# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Athanassios Boudalis' _publ_contact_author_email TBOU@IMS.DEMOKRITOS.GR _publ_section_title ; Isomorphous replacement of MII ions in MII-GdIII dimers (MII = CuII, MnII, NiII, CoII, ZnII): magnetic studies of the products ; loop_ _publ_author_name 'Athanassios Boudalis' 'Belen Abarca' 'Rosa Adam' 'Rafael Ballesteros' 'Anastasia N. Georgopoulou' ; V.Psycharis ; 'Catherine Raptopoulou' # Attachment 'Dalton.cif' data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 755832' #TrackingRef 'Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H72 Cl2 Cu Gd N9 O21' _chemical_formula_weight 1607.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.3013(2) _cell_length_b 20.5209(3) _cell_length_c 22.6575(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.3630(10) _cell_angle_gamma 90.00 _cell_volume 6860.15(18) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 45989 _cell_measurement_theta_min 6.82 _cell_measurement_theta_max 71.73 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 7.975 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.566 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44868 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 7.14 _diffrn_reflns_theta_max 65.00 _reflns_number_total 10120 _reflns_number_gt 9312 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0003(12) _refine_ls_number_reflns 10120 _refine_ls_number_parameters 895 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd Gd 0.264619(19) 0.959235(12) 0.845224(16) 0.02986(9) Uani 1 1 d . . . Cu Cu 0.45002(5) 0.91129(4) 0.91633(4) 0.0385(2) Uani 1 1 d . . . O1 O 0.4114(2) 0.94881(15) 0.83194(17) 0.0305(9) Uani 1 1 d . . . O3 O 0.1285(2) 0.90371(16) 0.78150(19) 0.0398(10) Uani 1 1 d . . . H3O H 0.0834 0.8988 0.7956 0.052 Uiso 1 1 calc R . . N1 N 0.5259(3) 0.8499(2) 0.8673(2) 0.0376(11) Uani 1 1 d . . . N2 N 0.2792(3) 0.89019(19) 0.7521(2) 0.0332(11) Uani 1 1 d . . . O31 O 0.3323(2) 0.86215(15) 0.89422(18) 0.0358(9) Uani 1 1 d . . . O33 O 0.1323(2) 1.01221(16) 0.86252(17) 0.0358(9) Uani 1 1 d . . . H33O H 0.1164 1.0490 0.8471 0.046 Uiso 1 1 calc R . . N31 N 0.4626(3) 0.8659(2) 0.9953(2) 0.0418(13) Uani 1 1 d . . . N32 N 0.1898(3) 0.90838(19) 0.9241(2) 0.0337(11) Uani 1 1 d . . . O61 O 0.3609(2) 0.99648(17) 0.93407(17) 0.0377(9) Uani 1 1 d . . . O63 O 0.2005(2) 1.02379(16) 0.75451(17) 0.0318(9) Uani 1 1 d . . . H63O H 0.1601 1.0068 0.7261 0.041 Uiso 1 1 calc R . . N61 N 0.5399(3) 0.9844(2) 0.9434(2) 0.0417(12) Uani 1 1 d . . . N62 N 0.3114(3) 1.07899(19) 0.8431(2) 0.0292(10) Uani 1 1 d . . . C1 C 0.5929(4) 0.8078(3) 0.8912(3) 0.0467(16) Uani 1 1 d . . . H1 H 0.5977 0.7913 0.9311 0.061 Uiso 1 1 calc R . . C2 C 0.6552(4) 0.7872(3) 0.8611(3) 0.0494(16) Uani 1 1 d . . . H2 H 0.7009 0.7565 0.8792 0.064 Uiso 1 1 calc R . . C3 C 0.6489(4) 0.8123(3) 0.8049(3) 0.0465(16) Uani 1 1 d . . . H3 H 0.6917 0.8002 0.7831 0.060 Uiso 1 1 calc R . . C4 C 0.5806(4) 0.8552(3) 0.7794(3) 0.0429(15) Uani 1 1 d . . . H4 H 0.5756 0.8729 0.7399 0.056 Uiso 1 1 calc R . . C5 C 0.5185(3) 0.8727(2) 0.8119(3) 0.0323(13) Uani 1 1 d . . . C6 C 0.4387(3) 0.9195(2) 0.7860(3) 0.0320(13) Uani 1 1 d . . . O2 O 0.4678(3) 0.96745(16) 0.74811(19) 0.0384(10) Uani 1 1 d . . . C7 C 0.3601(3) 0.8846(2) 0.7411(3) 0.0338(13) Uani 1 1 d . . . C8 C 0.3705(4) 0.8486(3) 0.6908(3) 0.0478(16) Uani 1 1 d . . . H8 H 0.4282 0.8458 0.6827 0.062 Uiso 1 1 calc R . . C9 C 0.2976(4) 0.8175(3) 0.6534(3) 0.0559(19) Uani 1 1 d . . . H9 H 0.3044 0.7930 0.6193 0.073 Uiso 1 1 calc R . . C10 C 0.2155(4) 0.8218(3) 0.6653(3) 0.0490(17) Uani 1 1 d . . . H10 H 0.1643 0.7998 0.6403 0.064 Uiso 1 1 calc R . . C11 C 0.2077(4) 0.8596(2) 0.7158(3) 0.0358(14) Uani 1 1 d . . . C12 C 0.1152(4) 0.8695(3) 0.7274(3) 0.0419(15) Uani 1 1 d . . . O4 O 0.0725(2) 0.80914(18) 0.7295(2) 0.0481(11) Uani 1 1 d . . . C13 C 0.0524(4) 0.9069(3) 0.6727(3) 0.0406(15) Uani 1 1 d . . . C14 C -0.0246(4) 0.8812(3) 0.6350(3) 0.059(2) Uani 1 1 d . . . H14 H -0.0433 0.8381 0.6411 0.077 Uiso 1 1 calc R . . C15 C -0.0752(5) 0.9197(4) 0.5873(4) 0.070(2) Uani 1 1 d . . . H15 H -0.1293 0.9033 0.5604 0.091 Uiso 1 1 calc R . . C16 C -0.0461(5) 0.9814(3) 0.5797(3) 0.0586(19) Uani 1 1 d . . . H16 H -0.0782 1.0081 0.5469 0.076 Uiso 1 1 calc R . . C17 C 0.0301(4) 1.0034(3) 0.6205(3) 0.0496(16) Uani 1 1 d . . . H17 H 0.0492 1.0467 0.6158 0.064 Uiso 1 1 calc R . . N3 N 0.0804(3) 0.9676(2) 0.6673(2) 0.0421(13) Uani 1 1 d . . . C18 C 0.5321(4) 1.0136(3) 0.7833(3) 0.0455(16) Uani 1 1 d D . . H18A H 0.5802 0.9903 0.8140 0.059 Uiso 1 1 calc R . . H18B H 0.5012 1.0438 0.8053 0.059 Uiso 1 1 calc R . . C19 C 0.5726(6) 1.0508(4) 0.7404(4) 0.090(3) Uani 1 1 d D . . H19A H 0.6195 1.0803 0.7638 0.117 Uiso 1 1 calc R . . H19B H 0.5253 1.0762 0.7122 0.117 Uiso 1 1 calc R . . H19C H 0.5997 1.0203 0.7170 0.117 Uiso 1 1 calc R . . C20 C 0.1216(5) 0.7651(3) 0.7758(4) 0.072(2) Uani 1 1 d D . . H20A H 0.1695 0.7893 0.8056 0.093 Uiso 1 1 calc R . . H20B H 0.1513 0.7314 0.7565 0.093 Uiso 1 1 calc R . . C21 C 0.0623(6) 0.7338(5) 0.8075(5) 0.140(5) Uani 1 1 d D . . H21A H 0.0964 0.7007 0.8355 0.181 Uiso 1 1 calc R . . H21B H 0.0118 0.7131 0.7777 0.181 Uiso 1 1 calc R . . H21C H 0.0387 0.7665 0.8308 0.181 Uiso 1 1 calc R . . C31 C 0.5361(4) 0.8667(3) 1.0439(3) 0.0523(17) Uani 1 1 d . . . H31 H 0.5868 0.8921 1.0412 0.068 Uiso 1 1 calc R . . C32 C 0.5417(5) 0.8328(3) 1.0971(4) 0.066(2) Uani 1 1 d . . . H32 H 0.5947 0.8344 1.1303 0.086 Uiso 1 1 calc R . . C33 C 0.4679(5) 0.7968(4) 1.1002(4) 0.077(2) Uani 1 1 d . . . H33 H 0.4676 0.7746 1.1370 0.100 Uiso 1 1 calc R . . C34 C 0.3935(5) 0.7927(3) 1.0497(4) 0.071(2) Uani 1 1 d . . . H34 H 0.3440 0.7653 1.0509 0.092 Uiso 1 1 calc R . . C35 C 0.3910(4) 0.8286(3) 0.9973(3) 0.0452(16) Uani 1 1 d . . . C36 C 0.3122(4) 0.8275(2) 0.9394(3) 0.0358(14) Uani 1 1 d . . . O32 O 0.2902(3) 0.76047(17) 0.92203(19) 0.0466(11) Uani 1 1 d . . . C37 C 0.2232(3) 0.8517(2) 0.9513(2) 0.0316(12) Uani 1 1 d . . . C38 C 0.1787(4) 0.8178(3) 0.9882(3) 0.0386(14) Uani 1 1 d . . . H38 H 0.2023 0.7777 1.0067 0.050 Uiso 1 1 calc R . . C39 C 0.1002(4) 0.8433(3) 0.9972(3) 0.0474(16) Uani 1 1 d . . . H39 H 0.0691 0.8208 1.0222 0.062 Uiso 1 1 calc R . . C40 C 0.0667(4) 0.9016(3) 0.9702(3) 0.0426(15) Uani 1 1 d . . . H40 H 0.0136 0.9204 0.9771 0.055 Uiso 1 1 calc R . . C41 C 0.1127(4) 0.9321(3) 0.9326(3) 0.0318(13) Uani 1 1 d . . . C42 C 0.0746(3) 0.9930(3) 0.8985(3) 0.0378(14) Uani 1 1 d . . . O34 O 0.0625(3) 1.04411(16) 0.9370(2) 0.0447(11) Uani 1 1 d . . . C43 C -0.0199(4) 0.9779(3) 0.8577(3) 0.0378(14) Uani 1 1 d . . . C44 C -0.0985(4) 0.9949(3) 0.8742(3) 0.0478(17) Uani 1 1 d . . . H44 H -0.0956 1.0198 0.9100 0.062 Uiso 1 1 calc R . . C45 C -0.1816(4) 0.9742(3) 0.8364(4) 0.0562(19) Uani 1 1 d . . . H45 H -0.2364 0.9862 0.8457 0.073 Uiso 1 1 calc R . . C46 C -0.1841(4) 0.9370(4) 0.7864(3) 0.0559(18) Uani 1 1 d . . . H46 H -0.2402 0.9222 0.7607 0.073 Uiso 1 1 calc R . . C47 C -0.1030(4) 0.9210(3) 0.7738(3) 0.0547(18) Uani 1 1 d . . . H47 H -0.1046 0.8946 0.7391 0.071 Uiso 1 1 calc R . . N33 N -0.0222(3) 0.9411(2) 0.8085(2) 0.0426(12) Uani 1 1 d . . . C48 C 0.3596(5) 0.7274(3) 0.9008(4) 0.077(3) Uani 1 1 d D . . H48A H 0.4177 0.7273 0.9332 0.100 Uiso 1 1 calc R . . H48B H 0.3691 0.7494 0.8641 0.100 Uiso 1 1 calc R . . C49 C 0.3272(7) 0.6599(3) 0.8858(5) 0.136(5) Uani 1 1 d D . . H49A H 0.3792 0.6304 0.8928 0.176 Uiso 1 1 calc R . . H49B H 0.2925 0.6576 0.8428 0.176 Uiso 1 1 calc R . . H49C H 0.2884 0.6471 0.9120 0.176 Uiso 1 1 calc R . . C50 C 0.1443(4) 1.0664(3) 0.9802(3) 0.0562(18) Uani 1 1 d D . . H50A H 0.1974 1.0535 0.9657 0.073 Uiso 1 1 calc R . . H50B H 0.1499 1.0452 1.0203 0.073 Uiso 1 1 calc R . . C51 C 0.1440(7) 1.1374(4) 0.9877(6) 0.167(6) Uani 1 1 d D . . H51A H 0.1951 1.1503 1.0219 0.217 Uiso 1 1 calc R . . H51B H 0.0871 1.1509 0.9961 0.217 Uiso 1 1 calc R . . H51C H 0.1498 1.1584 0.9500 0.217 Uiso 1 1 calc R . . C61 C 0.6309(4) 0.9751(3) 0.9509(3) 0.0449(16) Uani 1 1 d . . . H61 H 0.6515 0.9324 0.9454 0.058 Uiso 1 1 calc R . . C62 C 0.6942(4) 1.0244(3) 0.9660(3) 0.0571(18) Uani 1 1 d . . . H62 H 0.7566 1.0164 0.9699 0.074 Uiso 1 1 calc R . . C63 C 0.6632(4) 1.0858(3) 0.9753(3) 0.062(2) Uani 1 1 d . . . H63 H 0.7043 1.1213 0.9852 0.081 Uiso 1 1 calc R . . C64 C 0.5737(4) 1.0951(3) 0.9701(3) 0.0565(19) Uani 1 1 d . . . H64 H 0.5525 1.1369 0.9777 0.073 Uiso 1 1 calc R . . C65 C 0.5124(4) 1.0435(2) 0.9538(3) 0.0368(14) Uani 1 1 d . . . C66 C 0.4084(4) 1.0539(3) 0.9452(3) 0.0357(14) Uani 1 1 d . . . O62 O 0.3981(3) 1.08813(19) 0.9982(2) 0.0510(11) Uani 1 1 d . . . C67 C 0.3702(4) 1.1031(3) 0.8941(3) 0.0348(13) Uani 1 1 d . . . C68 C 0.3929(4) 1.1687(3) 0.8987(3) 0.0466(16) Uani 1 1 d . . . H68 H 0.4314 1.1854 0.9356 0.061 Uiso 1 1 calc R . . C69 C 0.3592(4) 1.2100(3) 0.8492(3) 0.0493(17) Uani 1 1 d . . . H69 H 0.3748 1.2549 0.8517 0.064 Uiso 1 1 calc R . . C70 C 0.3030(4) 1.1845(3) 0.7966(3) 0.0406(15) Uani 1 1 d . . . H70 H 0.2820 1.2106 0.7610 0.053 Uiso 1 1 calc R . . C71 C 0.2780(3) 1.1201(2) 0.7969(3) 0.0319(13) Uani 1 1 d . . . C72 C 0.2055(4) 1.0915(2) 0.7434(3) 0.0346(14) Uani 1 1 d . . . O64 O 0.2214(3) 1.10368(17) 0.68747(18) 0.0427(10) Uani 1 1 d . . . C73 C 0.1147(3) 1.1250(2) 0.7426(3) 0.0327(13) Uani 1 1 d . . . C74 C 0.0741(4) 1.1690(2) 0.6967(3) 0.0431(15) Uani 1 1 d . . . H74 H 0.0995 1.1782 0.6637 0.056 Uiso 1 1 calc R . . C75 C -0.0047(4) 1.1987(3) 0.7014(3) 0.0529(17) Uani 1 1 d . . . H75 H -0.0343 1.2289 0.6709 0.069 Uiso 1 1 calc R . . C76 C -0.0404(4) 1.1859(3) 0.7481(3) 0.0545(18) Uani 1 1 d . . . H76 H -0.0943 1.2070 0.7513 0.071 Uiso 1 1 calc R . . C77 C 0.0036(4) 1.1412(3) 0.7916(3) 0.0552(18) Uani 1 1 d . . . H77 H -0.0210 1.1320 0.8251 0.072 Uiso 1 1 calc R . . N63 N 0.0789(3) 1.1105(2) 0.7886(2) 0.0410(12) Uani 1 1 d . . . C78 C 0.4149(7) 1.0498(4) 1.0545(4) 0.085(3) Uani 1 1 d D . . H78A H 0.3657 1.0583 1.0744 0.111 Uiso 1 1 calc R . . H78B H 0.4129 1.0030 1.0439 0.111 Uiso 1 1 calc R . . C79 C 0.5003(9) 1.0638(7) 1.0975(5) 0.164(6) Uani 1 1 d D . . H79A H 0.5085 1.0351 1.1332 0.213 Uiso 1 1 calc R . . H79B H 0.5012 1.1093 1.1107 0.213 Uiso 1 1 calc R . . H79C H 0.5495 1.0564 1.0780 0.213 Uiso 1 1 calc R . . C80 C 0.3073(4) 1.0812(3) 0.6815(3) 0.060(2) Uani 1 1 d D . . H80A H 0.3240 1.0399 0.7042 0.078 Uiso 1 1 calc R . . H80B H 0.3549 1.1139 0.6986 0.078 Uiso 1 1 calc R . . C81 C 0.3006(7) 1.0712(6) 0.6177(4) 0.143(5) Uani 1 1 d D . . H81A H 0.3604 1.0769 0.6103 0.186 Uiso 1 1 calc R . . H81B H 0.2581 1.1029 0.5933 0.186 Uiso 1 1 calc R . . H81C H 0.2785 1.0270 0.6060 0.186 Uiso 1 1 calc R . . Cl1 Cl 0.34035(11) 0.65897(8) 0.51169(9) 0.0613(5) Uani 1 1 d . . . O91 O 0.3253(6) 0.5982(4) 0.4794(4) 0.071(2) Uiso 0.65 1 d P A 1 O92 O 0.3643(6) 0.7012(4) 0.4684(5) 0.088(3) Uiso 0.65 1 d P A 1 O93 O 0.2626(8) 0.6825(6) 0.5289(5) 0.102(4) Uiso 0.65 1 d P A 1 O94 O 0.4132(8) 0.6506(5) 0.5654(5) 0.088(4) Uiso 0.65 1 d P A 1 O91A O 0.3239(17) 0.6234(13) 0.4558(12) 0.143(9) Uiso 0.35 1 d P A 2 O92A O 0.3620(11) 0.7233(8) 0.4988(8) 0.085(5) Uiso 0.35 1 d P A 2 O93A O 0.2560(12) 0.6558(9) 0.5283(9) 0.076(6) Uiso 0.35 1 d P A 2 O94A O 0.4112(12) 0.6286(9) 0.5548(9) 0.072(6) Uiso 0.35 1 d P A 2 Cl2 Cl 0.72999(12) 0.80750(8) 0.63754(9) 0.0599(5) Uani 1 1 d . . . O95 O 0.6496(11) 0.7734(7) 0.6216(8) 0.163(6) Uiso 0.65 1 d P B 3 O96 O 0.7547(5) 0.8214(4) 0.5836(4) 0.069(2) Uiso 0.65 1 d P B 3 O97 O 0.8134(9) 0.7797(6) 0.6799(6) 0.123(4) Uiso 0.65 1 d P B 3 O98 O 0.7101(8) 0.8674(6) 0.6608(5) 0.130(4) Uiso 0.65 1 d P B 3 O95A O 0.667(2) 0.7698(13) 0.5935(14) 0.158(11) Uiso 0.35 1 d P B 4 O96A O 0.7650(14) 0.8591(10) 0.6119(10) 0.126(7) Uiso 0.35 1 d P B 4 O97A O 0.7854(17) 0.7521(12) 0.6549(12) 0.135(9) Uiso 0.35 1 d P B 4 O98A O 0.6925(11) 0.8183(9) 0.6848(9) 0.099(5) Uiso 0.35 1 d P B 4 O99 O 0.2610(4) 0.6436(3) 0.6576(3) 0.0819(16) Uani 1 1 d . . . H99O H 0.2703 0.6540 0.6239 0.107 Uiso 1 1 calc R . . C91 C 0.2934(6) 0.5796(4) 0.6735(4) 0.085(3) Uani 1 1 d . . . H91A H 0.2885 0.5694 0.7152 