# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 901272' #TrackingRef '1-2-3.cif' _vrf_PLAT_420 ; PROBLEM: D-H without acceptor (O3W-H3WA and O4W-H4WA) RESPONSE: A weak hydrogen bond (according to G. R. Desiraju and T. Steiner,The Weak Hydrogen Bond, Oxford University Press, 2001) involving the hydrogen atom H4WA and the symmetry related oxygen atom O23' ( ' = x, -y+0.5, z+0.5) is present (the H4WA...O23' distance is 2.79(1)A) ; _vrf_PLAT_910 ; PROBLEM: Missing # of FCF Reflections Below Th(Min) ..... 45 RESPONSE: Data were collected with a CCD detector. The reflections in question were affected by the beam-stop. Only a small number of reflections are missing out of the total number of reflections observed. Resolution and completeness statistics #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.991 5212 5167 45 23.01 0.550 0.993 6927 6879 48 25.24 0.600 0.994 9002 8952 50 #----------------------------------------------------------- ACTA Min. Res. --- ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H48 Cl3 Cu2 Gd N4 O30' _chemical_formula_weight 1359.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6924(4) _cell_length_b 23.6542(8) _cell_length_c 16.2397(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.983(4) _cell_angle_gamma 90.00 _cell_volume 4973.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 7172 _cell_measurement_theta_min 4.2579 _cell_measurement_theta_max 29.2950 _exptl_crystal_description parallelepipedal _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2724 _exptl_absorpt_coefficient_mu 2.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.57013 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.4547 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23075 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.1121 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 29.35 _reflns_number_total 11286 _reflns_number_gt 5949 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_structure_solution 'SIR2004 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farruggia, 1997)' _computing_publication_material 'PARST97 (Nardelli, 1995)' _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^ > 2\s(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. 22 restrains were used in the refinement. In particular four of them are related to the position of the methyl carbon in one of the two models proposed for the disordered ligand; the others are related to the O-H and H...H distances in the five water molecules. ; _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^)+(0.0831P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11286 _refine_ls_number_parameters 640 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1562 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.04876(2) 0.121777(16) 0.83271(2) 0.03877(13) Uani 1 1 d . A . O2W O 0.0050(4) 0.1288(3) 0.9637(4) 0.0610(16) Uani 1 1 d D A . H2WA H -0.044(5) 0.150(3) 0.958(5) 0.073 Uiso 1 1 d D . . H2WB H 0.011(6) 0.108(3) 1.007(4) 0.073 Uiso 1 1 d D . . Cu1A Cu 0.30844(6) 0.16695(4) 0.91259(6) 0.0462(3) Uani 1 1 d . . . O1WA O 0.3513(5) 0.0984(3) 0.8282(4) 0.0736(19) Uani 1 1 d D A . H1WB H 0.292(2) 0.091(5) 0.800(5) 0.088 Uiso 1 1 d D . . H1WA H 0.390(5) 0.093(4) 0.800(5) 0.088 Uiso 1 1 d D . . O1A O 0.2176(3) 0.1137(2) 0.9437(4) 0.0480(13) Uani 1 1 d . A . O2A O 0.0877(4) 0.0295(2) 0.9176(4) 0.0540(14) Uani 1 1 d . A . O3A O 0.3869(5) 0.0016(3) 1.0556(5) 0.082(2) Uani 1 1 d . A . O4A O 0.1774(3) 0.1901(2) 0.8361(3) 0.0479(13) Uani 1 1 d . A . O5A O 0.0266(4) 0.1693(3) 0.6897(3) 0.0522(14) Uani 1 1 d . A . O6A O 0.2287(4) 0.2971(3) 0.6989(4) 0.0667(17) Uani 1 1 d . . . N1A N 0.4217(4) 0.1519(3) 1.0247(4) 0.0518(18) Uani 1 1 d . A . N2A N 0.3921(5) 0.2307(3) 0.8861(4) 0.0525(18) Uani 1 1 d . A . C1A C 0.3155(9) -0.0405(5) 1.0423(8) 0.091(4) Uani 1 1 d . . . H1A H 0.3381 -0.0764 1.0630 0.109 Uiso 1 1 calc R . . C2A C 0.2166(8) -0.0330(4) 1.0019(7) 0.077(3) Uani 1 1 d . A . H2A H 0.1707 -0.0627 0.9983 0.092 Uiso 1 1 calc R . . C3A C 0.1794(7) 0.0196(4) 0.9639(6) 0.054(2) Uani 1 1 d . . . C4A C 0.2571(6) 0.0651(4) 0.9803(5) 0.054(2) Uani 1 1 d . A . C5A C 0.3541(6) 0.0540(4) 1.0214(6) 0.059(2) Uani 1 1 d . . . C6A C 0.4480(6) 0.0920(4) 1.0349(6) 0.067(3) Uani 1 1 d . A . H6A1 H 0.4963 0.0857 1.0929 0.080 Uiso 1 1 calc R . . H6A2 H 0.4822 0.0815 0.9934 0.080 Uiso 1 1 calc R . . C7A C 0.5089(6) 0.1879(5) 1.0207(6) 0.072(3) Uani 1 1 d . . . H7A1 H 0.5486 0.1679 0.9901 0.086 Uiso 1 1 calc R A . H7A2 H 0.5542 0.1957 1.0793 0.086 Uiso 1 1 calc R . . C8A C 0.4703(6) 0.2421(4) 0.9750(6) 0.064(3) Uani 1 1 d . A . H8A1 H 0.5277 0.2636 0.9685 0.076 Uiso 1 1 calc R . . H8A2 H 0.4384 0.2645 1.0095 0.076 Uiso 1 1 calc R . . C9A C 0.3246(6) 0.2806(4) 0.8518(6) 0.067(3) Uani 1 1 d . . . H9A1 H 0.3654 0.3110 0.8395 0.081 Uiso 1 1 calc R A . H9A2 H 0.2954 0.2938 0.8953 0.081 Uiso 1 1 calc R . . C10A C 0.2377(6) 0.2647(4) 0.7687(6) 0.059(2) Uani 1 1 d . A . C11A C 0.1534(7) 0.2853(4) 0.6249(7) 0.073(3) Uani 1 1 d . . . H11A H 0.1488 0.3069 0.5760 0.087 Uiso 1 1 calc R . . C12A C 0.0828(6) 0.2434(4) 0.6171(6) 0.065(3) Uani 1 1 d . A . H12A H 0.0315 0.2372 0.5640 0.078 Uiso 1 1 calc R . . C13A C 0.0875(5) 0.2099(3) 0.6887(5) 0.0436(18) Uani 1 1 d . . . C14A C 0.1699(6) 0.2221(4) 0.7655(6) 0.049(2) Uani 1 1 d . A . C15A C 0.3886(7) 0.1702(5) 1.0995(6) 0.074(3) Uani 1 1 d . . . H15A H 0.3704 0.2096 1.0933 0.110 Uiso 1 1 calc R A . H15B H 0.4442 0.1645 1.1529 0.110 Uiso 1 1 calc R . . H15C H 0.3299 0.1484 1.1003 0.110 Uiso 1 1 calc R . . C16A C 0.4485(6) 0.2161(4) 0.8252(6) 0.067(3) Uani 1 1 d . . . H16A H 0.4915 0.1837 0.8467 0.101 Uiso 1 1 calc R A . H16B H 0.4908 0.2474 0.8203 0.101 Uiso 1 1 calc R . . H16C H 0.3999 0.2076 0.7689 0.101 Uiso 1 1 calc R . . Cu1B Cu -0.18881(6) 0.07536(4) 0.68481(6) 0.0457(3) Uani 1 1 d . . . O1WB O -0.1518(5) 0.1281(3) 0.5732(5) 0.076(2) Uani 1 1 d D A . H1WC H -0.0878(18) 0.126(3) 0.589(7) 0.091 Uiso 1 1 d D . . H1WD H -0.168(6) 0.1606(18) 0.556(7) 0.091 Uiso 1 1 d D . . O1B O -0.1338(10) 0.1330(6) 0.7687(9) 0.034(4) Uiso 0.50 1 d P A 1 O2B O -0.0255(10) 0.2205(6) 0.8348(9) 0.035(4) Uiso 0.50 1 d P A 1 O3B O -0.3284(8) 0.2417(5) 0.7167(8) 0.051(3) Uiso 0.50 1 d P A 1 O4B O -0.0465(11) 0.0557(6) 0.7226(10) 0.039(4) Uiso 0.50 1 d P A 1 O5B O 0.1512(14) 0.0639(8) 0.7593(12) 0.060(6) Uiso 0.50 1 d P A 1 O6B O -0.0175(8) -0.0467(5) 0.5707(8) 0.047(3) Uiso 0.50 1 d P A 1 N1B N -0.3334(15) 0.0921(9) 0.6703(14) 0.056(7) Uiso 0.50 1 d P A 1 N2B N -0.2413(12) 0.0004(7) 0.6310(11) 0.046(5) Uiso 0.50 1 d P A 1 C1B C -0.2715(14) 0.2856(8) 0.7626(12) 0.045(5) Uiso 0.50 1 d P A 1 H1B H -0.2996 0.3217 0.7584 0.054 Uiso 0.50 1 calc PR A 1 C2B C -0.188(2) 0.2770(12) 0.8066(17) 0.056(8) Uiso 0.50 1 d P A 1 H2B H -0.1563 0.3051 0.8465 0.067 Uiso 0.50 1 calc PR A 1 C3B C -0.127(2) 0.2271(12) 0.8060(17) 0.032(7) Uiso 0.50 1 d P A 1 C4B C -0.181(2) 0.1880(12) 0.7726(19) 0.061(10) Uiso 0.50 1 d P A 1 C5B C -0.2845(12) 0.1935(8) 0.7161(12) 0.044(4) Uiso 0.50 1 d P A 1 C6B C -0.3590(13) 0.1499(7) 0.6506(11) 0.059(4) Uiso 0.50 1 d PD A 1 H6B1 H -0.4290 0.1562 0.6505 0.071 Uiso 0.50 1 calc PR A 1 H6B2 H -0.3577 0.1576 0.5923 0.071 Uiso 0.50 1 calc PR A 1 C7B C -0.3894(13) 0.0557(8) 0.5995(10) 0.056(5) Uiso 0.50 1 d PD A 1 H7B1 H -0.4591 0.0514 0.6015 0.067 Uiso 0.50 1 calc PR A 1 H7B2 H -0.3947 0.0747 0.5453 0.067 Uiso 0.50 1 calc PR A 1 C8B C -0.3507(17) 0.0046(10) 0.5973(16) 0.054(7) Uiso 0.50 1 d P A 1 H8B1 H -0.3731 -0.0083 0.5373 0.065 Uiso 0.50 1 calc PR A 1 H8B2 H -0.3797 -0.0210 0.6298 0.065 Uiso 0.50 1 calc PR A 1 C9B C -0.1776(10) -0.0150(7) 0.5724(10) 0.041(3) Uiso 0.50 1 d P A 1 H9B1 H -0.1955 -0.0532 0.5513 0.049 Uiso 0.50 1 calc PR A 1 H9B2 H -0.1981 0.0099 0.5222 0.049 Uiso 0.50 1 calc PR A 1 C10B C -0.0659(12) -0.0118(8) 0.6117(12) 0.046(4) Uiso 0.50 1 d P A 1 C11B C 0.0808(15) -0.0492(9) 0.5952(14) 0.056(6) Uiso 0.50 1 d P A 1 H11B H 0.1114 -0.0758 0.5691 0.067 Uiso 0.50 1 calc PR A 1 C12B C 0.1454(17) -0.0138(10) 0.6597(15) 0.048(6) Uiso 0.50 1 d P A 1 H12B H 0.2163 -0.0115 0.6702 0.058 Uiso 0.50 1 calc PR A 1 C13B C 0.097(2) 0.0170(12) 0.7059(18) 0.057(10) Uiso 0.50 1 d P A 1 C14B C -0.0102(15) 0.0208(9) 0.6805(14) 0.042(6) Uiso 0.50 1 d P A 1 C15B C -0.3494(14) 0.0761(8) 0.7549(9) 0.076(6) Uiso 0.50 1 d PD A 1 H15D H -0.3317 0.0370 0.7674 0.114 Uiso 0.50 1 calc PR A 1 H15E H -0.4205 0.0818 0.7500 0.114 Uiso 0.50 1 calc PR A 1 H15F H -0.3062 0.0992 0.8010 0.114 Uiso 0.50 1 calc PR A 1 C16B C -0.2230(12) -0.0437(7) 0.6950(11) 0.055(4) Uiso 0.50 1 d P A 1 H16D H -0.1500 -0.0491 0.7216 0.082 Uiso 0.50 1 calc PR A 1 H16E H -0.2540 -0.0782 0.6675 0.082 Uiso 0.50 1 calc PR A 1 H16F H -0.2529 -0.0333 0.7388 0.082 Uiso 0.50 1 calc PR A 1 N1C N -0.3398(13) 0.1009(8) 0.6511(13) 0.041(5) Uiso 0.50 1 d P A 2 N2C N -0.2270(12) 0.0049(7) 0.6089(12) 0.048(5) Uiso 0.50 1 d P A 2 O1C O -0.1411(11) 0.1265(7) 0.7839(10) 0.045(5) Uiso 0.50 1 d P A 2 O2C O -0.0226(11) 0.2187(7) 0.8558(10) 0.044(5) Uiso 0.50 1 d P A 2 O3C O -0.3400(9) 0.2310(6) 0.7489(9) 0.058(3) Uiso 0.50 1 d P A 2 O4C O -0.0467(10) 0.0494(6) 0.7411(9) 0.035(4) Uiso 0.50 1 d P A 2 O5C O 0.1536(11) 0.0545(7) 0.7744(10) 0.033(4) Uiso 0.50 1 d P A 2 O6C O -0.0013(9) -0.0637(6) 0.6111(9) 0.065(4) Uiso 0.50 1 d P A 2 C1C C -0.2882(17) 0.2759(10) 0.7829(15) 0.067(7) Uiso 0.50 1 d P A 2 H1C H -0.3252 0.3071 0.7915 0.080 Uiso 0.50 1 calc PR A 2 C2C C -0.1638(19) 0.2816(12) 0.8113(15) 0.050(8) Uiso 0.50 1 d P A 2 H2C H -0.1290 0.3160 0.8219 0.060 Uiso 0.50 1 calc PR A 2 C3C C -0.112(2) 0.2269(16) 0.819(2) 0.055(11) Uiso 0.50 1 d P A 2 C4C C -0.1898(16) 0.1748(10) 0.7696(14) 0.032(6) Uiso 0.50 1 d P A 2 C5C C -0.2889(12) 0.1818(7) 0.7504(12) 0.044(4) Uiso 0.50 1 d P A 2 C6C C -0.3612(13) 0.1296(8) 0.7224(9) 0.059(4) Uiso 0.50 1 d PD A 2 H6C1 H -0.3498 0.1040 0.7713 0.071 Uiso 0.50 1 calc PR A 2 H6C2 H -0.4328 0.1417 0.7040 0.071 Uiso 0.50 1 calc PR A 2 C7C C -0.4024(12) 0.0470(6) 0.6327(12) 0.050(4) Uiso 0.50 1 d PD A 2 H7C1 H -0.4730 0.0544 0.5965 0.060 Uiso 0.50 1 calc PR A 2 H7C2 H -0.4031 0.0293 0.6864 0.060 Uiso 0.50 1 calc PR A 2 C8C C -0.3389(18) 0.0041(11) 0.5778(17) 0.061(8) Uiso 0.50 1 d P A 2 H8C1 H -0.3611 -0.0346 0.5805 0.073 Uiso 0.50 1 calc PR A 2 H8C2 H -0.3621 0.0151 0.5170 0.073 Uiso 0.50 1 calc PR A 2 C9C C -0.1625(15) -0.0443(10) 0.6364(16) 0.089(7) Uiso 0.50 1 d P A 2 H9C1 H -0.1838 -0.0736 0.5924 0.106 Uiso 0.50 1 calc PR A 2 H9C2 H -0.1688 -0.0589 0.6903 0.106 Uiso 0.50 1 calc PR A 2 C10C C -0.0514(14) -0.0273(9) 0.6499(14) 0.061(5) Uiso 0.50 1 d P A 2 C11C C 0.1042(18) -0.0558(11) 0.6280(17) 0.073(7) Uiso 0.50 1 d P A 2 H11C H 0.1367 -0.0779 0.5973 0.087 Uiso 0.50 1 calc PR A 2 C12C C 0.1607(18) -0.0193(11) 0.6840(16) 0.054(7) Uiso 0.50 1 d P A 2 H12C H 0.2323 -0.0215 0.7006 0.065 Uiso 0.50 1 calc PR A 2 C13C C 0.1136(17) 0.0244(11) 0.7203(16) 0.037(6) Uiso 0.50 1 d P