# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Philip Coppens' 'Marc Messerschmidt' 'Cara L. Nygren' 'Shao-Liang Zheng.' _publ_contact_author_name 'Philip Coppens' _publ_contact_author_address ; Department of Chemistry State University of New York at Buffalo Buffalo New York 14260-3000 UNITED STATES OF AMERICA ; _publ_contact_author_email COPPENS@ACSU.BUFFALO.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Ligand-unsupported Au(I) Chains with Short Au(I)...Au(I) Contacts ; data_Au(NH3)2ClO4 _database_code_depnum_ccdc_archive 'CCDC 607983' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Au(NH3)2ClO4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H6 Au Cl N2 O4' _chemical_formula_weight 330.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 14.769(3) _cell_length_b 5.9797(13) _cell_length_c 7.7564(17) _cell_angle_alpha 90.00 _cell_angle_beta 115.824(4) _cell_angle_gamma 90.00 _cell_volume 616.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 282 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 24.231 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.3242 _exptl_absorpt_correction_T_max 0.6429 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5521 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 30.59 _reflns_number_total 1019 _reflns_number_gt 953 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0111P)^2^+4.6875P] 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 0.0033(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1019 _refine_ls_number_parameters 59 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0191 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0450 _refine_ls_wR_factor_gt 0.0439 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.0000 0.0000 0.0000 0.02200(11) Uani 1 4 d S . . Au2 Au 0.0000 0.5000 0.0000 0.02086(11) Uani 1 4 d S . . N1 N 0.1544(3) 0.0000 0.1327(8) 0.0322(10) Uani 1 2 d S . . H1A H 0.1770 -0.1419 0.1520 0.048 Uiso 0.50 1 d PR . . H1B H 0.1778 0.0710 0.0579 0.048 Uiso 0.50 1 d PR . . H1C H 0.1762 0.0710 0.2460 0.048 Uiso 0.50 1 d PR . . N2 N 0.0142(4) 0.5000 0.2752(7) 0.0296(9) Uani 1 2 d S . . H2A H 0.0163 0.6419 0.3154 0.044 Uiso 0.50 1 d PR . . H2B H -0.0388 0.4290 0.2783 0.044 Uiso 0.50 1 d PR . . H2C H 0.0713 0.4290 0.3525 0.044 Uiso 0.50 1 d PR . . Cl1 Cl 0.17242(10) 0.0000 0.65291(18) 0.0253(2) Uani 1 2 d S . . O1 O 0.2639(4) 0.0000 0.6401(13) 0.081(2) Uani 1 2 d S . . O2 O 0.1564(10) -0.1911(19) 0.7478(13) 0.038(2) Uani 0.50 1 d P . . O3 O 0.0965(6) 0.0000 0.4526(10) 0.087(2) Uani 1 2 d S . . O4 O 0.1368(16) 0.204(3) 0.663(4) 0.131(10) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02237(15) 0.01236(13) 0.03246(16) 0.000 0.01303(11) 0.000 Au2 0.02238(14) 0.01305(13) 0.02731(16) 0.000 0.01096(10) 0.000 N1 0.026(2) 0.027(2) 0.045(3) 0.000 0.016(2) 0.000 N2 0.033(2) 0.026(2) 0.032(2) 0.000 0.0155(19) 0.000 Cl1 0.0287(5) 0.0229(5) 0.0270(5) 0.000 0.0146(4) 0.000 O1 0.039(3) 0.069(4) 0.156(8) 0.000 0.062(4) 0.000 O2 0.054(5) 0.025(4) 0.044(4) 0.018(3) 0.029(4) 0.007(4) O3 0.076(5) 0.118(7) 0.047(3) 0.000 0.009(3) 0.000 O4 0.091(13) 0.040(6) 0.30(3) 0.039(15) 0.123(19) 0.029(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N1 2.053(5) . ? Au1 N1 2.053(5) 5 ? Au1 Au2 2.9899(6) . ? Au1 Au2 2.9899(6) 1_545 ? Au2 N2 2.052(5) 5_565 ? Au2 N2 2.052(5) . ? Au2 Au1 2.9898(6) 1_565 ? Cl1 O4 1.346(17) . ? Cl1 O4 1.346(17) 6 ? Cl1 O1 1.398(5) . ? Cl1 O2 1.433(10) 6 ? Cl1 O2 1.433(10) . ? Cl1 O3 1.468(7) . ? O2 O4 0.60(3) 6 ? O4 O2 0.60(3) 6 ? 