Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'Barbara Sieklucka' _publ_contact_author_address ; Faculty of Chemistry Jagiellonian University Ingardena 3 Krakow 30-060 POLAND ; _publ_contact_author_email SIEKLUCK@CHEMIA.UJ.EDU.PL _publ_section_title ; [Ln(terpy)]3+ (Ln=Sm, Gd) Entity Forms Isolated Magnetic Chain with [W(CN)8]3- ; loop_ _publ_author_name 'Barbara Sieklucka' 'Maria Balanda' 'Krzysztof Lewinski' 'Robert Pelka' 'Pawel Przychodzen' ; K.Tomala ; data_pp22 _database_code_depnum_ccdc_archive 'CCDC 271198' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '((C N)8 W), ((C15 H11 N3)(C3 H7 N O)4 Sm), (C2 H6 O), (H2 O)6' _chemical_formula_sum 'C37 H57 N15 O11 Sm W' _chemical_formula_weight 1222.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.50900(10) _cell_length_b 23.6780(3) _cell_length_c 14.74700(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.8760(7) _cell_angle_gamma 90.00 _cell_volume 5065.65(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10440 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 45.294 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 3.483 _exptl_absorpt_correction_type 'multi-scan (DENZO-SMN; Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.3032 _exptl_absorpt_correction_T_max 0.5729 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans with the \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19058 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11288 _reflns_number_gt 9152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1997-2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0351P)^2^+8.3870P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00088(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11288 _refine_ls_number_parameters 580 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.036 _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 W1 W 0.408165(11) 0.770904(7) 0.338008(10) 0.02531(6) Uani 1 1 d . . . C1 C 0.4743(3) 0.80639(18) 0.4579(3) 0.0321(9) Uani 1 1 d . . . N1 N 0.5097(3) 0.82325(16) 0.5223(2) 0.0380(9) Uani 1 1 d . . . C2 C 0.3028(3) 0.8220(2) 0.4006(3) 0.0399(10) Uani 1 1 d . . . N2 N 0.2463(3) 0.8484(2) 0.4334(3) 0.0608(13) Uani 1 1 d . . . C3 C 0.3540(3) 0.7193(2) 0.4466(3) 0.0408(11) Uani 1 1 d . . . N3 N 0.3257(3) 0.6933(2) 0.5049(3) 0.0604(13) Uani 1 1 d . . . C4 C 0.3673(3) 0.8360(2) 0.2421(3) 0.0417(11) Uani 1 1 d . . . N4 N 0.3450(4) 0.8696(2) 0.1911(3) 0.0647(14) Uani 1 1 d . . . C5 C 0.2820(3) 0.73471(19) 0.2853(3) 0.0330(9) Uani 1 1 d . . . N5 N 0.2171(3) 0.71417(18) 0.2556(3) 0.0406(9) Uani 1 1 d . . . C6 C 0.4369(3) 0.72984(19) 0.2106(3) 0.0345(10) Uani 1 1 d . . . N6 N 0.4496(3) 0.7065(2) 0.1438(3) 0.0549(12) Uani 1 1 d . . . C7 C 0.5098(4) 0.7063(2) 0.3683(3) 0.0419(11) Uani 1 1 d . . . N7 N 0.5627(4) 0.6723(2) 0.3849(3) 0.0657(14) Uani 1 1 d . . . C8 C 0.5352(3) 0.8102(2) 0.2945(3) 0.0366(10) Uani 1 1 d . . . N8 N 0.6016(3) 0.8300(2) 0.2698(3) 0.0569(12) Uani 1 1 d . . . Sm Sm 0.591211(13) 0.845454(9) 0.676702(13) 0.02562(7) Uani 1 1 d . . . N11 N 0.5540(3) 0.83857(17) 0.8482(2) 0.0385(9) Uani 1 1 d . . . N12 N 0.5368(3) 0.93737(15) 0.7566(2) 0.0350(8) Uani 1 1 d . . . N13 N 0.5903(3) 0.93696(16) 0.5804(3) 0.0369(8) Uani 1 1 d . . . C11 C 0.5705(4) 0.7910(3) 0.8947(4) 0.0520(13) Uani 1 1 d . . . H11 H 0.5959 0.7605 0.8642 0.062 Uiso 1 1 calc R . . C12 C 0.5518(4) 0.7851(3) 0.9851(4) 0.0647(17) Uani 1 1 d . . . H12 H 0.5646 0.7514 1.0152 0.078 Uiso 1 1 calc R . . C13 C 0.5140(5) 0.8299(3) 1.0299(4) 0.081(2) Uani 1 1 d . . . H13 H 0.5010 0.8273 1.0914 0.097 Uiso 1 1 calc R . . C14 C 0.4956(5) 0.8784(3) 0.9830(4) 0.0663(17) Uani 1 1 d . . . H14 H 0.4697 0.9092 1.0124 0.080 Uiso 1 1 calc R . . C15 C 0.5153(3) 0.8819(2) 0.8920(3) 0.0431(11) Uani 1 1 d . . . C16 C 0.4987(3) 0.9341(2) 0.8392(3) 0.0418(11) Uani 1 1 d . . . C17 C 0.4460(5) 0.9788(3) 0.8725(4) 0.0632(16) Uani 1 1 d . . . H17 H 0.4182 0.9758 0.9287 0.076 Uiso 1 1 calc R . . C18 C 0.4355(5) 1.0271(3) 0.8222(5) 0.0723(19) Uani 1 1 d . . . H18 H 0.3992 1.0566 0.8430 0.087 Uiso 1 1 calc R . . C19 C 0.4788(4) 1.0312(2) 0.7414(4) 0.0554(15) Uani 1 1 d . . . H19 H 0.4751 1.0644 0.7079 0.067 Uiso 1 1 calc R . . C20 C 0.5287(3) 0.98541(19) 0.7090(3) 0.0415(11) Uani 1 1 d . . . C21 C 0.5723(3) 0.9867(2) 0.6197(3) 0.0399(11) Uani 1 1 d . . . C22 C 0.5954(5) 1.0373(2) 0.5766(4) 0.0600(16) Uani 1 1 d . . . H22 H 0.5835 1.0715 0.6048 0.072 Uiso 1 1 calc R . . C23 C 0.6351(5) 1.0366(2) 0.4934(4) 0.0654(18) Uani 1 1 d . . . H23 H 0.6497 1.0702 0.4640 0.079 Uiso 1 1 calc R . . C24 C 0.6530(4) 0.9857(2) 0.4540(4) 0.0539(14) Uani 1 1 d . . . H24 H 0.6810 0.9839 0.3978 0.065 Uiso 1 1 calc R . . C25 C 0.6289(4) 0.9370(2) 0.4989(3) 0.0478(12) Uani 1 1 d . . . H25 H 0.6400 0.9025 0.4710 0.057 