Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Mike Ward' 'Zoe R. Bell' 'Stephen Faulkner' 'Simon J. A. Pope' 'Nail M. Shavaleev' _publ_contact_author_name 'Prof Mike Ward' _publ_contact_author_address ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email MIKE.WARD@BRISTOL.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Efficient visible-light sensitisation of near-infrared luminescence from Yb(III), Nd(III) and Er(III) complexes of 3,6-bis(2-pyridyl)tetrazine ; #======================================================= data_jedis _database_code_CSD 200935 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30.50 H17 Cl F9 N3 O6 S3 Yb' _chemical_formula_weight 997.14 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' Yb Yb -0.3850 5.5486 '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' _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 10.335(7) _cell_length_b 19.431(10) _cell_length_c 19.085(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.22(7) _cell_angle_gamma 90.00 _cell_volume 3698(4) _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 needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 2.861 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.41 _exptl_absorpt_correction_T_max 0.85 _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 (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19988 _diffrn_reflns_av_R_equivalents 0.1887 _diffrn_reflns_av_sigmaI/netI 0.2051 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6516 _reflns_number_gt 3069 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0810P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6516 _refine_ls_number_parameters 492 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1728 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.1932 _refine_ls_wR_factor_gt 0.1495 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.078 _refine_ls_shift/su_mean 0.003 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 Yb1 Yb 0.94415(7) 0.81681(3) 0.07147(3) 0.0367(3) Uani 1 1 d . . . S16 S 0.7494(4) 0.8122(2) 0.2864(2) 0.0556(11) Uani 1 1 d . . . S26 S 1.3478(5) 0.7814(3) -0.0125(3) 0.0654(13) Uani 1 1 d . . . S36 S 1.2718(7) 0.6288(3) 0.1698(3) 0.0996(19) Uani 1 1 d U . . F121 F 1.3965(10) 0.8590(8) 0.3034(6) 0.127(6) Uani 1 1 d . . . F122 F 1.4038(10) 0.8274(6) 0.1992(7) 0.097(4) Uani 1 1 d . . . F123 F 1.3668(9) 0.9317(5) 0.2179(5) 0.068(3) Uani 1 1 d . . . F221 F 0.7009(13) 0.9437(6) -0.1304(6) 0.103(4) Uani 1 1 d . . . F222 F 0.6388(10) 0.8524(6) -0.1863(6) 0.093(4) Uani 1 1 d . . . F223 F 0.7834(10) 0.9133(6) -0.2143(5) 0.075(3) Uani 1 1 d . . . F321 F 0.5595(10) 0.6512(5) 0.0302(6) 0.078(3) Uani 1 1 d . . . F322 F 0.5614(11) 0.7156(6) 0.1207(6) 0.084(3) Uani 1 1 d . . . F323 F 0.6197(10) 0.6100(6) 0.1366(6) 0.084(3) Uani 1 1 d . . . O11 O 1.1393(11) 0.8541(5) 0.1442(6) 0.047(3) Uani 1 1 d . . . O14 O 0.9129(10) 0.8205(5) 0.1856(5) 0.042(2) Uani 1 1 d . . . O21 O 0.8174(10) 0.8391(5) -0.0450(5) 0.041(3) Uani 1 1 d . . . O24 O 1.0765(9) 0.7941(5) -0.0017(5) 0.042(3) Uani 1 1 d . . . O31 O 0.7720(10) 0.7435(5) 0.0654(5) 0.044(3) Uani 1 1 d . . . O34 O 1.0435(11) 0.7156(5) 0.1114(5) 0.046(3) Uani 1 1 d . . . N41 N 0.9905(11) 0.9374(5) 0.0304(5) 0.028(3) Uani 1 1 d . . . N42 N 1.0974(11) 0.9499(6) 0.0050(6) 0.036(3) Uani 1 1 d . . . N51 N 0.7728(12) 0.9075(6) 0.0769(6) 0.036(3) Uani 1 1 d . . . C11 C 1.1887(17) 0.8547(9) 0.2114(10) 0.056(5) Uani 1 1 d . . . C12 C 1.3395(19) 0.8670(10) 0.2335(11) 0.061(5) Uani 1 1 d . . . C13 C 1.1204(16) 0.8433(8) 0.2658(8) 0.049(4) Uani 1 1 d . . . H13A H 1.1701 