Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_publication_text _publ_requested_journal 'Dalton Trans.' _publ_contact_author_name 'Howard Patterson' _publ_contact_author_address ; Department of Chemistry University of Maine Orono, Maine 04469 ; _publ_contact_author_email Howard_Patterson@umit.maine.edu _publ_contact_author_phone 207-581-1178 loop_ _publ_author_name _publ_author_address 'Patterson, Howard' ;Department of Chemistry University of Maine Orono, Maine 04469 ; 'Larochelle, Christie' ;Department of Chemistry University of Maine Orono, Maine 04469 ; 'Colis, Julie C.F.' ;Department of Chemistry University of Maine Orono, Maine 04469 ; 'Staples, Richard' ;Department of Chemistry and Chemical Biology Harvard University Cambridge, MA 02138 ; 'Herst-Irmer, Regina' ;Department of Structural Chemistry University of Gottingen Tammannstr 4, Germany ; data_hp3r _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Ag3 La N6 O3' _chemical_formula_weight 672.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 63/m c m' _symmetry_Int_Tables_number 193 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 6.717(2) _cell_length_b 6.717(2) _cell_length_c 18.951(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 740.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4362 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 23.27 _exptl_crystal_description block_cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 6.744 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.559403 _exptl_absorpt_correction_T_max 0.914451 _exptl_absorpt_process_details SADABS _exptl_special_details ; Data was collected using a BRUKER SMART CCD (charge coupled device) based diffractometer equipped with an LT-2 low-temperature apparatus operating at 213 K. A suitable crystal was chosen and mounted on a glass fiber using grease. Data were measured using omega scans of 0.3\% per frame for 10 s , such that a sphere was collected. A total of 2850 frames were collected with a final resolution of 0.75 \%A. The first 50 frames were recollected at the end of data collection to monitor for decay. Cell parameters were retrieved using SMART software and refined using SAINT on all observed reflections. Data reduction was performed using the SAINT software which corrects for Lp and decay. Absorption corrections were applied using SADABS based on Blessing, (1995). The structures are solved by the direct method using the SHELX-90 program and refined by least squares method on F2 SHELXL-93, incorporated in SHELXTL V5.1. Oxygen-bound H atoms were placed in idealized positions and refined as a riding model. O-H = 0.83A and Uiso(H) = 1.2Ueq(O). ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD' _diffrn_measurement_method '\w, 0.3 deg' _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13376 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0072 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.29 _reflns_number_total 364 _reflns_number_gt 361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (BRUKER, V5.007, 1997)' _computing_cell_refinement 'SMART (BRUKER, V5.054, 1998)' _computing_data_reduction 'SAINT (BRUKER, V6.01, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (BRUKER, 1998, V5.1)' _computing_publication_material 'XCIF (Sheldrick and BRUKER, 