0.110 Uiso 1 1 calc R . . H91B H 0.3582 0.5774 0.6741 0.110 Uiso 1 1 calc R . . C92 C 0.2436(6) 0.5315(4) 0.6312(4) 0.090(3) Uani 1 1 d . . . H92A H 0.2713 0.4886 0.6419 0.117 Uiso 1 1 calc R . . H92B H 0.2450 0.5429 0.5895 0.117 Uiso 1 1 calc R . . H92C H 0.1806 0.5304 0.6336 0.117 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 Gd 0.02158(15) 0.02993(14) 0.0383(2) 0.00388(16) 0.00836(14) 0.00213(14) Cu 0.0272(4) 0.0411(4) 0.0459(6) 0.0075(4) 0.0072(4) 0.0011(4) O1 0.0191(19) 0.0373(19) 0.034(3) -0.0031(16) 0.0061(18) 0.0006(14) O3 0.024(2) 0.043(2) 0.052(3) -0.0082(19) 0.011(2) -0.0068(16) N1 0.028(3) 0.041(3) 0.043(3) 0.010(2) 0.007(2) 0.008(2) N2 0.032(3) 0.026(2) 0.041(3) 0.000(2) 0.010(2) 0.0026(18) O31 0.035(2) 0.0285(18) 0.049(3) 0.0161(17) 0.020(2) 0.0069(16) O33 0.027(2) 0.0368(19) 0.048(3) 0.0127(18) 0.0180(19) 0.0108(16) N31 0.025(3) 0.047(3) 0.053(4) 0.012(3) 0.009(3) 0.002(2) N32 0.024(2) 0.038(2) 0.041(3) 0.007(2) 0.011(2) 0.0023(18) O61 0.032(2) 0.039(2) 0.042(3) 0.0048(18) 0.010(2) -0.0028(16) O63 0.032(2) 0.0278(17) 0.030(2) -0.0010(16) -0.0020(19) 0.0036(15) N61 0.033(3) 0.047(3) 0.046(4) 0.006(2) 0.012(3) 0.002(2) N62 0.029(3) 0.026(2) 0.032(3) -0.003(2) 0.008(2) 0.0027(18) C1 0.036(3) 0.047(3) 0.058(5) 0.008(3) 0.013(3) 0.003(3) C2 0.034(3) 0.044(3) 0.067(5) -0.005(3) 0.007(3) 0.015(3) C3 0.032(3) 0.048(3) 0.061(5) 0.000(3) 0.014(3) 0.009(3) C4 0.028(3) 0.046(3) 0.056(5) -0.002(3) 0.013(3) 0.009(2) C5 0.028(3) 0.027(3) 0.042(4) 0.000(2) 0.009(3) 0.002(2) C6 0.022(3) 0.033(3) 0.041(4) 0.003(3) 0.009(3) 0.004(2) O2 0.032(2) 0.040(2) 0.045(3) 0.0108(18) 0.014(2) 0.0026(16) C7 0.027(3) 0.028(3) 0.046(4) 0.002(2) 0.009(3) 0.009(2) C8 0.033(3) 0.049(3) 0.057(5) -0.014(3) 0.005(3) 0.007(3) C9 0.050(4) 0.056(4) 0.060(5) -0.023(3) 0.011(4) 0.017(3) C10 0.031(3) 0.040(3) 0.064(5) -0.009(3) -0.008(3) 0.005(3) C11 0.030(3) 0.026(3) 0.047(4) 0.000(3) 0.003(3) 0.003(2) C12 0.023(3) 0.036(3) 0.062(5) 0.001(3) 0.004(3) -0.001(2) O4 0.034(2) 0.040(2) 0.062(3) 0.007(2) -0.003(2) -0.0085(17) C13 0.028(3) 0.047(3) 0.041(4) 0.002(3) -0.001(3) 0.006(3) C14 0.046(4) 0.049(4) 0.068(6) 0.001(4) -0.009(4) -0.022(3) C15 0.041(4) 0.090(6) 0.062(6) 0.002(4) -0.018(4) -0.003(4) C16 0.050(4) 0.068(4) 0.048(5) 0.017(4) -0.005(4) 0.007(4) C17 0.040(4) 0.050(4) 0.051(5) 0.007(3) -0.001(3) 0.001(3) N3 0.040(3) 0.040(3) 0.042(4) -0.003(2) 0.002(3) 0.001(2) C18 0.044(4) 0.045(3) 0.047(5) 0.000(3) 0.011(3) -0.013(3) C19 0.089(6) 0.101(6) 0.088(7) 0.028(5) 0.036(6) -0.039(5) C20 0.063(5) 0.053(4) 0.092(6) 0.009(4) 0.009(5) -0.016(4) C21 0.096(7) 0.157(10) 0.184(12) 0.087(9) 0.070(8) -0.004(7) C31 0.036(4) 0.065(4) 0.051(5) 0.017(4) 0.004(4) 0.001(3) C32 0.038(4) 0.068(4) 0.086(6) 0.026(4) 0.007(4) 0.003(3) C33 0.060(5) 0.083(5) 0.074(6) 0.034(5) -0.009(5) -0.009(4) C34 0.051(4) 0.080(5) 0.079(6) 0.043(4) 0.012(4) -0.013(4) C35 0.035(3) 0.040(3) 0.062(5) 0.021(3) 0.014(3) 0.004(3) C36 0.032(3) 0.031(3) 0.048(4) 0.016(3) 0.015(3) 0.004(2) O32 0.045(2) 0.036(2) 0.067(3) 0.008(2) 0.030(2) 0.0053(18) C37 0.028(3) 0.034(3) 0.030(4) 0.008(2) 0.003(3) 0.002(2) C38 0.037(3) 0.039(3) 0.041(4) 0.012(3) 0.012(3) 0.002(3) C39 0.042(4) 0.049(3) 0.055(5) 0.012(3) 0.020(3) 0.004(3) C40 0.033(3) 0.057(4) 0.042(4) -0.002(3) 0.017(3) 0.002(3) C41 0.028(3) 0.038(3) 0.028(4) 0.001(2) 0.005(3) -0.001(2) C42 0.025(3) 0.042(3) 0.051(4) 0.002(3) 0.017(3) 0.000(2) O34 0.036(2) 0.043(2) 0.057(3) -0.0044(19) 0.016(2) 0.0077(17) C43 0.033(3) 0.038(3) 0.044(4) 0.008(3) 0.011(3) 0.007(2) C44 0.028(3) 0.056(4) 0.063(5) 0.008(3) 0.020(3) 0.011(3) C45 0.026(4) 0.077(4) 0.067(6) 0.014(4) 0.015(4) 0.010(3) C46 0.024(3) 0.091(5) 0.048(5) 0.014(4) 0.001(3) 0.000(3) C47 0.034(4) 0.068(4) 0.059(5) -0.011(4) 0.007(4) -0.011(3) N33 0.025(3) 0.049(3) 0.053(4) -0.002(3) 0.011(3) -0.004(2) C48 0.075(5) 0.041(4) 0.140(8) 0.001(4) 0.070(6) 0.009(3) C49 0.174(9) 0.042(4) 0.260(13) -0.016(6) 0.178(10) -0.002(5) C50 0.049(4) 0.055(4) 0.062(5) -0.004(4) 0.010(4) 0.002(3) C51 0.142(10) 0.070(6) 0.217(14) -0.034(7) -0.077(10) 0.008(6) C61 0.030(3) 0.057(4) 0.046(5) -0.003(3) 0.006(3) 0.001(3) C62 0.034(4) 0.082(5) 0.054(5) -0.007(4) 0.008(4) -0.017(3) C63 0.039(4) 0.062(4) 0.079(6) -0.023(4) 0.004(4) -0.010(3) C64 0.032(4) 0.063(4) 0.068(5) -0.018(4) 0.001(4) -0.006(3) C65 0.038(4) 0.044(3) 0.028(4) 0.002(2) 0.007(3) 0.000(2) C66 0.033(3) 0.040(3) 0.030(4) -0.005(3) 0.001(3) -0.007(2) O62 0.057(3) 0.059(3) 0.038(3) -0.012(2) 0.014(2) 0.000(2) C67 0.027(3) 0.038(3) 0.040(4) -0.001(3) 0.011(3) 0.000(2) C68 0.038(4) 0.042(3) 0.055(5) -0.017(3) 0.005(3) -0.007(3) C69 0.044(4) 0.034(3) 0.071(5) 0.002(3) 0.016(4) -0.002(3) C70 0.032(3) 0.043(3) 0.049(4) 0.014(3) 0.017(3) 0.006(3) C71 0.022(3) 0.033(3) 0.043(4) -0.001(3) 0.013(3) 0.004(2) C72 0.036(3) 0.028(3) 0.042(4) 0.008(2) 0.013(3) 0.009(2) O64 0.043(2) 0.044(2) 0.045(3) 0.0118(19) 0.020(2) 0.0144(18) C73 0.025(3) 0.031(3) 0.039(4) 0.004(2) 0.003(3) 0.002(2) C74 0.045(4) 0.037(3) 0.046(4) 0.005(3) 0.007(3) 0.012(3) C75 0.041(4) 0.043(3) 0.070(5) 0.002(3) 0.007(4) 0.023(3) C76 0.037(4) 0.046(3) 0.079(6) 0.009(3) 0.013(4) 0.016(3) C77 0.039(4) 0.059(4) 0.073(5) 0.006(4) 0.024(4) 0.011(3) N63 0.032(3) 0.038(2) 0.055(4) 0.016(2) 0.014(3) 0.017(2) C78 0.128(9) 0.069(5) 0.063(7) 0.005(4) 0.033(7) 0.006(5) C79 0.165(13) 0.273(15) 0.053(8) 0.046(9) 0.027(9) 0.098(12) C80 0.050(4) 0.072(5) 0.068(6) 0.008(4) 0.033(4) 0.018(3) C81 0.096(8) 0.264(13) 0.074(8) -0.034(8) 0.033(6) 0.072(8) Cl1 0.0447(9) 0.0667(11) 0.0688(14) 0.0199(10) 0.0084(10) -0.0081(8) Cl2 0.0725(12) 0.0525(9) 0.0625(13) -0.0019(9) 0.0317(11) -0.0148(9) O99 0.063(3) 0.079(4) 0.102(5) 0.014(3) 0.017(3) 0.009(3) C91 0.082(6) 0.095(7) 0.074(7) -0.008(5) 0.016(5) -0.017(5) C92 0.083(7) 0.100(7) 0.083(7) 0.002(5) 0.017(6) -0.012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O61 2.288(4) . ? Gd O1 2.353(3) . ? Gd O31 2.380(3) . ? Gd O33 2.419(3) . ? Gd O63 2.424(4) . ? Gd O3 2.475(4) . ? Gd N62 2.564(4) . ? Gd N32 2.585(4) . ? Gd N2 2.600(4) . ? Gd Cu 3.0314(9) . ? Cu N31 1.981(5) . ? Cu O1 2.000(4) . ? Cu O31 2.009(4) . ? Cu N61 2.017(5) . ? Cu N1 2.202(4) . ? Cu O61 2.316(3) . ? O1 C6 1.360(6) . ? O3 C12 1.379(7) . ? O3 H3O 0.8400 . ? N1 C5 1.316(6) . ? N1 C1 1.341(7) . ? N2 C7 1.331(6) . ? N2 C11 1.337(6) . ? O31 C36 1.346(6) . ? O33 C42 1.408(5) . ? O33 H33O 0.8400 . ? N31 C35 1.347(6) . ? N31 C31 1.350(8) . ? N32 C41 1.335(6) . ? N32 C37 1.351(6) . ? O61 C66 1.372(6) . ? O63 C72 1.418(5) . ? O63 H63O 0.8400 . ? N61 C65 1.325(6) . ? N61 C61 1.370(7) . ? N62 C71 1.337(6) . ? N62 C67 1.355(7) . ? C1 C2 1.377(7) . ? C1 H1 0.9500 . ? C2 C3 1.354(8) . ? C2 H2 0.9500 . ? C3 C4 1.372(7) . ? C3 H3 0.9500 . ? C4 C5 1.394(7) . ? C4 H4 0.9500 . ? C5 C6 1.542(6) . ? C6 O2 1.451(6) . ? C6 C7 1.530(7) . ? O2 C18 1.444(6) . ? C7 C8 1.403(7) . ? C8 C9 1.367(8) . ? C8 H8 0.9500 . ? C9 C10 1.356(8) . ? C9 H9 0.9500 . ? C10 C11 1.413(8) . ? C10 H10 0.9500 . ? C11 C12 1.521(7) . ? C12 O4 1.407(6) . ? C12 C13 1.556(8) . ? O4 C20 1.437(8) . ? C13 N3 1.333(6) . ? C13 C14 1.364(8) . ? C14 C15 1.396(9) . ? C14 H14 0.9500 . ? C15 C16 1.368(9) . ? C15 H15 0.9500 . ? C16 C17 1.358(9) . ? C16 H16 0.9500 . ? C17 N3 1.351(7) . ? C17 H17 0.9500 . ? C18 C19 1.495(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.448(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C31 C32 1.374(9) . ? C31 H31 0.9500 . ? C32 C33 1.367(9) . ? C32 H32 0.9500 . ? C33 C34 1.387(10) . ? C33 H33 0.9500 . ? C34 C35 1.389(8) . ? C34 H34 0.9500 . ? C35 C36 1.529(9) . ? C36 O32 1.446(6) . ? C36 C37 1.540(7) . ? O32 C48 1.446(6) . ? C37 C38 1.395(6) . ? C38 C39 1.375(7) . ? C38 H38 0.9500 . ? C39 C40 1.378(7) . ? C39 H39 0.9500 . ? C40 C41 1.391(7) . ? C40 H40 0.9500 . ? C41 C42 1.503(7) . ? C42 O34 1.409(6) . ? C42 C43 1.526(8) . ? O34 C50 1.444(7) . ? C43 N33 1.340(7) . ? C43 C44 1.396(7) . ? C44 C45 1.397(9) . ? C44 H44 0.9500 . ? C45 C46 1.360(9) . ? C45 H45 0.9500 . ? C46 C47 1.384(8) . ? C46 H46 0.9500 . ? C47 N33 1.342(7) . ? C47 H47 0.9500 . ? C48 C49 1.480(8) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.467(9) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C61 C62 1.379(8) . ? C61 H61 0.9500 . ? C62 C63 1.382(8) . ? C62 H62 0.9500 . ? C63 C64 1.357(8) . ? C63 H63 0.9500 . ? C64 C65 1.398(8) . ? C64 H64 0.9500 . ? C65 C66 1.565(8) . ? C66 O62 1.435(6) . ? C66 C67 1.531(8) . ? O62 C78 1.463(9) . ? C67 C68 1.387(7) . ? C68 C69 1.391(9) . ? C68 H68 0.9500 . ? C69 C70 1.376(8) . ? C69 H69 0.9500 . ? C70 C71 1.375(7) . ? C70 H70 0.9500 . ? C71 C72 1.528(8) . ? C72 O64 1.374(6) . ? C72 C73 1.546(7) . ? O64 C80 1.433(6) . ? C73 N63 1.333(6) . ? C73 C74 1.392(7) . ? C74 C75 1.380(7) . ? C74 H74 0.9500 . ? C75 C76 1.339(8) . ? C75 H75 0.9500 . ? C76 C77 1.384(8) . ? C76 H76 0.9500 . ? C77 N63 1.331(6) . ? C77 H77 0.9500 . ? C78 C79 1.436(12) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.436(9) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? Cl1 O94A 1.399(19) . ? Cl1 O92A 1.411(16) . ? Cl1 O91A 1.43(3) . ? Cl1 O94 1.427(12) . ? Cl1 O92 1.429(9) . ? Cl1 O93 1.431(12) . ? Cl1 O91 1.434(8) . ? Cl1 O93A 1.438(18) . ? Cl2 O98A 1.359(18) . ? Cl2 O95 1.377(16) . ? Cl2 O96A 1.38(2) . ? Cl2 O96 1.402(8) . ? Cl2 O98 1.403(11) . ? Cl2 O97A 1.41(2) . ? Cl2 O95A 1.42(3) . ? Cl2 O97 1.492(13) . ? O99 C91 1.416(9) . ? O99 H99O 0.8400 . ? C91 C92 1.444(10) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? 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 O61 Gd O1 74.27(12) . . ? O61 Gd O31 76.70(13) . . ? O1 Gd O31 70.82(11) . . ? O61 Gd O33 94.53(12) . . ? O1 Gd O33 158.33(11) . . ? O31 Gd O33 125.45(11) . . ? O61 Gd O63 125.82(12) . . ? O1 Gd O63 97.31(12) . . ? O31 Gd O63 151.82(12) . . ? O33 Gd O63 73.94(12) . . ? O61 Gd O3 155.94(12) . . ? O1 Gd O3 124.57(12) . . ? O31 Gd O3 94.68(13) . . ? O33 Gd O3 71.98(12) . . ? O63 Gd O3 70.59(12) . . ? O61 Gd N62 65.05(14) . . ? O1 Gd N62 78.71(11) . . ? O31 Gd N62 136.22(14) . . ? O33 Gd N62 79.74(11) . . ? O63 Gd N62 60.84(13) . . ? O3 Gd N62 128.78(13) . . ? O61 Gd N32 80.00(13) . . ? O1 Gd N32 131.63(13) . . ? O31 Gd N32 63.72(11) . . ? O33 Gd N32 61.74(12) . . ? O63 Gd N32 130.78(12) . . ? O3 Gd N32 76.07(14) . . ? N62 Gd N32 125.23(13) . . ? O61 Gd N2 136.25(13) . . ? O1 Gd N2 63.69(13) . . ? O31 Gd N2 78.58(13) . . ? O33 Gd N2 129.17(13) . . ? O63 Gd N2 73.27(12) . . ? O3 Gd N2 61.01(13) . . ? N62 Gd N2 115.03(13) . . ? N32 Gd N2 119.36(13) . . ? O61 Gd Cu 49.23(9) . . ? O1 Gd Cu 41.24(9) . . ? O31 Gd Cu 41.43(9) . . ? O33 Gd Cu 139.92(9) . . ? O63 Gd Cu 137.72(8) . . ? O3 Gd Cu 133.22(8) . . ? N62 Gd Cu 95.42(10) . . ? N32 Gd Cu 91.43(10) . . ? N2 Gd Cu 89.15(10) . . ? N31 Cu O1 167.96(17) . . ? N31 Cu O31 81.68(17) . . ? O1 Cu O31 86.34(14) . . ? N31 Cu N61 100.4(2) . . ? O1 Cu N61 90.55(17) . . ? O31 Cu N61 160.59(16) . . ? N31 Cu N1 104.41(18) . . ? O1 Cu N1 78.45(15) . . ? O31 Cu N1 98.33(15) . . ? N61 Cu N1 99.81(17) . . ? N31 Cu O61 96.82(16) . . ? O1 Cu O61 80.61(13) . . ? O31 Cu O61 83.80(12) . . ? N61 Cu O61 76.79(15) . . ? N1 Cu O61 158.76(15) . . ? N31 Cu Gd 119.07(13) . . ? O1 Cu Gd 50.86(9) . . ? O31 Cu Gd 51.63(9) . . ? N61 Cu Gd 112.76(13) . . ? N1 Cu Gd 117.49(13) . . ? O61 Cu Gd 48.43(10) . . ? C6 O1 Cu 119.2(3) . . ? C6 O1 Gd 129.4(3) . . ? Cu O1 Gd 87.90(13) . . ? C12 O3 Gd 131.0(3) . . ? C12 O3 H3O 109.5 . . ? Gd O3 H3O 118.9 . . ? C5 N1 C1 118.5(5) . . ? C5 N1 Cu 110.8(3) . . ? C1 N1 Cu 127.9(4) . . ? C7 N2 C11 119.6(5) . . ? C7 N2 Gd 118.8(4) . . ? C11 N2 Gd 121.5(3) . . ? C36 O31 Cu 116.5(4) . . ? C36 O31 Gd 129.6(3) . . ? Cu O31 Gd 86.95(11) . . ? C42 O33 Gd 130.4(3) . . ? C42 O33 H33O 109.5 . . ? Gd O33 H33O 120.0 . . ? C35 N31 C31 119.2(5) . . ? C35 N31 Cu 114.4(4) . . ? C31 N31 Cu 126.3(4) . . ? C41 N32 C37 119.4(4) . . ? C41 N32 Gd 121.4(3) . . ? C37 N32 Gd 118.6(3) . . ? C66 O61 Gd 129.4(3) . . ? C66 O61 Cu 111.9(3) . . ? Gd O61 Cu 82.34(12) . . ? C72 O63 Gd 131.1(3) . . ? C72 O63 H63O 109.5 . . ? Gd O63 H63O 118.2 . . ? C65 N61 C61 