Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mike Ward' _publ_contact_author_address ; Department of Chemistry University of Sheffield Dainton Building Sheffield S3 7HF UK ; _publ_contact_author_fax '01142 229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_section_title ; Sensitised near-infrared luminescence from lanthanide(III) centres using Re(I) and Pt(II) diimine complexes as energy donors in d-f dinuclear complexes based on 2,3-bis(2-pyridyl)pyrazine ; _publ_contact_letter ; This CIF file contains details of the 4 crystal structures in the paper Sensitised near-infrared luminescence from lanthanide(III) centres... by F. Kennedy et al, submitted to Dalton Trans. for publication. ; loop_ _publ_author_name M.Ward Z.R.Bell S.Faulkner J.Jeffrey F.Kennedy T.Koullourou ; N.M.Shavaleev ; #======================================================== data_erases _database_code_depnum_ccdc_archive 'CCDC 626876' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 N4 Pt' _chemical_formula_weight 659.64 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' Pt Pt -1.7033 8.3905 '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 9.3819(16) _cell_length_b 19.480(4) _cell_length_c 14.6718(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.031(19) _cell_angle_gamma 90.00 _cell_volume 2681.4(8) _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 orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 5.260 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.50 _exptl_absorpt_process_details ? _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 'Siemens SMART area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16986 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6118 _reflns_number_gt 4757 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0193P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6118 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 Pt1 Pt 0.59269(3) 0.556659(11) 0.64166(2) 0.02365(7) Uani 1 1 d . . . N11 N 0.6328(5) 0.4531(3) 0.6389(4) 0.0271(12) Uani 1 1 d . . . N21 N 0.3977(7) 0.5175(3) 0.6031(3) 0.0218(11) Uani 1 1 d . . . N24 N 0.1382(6) 0.4577(3) 0.5641(4) 0.0310(15) Uani 1 1 d . . . N31 N 0.2463(7) 0.3144(3) 0.6703(4) 0.0383(17) Uani 1 1 d . . . C12 C 0.5239(8) 0.4125(4) 0.6121(4) 0.0257(17) Uani 1 1 d . . . C13 C 0.5465(7) 0.3441(4) 0.5908(4) 0.0237(18) Uani 1 1 d . . . H13A H 0.4707 0.3166 0.5681 0.028 Uiso 1 1 calc R . . C14 C 0.6816(8) 0.3160(4) 0.6028(5) 0.034(2) Uani 1 1 d . . . H14A H 0.6994 0.2694 0.5872 0.041 Uiso 1 1 calc R . . C15 C 0.7897(7) 0.3566(3) 0.6378(6) 0.0365(17) Uani 1 1 d . . . H15A H 0.8805 0.3378 0.6517 0.044 Uiso 1 1 calc R . . C16 C 0.7617(7) 0.4248(3) 0.6516(5) 0.0311(17) Uani 1 1 d . . . H16A H 0.8375 0.4536 0.6712 0.037 Uiso 1 1 calc R . . C22 C 0.2819(7) 0.5571(4) 0.5858(4) 0.0274(15) Uani 1 1 d . . . H22A H 0.2884 0.6057 0.5888 0.033 Uiso 1 1 calc R . . C23 C 0.1529(7) 0.5253(4) 0.5635(5) 0.0313(17) Uani 1 1 d . . . H23A H 0.0734 0.5530 0.5475 0.038 Uiso 1 1 calc R . . C25 C 0.2515(8) 0.4189(4) 0.5845(5) 0.0252(16) Uani 1 1 d . . . C26 C 0.3854(7) 0.4488(4) 0.5998(4) 0.0246(15) Uani 1 1 d . . . C32 C 0.2198(8) 0.3436(4) 0.5899(5) 0.0287(18) Uani 1 1 d . . . C33 C 0.1698(8) 0.3090(4) 0.5136(5) 0.0322(18) Uani 1 1 d . . . H33A H 0.1531 0.3324 0.4578 0.039 Uiso 1 1 calc R . . C34 C 0.1453(9) 0.2393(4) 0.5218(6) 0.048(2) Uani 1 1 d . . . H34A H 0.1097 0.2134 0.4718 0.058 Uiso 1 1 calc R . . C35 C 0.1736(9) 0.2084(5) 0.6039(6) 0.048(2) Uani 1 1 d . . . H35A H 0.1609 0.1603 0.6105 0.058 Uiso 1 1 calc R . . C36 C 0.2205(8) 0.2470(4) 0.6770(6) 0.042(2) Uani 1 1 d . . . H36A H 0.2349 0.2250 0.7340 0.050 Uiso 1 1 calc R . . C51 C 0.5399(7) 0.6533(3) 0.6359(6) 0.0281(16) Uani 1 1 d . . . C52 C 0.4966(8) 0.7113(4) 0.6306(6) 0.0342(18) Uani 1 1 d . . . C53 C 0.4346(8) 0.7793(4) 0.6215(4) 0.0320(18) Uani 1 1 d . . . C54 C 0.5084(8) 0.8386(4) 0.6477(6) 0.0418(18) Uani 1 1 d . . . H54A H 0.6012 0.8346 0.6731 0.050 Uiso 1 1 calc R . . C55 C 0.4479(9) 0.9028(4) 0.6370(6) 0.0421(19) Uani 1 1 d . . . H55A H 0.5016 0.9422 0.6534 0.051 Uiso 1 1 calc R . . C56 C 0.3120(10) 0.9112(5) 0.6033(5) 0.041(2) Uani 1 1 d . . . C57 C 0.2468(10) 0.9832(4) 0.5901(6) 0.052(3) Uani 1 1 d . . . H57A H 0.3152 1.0127 0.5582 0.078 Uiso 1 1 calc R . . H57B H 0.2244 1.0032 0.6497 0.078 Uiso 1 1 calc R . . H57C H 0.1593 0.9795 0.5539 0.078 Uiso 1 1 calc R . . C58 C 0.2375(9) 0.8527(4) 0.5814(6) 0.043(2) Uani 1 1 d . . . H58A H 0.1423 0.8568 0.5601 0.051 Uiso 1 1 calc R . . C59 C 0.2972(8) 0.7881(4) 0.5897(5) 0.040(2) Uani 1 1 d . . . H59A H 0.2426 0.7490 0.5732 0.048 Uiso 1 1 calc R . . C61 C 0.7818(8) 0.5834(4) 0.6858(5) 0.0274(16) Uani 1 1 d . . . C62 C 0.8967(9) 0.5911(3) 0.7151(4) 0.0295(16) Uani 1 1 d . . . C63 C 1.0388(8) 0.5987(4) 0.7537(5) 0.0305(17) Uani 1 1 d . . . C64 C 1.1055(9) 0.5438(4) 0.7999(5) 0.0407(19) Uani 1 1 d . . . H64A H 1.0587 0.5007 0.8050 0.049 Uiso 1 1 calc R . . C65 C 1.2401(9) 0.5531(5) 0.8378(5) 0.051(2) Uani 1 1 d . . . H65A H 1.2835 0.5164 0.8702 0.061 Uiso 1 1 calc R . . C66 C 1.3120(8) 0.6146(6) 0.8295(6) 0.049(3) Uani 1 1 d . . . C67 C 1.4616(8) 0.6256(6) 0.8716(7) 0.071(4) Uani 1 1 d . . . H67A H 1.5106 0.5813 0.8767 0.107 Uiso 1 1 calc R . . H67B H 1.4518 0.6460 0.9323 0.107 Uiso 1 1 calc R . . H67C H 1.5172 0.6564 0.8326 0.107 Uiso 1 1 calc R . . C68 C 1.2487(9) 0.6685(5) 0.7813(5) 0.046(2) Uani 1 1 d . . . H68A H 1.2980 0.7107 0.7736 0.055 Uiso 1 1 calc R . . C69 C 1.1143(9) 0.6601(4) 0.7450(4) 0.0350(18) Uani 1 1 d . . . H69A H 1.0717 0.6972 0.7130 0.042 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 Pt1 0.02317(10) 0.02777(11) 0.02001(10) -0.00018(18) -0.00136(14) -0.00135(17) N11 0.027(3) 0.032(3) 0.022(2) 0.004(3) -0.004(3) -0.002(2) N21 0.023(3) 0.027(3) 0.016(2) 0.001(2) -0.001(3) -0.005(3) N24 0.024(3) 0.043(4) 0.026(3) 0.000(3) -0.004(3) 0.001(3) N31 0.031(4) 0.046(4) 0.039(4) 0.013(3) 0.001(3) -0.002(3) C12 0.027(4) 0.034(4) 0.016(4) 0.001(3) 0.005(3) -0.007(3) C13 0.029(4) 0.030(4) 0.012(3) 0.005(3) -0.011(3) 0.000(3) C14 0.028(4) 0.031(5) 0.043(5) 0.004(4) 0.010(4) 0.008(4) C15 0.026(4) 0.034(4) 0.050(4) 0.005(5) -0.005(5) 0.005(3) C16 0.024(4) 0.039(4) 0.030(4) 0.004(4) -0.005(4) -0.006(3) C22 0.022(3) 0.038(4) 0.023(3) 0.001(4) 0.001(3) -0.003(4) C23 0.020(4) 0.043(5) 0.031(4) 0.003(4) -0.003(3) 0.006(3) C25 0.027(4) 0.031(4) 0.017(3) 0.002(3) -0.001(3) -0.007(3) C26 0.024(4) 0.031(4) 0.019(3) 0.003(3) -0.004(3) -0.004(4) C32 0.016(4) 0.032(5) 0.037(5) 0.003(4) 0.003(4) -0.008(3) C33 0.031(4) 0.033(5) 0.032(4) -0.001(3) -0.002(4) -0.010(3) C34 0.042(5) 0.047(5) 0.057(6) 0.001(4) 0.000(4) -0.015(4) C35 0.046(5) 0.041(5) 0.057(6) 0.018(4) 0.002(4) -0.015(4) C36 0.040(5) 0.044(5) 0.041(5) 0.016(4) 0.001(4) -0.009(4) C51 0.031(4) 0.028(4) 0.025(3) -0.001(4) 0.008(4) -0.005(3) C52 0.031(4) 0.044(5) 0.028(4) 0.002(4) -0.004(4) -0.008(3) C53 0.034(4) 0.038(4) 0.024(4) -0.003(3) 0.000(3) 0.003(3) C54 0.044(4) 0.043(5) 0.038(4) -0.002(5) -0.010(5) 0.002(4) C55 0.065(6) 0.027(4) 0.034(4) 0.002(4) -0.010(5) 0.001(4) C56 0.054(6) 0.043(5) 0.025(4) 0.005(4) 0.005(4) 0.012(5) C57 0.073(7) 0.032(5) 0.051(6) -0.010(4) 0.009(5) 0.010(5) C58 0.038(5) 0.048(6) 0.042(5) -0.002(4) -0.001(4) 0.007(4) C59 0.034(5) 0.040(5) 0.046(5) -0.005(4) 0.000(4) -0.002(4) C61 0.030(4) 0.025(4) 0.028(4) 0.002(3) -0.006(3) -0.001(3) C62 0.029(4) 0.025(4) 0.034(4) -0.002(3) 0.001(4) -0.006(4) C63 0.028(4) 0.040(5) 0.023(4) -0.002(3) 0.002(3) -0.003(3) C64 0.034(4) 0.051(5) 0.037(4) 0.006(3) 0.005(4) -0.009(4) C65 0.033(4) 0.090(7) 0.029(5) 0.013(5) -0.001(3) 0.019(5) C66 0.020(4) 0.095(8) 0.031(5) -0.017(5) -0.002(4) -0.009(5) C67 0.025(4) 0.145(11) 0.043(6) -0.018(7) 0.001(5) -0.014(5) C68 0.031(5) 0.071(6) 0.036(5) -0.020(5) 0.011(4) -0.013(5) C69 0.035(5) 0.041(4) 0.029(4) -0.006(3) 0.001(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C51 1.948(7) . ? Pt1 C61 1.959(7) . ? Pt1 N11 2.053(5) . ? Pt1 N21 2.061(6) . ? N11 C16 1.342(8) . ? N11 C12 1.351(8) . ? N21 C26 1.345(8) . ? N21 C22 1.355(9) . ? N24 C23 1.324(9) . ? N24 C25 1.338(9) . ? N31 C32 1.332(9) . ? N31 C36 1.338(10) . ? C12 C13 1.385(10) . ? C12 C26 1.490(10) . ? C13 C14 1.391(9) . ? C13 H13A 0.9500 . ? C14 C15 1.385(10) . ? C14 H14A 0.9500 . ? C15 C16 1.369(9) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C22 C23 1.398(10) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C25 C26 1.403(9) . ? C25 C32 1.499(9) . ? C32 C33 1.389(10) . ? C33 C34 1.382(10) . ? C33 H33A 0.9500 . ? C34 C35 1.372(11) . ? C34 H34A 0.9500 . ? C35 C36 1.382(11) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C51 C52 1.204(9) . ? C52 C53 1.452(10) . ? C53 C59 1.381(10) . ? C53 C54 1.401(10) . ? C54 C55 1.383(10) . ? C54 H54A 0.9500 . ? C55 C56 1.377(11) . ? C55 H55A 0.9500 . ? C56 C58 1.374(11) . ? C56 C57 1.543(11) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.383(10) . ? C58 H58A 0.9500 . ? C59 H59A 0.9500 . ? C61 C62 1.170(10) . ? C62 C63 1.455(10) . ? C63 C69 1.395(10) . ? C63 C64 1.413(10) . ? C64 C65 1.393(11) . ? C64 H64A 0.9500 . ? C65 C66 1.379(12) . ? C65 H65A 0.9500 . ? C66 C68 1.399(12) . ? C66 C67 1.549(11) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.379(11) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? 