# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 777373' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H32 Br6 Cu6 N6 O16 Sm2), 7(H2 O)' _chemical_formula_sum ' C72 H78 Br12 Cu12 N12 O39 Sm4' _chemical_formula_weight 4058.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.851(4) _cell_length_b 14.822(6) _cell_length_c 20.233(9) _cell_angle_alpha 73.448(5) _cell_angle_beta 82.987(5) _cell_angle_gamma 77.721(5) _cell_volume 2761(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 8.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2178 _exptl_absorpt_correction_T_max 0.5405 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26322 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.20 _reflns_number_total 9910 _reflns_number_gt 7455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0560P)^2^+19.4128P] 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 9910 _refine_ls_number_parameters 682 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Sm1 Sm 0.66373(4) 0.95299(3) 0.18839(3) 0.02844(14) Uani 1 1 d . . . Sm2 Sm 0.12957(4) 0.94780(3) 0.20334(3) 0.02681(14) Uani 1 1 d . . . Br1 Br 0.50232(14) 0.57690(12) 0.13579(8) 0.0727(4) Uani 1 1 d . . . Br2 Br 0.37573(12) 0.38309(8) 0.05492(6) 0.0486(3) Uani 1 1 d . . . Br3 Br 0.96259(11) 0.50287(7) 0.33786(6) 0.0419(3) Uani 1 1 d . . . Br4 Br 0.78374(13) 0.32436(9) 0.27204(8) 0.0618(4) Uani 1 1 d . . . Br5 Br 0.67271(12) 0.37325(9) 0.49180(6) 0.0507(3) Uani 1 1 d . . . Br6 Br 1.01729(14) 0.18481(10) 0.43655(8) 0.0705(4) Uani 1 1 d . . . C1 C 0.0235(12) 0.5204(7) 0.1438(6) 0.048(3) Uani 1 1 d . . . H1 H 0.0400 0.4560 0.1445 0.057 Uiso 1 1 calc R . . C2 C -0.1104(11) 0.5665(8) 0.1483(6) 0.046(3) Uani 1 1 d . . . H2 H -0.1831 0.5334 0.1533 0.055 Uiso 1 1 calc R . . C3 C -0.1382(10) 0.6636(7) 0.1452(6) 0.040(2) Uani 1 1 d . . . H3 H -0.2293 0.6972 0.1464 0.048 Uiso 1 1 calc R . . C4 C -0.0267(9) 0.7085(7) 0.1404(5) 0.033(2) Uani 1 1 d . . . C5 C 0.1068(10) 0.6562(7) 0.1379(6) 0.042(3) Uani 1 1 d . . . H5 H 0.1812 0.6866 0.1358 0.050 Uiso 1 1 calc R . . C6 C -0.0461(10) 0.8130(7) 0.1390(6) 0.038(2) Uani 1 1 d . . . C7 C 0.8862(11) 0.3990(8) 0.0427(6) 0.045(3) Uani 1 1 d . . . H7 H 0.8957 0.4628 0.0267 0.054 Uiso 1 1 calc R . . C8 C 1.0047(11) 0.3319(8) 0.0489(7) 0.056(3) Uani 1 1 d . . . H8 H 1.0912 0.3499 0.0366 0.067 Uiso 1 1 calc R . . C9 C 0.9950(10) 0.2364(7) 0.0737(7) 0.052(3) Uani 1 1 d . . . H9 H 1.0741 0.1886 0.0800 0.063 Uiso 1 1 calc R . . C10 C 0.8641(9) 0.2148(6) 0.0888(5) 0.030(2) Uani 1 1 d . . . C11 C 0.7490(10) 0.2888(6) 0.0796(5) 0.035(2) Uani 1 1 d . . . H11 H 0.6610 0.2729 0.0893 0.042 Uiso 1 1 calc R . . C12 C 0.8418(9) 0.1133(7) 0.1152(5) 0.033(2) Uani 1 1 d . . . C13 C 0.5626(9) 0.6251(6) 0.2913(5) 0.030(2) Uani 1 1 d . . . H13 H 0.6468 0.6461 0.2781 0.036 Uiso 1 1 calc R . . C14 C 0.4409(8) 0.6898(6) 0.2720(5) 0.027(2) Uani 1 1 d . . . C15 C 0.3159(9) 0.6582(7) 0.2924(6) 0.039(2) Uani 1 1 d . . . H15 H 0.2319 0.6991 0.2800 0.047 Uiso 1 1 calc R . . C16 C 0.3182(10) 0.5652(8) 0.3314(6) 0.047(3) Uani 1 1 d . . . H16 H 0.2353 0.5427 0.3457 0.057 Uiso 1 1 calc R . . C17 C 0.4425(11) 0.5060(8) 0.3489(6) 0.047(3) Uani 1 1 d . . . H17 H 0.4419 0.4440 0.3764 0.057 Uiso 1 1 calc R . . C18 C 0.4477(9) 0.7897(6) 0.2283(5) 0.032(2) Uani 1 1 d . . . C19 C 1.0181(10) 0.2980(7) 0.5778(5) 0.034(2) Uani 1 1 d . . . H19 H 0.9305 0.2814 0.5873 0.041 Uiso 1 1 calc R . . C20 C 1.1174(9) 0.2537(6) 0.6259(5) 0.030(2) Uani 1 1 d . . . C21 C 1.2492(10) 0.2784(7) 0.6113(5) 0.036(2) Uani 1 1 d . . . H21 H 1.3196 0.2488 0.6414 0.044 Uiso 1 1 calc R . . C22 C 1.2725(11) 0.3485(8) 0.5507(6) 0.046(3) Uani 1 1 d . . . H22 H 1.3577 0.3685 0.5406 0.055 Uiso 1 1 calc R . . C23 C 1.1693(11) 0.3870(8) 0.5067(6) 0.044(3) Uani 1 1 d . . . H23 H 1.1871 0.4326 0.4660 0.053 Uiso 1 1 calc R . . C24 C 1.0823(10) 0.1839(7) 0.6905(6) 0.038(2) Uani 1 1 d . . . C25 C 0.5141(13) 0.1749(9) 0.4632(7) 0.058(3) Uani 1 1 d . . . H25 H 0.4953 0.2107 0.4954 0.070 Uiso 1 1 calc R . . C26 C 0.4140(13) 0.1258(11) 0.4567(7) 0.071(4) Uani 1 1 d . . . H26 H 0.3313 0.1273 0.4843 0.085 Uiso 1 1 calc R . . C27 C 0.4409(13) 0.0749(10) 0.4081(7) 0.060(3) Uani 1 1 d . . . H27 H 0.3751 0.0418 0.4022 0.072 Uiso 1 1 calc R . . C28 C 0.5636(10) 0.0723(8) 0.3683(6) 0.041(2) Uani 1 1 d . . . C29 C 0.6590(11) 0.1234(8) 0.3802(6) 0.050(3) Uani 1 1 d . . . H29 H 0.7437 0.1217 0.3542 0.060 Uiso 1 1 calc R . . C30 C 0.5982(10) 0.0226(7) 0.3126(6) 0.040(3) Uani 1 1 d . . . C31 C 1.1926(10) 0.2275(7) 0.2460(6) 0.038(2) Uani 1 1 d . . . H31 H 1.1179 0.1988 0.2448 0.046 Uiso 1 1 calc R . . C32 C 1.3203(8) 0.1924(6) 0.2178(5) 0.0248(19) Uani 1 1 d . . . C33 C 1.4342(10) 0.2344(7) 0.2208(5) 0.035(2) Uani 1 1 d . . . H33 H 1.5228 0.2120 0.2034 0.042 Uiso 1 1 calc R . . C34 C 1.4096(10) 0.3101(7) 0.2508(6) 0.043(3) Uani 1 1 d . . . H34 H 1.4825 0.3393 0.2538 0.052 Uiso 1 1 calc R . . C35 C 1.2785(10) 0.3418(7) 0.2758(6) 0.043(3) Uani 1 1 d . . . H35 H 1.2640 0.3942 0.2942 0.052 Uiso 1 1 calc R . . C36 C 1.3360(9) 0.1100(6) 0.1870(5) 0.027(2) Uani 1 1 d . . . Cu1 Cu 0.32821(15) 0.50302(11) 0.11462(9) 0.0633(4) Uani 1 1 d . . . Cu2 Cu 0.59362(16) 0.48721(10) 0.05298(9) 0.0650(5) Uani 1 1 d . . . Cu3 Cu 0.74107(15) 0.43905(11) 0.34141(10) 0.0681(5) Uani 1 1 d . . . Cu4 Cu 0.90164(17) 0.40014(12) 0.44665(8) 0.0603(4) Uani 1 1 d . . . Cu5 Cu 0.77388(16) 0.25655(11) 0.42846(10) 0.0640(4) Uani 1 1 d . . . Cu6 Cu 0.98540(15) 0.33135(13) 0.32708(10) 0.0675(5) Uani 1 1 d . . . N1 N 0.1342(9) 0.5629(6) 0.1385(5) 0.047(2) Uani 1 1 d . . . N2 N 0.7574(8) 0.3813(5) 0.0576(4) 0.0363(19) Uani 1 1 d . . . N3 N 0.5657(8) 0.5337(5) 0.3280(4) 0.0348(19) Uani 1 1 d . . . N4 N 1.0415(8) 0.3629(6) 0.5188(4) 0.038(2) Uani 1 1 d . . . N5 N 0.6346(9) 0.1742(7) 0.4266(5) 0.050(2) Uani 1 1 d . . . N6 N 1.1695(8) 0.3009(6) 0.2751(5) 0.043(2) Uani 1 1 d . . . O1 O 0.0557(7) 0.8408(5) 0.1513(4) 0.049(2) Uani 1 1 d . . . O2 O -0.1661(7) 0.8628(5) 0.1262(4) 0.0422(17) Uani 1 1 d . . . O3 O 0.7253(7) 0.0960(5) 0.1080(4) 0.0484(19) Uani 1 1 d . . . O4 O 0.9363(7) 0.0493(5) 0.1446(4) 0.0452(18) Uani 1 1 d . . . O5 O 0.3393(6) 0.8390(5) 0.2013(4) 0.0420(17) Uani 1 1 d . . . O6 O 0.5625(7) 0.8163(5) 0.2219(4) 0.053(2) Uani 1 1 d . . . O7 O 0.9591(7) 0.1671(5) 0.7015(4) 0.0471(19) Uani 1 1 d . . . O8 O 1.1752(7) 0.1438(6) 0.7328(4) 0.053(2) Uani 1 1 d . . . O9 O 0.5328(7) -0.0388(5) 0.3084(4) 0.0479(19) Uani 1 1 d . . . O10 O 0.6948(7) 0.0479(5) 0.2667(4) 0.0421(17) Uani 1 1 d . . . O11 O 1.2283(7) 0.0857(5) 0.1781(4) 0.0407(17) Uani 1 1 d . . . O12 O 1.4563(7) 0.0691(5) 0.1732(4) 0.0488(19) Uani 1 1 d . . . O1W O 0.5632(9) 0.9577(6) 0.0791(5) 0.066(2) Uani 1 1 d . . . O2W O 0.2584(8) 0.9317(6) 0.3090(4) 0.057(2) Uani 1 1 d . . . O3W O -0.0236(7) 1.0395(5) 0.2798(4) 0.0467(19) Uani 1 1 d . . . O4W O 0.2270(9) 0.9764(6) 0.0787(4) 0.059(2) Uani 1 1 d . . . O5W O 0.0720(14) 0.9680(8) 0.4148(6) 0.107(4) Uani 1 1 d . . . O6W O 0.0000 0.0000 0.0000 0.123(7) Uani 1 2 d S . . O7W O 0.4028(17) 0.8232(10) 0.0282(7) 0.135(5) Uani 1 1 d . . . O8W O 0.675(2) 0.8426(13) 0.9957(9) 0.196(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0155(2) 0.0218(2) 0.0456(3) -0.0053(2) -0.00294(19) -0.00277(17) Sm2 0.0156(2) 0.0226(2) 0.0409(3) -0.0053(2) -0.00520(19) -0.00317(17) Br1 0.0540(8) 0.1004(11) 0.0812(10) -0.0544(9) -0.0042(7) -0.0108(7) Br2 0.0430(6) 0.0413(6) 0.0572(7) -0.0105(5) -0.0036(5) -0.0019(5) Br3 0.0378(6) 0.0412(6) 0.0489(7) -0.0131(5) 0.0009(5) -0.0125(4) Br4 0.0520(7) 0.0570(7) 0.0839(10) -0.0199(7) -0.0196(7) -0.0166(6) Br5 0.0420(6) 0.0556(7) 0.0582(7) -0.0207(6) -0.0021(5) -0.0100(5) Br6 0.0568(8) 0.0587(8) 0.0868(11) -0.0120(7) -0.0070(7) 0.0001(6) C1 0.051(7) 0.030(6) 0.069(8) -0.016(5) -0.016(6) -0.009(5) C2 0.040(6) 0.044(6) 0.058(7) -0.010(5) -0.004(5) -0.020(5) C3 0.026(5) 0.041(6) 0.063(7) -0.027(5) -0.007(5) -0.005(4) C4 0.026(5) 0.035(5) 0.039(6) -0.011(4) -0.001(4) -0.008(4) C5 0.025(5) 0.041(6) 0.068(8) -0.029(5) 0.000(5) -0.007(4) C6 0.025(5) 0.039(6) 0.053(7) -0.021(5) -0.002(5) -0.001(4) C7 0.041(6) 0.037(6) 0.058(7) -0.002(5) -0.005(5) -0.021(5) C8 0.025(5) 0.048(7) 0.088(10) 0.000(6) -0.005(6) -0.014(5) C9 0.024(5) 0.035(6) 0.094(10) -0.009(6) -0.012(5) -0.001(4) C10 0.020(4) 0.024(5) 0.043(6) -0.002(4) -0.006(4) -0.005(4) C11 0.026(5) 0.031(5) 0.041(6) 0.002(4) 0.000(4) -0.009(4) C12 0.025(5) 0.034(5) 0.037(6) -0.008(4) -0.003(4) 0.000(4) C13 0.017(4) 0.032(5) 0.042(6) -0.008(4) -0.008(4) -0.004(4) C14 0.018(4) 0.020(4) 0.048(6) -0.018(4) -0.007(4) 0.001(3) C15 0.015(4) 0.035(6) 0.063(7) -0.013(5) -0.005(4) 0.001(4) C16 0.025(5) 0.050(7) 0.066(8) -0.007(6) 0.004(5) -0.020(5) C17 0.049(7) 0.034(6) 0.052(7) 0.002(5) -0.010(5) -0.010(5) C18 0.021(5) 0.028(5) 0.046(6) -0.013(4) 0.001(4) -0.001(4) C19 0.027(5) 0.041(6) 0.038(6) -0.011(5) -0.001(4) -0.014(4) C20 0.021(4) 0.023(5) 0.046(6) -0.010(4) -0.008(4) -0.001(4) C21 0.029(5) 0.039(6) 0.044(6) -0.015(5) 0.000(4) -0.008(4) C22 0.029(5) 0.052(7) 0.057(7) -0.012(6) 0.005(5) -0.020(5) C23 0.044(6) 0.043(6) 0.039(6) 0.000(5) 0.011(5) -0.016(5) C24 0.023(5) 0.033(5) 0.054(7) -0.008(5) -0.006(5) 0.002(4) C25 0.058(8) 0.064(8) 0.067(9) -0.041(7) 0.014(6) -0.018(6) C26 0.040(7) 0.123(12) 0.063(9) -0.048(9) 0.023(6) -0.027(7) C27 0.047(7) 0.078(9) 0.067(9) -0.027(7) 0.008(6) -0.032(6) C28 0.023(5) 0.048(6) 0.048(7) -0.014(5) -0.001(4) 0.000(4) C29 0.030(6) 0.060(7) 0.060(8) -0.017(6) -0.001(5) -0.010(5) C30 0.021(5) 0.033(5) 0.063(7) -0.005(5) -0.003(5) -0.006(4) C31 0.023(5) 0.034(5) 0.062(7) -0.019(5) -0.002(5) -0.005(4) C32 0.017(4) 0.026(5) 0.032(5) -0.006(4) -0.002(4) -0.007(3) C33 0.031(5) 0.032(5) 0.038(6) -0.003(4) -0.006(4) -0.004(4) C34 0.031(5) 0.036(6) 0.070(8) -0.015(5) -0.015(5) -0.014(4) C35 0.038(6) 0.037(6) 0.066(8) -0.023(5) -0.017(5) -0.012(5) C36 0.025(5) 0.015(4) 0.043(6) -0.008(4) -0.008(4) -0.002(3) Cu1 0.0451(8) 0.0539(9) 0.0884(12) -0.0277(8) -0.0142(8) 0.0134(7) Cu2 0.0545(9) 0.0409(8) 0.0862(12) -0.0155(8) 0.0069(8) 0.0116(7) Cu3 0.0411(8) 0.0431(8) 0.1070(14) -0.0060(8) -0.0214(8) 0.0103(6) Cu4 0.0635(10) 0.0711(10) 0.0451(9) -0.0044(7) -0.0143(7) -0.0191(8) Cu5 0.0512(9) 0.0573(9) 0.0937(13) -0.0314(9) -0.0043(8) -0.0171(7) Cu6 0.0341(8) 0.0810(11) 0.0977(13) -0.0516(10) 0.0070(8) -0.0018(7) N1 0.041(5) 0.038(5) 0.064(6) -0.024(5) -0.010(4) 0.004(4) N2 0.034(5) 0.030(4) 0.040(5) -0.004(4) -0.005(4) -0.001(3) N3 0.030(4) 0.024(4) 0.045(5) -0.003(4) -0.007(4) -0.001(3) N4 0.033(5) 0.040(5) 0.039(5) 0.001(4) -0.005(4) -0.011(4) N5 0.041(5) 0.052(6) 0.066(7) -0.032(5) 0.008(5) -0.015(4) N6 0.028(4) 0.046(5) 0.059(6) -0.024(5) -0.009(4) -0.002(4) O1 0.030(4) 0.040(4) 0.090(6) -0.038(4) -0.009(4) -0.007(3) O2 0.027(4) 0.041(4) 0.059(5) -0.020(4) -0.011(3) 0.008(3) O3 0.036(4) 0.032(4) 0.073(6) 0.000(4) -0.006(4) -0.015(3) O4 0.042(4) 0.027(4) 0.061(5) -0.006(3) -0.019(4) 0.007(3) O5 0.022(3) 0.036(4) 0.056(5) -0.001(3) 0.000(3) 0.003(3) O6 0.028(4) 0.029(4) 0.094(6) 0.002(4) -0.011(4) -0.013(3) O7 0.031(4) 0.044(4) 0.057(5) 0.005(4) 0.003(3) -0.015(3) O8 0.033(4) 0.064(5) 0.050(5) -0.004(4) -0.010(3) 0.005(4) O9 0.035(4) 0.056(5) 0.060(5) -0.025(4) 0.009(3) -0.020(4) O10 0.024(4) 0.046(4) 0.062(5) -0.022(4) 0.000(3) -0.012(3) O11 0.027(4) 0.034(4) 0.064(5) -0.017(3) -0.002(3) -0.008(3) O12 0.027(4) 0.048(4) 0.075(6) -0.030(4) -0.009(4) 0.007(3) O1W 0.054(5) 0.076(6) 0.075(6) -0.028(5) -0.025(4) -0.003(4) O2W 0.036(4) 0.085(6) 0.054(5) -0.019(4) -0.009(4) -0.017(4) O3W 0.026(4) 0.061(5) 0.059(5) -0.030(4) 0.005(3) -0.007(3) O4W 0.061(5) 0.065(5) 0.048(5) -0.008(4) 0.002(4) -0.017(4) O5W 0.152(12) 0.100(8) 0.066(7) -0.024(6) 0.017(7) -0.031(8) O6W 0.099(13) 0.193(19) 0.063(10) -0.022(11) -0.025(9) -0.007(12) O7W 0.183(15) 0.124(11) 0.093(10) -0.042(8) -0.021(9) 0.004(10) O8W 0.27(2) 0.167(16) 0.147(15) -0.068(13) 0.052(15) -0.019(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O8 2.338(7) 2_766 ? Sm1 O6 2.339(7) . ? Sm1 O12 2.364(6) 1_465 ? Sm1 O2 2.382(7) 1_655 ? Sm1 O3 2.419(7) 1_565 ? Sm1 O10 2.481(7) 1_565 ? Sm1 O1W 2.508(8) . ? Sm1 O9 2.629(7) 1_565 ? Sm1 C30 2.932(11) 1_565 ? Sm2 O5 2.339(6) . ? Sm2 O11 2.349(7) 1_465 ? Sm2 O4 2.370(6) 1_465 ? Sm2 O7 2.393(7) 2_666 ? Sm2 O1 2.404(7) . ? Sm2 O3W 2.505(7) . ? Sm2 O4W 2.537(8) . ? Sm2 O2W 2.546(7) . ? Br1 Cu1 2.360(2) . ? Br1 Cu2 2.403(2) . ? Br2 Cu1 2.360(2) . ? Br2 Cu2 2.499(2) 2_665 ? Br2 Cu2 2.889(2) . ? Br3 Cu4 2.383(2) . ? Br3 Cu3 2.542(2) . ? Br3 Cu6 2.573(2) . ? Br4 Cu6 2.427(2) . ? Br4 Cu3 2.439(2) . ? Br5 Cu4 2.398(2) . ? Br5 Cu5 2.418(2) . ? Br6 Cu5 2.412(2) . ? Br6 Cu6 2.619(3) . ? C1 N1 1.350(14) . ? C1 C2 1.355(15) . ? C1 H1 0.9300 . ? C2 C3 1.392(14) . ? C2 H2 0.9300 . ? C3 C4 1.381(13) . ? C3 H3 0.9300 . ? C4 C5 1.381(13) . ? C4 C6 1.511(13) . ? C5 N1 1.348(12) . ? C5 H5 0.9300 . ? C6 O1 1.239(12) . ? C6 O2 1.266(11) . ? C7 N2 1.332(13) . ? C7 C8 1.356(14) . ? C7 H7 0.9300 . ? C8 C9 1.380(15) . ? C8 H8 0.9300 . ? C9 C10 1.372(13) . ? C9 H9 0.9300 . ? C10 C11 1.389(12) . ? C10 C12 1.500(13) . ? C11 N2 1.332(12) . ? C11 H11 0.9300 . ? C12 O4 1.248(11) . ? C12 O3 1.261(11) . ? C13 N3 1.342(11) . ? C13 C14 1.386(11) . ? C13 H13 0.9300 . ? C14 C15 1.385(13) . ? C14 C18 1.504(13) . ? C15 C16 1.377(14) . ? C15 H15 0.9300 . ? C16 C17 1.366(14) . ? C16 H16 0.9300 . ? C17 N3 1.345(13) . ? C17 H17 0.9300 . ? C18 O5 1.247(11) . ? C18 O6 1.256(11) . ? C19 N4 1.333(12) . ? C19 C20 1.390(13) . ? C19 H19 0.9300 . ? C20 C21 1.397(13) . ? C20 C24 1.473(14) . ? C21 C22 1.394(14) . ? C21 H21 0.9300 . ? C22 C23 1.355(15) . ? C22 H22 0.9300 . ? C23 N4 1.356(13) . ? C23 H23 0.9300 . ? C24 O8 1.262(12) . ? C24 O7 1.271(11) . ? C25 N5 1.320(14) . ? C25 C26 1.382(17) . ? C25 H25 0.9300 . ? C26 C27 1.371(17) . ? C26 H26 0.9300 . ? C27 C28 1.368(15) . ? C27 H27 0.9300 . ? C28 C29 1.405(15) . ? C28 C30 1.484(15) . ? C29 N5 1.333(14) . ? C29 H29 0.9300 . ? C30 O9 1.248(12) . ? C30 O10 1.284(12) . ? C30 Sm1 2.932(11) 1_545 ? C31 N6 1.346(12) . ? C31 C32 1.376(12) . ? C31 H31 0.9300 . ? C32 C33 1.409(12) . ? C32 C36 1.495(12) . ? C33 C34 1.386(14) . ? C33 H33 0.9300 . ? C34 C35 1.364(15) . ? C34 H34 0.9300 . ? C35 N6 1.345(13) . ? C35 H35 0.9300 . ? C36 O11 1.238(10) . ? C36 O12 1.249(10) . ? Cu1 N1 1.993(9) . ? Cu2 N2 1.988(8) . ? Cu2 Br2 2.499(2) 2_665 ? Cu2 Cu2 2.889(4) 2_665 ? Cu3 N3 1.973(7) . ? Cu4 N4 2.010(8) . ? Cu5 N5 2.031(9) . ? Cu6 N6 2.014(9) . ? O2 Sm1 2.382(6) 1_455 ? O3 Sm1 2.419(7) 1_545 ? O4 Sm2 2.370(6) 1_645 ? O7 Sm2 2.393(7) 2_666 ? O8 Sm1 2.338(7) 2_766 ? O9 Sm1 2.629(7) 1_545 ? O10 Sm1 2.481(7) 1_545 ? O11 Sm2 2.349(7) 1_645 ? O12 Sm1 2.364(6) 1_645 ? 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 O8 Sm1 O6 82.0(3) 2_766 . ? O8 Sm1 O12 145.4(3) 2_766 1_465 ? O6 Sm1 O12 97.9(3) . 1_465 ? O8 Sm1 O2 73.3(3) 2_766 1_655 ? O6 Sm1 O2 84.8(3) . 1_655 ? O12 Sm1 O2 141.3(3) 1_465 1_655 ? O8 Sm1 O3 118.7(3) 2_766 1_565 ? O6 Sm1 O3 154.7(3) . 1_565 ? O12 Sm1 O3 73.7(3) 1_465 1_565 ? O2 Sm1 O3 87.5(3) 1_655 1_565 ? O8 Sm1 O10 72.6(3) 2_766 1_565 ? O6 Sm1 O10 125.0(3) . 1_565 ? O12 Sm1 O10 79.6(2) 1_465 1_565 ? O2 Sm1 O10 129.7(2) 1_655 1_565 ? O3 Sm1 O10 77.8(3) 1_565 1_565 ? O8 Sm1 O1W 141.0(3) 2_766 . ? O6 Sm1 O1W 77.8(3) . . ? O12 Sm1 O1W 71.0(3) 1_465 . ? O2 Sm1 O1W 71.9(3) 1_655 . ? O3 Sm1 O1W 76.9(3) 1_565 . ? O10 Sm1 O1W 145.5(3) 1_565 . ? O8 Sm1 O9 77.1(3) 2_766 1_565 ? O6 Sm1 O9 76.5(3) . 1_565 ? O12 Sm1 O9 69.3(3) 1_465 1_565 ? O2 Sm1 O9 146.9(2) 1_655 1_565 ? O3 Sm1 O9 120.2(3) 1_565 1_565 ? O10 Sm1 O9 50.9(2) 1_565 1_565 ? O1W Sm1 O9 128.5(3) . 1_565 ? O8 Sm1 C30 74.3(3) 2_766 1_565 ? O6 Sm1 C30 100.9(3) . 