# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1515 data_Gd(H2O)(NO3)2[enPd(dmpymo)]4(NO3)5.6H2O _audit_creation_method SHELXL-97 _chemical_name_common Gd(H2O)(NO3)2[enPd(dmpymo)]4(NO3)5.6H2O _chemical_formula_moiety 'C32 H74 Gd N23 O32 Pd4' _chemical_formula_sum 'C32 H74 Gd N23 O32 Pd4' _chemical_formula_weight 1876.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 26.8830(12) _cell_length_b 13.2671(7) _cell_length_c 17.9605(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6405.8(5) _cell_formula_units 4.0 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 12.6 _cell_measurement_theta_max 16.1 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.397 _exptl_crystal_size_min 0.280 _exptl_crystal_density_diffrn 1.927 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3684 _diffrn_measurement_device 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method ; Scan width (omega) = 0.99 - 1.57, scan ratio 2theta:omega = 1.00 I(Net) and sigma(I) from profile fitting (Clegg, 1981) ; _exptl_absorpt_coefficient_mu 2.224 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3517 _exptl_absorpt_correction_T_max 0.4669 _exptl_absorpt_process_details ; Psi Scan Reflections used Mu * R = 0.53 H K L 2Theta Chi Imin/Imax 1 1 0 3.8 76.4 0.689 2 2 0 7.6 76.4 0.787 2 2 1 7.8 86.1 0.822 3 3 1 11.6 83.4 0.825 3 4 4 14.3 77.2 0.804 3 5 1 14.7 76.9 0.774 4 5 5 18.4 78.4 0.794 5 5 0 19.2 76.4 0.832 5 4 5 19.5 76.8 0.808 4 7 5 21.6 75.9 0.794 5 6 5 22.0 82.7 0.794 5 8 5 25.2 79.4 0.774 ; _diffrn_ambient_temperature 293(1) _diffrn_radiation_collimation '0.8 mm' _diffrn_radiation_detector 'NaI(Tl) scintillation counter' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 90 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4.5 _diffrn_reflns_number 8075 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_av_sigmaI/netI 0.0926 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _reflns_number_total 8075 _reflns_number_observed 4269 _reflns_observed_criterion >4sigma(I) _reflns_d_resolution_high 0.770 _reflns_d_resolution_low 13.422 _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 34 _exptl_special_details ; ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics xp _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^)+(0.0885P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7668 _refine_ls_number_parameters 417 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 