1997, V5.1)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+1.6378P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 364 _refine_ls_number_parameters 23 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0177 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0417 _refine_ls_wR_factor_gt 0.0415 _refine_ls_goodness_of_fit_ref 1.297 _refine_ls_restrained_S_all 1.297 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.0000 0.0000 0.2500 0.01233(13) Uani 1 12 d S . . Ag1 Ag 0.5000 0.5000 0.0000 0.03120(14) Uani 1 4 d S . . N1 N 0.2708(5) 0.2708(5) 0.14807(15) 0.0259(6) Uani 1 2 d S . . C1 C 0.3515(6) 0.3515(6) 0.09501(17) 0.0240(7) Uani 1 2 d S . . O1 O 0.3765(6) 0.0000 0.2500 0.0403(11) Uani 1 4 d S . . H1 H 0.4177 0.0000 0.2087 0.048 Uiso 1 2 calc SR . . 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 La1 0.01451(15) 0.01451(15) 0.00795(19) 0.000 0.000 0.00726(8) Ag1 0.0368(2) 0.0368(2) 0.01995(19) 0.01278(14) 0.01278(14) 0.01843(19) N1 0.0256(11) 0.0256(11) 0.0220(13) 0.0044(10) 0.0044(10) 0.0094(14) C1 0.0233(12) 0.0233(12) 0.0222(14) 0.0028(12) 0.0028(12) 0.0092(14) O1 0.0329(15) 0.088(4) 0.0183(15) 0.000 0.000 0.0441(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.529(4) 3 ? La1 O1 2.529(4) 2 ? La1 O1 2.529(4) . ? La1 N1 2.653(3) 16_556 ? La1 N1 2.653(3) 2 ? La1 N1 2.653(3) 3 ? La1 N1 2.653(3) 17_556 ? La1 N1 2.653(3) 18_556 ? La1 N1 2.653(3) . ? Ag1 C1 2.058(3) . ? Ag1 C1 2.058(3) 13_665 ? Ag1 Ag1 3.3585(10) 2_655 ? Ag1 Ag1 3.3585(10) 2_665 ? Ag1 Ag1 3.3585(10) 3_565 ? Ag1 Ag1 3.3585(10) 3_665 ? N1 C1 1.142(4) . ? O1 H1 0.8300 . ? 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 O1 La1 O1 120.0 3 2 ? O1 La1 O1 120.0 3 . ? O1 La1 O1 120.000(1) 2 . ? O1 La1 N1 133.28(7) 3 16_556 ? O1 La1 N1 69.95(3) 2 16_556 ? O1 La1 N1 69.95(3) . 16_556 ? O1 La1 N1 69.95(3) 3 2 ? O1 La1 N1 69.95(3) 2 2 ? O1 La1 N1 133.28(7) . 2 ? N1 La1 N1 139.91(5) 16_556 2 ? O1 La1 N1 69.95(3) 3 3 ? O1 La1 N1 133.28(7) 2 3 ? O1 La1 N1 69.95(3) . 3 ? N1 La1 N1 139.91(5) 16_556 3 ? N1 La1 N1 72.84(10) 2 3 ? O1 La1 N1 69.95(3) 3 17_556 ? O1 La1 N1 69.95(3) 2 17_556 ? O1 La1 N1 133.28(7) . 17_556 ? N1 La1 N1 72.84(10) 16_556 17_556 ? N1 La1 N1 93.45(13) 2 17_556 ? N1 La1 N1 139.91(5) 3 17_556 ? O1 La1 N1 69.95(3) 3 18_556 ? O1 La1 N1 133.28(7) 2 18_556 ? O1 La1 N1 69.95(3) . 18_556 ? N1 La1 N1 72.84(10) 16_556 18_556 ? N1 La1 N1 139.91(5) 2 18_556 ? N1 La1 N1 93.45(13) 3 18_556 ? N1 La1 N1 72.84(10) 17_556 18_556 ? O1 La1 N1 133.28(7) 3 . ? O1 La1 N1 69.95(3) 2 . ? O1 La1 N1 69.95(3) . . ? N1 La1 N1 93.45(13) 16_556 . ? N1 La1 N1 72.84(10) 2 . ? N1 La1 N1 72.84(10) 3 . ? N1 La1 N1 139.91(5) 17_556 . ? N1 La1 N1 139.91(5) 18_556 . ? C1 Ag1 C1 180.0(2) . 13_665 ? C1 Ag1 Ag1 75.98(5) . 2_655 ? C1 Ag1 Ag1 104.02(5) 13_665 2_655 ? C1 Ag1 Ag1 104.02(5) . 2_665 ? C1 Ag1 Ag1 75.98(5) 13_665 2_665 ? Ag1 Ag1 Ag1 180.0 2_655 2_665 ? C1 Ag1 Ag1 75.98(5) . 3_565 ? C1 Ag1 Ag1 104.02(5) 13_665 3_565 ? Ag1 Ag1 Ag1 120.0 2_655 3_565 ? Ag1 Ag1 Ag1 60.0 2_665 3_565 ? C1 Ag1 Ag1 104.02(5) . 