Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Diaz, Carmen' 'El Fallah, Mohamed S.' 'Figuerola, Albert' 'Maestro, Miguel' 'Ribas, Joan' _publ_contact_author_name 'Prof Joan Ribas' _publ_contact_author_address ; Prof Joan Ribas Department Quimica Inorganica Universitat de Barcelona C/ Diagonal, 647 Barcelona SPAIN 08028 ; _publ_contact_author_email 'JOAN.RIBAS@QI.UB.ES' data_for_complex_1 _database_code_CSD 150442 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H28 Cr Gd N10 O4, 3(H2 O)' _chemical_formula_sum 'C18 H34 Cr Gd N10 O7' _chemical_formula_weight 711.80 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M '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 13.1592(2) _cell_length_b 12.8779(2) _cell_length_c 18.9782(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.83 _cell_angle_gamma 90.00 _cell_volume 3025.30(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 2.582 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3308 _exptl_absorpt_correction_T_max 0.4248 _exptl_absorpt_process_details 'Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20152 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7471 _reflns_number_gt 6672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7471 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Gd1 Gd 0.027017(8) 0.923121(8) 0.224814(6) 0.01324(4) Uani 1 1 d . . . Cr1 Cr 0.04182(3) 1.35923(3) 0.261327(19) 0.01218(8) Uani 1 1 d . . . O1 O -0.10624(14) 0.79719(14) 0.21678(13) 0.0327(5) Uani 1 1 d . . . H1A H -0.1749 0.7987 0.2127 0.039 Uiso 1 1 d R . . H1B H -0.0838 0.7311 0.2304 0.039 Uiso 1 1 d R . . O2 O 0.00943(14) 0.96559(14) 0.09794(9) 0.0231(4) Uani 1 1 d . . . H2A H 0.0410 0.9337 0.0732 0.028 Uiso 1 1 d R . . H2B H -0.0260 1.0229 0.0737 0.028 Uiso 1 1 d R . . O3 O -0.09938(14) 1.12524(14) 0.00441(10) 0.0252(4) Uani 1 1 d . . . H3A H -0.1710 1.1251 -0.0130 0.030 Uiso 1 1 d R . . H3B H -0.0936 1.1943 0.0153 0.030 Uiso 1 1 d R . . O4 O 0.11825(16) 0.82024(16) 0.33154(11) 0.0332(5) Uani 1 1 d . . . O5 O 0.06607(14) 0.77448(14) 0.16572(11) 0.0266(4) Uani 1 1 d . . . O6 O -0.14307(13) 1.00583(14) 0.16817(10) 0.0241(4) Uani 1 1 d . . . O7 O -0.02280(16) 0.98041(16) 0.32865(11) 0.0311(4) Uani 1 1 d . . . N1 N 0.07602(16) 1.11250(16) 0.24679(12) 0.0207(4) Uani 1 1 d . . . N2 N -0.0330(2) 1.59755(19) 0.25538(16) 0.0333(6) Uani 1 1 d . . . N3 N 0.22507(17) 0.93223(15) 0.24212(13) 0.0210(4) Uani 1 1 d . . . N4 N -0.0588(2) 1.3202(2) 0.08359(13) 0.0375(6) Uani 1 1 d . . . N5 N -0.18295(18) 1.3026(2) 0.28481(15) 0.0339(6) Uani 1 1 d . . . N6 N 0.1714(2) 1.3685(2) 0.43855(13) 0.0363(6) Uani 1 1 d . . . N7 N 0.21836(18) 0.69299(18) 0.40451(13) 0.0282(5) Uani 1 1 d . . . N8 N 0.1026(2) 0.63673(17) 0.10493(12) 0.0277(5) Uani 1 1 d . . . N9 N -0.28820(16) 1.11106(17) 0.12102(12) 0.0219(4) Uani 1 1 d . . . N10 N -0.1184(2) 1.0579(2) 0.39254(14) 0.0310(5) Uani 1 1 d . . . C1 C 0.07319(17) 1.20069(18) 0.25624(13) 0.0169(4) Uani 1 1 d . . . C2 C -0.00375(19) 1.51314(19) 0.25797(14) 0.0205(5) Uani 1 1 d . . . C3 C 0.19000(19) 1.40670(17) 0.25515(13) 0.0168(4) Uani 1 1 d . . . C4 C -0.0255(2) 1.34252(19) 0.14607(14) 0.0214(5) Uani 1 1 d . . . C5 C -0.10254(19) 1.32079(18) 0.27577(14) 0.0198(5) Uani 1 1 d . . . C6 C 0.1195(2) 1.3639(2) 0.37609(14) 0.0212(5) Uani 1 1 d . . . C7 C 0.1932(3) 0.7580(3) 0.34835(19) 0.0411(8) Uani 1 1 d . . . H7A H 0.2371 0.7570 0.3176 0.049 Uiso 1 1 calc R . . C8 C 0.1310(2) 0.7174(2) 0.14972(15) 0.0278(6) Uani 1 1 d . . . H8A H 0.2058 0.7329 0.1712 0.033 Uiso 1 1 calc R . . C9 C -0.1847(2) 1.0939(2) 0.15431(14) 0.0215(5) Uani 1 1 d . . . H9A H -0.1383 1.1524 0.1689 0.026 Uiso 1 1 calc R . . C10 C -0.1090(2) 0.9955(2) 0.34001(15) 0.0287(6) Uani 1 1 d . . . H10A H -0.1717 0.9602 0.3092 0.034 Uiso 1 1 calc R . . C11 C 0.3073(3) 0.6205(3) 0.4163(2) 0.0518(9) Uani 1 1 d . . . H11A H 0.3432 0.6340 0.3797 0.078 Uiso 1 1 calc R . . H11B H 0.2794 0.5493 0.4101 0.078 Uiso 1 1 calc R . . H11C H 0.3592 0.6293 0.4670 0.078 Uiso 1 1 calc R . . C12 C 0.1514(3) 0.6801(4) 0.4497(2) 0.0630(12) Uani 1 1 d . . . H12A H 0.0976 0.7359 0.4387 0.094 Uiso 1 1 calc R . . H12B H 0.1962 0.6828 0.5028 0.094 Uiso 1 1 