0.8438 0.3153 0.059 Uiso 1 1 calc R . . C14 C 0.9843(16) 0.8316(7) 0.2492(8) 0.041(4) Uani 1 1 d . . . C15 C 0.9153(15) 0.8311(7) 0.3080(8) 0.042(4) Uani 1 1 d . . . C17 C 0.7486(19) 0.8225(8) 0.3743(8) 0.055(4) Uani 1 1 d . . . H17 H 0.6707 0.8158 0.3911 0.066 Uiso 1 1 calc R . . C18 C 0.8690(19) 0.8412(8) 0.4190(9) 0.056(5) Uani 1 1 d . . . H18 H 0.8835 0.8494 0.4696 0.067 Uiso 1 1 calc R . . C19 C 0.9697(16) 0.8471(7) 0.3821(7) 0.037(4) Uani 1 1 d . . . H19A H 1.0601 0.8598 0.4035 0.044 Uiso 1 1 calc R . . C21 C 0.8533(14) 0.8519(7) -0.1016(7) 0.030(3) Uani 1 1 d . . . C22 C 0.7490(19) 0.8898(10) -0.1585(9) 0.059(5) Uani 1 1 d . . . C23 C 0.9712(16) 0.8389(8) -0.1165(9) 0.049(4) Uani 1 1 d . . . H23A H 0.9799 0.8494 -0.1637 0.059 Uiso 1 1 calc R . . C24 C 1.0837(13) 0.8103(7) -0.0649(8) 0.041(4) Uani 1 1 d . . . C25 C 1.2109(14) 0.8029(6) -0.0834(7) 0.036(4) Uani 1 1 d . . . C27 C 1.4542(19) 0.7855(9) -0.0685(10) 0.063(5) Uani 1 1 d . . . H27 H 1.5481 0.7776 -0.0535 0.076 Uiso 1 1 calc R . . C28 C 1.3833(17) 0.8021(8) -0.1381(9) 0.056(5) Uani 1 1 d . . . H28A H 1.4274 0.8065 -0.1757 0.067 Uiso 1 1 calc R . . C29 C 1.2397(13) 0.8125(7) -0.1527(7) 0.033(3) Uani 1 1 d . . . H29 H 1.1783 0.8232 -0.1979 0.040 Uiso 1 1 calc R . . C31 C 0.7682(16) 0.6872(9) 0.0986(7) 0.042(4) Uani 1 1 d . . . C33 C 0.8718(18) 0.6463(8) 0.1339(8) 0.053(5) Uani 1 1 d . . . H33A H 0.8522 0.6059 0.1571 0.064 Uiso 1 1 calc R . . C32 C 0.6253(19) 0.6662(9) 0.0973(9) 0.058(5) Uani 1 1 d . . . C34 C 1.0087(17) 0.6613(8) 0.1376(8) 0.043(4) Uani 1 1 d . . . C35 C 1.1128(15) 0.6085(8) 0.1680(7) 0.045(4) Uani 1 1 d U . . C37 C 1.325(2) 0.5533(11) 0.2070(9) 0.090(8) Uani 1 1 d U . . H37 H 1.4147 0.5369 0.2210 0.108 Uiso 1 1 calc R . . C38 C 1.206(4) 0.5174(13) 0.2138(14) 0.177(18) Uani 1 1 d U . . H38A H 1.2195 0.4723 0.2336 0.213 Uiso 1 1 calc R . . C39 C 1.0891(13) 0.5378(7) 0.1972(7) 0.022(3) Uiso 1 1 d . . . H39 H 1.0089 0.5163 0.2013 0.027 Uiso 1 1 calc R . . C42 C 0.9020(14) 0.9876(7) 0.0264(7) 0.032(4) Uani 1 1 d . . . C52 C 0.7828(14) 0.9733(7) 0.0548(7) 0.036(4) Uani 1 1 d . . . C53 C 0.6939(14) 1.0246(8) 0.0593(8) 0.046(4) Uani 1 1 d . . . H53A H 0.7079 1.0706 0.0459 0.055 Uiso 1 1 calc R . . C54 C 0.5816(15) 1.0073(9) 0.0841(9) 0.053(4) Uani 1 1 d . . . H54A H 0.5143 1.0403 0.0852 0.064 Uiso 1 1 calc R . . C55 C 0.5731(16) 0.9404(9) 0.1069(8) 0.051(4) Uani 1 1 d . . . H55A H 0.5016 0.9269 0.1266 0.061 Uiso 1 1 calc R . . C56 C 0.6671(15) 0.8943(8) 0.1010(7) 0.040(4) Uani 1 1 d . . . H56A H 0.6561 0.8483 0.1154 0.048 Uiso 1 1 calc R . . C100 C 0.693(4) 0.030(3) 0.504(2) 0.096(16) Uani 0.50 1 d P . . H10A H 0.6597 0.0681 0.4701 0.115 Uiso 0.50 1 calc PR . . H10B H 0.6372 -0.0108 0.4851 0.115 Uiso 0.50 1 calc PR . . Cl11 Cl 0.8536(15) 0.0114(5) 0.4983(6) 0.100(4) Uani 0.50 1 d P . . Cl12 Cl 0.6637(11) 0.0491(6) 0.5768(5) 0.088(3) Uani 0.50 1 d P . . 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 Yb1 0.0440(4) 0.0366(4) 0.0350(4) 0.0065(4) 0.0199(3) -0.0011(4) S16 0.057(3) 0.068(3) 0.048(2) 0.004(3) 0.025(2) -0.008(3) S26 0.063(3) 0.070(3) 0.067(3) 0.007(3) 0.024(3) 0.013(3) S36 0.100(5) 0.102(5) 0.095(4) 0.005(4) 0.022(4) 0.018(4) F121 0.046(7) 0.251(17) 0.073(8) 0.079(10) -0.005(6) -0.040(9) F122 0.045(6) 0.078(8) 0.168(12) -0.020(8) 0.030(7) -0.005(6) F123 0.048(6) 0.071(7) 0.087(7) 0.001(6) 0.021(5) -0.010(5) F221 0.147(11) 0.101(9) 0.067(7) 0.030(7) 0.040(7) 0.080(9) F222 0.044(7) 0.115(9) 0.104(9) 0.043(8) -0.011(6) -0.018(7) F223 0.061(7) 0.118(9) 0.054(6) 0.034(6) 0.028(5) 0.030(6) F321 0.069(7) 0.083(7) 0.072(7) 0.018(6) 