3_665 ? C1 Ag1 Ag1 75.98(5) 13_665 3_665 ? Ag1 Ag1 Ag1 60.0 2_655 3_665 ? Ag1 Ag1 Ag1 120.0 2_665 3_665 ? Ag1 Ag1 Ag1 180.0 3_565 3_665 ? C1 N1 La1 165.1(3) . . ? N1 C1 Ag1 179.3(4) . . ? La1 O1 H1 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 La1 N1 C1 0.000(1) 3 . . . ? O1 La1 N1 C1 -112.80(2) 2 . . . ? O1 La1 N1 C1 112.80(2) . . . . ? N1 La1 N1 C1 180.000(1) 16_556 . . . ? N1 La1 N1 C1 -38.41(3) 2 . . . ? N1 La1 N1 C1 38.42(3) 3 . . . ? N1 La1 N1 C1 -112.80(2) 17_556 . . . ? N1 La1 N1 C1 112.80(2) 18_556 . . . ? La1 N1 C1 Ag1 180(4) . . . . ? C1 Ag1 C1 N1 0(100) 13_665 . . . ? Ag1 Ag1 C1 N1 116.79(4) 2_655 . . . ? Ag1 Ag1 C1 N1 -63.21(4) 2_665 . . . ? Ag1 Ag1 C1 N1 -116.80(2) 3_565 . . . ? Ag1 Ag1 C1 N1 63.20(2) 3_665 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.466 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.088 data_hp10t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Ag2.50 Au0.50 La N6 O3' _chemical_formula_weight 717.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P63/mcm _symmetry_Int_Tables_number 193 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 6.692(2) _cell_length_b 6.692(2) _cell_length_c 18.943(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 734.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 236 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.46 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 11.117 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5197 _exptl_absorpt_correction_T_max 0.5197 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w, 0.3 deg' _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4196 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.25 _reflns_number_total 362 _reflns_number_gt 358 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (BRUKER, V5.007, 1997)' _computing_cell_refinement 'SMART (BRUKER, V5.054, 1998)' _computing_data_reduction 'SAINT (BRUKER, V6.01, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (BRUKER, 1998, V5.1)' _computing_publication_material 'XCIF (Sheldrick and BRUKER, 1997, V5.1)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+5.3451P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 362 _refine_ls_number_parameters 26 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0556 _refine_ls_goodness_of_fit_ref 1.534 _refine_ls_restrained_S_all 1.534 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.0000 0.0000 0.2500 0.0106(3) Uani 1 12 d S . . Ag1 Ag 0.5000 0.5000 0.0000 0.0251(2) Uani 0.833(8) 4 d SP . 1 Au1 Au 0.5000 0.5000 0.0000 0.0251(2) Uani 0.167(8) 4 d SP . 2 N1 N 0.2726(10) 0.2726(10) 0.1480(3) 0.0238(15) Uani 1 2 d S . . C1 C 0.3525(12) 0.3525(12) 0.0945(4) 0.0212(16) Uani 1 2 d S . . O1 O 0.3777(12) 0.0000 0.2500 0.037(3) Uani 1 4 d S . . H1 H 0.433(14) 0.0000 0.206(5) 0.045 Uiso 1 2 d S . . 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 La1 0.0124(3) 0.0124(3) 0.0072(4) 0.000 0.000 0.00618(16) Ag1 0.0290(3) 0.0290(3) 0.0161(3) 0.0105(3) 0.0105(3) 0.0138(3) Au1 0.0290(3) 0.0290(3) 0.0161(3) 0.0105(3) 0.0105(3) 0.0138(3) N1 0.023(3) 0.023(3) 0.019(3) 0.004(2) 0.004(2) 0.006(3) C1 0.020(3) 0.020(3) 0.022(3) 0.003(3) 0.003(3) 0.008(3) O1 0.029(3) 0.083(8) 0.018(4) 0.000 0.000 0.041(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.528(8) 3 ? La1 O1 2.528(8) 2 ? La1 O1 2.528(8) . ? La1 N1 2.657(6) 16_556 ? La1 N1 2.657(6) 2 ? La1 N1 2.657(6) 3 ? La1 N1 2.657(6) 17_556 ? La1 N1 2.657(6) . ? La1 N1 2.657(6) 18_556 ? Ag1 C1 2.044(7) 13_665 ? Ag1 C1 2.044(7) . ? Ag1 Ag1 3.3460(10) 2_655 ? Ag1 Ag1 3.3460(10) 2_665 ? Ag1 Ag1 3.3460(10) 3_565 ? Ag1 Ag1 3.3460(10) 3_665 ? Au1 C1 2.044(7) 13_665 ? Au1 C1 2.044(7) . ? Au1 Au1 3.3460(10) 2_655 ? Au1 Au1 3.3460(10) 2_665 ? Au1 Au1 3.3460(10) 3_565 ? Au1 Au1 3.3460(10) 3_665 ? N1 C1 1.146(10) . ? O1 H1 0.92(9) . ? 