13.705 _refine_ls_shift/su_mean 0.188 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.785560(18) 0.7500 0.76631(3) 0.03670(15) Uani 1 2 d S . . Pd1 Pd 0.89356(2) 0.96345(5) 0.71743(4) 0.04379(17) Uani 1 1 d . . . Pd2 Pd 0.68199(2) 0.96471(5) 0.69824(4) 0.04687(18) Uani 1 1 d . . . C2A C 0.6723(4) 0.7500 0.6660(6) 0.050(3) Uani 1 2 d S . . O2A O 0.7080(3) 0.7500 0.7106(5) 0.054(2) Uani 1 2 d S . . N3A N 0.6528(2) 0.8408(5) 0.6433(3) 0.0455(15) Uani 1 1 d . . . C4A C 0.6129(3) 0.8401(7) 0.5983(4) 0.053(2) Uani 1 1 d . . . C41A C 0.5879(4) 0.9377(8) 0.5794(6) 0.070(3) Uani 1 1 d . . . H41A H 0.6062 0.9924 0.6012 0.106 Uiso 1 1 calc R . . H41B H 0.5546 0.9374 0.5987 0.106 Uiso 1 1 calc R . . H41C H 0.5870 0.9458 0.5263 0.106 Uiso 1 1 calc R . . C5A C 0.5933(5) 0.7500 0.5720(8) 0.060(3) Uani 1 2 d S . . H5AA H 0.5677 0.7500 0.5373 0.072 Uiso 1 2 calc SR . . N1B N 0.7466(2) 0.9812(5) 0.6354(4) 0.0505(17) Uani 1 1 d . . . C2B C 0.7893(3) 0.9595(6) 0.6720(5) 0.0463(18) Uani 1 1 d . . . O2B O 0.78700(19) 0.9201(4) 0.7363(3) 0.0472(13) Uani 1 1 d . . . N3B N 0.8350(2) 0.9833(5) 0.6429(4) 0.0472(15) Uani 1 1 d . . . C4B C 0.8367(3) 1.0264(7) 0.5753(5) 0.057(2) Uani 1 1 d . . . C41B C 0.8864(3) 1.0537(8) 0.5455(6) 0.074(3) Uani 1 1 d . . . H41D H 0.9115 1.0353 0.5809 0.111 Uiso 1 1 calc R . . H41E H 0.8877 1.1250 0.5366 0.111 Uiso 1 1 calc R . . H41F H 0.8920 1.0183 0.4996 0.111 Uiso 1 1 calc R . . C5B C 0.7940(3) 1.0446(8) 0.5358(5) 0.063(3) Uani 1 1 d . . . H5BA H 0.7957 1.0699 0.4876 0.075 Uiso 1 1 calc R . . C6B C 0.7490(3) 1.0253(7) 0.5681(5) 0.056(2) Uani 1 1 d . . . C61B C 0.7011(4) 1.0544(10) 0.5312(7) 0.089(4) Uani 1 1 d . . . H61A H 0.6737 1.0349 0.5622 0.133 Uiso 1 1 calc R . . H61B H 0.6986 1.0210 0.4839 0.133 Uiso 1 1 calc R . . H61C H 0.7004 1.1261 0.5238 0.133 Uiso 1 1 calc R . . N1C N 0.9259(2) 0.8402(5) 0.6662(3) 0.0437(14) Uani 1 1 d . . . C2C C 0.9051(4) 0.7500 0.6861(6) 0.041(2) Uani 1 2 d S . . O2C O 0.8675(3) 0.7500 0.7280(4) 0.0477(18) Uani 1 2 d S . . C5C C 0.9885(4) 0.7500 0.6024(7) 0.059(3) Uani 1 2 d S . . H5CA H 1.0158 0.7500 0.5706 0.071 Uiso 1 2 calc SR . . C6C C 0.9685(3) 0.8412(7) 0.6259(4) 0.0489(19) Uani 1 1 d . . . C61C C 0.9932(3) 0.9374(8) 0.6089(6) 0.063(2) Uani 1 1 d . . . H61D H 0.9739 0.9920 0.6289 0.095 Uiso 1 1 calc R . . H61E H 0.9960 0.9451 0.5559 0.095 Uiso 1 1 calc R . . H61F H 1.0257 0.9379 0.6308 0.095 Uiso 1 1 calc R . . N11 N 