Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email M.SCHRODER@NOTTINGHAM.AC.UK _publ_contact_author_name 'Prof M Schroder' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name M.Schroder A.J.Blake M.W.George L.Tei J.A.Weinstein C.Wilson data_GDN3CB _database_code_CSD 193873 _refine_special_details ; Disordered solvents modelled as two waters, one with 0.5 and one with 0.25 occupancy; half a MeOH with the C atom modelled over two sites (occupancies 0.3 and 0.2) with a 0.25 occupancy MeOH in the same region. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.75 H45.5 Gd N6 O9.50' _chemical_formula_weight 724.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 28.0190(12) _cell_length_b 28.0190(12) _cell_length_c 23.1774(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 15758.0(13) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6625 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 27.14 _exptl_crystal_description Column _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6642 _exptl_absorpt_coefficient_mu 1.945 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.657 _exptl_absorpt_correction_T_max 0.813 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '1% variation, not corrected' _diffrn_reflns_number 33270 _diffrn_reflns_av_R_equivalents 0.090 _diffrn_reflns_av_sigmaI/netI 0.093 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.81 _reflns_number_total 8374 _reflns_number_gt 5400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0656P)^2^+48.18P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier map' _atom_sites_solution_hydrogens 'placed geometrically, MeOH from delta-F' _refine_ls_hydrogen_treatment 'riding model, rigid rotating group for MeOH' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8371 _refine_ls_number_parameters 367 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1058 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 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 0.010578(12) 0.718700(13) 0.642702(13) 0.02052(10) Uani 1 1 d . . . N1 N -0.0252(2) 0.7198(2) 0.5363(2) 0.0252(12) Uani 1 1 d . . . C1C C 0.0391(3) 0.8500(3) 0.6495(3) 0.0286(15) Uani 1 1 d . . . H1C1 H 0.0531 0.8886 0.6373 0.034 Uiso 1 1 calc R . . H1C2 H 0.0610 0.8504 0.6832 0.034 Uiso 1 1 calc R . . C1A C -0.0780(3) 0.6673(3) 0.5315(3) 0.0265(14) Uani 1 1 d . . . H1A1 H -0.0944 0.6652 0.4931 0.032 Uiso 1 1 calc R . . H1A2 H -0.1039 0.6664 0.5611 0.032 Uiso 1 1 calc R . . C1B C 0.1242(3) 0.7287(3) 0.5828(3) 0.0287(15) Uani 1 1 d . . . H1B1 H 0.1526 0.7364 0.5533 0.034 Uiso 1 1 calc R . . H1B2 H 0.1033 0.6884 0.5895 0.034 Uiso 1 1 calc R . . C2 C 0.0131(3) 0.7246(3) 0.4887(3) 0.0271(14) Uani 1 1 d . . . H2A H -0.0083 0.6975 0.4582 0.033 Uiso 1 1 calc R . . H2B H 0.0296 0.7619 0.4715 0.033 Uiso 1 1 calc R . . C2C C -0.0205(3) 0.8247(3) 0.6668(3) 0.0309(15) Uani 1 1 d . . . H2C1 H -0.0232 0.8405 0.7041 0.037 Uiso 1 1 calc R . . H2C2 H -0.0408 0.8332 0.6374 0.037 Uiso 1 1 calc R . . C2A C -0.0702(3) 0.6187(3) 0.5394(3) 0.0297(15) Uani 1 1 d . . . H2A1 H -0.1066 0.5848 0.5434 0.036 Uiso 1 1 calc R . . H2A2 H -0.0516 0.6144 0.5051 0.036 Uiso 1 1 calc R . . C2B C 0.1519(3) 0.7576(3) 0.6383(3) 0.0314(16) Uani 1 1 d . . . H2B1 H 0.1692 0.7383 0.6571 0.038 Uiso 1 1 calc R . . H2B2 H 0.1811 0.7959 0.6301 0.038 Uiso 1 1 calc R . . N3C N -0.0452(2) 0.7649(2) 0.6725(2) 0.0228(11) Uani 1 1 d . . . N3B N 0.1104(2) 0.7576(2) 0.6765(2) 0.0269(12) Uani 1 1 d . . . N3A N -0.0372(2) 0.6257(2) 0.5905(2) 0.0251(12) Uani 1 1 d . . . C3 C 0.0583(3) 0.7149(3) 0.5088(3) 0.0266(14) Uani 1 1 d . . . H3A H 0.0427 0.6752 0.5171 0.032 Uiso 1 1 calc R . . H3B H 0.0857 0.7250 0.4776 0.032 Uiso 1 1 calc R . . N4 N 0.0862(2) 0.7469(2) 0.5611(2) 0.0253(12) Uani 1 1 d . . . C4A C -0.0361(3) 0.5846(3) 0.6134(3) 0.0291(15) Uani 1 1 d . . . C4C C -0.0895(3) 0.7367(3) 0.7010(3) 0.0246(14) Uani 1 1 d . . . C4B C 0.1220(3) 0.7703(3) 0.7294(3) 0.0275(15) Uani 1 1 d . . . C5C C -0.1098(3) 0.6749(3) 0.7041(3) 0.0242(14) Uani 1 1 d . . . C5B C 0.0752(3) 0.7680(3) 0.7653(3) 0.0288(15) Uani 1 1 d . . . C5A C -0.0016(3) 0.5980(3) 0.6680(3) 0.0305(15) Uani 1 1 d . . . C5 C -0.0352(3) 0.7668(3) 0.5358(3) 0.0308(15) Uani 1 1 d . . . H5A H -0.0636 0.7605 0.5650 0.037 Uiso 1 1 calc R . . H5B H -0.0496 0.7691 0.4975 0.037 Uiso 1 1 calc R . . O6A O 0.02469(19) 0.64880(19) 0.6829(2) 0.0319(11) Uani 1 1 d . . . O6C O -0.07951(17) 0.65906(17) 0.68018(19) 0.0262(10) Uani 1 1 d . . . O6B O 0.03100(19) 0.7541(2) 0.73832(18) 0.0325(11) Uani 1 1 d . . . C6 C 0.0173(3) 0.8216(3) 0.5487(3) 0.0325(16) Uani 1 1 d . . . H6A H 0.0427 0.8318 0.5154 0.039 Uiso 1 1 calc R . . H6B H 0.0076 0.8508 0.5538 0.039 Uiso 1 1 calc R . . O7C O -0.15409(17) 0.64487(18) 0.72928(19) 0.0286(10) Uani 1 1 d . . . N7 N 0.0460(2) 0.8188(2) 0.6014(2) 0.0261(12) Uani 1 1 d . . . O7A O -0.0009(3) 0.5605(2) 0.6939(2) 0.0561(16) Uani 1 1 d . . . O7B O 0.0837(2) 0.7804(2) 0.8170(2) 0.0480(15) Uani 1 1 d . . . C8 C 0.1057(3) 0.8419(3) 0.5898(3) 0.0317(16) Uani 1 1 d . . . H8A H 0.1249 0.8445 0.6265 0.038 Uiso 1 1 calc R . . H8B H 0.1212 0.8796 0.5740 0.038 Uiso 1 1 calc R . . C8A C -0.0663(3) 0.5273(3) 0.5928(3) 0.0426(19) Uani 1 1 d . . . H8A1 H -0.1054 0.5155 0.5889 0.064 Uiso 1 1 calc R . . H8A2 H -0.0618 0.5034 0.6205 0.064 Uiso 1 1 calc R . . H8A3 H -0.0516 0.5248 0.5553 0.064 Uiso 1 1 calc R . . C8B C 0.1757(3) 0.7865(4) 0.7580(3) 0.044(2) Uani 1 1 d . . . H8B1 H 0.1762 0.7533 0.7705 0.066 Uiso 1 1 calc R . . H8B2 H 0.1804 0.8097 0.7915 0.066 Uiso 1 1 calc R . . H8B3 H 0.2059 0.8070 0.7306 0.066 Uiso 1 1 calc R . . C8C C -0.1221(3) 0.7573(3) 0.7327(3) 0.0354(17) Uani 1 1 d . . . H8C1 H -0.1026 0.7977 0.7313 0.053 Uiso 1 1 calc R . . H8C2 H -0.1267 0.7452 0.7730 0.053 Uiso 1 1 calc R . . H8C3 H -0.1584 0.7426 0.7146 0.053 Uiso 1 1 calc R . . C9 C 0.1167(3) 0.8071(3) 0.5476(3) 0.0304(15) Uani 1 1 d . . . H9A H 0.1063 0.8127 0.5084 0.036 Uiso 1 1 calc R . . H9B H 0.1567 0.8202 0.5473 0.036 Uiso 1 1 calc R . . O1M O -0.1922(2) 0.5364(2) 0.7426(2) 0.0451(13) Uani 1 1 d D . . C1M C -0.1645(4) 0.5161(4) 0.7137(4) 0.063(3) Uani 1 1 d D . . H1M1 H -0.1269 0.5458 0.7058 0.095 Uiso 1 1 calc R . . H1M2 H -0.1834 0.4999 0.6772 0.095 Uiso 1 1 calc R . . H1M3 H -0.1631 0.4876 0.7371 0.095 Uiso 1 1 calc R . . C2M C 0.0346(5) 0.8577(5) 0.8402(5) 0.100(4) Uiso 1 1 d D . . H2M1 H 0.0174 0.8730 0.8652 0.150 Uiso 1 1 calc R . . H2M2 H 0.0646 0.8874 0.8182 0.150 Uiso 1 1 calc R . . H2M3 H 0.0495 0.8391 0.8639 0.150 Uiso 1 1 calc R . . O2M O -0.0026(5) 0.8219(5) 0.8043(5) 0.134(4) Uiso 1 1 d D . . H2M H -0.0298 0.8267 0.8031 0.200 Uiso 1 1 calc R . . O1W O -0.0586(6) 0.8911(6) 0.5310(6) 0.080(4) Uiso 0.50 1 d P . . O2W O 0.3081(14) 0.7986(14) 0.7124(14) 0.097(10) Uiso 0.25 1 d P . . O3M O 0.3186(7) 0.8713(8) 0.5864(9) 0.116(6) Uiso 0.50 1 d PD . . C3M C 0.2685(8) 0.8406(10) 0.5651(11) 0.037(6) Uiso 0.30 1 d PD A 1 C3M' C 0.2902(14) 0.8173(8) 0.5934(18) 0.029(8) Uiso 0.20 1 d PD A 2 O4M O 0.3067(12) 0.8425(14) 0.6202(11) 0.076(8) Uiso 0.25 1 d PD A 3 C4M C 0.2845(12) 0.8292(12) 0.5684(11) 0.030(6) Uiso 0.25 1 d PD A 3 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 0.01800(17) 0.02054(17) 0.01866(15) 0.00181(12) -0.00091(12) 0.00634(14) N1 0.028(3) 0.027(3) 0.021(3) 0.000(2) -0.004(2) 0.015(3) C1C 0.030(4) 0.020(3) 0.024(3) 0.000(3) 0.002(3) 0.004(3) C1A 0.023(3) 0.028(4) 0.024(3) -0.001(3) -0.004(3) 0.009(3) C1B 0.026(4) 0.033(4) 0.027(4) 0.001(3) 0.002(3) 0.015(3) C2 0.029(4) 0.027(4) 0.020(3) 0.000(3) 0.001(3) 0.011(3) C2C 0.039(4) 0.024(3) 0.032(4) 0.002(3) 0.001(3) 0.018(3) C2A 0.024(3) 0.028(4) 0.032(4) -0.006(3) -0.004(3) 0.010(3) C2B 0.016(3) 0.035(4) 0.034(4) 0.000(3) 0.000(3) 0.006(3) N3C 0.020(3) 0.021(3) 0.021(3) -0.001(2) -0.004(2) 0.006(2) N3B 0.024(3) 0.028(3) 0.025(3) 0.001(2) -0.003(2) 0.009(2) N3A 0.018(3) 0.024(3) 0.030(3) -0.003(2) 0.000(2) 0.007(2) C3 0.023(3) 0.026(3) 0.026(3) 0.000(3) 0.004(3) 0.009(3) N4 0.024(3) 0.024(3) 0.023(3) -0.002(2) -0.001(2) 0.008(2) C4A 0.030(4) 0.027(4) 0.028(4) 0.001(3) 0.005(3) 0.013(3) C4C 0.022(3) 0.031(4) 0.022(3) -0.004(3) -0.004(3) 0.013(3) C4B 0.023(3) 0.025(3) 0.027(4) 0.001(3) -0.004(3) 0.006(3) C5C 0.021(3) 0.028(3) 0.019(3) 0.001(3) -0.004(2) 0.008(3) C5B 0.028(4) 0.026(4) 0.022(3) 0.000(3) -0.005(3) 0.006(3) C5A 0.034(4) 0.030(4) 0.034(4) 0.007(3) 0.008(3) 0.021(3) C5 0.036(4) 0.038(4) 0.023(3) 0.000(3) -0.004(3) 0.022(3) O6A 0.029(3) 0.032(3) 0.034(3) 0.007(2) -0.007(2) 0.014(2) O6C 0.023(2) 0.023(2) 0.030(2) -0.0003(19) 0.0021(19) 0.010(2) O6B 0.031(3) 0.044(3) 0.019(2) 0.002(2) -0.0013(19) 0.016(2) C6 0.042(4) 0.030(4) 0.027(4) 0.006(3) 0.000(3) 0.019(3) O7C 0.019(2) 0.032(3) 0.029(2) 0.003(2) 0.0037(19) 0.008(2) N7 0.029(3) 0.019(3) 0.020(3) 0.004(2) 0.002(2) 0.004(2) O7A 0.085(5) 0.040(3) 0.055(4) 0.007(3) -0.007(3) 0.040(3) O7B 0.032(3) 0.070(4) 0.026(3) -0.012(3) -0.004(2) 0.013(3) C8 0.029(4) 0.022(3) 0.030(4) 0.004(3) 0.008(3) 0.002(3) C8A 0.056(5) 0.025(4) 0.041(4) 0.005(3) 0.008(4) 0.016(4) C8B 0.027(4) 0.061(5) 0.039(4) -0.011(4) -0.014(3) 0.018(4) C8C 0.030(4) 0.031(4) 0.042(4) -0.003(3) 0.005(3) 0.013(3) C9 0.026(4) 0.028(4) 0.027(4) 0.004(3) 0.006(3) 0.006(3) O1M 0.049(3) 0.041(3) 0.049(3) 0.001(3) -0.008(3) 0.025(3) C1M 0.086(7) 0.053(6) 0.061(6) -0.013(5) -0.030(5) 0.042(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N1 2.668(5) . y Gd1 N4 2.648(5) . y Gd1 N7 