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 C51 Pt1 C61 89.3(3) . . ? C51 Pt1 N11 174.5(3) . . ? C61 Pt1 N11 95.8(2) . . ? C51 Pt1 N21 96.9(2) . . ? C61 Pt1 N21 173.1(2) . . ? N11 Pt1 N21 78.1(2) . . ? C16 N11 C12 118.8(6) . . ? C16 N11 Pt1 124.4(4) . . ? C12 N11 Pt1 116.3(4) . . ? C26 N21 C22 119.4(6) . . ? C26 N21 Pt1 117.0(5) . . ? C22 N21 Pt1 123.5(5) . . ? C23 N24 C25 118.8(6) . . ? C32 N31 C36 116.7(7) . . ? N11 C12 C13 120.9(7) . . ? N11 C12 C26 114.6(6) . . ? C13 C12 C26 124.3(7) . . ? C12 C13 C14 119.3(7) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.3 . . ? C15 C14 C13 119.2(7) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C16 C15 C14 118.0(7) . . ? C16 C15 H15A 121.0 . . ? C14 C15 H15A 121.0 . . ? N11 C16 C15 123.4(6) . . ? N11 C16 H16A 118.3 . . ? C15 C16 H16A 118.3 . . ? N21 C22 C23 119.1(7) . . ? N21 C22 H22A 120.5 . . ? C23 C22 H22A 120.5 . . ? N24 C23 C22 121.9(7) . . ? N24 C23 H23A 119.0 . . ? C22 C23 H23A 119.0 . . ? N24 C25 C26 120.8(6) . . ? N24 C25 C32 114.0(6) . . ? C26 C25 C32 125.2(7) . . ? N21 C26 C25 119.7(6) . . ? N21 C26 C12 113.2(6) . . ? C25 C26 C12 127.0(6) . . ? N31 C32 C33 124.7(7) . . ? N31 C32 C25 115.3(7) . . ? C33 C32 C25 119.9(7) . . ? C34 C33 C32 117.6(7) . . ? C34 C33 H33A 121.2 . . ? C32 C33 H33A 121.2 . . ? C35 C34 C33 118.4(8) . . ? C35 C34 H34A 120.8 . . ? C33 C34 H34A 120.8 . . ? C34 C35 C36 120.2(8) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? N31 C36 C35 122.3(7) . . ? N31 C36 H36A 118.8 . . ? C35 C36 H36A 118.8 . . ? C52 C51 Pt1 174.9(6) . . ? C51 C52 C53 175.7(8) . . ? C59 C53 C54 116.8(7) . . ? C59 C53 C52 121.2(7) . . ? C54 C53 C52 121.9(6) . . ? C55 C54 C53 120.8(7) . . ? C55 C54 H54A 119.6 . . ? C53 C54 H54A 119.6 . . ? C56 C55 C54 121.9(8) . . ? C56 C55 H55A 119.0 . . ? C54 C55 H55A 119.0 . . ? C58 C56 C55 117.1(8) . . ? C58 C56 C57 121.5(8) . . ? C55 C56 C57 121.4(8) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 C59 121.8(8) . . ? C56 C58 H58A 119.1 . . ? C59 C58 H58A 119.1 . . ? C53 C59 C58 121.4(8) . . ? C53 C59 H59A 119.3 . . ? C58 C59 H59A 119.3 . . ? C62 C61 Pt1 171.8(6) . . ? C61 C62 C63 178.0(8) . . ? C69 C63 C64 117.9(7) . . ? C69 C63 C62 121.2(7) . . ? C64 C63 C62 120.9(7) . . ? C65 C64 C63 119.6(8) . . ? C65 C64 H64A 120.2 . . ? C63 C64 H64A 120.2 . . ? C66 C65 C64 121.4(8) . . ? C66 C65 H65A 119.3 . . ? C64 C65 H65A 119.3 . . ? C65 C66 C68 119.3(8) . . ? C65 C66 C67 121.8(10) . . ? C68 C66 C67 118.8(9) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 C66 119.6(8) . . ? C69 C68 H68A 120.2 . . ? C66 C68 H68A 120.2 . . ? C68 C69 C63 122.1(8) . . ? C68 C69 H69A 118.9 . . ? C63 C69 H69A 118.9 . . ? 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 C51 Pt1 N11 C16 150(3) . . . . ? C61 Pt1 N11 C16 -8.8(7) . . . . ? N21 Pt1 N11 C16 174.4(7) . . . . ? C51 Pt1 N11 C12 -22(3) . . . . ? C61 Pt1 N11 C12 179.1(5) . . . . ? N21 Pt1 N11 C12 2.3(5) . . . . ? C51 Pt1 N21 C26 -178.6(5) . . . . ? C61 Pt1 N21 C26 -25(2) . . . . ? N11 Pt1 N21 C26 3.7(4) . . . . ? C51 Pt1 N21 C22 -2.0(5) . . . . ? C61 Pt1 N21 C22 152(2) . . . . ? N11 Pt1 N21 C22 -179.7(5) . . . . ? C16 N11 C12 C13 -5.2(10) . . . . ? Pt1 N11 C12 C13 167.3(5) . . . . ? C16 N11 C12 C26 -179.9(6) . . . . ? Pt1 N11 C12 C26 -7.3(7) . . . . ? N11 C12 C13 C14 4.2(10) . . . . ? C26 C12 C13 C14 178.3(6) . . . . ? C12 C13 C14 C15 1.4(11) . . . . ? C13 C14 C15 C16 -5.6(12) . . . . ? C12 N11 C16 C15 0.8(12) . . . . ? Pt1 N11 C16 C15 -171.1(6) . . . . ? C14 C15 C16 N11 4.7(13) . . . . ? C26 N21 C22 C23 -1.0(9) . . . . ? Pt1 N21 C22 C23 -177.5(5) . . . . ? C25 N24 C23 C22 -1.6(10) . . . . ? N21 C22 C23 N24 4.1(10) . . . . ? C23 N24 C25 C26 -3.7(10) . . . . ? C23 N24 C25 C32 175.6(6) . . . . ? C22 N21 C26 C25 -4.2(9) . . . . ? Pt1 N21 C26 C25 172.6(5) . . . . ? C22 N21 C26 C12 174.8(5) . . . . ? Pt1 N21 C26 C12 -8.4(6) . . . . ? N24 C25 C26 N21 6.7(10) . . . . ? C32 C25 C26 N21 -172.5(6) . . . . ? N24 C25 C26 C12 -172.1(6) . . . . ? C32 C25 C26 C12 8.6(11) . . . . ? N11 C12 C26 N21 10.2(8) . . . . ? C13 C12 C26 N21 -164.2(6) . . . . ? N11 C12 C26 C25 -170.8(7) . . . . ? C13 C12 C26 C25 14.7(11) . . . . ? C36 N31 C32 C33 -1.0(12) . . . . ? C36 N31 C32 C25 -179.3(6) . . . . ? N24 C25 C32 N31 -120.0(7) . . . . ? C26 C25 C32 N31 59.3(10) . . . . ? N24 C25 C32 C33 61.5(9) . . . . ? C26 C25 C32 C33 -119.1(8) . . . . ? N31 C32 C33 C34 0.3(12) . . . . ? C25 C32 C33 C34 178.6(7) . . . . ? C32 C33 C34 C35 -1.0(12) . . . . ? C33 C34 C35 C36 2.3(13) . . . . ? C32 N31 C36 C35 2.3(12) . . . . ? C34 C35 C36 N31 -3.1(14) . . . . ? C61 Pt1 C51 C52 -175(9) . . . . ? N11 Pt1 C51 C52 26(11) . . . . ? N21 Pt1 C51 C52 2(9) . . . . ? Pt1 C51 C52 C53 -8(20) . . . . ? C51 C52 C53 C59 2(13) . . . . ? C51 C52 C53 C54 179(100) . . . . ? C59 C53 C54 C55 -3.5(12) . . . . ? C52 C53 C54 C55 179.0(8) . . . . ? C53 C54 C55 C56 2.1(14) . . . . ? C54 C55 C56 C58 0.8(13) . . . . ? C54 C55 C56 C57 -178.9(8) . . . . ? C55 C56 C58 C59 -2.2(12) . . . . ? C57 C56 C58 C59 177.4(8) . . . . ? C54 C53 C59 C58 2.0(12) . . . . ? C52 C53 C59 C58 179.6(7) . . . . ? C56 C58 C59 C53 0.8(13) . . . . ? C51 Pt1 C61 C62 166(5) . . . . ? N11 Pt1 C61 C62 -16(5) . . . . ? N21 Pt1 C61 C62 12(6) . . . . ? Pt1 C61 C62 C63 -29(28) . . . . ? C61 C62 C63 C69 -159(25) . . . . ? C61 C62 C63 C64 22(25) . . . . ? C69 C63 C64 C65 2.4(10) . . . . ? C62 C63 C64 C65 -178.6(7) . . . . ? C63 C64 C65 C66 -1.6(11) . . . . ? C64 C65 C66 C68 -0.5(12) . . . . ? C64 C65 C66 C67 179.8(7) . . . . ? C65 C66 C68 C69 1.6(12) . . . . ? C67 C66 C68 C69 -178.6(7) . . . . ? C66 C68 C69 C63 -0.8(11) . . . . ? C64 C63 C69 C68 -1.2(11) . . . . ? C62 C63 C69 C68 179.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.366 _refine_diff_density_min -1.361 _refine_diff_density_rms 0.183 #===END data_fudge _database_code_depnum_ccdc_archive 'CCDC 626877' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H21 Cl F18 Gd N4 O11 Re' _chemical_formula_weight 1478.53 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Re Re -1.0185 7.2310 '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' _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 9.525(2) _cell_length_b 13.034(3) _cell_length_c 23.796(6) _cell_angle_alpha 105.83(3) _cell_angle_beta 90.746(19) _cell_angle_gamma 108.622(17) _cell_volume 2677.0(11) _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 orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1414 _exptl_absorpt_coefficient_mu 3.656 _exptl_absorpt_correction_type 'empirical, multi-scan' _exptl_absorpt_correction_T_min 0.25 _exptl_absorpt_correction_T_max 0.48 _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 'Siemens SMART CCD area detector' _diffrn_measurement_method 'omega rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22934 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9403 _reflns_number_gt 6984 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1145P)^2^+7.8773P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9403 _refine_ls_number_parameters 618 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1907 _refine_ls_wR_factor_gt 0.1795 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.066 _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 Re1 Re 0.02918(4) 0.90768(3) 0.115021(18) 0.03350(16) Uani 1 1 d . . . Cl5 Cl -0.0561(3) 0.7619(3) 0.16668(12) 0.0493(7) Uani 1 1 d . . . O41 O -0.0542(9) 1.0799(8) 0.2117(4) 0.061(2) Uani 1 1 d . . . O51 O 0.1464(9) 1.0837(7) 0.0494(4) 0.056(2) Uani 1 1 d . . . O61 O -0.2883(8) 0.8517(7) 0.0578(3) 0.050(2) Uani 1 1 d . . . N11 N 0.2499(9) 0.9437(7) 0.1567(4) 0.0339(18) Uani 1 1 d . . . N21 N 0.1167(9) 0.7785(6) 0.0584(4) 0.0318(18) Uani 1 1 d . . . N24 N 0.2291(9) 0.6058(7) 0.0084(4) 0.0338(19) Uani 1 1 d . . . N31 N 0.3862(10) 0.6562(7) 0.1490(4) 0.040(2) Uani 1 1 d . . . C12 C 0.3272(10) 0.8731(8) 0.1323(4) 0.031(2) Uani 1 1 d . . . C13 C 0.4752(11) 0.9013(8) 0.1498(5) 0.039(2) Uani 1 1 d . . . H13A H 0.5280 0.8529 0.1313 0.047 Uiso 1 1 calc R . . C14 C 0.5494(12) 0.9996(10) 0.1942(5) 0.048(3) Uani 1 1 d . . . H14A H 0.6519 1.0186 0.2067 0.058 Uiso 1 1 calc R . . C15 C 0.4693(12) 1.0699(9) 0.2200(5) 0.048(3) Uani 1 1 d . . . H15A H 0.5155 1.1373 0.2510 0.057 Uiso 1 1 calc R . . C16 C 0.3218(12) 1.0391(9) 0.1992(5) 0.042(2) Uani 1 1 d . . . H16A H 0.2683 1.0882 0.2160 0.051 Uiso 1 1 calc R . . C22 C 0.0500(11) 0.7021(8) 0.0056(4) 0.034(2) Uani 1 1 d . . . C23 C 0.1128(10) 0.6158(8) -0.0216(4) 0.032(2) Uani 1 1 d . . . C25 C 0.2879(10) 0.6770(8) 0.0599(4) 0.031(2) Uani 1 1 d . . . C26 C 0.2415(10) 0.7738(8) 0.0832(4) 0.030(2) Uani 1 1 d . . . C27 C -0.0745(12) 0.7057(10) -0.0244(5) 0.044(3) Uani 1 1 d . . . H27A H -0.1210 0.7595 -0.0072 0.053 Uiso 1 1 calc R . . C28 C -0.1292(12) 0.6306(10) -0.0793(5) 0.045(3) Uani 1 1 d . . . H28A H -0.2149 0.6326 -0.0993 0.054 Uiso 1 1 calc R . . C29 C -0.0629(11) 0.5519(9) -0.1064(5) 0.040(2) Uani 1 1 d . . . H29A H -0.1007 0.5033 -0.1450 0.048 Uiso 1 1 calc R . . C30 C 0.0553(11) 0.5444(9) -0.0778(4) 0.040(2) Uani 1 1 d . . . H30A H 0.0995 0.4898 -0.0963 0.048 Uiso 1 1 calc R . . C32 C 0.3977(11) 0.6486(8) 0.0905(4) 0.033(2) Uani 1 1 d . . . C33 C 0.5009(11) 0.6093(8) 0.0614(5) 0.040(2) Uani 1 1 d . . . H33A H 0.5078 0.6059 0.0212 0.048 Uiso 1 1 calc R . . C34 C 0.5952(13) 0.5746(9) 0.0903(5) 0.046(3) Uani 1 1 d . . . H34A H 0.6662 0.5459 0.0700 0.056 Uiso 1 1 calc R . . C35 C 0.5855(13) 0.5819(10) 0.1482(6) 0.052(3) Uani 1 1 d . . . H35A H 0.6498 0.5587 0.1689 0.063 Uiso 1 1 calc R . . C36 C 0.4806(12) 0.6236(9) 0.1761(5) 0.043(3) Uani 1 1 d . . . H36A H 0.4752 0.6293 0.2166 0.051 Uiso 1 1 calc R . . C41 C -0.0210(12) 1.0170(10) 0.1755(5) 0.041(2) Uani 1 1 d . . . C51 C 0.1030(11) 1.0175(9) 0.0735(5) 0.040(2) Uani 1 1 d . . . C61 C -0.1675(13) 0.8714(9) 0.0784(5) 0.040(3) Uani 1 1 d . . . Gd1 Gd 0.16499(9) -0.31695(6) 0.32033(3) 0.0621(2) Uani 1 1 d . . . O1 O -0.0734(13) -0.3080(11) 0.2885(5) 0.094(4) Uani 1 1 d . . . O2 O 0.1860(10) -0.2957(7) 0.2241(4) 0.060(2) Uani 1 1 d . . . O111 O 0.2860(13) -0.3737(10) 0.3873(4) 0.086(3) Uani 1 1 d . . . O115 O 0.0661(15) -0.2751(11) 0.4097(4) 0.098(4) Uani 1 1 d . . . O121 O 0.4247(13) -0.2225(8) 0.3228(4) 0.077(3) Uani 1 1 d . . . O125 O 0.2005(17) -0.1247(10) 0.3431(5) 0.098(4) Uani 1 1 d . . . O131 O 0.2258(10) -0.4778(7) 0.2648(4) 0.059(2) Uani 1 1 d . . . O135 O -0.0303(12) -0.4860(8) 0.3214(4) 0.068(3) Uani 1 1 d . . . C112 C 0.264(3) -0.391(3) 0.4335(9) 0.140(10) Uani 1 1 d . . . C113 C 0.147(3) -0.383(3) 0.4651(14) 0.163(10) Uiso 1 1 d . . . H11A H 0.1155 -0.4241 0.4929 0.196 Uiso 1 1 calc R . . C114 C 0.072(3) -0.305(2) 