0.7042(3) 1.0835(6) 0.7601(5) 0.070(2) Uani 1 1 d . . . H11C H 0.7315 1.0670 0.7863 0.084 Uiso 1 1 calc R . . H11D H 0.7118 1.1356 0.7302 0.084 Uiso 1 1 calc R . . C11 C 0.6636(4) 1.1134(8) 0.8120(7) 0.076(3) Uani 1 1 d . . . H11A H 0.6772 1.1497 0.8542 0.092 Uiso 1 1 calc R . . H11B H 0.6400 1.1570 0.7867 0.092 Uiso 1 1 calc R . . N12 N 0.6241(3) 0.9626(6) 0.7709(4) 0.0559(18) Uani 1 1 d . . . H12C H 0.5970 0.9904 0.7497 0.067 Uiso 1 1 calc R . . H12D H 0.6167 0.8986 0.7834 0.067 Uiso 1 1 calc R . . C12 C 0.6383(3) 1.0202(7) 0.8376(5) 0.059(2) Uani 1 1 d . . . H12A H 0.6606 0.9807 0.8685 0.070 Uiso 1 1 calc R . . H12B H 0.6090 1.0370 0.8666 0.070 Uiso 1 1 calc R . . N21 N 0.9454(3) 0.9543(6) 0.7995(4) 0.0529(17) Uani 1 1 d . . . H21C H 0.9505 0.8895 0.8122 0.063 Uiso 1 1 calc R . . H21D H 0.9745 0.9803 0.7836 0.063 Uiso 1 1 calc R . . C21 C 0.9270(4) 1.0121(8) 0.8648(5) 0.066(3) Uani 1 1 d . . . H21A H 0.9027 0.9724 0.8919 0.079 Uiso 1 1 calc R . . H21B H 0.9544 1.0273 0.8982 0.079 Uiso 1 1 calc R . . N22 N 0.8673(3) 1.0792(6) 0.7802(5) 0.065(2) Uani 1 1 d . . . H22C H 0.8616 1.1332 0.7511 0.077 Uiso 1 1 calc R . . H22D H 0.8384 1.0613 0.8017 0.077 Uiso 1 1 calc R . . C22 C 0.9043(4) 1.1054(8) 0.8384(7) 0.077(3) Uani 1 1 d . . . H22A H 0.9296 1.1496 0.8179 0.092 Uiso 1 1 calc R . . H22B H 0.8881 1.1400 0.8793 0.092 Uiso 1 1 calc R . . N31 N 0.7059(4) 0.7500 0.8808(5) 0.051(2) Uani 1 2 d S . . O31 O 0.7261(2) 0.8307(5) 0.8583(3) 0.0577(15) Uani 1 1 d . . . O32 O 0.6694(3) 0.7500 0.9208(6) 0.075(3) Uani 1 2 d S . . N41 N 0.8461(4) 0.7500 0.9034(5) 0.054(3) Uani 1 2 d S . . O41 O 0.8331(2) 0.8304(5) 0.8705(3) 0.0597(15) Uani 1 1 d . . . O42 O 0.8687(4) 0.7500 0.9615(5) 0.084(3) Uani 1 2 d S . . N51 N 0.7890(5) 1.2500 0.6728(8) 0.084(4) Uiso 1 2 d SD . . O51 O 0.7496(5) 1.2500 0.6375(10) 0.151(6) Uiso 1 2 d SD . . O52 O 0.8282(5) 1.2500 0.6357(11) 0.180(8) Uiso 1 2 d SD . . O53 O 0.7897(7) 1.2500 0.7327(12) 0.150(7) Uiso 1 2 d S . . N61 N 0.9609(6) 0.7500 0.3945(10) 0.108(5) Uiso 1 2 d SD . . O61 O 0.9507(6) 0.8281(10) 0.4258(8) 0.196(6) Uiso 1 1 d D . . O62 O 0.9876(9) 0.7500 0.3392(11) 0.230(11) Uiso 1 2 d SD . . N71 N 0.5211(6) 1.2500 0.5686(8) 0.092(4) Uiso 1 2 d SD . . O72 O 0.5354(6) 1.2500 0.6336(7) 0.137(6) Uiso 1 2 d SD . . O71 O 0.5170(4) 1.1703(8) 0.5349(6) 0.145(4) Uiso 1 1 d D . . N81 N 0.5549(4) 0.7500 0.7529(6) 0.056(3) Uani 1 2 d S . . O81 O 0.5369(2) 0.8314(5) 