117.7(5) . . ? C65 N61 Cu 120.7(4) . . ? C61 N61 Cu 121.5(4) . . ? C71 N62 C67 117.8(5) . . ? C71 N62 Gd 124.7(4) . . ? C67 N62 Gd 117.4(3) . . ? N1 C1 C2 123.6(6) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 117.7(6) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 119.7(6) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 119.6(6) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 120.9(5) . . ? N1 C5 C6 116.3(4) . . ? C4 C5 C6 122.8(5) . . ? O1 C6 O2 110.9(4) . . ? O1 C6 C7 111.6(4) . . ? O2 C6 C7 103.5(4) . . ? O1 C6 C5 110.9(4) . . ? O2 C6 C5 108.1(4) . . ? C7 C6 C5 111.5(4) . . ? C18 O2 C6 112.9(4) . . ? N2 C7 C8 120.6(5) . . ? N2 C7 C6 116.2(5) . . ? C8 C7 C6 123.2(5) . . ? C9 C8 C7 120.0(6) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 119.6(6) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 118.5(6) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? N2 C11 C10 121.7(5) . . ? N2 C11 C12 118.5(5) . . ? C10 C11 C12 119.7(5) . . ? O3 C12 O4 112.2(5) . . ? O3 C12 C11 107.3(5) . . ? O4 C12 C11 110.5(4) . . ? O3 C12 C13 111.8(4) . . ? O4 C12 C13 105.5(5) . . ? C11 C12 C13 109.5(5) . . ? C12 O4 C20 114.9(5) . . ? N3 C13 C14 123.4(6) . . ? N3 C13 C12 112.8(5) . . ? C14 C13 C12 123.8(5) . . ? C13 C14 C15 118.4(6) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 119.3(7) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 118.1(6) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? N3 C17 C16 124.1(6) . . ? N3 C17 H17 117.9 . . ? C16 C17 H17 117.9 . . ? C13 N3 C17 116.7(5) . . ? O2 C18 C19 108.4(5) . . ? O2 C18 H18A 110.0 . . ? C19 C18 H18A 110.0 . . ? O2 C18 H18B 110.0 . . ? C19 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C20 C21 111.4(6) . . ? O4 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? O4 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N31 C31 C32 123.7(6) . . ? N31 C31 H31 118.1 . . ? C32 C31 H31 118.1 . . ? C33 C32 C31 117.3(7) . . ? C33 C32 H32 121.4 . . ? C31 C32 H32 121.4 . . ? C32 C33 C34 119.9(8) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C35 120.2(6) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? N31 C35 C34 119.5(6) . . ? N31 C35 C36 116.2(5) . . ? C34 C35 C36 124.3(5) . . ? O31 C36 O32 112.3(5) . . ? O31 C36 C35 111.0(4) . . ? O32 C36 C35 108.7(4) . . ? O31 C36 C37 110.8(4) . . ? O32 C36 C37 101.6(4) . . ? C35 C36 C37 112.2(5) . . ? C48 O32 C36 113.5(4) . . ? N32 C37 C38 121.2(5) . . ? N32 C37 C36 116.3(4) . . ? C38 C37 C36 122.6(4) . . ? C39 C38 C37 118.8(5) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C38 C39 C40 120.1(5) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C41 118.3(5) . . ? C39 C40 H40 120.8 . . ? C41 C40 H40 120.8 . . ? N32 C41 C40 122.2(5) . . ? N32 C41 C42 117.9(4) . . ? C40 C41 C42 119.9(5) . . ? O33 C42 O34 110.8(4) . . ? O33 C42 C41 108.2(4) . . ? O34 C42 C41 113.4(5) . . ? O33 C42 C43 110.2(5) . . ? O34 C42 C43 105.5(4) . . ? C41 C42 C43 108.6(4) . . ? C42 O34 C50 115.0(4) . . ? N33 C43 C44 121.9(6) . . ? N33 C43 C42 115.5(5) . . ? C44 C43 C42 122.2(6) . . ? C43 C44 C45 118.0(6) . . ? C43 C44 H44 121.0 . . ? C45 C44 H44 121.0 . . ? C46 C45 C44 120.1(6) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 118.4(6) . . ? C45 C46 H46 120.8 . . ? C47 C46 H46 120.8 . . ? N33 C47 C46 123.0(6) . . ? N33 C47 H47 118.5 . . ? C46 C47 H47 118.5 . . ? C43 N33 C47 118.5(5) . . ? O32 C48 C49 106.5(5) . . ? O32 C48 H48A 110.4 . . ? C49 C48 H48A 110.4 . . ? O32 C48 H48B 110.4 . . ? C49 C48 H48B 110.4 . . ? H48A C48 H48B 108.6 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O34 C50 C51 111.3(6) . . ? O34 C50 H50A 109.4 . . ? C51 C50 H50A 109.4 . . ? O34 C50 H50B 109.4 . . ? C51 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N61 C61 C62 123.5(6) . . ? N61 C61 H61 118.2 . . ? C62 C61 H61 118.2 . . ? C61 C62 C63 117.4(6) . . ? C61 C62 H62 121.3 . . ? C63 C62 H62 121.3 . . ? C64 C63 C62 119.6(6) . . ? C64 C63 H63 120.2 . . ? C62 C63 H63 120.2 . . ? C63 C64 C65 120.5(6) . . ? C63 C64 H64 119.7 . . ? C65 C64 H64 119.7 . . ? N61 C65 C64 121.2(6) . . ? N61 C65 C66 117.6(5) . . ? C64 C65 C66 121.2(5) . . ? O61 C66 O62 113.8(4) . . ? O61 C66 C67 110.5(5) . . ? O62 C66 C67 101.8(4) . . ? O61 C66 C65 112.1(4) . . ? O62 C66 C65 107.3(5) . . ? C67 C66 C65 110.8(4) . . ? C66 O62 C78 115.7(5) . . ? N62 C67 C68 121.0(6) . . ? N62 C67 C66 116.0(5) . . ? C68 C67 C66 123.1(6) . . ? C67 C68 C69 119.9(6) . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C70 C69 C68 118.7(5) . . ? C70 C69 H69 120.7 . . ? C68 C69 H69 120.7 . . ? C71 C70 C69 118.1(6) . . ? C71 C70 H70 121.0 . . ? C69 C70 H70 121.0 . . ? N62 C71 C70 124.2(5) . . ? N62 C71 C72 115.2(4) . . ? C70 C71 C72 120.6(5) . . ? O64 C72 O63 111.9(4) . . ? O64 C72 C71 113.1(4) . . ? O63 C72 C71 107.3(4) . . ? O64 C72 C73 106.7(4) . . ? O63 C72 C73 110.3(4) . . ? C71 C72 C73 107.4(4) . . ? C72 O64 C80 114.9(5) . . ? N63 C73 C74 122.3(5) . . ? N63 C73 C72 116.4(5) . . ? C74 C73 C72 121.3(5) . . ? C75 C74 C73 117.0(6) . . ? C75 C74 H74 121.5 . . ? C73 C74 H74 121.5 . . ? C76 C75 C74 121.5(6) . . ? C76 C75 H75 119.2 . . ? C74 C75 H75 119.2 . . ? C75 C76 C77 117.9(6) . . ? C75 C76 H76 121.0 . . ? C77 C76 H76 121.0 . . ? N63 C77 C76 122.8(6) . . ? N63 C77 H77 118.6 . . ? C76 C77 H77 118.6 . . ? C77 N63 C73 118.4(5) . . ? C79 C78 O62 113.8(8) . . ? C79 C78 H78A 108.8 . . ? O62 C78 H78A 108.8 . . ? C79 C78 H78B 108.8 . . ? O62 C78 H78B 108.8 . . ? H78A C78 H78B 107.7 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O64 C80 C81 108.5(6) . . ? O64 C80 H80A 110.0 . . ? C81 C80 H80A 110.0 . . ? O64 C80 H80B 110.0 . . ? C81 C80 H80B 110.0 . . ? H80A C80 H80B 108.4 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? O94A Cl1 O92A 112.4(10) . . ? O94A Cl1 O91A 108.3(13) . . ? O92A Cl1 O91A 106.9(13) . . ? O94A Cl1 O94 20.7(9) . . ? O92A Cl1 O94 96.7(8) . . ? O91A Cl1 O94 127.7(11) . . ? O94A Cl1 O92 117.3(8) . . ? O92A Cl1 O92 34.1(7) . . ? O91A Cl1 O92 73.5(11) . . ? O94 Cl1 O92 112.0(6) . . ? O94A Cl1 O93 120.4(9) . . ? O92A Cl1 O93 89.9(8) . . ? O91A Cl1 O93 116.9(11) . . ? O94 Cl1 O93 109.0(7) . . ? O92 Cl1 O93 111.5(6) . . ? O94A Cl1 O91 87.6(8) . . ? O92A Cl1 O91 136.4(8) . . ? O91A Cl1 O91 30.1(10) . . ? O94 Cl1 O91 108.3(6) . . ? O92 Cl1 O91 102.3(5) . . ? O93 Cl1 O91 113.6(6) . . ? O94A Cl1 O93A 112.3(10) . . ? O92A Cl1 O93A 111.9(10) . . ? O91A Cl1 O93A 104.5(12) . . ? O94 Cl1 O93A 108.9(9) . . ? O92 Cl1 O93A 128.2(9) . . ? O93 Cl1 O93A 22.4(8) . . ? O91 Cl1 O93A 93.4(8) . . ? O98A Cl2 O95 75.8(9) . . ? O98A Cl2 O96A 119.8(12) . . ? O95 Cl2 O96A 134.2(12) . . ? O98A Cl2 O96 157.1(8) . . ? O95 Cl2 O96 107.6(8) . . ? O96A Cl2 O96 41.7(8) . . ? O98A Cl2 O98 51.9(7) . . ? O95 Cl2 O98 106.0(8) . . ? O96A Cl2 O98 68.5(9) . . ? O96 Cl2 O98 106.5(6) . . ? O98A Cl2 O97A 105.0(12) . . ? O95 Cl2 O97A 95.3(12) . . ? O96A Cl2 O97A 117.6(13) . . ? O96 Cl2 O97A 97.3(10) . . ? O98 Cl2 O97A 140.9(12) . . ? O98A Cl2 O95A 107.1(14) . . ? O95 Cl2 O95A 31.4(12) . . ? O96A Cl2 O95A 112.9(15) . . ? O96 Cl2 O95A 77.7(13) . . ? O98 Cl2 O95A 124.6(13) . . ? O97A Cl2 O95A 90.1(15) . . ? O98A Cl2 O97 91.3(9) . . ? O95 Cl2 O97 121.8(8) . . ? O96A Cl2 O97 101.7(10) . . ? O96 Cl2 O97 104.9(6) . . ? O98 Cl2 O97 109.1(7) . . ? O97A Cl2 O97 33.3(10) . . ? O95A Cl2 O97 123.3(12) . . ? C91 O99 H99O 109.5 . . ? O99 C91 C92 112.2(8) . . ? O99 C91 H91A 109.2 . . ? C92 C91 H91A 109.2 . . ? O99 C91 H91B 109.2 . . ? C92 C91 H91B 109.2 . . ? H91A C91 H91B 107.9 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.899 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.067 # start Validation Reply Form _vrf_PLAT220_Complex1 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.28 Ratio RESPONSE: This is due to the large thermal motion of the methyl carbon atoms of the ligand. Attempts to refine these atoms over two disordered positions converged at occupation factors 0.87 and 0.13 with isotropic model. The anisotropic model for the two positions led to analogous alerts for the site with the largest occupancy. It was thus decided to refine the structure without disorder. ; _vrf_PLAT222_Complex1 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.29 Ratio RESPONSE: This is due to the large thermal motion of the methyl carbon atoms. All hydrogen atoms were introduced at caclulated positions as riding on bonded atoms and were refined with U equal to 1.3 times the Ueq of the respective atom. ; # end Validation Reply Form #===END data_Complex3 _database_code_depnum_ccdc_archive 'CCDC 755833' #TrackingRef 'Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H72 Cl2 Gd N9 Ni O21' _chemical_formula_weight 1602.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.2166(2) _cell_length_b 20.4545(3) _cell_length_c 22.7423(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.0320(10) _cell_angle_gamma 90.00 _cell_volume 6836.27(18) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 41268 _cell_measurement_theta_min 6.83 _cell_measurement_theta_max 71.85 _exptl_crystal_description parallelepiped _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3276 _exptl_absorpt_coefficient_mu 7.962 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.548 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43530 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.1292 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 7.16 _diffrn_reflns_theta_max 65.00 _reflns_number_total 10380 _reflns_number_gt 8044 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(2) _refine_ls_number_reflns 10380 _refine_ls_number_parameters 897 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1454 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd Gd 0.73539(3) 0.04136(2) 0.15575(3) 0.03923(16) Uani 1 1 d . . . Ni Ni 0.54926(10) 0.08097(7) 0.08445(6) 0.0416(4) Uani 1 1 d . . . O1 O 0.5909(4) 0.0454(2) 0.1718(3) 0.0339(14) Uani 1 1 d . . . O3 O 0.8701(4) 0.0970(3) 0.2176(3) 0.0480(16) Uani 1 1 d . . . HO3 H 0.9152 0.1023 0.2033 0.062 Uiso 1 1 calc R . . N1 N 0.4747(5) 0.1409(3) 0.1265(4) 0.0466(19) Uani 1 1 d . . . N2 N 0.7205(5) 0.1093(3) 0.2474(3) 0.0427(18) Uani 1 1 d . . . O31 O 0.6653(4) 0.1358(3) 0.1072(3) 0.0444(15) Uani 1 1 d . . . O33 O 0.8672(4) -0.0128(3) 0.1369(2) 0.0435(15) Uani 1 1 d . . . HO33 H 0.8777 -0.0519 0.1478 0.056 Uiso 1 1 calc R . . N31 N 0.5351(5) 0.1299(4) 0.0047(4) 0.0473(19) Uani 1 1 d . . . N32 N 0.8087(6) 0.0903(3) 0.0752(4) 0.048(2) Uani 1 1 d . . . O61 O 0.6308(4) 0.0072(3) 0.0667(2) 0.0419(15) Uani 1 1 d . . . O63 O 0.7991(4) -0.0246(3) 0.2449(3) 0.0404(15) Uani 1 1 d . . . HO63 H 0.8187 -0.0059 0.2786 0.052 Uiso 1 1 calc R . . N61 N 0.4542(5) 0.0096(4) 0.0573(3) 0.0386(18) Uani 1 1 d . . . N62 N 0.6880(5) -0.0784(3) 0.1541(3) 0.0381(17) Uani 1 1 d . . . C1 C 0.4086(7) 0.1829(5) 0.0979(5) 0.057(3) Uani 1 1 d . . . H1 H 0.4038 0.1938 0.0566 0.074 Uiso 1 1 calc R . . C2 C 0.3478(7) 0.2103(5) 0.1266(5) 0.057(3) Uani 1 1 d . . . H2 H 0.3031 0.2407 0.1062 0.074 Uiso 1 1 calc R . . C3 C 0.3544(7) 0.1919(5) 0.1862(5) 0.057(3) Uani 1 1 d . . . H3 H 0.3125 0.2087 0.2070 0.075 Uiso 1 1 calc R . . C4 C 0.4216(7) 0.1493(4) 0.2154(5) 0.049(2) Uani 1 1 d . . . H4 H 0.4264 0.1364 0.2562 0.064 Uiso 1 1 calc R . . C5 C 0.4815(6) 0.1257(4) 0.1848(4) 0.040(2) Uani 1 1 d . . . C6 C 0.5597(6) 0.0779(4) 0.2147(4) 0.037(2) Uani 1 1 d . . . O2 O 0.5260(4) 0.0341(3) 0.2530(3) 0.0417(15) Uani 1 1 d . . . C7 C 0.6372(7) 0.1149(4) 0.2590(4) 0.046(2) Uani 1 1 d . . . C8 C 0.6264(7) 0.1498(5) 0.3096(5) 0.059(3) Uani 1 1 d . . . H8 H 0.5688 0.1511 0.3185 0.077 Uiso 1 1 calc R . . C9 C 0.6983(8) 0.1818(5) 0.3459(5) 0.063(3) Uani 1 1 d . . . H9 H 0.6904 0.2066 0.3796 0.082 Uiso 1 1 calc R . . C10 C 0.7818(8) 0.1786(4) 0.3344(5) 0.057(3) Uani 1 1 d . . . H10 H 0.8320 0.2016 0.3594 0.074 Uiso 1 1 calc R . . C11 C 0.7928(6) 0.1403(4) 0.2843(4) 0.042(2) Uani 1 1 d . . . C12 C 0.8834(6) 0.1321(4) 0.2726(4) 0.044(2) Uani 1 1 d . . . O4 O 0.9271(5) 0.1920(3) 0.2711(3) 0.0575(19) Uani 1 1 d . . . C13 C 0.9464(6) 0.0933(4) 0.3259(4) 0.044(2) Uani 1 