6228(5) 0.0407(12) Uani 1 1 d U . . O2 O 0.7860(5) 0.2525(4) 0.6802(4) 0.0352(11) Uani 1 1 d U . . H2A H 0.7121 0.3026 0.6952 0.042 Uiso 1 1 calc R . . O3 O 0.6466(6) 0.1493(6) 1.0333(6) 0.0620(17) Uani 1 1 d U . . H3B H 0.5816 0.0875 1.0877 0.074 Uiso 1 1 calc R . . O4 O 0.8786(5) -0.1127(4) 0.9260(5) 0.0357(11) Uani 1 1 d U . . H4A H 0.9009 -0.1013 0.9803 0.043 Uiso 1 1 calc R . . N1 N 0.7790(6) 0.6157(5) 0.4022(6) 0.0384(14) Uani 1 1 d U . . H1A H 0.8474 0.6652 0.3208 0.046 Uiso 1 1 calc R . . N2 N 0.6623(6) 0.4520(5) 0.6034(6) 0.0353(14) Uani 1 1 d U . . C1 C 1.0947(9) 0.0333(8) 0.5984(8) 0.058(2) Uani 1 1 d U . . H1B H 1.1106 0.0242 0.5158 0.087 Uiso 1 1 calc R . . H1C H 1.0628 -0.0494 0.6782 0.087 Uiso 1 1 calc R . . H1D H 1.1844 0.0712 0.5846 0.087 Uiso 1 1 calc R . . C2 C 1.0110(7) 0.2336(6) 0.5195(6) 0.0327(16) Uani 1 1 d U . . C3 C 1.1323(7) 0.2850(7) 0.3926(7) 0.0382(17) Uani 1 1 d U . . H3A H 1.2066 0.2368 0.3706 0.046 Uiso 1 1 calc R . . C4 C 1.1434(7) 0.4090(7) 0.2976(7) 0.0384(17) Uani 1 1 d U . . C5 C 1.0349(8) 0.4808(7) 0.3231(7) 0.0377(17) Uani 1 1 d U . . H5A H 1.0437 0.5633 0.2554 0.045 Uiso 1 1 calc R . . C6 C 0.9077(7) 0.4281(6) 0.4545(7) 0.0338(16) Uani 1 1 d U . . C7 C 0.8968(7) 0.3055(6) 0.5547(7) 0.0338(16) Uani 1 1 d U . . C8 C 0.7881(8) 0.4989(6) 0.4852(7) 0.0353(16) Uani 1 1 d U . . C9 C 0.6428(8) 0.6457(6) 0.4665(7) 0.0375(17) Uani 1 1 d U . . C10 C 0.5775(9) 0.7532(7) 0.4229(9) 0.050(2) Uani 1 1 d U . . H10A H 0.6278 0.8237 0.3362 0.060 Uiso 1 1 calc R . . C11 C 0.4368(10) 0.7516(8) 0.5118(9) 0.054(2) Uani 1 1 d U . . H11A H 0.3894 0.8212 0.4839 0.065 Uiso 1 1 calc R . . C12 C 0.3624(9) 0.6476(8) 0.6438(9) 0.054(2) Uani 1 1 d U . . H12A H 0.2674 0.6505 0.7031 0.064 Uiso 1 1 calc R . . C13 C 0.4264(9) 0.5412(7) 0.6880(9) 0.051(2) Uani 1 1 d U . . H13A H 0.3769 0.4719 0.7759 0.062 Uiso 1 1 calc R . . C14 C 0.5693(8) 0.5414(6) 0.5952(7) 0.0362(16) Uani 1 1 d U . . C15 C 0.6870(15) 0.1015(13) 1.2151(18) 0.127(6) Uani 1 1 d U . . H15A H 0.7077 0.1309 1.2716 0.191 Uiso 1 1 calc R . . H15B H 0.7645 0.0577 1.1782 0.191 Uiso 1 1 calc R . . H15C H 0.5961 0.0440 1.2719 0.191 Uiso 1 1 calc R . . C16 C 0.6771(13) 0.1998(12) 1.1103(13) 0.091(3) Uani 1 1 d U . . H16B H 0.7685 0.2587 1.0515 0.110 Uiso 1 1 calc R . . H16A H 0.5992 0.2451 1.1458 0.110 Uiso 1 1 calc R . . C17 C 0.9528(10) -0.3156(10) 0.9262(12) 0.077(3) Uani 1 1 d U . . H17A H 0.9146 -0.4041 0.9658 0.116 Uiso 1 1 calc R . . H17B H 1.0278 -0.3088 0.9529 0.116 Uiso 1 1 calc R . . H17C H 0.9935 -0.2787 0.8254 0.116 Uiso 1 1 calc R . . C18 C 0.8337(9) -0.2468(7) 0.9794(9) 0.052(2) Uani 1 1 d U . . H18A H 0.7571 -0.2569 0.9547 0.062 Uiso 1 1 calc R . . H18B H 0.7921 -0.2861 1.0815 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0356(2) 0.0376(2) 0.02680(19) -0.00972(15) -0.00090(14) 0.00209(14) Br1 0.0451(5) 0.0568(5) 0.0346(4) -0.0152(4) 0.0188(4) -0.0169(4) Cl1 0.0343(9) 0.0283(9) 0.0336(9) -0.0013(7) -0.0069(7) -0.0067(7) Cl2 0.0393(10) 0.0651(13) 0.0374(10) -0.0345(10) -0.0003(8) 0.0034(9) Cl3 0.0309(9) 0.0376(9) 0.0231(8) -0.0017(7) 0.0013(7) 0.0052(7) O1 0.038(3) 0.042(3) 0.022(2) -0.011(2) 0.001(2) 0.008(2) O2 0.030(2) 0.032(2) 0.022(2) -0.009(2) 0.0034(19) 0.0064(19) O3 0.046(3) 0.095(4) 0.050(3) -0.053(3) -0.001(3) -0.013(3) O4 0.032(2) 0.029(2) 0.034(3) -0.011(2) -0.007(2) 0.0031(19) N1 0.044(3) 0.027(3) 0.026(3) -0.007(2) -0.003(3) -0.007(2) N2 0.029(3) 0.031(3) 0.031(3) -0.012(2) -0.002(2) -0.001(2) C1 0.056(5) 0.051(5) 0.033(4) -0.013(4) 0.003(4) 0.022(4) C2 0.031(3) 0.034(4) 0.018(3) -0.012(3) 0.002(3) -0.001(3) C3 0.029(4) 0.039(4) 0.035(4) -0.020(3) 0.000(3) -0.003(3) C4 0.031(4) 0.039(4) 0.026(3) -0.014(3) 0.005(3) -0.011(3) C5 0.044(4) 0.030(3) 0.023(3) -0.010(3) -0.001(3) -0.011(3) C6 0.032(3) 0.034(4) 0.026(3) -0.015(3) -0.002(3) -0.004(3) C7 0.036(4) 0.031(3) 0.024(3) -0.011(3) -0.004(3) -0.004(3) C8 0.039(4) 0.032(4) 0.025(3) -0.008(3) -0.009(3) -0.008(3) C9 0.043(4) 0.030(4) 0.033(4) -0.011(3) -0.013(3) -0.005(3) C10 0.054(5) 0.037(4) 0.046(4) -0.009(3) -0.021(4) 0.003(3) C11 0.061(5) 0.040(4) 0.065(5) -0.019(4) -0.035(4) 0.010(4) C12 0.043(4) 0.050(4) 0.062(5) -0.027(4) -0.016(4) 0.009(3) C13 0.044(4) 0.038(4) 0.055(5) -0.016(4) -0.011(4) 0.002(3) C14 0.037(4) 0.029(3) 0.034(4) -0.013(3) -0.009(3) 0.001(3) C15 0.086(9) 0.082(9) 0.178(16) -0.041(10) -0.044(10) 0.008(7) C16 0.076(6) 0.091(7) 0.086(7) -0.040(6) -0.016(5) 0.003(5) C17 0.056(6) 0.070(6) 0.114(9) -0.054(6) -0.031(6) 0.013(5) C18 0.043(4) 0.035(4) 0.066(5) -0.016(4) -0.022(4) 0.007(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 2.234(4) . ? Er1 O3 2.410(5) . ? Er1 O4 2.431(4) . ? Er1 Cl2 2.671(2) . ? Er1 O1 2.693(5) . ? Er1 Cl1 2.8038(19) . ? Er1 Cl3 2.812(3) . ? Er1 Cl3 2.8303(19) 2_657 ? Br1 C4 1.897(6) . ? Cl3 Er1 2.8303(19) 2_657 ? O1 C2 1.351(8) . ? O1 C1 1.431(9) . ? O2 C7 1.308(7) . ? O2 H2A 0.9300 . ? O3 C16 1.404(13) . ? O3 H3B 0.8200 . ? O4 C18 1.436(9) . ? O4 H4A 0.8200 . ? N1 C8 1.322(9) . ? N1 C9 1.377(9) . ? N1 H1A 0.8600 . ? N2 C8 1.336(8) . ? N2 C14 1.370(9) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.364(9) . ? C2 C7 1.415(9) . ? C3 C4 1.374(10) . ? C3 H3A 0.9300 . ? C4 C5 1.356(10) . ? C5 C6 1.420(9) . ? C5 H5A 0.9300 . ? C6 C7 1.385(9) . ? C6 C8 1.436(10) . ? C9 C14 1.377(9) . ? C9 C10 1.389(10) . ? C10 C11 1.362(12) . ? C10 H10A 0.9300 . ? C11 C12 1.397(11) . ? C11 H11A 0.9300 . ? C12 C13 1.373(11) . ? C12 H12A 0.9300 . ? C13 C14 1.397(10) . ? C13 H13A 0.9300 . ? C15 C16 1.313(17) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16B 0.9700 . ? C16 H16A 0.9700 . ? C17 C18 1.476(12) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9700 . ? C18 H18B 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 O2 Er1 O3 93.8(2) . . ? O2 Er1 O4 136.38(15) . . ? O3 Er1 O4 113.8(2) . . ? O2 Er1 Cl2 93.61(13) . . ? O3 Er1 Cl2 146.70(14) . . ? O4 Er1 Cl2 81.59(13) . . ? O2 Er1 O1 61.93(15) . . ? O3 Er1 O1 137.17(17) . . ? O4 Er1 O1 75.24(15) . . ? Cl2 Er1 O1 73.87(12) . . ? O2 Er1 Cl1 84.70(14) . . ? O3 Er1 Cl1 73.87(14) . . ? O4 Er1 Cl1 72.42(12) . . ? Cl2 Er1 Cl1 139.20(6) . . ? O1 Er1 Cl1 69.47(12) . . ? O2 Er1 Cl3 147.51(12) . . ? O3 Er1 Cl3 74.82(15) . . ? O4 Er1 Cl3 75.01(11) . . ? Cl2 Er1 Cl3 81.67(6) . . ? O1 Er1 Cl3 143.73(11) . . ? Cl1 Er1 Cl3 119.48(6) . . ? O2 Er1 Cl3 73.25(13) . 2_657 ? O3 Er1 Cl3 70.50(15) . 2_657 ? O4 Er1 Cl3 146.34(11) . 2_657 ? Cl2 Er1 Cl3 80.71(6) . 2_657 ? O1 Er1 Cl3 125.92(11) . 2_657 ? Cl1 Er1 Cl3 136.21(6) . 2_657 ? Cl3 Er1 Cl3 74.27(7) . 2_657 ? Er1 Cl3 Er1 105.73(7) . 2_657 ? C2 O1 C1 117.4(5) . . ? C2 O1 Er1 114.9(4) . . ? C1 O1 Er1 127.2(4) . . ? C7 O2 Er1 131.4(4) . . ? C7 O2 H2A 114.3 . . ? Er1 O2 H2A 114.3 . . ? C16 O3 Er1 146.5(6) . . ? C16 O3 H3B 109.5 . . ? Er1 O3 H3B 90.6 . . ? C18 O4 Er1 128.2(4) . . ? C18 O4 H4A 109.5 . . ? Er1 O4 H4A 102.0 . . ? C8 N1 C9 109.2(6) . . ? C8 N1 H1A 125.4 . . ? C9 N1 H1A 125.4 . . ? C8 N2 C14 109.0(6) . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O1 C2 C3 125.8(6) . . ? O1 C2 C7 113.0(5) . . ? C3 C2 C7 121.2(6) . . ? C2 C3 C4 119.2(7) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 122.3(6) . . ? C5 C4 Br1 119.2(5) . . ? C3 C4 Br1 118.5(5) . . ? C4 C5 C6 119.1(6) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C7 C6 C5 119.8(6) . . ? C7 C6 C8 119.0(6) . . ? C5 C6 C8 121.2(6) . . ? O2 C7 C6 123.3(6) . . ? O2 C7 C2 118.3(6) . . ? C6 C7 C2 118.4(6) . . ? N1 C8 N2 108.7(6) . . ? N1 C8 C6 127.2(6) . . ? N2 C8 C6 124.1(6) . . ? N1 C9 C14 106.4(6) . . ? N1 C9 C10 132.0(7) . . ? C14 C9 C10 121.5(7) . . ? C11 C10 C9 117.5(7) . . ? C11 C10 H10A 121.3 . . ? C9 C10 H10A 121.3 . . ? C10 C11 C12 121.4(8) . . ? C10 C11 H11A 119.3 . . ? C12 C11 H11A 119.3 . . ? C13 C12 C11 121.4(8) . . ? C13 C12 H12A 119.3 . . ? C11 C12 H12A 119.3 . . ? C12 C13 C14 117.1(7) . . ? C12 C13 H13A 121.4 . . ? C14 C13 H13A 121.4 . . ? N2 C14 C9 106.7(6) . . ? N2 C14 C13 132.4(7) . . ? C9 C14 C13 120.9(7) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C15 C16 O3 106.0(12) . . ? C15 C16 H16B 110.5 . . ? O3 C16 H16B 110.5 . . ? C15 C16 H16A 110.5 . . ? O3 C16 H16A 110.5 . . ? H16B C16 H16A 108.7 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 C17 114.2(7) . . ? O4 C18 H18A 108.7 . . ? C17 C18 H18A 108.7 . . ? O4 C18 H18B 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.147 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.136 # Attachment '- Complex-3.CIF' data_complex-3 _database_code_depnum_ccdc_archive 'CCDC 777195' #TrackingRef '- Complex-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H38 Br2 Cl6 Gd2 N4 O8' _chemical_formula_sum 'C32 H38 Br2 Cl6 Gd2 N4 O8' _chemical_formula_weight 1293.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.326(3) _cell_length_b 23.037(5) _cell_length_c 7.3627(15) _cell_angle_alpha 90.00 _cell_angle_beta 98.52(3) _cell_angle_gamma 90.00 _cell_volume 2067.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4228 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 5.552 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.4703 _exptl_absorpt_correction_T_max 0.6650 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6822 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3587 _reflns_number_gt 2661 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0835P)^2^+3.7709P] 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 3587 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.2085 _refine_ls_wR_factor_gt 0.1942 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 1.17039(6) -0.03168(3) 0.12971(11) 0.0284(3) Uani 1 1 d U . . Br1 Br 1.45627(13) -0.32305(7) 0.1152(2) 0.0343(4) Uani 1 1 d U . . Cl3 Cl 0.9446(3) -0.05679(17) 0.0910(6) 0.0363(9) Uani 1 1 d U . . Cl2 Cl 1.1482(3) -0.08125(16) -0.2240(5) 0.0348(9) Uani 1 1 d U . . Cl1 Cl 1.3274(4) 0.04499(17) 0.1098(7) 0.0425(10) Uani 1 1 d U . . N1 N 1.0277(10) -0.2911(5) 0.2698(16) 0.025(3) Uani 1 1 d U . . H1A H 1.0599 -0.3242 0.2676 0.030 Uiso 1 1 calc R . . N2 N 0.9979(10) -0.1982(5) 0.2492(17) 0.027(3) Uani 1 1 d U . . O1 O 1.3450(8) -0.1017(4) 0.1241(15) 0.032(2) Uani 1 1 d U . . O2 O 1.1510(9) -0.1254(4) 0.2025(15) 0.032(2) Uani 1 1 d U . . H2A H 1.0870 -0.1336 0.2506 0.038 Uiso 1 1 calc R . . O3 O 1.0890(10) 0.0277(5) 0.3429(16) 0.040(3) Uani 1 1 d U . . H3C H 1.0403 0.0433 0.2716 0.048 Uiso 1 1 calc R . . O4 O 1.2695(9) -0.0422(5) 0.4441(16) 0.039(3) Uani 1 1 d U . . H4B H 1.2173 -0.0382 0.5002 0.046 Uiso 1 1 calc R . . C1 C 1.4508(14) -0.0867(8) 0.088(3) 0.044(4) Uani 1 1 d U . . H1B H 1.4721 -0.1127 -0.0028 0.066 Uiso 1 1 calc R . . H1C H 1.5023 -0.0895 0.1986 0.066 Uiso 1 1 calc R . . H1D H 1.4499 -0.0476 0.0419 0.066 Uiso 1 1 calc R . . C2 C 1.3213(13) -0.1598(6) 0.138(2) 0.028(3) Uani 1 1 d U . . C3 C 1.3908(14) -0.2039(7) 0.118(2) 0.031(4) Uani 1 1 d U . . H3A H 1.4606 -0.1962 0.0902 0.037 Uiso 1 1 calc R . . C4 C 1.3570(12) -0.2617(7) 0.140(2) 0.028(3) Uani 1 1 d U . . C5 C 1.2532(12) -0.2739(7) 0.1809(19) 0.027(3) Uani 1 1 d U . . H5A H 1.2316 -0.3121 0.1951 0.033 Uiso 1 1 calc R . . C6 C 1.1808(11) -0.2278(6) 0.2009(18) 0.022(3) Uani 1 1 d U . . C7 C 1.2149(12) -0.1714(6) 0.1890(19) 0.026(3) Uani 1 1 d U . . C8 C 1.0730(13) -0.2386(7) 0.246(2) 0.027(3) Uani 1 1 d U . . C9 C 0.9172(13) -0.2818(7) 0.298(2) 0.029(3) Uani 1 1 d U . . C10 C 0.8385(12) -0.3201(7) 0.335(2) 0.029(3) Uani 1 1 d U . . H10A H 0.8519 -0.3598 0.3450 0.035 Uiso 1 1 calc R . . C11 C 0.7384(13) -0.2966(7) 0.355(2) 0.034(4) Uani 1 1 d U . . H11A H 0.6823 -0.3212 0.3781 0.040 Uiso 1 1 calc R . . C12 C 0.7180(14) -0.2364(7) 0.340(2) 0.035(4) Uani 1 1 d U . . H12A H 0.6492 -0.2217 0.3530 0.042 Uiso 1 1 calc R . . C13 C 0.8012(13) -0.1992(7) 0.308(2) 0.033(4) Uani 1 1 d U . . H13A H 0.7908 -0.1592 0.3019 0.039 Uiso 1 1 calc R . . C14 C 0.9000(12) -0.2237(6) 0.283(2) 0.025(3) Uani 1 1 d U . . C15 C 1.1337(19) 0.0667(9) 0.470(3) 0.060(6) Uani 1 1 d U . . H15A H 1.0767 0.0905 0.5064 0.091 Uiso 1 1 calc R . . H15B H 1.1849 0.0908 0.4179 0.091 Uiso 1 1 calc R . . H15C H 1.1711 0.0466 0.5749 0.091 Uiso 1 1 calc R . . C16 C 1.3648(17) -0.0189(10) 0.549(3) 0.060(6) Uani 1 1 d U . . H16A H 1.3756 -0.0364 0.6687 0.090 Uiso 1 1 calc R . . H16B H 1.3565 0.0223 0.5609 0.090 Uiso 1 1 calc R . . H16C H 1.4272 -0.0268 0.4888 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0264(4) 0.0220(4) 0.0384(5) 0.0018(3) 0.0100(3) -0.0014(3) Br1 0.0319(9) 0.0348(9) 0.0368(8) 0.0000(7) 0.0069(7) 0.0077(7) Cl3 0.029(2) 0.0261(19) 0.055(2) 0.0033(17) 0.0085(18) -0.0043(16) Cl2 0.036(2) 0.0288(19) 0.042(2) -0.0020(16) 0.0131(17) -0.0002(17) Cl1 0.035(2) 0.030(2) 0.065(3) 0.0051(19) 0.017(2) -0.0034(17) N1 0.030(6) 0.017(5) 0.030(6) 0.000(4) 0.007(5) 0.001(5) N2 0.022(6) 0.030(6) 0.030(5) 0.006(5) 0.009(5) -0.006(5) O1 0.025(5) 0.029(5) 0.044(5) -0.001(4) 0.013(4) 0.002(4) O2 0.030(5) 0.025(5) 0.042(5) 0.004(4) 0.012(4) 0.004(4) O3 0.038(6) 0.043(6) 0.040(5) 0.000(5) 0.011(5) 0.007(5) O4 0.032(5) 0.037(5) 0.048(6) 0.002(5) 0.010(5) -0.001(5) C1 0.039(8) 0.045(8) 0.049(8) 0.003(6) 0.015(6) -0.002(6) C2 0.029(7) 0.026(6) 0.029(6) 0.002(5) 0.003(5) -0.007(6) C3 0.031(7) 0.037(7) 0.027(6) -0.007(5) 0.011(6) 0.004(6) C4 0.027(7) 0.033(7) 0.024(6) -0.003(5) 0.003(5) 0.002(6) C5 0.026(7) 0.028(6) 0.029(6) -0.007(5) 0.006(5) -0.002(5) C6 0.020(6) 0.027(6) 0.018(5) 0.004(5) -0.002(5) -0.003(5) C7 0.023(6) 0.029(6) 0.026(6) 0.004(5) 0.000(5) 0.004(5) C8 0.027(7) 0.032(6) 0.022(6) -0.007(5) 0.000(5) -0.002(6) C9 0.031(7) 0.028(6) 0.029(6) -0.006(5) 0.006(5) -0.003(6) C10 0.024(7) 0.030(7) 0.034(7) 0.003(5) 0.008(5) -0.005(6) C11 0.029(7) 0.040(7) 0.030(6) -0.003(6) -0.001(6) -0.005(6) C12 0.028(7) 0.040(7) 0.035(7) 0.000(6) 0.000(6) 0.006(6) C13 0.037(7) 0.028(7) 0.033(6) -0.002(6) 0.005(6) 0.006(6) C14 0.019(6) 0.027(6) 0.029(6) -0.002(5) 0.002(5) 0.000(5) C15 0.070(9) 0.052(9) 0.059(9) -0.001(7) 0.009(7) 0.003(7) C16 0.051(9) 0.063(9) 0.064(9) 0.007(7) 0.002(7) -0.005(7) _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 2.247(10) . ? Gd1 O3 2.410(11) . ? Gd1 O4 2.464(12) . ? Gd1 Cl1 2.640(4) . ? Gd1 O1 2.695(10) . ? Gd1 Cl3 2.816(4) . ? Gd1 Cl2 2.820(4) . ? Gd1 Cl3 2.850(4) 3_755 ? Br1 C4 1.896(15) . ? Cl3 Gd1 2.850(4) 3_755 ? N1 C8 1.353(19) . ? N1 C9 1.43(2) . ? N1 H1A 0.8600 . ? N2 C8 1.32(2) . ? N2 C14 1.398(19) . ? O1 C2 1.378(18) . ? O1 C1 1.413(19) . ? O2 C7 1.332(18) . ? O2 H2A 0.9300 . ? O3 C15 1.35(2) . ? O3 H3C 0.8200 . ? O4 C16 1.41(2) . ? O4 H4B 0.8200 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.35(2) . ? C2 C7 1.44(2) . ? C3 C4 1.41(2) . ? C3 H3A 0.9300 . ? C4 C5 1.39(2) . ? C5 C6 1.41(2) . ? C5 H5A 0.9300 . ? C6 C7 1.37(2) . ? C6 C8 1.44(2) . ? C9 C14 1.36(2) . ? C9 C10 1.37(2) . ? C10 C11 1.38(2) . ? C10 H10A 0.9300 . ? C11 C12 1.41(2) . ? C11 H11A 0.9300 . ? C12 C13 1.38(2) . ? C12 H12A 0.9300 . ? C13 C14 1.38(2) . ? C13 H13A 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O3 108.7(4) . . ? O2 Gd1 O4 74.8(4) . . ? O3 Gd1 O4 68.9(4) . . ? O2 Gd1 Cl1 139.6(3) . . ? O3 Gd1 Cl1 92.1(3) . . ? O4 Gd1 Cl1 81.5(3) . . ? O2 Gd1 O1 62.7(3) . . ? O3 Gd1 O1 139.5(4) . . ? O4 Gd1 O1 70.7(4) . . ? Cl1 Gd1 O1 78.8(2) . . ? O2 Gd1 Cl3 71.8(3) . . ? O3 Gd1 Cl3 71.4(3) . . ? O4 Gd1 Cl3 114.8(3) . . ? Cl1 Gd1 Cl3 148.60(13) . . ? O1 Gd1 Cl3 130.9(2) . . ? O2 Gd1 Cl2 80.3(3) . . ? O3 Gd1 Cl2 147.0(3) . . ? O4 Gd1 Cl2 142.6(3) . . ? Cl1 Gd1 Cl2 101.03(14) . . ? O1 Gd1 Cl2 73.3(3) . . ? Cl3 Gd1 Cl2 82.18(12) . . ? O2 Gd1 Cl3 139.7(3) . 3_755 ? O3 Gd1 Cl3 75.3(3) . 3_755 ? O4 Gd1 Cl3 137.8(3) . 3_755 ? Cl1 Gd1 Cl3 78.26(13) . 3_755 ? O1 Gd1 Cl3 138.6(2) . 3_755 ? Cl3 Gd1 Cl3 71.85(13) . 3_755 ? Cl2 Gd1 Cl3 77.93(12) . 3_755 ? Gd1 Cl3 Gd1 108.15(13) . 