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 O1 La1 O1 120.000(1) 3 2 ? O1 La1 O1 120.000(1) 3 . ? O1 La1 O1 120.000(2) 2 . ? O1 La1 N1 133.37(14) 3 16_556 ? O1 La1 N1 69.92(5) 2 16_556 ? O1 La1 N1 69.92(5) . 16_556 ? O1 La1 N1 69.92(6) 3 2 ? O1 La1 N1 69.92(5) 2 2 ? O1 La1 N1 133.37(14) . 2 ? N1 La1 N1 139.84(11) 16_556 2 ? O1 La1 N1 69.92(6) 3 3 ? O1 La1 N1 133.37(14) 2 3 ? O1 La1 N1 69.92(5) . 3 ? N1 La1 N1 139.84(11) 16_556 3 ? N1 La1 N1 73.0(2) 2 3 ? O1 La1 N1 69.92(6) 3 17_556 ? O1 La1 N1 69.92(5) 2 17_556 ? O1 La1 N1 133.37(14) . 17_556 ? N1 La1 N1 73.0(2) 16_556 17_556 ? N1 La1 N1 93.3(3) 2 17_556 ? N1 La1 N1 139.84(11) 3 17_556 ? O1 La1 N1 133.37(14) 3 . ? O1 La1 N1 69.92(5) 2 . ? O1 La1 N1 69.92(5) . . ? N1 La1 N1 93.3(3) 16_556 . ? N1 La1 N1 73.0(2) 2 . ? N1 La1 N1 73.0(2) 3 . ? N1 La1 N1 139.84(11) 17_556 . ? O1 La1 N1 69.92(6) 3 18_556 ? O1 La1 N1 133.37(14) 2 18_556 ? O1 La1 N1 69.92(5) . 18_556 ? N1 La1 N1 73.0(2) 16_556 18_556 ? N1 La1 N1 139.84(11) 2 18_556 ? N1 La1 N1 93.3(3) 3 18_556 ? N1 La1 N1 73.0(2) 17_556 18_556 ? N1 La1 N1 139.84(11) . 18_556 ? C1 Ag1 C1 180.0(4) 13_665 . ? C1 Ag1 Ag1 103.97(10) 13_665 2_655 ? C1 Ag1 Ag1 76.03(10) . 2_655 ? C1 Ag1 Ag1 76.03(10) 13_665 2_665 ? C1 Ag1 Ag1 103.97(10) . 2_665 ? Ag1 Ag1 Ag1 180.0 2_655 2_665 ? C1 Ag1 Ag1 103.97(10) 13_665 3_565 ? C1 Ag1 Ag1 76.03(10) . 3_565 ? Ag1 Ag1 Ag1 120.0 2_655 3_565 ? Ag1 Ag1 Ag1 60.0 2_665 3_565 ? C1 Ag1 Ag1 76.03(10) 13_665 3_665 ? C1 Ag1 Ag1 103.97(10) . 3_665 ? Ag1 Ag1 Ag1 60.0 2_655 3_665 ? Ag1 Ag1 Ag1 120.0 2_665 3_665 ? Ag1 Ag1 Ag1 180.0 3_565 3_665 ? C1 Au1 C1 180.0(4) 13_665 . ? C1 Au1 Au1 103.97(10) 13_665 2_655 ? C1 Au1 Au1 76.03(10) . 2_655 ? C1 Au1 Au1 76.03(10) 13_665 2_665 ? C1 Au1 Au1 103.97(10) . 2_665 ? Au1 Au1 Au1 180.0 2_655 2_665 ? C1 Au1 Au1 103.97(10) 13_665 3_565 ? C1 Au1 Au1 76.03(10) . 3_565 ? Au1 Au1 Au1 120.0 2_655 3_565 ? Au1 Au1 Au1 60.0 2_665 3_565 ? C1 Au1 Au1 76.03(10) 13_665 3_665 ? C1 Au1 Au1 103.97(10) . 3_665 ? Au1 Au1 Au1 60.0 2_655 3_665 ? Au1 Au1 Au1 120.0 2_665 3_665 ? Au1 Au1 Au1 180.0 3_565 3_665 ? C1 N1 La1 164.4(6) . . ? N1 C1 Ag1 178.9(8) . . ? N1 C1 Au1 178.9(8) . . ? Ag1 C1 Au1 0.0 . . ? La1 O1 H1 114(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 La1 N1 C1 0.000(2) 3 . . . ? O1 La1 N1 C1 -112.77(5) 2 . . . ? O1 La1 N1 C1 112.77(5) . . . . ? N1 La1 N1 C1 180.000(2) 16_556 . . . ? N1 La1 N1 C1 -38.46(6) 2 . . . ? N1 La1 N1 C1 38.46(6) 3 . . . ? N1 La1 N1 C1 -112.77(5) 17_556 . . . ? N1 La1 N1 C1 112.77(5) 18_556 . . . ? La1 N1 C1 Ag1 180(3) . . . . ? La1 N1 C1 Au1 180(3) . . . . ? C1 Ag1 C1 N1 0(100) 13_665 . . . ? Ag1 Ag1 C1 N1 116.82(7) 2_655 . . . ? Ag1 Ag1 C1 N1 -63.18(7) 2_665 . . . ? Ag1 Ag1 C1 N1 -116.82(4) 3_565 . . . ? Ag1 Ag1 C1 N1 63.18(4) 3_665 . . . ? C1 Ag1 C1 Au1 0(100) 13_665 . . . ? Ag1 Ag1 C1 Au1 0(100) 2_655 . . . ? Ag1 Ag1 C1 Au1 0(100) 2_665 . . . ? Ag1 Ag1 C1 Au1 0(100) 3_565 . . . ? Ag1 Ag1 C1 Au1 0(48) 3_665 . . . ? C1 Au1 C1 N1 0(100) 13_665 . . . ? Au1 Au1 C1 N1 116.82(7) 2_655 . . . ? Au1 Au1 C1 N1 -63.18(7) 2_665 . . . ? Au1 Au1 C1 N1 -116.82(4) 3_565 . . . ? Au1 Au1 C1 N1 63.18(4) 3_665 . . . ? C1 Au1 C1 Ag1 0(100) 13_665 . . . ? Au1 Au1 C1 Ag1 0(100) 2_655 . . . ? Au1 Au1 C1 Ag1 0(100) 2_665 . . . ? Au1 Au1 C1 Ag1 0(100) 3_565 . . . ? Au1 Au1 C1 Ag1 0(48) 3_665 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.058 _refine_diff_density_min -1.282 _refine_diff_density_rms 0.139 data_hp1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Ag Au2 La N6 O3' _chemical_formula_weight 850.