Uiso 1 1 calc R . . O31 O 0.4247(2) 0.85253(15) 0.6901(2) 0.0451(8) Uani 1 1 d . . . C31 C 0.3571(3) 0.8233(2) 0.6676(3) 0.0414(11) Uani 1 1 d . . . H31 H 0.3685 0.7890 0.6389 0.050 Uiso 1 1 calc R . . N31 N 0.2716(3) 0.83685(19) 0.6811(3) 0.0447(10) Uani 1 1 d . . . C32 C 0.1952(4) 0.8006(3) 0.6526(5) 0.0705(18) Uani 1 1 d . . . H32A H 0.2191 0.7666 0.6261 0.106 Uiso 1 1 calc R . . H32B H 0.1575 0.8201 0.6087 0.106 Uiso 1 1 calc R . . H32C H 0.1589 0.7911 0.7042 0.106 Uiso 1 1 calc R . . C33 C 0.2482(4) 0.8902(3) 0.7221(6) 0.082(2) Uani 1 1 d . . . H33A H 0.3037 0.9103 0.7376 0.123 Uiso 1 1 calc R . . H33B H 0.2134 0.8836 0.7759 0.123 Uiso 1 1 calc R . . H33C H 0.2120 0.9122 0.6800 0.123 Uiso 1 1 calc R . . O41 O 0.5409(3) 0.74893(14) 0.6849(2) 0.0482(9) Uani 1 1 d . . . C41 C 0.5313(4) 0.7059(2) 0.6380(4) 0.0501(13) Uani 1 1 d . . . H41 H 0.5237 0.7110 0.5758 0.060 Uiso 1 1 calc R . . N41 N 0.5308(4) 0.65458(18) 0.6675(3) 0.0586(12) Uani 1 1 d . . . C42 C 0.5434(12) 0.6438(4) 0.7623(6) 0.192(7) Uani 1 1 d . . . H42A H 0.5525 0.6789 0.7938 0.288 Uiso 1 1 calc R . . H42B H 0.5964 0.6201 0.7716 0.288 Uiso 1 1 calc R . . H42C H 0.4898 0.6252 0.7852 0.288 Uiso 1 1 calc R . . C43 C 0.5176(7) 0.6065(3) 0.6072(5) 0.100(3) Uani 1 1 d . . . H43A H 0.5142 0.6195 0.5455 0.150 Uiso 1 1 calc R . . H43B H 0.4614 0.5875 0.6219 0.150 Uiso 1 1 calc R . . H43C H 0.5685 0.5809 0.6143 0.150 Uiso 1 1 calc R . . O51 O 0.7022(2) 0.81710(15) 0.5662(2) 0.0493(8) Uiso 1 1 d D . . C51A C 0.7380(8) 0.8071(5) 0.4934(7) 0.054(3) Uiso 0.493(13) 1 d PD . . N51A N 0.7629(7) 0.7525(4) 0.4690(6) 0.042(3) Uiso 0.493(13) 1 d PD . . C52A C 0.8032(11) 0.7500(8) 0.3763(9) 0.089(5) Uiso 0.493(13) 1 d PD . . C53A C 0.7551(13) 0.7078(7) 0.5296(12) 0.103(6) Uiso 0.493(13) 1 d PD . . C51B C 0.7299(9) 0.7699(5) 0.5379(9) 0.068(4) Uiso 0.507(13) 1 d PD . . N51B N 0.7787(8) 0.7716(5) 0.4594(8) 0.063(3) Uiso 0.507(13) 1 d PD . . C52B C 0.797(2) 0.7076(8) 0.4372(19) 0.181(12) Uiso 0.507(13) 1 d PD . . C53B C 0.799(2) 0.8105(11) 0.3939(18) 0.192(13) Uiso 0.507(13) 1 d PD . . O61 O 0.7238(2) 0.90393(15) 0.7134(3) 0.0511(9) Uani 1 1 d . . . C61 C 0.8065(4) 0.9032(3) 0.7293(5) 0.075(2) Uani 1 1 d . . . H61 H 0.8295 0.8708 0.7572 0.090 Uiso 1 1 calc R . . N61 N 0.8656(4) 0.9421(3) 0.7118(4) 0.0725(15) Uani 1 1 d . . . C62 C 0.9628(6) 0.9396(4) 0.7353(10) 0.160(6) Uani 1 1 d . . . H62A H 0.9919 0.9743 0.7183 0.240 Uiso 1 1 calc R . . H62B H 0.9907 0.9087 0.7036 0.240 Uiso 1 1 calc R . . H62C H 0.9700 0.9340 0.7995 0.240 Uiso 1 1 calc R . . C63 C 0.8392(8) 0.9905(5) 0.6620(10) 0.189(7) Uani 1 1 d . . . H63A H 0.8914 1.0151 0.6558 0.284 Uiso 1 1 calc R . . H63B H 0.7912 1.0100 0.6933 0.284 Uiso 1 1 calc R . . H63C H 0.8171 0.9794 0.6030 0.284 Uiso 1 1 calc R . . O71 O 0.7216(6) 1.0518(2) 0.9427(4) 0.112(2) Uani 1 1 d . . . H71 H 0.7579 1.0523 0.9858 0.168 Uiso 1 1 calc R . . C72 C 0.7223(9) 1.0000(4) 0.9036(6) 0.128(4) Uani 1 1 d . . . H72A H 0.7620 1.0022 0.8513 0.154 Uiso 1 1 calc R . . H72B H 0.6605 0.9926 0.8807 0.154 Uiso 1 1 calc R . . C73 C 0.7511(10) 0.9511(4) 0.9561(7) 0.154(5) Uani 1 1 d . . . H73A H 0.7512 0.9183 0.9178 0.232 Uiso 1 1 calc R . . H73B H 0.7091 0.9453 1.0049 0.232 Uiso 1 1 calc R . . H73C H 0.8120 0.9573 0.9804 0.232 Uiso 1 1 calc R . . O1 O 0.7627(4) 0.8679(2) 0.1683(4) 0.111(2) Uani 1 1 d . . . O2 O 0.8532(5) 1.0566(3) 0.0907(4) 0.112(2) Uani 1 1 d . . . O3 O 0.8822(6) 0.9685(3) 0.4110(5) 0.150(3) Uani 1 1 d . . . O4 O 0.8262(6) 0.9724(2) 0.2299(4) 0.119(2) Uani 1 1 d . . . O5 O 0.1123(6) 0.9240(3) 0.5127(6) 0.152(3) Uani 1 1 d . . . O6 O 0.4565(7) 0.6299(4) -0.0149(5) 0.174(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02564(9) 0.02837(9) 0.02185(9) -0.00058(6) -0.00187(6) -0.00382(6) C1 0.032(2) 0.033(2) 0.031(2) -0.0008(17) -0.0028(18) -0.0037(18) N1 0.039(2) 0.043(2) 0.0327(19) -0.0028(16) -0.0051(17) -0.0061(17) C2 0.042(3) 0.043(3) 0.034(2) -0.002(2) -0.006(2) -0.001(2) N2 0.051(3) 0.065(3) 0.067(3) -0.016(3) 0.009(2) 0.014(2) C3 0.043(3) 0.042(3) 0.038(2) 0.006(2) -0.002(2) -0.011(2) N3 0.060(3) 0.068(3) 0.053(3) 0.022(2) 0.008(2) -0.010(3) C4 0.041(3) 0.046(3) 0.038(2) 0.007(2) 0.001(2) 0.002(2) N4 0.069(3) 0.069(3) 0.056(3) 0.026(3) -0.001(2) 0.013(3) C5 0.030(2) 0.040(2) 0.029(2) -0.0061(18) -0.0014(18) -0.0031(18) N5 0.032(2) 0.054(2) 0.035(2) -0.0107(18) -0.0015(17) -0.0064(18) C6 0.033(2) 0.043(3) 0.028(2) -0.0022(18) 0.0027(18) -0.0060(19) N6 0.058(3) 0.069(3) 0.038(2) -0.013(2) 0.006(2) -0.008(2) C7 0.052(3) 0.043(3) 0.031(2) 0.0029(19) 0.000(2) 0.006(2) N7 0.069(3) 0.068(3) 0.059(3) 0.012(3) -0.001(3) 0.027(3) C8 0.033(2) 0.041(2) 0.036(2) 0.0011(19) 0.0027(19) -0.004(2) N8 0.049(3) 0.058(3) 0.064(3) 0.002(2) 0.015(2) -0.012(2) Sm 0.02508(11) 0.02802(11) 0.02364(11) 