2.641(5) . y Gd1 N3A 2.561(5) . y Gd1 N3B 2.565(5) . y Gd1 N3C 2.574(5) . y Gd1 O6A 2.373(4) . y Gd1 O6B 2.378(4) . y Gd1 O6C 2.388(4) . y N1 C5 1.477(8) . ? N1 C1A 1.478(8) . ? N1 C2 1.497(8) . ? C1C N7 1.490(8) . ? C1C C2C 1.506(9) . ? C1A C2A 1.496(9) . ? C1B N4 1.480(8) . ? C1B C2B 1.512(9) . ? C2 C3 1.496(9) . ? C2C N3C 1.463(8) . ? C2A N3A 1.453(8) . ? C2B N3B 1.460(8) . ? N3C C4C 1.274(8) . ? N3B C4B 1.274(8) . ? N3A C4A 1.283(8) . ? C3 N4 1.478(8) . ? N4 C9 1.494(8) . ? C4A C8A 1.471(9) . ? C4A C5A 1.520(10) . ? C4C C8C 1.495(9) . ? C4C C5C 1.532(9) . ? C4B C8B 1.493(9) . ? C4B C5B 1.524(10) . ? C5C O7C 1.243(7) . ? C5C O6C 1.264(7) . ? C5B O7B 1.236(8) . ? C5B O6B 1.264(8) . ? C5A O7A 1.218(8) . ? C5A O6A 1.281(8) . ? C5 C6 1.534(10) . ? C6 N7 1.486(8) . ? N7 C8 1.486(8) . ? C8 C9 1.515(9) . ? O1M C1M 1.350(8) . ? C2M O2M 1.319(9) . ? O3M O4M 1.05(3) . ? O3M C4M 1.16(3) . ? O3M C3M' 1.321(11) . ? O3M C3M 1.322(11) . ? O4M C4M 1.318(11) . ? 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 N4 Gd1 N1 65.51(16) . . y N7 Gd1 N1 66.25(16) . . y N7 Gd1 N4 66.67(17) . . y N3A Gd1 N1 64.30(17) . . y N3B Gd1 N1 127.83(17) . . y N3C Gd1 N1 85.17(16) . . y O6A Gd1 N1 126.18(16) . . y O6B Gd1 N1 150.50(16) . . y O6C Gd1 N1 94.16(16) . . y N3A Gd1 N4 84.25(16) . . y N3B Gd1 N4 63.33(16) . . y N3C Gd1 N4 129.60(16) . . y O6A Gd1 N4 95.06(17) . . y O6B Gd1 N4 123.44(16) . . y O6C Gd1 N4 151.26(15) . . y N3A Gd1 N7 129.53(17) . . y N3B Gd1 N7 84.74(17) . . y N3C Gd1 N7 64.13(16) . . y O6A Gd1 N7 152.68(17) . . y O6B Gd1 N7 90.62(16) . . y O6C Gd1 N7 125.43(16) . . y N3A Gd1 N3C 119.90(16) . . y N3A Gd1 N3B 118.72(17) . . y N3B Gd1 N3C 120.86(16) . . y O6A Gd1 N3A 64.14(17) . . y O6B Gd1 N3A 139.38(17) . . y O6C Gd1 N3A 68.15(15) . . y O6A Gd1 N3B 68.54(16) . . y O6B Gd1 N3B 63.55(16) . . y O6C Gd1 N3B 137.15(16) . . y O6A Gd1 N3C 134.76(17) . . y O6B Gd1 N3C 67.71(16) . . y O6C Gd1 N3C 63.83(15) . . y O6A Gd1 O6B 82.75(17) . . y O6A Gd1 O6C 80.43(16) . . y O6B Gd1 O6C 84.40(15) . . y C5 N1 C1A 110.2(5) . . ? C5 N1 C2 111.2(5) . . ? C1A N1 C2 110.5(5) . . ? C5 N1 Gd1 104.9(4) . . ? C1A N1 Gd1 104.6(4) . . ? C2 N1 Gd1 115.2(4) . . ? N7 C1C C2C 111.2(5) . . ? N1 C1A C2A 111.6(5) . . ? N4 C1B C2B 111.8(5) . . ? C3 C2 N1 112.8(5) . . ? N3C C2C C1C 110.0(5) . . ? N3A C2A C1A 110.4(5) . . ? N3B C2B C1B 108.6(5) . . ? C4C N3C C2C 120.9(6) . . ? C4C N3C Gd1 118.4(4) . . ? C2C N3C Gd1 119.5(4) . . ? C4B N3B C2B 119.5(6) . . ? C4B N3B Gd1 118.9(4) . . ? C2B N3B Gd1 121.0(4) . . ? C4A N3A C2A 121.0(6) . . ? C4A N3A Gd1 118.8(4) . . ? C2A N3A Gd1 119.8(4) . . ? N4 C3 C2 112.6(5) . . ? C3 N4 C1B 108.8(5) . . ? C3 N4 C9 110.1(5) . . ? C1B N4 C9 110.9(5) . . ? C3 N4 Gd1 107.6(4) . . ? C1B N4 Gd1 105.1(4) . . ? C9 N4 Gd1 114.1(4) . . ? N3A C4A C8A 125.9(7) . . ? N3A C4A C5A 114.9(6) . . ? C8A C4A C5A 119.1(6) . . ? N3C C4C C8C 127.6(6) . . ? N3C C4C C5C 114.9(6) . . ? C8C C4C C5C 117.5(6) . . ? N3B C4B C8B 126.0(6) . . ? N3B C4B C5B 114.9(6) . . ? C8B C4B C5B 119.1(6) . . ? O7C C5C O6C 125.9(6) . . ? O7C C5C C4C 117.8(6) . . ? O6C C5C C4C 116.2(5) . . ? O7B C5B O6B 125.9(7) . . ? O7B C5B C4B 118.5(6) . . ? O6B C5B C4B 115.6(5) . . ? O7A C5A O6A 125.3(7) . . ? O7A C5A C4A 118.7(7) . . ? O6A C5A C4A 116.0(6) . . ? N1 C5 C6 112.1(5) . . ? C5A O6A Gd1 124.9(4) . . ? C5C O6C Gd1 125.0(4) . . ? C5B O6B Gd1 125.7(4) . . ? N7 C6 C5 112.4(5) . . ? C8 N7 C6 110.4(5) . . ? C8 N7 C1C 109.3(5) . . ? C6 N7 C1C 110.4(5) . . ? C8 N7 Gd1 105.8(4) . . ? C6 N7 Gd1 115.4(4) . . ? C1C N7 Gd1 105.3(3) . . ? N7 C8 C9 112.5(5) . . ? N4 C9 C8 113.8(5) . . ? O4M O3M C4M 72.8(16) . . ? O4M O3M C3M' 41.5(18) . . ? C4M O3M C3M' 33.2(17) . . ? O4M O3M C3M 87(2) . . ? C4M O3M C3M 30.6(17) . . ? C3M' O3M C3M 58(2) . . ? O3M O4M C4M 57.5(19) . . ? O3M C4M O4M 49.7(16) . . ? 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 O6A Gd1 N1 C5 171.4(4) . . . . ? O6B Gd1 N1 C5 4.2(6) . . . . ? O6C Gd1 N1 C5 90.2(4) . . . . ? N3A Gd1 N1 C5 153.5(4) . . . . ? N3B Gd1 N1 C5 -99.0(4) . . . . ? N3C Gd1 N1 C5 26.9(4) . . . . ? N7 Gd1 N1 C5 -36.9(4) . . . . ? N4 Gd1 N1 C5 -111.0(4) . . . . ? O6A Gd1 N1 C1A 55.4(4) . . . . ? O6B Gd1 N1 C1A -111.8(4) . . . . ? O6C Gd1 N1 C1A -25.8(4) . . . . ? N3A Gd1 N1 C1A 37.5(4) . . . . ? N3B Gd1 N1 C1A 145.1(4) . . . . ? N3C Gd1 N1 C1A -89.1(4) . . . . ? N7 Gd1 N1 C1A -152.9(4) . . . . ? N4 Gd1 N1 C1A 133.1(4) . . . . ? O6A Gd1 N1 C2 -66.1(4) . . . . ? O6B Gd1 N1 C2 126.7(4) . . . . ? O6C Gd1 N1 C2 -147.3(4) . . . . ? N3A Gd1 N1 C2 -84.0(4) . . . . ? N3B Gd1 N1 C2 23.6(5) . . . . ? N3C Gd1 N1 C2 149.4(4) . . . . ? N7 Gd1 N1 C2 85.6(4) . . . . ? N4 Gd1 N1 C2 11.6(4) . . . . ? C5 N1 C1A C2A -172.7(5) . . . . ? C2 N1 C1A C2A 