# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- DLeznoff LnAuCN2.cif' #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Daniel B. Leznoff' _publ_contact_author_address ; Leznoff, Daniel B. Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; _publ_contact_author_phone +1-778-782-4887 _publ_contact_author_fax +1-778-782-3765 _publ_contact_author_email dleznoff@sfu.ca #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; INSERT TITLE ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address R.J.Roberts ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; X.Li ; Department of Chemistry University of Maine Orono, ME United states 04469 ; T.F.Lacey ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; Z.Pan ; Department of Chemistry University of Maine Orono, ME United states 04469 ; H.H.Patterson ; Department of Chemistry University of Maine Orono, ME United states 04469 ; D.B.Leznoff ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; ## -------------------REFERENCES ----------------------## _publ_section_references ; International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. # CRYSTALS # Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 #ORTEP-3 version 1.073 # Farrugia, L.J., (1997) J. Appl. Cryst. 30, 565. # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_1-Nd _database_code_depnum_ccdc_archive 'CCDC 864724' #TrackingRef '- DLeznoff LnAuCN2.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C34 H72 Au N8 Nd O12' _chemical_formula_moiety 'C2 Au N6 Nd O12, 2(C16 H36 N)' _chemical_formula_weight 1126.21 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'I 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,-z x+1,-y+1,-z+1/2 -x,y+1/2,-z+1/2 -x+1/2,y+1,-z+1 -x+1/2,-y,z+1/2 -x+1,-y+1/2,z+1 #------------------------------------------------ _cell_length_a 11.8889(15) _cell_length_b 11.9354(15) _cell_length_c 35.238(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5000.2(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9918 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.81 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 4.014 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4351 _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 293 _diffrn_reflns_number 5877 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_min 1.801 _diffrn_reflns_theta_max 28.375 _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.821 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 44 #========================================================================== # 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 4875 _refine_ls_number_restraints 0 _refine_ls_number_parameters 260 _oxford_refine_ls_R_factor_ref 0.0326 _refine_ls_wR_factor_ref 0.0270 _refine_ls_goodness_of_fit_ref 1.0839 # The values computed from all data _oxford_reflns_number_all 5877 _refine_ls_R_factor_all 0.0439 _refine_ls_wR_factor_all 0.0312 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5012 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_gt 0.0274 _reflns_number_total 5877 _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: 0.594 0.457 0.647 0.222 0.213 ; _refine_ls_shift/su_max 0.0009033 _refine_diff_density_min -1.13 _refine_diff_density_max 1.40 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 44 _oxford_refine_ls_scale 0.05559(5) _oxford_diffrn_Wilson_B_factor 2.86 _oxford_diffrn_Wilson_scale 1493.58 # Number of reflections without Friedels Law is 5877 # Number of reflections with Friedels Law is 3336 # Theoretical number of reflections is about 3131 #--------------------------------------------------------- _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 diffmap # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method None # The Flack parameter was determined before Friedel pairs were merged _refine_ls_abs_structure_Flack 0.023(6) _refine_ls_abs_structure_details 'Flack (1983), 2541 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad #========================================================== # 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' Nd -0.1943 3.0179 22.6845 2.6625 19.6847 0.2106 12.7740 15.8850 2.8514 137.9030 1.9849 '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 0.41677(2) 0.5000 0.2500 0.0382 1.0000 Uani S T . . . . Nd1 Nd 0.5000 0.7500 0.383364(10) 0.0316 1.0000 Uani S T . . . . O1 O 0.4081(3) 0.9450(3) 0.39027(12) 0.0524 1.0000 Uani . . . . . . O2 O 0.3086(3) 0.8217(3) 0.36120(12) 0.0491 1.0000 Uani . . . . . . O3 O 0.2414(3) 0.9887(5) 0.37029(15) 0.0744 1.0000 Uani . . . . . . O4 O 0.3669(3) 0.6035(3) 0.40731(13) 0.0552 1.0000 Uani . . . . . . O5 O 0.3775(4) 0.7501(6) 0.44184(11) 0.0710 1.0000 Uani . . . . . . O6 O 0.2700(4) 0.6129(6) 0.45944(15) 0.0882 1.0000 Uani . . . . . . N1 N 0.4417(4) 0.6353(4) 0.32519(13) 0.0463 1.0000 Uani . . . . . . N2 N 0.3190(4) 0.9185(4) 0.37431(15) 0.0461 1.0000 Uani . . . . . . N3 N 0.3369(4) 0.6542(6) 0.43645(15) 0.0581 1.0000 Uani . . . . . . N4 N 0.5000 0.7500 0.58738(17) 0.0464 1.0000 Uani S T . . . . N5 N 0.5000 0.2500 0.35281(15) 0.0373 1.0000 Uani S T . . . . C1 C 0.5734(5) 0.6753(5) 0.56262(16) 0.0485 1.0000 Uani . . . . . . C2 C 0.5119(6) 0.5993(5) 0.53529(17) 0.0560 1.0000 Uani . . . . . . C3 C 0.5997(7) 0.5342(6) 0.5130(2) 0.0730 1.0000 Uani . . . . . . C4 C 0.5498(7) 0.4532(7) 0.4854(2) 0.0901 1.0000 Uani . . . . . . C5 C 0.5815(5) 0.8178(5) 0.61183(16) 0.0504 1.0000 Uani . . . . . . C6 C 0.5262(5) 0.8987(6) 0.6398(2) 0.0669 1.0000 Uani . . . . . . C7 C 0.6168(6) 0.9486(7) 0.6650(2) 0.0751 1.0000 Uani . . . . . . C8 C 0.5731(9) 1.0341(9) 0.6926(3) 0.1151 1.0000 Uani . . . . . . C9 C 0.5695(5) 0.3292(4) 0.32875(16) 0.0431 1.0000 Uani . . . . . . C10 C 0.6483(6) 0.2741(5) 0.30054(18) 0.0594 1.0000 Uani . . . . . . C11 C 0.7132(6) 0.3610(6) 0.2781(2) 0.0644 1.0000 Uani . . . . . . C12 C 0.7874(7) 0.3162(6) 0.2485(3) 0.0858 1.0000 Uani . . . . . . C13 C 0.4243(5) 0.3232(4) 0.37774(16) 0.0457 1.0000 Uani . . . . . . C14 C 0.3486(6) 0.2594(7) 0.4062(2) 0.0703 1.0000 Uani . . . . . . C15 C 0.2622(10) 0.3297(7) 0.4228(4) 0.1308 1.0000 Uani . . . . . . C16 C 0.1781(11) 0.2741(11) 0.4457(4) 0.1613 1.0000 Uani . . . . . . C17 C 0.4249(5) 0.5847(4) 0.29794(14) 0.0396 1.0000 Uani . . . . . . H11 H 0.6172 0.6307 0.5797 0.061(8) 1.0000 Uiso R . . . . . H12 H 0.6231 0.7238 0.5480 0.061(8) 1.0000 Uiso R . . . . . H21 H 0.4675 0.6440 0.5169 0.078(8) 1.0000 Uiso R . . . . . H22 H 0.4628 0.5486 0.5491 0.078(8) 1.0000 Uiso R . . . . . H31 H 0.6524 0.4959 0.5296 0.100(8) 1.0000 Uiso R . . . . . H32 H 0.6386 0.5878 0.4971 0.101(8) 1.0000 Uiso R . . . . . H41 H 0.6110 0.4136 0.4726 0.139(8) 1.0000 Uiso R . . . . . H42 H 0.5059 0.4001 0.4993 0.139(8) 1.0000 Uiso R . . . . . H43 H 0.5029 0.4884 0.4671 0.139(8) 1.0000 Uiso R . . . . . H51 H 0.6264 0.8627 0.5941 0.057(8) 1.0000 Uiso R . . . . . H52 H 0.6313 0.7661 0.6259 0.057(8) 1.0000 Uiso R . . . . . H61 H 0.4726 0.8619 0.6560 0.063(8) 1.0000 Uiso R . . . . . H62 H 0.4902 0.9558 0.6252 0.063(8) 1.0000 Uiso R . . . . . H71 H 0.6538 0.8890 0.6792 0.081(8) 1.0000 Uiso R . . . . . H72 H 0.6703 0.9841 0.6482 0.081(8) 1.0000 Uiso R . . . . . H81 H 0.6363 1.0646 0.7061 0.177(8) 1.0000 Uiso R . . . . . H82 H 0.5211 1.0020 0.7102 0.177(8) 1.0000 Uiso R . . . . . H83 H 0.5353 1.0933 0.6785 0.177(8) 1.0000 Uiso R . . . . . H91 H 0.6125 0.3722 0.3465 0.067(8) 1.0000 Uiso R . . . . . H92 H 0.5210 0.3766 0.3147 0.068(8) 1.0000 Uiso R . . . . . H101 H 0.6078 0.2251 0.2832 0.080(8) 1.0000 Uiso R . . . . . H102 H 0.7006 0.2326 0.3152 0.080(8) 1.0000 Uiso R . . . . . H111 H 0.7594 0.4010 0.2955 0.085(8) 1.0000 Uiso R . . . . . H112 H 0.6609 0.4111 0.2668 0.085(8) 1.0000 Uiso R . . . . . H121 H 0.8246 0.3769 0.2364 0.118(8) 1.0000 Uiso R . . . . . H122 H 0.8417 0.2668 0.2591 0.118(8) 1.0000 Uiso R . . . . . H123 H 0.7432 0.2769 0.2304 0.118(8) 1.0000 Uiso R . . . . . H131 H 0.4747 0.3727 0.3922 0.055(10) 1.0000 Uiso R . . . . . H132 H 0.3738 0.3639 0.3621 0.056(10) 1.0000 Uiso R . . . . . H141 H 0.3130 0.1962 0.3925 0.087(10) 1.0000 Uiso R . . . . . H142 H 0.3954 0.2256 0.4260 0.086(10) 1.0000 Uiso R . . . . . H151 H 0.2981 0.3900 0.4376 0.155(10) 1.0000 Uiso R . . . . . H152 H 0.2196 0.3615 0.4017 0.155(10) 1.0000 Uiso R . . . . . H161 H 0.1401 0.3241 0.4622 0.272(10) 1.0000 Uiso R . . . . . H162 H 0.2156 0.2162 0.4607 0.272(10) 1.0000 Uiso R . . . . . H163 H 0.1237 0.2379 0.4292 0.272(10) 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 0.04687(17) 0.03706(14) 0.03072(13) -0.00423(15) 