calc R . . H12C H 0.1145 0.6129 0.4386 0.094 Uiso 1 1 calc R . . C13 C 0.1824(3) 0.5723(3) 0.08807(19) 0.0508(10) Uani 1 1 d . . . H13A H 0.2548 0.6007 0.1133 0.076 Uiso 1 1 calc R . . H13B H 0.1674 0.5715 0.0338 0.076 Uiso 1 1 calc R . . H13C H 0.1787 0.5014 0.1057 0.076 Uiso 1 1 calc R . . C14 C -0.0109(3) 0.6105(3) 0.06933(19) 0.0430(8) Uani 1 1 d . . . H14A H -0.0547 0.6532 0.0908 0.065 Uiso 1 1 calc R . . H14B H -0.0219 0.5369 0.0778 0.065 Uiso 1 1 calc R . . H14C H -0.0326 0.6237 0.0154 0.065 Uiso 1 1 calc R . . C15 C -0.3306(2) 1.2167(2) 0.10597(17) 0.0359(7) Uani 1 1 d . . . H15A H -0.2708 1.2664 0.1230 0.054 Uiso 1 1 calc R . . H15B H -0.3813 1.2292 0.1328 0.054 Uiso 1 1 calc R . . H15C H -0.3680 1.2254 0.0520 0.054 Uiso 1 1 calc R . . C16 C -0.3651(2) 1.0259(2) 0.09511(16) 0.0302(6) Uani 1 1 d . . . H16A H -0.3270 0.9595 0.1084 0.045 Uiso 1 1 calc R . . H16B H -0.3996 1.0301 0.0406 0.045 Uiso 1 1 calc R . . H16C H -0.4204 1.0309 0.1189 0.045 Uiso 1 1 calc R . . C17 C -0.2227(3) 1.0739(3) 0.4021(2) 0.0589(12) Uani 1 1 d . . . H17A H -0.2768 1.0284 0.3678 0.088 Uiso 1 1 calc R . . H17B H -0.2448 1.1465 0.3913 0.088 Uiso 1 1 calc R . . H17C H -0.2166 1.0576 0.4539 0.088 Uiso 1 1 calc R . . C18 C -0.0287(3) 1.1204(3) 0.4378(2) 0.0457(8) Uani 1 1 d . . . H18A H 0.0365 1.1017 0.4267 0.069 Uiso 1 1 calc R . . H18B H -0.0167 1.1079 0.4909 0.069 Uiso 1 1 calc R . . H18C H -0.0451 1.1940 0.4264 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01119(7) 0.01229(7) 0.01682(7) 0.00098(4) 0.00550(5) 0.00171(4) Cr1 0.00989(16) 0.01215(16) 0.01427(17) -0.00068(12) 0.00379(13) -0.00015(12) O1 0.0158(8) 0.0164(8) 0.0703(15) 0.0096(9) 0.0203(9) 0.0031(7) O2 0.0258(9) 0.0257(9) 0.0189(8) 0.0023(7) 0.0090(7) 0.0058(7) O3 0.0238(9) 0.0266(10) 0.0229(9) -0.0027(7) 0.0052(7) 0.0040(7) O4 0.0322(10) 0.0388(11) 0.0303(10) 0.0175(8) 0.0129(9) 0.0167(9) O5 0.0266(9) 0.0187(9) 0.0374(11) -0.0075(8) 0.0148(8) 0.0000(7) O6 0.0169(8) 0.0226(9) 0.0305(10) 0.0033(7) 0.0051(7) 0.0060(7) O7 0.0334(10) 0.0368(11) 0.0289(10) 0.0018(8) 0.0183(8) 0.0085(9) N1 0.0164(10) 0.0165(10) 0.0279(11) -0.0021(8) 0.0060(8) -0.0002(8) N2 0.0403(15) 0.0186(11) 0.0454(15) 0.0049(10) 0.0204(12) 0.0060(10) N3 0.0167(10) 0.0193(10) 0.0266(11) -0.0007(8) 0.0069(9) -0.0001(7) N4 0.0520(16) 0.0331(13) 0.0215(12) 0.0002(9) 0.0048(11) -0.0075(12) N5 0.0214(11) 0.0363(13) 0.0490(16) -0.0096(11) 0.0185(11) -0.0045(10) N6 0.0319(13) 0.0530(17) 0.0200(11) -0.0003(11) 0.0037(10) -0.0031(11) N7 0.0251(11) 0.0276(12) 0.0303(12) 0.0104(9) 0.0072(9) 0.0076(9) N8 0.0407(13) 0.0203(11) 0.0196(10) -0.0031(8) 0.0068(9) 0.0072(9) N9 0.0181(10) 0.0250(11) 0.0197(10) -0.0008(8) 0.0026(8) 0.0065(8) N10 0.0276(12) 0.0406(14) 0.0276(12) -0.0038(10) 0.0130(10) 0.0067(10) C1 0.0102(10) 0.0211(11) 0.0182(11) 0.0023(9) 0.0032(8) 0.0003(8) C2 0.0198(11) 0.0198(12) 0.0229(12) 0.0006(9) 0.0086(10) 0.0007(9) C3 0.0173(11) 0.0153(10) 0.0191(11) -0.0011(8) 0.0077(9) 0.0003(8) C4 0.0239(12) 0.0176(11) 0.0214(12) 0.0008(9) 0.0061(10) -0.0027(9) C5 0.0187(11) 0.0173(11) 0.0239(12) -0.0031(9) 0.0077(10) 0.0000(9) C6 0.0182(11) 0.0240(12) 0.0219(12) 0.0004(9) 0.0077(9) -0.0011(9) C7 0.0401(17) 0.0469(19) 0.0430(18) 0.0206(15) 0.0229(15) 0.0193(14) C8 0.0259(13) 0.0262(13) 0.0278(13) -0.0061(10) 0.0046(11) 0.0061(10) C9 0.0191(12) 0.0213(12) 0.0219(12) -0.0005(9) 0.0039(10) 0.0026(9) C10 0.0301(14) 0.0324(14) 0.0261(13) 0.0009(11) 0.0128(11) 0.0031(11) C11 0.0423(19) 0.052(2) 0.062(2) 0.0238(18) 0.0181(18) 0.0245(17) C12 0.068(3) 0.074(3) 0.060(3) 0.028(2) 0.040(2) 0.024(2) C13 0.069(3) 0.048(2) 0.0263(16) -0.0095(13) 0.0053(16) 0.0365(18) C14 0.056(2) 0.0424(17) 0.0381(17) -0.0174(14) 0.0250(16) -0.0262(16) C15 0.0355(15) 0.0309(15) 0.0322(15) -0.0038(12) -0.0003(12) 0.0178(12) C16 0.0186(12) 0.0378(16) 0.0308(14) 0.0024(12) 0.0041(11) -0.0002(11) C17 0.038(2) 0.096(4) 0.052(2) -0.011(2) 0.0273(18) 0.0133(19) C18 0.0458(19) 0.0468(19) 0.0434(19) -0.0152(15) 0.0135(15) -0.0007(16) _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 O1 2.3552(17) . ? Gd1 O5 2.3617(17) . ? Gd1 O4 2.3768(18) . ? Gd1 O6 2.3805(16) . ? Gd1 O7 2.3946(18) . ? Gd1 O2 2.4026(17) . ? Gd1 