1 d . . . C14 C 1.0236(7) 0.1183(5) 0.3642(5) 0.069(3) Uani 1 1 d . . . H14 H 1.0423 0.1616 0.3583 0.090 Uiso 1 1 calc R . . C15 C 1.0748(8) 0.0803(6) 0.4119(6) 0.076(4) Uani 1 1 d . . . H15 H 1.1283 0.0972 0.4390 0.098 Uiso 1 1 calc R . . C16 C 1.0455(8) 0.0178(5) 0.4183(5) 0.066(3) Uani 1 1 d . . . H16 H 1.0790 -0.0103 0.4493 0.086 Uiso 1 1 calc R . . C17 C 0.9675(7) -0.0024(5) 0.3790(4) 0.055(3) Uani 1 1 d . . . H17 H 0.9461 -0.0449 0.3848 0.072 Uiso 1 1 calc R . . N3 N 0.9177(6) 0.0334(4) 0.3323(4) 0.049(2) Uani 1 1 d . . . C18 C 0.4620(7) -0.0131(5) 0.2187(5) 0.056(3) Uani 1 1 d D . . H18A H 0.4938 -0.0449 0.1987 0.073 Uiso 1 1 calc R . . H18B H 0.4147 0.0093 0.1869 0.073 Uiso 1 1 calc R . . C19 C 0.4190(9) -0.0478(6) 0.2630(5) 0.080(4) Uani 1 1 d D . . H19A H 0.3682 -0.0748 0.2403 0.104 Uiso 1 1 calc R . . H19B H 0.3966 -0.0154 0.2873 0.104 Uiso 1 1 calc R . . H19C H 0.4645 -0.0757 0.2899 0.104 Uiso 1 1 calc R . . C20 C 0.8785(8) 0.2351(5) 0.2238(6) 0.073(4) Uani 1 1 d D . . H20A H 0.8434 0.2671 0.2413 0.095 Uiso 1 1 calc R . . H20B H 0.8350 0.2095 0.1924 0.095 Uiso 1 1 calc R . . C21 C 0.9409(11) 0.2699(10) 0.1959(10) 0.185(11) Uani 1 1 d D . . H21A H 0.9858 0.2937 0.2273 0.241 Uiso 1 1 calc R . . H21B H 0.9067 0.3008 0.1656 0.241 Uiso 1 1 calc R . . H21C H 0.9723 0.2384 0.1759 0.241 Uiso 1 1 calc R . . C31 C 0.4610(7) 0.1278(5) -0.0439(4) 0.053(3) Uani 1 1 d . . . H31 H 0.4121 0.0994 -0.0427 0.069 Uiso 1 1 calc R . . C32 C 0.4551(8) 0.1659(6) -0.0947(5) 0.071(3) Uani 1 1 d . . . H32 H 0.4025 0.1645 -0.1281 0.092 Uiso 1 1 calc R . . C33 C 0.5256(10) 0.2051(7) -0.0959(6) 0.102(5) Uani 1 1 d . . . H33 H 0.5230 0.2303 -0.1315 0.132 Uiso 1 1 calc R . . C34 C 0.6017(9) 0.2102(7) -0.0474(6) 0.088(4) Uani 1 1 d . . . H34 H 0.6498 0.2397 -0.0478 0.114 Uiso 1 1 calc R . . C35 C 0.6042(7) 0.1682(5) 0.0040(4) 0.050(3) Uani 1 1 d . . . C36 C 0.6865(7) 0.1711(4) 0.0608(4) 0.047(2) Uani 1 1 d . . . O32 O 0.7084(5) 0.2377(3) 0.0783(3) 0.0530(17) Uani 1 1 d . . . C37 C 0.7735(6) 0.1459(4) 0.0485(4) 0.040(2) Uani 1 1 d . . . C38 C 0.8196(7) 0.1799(5) 0.0105(4) 0.048(2) Uani 1 1 d . . . H38 H 0.7970 0.2207 -0.0072 0.063 Uiso 1 1 calc R . . C39 C 0.8951(7) 0.1540(5) 0.0000(5) 0.053(3) Uani 1 1 d . . . H39 H 0.9244 0.1757 -0.0267 0.069 Uiso 1 1 calc R . . C40 C 0.9308(7) 0.0960(5) 0.0277(4) 0.049(2) Uani 1 1 d . . . H40 H 0.9846 0.0775 0.0208 0.064 Uiso 1 1 calc R . . C41 C 0.8851(6) 0.0659(4) 0.0659(4) 0.039(2) Uani 1 1 d . . . C42 C 0.9271(7) 0.0066(4) 0.1020(4) 0.042(2) Uani 1 1 d . . . O34 O 0.9391(5) -0.0451(3) 0.0645(3) 0.0527(18) Uani 1 1 d . . . C43 C 1.0213(7) 0.0228(5) 0.1413(4) 0.045(2) Uani 1 1 d . . . C44 C 1.0986(7) 0.0067(5) 0.1255(5) 0.058(3) Uani 1 1 d . . . H44 H 1.0960 -0.0194 0.0905 0.075 Uiso 1 1 calc R . . C45 C 1.1832(8) 0.0292(6) 0.1617(6) 0.071(3) Uani 1 1 d . . . H45 H 1.2383 0.0190 0.1515 0.092 Uiso 1 1 calc R . . C46 C 1.1834(9) 0.0652(6) 0.2106(5) 0.070(3) Uani 1 1 d . . . H46 H 1.2398 0.0790 0.2366 0.092 Uiso 1 1 calc R . . C47 C 1.1038(8) 0.0826(5) 0.2241(5) 0.064(3) Uani 1 1 d . . . H47 H 1.1060 0.1111 0.2574 0.083 Uiso 1 1 calc R . . N33 N 1.0221(6) 0.0601(4) 0.1911(4) 0.052(2) Uani 1 1 d . . . C48 C 0.6384(9) 0.2702(5) 0.0999(7) 0.087(4) Uani 1 1 d D . . H48A H 0.6309 0.2491 0.1375 0.113 Uiso 1 1 calc R . . H48B H 0.5795 0.2688 0.0686 0.113 Uiso 1 1 calc R . . C49 C 0.6707(13) 0.3399(6) 0.1124(9) 0.159(9) Uani 1 1 d D . . H49A H 0.6398 0.3600 0.1407 0.206 Uiso 1 1 calc R . . H49B H 0.6566 0.3646 0.0742 0.206 Uiso 1 1 calc R . . H49C H 0.7365 0.3402 0.1305 0.206 Uiso 1 1 calc R . . C50 C 0.8587(8) -0.0683(6) 0.0220(6) 0.073(3) Uani 1 1 d D . . H50A H 0.8492 -0.0437 -0.0166 0.094 Uiso 1 1 calc R . . H50B H 0.8054 -0.0606 0.0385 0.094 Uiso 1 1 calc R . . C51 C 0.8661(14) -0.1390(6) 0.0100(8) 0.173(10) Uani 1 1 d D . . H51A H 0.9225 -0.1472 -0.0019 0.224 Uiso 1 1 calc R . . H51B H 0.8139 -0.1526 -0.0229 0.224 Uiso 1 1 calc R . . H51C H 0.8668 -0.1639 0.0470 0.224 Uiso 1 1 calc R . . C61 C 0.3632(6) 0.0163(5) 0.0505(4) 0.042(2) Uani 1 1 d . . . H61 H 0.3407 0.0574 0.0596 0.055 Uiso 1 1 calc R . . C62 C 0.3033(8) -0.0328(5) 0.0315(5) 0.058(3) Uani 1 1 d . . . H62 H 0.2402 -0.0265 0.0276 0.076 Uiso 1 1 calc R . . C63 C 0.3362(8) -0.0933(6) 0.0177(5) 0.076(4) Uani 1 1 d . . . H63 H 0.2955 -0.1286 0.0040 0.099 Uiso 1 1 calc R . . C64 C 0.4285(8) -0.1011(6) 0.0243(5) 0.069(3) Uani 1 1 d . . . H64 H 0.4523 -0.1418 0.0155 0.090 Uiso 1 1 calc R . . C65 C 0.4865(7) -0.0474(5) 0.0442(4) 0.045(2) Uani 1 1 d . . . C66 C 0.5884(7) -0.0532(5) 0.0541(4) 0.044(2) Uani 1 1 d . . . O62 O 0.6078(5) -0.0838(3) 0.0009(3) 0.0553(18) Uani 1 1 d . . . C67 C 0.6300(6) -0.1034(4) 0.1040(4) 0.044(2) Uani 1 1 d . . . C68 C 0.6092(7) -0.1685(5) 0.0985(5) 0.054(3) Uani 1 1 d . . . H68 H 0.5725 -0.1851 0.0612 0.070 Uiso 1 1 calc R . . C69 C 0.6416(7) -0.2104(5) 0.1474(4) 0.052(3) Uani 1 1 d . . . H69 H 0.6259 -0.2555 0.1445 0.067 Uiso 1 1 calc R . . C70 C 0.6971(6) -0.1851(4) 0.2000(4) 0.044(2) Uani 1 1 d . . . H70 H 0.7178 -0.2115 0.2353 0.057 Uiso 1 1 calc R . . C71 C 0.7216(6) -0.1204(4) 0.2000(4) 0.0326(18) Uani 1 1 d . . . C72 C 0.7940(7) -0.0919(4) 0.2542(4) 0.042(2) Uani 1 1 d . . . O64 O 0.7751(4) -0.1064(3) 0.3102(3) 0.0483(16) Uani 1 1 d . . . C73 C 0.8854(6) -0.1260(4) 0.2571(4) 0.040(2) Uani 1 1 d . . . C74 C 0.9240(7) -0.1699(4) 0.3032(4) 0.047(2) Uani 1 1 d . . . H74 H 0.8967 -0.1794 0.3353 0.061 Uiso 1 1 calc R . . C75 C 1.0054(7) -0.1992(5) 0.2995(5) 0.058(3) Uani 1 1 d . . . H75 H 1.0361 -0.2283 0.3307 0.076 Uiso 1 1 calc R . . C76 C 1.0408(8) -0.1865(5) 0.2521(5) 0.062(3) Uani 1 1 d . . . H76 H 1.0943 -0.2083 0.2486 0.081 Uiso 1 1 calc R . . C77 C 0.9985(7) -0.1417(5) 0.2088(5) 0.066(3) Uani 1 1 d . . . H77 H 1.0251 -0.1320 0.1764 0.086 Uiso 1 1 calc R . . N63 N 0.9219(5) -0.1115(4) 0.2107(3) 0.047(2) Uani 1 1 d . . . C78 C 0.5876(12) -0.0458(6) -0.0538(6) 0.107(6) Uani 1 1 d D . . H78A H 0.6358 -0.0535 -0.0751 0.139 Uiso 1 1 calc R . . H78B H 0.5895 0.0011 -0.0427 0.139 Uiso 1 1 calc R . . C79 C 0.4991(13) -0.0600(11) -0.0960(7) 0.194(11) Uani 1 1 d DU . . H79A H 0.4901 -0.0315 -0.1317 0.252 Uiso 1 1 calc R . . H79B H 0.4507 -0.0521 -0.0756 0.252 Uiso 1 1 calc R . . H79C H 0.4974 -0.1058 -0.1088 0.252 Uiso 1 1 calc R . . C80 C 0.6866(8) -0.0846(6) 0.3144(5) 0.067(3) Uani 1 1 d D . . H80A H 0.6393 -0.1163 0.2942 0.088 Uiso 1 1 calc R . . H80B H 0.6720 -0.0416 0.2943 0.088 Uiso 1 1 calc R . . C81 C 0.6896(14) -0.0794(12) 0.3796(6) 0.188(11) Uani 1 1 d DU . . H81A H 0.6303 -0.0648 0.3839 0.245 Uiso 1 1 calc R . . H81B H 0.7364 -0.0477 0.3992 0.245 Uiso 1 1 calc R . . H81C H 0.7042 -0.1222 0.3991 0.245 Uiso 1 1 calc R . . Cl1 Cl 0.2703(2) 0.19300(14) 0.35790(12) 0.0674(8) Uani 1 1 d D . . O91 O 0.3310(12) 0.2289(8) 0.4045(7) 0.100(6) Uiso 0.55 1 d PD A 1 O92 O 0.2422(13) 0.1314(8) 0.3755(8) 0.117(6) Uiso 0.55 1 d PD A 1 O93 O 0.1936(14) 0.2200(12) 0.3121(10) 0.160(11) Uiso 0.55 1 d PD A 1 O94 O 0.3086(10) 0.1890(8) 0.3076(6) 0.085(4) Uiso 0.55 1 d PD A 1 O91A O 0.364(3) 0.2184(18) 0.3790(18) 0.194(16) Uiso 0.45 1 d P A 2 O92A O 0.2357(12) 0.1788(9) 0.4072(8) 0.074(5) Uiso 0.45 1 d P A 2 O93A O 0.1846(16) 0.2384(12) 0.3402(11) 0.101(8) Uiso 0.45 1 d P A 2 O94A O 0.2985(18) 0.1268(12) 0.3417(12) 0.126(8) Uiso 0.45 1 d P A 2 Cl2 Cl 0.65605(19) 0.34296(13) 0.48659(12) 0.0592(7) Uani 1 1 d . . . O95 O 0.6757(6) 0.4019(4) 0.5211(4) 0.108(3) Uani 1 1 d . . . O96 O 0.6341(7) 0.2949(5) 0.5238(5) 0.133(4) Uani 1 1 d . . . O97 O 0.7340(6) 0.3250(6) 0.4680(5) 0.117(4) Uani 1 1 d . . . O98 O 0.5818(6) 0.3574(4) 0.4354(3) 0.088(3) Uani 1 1 d . . . O99 O 0.7366(7) 0.3565(5) 0.3411(4) 0.095(3) Uani 1 1 d . . . H99 H 0.7299 0.3459 0.3754 0.124 Uiso 1 1 calc R . . C91 C 0.7020(11) 0.4207(6) 0.3260(6) 0.088(4) Uani 1 1 d . . . H91A H 0.6373 0.4221 0.3267 0.115 Uiso 1 1 calc R . . H91B H 0.7056 0.4316 0.2843 0.115 Uiso 1 1 calc R . . C92 C 0.7534(11) 0.4694(7) 0.3689(6) 0.099(5) Uani 1 1 d . . . H92A H 0.7216 0.5115 0.3620 0.128 Uiso 1 1 calc R . . H92B H 0.8144 0.4743 0.3626 0.128 Uiso 1 1 calc R . . H92C H 0.7585 0.4549 0.4107 0.128 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 Gd 0.0288(3) 0.0359(3) 0.0523(3) 0.0047(2) 0.0092(2) 0.0029(3) Ni 0.0341(10) 0.0386(8) 0.0514(9) 0.0060(7) 0.0096(7) 0.0010(7) O1 0.023(4) 0.034(3) 0.044(3) -0.005(2) 0.008(3) 0.003(2) O3 0.041(4) 0.042(4) 0.063(4) 0.001(3) 0.018(3) 0.003(3) N1 0.036(5) 0.038(4) 0.068(5) 0.005(4) 0.016(4) -0.007(4) N2 0.043(5) 0.032(4) 0.052(4) -0.001(3) 0.010(4) 0.006(3) O31 0.044(4) 0.038(3) 0.056(4) 0.019(3) 0.023(3) 0.007(3) O33 0.048(4) 0.037(3) 0.047(3) 0.003(3) 0.015(3) 0.021(3) N31 0.033(5) 0.048(5) 0.059(5) 0.003(4) 0.010(4) -0.003(4) N32 0.044(5) 0.034(4) 0.066(5) 0.004(3) 0.017(4) -0.005(4) O61 0.036(4) 0.047(4) 0.040(3) 0.000(3) 0.004(3) -0.003(3) O63 0.052(4) 0.024(3) 0.041(3) 0.011(2) 0.005(3) 0.012(3) N61 0.034(5) 0.043(4) 0.036(4) -0.001(3) 0.004(3) 0.013(4) N62 0.026(4) 0.030(4) 0.054(4) 0.007(3) 0.003(3) -0.002(3) C1 0.042(7) 0.040(5) 0.086(7) 0.011(5) 0.015(6) 0.005(5) C2 0.030(6) 0.045(6) 0.092(8) -0.005(5) 0.008(5) 0.008(5) C3 0.044(7) 0.054(6) 0.072(7) 0.000(5) 0.013(6) 0.018(5) C4 0.036(6) 0.035(5) 0.077(7) -0.003(4) 0.015(5) 0.009(4) C5 0.036(6) 0.033(5) 0.055(5) -0.006(4) 0.016(4) -0.002(4) C6 0.022(5) 0.035(5) 0.055(5) 0.001(4) 0.007(4) 0.004(4) O2 0.035(4) 0.039(3) 0.052(4) 0.008(3) 0.014(3) 0.002(3) C7 0.039(6) 0.035(5) 0.063(6) -0.001(4) 0.012(5) 0.016(4) C8 0.038(7) 0.061(7) 0.071(7) -0.017(5) 0.001(5) 0.015(5) C9 0.042(7) 0.065(7) 0.073(7) -0.013(5) 0.000(6) 0.024(6) C10 0.049(7) 0.040(5) 0.075(7) -0.018(5) 0.003(6) 0.009(5) C11 0.029(6) 0.030(4) 0.058(5) -0.011(4) -0.006(4) -0.001(4) C12 0.035(6) 0.040(5) 0.053(5) -0.005(4) 0.005(4) -0.005(4) O4 0.052(5) 0.038(4) 0.075(5) 0.006(3) 0.003(4) -0.009(3) C13 0.033(6) 0.040(5) 0.056(5) 0.000(4) 0.006(4) 0.008(4) C14 0.039(7) 0.057(7) 0.093(8) -0.002(6) -0.017(6) -0.017(5) C15 0.045(8) 0.078(9) 0.086(8) -0.007(7) -0.014(6) 0.001(6) C16 0.062(8) 0.049(6) 0.076(7) 0.007(6) -0.004(6) 0.002(6) C17 0.044(7) 0.058(6) 0.058(6) -0.003(5) 0.002(5) 0.000(5) N3 0.036(5) 0.043(5) 0.055(5) 0.007(3) -0.011(4) 0.008(4) C18 0.055(7) 0.051(6) 0.068(6) -0.005(5) 0.026(6) -0.012(5) C19 0.077(10) 0.092(9) 0.078(8) 0.029(6) 0.030(7) -0.029(7) C20 0.068(9) 0.038(6) 0.102(9) 0.007(6) 0.000(7) -0.006(6) C21 0.083(13) 0.22(2) 0.27(2) 0.17(2) 0.069(15) 0.004(13) C31 0.040(7) 0.063(6) 0.053(6) 0.019(5) 0.003(5) 0.012(5) C32 0.037(7) 0.093(9) 0.073(7) 0.041(6) -0.002(6) 0.001(6) C33 0.074(10) 0.109(11) 0.096(10) 0.057(9) -0.024(8) -0.020(8) C34 0.062(9) 0.106(10) 0.089(9) 0.061(8) 0.008(7) -0.010(7) C35 0.044(7) 0.057(6) 0.044(5) 0.024(4) 0.003(5) 0.018(5) C36 0.042(6) 0.033(5) 0.064(6) 0.014(4) 0.011(5) -0.007(4) O32 0.055(5) 0.039(4) 0.073(4) 0.010(3) 0.032(4) 0.002(3) C37 0.038(6) 0.035(5) 0.050(5) 0.016(4) 0.017(4) -0.002(4) C38 0.036(6) 0.049(6) 0.066(6) 0.009(5) 0.025(5) 0.004(5) C39 0.044(7) 0.051(6) 0.067(6) 0.018(5) 0.019(5) 0.001(5) C40 0.040(6) 0.055(6) 0.059(6) 0.002(5) 0.022(5) 0.005(5) C41 0.017(5) 0.047(5) 0.052(5) 0.007(4) 0.007(4) 0.002(4) C42 0.043(6) 0.037(5) 0.051(5) 0.005(4) 0.019(4) 0.005(4) O34 0.035(5) 0.052(4) 0.073(5) 0.001(3) 0.019(4) 0.006(3) C43 0.024(6) 0.053(6) 0.056(6) 0.004(5) 0.006(4) 0.004(4) C44 0.042(7) 0.055(6) 0.075(7) 0.015(5) 0.015(6) 0.004(5) C45 0.034(8) 0.094(9) 0.085(9) 0.013(7) 0.015(6) 0.003(6) C46 0.046(8) 0.090(9) 0.068(7) -0.003(6) 0.003(6) 0.005(7) C47 0.047(8) 0.072(8) 0.067(7) -0.003(6) 0.006(6) -0.005(6) N33 0.031(5) 0.054(5) 0.069(5) -0.003(4) 0.010(4) -0.003(4) C48 0.085(10) 0.052(7) 0.157(13) 0.012(8) 0.090(10) 0.020(7) C49 0.22(2) 0.043(7) 0.29(2) -0.023(11) 0.201(19) -0.003(10) C50 0.050(8) 0.074(8) 0.088(8) -0.015(7) 0.007(7) -0.005(6) C51 0.23(2) 0.052(8) 0.178(18) -0.020(10) -0.054(17) 0.021(12) C61 0.025(6) 0.054(6) 0.044(5) 0.005(4) 0.001(4) -0.002(4) C62 0.039(7) 0.059(7) 0.072(7) -0.006(5) 0.007(6) -0.009(5) C63 0.047(8) 0.069(8) 0.097(9) -0.026(7) -0.007(7) 0.003(6) C64 