# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_JT2-9a #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C23 H16 Au1 Eu1 N10 O6' _chemical_formula_moiety 'C23 H16 Au1 Eu1 N10 O6' _chemical_formula_weight 877.37 #============================================================= # 6. CRYSTAL DATA _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 10.8762(2) _cell_length_b 10.9064(2) _cell_length_c 12.2510(2) _cell_angle_alpha 75.9520(10) _cell_angle_beta 76.2750(10) _cell_angle_gamma 78.3780(10) _cell_volume 1353.45(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9989 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.42 _cell_measurement_temperature 296(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.087 _exptl_crystal_size_mid 0.088 _exptl_crystal_size_max 0.157 _exptl_crystal_density_diffrn 2.153 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 7.768 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(Sheldrich , 1996)' _exptl_absorpt_correction_T_min 0.6169 _exptl_absorpt_correction_T_max 0.7457 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 39033 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_min 1.748 _diffrn_reflns_theta_max 28.459 _diffrn_reflns_theta_full 28.459 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 5431 _refine_ls_number_restraints 0 _refine_ls_number_parameters 386 _oxford_refine_ls_R_factor_ref 0.0267 _refine_ls_wR_factor_ref 0.0192 _refine_ls_goodness_of_fit_ref 1.1411 # The values computed from all data _oxford_reflns_number_all 6828 _refine_ls_R_factor_all 0.0383 _refine_ls_wR_factor_all 0.0247 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5533 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_gt 0.0194 _reflns_number_total 6828 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.470 0.539 0.510 0.265 0.165 ; _refine_ls_shift/su_max 0.0010160 _refine_diff_density_min -0.87 _refine_diff_density_max 1.79 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_refine_ls_scale 0.10413(7) _oxford_diffrn_Wilson_B_factor 2.07 _oxford_diffrn_Wilson_scale 102.85 # Number of reflections with Friedels Law is 6828 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 13670 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Eu -0.1578 3.6682 24.6274 2.3879 19.0886 0.1942 13.7603 13.7546 2.9227 123.1740 2.5745 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956 12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # TODO check _oxford_atom_site_special_shape 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Au1 Au 0.888680(17) 0.193881(14) 0.181256(14) 0.0354 1.0000 Uani . . . . . . Eu1 Eu 0.794388(17) 0.694161(15) 0.250729(14) 0.0218 1.0000 Uani . . . . . . O1 O 0.8776(4) 0.7384(3) 0.0392(3) 0.0533 1.0000 Uani . . . . . . O2 O 0.6783(3) 0.8027(4) 0.0973(3) 0.0549 1.0000 Uani . . . . . . O3 O 0.7598(5) 0.8410(5) -0.0837(3) 0.0861 1.0000 Uani . . . . . . O4 O 0.7301(3) 0.5176(3) 0.4141(2) 0.0357 1.0000 Uani . . . . . . O5 O 0.6118(3) 0.5744(3) 0.2870(3) 0.0408 1.0000 Uani . . . . . . O6 O 0.5791(4) 0.4105(3) 0.4249(4) 0.0722 1.0000 Uani . . . . . . N1 N 1.0206(3) 0.6336(3) 0.2772(3) 0.0275 1.0000 Uani . . . . . . N2 N 1.1729(3) 0.5937(3) 0.3806(3) 0.0323 1.0000 Uani . . . . . . N3 N 0.8352(3) 0.7259(3) 0.4405(2) 0.0267 1.0000 Uani . . . . . . N4 N 0.6050(3) 0.8045(3) 0.3744(3) 0.0309 1.0000 Uani . . . . . . N5 N 0.5025(3) 0.8445(3) 0.5457(3) 0.0341 1.0000 Uani . . . . . . N6 N 0.8700(4) 0.4810(3) 0.1890(3) 0.0391 1.0000 Uani . . . . . . N7 N 0.8637(4) 0.9083(3) 0.2051(3) 0.0439 1.0000 Uani . . . . . . N8 N 0.7721(4) 0.7944(4) 0.0139(3) 0.0481 1.0000 Uani . . . . . . N9 N 0.6370(3) 0.4978(3) 0.3773(3) 0.0365 1.0000 Uani . . . . . . N10 N 0.5534(5) 0.1488(6) 0.2126(4) 0.0741 1.0000 Uani . . . . . . C1 C 1.1348(4) 0.5815(4) 0.2140(3) 0.0313 1.0000 Uani . . . . . . C2 C 1.1615(4) 0.5526(4) 0.1051(4) 0.0387 1.0000 Uani . . . . . . C3 C 1.2836(5) 0.4979(5) 0.0660(4) 0.0484 1.0000 Uani . . . . . . C4 C 1.3795(5) 0.4724(5) 0.1308(5) 0.0523 1.0000 Uani . . . . . . C5 C 1.3549(4) 0.5007(5) 0.2382(4) 0.0446 1.0000 Uani . . . . . . C6 C 1.2318(4) 0.5562(4) 0.2784(3) 0.0344 1.0000 Uani . . . . . . C7 C 1.0494(4) 0.6388(3) 0.3762(3) 0.0289 1.0000 Uani . . . . . . C8 C 0.9516(4) 0.6881(3) 0.4666(3) 0.0297 1.0000 Uani . . . . . . C9 C 0.9756(4) 0.6933(4) 0.5725(3) 0.0360 1.0000 Uani . . . . . . C10 C 0.8745(5) 0.7391(4) 0.6513(3) 0.0421 1.0000 Uani . . . . . . C11 C 0.7545(4) 0.7788(4) 0.6249(3) 0.0379 1.0000 Uani . . . . . . C12 C 0.7387(4) 0.7701(3) 0.5178(3) 0.0306 1.0000 Uani . . . . . . C13 C 0.6157(4) 0.8072(3) 0.4800(3) 0.0300 1.0000 Uani . . . . . . C14 C 0.4103(4) 0.8658(3) 0.4809(3) 0.0319 1.0000 Uani . . . . . . C15 C 0.2772(4) 0.9014(4) 0.5053(4) 0.0415 1.0000 Uani . . . . . . C16 C 0.2140(4) 0.9112(4) 0.4186(4) 0.0465 1.0000 Uani . . . . . . C17 C 0.2780(5) 0.8876(5) 0.3116(4) 0.0488 1.0000 Uani . . . . . . C18 C 0.4087(4) 0.8527(5) 0.2869(4) 0.0450 1.0000 Uani . . . . . . C19 C 0.4763(4) 0.8416(4) 0.3733(3) 0.0323 1.0000 Uani . . . . . . C20 C 0.8815(4) 0.3757(4) 0.1820(3) 0.0328 1.0000 Uani . . . . . . C21 C 0.8808(4) 1.0115(4) 0.1919(4) 0.0390 1.0000 Uani . . . . . . C22 C 0.6337(12) 0.1498(8) -0.0016(5) 0.1030 1.0000 Uani . . . . . . C23 C 0.5871(5) 0.1490(5) 0.1198(4) 0.0551 1.0000 Uani . . . . . . H21 H 1.0978 0.5701 0.0620 0.052(14) 1.0000 Uiso R . . . . . H31 H 1.3046 0.4770 -0.0062 0.025(10) 1.0000 Uiso R . . . . . H41 H 1.4621 0.4349 0.1020 0.070(18) 1.0000 Uiso R . . . . . H51 H 1.4182 0.4843 0.2819 0.068(17) 1.0000 Uiso R . . . . . H91 H 1.0570 0.6660 0.5883 0.026(10) 1.0000 Uiso R . . . . . H101 H 0.8877 0.7431 0.7224 0.072(18) 1.0000 Uiso R . . . . . H111 H 0.6855 0.8101 0.6773 0.038(12) 1.0000 Uiso R . . . . . H151 H 0.2351 0.9175 0.5768 0.047(13) 1.0000 Uiso R . . . . . H161 H 0.1250 0.9340 0.4319 0.066(17) 1.0000 Uiso R . . . . . H171 H 0.2303 0.8971 0.2551 0.066(16) 1.0000 Uiso R . . . . . H181 H 0.4514 0.8363 0.2149 0.054(14) 1.0000 Uiso R . . . . . H222 H 0.6022 0.0827 -0.0203 0.26(8) 1.0000 Uiso R . . . . . H221 H 0.7258 0.1350 -0.0179 0.29(10) 1.0000 Uiso R . . . . . H223 H 0.6026 0.2307 -0.0449 0.12(3) 1.0000 Uiso R . . . . . H52 H 0.4888 0.8544 0.6228 0.040(12) 1.0000 Uiso R . . . . . H22 H 1.2128 0.5889 0.4429 0.031(11) 1.0000 Uiso 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 Au1 0.05125(12) 0.02110(7) 0.03682(9) -0.00667(6) -0.00805(7) -0.01227(7) Eu1 0.02992(10) 0.01704(8) 0.02123(9) -0.00164(6) -0.00964(7) -0.00710(7) O1 0.059(2) 0.0545(19) 0.0338(16) -0.0042(14) -0.0009(15) 0.0055(17) O2 0.0422(18) 0.078(2) 0.0365(17) 0.0051(16) -0.0146(15) -0.0030(17) O3 0.119(4) 0.099(3) 0.0250(17) 0.0072(19) -0.021(2) 0.001(3) O4 0.0431(16) 0.0352(14) 0.0325(14) 0.0021(11) -0.0167(12) -0.0144(12) O5 0.0432(17) 0.0358(15) 0.0504(17) 0.0018(13) -0.0255(14) -0.0158(13) O6 0.075(3) 0.048(2) 0.093(3) 0.0216(19) -0.026(2) -0.0410(19) N1 0.0331(17) 0.0250(14) 0.0275(15) -0.0049(12) -0.0129(13) -0.0042(12) N2 0.0373(18) 0.0347(16) 0.0307(16) -0.0006(13) -0.0174(14) -0.0133(14) N3 0.0374(17) 0.0221(13) 0.0249(14) -0.0042(11) -0.0106(13) -0.0096(12) N4 0.0357(18) 0.0341(16) 0.0246(15) -0.0050(12) -0.0075(13) -0.0088(14) N5 0.043(2) 0.0328(16) 0.0267(16) -0.0074(13) -0.0053(14) -0.0064(14) N6 0.054(2) 0.0263(15) 0.0417(19) -0.0115(14) -0.0109(17) -0.0092(15) N7 0.061(3) 0.0238(16) 0.049(2) -0.0041(15) -0.0114(18) -0.0138(16) N8 0.073(3) 0.044(2) 0.0256(18) -0.0009(15) -0.0122(18) -0.009(2) N9 0.0411(19) 0.0262(15) 0.0431(19) 0.0010(13) -0.0107(15) -0.0143(14) N10 0.072(3) 0.101(4) 0.048(3) -0.027(3) -0.013(2) 0.003(3) C1 0.031(2) 0.0295(18) 0.035(2) -0.0031(15) -0.0107(16) -0.0069(15) C2 0.035(2) 0.048(2) 0.037(2) -0.0121(18) -0.0123(18) -0.0052(18) C3 0.043(3) 0.062(3) 0.041(2) -0.018(2) -0.004(2) -0.007(2) C4 0.038(3) 0.058(3) 0.056(3) -0.007(2) -0.009(2) -0.005(2) C5 0.031(2) 0.051(3) 0.050(3) 0.001(2) -0.0135(19) -0.0105(19) C6 0.036(2) 0.0324(19) 0.039(2) -0.0016(16) -0.0149(17) -0.0125(16) C7 0.035(2) 0.0251(16) 0.0319(18) -0.0009(14) -0.0153(16) -0.0118(15) C8 0.043(2) 0.0211(15) 0.0294(18) -0.0019(13) -0.0148(16) -0.0107(15) C9 0.052(3) 0.0344(19) 0.0281(19) -0.0032(15) -0.0200(18) -0.0103(18) C10 0.063(3) 0.042(2) 0.030(2) -0.0078(17) -0.020(2) -0.015(2) C11 0.054(3) 0.039(2) 0.0263(18) -0.0105(16) -0.0099(18) -0.0116(19) C12 0.044(2) 0.0245(16) 0.0288(18) -0.0058(14) -0.0110(16) -0.0120(16) C13 0.038(2) 0.0258(16) 0.0268(17) -0.0027(14) -0.0056(15) -0.0104(15) C14 0.042(2) 0.0230(16) 0.0273(18) 0.0014(14) -0.0033(16) -0.0094(15) C15 0.043(2) 0.036(2) 0.037(2) -0.0061(17) 0.0065(18) -0.0058(18) C16 0.031(2) 0.043(2) 0.059(3) -0.005(2) -0.004(2) -0.0036(18) C17 0.043(3) 0.055(3) 0.051(3) -0.008(2) -0.018(2) -0.007(2) C18 0.041(3) 0.060(3) 0.035(2) -0.011(2) -0.0101(19) -0.005(2) C19 0.036(2) 0.0294(18) 0.0318(19) -0.0034(15) -0.0069(16) -0.0078(16) C20 0.045(2) 0.0285(18) 0.0291(19) -0.0079(15) -0.0101(17) -0.0093(16) C21 0.049(3) 0.0258(18) 0.042(2) -0.0042(16) -0.0063(19) -0.0111(17) C22 0.176(10) 0.092(5) 0.037(3) -0.017(3) -0.019(4) -0.009(6) C23 0.063(3) 0.060(3) 0.043(3) -0.018(2) -0.016(2) 0.004(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Au1 . C21 1_545 1.980(4) yes Au1 . C20 . 1.971(4) yes Eu1 . O1 . 2.495(3) yes Eu1 . O2 . 2.444(3) yes Eu1 . O4 . 2.492(3) yes Eu1 . O5 . 2.489(3) yes Eu1 . N1 . 2.493(3) yes Eu1 . N3 . 2.582(3) yes Eu1 . N4 . 2.528(3) yes Eu1 . N6 . 2.538(3) yes Eu1 . N7 . 2.492(3) yes Eu1 . N8 . 2.891(4) yes Eu1 . N9 . 2.920(3) yes O1 . N8 . 1.257(5) yes O2 . N8 . 1.268(5) yes O3 . N8 . 1.208(5) yes O4 . N9 . 1.276(4) yes O5 . N9 . 1.265(4) yes O6 . N9 . 1.200(4) yes N1 . C1 . 1.392(5) yes N1 . C7 . 1.338(4) yes N2 . C6 . 1.381(5) yes N2 . C7 . 1.344(5) yes N2 . H22 . 0.950 no N3 . C8 . 1.340(5) yes N3 . C12 . 1.333(5) yes N4 . C13 . 1.335(5) yes N4 . C19 . 1.379(5) yes N5 . C13 . 1.348(5) yes N5 . C14 . 1.373(5) yes N5 . H52 . 0.950 no N6 . C20 . 1.152(5) yes N7 . C21 . 1.144(5) yes N10 . C23 . 1.109(7) yes C1 . C2 . 1.395(6) yes C1 . C6 . 1.409(5) yes C2 . C3 . 1.366(6) yes C2 . H21 . 0.932 no C3 . C4 . 1.401(7) yes C3 . H31 . 0.931 no C4 . C5 . 1.378(7) yes C4 . H41 . 0.933 no C5 . C6 . 1.380(6) yes C5 . H51 . 0.933 no C7 . C8 . 1.466(6) yes C8 . C9 . 1.398(5) yes C9 . C10 . 1.379(6) yes C9 . H91 . 0.926 no C10 . C11 . 1.378(6) yes C10 . H101 . 0.927 no C11 . C12 . 1.392(5) yes C11 . H111 . 0.930 no C12 . C13 . 