Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 _publ_contact_author_name 'Prof. David Parker' _publ_contact_author_address ; Department of Chemistry Durham University Durham DH1 3LE UK ; _publ_contact_author_phone '+44 191 374 3133' _publ_contact_author_fax '+44 191 3844737' _publ_contact_author_email david.parker@durham.ac.uk loop_ _publ_author_name 'Alessandro Barge' 'Mauro Botta' 'David Parker' 'Horst Puschmann' _publ_requested_journal 'Chemical Communications' _publ_section_title ; The Nature of Anion Determines the Rate if Water Exchange in a Metal Complex ; #============================================ data_02srv249 _database_code_CSD 204855 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H34 Gd1 N8 O5 3+,3(N O3 1-),3(H2 O)' _chemical_formula_sum 'C16 H40 Gd N11 O17' _chemical_formula_weight 815.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2067(2) _cell_length_b 10.3352(2) _cell_length_c 16.0092(3) _cell_angle_alpha 91.6440(10) _cell_angle_beta 99.2690(10) _cell_angle_gamma 116.0800(10) _cell_volume 1487.57(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6249 _cell_measurement_theta_min 2.586 _cell_measurement_theta_max 30.014 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 826 _exptl_absorpt_coefficient_mu 2.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4212 _exptl_absorpt_correction_T_max 0.6537 _exptl_absorpt_process_details 'SADABS v.2.03 (Sheldrick, 2001), R(int)=0.0719 before correction' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of 3 sets of \w scans; each set at different \f and/or 2\q angles and each scan (5 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.85 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 6K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 12937 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 26.99 _reflns_number_total 6435 _reflns_number_gt 6262 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.049 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.049 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 1997)' _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^)+(0.0243P)^2^+1.2457P] 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 6435 _refine_ls_number_parameters 441 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0196 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0491 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.017 _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 0.733115(9) 0.673440(9) 0.734700(5) 0.01205(4) Uani 1 1 d . . . O1 O 0.95194(15) 0.88797(15) 0.79193(9) 0.0172(3) Uani 1 1 d . . . O2 O 0.88769(16) 0.63318(15) 0.65268(9) 0.0175(3) Uani 1 1 d . . . O3 O 0.54942(15) 0.56154(15) 0.60921(8) 0.0162(3) Uani 1 1 d . . . O4 O 0.59455(16) 0.80463(15) 0.74876(9) 0.0166(3) Uani 1 1 d . . . O5 O 0.79177(16) 0.85805(16) 0.63396(9) 0.0185(3) Uani 1 1 d . . . H5A H 0.7143 0.8521 0.6058 0.028 Uiso 1 1 calc R . . H5BB H 0.818(4) 0.939(4) 0.661(2) 0.043(9) Uiso 1 1 d . . . N1 N 0.93183(19) 0.63112(18) 0.84575(10) 0.0157(3) Uani 1 1 d . . . N2 N 0.68874(18) 0.40020(17) 0.71916(10) 0.0153(3) Uani 1 1 d . . . N3 N 0.47058(18) 0.49388(17) 0.76517(10) 0.0148(3) Uani 1 1 d . . . N4 N 0.71530(18) 0.72628(18) 0.89211(10) 0.0152(3) Uani 1 1 d . . . N11 N 1.1895(2) 1.0110(2) 0.86002(12) 0.0229(4) Uani 1 1 d . . . H11A H 1.1878 1.0928 0.8540 0.028 Uiso 1 1 calc R . . H11B H 1.2691 1.0090 0.8858 0.028 Uiso 1 1 calc R . . N21 N 0.9815(2) 0.49708(19) 0.59760(11) 0.0208(3) Uani 1 1 d . . . H21A H 1.0574 0.5728 0.5890 0.025 Uiso 1 1 calc R . . H21B H 0.9726 0.4121 0.5839 0.025 Uiso 1 1 calc R . . N31 N 0.31482(19) 0.41458(19) 0.54202(11) 0.0184(3) Uani 1 1 d . . . H31A H 0.3427 0.4122 0.4943 0.022 Uiso 1 1 calc R . . H31B H 0.2225 0.3672 0.5450 0.022 Uiso 1 1 calc R . . N41 N 0.5240(2) 0.9413(2) 0.82472(12) 0.0232(4) Uani 1 1 d . . . H41A H 0.4679 0.9475 0.7804 0.028 Uiso 1 1 calc R . . H41B H 0.5304 0.9832 0.8734 0.028 Uiso 1 1 calc R . . C1 C 0.9278(2) 0.4882(2) 0.82434(13) 0.0186(4) Uani 1 1 d . . . H1A H 0.9765 0.4626 0.8737 0.022 Uiso 1 1 calc R . . H1B H 0.9818 0.4948 0.7787 0.022 Uiso 1 1 calc R . . C2 C 0.7692(2) 0.3710(2) 0.79695(13) 0.0187(4) Uani 1 1 d . . . H2A H 0.7700 0.2786 0.7858 0.022 Uiso 1 1 calc R . . H2B H 0.7162 0.3637 0.8431 0.022 Uiso 1 1 calc R . . C3 C 0.5278(2) 0.2988(2) 0.70832(13) 0.0174(4) Uani 1 1 d . . . H3A H 0.5161 0.2020 0.7167 0.021 Uiso 1 1 calc R . . H3B H 0.4788 0.2960 0.6506 0.021 Uiso 1 1 calc R . . C4 C 0.4541(2) 0.3437(2) 0.77072(13) 0.0175(4) Uani 1 1 d . . . H4A H 0.3491 0.2763 0.7601 0.021 Uiso 1 1 calc R . . H4B H 0.4969 0.3370 0.8281 0.021 Uiso 1 1 calc R . . C5 C 0.4447(2) 0.5460(2) 0.84610(12) 0.0166(4) Uani 1 1 d . . . H5B H 0.3642 0.4669 0.8651 0.020 Uiso 1 1 calc R . . H5C H 0.4157 0.6226 0.8359 0.020 Uiso 1 1 calc R . . C6 C 0.5844(2) 0.6027(2) 0.91536(12) 0.0177(4) Uani 1 1 d . . . H6A H 0.5633 0.6341 0.9671 0.021 Uiso 1 1 calc R . . H6B H 0.6098 0.5242 0.9272 0.021 Uiso 1 1 calc R . . C7 C 0.8519(2) 0.7495(2) 0.95362(12) 0.0182(4) Uani 1 1 d . . . H7A H 0.8312 0.7442 1.0108 0.022 Uiso 1 1 calc R . . H7B H 0.9299 0.8459 0.9514 0.022 Uiso 1 1 calc R . . C8 C 0.9060(2) 0.6384(2) 0.93482(12) 0.0192(4) Uani 1 1 d . . . H8A H 0.9980 0.6619 0.9743 0.023 Uiso 1 1 calc R . . H8B H 0.8331 0.5436 0.9444 0.023 Uiso 1 1 calc R . . C10 C 1.0786(2) 0.7484(2) 0.83900(13) 0.0185(4) Uani 1 1 d . . . H10A H 1.1110 0.7231 0.7900 0.022 Uiso 1 1 calc R . . H10B H 1.1511 0.7595 0.8895 0.022 Uiso 1 1 calc R . . C11 C 1.0702(2) 0.8893(2) 0.82988(12) 0.0171(4) Uani 1 1 d . . . C20 C 0.7446(2) 0.3758(2) 0.64329(13) 0.0182(4) Uani 1 1 d . . . H20A H 0.6668 0.3489 0.5931 0.022 Uiso 1 1 calc R . . H20B H 0.7708 0.2967 0.6499 0.022 Uiso 1 1 calc R . . C21 C 0.8794(2) 0.5112(2) 0.63165(12) 0.0168(4) Uani 1 1 d . . . C30 C 0.3594(2) 0.4927(2) 0.69257(12) 0.0155(4) Uani 1 1 d . . . H30A H 0.3444 0.5784 0.7003 0.019 Uiso 1 1 calc R . . H30B H 0.2651 0.4081 0.6905 0.019 Uiso 1 1 calc R . . C31 C 0.4126(2) 0.4900(2) 0.60992(12) 0.0154(4) Uani 1 1 d . . . C40 C 0.6974(2) 0.8610(2) 0.89794(12) 0.0179(4) Uani 1 1 d . . . H40A H 0.7942 0.9445 0.9061 0.021 Uiso 1 1 calc R . . H40B H 0.6533 0.8643 0.9468 0.021 Uiso 1 1 calc R . . C41 C 0.5998(2) 0.8677(2) 0.81805(13) 0.0168(4) Uani 1 1 d . . . N10 N 0.61918(19) 0.21459(19) 0.98148(10) 0.0180(3) Uani 1 1 d . . . O11 O 0.6623(2) 0.11865(18) 0.99015(11) 0.0318(4) Uani 1 1 d . . . O12 O 0.69452(19) 0.33782(17) 1.02099(11) 0.0277(3) Uani 1 1 d . . . O13 O 0.49847(17) 0.18518(17) 0.93163(10) 0.0237(3) Uani 1 1 d . . . N20 N 1.3220(2) 0.8283(2) 0.61863(12) 0.0271(4) Uani 1 1 d . . . O21 O 1.2606(2) 0.8176(3) 0.68048(12) 0.0538(6) Uani 1 1 d . . . O22 O 1.4248(2) 0.9465(2) 0.60858(16) 0.0521(6) Uani 1 1 d . . . O23 O 1.2836(2) 0.7209(2) 0.56746(12) 0.0431(5) Uani 1 1 d . . . N30 N 0.9799(2) 1.1784(2) 0.78465(14) 0.0262(4) Uani 1 1 d . . . O31A O 1.1198(2) 1.2386(2) 0.79459(18) 0.0323(5) Uani 0.73 1 d P A 1 O32A O 0.9270(3) 1.1651(2) 0.85311(13) 0.0226(4) Uani 0.73 1 d P A 1 O33A O 0.8990(3) 1.1437(3) 0.71506(15) 0.0253(5) Uani 0.73 1 d P A 1 O31B O 1.0786(10) 1.1896(9) 0.7311(6) 0.0497(19) Uiso 0.27 1 d P A 2 O32B O 1.0068(13) 1.2032(12) 0.8498(7) 0.060(3) Uiso 0.27 1 d P A 2 O33B O 0.8469(8) 1.1090(8) 0.7320(5) 0.0237(17) Uiso 0.27 1 d P A 2 O1W O 0.98746(18) 0.75901(17) 0.43603(11) 0.0256(3) Uani 1 1 d D . . H1W1 H 0.997(3) 0.804(3) 0.3926(15) 0.038 Uiso 1 1 d D . . H1W2 H 1.018(3) 0.819(3) 0.4795(15) 0.038 Uiso 1 1 d D . . O2W O 1.4170(2) 1.1563(2) 0.49584(11) 0.0319(4) Uani 1 1 d D . . H2W1 H 1.483(3) 1.153(4) 0.473(2) 0.048 Uiso 1 1 d D . . H2W2 H 1.399(4) 1.089(3) 0.5288(19) 0.048 Uiso 1 1 d D . . O3W O 1.0793(2) 0.9440(2) 0.58412(13) 0.0366(4) Uani 1 1 d D . . H3W1 H 0.992(3) 0.913(4) 0.598(2) 0.055 Uiso 1 1 d D . . H3W2 H 1.130(4) 0.917(4) 0.6232(18) 0.055 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd 0.01257(6) 0.01261(5) 0.01190(5) 0.00146(3) 0.00298(3) 0.00628(4) O1 0.0153(7) 0.0170(7) 0.0190(7) 0.0027(5) 0.0021(5) 0.0073(6) O2 0.0193(7) 0.0170(7) 0.0186(7) 0.0031(5) 0.0069(5) 0.0093(6) O3 0.0152(7) 0.0170(6) 0.0150(6) 0.0017(5) 0.0042(5) 0.0055(5) O4 0.0192(7) 0.0173(7) 0.0154(6) 0.0019(5) 0.0039(5) 0.0099(6) O5 0.0184(7) 0.0178(7) 0.0191(7) 0.0027(6) 0.0025(5) 0.0083(6) N1 0.0181(8) 0.0170(8) 0.0151(8) 0.0031(6) 0.0040(6) 0.0104(7) N2 0.0165(8) 0.0153(7) 0.0151(7) 0.0024(6) 0.0051(6) 0.0074(6) N3 0.0182(8) 0.0145(7) 0.0136(7) 0.0019(6) 0.0043(6) 0.0087(6) N4 0.0156(8) 0.0168(8) 0.0144(7) 0.0013(6) 0.0026(6) 0.0085(7) N11 0.0165(8) 0.0213(9) 0.0281(9) 0.0003(7) 0.0002(7) 0.0074(7) N21 0.0214(9) 