0.000(6) -0.020(6) F322 0.070(8) 0.092(8) 0.109(9) 0.004(7) 0.056(7) 0.000(7) F323 0.057(7) 0.099(8) 0.091(8) 0.047(7) 0.011(6) -0.029(6) O11 0.058(8) 0.048(7) 0.039(7) 0.006(6) 0.018(6) -0.004(6) O14 0.055(6) 0.047(6) 0.026(5) 0.000(5) 0.015(5) -0.007(6) O21 0.045(6) 0.044(6) 0.040(6) 0.007(5) 0.021(5) 0.001(5) O24 0.042(6) 0.054(7) 0.036(6) 0.004(5) 0.021(5) 0.003(5) O31 0.056(7) 0.044(6) 0.035(6) 0.017(5) 0.020(5) 0.002(5) O34 0.065(8) 0.036(6) 0.042(6) 0.002(5) 0.023(6) -0.015(6) N41 0.029(7) 0.022(6) 0.032(6) 0.001(5) 0.007(5) 0.005(5) N42 0.036(7) 0.043(7) 0.035(7) 0.011(6) 0.021(6) -0.003(6) N51 0.042(8) 0.034(7) 0.041(7) 0.002(6) 0.026(6) 0.000(6) C11 0.052(12) 0.051(11) 0.070(13) 0.012(10) 0.026(10) -0.004(9) C12 0.061(13) 0.055(13) 0.071(14) 0.016(11) 0.023(11) 0.006(11) C13 0.045(11) 0.057(11) 0.038(9) 0.012(8) -0.001(8) -0.007(9) C14 0.042(10) 0.041(10) 0.042(9) 0.022(8) 0.015(8) -0.001(8) C15 0.052(10) 0.040(10) 0.043(9) 0.001(7) 0.024(8) 0.003(8) C17 0.074(13) 0.049(10) 0.053(10) 0.021(10) 0.036(10) 0.011(11) C18 0.067(13) 0.063(12) 0.043(10) 0.002(9) 0.024(10) 0.006(10) C19 0.056(10) 0.031(8) 0.027(8) 0.000(7) 0.019(7) -0.002(7) C21 0.026(8) 0.037(8) 0.026(8) -0.008(7) 0.002(7) -0.001(7) C22 0.067(13) 0.085(14) 0.037(10) 0.010(10) 0.034(10) 0.019(12) C23 0.046(11) 0.057(11) 0.050(10) 0.011(8) 0.023(8) 0.003(9) C24 0.035(10) 0.032(8) 0.058(10) -0.010(9) 0.014(8) -0.002(8) C25 0.037(9) 0.024(8) 0.045(9) 0.014(7) 0.012(7) 0.019(7) C27 0.054(12) 0.073(12) 0.073(13) -0.008(11) 0.035(10) 0.003(10) C28 0.057(11) 0.062(12) 0.057(11) 0.000(9) 0.029(9) -0.005(9) C29 0.027(8) 0.031(7) 0.051(9) -0.006(8) 0.026(7) -0.004(7) C31 0.052(10) 0.045(9) 0.029(8) -0.002(9) 0.010(7) -0.021(10) C33 0.070(13) 0.052(11) 0.042(10) 0.015(9) 0.023(9) -0.010(10) C32 0.068(13) 0.065(13) 0.037(10) 0.031(9) 0.006(9) -0.020(11) C34 0.056(11) 0.047(10) 0.029(9) -0.005(7) 0.012(8) -0.006(9) C35 0.033(9) 0.061(11) 0.034(9) 0.005(8) -0.006(7) -0.005(8) C37 0.117(18) 0.076(14) 0.049(12) -0.005(11) -0.025(12) 0.076(14) C38 0.39(5) 0.08(2) 0.10(2) -0.043(16) 0.13(3) -0.12(3) C42 0.039(9) 0.029(8) 0.032(8) -0.014(7) 0.016(7) -0.013(7) C52 0.035(9) 0.044(9) 0.037(9) -0.004(7) 0.027(7) -0.005(8) C53 0.036(9) 0.041(9) 0.076(12) -0.002(8) 0.039(9) -0.003(8) C54 0.036(10) 0.064(12) 0.064(11) 0.002(10) 0.022(9) 0.006(9) C55 0.044(10) 0.063(12) 0.060(11) -0.010(10) 0.036(9) -0.013(9) C56 0.043(10) 0.044(9) 0.038(9) 0.011(8) 0.021(8) 0.000(8) C100 0.05(3) 0.14(4) 0.08(3) 0.06(3) 0.00(2) -0.01(3) Cl11 0.173(13) 0.059(6) 0.063(7) -0.007(5) 0.020(7) 0.011(7) Cl12 0.093(8) 0.103(8) 0.052(6) 0.011(6) -0.009(5) -0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O24 2.239(9) . ? Yb1 O11 2.247(11) . ? Yb1 O34 2.257(10) . ? Yb1 O31 2.259(10) . ? Yb1 O14 2.286(8) . ? Yb1 O21 2.305(10) . ? Yb1 N51 2.520(11) . ? Yb1 N41 2.555(10) . ? S16 C17 1.693(15) . ? S16 C15 1.694(16) . ? S26 C27 1.725(16) . ? S26 C25 1.732(14) . ? S36 C37 1.661(19) . ? S36 C35 1.681(16) . ? F121 C12 1.32(2) . ? F122 C12 1.300(19) . ? F123 C12 1.339(18) . ? F221 C22 1.331(18) . ? F222 C22 1.34(2) . ? F223 C22 1.292(16) . ? F321 C32 1.316(18) . ? F322 C32 1.31(2) . ? F323 C32 1.335(16) . ? O11 C11 1.249(19) . ? O14 C14 1.262(16) . ? O21 C21 1.256(15) . ? O24 C24 1.268(16) . ? O31 C31 1.270(17) . ? O34 C34 1.259(16) . ? N41 C42 1.326(16) . ? N41 N42 1.340(14) . ? N42 C42 1.356(16) 3_775 ? N51 C56 1.317(16) . ? N51 C52 1.359(16) . ? C11 C13 1.42(2) . ? C11 C12 1.52(2) . ? C13 C14 1.38(2) . ? C14 C15 1.480(19) . ? C15 C19 1.411(19) . ? C17 C18 1.36(2) . ? C18 C19 1.41(2) . ? C21 C23 