1.466(6) yes C14 . C15 . 1.400(6) yes C14 . C19 . 1.403(5) yes C15 . C16 . 1.370(7) yes C15 . H151 . 0.927 no C16 . C17 . 1.389(7) yes C16 . H161 . 0.934 no C17 . C18 . 1.375(7) yes C17 . H171 . 0.934 no C18 . C19 . 1.394(6) yes C18 . H181 . 0.936 no C22 . C23 . 1.451(8) yes C22 . H222 . 0.962 no C22 . H221 . 0.962 no C22 . H223 . 0.956 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C21 1_545 Au1 . C20 . 174.55(18) yes O1 . Eu1 . O2 . 51.44(11) yes O1 . Eu1 . O4 . 141.47(10) yes O2 . Eu1 . O4 . 127.04(10) yes O1 . Eu1 . O5 . 107.04(11) yes O2 . Eu1 . O5 . 76.07(11) yes O4 . Eu1 . O5 . 51.18(9) yes O1 . Eu1 . N1 . 88.19(11) yes O2 . Eu1 . N1 . 138.23(11) yes O4 . Eu1 . N1 . 90.19(9) yes O5 . Eu1 . N1 . 134.29(9) yes O1 . Eu1 . N3 . 141.90(11) yes O2 . Eu1 . N3 . 140.78(11) yes O4 . Eu1 . N3 . 68.46(9) yes O5 . Eu1 . N3 . 111.04(9) yes N1 . Eu1 . N3 . 64.44(10) yes O1 . Eu1 . N4 . 131.48(10) yes O2 . Eu1 . N4 . 83.20(11) yes O4 . Eu1 . N4 . 76.85(10) yes O5 . Eu1 . N4 . 71.74(10) yes N1 . Eu1 . N4 . 128.49(9) yes O1 . Eu1 . N6 . 72.13(11) yes O2 . Eu1 . N6 . 98.14(12) yes O4 . Eu1 . N6 . 70.26(11) yes O5 . Eu1 . N6 . 69.48(11) yes N1 . Eu1 . N6 . 75.25(11) yes O1 . Eu1 . N7 . 74.71(12) yes O2 . Eu1 . N7 . 80.04(13) yes O4 . Eu1 . N7 . 142.35(11) yes O5 . Eu1 . N7 . 146.24(12) yes N1 . Eu1 . N7 . 78.92(11) yes O1 . Eu1 . N8 . 25.66(12) yes O2 . Eu1 . N8 . 25.78(12) yes O4 . Eu1 . N8 . 140.38(10) yes O5 . Eu1 . N8 . 91.83(11) yes N1 . Eu1 . N8 . 113.26(12) yes O1 . Eu1 . N9 . 125.63(11) yes O2 . Eu1 . N9 . 101.54(11) yes O4 . Eu1 . N9 . 25.75(9) yes O5 . Eu1 . N9 . 25.48(9) yes N1 . Eu1 . N9 . 112.40(10) yes N3 . Eu1 . N4 . 64.42(10) yes N3 . Eu1 . N6 . 120.75(10) yes N4 . Eu1 . N6 . 139.56(11) yes N3 . Eu1 . N7 . 74.37(11) yes N4 . Eu1 . N7 . 82.11(12) yes N6 . Eu1 . N7 . 138.16(12) yes N3 . Eu1 . N8 . 149.92(10) yes N4 . Eu1 . N8 . 107.58(11) yes N6 . Eu1 . N8 . 84.84(11) yes N7 . Eu1 . N8 . 75.81(12) yes N3 . Eu1 . N9 . 90.52(9) yes N4 . Eu1 . N9 . 73.76(10) yes N6 . Eu1 . N9 . 66.34(11) yes N7 . Eu1 . N9 . 155.37(12) yes N8 . Eu1 . N9 . 115.91(11) yes Eu1 . O1 . N8 . 95.1(2) yes Eu1 . O2 . N8 . 97.2(2) yes Eu1 . O4 . N9 . 96.2(2) yes Eu1 . O5 . N9 . 96.69(19) yes Eu1 . N1 . C1 . 135.0(2) yes Eu1 . N1 . C7 . 119.7(3) yes C1 . N1 . C7 . 105.0(3) yes C6 . N2 . C7 . 108.0(3) yes C6 . N2 . H22 . 126.1 no C7 . N2 . H22 . 126.0 no Eu1 . N3 . C8 . 120.2(2) yes Eu1 . N3 . C12 . 120.5(2) yes C8 . N3 . C12 . 119.1(3) yes Eu1 . N4 . C13 . 117.7(3) yes Eu1 . N4 . C19 . 135.6(2) yes C13 . N4 . C19 . 104.9(3) yes C13 . N5 . C14 . 107.5(3) yes C13 . N5 . H52 . 126.4 no C14 . N5 . H52 . 126.1 no Eu1 . N6 . C20 . 163.9(3) yes Eu1 . N7 . C21 . 171.5(4) yes Eu1 . N8 . O2 . 57.00(19) yes Eu1 . N8 . O1 . 59.3(2) yes O2 . N8 . O1 . 116.3(3) yes Eu1 . N8 . O3 . 177.2(4) yes O2 . N8 . O3 . 121.0(5) yes O1 . N8 . O3 . 122.7(5) yes Eu1 . N9 . O4 . 58.04(17) yes Eu1 . N9 . O5 . 57.82(16) yes O4 . N9 . O5 . 115.7(3) yes Eu1 . N9 . O6 . 174.9(3) yes O4 . N9 . O6 . 121.6(4) yes O5 . N9 . O6 . 122.7(4) yes N1 . C1 . C2 . 130.4(3) yes N1 . C1 . C6 . 109.3(3) yes C2 . C1 . C6 . 120.3(4) yes C1 . C2 . C3 . 117.2(4) yes C1 . C2 . H21 . 120.5 no C3 . C2 . H21 . 122.3 no C2 . C3 . C4 . 122.2(4) yes C2 . C3 . H31 . 119.4 no C4 . C3 . H31 . 118.4 no C3 . C4 . C5 . 121.4(5) yes C3 . C4 . H41 . 120.4 no C5 . C4 . H41 . 118.2 no C4 . C5 . C6 . 116.8(4) yes C4 . C5 . H51 . 122.0 no C6 . C5 . H51 . 121.2 no C1 . C6 . N2 . 105.2(4) yes C1 . C6 . C5 . 122.1(4) yes N2 . C6 . C5 . 132.7(4) yes N2 . C7 . N1 . 112.5(3) yes N2 . C7 . C8 . 126.4(3) yes N1 . C7 . C8 . 121.1(3) yes C7 . C8 . N3 . 114.2(3) yes C7 . C8 . C9 . 123.6(4) yes N3 . C8 . C9 . 122.2(4) yes C8 . C9 . C10 . 117.8(4) yes C8 . C9 . H91 . 120.3 no C10 . C9 . H91 . 121.9 no C9 . C10 . C11 . 120.3(4) yes C9 . C10 . H101 . 119.6 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 118.2(4) yes C10 . C11 . H111 . 121.3 no C12 . C11 . H111 . 120.5 no C11 . C12 . N3 . 122.3(4) yes C11 . C12 . C13 . 123.5(4) yes N3 . C12 . C13 . 114.1(3) yes C12 . C13 . N5 . 125.3(3) yes C12 . C13 . N4 . 122.1(3) yes N5 . C13 . N4 . 112.5(3) yes N5 . C14 . C15 . 132.6(4) yes N5 . C14 . C19 . 105.3(3) yes C15 . C14 . C19 . 122.0(4) yes C14 . C15 . C16 . 116.6(4) yes C14 . C15 . H151 . 121.1 no C16 . C15 . H151 . 122.4 no C15 . C16 . C17 . 122.0(4) yes C15 . C16 . H161 . 119.1 no C17 . C16 . H161 . 118.9 no C16 . C17 . C18 . 121.7(4) yes C16 . C17 . H171 . 118.5 no C18 . C17 . H171 . 119.8 no C17 . C18 . C19 . 117.9(4) yes C17 . C18 . H181 . 121.5 no C19 . C18 . H181 . 120.6 no C14 . C19 . C18 . 119.8(4) yes C14 . C19 . N4 . 109.7(3) yes C18 . C19 . N4 . 130.5(4) yes N6 . C20 . Au1 . 175.1(4) yes Au1 1_565 C21 . N7 . 172.7(4) yes C23 . C22 . H222 . 108.5 no C23 . C22 . H221 . 109.7 no H222 . C22 . H221 . 109.6 no C23 . C22 . H223 . 108.9 no H222 . C22 . H223 . 109.9 no H221 . C22 . H223 . 110.3 no C22 . C23 . N10 . 178.8(8) yes _database_code_depnum_ccdc_archive 'CCDC 952846' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_JT2-7d #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C23 H16 Au1 N10 O6 Tb1' _chemical_formula_moiety 'C23 H16 Au1 N10 O6 Tb1' _chemical_formula_weight 884.34 #============================================================= # 6. CRYSTAL DATA _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 10.8442(2) _cell_length_b 10.8853(2) _cell_length_c 12.2574(3) _cell_angle_alpha 75.7330(10) _cell_angle_beta 76.4370(10) _cell_angle_gamma 78.8200(10) _cell_volume 1348.86(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3576 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 24.35 _cell_measurement_temperature 296(2) _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_min 0.042 _exptl_crystal_size_mid 0.049 _exptl_crystal_size_max 0.101 _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 8.091 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(Sheldrich , 1996)' _exptl_absorpt_correction_T_min 0.6333 _exptl_absorpt_correction_T_max 0.7452 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 13780 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_min 1.951 _diffrn_reflns_theta_max 25.322 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.322 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 3741 _refine_ls_number_restraints 0 _refine_ls_number_parameters 372 _oxford_refine_ls_R_factor_ref 0.0279 _refine_ls_wR_factor_ref 0.0228 _refine_ls_goodness_of_fit_ref 1.1422 # The values computed from all data _oxford_reflns_number_all 4886 _refine_ls_R_factor_all 0.0413 _refine_ls_wR_factor_all 0.0278 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3879 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_gt 0.0233 _reflns_number_total 4886 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.387 0.251 0.341 0.151 0.141 ; _refine_ls_shift/su_max 0.0013294 _refine_diff_density_min -0.52 _refine_diff_density_max 0.63 _reflns_limit_h_min -12 _reflns_limit_h_max 13 _reflns_limit_k_min -12 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_refine_ls_scale 0.10891(10) _oxford_diffrn_Wilson_B_factor 2.51 _oxford_diffrn_Wilson_scale 89.77 # Number of reflections with Friedels Law is 4886 # Number of reflections without Friedels Law is 8612 # Theoretical number of reflections is about 4925 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Tb -0.1723 4.1537 25.8976 2.2426 18.2185 0.1961 14.3167 12.6648 2.9535 115.3620 3.5822 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956 12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # TODO check _oxford_atom_site_special_shape 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Au1 Au 0.38637(3) 1.69431(2) 0.18364(2) 0.0387 1.0000 Uani . . . . . . Tb1 Tb 0.29578(3) 1.19300(2) 0.25166(2) 0.0271 1.0000 Uani . . . . . . O1 O 0.3831(5) 1.2394(5) 0.0436(4) 0.0520 1.0000 Uani . . . . . . O2 O 0.1823(5) 1.2985(5) 0.0991(4) 0.0552 1.0000 Uani . . . . . . O3 O 0.2672(6) 1.3399(6) -0.0818(5) 0.0857 1.0000 Uani . . . . . . O4 O 0.2308(4) 1.0176(4) 0.4141(4) 0.0406 1.0000 Uani . . . . . . O5 O 0.0763(6) 0.9117(5) 0.4259(5) 0.0766 1.0000 Uani . . . . . . O6 O 0.1130(4) 1.0748(4) 0.2862(4) 0.0446 1.0000 Uani . . . . . . N1 N 0.1082(5) 1.3020(5) 0.3722(4) 0.0344 1.0000 Uani . . . . . . N2 N 0.0043(5) 1.3436(5) 0.5424(5) 0.0408 1.0000 Uani . . . . . . N3 N 0.3373(5) 1.2255(4) 0.4380(4) 0.0304 1.0000 Uani . . . . . . N4 N 0.5218(5) 1.1333(4) 0.2758(4) 0.0329 1.0000 Uani . . . . . . N5 N 0.6753(5) 1.0926(5) 0.3791(4) 0.0363 1.0000 Uani . . . . . . N6 N 0.3676(6) 0.9824(5) 0.1911(5) 0.0439 1.0000 Uani . . . . . . N7 N 0.3610(6) 1.4074(5) 0.2073(5) 0.0461 1.0000 Uani . . . . . . N8 N 0.2774(7) 1.2933(6) 0.0160(5) 0.0516 1.0000 Uani . . . . . . N9 N 0.1367(5) 0.9991(5) 0.3770(5) 0.0409 1.0000 Uani . . . . . . N10 N 0.0493(7) 0.6487(8) 0.2178(6) 0.0729 1.0000 Uani . . . . . . C1 C -0.0217(6) 1.3384(5) 0.3701(5) 0.0354 1.0000 Uani . . . . . . C2 C -0.0888(7) 1.3509(7) 0.2827(6) 0.0488 1.0000 Uani . . . . . . C3 C -0.2200(7) 1.3874(7) 0.3062(6) 0.0495 1.0000 Uani . . . . . . C4 C -0.2834(7) 1.4100(6) 0.4145(7) 0.0500 1.0000 Uani . . . . . . C5 C -0.2200(7) 1.4002(6) 0.5013(6) 0.0450 1.0000 Uani . . . . . . C6 C -0.0880(6) 1.3658(5) 0.4756(5) 0.0359 1.0000 Uani . . . . . . C7 C 0.1188(6) 1.3058(5) 0.4767(5) 0.0334 1.0000 Uani . . . . . . C8 C 0.2405(6) 1.2682(5) 0.5156(5) 0.0342 1.0000 Uani . . . . . . C9 C 0.2569(7) 1.2773(6) 0.6232(5) 0.0414 1.0000 Uani . . . . . . C10 C 0.3780(7) 1.2394(6) 0.6485(6) 0.0474 1.0000 Uani . . . . . . C11 C 0.4772(7) 1.1923(6) 0.5710(5) 0.0410 1.0000 Uani . . . . . . C12 C 0.4532(6) 1.1870(5) 0.4642(5) 0.0334 1.0000 Uani . . . . . . C13 C 0.5515(6) 1.1387(5) 0.3745(5) 0.0322 1.0000 Uani . . . . . . C14 C 0.7313(6) 1.0567(6) 0.2772(6) 0.0387 1.0000 Uani . . . . . . C15 C 0.8548(6) 0.9992(7) 0.2366(6) 0.0470 1.0000 Uani . . . . . . C16 C 0.8788(7) 0.9727(7) 0.1295(7) 0.0521 1.0000 Uani . . . . . . C17 C 0.7823(7) 0.9981(7) 0.0645(7) 0.0533 1.0000 Uani . . . . . . C18 C 0.6606(6) 1.0515(7) 0.1041(6) 0.0422 1.0000 Uani . . . . . . C19 C 0.6352(6) 1.0820(5) 0.2115(5) 0.0340 1.0000 Uani . . . . . . C20 C 0.3786(6) 0.8780(6) 0.1829(5) 0.0351 1.0000 Uani . . . . . . C22 C 0.3779(7) 1.5108(6) 0.1951(6) 0.0432 1.0000 Uani . . . . . . C23 C 0.1280(12) 0.6468(11) 0.0035(7) 0.1015 1.0000 Uani . . . . . . C24 C 0.0822(8) 0.6476(7) 0.1253(7) 0.0593 