0.0000 0.0000 Nd1 0.03216(19) 0.03277(19) 0.02997(18) 0.0000 0.0000 -0.00359(17) O1 0.039(2) 0.0378(17) 0.080(3) -0.0052(18) -0.005(2) -0.0020(18) O2 0.042(2) 0.038(2) 0.067(3) 0.0065(19) -0.0065(19) -0.0047(17) O3 0.039(2) 0.054(3) 0.130(4) 0.026(3) 0.001(2) 0.004(2) O4 0.046(2) 0.049(2) 0.071(3) 0.007(2) 0.023(2) -0.0034(19) O5 0.062(3) 0.108(4) 0.043(2) -0.016(3) 0.0137(18) -0.017(3) O6 0.055(3) 0.136(5) 0.074(3) 0.055(3) 0.026(3) 0.004(3) N1 0.053(3) 0.045(3) 0.040(3) -0.005(2) -0.003(2) -0.002(2) N2 0.025(2) 0.036(2) 0.077(3) 0.014(2) 0.010(2) -0.0028(18) N3 0.033(3) 0.091(4) 0.051(3) 0.025(3) 0.009(2) 0.008(3) N4 0.028(3) 0.059(4) 0.053(4) 0.0000 0.0000 0.009(3) N5 0.042(3) 0.032(3) 0.038(3) 0.0000 0.0000 0.004(3) C1 0.029(3) 0.062(3) 0.055(3) 0.007(3) 0.005(3) 0.013(3) C2 0.040(3) 0.069(4) 0.059(3) -0.006(3) 0.008(3) 0.005(3) C3 0.075(5) 0.073(5) 0.071(4) -0.006(4) 0.018(4) 0.023(4) C4 0.107(7) 0.097(6) 0.066(4) -0.003(4) 0.003(5) 0.045(5) C5 0.028(2) 0.074(4) 0.049(3) 0.004(3) -0.007(3) -0.001(3) C6 0.044(4) 0.081(5) 0.076(4) -0.011(4) 0.002(3) -0.012(3) C7 0.061(4) 0.103(6) 0.061(4) -0.007(4) -0.006(3) -0.020(4) C8 0.108(7) 0.150(11) 0.088(5) -0.053(6) 0.011(6) -0.040(7) C9 0.041(3) 0.036(3) 0.052(3) 0.003(2) -0.002(3) -0.004(2) C10 0.070(4) 0.046(4) 0.062(4) -0.005(3) 0.018(3) -0.010(3) C11 0.051(4) 0.062(4) 0.080(5) 0.013(4) 0.017(3) 0.002(3) C12 0.100(6) 0.091(5) 0.066(4) 0.001(6) 0.009(6) -0.023(4) C13 0.048(3) 0.036(3) 0.053(3) -0.002(2) 0.013(3) 0.006(2) C14 0.078(4) 0.068(4) 0.065(4) -0.006(4) 0.018(4) -0.003(4) C15 0.129(9) 0.061(5) 0.203(12) 0.011(6) 0.123(9) 0.007(5) C16 0.143(10) 0.127(10) 0.213(13) 0.058(9) 0.132(10) 0.040(8) C17 0.044(3) 0.039(3) 0.035(3) -0.001(2) 0.004(3) 0.001(3) 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 . C17 4_455 1.971(5) yes Au1 . C17 . 1.971(5) yes Nd1 . O1 8_564 2.583(4) yes Nd1 . O2 8_564 2.554(4) yes Nd1 . O5 8_564 2.523(4) yes Nd1 . O4 8_564 2.505(4) yes Nd1 . N1 8_564 2.560(4) yes Nd1 . O1 . 2.583(4) yes Nd1 . O2 . 2.554(4) yes Nd1 . O4 . 2.505(4) yes Nd1 . O5 . 2.523(4) yes Nd1 . N1 . 2.560(4) yes O1 . N2 . 1.241(6) yes O2 . N2 . 1.250(6) yes O3 . N2 . 1.255(6) yes O4 . N3 . 1.244(7) yes O5 . N3 . 1.256(8) yes O6 . N3 . 1.238(6) yes N1 . C17 . 1.152(7) yes N4 . C5 8_564 1.529(7) yes N4 . C1 8_564 1.522(6) yes N4 . C1 . 1.522(6) yes N4 . C5 . 1.529(7) yes N5 . C13 8_554 1.531(6) yes N5 . C9 8_554 1.514(6) yes N5 . C9 . 1.514(6) yes N5 . C13 . 1.531(6) yes C1 . C2 . 1.512(8) yes C1 . H11 . 0.959 no C1 . H12 . 0.974 no C2 . C3 . 1.520(9) yes C2 . H21 . 0.993 no C2 . H22 . 0.973 no C3 . C4 . 1.493(11) yes C3 . H31 . 0.974 no C3 . H32 . 0.967 no C4 . H41 . 0.979 no C4 . H42 . 0.956 no C4 . H43 . 0.952 no C5 . C6 . 1.529(9) yes C5 . H51 . 0.980 no C5 . H52 . 0.988 no C6 . C7 . 1.517(9) yes C6 . H61 . 0.961 no C6 . H62 . 0.956 no C7 . C8 . 1.501(11) yes C7 . H71 . 0.975 no C7 . H72 . 0.967 no C8 . H81 . 0.962 no C8 . H82 . 0.957 no C8 . H83 . 0.973 no C9 . C10 . 1.516(8) yes C9 . H91 . 0.957 no C9 . H92 . 0.947 no C10 . C11 . 1.514(9) yes C10 . H101 . 0.973 no C10 . H102 . 0.947 no C11 . C12 . 1.468(11) yes C11 . H111 . 0.950 no C11 . H112 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . C14 . 1.547(9) yes C13 . H131 . 0.984 no C13 . H132 . 0.949 no C14 . C15 . 1.450(11) yes C14 . H141 . 0.990 no C14 . H142 . 0.980 no C15 . C16 . 1.445(12) yes C15 . H151 . 0.985 no C15 . H152 . 0.977 no C16 . H161 . 0.948 no C16 . H162 . 0.978 no C16 . H163 . 0.971 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 C17 4_455 Au1 . C17 . 174.4(4) yes O1 8_564 Nd1 . O2 8_564 49.45(12) yes O1 8_564 Nd1 . O5 8_564 71.26(18) yes O2 8_564 Nd1 . O5 8_564 74.66(15) yes O1 8_564 Nd1 . O4 8_564 109.29(14) yes O2 8_564 Nd1 . O4 8_564 76.95(13) yes O5 8_564 Nd1 . O4 8_564 50.24(17) yes O1 8_564 Nd1 . N1 8_564 116.28(14) yes O2 8_564 Nd1 . N1 8_564 72.13(14) yes O5 8_564 Nd1 . N1 8_564 119.85(16) yes O4 8_564 Nd1 . N1 8_564 74.07(15) yes O1 8_564 Nd1 . O1 . 169.2(2) yes O2 8_564 Nd1 . O1 . 135.05(12) yes O5 8_564 Nd1 . O1 . 99.64(18) yes O4 8_564 Nd1 . O1 . 66.80(13) yes N1 8_564 Nd1 . O1 . 73.03(15) yes O1 8_564 Nd1 . O2 . 135.05(12) yes O2 8_564 Nd1 . O2 . 144.38(19) yes O5 8_564 Nd1 . O2 . 139.83(15) yes O4 8_564 Nd1 . O2 . 115.59(13) yes N1 8_564 Nd1 . O2 . 79.46(14) yes O1 8_564 Nd1 . O4 . 66.80(13) yes O2 8_564 Nd1 . O4 . 115.59(13) yes O5 8_564 Nd1 . O4 . 95.11(17) yes O4 8_564 Nd1 . O4 . 140.6(2) yes N1 8_564 Nd1 . O4 . 144.49(16) yes O1 8_564 Nd1 . O5 . 99.64(18) yes O2 8_564 Nd1 . O5 . 139.83(15) yes O5 8_564 Nd1 . O5 . 70.5(2) yes O4 8_564 Nd1 . O5 . 95.11(17) yes N1 8_564 Nd1 . O5 . 144.08(19) yes O1 8_564 Nd1 . N1 . 73.03(15) yes O2 8_564 Nd1 . N1 . 79.46(14) yes O5 8_564 Nd1 . N1 . 144.08(19) yes O4 8_564 Nd1 . N1 . 144.49(16) yes N1 8_564 Nd1 . N1 . 73.6(2) yes O1 . Nd1 . O2 . 49.45(12) yes O1 . Nd1 . O4 . 109.29(14) yes O2 . Nd1 . O4 . 76.95(13) yes O1 . Nd1 . O5 . 71.26(18) yes O2 . Nd1 . O5 . 74.66(15) yes O4 . Nd1 . O5 . 50.24(17) yes O1 . Nd1 . N1 . 116.28(14) yes O2 . Nd1 . N1 . 72.13(14) yes O4 . Nd1 . N1 . 74.07(15) yes O5 . Nd1 . N1 . 119.85(16) yes Nd1 . O1 . N2 . 95.1(3) yes Nd1 . O2 . N2 . 96.2(3) yes Nd1 . O4 . N3 . 96.9(4) yes Nd1 . O5 . N3 . 95.6(3) yes Nd1 . N1 . C17 . 174.1(5) yes O3 . N2 . O2 . 120.2(5) yes O3 . N2 . O1 . 120.6(5) yes O2 . N2 . O1 . 119.2(4) yes O5 . N3 . O4 . 117.2(5) yes O5 . N3 . O6 . 120.7(6) yes O4 . N3 . O6 . 122.0(7) yes C5 8_564 N4 . C1 8_564 105.6(3) yes C5 8_564 N4 . C1 . 112.1(3) yes C1 8_564 N4 . C1 . 110.1(6) yes C5 8_564 N4 . C5 . 111.4(6) yes C1 8_564 N4 . C5 . 112.1(3) yes C1 . N4 . C5 . 105.6(3) yes C13 8_554 N5 . C9 8_554 106.6(3) yes C13 8_554 N5 . C9 . 110.9(3) yes C9 8_554 N5 . C9 . 111.9(6) yes C13 8_554 N5 . C13 . 110.0(6) yes C9 8_554 N5 . C13 . 110.9(3) yes C9 . N5 . C13 . 106.6(3) yes N4 . C1 . C2 . 116.1(4) yes N4 . C1 . H11 . 106.1 no C2 . C1 . H11 . 109.2 no N4 . C1 . H12 . 107.6 no C2 . C1 . H12 . 108.2 no H11 . C1 . H12 . 109.4 no C1 . C2 . C3 . 107.7(6) yes C1 . C2 . H21 . 110.6 no C3 . C2 . H21 . 107.6 no C1 . C2 . H22 . 110.1 no C3 . C2 . H22 . 110.7 no H21 . C2 . H22 . 110.1 no C2 . C3 . C4 . 113.2(7) yes C2 . C3 . H31 . 111.7 no C4 . C3 . H31 . 110.1 no C2 . C3 . H32 . 106.9 no C4 . C3 . H32 . 104.0 no H31 . C3 . H32 . 110.6 no C3 . C4 . H41 . 108.6 no C3 . C4 . H42 . 108.4 no H41 . C4 . H42 . 108.8 no C3 . C4 . H43 . 112.9 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 108.6 no N4 . C5 . C6 . 115.2(4) yes N4 . C5 . H51 . 105.9 no C6 . C5 . H51 . 107.5 no N4 . C5 . H52 . 109.4 no C6 . C5 . H52 . 109.1 no H51 . C5 . H52 . 109.6 no C5 . C6 . C7 . 108.6(5) yes C5 . C6 . H61 . 112.3 no C7 . C6 . H61 . 107.7 no C5 . C6 . H62 . 107.1 no C7 . C6 . H62 . 110.6 no H61 . C6 . H62 . 110.4 no C6 . C7 . C8 . 113.6(7) yes C6 . C7 . H71 . 109.5 no C8 . C7 . H71 . 108.7 no C6 . C7 . H72 . 106.3 no C8 . C7 . H72 . 109.1 no H71 . C7 . H72 . 109.7 no C7 . C8 . H81 . 108.0 no C7 . C8 . H82 . 111.9 no H81 . C8 . H82 . 109.6 no C7 . C8 . H83 . 108.9 no H81 . C8 . H83 . 109.7 no H82 . C8 . H83 . 108.8 no N5 . C9 . C10 . 115.7(4) yes N5 . C9 . H91 . 105.2 no C10 . C9 . H91 . 109.3 no N5 . C9 . H92 . 109.4 no C10 . C9 . H92 . 107.1 no H91 . C9 . H92 . 110.2 no C9 . C10 . C11 . 111.1(5) yes C9 . C10 . H101 . 111.4 no C11 . C10 . H101 . 109.7 no C9 . C10 . H102 . 106.0 no C11 . C10 . H102 . 108.0 no H101 . C10 . H102 . 110.5 no C10 . C11 . C12 . 115.3(6) yes C10 . C11 . H111 . 107.6 no C12 . C11 . H111 . 107.0 no C10 . C11 . H112 . 108.5 no C12 . C11 . H112 . 108.9 no H111 . C11 . H112 . 109.5 no C11 . C12 . H121 . 108.7 no C11 . C12 . H122 . 110.8 no H121 . C12 . H122 . 109.5 no C11 . C12 . H123 . 108.9 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no N5 . C13 . C14 . 115.6(4) yes N5 . C13 . H131 . 106.4 no C14 . C13 . H131 . 108.2 no N5 . C13 . H132 . 109.3 no C14 . C13 . H132 . 105.1 no H131 . C13 . H132 . 112.3 no C13 . C14 . C15 . 112.9(7) yes C13 . C14 . H141 . 108.0 no C15 . C14 . H141 . 109.5 no C13 . C14 . H142 . 109.5 no C15 . C14 . H142 . 110.6 no H141 . C14 . H142 . 106.1 no C14 . C15 . C16 . 116.8(8) yes C14 . C15 . H151 . 109.2 no C16 . C15 . H151 . 110.0 no C14 . C15 . H152 . 106.4 no C16 . C15 . H152 . 104.2 no H151 . C15 . H152 . 110.0 no C15 . C16 . H161 . 112.5 no C15 . C16 . H162 . 108.1 no H161 . C16 . H162 . 109.3 no C15 . C16 . H163 . 109.4 no H161 . C16 . H163 . 109.2 no H162 . C16 . H163 . 108.3 no N1 . C17 . Au1 . 172.7(5) yes data_2-Eu _database_code_depnum_ccdc_archive 'CCDC 864725' #TrackingRef '- DLeznoff LnAuCN2.