1_565 ? O12 Sm1 C30 71.7(3) 1_465 1_565 ? O2 Sm1 C30 146.0(2) 1_655 1_565 ? O3 Sm1 C30 98.9(3) 1_565 1_565 ? O10 Sm1 C30 25.7(2) 1_565 1_565 ? O1W Sm1 C30 142.1(3) . 1_565 ? O9 Sm1 C30 25.2(2) 1_565 1_565 ? O5 Sm2 O11 96.5(2) . 1_465 ? O5 Sm2 O4 149.2(3) . 1_465 ? O11 Sm2 O4 86.1(2) 1_465 1_465 ? O5 Sm2 O7 89.6(2) . 2_666 ? O11 Sm2 O7 141.4(3) 1_465 2_666 ? O4 Sm2 O7 107.4(2) 1_465 2_666 ? O5 Sm2 O1 80.9(2) . . ? O11 Sm2 O1 143.1(3) 1_465 . ? O4 Sm2 O1 78.9(2) 1_465 . ? O7 Sm2 O1 75.4(3) 2_666 . ? O5 Sm2 O3W 141.5(3) . . ? O11 Sm2 O3W 79.0(2) 1_465 . ? O4 Sm2 O3W 69.2(2) 1_465 . ? O7 Sm2 O3W 73.0(3) 2_666 . ? O1 Sm2 O3W 124.8(2) . . ? O5 Sm2 O4W 72.6(3) . . ? O11 Sm2 O4W 73.4(3) 1_465 . ? O4 Sm2 O4W 78.8(3) 1_465 . ? O7 Sm2 O4W 143.7(3) 2_666 . ? O1 Sm2 O4W 70.8(3) . . ? O3W Sm2 O4W 138.7(3) . . ? O5 Sm2 O2W 71.1(3) . . ? O11 Sm2 O2W 74.4(3) 1_465 . ? O4 Sm2 O2W 138.2(3) 1_465 . ? O7 Sm2 O2W 71.8(3) 2_666 . ? O1 Sm2 O2W 136.4(3) . . ? O3W Sm2 O2W 70.9(2) . . ? O4W Sm2 O2W 127.4(3) . . ? Cu1 Br1 Cu2 70.48(7) . . ? Cu1 Br2 Cu2 87.21(8) . 2_665 ? Cu1 Br2 Cu2 62.21(6) . . ? Cu2 Br2 Cu2 64.38(7) 2_665 . ? Cu4 Br3 Cu3 65.42(6) . . ? Cu4 Br3 Cu6 70.13(7) . . ? Cu3 Br3 Cu6 61.71(5) . . ? Cu6 Br4 Cu3 65.26(6) . . ? Cu4 Br5 Cu5 71.66(6) . . ? Cu5 Br6 Cu6 70.31(6) . . ? N1 C1 C2 123.6(10) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 119.4(10) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 118.1(9) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C5 119.1(9) . . ? C3 C4 C6 122.1(8) . . ? C5 C4 C6 118.8(8) . . ? N1 C5 C4 123.0(9) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? O1 C6 O2 126.7(9) . . ? O1 C6 C4 117.1(8) . . ? O2 C6 C4 116.3(8) . . ? N2 C7 C8 125.6(10) . . ? N2 C7 H7 117.2 . . ? C8 C7 H7 117.2 . . ? C7 C8 C9 118.9(10) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 117.5(9) . . ? C10 C9 H9 121.2 . . ? C8 C9 H9 121.2 . . ? C9 C10 C11 119.1(9) . . ? C9 C10 C12 121.8(8) . . ? C11 C10 C12 119.1(8) . . ? N2 C11 C10 123.8(9) . . ? N2 C11 H11 118.1 . . ? C10 C11 H11 118.1 . . ? O4 C12 O3 122.1(9) . . ? O4 C12 C10 119.8(8) . . ? O3 C12 C10 118.1(8) . . ? N3 C13 C14 123.6(8) . . ? N3 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C15 C14 C13 117.9(8) . . ? C15 C14 C18 122.1(8) . . ? C13 C14 C18 120.0(8) . . ? C16 C15 C14 118.8(8) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C17 C16 C15 119.8(9) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? N3 C17 C16 122.7(9) . . ? N3 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? O5 C18 O6 125.5(9) . . ? O5 C18 C14 117.4(8) . . ? O6 C18 C14 117.0(8) . . ? N4 C19 C20 123.6(9) . . ? N4 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? C19 C20 C21 118.1(9) . . ? C19 C20 C24 120.1(8) . . ? C21 C20 C24 121.8(8) . . ? C22 C21 C20 118.4(9) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C23 C22 C21 119.1(9) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? N4 C23 C22 123.7(10) . . ? N4 C23 H23 118.2 . . ? C22 C23 H23 118.2 . . ? O8 C24 O7 122.7(10) . . ? O8 C24 C20 118.8(9) . . ? O7 C24 C20 118.5(8) . . ? N5 C25 C26 124.2(11) . . ? N5 C25 H25 117.9 . . ? C26 C25 H25 117.9 . . ? C27 C26 C25 117.6(11) . . ? C27 C26 H26 121.2 . . ? C25 C26 H26 121.2 . . ? C28 C27 C26 120.8(11) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 116.8(11) . . ? C27 C28 C30 124.1(10) . . ? C29 C28 C30 119.1(9) . . ? N5 C29 C28 123.6(10) . . ? N5 C29 H29 118.2 . . ? C28 C29 H29 118.2 . . ? O9 C30 O10 120.6(10) . . ? O9 C30 C28 121.8(9) . . ? O10 C30 C28 117.5(9) . . ? O9 C30 Sm1 63.7(6) . 1_545 ? O10 C30 Sm1 57.1(5) . 1_545 ? C28 C30 Sm1 171.5(7) . 1_545 ? N6 C31 C32 123.8(9) . . ? N6 C31 H31 118.1 . . ? C32 C31 H31 118.1 . . ? C31 C32 C33 118.2(9) . . ? C31 C32 C36 119.9(8) . . ? C33 C32 C36 121.9(8) . . ? C34 C33 C32 117.7(9) . . ? C34 C33 H33 121.2 . . ? C32 C33 H33 121.2 . . ? C35 C34 C33 120.1(9) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? N6 C35 C34 123.0(9) . . ? N6 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? O11 C36 O12 124.4(8) . . ? O11 C36 C32 117.5(8) . . ? O12 C36 C32 118.1(8) . . ? N1 Cu1 Br2 121.9(3) . . ? N1 Cu1 Br1 114.6(3) . . ? Br2 Cu1 Br1 122.87(8) . . ? N2 Cu2 Br1 129.2(3) . . ? N2 Cu2 Br2 108.5(2) . 2_665 ? Br1 Cu2 Br2 102.15(8) . 2_665 ? N2 Cu2 Br2 99.3(2) . . ? Br1 Cu2 Br2 102.74(7) . . ? Br2 Cu2 Br2 115.62(7) 2_665 . ? N2 Cu2 Cu2 115.8(3) . 2_665 ? Br1 Cu2 Cu2 113.75(8) . 2_665 ? Br2 Cu2 Cu2 64.36(7) 2_665 2_665 ? Br2 Cu2 Cu2 51.26(6) . 2_665 ? N3 Cu3 Br4 116.2(3) . . ? N3 Cu3 Br3 117.0(2) . . ? Br4 Cu3 Br3 108.97(8) . . ? N4 Cu4 Br3 116.5(2) . . ? N4 Cu4 Br5 114.0(2) . . ? Br3 Cu4 Br5 126.92(8) . . ? N5 Cu5 Br6 119.3(3) . . ? N5 Cu5 Br5 110.4(3) . . ? Br6 Cu5 Br5 119.41(8) . . ? N6 Cu6 Br4 114.8(3) . . ? N6 Cu6 Br3 106.8(3) . . ? Br4 Cu6 Br3 108.33(7) . . ? N6 Cu6 Br6 99.1(3) . . ? Br4 Cu6 Br6 107.50(8) . . ? Br3 Cu6 Br6 120.48(8) . . ? C5 N1 C1 116.7(9) . . ? C5 N1 Cu1 118.9(7) . . ? C1 N1 Cu1 123.4(7) . . ? C11 N2 C7 115.0(8) . . ? C11 N2 Cu2 123.7(7) . . ? C7 N2 Cu2 121.2(7) . . ? C13 N3 C17 117.1(8) . . ? C13 N3 Cu3 122.0(6) . . ? C17 N3 Cu3 120.5(7) . . ? C19 N4 C23 117.1(8) . . ? C19 N4 Cu4 118.4(6) . . ? C23 N4 Cu4 123.6(7) . . ? C25 N5 C29 117.1(10) . . ? C25 N5 Cu5 124.5(8) . . ? C29 N5 Cu5 118.0(7) . . ? C35 N6 C31 117.2(9) . . ? C35 N6 Cu6 122.9(7) . . ? C31 N6 Cu6 119.2(7) . . ? C6 O1 Sm2 144.9(6) . . ? C6 O2 Sm1 133.7(7) . 1_455 ? C12 O3 Sm1 115.3(6) . 1_545 ? C12 O4 Sm2 171.0(7) . 1_645 ? C18 O5 Sm2 151.6(7) . . ? C18 O6 Sm1 142.3(6) . . ? C24 O7 Sm2 127.4(6) . 2_666 ? C24 O8 Sm1 170.9(8) . 2_766 ? C30 O9 Sm1 91.1(6) . 1_545 ? C30 O10 Sm1 97.2(6) . 1_545 ? C36 O11 Sm2 139.7(6) . 1_645 ? C36 O12 Sm1 158.2(7) . 1_645 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.043 _refine_diff_density_min -1.399 _refine_diff_density_rms 0.186 data_2 _database_code_depnum_ccdc_archive 'CCDC 777374' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H32 Br6 Cu6 Eu2 N6 O16), 7(H2 O)' _chemical_formula_sum 'C72 H78 Br12 Cu12 Eu4 N12 O39' _chemical_formula_weight 4064.70 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' Cu Cu 0.3201 1.2651 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8257(14) _cell_length_b 14.790(2) _cell_length_c 20.182(3) _cell_angle_alpha 73.386(2) _cell_angle_beta 82.825(2) _cell_angle_gamma 77.750(2) _cell_volume 2739.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9821 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 8.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2426 _exptl_absorpt_correction_T_max 0.5335 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26246 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.20 _reflns_number_total 9821 _reflns_number_gt 6784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0408P)^2^+4.3525P] 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 9821 _refine_ls_number_parameters 682 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Br1 Br 0.17226(10) 0.87338(7) 0.49172(6) 0.0477(3) Uani 1 1 d . . . Br2 Br 0.51858(11) 0.68529(8) 0.43593(7) 0.0603(3) Uani 1 1 d . . . Br3 Br 0.28284(11) 0.82552(8) 0.27198(6) 0.0575(3) Uani 1 1 d . . . Br4 Br 0.46308(9) 1.00365(6) 0.33769(5) 0.0383(2) Uani 1 1 d . . . Br5 Br 0.99812(11) -0.07818(9) 0.86411(7) 0.0641(3) Uani 1 1 d . . . Br6 Br 1.12418(10) 0.11661(7) 0.94468(5) 0.0427(2) Uani 1 1 d . . . C1 C 0.5834(9) 0.6817(6) 0.6914(5) 0.031(2) Uani 1 1 d . . . C2 C 0.6164(7) 0.7542(5) 0.6257(4) 0.0236(18) Uani 1 1 d . . . C3 C 0.7473(8) 0.7789(6) 0.6116(5) 0.034(2) Uani 1 1 d . . . H3 H 0.8169 0.7495 0.6423 0.040 Uiso 1 1 calc R . . C4 C 0.7729(8) 0.8479(6) 0.5513(5) 0.039(2) Uani 1 1 d . . . H4 H 0.8592 0.8668 0.5412 0.047 Uiso 1 1 calc R . . C5 C 0.6704(9) 0.8872(7) 0.5075(5) 0.040(2) Uani 1 1 d . . . H5 H 0.6886 0.9334 0.4669 0.048 Uiso 1 1 calc R . . C6 C 0.5176(9) 0.7968(6) 0.5793(5) 0.032(2) Uani 1 1 d . . . H6 H 0.4300 0.7797 0.5893 0.038 Uiso 1 1 calc R . . C7 C 0.0984(9) 0.5227(6) 0.3125(5) 0.035(2) Uani 1 1 d . . . C8 C 0.0638(9) 0.5732(7) 0.3683(5) 0.039(2) Uani 1 1 d . . . C9 C 0.1606(9) 0.6239(7) 0.3796(5) 0.041(2) Uani 1 1 d . . . H9 H 0.2455 0.6222 0.3533 0.049 Uiso 1 1 calc R . . C10 C 0.0177(11) 0.6739(8) 0.4638(6) 0.058(3) Uani 1 1 d . . . H10 H 0.0010 0.7076 0.4974 0.069 Uiso 1 1 calc R . . C11 C -0.0843(11) 0.6258(9) 0.4559(6) 0.066(4) Uani 1 1 d . . . H11 H -0.1684 0.6289 0.4828 0.079 Uiso 1 1 calc R . . C12 C -0.0585(10) 0.5746(8) 0.4087(6) 0.058(3) Uani 1 1 d . . . H12 H -0.1240 0.5404 0.4036 0.070 Uiso 1 1 calc R . . C13 C -0.0519(8) 1.2901(6) 0.2289(5) 0.031(2) Uani 1 1 d . . . C14 C -0.0583(8) 1.1906(5) 0.2722(4) 0.0247(19) Uani 1 1 d . . . C15 C -0.1845(8) 1.1593(6) 0.2930(5) 0.036(2) Uani 1 1 d . . . H15 H -0.2689 1.2003 0.2812 0.044 Uiso 1 1 calc R . . C16 C -0.1809(9) 1.0676(7) 0.3308(5) 0.044(3) Uani 1 1 d . . . H16 H -0.2638 1.0446 0.3445 0.053 Uiso 1 1 calc R . . C17 C -0.0565(10) 1.0078(7) 0.3493(5) 0.048(3) Uani 1 1 d . . . H17 H -0.0579 0.9463 0.3779 0.058 Uiso 1 1 calc R . . C18 C 0.0625(8) 1.1266(5) 0.2910(4) 0.028(2) Uani 1 1 d . . . H18 H 0.1468 1.1480 0.2775 0.033 Uiso 1 1 calc R . . C19 C 0.8372(8) 0.6098(5) 0.1881(4) 0.0266(19) Uani 1 1 d . . . C20 C 0.8217(8) 0.6915(6) 0.2181(4) 0.0272(19) Uani 1 1 d . . . C21 C 0.6915(8) 0.7284(6) 0.2450(5) 0.037(2) Uani 1 1 d . . . H21 H 0.6159 0.7009 0.2430 0.044 Uiso 1 1 calc R . . C22 C 0.7787(10) 0.8428(7) 0.2756(5) 0.049(3) Uani 1 1 d . . . H22 H 0.7647 0.8943 0.2950 0.058 Uiso 1 1 calc R . . C23 C 0.9102(9) 0.8104(6) 0.2496(5) 0.044(3) Uani 1 1 d . . . H23 H 0.9836 0.8403 0.2512 0.053 Uiso 1 1 calc R . . C24 C 0.9334(8) 0.7343(6) 0.2212(4) 0.032(2) Uani 1 1 d . . . H24 H 1.0226 0.7114 0.2042 0.039 Uiso 1 1 calc R . . C25 C 0.6545(9) 0.3870(6) 0.8841(5) 0.031(2) Uani 1 1 d . . . C26 C 0.6364(8) 0.2845(6) 0.9103(5) 0.031(2) Uani 1 1 d . . . C27 C 0.5038(9) 0.2626(6) 0.9258(6) 0.049(3) Uani 1 1 d . . . H27 H 0.4246 0.3107 0.9198 0.059 Uiso 1 1 calc R . . C28 C 0.4933(10) 0.1668(7) 0.9503(6) 0.056(3) Uani 1 1 d . . . H28 H 0.4065 0.1487 0.9616 0.068 Uiso 1 1 calc R . . C29 C 0.6144(9) 0.0987(7) 0.9575(5) 0.043(2) Uani 1 1 d . . . H29 H 0.6060 0.0345 0.9744 0.052 Uiso 1 1 calc R . . C30 C 0.7504(8) 0.2119(6) 0.9189(5) 0.033(2) Uani 1 1 d . . . H30 H 0.8384 0.2281 0.9080 0.039 Uiso 1 1 calc R . . C31 C 1.5455(8) -0.3147(6) 0.8612(5) 0.031(2) Uani 1 1 d . . . C32 C 1.5270(8) -0.2100(6) 0.8599(5) 0.032(2) Uani 1 1 d . . . C33 C 1.3923(8) -0.1568(6) 0.8626(5) 0.038(2) Uani 1 1 d . . . H33 H 1.3170 -0.1868 0.8652 0.046 Uiso 1 1 calc R . . C34 C 1.4783(9) -0.0231(6) 0.8569(5) 0.045(3) Uani 1 1 d . . . H34 H 1.4624 0.0413 0.8565 0.053 Uiso 1 1 calc R . . C35 C 1.6105(9) -0.0683(7) 0.8526(5) 0.044(2) Uani 1 1 d . . . H35 H 1.6836 -0.0354 0.8478 0.053 Uiso 1 1 calc R . . C36 C 1.6373(8) -0.1650(6) 0.8552(5) 0.036(2) Uani 1 1 d . . . H36 H 1.7285 -0.1987 0.8539 0.043 Uiso 1 1 calc R . . Cu1 Cu 0.40210(14) 0.89984(10) 0.44654(7) 0.0577(4) Uani 1 1 d . . . Cu2 Cu 0.27428(14) 0.75730(10) 0.42757(8) 0.0619(4) Uani 1 1 d . . . Cu3 Cu 0.24132(13) 0.93985(9) 0.34139(9) 0.0660(4) Uani 1 1 d . . . Cu4 Cu 0.48543(13) 0.83311(11) 0.32588(8) 0.0654(4) Uani 1 1 d . . . Cu5 Cu 0.90859(14) 0.01357(9) 0.94655(8) 0.0611(4) Uani 1 1 d . . . Cu6 Cu 1.17289(13) -0.00381(9) 0.88516(8) 0.0602(4) Uani 1 1 d . . . Eu1 Eu 0.83576(4) 0.54676(3) 0.81086(2) 0.02666(12) Uani 1 1 d . . . Eu2 Eu 0.36909(4) 0.55188(3) 0.79651(2) 0.02526(12) Uani 1 1 d . . . N1 N 0.5411(7) 0.8628(5) 0.5193(4) 0.0382(19) Uani 1 1 d . . . N2 N 0.1358(8) 0.6738(6) 0.4258(4) 0.046(2) Uani 1 1 d . . . N3 N 0.0662(7) 1.0348(5) 0.3278(4) 0.0326(17) Uani 1 1 d . . . N4 N 0.6699(7) 0.8020(5) 0.2738(4) 0.041(2) Uani 1 1 d . . . N5 N 0.7424(7) 0.1185(5) 0.9420(4) 0.0343(18) Uani 1 1 d . . . N6 N 1.3674(8) -0.0638(5) 0.8617(4) 0.046(2) Uani 1 1 d . . . O1 O 0.6748(6) 0.6423(5) 0.7325(4) 0.0503(18) Uani 1 1 d . . . O2 O 0.4598(6) 0.6664(4) 0.7013(3) 0.0428(17) Uani 1 1 d . . . O3 O 0.0314(6) 0.4618(5) 0.3090(4) 0.0496(18) Uani 1 1 d . . . O4 O 0.1973(6) 0.5477(4) 0.2664(3) 0.0423(16) Uani 1 1 d . . . O5 O -0.1604(6) 1.3400(4) 0.2017(3) 0.0398(16) Uani 1 1 d . . . O6 O 0.0613(6) 1.3178(4) 0.2224(4) 0.0446(17) Uani 1 1 d . . . O7 O 0.7309(5) 0.5849(4) 0.1788(3) 0.0365(15) Uani 1 1 d . . . O8 O 0.9578(6) 0.5684(4) 0.1733(4) 0.0439(17) Uani 1 1 d . . . O9 O 0.5587(6) 0.4508(4) 0.8541(4) 0.0445(17) Uani 1 1 d . . . O10 O 0.7713(6) 0.4055(4) 0.8902(4) 0.0456(17) Uani 1 1 d . . . O11 O 1.4432(6) -0.3412(4) 0.8470(4) 0.0463(18) Uani 1 1 d . . . O12 O 1.6641(6) -0.3650(4) 0.8740(3) 0.0382(15) Uani 1 1 d . . . O1W O 0.9334(7) 0.5411(5) 0.9199(4) 0.063(2) Uani 1 1 d . . . O2W O 0.5215(6) 0.4604(4) 0.7201(3) 0.0421(16) Uani 1 1 d . . . O3W O 0.2398(6) 0.5691(5) 0.6914(4) 0.0541(19) Uani 1 1 d . . . O4W O 0.2731(7) 0.5225(5) 0.9206(3) 0.0563(19) Uani 1 1 d . . . O5W O 0.4271(11) 0.5326(6) 0.5848(5) 0.101(3) Uani 1 1 d . . . O6W O 0.5000 0.5000 0.0000 0.123(6) Uani 1 2 d S . . O7W O 0.8972(13) 0.3255(7) 0.0263(5) 0.125(4) Uani 1 1 d . . . O8W O 0.1766(17) 0.3437(9) 0.9955(7) 0.180(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0420(5) 0.0518(6) 0.0531(7) -0.0203(5) -0.0014(5) -0.0095(5) Br2 0.0495(6) 0.0489(6) 0.0735(9) -0.0085(6) -0.0062(6) 0.0007(5) Br3 0.0513(6) 0.0541(7) 0.0744(9) -0.0184(6) -0.0175(6) -0.0164(5) Br4 0.0372(5) 0.0370(5) 0.0427(6) -0.0122(5) 0.0012(4) -0.0114(4) Br5 0.0499(6) 0.0889(9) 0.0705(9) -0.0508(7) -0.0016(6) -0.0110(6) Br6 0.0417(5) 0.0352(5) 0.0486(7) -0.0102(5) -0.0029(5) -0.0028(4) C1 0.030(5) 0.024(4) 0.032(6) 0.000(4) -0.001(4) 0.001(4) C2 0.023(4) 0.016(4) 0.031(5) -0.003(4) -0.006(4) -0.004(3) C3 0.027(4) 0.037(5) 0.041(6) -0.016(5) -0.001(4) -0.010(4) C4 0.022(4) 0.042(5) 0.057(7) -0.015(5) 0.007(5) -0.017(4) C5 0.036(5) 0.046(6) 0.037(6) -0.005(5) 0.008(5) -0.017(4) C6 0.036(5) 0.031(5) 0.028(5) -0.004(4) -0.004(4) -0.010(4) C7 0.034(5) 0.034(5) 0.036(6) -0.006(5) -0.006(4) -0.005(4) C8 0.030(5) 0.045(6) 0.046(6) -0.015(5) 0.002(4) -0.012(4) C9 0.024(4) 0.053(6) 0.055(7) -0.030(6) -0.001(4) -0.007(4) C10 0.064(7) 0.065(7) 0.062(8) -0.048(6) 0.021(6) -0.023(6) C11 0.040(6) 0.094(9) 0.079(9) -0.049(8) 0.026(6) -0.026(6) C12 0.039(6) 0.080(8) 0.068(8) -0.027(7) 0.007(6) -0.033(6) C13 0.030(5) 0.020(4) 0.040(6) -0.008(4) -0.005(4) 0.002(4) C14 0.023(4) 0.021(4) 0.032(5) -0.012(4) -0.005(4) 0.002(3) C15 0.022(4) 0.036(5) 0.048(6) -0.012(5) 0.005(4) -0.002(4) C16 0.027(5) 0.046(6) 0.056(7) 0.000(5) 0.006(5) -0.024(4) C17 0.051(6) 0.045(6) 0.045(7) 0.001(5) -0.016(5) -0.010(5) C18 0.018(4) 0.027(4) 0.042(6) -0.011(4) -0.005(4) -0.007(3) C19 0.024(4) 0.017(4) 0.037(6) -0.003(4) -0.004(4) -0.004(3) C20 0.019(4) 0.031(5) 0.028(5) -0.001(4) -0.002(4) -0.006(3) C21 0.025(4) 0.027(5) 0.057(7) -0.010(5) -0.002(4) -0.002(4) C22 0.052(6) 0.039(6) 0.066(8) -0.027(6) -0.004(6) -0.015(5) C23 0.031(5) 0.043(6) 0.071(8) -0.027(6) -0.009(5) -0.014(4) C24 0.022(4) 0.037(5) 0.033(6) -0.003(4) 0.006(4) -0.008(4) C25 0.034(5) 0.026(5) 0.033(6) -0.004(4) -0.005(4) -0.008(4) C26 0.021(4) 0.025(4) 0.043(6) -0.005(4) -0.002(4) -0.005(3) C27 0.028(5) 0.031(5) 0.080(8) -0.006(5) -0.010(5) 0.004(4) C28 0.037(6) 0.038(6) 0.087(9) 0.003(6) -0.009(6) -0.014(5) C29 0.043(6) 0.037(5) 0.049(7) 0.002(5) -0.011(5) -0.021(4) C30 0.025(4) 0.030(5) 0.044(6) -0.010(4) -0.003(4) -0.007(4) C31 0.018(4) 0.031(5) 0.045(6) -0.018(4) 0.003(4) 0.001(4) C32 0.023(4) 0.034(5) 0.044(6) -0.015(4) -0.006(4) -0.004(4) C33 0.026(4) 0.032(5) 0.064(7) -0.026(5) -0.002(4) -0.006(4) C34 0.045(6) 0.025(5) 0.067(8) -0.013(5) -0.006(5) -0.012(4) C35 0.034(5) 0.041(6) 0.061(7) -0.013(5) -0.010(5) -0.011(4) C36 0.020(4) 0.040(5) 0.049(6) -0.017(5) -0.001(4) -0.001(4) Cu1 0.0624(8) 0.0672(9) 0.0422(8) -0.0030(7) -0.0148(7) -0.0185(7) Cu2 