3_755 ? C8 N1 C9 107.8(12) . . ? C8 N1 H1A 126.1 . . ? C9 N1 H1A 126.1 . . ? C8 N2 C14 109.4(12) . . ? C2 O1 C1 117.7(12) . . ? C2 O1 Gd1 113.7(9) . . ? C1 O1 Gd1 128.2(10) . . ? C7 O2 Gd1 131.4(9) . . ? C7 O2 H2A 114.3 . . ? Gd1 O2 H2A 114.3 . . ? C15 O3 Gd1 131.3(12) . . ? C15 O3 H3C 109.5 . . ? Gd1 O3 H3C 99.7 . . ? C16 O4 Gd1 137.2(11) . . ? C16 O4 H4B 109.5 . . ? Gd1 O4 H4B 98.4 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C3 C2 O1 125.2(14) . . ? C3 C2 C7 120.5(14) . . ? O1 C2 C7 114.3(13) . . ? C2 C3 C4 119.6(15) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 120.9(14) . . ? C5 C4 Br1 119.9(12) . . ? C3 C4 Br1 119.2(11) . . ? C4 C5 C6 119.3(14) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C7 C6 C5 120.2(13) . . ? C7 C6 C8 118.7(14) . . ? C5 C6 C8 121.0(13) . . ? O2 C7 C6 123.9(14) . . ? O2 C7 C2 116.3(13) . . ? C6 C7 C2 119.3(13) . . ? N2 C8 N1 109.1(13) . . ? N2 C8 C6 123.8(14) . . ? N1 C8 C6 126.6(14) . . ? C14 C9 C10 123.1(15) . . ? C14 C9 N1 106.1(13) . . ? C10 C9 N1 130.7(14) . . ? C9 C10 C11 116.1(15) . . ? C9 C10 H10A 122.0 . . ? C11 C10 H10A 122.0 . . ? C10 C11 C12 122.2(16) . . ? C10 C11 H11A 118.9 . . ? C12 C11 H11A 118.9 . . ? C13 C12 C11 119.5(16) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C14 C13 C12 117.4(15) . . ? C14 C13 H13A 121.3 . . ? C12 C13 H13A 121.3 . . ? C9 C14 C13 121.6(14) . . ? C9 C14 N2 107.5(13) . . ? C13 C14 N2 130.8(14) . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O4 C16 H16A 109.5 . . ? O4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.857 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.279 # Attachment '- Complex-4.CIF' data_complex-4 _database_code_depnum_ccdc_archive 'CCDC 777196' #TrackingRef '- Complex-4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H38 Br2 Cl6 N4 O8 Yb2' _chemical_formula_sum 'C32 H38 Br2 Cl6 N4 O8 Yb2' _chemical_formula_weight 1325.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5470(19) _cell_length_b 11.510(2) _cell_length_c 11.745(2) _cell_angle_alpha 64.26(3) _cell_angle_beta 67.15(4) _cell_angle_gamma 85.79(3) _cell_volume 1064.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 2941 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634 _exptl_absorpt_coefficient_mu 6.671 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.3797 _exptl_absorpt_correction_T_max 0.5551 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5858 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0961 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3734 _reflns_number_gt 2685 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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^)+(0.0492P)^2^+3.7371P] 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 3734 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.75261(6) 0.43616(5) 0.14172(5) 0.02876(19) Uani 1 1 d U . . Br1 Br 0.20834(13) 0.00667(10) 0.87988(11) 0.0333(3) Uani 1 1 d U . . Cl1 Cl 0.4852(3) 0.3436(2) 0.1473(2) 0.0213(5) Uani 1 1 d U . . Cl2 Cl 0.8347(3) 0.5648(2) 0.2530(2) 0.0235(6) Uani 1 1 d U . . Cl3 Cl 1.0486(3) 0.3576(2) 0.1053(2) 0.0207(5) Uani 1 1 d U . . N1 N 0.7615(9) -0.1274(8) 0.5853(8) 0.0195(19) Uani 1 1 d U . . H1A H 0.6980 -0.1770 0.6673 0.023 Uiso 1 1 calc R . . N2 N 0.8617(9) 0.0381(8) 0.3871(8) 0.0187(18) Uani 1 1 d U . . O1 O 0.5130(7) 0.3858(6) 0.3845(6) 0.0206(16) Uani 1 1 d U . . O2 O 0.7211(7) 0.2432(6) 0.3206(6) 0.0171(15) Uani 1 1 d U . . H2A H 0.7987 0.1918 0.3027 0.021 Uiso 1 1 calc R . . O3 O 0.8338(8) 0.3548(6) -0.0303(7) 0.0240(16) Uani 1 1 d U . . H3C H 0.9219 0.3904 -0.0727 0.029 Uiso 1 1 calc R . . O4 O 0.6009(7) 0.6155(6) 0.0911(7) 0.0222(16) Uani 1 1 d U . . H4B H 0.5880 0.6142 0.0265 0.027 Uiso 1 1 calc R . . C1 C 0.3917(12) 0.4637(10) 0.4113(10) 0.028(3) Uani 1 1 d U . . H1B H 0.3738 0.4674 0.4959 0.042 Uiso 1 1 calc R . . H1C H 0.3002 0.4261 0.4188 0.042 Uiso 1 1 calc R . . H1D H 0.4199 0.5499 0.3372 0.042 Uiso 1 1 calc R . . C2 C 0.4953(11) 0.2633(9) 0.4843(9) 0.017(2) Uani 1 1 d U . . C3 C 0.3761(11) 0.2093(9) 0.6134(10) 0.019(2) Uani 1 1 d U . . H3A H 0.2972 0.2573 0.6377 0.023 Uiso 1 1 calc R . . C4 C 0.3761(11) 0.0828(10) 0.7057(10) 0.022(2) Uani 1 1 d U . . C5 C 0.4917(11) 0.0096(9) 0.6745(9) 0.019(2) Uani 1 1 d U . . H5A H 0.4905 -0.0742 0.7391 0.023 Uiso 1 1 calc R . . C6 C 0.6117(10) 0.0629(8) 0.5441(9) 0.015(2) Uani 1 1 d U . . C7 C 0.6157(11) 0.1886(9) 0.4446(9) 0.017(2) Uani 1 1 d U . . C8 C 0.7417(11) -0.0087(9) 0.5071(9) 0.017(2) Uani 1 1 d U . . C9 C 0.9013(11) -0.1597(9) 0.5140(10) 0.020(2) Uani 1 1 d U . . C10 C 0.9770(12) -0.2708(10) 0.5501(11) 0.030(3) Uani 1 1 d U . . H10A H 0.9352 -0.3423 0.6357 0.036 Uiso 1 1 calc R . . C11 C 1.1170(12) -0.2678(10) 0.4514(11) 0.028(3) Uani 1 1 d U . . H11A H 1.1719 -0.3389 0.4712 0.033 Uiso 1 1 calc R . . C12 C 1.1780(12) -0.1617(11) 0.3238(11) 0.032(3) Uani 1 1 d U . . H12A H 1.2721 -0.1648 0.2601 0.038 Uiso 1 1 calc R . . C13 C 1.1059(12) -0.0523(11) 0.2870(11) 0.028(3) Uani 1 1 d U . . H13A H 1.1489 0.0187 0.2012 0.034 Uiso 1 1 calc R . . C14 C 0.9637(11) -0.0539(10) 0.3862(10) 0.021(2) Uani 1 1 d U . . C15 C 0.7770(14) 0.3524(13) -0.1229(12) 0.041(3) Uani 1 1 d U . . H15A H 0.8442 0.3112 -0.1757 0.061 Uiso 1 1 calc R . . H15B H 0.7711 0.4396 -0.1837 0.061 Uiso 1 1 calc R . . H15C H 0.6769 0.3046 -0.0727 0.061 Uiso 1 1 calc R . . C16 C 0.6310(13) 0.7474(10) 0.0634(12) 0.033(3) Uani 1 1 d U . . H16A H 0.5484 0.7947 0.0466 0.050 Uiso 1 1 calc R . . H16B H 0.7247 0.7867 -0.0162 0.050 Uiso 1 1 calc R . . H16C H 0.6400 0.7491 0.1413 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.0268(3) 0.0299(3) 0.0258(3) -0.0138(2) -0.0054(2) 0.0052(2) Br1 0.0295(6) 0.0287(6) 0.0225(6) -0.0110(5) 0.0096(5) -0.0048(5) Cl1 0.0193(13) 0.0187(12) 0.0194(12) -0.0055(10) -0.0040(11) -0.0018(10) Cl2 0.0198(13) 0.0328(14) 0.0220(13) -0.0200(11) -0.0036(11) 0.0046(11) Cl3 0.0168(12) 0.0230(13) 0.0160(12) -0.0077(10) -0.0021(10) 0.0052(10) N1 0.019(4) 0.023(4) 0.012(4) -0.009(3) 0.000(3) 0.002(3) N2 0.016(4) 0.021(4) 0.018(4) -0.012(3) -0.003(3) 0.004(3) O1 0.021(4) 0.024(4) 0.012(3) -0.010(3) -0.001(3) 0.010(3) O2 0.016(3) 0.019(3) 0.013(3) -0.009(3) 0.000(3) 0.005(3) O3 0.019(4) 0.030(4) 0.024(4) -0.017(3) -0.004(3) 0.001(3) O4 0.022(4) 0.025(4) 0.020(3) -0.011(3) -0.007(3) 0.006(3) C1 0.027(5) 0.023(5) 0.024(5) -0.009(4) -0.004(4) 0.012(4) C2 0.017(5) 0.027(5) 0.013(4) -0.013(4) -0.008(4) 0.004(4) C3 0.017(5) 0.021(5) 0.021(5) -0.014(4) -0.005(4) 0.006(4) C4 0.021(5) 0.025(5) 0.015(5) -0.005(4) -0.005(4) -0.002(4) C5 0.024(5) 0.014(5) 0.011(4) -0.002(4) -0.003(4) -0.002(4) C6 0.015(5) 0.012(4) 0.019(5) -0.008(4) -0.006(4) -0.003(4) C7 0.014(5) 0.022(5) 0.018(5) -0.014(4) 0.000(4) -0.002(4) C8 0.013(5) 0.020(5) 0.012(4) -0.006(4) 0.001(4) -0.003(4) C9 0.024(5) 0.021(5) 0.023(5) -0.016(4) -0.010(4) 0.003(4) C10 0.033(6) 0.024(5) 0.029(5) -0.009(4) -0.011(5) 0.005(4) C11 0.029(5) 0.026(5) 0.040(6) -0.021(4) -0.019(5) 0.012(4) C12 0.021(5) 0.041(6) 0.029(5) -0.025(5) 0.004(4) 0.006(4) C13 0.025(5) 0.033(6) 0.029(5) -0.019(4) -0.007(4) 0.005(4) C14 0.021(5) 0.030(5) 0.020(5) -0.016(4) -0.009(4) 0.004(4) C15 0.036(6) 0.058(7) 0.034(6) -0.029(5) -0.009(5) 0.004(5) C16 0.031(6) 0.025(5) 0.042(6) -0.018(4) -0.011(5) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O2 2.234(6) . ? Yb1 O4 2.424(6) . ? Yb1 O3 2.425(6) . ? Yb1 Cl2 2.676(3) . ? Yb1 O1 2.719(6) . ? Yb1 Cl1 2.804(3) . ? Yb1 Cl3 2.830(2) . ? Yb1 Cl3 2.839(3) 2_765 ? Br1 C4 1.904(10) . ? Cl3 Yb1 2.839(3) 2_765 ? N1 C8 1.324(12) . ? N1 C9 1.397(12) . ? N1 H1A 0.8600 . ? N2 C8 1.329(11) . ? N2 C14 1.386(12) . ? O1 C2 1.356(11) . ? O1 C1 1.433(11) . ? O2 C7 1.300(11) . ? O2 H2A 0.9300 . ? O3 C15 1.401(13) . ? O3 H3C 0.8200 . ? O4 C16 1.435(12) . ? O4 H4B 0.8200 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.388(13) . ? C2 C7 1.436(13) . ? C3 C4 1.387(13) . ? C3 H3A 0.9300 . ? C4 C5 1.371(14) . ? C5 C6 1.399(13) . ? C5 H5A 0.9300 . ? C6 C7 1.402(13) . ? C6 C8 1.466(13) . ? C9 C14 1.384(13) . ? C9 C10 1.403(14) . ? C10 C11 1.378(15) . ? C10 H10A 0.9300 . ? C11 C12 1.384(15) . ? C11 H11A 0.9300 . ? C12 C13 1.370(15) . ? C12 H12A 0.9300 . ? C13 C14 1.399(14) . ? C13 H13A 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Yb1 O4 135.5(2) . . ? O2 Yb1 O3 95.7(2) . . ? O4 Yb1 O3 112.5(2) . . ? O2 Yb1 Cl2 93.48(17) . . ? O4 Yb1 Cl2 81.35(17) . . ? O3 Yb1 Cl2 146.99(17) . . ? O2 Yb1 O1 61.8(2) . . ? O4 Yb1 O1 74.5(2) . . ? O3 Yb1 O1 137.5(2) . . ? Cl2 Yb1 O1 74.01(16) . . ? O2 Yb1 Cl1 84.63(18) . . ? O4 Yb1 Cl1 72.23(17) . . ? O3 Yb1 Cl1 73.49(17) . . ? Cl2 Yb1 Cl1 139.07(8) . . ? O1 Yb1 Cl1 69.17(16) . . ? O2 Yb1 Cl3 73.82(17) . . ? O4 Yb1 Cl3 146.84(17) . . ? O3 Yb1 Cl3 70.64(17) . . ? Cl2 Yb1 Cl3 81.72(8) . . ? O1 Yb1 Cl3 127.01(15) . . ? Cl1 Yb1 Cl3 135.53(7) . . ? O2 Yb1 Cl3 149.22(17) . 2_765 ? O4 Yb1 Cl3 74.06(16) . 2_765 ? O3 Yb1 Cl3 74.41(17) . 2_765 ? Cl2 Yb1 Cl3 81.57(8) . 2_765 ? O1 Yb1 Cl3 142.49(14) . 2_765 ? Cl1 Yb1 Cl3 118.69(8) . 2_765 ? Cl3 Yb1 Cl3 75.40(8) . 2_765 ? Yb1 Cl3 Yb1 104.60(8) . 2_765 ? C8 N1 C9 109.4(8) . . ? C8 N1 H1A 125.3 . . ? C9 N1 H1A 125.3 . . ? C8 N2 C14 109.6(8) . . ? C2 O1 C1 116.8(7) . . ? C2 O1 Yb1 114.4(5) . . ? C1 O1 Yb1 127.9(5) . . ? C7 O2 Yb1 132.6(6) . . ? C7 O2 H2A 113.7 . . ? Yb1 O2 H2A 113.7 . . ? C15 O3 Yb1 135.0(6) . . ? C15 O3 H3C 109.5 . . ? Yb1 O3 H3C 97.8 . . ? C16 O4 Yb1 129.8(6) . . ? C16 O4 H4B 109.5 . . ? Yb1 O4 H4B 100.5 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O1 C2 C3 126.1(8) . . ? O1 C2 C7 113.1(8) . . ? C3 C2 C7 120.7(9) . . ? C4 C3 C2 119.2(9) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C5 C4 C3 122.1(9) . . ? C5 C4 Br1 118.7(7) . . ? C3 C4 Br1 119.1(7) . . ? C4 C5 C6 119.0(9) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C5 C6 C7 121.6(8) . . ? C5 C6 C8 121.4(8) . . ? C7 C6 C8 116.9(8) . . ? O2 C7 C6 125.0(8) . . ? O2 C7 C2 117.8(8) . . ? C6 C7 C2 117.2(8) . . ? N1 C8 N2 108.7(8) . . ? N1 C8 C6 126.9(8) . . ? N2 C8 C6 124.4(8) . . ? C14 C9 N1 105.9(8) . . ? C14 C9 C10 121.7(9) . . ? N1 C9 C10 132.4(9) . . ? C11 C10 C9 116.1(10) . . ? C11 C10 H10A 121.9 . . ? C9 C10 H10A 121.9 . . ? C10 C11 C12 121.7(10) . . ? C10 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? C13 C12 C11 123.0(10) . . ? C13 C12 H12A 118.5 . . ? C11 C12 H12A 118.5 . . ? C12 C13 C14 116.0(10) . . ? C12 C13 H13A 122.0 . . ? C14 C13 H13A 122.0 . . ? C9 C14 N2 106.3(8) . . ? C9 C14 C13 121.6(9) . . ? N2 C14 C13 132.1(9) . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O4 C16 H16A 109.5 . . ? O4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.754 _refine_diff_density_min -1.156 _refine_diff_density_rms 0.226 # Attachment '- Complex-5.CIF' data_complex-5 _database_code_depnum_ccdc_archive 'CCDC 777197' #TrackingRef '- Complex-5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H26 Br2 Cl3 Eu N4 O5, 2(O)' _chemical_formula_sum 'C29 H26 Br2 Cl3 Eu N4 O7' _chemical_formula_weight 960.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7927(18) _cell_length_b 18.011(4) _cell_length_c 26.437(5) _cell_angle_alpha 93.16(3) _cell_angle_beta 94.13(4) _cell_angle_gamma 92.89(3) _cell_volume 4163.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 13017 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 3.660 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5588 _exptl_absorpt_correction_T_max 0.8103 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24249 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.2276 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14396 _reflns_number_gt 5930 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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. Hydrogen atoms of water molecules were not added. ; _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^)+(0.0945P)^2^+3.6836P] 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 14396 _refine_ls_number_parameters 842 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1730 _refine_ls_R_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.1951 _refine_ls_wR_factor_gt 0.1697 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.96024(10) 0.73546(5) 0.02588(3) 0.0479(3) Uani 1 1 d U . . Br1 Br 1.0755(2) 0.40465(11) 0.19072(7) 0.0642(6) Uani 1 1 d U . . Br1' Br 0.9537(4) 1.02475(14) -0.18609(9) 0.1066(10) Uani 1 1 d U . . Cl1 Cl 0.7701(5) 0.6382(3) -0.03140(17) 0.0590(12) Uani 1 1 d U . . Cl2 Cl 1.2238(5) 0.7749(2) 0.08836(16) 0.0570(12) Uani 1 1 d U . . Cl3 Cl 0.7189(5) 0.8136(2) 0.06343(17) 0.0593(13) Uani 1 1 d U . . O1 O 1.0663(13) 0.6000(6) 0.0484(4) 0.054(3) Uani 1 1 d U . . O2 O 0.8944(12) 0.6848(6) 0.0977(4) 0.049(3) Uani 1 1 d U . . H2B H 0.8327 0.7143 0.1166 0.059 Uiso 1 1 calc R . . O3 O 1.1544(13) 0.7053(6) -0.0311(4) 0.054(3) Uani 1 1 d U . . H3B H 1.2007 0.7453 -0.0230 0.065 Uiso 1 1 calc R . . O1' O 0.8381(14) 0.7972(7) -0.0761(4) 0.060(3) Uani 1 1 d U . . O2' O 1.0226(13) 0.8510(6) -0.0001(4) 0.060(3) Uani 1 1 d U . . H2'B H 1.0745 0.8801 0.0265 0.072 Uiso 1 1 calc R . . N1 N 0.7100(15) 0.6441(7) 0.2349(5) 0.046(4) Uani 1 1 d U . . H1A H 0.7215 0.6072 0.2539 0.055 Uiso 1 1 calc R . . N2 N 0.7234(15) 0.7132(7) 0.1697(5) 0.044(3) Uani 1 1 d U . . N1' N 1.2982(16) 1.0448(8) -0.0010(5) 0.058(4) Uani 1 1 d U . . H1'A H 1.2945 1.0786 -0.0227 0.070 Uiso 1 1 calc R . . N2' N 1.2521(16) 0.9431(8) 0.0371(5) 0.050(4) Uani 1 1 d U . . C1 C 1.171(2) 0.5565(9) 0.0219(6) 0.053(5) Uani 1 1 d U . . H1B H 1.1237 0.5080 0.0124 0.080 Uiso 1 1 calc R . . H1C H 1.2615 0.5516 0.0436 0.080 Uiso 1 1 calc R . . H1D H 1.1966 0.5806 -0.0080 0.080 Uiso 1 1 calc R . . C2 C 1.0218(18) 0.5728(9) 0.0931(6) 0.039(4) Uani 1 1 d U . . C3 C 1.0573(19) 0.5099(9) 0.1135(6) 0.042(4) Uani 1 1 d U . . H3A H 1.1189 0.4774 0.0970 0.051 Uiso 1 1 calc R . . C4 C 1.0037(18) 0.4926(9) 0.1590(6) 0.043(4) Uani 1 1 d U . . C5 C 0.914(2) 0.5361(10) 0.1852(6) 0.052(5) Uani 1 1 d U . . H5A H 0.8811 0.5228 0.2163 0.062 Uiso 1 1 calc R . . C6 C 0.8700(18) 0.6026(8) 0.1640(6) 0.040(4) Uani 1 1 d U . . C7 C 0.925(2) 0.6235(10) 0.1179(6) 0.049(4) Uani 1 1 d U . . C8 C 0.7718(19) 0.6516(9) 0.1896(6) 0.043(4) Uani 1 1 d U . . C9 C 0.627(2) 0.7040(10) 0.2452(6) 0.051(5) Uani 1 1 d U . . C10 C 0.539(2) 0.7213(11) 0.2856(7) 0.068(6) Uani 1 1 d U . . H10C H 0.5279 0.6899 0.3119 0.081 Uiso 1 1 calc R . . C11 C 0.471(2) 0.7872(11) 0.2838(7) 0.063(5) Uani 1 1 d U . . H11B H 0.4160 0.8020 0.3111 0.076 Uiso 1 1 calc R . . C12 C 0.477(2) 0.8345(11) 0.2431(7) 0.062(5) Uani 1 1 d U . . H12A H 0.4293 0.8794 0.2441 0.075 Uiso 1 1 calc R . . C13 C 0.558(2) 0.8131(10) 0.2007(7) 0.058(5) Uani 1 1 d U . . H13A H 0.5594 0.8412 0.1722 0.069 Uiso 1 1 calc R . . C14 C 0.631(2) 0.7502(10) 0.2038(6) 0.048(4) Uani 1 1 d U . . C15 C 1.146(2) 0.6927(11) -0.0846(7) 0.071(6) Uani 1 1 d U . . H1WA H 1.2458 0.6830 -0.0952 0.106 Uiso 1 1 calc R . . H1WB H 1.1099 0.7359 -0.1003 0.106 Uiso 1 1 calc R . . H1WC H 1.0773 0.6505 -0.0945 0.106 Uiso 1 1 calc R . . C1' C 0.744(2) 0.7672(10) -0.1181(7) 0.062(5) Uani 1 1 d U . . H1'B H 0.7972 0.7709 -0.1484 0.093 Uiso 1 1 calc R . . H1'C H 0.6528 0.7944 -0.1213 0.093 Uiso 1 1 calc R . . H1'D H 0.7169 0.7159 -0.1134 0.093 Uiso 1 1 calc R . . C2' C 0.911(2) 0.8637(10) -0.0827(7) 0.054(5) Uani 1 1 d U . . C3' C 0.896(2) 0.9034(11) -0.1255(8) 0.071(6) Uani 1 1 d U . . H3'A H 0.8296 0.8868 -0.1532 0.086 Uiso 1 1 calc R . . C4' C 0.985(2) 0.9694(10) -0.1259(7) 0.056(5) Uani 1 1 d U . . C5' C 1.079(2) 0.9985(11) -0.0892(7) 0.061(5) Uani 1 1 d U . . H5'A H 1.1286 1.0448 -0.0917 0.074 Uiso 1 1 calc R . . C6' C 1.104(2) 0.9572(9) -0.0442(6) 0.048(4) Uani 1 1 d U . . C7' C 1.008(2) 0.8896(11) -0.0411(7) 0.065(5) Uani 1 1 d U . . C8' C 1.2124(19) 0.9811(9) -0.0045(6) 0.047(4) Uani 1 1 d U . . C9' C 1.394(2) 1.0479(11) 0.0431(8) 0.067(5) Uani 1 1 d U . . C10' C 1.502(2) 1.1016(11) 0.0649(7) 0.065(5) Uani 1 1 d U . . H10A H 1.5185 1.1462 0.0495 0.078 Uiso 1 1 calc R . . C11' C 1.585(2) 1.0883(11) 0.1099(7) 0.071(6) Uani 1 1 d U . . H11D H 1.6596 1.1226 0.1247 0.085 Uiso 1 1 calc R . . C12' C 1.550(3) 1.0198(12) 0.1329(8) 0.080(6) Uani 1 1 d U . . H12C H 1.6023 