0.045(8) 0.066(7) 0.087(8) -0.011(6) 0.000(6) 0.001(6) C65 0.034(7) 0.056(6) 0.042(5) 0.000(4) 0.003(4) 0.002(4) C66 0.033(6) 0.057(6) 0.042(5) -0.008(4) 0.009(4) 0.000(5) O62 0.065(5) 0.064(4) 0.039(3) -0.007(3) 0.016(3) 0.017(4) C67 0.037(6) 0.044(5) 0.049(5) 0.001(4) 0.012(4) 0.004(4) C68 0.053(7) 0.042(5) 0.063(6) 0.004(5) 0.009(5) -0.002(5) C69 0.045(7) 0.041(5) 0.069(6) 0.003(5) 0.014(5) 0.015(5) C70 0.044(6) 0.034(5) 0.053(5) 0.011(4) 0.009(5) 0.001(4) C71 0.025(5) 0.037(4) 0.041(4) -0.003(4) 0.017(4) 0.014(4) C72 0.052(7) 0.029(4) 0.045(5) 0.004(4) 0.012(5) 0.008(4) O64 0.042(4) 0.051(4) 0.053(4) 0.005(3) 0.014(3) 0.013(3) C73 0.037(6) 0.034(5) 0.046(5) 0.005(4) 0.001(4) 0.004(4) C74 0.047(7) 0.040(5) 0.049(5) -0.001(4) 0.003(5) 0.004(4) C75 0.045(7) 0.048(6) 0.076(7) 0.008(5) 0.008(6) 0.017(5) C76 0.043(7) 0.051(6) 0.088(8) 0.010(6) 0.008(6) 0.018(5) C77 0.042(7) 0.074(8) 0.086(8) 0.014(6) 0.025(6) 0.027(6) N63 0.042(5) 0.037(4) 0.062(5) 0.007(4) 0.015(4) 0.010(4) C78 0.177(19) 0.090(10) 0.055(8) 0.026(6) 0.030(10) 0.026(10) C79 0.16(2) 0.36(3) 0.060(10) 0.072(14) 0.028(12) 0.10(2) C80 0.062(9) 0.073(8) 0.069(7) 0.010(6) 0.019(6) 0.026(6) C81 0.172(19) 0.33(3) 0.086(12) 0.017(14) 0.073(12) 0.128(19) Cl1 0.082(2) 0.0620(16) 0.0609(15) 0.0002(13) 0.0236(15) -0.0233(16) Cl2 0.0481(17) 0.0574(15) 0.0675(15) 0.0126(12) 0.0066(13) -0.0075(13) O95 0.084(7) 0.089(6) 0.138(8) -0.040(6) 0.004(6) -0.015(5) O96 0.123(8) 0.109(7) 0.156(9) 0.095(7) 0.016(7) -0.028(6) O97 0.061(7) 0.170(11) 0.116(7) 0.000(7) 0.014(6) 0.041(7) O98 0.071(6) 0.107(7) 0.065(5) 0.014(4) -0.020(4) 0.004(5) O99 0.092(7) 0.088(7) 0.108(7) 0.005(5) 0.029(6) -0.001(6) C91 0.111(13) 0.073(9) 0.077(8) -0.003(7) 0.018(8) -0.010(9) C92 0.100(13) 0.109(12) 0.081(10) 0.022(8) 0.012(8) -0.017(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O1 2.321(6) . ? Gd O61 2.335(5) . ? Gd O31 2.340(5) . ? Gd O63 2.419(5) . ? Gd O33 2.425(6) . ? Gd O3 2.446(6) . ? Gd N62 2.552(6) . ? Gd N2 2.563(7) . ? Gd N32 2.580(8) . ? Gd Ni 2.9875(16) . ? Ni N31 2.034(8) . ? Ni N61 2.034(8) . ? Ni O31 2.041(6) . ? Ni O1 2.055(6) . ? Ni O61 2.060(6) . ? Ni N1 2.066(8) . ? O1 C6 1.364(10) . ? O3 C12 1.409(10) . ? O3 HO3 0.8400 . ? N1 C5 1.339(10) . ? N1 C1 1.353(11) . ? N2 C11 1.356(10) . ? N2 C7 1.365(11) . ? O31 C36 1.383(10) . ? O33 C42 1.412(10) . ? O33 HO33 0.8400 . ? N31 C35 1.314(12) . ? N31 C31 1.360(11) . ? N32 C41 1.332(11) . ? N32 C37 1.336(10) . ? O61 C66 1.389(11) . ? O63 C72 1.398(9) . ? O63 HO63 0.8400 . ? N61 C65 1.330(11) . ? N61 C61 1.361(11) . ? N62 C71 1.345(9) . ? N62 C67 1.349(11) . ? C1 C2 1.384(13) . ? C1 H1 0.9500 . ? C2 C3 1.385(14) . ? C2 H2 0.9500 . ? C3 C4 1.377(12) . ? C3 H3 0.9500 . ? C4 C5 1.371(12) . ? C4 H4 0.9500 . ? C5 C6 1.554(11) . ? C6 O2 1.435(10) . ? C6 C7 1.536(12) . ? O2 C18 1.447(11) . ? C7 C8 1.399(13) . ? C8 C9 1.356(14) . ? C8 H8 0.9500 . ? C9 C10 1.364(15) . ? C9 H9 0.9500 . ? C10 C11 1.428(12) . ? C10 H10 0.9500 . ? C11 C12 1.481(13) . ? C12 O4 1.397(10) . ? C12 C13 1.554(12) . ? O4 C20 1.438(12) . ? C13 N3 1.322(11) . ? C13 C14 1.367(13) . ? C14 C15 1.396(15) . ? C14 H14 0.9500 . ? C15 C16 1.375(15) . ? C15 H15 0.9500 . ? C16 C17 1.351(13) . ? C16 H16 0.9500 . ? C17 N3 1.350(11) . ? C17 H17 0.9500 . ? C18 C19 1.511(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.458(13) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C31 C32 1.377(12) . ? C31 H31 0.9500 . ? C32 C33 1.347(15) . ? C32 H32 0.9500 . ? C33 C34 1.381(16) . ? C33 H33 0.9500 . ? C34 C35 1.443(12) . ? C34 H34 0.9500 . ? C35 C36 1.550(13) . ? C36 O32 1.434(10) . ? C36 C37 1.513(13) . ? O32 C48 1.445(11) . ? C37 C38 1.427(11) . ? C38 C39 1.342(13) . ? C38 H38 0.9500 . ? C39 C40 1.388(12) . ? C39 H39 0.9500 . ? C40 C41 1.391(12) . ? C40 H40 0.9500 . ? C41 C42 1.509(12) . ? C42 O34 1.399(10) . ? C42 C43 1.517(13) . ? O34 C50 1.429(12) . ? C43 C44 1.357(14) . ? C43 N33 1.365(12) . ? C44 C45 1.412(15) . ? C44 H44 0.9500 . ? C45 C46 1.333(16) . ? C45 H45 0.9500 . ? C46 C47 1.371(15) . ? C46 H46 0.9500 . ? C47 N33 1.354(13) . ? C47 H47 0.9500 . ? C48 C49 1.510(13) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.481(13) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C61 C62 1.350(12) . ? C61 H61 0.9500 . ? C62 C63 1.401(14) . ? C62 H62 0.9500 . ? C63 C64 1.382(15) . ? C63 H63 0.9500 . ? C64 C65 1.408(13) . ? C64 H64 0.9500 . ? C65 C66 1.514(14) . ? C66 O62 1.458(10) . ? C66 C67 1.537(12) . ? O62 C78 1.432(12) . ? C67 C68 1.367(12) . ? C68 C69 1.389(12) . ? C68 H68 0.9500 . ? C69 C70 1.374(12) . ? C69 H69 0.9500 . ? C70 C71 1.376(11) . ? C70 H70 0.9500 . ? C71 C72 1.538(11) . ? C72 O64 1.408(10) . ? C72 C73 1.541(12) . ? O64 C80 1.445(12) . ? C73 N63 1.348(11) . ? C73 C74 1.389(11) . ? C74 C75 1.399(13) . ? C74 H74 0.9500 . ? C75 C76 1.350(14) . ? C75 H75 0.9500 . ? C76 C77 1.376(13) . ? C76 H76 0.9500 . ? C77 N63 1.331(11) . ? C77 H77 0.9500 . ? C78 C79 1.465(16) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.476(13) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? Cl1 O92A 1.386(17) . ? Cl1 O94 1.414(12) . ? Cl1 O91 1.417(13) . ? Cl1 O92 1.421(13) . ? Cl1 O93 1.457(15) . ? Cl1 O91A 1.48(4) . ? Cl1 O94A 1.49(3) . ? Cl1 O93A 1.57(2) . ? Cl2 O96 1.392(8) . ? Cl2 O97 1.408(9) . ? Cl2 O98 1.427(7) . ? Cl2 O95 1.427(8) . ? O99 C91 1.424(14) . ? O99 H99 0.8400 . ? C91 C92 1.469(16) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd O61 71.7(2) . . ? O1 Gd O31 73.16(19) . . ? O61 Gd O31 73.3(2) . . ? O1 Gd O63 94.5(2) . . ? O61 Gd O63 126.5(2) . . ? O31 Gd O63 153.0(2) . . ? O1 Gd O33 154.78(19) . . ? O61 Gd O33 96.8(2) . . ? O31 Gd O33 126.2(2) . . ? O63 Gd O33 73.9(2) . . ? O1 Gd O3 125.4(2) . . ? O61 Gd O3 156.9(2) . . ? O31 Gd O3 95.7(2) . . ? O63 Gd O3 71.6(2) . . ? O33 Gd O3 72.9(2) . . ? O1 Gd N62 76.2(2) . . ? O61 Gd N62 64.7(2) . . ? O31 Gd N62 133.9(2) . . ? O63 Gd N62 61.7(2) . . ? O33 Gd N62 78.6(2) . . ? O3 Gd N62 130.3(2) . . ? O1 Gd N2 64.3(2) . . ? O61 Gd N2 133.1(2) . . ? O31 Gd N2 79.1(2) . . ? O63 Gd N2 73.9(2) . . ? O33 Gd N2 130.0(2) . . ? O3 Gd N2 61.2(2) . . ? N62 Gd N2 116.6(2) . . ? O1 Gd N32 134.3(2) . . ? O61 Gd N32 79.8(2) . . ? O31 Gd N32 64.7(2) . . ? O63 Gd N32 131.2(2) . . ? O33 Gd N32 61.5(2) . . ? O3 Gd N32 77.0(2) . . ? N62 Gd N32 122.3(2) . . ? N2 Gd N32 120.8(2) . . ? O1 Gd Ni 43.32(14) . . ? O61 Gd Ni 43.41(15) . . ? O31 Gd Ni 42.94(16) . . ? O63 Gd Ni 136.35(15) . . ? O33 Gd Ni 137.67(13) . . ? O3 Gd Ni 136.13(14) . . ? N62 Gd Ni 91.62(16) . . ? N2 Gd Ni 91.30(17) . . ? N32 Gd Ni 91.89(18) . . ? N31 Ni N61 100.4(3) . . ? N31 Ni O31 80.8(3) . . ? N61 Ni O31 166.1(3) . . ? N31 Ni O1 166.2(3) . . ? N61 Ni O1 93.2(2) . . ? O31 Ni O1 85.4(2) . . ? N31 Ni O61 96.7(3) . . ? N61 Ni O61 80.3(3) . . ? O31 Ni O61 85.8(2) . . ? O1 Ni O61 83.1(2) . . ? N31 Ni N1 100.2(3) . . ? N61 Ni N1 97.7(3) . . ? O31 Ni N1 95.7(3) . . ? O1 Ni N1 80.3(3) . . ? O61 Ni N1 163.1(3) . . ? N31 Ni Gd 118.9(2) . . ? N61 Ni Gd 118.0(2) . . ? O31 Ni Gd 51.36(16) . . ? O1 Ni Gd 50.81(17) . . ? O61 Ni Gd 51.16(15) . . ? N1 Ni Gd 117.8(2) . . ? C6 O1 Ni 116.2(5) . . ? C6 O1 Gd 130.5(5) . . ? Ni O1 Gd 85.9(2) . . ? C12 O3 Gd 130.8(5) . . ? C12 O3 HO3 109.5 . . ? Gd O3 HO3 119.0 . . ? C5 N1 C1 118.8(9) . . ? C5 N1 Ni 114.2(6) . . ? C1 N1 Ni 125.6(7) . . ? C11 N2 C7 119.0(8) . . ? C11 N2 Gd 121.9(6) . . ? C7 N2 Gd 119.1(6) . . ? C36 O31 Ni 116.8(5) . . ? C36 O31 Gd 128.5(6) . . ? Ni O31 Gd 85.7(2) . . ? C42 O33 Gd 130.9(5) . . ? C42 O33 HO33 109.5 . . ? Gd O33 HO33 119.0 . . ? C35 N31 C31 120.4(8) . . ? C35 N31 Ni 113.9(6) . . ? C31 N31 Ni 125.6(7) . . ? C41 N32 C37 120.6(8) . . ? C41 N32 Gd 121.6(6) . . ? C37 N32 Gd 117.3(6) . . ? C66 O61 Ni 114.9(6) . . ? C66 O61 Gd 128.4(5) . . ? Ni O61 Gd 85.4(2) . . ? C72 O63 Gd 130.6(5) . . ? C72 O63 HO63 109.5 . . ? Gd O63 HO63 118.7 . . ? C65 N61 C61 119.1(9) . . ? C65 N61 Ni 115.0(7) . . ? C61 N61 Ni 125.9(6) . . ? C71 N62 C67 116.7(7) . . ? C71 N62 Gd 123.5(5) . . ? C67 N62 Gd 119.7(5) . . ? N1 C1 C2 122.3(11) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C1 C2 C3 117.8(10) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 119.9(10) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 119.2(10) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 122.0(9) . . ? N1 C5 C6 115.7(8) . . ? C4 C5 C6 122.3(8) . . ? O1 C6 O2 112.1(6) . . ? O1 C6 C7 111.1(7) . . ? O2 C6 C7 104.1(7) . . ? O1 C6 C5 111.2(7) . . ? O2 C6 C5 107.7(7) . . ? C7 C6 C5 110.3(7) . . ? C6 O2 C18 112.7(7) . . ? N2 C7 C8 121.0(9) . . ? N2 C7 C6 115.1(8) . . ? C8 C7 C6 123.9(9) . . ? C9 C8 C7 120.0(11) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.2(11) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 119.2(10) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N2 C11 C10 120.4(9) . . ? N2 C11 C12 118.7(8) . . ? C10 C11 C12 120.9(8) . . ? O4 C12 O3 112.6(8) . . ? O4 C12 C11 112.1(8) . . ? O3 C12 C11 106.9(7) . . ? O4 C12 C13 105.4(7) . . ? O3 C12 C13 110.5(7) . . ? C11 C12 C13 109.4(8) . . ? C12 O4 C20 113.6(7) . . ? N3 C13 C14 122.1(9) . . ? N3 C13 C12 113.9(8) . . ? C14 C13 C12 124.0(9) . . ? C13 C14 C15 120.0(10) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 118.0(10) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? C17 C16 C15 117.8(10) . . ? C17 C16 H16 121.1 . . ? C15 C16 H16 121.1 . . ? N3 C17 C16 124.9(10) . . ? N3 C17 H17 117.5 . . ? C16 C17 H17 117.5 . . ? C13 N3 C17 117.1(8) . . ? O2 C18 C19 107.5(8) . . ? O2 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? O2 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C20 C21 111.0(11) . . ? O4 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? O4 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N31 C31 C32 121.6(10) . . ? N31 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C33 C32 C31 118.4(11) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C32 C33 C34 122.4(11) . . ? C32 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? C33 C34 C35 116.3(11) . . ? C33 C34 H34 121.9 . . ? C35 C34 H34 121.9 . . ? N31 C35 C34 120.8(9) . . ? N31 C35 C36 119.2(8) . . ? C34 C35 C36 119.9(10) . . ? O31 C36 O32 111.6(8) . . ? O31 C36 C37 110.6(7) . . ? O32 C36 C37 102.8(7) . . ? O31 C36 C35 108.5(8) . . ? O32 C36 C35 110.3(7) . . ? C37 C36 C35 112.9(8) . . ? C36 O32 C48 113.1(8) . . ? N32 C37 C38 119.3(9) . . ? N32 C37 C36 118.1(7) . . ? C38 C37 C36 122.5(8) . . ? C39 C38 C37 119.6(9) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 120.7(9) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C41 117.5(9) . . ? C39 C40 H40 121.2 . . ? C41 C40 H40 121.2 . . ? N32 C41 C40 122.2(8) . . ? N32 C41 C42 118.5(8) . . ? C40 C41 C42 119.0(8) . . ? O34 C42 O33 109.6(7) . . ? O34 C42 C41 112.3(8) . . ? O33 C42 C41 106.7(7) . . ? O34 C42 C43 105.7(8) . . ? O33 C42 C43 112.2(8) . . ? C41 C42 C43 110.4(8) . . ? C42 O34 C50 116.0(8) . . ? C44 C43 N33 122.3(9) . . ? C44 C43 C42 122.9(9) . . ? N33 C43 C42 114.5(8) . . ? C43 C44 C45 119.1(11) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C46 C45 C44 118.1(12) . . ? C46 C45 H45 120.9 . . ? C44 C45 H45 120.9 . . ? C45 C46 C47 121.2(12) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? N33 C47 C46 121.7(11) . . ? N33 C47 H47 119.1 . . ? C46 C47 H47 119.1 . . ? C47 N33 C43 117.3(9) . . ? O32 C48 C49 105.4(9) . . ? O32 C48 H48A 110.7 . . ? C49 C48 H48A 110.7 . . ? O32 C48 H48B 110.7 . . ? C49 C48 H48B 110.7 . . ? H48A C48 H48B 108.8 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O34 C50 C51 110.9(11) . . ? O34 C50 H50A 109.5 . . ? C51 C50 H50A 109.5 . . ? O34 C50 H50B 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C62 C61 N61 123.0(10) . . ? C62 C61 H61 118.5 . . ? N61 C61 H61 118.5 . . ? C61 C62 C63 118.5(11) . . ? C61 C62 H62 120.7 . . ? C63 C62 H62 120.7 . . ? C64 C63 C62 119.4(11) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C63 C64 C65 118.6(11) . . ? C63 C64 H64 120.7 . . ? C65 C64 H64 120.7 . . ? N61 C65 C64 121.4(10) . . ? N61 C65 C66 117.3(9) . . ? C64 C65 C66 121.3(9) . . ? O61 C66 O62 111.7(8) . . ? O61 