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P63/mcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 6.664(4) _cell_length_b 6.664(4) _cell_length_c 18.871(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 725.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 230 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.78 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 24.375 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.1942 _exptl_absorpt_correction_T_max 0.3225 _exptl_absorpt_process_details SADABS _exptl_special_details ; Data was collected using a BRUKER SMART CCD (charge coupled device) based diffractometer equipped with an LT-2 low-temperature apparatus operating at 213 K. A suitable crystal was chosen and mounted on a glass fiber using grease. Data were measured using omega scans of 0.3\% per frame for 30 s , such that a hemisphere was collected. A total of 1271 frames were collected with a final resolution of 0.75 \%A. The first 50 frames were recollected at the end of data collection to monitor for decay. Cell parameters were retrieved using SMART software and refined using SAINT on all observed reflections. Data reduction was performed using the SAINT software which corrects for Lp and decay. Absorption corrections were applied using SADABS based on Blessing, (1995). The structures are solved by the direct method using the SHELX-90 program and refined by least squares method on F2 SHELXL-93, incorporated in SHELXTL V5.1. Carbon-bound H atoms were placed in idealized positions and refined as a riding model. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w, 0.3 deg' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4178 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.47 _reflns_number_total 363 _reflns_number_gt 349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (BRUKER, V5.007, 1997)' _computing_cell_refinement 'SMART (BRUKER, V5.054, 1998)' _computing_data_reduction 'SAINT (BRUKER, V6.01, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (BRUKER, 1998, V5.1)' _computing_publication_material 'XCIF (Sheldrick and BRUKER, 1997, V5.1)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+14.7550P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 363 _refine_ls_number_parameters 28 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.429 _refine_ls_restrained_S_all 1.427 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.0000 -1.0000 0.2500 0.0103(5) Uani 1 12 d S . . O1 O 0.3826(19) -0.6174(19) 0.2500 0.028(3) Uani 1 4 d SD . . H1 H 0.44(4) -0.56(4) 0.212(7) 0.13(12) Uiso 1 2 d SD . . Au1 Au 0.0000 -0.5000 0.0000 0.0216(3) Uani 0.616(16) 4 d SP . 1 Ag1 Ag 0.0000 -0.5000 0.0000 0.0216(3) Uani 0.384(16) 4 d SP . 2 C1 C 0.0000 -0.6473(19) 0.0947(5) 0.016(2) Uani 1 2 d S . . N1 N 0.0000 -0.7228(15) 0.1477(5) 0.018(2) Uani 1 2 d S . . 