A 2 C14C C 0.0043(16) 0.0128(9) 0.7032(14) 0.044(6) Uiso 0.50 1 d P A 2 C15C C -0.3727(12) 0.1365(6) 0.5718(9) 0.058(4) Uiso 0.50 1 d PD A 2 H15G H -0.3581 0.1172 0.5251 0.087 Uiso 0.50 1 calc PR A 2 H15H H -0.3360 0.1717 0.5832 0.087 Uiso 0.50 1 calc PR A 2 H15I H -0.4456 0.1436 0.5556 0.087 Uiso 0.50 1 calc PR A 2 C16C C -0.2223(17) 0.0147(10) 0.5165(16) 0.092(7) Uiso 0.50 1 d P A 2 H16G H -0.2636 0.0470 0.4910 0.138 Uiso 0.50 1 calc PR A 2 H16H H -0.2484 -0.0181 0.4813 0.138 Uiso 0.50 1 calc PR A 2 H16I H -0.1520 0.0213 0.5195 0.138 Uiso 0.50 1 calc PR A 2 Cl1 Cl -0.22506(16) 0.20648(12) 1.01175(17) 0.0676(7) Uani 1 1 d . . . O11 O -0.2667(7) 0.2583(5) 1.0161(10) 0.175(5) Uani 1 1 d . . . O12 O -0.2940(5) 0.1758(4) 0.9410(6) 0.103(3) Uani 1 1 d . . . O13 O -0.2236(9) 0.1764(7) 1.0854(7) 0.194(6) Uani 1 1 d . . . O14 O -0.1308(5) 0.2079(4) 1.0013(7) 0.135(4) Uani 1 1 d . . . Cl2 Cl 0.31350(18) 0.13829(11) 0.58554(16) 0.0633(6) Uani 1 1 d . . . O21 O 0.3490(6) 0.1211(4) 0.5187(6) 0.110(3) Uani 1 1 d . . . O22 O 0.3741(9) 0.1082(6) 0.6577(8) 0.180(5) Uani 1 1 d . . . O23 O 0.2159(7) 0.1228(5) 0.5749(9) 0.171(5) Uani 1 1 d . . . O24 O 0.3254(11) 0.1965(4) 0.5994(10) 0.194(6) Uani 1 1 d . . . Cl3 Cl 0.4457(2) -0.08849(17) 0.6803(2) 0.1010(10) Uiso 1 1 d . . . O31 O 0.4609(11) -0.1391(8) 0.6600(11) 0.222(6) Uiso 1 1 d . . . O32 O 0.3980(8) -0.0947(5) 0.7454(8) 0.149(4) Uiso 1 1 d . . . O33A O 0.5497(14) -0.0738(9) 0.7388(14) 0.134(6) Uiso 0.50 1 d P . . O33B O 0.3251(19) -0.0936(12) 0.6179(18) 0.184(10) Uiso 0.50 1 d P . . O34 O 0.4354(14) -0.0425(9) 0.6334(14) 0.273(8) Uiso 1 1 d . . . O3W O 0.0499(5) 0.0642(3) 1.1059(5) 0.078(2) Uani 1 1 d D . . H3WA H 0.101(4) 0.050(4) 1.140(5) 0.094 Uiso 1 1 d D . . H3WB H 0.001(4) 0.062(5) 1.124(6) 0.094 Uiso 1 1 d D . . O4W O 0.0832(7) 0.3204(4) 0.8819(7) 0.122(3) Uani 1 1 d D . . H4WA H 0.134(6) 0.340(5) 0.902(9) 0.146 Uiso 1 1 d D . . H4WB H 0.034(6) 0.333(6) 0.895(10) 0.146 Uiso 1 1 d D . . O5W O -0.0084(10) 0.1344(4) 1.2191(8) 0.129(3) Uani 1 1 d D . . H5WA H 0.036(10) 0.143(5) 1.197(11) 0.155 Uiso 1 1 d D . . H5WB H -0.019(11) 0.1002(17) 1.211(11) 0.155 Uiso 1 1 d 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 Gd1 0.03385(19) 0.0399(2) 0.0402(2) -0.00021(19) 0.00886(14) -0.00071(18) O2W 0.066(4) 0.070(5) 0.052(4) 0.006(3) 0.026(3) 0.014(3) Cu1A 0.0339(4) 0.0586(7) 0.0431(6) -0.0012(5) 0.0084(4) -0.0025(4) O1WA 0.060(4) 0.092(5) 0.071(5) -0.029(4) 0.025(3) -0.007(4) O1A 0.034(2) 0.051(4) 0.054(3) 0.007(3) 0.007(2) 0.000(2) O2A 0.057(3) 0.039(3) 0.063(4) 0.008(3) 0.016(3) 0.004(3) O3A 0.064(4) 0.092(6) 0.083(5) 0.024(4) 0.013(3) 0.029(4) O4A 0.029(2) 0.058(4) 0.051(3) 0.009(3) 0.006(2) -0.002(2) O5A 0.042(3) 0.066(4) 0.042(3) -0.003(3) 0.005(2) -0.006(3) O6A 0.052(3) 0.071(4) 0.073(4) 0.032(4) 0.015(3) 0.004(3) N1A 0.040(3) 0.071(5) 0.039(4) -0.003(4) 0.005(3) 0.010(4) N2A 0.047(4) 0.066(5) 0.045(4) -0.009(4) 0.015(3) -0.011(4) C1A 0.095(8) 0.066(8) 0.109(10) 0.038(7) 0.030(7) 0.006(7) C2A 0.075(7) 0.061(7) 0.095(8) 0.017(6) 0.026(6) 0.012(6) C3A 0.065(5) 0.045(5) 0.056(5) 0.009(4) 0.025(4) 0.007(5) C4A 0.055(5) 0.066(6) 0.039(5) 0.015(4) 0.015(4) 0.022(5) C5A 0.040(4) 0.073(7) 0.058(6) 0.021(5) 0.009(4) 0.016(5) C6A 0.057(5) 0.081(7) 0.053(6) 0.008(5) 0.004(4) 0.028(5) C7A 0.039(4) 0.125(10) 0.045(5) -0.001(6) 0.005(4) -0.006(5) C8A 0.045(5) 0.069(7) 0.069(6) -0.003(5) 0.009(4) -0.021(5) C9A 0.054(5) 0.067(7) 0.079(7) -0.003(6) 0.019(5) -0.024(5) C10A 0.041(4) 0.062(6) 0.073(6) 0.025(5) 0.018(4) 0.003(4) C11A 0.061(5) 0.078(7) 0.074(7) 0.042(6) 0.016(5) 0.009(6) C12A 0.044(4) 0.082(7) 0.063(6) 0.018(5) 0.008(4) 0.006(5) C13A 0.036(4) 0.043(5) 0.046(5) 0.007(4) 0.006(3) 0.008(4) C14A 0.041(4) 0.046(5) 0.062(6) 0.019(4) 0.019(4) 0.008(4) C15A 0.075(6) 0.102(9) 0.042(5) 0.000(5) 0.016(4) 0.011(6) C16A 0.062(5) 0.081(7) 0.066(6) 0.007(5) 0.031(5) 0.004(5) Cu1B 0.0416(5) 0.0436(6) 0.0450(6) -0.0050(5) 0.0047(4) -0.0036(4) O1WB 0.061(4) 0.098(6) 0.060(4) 0.015(4) 0.007(3) -0.005(4) Cl1 0.0507(12) 0.0858(19) 0.0697(16) -0.0104(14) 0.0242(11) 0.0073(13) O11 0.121(7) 0.120(9) 0.287(16) -0.083(10) 0.071(8) 0.014(6) O12 0.073(4) 0.117(7) 0.111(6) -0.030(6) 0.021(4) -0.015(5) O13 0.174(10) 0.32(2) 0.080(7) 0.026(10) 0.033(7) -0.047(11) O14 0.056(4) 0.182(10) 0.168(9) -0.076(8) 0.038(5) -0.010(5) Cl2 0.0679(14) 0.0614(15) 0.0573(14) -0.0104(12) 0.0160(11) -0.0082(12) O21 0.118(6) 0.125(8) 0.097(6) -0.031(6) 0.049(5) -0.013(5) O22 0.173(10) 0.262(16) 0.117(9) 0.058(9) 0.064(8) 0.088(10) O23 0.103(7) 0.221(13) 0.203(12) -0.097(10) 0.069(7) -0.055(7) O24 0.339(16) 0.051(6) 0.275(16) -0.016(8) 0.216(14) -0.027(8) O3W 0.085(4) 0.062(5) 0.079(5) 0.021(4) 0.014(4) -0.008(4) O4W 0.124(7) 0.115(8) 0.109(7) -0.010(6) 0.014(6) -0.034(6) O5W 0.188(11) 0.101(8) 0.104(7) 0.004(7) 0.054(7) 0.023(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O4C 2.364(14) . ? Gd1 O4A 2.378(5) . ? Gd1 O1B 2.390(13) . ? Gd1 O2W 2.397(5) . ? Gd1 O4B 2.414(15) . ? Gd1 O1A 2.433(5) . ? Gd1 O1C 2.461(15) . ? Gd1 O5A 2.509(5) . ? Gd1 O5B 2.521(19) . ? Gd1 O5C 2.524(15) . ? Gd1 O2A 2.544(5) . ? Gd1 O2B 2.550(15) . ? O2W H2WA 0.82(2) . ? O2W H2WB 0.84(2) . ? Cu1A O4A 1.901(5) . ? Cu1A O1A 1.949(5) . ? Cu1A N1A 2.002(6) . ? Cu1A N2A 2.023(7) . ? Cu1A O1WA 2.319(6) . ? O1WA H1WB 0.81(2) . ? O1WA H1WA 0.82(2) . ? O1A C4A 1.326(9) . ? O2A C3A 1.258(9) . ? O3A C1A 1.362(12) . ? O3A C5A 1.372(11) . ? O4A C14A 1.348(9) . ? O5A C13A 1.276(9) . ? O6A C11A 1.333(11) . ? O6A C10A 1.341(10) . ? N1A C6A 1.458(11) . ? N1A C7A 1.485(11) . ? N1A C15A 1.493(10) . ? N2A C16A 1.481(10) . ? N2A C9A 1.490(11) . ? N2A C8A 1.517(10) . ? C1A C2A 1.310(13) . ? C1A H1A 0.9300 . ? C2A C3A 1.409(12) . ? C2A H2A 0.9300 . ? C3A C4A 1.474(12) . ? C4A C5A 1.305(10) . ? C5A C6A 1.525(12) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C7A C8A 1.490(13) . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C9A C10A 1.528(12) . ? C9A H9A1 0.9700 . ? C9A H9A2 0.9700 . ? C10A C14A 1.360(11) . ? C11A C12A 1.361(12) . ? C11A H11A 0.9300 . ? C12A C13A 1.390(11) . ? C12A H12A 0.9300 . ? C13A C14A 1.412(11) . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? Cu1B O4B 1.901(14) . ? Cu1B O1B 1.901(14) . ? Cu1B O1C 1.949(16) . ? Cu1B N1B 1.96(2) . ? Cu1B O4C 1.959(14) . ? Cu1B N2B 2.004(16) . ? Cu1B N2C 2.037(17) . ? Cu1B N1C 2.049(18) . ? Cu1B O1WB 2.387(7) . ? O1WB H1WC 0.83(2) . ? O1WB H1WD 0.82(2) . ? O1B C4B 1.46(3) . ? O2B C3B 1.32(3) . ? O3B C5B 1.290(19) . ? O3B C1B 1.37(2) . ? O4B C14B 1.27(2) . ? O5B C13B 1.46(3) . ? O6B C11B 1.28(2) . ? O6B C10B 1.361(19) . ? N1B C6B 1.42(3) . ? N1B C7B 1.44(3) . ? N1B C15B 1.51(2) . ? N2B C8B 1.42(3) . ? N2B C16B 1.44(2) . ? N2B C9B 1.53(2) . ? C1B C2B 1.15(3) . ? C1B H1B 0.9300 . ? C2B C3B 1.45(4) . ? C2B H2B 0.9300 . ? C3B C4B 1.20(3) . ? C4B C5B 1.43(3) . ? C5B C6B 1.59(2) . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? C7B C8B 1.33(3) . ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C9B C10B 1.46(2) . ? C9B H9B1 0.9700 . ? C9B H9B2 0.9700 . ? C10B C14B 1.37(3) . ? C11B C12B 1.41(3) . ? C11B H11B 0.9300 . ? C12B C13B 1.37(3) . ? C12B H12B 0.9300 . ? C13B C14B 1.39(3) . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? N1C C6C 1.45(2) . ? N1C C15C 1.48(2) . ? N1C C7C 1.51(2) . ? N2C C9C 1.44(3) . ? N2C C8C 1.45(3) . ? N2C C16C 1.54(3) . ? O1C C4C 1.30(3) . ? O2C C3C 1.19(3) . ? O3C C1C 1.30(2) . ? O3C C5C 1.35(2) . ? O4C C14C 1.38(3) . ? O5C C13C 1.13(3) . ? O6C C10C 1.38(2) . ? O6C C11C 1.39(2) . ? C1C C2C 1.62(3) . ? C1C H1C 0.9300 . ? C2C C3C 1.46(4) . ? C2C H2C 0.9300 . ? C3C C4C 1.65(4) . ? C4C C5C 1.30(2) . ? C5C C6C 1.56(2) . ? C6C H6C1 0.9700 . ? C6C H6C2 0.9700 . ? C7C C8C 1.76(3) . ? C7C H7C1 0.9700 . ? C7C H7C2 0.9700 . ? C8C H8C1 0.9700 . ? C8C H8C2 0.9700 . ? C9C C10C 1.52(3) . ? C9C H9C1 0.9700 . ? C9C H9C2 0.9700 . ? C10C C14C 1.34(3) . ? C11C C12C 1.31(3) . ? C11C H11C 0.9300 . ? C12C C13C 1.44(3) . ? C12C H12C 0.9300 . ? C13C C14C 1.46(3) . ? C15C H15G 0.9600 . ? C15C H15H 0.9600 . ? C15C H15I 0.9600 . ? C16C H16G 0.9600 . ? C16C H16H 0.9600 . ? C16C H16I 0.9600 . ? Cl1 O14 1.356(7) . ? Cl1 O11 1.363(10) . ? Cl1 O13 1.386(11) . ? Cl1 O12 1.425(8) . ? Cl2 O23 1.341(9) . ? Cl2 O21 1.387(8) . ? Cl2 O22 1.392(11) . ? Cl2 O24 1.397(9) . ? Cl3 O31 1.276(17) . ? Cl3 O34 1.31(2) . ? Cl3 O32 1.421(11) . ? Cl3 O33A 1.473(19) . ? Cl3 O33B 1.64(3) . ? O3W H3WA 0.81(2) . ? O3W H3WB 0.82(2) . ? O4W H4WA 0.81(2) . ? O4W H4WB 0.82(2) . ? O5W H5WA 0.82(2) . ? O5W H5WB 0.83(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4C Gd1 O4A 139.5(4) . . ? O4C Gd1 O1B 61.3(5) . . ? O4A Gd1 O1B 126.6(4) . . ? O4C Gd1 O2W 111.2(4) . . ? O4A Gd1 O2W 109.2(2) . . ? O1B Gd1 O2W 81.4(4) . . ? O4C Gd1 O4B 8.0(5) . . ? O4A Gd1 O4B 132.5(4) . . ? O1B Gd1 O4B 60.9(5) . . ? O2W Gd1 O4B 118.2(4) . . ? O4C Gd1 O1A 127.4(4) . . ? O4A Gd1 O1A 61.20(17) . . ? O1B Gd1 O1A 159.8(4) . . ? O2W Gd1 O1A 78.45(19) . . ? O4B Gd1 O1A 130.7(4) . . ? O4C Gd1 O1C 61.3(5) . . ? O4A Gd1 O1C 132.3(4) . . ? O1B Gd1 O1C 7.7(5) . . ? O2W Gd1 O1C 74.9(4) . . ? O4B Gd1 O1C 62.1(5) . . ? O1A Gd1 O1C 153.1(4) . . ? O4C Gd1 O5A 82.3(4) . . ? O4A Gd1 O5A 65.31(17) . . ? O1B Gd1 O5A 75.7(4) . . ? O2W Gd1 O5A 143.2(2) . . ? O4B Gd1 O5A 74.4(4) . . ? O1A Gd1 O5A 121.38(16) . . ? O1C Gd1 O5A 83.4(4) . . ? O4C Gd1 O5B 65.7(5) . . ? O4A Gd1 O5B 81.9(4) . . ? O1B Gd1 O5B 121.3(5) . . ? O2W Gd1 O5B 142.7(4) . . ? O4B Gd1 O5B 63.1(5) . . ? O1A Gd1 O5B 76.5(4) . . ? O1C Gd1 O5B 124.4(6) . . ? O5A Gd1 O5B 74.0(4) . . ? O4C Gd1 O5C 64.7(5) . . ? O4A Gd1 O5C 86.0(4) . . ? O1B Gd1 O5C 123.3(5) . . ? O2W Gd1 O5C 135.5(4) . . ? O4B Gd1 O5C 63.2(5) . . ? O1A Gd1 O5C 73.1(4) . . ? O1C Gd1 O5C 125.3(5) . . ? O5A Gd1 O5C 81.2(4) . . ? O5B Gd1 O5C 7.4(6) . . ? O4C Gd1 O2A 72.3(4) . . ? O4A Gd1 O2A 123.23(17) . . ? O1B Gd1 O2A 109.7(4) . . ? O2W Gd1 O2A 69.3(2) . . ? O4B Gd1 O2A 79.2(4) . . ? O1A Gd1 O2A 63.26(17) . . ? O1C Gd1 O2A 103.1(4) . . ? O5A Gd1 O2A 145.82(19) . . ? O5B Gd1 O2A 74.9(4) . . ? O5C Gd1 O2A 67.6(4) . . ? O4C Gd1 O2B 122.0(5) . . ? O4A Gd1 O2B 70.9(3) . . ? O1B Gd1 O2B 62.5(5) . . ? O2W Gd1 O2B 73.1(4) . . ? O4B Gd1 O2B 118.8(5) . . ? O1A Gd1 O2B 110.4(3) . . ? O1C Gd1 O2B 65.1(5) . . ? O5A Gd1 O2B 70.9(4) . . ? O5B Gd1 O2B 142.1(5) . . ? O5C Gd1 O2B 149.2(5) . . ? O2A Gd1 O2B 142.4(4) . . ? Gd1 O2W H2WA 112(5) . . ? Gd1 O2W H2WB 135(6) . . ? H2WA O2W H2WB 108(3) . . ? O4A Cu1A O1A 79.0(2) . . ? O4A Cu1A N1A 158.9(3) . . ? O1A Cu1A N1A 91.2(3) . . ? O4A Cu1A N2A 97.2(3) . . ? O1A Cu1A N2A 172.0(3) . . ? N1A Cu1A N2A 90.1(3) . . ? O4A Cu1A O1WA 100.5(2) . . ? O1A Cu1A O1WA 90.4(2) . . ? N1A Cu1A O1WA 98.2(3) . . ? N2A Cu1A O1WA 97.3(3) . . ? O4A Cu1A Gd1 39.06(16) . . ? O1A Cu1A Gd1 41.25(15) . . ? N1A Cu1A Gd1 132.1(2) . . ? N2A Cu1A Gd1 136.02(19) . . ? O1WA Cu1A Gd1 89.39(15) . . ? Cu1A O1WA H1WB 94(6) . . ? Cu1A O1WA H1WA 141(7) . . ? H1WB O1WA