64.0(7) . . . . ? Gd1 N1 C1A C2A -60.5(6) . . . . ? C5 N1 C2 C3 132.3(6) . . . . ? C1A N1 C2 C3 -105.0(6) . . . . ? Gd1 N1 C2 C3 13.2(6) . . . . ? N7 C1C C2C N3C 46.3(7) . . . . ? N1 C1A C2A N3A 48.6(7) . . . . ? N4 C1B C2B N3B 45.1(7) . . . . ? C1C C2C N3C C4C 160.9(6) . . . . ? C1C C2C N3C Gd1 -6.5(7) . . . . ? O6A Gd1 N3C C4C -30.5(5) . . . . ? O6B Gd1 N3C C4C -83.7(5) . . . . ? O6C Gd1 N3C C4C 11.1(4) . . . . ? N3A Gd1 N3C C4C 51.6(5) . . . . ? N3B Gd1 N3C C4C -120.1(4) . . . . ? N7 Gd1 N3C C4C 174.0(5) . . . . ? N4 Gd1 N3C C4C 160.6(4) . . . . ? N1 Gd1 N3C C4C 108.1(5) . . . . ? O6A Gd1 N3C C2C 137.2(4) . . . . ? O6B Gd1 N3C C2C 84.0(4) . . . . ? O6C Gd1 N3C C2C 178.8(5) . . . . ? N3A Gd1 N3C C2C -140.7(4) . . . . ? N3B Gd1 N3C C2C 47.6(5) . . . . ? N7 Gd1 N3C C2C -18.3(4) . . . . ? N4 Gd1 N3C C2C -31.7(5) . . . . ? N1 Gd1 N3C C2C -84.2(4) . . . . ? C1B C2B N3B C4B 166.9(6) . . . . ? C1B C2B N3B Gd1 -3.9(7) . . . . ? O6A Gd1 N3B C4B -83.4(5) . . . . ? O6B Gd1 N3B C4B 9.1(5) . . . . ? O6C Gd1 N3B C4B -36.7(6) . . . . ? N3A Gd1 N3B C4B -124.8(5) . . . . ? N3C Gd1 N3B C4B 46.9(5) . . . . ? N7 Gd1 N3B C4B 102.4(5) . . . . ? N4 Gd1 N3B C4B 168.9(5) . . . . ? N1 Gd1 N3B C4B 156.7(5) . . . . ? O6A Gd1 N3B C2B 87.5(5) . . . . ? O6B Gd1 N3B C2B -180.0(5) . . . . ? O6C Gd1 N3B C2B 134.2(4) . . . . ? N3A Gd1 N3B C2B 46.1(5) . . . . ? N3C Gd1 N3B C2B -142.2(5) . . . . ? N7 Gd1 N3B C2B -86.7(5) . . . . ? N4 Gd1 N3B C2B -20.2(5) . . . . ? N1 Gd1 N3B C2B -32.4(6) . . . . ? C1A C2A N3A C4A 163.3(6) . . . . ? C1A C2A N3A Gd1 -9.5(7) . . . . ? O6A Gd1 N3A C4A 7.4(5) . . . . ? O6B Gd1 N3A C4A -31.3(6) . . . . ? O6C Gd1 N3A C4A -82.4(5) . . . . ? N3B Gd1 N3A C4A 50.5(5) . . . . ? N3C Gd1 N3A C4A -121.2(5) . . . . ? N7 Gd1 N3A C4A 159.0(4) . . . . ? N4 Gd1 N3A C4A 105.8(5) . . . . ? N1 Gd1 N3A C4A 171.4(5) . . . . ? O6A Gd1 N3A C2A -179.7(5) . . . . ? O6B Gd1 N3A C2A 141.6(4) . . . . ? O6C Gd1 N3A C2A 90.6(5) . . . . ? N3B Gd1 N3A C2A -136.5(4) . . . . ? N3C Gd1 N3A C2A 51.7(5) . . . . ? N7 Gd1 N3A C2A -28.0(5) . . . . ? N4 Gd1 N3A C2A -81.2(5) . . . . ? N1 Gd1 N3A C2A -15.7(4) . . . . ? N1 C2 C3 N4 -48.8(7) . . . . ? C2 C3 N4 C1B 171.7(5) . . . . ? C2 C3 N4 C9 -66.7(7) . . . . ? C2 C3 N4 Gd1 58.3(6) . . . . ? C2B C1B N4 C3 -176.9(5) . . . . ? C2B C1B N4 C9 61.9(7) . . . . ? C2B C1B N4 Gd1 -61.8(5) . . . . ? O6A Gd1 N4 C3 93.0(4) . . . . ? O6B Gd1 N4 C3 177.6(4) . . . . ? O6C Gd1 N4 C3 13.7(6) . . . . ? N3A Gd1 N4 C3 29.6(4) . . . . ? N3B Gd1 N4 C3 155.9(4) . . . . ? N3C Gd1 N4 C3 -94.9(4) . . . . ? N7 Gd1 N4 C3 -108.1(4) . . . . ? N1 Gd1 N4 C3 -34.7(4) . . . . ? O6A Gd1 N4 C1B -22.9(4) . . . . ? O6B Gd1 N4 C1B 61.8(4) . . . . ? O6C Gd1 N4 C1B -102.2(4) . . . . ? N3A Gd1 N4 C1B -86.2(4) . . . . ? N3B Gd1 N4 C1B 40.1(4) . . . . ? N3C Gd1 N4 C1B 149.3(3) . . . . ? N7 Gd1 N4 C1B 136.1(4) . . . . ? N1 Gd1 N4 C1B -150.5(4) . . . . ? O6A Gd1 N4 C9 -144.5(4) . . . . ? O6B Gd1 N4 C9 -59.9(5) . . . . ? O6C Gd1 N4 C9 136.2(4) . . . . ? N3A Gd1 N4 C9 152.2(4) . . . . ? N3B Gd1 N4 C9 -81.6(4) . . . . ? N3C Gd1 N4 C9 27.6(5) . . . . ? N7 Gd1 N4 C9 14.4(4) . . . . ? N1 Gd1 N4 C9 87.8(4) . . . . ? C2A N3A C4A C8A 0.0(10) . . . . ? Gd1 N3A C4A C8A 172.9(5) . . . . ? C2A N3A C4A C5A -177.7(6) . . . . ? Gd1 N3A C4A C5A -4.8(7) . . . . ? C2C N3C C4C C8C -0.9(10) . . . . ? Gd1 N3C C4C C8C 166.7(5) . . . . ? C2C N3C C4C C5C -178.8(5) . . . . ? Gd1 N3C C4C C5C -11.3(7) . . . . ? C2B N3B C4B C8B 0.6(10) . . . . ? Gd1 N3B C4B C8B 171.7(6) . . . . ? C2B N3B C4B C5B -179.1(6) . . . . ? Gd1 N3B C4B C5B -8.1(8) . . . . ? N3C C4C C5C O7C -176.9(6) . . . . ? C8C C4C C5C O7C 5.0(9) . . . . ? N3C C4C C5C O6C 2.7(8) . . . . ? C8C C4C C5C O6C -175.5(6) . . . . ? N3B C4B C5B O7B -179.2(6) . . . . ? C8B C4B C5B O7B 1.1(10) . . . . ? N3B C4B C5B O6B -0.4(9) . . . . ? C8B C4B C5B O6B 179.9(6) . . . . ? N3A C4A C5A O7A 176.2(7) . . . . ? C8A C4A C5A O7A -1.7(10) . . . . ? N3A C4A C5A O6A -3.8(9) . . . . ? C8A C4A C5A O6A 178.4(6) . . . . ? C1A N1 C5 C6 172.4(5) . . . . ? C2 N1 C5 C6 -64.8(7) . . . . ? Gd1 N1 C5 C6 60.3(6) . . . . ? O7A C5A O6A Gd1 -168.1(6) . . . . ? C4A C5A O6A Gd1 11.8(8) . . . . ? O6B Gd1 O6A C5A 145.6(5) . . . . ? O6C Gd1 O6A C5A 60.0(5) . . . . ? N3A Gd1 O6A C5A -10.2(5) . . . . ? N3B Gd1 O6A C5A -150.1(6) . . . . ? N3C Gd1 O6A C5A 97.2(5) . . . . ? N7 Gd1 O6A C5A -137.3(5) . . . . ? N4 Gd1 O6A C5A -91.3(5) . . . . ? N1 Gd1 O6A C5A -28.1(6) . . . . ? O7C C5C O6C Gd1 -171.9(5) . . . . ? C4C C5C O6C Gd1 8.6(7) . . . . ? O6A Gd1 O6C C5C 141.3(5) . . . . ? O6B Gd1 O6C C5C 57.7(5) . . . . ? N3A Gd1 O6C C5C -152.9(5) . . . . ? N3B Gd1 O6C C5C 97.9(5) . . . . ? N3C Gd1 O6C C5C -10.2(4) . . . . ? N7 Gd1 O6C C5C -29.1(5) . . . . ? N4 Gd1 