0.0532(8) 0.0559(8) 0.0870(12) -0.0303(8) -0.0031(8) -0.0184(7) Cu3 0.0412(7) 0.0425(8) 0.1010(13) -0.0057(8) -0.0190(8) 0.0106(6) Cu4 0.0352(7) 0.0788(10) 0.0939(12) -0.0525(9) 0.0066(7) -0.0019(6) Cu5 0.0559(8) 0.0368(7) 0.0787(11) -0.0150(7) 0.0048(7) 0.0110(6) Cu6 0.0450(7) 0.0508(8) 0.0834(11) -0.0279(8) -0.0122(7) 0.0122(6) Eu1 0.0163(2) 0.0204(2) 0.0417(3) -0.0057(2) -0.00270(19) -0.00312(16) Eu2 0.0156(2) 0.0216(2) 0.0377(3) -0.0054(2) -0.00486(18) -0.00328(16) N1 0.036(4) 0.039(4) 0.038(5) -0.005(4) -0.001(4) -0.011(3) N2 0.040(5) 0.051(5) 0.051(6) -0.023(5) 0.008(4) -0.013(4) N3 0.028(4) 0.023(4) 0.044(5) -0.002(3) -0.007(3) -0.004(3) N4 0.030(4) 0.034(4) 0.064(6) -0.022(4) -0.001(4) -0.007(3) N5 0.034(4) 0.024(4) 0.042(5) -0.008(4) 0.004(4) -0.005(3) N6 0.041(5) 0.040(5) 0.060(6) -0.023(4) -0.012(4) 0.006(4) O1 0.037(4) 0.052(4) 0.050(5) 0.004(4) -0.016(3) 0.000(3) O2 0.030(3) 0.040(4) 0.047(4) 0.013(3) -0.003(3) -0.016(3) O3 0.034(3) 0.058(4) 0.063(5) -0.023(4) 0.006(3) -0.018(3) O4 0.028(3) 0.053(4) 0.055(5) -0.021(4) 0.000(3) -0.019(3) O5 0.024(3) 0.033(3) 0.052(4) -0.002(3) -0.008(3) 0.004(3) O6 0.024(3) 0.030(3) 0.079(5) -0.006(3) -0.006(3) -0.013(3) O7 0.028(3) 0.029(3) 0.057(5) -0.015(3) -0.004(3) -0.009(3) O8 0.025(3) 0.042(4) 0.067(5) -0.027(4) -0.006(3) 0.006(3) O9 0.041(4) 0.024(3) 0.066(5) -0.009(3) -0.029(3) 0.011(3) O10 0.037(4) 0.033(4) 0.062(5) 0.004(3) -0.012(3) -0.015(3) O11 0.027(3) 0.040(4) 0.084(6) -0.035(4) 0.002(3) -0.012(3) O12 0.026(3) 0.040(4) 0.049(4) -0.019(3) -0.007(3) 0.006(3) O1W 0.054(4) 0.069(5) 0.071(6) -0.026(4) -0.033(4) 0.003(4) O2W 0.031(3) 0.051(4) 0.046(4) -0.021(3) 0.003(3) -0.004(3) O3W 0.037(4) 0.080(5) 0.048(5) -0.014(4) -0.011(3) -0.016(3) O4W 0.068(5) 0.063(5) 0.036(4) -0.012(4) 0.000(4) -0.011(4) O5W 0.137(8) 0.087(7) 0.079(7) -0.030(6) 0.029(6) -0.031(6) O6W 0.099(10) 0.199(16) 0.057(9) -0.020(10) -0.030(8) -0.007(11) O7W 0.176(11) 0.106(8) 0.089(8) -0.037(7) -0.014(7) 0.000(7) O8W 0.263(17) 0.144(11) 0.114(11) -0.050(9) 0.041(11) -0.011(11) _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 Br1 Cu1 2.3961(17) . ? Br1 Cu2 2.4175(17) . ? Br2 Cu2 2.4162(17) . ? Br2 Cu4 2.631(2) . ? Br3 Cu4 2.4214(17) . ? Br3 Cu3 2.4305(19) . ? Br4 Cu1 2.3823(16) . ? Br4 Cu3 2.5368(16) . ? Br4 Cu4 2.5618(17) . ? Br5 Cu6 2.3644(17) . ? Br5 Cu5 2.4088(17) . ? Br6 Cu6 2.3584(16) . ? Br6 Cu5 2.5098(18) 2_757 ? Br6 Cu5 2.8511(17) . ? C1 O1 1.233(10) . ? C1 O2 1.263(9) . ? C1 C2 1.497(11) . ? C2 C6 1.359(11) . ? C2 C3 1.384(10) . ? C3 C4 1.381(12) . ? C3 H3 0.9300 . ? C4 C5 1.347(12) . ? C4 H4 0.9300 . ? C5 N1 1.367(11) . ? C5 H5 0.9300 . ? C6 N1 1.350(11) . ? C6 H6 0.9300 . ? C7 O3 1.244(10) . ? C7 O4 1.296(10) . ? C7 C8 1.490(12) . ? C7 Eu1 2.907(9) 2_666 ? C8 C12 1.365(12) . ? C8 C9 1.405(12) . ? C9 N2 1.318(11) . ? C9 H9 0.9300 . ? C10 N2 1.308(11) . ? C10 C11 1.393(14) . ? C10 H10 0.9300 . ? C11 C12 1.347(14) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 O6 1.243(9) . ? C13 O5 1.251(9) . ? C13 C14 1.492(11) . ? C14 C18 1.371(10) . ? C14 C15 1.389(11) . ? C15 C16 1.347(12) . ? C15 H15 0.9300 . ? C16 C17 1.372(12) . ? C16 H16 0.9300 . ? C17 N3 1.333(11) . ? C17 H17 0.9300 . ? C18 N3 1.344(10) . ? C18 H18 0.9300 . ? C19 O7 1.230(9) . ? C19 O8 1.256(9) . ? C19 C20 1.472(11) . ? C20 C21 1.389(11) . ? C20 C24 1.394(11) . ? C21 N4 1.342(11) . ? C21 H21 0.9300 . ? C22 N4 1.344(11) . ? C22 C23 1.374(12) . ? C22 H22 0.9300 . ? C23 C24 1.370(12) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O9 1.258(9) . ? C25 O10 1.262(9) . ? C25 C26 1.498(11) . ? C26 C30 1.367(11) . ? C26 C27 1.386(11) . ? C27 C28 1.382(12) . ? C27 H27 0.9300 . ? C28 C29 1.379(12) . ? C28 H28 0.9300 . ? C29 N5 1.331(10) . ? C29 H29 0.9300 . ? C30 N5 1.342(10) . ? C30 H30 0.9300 . ? C31 O11 1.244(9) . ? C31 O12 1.256(9) . ? C31 C32 1.513(11) . ? C32 C36 1.368(11) . ? C32 C33 1.392(11) . ? C33 N6 1.340(10) . ? C33 H33 0.9300 . ? C34 C35 1.334(12) . ? C34 N6 1.333(11) . ? C34 H34 0.9300 . ? C35 C36 1.385(12) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? Cu1 N1 2.011(7) . ? Cu2 N2 2.032(8) . ? Cu3 N3 1.970(6) . ? Cu4 N4 2.011(7) . ? Cu5 N5 1.991(7) . ? Cu5 Br6 2.5098(17) 2_757 ? Cu5 Cu5 2.865(3) 2_757 ? Cu6 N6 1.989(7) . ? Eu1 O1 2.324(6) . ? Eu1 O6 2.326(5) 2_676 ? Eu1 O8 2.346(5) 2_766 ? Eu1 O12 2.377(5) 1_465 ? Eu1 O10 2.393(6) . ? Eu1 O4 2.459(6) 2_666 ? Eu1 O1W 2.482(7) . ? Eu1 O3 2.624(7) 2_666 ? Eu1 C7 2.907(9) 2_666 ? Eu2 O5 2.321(5) 2_576 ? Eu2 O9 2.329(5) . ? Eu2 O7 2.335(5) 2_666 ? Eu2 O11 2.380(6) 1_465 ? Eu2 O2 2.389(6) . ? Eu2 O2W 2.492(6) . ? Eu2 O4W 2.513(7) . ? Eu2 O3W 2.532(6) . ? O3 Eu1 2.624(7) 2_666 ? O4 Eu1 2.459(6) 2_666 ? O5 Eu2 2.321(5) 2_576 ? O6 Eu1 2.326(5) 2_676 ? O7 Eu2 2.335(5) 2_666 ? O8 Eu1 2.346(5) 2_766 ? O11 Eu2 2.380(6) 1_645 ? O12 Eu1 2.378(5) 1_645 ? 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 Cu1 Br1 Cu2 71.31(5) . . ? Cu2 Br2 Cu4 69.86(5) . . ? Cu4 Br3 Cu3 65.19(5) . . ? Cu1 Br4 Cu3 65.36(5) . . ? Cu1 Br4 Cu4 70.22(6) . . ? Cu3 Br4 Cu4 61.68(4) . . ? Cu6 Br5 Cu5 69.69(6) . . ? Cu6 Br6 Cu5 87.22(6) . 2_757 ? Cu6 Br6 Cu5 62.30(5) . . ? Cu5 Br6 Cu5 64.25(6) 2_757 . ? O1 C1 O2 124.3(8) . . ? O1 C1 C2 119.4(7) . . ? O2 C1 C2 116.3(7) . . ? C6 C2 C3 119.3(8) . . ? C6 C2 C1 120.1(7) . . ? C3 C2 C1 120.6(7) . . ? C4 C3 C2 119.0(8) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C5 C4 C3 118.7(8) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 N1 123.6(9) . . ? C4 C5 H5 118.2 . . ? N1 C5 H5 118.2 . . ? N1 C6 C2 122.8(8) . . ? N1 C6 H6 118.6 . . ? C2 C6 H6 118.6 . . ? O3 C7 O4 121.5(8) . . ? O3 C7 C8 121.3(8) . . ? O4 C7 C8 117.1(8) . . ? O3 C7 Eu1 64.5(5) . 2_666 ? O4 C7 Eu1 57.2(4) . 2_666 ? C8 C7 Eu1 171.2(6) . 2_666 ? C12 C8 C9 117.7(9) . . ? C12 C8 C7 123.7(8) . . ? C9 C8 C7 118.6(8) . . ? N2 C9 C8 122.5(8) . . ? N2 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? N2 C10 C11 122.8(9) . . ? N2 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C12 C11 C10 118.7(9) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C8 119.9(9) . . ? C11 C12 H12 120.1 . . ? C8 C12 H12 120.1 . . ? O6 C13 O5 124.5(8) . . ? O6 C13 C14 117.6(7) . . ? O5 C13 C14 117.8(7) . . ? C18 C14 C15 118.3(7) . . ? C18 C14 C13 119.9(7) . . ? C15 C14 C13 121.7(7) . . ? C16 C15 C14 117.9(8) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? C15 C16 C17 120.9(8) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? N3 C17 C16 122.4(9) . . ? N3 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? N3 C18 C14 123.8(7) . . ? N3 C18 H18 118.1 . . ? C14 C18 H18 118.1 . . ? O7 C19 O8 122.9(7) . . ? O7 C19 C20 118.3(7) . . ? O8 C19 C20 118.9(7) . . ? C21 C20 C24 117.6(8) . . ? C21 C20 C19 119.7(7) . . ? C24 C20 C19 122.7(7) . . ? N4 C21 C20 122.9(8) . . ? N4 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? N4 C22 C23 121.7(8) . . ? N4 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C24 C23 C22 120.1(8) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C20 119.2(8) . . ? C23 C24 H24 120.4 . . ? C20 C24 H24 120.4 . . ? O9 C25 O10 121.8(8) . . ? O9 C25 C26 120.6(7) . . ? O10 C25 C26 117.5(7) . . ? C30 C26 C27 119.5(8) . . ? C30 C26 C25 120.3(7) . . ? C27 C26 C25 120.2(7) . . ? C28 C27 C26 117.7(8) . . ? C28 C27 H27 121.2 . . ? C26 C27 H27 121.2 . . ? C29 C28 C27 118.6(9) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? N5 C29 C28 124.5(8) . . ? N5 C29 H29 117.8 . . ? C28 C29 H29 117.8 . . ? N5 C30 C26 123.7(7) . . ? N5 C30 H30 118.1 . . ? C26 C30 H30 118.1 . . ? O11 C31 O12 126.7(8) . . ? O11 C31 C32 116.7(7) . . ? O12 C31 C32 116.5(7) . . ? C36 C32 C33 118.5(8) . . ? C36 C32 C31 122.7(7) . . ? C33 C32 C31 118.8(7) . . ? N6 C33 C32 122.4(8) . . ? N6 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C35 C34 N6 124.6(8) . . ? C35 C34 H34 117.7 . . ? N6 C34 H34 117.7 . . ? C34 C35 C36 118.9(8) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C32 C36 C35 118.8(8) . . ? C32 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? N1 Cu1 Br4 116.6(2) . . ? N1 Cu1 Br1 113.9(2) . . ? Br4 Cu1 Br1 126.66(7) . . ? N2 Cu2 Br2 118.8(2) . . ? N2 Cu2 Br1 110.5(2) . . ? Br2 Cu2 Br1 119.31(7) . . ? N3 Cu3 Br3 116.0(2) . . ? N3 Cu3 Br4 116.9(2) . . ? Br3 Cu3 Br4 109.21(6) . . ? N4 Cu4 Br3 115.2(2) . . ? N4 Cu4 Br4 107.2(2) . . ? Br3 Cu4 Br4 108.68(6) . . ? N4 Cu4 Br2 98.5(2) . . ? Br3 Cu4 Br2 107.27(7) . . ? Br4 Cu4 Br2 120.09(7) . . ? N5 Cu5 Br5 128.8(2) . . ? N5 Cu5 Br6 107.7(2) . 2_757 ? Br5 Cu5 Br6 101.62(6) . 2_757 ? N5 Cu5 Br6 100.1(2) . . ? Br5 Cu5 Br6 103.66(6) . . ? Br6 Cu5 Br6 115.76(6) 2_757 . ? N5 Cu5 Cu5 116.2(2) . 2_757 ? Br5 Cu5 Cu5 114.29(7) . 2_757 ? Br6 Cu5 Cu5 63.67(6) 2_757 2_757 ? Br6 Cu5 Cu5 52.09(5) . 2_757 ? N6 Cu6 Br6 121.9(2) . . ? N6 Cu6 Br5 114.8(2) . . ? Br6 Cu6 Br5 122.69(6) . . ? O1 Eu1 O6 82.8(2) . 2_676 ? O1 Eu1 O8 145.8(2) . 2_766 ? O6 Eu1 O8 97.3(2) 2_676 2_766 ? O1 Eu1 O12 73.6(2) . 1_465 ? O6 Eu1 O12 85.9(2) 2_676 1_465 ? O8 Eu1 O12 140.6(2) 2_766 1_465 ? O1 Eu1 O10 117.6(2) . . ? O6 Eu1 O10 155.0(2) 2_676 . ? O8 Eu1 O10 74.2(2) 2_766 . ? O12 Eu1 O10 86.4(2) 1_465 . ? O1 Eu1 O4 72.2(2) . 2_666 ? O6 Eu1 O4 125.4(2) 2_676 2_666 ? O8 Eu1 O4 80.4(2) 2_766 2_666 ? O12 Eu1 O4 128.80(19) 1_465 2_666 ? O10 Eu1 O4 77.1(2) . 2_666 ? O1 Eu1 O1W 141.3(2) . . ? O6 Eu1 O1W 78.1(2) 2_676 . ? O8 Eu1 O1W 70.7(2) 2_766 . ? O12 Eu1 O1W 71.7(2) 1_465 . ? O10 Eu1 O1W 76.9(2) . . ? O4 Eu1 O1W 145.3(2) 2_666 . ? O1 Eu1 O3 77.5(2) . 2_666 ? O6 Eu1 O3 76.3(2) 2_676 2_666 ? O8 Eu1 O3 69.4(2) 2_766 2_666 ? O12 Eu1 O3 147.7(2) 1_465 2_666 ? O10 Eu1 O3 120.2(2) . 2_666 ? O4 Eu1 O3 51.58(19) 2_666 2_666 ? O1W Eu1 O3 128.6(2) . 2_666 ? O1 Eu1 C7 74.3(2) . 2_666 ? O6 Eu1 C7 100.9(2) 2_676 2_666 ? O8 Eu1 C7 72.1(2) 2_766 2_666 ? O12 Eu1 C7 146.1(2) 1_465 2_666 ? O10 Eu1 C7 98.7(2) . 2_666 ? O4 Eu1 C7 26.3(2) 2_666 2_666 ? O1W Eu1 C7 142.2(2) . 2_666 ? O3 Eu1 C7 25.3(2) 2_666 2_666 ? O5 Eu2 O9 149.5(2) 2_576 . ? O5 Eu2 O7 96.2(2) 2_576 2_666 ? O9 Eu2 O7 86.1(2) . 2_666 ? O5 Eu2 O11 81.1(2) 2_576 1_465 ? O9 Eu2 O11 79.5(2) . 1_465 ? O7 Eu2 O11 144.0(2) 2_666 1_465 ? O5 Eu2 O2 89.9(2) 2_576 . ? O9 Eu2 O2 107.3(2) . . ? O7 Eu2 O2 141.2(2) 2_666 . ? O11 Eu2 O2 74.8(2) 1_465 . ? O5 Eu2 O2W 141.3(2) 2_576 . ? O9 Eu2 O2W 69.0(2) . . ? O7 Eu2 O2W 78.9(2) 2_666 . ? O11 Eu2 O2W 124.60(19) 1_465 . ? O2 Eu2 O2W 72.9(2) . . ? O5 Eu2 O4W 73.1(2) 2_576 . ? O9 Eu2 O4W 78.5(2) . . ? O7 Eu2 O4W 73.5(2) 2_666 . ? O11 Eu2 O4W 71.4(2) 1_465 . ? O2 Eu2 O4W 144.0(2) . . ? O2W Eu2 O4W 138.4(2) . . ? O5 Eu2 O3W 70.5(2) 2_576 . ? O9 Eu2 O3W 138.3(2) . . ? O7 Eu2 O3W 74.2(2) 2_666 . ? O11 Eu2 O3W 135.7(2) 1_465 . ? O2 Eu2 O3W 72.0(2) . . ? O2W Eu2 O3W 71.3(2) . . ? O4W Eu2 O3W 127.4(2) . . ? C6 N1 C5 116.6(8) . . ? C6 N1 Cu1 118.7(6) . . ? C5 N1 Cu1 123.7(6) . . ? C10 N2 C9 118.4(8) . . ? C10 N2 Cu2 123.3(7) . . ? C9 N2 Cu2 118.0(6) . . ? C17 N3 C18 116.6(7) . . ? C17 N3 Cu3 120.6(6) . . ? C18 N3 Cu3 122.5(5) . . ? C21 N4 C22 118.5(8) . . ? C21 N4 Cu4 118.8(6) . . ? C22 N4 Cu4 122.0(6) . . ? C29 N5 C30 116.0(7) . . ? C29 N5 Cu5 120.7(6) . . ? C30 N5 Cu5 123.1(5) . . ? C34 N6 C33 116.9(8) . . ? C34 N6 Cu6 124.2(6) . . ? C33 N6 Cu6 117.9(6) . . ? C1 O1 Eu1 171.3(6) . . ? C1 O2 Eu2 126.4(5) . . ? C7 O3 Eu1 90.2(5) . 2_666 ? C7 O4 Eu1 96.5(5) . 2_666 ? C13 O5 Eu2 151.7(6) . 2_576 ? C13 O6 Eu1 143.7(5) . 2_676 ? C19 O7 Eu2 140.5(5) . 2_666 ? C19 O8 Eu1 157.5(6) . 2_766 ? C25 O9 Eu2 172.2(5) . . ? C25 O10 Eu1 117.1(5) . . ? C31 O11 Eu2 145.4(5) . 1_645 ? C31 O12 Eu1 133.7(6) . 1_645 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.386 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.165 data_3 _database_code_depnum_ccdc_archive 'CCDC 777375' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H32 Br6 Cu6 N6 O16 Tb2), 7(H2 O)' _chemical_formula_sum 'C72 H78 Br12 Cu12 N12 O39 Tb4' _chemical_formula_weight 4092.54 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' Cu Cu 0.3201 1.2651 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8116(7) _cell_length_b 14.7661(10) _cell_length_c 20.1753(14) _cell_angle_alpha 73.2130(10) _cell_angle_beta 82.5410(10) _cell_angle_gamma 77.7480(10) _cell_volume 2727.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9788 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 9.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2133 _exptl_absorpt_correction_T_max 0.5616 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26434 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.20 _reflns_number_total 9788 _reflns_number_gt 7786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0295P)^2^+4.1379P] 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 9788 _refine_ls_number_parameters 682 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Br1 Br 0.66995(7) 0.37214(5) 0.49209(4) 0.04877(19) Uani 1 1 d . . . Br2 Br 0.96196(7) 0.50323(4) 0.33781(3) 0.03889(16) Uani 1 1 d . . . Br3 Br 1.01693(9) 0.18489(6) 0.43591(5) 0.0676(2) Uani 1 1 d . . . Br4 Br 0.78267(8) 0.32493(6) 0.27178(5) 0.0589(2) Uani 1 1 d . . . Br5 Br 0.50124(9) 0.57825(7) 0.13585(5) 0.0688(3) Uani 1 1 d . . . Br6 Br 0.37655(7) 0.38384(5) 0.05534(4) 0.04332(17) Uani 1 1 d . . . C1 C 0.4473(6) 0.7921(4) 0.2284(3) 0.0287(13) Uani 1 1 d . . . C2 C 0.4404(6) 0.6910(4) 0.2716(3) 0.0249(13) Uani 1 1 d . . . C3 C 0.5626(6) 0.6267(4) 0.2907(3) 0.0291(13) Uani 1 1 d . . . H3 H 0.6473 0.6479 0.2772 0.035 Uiso 1 1 calc R . . C4 C 0.4387(7) 0.5074(5) 0.3474(4) 0.0432(17) Uani 1 1 d . . . H4 H 0.4373 0.4441 0.3730 0.052 Uiso 1 1 calc R . . C5 C 0.3153(6) 0.5673(4) 0.3316(4) 0.0425(17) Uani 1 1 d . . . H5 H 0.2314 0.5456 0.3474 0.051 Uiso 1 1 calc R . . C6 C 0.3150(6) 0.6598(4) 0.2924(3) 0.0358(15) Uani 1 1 d . . . H6 H 0.2312 0.7011 0.2798 0.043 Uiso 1 1 calc R . . C7 C -0.0453(6) 0.8159(4) 0.1400(3) 0.0291(13) Uani 1 1 d . . . C8 C -0.0265(6) 0.7118(4) 0.1404(3) 0.0278(13) Uani 1 1 d . . . C9 C 0.1066(6) 0.6587(4) 0.1374(3) 0.0374(15) Uani 1 1 d . . . H9 H 0.1822 0.6887 0.1350 0.045 Uiso 1 1 calc R . . C10 C 0.0213(7) 0.5230(4) 0.1448(4) 0.0454(18) Uani 1 1 d . . . H10 H 0.0375 0.4579 0.1470 0.054 Uiso 1 1 calc R . . C11 C -0.1148(7) 0.5703(5) 0.1488(4) 0.0428(17) Uani 1 1 d . . . H11 H -0.1887 0.5380 0.1537 0.051 Uiso 1 1 calc R . . C12 C -0.1393(6) 0.6673(4) 0.1454(3) 0.0341(15) Uani 1 1 d . . . H12 H -0.2302 0.7020 0.1465 0.041 Uiso 1 1 calc R . . C13 C 0.8484(6) 0.1115(4) 0.1176(3) 0.0281(13) Uani 1 1 d . . . C14 C 0.8663(6) 0.2147(4) 0.0896(3) 0.0277(13) Uani 1 1 d . . . C15 C 0.9976(7) 0.2381(5) 0.0756(4) 0.0483(19) Uani 1 1 d . . . H15 H 1.0778 0.1910 0.0829 0.058 Uiso 1 1 calc R . . C16 C 1.0052(7) 0.3342(5) 0.0501(4) 0.054(2) Uani 1 1 d . . . H16 H 1.0919 0.3527 0.0379 0.065 Uiso 1 1 calc R . . C17 C 0.8865(7) 0.4019(4) 0.0428(4) 0.0401(16) Uani 1 1 d . . . H17 H 0.8946 0.4663 0.0262 0.048 Uiso 1 1 calc R . . C18 C 0.7515(6) 0.2874(4) 0.0807(3) 0.0306(14) Uani 1 1 d . . . H18 H 0.6635 0.2705 0.0911 0.037 Uiso 1 1 calc R . . C19 C 0.5984(6) 0.0209(4) 0.3126(4) 0.0376(16) Uani 1 1 d . . . C20 C 0.5642(6) 0.0708(4) 0.3686(3) 0.0364(15) Uani 1 1 d . . . C21 C 0.6577(7) 0.1226(5) 0.3798(4) 0.0431(17) Uani 1 1 d . . . H21 H 0.7420 0.1224 0.3527 0.052 Uiso 1 1 calc R . . C22 C 0.5122(8) 0.1724(5) 0.4639(4) 0.057(2) Uani 1 1 d . . . H22 H 0.4938 0.2070 0.4970 0.068 Uiso 1 1 calc R . . C23 C 0.4118(8) 0.1254(6) 0.4570(4) 0.066(2) Uani 1 1 d . . . H23 H 0.3275 0.1286 0.4840 0.079 Uiso 1 1 calc R . . C24 C 0.4389(7) 0.0728(5) 0.4087(4) 0.055(2) Uani 1 1 d . . . H24 H 0.3732 0.0389 0.4032 0.066 Uiso 1 1 calc R . . C25 C 1.3387(6) 0.1077(4) 0.1887(3) 0.0266(13) Uani 1 1 d . . . C26 C 1.3230(5) 0.1917(4) 0.2182(3) 0.0258(13) Uani 1 1 d . . . C27 C 1.4343(6) 0.2335(4) 