0.00022(7) -0.00326(8) 0.00036(8) N11 0.037(2) 0.046(2) 0.0320(19) 0.0061(16) 0.0025(16) 0.0031(17) N12 0.035(2) 0.0327(19) 0.0367(19) -0.0060(15) -0.0040(16) -0.0003(16) N13 0.039(2) 0.034(2) 0.038(2) 0.0037(16) -0.0073(17) -0.0027(17) C11 0.054(3) 0.061(3) 0.042(3) 0.014(2) 0.011(2) 0.009(3) C12 0.061(4) 0.090(5) 0.043(3) 0.026(3) 0.006(3) 0.010(3) C13 0.102(6) 0.105(6) 0.036(3) 0.008(3) 0.019(3) 0.002(5) C14 0.084(4) 0.080(4) 0.035(3) -0.009(3) 0.012(3) 0.001(4) C15 0.046(3) 0.055(3) 0.029(2) -0.005(2) 0.003(2) -0.001(2) C16 0.041(3) 0.045(3) 0.039(2) -0.013(2) -0.002(2) 0.001(2) C17 0.076(4) 0.065(4) 0.050(3) -0.021(3) 0.005(3) 0.013(3) C18 0.085(5) 0.055(4) 0.077(5) -0.025(3) -0.010(4) 0.029(3) C19 0.070(4) 0.034(3) 0.062(4) -0.008(2) -0.014(3) 0.012(2) C20 0.047(3) 0.032(2) 0.046(3) -0.007(2) -0.014(2) 0.002(2) C21 0.038(2) 0.036(2) 0.045(3) 0.005(2) -0.015(2) -0.0035(19) C22 0.082(4) 0.034(3) 0.063(4) 0.011(2) -0.016(3) -0.007(3) C23 0.078(4) 0.050(3) 0.067(4) 0.026(3) -0.017(3) -0.020(3) C24 0.059(3) 0.059(3) 0.043(3) 0.019(3) -0.001(3) -0.013(3) C25 0.057(3) 0.052(3) 0.035(2) 0.009(2) 0.001(2) -0.002(3) O31 0.0306(17) 0.055(2) 0.049(2) -0.0093(16) -0.0022(15) -0.0057(15) C31 0.035(2) 0.046(3) 0.043(3) -0.002(2) -0.001(2) 0.003(2) N31 0.030(2) 0.059(3) 0.046(2) 0.000(2) 0.0038(17) -0.0060(19) C32 0.041(3) 0.086(5) 0.085(5) 0.004(4) -0.002(3) -0.025(3) C33 0.049(3) 0.080(5) 0.117(6) -0.028(4) 0.019(4) 0.004(3) O41 0.059(2) 0.0334(17) 0.052(2) 0.0036(15) -0.0117(18) -0.0104(16) C41 0.052(3) 0.046(3) 0.053(3) 0.010(2) -0.011(3) -0.003(2) N41 0.082(4) 0.035(2) 0.059(3) 0.008(2) 0.003(3) -0.001(2) C42 0.43(2) 0.062(5) 0.080(6) 0.031(5) -0.031(10) -0.029(9) C43 0.159(8) 0.047(4) 0.093(6) -0.016(4) 0.021(6) -0.001(5) O61 0.0337(18) 0.054(2) 0.065(2) -0.0071(18) -0.0110(16) -0.0067(15) C61 0.046(3) 0.047(3) 0.132(6) -0.026(4) -0.007(4) -0.006(3) N61 0.052(3) 0.073(4) 0.093(4) -0.009(3) -0.002(3) -0.023(3) C62 0.052(5) 0.107(8) 0.321(18) -0.018(10) -0.023(7) -0.020(5) C63 0.134(9) 0.188(12) 0.243(15) 0.143(12) -0.089(10) -0.089(9) O71 0.173(7) 0.075(4) 0.088(4) 0.000(3) -0.038(4) 0.018(4) C72 0.188(11) 0.106(8) 0.089(6) -0.025(6) -0.038(7) -0.004(7) C73 0.261(16) 0.088(7) 0.114(8) 0.024(6) -0.025(9) 0.018(9) O1 0.126(5) 0.097(4) 0.111(4) -0.049(3) 0.068(4) -0.053(4) O2 0.159(6) 0.090(4) 0.088(4) -0.002(3) -0.010(4) -0.039(4) O3 0.182(8) 0.149(7) 0.119(6) -0.010(5) -0.007(5) 0.037(5) O4 0.177(7) 0.085(4) 0.093(4) -0.016(3) -0.019(4) -0.018(4) O5 0.164(7) 0.118(6) 0.176(7) -0.011(5) 0.070(6) 0.031(5) O6 0.233(10) 0.168(8) 0.121(6) -0.055(5) 0.025(6) -0.020(7) _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 W1 C5 2.156(4) . ? W1 C6 2.162(4) . ? W1 C7 2.166(5) . ? W1 C4 2.168(5) . ? W1 C2 2.168(5) . ? W1 C8 2.170(5) . ? W1 C1 2.169(4) . ? W1 C3 2.172(5) . ? C1 N1 1.144(5) . ? N1 Sm 2.603(4) . ? C2 N2 1.143(6) . ? C3 N3 1.138(6) . ? C4 N4 1.138(6) . ? C5 N5 1.140(6) . ? N5 Sm 2.573(4) 4_575 ? C6 N6 1.147(6) . ? C7 N7 1.137(6) . ? C8 N8 1.137(6) . ? Sm O41 2.403(3) . ? Sm O51 2.404(4) . ? Sm O61 2.424(3) . ? Sm O31 2.433(3) . ? Sm N5 2.573(4) 4_676 ? Sm N13 2.591(4) . ? Sm N11 2.600(4) . ? Sm N12 2.603(4) . ? N11 C11 1.337(6) . ? N11 C15 1.341(6) . ? N12 C20 1.341(6) . ? N12 C16 1.348(6) . ? N13 C25 1.334(6) . ? N13 C21 1.339(6) . ? C11 C12 1.372(7) . ? C11 H11 0.9300 . ? C12 C13 1.369(10) . ? C12 H12 0.9300 . ? C13 C14 1.367(9) . ? C13 H13 0.9300 . ? C14 C15 1.378(7) . ? C14 H14 0.9300 . ? C15 C16 1.478(7) . ? C16 C17 1.399(7) . ? C17 C18 1.370(9) . ? C17 H17 0.9300 . ? C18 C19 1.359(9) . ? C18 H18 0.9300 . ? C19 C20 1.392(7) . ? C19 H19 0.9300 . ? C20 C21 1.471(7) . ? C21 C22 1.399(7) . ? C22 C23 1.364(9) . ? C22 H22 0.9300 . ? C23 C24 1.365(9) . ? C23 H23 0.9300 . ? C24 C25 1.377(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? O31 C31 1.242(6) . ? C31 N31 1.299(6) . ? C31 H31 0.9300 . ? N31 C33 1.444(8) . ? N31 C32 1.459(7) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? O41 C41 1.237(6) . ? C41 N41 1.291(7) . ? C41 H41 0.9300 . ? N41 C42 1.431(9) . ? N41 C43 1.455(8) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? O51 C51A 1.223(10) . ? O51 C51B 1.260(11) . ? C51A N51A 1.392(12) . ? N51A C53A 1.392(14) . ? N51A C52A 1.496(13) . ? C51B N51B 1.368(14) . ? N51B C53B 1.371(17) . ? N51B C52B 1.573(16) . ? O61 C61 1.220(7) . ? C61 N61 1.288(8) . ? C61 H61 0.9300 . ? N61 C63 1.410(11) . ? N61 C62 1.447(9) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? O71 C72 1.355(10) . ? O71 H71 0.8200 . ? C72 C73 1.452(13) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 W1 C6 71.45(16) . . ? C5 W1 C7 111.43(18) . . ? C6 W1 C7 73.83(17) . . ? C5 W1 C4 79.93(18) . . ? C6 W1 C4 78.92(18) . . ? C7 W1 C4 144.57(18) . . ? C5 W1 C2 76.98(17) . . ? C6 W1 C2 140.19(17) . . ? C7 W1 C2 142.07(17) . . ? C4 W1 C2 72.14(18) . . ? C5 W1 C8 141.65(16) . . ? C6 W1 C8 76.12(17) . . ? C7 W1 C8 77.60(19) . . ? C4 W1 C8 74.18(18) . . ? C2 W1 C8 119.63(18) . . ? C5 W1 C1 144.20(16) . . ? C6 W1 C1 142.56(17) . . ? C7 W1 C1 79.29(17) . . ? C4 W1 C1 111.67(17) . . ? C2 W1 C1 75.09(16) . . ? C8 W1 C1 72.98(16) . . ? C5 W1 C3 74.16(17) . . ? C6 W1 C3 117.68(18) . . ? C7 W1 C3 72.76(19) . . ? C4 W1 C3 141.49(19) . . ? C2 W1 C3 74.58(19) . . ? C8 W1 C3 141.08(17) . . ? C1 W1 C3 77.15(17) . . ? N1 C1 W1 177.6(4) . . ? C1 N1 Sm 171.2(4) . . ? N2 C2 W1 179.1(5) . . ? N3 C3 W1 178.4(5) . . ? N4 C4 W1 178.9(5) . . ? N5 C5 W1 177.4(4) . . ? C5 N5 Sm 169.6(4) . 