O6C C5C -135.7(5) . . . . ? N1 Gd1 O6C C5C -92.7(5) . . . . ? O7B C5B O6B Gd1 -171.3(5) . . . . ? C4B C5B O6B Gd1 10.0(8) . . . . ? O6A Gd1 O6B C5B 59.5(5) . . . . ? O6C Gd1 O6B C5B 140.5(5) . . . . ? N3A Gd1 O6B C5B 94.1(6) . . . . ? N3B Gd1 O6B C5B -10.1(5) . . . . ? N3C Gd1 O6B C5B -155.5(6) . . . . ? N7 Gd1 O6B C5B -93.9(5) . . . . ? N4 Gd1 O6B C5B -31.8(6) . . . . ? N1 Gd1 O6B C5B -130.9(5) . . . . ? N1 C5 C6 N7 -50.4(8) . . . . ? C5 C6 N7 C8 131.6(6) . . . . ? C5 C6 N7 C1C -107.5(6) . . . . ? C5 C6 N7 Gd1 11.7(7) . . . . ? C2C C1C N7 C8 -174.5(5) . . . . ? C2C C1C N7 C6 63.9(7) . . . . ? C2C C1C N7 Gd1 -61.2(6) . . . . ? O6A Gd1 N7 C8 14.8(6) . . . . ? O6B Gd1 N7 C8 90.1(4) . . . . ? O6C Gd1 N7 C8 173.6(3) . . . . ? N3A Gd1 N7 C8 -96.7(4) . . . . ? N3B Gd1 N7 C8 26.7(4) . . . . ? N3C Gd1 N7 C8 154.8(4) . . . . ? N4 Gd1 N7 C8 -36.5(4) . . . . ? N1 Gd1 N7 C8 -108.8(4) . . . . ? O6A Gd1 N7 C6 137.1(5) . . . . ? O6B Gd1 N7 C6 -147.6(4) . . . . ? O6C Gd1 N7 C6 -64.0(5) . . . . ? N3A Gd1 N7 C6 25.7(5) . . . . ? N3B Gd1 N7 C6 149.1(5) . . . . ? N3C Gd1 N7 C6 -82.8(4) . . . . ? N4 Gd1 N7 C6 85.9(4) . . . . ? N1 Gd1 N7 C6 13.5(4) . . . . ? O6A Gd1 N7 C1C -100.9(5) . . . . ? O6B Gd1 N7 C1C -25.6(4) . . . . ? O6C Gd1 N7 C1C 58.0(4) . . . . ? N3A Gd1 N7 C1C 147.7(4) . . . . ? N3B Gd1 N7 C1C -88.9(4) . . . . ? N3C Gd1 N7 C1C 39.2(4) . . . . ? N4 Gd1 N7 C1C -152.1(4) . . . . ? N1 Gd1 N7 C1C 135.5(4) . . . . ? C6 N7 C8 C9 -66.8(7) . . . . ? C1C N7 C8 C9 171.5(5) . . . . ? Gd1 N7 C8 C9 58.6(6) . . . . ? C3 N4 C9 C8 131.1(6) . . . . ? C1B N4 C9 C8 -108.4(6) . . . . ? Gd1 N4 C9 C8 10.0(7) . . . . ? N7 C8 C9 N4 -47.6(8) . . . . ? C3M' O3M O4M C4M -14(4) . . . . ? C3M O3M O4M C4M 27.4(18) . . . . ? C3M' O3M C4M O4M 17(4) . . . . ? C3M O3M C4M O4M -115(4) . . . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.29 _refine_diff_density_min -1.12 _refine_diff_density_rms 0.16 data_GDN3AC _database_code_CSD 195031 _exptl_special_details ; Only the Gd could be refined with anisotropic displacement parameters due to the limited quality of the diffraction data. Therefore O, N, C and H atoms were refined isotropically. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H29 Gd N5 O6, C H4 O' _chemical_formula_sum 'C19 H33 Gd N5 O7' _chemical_formula_weight 600.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.213(2) _cell_length_b 15.138(3) _cell_length_c 15.278(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.476(4) _cell_angle_gamma 90.00 _cell_volume 2413.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2412 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.24 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 2.795 _exptl_absorpt_correction_type 'Multi-scan + refdelf' _exptl_absorpt_correction_T_min 0.180 _exptl_absorpt_correction_T_max 0.515 _exptl_absorpt_process_details ; Reported Tmin and Tmax are from two corrections multiplied. SADABS, Bruker (1999) and Parkin S, Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 11249 _diffrn_reflns_av_R_equivalents 0.099 _diffrn_reflns_av_sigmaI/netI 0.127 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4229 _reflns_number_gt 2665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0335P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier map' _atom_sites_solution_hydrogens 'placed geometrically. MeOH hydrogens omitted ' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4229 _refine_ls_number_parameters 145 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1363 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd Gd 0.16841(5) 0.81459(4) 0.06532(3) 0.02817(17) Uani 1 1 d . . . N1 N 0.0646(8) 0.8174(7) 0.1969(5) 0.037(2) Uiso 1 1 d . . . C2 C 0.1561(10) 0.8043(8) 0.2947(7) 0.042(3) Uiso 1 1 d . . . H2A H 0.1216 0.7589 0.3257 0.050 Uiso 1 1 calc R . . H2B H 0.1641 0.8602 0.3301 0.050 Uiso 1 1 calc R . . C3 C 0.2907(10) 0.7753(8) 0.2990(7) 0.036(3) Uiso 1 1 d . . . H3A H 0.3513 0.7786 0.3651 0.043 Uiso 1 1 calc R . . H3B H 0.2865 0.7129 0.2786 0.043 Uiso 1 1 calc R . . N4 N 0.3409(8) 0.8303(5) 0.2392(5) 0.0286(19) Uiso 1 1 d . . . C5 C 0.3640(11) 0.9235(8) 0.2746(7) 0.040(3) Uiso 1 1 d . . . H5A H 0.4576 0.9339 0.3029 0.047 Uiso 1 1 calc R . . H5B H 0.3285 0.9312 0.3246 0.047 Uiso 1 1 calc R . . C6 C 0.3039(11) 0.9927(8) 0.1975(7) 0.043(3) Uiso 1 1 d . . . H6A H 0.3073 1.0513 0.2271 0.052 Uiso 1 1 calc R . . H6B H 0.3544 0.9961 0.1563 0.052 Uiso 1 1 calc R . . N7 N 0.1680(8) 0.9710(6) 0.1394(6) 0.036(2) Uiso 1 1 d . . . C8 C 0.0771(11) 0.9830(8) 0.1943(8) 0.046(3) Uiso 1 1 d . . . H8A H 0.1289 0.9932 0.2615 0.055 Uiso 1 1 calc R . . H8B H 0.0231 1.0360 0.1702 0.055 Uiso 1 1 calc R . . C9 C -0.0066(11) 0.9056(8) 0.1857(8) 0.044(3) Uiso 