0.4526(13) 0.137(8) Uiso 1 1 d . . . C116 C 0.377(4) -0.451(3) 0.4534(15) 0.145(9) Uiso 1 1 d . . . C122 C 0.503(2) -0.1235(13) 0.3319(7) 0.082(5) Uani 1 1 d D . . C123 C 0.457(3) -0.0289(15) 0.3432(9) 0.115(7) Uani 1 1 d . . . H12A H 0.5283 0.0425 0.3454 0.138 Uiso 1 1 calc R . . C124 C 0.312(3) -0.0345(17) 0.3513(8) 0.108(8) Uani 1 1 d D . . C126 C 0.668(2) -0.1066(15) 0.3257(9) 0.116(8) Uani 1 1 d D . . C127 C 0.266(4) 0.076(3) 0.3570(16) 0.166(11) Uiso 1 1 d D . . C132 C 0.1909(15) -0.5769(10) 0.2694(5) 0.051(3) Uani 1 1 d . . . C133 C 0.0677(16) -0.6352(12) 0.2939(6) 0.065(4) Uani 1 1 d . . . H13B H 0.0554 -0.7095 0.2955 0.079 Uiso 1 1 calc R . . C134 C -0.0365(16) -0.5838(15) 0.3158(6) 0.069(4) Uani 1 1 d . . . C136 C 0.2911(18) -0.6420(12) 0.2417(7) 0.069(4) Uani 1 1 d . . . C137 C -0.1768(17) -0.6570(15) 0.3362(7) 0.074(4) Uani 1 1 d . . . F11 F 0.3561(19) -0.5423(16) 0.4175(8) 0.177(6) Uiso 1 1 d . . . F12 F 0.335(3) -0.472(2) 0.5020(11) 0.243(10) Uiso 1 1 d . . . F13 F 0.501(3) -0.381(2) 0.4624(10) 0.233(9) Uiso 1 1 d . . . F21 F 0.7509(16) 0.0030(13) 0.3344(7) 0.145(5) Uiso 1 1 d . . . F22 F 0.7308(17) -0.1430(13) 0.3616(7) 0.151(5) Uiso 1 1 d . . . F23 F 0.6917(14) -0.1628(11) 0.2739(6) 0.129(4) Uiso 1 1 d . . . F24 F 0.1603(19) 0.0616(14) 0.3176(8) 0.167(6) Uiso 1 1 d . . . F25 F 0.365(2) 0.1557(17) 0.3632(8) 0.189(7) Uiso 1 1 d . . . F26 F 0.195(2) 0.0843(16) 0.4081(9) 0.198(7) Uiso 1 1 d . . . F31 F 0.3230(13) -0.6998(8) 0.2743(4) 0.102(3) Uani 1 1 d U . . F32 F 0.2216(14) -0.7254(11) 0.1917(4) 0.117(4) Uani 1 1 d U . . F33 F 0.4151(14) -0.5805(10) 0.2282(8) 0.166(7) Uani 1 1 d U . . F34 F -0.1891(12) -0.6114(12) 0.3887(4) 0.134(5) Uani 1 1 d U . . F35 F -0.2970(12) -0.6600(11) 0.3054(5) 0.124(4) Uani 1 1 d U . . F36 F -0.1854(17) -0.7580(11) 0.3273(9) 0.186(8) Uani 1 1 d U . . C201 C 0.5561(16) 1.1722(13) 0.0548(7) 0.066(4) Uani 1 1 d . . . H20A H 0.4809 1.1485 0.0229 0.079 Uiso 1 1 calc R . . C202 C 0.6634(16) 1.1257(12) 0.0498(7) 0.068(4) Uani 1 1 d . . . H20B H 0.6652 1.0699 0.0147 0.082 Uiso 1 1 calc R . . C203 C 0.7743(15) 1.1609(13) 0.0978(7) 0.067(4) Uani 1 1 d . . . H20C H 0.8491 1.1267 0.0959 0.081 Uiso 1 1 calc R . . C204 C 0.7732(15) 1.2438(14) 0.1463(7) 0.071(4) Uani 1 1 d . . . H20D H 0.8504 1.2701 0.1778 0.085 Uiso 1 1 calc R . . C205 C 0.6623(18) 1.2899(13) 0.1507(7) 0.072(4) Uani 1 1 d . . . H20E H 0.6603 1.3471 0.1851 0.086 Uiso 1 1 calc R . . C206 C 0.5518(17) 1.2509(15) 0.1034(9) 0.080(5) Uani 1 1 d . . . H20F H 0.4726 1.2809 0.1059 0.096 Uiso 1 1 calc R . . F16 F -0.153(2) -0.2927(19) 0.4799(10) 0.212(8) Uiso 1 1 d . . . F15 F -0.065(3) -0.346(2) 0.5324(11) 0.253(10) Uiso 1 1 d . . . F14 F -0.004(3) -0.180(2) 0.5106(13) 0.253(11) Uiso 1 1 d . . . C117 C 0.009(4) -0.232(4) 0.5411(17) 0.190(14) Uiso 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 Re1 0.0346(2) 0.0369(2) 0.0332(2) 0.01011(17) 0.01199(16) 0.01754(17) Cl5 0.0509(15) 0.0587(17) 0.0437(15) 0.0247(13) 0.0164(13) 0.0173(13) O41 0.054(5) 0.072(6) 0.057(5) -0.002(5) 0.005(4) 0.037(5) O51 0.053(5) 0.053(5) 0.073(6) 0.032(5) 0.016(4) 0.019(4) O61 0.035(4) 0.074(6) 0.045(5) 0.017(4) 0.006(4) 0.023(4) N11 0.034(4) 0.038(5) 0.034(5) 0.009(4) 0.010(4) 0.019(4) N21 0.040(4) 0.024(4) 0.037(5) 0.014(4) 0.024(4) 0.012(3) N24 0.038(4) 0.035(4) 0.032(5) 0.014(4) 0.013(4) 0.012(4) N31 0.044(5) 0.033(4) 0.042(5) 0.007(4) 0.009(4) 0.015(4) C12 0.037(5) 0.031(5) 0.033(5) 0.019(4) 0.012(4) 0.013(4) C13 0.043(6) 0.027(5) 0.047(6) 0.007(5) 0.016(5) 0.012(4) C14 0.038(6) 0.049(7) 0.058(7) 0.012(6) 0.014(5) 0.016(5) C15 0.048(6) 0.039(6) 0.048(7) 0.001(5) 0.003(5) 0.011(5) C16 0.042(6) 0.042(6) 0.045(6) 0.006(5) 0.002(5) 0.023(5) C22 0.042(5) 0.039(5) 0.025(5) 0.012(4) 0.011(4) 0.015(4) C23 0.031(5) 0.029(5) 0.039(6) 0.015(4) 0.009(4) 0.007(4) C25 0.037(5) 0.028(5) 0.030(5) 0.011(4) 0.017(4) 0.009(4) C26 0.035(5) 0.029(5) 0.034(5) 0.015(4) 0.015(4) 0.014(4) C27 0.046(6) 0.057(7) 0.037(6) 0.015(5) 0.010(5) 0.028(5) C28 0.046(6) 0.053(7) 0.043(6) 0.016(5) 0.007(5) 0.023(5) C29 0.042(6) 0.038(6) 0.033(6) 0.013(5) 0.004(5) 0.004(5) C30 0.044(6) 0.035(5) 0.032(6) 0.003(4) 0.012(5) 0.007(5) C32 0.038(5) 0.025(5) 0.039(6) 0.008(4) 0.014(4) 0.015(4) C33 0.039(5) 0.031(5) 0.045(6) 0.006(5) 0.009(5) 0.012(4) C34 0.053(7) 0.037(6) 0.046(7) -0.002(5) 0.000(5) 0.023(5) C35 0.051(7) 0.048(7) 0.059(8) 0.008(6) -0.004(6) 0.026(6) C36 0.052(6) 0.042(6) 0.031(6) 0.010(5) -0.006(5) 0.013(5) C41 0.041(6) 0.048(6) 0.040(6) 0.011(5) 0.004(5) 0.025(5) C51 0.039(5) 0.042(6) 0.047(6) 0.015(5) 0.008(5) 0.024(5) C61 0.055(7) 0.038(6) 0.033(6) 0.012(5) 0.017(5) 0.020(5) Gd1 0.0963(5) 0.0666(4) 0.0376(4) 0.0163(3) 0.0251(3) 0.0445(4) O1 0.116(9) 0.139(11) 0.076(7) 0.068(8) 0.051(7) 0.077(8) O2 0.086(6) 0.066(6) 0.049(5) 0.028(4) 0.033(5) 0.046(5) O111 0.114(9) 0.116(9) 0.051(6) 0.040(6) 0.023(6) 0.056(7) O115 0.140(11) 0.128(10) 0.040(5) 0.017(6) 0.025(6) 0.071(9) O121 0.116(8) 0.045(5) 0.068(6) 0.006(5) 0.019(6) 0.031(5) O125 0.169(12) 0.075(7) 0.080(8) 0.028(6) 0.063(8) 0.073(8) O131 0.080(6) 0.059(5) 0.051(5) 0.020(4) 0.020(5) 0.036(5) O135 0.096(7) 0.067(6) 0.052(5) 0.025(5) 0.018(5) 0.036(5) C112 0.134(18) 0.28(3) 0.069(12) 0.084(17) 0.053(12) 0.12(2) C122 0.105(13) 0.058(10) 0.063(10) 0.007(7) 0.000(9) 0.009(9) C123 0.16(2) 0.055(10) 0.109(16) -0.003(10) 0.016(15) 0.032(12) C124 0.21(3) 0.080(13) 0.077(12) 0.037(10) 0.072(15) 0.095(16) C126 0.142(19) 0.064(11) 0.081(13) -0.001(10) -0.022(13) -0.027(12) C132 0.077(8) 0.045(7) 0.037(6) 0.013(5) 0.001(6) 0.026(6) C133 0.082(9) 0.062(8) 0.065(9) 0.027(7) 0.011(8) 0.034(7) C134 0.070(9) 0.094(12) 0.050(8) 0.034(8) 0.006(7) 0.024(8) C136 0.089(10) 0.056(8) 0.080(11) 0.032(8) 0.015(9) 0.038(8) C137 0.065(9) 0.096(12) 0.054(9) 0.031(8) 0.006(7) 0.012(8) F31 0.176(10) 0.095(7) 0.073(6) 0.025(5) -0.002(6) 0.096(7) F32 0.142(9) 0.159(10) 0.066(6) 0.006(7) 0.013(6) 0.097(8) F33 0.121(9) 0.104(8) 0.35(2) 0.134(11) 0.134(12) 0.075(7) F34 0.106(8) 0.184(12) 0.065(6) 0.036(7) 0.032(6) -0.014(8) F35 0.090(7) 0.155(11) 0.107(8) 0.038(8) -0.005(6) 0.016(7) F36 0.172(13) 0.104(9) 0.32(2) 0.117(12) 0.158(14) 0.053(9) C201 0.055(8) 0.078(10) 0.068(10) 0.037(8) 0.000(7) 0.013(7) C202 0.064(9) 0.053(8) 0.076(10) 0.023(7) 0.015(8) -0.001(7) C203 0.050(7) 0.083(10) 0.090(11) 0.055(10) 0.032(8) 0.025(7) C204 0.052(8) 0.081(10) 0.070(10) 0.041(9) -0.006(7) -0.008(7) C205 0.082(10) 0.066(9) 0.077(10) 0.033(8) 0.034(9) 0.027(8) C206 0.066(9) 0.098(12) 0.111(14) 0.059(12) 0.033(10) 0.050(9) _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 Re1 C61 1.912(12) . ? Re1 C41 1.914(11) . ? Re1 C51 1.916(11) . ? Re1 N11 2.164(8) . ? Re1 N21 2.243(8) . ? Re1 Cl5 2.469(3) . ? O41 C41 1.141(13) . ? O51 C51 1.135(12) . ? O61 C61 1.166(13) . ? N11 C16 1.339(13) . ? N11 C12 1.371(13) . ? N21 C26 1.346(13) . ? N21 C22 1.367(13) . ? N24 C25 1.306(12) . ? N24 C23 1.370(13) . ? N31 C36 1.335(14) . ? N31 C32 1.377(13) . ? C12 C13 1.366(14) . ? C12 C26 1.477(14) . ? C13 C14 1.386(15) . ? C13 H13A 0.9500 . ? C14 C15 1.396(16) . ? C14 H14A 0.9500 . ? C15 C16 1.375(15) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C22 C27 1.397(15) . ? C22 C23 1.445(14) . ? C23 C30 1.390(14) . ? C25 C26 1.440(13) . ? C25 C32 1.462(14) . ? C27 C28 1.377(15) . ? C27 H27A 0.9500 . ? C28 C29 1.389(16) . ? C28 H28A 0.9500 . ? C29 C30 1.352(15) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C32 C33 1.361(14) . ? C33 C34 1.377(16) . ? C33 H33A 0.9500 . ? C34 C35 1.362(17) . ? C34 H34A 0.9500 . ? C35 C36 1.379(16) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? Gd1 O125 2.323(12) . ? Gd1 O115 2.335(10) . ? Gd1 O111 2.356(10) . ? Gd1 O121 2.377(11) . ? Gd1 O2 2.385(8) . ? Gd1 O135 2.393(10) . ? Gd1 O131 2.400(8) . ? Gd1 O1 2.432(12) . ? O111 C112 1.192(19) . ? O115 C114 1.19(3) . ? O121 C122 1.223(17) . ? O125 C124 1.27(3) . ? O131 C132 1.263(14) . ? O135 C134 1.227(18) . ? C112 C113 1.37(3) . ? C112 C116 1.64(4) . ? C113 C114 1.51(4) . ? C113 H11A 0.9500 . ? C116 F13 1.21(3) . ? C116 F11 1.22(3) . ? C116 F12 1.30(3) . ? C122 C123 1.40(3) . ? C122 C126 1.53(2) . ? C123 C124 1.38(3) . ? C123 H12A 0.9500 . ? C124 C127 1.60(3) . ? C126 F22 1.31(2) . ? C126 F23 1.32(2) . ? C126 F21 1.35(2) . ? C127 F25 1.13(3) . ? C127 F24 1.30(3) . ? C127 F26 1.39(3) . ? C132 C133 1.409(18) . ? C132 C136 1.514(19) . ? C133 C134 1.40(2) . ? C133 H13B 0.9500 . ? C134 C137 1.54(2) . ? C136 F33 1.299(17) . ? C136 F31 1.312(15) . ? C136 F32 1.361(18) . ? C137 F36 1.25(2) . ? C137 F34 1.255(18) . ? C137 F35 1.335(18) . ? C201 C206 1.33(2) . ? C201 C202 1.34(2) . ? C201 H20A 0.9500 . ? C202 C203 1.41(2) . ? C202 H20B 0.9500 . ? C203 C204 1.35(2) . ? C203 H20C 0.9500 . ? C204 C205 1.36(2) . ? C204 H20D 0.9500 . ? C205 C206 1.40(2) . ? C205 H20E 0.9500 . ? C206 H20F 0.9500 . ? F16 F14 1.66(3) . ? F16 C117 1.91(4) . ? F15 C117 1.38(4) . ? F14 C117 1.15(4) . ? 