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 N1 Au1 N1 180.00(13) . 5 ? N1 Au1 Au2 90.0 . . ? N1 Au1 Au2 90.0 5 . ? N1 Au1 Au2 90.0 . 1_545 ? N1 Au1 Au2 90.0 5 1_545 ? Au2 Au1 Au2 180.0 . 1_545 ? N2 Au2 N2 180.0(3) 5_565 . ? N2 Au2 Au1 90.0 5_565 1_565 ? N2 Au2 Au1 90.0 . 1_565 ? N2 Au2 Au1 90.0 5_565 . ? N2 Au2 Au1 90.0 . . ? Au1 Au2 Au1 180.0 1_565 . ? O4 Cl1 O4 130.4(17) . 6 ? O4 Cl1 O1 114.8(8) . . ? O4 Cl1 O1 114.8(8) 6 . ? O4 Cl1 O2 24.6(13) . 6 ? O4 Cl1 O2 122.6(9) 6 6 ? O1 Cl1 O2 114.7(6) . 6 ? O4 Cl1 O2 122.6(9) . . ? O4 Cl1 O2 24.6(13) 6 . ? O1 Cl1 O2 114.7(6) . . ? O2 Cl1 O2 105.7(9) 6 . ? O4 Cl1 O3 85.6(12) . . ? O4 Cl1 O3 85.6(12) 6 . ? O1 Cl1 O3 104.0(5) . . ? O2 Cl1 O3 108.8(5) 6 . ? O2 Cl1 O3 108.8(5) . . ? O4 O2 Cl1 69(2) 6 . ? O2 O4 Cl1 86(3) 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 N1 Au1 Au2 N2 96.3(2) . . . 5_565 ? N1 Au1 Au2 N2 -83.7(2) 5 . . 5_565 ? Au2 Au1 Au2 N2 0.0 1_545 . . 5_565 ? N1 Au1 Au2 N2 -83.7(2) . . . . ? N1 Au1 Au2 N2 96.3(2) 5 . . . ? Au2 Au1 Au2 N2 0.0 1_545 . . . ? N1 Au1 Au2 Au1 0.0 . . . 1_565 ? N1 Au1 Au2 Au1 0.0 5 . . 1_565 ? Au2 Au1 Au2 Au1 0.0 1_545 . . 1_565 ? O4 Cl1 O2 O4 117(4) . . . 6 ? O1 Cl1 O2 O4 -96(3) . . . 6 ? O2 Cl1 O2 O4 137(3) 6 . . 6 ? O3 Cl1 O2 O4 20(3) . . . 6 ? O4 Cl1 O4 O2 81(4) 6 . . 6 ? O1 Cl1 O4 O2 -96(3) . . . 6 ? O2 Cl1 O4 O2 52(3) . . . 6 ? O3 Cl1 O4 O2 161(3) . . . 6 ? 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 N1 H1A O2 0.90 2.45 3.134(13) 133.3 7_546 N1 H1A O1 0.90 2.59 3.413(5) 151.9 7_546 N1 H1A O4 0.90 2.65 3.30(2) 129.7 4_546 N1 H1B O2 0.90 2.40 3.208(12) 150.3 6_554 N1 H1B O2 0.90 2.66 3.134(13) 113.8 4_556 N1 H1C O3 0.90 2.40 2.957(10) 119.9 . N2 H2A O3 0.90 2.45 3.294(4) 155.5 1_565 N2 H2A O4 0.90 2.51 3.044(19) 118.2 5_566 N2 H2A O2 0.90 2.58 3.067(13) 114.7 2_566 N2 H2B O4 0.90 2.16 3.044(19) 165.4 2_556 N2 H2B O2 0.90 2.19 3.067(14) 165.9 5_556 N2 H2C O1 0.90 2.45 3.048(7) 124.6 7_556 N2 H2C O4 0.90 2.55 3.27(2) 137.5 . N2 H2C O3 0.90 2.66 3.294(4) 128.3 . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.59 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.855 _refine_diff_density_min -1.057 _refine_diff_density_rms 0.181 # Attachment '2.cif' data_Au(NH3)2NO3 _database_code_depnum_ccdc_archive 'CCDC 607984' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Au(NH3)2NO3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H6 Au N3 O3' _chemical_formula_weight 293.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Immm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 6.1828(17) _cell_length_b 10.976(4) _cell_length_c 7.5983(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 515.