0.2214(3) 0.0313(14) Uani 1 1 d . . . H27 H 1.5236 0.2098 0.2048 0.038 Uiso 1 1 calc R . . C28 C 1.4121(6) 0.3103(4) 0.2492(4) 0.0396(16) Uani 1 1 d . . . H28 H 1.4855 0.3400 0.2512 0.047 Uiso 1 1 calc R . . C29 C 1.2783(7) 0.3424(5) 0.2742(4) 0.0458(18) Uani 1 1 d . . . H29 H 1.2633 0.3954 0.2920 0.055 Uiso 1 1 calc R . . C30 C 1.1925(6) 0.2287(4) 0.2449(3) 0.0384(16) Uani 1 1 d . . . H30 H 1.1170 0.2013 0.2424 0.046 Uiso 1 1 calc R . . C31 C 1.0841(6) 0.1819(4) 0.6922(3) 0.0324(14) Uani 1 1 d . . . C32 C 1.1176(6) 0.2540(4) 0.6260(3) 0.0281(13) Uani 1 1 d . . . C33 C 1.0172(6) 0.2969(4) 0.5785(3) 0.0317(14) Uani 1 1 d . . . H33 H 0.9297 0.2792 0.5890 0.038 Uiso 1 1 calc R . . C34 C 1.1651(7) 0.3881(5) 0.5057(3) 0.0415(16) Uani 1 1 d . . . H34 H 1.1814 0.4347 0.4648 0.050 Uiso 1 1 calc R . . C35 C 1.2721(7) 0.3494(4) 0.5496(4) 0.0414(16) Uani 1 1 d . . . H35 H 1.3576 0.3698 0.5387 0.050 Uiso 1 1 calc R . . C36 C 1.2485(6) 0.2793(4) 0.6100(3) 0.0337(14) Uani 1 1 d . . . H36 H 1.3197 0.2495 0.6396 0.040 Uiso 1 1 calc R . . Cu1 Cu 0.73999(10) 0.43968(6) 0.34138(6) 0.0660(3) Uani 1 1 d . . . Cu2 Cu 0.77255(10) 0.25605(7) 0.42780(6) 0.0622(3) Uani 1 1 d . . . Cu3 Cu 0.89987(10) 0.39892(7) 0.44703(5) 0.0571(3) Uani 1 1 d . . . Cu4 Cu 0.98478(9) 0.33271(8) 0.32572(6) 0.0650(3) Uani 1 1 d . . . Cu5 Cu 0.32627(9) 0.50407(6) 0.11508(6) 0.0587(3) Uani 1 1 d . . . Cu6 Cu 0.59103(10) 0.48578(6) 0.05367(6) 0.0599(3) Uani 1 1 d . . . N1 N 0.5643(5) 0.5353(3) 0.3277(3) 0.0317(12) Uani 1 1 d . . . N2 N 0.1320(5) 0.5657(4) 0.1378(3) 0.0411(14) Uani 1 1 d . . . N3 N 0.7580(5) 0.3803(3) 0.0583(3) 0.0338(12) Uani 1 1 d . . . N4 N 0.6345(6) 0.1726(4) 0.4268(3) 0.0480(15) Uani 1 1 d . . . N5 N 1.1690(5) 0.3017(4) 0.2741(3) 0.0413(14) Uani 1 1 d . . . N6 N 1.0388(5) 0.3624(4) 0.5186(3) 0.0385(13) Uani 1 1 d . . . O1 O 0.5624(4) 0.8184(3) 0.2219(3) 0.0453(12) Uani 1 1 d . . . O2 O 0.3391(4) 0.8419(3) 0.2009(2) 0.0390(11) Uani 1 1 d . . . O3 O 0.0576(4) 0.8429(3) 0.1531(3) 0.0424(11) Uani 1 1 d . . . O4 O -0.1649(4) 0.8671(3) 0.1277(2) 0.0368(10) Uani 1 1 d . . . O5 O 0.7320(4) 0.0924(3) 0.1126(2) 0.0385(11) Uani 1 1 d . . . O6 O 0.9464(4) 0.0497(3) 0.1450(2) 0.0427(11) Uani 1 1 d . . . O7 O 0.5318(4) -0.0411(3) 0.3096(2) 0.0456(12) Uani 1 1 d . . . O8 O 0.6965(4) 0.0457(3) 0.2665(2) 0.0383(10) Uani 1 1 d . . . O9 O 1.2305(4) 0.0833(3) 0.1796(2) 0.0373(11) Uani 1 1 d . . . O10 O 1.4597(4) 0.0660(3) 0.1749(2) 0.0426(11) Uani 1 1 d . . . O11 O 0.9615(4) 0.1645(3) 0.7030(2) 0.0428(11) Uani 1 1 d . . . O12 O 1.1784(4) 0.1434(3) 0.7322(2) 0.0439(11) Uani 1 1 d . . . O1W O 0.5708(5) 0.9600(4) 0.0811(3) 0.0565(13) Uani 1 1 d . . . O2W O 0.2575(5) 0.9298(3) 0.3086(2) 0.0495(12) Uani 1 1 d . . . O3W O -0.0209(4) 1.0398(3) 0.2787(2) 0.0411(11) Uani 1 1 d . . . O4W O 0.2283(5) 0.9777(3) 0.0807(2) 0.0528(13) Uani 1 1 d . . . O5W O 0.0692(8) 0.9677(5) 0.4151(3) 0.104(2) Uani 1 1 d . . . O6W O 0.0000 0.0000 0.0000 0.110(4) Uani 1 2 d S . . O7W O 0.3960(10) 0.8255(6) 0.0249(4) 0.127(3) Uani 1 1 d . . . O8W O 0.6690(11) 0.8430(6) 0.9947(5) 0.153(4) Uani 1 1 d . . . Tb1 Tb 0.66412(3) 0.952812(18) 0.189853(15) 0.02586(8) Uani 1 1 d . . . Tb2 Tb 0.13180(3) 0.948123(18) 0.203583(15) 0.02438(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0427(4) 0.0538(4) 0.0533(5) -0.0210(4) -0.0004(3) -0.0092(3) Br2 0.0391(4) 0.0372(3) 0.0415(4) -0.0116(3) 0.0016(3) -0.0110(3) Br3 0.0580(5) 0.0557(5) 0.0794(6) -0.0105(4) -0.0069(4) 0.0008(4) Br4 0.0524(5) 0.0553(5) 0.0763(6) -0.0187(4) -0.0187(4) -0.0159(4) Br5 0.0536(5) 0.0942(6) 0.0773(6) -0.0550(5) -0.0011(4) -0.0122(4) Br6 0.0418(4) 0.0349(3) 0.0498(4) -0.0092(3) -0.0025(3) -0.0032(3) C1 0.022(3) 0.024(3) 0.043(4) -0.016(3) -0.003(3) 0.000(2) C2 0.025(3) 0.020(3) 0.034(3) -0.013(3) -0.003(3) -0.005(2) C3 0.023(3) 0.028(3) 0.035(4) -0.008(3) -0.004(3) -0.002(2) C4 0.047(4) 0.034(4) 0.046(4) -0.001(3) -0.002(3) -0.015(3) C5 0.025(3) 0.037(4) 0.063(5) -0.007(3) -0.002(3) -0.011(3) C6 0.022(3) 0.033(3) 0.049(4) -0.009(3) -0.001(3) -0.002(3) C7 0.027(3) 0.030(3) 0.032(4) -0.012(3) 0.003(3) -0.007(3) C8 0.024(3) 0.031(3) 0.029(3) -0.011(3) -0.004(3) -0.002(2) C9 0.027(3) 0.036(3) 0.055(5) -0.022(3) -0.004(3) -0.005(3) C10 0.052(4) 0.027(3) 0.062(5) -0.018(3) -0.011(4) -0.006(3) C11 0.041(4) 0.039(4) 0.053(5) -0.012(3) -0.006(3) -0.016(3) C12 0.022(3) 0.041(4) 0.043(4) -0.015(3) -0.002(3) -0.007(3) C13 0.031(3) 0.025(3) 0.026(3) -0.003(3) 0.000(3) -0.007(3) C14 0.025(3) 0.020(3) 0.034(4) -0.002(3) -0.002(3) -0.005(2) C15 0.024(3) 0.035(4) 0.079(6) -0.005(4) -0.010(3) -0.001(3) C16 0.034(4) 0.040(4) 0.082(6) 0.003(4) -0.007(4) -0.021(3) C17 0.044(4) 0.021(3) 0.052(4) 0.002(3) -0.010(3) -0.012(3) C18 0.023(3) 0.021(3) 0.043(4) -0.003(3) 0.001(3) -0.004(2) C19 0.025(3) 0.034(3) 0.051(5) -0.009(3) -0.008(3) -0.001(3) C20 0.030(3) 0.034(3) 0.044(4) -0.008(3) 0.001(3) -0.006(3) C21 0.031(4) 0.053(4) 0.052(5) -0.024(4) 0.002(3) -0.012(3) C22 0.052(5) 0.068(5) 0.060(5) -0.037(4) 0.015(4) -0.017(4) C23 0.052(5) 0.100(7) 0.057(5) -0.042(5) 0.024(4) -0.026(5) C24 0.040(4) 0.067(5) 0.065(5) -0.022(4) 0.004(4) -0.026(4) C25 0.028(3) 0.021(3) 0.030(3) -0.005(2) -0.006(3) -0.002(2) C26 0.020(3) 0.019(3) 0.035(4) -0.004(2) -0.004(2) -0.001(2) C27 0.019(3) 0.031(3) 0.041(4) -0.006(3) -0.001(3) -0.004(2) C28 0.031(4) 0.037(4) 0.059(5) -0.017(3) -0.008(3) -0.014(3) C29 0.046(4) 0.038(4) 0.061(5) -0.022(4) -0.014(4) -0.006(3) C30 0.029(3) 0.037(4) 0.053(4) -0.018(3) -0.004(3) -0.005(3) C31 0.030(3) 0.022(3) 0.040(4) -0.006(3) 0.000(3) 0.000(3) C32 0.023(3) 0.025(3) 0.037(4) -0.009(3) 0.000(3) -0.007(2) C33 0.026(3) 0.033(3) 0.035(4) -0.005(3) -0.002(3) -0.010(3) C34 0.050(4) 0.041(4) 0.031(4) -0.003(3) 0.004(3) -0.017(3) C35 0.031(4) 0.044(4) 0.049(4) -0.010(3) 0.006(3) -0.018(3) C36 0.024(3) 0.037(3) 0.040(4) -0.013(3) 0.001(3) -0.005(3) Cu1 0.0417(5) 0.0424(5) 0.1007(9) -0.0053(5) -0.0208(5) 0.0111(4) Cu2 0.0549(6) 0.0551(6) 0.0869(8) -0.0304(5) -0.0033(5) -0.0177(5) Cu3 0.0622(6) 0.0670(6) 0.0402(5) -0.0026(5) -0.0137(5) -0.0185(5) Cu4 0.0348(5) 0.0785(7) 0.0931(8) -0.0526(6) 0.0074(5) -0.0013(5) Cu5 0.0433(5) 0.0490(5) 0.0826(8) -0.0281(5) -0.0102(5) 0.0118(4) Cu6 0.0533(6) 0.0341(5) 0.0787(7) -0.0122(5) 0.0066(5) 0.0106(4) N1 0.028(3) 0.026(3) 0.039(3) -0.003(2) -0.007(2) -0.005(2) N2 0.034(3) 0.031(3) 0.061(4) -0.021(3) -0.007(3) 0.004(2) N3 0.033(3) 0.024(3) 0.039(3) -0.004(2) -0.003(2) -0.001(2) N4 0.045(4) 0.049(3) 0.058(4) -0.027(3) 0.005(3) -0.014(3) N5 0.030(3) 0.043(3) 0.060(4) -0.031(3) -0.004(3) -0.003(2) N6 0.041(3) 0.037(3) 0.035(3) -0.003(3) -0.001(3) -0.012(2) O1 0.028(2) 0.026(2) 0.077(4) 0.002(2) -0.009(2) -0.0117(18) O2 0.025(2) 0.031(2) 0.053(3) -0.003(2) -0.004(2) 0.0034(18) O3 0.027(2) 0.035(2) 0.074(4) -0.030(2) -0.007(2) -0.0016(19) O4 0.027(2) 0.034(2) 0.050(3) -0.018(2) -0.009(2) 0.0056(18) O5 0.032(2) 0.027(2) 0.051(3) 0.000(2) -0.002(2) -0.0101(18) O6 0.040(3) 0.023(2) 0.062(3) -0.008(2) -0.022(2) 0.0085(19) O7 0.036(3) 0.049(3) 0.060(3) -0.023(2) 0.002(2) -0.017(2) O8 0.027(2) 0.045(3) 0.047(3) -0.016(2) 0.000(2) -0.0114(19) O9 0.026(2) 0.027(2) 0.064(3) -0.017(2) -0.005(2) -0.0076(18) O10 0.023(2) 0.043(3) 0.065(3) -0.029(2) -0.005(2) 0.0073(19) O11 0.031(2) 0.038(2) 0.050(3) 0.006(2) -0.003(2) -0.013(2) O12 0.031(2) 0.050(3) 0.039(3) 0.003(2) -0.010(2) 0.003(2) O1W 0.047(3) 0.066(3) 0.059(3) -0.020(3) -0.019(3) -0.002(2) O2W 0.037(3) 0.071(3) 0.045(3) -0.014(3) -0.012(2) -0.016(2) O3W 0.029(2) 0.050(3) 0.047(3) -0.024(2) 0.005(2) -0.003(2) O4W 0.065(3) 0.053(3) 0.038(3) -0.008(2) 0.003(2) -0.016(3) O5W 0.156(7) 0.095(5) 0.060(4) -0.028(4) 0.015(4) -0.021(5) O6W 0.101(8) 0.167(10) 0.059(6) -0.026(6) -0.027(5) -0.015(7) O7W 0.178(8) 0.109(6) 0.093(6) -0.041(5) -0.011(6) -0.001(6) O8W 0.197(10) 0.130(7) 0.122(7) -0.047(6) 0.038(7) -0.023(7) Tb1 0.01649(14) 0.01950(14) 0.03952(19) -0.00487(12) -0.00249(12) -0.00283(10) Tb2 0.01676(14) 0.02023(14) 0.03467(18) -0.00463(12) -0.00427(12) -0.00263(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 Br1 Cu3 2.3896(12) . ? Br1 Cu2 2.4180(12) . ? Br2 Cu3 2.3851(11) . ? Br2 Cu1 2.5331(12) . ? Br2 Cu4 2.5594(12) . ? Br3 Cu2 2.4111(13) . ? Br3 Cu4 2.6254(15) . ? Br4 Cu4 2.4207(13) . ? Br4 Cu1 2.4370(14) . ? Br5 Cu5 2.3606(13) . ? Br5 Cu6 2.4098(12) . ? Br6 Cu5 2.3575(11) . ? Br6 Cu6 2.5055(12) 2_665 ? Br6 Cu6 2.8270(12) . ? C1 O1 1.249(6) . ? C1 O2 1.250(6) . ? C1 C2 1.507(7) . ? C2 C6 1.377(8) . ? C2 C3 1.383(7) . ? C3 N1 1.338(7) . ? C3 H3 0.9300 . ? C4 C5 1.353(9) . ? C4 N1 1.356(8) . ? C4 H4 0.9300 . ? C5 C6 1.367(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O3 1.245(7) . ? C7 O4 1.265(7) . ? C7 C8 1.507(8) . ? C8 C9 1.377(8) . ? C8 C12 1.382(8) . ? C9 N2 1.341(7) . ? C9 H9 0.9300 . ? C10 N2 1.339(8) . ? C10 C11 1.374(9) . ? C10 H10 0.9300 . ? C11 C12 1.384(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 O6 1.239(7) . ? C13 O5 1.256(7) . ? C13 C14 1.504(7) . ? C14 C18 1.372(7) . ? C14 C15 1.377(8) . ? C15 C16 1.377(8) . ? C15 H15 0.9300 . ? C16 C17 1.358(9) . ? C16 H16 0.9300 . ? C17 N3 1.341(8) . ? C17 H17 0.9300 . ? C18 N3 1.327(7) . ? C18 H18 0.9300 . ? C19 O7 1.251(7) . ? C19 O8 1.283(7) . ? C19 C20 1.487(9) . ? C19 Tb1 2.882(7) 1_545 ? C20 C24 1.382(9) . ? C20 C21 1.388(8) . ? C21 N4 1.333(8) . ? C21 H21 0.9300 . ? C22 N4 1.329(9) . ? C22 C23 1.361(10) . ? C22 H22 0.9300 . ? C23 C24 1.381(10) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O9 1.242(6) . ? C25 O10 1.253(6) . ? C25 C26 1.495(8) . ? C26 C27 1.380(7) . ? C26 C30 1.387(8) . ? C27 C28 1.370(8) . ? C27 H27 0.9300 . ? C28 C29 1.380(9) . ? C28 H28 0.9300 . ? C29 N5 1.335(8) . ? C29 H29 0.9300 . ? C30 N5 1.337(8) . ? C30 H30 0.9300 . ? C31 O12 1.239(7) . ? C31 O11 1.262(7) . ? C31 C32 1.496(8) . ? C32 C33 1.385(8) . ? C32 C36 1.386(8) . ? C33 N6 1.337(7) . ? C33 H33 0.9300 . ? C34 N6 1.344(8) . ? C34 C35 1.381(9) . ? C34 H34 0.9300 . ? C35 C36 1.382(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? Cu1 N1 1.976(5) . ? Cu2 N4 2.021(6) . ? Cu3 N6 1.995(5) . ? Cu4 N5 1.999(5) . ? Cu5 N2 1.987(5) . ? Cu5 Cu6 2.7232(13) . ? Cu6 N3 1.998(5) . ? Cu6 Br6 2.5055(12) 2_665 ? Cu6 Cu6 2.867(2) 2_665 ? O1 Tb1 2.299(4) . ? O2 Tb2 2.295(4) . ? O3 Tb2 2.360(4) . ? O4 Tb1 2.337(4) 1_455 ? O5 Tb1 2.362(4) 1_545 ? O6 Tb2 2.309(4) 1_645 ? O7 Tb1 2.606(5) 1_545 ? O8 Tb1 2.431(4) 1_545 ? O9 Tb2 2.301(4) 1_645 ? O10 Tb1 2.313(4) 1_645 ? O11 Tb2 2.354(4) 2_666 ? O12 Tb1 2.299(4) 2_766 ? O1W Tb1 2.452(5) . ? O2W Tb2 2.507(4) . ? O3W Tb2 2.472(4) . ? O4W Tb2 2.485(5) . ? Tb1 O12 2.299(4) 2_766 ? Tb1 O10 2.313(4) 1_465 ? Tb1 O4 2.337(4) 1_655 ? Tb1 O5 2.362(4) 1_565 ? Tb1 O8 2.431(4) 1_565 ? Tb1 O7 2.606(5) 1_565 ? Tb1 C19 2.882(7) 1_565 ? Tb2 O9 2.301(4) 1_465 ? Tb2 O6 2.309(4) 1_465 ? Tb2 O11 2.354(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 Cu3 Br1 Cu2 71.44(4) . . ? Cu3 Br2 Cu1 65.49(4) . . ? Cu3 Br2 Cu4 70.41(4) . . ? Cu1 Br2 Cu4 61.82(3) . . ? Cu2 Br3 Cu4 70.11(4) . . ? Cu4 Br4 Cu1 65.17(4) . . ? Cu5 Br5 Cu6 69.61(4) . . ? Cu5 Br6 Cu6 87.46(4) . 2_665 ? Cu5 Br6 Cu6 62.60(3) . . ? Cu6 Br6 Cu6 64.71(4) 2_665 . ? O1 C1 O2 125.4(5) . . ? O1 C1 C2 116.9(5) . . ? O2 C1 C2 117.7(5) . . ? C6 C2 C3 118.5(5) . . ? C6 C2 C1 121.8(5) . . ? C3 C2 C1 119.7(5) . . ? N1 C3 C2 122.9(5) . . ? N1 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C5 C4 N1 123.2(6) . . ? C5 C4 H4 118.4 . . ? N1 C4 H4 118.4 . . ? C4 C5 C6 119.4(6) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C5 C6 C2 119.2(5) . . ? C5 C6 H6 120.4 . . ? C2 C6 H6 120.4 . . ? O3 C7 O4 126.3(5) . . ? O3 C7 C8 116.8(5) . . ? O4 C7 C8 116.9(5) . . ? C9 C8 C12 118.9(5) . . ? C9 C8 C7 119.3(5) . . ? C12 C8 C7 121.8(5) . . ? N2 C9 C8 122.8(6) . . ? N2 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? N2 C10 C11 123.6(6) . . ? N2 C10 H10 118.2 . . ? C11 C10 H10 118.2 . . ? C10 C11 C12 118.4(6) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C8 C12 C11 118.9(6) . . ? C8 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? O6 C13 O5 122.9(5) . . ? O6 C13 C14 119.6(5) . . ? O5 C13 C14 117.4(5) . . ? C18 C14 C15 118.9(5) . . ? C18 C14 C13 120.2(5) . . ? C15 C14 C13 120.8(5) . . ? C14 C15 C16 117.3(6) . . ? C14 C15 H15 121.4 . . ? C16 C15 H15 121.4 . . ? C17 C16 C15 120.2(6) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? N3 C17 C16 123.1(5) . . ? N3 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? N3 C18 C14 124.1(5) . . ? N3 C18 H18 117.9 . . ? C14 C18 H18 117.9 . . ? O7 C19 O8 121.4(6) . . ? O7 C19 C20 121.3(6) . . ? O8 C19 C20 117.3(5) . . ? O7 C19 Tb1 64.7(4) . 1_545 ? O8 C19 Tb1 56.9(3) . 1_545 ? C20 C19 Tb1 171.3(4) . 1_545 ? C24 C20 C21 117.2(6) . . ? C24 C20 C19 123.0(6) . . ? C21 C20 C19 119.7(6) . . ? N4 C21 C20 124.2(6) . . ? N4 C21 H21 117.9 . . ? C20 C21 H21 117.9 . . ? N4 C22 C23 124.8(7) . . ? N4 C22 H22 117.6 . . ? C23 C22 H22 117.6 . . ? C22 C23 C24 118.0(7) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C23 C24 C20 119.5(7) . . ? C23 C24 H24 120.2 . . ? C20 C24 H24 120.2 . . ? O9 C25 O10 123.8(5) . . ? O9 C25 C26 117.8(5) . . ? O10 C25 C26 118.3(5) . . ? C27 C26 C30 117.9(5) . . ? C27 C26 C25 122.6(5) . . ? C30 C26 C25 119.5(5) . . ? C28 C27 C26 119.5(5) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 118.4(6) . . ? C27 C28 H28 120.8 . . ? C29 C28 H28 120.8 . . ? N5 C29 C28 123.8(6) . . ? N5 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? N5 C30 C26 123.7(6) . . ? N5 C30 H30 118.1 . . ? C26 C30 H30 118.1 . . ? O12 C31 O11 124.8(6) . . ? O12 C31 C32 118.0(5) . . ? O11 C31 C32 117.3(5) . . ? C33 C32 C36 118.2(5) . . ? C33 C32 C31 120.2(5) . . ? C36 C32 C31 121.6(5) . . ? N6 C33 C32 123.7(5) . . ? N6 C33 H33 118.1 . . ? C32 C33 H33 118.1 . . ? N6 C34 C35 123.9(6) . . ? N6 C34 H34 118.0 . . ? C35 C34 H34 118.0 . . ? C34 C35 C36 118.1(6) . . ? C34 C35 H35 121.0 . . ? C36 C35 H35 121.0 . . ? C35 C36 C32 119.3(6) . . ? C35 C36 H36 120.4 . . ? C32 C36 H36 120.4 . . ? N1 Cu1 Br4 116.11(15) . . ? N1 Cu1 Br2 116.92(14) . . ? Br4 Cu1 Br2 109.13(5) . . ? N4 Cu2 Br3 119.07(17) . . ? N4 Cu2 Br1 110.38(16) . . ? Br3 Cu2 Br1 119.11(5) . . ? N6 Cu3 Br2 116.13(15) . . ? N6 Cu3 Br1 114.45(15) . . ? Br2 Cu3 Br1 126.65(5) . . ? N5 Cu4 Br4 115.19(16) . . ? N5 Cu4 Br2 107.35(15) . . ? Br4 Cu4 Br2 108.79(4) . . ? N5 Cu4 Br3 98.44(17) . . ? Br4 Cu4 Br3 107.28(5) . . ? Br2 Cu4 Br3 119.85(5) . . ? N2 Cu5 Br6 122.50(16) . . ? N2 Cu5 Br5 114.47(15) . . ? Br6 Cu5 Br5 122.29(5) . . ? N2 Cu5 Cu6 159.07(16) . . ? Br6 Cu5 Cu6 67.17(4) . . ? Br5 Cu5 Cu6 56.04(4) . . ? N3 Cu6 Br5 128.82(16) . . ? N3 Cu6 Br6 107.91(15) . 2_665 ? Br5 Cu6 Br6 101.38(4) . 2_665 ? N3 Cu6 Cu5 136.21(15) . . ? Br5 Cu6 Cu5 54.34(3) . . ? Br6 Cu6 Cu5 113.90(4) 2_665 . ? N3 Cu6 Br6 100.21(15) . . ? Br5 Cu6 Br6 103.91(4) . . ? Br6 Cu6 Br6 115.29(4) 2_665 . ? Cu5 Cu6 Br6 50.23(3) . . ? N3 Cu6 Cu6 116.33(16) . 2_665 ? Br5 Cu6 Cu6 114.18(5) . 2_665 ? Br6 Cu6 Cu6 63.08(4) 2_665 2_665 ? Cu5 Cu6 Cu6 73.93(4) . 2_665 ? Br6 Cu6 Cu6 52.21(4) . 2_665 ? C3 N1 C4 116.9(5) . . ? C3 N1 Cu1 121.9(4) . . ? C4 N1 Cu1 120.6(4) . . ? C10 N2 C9 117.3(5) . . ? C10 N2 Cu5 123.3(4) . . ? C9 N2 Cu5 118.8(4) . . ? C18 N3 C17 116.3(5) . . ? C18 N3 Cu6 123.7(4) . . ? C17 N3 Cu6 119.8(4) . . ? C22 N4 C21 116.2(6) . . ? C22 N4 Cu2 124.8(5) . . ? C21 N4 Cu2 118.4(5) . . ? C29 N5 C30 116.7(6) . . ? C29 N5 Cu4 123.2(4) . . ? C30 N5 Cu4 119.6(4) . . ? C33 N6 C34 116.7(5) . . ? C33 N6 Cu3 119.3(4) . . ? C34 N6 Cu3 123.0(4) . . ? C1 O1 Tb1 142.5(4) . . ? C1 O2 Tb2 151.1(4) . . ? C7 O3 Tb2 145.2(4) . . ? C7 O4 Tb1 134.5(4) . 1_455 ? C13 O5 Tb1 118.9(4) . 1_545 ? C13 O6 Tb2 172.8(4) . 1_645 ? C19 O7 Tb1 89.5(4) . 1_545 ? C19 O8 Tb1 96.9(4) . 1_545 ? C25 O9 Tb2 140.2(4) . 