1.0000 Uani . . . . . . H21 H -0.0462 1.3335 0.2119 0.0599 1.0000 Uiso R . . . . . H31 H -0.2669 1.3974 0.2494 0.0632 1.0000 Uiso R . . . . . H41 H -0.3718 1.4319 0.4282 0.0588 1.0000 Uiso R . . . . . H51 H -0.2612 1.4160 0.5725 0.0581 1.0000 Uiso R . . . . . H91 H 0.1884 1.3075 0.6761 0.0498 1.0000 Uiso R . . . . . H101 H 0.3921 1.2451 0.7188 0.0582 1.0000 Uiso R . . . . . H111 H 0.5583 1.1639 0.5872 0.0500 1.0000 Uiso R . . . . . H151 H 0.9177 0.9806 0.2801 0.0577 1.0000 Uiso R . . . . . H161 H 0.9610 0.9378 0.0987 0.0640 1.0000 Uiso R . . . . . H171 H 0.8017 0.9780 -0.0076 0.0660 1.0000 Uiso R . . . . . H181 H 0.5971 1.0667 0.0617 0.0529 1.0000 Uiso R . . . . . H232 H 0.0864 0.7215 -0.0412 0.1579 1.0000 Uiso R . . . . . H231 H 0.2187 0.6474 -0.0159 0.1581 1.0000 Uiso R . . . . . H233 H 0.1086 0.5717 -0.0125 0.1580 1.0000 Uiso R . . . . . H22 H -0.0098 1.3534 0.6194 0.13(4) 1.0000 Uiso R . . . . . H52 H 0.7162 1.0869 0.4411 0.09(3) 1.0000 Uiso 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 Au1 0.05412(19) 0.02521(13) 0.03999(16) -0.00863(11) -0.00898(13) -0.01168(12) Tb1 0.03562(18) 0.02256(15) 0.02621(16) -0.00333(12) -0.01123(13) -0.00729(12) O1 0.057(3) 0.051(3) 0.037(3) -0.006(2) -0.003(2) 0.006(2) O2 0.048(3) 0.075(3) 0.036(3) 0.002(2) -0.015(2) -0.002(3) O3 0.104(5) 0.100(5) 0.038(3) 0.014(3) -0.027(3) 0.001(4) O4 0.046(3) 0.045(2) 0.034(2) -0.0013(19) -0.015(2) -0.015(2) O5 0.085(4) 0.058(3) 0.089(4) 0.019(3) -0.029(4) -0.042(3) O6 0.047(3) 0.042(3) 0.051(3) -0.002(2) -0.024(2) -0.016(2) N1 0.035(3) 0.041(3) 0.024(3) -0.006(2) -0.002(2) -0.004(2) N2 0.057(4) 0.035(3) 0.034(3) -0.008(2) -0.012(3) -0.010(3) N3 0.039(3) 0.028(2) 0.029(3) -0.004(2) -0.013(2) -0.011(2) N4 0.035(3) 0.033(3) 0.035(3) -0.008(2) -0.012(2) -0.005(2) N5 0.033(3) 0.047(3) 0.037(3) -0.006(2) -0.021(2) -0.012(2) N6 0.054(4) 0.035(3) 0.047(3) -0.013(2) -0.011(3) -0.009(3) N7 0.059(4) 0.032(3) 0.046(3) -0.005(3) -0.006(3) -0.013(3) N8 0.075(5) 0.045(3) 0.034(3) -0.003(3) -0.017(3) -0.005(3) N9 0.044(3) 0.030(3) 0.049(3) -0.001(2) -0.008(3) -0.015(2) N10 0.077(5) 0.098(6) 0.042(4) -0.028(4) -0.011(4) 0.006(4) C1 0.042(4) 0.026(3) 0.035(3) -0.004(2) -0.003(3) -0.006(3) C2 0.049(4) 0.063(5) 0.036(4) -0.012(3) -0.012(3) -0.008(4) C3 0.039(4) 0.061(4) 0.052(4) -0.012(4) -0.019(3) -0.005(3) C4 0.040(4) 0.041(4) 0.064(5) -0.008(3) -0.002(4) -0.006(3) C5 0.053(4) 0.040(4) 0.039(4) -0.010(3) -0.002(3) -0.005(3) C6 0.048(4) 0.029(3) 0.028(3) 0.002(2) -0.004(3) -0.011(3) C7 0.042(4) 0.028(3) 0.029(3) -0.006(2) -0.006(3) -0.004(3) C8 0.049(4) 0.032(3) 0.026(3) -0.007(2) -0.010(3) -0.012(3) C9 0.052(4) 0.039(3) 0.036(4) -0.008(3) -0.012(3) -0.007(3) C10 0.065(5) 0.052(4) 0.039(4) -0.013(3) -0.026(4) -0.017(4) C11 0.049(4) 0.044(4) 0.039(4) -0.008(3) -0.024(3) -0.011(3) C12 0.048(4) 0.023(3) 0.034(3) -0.001(2) -0.016(3) -0.011(3) C13 0.040(4) 0.031(3) 0.029(3) 0.002(2) -0.013(3) -0.014(3) C14 0.041(4) 0.036(3) 0.040(4) -0.001(3) -0.016(3) -0.007(3) C15 0.036(4) 0.052(4) 0.053(4) 0.000(3) -0.018(3) -0.010(3) C16 0.034(4) 0.063(5) 0.057(5) -0.010(4) -0.005(3) -0.007(3) C17 0.050(5) 0.058(4) 0.052(4) -0.015(4) -0.006(4) -0.009(4) C18 0.035(4) 0.059(4) 0.039(4) -0.020(3) -0.010(3) -0.005(3) C19 0.037(4) 0.030(3) 0.040(4) -0.005(3) -0.020(3) -0.004(3) C20 0.050(4) 0.030(3) 0.030(3) -0.011(3) -0.009(3) -0.010(3) C22 0.053(4) 0.033(4) 0.044(4) -0.009(3) -0.007(3) -0.006(3) C23 0.159(11) 0.103(8) 0.041(5) -0.020(5) -0.023(6) -0.004(7) C24 0.061(5) 0.058(5) 0.055(5) -0.010(4) -0.016(4) 0.003(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Au1 . C20 1_565 1.982(6) yes Au1 . C22 . 1.986(6) yes Tb1 . O1 . 2.465(4) yes Tb1 . O2 . 2.409(4) yes Tb1 . O4 . 2.469(4) yes Tb1 . O6 . 2.468(4) yes Tb1 . N1 . 2.499(5) yes Tb1 . N3 . 2.547(4) yes Tb1 . N4 . 2.479(5) yes Tb1 . N6 . 2.508(5) yes Tb1 . N7 . 2.465(5) yes Tb1 . N8 . 2.865(6) yes Tb1 . N9 . 2.891(5) yes O1 . N8 . 1.263(7) yes O2 . N8 . 1.272(8) yes O3 . N8 . 1.203(7) yes O4 . N9 . 1.277(6) yes O5 . N9 . 1.212(7) yes O6 . N9 . 1.258(6) yes N1 . C1 . 1.392(8) yes N1 . C7 . 1.324(7) yes N2 . C6 . 1.388(8) yes N2 . C7 . 1.362(8) yes N2 . H22 . 0.950 no N3 . C8 . 1.336(8) yes N3 . C12 . 1.333(8) yes N4 . C13 . 1.340(7) yes N4 . C19 . 1.393(8) yes N5 . C13 . 1.348(8) yes N5 . C14 . 1.369(8) yes N5 . H52 . 0.950 no N6 . C20 . 1.147(7) yes N7 . C22 . 1.144(8) yes N10 . C24 . 1.108(10) yes C1 . C2 . 1.397(9) yes C1 . C6 . 1.396(8) yes C2 . C3 . 1.382(10) yes C2 . H21 . 0.927 no C3 . C4 . 1.402(10) yes C3 . H31 . 0.928 no C4 . C5 . 1.369(10) yes C4 . H41 . 0.927 no C5 . C6 . 1.388(9) yes C5 . H51 . 0.923 no C7 . C8 . 1.459(9) yes C8 . C9 . 1.400(8) yes C9 . C10 . 1.382(9) yes C9 . H91 . 0.929 no C10 . C11 . 1.367(10) yes C10 . H101 . 0.928 no C11 . C12 . 1.410(8) yes C11 . H111 . 0.924 no C12 . C13 . 1.463(9) yes C14 . C15 . 1.396(10) yes C14 . C19 . 1.408(8) yes C15 . C16 . 1.368(10) yes C15 . H151 . 0.924 no C16 . C17 . 1.406(10) yes C16 . H161 . 0.930 no C17 . C18 . 1.362(9) yes C17 . H171 . 0.929 no C18 . C19 . 1.390(9) yes C18 . H181 . 0.924 no C23 . C24 . 1.460(12) yes C23 . H232 . 0.959 no C23 . H231 . 0.957 no C23 . H233 . 0.957 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C20 1_565 Au1 . C22 . 174.4(3) yes O1 . Tb1 . O2 . 52.18(17) yes O1 . Tb1 . O4 . 142.32(15) yes O2 . Tb1 . O4 . 126.92(16) yes O1 . Tb1 . O6 . 108.16(16) yes O2 . Tb1 . O6 . 75.45(16) yes O4 . Tb1 . O6 . 51.65(14) yes O1 . Tb1 . N1 . 131.66(15) yes O2 . Tb1 . N1 . 83.28(17) yes O4 . Tb1 . N1 . 76.95(15) yes O6 . Tb1 . N1 . 71.58(16) yes O1 . Tb1 . N3 . 140.04(16) yes O2 . Tb1 . N3 . 141.12(17) yes O4 . Tb1 . N3 . 68.83(14) yes O6 . Tb1 . N3 . 111.80(15) yes N1 . Tb1 . N3 . 64.86(16) yes O1 . Tb1 . N4 . 86.20(17) yes O2 . Tb1 . N4 . 137.34(17) yes O4 . Tb1 . N4 . 90.74(15) yes O6 . Tb1 . N4 . 134.83(15) yes N1 . Tb1 . N4 . 129.52(16) yes O1 . Tb1 . N6 . 72.61(17) yes O2 . Tb1 . N6 . 97.27(18) yes O4 . Tb1 . N6 . 70.30(16) yes O6 . Tb1 . N6 . 69.20(17) yes N1 . Tb1 . N6 . 139.21(17) yes O1 . Tb1 . N7 . 74.20(17) yes O2 . Tb1 . N7 . 79.85(19) yes O4 . Tb1 . N7 . 142.02(16) yes O6 . Tb1 . N7 . 144.77(18) yes N1 . Tb1 . N7 . 81.00(18) yes O1 . Tb1 . N8 . 26.06(17) yes O2 . Tb1 . N8 . 26.12(17) yes O4 . Tb1 . N8 . 140.93(15) yes O6 . Tb1 . N8 . 92.03(17) yes N1 . Tb1 . N8 . 107.74(17) yes O1 . Tb1 . N9 . 126.93(16) yes O2 . Tb1 . N9 . 101.05(17) yes O4 . Tb1 . N9 . 26.06(14) yes O6 . Tb1 . N9 . 25.63(14) yes N1 . Tb1 . N9 . 73.44(16) yes N3 . Tb1 . N4 . 65.03(16) yes N3 . Tb1 . N6 . 121.30(16) yes N4 . Tb1 . N6 . 75.35(17) yes N3 . Tb1 . N7 . 73.90(16) yes N4 . Tb1 . N7 . 79.93(17) yes N6 . Tb1 . N7 . 139.49(18) yes N3 . Tb1 . N8 . 149.21(15) yes N4 . Tb1 . N8 . 111.82(18) yes N6 . Tb1 . N8 . 84.59(17) yes N7 . Tb1 . N8 . 75.42(17) yes N3 . Tb1 . N9 . 91.04(15) yes N4 . Tb1 . N9 . 113.19(15) yes N6 . Tb1 . N9 . 66.41(17) yes N7 . Tb1 . N9 . 154.07(18) yes N8 . Tb1 . N9 . 116.30(17) yes Tb1 . O1 . N8 . 94.9(4) yes Tb1 . O2 . N8 . 97.4(4) yes Tb1 . O4 . N9 . 95.8(3) yes Tb1 . O6 . N9 . 96.3(3) yes Tb1 . N1 . C1 . 135.4(4) yes Tb1 . N1 . C7 . 117.7(4) yes C1 . N1 . C7 . 105.1(5) yes C6 . N2 . C7 . 107.2(5) yes C6 . N2 . H22 . 126.2 no C7 . N2 . H22 . 126.5 no Tb1 . N3 . C8 . 120.3(4) yes Tb1 . N3 . C12 . 120.1(4) yes C8 . N3 . C12 . 119.2(5) yes Tb1 . N4 . C13 . 119.3(4) yes Tb1 . N4 . C19 . 135.0(4) yes C13 . N4 . C19 . 105.5(5) yes C13 . N5 . C14 . 107.1(5) yes C13 . N5 . H52 . 126.4 no C14 . N5 . H52 . 126.4 no Tb1 . N6 . C20 . 164.8(5) yes Tb1 . N7 . C22 . 171.9(6) yes Tb1 . N8 . O2 . 56.5(3) yes Tb1 . N8 . O1 . 59.0(3) yes O2 . N8 . O1 . 115.5(5) yes Tb1 . N8 . O3 . 177.4(5) yes O2 . N8 . O3 . 121.8(7) yes O1 . N8 . O3 . 122.6(7) yes O4 . N9 . Tb1 . 58.2(3) yes O4 . N9 . O6 . 116.1(5) yes Tb1 . N9 . O6 . 58.0(3) yes O4 . N9 . O5 . 121.3(5) yes Tb1 . N9 . O5 . 175.5(5) yes O6 . N9 . O5 . 122.6(6) yes N1 . C1 . C2 . 130.6(6) yes N1 . C1 . C6 . 109.9(5) yes C2 . C1 . C6 . 119.4(6) yes C1 . C2 . C3 . 117.8(6) yes C1 . C2 . H21 . 120.6 no C3 . C2 . H21 . 121.6 no C2 . C3 . C4 . 120.9(6) yes C2 . C3 . H31 . 119.7 no C4 . C3 . H31 . 119.4 no C3 . C4 . C5 . 122.5(7) yes C3 . C4 . H41 . 118.8 no C5 . C4 . H41 . 118.6 no C4 . C5 . C6 . 115.8(6) yes C4 . C5 . H51 . 122.9 no C6 . C5 . H51 . 121.4 no C1 . C6 . C5 . 123.5(6) yes C1 . C6 . N2 . 105.2(6) yes C5 . C6 . N2 . 131.3(6) yes N2 . C7 . N1 . 112.6(5) yes N2 . C7 . C8 . 125.1(5) yes N1 . C7 . C8 . 122.3(5) yes C7 . C8 . N3 . 113.7(5) yes C7 . C8 . C9 . 124.0(6) yes N3 . C8 . C9 . 122.3(6) yes C8 . C9 . C10 . 117.9(6) yes C8 . C9 . H91 . 121.1 no C10 . C9 . H91 . 121.0 no C9 . C10 . C11 . 120.4(6) yes C9 . C10 . H101 . 119.9 no C11 . C10 . H101 . 119.7 no C10 . C11 . C12 . 118.3(6) yes C10 . C11 . H111 . 121.8 no C12 . C11 . H111 . 120.0 no C11 . C12 . N3 . 121.9(6) yes C11 . C12 . C13 . 123.2(6) yes N3 . C12 . C13 . 114.9(5) yes C12 . C13 . N5 . 127.1(5) yes C12 . C13 . N4 . 120.4(5) yes N5 . C13 . N4 . 112.5(5) yes N5 . C14 . C15 . 132.1(6) yes N5 . C14 . C19 . 106.9(6) yes C15 . C14 . C19 . 121.0(6) yes C14 . C15 . C16 . 117.1(6) yes C14 . C15 . H151 . 121.3 no C16 . C15 . H151 . 121.6 no C15 . C16 . C17 . 121.6(7) yes C15 . C16 . H161 . 119.2 no C17 . C16 . H161 . 119.2 no C16 . C17 . C18 . 121.9(7) yes C16 . C17 . H171 . 119.3 no C18 . C17 . H171 . 118.8 no C17 . C18 . C19 . 117.4(6) yes C17 . C18 . H181 . 121.7 no C19 . C18 . H181 . 121.0 no C14 . C19 . N4 . 108.0(5) yes C14 . C19 . C18 . 121.0(6) yes N4 . C19 . C18 . 130.9(5) yes Au1 1_545 C20 . N6 . 174.4(6) yes Au1 . C22 . N7 . 173.3(6) yes C24 . C23 . H232 . 109.2 no C24 . C23 . H231 . 109.6 no H232 . C23 . H231 . 109.4 no C24 . C23 . H233 . 109.6 no H232 . C23 . H233 . 109.4 no H231 . C23 . H233 . 109.6 no C23 . C24 . N10 . 