H1WA 112(4) . . ? C4A O1A Cu1A 118.4(5) . . ? C4A O1A Gd1 123.4(5) . . ? Cu1A O1A Gd1 106.9(2) . . ? C3A O2A Gd1 118.4(5) . . ? C1A O3A C5A 118.1(7) . . ? C14A O4A Cu1A 120.8(4) . . ? C14A O4A Gd1 120.7(4) . . ? Cu1A O4A Gd1 110.7(2) . . ? C13A O5A Gd1 117.8(4) . . ? C11A O6A C10A 118.3(7) . . ? C6A N1A C7A 113.0(7) . . ? C6A N1A C15A 108.6(7) . . ? C7A N1A C15A 109.3(7) . . ? C6A N1A Cu1A 111.5(5) . . ? C7A N1A Cu1A 104.7(5) . . ? C15A N1A Cu1A 109.7(5) . . ? C16A N2A C9A 109.3(7) . . ? C16A N2A C8A 108.5(6) . . ? C9A N2A C8A 112.0(7) . . ? C16A N2A Cu1A 115.0(6) . . ? C9A N2A Cu1A 110.2(4) . . ? C8A N2A Cu1A 101.8(5) . . ? C2A C1A O3A 123.6(10) . . ? C2A C1A H1A 118.2 . . ? O3A C1A H1A 118.2 . . ? C1A C2A C3A 120.3(10) . . ? C1A C2A H2A 119.8 . . ? C3A C2A H2A 119.8 . . ? O2A C3A C2A 125.1(9) . . ? O2A C3A C4A 119.6(8) . . ? C2A C3A C4A 115.4(8) . . ? C5A C4A O1A 127.0(9) . . ? C5A C4A C3A 120.0(8) . . ? O1A C4A C3A 112.7(6) . . ? C4A C5A O3A 122.2(8) . . ? C4A C5A C6A 128.7(9) . . ? O3A C5A C6A 108.9(7) . . ? N1A C6A C5A 113.0(7) . . ? N1A C6A H6A1 109.0 . . ? C5A C6A H6A1 109.0 . . ? N1A C6A H6A2 109.0 . . ? C5A C6A H6A2 109.0 . . ? H6A1 C6A H6A2 107.8 . . ? N1A C7A C8A 110.8(6) . . ? N1A C7A H7A1 109.5 . . ? C8A C7A H7A1 109.5 . . ? N1A C7A H7A2 109.5 . . ? C8A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 108.1 . . ? C7A C8A N2A 110.3(7) . . ? C7A C8A H8A1 109.6 . . ? N2A C8A H8A1 109.6 . . ? C7A C8A H8A2 109.6 . . ? N2A C8A H8A2 109.6 . . ? H8A1 C8A H8A2 108.1 . . ? N2A C9A C10A 110.2(8) . . ? N2A C9A H9A1 109.6 . . ? C10A C9A H9A1 109.6 . . ? N2A C9A H9A2 109.6 . . ? C10A C9A H9A2 109.6 . . ? H9A1 C9A H9A2 108.1 . . ? O6A C10A C14A 121.2(8) . . ? O6A C10A C9A 115.9(7) . . ? C14A C10A C9A 122.8(8) . . ? O6A C11A C12A 123.6(8) . . ? O6A C11A H11A 118.2 . . ? C12A C11A H11A 118.2 . . ? C11A C12A C13A 119.9(8) . . ? C11A C12A H12A 120.1 . . ? C13A C12A H12A 120.1 . . ? O5A C13A C12A 125.9(7) . . ? O5A C13A C14A 118.7(7) . . ? C12A C13A C14A 115.5(7) . . ? O4A C14A C10A 121.4(7) . . ? O4A C14A C13A 117.1(7) . . ? C10A C14A C13A 121.5(8) . . ? N1A C15A H15A 109.5 . . ? N1A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? N1A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? N2A C16A H16A 109.5 . . ? N2A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? N2A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? O4B Cu1B O1B 79.6(6) . . ? O4B Cu1B O1C 81.5(6) . . ? O1B Cu1B O1C 9.8(7) . . ? O4B Cu1B N1B 168.3(8) . . ? O1B Cu1B N1B 95.2(8) . . ? O1C Cu1B N1B 91.6(8) . . ? O4B Cu1B O4C 9.8(7) . . ? O1B Cu1B O4C 77.8(6) . . ? O1C Cu1B O4C 78.1(6) . . ? N1B Cu1B O4C 158.7(8) . . ? O4B Cu1B N2B 96.3(6) . . ? O1B Cu1B N2B 161.7(7) . . ? O1C Cu1B N2B 152.4(7) . . ? N1B Cu1B N2B 85.5(8) . . ? O4C Cu1B N2B 95.0(6) . . ? O4B Cu1B N2C 91.7(6) . . ? O1B Cu1B N2C 169.8(6) . . ? O1C Cu1B N2C 163.5(7) . . ? N1B Cu1B N2C 92.4(8) . . ? O4C Cu1B N2C 92.7(6) . . ? N2B Cu1B N2C 13.4(6) . . ? O4B Cu1B N1C 175.9(7) . . ? O1B Cu1B N1C 96.3(7) . . ? O1C Cu1B N1C 94.3(7) . . ? N1B Cu1B N1C 10.0(9) . . ? O4C Cu1B N1C 168.2(7) . . ? N2B Cu1B N1C 87.5(7) . . ? N2C Cu1B N1C 92.3(7) . . ? O4B Cu1B O1WB 85.7(5) . . ? O1B Cu1B O1WB 92.1(5) . . ? O1C Cu1B O1WB 101.9(5) . . ? N1B Cu1B O1WB 105.0(6) . . ? O4C Cu1B O1WB 95.4(4) . . ? N2B Cu1B O1WB 105.4(5) . . ? N2C Cu1B O1WB 92.5(5) . . ? N1C Cu1B O1WB 95.0(6) . . ? O4B Cu1B Gd1 40.2(5) . . ? O1B Cu1B Gd1 39.4(4) . . ? O1C Cu1B Gd1 42.1(4) . . ? N1B Cu1B Gd1 133.7(7) . . ? O4C Cu1B Gd1 39.2(4) . . ? N2B Cu1B Gd1 133.8(4) . . ? N2C Cu1B Gd1 131.6(4) . . ? N1C Cu1B Gd1 135.7(5) . . ? O1WB Cu1B Gd1 88.72(15) . . ? Cu1B O1WB H1WC 101(7) . . ? Cu1B O1WB H1WD 130(8) . . ? H1WC O1WB H1WD 108(3) . . ? C4B O1B Cu1B 126.4(15) . . ? C4B O1B Gd1 119.5(14) . . ? Cu1B O1B Gd1 110.2(6) . . ? C3B O2B Gd1 118.8(15) . . ? C5B O3B C1B 119.4(13) . . ? C14B O4B Cu1B 121.6(14) . . ? C14B O4B Gd1 127.4(13) . . ? Cu1B O4B Gd1 109.3(7) . . ? C13B O5B Gd1 116.0(14) . . ? C11B O6B C10B 120.5(15) . . ? C6B N1B C7B 111.5(17) . . ? C6B N1B C15B 110.5(17) . . ? C7B N1B C15B 112.3(16) . . ? C6B N1B Cu1B 112.8(13) . . ? C7B N1B Cu1B 103.3(14) . . ? C15B N1B Cu1B 106.3(13) . . ? C8B N2B C16B 104.1(16) . . ? C8B N2B C9B 121.3(16) . . ? C16B N2B C9B 106.1(13) . . ? C8B N2B Cu1B 106.9(13) . . ? C16B N2B Cu1B 111.9(12) . . ? C9B N2B Cu1B 106.6(10) . . ? C2B C1B O3B 119(2) . . ? C2B C1B H1B 120.6 . . ? O3B C1B H1B 120.6 . . ? C1B C2B C3B 127(3) . . ? C1B C2B H2B 116.6 . . ? C3B C2B H2B 116.6 . . ? C4B C3B O2B 119(3) . . ? C4B C3B C2B 111(3) . . ? O2B C3B C2B 130(3) . . ? C3B C4B C5B 124(3) . . ? C3B C4B O1B 120(3) . . ? C5B C4B O1B 114(2) . . ? O3B C5B C4B 116.5(18) . . ? O3B C5B C6B 112.2(13) . . ? C4B C5B C6B 131.2(18) . . ? N1B C6B C5B 114.6(14) . . ? N1B C6B H6B1 108.6 . . ? C5B C6B H6B1 108.6 . . ? N1B C6B H6B2 108.6 . . ? C5B C6B H6B2 108.6 . . ? H6B1 C6B H6B2 107.6 . . ? C8B C7B N1B 116.9(17) . . ? C8B C7B H7B1 108.1 . . ? N1B C7B H7B1 108.1 . . ? C8B C7B H7B2 108.1 . . ? N1B C7B H7B2 108.1 . . ? H7B1 C7B H7B2 107.3 . . ? C7B C8B N2B 115.7(19) . . ? C7B C8B H8B1 108.4 . . ? N2B C8B H8B1 108.4 . . ? C7B C8B H8B2 108.4 . . ? N2B C8B H8B2 108.4 . . ? H8B1 C8B H8B2 107.4 . . ? C10B C9B N2B 116.5(13) . . ? C10B C9B H9B1 108.2 . . ? N2B C9B H9B1 108.2 . . ? C10B C9B H9B2 108.2 . . ? N2B C9B H9B2 108.2 . . ? H9B1 C9B H9B2 107.3 . . ? O6B C10B C14B 120.8(15) . . ? O6B C10B C9B 111.3(14) . . ? C14B C10B C9B 127.9(16) . . ? O6B C11B C12B 123.3(19) . . ? O6B C11B H11B 118.3 . . ? C12B C11B H11B 118.3 . . ? C13B C12B C11B 115(2) . . ? C13B C12B H12B 122.5 . . ? C11B C12B H12B 122.5 . . ? C12B C13B C14B 122(2) . . ? C12B C13B O5B 119(2) . . ? C14B C13B O5B 115(2) . . ? O4B C14B C10B 126.5(18) . . ? O4B C14B C13B 116(2) . . ? C10B C14B C13B 117(2) . . ? N1B C15B H15D 109.5 . . ? N1B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? N1B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? N2B C16B H16D 109.5 . . ? N2B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? N2B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C6C N1C C15C 110.1(15) . . ? C6C N1C C7C 107.7(15) . . ? C15C N1C C7C 108.3(14) . . ? C6C N1C Cu1B 111.9(13) . . ? C15C N1C Cu1B 113.3(12) . . ? C7C N1C Cu1B 105.2(12) . . ? C9C N2C C8C 124.6(17) . . ? C9C N2C C16C 102.0(17) . . ? C8C N2C C16C 92.2(16) . . ? C9C N2C Cu1B 117.5(13) . . ? C8C N2C Cu1B 104.9(13) . . ? C16C N2C Cu1B 112.5(13) . . ? C4C O1C Cu1B 112.4(13) . . ? C4C O1C Gd1 121.5(13) . . ? Cu1B O1C Gd1 105.8(7) . . ? C3C O2C Gd1 117(2) . . ? C1C O3C C5C 119.3(15) . . ? C14C O4C Cu1B 124.0(13) . . ? C14C O4C Gd1 118.6(12) . . ? Cu1B O4C Gd1 109.2(6) . . ? C13C O5C Gd1 120.1(14) . . ? C10C O6C C11C 117.7(17) . . ? O3C C1C C2C 125(2) . . ? O3C C1C H1C 117.7 . . ? C2C C1C H1C 117.7 . . ? C3C C2C C1C 113(2) . . ? C3C C2C H2C 123.7 . . ? C1C C2C H2C 123.7 . . ? O2C C3C C2C 125(3) . . ? O2C C3C C4C 121(3) . . ? C2C C3C C4C 114(2) . . ? C5C C4C O1C 126(2) . . ? C5C C4C C3C 118(2) . . ? O1C C4C C3C 111(2) . . ? C4C C5C O3C 127.4(17) . . ? C4C C5C C6C 118.9(17) . . ? O3C C5C C6C 113.6(13) . . ? N1C C6C C5C 109.2(14) . . ? N1C C6C H6C1 109.8 . . ? C5C C6C H6C1 109.8 . . ? N1C C6C H6C2 109.8 . . ? C5C C6C H6C2 109.8 . . ? H6C1 C6C H6C2 108.3 . . ? N1C C7C C8C 104.2(14) . . ? N1C C7C H7C1 110.9 . . ? C8C C7C H7C1 110.9 . . ? N1C C7C H7C2 110.9 . . ? C8C C7C H7C2 110.9 . . ? H7C1 C7C H7C2 108.9 . . ? N2C C8C C7C 117.2(17) . . ? N2C C8C H8C1 108.0 . . ? C7C C8C H8C1 108.0 . . ? N2C C8C H8C2 108.0 . . ? C7C C8C H8C2 108.0 . . ? H8C1 C8C H8C2 107.2 . . ? N2C C9C C10C 108.3(18) . . ? N2C C9C H9C1 110.0 . . ? C10C C9C H9C1 110.0 . . ? N2C C9C H9C2 110.0 . . ? C10C C9C H9C2 110.0 . . ? H9C1 C9C H9C2 108.4 . . ? C14C C10C O6C 118.3(17) . . ? C14C C10C C9C 127.8(19) . . ? O6C C10C C9C 113.1(17) . . ? C12C C11C O6C 125(2) . . ? C12C C11C H11C 117.7 . . ? O6C C11C H11C 117.7 . . ? C11C C12C C13C 121(2) . . ? C11C C12C H12C 119.5 . . ? C13C C12C H12C 119.5 . . ? O5C C13C C12C 127(2) . . ? O5C C13C C14C 118(2) . . ? C12C C13C C14C 111(2) . . ? C10C C14C O4C 117.9(18) . . ? C10C C14C C13C 126(2) . . ? O4C C14C C13C 115.8(18) . . ? N1C C15C H15G 109.5 . . ? N1C C15C H15H 109.5 . . ? H15G C15C H15H 109.5 . . ? N1C C15C H15I 109.5 . . ? H15G C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? N2C C16C H16G 109.5 . . ? N2C C16C H16H 109.5 . . ? H16G C16C H16H 109.5 . . ? N2C C16C H16I 109.5 . . ? H16G C16C H16I 109.5 . . ? H16H C16C H16I 109.5 . . ? O14 Cl1 O11 114.5(7) . . ? O14 Cl1 O13 111.9(7) . . ? O11 Cl1 O13 107.8(9) . . ? O14 Cl1 O12 108.7(5) . . ? O11 Cl1 O12 108.7(6) . . ? O13 Cl1 O12 104.7(7) . . ? O23 Cl2 O21 114.0(6) . . ? O23 Cl2 O22 105.4(8) . . ? O21 Cl2 O22 104.1(6) . . ? O23 Cl2 O24 110.5(7) . . ? O21 Cl2 O24 111.3(6) . . ? O22 Cl2 O24 111.3(9) . . ? O31 Cl3 O34 128.7(12) . . ? O31 Cl3 O32 104.4(9) . . ? O34 Cl3 O32 122.0(10) . . ? O31 Cl3 O33A 100.5(11) . . ? O34 Cl3 O33A 94.5(11) . . ? O32 Cl3 O33A 97.2(9) . . ? O31 Cl3 O33B 89.3(12) . . ? O34 Cl3 O33B 78.8(12) . . ? O32 Cl3 O33B 80.7(10) . . ? O33A Cl3 O33B 170.2(13) . . ? H3WA O3W H3WB 110(4) . . ? H4WA O4W H4WB 111(4) . . ? H5WA O5W H5WB 108(4) . . ? _diffrn_measured_fraction_theta_max 0.825 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.406 _refine_diff_density_min -1.954 _refine_diff_density_rms 0.143 data_2 _database_code_depnum_ccdc_archive 'CCDC 901273' #TrackingRef '1-2-3.cif' _vrf_PLAT_241 ; PROBLEM: Check High Ueq as compared to neighbors for C6B, C7B, C9B RESPONSE: The presence of disorder involving the atoms of the fragment connecting the two maltol rings in the ligand labelled as B has been taken into account. Due to the fact that it was not possible to locate a second position for C16b no double positions were introduced. ; _vfr_PLAT_420 ; PROBLEM: D-H without acceptor ...O2W-H2W1 RESPONSE: A weak hydrogen bond (according to G. R. Desiraju and T. Steiner, The Weak Hydrogen Bond, Oxford University Press, 2001) involving the hydrogen atom H2W1 and the oxygen atom O2A is present. The H2W1...O2A distance is 2.64(6)A) ; _vrf_PLAT_910 ; PROBLEM: Missing # of FCF Reflections Below Th(Min) ..... 41 RESPONSE: Data were collected with a CCD detector. The reflections in question were affected by the beam-stop. Only a small number of reflections are missing out of the total number of reflections observed. Resolution and completeness statistics #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.985 4912 4837 75 23.01 0.550 0.980 6541 6410 131 25.24 0.600 0.972 8490 8254 236 #----------------------------------------------------------- ACTA Min. Res. --- ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Cl3 Cu2 N4 O26 Y' _chemical_formula_weight 1219.