1.346(19) . ? C21 C22 1.51(2) . ? C23 C24 1.42(2) . ? C24 C25 1.455(18) . ? C25 C29 1.443(18) . ? C27 C28 1.38(2) . ? C28 C29 1.45(2) . ? C31 C33 1.36(2) . ? C31 C32 1.53(2) . ? C33 C34 1.43(2) . ? C34 C35 1.49(2) . ? C35 C39 1.53(2) . ? C37 C38 1.45(3) . ? C38 C39 1.23(4) . ? C42 N42 1.356(16) 3_775 ? C42 C52 1.496(17) . ? C52 C53 1.373(19) . ? C53 C54 1.405(19) . ? C54 C55 1.38(2) . ? C55 C56 1.35(2) . ? C100 Cl12 1.54(4) . ? C100 Cl11 1.73(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 O24 Yb1 O11 81.5(4) . . ? O24 Yb1 O34 74.9(3) . . ? O11 Yb1 O34 79.5(4) . . ? O24 Yb1 O31 116.4(3) . . ? O11 Yb1 O31 143.3(3) . . ? O34 Yb1 O31 75.5(4) . . ? O24 Yb1 O14 149.6(4) . . ? O11 Yb1 O14 74.3(4) . . ? O34 Yb1 O14 82.6(3) . . ? O31 Yb1 O14 76.2(3) . . ? O24 Yb1 O21 73.8(3) . . ? O11 Yb1 O21 136.5(3) . . ? O34 Yb1 O21 125.6(3) . . ? O31 Yb1 O21 80.1(3) . . ? O14 Yb1 O21 136.6(3) . . ? O24 Yb1 N51 135.6(3) . . ? O11 Yb1 N51 106.0(4) . . ? O34 Yb1 N51 149.1(3) . . ? O31 Yb1 N51 83.7(4) . . ? O14 Yb1 N51 70.3(4) . . ? O21 Yb1 N51 71.4(3) . . ? O24 Yb1 N41 78.2(3) . . ? O11 Yb1 N41 71.6(4) . . ? O34 Yb1 N41 142.9(4) . . ? O31 Yb1 N41 140.5(3) . . ? O14 Yb1 N41 110.4(3) . . ? O21 Yb1 N41 68.7(3) . . ? N51 Yb1 N41 64.0(3) . . ? C17 S16 C15 90.0(8) . . ? C27 S26 C25 91.6(8) . . ? C37 S36 C35 90.7(11) . . ? C11 O11 Yb1 134.1(10) . . ? C14 O14 Yb1 136.7(9) . . ? C21 O21 Yb1 130.2(9) . . ? C24 O24 Yb1 138.0(9) . . ? C31 O31 Yb1 130.1(10) . . ? C34 O34 Yb1 135.4(10) . . ? C42 N41 N42 117.9(11) . . ? C42 N41 Yb1 120.7(9) . . ? N42 N41 Yb1 121.1(8) . . ? N41 N42 C42 115.0(11) . 3_775 ? C56 N51 C52 115.4(12) . . ? C56 N51 Yb1 122.3(9) . . ? C52 N51 Yb1 122.3(8) . . ? O11 C11 C13 127.0(16) . . ? O11 C11 C12 113.5(14) . . ? C13 C11 C12 119.5(17) . . ? F122 C12 F121 106.7(16) . . ? F122 C12 F123 106.2(15) . . ? F121 C12 F123 105.8(16) . . ? F122 C12 C11 112.9(16) . . ? F121 C12 C11 114.5(15) . . ? F123 C12 C11 110.3(15) . . ? C14 C13 C11 122.2(15) . . ? O14 C14 C13 123.6(13) . . ? O14 C14 C15 116.8(13) . . ? C13 C14 C15 119.6(14) . . ? C19 C15 C14 127.8(14) . . ? C19 C15 S16 113.8(11) . . ? C14 C15 S16 118.3(11) . . ? C18 C17 S16 114.3(13) . . ? C17 C18 C19 112.5(15) . . ? C18 C19 C15 109.4(15) . . ? O21 C21 C23 129.2(14) . . ? O21 C21 C22 113.6(12) . . ? C23 C21 C22 117.1(13) . . ? F223 C22 F221 105.5(15) . . ? F223 C22 F222 104.8(14) . . ? F221 C22 F222 102.6(15) . . ? F223 C22 C21 117.9(15) . . ? F221 C22 C21 111.5(14) . . ? F222 C22 C21 113.2(15) . . ? C21 C23 C24 123.2(14) . . ? O24 C24 C23 120.9(13) . . ? O24 C24 C25 119.3(13) . . ? C23 C24 C25 119.7(14) . . ? C29 C25 C24 128.9(13) . . ? C29 C25 S26 115.1(10) . . ? C24 C25 S26 116.0(11) . . ? C28 C27 S26 110.1(13) . . ? C27 C28 C29 118.5(14) . . ? C25 C29 C28 104.6(13) . . ? O31 C31 C33 128.8(14) . . ? O31 C31 C32 112.2(14) . . ? C33 C31 C32 119.0(14) . . ? C31 C33 C34 123.1(14) . . ? F322 C32 F321 108.5(16) . . ? F322 C32 F323 107.9(15) . . ? F321 C32 F323 106.1(14) . . ? F322 C32 C31 111.8(15) . . ? F321 C32 C31 109.1(13) . . ? F323 C32 C31 113.2(15) . . ? O34 C34 C33 122.3(15) . . ? O34 C34 C35 118.6(15) . . ? C33 C34 C35 118.9(14) . . ? C34 C35 C39 126.4(13) . . ? C34 C35 S36 116.6(12) . . ? C39 C35 S36 117.0(11) . . ? C38 C37 S36 105.7(19) . . ? C39 C38 C37 128(3) . . ? C38 C39 C35 98.3(17) . . ? N41 C42 N42 127.0(12) . 