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C34 H72 Au1 Eu1 N8 O12' _chemical_formula_moiety 'C2 Au Eu N6 O12, 2(C16 H36 N)' _chemical_formula_weight 1133.92 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'I 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,-z x+1,-y+1,-z+1/2 -x,y+1/2,-z+1/2 -x+1/2,y+1,-z+1 -x+1/2,-y,z+1/2 -x+1,-y+1/2,z+1 #------------------------------------------------ _cell_length_a 12.0175(13) _cell_length_b 12.0203(14) _cell_length_c 35.042(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5062.0(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9879 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 29.06 _cell_measurement_temperature 293 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.228 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_max 0.284 _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 4.179 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6066 _exptl_absorpt_correction_T_max 0.7461 #============================================================================= # 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 293 _diffrn_reflns_number 7762 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_min 1.791 _diffrn_reflns_theta_max 30.662 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.662 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 49 #========================================================================== # 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 6418 _refine_ls_number_restraints 0 _refine_ls_number_parameters 261 _oxford_refine_ls_R_factor_ref 0.0225 _refine_ls_wR_factor_ref 0.0194 _refine_ls_goodness_of_fit_ref 1.0644 # The values computed from all data _oxford_reflns_number_all 7762 _refine_ls_R_factor_all 0.0569 _refine_ls_wR_factor_all 0.0472 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6566 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_gt 0.0196 _reflns_number_total 7762 _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: 0.227 0.220 0.189 0.852E-01 0.309E-01 ; _refine_ls_shift/su_max 0.0007397 _refine_diff_density_min -0.53 _refine_diff_density_max 1.79 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 49 _oxford_refine_ls_scale 0.06307(4) _oxford_diffrn_Wilson_B_factor 3.81 _oxford_diffrn_Wilson_scale 296.81 # Number of reflections without Friedels Law is 7762 # Number of reflections with Friedels Law is 4303 # Theoretical number of reflections is about 3910 #--------------------------------------------------------- _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 _refine_ls_abs_structure_Flack 0.29(4) _refine_ls_abs_structure_details 'Flack (1983), 3459 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad #========================================================== # 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' 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' 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' 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 -0.42053(2) -0.5000 -0.2500 0.0598 1.0000 Uani S T . . . . Eu1 Eu -0.5000 -0.2500 -0.381751(8) 0.0449 1.0000 Uani S T . . . . O1 O -0.3125(3) -0.1806(3) -0.36006(11) 0.0760 1.0000 Uani . . . . . . O2 O -0.4116(3) -0.0605(2) -0.38889(12) 0.0799 1.0000 Uani . . . . . . O3 O -0.2462(3) -0.0173(4) -0.36997(16) 0.1136 1.0000 Uani . . . . . . O4 O -0.6312(3) -0.1073(3) -0.40569(11) 0.0854 1.0000 Uani . . . . . . O5 O -0.6189(4) -0.2487(5) -0.44018(10) 0.1035 1.0000 Uani . . . . . . O6 O -0.7237(4) -0.1135(5) -0.45726(14) 0.1298 1.0000 Uani . . . . . . N1 N -0.4443(4) -0.3633(3) -0.32446(10) 0.0725 1.0000 Uani . . . . . . N2 N 0.0000 -0.7500 -0.08818(14) 0.0715 1.0000 Uani S T . . . . N3 N -0.5000 -0.7500 -0.35266(13) 0.0625 1.0000 Uani S T . . . . N4 N -0.3220(4) -0.0847(3) -0.37283(13) 0.0708 1.0000 Uani . . . . . . N5 N -0.6603(4) -0.1549(5) -0.43492(13) 0.0805 1.0000 Uani . . . . . . C1 C 0.0773(5) -0.8178(5) -0.11279(16) 0.0868 1.0000 Uani . . . . . . C2 C 0.0269(6) -0.8974(7) -0.1411(2) 0.1149 1.0000 Uani . . . . . . C3 C 0.1132(8) -0.9519(8) -0.1652(2) 0.1384 1.0000 Uani . . . . . . C4 C 0.0709(12) -1.0267(15) -0.1925(4) 0.2557 1.0000 Uani . . . . . . C5 C 0.0718(5) -0.6761(5) -0.06384(14) 0.0766 1.0000 Uani . . . . . . C6 C 0.0128(6) -0.6004(5) -0.03629(16) 0.0882 1.0000 Uani . . . . . . C7 C 0.0967(7) -0.5332(7) -0.0143(3) 0.1264 1.0000 Uani . . . . . . C8 C 0.0492(8) -0.4517(6) 0.0129(2) 0.1387 1.0000 Uani . . . . . . C9 C -0.4237(5) -0.6774(4) -0.37728(15) 0.0733 1.0000 Uani . . . . . . C10 C -0.3490(7) -0.7390(6) -0.4048(2) 0.1119 1.0000 Uani . . . . . . C11 C -0.2621(12) -0.6721(8) -0.4215(4) 0.1975 1.0000 Uani . . . . . . C12 C -0.1791(14) -0.7182(14) -0.4410(5) 0.2853 1.0000 Uani . . . . . . C13 C -0.5706(5) -0.6730(4) -0.32827(14) 0.0711 1.0000 Uani . . . . . . C14 C -0.6489(6) -0.7252(4) -0.30074(16) 0.0905 1.0000 Uani . . . . . . C15 C -0.7123(6) -0.6408(6) -0.2785(2) 0.1061 1.0000 Uani . . . . . . C16 C -0.7878(7) -0.6873(8) -0.2494(3) 0.1496 1.0000 Uani . . . . . . C17 C -0.4288(5) -0.4116(4) -0.29725(12) 0.0655 1.0000 Uani . . . . . . H11 H 0.1234 -0.8604 -0.0963 0.099(10) 1.0000 Uiso R . . . . . H12 H 0.1219 -0.7673 -0.1270 0.099(10) 1.0000 Uiso R . . . . . H21 H -0.0133 -0.9524 -0.1273 0.129(10) 1.0000 Uiso R . . . . . H22 H -0.0227 -0.8571 -0.1570 0.129(10) 1.0000 Uiso R . . . . . H31 H 0.1647 -0.9882 -0.1488 0.166(10) 1.0000 Uiso R . . . . . H32 H 0.1506 -0.8962 -0.1795 0.166(10) 1.0000 Uiso R . . . . . H41 H 0.1305 -1.0579 -0.2067 0.253(10) 1.0000 Uiso R . . . . . H42 H 0.0339 -1.0839 -0.1787 0.253(10) 1.0000 Uiso R . . . . . H43 H 0.0199 -0.9919 -0.2094 0.253(10) 1.0000 Uiso R . . . . . H51 H 0.1197 -0.7231 -0.0495 0.122(10) 1.0000 Uiso R . . . . . H52 H 0.1151 -0.6306 -0.0803 0.122(10) 1.0000 Uiso R . . . . . H61 H -0.0282 -0.6440 -0.0186 0.132(10) 1.0000 Uiso R . . . . . H62 H -0.0366 -0.5531 -0.0499 0.132(10) 1.0000 Uiso R . . . . . H71 H 0.1445 -0.5817 -0.0005 0.170(10) 1.0000 Uiso R . . . . . H72 H 0.1388 -0.4926 -0.0325 0.170(10) 1.0000 Uiso R . . . . . H81 H 0.1062 -0.4105 0.0252 0.177(10) 1.0000 Uiso R . . . . . H82 H 0.0072 -0.4914 0.0314 0.177(10) 1.0000 Uiso R . . . . . H83 H 0.0016 -0.4022 -0.0005 0.177(10) 1.0000 Uiso R . . . . . H91 H -0.4693 -0.6305 -0.3925 0.073(9) 1.0000 Uiso R . . . . . H92 H -0.3789 -0.6330 -0.3609 0.073(9) 1.0000 Uiso R . . . . . H101 H -0.3916 -0.7683 -0.4253 0.118(9) 1.0000 Uiso R . . . . . H102 H -0.3163 -0.7984 -0.3908 0.118(9) 1.0000 Uiso R . . . . . H131 H -0.6120 -0.6277 -0.3454 0.077(7) 1.0000 Uiso R . . . . . H132 H -0.5216 -0.6277 -0.3137 0.077(7) 1.0000 Uiso R . . . . . H141 H -0.7014 -0.7678 -0.3148 0.098(7) 1.0000 Uiso R . . . . . H142 H -0.6096 -0.7726 -0.2837 0.098(7) 1.0000 Uiso R . . . . . H151 H -0.7538 -0.5956 -0.2956 0.112(7) 1.0000 Uiso R . . . . . H152 H -0.6591 -0.5963 -0.2655 0.112(7) 1.0000 Uiso R . . . . . H161 H -0.8237 -0.6288 -0.2359 0.157(7) 1.0000 Uiso R . . . . . H162 H -0.8420 -0.7315 -0.2620 0.157(7) 1.0000 Uiso R . . . . . H163 H -0.7473 -0.7322 -0.2319 0.157(7) 1.0000 Uiso R . . . . . H111 H -0.2969 -0.6177 -0.4371 0.258(9) 1.0000 Uiso R . . . . . H112 H -0.2271 -0.6367 -0.4005 0.258(9) 1.0000 Uiso R . . . . . H121 H -0.1282 -0.6624 -0.4490 0.296(9) 1.0000 Uiso R . . . . . H122 H -0.2108 -0.7532 -0.4627 0.296(9) 1.0000 Uiso R . . . . . H123 H -0.1410 -0.7721 -0.4261 0.296(9) 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 0.08590(19) 0.05151(12) 0.04199(9) 0.00869(11) 0.0000 0.0000 Eu1 0.05512(16) 0.04262(13) 0.03708(11) 0.0000 0.0000 0.00724(14) O1 0.069(2) 0.067(2) 0.092(2) -0.0110(18) -0.0133(18) 0.0106(17) O2 0.073(2) 0.0541(15) 0.113(3) 0.0084(17) -0.004(2) 0.0065(17) O3 0.074(2) 0.069(3) 0.198(5) -0.035(3) 0.015(3) -0.0161(19) O4 0.092(3) 0.074(2) 0.090(2) 0.0140(19) -0.026(2) 0.0168(18) O5 0.110(3) 0.133(3) 0.0674(19) -0.012(3) -0.0240(19) 0.011(3) O6 0.104(4) 0.182(5) 0.104(3) 0.068(3) -0.047(3) -0.014(3) N1 0.101(3) 0.069(2) 0.0474(18) 0.0149(16) -0.010(2) 0.007(2) N2 0.043(3) 0.093(4) 0.078(3) 0.0000 0.0000 -0.011(3) N3 0.079(3) 0.038(2) 0.070(3) 0.0000 0.0000 0.000(3) N4 0.058(3) 0.052(2) 0.102(3) -0.0141(19) 0.013(2) 0.0065(17) N5 0.069(3) 0.103(3) 0.069(3) 0.032(2) -0.014(2) -0.006(3) C1 0.058(3) 0.115(4) 0.088(3) -0.002(3) 0.012(3) -0.009(3) C2 0.099(6) 0.140(6) 0.106(5) -0.026(4) 0.003(4) 0.001(4) C3 0.147(9) 0.154(7) 0.115(5) -0.035(5) 0.014(5) 0.032(5) C4 0.241(16) 0.35(2) 0.177(9) -0.134(13) -0.057(10) 0.129(17) C5 0.052(3) 0.092(3) 0.087(3) 0.007(3) -0.010(3) -0.021(2) C6 0.084(4) 0.088(3) 0.093(3) -0.011(3) -0.008(3) -0.013(3) C7 0.135(7) 0.131(7) 0.113(5) -0.007(5) -0.025(5) -0.053(5) C8 0.199(11) 0.116(5) 0.101(5) -0.018(4) -0.010(5) -0.057(6) C9 0.079(3) 0.055(2) 0.086(3) 0.004(2) 0.008(3) -0.004(2) C10 0.133(6) 0.084(4) 0.119(5) -0.011(4) 0.037(4) -0.003(5) C11 0.236(14) 0.122(7) 0.235(13) -0.025(8) 0.152(12) -0.017(8) C12 0.237(16) 0.228(16) 0.39(2) 0.008(16) 0.195(17) -0.046(13) C13 0.079(3) 0.047(2) 0.087(3) -0.003(2) 0.002(3) 0.011(2) C14 0.113(5) 0.065(3) 0.093(3) 0.005(3) 0.017(3) 0.011(3) C15 0.110(6) 0.095(4) 0.113(5) -0.020(4) 0.023(4) 0.009(3) C16 0.150(8) 0.179(8) 0.119(5) -0.004(8) 0.032(7) 0.021(5) C17 0.088(3) 0.058(2) 0.050(2) 0.0040(17) -0.001(2) 0.001(2) loop_ _oxford_twin_element_scale_factors 0.6727(4) 0.3273(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 . C17 4_434 1.970(4) yes Au1 . C17 . 