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 C61 Re1 C41 85.3(4) . . ? C61 Re1 C51 89.6(4) . . ? C41 Re1 C51 90.3(5) . . ? C61 Re1 N11 178.3(4) . . ? C41 Re1 N11 95.5(4) . . ? C51 Re1 N11 92.0(4) . . ? C61 Re1 N21 104.5(4) . . ? C41 Re1 N21 168.8(4) . . ? C51 Re1 N21 95.4(4) . . ? N11 Re1 N21 74.6(3) . . ? C61 Re1 Cl5 92.2(3) . . ? C41 Re1 Cl5 92.2(3) . . ? C51 Re1 Cl5 177.1(3) . . ? N11 Re1 Cl5 86.2(2) . . ? N21 Re1 Cl5 81.96(19) . . ? C16 N11 C12 118.4(8) . . ? C16 N11 Re1 123.3(7) . . ? C12 N11 Re1 117.6(6) . . ? C26 N21 C22 119.5(8) . . ? C26 N21 Re1 113.9(6) . . ? C22 N21 Re1 126.5(7) . . ? C25 N24 C23 120.6(9) . . ? C36 N31 C32 117.2(9) . . ? C13 C12 N11 120.6(9) . . ? C13 C12 C26 124.6(9) . . ? N11 C12 C26 114.5(8) . . ? C12 C13 C14 121.0(10) . . ? C12 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? C13 C14 C15 118.2(10) . . ? C13 C14 H14A 120.9 . . ? C15 C14 H14A 120.9 . . ? C16 C15 C14 118.3(10) . . ? C16 C15 H15A 120.8 . . ? C14 C15 H15A 120.8 . . ? N11 C16 C15 123.4(10) . . ? N11 C16 H16A 118.3 . . ? C15 C16 H16A 118.3 . . ? N21 C22 C27 122.8(9) . . ? N21 C22 C23 119.0(9) . . ? C27 C22 C23 118.1(9) . . ? N24 C23 C30 120.9(9) . . ? N24 C23 C22 119.4(9) . . ? C30 C23 C22 119.8(9) . . ? N24 C25 C26 120.3(9) . . ? N24 C25 C32 115.1(8) . . ? C26 C25 C32 124.7(9) . . ? N21 C26 C25 119.8(9) . . ? N21 C26 C12 116.6(8) . . ? C25 C26 C12 123.6(9) . . ? C28 C27 C22 119.4(10) . . ? C28 C27 H27A 120.3 . . ? C22 C27 H27A 120.3 . . ? C27 C28 C29 122.0(10) . . ? C27 C28 H28A 119.0 . . ? C29 C28 H28A 119.0 . . ? C30 C29 C28 120.0(10) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C23 120.7(10) . . ? C29 C30 H30A 119.7 . . ? C23 C30 H30A 119.7 . . ? C33 C32 N31 121.5(9) . . ? C33 C32 C25 121.2(9) . . ? N31 C32 C25 117.2(8) . . ? C32 C33 C34 119.9(11) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C35 C34 C33 119.3(11) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C34 C35 C36 118.7(11) . . ? C34 C35 H35A 120.6 . . ? C36 C35 H35A 120.6 . . ? N31 C36 C35 123.3(10) . . ? N31 C36 H36A 118.3 . . ? C35 C36 H36A 118.3 . . ? O41 C41 Re1 178.1(11) . . ? O51 C51 Re1 179.1(10) . . ? O61 C61 Re1 177.7(9) . . ? O125 Gd1 O115 75.5(4) . . ? O125 Gd1 O111 116.4(5) . . ? O115 Gd1 O111 72.5(4) . . ? O125 Gd1 O121 73.2(4) . . ? O115 Gd1 O121 115.4(4) . . ? O111 Gd1 O121 73.5(4) . . ? O125 Gd1 O2 81.1(3) . . ? O115 Gd1 O2 147.8(4) . . ? O111 Gd1 O2 138.8(3) . . ? O121 Gd1 O2 77.3(3) . . ? O125 Gd1 O135 137.3(4) . . ? O115 Gd1 O135 73.5(4) . . ? O111 Gd1 O135 80.8(4) . . ? O121 Gd1 O135 147.8(3) . . ? O2 Gd1 O135 112.3(3) . . ? O125 Gd1 O131 149.3(4) . . ? O115 Gd1 O131 133.4(4) . . ? O111 Gd1 O131 72.7(3) . . ? O121 Gd1 O131 82.7(3) . . ? O2 Gd1 O131 75.3(3) . . ? O135 Gd1 O131 71.1(3) . . ? O125 Gd1 O1 75.3(5) . . ? O115 Gd1 O1 78.6(4) . . ? O111 Gd1 O1 143.9(3) . . ? O121 Gd1 O1 140.2(4) . . ? O2 Gd1 O1 74.3(3) . . ? O135 Gd1 O1 70.5(4) . . ? O131 Gd1 O1 115.7(4) . . ? C112 O111 Gd1 136.3(13) . . ? C114 O115 Gd1 132.1(17) . . ? C122 O121 Gd1 134.4(11) . . ? C124 O125 Gd1 135.8(12) . . ? C132 O131 Gd1 130.8(8) . . ? C134 O135 Gd1 134.1(10) . . ? O111 C112 C113 127(2) . . ? O111 C112 C116 112.7(19) . . ? C113 C112 C116 119(2) . . ? C112 C113 C114 115(3) . . ? C112 C113 H11A 122.5 . . ? C114 C113 H11A 122.5 . . ? O115 C114 C113 130(3) . . ? F13 C116 F11 118(3) . . ? F13 C116 F12 110(3) . . ? F11 C116 F12 106(3) . . ? F13 C116 C112 107(3) . . ? F11 C116 C112 109(3) . . ? F12 C116 C112 106(3) . . ? O121 C122 C123 127.3(19) . . ? O121 C122 C126 114.1(16) . . ? C123 C122 C126 118.6(17) . . ? C124 C123 C122 123.1(19) . . ? C124 C123 H12A 118.4 . . ? C122 C123 H12A 118.4 . . ? O125 C124 C123 125.8(16) . . ? O125 C124 C127 113(2) . . ? C123 C124 C127 119(2) . . ? F22 C126 F23 103(2) . . ? F22 C126 F21 106.3(16) . . ? F23 C126 F21 106.5(18) . . ? F22 C126 C122 114.3(18) . . ? F23 C126 C122 113.4(15) . . ? F21 C126 C122 112.8(19) . . ? F25 C127 F24 114(3) . . ? F25 C127 F26 109(3) . . ? F24 C127 F26 102(3) . . ? F25 C127 C124 113(3) . . ? F24 C127 C124 114(3) . . ? F26 C127 C124 102(2) . . ? O131 C132 C133 128.3(12) . . ? O131 C132 C136 114.7(11) . . ? C133 C132 C136 116.9(11) . . ? C134 C133 C132 120.1(13) . . ? C134 C133 H13B 119.9 . . ? C132 C133 H13B 119.9 . . ? O135 C134 C133 127.8(14) . . ? O135 C134 C137 115.0(15) . . ? C133 C134 C137 117.2(15) . . ? F33 C136 F31 108.3(14) . . ? F33 C136 F32 106.7(15) . . ? F31 C136 F32 101.7(11) . . ? F33 C136 C132 114.6(12) . . ? F31 C136 C132 112.7(12) . . ? F32 C136 C132 111.8(12) . . ? F36 C137 F34 112.0(16) . . ? F36 C137 F35 105.7(16) . . ? F34 C137 F35 105.2(15) . . ? F36 C137 C134 114.2(15) . . ? F34 C137 C134 110.6(14) . . ? F35 C137 C134 108.6(12) . . ? C206 C201 C202 121.7(15) . . ? C206 C201 H20A 119.1 . . ? C202 C201 H20A 119.1 . . ? C201 C202 C203 118.7(15) . . ? C201 C202 H20B 120.6 . . ? C203 C202 H20B 120.6 . . ? C204 C203 C202 119.6(14) . . ? C204 C203 H20C 120.2 . . ? C202 C203 H20C 120.2 . . ? C203 C204 C205 120.7(14) . . ? C203 C204 H20D 119.7 . . ? C205 C204 H20D 119.7 . . ? C204 C205 C206 118.4(15) . . ? C204 C205 H20E 120.8 . . ? C206 C205 H20E 120.8 . . ? C201 C206 C205 120.8(14) . . ? C201 C206 H20F 119.6 . . ? C205 C206 H20F 119.6 . . ? F14 F16 C117 36.6(13) . . ? C117 F14 F16 84(3) . . ? F14 C117 F15 126(4) . . ? F14 C117 F16 60(2) . . ? F15 C117 F16 67(2) . . ? 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 C61 Re1 N11 C16 -134(13) . . . . ? C41 Re1 N11 C16 -18.3(9) . . . . ? C51 Re1 N11 C16 72.1(9) . . . . ? N21 Re1 N11 C16 167.2(9) . . . . ? Cl5 Re1 N11 C16 -110.1(8) . . . . ? C61 Re1 N11 C12 56(13) . . . . ? C41 Re1 N11 C12 171.7(7) . . . . ? C51 Re1 N11 C12 -97.9(7) . . . . ? N21 Re1 N11 C12 -2.9(6) . . . . ? Cl5 Re1 N11 C12 79.8(6) . . . . ? C61 Re1 N21 C26 -166.7(6) . . . . ? C41 Re1 N21 C26 -17(2) . . . . ? C51 Re1 N21 C26 102.4(6) . . . . ? N11 Re1 N21 C26 11.8(6) . . . . ? Cl5 Re1 N21 C26 -76.5(6) . . . . ? C61 Re1 N21 C22 8.0(8) . . . . ? C41 Re1 N21 C22 157.3(18) . . . . ? C51 Re1 N21 C22 -83.0(8) . . . . ? N11 Re1 N21 C22 -173.5(8) . . . . ? Cl5 Re1 N21 C22 98.2(7) . . . . ? C16 N11 C12 C13 -1.9(14) . . . . ? Re1 N11 C12 C13 168.7(7) . . . . ? C16 N11 C12 C26 -176.2(8) . . . . ? Re1 N11 C12 C26 -5.7(10) . . . . ? N11 C12 C13 C14 2.5(15) . . . . ? C26 C12 C13 C14 176.3(9) . . . . ? C12 C13 C14 C15 -0.9(16) . . . . ? C13 C14 C15 C16 -1.2(17) . . . . ? C12 N11 C16 C15 -0.4(16) . . . . ? Re1 N11 C16 C15 -170.3(9) . . . . ? C14 C15 C16 N11 1.9(17) . . . . ? C26 N21 C22 C27 -176.1(9) . . . . ? Re1 N21 C22 C27 9.5(13) . . . . ? C26 N21 C22 C23 1.9(12) . . . . ? Re1 N21 C22 C23 -172.5(6) . . . . ? C25 N24 C23 C30 176.3(8) . . . . ? C25 N24 C23 C22 -3.4(12) . . . . ? N21 C22 C23 N24 5.9(13) . . . . ? C27 C22 C23 N24 -176.0(8) . . . . ? N21 C22 C23 C30 -173.8(8) . . . . ? C27 C22 C23 C30 4.3(13) . . . . ? C23 N24 C25 C26 -6.4(12) . . . . ? C23 N24 C25 C32 172.4(8) . . . . ? C22 N21 C26 C25 -11.6(12) . . . . ? Re1 N21 C26 C25 163.5(6) . . . . ? C22 N21 C26 C12 166.1(8) . . . . ? Re1 N21 C26 C12 -18.9(9) . . . . ? N24 C25 C26 N21 14.3(13) . . . . ? C32 C25 C26 N21 -164.3(8) . . . . ? N24 C25 C26 C12 -163.2(8) . . . . ? C32 C25 C26 C12 18.2(13) . . . . ? C13 C12 C26 N21 -157.4(9) . . . . ? N11 C12 C26 N21 16.6(11) . . . . ? C13 C12 C26 C25 20.1(14) . . . . ? N11 C12 C26 C25 -165.8(8) . . . . ? N21 C22 C27 C28 175.6(9) . . . . ? C23 C22 C27 C28 -2.4(14) . . . . ? C22 C27 C28 C29 -1.0(16) . . . . ? C27 C28 C29 C30 2.7(16) . . . . ? C28 C29 C30 C23 -0.8(15) . . . . ? N24 C23 C30 C29 177.6(9) . . . . ? C22 C23 C30 C29 -2.7(14) . . . . ? C36 N31 C32 C33 0.0(14) . . . . ? C36 N31 C32 C25 176.0(8) . . . . ? N24 C25 C32 C33 41.8(12) . . . . ? C26 C25 C32 C33 -139.5(9) . . . . ? N24 C25 C32 N31 -134.1(9) . . . . ? C26 C25 C32 N31 44.6(13) . . . . ? N31 C32 C33 C34 1.0(15) . . . . ? C25 C32 C33 C34 -174.8(9) . . . . ? C32 C33 C34 C35 -1.1(16) . . . . ? C33 C34 C35 C36 0.3(17) . . . . ? C32 N31 C36 C35 -0.9(15) . . . . ? C34 C35 C36 N31 0.8(17) . . . . ? C61 Re1 C41 O41 57(32) . . . . ? C51 Re1 C41 O41 146(32) . . . . ? N11 Re1 C41 O41 -122(32) . . . . ? N21 Re1 C41 O41 -94(31) . . . . ? Cl5 Re1 C41 O41 -35(32) . . . . ? C61 Re1 C51 O51 90(66) . . . . ? C41 Re1 C51 O51 5(66) . . . . ? N11 Re1 C51 O51 -90(66) . . . . ? N21 Re1 C51 O51 -165(100) . . . . ? Cl5 Re1 C51 O51 -142(61) . . . . ? C41 Re1 C61 O61 -6(24) . . . . ? C51 Re1 C61 O61 -97(24) . . . . ? N11 Re1 C61 O61 110(24) . . . . ? N21 Re1 C61 O61 168(24) . . . . ? Cl5 Re1 C61 O61 86(24) . . . . ? O125 Gd1 O111 C112 79(3) . . . . ? O115 Gd1 O111 C112 16(3) . . . . ? O121 Gd1 O111 C112 140(3) . . . . ? O2 Gd1 O111 C112 -173(2) . . . . ? O135 Gd1 O111 C112 -59(3) . . . . ? O131 Gd1 O111 C112 -132(3) . . . . ? O1 Gd1 O111 C112 -22(3) . . . . ? O125 Gd1 O115 C114 -139(2) . . . . ? O111 Gd1 O115 C114 -15(2) . . . . ? O121 Gd1 O115 C114 -76(2) . . . . ? O2 Gd1 O115 C114 176(2) . . . . ? O135 Gd1 O115 C114 70(2) . . . . ? O131 Gd1 O115 C114 29(2) . . . . ? O1 Gd1 O115 C114 143(2) . . . . ? O125 Gd1 O121 C122 -0.7(14) . . . . ? O115 Gd1 O121 C122 -65.0(15) . . . . ? O111 Gd1 O121 C122 -125.8(15) . . . . ? O2 Gd1 O121 C122 83.6(15) . . . . ? O135 Gd1 O121 C122 -164.4(13) . . . . ? O131 Gd1 O121 C122 160.1(15) . . . . ? O1 Gd1 O121 C122 38.2(17) . . . . ? O115 Gd1 O125 C124 121.5(17) . . . . ? O111 Gd1 O125 C124 59.9(17) . . . . ? O121 Gd1 O125 C124 -1.3(16) . . . . ? O2 Gd1 O125 C124 -80.7(17) . . . . ? O135 Gd1 O125 C124 165.9(15) . . . . ? O131 Gd1 O125 C124 -41(2) . . . . ? O1 Gd1 O125 C124 -156.7(17) . . . . ? O125 Gd1 O131 C132 170.5(11) . . . . ? O115 Gd1 O131 C132 14.1(13) . . . . ? O111 Gd1 O131 C132 57.5(11) . . . . ? O121 Gd1 O131 C132 132.5(11) . . . . ? O2 Gd1 O131 C132 -148.8(11) . . . . ? O135 Gd1 O131 C132 -28.4(10) . . . . ? O1 Gd1 O131 C132 -84.6(11) . . . . ? O125 Gd1 O135 C134 -169.0(12) . . . . ? O115 Gd1 O135 C134 -124.0(13) . . . . ? O111 Gd1 O135 C134 -49.6(13) . . . . ? O121 Gd1 O135 C134 -12.3(15) . . . . ? O2 Gd1 O135 C134 89.6(13) . . . . ? O131 Gd1 O135 C134 25.2(12) . . . . ? O1 Gd1 O135 C134 152.5(13) . . . . ? Gd1 O111 C112 C113 1(5) . . . . ? Gd1 O111 C112 C116 170.1(15) . . . . ? O111 C112 C113 C114 -24(5) . . . . ? C116 C112 C113 C114 167(3) . . . . ? Gd1 O115 C114 C113 0(4) . . . . ? C112 C113 C114 O115 25(5) . . . . ? O111 C112 C116 F13 67(4) . . . . ? C113 C112 C116 F13 -123(3) . . . . ? O111 C112 C116 F11 -62(4) . . . . ? C113 C112 C116 F11 109(3) . . . . ? O111 C112 C116 F12 -176(3) . . . . ? C113 C112 C116 F12 -5(4) . . . . ? Gd1 O121 C122 C123 -2(3) . . . . ? Gd1 O121 C122 C126 -177.4(11) . . . . ? O121 C122 C123 C124 7(3) . . . . ? C126 C122 C123 C124 -178.0(19) . . . . ? Gd1 O125 C124 C123 6(3) . . . . ? Gd1 O125 C124 C127 171.6(16) . . . . ? C122 C123 C124 O125 -9(4) . . . . ? C122 C123 C124 C127 -173(2) . . . . ? O121 C122 C126 F22 -60(2) . . . . ? C123 C122 C126 F22 124(2) . . . . ? O121 C122 C126 F23 57(2) . . . . ? C123 C122 C126 F23 -119(2) . . . . ? O121 C122 