178.8(10) yes _database_code_depnum_ccdc_archive 'CCDC 952847' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_JT2-9d #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C23 H16 Au1 Gd1 N10 O6' _chemical_formula_moiety 'C23 H16 Au1 Gd1 N10 O6' _chemical_formula_weight 882.66 #============================================================= # 6. CRYSTAL DATA _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 10.847(2) _cell_length_b 10.8781(19) _cell_length_c 12.255(2) _cell_angle_alpha 75.675(10) _cell_angle_beta 76.336(9) _cell_angle_gamma 78.430(10) _cell_volume 1345.9(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9192 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 29.00 _cell_measurement_temperature 296(2) _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_min 0.099 _exptl_crystal_size_mid 0.114 _exptl_crystal_size_max 0.221 _exptl_crystal_density_diffrn 2.178 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 830 _exptl_absorpt_coefficient_mu 7.945 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(Sheldrich , 1996)' _exptl_absorpt_correction_T_min 0.4796 _exptl_absorpt_correction_T_max 0.7454 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 15846 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_min 1.749 _diffrn_reflns_theta_max 26.451 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.922 _diffrn_measured_fraction_theta_full 0.9976 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 4633 _refine_ls_number_restraints 0 _refine_ls_number_parameters 386 _oxford_refine_ls_R_factor_ref 0.0200 _refine_ls_wR_factor_ref 0.0151 _refine_ls_goodness_of_fit_ref 1.1238 # The values computed from all data _oxford_reflns_number_all 5498 _refine_ls_R_factor_all 0.0254 _refine_ls_wR_factor_all 0.0164 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4696 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_gt 0.0152 _reflns_number_total 5498 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.387 0.420 0.417 0.210 0.143 ; _refine_ls_shift/su_max 0.0027059 _refine_diff_density_min -0.41 _refine_diff_density_max 0.66 _reflns_limit_h_min -12 _reflns_limit_h_max 13 _reflns_limit_k_min -12 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_refine_ls_scale 0.11124(7) _oxford_diffrn_Wilson_B_factor 2.42 _oxford_diffrn_Wilson_scale 85.52 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 5498 # Theoretical number of reflections is about 11072 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.1653 3.9035 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956 12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # TODO check _oxford_atom_site_special_shape 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Au1 Au 0.112710(14) 1.305735(12) 0.317710(12) 0.0369 1.0000 Uani . . . . . . Gd1 Gd 0.204934(15) 0.806462(13) 0.249017(12) 0.0251 1.0000 Uani . . . . . . O1 O 0.2696(2) 0.9821(2) 0.0855(2) 0.0388 1.0000 Uani . . . . . . O2 O 0.3884(2) 0.9259(2) 0.2127(2) 0.0428 1.0000 Uani . . . . . . O3 O 0.4232(3) 1.0888(3) 0.0745(3) 0.0728 1.0000 Uani . . . . . . O4 O 0.3197(3) 0.6989(3) 0.4027(2) 0.0545 1.0000 Uani . . . . . . O5 O 0.1204(3) 0.7610(3) 0.4594(2) 0.0518 1.0000 Uani . . . . . . O6 O 0.2364(4) 0.6587(4) 0.5831(3) 0.0840 1.0000 Uani . . . . . . N1 N -0.0213(3) 0.8666(2) 0.2235(2) 0.0321 1.0000 Uani . . . . . . N2 N -0.1742(3) 0.9069(3) 0.1209(2) 0.0348 1.0000 Uani . . . . . . N3 N 0.1637(3) 0.7750(2) 0.0606(2) 0.0290 1.0000 Uani . . . . . . N4 N 0.3930(3) 0.6970(3) 0.1270(2) 0.0347 1.0000 Uani . . . . . . N5 N 0.4961(3) 0.6559(3) -0.0445(2) 0.0358 1.0000 Uani . . . . . . N6 N 0.1372(3) 0.5914(3) 0.2938(3) 0.0451 1.0000 Uani . . . . . . N7 N 0.1312(3) 1.0185(3) 0.3108(3) 0.0408 1.0000 Uani . . . . . . N8 N 0.3635(3) 1.0018(3) 0.1233(3) 0.0400 1.0000 Uani . . . . . . N9 N 0.2249(4) 0.7055(3) 0.4857(3) 0.0470 1.0000 Uani . . . . . . N10 N 0.4489(4) 0.3520(5) 0.2850(4) 0.0748 1.0000 Uani . . . . . . C1 C -0.1349(3) 0.9184(3) 0.2870(3) 0.0315 1.0000 Uani . . . . . . C2 C -0.1611(4) 0.9488(4) 0.3954(3) 0.0423 1.0000 Uani . . . . . . C3 C -0.2836(4) 1.0023(4) 0.4353(4) 0.0509 1.0000 Uani . . . . . . C4 C -0.3794(4) 1.0283(4) 0.3698(4) 0.0543 1.0000 Uani . . . . . . C5 C -0.3554(4) 0.9993(4) 0.2628(4) 0.0474 1.0000 Uani . . . . . . C6 C -0.2314(3) 0.9448(3) 0.2229(3) 0.0340 1.0000 Uani . . . . . . C7 C -0.0503(3) 0.8616(3) 0.1243(3) 0.0318 1.0000 Uani . . . . . . C8 C 0.0467(3) 0.8129(3) 0.0341(3) 0.0319 1.0000 Uani . . . . . . C9 C 0.0233(4) 0.8065(3) -0.0712(3) 0.0385 1.0000 Uani . . . . . . C10 C 0.1223(4) 0.7612(4) -0.1496(3) 0.0446 1.0000 Uani . . . . . . C11 C 0.2440(4) 0.7213(3) -0.1227(3) 0.0415 1.0000 Uani . . . . . . C12 C 0.2597(3) 0.7304(3) -0.0165(3) 0.0325 1.0000 Uani . . . . . . C13 C 0.3832(3) 0.6933(3) 0.0210(3) 0.0339 1.0000 Uani . . . . . . C14 C 0.5883(3) 0.6354(3) 0.0218(3) 0.0363 1.0000 Uani . . . . . . C15 C 0.7206(4) 0.5982(4) -0.0030(3) 0.0454 1.0000 Uani . . . . . . C16 C 0.7853(4) 0.5889(4) 0.0834(4) 0.0480 1.0000 Uani . . . . . . C17 C 0.7214(4) 0.6126(4) 0.1908(4) 0.0506 1.0000 Uani . . . . . . C18 C 0.5908(4) 0.6492(4) 0.2151(3) 0.0469 1.0000 Uani . . . . . . C19 C 0.5234(3) 0.6602(3) 0.1280(3) 0.0357 1.0000 Uani . . . . . . C20 C 0.1207(4) 0.4890(3) 0.3071(3) 0.0418 1.0000 Uani . . . . . . C21 C 0.1207(3) 1.1229(3) 0.3167(3) 0.0337 1.0000 Uani . . . . . . C22 C 0.3704(9) 0.3506(7) 0.4987(5) 0.1049 1.0000 Uani . . . . . . C23 C 0.4154(5) 0.3528(4) 0.3774(4) 0.0580 1.0000 Uani . . . . . . H21 H -0.0980 0.9317 0.4381 0.031(9) 1.0000 Uiso R . . . . . H22 H -0.2150 0.9118 0.0590 0.045(10) 1.0000 Uiso R . . . . . H31 H -0.3038 1.0219 0.5080 0.040(10) 1.0000 Uiso R . . . . . H41 H -0.4626 1.0655 0.3993 0.079(16) 1.0000 Uiso R . . . . . H51 H -0.4191 1.0150 0.2193 0.055(12) 1.0000 Uiso R . . . . . H52 H 0.5097 0.6457 -0.1215 0.080(16) 1.0000 Uiso R . . . . . H91 H -0.0593 0.8331 -0.0867 0.022(8) 1.0000 Uiso R . . . . . H101 H 0.1092 0.7576 -0.2202 0.077(15) 1.0000 Uiso R . . . . . H111 H 0.3135 0.6884 -0.1747 0.063(14) 1.0000 Uiso R . . . . . H151 H 0.7635 0.5816 -0.0744 0.043(10) 1.0000 Uiso R . . . . . H161 H 0.8749 0.5657 0.0697 0.054(12) 1.0000 Uiso R . . . . . H171 H 0.7690 0.6023 0.2472 0.062(13) 1.0000 Uiso R . . . . . H181 H 0.5487 0.6661 0.2869 0.047(11) 1.0000 Uiso R . . . . . H221 H 0.3903 0.2652 0.5403 0.11(2) 1.0000 Uiso R . . . . . H222 H 0.4134 0.4084 0.5186 0.16(3) 1.0000 Uiso R . . . . . H223 H 0.2792 0.3786 0.5114 0.22(6) 1.0000 Uiso 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 Au1 0.05138(10) 0.02429(7) 0.03745(8) -0.00676(6) -0.00772(6) -0.01219(6) Gd1 0.03256(9) 0.02149(8) 0.02347(8) -0.00162(6) -0.00992(6) -0.00757(6) O1 0.0491(15) 0.0367(12) 0.0331(12) 0.0021(10) -0.0167(11) -0.0139(11) O2 0.0435(14) 0.0392(13) 0.0501(15) 0.0020(12) -0.0248(13) -0.0120(11) O3 0.077(2) 0.0516(17) 0.088(2) 0.0208(16) -0.0237(18) -0.0410(16) O4 0.0452(16) 0.077(2) 0.0331(14) 0.0026(13) -0.0111(12) -0.0037(14) O5 0.0557(17) 0.0553(16) 0.0335(14) -0.0047(12) -0.0034(12) 0.0047(14) O6 0.109(3) 0.097(3) 0.0311(16) 0.0094(16) -0.0253(17) 0.004(2) N1 0.0375(16) 0.0302(13) 0.0311(14) -0.0037(11) -0.0147(12) -0.0050(12) N2 0.0349(16) 0.0417(15) 0.0311(15) -0.0013(12) -0.0151(12) -0.0111(12) N3 0.0377(15) 0.0251(12) 0.0268(13) -0.0026(10) -0.0104(12) -0.0093(11) N4 0.0373(16) 0.0368(15) 0.0314(14) -0.0059(12) -0.0107(12) -0.0056(12) N5 0.0461(18) 0.0339(14) 0.0275(14) -0.0057(12) -0.0043(13) -0.0105(13) N6 0.061(2) 0.0292(15) 0.0461(18) -0.0049(13) -0.0117(15) -0.0115(14) N7 0.0533(19) 0.0284(15) 0.0429(17) -0.0082(12) -0.0106(14) -0.0089(13) N8 0.0407(17) 0.0332(15) 0.0471(18) -0.0006(13) -0.0106(14) -0.0152(13) N9 0.067(2) 0.0425(17) 0.0275(16) 0.0011(13) -0.0109(16) -0.0078(16) N10 0.070(3) 0.097(3) 0.053(3) -0.021(2) -0.013(2) 0.006(2) C1 0.0311(17) 0.0310(16) 0.0338(17) -0.0031(13) -0.0092(14) -0.0088(13) C2 0.039(2) 0.056(2) 0.0340(19) -0.0116(16) -0.0104(16) -0.0068(17) C3 0.046(2) 0.065(3) 0.042(2) -0.0141(19) -0.0061(18) -0.0099(19) C4 0.036(2) 0.062(3) 0.057(3) -0.006(2) -0.0020(19) -0.0062(19) C5 0.035(2) 0.054(2) 0.049(2) 0.0033(18) -0.0135(17) -0.0105(17) C6 0.0354(18) 0.0318(16) 0.0355(18) 0.0024(14) -0.0134(14) -0.0108(14) C7 0.0393(19) 0.0271(15) 0.0336(17) 0.0004(13) -0.0173(14) -0.0120(13) C8 0.0421(19) 0.0254(15) 0.0326(17) -0.0028(13) -0.0124(14) -0.0134(14) C9 0.047(2) 0.0405(18) 0.0340(18) -0.0049(15) -0.0186(16) -0.0119(16) C10 0.061(3) 0.052(2) 0.0276(18) -0.0099(16) -0.0167(17) -0.0148(18) C11 0.057(2) 0.0399(18) 0.0317(18) -0.0064(15) -0.0129(17) -0.0122(17) C12 0.046(2) 0.0256(15) 0.0273(16) -0.0021(12) -0.0090(14) -0.0120(14) C13 0.042(2) 0.0310(16) 0.0306(17) -0.0062(13) -0.0075(15) -0.0100(14) C14 0.045(2) 0.0300(16) 0.0315(17) -0.0017(13) -0.0060(15) -0.0072(14) C15 0.044(2) 0.0401(19) 0.046(2) -0.0075(16) 0.0023(17) -0.0055(16) C16 0.037(2) 0.044(2) 0.056(2) 0.0001(18) -0.0070(18) -0.0050(16) C17 0.045(2) 0.056(2) 0.052(2) -0.0098(19) -0.0184(19) -0.0043(18) C18 0.047(2) 0.061(2) 0.0320(19) -0.0048(17) -0.0137(17) -0.0071(18) C19 0.0372(19) 0.0323(17) 0.0351(18) -0.0032(14) -0.0063(15) -0.0052(14) C20 0.056(2) 0.0283(17) 0.043(2) -0.0110(15) -0.0071(17) -0.0101(16) C21 0.045(2) 0.0272(16) 0.0326(17) -0.0069(13) -0.0079(15) -0.0131(14) C22 0.171(8) 0.093(5) 0.046(3) -0.015(3) -0.024(4) -0.006(5) C23 0.063(3) 0.068(3) 0.045(3) -0.014(2) -0.020(2) 0.002(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Au1 . C20 1_565 1.983(3) yes Au1 . C21 . 1.976(3) yes Gd1 . O1 . 2.477(2) yes Gd1 . O2 . 2.486(2) yes Gd1 . O4 . 2.429(3) yes Gd1 . O5 . 2.483(3) yes Gd1 . N1 . 2.484(3) yes Gd1 . N3 . 2.567(2) yes Gd1 . N4 . 2.506(3) yes Gd1 . N6 . 2.485(3) yes Gd1 . N7 . 2.524(3) yes Gd1 . N8 . 2.905(3) yes Gd1 . N9 . 2.879(3) yes O1 . N8 . 1.288(4) yes O2 . N8 . 1.248(4) yes O3 . N8 . 1.206(4) yes O4 . N9 . 1.268(4) yes O5 . N9 . 1.247(4) yes O6 . N9 . 1.202(4) yes N1 . C1 . 1.388(4) yes N1 . C7 . 1.341(4) yes N2 . C6 . 1.381(5) yes N2 . C7 . 1.342(4) yes N2 . H22 . 0.950 no N3 . C8 . 1.343(4) yes N3 . C12 . 1.332(4) yes N4 . C13 . 1.339(4) yes N4 . C19 . 1.393(4) yes N5 . C13 . 1.345(5) yes N5 . C14 . 1.385(5) yes N5 . H52 . 0.950 no N6 . C20 . 1.130(4) yes N7 . C21 . 1.137(4) yes N10 . C23 . 1.107(6) yes C1 . C2 . 1.399(5) yes C1 . C6 . 1.397(5) yes C2 . C3 . 1.366(5) yes C2 . H21 . 0.921 no C3 . C4 . 1.404(6) yes C3 . H31 . 0.932 no C4 . C5 . 1.377(6) yes C4 . H41 . 0.938 no C5 . C6 . 1.382(5) yes C5 . H51 . 0.935 no C7 . C8 . 1.459(5) yes C8 . C9 . 1.393(5) yes C9 . C10 . 1.361(6) yes C9 . H91 . 0.933 no C10 . C11 . 1.394(6) yes C10 . H101 . 0.922 no C11 . C12 . 1.381(5) yes C11 . H111 . 0.937 no C12 . C13 . 1.466(5) yes C14 . C15 . 1.392(5) yes C14 . C19 . 1.388(5) yes C15 . C16 . 1.376(6) yes C15 . H151 . 0.931 no C16 . C17 . 1.395(6) yes C16 . H161 . 0.939 no C17 . C18 . 1.373(6) yes C17 . H171 . 0.930 no C18 . C19 . 1.400(5) yes C18 . H181 . 0.934 no C22 . C23 . 1.447(7) yes C22 . H221 . 0.952 no C22 . H222 . 0.959 no C22 . H223 . 0.962 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C20 1_565 Au1 . C21 . 