1.970(4) yes Eu1 . N5 8_344 2.914(4) yes Eu1 . N4 8_344 2.936(4) yes Eu1 . O2 8_344 2.526(3) yes Eu1 . O1 8_344 2.520(4) yes Eu1 . N1 8_344 2.517(3) yes Eu1 . O5 8_344 2.497(3) yes Eu1 . O4 8_344 2.476(3) yes Eu1 . O1 . 2.520(4) yes Eu1 . O2 . 2.526(3) yes Eu1 . O4 . 2.476(3) yes Eu1 . O5 . 2.497(3) yes Eu1 . N1 . 2.517(3) yes Eu1 . N4 . 2.936(4) yes Eu1 . N5 . 2.914(4) yes O1 . N4 . 1.242(6) yes O2 . N4 . 1.249(6) yes O3 . N4 . 1.224(5) yes O4 . N5 . 1.224(6) yes O5 . N5 . 1.246(7) yes O6 . N5 . 1.200(6) yes N1 . C17 . 1.132(5) yes N2 . C1 8_434 1.507(6) yes N2 . C5 8_434 1.504(5) yes N2 . C1 . 1.507(6) yes N2 . C5 . 1.504(5) yes N3 . C9 8_334 1.532(5) yes N3 . C13 8_334 1.519(5) yes N3 . C9 . 1.532(5) yes N3 . C13 . 1.519(5) yes C1 . C2 . 1.505(9) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C2 . C3 . 1.488(11) yes C2 . H21 . 0.950 no C2 . H22 . 0.950 no C3 . C4 . 1.408(14) yes C3 . H31 . 0.950 no C3 . H32 . 0.950 no C4 . H41 . 0.950 no C4 . H42 . 0.950 no C4 . H43 . 0.950 no C5 . C6 . 1.505(8) yes C5 . H51 . 0.950 no C5 . H52 . 0.950 no C6 . C7 . 1.505(9) yes C6 . H61 . 0.950 no C6 . H62 . 0.950 no C7 . C8 . 1.480(11) yes C7 . H71 . 0.950 no C7 . H72 . 0.950 no C8 . H81 . 0.950 no C8 . H82 . 0.950 no C8 . H83 . 0.950 no C9 . C10 . 1.511(8) yes C9 . H91 . 0.950 no C9 . H92 . 0.950 no C10 . C11 . 1.442(12) yes C10 . H101 . 0.950 no C10 . H102 . 0.950 no C11 . C12 . 1.329(15) yes C11 . H111 . 0.950 no C11 . H112 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . C14 . 1.487(8) yes C13 . H131 . 0.950 no C13 . H132 . 0.950 no C14 . C15 . 1.489(9) yes C14 . H141 . 0.950 no C14 . H142 . 0.950 no C15 . C16 . 1.476(11) yes C15 . H151 . 0.950 no C15 . H152 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 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 C17 4_434 Au1 . C17 . 174.2(4) yes N5 8_344 Eu1 . N4 8_344 106.52(14) yes N5 8_344 Eu1 . O2 8_344 82.01(13) yes N4 8_344 Eu1 . O2 8_344 25.03(12) yes N5 8_344 Eu1 . O1 8_344 130.86(13) yes N4 8_344 Eu1 . O1 8_344 24.84(13) yes O2 8_344 Eu1 . O1 8_344 49.86(11) yes N5 8_344 Eu1 . N1 8_344 153.94(14) yes N4 8_344 Eu1 . N1 8_344 95.02(14) yes O2 8_344 Eu1 . N1 8_344 117.08(13) yes O1 8_344 Eu1 . N1 8_344 72.58(14) yes N5 8_344 Eu1 . O5 8_344 25.15(15) yes N4 8_344 Eu1 . O5 8_344 120.01(16) yes O2 8_344 Eu1 . O5 8_344 98.85(16) yes O1 8_344 Eu1 . O5 8_344 139.20(14) yes N1 8_344 Eu1 . O5 8_344 144.07(17) yes N5 8_344 Eu1 . O4 8_344 24.58(14) yes N4 8_344 Eu1 . O4 8_344 91.79(14) yes O2 8_344 Eu1 . O4 8_344 67.02(14) yes O1 8_344 Eu1 . O4 8_344 116.25(13) yes N1 8_344 Eu1 . O4 8_344 144.54(14) yes N5 8_344 Eu1 . O1 . 74.43(12) yes N4 8_344 Eu1 . O1 . 147.48(12) yes O2 8_344 Eu1 . O1 . 134.78(11) yes O1 8_344 Eu1 . O1 . 144.89(18) yes N1 8_344 Eu1 . O1 . 79.53(14) yes N5 8_344 Eu1 . O2 . 90.71(14) yes N4 8_344 Eu1 . O2 . 158.01(11) yes O2 8_344 Eu1 . O2 . 168.63(19) yes O1 8_344 Eu1 . O2 . 134.78(11) yes N1 8_344 Eu1 . O2 . 72.71(13) yes N5 8_344 Eu1 . O4 . 118.44(16) yes N4 8_344 Eu1 . O4 . 92.35(13) yes O2 8_344 Eu1 . O4 . 108.87(14) yes O1 8_344 Eu1 . O4 . 76.24(13) yes N1 8_344 Eu1 . O4 . 74.09(14) yes N5 8_344 Eu1 . O5 . 81.74(16) yes N4 8_344 Eu1 . O5 . 71.01(15) yes O2 8_344 Eu1 . O5 . 71.56(17) yes O1 8_344 Eu1 . O5 . 74.79(14) yes N1 8_344 Eu1 . O5 . 119.90(16) yes N5 8_344 Eu1 . N1 . 97.00(16) yes N4 8_344 Eu1 . N1 . 75.09(13) yes O2 8_344 Eu1 . N1 . 72.71(13) yes O1 8_344 Eu1 . N1 . 79.53(14) yes N1 8_344 Eu1 . N1 . 74.18(19) yes N5 8_344 Eu1 . N4 . 81.49(12) yes N4 8_344 Eu1 . N4 . 167.77(18) yes O2 8_344 Eu1 . N4 . 158.01(11) yes O1 8_344 Eu1 . N4 . 147.48(12) yes N1 8_344 Eu1 . N4 . 75.09(13) yes N5 8_344 Eu1 . N5 . 100.5(2) yes N4 8_344 Eu1 . N5 . 81.49(12) yes O2 8_344 Eu1 . N5 . 90.71(14) yes O1 8_344 Eu1 . N5 . 74.43(12) yes N1 8_344 Eu1 . N5 . 97.00(16) yes O5 8_344 Eu1 . O4 8_344 49.73(16) yes O5 8_344 Eu1 . O1 . 74.79(14) yes O4 8_344 Eu1 . O1 . 76.24(13) yes O5 8_344 Eu1 . O2 . 71.56(17) yes O4 8_344 Eu1 . O2 . 108.87(14) yes O1 . Eu1 . O2 . 49.86(11) yes O5 8_344 Eu1 . O4 . 95.21(16) yes O4 8_344 Eu1 . O4 . 140.40(19) yes O1 . Eu1 . O4 . 116.25(13) yes O2 . Eu1 . O4 . 67.02(14) yes O5 8_344 Eu1 . O5 . 69.8(2) yes O4 8_344 Eu1 . O5 . 95.21(16) yes O1 . Eu1 . O5 . 139.20(14) yes O2 . Eu1 . O5 . 98.85(16) yes O4 . Eu1 . O5 . 49.73(16) yes O5 8_344 Eu1 . N1 . 119.90(16) yes O4 8_344 Eu1 . N1 . 74.09(14) yes O1 . Eu1 . N1 . 72.58(14) yes O2 . Eu1 . N1 . 117.08(13) yes O4 . Eu1 . N1 . 144.54(14) yes O5 8_344 Eu1 . N4 . 71.01(15) yes O4 8_344 Eu1 . N4 . 92.35(13) yes O1 . Eu1 . N4 . 24.84(13) yes O2 . Eu1 . N4 . 25.03(12) yes O4 . Eu1 . N4 . 91.79(14) yes O5 8_344 Eu1 . N5 . 81.74(16) yes O4 8_344 Eu1 . N5 . 118.44(16) yes O1 . Eu1 . N5 . 130.86(13) yes O2 . Eu1 . N5 . 82.01(13) yes O4 . Eu1 . N5 . 24.58(14) yes O5 . Eu1 . N1 . 144.07(17) yes O5 . Eu1 . N4 . 120.01(16) yes N1 . Eu1 . N4 . 95.02(14) yes O5 . Eu1 . N5 . 25.15(15) yes N1 . Eu1 . N5 . 153.94(14) yes N4 . Eu1 . N5 . 106.52(14) yes Eu1 . O1 . N4 . 96.7(3) yes Eu1 . O2 . N4 . 96.2(2) yes Eu1 . O4 . N5 . 98.1(3) yes Eu1 . O5 . N5 . 96.5(3) yes Eu1 . N1 . C17 . 173.4(5) yes C1 8_434 N2 . C5 8_434 106.9(3) yes C1 8_434 N2 . C1 . 110.2(6) yes C5 8_434 N2 . C1 . 111.0(3) yes C1 8_434 N2 . C5 . 111.0(3) yes C5 8_434 N2 . C5 . 110.9(5) yes C1 . N2 . C5 . 106.9(3) yes C9 8_334 N3 . C13 8_334 107.7(3) yes C9 8_334 N3 . C9 . 111.4(5) yes C13 8_334 N3 . C9 . 109.3(3) yes C9 8_334 N3 . C13 . 109.3(3) yes C13 8_334 N3 . C13 . 111.5(5) yes C9 . N3 . C13 . 107.7(3) yes Eu1 . N4 . O2 . 58.8(2) yes Eu1 . N4 . O1 . 58.5(2) yes O2 . N4 . O1 . 117.3(4) yes Eu1 . N4 . O3 . 178.1(3) yes O2 . N4 . O3 . 121.7(5) yes O1 . N4 . O3 . 121.1(5) yes Eu1 . N5 . O5 . 58.4(2) yes Eu1 . N5 . O4 . 57.3(2) yes O5 . N5 . O4 . 115.6(4) yes Eu1 . N5 . O6 . 177.9(4) yes O5 . N5 . O6 . 122.1(6) yes O4 . N5 . O6 . 122.2(6) yes N2 . C1 . C2 . 118.2(5) yes N2 . C1 . H11 . 107.7 no C2 . C1 . H11 . 107.0 no N2 . C1 . H12 . 107.5 no C2 . C1 . H12 . 106.8 no H11 . C1 . H12 . 109.5 no C1 . C2 . C3 . 111.9(6) yes C1 . C2 . H21 . 108.3 no C3 . C2 . H21 . 109.6 no C1 . C2 . H22 . 108.3 no C3 . C2 . H22 . 109.2 no H21 . C2 . H22 . 109.5 no C2 . C3 . C4 . 114.6(9) yes C2 . C3 . H31 . 108.3 no C4 . C3 . H31 . 110.7 no C2 . C3 . H32 . 108.6 no C4 . C3 . H32 . 105.2 no H31 . C3 . H32 . 109.5 no C3 . C4 . H41 . 109.7 no C3 . C4 . H42 . 106.6 no H41 . C4 . H42 . 109.5 no C3 . C4 . H43 . 112.1 no H41 . C4 . H43 . 109.5 no H42 . C4 . H43 . 109.5 no N2 . C5 . C6 . 116.8(5) yes N2 . C5 . H51 . 107.3 no C6 . C5 . H51 . 107.7 no N2 . C5 . H52 . 108.0 no C6 . C5 . H52 . 107.4 no H51 . C5 . H52 . 109.5 no C5 . C6 . C7 . 109.8(6) yes C5 . C6 . H61 . 109.3 no C7 . C6 . H61 . 108.0 no C5 . C6 . H62 . 109.6 no C7 . C6 . H62 . 110.8 no H61 . C6 . H62 . 109.5 no C6 . C7 . C8 . 115.3(8) yes C6 . C7 . H71 . 109.6 no C8 . C7 . H71 . 108.3 no C6 . C7 . H72 . 106.8 no C8 . C7 . H72 . 107.3 no H71 . C7 . H72 . 109.5 no C7 . C8 . H81 . 111.1 no C7 . C8 . H82 . 108.2 no H81 . C8 . H82 . 109.5 no C7 . C8 . H83 . 109.1 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no N3 . C9 . C10 . 115.8(4) yes N3 . C9 . H91 . 108.0 no C10 . C9 . H91 . 106.0 no N3 . C9 . H92 . 108.7 no C10 . C9 . H92 . 108.8 no H91 . C9 . H92 . 109.5 no C9 . C10 . C11 . 114.6(6) yes C9 . C10 . H101 . 110.1 no C11 . C10 . H101 . 106.8 no C9 . C10 . H102 . 106.6 no C11 . C10 . H102 . 109.2 no H101 . C10 . H102 . 109.5 no C10 . C11 . C12 . 121.3(10) yes C10 . C11 . H111 . 107.4 no C12 . C11 . H111 . 108.8 no C10 . C11 . H112 . 104.7 no C12 . C11 . H112 . 104.7 no H111 . C11 . H112 . 109.5 no C11 . C12 . H121 . 109.9 no C11 . C12 . H122 . 