N3 2.517(2) . ? Gd1 N1 2.521(2) . ? Cr1 C2 2.065(2) . ? Cr1 C6 2.069(2) . ? Cr1 C5 2.069(2) . ? Cr1 C4 2.074(2) . ? Cr1 C3 2.084(2) . ? Cr1 C1 2.092(2) . ? O4 C7 1.226(3) . ? O5 C8 1.240(3) . ? O6 C9 1.248(3) . ? O7 C10 1.240(3) . ? N1 C1 1.152(3) . ? N2 C2 1.149(3) . ? N3 C3 1.149(3) 2_545 ? N4 C4 1.152(3) . ? N5 C5 1.152(3) . ? N6 C6 1.151(3) . ? N7 C7 1.307(4) . ? N7 C12 1.433(4) . ? N7 C11 1.454(4) . ? N8 C8 1.314(3) . ? N8 C14 1.455(4) . ? N8 C13 1.456(4) . ? N9 C9 1.311(3) . ? N9 C16 1.460(4) . ? N9 C15 1.462(3) . ? N10 C10 1.318(4) . ? N10 C18 1.446(4) . ? N10 C17 1.459(4) . ? C3 N3 1.149(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O5 71.84(6) . . ? O1 Gd1 O4 79.69(7) . . ? O5 Gd1 O4 79.89(7) . . ? O1 Gd1 O6 73.35(6) . . ? O5 Gd1 O6 118.10(6) . . ? O4 Gd1 O6 139.46(6) . . ? O1 Gd1 O7 81.93(7) . . ? O5 Gd1 O7 143.61(7) . . ? O4 Gd1 O7 70.77(7) . . ? O6 Gd1 O7 75.87(6) . . ? O1 Gd1 O2 105.99(7) . . ? O5 Gd1 O2 70.79(6) . . ? O4 Gd1 O2 146.10(6) . . ? O6 Gd1 O2 71.91(6) . . ? O7 Gd1 O2 142.61(6) . . ? O1 Gd1 N3 139.10(6) . . ? O5 Gd1 N3 73.57(6) . . ? O4 Gd1 N3 73.35(7) . . ? O6 Gd1 N3 144.24(6) . . ? O7 Gd1 N3 116.03(7) . . ? O2 Gd1 N3 82.15(7) . . ? O1 Gd1 N1 145.08(6) . . ? O5 Gd1 N1 141.08(7) . . ? O4 Gd1 N1 111.80(7) . . ? O6 Gd1 N1 77.90(6) . . ? O7 Gd1 N1 72.05(7) . . ? O2 Gd1 N1 82.98(7) . . ? N3 Gd1 N1 74.80(6) . . ? C2 Cr1 C6 92.24(10) . . ? C2 Cr1 C5 87.91(9) . . ? C6 Cr1 C5 90.86(10) . . ? C2 Cr1 C4 92.94(10) . . ? C6 Cr1 C4 174.25(10) . . ? C5 Cr1 C4 91.83(10) . . ? C2 Cr1 C3 89.09(9) . . ? C6 Cr1 C3 85.04(10) . . ? C5 Cr1 C3 174.83(9) . . ? C4 Cr1 C3 92.54(10) . . ? C2 Cr1 C1 174.27(9) . . ? C6 Cr1 C1 92.42(9) . . ? C5 Cr1 C1 88.68(9) . . ? C4 Cr1 C1 82.56(9) . . ? C3 Cr1 C1 94.63(9) . . ? C7 O4 Gd1 135.7(2) . . ? C8 O5 Gd1 151.12(17) . . ? C9 O6 Gd1 141.26(17) . . ? C10 O7 Gd1 135.52(19) . . ? C1 N1 Gd1 163.58(18) . . ? C3 N3 Gd1 160.19(18) 2_545 . ? C7 N7 C12 121.7(3) . . ? C7 N7 C11 120.4(3) . . ? C12 N7 C11 117.4(3) . . ? C8 N8 C14 120.3(2) . . ? C8 N8 C13 121.7(3) . . ? C14 N8 C13 118.0(2) . . ? C9 N9 C16 121.6(2) . . ? C9 N9 C15 121.1(2) . . ? C16 N9 C15 117.3(2) . . ? C10 N10 C18 121.4(3) . . ? C10 N10 C17 121.0(3) . . ? C18 N10 C17 117.4(3) . . ? N1 C1 Cr1 170.6(2) . . ? N2 C2 Cr1 177.5(2) . . ? N3 C3 Cr1 174.5(2) 2 . ? N4 C4 Cr1 171.2(2) . . ? N5 C5 Cr1 177.8(2) . . ? N6 C6 Cr1 173.6(2) . . ? O4 C7 N7 126.2(3) . . ? O5 C8 N8 124.0(3) . . ? O6 C9 N9 124.4(2) . . ? O7 C10 N10 123.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Gd1 O4 C7 107.8(3) . . . . ? O5 Gd1 O4 C7 34.6(3) . . . . ? O6 Gd1 O4 C7 156.5(3) . . . . ? O7 Gd1 O4 C7 -167.2(3) . . . . ? O2 Gd1 O4 C7 4.4(4) . . . . ? N3 Gd1 O4 C7 -41.1(3) . . . . ? N1 Gd1 O4 C7 -106.6(3) . . . . ? O1 Gd1 O5 C8 -152.8(4) . . . . ? O4 Gd1 O5 C8 -70.5(4) . . . . ? O6 Gd1 O5 C8 148.3(4) . . . . ? O7 Gd1 O5 C8 -106.8(4) . . . . ? O2 Gd1 O5 C8 92.2(4) . . . . ? N3 Gd1 O5 C8 5.0(4) . . . . ? N1 Gd1 O5 C8 41.8(4) . . . . ? O1 Gd1 O6 C9 162.4(3) . . . . ? O5 Gd1 O6 C9 -139.5(3) . . . . ? O4 Gd1 O6 C9 112.0(3) . . . . ? O7 Gd1 O6 C9 76.7(3) . . . . ? O2 Gd1 O6 C9 -84.0(3) . . . . ? N3 Gd1 O6 C9 -38.4(3) . . . . ? N1 Gd1 O6 C9 2.5(3) . . . . ? O1 Gd1 O7 C10 -45.6(3) . . . . ? O5 Gd1 O7 C10 -89.3(3) . . . . ? O4 Gd1 O7 C10 -127.4(3) . . . . ? O6 Gd1 O7 C10 29.2(3) . . . . ? O2 Gd1 O7 C10 60.3(3) . . . . ? N3 Gd1 O7 C10 173.1(3) . . . . ? N1 Gd1 O7 C10 110.8(3) . . . . ? O1 Gd1 N1 C1 -7.4(7) . . . . ? O5 Gd1 N1 C1 147.8(7) . . . . ? O4 Gd1 N1 C1 -111.0(7) . . . . ? O6 Gd1 N1 C1 27.7(7) . . . . ? O7 Gd1 N1 C1 -51.2(7) . . . . ? O2 Gd1 N1 C1 100.6(7) . . . . ? N3 Gd1 N1 C1 -175.7(7) . . . . ? O1 Gd1 N3 C3 15.3(6) . . . 2_545 ? O5 Gd1 N3 C3 -17.9(6) . . . 2_545 ? O4 Gd1 N3 C3 66.2(6) . . . 2_545 ? O6 Gd1 N3 C3 -133.4(6) . . . 2_545 ? O7 Gd1 N3 C3 124.3(6) . . . 2_545 ? O2 Gd1 N3 C3 -90.1(6) . . . 2_545 ? N1 Gd1 N3 C3 -174.9(6) . . . 2_545 ? Gd1 N1 C1 Cr1 -35.4(18) . . . . ? C2 Cr1 C1 N1 -7(2) . . . . ? C6 Cr1 C1 N1 137.3(13) . . . . ? C5 Cr1 C1 N1 46.5(13) . . . . ? C4 Cr1 C1 N1 -45.5(13) . . . . ? C3 Cr1 C1 N1 -137.5(13) . . . . ? C6 Cr1 C2 N2 -113(5) . . . . ? C5 Cr1 C2 N2 -22(5) . . . . ? C4 Cr1 C2 N2 70(5) . . . . ? C3 Cr1 C2 N2 162(5) . . . . ? C1 Cr1 C2 N2 32(6) . . . . ? C2 Cr1 C3 N3 96(2) . . . 