4_575 ? N6 C6 W1 177.3(4) . . ? N7 C7 W1 179.3(5) . . ? N8 C8 W1 178.3(5) . . ? O41 Sm O51 88.60(13) . . ? O41 Sm O61 140.60(12) . . ? O51 Sm O61 76.94(12) . . ? O41 Sm O31 76.03(12) . . ? O51 Sm O31 138.64(12) . . ? O61 Sm O31 136.70(12) . . ? O41 Sm N5 70.71(13) . 4_676 ? O51 Sm N5 71.04(12) . 4_676 ? O61 Sm N5 69.94(13) . 4_676 ? O31 Sm N5 134.45(12) . 4_676 ? O41 Sm N13 145.48(11) . . ? O51 Sm N13 81.94(12) . . ? O61 Sm N13 69.04(12) . . ? O31 Sm N13 89.44(12) . . ? N5 Sm N13 134.79(12) 4_676 . ? O41 Sm N11 79.85(12) . . ? O51 Sm N11 142.51(12) . . ? O61 Sm N11 89.66(13) . . ? O31 Sm N11 72.77(12) . . ? N5 Sm N11 71.48(12) 4_676 . ? N13 Sm N11 125.90(12) . . ? O41 Sm N1 73.58(12) . . ? O51 Sm N1 69.55(12) . . ? O61 Sm N1 131.23(12) . . ? O31 Sm N1 69.30(12) . . ? N5 Sm N1 126.49(13) 4_676 . ? N13 Sm N1 72.00(12) . . ? N11 Sm N1 137.73(12) . . ? O41 Sm N12 132.69(13) . . ? O51 Sm N12 138.70(12) . . ? O61 Sm N12 70.51(12) . . ? O31 Sm N12 66.24(11) . . ? N5 Sm N12 118.19(12) 4_676 . ? N13 Sm N12 63.24(12) . . ? N11 Sm N12 62.81(12) . . ? N1 Sm N12 115.33(12) . . ? C11 N11 C15 118.1(4) . . ? C11 N11 Sm 120.8(3) . . ? C15 N11 Sm 121.0(3) . . ? C20 N12 C16 119.2(4) . . ? C20 N12 Sm 119.8(3) . . ? C16 N12 Sm 119.5(3) . . ? C25 N13 C21 118.5(4) . . ? C25 N13 Sm 119.7(3) . . ? C21 N13 Sm 119.8(3) . . ? N11 C11 C12 123.2(6) . . ? N11 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C13 C12 C11 118.5(6) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C14 C13 C12 118.9(6) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 120.2(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? N11 C15 C14 121.1(5) . . ? N11 C15 C16 116.9(4) . . ? C14 C15 C16 121.9(5) . . ? N12 C16 C17 120.5(5) . . ? N12 C16 C15 117.3(4) . . ? C17 C16 C15 122.2(5) . . ? C18 C17 C16 119.9(6) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 119.0(6) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 119.7(5) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N12 C20 C19 121.6(5) . . ? N12 C20 C21 116.7(4) . . ? C19 C20 C21 121.7(5) . . ? N13 C21 C22 120.4(5) . . ? N13 C21 C20 117.3(4) . . ? C22 C21 C20 122.2(5) . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 118.5(5) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C23 C24 C25 119.0(5) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? N13 C25 C24 123.1(5) . . ? N13 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C31 O31 Sm 136.1(3) . . ? O31 C31 N31 124.9(5) . . ? O31 C31 H31 117.5 . . ? N31 C31 H31 117.5 . . ? C31 N31 C33 120.8(5) . . ? C31 N31 C32 122.2(5) . . ? C33 N31 C32 117.0(5) . . ? N31 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N31 C33 H33A 109.5 . . ? N31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C41 O41 Sm 141.9(4) . . ? O41 C41 N41 126.1(5) . . ? O41 C41 H41 117.0 . . ? N41 C41 H41 117.0 . . ? C41 N41 C42 119.7(6) . . ? C41 N41 C43 122.1(5) . . ? C42 N41 C43 118.2(6) . . ? N41 C42 H42A 109.5 . . ? N41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N41 C43 H43A 109.5 . . ? N41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C51A O51 C51B 52.9(7) . . ? C51A O51 Sm 161.3(6) . . ? C51B O51 Sm 133.8(6) . . ? O51 C51A N51A 121.5(10) . . ? C51A N51A C53A 121.1(11) . . ? C51A N51A C52A 112.2(10) . . ? C53A N51A C52A 126.5(12) . . ? O51 C51B N51B 115.3(11) . . ? C51B N51B C53B 137.3(17) . . ? C51B N51B C52B 104.0(14) . . ? C53B N51B C52B 117.6(17) . . ? C61 O61 Sm 144.1(4) . . ? O61 C61 N61 127.4(7) . . ? O61 C61 H61 116.3 . . ? N61 C61 H61 116.3 . . ? C61 N61 C63 120.6(7) . . ? C61 N61 C62 124.8(7) . . ? C63 N61 C62 114.5(7) . . ? N61 C62 H62A 109.5 . . ? N61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N61 C63 H63A 109.5 . . ? N61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C72 O71 H71 109.5 . . ? O71 C72 C73 119.9(8) . . ? O71 C72 H72A 107.3 . . ? C73 C72 H72A 107.3 . . ? O71 C72 H72B 107.3 . . ? C73 C72 H72B 107.3 . . ? H72A C72 H72B 106.9 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.333 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.111 data_pp20 _database_code_depnum_ccdc_archive 'CCDC 271199' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '((C N)8 W), ((C15 H11 N3)(C3 H7 N O)4 Gd), (C2 H6 O), (H2 O)6' _chemical_formula_sum 'C37 H57 Gd N15 O11 W' _chemical_formula_weight 1229.08 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.48200(10) _cell_length_b 23.6880(3) _cell_length_c 14.71300(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.1910(10) _cell_angle_gamma 90.00 _cell_volume 5046.20(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11917 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 44.170 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 3.647 _exptl_absorpt_correction_type 'multi-scan (DENZO-SMN; Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.3617 _exptl_absorpt_correction_T_max 0.7590 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans with the \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19832 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11539 _reflns_number_gt 9570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1997-2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. Hydrogen atoms of water molecules were not observed on Fourier maps and were not used in refinement. Molecule DMF(5) was disordered. Two alternative rigid molecules with complementary occupancy factors were used in refinement. All atoms of this molecule were refined with isotropic displacement parameter, no hydrogen atoms in this molecule were used in refinement. ; _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^)+(0.0262P)^2^+11.4270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00062(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11539 _refine_ls_number_parameters 580 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.042 _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 W1 W 0.407304(11) 0.771031(7) 0.339695(10) 0.02601(6) Uani 1 1 d . . . C1 C 0.4735(3) 0.80629(19) 0.4597(2) 0.0318(9) Uani 1 1 d . . . N1 N 0.5096(3) 0.82342(17) 0.5243(2) 0.0396(9) Uani 1 1 d . . . C2 C 0.3020(3) 0.8222(2) 0.4025(3) 0.0390(10) Uani 1 1 d . . . N2 N 0.2461(3) 0.8485(2) 0.4342(3) 0.0609(13) Uani 1 1 d . . . C3 C 0.3528(3) 0.7197(2) 0.4484(3) 0.0396(10) Uani 1 1 d . . . N3 N 0.3252(3) 0.6941(2) 0.5076(3) 0.0586(12) Uani 1 1 d . . . C4 C 0.3664(3) 0.8357(2) 0.2432(3) 0.0426(11) Uani 1 1 d . . . N4 N 0.3433(4) 0.8692(2) 0.1921(3) 0.0679(14) Uani 1 1 d . . . C5 C 0.2818(3) 0.73423(19) 0.2864(3) 0.0331(9) Uani 1 1 d . . . N5 N 0.2171(3) 0.71314(18) 0.2565(2) 0.0409(9) Uani 1 1 d . . . C6 C 0.4362(3) 0.7303(2) 0.2117(3) 0.0366(10) Uani 1 1 d . . . N6 N 0.4495(3) 0.7074(2) 0.1447(3) 0.0540(11) Uani 1 1 d . . . C7 C 0.5095(4) 0.7063(2) 0.3703(3) 0.0452(11) Uani 1 1 d . . . N7 N 0.5623(4) 0.6717(2) 0.3863(3) 0.0688(14) Uani 1 1 d . . . C8 C 0.5348(3) 0.8100(2) 0.2963(3) 0.0394(10) Uani 1 1 d . . . N8 N 0.6008(3) 0.8304(2) 0.2726(3) 0.0595(12) Uani 1 1 d . . . Gd2 Gd 0.590773(13) 0.846087(8) 0.678456(12) 0.02595(6) Uani 1 1 d . . . N11 N 0.5541(3) 0.83899(17) 0.8489(2) 0.0372(8) Uani 1 1 d . . . N12 N 0.5378(2) 0.93725(16) 0.7572(2) 0.0347(8) Uani 1 1 d . . . N13 N 0.5901(3) 0.93597(16) 0.5811(2) 0.0381(8) Uani 1 1 d . . . C11 C 0.5709(3) 0.7914(2) 0.8956(3) 0.0494(12) Uani 1 1 d . . . H11 H 0.5972 0.7611 0.8652 0.059 Uiso 1 1 calc R . . C12 C 0.5513(4) 0.7848(3) 0.9859(4) 0.0642(16) Uani 1 1 d . . . H12 H 0.5632 0.7510 1.0159 0.077 Uiso 1 1 calc R . . C13 C 0.5136(5) 0.8300(3) 1.0306(4) 0.076(2) Uani 1 1 d . . . H13 H 0.5008 0.8275 1.0922 0.091 Uiso 1 1 calc R . . C14 C 0.4952(5) 0.8785(3) 0.9837(4) 0.0675(17) Uani 1 1 d . . . H14 H 0.4687 0.9091 1.0130 0.081 Uiso 1 1 calc R . . C15 C 0.5158(3) 0.8822(2) 0.8922(3) 0.0415(10) Uani 1 1 d . . . C16 C 0.4989(3) 0.9345(2) 0.8398(3) 0.0417(11) Uani 1 1 d . . . C17 C 0.4477(4) 0.9792(3) 0.8733(4) 0.0611(15) Uani 1 1 d . . . H17 H 0.4202 0.9763 0.9297 0.073 Uiso 1 1 calc R . . C18 C 0.4381(5) 1.0273(3) 0.8232(4) 0.0707(18) Uani 1 1 d . . . H18 H 0.4029 1.0572 0.8445 0.085 Uiso 1 1 calc R . . C19 C 0.4807(4) 1.0313(2) 0.7409(4) 0.0583(15) Uani 1 1 d . . . H19 H 0.4771 1.0644 0.7071 0.070 Uiso 1 1 calc R . . C20 C 0.5293(3) 0.9853(2) 0.7090(3) 0.0427(11) Uani 1 1 d . . . C21 C 0.5735(3) 0.9863(2) 0.6194(3) 0.0417(11) Uani 1 1 d . . . C22 C 0.5957(4) 1.0365(2) 0.5768(4) 0.0574(14) Uani 1 1 d . . . H22 H 0.5836 1.0708 0.6050 0.069 Uiso 1 1 calc R . . C23 C 0.6353(5) 1.0357(3) 0.4935(4) 0.0683(18) Uani 1 1 d . . . H23 H 0.6503 1.0692 0.4644 0.082 Uiso 1 1 calc R . . C24 C 0.6528(4) 0.9849(3) 0.4537(4) 0.0573(14) Uani 1 1 d . . . H24 H 0.6805 0.9832 0.3973 0.069 Uiso 1 1 calc R . . C25 C 0.6284(4) 0.9354(2) 0.4989(3) 0.0489(12) Uani 1 1 d . . . H25 H 0.6391 0.9008 0.4710 0.059 Uiso 1 1 calc R . . O31 O 0.4250(2) 0.85333(15) 0.6916(2) 