3_775 ? N41 C42 C52 117.7(12) . . ? N42 C42 C52 115.2(12) 3_775 . ? N51 C52 C53 123.9(12) . . ? N51 C52 C42 115.1(12) . . ? C53 C52 C42 121.1(13) . . ? C52 C53 C54 118.2(14) . . ? C55 C54 C53 117.2(15) . . ? C56 C55 C54 119.5(14) . . ? N51 C56 C55 125.6(14) . . ? Cl12 C100 Cl11 122(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.105 _refine_diff_density_min -1.149 _refine_diff_density_rms 0.186 #=END data_cars _database_code_CSD 200936 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H18 Cl2 F9 Gd N3 O6 S3' _chemical_formula_weight 1023.81 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' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2615(12) _cell_length_b 19.677(3) _cell_length_c 19.167(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.384(13) _cell_angle_gamma 90.00 _cell_volume 3731.3(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 colourless _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 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 2.180 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.79 _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 (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24538 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0894 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8581 _reflns_number_gt 5262 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0457P)^2^+3.1345P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8581 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Gd1 Gd 0.12186(3) 0.815080(14) 0.070810(15) 0.03439(10) Uani 1 1 d . . . S16 S -0.3743(2) 0.78350(11) -0.01713(11) 0.0556(8) Uani 0.811(7) 1 d P A 1 S16' S -0.4032(4) 0.8164(2) -0.1592(3) 0.0661(18) Uani 0.189(7) 1 d P A 2 S26 S 0.53305(16) 0.81080(9) 0.28848(9) 0.0507(4) Uani 1 1 d . . . S36' S -0.1041(2) 0.62319(12) 0.16828(13) 0.0540(9) Uani 0.630(7) 1 d P B 1 S36 S 0.1075(4) 0.5326(2) 0.1956(2) 0.0753(15) Uani 0.370(7) 1 d P B 2 F121 F 0.1624(5) 0.8575(3) -0.1920(3) 0.0962(17) Uani 1 1 d . . . F122 F 0.1656(5) 0.9463(2) -0.1304(2) 0.0936(16) Uani 1 1 d . . . F123 F -0.0094(4) 0.9216(2) -0.21398(19) 0.0642(11) Uani 1 1 d . . . F221 F -0.0968(4) 0.8604(3) 0.3096(3) 0.109(2) Uani 1 1 d . . . F222 F -0.2118(4) 0.8279(2) 0.2056(3) 0.0961(16) Uani 1 1 d . . . F223 F -0.1529(4) 0.9313(2) 0.2235(2) 0.0693(11) Uani 1 1 d . . . F321 F 0.4848(4) 0.6538(2) 0.0334(2) 0.0691(12) Uani 1 1 d . . . F322 F 0.5631(4) 0.7175(2) 0.1252(2) 0.0700(12) Uani 1 1 d . . . F323 F 0.5246(4) 0.6123(2) 0.1403(2) 0.0765(13) Uani 1 1 d . . . O11 O 0.1307(4) 0.84076(19) -0.0488(2) 0.0386(9) Uani 1 1 d . . . O14 O -0.0910(4) 0.79521(18) -0.0052(2) 0.0373(9) Uani 1 1 d . . . O21 O -0.0025(4) 0.8532(2) 0.1478(2) 0.0435(10) Uani 1 1 d . . . O24 O 0.2688(4) 0.8192(2) 0.18917(19) 0.0406(9) Uani 1 1 d . . . O31 O 0.2954(4) 0.74123(19) 0.06523(19) 0.0380(9) Uani 1 1 d . . . O34 O 0.0648(4) 0.7099(2) 0.1096(2) 0.0413(10) Uani 1 1 d . . . N41 N 0.0382(4) 0.9395(2) 0.0317(2) 0.0337(11) Uani 1 1 d . . . N42 N -0.0922(4) 0.9515(2) 0.0050(2) 0.0366(11) Uani 1 1 d . . . N51 N 0.3034(4) 0.9083(2) 0.0770(2) 0.0347(11) Uani 1 1 d . . . C11 C 0.0375(6) 0.8560(3) -0.1051(3) 0.0350(13) Uani 1 1 d . . . C12 C 0.0878(6) 0.8949(4) -0.1611(3) 0.0480(16) Uani 1 1 d . . . C13 C -0.0993(6) 0.8433(3) -0.1189(3) 0.0371(13) Uani 1 1 d . . . H13A H -0.1565 0.8556 -0.1648 0.044 Uiso 1 1 calc R . . C14 C -0.1580(6) 0.8128(3) -0.0677(3) 0.0381(13) Uani 1 1 d . A . C15 C -0.3044(6) 0.8040(3) -0.0852(3) 0.0368(14) Uani 1 1 d . . . C17 C -0.5288(7) 0.7886(4) -0.0729(4) 0.0593(19) Uani 1 1 d . . . H17 H -0.6076 0.7805 -0.0570 0.071 Uiso 1 1 calc R A 1 C18 C -0.5349(6) 0.8045(3) -0.1409(4) 0.0545(18) Uani 1 1 d . A . H18 H -0.6190 0.8082 -0.1765 0.065 Uiso 1 1 calc R C 1 C19 C -0.4032(4) 0.8164(2) -0.1592(3) 0.0661(18) Uani 0.811(7) 1 d P A 1 C19' C -0.3743(2) 