1 1 d . . . H9A H -0.0768 0.9070 0.1233 0.053 Uiso 1 1 calc R . . H9B H -0.0456 0.9096 0.2341 0.053 Uiso 1 1 calc R . . C1A C -0.0305(12) 0.7422(9) 0.1744(8) 0.048(3) Uiso 1 1 d . . . H1A1 H -0.0991 0.7533 0.1126 0.057 Uiso 1 1 calc R . . H1A2 H -0.0706 0.7404 0.2223 0.057 Uiso 1 1 calc R . . C2A C 0.0304(12) 0.6534(9) 0.1718(8) 0.050(3) Uiso 1 1 d . . . H2A1 H 0.0790 0.6330 0.2367 0.060 Uiso 1 1 calc R . . H2A2 H -0.0371 0.6093 0.1408 0.060 Uiso 1 1 calc R . . N3A N 0.1169(9) 0.6619(6) 0.1197(6) 0.037(2) Uiso 1 1 d . . . C4A C 0.1624(11) 0.5886(8) 0.0920(7) 0.041(3) Uiso 1 1 d . A . C5A C 0.2488(12) 0.6105(9) 0.0340(8) 0.047(3) Uiso 1 1 d D . . O6A O 0.2826(6) 0.6919(5) 0.0340(4) 0.0340(16) Uiso 1 1 d . A . O7A O 0.2556(13) 0.5465(8) -0.0174(8) 0.041(3) Uiso 0.65 1 d PD A 1 O7A' O 0.318(3) 0.5516(18) 0.014(2) 0.074(9) Uiso 0.35 1 d PD A 2 C8A C 0.1432(14) 0.4965(10) 0.1177(9) 0.065(4) Uiso 1 1 d . . . H8A1 H 0.1851 0.4888 0.1859 0.098 Uiso 1 1 calc R A . H8A2 H 0.1804 0.4553 0.0854 0.098 Uiso 1 1 calc R . . H8A3 H 0.0512 0.4847 0.0990 0.098 Uiso 1 1 calc R . . C1B C 0.4595(10) 0.7892(7) 0.2351(7) 0.034(3) Uiso 1 1 d . . . H1B1 H 0.4418 0.7266 0.2157 0.040 Uiso 1 1 calc R . . H1B2 H 0.5272 0.7902 0.2987 0.040 Uiso 1 1 calc R . . C2B C 0.5087(10) 0.8377(7) 0.1651(6) 0.032(3) Uiso 1 1 d . . . H2B1 H 0.5537 0.8928 0.1940 0.039 Uiso 1 1 calc R . . H2B2 H 0.5698 0.7996 0.1494 0.039 Uiso 1 1 calc R . . N3B N 0.3976(8) 0.8589(6) 0.0787(5) 0.0279(19) Uiso 1 1 d . . . C4B C 0.4137(9) 0.8820(7) 0.0024(6) 0.029(2) Uiso 1 1 d . . . C5B C 0.2902(9) 0.9092(7) -0.0760(6) 0.029(2) Uiso 1 1 d . . . O6B O 0.1840(7) 0.8923(5) -0.0657(4) 0.0349(17) Uiso 1 1 d . . . O7B O 0.3004(7) 0.9469(5) -0.1488(5) 0.0418(19) Uiso 1 1 d . . . C8B C 0.5420(11) 0.8847(9) -0.0116(8) 0.046(3) Uiso 1 1 d . . . H8B1 H 0.6038 0.9194 0.0389 0.069 Uiso 1 1 calc R . . H8B2 H 0.5299 0.9120 -0.0724 0.069 Uiso 1 1 calc R . . H8B3 H 0.5745 0.8244 -0.0104 0.069 Uiso 1 1 calc R . . O1AC O 0.0014(7) 0.7365(5) -0.0672(5) 0.0384(18) Uiso 1 1 d . . . O2AC O -0.0569(7) 0.8629(5) -0.0207(4) 0.0357(17) Uiso 1 1 d . . . C3AC C -0.0838(10) 0.7938(7) -0.0708(7) 0.031(2) Uiso 1 1 d . . . C4AC C -0.2224(12) 0.7733(10) -0.1330(8) 0.056(3) Uiso 1 1 d . . . H4A1 H -0.2263 0.7556 -0.1957 0.084 Uiso 1 1 calc R . . H4A2 H -0.2753 0.8260 -0.1383 0.084 Uiso 1 1 calc R . . H4A3 H -0.2547 0.7251 -0.1049 0.084 Uiso 1 1 calc R . . C1M C 0.5825(15) 0.6245(11) 0.0487(10) 0.071(4) Uiso 1 1 d D . . O1M O 0.6608(18) 0.6266(13) -0.0054(13) 0.099(6) Uiso 0.65 1 d PD B 1 O1M' O 0.712(2) 0.614(3) 0.068(3) 0.145(16) Uiso 0.35 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd 0.0384(3) 0.0383(3) 0.0155(2) 0.0045(3) 0.01885(19) 0.0058(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd N1 2.667(8) . Y Gd N4 2.664(7) . Y Gd N7 2.625(9) . Y Gd N3A 2.593(9) . Y Gd N3B 2.591(8) . Y Gd O6A 2.401(7) . Y Gd O6B 2.382(7) . Y Gd O1AC 2.496(7) . Y Gd O2AC 2.492(7) . Y Gd C3AC 2.849(10) . ? N1 C2 1.484(13) . ? N1 C1A 1.512(15) . ? N1 C9 1.532(14) . ? C2 C3 1.550(15) . ? C3 N4 1.490(13) . ? N4 C1B 1.489(13) . ? N4 C5 1.499(14) . ? C5 C6 1.535(15) . ? C6 N7 1.493(14) . ? N7 C8 1.550(14) . ? C8 C9 1.477(16) . ? C1A C2A 1.514(17) . ? C2A N3A 1.469(15) . ? N3A C4A 1.352(14) . ? C4A C8A 1.486(18) . ? C4A C5A 1.568(16) . ? C5A O7A 1.267(15) . ? C5A O7A' 1.29(2) . ? C5A O6A 1.290(14) . ? C1B C2B 1.557(14) . ? C2B N3B 1.480(12) . ? N3B C4B 1.292(12) . ? C4B C5B 1.518(13) . ? C4B C8B 1.531(15) . ? C5B O6B 1.283(11) . ? C5B O7B 1.292(11) . ? O1AC C3AC 1.276(12) . ? O2AC C3AC 1.267(12) . ? C3AC C4AC 1.528(16) . ? C1M O1M' 1.38(2) . ? C1M O1M 1.41(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 N4 Gd N1 66.7(2) . . Y N7 Gd N1 65.8(3) . . Y N7 Gd N4 66.7(3) . . Y N3B Gd N1 129.1(2) . . Y N3A Gd N1 64.1(3) . . Y O6B Gd N1 144.3(3) . . Y O6A Gd N1 125.1(3) . . Y O2AC Gd N1 75.8(2) . . Y O1AC Gd N1 102.4(3) . . Y N3B Gd N4 64.0(2) . . Y N3A Gd N4 85.7(3) . . Y O6B Gd N4 123.0(2) . . Y O6A Gd N4 91.3(2) . . Y O2AC Gd N4 136.5(2) . . Y O1AC Gd N4 155.0(2) . . Y N3B Gd N7 83.7(3) . . Y N3A Gd N7 129.1(3) . . Y O6B Gd N7 85.9(3) . . Y O6A Gd N7 150.3(3) . . Y O2AC Gd N7 78.5(3) . . Y O1AC Gd N7 131.1(3) . . Y N3B Gd N3A 122.4(3) . . Y O6B Gd N3A 143.4(3) . . Y O6A Gd N3A 64.6(3) . . Y O2AC Gd N3A 97.4(3) . . Y O1AC Gd N3A 69.4(3) . . Y O6B Gd N3B 64.1(2) . . Y O6A Gd N3B 68.3(3) . . Y O2AC Gd N3B 138.6(2) . . Y O1AC Gd N3B 127.9(2) . . Y O6B Gd O6A 90.3(2) . . Y O6B Gd O2AC 77.5(2) . . Y O6A Gd O2AC 129.3(2) . . Y O6B Gd O1AC 79.4(2) . . Y O6A Gd O1AC 76.6(2) . . Y O2AC Gd O1AC 52.9(2) . . Y O6B Gd C3AC 78.5(3) . . ? O6A Gd C3AC 103.2(3) . . ? O2AC Gd C3AC 26.4(3) . . ? O1AC Gd C3AC 26.6(3) . . ? N3B