0.0439(8) Uani 1 1 d . . . C31 C 0.3571(3) 0.8242(2) 0.6692(3) 0.0423(11) Uani 1 1 d . . . H31 H 0.3683 0.7900 0.6404 0.051 Uiso 1 1 calc R . . N31 N 0.2723(3) 0.83757(19) 0.6829(3) 0.0449(9) Uani 1 1 d . . . C32 C 0.1951(4) 0.8016(3) 0.6551(4) 0.0720(18) Uani 1 1 d . . . H32A H 0.2183 0.7675 0.6285 0.108 Uiso 1 1 calc R . . H32B H 0.1569 0.8212 0.6112 0.108 Uiso 1 1 calc R . . H32C H 0.1592 0.7924 0.7072 0.108 Uiso 1 1 calc R . . C33 C 0.2490(5) 0.8913(3) 0.7247(6) 0.089(2) Uani 1 1 d . . . H33A H 0.3047 0.9114 0.7402 0.134 Uiso 1 1 calc R . . H33B H 0.2145 0.8846 0.7787 0.134 Uiso 1 1 calc R . . H33C H 0.2124 0.9133 0.6827 0.134 Uiso 1 1 calc R . . O41 O 0.5411(2) 0.75018(14) 0.6867(2) 0.0472(8) Uani 1 1 d . . . C41 C 0.5315(4) 0.7072(2) 0.6406(3) 0.0486(12) Uani 1 1 d . . . H41 H 0.5240 0.7120 0.5781 0.058 Uiso 1 1 calc R . . N41 N 0.5307(4) 0.65633(18) 0.6709(3) 0.0594(12) Uani 1 1 d . . . C42 C 0.5380(10) 0.6451(4) 0.7663(6) 0.172(6) Uani 1 1 d . . . H42A H 0.5472 0.6799 0.7987 0.258 Uiso 1 1 calc R . . H42B H 0.5894 0.6204 0.7782 0.258 Uiso 1 1 calc R . . H42C H 0.4822 0.6274 0.7860 0.258 Uiso 1 1 calc R . . C43 C 0.5174(7) 0.6083(3) 0.6097(5) 0.103(3) Uani 1 1 d . . . H43A H 0.5141 0.6215 0.5480 0.154 Uiso 1 1 calc R . . H43B H 0.4611 0.5892 0.6239 0.154 Uiso 1 1 calc R . . H43C H 0.5684 0.5827 0.6169 0.154 Uiso 1 1 calc R . . O51 O 0.7009(2) 0.81734(15) 0.5693(2) 0.0477(8) Uiso 1 1 d D . . C51A C 0.7353(8) 0.8060(5) 0.4975(7) 0.050(3) Uiso 0.439(12) 1 d PD . . N51A N 0.7621(7) 0.7533(4) 0.4730(6) 0.038(3) Uiso 0.439(12) 1 d PD . . C52A C 0.8020(11) 0.7513(7) 0.3799(9) 0.072(5) Uiso 0.439(12) 1 d PD . . C53A C 0.7570(14) 0.7074(8) 0.5295(12) 0.096(6) Uiso 0.439(12) 1 d PD . . C51B C 0.7278(8) 0.7708(5) 0.5401(8) 0.073(4) Uiso 0.561(12) 1 d PD . . N51B N 0.7767(7) 0.7730(5) 0.4616(7) 0.063(3) Uiso 0.561(12) 1 d PD . . C52B C 0.7965(18) 0.7097(8) 0.4371(17) 0.176(10) Uiso 0.561(12) 1 d PD . . C53B C 0.806(2) 0.8133(10) 0.4042(18) 0.210(13) Uiso 0.561(12) 1 d PD . . O61 O 0.7224(2) 0.90431(16) 0.7154(2) 0.0509(9) Uani 1 1 d . . . C61 C 0.8056(4) 0.9038(3) 0.7257(6) 0.082(2) Uani 1 1 d . . . H61 H 0.8306 0.8701 0.7473 0.098 Uiso 1 1 calc R . . N61 N 0.8637(4) 0.9431(3) 0.7110(4) 0.0774(16) Uani 1 1 d . . . C62 C 0.9622(6) 0.9397(5) 0.7274(11) 0.180(6) Uani 1 1 d . . . H62A H 0.9905 0.9746 0.7102 0.271 Uiso 1 1 calc R . . H62B H 0.9871 0.9094 0.6922 0.271 Uiso 1 1 calc R . . H62C H 0.9743 0.9328 0.7908 0.271 Uiso 1 1 calc R . . C63 C 0.8353(9) 0.9935(6) 0.6694(12) 0.245(11) Uani 1 1 d . . . H63A H 0.8875 1.0181 0.6632 0.368 Uiso 1 1 calc R . . H63B H 0.7899 1.0116 0.7061 0.368 Uiso 1 1 calc R . . H63C H 0.8089 0.9855 0.6104 0.368 Uiso 1 1 calc R . . O71 O 0.7193(6) 1.0510(3) 0.9452(4) 0.123(2) Uani 1 1 d . . . H71 H 0.7520 1.0509 0.9914 0.184 Uiso 1 1 calc R . . C72 C 0.7232(10) 1.0002(6) 0.9047(8) 0.172(6) Uani 1 1 d . . . H72A H 0.7660 1.0038 0.8553 0.207 Uiso 1 1 calc R . . H72B H 0.6628 0.9935 0.8770 0.207 Uiso 1 1 calc R . . C73 C 0.7492(11) 0.9472(5) 0.9553(8) 0.179(6) Uani 1 1 d . . . H73A H 0.7482 0.9158 0.9141 0.268 Uiso 1 1 calc R . . H73B H 0.7060 0.9407 1.0028 0.268 Uiso 1 1 calc R . . H73C H 0.8102 0.9513 0.9814 0.268 Uiso 1 1 calc R . . O1 O 0.7615(4) 0.8675(3) 0.1692(4) 0.119(2) Uani 1 1 d . . . O2 O 0.8574(5) 1.0557(3) 0.0896(4) 0.122(2) Uani 1 1 d . . . O3 O 0.8838(6) 0.9679(3) 0.4129(5) 0.151(3) Uani 1 1 d . . . O4 O 0.8262(5) 0.9721(3) 0.2305(4) 0.125(2) Uani 1 1 d . . . O5 O 0.1104(6) 0.9251(3) 0.5112(6) 0.158(3) Uani 1 1 d . . . O6 O 0.4575(7) 0.6299(4) -0.0136(6) 0.196(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02585(9) 0.03058(9) 0.02151(8) -0.00073(5) -0.00137(5) -0.00417(6) C1 0.030(2) 0.042(2) 0.0233(19) -0.0015(16) -0.0045(15) -0.0067(18) N1 0.038(2) 0.045(2) 0.035(2) -0.0018(16) -0.0029(15) -0.0068(17) C2 0.039(3) 0.045(3) 0.033(2) -0.0060(18) 0.0010(18) 0.003(2) N2 0.057(3) 0.065(3) 0.061(3) -0.017(2) 0.005(2) 0.014(2) C3 0.039(3) 0.043(3) 0.036(2) 0.0074(19) -0.0011(18) -0.007(2) N3 0.059(3) 0.064(3) 0.054(3) 0.017(2) 0.008(2) -0.005(2) C4 0.048(3) 0.046(3) 0.034(2) 0.0080(19) 0.0005(19) 0.006(2) N4 0.074(3) 0.073(4) 0.057(3) 0.024(2) 0.002(2) 0.013(3) C5 0.032(2) 0.040(2) 0.027(2) -0.0056(16) 0.0005(16) -0.0026(19) N5 0.031(2) 0.057(3) 0.0344(19) -0.0089(17) -0.0011(15) -0.0058(18) C6 0.032(2) 0.047(3) 0.031(2) -0.0030(18) 0.0022(16) -0.004(2) N6 0.054(3) 0.069(3) 0.039(2) -0.013(2) 0.0096(18) -0.005(2) C7 0.053(3) 0.052(3) 0.031(2) 0.0002(19) 0.0036(19) 0.002(2) N7 0.072(3) 0.071(3) 0.064(3) 0.013(2) 0.003(2) 0.034(3) C8 0.034(2) 0.044(3) 0.040(2) -0.0004(19) 0.0012(18) -0.003(2) N8 0.049(3) 0.063(3) 0.066(3) 0.004(2) 0.013(2) -0.015(2) Gd2 0.02492(11) 0.02972(11) 0.02306(10) 0.00035(7) -0.00315(7) 0.00015(8) N11 