2 ? C6 Cr1 C3 N3 4(2) . . . 2 ? C5 Cr1 C3 N3 42(3) . . . 2 ? C4 Cr1 C3 N3 -171(2) . . . 2 ? C1 Cr1 C3 N3 -88(2) . . . 2 ? C2 Cr1 C4 N4 -178.1(16) . . . . ? C6 Cr1 C4 N4 28(2) . . . . ? C5 Cr1 C4 N4 -90.1(16) . . . . ? C3 Cr1 C4 N4 92.7(16) . . . . ? C1 Cr1 C4 N4 -1.7(16) . . . . ? C2 Cr1 C5 N5 -26(6) . . . . ? C6 Cr1 C5 N5 67(6) . . . . ? C4 Cr1 C5 N5 -118(6) . . . . ? C3 Cr1 C5 N5 29(7) . . . . ? C1 Cr1 C5 N5 159(6) . . . . ? C2 Cr1 C6 N6 -94(2) . . . . ? C5 Cr1 C6 N6 178(100) . . . . ? C4 Cr1 C6 N6 60(3) . . . . ? C3 Cr1 C6 N6 -5(2) . . . . ? C1 Cr1 C6 N6 89(2) . . . . ? Gd1 O4 C7 N7 -165.1(2) . . . . ? C12 N7 C7 O4 6.6(6) . . . . ? C11 N7 C7 O4 177.7(3) . . . . ? Gd1 O5 C8 N8 -174.9(2) . . . . ? C14 N8 C8 O5 1.2(4) . . . . ? C13 N8 C8 O5 180.0(3) . . . . ? Gd1 O6 C9 N9 -178.82(18) . . . . ? C16 N9 C9 O6 -1.5(4) . . . . ? C15 N9 C9 O6 -179.3(3) . . . . ? Gd1 O7 C10 N10 -157.1(2) . . . . ? C18 N10 C10 O7 4.9(5) . . . . ? C17 N10 C10 O7 178.8(3) . . . . ? 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 O1 H1A N5 0.88 1.89 2.765(3) 173.9 2_445 O1 H2A N2 0.91 1.85 2.756(3) 176.9 1_545 O2 H2A O3 0.83 2.03 2.847(2) 168.3 3_575 O2 H2B O3 0.91 1.88 2.775(2) 167.2 . O3 H3A N6 0.89 1.96 2.848(3) 173.9 4_585 O3 H3B N4 0.91 2.03 2.881(3) 155.3 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.813 _refine_diff_density_min -2.536 _refine_diff_density_rms 0.170 data_for_complex_2 _database_code_CSD 150443 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H36 Cr Gd N11 O8' _chemical_formula_sum 'C31 H36 Cr Gd N11 O8' _chemical_formula_weight 899.96 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' 'Cr' 'Cr' 0.3209 0.6236 '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 9.8152(3) _cell_length_b 10.7725(3) _cell_length_c 19.7038(6) _cell_angle_alpha 83.55 _cell_angle_beta 83.7750(10) _cell_angle_gamma 65.0920(10) _cell_volume 1873.30(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 2.107 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3903 _exptl_absorpt_correction_T_max 0.6780 _exptl_absorpt_process_details 'Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -2.08 _diffrn_reflns_number 12920 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8824 _reflns_number_gt 7867 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8824 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.279224(15) 0.090463(14) 0.246036(7) 0.01304(5) Uani 1 1 d . . . Cr1 Cr 0.72337(5) -0.45703(5) 0.22669(2) 0.01379(10) Uani 1 1 d . . . O1 O 0.3154(3) 0.2782(2) 0.18243(12) 0.0241(5) Uani 1 1 d . . . H1A H 0.2598 0.3213 0.1498 0.029 Uiso 1 1 d R . . H1B H 0.3586 0.3308 0.1858 0.029 Uiso 1 1 d R . . O2 O 0.2540(3) -0.0111(3) 0.35578(11) 0.0295(6) Uani 1 1 d . . . H2A H 0.2429 -0.0857 0.3627 0.035 Uiso 1 1 d R . . H2B H 0.2787 0.0041 0.3930 0.035 Uiso 1 1 d R . . O3 O 0.2779(3) 0.0729(2) 0.12491(11) 0.0224(5) Uani 1 1 d . . . H3A H 0.2295 0.1438 0.0993 0.027 Uiso 1 1 d R . . H3B H 0.2456 0.0148 0.1164 0.027 Uiso 1 1 d R . . O4 O 0.1345(2) -0.0373(2) 0.23556(11) 0.0189(4) Uani 1 1 d . . . H4A H 0.0821 -0.0138 0.2009 0.023 Uiso 1 1 d R . . H4B H 0.1659 -0.1240 0.2369 0.023 Uiso 1 1 d R . . O5 O 0.1349(3) 0.3429(2) 0.07120(12) 0.0275(5) Uani 1 1 d . . . H5A H 0.1649 0.3573 0.0302 0.033 Uiso 1 1 d R . . H5B H 0.0465 0.4063 0.0695 0.033 Uiso 1 1 d R . . O6 O 0.2268(3) -0.3143(2) 0.25937(13) 0.0293(5) Uani 1 1 d . . . H6A H 0.2983 -0.3833 0.2423 0.035 Uiso 1 1 d R . . H6B H 0.1572 -0.3390 0.2541 0.035 Uiso 1 1 d R . . O7 O 0.4164(7) -0.3845(6) 0.4841(3) 0.0491(17) Uani 0.555(6) 1 d P A 1 H7A H 0.4323 -0.4499 0.4595 0.059 Uiso 0.555(6) 1 d PR A 1 H7B H 0.4227 -0.3998 0.5271 0.059 Uiso 0.555(6) 1 d PR A 1 O8 O 0.2125(8) -0.2315(6) 0.3895(3) 0.0446(16) Uani 0.555(6) 1 d P A 1 H8A H 0.2735 -0.2764 0.4200 0.053 Uiso 0.555(6) 1 d PR A 1 H8B H 0.2595 -0.2885 0.3595 0.053 Uiso 0.555(6) 1 d PR A 1 O7' O 0.1866(13) -0.2482(11) 0.5178(5) 0.098(4) Uani 0.445(6) 1 d P A 2 H7A' H 0.2334 -0.3158 0.5455 0.118 Uiso 0.445(6) 1 d PR A 2 H7B' H 0.2670 -0.2555 0.4941 0.118 Uiso 0.445(6) 1 d PR A 2 O8' O 