0.7318(4) 0.0668(18) Uani 1 1 d . . . O82 O 0.5927(3) 0.7500 0.7945(6) 0.067(2) Uani 1 2 d S . . N91 N 0.7254(9) 0.7500 0.4606(14) 0.058(6) Uiso 0.50 2 d SPD . . O91 O 0.7255(10) 0.8140(17) 0.5099(13) 0.131(9) Uiso 0.50 1 d PD . . O92 O 0.6904(16) 0.7500 0.416(2) 0.20(3) Uiso 0.50 2 d SPD . . N911 N 0.753(5) 0.7500 0.419(9) 0.27(7) Uiso 0.50 2 d SP . . O911 O 0.7606(12) 0.8291(4) 0.457(2) 0.216(12) Uiso 0.50 1 d PD . . O921 O 0.6921(13) 0.7500 0.460(5) 0.24(3) Uiso 0.50 2 d SPD . . O1W O 0.7913(3) 0.7500 0.6279(5) 0.061(2) Uani 1 2 d S . . O2W O 0.9601(4) 0.7500 0.8681(6) 0.072(3) Uani 1 2 d S . . O3W O 1.0332(3) 1.0905(6) 0.7663(4) 0.082(2) Uani 1 1 d . . . O4W O 0.7796(4) 1.0432(10) 0.8710(7) 0.146(4) Uiso 1 1 d . . . O5W O 0.8583(7) 0.7500 0.5119(11) 0.157(7) Uiso 1 2 d S . . O6W O 0.6440(10) 1.2500 0.6502(16) 0.099(8) Uiso 0.50 2 d SP . . O7W O 0.9133(11) 1.2500 0.6875(17) 0.104(10) Uiso 0.50 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0358(3) 0.0399(3) 0.0344(3) 0.000 0.00073(19) 0.000 Pd1 0.0382(3) 0.0438(3) 0.0494(3) 0.0036(3) 0.0017(2) -0.0007(2) Pd2 0.0382(3) 0.0475(4) 0.0549(4) 0.0094(3) -0.0003(2) 0.0008(2) C2A 0.034(5) 0.083(9) 0.033(5) 0.000 -0.002(4) 0.000 O2A 0.048(5) 0.055(5) 0.058(5) 0.000 -0.019(4) 0.000 N3A 0.039(3) 0.056(4) 0.042(3) 0.006(3) -0.003(3) -0.003(3) C4A 0.044(4) 0.074(6) 0.040(4) 0.002(4) 0.006(3) 0.001(4) C41A 0.063(6) 0.082(7) 0.066(6) 0.013(5) -0.016(5) -0.002(5) C5A 0.047(6) 0.076(9) 0.057(8) 0.000 -0.009(6) 0.000 N1B 0.039(3) 0.050(4) 0.063(4) 0.020(3) -0.003(3) 0.005(3) C2B 0.036(4) 0.050(5) 0.053(5) 0.008(4) 0.001(3) 0.001(3) O2B 0.048(3) 0.046(3) 0.048(3) 0.016(3) -0.002(2) 0.002(2) N3B 0.042(3) 0.047(4) 0.052(4) 0.007(3) 0.003(3) -0.002(3) C4B 0.059(5) 0.058(5) 0.054(5) 0.018(4) 0.001(4) 0.001(4) C41B 0.062(6) 0.082(7) 0.078(7) 0.026(6) 0.020(5) -0.003(5) C5B 0.066(5) 0.075(7) 0.047(5) 0.031(5) -0.002(4) 0.004(5) C6B 0.046(4) 0.067(6) 0.056(5) 0.021(4) 0.000(4) 0.005(4) C61B 0.061(6) 0.117(10) 0.088(8) 0.054(8) -0.006(6) 0.014(6) N1C 0.038(3) 0.050(4) 0.044(3) 0.007(3) 0.003(3) -0.002(3) C2C 0.030(5) 0.060(7) 0.033(5) 0.000 -0.003(4) 0.000 O2C 0.045(4) 0.049(5) 0.050(4) 0.000 0.010(3) 0.000 C5C 0.038(6) 0.100(11) 0.040(6) 0.000 0.002(5) 0.000 C6C 0.037(4) 0.068(6) 0.041(4) 0.004(4) 0.006(3) -0.002(4) C61C 0.043(4) 0.073(6) 0.073(6) 0.019(5) 0.004(4) -0.006(4) N11 0.055(4) 0.052(5) 0.102(7) -0.004(5) 0.011(4) -0.008(4) C11 0.068(6) 