C126 F21 178.3(15) . . . . ? C123 C122 C126 F21 2(3) . . . . ? O125 C124 C127 F25 -179(3) . . . . ? C123 C124 C127 F25 -12(4) . . . . ? O125 C124 C127 F24 -46(3) . . . . ? C123 C124 C127 F24 121(3) . . . . ? O125 C124 C127 F26 64(3) . . . . ? C123 C124 C127 F26 -129(2) . . . . ? Gd1 O131 C132 C133 24.0(19) . . . . ? Gd1 O131 C132 C136 -159.7(9) . . . . ? O131 C132 C133 C134 2(2) . . . . ? C136 C132 C133 C134 -174.7(13) . . . . ? Gd1 O135 C134 C133 -15(2) . . . . ? Gd1 O135 C134 C137 164.2(9) . . . . ? C132 C133 C134 O135 -7(2) . . . . ? C132 C133 C134 C137 173.9(12) . . . . ? O131 C132 C136 F33 14(2) . . . . ? C133 C132 C136 F33 -169.6(15) . . . . ? O131 C132 C136 F31 138.1(13) . . . . ? C133 C132 C136 F31 -45.2(18) . . . . ? O131 C132 C136 F32 -108.0(13) . . . . ? C133 C132 C136 F32 68.8(15) . . . . ? O135 C134 C137 F36 176.3(16) . . . . ? C133 C134 C137 F36 -4(2) . . . . ? O135 C134 C137 F34 -56.3(19) . . . . ? C133 C134 C137 F34 123.3(17) . . . . ? O135 C134 C137 F35 58.7(18) . . . . ? C133 C134 C137 F35 -121.7(16) . . . . ? C206 C201 C202 C203 0(2) . . . . ? C201 C202 C203 C204 -2.8(19) . . . . ? C202 C203 C204 C205 3.1(19) . . . . ? C203 C204 C205 C206 -1(2) . . . . ? C202 C201 C206 C205 2(2) . . . . ? C204 C205 C206 C201 -1(2) . . . . ? F16 F14 C117 F15 13(5) . . . . ? F14 F16 C117 F15 -169(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.568 _refine_diff_density_min -3.559 _refine_diff_density_rms 0.187 #===END data_larges _database_code_depnum_ccdc_archive 'CCDC 626878' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H11 Cl4 N4 O3 Re' _chemical_formula_weight 659.31 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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 6.4657(16) _cell_length_b 19.437(5) _cell_length_c 17.053(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.969(5) _cell_angle_gamma 90.00 _cell_volume 2135.0(9) _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 orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 6.220 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.14 _exptl_absorpt_correction_T_max 0.49 _exptl_absorpt_process_details ? _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 'Siemens SMART area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11953 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.53 _reflns_number_total 4571 _reflns_number_gt 3670 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0446P)^2^+2.4169P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4571 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 Re1 Re 0.41627(3) 0.726113(11) 0.199337(12) 0.02027(9) Uani 1 1 d . . . Cl1 Cl 0.6053(2) 0.83324(8) 0.23360(9) 0.0330(3) Uani 1 1 d . . . Cl11 Cl 0.5875(6) 0.50439(14) 0.14898(16) 0.1105(13) Uani 1 1 d . . . Cl12 Cl 0.9429(4) 0.41490(14) 0.17491(16) 0.0747(7) Uani 1 1 d . . . Cl13 Cl 0.6823(4) 0.40952(15) 0.02966(14) 0.0744(7) Uani 1 1 d . . . O41 O 0.1667(8) 0.5976(3) 0.1547(3) 0.0494(13) Uani 1 1 d . . . O51 O 0.1553(8) 0.7388(2) 0.3411(3) 0.0395(12) Uani 1 1 d . . . O61 O 0.7516(7) 0.6443(2) 0.2975(3) 0.0364(10) Uani 1 1 d . . . N11 N 0.5771(7) 0.7264(2) 0.0927(3) 0.0235(10) Uani 1 1 d . . . N21 N 0.2366(7) 0.7927(2) 0.1180(2) 0.0185(9) Uani 1 1 d . . . N24 N 0.0523(7) 0.8925(2) 0.0202(3) 0.0252(10) Uani 1 1 d . . . N31 N 0.5484(7) 0.9213(2) -0.0306(3) 0.0223(10) Uani 1 1 d . . . C12 C 0.5057(8) 0.7696(3) 0.0345(3) 0.0187(11) Uani 1 1 d . . . C13 C 0.5863(9) 0.7682(3) -0.0390(4) 0.0249(12) Uani 1 1 d . . . H13A H 0.5309 0.7973 -0.0804 0.030 Uiso 1 1 calc R . . C14 C 0.7492(10) 0.7236(3) -0.0502(4) 0.0308(14) Uani 1 1 d . . . H14A H 0.8073 0.7223 -0.0995 0.037 Uiso 1 1 calc R . . C15 C 0.8264(9) 0.6811(3) 0.0103(4) 0.0321(14) Uani 1 1 d . . . H15A H 0.9393 0.6510 0.0038 0.038 Uiso 1 1 calc R . . C16 C 0.7359(9) 0.6835(3) 0.0802(4) 0.0291(13) Uani 1 1 d . . . H16A H 0.7870 0.6538 0.1216 0.035 Uiso 1 1 calc R . . C22 C 0.3252(8) 0.8126(3) 0.0514(3) 0.0189(10) Uani 1 1 d . . . C23 C 0.2404(8) 0.8679(3) 0.0073(3) 0.0211(11) Uani 1 1 d . . . C25 C -0.0431(9) 0.8681(3) 0.0804(3) 0.0266(12) Uani 1 1 d . . . H25A H -0.1799 0.8831 0.0878 0.032 Uiso 1 1 calc R . . C26 C 0.0543(8) 0.8209(3) 0.1330(3) 0.0228(11) Uani 1 1 d . . . H26A H -0.0082 0.8086 0.1794 0.027 Uiso 1 1 calc R . . C32 C 0.3491(9) 0.9080(3) -0.0514(3) 0.0226(11) Uani 1 1 d . . . C33 C 0.2375(9) 0.9355(3) -0.1179(3) 0.0275(12) Uani 1 1 d . . . H33A H 0.0962 0.9236 -0.1308 0.033 Uiso 1 1 calc R . . C34 C 0.3384(10) 0.9806(3) -0.1645(4) 0.0310(14) Uani 1 1 d . . . H34A H 0.2685 1.0004 -0.2104 0.037 Uiso 1 1 calc R . . C35 C 0.5439(10) 0.9959(3) -0.1423(3) 0.0300(13) Uani 1 1 d . . . H35A H 0.6165 1.0278 -0.1720 0.036 Uiso 1 1 calc R . . C36 C 0.6434(9) 0.9646(3) -0.0767(3) 0.0262(12) Uani 1 1 d . . . H36A H 0.7863 0.9743 -0.0637 0.031 Uiso 1 1 calc R . . C41 C 0.2542(8) 0.6417(3) 0.1651(4) 0.0211(12) Uani 1 1 d . . . C51 C 0.2502(10) 0.7338(3) 0.2870(4) 0.0267(13) Uani 1 1 d . . . C61 C 0.6220(9) 0.6730(3) 0.2621(3) 0.0282(13) Uani 1 1 d . . . C100 C 0.6882(13) 0.4247(4) 0.1304(5) 0.052(2) Uani 1 1 d . . . H100 H 0.5989 0.3893 0.1534 0.063 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 Re1 0.01961(13) 0.02432(13) 0.01736(13) 0.00321(9) 0.00440(8) 0.00359(9) Cl1 0.0302(8) 0.0377(8) 0.0317(8) -0.0024(6) 0.0057(6) -0.0017(6) Cl11 0.198(4) 0.0750(17) 0.0651(16) 0.0119(13) 0.0478(19) 0.079(2) Cl12 0.0757(16) 0.0750(15) 0.0678(15) 0.0040(13) -0.0261(12) -0.0045(12) Cl13 0.0608(14) 0.1085(19) 0.0532(13) -0.0252(13) 0.0009(11) 0.0170(14) O41 0.052(3) 0.047(3) 0.048(3) 0.003(3) 0.001(3) 0.014(3) O51 0.037(3) 0.050(3) 0.035(3) 0.004(2) 0.021(2) 0.003(2) O61 0.031(2) 0.042(3) 0.034(3) 0.014(2) -0.007(2) 0.006(2) N11 0.017(2) 0.027(2) 0.028(3) -0.003(2) 0.010(2) -0.0018(19) N21 0.018(2) 0.027(2) 0.010(2) 0.0054(17) -0.0009(17) 0.0032(18) N24 0.021(2) 0.027(2) 0.029(3) 0.002(2) 0.003(2) 0.0021(19) N31 0.021(2) 0.022(2) 0.025(2) 0.0007(19) 0.0047(19) 0.0016(19) C12 0.018(3) 0.020(3) 0.017(3) 0.000(2) 0.000(2) 0.000(2) C13 0.028(3) 0.025(3) 0.023(3) 0.004(2) 0.007(2) 0.004(2) C14 0.034(3) 0.036(3) 0.023(3) -0.004(2) 0.010(3) 0.005(3) C15 0.029(3) 0.039(3) 0.029(3) -0.002(3) 0.007(3) 0.011(3) C16 0.028(3) 0.034(3) 0.025(3) 0.002(3) 0.005(2) 0.005(3) C22 0.018(2) 0.022(3) 0.016(2) -0.001(2) -0.001(2) -0.003(2) C23 0.017(3) 0.021(3) 0.025(3) -0.003(2) 0.002(2) -0.001(2) C25 0.016(3) 0.032(3) 0.032(3) -0.003(3) 0.005(2) 0.001(2) C26 0.019(3) 0.024(3) 0.026(3) -0.006(2) 0.007(2) -0.001(2) C32 0.029(3) 0.021(3) 0.019(3) 0.002(2) 0.006(2) 0.002(2) C33 0.026(3) 0.030(3) 0.026(3) 0.003(2) -0.003(2) 0.004(2) C34 0.037(3) 0.034(3) 0.021(3) 0.009(2) 0.003(3) 0.008(3) C35 0.039(3) 0.025(3) 0.027(3) 0.002(2) 0.012(3) 0.001(3) C36 0.027(3) 0.022(3) 0.031(3) 0.002(2) 0.009(2) 0.001(2) C41 0.013(2) 0.015(3) 0.036(3) 0.017(2) 0.009(2) 0.003(2) C51 0.028(3) 0.030(3) 0.022(3) 0.012(2) 0.000(2) 0.007(2) C61 0.027(3) 0.034(3) 0.025(3) 0.000(3) 0.007(2) -0.005(3) C100 0.066(5) 0.051(5) 0.041(4) 0.003(4) 0.011(4) 0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C51 1.920(6) . ? Re1 C61 1.932(6) . ? Re1 C41 2.006(6) . ? Re1 N21 2.161(4) . ? Re1 N11 2.171(5) . ? Re1 Cl1 2.4592(16) . ? Cl11 C100 1.721(8) . ? Cl12 C100 1.763(9) . ? Cl13 C100 1.740(8) . ? O41 C41 1.034(7) . ? O51 C51 1.156(8) . ? O61 C61 1.136(7) . ? N11 C12 1.350(7) . ? N11 C16 1.354(7) . ? N21 C26 1.344(7) . ? N21 C22 1.371(7) . ? N24 C25 1.330(7) . ? N24 C23 1.343(7) . ? N31 C32 1.332(7) . ? N31 C36 1.337(7) . ? C12 C13 1.399(8) . ? C12 C22 1.483(7) . ? C13 C14 1.391(8) . ? C13 H13A 0.9500 . ? C14 C15 1.381(9) . ? C14 H14A 0.9500 . ? C15 C16 1.373(8) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C22 C23 1.396(7) . ? C23 C32 1.492(7) . ? C25 C26 1.394(8) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C32 C33 1.397(8) . ? C33 C34 1.383(8) . ? C33 H33A 0.9500 . ? C34 C35 1.383(9) . ? C34 H34A 0.9500 . ? C35 C36 1.383(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C100 H100 1.0000 . ? 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 C51 Re1 C61 90.8(2) . . ? C51 Re1 C41 88.7(2) . . ? C61 Re1 C41 92.4(2) . . ? C51 Re1 N21 98.5(2) . . ? C61 Re1 N21 169.0(2) . . ? C41 Re1 N21 93.72(19) . . ? C51 Re1 N11 172.9(2) . . ? C61 Re1 N11 96.2(2) . . ? C41 Re1 N11 92.0(2) . . ? N21 Re1 N11 74.38(17) . . ? C51 Re1 Cl1 92.83(19) . . ? C61 Re1 Cl1 90.93(18) . . ? C41 Re1 Cl1 176.33(15) . . ? N21 Re1 Cl1 82.75(13) . . ? N11 Re1 Cl1 86.11(13) . . ? C12 N11 C16 118.8(5) . . ? C12 N11 Re1 117.3(4) . . ? C16 N11 Re1 123.7(4) . . ? C26 N21 C22 118.6(5) . . ? C26 N21 Re1 123.6(4) . . ? C22 N21 Re1 117.4(3) . . ? C25 N24 C23 119.1(5) . . ? C32 N31 C36 116.6(5) . . ? N11 C12 C13 121.1(5) . . ? N11 C12 C22 115.6(5) . . ? C13 C12 C22 123.0(5) . . ? C14 C13 C12 118.8(5) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C15 C14 C13 119.9(6) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C16 C15 C14 118.4(6) . . ? C16 C15 H15A 120.8 . . ? C14 C15 H15A 120.8 . . ? N11 C16 C15 123.0(6) . . ? N11 C16 H16A 118.5 . . ? C15 C16 H16A 118.5 . . ? N21 C22 C23 119.3(5) . . ? N21 C22 C12 113.2(4) . . ? C23 C22 C12 127.4(5) . . ? N24 C23 C22 120.3(5) . . ? N24 C23 C32 114.2(5) . . ? C22 C23 C32 125.3(5) . . ? N24 C25 C26 121.2(5) . . ? N24 C25 H25A 119.4 . . ? C26 C25 H25A 119.4 . . ? N21 C26 C25 120.0(5) . . ? N21 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? N31 C32 C33 124.2(5) . . ? N31 C32 C23 115.0(5) . . ? C33 C32 C23 120.4(5) . . ? C34 C33 C32 118.3(6) . . ? C34 C33 H33A 120.9 . . ? C32 C33 H33A 120.9 . . ? C35 C34 C33 117.9(6) . . ? C35 C34 H34A 121.0 . . ? C33 C34 H34A 121.0 . . ? C36 C35 C34 119.7(6) . . ? C36 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? N31 C36 C35 123.2(6) . . ? N31 C36 H36A 118.4 . . ? C35 C36 H36A 118.4 . . ? O41 C41 Re1 172.9(6) . . ? O51 C51 Re1 178.0(6) . . ? O61 C61 Re1 176.0(5) . . ? Cl11 C100 Cl13 111.0(4) . . ? Cl11 C100 Cl12 111.8(5) . . ? Cl13 C100 Cl12 110.3(4) . . ? Cl11 C100 H100 107.8 . . ? Cl13 C100 H100 107.8 . . ? Cl12 C100 H100 107.8 . . ? 