1_645 ? C25 O10 Tb1 158.6(4) . 1_645 ? C31 O11 Tb2 128.5(4) . 2_666 ? C31 O12 Tb1 169.5(4) . 2_766 ? O12 Tb1 O1 82.35(15) 2_766 . ? O12 Tb1 O10 145.48(16) 2_766 1_465 ? O1 Tb1 O10 97.17(15) . 1_465 ? O12 Tb1 O4 73.49(15) 2_766 1_655 ? O1 Tb1 O4 86.00(15) . 1_655 ? O10 Tb1 O4 141.03(15) 1_465 1_655 ? O12 Tb1 O5 117.12(15) 2_766 1_565 ? O1 Tb1 O5 155.60(17) . 1_565 ? O10 Tb1 O5 75.31(15) 1_465 1_565 ? O4 Tb1 O5 85.93(15) 1_655 1_565 ? O12 Tb1 O8 72.40(15) 2_766 1_565 ? O1 Tb1 O8 125.78(16) . 1_565 ? O10 Tb1 O8 80.48(14) 1_465 1_565 ? O4 Tb1 O8 128.27(14) 1_655 1_565 ? O5 Tb1 O8 76.54(15) 1_565 1_565 ? O12 Tb1 O1W 141.04(16) 2_766 . ? O1 Tb1 O1W 78.41(17) . . ? O10 Tb1 O1W 71.03(16) 1_465 . ? O4 Tb1 O1W 71.66(15) 1_655 . ? O5 Tb1 O1W 77.20(16) 1_565 . ? O8 Tb1 O1W 145.19(15) 1_565 . ? O12 Tb1 O7 76.92(15) 2_766 1_565 ? O1 Tb1 O7 76.32(16) . 1_565 ? O10 Tb1 O7 69.54(15) 1_465 1_565 ? O4 Tb1 O7 147.22(15) 1_655 1_565 ? O5 Tb1 O7 120.55(14) 1_565 1_565 ? O8 Tb1 O7 51.89(13) 1_565 1_565 ? O1W Tb1 O7 129.35(15) . 1_565 ? O12 Tb1 C19 74.24(16) 2_766 1_565 ? O1 Tb1 C19 101.30(18) . 1_565 ? O10 Tb1 C19 72.02(16) 1_465 1_565 ? O4 Tb1 C19 145.58(16) 1_655 1_565 ? O5 Tb1 C19 98.35(17) 1_565 1_565 ? O8 Tb1 C19 26.23(15) 1_565 1_565 ? O1W Tb1 C19 142.68(16) . 1_565 ? O7 Tb1 C19 25.72(15) 1_565 1_565 ? O2 Tb2 O9 95.89(14) . 1_465 ? O2 Tb2 O6 148.59(17) . 1_465 ? O9 Tb2 O6 85.50(14) 1_465 1_465 ? O2 Tb2 O11 91.00(15) . 2_666 ? O9 Tb2 O11 141.40(16) 1_465 2_666 ? O6 Tb2 O11 107.40(15) 1_465 2_666 ? O2 Tb2 O3 81.44(15) . . ? O9 Tb2 O3 143.98(17) 1_465 . ? O6 Tb2 O3 79.35(14) 1_465 . ? O11 Tb2 O3 74.60(16) 2_666 . ? O2 Tb2 O3W 141.97(16) . . ? O9 Tb2 O3W 78.53(14) 1_465 . ? O6 Tb2 O3W 69.13(15) 1_465 . ? O11 Tb2 O3W 72.97(15) 2_666 . ? O3 Tb2 O3W 124.41(14) . . ? O2 Tb2 O4W 72.59(16) . . ? O9 Tb2 O4W 73.58(16) 1_465 . ? O6 Tb2 O4W 77.81(17) 1_465 . ? O11 Tb2 O4W 143.93(16) 2_666 . ? O3 Tb2 O4W 71.37(16) . . ? O3W Tb2 O4W 137.97(15) . . ? O2 Tb2 O2W 70.88(16) . . ? O9 Tb2 O2W 74.48(15) 1_465 . ? O6 Tb2 O2W 138.47(16) 1_465 . ? O11 Tb2 O2W 72.10(15) 2_666 . ? O3 Tb2 O2W 135.71(16) . . ? O3W Tb2 O2W 71.40(15) . . ? O4W Tb2 O2W 127.78(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.266 _refine_diff_density_min -1.156 _refine_diff_density_rms 0.131 data_4 _database_code_depnum_ccdc_archive 'CCDC 777376' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H12 Br2 Cu2 Gd N2 O8, 2(H2 O)' _chemical_formula_sum 'C13 H16 Br2 Cu2 Gd N2 O10' _chemical_formula_weight 804.43 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' Cu Cu 0.3201 1.2651 '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 orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall -P2n2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.9176(8) _cell_length_b 32.983(3) _cell_length_c 12.9111(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4223.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5190 _cell_measurement_theta_min 1.23 _cell_measurement_theta_max 28.26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 8.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1887 _exptl_absorpt_correction_T_max 0.2961 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40482 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 28.26 _reflns_number_total 5190 _reflns_number_gt 3156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0114P)^2^+73.8981P] 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 5190 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1150 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Br1 Br 0.11809(17) 0.27892(4) 0.11395(11) 0.0706(4) Uani 1 1 d . . . Br2 Br -0.16662(18) 0.19658(5) 0.13277(12) 0.0785(5) Uani 1 1 d . . . C1 C -0.2422(10) -0.0787(3) 0.1836(7) 0.034(2) Uani 1 1 d . . . C2 C -0.1957(9) -0.1205(3) 0.1569(7) 0.027(2) Uani 1 1 d . . . C3 C -0.0640(10) -0.1293(3) 0.1299(8) 0.040(3) Uani 1 1 d . . . H3 H -0.0012 -0.1085 0.1234 0.048 Uiso 1 1 calc R . . C4 C -0.0265(12) -0.1684(4) 0.1127(9) 0.053(3) Uani 1 1 d . . . H4 H 0.0620 -0.1746 0.0951 0.063 Uiso 1 1 calc R . . C5 C -0.1211(14) -0.1987(3) 0.1217(9) 0.054(3) Uani 1 1 d . . . H5 H -0.0952 -0.2254 0.1094 0.065 Uiso 1 1 calc R . . C6 C -0.2849(11) -0.1526(3) 0.1626(8) 0.040(3) Uani 1 1 d . . . H6 H -0.3746 -0.1469 0.1778 0.048 Uiso 1 1 calc R . . C7 C 0.2621(11) 0.0573(3) 0.1809(7) 0.033(2) Uani 1 1 d . . . C8 C 0.2950(10) 0.0997(3) 0.1490(7) 0.032(2) Uani 1 1 d . . . C9 C 0.4252(11) 0.1124(4) 0.1267(10) 0.051(3) Uani 1 1 d . . . H9 H 0.4963 0.0940 0.1293 0.061 Uiso 1 1 calc R . . C10 C 0.4485(13) 0.1519(4) 0.1011(11) 0.067(4) Uani 1 1 d . . . H10 H 0.5349 0.1609 0.0847 0.080 Uiso 1 1 calc R . . C11 C 0.3417(14) 0.1781(4) 0.1001(10) 0.059(3) Uani 1 1 d . . . H11 H 0.3583 0.2051 0.0843 0.071 Uiso 1 1 calc R . . C12 C 0.1943(11) 0.1281(3) 0.1422(8) 0.039(3) Uani 1 1 d . . . H12 H 0.1062 0.1196 0.1536 0.047 Uiso 1 1 calc R . . C13 C -0.0626(9) -0.0144(3) 0.5009(7) 0.027(2) Uani 1 1 d . . . Cu1 Cu -0.3826(2) -0.23468(6) 0.18562(19) 0.0960(7) Uani 1 1 d . . . Cu2 Cu 0.0701(2) 0.20735(6) 0.14905(17) 0.0899(7) Uani 1 1 d . . . Gd1 Gd 0.0000 -0.003509(19) 0.2500 0.02580(16) Uani 1 2 d S . . Gd2 Gd 0.5000 -0.01792(2) 0.2500 0.03120(17) Uani 1 2 d S . . N1 N -0.2501(11) -0.1910(3) 0.1477(8) 0.055(3) Uani 1 1 d . . . N2 N 0.2147(10) 0.1671(3) 0.1203(7) 0.046(2) Uani 1 1 d . . . O1 O -0.1567(7) -0.0518(2) 0.2026(5) 0.0401(17) Uani 1 1 d . . . O2 O -0.3684(7) -0.0725(2) 0.1868(5) 0.0415(18) Uani 1 1 d . . . O3 O 0.1419(7) 0.0498(2) 0.2007(6) 0.0406(18) Uani 1 1 d . . . O4 O 0.3564(8) 0.0324(2) 0.1874(7) 0.054(2) Uani 1 1 d . . . O5 O -0.1062(6) -0.0262(2) 0.4150(5) 0.0323(15) Uani 1 1 d . . . O6 O -0.1094(6) -0.0229(2) 0.5893(5) 0.0341(16) Uani 1 1 d . . . O1W O 0.6965(14) 0.8760(3) 0.4214(11) 0.124(5) Uani 1 1 d . . . O2W O 0.797(2) 0.8951(4) 0.5857(15) 0.207(9) Uani 1 1 d . . . O3W O 0.3866(7) 0.0101(3) 0.4037(6) 0.055(2) Uani 1 1 d . . . O4W O 0.6223(7) -0.0470(2) 0.4007(5) 0.0393(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0909(11) 0.0508(8) 0.0700(9) 0.0121(7) 0.0086(8) 0.0008(8) Br2 0.0896(11) 0.0712(10) 0.0748(10) -0.0096(8) -0.0027(9) -0.0014(9) C1 0.029(6) 0.051(7) 0.023(4) 0.005(5) 0.000(5) -0.004(5) C2 0.028(5) 0.028(5) 0.026(5) -0.004(4) -0.002(4) -0.003(4) C3 0.027(6) 0.059(7) 0.034(6) -0.002(5) 0.000(5) -0.003(5) C4 0.050(8) 0.053(7) 0.056(7) -0.006(6) 0.013(6) 0.016(6) C5 0.082(10) 0.033(6) 0.047(7) -0.002(5) -0.014(7) 0.019(7) C6 0.032(6) 0.039(6) 0.049(7) 0.000(5) 0.003(5) -0.002(5) C7 0.034(6) 0.031(6) 0.034(5) 0.004(4) 0.006(5) -0.004(5) C8 0.026(5) 0.038(6) 0.031(5) 0.004(4) 0.004(4) -0.013(5) C9 0.027(6) 0.056(8) 0.070(8) 0.011(6) 0.006(6) -0.007(5) C10 0.039(7) 0.065(9) 0.097(11) 0.007(8) 0.021(8) -0.015(7) C11 0.073(10) 0.035(7) 0.069(9) 0.003(6) 0.010(8) -0.015(7) C12 0.031(6) 0.033(6) 0.054(7) 0.012(5) 0.000(5) 0.000(5) C13 0.015(4) 0.042(6) 0.025(5) -0.003(4) -0.004(4) 0.001(4) Cu1 0.1118(17) 0.0532(11) 0.1229(18) -0.0098(11) 0.0105(14) -0.0366(11) Cu2 0.0977(15) 0.0589(11) 0.1130(16) 0.0086(11) 0.0172(13) 0.0386(11) Gd1 0.0198(3) 0.0301(4) 0.0275(3) 0.000 0.0043(3) 0.000 Gd2 0.0222(3) 0.0358(4) 0.0356(3) 0.000 0.0031(4) 0.000 N1 0.060(7) 0.041(6) 0.065(7) -0.004(5) 0.000(6) 0.001(5) N2 0.053(6) 0.038(5) 0.046(5) 0.000(4) 0.004(5) 0.009(5) O1 0.034(4) 0.038(4) 0.048(4) -0.013(3) -0.003(4) -0.006(3) O2 0.028(4) 0.050(5) 0.046(4) -0.006(4) -0.001(3) 0.008(3) O3 0.036(4) 0.034(4) 0.052(4) 0.005(3) 0.018(4) -0.012(3) O4 0.044(5) 0.038(4) 0.079(6) 0.012(4) 0.005(4) 0.014(4) O5 0.026(4) 0.047(4) 0.024(3) 0.001(3) 0.004(3) -0.011(3) O6 0.023(4) 0.049(4) 0.030(4) -0.002(3) 0.005(3) -0.009(3) O1W 0.145(12) 0.077(8) 0.150(12) 0.002(8) 0.009(10) -0.010(8) O2W 0.30(3) 0.098(11) 0.221(19) 0.007(12) 0.040(18) -0.045(14) O3W 0.022(4) 0.087(6) 0.055(5) -0.029(5) 0.005(4) 0.003(4) O4W 0.030(4) 0.054(5) 0.034(4) 0.004(3) -0.003(3) -0.008(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 Br1 Cu2 2.450(2) . ? Br1 Cu1 2.552(3) 8_565 ? Br1 Cu1 2.626(3) 6_666 ? Br2 Cu2 2.384(3) . ? Br2 Cu1 2.418(3) 8_565 ? C1 O1 1.250(12) . ? C1 O2 1.269(12) . ? C1 C2 1.495(14) . ? C2 C6 1.381(13) . ? C2 C3 1.383(13) . ? C3 C4 1.361(15) . ? C3 H3 0.9300 . ? C4 C5 1.375(17) . ? C4 H4 0.9300 . ? C5 N1 1.347(15) . ? C5 H5 0.9300 . ? C6 N1 1.326(13) . ? C6 H6 0.9300 . ? C7 O3 1.243(11) . ? C7 O4 1.246(12) . ? C7 C8 1.496(13) . ? C8 C12 1.373(14) . ? C8 C9 1.387(14) . ? C9 C10 1.366(16) . ? C9 H9 0.9300 . ? C10 C11 1.366(17) . ? C10 H10 0.9300 . ? C11 N2 1.335(15) . ? C11 H11 0.9300 . ? C12 N2 1.332(12) . ? C12 H12 0.9300 . ? C13 O5 1.252(10) . ? C13 O6 1.263(10) . ? C13 C13 1.565(18) 5_556 ? Cu1 N1 2.011(10) . ? Cu1 Br2 2.418(3) 8 ? Cu1 Br1 2.552(3) 8 ? Cu1 Br1 2.626(3) 6_556 ? Cu1 Cu2 2.709(3) 8 ? Cu1 Cu1 2.861(5) 3_455 ? Cu1 Cu2 2.904(3) 6_556 ? Cu2 N2 1.989(9) . ? Cu2 Cu1 2.709(3) 8_565 ? Cu2 Cu1 2.904(3) 6_666 ? Cu2 Cu2 2.955(4) 3 ? Gd1 O1 2.309(7) . ? Gd1 O1 2.309(7) 3 ? Gd1 O3 2.341(6) . ? Gd1 O3 2.341(6) 3 ? Gd1 O5 2.492(6) . ? Gd1 O5 2.492(6) 3 ? Gd1 O6 2.498(6) 5_556 ? Gd1 O6 2.498(6) 7 ? Gd2 O4 2.332(7) . ? Gd2 O4 2.332(7) 3_655 ? Gd2 O2 2.368(7) 3 ? Gd2 O2 2.368(7) 1_655 ? Gd2 O3W 2.461(7) 3_655 ? Gd2 O3W 2.461(7) . ? Gd2 O4W 2.485(7) . ? Gd2 O4W 2.485(7) 3_655 ? O2 Gd2 2.368(7) 1_455 ? O6 Gd1 2.498(6) 5_556 ? 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 Cu2 Br1 Cu1 65.54(7) . 8_565 ? Cu2 Br1 Cu1 69.68(7) . 6_666 ? Cu1 Br1 Cu1 67.07(9) 8_565 6_666 ? Cu2 Br2 Cu1 68.68(8) . 8_565 ? O1 C1 O2 123.3(10) . . ? O1 C1 C2 119.3(9) . . ? O2 C1 C2 117.4(9) . . ? C6 C2 C3 117.3(9) . . ? C6 C2 C1 119.8(9) . . ? C3 C2 C1 122.9(9) . . ? C4 C3 C2 119.8(10) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.3(11) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 122.1(11) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N1 C6 C2 123.9(10) . . ? N1 C6 H6 118.1 . . ? C2 C6 H6 118.1 . . ? O3 C7 O4 125.1(9) . . ? O3 C7 C8 116.8(9) . . ? O4 C7 C8 118.0(9) . . ? C12 C8 C9 117.3(10) . . ? C12 C8 C7 119.9(9) . . ? C9 C8 C7 122.8(10) . . ? C10 C9 C8 119.7(11) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 118.2(12) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? N2 C11 C10 124.0(11) . . ? N2 C11 H11 118.0 . . ? C10 C11 H11 118.0 . . ? N2 C12 C8 124.2(10) . . ? N2 C12 H12 117.9 . . ? C8 C12 H12 117.9 . . ? O5 C13 O6 127.2(8) . . ? O5 C13 C13 116.7(10) . 5_556 ? O6 C13 C13 116.1(9) . 5_556 ? N1 Cu1 Br2 118.1(3) . 8 ? N1 Cu1 Br1 112.6(3) . 8 ? Br2 Cu1 Br1 104.31(9) 8 8 ? N1 Cu1 Br1 96.7(3) . 6_556 ? Br2 Cu1 Br1 115.96(10) 8 6_556 ? Br1 Cu1 Br1 109.24(9) 8 6_556 ? N1 Cu1 Cu2 155.8(3) . 8 ? Br2 Cu1 Cu2 55.07(7) 8 8 ? Br1 Cu1 Cu2 55.42(7) 8 8 ? Br1 Cu1 Cu2 107.10(9) 6_556 8 ? N1 Cu1 Cu1 132.3(3) . 3_455 ? Br2 Cu1 Cu1 109.16(7) 8 3_455 ? Br1 Cu1 Cu1 57.71(9) 8 3_455 ? Br1 Cu1 Cu1 55.22(9) 6_556 3_455 ? Cu2 Cu1 Cu1 62.77(8) 8 3_455 ? N1 Cu1 Cu2 139.2(3) . 6_556 ? Br2 Cu1 Cu2 67.82(7) 8 6_556 ? Br1 Cu1 Cu2 103.56(9) 8 6_556 ? Br1 Cu1 Cu2 52.31(7) 6_556 6_556 ? Cu2 Cu1 Cu2 63.41(9) 8 6_556 ? Cu1 Cu1 Cu2 56.04(7) 3_455 6_556 ? N2 Cu2 Br2 126.5(3) . . ? N2 Cu2 Br1 117.9(3) . . ? Br2 Cu2 Br1 108.57(9) . . ? N2 Cu2 Cu1 176.9(3) . 8_565 ? Br2 Cu2 Cu1 56.25(7) . 8_565 ? Br1 Cu2 Cu1 59.04(7) . 8_565 ? N2 Cu2 Cu1 117.4(3) . 6_666 ? Br2 Cu2 Cu1 108.79(9) . 6_666 ? Br1 Cu2 Cu1 58.01(7) . 6_666 ? Cu1 Cu2 Cu1 61.18(10) 8_565 6_666 ? N2 Cu2 Cu2 120.3(3) . 3 ? Br2 Cu2 Cu2 67.31(9) . 3 ? Br1 Cu2 Cu2 104.75(6) . 3 ? Cu1 Cu2 Cu2 61.51(8) 8_565 3 ? Cu1 Cu2 Cu2 55.07(7) 6_666 3 ? O1 Gd1 O1 92.6(4) . 3 ? O1 Gd1 O3 148.4(3) . . ? O1 Gd1 O3 100.7(2) 3 . ? O1 Gd1 O3 100.7(2) . 3 ? O1 Gd1 O3 148.4(3) 3 3 ? O3 Gd1 O3 82.6(3) . 3 ? O1 Gd1 O5 74.6(2) . . ? O1 Gd1 O5 81.4(2) 3 . ? O3 Gd1 O5 135.5(2) . . ? O3 Gd1 O5 74.9(2) 3 . ? O1 Gd1 O5 81.4(2) . 3 ? O1 Gd1 O5 74.6(2) 3 3 ? O3 Gd1 O5 74.9(2) . 3 ? O3 Gd1 O5 135.5(2) 3 3 ? O5 Gd1 O5 145.0(3) . 3 ? O1 Gd1 O6 138.9(2) . 5_556 ? O1 Gd1 O6 74.2(2) 3 5_556 ? O3 Gd1 O6 72.7(2) . 5_556 ? O3 Gd1 O6 76.9(2) 3 5_556 ? O5 Gd1 O6 65.1(2) . 5_556 ? O5 Gd1 O6 129.1(2) 3 5_556 ? O1 Gd1 O6 74.2(2) . 7 ? O1 Gd1 O6 138.9(2) 3 7 ? O3 Gd1 O6 76.9(2) . 7 ? O3 Gd1 O6 72.7(2) 3 7 ? O5 Gd1 O6 129.1(2) . 7 ? O5 Gd1 O6 65.1(2) 3 7 ? O6 Gd1 O6 139.2(3) 5_556 7 ? O4 Gd2 O4 89.2(4) . 3_655 ? O4 Gd2 O2 108.9(3) . 3 ? O4 Gd2 O2 139.3(3) 3_655 3 ? O4 Gd2 O2 139.3(3) . 1_655 ? O4 Gd2 O2 108.9(3) 3_655 1_655 ? O2 Gd2 O2 81.1(4) 3 1_655 ? O4 Gd2 O3W 74.5(3) . 3_655 ? O4 Gd2 O3W 74.5(3) 3_655 3_655 ? O2 Gd2 O3W 144.6(3) 3 3_655 ? O2 Gd2 O3W 75.9(3) 1_655 3_655 ? O4 Gd2 O3W 74.5(3) . . ? O4 Gd2 O3W 74.5(3) 3_655 . ? O2 Gd2 O3W 75.9(3) 3 . ? O2 Gd2 O3W 144.6(3) 1_655 . ? O3W Gd2 O3W 135.9(4) 3_655 . ? O4 Gd2 O4W 147.5(3) . . ? O4 Gd2 O4W 72.9(3) 3_655 . ? O2 Gd2 O4W 72.9(2) 3 . ? O2 Gd2 O4W 73.0(2) 1_655 . ? O3W Gd2 O4W 123.6(2) 3_655 . ? O3W Gd2 O4W 74.7(3) . . ? O4 Gd2 O4W 72.9(3) . 3_655 ? O4 Gd2 O4W 147.5(3) 3_655 3_655 ? O2 Gd2 O4W 73.0(2) 3 3_655 ? O2 Gd2 O4W 72.9(2) 1_655 3_655 ? O3W Gd2 O4W 74.7(3) 3_655 3_655 ? O3W Gd2 O4W 123.6(2) . 3_655 ? O4W Gd2 O4W 134.6(3) . 3_655 ? C6 N1 C5 117.6(10) . . ? C6 N1 Cu1 118.6(8) . . ? C5 N1 Cu1 123.1(8) . . ? C12 N2 C11 116.4(10) . . ? C12 N2 Cu2 119.6(8) . . ? C11 N2 Cu2 122.4(8) . . ? C1 O1 Gd1 175.9(7) . . ? C1 O2 Gd2 132.6(7) . 1_455 ? C7 O3 Gd1 141.3(7) . . ? C7 O4 Gd2 161.8(7) . . ? C13 O5 Gd1 121.2(6) . . ? C13 O6 Gd1 120.9(6) . 