107.2 no H121 . C12 . H122 . 109.5 no C11 . C12 . H123 . 111.3 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no N3 . C13 . C14 . 117.5(4) yes N3 . C13 . H131 . 106.7 no C14 . C13 . H131 . 108.7 no N3 . C13 . H132 . 107.8 no C14 . C13 . H132 . 106.6 no H131 . C13 . H132 . 109.5 no C13 . C14 . C15 . 112.1(5) yes C13 . C14 . H141 . 108.1 no C15 . C14 . H141 . 107.4 no C13 . C14 . H142 . 110.2 no C15 . C14 . H142 . 109.5 no H141 . C14 . H142 . 109.5 no C14 . C15 . C16 . 114.7(7) yes C14 . C15 . H151 . 109.1 no C16 . C15 . H151 . 109.3 no C14 . C15 . H152 . 106.9 no C16 . C15 . H152 . 107.2 no H151 . C15 . H152 . 109.5 no C15 . C16 . H161 . 110.0 no C15 . C16 . H162 . 108.1 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 110.2 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no Au1 . C17 . N1 . 173.4(6) yes data_3-Gd _database_code_depnum_ccdc_archive 'CCDC 864726' #TrackingRef '- DLeznoff LnAuCN2.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C34 H72 Au1 Gd1 N8 O12' _chemical_formula_moiety 'C2 Au Gd N6 O12, 2(C16 H36 N)' _chemical_formula_weight 1139.22 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 -x,-y+1/2,z -x+1/2,-y+1,z+1/2 x,-y,-z+1/2 x+1/2,-y+1/2,-z+1 -x,y+1/2,-z+1/2 -x+1/2,y+1,-z+1 #------------------------------------------------ _cell_length_a 11.9857(2) _cell_length_b 12.0414(2) _cell_length_c 35.0246(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5054.91(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9975 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 293 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_min 0.184 _exptl_crystal_size_mid 0.199 _exptl_crystal_size_max 0.234 _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2284 _exptl_absorpt_coefficient_mu 4.256 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6728 _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 293 _diffrn_reflns_number 14528 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_theta_min 1.788 _diffrn_reflns_theta_max 25.588 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.076 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 37 #========================================================================== # 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 3987 _refine_ls_number_restraints 0 _refine_ls_number_parameters 261 _oxford_refine_ls_R_factor_ref 0.0425 _refine_ls_wR_factor_ref 0.0250 _refine_ls_goodness_of_fit_ref 1.0601 # The values computed from all data _oxford_reflns_number_all 4596 _refine_ls_R_factor_all 0.0500 _refine_ls_wR_factor_all 0.0439 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4091 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_gt 0.0252 _reflns_number_total 4617 _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: 0.848 0.906 1.01 0.443 0.338 ; _refine_ls_shift/su_max 0.0005400 _refine_diff_density_min -1.52 _refine_diff_density_max 2.39 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 41 _oxford_refine_ls_scale 0.05533(6) _oxford_diffrn_Wilson_B_factor 3.94 _oxford_diffrn_Wilson_scale 100.85 # Number of reflections without Friedels Law is 4617 # Number of reflections with Friedels Law is 2641 # Theoretical number of reflections is about 2381 #--------------------------------------------------------- _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 _refine_ls_abs_structure_Flack 0.16(3) _refine_ls_abs_structure_details 'Flack (1983), 1976 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad #========================================================== # 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 0.57901(4) 0.5000 0.2500 0.0598 1.0000 Uani S T . . . . Gd1 Gd 0.5000 0.2500 0.118588(14) 0.0454 1.0000 Uani S T . . . . O1 O 0.3117(5) 0.3198(5) 0.14020(17) 0.0770 1.0000 Uani . . . . . . O2 O 0.4120(6) 0.4406(5) 0.11152(18) 0.0826 1.0000 Uani . . . . . . O3 O 0.2465(6) 0.4814(7) 0.1308(2) 0.1154 1.0000 Uani . . . . . . O4 O 0.6179(7) 0.2493(9) 0.06041(16) 0.1074 1.0000 Uani . . . . . . O5 O 0.6314(6) 0.3924(6) 0.0943(2) 0.0871 1.0000 Uani . . . . . . O6 O 0.7238(8) 0.3842(8) 0.0426(2) 0.1292 1.0000 Uani . . . . . . N1 N 0.5542(7) 0.3628(6) 0.17540(19) 0.0714 1.0000 Uani . . . . . . N2 N 0.3210(6) 0.4176(6) 0.1266(2) 0.0618 1.0000 Uani . . . . . . N3 N 0.6592(8) 0.3437(9) 0.0650(2) 0.0816 1.0000 Uani . . . . . . N4 N 0.0000 0.2500 0.0883(2) 0.0696 1.0000 Uani S T . . . . N5 N 0.5000 0.7500 0.1473(2) 0.0645 1.0000 Uani S T . . . . C1 C 0.0817(8) 0.1825(9) 0.1130(3) 0.0848 1.0000 Uani . . . . . . C2 C 0.0271(11) 0.1029(11) 0.1409(3) 0.1185 1.0000 Uani . . . . . . C3 C 0.1125(12) 0.0486(13) 0.1651(3) 0.1404 1.0000 Uani . . . . . . C4 C 0.0738(17) -0.029(2) 0.1916(5) 0.2353 1.0000 Uani . . . . . . C5 C 0.0712(9) 0.3230(8) 0.0636(2) 0.0777 1.0000 Uani . . . . . . C6 C 0.0125(10) 0.3974(8) 0.0364(3) 0.0857 1.0000 Uani . . . . . . C7 C 0.0991(13) 0.4629(12) 0.0142(4) 0.1329 1.0000 Uani . . . . . . C8 C 0.0528(12) 0.5440(11) -0.0133(3) 0.1274 1.0000 Uani . . . . . . C9 C 0.5729(10) 0.6783(8) 0.1224(3) 0.0869 1.0000 Uani . . . . . . C10 C 0.6516(14) 0.7391(11) 0.0944(3) 0.1195 1.0000 Uani . . . . . . C11 C 0.734(2) 0.6687(12) 0.0771(5) 0.1849 1.0000 Uani . . . . . . C12 C 0.816(2) 0.7167(19) 0.0576(8) 0.2617 1.0000 Uani . . . . . . C13 C 0.4289(9) 0.6730(6) 0.1716(2) 0.0677 1.0000 Uani . . . . . . C14 C 0.3512(11) 0.7251(9) 0.1990(3) 0.0937 1.0000 Uani . . . . . . C15 C 0.2879(11) 0.6412(12) 0.2211(4) 0.1119 1.0000 Uani . . . . . . C16 C 0.2139(11) 0.6878(10) 0.2512(4) 0.1421 1.0000 Uani . . . . . . C17 C 0.5692(9) 0.4107(6) 0.2024(2) 0.0638 1.0000 Uani . . . . . . H11 H 0.1278 0.2332 0.1279 0.088(16) 1.0000 Uiso R . . . . . H12 H 0.1291 0.1390 0.0963 0.088(16) 1.0000 Uiso R . . . . . H21 H -0.0248 0.1433 0.1569 0.146(16) 1.0000 Uiso R . . . . . H22 H -0.0124 0.0462 0.1267 0.146(16) 1.0000 Uiso R . . . . . H31 H 0.1503 0.1063 0.1794 0.162(16) 1.0000 Uiso R . . . . . H32 H 0.1647 0.0121 0.1480 0.162(16) 1.0000 Uiso R . . . . . H41 H 0.1295 -0.0417 0.2108 0.321(16) 1.0000 Uiso R . . . . . H42 H 0.0068 -0.0015 0.2033 0.321(16) 1.0000 Uiso R . . . . . H43 H 0.0580 -0.0965 0.1782 0.321(16) 1.0000 Uiso R . . . . . H51 H 0.1128 0.3703 0.0806 0.084(13) 1.0000 Uiso R . . . . . H52 H 0.1215 0.2758 0.0491 0.084(13) 1.0000 Uiso R . . . . . H61 H -0.0349 0.4495 0.0496 0.103(13) 1.0000 Uiso R . . . . . H62 H -0.0323 0.3541 0.0187 0.103(13) 1.0000 Uiso R . . . . . H71 H 0.1452 0.5032 0.0323 0.128(13) 1.0000 Uiso R . . . . . H72 H 0.1444 0.4106 0.0000 0.128(13) 1.0000 Uiso R . . . . . H81 H 0.1018 0.5608 -0.0341 0.161(13) 1.0000 Uiso R . . . . . H82 H 0.0351 0.6110 0.0002 0.161(13) 1.0000 Uiso R . . . . . H83 H -0.0145 0.5110 -0.0227 0.161(13) 1.0000 Uiso R . . . . . H91 H 0.6170 0.6310 0.1386 0.078(15) 1.0000 Uiso R . . . . . H92 H 0.5240 0.6332 0.1069 0.078(15) 1.0000 Uiso R . . . . . H101 H 0.6902 0.7951 0.1093 0.098(15) 1.0000 Uiso R . . . . . H102 H 0.6091 0.7748 0.0743 0.098(15) 1.0000 Uiso R . . . . . H131 H 0.4776 0.6245 0.1858 0.037(8) 1.0000 Uiso R . . . . . H132 H 0.3844 0.6296 0.1540 0.037(8) 1.0000 Uiso R . . . . . H141 H 0.3950 0.7681 0.2168 0.062(8) 1.0000 Uiso R . . . . . H142 H 0.3010 0.7738 0.1853 0.062(8) 1.0000 Uiso R . . . . . H151 H 0.3384 0.5890 0.2330 0.086(8) 1.0000 Uiso R . . . . . H152 H 0.2403 0.6021 0.2033 0.086(8) 1.0000 Uiso R . . . . . H161 H 0.1429 0.6504 0.2522 0.149(8) 1.0000 Uiso R . . . . . H162 H 0.2506 0.6820 0.2754 0.149(8) 1.0000 Uiso R . . . . . H163 H 0.2024 0.7646 0.2451 0.149(8) 1.0000 Uiso R . . . . . H111 H 0.7655 0.6247 0.0968 0.193(15) 1.0000 Uiso R . . . . . H112 H 0.6966 0.6218 0.0594 0.193(15) 1.0000 Uiso R . . . . . H121 H 0.8664 0.6635 0.0473 0.281(15) 1.0000 Uiso R . . . . . H122 H 0.8551 0.7634 0.0750 0.281(15) 1.0000 Uiso R . . . . . H123 H 0.7861 0.7604 0.0375 0.281(15) 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 0.0835(4) 0.0521(3) 0.0439(2) -0.0089(3) 0.0000 0.0000 Gd1 0.0532(3) 0.0442(3) 0.0389(3) 0.0000 0.0000 -0.0071(3) O1 0.069(5) 0.068(4) 0.093(4) -0.015(4) 0.016(3) -0.004(3) O2 0.070(5) 0.059(3) 0.118(4) 0.015(3) 0.009(4) -0.007(3) O3 0.076(5) 0.080(5) 0.190(7) -0.039(5) -0.001(4) 0.005(4) O4 0.119(7) 0.138(6) 0.065(4) -0.006(5) 0.030(3) -0.022(7) O5 0.090(5) 0.086(5) 0.086(4) 0.007(4) 0.027(4) -0.021(4) O6 0.113(7) 0.175(8) 0.100(5) 0.061(6) 0.057(5) 0.031(6) N1 0.088(6) 0.069(4) 0.057(4) -0.017(4) -0.011(4) -0.001(4) N2 0.037(4) 0.043(4) 0.105(6) -0.019(4) -0.003(4) 0.000(3) N3 0.068(6) 0.109(7) 0.068(5) 0.035(5) 0.015(5) 0.010(6) N4 0.035(5) 0.095(6) 0.079(6) 0.0000 0.0000 -0.019(7) N5 0.081(7) 0.043(4) 0.069(5) 0.0000 0.0000 0.009(6) C1 0.046(5) 0.114(7) 0.094(6) 0.002(6) -0.016(6) -0.013(5) C2 0.088(11) 0.151(11) 0.116(8) 0.027(8) 0.011(7) 0.004(8) C3 0.158(16) 0.175(14) 0.088(7) 0.030(8) -0.012(8) 0.056(10) C4 0.24(2) 0.31(3) 0.164(12) 0.098(18) 0.016(14) 0.11(2) C5 0.058(6) 0.088(6) 0.087(6) -0.015(5) 0.009(5) -0.020(5) C6 0.082(8) 0.089(6) 0.086(6) 0.007(5) 0.008(6) -0.007(7) C7 0.160(15) 0.130(12) 0.109(9) 0.023(9) -0.001(10) -0.018(10) C8 0.130(12) 0.153(11) 0.098(7) 0.008(8) -0.009(8) -0.056(9) C9 0.117(8) 0.065(5) 0.079(6) -0.010(5) 0.009(7) 0.012(6) C10 0.183(12) 0.091(7) 0.085(7) -0.009(8) 0.044(8) -0.025(10) C11 0.25(2) 0.094(10) 0.207(16) -0.004(11) 0.153(17) -0.016(13) C12 0.22(3) 0.19(2) 0.38(3) 0.00(2) 0.14(3) 0.024(18) C13 0.079(6) 0.045(4) 0.079(5) 0.004(4) -0.010(6) -0.015(5) C14 0.117(9) 0.081(8) 0.083(6) -0.001(6) 0.014(6) -0.019(6) C15 0.106(11) 0.125(10) 0.104(8) 0.015(8) 0.012(8) 0.011(8) C16 0.157(14) 0.150(11) 0.120(8) 0.004(11) 0.025(12) -0.042(9) C17 0.079(6) 0.053(5) 0.059(5) 0.006(4) -0.006(5) 0.001(5) loop_ _oxford_twin_element_scale_factors 0.8799(9) 0.1201(9) 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 . C17 5_565 1.987(8) yes Au1 . C17 . 