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 C51 Re1 N11 C12 4(2) . . . . ? C61 Re1 N11 C12 -168.2(4) . . . . ? C41 Re1 N11 C12 99.2(4) . . . . ? N21 Re1 N11 C12 5.9(4) . . . . ? Cl1 Re1 N11 C12 -77.7(4) . . . . ? C51 Re1 N11 C16 -172.3(17) . . . . ? C61 Re1 N11 C16 15.5(5) . . . . ? C41 Re1 N11 C16 -77.2(5) . . . . ? N21 Re1 N11 C16 -170.5(5) . . . . ? Cl1 Re1 N11 C16 106.0(5) . . . . ? C51 Re1 N21 C26 -5.6(5) . . . . ? C61 Re1 N21 C26 -152.9(10) . . . . ? C41 Re1 N21 C26 83.6(4) . . . . ? N11 Re1 N21 C26 174.7(5) . . . . ? Cl1 Re1 N21 C26 -97.4(4) . . . . ? C51 Re1 N21 C22 167.5(4) . . . . ? C61 Re1 N21 C22 20.2(13) . . . . ? C41 Re1 N21 C22 -103.3(4) . . . . ? N11 Re1 N21 C22 -12.3(4) . . . . ? Cl1 Re1 N21 C22 75.7(4) . . . . ? C16 N11 C12 C13 3.0(8) . . . . ? Re1 N11 C12 C13 -173.5(4) . . . . ? C16 N11 C12 C22 177.2(5) . . . . ? Re1 N11 C12 C22 0.7(6) . . . . ? N11 C12 C13 C14 -3.0(9) . . . . ? C22 C12 C13 C14 -176.7(5) . . . . ? C12 C13 C14 C15 0.8(9) . . . . ? C13 C14 C15 C16 1.2(10) . . . . ? C12 N11 C16 C15 -1.0(9) . . . . ? Re1 N11 C16 C15 175.3(5) . . . . ? C14 C15 C16 N11 -1.2(10) . . . . ? C26 N21 C22 C23 9.0(8) . . . . ? Re1 N21 C22 C23 -164.4(4) . . . . ? C26 N21 C22 C12 -170.2(5) . . . . ? Re1 N21 C22 C12 16.4(6) . . . . ? N11 C12 C22 N21 -11.0(7) . . . . ? C13 C12 C22 N21 163.0(5) . . . . ? N11 C12 C22 C23 169.8(5) . . . . ? C13 C12 C22 C23 -16.1(9) . . . . ? C25 N24 C23 C22 6.5(8) . . . . ? C25 N24 C23 C32 -168.8(5) . . . . ? N21 C22 C23 N24 -13.3(8) . . . . ? C12 C22 C23 N24 165.8(5) . . . . ? N21 C22 C23 C32 161.5(5) . . . . ? C12 C22 C23 C32 -19.4(9) . . . . ? C23 N24 C25 C26 4.1(8) . . . . ? C22 N21 C26 C25 1.4(8) . . . . ? Re1 N21 C26 C25 174.3(4) . . . . ? N24 C25 C26 N21 -8.3(9) . . . . ? C36 N31 C32 C33 0.9(8) . . . . ? C36 N31 C32 C23 -171.5(5) . . . . ? N24 C23 C32 N31 134.8(5) . . . . ? C22 C23 C32 N31 -40.2(8) . . . . ? N24 C23 C32 C33 -37.8(7) . . . . ? C22 C23 C32 C33 147.1(6) . . . . ? N31 C32 C33 C34 -1.3(9) . . . . ? C23 C32 C33 C34 170.6(5) . . . . ? C32 C33 C34 C35 -0.2(9) . . . . ? C33 C34 C35 C36 2.1(9) . . . . ? C32 N31 C36 C35 1.1(8) . . . . ? C34 C35 C36 N31 -2.6(9) . . . . ? C51 Re1 C41 O41 -24(4) . . . . ? C61 Re1 C41 O41 67(4) . . . . ? N21 Re1 C41 O41 -122(4) . . . . ? N11 Re1 C41 O41 163(4) . . . . ? Cl1 Re1 C41 O41 -138(3) . . . . ? C61 Re1 C51 O51 44(15) . . . . ? C41 Re1 C51 O51 136(15) . . . . ? N21 Re1 C51 O51 -130(15) . . . . ? N11 Re1 C51 O51 -128(15) . . . . ? Cl1 Re1 C51 O51 -47(15) . . . . ? C51 Re1 C61 O61 -132(8) . . . . ? C41 Re1 C61 O61 139(8) . . . . ? N21 Re1 C61 O61 16(9) . . . . ? N11 Re1 C61 O61 47(8) . . . . ? Cl1 Re1 C61 O61 -39(8) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.378 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.164 #===END data_luckys _database_code_depnum_ccdc_archive 'CCDC 626879' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H22 Cl F9 Gd N4 O9 Re S3' _chemical_formula_weight 1360.71 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Re Re -1.0185 7.2310 '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 8.849(4) _cell_length_b 38.843(11) _cell_length_c 13.404(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.26(4) _cell_angle_gamma 90.00 _cell_volume 4519(3) _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 orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2612 _exptl_absorpt_coefficient_mu 4.426 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.12 _exptl_absorpt_correction_T_max 0.51 _exptl_absorpt_process_details ? _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 'Siemens SMART area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28948 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.53 _reflns_number_total 10353 _reflns_number_gt 8086 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0314P)^2^+2.7290P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10353 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0782 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.17044(3) 0.332320(5) 0.257361(15) 0.02366(6) Uani 1 1 d . . . Re1 Re 0.33834(2) 0.457492(4) 0.680883(13) 0.02522(6) Uani 1 1 d . . . Cl1 Cl 0.13973(15) 0.42625(3) 0.75015(9) 0.0404(3) Uani 1 1 d . . . F421 F -0.1492(5) 0.23656(9) 0.0558(3) 0.0708(11) Uani 1 1 d . . . F422 F -0.1214(4) 0.22228(8) 0.2127(3) 0.0638(10) Uani 1 1 d . . . F423 F -0.3402(4) 0.24127(9) 0.1333(3) 0.0809(13) Uani 1 1 d . . . F521 F 0.4714(4) 0.22273(9) 0.2692(4) 0.0883(15) Uani 1 1 d . . . F523 F 0.4796(5) 0.23163(10) 0.4272(4) 0.0903(14) Uani 1 1 d . . . F524 F 0.6817(4) 0.23944(9) 0.3636(3) 0.0756(12) Uani 1 1 d . . . F621 F 0.1973(4) 0.31184(9) -0.1110(2) 0.0659(11) Uani 1 1 d . . . F622 F -0.0335(5) 0.30603(9) -0.0905(2) 0.0705(12) Uani 1 1 d . . . F623 F 0.0278(4) 0.34944(7) -0.17077(19) 0.0423(7) Uani 1 1 d . . . O41 O 0.0038(4) 0.28460(8) 0.2229(2) 0.0321(7) Uani 1 1 d . . . O44 O -0.0819(4) 0.35379(8) 0.2179(2) 0.0354(8) Uani 1 1 d . . . O51 O 0.3462(4) 0.28520(8) 0.2710(2) 0.0345(8) Uani 1 1 d . . . O54 O 0.4151(4) 0.35369(8) 0.3304(2) 0.0316(7) Uani 1 1 d . . . O61 O 0.1567(4) 0.32702(8) 0.0845(2) 0.0313(7) Uani 1 1 d . . . O64 O 0.1858(4) 0.38859(8) 0.1904(2) 0.0317(7) Uani 1 1 d . . . O71 O 0.4299(4) 0.49351(10) 0.8872(3) 0.0477(10) Uani 1 1 d . . . O81 O 0.6037(5) 0.49235(11) 0.6022(3) 0.0533(11) Uani 1 1 d . . . O91 O 0.1242(5) 0.51815(10) 0.6078(3) 0.0638(12) Uani 1 1 d . . . N11 N 0.1934(5) 0.30774(9) 0.4373(3) 0.0271(8) Uani 1 1 d . . . N21 N 0.1401(4) 0.37537(9) 0.4079(3) 0.0234(8) Uani 1 1 d . . . N24 N 0.2632(4) 0.42379(9) 0.5515(2) 0.0226(8) Uani 1 1 d . . . N31 N 0.4692(4) 0.41055(9) 0.7161(3) 0.0248(8) Uani 1 1 d . . . C12 C 0.2136(5) 0.32825(11) 0.5206(3) 0.0242(9) Uani 1 1 d . . . C13 C 0.2072(5) 0.31588(11) 0.6166(3) 0.0271(10) Uani 1 1 d . . . H13A H 0.2147 0.3312 0.6725 0.033 Uiso 1 1 calc R . . C14 C 0.1900(6) 0.28118(12) 0.6299(4) 0.0368(12) Uani 1 1 d . . . H14A H 0.1843 0.2722 0.6950 0.044 Uiso 1 1 calc R . . C15 C 0.1811(7) 0.25949(12) 0.5475(4) 0.0442(14) Uani 1 1 d . . . H15A H 0.1765 0.2352 0.5555 0.053 Uiso 1 1 calc R . . C16 C 0.1791(6) 0.27389(12) 0.4530(4) 0.0380(13) Uani 1 1 d . . . H16A H 0.1669 0.2590 0.3959 0.046 Uiso 1 1 calc R . . C22 C 0.2233(5) 0.36542(11) 0.4992(3) 0.0226(9) Uani 1 1 d . . . C23 C 0.3007(5) 0.38992(10) 0.5670(3) 0.0205(9) Uani 1 1 d . . . C25 C 0.1667(5) 0.43290(11) 0.4660(3) 0.0264(10) Uani 1 1 d . . . H25A H 0.1344 0.4562 0.4562 0.032 Uiso 1 1 calc R . . C26 C 0.1133(5) 0.40868(11) 0.3916(3) 0.0261(10) Uani 1 1 d . . . H26A H 0.0565 0.4161 0.3276 0.031 Uiso 1 1 calc R . . C32 C 0.4307(5) 0.38333(11) 0.6523(3) 0.0227(9) Uani 1 1 d . . . C33 C 0.5204(5) 0.35359(11) 0.6633(3) 0.0270(10) Uani 1 1 d . . . H33A H 0.4961 0.3352 0.6160 0.032 Uiso 1 1 calc R . . C34 C 0.6447(5) 0.35082(12) 0.7431(4) 0.0335(11) Uani 1 1 d . . . H34A H 0.7054 0.3305 0.7520 0.040 Uiso 1 1 calc R . . C35 C 0.6798(6) 0.37801(13) 0.8099(4) 0.0383(12) Uani 1 1 d . . . H35A H 0.7635 0.3765 0.8661 0.046 Uiso 1 1 calc R . . C36 C 0.5913(6) 0.40747(13) 0.7939(3) 0.0330(11) Uani 1 1 d . . . H36A H 0.6172 0.4263 0.8391 0.040 Uiso 1 1 calc R . . C41 C -0.1339(6) 0.28224(12) 0.1739(3) 0.0333(11) Uani 1 1 d . . . C42 C -0.1863(7) 0.24541(14) 0.1443(5) 0.0528(16) Uani 1 1 d . . . C43 C -0.2379(6) 0.30787(13) 0.1421(4) 0.0385(12) Uani 1 1 d . . . H43A H -0.3365 0.3017 0.1042 0.046 Uiso 1 1 calc R . . C44 C -0.2056(6) 0.34326(12) 0.1628(4) 0.0330(11) Uani 1 1 d . . . C45 C -0.3180(5) 0.36911(12) 0.1163(4) 0.0326(11) Uani 1 1 d . . . C47 C -0.4406(7) 0.42427(14) 0.0612(4) 0.0491(14) Uani 1 1 d . . . H47 H -0.4713 0.4476 0.0494 0.059 Uiso 1 1 calc R . . C48 C -0.5189(6) 0.39761(15) 0.0138(5) 0.0464(14) Uani 1 1 d . . . H48A H -0.6114 0.4000 -0.0354 0.056 Uiso 1 1 calc R . . C49 C -0.4505(6) 0.36582(14) 0.0442(4) 0.0382(12) Uani 1 1 d . . . H49A H -0.4913 0.3443 0.0177 0.046 Uiso 1 1 calc R . . C51 C 0.4788(6) 0.28130(13) 0.3255(4) 0.0378(12) Uani 1 1 d . . . C52 C 0.5287(7) 0.24338(17) 0.3445(6) 0.0611(19) Uani 1 1 d . . . C53 C 0.5793(6) 0.30571(13) 0.3745(4) 0.0392(12) Uani 1 1 d . . . H53A H 0.6783 0.2985 0.4092 0.047 Uiso 1 1 calc R . . C54 C 0.5418(6) 0.34092(12) 0.3754(3) 0.0301(10) Uani 1 1 d . . . C55 C 0.6530(6) 0.36453(12) 0.4372(4) 0.0322(11) Uani 1 1 d . . . C57 C 0.7721(7) 0.41458(17) 0.5291(5) 0.0562(18) Uani 1 1 d . . . H57 H 0.7997 0.4367 0.5568 0.067 Uiso 1 1 calc R . . C58 C 0.8554(7) 0.38634(18) 0.5569(5) 0.0540(16) Uani 1 1 d . . . H58A H 0.9475 0.3868 0.6071 0.065 Uiso 1 1 calc R . . C59 C 0.7979(4) 0.35578(11) 0.5069(3) 0.0202(9) Uani 1 1 d . . . H59 H 0.8441 0.3336 0.5164 0.024 Uiso 1 1 calc R . . C61 C 0.1160(5) 0.34786(11) 0.0108(3) 0.0250(9) Uani 1 1 d . . . C62 C 0.0779(6) 0.32921(12) -0.0913(3) 0.0357(12) Uani 1 1 d . . . C63 C 0.1078(5) 0.38312(11) 0.0121(3) 0.0266(10) Uani 1 1 d . . . H63A H 0.0708 0.3951 -0.0497 0.032 Uiso 1 1 calc R . . C64 C 0.1534(5) 0.40215(11) 0.1038(3) 0.0263(10) Uani 1 1 d . . . C65 C 0.1654(5) 0.43961(11) 0.0976(3) 0.0270(10) Uani 1 1 d . . . C67 C 0.1988(7) 0.50081(13) 0.1449(4) 0.0458(14) Uani 1 1 d . . . H67 H 0.2113 0.5228 0.1767 0.055 Uiso 1 1 calc R . . C68 C 0.1803(6) 0.49592(12) 0.0445(4) 0.0348(11) Uani 1 1 d . . . H68A H 0.1802 0.5141 -0.0029 0.042 Uiso 1 1 calc R . . C69 C 0.1612(5) 0.46103(12) 0.0162(4) 0.0319(11) Uani 1 1 d . . . H69A H 0.1468 0.4532 -0.0521 0.038 Uiso 1 1 calc R . . C71 C 0.3982(6) 0.48070(12) 0.8090(4) 0.0322(11) Uani 1 1 d . . . C81 C 0.5045(6) 0.47878(12) 0.6288(3) 0.0290(10) Uani 1 1 d . . . C91 C 0.2047(6) 0.49564(13) 0.6370(4) 0.0370(12) Uani 1 1 d . . . S46 S -0.27874(18) 0.41171(4) 0.14558(12) 0.0535(4) Uani 1 1 d . . . S56 S 0.6125(2) 0.40705(4) 0.43972(13) 0.0555(4) Uani 1 1 d . . . S66 S 0.1973(2) 0.46304(3) 0.20901(10) 0.0554(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 Gd1 0.03393(13) 0.01815(11) 