1.0116 0.1638 0.095 Uiso 1 1 calc R . . C13' C 1.444(2) 0.9649(11) 0.1118(7) 0.069(6) Uani 1 1 d U . . H13D H 1.4253 0.9203 0.1271 0.082 Uiso 1 1 calc R . . C14' C 1.370(2) 0.9814(10) 0.0667(7) 0.056(5) Uani 1 1 d U . . Eu2 Eu 0.44443(12) 0.42473(6) 0.31845(4) 0.0624(4) Uani 1 1 d U . . Br1M Br 0.5049(5) 0.26457(18) 0.58417(10) 0.1528(15) Uani 1 1 d U . . Br1N Br 0.5930(2) 0.55413(12) 0.05738(7) 0.0649(6) Uani 1 1 d U . . Cl1M Cl 0.2715(7) 0.3093(3) 0.2742(2) 0.0861(17) Uani 1 1 d U . . Cl2M Cl 0.7058(6) 0.5218(3) 0.31831(17) 0.0665(14) Uani 1 1 d U . . Cl3M Cl 0.1987(6) 0.5014(3) 0.35591(18) 0.0757(15) Uani 1 1 d U . . O1M O 0.3500(17) 0.3246(8) 0.3962(5) 0.082(4) Uani 1 1 d U . . O2M O 0.5305(15) 0.4432(7) 0.4016(4) 0.071(4) Uani 1 1 d U . . H2MA H 0.5848 0.4888 0.4074 0.085 Uiso 1 1 calc R . . O1N O 0.5362(13) 0.4091(7) 0.2241(4) 0.060(3) Uani 1 1 d U . . O2N O 0.3676(13) 0.5054(6) 0.2618(4) 0.057(3) Uani 1 1 d U . . H2NB H 0.2915 0.5358 0.2718 0.069 Uiso 1 1 calc R . . O3' O 0.6415(16) 0.3368(7) 0.3208(5) 0.096(4) Uani 1 1 d U . . H1BB H 0.7297 0.3509 0.3055 0.144 Uiso 1 1 calc R . . N1M N 0.8078(19) 0.5244(9) 0.5281(6) 0.070(5) Uani 1 1 d U . . H1MA H 0.8080 0.5101 0.5586 0.084 Uiso 1 1 calc R . . N2M N 0.7501(18) 0.5319(9) 0.4485(5) 0.063(4) Uani 1 1 d U . . N1N N 0.2129(15) 0.6905(7) 0.1929(5) 0.045(3) Uani 1 1 d U . . H1NA H 0.2282 0.7053 0.1632 0.053 Uiso 1 1 calc R . . N2N N 0.2151(16) 0.6229(8) 0.2578(5) 0.050(4) Uani 1 1 d U . . C1M C 0.249(3) 0.2592(13) 0.3902(9) 0.098(8) Uani 1 1 d U . . H1MB H 0.1803 0.2599 0.4167 0.147 Uiso 1 1 calc R . . H1MC H 0.3079 0.2158 0.3920 0.147 Uiso 1 1 calc R . . H1MD H 0.1920 0.2581 0.3578 0.147 Uiso 1 1 calc R . . C2M C 0.432(2) 0.3421(11) 0.4407(7) 0.062(5) Uani 1 1 d U . . C3M C 0.416(3) 0.2975(12) 0.4823(8) 0.081(6) Uani 1 1 d U . . H3MA H 0.3512 0.2551 0.4816 0.097 Uiso 1 1 calc R . . C4M C 0.513(3) 0.3257(12) 0.5257(7) 0.077(6) Uani 1 1 d U . . C5M C 0.605(3) 0.3856(13) 0.5294(8) 0.083(6) Uani 1 1 d U . . H5MA H 0.6616 0.3996 0.5597 0.099 Uiso 1 1 calc R . . C6M C 0.615(2) 0.4284(12) 0.4870(7) 0.068(6) Uani 1 1 d U . . C7M C 0.526(2) 0.4080(12) 0.4439(8) 0.069(6) Uani 1 1 d U . . C8M C 0.719(2) 0.4910(12) 0.4888(7) 0.066(5) Uani 1 1 d U . . C9M C 0.899(2) 0.5842(12) 0.5145(7) 0.065(5) Uani 1 1 d U . . C10M C 1.001(2) 0.6307(12) 0.5401(8) 0.077(6) Uani 1 1 d U . . H10B H 1.0240 0.6274 0.5748 0.093 Uiso 1 1 calc R . . C11M C 1.072(3) 0.6832(13) 0.5143(8) 0.090(7) Uani 1 1 d U . . H11C H 1.1492 0.7145 0.5312 0.108 Uiso 1 1 calc R . . C12M C 1.033(3) 0.6920(13) 0.4625(8) 0.088(7) Uani 1 1 d U . . H12D H 1.0775 0.7305 0.4458 0.106 Uiso 1 1 calc R . . C13M C 0.926(3) 0.6415(14) 0.4373(9) 0.092(7) Uani 1 1 d U . . H13C H 0.8994 0.6442 0.4027 0.111 Uiso 1 1 calc R . . C14M C 0.860(2) 0.5879(11) 0.4640(7) 0.067(5) Uani 1 1 d U . . C1N C 0.612(2) 0.3471(11) 0.2019(8) 0.078(6) Uani 1 1 d U . . H1NB H 0.5604 0.3307 0.1698 0.117 Uiso 1 1 calc R . . H1NC H 0.6113 0.3069 0.2243 0.117 Uiso 1 1 calc R . . H1ND H 0.7162 0.3625 0.1971 0.117 Uiso 1 1 calc R . . C2N C 0.506(2) 0.4662(10) 0.1923(7) 0.055(5) Uani 1 1 d U . . C3N C 0.553(2) 0.4752(10) 0.1459(6) 0.054(5) Uani 1 1 d U . . H3NA H 0.6152 0.4410 0.1313 0.065 Uiso 1 1 calc R . . C4N C 0.5082(19) 0.5358(10) 0.1201(6) 0.050(4) Uani 1 1 d U . . C5N C 0.4192(19) 0.5868(9) 0.1400(6) 0.045(4) Uani 1 1 d U . . H5NA H 0.3918 0.6270 0.1213 0.055 Uiso 1 1 calc R . . C6N C 0.3654(19) 0.5801(9) 0.1903(6) 0.044(4) Uani 1 1 d U . . C7N C 0.414(2) 0.5165(10) 0.2158(6) 0.049(4) Uani 1 1 d U . . C8N C 0.2682(19) 0.6316(10) 0.2119(6) 0.049(4) Uani 1 1 d U . . C9N C 0.127(2) 0.7252(9) 0.2272(6) 0.049(4) Uani 1 1 d U . . C10N C 0.048(2) 0.7901(11) 0.2263(7) 0.061(5) Uani 1 1 d U . . H10D H 0.0460 0.8188 0.1981 0.073 Uiso 1 1 calc R . . C11N C -0.029(2) 0.8113(11) 0.2691(7) 0.065(5) Uani 1 1 d U . . H11A H -0.0824 0.8545 0.2698 0.078 Uiso 1 1 calc R . . C12N C -0.023(2) 0.7663(11) 0.3109(7) 0.068(6) Uani 1 1 d U . . H12B H -0.0726 0.7804 0.3396 0.082 Uiso 1 1 calc R . . C13N C 0.053(2) 0.7028(11) 0.3100(7) 0.065(5) Uani 1 1 d U . . H13B H 0.0531 0.6726 0.3374 0.078 Uiso 1 1 calc R . . C14N C 0.128(2) 0.6838(10) 0.2686(6) 0.052(5) Uani 1 1 d U . . C16 C 0.641(5) 0.278(2) 0.3390(15) 0.208(18) Uiso 1 1 d . . . H16A H 0.7359 0.2550 0.3337 0.312 Uiso 1 1 calc R . . H16B H 0.5580 0.2460 0.3231 0.312 Uiso 1 1 calc R . . H16C H 0.6297 0.2839 0.3748 0.312 Uiso 1 1 calc R . . O1W O 0.9416(17) 0.3697(8) 0.3219(5) 0.090(4) Uani 1 1 d U . . O2W O 1.5468(16) 1.2775(8) 0.0109(5) 0.080(4) Uani 1 1 d U . . O3W O 0.428(7) 0.113(3) 0.262(2) 0.23(2) Uani 0.50 1 d PU . . O3W' O 1.384(8) 0.880(4) 0.549(2) 0.24(3) Uani 0.50 1 d PU . . O4W O 0.894(5) 1.196(2) 0.2262(15) 0.138(13) Uani 0.50 1 d PU . . O4W' O 0.818(5) 1.111(2) 0.2809(17) 0.158(16) Uani 0.50 1 d PU . . 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 0.0426(6) 0.0525(6) 0.0521(6) 0.0183(4) 0.0153(4) 0.0036(4) Br1 0.0625(14) 0.0662(13) 0.0681(12) 0.0273(10) 0.0096(10) 0.0131(10) Br1' 0.162(3) 0.0840(17) 0.0751(15) 0.0408(13) 0.0056(15) -0.0112(17) Cl1 0.055(3) 0.061(3) 0.063(3) 0.014(2) 0.011(2) 0.003(2) Cl2 0.056(3) 0.059(3) 0.057(3) 0.019(2) 0.001(2) -0.003(2) Cl3 0.060(3) 0.054(3) 0.069(3) 0.024(2) 0.020(2) 0.006(2) O1 0.047(6) 0.063(6) 0.052(6) 0.005(5) 0.006(5) 0.014(5) O2 0.053(6) 0.052(6) 0.047(5) 0.021(5) 0.017(5) 0.009(5) O3 0.051(6) 0.058(6) 0.054(6) 0.003(5) 0.010(5) -0.002(5) O1' 0.061(7) 0.059(7) 0.062(6) 0.018(5) 0.012(6) -0.001(6) O2' 0.055(7) 0.056(6) 0.070(6) 0.021(5) 0.006(5) 0.007(5) N1 0.053(7) 0.046(7) 0.039(6) 0.010(6) 0.006(6) -0.001(6) N2 0.044(7) 0.037(6) 0.052(7) 0.009(6) 0.008(6) 0.006(6) N1' 0.053(7) 0.065(8) 0.060(7) 0.018(6) 0.020(6) -0.002(6) N2' 0.050(7) 0.050(7) 0.054(7) 0.017(6) 0.011(6) 0.013(6) C1 0.055(8) 0.053(8) 0.053(8) 0.000(7) 0.011(7) 0.002(7) C2 0.034(8) 0.040(7) 0.043(7) 0.002(6) -0.005(6) 0.011(6) C3 0.047(8) 0.034(7) 0.046(7) 0.002(6) 0.001(6) 0.004(6) C4 0.036(8) 0.039(7) 0.054(8) 0.014(6) 0.001(6) -0.004(6) C5 0.047(8) 0.058(8) 0.051(8) 0.006(7) 0.010(7) 0.002(7) C6 0.039(8) 0.036(7) 0.047(7) 0.015(6) -0.001(6) 0.003(6) C7 0.047(8) 0.049(8) 0.052(8) 0.012(7) 0.002(7) -0.005(7) C8 0.038(8) 0.040(8) 0.048(7) -0.006(6) 0.000(6) -0.002(7) C9 0.056(8) 0.046(8) 0.051(8) 0.002(7) 0.007(7) -0.005(7) C10 0.072(9) 0.069(9) 0.064(8) 0.009(7) 0.010(7) 0.007(8) C11 0.066(9) 0.073(9) 0.053(8) 0.003(7) 0.021(7) 0.002(8) C12 0.057(9) 0.064(9) 0.068(8) 0.004(7) 0.012(7) 0.010(7) C13 0.058(9) 0.058(8) 0.059(8) 0.005(7) 0.014(7) 0.006(7) C14 0.047(8) 0.047(8) 0.052(8) 0.014(7) 0.001(7) -0.001(7) C15 0.070(9) 0.079(9) 0.066(9) 0.010(7) 0.007(7) 0.019(8) C1' 0.064(9) 0.061(9) 0.063(8) 0.011(7) 0.011(7) 0.006(7) C2' 0.055(9) 0.050(8) 0.058(8) 0.014(7) 0.010(7) 0.008(7) C3' 0.064(9) 0.076(9) 0.076(9) 0.006(8) 0.016(8) 0.011(8) C4' 0.066(9) 0.051(8) 0.051(8) 0.016(7) 0.010(7) -0.007(7) C5' 0.064(9) 0.059(9) 0.064(8) 0.015(7) 0.012(7) 0.004(7) C6' 0.054(8) 0.037(7) 0.057(8) 0.005(6) 0.021(7) 0.005(7) C7' 0.057(9) 0.072(9) 0.071(9) 0.016(8) 0.022(7) 0.015(7) C8' 0.040(8) 0.044(8) 0.060(8) 0.014(7) 0.010(7) 0.006(7) C9' 0.058(9) 0.073(9) 0.072(9) 0.010(8) 0.013(7) 0.008(8) C10' 0.063(9) 0.064(9) 0.069(9) 0.002(7) 0.017(7) 0.003(8) C11' 0.063(9) 0.072(9) 0.077(9) 0.009(8) 0.010(8) -0.010(8) C12' 0.075(10) 0.081(10) 0.084(9) 0.013(8) 0.010(8) -0.001(8) C13' 0.072(9) 0.062(9) 0.076(9) 0.027(7) 0.009(8) 0.007(8) C14' 0.058(9) 0.053(8) 0.062(8) 0.017(7) 0.018(7) 0.009(7) Eu2 0.0591(7) 0.0713(7) 0.0606(6) 0.0299(5) 0.0104(5) 0.0040(5) Br1M 0.273(4) 0.120(2) 0.0672(16) 0.0422(16) 0.017(2) -0.015(3) Br1N 0.0467(12) 0.0954(16) 0.0559(11) 0.0191(10) 0.0167(9) 0.0019(11) Cl1M 0.085(4) 0.087(4) 0.088(4) 0.031(3) 0.005(3) -0.013(3) Cl2M 0.066(3) 0.077(3) 0.060(3) 0.030(2) 0.007(2) -0.005(3) Cl3M 0.075(4) 0.098(4) 0.057(3) 0.018(3) 0.017(3) 0.007(3) O1M 0.079(8) 0.093(8) 0.076(7) 0.021(6) 0.012(6) 0.006(7) O2M 0.079(7) 0.081(7) 0.055(6) 0.029(6) 0.006(6) 0.000(6) O1N 0.056(7) 0.056(6) 0.070(6) 0.012(6) 0.014(5) 0.008(5) O2N 0.053(7) 0.065(6) 0.057(6) 0.017(5) 0.014(5) 0.010(5) O3' 0.104(8) 0.093(7) 0.096(7) 0.038(6) 0.007(6) 0.018(6) N1M 0.066(8) 0.077(8) 0.067(8) -0.003(7) 0.007(7) 0.019(7) N2M 0.067(8) 0.071(8) 0.055(7) 0.018(6) 0.022(6) 0.011(7) N1N 0.039(7) 0.051(7) 0.044(6) 0.005(6) 0.008(6) 0.003(6) N2N 0.049(7) 0.059(7) 0.044(6) 0.013(6) 0.008(6) 0.006(6) C1M 0.094(11) 0.101(11) 0.101(10) 0.011(8) 0.013(8) 0.006(9) C2M 0.061(9) 0.071(9) 0.057(8) 0.013(7) 0.003(7) 0.016(8) C3M 0.086(10) 0.085(10) 0.075(9) 0.008(8) 0.017(8) 0.011(8) C4M 0.095(10) 0.078(9) 0.058(9) 0.012(8) 0.007(8) 0.009(8) C5M 0.083(10) 0.093(10) 0.074(9) 0.013(8) 0.007(8) 0.012(8) C6M 0.069(9) 0.075(9) 0.064(9) 0.006(7) 0.017(8) 0.019(8) C7M 0.066(9) 0.079(9) 0.067(9) 0.021(8) 0.014(8) 0.008(8) C8M 0.059(9) 0.076(9) 0.065(9) 0.015(8) -0.002(7) 0.011(8) C9M 0.062(9) 0.074(9) 0.059(8) 0.005(7) 0.011(7) 0.002(8) C10M 0.076(10) 0.084(10) 0.074(9) 0.004(8) 0.015(8) 0.009(8) C11M 0.083(10) 0.103(11) 0.083(10) 0.005(8) 0.009(8) -0.002(8) C12M 0.088(10) 0.100(10) 0.079(10) 0.007(8) 0.016(8) 0.002(8) C13M 0.091(11) 0.105(11) 0.083(10) 0.008(8) 0.015(8) 0.006(9) C14M 0.072(9) 0.072(9) 0.060(8) 0.013(7) 0.019(7) 0.012(8) C1N 0.073(10) 0.080(10) 0.081(9) 0.005(8) 0.011(8) 0.012(8) C2N 0.055(9) 0.056(8) 0.056(8) 0.012(7) 0.012(7) 0.010(7) C3N 0.050(8) 0.056(8) 0.058(8) 0.001(7) 0.015(7) -0.001(7) C4N 0.044(8) 0.055(8) 0.052(8) 0.009(7) 0.015(7) 0.002(7) C5N 0.045(8) 0.044(8) 0.047(7) 0.007(6) 0.008(6) -0.007(7) C6N 0.040(8) 0.047(8) 0.044(7) 0.003(6) 0.004(6) -0.002(7) C7N 0.044(8) 0.057(8) 0.048(8) 0.011(7) 0.004(7) -0.005(7) C8N 0.039(8) 0.058(8) 0.053(8) 0.011(7) 0.006(7) -0.002(7) C9N 0.049(8) 0.044(8) 0.054(8) 0.010(7) 0.010(7) -0.003(7) C10N 0.061(9) 0.068(9) 0.055(8) 0.008(7) 0.008(7) 0.004(7) C11N 0.060(9) 0.063(9) 0.073(9) 0.008(7) 0.007(7) 0.003(7) C12N 0.067(9) 0.077(9) 0.061(8) -0.001(8) 0.008(7) 0.006(8) C13N 0.066(9) 0.064(9) 0.068(9) 0.015(7) 0.011(7) -0.003(7) C14N 0.053(8) 0.058(8) 0.046(8) 0.007(7) 0.007(7) 0.001(7) O1W 0.088(8) 0.092(8) 0.090(7) 0.017(6) 0.016(6) -0.003(7) O2W 0.066(7) 0.093(8) 0.081(7) 0.013(6) 0.004(6) 0.002(6) O3W 0.23(3) 0.23(3) 0.23(3) 0.012(10) 0.013(10) 0.016(10) O3W' 0.24(3) 0.24(3) 0.24(3) 0.009(10) 0.016(10) 0.018(10) O4W 0.136(16) 0.135(16) 0.143(16) -0.001(10) 0.016(10) 0.007(10) O4W' 0.152(18) 0.158(18) 0.164(18) -0.003(10) 0.020(10) 0.008(10) _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 O2 2.252(9) . ? Eu1 O2' 2.280(11) . ? Eu1 O3 2.419(11) . ? Eu1 Cl1 2.684(5) . ? Eu1 O1 2.736(11) . ? Eu1 Cl2 2.785(5) . ? Eu1 Cl3 2.814(5) . ? Eu1 O1' 3.114(11) . ? Eu1 C7 3.266(16) . ? Br1 C4 1.945(15) . ? Br1' C4' 1.935(16) . ? O1 C2 1.379(17) . ? O1 C1 1.43(2) . ? O2 C7 1.283(18) . ? O2 H2B 0.9300 . ? O3 C15 1.417(19) . ? O3 H3B 0.8200 . ? O1' C2' 1.357(19) . ? O1' C1' 1.40(2) . ? O2' C7' 1.32(2) . ? O2' H2'B 0.9300 . ? N1 C9 1.36(2) . ? N1 C8 1.361(19) . ? N1 H1A 0.8600 . ? N2 C8 1.331(19) . ? N2 C14 1.42(2) . ? N1' C8' 1.34(2) . ? N1' C9' 1.39(2) . ? N1' H1'A 0.8600 . ? N2' C8' 1.362(19) . ? N2' C14' 1.38(2) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.32(2) . ? C2 C7 1.45(2) . ? C3 C4 1.37(2) . ? C3 H3A 0.9300 . ? C4 C5 1.34(2) . ? C5 C6 1.41(2) . ? C5 H5A 0.9300 . ? C6 C7 1.41(2) . ? C6 C8 1.44(2) . ? C9 C10 1.39(2) . ? C9 C14 1.41(2) . ? C10 C11 1.36(3) . ? C10 H10C 0.9300 . ? C11 C12 1.41(2) . ? C11 H11B 0.9300 . ? C12 C13 1.41(2) . ? C12 H12A 0.9300 . ? C13 C14 1.33(2) . ? C13 H13A 0.9300 . ? C15 H1WA 0.9600 . ? C15 H1WB 0.9600 . ? C15 H1WC 0.9600 . ? C1' H1'B 0.9600 . ? C1' H1'C 0.9600 . ? C1' H1'D 0.9600 . ? C2' C3' 1.37(2) . ? C2' C7' 1.39(2) . ? C3' C4' 1.39(2) . ? C3' H3'A 0.9300 . ? C4' C5' 1.29(2) . ? C5' C6' 1.45(2) . ? C5' H5'A 0.9300 . ? C6' C8' 1.40(2) . ? C6' C7' 1.45(2) . ? C9' C10' 1.39(3) . ? C9' C14' 1.40(2) . ? C10' C11' 1.39(3) . ? C10' H10A 0.9300 . ? C11' C12' 1.43(3) . ? C11' H11D 0.9300 . ? C12' C13' 1.39(3) . ? C12' H12C 0.9300 . ? C13' C14' 1.37(2) . ? C13' H13D 0.9300 . ? Eu2 O2N 2.238(11) . ? Eu2 O2M 2.272(12) . ? Eu2 O3' 2.405(14) . ? Eu2 Cl1M 2.675(6) . ? Eu2 O1N 2.682(12) . ? Eu2 Cl2M 2.817(5) . ? Eu2 Cl3M 2.831(6) . ? Eu2 O1M 2.944(13) . ? Eu2 C7N 3.255(16) . ? Br1M C4M 1.950(19) . ? Br1N C4N 1.905(15) . ? O1M C2M 1.35(2) . ? O1M C1M 1.43(2) . ? O2M C7M 1.32(2) . ? O2M H2MA 0.9300 . ? O1N C2N 1.387(19) . ? O1N C1N 1.45(2) . ? O2N C7N 1.331(18) . ? O2N H2NB 0.9300 . ? O3' C16 1.20(4) . ? O3' H1BB 0.9300 . ? N1M C8M 1.35(2) . ? N1M C9M 1.39(2) . ? N1M H1MA 0.8600 . ? N2M C8M 1.37(2) . ? N2M C14M 1.38(2) . ? N1N C8N 1.30(2) . ? N1N C9N 1.37(2) . ? N1N H1NA 0.8600 . ? N2N C8N 1.345(19) . ? N2N C14N 1.40(2) . ? C1M H1MB 0.9600 . ? C1M H1MC 0.9600 . ? C1M H1MD 0.9600 . ? C2M C7M 1.41(3) . ? C2M C3M 1.41(2) . ? C3M C4M 1.43(3) . ? C3M H3MA 0.9300 . ? C4M C5M 1.31(3) . ? C5M C6M 1.40(3) . ? C5M H5MA 0.9300 . ? C6M C7M 1.36(3) . ? C6M C8M 1.41(3) . ? C9M C10M 1.32(3) . ? C9M C14M 1.36(2) . ? C10M C11M 1.35(3) . ? C10M H10B 0.9300 . ? C11M C12M 1.41(3) . ? C11M H11C 0.9300 . ? C12M C13M 1.38(3) . ? C12M H12D 0.9300 . ? C13M C14M 1.36(3) . ? C13M H13C 0.9300 . ? C1N H1NB 0.9600 . ? C1N H1NC 0.9600 . ? C1N H1ND 0.9600 . ? C2N C3N 1.34(2) . ? C2N C7N 1.39(2) . ? C3N C4N 1.38(2) . ? C3N H3NA 0.9300 . ? C4N C5N 1.35(2) . ? C5N C6N 1.45(2) . ? C5N H5NA 0.9300 . ? C6N C8N 1.42(2) . ? C6N C7N 1.43(2) . ? C9N C14N 1.36(2) . ? C9N C10N 1.39(2) . ? C10N C11N 1.40(2) . ? C10N H10D 0.9300 . ? C11N C12N 1.41(2) . ? C11N H11A 0.9300 . ? C12N C13N 1.35(3) . ? C12N H12B 0.9300 . ? C13N C14N 1.35(2) . ? C13N H13B 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Eu1 O2' 137.6(4) . . ? O2 Eu1 O3 131.4(4) . . ? O2' Eu1 O3 79.9(4) . . ? O2 Eu1 Cl1 91.6(3) . . ? O2' Eu1 Cl1 121.7(3) . . ? O3 Eu1 Cl1 87.4(3) . . ? O2 Eu1 O1 61.2(4) . . ? O2' Eu1 O1 145.5(4) . . ? O3 Eu1 O1 71.5(3) . . ? Cl1 Eu1 O1 76.5(3) . . ? O2 Eu1 Cl2 80.5(3) . . ? O2' Eu1 Cl2 78.7(3) . . ? O3 Eu1 Cl2 79.4(3) . . ? Cl1 Eu1 Cl2 153.44(15) . . ? O1 Eu1 Cl2 77.5(3) . . ? O2 Eu1 Cl3 71.5(3) . . ? O2' Eu1 Cl3 80.5(3) . . ? O3 Eu1 Cl3 157.0(3) . . ? Cl1 Eu1 Cl3 92.94(15) . . ? O1 Eu1 Cl3 130.9(2) . . ? Cl2 Eu1 Cl3 108.18(15) . . ? O2 Eu1 O1' 145.1(4) . . ? O2' Eu1 O1' 55.1(4) . . ? O3 Eu1 O1' 76.8(3) . . ? Cl1 Eu1 O1' 66.6(2) . . ? O1 Eu1 O1' 131.8(3) . . ? Cl2 Eu1 O1' 130.8(2) . . ? Cl3 Eu1 O1' 82.3(2) . . ? O2 Eu1 C7 16.7(4) . . ? O2' Eu1 C7 149.5(4) . . ? O3 Eu1 C7 115.2(4) . . ? Cl1 Eu1 C7 86.7(3) . . ? O1 Eu1 C7 44.5(4) . . ? Cl2 Eu1 C7 78.4(3) . . ? Cl3 Eu1 C7 87.7(3) . . ? O1' Eu1 C7 150.8(4) . . ? C2 O1 C1 115.9(12) . . ? C2 O1 Eu1 115.4(9) . . ? C1 O1 Eu1 128.5(9) . . ? C7 O2 Eu1 133.1(11) . . ? C7 O2 H2B 113.5 . . ? Eu1 O2 H2B 113.5 . . ? C15 O3 Eu1 131.1(11) . . ? C15 O3 H3B 109.5 . . ? Eu1 O3 H3B 90.4 . . ? C2' O1' C1' 115.2(13) . . ? C2' O1' Eu1 109.9(10) . . ? C1' O1' Eu1 134.1(9) . . ? C7' O2' Eu1 139.9(12) . . ? C7' O2' H2'B 110.1 . . ? Eu1 O2' H2'B 110.1 . . ? C9 N1 C8 109.1(13) . . ? C9 N1 H1A 125.4 . . ? C8 N1 H1A 125.4 . . ? C8 N2 C14 109.5(12) . . ? C8' N1' C9' 109.4(15) . . ? C8' N1' H1'A 125.3 . . ? C9' N1' H1'A 125.3 . . ? C8' N2' C14' 110.5(14) . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C3 C2 O1 128.4(15) . . ? C3 C2 C7 120.8(15) . . ? O1 C2 C7 110.8(13) . . ? C2 C3 C4 120.1(16) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 123.7(15) . . ? C5 C4 Br1 117.6(12) . . ? C3 C4 Br1 118.5(13) . . ? C4 C5 C6 117.9(15) . . ? C4 C5 H5A 121.1 . . ? C6 C5 H5A 121.1 . . ? C7 C6 C5 120.6(16) . . ? C7 C6 C8 118.4(14) . . ? C5 C6 C8 121.0(14) . . ? O2 C7 C6 123.6(16) . . ? O2 C7 C2 119.5(14) . . ? C6 C7 C2 116.9(15) . . ? O2 C7 Eu1 30.2(7) . . ? C6 C7 Eu1 153.8(13) . . ? C2 C7 Eu1 89.3(9) . . ? N2 C8 N1 108.8(14) . . ? N2 C8 C6 122.5(14) . . ? N1 C8 C6 128.7(15) . . ? N1 C9 C10 131.3(16) . . ? N1 C9 C14 108.3(15) . . ? C10 C9 C14 120.2(18) . . ? C11 C10 C9 115.6(17) . . ? C11 C10 H10C 122.2 . . ? C9 C10 H10C 122.2 . . ? C10 C11 C12 124.1(18) . . ? C10 C11 H11B 118.0 . . ? C12 C11 H11B 118.0 . . ? C11 C12 C13 119.3(18) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C14 C13 C12 116.2(17) . . ? C14 C13 H13A 121.9 . . ? C12 C13 H13A 121.9 . . ? C13 C14 C9 124.3(17) . . ? C13 C14 N2 131.4(15) . . ? C9 C14 N2 104.3(15) . . ? O3 C15 H1WA 109.5 . . ? O3 C15 H1WB 109.5 . . ? H1WA C15 H1WB 109.5 . . ? O3 C15 H1WC 109.5 . . ? H1WA C15 H1WC 109.5 . . ? H1WB C15 H1WC 109.5 . . ? O1' C1' H1'B 109.5 . . ? O1' C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? O1' C1' H1'D 109.5 . . ? H1'B C1' H1'D 109.5 . . ? H1'C C1' H1'D 109.5 . . ? O1' C2' C3' 125.6(18) . . ? O1' C2' C7' 113.2(15) . . ? C3' C2' C7' 121.2(17) . . ? C2' C3' C4' 117.3(19) . . ? C2' C3' H3'A 121.3 . . ? C4' C3' H3'A 121.3 . . ? C5' C4' C3' 126.4(17) . . ? C5' C4' Br1' 118.0(13) . . ? C3' C4' Br1' 115.4(15) . . ? C4' C5' C6' 118.3(17) . . ? C4' C5' H5'A 120.9 . . ? C6' C5' H5'A 120.9 . . ? C8' C6' C5' 122.3(15) . . ? C8' C6' C7' 120.6(15) . . ? C5' C6' C7' 117.1(17) . . ? O2' C7' C2' 120.9(17) . . ? O2' C7' C6' 119.6(18) . . ? C2' C7' C6' 119.3(16) . . ? N1' C8' N2' 107.3(15) . . ? N1' C8' C6' 126.3(15) . . ? N2' C8' C6' 126.4(15) . . ? N1' C9' C10' 132.6(18) . . ? N1' C9' C14' 107.6(18) . . ? C10' C9' C14' 119.7(19) . . ? C11' C10' C9' 119.5(18) . . ? C11' C10' H10A 120.2 . . ? C9' C10' H10A 120.2 . . ? C10' C11' C12' 117.7(19) . . ? C10' C11' H11D 121.2 . . ? C12' C11' H11D 121.2 . . ? C13' C12' C11' 124(2) . . ? C13' C12' H12C 117.9 . . ? C11' C12' H12C 117.9 . . ? C14' C13' C12' 114.8(18) . . ? C14' C13' H13D 122.6 . . ? C12' C13' H13D 122.6 . . ? C13' C14' N2' 130.8(16) . . ? C13' C14' C9' 124.1(19) . . ? N2' C14' C9' 104.9(16) . . ? O2N Eu2 O2M 130.9(4) . . ? O2N Eu2 O3' 133.3(4) . . ? O2M Eu2 O3' 80.9(5) . . ? O2N Eu2 Cl1M 94.8(3) . . ? O2M Eu2 Cl1M 127.8(3) . . ? O3' Eu2 Cl1M 83.8(4) . . ? O2N Eu2 O1N 61.5(4) . . ? O2M Eu2 O1N 143.2(4) . . ? O3' Eu2 O1N 73.2(4) . . ? Cl1M Eu2 O1N 75.2(3) . . ? O2N Eu2 Cl2M 78.3(3) . . ? O2M Eu2 Cl2M 75.3(3) . . ? O3' Eu2 Cl2M 79.5(3) . . ? Cl1M Eu2 Cl2M 148.75(17) . . ? O1N Eu2 Cl2M 74.7(3) . . ? O2N Eu2 Cl3M 71.2(3) . . ? O2M Eu2 Cl3M 80.3(4) . . ? O3' Eu2 Cl3M 155.5(3) . . ? Cl1M Eu2 Cl3M 95.57(18) . . ? O1N Eu2 Cl3M 130.5(3) . . ? Cl2M Eu2 Cl3M 110.43(16) . . ? O2N Eu2 O1M 145.7(4) . . ? O2M Eu2 O1M 57.7(4) . . ? O3' Eu2 O1M 77.2(4) . . ? Cl1M Eu2 O1M 70.3(3) . . ? O1N Eu2 O1M 136.4(4) . . ? Cl2M Eu2 O1M 130.0(3) . . ? Cl3M Eu2 O1M 79.5(3) . . ? O2N Eu2 C7N 18.3(4) . . ? O2M Eu2 C7N 139.6(4) . . ? O3' Eu2 C7N 115.0(4) . . ? Cl1M Eu2 C7N 91.8(3) . . ? O1N Eu2 C7N 43.7(4) . . ? Cl2M Eu2 C7N 72.0(3) . . ? Cl3M Eu2 C7N 89.5(3) . . ? O1M Eu2 C7N 157.7(4) . . ? C2M O1M C1M 120.3(16) . . ? C2M O1M Eu2 110.3(11) . . ? C1M O1M Eu2 128.8(12) . . ? C7M O2M Eu2 138.5(13) . . ? C7M O2M H2MA 110.7 . . ? Eu2 O2M H2MA 110.7 . . ? C2N O1N C1N 115.8(14) . . ? C2N O1N Eu2 116.7(10) . . ? C1N O1N Eu2 127.4(10) . . ? C7N O2N Eu2 129.9(11) . . ? C7N O2N H2NB 115.1 . . ? Eu2 O2N H2NB 115.1 . . ? C16 O3' Eu2 129(2) . . ? C16 O3' H1BB 115.7 . . ? Eu2 O3' H1BB 115.7 . . ? C8M N1M C9M 113.5(17) . . ? C8M N1M H1MA 123.3 . . ? C9M N1M H1MA 123.3 . . ? C8M N2M C14M 109.4(16) . . ? C8N N1N C9N 109.7(14) . . ? C8N N1N H1NA 125.1 . . ? C9N N1N H1NA 125.1 . . ? C8N N2N C14N 107.2(13) . . ? O1M C1M H1MB 109.5 . . ? O1M C1M H1MC 109.5 . . ? H1MB C1M H1MC 109.5 . . ? O1M C1M H1MD 109.5 . . ? H1MB C1M H1MD 109.5 . . ? H1MC C1M H1MD 109.5 . . ? O1M C2M C7M 117.0(16) . . ? O1M C2M C3M 120.5(18) . . ? C7M C2M C3M 122.5(19) . . ? C2M C3M C4M 111.6(19) . . ? C2M C3M H3MA 124.2 . . ? C4M C3M H3MA 124.2 . . ? C5M C4M C3M 127(2) . . ? C5M C4M Br1M 118.6(17) . . ? C3M C4M Br1M 114.1(16) . . ? C4M C5M C6M 119(2) . . ? C4M C5M H5MA 120.5 . . ? C6M C5M H5MA 120.5 . . ? C7M C6M C5M 119(2) . . ? C7M C6M C8M 120.5(18) . . ? C5M C6M C8M 121(2) . . ? O2M C7M C6M 123.7(19) . . ? O2M C7M C2M 115.5(18) . . ? C6M C7M C2M 120.6(18) . . ? N1M C8M N2M 104.2(17) . . ? N1M C8M C6M 130.4(18) . . ? N2M C8M C6M 125.4(19) . . ? C10M C9M C14M 123(2) . . ? C10M C9M N1M 133.3(19) . . ? C14M C9M N1M 103.4(18) . . ? C9M C10M C11M 118(2) . . ? C9M C10M H10B 121.1 . . ? C11M C10M H10B 121.1 . . ? C10M C11M C12M 122(2) . . ? C10M C11M H11C 119.1 . . ? C12M C11M H11C 119.1 . . ? C13M C12M C11M 118(2) . . ? C13M C12M H12D 121.0 . . ? C11M C12M H12D 121.0 . . ? C14M C13M C12M 119(2) . . ? C14M C13M H13C 120.7 . . ? C12M C13M H13C 120.7 . . ? C13M C14M C9M 120(2) . . ? C13M C14M N2M 130.2(19) . . ? C9M C14M N2M 109.5(17) . . ? O1N C1N H1NB 109.5 . . ? O1N C1N H1NC 109.5 . . ? H1NB C1N H1NC 109.5 . . ? O1N C1N H1ND 109.5 . . ? H1NB C1N H1ND 109.5 . . ? H1NC C1N H1ND 109.5 . . ? C3N C2N O1N 128.0(17) . . ? C3N C2N C7N 122.4(17) . . ? O1N C2N C7N 109.6(14) . . ? C2N C3N C4N 119.0(17) . . ? C2N C3N H3NA 120.5 . . ? C4N C3N H3NA 120.5 . . ? C5N C4N C3N 122.3(15) . . ? C5N C4N Br1N 118.5(13) . . ? C3N C4N Br1N 118.8(13) . . ? C4N C5N C6N 121.0(15) . . ? C4N C5N H5NA 119.5 . . ? C6N C5N H5NA 119.5 . . ? C8N C6N C7N 122.4(15) . . ? C8N C6N C5N 122.5(15) . . ? C7N C6N C5N 115.0(15) . . ? O2N C7N C2N 120.8(15) . . ? O2N C7N C6N 118.9(16) . . ? C2N C7N C6N 120.3(15) . . ? O2N C7N Eu2 31.8(7) . . ? C2N C7N Eu2 89.5(10) . . ? C6N C7N Eu2 149.8(12) . . ? N1N C8N N2N 109.4(16) . . ? N1N C8N C6N 129.0(15) . . ? N2N C8N C6N 121.5(16) . . ? C14N C9N N1N 107.2(16) . . ? C14N C9N C10N 120.0(17) . . ? N1N C9N C10N 132.8(15) . . ? C9N C10N C11N 118.4(17) . . ? C9N C10N H10D 120.8 . . ? C11N C10N H10D 120.8 . . ? C10N C11N C12N 119.0(19) . . ? C10N C11N H11A 120.5 . . ? C12N C11N H11A 120.5 . . ? C13N C12N C11N 120.9(19) . . ? C13N C12N H12B 119.5 . . ? C11N C12N H12B 119.5 . . ? C12N C13N C14N 119.2(18) . . ? C12N C13N H13B 120.4 . . ? C14N C13N H13B 120.4 . . ? C13N C14N C9N 122.4(19) . . ? C13N C14N N2N 131.2(16) . . ? C9N C14N N2N 106.3(15) . . ? O3' C16 H16A 109.5 . . ? O3' C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O3' C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.288 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.163 # Attachment '- Complex-6.CIF' data_Complex-6 _database_code_depnum_ccdc_archive 'CCDC 777198' #TrackingRef '- Complex-6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C28 H22 Br2 Er N4 O8), 6(Cl), O' _chemical_formula_sum 'C56 H44 Br4 Cl6 Er2 N8 O17' _chemical_formula_weight 1967.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8838(16) _cell_length_b 14.174(3) _cell_length_c 16.683(3) _cell_angle_alpha 98.85(3) _cell_angle_beta 99.52(4) _cell_angle_gamma 99.55(3) _cell_volume 1781.4(7) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5653 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 950 _exptl_absorpt_coefficient_mu 4.875 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.4135 _exptl_absorpt_correction_T_max 0.5093 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10237 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6232 _reflns_number_gt 5440 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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. Hydrogen atoms of water molecules were not added. ; _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^)+(0.0245P)^2^+2.5682P] 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 6232 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.33599(4) 0.15643(2) 0.82860(2) 0.02312(12) Uani 1 1 d U . . Br1 Br -0.11016(12) -0.31819(6) 0.54959(6) 0.0436(2) Uani 1 1 d U . . Br1' Br 0.72851(13) 0.65374(6) 0.77614(6) 0.0445(2) Uani 1 1 d U . . C1' C 0.2889(11) 0.3044(6) 0.6704(5) 0.0325(18) Uani 1 1 d U . . H1'B H 0.2335 0.3599 0.6711 0.049 Uiso 1 1 calc R . . H1'C H 0.2034 0.2463 0.6458 0.049 Uiso 1 1 calc R . . H1'D H 0.3799 0.3111 0.6387 0.049 Uiso 1 1 calc R . . C2' C 0.4791(10) 0.3830(6) 0.7991(5) 0.0300(17) Uani 1 1 d U . . C3' C 0.5374(11) 0.4624(6) 0.7668(5) 0.0320(18) Uani 1 1 d U . . H3'A H 0.5007 0.4641 0.7112 0.038 Uiso 1 1 calc R . . C4' C 0.6549(11) 0.5419(6) 0.8203(5) 0.0309(18) Uani 1 1 d U . . C5' C 0.7126(10) 0.5390(6) 0.9013(5) 0.0303(18) Uani 1 1 d U . . H5'A H 0.7925 0.5913 0.9352 0.036 Uiso 1 1 calc R . . C6' C 0.6508(10) 0.4566(6) 0.9337(5) 0.0272(17) Uani 1 1 d U . . C7' C 0.5289(10) 0.3767(5) 0.8833(5) 0.0271(17) Uani 1 1 d U . . C8' C 0.7126(10) 0.4532(6) 1.0189(5) 0.0284(17) Uani 1 1 d U . . C9' C 0.8608(11) 0.4941(6) 1.1492(5) 0.0306(18) Uani 1 1 d U . . C10' C 0.9703(12) 0.5403(6) 1.2244(6) 0.039(2) Uani 1 1 d U . . H10A H 1.0463 0.5996 1.2300 0.047 Uiso 1 1 calc R . . C11' C 0.9587(12) 0.4922(7) 1.2901(6) 0.043(2) Uani 1 1 d U . . H11A H 1.0291 0.5198 1.3415 0.052 Uiso 1 1 calc R . . C12' C 0.8439(12) 0.4032(7) 1.2810(6) 0.040(2) Uani 1 1 d U . . H12A H 0.8387 0.3739 1.3270 0.048 Uiso 1 1 calc R . . C13' C 0.7380(11) 0.3573(6) 1.2065(6) 0.038(2) Uani 1 1 d U . . H13B H 0.6641 0.2972 1.2006 0.046 Uiso 1 1 calc R . . C14' C 0.7477(10) 0.4054(6) 1.1408(5) 0.0296(17) Uani 1 1 d U . . Cl1 Cl 0.4554(5) 0.1335(2) 0.09459(15) 0.0702(9) Uani 1 1 d U . . Cl2 Cl 0.7835(3) 0.22772(15) 0.65452(12) 0.0370(5) Uani 1 1 d U . . Cl3 Cl 1.0705(3) -0.28175(14) 0.05523(12) 0.0336(4) Uani 1 1 d U . . O1 O 0.1642(8) -0.0163(4) 0.7934(3) 0.0340(13) Uani 1 1 d U . . O2 O 0.2930(7) 0.0877(4) 0.6940(3) 0.0290(12) Uani 1 1 d U . . H2A H 0.3413 0.1251 0.6592 0.035 Uiso 1 1 calc R . . O1' O 0.3630(7) 0.2984(4) 0.7530(3) 0.0316(12) Uani 1 1 d U . . O2' O 0.4621(7) 0.2988(4) 0.9094(3) 0.0291(12) Uani 1 1 d U . . H2'A H 0.4680 0.3035 0.9660 0.035 Uiso 1 1 calc R . . N1 N 0.2555(9) -0.0163(5) 0.4401(4) 0.0320(15) Uani 1 1 d U . . H1A H 0.2010 -0.0725 0.4125 0.038 Uiso 1 1 calc R . . N2 N 0.3616(8) 0.1044(5) 0.5433(4) 0.0277(14) Uani 1 1 d U . . N1' N 0.8375(9) 0.5218(5) 1.0729(4) 0.0315(15) Uani 1 1 d U . . H1'A H 0.8931 0.5739 1.0614 0.038 Uiso 1 1 calc R . . N2' N 0.6584(9) 0.3829(5) 1.0590(4) 0.0296(15) Uani 1 1 d U . . C1 C 0.0925(14) -0.0738(7) 0.8489(6) 0.048(2) Uani 1 1 d U . . H1B H 0.1297 -0.1352 0.8427 0.072 Uiso 1 1 calc R . . H1C H -0.0333 -0.0847 0.8358 0.072 Uiso 1 1 calc R . . H1D H 0.1334 -0.0396 0.9049 0.072 Uiso 1 1 calc R . . C2 C 0.1299(10) -0.0614(6) 0.7102(5) 0.0292(17) Uani 1 1 d U . . C3 C 0.0368(10) -0.1537(6) 0.6789(5) 0.0312(18) Uani 1 1 d U . . H3A H -0.0131 -0.1916 0.7130 0.037 Uiso 1 1 calc R . . C4 C 0.0190(10) -0.1891(6) 0.5953(5) 0.0314(18) Uani 1 1 d U . . C5 C 0.0897(10) -0.1360(6) 0.5443(5) 0.0301(17) Uani 1 1 d U . . H5A H 0.0752 -0.1618 0.4883 0.036 Uiso 1 1 calc R . . C6 C 0.1847(10) -0.0417(6) 0.5765(5) 0.0282(17) Uani 1 1 d U . . C7 C 0.2053(10) -0.0009(5) 0.6601(5) 0.0260(16) Uani 1 1 d U . . C8 C 0.2654(10) 0.0142(6) 0.5207(5) 0.0265(16) Uani 1 1 d U . . C9 C 0.3461(11) 0.0561(6) 0.4078(5) 0.0313(18) Uani 1 1 d U . . C10 C 0.3698(13) 0.0598(7) 0.3275(5) 0.043(2) Uani 1 1 d U . . H10B H 0.3229 0.0080 0.2837 0.051 Uiso 1 1 calc R . . C11 C 0.4675(13) 0.1456(8) 0.3172(6) 0.046(2) Uani 1 1 d U . . H11B H 0.4885 0.1510 0.2647 0.056 Uiso 1 1 calc R . . C12 C 0.5361(14) 0.2239(8) 0.3813(6) 0.050(2) Uani 1 1 d U . . H12B H 0.5984 0.2806 0.3703 0.060 Uiso 1 1 calc R . . C13 C 0.5137(12) 0.2196(7) 0.4622(6) 0.042(2) Uani 1 1 d U . . H13A H 0.5615 0.2714 0.5059 0.050 Uiso 1 1 calc R . . C14 C 0.4162(10) 0.1337(6) 0.4732(5) 0.0302(17) Uani 1 1 d U . . O1W O 0.6177(7) 0.1734(4) 0.8002(3) 0.0364(13) Uani 1 1 d U . . O2W O 0.1981(7) 0.1481(4) 0.9436(3) 0.0337(13) Uani 1 1 d U . . O3W O 0.0549(7) 0.1887(4) 0.7927(4) 0.0382(14) Uani 1 1 d U . . O4W O 0.4949(8) 0.0774(4) 0.9162(4) 0.0385(14) Uani 1 1 d U . . O5W O 0.505(3) 0.5015(16) 0.5436(12) 0.108(7) Uani 0.50 1 d PU . . 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 0.02335(18) 0.02639(19) 0.02008(18) 0.00358(13) 0.00515(13) 0.00600(13) Br1 0.0430(5) 0.0359(5) 0.0411(5) 0.0017(4) -0.0042(4) -0.0057(4) Br1' 0.0468(5) 0.0346(5) 0.0560(6) 0.0172(4) 0.0160(4) 0.0051(4) C1' 0.028(4) 0.038(4) 0.029(4) 0.005(3) 0.000(3) 0.007(3) C2' 0.026(4) 0.032(4) 0.032(4) 0.003(3) 0.005(3) 0.009(3) C3' 0.034(4) 0.034(4) 0.029(4) 0.006(3) 0.007(3) 0.010(3) C4' 0.033(4) 0.026(4) 0.039(4) 0.009(3) 0.017(3) 0.008(3) C5' 0.029(4) 0.029(4) 0.034(4) 0.002(3) 0.011(3) 0.008(3) C6' 0.023(4) 0.030(4) 0.031(4) 0.001(3) 0.011(3) 0.010(3) C7' 0.027(4) 0.028(4) 0.030(4) 0.006(3) 0.012(3) 0.009(3) C8' 0.027(4) 0.028(4) 0.031(4) -0.003(3) 0.011(3) 0.010(3) C9' 0.033(4) 0.033(4) 0.027(4) 0.002(3) 0.008(3) 0.012(3) C10' 0.039(4) 0.035(4) 0.040(5) -0.002(4) 0.000(4) 0.012(4) C11' 0.040(5) 0.057(5) 0.035(5) 0.007(4) 0.007(4) 0.016(4) C12' 0.042(5) 0.049(5) 0.034(4) 0.012(4) 0.005(4) 0.017(4) C13' 0.036(4) 0.036(4) 0.045(5) 0.009(4) 0.011(4) 0.010(4) C14' 0.028(4) 0.036(4) 0.026(4) 0.000(3) 0.008(3) 0.013(3) Cl1 0.118(3) 0.0682(17) 0.0286(12) -0.0013(12) -0.0039(14) 0.0587(18) Cl2 0.0384(11) 0.0437(12) 0.0235(10) -0.0014(8) 0.0023(8) 0.0039(9) Cl3 0.0291(10) 0.0347(10) 0.0342(11) -0.0028(8) 0.0069(8) 0.0065(8) O1 0.041(3) 0.038(3) 0.024(3) 0.006(2) 0.010(2) 0.005(2) O2 0.032(3) 0.028(3) 0.025(3) 0.003(2) 0.009(2) 0.000(2) O1' 0.033(3) 0.034(3) 0.027(3) 0.004(2) 0.002(2) 0.010(2) O2' 0.033(3) 0.030(3) 0.024(3) 0.002(2) 0.009(2) 0.004(2) N1 0.033(3) 0.035(4) 0.025(3) 0.000(3) 0.003(3) 0.007(3) N2 0.032(3) 0.029(3) 0.025(3) 0.009(3) 0.008(3) 0.009(3) N1' 0.034(3) 0.027(3) 0.034(4) 0.002(3) 0.007(3) 0.007(3) N2' 0.031(3) 0.028(3) 0.031(3) 0.001(3) 0.010(3) 0.009(3) C1 0.064(6) 0.049(5) 0.034(5) 0.017(4) 0.018(4) -0.002(4) C2 0.026(4) 0.039(4) 0.026(4) 0.008(3) 0.008(3) 0.011(3) C3 0.027(4) 0.032(4) 0.035(4) 0.011(3) 0.006(3) 0.003(3) C4 0.027(4) 0.029(4) 0.032(4) -0.001(3) 0.001(3) 0.000(3) C5 0.029(4) 0.036(4) 0.025(4) 0.003(3) 0.000(3) 0.011(3) C6 0.029(4) 0.031(4) 0.024(4) 0.003(3) 0.003(3) 0.009(3) C7 0.023(4) 0.028(4) 0.029(4) 0.007(3) 0.006(3) 0.006(3) C8 0.023(4) 0.037(4) 0.022(4) 0.003(3) 0.004(3) 0.012(3) C9 0.033(4) 0.042(4) 0.027(4) 0.012(3) 0.009(3) 0.020(3) C10 0.050(5) 0.055(5) 0.027(4) 0.009(4) 0.007(4) 0.020(4) C11 0.050(5) 0.066(6) 0.038(5) 0.027(4) 0.017(4) 0.028(4) C12 0.053(5) 0.053(5) 0.052(5) 0.025(4) 0.016(4) 0.016(4) C13 0.044(5) 0.045(5) 0.045(5) 0.017(4) 0.013(4) 0.016(4) C14 0.030(4) 0.040(4) 0.023(4) 0.011(3) 0.006(3) 0.012(3) O1W 0.031(3) 0.048(3) 0.029(3) 0.000(3) 0.007(2) 0.010(3) O2W 0.034(3) 0.040(3) 0.032(3) 0.011(2) 0.011(2) 0.010(2) O3W 0.032(3) 0.050(3) 0.035(3) 0.007(3) 0.008(2) 0.015(3) O4W 0.039(3) 0.043(3) 0.037(3) 0.011(3) 0.008(3) 0.014(3) O5W 0.123(10) 0.100(10) 0.086(9) 0.016(8) 0.028(8) -0.028(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O2' 2.221(5) . ? Er1 O2 2.253(5) . ? Er1 O4W 2.308(6) . ? Er1 O1W 2.329(6) . ? Er1 O3W 2.337(6) . ? Er1 O2W 2.365(5) . ? Er1 O1 2.523(6) . ? Er1 O1' 2.532(5) . ? Br1 C4 1.914(8) . ? Br1' C4' 1.894(8) . ? C1' O1' 1.426(9) . ? C1' H1'B 0.9600 . ? C1' H1'C 0.9600 . ? C1' H1'D 0.9600 . ? C2' C3' 1.365(11) . ? C2' O1' 1.410(10) . ? C2' C7' 1.416(11) . ? C3' C4' 1.413(12) . ? C3' H3'A 0.9300 . ? C4' C5' 1.363(12) . ? C5' C6' 1.409(11) . ? C5' H5'A 0.9300 . ? C6' C7' 1.411(11) . ? C6' C8' 1.435(11) . ? C7' O2' 1.310(9) . ? C8' N2' 1.334(10) . ? C8' N1' 1.358(10) . ? C9' N1' 1.381(10) . ? C9' C14' 1.389(12) . ? C9' C10' 1.396(12) . ? C10' C11' 1.385(13) . ? C10' H10A 0.9300 . ? C11' C12' 1.397(14) . ? C11' H11A 0.9300 . ? C12' C13' 1.376(13) . ? C12' H12A 0.9300 . ? C13' C14' 1.383(12) . ? C13' H13B 0.9300 . ? C14' N2' 1.391(10) . ? O1 C2 1.398(9) . ? O1 C1 1.446(10) . ? O2 C7 1.319(9) . ? O2 H2A 0.9300 . ? O2' H2'A 0.9300 . ? N1 C8 1.332(10) . ? N1 C9 1.382(11) . ? N1 H1A 0.8600 . ? N2 C8 1.337(10) . ? N2 C14 1.408(10) . ? N1' H1'A 0.8600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.366(12) . ? C2 C7 1.414(11) . ? C3 C4 1.383(11) . ? C3 H3A 0.9300 . ? C4 C5 1.348(11) . ? C5 C6 1.396(11) . ? C5 H5A 0.9300 . ? C6 C7 1.398(11) . ? C6 C8 1.468(11) . ? C9 C10 1.390(12) . ? C9 C14 1.392(12) . ? C10 C11 1.377(14) . ? C10 H10B 0.9300 . ? C11 C12 1.382(15) . ? C11 H11B 0.9300 . ? C12 C13 1.399(13) . ? C12 H12B 0.9300 . ? C13 C14 1.383(12) . ? C13 H13A 0.9300 . ? O5W O5W 1.44(4) 2_666 ? 