0.069(7) 0.093(8) -0.017(6) -0.004(6) 0.011(5) N12 0.040(3) 0.059(5) 0.070(5) 0.004(4) 0.006(3) 0.001(3) C12 0.054(5) 0.060(6) 0.062(5) -0.001(4) 0.000(4) 0.008(4) N21 0.048(4) 0.059(5) 0.051(4) -0.010(3) -0.005(3) 0.000(3) C21 0.065(6) 0.079(7) 0.054(5) -0.014(5) 0.002(4) 0.003(5) N22 0.056(4) 0.053(5) 0.085(6) -0.012(4) -0.001(4) 0.003(4) C22 0.068(6) 0.062(6) 0.100(8) -0.027(6) -0.019(6) 0.002(5) N31 0.047(5) 0.070(7) 0.037(5) 0.000 0.010(4) 0.000 O31 0.072(4) 0.046(3) 0.055(3) -0.009(3) 0.016(3) -0.007(3) O32 0.058(5) 0.093(8) 0.073(6) 0.000 0.021(5) 0.000 N41 0.045(5) 0.087(8) 0.030(5) 0.000 0.004(4) 0.000 O41 0.064(4) 0.064(4) 0.051(3) -0.013(3) -0.009(3) 0.010(3) O42 0.059(6) 0.149(11) 0.043(5) 0.000 -0.015(4) 0.000 N81 0.039(5) 0.063(7) 0.065(7) 0.000 0.007(5) 0.000 O81 0.059(4) 0.064(4) 0.077(4) 0.009(3) -0.002(3) 0.010(3) O82 0.048(5) 0.071(6) 0.081(7) 0.000 -0.015(5) 0.000 O1W 0.061(5) 0.077(6) 0.046(5) 0.000 0.000(4) 0.000 O2W 0.060(6) 0.076(7) 0.081(7) 0.000 0.012(5) 0.000 O3W 0.069(5) 0.072(5) 0.104(6) -0.007(4) 0.010(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2C 2.307(8) . ? Gd1 O2A 2.314(7) . ? Gd1 O2B 2.321(6) 7_575 ? Gd1 O2B 2.321(6) . ? Gd1 O1W 2.491(9) . ? Gd1 O41 2.504(6) . ? Gd1 O41 2.504(6) 7_575 ? Gd1 O31 2.536(6) 7_575 ? Gd1 O31 2.536(6) . ? Gd1 N41 2.950(10) . ? Gd1 N31 2.969(9) . ? Pd1 N21 2.033(7) . ? Pd1 N22 2.032(8) . ? Pd1 N1C 2.067(7) . ? Pd1 N3B 2.083(7) . ? Pd1 Pd1 5.6637(17) 7_575 ? Pd1 Pd2 5.6981(14) . ? Pd1 Pd2 8.0458(15) 7_575 ? Pd2 N11 2.019(8) . ? Pd2 N12 2.032(7) . ? Pd2 N3A 2.071(7) . ? Pd2 N1B 2.084(7) . ? C2A O2A 1.250(13) . ? C2A N3A 1.375(8) 7_575 ? C2A N3A 1.375(8) . ? O2A O2C 4.300(12) . ? N3A C4A 1.344(10) . ? C4A C5A 1.388(11) . ? C4A C41A 1.497(13) . ? C5A C4A 1.388(11) 7_575 ? C5A C5C 10.638(17) . ? N1B C6B 1.343(10) . ? N1B C2B 1.353(9) . ? C2B O2B 1.268(10) . ? C2B N3B 1.373(9) . ? O2B O2B 4.514(12) 7_575 ? N3B C4B 1.343(10) . ? C4B C5B 1.371(12) . ? C4B C41B 1.482(12) . ? C5B C6B 1.367(12) . ? C5B C5B 7.82(2) 7_575 ? C6B C61B 1.498(12) . ? N1C C6C 1.354(9) . ? N1C C2C 1.368(8) . ? C2C O2C 1.261(12) . ? C2C N1C 1.368(8) 7_575 ? C5C C6C 1.390(10) 7_575 ? C5C C6C 1.390(10) . ? C6C C61C 1.471(12) . ? N11 C11 1.489(13) . ? C11 C12 1.484(14) . ? N12 C12 1.472(12) . ? N21 C21 1.486(11) . ? C21 C22 1.460(14) . ? N22 C22 1.484(12) . ? N31 O32 1.215(12) . ? N31 O31 1.267(7) . ? N31 O31 1.267(7) 7_575 ? N41 O42 