0.0179(8) 0.0255(9) 0.0014(7) 0.0097(7) 0.0093(7) N31 0.0158(8) 0.0223(8) 0.0158(8) 0.0009(7) 0.0050(6) 0.0069(7) N41 0.0258(10) 0.0252(9) 0.0222(9) -0.0034(7) 0.0002(7) 0.0166(8) C1 0.0210(10) 0.0206(10) 0.0196(9) 0.0044(8) 0.0037(8) 0.0140(8) C2 0.0216(10) 0.0177(9) 0.0206(9) 0.0060(8) 0.0054(8) 0.0117(8) C3 0.0177(9) 0.0126(8) 0.0217(9) 0.0024(7) 0.0058(7) 0.0061(7) C4 0.0186(9) 0.0152(9) 0.0206(9) 0.0054(7) 0.0076(7) 0.0079(8) C5 0.0179(9) 0.0188(9) 0.0142(8) 0.0022(7) 0.0066(7) 0.0081(8) C6 0.0190(10) 0.0209(9) 0.0141(9) 0.0038(7) 0.0058(7) 0.0087(8) C7 0.0191(10) 0.0240(10) 0.0118(8) -0.0001(7) 0.0011(7) 0.0107(8) C8 0.0218(10) 0.0259(10) 0.0133(9) 0.0041(8) 0.0025(7) 0.0139(8) C10 0.0153(9) 0.0220(10) 0.0194(9) 0.0021(8) 0.0022(7) 0.0098(8) C11 0.0171(9) 0.0213(9) 0.0138(8) 0.0006(7) 0.0044(7) 0.0090(8) C20 0.0201(10) 0.0161(9) 0.0204(9) 0.0004(7) 0.0068(8) 0.0091(8) C21 0.0179(9) 0.0199(9) 0.0137(8) 0.0011(7) 0.0018(7) 0.0102(8) C30 0.0139(9) 0.0175(9) 0.0151(9) 0.0015(7) 0.0038(7) 0.0068(7) C31 0.0167(9) 0.0144(8) 0.0169(9) 0.0021(7) 0.0038(7) 0.0083(7) C40 0.0214(10) 0.0183(9) 0.0160(9) -0.0017(7) 0.0024(7) 0.0114(8) C41 0.0145(9) 0.0144(9) 0.0198(9) 0.0005(7) 0.0042(7) 0.0049(7) N10 0.0203(8) 0.0201(8) 0.0148(8) 0.0036(6) 0.0046(6) 0.0096(7) O11 0.0398(10) 0.0296(8) 0.0306(8) -0.0074(7) -0.0090(7) 0.0255(8) O12 0.0293(8) 0.0189(7) 0.0317(8) -0.0014(6) 0.0001(7) 0.0102(7) O13 0.0187(7) 0.0287(8) 0.0221(7) 0.0067(6) -0.0001(6) 0.0103(6) N20 0.0256(10) 0.0288(10) 0.0278(10) 0.0031(8) 0.0009(8) 0.0146(8) O21 0.0373(11) 0.1038(19) 0.0300(10) 0.0028(11) 0.0092(8) 0.0399(12) O22 0.0386(11) 0.0271(9) 0.0760(15) 0.0165(10) -0.0043(10) 0.0064(9) O23 0.0504(12) 0.0375(10) 0.0368(10) -0.0074(8) 0.0030(9) 0.0183(9) N30 0.0224(9) 0.0205(9) 0.0393(12) 0.0113(8) 0.0084(8) 0.0117(8) O31A 0.0156(10) 0.0249(11) 0.0573(16) 0.0135(11) 0.0132(10) 0.0075(9) O32A 0.0315(13) 0.0246(11) 0.0190(10) 0.0063(8) 0.0109(9) 0.0168(10) O33A 0.0348(14) 0.0222(12) 0.0211(11) 0.0034(9) 0.0030(11) 0.0155(11) O1W 0.0238(8) 0.0217(8) 0.0302(8) 0.0036(6) 0.0076(7) 0.0085(6) O2W 0.0361(10) 0.0378(10) 0.0264(8) 0.0065(7) 0.0037(7) 0.0213(8) O3W 0.0331(10) 0.0392(10) 0.0412(10) 0.0065(8) 0.0131(8) 0.0176(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O2 2.3665(14) . ? Gd O1 2.3694(14) . ? Gd O3 2.3739(13) . ? Gd O4 2.3791(13) . ? Gd O5 2.4664(14) . ? Gd N4 2.6148(16) . ? Gd N3 2.6387(17) . ? Gd N2 2.6535(16) . ? Gd N1 2.6700(16) . ? O1 C11 1.255(2) . ? O2 C21 1.258(2) . ? O3 C31 1.263(2) . ? O4 C41 1.252(2) . ? O5 H5A 0.8200 . ? O5 H5BB 0.84(3) . ? N1 C10 1.479(3) . ? N1 C1 1.489(2) . ? N1 C8 1.497(2) . ? N2 C20 1.482(2) . ? N2 C3 1.487(3) . ? N2 C2 1.492(2) . ? N3 C30 1.484(2) . ? N3 C4 1.493(2) . ? N3 C5 1.494(2) . ? N4 C40 1.484(2) . ? N4 C7 1.490(2) . ? N4 C6 1.497(3) . ? N11 C11 1.314(3) . ? N11 H11A 0.8600 . ? N11 H11B 0.8600 . ? N21 C21 1.310(3) . ? N21 H21A 0.8600 . ? N21 H21B 0.8600 . ? N31 C31 1.305(3) . ? N31 H31A 0.8600 . ? N31 H31B 0.8600 . ? N41 C41 1.314(3) . ? N41 H41A 0.8600 . ? N41 H41B 0.8600 . ? C1 C2 1.516(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.518(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.524(3) . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.519(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 C11 1.506(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C20 C21 1.513(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C30 C31 1.513(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C40 C41 1.513(3) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? N10 O12 1.245(2) . ? N10 O11 1.252(2) . ? N10 O13 1.260(2) . ? N20 O23 1.232(3) . ? N20 O21 1.237(3) . ? N20 O22 1.248(3) . ? N30 O32B 1.030(11) . ? N30 O33A 1.213(3) . ? N30 O31A 1.261(3) . ? N30 O32A 1.283(3) . ? N30 O33B 1.345(7) . ? N30 O31B 1.394(9) . ? O1W H1W1 0.844(18) . ? O1W H1W2 0.839(18) . ? O2W H2W1 0.836(18) . ? O2W H2W2 0.860(18) . ? O3W H3W1 0.870(18) . ? O3W H3W2 0.875(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd O1 83.83(5) . . ? O2 Gd O3 83.18(5) . . ? O1 Gd O3 142.66(5) . . ? O2 Gd O4 144.66(5) . . ? O1 Gd O4 88.18(5) . . ? O3 Gd O4 82.61(5) . . ? O2 Gd O5 73.64(5) . . ? O1 Gd O5 68.13(5) . . ? O3 Gd O5 74.64(5) . . ? O4 Gd O5 71.44(5) . . ? O2 Gd N4 141.81(5) . . ? O1 Gd N4 74.07(5) . . ? O3 Gd N4 132.31(5) . . ? O4 Gd N4 66.39(5) . . ? O5 Gd N4 123.13(5) . . ? O2 Gd N3 130.48(5) . . ? O1 Gd N3 142.81(5) . . ? O3 Gd N3 66.60(5) . . ? O4 Gd N3 71.15(5) . . ? O5 Gd N3 128.50(5) . . ? N4 Gd N3 69.41(5) . . ? O2 Gd N2 66.33(5) . . ? O1 Gd N2 129.99(5) . . ? O3 Gd N2 74.68(5) . . ? O4 Gd N2 138.70(5) . . ? O5 Gd N2 131.61(5) . . ? N4 Gd N2 105.20(5) . . ? N3 Gd N2 68.28(5) . . ? O2 Gd N1 74.36(5) . . ? O1 Gd N1 65.72(5) . . ? O3 Gd N1 141.65(5) . . ? O4 Gd N1 132.32(5) . . ? O5 Gd N1 125.63(5) . . ? N4 Gd N1 68.29(5) . . ? N3 Gd N1 105.71(5) . . ? N2 Gd N1 67.97(5) . . ? C11 O1 Gd 123.89(13) . . ? C21 O2 Gd 125.00(13) . . ? C31 O3 Gd 123.18(12) . . ? C41 O4 Gd 123.29(12) . . ? Gd O5 H5A 109.5 . . ? Gd O5 H5BB 109(2) . . ? H5A O5 H5BB 96.4 . . ? C10 N1 C1 109.39(15) . . ? C10 N1 C8 110.22(15) . . ? C1 N1 C8 108.38(15) . . ? C10 N1 Gd 105.66(11) . . ? C1 N1 Gd 111.53(11) . . ? C8 N1 Gd 111.64(11) . . ? C20 N2 C3 109.17(15) . . ? C20 N2 C2 110.03(15) . . ? C3 N2 C2 108.39(15) . . ? C20 N2 Gd 108.49(11) . . ? C3 N2 Gd 110.77(11) . . ? C2 N2 Gd 109.98(11) . . ? C30 N3 C4 109.41(15) . . ? C30 N3 C5 109.50(15) . . ? C4 N3 C5 108.85(15) . . ? C30 N3 Gd 106.05(11) . . ? C4 N3 Gd 112.18(11) . . ? C5 N3 Gd 110.80(11) . . ? C40 N4 C7 108.30(15) . . ? C40 N4 C6 110.11(15) . . ? C7 N4 C6 108.74(15) . . ? C40 N4 Gd 107.38(11) . . ? C7 N4 Gd 112.24(11) . . ? C6 N4 Gd 110.05(11) . . ? C11 N11 H11A 120.0 . . ? C11 N11 H11B 120.0 . . ? H11A N11 H11B 120.0 . . ? C21 N21 H21A 120.0 . . ? C21 N21 H21B 120.0 . . ? H21A N21 H21B 120.0 . . ? C31 N31 H31A 120.0 . . ? C31 N31 H31B 120.0 . . ? H31A N31 H31B 120.0 . . ? C41 N41 H41A 120.0 . . ? C41 N41 H41B 120.0 . . ? H41A N41 H41B 120.0 . . ? N1 C1 C2 111.02(16) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 112.50(16) . . ? N2 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? N2 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N2 C3 C4 111.86(16) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C3 113.50(16) . . ? N3 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? N3 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? N3 C5 C6 111.05(16) . . ? N3 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? N3 C5 H5C 109.4 . . ? C6 C5 H5C 109.4 . . ? H5B C5 H5C 108.0 . . ? N4 C6 C5 113.45(16) . . ? N4 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? N4 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N4 C7 C8 112.27(16) . . ? N4 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N4 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N1 C8 C7 113.43(16) . . ? N1 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? N1 C10 C11 110.59(16) . . ? N1 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? O1 C11 N11 121.84(19) . . ? O1 C11 C10 119.56(18) . . ? N11 C11 C10 118.57(18) . . ? N2 C20 C21 110.72(16) . . ? N2 C20 H20A 109.5 . . ? C21 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? O2 C21 N21 122.23(19) . . ? O2 C21 C20 119.06(17) . . ? N21 C21 C20 118.67(18) . . ? N3 C30 C31 110.04(15) . . ? N3 C30 H30A 109.7 . . ? C31 C30 H30A 109.7 . . ? N3 C30 H30B 109.7 . . ? C31 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? O3 C31 N31 122.64(18) . . ? O3 C31 C30 118.79(17) . . ? N31 C31 C30 118.57(18) . . ? N4 C40 C41 110.95(15) . . ? N4 C40 H40A 109.4 . . ? C41 C40 H40A 109.4 . . ? N4 C40 H40B 109.4 . . ? C41 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? O4 C41 N41 122.64(19) . . ? O4 C41 C40 119.50(17) . . ? N41 C41 C40 117.86(17) . . ? O12 N10 O11 120.75(17) . . ? O12 N10 O13 120.15(17) . . ? O11 N10 O13 119.09(17) . . ? O23 N20 O21 119.9(2) . . ? O23 N20 O22 119.7(2) . . ? O21 N20 O22 120.4(2) . . ? O32B N30 O33A 155.6(7) . . ? O32B N30 O31A 80.5(7) . . ? O33A N30 O31A 122.8(3) . . ? O32B N30 O32A 35.5(6) . . ? O33A N30 O32A 121.1(2) . . ? O31A N30 O32A 115.9(2) . . ? O32B N30 O33B 130.7(8) . . ? O33A N30 O33B 26.9(3) . . ? O31A N30 O33B 148.8(4) . . ? O32A N30 O33B 95.2(4) . . ? O32B N30 O31B 126.0(8) . . ? O33A N30 O31B 78.3(4) . . ? O31A N30 O31B 46.4(4) . . ? O32A N30 O31B 159.0(4) . . ? O33B N30 O31B 102.6(5) . . ? H1W1 O1W H1W2 109(3) . . ? H2W1 O2W H2W2 103(3) . . ? H3W1 O3W H3W2 104(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.125 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.076