5_556 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.191 _refine_diff_density_min -1.363 _refine_diff_density_rms 0.186 data_5 _database_code_depnum_ccdc_archive 'CCDC 777377' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H12 Br2 Cu2 Er N2 O8, 2(H2 O)' _chemical_formula_sum 'C13 H16 Br2 Cu2 Er N2 O10' _chemical_formula_weight 814.44 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' Cu Cu 0.3201 1.2651 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall -P2n2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.8237(17) _cell_length_b 32.797(6) _cell_length_c 12.751(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4108.3(12) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4882 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 27.95 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 10.045 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1526 _exptl_absorpt_correction_T_max 0.2963 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42386 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.95 _reflns_number_total 4882 _reflns_number_gt 3476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0000P)^2^+265.7565P] 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 4882 _refine_ls_number_parameters 272 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.2021 _refine_ls_wR_factor_gt 0.1879 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.247 _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 Br1 Br -0.1184(3) 0.27905(7) 0.11200(19) 0.0582(6) Uani 1 1 d . . . Br2 Br 0.1700(3) 0.19688(8) 0.1325(2) 0.0642(7) Uani 1 1 d . . . C1 C -0.343(2) 0.1779(6) 0.0996(18) 0.049(6) Uani 1 1 d . . . H1 H -0.3603 0.2051 0.0838 0.059 Uiso 1 1 calc R . . C2 C -0.450(2) 0.1510(7) 0.103(2) 0.061(7) Uani 1 1 d . . . H2 H -0.5382 0.1600 0.0878 0.073 Uiso 1 1 calc R . . C3 C -0.4277(18) 0.1110(6) 0.1273(17) 0.040(5) Uani 1 1 d . . . H3 H -0.4993 0.0925 0.1301 0.048 Uiso 1 1 calc R . . C4 C -0.2962(17) 0.0988(5) 0.1479(13) 0.026(4) Uani 1 1 d . . . C5 C -0.1935(18) 0.1273(5) 0.1428(15) 0.033(4) Uani 1 1 d . . . H5 H -0.1051 0.1188 0.1569 0.040 Uiso 1 1 calc R . . C6 C -0.2624(17) 0.0564(6) 0.1810(12) 0.028(4) Uani 1 1 d . . . C7 C 0.0608(15) -0.0151(5) 0.5010(11) 0.021(3) Uani 1 1 d . . . C8 C 0.117(2) -0.1982(6) 0.1227(15) 0.042(5) Uani 1 1 d . . . H8 H 0.0897 -0.2251 0.1132 0.050 Uiso 1 1 calc R . . C9 C 0.0238(19) -0.1666(6) 0.1105(16) 0.044(5) Uani 1 1 d . . . H9 H -0.0648 -0.1723 0.0893 0.052 Uiso 1 1 calc R . . C10 C 0.0620(19) -0.1271(6) 0.1296(14) 0.035(4) Uani 1 1 d . . . H10 H -0.0017 -0.1062 0.1247 0.041 Uiso 1 1 calc R . . C11 C 0.1941(17) -0.1184(5) 0.1557(12) 0.024(3) Uani 1 1 d U . . C12 C 0.2853(18) -0.1513(6) 0.1649(14) 0.032(4) Uani 1 1 d . . . H12 H 0.3754 -0.1461 0.1832 0.039 Uiso 1 1 calc R . . C13 C 0.2425(17) -0.0768(6) 0.1850(12) 0.028(4) Uani 1 1 d . . . Cu1 Cu -0.0695(4) 0.20736(10) 0.1494(3) 0.0761(11) Uani 1 1 d . . . Cu2 Cu -0.1180(4) 0.26616(10) 0.3142(3) 0.0799(11) Uani 1 1 d . . . Er1 Er 0.5000 -0.01776(3) 0.2500 0.0250(3) Uani 1 2 d S . . Er2 Er 0.0000 -0.00308(3) 0.2500 0.0213(2) Uani 1 2 d S . . N1 N -0.2135(17) 0.1662(5) 0.1190(13) 0.039(4) Uani 1 1 d . . . N2 N 0.2454(18) -0.1900(5) 0.1479(15) 0.048(4) Uani 1 1 d . . . O1 O -0.1404(12) 0.0486(4) 0.2015(11) 0.035(3) Uani 1 1 d . . . O2 O -0.3574(13) 0.0310(4) 0.1887(12) 0.044(4) Uani 1 1 d . . . O3 O 0.1054(11) -0.0265(4) 0.4143(9) 0.029(3) Uani 1 1 d . . . O4 O 0.1074(11) -0.0238(4) 0.5903(9) 0.029(3) Uani 1 1 d . . . O5 O 0.1544(12) -0.0505(4) 0.2026(10) 0.034(3) Uani 1 1 d . . . O6 O 0.3685(12) -0.0703(4) 0.1890(10) 0.034(3) Uani 1 1 d . . . O1W O 0.3876(13) 0.0101(5) 0.0996(12) 0.054(4) Uani 1 1 d . . . O2W O 0.6181(12) -0.0460(4) 0.1001(10) 0.037(3) Uani 1 1 d . . . O3W O 0.694(3) 0.8775(6) 0.077(2) 0.131(10) Uani 1 1 d . . . O4W O 0.794(5) 0.8951(9) 0.918(3) 0.207(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0761(17) 0.0456(13) 0.0530(14) 0.0096(11) -0.0078(12) -0.0003(12) Br2 0.0729(17) 0.0618(16) 0.0578(15) -0.0098(13) 0.0053(13) 0.0028(13) C1 0.066(15) 0.025(10) 0.056(14) 0.009(9) -0.008(12) 0.014(10) C2 0.036(11) 0.048(13) 0.10(2) 0.009(14) -0.020(13) 0.021(10) C3 0.023(9) 0.043(11) 0.054(13) 0.020(10) -0.006(8) 0.003(8) C4 0.026(8) 0.029(9) 0.024(8) 0.008(7) -0.011(6) 0.003(7) C5 0.028(9) 0.023(9) 0.048(11) 0.006(8) -0.002(8) -0.003(7) C6 0.027(8) 0.036(10) 0.020(8) 0.007(7) -0.008(7) 0.000(7) C7 0.019(7) 0.037(9) 0.008(6) -0.008(7) 0.002(5) -0.001(6) C8 0.067(14) 0.027(10) 0.032(10) 0.006(8) 0.001(10) -0.020(10) C9 0.031(11) 0.053(13) 0.047(12) -0.006(10) -0.015(9) -0.009(9) C10 0.031(9) 0.048(12) 0.024(9) -0.002(8) -0.002(7) 0.001(9) C11 0.028(7) 0.030(7) 0.013(6) -0.006(5) 0.000(5) 0.005(6) C12 0.028(9) 0.040(11) 0.028(9) -0.002(8) -0.003(7) 0.005(8) C13 0.028(8) 0.035(10) 0.021(8) 0.001(7) -0.007(7) 0.003(7) Cu1 0.081(2) 0.0513(19) 0.095(3) 0.0047(18) -0.016(2) -0.0318(18) Cu2 0.091(3) 0.0457(18) 0.103(3) 0.0094(18) 0.011(2) 0.0299(18) Er1 0.0155(4) 0.0267(5) 0.0327(5) 0.000 -0.0100(5) 0.000 Er2 0.0140(4) 0.0228(5) 0.0272(5) 0.000 -0.0130(4) 0.000 N1 0.049(10) 0.032(9) 0.035(9) 0.001(7) -0.004(7) -0.010(8) N2 0.047(10) 0.027(9) 0.070(12) -0.012(9) 0.004(10) -0.002(8) O1 0.024(6) 0.033(7) 0.047(8) 0.006(6) -0.011(6) 0.008(5) O2 0.027(7) 0.032(7) 0.073(10) 0.014(7) -0.003(7) -0.013(6) O3 0.021(6) 0.048(8) 0.018(6) 0.000(5) -0.007(5) 0.003(5) O4 0.022(6) 0.041(7) 0.024(6) -0.001(5) -0.005(5) 0.009(5) O5 0.028(6) 0.024(6) 0.049(8) -0.010(6) -0.005(6) 0.007(5) O6 0.021(6) 0.045(8) 0.037(7) -0.006(6) -0.003(5) 0.000(5) O1W 0.018(6) 0.081(12) 0.063(10) 0.030(9) -0.003(7) -0.001(7) O2W 0.028(6) 0.056(9) 0.028(7) -0.010(6) 0.000(5) -0.013(6) O3W 0.17(3) 0.048(13) 0.18(3) -0.004(15) -0.02(2) -0.023(15) O4W 0.27(5) 0.11(2) 0.24(4) 0.00(3) -0.08(4) -0.03(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 Br1 Cu1 2.447(4) . ? Br1 Cu2 2.542(5) 3 ? Br1 Cu2 2.612(5) . ? Br2 Cu1 2.387(5) . ? Br2 Cu2 2.426(4) 3 ? C1 N1 1.35(3) . ? C1 C2 1.38(3) . ? C1 H1 0.9300 . ? C2 C3 1.37(3) . ? C2 H2 0.9300 . ? C3 C4 1.38(2) . ? C3 H3 0.9300 . ? C4 C5 1.38(2) . ? C4 C6 1.49(2) . ? C5 N1 1.32(2) . ? C5 H5 0.9300 . ? C6 O1 1.25(2) . ? C6 O2 1.26(2) . ? C7 O3 1.245(18) . ? C7 O4 1.260(18) . ? C7 C7 1.55(3) 5_556 ? C8 N2 1.33(3) . ? C8 C9 1.39(3) . ? C8 H8 0.9300 . ? C9 C10 1.37(3) . ? C9 H9 0.9300 . ? C10 C11 1.37(2) . ? C10 H10 0.9300 . ? C11 C12 1.41(2) . ? C11 C13 1.49(2) . ? C12 N2 1.35(2) . ? C12 H12 0.9300 . ? C13 O5 1.24(2) . ? C13 O6 1.26(2) . ? Cu1 N1 1.994(16) . ? Cu1 Cu2 2.707(4) 3 ? Cu1 Cu1 2.906(8) 3 ? Cu2 N2 2.027(18) 6_566 ? Cu2 Br2 2.426(4) 3 ? Cu2 Br1 2.542(5) 3 ? Cu2 Cu1 2.707(4) 3 ? Cu2 Cu2 2.838(8) 3 ? Er1 O2 2.265(12) 1_655 ? Er1 O2 2.265(12) 3 ? Er1 O6 2.290(12) . ? Er1 O6 2.290(12) 3_655 ? Er1 O1W 2.394(14) 3_655 ? Er1 O1W 2.394(14) . ? Er1 O2W 2.421(12) 3_655 ? Er1 O2W 2.421(12) . ? Er2 O5 2.255(11) . ? Er2 O5 2.255(11) 3 ? Er2 O1 2.271(11) 3 ? Er2 O1 2.271(11) . ? Er2 O4 2.457(11) 5_556 ? Er2 O4 2.457(11) 7 ? Er2 O3 2.460(11) 3 ? Er2 O3 2.460(11) . ? N2 Cu2 2.027(18) 6_656 ? O2 Er1 2.265(12) 1_455 ? O4 Er2 2.457(11) 5_556 ? 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 Cu1 Br1 Cu2 65.69(12) . 3 ? Cu1 Br1 Cu2 69.63(13) . . ? Cu2 Br1 Cu2 66.81(16) 3 . ? Cu1 Br2 Cu2 68.45(14) . 3 ? N1 C1 C2 122.2(18) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.8(19) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 118.4(19) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 118.7(16) . . ? C5 C4 C6 119.0(15) . . ? C3 C4 C6 122.3(16) . . ? N1 C5 C4 123.8(17) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? O1 C6 O2 123.9(17) . . ? O1 C6 C4 117.6(16) . . ? O2 C6 C4 118.4(15) . . ? O3 C7 O4 127.4(15) . . ? O3 C7 C7 116.5(16) . 5_556 ? O4 C7 C7 115.9(15) . 5_556 ? N2 C8 C9 120.0(18) . . ? N2 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.2(17) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.0(18) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 117.7(17) . . ? C10 C11 C13 123.6(16) . . ? C12 C11 C13 118.5(15) . . ? N2 C12 C11 121.5(17) . . ? N2 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? O5 C13 O6 124.3(17) . . ? O5 C13 C11 117.2(15) . . ? O6 C13 C11 118.6(16) . . ? N1 Cu1 Br2 125.7(5) . . ? N1 Cu1 Br1 118.3(5) . . ? Br2 Cu1 Br1 108.33(15) . . ? N1 Cu1 Cu2 177.1(5) . 3 ? Br2 Cu1 Cu2 56.46(13) . 3 ? Br1 Cu1 Cu2 58.84(12) . 3 ? N1 Cu1 Cu1 120.3(5) . 3 ? Br2 Cu1 Cu1 67.47(15) . 3 ? Br1 Cu1 Cu1 105.33(11) . 3 ? Cu2 Cu1 Cu1 61.90(14) 3 3 ? N2 Cu2 Br2 117.3(5) 6_566 3 ? N2 Cu2 Br1 113.5(5) 6_566 3 ? Br2 Cu2 Br1 104.13(16) 3 3 ? N2 Cu2 Br1 96.9(6) 6_566 . ? Br2 Cu2 Br1 115.33(18) 3 . ? Br1 Cu2 Br1 109.87(16) 3 . ? N2 Cu2 Cu1 156.3(6) 6_566 3 ? Br2 Cu2 Cu1 55.09(13) 3 3 ? Br1 Cu2 Cu1 55.47(12) 3 3 ? Br1 Cu2 Cu1 106.60(16) . 3 ? N2 Cu2 Cu2 132.7(5) 6_566 3 ? Br2 Cu2 Cu2 109.48(11) 3 3 ? Br1 Cu2 Cu2 57.78(15) 3 3 ? Br1 Cu2 Cu2 55.41(15) . 3 ? Cu1 Cu2 Cu2 62.81(15) 3 3 ? O2 Er1 O2 90.2(7) 1_655 3 ? O2 Er1 O6 139.7(5) 1_655 . ? O2 Er1 O6 107.4(4) 3 . ? O2 Er1 O6 107.4(4) 1_655 3_655 ? O2 Er1 O6 139.7(5) 3 3_655 ? O6 Er1 O6 82.4(6) . 3_655 ? O2 Er1 O1W 73.8(6) 1_655 3_655 ? O2 Er1 O1W 74.9(5) 3 3_655 ? O6 Er1 O1W 145.0(5) . 3_655 ? O6 Er1 O1W 75.8(5) 3_655 3_655 ? O2 Er1 O1W 74.9(5) 1_655 . ? O2 Er1 O1W 73.8(6) 3 . ? O6 Er1 O1W 75.8(5) . . ? O6 Er1 O1W 145.0(5) 3_655 . ? O1W Er1 O1W 135.1(8) 3_655 . ? O2 Er1 O2W 147.1(5) 1_655 3_655 ? O2 Er1 O2W 72.6(5) 3 3_655 ? O6 Er1 O2W 73.1(5) . 3_655 ? O6 Er1 O2W 73.4(4) 3_655 3_655 ? O1W Er1 O2W 74.6(5) 3_655 3_655 ? O1W Er1 O2W 123.9(4) . 3_655 ? O2 Er1 O2W 72.6(5) 1_655 . ? O2 Er1 O2W 147.1(5) 3 . ? O6 Er1 O2W 73.4(4) . . ? O6 Er1 O2W 73.1(5) 3_655 . ? O1W Er1 O2W 123.9(4) 3_655 . ? O1W Er1 O2W 74.6(5) . . ? O2W Er1 O2W 135.0(6) 3_655 . ? O5 Er2 O5 92.7(6) . 3 ? O5 Er2 O1 100.3(4) . 3 ? O5 Er2 O1 148.3(5) 3 3 ? O5 Er2 O1 148.3(5) . . ? O5 Er2 O1 100.3(4) 3 . ? O1 Er2 O1 83.4(6) 3 . ? O5 Er2 O4 139.3(4) . 5_556 ? O5 Er2 O4 74.7(4) 3 5_556 ? O1 Er2 O4 76.6(4) 3 5_556 ? O1 Er2 O4 72.4(4) . 5_556 ? O5 Er2 O4 74.7(4) . 7 ? O5 Er2 O4 139.3(4) 3 7 ? O1 Er2 O4 72.4(4) 3 7 ? O1 Er2 O4 76.6(4) . 7 ? O4 Er2 O4 138.0(6) 5_556 7 ? O5 Er2 O3 80.8(4) . 3 ? O5 Er2 O3 74.3(4) 3 3 ? O1 Er2 O3 136.1(4) 3 3 ? O1 Er2 O3 75.3(4) . 3 ? O4 Er2 O3 129.6(4) 5_556 3 ? O4 Er2 O3 65.6(4) 7 3 ? O5 Er2 O3 74.3(4) . . ? O5 Er2 O3 80.8(4) 3 . ? O1 Er2 O3 75.3(4) 3 . ? O1 Er2 O3 136.1(4) . . ? O4 Er2 O3 65.6(4) 5_556 . ? O4 Er2 O3 129.6(4) 7 . ? O3 Er2 O3 143.7(6) 3 . ? C5 N1 C1 117.1(17) . . ? C5 N1 Cu1 120.2(13) . . ? C1 N1 Cu1 120.7(14) . . ? C8 N2 C12 120.5(18) . . ? C8 N2 Cu2 122.8(14) . 6_656 ? C12 N2 Cu2 116.0(14) . 6_656 ? C6 O1 Er2 142.2(12) . . ? C6 O2 Er1 162.9(13) . 1_455 ? C7 O3 Er2 121.0(10) . . ? C7 O4 Er2 120.9(10) . 5_556 ? C13 O5 Er2 174.8(12) . . ? C13 O6 Er1 134.1(12) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 3.143 _refine_diff_density_min -3.439 _refine_diff_density_rms 0.298 data_8 _database_code_depnum_ccdc_archive 'CCDC 777378' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H13 Br3 Cu3 N2 O7 Tb' _chemical_formula_sum 'C14 H13 Br3 Cu3 N2 O7 Tb' _chemical_formula_weight 910.53 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' Cu Cu 0.3201 1.2651 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc 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 18.034(2) _cell_length_b 15.374(2) _cell_length_c 7.5997(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.1810(10) _cell_angle_gamma 90.00 _cell_volume 2101.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4942 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 27.82 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 12.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1964 _exptl_absorpt_correction_T_max 0.4453 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23321 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.82 _reflns_number_total 4942 _reflns_number_gt 4247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0508P)^2^+124.4343P] 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 4942 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.2016 _refine_ls_wR_factor_gt 0.1971 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.51826(11) 0.91105(13) 0.1762(3) 0.0462(4) Uani 1 1 d . . . Br2 Br 0.50207(10) 0.84532(12) 0.6607(3) 0.0427(4) Uani 1 1 d . . . Br3 Br 0.67888(10) 1.02760(12) 0.5892(3) 0.0478(5) Uani 1 1 d . . . C1 C 0.6421(8) 0.7251(11) 0.452(2) 0.032(3) Uani 1 1 d . . . H1 H 0.5939 0.7206 0.4876 0.039 Uiso 1 1 calc R . . C2 C 0.6810(9) 0.6505(10) 0.425(2) 0.034(3) Uani 1 1 d . . . H2 H 0.6596 0.5965 0.4426 0.041 Uiso 1 1 calc R . . C3 C 0.7525(8) 0.6563(9) 0.371(2) 0.028(3) Uani 1 1 d . . . H3 H 0.7800 0.6063 0.3527 0.034 Uiso 1 1 calc R . . C4 C 0.7825(7) 0.7386(9) 0.3446(18) 0.022(3) Uani 1 1 d . . . C5 C 0.7388(8) 0.8109(9) 0.3761(19) 0.025(3) Uani 1 1 d . . . H5 H 0.7580 0.8661 0.3589 0.030 Uiso 1 1 calc R . . C6 C 0.8598(7) 0.7489(8) 0.2848(18) 0.020(2) Uani 1 1 d . . . C7 C 1.3453(9) 0.8135(12) -0.043(3) 0.043(4) Uani 1 1 d . . . H7 H 1.3924 0.7885 -0.0378 0.052 Uiso 1 1 calc R . . C8 C 1.2861(10) 0.7668(12) 0.012(3) 0.050(5) Uani 1 1 d . . . H8 H 1.2941 0.7112 0.0577 0.060 Uiso 1 1 calc R . . C9 C 1.2145(9) 0.8010(11) -0.001(3) 0.040(4) Uani 1 1 d . . . H9 H 1.1737 0.7692 0.0310 0.048 Uiso 1 1 calc R . . C10 C 1.2074(8) 0.8858(9) -0.064(2) 0.026(3) Uani 1 1 d . . . C11 C 1.2681(8) 0.9299(10) -0.115(2) 0.030(3) Uani 1 1 d . . . H11 H 1.2619 0.9859 -0.1601 0.036 Uiso 1 1 calc R . . C12 C 1.1315(8) 0.9279(9) -0.075(2) 0.026(3) Uani 1 1 d . . . C13 C 1.0530(8) 0.9645(10) 0.314(2) 0.028(3) Uani 1 1 d . . . C14 C 1.1147(10) 0.9974(14) 0.447(2) 0.046(4) Uani 1 1 d . . . H14A H 1.1178 0.9606 0.5490 0.069 Uiso 1 1 calc R . . H14B H 1.1037 1.0558 0.4809 0.069 Uiso 1 1 calc R . . H14C H 1.1613 0.9964 0.3932 0.069 Uiso 1 1 calc R . . Cu1 Cu 0.60377(13) 0.90861(15) 0.4754(4) 0.0516(7) Uani 1 1 d . . . Cu2 Cu 0.44694(14) 0.93451(18) 0.4273(4) 0.0530(6) Uani 1 1 d . . . Cu3 Cu 0.42398(14) 0.95459(19) 0.8077(5) 0.0660(8) Uani 1 1 d . . . N1 N 0.6705(7) 0.8038(8) 0.4299(18) 0.029(3) Uani 1 1 d . . . N2 N 1.3352(8) 0.8953(9) -0.104(2) 0.042(4) Uani 1 1 d . . . O1 O 0.8757(6) 0.8181(6) 0.2131(15) 0.029(2) Uani 1 1 d . . . O2 O 0.9016(5) 0.6837(6) 0.3114(14) 0.026(2) Uani 1 1 d . . . O3 O 1.0265(7) 0.8909(7) 0.3310(15) 0.035(2) Uani 1 1 d . . . O4 O 1.0339(5) 1.0096(7) 0.1789(13) 0.025(2) Uani 1 1 d . . . O5 O 1.0776(5) 0.8786(7) -0.0513(16) 0.031(2) Uani 1 1 d . . . O6 O 1.1275(6) 1.0093(6) -0.0949(15) 0.030(2) Uani 1 1 d . . . O1W O 1.0050(7) 0.7405(7) 0.0819(15) 0.035(3) Uani 1 1 d . . . Tb1 Tb 0.96122(3) 0.88652(4) 0.04659(8) 0.01470(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0454(10) 0.0443(10) 0.0487(11) -0.0028(8) 0.0026(8) 0.0031(8) Br2 0.0341(8) 0.0458(10) 0.0490(10) 0.0005(8) 0.0086(7) 0.0099(7) Br3 0.0319(9) 0.0391(9) 0.0714(13) 0.0039(9) -0.0023(8) 0.0001(7) C1 0.016(6) 0.041(9) 0.041(9) -0.001(7) 0.009(6) -0.007(6) C2 0.032(8) 0.028(8) 0.043(9) 0.000(7) 0.009(7) -0.010(6) C3 0.029(7) 0.017(6) 0.038(8) -0.001(6) -0.002(6) 0.000(5) C4 0.018(6) 0.024(6) 0.025(7) 0.006(5) -0.006(5) 0.002(5) C5 0.025(7) 0.016(6) 0.034(7) 0.005(5) 0.002(6) -0.002(5) C6 0.018(6) 0.020(6) 0.022(6) 0.001(5) 0.001(5) -0.005(5) C7 0.025(8) 0.038(9) 0.065(12) -0.001(8) -0.003(8) 0.008(7) C8 0.030(9) 0.032(9) 0.087(15) 0.021(9) 0.007(9) 0.015(7) C9 0.023(7) 0.032(8) 0.067(12) 0.010(8) 0.005(8) 0.006(6) C10 0.020(6) 0.023(7) 0.035(8) 0.008(6) 0.006(6) 0.007(5) C11 0.026(7) 0.027(7) 0.038(8) 0.006(6) 0.007(6) 0.005(6) C12 0.020(6) 0.019(6) 0.038(8) -0.001(6) -0.003(6) 0.000(5) C13 0.025(7) 0.034(8) 0.026(7) -0.001(6) 0.007(6) -0.004(6) C14 0.042(10) 0.057(12) 0.037(9) -0.005(8) -0.013(8) -0.007(9) Cu1 0.0334(11) 0.0362(12) 0.0858(19) -0.0104(12) 0.0086(12) 0.0088(9) Cu2 0.0403(13) 0.0521(14) 0.0659(16) -0.0046(12) -0.0001(11) 0.0125(11) Cu3 0.0337(12) 0.0556(16) 0.111(3) -0.0071(16) 0.0229(14) -0.0068(11) N1 0.017(5) 0.029(6) 0.042(7) -0.002(5) -0.001(5) 0.002(5) N2 0.031(7) 0.032(7) 0.066(10) -0.007(7) 0.022(7) 0.003(6) O1 0.029(5) 0.019(5) 0.041(6) 0.005(4) 0.004(5) -0.004(4) O2 0.018(4) 0.025(5) 0.034(5) 0.003(4) 0.004(4) 0.006(4) O3 0.041(6) 0.028(5) 0.034(6) 0.007(5) -0.008(5) -0.005(5) O4 0.022(5) 0.028(5) 0.024(5) -0.001(4) -0.003(4) -0.004(4) O5 0.017(5) 0.023(5) 0.053(7) 0.004(5) 0.008(4) 0.001(4) O6 0.023(5) 0.021(5) 0.045(6) 0.008(4) 0.010(4) 0.007(4) O1W 0.044(6) 0.024(5) 0.040(6) 0.005(5) 0.016(5) 0.005(5) Tb1 0.0131(3) 0.0112(3) 0.0198(3) 0.0003(2) 0.0005(2) -0.0016(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 Br1 Cu3 2.312(3) 3_676 ? Br1 Cu2 2.405(3) . ? Br1 Cu1 2.653(4) . ? Br2 Cu3 2.506(3) . ? Br2 Cu1 2.583(3) . ? Br3 Cu2 2.337(3) 3_676 ? Br3 Cu1 2.400(3) . ? C1 N1 1.33(2) . ? C1 C2 1.37(2) . ? C1 H1 0.9300 . ? C2 C3 1.38(2) . ? C2 H2 0.9300 . ? C3 C4 1.398(19) . ? C3 H3 0.9300 . ? C4 C5 1.393(19) . ? C4 C6 1.505(18) . ? C5 N1 1.330(18) . ? C5 H5 0.9300 . ? C6 O1 1.239(16) . ? C6 O2 1.261(16) . ? C7 N2 1.35(2) . ? C7 C8 1.37(3) . ? C7 H7 0.9300 . ? C8 C9 1.39(2) . ? C8 H8 0.9300 . ? C9 C10 1.39(2) . ? C9 H9 0.9300 . ? C10 C11 1.37(2) . ? C10 C12 1.511(19) . ? C11 N2 1.32(2) . ? C11 H11 0.9300 . ? C12 O5 1.257(17) . ? C12 O6 1.261(17) . ? C13 O3 1.239(18) . ? C13 O4 1.269(18) . ? C13 C14 1.53(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? Cu1 N1 2.056(13) . ? Cu1 Cu2 2.701(3) 3_676 ? Cu1 Cu3 3.024(5) 3_676 ? Cu2 Br3 2.337(3) 3_676 ? Cu2 Cu1 2.701(3) 3_676 ? Cu2 Cu2 2.938(6) 3_676 ? Cu3 N2 2.001(15) 1_456 ? Cu3 Br1 2.313(3) 3_676 ? Cu3 Cu1 3.024(5) 3_676 ? N2 Cu3 2.001(14) 1_654 ? O1 Tb1 2.317(10) . ? O2 Tb1 2.288(10) 4_576 ? O3 Tb1 2.385(11) . ? O4 Tb1 2.348(10) 3_775 ? O4 Tb1 2.473(10) . ? O5 Tb1 2.280(10) . ? O6 Tb1 2.312(10) 3_775 ? O1W Tb1 2.389(11) . ? Tb1 O2 2.288(10) 4_575 ? Tb1 O6 2.312(10) 3_775 ? Tb1 O4 2.348(10) 3_775 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu3 Br1 Cu2 95.10(13) 3_676 . ? Cu3 Br1 Cu1 74.69(12) 3_676 . ? Cu2 Br1 Cu1 68.48(10) . . ? Cu3 Br2 Cu1 115.77(11) . . ? Cu2 Br3 Cu1 69.53(10) 3_676 . ? N1 C1 C2 122.5(13) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 119.4(14) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 118.6(14) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 117.9(13) . . ? C5 C4 C6 121.1(12) . . ? C3 C4 C6 121.0(12) . . ? N1 C5 C4 122.4(13) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? O1 C6 O2 126.7(12) . . ? O1 C6 C4 118.2(12) . . ? O2 C6 C4 115.1(11) . . ? N2 C7 C8 120.2(15) . . ? N2 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 121.2(16) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C10 116.1(15) . . ? C8 C9 H9 122.0 . . ? C10 C9 H9 122.0 . . ? C11 C10 C9 120.5(14) . . ? C11 C10 C12 120.8(13) . . ? C9 C10 C12 118.8(13) . . ? N2 C11 C10 122.0(14) . . ? N2 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? O5 C12 O6 125.2(13) . . ? O5 C12 C10 116.1(12) . . ? O6 C12 C10 118.4(12) . . ? O3 C13 O4 119.8(14) . . ? O3 C13 C14 120.2(15) . . ? O4 C13 C14 119.6(14) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 Cu1 Br3 109.7(4) . . ? N1 Cu1 Br2 104.1(4) . . ? Br3 Cu1 Br2 119.69(13) . . ? N1 Cu1 Br1 100.2(4) . . ? Br3 Cu1 Br1 125.14(13) . . ? Br2 Cu1 Br1 94.65(10) . . ? N1 Cu1 Cu2 163.7(4) . 