0.78350(11) -0.01713(11) 0.0556(8) Uani 0.189(7) 1 d P A 2 C21 C 0.0178(6) 0.8531(3) 0.2157(4) 0.0448(15) Uani 1 1 d . . . C22 C -0.1107(7) 0.8681(4) 0.2393(4) 0.0579(19) Uani 1 1 d . . . C23 C 0.1356(6) 0.8435(3) 0.2686(3) 0.0481(16) Uani 1 1 d . . . H23A H 0.1342 0.8459 0.3179 0.058 Uiso 1 1 calc R . . C24 C 0.2597(6) 0.8300(3) 0.2518(3) 0.0359(14) Uani 1 1 d . . . C25 C 0.3867(6) 0.8302(3) 0.3099(3) 0.0373(14) Uani 1 1 d . . . C27 C 0.6232(7) 0.8213(3) 0.3751(3) 0.0517(17) Uani 1 1 d . . . H27 H 0.7184 0.8153 0.3911 0.062 Uiso 1 1 calc R . . C28 C 0.5467(7) 0.8389(3) 0.4192(4) 0.0546(18) Uani 1 1 d . . . H28A H 0.5830 0.8465 0.4696 0.066 Uiso 1 1 calc R . . C29 C 0.4070(6) 0.8454(3) 0.3840(3) 0.0370(13) Uani 1 1 d . . . H29 H 0.3385 0.8579 0.4066 0.044 Uiso 1 1 calc R . . C31 C 0.3336(6) 0.6862(3) 0.1001(3) 0.0389(13) Uani 1 1 d . . . C32 C 0.4781(7) 0.6667(4) 0.1007(4) 0.0537(18) Uani 1 1 d . . . C33 C 0.2632(6) 0.6441(3) 0.1336(3) 0.0423(15) Uani 1 1 d . . . H33A H 0.3068 0.6046 0.1573 0.051 Uiso 1 1 calc R . . C34 C 0.1273(6) 0.6570(3) 0.1346(3) 0.0382(14) Uani 1 1 d . B . C35 C 0.0531(6) 0.6056(3) 0.1650(3) 0.0434(15) Uani 1 1 d . . . C37 C -0.0181(11) 0.5086(4) 0.2161(5) 0.089(3) Uani 1 1 d . . . H37 H -0.0217 0.4647 0.2363 0.106 Uiso 1 1 calc R B 1 C38 C -0.1231(9) 0.5510(4) 0.2049(4) 0.073(2) Uani 1 1 d . B . H38 H -0.2038 0.5395 0.2176 0.087 Uiso 1 1 calc R D 1 C39' C 0.1075(4) 0.5326(2) 0.1956(2) 0.0753(15) Uani 0.630(7) 1 d P B 1 C39 C -0.1041(2) 0.62319(12) 0.16828(13) 0.0540(9) Uani 0.370(7) 1 d P B 2 C42 C 0.1261(5) 0.9874(3) 0.0259(3) 0.0329(13) Uani 1 1 d . . . C52 C 0.2718(5) 0.9730(3) 0.0551(3) 0.0343(13) Uani 1 1 d . . . C53 C 0.3674(6) 1.0227(3) 0.0592(3) 0.0456(16) Uani 1 1 d . . . H53A H 0.3412 1.0678 0.0438 0.055 Uiso 1 1 calc R . . C54 C 0.5030(6) 1.0063(4) 0.0862(4) 0.0571(18) Uani 1 1 d . . . H54A H 0.5713 1.0398 0.0905 0.069 Uiso 1 1 calc R . . C55 C 0.5357(6) 0.9403(3) 0.1067(3) 0.0472(16) Uani 1 1 d . . . H55A H 0.6277 0.9272 0.1246 0.057 Uiso 1 1 calc R . . C56 C 0.4340(6) 0.8931(3) 0.1009(3) 0.0436(15) Uani 1 1 d . . . H56A H 0.4584 0.8474 0.1147 0.052 Uiso 1 1 calc R . . C100 C 0.6918(15) 0.5211(12) 0.0113(8) 0.292(14) Uani 1 1 d . . . H10A H 0.6909 0.5583 0.0460 0.350 Uiso 1 1 calc R . . H10B H 0.6576 0.4791 0.0287 0.350 Uiso 1 1 calc R . . Cl1 Cl 0.5934(4) 0.5426(2) -0.0762(2) 0.1733(15) Uani 1 1 d . . . Cl2 Cl 0.8536(6) 0.5088(2) 0.0013(2) 0.206(2) 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 0.02902(15) 0.03501(16) 0.03592(16) 0.00537(14) 0.00295(11) 0.00441(14) S16 0.0429(12) 0.0664(15) 0.0587(14) 0.0048(10) 0.0156(10) -0.0162(10) S16' 0.032(2) 0.059(3) 0.101(4) -0.007(3) 0.007(2) -0.002(2) S26 0.0390(9) 0.0652(11) 0.0458(9) 0.0059(8) 0.0076(7) 0.0105(9) S36' 0.0564(17) 0.0562(17) 0.0536(16) 0.0026(11) 0.0218(13) -0.0103(12) S36 0.096(3) 0.067(3) 0.075(3) 0.015(2) 0.045(2) 0.004(2) F121 0.091(3) 0.127(4) 0.095(4) 0.045(3) 0.067(3) 0.046(3) F122 0.103(4) 0.101(4) 0.064(3) 0.020(3) 0.001(3) -0.066(3) F123 0.043(2) 0.098(3) 0.047(2) 0.029(2) 0.0049(19) -0.004(2) F221 0.062(3) 0.205(6) 0.076(3) 0.057(4) 0.044(3) 0.053(3) F222 0.047(3) 0.101(4) 0.152(5) 0.005(3) 0.047(3) -0.008(3) F223 0.053(2) 0.074(3) 0.088(3) 0.006(2) 0.032(2) 0.022(2) F321 0.076(3) 0.076(3) 0.068(3) 0.007(2) 0.040(2) 0.026(2) F322 0.039(2) 0.078(3) 0.089(3) -0.001(2) 0.010(2) 0.005(2) F323 0.067(3) 0.078(3) 0.092(3) 0.044(2) 0.036(2) 0.043(2) O11 0.030(2) 0.047(2) 0.036(2) 0.0031(18) 0.0025(19) 0.0027(18) O14 0.033(2) 0.038(2) 0.037(2) 0.0071(17) 0.0041(19) -0.0022(17) O21 0.032(2) 0.052(3) 0.043(3) 0.007(2) 