1.987(8) yes Gd1 . O2 3_655 2.538(6) yes Gd1 . O1 3_655 2.525(6) yes Gd1 . N1 3_655 2.495(7) yes Gd1 . O4 3_655 2.480(6) yes Gd1 . O5 3_655 2.478(6) yes Gd1 . O1 . 2.525(6) yes Gd1 . O2 . 2.538(6) yes Gd1 . O4 . 2.480(6) yes Gd1 . O5 . 2.478(6) yes Gd1 . N1 . 2.495(7) yes O1 . N2 . 1.275(8) yes O2 . N2 . 1.243(8) yes O3 . N2 . 1.187(8) yes O4 . N3 . 1.250(12) yes O5 . N3 . 1.226(10) yes O6 . N3 . 1.205(10) yes N1 . C17 . 1.123(9) yes N4 . C1 3_555 1.538(10) yes N4 . C5 3_555 1.501(10) yes N4 . C1 . 1.538(10) yes N4 . C5 . 1.501(10) yes N5 . C13 3_665 1.522(9) yes N5 . C9 3_665 1.505(10) yes N5 . C9 . 1.505(10) yes N5 . C13 . 1.522(9) yes C1 . C2 . 1.519(14) yes C1 . H11 . 0.974 no C1 . H12 . 0.968 no C2 . C3 . 1.481(16) yes C2 . H21 . 0.968 no C2 . H22 . 0.968 no C3 . C4 . 1.39(2) yes C3 . H31 . 0.969 no C3 . H32 . 0.971 no C4 . H41 . 0.960 no C4 . H42 . 0.960 no C4 . H43 . 0.961 no C5 . C6 . 1.485(13) yes C5 . H51 . 0.965 no C5 . H52 . 0.971 no C6 . C7 . 1.516(15) yes C6 . H61 . 0.965 no C6 . H62 . 0.971 no C7 . C8 . 1.480(16) yes C7 . H71 . 0.969 no C7 . H72 . 0.970 no C8 . H81 . 0.958 no C8 . H82 . 0.959 no C8 . H83 . 0.958 no C9 . C10 . 1.544(14) yes C9 . H91 . 0.963 no C9 . H92 . 0.966 no C10 . C11 . 1.43(2) yes C10 . H101 . 0.970 no C10 . H102 . 0.971 no C11 . C12 . 1.34(2) yes C11 . H111 . 0.950 no C11 . H112 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . C14 . 1.476(13) yes C13 . H131 . 0.964 no C13 . H132 . 0.969 no C14 . C15 . 1.481(15) yes C14 . H141 . 0.966 no C14 . H142 . 0.967 no C15 . C16 . 1.488(16) yes C15 . H151 . 0.967 no C15 . H152 . 0.968 no C16 . H161 . 0.964 no C16 . H162 . 0.957 no C16 . H163 . 0.958 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 C17 5_565 Au1 . C17 . 173.2(6) yes O2 3_655 Gd1 . O1 3_655 50.0(2) yes O2 3_655 Gd1 . N1 3_655 72.2(2) yes O1 3_655 Gd1 . N1 3_655 79.2(2) yes O2 3_655 Gd1 . O4 3_655 99.2(3) yes O1 3_655 Gd1 . O4 3_655 139.2(2) yes N1 3_655 Gd1 . O4 3_655 120.6(3) yes O2 3_655 Gd1 . O5 3_655 66.7(2) yes O1 3_655 Gd1 . O5 3_655 116.1(2) yes N1 3_655 Gd1 . O5 3_655 74.5(2) yes O4 3_655 Gd1 . O5 3_655 50.0(3) yes O2 3_655 Gd1 . O1 . 134.6(2) yes O1 3_655 Gd1 . O1 . 145.1(3) yes N1 3_655 Gd1 . O1 . 73.1(2) yes O4 3_655 Gd1 . O1 . 74.7(2) yes O5 3_655 Gd1 . O1 . 76.4(2) yes O2 3_655 Gd1 . O2 . 168.8(3) yes O1 3_655 Gd1 . O2 . 134.6(2) yes N1 3_655 Gd1 . O2 . 117.5(2) yes O4 3_655 Gd1 . O2 . 71.3(3) yes O5 3_655 Gd1 . O2 . 109.1(2) yes O2 3_655 Gd1 . O4 . 71.3(3) yes O1 3_655 Gd1 . O4 . 74.7(2) yes N1 3_655 Gd1 . O4 . 143.3(3) yes O4 3_655 Gd1 . O4 . 69.5(4) yes O5 3_655 Gd1 . O4 . 94.4(3) yes O2 3_655 Gd1 . O5 . 109.1(2) yes O1 3_655 Gd1 . O5 . 76.4(2) yes N1 3_655 Gd1 . O5 . 144.7(2) yes O4 3_655 Gd1 . O5 . 94.4(3) yes O5 3_655 Gd1 . O5 . 139.8(3) yes O2 3_655 Gd1 . N1 . 117.5(2) yes O1 3_655 Gd1 . N1 . 73.1(2) yes N1 3_655 Gd1 . N1 . 74.2(3) yes O4 3_655 Gd1 . N1 . 143.3(3) yes O5 3_655 Gd1 . N1 . 144.7(2) yes O1 . Gd1 . O2 . 50.0(2) yes O1 . Gd1 . O4 . 139.2(2) yes O2 . Gd1 . O4 . 99.2(3) yes O1 . Gd1 . O5 . 116.1(2) yes O2 . Gd1 . O5 . 66.7(2) yes O4 . Gd1 . O5 . 50.0(3) yes O1 . Gd1 . N1 . 79.2(2) yes O2 . Gd1 . N1 . 72.2(2) yes O4 . Gd1 . N1 . 120.6(3) yes O5 . Gd1 . N1 . 74.5(2) yes Gd1 . O1 . N2 . 96.7(5) yes Gd1 . O2 . N2 . 97.0(4) yes Gd1 . O4 . N3 . 96.7(6) yes Gd1 . O5 . N3 . 97.4(6) yes Gd1 . N1 . C17 . 173.5(8) yes O1 . N2 . O2 . 116.2(6) yes O1 . N2 . O3 . 119.0(8) yes O2 . N2 . O3 . 124.7(8) yes O4 . N3 . O5 . 115.8(8) yes O4 . N3 . O6 . 122.5(10) yes O5 . N3 . O6 . 121.7(11) yes C1 3_555 N4 . C5 3_555 105.7(5) yes C1 3_555 N4 . C1 . 111.7(9) yes C5 3_555 N4 . C1 . 112.2(5) yes C1 3_555 N4 . C5 . 112.2(5) yes C5 3_555 N4 . C5 . 109.4(8) yes C1 . N4 . C5 . 105.7(5) yes C13 3_665 N5 . C9 3_665 107.5(5) yes C13 3_665 N5 . C9 . 110.4(6) yes C9 3_665 N5 . C9 . 109.3(9) yes C13 3_665 N5 . C13 . 111.7(8) yes C9 3_665 N5 . C13 . 110.4(6) yes C9 . N5 . C13 . 107.5(5) yes N4 . C1 . C2 . 114.9(8) yes N4 . C1 . H11 . 109.3 no C2 . C1 . H11 . 107.2 no N4 . C1 . H12 . 108.8 no C2 . C1 . H12 . 107.4 no H11 . C1 . H12 . 109.2 no C1 . C2 . C3 . 110.4(11) yes C1 . C2 . H21 . 109.4 no C3 . C2 . H21 . 109.6 no C1 . C2 . H22 . 109.0 no C3 . C2 . H22 . 108.7 no H21 . C2 . H22 . 109.7 no C2 . C3 . C4 . 116.4(15) yes C2 . C3 . H31 . 107.6 no C4 . C3 . H31 . 106.9 no C2 . C3 . H32 . 107.0 no C4 . C3 . H32 . 108.8 no H31 . C3 . H32 . 110.1 no C3 . C4 . H41 . 110.1 no C3 . C4 . H42 . 109.6 no H41 . C4 . H42 . 109.6 no C3 . C4 . H43 . 107.9 no H41 . C4 . H43 . 110.0 no H42 . C4 . H43 . 109.7 no N4 . C5 . C6 . 117.0(8) yes N4 . C5 . H51 . 106.4 no C6 . C5 . H51 . 106.6 no N4 . C5 . H52 . 108.2 no C6 . C5 . H52 . 108.2 no H51 . C5 . H52 . 110.4 no C5 . C6 . C7 . 108.5(11) yes C5 . C6 . H61 . 111.2 no C7 . C6 . H61 . 108.1 no C5 . C6 . H62 . 110.3 no C7 . C6 . H62 . 109.3 no H61 . C6 . H62 . 109.3 no C6 . C7 . C8 . 114.7(13) yes C6 . C7 . H71 . 108.5 no C8 . C7 . H71 . 107.9 no C6 . C7 . H72 . 108.0 no C8 . C7 . H72 . 107.7 no H71 . C7 . H72 . 110.0 no C7 . C8 . H81 . 113.8 no C7 . C8 . H82 . 108.5 no H81 . C8 . H82 . 109.5 no C7 . C8 . H83 . 105.5 no H81 . C8 . H83 . 109.9 no H82 . C8 . H83 . 109.5 no N5 . C9 . C10 . 116.7(8) yes N5 . C9 . H91 . 108.5 no C10 . C9 . H91 . 108.6 no N5 . C9 . H92 . 107.2 no C10 . C9 . H92 . 106.3 no H91 . C9 . H92 . 109.4 no C9 . C10 . C11 . 114.0(11) yes C9 . C10 . H101 . 106.3 no C11 . C10 . H101 . 108.1 no C9 . C10 . H102 . 110.6 no C11 . C10 . H102 . 108.3 no H101 . C10 . H102 . 109.5 no C10 . C11 . C12 . 118.0(15) yes C10 . C11 . H111 . 107.4 no C12 . C11 . H111 . 108.3 no C10 . C11 . H112 . 107.9 no C12 . C11 . H112 . 105.6 no H111 . C11 . H112 . 109.5 no C11 . C12 . H121 . 111.8 no C11 . C12 . H122 . 106.9 no H121 . C12 . H122 . 109.5 no C11 . C12 . H123 . 109.7 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no N5 . C13 . C14 . 117.4(6) yes N5 . C13 . H131 . 108.6 no C14 . C13 . H131 . 107.8 no N5 . C13 . H132 . 106.2 no C14 . C13 . H132 . 107.2 no H131 . C13 . H132 . 109.6 no C13 . C14 . C15 . 111.9(9) yes C13 . C14 . H141 . 107.7 no C15 . C14 . H141 . 107.8 no C13 . C14 . H142 . 109.1 no C15 . C14 . H142 . 110.8 no H141 . C14 . H142 . 109.5 no C14 . C15 . C16 . 114.7(11) yes C14 . C15 . H151 . 110.3 no C16 . C15 . H151 . 108.3 no C14 . C15 . H152 . 107.3 no C16 . C15 . H152 . 106.8 no H151 . C15 . H152 . 109.3 no C15 . C16 . H161 . 112.1 no C15 . C16 . H162 . 109.0 no H161 . C16 . H162 . 109.8 no C15 . C16 . H163 . 107.0 no H161 . C16 . H163 . 109.4 no H162 . C16 . H163 . 109.5 no Au1 . C17 . N1 . 174.0(9) yes data_4-Tb _database_code_depnum_ccdc_archive 'CCDC 864727' #TrackingRef '- DLeznoff LnAuCN2.