174.32(15) yes O1 . Gd1 . O2 . 51.37(7) yes O1 . Gd1 . O4 . 127.13(9) yes O2 . Gd1 . O4 . 75.95(9) yes O1 . Gd1 . O5 . 142.05(9) yes O2 . Gd1 . O5 . 107.55(9) yes O4 . Gd1 . O5 . 51.46(10) yes O1 . Gd1 . N1 . 90.51(9) yes O2 . Gd1 . N1 . 134.61(8) yes O4 . Gd1 . N1 . 137.68(9) yes O5 . Gd1 . N1 . 87.47(10) yes O1 . Gd1 . N3 . 68.32(8) yes O2 . Gd1 . N3 . 111.15(8) yes O4 . Gd1 . N3 . 141.16(10) yes O5 . Gd1 . N3 . 141.29(9) yes N1 . Gd1 . N3 . 64.62(9) yes O1 . Gd1 . N4 . 76.61(9) yes O2 . Gd1 . N4 . 71.58(9) yes O4 . Gd1 . N4 . 83.54(10) yes O5 . Gd1 . N4 . 131.60(9) yes N1 . Gd1 . N4 . 128.77(9) yes O1 . Gd1 . N6 . 141.77(9) yes O2 . Gd1 . N6 . 145.66(10) yes O4 . Gd1 . N6 . 80.18(11) yes O5 . Gd1 . N6 . 74.75(10) yes N1 . Gd1 . N6 . 79.15(10) yes O1 . Gd1 . N7 . 70.73(9) yes O2 . Gd1 . N7 . 69.39(10) yes O4 . Gd1 . N7 . 97.31(10) yes O5 . Gd1 . N7 . 72.08(10) yes N1 . Gd1 . N7 . 75.60(10) yes O1 . Gd1 . N8 . 26.17(8) yes O2 . Gd1 . N8 . 25.26(8) yes O4 . Gd1 . N8 . 101.20(9) yes O5 . Gd1 . N8 . 125.96(10) yes N1 . Gd1 . N8 . 112.98(9) yes O1 . Gd1 . N9 . 140.94(9) yes O2 . Gd1 . N9 . 92.21(9) yes O4 . Gd1 . N9 . 25.91(10) yes O5 . Gd1 . N9 . 25.55(9) yes N1 . Gd1 . N9 . 112.46(10) yes N3 . Gd1 . N4 . 64.53(9) yes N3 . Gd1 . N6 . 74.05(9) yes N4 . Gd1 . N6 . 81.58(10) yes N3 . Gd1 . N7 . 121.21(9) yes N4 . Gd1 . N7 . 139.42(10) yes N6 . Gd1 . N7 . 138.76(10) yes N3 . Gd1 . N8 . 90.82(9) yes N4 . Gd1 . N8 . 73.57(9) yes N6 . Gd1 . N8 . 154.72(10) yes N7 . Gd1 . N8 . 66.44(10) yes N3 . Gd1 . N9 . 149.63(8) yes N4 . Gd1 . N9 . 107.89(10) yes N6 . Gd1 . N9 . 75.75(10) yes N7 . Gd1 . N9 . 84.42(10) yes N8 . Gd1 . N9 . 116.05(9) yes Gd1 . O1 . N8 . 95.79(17) yes Gd1 . O2 . N8 . 96.52(17) yes Gd1 . O4 . N9 . 97.3(2) yes Gd1 . O5 . N9 . 95.3(2) yes Gd1 . N1 . C1 . 134.8(2) yes Gd1 . N1 . C7 . 119.4(2) yes C1 . N1 . C7 . 105.5(3) yes C6 . N2 . C7 . 107.9(3) yes C6 . N2 . H22 . 126.2 no C7 . N2 . H22 . 125.9 no Gd1 . N3 . C8 . 120.4(2) yes Gd1 . N3 . C12 . 120.6(2) yes C8 . N3 . C12 . 118.7(3) yes Gd1 . N4 . C13 . 118.3(2) yes Gd1 . N4 . C19 . 135.6(2) yes C13 . N4 . C19 . 104.3(3) yes C13 . N5 . C14 . 106.7(3) yes C13 . N5 . H52 . 126.5 no C14 . N5 . H52 . 126.8 no Gd1 . N6 . C20 . 171.7(3) yes Gd1 . N7 . C21 . 163.4(3) yes O1 . N8 . Gd1 . 58.04(14) yes O1 . N8 . O2 . 116.1(2) yes Gd1 . N8 . O2 . 58.22(15) yes O1 . N8 . O3 . 121.4(3) yes Gd1 . N8 . O3 . 175.6(3) yes O2 . N8 . O3 . 122.5(3) yes Gd1 . N9 . O4 . 56.79(16) yes Gd1 . N9 . O5 . 59.18(17) yes O4 . N9 . O5 . 116.0(3) yes Gd1 . N9 . O6 . 177.2(3) yes O4 . N9 . O6 . 121.2(4) yes O5 . N9 . O6 . 122.9(4) yes N1 . C1 . C2 . 130.8(3) yes N1 . C1 . C6 . 109.1(3) yes C2 . C1 . C6 . 120.1(3) yes C1 . C2 . C3 . 117.5(3) yes C1 . C2 . H21 . 120.6 no C3 . C2 . H21 . 121.9 no C2 . C3 . C4 . 121.6(4) yes C2 . C3 . H31 . 119.0 no C4 . C3 . H31 . 119.3 no C3 . C4 . C5 . 121.7(4) yes C3 . C4 . H41 . 119.7 no C5 . C4 . H41 . 118.5 no C4 . C5 . C6 . 116.4(4) yes C4 . C5 . H51 . 122.2 no C6 . C5 . H51 . 121.4 no C1 . C6 . C5 . 122.6(3) yes C1 . C6 . N2 . 105.7(3) yes C5 . C6 . N2 . 131.7(3) yes N2 . C7 . N1 . 111.9(3) yes N2 . C7 . C8 . 126.7(3) yes N1 . C7 . C8 . 121.4(3) yes C7 . C8 . N3 . 113.8(3) yes C7 . C8 . C9 . 124.2(3) yes N3 . C8 . C9 . 121.9(3) yes C8 . C9 . C10 . 118.8(3) yes C8 . C9 . H91 . 119.7 no C10 . C9 . H91 . 121.4 no C9 . C10 . C11 . 119.7(3) yes C9 . C10 . H101 . 120.2 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 118.1(4) yes C10 . C11 . H111 . 121.4 no C12 . C11 . H111 . 120.5 no C11 . C12 . N3 . 122.7(3) yes C11 . C12 . C13 . 123.3(3) yes N3 . C12 . C13 . 114.0(3) yes C12 . C13 . N5 . 125.3(3) yes C12 . C13 . N4 . 121.4(3) yes N5 . C13 . N4 . 113.3(3) yes N5 . C14 . C15 . 131.3(3) yes N5 . C14 . C19 . 106.1(3) yes C15 . C14 . C19 . 122.6(3) yes C14 . C15 . C16 . 116.3(4) yes C14 . C15 . H151 . 122.1 no C16 . C15 . H151 . 121.6 no C15 . C16 . C17 . 121.8(4) yes C15 . C16 . H161 . 119.1 no C17 . C16 . H161 . 119.2 no C16 . C17 . C18 . 121.8(4) yes C16 . C17 . H171 . 118.6 no C18 . C17 . H171 . 119.6 no C17 . C18 . C19 . 117.3(4) yes C17 . C18 . H181 . 121.4 no C19 . C18 . H181 . 121.3 no C18 . C19 . N4 . 130.1(3) yes C18 . C19 . C14 . 120.2(3) yes N4 . C19 . C14 . 109.7(3) yes Au1 1_545 C20 . N6 . 172.9(4) yes Au1 . C21 . N7 . 176.0(3) yes C23 . C22 . H221 . 108.4 no C23 . C22 . H222 . 107.6 no H221 . C22 . H222 . 111.1 no C23 . C22 . H223 . 107.9 no H221 . C22 . H223 . 111.0 no H222 . C22 . H223 . 110.7 no C22 . C23 . N10 . 178.5(6) yes _database_code_depnum_ccdc_archive 'CCDC 952848' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_JT2-9b #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C48 H32 Au3 Eu N18' _chemical_formula_moiety 'C48 H32 Au3 Eu N18' _chemical_formula_weight 1603.77 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' #------------------------------------------------ _cell_length_a 15.3869(3) _cell_length_b 17.6799(3) _cell_length_c 18.9791(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5163.05(17) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9922 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 25.89 _cell_measurement_temperature 296(2) _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_min 0.032 _exptl_crystal_size_mid 0.057 _exptl_crystal_size_max 0.192 _exptl_crystal_density_diffrn 2.063 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 9.748 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(Sheldrich , 1996)' _exptl_absorpt_correction_T_min 0.4977 _exptl_absorpt_correction_T_max 0.7454 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\f and \w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 59086 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_theta_min 1.574 _diffrn_reflns_theta_max 26.371 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 10550 _reflns_number_gt 8896 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.815 _reflns_Friedel_fraction_max 0.998 _reflns_Friedel_fraction_full 0.999 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0255P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 3519 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.005(4) _refine_ls_number_reflns 10550 _refine_ls_number_parameters 633 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.902 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.529 _refine_diff_density_min -0.941 #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # TODO check _oxford_atom_site_special_shape 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.2792(4) 0.7018(4) 0.1051(4) 0.0344(17) Uani 1 1 d . . . . . C1 C 0.3431(6) 0.6487(6) 0.0889(5) 0.041(2) Uani 1 1 d . . . . . Eu1 Eu 0.27296(3) 0.83971(2) 0.14845(2) 0.02621(10) Uani 1 1 d . . . . . Au1 Au 0.62106(2) 0.86607(2) 0.11122(2) 0.04281(11) Uani 1 1 d . . . . . N2 N 0.2163(5) 0.5985(5) 0.0607(4) 0.048(2) Uani 1 1 d . . . . . H22 H 0.1763 0.5681 0.0465 0.058 Uiso 1 1 calc R U . . . C2 C 0.4339(6) 0.6512(6) 0.0953(6) 0.052(3) Uani 1 1 d . . . . . H2 H 0.4624 0.6930 0.1141 0.062 Uiso 1 1 calc R U . . . Au2 Au 0.18030(3) 0.80319(2) -0.13523(2) 0.04374(11) Uani 1 1 d . . . . . N3 N 0.1252(4) 0.7796(4) 0.1153(4) 0.0314(17) Uani 1 1 d . . . . . Au3 Au 0.10471(3) 0.73875(3) 0.39301(2) 0.06358(15) Uani 1 1 d . . . . . C3 C 0.4783(8) 0.5888(7) 0.0724(7) 0.063(3) Uani 1 1 d . . . . . H3 H 0.5385 0.5887 0.0773 0.076 Uiso 1 1 calc R U . . . N4 N 0.1370(4) 0.9251(4) 0.1639(4) 0.0340(18) Uani 1 1 d . . . . . C4 C 0.4398(8) 0.5260(7) 0.0424(6) 0.063(3) Uani 1 1 d . . . . . H4 H 0.4740 0.4863 0.0260 0.076 Uiso 1 1 calc R U . . . C41 C 0.2253(6) 0.8229(6) -0.0393(5) 0.042(2) Uani 1 1 d . . . . . C9 C 0.0441(6) 0.6743(6) 0.0716(6) 0.047(3) Uani 1 1 d . . . . . H9 H 0.0432 0.6240 0.0573 0.057 Uiso 1 1 calc R U . . . N9 N 0.3031(4) 0.9766(4) 0.1065(4) 0.0320(17) Uani 1 1 d . . . . . C8 C 0.1214(6) 0.7086(5) 0.0916(4) 0.035(2) Uani 1 1 d . . . . . N8 N 0.3880(4) 0.9183(4) 0.2205(4) 0.0307(17) Uani 1 1 d . . . . . C7 C 0.2047(6) 0.6696(5) 0.0873(5) 0.035(2) Uani 1 1 d . . . . . N7 N 0.4299(5) 0.7726(4) 0.3477(4) 0.0363(18) Uani 1 1 d . . . . . H7 H 0.4624 0.7904 0.3807 0.044 Uiso 1 1 calc R U . . . C6 C 0.3042(7) 0.5849(6) 0.0609(6) 0.050(3) Uani 1 1 d . . . . . N6 N 0.3584(4) 0.7670(4) 0.2461(4) 0.0327(18) Uani 1 1 d . . . . . N5 N -0.0061(5) 0.9436(5) 0.1562(5) 0.047(2) Uani 1 1 d . . . . . H5 H -0.0599 0.9353 0.1466 0.056 Uiso 1 1 calc R U . . . C5 C 0.3506(8) 0.5222(7) 0.0369(7) 0.064(3) Uani 1 1 d . . . . . H5A H 0.3228 0.4801 0.0181 0.077 Uiso 1 1 calc R U . . . C39 C 0.4954(6) 0.8456(6) 0.0995(5) 0.038(2) Uani 1 1 d . . . . . C12 C 0.0511(5) 0.8195(5) 0.1178(5) 0.032(2) Uani 1 1 d . . . . . N12 N 0.8154(6) 0.9103(5) 0.1353(6) 0.075(3) Uani 1 1 d . . . . . C11 C -0.0278(6) 0.7902(6) 0.0958(6) 0.048(3) Uani 1 1 d . . . . . H11 H -0.0775 0.8201 0.0963 0.058 Uiso 1 1 calc R U . . . N11 N 0.4229(5) 0.8350(5) 0.0966(4) 0.0395(19) Uani 1 1 d . . . . . C10 C -0.0316(7) 0.7164(7) 0.0733(6) 0.057(3) Uani 1 1 d . . . . . H10 H -0.0842 0.6951 0.0594 0.068 Uiso 1 1 calc R U . . . N10 N 0.3622(5) 1.0906(4) 0.1197(4) 0.044(2) Uani 1 1 d . . . . . H10A H 0.3960 1.1255 0.1353 0.052 Uiso 1 1 calc R U . . . C14 C 0.0281(6) 1.0085(6) 0.1865(6) 0.045(3) Uani 1 1 d . . . . . N14 N 0.1060(7) 0.7841(6) -0.2867(5) 0.074(3) Uani 1 1 d . . . . . C13 C 0.0605(5) 0.8961(5) 0.1446(5) 0.034(2) Uani 1 1 d . . . . . N13 N 0.2483(5) 0.8373(5) 0.0168(4) 0.040(2) Uani 1 1 d . . . . . C16 C 0.0400(7) 1.1281(7) 0.2390(7) 0.064(3) Uani 1 1 d . . . . . H16 H 0.0161 1.1734 0.2546 0.076 Uiso 1 1 calc R U . . . N16 N 0.1869(6) 0.8092(5) 0.2578(4) 0.055(2) Uani 1 1 d . . . . . C15 C -0.0128(7) 1.0742(7) 0.2098(7) 0.060(3) Uani 1 1 d . . . . . H15 H -0.0725 1.0810 0.2057 0.073 Uiso 1 1 calc R U . . . N15 N 0.0352(8) 0.6789(6) 0.5362(5) 0.080(4) Uani 1 1 d . . . . . C42 C 0.1332(7) 0.7898(6) -0.2304(6) 0.052(3) Uani 1 1 d . . . . . C19 C 0.1167(6) 0.9966(5) 0.1911(5) 0.035(2) Uani 1 1 d . . . . . C25 C 0.3899(6) 0.7038(5) 0.3480(5) 0.036(2) Uani 1 1 d . . . . . C24 C 0.3865(7) 0.6474(6) 0.3985(5) 0.051(3) Uani 1 1 d . . . . . H24 H 0.4177 0.6508 0.4403 0.061 Uiso 1 1 calc R U . . . C23 C 0.3352(8) 0.5865(6) 0.3839(6) 0.060(3) Uani 1 1 d . . . . . H23 H 0.3298 0.5478 0.4168 0.072 Uiso 1 1 calc R U . . . C22 C 0.2912(8) 0.5817(6) 0.3210(7) 0.059(3) Uani 1 1 d . . . . . H222 H 0.2585 0.5383 