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 La1 0.0113(6) 0.0113(6) 0.0084(7) 0.000 0.000 0.0057(3) O1 0.020(5) 0.020(5) 0.016(6) 0.000 0.000 -0.010(5) Au1 0.0259(5) 0.0244(4) 0.0150(4) 0.0061(3) 0.000 0.0129(2) Ag1 0.0259(5) 0.0244(4) 0.0150(4) 0.0061(3) 0.000 0.0129(2) C1 0.008(5) 0.020(4) 0.015(4) 0.002(4) 0.000 0.004(2) N1 0.019(5) 0.017(4) 0.019(5) 0.002(3) 0.000 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.550(13) . ? La1 O1 2.550(13) 3_645 ? La1 O1 2.550(13) 2_435 ? La1 N1 2.672(10) 2_435 ? La1 N1 2.672(10) 18_646 ? La1 N1 2.672(10) 16_556 ? La1 N1 2.672(10) 17_436 ? La1 N1 2.672(10) . ? La1 N1 2.672(10) 3_645 ? O1 H1 0.80(2) . ? Au1 C1 2.039(11) 13_545 ? Au1 C1 2.039(11) . ? Au1 Au1 3.3320(19) 3_655 ? Au1 Au1 3.3320(19) 3_545 ? Au1 Au1 3.3319(19) 2_445 ? Au1 Au1 3.3319(19) 2_545 ? Ag1 C1 2.039(11) 13_545 ? Ag1 C1 2.039(11) . ? Ag1 Ag1 3.3320(19) 3_655 ? Ag1 Ag1 3.3320(19) 3_545 ? Ag1 Ag1 3.3319(19) 2_445 ? Ag1 Ag1 3.3319(19) 2_545 ? C1 N1 1.120(15) . ? 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 O1 La1 O1 120.0 . 3_645 ? O1 La1 O1 120.000(1) . 2_435 ? O1 La1 O1 120.000(1) 3_645 2_435 ? O1 La1 N1 133.7(2) . 2_435 ? O1 La1 N1 69.78(8) 3_645 2_435 ? O1 La1 N1 69.78(8) 2_435 2_435 ? O1 La1 N1 69.78(8) . 18_646 ? O1 La1 N1 69.78(8) 3_645 18_646 ? O1 La1 N1 133.7(2) 2_435 18_646 ? N1 La1 N1 139.56(17) 2_435 18_646 ? O1 La1 N1 69.78(8) . 16_556 ? O1 La1 N1 133.7(2) 3_645 16_556 ? O1 La1 N1 69.78(8) 2_435 16_556 ? N1 La1 N1 139.56(17) 2_435 16_556 ? N1 La1 N1 73.5(3) 18_646 16_556 ? O1 La1 N1 133.7(2) . 17_436 ? O1 La1 N1 69.78(8) 3_645 17_436 ? O1 La1 N1 69.78(8) 2_435 17_436 ? N1 La1 N1 92.5(4) 2_435 17_436 ? N1 La1 N1 73.5(3) 18_646 17_436 ? N1 La1 N1 73.5(3) 16_556 17_436 ? O1 La1 N1 69.78(8) . . ? O1 La1 N1 133.7(2) 3_645 . ? O1 La1 N1 69.78(8) 2_435 . ? N1 La1 N1 73.5(3) 2_435 . ? N1 La1 N1 139.56(17) 18_646 . ? N1 La1 N1 92.5(4) 16_556 . ? N1 La1 N1 139.56(17) 17_436 . ? O1 La1 N1 69.78(8) . 3_645 ? O1 La1 N1 69.78(8) 3_645 3_645 ? O1 La1 N1 133.7(2) 2_435 3_645 ? N1 La1 N1 73.5(3) 2_435 3_645 ? N1 La1 N1 92.5(4) 18_646 3_645 ? N1 La1 N1 139.56(17) 16_556 3_645 ? N1 La1 N1 139.56(17) 17_436 3_645 ? N1 La1 N1 73.5(3) . 3_645 ? H1 O1 La1 117(10) . . ? C1 Au1 C1 180.0(7) 13_545 . ? C1 Au1 Au1 76.07(16) 13_545 3_655 ? C1 Au1 Au1 103.93(16) . 3_655 ? C1 Au1 Au1 103.93(16) 13_545 3_545 ? C1 Au1 Au1 76.07(16) . 3_545 ? Au1 Au1 Au1 180.0 3_655 3_545 ? C1 Au1 Au1 76.07(16) 13_545 2_445 ? C1 Au1 Au1 103.93(16) . 2_445 ? Au1 Au1 Au1 120.0 3_655 2_445 ? Au1 Au1 Au1 60.0 3_545 2_445 ? C1 Au1 Au1 103.93(16) 13_545 2_545 ? C1 Au1 Au1 76.07(16) . 2_545 ? Au1 Au1 Au1 60.0 3_655 2_545 ? Au1 Au1 Au1 120.0 3_545 2_545 ? Au1 Au1 Au1 180.0 2_445 2_545 ? C1 Ag1 C1 180.0(7) 13_545 . ? C1 Ag1 Ag1 76.07(16) 13_545 3_655 ? C1 Ag1 Ag1 103.93(16) . 3_655 ? C1 Ag1 Ag1 103.93(16) 13_545 3_545 ? C1 Ag1 Ag1 76.07(16) . 3_545 ? Ag1 Ag1 Ag1 180.0 3_655 3_545 ? C1 Ag1 Ag1 76.07(16) 13_545 2_445 ? C1 Ag1 Ag1 103.93(16) . 2_445 ? Ag1 Ag1 Ag1 120.0 3_655 2_445 ? Ag1 Ag1 Ag1 60.0 3_545 2_445 ? C1 Ag1 Ag1 103.93(16) 13_545 2_545 ? C1 Ag1 Ag1 76.07(16) . 