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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 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 13.050(10) _cell_length_b 23.765(5) _cell_length_c 15.900(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.98(7) _cell_angle_gamma 90.00 _cell_volume 4690(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 1752 _cell_measurement_theta_min 4.1877 _cell_measurement_theta_max 29.0411 _exptl_crystal_description parallelepipedal _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 2.389 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.55408 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.4547 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19548 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.3638 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 29.13 _reflns_number_total 10120 _reflns_number_gt 2939 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_structure_solution 'SIR2004 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farruggia, 1997)' _computing_publication_material 'PARST97 (Nardelli, 1995)' _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^ > 2\s(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. 56 restrains were used in the refinement, they are related to the distances between Cl-O and O...O atoms in the perchlorate anions (in two of them the oxygen atoms are in double position) and to the O-H and H...H distances in the two water molecules. ; _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^)+(0.0674P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10120 _refine_ls_number_parameters 618 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.2061 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 0.762 _refine_ls_restrained_S_all 0.780 _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 Y1 Y 0.55634(7) 0.10065(3) 0.38790(5) 0.0595(3) Uani 1 1 d . . . O2W O 0.4875(4) 0.0886(2) 0.5134(4) 0.0732(17) Uani 1 1 d D . . Cu1A Cu 0.80506(8) 0.17101(4) 0.44139(6) 0.0617(3) Uani 1 1 d . . . O1A O 0.7314(4) 0.11277(18) 0.4904(3) 0.0616(15) Uani 1 1 d . . . O2A O 0.6300(5) 0.01441(18) 0.4770(3) 0.0623(15) Uani 1 1 d . . . O3A O 0.9569(5) 0.0216(3) 0.5949(4) 0.0782(18) Uani 1 1 d . . . O4A O 0.6645(4) 0.17507(18) 0.3615(3) 0.0659(15) Uani 1 1 d . . . O5A O 0.4984(5) 0.1392(3) 0.2309(3) 0.0854(19) Uani 1 1 d . . . O6A O 0.6671(6) 0.2812(3) 0.2034(5) 0.103(2) Uani 1 1 d . . . N1A N 0.9292(5) 0.1713(3) 0.5512(4) 0.0631(18) Uani 1 1 d . . . N2A N 0.8698(6) 0.2398(3) 0.3996(4) 0.071(2) Uani 1 1 d . . . C1A C 0.9061(9) -0.0273(4) 0.5916(7) 0.093(3) Uani 1 1 d . . . H1A H 0.9465 -0.0590 0.6154 0.112 Uiso 1 1 calc R . . C2A C 0.8015(9) -0.0328(3) 0.5561(6) 0.090(3) Uani 1 1 d . . . H2A H 0.7707 -0.0682 0.5547 0.108 Uiso 1 1 calc R . . C3A C 0.7314(8) 0.0154(3) 0.5183(5) 0.065(2) Uani 1 1 d . . . C4A C 0.7918(7) 0.0682(3) 0.5268(5) 0.052(2) Uani 1 1 d . . . C5A C 0.9029(7) 0.0686(3) 0.5652(4) 0.058(2) Uani 1 1 d . . . C6A C 0.9814(7) 0.1160(3) 0.5703(5) 0.080(3) Uani 1 1 d . . . H6A1 H 1.0332 0.1167 0.6291 0.095 Uiso 1 1 calc R . . H6A2 H 1.0207 0.1088 0.5286 0.095 Uiso 1 1 calc R . . C7A C 1.0060(8) 0.2137(4) 0.5372(6) 0.099(3) Uani 1 1 d . . . H7A1 H 1.0511 0.1968 0.5057 0.118 Uiso 1 1 calc R . . H7A2 H 1.0521 0.2273 0.5937 0.118 Uiso 1 1 calc R . . C8A C 0.9424(8) 0.2620(4) 0.4840(6) 0.090(3) Uani 1 1 d . . . H8A1 H 0.9004 0.2802 0.5171 0.108 Uiso 1 1 calc R . . H8A2 H 0.9911 0.2896 0.4724 0.108 Uiso 1 1 calc R . . C9A C 0.7781(8) 0.2783(3) 0.3552(6) 0.087(3) Uani 1 1 d . . . H9A1 H 0.7465 0.2917 0.3993 0.104 Uiso 1 1 calc R . . H9A2 H 0.8067 0.3108 0.3330 0.104 Uiso 1 1 calc R . . C10A C 0.6931(8) 0.2536(4) 0.2825(7) 0.078(3) Uani 1 1 d . . . C11A C 0.5873(10) 0.2616(5) 0.1367(8) 0.104(4) Uani 1 1 d . . . H11A H 0.5724 0.2812 0.0837 0.124 Uiso 1 1 calc R . . C12A C 0.5228(9) 0.2148(5) 0.1364(7) 0.113(4) Uani 1 1 d . . . H12A H 0.4664 0.2046 0.0868 0.136 Uiso 1 1 calc R . . C13A C 0.5485(8) 0.1835(4) 0.2166(6) 0.080(3) Uani 1 1 d . . . C14A C 0.6407(8) 0.2051(4) 0.2861(5) 0.070(3) Uani 1 1 d . . . C15A C 0.8862(8) 0.1910(3) 0.6233(5) 0.091(3) Uani 1 1 d . . . H15A H 0.8526 0.2271 0.6079 0.137 Uiso 1 1 calc R . . H15B H 0.9444 0.1941 0.6776 0.137 Uiso 1 1 calc R . . H15C H 0.8342 0.1644 0.6306 0.137 Uiso 1 1 calc R . . C16A C 0.9301(8) 0.2268(3) 0.3358(6) 0.095(3) Uani 1 1 d . . . H16A H 0.9879 0.2013 0.3627 0.143 Uiso 1 1 calc R . . H16B H 0.9590 0.2610 0.3201 0.143 Uiso 1 1 calc R . . H16C H 0.8821 0.2099 0.2836 0.143 Uiso 1 1 calc R . . Cu1B Cu 0.32965(8) 0.05897(4) 0.22926(6) 0.0672(4) Uani 1 1 d . . . O1B O 0.3615(4) 0.10760(19) 0.3288(3) 0.0661(15) Uani 1 1 d . . . O2B O 0.4841(5) 0.1893(2) 0.4201(4) 0.0754(18) Uani 1 1 d . . . O3B O 0.1743(6) 0.2249(3) 0.2672(5) 0.110(2) Uani 1 1 d . . . O4B O 0.4705(4) 0.02943(19) 0.2888(3) 0.0683(16) Uani 1 1 d . . . O5B O 0.6804(4) 0.0482(2) 0.3273(3) 0.0663(15) Uani 1 1 d . . . O6B O 0.5445(8) -0.0581(4) 0.1297(5) 0.149(4) Uani 1 1 d . . . N1B N 0.1875(7) 0.0924(3) 0.1674(5) 0.086(2) Uani 1 1 d . . . N2B N 0.2886(7) -0.0059(4) 0.1497(7) 0.117(3) Uani 1 1 d . . . C1B C 0.2354(11) 0.2639(4) 0.3154(7) 0.105(4) Uani 1 1 d . . . H1B H 0.2066 0.3000 0.3113 0.126 Uiso 1 1 calc R . . C2B C 0.3367(10) 0.2568(4) 0.3709(6) 0.089(3) Uani 1 1 d . . . H2B H 0.3727 0.2867 0.4050 0.107 Uiso 1 1 calc R . . C3B C 0.3900(8) 0.2014(3) 0.3771(6) 0.064(2) Uani 1 1 d . . . C4B C 0.3192(7) 0.1598(3) 0.3229(5) 0.062(2) Uani 1 1 d . . . C5B C 0.2195(8) 0.1717(4) 0.2716(7) 0.090(3) Uani 1 1 d . . . C6B C 0.1402(8) 0.1247(6) 0.2180(8) 0.171(6) Uani 1 1 d . . . H6B1 H 0.1193 0.1005 0.2591 0.205 Uiso 1 1 calc R . . H6B2 H 0.0756 0.1423 0.1797 0.205 Uiso 1 1 calc R . . C7B C 0.1200(9) 0.0499(4) 0.1187(9) 0.142(5) Uani 1 1 d . . . H7B1 H 0.0675 0.0668 0.0678 0.171 Uiso 1 1 calc R . . H7B2 H 0.0810 0.0330 0.1552 0.171 Uiso 1 1 calc R . . C8B C 0.1792(8) 0.0050(4) 0.0874(6) 0.099(3) Uani 1 1 d . . . H8B1 H 0.1376 -0.0295 0.0791 0.119 Uiso 1 1 calc R . . H8B2 H 0.1858 0.0159 0.0305 0.119 Uiso 1 1 calc R . . C9B C 0.3658(11) -0.0290(6) 0.1130(9) 0.177(7) Uani 1 1 d . . . H9B1 H 0.3612 -0.0086 0.0591 0.213 Uiso 1 1 calc R . . H9B2 H 0.3458 -0.0677 0.0966 0.213 Uiso 1 1 calc R . . C10B C 0.4828(10) -0.0283(4) 0.1715(8) 0.112(4) Uani 1 1 d . . . C11B C 0.6549(14) -0.0537(5) 0.1609(8) 0.136(5) Uani 1 1 d . . . H11B H 0.6961 -0.0746 0.1338 0.163 Uiso 1 1 calc R . . C12B C 0.7040(8) -0.0209(4) 0.2278(6) 0.095(3) Uani 1 1 d . . . H12B H 0.7788 -0.0189 0.2481 0.115 Uiso 1 1 calc R . . C13B C 0.6407(9) 0.0116(3) 0.2689(6) 0.075(3) Uani 1 1 d . . . C14B C 0.5263(8) 0.0023(3) 0.2430(6) 0.072(3) Uani 1 1 d . . . C15B C 0.2073(9) 0.1344(5) 0.0993(7) 0.148(5) Uani 1 1 d . . . H15D H 0.2531 0.1643 0.1301 0.222 Uiso 1 1 calc R . . H15E H 0.1397 0.1497 0.0638 0.222 Uiso 1 1 calc R . . H15F H 0.2413 0.1152 0.0620 0.222 Uiso 1 1 calc R . . C16B C 0.2714(11) -0.0547(5) 0.2122(10) 0.197(8) Uani 1 1 d . . . H16D H 0.2218 -0.0423 0.2422 0.296 Uiso 1 1 calc R . . H16E H 0.3391 -0.0640 0.2550 0.296 Uiso 1 1 calc R . . H16F H 0.2427 -0.0874 0.1773 0.296 Uiso 1 1 calc R . . Cl1 Cl 0.7879(2) 0.12542(11) 0.10258(17) 0.1032(9) Uani 1 1 d D . . O11 O 0.8668(10) 0.1077(6) 0.1873(6) 0.212(7) Uiso 0.60 1 d PD A 1 O12 O 0.6930(7) 0.0931(5) 0.0893(9) 0.157(6) Uiso 0.60 1 d PD A 1 O13 O 0.7719(11) 0.1839(3) 0.1072(10) 0.174(6) Uiso 0.60 1 d PD A 1 O14 O 0.8399(8) 0.1129(5) 0.0364(6) 0.131(4) Uiso 0.60 1 d PD A 1 O15 O 0.8639(11) 0.1612(7) 0.1620(10) 0.157(8) Uiso 0.40 1 d PD A 2 O16 O 0.7206(12) 0.1605(7) 0.0296(9) 0.160(8) Uiso 0.40 1 d PD A 2 O17 O 0.7141(13) 0.1043(8) 0.1483(12) 0.212(12) Uiso 0.40 1 d PD A 2 O18 O 0.8335(14) 0.0813(6) 0.0681(12) 0.203(12) Uiso 0.40 1 d PD A 2 Cl2 Cl 0.9559(2) -0.09537(10) 0.15240(16) 0.0990(9) Uani 1 1 d D . . O21 O 1.0212(9) -0.1199(5) 0.1033(8) 0.147(5) Uiso 0.60 1 d PD B 1 O22 O 0.9103(8) -0.0447(4) 0.1114(8) 0.137(4) Uiso 0.60 1 d PD B 1 O23 O 0.8929(10) -0.1309(5) 0.1823(9) 0.192(6) Uiso 0.60 1 d PD B 1 O24 O 1.0432(9) -0.0752(6) 0.2357(6) 0.216(7) Uiso 0.60 1 d PD B 1 O25 O 0.8495(8) -0.1170(6) 0.1053(10) 0.130(6) Uiso 0.40 1 d PD B 2 O26 O 0.9525(15) -0.0470(6) 0.2022(12) 0.201(10) Uiso 0.40 1 d PD B 2 O27 O 1.0065(15) -0.0824(9) 0.0840(10) 0.224(13) Uiso 0.40 1 d PD B 2 O28 O 1.0171(14) -0.1395(6) 0.2060(12) 0.221(11) Uiso 0.40 1 d PD B 2 Cl3 Cl 0.3039(3) 0.17132(14) 0.6107(3) 0.1555(15) Uani 1 1 d D . . O31 O 0.2885(7) 0.2305(3) 0.6219(7) 0.221(5) Uani 1 1 d D . . O32 O 0.2337(6) 0.1399(4) 0.6429(5) 0.191(4) Uani 1 1 d D . . O33 O 0.2694(13) 0.1633(4) 0.5154(5) 0.381(13) Uani 1 1 d D . . O34 O 0.4124(6) 0.1553(4) 0.6466(11) 0.411(15) Uani 1 1 d D . . O1WA O 0.8703(5) 0.1043(2) 0.3569(4) 0.0776(18) Uani 1 1 d D . . H2W1 H 0.545(3) 0.104(2) 0.529(5) 0.093 Uiso 1 1 d D . . H2W2 H 0.491(5) 0.0558(14) 0.531(5) 0.093 Uiso 1 1 d D . . H1W1 H 0.920(5) 0.091(3) 0.343(5) 0.093 Uiso 1 1 d D . . H1W2 H 0.847(5) 0.1331(19) 0.329(4) 0.093 Uiso 1 1 d 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 Y1 0.0706(6) 0.0534(5) 0.0444(5) -0.0072(4) 0.0029(4) 0.0012(4) O2W 0.090(5) 0.071(4) 0.054(4) 0.004(3) 0.017(3) -0.008(3) Cu1A 0.0823(8) 0.0552(6) 0.0407(6) -0.0002(5) 0.0089(5) -0.0067(5) O1A 0.077(4) 0.047(3) 0.051(3) -0.003(2) 0.005(3) -0.007(3) O2A 0.067(4) 0.052(3) 0.064(4) 0.000(3) 0.014(3) -0.006(3) O3A 0.079(5) 0.072(4) 0.074(4) 0.018(3) 0.010(3) 0.015(4) O4A 0.089(4) 0.059(3) 0.043(3) 0.018(3) 0.011(3) -0.004(3) O5A 0.101(5) 0.093(4) 0.048(4) 0.008(3) 0.002(3) 0.013(4) O6A 0.105(6) 0.103(5) 0.098(6) 0.056(5) 0.027(5) 0.014(4) N1A 0.064(5) 0.070(4) 0.047(4) -0.009(4) 0.005(4) -0.032(4) N2A 0.094(6) 0.068(4) 0.049(5) 0.016(4) 0.021(4) 0.014(4) C1A 0.071(8) 0.075(7) 0.118(9) 0.038(6) 0.005(7) 0.043(6) C2A 0.127(10) 0.043(5) 0.089(7) 0.031(5) 0.016(7) 0.034(6) C3A 0.084(7) 0.074(6) 0.041(5) -0.003(4) 0.026(5) -0.009(6) C4A 0.073(6) 0.033(4) 0.043(5) 0.014(4) 0.007(4) 0.017(4) C5A 0.071(6) 0.056(5) 0.034(5) 0.004(4) -0.001(4) 0.003(5) C6A 0.099(8) 0.080(6) 0.044(5) -0.001(5) -0.001(5) -0.001(6) C7A 0.112(9) 0.088(7) 0.068(7) -0.005(6) -0.012(6) -0.012(7) C8A 0.108(8) 0.095(7) 0.065(7) -0.025(6) 0.022(6) -0.042(6) C9A 0.103(8) 0.073(6) 0.086(8) 0.018(6) 0.031(7) -0.004(6) C10A 0.097(8) 0.063(6) 0.080(8) 0.028(6) 0.036(6) 0.010(6) C11A 0.104(10) 0.123(10) 0.086(9) 0.044(8) 0.032(8) 0.028(8) C12A 0.092(9) 0.149(10) 0.092(8) 0.065(8) 0.021(7) 0.075(8) C13A 0.074(7) 0.088(7) 0.063(6) 0.036(6) -0.002(5) 0.052(6) C14A 0.083(7) 0.076(6) 0.051(6) 0.033(5) 0.023(5) 0.055(6) C15A 0.150(9) 0.094(6) 0.028(5) -0.023(4) 0.024(5) -0.007(6) C16A 0.118(9) 0.094(7) 0.073(7) 0.008(5) 0.028(7) -0.018(6) Cu1B 0.0781(8) 0.0577(6) 0.0519(6) -0.0040(5) -0.0002(5) -0.0033(5) O1B 0.061(4) 0.046(3) 0.076(4) -0.008(3) 0.000(3) -0.007(3) O2B 0.082(5) 0.069(4) 0.064(4) -0.014(3) 0.006(3) -0.014(3) O3B 0.107(6) 0.102(5) 0.104(6) -0.002(4) 0.005(4) 0.041(5) O4B 0.088(5) 0.056(3) 0.050(4) -0.010(3) 0.006(3) 0.010(3) O5B 0.075(4) 0.070(3) 0.052(3) -0.007(3) 0.018(3) 0.006(3) O6B 0.142(8) 0.171(7) 0.117(7) -0.100(6) 0.016(6) 0.019(7) N1B 0.103(7) 