0.3195(8) -0.2904(6) 0.3808(3) 0.0318(15) Uani 0.445(6) 1 d P A 2 H8C' H 0.2838 -0.2823 0.4221 0.038 Uiso 0.445(6) 1 d PR A 2 H8D' H 0.2722 -0.3039 0.3507 0.038 Uiso 0.445(6) 1 d PR A 2 N1 N 0.4664(3) -0.1482(3) 0.23103(14) 0.0222(6) Uani 1 1 d . . . N2 N 0.6647(4) -0.4980(4) 0.38966(16) 0.0427(9) Uani 1 1 d . . . N3 N 0.9630(4) -0.3359(4) 0.24493(18) 0.0362(7) Uani 1 1 d . . . N4 N 0.0177(3) 0.2580(3) 0.22867(14) 0.0212(5) Uani 1 1 d . . . N5 N 0.8001(4) -0.4207(3) 0.06463(15) 0.0324(7) Uani 1 1 d . . . N6 N 0.4868(3) -0.5844(3) 0.20925(15) 0.0268(6) Uani 1 1 d . . . N7 N 0.5159(3) 0.0919(3) 0.28584(13) 0.0190(5) Uani 1 1 d . . . N8 N 0.2393(3) 0.2599(3) 0.33600(13) 0.0214(6) Uani 1 1 d . . . N9 N 1.2382(3) -0.1496(3) 0.08792(14) 0.0230(6) Uani 1 1 d . . . N10 N 0.9548(3) 0.0378(3) 0.11973(15) 0.0295(7) Uani 1 1 d . . . N11 N 0.3074(4) 0.0423(3) 0.48325(15) 0.0337(7) Uani 1 1 d . . . C1 C 0.5532(3) -0.2603(3) 0.22819(16) 0.0189(6) Uani 1 1 d . . . C2 C 0.6881(4) -0.4850(3) 0.33161(17) 0.0234(7) Uani 1 1 d . . . C3 C 0.8753(3) -0.3766(3) 0.23916(17) 0.0215(6) Uani 1 1 d . . . C4 C 0.9067(3) -0.6460(3) 0.22687(15) 0.0168(6) Uani 1 1 d . . . C5 C 0.7672(3) -0.4320(3) 0.12181(16) 0.0210(6) Uani 1 1 d . . . C6 C 0.5725(3) -0.5410(3) 0.21437(16) 0.0189(6) Uani 1 1 d . . . C7 C 0.6533(4) 0.0068(4) 0.26099(18) 0.0250(7) Uani 1 1 d . . . H7C H 0.6593 -0.0536 0.2294 0.030 Uiso 1 1 calc R . . C8 C 0.7853(4) 0.0048(4) 0.2798(2) 0.0319(8) Uani 1 1 d . . . H8C H 0.8777 -0.0557 0.2612 0.038 Uiso 1 1 calc R . . C9 C 0.7789(4) 0.0926(4) 0.3261(2) 0.0363(9) Uani 1 1 d . . . H9A H 0.8667 0.0929 0.3395 0.044 Uiso 1 1 calc R . . C10 C 0.6397(4) 0.1810(4) 0.3527(2) 0.0332(8) Uani 1 1 d . . . H10A H 0.6329 0.2414 0.3844 0.040 Uiso 1 1 calc R . . C11 C 0.5088(4) 0.1789(3) 0.33161(16) 0.0211(6) Uani 1 1 d . . . C12 C 0.3580(4) 0.2718(3) 0.35828(16) 0.0221(6) Uani 1 1 d . . . C13 C 0.3382(5) 0.3667(4) 0.4052(2) 0.0367(9) Uani 1 1 d . . . H13A H 0.4212 0.3744 0.4197 0.044 Uiso 1 1 calc R . . C14 C 0.1959(5) 0.4485(4) 0.4299(2) 0.0408(10) Uani 1 1 d . . . H14A H 0.1816 0.5122 0.4611 0.049 Uiso 1 1 calc R . . C15 C 0.0741(5) 0.4355(4) 0.40822(18) 0.0327(8) Uani 1 1 d . . . H15A H -0.0235 0.4899 0.4243 0.039 Uiso 1 1 calc R . . C16 C 0.1011(4) 0.3396(4) 0.36190(17) 0.0276(7) Uani 1 1 d . . . H16A H 0.0192 0.3296 0.3478 0.033 Uiso 1 1 calc R . . C17 C 1.3781(4) -0.2464(4) 0.08016(17) 0.0255(7) Uani 1 1 d . . . H17A H 1.4579 -0.2235 0.0846 0.031 Uiso 1 1 calc R . . C18 C 1.4104(4) -0.3787(4) 0.06589(17) 0.0281(7) Uani 1 1 d . . . H18A H 1.5095 -0.4432 0.0605 0.034 Uiso 1 1 calc R . . C19 C 1.2924(4) -0.4127(4) 0.0599(2) 0.0324(8) Uani 1 1 d . . . H19A H 1.3107 -0.5012 0.0503 0.039 Uiso 1 1 calc R . . C20 C 1.1467(4) -0.3150(4) 0.06812(19) 0.0305(8) Uani 1 1 d . . . H20A H 1.0656 -0.3367 0.0647 0.037 Uiso 1 1 calc R . . C21 C 1.1233(4) -0.1831(4) 0.08162(16) 0.0233(7) Uani 1 1 d . . . C22 C 0.9690(4) -0.0709(4) 0.08811(16) 0.0242(7) Uani 1 1 d . . . C23 C 0.8471(4) -0.0788(4) 0.0619(2) 0.0358(9) Uani 1 1 d . . . H23A H 0.8593 -0.1565 0.0411 0.043 Uiso 1 1 calc R . . C24 C 0.7078(4) 0.0303(5) 0.0673(2) 0.0393(9) Uani 1 1 d . . . H24A H 0.6246 0.0265 0.0507 0.047 Uiso 1 1 calc R . . C25 C 0.6934(4) 0.1448(4) 0.09747(19) 0.0355(9) Uani 1 1 d . . . H25A H 0.6016 0.2209 0.1004 0.043 Uiso 1 1 calc R . . C26 C 0.8191(4) 0.1430(4) 0.12306(19) 0.0342(8) Uani 1 1 d . . . H26A H 0.8091 0.2198 0.1440 0.041 Uiso 1 1 calc R . . C27 C 0.1675(5) 0.1163(4) 0.5085(2) 0.0401(9) Uani 1 1 d . . . H27A H 0.0877 0.1135 0.4882 0.048 Uiso 1 1 calc R . . C28 C 0.1349(6) 0.1960(4) 0.5627(2) 0.0437(10) Uani 1 1 d . . . H28A H 0.0361 0.2435 0.5797 0.052 Uiso 1 1 calc R . . C29 C 0.2535(6) 0.2033(4) 0.5911(2) 0.0415(10) Uani 1 1 d . . . H29A H 0.2352 0.2590 0.6268 0.050 Uiso 1 1 calc R . . C30 C 0.3981(5) 0.1284(4) 0.56667(18) 0.0347(9) Uani 1 1 d . . . H30A H 0.4786 0.1330 0.5854 0.042 Uiso 1 1 calc R . . C31 C 0.4231(5) 0.0448(4) 0.51318(17) 0.0290(8) 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 Gd1 0.00601(7) 0.01264(8) 0.01967(8) -0.00322(5) -0.00081(5) -0.00260(5) Cr1 0.0054(2) 0.0134(2) 0.0214(2) -0.00379(17) 0.00052(17) -0.00253(17) O1 