0.004(2) 0.0089(19) O24 0.037(2) 0.051(3) 0.032(2) 0.0019(19) 0.0049(18) 0.008(2) O31 0.040(2) 0.037(2) 0.037(2) 0.0059(18) 0.0092(19) 0.0063(19) O34 0.038(2) 0.038(2) 0.045(2) 0.0125(19) 0.005(2) 0.0088(19) N41 0.026(2) 0.036(3) 0.040(3) 0.003(2) 0.009(2) 0.003(2) N42 0.028(3) 0.039(3) 0.041(3) -0.001(2) 0.006(2) 0.005(2) N51 0.026(2) 0.037(3) 0.039(3) 0.004(2) 0.005(2) 0.007(2) C11 0.036(3) 0.033(3) 0.036(3) -0.004(3) 0.008(3) 0.001(3) C12 0.035(4) 0.065(5) 0.042(4) 0.012(3) 0.007(3) -0.003(3) C13 0.031(3) 0.043(3) 0.031(3) 0.000(3) -0.003(3) 0.002(3) C14 0.033(3) 0.035(3) 0.043(3) -0.003(3) 0.005(3) -0.001(3) C15 0.033(3) 0.033(3) 0.043(3) -0.001(3) 0.007(3) -0.004(3) C17 0.038(4) 0.063(5) 0.076(5) -0.007(4) 0.013(4) -0.016(3) C18 0.032(3) 0.068(5) 0.060(4) -0.001(4) 0.005(3) -0.002(3) C19 0.032(2) 0.059(3) 0.101(4) -0.007(3) 0.007(2) -0.002(2) C19' 0.0429(12) 0.0664(15) 0.0587(14) 0.0048(10) 0.0156(10) -0.0162(10) C21 0.037(4) 0.044(4) 0.055(4) 0.011(3) 0.014(3) 0.007(3) C22 0.041(4) 0.080(6) 0.056(5) 0.023(4) 0.021(4) 0.017(4) C23 0.041(4) 0.062(4) 0.044(4) 0.019(3) 0.015(3) 0.015(3) C24 0.037(3) 0.034(3) 0.036(3) 0.007(2) 0.009(3) 0.003(3) C25 0.032(3) 0.037(4) 0.041(3) 0.004(3) 0.006(3) 0.006(2) C27 0.039(4) 0.056(4) 0.051(4) 0.005(3) -0.004(3) -0.003(3) C28 0.062(5) 0.063(5) 0.035(4) 0.006(3) 0.006(4) 0.001(4) C29 0.034(3) 0.043(3) 0.032(3) 0.005(3) 0.006(3) 0.001(3) C31 0.046(3) 0.035(3) 0.033(3) -0.003(3) 0.005(3) 0.005(3) C32 0.055(4) 0.059(5) 0.049(4) 0.013(3) 0.017(4) 0.022(4) C33 0.044(4) 0.046(4) 0.034(3) 0.016(3) 0.007(3) 0.013(3) C34 0.046(4) 0.041(3) 0.024(3) -0.001(3) 0.003(3) 0.000(3) C35 0.056(4) 0.040(4) 0.037(3) 0.002(3) 0.017(3) 0.003(3) C37 0.140(9) 0.053(5) 0.095(7) 0.016(5) 0.071(7) 0.004(6) C38 0.092(6) 0.063(5) 0.082(6) -0.003(4) 0.056(5) -0.017(5) C39' 0.096(3) 0.067(3) 0.075(3) 0.015(2) 0.045(2) 0.004(2) C39 0.0564(17) 0.0562(17) 0.0536(16) 0.0026(11) 0.0218(13) -0.0103(12) C42 0.031(3) 0.032(3) 0.032(3) -0.002(2) 0.002(3) 0.006(3) C52 0.027(3) 0.038(3) 0.035(3) -0.001(3) 0.003(3) 0.001(3) C53 0.032(3) 0.039(4) 0.063(4) -0.004(3) 0.008(3) 0.004(3) C54 0.034(4) 0.056(5) 0.076(5) -0.005(4) 0.007(4) -0.004(3) C55 0.024(3) 0.055(4) 0.057(4) -0.004(3) 0.002(3) 0.005(3) C56 0.035(3) 0.048(4) 0.046(4) 0.002(3) 0.006(3) 0.012(3) C100 0.125(12) 0.63(4) 0.134(13) -0.175(19) 0.050(10) -0.031(18) Cl1 0.214(4) 0.172(4) 0.147(3) -0.019(3) 0.070(3) -0.031(3) Cl2 0.312(6) 0.149(3) 0.152(3) -0.013(3) 0.052(4) 0.045(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 Gd1 O14 2.314(4) . ? Gd1 O21 2.317(4) . ? Gd1 O31 2.322(4) . ? Gd1 O34 2.325(4) . ? Gd1 O24 2.369(4) . ? Gd1 O11 2.372(4) . ? Gd1 N51 2.595(5) . ? Gd1 N41 2.636(4) . ? S16 C17 1.663(7) . ? S16 C15 1.696(6) . ? S16' C18 1.502(8) . ? S16' C15 1.529(7) . ? S26 C27 1.686(6) . ? S26 C25 1.702(6) . ? S36' C38 1.620(8) . ? S36' C35 1.667(7) . ? S36 C37 1.519(10) . ? S36 C35 1.594(7) . ? F121 C12 1.312(7) . ? F122 C12 1.325(7) . ? F123 C12 1.327(7) . ? F221 C22 1.326(8) . ? F222 C22 1.328(8) . ? F223 C22 1.324(8) . ? F321 C32 1.335(7) . ? F322 C32 1.327(8) . ? F323 C32 1.327(7) . ? O11 C11 1.273(6) . ? O14 C14 1.261(6) . ? O21 C21 1.262(7) . ? O24 C24 1.248(6) . ? O31 C31 1.279(7) . ? O34 C34 1.250(7) . ? N41 N42 1.321(6) . ? N41 C42 1.331(7) . ? N42 C42 1.345(7) 3_575 ? N51 C56 1.330(7) . ? N51 C52 1.352(7) . ? C11 C13 1.381(8) . ? C11 C12 1.516(8) . ? C13 C14 1.415(8) . ? C14 C15 1.459(8) . ? C17 C18 1.326(9) . ? C21 C23 1.370(8) . ? C21 C22 1.531(9) . ? C23 C24 1.418(8) . ? C24 C25 1.472(8) . ? C25 C29 1.413(8) . ? C27 C28 1.343(9) . ? C28 C29 1.419(8) . ? C31 C33 1.366(8) . ? C31 C32 1.528(9) . ? C33 C34 1.421(8) . ? C34 C35 1.476(8) . ? C37 C38 1.334(11) . ? C42 N42 1.345(7) 3_575 ? C42 C52 1.478(7) . ? C52 C53 1.374(8) . ? C53 C54 1.388(8) . ? C54 C55 1.372(9) . ? C55 C56 1.380(8) . ? C100 Cl2 1.738(13) . ? C100 Cl1 1.765(16) . ? 