C66 C65 111.4(8) . . ? O62 C66 C65 109.3(7) . . ? O61 C66 C67 111.2(7) . . ? O62 C66 C67 101.1(7) . . ? C65 C66 C67 111.8(8) . . ? C78 O62 C66 116.4(8) . . ? N62 C67 C68 122.0(9) . . ? N62 C67 C66 115.2(8) . . ? C68 C67 C66 122.8(9) . . ? C67 C68 C69 120.2(10) . . ? C67 C68 H68 119.9 . . ? C69 C68 H68 119.9 . . ? C70 C69 C68 118.3(9) . . ? C70 C69 H69 120.8 . . ? C68 C69 H69 120.8 . . ? C69 C70 C71 117.9(8) . . ? C69 C70 H70 121.0 . . ? C71 C70 H70 121.0 . . ? N62 C71 C70 124.4(8) . . ? N62 C71 C72 115.4(7) . . ? C70 C71 C72 120.1(7) . . ? O63 C72 O64 112.1(7) . . ? O63 C72 C71 107.9(6) . . ? O64 C72 C71 111.9(8) . . ? O63 C72 C73 111.5(7) . . ? O64 C72 C73 105.0(7) . . ? C71 C72 C73 108.4(7) . . ? C72 O64 C80 114.1(7) . . ? N63 C73 C74 123.7(9) . . ? N63 C73 C72 114.6(7) . . ? C74 C73 C72 121.7(8) . . ? C73 C74 C75 116.1(9) . . ? C73 C74 H74 122.0 . . ? C75 C74 H74 122.0 . . ? C76 C75 C74 120.6(9) . . ? C76 C75 H75 119.7 . . ? C74 C75 H75 119.7 . . ? C75 C76 C77 119.4(10) . . ? C75 C76 H76 120.3 . . ? C77 C76 H76 120.3 . . ? N63 C77 C76 122.5(10) . . ? N63 C77 H77 118.7 . . ? C76 C77 H77 118.7 . . ? C77 N63 C73 117.7(8) . . ? O62 C78 C79 114.5(12) . . ? O62 C78 H78A 108.6 . . ? C79 C78 H78A 108.6 . . ? O62 C78 H78B 108.6 . . ? C79 C78 H78B 108.6 . . ? H78A C78 H78B 107.6 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O64 C80 C81 107.7(10) . . ? O64 C80 H80A 110.2 . . ? C81 C80 H80A 110.2 . . ? O64 C80 H80B 110.2 . . ? C81 C80 H80B 110.2 . . ? H80A C80 H80B 108.5 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? O92A Cl1 O94 164.6(10) . . ? O92A Cl1 O91 79.3(11) . . ? O94 Cl1 O91 108.0(10) . . ? O92A Cl1 O92 51.9(9) . . ? O94 Cl1 O92 113.2(10) . . ? O91 Cl1 O92 115.7(10) . . ? O92A Cl1 O93 104.9(13) . . ? O94 Cl1 O93 82.2(11) . . ? O91 Cl1 O93 125.8(13) . . ? O92 Cl1 O93 107.1(12) . . ? O92A Cl1 O91A 110.4(17) . . ? O94 Cl1 O91A 73.6(16) . . ? O91 Cl1 O91A 35.7(15) . . ? O92 Cl1 O91A 123.8(16) . . ? O93 Cl1 O91A 128.8(17) . . ? O92A Cl1 O94A 101.7(12) . . ? O94 Cl1 O94A 62.9(11) . . ? O91 Cl1 O94A 118.7(13) . . ? O92 Cl1 O94A 52.6(11) . . ? O93 Cl1 O94A 113.3(14) . . ? O91A Cl1 O94A 94.8(18) . . ? O92A Cl1 O93A 82.3(12) . . ? O94 Cl1 O93A 108.5(11) . . ? O91 Cl1 O93A 102.9(12) . . ? O92 Cl1 O93A 107.9(12) . . ? O93 Cl1 O93A 29.8(11) . . ? O91A Cl1 O93A 123.1(17) . . ? O94A Cl1 O93A 138.3(13) . . ? O96 Cl2 O97 110.6(7) . . ? O96 Cl2 O98 112.2(6) . . ? O97 Cl2 O98 111.1(6) . . ? O96 Cl2 O95 108.2(7) . . ? O97 Cl2 O95 108.2(6) . . ? O98 Cl2 O95 106.4(6) . . ? C91 O99 H99 109.5 . . ? O99 C91 C92 111.5(12) . . ? O99 C91 H91A 109.3 . . ? C92 C91 H91A 109.3 . . ? O99 C91 H91B 109.3 . . ? C92 C91 H91B 109.3 . . ? H91A C91 H91B 108.0 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.825 _refine_diff_density_min -1.501 _refine_diff_density_rms 0.092 # start Validation Reply Form _vrf_PLAT220_Complex3 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.85 Ratio RESPONSE: This is due to the large thermal motion of the methyl carbon atoms of the ligand. Attempts to refine these atoms over two disordered positions converged at occupation factors 0.87 and 0.13 with isotropic model. The anisotropic model for the two positions led to analogous alerts for the site with the largest occupancy. It was thus decided to refine the structure without disorder. ; # end Validation Reply Form #===END # end Validation Reply Form #==END data_Complex2 _database_code_depnum_ccdc_archive 'CCDC 756139' #TrackingRef 'Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H72 Cl2 Gd Mn N9 O21' _chemical_formula_weight 1598.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.338(2) _cell_length_b 20.491(2) _cell_length_c 23.225(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.096(7) _cell_angle_gamma 90.00 _cell_volume 7013.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 42640 _cell_measurement_theta_min 6.85 _cell_measurement_theta_max 71.99 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 8.892 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.520 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41812 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 7.15 _diffrn_reflns_theta_max 64.49 _reflns_number_total 10288 _reflns_number_gt 9522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.101(3) _refine_ls_number_reflns 10288 _refine_ls_number_parameters 894 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.008 _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 Gd Gd 0.26724(2) 0.952995(13) 0.845904(19) 0.03489(10) Uani 1 1 d . . . O3 O 0.1271(3) 0.89739(18) 0.7899(2) 0.0433(10) Uani 1 1 d . . . H3O H 0.0801 0.9032 0.8010 0.056 Uiso 1 1 calc R . . O33 O 0.1383(2) 1.01069(18) 0.86324(19) 0.0380(9) Uani 1 1 d . . . H33O H 0.1094 1.0311 0.8325 0.049 Uiso 1 1 calc R . . O63 O 0.1993(3) 1.01249(17) 0.75473(19) 0.0398(10) Uani 1 1 d . . . H63O H 0.1647 0.9924 0.7257 0.052 Uiso 1 1 calc R . . N2 N 0.2719(3) 0.8767(2) 0.7579(2) 0.0363(11) Uani 1 1 d . . . N32 N 0.1948(3) 0.9089(2) 0.9276(2) 0.0354(11) Uani 1 1 d . . . N62 N 0.3123(3) 1.0731(2) 0.8374(2) 0.0325(11) Uani 1 1 d . . . Mn Mn 0.46356(6) 0.91231(4) 0.91786(4) 0.0364(2) Uani 1 1 d . . . O1 O 0.4077(3) 0.94080(17) 0.82613(19) 0.0342(9) Uani 1 1 d . . . O31 O 0.3351(3) 0.86111(17) 0.89996(19) 0.0369(10) Uani 1 1 d . . . O61 O 0.3791(2) 0.99481(17) 0.92864(18) 0.0352(9) Uani 1 1 d . . . N1 N 0.5339(3) 0.8485(2) 0.8676(3) 0.0387(12) Uani 1 1 d . . . N31 N 0.4696(3) 0.8625(2) 1.0012(3) 0.0423(13) Uani 1 1 d . . . N61 N 0.5576(3) 0.9944(2) 0.9380(2) 0.0432(13) Uani 1 1 d . . . O2 O 0.4557(3) 0.94941(17) 0.7395(2) 0.0402(11) Uani 1 1 d . . . O4 O 0.0634(3) 0.7994(2) 0.7456(2) 0.0546(12) Uani 1 1 d . . . N3 N 0.0745(4) 0.9526(2) 0.6727(3) 0.0527(16) Uani 1 1 d . . . C1 C 0.6046(4) 0.8091(3) 0.8931(3) 0.0520(18) Uani 1 1 d . . . H1 H 0.6166 0.7988 0.9345 0.068 Uiso 1 1 calc R . . C2 C 0.6599(4) 0.7831(3) 0.8611(4) 0.0547(18) Uani 1 1 d . . . H2 H 0.7085 0.7547 0.8797 0.071 Uiso 1 1 calc R . . C3 C 0.6422(4) 0.7998(3) 0.8003(4) 0.0575(19) Uani 1 1 d . . . H3 H 0.6798 0.7836 0.7772 0.075 Uiso 1 1 calc R . . C4 C 0.5701(4) 0.8400(3) 0.7746(3) 0.0462(16) Uani 1 1 d . . . H4 H 0.5573 0.8520 0.7335 0.060 Uiso 1 1 calc R . . C5 C 0.5159(4) 0.8629(3) 0.8097(3) 0.0375(14) Uani 1 1 d . . . C6 C 0.4322(4) 0.9075(3) 0.7826(3) 0.0346(14) Uani 1 1 d . . . C7 C 0.3511(4) 0.8675(2) 0.7443(3) 0.0348(14) Uani 1 1 d . . . C8 C 0.3576(4) 0.8269(3) 0.6985(3) 0.0370(14) Uani 1 1 d . . . H8 H 0.4142 0.8212 0.6899 0.048 Uiso 1 1 calc R . . C9 C 0.2808(4) 0.7942(3) 0.6648(3) 0.0447(16) Uani 1 1 d . . . H9 H 0.2840 0.7664 0.6327 0.058 Uiso 1 1 calc R . . C10 C 0.2015(4) 0.8027(3) 0.6788(3) 0.0470(17) Uani 1 1 d . . . H10 H 0.1482 0.7806 0.6569 0.061 Uiso 1 1 calc R . . C11 C 0.1993(4) 0.8443(3) 0.7256(3) 0.0379(15) Uani 1 1 d . . . C12 C 0.1066(4) 0.8581(3) 0.7385(3) 0.0425(15) Uani 1 1 d . . . C13 C 0.0447(4) 0.8925(3) 0.6841(3) 0.0447(16) Uani 1 1 d . . . C14 C -0.0330(5) 0.8661(4) 0.6485(4) 0.065(2) Uani 1 1 d . . . H14 H -0.0532 0.8245 0.6574 0.084 Uiso 1 1 calc R . . C15 C -0.0831(5) 0.9019(5) 0.5980(4) 0.080(3) Uani 1 1 d . . . H15 H -0.1375 0.8845 0.5724 0.104 Uiso 1 1 calc R . . C16 C -0.0517(6) 0.9625(4) 0.5864(4) 0.071(2) Uani 1 1 d . . . H16 H -0.0832 0.9869 0.5522 0.093 Uiso 1 1 calc R . . C17 C 0.0240(5) 0.9858(4) 0.6246(4) 0.062(2) Uani 1 1 d . . . H17 H 0.0436 1.0283 0.6174 0.081 Uiso 1 1 calc R . . C18 C 0.5220(5) 0.9980(3) 0.7684(3) 0.0541(18) Uani 1 1 d D . . H18A H 0.5700 0.9781 0.8013 0.070 Uiso 1 1 calc R . . H18B H 0.4927 1.0335 0.7852 0.070 Uiso 1 1 calc R . . C19 C 0.5621(6) 1.0244(4) 0.7192(4) 0.076(2) Uani 1 1 d D . . H19A H 0.6027 1.0610 0.7351 0.099 Uiso 1 1 calc R . . H19B H 0.5128 1.0393 0.6851 0.099 Uiso 1 1 calc R . . H19C H 0.5962 0.9897 0.7061 0.099 Uiso 1 1 calc R . . C20 C 0.1093(6) 0.7630(4) 0.7990(5) 0.083(3) Uani 1 1 d D . . H20A H 0.0976 0.7837 0.8347 0.108 Uiso 1 1 calc R . . H20B H 0.1756 0.7635 0.8042 0.108 Uiso 1 1 calc R . . C21 C 0.0762(8) 0.6953(5) 0.7936(5) 0.107(4) Uani 1 1 d D . . H21A H 0.0879 0.6770 0.8344 0.139 Uiso 1 1 d . . . H21B H 0.1095 0.6705 0.7710 0.139 Uiso 1 1 d . . . H21C H 0.0115 0.6954 0.7740 0.139 Uiso 1 1 d . . . O32 O 0.2982(3) 0.75979(18) 0.9313(2) 0.0474(12) Uani 1 1 d . . . O34 O 0.0702(3) 1.04869(18) 0.9343(2) 0.0475(12) Uani 1 1 d . . . N33 N -0.0211(4) 0.9394(3) 0.8135(3) 0.0486(14) Uani 1 1 d . . . C31 C 0.5423(5) 0.8652(3) 1.0517(4) 0.0510(18) Uani 1 1 d . . . H31 H 0.5961 0.8863 1.0489 0.066 Uiso 1 1 calc R . . C32 C 0.5412(5) 0.8394(3) 1.1047(4) 0.062(2) Uani 1 1 d . . . H32 H 0.5927 0.8425 1.1386 0.081 Uiso 1 1 calc R . . C33 C 0.4625(5) 0.8080(4) 1.1087(4) 0.067(2) Uani 1 1 d . . . H33 H 0.4590 0.7902 1.1457 0.087 Uiso 1 1 calc R . . C34 C 0.3893(5) 0.8032(4) 1.0580(4) 0.064(2) Uani 1 1 d . . . H34 H 0.3362 0.7803 1.0597 0.083 Uiso 1 1 calc R . . C35 C 0.3939(4) 0.8319(3) 1.0048(3) 0.0440(16) Uani 1 1 d . . . C36 C 0.3152(4) 0.8282(3) 0.9449(3) 0.0411(15) Uani 1 1 d . . . C37 C 0.2254(4) 0.8525(3) 0.9545(3) 0.0371(14) Uani 1 1 d . . . C38 C 0.1776(4) 0.8194(3) 0.9888(3) 0.0463(18) Uani 1 1 d . . . H38 H 0.1991 0.7786 1.0067 0.060 Uiso 1 1 calc R . . C39 C 0.0993(4) 0.8461(3) 0.9964(3) 0.0520(18) Uani 1 1 d . . . H39 H 0.0659 0.8237 1.0192 0.068 Uiso 1 1 calc R . . C40 C 0.0700(4) 0.9053(3) 0.9710(3) 0.0477(16) Uani 1 1 d . . . H40 H 0.0185 0.9260 0.9779 0.062 Uiso 1 1 calc R . . C41 C 0.1175(4) 0.9344(3) 0.9345(3) 0.0401(15) Uani 1 1 d . . . C42 C 0.0805(4) 0.9955(3) 0.8980(3) 0.0423(15) Uani 1 1 d . . . C43 C -0.0170(4) 0.9792(3) 0.8593(3) 0.0408(15) Uani 1 1 d . . . C44 C -0.0948(4) 0.9996(3) 0.8737(3) 0.0517(18) Uani 1 1 d . . . H44 H -0.0901 1.0275 0.9071 0.067 Uiso 1 1 calc R . . C45 C -0.1783(5) 0.9793(4) 0.8396(4) 0.064(2) Uani 1 1 d . . . H45 H -0.2318 0.9932 0.8491 0.084 Uiso 1 1 calc R . . C46 C -0.1836(5) 0.9395(4) 0.7927(4) 0.059(2) Uani 1 1 d . . . H46 H -0.2408 0.9253 0.7681 0.076 Uiso 1 1 calc R . . C47 C -0.1029(4) 0.9195(4) 0.7809(4) 0.060(2) Uani 1 1 d . . . H47 H -0.1064 0.8905 0.7484 0.077 Uiso 1 1 calc R . . C48 C 0.3721(5) 0.7287(3) 0.9149(4) 0.071(3) Uani 1 1 d D . . H48A H 0.3846 0.7522 0.8808 0.092 Uiso 1 1 calc R . . H48B H 0.4276 0.7302 0.9491 0.092 Uiso 1 1 calc R . . C49 C 0.3493(10) 0.6625(5) 0.8985(9) 0.208(10) Uani 1 1 d D . . H49A H 0.3509 0.6370 0.9345 0.271 Uiso 1 1 calc R . . H49B H 0.3932 0.6445 0.8791 0.271 Uiso 1 1 calc R . . H49C H 0.2883 0.6606 0.8707 0.271 Uiso 1 1 calc R . . C50 C 0.1537(5) 1.0720(4) 0.9745(4) 0.063(2) Uani 1 1 d D . . H50A H 0.1986 1.0808 0.9520 0.082 Uiso 1 1 calc R . . H50B H 0.1792 1.0385 1.0053 0.082 Uiso 1 1 calc R . . C51 C 0.1355(8) 1.1318(6) 1.0033(6) 0.143(6) Uani 1 1 d D . . H51A H 0.1353 1.1225 1.0445 0.187 Uiso 1 1 d . . . H51B H 0.0786 1.1502 0.9807 0.187 Uiso 1 1 d . . . H51C H 0.1855 1.1631 1.0042 0.187 Uiso 1 1 d . . . O62 O 0.4016(3) 1.08910(19) 0.9865(2) 0.0459(11) Uani 1 1 d . . . O64 O 0.2139(3) 1.0876(2) 0.6836(2) 0.0501(12) Uani 1 1 d . . . N63 N 0.0772(4) 1.1006(2) 0.7846(3) 0.0509(15) Uani 1 1 d . . . C61 C 0.6485(4) 0.9912(3) 0.9450(3) 0.0465(16) Uani 1 1 d . . . H61 H 0.6741 0.9501 0.9397 0.060 Uiso 1 1 calc R . . C62 C 0.7048(5) 1.0436(3) 0.9594(4) 0.057(2) Uani 1 1 d . . . H62 H 0.7675 1.0391 0.9622 0.074 Uiso 1 1 calc R . . C63 C 0.6711(5) 1.1025(4) 0.9696(4) 0.067(2) Uani 1 1 d . . . H63 H 0.7092 1.1397 0.9800 0.087 Uiso 1 1 calc R . . C64 C 0.5779(4) 1.1062(3) 0.9640(3) 0.0523(19) Uani 1 1 d . . . H64 H 0.5522 1.1465 0.9715 0.068 Uiso 1 1 calc R . . C65 C 0.5235(4) 1.0525(3) 0.9480(3) 0.0389(15) Uani 1 1 d . . . C66 C 0.4169(4) 1.0554(3) 0.9371(3) 0.0386(15) Uani 1 1 d . . . C67 C 0.3742(4) 1.1017(3) 0.8843(3) 0.0403(15) Uani 1 1 d . . . C68 C 0.3931(4) 1.1676(3) 0.8867(4) 0.0529(19) Uani 1 1 d . . . H68 H 0.4301 1.1874 0.9220 0.069 Uiso 1 1 calc R . . C69 C 0.3553(5) 1.2040(3) 0.8349(4) 0.063(2) Uani 1 1 d . . . H69 H 0.3695 1.2490 0.8341 0.082 Uiso 1 1 calc R . . C70 C 0.2984(4) 1.1756(3) 0.7855(3) 0.0420(15) Uani 