2_545 ? Ag1 Ag1 Ag1 60.0 3_655 2_545 ? Ag1 Ag1 Ag1 120.0 3_545 2_545 ? Ag1 Ag1 Ag1 180.0 2_445 2_545 ? N1 C1 Au1 177.9(11) . . ? N1 C1 Ag1 177.9(11) . . ? Au1 C1 Ag1 0.0 . . ? C1 N1 La1 163.0(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 La1 O1 H1 90.000(4) 3_645 . . . ? O1 La1 O1 H1 -90.000(4) 2_435 . . . ? N1 La1 O1 H1 0.000(5) 2_435 . . . ? N1 La1 O1 H1 140.4(2) 18_646 . . . ? N1 La1 O1 H1 -140.4(2) 16_556 . . . ? N1 La1 O1 H1 180.000(4) 17_436 . . . ? N1 La1 O1 H1 -39.6(2) . . . . ? N1 La1 O1 H1 39.6(2) 3_645 . . . ? C1 Au1 C1 N1 117(100) 13_545 . . . ? Au1 Au1 C1 N1 63.16(10) 3_655 . . . ? Au1 Au1 C1 N1 -116.84(10) 3_545 . . . ? Au1 Au1 C1 N1 -63.16(10) 2_445 . . . ? Au1 Au1 C1 N1 116.84(10) 2_545 . . . ? C1 Au1 C1 Ag1 0(100) 13_545 . . . ? Au1 Au1 C1 Ag1 0(100) 3_655 . . . ? Au1 Au1 C1 Ag1 0(100) 3_545 . . . ? Au1 Au1 C1 Ag1 0(100) 2_445 . . . ? Au1 Au1 C1 Ag1 0(100) 2_545 . . . ? C1 Ag1 C1 N1 117(100) 13_545 . . . ? Ag1 Ag1 C1 N1 63.16(10) 3_655 . . . ? Ag1 Ag1 C1 N1 -116.84(10) 3_545 . . . ? Ag1 Ag1 C1 N1 -63.16(10) 2_445 . . . ? Ag1 Ag1 C1 N1 116.84(10) 2_545 . . . ? C1 Ag1 C1 Au1 0(100) 13_545 . . . ? Ag1 Ag1 C1 Au1 0(100) 3_655 . . . ? Ag1 Ag1 C1 Au1 0(100) 3_545 . . . ? Ag1 Ag1 C1 Au1 0(100) 2_445 . . . ? Ag1 Ag1 C1 Au1 0(100) 2_545 . . . ? Au1 C1 N1 La1 180.00(2) . . . . ? Ag1 C1 N1 La1 180.00(2) . . . . ? O1 La1 N1 C1 112.65(7) . . . . ? O1 La1 N1 C1 0.000(3) 3_645 . . . ? O1 La1 N1 C1 -112.65(7) 2_435 . . . ? N1 La1 N1 C1 -38.62(10) 2_435 . . . ? N1 La1 N1 C1 112.65(7) 18_646 . . . ? N1 La1 N1 C1 180.000(3) 16_556 . . . ? N1 La1 N1 C1 -112.65(7) 17_436 . . . ? N1 La1 N1 C1 38.62(10) 3_645 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N1 0.80(2) 2.26(13) 2.978(14) 150(25) 2_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.775 _refine_diff_density_min -1.266 _refine_diff_density_rms 0.196 data_hp4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Au3 La N6 O3' _chemical_formula_weight 939.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P63/mcm _symmetry_Int_Tables_number 193 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 6.664(2) _cell_length_b 6.664(2) _cell_length_c 18.741(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 720.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Chunk _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 33.350 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.7435 _exptl_absorpt_correction_T_max 0.9456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w, 0.3 deg' _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6508 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0124 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.23 _reflns_number_total 359 _reflns_number_gt 345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (BRUKER, V5.007, 1997)' _computing_cell_refinement 'SMART (BRUKER, V5.054, 1998)' _computing_data_reduction 'SAINT (BRUKER, V6.01, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (BRUKER, 1998, V5.1)' _computing_publication_material 'XCIF (Sheldrick and BRUKER, 1997, V5.1)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+60.7368P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0.0064(11) _refine_ls_number_reflns 359 _refine_ls_number_parameters 25 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.327 _refine_ls_restrained_S_all 1.301 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.0000 0.0000 0.2500 0.0122(5) Uani 1 12 d SU . . Au1 Au 0.5000 0.5000 0.0000 0.0170(3) Uani 1 4 d SU . . N1 N 0.277(2) 0.277(2) 0.1474(7) 0.015(3) Uani 1 2 d SU . . C1 C 0.357(3) 0.357(3) 0.0934(7) 0.007(3) Uani 1 2 d SU . . O1 O 0.374(3) 0.0000 0.2500 0.023(5) Uani 1 4 d SDU . . H1 H 0.449(6) 0.0000 0.2900(5) 0.028 Uiso 1 2 d SD . . 