0.01610(10) -0.00167(8) -0.00199(9) -0.00091(9) Re1 0.03493(11) 0.01699(9) 0.02070(9) -0.00320(7) -0.00203(7) -0.00038(7) Cl1 0.0445(8) 0.0458(8) 0.0307(6) -0.0090(5) 0.0071(5) -0.0136(6) F421 0.094(3) 0.042(2) 0.060(2) -0.0148(18) -0.025(2) -0.0069(19) F422 0.060(2) 0.0344(18) 0.086(3) 0.0260(17) -0.0151(19) -0.0127(16) F423 0.049(2) 0.043(2) 0.133(4) 0.021(2) -0.026(2) -0.0224(17) F521 0.061(2) 0.048(2) 0.133(4) -0.049(2) -0.037(2) 0.0201(18) F523 0.107(4) 0.041(2) 0.120(4) 0.022(2) 0.016(3) 0.021(2) F524 0.050(2) 0.055(2) 0.105(3) -0.034(2) -0.026(2) 0.0239(17) F621 0.084(3) 0.075(3) 0.0351(18) -0.0168(17) 0.0026(18) 0.043(2) F622 0.108(3) 0.061(2) 0.0364(18) -0.0097(16) 0.0004(19) -0.049(2) F623 0.067(2) 0.0341(16) 0.0204(13) 0.0000(12) -0.0049(13) 0.0055(14) O41 0.040(2) 0.0250(17) 0.0277(17) 0.0014(13) -0.0031(15) -0.0029(14) O44 0.037(2) 0.0277(18) 0.0360(19) -0.0061(14) -0.0052(15) 0.0011(14) O51 0.038(2) 0.0301(19) 0.0315(17) -0.0140(14) -0.0039(15) 0.0043(15) O54 0.0346(19) 0.0266(18) 0.0314(18) -0.0028(14) 0.0008(15) -0.0030(14) O61 0.050(2) 0.0193(16) 0.0223(16) 0.0013(12) 0.0020(15) 0.0014(14) O64 0.050(2) 0.0207(16) 0.0228(16) -0.0002(13) 0.0033(15) -0.0045(14) O71 0.058(3) 0.047(2) 0.035(2) -0.0207(18) 0.0036(18) -0.0097(19) O81 0.055(3) 0.059(3) 0.043(2) -0.0007(19) 0.005(2) -0.018(2) O91 0.065(3) 0.037(2) 0.079(3) 0.000(2) -0.012(2) 0.019(2) N11 0.042(2) 0.0168(19) 0.0210(19) -0.0024(14) 0.0014(17) -0.0002(16) N21 0.031(2) 0.0196(19) 0.0182(17) -0.0024(14) 0.0004(15) -0.0007(15) N24 0.032(2) 0.0185(18) 0.0164(17) -0.0019(14) 0.0019(15) 0.0012(15) N31 0.032(2) 0.023(2) 0.0179(17) 0.0009(14) -0.0013(15) -0.0019(15) C12 0.027(2) 0.024(2) 0.019(2) 0.0008(17) -0.0015(18) 0.0010(18) C13 0.037(3) 0.021(2) 0.022(2) 0.0000(18) 0.0021(19) -0.0042(19) C14 0.050(3) 0.031(3) 0.026(2) 0.007(2) -0.001(2) -0.005(2) C15 0.079(4) 0.017(2) 0.035(3) 0.004(2) 0.005(3) -0.004(2) C16 0.068(4) 0.018(2) 0.024(2) 0.0015(19) 0.000(2) -0.006(2) C22 0.028(2) 0.023(2) 0.016(2) -0.0012(16) 0.0007(17) -0.0018(18) C23 0.026(2) 0.019(2) 0.016(2) -0.0014(16) 0.0038(17) 0.0035(17) C25 0.034(3) 0.021(2) 0.022(2) 0.0000(17) 0.0004(19) 0.0030(19) C26 0.033(3) 0.022(2) 0.021(2) -0.0003(17) -0.0023(19) 0.0059(18) C32 0.029(2) 0.022(2) 0.016(2) 0.0011(16) 0.0010(17) -0.0009(18) C33 0.027(2) 0.025(2) 0.029(2) -0.0041(19) 0.0037(19) -0.0005(19) C34 0.030(3) 0.027(3) 0.040(3) 0.001(2) -0.001(2) 0.004(2) C35 0.031(3) 0.041(3) 0.035(3) 0.002(2) -0.011(2) 0.004(2) C36 0.036(3) 0.033(3) 0.025(2) 0.000(2) -0.006(2) -0.004(2) C41 0.037(3) 0.029(3) 0.029(2) 0.004(2) -0.004(2) -0.006(2) C42 0.051(4) 0.025(3) 0.070(4) 0.006(3) -0.020(3) -0.005(2) C43 0.033(3) 0.032(3) 0.044(3) 0.003(2) -0.007(2) -0.008(2) C44 0.038(3) 0.030(3) 0.030(3) 0.001(2) 0.002(2) 0.001(2) C45 0.029(3) 0.026(3) 0.042(3) -0.002(2) 0.004(2) 0.002(2) C47 0.048(3) 0.033(3) 0.064(4) -0.002(3) 0.005(3) 0.010(3) C48 0.030(3) 0.050(4) 0.059(4) 0.012(3) 0.006(3) 0.009(2) C49 0.030(3) 0.037(3) 0.047(3) 0.001(2) 0.006(2) 0.003(2) C51 0.041(3) 0.032(3) 0.037(3) -0.016(2) -0.002(2) 0.009(2) C52 0.050(4) 0.045(4) 0.079(5) -0.025(3) -0.012(3) 0.016(3) C53 0.031(3) 0.041(3) 0.042(3) -0.008(2) -0.002(2) 0.003(2) C54 0.032(3) 0.036(3) 0.022(2) -0.0053(19) 0.006(2) -0.007(2) C55 0.034(3) 0.033(3) 0.034(3) -0.008(2) 0.016(2) -0.009(2) C57 0.063(4) 0.054(4) 0.060(4) -0.027(3) 0.031(3) -0.038(3) C58 0.034(3) 0.076(5) 0.052(4) -0.016(3) 0.009(3) -0.014(3) C59 0.0094(19) 0.034(2) 0.017(2) -0.0105(17) 0.0026(15) -0.0092(17) C61 0.026(2) 0.026(2) 0.022(2) -0.0024(18) 0.0028(18) -0.0004(18) C62 0.055(3) 0.030(3) 0.020(2) 0.0010(19) 0.000(2) 0.006(2) C63 0.028(2) 0.027(2) 0.023(2) 0.0008(18) 0.0017(19) -0.0002(19) C64 0.030(3) 0.024(2) 0.024(2) 0.0014(18) 0.0030(19) 0.0014(19) C65 0.036(3) 0.019(2) 0.025(2) -0.0032(17) 0.004(2) -0.0025(19) C67 0.068(4) 0.019(3) 0.047(3) -0.004(2) 0.005(3) -0.015(2) C68 0.037(3) 0.022(2) 0.044(3) 0.007(2) 0.007(2) -0.002(2) C69 0.033(3) 0.030(3) 0.033(3) 0.002(2) 0.007(2) 0.003(2) C71 0.039(3) 0.025(3) 0.032(3) -0.005(2) 0.004(2) 0.001(2) C81 0.035(3) 0.025(2) 0.023(2) 0.0024(18) -0.004(2) -0.011(2) C91 0.045(3) 0.027(3) 0.034(3) -0.007(2) -0.003(2) -0.001(2) S46 0.0543(9) 0.0326(8) 0.0653(10) -0.0099(7) -0.0086(8) 0.0059(6) S56 0.0631(10) 0.0448(9) 0.0587(9) -0.0087(7) 0.0125(8) -0.0126(7) S66 0.1063(14) 0.0266(7) 0.0322(7) -0.0060(6) 0.0110(8) -0.0228(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 Gd1 O61 2.306(3) . ? Gd1 O44 2.345(3) . ? Gd1 O54 2.347(3) . ? Gd1 O41 2.357(3) . ? Gd1 O64 2.377(3) . ? Gd1 O51 2.386(3) . ? Gd1 N11 2.564(4) . ? Gd1 N21 2.674(3) . ? Re1 C91 1.916(5) . ? Re1 C71 1.920(5) . ? Re1 C81 1.932(5) . ? Re1 N31 2.162(4) . ? Re1 N24 2.171(3) . ? Re1 Cl1 2.4620(15) . ? F421 C42 1.336(7) . ? F422 C42 1.331(6) . ? F423 C42 1.350(7) . ? F521 C52 1.311(7) . ? F523 C52 1.347(8) . ? F524 C52 1.337(7) . ? F621 C62 1.323(6) . ? F622 C62 1.337(6) . ? F623 C62 1.328(5) . ? O41 C41 1.269(5) . ? O44 C44 1.263(6) . ? O51 C51 1.264(6) . ? O54 C54 1.265(6) . ? O61 C61 1.273(5) . ? O64 C64 1.256(5) . ? O71 C71 1.145(5) . ? O81 C81 1.139(6) . ? O91 C91 1.147(6) . ? N11 C16 1.341(6) . ? N11 C12 1.356(5) . ? N21 C26 1.326(5) . ? N21 C22 1.356(5) . ? N24 C25 1.336(5) . ? N24 C23 1.363(5) . ? N31 C36 1.352(5) . ? N31 C32 1.361(5) . ? C12 C13 1.385(6) . ? C12 C22 1.478(6) . ? C13 C14 1.372(6) . ? C13 H13A 0.9500 . ? C14 C15 1.379(7) . ? C14 H14A 0.9500 . ? C15 C16 1.382(7) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C22 C23 1.399(6) . ? C23 C32 1.478(6) . ? C25 C26 1.386(6) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C32 C33 1.393(6) . ? C33 C34 1.381(6) . ? C33 H33A 0.9500 . ? C34 C35 1.380(7) . ? C34 H34A 0.9500 . ? C35 C36 1.379(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C43 1.367(7) . ? C41 C42 1.532(7) . ? C43 C44 1.420(7) . ? C43 H43A 0.9500 . ? C44 C45 1.464(7) . ? C45 C49 1.372(7) . ? C45 S46 1.720(5) . ? C47 C48 1.335(8) . ? C47 S46 1.714(6) . ? C47 H47 0.9500 . ? C48 C49 1.400(7) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C51 C53 1.376(7) . ? C51 C52 1.544(8) . ? C53 C54 1.408(7) . ? C53 H53A 0.9500 . ? C54 C55 1.476(6) . ? C55 C59 1.471(6) . ? C55 S56 1.692(5) . ? C57 C58 1.334(9) . ? C57 S56 1.690(6) . ? C57 H57 0.9500 . ? C58 C59 1.408(7) . ? C58 H58A 0.9500 . ? C59 H59 0.9500 . ? C61 C63 1.372(6) . ? C61 C62 1.527(6) . ? C63 C64 1.424(6) . ? C63 H63A 0.9500 . ? C64 C65 1.462(6) . ? C65 C69 1.366(6) . ? C65 S66 1.724(4) . ? C67 C68 1.338(7) . ? C67 S66 1.701(5) . ? C67 H67 0.9500 . ? C68 C69 1.409(6) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? 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 O61 Gd1 O44 86.81(12) . . ? O61 Gd1 O54 108.31(12) . . ? O44 Gd1 O54 136.75(11) . . ? O61 Gd1 O41 79.92(11) . . ? O44 Gd1 O41 72.77(11) . . ? O54 Gd1 O41 148.28(11) . . ? O61 Gd1 O64 72.44(10) . . ? O44 Gd1 O64 73.15(12) . . ? O54 Gd1 O64 73.50(11) . . ? O41 Gd1 O64 136.80(11) . . ? O61 Gd1 O51 85.07(11) . . ? O44 Gd1 O51 150.22(11) . . ? O54 Gd1 O51 72.83(11) . . ? O41 Gd1 O51 77.61(12) . . ? O64 Gd1 O51 130.53(12) . . ? O61 Gd1 N11 152.96(11) . . ? O44 Gd1 N11 103.97(13) . . ? O54 Gd1 N11 80.92(12) . . ? O41 Gd1 N11 79.80(11) . . ? O64 Gd1 N11 134.24(11) . . ? O51 Gd1 N11 73.24(12) . . ? O61 Gd1 N21 145.15(10) . . ? O44 Gd1 N21 73.50(11) . . ? O54 Gd1 N21 71.60(11) . . ? O41 Gd1 N21 119.22(11) . . ? O64 Gd1 N21 74.42(11) . . ? O51 Gd1 N21 125.60(11) . . ? N11 Gd1 N21 61.62(11) . . ? C91 Re1 C71 87.6(2) . . ? C91 Re1 C81 91.5(2) . . ? C71 Re1 C81 91.5(2) . . ? C91 Re1 N31 172.62(17) . . ? C71 Re1 N31 99.09(17) . . ? C81 Re1 N31 91.54(17) . . ? C91 Re1 N24 98.43(17) . . ? C71 Re1 N24 170.25(17) . . ? C81 Re1 N24 96.04(16) . . ? N31 Re1 N24 74.55(13) . . ? C91 Re1 Cl1 93.08(17) . . ? C71 Re1 Cl1 89.24(15) . . ? C81 Re1 Cl1 175.41(15) . . ? N31 Re1 Cl1 83.88(10) . . ? N24 Re1 Cl1 82.79(10) . . ? C41 O41 Gd1 131.2(3) . . ? C44 O44 Gd1 134.0(3) . . ? C51 O51 Gd1 130.8(3) . . ? C54 O54 Gd1 136.0(3) . . ? C61 O61 Gd1 132.4(3) . . ? C64 O64 Gd1 135.6(3) . . ? C16 N11 C12 116.6(4) . . ? C16 N11 Gd1 121.3(3) . . ? C12 N11 Gd1 122.0(3) . . ? C26 N21 C22 118.4(4) . . ? C26 N21 Gd1 121.8(3) . . ? C22 N21 Gd1 112.7(3) . . ? C25 N24 C23 118.8(4) . . ? C25 N24 Re1 124.8(3) . . ? C23 N24 Re1 115.6(3) . . ? C36 N31 C32 118.7(4) . . ? C36 N31 Re1 123.8(3) . . ? C32 N31 Re1 117.4(3) . . ? N11 C12 C13 122.6(4) . . ? N11 C12 C22 114.7(4) . . ? C13 C12 C22 122.3(4) . . ? C14 C13 C12 119.2(4) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C15 119.1(4) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? C14 C15 C16 118.4(4) . . ? C14 C15 H15A 120.8 . . ? C16 C15 H15A 120.8 . . ? N11 C16 C15 123.8(4) . . ? N11 C16 H16A 118.1 . . ? C15 C16 H16A 118.1 . . ? N21 C22 C23 120.2(4) . . ? N21 C22 C12 114.3(4) . . ? C23 C22 C12 125.3(4) . . ? N24 C23 C22 119.0(4) . . ? N24 C23 C32 114.5(4) . . ? C22 C23 C32 126.4(4) . . ? N24 C25 C26 120.6(4) . . ? N24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? N21 C26 C25 121.3(4) . . ? N21 C26 H26A 119.4 . . ? C25 C26 H26A 119.4 . . ? N31 C32 C33 120.7(4) . . ? N31 C32 C23 114.4(4) . . ? C33 C32 C23 124.6(4) . . ? C34 C33 C32 119.9(4) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C35 C34 C33 119.1(4) . . ? C35 C34 H34A 120.4 . . ? C33 C34 H34A 120.4 . . ? C36 C35 C34 119.0(4) . . ? C36 C35 H35A 120.5 . . ? C34 C35 H35A 120.5 . . ? N31 C36 C35 122.5(4) . . ? N31 C36 H36A 118.7 . . ? C35 C36 H36A 118.7 . . ? O41 C41 C43 129.0(5) . . ? O41 C41 C42 114.4(4) . . ? C43 C41 C42 116.6(4) . . ? F422 C42 F421 106.9(5) . . ? F422 C42 F423 106.5(5) . . ? F421 C42 F423 106.9(5) . . ? F422 C42 C41 112.5(5) . . ? F421 C42 C41 110.9(5) . . ? F423 C42 C41 112.8(5) . . ? C41 C43 C44 123.1(5) . . ? C41 C43 H43A 118.4 . . ? C44 C43 H43A 118.4 . . ? O44 C44 C43 123.1(4) . . ? O44 C44 C45 117.8(4) . . ? C43 C44 C45 119.1(4) . . ? C49 C45 C44 130.7(5) . . ? C49 C45 S46 110.9(4) . . ? C44 C45 S46 