1 1 d . . . H70 H 0.2756 1.1995 0.7494 0.055 Uiso 1 1 calc R . . C71 C 0.2747(4) 1.1106(3) 0.7897(3) 0.0380(14) Uani 1 1 d . . . C72 C 0.2006(4) 1.0788(3) 0.7406(3) 0.0390(15) Uani 1 1 d . . . C73 C 0.1101(4) 1.1116(3) 0.7379(3) 0.0404(15) Uani 1 1 d . . . C74 C 0.0654(4) 1.1523(3) 0.6902(3) 0.0458(16) Uani 1 1 d . . . H74 H 0.0888 1.1592 0.6568 0.060 Uiso 1 1 calc R . . C75 C -0.0149(5) 1.1820(3) 0.6938(4) 0.059(2) Uani 1 1 d . . . H75 H -0.0462 1.2105 0.6626 0.076 Uiso 1 1 calc R . . C76 C -0.0485(5) 1.1713(3) 0.7402(4) 0.060(2) Uani 1 1 d . . . H76 H -0.1035 1.1914 0.7420 0.078 Uiso 1 1 calc R . . C77 C -0.0010(4) 1.1301(3) 0.7860(4) 0.0561(19) Uani 1 1 d . . . H77 H -0.0243 1.1226 0.8193 0.073 Uiso 1 1 calc R . . C78 C 0.4344(7) 1.0546(4) 1.0423(4) 0.067(2) Uani 1 1 d D . . H78A H 0.4992 1.0432 1.0492 0.094 Uiso 1 1 calc R . . H78B H 0.3995 1.0137 1.0414 0.094 Uiso 1 1 calc R . . C79 C 0.4226(8) 1.0982(5) 1.0909(4) 0.099(3) Uani 1 1 d D . . H79A H 0.4432 1.0756 1.1295 0.148 Uiso 1 1 calc R . . H79B H 0.3584 1.1098 1.0832 0.148 Uiso 1 1 calc R . . H79C H 0.4586 1.1380 1.0920 0.148 Uiso 1 1 calc R . . C80 C 0.3014(6) 1.0664(4) 0.6781(4) 0.066(2) Uani 1 1 d D . . H80A H 0.3478 1.1003 0.6938 0.086 Uiso 1 1 calc R . . H80B H 0.3204 1.0258 0.7013 0.086 Uiso 1 1 calc R . . C81 C 0.2924(8) 1.0548(6) 0.6153(5) 0.111(4) Uani 1 1 d D . . H81A H 0.3522 1.0577 0.6080 0.145 Uiso 1 1 calc R . . H81B H 0.2520 1.0877 0.5912 0.145 Uiso 1 1 calc R . . H81C H 0.2669 1.0113 0.6043 0.145 Uiso 1 1 calc R . . Cl1 Cl 0.34578(12) 0.64658(10) 0.50777(10) 0.0712(6) Uani 1 1 d D . . O91 O 0.3370(6) 0.5842(4) 0.4757(5) 0.083(3) Uiso 0.65 1 d PD A 1 O92 O 0.3658(7) 0.6933(5) 0.4677(5) 0.093(3) Uiso 0.65 1 d PD A 1 O93 O 0.2664(7) 0.6655(6) 0.5248(6) 0.093(4) Uiso 0.65 1 d PD A 1 O94 O 0.4217(6) 0.6368(5) 0.5582(4) 0.078(3) Uiso 0.65 1 d PD A 1 O91A O 0.3235(17) 0.6190(12) 0.4482(8) 0.144(9) Uiso 0.35 1 d PD A 2 O92A O 0.3767(15) 0.7126(8) 0.5098(13) 0.136(9) Uiso 0.35 1 d PD A 2 O93A O 0.2599(10) 0.6421(9) 0.5228(9) 0.066(5) Uiso 0.35 1 d PD A 2 O94A O 0.4045(14) 0.6029(10) 0.5496(9) 0.118(8) Uiso 0.35 1 d PD A 2 Cl2 Cl 0.71257(15) 0.80058(9) 0.63933(10) 0.0672(5) Uani 1 1 d D . . O95 O 0.6415(13) 0.7568(10) 0.6291(10) 0.181(8) Uiso 0.53 1 d PD B 3 O96 O 0.7098(12) 0.8197(8) 0.5797(6) 0.120(7) Uiso 0.53 1 d PD B 3 O97 O 0.7989(10) 0.7765(9) 0.6770(8) 0.143(6) Uiso 0.53 1 d PD B 3 O98 O 0.6958(13) 0.8595(7) 0.6644(8) 0.153(6) Uiso 0.53 1 d PD B 3 O95A O 0.6217(10) 0.7937(10) 0.6448(9) 0.136(6) Uiso 0.47 1 d PD B 4 O96A O 0.7448(12) 0.8204(7) 0.5916(7) 0.084(5) Uiso 0.47 1 d PD B 4 O97A O 0.7402(12) 0.7315(6) 0.6414(8) 0.126(6) Uiso 0.47 1 d PD B 4 O98A O 0.7629(13) 0.8273(10) 0.6953(7) 0.146(7) Uiso 0.47 1 d PD B 4 O99 O 0.2583(4) 0.6273(3) 0.6454(3) 0.0828(18) Uani 1 1 d . . . H99O H 0.2259 0.6274 0.6097 0.108 Uiso 1 1 calc R . . C91 C 0.2846(7) 0.5633(5) 0.6630(6) 0.096(3) Uani 1 1 d . . . H91A H 0.2791 0.5566 0.7040 0.124 Uiso 1 1 calc R . . H91B H 0.3494 0.5581 0.6647 0.124 Uiso 1 1 calc R . . C92 C 0.2326(7) 0.5120(5) 0.6241(5) 0.099(3) Uani 1 1 d . . . H92A H 0.2641 0.4702 0.6340 0.128 Uiso 1 1 calc R . . H92B H 0.2269 0.5229 0.5821 0.128 Uiso 1 1 calc R . . H92C H 0.1720 0.5089 0.6302 0.128 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 Gd 0.02959(16) 0.03474(16) 0.0390(2) 0.00013(17) 0.00738(14) 0.00647(15) O3 0.029(2) 0.046(2) 0.051(3) -0.012(2) 0.005(2) -0.0029(18) O33 0.030(2) 0.047(2) 0.035(3) 0.001(2) 0.0053(19) 0.0151(17) O63 0.039(2) 0.031(2) 0.044(3) -0.0042(19) 0.002(2) 0.0069(17) N2 0.031(3) 0.034(2) 0.040(3) 0.001(2) 0.003(2) 0.007(2) N32 0.027(2) 0.037(3) 0.039(3) 0.001(2) 0.004(2) 0.007(2) N62 0.029(2) 0.036(2) 0.031(3) -0.001(2) 0.004(2) 0.002(2) Mn 0.0297(5) 0.0395(5) 0.0387(6) 0.0029(4) 0.0072(5) 0.0059(4) O1 0.029(2) 0.0350(19) 0.038(3) -0.0006(18) 0.007(2) 0.0059(16) O31 0.032(2) 0.036(2) 0.045(3) 0.0014(19) 0.014(2) 0.0063(16) O61 0.034(2) 0.032(2) 0.039(3) 0.0004(18) 0.008(2) 0.0007(16) N1 0.029(2) 0.039(3) 0.045(3) 0.002(2) 0.006(2) 0.006(2) N31 0.039(3) 0.040(3) 0.047(4) 0.007(3) 0.011(3) 0.005(2) N61 0.044(3) 0.040(3) 0.047(4) 0.001(2) 0.016(3) 0.003(2) O2 0.040(2) 0.040(2) 0.042(3) 0.0062(19) 0.015(2) 0.0042(17) O4 0.039(2) 0.054(3) 0.068(4) -0.002(3) 0.010(2) -0.007(2) N3 0.053(4) 0.047(3) 0.050(4) -0.004(3) 0.000(3) 0.007(2) C1 0.046(4) 0.053(4) 0.054(5) 0.009(3) 0.009(4) 0.015(3) C2 0.041(4) 0.057(4) 0.060(5) 0.004(4) 0.004(4) 0.023(3) C3 0.042(4) 0.067(4) 0.064(6) -0.007(4) 0.015(4) 0.017(3) C4 0.037(3) 0.054(4) 0.047(4) -0.003(3) 0.012(3) 0.010(3) C5 0.031(3) 0.034(3) 0.045(4) -0.001(3) 0.006(3) 0.004(2) C6 0.031(3) 0.036(3) 0.039(4) 0.000(3) 0.013(3) 0.012(2) C7 0.030(3) 0.028(3) 0.045(4) 0.001(3) 0.009(3) 0.010(2) C8 0.040(3) 0.041(3) 0.025(4) -0.003(3) 0.003(3) 0.008(3) C9 0.057(4) 0.039(3) 0.036(4) -0.010(3) 0.009(3) 0.013(3) C10 0.041(4) 0.038(3) 0.053(5) -0.011(3) -0.002(3) 0.006(3) C11 0.031(3) 0.034(3) 0.044(4) -0.004(3) 0.004(3) 0.010(2) C12 0.032(3) 0.045(3) 0.046(4) -0.008(3) 0.004(3) -0.002(3) C13 0.036(3) 0.054(4) 0.041(4) -0.012(3) 0.005(3) 0.007(3) C14 0.043(4) 0.077(5) 0.064(6) -0.019(4) -0.001(4) -0.002(4) C15 0.042(4) 0.108(7) 0.071(7) -0.017(6) -0.018(4) 0.003(5) C16 0.060(5) 0.083(6) 0.053(6) 0.007(4) -0.014(5) 0.016(4) C17 0.063(5) 0.057(4) 0.053(5) 0.002(4) -0.007(4) 0.013(4) C18 0.049(4) 0.052(4) 0.063(5) 0.001(4) 0.018(4) -0.004(3) C19 0.067(5) 0.087(5) 0.075(7) 0.021(5) 0.020(5) -0.019(5) C20 0.085(6) 0.054(5) 0.100(8) 0.010(5) 0.010(6) -0.014(4) C21 0.123(9) 0.096(7) 0.096(9) 0.011(6) 0.018(7) -0.038(6) O32 0.047(2) 0.031(2) 0.071(4) 0.002(2) 0.028(2) 0.0039(18) O34 0.039(3) 0.050(3) 0.054(3) -0.012(2) 0.013(2) 0.0138(18) N33 0.033(3) 0.058(3) 0.055(4) -0.003(3) 0.011(3) 0.005(2) C31 0.044(4) 0.053(4) 0.052(5) 0.005(4) 0.007(4) -0.001(3) C32 0.054(4) 0.063(4) 0.060(6) 0.022(4) 0.002(4) 0.013(4) C33 0.052(5) 0.086(6) 0.056(6) 0.029(5) 0.002(4) 0.001(4) C34 0.057(5) 0.071(5) 0.065(6) 0.030(4) 0.021(4) 0.003(4) C35 0.042(4) 0.034(3) 0.056(5) 0.005(3) 0.012(4) 0.012(3) C36 0.037(3) 0.036(3) 0.053(5) 0.004(3) 0.018(3) 0.009(3) C37 0.031(3) 0.041(3) 0.037(4) -0.004(3) 0.007(3) 0.002(2) C38 0.038(3) 0.044(4) 0.061(5) 0.004(3) 0.019(4) -0.001(3) C39 0.049(4) 0.069(4) 0.046(4) 0.016(4) 0.026(4) 0.011(3) C40 0.042(4) 0.058(4) 0.049(5) 0.007(3) 0.021(3) 0.007(3) C41 0.036(3) 0.041(3) 0.040(4) -0.004(3) 0.005(3) 0.005(3) C42 0.031(3) 0.048(3) 0.046(4) 0.000(3) 0.007(3) 0.009(3) C43 0.036(3) 0.042(3) 0.042(4) 0.003(3) 0.007(3) 0.010(3) C44 0.036(4) 0.069(4) 0.052(5) 0.000(4) 0.015(3) 0.013(3) C45 0.031(4) 0.102(6) 0.062(6) 0.011(5) 0.016(4) 0.017(4) C46 0.031(4) 0.090(5) 0.052(5) -0.002(4) 0.006(4) 0.003(3) C47 0.036(4) 0.077(5) 0.062(6) -0.007(4) 0.007(4) -0.003(3) C48 0.067(5) 0.043(4) 0.114(8) -0.006(4) 0.046(5) 0.014(3) C49 0.211(15) 0.081(7) 0.42(3) -0.066(12) 0.239(19) -0.019(9) C50 0.050(4) 0.071(5) 0.057(6) -0.022(4) -0.003(4) 0.016(4) C51 0.107(9) 0.126(9) 0.160(13) -0.082(9) -0.023(8) 0.026(7) O62 0.053(3) 0.048(2) 0.039(3) -0.010(2) 0.016(2) 0.010(2) O64 0.052(3) 0.057(3) 0.042(3) 0.012(2) 0.014(2) 0.022(2) N63 0.040(3) 0.043(3) 0.070(5) 0.010(3) 0.017(3) 0.013(2) C61 0.027(3) 0.059(4) 0.051(5) 0.000(3) 0.008(3) -0.004(3) C62 0.035(4) 0.064(5) 0.069(6) -0.004(4) 0.008(4) -0.002(3) C63 0.045(4) 0.074(5) 0.076(6) -0.019(4) 0.005(4) -0.011(4) C64 0.033(3) 0.051(4) 0.062(5) -0.016(3) -0.006(3) 0.001(3) C65 0.031(3) 0.044(3) 0.039(4) 0.005(3) 0.005(3) 0.002(2) C66 0.037(3) 0.038(3) 0.040(4) -0.001(3) 0.008(3) 0.003(2) C67 0.034(3) 0.040(3) 0.051(4) 0.002(3) 0.018(3) 0.005(2) C68 0.032(3) 0.044(4) 0.072(6) 0.001(4) -0.004(4) -0.007(3) C69 0.043(4) 0.036(3) 0.110(7) 0.019(4) 0.021(5) 0.000(3) C70 0.037(3) 0.039(3) 0.048(4) 0.008(3) 0.009(3) 0.004(3) C71 0.034(3) 0.037(3) 0.043(4) 0.000(3) 0.011(3) 0.013(2) C72 0.040(3) 0.037(3) 0.038(4) 0.005(3) 0.008(3) 0.010(3) C73 0.036(3) 0.039(3) 0.043(4) -0.001(3) 0.004(3) 0.010(3) C74 0.045(4) 0.041(3) 0.048(4) 0.005(3) 0.009(3) 0.009(3) C75 0.048(4) 0.040(3) 0.078(6) 0.012(4) 0.002(4) 0.018(3) C76 0.040(4) 0.051(4) 0.087(6) 0.014(4) 0.015(4) 0.020(3) C77 0.043(4) 0.050(4) 0.077(6) 0.007(4) 0.019(4) 0.016(3) C78 0.097(7) 0.066(5) 0.045(5) 0.006(4) 0.029(5) 0.017(4) C79 0.142(10) 0.100(7) 0.058(6) -0.020(6) 0.034(7) 0.012(6) C80 0.071(5) 0.080(5) 0.053(6) 0.007(4) 0.027(5) 0.031(4) C81 0.105(9) 0.169(11) 0.068(8) -0.021(7) 0.038(7) 0.036(7) Cl1 0.0437(10) 0.0837(13) 0.0785(16) 0.0143(11) 0.0039(10) -0.0091(9) Cl2 0.0841(14) 0.0625(11) 0.0625(14) 0.0060(10) 0.0329(12) -0.0092(10) O99 0.056(4) 0.080(4) 0.101(6) -0.009(4) 0.004(3) 0.007(3) C91 0.075(7) 0.095(7) 0.113(10) -0.005(7) 0.019(7) 0.001(6) C92 0.106(8) 0.086(7) 0.109(9) 0.000(6) 0.037(7) 0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O1 2.337(4) . ? Gd O31 2.341(4) . ? Gd O61 2.354(4) . ? Gd O63 2.415(4) . ? Gd O33 2.431(3) . ? Gd O3 2.461(4) . ? Gd N62 2.578(5) . ? Gd N2 2.590(5) . ? Gd N32 2.611(5) . ? Gd Mn 3.1248(10) . ? O3 C12 1.401(7) . ? O3 H3O 0.8400 . ? O33 C42 1.391(7) . ? O33 H33O 0.8400 . ? O63 C72 1.398(7) . ? O63 H63O 0.8400 . ? N2 C11 1.334(7) . ? N2 C7 1.351(7) . ? N32 C37 1.335(7) . ? N32 C41 1.345(7) . ? N62 C71 1.339(7) . ? N62 C67 1.364(8) . ? Mn O1 2.145(4) . ? Mn N31 2.167(5) . ? Mn O31 2.168(4) . ? Mn N61 2.180(5) . ? Mn O61 2.186(4) . ? Mn N1 2.222(5) . ? O1 C6 1.356(7) . ? O31 C36 1.347(7) . ? O61 C66 1.361(7) . ? N1 C5 1.328(8) . ? N1 C1 1.350(7) . ? N31 C35 1.343(8) . ? N31 C31 1.377(9) . ? N61 C65 1.348(7) . ? N61 C61 1.360(7) . ? O2 C6 1.438(7) . ? O2 C18 1.448(8) . ? O4 C12 1.405(7) . ? O4 C20 1.452(10) . ? N3 C17 1.353(9) . ? N3 C13 1.365(8) . ? C1 C2 1.380(9) . ? C1 H1 0.9500 . ? C2 C3 1.405(10) . ? C2 H2 0.9500 . ? C3 C4 1.376(9) . ? C3 H3 0.9500 . ? C4 C5 1.397(8) . ? C4 H4 0.9500 . ? C5 C6 1.560(7) . ? C6 C7 1.549(8) . ? C7 C8 1.375(8) . ? C8 C9 1.392(9) . ? C8 H8 0.9500 . ? C9 C10 1.354(9) . ? C9 H9 0.9500 . ? C10 C11 1.389(9) . ? C10 H10 0.9500 . ? C11 C12 1.558(8) . ? C12 C13 1.526(9) . ? C13 C14 1.361(9) . ? C14 C15 1.416(12) . ? C14 H14 0.9500 . ? C15 C16 1.386(12) . ? C15 H15 0.9500 . ? C16 C17 1.339(11) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.537(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.470(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9884 . ? C21 H21B 0.9695 . ? C21 H21C 0.9702 . ? O32 C48 1.441(7) . ? O32 C36 1.444(7) . ? O34 C42 1.413(7) . ? O34 C50 1.443(9) . ? N33 C43 1.328(8) . ? N33 C47 1.337(8) . ? C31 C32 1.345(10) . ? C31 H31 0.9500 . ? C32 C33 1.392(10) . ? C32 H32 0.9500 . ? C33 C34 1.386(11) . ? C33 H33 0.9500 . ? C34 C35 1.388(9) . ? C34 H34 0.9500 . ? C35 C36 1.571(10) . ? C36 C37 1.539(8) . ? C37 C38 1.398(9) . ? C38 C39 1.375(8) . ? C38 H38 0.9500 . ? C39 C40 1.370(9) . ? C39 H39 0.9500 . ? C40 C41 1.394(8) . ? C40 H40 0.9500 . ? C41 C42 1.530(8) . ? C42 C43 1.552(9) . ? C43 C44 1.389(8) . ? C44 C45 1.370(10) . ? C44 H44 0.9500 . ? C45 C46 1.346(11) . ? C45 H45 0.9500 . ? C46 C47 1.402(9) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.425(11) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.459(10) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9783 . ? C51 H51B 0.9613 . ? C51 H51C 0.9945 . ? O62 C66 1.412(7) . ? O62 C78 1.439(9) . ? O64 C72 1.405(7) . ? O64 C80 1.451(8) . ? N63 C73 1.337(8) . ? N63 C77 1.351(7) . ? C61 C62 1.361(9) . ? C61 H61 0.9500 . ? C62 C63 1.359(10) . ? C62 H62 0.9500 . ? C63 C64 1.400(9) . ? C63 H63 0.9500 . ? C64 C65 1.369(8) . ? C64 H64 0.9500 . ? C65 C66 1.585(8) . ? C66 C67 1.545(9) . ? C67 C68 1.379(8) . ? C68 C69 1.397(10) . ? C68 H68 0.9500 . ? C69 C70 1.364(10) . ? C69 H69 0.9500 . ? C70 C71 1.392(8) . ? C70 H70 0.9500 . ? C71 C72 1.517(9) . ? C72 C73 1.528(8) . ? C73 C74 1.403(9) . ? C74 C75 1.398(9) . ? C74 H74 0.9500 . ? C75 C76 1.335(11) . ? C75 H75 0.9500 . ? C76 C77 1.395(10) . ? C76 H76 0.9500 . ? C77 H77 0.9500 . ? C78 C79 1.490(10) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.444(10) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? Cl1 