0.100(6) 0.044(4) 0.010(4) 0.006(4) -0.020(5) N2B 0.077(7) 0.113(7) 0.125(8) -0.067(6) -0.022(6) -0.002(5) C1B 0.162(12) 0.074(7) 0.063(7) 0.014(6) 0.009(7) 0.031(8) C2B 0.158(11) 0.066(6) 0.054(6) 0.002(5) 0.048(7) 0.011(7) C3B 0.093(8) 0.052(6) 0.054(6) -0.007(4) 0.035(5) -0.008(6) C4B 0.071(7) 0.052(5) 0.064(6) 0.003(4) 0.024(5) 0.001(5) C5B 0.066(7) 0.088(7) 0.098(8) 0.000(6) 0.001(6) 0.014(6) C6B 0.054(8) 0.319(18) 0.112(10) -0.076(12) -0.015(7) 0.033(10) C7B 0.097(10) 0.086(8) 0.196(14) -0.017(8) -0.026(9) -0.008(7) C8B 0.098(9) 0.114(8) 0.057(6) -0.004(6) -0.018(6) -0.042(7) C9B 0.108(12) 0.244(15) 0.151(13) -0.146(12) -0.003(10) -0.040(11) C10B 0.121(11) 0.102(8) 0.106(9) -0.049(7) 0.026(8) -0.006(7) C11B 0.181(15) 0.134(10) 0.104(10) -0.044(9) 0.062(10) 0.032(11) C12B 0.117(9) 0.086(6) 0.065(7) -0.024(6) 0.001(6) 0.031(6) C13B 0.128(10) 0.049(5) 0.043(5) -0.011(4) 0.020(6) 0.008(6) C14B 0.079(8) 0.054(5) 0.054(6) -0.019(4) -0.020(5) -0.019(5) C15B 0.162(12) 0.151(10) 0.101(9) 0.042(8) -0.004(8) 0.010(9) C16B 0.207(16) 0.088(8) 0.218(17) -0.009(10) -0.048(13) -0.026(9) Cl1 0.127(2) 0.1002(19) 0.0808(19) -0.0144(15) 0.0303(18) -0.0141(17) Cl2 0.137(3) 0.0839(17) 0.0792(17) 0.0151(15) 0.0381(17) 0.0161(17) Cl3 0.167(4) 0.111(3) 0.232(5) -0.052(3) 0.125(4) -0.038(3) O31 0.206(10) 0.116(6) 0.382(15) -0.128(8) 0.152(10) -0.024(6) O32 0.112(7) 0.250(10) 0.202(10) 0.092(8) 0.032(7) -0.012(7) O33 0.90(4) 0.158(9) 0.225(13) 0.024(10) 0.38(2) 0.042(16) O34 0.241(15) 0.141(9) 0.96(5) -0.145(16) 0.34(2) -0.032(10) O1WA 0.077(5) 0.083(4) 0.060(4) -0.002(3) 0.003(3) 0.035(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Y1 O4B 2.348(5) . ? Y1 O1A 2.379(5) . ? Y1 O4A 2.379(5) . ? Y1 O2B 2.427(6) . ? Y1 O1B 2.429(5) . ? Y1 O2W 2.444(7) . ? Y1 O5B 2.463(5) . ? Y1 O2A 2.508(5) . ? Y1 O5A 2.545(6) . ? Y1 Cu1B 3.389(3) . ? Y1 Cu1A 3.514(3) . ? Y1 H2W1 2.29(9) . ? O2W H2W1 0.80(2) . ? O2W H2W2 0.82(2) . ? Cu1A O4A 1.884(5) . ? Cu1A O1A 1.977(5) . ? Cu1A N1A 1.981(6) . ? Cu1A N2A 2.044(6) . ? Cu1A O1WA 2.399(5) . ? O1A C4A 1.341(7) . ? O2A C3A 1.283(9) . ? O3A C5A 1.328(8) . ? O3A C1A 1.332(10) . ? O4A C14A 1.348(8) . ? O5A C13A 1.297(10) . ? O6A C11A 1.321(11) . ? O6A C10A 1.365(10) . ? N1A C6A 1.469(9) . ? N1A C7A 1.485(10) . ? N1A C15A 1.498(9) . ? N2A C8A 1.481(9) . ? N2A C16A 1.495(10) . ? N2A C9A 1.499(10) . ? C1A C2A 1.313(11) . ? C1A H1A 0.9300 . ? C2A C3A 1.475(11) . ? C2A H2A 0.9300 . ? C3A C4A 1.464(10) . ? C4A C5A 1.389(10) . ? C5A C6A 1.507(10) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C7A C8A 1.512(10) . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C9A C10A 1.456(11) . ? C9A H9A1 0.9700 . ? C9A H9A2 0.9700 . ? C10A C14A 1.350(11) . ? C11A C12A 1.393(13) . ? C11A H11A 0.9300 . ? C12A C13A 1.422(11) . ? C12A H12A 0.9300 . ? C13A C14A 1.453(12) . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? Cu1B O1B 1.899(5) . ? Cu1B O4B 1.922(5) . ? Cu1B N2B 1.961(7) . ? Cu1B N1B 1.978(8) . ? O1B C4B 1.350(8) . ? O2B C3B 1.240(9) . ? O3B C1B 1.306(11) . ? O3B C5B 1.387(9) . ? O4B C14B 1.343(10) . ? O5B C13B 1.262(8) . ? O6B C11B 1.375(14) . ? O6B C10B 1.386(12) . ? N1B C6B 1.388(12) . ? N1B C7B 1.404(11) . ? N1B C15B 1.551(11) . ? N2B C9B 1.421(14) . ? N2B C8B 1.487(11) . ? N2B C16B 1.588(15) . ? C1B C2B 1.355(13) . ? C1B H1B 0.9300 . ? C2B C3B 1.477(11) . ? C2B H2B 0.9300 . ? C3B C4B 1.444(10) . ? C4B C5B 1.335(10) . ? C5B C6B 1.582(13) . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? C7B C8B 1.490(13) . ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C9B C10B 1.523(14) . ? C9B H9B1 0.9700 . ? C9B H9B2 0.9700 . ? C10B C14B 1.321(11) . ? C11B C12B 1.315(13) . ? C11B H11B 0.9300 . ? C12B C13B 1.427(12) . ? C12B H12B 0.9300 . ? C13B C14B 1.437(12) . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? Cl1 O18 1.398(8) . ? Cl1 O13 1.411(7) . ? Cl1 O12 1.417(7) . ? Cl1 O15 1.422(8) . ? Cl1 O14 1.449(7) . ? Cl1 O17 1.463(8) . ? Cl1 O16 1.478(8) . ? Cl1 O11 1.482(7) . ? Cl2 O23 1.363(7) . ? Cl2 O26 1.404(8) . ? Cl2 O22 1.410(7) . ? Cl2 O28 1.430(8) . ? Cl2 O21 1.444(7) . ? Cl2 O25 1.453(8) . ? Cl2 O27 1.468(8) . ? Cl2 O24 1.532(7) . ? Cl3 O32 1.397(6) . ? Cl3 O34 1.406(7) . ? Cl3 O31 1.439(5) . ? Cl3 O33 1.453(7) . ? O1WA H1W1 0.81(2) . ? O1WA H1W2 0.82(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4B Y1 O1A 134.86(18) . . ? O4B Y1 O4A 127.13(19) . . ? O1A Y1 O4A 62.24(16) . . ? O4B Y1 O2B 129.2(2) . . ? O1A Y1 O2B 95.96(18) . . ? O4A Y1 O2B 71.46(19) . . ? O4B Y1 O1B 64.14(18) . . ? O1A Y1 O1B 157.83(17) . . ? O4A Y1 O1B 119.23(17) . . ? O2B Y1 O1B 66.06(17) . . ? O4B Y1 O2W 104.1(2) . . ? O1A Y1 O2W 88.41(18) . . ? O4A Y1 O2W 128.19(18) . . ? O2B Y1 O2W 70.42(19) . . ? O1B Y1 O2W 73.70(19) . . ? O4B Y1 O5B 66.89(19) . . ? O1A Y1 O5B 73.81(18) . . ? O4A Y1 O5B 79.05(18) . . ? O2B Y1 O5B 150.13(18) . . ? O1B Y1 O5B 128.23(18) . . ? O2W Y1 O5B 135.36(17) . . ? O4B Y1 O2A 79.07(17) . . ? O1A Y1 O2A 65.94(16) . . ? O4A Y1 O2A 124.19(18) . . ? O2B Y1 O2A 134.14(18) . . ? O1B Y1 O2A 116.56(18) . . ? O2W Y1 O2A 67.47(17) . . ? O5B Y1 O2A 67.90(17) . . ? O4B Y1 O5A 70.46(19) . . ? O1A Y1 O5A 124.1(2) . . ? O4A Y1 O5A 64.68(19) . . ? O2B Y1 O5A 82.94(19) . . ? O1B Y1 O5A 68.7(2) . . ? O2W Y1 O5A 140.34(19) . . ? O5B Y1 O5A 80.25(18) . . ? O2A Y1 O5A 142.59(17) . . ? O4B Y1 Cu1B 33.28(13) . . ? O1A Y1 Cu1B 168.01(12) . . ? O4A Y1 Cu1B 121.00(12) . . ? O2B Y1 Cu1B 95.97(14) . . ? O1B Y1 Cu1B 33.17(12) . . ? O2W Y1 Cu1B 96.71(14) . . ? O5B Y1 Cu1B 95.11(13) . . ? O2A Y1 Cu1B 106.02(13) . . ? O5A Y1 Cu1B 56.54(16) . . ? O4B Y1 Cu1A 135.96(16) . . ? O1A Y1 Cu1A 32.51(12) . . ? O4A Y1 Cu1A 30.13(11) . . ? O2B Y1 Cu1A 85.75(15) . . ? O1B Y1 Cu1A 147.09(11) . . ? O2W Y1 Cu1A 113.77(14) . . ? O5B Y1 Cu1A 70.48(13) . . ? O2A Y1 Cu1A 95.03(14) . . ? O5A Y1 Cu1A 92.21(16) . . ? Cu1B Y1 Cu1A 147.98(5) . . ? O4B Y1 H2W1 121.3(8) . . ? O1A Y1 H2W1 70.4(8) . . ? O4A Y1 H2W1 111.6(8) . . ? O2B Y1 H2W1 67.5(16) . . ? O1B Y1 H2W1 90.0(11) . . ? O2W Y1 H2W1 19.1(5) . . ? O5B Y1 H2W1 130.4(16) . . ? O2A Y1 H2W1 66.7(16) . . ? O5A Y1 H2W1 149.0(16) . . ? Cu1B Y1 H2W1 115.6(6) . . ? Cu1A Y1 H2W1 94.6(5) . . ? Y1 O2W H2W1 69(7) . . ? Y1 O2W H2W2 113(6) . . ? H2W1 O2W H2W2 112(4) . . ? O4A Cu1A O1A 79.1(2) . . ? O4A Cu1A N1A 162.7(3) . . ? O1A Cu1A N1A 91.2(2) . . ? O4A Cu1A N2A 98.9(2) . . ? O1A Cu1A N2A 171.3(3) . . ? N1A Cu1A N2A 88.6(3) . . ? O4A Cu1A O1WA 95.5(2) . . ? O1A Cu1A O1WA 93.3(2) . . ? N1A Cu1A O1WA 99.3(3) . . ? N2A Cu1A O1WA 95.3(3) . . ? O4A Cu1A Y1 39.35(14) . . ? O1A Cu1A Y1 40.28(14) . . ? N1A Cu1A Y1 131.1(2) . . ? N2A Cu1A Y1 138.2(2) . . ? O1WA Cu1A Y1 90.63(16) . . ? C4A O1A Cu1A 115.5(5) . . ? C4A O1A Y1 120.8(4) . . ? Cu1A O1A Y1 107.2(2) . . ? C3A O2A Y1 115.4(5) . . ? C5A O3A C1A 121.2(7) . . ? C14A O4A Cu1A 122.4(5) . . ? C14A O4A Y1 124.4(6) . . ? Cu1A O4A Y1 110.5(2) . . ? C13A O5A Y1 116.9(5) . . ? C11A O6A C10A 118.7(9) . . ? C6A N1A C7A 110.3(7) . . ? C6A N1A C15A 112.3(6) . . ? C7A N1A C15A 109.4(6) . . ? C6A N1A Cu1A 112.4(4) . . ? C7A N1A Cu1A 106.0(5) . . ? C15A N1A Cu1A 106.1(5) . . ? C8A N2A C16A 111.5(7) . . ? C8A N2A C9A 113.8(7) . . ? C16A N2A C9A 108.5(6) . . ? C8A N2A Cu1A 101.7(5) . . ? C16A N2A Cu1A 114.4(5) . . ? C9A N2A Cu1A 106.9(5) . . ? C2A C1A O3A 122.9(8) . . ? C2A C1A H1A 118.6 . . ? O3A C1A H1A 118.6 . . ? C1A C2A C3A 122.0(9) . . ? C1A C2A H2A 119.0 . . ? C3A C2A H2A 119.0 . . ? O2A C3A C4A 120.3(7) . . ? O2A C3A C2A 127.3(8) . . ? C4A C3A C2A 112.3(8) . . ? O1A C4A C5A 125.3(7) . . ? O1A C4A C3A 114.1(7) . . ? C5A C4A C3A 120.5(7) . . ? O3A C5A C4A 121.1(7) . . ? O3A C5A C6A 109.4(7) . . ? C4A C5A C6A 129.1(7) . . ? N1A C6A C5A 113.2(7) . . ? N1A C6A H6A1 108.9 . . ? C5A C6A H6A1 108.9 . . ? N1A C6A H6A2 108.9 . . ? C5A C6A H6A2 108.9 . . ? H6A1 C6A H6A2 107.8 . . ? N1A C7A C8A 108.6(8) . . ? N1A C7A H7A1 110.0 . . ? C8A C7A H7A1 110.0 . . ? N1A C7A H7A2 110.0 . . ? C8A C7A H7A2 110.0 . . ? H7A1 C7A H7A2 108.3 . . ? N2A C8A C7A 108.9(7) . . ? N2A C8A H8A1 109.9 . . ? C7A C8A H8A1 109.9 . . ? N2A C8A H8A2 109.9 . . ? C7A C8A H8A2 109.9 . . ? H8A1 C8A H8A2 108.3 . . ? C10A C9A N2A 115.5(7) . . ? C10A C9A H9A1 108.4 . . ? N2A C9A H9A1 108.4 . . ? C10A C9A H9A2 108.4 . . ? N2A C9A H9A2 108.4 . . ? H9A1 C9A H9A2 107.5 . . ? C14A C10A O6A 117.6(9) . . ? C14A C10A C9A 125.6(8) . . ? O6A C10A C9A 116.7(9) . . ? O6A C11A C12A 127.6(10) . . ? O6A C11A H11A 116.2 . . ? C12A C11A H11A 116.2 . . ? C11A C12A C13A 116.0(11) . . ? C11A C12A H12A 122.0 . . ? C13A C12A H12A 122.0 . . ? O5A C13A C12A 126.2(10) . . ? O5A C13A C14A 119.8(8) . . ? C12A C13A C14A 114.0(10) . . ? O4A C14A C10A 120.7(9) . . ? O4A C14A C13A 113.5(8) . . ? C10A C14A C13A 125.5(8) . . ? N1A C15A H15A 109.5 . . ? N1A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? N1A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? N2A C16A H16A 109.5 . . ? N2A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? N2A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? O1B Cu1B O4B 83.2(2) . . ? O1B Cu1B N2B 164.1(4) . . ? O4B Cu1B N2B 93.4(3) . . ? O1B Cu1B N1B 95.8(3) . . ? O4B Cu1B N1B 177.6(3) . . ? N2B Cu1B N1B 88.1(4) . . ? O1B Cu1B Y1 44.42(16) . . ? O4B Cu1B Y1 42.08(15) . . ? N2B Cu1B Y1 135.4(3) . . ? N1B Cu1B Y1 136.2(2) . . ? C4B O1B Cu1B 121.5(5) . . ? C4B O1B Y1 116.5(5) . . ? Cu1B O1B Y1 102.4(2) . . ? C3B O2B Y1 117.9(5) . . ? C1B O3B C5B 116.4(8) . . ? C14B O4B Cu1B 120.3(5) . . ? C14B O4B Y1 119.0(5) . . ? Cu1B O4B Y1 104.6(2) . . ? C13B O5B Y1 117.8(6) . . ? C11B O6B C10B 119.1(9) . . ? C6B N1B C7B 113.7(10) . . ? C6B N1B C15B 104.4(9) . . ? C7B N1B C15B 106.8(8) . . ? C6B N1B Cu1B 116.7(6) . . ? C7B N1B Cu1B 108.6(6) . . ? C15B N1B Cu1B 105.8(6) . . ? C9B N2B C8B 116.8(10) . . ? C9B N2B C16B 103.3(10) . . ? C8B N2B C16B 104.6(9) . . ? C9B N2B Cu1B 118.8(8) . . ? C8B N2B Cu1B 107.9(6) . . ? C16B N2B Cu1B 103.5(8) . . ? O3B C1B C2B 126.1(9) . . ? O3B C1B H1B 116.9 . . ? C2B C1B H1B 116.9 . . ? C1B C2B C3B 120.0(9) . . ? C1B C2B H2B 120.0 . . ? C3B C2B H2B 120.0 . . ? O2B C3B C4B 120.9(8) . . ? O2B C3B C2B 127.5(8) . . ? C4B C3B C2B 111.6(8) . . ? C5B C4B O1B 122.5(8) . . ? C5B C4B C3B 122.9(8) . . ? O1B C4B C3B 114.5(7) . . ? C4B C5B O3B 122.9(8) . . ? C4B C5B C6B 122.1(9) . . ? O3B C5B C6B 114.8(9) . . ? N1B C6B C5B 111.7(9) . . ? N1B C6B H6B1 109.3 . . ? C5B C6B H6B1 109.3 . . ? N1B C6B H6B2 109.3 . . ? C5B C6B H6B2 109.3 . . ? H6B1 C6B H6B2 107.9 . . ? N1B C7B C8B 113.4(10) . . ? N1B C7B H7B1 108.9 . . ? C8B C7B H7B1 108.9 . . ? N1B C7B H7B2 108.9 . . ? C8B C7B H7B2 108.9 . . ? H7B1 C7B H7B2 107.7 . . ? N2B C8B C7B 113.1(8) . . ? N2B C8B H8B1 109.0 . . ? C7B C8B H8B1 109.0 . . ? N2B C8B H8B2 109.0 . . ? C7B C8B H8B2 109.0 . . ? H8B1 C8B H8B2 107.8 . . ? N2B C9B C10B 116.7(10) . . ? N2B C9B H9B1 108.1 . . ? C10B C9B H9B1 108.1 . . ? N2B C9B H9B2 108.1 . . ? C10B C9B H9B2 108.1 . . ? H9B1 C9B H9B2 107.3 . . ? C14B C10B O6B 122.4(11) . . ? C14B C10B C9B 127.9(11) . . ? O6B C10B C9B 108.8(10) . . ? C12B C11B O6B 122.1(11) . . ? C12B C11B H11B 119.0 . . ? O6B C11B H11B 119.0 . . ? C11B C12B C13B 119.0(11) . . ? C11B C12B H12B 120.5 . . ? C13B C12B H12B 120.5 . . ? O5B C13B C12B 123.1(10) . . ? O5B C13B C14B 118.1(9) . . ? C12B C13B C14B 118.8(9) . . ? C10B C14B O4B 124.8(10) . . ? C10B C14B C13B 117.6(11) . . ? O4B C14B C13B 117.4(7) . . ? N1B C15B H15D 109.5 . . ? N1B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? N1B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? N2B C16B H16D 109.5 . . ? N2B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? N2B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? O18 Cl1 O13 147.9(10) . . ? O18 Cl1 O12 89.6(9) . . ? O13 Cl1 O12 113.9(6) . . ? O18 Cl1 O15 114.5(8) . . ? O13 Cl1 O15 57.3(7) . . ? O12 Cl1 O15 145.3(9) . . ? O18 Cl1 O14 37.8(8) . . ? O13 Cl1 O14 110.5(6) . . ? O12 Cl1 O14 111.4(6) . . ? O15 Cl1 O14 102.6(9) . . ? O18 Cl1 O17 111.2(8) . . ? O13 Cl1 O17 100.4(10) . . ? O12 Cl1 O17 37.6(9) . . ? O15 Cl1 O17 107.9(7) . . ? O14 Cl1 O17 145.0(9) . . ? O18 Cl1 O16 109.7(7) . . ? O13 Cl1 O16 54.8(7) . . ? O12 Cl1 O16 84.8(8) . . ? O15 Cl1 O16 108.0(7) . . ? O14 Cl1 O16 81.0(8) . . ? O17 Cl1 O16 105.1(7) . . ? O18 Cl1 O11 83.3(9) . . ? O13 Cl1 O11 107.8(6) . . ? O12 Cl1 O11 108.1(6) . . ? O15 Cl1 O11 54.5(7) . . ? O14 Cl1 O11 104.6(6) . . ? O17 Cl1 O11 80.2(9) . . ? O16 Cl1 O11 162.2(7) . . ? O23 Cl2 O26 100.5(10) . . ? O23 Cl2 O22 118.4(6) . . ? O26 Cl2 O22 58.6(8) . . ? O23 Cl2 O28 67.9(8) . . ? O26 Cl2 O28 112.0(8) . . ? O22 Cl2 O28 168.6(8) . . ? O23 Cl2 O21 117.3(6) . . ? O26 Cl2 O21 139.6(9) . . ? O22 Cl2 O21 109.3(6) . . ? O28 Cl2 O21 73.3(9) . . ? O23 Cl2 O25 51.5(7) . . ? O26 Cl2 O25 112.8(7) . . ? O22 Cl2 O25 82.1(7) . . ? O28 Cl2 O25 108.5(7) . . ? O21 Cl2 O25 102.0(8) . . ? O23 Cl2 O27 147.8(10) . . ? O26 Cl2 O27 110.2(7) . . ? O22 Cl2 O27 72.6(9) . . ? O28 Cl2 O27 107.4(7) . . ? O21 Cl2 O27 37.8(8) . . ? O25 Cl2 O27 105.6(7) . . ? O23 Cl2 O24 105.0(6) . . ? O26 Cl2 O24 53.2(8) . . ? O22 Cl2 O24 103.2(6) . . ? O28 Cl2 O24 65.5(8) . . ? O21 Cl2 O24 100.9(6) . . ? O25 Cl2 O24 153.2(8) . . ? O27 Cl2 O24 101.0(9) . . ? O32 Cl3 O34 113.5(7) . . ? O32 Cl3 O31 110.1(5) . . ? O34 Cl3 O31 112.1(5) . . ? O32 Cl3 O33 106.5(6) . . ? O34 Cl3 O33 109.7(6) . . ? O31 Cl3 O33 104.3(6) . . ? Cu1A O1WA H1W1 150(6) . . ? Cu1A O1WA H1W2 67(5) . . ? H1W1 O1WA H1W2 112(4) . . ? _diffrn_measured_fraction_theta_max 0.802 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.645 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.082 data_3 _database_code_depnum_ccdc_archive 'CCDC 901274' #TrackingRef '1-2-3.cif' _vfr_PLAT_973 ; PROBLEM: Large calc. positive residual density on Gd1 RESPONSE: The high max. difference electron density peak of 1.453 is located at a distance of 0.95 A from Gd1. ; _vfr_PLAT_420 ; PROBLEM: D-H without acceptor ...O1W-H1WB RESPONSE: A weak hydrogen bond (according to G. R. Desiraju and T. Steiner, The Weak Hydrogen Bond, Oxford University Press, 2001) involving the hydrogen atom H1WB and the symmetry related oxygen atom O23' (' = -x, y+0.5, -z+1.5) is present. The H1WB...O23' distance is 3.0(1)A) ; _vfr_PLAT_910 ; PROBLEM: Missing # of FCF Reflections Below Th(Min) ..... 37 RESPONSE: Data were collected with a CCD detector. The reflections in question were affected by the beam-stop. Only a small number of reflections are missing out of the total number of reflections observed. Resolution and completeness statistics #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.994 5875 5837 38 23.01 0.550 0.995 7803 7763 40 25.24 0.600 0.995 10144 10096 48 #----------------------------------------------------------- ACTA Min. Res. --- ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H64 Cl3 Co2 Gd N8 O26' _chemical_formula_weight 1502.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4681(5) _cell_length_b 24.7525(7) _cell_length_c 15.9297(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.196(4) _cell_angle_gamma 90.00 _cell_volume 5606.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 11336 _cell_measurement_theta_min 3.7336 _cell_measurement_theta_max 32.5319 _exptl_crystal_description parallelepipedal _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3044 _exptl_absorpt_coefficient_mu 1.991 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63556 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.4547 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42128 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_sigmaI/netI 0.1299 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 32.52 _reflns_number_total 18089 _reflns_number_gt 8902 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_structure_solution 'SIR2004 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farruggia, 1997)' _computing_publication_material 'PARST97 (Nardelli, 1995)' _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^ > 2\s(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. 36 restrains were used in the refinement, they are related to the distances between Cl-O and O...O atoms in the three perchlorate anions and to the O-H and H...H distances in the two water molecules. ; _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^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18089 _refine_ls_number_parameters 770 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1474 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1433 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.233737(18) 0.384932(10) 0.950365(18) 0.03275(8) Uani 1 1 d . . . Co1A Co 0.41787(5) 0.33954(3) 1.16740(5) 0.03369(17) Uani 1 1 d . . . Co1B Co -0.01059(5) 0.39062(3) 0.78029(5) 0.03415(16) Uani 1 1 d . . . O1A O 0.2895(2) 0.31808(13) 1.0643(2) 0.0362(8) Uani 1 1 d . . . O2A O 0.2187(3) 0.29234(14) 0.8873(2) 0.0430(9) Uani 1 1 d . . . O3A O 0.2047(3) 0.18374(16) 1.0717(3) 0.0570(11) Uani 1 1 d . . . O4A O 0.3863(3) 0.39965(13) 1.0664(2) 0.0391(9) Uani 1 1 d . . . O5A O 0.2697(3) 0.47864(15) 0.9724(3) 0.0465(10) Uani 1 1 d . . . O6A O 0.5376(3) 0.51674(17) 1.1338(3) 0.0587(12) Uani 1 1 d . . . N1A N 0.4123(3) 0.37530(18) 1.2887(3) 0.0436(11) Uani 1 1 d . . . N2A N 0.3748(3) 0.26162(18) 1.2368(3) 0.0410(11) Uani 1 1 d . . . N3A N 0.5141(3) 0.27885(18) 1.1636(3) 0.0421(11) Uani 1 1 d . . . N4A N 0.5639(3) 0.38728(19) 1.2311(3) 0.0441(11) Uani 1 1 d . . . C1A C 0.3666(5) 0.3378(3) 1.3317(4) 0.0545(16) Uani 1 1 d . . . H1A1 H 0.2989 0.3395 1.2986 0.065 Uiso 1 1 calc R . . H1A2 H 0.3811 0.3491 1.3941 0.065 Uiso 1 1 calc R . . C2A C 0.3992(5) 0.2804(3) 1.3316(4) 0.0524(16) Uani 1 1 d . . . H2A1 H 0.4668 0.2784 1.3653 0.063 Uiso 1 1 calc R . . H2A2 H 0.3697 0.2572 1.3616 0.063 Uiso 1 1 calc R . . C3A C 0.4347(4) 0.2162(2) 1.2325(4) 0.0495(15) Uani 1 1 d . . . H3A1 H 0.4025 0.1957 1.1769 0.059 Uiso 1 1 calc R . . H3A2 H 0.4463 0.1923 1.2840 0.059 Uiso 1 1 calc R . . C4A C 0.5270(4) 0.2367(2) 1.2341(4) 0.0523(16) Uani 1 1 d . . . H4A1 H 0.5637 0.2516 1.2939 0.063 Uiso 1 1 calc R . . H4A2 H 0.5620 0.2067 1.2238 0.063 Uiso 1 1 calc R . . C5A C 0.6076(4) 0.3033(3) 1.1815(4) 0.0533(16) Uani 1 1 d . . . H5A1 H 0.6059 0.3209 1.1265 0.064 Uiso 1 1 calc R . . H5A2 H 0.6548 0.2751 1.1974 0.064 Uiso 1 1 calc R . . C6A C 0.6340(4) 0.3438(3) 1.2576(4) 0.0561(17) Uani 1 1 d . . . H6A1 H 0.6360 0.3265 1.3130 0.067 Uiso 1 1 calc R . . H6A2 H 0.6958 0.3586 1.2693 0.067 Uiso 1 1 calc R . . C7A C 0.5656(5) 0.4173(3) 1.3128(4) 0.0565(17) Uani 1 1 d . . . H7A1 H 0.5396 0.4532 1.2948 0.068 Uiso 1 1 calc R . . H7A2 H 0.6301 0.4212 1.3565 0.068 Uiso 1 1 calc R . . C8A C 0.5094(4) 0.3876(3) 1.3561(4) 0.0564(16) Uani 1 1 d . . . H8A1 H 0.5411 0.3541 1.3823 0.068 Uiso 1 1 calc R . . H8A2 H 0.5056 0.4093 1.4053 0.068 Uiso 1 1 calc R . . C9A C 0.3563(5) 0.4257(2) 1.2649(4) 0.0587(17) Uani 1 1 d . . . H9A1 H 0.3844 0.4506 1.2368 0.088 Uiso 1 1 calc R . . H9A2 H 0.3550 0.4417 1.3193 0.088 Uiso 1 1 calc R . . H9A3 H 0.2933 0.4176 1.2232 0.088 Uiso 1 1 calc R . . C10A C 0.4793(4) 0.2534(3) 1.0721(4) 0.0554(16) Uani 1 1 d . . . H10A H 0.4188 0.2375 1.0591 0.083 Uiso 1 1 calc R . . H10B H 0.5227 0.2259 1.0711 0.083 Uiso 1 1 calc R . . H10C H 0.4740 0.2804 1.0270 0.083 Uiso 1 1 calc R . . C11A C 0.2761(4) 0.2441(2) 1.1980(4) 0.0429(13) Uani 1 1 d . . . H11A H 0.2371 0.2718 1.2083 0.051 Uiso 1 1 calc R . . H11B H 0.2696 0.2115 1.2288 0.051 Uiso 1 1 calc R . . C12A C 0.2432(4) 0.2335(2) 1.0993(4) 0.0399(13) Uani 1 1 d . . . C13A C 0.2507(3) 0.2696(2) 1.0389(4) 0.0340(12) Uani 1 1 d . . . C14A C 0.2150(4) 0.2573(2) 0.9424(4) 0.0379(13) Uani 1 1 d . . . C15A C 0.1758(5) 0.2047(2) 0.9176(5) 0.0575(17) Uani 1 1 d . . . H15A H 0.1524 0.1936 0.8569 0.069 Uiso 1 1 calc R . . C16A C 0.1731(5) 0.1711(3) 0.9831(5) 0.068(2) Uani 1 1 d . . . H16A H 0.1475 0.1369 0.9655 0.082 Uiso 1 1 calc R . . C17A C 0.5849(4) 0.4251(3) 1.1698(4) 0.0502(15) Uani 1 1 d . . . H17A H 0.5956 0.4046 1.1229 0.060 Uiso 1 1 calc R . . H17B H 0.6423 0.4446 1.2047 0.060 Uiso 1 1 calc R . . C18A C 0.5081(4) 0.4646(2) 1.1255(4) 0.0458(14) Uani 1 1 d . . . C19A C 0.4180(4) 0.4508(2) 1.0756(4) 0.0397(13) Uani 1 1 d . . . C20A C 0.3509(4) 0.4920(2) 1.0257(4) 0.0404(13) Uani 1 1 d . . . C21A C 0.3851(5) 0.5459(2) 1.0408(4) 0.0534(16) Uani 1 1 d . . . H21A H 0.3448 0.5745 1.0135 0.064 Uiso 1 1 calc R . . C22A C 0.4752(5) 0.5556(3) 1.0942(5) 0.0608(18) Uani 1 1 d . . . H22A H 0.4954 0.5913 1.1042 0.073 Uiso 1 1 calc R . . O1B O 0.1280(2) 0.41602(14) 0.8054(2) 0.0350(8) Uani 1 1 d . . . O2B O 0.3085(3) 0.39072(15) 0.8440(3) 0.0437(9) Uani 1 1 d . . . O3B O 0.1607(3) 0.47125(16) 0.6108(3) 0.0560(11) Uani 1 1 d . . . O4B O 0.0742(2) 0.36300(14) 0.9101(2) 0.0342(8) Uani 1 1 d . . . O5B O 0.1761(3) 0.40846(16) 1.0697(3) 0.0472(10) Uani 1 1 d . . . O6B O -0.0490(3) 0.31612(17) 1.0454(3) 0.0611(13) Uani 1 1 d . . . N1B N -0.1035(3) 0.45077(18) 0.7984(3) 0.0466(12) Uani 1 1 d . . . N2B N -0.0448(3) 0.44388(19) 0.6473(3) 0.0464(12) Uani 1 1 d . . . N3B N -0.0471(4) 0.33109(18) 0.6729(3) 0.0482(12) Uani 1 1 d . . . N4B N -0.1244(3) 0.33655(19) 0.8115(4) 0.0485(12) Uani 1 1 d . . . C1B C -0.1177(5) 0.4958(3) 0.7333(4) 0.0590(17) Uani 1 1 d . . . H1B1 H -0.0643 0.5201 0.7562 0.071 Uiso 1 1 calc R . . H1B2 H -0.1735 0.5159 0.7277 0.071 Uiso 1 1 calc R . . C2B C -0.1288(4) 0.4748(3) 0.6410(4) 0.0598(18) Uani 1 1 d . . . H2B1 H -0.1839 0.4518 0.6168 0.072 Uiso 1 1 calc R . . H2B2 H -0.1380 0.5049 0.5993 0.072 Uiso 1 1 calc R . . C3B C -0.0658(5) 0.4079(3) 0.5686(4) 0.0633(18) Uani 1 1 d . . . H3B1 H -0.0086 0.4006 0.5593 0.076 Uiso 1 1 calc R . . H3B2 H -0.1101 0.4253 0.5141 0.076 Uiso 1 1 calc R . . C4B C -0.1060(5) 0.3567(3) 0.5839(4) 0.0620(18) Uani 1 1 d . . . H4B1 H -0.1123 0.3318 0.5348 0.074 Uiso 1 1 calc R . . H4B2 H -0.1684 0.3634 0.5823 0.074 Uiso 1 1 calc R . . C5B C -0.0988(5) 