0.0237(12) 0.0242(12) 0.0319(12) 0.0057(9) -0.0110(10) -0.0167(10) O2 0.0439(16) 0.0347(14) 0.0227(11) -0.0001(10) -0.0048(11) -0.0286(13) O3 0.0240(12) 0.0200(11) 0.0249(11) -0.0038(9) -0.0032(9) -0.0100(10) O4 0.0123(10) 0.0201(11) 0.0269(11) -0.0042(9) -0.0025(9) -0.0083(9) O5 0.0223(12) 0.0305(13) 0.0255(12) 0.0044(10) -0.0019(10) -0.0082(11) O6 0.0147(11) 0.0224(12) 0.0532(16) -0.0081(11) -0.0023(11) -0.0089(10) O7 0.049(4) 0.065(4) 0.035(3) 0.000(3) -0.006(3) -0.025(3) O8 0.059(5) 0.040(3) 0.044(3) 0.003(2) -0.012(3) -0.029(3) O7' 0.079(8) 0.101(8) 0.079(7) 0.006(6) 0.001(6) -0.006(6) O8' 0.037(4) 0.028(3) 0.033(3) -0.004(2) -0.001(3) -0.016(3) N1 0.0110(12) 0.0194(13) 0.0345(15) -0.0050(11) -0.0026(11) -0.0035(11) N2 0.049(2) 0.057(2) 0.0281(16) -0.0055(15) 0.0038(15) -0.029(2) N3 0.0225(15) 0.0375(18) 0.054(2) -0.0105(15) -0.0027(15) -0.0158(14) N4 0.0143(12) 0.0210(14) 0.0288(14) -0.0054(11) -0.0029(11) -0.0066(11) N5 0.0278(16) 0.0432(19) 0.0268(15) -0.0021(13) -0.0010(13) -0.0155(15) N6 0.0217(14) 0.0276(15) 0.0356(16) 0.0015(12) -0.0053(12) -0.0147(13) N7 0.0152(12) 0.0209(13) 0.0222(12) 0.0011(10) -0.0031(10) -0.0091(11) N8 0.0201(13) 0.0185(13) 0.0217(13) -0.0068(10) -0.0017(11) -0.0028(11) N9 0.0188(13) 0.0261(15) 0.0252(13) -0.0062(11) -0.0018(11) -0.0094(12) N10 0.0201(14) 0.0311(16) 0.0363(16) -0.0119(13) -0.0040(12) -0.0070(13) N11 0.043(2) 0.0368(18) 0.0247(14) -0.0016(13) -0.0050(14) -0.0200(16) C1 0.0109(13) 0.0223(16) 0.0249(15) -0.0046(12) 0.0002(11) -0.0076(12) C2 0.0178(15) 0.0252(17) 0.0276(16) -0.0056(13) 0.0016(13) -0.0092(13) C3 0.0123(14) 0.0200(15) 0.0322(16) -0.0083(13) 0.0018(12) -0.0058(12) C4 0.0079(12) 0.0177(14) 0.0246(14) -0.0045(11) -0.0016(11) -0.0042(11) C5 0.0101(13) 0.0239(16) 0.0285(16) -0.0047(13) -0.0011(12) -0.0059(12) C6 0.0139(14) 0.0178(15) 0.0242(15) -0.0023(11) -0.0003(12) -0.0058(12) C7 0.0148(15) 0.0282(17) 0.0330(17) 0.0000(14) 0.0001(13) -0.0107(14) C8 0.0147(15) 0.036(2) 0.045(2) 0.0055(16) -0.0022(15) -0.0127(15) C9 0.0220(17) 0.042(2) 0.053(2) 0.0097(18) -0.0169(17) -0.0211(17) C10 0.032(2) 0.034(2) 0.045(2) 0.0022(16) -0.0156(17) -0.0230(17) C11 0.0213(15) 0.0216(15) 0.0250(15) 0.0026(12) -0.0065(13) -0.0133(13) C12 0.0263(17) 0.0211(16) 0.0226(15) -0.0003(12) -0.0047(13) -0.0129(14) C13 0.042(2) 0.040(2) 0.039(2) -0.0145(17) -0.0014(18) -0.025(2) C14 0.055(3) 0.037(2) 0.037(2) -0.0207(17) 0.0077(19) -0.024(2) C15 0.037(2) 0.0247(18) 0.0289(17) -0.0099(14) 0.0039(16) -0.0050(16) C16 0.0248(17) 0.0266(18) 0.0248(16) -0.0079(13) -0.0025(13) -0.0027(14) C17 0.0184(15) 0.0316(18) 0.0268(16) -0.0085(14) -0.0020(13) -0.0092(14) C18 0.0244(17) 0.0254(17) 0.0292(17) -0.0074(14) -0.0015(14) -0.0040(14) C19 0.034(2) 0.0235(18) 0.040(2) -0.0070(15) -0.0017(16) -0.0111(16) C20 0.0269(18) 0.0319(19) 0.0395(19) -0.0096(16) -0.0013(15) -0.0173(16) C21 0.0210(16) 0.0271(17) 0.0236(15) -0.0050(13) -0.0011(13) -0.0110(14) C22 0.0199(16) 0.0310(18) 0.0234(15) -0.0031(13) -0.0016(13) -0.0118(14) C23 0.0270(19) 0.039(2) 0.045(2) -0.0097(17) -0.0092(17) -0.0139(17) C24 0.0215(18) 0.053(3) 0.044(2) -0.0030(19) -0.0116(17) -0.0146(18) C25 0.0193(17) 0.046(2) 0.0329(19) -0.0044(17) -0.0032(15) -0.0051(16) C26 0.0232(18) 0.035(2) 0.038(2) -0.0122(16) -0.0045(15) -0.0027(16) C27 0.045(2) 0.043(2) 0.036(2) -0.0013(17) -0.0040(18) -0.021(2) C28 0.048(3) 0.039(2) 0.038(2) 0.0013(18) 0.0020(19) -0.013(2) C29 0.059(3) 0.030(2) 0.0302(19) -0.0073(16) -0.0017(19) -0.012(2) C30 0.049(2) 0.0292(19) 0.0268(17) -0.0036(15) -0.0061(17) -0.0153(18) C31 0.045(2) 0.0256(18) 0.0198(15) 0.0006(13) -0.0054(15) -0.0173(17) _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 O2 2.348(2) . ? Gd1 O1 2.392(2) . ? Gd1 O4 2.393(2) . ? Gd1 O3 2.417(2) . ? Gd1 N4 2.472(3) . ? Gd1 N1 2.479(3) . ? Gd1 N7 2.537(3) . ? Gd1 N8 2.569(2) . ? Cr1 C3 2.062(3) . ? Cr1 C2 2.068(3) . ? Cr1 C4 2.072(3) . ? Cr1 C1 2.074(3) . ? Cr1 C5 2.076(3) . ? Cr1 C6 2.080(3) . ? N1 C1 1.151(4) . ? N2 C2 1.147(4) . ? N3 C3 1.139(4) . ? N4 C4 1.145(4) 1_465 ? N5 C5 1.145(4) . ? N6 C6 1.138(4) . ? N7 C7 1.347(4) . ? N7 C11 1.349(4) . ? N8 C16 1.343(4) . ? N8 C12 1.348(4) . ? N9 C17 1.334(4) . ? N9 C21 1.342(4) . ? N10 C22 1.336(4) . ? N10 C26 1.338(5) . ? N11 C27 1.338(5) . ? N11 C31 1.346(5) . ? C4 N4 1.145(4) 1_645 ? C7 C8 1.377(5) . ? C8 C9 1.364(6) . ? C9 C10 1.381(6) . ? C10 C11 1.402(4) . ? C11 C12 1.473(5) . ? C12 C13 1.394(5) . ? C13 C14 1.370(6) . ? C14 C15 1.376(6) . ? C15 C16 1.378(5) . ? C17 C18 1.379(5) . ? C18 C19 1.374(5) . ? C19 C20 1.378(5) . ? C20 C21 1.393(5) . ? C21 C22 1.491(5) . ? C22 C23 1.391(5) . ? C23 C24 1.380(6) . ? C24 C25 1.376(6) . ? C25 C26 1.374(5) . ? C27 C28 1.370(6) . ? C28 C29 1.380(7) . ? C29 C30 1.367(6) . ? C30 C31 1.398(5) . ? C31 C31 1.481(8) 2_656 ? 