O94 1.418(9) . ? Cl1 O92 1.427(9) . ? Cl1 O92A 1.431(15) . ? Cl1 O93 1.434(10) . ? Cl1 O94A 1.438(15) . ? Cl1 O91A 1.445(15) . ? Cl1 O93A 1.455(12) . ? Cl1 O91 1.466(8) . ? Cl2 O95 1.379(14) . ? Cl2 O96A 1.394(11) . ? Cl2 O98 1.394(13) . ? Cl2 O98A 1.424(14) . ? Cl2 O96 1.428(13) . ? Cl2 O95A 1.442(13) . ? Cl2 O97 1.456(13) . ? Cl2 O97A 1.476(13) . ? O99 C91 1.400(11) . ? O99 H99O 0.8400 . ? C91 C92 1.468(14) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd O31 73.88(13) . . ? O1 Gd O61 72.33(14) . . ? O31 Gd O61 74.92(13) . . ? O1 Gd O63 94.52(14) . . ? O31 Gd O63 153.62(13) . . ? O61 Gd O63 124.86(13) . . ? O1 Gd O33 157.04(13) . . ? O31 Gd O33 124.29(13) . . ? O61 Gd O33 97.47(13) . . ? O63 Gd O33 74.15(14) . . ? O1 Gd O3 124.31(14) . . ? O31 Gd O3 95.99(14) . . ? O61 Gd O3 158.73(14) . . ? O63 Gd O3 70.67(14) . . ? O33 Gd O3 71.45(13) . . ? O1 Gd N62 78.79(13) . . ? O31 Gd N62 136.06(15) . . ? O61 Gd N62 64.23(14) . . ? O63 Gd N62 60.68(14) . . ? O33 Gd N62 78.25(13) . . ? O3 Gd N62 127.91(15) . . ? O1 Gd N2 63.39(14) . . ? O31 Gd N2 80.33(15) . . ? O61 Gd N2 133.68(14) . . ? O63 Gd N2 73.29(14) . . ? O33 Gd N2 128.74(14) . . ? O3 Gd N2 60.93(14) . . ? N62 Gd N2 116.68(15) . . ? O1 Gd N32 134.97(14) . . ? O31 Gd N32 63.10(13) . . ? O61 Gd N32 83.87(14) . . ? O63 Gd N32 130.15(14) . . ? O33 Gd N32 61.22(13) . . ? O3 Gd N32 74.89(15) . . ? N62 Gd N32 124.27(14) . . ? N2 Gd N32 118.35(15) . . ? O1 Gd Mn 43.33(11) . . ? O31 Gd Mn 43.89(9) . . ? O61 Gd Mn 44.31(9) . . ? O63 Gd Mn 136.15(9) . . ? O33 Gd Mn 138.46(10) . . ? O3 Gd Mn 136.87(10) . . ? N62 Gd Mn 93.25(11) . . ? N2 Gd Mn 91.59(11) . . ? N32 Gd Mn 93.44(10) . . ? C12 O3 Gd 132.3(3) . . ? C12 O3 H3O 109.5 . . ? Gd O3 H3O 118.1 . . ? C42 O33 Gd 131.8(3) . . ? C42 O33 H33O 109.5 . . ? Gd O33 H33O 111.3 . . ? C72 O63 Gd 131.7(4) . . ? C72 O63 H63O 109.5 . . ? Gd O63 H63O 118.6 . . ? C11 N2 C7 117.6(5) . . ? C11 N2 Gd 122.9(4) . . ? C7 N2 Gd 119.5(4) . . ? C37 N32 C41 119.1(5) . . ? C37 N32 Gd 118.3(3) . . ? C41 N32 Gd 121.3(4) . . ? C71 N62 C67 117.3(5) . . ? C71 N62 Gd 123.3(4) . . ? C67 N62 Gd 119.4(4) . . ? O1 Mn N31 157.15(18) . . ? O1 Mn O31 81.35(15) . . ? N31 Mn O31 75.82(18) . . ? O1 Mn N61 93.50(18) . . ? N31 Mn N61 108.1(2) . . ? O31 Mn N61 157.89(16) . . ? O1 Mn O61 79.46(15) . . ? N31 Mn O61 98.17(17) . . ? O31 Mn O61 81.98(13) . . ? N61 Mn O61 75.94(16) . . ? O1 Mn N1 75.90(17) . . ? N31 Mn N1 106.59(19) . . ? O31 Mn N1 99.35(16) . . ? N61 Mn N1 100.20(18) . . ? O61 Mn N1 154.79(18) . . ? O1 Mn Gd 48.38(10) . . ? N31 Mn Gd 113.56(14) . . ? O31 Mn Gd 48.46(10) . . ? N61 Mn Gd 113.02(14) . . ? O61 Mn Gd 48.79(11) . . ? N1 Mn Gd 114.34(14) . . ? C6 O1 Mn 119.1(3) . . ? C6 O1 Gd 131.4(3) . . ? Mn O1 Gd 88.29(15) . . ? C36 O31 Mn 118.9(4) . . ? C36 O31 Gd 131.0(3) . . ? Mn O31 Gd 87.65(13) . . ? C66 O61 Mn 118.7(3) . . ? C66 O61 Gd 129.4(4) . . ? Mn O61 Gd 86.90(13) . . ? C5 N1 C1 119.6(5) . . ? C5 N1 Mn 114.0(4) . . ? C1 N1 Mn 124.7(5) . . ? C35 N31 C31 118.4(6) . . ? C35 N31 Mn 116.9(5) . . ? C31 N31 Mn 124.5(4) . . ? C65 N61 C61 117.1(5) . . ? C65 N61 Mn 117.0(4) . . ? C61 N61 Mn 125.7(4) . . ? C6 O2 C18 111.6(5) . . ? C12 O4 C20 114.1(5) . . ? C17 N3 C13 118.0(6) . . ? N1 C1 C2 122.2(7) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C1 C2 C3 118.1(6) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C4 C3 C2 119.4(6) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 118.9(7) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.8(6) . . ? N1 C5 C6 117.1(5) . . ? C4 C5 C6 121.1(6) . . ? O1 C6 O2 113.2(4) . . ? O1 C6 C7 110.5(4) . . ? O2 C6 C7 103.5(5) . . ? O1 C6 C5 111.2(5) . . ? O2 C6 C5 107.1(4) . . ? C7 C6 C5 111.2(4) . . ? N2 C7 C8 121.9(6) . . ? N2 C7 C6 115.0(5) . . ? C8 C7 C6 123.1(5) . . ? C7 C8 C9 119.6(6) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 118.7(6) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C11 119.0(6) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? N2 C11 C10 123.3(5) . . ? N2 C11 C12 117.7(5) . . ? C10 C11 C12 118.9(6) . . ? O3 C12 O4 113.1(5) . . ? O3 C12 C13 112.4(5) . . ? O4 C12 C13 106.7(5) . . ? O3 C12 C11 105.5(5) . . ? O4 C12 C11 110.7(5) . . ? C13 C12 C11 108.5(5) . . ? C14 C13 N3 121.6(7) . . ? C14 C13 C12 124.0(7) . . ? N3 C13 C12 114.4(6) . . ? C13 C14 C15 118.8(8) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 119.1(8) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 118.4(8) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C16 C17 N3 124.1(8) . . ? C16 C17 H17 118.0 . . ? N3 C17 H17 118.0 . . ? O2 C18 C19 105.8(6) . . ? O2 C18 H18A 110.6 . . ? C19 C18 H18A 110.6 . . ? O2 C18 H18B 110.6 . . ? C19 C18 H18B 110.6 . . ? H18A C18 H18B 108.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C20 C21 109.8(8) . . ? O4 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? O4 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C20 C21 H21A 108.0 . . ? C20 C21 H21B 108.6 . . ? H21A C21 H21B 109.7 . . ? C20 C21 H21C 108.8 . . ? H21A C21 H21C 109.8 . . ? H21B C21 H21C 111.7 . . ? C48 O32 C36 112.3(4) . . ? C42 O34 C50 114.6(5) . . ? C43 N33 C47 118.0(6) . . ? C32 C31 N31 123.4(7) . . ? C32 C31 H31 118.3 . . ? N31 C31 H31 118.3 . . ? C31 C32 C33 118.3(8) . . ? C31 C32 H32 120.9 . . ? C33 C32 H32 120.9 . . ? C34 C33 C32 119.3(8) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 119.8(7) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? N31 C35 C34 120.8(7) . . ? N31 C35 C36 115.6(6) . . ? C34 C35 C36 123.5(6) . . ? O31 C36 O32 112.6(5) . . ? O31 C36 C37 110.7(5) . . ? O32 C36 C37 103.4(4) . . ? O31 C36 C35 112.3(5) . . ? O32 C36 C35 106.7(5) . . ? C37 C36 C35 110.7(5) . . ? N32 C37 C38 121.0(5) . . ? N32 C37 C36 115.1(5) . . ? C38 C37 C36 123.8(5) . . ? C39 C38 C37 119.7(6) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C40 C39 C38 119.4(6) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C39 C40 C41 118.5(6) . . ? C39 C40 H40 120.8 . . ? C41 C40 H40 120.8 . . ? N32 C41 C40 122.2(6) . . ? N32 C41 C42 117.1(5) . . ? C40 C41 C42 120.7(5) . . ? O33 C42 O34 111.6(5) . . ? O33 C42 C41 107.8(4) . . ? O34 C42 C41 112.8(6) . . ? O33 C42 C43 112.3(5) . . ? O34 C42 C43 105.2(4) . . ? C41 C42 C43 107.2(5) . . ? N33 C43 C44 121.6(6) . . ? N33 C43 C42 114.8(5) . . ? C44 C43 C42 123.3(6) . . ? C45 C44 C43 119.8(7) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C46 C45 C44 119.3(6) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C45 C46 C47 118.5(7) . . ? C45 C46 H46 120.8 . . ? C47 C46 H46 120.8 . . ? N33 C47 C46 122.7(7) . . ? N33 C47 H47 118.6 . . ? C46 C47 H47 118.6 . . ? C49 C48 O32 109.8(7) . . ? C49 C48 H48A 109.7 . . ? O32 C48 H48A 109.7 . . ? C49 C48 H48B 109.7 . . ? O32 C48 H48B 109.7 . . ? H48A C48 H48B 108.2 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O34 C50 C51 109.1(7) . . ? O34 C50 H50A 109.9 . . ? C51 C50 H50A 109.9 . . ? O34 C50 H50B 109.9 . . ? C51 C50 H50B 109.9 . . ? H50A C50 H50B 108.3 . . ? C50 C51 H51A 109.7 . . ? C50 C51 H51B 109.8 . . ? H51A C51 H51B 111.2 . . ? C50 C51 H51C 107.9 . . ? H51A C51 H51C 108.4 . . ? H51B C51 H51C 109.8 . . ? C66 O62 C78 113.3(5) . . ? C72 O64 C80 115.1(5) . . ? C73 N63 C77 118.8(6) . . ? N61 C61 C62 123.4(6) . . ? N61 C61 H61 118.3 . . ? C62 C61 H61 118.3 . . ? C63 C62 C61 119.8(7) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 117.4(7) . . ? C62 C63 H63 121.3 . . ? C64 C63 H63 121.3 . . ? C65 C64 C63 120.7(6) . . ? C65 C64 H64 119.6 . . ? C63 C64 H64 119.6 . . ? N61 C65 C64 121.4(6) . . ? N61 C65 C66 116.0(5) . . ? C64 C65 C66 122.5(5) . . ? O61 C66 O62 113.8(5) . . ? O61 C66 C67 112.0(6) . . ? O62 C66 C67 102.4(4) . . ? O61 C66 C65 111.6(4) . . ? O62 C66 C65 106.6(5) . . ? C67 C66 C65 109.9(5) . . ? N62 C67 C68 123.0(6) . . ? N62 C67 C66 114.8(5) . . ? C68 C67 C66 122.1(6) . . ? C67 C68 C69 117.2(7) . . ? C67 C68 H68 121.4 . . ? C69 C68 H68 121.4 . . ? C70 C69 C68 120.8(6) . . ? C70 C69 H69 119.6 . . ? C68 C69 H69 119.6 . . ? C69 C70 C71 117.9(6) . . ? C69 C70 H70 121.1 . . ? C71 C70 H70 121.1 . . ? N62 C71 C70 123.2(6) . . ? N62 C71 C72 115.8(5) . . ? C70 C71 C72 121.0(6) . . ? O63 C72 O64 111.2(5) . . ? O63 C72 C71 107.2(5) . . ? O64 C72 C71 112.3(5) . . ? O63 C72 C73 111.5(5) . . ? O64 C72 C73 105.8(5) . . ? C71 C72 C73 108.9(5) . . ? N63 C73 C74 121.9(5) . . ? N63 C73 C72 115.8(5) . . ? C74 C73 C72 122.2(6) . . ? C75 C74 C73 117.2(7) . . ? C75 C74 H74 121.4 . . ? C73 C74 H74 121.4 . . ? C76 C75 C74 121.3(7) . . ? C76 C75 H75 119.3 . . ? C74 C75 H75 119.3 . . ? C75 C76 C77 118.6(6) . . ? C75 C76 H76 120.7 . . ? C77 C76 H76 120.7 . . ? N63 C77 C76 122.1(7) . . ? N63 C77 H77 119.0 . . ? C76 C77 H77 119.0 . . ? O62 C78 C79 107.5(6) . . ? O62 C78 H78A 110.2 . . ? C79 C78 H78A 110.2 . . ? O62 C78 H78B 110.2 . . ? C79 C78 H78B 110.2 . . ? H78A C78 H78B 108.5 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C81 C80 O64 107.9(7) . . ? C81 C80 H80A 110.1 . . ? O64 C80 H80A 110.1 . . ? C81 C80 H80B 110.1 . . ? O64 C80 H80B 110.1 . . ? H80A C80 H80B 108.4 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? O94 Cl1 O92 110.9(6) . . ? O94 Cl1 O92A 85.3(11) . . ? O92 Cl1 O92A 42.0(10) . . ? O94 Cl1 O93 112.1(7) . . ? O92 Cl1 O93 110.5(7) . . ? O92A Cl1 O93 92.0(11) . . ? O94 Cl1 O94A 30.4(9) . . ? O92 Cl1 O94A 130.6(10) . . ? O92A Cl1 O94A 115.3(14) . . ? O93 Cl1 O94A 113.8(11) . . ? O94 Cl1 O91A 131.1(11) . . ? O92 Cl1 O91A 71.0(11) . . ? O92A Cl1 O91A 112.9(14) . . ? O93 Cl1 O91A 112.1(12) . . ? O94A Cl1 O91A 109.9(13) . . ? O94 Cl1 O93A 112.6(9) . . ? O92 Cl1 O93A 124.8(9) . . ? O92A Cl1 O93A 111.5(12) . . ? O93 Cl1 O93A 19.5(8) . . ? O94A Cl1 O93A 103.7(11) . . ? O91A Cl1 O93A 102.4(12) . . ? O94 Cl1 O91 103.6(6) . . ? O92 Cl1 O91 105.0(6) . . ? O92A Cl1 O91 145.4(12) . . ? O93 Cl1 O91 114.2(6) . . ? O94A Cl1 O91 75.7(10) . . ? O91A Cl1 O91 37.7(10) . . ? O93A Cl1 O91 96.0(8) . . ? O95 Cl2 O96A 119.3(12) . . ? O95 Cl2 O98 114.0(12) . . ? O96A Cl2 O98 103.1(10) . . ? O95 Cl2 O98A 127.5(13) . . ? O96A Cl2 O98A 113.0(10) . . ? O98 Cl2 O98A 53.3(9) . . ? O95 Cl2 O96 101.6(12) . . ? O96A Cl2 O96 21.7(10) . . ? O98 Cl2 O96 102.0(10) . . ? O98A Cl2 O96 129.9(11) . . ? O95 Cl2 O95A 38.3(10) . . ? O96A Cl2 O95A 131.6(11) . . ? O98 Cl2 O95A 75.7(11) . . ? O98A Cl2 O95A 104.5(11) . . ? O96 Cl2 O95A 110.0(11) . . ? O95 Cl2 O97 115.2(11) . . ? O96A Cl2 O97 96.4(11) . . ? O98 Cl2 O97 106.6(10) . . ? O98A Cl2 O97 53.8(9) . . ? O96 Cl2 O97 116.9(10) . . ? O95A Cl2 O97 130.9(10) . . ? O95 Cl2 O97A 65.7(10) . . ? O96A Cl2 O97A 98.2(9) . . ? O98 Cl2 O97A 154.5(11) . . ? O98A Cl2 O97A 105.1(11) . . ? O96 Cl2 O97A 103.0(10) . . ? O95A Cl2 O97A 100.4(10) . . ? O97 Cl2 O97A 56.6(9) . . ? C91 O99 H99O 109.5 . . ? O99 C91 C92 115.3(9) . . ? O99 C91 H91A 108.5 . . ? C92 C91 H91A 108.5 . . ? O99 C91 H91B 108.5 . . ? C92 C91 H91B 108.5 . . ? H91A C91 H91B 107.5 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 64.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.893 _refine_diff_density_min -1.060 _refine_diff_density_rms 0.061 # start Validation Reply Form _vrf_PLAT220_Complex2 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.98 Ratio RESPONSE: This is due to the large thermal motion of the methyl carbon atoms of the ligand. Attempts to refine these atoms over two disordered positions converged at occupation factors 0.87 and 0.13 with isotropic model. The anisotropic model for the two positions led to analogous alerts for the site with the largest occupancy. It was thus decided to refine the structure without disorder. ; _vrf_PLAT222_Complex2 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.65 Ratio RESPONSE: This is due to the large thermal motion of the methyl carbon atoms. All hydrogen atoms were introduced at calculated positions as riding on bonded atoms and were refined with U equal to 1.3 times the Ueq of the respective atom. ; _vrf_PLAT242_Complex2 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C48 RESPONSE: This is probably a false alert due to the large thermal motion of the neighboring atoms. ;