0.036(2) 0.047(2) 0.0285(18) 0.0037(15) 0.0027(14) 0.0049(17) N12 0.034(2) 0.036(2) 0.0340(18) -0.0040(14) -0.0036(14) -0.0001(16) N13 0.040(2) 0.038(2) 0.0357(19) 0.0063(15) -0.0060(15) -0.0032(17) C11 0.046(3) 0.063(3) 0.039(3) 0.017(2) 0.009(2) 0.010(2) C12 0.063(4) 0.086(4) 0.044(3) 0.026(3) 0.009(3) 0.008(3) C13 0.102(5) 0.097(5) 0.031(3) 0.010(3) 0.019(3) 0.001(4) C14 0.080(4) 0.083(5) 0.040(3) -0.004(3) 0.017(3) 0.004(4) C15 0.038(2) 0.053(3) 0.034(2) -0.0072(19) 0.0011(17) -0.001(2) C16 0.040(3) 0.047(3) 0.037(2) -0.0111(19) -0.0039(18) 0.003(2) C17 0.070(4) 0.063(4) 0.050(3) -0.018(3) 0.005(3) 0.014(3) C18 0.087(5) 0.057(4) 0.068(4) -0.026(3) -0.008(3) 0.028(3) C19 0.075(4) 0.038(3) 0.061(3) -0.012(2) -0.012(3) 0.013(3) C20 0.047(3) 0.033(2) 0.048(3) -0.0055(19) -0.012(2) -0.002(2) C21 0.041(3) 0.038(3) 0.045(3) 0.0002(19) -0.0153(19) -0.003(2) C22 0.072(4) 0.033(3) 0.067(4) 0.012(2) -0.011(3) -0.004(3) C23 0.086(5) 0.055(4) 0.063(4) 0.023(3) -0.011(3) -0.021(3) C24 0.060(3) 0.065(4) 0.047(3) 0.020(3) 0.000(2) -0.013(3) C25 0.053(3) 0.056(3) 0.038(3) 0.009(2) 0.000(2) 0.001(3) O31 0.0286(17) 0.055(2) 0.0484(19) -0.0087(15) -0.0007(13) -0.0041(15) C31 0.034(2) 0.048(3) 0.045(3) -0.006(2) 0.0029(19) -0.003(2) N31 0.029(2) 0.058(3) 0.048(2) -0.0012(18) 0.0039(16) -0.0049(18) C32 0.041(3) 0.093(5) 0.082(4) 0.006(4) -0.001(3) -0.028(3) C33 0.051(4) 0.089(5) 0.128(6) -0.035(5) 0.018(4) 0.007(4) O41 0.055(2) 0.0364(18) 0.0502(19) 0.0048(15) -0.0096(15) -0.0112(16) C41 0.053(3) 0.045(3) 0.047(3) 0.005(2) -0.008(2) 0.001(2) N41 0.085(4) 0.033(2) 0.060(3) 0.0057(19) 0.005(2) 0.000(2) C42 0.38(2) 0.068(6) 0.069(5) 0.024(4) -0.020(8) -0.024(9) C43 0.175(9) 0.044(4) 0.090(5) -0.010(3) 0.025(5) -0.007(5) O61 0.0348(19) 0.055(2) 0.063(2) -0.0054(17) -0.0078(15) -0.0080(16) C61 0.040(3) 0.048(4) 0.158(7) -0.028(4) -0.006(4) -0.007(3) N61 0.049(3) 0.084(4) 0.099(4) -0.015(3) 0.000(3) -0.031(3) C62 0.050(5) 0.112(8) 0.38(2) -0.030(11) 0.004(8) -0.023(5) C63 0.142(11) 0.206(15) 0.38(2) 0.204(16) -0.127(13) -0.098(10) O71 0.195(7) 0.086(4) 0.085(4) -0.005(3) -0.037(4) 0.029(4) C72 0.227(15) 0.182(14) 0.107(8) -0.044(9) -0.033(9) -0.025(12) C73 0.283(18) 0.124(10) 0.129(9) 0.056(8) -0.012(10) 0.034(11) O1 0.133(5) 0.104(4) 0.124(5) -0.052(4) 0.080(4) -0.057(4) O2 0.163(6) 0.107(5) 0.096(4) -0.010(3) -0.002(4) -0.041(4) O3 0.186(8) 0.147(7) 0.120(6) -0.009(5) -0.006(5) 0.023(6) O4 0.178(7) 0.089(4) 0.108(5) -0.022(3) -0.019(4) -0.016(4) O5 0.160(7) 0.121(6) 0.195(7) -0.010(5) 0.081(6) 0.030(5) O6 0.276(12) 0.175(9) 0.137(7) -0.061(6) 0.029(7) -0.022(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 W1 C5 2.149(4) . ? W1 C1 2.159(4) . ? W1 C4 2.162(4) . ? W1 C6 2.165(4) . ? W1 C2 2.170(5) . ? W1 C3 2.171(4) . ? W1 C7 2.171(5) . ? W1 C8 2.172(5) . ? C1 N1 1.150(5) . ? N1 Gd2 2.589(4) . ? C2 N2 1.129(6) . ? C3 N3 1.140(6) . ? C4 N4 1.140(6) . ? C5 N5 1.143(5) . ? N5 Gd2 2.558(4) 4_575 ? C6 N6 1.145(6) . ? C7 N7 1.143(7) . ? C8 N8 1.132(6) . ? Gd2 O51 2.385(3) . ? Gd2 O41 2.387(3) . ? Gd2 O61 2.406(3) . ? Gd2 O31 2.419(3) . ? Gd2 N5 2.558(4) 4_676 ? Gd2 N13 2.566(4) . ? Gd2 N12 2.575(4) . ? Gd2 N11 2.579(3) . ? N11 C15 1.333(6) . ? N11 C11 1.340(6) . ? N12 C20 1.345(6) . ? N12 C16 1.351(6) . ? N13 C25 1.341(6) . ? N13 C21 1.343(6) . ? C11 C12 1.373(7) . ? C11 H11 0.9300 . ? C12 C13 1.375(9) . ? C12 H12 0.9300 . ? C13 C14 1.364(9) . ? C13 H13 0.9300 . ? C14 C15 1.388(7) . ? C14 H14 0.9300 . ? C15 C16 1.477(7) . ? C16 C17 1.389(7) . ? C17 C18 1.364(9) . ? C17 H17 0.9300 . ? C18 C19 1.374(9) . ? C18 H18 0.9300 . ? C19 C20 1.385(7) . ? C19 H19 0.9300 . ? C20 C21 1.478(7) . ? C21 C22 1.386(7) . ? C22 C23 1.364(9) . ? C22 H22 0.9300 . ? C23 C24 1.364(9) . ? C23 H23 0.9300 . ? C24 C25 1.396(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? O31 C31 1.240(5) . ? C31 N31 1.289(6) . ? C31 H31 0.9300 . ? N31 C33 1.456(8) . ? N31 C32 1.457(7) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? O41 C41 1.229(6) . ? C41 N41 1.286(6) . ? C41 H41 0.9300 . ? N41 C42 1.430(9) . ? N41 C43 1.461(8) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? O51 C51A 1.208(10) . ? O51 C51B 1.250(11) . ? C51A N51A 1.359(13) . ? N51A C53A 1.373(15) . ? N51A C52A 1.499(13) . ? C51B N51B 1.368(13) . ? N51B C53B 1.346(17) . ? N51B C52B 1.570(16) . ? O61 C61 1.211(7) . ? C61 N61 1.277(8) . ? C61 H61 0.9300 . ? N61 C63 1.400(12) . ? N61 C62 1.443(10) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? O71 C72 1.345(13) . ? O71 H71 0.8200 . ? C72 C73 1.503(16) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 W1 C1 144.37(15) . . ? C5 W1 C4 80.20(18) . . ? C1 W1 C4 111.93(18) . . ? C5 W1 C6 71.30(16) . . ? C1 W1 C6 142.47(16) . . ? C4 W1 C6 78.45(18) . . ? C5 W1 C2 77.62(16) . . ? C1 W1 C2 74.90(16) . . ? C4 W1 C2 72.45(17) . . ? C6 W1 C2 140.35(17) . . ? C5 W1 C3 73.97(16) . . ? C1 W1 C3 77.09(16) . . ? C4 W1 C3 141.42(18) . . ? C6 W1 C3 118.10(18) . . ? C2 W1 C3 74.35(18) . . ? C5 W1 C7 110.92(18) . . ? C1 W1 C7 79.30(17) . . ? C4 W1 C7 144.31(18) . . ? C6 W1 C7 73.89(17) . . ? C2 W1 C7 142.02(17) . . ? C3 W1 C7 73.03(18) . . ? C5 W1 C8 141.53(16) . . ? C1 W1 C8 73.14(16) . . ? C4 W1 C8 74.26(18) . . ? C6 W1 C8 75.70(17) . . ? C2 W1 C8 119.76(18) . . ? C3 W1 C8 141.16(17) . . ? C7 W1 C8 77.37(19) . . ? N1 C1 W1 177.9(4) . . ? C1 N1 Gd2 171.2(4) . . ? N2 C2 W1 178.8(5) . . ? N3 C3 W1 177.6(5) . . ? N4 C4 W1 178.7(5) . . ? N5 C5 W1 177.4(4) . . ? C5 N5 Gd2 170.4(4) . 