0.3125 0.071 Uiso 1 1 calc R U . . . C21 C 0.2923(7) 0.6366(6) 0.2700(6) 0.048(3) Uani 1 1 d . . . . . H21 H 0.2606 0.6321 0.2286 0.058 Uiso 1 1 calc R U . . . C20 C 0.3442(6) 0.7002(5) 0.2840(5) 0.035(2) Uani 1 1 d . . . . . C26 C 0.4100(5) 0.8079(5) 0.2872(4) 0.031(2) Uani 1 1 d . . . . . C31 C 0.4132(6) 0.9873(5) 0.1982(5) 0.032(2) Uani 1 1 d . . . . . C27 C 0.4378(5) 0.8842(5) 0.2693(4) 0.031(2) Uani 1 1 d . . . . . C32 C 0.3604(5) 1.0180(5) 0.1415(5) 0.0287(19) Uani 1 1 d . . . . . C28 C 0.5123(7) 0.9164(6) 0.2983(5) 0.045(3) Uani 1 1 d . . . . . H28 H 0.5452 0.8907 0.3318 0.054 Uiso 1 1 calc R U . . . C33 C 0.3006(6) 1.0987(6) 0.0681(5) 0.041(2) Uani 1 1 d . . . . . C30 C 0.4867(6) 1.0238(6) 0.2244(5) 0.043(3) Uani 1 1 d . . . . . H30 H 0.5027 1.0714 0.2081 0.051 Uiso 1 1 calc R U . . . C29 C 0.5353(7) 0.9869(6) 0.2759(6) 0.051(3) Uani 1 1 d . . . . . H29 H 0.5839 1.0105 0.2951 0.061 Uiso 1 1 calc R U . . . C38 C 0.2628(6) 1.0273(5) 0.0599(5) 0.039(2) Uani 1 1 d . . . . . C35 C 0.2109(9) 1.1497(7) -0.0182(7) 0.080(4) Uani 1 1 d . . . . . H35 H 0.1929 1.1898 -0.0463 0.096 Uiso 1 1 calc R U . . . C34 C 0.2748(8) 1.1616(6) 0.0294(6) 0.062(3) Uani 1 1 d . . . . . H34 H 0.2999 1.2089 0.0359 0.074 Uiso 1 1 calc R U . . . C18 C 0.1683(6) 1.0521(6) 0.2229(6) 0.047(3) Uani 1 1 d . . . . . H18 H 0.2279 1.0455 0.2283 0.057 Uiso 1 1 calc R U . . . C17 C 0.1283(8) 1.1160(6) 0.2455(6) 0.057(3) Uani 1 1 d . . . . . H17 H 0.1619 1.1535 0.2665 0.069 Uiso 1 1 calc R U . . . N17 N 0.0584(14) 0.4840(10) 0.0362(11) 0.162(9) Uani 1 1 d . . . . . C47 C 0.858(4) 0.823(3) 0.322(4) 0.42(3) Uani 1 1 d D U . . . H47A H 0.8437 0.7986 0.2781 0.627 Uiso 1 1 calc R U . . . H47B H 0.8795 0.7865 0.3546 0.627 Uiso 1 1 calc R U . . . H47C H 0.9014 0.8610 0.3135 0.627 Uiso 1 1 calc R U . . . C48 C 0.788(5) 0.855(4) 0.348(5) 0.42(3) Uani 1 1 d D U . . . C43 C 0.0587(9) 0.6971(7) 0.4824(6) 0.067(3) Uani 1 1 d . . . . . C44 C 0.1543(7) 0.7842(7) 0.3065(6) 0.061(3) Uani 1 1 d . . . . . C40 C 0.7458(6) 0.8920(6) 0.1261(6) 0.052(3) Uani 1 1 d . . . . . C36 C 0.1712(9) 1.0795(8) -0.0268(7) 0.076(4) Uani 1 1 d . . . . . H36 H 0.1254 1.0749 -0.0584 0.091 Uiso 1 1 calc R U . . . C37 C 0.1980(7) 1.0166(6) 0.0105(6) 0.051(3) Uani 1 1 d . . . . . H37 H 0.1736 0.9692 0.0027 0.062 Uiso 1 1 calc R U . . . C45 C -0.0827(11) 0.4515(14) 0.1079(9) 0.191(13) Uani 1 1 d . . . . . H45A H -0.1340 0.4576 0.0797 0.287 Uiso 1 1 calc R U . . . H45B H -0.0867 0.4832 0.1489 0.287 Uiso 1 1 calc R U . . . H45C H -0.0776 0.3996 0.1223 0.287 Uiso 1 1 calc R U . . . C46 C -0.0061(15) 0.4730(10) 0.0665(10) 0.110(6) Uani 1 1 d . . . . . N18 N 0.813(3) 0.948(2) 0.3235(19) 0.333(18) Uani 1 1 d D U . . . 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 N1 0.027(4) 0.034(4) 0.042(4) -0.002(4) -0.003(4) 0.003(4) C1 0.041(6) 0.040(6) 0.042(6) 0.000(5) -0.003(4) 0.000(5) Eu1 0.0187(2) 0.0327(2) 0.0272(2) 0.00224(19) -0.00148(17) -0.00367(18) Au1 0.02147(17) 0.0441(2) 0.0628(3) -0.0040(2) 0.00030(17) -0.00115(17) N2 0.033(5) 0.047(6) 0.064(6) -0.016(5) -0.005(4) -0.006(4) C2 0.038(6) 0.041(7) 0.076(8) -0.001(6) -0.004(5) -0.001(5) Au2 0.0452(2) 0.0532(2) 0.0328(2) 0.00168(19) -0.00545(17) -0.00633(19) N3 0.025(4) 0.036(4) 0.033(4) -0.001(3) -0.001(3) 0.000(3) Au3 0.0697(3) 0.0825(4) 0.0385(2) 0.0063(2) 0.0196(2) -0.0130(3) C3 0.041(7) 0.050(8) 0.099(10) -0.006(7) -0.006(6) 0.016(6) N4 0.024(4) 0.037(5) 0.042(5) -0.002(4) 0.000(3) -0.009(3) C4 0.059(8) 0.060(9) 0.070(8) 0.001(7) 0.006(6) 0.024(7) C41 0.035(5) 0.047(7) 0.043(6) 0.007(5) 0.003(5) 0.000(5) C9 0.040(6) 0.043(7) 0.059(7) -0.020(5) -0.002(5) -0.010(5) N9 0.026(4) 0.036(4) 0.034(4) 0.009(4) -0.006(3) -0.003(3) C8 0.031(5) 0.041(6) 0.033(5) -0.003(4) -0.002(4) -0.002(5) N8 0.026(4) 0.040(5) 0.026(4) 0.007(3) 0.000(3) -0.006(4) C7 0.034(5) 0.034(6) 0.036(5) -0.006(4) -0.002(4) -0.004(4) N7 0.037(4) 0.044(5) 0.028(4) 0.009(4) -0.001(3) 0.005(4) C6 0.049(7) 0.045(7) 0.056(7) -0.011(5) -0.002(5) 0.006(5) N6 0.030(4) 0.033(4) 0.035(4) 0.009(4) -0.003(3) 0.002(3) N5 0.015(4) 0.052(5) 0.074(6) -0.015(5) -0.010(4) 0.000(4) C5 0.062(8) 0.050(7) 0.080(9) -0.023(7) -0.002(6) 0.010(6) C39 0.034(5) 0.043(6) 0.036(5) 0.007(5) 0.003(4) 0.000(4) C12 0.021(4) 0.042(6) 0.035(5) -0.003(4) 0.000(4) -0.003(4) N12 0.024(5) 0.073(7) 0.130(10) -0.023(7) -0.006(6) 0.001(5) C11 0.023(5) 0.059(7) 0.062(7) -0.008(6) -0.003(5) -0.002(5) N11 0.024(4) 0.050(5) 0.044(5) -0.004(4) 0.004(3) -0.006(4) C10 0.030(6) 0.067(9) 0.073(8) -0.021(7) -0.004(5) -0.006(5) N10 0.046(5) 0.038(5) 0.047(5) 0.013(4) -0.010(4) -0.011(4) C14 0.029(5) 0.050(7) 0.056(7) -0.004(5) -0.010(5) 0.004(5) N14 0.094(8) 0.084(8) 0.043(6) 0.012(5) -0.015(6) -0.038(7) C13 0.021(4) 0.036(5) 0.045(6) 0.002(5) -0.003(4) 0.001(4) N13 0.037(5) 0.051(5) 0.033(4) -0.003(4) 0.000(3) -0.006(4) C16 0.046(7) 0.042(7) 0.103(10) -0.027(7) 0.001(6) 0.012(6) N16 0.043(5) 0.079(7) 0.043(5) 0.022(5) 0.012(4) 0.009(5) C15 0.040(6) 0.047(7) 0.094(10) -0.013(7) 0.003(6) 0.011(6) N15 0.118(10) 0.072(8) 0.049(6) 0.001(5) 0.032(6) -0.021(7) C42 0.068(8) 0.040(6) 0.046(6) 0.010(5) -0.008(6) -0.020(6) C19 0.030(5) 0.036(6) 0.039(5) 0.005(4) 0.004(4) -0.001(4) C25 0.040(5) 0.034(5) 0.034(5) 0.008(4) 0.001(4) 0.006(5) C24 0.069(7) 0.042(7) 0.041(6) 0.007(5) 0.004(6) 0.007(6) C23 0.085(9) 0.039(7) 0.056(7) 0.019(6) 0.006(7) 0.013(6) C22 0.066(8) 0.033(6) 0.078(9) 0.019(6) 0.011(7) -0.003(6) C21 0.047(6) 0.044(6) 0.054(6) 0.005(5) -0.004(5) -0.005(5) C20 0.038(5) 0.027(5) 0.041(5) 0.008(4) 0.004(4) 0.000(4) C26 0.028(5) 0.036(5) 0.029(4) -0.001(4) -0.004(4) 0.006(4) C31 0.026(5) 0.037(6) 0.034(5) 0.002(4) 0.000(4) -0.006(4) C27 0.025(5) 0.038(6) 0.029(5) 0.002(4) 0.002(4) 0.002(4) C32 0.026(4) 0.028(5) 0.032(5) -0.002(4) 0.002(4) -0.012(4) C28 0.046(6) 0.050(7) 0.039(6) 0.011(5) -0.013(5) -0.014(5) C33 0.036(6) 0.041(6) 0.048(6) 0.010(5) -0.002(4) -0.003(5) C30 0.039(6) 0.040(6) 0.050(6) 0.008(5) -0.005(5) -0.010(5) C29 0.048(7) 0.053(7) 0.052(7) 0.003(6) -0.022(5) -0.019(6) C38 0.035(5) 0.036(6) 0.045(6) 0.012(5) -0.002(5) -0.004(5) C35 0.095(10) 0.050(8) 0.095(10) 0.043(7) -0.032(8) -0.011(8) C34 0.065(8) 0.040(6) 0.080(8) 0.029(6) -0.021(7) -0.011(6) C18 0.027(5) 0.040(6) 0.076(8) -0.016(6) -0.004(5) -0.007(5) C17 0.056(7) 0.039(6) 0.077(8) -0.015(6) 0.005(6) -0.017(6) N17 0.20(2) 0.095(12) 0.19(2) -0.055(12) 0.084(16) -0.043(13) C47 0.45(8) 0.34(4) 0.46(8) -0.07(6) -0.15(6) 0.10(5) C48 0.48(8) 0.33(5) 0.44(7) -0.04(5) -0.01(7) 0.02(6) C43 0.086(9) 0.067(8) 0.049(7) 0.002(7) 0.016(6) -0.020(7) C44 0.055(7) 0.086(10) 0.043(6) 0.009(6) 0.014(5) 0.006(6) C40 0.035(6) 0.038(6) 0.085(9) -0.006(6) -0.005(5) 0.004(5) C36 0.069(9) 0.075(9) 0.083(9) 0.032(8) -0.036(7) -0.003(7) C37 0.045(6) 0.050(7) 0.060(7) 0.011(6) -0.017(5) -0.003(5) C45 0.108(13) 0.36(3) 0.104(14) -0.108(18) 0.052(12) -0.148(18) C46 0.151(19) 0.066(11) 0.114(15) -0.017(10) 0.027(13) -0.012(12) N18 0.41(5) 0.34(4) 0.24(3) 0.00(3) -0.03(3) 0.07(4) 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 N1 C7 1.322(11) . ? N1 C1 1.394(12) . ? N1 Eu1 2.575(7) . ? C1 C6 1.381(14) . ? C1 C2 1.404(13) . ? Eu1 N11 2.509(7) . ? Eu1 N16 2.520(8) . ? Eu1 N13 2.527(8) . ? Eu1 N3 2.588(7) . ? Eu1 N9 2.590(7) . ? Eu1 N4 2.596(7) . ? Eu1 N6 2.611(7) . ? Eu1 N8 2.632(7) . ? Au1 C39 1.980(9) . ? Au1 C40 1.993(10) . ? Au1 Au2 3.1611(6) 4_565 ? N2 C7 1.367(11) . ? N2 C6 1.374(13) . ? C2 C3 1.368(14) . ? Au2 C42 1.961(11) . ? Au2 C41 1.979(10) . ? Au2 Au1 3.1611(6) 4_465 ? N3 C8 1.335(11) . ? N3 C12 1.341(10) . ? Au3 C43 1.980(12) . ? Au3 C44 1.982(11) . ? C3 C4 1.381(16) . ? N4 C13 1.335(10) . ? N4 C19 1.400(11) . ? C4 C5 1.379(16) . ? C41 N13 1.150(12) . ? C9 C10 1.382(14) . ? C9 C8 1.389(13) . ? N9 C32 1.324(10) . ? N9 C38 1.404(11) . ? C8 C7 1.458(12) . ? N8 C27 1.344(10) . ? N8 C31 1.349(11) . ? N7 C26 1.342(11) . ? N7 C25 1.364(11) . ? C6 C5 1.396(15) . ? N6 C26 1.327(11) . ? N6 C20 1.400(11) . ? N5 C13 1.343(11) . ? N5 C14 1.387(12) . ? C39 N11 1.133(11) . ? C12 C11 1.384(12) . ? C12 C13 1.455(12) . ? N12 C40 1.133(12) . ? C11 C10 1.375(14) . ? N10 C32 1.349(10) . ? N10 C33 1.371(11) . ? C14 C19 1.383(13) . ? C14 C15 1.393(14) . ? N14 C42 1.151(13) . ? C16 C15 1.370(15) . ? C16 C17 1.381(15) . ? N16 C44 1.140(12) . ? N15 C43 1.131(13) . ? C19 C18 1.399(13) . ? C25 C24 1.385(13) . ? C25 C20 1.404(12) . ? C24 C23 1.363(15) . ? C23 C22 1.375(16) . ? C22 C21 1.372(14) . ? C21 C20 1.404(13) . ? C26 C27 1.456(13) . ? C31 C30 1.393(13) . ? C31 C32 1.454(12) . ? C27 C28 1.394(12) . ? C28 C29 1.364(14) . ? C33 C34 1.391(13) . ? C33 C38 1.397(13) . ? C30 C29 1.393(13) . ? C38 C37 1.382(13) . ? C35 C34 1.351(16) . ? C35 C36 1.392(17) . ? C18 C17 1.356(14) . ? N17 C46 1.16(2) . ? C47 C48 1.31(7) . ? C48 N18 1.74(7) . ? C36 C37 1.382(15) . ? C45 C46 1.47(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 N1 C1 105.3(7) . . ? C7 N1 Eu1 117.2(6) . . ? C1 N1 Eu1 137.3(6) . . ? C6 C1 N1 109.2(9) . . ? C6 C1 C2 119.3(10) . . ? N1 C1 C2 131.4(9) . . ? N11 Eu1 N16 143.0(3) . . ? N11 Eu1 N13 75.5(2) . . ? N16 Eu1 N13 137.0(3) . . ? N11 Eu1 N1 79.0(2) . . ? N16 Eu1 N1 94.6(3) . . ? N13 Eu1 N1 71.0(2) . . ? N11 Eu1 N3 134.3(2) . . ? N16 Eu1 N3 69.5(3) . . ? N13 Eu1 N3 67.7(2) . . ? N1 Eu1 N3 64.3(2) . . ? N11 Eu1 N9 75.3(2) . . ? N16 Eu1 N9 123.2(3) . . ? N13 Eu1 N9 74.9(2) . . ? N1 Eu1 N9 141.3(2) . . ? N3 Eu1 N9 117.8(2) . . ? N11 Eu1 N4 143.5(2) . . ? N16 Eu1 N4 66.9(3) . . ? N13 Eu1 N4 90.1(2) . . ? N1 Eu1 N4 128.1(2) . . ? N3 Eu1 N4 63.8(2) . . ? N9 Eu1 N4 68.6(2) . . ? N11 Eu1 N6 78.4(2) . . ? N16 Eu1 N6 64.8(2) . . ? N13 Eu1 N6 140.3(2) . . ? N1 Eu1 N6 75.0(2) . . ? N3 Eu1 N6 114.4(2) . . ? N9 Eu1 N6 126.0(2) . . ? N4 Eu1 N6 127.7(2) . . ? N11 Eu1 N8 66.6(2) . . ? N16 Eu1 N8 92.2(3) . . ? N13 Eu1 N8 128.5(2) . . ? N1 Eu1 N8 129.8(2) . . ? N3 Eu1 N8 159.0(2) . . ? N9 Eu1 N8 63.0(2) . . ? N4 Eu1 N8 100.1(2) . . ? N6 Eu1 N8 63.4(2) . . ? C39 Au1 C40 176.7(4) . . ? C39 Au1 Au2 97.2(3) . 4_565 ? C40 Au1 Au2 85.4(3) . 4_565 ? C7 N2 C6 106.7(8) . . ? C3 C2 C1 116.4(10) . . ? C42 Au2 C41 176.6(4) . . ? C42 Au2 Au1 85.0(3) . 4_465 ? C41 Au2 Au1 97.7(3) . 