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 O2 137.91(19) . . ? O2' Er1 O4W 90.2(2) . . ? O2 Er1 O4W 113.8(2) . . ? O2' Er1 O1W 79.4(2) . . ? O2 Er1 O1W 76.1(2) . . ? O4W Er1 O1W 72.6(2) . . ? O2' Er1 O3W 98.2(2) . . ? O2 Er1 O3W 84.2(2) . . ? O4W Er1 O3W 141.4(2) . . ? O1W Er1 O3W 145.9(2) . . ? O2' Er1 O2W 79.0(2) . . ? O2 Er1 O2W 139.6(2) . . ? O4W Er1 O2W 72.7(2) . . ? O1W Er1 O2W 138.7(2) . . ? O3W Er1 O2W 72.1(2) . . ? O2' Er1 O1 156.35(18) . . ? O2 Er1 O1 65.72(18) . . ? O4W Er1 O1 76.7(2) . . ? O1W Er1 O1 114.21(19) . . ? O3W Er1 O1 81.2(2) . . ? O2W Er1 O1 78.36(19) . . ? O2' Er1 O1' 65.82(18) . . ? O2 Er1 O1' 75.15(18) . . ? O4W Er1 O1' 143.1(2) . . ? O1W Er1 O1' 75.49(19) . . ? O3W Er1 O1' 72.7(2) . . ? O2W Er1 O1' 124.98(18) . . ? O1 Er1 O1' 134.65(18) . . ? O1' C1' H1'B 109.5 . . ? O1' C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? O1' C1' H1'D 109.5 . . ? H1'B C1' H1'D 109.5 . . ? H1'C C1' H1'D 109.5 . . ? C3' C2' O1' 124.3(7) . . ? C3' C2' C7' 123.5(8) . . ? O1' C2' C7' 112.2(7) . . ? C2' C3' C4' 118.1(8) . . ? C2' C3' H3'A 121.0 . . ? C4' C3' H3'A 121.0 . . ? C5' C4' C3' 121.3(7) . . ? C5' C4' Br1' 120.8(6) . . ? C3' C4' Br1' 117.9(6) . . ? C4' C5' C6' 119.8(8) . . ? C4' C5' H5'A 120.1 . . ? C6' C5' H5'A 120.1 . . ? C5' C6' C7' 120.9(7) . . ? C5' C6' C8' 119.8(7) . . ? C7' C6' C8' 119.3(7) . . ? O2' C7' C6' 124.4(7) . . ? O2' C7' C2' 119.2(7) . . ? C6' C7' C2' 116.3(7) . . ? N2' C8' N1' 108.1(7) . . ? N2' C8' C6' 126.4(7) . . ? N1' C8' C6' 125.5(7) . . ? N1' C9' C14' 107.0(7) . . ? N1' C9' C10' 130.9(8) . . ? C14' C9' C10' 122.1(8) . . ? C11' C10' C9' 115.8(9) . . ? C11' C10' H10A 122.1 . . ? C9' C10' H10A 122.1 . . ? C10' C11' C12' 121.6(9) . . ? C10' C11' H11A 119.2 . . ? C12' C11' H11A 119.2 . . ? C13' C12' C11' 122.3(9) . . ? C13' C12' H12A 118.8 . . ? C11' C12' H12A 118.8 . . ? C12' C13' C14' 116.3(8) . . ? C12' C13' H13B 121.8 . . ? C14' C13' H13B 121.8 . . ? C13' C14' C9' 121.8(8) . . ? C13' C14' N2' 132.0(8) . . ? C9' C14' N2' 106.2(7) . . ? C2 O1 C1 115.8(7) . . ? C2 O1 Er1 116.5(4) . . ? C1 O1 Er1 127.7(5) . . ? C7 O2 Er1 125.8(5) . . ? C7 O2 H2A 117.1 . . ? Er1 O2 H2A 117.1 . . ? C2' O1' C1' 115.3(6) . . ? C2' O1' Er1 114.0(4) . . ? C1' O1' Er1 130.6(5) . . ? C7' O2' Er1 125.0(5) . . ? C7' O2' H2'A 117.5 . . ? Er1 O2' H2'A 117.5 . . ? C8 N1 C9 109.6(7) . . ? C8 N1 H1A 125.2 . . ? C9 N1 H1A 125.2 . . ? C8 N2 C14 108.5(6) . . ? C8' N1' C9' 109.0(7) . . ? C8' N1' H1'A 125.5 . . ? C9' N1' H1'A 125.5 . . ? C8' N2' C14' 109.8(7) . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C3 C2 O1 125.1(7) . . ? C3 C2 C7 122.5(7) . . ? O1 C2 C7 112.4(7) . . ? C2 C3 C4 118.2(7) . . ? C2 C3 H3A 120.9 . . ? C4 C3 H3A 120.9 . . ? C5 C4 C3 122.4(8) . . ? C5 C4 Br1 118.3(6) . . ? C3 C4 Br1 119.3(6) . . ? C4 C5 C6 119.2(7) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C5 C6 C7 121.3(7) . . ? C5 C6 C8 118.6(7) . . ? C7 C6 C8 120.1(7) . . ? O2 C7 C6 124.0(7) . . ? O2 C7 C2 119.6(7) . . ? C6 C7 C2 116.4(7) . . ? N1 C8 N2 109.2(7) . . ? N1 C8 C6 125.8(7) . . ? N2 C8 C6 125.0(7) . . ? N1 C9 C10 131.1(8) . . ? N1 C9 C14 106.6(7) . . ? C10 C9 C14 122.3(8) . . ? C11 C10 C9 115.4(9) . . ? C11 C10 H10B 122.3 . . ? C9 C10 H10B 122.3 . . ? C10 C11 C12 123.1(9) . . ? C10 C11 H11B 118.5 . . ? C12 C11 H11B 118.5 . . ? C11 C12 C13 121.4(9) . . ? C11 C12 H12B 119.3 . . ? C13 C12 H12B 119.3 . . ? C14 C13 C12 115.9(9) . . ? C14 C13 H13A 122.1 . . ? C12 C13 H13A 122.1 . . ? C13 C14 C9 121.9(8) . . ? C13 C14 N2 132.0(8) . . ? C9 C14 N2 106.0(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.632 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.158 # Attachment '- Complex-7.CIF' data_complex-7 _database_code_depnum_ccdc_archive 'CCDC 777199' #TrackingRef '- Complex-7.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C28 H22 Br2 N4 O8 Yb), Cl2, 4(Cl), O' _chemical_formula_sum 'C56 H44 Br4 Cl6 N8 O17 Yb2' _chemical_formula_weight 1979.37 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0269(16) _cell_length_b 14.719(3) _cell_length_c 16.140(3) _cell_angle_alpha 97.70(3) _cell_angle_beta 94.74(4) _cell_angle_gamma 104.75(3) _cell_volume 1813.7(7) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6188 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 954 _exptl_absorpt_coefficient_mu 5.053 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.3895 _exptl_absorpt_correction_T_max 0.4632 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9934 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6289 _reflns_number_gt 5482 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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. Hydrogen atoms of water molecules were not added. ; _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^)+(0.0561P)^2^+1.0593P] 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 6289 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Yb1 Yb 0.13668(3) 0.334504(18) 0.149657(16) 0.02502(11) Uani 1 1 d U . . Br1 Br -0.14202(10) -0.17225(5) 0.21418(5) 0.0486(2) Uani 1 1 d U . . Br1' Br 0.67427(8) 0.77318(5) 0.43082(5) 0.04064(19) Uani 1 1 d U . . Cl1 Cl -0.34154(19) 0.32492(12) 0.33729(10) 0.0360(4) Uani 1 1 d U . . Cl2 Cl 0.5613(2) 0.24024(12) 0.03187(10) 0.0373(4) Uani 1 1 d U . . Cl3 Cl 0.0997(8) 0.4115(4) -0.1158(3) 0.0562(13) Uani 0.50 1 d PU . . Cl3' Cl 0.0017(9) 0.3702(4) -0.1094(3) 0.0663(16) Uani 0.50 1 d PU . . O1 O 0.1295(6) 0.1965(3) 0.2286(3) 0.0329(10) Uani 1 1 d U . . O2 O 0.0104(5) 0.1936(3) 0.0732(3) 0.0303(10) Uani 1 1 d U . . H2M H -0.0103 0.1908 0.0152 0.045 Uiso 1 1 calc R . . O1' O 0.3177(6) 0.5058(3) 0.1804(3) 0.0323(10) Uani 1 1 d U . . O2' O 0.1600(5) 0.4017(3) 0.2820(3) 0.0286(9) Uani 1 1 d U . . H2'M H 0.0849 0.3699 0.3160 0.043 Uiso 1 1 calc R . . N1 N -0.3582(7) -0.0412(4) -0.0722(3) 0.0322(12) Uani 1 1 d U . . H1A H -0.3960 -0.0971 -0.0593 0.039 Uiso 1 1 calc R . . N2 N -0.2101(7) 0.1064(4) -0.0637(3) 0.0307(12) Uani 1 1 d U . . N1' N 0.2137(6) 0.4820(4) 0.5439(3) 0.0287(11) Uani 1 1 d U . . H1'A H 0.2847 0.5317 0.5738 0.034 Uiso 1 1 calc R . . N2' N 0.0756(6) 0.3783(4) 0.4359(3) 0.0285(11) Uani 1 1 d U . . C1 C 0.2096(8) 0.1994(5) 0.3118(4) 0.0320(14) Uani 1 1 d U . . H1B H 0.2847 0.1580 0.3099 0.048 Uiso 1 1 calc R . . H1C H 0.1216 0.1790 0.3472 0.048 Uiso 1 1 calc R . . H1D H 0.2762 0.2634 0.3340 0.048 Uiso 1 1 calc R . . C2 C 0.0288(8) 0.1088(5) 0.1868(4) 0.0302(14) Uani 1 1 d U . . C3 C -0.0021(8) 0.0263(4) 0.2194(4) 0.0311(14) Uani 1 1 d U . . H3A H 0.0473 0.0251 0.2732 0.037 Uiso 1 1 calc R . . C4 C -0.1092(8) -0.0562(5) 0.1704(4) 0.0342(15) Uani 1 1 d U . . C5 C -0.1876(8) -0.0562(5) 0.0923(4) 0.0326(14) Uani 1 1 d U . . H5A H -0.2633 -0.1116 0.0620 0.039 Uiso 1 1 calc R . . C6 C -0.1525(8) 0.0291(4) 0.0578(4) 0.0280(13) Uani 1 1 d U . . C7 C -0.0380(8) 0.1131(5) 0.1033(4) 0.0293(14) Uani 1 1 d U . . C8 C -0.2356(8) 0.0316(5) -0.0243(4) 0.0298(14) Uani 1 1 d U . . C9 C -0.4136(8) -0.0115(5) -0.1453(4) 0.0315(14) Uani 1 1 d U . . C10 C -0.5356(8) -0.0572(5) -0.2134(4) 0.0396(16) Uani 1 1 d U . . H10A H -0.5971 -0.1208 -0.2177 0.047 Uiso 1 1 calc R . . C11 C -0.5611(9) -0.0039(6) -0.2740(5) 0.0464(18) Uani 1 1 d U . . H11B H -0.6433 -0.0324 -0.3204 0.056 Uiso 1 1 calc R . . C12 C -0.4695(10) 0.0911(6) -0.2695(5) 0.0459(18) Uani 1 1 d U . . H12B H -0.4914 0.1238 -0.3128 0.055 Uiso 1 1 calc R . . C13 C -0.3462(9) 0.1379(5) -0.2015(5) 0.0410(16) Uani 1 1 d U . . H13A H -0.2846 0.2014 -0.1975 0.049 Uiso 1 1 calc R . . C14 C -0.3203(8) 0.0834(5) -0.1393(4) 0.0337(15) Uani 1 1 d U . . C1' C 0.3986(11) 0.5628(6) 0.1216(5) 0.0492(19) Uani 1 1 d U . . H1'B H 0.3831 0.6256 0.1336 0.074 Uiso 1 1 calc R . . H1'C H 0.3464 0.5342 0.0654 0.074 Uiso 1 1 calc R . . H1'D H 0.5203 0.5668 0.1265 0.074 Uiso 1 1 calc R . . C2' C 0.3639(8) 0.5422(5) 0.2655(4) 0.0315(14) Uani 1 1 d U . . C3' C 0.4857(8) 0.6274(4) 0.2978(4) 0.0305(14) Uani 1 1 d U . . H3'A H 0.5474 0.6649 0.2627 0.037 Uiso 1 1 calc R . . C4' C 0.5126(8) 0.6548(4) 0.3851(4) 0.0297(14) Uani 1 1 d U . . C5' C 0.4240(8) 0.6025(4) 0.4384(4) 0.0299(14) Uani 1 1 d U . . H5'A H 0.4440 0.6240 0.4961 0.036 Uiso 1 1 calc R . . C6' C 0.3010(8) 0.5150(4) 0.4053(4) 0.0285(13) Uani 1 1 d U . . C7' C 0.2709(7) 0.4830(4) 0.3172(4) 0.0277(13) Uani 1 1 d U . . C8' C 0.2002(8) 0.4599(4) 0.4602(4) 0.0264(13) Uani 1 1 d U . . C9' C 0.0944(8) 0.4120(5) 0.5754(4) 0.0310(14) Uani 1 1 d U . . C10' C 0.0600(9) 0.4006(5) 0.6572(4) 0.0368(15) Uani 1 1 d U . . H10B H 0.1195 0.4449 0.7036 0.044 Uiso 1 1 calc R . . C11' C -0.0653(9) 0.3212(5) 0.6659(4) 0.0401(17) Uani 1 1 d U . . H11A H -0.0917 0.3111 0.7195 0.048 Uiso 1 1 calc R . . C12' C -0.1559(9) 0.2541(5) 0.5953(5) 0.0409(17) Uani 1 1 d U . . H12A H -0.2397 0.2006 0.6037 0.049 Uiso 1 1 calc R . . C13' C -0.1233(8) 0.2658(5) 0.5144(4) 0.0346(15) Uani 1 1 d U . . H13B H -0.1840 0.2221 0.4679 0.042 Uiso 1 1 calc R . . C14' C 0.0047(8) 0.3462(5) 0.5060(4) 0.0292(13) Uani 1 1 d U . . O1W O 0.4184(5) 0.3297(4) 0.1830(3) 0.0387(11) Uani 1 1 d U . . O2W O 0.2725(6) 0.3452(3) 0.0271(3) 0.0376(11) Uani 1 1 d U . . O3W O -0.1444(6) 0.2943(4) 0.1857(3) 0.0405(11) Uani 1 1 d U . . O4W O -0.0103(6) 0.4122(4) 0.0688(3) 0.0482(13) Uani 1 1 d U . . O5W O -0.893(3) -0.0028(13) -0.5181(15) 0.138(7) Uani 0.50 1 d PU . . 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 Yb1 0.02285(15) 0.03087(17) 0.02177(16) 0.00593(11) -0.00104(10) 0.00831(11) Br1 0.0458(4) 0.0348(4) 0.0663(5) 0.0179(4) -0.0024(4) 0.0104(3) Br1' 0.0333(3) 0.0321(4) 0.0499(4) 0.0038(3) -0.0078(3) 0.0024(3) Cl1 0.0284(8) 0.0503(10) 0.0248(8) -0.0021(7) -0.0046(6) 0.0094(7) Cl2 0.0300(8) 0.0437(9) 0.0356(9) -0.0020(7) -0.0004(7) 0.0112(7) Cl3 0.091(4) 0.071(3) 0.027(2) 0.011(2) 0.005(3) 0.058(3) Cl3' 0.102(4) 0.070(4) 0.032(2) -0.014(2) -0.026(3) 0.054(3) O1 0.038(2) 0.030(2) 0.028(2) 0.0040(19) -0.0098(19) 0.0086(19) O2 0.035(2) 0.034(2) 0.023(2) 0.0076(18) -0.0002(18) 0.0099(19) O1' 0.037(2) 0.033(2) 0.025(2) 0.0064(19) 0.0038(18) 0.0038(19) O2' 0.024(2) 0.032(2) 0.026(2) 0.0057(18) 0.0029(17) 0.0009(18) N1 0.031(3) 0.033(3) 0.030(3) -0.005(2) -0.004(2) 0.012(2) N2 0.033(3) 0.034(3) 0.028(3) 0.003(2) 0.001(2) 0.015(2) N1' 0.029(3) 0.036(3) 0.022(3) 0.005(2) -0.002(2) 0.012(2) N2' 0.029(3) 0.030(3) 0.026(3) 0.008(2) -0.001(2) 0.007(2) C1 0.034(3) 0.034(3) 0.026(3) 0.005(3) -0.006(3) 0.009(3) C2 0.026(3) 0.035(3) 0.031(3) 0.005(3) -0.002(3) 0.013(3) C3 0.029(3) 0.030(3) 0.034(3) 0.008(3) -0.003(3) 0.010(3) C4 0.033(3) 0.030(3) 0.045(4) 0.010(3) 0.003(3) 0.016(3) C5 0.028(3) 0.033(3) 0.036(3) -0.001(3) -0.001(3) 0.012(3) C6 0.026(3) 0.033(3) 0.026(3) 0.000(3) 0.003(2) 0.012(2) C7 0.026(3) 0.037(3) 0.028(3) 0.004(3) 0.002(2) 0.014(3) C8 0.023(3) 0.039(3) 0.027(3) -0.001(3) 0.002(2) 0.012(3) C9 0.029(3) 0.036(3) 0.030(3) -0.001(3) 0.002(3) 0.014(3) C10 0.028(3) 0.050(4) 0.035(4) -0.002(3) -0.005(3) 0.008(3) C11 0.037(4) 0.065(5) 0.033(4) 0.004(3) -0.009(3) 0.013(3) C12 0.046(4) 0.063(5) 0.032(4) 0.011(3) 0.001(3) 0.020(4) C13 0.043(4) 0.044(4) 0.040(4) 0.008(3) 0.005(3) 0.018(3) C14 0.028(3) 0.043(4) 0.030(3) -0.002(3) 0.002(3) 0.014(3) C1' 0.063(5) 0.047(4) 0.033(4) 0.013(3) 0.014(3) 0.000(3) C2' 0.030(3) 0.034(3) 0.033(3) 0.009(3) 0.003(3) 0.012(3) C3' 0.030(3) 0.030(3) 0.032(3) 0.010(3) 0.001(3) 0.008(3) C4' 0.023(3) 0.027(3) 0.038(4) 0.003(3) -0.004(3) 0.008(2) C5' 0.028(3) 0.033(3) 0.027(3) -0.002(3) -0.007(3) 0.012(3) C6' 0.023(3) 0.034(3) 0.028(3) 0.005(3) -0.004(2) 0.009(2) C7' 0.022(3) 0.032(3) 0.032(3) 0.008(3) -0.001(2) 0.011(2) C8' 0.028(3) 0.031(3) 0.023(3) 0.003(2) 0.000(2) 0.014(3) C9' 0.032(3) 0.037(3) 0.028(3) 0.008(3) 0.001(3) 0.017(3) C10' 0.040(3) 0.052(4) 0.026(3) 0.012(3) 0.006(3) 0.024(3) C11' 0.042(4) 0.059(4) 0.032(4) 0.017(3) 0.008(3) 0.029(3) C12' 0.038(4) 0.050(4) 0.041(4) 0.019(3) 0.007(3) 0.016(3) C13' 0.031(3) 0.036(3) 0.038(4) 0.015(3) 0.004(3) 0.008(3) C14' 0.030(3) 0.035(3) 0.025(3) 0.007(3) 0.001(2) 0.012(3) O1W 0.027(2) 0.065(3) 0.029(2) 0.012(2) 0.0002(18) 0.021(2) O2W 0.034(2) 0.051(3) 0.030(2) 0.014(2) 0.0035(19) 0.011(2) O3W 0.026(2) 0.062(3) 0.030(2) 0.001(2) -0.0002(18) 0.010(2) O4W 0.036(3) 0.055(3) 0.060(3) 0.030(3) -0.004(2) 0.015(2) O5W 0.171(11) 0.067(8) 0.156(11) 0.001(8) 0.013(9) 0.005(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O2' 2.201(4) . ? Yb1 O2 2.211(4) . ? Yb1 O4W 2.287(5) . ? Yb1 O1W 2.302(4) . ? Yb1 O3W 2.325(4) . ? Yb1 O2W 2.341(5) . ? Yb1 O1' 2.528(4) . ? Yb1 O1 2.530(4) . ? Yb1 C7' 3.159(6) . ? Yb1 C7 3.161(7) . ? Br1 C4 1.900(7) . ? Br1' C4' 1.900(6) . ? Cl3 Cl3' 0.887(7) . ? O1 C2 1.384(8) . ? O1 C1 1.430(7) . ? O2 C7 1.320(8) . ? O2 H2M 0.9300 . ? O1' C2' 1.389(8) . ? O1' C1' 1.437(8) . ? O2' C7' 1.318(7) . ? O2' H2'M 0.9300 . ? N1 C8 1.352(8) . ? N1 C9 1.391(8) . ? N1 H1A 0.8600 . ? N2 C8 1.324(8) . ? N2 C14 1.394(8) . ? N1' C8' 1.334(8) . ? N1' C9' 1.399(8) . ? N1' H1'A 0.8600 . ? N2' C8' 1.340(8) . ? N2' C14' 1.392(8) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.361(9) . ? C2 C7 1.425(9) . ? C3 C4 1.392(9) . ? C3 H3A 0.9300 . ? C4 C5 1.362(9) . ? C5 C6 1.414(9) . ? C5 H5A 0.9300 . ? C6 C7 1.406(9) . ? C6 C8 1.443(9) . ? C9 C10 1.381(9) . ? C9 C14 1.392(10) . ? C10 C11 1.367(11) . ? C10 H10A 0.9300 . ? C11 C12 1.394(11) . ? C11 H11B 0.9300 . ? C12 C13 1.389(10) . ? C12 H12B 0.9300 . ? C13 C14 1.401(10) . ? C13 H13A 0.9300 . ? C1' H1'B 0.9600 . ? C1' H1'C 0.9600 . ? C1' H1'D 0.9600 . ? C2' C3' 1.384(9) . ? C2' C7' 1.407(9) . ? C3' C4' 1.395(9) . ? C3' H3'A 0.9300 . ? C4' C5' 1.355(9) . ? C5' C6' 1.414(9) . ? C5' H5'A 0.9300 . ? C6' C7' 1.418(9) . ? C6' C8' 1.441(9) . ? C9' C14' 1.390(9) . ? C9' C10' 1.394(9) . ? C10' C11' 1.366(10) . ? C10' H10B 0.9300 . ? C11' C12' 1.414(10) . ? C11' H11A 0.9300 . ? C12' C13' 1.377(10) . ? C12' H12A 0.9300 . ? C13' C14' 1.387(9) . ? C13' H13B 0.9300 . ? 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' Yb1 O2 137.14(15) . . ? O2' Yb1 O4W 108.04(19) . . ? O2 Yb1 O4W 93.34(18) . . ? O2' Yb1 O1W 84.60(16) . . ? O2 Yb1 O1W 103.87(17) . . ? O4W Yb1 O1W 138.24(18) . . ? O2' Yb1 O3W 75.16(16) . . ? O2 Yb1 O3W 74.97(17) . . ? O4W Yb1 O3W 75.55(18) . . ? O1W Yb1 O3W 145.44(17) . . ? O2' Yb1 O2W 142.56(16) . . ? O2 Yb1 O2W 78.30(16) . . ? O4W Yb1 O2W 74.16(18) . . ? O1W Yb1 O2W 72.62(16) . . ? O3W Yb1 O2W 137.88(16) . . ? O2' Yb1 O1' 65.73(15) . . ? O2 Yb1 O1' 157.12(15) . . ? O4W Yb1 O1' 75.75(17) . . ? O1W Yb1 O1' 73.89(17) . . ? O3W Yb1 O1' 120.09(16) . . ? O2W Yb1 O1' 79.38(16) . . ? O2' Yb1 O1 77.41(15) . . ? O2 Yb1 O1 66.13(14) . . ? O4W Yb1 O1 148.65(16) . . ? O1W Yb1 O1 72.10(16) . . ? O3W Yb1 O1 76.28(17) . . ? O2W Yb1 O1 120.73(16) . . ? O1' Yb1 O1 131.41(14) . . ? O2' Yb1 C7' 19.77(16) . . ? O2 Yb1 C7' 155.95(16) . . ? O4W Yb1 C7' 102.88(18) . . ? O1W Yb1 C7' 75.57(16) . . ? O3W Yb1 C7' 91.85(16) . . ? O2W Yb1 C7' 122.99(16) . . ? O1' Yb1 C7' 46.61(15) . . ? O1 Yb1 C7' 91.47(15) . . ? O2' Yb1 C7 118.18(16) . . ? O2 Yb1 C7 19.96(16) . . ? O4W Yb1 C7 108.92(17) . . ? O1W Yb1 C7 98.39(17) . . ? O3W Yb1 C7 68.50(17) . . ? O2W Yb1 C7 94.71(17) . . ? O1' Yb1 C7 171.34(15) . . ? O1 Yb1 C7 46.83(15) . . ? C7' Yb1 C7 136.15(16) . . ? C2 O1 C1 117.0(5) . . ? C2 O1 Yb1 115.2(3) . . ? C1 O1 Yb1 127.7(4) . . ? C7 O2 Yb1 125.2(4) . . ? C7 O2 H2M 117.4 . . ? Yb1 O2 H2M 117.4 . . ? C2' O1' C1' 117.2(5) . . ? C2' O1' Yb1 114.5(4) . . ? C1' O1' Yb1 127.5(4) . . ? C7' O2' Yb1 125.8(4) . . ? C7' O2' H2'M 117.1 . . ? Yb1 O2' H2'M 117.1 . . ? C8 N1 C9 109.3(6) . . ? C8 N1 H1A 125.4 . . ? C9 N1 H1A 125.4 . . ? C8 N2 C14 109.4(5) . . ? C8' N1' C9' 109.5(5) . . ? C8' N1' H1'A 125.3 . . ? C9' N1' H1'A 125.3 . . ? C8' N2' C14' 109.7(5) . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C3 C2 O1 125.2(6) . . ? C3 C2 C7 122.5(6) . . ? O1 C2 C7 112.4(5) . . ? C2 C3 C4 118.7(6) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 122.0(6) . . ? C5 C4 Br1 119.6(5) . . ? C3 C4 Br1 118.3(5) . . ? C4 C5 C6 119.2(6) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C7 C6 C5 120.6(6) . . ? C7 C6 C8 118.9(6) . . ? C5 C6 C8 120.4(6) . . ? O2 C7 C6 124.2(6) . . ? O2 C7 C2 119.2(6) . . ? C6 C7 C2 116.6(6) . . ? O2 C7 Yb1 34.9(3) . . ? C6 C7 Yb1 156.5(4) . . ? C2 C7 Yb1 85.4(4) . . ? N2 C8 N1 108.7(6) . . ? N2 C8 C6 125.8(6) . . ? N1 C8 C6 125.4(6) . . ? C10 C9 N1 132.3(6) . . ? C10 C9 C14 121.9(6) . . ? N1 C9 C14 105.8(5) . . ? C11 C10 C9 116.3(7) . . ? C11 C10 H10A 121.9 . . ? C9 C10 H10A 121.9 . . ? C10 C11 C12 123.0(7) . . ? C10 C11 H11B 118.5 . . ? C12 C11 H11B 118.5 . . ? C13 C12 C11 121.2(7) . . ? C13 C12 H12B 119.4 . . ? C11 C12 H12B 119.4 . . ? C12 C13 C14 115.8(7) . . ? C12 C13 H13A 122.1 . . ? C14 C13 H13A 122.1 . . ? C9 C14 N2 106.8(6) . . ? C9 C14 C13 121.8(6) . . ? N2 C14 C13 131.4(6) . . ? O1' C1' H1'B 109.5 . . ? O1' C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? O1' C1' H1'D 109.5 . . ? H1'B C1' H1'D 109.5 . . ? H1'C C1' H1'D 109.5 . . ? C3' C2' O1' 125.1(6) . . ? C3' C2' C7' 122.5(6) . . ? O1' C2' C7' 112.4(5) . . ? C2' C3' C4' 117.6(6) . . ? C2' C3' H3'A 121.2 . . ? C4' C3' H3'A 121.2 . . ? C5' C4' C3' 122.9(6) . . ? C5' C4' Br1' 118.6(5) . . ? C3' C4' Br1' 118.4(5) . . ? C4' C5' C6' 119.4(6) . . ? C4' C5' H5'A 120.3 . . ? C6' C5' H5'A 120.3 . . ? C5' C6' C7' 120.0(6) . . ? C5' C6' C8' 120.5(6) . . ? C7' C6' C8' 119.5(5) . . ? O2' C7' C2' 119.1(6) . . ? O2' C7' C6' 123.4(6) . . ? C2' C7' C6' 117.5(6) . . ? O2' C7' Yb1 34.4(3) . . ? C2' C7' Yb1 85.3(4) . . ? C6' C7' Yb1 156.5(4) . . ? N1' C8' N2' 108.4(5) . . ? N1' C8' C6' 125.8(6) . . ? N2' C8' C6' 125.8(5) . . ? C14' C9' C10' 121.7(6) . . ? C14' C9' N1' 106.3(5) . . ? C10' C9' N1' 132.0(6) . . ? C11' C10' C9' 116.7(7) . . ? C11' C10' H10B 121.6 . . ? C9' C10' H10B 121.6 . . ? C10' C11' C12' 121.6(7) . . ? C10' C11' H11A 119.2 . . ? C12' C11' H11A 119.2 . . ? C13' C12' C11' 121.7(7) . . ? C13' C12' H12A 119.1 . . ? C11' C12' H12A 119.1 . . ? C12' C13' C14' 116.5(7) . . ? C12' C13' H13B 121.8 . . ? C14' C13' H13B 121.8 . . ? C13' C14' C9' 121.8(6) . . ? C13' C14' N2' 132.0(6) . . ? C9' C14' N2' 106.1(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.777 _refine_diff_density_min -1.335 _refine_diff_density_rms 0.158 # Attachment '- Complex-8.CIF' data_complex-8 _database_code_depnum_ccdc_archive 'CCDC 777200' #TrackingRef '- Complex-8.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H44 Br4 N8 Nd O9, 4(C H4 O), 3(Cl)' _chemical_formula_sum 'C60 H60 Br4 Cl3 N8 Nd O13' _chemical_formula_weight 1671.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 17.803(4) _cell_length_b 22.524(5) _cell_length_c 16.122(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.51(3) _cell_angle_gamma 90.00 _cell_volume 6376(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 11836 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3324 _exptl_absorpt_coefficient_mu 3.516 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.6206 _exptl_absorpt_correction_T_max 0.7426 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19198 _diffrn_reflns_av_R_equivalents 0.0959 _diffrn_reflns_av_sigmaI/netI 0.1120 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5592 _reflns_number_gt 3307 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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. Hydrogen atoms of water molecules were not added. ; _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^)+(0.0574P)^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 5592 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.0000 0.33854(2) 0.7500 0.03188(19) Uani 1 2 d SU . . Br1 Br 0.40502(4) 0.29359(4) 0.67310(5) 0.0505(3) Uani 1 1 d U . . Br1' Br 0.24578(4) 0.49055(3) 1.09821(5) 0.0424(2) Uani 1 1 d U . . Cl1 Cl 0.0000 0.51249(12) 0.7500 0.0481(7) Uani 1 2 d SU . . Cl2 Cl 0.03348(11) 0.12638(8) 0.95998(12) 0.0459(5) Uani 1 1 d U . . N1 N 0.3061(3) 0.4879(2) 0.8481(3) 0.0334(14) Uani 1 1 d U . . H1A H 0.3526 0.4768 0.8508 0.040 Uiso 1 1 calc R . . N2 N 0.1798(3) 0.4894(2) 0.8158(3) 0.0286(13) Uani 1 1 d U . . N1' N 0.3428(3) 0.2918(2) 0.9372(3) 0.0341(14) Uani 1 1 d U . . H1'A H 0.3709 0.3166 0.9690 0.041 Uiso 1 1 calc R . . N2' N 0.2418(3) 0.2467(2) 0.8670(3) 0.0347(15) Uani 1 1 d U . . O1 O 0.1055(3) 0.29683(19) 0.6599(3) 0.0360(12) Uani 1 1 d U . . O2 O 0.1089(2) 0.39610(19) 0.7420(3) 0.0321(11) Uani 1 1 d U . . H2M H 0.1048 0.4369 0.7492 0.048 Uiso 1 1 calc R . . O1' O 0.0176(2) 0.38428(19) 0.9025(3) 0.0356(12) Uani 1 1 d U . . O2' O 0.1032(2) 0.3003(2) 0.8576(3) 0.0338(12) Uani 1 1 d U . . H2N H 0.1170 0.2605 0.8598 0.051 Uiso 1 1 calc R . . C1 C 0.0987(4) 0.2459(3) 0.6064(4) 0.0411(19) Uani 1 1 d U . . H1B H 0.1444 0.2414 0.5826 0.062 Uiso 1 1 calc R . . H1C H 0.0560 0.2510 0.5620 0.062 Uiso 1 1 calc R . . H1D H 0.0910 0.2112 0.6386 0.062 Uiso 1 1 calc R . . C2 C 0.1768(4) 0.3216(3) 0.6835(4) 0.0310(17) Uani 1 1 d U . . C3 C 0.2440(4) 0.2981(3) 0.6664(4) 0.0360(18) Uani 1 1 d U . . H3A H 0.2442 0.2632 0.6357 0.043 Uiso 1 1 calc R . . C4 C 0.3123(4) 0.3281(3) 0.6960(4) 0.0387(19) Uani 1 1 d U . . C5 C 0.3140(4) 0.3801(3) 0.7413(4) 0.0345(18) Uani 1 1 d U . . H5A H 0.3600 0.3990 0.7604 0.041 Uiso 1 1 calc R . . C6 C 0.2455(4) 0.4040(3) 0.7582(4) 0.0285(17) Uani 1 1 d U . . C7 C 0.1746(4) 0.3760(3) 0.7283(4) 0.0270(16) Uani 1 1 d U . . C8 C 0.2437(4) 0.4590(3) 0.8059(4) 0.0316(17) Uani 1 1 d U . . C9 C 0.2815(4) 0.5385(3) 0.8860(4) 0.0356(18) Uani 1 1 d U . . C10 C 0.3212(4) 0.5829(3) 0.9359(4) 0.041(2) Uani 1 1 d U . . H10B H 0.3741 0.5827 0.9486 0.050 Uiso 1 1 calc R . . C11 C 0.2783(5) 0.6270(3) 0.9658(5) 0.048(2) Uani 1 1 d U . . H11B H 0.3030 0.6567 0.9999 0.057 Uiso 1 1 calc R . . C12 C 0.1985(5) 0.6279(3) 0.9456(5) 0.046(2) Uani 1 1 d U . . H12A H 0.1716 0.6585 0.9660 0.055 Uiso 1 1 calc R . . C13 C 0.1589(4) 0.5839(3) 0.8957(4) 0.041(2) Uani 1 1 d U . . H13B H 0.1060 0.5841 0.8829 0.049 Uiso 1 1 calc R . . C14 C 0.2028(4) 0.5391(3) 0.8657(4) 0.0339(18) Uani 1 1 d U . . C1' C -0.0328(4) 0.4259(3) 0.9341(5) 0.044(2) Uani 1 1 d U . . H1'B H -0.0130 0.4353 0.9916 0.066 Uiso 1 1 calc R . . H1'C H -0.0824 0.4086 0.9306 0.066 Uiso 1 1 calc R . . H1'D H -0.0363 0.4615 0.9010 0.066 Uiso 1 1 calc R . . C2' C 0.0947(4) 0.3871(3) 0.9378(4) 0.0305(17) Uani 1 1 d U . . C3' C 0.1260(4) 0.4306(3) 0.9921(4) 0.0318(17) Uani 1 1 d U . . H3'A H 0.0960 0.4608 1.0086 0.038 Uiso 1 1 calc R . . C4' C 0.2039(4) 0.4285(3) 1.0220(4) 0.0309(17) Uani 1 1 d U . . C5' C 0.2499(4) 0.3852(3) 0.9990(4) 0.0340(18) Uani 1 1 d U . . H5'A H 0.3019 0.3853 1.0195 0.041 Uiso 1 1 calc R . . C6' C 0.2167(4) 0.3394(3) 0.9423(4) 0.0285(16) Uani 1 1 d U . . C7' C 0.1373(4) 0.3387(3) 0.9110(4) 0.0310(17) Uani 1 1 d U . . C8' C 0.2663(4) 0.2949(3) 0.9164(4) 0.0289(16) Uani 1 1 d U . . C9' C 0.3691(4) 0.2423(3) 0.8993(4) 0.0331(18) Uani 1 1 d U . . C10' C 0.4444(4) 0.2219(3) 0.9016(4) 0.0379(19) Uani 1 1 d U . . H10A H 0.4861 0.2414 0.9320 0.046 Uiso 1 1 calc R . . C11' C 0.4522(4) 0.1710(3) 0.8555(4) 0.0381(19) Uani 1 1 d U . . H11A H 0.5006 0.1558 0.8546 0.046 Uiso 1 1 calc R . . C12' C 0.3883(5) 0.1416(3) 0.8097(5) 0.045(2) Uani 1 1 d U . . H12B H 0.3958 0.1076 0.7794 0.054 Uiso 1 1 calc R . . C13' C 0.3154(4) 0.1621(3) 0.8087(4) 0.0358(17) Uani 1 1 d U . . H13A H 0.2735 0.1424 0.7789 0.043 Uiso 1 1 calc R . . C14' C 0.3068(4) 0.2141(3) 0.8546(4) 0.0325(18) Uani 1 1 d U . . O1W O 0.0000 0.2312(3) 0.7500 0.0343(16) Uani 1 2 d SU . . C15 C 0.5268(5) 0.4682(4) 0.8724(6) 0.071(3) Uani 1 1 d U . . H15A H 0.5588 0.4667 0.9265 0.085 Uiso 1 1 calc R . . H15C H 0.5243 0.5082 0.8518 0.085 Uiso 1 1 calc R . . H15B H 0.5476 0.4429 0.8339 0.085 Uiso 1 1 calc R . . O3 O 0.4532(3) 0.4486(3) 0.8799(4) 0.0698(18) Uani 1 1 d U . . H3M H 0.4539 0.4339 0.9265 0.105 Uiso 1 1 calc R . . C16 C 0.1089(4) 0.1061(3) 0.7578(5) 0.052(2) Uani 1 1 d U . . H16C H 0.0583 0.1042 0.7260 0.062 Uiso 1 1 calc R . . H16B H 0.1189 0.0709 0.7914 0.062 Uiso 1 1 calc R . . H16A H 0.1451 0.1091 0.7200 0.062 Uiso 1 1 calc R . . O4 O 0.1154(3) 0.1577(2) 0.8120(3) 0.0454(13) Uani 1 1 d U . . H4M H 0.0964 0.1504 0.8539 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0247(3) 0.0364(3) 0.0361(4) 0.000 0.0097(3) 0.000 Br1 0.0338(5) 0.0660(6) 0.0550(6) -0.0018(4) 0.0168(4) 0.0120(4) Br1' 0.0440(5) 0.0432(5) 0.0399(5) -0.0080(4) 0.0065(4) -0.0026(4) Cl1 0.0302(16) 0.0493(16) 0.066(2) 0.000 0.0135(14) 0.000 Cl2 0.0388(12) 0.0542(12) 0.0452(12) 0.0008(10) 0.0080(10) -0.0060(10) N1 0.028(3) 0.041(3) 0.032(3) -0.002(3) 0.006(3) -0.001(3) N2 0.036(3) 0.028(3) 0.025(3) -0.002(3) 0.014(3) 0.006(3) N1' 0.027(4) 0.040(3) 0.037(3) -0.004(3) 0.009(3) -0.004(3) N2' 0.037(4) 0.034(3) 0.037(3) -0.003(3) 0.016(3) 0.000(3) O1 0.031(3) 0.037(3) 0.041(3) -0.010(2) 0.008(2) -0.003(2) O2 0.031(3) 0.030(3) 0.037(3) 0.001(2) 0.009(2) 0.005(2) O1' 0.023(3) 0.043(3) 0.043(3) -0.005(2) 0.011(2) 0.008(2) O2' 0.032(3) 0.030(3) 0.041(3) 0.001(2) 0.011(2) 0.001(2) C1 0.046(5) 0.043(4) 0.037(4) -0.008(4) 0.017(4) -0.009(4) C2 0.028(4) 0.037(4) 0.029(4) 0.000(3) 0.008(3) -0.001(3) C3 0.037(5) 0.038(4) 0.035(4) 0.000(3) 0.012(4) 0.002(3) C4 0.031(4) 0.051(5) 0.038(4) -0.002(4) 0.017(3) 0.010(4) C5 0.027(4) 0.045(4) 0.034(4) 0.002(4) 0.013(3) -0.003(3) C6 0.026(4) 0.033(4) 0.027(4) 0.000(3) 0.005(3) 0.000(3) C7 0.024(4) 0.031(4) 0.028(4) 0.008(3) 0.012(3) 0.002(3) C8 0.030(4) 0.038(4) 0.028(4) 0.005(3) 0.007(3) -0.005(3) C9 0.035(4) 0.039(4) 0.034(4) -0.001(3) 0.010(3) -0.011(3) C10 0.033(4) 0.056(5) 0.036(4) -0.003(4) 0.010(4) -0.022(4) C11 0.069(6) 0.040(4) 0.038(4) 0.001(4) 0.018(4) -0.016(4) C12 0.055(5) 0.043(4) 0.044(4) -0.006(4) 0.016(4) -0.005(4) C13 0.045(5) 0.044(4) 0.036(4) -0.002(4) 0.015(4) -0.003(4) C14 0.034(4) 0.034(4) 0.036(4) -0.002(3) 0.012(3) -0.007(3) C1' 0.040(4) 0.046(4) 0.049(5) -0.010(4) 0.014(4) 0.007(4) C2' 0.029(4) 0.033(4) 0.032(4) 0.004(3) 0.011(3) 0.002(3) C3' 0.031(4) 0.034(4) 0.034(4) 0.000(3) 0.018(3) 0.004(3) C4' 0.032(4) 0.033(4) 0.027(4) -0.008(3) 0.004(3) -0.007(3) C5' 0.032(4) 0.042(4) 0.029(4) 0.008(3) 0.006(3) 0.008(3) C6' 0.026(4) 0.032(4) 0.030(4) 0.003(3) 0.013(3) 0.000(3) C7' 0.040(4) 0.030(4) 0.025(4) 0.000(3) 0.010(3) -0.001(3) C8' 0.024(4) 0.033(4) 0.032(4) 0.001(3) 0.011(3) -0.005(3) C9' 0.033(4) 0.038(4) 0.031(4) 0.006(3) 0.014(3) 0.001(3) C10' 0.036(4) 0.041(4) 0.039(4) 0.003(4) 0.010(3) 0.003(3) C11' 0.032(4) 0.049(4) 0.034(4) 0.012(4) 0.009(3) 0.016(4) C12' 0.052(5) 0.047(4) 0.041(4) -0.001(4) 0.019(4) 0.014(4) C13' 0.033(4) 0.040(4) 0.035(4) -0.002(4) 0.006(3) -0.006(3) C14' 0.028(4) 0.043(4) 0.029(4) 0.011(3) 0.012(3) 0.004(3) O1W 0.028(4) 0.040(4) 0.035(4) 0.000 0.005(3) 0.000 C15 0.066(6) 0.074(5) 0.073(6) 0.017(5) 0.014(5) -0.011(5) O3 0.045(4) 0.090(4) 0.072(4) 0.024(3) 0.004(3) -0.005(3) C16 0.043(5) 0.060(5) 0.052(5) -0.002(4) 0.008(4) 0.001(4) O4 0.042(3) 0.052(3) 0.045(3) -0.007(3) 0.014(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O2 2.354(4) . ? Nd1 O2 2.354(4) 2_556 ? Nd1 O1W 2.417(6) . ? Nd1 O2' 2.464(5) 2_556 ? Nd1 O2' 2.464(5) . ? Nd1 O1' 2.637(5) . ? Nd1 O1' 2.637(5) 2_556 ? Nd1 O1 2.725(4) 2_556 ? Nd1 O1 2.725(4) . ? Br1 C4 1.915(7) . ? Br1' C4' 1.927(6) . ? N1 C8 1.367(8) . ? N1 C9 1.398(8) . ? N1 H1A 0.8600 . ? N2 C8 1.359(8) . ? N2 C14 1.400(8) . ? N1' C8' 1.350(8) . ? N1' C9' 1.389(8) . ? N1' H1'A 0.8600 . ? N2' C8' 1.373(8) . ? N2' C14' 1.412(8) . ? O1 C2 1.381(8) . ? O1 C1 1.427(7) . ? O2 C7 1.307(7) . ? O2 H2M 0.9300 . ? O1' C2' 1.398(8) . ? O1' C1' 1.447(7) . ? O2' C7' 1.298(8) . ? O2' H2N 0.9300 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.377(9) . ? C2 C7 1.426(9) . ? C3 C4 1.403(10) . ? C3 H3A 0.9300 . ? C4 C5 1.378(9) . ? C5 C6 1.400(9) . ? C5 H5A 0.9300 . ? C6 C7 1.423(9) . ? C6 C8 1.461(9) . ? C9 C14 1.385(10) . ? C9 C10 1.399(9) . ? C10 C11 1.388(10) . ? C10 H10B 0.9300 . ? C11 C12 1.403(10) . ? C11 H11B 0.9300 . ? C12 C13 1.392(10) . ? C12 H12A 0.9300 . ? C13 C14 1.410(9) . ? C13 H13B 0.9300 . ? C1' H1'B 0.9600 . ? C1' H1'C 0.9600 . ? C1' H1'D 0.9600 . ? C2' C3' 1.370(9) . ? C2' C7' 1.436(9) . ? C3' C4' 1.392(9) . ? C3' H3'A 0.9300 . ? C4' C5' 1.364(9) . ? C5' C6' 1.438(9) . ? C5' H5'A 0.9300 . ? C6' C7' 1.420(9) . ? C6' C8' 1.443(9) . ? C9' C14' 1.375(9) . ? C9' C10' 1.412(9) . ? C10' C11' 1.386(9) . ? C10' H10A 0.9300 . ? C11' C12' 1.414(10) . ? C11' H11A 0.9300 . ? C12' C13' 1.375(10) . ? C12' H12B 0.9300 . ? C13' C14' 1.408(9) . ? C13' H13A 0.9300 . ? C15 O3 1.406(9) . ? C15 H15A 0.9600 . ? C15 H15C 0.9600 . ? C15 H15B 0.9600 . ? O3 H3M 0.8200 . ? C16 O4 1.448(8) . ? C16 H16C 0.9600 . ? C16 H16B 0.9600 . ? C16 H16A 0.9600 . ? O4 H4M 0.8200 . ? 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 Nd1 O2 113.2(2) . 2_556 ? O2 Nd1 O1W 123.42(11) . . ? O2 Nd1 O1W 123.42(11) 2_556 . ? O2 Nd1 O2' 132.74(15) . 2_556 ? O2 Nd1 O2' 72.90(14) 2_556 2_556 ? O1W Nd1 O2' 69.57(11) . 2_556 ? O2 Nd1 O2' 72.90(14) . . ? O2 Nd1 O2' 132.74(15) 2_556 . ? O1W Nd1 O2' 69.57(11) . . ? O2' Nd1 O2' 139.1(2) 2_556 . ? O2 Nd1 O1' 82.19(14) . . ? O2 Nd1 O1' 72.87(14) 2_556 . ? O1W Nd1 O1' 113.00(10) . . ? O2' Nd1 O1' 138.84(14) 2_556 . ? O2' Nd1 O1' 61.31(14) . . ? O2 Nd1 O1' 72.87(14) . 2_556 ? O2 Nd1 O1' 82.19(14) 2_556 2_556 ? O1W Nd1 O1' 113.00(10) . 2_556 ? O2' Nd1 O1' 61.31(14) 2_556 2_556 ? O2' Nd1 O1' 138.84(14) . 2_556 ? O1' Nd1 O1' 134.00(19) . 2_556 ? O2 Nd1 O1 150.00(14) . 2_556 ? O2 Nd1 O1 60.90(14) 2_556 2_556 ? O1W Nd1 O1 69.83(9) . 2_556 ? O2' Nd1 O1 75.85(14) 2_556 2_556 ? O2' Nd1 O1 90.21(14) . 2_556 ? O1' Nd1 O1 67.89(14) . 2_556 ? O1' Nd1 O1 130.23(13) 2_556 2_556 ? O2 Nd1 O1 60.90(14) . . ? O2 Nd1 O1 150.00(14) 2_556 . ? O1W Nd1 O1 69.83(9) . . ? O2' Nd1 O1 90.21(14) 2_556 . ? O2' Nd1 O1 75.85(14) . . ? O1' Nd1 O1 130.23(13) . . ? O1' Nd1 O1 67.89(14) 2_556 . ? O1 Nd1 O1 139.67(19) 2_556 . ? C8 N1 C9 108.6(6) . . ? C8 N1 H1A 125.7 . . ? C9 N1 H1A 125.7 . . ? C8 N2 C14 107.5(6) . . ? C8' N1' C9' 109.4(6) . . ? C8' N1' H1'A 125.3 . . ? C9' N1' H1'A 125.3 . . ? C8' N2' C14' 107.7(6) . . ? C2 O1 C1 118.3(5) . . ? C2 O1 Nd1 113.4(4) . . ? C1 O1 Nd1 127.0(4) . . ? C7 O2 Nd1 125.9(4) . . ? C7 O2 H2M 117.0 . . ? Nd1 O2 H2M 117.0 . . ? C2' O1' C1' 116.8(5) . . ? C2' O1' Nd1 110.8(4) . . ? C1' O1' Nd1 126.6(4) . . ? C7' O2' Nd1 116.6(4) . . ? C7' O2' H2N 121.7 . . ? Nd1 O2' H2N 121.7 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C3 C2 O1 125.4(6) . . ? C3 C2 C7 121.9(6) . . ? O1 C2 C7 112.7(6) . . ? C2 C3 C4 118.7(7) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 122.1(6) . . ? C5 C4 Br1 120.2(6) . . ? C3 C4 Br1 117.7(5) . . ? C4 C5 C6 119.1(6) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C5 C6 C7 121.1(6) . . ? C5 C6 C8 121.6(6) . . ? C7 C6 C8 117.3(6) . . ? O2 C7 C6 123.9(6) . . ? O2 C7 C2 118.9(6) . . ? C6 C7 C2 117.1(6) . . ? N2 C8 N1 109.2(6) . . ? N2 C8 C6 125.5(6) . . ? N1 C8 C6 125.4(6) . . ? C14 C9 N1 106.4(6) . . ? C14 C9 C10 121.6(7) . . ? N1 C9 C10 131.9(7) . . ? C11 C10 C9 117.1(7) . . ? C11 C10 H10B 121.4 . . ? C9 C10 H10B 121.4 . . ? C10 C11 C12 121.6(7) . . ? C10 C11 H11B 119.2 . . ? C12 C11 H11B 119.2 . . ? C13 C12 C11 121.4(7) . . ? C13 C12 H12A 119.3 . . ? C11 C12 H12A 119.3 . . ? C12 C13 C14 116.8(7) . . ? C12 C13 H13B 121.6 . . ? C14 C13 H13B 121.6 . . ? C9 C14 N2 108.4(6) . . ? C9 C14 C13 121.5(7) . . ? N2 C14 C13 130.1(7) . . ? O1' C1' H1'B 109.5 . . ? O1' C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? O1' C1' H1'D 109.5 . . ? H1'B C1' H1'D 109.5 . . ? H1'C C1' H1'D 109.5 . . ? C3' C2' O1' 124.2(6) . . ? C3' C2' C7' 123.8(7) . . ? O1' C2' C7' 112.1(6) . . ? C2' C3' C4' 118.3(6) . . ? C2' C3' H3'A 120.8 . . ? C4' C3' H3'A 120.8 . . ? C5' C4' C3' 122.6(6) . . ? C5' C4' Br1' 120.4(5) . . ? C3' C4' Br1' 117.0(5) . . ? C4' C5' C6' 118.9(6) . . ? C4' C5' H5'A 120.5 . . ? C6' C5' H5'A 120.5 . . ? C7' C6' C5' 121.0(6) . . ? C7' C6' C8' 120.6(6) . . ? C5' C6' C8' 118.4(6) . . ? O2' C7' C6' 125.0(6) . . ? O2' C7' C2' 119.5(6) . . ? C6' C7' C2' 115.4(6) . . ? N1' C8' N2' 108.3(6) . . ? N1' C8' C6' 127.2(6) . . ? N2' C8' C6' 124.5(6) . . ? C14' C9' N1' 107.4(6) . . ? C14' C9' C10' 123.0(7) . . ? N1' C9' C10' 129.6(7) . . ? C11' C10' C9' 115.7(7) . . ? C11' C10' H10A 122.2 . . ? C9' C10' H10A 122.2 . . ? C10' C11' C12' 121.6(7) . . ? C10' C11' H11A 119.2 . . ? C12' C11' H11A 119.2 . . ? C13' C12' C11' 121.7(7) . . ? C13' C12' H12B 119.2 . . ? C11' C12' H12B 119.2 . . ? C12' C13' C14' 117.3(7) . . ? C12' C13' H13A 121.4 . . ? C14' C13' H13A 121.4 . . ? C9' C14' C13' 120.7(6) . . ? C9' C14' N2' 107.2(6) . . ? C13' C14' N2' 132.1(7) . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C15 O3 H3M 109.5 . . ? O4 C16 H16C 109.5 . . ? O4 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? O4 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? C16 O4 H4M 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.071 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.129 # Attachment '- Complex-9.CIF' data_complex-9 _database_code_depnum_ccdc_archive 'CCDC 777201' #TrackingRef '- Complex-9.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H44 Br4 Gd N8 O9, 4(C H4 O), 3(Cl)' _chemical_formula_sum 'C60 H60 Br4 Cl3 Gd N8 O13' _chemical_formula_weight 1684.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 17.595(4) _cell_length_b 22.565(5) _cell_length_c 16.060(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.41(3) _cell_angle_gamma 90.00 _cell_volume 6291(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6480 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3340 _exptl_absorpt_coefficient_mu 3.792 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5821 _exptl_absorpt_correction_T_max 0.8044 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10591 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5508 _reflns_number_gt 4377 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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. Hydrogen atoms of water molecules were not added. ; _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^)+(0.0323P)^2^+3.1390P] 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 5508 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.0000 0.336382(13) 0.7500 0.01756(9) Uani 1 2 d SU . . Br1 Br 0.40378(3) 0.29641(2) 0.67310(3) 0.03855(14) Uani 1 1 d U . . Br1' Br 0.24500(3) 0.48913(2) 1.09794(3) 0.02999(13) Uani 1 1 d U . . Cl1 Cl 0.0000 0.51795(7) 0.7500 0.0332(4) Uani 1 2 d SU . . Cl2 Cl 0.03257(6) 0.12719(5) 0.96112(7) 0.0319(3) Uani 1 1 d U . . N1 N 0.30383(19) 0.48842(15) 0.8473(2) 0.0240(8) Uani 1 1 d U . . H1A H 0.3508 0.4773 0.8491 0.029 Uiso 1 1 calc R . . N2 N 0.17771(19) 0.49012(15) 0.81646(19) 0.0213(8) Uani 1 1 d U . . N1' N 0.34202(18) 0.29218(15) 0.93706(19) 0.0213(8) Uani 1 1 d U . . H1'A H 0.3700 0.3171 0.9691 0.026 Uiso 1 1 calc R . . N2' N 0.24132(18) 0.24716(15) 0.86754(19) 0.0198(8) Uani 1 1 d U . . O1 O 0.10260(15) 0.29791(12) 0.66165(16) 0.0230(6) Uani 1 1 d U . . O2 O 0.10505(14) 0.39573(12) 0.74512(16) 0.0189(6) Uani 1 1 d U . . H2M H 0.0998 0.4362 0.7540 0.028 Uiso 1 1 calc R . . O1' O 0.01619(15) 0.38493(12) 0.90008(16) 0.0230(6) Uani 1 1 d U . . O2' O 0.10147(15) 0.30007(12) 0.85758(16) 0.0194(6) Uani 1 1 d U . . H2N H 0.1153 0.2603 0.8611 0.029 Uiso 1 1 calc R . . C1 C 0.0959(3) 0.2476(2) 0.6061(3) 0.0314(11) Uani 1 1 d U . . H1B H 0.1152 0.2577 0.5554 0.047 Uiso 1 1 calc R . . H1C H 0.0427 0.2363 0.5922 0.047 Uiso 1 1 calc R . . H1D H 0.1252 0.2152 0.6336 0.047 Uiso 1 1 calc R . . C2 C 0.1743(2) 0.32285(18) 0.6849(2) 0.0211(9) Uani 1 1 d U . . C3 C 0.2417(2) 0.29976(19) 0.6675(2) 0.0226(10) Uani 1 1 d U . . H3A H 0.2420 0.2648 0.6368 0.027 Uiso 1 1 calc R . . C4 C 0.3102(2) 0.3297(2) 0.6969(3) 0.0251(10) Uani 1 1 d U . . C5 C 0.3121(2) 0.38111(19) 0.7413(2) 0.0234(10) Uani 1 1 d U . . H5A H 0.3587 0.4001 0.7601 0.028 Uiso 1 1 calc R . . C6 C 0.2417(2) 0.40547(18) 0.7588(2) 0.0195(9) Uani 1 1 d U . . C7 C 0.1718(2) 0.37647(17) 0.7307(2) 0.0189(9) Uani 1 1 d U . . C8 C 0.2415(2) 0.45969(18) 0.8062(2) 0.0199(9) Uani 1 1 d U . . C9 C 0.2806(2) 0.5386(2) 0.8860(2) 0.0253(10) Uani 1 1 d U . . C10 C 0.3213(3) 0.5824(2) 0.9354(3) 0.0316(11) Uani 1 1 d U . . H10B H 0.3748 0.5821 0.9480 0.038 Uiso 1 1 calc R . . C11 C 0.2785(3) 0.6262(2) 0.9647(3) 0.0357(12) Uani 1 1 d U . . H11B H 0.3038 0.6559 0.9985 0.043 Uiso 1 1 calc R . . C12 C 0.1983(3) 0.6277(2) 0.9455(3) 0.0365(12) Uani 1 1 d U . . H12A H 0.1718 0.6584 0.9665 0.044 Uiso 1 1 calc R . . C13 C 0.1572(3) 0.58453(19) 0.8959(2) 0.0280(10) Uani 1 1 d U . . H13B H 0.1037 0.5853 0.8832 0.034 Uiso 1 1 calc R . . C14 C 0.2004(2) 0.53980(18) 0.8661(2) 0.0229(10) Uani 1 1 d U . . C1' C -0.0342(2) 0.4268(2) 0.9312(3) 0.0288(10) Uani 1 1 d U . . H1'B H -0.0143 0.4363 0.9889 0.043 Uiso 1 1 calc R . . H1'C H -0.0847 0.4099 0.9276 0.043 Uiso 1 1 calc R . . H1'D H -0.0371 0.4623 0.8977 0.043 Uiso 1 1 calc R . . C2' C 0.0925(2) 0.38711(18) 0.9366(2) 0.0202(9) Uani 1 1 d U . . C3' C 0.1243(2) 0.43054(18) 0.9910(2) 0.0210(9) Uani 1 1 d U . . H3'A H 0.0942 0.4610 1.0070 0.025 Uiso 1 1 calc R . . C4' C 0.2032(2) 0.42783(18) 1.0218(2) 0.0200(9) Uani 1 1 d U . . C5' C 0.2488(2) 0.38435(18) 0.9989(2) 0.0201(9) Uani 1 1 d U . . H5'A H 0.3014 0.3841 1.0194 0.024 Uiso 1 1 calc R . . C6' C 0.2155(2) 0.33921(17) 0.9431(2) 0.0175(9) Uani 1 1 d U . . C7' C 0.1358(2) 0.33934(18) 0.9104(2) 0.0172(9) Uani 1 1 d U . . C8' C 0.2647(2) 0.29461(18) 0.9167(2) 0.0203(9) Uani 1 1 d U . . C9' C 0.3696(2) 0.24384(18) 0.8990(2) 0.0213(9) Uani 1 1 d U . . C10' C 0.4443(2) 0.2236(2) 0.8999(3) 0.0262(10) Uani 1 1 d U . . H10A H 0.4867 0.2432 0.9297 0.031 Uiso 1 1 calc R . . C11' C 0.4520(3) 0.1730(2) 0.8542(3) 0.0304(11) Uani 1 1 d U . . H11A H 0.5012 0.1581 0.8531 0.036 Uiso 1 1 calc R . . C12' C 0.3887(3) 0.1432(2) 0.8094(3) 0.0323(11) Uani 1 1 d U . . H12B H 0.3966 0.1090 0.7796 0.039 Uiso 1 1 calc R . . C13' C 0.3152(3) 0.16353(19) 0.8086(3) 0.0277(10) Uani 1 1 d U . . H13A H 0.2729 0.1439 0.7786 0.033 Uiso 1 1 calc R . . C14' C 0.3063(2) 0.21464(19) 0.8545(2) 0.0205(9) Uani 1 1 d U . . C15 C 0.5259(3) 0.4699(3) 0.8726(4) 0.0553(15) Uani 1 1 d U . . H15A H 0.5583 0.4685 0.9268 0.066 Uiso 1 1 calc R . . H15C H 0.5225 0.5100 0.8522 0.066 Uiso 1 1 calc R . . H15B H 0.5473 0.4452 0.8336 0.066 Uiso 1 1 calc R . . O3 O 0.45245(18) 0.44959(17) 0.8800(2) 0.0551(10) Uani 1 1 d U . . H3B H 0.4557 0.4166 0.9018 0.066 Uiso 1 1 calc R . . C16 C 0.1097(3) 0.1084(2) 0.7579(3) 0.0381(12) Uani 1 1 d U . . H16C H 0.0588 0.1061 0.7256 0.046 Uiso 1 1 calc R . . H16B H 0.1203 0.0729 0.7908 0.046 Uiso 1 1 calc R . . H16A H 0.1466 0.1124 0.7204 0.046 Uiso 1 1 calc R . . O4 O 0.11460(16) 0.15856(13) 0.81276(17) 0.0296(7) Uani 1 1 d U . . H4M H 0.0952 0.1504 0.8544 0.044 Uiso 1 1 calc R . . O1W O 0.0000 0.23238(17) 0.7500 0.0247(9) Uani 1 2 d SU . . 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 0.01118(15) 0.01977(16) 0.02129(16) 0.000 0.00131(11) 0.000 Br1 0.0212(3) 0.0533(3) 0.0426(3) -0.0013(2) 0.0094(2) 0.0125(2) Br1' 0.0301(3) 0.0302(3) 0.0271(2) -0.00865(19) -0.00279(19) -0.0025(2) Cl1 0.0179(8) 0.0264(9) 0.0546(10) 0.000 0.0042(7) 0.000 Cl2 0.0239(6) 0.0367(7) 0.0329(6) 0.0014(5) -0.0017(5) -0.0049(5) N1 0.0134(18) 0.032(2) 0.0255(18) 0.0011(16) 0.0008(15) -0.0030(16) N2 0.0220(19) 0.0231(19) 0.0191(17) -0.0009(15) 0.0041(14) 0.0004(16) N1' 0.0161(18) 0.0251(19) 0.0216(17) -0.0019(15) 0.0003(14) -0.0005(15) N2' 0.0189(18) 0.0196(18) 0.0209(17) -0.0008(15) 0.0037(14) 0.0008(15) O1 0.0173(15) 0.0222(15) 0.0292(15) -0.0072(13) 0.0027(12) -0.0010(13) O2 0.0149(15) 0.0155(14) 0.0264(14) -0.0004(12) 0.0039(12) 0.0028(12) O1' 0.0142(15) 0.0282(16) 0.0267(15) -0.0070(13) 0.0031(12) 0.0045(13) O2' 0.0167(15) 0.0155(14) 0.0250(14) -0.0005(12) 0.0000(12) 0.0032(12) C1 0.037(3) 0.030(3) 0.029(2) -0.010(2) 0.009(2) -0.007(2) C2 0.017(2) 0.026(2) 0.019(2) 0.0033(17) 0.0007(17) 0.0017(18) C3 0.023(2) 0.025(2) 0.019(2) -0.0011(18) 0.0028(18) 0.0053(19) C4 0.018(2) 0.034(3) 0.024(2) 0.002(2) 0.0053(18) 0.009(2) C5 0.014(2) 0.032(2) 0.024(2) 0.0040(19) 0.0012(17) -0.0010(19) C6 0.015(2) 0.024(2) 0.019(2) 0.0064(18) 0.0030(16) 0.0016(18) C7 0.018(2) 0.019(2) 0.0192(19) 0.0046(17) 0.0013(17) 0.0031(18) C8 0.018(2) 0.026(2) 0.0167(19) 0.0046(18) 0.0041(17) -0.0014(19) C9 0.024(2) 0.031(3) 0.020(2) 0.0033(19) 0.0018(18) -0.007(2) C10 0.030(3) 0.037(3) 0.026(2) -0.001(2) -0.001(2) -0.014(2) C11 0.050(3) 0.030(3) 0.026(2) -0.004(2) 0.003(2) -0.017(2) C12 0.050(3) 0.031(3) 0.031(2) -0.004(2) 0.012(2) -0.003(2) C13 0.030(3) 0.029(2) 0.026(2) -0.002(2) 0.0053(19) -0.002(2) C14 0.024(2) 0.025(2) 0.019(2) 0.0031(18) 0.0037(18) -0.0065(19) C1' 0.019(2) 0.039(3) 0.029(2) -0.011(2) 0.0046(18) 0.009(2) C2' 0.014(2) 0.027(2) 0.019(2) 0.0002(18) 0.0012(17) 0.0011(18) C3' 0.020(2) 0.022(2) 0.022(2) 0.0003(18) 0.0038(17) 0.0037(18) C4' 0.022(2) 0.021(2) 0.0159(19) -0.0018(17) 0.0006(17) -0.0064(19) C5' 0.016(2) 0.026(2) 0.0180(19) 0.0002(18) 0.0004(17) -0.0014(19) C6' 0.016(2) 0.019(2) 0.0183(19) 0.0010(17) 0.0061(16) 0.0018(18) C7' 0.018(2) 0.020(2) 0.0143(18) 0.0031(17) 0.0024(16) 0.0014(18) C8' 0.018(2) 0.028(2) 0.0147(19) 0.0023(18) 0.0012(16) -0.0019(19) C9' 0.023(2) 0.025(2) 0.0156(19) 0.0012(18) 0.0005(17) 0.0018(19) C10' 0.015(2) 0.037(3) 0.026(2) 0.003(2) 0.0020(18) 0.004(2) C11' 0.024(2) 0.039(3) 0.029(2) 0.011(2) 0.009(2) 0.014(2) C12' 0.034(3) 0.031(3) 0.033(2) 0.001(2) 0.009(2) 0.011(2) C13' 0.028(2) 0.028(2) 0.027(2) 0.001(2) 0.0051(19) -0.001(2) C14' 0.016(2) 0.029(2) 0.0176(19) 0.0046(18) 0.0040(17) 0.0047(19) C15 0.041(3) 0.061(4) 0.062(3) 0.017(3) 0.002(3) -0.005(3) O3 0.0256(19) 0.070(3) 0.066(2) 0.032(2) -0.0032(17) -0.0021(18) C16 0.037(3) 0.039(3) 0.037(3) -0.002(2) 0.003(2) 0.008(2) O4 0.0264(17) 0.0320(17) 0.0300(16) -0.0002(14) 0.0034(13) 0.0027(14) O1W 0.019(2) 0.024(2) 0.029(2) 0.000 0.0000(17) 0.000 _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 2.294(3) . ? Gd1 O2 2.294(3) 2_556 ? Gd1 O1W 2.347(4) . ? Gd1 O2' 2.416(3) 2_556 ? Gd1 O2' 2.416(3) . ? Gd1 O1 2.620(3) 2_556 ? Gd1 O1 2.620(3) . ? Gd1 O1' 2.620(3) . ? Gd1 O1' 2.620(3) 2_556 ? Br1 C4 1.904(4) . ? Br1' C4' 1.912(4) . ? N1 C8 1.349(5) . ? N1 C9 1.385(5) . ? N1 H1A 0.8600 . ? N2 C8 1.349(5) . ? N2 C14 1.396(5) . ? N1' C8' 1.348(5) . ? N1' C9' 1.378(5) . ? N1' H1'A 0.8600 . ? N2' C8' 1.354(5) . ? N2' C14' 1.403(5) . ? O1 C2 1.376(5) . ? O1 C1 1.437(5) . ? O2 C7 1.308(5) . ? O2 H2M 0.9300 . ? O1' C2' 1.376(4) . ? O1' C1' 1.440(5) . ? O2' C7' 1.305(5) . ? O2' H2N 0.9300 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.365(6) . ? C2 C7 1.420(6) . ? C3 C4 1.395(6) . ? C3 H3A 0.9300 . ? C4 C5 1.359(6) . ? C5 C6 1.425(5) . ? C5 H5A 0.9300 . ? C6 C7 1.401(5) . ? C6 C8 1.442(6) . ? C9 C10 1.392(6) . ? C9 C14 1.394(6) . ? C10 C11 1.370(6) . ? C10 H10B 0.9300 . ? C11 C12 1.395(7) . ? C11 H11B 0.9300 . ? C12 C13 1.384(6) . ? C12 H12A 0.9300 . ? C13 C14 1.395(6) . ? C13 H13B 0.9300 . ? C1' H1'B 0.9600 . ? C1' H1'C 0.9600 . ? C1' H1'D 0.9600 . ? C2' C3' 1.370(6) . ? C2' C7' 1.423(6) . ? C3' C4' 1.397(5) . ? C3' H3'A 0.9300 . ? C4' C5' 1.356(6) . ? C5' C6' 1.418(5) . ? C5' H5'A 0.9300 . ? C6' C7' 1.414(5) . ? C6' C8' 1.436(6) . ? C9' C14' 1.387(6) . ? C9' C10' 1.388(6) . ? C10' C11' 1.376(6) . ? C10' H10A 0.9300 . ? C11' C12' 1.395(6) . ? C11' H11A 0.9300 . ? C12' C13' 1.372(6) . ? C12' H12B 0.9300 . ? C13' C14' 1.391(6) . ? C13' H13A 0.9300 . ? C15 O3 1.394(6) . ? C15 H15A 0.9600 . ? C15 H15C 0.9600 . ? C15 H15B 0.9600 . ? O3 H3B 0.8200 . ? C16 O4 1.429(5) . ? C16 H16C 0.9600 . ? C16 H16B 0.9600 . ? C16 H16A 0.9600 . ? O4 H4M 0.8200 . ? 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 O2 108.57(13) . 2_556 ? O2 Gd1 O1W 125.72(6) . . ? O2 Gd1 O1W 125.71(6) 2_556 . ? O2 Gd1 O2' 132.76(9) . 2_556 ? O2 Gd1 O2' 73.57(9) 2_556 2_556 ? O1W Gd1 O2' 70.17(6) . 2_556 ? O2 Gd1 O2' 73.57(9) . . ? O2 Gd1 O2' 132.76(9) 2_556 . ? O1W Gd1 O2' 70.17(6) . . ? O2' Gd1 O2' 140.34(13) 2_556 . ? O2 Gd1 O1 147.38(9) . 2_556 ? O2 Gd1 O1 62.91(9) 2_556 2_556 ? O1W Gd1 O1 70.65(6) . 2_556 ? O2' Gd1 O1 77.34(9) 2_556 2_556 ? O2' Gd1 O1 89.68(8) . 2_556 ? O2 Gd1 O1 62.91(9) . . ? O2 Gd1 O1 147.38(9) 2_556 . ? O1W Gd1 O1 70.65(6) . . ? O2' Gd1 O1 89.68(8) 2_556 . ? O2' Gd1 O1 77.34(9) . . ? O1 Gd1 O1 141.30(12) 2_556 . ? O2 Gd1 O1' 79.65(9) . . ? O2 Gd1 O1' 72.03(9) 2_556 . ? O1W Gd1 O1' 114.71(6) . . ? O2' Gd1 O1' 139.12(8) 2_556 . ? O2' Gd1 O1' 61.81(9) . . ? O1 Gd1 O1' 67.74(9) 2_556 . ? O1 Gd1 O1' 130.98(8) . . ? O2 Gd1 O1' 72.03(9) . 2_556 ? O2 Gd1 O1' 79.65(9) 2_556 2_556 ? O1W Gd1 O1' 114.71(6) . 2_556 ? O2' Gd1 O1' 61.81(9) 2_556 2_556 ? O2' Gd1 O1' 139.12(8) . 2_556 ? O1 Gd1 O1' 130.98(8) 2_556 2_556 ? O1 Gd1 O1' 67.74(9) . 2_556 ? O1' Gd1 O1' 130.57(12) . 2_556 ? C8 N1 C9 109.6(3) . . ? C8 N1 H1A 125.2 . . ? C9 N1 H1A 125.2 . . ? C8 N2 C14 108.2(3) . . ? C8' N1' C9' 109.9(3) . . ? C8' N1' H1'A 125.1 . . ? C9' N1' H1'A 125.1 . . ? C8' N2' C14' 108.9(3) . . ? C2 O1 C1 118.1(3) . . ? C2 O1 Gd1 113.6(2) . . ? C1 O1 Gd1 127.1(2) . . ? C7 O2 Gd1 124.3(2) . . ? C7 O2 H2M 117.8 . . ? Gd1 O2 H2M 117.8 . . ? C2' O1' C1' 116.2(3) . . ? C2' O1' Gd1 111.1(2) . . ? C1' O1' Gd1 127.8(2) . . ? C7' O2' Gd1 116.4(2) . . ? C7' O2' H2N 121.8 . . ? Gd1 O2' H2N 121.8 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C3 C2 O1 125.3(4) . . ? C3 C2 C7 122.1(4) . . ? O1 C2 C7 112.6(3) . . ? C2 C3 C4 118.5(4) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 122.4(4) . . ? C5 C4 Br1 119.6(3) . . ? C3 C4 Br1 117.9(3) . . ? C4 C5 C6 119.0(4) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C7 C6 C5 120.1(4) . . ? C7 C6 C8 119.3(4) . . ? C5 C6 C8 120.6(4) . . ? O2 C7 C6 123.6(4) . . ? O2 C7 C2 118.6(4) . . ? C6 C7 C2 117.7(4) . . ? N1 C8 N2 108.8(4) . . ? N1 C8 C6 126.5(4) . . ? N2 C8 C6 124.8(4) . . ? N1 C9 C10 132.4(4) . . ? N1 C9 C14 106.0(3) . . ? C10 C9 C14 121.6(4) . . ? C11 C10 C9 116.5(4) . . ? C11 C10 H10B 121.7 . . ? C9 C10 H10B 121.7 . . ? C10 C11 C12 122.3(4) . . ? C10 C11 H11B 118.8 . . ? C12 C11 H11B 118.8 . . ? C13 C12 C11 121.7(4) . . ? C13 C12 H12A 119.2 . . ? C11 C12 H12A 119.2 . . ? C12 C13 C14 116.3(4) . . ? C12 C13 H13B 121.9 . . ? C14 C13 H13B 121.9 . . ? C9 C14 C13 121.6(4) . . ? C9 C14 N2 107.4(4) . . ? C13 C14 N2 131.0(4) . . ? O1' C1' H1'B 109.5 . . ? O1' C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? O1' C1' H1'D 109.5 . . ? H1'B C1' H1'D 109.5 . . ? H1'C C1' H1'D 109.5 . . ? C3' C2' O1' 124.5(4) . . ? C3' C2' C7' 123.2(4) . . ? O1' C2' C7' 112.3(3) . . ? C2' C3' C4' 118.2(4) . . ? C2' C3' H3'A 120.9 . . ? C4' C3' H3'A 120.9 . . ? C5' C4' C3' 122.2(4) . . ? C5' C4' Br1' 121.0(3) . . ? C3' C4' Br1' 116.8(3) . . ? C4' C5' C6' 119.3(4) . . ? C4' C5' H5'A 120.4 . . ? C6' C5' H5'A 120.4 . . ? C7' C6' C5' 121.0(4) . . ? C7' C6' C8' 120.0(4) . . ? C5' C6' C8' 118.9(3) . . ? O2' C7' C6' 124.4(4) . . ? O2' C7' C2' 119.6(3) . . ? C6' C7' C2' 116.0(3) . . ? N1' C8' N2' 107.9(3) . . ? N1' C8' C6' 126.2(4) . . ? N2' C8' C6' 125.9(4) . . ? N1' C9' C14' 107.0(3) . . ? N1' C9' C10' 131.1(4) . . ? C14' C9' C10' 121.9(4) . . ? C11' C10' C9' 116.3(4) . . ? C11' C10' H10A 121.8 . . ? C9' C10' H10A 121.8 . . ? C10' C11' C12' 122.3(4) . . ? C10' C11' H11A 118.9 . . ? C12' C11' H11A 118.9 . . ? C13' C12' C11' 121.1(4) . . ? C13' C12' H12B 119.4 . . ? C11' C12' H12B 119.4 . . ? C12' C13' C14' 117.3(4) . . ? C12' C13' H13A 121.3 . . ? C14' C13' H13A 121.3 . . ? C9' C14' C13' 121.1(4) . . ? C9' C14' N2' 106.3(3) . . ? C13' C14' N2' 132.6(4) . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C15 O3 H3B 109.5 . . ? O4 C16 H16C 109.5 . . ? O4 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? O4 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? C16 O4 H4M 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.736 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.104 # Attachment '- Complex-10.CIF' data_complex-10 _database_code_depnum_ccdc_archive 'CCDC 777202' #TrackingRef '- Complex-10.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H44 Br4 Eu N8 O9, 4(C H4 O), 3(Cl)' _chemical_formula_sum 'C60 H60 Br4 Cl3 Eu N8 O13' _chemical_formula_weight 1679.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 17.720(4) _cell_length_b 22.332(5) _cell_length_c 16.130(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.52(3) _cell_angle_gamma 90.00 _cell_volume 6295(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6575 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 3.733 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.5695 _exptl_absorpt_correction_T_max 0.7544 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10762 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5549 _reflns_number_gt 4377 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _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. Hydrogen atoms of water molecules were not added. ; _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^)+(0.0349P)^2^+3.1960P] 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 5549 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Eu1 Eu 0.0000 0.338587(15) 0.7500 0.02081(11) Uani 1 2 d SU . . Br1 Br 0.40491(3) 0.29351(3) 0.67311(3) 0.03478(15) Uani 1 1 d U . . Br1' Br 0.24571(3) 0.49044(2) 1.09837(3) 0.02651(13) Uani 1 1 d U . . Cl1 Cl 0.0000 0.51259(8) 0.7500 0.0323(4) Uani 1 2 d SU . . Cl2 Cl 0.03352(6) 0.12643(6) 0.96002(7) 0.0293(3) Uani 1 1 d U . . N1 N 0.30610(19) 0.48800(17) 0.8476(2) 0.0201(8) Uani 1 1 d U . . H1A H 0.3529 0.4769 0.8498 0.024 Uiso 1 1 calc R . . N2 N 0.1810(2) 0.48944(16) 0.8164(2) 0.0185(8) Uani 1 1 d U . . N1' N 0.34260(19) 0.29158(16) 0.9376(2) 0.0174(8) Uani 1 1 d U . . H1'A H 0.3706 0.3165 0.9697 0.021 Uiso 1 1 calc R . . N2' N 0.24251(19) 0.24734(16) 0.8672(2) 0.0174(8) Uani 1 1 d U . . O1 O 0.10519(16) 0.29707(13) 0.66000(18) 0.0212(7) Uani 1 1 d U . . O2 O 0.10882(15) 0.39590(13) 0.74243(17) 0.0167(6) Uani 1 1 d U . . H2M H 0.1048 0.4370 0.7496 0.025 Uiso 1 1 calc R . . O1' O 0.01739(15) 0.38439(14) 0.90286(17) 0.0195(7) Uani 1 1 d U . . O2' O 0.10352(15) 0.30009(13) 0.85807(17) 0.0168(6) Uani 1 1 d U . . H2N H 0.1176 0.2599 0.8608 0.025 Uiso 1 1 calc R . . C1 C 0.0986(3) 0.2460(2) 0.6063(3) 0.0292(11) Uani 1 1 d U . . H1B H 0.1171 0.2558 0.5553 0.044 Uiso 1 1 calc R . . H1C H 0.0459 0.2341 0.5932 0.044 Uiso 1 1 calc R . . H1D H 0.1282 0.2137 0.6341 0.044 Uiso 1 1 calc R . . C2 C 0.1771(2) 0.3219(2) 0.6834(3) 0.0177(10) Uani 1 1 d U . . C3 C 0.2441(2) 0.2975(2) 0.6665(3) 0.0205(10) Uani 1 1 d U . . H3A H 0.2441 0.2621 0.6361 0.025 Uiso 1 1 calc R . . C4 C 0.3122(2) 0.3276(2) 0.6965(3) 0.0212(10) Uani 1 1 d U . . C5 C 0.3142(2) 0.3794(2) 0.7416(3) 0.0196(10) Uani 1 1 d U . . H5A H 0.3607 0.3980 0.7612 0.024 Uiso 1 1 calc R . . C6 C 0.2451(2) 0.4044(2) 0.7584(3) 0.0176(10) Uani 1 1 d U . . C7 C 0.1745(2) 0.3756(2) 0.7291(2) 0.0167(9) Uani 1 1 d U . . C8 C 0.2441(2) 0.4590(2) 0.8060(2) 0.0172(10) Uani 1 1 d U . . C9 C 0.2820(2) 0.5385(2) 0.8862(3) 0.0222(10) Uani 1 1 d U . . C10 C 0.3222(3) 0.5832(2) 0.9363(3) 0.0285(12) Uani 1 1 d U . . H10B H 0.3753 0.5834 0.9491 0.034 Uiso 1 1 calc R . . C11 C 0.2790(3) 0.6263(2) 0.9649(3) 0.0317(12) Uani 1 1 d U . . H11B H 0.3036 0.6565 0.9988 0.038 Uiso 1 1 calc R . . C12 C 0.1991(3) 0.6271(2) 0.9456(3) 0.0331(12) Uani 1 1 d U . . H12A H 0.1723 0.6578 0.9667 0.040 Uiso 1 1 calc R . . C13 C 0.1595(3) 0.5838(2) 0.8964(3) 0.0253(11) Uani 1 1 d U . . H13B H 0.1063 0.5843 0.8835 0.030 Uiso 1 1 calc R . . C14 C 0.2026(2) 0.5394(2) 0.8666(3) 0.0203(10) Uani 1 1 d U . . C1' C -0.0322(2) 0.4268(2) 0.9345(3) 0.0261(11) Uani 1 1 d U . . H1'B H -0.0122 0.4360 0.9920 0.039 Uiso 1 1 calc R . . H1'C H -0.0825 0.4098 0.9309 0.039 Uiso 1 1 calc R . . H1'D H -0.0351 0.4627 0.9015 0.039 Uiso 1 1 calc R . . C2' C 0.0944(2) 0.3869(2) 0.9384(2) 0.0154(9) Uani 1 1 d U . . C3' C 0.1254(2) 0.4307(2) 0.9924(3) 0.0169(9) Uani 1 1 d U . . H3'A H 0.0951 0.4610 1.0089 0.020 Uiso 1 1 calc R . . C4' C 0.2043(2) 0.4287(2) 1.0224(2) 0.0181(10) Uani 1 1 d U . . C5' C 0.2497(2) 0.38549(19) 0.9991(2) 0.0162(9) Uani 1 1 d U . . H5'A H 0.3020 0.3857 1.0192 0.019 Uiso 1 1 calc R . . C6' C 0.2168(2) 0.33966(19) 0.9435(2) 0.0148(9) Uani 1 1 d U . . C7' C 0.1371(2) 0.33929(19) 0.9109(2) 0.0154(9) Uani 1 1 d U . . C8' C 0.2652(2) 0.2950(2) 0.9169(3) 0.0179(10) Uani 1 1 d U . . C9' C 0.3698(2) 0.2426(2) 0.8997(3) 0.0176(10) Uani 1 1 d U . . C10' C 0.4439(2) 0.2221(2) 0.9009(3) 0.0228(10) Uani 1 1 d U . . H10A H 0.4860 0.2417 0.9310 0.027 Uiso 1 1 calc R . . C11' C 0.4514(3) 0.1713(2) 0.8554(3) 0.0284(11) Uani 1 1 d U . . H11A H 0.5001 0.1560 0.8547 0.034 Uiso 1 1 calc R . . C12' C 0.3885(3) 0.1417(2) 0.8100(3) 0.0273(11) Uani 1 1 d U . . H12B H 0.3964 0.1074 0.7799 0.033 Uiso 1 1 calc R . . C13' C 0.3149(3) 0.1623(2) 0.8087(3) 0.0257(11) Uani 1 1 d U . . H13A H 0.2729 0.1426 0.7785 0.031 Uiso 1 1 calc R . . C14' C 0.3066(2) 0.2136(2) 0.8546(3) 0.0177(10) Uani 1 1 d U . . C15 C 0.5265(3) 0.4676(3) 0.8720(4) 0.0518(16) Uani 1 1 d U . . H1WA H 0.5589 0.4663 0.9259 0.062 Uiso 1 1 calc R . . H1WC H 0.5243 0.5078 0.8508 0.062 Uiso 1 1 calc R . . H1WB H 0.5468 0.4417 0.8336 0.062 Uiso 1 1 calc R . . O3 O 0.45375(19) 0.4489(2) 0.8801(2) 0.0514(11) Uani 1 1 d U . . H3B H 0.4561 0.4155 0.9017 0.062 Uiso 1 1 calc R . . C16 C 0.1094(3) 0.1068(2) 0.7581(3) 0.0344(12) Uani 1 1 d U . . H2WC H 0.0587 0.1047 0.7261 0.041 Uiso 1 1 calc R . . H2WB H 0.1197 0.0711 0.7913 0.041 Uiso 1 1 calc R . . H2WA H 0.1459 0.1103 0.7206 0.041 Uiso 1 1 calc R . . O4 O 0.11507(17) 0.15760(14) 0.81210(19) 0.0261(7) Uani 1 1 d U . . H3WD H 0.0959 0.1498 0.8537 0.039 Uiso 1 1 calc R . . O1W O 0.0000 0.23158(19) 0.7500 0.0208(10) Uani 1 2 d SU . . 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 0.01323(17) 0.0251(2) 0.02353(18) 0.000 0.00135(13) 0.000 Br1 0.0184(2) 0.0480(4) 0.0394(3) -0.0011(3) 0.0091(2) 0.0125(2) Br1' 0.0276(3) 0.0264(3) 0.0232(2) -0.0078(2) -0.0026(2) -0.0031(2) Cl1 0.0162(8) 0.0297(10) 0.0510(11) 0.000 0.0054(8) 0.000 Cl2 0.0207(6) 0.0367(7) 0.0287(6) 0.0020(5) -0.0014(5) -0.0059(5) N1 0.0124(18) 0.026(2) 0.0213(19) 0.0007(17) 0.0016(15) -0.0018(16) N2 0.0214(19) 0.017(2) 0.0172(18) -0.0016(16) 0.0047(15) -0.0013(16) N1' 0.0126(17) 0.021(2) 0.0183(18) -0.0027(16) 0.0015(15) -0.0016(15) N2' 0.0148(17) 0.019(2) 0.0183(18) -0.0011(16) 0.0034(15) 0.0025(15) O1 0.0152(15) 0.0212(17) 0.0266(16) -0.0086(14) 0.0020(13) -0.0020(13) O2 0.0113(14) 0.0157(16) 0.0233(15) -0.0018(13) 0.0035(12) 0.0020(12) O1' 0.0105(14) 0.0249(18) 0.0222(15) -0.0080(13) -0.0003(12) 0.0049(13) O2' 0.0129(14) 0.0141(16) 0.0225(15) -0.0014(13) -0.0001(12) 0.0026(12) C1 0.033(3) 0.025(3) 0.030(3) -0.010(2) 0.008(2) -0.006(2) C2 0.015(2) 0.022(2) 0.016(2) 0.0009(18) 0.0004(18) -0.0008(18) C3 0.022(2) 0.022(2) 0.019(2) 0.0009(19) 0.0061(19) 0.0051(19) C4 0.013(2) 0.030(3) 0.021(2) 0.004(2) 0.0039(18) 0.0080(19) C5 0.009(2) 0.030(3) 0.020(2) 0.002(2) 0.0035(18) 0.0004(18) C6 0.015(2) 0.022(2) 0.014(2) 0.0039(18) 0.0007(17) -0.0001(18) C7 0.016(2) 0.020(2) 0.014(2) 0.0062(18) 0.0018(17) 0.0013(18) C8 0.016(2) 0.021(2) 0.014(2) 0.0062(18) 0.0022(18) -0.0047(19) C9 0.022(2) 0.028(3) 0.017(2) 0.003(2) 0.0052(19) -0.005(2) C10 0.028(2) 0.033(3) 0.023(2) 0.000(2) 0.000(2) -0.016(2) C11 0.043(3) 0.028(3) 0.024(2) -0.004(2) 0.004(2) -0.017(2) C12 0.047(3) 0.023(3) 0.029(3) -0.002(2) 0.009(2) 0.000(2) C13 0.027(2) 0.026(3) 0.024(2) -0.002(2) 0.007(2) -0.001(2) C14 0.023(2) 0.019(2) 0.019(2) 0.0001(19) 0.0047(19) -0.0055(19) C1' 0.014(2) 0.035(3) 0.028(2) -0.012(2) 0.0005(19) 0.009(2) C2' 0.011(2) 0.022(2) 0.013(2) 0.0009(18) 0.0039(17) 0.0016(18) C3' 0.016(2) 0.017(2) 0.019(2) -0.0005(18) 0.0067(18) 0.0037(18) C4' 0.020(2) 0.021(2) 0.013(2) -0.0006(18) 0.0020(18) -0.0034(19) C5' 0.014(2) 0.021(2) 0.013(2) 0.0015(18) -0.0009(17) -0.0008(18) C6' 0.015(2) 0.017(2) 0.0129(19) 0.0020(18) 0.0047(17) 0.0021(18) C7' 0.015(2) 0.016(2) 0.014(2) 0.0050(18) 0.0015(17) -0.0004(18) C8' 0.013(2) 0.027(3) 0.015(2) 0.0003(19) 0.0036(17) -0.0052(19) C9' 0.017(2) 0.023(2) 0.014(2) 0.0032(19) 0.0050(18) 0.0011(19) C10' 0.014(2) 0.030(3) 0.025(2) 0.005(2) 0.0029(19) 0.0021(19) C11' 0.023(2) 0.034(3) 0.030(3) 0.007(2) 0.007(2) 0.013(2) C12' 0.030(3) 0.025(3) 0.029(2) -0.001(2) 0.011(2) 0.010(2) C13' 0.025(2) 0.027(3) 0.026(2) -0.002(2) 0.005(2) -0.002(2) C14' 0.015(2) 0.024(3) 0.015(2) 0.0043(19) 0.0038(17) 0.0037(19) C15 0.042(3) 0.056(4) 0.057(4) 0.013(3) 0.007(3) -0.006(3) O3 0.0241(19) 0.067(3) 0.059(2) 0.028(2) -0.0054(18) -0.0027(19) C16 0.033(3) 0.036(3) 0.034(3) -0.001(2) 0.005(2) 0.006(2) O4 0.0255(17) 0.0270(19) 0.0257(16) -0.0002(15) 0.0038(14) 0.0023(14) O1W 0.015(2) 0.024(2) 0.023(2) 0.000 0.0024(18) 0.000 _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 O2 2.334(3) . ? Eu1 O2 2.334(3) 2_556 ? Eu1 O1W 2.390(4) . ? Eu1 O2' 2.467(3) 2_556 ? Eu1 O2' 2.467(3) . ? Eu1 O1' 2.640(3) . ? Eu1 O1' 2.640(3) 2_556 ? Eu1 O1 2.709(3) . ? Eu1 O1 2.709(3) 2_556 ? Eu1 C7' 3.248(4) . ? Eu1 C7' 3.248(4) 2_556 ? Br1 C4 1.905(4) . ? Br1' C4' 1.908(4) . ? N1 C8 1.354(5) . ? N1 C9 1.388(6) . ? N1 H1A 0.8600 . ? N2 C8 1.341(5) . ? N2 C14 1.394(6) . ? N1' C8' 1.359(5) . ? N1' C9' 1.378(6) . ? N1' H1'A 0.8600 . ? N2' C8' 1.352(6) . ? N2' C14' 1.405(5) . ? O1 C2 1.385(5) . ? O1 C1 1.426(5) . ? O2 C7 1.300(5) . ? O2 H2M 0.9300 . ? O1' C2' 1.392(5) . ? O1' C1' 1.442(5) . ? O2' C7' 1.296(5) . ? O2' H2N 0.9300 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.374(6) . ? C2 C7 1.411(6) . ? C3 C4 1.396(6) . ? C3 H3A 0.9300 . ? C4 C5 1.364(6) . ? C5 C6 1.413(6) . ? C5 H5A 0.9300 . ? C6 C7 1.417(6) . ? C6 C8 1.443(6) . ? C9 C14 1.391(6) . ? C9 C10 1.402(6) . ? C10 C11 1.356(7) . ? C10 H10B 0.9300 . ? C11 C12 1.398(7) . ? C11 H11B 0.9300 . ? C12 C13 1.369(7) . ? C12 H12A 0.9300 . ? C13 C14 1.386(6) . ? C13 H13B 0.9300 . ? C1' H1'B 0.9600 . ? C1' H1'C 0.9600 . ? C1' H1'D 0.9600 . ? C2' C3' 1.363(6) . ? C2' C7' 1.418(6) . ? C3' C4' 1.403(6) . ? C3' H3'A 0.9300 . ? C4' C5' 1.349(6) . ? C5' C6' 1.421(6) . ? C5' H5'A 0.9300 . ? C6' C7' 1.423(6) . ? C6' C8' 1.427(6) . ? C9' C10' 1.387(6) . ? C9' C14' 1.390(6) . ? C10' C11' 1.371(7) . ? C10' H10A 0.9300 . ? C11' C12' 1.394(7) . ? C11' H11A 0.9300 . ? C12' C13' 1.380(6) . ? C12' H12B 0.9300 . ? C13' C14' 1.385(6) . ? C13' H13A 0.9300 . ? C15 O3 1.381(6) . ? C15 H1WA 0.9600 . ? C15 H1WC 0.9600 . ? C15 H1WB 0.9600 . ? O3 H3B 0.8200 . ? C16 O4 1.424(6) . ? C16 H2WC 0.9600 . ? C16 H2WB 0.9600 . ? C16 H2WA 0.9600 . ? O4 H3WD 0.8200 . ? 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 Eu1 O2 113.50(14) . 2_556 ? O2 Eu1 O1W 123.25(7) . . ? O2 Eu1 O1W 123.25(7) 2_556 . ? O2 Eu1 O2' 132.71(9) . 2_556 ? O2 Eu1 O2' 72.78(9) 2_556 2_556 ? O1W Eu1 O2' 69.60(7) . 2_556 ? O2 Eu1 O2' 72.78(9) . . ? O2 Eu1 O2' 132.71(9) 2_556 . ? O1W Eu1 O2' 69.60(7) . . ? O2' Eu1 O2' 139.20(14) 2_556 . ? O2 Eu1 O1' 82.33(9) . . ? O2 Eu1 O1' 73.05(9) 2_556 . ? O1W Eu1 O1' 112.80(7) . . ? O2' Eu1 O1' 138.88(9) 2_556 . ? O2' Eu1 O1' 61.11(9) . . ? O2 Eu1 O1' 73.05(9) . 2_556 ? O2 Eu1 O1' 82.33(9) 2_556 2_556 ? O1W Eu1 O1' 112.80(7) . 2_556 ? O2' Eu1 O1' 61.11(9) 2_556 2_556 ? O2' Eu1 O1' 138.88(9) . 2_556 ? O1' Eu1 O1' 134.41(13) . 2_556 ? O2 Eu1 O1 60.79(9) . . ? O2 Eu1 O1 149.69(9) 2_556 . ? O1W Eu1 O1 69.98(6) . . ? O2' Eu1 O1 89.96(9) 2_556 . ? O2' Eu1 O1 76.24(9) . . ? O1' Eu1 O1 130.45(8) . . ? O1' Eu1 O1 67.44(9) 2_556 . ? O2 Eu1 O1 149.69(9) . 2_556 ? O2 Eu1 O1 60.79(9) 2_556 2_556 ? O1W Eu1 O1 69.98(7) . 2_556 ? O2' Eu1 O1 76.24(9) 2_556 2_556 ? O2' Eu1 O1 89.96(9) . 2_556 ? O1' Eu1 O1 67.44(9) . 2_556 ? O1' Eu1 O1 130.45(8) 2_556 2_556 ? O1 Eu1 O1 139.97(13) . 2_556 ? O2 Eu1 C7' 61.56(10) . . ? O2 Eu1 C7' 118.09(10) 2_556 . ? O1W Eu1 C7' 90.28(8) . . ? O2' Eu1 C7' 159.51(10) 2_556 . ? O2' Eu1 C7' 21.03(10) . . ? O1' Eu1 C7' 45.24(10) . . ? O1' Eu1 C7' 134.46(9) 2_556 . ? O1 Eu1 C7' 86.53(10) . . ? O1 Eu1 C7' 93.66(9) 2_556 . ? O2 Eu1 C7' 118.09(10) . 2_556 ? O2 Eu1 C7' 61.56(10) 2_556 2_556 ? O1W Eu1 C7' 90.28(8) . 2_556 ? O2' Eu1 C7' 21.03(10) 2_556 2_556 ? O2' Eu1 C7' 159.51(10) . 2_556 ? O1' Eu1 C7' 134.46(9) . 2_556 ? O1' Eu1 C7' 45.24(10) 2_556 2_556 ? O1 Eu1 C7' 93.66(9) . 2_556 ? O1 Eu1 C7' 86.53(10) 2_556 2_556 ? C7' Eu1 C7' 179.44(15) . 2_556 ? C8 N1 C9 109.0(4) . . ? C8 N1 H1A 125.5 . . ? C9 N1 H1A 125.5 . . ? C8 N2 C14 108.9(3) . . ? C8' N1' C9' 110.4(4) . . ? C8' N1' H1'A 124.8 . . ? C9' N1' H1'A 124.8 . . ? C8' N2' C14' 109.8(3) . . ? C2 O1 C1 117.8(3) . . ? C2 O1 Eu1 113.6(2) . . ? C1 O1 Eu1 127.2(3) . . ? C7 O2 Eu1 126.0(3) . . ? C7 O2 H2M 117.0 . . ? Eu1 O2 H2M 117.0 . . ? C2' O1' C1' 116.3(3) . . ? C2' O1' Eu1 110.8(2) . . ? C1' O1' Eu1 126.9(2) . . ? C7' O2' Eu1 115.9(2) . . ? C7' O2' H2N 122.1 . . ? Eu1 O2' H2N 122.1 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C3 C2 O1 125.0(4) . . ? C3 C2 C7 123.0(4) . . ? O1 C2 C7 112.0(4) . . ? C2 C3 C4 117.7(4) . . ? C2 C3 H3A 121.2 . . ? C4 C3 H3A 121.2 . . ? C5 C4 C3 122.6(4) . . ? C5 C4 Br1 119.8(3) . . ? C3 C4 Br1 117.6(3) . . ? C4 C5 C6 119.4(4) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C5 C6 C7 120.1(4) . . ? C5 C6 C8 121.6(4) . . ? C7 C6 C8 118.3(4) . . ? O2 C7 C2 119.4(4) . . ? O2 C7 C6 123.4(4) . . ? C2 C7 C6 117.2(4) . . ? N2 C8 N1 108.7(4) . . ? N2 C8 C6 125.3(4) . . ? N1 C8 C6 125.9(4) . . ? N1 C9 C14 106.5(4) . . ? N1 C9 C10 132.3(4) . . ? C14 C9 C10 121.2(4) . . ? C11 C10 C9 116.1(4) . . ? C11 C10 H10B 121.9 . . ? C9 C10 H10B 121.9 . . ? C10 C11 C12 122.8(5) . . ? C10 C11 H11B 118.6 . . ? C12 C11 H11B 118.6 . . ? C13 C12 C11 121.5(5) . . ? C13 C12 H12A 119.2 . . ? C11 C12 H12A 119.2 . . ? C12 C13 C14 116.6(4) . . ? C12 C13 H13B 121.7 . . ? C14 C13 H13B 121.7 . . ? C13 C14 C9 121.8(4) . . ? C13 C14 N2 131.3(4) . . ? C9 C14 N2 106.9(4) . . ? O1' C1' H1'B 109.5 . . ? O1' C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? O1' C1' H1'D 109.5 . . ? H1'B C1' H1'D 109.5 . . ? H1'C C1' H1'D 109.5 . . ? C3' C2' O1' 123.8(4) . . ? C3' C2' C7' 123.9(4) . . ? O1' C2' C7' 112.3(4) . . ? C2' C3' C4' 118.1(4) . . ? C2' C3' H3'A 120.9 . . ? C4' C3' H3'A 120.9 . . ? C5' C4' C3' 122.1(4) . . ? C5' C4' Br1' 120.8(3) . . ? C3' C4' Br1' 117.0(3) . . ? C4' C5' C6' 119.4(4) . . ? C4' C5' H5'A 120.3 . . ? C6' C5' H5'A 120.3 . . ? C5' C6' C7' 121.0(4) . . ? C5' C6' C8' 119.3(4) . . ? C7' C6' C8' 119.5(4) . . ? O2' C7' C2' 120.1(4) . . ? O2' C7' C6' 124.6(4) . . ? C2' C7' C6' 115.3(4) . . ? O2' C7' Eu1 43.11(18) . . ? C2' C7' Eu1 83.5(2) . . ? C6' C7' Eu1 149.4(3) . . ? N2' C8' N1' 106.9(4) . . ? N2' C8' C6' 126.4(4) . . ? N1' C8' C6' 126.6(4) . . ? N1' C9' C10' 130.9(4) . . ? N1' C9' C14' 106.9(4) . . ? C10' C9' C14' 122.2(4) . . ? C11' C10' C9' 116.2(4) . . ? C11' C10' H10A 121.9 . . ? C9' C10' H10A 121.9 . . ? C10' C11' C12' 122.2(4) . . ? C10' C11' H11A 118.9 . . ? C12' C11' H11A 118.9 . . ? C13' C12' C11' 121.4(5) . . ? C13' C12' H12B 119.3 . . ? C11' C12' H12B 119.3 . . ? C12' C13' C14' 116.9(4) . . ? C12' C13' H13A 121.6 . . ? C14' C13' H13A 121.6 . . ? C13' C14' C9' 121.1(4) . . ? C13' C14' N2' 132.9(4) . . ? C9' C14' N2' 106.0(4) . . ? O3 C15 H1WA 109.5 . . ? O3 C15 H1WC 109.5 . . ? H1WA C15 H1WC 109.5 . . ? O3 C15 H1WB 109.5 . . ? H1WA C15 H1WB 109.5 . . ? H1WC C15 H1WB 109.5 . . ? C15 O3 H3B 109.5 . . ? O4 C16 H2WC 109.5 . . ? O4 C16 H2WB 109.5 . . ? H2WC C16 H2WB 109.5 . . ? O4 C16 H2WA 109.5 . . ? H2WC C16 H2WA 109.5 . . ? H2WB C16 H2WA 109.5 . . ? C16 O4 H3WD 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.744 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.108