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 O14 Gd1 O21 82.43(14) . . ? O14 Gd1 O31 118.18(13) . . ? O21 Gd1 O31 142.21(13) . . ? O14 Gd1 O34 77.03(13) . . ? O21 Gd1 O34 81.72(14) . . ? O31 Gd1 O34 73.68(13) . . ? O14 Gd1 O24 149.68(14) . . ? O21 Gd1 O24 72.38(13) . . ? O31 Gd1 O24 76.37(13) . . ? O34 Gd1 O24 82.78(14) . . ? O14 Gd1 O11 72.51(13) . . ? O21 Gd1 O11 135.67(13) . . ? O31 Gd1 O11 82.10(13) . . ? O34 Gd1 O11 125.17(14) . . ? O24 Gd1 O11 137.74(13) . . ? O14 Gd1 N51 133.98(13) . . ? O21 Gd1 N51 104.63(14) . . ? O31 Gd1 N51 83.95(14) . . ? O34 Gd1 N51 148.53(14) . . ? O24 Gd1 N51 70.44(14) . . ? O11 Gd1 N51 71.49(13) . . ? O14 Gd1 N41 78.23(13) . . ? O21 Gd1 N41 71.80(14) . . ? O31 Gd1 N41 139.81(13) . . ? O34 Gd1 N41 145.73(14) . . ? O24 Gd1 N41 108.49(13) . . ? O11 Gd1 N41 67.71(13) . . ? N51 Gd1 N41 62.13(13) . . ? C17 S16 C15 91.0(3) . . ? C18 S16' C15 100.1(5) . . ? C27 S26 C25 91.4(3) . . ? C38 S36' C35 93.6(4) . . ? C37 S36 C35 97.9(5) . . ? C11 O11 Gd1 131.1(3) . . ? C14 O14 Gd1 137.5(4) . . ? C21 O21 Gd1 133.5(4) . . ? C24 O24 Gd1 137.4(4) . . ? C31 O31 Gd1 129.7(4) . . ? C34 O34 Gd1 135.8(4) . . ? N42 N41 C42 118.7(4) . . ? N42 N41 Gd1 119.8(3) . . ? C42 N41 Gd1 120.3(3) . . ? N41 N42 C42 116.6(5) . 3_575 ? C56 N51 C52 117.1(5) . . ? C56 N51 Gd1 120.1(4) . . ? C52 N51 Gd1 122.7(3) . . ? O11 C11 C13 128.0(5) . . ? O11 C11 C12 113.5(5) . . ? C13 C11 C12 118.4(5) . . ? F121 C12 F122 105.9(6) . . ? F121 C12 F123 106.7(5) . . ? F122 C12 F123 106.2(6) . . ? F121 C12 C11 112.6(5) . . ? F122 C12 C11 110.4(5) . . ? F123 C12 C11 114.4(5) . . ? C11 C13 C14 122.9(5) . . ? O14 C14 C13 123.4(5) . . ? O14 C14 C15 117.1(5) . . ? C13 C14 C15 119.5(5) . . ? C14 C15 S16' 125.7(5) . . ? C14 C15 S16 118.1(4) . . ? S16' C15 S16 116.1(4) . . ? C18 C17 S16 115.8(6) . . ? C17 C18 S16' 117.1(6) . . ? O21 C21 C23 129.5(6) . . ? O21 C21 C22 112.6(5) . . ? C23 C21 C22 117.9(6) . . ? F223 C22 F221 106.2(6) . . ? F223 C22 F222 106.4(6) . . ? F221 C22 F222 106.5(6) . . ? F223 C22 C21 111.7(6) . . ? F221 C22 C21 114.1(6) . . ? F222 C22 C21 111.4(6) . . ? C21 C23 C24 121.8(6) . . ? O24 C24 C23 123.5(5) . . ? O24 C24 C25 116.7(5) . . ? C23 C24 C25 119.8(5) . . ? C29 C25 C24 128.7(5) . . ? C29 C25 S26 112.7(4) . . ? C24 C25 S26 118.6(4) . . ? C28 C27 S26 113.1(5) . . ? C27 C28 C29 114.2(6) . . ? C25 C29 C28 108.7(5) . . ? O31 C31 C33 129.1(6) . . ? O31 C31 C32 112.3(5) . . ? C33 C31 C32 118.6(5) . . ? F323 C32 F322 107.6(6) . . ? F323 C32 F321 107.2(5) . . ? F322 C32 F321 106.7(6) . . ? F323 C32 C31 114.1(6) . . ? F322 C32 C31 111.1(5) . . ? F321 C32 C31 109.8(5) . . ? C31 C33 C34 122.8(5) . . ? O34 C34 C33 123.3(6) . . ? O34 C34 C35 117.1(5) . . ? C33 C34 C35 119.6(5) . . ? C34 C35 S36 126.5(5) . . ? C34 C35 S36' 118.6(5) . . ? S36 C35 S36' 114.9(4) . . ? C38 C37 S36 117.9(7) . . ? C37 C38 S36' 115.7(6) . . ? N41 C42 N42 124.7(5) . 3_575 ? N41 C42 C52 118.2(5) . . ? N42 C42 C52 117.1(5) 3_575 . ? N51 C52 C53 123.0(5) . . ? N51 C52 C42 115.7(5) . . ? C53 C52 C42 121.3(5) . . ? C52 C53 C54 119.0(6) . . ? C55 C54 C53 118.2(6) . . ? C54 C55 C56 119.4(6) . . ? N51 C56 C55 123.2(6) . . ? Cl2 C100 Cl1 104.5(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.153 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.117 #=END