3_676 ? Br3 Cu1 Cu2 54.14(9) . 3_676 ? Br2 Cu1 Cu2 85.37(10) . 3_676 ? Br1 Cu1 Cu2 91.98(10) . 3_676 ? N1 Cu1 Cu3 119.6(4) . 3_676 ? Br3 Cu1 Cu3 77.65(10) . 3_676 ? Br2 Cu1 Cu3 124.24(10) . 3_676 ? Br1 Cu1 Cu3 47.52(9) . 3_676 ? Cu2 Cu1 Cu3 62.09(10) 3_676 3_676 ? Br3 Cu2 Br1 124.61(14) 3_676 . ? Br3 Cu2 Cu1 56.32(9) 3_676 3_676 ? Br1 Cu2 Cu1 124.21(14) . 3_676 ? Br3 Cu2 Cu2 116.92(15) 3_676 3_676 ? Br1 Cu2 Cu2 91.70(14) . 3_676 ? Cu1 Cu2 Cu2 60.62(10) 3_676 3_676 ? N2 Cu3 Br1 139.2(4) 1_456 3_676 ? N2 Cu3 Br2 109.5(4) 1_456 . ? Br1 Cu3 Br2 110.90(12) 3_676 . ? N2 Cu3 Cu1 117.5(5) 1_456 3_676 ? Br1 Cu3 Cu1 57.79(10) 3_676 3_676 ? Br2 Cu3 Cu1 102.61(13) . 3_676 ? C1 N1 C5 119.2(13) . . ? C1 N1 Cu1 117.1(10) . . ? C5 N1 Cu1 123.6(10) . . ? C11 N2 C7 120.0(15) . . ? C11 N2 Cu3 123.1(12) . 1_654 ? C7 N2 Cu3 116.7(12) . 1_654 ? C6 O1 Tb1 144.6(10) . . ? C6 O2 Tb1 137.9(9) . 4_576 ? C13 O3 Tb1 95.9(9) . . ? C13 O4 Tb1 160.3(9) . 3_775 ? C13 O4 Tb1 90.9(9) . . ? Tb1 O4 Tb1 105.7(4) 3_775 . ? C12 O5 Tb1 139.0(10) . . ? C12 O6 Tb1 134.7(9) . 3_775 ? O5 Tb1 O2 96.4(4) . 4_575 ? O5 Tb1 O6 138.8(4) . 3_775 ? O2 Tb1 O6 99.2(4) 4_575 3_775 ? O5 Tb1 O1 144.9(4) . . ? O2 Tb1 O1 85.3(4) 4_575 . ? O6 Tb1 O1 74.5(4) 3_775 . ? O5 Tb1 O4 73.4(4) . 3_775 ? O2 Tb1 O4 78.0(3) 4_575 3_775 ? O6 Tb1 O4 73.0(4) 3_775 3_775 ? O1 Tb1 O4 140.3(4) . 3_775 ? O5 Tb1 O3 83.8(4) . . ? O2 Tb1 O3 153.3(4) 4_575 . ? O6 Tb1 O3 97.9(4) 3_775 . ? O1 Tb1 O3 79.7(4) . . ? O4 Tb1 O3 126.8(3) 3_775 . ? O5 Tb1 O1W 71.5(4) . . ? O2 Tb1 O1W 77.1(4) 4_575 . ? O6 Tb1 O1W 149.3(4) 3_775 . ? O1 Tb1 O1W 74.9(4) . . ? O4 Tb1 O1W 133.7(4) 3_775 . ? O3 Tb1 O1W 77.7(4) . . ? O5 Tb1 O4 72.6(4) . . ? O2 Tb1 O4 152.1(3) 4_575 . ? O6 Tb1 O4 75.9(4) 3_775 . ? O1 Tb1 O4 118.6(4) . . ? O4 Tb1 O4 74.3(4) 3_775 . ? O3 Tb1 O4 53.0(3) . . ? O1W Tb1 O4 120.9(4) . . ? O5 Tb1 Tb1 68.4(3) . 3_775 ? O2 Tb1 Tb1 116.2(3) 4_575 3_775 ? O6 Tb1 Tb1 70.5(3) 3_775 3_775 ? O1 Tb1 Tb1 141.1(3) . 3_775 ? O4 Tb1 Tb1 38.3(2) 3_775 3_775 ? O3 Tb1 Tb1 88.8(3) . 3_775 ? O1W Tb1 Tb1 138.8(3) . 3_775 ? O4 Tb1 Tb1 36.0(2) . 3_775 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 5.042 _refine_diff_density_min -2.658 _refine_diff_density_rms 0.367 data_9 _database_code_depnum_ccdc_archive 'CCDC 777379' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H32 Br7 Cu7 Er2 N6 O16' _chemical_formula_sum 'C36 H32 Br7 Cu7 Er2 N6 O16' _chemical_formula_weight 2143.35 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' Cu Cu 0.3201 1.2651 '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 monoclinic _symmetry_space_group_name_H-M P2/n _symmetry_space_group_name_Hall -P2yac loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 16.4842(17) _cell_length_b 9.8497(10) _cell_length_c 17.4990(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.952(2) _cell_angle_gamma 90.00 _cell_volume 2789.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6495 _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 27.78 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 10.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1316 _exptl_absorpt_correction_T_max 0.3867 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16884 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.78 _reflns_number_total 6495 _reflns_number_gt 3774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0790P)^2^+5.2852P] 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 6495 _refine_ls_number_parameters 368 _refine_ls_number_restraints 252 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1626 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.046 _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 Cu1 Cu 0.39820(11) 0.65696(16) 0.84309(12) 0.0797(6) Uani 1 1 d U . . Cu2 Cu 0.39341(14) 0.88995(19) 0.92071(12) 0.0929(7) Uani 1 1 d U . . Cu3 Cu 0.28356(13) 0.7453(3) 0.60608(18) 0.1189(9) Uani 1 1 d U . . Br1 Br 0.46284(8) 0.86688(13) 0.81255(8) 0.0617(4) Uani 1 1 d U . . Br2 Br 0.35517(8) 0.68261(13) 0.97634(8) 0.0626(4) Uani 1 1 d U . . Br3 Br 0.2500 0.6682(2) 0.7500 0.0561(7) Uani 0.746(4) 2 d SPU . 1 Br4 Br 0.2820(2) 0.9868(3) 0.63945(19) 0.1318(15) Uani 0.746(4) 1 d PU . 1 Cu4 Cu 0.1894(5) 0.8948(6) 0.7453(5) 0.119(2) Uani 0.3729(18) 1 d PU . 1 Cu5 Cu 0.3305(8) 0.9128(13) 0.7065(7) 0.050(3) Uani 0.1271(18) 1 d PU . 2 Br5 Br 0.2401(14) 1.0699(17) 0.7228(10) 0.123(7) Uani 0.1271(18) 1 d PU . 2 Br6 Br 0.3541(5) 0.9389(7) 0.5801(4) 0.096(3) Uani 0.254(4) 1 d PU . 2 C1 C 0.4297(9) 1.1709(14) 0.9572(8) 0.071(4) Uani 1 1 d U . . H1 H 0.4664 1.1612 0.9217 0.085 Uiso 1 1 calc R . . C2 C 0.3513(7) 1.0764(10) 1.0346(6) 0.047(3) Uani 1 1 d U . . H2 H 0.3287 0.9979 1.0541 0.057 Uiso 1 1 calc R . . C3 C 0.4140(9) 1.2985(13) 0.9814(8) 0.069(4) Uani 1 1 d U . . H3 H 0.4363 1.3758 0.9603 0.083 Uiso 1 1 calc R . . C4 C 0.3665(7) 1.3134(9) 1.0354(6) 0.044(3) Uani 1 1 d U . . H4 H 0.3549 1.4012 1.0530 0.053 Uiso 1 1 calc R . . C5 C 0.3352(6) 1.2010(9) 1.0646(6) 0.038(2) Uani 1 1 d U . . C6 C 0.2876(6) 1.2099(10) 1.1289(6) 0.039(2) Uani 1 1 d U . . C7 C 0.6307(6) 0.2907(10) 0.7957(6) 0.040(2) Uani 1 1 d U . . C8 C 0.5416(6) 0.3230(9) 0.7918(6) 0.035(2) Uani 1 1 d U . . C9 C 0.4814(8) 0.2284(11) 0.7609(8) 0.064(3) Uani 1 1 d U . . H9 H 0.4966 0.1420 0.7440 0.076 Uiso 1 1 calc R . . C10 C 0.3996(9) 0.2626(15) 0.7552(9) 0.086(4) Uani 1 1 d U . . H10 H 0.3570 0.2002 0.7347 0.104 Uiso 1 1 calc R . . C11 C 0.3810(8) 0.3878(14) 0.7798(9) 0.073(4) Uani 1 1 d U . . H11 H 0.3244 0.4114 0.7747 0.087 Uiso 1 1 calc R . . C12 C 0.5145(6) 0.4451(9) 0.8143(6) 0.036(2) Uani 1 1 d U . . H12 H 0.5551 0.5108 0.8344 0.043 Uiso 1 1 calc R . . C13 C 0.5930(7) 0.5352(11) 0.6576(6) 0.042(2) Uani 1 1 d U . . C14 C 0.5050(7) 0.5182(12) 0.6187(7) 0.051(3) Uani 1 1 d U . . C15 C 0.4776(8) 0.4042(15) 0.5769(8) 0.069(4) Uani 1 1 d U . . H15 H 0.5160 0.3345 0.5716 0.082 Uiso 1 1 calc R . . C16 C 0.3950(9) 0.3877(17) 0.5421(9) 0.084(4) Uani 1 1 d U . . H16 H 0.3742 0.3089 0.5137 0.101 Uiso 1 1 calc R . . C17 C 0.3460(10) 0.4980(19) 0.5530(10) 0.087(5) Uani 1 1 d U . . H17 H 0.2895 0.4915 0.5288 0.104 Uiso 1 1 calc R . . C18 C 0.4474(7) 0.6166(12) 0.6257(7) 0.057(3) Uani 1 1 d U . . H18 H 0.4645 0.6953 0.6559 0.069 Uiso 1 1 calc R . . Er1 Er 0.7500 0.04170(6) 0.7500 0.0384(2) Uani 1 2 d SU . . Er2 Er 0.7500 0.54010(5) 0.7500 0.03115(18) Uani 1 2 d SU . . N1 N 0.3959(6) 1.0597(9) 0.9809(6) 0.056(3) Uani 1 1 d U . . N2 N 0.4368(5) 0.4790(8) 0.8104(5) 0.045(2) Uani 1 1 d U . . N3 N 0.3663(7) 0.6039(13) 0.5903(7) 0.070(3) Uani 1 1 d U . . O1 O 0.2739(5) 1.3216(7) 1.1545(5) 0.056(2) Uani 1 1 d U . . O2 O 0.2635(6) 1.0979(9) 1.1531(5) 0.069(2) Uani 1 1 d U . . O3 O 0.6483(5) 0.1677(7) 0.7859(5) 0.061(2) Uani 1 1 d U . . O4 O 0.6814(4) 0.3839(7) 0.8085(4) 0.0474(18) Uani 1 1 d U . . O5 O 0.6124(4) 0.6347(7) 0.7026(4) 0.0455(17) Uani 1 1 d U . . O6 O 0.6449(5) 0.4460(7) 0.6471(4) 0.0471(18) Uani 1 1 d U . . O1W O 0.6830(6) 0.1608(8) 0.6331(5) 0.068(2) Uani 1 1 d U . . O2W O 0.6169(5) -0.0803(7) 0.7076(5) 0.056(2) Uani 1 1 d U . . 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 Cu1 0.0725(12) 0.0466(9) 0.1200(16) -0.0206(9) 0.0180(11) 0.0136(8) Cu2 0.1293(18) 0.0666(11) 0.0947(15) -0.0321(10) 0.0517(13) 0.0015(11) Cu3 0.0645(14) 0.0979(15) 0.187(3) 0.0098(16) 0.0047(15) 0.0132(12) Br1 0.0632(8) 0.0588(7) 0.0683(9) -0.0061(6) 0.0261(7) -0.0143(6) Br2 0.0496(7) 0.0646(8) 0.0734(9) 0.0089(6) 0.0111(6) -0.0018(6) Br3 0.0326(12) 0.0592(14) 0.0719(17) 0.000 -0.0014(10) 0.000 Br4 0.155(3) 0.0703(15) 0.139(3) -0.0019(15) -0.050(2) -0.0223(16) Cu4 0.137(5) 0.068(3) 0.136(6) -0.001(4) -0.015(5) 0.016(3) Cu5 0.055(6) 0.058(6) 0.043(6) 0.005(5) 0.020(5) 0.014(5) Br5 0.116(9) 0.121(9) 0.136(12) 0.003(7) 0.034(9) 0.006(8) Br6 0.089(5) 0.093(5) 0.098(5) 0.028(4) -0.007(4) -0.024(3) C1 0.074(7) 0.080(7) 0.071(7) -0.004(6) 0.044(6) -0.003(6) C2 0.060(6) 0.032(5) 0.056(6) -0.005(4) 0.028(5) -0.005(4) C3 0.078(7) 0.069(7) 0.069(7) 0.005(6) 0.033(6) -0.019(6) C4 0.058(6) 0.028(5) 0.047(6) 0.002(4) 0.011(5) -0.005(4) C5 0.039(5) 0.036(5) 0.039(5) 0.001(4) 0.012(4) -0.002(4) C6 0.034(5) 0.039(5) 0.044(5) 0.006(4) 0.010(4) 0.007(4) C7 0.035(5) 0.043(5) 0.047(6) 0.004(4) 0.021(4) 0.006(4) C8 0.038(5) 0.028(4) 0.039(5) 0.002(4) 0.006(4) -0.005(4) C9 0.060(7) 0.033(5) 0.094(8) -0.020(5) 0.005(6) 0.004(5) C10 0.070(8) 0.066(7) 0.112(9) -0.021(7) -0.013(7) -0.004(6) C11 0.049(6) 0.062(7) 0.101(8) -0.002(6) -0.001(6) 0.010(6) C12 0.039(5) 0.025(4) 0.044(5) -0.002(4) 0.010(4) -0.008(4) C13 0.047(5) 0.043(5) 0.039(5) 0.014(4) 0.012(4) -0.001(5) C14 0.048(6) 0.059(6) 0.046(6) 0.009(5) 0.013(5) -0.004(5) C15 0.064(7) 0.074(7) 0.065(7) 0.007(6) 0.002(6) -0.002(6) C16 0.072(8) 0.096(8) 0.076(8) -0.012(7) -0.004(6) -0.012(7) C17 0.067(8) 0.104(8) 0.086(8) -0.001(7) 0.006(7) 0.004(7) C18 0.055(6) 0.058(6) 0.059(7) 0.000(5) 0.011(5) 0.001(5) Er1 0.0426(4) 0.0231(3) 0.0555(5) 0.000 0.0249(3) 0.000 Er2 0.0332(3) 0.0219(3) 0.0420(4) 0.000 0.0163(3) 0.000 N1 0.060(6) 0.053(5) 0.062(6) -0.007(4) 0.028(5) -0.009(4) N2 0.040(5) 0.031(4) 0.059(5) -0.004(4) 0.003(4) 0.000(4) N3 0.049(6) 0.087(7) 0.072(7) 0.003(6) 0.003(5) 0.002(5) O1 0.063(5) 0.050(4) 0.059(5) -0.017(3) 0.023(4) 0.010(4) O2 0.085(6) 0.064(5) 0.068(5) 0.017(4) 0.043(5) 0.003(4) O3 0.059(5) 0.042(4) 0.086(6) -0.021(4) 0.026(4) 0.007(3) O4 0.043(4) 0.046(4) 0.056(5) 0.018(3) 0.017(3) -0.006(3) O5 0.037(4) 0.040(4) 0.059(5) 0.002(3) 0.007(3) 0.002(3) O6 0.048(4) 0.043(4) 0.051(4) -0.012(3) 0.010(3) 0.002(3) O1W 0.081(6) 0.047(4) 0.075(6) 0.001(4) 0.012(4) -0.004(4) O2W 0.050(4) 0.039(4) 0.083(5) -0.012(4) 0.024(4) -0.004(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 Cu1 N2 1.985(8) . ? Cu1 Br1 2.432(2) . ? Cu1 Br2 2.575(2) . ? Cu1 Br3 2.669(2) . ? Cu1 Cu4 3.020(7) 2_556 ? Cu2 N1 1.973(9) . ? Cu2 Br2 2.398(2) . ? Cu2 Br1 2.401(2) . ? Cu2 Cu4 2.967(8) 2_556 ? Cu3 N3 2.005(12) . ? Cu3 Br6 2.323(7) . ? Cu3 Br4 2.450(4) . ? Cu3 Br2 2.537(3) 2_556 ? Cu3 Br3 2.785(3) . ? Cu3 Cu4 2.948(8) 2_556 ? Br1 Cu4 2.537(7) 2_556 ? Br1 Cu5 2.621(14) . ? Br2 Cu3 2.537(3) 2_556 ? Br3 Cu4 2.440(7) 2_556 ? Br3 Cu4 2.440(7) . ? Br3 Cu1 2.669(2) 2_556 ? Br3 Cu3 2.785(3) 2_556 ? Br4 Cu4 2.179(9) 2_556 ? Br4 Cu4 2.767(10) . ? Cu4 Cu4 1.972(16) 2_556 ? Cu4 Br4 2.179(9) 2_556 ? Cu4 Br1 2.537(7) 2_556 ? Cu4 Cu3 2.948(8) 2_556 ? Cu4 Cu2 2.967(8) 2_556 ? Cu4 Cu1 3.020(7) 2_556 ? Cu5 Br5 2.20(2) . ? Cu5 Br6 2.331(14) . ? Cu5 Br5 2.41(2) 2_556 ? Br5 Br5 0.95(3) 2_556 ? Br5 Cu5 2.41(2) 2_556 ? C1 N1 1.331(15) . ? C1 C3 1.366(17) . ? C1 H1 0.9500 . ? C2 N1 1.308(12) . ? C2 C5 1.380(13) . ? C2 H2 0.9500 . ? C3 C4 1.345(15) . ? C3 H3 0.9500 . ? C4 C5 1.361(12) . ? C4 H4 0.9500 . ? C5 C6 1.492(13) . ? C6 O1 1.225(11) . ? C6 O2 1.272(12) . ? C7 O4 1.234(12) . ? C7 O3 1.264(11) . ? C7 C8 1.491(13) . ? C8 C12 1.368(12) . ? C8 C9 1.393(15) . ? C9 C10 1.376(17) . ? C9 H9 0.9500 . ? C10 C11 1.361(18) . ? C10 H10 0.9500 . ? C11 N2 1.323(15) . ? C11 H11 0.9500 . ? C12 N2 1.313(12) . ? C12 H12 0.9500 . ? C13 O5 1.259(12) . ? C13 O6 1.264(12) . ? C13 C14 1.490(16) . ? C14 C15 1.369(17) . ? C14 C18 1.379(16) . ? C15 C16 1.392(18) . ? C15 H15 0.9500 . ? C16 C17 1.39(2) . ? C16 H16 0.9500 . ? C17 N3 1.242(19) . ? C17 H17 0.9500 . ? C18 N3 1.369(15) . ? C18 H18 0.9500 . ? Er1 O2 2.226(8) 4_665 ? Er1 O2 2.226(8) 3_667 ? Er1 O3 2.269(7) . ? Er1 O3 2.269(7) 2_656 ? Er1 O1W 2.433(9) . ? Er1 O1W 2.433(9) 2_656 ? Er1 O2W 2.488(8) . ? Er1 O2W 2.488(7) 2_656 ? Er2 O1 2.248(7) 3_677 ? Er2 O1 2.248(7) 4_675 ? Er2 O4 2.266(6) . ? Er2 O4 2.266(6) 2_656 ? Er2 O6 2.432(7) . ? Er2 O6 2.432(7) 2_656 ? Er2 O5 2.447(7) 2_656 ? Er2 O5 2.447(7) . ? Er2 C13 2.779(11) 2_656 ? O1 Er2 2.248(7) 3_677 ? O2 Er1 2.226(8) 3_667 ? 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 N2 Cu1 Br1 120.6(3) . . ? N2 Cu1 Br2 120.4(3) . . ? Br1 Cu1 Br2 108.86(7) . . ? N2 Cu1 Br3 99.6(3) . . ? Br1 Cu1 Br3 102.67(9) . . ? Br2 Cu1 Br3 99.84(7) . . ? N2 Cu1 Cu4 133.2(3) . 2_556 ? Br1 Cu1 Cu4 54.18(14) . 2_556 ? Br2 Cu1 Cu4 101.57(18) . 2_556 ? Br3 Cu1 Cu4 50.35(14) . 2_556 ? N1 Cu2 Br2 119.0(3) . . ? N1 Cu2 Br1 122.5(3) . . ? Br2 Cu2 Br1 116.16(8) . . ? N1 Cu2 Cu4 117.9(3) . 2_556 ? Br2 Cu2 Cu4 107.68(15) . 2_556 ? Br1 Cu2 Cu4 55.20(17) . 2_556 ? N3 Cu3 Br6 99.5(4) . . ? N3 Cu3 Br4 138.2(4) . . ? Br6 Cu3 Br4 43.8(2) . . ? N3 Cu3 Br2 108.4(4) . 2_556 ? Br6 Cu3 Br2 121.3(2) . 2_556 ? Br4 Cu3 Br2 108.83(11) . 2_556 ? N3 Cu3 Br3 101.1(3) . . ? Br6 Cu3 Br3 126.4(2) . . ? Br4 Cu3 Br3 92.09(13) . . ? Br2 Cu3 Br3 97.77(9) 2_556 . ? N3 Cu3 Cu4 118.4(4) . 2_556 ? Br6 Cu3 Cu4 76.4(3) . 2_556 ? Br4 Cu3 Cu4 46.49(16) . 2_556 ? Br2 Cu3 Cu4 126.28(18) 2_556 2_556 ? Br3 Cu3 Cu4 50.29(16) . 2_556 ? Cu2 Br1 Cu1 67.23(7) . . ? Cu2 Br1 Cu4 73.8(2) . 2_556 ? Cu1 Br1 Cu4 74.82(17) . 2_556 ? Cu2 Br1 Cu5 94.8(2) . . ? Cu1 Br1 Cu5 87.8(3) . . ? Cu2 Br2 Cu3 80.79(9) . 2_556 ? Cu2 Br2 Cu1 64.98(6) . . ? Cu3 Br2 Cu1 83.27(9) 2_556 . ? Cu4 Br3 Cu4 47.7(4) 2_556 . ? Cu4 Br3 Cu1 72.31(18) 2_556 . ? Cu4 Br3 Cu1 112.30(19) . . ? Cu4 Br3 Cu1 112.30(18) 2_556 2_556 ? Cu4 Br3 Cu1 72.31(18) . 2_556 ? Cu1 Br3 Cu1 175.27(12) . 2_556 ? Cu4 Br3 Cu3 82.6(2) 2_556 2_556 ? Cu4 Br3 Cu3 68.3(2) . 2_556 ? Cu1 Br3 Cu3 77.02(6) . 2_556 ? Cu1 Br3 Cu3 104.31(7) 2_556 2_556 ? Cu4 Br3 Cu3 68.3(2) 2_556 . ? Cu4 Br3 Cu3 82.6(2) . . ? Cu1 Br3 Cu3 104.31(7) . . ? Cu1 Br3 Cu3 77.02(6) 2_556 . ? Cu3 Br3 Cu3 148.33(14) 2_556 . ? Cu4 Br4 Cu3 78.9(2) 2_556 . ? Cu4 Br4 Cu4 45.1(3) 2_556 . ? Cu3 Br4 Cu4 82.75(17) . . ? Cu4 Cu4 Br4 83.5(4) 2_556 2_556 ? Cu4 Cu4 Br3 66.17(18) 2_556 . ? Br4 Cu4 Br3 109.5(3) 2_556 . ? Cu4 Cu4 Br1 160.5(7) 2_556 2_556 ? Br4 Cu4 Br1 116.0(4) 2_556 2_556 ? Br3 Cu4 Br1 106.4(3) . 2_556 ? Cu4 Cu4 Br4 51.5(4) 2_556 . ? Br4 Cu4 Br4 115.7(3) 2_556 . ? Br3 Cu4 Br4 92.7(3) . . ? Br1 Cu4 Br4 113.5(3) 2_556 . ? Cu4 Cu4 Cu3 86.9(4) 2_556 2_556 ? Br4 Cu4 Cu3 54.6(2) 2_556 2_556 ? Br3 Cu4 Cu3 61.39(16) . 2_556 ? Br1 Cu4 Cu3 105.7(3) 2_556 2_556 ? Br4 Cu4 Cu3 138.1(3) . 2_556 ? Cu4 Cu4 Cu2 110.6(6) 2_556 2_556 ? Br4 Cu4 Cu2 153.0(3) 2_556 2_556 ? Br3 Cu4 Cu2 97.3(3) . 2_556 ? Br1 Cu4 Cu2 51.01(14) 2_556 2_556 ? Br4 Cu4 Cu2 63.9(2) . 2_556 ? Cu3 Cu4 Cu2 145.1(3) 2_556 2_556 ? Cu4 Cu4 Cu1 114.9(4) 2_556 2_556 ? Br4 Cu4 Cu1 142.6(4) 2_556 2_556 ? Br3 Cu4 Cu1 57.35(14) . 2_556 ? Br1 Cu4 Cu1 51.00(14) 2_556 2_556 ? Br4 Cu4 Cu1 100.5(3) . 2_556 ? Cu3 Cu4 Cu1 92.4(2) 2_556 2_556 ? Cu2 Cu4 Cu1 53.08(14) 2_556 2_556 ? Br5 Cu5 Br6 106.5(7) . . ? Br5 Cu5 Br5 23.1(9) . 