0.2855(3) 0.6921(5) 0.0595(18) Uani 1 1 d . . . H5B1 H -0.0547 0.2620 0.7377 0.071 Uiso 1 1 calc R . . H5B2 H -0.1298 0.2646 0.6369 0.071 Uiso 1 1 calc R . . C6B C -0.1706(5) 0.3057(3) 0.7259(5) 0.0646(19) Uani 1 1 d . . . H6B1 H -0.2154 0.3287 0.6799 0.077 Uiso 1 1 calc R . . H6B2 H -0.2046 0.2754 0.7367 0.077 Uiso 1 1 calc R . . C7B C -0.1891(4) 0.3736(3) 0.8299(5) 0.0595(18) Uani 1 1 d . . . H7B1 H -0.1665 0.3803 0.8951 0.071 Uiso 1 1 calc R . . H7B2 H -0.2508 0.3570 0.8105 0.071 Uiso 1 1 calc R . . C8B C -0.1968(4) 0.4262(3) 0.7802(5) 0.0622(18) Uani 1 1 d . . . H8B1 H -0.2292 0.4201 0.7150 0.075 Uiso 1 1 calc R . . H8B2 H -0.2341 0.4513 0.7987 0.075 Uiso 1 1 calc R . . C9B C -0.0630(5) 0.4732(2) 0.8926(4) 0.0618(18) Uani 1 1 d . . . H9B1 H -0.0532 0.4445 0.9359 0.093 Uiso 1 1 calc R . . H9B2 H -0.1056 0.4993 0.8996 0.093 Uiso 1 1 calc R . . H9B3 H -0.0040 0.4903 0.9030 0.093 Uiso 1 1 calc R . . C11B C 0.0270(4) 0.4839(2) 0.6483(4) 0.0489(15) Uani 1 1 d . . . H11C H 0.0068 0.5009 0.5888 0.059 Uiso 1 1 calc R . . H11D H 0.0320 0.5118 0.6927 0.059 Uiso 1 1 calc R . . C12B C 0.1202(4) 0.4592(2) 0.6710(4) 0.0423(13) Uani 1 1 d . . . C13B C 0.1668(4) 0.4295(2) 0.7470(3) 0.0349(12) Uani 1 1 d . . . C14B C 0.2631(4) 0.4144(2) 0.7698(4) 0.0379(13) Uani 1 1 d . . . C15B C 0.2997(4) 0.4271(2) 0.7025(4) 0.0485(15) Uani 1 1 d . . . H15B H 0.3601 0.4161 0.7110 0.058 Uiso 1 1 calc R . . C16B C 0.2483(5) 0.4545(3) 0.6280(5) 0.0584(17) Uani 1 1 d . . . H16B H 0.2743 0.4625 0.5859 0.070 Uiso 1 1 calc R . . C17B C -0.0863(4) 0.2972(2) 0.8871(4) 0.0506(16) Uani 1 1 d . . . H17C H -0.1379 0.2796 0.8965 0.061 Uiso 1 1 calc R . . H17D H -0.0509 0.2697 0.8711 0.061 Uiso 1 1 calc R . . C18B C -0.0246(4) 0.3241(2) 0.9725(4) 0.0473(15) Uani 1 1 d . . . C19B C 0.0500(4) 0.35466(19) 0.9808(4) 0.0352(12) Uani 1 1 d . . . C20B C 0.1066(4) 0.3802(2) 1.0655(4) 0.0411(13) Uani 1 1 d . . . C21B C 0.0774(5) 0.3709(3) 1.1394(4) 0.0551(17) Uani 1 1 d . . . H21B H 0.1103 0.3862 1.1965 0.066 Uiso 1 1 calc R . . C22B C 0.0026(6) 0.3401(3) 1.1249(5) 0.066(2) Uani 1 1 d . . . H22B H -0.0153 0.3347 1.1736 0.079 Uiso 1 1 calc R . . Cl1 Cl 0.68196(12) 0.28692(9) 0.98098(12) 0.0676(5) Uani 1 1 d D . . O11 O 0.7174(4) 0.2795(4) 0.9142(4) 0.154(3) Uani 1 1 d D . . O12 O 0.6659(5) 0.2365(2) 1.0103(6) 0.153(3) Uani 1 1 d D . . O13 O 0.5946(3) 0.3138(2) 0.9463(4) 0.0937(17) Uani 1 1 d D . . O14 O 0.7442(4) 0.3152(3) 1.0553(4) 0.143(3) Uani 1 1 d D . . Cl2 Cl -0.07484(14) 0.13259(7) 0.83008(13) 0.0669(5) Uani 1 1 d D . . O21 O 0.0069(3) 0.11144(19) 0.8225(4) 0.0872(16) Uani 1 1 d D . . O22 O -0.0464(6) 0.1637(3) 0.9122(4) 0.140(3) Uani 1 1 d D . . O23 O -0.1186(5) 0.1686(3) 0.7588(4) 0.137(3) Uani 1 1 d D . . O24 O -0.1344(4) 0.0917(2) 0.8343(5) 0.111(2) Uani 1 1 d D . . Cl3 Cl 0.52670(16) 0.08596(8) 1.13075(14) 0.0758(5) Uani 1 1 d D . . O31 O 0.4403(4) 0.1099(3) 1.0787(4) 0.117(2) Uani 1 1 d D . . O32 O 0.5965(5) 0.1144(3) 1.1155(6) 0.175(4) Uani 1 1 d D . . O33 O 0.5439(6) 0.0877(5) 1.2216(4) 0.204(5) Uani 1 1 d D . . O34 O 0.5271(8) 0.0346(2) 1.1029(7) 0.223(5) Uani 1 1 d D . . O1W O 0.1260(7) 0.5593(4) 0.9034(10) 0.216(5) Uani 1 1 d D . . H1WA H 0.155(10) 0.530(3) 0.922(10) 0.259 Uiso 1 1 d D . . H1WB H 0.146(12) 0.571(6) 0.865(9) 0.259 Uiso 1 1 d D . . O2W O 0.3346(5) 0.0094(6) 0.9712(7) 0.211(5) Uani 1 1 d D . . H2WA H 0.377(8) 0.031(5) 1.007(9) 0.254 Uiso 1 1 d D . . H2WB H 0.361(9) -0.008(5) 0.943(9) 0.254 Uiso 1 1 d D . . C10B C 0.0410(5) 0.3100(3) 0.6686(5) 0.0584(17) Uani 1 1 d . . . H10D H 0.0752 0.3392 0.6564 0.088 Uiso 1 1 calc R . . H10E H 0.0258 0.2836 0.6207 0.088 Uiso 1 1 calc R . . H10F H 0.0790 0.2935 0.7259 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02752(13) 0.03643(14) 0.03129(14) 0.00265(12) 0.00836(10) -0.00162(13) Co1A 0.0275(4) 0.0420(4) 0.0291(4) 0.0005(3) 0.0086(3) 0.0012(3) Co1B 0.0281(4) 0.0362(4) 0.0364(4) -0.0022(3) 0.0108(3) 0.0000(3) O1A 0.032(2) 0.036(2) 0.034(2) 0.0044(15) 0.0060(17) -0.0062(15) O2A 0.049(2) 0.045(2) 0.036(2) -0.0008(18) 0.017(2) 0.0024(19) O3A 0.057(3) 0.046(2) 0.059(3) 0.007(2) 0.014(2) -0.013(2) O4A 0.033(2) 0.038(2) 0.038(2) 0.0047(16) 0.0062(18) -0.0047(16) O5A 0.040(2) 0.042(2) 0.046(3) 0.0030(18) 0.0047(19) -0.0014(18) O6A 0.058(3) 0.052(3) 0.058(3) 0.000(2) 0.014(2) -0.024(2) N1A 0.040(3) 0.055(3) 0.035(3) -0.007(2) 0.015(2) -0.001(2) N2A 0.038(3) 0.049(3) 0.030(3) 0.008(2) 0.007(2) 0.001(2) N3A 0.033(3) 0.052(3) 0.039(3) 0.003(2) 0.011(2) 0.008(2) N4A 0.033(2) 0.059(3) 0.033(3) 0.003(2) 0.006(2) -0.005(2) C1A 0.049(4) 0.081(5) 0.036(4) -0.014(3) 0.020(3) -0.013(4) C2A 0.054(4) 0.067(4) 0.035(3) 0.007(3) 0.016(3) -0.010(3) C3A 0.051(4) 0.049(4) 0.042(4) 0.009(3) 0.011(3) 0.009(3) C4A 0.043(4) 0.058(4) 0.045(4) 0.008(3) 0.006(3) 0.010(3) C5A 0.031(3) 0.068(4) 0.062(4) 0.007(3) 0.019(3) 0.011(3) C6A 0.025(3) 0.079(5) 0.050(4) 0.009(3) -0.001(3) -0.002(3) C7A 0.051(4) 0.064(4) 0.051(4) -0.010(3) 0.016(3) -0.015(3) C8A 0.047(4) 0.079(5) 0.034(3) -0.012(3) 0.006(3) -0.006(4) C9A 0.063(4) 0.062(4) 0.050(4) -0.010(3) 0.021(4) 0.007(4) C10A 0.045(4) 0.071(4) 0.053(4) -0.005(3) 0.022(3) 0.009(3) C11A 0.041(3) 0.047(3) 0.040(3) 0.010(3) 0.016(3) -0.006(3) C12A 0.029(3) 0.043(3) 0.044(3) 0.006(3) 0.011(3) -0.007(2) C13A 0.024(3) 0.038(3) 0.037(3) 0.001(2) 0.008(2) 0.000(2) C14A 0.032(3) 0.041(3) 0.041(3) 0.003(3) 0.015(3) 0.002(2) C15A 0.073(5) 0.040(3) 0.050(4) -0.006(3) 0.014(4) -0.009(3) C16A 0.076(5) 0.041(4) 0.074(5) -0.009(4) 0.014(4) -0.020(3) C17A 0.033(3) 0.069(4) 0.042(4) -0.001(3) 0.008(3) -0.015(3) C18A 0.044(3) 0.049(3) 0.038(3) -0.001(3) 0.009(3) -0.016(3) C19A 0.039(3) 0.043(3) 0.032(3) -0.001(2) 0.008(3) -0.013(3) C20A 0.044(4) 0.044(3) 0.028(3) 0.000(2) 0.009(3) -0.008(3) C21A 0.070(5) 0.039(3) 0.049(4) 0.002(3) 0.021(4) -0.009(3) C22A 0.070(5) 0.046(4) 0.063(5) -0.005(3) 0.022(4) -0.022(4) O1B 0.0292(19) 0.045(2) 0.031(2) 0.0084(16) 0.0124(17) -0.0029(16) O2B 0.033(2) 0.053(2) 0.048(2) 0.006(2) 0.0190(19) -0.0011(19) O3B 0.070(3) 0.063(3) 0.042(3) 0.011(2) 0.029(2) -0.006(2) O4B 0.0222(18) 0.053(2) 0.0261(19) 0.0070(16) 0.0081(16) -0.0034(16) O5B 0.043(2) 0.056(2) 0.043(2) -0.0119(19) 0.016(2) -0.002(2) O6B 0.077(3) 0.054(3) 0.081(4) 0.012(2) 0.061(3) 0.002(2) N1B 0.037(3) 0.044(3) 0.059(3) -0.001(2) 0.020(3) 0.005(2) N2B 0.044(3) 0.050(3) 0.037(3) 0.002(2) 0.007(2) 0.003(2) N3B 0.051(3) 0.040(3) 0.054(3) -0.013(2) 0.022(3) -0.012(2) N4B 0.029(3) 0.052(3) 0.067(4) -0.003(3) 0.021(3) -0.006(2) C1B 0.052(4) 0.055(4) 0.067(5) 0.010(3) 0.021(4) 0.021(3) C2B 0.041(4) 0.067(4) 0.057(4) 0.017(3) 0.005(3) 0.013(3) C3B 0.064(5) 0.080(5) 0.037(4) 0.001(3) 0.010(3) -0.004(4) C4B 0.050(4) 0.084(5) 0.041(4) -0.013(3) 0.006(3) -0.007(4) C5B 0.051(4) 0.056(4) 0.067(5) -0.026(3) 0.019(4) -0.019(3) C6B 0.049(4) 0.059(4) 0.085(5) -0.011(4) 0.026(4) -0.025(3) C7B 0.034(3) 0.071(5) 0.077(5) 0.005(4) 0.027(3) 0.005(3) C8B 0.039(4) 0.066(4) 0.082(5) -0.006(4) 0.025(4) 0.010(3) C9B 0.070(5) 0.048(4) 0.070(5) -0.001(3) 0.030(4) 0.016(3) C11B 0.055(4) 0.048(3) 0.038(3) 0.010(3) 0.011(3) 0.002(3) C12B 0.045(3) 0.043(3) 0.039(3) 0.005(3) 0.017(3) -0.005(3) C13B 0.035(3) 0.038(3) 0.030(3) 0.000(2) 0.010(2) -0.009(2) C14B 0.037(3) 0.036(3) 0.042(3) -0.008(2) 0.017(3) -0.012(2) C15B 0.050(4) 0.054(4) 0.052(4) -0.011(3) 0.031(3) -0.016(3) C16B 0.065(5) 0.068(4) 0.051(4) 0.002(3) 0.033(4) -0.015(4) C17B 0.046(4) 0.047(3) 0.069(5) -0.005(3) 0.034(4) -0.009(3) C18B 0.048(4) 0.040(3) 0.068(4) 0.013(3) 0.038(4) 0.009(3) C19B 0.037(3) 0.031(3) 0.045(3) 0.010(2) 0.024(3) 0.009(2) C20B 0.048(3) 0.033(3) 0.049(4) 0.010(3) 0.026(3) 0.016(3) C21B 0.074(5) 0.056(4) 0.046(4) -0.003(3) 0.034(4) 0.009(3) C22B 0.096(6) 0.059(4) 0.074(5) 0.021(4) 0.067(5) 0.023(4) Cl1 0.0402(9) 0.1156(16) 0.0434(10) 0.0079(9) 0.0126(8) -0.0080(10) O11 0.071(4) 0.334(11) 0.072(4) -0.015(5) 0.044(4) -0.051(5) O12 0.163(7) 0.124(6) 0.223(9) 0.070(6) 0.131(7) 0.041(5) O13 0.057(3) 0.111(4) 0.081(4) 0.016(3) -0.007(3) 0.009(3) O14 0.066(4) 0.233(9) 0.092(5) -0.064(5) -0.011(4) -0.006(5) Cl2 0.0806(13) 0.0616(10) 0.0706(13) 0.0147(9) 0.0428(11) 0.0123(10) O21 0.072(4) 0.081(4) 0.116(5) -0.019(3) 0.045(3) -0.008(3) O22 0.218(9) 0.132(6) 0.105(5) -0.025(4) 0.101(6) -0.005(5) O23 0.154(7) 0.146(6) 0.132(6) 0.093(5) 0.078(5) 0.066(5) O24 0.089(4) 0.078(4) 0.186(7) 0.023(4) 0.074(5) 0.001(3) Cl3 0.0880(15) 0.0726(13) 0.0661(13) 0.0010(10) 0.0296(12) 0.0057(11) O31 0.081(4) 0.145(6) 0.100(5) 0.012(4) 0.009(4) 0.017(4) O32 0.100(6) 0.240(10) 0.195(9) 0.081(7) 0.068(6) -0.004(6) O33 0.190(9) 0.370(14) 0.058(5) 0.033(6) 0.056(5) 0.054(9) O34 0.281(13) 0.083(5) 0.227(10) -0.048(6) 0.017(9) 0.042(6) O1W 0.123(7) 0.165(9) 0.375(17) 0.125(9) 0.114(9) 0.070(6) O2W 0.090(6) 0.412(17) 0.146(8) -0.108(9) 0.062(6) -0.087(8) C10B 0.060(4) 0.055(4) 0.064(5) -0.018(3) 0.028(4) 0.000(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1A 2.354(3) . ? Gd1 O4B 2.356(3) . ? Gd1 O1B 2.372(3) . ? Gd1 O5A 2.379(4) . ? Gd1 O4A 2.384(4) . ? Gd1 O2B 2.403(3) . ? Gd1 O5B 2.466(4) . ? Gd1 O2A 2.476(4) . ? Co1A O1A 2.087(3) . ? Co1A O4A 2.102(3) . ? Co1A N3A 2.133(4) . ? Co1A N1A 2.158(4) . ? Co1A N4A 2.392(5) . ? Co1A N2A 2.443(4) . ? Co1B O4B 2.080(3) . ? Co1B O1B 2.115(3) . ? Co1B N3B 2.158(4) . ? Co1B N1B 2.166(4) . ? Co1B N2B 2.371(5) . ? Co1B N4B 2.413(4) . ? O1A C13A 1.332(6) . ? O2A C14A 1.251(6) . ? O3A C16A 1.336(8) . ? O3A C12A 1.363(6) . ? O4A C19A 1.346(6) . ? O5A C20A 1.251(6) . ? O6A C22A 1.333(8) . ? O6A C18A 1.357(6) . ? N1A C9A 1.481(7) . ? N1A C1A 1.487(7) . ? N1A C8A 1.493(7) . ? N2A C11A 1.469(7) . ? N2A C3A 1.476(7) . ? N2A C2A 1.480(7) . ? N3A C10A 1.480(7) . ? N3A C5A 1.488(7) . ? N3A C4A 1.488(7) . ? N4A C6A 1.467(7) . ? N4A C17A 1.479(7) . ? N4A C7A 1.489(7) . ? C1A C2A 1.507(8) . ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A C4A 1.506(8) . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? C5A C6A 1.500(8) . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C7A C8A 1.499(8) . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C10A H10A 0.9600 . ? C10A H10B 0.9600 . ? C10A H10C 0.9600 . ? C11A C12A 1.472(7) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C12A C13A 1.351(7) . ? C13A C14A 1.446(7) . ? C14A C15A 1.426(8) . ? C15A C16A 1.347(9) . ? C15A H15A 0.9300 . ? C16A H16A 0.9300 . ? C17A C18A 1.485(8) . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C18A C19A 1.348(7) . ? C19A C20A 1.447(7) . ? C20A C21A 1.422(7) . ? C21A C22A 1.338(9) . ? C21A H21A 0.9300 . ? C22A H22A 0.9300 . ? O1B C13B 1.333(6) . ? O2B C14B 1.257(6) . ? O3B C16B 1.338(8) . ? O3B C12B 1.369(6) . ? O4B C19B 1.335(6) . ? O5B C20B 1.263(7) . ? O6B C22B 1.340(9) . ? O6B C18B 1.369(6) . ? N1B C1B 1.478(7) . ? N1B C8B 1.485(7) . ? N1B C9B 1.487(8) . ? N2B C3B 1.466(7) . ? N2B C2B 1.478(7) . ? N2B C11B 1.483(7) . ? N3B C5B 1.483(7) . ? N3B C10B 1.486(7) . ? N3B C4B 1.491(8) . ? N4B C7B 1.470(7) . ? N4B C6B 1.478(8) . ? N4B C17B 1.480(7) . ? C1B C2B 1.504(8) . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B C4B 1.475(9) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? C5B C6B 1.497(8) . ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? C7B C8B 1.506(8) . ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? C11B C12B 1.475(8) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12B C13B 1.356(7) . ? C13B C14B 1.436(7) . ? C14B C15B 1.432(7) . ? C15B C16B 1.325(8) . ? C15B H15B 0.9300 . ? C16B H16B 0.9300 . ? C17B C18B 1.477(8) . ? C17B H17C 0.9700 . ? C17B H17D 0.9700 . ? C18B C19B 1.342(7) . ? C19B C20B 1.433(8) . ? C20B C21B 1.436(8) . ? C21B C22B 1.327(9) . ? C21B H21B 0.9300 . ? C22B H22B 0.9300 . ? Cl1 O14 1.386(5) . ? Cl1 O11 1.388(5) . ? Cl1 O12 1.389(5) . ? Cl1 O13 1.410(5) . ? Cl2 O24 1.388(5) . ? Cl2 O23 1.391(5) . ? Cl2 O21 1.417(5) . ? Cl2 O22 1.430(5) . ? Cl3 O34 1.348(6) . ? Cl3 O33 1.365(5) . ? Cl3 O32 1.388(6) . ? Cl3 O31 1.396(5) . ? O1W H1WA 0.85(2) . ? O1W H1WB 0.85(2) . ? O2W H2WA 0.85(2) . ? O2W H2WB 0.84(2) . ? C10B H10D 0.9600 . ? C10B H10E 0.9600 . ? C10B H10F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Gd1 O4B 94.28(11) . . ? O1A Gd1 O1B 151.80(12) . . ? O4B Gd1 O1B 64.06(11) . . ? O1A Gd1 O5A 125.31(12) . . ? O4B Gd1 O5A 115.09(13) . . ? O1B Gd1 O5A 81.91(13) . . ? O1A Gd1 O4A 63.85(11) . . ? O4B Gd1 O4A 149.02(12) . . ? O1B Gd1 O4A 142.94(11) . . ? O5A Gd1 O4A 68.52(12) . . ? O1A Gd1 O2B 116.96(12) . . ? O4B Gd1 O2B 124.41(12) . . ? O1B Gd1 O2B 68.46(12) . . ? O5A Gd1 O2B 84.06(13) . . ? O4A Gd1 O2B 86.19(13) . . ? O1A Gd1 O5B 72.89(12) . . ? O4B Gd1 O5B 66.84(12) . . ? O1B Gd1 O5B 110.73(12) . . ? O5A Gd1 O5B 77.90(13) . . ? O4A Gd1 O5B 85.06(13) . . ? O2B Gd1 O5B 161.81(13) . . ? O1A Gd1 O2A 67.01(12) . . ? O4B Gd1 O2A 75.82(12) . . ? O1B Gd1 O2A 89.22(12) . . ? O5A Gd1 O2A 160.31(12) . . ? O4A Gd1 O2A 111.25(12) . . ? O2B Gd1 O2A 76.33(12) . . ? O5B Gd1 O2A 121.76(12) . . ? O1A Co1A O4A 73.48(13) . . ? O1A Co1A N3A 104.87(16) . . ? O4A Co1A N3A 115.52(16) . . ? O1A Co1A N1A 116.66(16) . . ? O4A Co1A N1A 108.41(16) . . ? N3A Co1A N1A 126.08(18) . . ? O1A Co1A N4A 155.02(14) . . ? O4A Co1A N4A 82.59(15) . . ? N3A Co1A N4A 78.88(17) . . ? N1A Co1A N4A 77.35(17) . . ? O1A Co1A N2A 79.10(14) . . ? O4A Co1A N2A 151.95(15) . . ? N3A Co1A N2A 76.99(16) . . ? N1A Co1A N2A 78.71(16) . . ? N4A Co1A N2A 125.32(15) . . ? O4B Co1B O1B 73.44(13) . . ? O4B Co1B N3B 115.42(17) . . ? O1B Co1B N3B 106.37(16) . . ? O4B Co1B N1B 106.56(17) . . ? O1B Co1B N1B 116.53(16) . . ? N3B Co1B N1B 126.51(19) . . ? O4B Co1B N2B 154.46(15) . . ? O1B Co1B N2B 81.73(15) . . ? N3B Co1B N2B 76.98(18) . . ? N1B Co1B N2B 79.10(18) . . ? O4B Co1B N4B 80.71(15) . . ? O1B Co1B N4B 153.24(15) . . ? N3B Co1B N4B 78.47(17) . . ? N1B Co1B N4B 77.17(17) . . ? N2B Co1B N4B 124.62(17) . . ? C13A O1A Co1A 130.0(3) . . ? C13A O1A Gd1 114.6(3) . . ? Co1A O1A Gd1 111.97(14) . . ? C14A O2A Gd1 112.3(3) . . ? C16A O3A C12A 118.9(5) . . ? C19A O4A Co1A 128.2(3) . . ? C19A O4A Gd1 115.8(3) . . ? Co1A O4A Gd1 110.23(14) . . ? C20A O5A Gd1 118.1(3) . . ? C22A O6A C18A 119.2(5) . . ? C9A N1A C1A 107.9(5) . . ? C9A N1A C8A 109.5(5) . . ? C1A N1A C8A 108.8(5) . . ? C9A N1A Co1A 110.0(3) . . ? C1A N1A Co1A 110.5(3) . . ? C8A N1A Co1A 110.2(3) . . ? C11A N2A C3A 108.8(4) . . ? C11A N2A C2A 109.2(4) . . ? C3A N2A C2A 112.0(5) . . ? C11A N2A Co1A 117.8(3) . . ? C3A N2A Co1A 106.9(3) . . ? C2A N2A Co1A 102.0(3) . . ? C10A N3A C5A 108.1(4) . . ? C10A N3A C4A 109.5(5) . . ? C5A N3A C4A 108.0(5) . . ? C10A N3A Co1A 109.9(3) . . ? C5A N3A Co1A 110.1(3) . . ? C4A N3A Co1A 111.1(3) . . ? C6A N4A C17A 108.9(4) . . ? C6A N4A C7A 111.0(5) . . ? C17A N4A C7A 109.1(5) . . ? C6A N4A Co1A 103.1(3) . . ? C17A N4A Co1A 116.7(3) . . ? C7A N4A Co1A 107.9(3) . . ? N1A C1A C2A 111.6(5) . . ? N1A C1A H1A1 109.3 . . ? C2A C1A H1A1 109.3 . . ? N1A C1A H1A2 109.3 . . ? C2A C1A H1A2 109.3 . . ? H1A1 C1A H1A2 108.0 . . ? N2A C2A C1A 110.2(5) . . ? N2A C2A H2A1 109.6 . . ? C1A C2A H2A1 109.6 . . ? N2A C2A H2A2 109.6 . . ? C1A C2A H2A2 109.6 . . ? H2A1 C2A H2A2 108.1 . . ? N2A C3A C4A 110.6(5) . . ? N2A C3A H3A1 109.5 . . ? C4A C3A H3A1 109.5 . . ? N2A C3A H3A2 109.5 . . ? C4A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 108.1 . . ? N3A C4A C3A 112.3(5) . . ? N3A C4A H4A1 109.2 . . ? C3A C4A H4A1 109.2 . . ? N3A C4A H4A2 109.2 . . ? C3A C4A H4A2 109.2 . . ? H4A1 C4A H4A2 107.9 . . ? N3A C5A C6A 111.2(5) . . ? N3A C5A H5A1 109.4 . . ? C6A C5A H5A1 109.4 . . ? N3A C5A H5A2 109.4 . . ? C6A C5A H5A2 109.4 . . ? H5A1 C5A H5A2 108.0 . . ? N4A C6A C5A 108.8(5) . . ? N4A C6A H6A1 109.9 . . ? C5A C6A H6A1 109.9 . . ? N4A C6A H6A2 109.9 . . ? C5A C6A H6A2 109.9 . . ? H6A1 C6A H6A2 108.3 . . ? N4A C7A C8A 110.1(5) . . ? N4A C7A H7A1 109.6 . . ? C8A C7A H7A1 109.6 . . ? N4A C7A H7A2 109.6 . . ? C8A C7A H7A2 109.6 . . ? H7A1 C7A H7A2 108.2 . . ? N1A C8A C7A 111.7(5) . . ? N1A C8A H8A1 109.3 . . ? C7A C8A H8A1 109.3 . . ? N1A C8A H8A2 109.3 . . ? C7A C8A H8A2 109.3 . . ? H8A1 C8A H8A2 107.9 . . ? N1A C9A H9A1 109.5 . . ? N1A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? N1A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? N3A C10A H10A 109.5 . . ? N3A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? N3A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? N2A C11A C12A 111.5(4) . . ? N2A C11A H11A 109.3 . . ? C12A C11A H11A 109.3 . . ? N2A C11A H11B 109.3 . . ? C12A C11A H11B 109.3 . . ? H11A C11A H11B 108.0 . . ? C13A C12A O3A 121.1(5) . . ? C13A C12A C11A 123.5(5) . . ? O3A C12A C11A 115.4(5) . . ? O1A C13A C12A 122.4(5) . . ? O1A C13A C14A 116.7(4) . . ? C12A C13A C14A 120.9(5) . . ? O2A C14A C15A 124.8(5) . . ? O2A C14A C13A 119.8(5) . . ? C15A C14A C13A 115.4(5) . . ? C16A C15A C14A 119.2(6) . . ? C16A C15A H15A 120.4 . . ? C14A C15A H15A 120.4 . . ? O3A C16A C15A 124.4(6) . . ? O3A C16A H16A 117.8 . . ? C15A C16A H16A 117.8 . . ? N4A C17A C18A 112.8(5) . . ? N4A C17A H17A 109.0 . . ? C18A C17A H17A 109.0 . . ? N4A C17A H17B 109.0 . . ? C18A C17A H17B 109.0 . . ? H17A C17A H17B 107.8 . . ? C19A C18A O6A 121.8(6) . . ? C19A C18A C17A 124.1(5) . . ? O6A C18A C17A 113.8(5) . . ? O4A C19A C18A 123.4(5) . . ? O4A C19A C20A 116.8(5) . . ? C18A C19A C20A 119.8(5) . . ? O5A C20A C21A 124.7(6) . . ? O5A C20A C19A 119.9(5) . . ? C21A C20A C19A 115.4(5) . . ? C22A C21A C20A 120.1(6) . . ? C22A C21A H21A 120.0 . . ? C20A C21A H21A 120.0 . . ? O6A C22A C21A 123.4(6) . . ? O6A C22A H22A 118.3 . . ? C21A C22A H22A 118.3 . . ? C13B O1B Co1B 130.1(3) . . ? C13B O1B Gd1 115.6(3) . . ? Co1B O1B Gd1 110.26(13) . . ? C14B O2B Gd1 116.4(3) . . ? C16B O3B C12B 119.6(5) . . ? C19B O4B Co1B 127.8(3) . . ? C19B O4B Gd1 114.7(3) . . ? Co1B O4B Gd1 112.19(13) . . ? C20B O5B Gd1 112.7(3) . . ? C22B O6B C18B 118.5(5) . . ? C1B N1B C8B 107.8(5) . . ? C1B N1B C9B 108.3(5) . . ? C8B N1B C9B 110.0(5) . . ? C1B N1B Co1B 110.4(3) . . ? C8B N1B Co1B 109.7(3) . . ? C9B N1B Co1B 110.7(4) . . ? C3B N2B C2B 111.3(5) . . ? C3B N2B C11B 109.2(5) . . ? C2B N2B C11B 106.8(5) . . ? C3B N2B Co1B 108.8(4) . . ? C2B N2B Co1B 103.3(3) . . ? C11B N2B Co1B 117.3(3) . . ? C5B N3B C10B 108.8(5) . . ? C5B N3B C4B 110.0(5) . . ? C10B N3B C4B 109.5(5) . . ? C5B N3B Co1B 110.5(4) . . ? C10B N3B Co1B 108.6(4) . . ? C4B N3B Co1B 109.6(4) . . ? C7B N4B C6B 112.7(5) . . ? C7B N4B C17B 109.3(5) . . ? C6B N4B C17B 107.7(5) . . ? C7B N4B Co1B 107.8(3) . . ? C6B N4B Co1B 102.9(3) . . ? C17B N4B Co1B 116.4(3) . . ? N1B C1B C2B 110.8(5) . . ? N1B C1B H1B1 109.5 . . ? C2B C1B H1B1 109.5 . . ? N1B C1B H1B2 109.5 . . ? C2B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 108.1 . . ? N2B C2B C1B 110.7(5) . . ? N2B C2B H2B1 109.5 . . ? C1B C2B H2B1 109.5 . . ? N2B C2B H2B2 109.5 . . ? C1B C2B H2B2 109.5 . . ? H2B1 C2B H2B2 108.1 . . ? N2B C3B C4B 110.3(5) . . ? N2B C3B H3B1 109.6 . . ? C4B C3B H3B1 109.6 . . ? N2B C3B H3B2 109.6 . . ? C4B C3B H3B2 109.6 . . ? H3B1 C3B H3B2 108.1 . . ? C3B C4B N3B 112.5(5) . . ? C3B C4B H4B1 109.1 . . ? N3B C4B H4B1 109.1 . . ? C3B C4B H4B2 109.1 . . ? N3B C4B H4B2 109.1 . . ? H4B1 C4B H4B2 107.8 . . ? N3B C5B C6B 110.9(5) . . ? N3B C5B H5B1 109.5 . . ? C6B C5B H5B1 109.5 . . ? N3B C5B H5B2 109.5 . . ? C6B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 108.1 . . ? N4B C6B C5B 110.3(5) . . ? N4B C6B H6B1 109.6 . . ? C5B C6B H6B1 109.6 . . ? N4B C6B H6B2 109.6 . . ? C5B C6B H6B2 109.6 . . ? H6B1 C6B H6B2 108.1 . . ? N4B C7B C8B 110.6(5) . . ? N4B C7B H7B1 109.5 . . ? C8B C7B H7B1 109.5 . . ? N4B C7B H7B2 109.5 . . ? C8B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 108.1 . . ? N1B C8B C7B 112.5(5) . . ? N1B C8B H8B1 109.1 . . ? C7B C8B H8B1 109.1 . . ? N1B C8B H8B2 109.1 . . ? C7B C8B H8B2 109.1 . . ? H8B1 C8B H8B2 107.8 . . ? N1B C9B H9B1 109.5 . . ? N1B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? N1B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C12B C11B N2B 112.3(5) . . ? C12B C11B H11C 109.1 . . ? N2B C11B H11C 109.1 . . ? C12B C11B H11D 109.1 . . ? N2B C11B H11D 109.1 . . ? H11C C11B H11D 107.9 . . ? C13B C12B O3B 121.0(5) . . ? C13B C12B C11B 124.7(5) . . ? O3B C12B C11B 114.2(5) . . ? O1B C13B C12B 122.1(5) . . ? O1B C13B C14B 117.8(5) . . ? C12B C13B C14B 120.0(5) . . ? O2B C14B C15B 124.6(5) . . ? O2B C14B C13B 119.9(5) . . ? C15B C14B C13B 115.5(5) . . ? C16B C15B C14B 120.5(6) . . ? C16B C15B H15B 119.7 . . ? C14B C15B H15B 119.7 . . ? C15B C16B O3B 123.0(5) . . ? C15B C16B H16B 118.5 . . ? O3B C16B H16B 118.5 . . ? C18B C17B N4B 111.0(5) . . ? C18B C17B H17C 109.4 . . ? N4B C17B H17C 109.4 . . ? C18B C17B H17D 109.4 . . ? N4B C17B H17D 109.4 . . ? H17C C17B H17D 108.0 . . ? C19B C18B O6B 120.8(6) . . ? C19B C18B C17B 124.3(5) . . ? O6B C18B C17B 115.0(5) . . ? O4B C19B C18B 121.4(5) . . ? O4B C19B C20B 117.1(5) . . ? C18B C19B C20B 121.5(5) . . ? O5B C20B C19B 119.1(5) . . ? O5B C20B C21B 125.5(6) . . ? C19B C20B C21B 115.4(5) . . ? C22B C21B C20B 118.9(6) . . ? C22B C21B H21B 120.5 . . ? C20B C21B H21B 120.5 . . ? C21B C22B O6B 124.9(6) . . ? C21B C22B H22B 117.6 . . ? O6B C22B H22B 117.6 . . ? O14 Cl1 O11 111.7(4) . . ? O14 Cl1 O12 108.9(5) . . ? O11 Cl1 O12 108.4(5) . . ? O14 Cl1 O13 109.4(4) . . ? O11 Cl1 O13 111.7(4) . . ? O12 Cl1 O13 106.6(4) . . ? O24 Cl2 O23 112.8(4) . . ? O24 Cl2 O21 111.5(3) . . ? O23 Cl2 O21 109.3(4) . . ? O24 Cl2 O22 108.6(4) . . ? O23 Cl2 O22 106.1(4) . . ? O21 Cl2 O22 108.3(4) . . ? O34 Cl3 O33 110.7(6) . . ? O34 Cl3 O32 108.4(6) . . ? O33 Cl3 O32 109.3(6) . . ? O34 Cl3 O31 109.4(5) . . ? O33 Cl3 O31 110.9(5) . . ? O32 Cl3 O31 108.0(4) . . ? H1WA O1W H1WB 105(3) . . ? H2WA O2W H2WB 105(3) . . ? N3B C10B H10D 109.5 . . ? N3B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? N3B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.241 _refine_diff_density_min -1.774 _refine_diff_density_rms 0.114