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 La1 0.0143(7) 0.0143(7) 0.0079(9) 0.000 0.000 0.0071(4) Au1 0.0194(4) 0.0194(4) 0.0100(3) 0.0069(3) 0.0069(3) 0.0080(4) N1 0.017(6) 0.017(6) 0.009(5) 0.004(4) 0.004(4) 0.007(7) C1 0.010(6) 0.010(6) 0.005(5) -0.001(4) -0.001(4) 0.008(6) O1 0.019(6) 0.058(14) 0.005(6) 0.000 0.000 0.029(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.496(19) 3 ? La1 O1 2.496(19) 2 ? La1 O1 2.496(19) . ? La1 N1 2.664(14) 16_556 ? La1 N1 2.664(14) 2 ? La1 N1 2.664(14) 3 ? La1 N1 2.664(14) . ? La1 N1 2.664(14) 17_556 ? La1 N1 2.664(14) 18_556 ? Au1 C1 1.994(14) . ? Au1 C1 1.994(14) 13_665 ? Au1 Au1 3.3320(10) 2_655 ? Au1 Au1 3.3320(10) 2_665 ? Au1 Au1 3.3320(10) 3_565 ? Au1 Au1 3.3320(10) 3_665 ? N1 C1 1.14(2) . ? O1 H1 0.90(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 O1 La1 O1 120.000(2) 3 2 ? O1 La1 O1 120.000(2) 3 . ? O1 La1 O1 120.000(5) 2 . ? O1 La1 N1 133.8(3) 3 16_556 ? O1 La1 N1 69.76(12) 2 16_556 ? O1 La1 N1 69.76(12) . 16_556 ? O1 La1 N1 69.76(12) 3 2 ? O1 La1 N1 69.76(12) 2 2 ? O1 La1 N1 133.8(3) . 2 ? N1 La1 N1 139.5(2) 16_556 2 ? O1 La1 N1 69.76(13) 3 3 ? O1 La1 N1 133.8(3) 2 3 ? O1 La1 N1 69.76(12) . 3 ? N1 La1 N1 139.5(2) 16_556 3 ? N1 La1 N1 73.6(5) 2 3 ? O1 La1 N1 133.8(3) 3 . ? O1 La1 N1 69.76(12) 2 . ? O1 La1 N1 69.76(12) . . ? N1 La1 N1 92.4(6) 16_556 . ? N1 La1 N1 73.6(5) 2 . ? N1 La1 N1 73.6(5) 3 . ? O1 La1 N1 69.76(12) 3 17_556 ? O1 La1 N1 69.76(12) 2 17_556 ? O1 La1 N1 133.8(3) . 17_556 ? N1 La1 N1 73.6(5) 16_556 17_556 ? N1 La1 N1 92.4(6) 2 17_556 ? N1 La1 N1 139.5(3) 3 17_556 ? N1 La1 N1 139.5(2) . 17_556 ? O1 La1 N1 69.76(12) 3 18_556 ? O1 La1 N1 133.8(3) 2 18_556 ? O1 La1 N1 69.76(12) . 18_556 ? N1 La1 N1 73.6(5) 16_556 18_556 ? N1 La1 N1 139.5(3) 2 18_556 ? N1 La1 N1 92.4(6) 3 18_556 ? N1 La1 N1 139.5(2) . 18_556 ? N1 La1 N1 73.6(5) 17_556 18_556 ? C1 Au1 C1 180.0(11) . 13_665 ? C1 Au1 Au1 76.2(2) . 2_655 ? C1 Au1 Au1 103.8(2) 13_665 2_655 ? C1 Au1 Au1 103.8(2) . 2_665 ? C1 Au1 Au1 76.2(2) 13_665 2_665 ? Au1 Au1 Au1 180.0 2_655 2_665 ? C1 Au1 Au1 76.2(2) . 3_565 ? C1 Au1 Au1 103.8(2) 13_665 3_565 ? Au1 Au1 Au1 120.0 2_655 3_565 ? Au1 Au1 Au1 60.0 2_665 3_565 ? C1 Au1 Au1 103.8(2) . 3_665 ? C1 Au1 Au1 76.2(2) 13_665 3_665 ? Au1 Au1 Au1 60.0 2_655 3_665 ? Au1 Au1 Au1 120.0 2_665 3_665 ? Au1 Au1 Au1 180.0 3_565 3_665 ? C1 N1 La1 164.1(14) . . ? N1 C1 Au1 179.3(18) . . ? La1 O1 H1 124(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 La1 N1 C1 0.000(4) 3 . . . ? O1 La1 N1 C1 -112.63(11) 2 . . . ? O1 La1 N1 C1 112.63(11) . . . . ? N1 La1 N1 C1 180.000(4) 16_556 . . . ? N1 La1 N1 C1 -38.65(15) 2 . . . ? N1 La1 N1 C1 38.65(15) 3 . . . ? N1 La1 N1 C1 -112.63(11) 17_556 . . . ? N1 La1 N1 C1 112.63(11) 18_556 . . . ? La1 N1 C1 Au1 180(17) . . . . ? C1 Au1 C1 N1 -117(100) 13_665 . . . ? Au1 Au1 C1 N1 116.9(2) 2_655 . . . ? Au1 Au1 C1 N1 -63.1(2) 2_665 . . . ? Au1 Au1 C1 N1 -116.89(8) 3_565 . . . ? Au1 Au1 C1 N1 63.11(8) 3_665 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.978 _refine_diff_density_min -9.213 _refine_diff_density_rms 0.361