2_556 ? Br6 Cu5 Br5 126.8(7) . 2_556 ? Br5 Cu5 Br1 121.4(7) . . ? Br6 Cu5 Br1 115.1(5) . . ? Br5 Cu5 Br1 99.5(6) 2_556 . ? Br5 Br5 Cu5 91(2) 2_556 . ? Br5 Br5 Cu5 65.9(19) 2_556 2_556 ? Cu5 Br5 Cu5 91.1(9) . 2_556 ? Cu3 Br6 Cu5 62.9(4) . . ? N1 C1 C3 123.0(11) . . ? N1 C1 H1 118.5 . . ? C3 C1 H1 118.5 . . ? N1 C2 C5 124.1(9) . . ? N1 C2 H2 118.0 . . ? C5 C2 H2 118.0 . . ? C4 C3 C1 119.2(11) . . ? C4 C3 H3 120.4 . . ? C1 C3 H3 120.4 . . ? C3 C4 C5 119.2(10) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C2 117.8(9) . . ? C4 C5 C6 121.8(9) . . ? C2 C5 C6 120.4(8) . . ? O1 C6 O2 124.5(10) . . ? O1 C6 C5 119.2(9) . . ? O2 C6 C5 116.3(9) . . ? O4 C7 O3 124.9(9) . . ? O4 C7 C8 118.5(8) . . ? O3 C7 C8 116.6(9) . . ? C12 C8 C9 116.9(9) . . ? C12 C8 C7 123.2(9) . . ? C9 C8 C7 119.8(9) . . ? C10 C9 C8 118.7(11) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C11 C10 C9 118.4(13) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? N2 C11 C10 124.3(13) . . ? N2 C11 H11 117.9 . . ? C10 C11 H11 117.9 . . ? N2 C12 C8 125.3(9) . . ? N2 C12 H12 117.3 . . ? C8 C12 H12 117.3 . . ? O5 C13 O6 122.2(10) . . ? O5 C13 C14 118.9(10) . . ? O6 C13 C14 118.8(10) . . ? C15 C14 C18 117.5(12) . . ? C15 C14 C13 122.0(11) . . ? C18 C14 C13 120.5(11) . . ? C14 C15 C16 121.7(14) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C17 C16 C15 113.3(15) . . ? C17 C16 H16 123.4 . . ? C15 C16 H16 123.4 . . ? N3 C17 C16 128.6(16) . . ? N3 C17 H17 115.7 . . ? C16 C17 H17 115.7 . . ? N3 C18 C14 121.7(12) . . ? N3 C18 H18 119.2 . . ? C14 C18 H18 119.2 . . ? O2 Er1 O2 103.7(5) 4_665 3_667 ? O2 Er1 O3 137.3(3) 4_665 . ? O2 Er1 O3 86.6(3) 3_667 . ? O2 Er1 O3 86.6(3) 4_665 2_656 ? O2 Er1 O3 137.3(3) 3_667 2_656 ? O3 Er1 O3 113.7(4) . 2_656 ? O2 Er1 O1W 75.7(3) 4_665 . ? O2 Er1 O1W 147.4(3) 3_667 . ? O3 Er1 O1W 74.2(3) . . ? O3 Er1 O1W 75.2(3) 2_656 . ? O2 Er1 O1W 147.4(3) 4_665 2_656 ? O2 Er1 O1W 75.7(3) 3_667 2_656 ? O3 Er1 O1W 75.2(3) . 2_656 ? O3 Er1 O1W 74.2(3) 2_656 2_656 ? O1W Er1 O1W 122.3(4) . 2_656 ? O2 Er1 O2W 71.6(3) 4_665 . ? O2 Er1 O2W 73.7(3) 3_667 . ? O3 Er1 O2W 72.0(3) . . ? O3 Er1 O2W 146.9(3) 2_656 . ? O1W Er1 O2W 75.4(3) . . ? O1W Er1 O2W 135.8(3) 2_656 . ? O2 Er1 O2W 73.7(3) 4_665 2_656 ? O2 Er1 O2W 71.6(3) 3_667 2_656 ? O3 Er1 O2W 146.9(3) . 2_656 ? O3 Er1 O2W 72.0(3) 2_656 2_656 ? O1W Er1 O2W 135.8(3) . 2_656 ? O1W Er1 O2W 75.4(3) 2_656 2_656 ? O2W Er1 O2W 122.2(3) . 2_656 ? O1 Er2 O1 105.4(4) 3_677 4_675 ? O1 Er2 O4 84.4(3) 3_677 . ? O1 Er2 O4 156.9(3) 4_675 . ? O1 Er2 O4 156.9(3) 3_677 2_656 ? O1 Er2 O4 84.4(3) 4_675 2_656 ? O4 Er2 O4 94.5(4) . 2_656 ? O1 Er2 O6 125.5(3) 3_677 . ? O1 Er2 O6 83.2(3) 4_675 . ? O4 Er2 O6 74.3(3) . . ? O4 Er2 O6 75.7(2) 2_656 . ? O1 Er2 O6 83.2(3) 3_677 2_656 ? O1 Er2 O6 125.5(3) 4_675 2_656 ? O4 Er2 O6 75.7(2) . 2_656 ? O4 Er2 O6 74.3(3) 2_656 2_656 ? O6 Er2 O6 135.2(3) . 2_656 ? O1 Er2 O5 78.4(3) 3_677 2_656 ? O1 Er2 O5 74.9(3) 4_675 2_656 ? O4 Er2 O5 128.0(3) . 2_656 ? O4 Er2 O5 84.3(2) 2_656 2_656 ? O6 Er2 O5 151.6(2) . 2_656 ? O6 Er2 O5 53.8(2) 2_656 2_656 ? O1 Er2 O5 74.9(3) 3_677 . ? O1 Er2 O5 78.4(3) 4_675 . ? O4 Er2 O5 84.3(2) . . ? O4 Er2 O5 128.0(3) 2_656 . ? O6 Er2 O5 53.8(2) . . ? O6 Er2 O5 151.6(2) 2_656 . ? O5 Er2 O5 135.3(3) 2_656 . ? O1 Er2 C13 81.6(3) 3_677 2_656 ? O1 Er2 C13 99.7(3) 4_675 2_656 ? O4 Er2 C13 102.4(3) . 2_656 ? O4 Er2 C13 76.2(3) 2_656 2_656 ? O6 Er2 C13 151.3(3) . 2_656 ? O6 Er2 C13 27.0(3) 2_656 2_656 ? O5 Er2 C13 26.9(3) 2_656 2_656 ? O5 Er2 C13 154.8(3) . 2_656 ? C2 N1 C1 116.5(10) . . ? C2 N1 Cu2 122.2(7) . . ? C1 N1 Cu2 119.9(8) . . ? C12 N2 C11 116.4(9) . . ? C12 N2 Cu1 124.9(7) . . ? C11 N2 Cu1 118.7(8) . . ? C17 N3 C18 117.2(13) . . ? C17 N3 Cu3 122.3(11) . . ? C18 N3 Cu3 120.3(9) . . ? C6 O1 Er2 152.4(8) . 3_677 ? C6 O2 Er1 150.6(8) . 3_667 ? C7 O3 Er1 139.7(7) . . ? C7 O4 Er2 143.4(7) . . ? C13 O5 Er2 91.4(6) . . ? C13 O6 Er2 92.0(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.78 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.288 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.195 data_10 _database_code_depnum_ccdc_archive 'CCDC 777380' #============================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H16 Cl3 Cu3 Gd N3 O8, H2 O' _chemical_formula_sum 'C18 H18 Cl3 Cu3 Gd N3 O9' _chemical_formula_weight 874.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc 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 9.5388(11) _cell_length_b 12.6589(14) _cell_length_c 21.400(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.5390(10) _cell_angle_gamma 90.00 _cell_volume 2555.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4592 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 25.20 _exptl_crystal_description block _exptl_crystal_colour 'green yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 5.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4437 _exptl_absorpt_correction_T_max 0.5885 _exptl_absorpt_process_details 'Apex2 (Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12989 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4592 _reflns_number_gt 3562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'Apex2 (Bruker, 2005)' _computing_data_reduction 'Apex2 (Bruker, 2005)' _computing_structure_solution 'SHELXTL 6.12 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.12' _computing_molecular_graphics 'SHELXTL 6.12' _computing_publication_material 'SHELXTL 6.12' _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^)+(0.0447P)^2^+8.9308P] 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 4592 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 C1 C 0.5068(7) 0.3191(5) 0.4799(3) 0.0209(15) Uani 1 1 d . . . C2 C 0.5558(7) 0.2110(5) 0.4614(3) 0.0218(16) Uani 1 1 d . . . C3 C 0.6985(8) 0.1884(6) 0.4672(4) 0.0292(18) Uani 1 1 d . . . H3 H 0.7660 0.2393 0.4815 0.035 Uiso 1 1 calc R . . C4 C 0.7387(8) 0.0883(7) 0.4514(4) 0.040(2) Uani 1 1 d . . . H4 H 0.8340 0.0699 0.4565 0.048 Uiso 1 1 calc R . . C5 C 0.6367(8) 0.0165(6) 0.4282(4) 0.036(2) Uani 1 1 d . . . H5 H 0.6646 -0.0511 0.4181 0.044 Uiso 1 1 calc R . . C6 C 0.4600(8) 0.1363(6) 0.4369(4) 0.0291(18) Uani 1 1 d . . . H6 H 0.3641 0.1530 0.4323 0.035 Uiso 1 1 calc R . . C7 C -0.0186(8) -0.3301(6) 0.4317(3) 0.0249(17) Uani 1 1 d . . . C8 C 0.0037(7) -0.2348(5) 0.3933(3) 0.0238(16) Uani 1 1 d . . . C9 C 0.1397(7) -0.2018(6) 0.3888(3) 0.0269(17) Uani 1 1 d . . . H9 H 0.2150 -0.2443 0.4063 0.032 Uiso 1 1 calc R . . C10 C 0.0580(9) -0.0560(6) 0.3317(4) 0.043(2) Uani 1 1 d . . . H10 H 0.0756 0.0058 0.3108 0.052 Uiso 1 1 calc R . . C11 C -0.0802(9) -0.0857(7) 0.3315(5) 0.055(3) Uani 1 1 d . . . H11 H -0.1539 -0.0464 0.3096 0.066 Uiso 1 1 calc R . . C12 C -0.1075(8) -0.1751(6) 0.3643(4) 0.039(2) Uani 1 1 d . . . H12 H -0.2004 -0.1948 0.3668 0.047 Uiso 1 1 calc R . . C13 C 0.0577(8) 0.6212(6) 0.6007(3) 0.0267(17) Uani 1 1 d . . . C14 C 0.1003(8) 0.6972(5) 0.6553(3) 0.0252(17) Uani 1 1 d . . . C15 C 0.2410(8) 0.7263(6) 0.6720(3) 0.0287(18) Uani 1 1 d . . . H15 H 0.3080 0.6971 0.6496 0.034 Uiso 1 1 calc R . . C16 C 0.1876(10) 0.8326(6) 0.7515(4) 0.038(2) Uani 1 1 d . . . H16 H 0.2173 0.8777 0.7852 0.046 Uiso 1 1 calc R . . C17 C 0.0477(10) 0.8087(7) 0.7378(4) 0.042(2) Uani 1 1 d . . . H17 H -0.0167 0.8383 0.7613 0.050 Uiso 1 1 calc R . . C18 C 0.0011(8) 0.7407(6) 0.6891(4) 0.0307(18) Uani 1 1 d . . . H18 H -0.0946 0.7243 0.6790 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.5020(2) -0.21581(16) 0.35559(10) 0.0391(5) Uani 1 1 d . . . Cl2 Cl 0.3584(3) 0.03705(17) 0.24936(11) 0.0466(6) Uani 1 1 d . . . Cl3 Cl 0.6236(3) -0.1805(2) 0.19970(12) 0.0587(7) Uani 1 1 d . . . Cu1 Cu 0.36048(11) -0.05740(8) 0.37542(5) 0.0405(3) Uani 1 1 d . . . Cu2 Cu 0.49387(14) -0.10681(11) 0.26760(6) 0.0635(4) Uani 1 1 d . . . Cu3 Cu 0.48901(13) 0.83008(11) 0.73656(6) 0.0596(4) Uani 1 1 d . . . Gd1 Gd 0.23187(3) 0.47896(3) 0.495681(16) 0.01960(12) Uani 1 1 d . . . N1 N 0.4975(7) 0.0403(5) 0.4193(3) 0.0305(15) Uani 1 1 d . . . N2 N 0.1690(7) -0.1110(5) 0.3603(3) 0.0321(15) Uani 1 1 d . . . N3 N 0.2849(7) 0.7936(5) 0.7182(3) 0.0326(16) Uani 1 1 d . . . O1 O 0.3759(5) 0.3302(4) 0.4794(2) 0.0280(12) Uani 1 1 d . . . O2 O 0.5974(5) 0.3885(4) 0.4944(3) 0.0330(13) Uani 1 1 d . . . O3 O 0.0850(6) -0.3871(4) 0.4496(3) 0.0348(13) Uani 1 1 d . . . O4 O -0.1422(5) -0.3437(4) 0.4437(3) 0.0355(13) Uani 1 1 d . . . O5 O 0.1562(5) 0.5735(4) 0.5809(2) 0.0343(13) Uani 1 1 d . . . O6 O -0.0710(5) 0.6145(4) 0.5802(3) 0.0351(13) Uani 1 1 d . . . O1W O 0.3979(5) 0.4434(4) 0.5988(2) 0.0268(12) Uani 1 1 d . . . O2W O 0.3110(6) 0.5044(4) 0.3910(2) 0.0365(14) Uani 1 1 d . . . O3W O 0.1078(13) 0.1473(10) 0.4655(7) 0.162(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(4) 0.021(4) 0.021(4) 0.002(3) 0.000(3) -0.004(3) C2 0.019(4) 0.019(4) 0.028(4) 0.003(3) 0.004(3) -0.004(3) C3 0.021(4) 0.029(4) 0.037(4) -0.005(3) 0.001(3) 0.001(3) C4 0.020(4) 0.044(5) 0.055(6) -0.015(4) 0.003(4) 0.011(4) C5 0.021(4) 0.030(4) 0.058(5) -0.016(4) 0.004(4) 0.005(4) C6 0.016(4) 0.028(4) 0.044(5) -0.003(3) 0.006(3) 0.001(3) C7 0.026(4) 0.025(4) 0.022(4) 0.003(3) -0.003(3) 0.000(3) C8 0.018(4) 0.023(4) 0.031(4) 0.001(3) 0.004(3) -0.001(3) C9 0.014(4) 0.026(4) 0.039(5) 0.001(3) 0.000(3) 0.000(3) C10 0.034(5) 0.024(4) 0.072(6) 0.019(4) 0.012(5) 0.000(4) C11 0.029(5) 0.045(6) 0.091(8) 0.041(5) 0.009(5) 0.017(4) C12 0.021(4) 0.036(5) 0.062(6) 0.015(4) 0.008(4) 0.004(4) C13 0.022(4) 0.027(4) 0.030(4) -0.003(3) 0.004(3) 0.001(3) C14 0.024(4) 0.018(4) 0.033(4) 0.000(3) 0.002(3) 0.001(3) C15 0.019(4) 0.033(4) 0.033(4) 0.001(3) -0.002(3) -0.005(3) C16 0.051(6) 0.032(5) 0.030(5) -0.008(4) -0.002(4) -0.002(4) C17 0.056(6) 0.033(5) 0.036(5) -0.003(4) 0.008(4) 0.010(4) C18 0.021(4) 0.029(4) 0.041(5) 0.001(4) 0.004(4) 0.001(3) Cl1 0.0345(11) 0.0310(11) 0.0502(13) -0.0013(9) 0.0004(10) 0.0056(9) Cl2 0.0475(14) 0.0439(13) 0.0474(13) -0.0001(10) 0.0040(11) -0.0134(11) Cl3 0.0518(15) 0.0592(16) 0.0706(17) 0.0156(13) 0.0271(13) 0.0054(13) Cu1 0.0282(6) 0.0315(6) 0.0619(7) -0.0090(5) 0.0065(5) -0.0131(5) Cu2 0.0444(7) 0.0729(9) 0.0714(9) -0.0159(7) 0.0026(7) -0.0072(7) Cu3 0.0413(7) 0.0665(9) 0.0666(9) -0.0156(7) -0.0068(6) -0.0195(6) Gd1 0.01185(18) 0.01871(19) 0.0281(2) -0.00090(15) 0.00241(14) -0.00064(14) N1 0.026(4) 0.025(4) 0.041(4) -0.006(3) 0.008(3) -0.006(3) N2 0.023(3) 0.027(4) 0.046(4) 0.003(3) 0.005(3) -0.006(3) N3 0.030(4) 0.029(4) 0.035(4) -0.001(3) -0.007(3) -0.009(3) O1 0.016(3) 0.023(3) 0.045(3) -0.005(2) 0.003(2) 0.004(2) O2 0.023(3) 0.022(3) 0.053(4) -0.008(2) 0.004(3) -0.010(2) O3 0.025(3) 0.029(3) 0.049(3) 0.012(3) 0.001(3) 0.011(3) O4 0.023(3) 0.035(3) 0.051(4) 0.012(3) 0.011(3) -0.003(2) O5 0.025(3) 0.039(3) 0.040(3) -0.014(3) 0.006(3) 0.004(3) O6 0.016(3) 0.042(3) 0.045(3) -0.010(3) -0.002(3) -0.003(2) O1W 0.017(3) 0.033(3) 0.029(3) 0.000(2) -0.001(2) 0.004(2) O2W 0.028(3) 0.050(4) 0.032(3) 0.001(3) 0.007(3) -0.006(3) O3W 0.113(9) 0.139(11) 0.237(14) -0.006(10) 0.038(10) 0.017(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 C1 O2 1.239(8) . ? C1 O1 1.255(8) . ? C1 C2 1.518(10) . ? C2 C6 1.364(10) . ? C2 C3 1.378(10) . ? C3 C4 1.380(11) . ? C3 H3 0.9300 . ? C4 C5 1.370(11) . ? C4 H4 0.9300 . ? C5 N1 1.347(10) . ? C5 H5 0.9300 . ? C6 N1 1.337(9) . ? C6 H6 0.9300 . ? C7 O3 1.238(8) . ? C7 O4 1.256(9) . ? C7 C8 1.491(10) . ? C8 C12 1.374(10) . ? C8 C9 1.380(9) . ? C9 N2 1.350(9) . ? C9 H9 0.9300 . ? C10 N2 1.337(10) . ? C10 C11 1.370(12) . ? C10 H10 0.9300 . ? C11 C12 1.377(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 O5 1.243(9) . ? C13 O6 1.244(9) . ? C13 C14 1.520(10) . ? C14 C15 1.387(10) . ? C14 C18 1.388(10) . ? C15 N3 1.325(9) . ? C15 H15 0.9300 . ? C16 N3 1.346(10) . ? C16 C17 1.357(12) . ? C16 H16 0.9300 . ? C17 C18 1.373(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? Cl1 Cu2 2.327(3) . ? Cl1 Cu1 2.489(2) . ? Cl2 Cu3 2.216(2) 3_666 ? Cl2 Cu2 2.234(3) . ? Cl3 Cu2 2.246(3) . ? Cl3 Cu3 2.481(3) 4_565 ? Cu1 N2 1.930(6) . ? Cu1 N1 1.938(6) . ? Cu2 Cu3 2.902(2) 4_565 ? Cu3 N3 1.983(7) . ? Cu3 Cl2 2.216(2) 3_666 ? Cu3 Cl3 2.481(3) 4_566 ? Cu3 Cu2 2.902(2) 4_566 ? Gd1 O3 2.324(5) 1_565 ? Gd1 O2 2.325(5) 3_666 ? Gd1 O6 2.378(5) 3_566 ? Gd1 O4 2.382(5) 3_556 ? Gd1 O5 2.381(5) . ? Gd1 O1 2.387(5) . ? Gd1 O2W 2.488(5) . ? Gd1 O1W 2.557(5) . ? O2 Gd1 2.325(5) 3_666 ? O3 Gd1 2.324(5) 1_545 ? O4 Gd1 2.382(5) 3_556 ? O6 Gd1 2.378(5) 3_566 ? 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 C1 O1 125.4(7) . . ? O2 C1 C2 118.3(6) . . ? O1 C1 C2 116.3(6) . . ? C6 C2 C3 119.2(7) . . ? C6 C2 C1 120.7(6) . . ? C3 C2 C1 120.1(6) . . ? C2 C3 C4 118.3(7) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 119.4(7) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 122.3(7) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N1 C6 C2 123.1(7) . . ? N1 C6 H6 118.5 . . ? C2 C6 H6 118.5 . . ? O3 C7 O4 126.0(7) . . ? O3 C7 C8 118.0(7) . . ? O4 C7 C8 116.0(6) . . ? C12 C8 C9 118.2(7) . . ? C12 C8 C7 122.0(7) . . ? C9 C8 C7 119.7(7) . . ? N2 C9 C8 123.4(7) . . ? N2 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? N2 C10 C11 123.7(7) . . ? N2 C10 H10 118.1 . . ? C11 C10 H10 118.1 . . ? C10 C11 C12 118.6(8) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C11 C12 C8 119.4(8) . . ? C11 C12 H12 120.3 . . ? C8 C12 H12 120.3 . . ? O5 C13 O6 127.1(7) . . ? O5 C13 C14 116.1(6) . . ? O6 C13 C14 116.8(7) . . ? C15 C14 C18 117.9(7) . . ? C15 C14 C13 120.3(7) . . ? C18 C14 C13 121.8(7) . . ? N3 C15 C14 123.3(8) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? N3 C16 C17 122.4(8) . . ? N3 C16 H16 118.8 . . ? C17 C16 H16 118.8 . . ? C16 C17 C18 120.1(8) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C14 118.4(8) . . ? C17 C18 H18 120.8 . . ? C14 C18 H18 120.8 . . ? Cu2 Cl1 Cu1 72.92(7) . . ? Cu3 Cl2 Cu2 104.11(11) 3_666 . ? Cu2 Cl3 Cu3 75.56(9) . 4_565 ? N2 Cu1 N1 149.2(3) . . ? N2 Cu1 Cl1 102.2(2) . . ? N1 Cu1 Cl1 104.7(2) . . ? Cl2 Cu2 Cl3 125.84(11) . . ? Cl2 Cu2 Cl1 125.01(10) . . ? Cl3 Cu2 Cl1 108.78(10) . . ? Cl2 Cu2 Cu3 139.89(8) . 4_565 ? Cl3 Cu2 Cu3 55.89(8) . 4_565 ? Cl1 Cu2 Cu3 66.74(7) . 4_565 ? N3 Cu3 Cl2 144.1(2) . 3_666 ? N3 Cu3 Cl3 107.4(2) . 4_566 ? Cl2 Cu3 Cl3 105.19(10) 3_666 4_566 ? N3 Cu3 Cu2 78.47(19) . 4_566 ? Cl2 Cu3 Cu2 136.08(9) 3_666 4_566 ? Cl3 Cu3 Cu2 48.56(7) 4_566 4_566 ? O3 Gd1 O2 83.23(19) 1_565 3_666 ? O3 Gd1 O6 77.64(19) 1_565 3_566 ? O2 Gd1 O6 142.52(19) 3_666 3_566 ? O3 Gd1 O4 120.87(18) 1_565 3_556 ? O2 Gd1 O4 140.53(19) 3_666 3_556 ? O6 Gd1 O4 76.51(19) 3_566 3_556 ? O3 Gd1 O5 74.12(19) 1_565 . ? O2 Gd1 O5 81.67(19) 3_666 . ? O6 Gd1 O5 122.36(18) 3_566 . ? O4 Gd1 O5 76.71(19) 3_556 . ? O3 Gd1 O1 146.87(18) 1_565 . ? O2 Gd1 O1 99.90(18) 3_666 . ? O6 Gd1 O1 80.49(17) 3_566 . ? O4 Gd1 O1 76.91(18) 3_556 . ? O5 Gd1 O1 139.01(18) . . ? O3 Gd1 O2W 76.57(19) 1_565 . ? O2 Gd1 O2W 71.77(18) 3_666 . ? O6 Gd1 O2W 72.58(18) 3_566 . ? O4 Gd1 O2W 139.85(19) 3_556 . ? O5 Gd1 O2W 142.31(19) . . ? O1 Gd1 O2W 73.29(18) . . ? O3 Gd1 O1W 138.72(18) 1_565 . ? O2 Gd1 O1W 73.29(18) 3_666 . ? O6 Gd1 O1W 139.11(17) 3_566 . ? O4 Gd1 O1W 68.31(17) 3_556 . ? O5 Gd1 O1W 69.32(17) . . ? O1 Gd1 O1W 72.01(16) . . ? O2W Gd1 O1W 124.59(17) . . ? C6 N1 C5 117.6(7) . . ? C6 N1 Cu1 121.8(5) . . ? C5 N1 Cu1 120.3(5) . . ? C10 N2 C9 116.5(7) . . ? C10 N2 Cu1 124.0(5) . . ? C9 N2 Cu1 118.6(5) . . ? C15 N3 C16 117.8(7) . . ? C15 N3 Cu3 119.3(6) . . ? C16 N3 Cu3 122.9(5) . . ? C1 O1 Gd1 132.9(5) . . ? C1 O2 Gd1 170.9(5) . 3_666 ? C7 O3 Gd1 163.8(5) . 1_545 ? C7 O4 Gd1 129.4(5) . 3_556 ? C13 O5 Gd1 146.7(5) . . ? C13 O6 Gd1 141.1(5) . 3_566 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.662 _refine_diff_density_min -1.414 _refine_diff_density_rms 0.177