1.209(12) . ? N41 O41 1.268(8) 7_575 ? N41 O41 1.268(8) . ? N51 O53 1.08(2) . ? N51 O51 1.234(9) . ? N51 O52 1.247(9) . ? N61 O61 1.210(8) . ? N61 O61 1.210(8) 7_575 ? N61 O62 1.227(9) . ? N71 O71 1.223(7) . ? N71 O71 1.223(7) 7_585 ? N71 O72 1.231(9) . ? N81 O81 1.243(8) 7_575 ? N81 O81 1.243(8) . ? N81 O82 1.262(13) . ? N91 O921 0.90(4) . ? N91 O911 1.42(3) . ? N91 O911 1.42(3) 7_575 ? N91 O92 1.234(10) . ? N91 O91 1.226(10) . ? N91 O91 1.226(10) 7_575 ? O91 N911 1.98(14) . ? O91 O911 1.36(4) . ? O91 O91 1.70(5) 7_575 ? O92 N911 1.69(14) . ? N911 O921 1.80(14) . ? N911 O91 1.98(14) 7_575 ? N911 O911 1.27(10) . ? N911 O911 1.27(10) 7_575 ? O911 O911 2.100(10) 7_575 ? 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 O2C Gd1 O2A 137.0(3) . . ? O2C Gd1 O2B 85.11(13) . 7_575 ? O2A Gd1 O2B 85.10(14) . 7_575 ? O2C Gd1 O2B 85.11(14) . . ? O2A Gd1 O2B 85.10(14) . . ? O2B Gd1 O2B 153.0(3) 7_575 . ? O2C Gd1 O1W 69.1(3) . . ? O2A Gd1 O1W 68.0(3) . . ? O2B Gd1 O1W 76.52(14) 7_575 . ? O2B Gd1 O1W 76.52(14) . . ? O2C Gd1 O41 74.7(2) . . ? O2A Gd1 O41 141.6(2) . . ? O2B Gd1 O41 125.4(2) 7_575 . ? O2B Gd1 O41 75.6(2) . . ? O1W Gd1 O41 135.5(2) . . ? O2C Gd1 O41 74.7(2) . 7_575 ? O2A Gd1 O41 141.6(2) . 7_575 ? O2B Gd1 O41 75.6(2) 7_575 7_575 ? O2B Gd1 O41 125.4(2) . 7_575 ? O1W Gd1 O41 135.5(2) . 7_575 ? O41 Gd1 O41 50.4(3) . 7_575 ? O2C Gd1 O31 142.7(2) . 7_575 ? O2A Gd1 O31 73.4(2) . 7_575 ? O2B Gd1 O31 75.61(19) 7_575 7_575 ? O2B Gd1 O31 124.92(19) . 7_575 ? O1W Gd1 O31 133.6(2) . 7_575 ? O41 Gd1 O31 90.9(2) . 7_575 ? O41 Gd1 O31 69.8(2) 7_575 7_575 ? O2C Gd1 O31 142.7(2) . . ? O2A Gd1 O31 73.4(2) . . ? O2B Gd1 O31 124.92(19) 7_575 . ? O2B Gd1 O31 75.61(19) . . ? O1W Gd1 O31 133.6(2) . . ? O41 Gd1 O31 69.8(2) . . ? O41 Gd1 O31 90.9(2) 7_575 . ? O31 Gd1 O31 49.9(3) 7_575 . ? O2C Gd1 N41 73.9(3) . . ? O2A Gd1 N41 149.1(3) . . ? O2B Gd1 N41 100.65(14) 7_575 . ? O2B Gd1 N41 100.65(14) . . ? O1W Gd1 N41 143.0(3) . . ? O41 Gd1 N41 25.21(15) . . ? O41 Gd1 N41 25.21(15) 7_575 . ? O31 Gd1 N41 78.7(2) 7_575 . ? O31 Gd1 N41 78.7(2) . . ? O2C Gd1 N31 153.5(3) . . ? O2A Gd1 N31 69.5(3) . . ? O2B Gd1 N31 99.96(14) 7_575 . ? O2B Gd1 N31 99.96(14) . . ? O1W Gd1 N31 137.4(3) . . ? O41 Gd1 N31 81.4(2) . . ? O41 Gd1 N31 81.4(2) 7_575 . ? O31 Gd1 N31 25.05(14) 7_575 . ? O31 Gd1 N31 25.05(14) . . ? N41 Gd1 N31 79.6(3) . . ? N21 Pd1 N22 83.1(3) . . ? N21 Pd1 N1C 89.3(3) . . ? N22 Pd1 N1C 172.1(3) . . ? N21 Pd1 N3B 172.7(3) . . ? N22 Pd1 N3B 89.9(3) . . ? N1C Pd1 N3B 97.6(3) . . ? N21 Pd1 Pd1 86.6(2) . 