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 Gd1 O1 145.36(8) . . ? O2 Gd1 O4 73.76(8) . . ? O1 Gd1 O4 135.88(7) . . ? O2 Gd1 O3 144.41(8) . . ? O1 Gd1 O3 70.21(8) . . ? O4 Gd1 O3 73.58(7) . . ? O2 Gd1 N4 101.90(9) . . ? O1 Gd1 N4 77.75(8) . . ? O4 Gd1 N4 72.66(8) . . ? O3 Gd1 N4 81.42(8) . . ? O2 Gd1 N1 80.20(9) . . ? O1 Gd1 N1 119.96(9) . . ? O4 Gd1 N1 74.64(8) . . ? O3 Gd1 N1 77.89(8) . . ? N4 Gd1 N1 145.06(9) . . ? O2 Gd1 N7 85.53(8) . . ? O1 Gd1 N7 73.32(8) . . ? O4 Gd1 N7 147.68(8) . . ? O3 Gd1 N7 116.27(8) . . ? N4 Gd1 N7 137.18(9) . . ? N1 Gd1 N7 77.63(9) . . ? O2 Gd1 N8 70.55(8) . . ? O1 Gd1 N8 75.53(8) . . ? O4 Gd1 N8 127.77(8) . . ? O3 Gd1 N8 143.29(8) . . ? N4 Gd1 N8 78.82(8) . . ? N1 Gd1 N8 132.54(9) . . ? N7 Gd1 N8 63.91(9) . . ? C3 Cr1 C2 90.91(13) . . ? C3 Cr1 C4 86.09(12) . . ? C2 Cr1 C4 90.05(13) . . ? C3 Cr1 C1 88.70(12) . . ? C2 Cr1 C1 89.74(13) . . ? C4 Cr1 C1 174.78(12) . . ? C3 Cr1 C5 87.61(13) . . ? C2 Cr1 C5 177.90(12) . . ? C4 Cr1 C5 88.36(12) . . ? C1 Cr1 C5 91.72(12) . . ? C3 Cr1 C6 179.17(13) . . ? C2 Cr1 C6 88.94(13) . . ? C4 Cr1 C6 93.09(12) . . ? C1 Cr1 C6 92.12(12) . . ? C5 Cr1 C6 92.52(12) . . ? C1 N1 Gd1 176.0(3) . . ? C4 N4 Gd1 165.0(2) 1_465 . ? C7 N7 C11 117.7(3) . . ? C7 N7 Gd1 121.0(2) . . ? C11 N7 Gd1 121.4(2) . . ? C16 N8 C12 117.9(3) . . ? C16 N8 Gd1 121.7(2) . . ? C12 N8 Gd1 120.4(2) . . ? C17 N9 C21 118.2(3) . . ? C22 N10 C26 117.5(3) . . ? C27 N11 C31 118.2(3) . . ? N1 C1 Cr1 174.8(3) . . ? N2 C2 Cr1 178.2(3) . . ? N3 C3 Cr1 177.6(3) . . ? N4 C4 Cr1 171.8(3) 1_645 . ? N5 C5 Cr1 176.0(3) . . ? N6 C6 Cr1 177.8(3) . . ? N7 C7 C8 123.5(3) . . ? C9 C8 C7 119.1(4) . . ? C8 C9 C10 118.9(3) . . ? C9 C10 C11 119.6(3) . . ? N7 C11 C10 121.3(3) . . ? N7 C11 C12 117.2(3) . . ? C10 C11 C12 121.5(3) . . ? N8 C12 C13 121.2(3) . . ? N8 C12 C11 117.0(3) . . ? C13 C12 C11 121.8(3) . . ? C14 C13 C12 119.7(4) . . ? C13 C14 C15 119.5(3) . . ? C14 C15 C16 118.0(4) . . ? N8 C16 C15 123.6(4) . . ? N9 C17 C18 123.4(3) . . ? C19 C18 C17 118.2(3) . . ? C18 C19 C20 119.6(3) . . ? C19 C20 C21 118.7(3) . . ? N9 C21 C20 121.8(3) . . ? N9 C21 C22 116.6(3) . . ? C20 C21 C22 121.5(3) . . ? N10 C22 C23 122.1(3) . . ? N10 C22 C21 116.4(3) . . ? C23 C22 C21 121.6(3) . . ? C24 C23 C22 119.0(4) . . ? C25 C24 C23 119.3(4) . . ? C26 C25 C24 117.9(4) . . ? N10 C26 C25 124.2(4) . . ? N11 C27 C28 123.8(4) . . ? C27 C28 C29 117.8(4) . . ? C30 C29 C28 119.9(4) . . ? C29 C30 C31 119.1(4) . . ? N11 C31 C30 121.1(4) . . ? N11 C31 C31 117.0(4) . 2_656 ? C30 C31 C31 122.0(4) . 2_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Gd1 N1 C1 -18(4) . . . . ? O1 Gd1 N1 C1 132(4) . . . . ? O4 Gd1 N1 C1 -94(4) . . . . ? O3 Gd1 N1 C1 -170(4) . . . . ? N4 Gd1 N1 C1 -115(4) . . . . ? N7 Gd1 N1 C1 70(4) . . . . ? N8 Gd1 N1 C1 34(4) . . . . ? O2 Gd1 N4 C4 90.7(10) . . . 1_465 ? O1 Gd1 N4 C4 -53.8(10) . . . 1_465 ? O4 Gd1 N4 C4 159.3(10) . . . 1_465 ? O3 Gd1 N4 C4 -125.3(10) . . . 1_465 ? N1 Gd1 N4 C4 -179.4(9) . . . 1_465 ? N7 Gd1 N4 C4 -5.6(11) . . . 1_465 ? N8 Gd1 N4 C4 23.6(10) . . . 