Gd C3AC 141.0(3) . . ? N3A Gd C3AC 81.8(3) . . ? N7 Gd C3AC 104.9(3) . . ? N4 Gd C3AC 154.5(3) . . ? N1 Gd C3AC 87.8(3) . . ? C2 N1 C1A 107.4(9) . . ? C2 N1 C9 111.7(8) . . ? C1A N1 C9 109.6(8) . . ? C2 N1 Gd 115.2(6) . . ? C1A N1 Gd 106.4(6) . . ? C9 N1 Gd 106.4(6) . . ? N1 C2 C3 112.6(9) . . ? N4 C3 C2 113.4(9) . . ? C1B N4 C3 109.6(8) . . ? C1B N4 C5 111.7(8) . . ? C3 N4 C5 111.0(8) . . ? C1B N4 Gd 104.7(5) . . ? C3 N4 Gd 105.2(6) . . ? C5 N4 Gd 114.2(6) . . ? N4 C5 C6 113.4(8) . . ? N7 C6 C5 111.8(9) . . ? C6 N7 C8 112.5(8) . . ? C6 N7 Gd 107.0(7) . . ? C8 N7 Gd 116.4(7) . . ? C9 C8 N7 112.4(10) . . ? C8 C9 N1 113.2(9) . . ? N1 C1A C2A 112.8(10) . . ? N3A C2A C1A 109.3(10) . . ? C4A N3A C2A 119.9(10) . . ? C4A N3A Gd 118.5(7) . . ? C2A N3A Gd 121.4(7) . . ? N3A C4A C8A 125.4(11) . . ? N3A C4A C5A 112.6(10) . . ? C8A C4A C5A 121.9(11) . . ? O7A C5A O7A' 31.2(14) . . ? O7A C5A O6A 130.2(12) . . ? O7A' C5A O6A 117.3(18) . . ? O7A C5A C4A 112.2(12) . . ? O7A' C5A C4A 122.5(18) . . ? O6A C5A C4A 116.4(10) . . ? C5A O6A Gd 124.1(7) . . ? N4 C1B C2B 112.2(8) . . ? N3B C2B C1B 108.7(8) . . ? C4B N3B C2B 120.9(8) . . ? C4B N3B Gd 117.4(6) . . ? C2B N3B Gd 120.1(6) . . ? N3B C4B C5B 113.4(8) . . ? N3B C4B C8B 125.6(9) . . ? C5B C4B C8B 121.0(9) . . ? O6B C5B O7B 124.9(9) . . ? O6B C5B C4B 117.9(8) . . ? O7B C5B C4B 117.1(8) . . ? C5B O6B Gd 124.0(6) . . ? C3AC O1AC Gd 92.3(6) . . ? C3AC O2AC Gd 92.7(6) . . ? O2AC C3AC O1AC 121.8(9) . . ? O2AC C3AC C4AC 120.4(10) . . ? O1AC C3AC C4AC 117.6(10) . . ? O2AC C3AC Gd 60.9(5) . . ? O1AC C3AC Gd 61.1(5) . . ? C4AC C3AC Gd 171.3(8) . . ? O1M' C1M O1M 45.2(18) . . ? 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 O6B Gd N1 C2 -128.7(7) . . . . ? O6A Gd N1 C2 60.1(8) . . . . ? O2AC Gd N1 C2 -171.5(8) . . . . ? O1AC Gd N1 C2 142.3(7) . . . . ? N3B Gd N1 C2 -29.2(9) . . . . ? N3A Gd N1 C2 82.7(8) . . . . ? N7 Gd N1 C2 -87.9(8) . . . . ? N4 Gd N1 C2 -14.1(7) . . . . ? C3AC Gd N1 C2 164.7(8) . . . . ? O6B Gd N1 C1A 112.5(7) . . . . ? O6A Gd N1 C1A -58.7(7) . . . . ? O2AC Gd N1 C1A 69.6(7) . . . . ? O1AC Gd N1 C1A 23.4(7) . . . . ? N3B Gd N1 C1A -148.0(6) . . . . ? N3A Gd N1 C1A -36.1(6) . . . . ? N7 Gd N1 C1A 153.2(7) . . . . ? N4 Gd N1 C1A -132.9(7) . . . . ? C3AC Gd N1 C1A 45.8(7) . . . . ? O6B Gd N1 C9 -4.4(8) . . . . ? O6A Gd N1 C9 -175.6(6) . . . . ? O2AC Gd N1 C9 -47.2(6) . . . . ? O1AC Gd N1 C9 -93.4(6) . . . . ? N3B Gd N1 C9 95.1(6) . . . . ? N3A Gd N1 C9 -153.0(7) . . . . ? N7 Gd N1 C9 36.4(6) . . . . ? N4 Gd N1 C9 110.2(7) . . . . ? C3AC Gd N1 C9 -71.0(6) . . . . ? C1A N1 C2 C3 108.3(11) . . . . ? C9 N1 C2 C3 -131.5(10) . . . . ? Gd N1 C2 C3 -10.0(12) . . . . ? N1 C2 C3 N4 48.0(13) . . . . ? C2 C3 N4 C1B -170.7(8) . . . . ? C2 C3 N4 C5 65.4(11) . . . . ? C2 C3 N4 Gd -58.6(9) . . . . ? O6B Gd N4 C1B -67.6(6) . . . . ? O6A Gd N4 C1B 23.6(6) . . . . ? O2AC Gd N4 C1B -175.7(5) . . . . ? O1AC Gd N4 C1B 83.5(8) . . . . ? N3B Gd N4 C1B -41.4(6) . . . . ? N3A Gd N4 C1B 88.0(6) . . . . ? N7 Gd N4 C1B -135.9(6) . . . . ? N1 Gd N4 C1B 151.6(7) . . . . ? C3AC Gd N4 C1B 148.7(7) . . . . ? O6B Gd N4 C3 176.8(6) . . . . ? O6A Gd N4 C3 -92.0(6) . . . . ? O2AC Gd N4 C3 68.7(7) . . . . ? O1AC Gd N4 C3 -32.1(9) . . . . ? N3B Gd N4 C3 -157.0(7) . . . . ? N3A Gd N4 C3 -27.5(6) . . . . ? N7 Gd N4 C3 108.5(6) . . . . ? N1 Gd N4 C3 36.0(6) . . . . ? C3AC Gd N4 C3 33.2(10) . . . . ? O6B Gd N4 C5 54.8(7) . . . . ? O6A Gd N4 C5 146.0(7) . . . . ? O2AC Gd N4 C5 -53.3(8) . . . . ? O1AC Gd N4 C5 -154.1(7) . . . . ? N3B Gd N4 C5 81.0(7) . . . . ? N3A Gd N4 C5 -149.5(7) . . . . ? N7 Gd N4 C5 -13.4(7) . . . . ? N1 Gd N4 C5 -86.0(7) . . . . ? C3AC Gd N4 C5 -88.8(9) . . . . ? C1B N4 C5 C6 107.4(10) . . . . ? C3 N4 C5 C6 -129.9(9) . . . . ? Gd N4 C5 C6 -11.2(11) . . . . ? N4 C5 C6 N7 47.7(13) . . . . ? C5 C6 N7 C8 70.6(12) . . . . ? C5 C6 N7 Gd -58.5(9) . . . . ? O6B Gd N7 C6 -92.3(6) . . . . ? O6A Gd N7 C6 -8.8(9) . . . . ? O2AC Gd N7 C6 -170.4(6) . . . . ? O1AC Gd N7 C6 -164.5(5) . . . . ? N3B Gd N7 C6 -28.0(6) . . . . ? N3A Gd N7 C6 99.3(7) . . . . ? N4 Gd N7 C6 36.3(6) . . . . ? N1 Gd N7 C6 110.1(6) . . . . ? C3AC Gd N7 C6 -169.3(6) . . . . ? O6B Gd N7 C8 140.9(7) . . . . ? O6A Gd N7 C8 -135.6(7) . . . . ? O2AC Gd N7 C8 62.8(7) . . . . ? O1AC Gd N7 C8 68.7(7) . . . . ? N3B Gd N7 C8 -154.8(7) . . . . ? N3A Gd N7 C8 -27.5(8) . . . . ? N4 Gd N7 C8 -90.5(7) . . . . ? N1 Gd N7 C8 -16.7(6) . . . . ? C3AC Gd N7 C8 64.0(7) . . . . ? C6 N7 C8 C9 -130.9(10) . . . . ? Gd N7 C8 C9 -6.9(12) . . . . ? N7 C8 C9 N1 44.1(13) . . . . ? C2 N1 C9 C8 68.6(12) . . . . ? C1A N1 C9 C8 -172.5(9) . . . . ? Gd N1 C9 C8 -57.8(10) . . . . ? C2 N1 C1A C2A -65.8(11) . . . . ? C9 N1 C1A C2A 172.7(9) . . . . ? Gd