4_465 ? C8 N3 C12 118.0(7) . . ? C8 N3 Eu1 120.4(6) . . ? C12 N3 Eu1 121.5(5) . . ? C43 Au3 C44 177.0(5) . . ? C2 C3 C4 124.4(11) . . ? C13 N4 C19 104.6(7) . . ? C13 N4 Eu1 117.1(6) . . ? C19 N4 Eu1 138.3(6) . . ? C5 C4 C3 119.8(11) . . ? N13 C41 Au2 176.5(9) . . ? C10 C9 C8 118.7(9) . . ? C32 N9 C38 104.9(7) . . ? C32 N9 Eu1 118.8(5) . . ? C38 N9 Eu1 135.4(6) . . ? N3 C8 C9 122.7(9) . . ? N3 C8 C7 115.2(8) . . ? C9 C8 C7 122.1(8) . . ? C27 N8 C31 117.2(7) . . ? C27 N8 Eu1 120.3(6) . . ? C31 N8 Eu1 120.6(5) . . ? N1 C7 N2 112.2(8) . . ? N1 C7 C8 122.9(8) . . ? N2 C7 C8 124.7(8) . . ? C26 N7 C25 108.4(8) . . ? N2 C6 C1 106.6(9) . . ? N2 C6 C5 129.9(10) . . ? C1 C6 C5 123.6(10) . . ? C26 N6 C20 104.5(7) . . ? C26 N6 Eu1 116.8(5) . . ? C20 N6 Eu1 134.6(6) . . ? C13 N5 C14 107.2(7) . . ? C4 C5 C6 116.5(11) . . ? N11 C39 Au1 176.1(9) . . ? N3 C12 C11 122.6(9) . . ? N3 C12 C13 114.7(7) . . ? C11 C12 C13 122.8(8) . . ? C10 C11 C12 119.1(9) . . ? C39 N11 Eu1 151.8(8) . . ? C11 C10 C9 118.9(10) . . ? C32 N10 C33 107.7(8) . . ? C19 C14 N5 105.9(9) . . ? C19 C14 C15 123.5(10) . . ? N5 C14 C15 130.5(9) . . ? N4 C13 N5 112.8(8) . . ? N4 C13 C12 122.8(8) . . ? N5 C13 C12 124.3(8) . . ? C41 N13 Eu1 164.7(8) . . ? C15 C16 C17 120.8(10) . . ? C44 N16 Eu1 168.8(9) . . ? C16 C15 C14 116.2(10) . . ? N14 C42 Au2 178.1(10) . . ? C14 C19 N4 109.5(8) . . ? C14 C19 C18 118.7(9) . . ? N4 C19 C18 131.7(9) . . ? N7 C25 C24 131.5(9) . . ? N7 C25 C20 105.2(7) . . ? C24 C25 C20 123.2(9) . . ? C23 C24 C25 116.7(10) . . ? C24 C23 C22 120.7(10) . . ? C21 C22 C23 124.2(11) . . ? C22 C21 C20 116.2(10) . . ? N6 C20 C21 131.8(9) . . ? N6 C20 C25 109.1(8) . . ? C21 C20 C25 119.0(9) . . ? N6 C26 N7 112.7(8) . . ? N6 C26 C27 122.9(8) . . ? N7 C26 C27 124.3(8) . . ? N8 C31 C30 122.7(8) . . ? N8 C31 C32 114.1(7) . . ? C30 C31 C32 123.0(8) . . ? N8 C27 C28 124.0(8) . . ? N8 C27 C26 114.1(7) . . ? C28 C27 C26 121.8(8) . . ? N9 C32 N10 112.7(8) . . ? N9 C32 C31 122.5(8) . . ? N10 C32 C31 124.8(8) . . ? C29 C28 C27 117.6(9) . . ? N10 C33 C34 131.1(10) . . ? N10 C33 C38 105.9(8) . . ? C34 C33 C38 123.0(9) . . ? C31 C30 C29 118.0(9) . . ? C28 C29 C30 120.5(9) . . ? C37 C38 C33 120.0(9) . . ? C37 C38 N9 131.2(9) . . ? C33 C38 N9 108.9(8) . . ? C34 C35 C36 122.4(11) . . ? C35 C34 C33 115.8(10) . . ? C17 C18 C19 117.6(9) . . ? C18 C17 C16 123.2(10) . . ? C47 C48 N18 97(7) . . ? N15 C43 Au3 174.0(12) . . ? N16 C44 Au3 176.6(11) . . ? N12 C40 Au1 176.6(10) . . ? C37 C36 C35 121.8(11) . . ? C38 C37 C36 116.9(10) . . ? N17 C46 C45 174(3) . . ? _database_code_depnum_ccdc_archive 'CCDC 952849' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_JT2-13f #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C48 H32 Au3 Gd N18' _chemical_formula_moiety 'C48 H32 Au3 Gd N18' _chemical_formula_weight 1606.05 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' #------------------------------------------------ _cell_length_a 15.366(2) _cell_length_b 17.645(2) _cell_length_c 18.959(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5140.8(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9945 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.55 _cell_measurement_temperature 296(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.040 _exptl_crystal_size_mid 0.086 _exptl_crystal_size_max 0.124 _exptl_crystal_density_diffrn 2.075 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 9.860 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details '(Sheldrich , 1996)' _exptl_absorpt_correction_T_min 0.4998 _exptl_absorpt_correction_T_max 0.7457 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\f and \w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 55294 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_theta_min 1.706 _diffrn_reflns_theta_max 28.282 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 12746 _reflns_number_gt 11013 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.825 _reflns_Friedel_fraction_max 0.998 _reflns_Friedel_fraction_full 0.997 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0132P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 3519 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.006(3) _refine_ls_number_reflns 12746 _refine_ls_number_parameters 632 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0531 _refine_ls_wR_factor_gt 0.0510 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.994 _refine_diff_density_min -1.042 #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) SHELXL-2013 (Sheldrick, 2013) ; #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom # TODO check _oxford_atom_site_special_shape 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.10468(3) 0.76105(2) 0.10718(2) 0.06186(11) Uani 1 1 d . . . . . C1 C 0.3438(5) 0.8003(4) 0.2166(4) 0.0364(16) Uani 1 1 d . . . . . N1 N 0.3582(4) 0.7336(3) 0.2543(3) 0.0325(13) Uani 1 1 d . . . . . Gd1 Gd 0.27291(2) 0.66062(2) 0.35168(2) 0.02462(7) Uani 1 1 d . . . . . Au2 Au 0.18054(2) 0.69677(2) 0.63517(2) 0.04194(8) Uani 1 1 d . . . . . N2 N 0.4298(4) 0.7277(3) 0.1522(3) 0.0355(13) Uani 1 1 d . . . . . H2 H 0.4624 0.7101 0.1192 0.043 Uiso 1 1 calc R U . . . C2 C 0.2928(5) 0.8633(4) 0.2312(4) 0.0470(19) Uani 1 1 d . . . . . H2A H 0.2624 0.8678 0.2735 0.056 Uiso 1 1 calc R U . . . Au3 Au 0.62082(2) 0.63422(2) 0.38902(2) 0.04141(8) Uani 1 1 d . . . . . N3 N 0.3880(4) 0.5823(3) 0.2794(3) 0.0269(11) Uani 1 1 d . . . . . C3 C 0.2892(6) 0.9192(4) 0.1800(5) 0.059(2) Uani 1 1 d . . . . . H3 H 0.2550 0.9617 0.1883 0.071 Uiso 1 1 calc R U . . . C4 C 0.3337(7) 0.9144(5) 0.1179(5) 0.062(3) Uani 1 1 d . . . . . H4 H 0.3290 0.9536 0.0853 0.074 Uiso 1 1 calc R U . . . N4 N 0.3027(3) 0.5242(3) 0.3934(3) 0.0323(12) Uani 1 1 d . . . . . C5 C 0.3854(6) 0.8529(4) 0.1023(4) 0.0483(19) Uani 1 1 d . . . . . H5 H 0.4162 0.8495 0.0602 0.058 Uiso 1 1 calc R U . . . N5 N 0.3616(4) 0.4104(3) 0.3807(3) 0.0404(15) Uani 1 1 d . . . . . H5A H 0.3946 0.3750 0.3646 0.048 Uiso 1 1 calc R U . . . N6 N 0.1368(4) 0.5749(3) 0.3364(3) 0.0335(13) Uani 1 1 d . . . . . C6 C 0.3890(5) 0.7968(4) 0.1525(3) 0.0350(15) Uani 1 1 d . . . . . N7 N -0.0054(4) 0.5560(3) 0.3437(4) 0.0446(16) Uani 1 1 d . . . . . H7 H -0.0592 0.5645 0.3531 0.054 Uiso 1 1 calc R U . . . C7 C 0.4097(4) 0.6926(4) 0.2127(3) 0.0314(15) Uani 1 1 d . . . . . C8 C 0.4379(5) 0.6164(4) 0.2311(3) 0.0329(15) Uani 1 1 d . . . . . N8 N 0.1250(3) 0.7208(3) 0.3844(3) 0.0303(12) Uani 1 1 d . . . . . N9 N 0.2795(4) 0.7988(3) 0.3945(3) 0.0338(12) Uani 1 1 d . . . . . C9 C 0.5111(5) 0.5828(4) 0.2018(4) 0.0440(19) Uani 1 1 d . . . . . H9 H 0.5434 0.6081 0.1676 0.053 Uiso 1 1 calc R U . . . C10 C 0.5348(6) 0.5126(5) 0.2239(4) 0.053(2) Uani 1 1 d . . . . . H10 H 0.5834 0.4888 0.2047 0.063 Uiso 1 1 calc R U . . . N10 N 0.2168(4) 0.9010(3) 0.4390(3) 0.0481(17) Uani 1 1 d . . . . . H10A H 0.1763 0.9312 0.4529 0.058 Uiso 1 1 calc R U . . . C11 C 0.4859(5) 0.4772(4) 0.2751(4) 0.0434(19) Uani 1 1 d . . . . . H11 H 0.5019 0.4295 0.2915 0.052 Uiso 1 1 calc R U . . . N11 N 0.1877(5) 0.6899(4) 0.2413(3) 0.0542(18) Uani 1 1 d . . . . . N12 N 0.0330(6) 0.8209(5) -0.0348(4) 0.078(3) Uani 1 1 d . . . . . C12 C 0.4128(5) 0.5128(4) 0.3020(3) 0.0319(15) Uani 1 1 d . . . . . C15 C 0.2740(7) 0.3398(5) 0.4712(5) 0.064(3) Uani 1 1 d . . . . . H15 H 0.2985 0.2923 0.4639 0.077 Uiso 1 1 calc R U . . . N15 N 0.4223(4) 0.6663(3) 0.4033(3) 0.0372(13) Uani 1 1 d . . . . . C14 C 0.3012(5) 0.4030(4) 0.4333(4) 0.0412(18) Uani 1 1 d . . . . . N14 N 0.1069(6) 0.7155(5) 0.7874(4) 0.074(3) Uani 1 1 d . . . . . C13 C 0.3601(4) 0.4830(3) 0.3589(4) 0.0306(14) Uani 1 1 d . . . . . N13 N 0.2477(4) 0.6638(3) 0.4830(3) 0.0375(14) Uani 1 1 d . . . . . C17 C 0.1713(7) 0.4217(5) 0.5286(5) 0.071(3) Uani 1 1 d . . . . . H17 H 0.1272 0.4269 0.5619 0.085 Uiso 1 1 calc R U . . . N17 N 0.5580(11) 0.4836(7) 0.5379(9) 0.143(6) Uani 1 1 d . . . . . C16 C 0.2103(7) 0.3509(5) 0.5192(6) 0.077(3) Uani 1 1 d . . . . . H16 H 0.1919 0.3103 0.5466 0.093 Uiso 1 1 calc R U . . . N16 N 0.8152(5) 0.5901(4) 0.3652(5) 0.077(3) Uani 1 1 d . . . . . C19 C 0.2640(5) 0.4738(4) 0.4413(4) 0.0380(17) Uani 1 1 d . . . . . C18 C 0.1968(6) 0.4850(5) 0.4896(4) 0.051(2) Uani 1 1 d . . . . . H18 H 0.1703 0.5320 0.4954 0.061 Uiso 1 1 calc R U . . . N18 N 0.692(3) 0.4521(16) 0.676(2) 0.43(2) Uani 1 1 d D U . . . C37 C 0.4328(5) 0.8494(4) 0.4036(5) 0.050(2) Uani 1 1 d . . . . . H37 H 0.4603 0.8078 0.3832 0.060 Uiso 1 1 calc R U . . . C36 C 0.4803(6) 0.9114(5) 0.4276(5) 0.059(2) Uani 1 1 d . . . . . H36 H 0.5406 0.9108 0.4238 0.071 Uiso 1 1 calc R U . . . C35 C 0.4400(7) 0.9736(5) 0.4569(5) 0.062(3) Uani 1 1 d . . . . . H35 H 0.4740 1.0139 0.4725 0.075 Uiso 1 1 calc R U . . . C34 C 0.3515(7) 0.9781(5) 0.4638(5) 0.061(2) Uani 1 1 d . . . . . H34 H 0.3245 1.0203 0.4835 0.073 Uiso 1 1 calc R U . . . C33 C 0.3038(6) 0.9154(4) 0.4396(4) 0.047(2) Uani 1 1 d . . . . . C32 C 0.2056(5) 0.8300(4) 0.4125(3) 0.0332(16) Uani 1 1 d . . . . . C31 C 0.1212(4) 0.7919(4) 0.4080(3) 0.0327(15) Uani 1 1 d . . . . . C30 C 0.0438(5) 0.8259(5) 0.4283(5) 0.050(2) Uani 1 1 d . . . . . H30 H 0.0428 0.8764 0.4425 0.060 Uiso 1 1 calc R U . . . C29 C -0.0308(5) 0.7839(5) 0.4270(5) 0.055(2) Uani 1 1 d . . . . . H29 H -0.0833 0.8050 0.4415 0.067 Uiso 1 1 calc R U . . . C28 C -0.0271(5) 0.7092(5) 0.4037(5) 0.053(2) Uani 1 1 d . . . . . H28 H -0.0769 0.6793 0.4027 0.064 Uiso 1 1 calc R U . . . C27 C 0.0511(4) 0.6808(4) 0.3826(4) 0.0347(16) Uani 1 1 d . . . . . C26 C 0.0611(4) 0.6034(4) 0.3560(4) 0.0334(15) Uani 1 1 d . . . . . C25 C 0.0279(5) 0.4914(4) 0.3132(4) 0.0447(19) Uani 1 1 d . . . . . C24 C -0.0130(6) 0.4254(5) 0.2906(5) 0.059(2) Uani 1 1 d . . . . . H24 H -0.0727 0.4180 0.2949 0.070 Uiso 1 1 calc R U . . . C23 C 0.0407(6) 0.3720(5) 0.2615(5) 0.063(3) Uani 1 1 d . . . . . H23 H 0.0170 0.3262 0.2468 0.075 Uiso 1 1 calc R U . . . C22 C 0.1289(6) 0.3840(4) 0.2534(5) 0.060(2) Uani 1 1 d . . . . . H22 H 0.1622 0.3469 0.2315 0.072 Uiso 1 1 calc R U . . . C21 C 0.1694(5) 0.4491(4) 0.2767(5) 0.049(2) Uani 1 1 d . . . . . H21 H 0.2289 0.4563 0.2712 0.059 Uiso 1 1 calc R U . . . C20 C 0.1172(5) 0.5034(4) 0.3088(4) 0.0369(16) Uani 1 1 d . . . . . C43 C 0.4950(5) 0.6554(4) 0.4014(4) 0.0374(16) Uani 1 1 d . . . . . C42 C 0.2260(5) 0.6772(4) 0.5389(4) 0.0392(17) Uani 1 1 d . . . . . C41 C 0.1332(6) 0.7108(4) 0.7319(4) 0.051(2) Uani 1 1 d . . . . . C40 C 0.0571(7) 0.8019(6) 0.0184(4) 0.065(3) Uani 1 1 d . . . . . C39 C 0.1545(6) 0.7160(5) 0.1936(4) 0.054(2) Uani 1 1 d . . . . . C38 C 0.3435(5) 0.8518(4) 0.4111(4) 0.0378(17) Uani 1 1 d . . . . . C48 C 0.690(3) 0.3834(17) 0.670(3) 0.40(3) Uani 1 1 d D U . . . C47 C 0.650(3) 0.3007(15) 0.677(2) 