4_575 ? N6 C6 W1 177.7(4) . . ? N7 C7 W1 179.0(5) . . ? N8 C8 W1 179.1(4) . . ? O51 Gd2 O41 88.21(12) . . ? O51 Gd2 O61 77.18(12) . . ? O41 Gd2 O61 140.56(12) . . ? O51 Gd2 O31 138.80(11) . . ? O41 Gd2 O31 76.29(12) . . ? O61 Gd2 O31 136.43(12) . . ? O51 Gd2 N5 70.37(12) . 4_676 ? O41 Gd2 N5 70.64(13) . 4_676 ? O61 Gd2 N5 69.96(13) . 4_676 ? O31 Gd2 N5 134.80(12) . 4_676 ? O51 Gd2 N13 81.71(12) . . ? O41 Gd2 N13 145.13(11) . . ? O61 Gd2 N13 69.16(12) . . ? O31 Gd2 N13 89.62(12) . . ? N5 Gd2 N13 134.43(12) 4_676 . ? O51 Gd2 N12 138.75(12) . . ? O41 Gd2 N12 133.03(12) . . ? O61 Gd2 N12 70.11(12) . . ? O31 Gd2 N12 66.36(11) . . ? N5 Gd2 N12 118.34(12) 4_676 . ? N13 Gd2 N12 63.76(12) . . ? O51 Gd2 N11 142.15(12) . . ? O41 Gd2 N11 79.65(12) . . ? O61 Gd2 N11 89.77(12) . . ? O31 Gd2 N11 72.69(11) . . ? N5 Gd2 N11 71.79(12) 4_676 . ? N13 Gd2 N11 126.76(12) . . ? N12 Gd2 N11 63.12(12) . . ? O51 Gd2 N1 69.43(12) . . ? O41 Gd2 N1 73.46(12) . . ? O61 Gd2 N1 131.28(12) . . ? O31 Gd2 N1 69.59(11) . . ? N5 Gd2 N1 125.93(13) 4_676 . ? N13 Gd2 N1 71.73(12) . . ? N12 Gd2 N1 115.72(12) . . ? N11 Gd2 N1 137.67(12) . . ? C15 N11 C11 118.3(4) . . ? C15 N11 Gd2 120.7(3) . . ? C11 N11 Gd2 121.0(3) . . ? C20 N12 C16 118.7(4) . . ? C20 N12 Gd2 119.8(3) . . ? C16 N12 Gd2 119.9(3) . . ? C25 N13 C21 118.0(4) . . ? C25 N13 Gd2 119.9(3) . . ? C21 N13 Gd2 120.1(3) . . ? N11 C11 C12 123.5(5) . . ? N11 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? C11 C12 C13 117.9(6) . . ? C11 C12 H12 121.1 . . ? C13 C12 H12 121.1 . . ? C14 C13 C12 119.3(5) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.1(6) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? N11 C15 C14 121.0(5) . . ? N11 C15 C16 117.4(4) . . ? C14 C15 C16 121.5(5) . . ? N12 C16 C17 121.3(5) . . ? N12 C16 C15 116.2(4) . . ? C17 C16 C15 122.5(5) . . ? C18 C17 C16 119.6(5) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 119.4(5) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 119.1(5) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? N12 C20 C19 121.9(5) . . ? N12 C20 C21 116.7(4) . . ? C19 C20 C21 121.4(5) . . ? N13 C21 C22 121.8(5) . . ? N13 C21 C20 116.4(4) . . ? C22 C21 C20 121.8(5) . . ? C23 C22 C21 119.9(5) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 119.0(5) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C25 119.0(5) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? N13 C25 C24 122.3(5) . . ? N13 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C31 O31 Gd2 136.2(3) . . ? O31 C31 N31 125.0(5) . . ? O31 C31 H31 117.5 . . ? N31 C31 H31 117.5 . . ? C31 N31 C33 120.7(5) . . ? C31 N31 C32 122.7(5) . . ? C33 N31 C32 116.5(5) . . ? N31 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N31 C33 H33A 109.5 . . ? N31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C41 O41 Gd2 142.3(3) . . ? O41 C41 N41 125.9(5) . . ? O41 C41 H41 117.0 . . ? N41 C41 H41 117.0 . . ? C41 N41 C42 120.9(6) . . ? C41 N41 C43 121.2(5) . . ? C42 N41 C43 117.8(6) . . ? N41 C42 H42A 109.5 . . ? N41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N41 C43 H43A 109.5 . . ? N41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C51A O51 C51B 50.6(7) . . ? C51A O51 Gd2 161.1(6) . . ? C51B O51 Gd2 134.6(6) . . ? O51 C51A N51A 124.2(10) . . ? C51A N51A C52A 112.9(11) . . ? C53A N51A C52A 123.8(12) . . ? O51 C51B N51B 115.4(10) . . ? C53B N51B C51B 136.8(16) . . ? C53B N51B C52B 118.2(16) . . ? C51B N51B C52B 104.9(13) . . ? C61 O61 Gd2 143.5(4) . . ? O61 C61 N61 129.0(7) . . ? O61 C61 H61 115.5 . . ? N61 C61 H61 115.5 . . ? C61 N61 C63 120.5(7) . . ? C61 N61 C62 125.7(8) . . ? C63 N61 C62 113.7(8) . . ? N61 C62 H62A 109.5 . . ? N61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N61 C63 H63A 109.5 . . ? N61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C72 O71 H71 109.5 . . ? O71 C72 C73 122.7(10) . . ? O71 C72 H72A 106.7 . . ? C73 C72 H72A 106.7 . . ? O71 C72 H72B 106.7 . . ? C73 C72 H72B 106.7 . . ? H72A C72 H72B 106.6 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.101 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.111