N1 C1A C2A 58.0(10) . . . . ? N1 C1A C2A N3A -44.4(13) . . . . ? C1A C2A N3A C4A -166.9(10) . . . . ? C1A C2A N3A Gd 7.3(12) . . . . ? O6B Gd N3A C4A 41.3(10) . . . . ? O6A Gd N3A C4A -9.8(7) . . . . ? O2AC Gd N3A C4A 120.3(8) . . . . ? O1AC Gd N3A C4A 74.7(8) . . . . ? N3B Gd N3A C4A -48.0(8) . . . . ? N7 Gd N3A C4A -158.5(7) . . . . ? N4 Gd N3A C4A -103.3(8) . . . . ? N1 Gd N3A C4A -169.4(8) . . . . ? C3AC Gd N3A C4A 99.0(8) . . . . ? O6B Gd N3A C2A -133.0(7) . . . . ? O6A Gd N3A C2A 175.9(9) . . . . ? O2AC Gd N3A C2A -53.9(8) . . . . ? O1AC Gd N3A C2A -99.6(8) . . . . ? N3B Gd N3A C2A 137.8(8) . . . . ? N7 Gd N3A C2A 27.3(9) . . . . ? N4 Gd N3A C2A 82.5(8) . . . . ? N1 Gd N3A C2A 16.3(7) . . . . ? C3AC Gd N3A C2A -75.2(8) . . . . ? C2A N3A C4A C8A -6.5(17) . . . . ? Gd N3A C4A C8A 179.2(9) . . . . ? C2A N3A C4A C5A 177.8(9) . . . . ? Gd N3A C4A C5A 3.4(11) . . . . ? N3A C4A C5A O7A -157.8(11) . . . . ? C8A C4A C5A O7A 26.3(17) . . . . ? N3A C4A C5A O7A' 169(2) . . . . ? C8A C4A C5A O7A' -7(2) . . . . ? N3A C4A C5A O6A 11.3(14) . . . . ? C8A C4A C5A O6A -164.6(11) . . . . ? O7A C5A O6A Gd 143.8(13) . . . . ? O7A' C5A O6A Gd 178.3(17) . . . . ? C4A C5A O6A Gd -22.9(13) . . . . ? O6B Gd O6A C5A -134.6(8) . . . . ? O2AC Gd O6A C5A -60.5(8) . . . . ? O1AC Gd O6A C5A -55.5(8) . . . . ? N3B Gd O6A C5A 163.6(8) . . . . ? N3A Gd O6A C5A 17.8(7) . . . . ? N7 Gd O6A C5A 143.1(8) . . . . ? N4 Gd O6A C5A 102.4(8) . . . . ? N1 Gd O6A C5A 40.3(8) . . . . ? C3AC Gd O6A C5A -56.4(8) . . . . ? C3 N4 C1B C2B 173.9(8) . . . . ? C5 N4 C1B C2B -62.7(10) . . . . ? Gd N4 C1B C2B 61.4(8) . . . . ? N4 C1B C2B N3B -42.5(11) . . . . ? C1B C2B N3B C4B -165.2(9) . . . . ? C1B C2B N3B Gd 0.1(10) . . . . ? O6B Gd N3B C4B -15.7(7) . . . . ? O6A Gd N3B C4B 85.8(7) . . . . ? O2AC Gd N3B C4B -39.5(9) . . . . ? O1AC Gd N3B C4B 34.7(8) . . . . ? N3A Gd N3B C4B 122.8(7) . . . . ? N7 Gd N3B C4B -104.3(8) . . . . ? N4 Gd N3B C4B -171.4(8) . . . . ? N1 Gd N3B C4B -155.9(7) . . . . ? C3AC Gd N3B C4B 1.7(10) . . . . ? O6B Gd N3B C2B 178.4(8) . . . . ? O6A Gd N3B C2B -80.0(7) . . . . ? O2AC Gd N3B C2B 154.6(6) . . . . ? O1AC Gd N3B C2B -131.2(7) . . . . ? N3A Gd N3B C2B -43.1(8) . . . . ? N7 Gd N3B C2B 89.9(7) . . . . ? N4 Gd N3B C2B 22.8(7) . . . . ? N1 Gd N3B C2B 38.2(8) . . . . ? C3AC Gd N3B C2B -164.1(6) . . . . ? C2B N3B C4B C5B -174.6(8) . . . . ? Gd N3B C4B C5B 19.6(11) . . . . ? C2B N3B C4B C8B 4.4(16) . . . . ? Gd N3B C4B C8B -161.3(9) . . . . ? N3B C4B C5B O6B -11.9(14) . . . . ? C8B C4B C5B O6B 169.0(10) . . . . ? N3B C4B C5B O7B 168.9(9) . . . . ? C8B C4B C5B O7B -10.1(15) . . . . ? O7B C5B O6B Gd 176.0(7) . . . . ? C4B C5B O6B Gd -3.1(13) . . . . ? O6A Gd O6B C5B -56.4(8) . . . . ? O2AC Gd O6B C5B 173.3(8) . . . . ? O1AC Gd O6B C5B -132.7(8) . . . . ? N3B Gd O6B C5B 9.1(7) . . . . ? N3A Gd O6B C5B -101.1(8) . . . . ? N7 Gd O6B C5B 94.2(8) . . . . ? N4 Gd O6B C5B 35.4(9) . . . . ? N1 Gd O6B C5B 130.8(8) . . . . ? C3AC Gd O6B C5B -159.8(8) . . . . ? O6B Gd O1AC C3AC -85.3(6) . . . . ? O6A Gd O1AC C3AC -178.2(6) . . . . ? O2AC Gd O1AC C3AC -3.0(6) . . . . ? N3B Gd O1AC C3AC -130.1(6) . . . . ? N3A Gd O1AC C3AC 114.2(6) . . . . ? N7 Gd O1AC C3AC -10.3(7) . . . . ? N4 Gd O1AC C3AC 119.0(7) . . . . ? N1 Gd O1AC C3AC 58.3(6) . . . . ? O6B Gd O2AC C3AC 89.1(6) . . . . ? O6A Gd O2AC C3AC 9.1(7) . . . . ? O1AC Gd O2AC C3AC 3.1(6) . . . . ? N3B Gd O2AC C3AC 111.0(6) . . . . ? N3A Gd O2AC C3AC -54.0(6) . . . . ? N7 Gd O2AC C3AC 177.5(6) . . . . ? N4 Gd O2AC C3AC -145.6(6) . . . . ? N1 Gd O2AC C3AC -114.9(6) . . . . ? Gd O2AC C3AC O1AC -5.6(10) . . . . ? Gd O2AC C3AC C4AC 170.2(9) . . . . ? Gd O1AC C3AC O2AC 5.6(10) . . . . ? Gd O1AC C3AC C4AC -170.3(8) . . . . ? O6B Gd C3AC O2AC -85.2(6) . . . . ? O6A Gd C3AC O2AC -172.8(6) . . . . ? O1AC Gd C3AC O2AC -174.6(10) . . . . ? N3B Gd C3AC O2AC -101.1(7) . . . . ? N3A Gd C3AC O2AC 125.8(6) . . . . ? N7 Gd C3AC O2AC -2.6(6) . . . . ? N4 Gd C3AC O2AC 64.3(9) . . . . ? N1 Gd C3AC O2AC 61.7(6) . . . . ? O6B Gd C3AC O1AC 89.4(6) . . . . ? O6A Gd C3AC O1AC 1.8(6) . . . . ? O2AC Gd C3AC O1AC 174.6(10) . . . . ? N3B Gd C3AC O1AC 73.4(7) . . . . ? N3A Gd C3AC O1AC -59.6(6) . . . . ? N7 Gd C3AC O1AC 172.0(5) . . . . ? N4 Gd C3AC O1AC -121.1(7) . . . . ? N1 Gd C3AC O1AC -123.7(6) . . . . ? O6B Gd C3AC C4AC 173(5) . . . . ? O6A Gd C3AC C4AC 86(5) . . . . ? O2AC Gd C3AC C4AC -101(5) . . . . ? O1AC Gd C3AC C4AC 84(5) . . . . ? N3B Gd C3AC C4AC 157(5) . . . . ? N3A Gd C3AC C4AC 24(5) . . . . ? N7 Gd C3AC C4AC -104(5) . . . . ? N4 Gd C3AC C4AC -37(6) . . . . ? N1 Gd C3AC C4AC -40(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.19 _refine_diff_density_min -1.32 _refine_diff_density_rms 0.19