0.36(2) Uani 1 1 d D U . . . C46 C 0.4912(14) 0.4728(7) 0.5673(8) 0.119(6) Uani 1 1 d . . . . . C45 C 0.4173(10) 0.4509(13) 0.6077(8) 0.191(11) Uani 1 1 d . . . . . H45A H 0.4301 0.4050 0.6329 0.287 Uiso 1 1 calc R U . . . H45B H 0.3687 0.4426 0.5769 0.287 Uiso 1 1 calc R U . . . H45C H 0.4033 0.4903 0.6407 0.287 Uiso 1 1 calc R U . . . C44 C 0.7462(5) 0.6078(4) 0.3754(5) 0.055(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 Au1 0.0685(3) 0.0811(2) 0.03596(16) 0.00593(17) -0.01915(17) 0.01287(19) C1 0.036(4) 0.034(3) 0.039(4) 0.006(3) -0.004(3) -0.003(3) N1 0.031(4) 0.035(3) 0.031(3) 0.008(2) 0.002(2) 0.003(2) Gd1 0.01773(16) 0.03196(14) 0.02417(14) 0.00236(13) 0.00123(12) 0.00350(12) Au2 0.04314(19) 0.05223(16) 0.03046(14) 0.00139(13) 0.00510(12) 0.00617(13) N2 0.039(4) 0.040(3) 0.028(3) 0.003(3) 0.006(3) -0.006(2) C2 0.051(6) 0.041(4) 0.049(4) 0.006(4) 0.003(4) 0.006(4) Au3 0.02013(14) 0.04368(14) 0.06041(19) -0.00370(14) -0.00022(13) 0.00110(11) N3 0.026(3) 0.035(3) 0.020(2) 0.003(2) 0.003(2) 0.006(2) C3 0.063(7) 0.037(4) 0.076(6) 0.013(4) -0.001(5) 0.006(4) C4 0.087(7) 0.045(4) 0.053(5) 0.022(4) -0.009(5) -0.016(5) N4 0.022(3) 0.039(3) 0.035(3) 0.012(3) 0.004(3) 0.004(2) C5 0.057(5) 0.044(4) 0.045(4) 0.010(3) 0.002(4) -0.018(4) N5 0.045(4) 0.033(3) 0.043(4) 0.011(3) 0.002(3) 0.009(3) N6 0.020(3) 0.037(3) 0.043(3) 0.002(3) 0.001(2) 0.007(2) C6 0.037(4) 0.038(3) 0.030(3) 0.006(3) -0.004(3) -0.008(3) N7 0.021(3) 0.045(3) 0.068(4) -0.012(3) 0.008(3) 0.002(3) C7 0.024(4) 0.042(4) 0.028(3) 0.000(3) 0.004(3) 0.000(3) C8 0.034(4) 0.041(4) 0.025(3) 0.001(3) 0.001(3) 0.000(3) N8 0.022(3) 0.037(3) 0.032(3) -0.003(2) 0.000(2) 0.005(2) N9 0.022(3) 0.036(3) 0.043(3) -0.004(3) 0.008(3) 0.001(2) C9 0.036(5) 0.057(5) 0.039(4) 0.014(4) 0.016(3) 0.007(4) C10 0.047(6) 0.062(5) 0.050(5) 0.008(4) 0.018(4) 0.025(4) N10 0.034(4) 0.048(4) 0.062(4) -0.021(3) 0.010(3) 0.001(3) C11 0.045(5) 0.041(4) 0.044(4) 0.005(3) 0.006(4) 0.018(3) N11 0.040(4) 0.079(5) 0.043(4) 0.023(4) -0.013(3) -0.010(4) N12 0.101(7) 0.082(6) 0.051(5) -0.002(4) -0.035(5) 0.025(5) C12 0.035(4) 0.036(3) 0.025(3) -0.002(3) 0.004(3) 0.005(3) C15 0.074(7) 0.044(4) 0.074(6) 0.029(4) 0.016(5) 0.013(5) N15 0.023(3) 0.050(3) 0.038(3) -0.005(3) -0.001(3) 0.007(3) C14 0.043(5) 0.036(4) 0.044(4) 0.011(3) 0.006(3) 0.004(3) N14 0.095(7) 0.083(6) 0.045(4) 0.010(4) 0.026(4) 0.039(5) C13 0.023(4) 0.035(3) 0.034(3) 0.004(3) -0.002(3) 0.011(3) N13 0.031(4) 0.049(3) 0.033(3) 0.002(3) 0.001(2) 0.003(3) C17 0.055(6) 0.079(6) 0.078(7) 0.036(5) 0.036(5) 0.006(5) N17 0.177(16) 0.089(8) 0.162(14) -0.034(9) 0.056(12) -0.020(9) C16 0.075(8) 0.063(6) 0.094(8) 0.045(5) 0.031(6) 0.005(5) N16 0.017(4) 0.070(5) 0.144(8) -0.025(5) 0.006(5) -0.002(3) C19 0.035(4) 0.040(4) 0.038(4) 0.016(3) 0.005(3) 0.007(3) C18 0.042(5) 0.051(4) 0.061(5) 0.013(4) 0.017(4) 0.004(4) N18 0.44(3) 0.45(3) 0.39(3) 0.05(2) -0.03(2) -0.04(2) C37 0.037(5) 0.039(4) 0.073(6) 0.000(4) 0.009(4) -0.003(3) C36 0.043(6) 0.049(5) 0.085(7) -0.001(5) 0.007(5) -0.010(4) C35 0.060(7) 0.065(6) 0.062(6) 0.001(5) -0.004(5) -0.029(5) C34 0.055(7) 0.052(5) 0.076(6) -0.016(5) 0.004(5) -0.008(4) C33 0.048(6) 0.039(4) 0.054(5) -0.008(4) 0.002(4) -0.008(4) C32 0.032(4) 0.037(3) 0.031(3) -0.001(3) 0.004(3) 0.006(3) C31 0.025(4) 0.036(3) 0.037(4) -0.006(3) 0.004(3) 0.005(3) C30 0.033(5) 0.051(5) 0.067(5) -0.021(4) 0.003(4) 0.007(4) C29 0.025(5) 0.067(6) 0.074(6) -0.020(5) 0.007(4) 0.011(4) C28 0.024(4) 0.064(5) 0.071(6) -0.018(5) 0.006(4) 0.005(4) C27 0.019(4) 0.052(4) 0.033(4) -0.003(3) 0.002(3) 0.003(3) C26 0.019(4) 0.042(4) 0.039(4) 0.001(3) 0.000(3) -0.002(3) C25 0.027(4) 0.053(4) 0.054(5) -0.003(4) 0.007(4) -0.001(3) C24 0.040(6) 0.049(5) 0.088(7) -0.011(5) -0.001(5) -0.014(4) C23 0.046(6) 0.053(5) 0.089(7) -0.023(5) 0.006(5) -0.013(4) C22 0.049(6) 0.046(4) 0.087(7) -0.022(4) -0.005(5) 0.008(4) C21 0.034(5) 0.044(4) 0.070(6) -0.010(4) -0.007(4) 0.006(4) C20 0.029(4) 0.039(4) 0.043(4) 0.000(3) 0.000(3) 0.001(3) C43 0.027(4) 0.047(4) 0.038(4) -0.006(3) -0.003(3) 0.001(3) C42 0.030(4) 0.050(4) 0.038(4) 0.004(3) 0.000(3) 0.002(3) C41 0.059(6) 0.052(5) 0.041(4) 0.007(4) 0.009(4) 0.017(4) C40 0.079(7) 0.075(6) 0.040(4) -0.006(5) -0.025(4) 0.023(5) C39 0.046(6) 0.081(6) 0.035(4) 0.013(4) -0.012(4) -0.004(4) C38 0.033(4) 0.040(4) 0.041(4) -0.002(3) 0.002(3) -0.005(3) C48 0.40(3) 0.40(3) 0.39(3) 0.009(14) -0.019(14) -0.006(14) C47 0.36(3) 0.34(3) 0.38(3) -0.01(2) -0.07(2) -0.03(2) C46 0.19(2) 0.063(8) 0.101(11) -0.015(7) 0.006(12) -0.022(10) C45 0.118(13) 0.36(3) 0.098(10) -0.109(15) 0.059(10) -0.141(16) C44 0.033(5) 0.045(4) 0.086(7) -0.005(4) 0.002(4) -0.008(3) 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 Au1 C40 1.972(8) . ? Au1 C39 1.976(8) . ? C1 C2 1.389(10) . ? C1 N1 1.395(8) . ? C1 C6 1.400(10) . ? N1 C7 1.333(8) . ? N1 Gd1 2.604(5) . ? Gd1 N15 2.498(6) . ? Gd1 N13 2.521(6) . ? Gd1 N11 2.522(6) . ? Gd1 N9 2.572(5) . ? Gd1 N4 2.576(5) . ? Gd1 N8 2.583(5) . ? Gd1 N6 2.597(6) . ? Gd1 N3 2.630(5) . ? Au2 C42 1.985(7) . ? Au2 C41 1.989(8) . ? Au2 Au3 3.1538(5) 4_466 ? N2 C7 1.339(8) . ? N2 C6 1.370(9) . ? C2 C3 1.384(11) . ? Au3 C43 1.983(7) . ? Au3 C44 1.999(9) . ? Au3 Au2 3.1538(5) 4_566 ? N3 C8 1.337(8) . ? N3 C12 1.354(8) . ? C3 C4 1.364(12) . ? C4 C5 1.377(12) . ? N4 C13 1.317(8) . ? N4 C19 1.403(8) . ? C5 C6 1.374(9) . ? N5 C13 1.348(8) . ? N5 C14 1.367(9) . ? N6 C26 1.321(8) . ? N6 C20 1.399(8) . ? N7 C26 1.340(8) . ? N7 C25 1.377(9) . ? C7 C8 1.455(10) . ? C8 C9 1.387(10) . ? N8 C31 1.334(8) . ? N8 C27 1.338(8) . ? N9 C32 1.308(8) . ? N9 C38 1.393(9) . ? C9 C10 1.358(10) . ? C10 C11 1.378(11) . ? N10 C32 1.361(8) . ? N10 C33 1.362(10) . ? C11 C12 1.386(10) . ? N11 C39 1.136(9) . ? N12 C40 1.126(10) . ? C12 C13 1.447(9) . ? C15 C16 1.350(13) . ? C15 C14 1.391(10) . ? N15 C43 1.133(8) . ? C14 C19 1.382(10) . ? N14 C41 1.130(10) . ? N13 C42 1.134(9) . ? C17 C18 1.396(11) . ? C17 C16 1.398(13) . ? N17 C46 1.18(2) . ? N16 C44 1.123(9) . ? C19 C18 1.394(10) . ? N18 C48 1.218(13) . ? C37 C38 1.380(10) . ? C37 C36 1.392(11) . ? C36 C35 1.377(13) . ? C35 C34 1.368(13) . ? C34 C33 1.404(11) . ? C33 C38 1.387(10) . ? C32 C31 1.464(10) . ? C31 C30 1.387(10) . ? C30 C29 1.365(11) . ? C29 C28 1.392(11) . ? C28 C27 1.362(10) . ? C27 C26 1.463(9) . ? C25 C20 1.391(11) . ? C25 C24 1.392(11) . ? C24 C23 1.368(12) . ? C23 C22 1.381(12) . ? C22 C21 1.378(11) . ? C21 C20 1.390(10) . ? C48 C47 1.589(13) . ? C46 C45 1.42(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 Au1 C39 177.3(4) . . ? C2 C1 N1 131.4(7) . . ? C2 C1 C6 119.3(6) . . ? N1 C1 C6 109.2(6) . . ? C7 N1 C1 104.3(5) . . ? C7 N1 Gd1 116.8(4) . . ? C1 N1 Gd1 134.6(4) . . ? N15 Gd1 N13 75.75(19) . . ? N15 Gd1 N11 142.6(2) . . ? N13 Gd1 N11 137.3(2) . . ? N15 Gd1 N9 78.59(19) . . ? N13 Gd1 N9 70.93(19) . . ? N11 Gd1 N9 95.1(2) . . ? N15 Gd1 N4 75.74(18) . . ? N13 Gd1 N4 75.19(19) . . ? N11 Gd1 N4 122.6(2) . . ? N9 Gd1 N4 141.46(18) . . ? N15 Gd1 N8 134.29(17) . . ? N13 Gd1 N8 67.58(18) . . ? N11 Gd1 N8 70.0(2) . . ? N9 Gd1 N8 64.51(16) . . ? N4 Gd1 N8 117.81(16) . . ? N15 Gd1 N6 143.84(18) . . ? N13 Gd1 N6 89.97(19) . . ? N11 Gd1 N6 66.9(2) . . ? N9 Gd1 N6 128.25(17) . . ? N4 Gd1 N6 68.48(17) . . ? N8 Gd1 N6 63.74(16) . . ? N15 Gd1 N1 78.19(19) . . ? N13 Gd1 N1 140.04(19) . . ? N11 Gd1 N1 64.7(2) . . ? N9 Gd1 N1 74.62(17) . . ? N4 Gd1 N1 126.22(17) . . ? N8 Gd1 N1 114.16(16) . . ? N6 Gd1 N1 127.87(18) . . ? N15 Gd1 N3 66.86(18) . . ? N13 Gd1 N3 129.06(17) . . ? N11 Gd1 N3 91.4(2) . . ? N9 Gd1 N3 129.50(17) . . ? N4 Gd1 N3 63.23(16) . . ? N8 Gd1 N3 158.80(16) . . ? N6 Gd1 N3 100.22(17) . . ? N1 Gd1 N3 63.39(16) . . ? C42 Au2 C41 177.1(3) . . ? C42 Au2 Au3 97.7(2) . 4_466 ? C41 Au2 Au3 84.8(2) . 4_466 ? C7 N2 C6 107.7(6) . . ? C3 C2 C1 116.8(8) . . ? C43 Au3 C44 177.2(3) . . ? C43 Au3 Au2 97.1(2) . 4_566 ? C44 Au3 Au2 85.5(2) . 4_566 ? C8 N3 C12 117.6(6) . . ? C8 N3 Gd1 120.4(4) . . ? C12 N3 Gd1 120.0(4) . . ? C4 C3 C2 122.8(8) . . ? C3 C4 C5 121.6(7) . . ? C13 N4 C19 104.9(5) . . ? C13 N4 Gd1 118.7(4) . . ? C19 N4 Gd1 135.8(4) . . ? C6 C5 C4 116.2(7) . . ? C13 N5 C14 107.7(6) . . ? C26 N6 C20 105.0(6) . . ? C26 N6 Gd1 117.1(4) . . ? C20 N6 Gd1 137.8(4) . . ? N2 C6 C5 131.0(7) . . ? N2 C6 C1 105.6(5) . . ? C5 C6 C1 123.3(7) . . ? C26 N7 C25 107.9(6) . . ? N1 C7 N2 113.1(6) . . ? N1 C7 C8 122.4(6) . . ? N2 C7 C8 124.4(6) . . ? N3 C8 C9 123.2(6) . . ? N3 C8 C7 114.2(6) . . ? C9 C8 C7 122.6(6) . . ? C31 N8 C27 117.8(6) . . ? C31 N8 Gd1 120.4(4) . . ? C27 N8 Gd1 121.6(4) . . ? C32 N9 C38 105.8(6) . . ? C32 N9 Gd1 116.5(4) . . ? C38 N9 Gd1 137.4(4) . . ? C10 C9 C8 118.9(7) . . ? C9 C10 C11 119.0(7) . . ? C32 N10 C33 107.4(6) . . ? C10 C11 C12 119.7(7) . . ? C39 N11 Gd1 167.7(7) . . ? N3 C12 C11 121.5(6) . . ? N3 C12 C13 114.1(6) . . ? C11 C12 C13 124.3(6) . . ? C16 C15 C14 116.8(8) . . ? C43 N15 Gd1 152.4(6) . . ? N5 C14 C19 106.0(6) . . ? N5 C14 C15 131.1(7) . . ? C19 C14 C15 122.9(7) . . ? N4 C13 N5 112.5(6) . . ? N4 C13 C12 123.1(5) . . ? N5 C13 C12 124.4(6) . . ? C42 N13 Gd1 166.3(6) . . ? C18 C17 C16 121.8(8) . . ? C15 C16 C17 121.8(8) . . ? C14 C19 C18 120.5(6) . . ? C14 C19 N4 109.0(6) . . ? C18 C19 N4 130.4(6) . . ? C19 C18 C17 116.2(7) . . ? C38 C37 C36 117.5(7) . . ? C35 C36 C37 121.5(9) . . ? C34 C35 C36 122.1(8) . . ? C35 C34 C33 116.2(8) . . ? N10 C33 C38 106.1(6) . . ? N10 C33 C34 131.4(8) . . ? C38 C33 C34 122.4(8) . . ? N9 C32 N10 112.0(6) . . ? N9 C32 C31 124.2(6) . . ? N10 C32 C31 123.8(6) . . ? N8 C31 C30 122.7(7) . . ? N8 C31 C32 114.4(6) . . ? C30 C31 C32 123.0(6) . . ? C29 C30 C31 118.7(7) . . ? C30 C29 C28 119.1(8) . . ? C27 C28 C29 118.6(8) . . ? N8 C27 C28 123.2(7) . . ? N8 C27 C26 114.3(6) . . ? C28 C27 C26 122.5(6) . . ? N6 C26 N7 112.6(6) . . ? N6 C26 C27 123.0(6) . . ? N7 C26 C27 124.2(6) . . ? N7 C25 C20 105.4(6) . . ? N7 C25 C24 130.9(8) . . ? C20 C25 C24 123.7(7) . . ? C23 C24 C25 115.3(8) . . ? C24 C23 C22 122.2(8) . . ? C21 C22 C23 122.3(8) . . ? C22 C21 C20 117.0(8) . . ? C21 C20 C25 119.4(7) . . ? C21 C20 N6 131.4(7) . . ? C25 C20 N6 109.1(6) . . ? N15 C43 Au3 174.9(6) . . ? N13 C42 Au2 176.0(7) . . ? N14 C41 Au2 177.0(7) . . ? N12 C40 Au1 174.9(9) . . ? N11 C39 Au1 176.0(8) . . ? C37 C38 C33 120.2(7) . . ? C37 C38 N9 131.1(7) . . ? C33 C38 N9 108.7(7) . . ? N18 C48 C47 157(3) . . ? N17 C46 C45 172(2) . . ? N16 C44 Au3 176.3(8) . . ? _database_code_depnum_ccdc_archive 'CCDC 952850'