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C34 H72 Au N8 O12 Tb' _chemical_formula_moiety 'C2 Au N6 O12 Tb, 2(C16 H36 N)' _chemical_formula_weight 1140.90 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,-z x+1,-y+1,-z+1/2 -x,y+1/2,-z+1/2 -x+1/2,y+1,-z+1 -x+1/2,-y,z+1/2 -x+1,-y+1/2,z+1 #------------------------------------------------ _cell_length_a 12.0111(5) _cell_length_b 12.0111(5) _cell_length_c 34.9402(16) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5040.7(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9885 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 30.27 _cell_measurement_temperature 296(2) _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_min 0.272 _exptl_crystal_size_mid 0.393 _exptl_crystal_size_max 0.490 _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 4.356 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5088 _exptl_absorpt_correction_T_max 0.7463 #============================================================================= # 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 293 _diffrn_reflns_number 7136 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_min 1.793 _diffrn_reflns_theta_max 29.742 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.742 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 48 #========================================================================== # 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 6029 _refine_ls_number_restraints 0 _refine_ls_number_parameters 261 _oxford_refine_ls_R_factor_ref 0.0228 _refine_ls_wR_factor_ref 0.0184 _refine_ls_goodness_of_fit_ref 1.0729 # The values computed from all data _oxford_reflns_number_all 7136 _refine_ls_R_factor_all 0.0313 _refine_ls_wR_factor_all 0.0257 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6146 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_gt 0.0186 _reflns_number_total 7136 _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: 0.245 0.240 0.212 0.968E-01 0.307E-01 ; _refine_ls_shift/su_max 0.0008564 _refine_diff_density_min -0.51 _refine_diff_density_max 1.22 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 48 _oxford_refine_ls_scale 0.06019(3) _oxford_diffrn_Wilson_B_factor 3.81 _oxford_diffrn_Wilson_scale 317.53 # Number of reflections without Friedels Law is 7136 # Number of reflections with Friedels Law is 3956 # Theoretical number of reflections is about 3574 #--------------------------------------------------------- _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 _refine_ls_abs_structure_Flack 0.29(4) _refine_ls_abs_structure_details 'Flack (1983), 3180 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad #========================================================== # 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 -0.42096(2) -0.5000 -0.2500 0.0587 1.0000 Uani S T . . . . Tb1 Tb -0.5000 -0.2500 -0.381170(8) 0.0452 1.0000 Uani S T . . . . O1 O -0.4126(3) -0.0614(2) -0.38824(12) 0.0794 1.0000 Uani . . . . . . O2 O -0.3144(3) -0.1815(3) -0.35967(11) 0.0755 1.0000 Uani . . . . . . O3 O -0.2462(3) -0.0194(4) -0.36907(16) 0.1131 1.0000 Uani . . . . . . O4 O -0.3829(4) -0.2477(5) -0.43929(10) 0.1022 1.0000 Uani . . . . . . O5 O -0.3704(3) -0.3902(3) -0.40541(11) 0.0825 1.0000 Uani . . . . . . O6 O -0.2783(4) -0.3826(5) -0.45759(14) 0.1235 1.0000 Uani . . . . . . N1 N -0.4455(4) -0.3629(3) -0.32444(10) 0.0688 1.0000 Uani . . . . . . N2 N -0.5000 -0.2500 -0.58817(14) 0.0717 1.0000 Uani S T . . . . N3 N -0.5000 -0.7500 -0.35243(13) 0.0637 1.0000 Uani S T . . . . N4 N -0.3225(4) -0.0853(3) -0.37240(12) 0.0683 1.0000 Uani . . . . . . N5 N -0.3413(4) -0.3425(5) -0.43454(13) 0.0800 1.0000 Uani . . . . . . C1 C -0.5715(5) -0.3242(4) -0.56395(14) 0.0760 1.0000 Uani . . . . . . C2 C -0.5131(6) -0.3984(5) -0.53620(16) 0.0875 1.0000 Uani . . . . . . C3 C -0.5956(7) -0.4679(7) -0.5141(2) 0.1234 1.0000 Uani . . . . . . C4 C -0.5476(9) -0.5465(7) -0.4866(2) 0.1447 1.0000 Uani . . . . . . C5 C -0.5782(5) -0.1828(5) -0.61307(17) 0.0860 1.0000 Uani . . . . . . C6 C -0.5275(6) -0.1039(7) -0.6413(2) 0.1172 1.0000 Uani . . . . . . C7 C -0.6137(8) -0.0488(8) -0.6656(2) 0.1388 1.0000 Uani . . . . . . C8 C -0.5703(12) 0.0284(14) -0.6927(3) 0.2435 1.0000 Uani . . . . . . C9 C -0.5697(5) -0.6727(3) -0.32806(14) 0.0691 1.0000 Uani . . . . . . C10 C -0.6500(6) -0.7248(4) -0.30079(16) 0.0893 1.0000 Uani . . . . . . C11 C -0.7111(6) -0.6413(6) -0.2779(2) 0.1012 1.0000 Uani . . . . . . C12 C -0.7901(7) -0.6871(7) -0.2497(3) 0.1405 1.0000 Uani . . . . . . C13 C -0.4247(5) -0.6774(3) -0.37754(15) 0.0699 1.0000 Uani . . . . . . C14 C -0.3489(7) -0.7388(6) -0.4047(2) 0.1122 1.0000 Uani . . . . . . C15 C -0.2604(12) -0.6691(7) -0.4212(4) 0.2026 1.0000 Uani . . . . . . C16 C -0.1786(13) -0.7180(14) -0.4416(5) 0.2801 1.0000 Uani . . . . . . C17 C -0.4299(5) -0.4115(3) -0.29755(11) 0.0610 1.0000 Uani . . . . . . H11 H -0.6120 -0.3729 -0.5811 0.106(9) 1.0000 Uiso R . . . . . H12 H -0.6231 -0.2774 -0.5503 0.106(9) 1.0000 Uiso R . . . . . H21 H -0.4719 -0.3528 -0.5185 0.118(9) 1.0000 Uiso R . . . . . H22 H -0.4622 -0.4461 -0.5501 0.117(9) 1.0000 Uiso R . . . . . H31 H -0.6374 -0.5104 -0.5335 0.163(9) 1.0000 Uiso R . . . . . H32 H -0.6461 -0.4193 -0.5003 0.162(9) 1.0000 Uiso R . . . . . H41 H -0.6067 -0.5719 -0.4696 0.200(9) 1.0000 Uiso R . . . . . H42 H -0.5166 -0.6085 -0.5007 0.200(9) 1.0000 Uiso R . . . . . H43 H -0.4911 -0.5084 -0.4719 0.200(9) 1.0000 Uiso R . . . . . H51 H -0.6251 -0.1391 -0.5961 0.109(11) 1.0000 Uiso R . . . . . H52 H -0.6253 -0.2349 -0.6274 0.108(11) 1.0000 Uiso R . . . . . H61 H -0.4752 -0.1445 -0.6573 0.135(11) 1.0000 Uiso R . . . . . H62 H -0.4886 -0.0460 -0.6265 0.135(11) 1.0000 Uiso R . . . . . H71 H -0.6538 -0.1053 -0.6798 0.172(11) 1.0000 Uiso R . . . . . H72 H -0.6660 -0.0090 -0.6490 0.172(11) 1.0000 Uiso R . . . . . H81 H -0.6201 0.0266 -0.7148 0.328(11) 1.0000 Uiso R . . . . . H82 H -0.4963 0.0061 -0.7006 0.328(11) 1.0000 Uiso R . . . . . H83 H -0.5701 0.1010 -0.6812 0.328(11) 1.0000 Uiso R . . . . . H91 H -0.6123 -0.6253 -0.3459 0.079(7) 1.0000 Uiso R . . . . . H92 H -0.5190 -0.6282 -0.3128 0.080(7) 1.0000 Uiso R . . . . . H101 H -0.6128 -0.7767 -0.2840 0.103(7) 1.0000 Uiso R . . . . . H102 H -0.7057 -0.7652 -0.3161 0.103(7) 1.0000 Uiso R . . . . . H111 H -0.7539 -0.5964 -0.2961 0.112(7) 1.0000 Uiso R . . . . . H112 H -0.6574 -0.5942 -0.2650 0.112(7) 1.0000 Uiso R . . . . . H121 H -0.8657 -0.6844 -0.2599 0.196(7) 1.0000 Uiso R . . . . . H122 H -0.7868 -0.6445 -0.2261 0.196(7) 1.0000 Uiso R . . . . . H123 H -0.7703 -0.7635 -0.2442 0.196(7) 1.0000 Uiso R . . . . . H131 H -0.3777 -0.6319 -0.3614 0.085(10) 1.0000 Uiso R . . . . . H132 H -0.4719 -0.6298 -0.3931 0.085(10) 1.0000 Uiso R . . . . . H141 H -0.3907 -0.7696 -0.4259 0.133(10) 1.0000 Uiso R . . . . . H142 H -0.3140 -0.7976 -0.3904 0.133(10) 1.0000 Uiso R . . . . . H151 H -0.2944 -0.6113 -0.4357 0.285(10) 1.0000 Uiso R . . . . . H152 H -0.2222 -0.6379 -0.4000 0.285(10) 1.0000 Uiso R . . . . . H161 H -0.1255 -0.6642 -0.4496 0.305(10) 1.0000 Uiso R . . . . . H162 H -0.2143 -0.7489 -0.4635 0.305(10) 1.0000 Uiso R . . . . . H163 H -0.1421 -0.7755 -0.4278 0.305(10) 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 0.0855(2) 0.04956(12) 0.04097(10) 0.00799(12) 0.0000 0.0000 Tb1 0.05733(17) 0.04164(13) 0.03650(11) 0.0000 0.0000 0.00648(14) O1 0.073(2) 0.0528(15) 0.112(3) 0.0081(17) -0.002(2) 0.0034(17) O2 0.068(2) 0.067(2) 0.091(2) -0.0124(18) -0.0124(17) 0.0073(17) O3 0.075(2) 0.069(3) 0.195(5) -0.036(3) 0.010(3) -0.0176(19) O4 0.114(3) 0.129(3) 0.0636(19) 0.013(2) 0.0229(18) 0.010(3) O5 0.089(3) 0.071(2) 0.087(2) -0.0088(18) 0.027(2) 0.0168(18) O6 0.099(3) 0.173(4) 0.099(3) -0.064(3) 0.048(3) -0.013(3) N1 0.095(3) 0.063(2) 0.0480(19) 0.0105(16) -0.007(2) 0.004(2) N2 0.042(3) 0.091(4) 0.083(3) 0.0000 0.0000 -0.009(4) N3 0.086(4) 0.036(2) 0.069(3) 0.0000 0.0000 -0.001(3) N4 0.068(3) 0.046(2) 0.090(3) -0.0133(18) 0.009(2) 0.0065(17) N5 0.066(3) 0.107(3) 0.067(3) -0.029(3) 0.011(2) -0.009(3) C1 0.055(3) 0.085(3) 0.088(3) -0.007(3) 0.011(3) -0.017(2) C2 0.077(4) 0.092(3) 0.093(3) 0.007(3) 0.011(3) -0.012(3) C3 0.133(7) 0.144(7) 0.093(5) 0.000(5) 0.025(5) -0.055(5) C4 0.201(11) 0.137(6) 0.097(5) 0.017(5) 0.014(6) -0.054(6) C5 0.063(3) 0.102(4) 0.093(4) 0.005(3) -0.015(4) -0.006(3) C6 0.089(5) 0.147(6) 0.116(5) 0.035(5) -0.012(4) -0.001(4) C7 0.158(9) 0.150(7) 0.109(5) 0.028(5) -0.010(5) 0.033(5) C8 0.252(16) 0.30(2) 0.178(9) 0.123(12) 0.047(10) 0.101(15) C9 0.082(3) 0.046(2) 0.079(3) -0.0006(19) 0.004(3) 0.009(2) C10 0.108(4) 0.070(3) 0.090(3) 0.001(3) 0.016(3) 0.013(3) C11 0.095(5) 0.098(4) 0.110(5) -0.024(4) 0.023(4) 0.005(3) C12 0.137(7) 0.165(7) 0.119(5) -0.004(7) 0.036(7) 0.022(5) C13 0.081(3) 0.047(2) 0.081(3) 0.000(2) 0.006(3) -0.007(2) C14 0.138(6) 0.086(4) 0.113(5) -0.006(4) 0.034(4) -0.005(5) C15 0.240(13) 0.111(7) 0.257(14) -0.018(7) 0.174(12) -0.022(8) C16 0.233(15) 0.233(16) 0.37(2) -0.023(16) 0.189(17) -0.038(13) C17 0.083(3) 0.057(2) 0.0433(18) 0.0058(16) 0.000(2) 0.000(2) loop_ _oxford_twin_element_scale_factors 0.7101(4) 0.2899(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 . C17 4_434 1.975(4) yes Au1 . C17 . 