118.2(4) . . ? C48 C47 S46 112.5(4) . . ? C48 C47 H47 123.8 . . ? S46 C47 H47 123.8 . . ? C47 C48 C49 113.0(5) . . ? C47 C48 H48A 123.5 . . ? C49 C48 H48A 123.5 . . ? C45 C49 C48 112.6(5) . . ? C45 C49 H49A 123.7 . . ? C48 C49 H49A 123.7 . . ? O51 C51 C53 129.3(5) . . ? O51 C51 C52 114.4(4) . . ? C53 C51 C52 116.2(5) . . ? F521 C52 F524 107.6(5) . . ? F521 C52 F523 106.7(6) . . ? F524 C52 F523 106.3(6) . . ? F521 C52 C51 113.7(5) . . ? F524 C52 C51 112.8(5) . . ? F523 C52 C51 109.3(5) . . ? C51 C53 C54 122.8(5) . . ? C51 C53 H53A 118.6 . . ? C54 C53 H53A 118.6 . . ? O54 C54 C53 124.4(4) . . ? O54 C54 C55 117.1(4) . . ? C53 C54 C55 118.4(4) . . ? C59 C55 C54 128.0(4) . . ? C59 C55 S56 112.0(3) . . ? C54 C55 S56 119.8(4) . . ? C58 C57 S56 113.3(4) . . ? C58 C57 H57 123.3 . . ? S56 C57 H57 123.3 . . ? C57 C58 C59 115.6(5) . . ? C57 C58 H58A 122.2 . . ? C59 C58 H58A 122.2 . . ? C58 C59 C55 107.3(5) . . ? C58 C59 H59 126.4 . . ? C55 C59 H59 126.4 . . ? O61 C61 C63 129.3(4) . . ? O61 C61 C62 111.9(4) . . ? C63 C61 C62 118.8(4) . . ? F621 C62 F623 107.3(4) . . ? F621 C62 F622 106.1(4) . . ? F623 C62 F622 105.9(4) . . ? F621 C62 C61 112.0(4) . . ? F623 C62 C61 114.8(4) . . ? F622 C62 C61 110.3(4) . . ? C61 C63 C64 121.5(4) . . ? C61 C63 H63A 119.3 . . ? C64 C63 H63A 119.3 . . ? O64 C64 C63 123.7(4) . . ? O64 C64 C65 117.6(4) . . ? C63 C64 C65 118.6(4) . . ? C69 C65 C64 131.3(4) . . ? C69 C65 S66 110.1(3) . . ? C64 C65 S66 118.5(3) . . ? C68 C67 S66 112.0(4) . . ? C68 C67 H67 124.0 . . ? S66 C67 H67 124.0 . . ? C67 C68 C69 113.1(4) . . ? C67 C68 H68A 123.5 . . ? C69 C68 H68A 123.5 . . ? C65 C69 C68 112.8(4) . . ? C65 C69 H69A 123.6 . . ? C68 C69 H69A 123.6 . . ? O71 C71 Re1 176.9(5) . . ? O81 C81 Re1 176.7(4) . . ? O91 C91 Re1 178.0(5) . . ? C47 S46 C45 91.0(3) . . ? C57 S56 C55 91.8(3) . . ? C67 S66 C65 91.9(2) . . ? 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 O61 Gd1 O41 C41 -68.8(4) . . . . ? O44 Gd1 O41 C41 21.0(4) . . . . ? O54 Gd1 O41 C41 -177.4(4) . . . . ? O64 Gd1 O41 C41 -18.4(5) . . . . ? O51 Gd1 O41 C41 -155.9(4) . . . . ? N11 Gd1 O41 C41 129.2(4) . . . . ? N21 Gd1 O41 C41 80.0(4) . . . . ? O61 Gd1 O44 C44 51.4(4) . . . . ? O54 Gd1 O44 C44 165.0(4) . . . . ? O41 Gd1 O44 C44 -29.0(4) . . . . ? O64 Gd1 O44 C44 124.0(4) . . . . ? O51 Gd1 O44 C44 -22.9(6) . . . . ? N11 Gd1 O44 C44 -103.5(4) . . . . ? N21 Gd1 O44 C44 -157.7(5) . . . . ? O61 Gd1 O51 C51 130.2(5) . . . . ? O44 Gd1 O51 C51 -155.0(4) . . . . ? O54 Gd1 O51 C51 19.3(4) . . . . ? O41 Gd1 O51 C51 -149.0(5) . . . . ? O64 Gd1 O51 C51 68.4(5) . . . . ? N11 Gd1 O51 C51 -66.1(4) . . . . ? N21 Gd1 O51 C51 -31.8(5) . . . . ? O61 Gd1 O54 C54 -97.5(4) . . . . ? O44 Gd1 O54 C54 157.1(4) . . . . ? O41 Gd1 O54 C54 3.2(5) . . . . ? O64 Gd1 O54 C54 -162.0(4) . . . . ? O51 Gd1 O54 C54 -18.8(4) . . . . ? N11 Gd1 O54 C54 56.3(4) . . . . ? N21 Gd1 O54 C54 119.3(4) . . . . ? O44 Gd1 O61 C61 49.8(4) . . . . ? O54 Gd1 O61 C61 -88.8(4) . . . . ? O41 Gd1 O61 C61 122.9(4) . . . . ? O64 Gd1 O61 C61 -23.5(4) . . . . ? O51 Gd1 O61 C61 -158.9(4) . . . . ? N11 Gd1 O61 C61 164.8(4) . . . . ? N21 Gd1 O61 C61 -4.9(5) . . . . ? O61 Gd1 O64 C64 18.1(4) . . . . ? O44 Gd1 O64 C64 -73.9(4) . . . . ? O54 Gd1 O64 C64 134.0(5) . . . . ? O41 Gd1 O64 C64 -34.7(5) . . . . ? O51 Gd1 O64 C64 85.2(5) . . . . ? N11 Gd1 O64 C64 -167.2(4) . . . . ? N21 Gd1 O64 C64 -151.0(5) . . . . ? O61 Gd1 N11 C16 -11.2(5) . . . . ? O44 Gd1 N11 C16 100.0(4) . . . . ? O54 Gd1 N11 C16 -123.9(4) . . . . ? O41 Gd1 N11 C16 30.8(4) . . . . ? O64 Gd1 N11 C16 179.9(3) . . . . ? O51 Gd1 N11 C16 -49.2(4) . . . . ? N21 Gd1 N11 C16 162.1(4) . . . . ? O61 Gd1 N11 C12 171.8(3) . . . . ? O44 Gd1 N11 C12 -77.0(4) . . . . ? O54 Gd1 N11 C12 59.1(3) . . . . ? O41 Gd1 N11 C12 -146.2(4) . . . . ? O64 Gd1 N11 C12 2.9(4) . . . . ? O51 Gd1 N11 C12 133.8(4) . . . . ? N21 Gd1 N11 C12 -14.9(3) . . . . ? O61 Gd1 N21 C26 -5.1(4) . . . . ? O44 Gd1 N21 C26 -63.3(3) . . . . ? O54 Gd1 N21 C26 90.7(3) . . . . ? O41 Gd1 N21 C26 -122.0(3) . . . . ? O64 Gd1 N21 C26 13.3(3) . . . . ? O51 Gd1 N21 C26 142.4(3) . . . . ? N11 Gd1 N21 C26 -179.8(4) . . . . ? O61 Gd1 N21 C22 -155.0(3) . . . . ? O44 Gd1 N21 C22 146.8(3) . . . . ? O54 Gd1 N21 C22 -59.2(3) . . . . ? O41 Gd1 N21 C22 88.1(3) . . . . ? O64 Gd1 N21 C22 -136.6(3) . . . . ? O51 Gd1 N21 C22 -7.6(3) . . . . ? N11 Gd1 N21 C22 30.3(3) . . . . ? C91 Re1 N24 C25 7.9(4) . . . . ? C71 Re1 N24 C25 135.4(10) . . . . ? C81 Re1 N24 C25 -84.5(4) . . . . ? N31 Re1 N24 C25 -174.4(4) . . . . ? Cl1 Re1 N24 C25 100.0(4) . . . . ? C91 Re1 N24 C23 -161.9(3) . . . . ? C71 Re1 N24 C23 -34.4(12) . . . . ? C81 Re1 N24 C23 105.7(3) . . . . ? N31 Re1 N24 C23 15.8(3) . . . . ? Cl1 Re1 N24 C23 -69.8(3) . . . . ? C91 Re1 N31 C36 -173.4(13) . . . . ? C71 Re1 N31 C36 -19.2(4) . . . . ? C81 Re1 N31 C36 72.6(4) . . . . ? N24 Re1 N31 C36 168.4(4) . . . . ? Cl1 Re1 N31 C36 -107.4(4) . . . . ? C91 Re1 N31 C32 10.5(16) . . . . ? C71 Re1 N31 C32 164.7(3) . . . . ? C81 Re1 N31 C32 -103.5(3) . . . . ? N24 Re1 N31 C32 -7.7(3) . . . . ? Cl1 Re1 N31 C32 76.5(3) . . . . ? C16 N11 C12 C13 -5.3(7) . . . . ? Gd1 N11 C12 C13 171.8(3) . . . . ? C16 N11 C12 C22 -178.0(4) . . . . ? Gd1 N11 C12 C22 -0.8(5) . . . . ? N11 C12 C13 C14 4.4(7) . . . . ? C22 C12 C13 C14 176.5(4) . . . . ? C12 C13 C14 C15 0.7(8) . . . . ? C13 C14 C15 C16 -4.5(8) . . . . ? C12 N11 C16 C15 1.2(8) . . . . ? Gd1 N11 C16 C15 -175.9(4) . . . . ? C14 C15 C16 N11 3.6(9) . . . . ? C26 N21 C22 C23 -10.8(6) . . . . ? Gd1 N21 C22 C23 140.2(3) . . . . ? C26 N21 C22 C12 165.0(4) . . . . ? Gd1 N21 C22 C12 -44.0(4) . . . . ? N11 C12 C22 N21 31.0(6) . . . . ? C13 C12 C22 N21 -141.7(4) . . . . ? N11 C12 C22 C23 -153.4(4) . . . . ? C13 C12 C22 C23 33.9(7) . . . . ? C25 N24 C23 C22 -7.5(6) . . . . ? Re1 N24 C23 C22 163.0(3) . . . . ? C25 N24 C23 C32 168.2(4) . . . . ? Re1 N24 C23 C32 -21.4(5) . . . . ? N21 C22 C23 N24 15.2(6) . . . . ? C12 C22 C23 N24 -160.1(4) . . . . ? N21 C22 C23 C32 -159.9(4) . . . . ? C12 C22 C23 C32 24.8(7) . . . . ? C23 N24 C25 C26 -4.0(6) . . . . ? Re1 N24 C25 C26 -173.5(3) . . . . ? C22 N21 C26 C25 -0.9(7) . . . . ? Gd1 N21 C26 C25 -149.2(3) . . . . ? N24 C25 C26 N21 8.6(7) . . . . ? C36 N31 C32 C33 -3.5(6) . . . . ? Re1 N31 C32 C33 172.8(3) . . . . ? C36 N31 C32 C23 -177.1(4) . . . . ? Re1 N31 C32 C23 -0.8(5) . . . . ? N24 C23 C32 N31 14.5(5) . . . . ? C22 C23 C32 N31 -170.2(4) . . . . ? N24 C23 C32 C33 -158.7(4) . . . . ? C22 C23 C32 C33 16.6(7) . . . . ? N31 C32 C33 C34 3.6(7) . . . . ? C23 C32 C33 C34 176.5(4) . . . . ? C32 C33 C34 C35 -1.2(7) . . . . ? C33 C34 C35 C36 -1.3(8) . . . . ? C32 N31 C36 C35 1.1(7) . . . . ? Re1 N31 C36 C35 -175.0(4) . . . . ? C34 C35 C36 N31 1.4(8) . . . . ? Gd1 O41 C41 C43 -13.7(8) . . . . ? Gd1 O41 C41 C42 164.1(4) . . . . ? O41 C41 C42 F422 32.8(7) . . . . ? C43 C41 C42 F422 -149.2(5) . . . . ? O41 C41 C42 F421 -86.9(5) . . . . ? C43 C41 C42 F421 91.2(6) . . . . ? O41 C41 C42 F423 153.3(5) . . . . ? C43 C41 C42 F423 -28.6(8) . . . . ? O41 C41 C43 C44 -1.6(9) . . . . ? C42 C41 C43 C44 -179.4(5) . . . . ? Gd1 O44 C44 C43 27.8(7) . . . . ? Gd1 O44 C44 C45 -150.5(3) . . . . ? C41 C43 C44 O44 -4.7(8) . . . . ? C41 C43 C44 C45 173.5(5) . . . . ? O44 C44 C45 C49 170.7(5) . . . . ? C43 C44 C45 C49 -7.6(8) . . . . ? O44 C44 C45 S46 -3.5(6) . . . . ? C43 C44 C45 S46 178.1(4) . . . . ? S46 C47 C48 C49 0.0(7) . . . . ? C44 C45 C49 C48 -174.8(5) . . . . ? S46 C45 C49 C48 -0.3(6) . . . . ? C47 C48 C49 C45 0.2(7) . . . . ? Gd1 O51 C51 C53 -18.4(9) . . . . ? Gd1 O51 C51 C52 157.3(4) . . . . ? O51 C51 C52 F521 31.3(8) . . . . ? C53 C51 C52 F521 -152.5(6) . . . . ? O51 C51 C52 F524 154.1(5) . . . . ? C53 C51 C52 F524 -29.6(8) . . . . ? O51 C51 C52 F523 -87.8(6) . . . . ? C53 C51 C52 F523 88.4(6) . . . . ? O51 C51 C53 C54 3.9(9) . . . . ? C52 C51 C53 C54 -171.6(5) . . . . ? Gd1 O54 C54 C53 15.1(7) . . . . ? Gd1 O54 C54 C55 -161.4(3) . . . . ? C51 C53 C54 O54 -1.4(8) . . . . ? C51 C53 C54 C55 175.1(5) . . . . ? O54 C54 C55 C59 171.4(4) . . . . ? C53 C54 C55 C59 -5.3(7) . . . . ? O54 C54 C55 S56 -3.6(6) . . . . ? C53 C54 C55 S56 179.7(4) . . . . ? S56 C57 C58 C59 0.7(7) . . . . ? C57 C58 C59 C55 -1.6(7) . . . . ? C54 C55 C59 C58 -173.6(5) . . . . ? S56 C55 C59 C58 1.8(5) . . . . ? Gd1 O61 C61 C63 20.5(7) . . . . ? Gd1 O61 C61 C62 -161.7(3) . . . . ? O61 C61 C62 F621 -60.3(6) . . . . ? C63 C61 C62 F621 117.7(5) . . . . ? O61 C61 C62 F623 177.0(4) . . . . ? C63 C61 C62 F623 -4.9(7) . . . . ? O61 C61 C62 F622 57.6(6) . . . . ? C63 C61 C62 F622 -124.4(5) . . . . ? O61 C61 C63 C64 2.6(8) . . . . ? C62 C61 C63 C64 -175.0(4) . . . . ? Gd1 O64 C64 C63 -7.6(7) . . . . ? Gd1 O64 C64 C65 173.2(3) . . . . ? C61 C63 C64 O64 -9.0(7) . . . . ? C61 C63 C64 C65 170.3(4) . . . . ? O64 C64 C65 C69 168.8(5) . . . . ? C63 C64 C65 C69 -10.5(8) . . . . ? O64 C64 C65 S66 -8.6(6) . . . . ? C63 C64 C65 S66 172.1(4) . . . . ? S66 C67 C68 C69 1.2(6) . . . . ? C64 C65 C69 C68 -178.8(5) . . . . ? S66 C65 C69 C68 -1.2(6) . . . . ? C67 C68 C69 C65 0.1(7) . . . . ? C91 Re1 C71 O71 105(9) . . . . ? C81 Re1 C71 O71 -163(9) . . . . ? N31 Re1 C71 O71 -72(9) . . . . ? N24 Re1 C71 O71 -23(10) . . . . ? Cl1 Re1 C71 O71 12(9) . . . . ? C91 Re1 C81 O81 78(8) . . . . ? C71 Re1 C81 O81 -10(8) . . . . ? N31 Re1 C81 O81 -109(8) . . . . ? N24 Re1 C81 O81 176(100) . . . . ? Cl1 Re1 C81 O81 -109(8) . . . . ? C71 Re1 C91 O91 166(15) . . . . ? C81 Re1 C91 O91 74(15) . . . . ? N31 Re1 C91 O91 -40(16) . . . . ? N24 Re1 C91 O91 -22(15) . . . . ? Cl1 Re1 C91 O91 -105(15) . . . . ? C48 C47 S46 C45 -0.1(5) . . . . ? C49 C45 S46 C47 0.2(4) . . . . ? C44 C45 S46 C47 175.5(4) . . . . ? C58 C57 S56 C55 0.3(5) . . . . ? C59 C55 S56 C57 -1.2(4) . . . . ? C54 C55 S56 C57 174.5(4) . . . . ? C68 C67 S66 C65 -1.6(5) . . . . ? C69 C65 S66 C67 1.6(4) . . . . ? C64 C65 S66 C67 179.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.326 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.127 #===END