7_575 ? N22 Pd1 Pd1 139.1(3) . 7_575 ? N1C Pd1 Pd1 37.74(17) . 7_575 ? N3B Pd1 Pd1 97.27(19) . 7_575 ? N21 Pd1 Pd2 136.8(2) . . ? N22 Pd1 Pd2 71.6(2) . . ? N1C Pd1 Pd2 113.28(17) . . ? N3B Pd1 Pd2 37.49(18) . . ? Pd1 Pd1 Pd2 90.168(9) 7_575 . ? N21 Pd1 Pd2 118.3(2) . 7_575 ? N22 Pd1 Pd2 108.2(2) . 7_575 ? N1C Pd1 Pd2 73.74(17) . 7_575 ? N3B Pd1 Pd2 61.82(18) . 7_575 ? Pd1 Pd1 Pd2 45.089(10) 7_575 7_575 ? Pd2 Pd1 Pd2 45.079(14) . 7_575 ? N11 Pd2 N12 83.3(3) . . ? N11 Pd2 N3A 173.6(3) . . ? N12 Pd2 N3A 90.3(3) . . ? N11 Pd2 N1B 88.3(3) . . ? N12 Pd2 N1B 171.3(3) . . ? N3A Pd2 N1B 98.1(3) . . ? N11 Pd2 Pd1 71.0(2) . . ? N12 Pd2 Pd1 136.6(2) . . ? N3A Pd2 Pd1 113.85(17) . . ? N1B Pd2 Pd1 36.94(18) . . ? O2A C2A N3A 118.8(5) . 7_575 ? O2A C2A N3A 118.8(5) . . ? N3A C2A N3A 122.4(9) 7_575 . ? C2A O2A Gd1 165.7(8) . . ? C2A O2A O2C 144.3(7) . . ? Gd1 O2A O2C 21.46(16) . . ? C4A N3A C2A 118.3(8) . . ? C4A N3A Pd2 126.5(6) . . ? C2A N3A Pd2 114.2(5) . . ? N3A C4A C5A 120.9(9) . . ? N3A C4A C41A 119.2(8) . . ? C5A C4A C41A 119.9(8) . . ? C4A C5A C4A 118.8(12) . 7_575 ? C4A C5A C5C 66.7(6) . . ? C4A C5A C5C 66.7(6) 7_575 . ? C6B N1B C2B 119.4(7) . . ? C6B N1B Pd2 124.9(5) . . ? C2B N1B Pd2 114.9(5) . . ? O2B C2B N1B 119.3(7) . . ? O2B C2B N3B 119.0(7) . . ? N1B C2B N3B 121.6(7) . . ? C2B O2B Gd1 127.8(6) . . ? C2B O2B O2B 114.3(5) . 7_575 ? Gd1 O2B O2B 13.48(14) . 7_575 ? C4B N3B C2B 118.2(7) . . ? C4B N3B Pd1 127.5(6) . . ? C2B N3B Pd1 113.7(5) . . ? N3B C4B C5B 120.9(8) . . ? N3B C4B C41B 117.5(8) . . ? C5B C4B C41B 121.6(8) . . ? C4B C5B C6B 119.3(8) . . ? C4B C5B C5B 79.8(6) . 7_575 ? C6B C5B C5B 79.2(6) . 7_575 ? N1B C6B C5B 120.3(7) . . ? N1B C6B C61B 118.0(8) . . ? C5B C6B C61B 121.6(8) . . ? C6C N1C C2C 119.5(7) . . ? C6C N1C Pd1 125.9(6) . . ? C2C N1C Pd1 113.9(5) . . ? O2C C2C N1C 118.9(5) . . ? O2C C2C N1C 118.9(5) . 7_575 ? N1C C2C N1C 122.1(9) . 7_575 ? C2C O2C Gd1 160.7(7) . . ? C2C O2C O2A 139.2(6) . . ? Gd1 O2C O2A 21.52(16) . . ? C6C C5C C6C 121.0(11) 7_575 . ? C6C C5C C5A 68.2(6) 7_575 . ? C6C C5C C5A 68.2(6) . . ? N1C C6C C5C 118.8(8) . . ? N1C C6C C61C 120.0(8) . . ? C5C C6C C61C 121.2(7) . . ? C11 N11 Pd2 109.6(6) . . ? C12 C11 N11 107.9(8) . . ? C12 N12 Pd2 108.4(5) . . ? N12 C12 C11 107.4(8) . . ? C21 N21 Pd1 108.2(5) . . ? C22 C21 N21 108.7(8) . . ? C22 N22 Pd1 109.6(6) . . ? C21 C22 N22 108.1(8) . . ? O32 N31 O31 122.3(4) . . ? O32 N31 O31 122.3(4) . 