1.975(4) yes Tb1 . O1 8_344 2.508(3) yes Tb1 . O2 8_344 2.492(3) yes Tb1 . N1 8_344 2.489(3) yes Tb1 . O4 8_344 2.471(3) yes Tb1 . O5 8_344 2.444(3) yes Tb1 . N5 8_344 2.889(4) yes Tb1 . N4 8_344 2.925(4) yes Tb1 . O1 . 2.508(3) yes Tb1 . O2 . 2.492(3) yes Tb1 . O4 . 2.471(3) yes Tb1 . O5 . 2.444(3) yes Tb1 . N1 . 2.489(3) yes Tb1 . N4 . 2.925(4) yes Tb1 . N5 . 2.889(4) yes O1 . N4 . 1.249(6) yes O2 . N4 . 1.242(5) yes O3 . N4 . 1.217(5) yes O4 . N5 . 1.255(7) yes O5 . N5 . 1.219(6) yes O6 . N5 . 1.206(6) yes N1 . C17 . 1.122(5) yes N2 . C5 8_344 1.514(6) yes N2 . C1 8_344 1.499(6) yes N2 . C1 . 1.499(6) yes N2 . C5 . 1.514(6) yes N3 . C13 8_334 1.532(5) yes N3 . C9 8_334 1.513(5) yes N3 . C9 . 1.513(5) yes N3 . C13 . 1.532(5) yes C1 . C2 . 1.491(8) yes C1 . H11 . 0.969 no C1 . H12 . 0.964 no C2 . C3 . 1.508(9) yes C2 . H21 . 0.962 no C2 . H22 . 0.970 no C3 . C4 . 1.465(11) yes C3 . H31 . 0.985 no C3 . H32 . 0.971 no C4 . H41 . 0.975 no C4 . H42 . 0.968 no C4 . H43 . 0.966 no C5 . C6 . 1.497(9) yes C5 . H51 . 0.972 no C5 . H52 . 0.982 no C6 . C7 . 1.494(11) yes C6 . H61 . 0.972 no C6 . H62 . 0.983 no C7 . C8 . 1.425(13) yes C7 . H71 . 0.969 no C7 . H72 . 0.979 no C8 . H81 . 0.974 no C8 . H82 . 0.969 no C8 . H83 . 0.961 no C9 . C10 . 1.493(8) yes C9 . H91 . 0.987 no C9 . H92 . 0.971 no C10 . C11 . 1.478(8) yes C10 . H101 . 0.966 no C10 . H102 . 0.984 no C11 . C12 . 1.473(10) yes C11 . H111 . 0.981 no C11 . H112 . 0.968 no C12 . H121 . 0.976 no C12 . H122 . 0.972 no C12 . H123 . 0.967 no C13 . C14 . 1.508(8) yes C13 . H131 . 0.967 no C13 . H132 . 0.971 no C14 . C15 . 1.471(12) yes C14 . H141 . 0.968 no C14 . H142 . 0.962 no C15 . C16 . 1.348(15) yes C15 . H151 . 0.950 no C15 . H152 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 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 C17 4_434 Au1 . C17 . 173.8(3) yes O1 8_344 Tb1 . O2 8_344 49.99(11) yes O1 8_344 Tb1 . N1 8_344 117.40(13) yes O2 8_344 Tb1 . N1 8_344 72.83(13) yes O1 8_344 Tb1 . O4 8_344 70.77(16) yes O2 8_344 Tb1 . O4 8_344 74.62(14) yes N1 8_344 Tb1 . O4 8_344 120.73(15) yes O1 8_344 Tb1 . O5 8_344 108.75(14) yes O2 8_344 Tb1 . O5 8_344 76.26(12) yes N1 8_344 Tb1 . O5 8_344 74.52(14) yes O4 8_344 Tb1 . O5 8_344 50.24(16) yes O1 8_344 Tb1 . N5 8_344 90.44(14) yes O2 8_344 Tb1 . N5 8_344 74.43(12) yes N1 8_344 Tb1 . N5 8_344 97.52(16) yes O4 8_344 Tb1 . N5 8_344 25.58(15) yes O5 8_344 Tb1 . N5 8_344 24.66(14) yes O1 8_344 Tb1 . N4 8_344 25.10(11) yes O2 8_344 Tb1 . N4 8_344 24.90(13) yes N1 8_344 Tb1 . N4 8_344 95.37(14) yes O4 8_344 Tb1 . N4 8_344 70.33(14) yes O5 8_344 Tb1 . N4 8_344 92.19(13) yes O1 8_344 Tb1 . O1 . 168.70(19) yes O2 8_344 Tb1 . O1 . 134.61(11) yes N1 8_344 Tb1 . O1 . 72.33(13) yes O4 8_344 Tb1 . O1 . 99.64(16) yes O5 8_344 Tb1 . O1 . 67.07(14) yes O1 8_344 Tb1 . O2 . 134.61(11) yes O2 8_344 Tb1 . O2 . 144.91(18) yes N1 8_344 Tb1 . O2 . 79.35(13) yes O4 8_344 Tb1 . O2 . 139.53(14) yes O5 8_344 Tb1 . O2 . 116.51(13) yes O1 8_344 Tb1 . O4 . 99.64(16) yes O2 8_344 Tb1 . O4 . 139.53(14) yes N1 8_344 Tb1 . O4 . 142.95(16) yes O4 8_344 Tb1 . O4 . 69.4(2) yes O5 8_344 Tb1 . O4 . 94.02(16) yes O1 8_344 Tb1 . O5 . 67.07(14) yes O2 8_344 Tb1 . O5 . 116.51(13) yes N1 8_344 Tb1 . O5 . 144.94(14) yes O4 8_344 Tb1 . O5 . 94.02(16) yes O5 8_344 Tb1 . O5 . 139.46(19) yes O1 8_344 Tb1 . N1 . 72.33(13) yes O2 8_344 Tb1 . N1 . 79.35(13) yes N1 8_344 Tb1 . N1 . 74.44(18) yes O4 8_344 Tb1 . N1 . 142.95(16) yes O5 8_344 Tb1 . N1 . 144.94(14) yes O1 8_344 Tb1 . N4 . 157.85(11) yes O2 8_344 Tb1 . N4 . 147.55(12) yes N1 8_344 Tb1 . N4 . 74.91(13) yes O4 8_344 Tb1 . N4 . 120.58(15) yes O5 8_344 Tb1 . N4 . 91.97(14) yes O1 8_344 Tb1 . N5 . 82.25(14) yes O2 8_344 Tb1 . N5 . 131.12(13) yes N1 8_344 Tb1 . N5 . 153.77(14) yes O4 8_344 Tb1 . N5 . 80.84(15) yes O5 8_344 Tb1 . N5 . 117.49(16) yes N5 8_344 Tb1 . N4 8_344 81.20(12) yes N5 8_344 Tb1 . O1 . 82.25(14) yes N4 8_344 Tb1 . O1 . 157.85(11) yes N5 8_344 Tb1 . O2 . 131.12(13) yes N4 8_344 Tb1 . O2 . 147.55(12) yes O1 . Tb1 . O2 . 49.99(11) yes N5 8_344 Tb1 . O4 . 80.84(15) yes N4 8_344 Tb1 . O4 . 120.58(15) yes O1 . Tb1 . O4 . 70.77(16) yes O2 . Tb1 . O4 . 74.62(14) yes N5 8_344 Tb1 . O5 . 117.49(16) yes N4 8_344 Tb1 . O5 . 91.97(14) yes O1 . Tb1 . O5 . 108.75(14) yes O2 . Tb1 . O5 . 76.26(12) yes O4 . Tb1 . O5 . 50.24(16) yes N5 8_344 Tb1 . N1 . 153.77(14) yes N4 8_344 Tb1 . N1 . 74.91(13) yes O1 . Tb1 . N1 . 117.40(13) yes O2 . Tb1 . N1 . 72.83(13) yes O4 . Tb1 . N1 . 120.73(15) yes N5 8_344 Tb1 . N4 . 106.75(14) yes N4 8_344 Tb1 . N4 . 167.98(17) yes O1 . Tb1 . N4 . 25.10(11) yes O2 . Tb1 . N4 . 24.90(13) yes O4 . Tb1 . N4 . 70.33(14) yes N5 8_344 Tb1 . N5 . 99.6(2) yes N4 8_344 Tb1 . N5 . 106.75(14) yes O1 . Tb1 . N5 . 90.44(14) yes O2 . Tb1 . N5 . 74.43(12) yes O4 . Tb1 . N5 . 25.58(15) yes O5 . Tb1 . N1 . 74.52(14) yes O5 . Tb1 . N4 . 92.19(13) yes N1 . Tb1 . N4 . 95.37(14) yes O5 . Tb1 . N5 . 24.66(14) yes N1 . Tb1 . N5 . 97.52(16) yes N4 . Tb1 . N5 . 81.20(12) yes Tb1 . O1 . N4 . 96.4(2) yes Tb1 . O2 . N4 . 97.4(3) yes Tb1 . O4 . N5 . 96.2(3) yes Tb1 . O5 . N5 . 98.5(3) yes Tb1 . N1 . C17 . 173.9(4) yes C5 8_344 N2 . C1 8_344 106.7(3) yes C5 8_344 N2 . C1 . 111.2(3) yes C1 8_344 N2 . C1 . 111.3(5) yes C5 8_344 N2 . C5 . 109.8(6) yes C1 8_344 N2 . C5 . 111.2(3) yes C1 . N2 . C5 . 106.7(3) yes C13 8_334 N3 . C9 8_334 107.4(3) yes C13 8_334 N3 . C9 . 110.2(3) yes C9 8_334 N3 . C9 . 111.5(5) yes C13 8_334 N3 . C13 . 110.1(5) yes C9 8_334 N3 . C13 . 110.2(3) yes C9 . N3 . C13 . 107.4(3) yes O1 . N4 . O2 . 116.1(4) yes O1 . N4 . Tb1 . 58.5(2) yes O2 . N4 . Tb1 . 57.7(2) yes O1 . N4 . O3 . 123.1(5) yes O2 . N4 . O3 . 120.8(5) yes Tb1 . N4 . O3 . 177.9(4) yes Tb1 . N5 . O4 . 58.2(2) yes Tb1 . N5 . O5 . 56.8(2) yes O4 . N5 . O5 . 115.0(4) yes Tb1 . N5 . O6 . 177.6(4) yes O4 . N5 . O6 . 121.6(6) yes O5 . N5 . O6 . 123.4(6) yes N2 . C1 . C2 . 117.0(5) yes N2 . C1 . H11 . 107.3 no C2 . C1 . H11 . 106.2 no N2 . C1 . H12 . 107.5 no C2 . C1 . H12 . 109.2 no H11 . C1 . H12 . 109.6 no C1 . C2 . C3 . 110.8(6) yes C1 . C2 . H21 . 108.6 no C3 . C2 . H21 . 108.9 no C1 . C2 . H22 . 108.8 no C3 . C2 . H22 . 110.1 no H21 . C2 . H22 . 109.5 no C2 . C3 . C4 . 115.7(7) yes C2 . C3 . H31 . 105.7 no C4 . C3 . H31 . 108.4 no C2 . C3 . H32 . 109.4 no C4 . C3 . H32 . 107.9 no H31 . C3 . H32 . 109.6 no C3 . C4 . H41 . 108.4 no C3 . C4 . H42 . 108.3 no H41 . C4 . H42 . 110.5 no C3 . C4 . H43 . 108.6 no H41 . C4 . H43 . 109.6 no H42 . C4 . H43 . 111.4 no N2 . C5 . C6 . 117.6(5) yes N2 . C5 . H51 . 107.3 no C6 . C5 . H51 . 107.2 no N2 . C5 . H52 . 108.1 no C6 . C5 . H52 . 107.6 no H51 . C5 . H52 . 108.7 no C5 . C6 . C7 . 111.9(6) yes C5 . C6 . H61 . 108.9 no C7 . C6 . H61 . 110.1 no C5 . C6 . H62 . 107.2 no C7 . C6 . H62 . 108.3 no H61 . C6 . H62 . 110.4 no C6 . C7 . C8 . 114.4(9) yes C6 . C7 . H71 . 108.9 no C8 . C7 . H71 . 107.3 no C6 . C7 . H72 . 108.9 no C8 . C7 . H72 . 108.1 no H71 . C7 . H72 . 109.0 no C7 . C8 . H81 . 106.7 no C7 . C8 . H82 . 110.2 no H81 . C8 . H82 . 109.5 no C7 . C8 . H83 . 108.2 no H81 . C8 . H83 . 110.7 no H82 . C8 . H83 . 111.5 no N3 . C9 . C10 . 117.4(4) yes N3 . C9 . H91 . 106.6 no C10 . C9 . H91 . 108.0 no N3 . C9 . H92 . 107.5 no C10 . C9 . H92 . 106.6 no H91 . C9 . H92 . 110.7 no C9 . C10 . C11 . 112.5(5) yes C9 . C10 . H101 . 111.0 no C11 . C10 . H101 . 109.8 no C9 . C10 . H102 . 107.4 no C11 . C10 . H102 . 107.0 no H101 . C10 . H102 . 109.0 no C10 . C11 . C12 . 115.4(6) yes C10 . C11 . H111 . 106.3 no C12 . C11 . H111 . 107.5 no C10 . C11 . H112 . 108.5 no C12 . C11 . H112 . 109.7 no H111 . C11 . H112 . 109.2 no C11 . C12 . H121 . 110.1 no C11 . C12 . H122 . 110.2 no H121 . C12 . H122 . 109.3 no C11 . C12 . H123 . 109.2 no H121 . C12 . H123 . 109.3 no H122 . C12 . H123 . 108.7 no N3 . C13 . C14 . 116.0(4) yes N3 . C13 . H131 . 109.4 no C14 . C13 . H131 . 106.8 no N3 . C13 . H132 . 108.1 no C14 . C13 . H132 . 106.8 no H131 . C13 . H132 . 109.5 no C13 . C14 . C15 . 113.9(6) yes C13 . C14 . H141 . 110.8 no C15 . C14 . H141 . 106.9 no C13 . C14 . H142 . 107.1 no C15 . C14 . H142 . 108.0 no H141 . C14 . H142 . 110.1 no C14 . C15 . C16 . 119.1(10) yes C14 . C15 . H151 . 108.3 no C16 . C15 . H151 . 110.6 no C14 . C15 . H152 . 105.5 no C16 . C15 . H152 . 103.4 no H151 . C15 . H152 . 109.5 no C15 . C16 . H161 . 110.3 no C15 . C16 . H162 . 105.4 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 112.6 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no Au1 . C17 . N1 . 173.4(5) yes