1_465 ? O2 Gd1 N7 C7 108.9(2) . . . . ? O1 Gd1 N7 C7 -98.9(2) . . . . ? O4 Gd1 N7 C7 59.3(3) . . . . ? O3 Gd1 N7 C7 -41.7(3) . . . . ? N4 Gd1 N7 C7 -148.4(2) . . . . ? N1 Gd1 N7 C7 28.0(2) . . . . ? N8 Gd1 N7 C7 179.4(3) . . . . ? O2 Gd1 N7 C11 -72.2(2) . . . . ? O1 Gd1 N7 C11 80.0(2) . . . . ? O4 Gd1 N7 C11 -121.8(2) . . . . ? O3 Gd1 N7 C11 137.2(2) . . . . ? N4 Gd1 N7 C11 30.5(3) . . . . ? N1 Gd1 N7 C11 -153.1(2) . . . . ? N8 Gd1 N7 C11 -1.7(2) . . . . ? O2 Gd1 N8 C16 -83.3(3) . . . . ? O1 Gd1 N8 C16 103.8(3) . . . . ? O4 Gd1 N8 C16 -33.7(3) . . . . ? O3 Gd1 N8 C16 82.4(3) . . . . ? N4 Gd1 N8 C16 23.8(3) . . . . ? N1 Gd1 N8 C16 -138.6(2) . . . . ? N7 Gd1 N8 C16 -177.9(3) . . . . ? O2 Gd1 N8 C12 97.2(2) . . . . ? O1 Gd1 N8 C12 -75.7(2) . . . . ? O4 Gd1 N8 C12 146.8(2) . . . . ? O3 Gd1 N8 C12 -97.0(3) . . . . ? N4 Gd1 N8 C12 -155.7(3) . . . . ? N1 Gd1 N8 C12 41.9(3) . . . . ? N7 Gd1 N8 C12 2.6(2) . . . . ? Gd1 N1 C1 Cr1 -68(6) . . . . ? C3 Cr1 C1 N1 -15(3) . . . . ? C2 Cr1 C1 N1 76(3) . . . . ? C4 Cr1 C1 N1 -12(4) . . . . ? C5 Cr1 C1 N1 -103(3) . . . . ? C6 Cr1 C1 N1 165(3) . . . . ? C3 Cr1 C2 N2 114(11) . . . . ? C4 Cr1 C2 N2 -160(11) . . . . ? C1 Cr1 C2 N2 25(11) . . . . ? C5 Cr1 C2 N2 159(9) . . . . ? C6 Cr1 C2 N2 -67(11) . . . . ? C2 Cr1 C3 N3 117(8) . . . . ? C4 Cr1 C3 N3 27(8) . . . . ? C1 Cr1 C3 N3 -153(8) . . . . ? C5 Cr1 C3 N3 -61(8) . . . . ? C6 Cr1 C3 N3 38(15) . . . . ? C3 Cr1 C4 N4 5(2) . . . 1_645 ? C2 Cr1 C4 N4 -86(2) . . . 1_645 ? C1 Cr1 C4 N4 2(3) . . . 1_645 ? C5 Cr1 C4 N4 93(2) . . . 1_645 ? C6 Cr1 C4 N4 -175(2) . . . 1_645 ? C3 Cr1 C5 N5 41(4) . . . . ? C2 Cr1 C5 N5 -4(7) . . . . ? C4 Cr1 C5 N5 -45(4) . . . . ? C1 Cr1 C5 N5 129(4) . . . . ? C6 Cr1 C5 N5 -138(4) . . . . ? C3 Cr1 C6 N6 124(10) . . . . ? C2 Cr1 C6 N6 45(8) . . . . ? C4 Cr1 C6 N6 135(8) . . . . ? C1 Cr1 C6 N6 -45(8) . . . . ? C5 Cr1 C6 N6 -137(8) . . . . ? C11 N7 C7 C8 -0.1(5) . . . . ? Gd1 N7 C7 C8 178.9(3) . . . . ? N7 C7 C8 C9 0.1(6) . . . . ? C7 C8 C9 C10 0.0(6) . . . . ? C8 C9 C10 C11 -0.2(6) . . . . ? C7 N7 C11 C10 -0.1(5) . . . . ? Gd1 N7 C11 C10 -179.0(2) . . . . ? C7 N7 C11 C12 179.8(3) . . . . ? Gd1 N7 C11 C12 0.8(4) . . . . ? C9 C10 C11 N7 0.2(5) . . . . ? C9 C10 C11 C12 -179.6(3) . . . . ? C16 N8 C12 C13 -1.8(5) . . . . ? Gd1 N8 C12 C13 177.7(3) . . . . ? C16 N8 C12 C11 177.2(3) . . . . ? Gd1 N8 C12 C11 -3.3(4) . . . . ? N7 C11 C12 N8 1.6(4) . . . . ? C10 C11 C12 N8 -178.6(3) . . . . ? N7 C11 C12 C13 -179.3(3) . . . . ? C10 C11 C12 C13 0.5(5) . . . . ? N8 C12 C13 C14 0.7(6) . . . . ? C11 C12 C13 C14 -178.3(4) . . . . ? C12 C13 C14 C15 0.2(6) . . . . ? C13 C14 C15 C16 -0.1(6) . . . . ? C12 N8 C16 C15 2.1(5) . . . . ? Gd1 N8 C16 C15 -177.4(3) . . . . ? C14 C15 C16 N8 -1.1(6) . . . . ? C21 N9 C17 C18 0.2(5) . . . . ? N9 C17 C18 C19 -0.5(5) . . . . ? C17 C18 C19 C20 0.0(5) . . . . ? C18 C19 C20 C21 0.7(6) . . . . ? C17 N9 C21 C20 0.7(5) . . . . ? C17 N9 C21 C22 -177.9(3) . . . . ? C19 C20 C21 N9 -1.1(5) . . . . ? C19 C20 C21 C22 177.3(3) . . . . ? C26 N10 C22 C23 -2.8(5) . . . . ? C26 N10 C22 C21 176.6(3) . . . . ? N9 C21 C22 N10 -20.0(4) . . . . ? C20 C21 C22 N10 161.4(3) . . . . ? N9 C21 C22 C23 159.3(3) . . . . ? C20 C21 C22 C23 -19.2(5) . . . . ? N10 C22 C23 C24 1.6(6) . . . . ? C21 C22 C23 C24 -177.7(4) . . . . ? C22 C23 C24 C25 0.9(6) . . . . ? C23 C24 C25 C26 -2.0(6) . . . . ? C22 N10 C26 C25 1.5(6) . . . . ? C24 C25 C26 N10 0.9(6) . . . . ? C31 N11 C27 C28 0.8(6) . . . . ? N11 C27 C28 C29 2.2(6) . . . . ? C27 C28 C29 C30 -2.4(6) . . . . ? C28 C29 C30 C31 -0.3(6) . . . . ? C27 N11 C31 C30 -3.6(5) . . . . ? C27 N11 C31 C31 176.3(4) . . . 2_656 ? C29 C30 C31 N11 3.4(6) . . . . ? C29 C30 C31 C31 -176.6(4) . . . 2_656 ? 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 O1 H1A O5 0.85 2.01 2.808(3) 155.7 . O1 H1B N6 0.85 1.95 2.787(4) 166.1 1_565 O2 H2A O8 0.85 1.74 2.579(6) 171.4 . O2 H2A O8' 0.85 2.01 2.795(6) 153.3 . O2 H2B N11 0.85 1.94 2.789(4) 172.1 . O3 H3A O5 0.85 1.98 2.783(3) 156.0 . O3 H3B N9 0.85 1.95 2.768(3) 161.9 1_455 O4 H4A N10 0.85 2.02 2.869(4) 178.2 1_455 O4 H4B O6 0.85 1.89 2.729(3) 168.2 . O5 H5A N5 0.85 1.96 2.801(4) 169.6 2_655 O5 H5B N5 0.85 2.35 3.205(4) 179.1 1_465 O6 H6A N6 0.85 2.29 3.130(4) 172.6 . O6 H6B N3 0.85 1.92 2.743(4) 162.3 1_455 O7 H7B N2 0.85 2.17 2.853(6) 136.8 2_646 O8 H8A O7' 0.85 2.02 2.507(11) 115.4 . O8 H8B O6 0.85 2.10 2.779(6) 136.5 . O7' H7A' N2 0.85 2.16 3.003(11) 171.9 2_646 O7' H7B' O8' 0.85 2.27 2.866(12) 126.9 . O8' H8C' O7' 0.85 2.02 2.866(12) 175.4 . O8' H8D' O6 0.85 1.93 2.725(7) 155.8 . _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 2.159 _refine_diff_density_min -3.427 _refine_diff_density_rms 0.125