7_575 ? O31 N31 O31 115.4(9) . 7_575 ? O32 N31 Gd1 172.4(8) . . ? O31 N31 Gd1 58.0(4) . . ? O31 N31 Gd1 58.0(4) 7_575 . ? N31 O31 Gd1 97.0(5) . . ? O42 N41 O41 122.7(5) . 7_575 ? O42 N41 O41 122.7(5) . . ? O41 N41 O41 114.5(9) 7_575 . ? O42 N41 Gd1 176.8(8) . . ? O41 N41 Gd1 57.3(5) 7_575 . ? O41 N41 Gd1 57.3(5) . . ? N41 O41 Gd1 97.5(5) . . ? O53 N51 O51 121.9(18) . . ? O53 N51 O52 121.4(19) . . ? O51 N51 O52 116.7(12) . . ? O61 N61 O61 117.9(19) . 7_575 ? O61 N61 O62 120.5(9) . . ? O61 N61 O62 120.5(9) 7_575 . ? O71 N71 O71 119.6(15) . 7_585 ? O71 N71 O72 119.9(7) . . ? O71 N71 O72 119.9(7) 7_585 . ? O81 N81 O81 120.6(11) 7_575 . ? O81 N81 O82 119.7(6) 7_575 . ? O81 N81 O82 119.7(6) . . ? O921 N91 O911 131.9(13) . . ? O921 N91 O911 131.9(13) . 7_575 ? O911 N91 O911 96(2) . 7_575 ? O921 N91 O92 39(5) . . ? O911 N91 O92 119(2) . . ? O911 N91 O92 119(2) 7_575 . ? O921 N91 O91 91(4) . . ? O911 N91 O91 61.4(17) . . ? O911 N91 O91 123(2) 7_575 . ? O92 N91 O91 117.9(13) . . ? O921 N91 O91 91(4) . 7_575 ? O911 N91 O91 123(2) . 7_575 ? O911 N91 O91 61.4(17) 7_575 7_575 ? O92 N91 O91 117.9(13) . 7_575 ? O91 N91 O91 88(3) . 7_575 ? N911 O91 N91 27(3) . . ? N911 O91 O911 39(3) . . ? N91 O91 O911 66.2(15) . . ? N911 O91 O91 65(2) . 7_575 ? N91 O91 O91 46.2(14) . 7_575 ? O911 O91 O91 98.5(10) . 7_575 ? N911 O92 N91 39(6) . . ? O921 N911 O92 26(3) . . ? O921 N911 O91 47(4) . . ? O92 N911 O91 70(5) . . ? O921 N911 O91 47(4) . 7_575 ? O92 N911 O91 70(5) . 7_575 ? O91 N911 O91 51(4) . 7_575 ? O921 N911 O911 86(8) . . ? O92 N911 O911 100(7) . . ? O91 N911 O911 43(5) . . ? O91 N911 O911 89(9) 7_575 . ? O921 N911 O911 86(8) . 7_575 ? O92 N911 O911 100(7) . 7_575 ? O91 N911 O911 89(9) . 7_575 ? O91 N911 O911 43(5) 7_575 7_575 ? O911 N911 O911 112(10) . 7_575 ? N91 O911 O91 52.4(11) . . ? N91 O911 O911 42.1(12) . 7_575 ? O91 O911 O911 81.5(10) . 7_575 ? N91 O911 N911 46(6) . . ? O91 O911 N911 98(7) . . ? O911 O911 N911 34(7) 7_575 . ? N911 O921 N91 25(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N21 H21C O2W 0.90 2.12 3.004(9) 166.5 . N21 H21D O3W 0.90 2.18 3.032(11) 158.7 . N11 H11C O4W 0.90 2.02 2.892(16) 162.5 . N22 H22D O4W 0.90 2.03 2.908(15) 165.7 . N22 H22C O7W 0.90 2.37 3.07(2) 134.4 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.473 _refine_diff_density_min -1.252 _refine_diff_density_rms 0.169