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 282 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 28.439 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.1632 _exptl_absorpt_correction_T_max 0.7641 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4128 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 30.52 _reflns_number_total 475 _reflns_number_gt 316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0005(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 475 _refine_ls_number_parameters 39 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0593 _refine_ls_wR_factor_gt 0.0493 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Au1 Au 0.5000 0.0000 0.0000 0.01320(19) Uani 1 8 d S . . Au2 Au 0.0000 0.0000 0.0000 0.01448(19) Uani 1 8 d S . . N1 N 0.5000 0.0000 0.2684(10) 0.0192(18) Uani 1 4 d S . . H1A H 0.6357 0.0000 0.3075 0.029 Uiso 0.50 2 d SPR . . H1B H 0.4321 -0.0662 0.3075 0.029 Uiso 0.25 1 d PR . . H1C H 0.4321 0.0662 0.3075 0.029 Uiso 0.25 1 d PR . . N2 N 0.0000 0.1628(9) 0.1329(14) 0.015(2) Uani 0.50 2 d SP . . H2A H -0.1372 0.1865 0.1524 0.023 Uiso 0.25 1 d PR . . H2B H 0.0686 0.1535 0.2365 0.023 Uiso 0.25 1 d PR . . H2C H 0.0686 0.2196 0.0683 0.023 Uiso 0.25 1 d PR . . N3 N 0.0000 0.1709(9) 0.5897(14) 0.017(2) Uani 0.50 2 d SP . . O1 O 0.1730(9) 0.1449(6) 0.521(3) 0.022(4) Uani 0.50 1 d P . . O2 O 0.0000 0.2233(12) 0.7327(12) 0.045(4) Uani 0.50 2 d SP . . 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 0.0105(3) 0.0172(3) 0.0119(3) 0.000 0.000 0.000 Au2 0.0107(3) 0.0194(3) 0.0133(3) 0.000 0.000 0.000 N1 0.009(3) 0.024(4) 0.024(5) 0.000 0.000 0.000 N2 0.014(5) 0.019(5) 0.013(5) 0.004(5) 0.000 0.000 N3 0.020(5) 0.015(5) 0.017(6) 0.002(4) 0.000 0.000 O1 0.012(2) 0.046(3) 0.007(12) 0.001(4) 0.003(4) 0.003(3) O2 0.091(12) 0.033(6) 0.011(6) -0.007(6) 0.000 0.000 _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 Au1 N1 2.039(8) 9_655 ? Au1 N1 2.039(8) . ? Au1 Au2 3.0914(9) . ? Au1 Au2 3.0914(9) 1_655 ? Au2 N2 2.052(10) 9 ? Au2 N2 2.052(10) . ? Au2 N2 2.052(10) 10 ? Au2 N2 2.052(10) 2 ? Au2 Au1 3.0914(9) 1_455 ? N2 O2 1.218(13) 10_556 ? N3 O1 1.223(13) 11 ? N3 O1 1.223(13) . ? N3 O2 1.229(13) . ? N3 N3 1.36(2) 10_556 ? N3 O1 1.391(18) 4_556 ? N3 O1 1.391(18) 10_556 ? O1 O1 0.32(5) 10_556 ? O1 N3 1.391(18) 10_556 ? O2 N2 1.218(13) 10_556 ? 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 N1 Au1 N1 180.0 9_655 . ? N1 Au1 Au2 90.0 9_655 . ? N1 Au1 Au2 90.0 . . ? N1 Au1 Au2 90.0 9_655 1_655 ? N1 Au1 Au2 90.0 . 1_655 ? Au2 Au1 Au2 180.0 . 1_655 ? N2 Au2 N2 180.0(6) 9 . ? N2 Au2 N2 121.1(6) 9 10 ? N2 Au2 N2 58.9(6) . 10 ? N2 Au2 N2 58.9(6) 9 2 ? N2 Au2 N2 121.1(6) . 2 ? N2 Au2 N2 180.0(6) 10 2 ? N2 Au2 Au1 90.0 9 1_455 ? N2 Au2 Au1 90.0 . 1_455 ? N2 Au2 Au1 90.0 10 1_455 ? N2 Au2 Au1 90.0 2 1_455 ? N2 Au2 Au1 90.0 9 . ? N2 Au2 Au1 90.0 . . ? N2 Au2 Au1 90.0 10 . ? N2 Au2 Au1 90.0 2 . ? Au1 Au2 Au1 180.0 1_455 . ? O2 N2 Au2 152.5(9) 10_556 . ? O1 N3 O1 122(2) 11 . ? O1 N3 O2 119.0(11) 11 . ? O1 N3 O2 119.0(11) . . ? O1 N3 N3 64.8(12) 11 10_556 ? O1 N3 N3 64.8(12) . 10_556 ? O2 N3 N3 152.1(7) . 10_556 ? O1 N3 O1 12(2) 11 4_556 ? O1 N3 O1 111.5(9) . 4_556 ? O2 N3 O1 129.1(8) . 4_556 ? N3 N3 O1 52.7(10) 10_556 4_556 ? O1 N3 O1 111.5(9) 11 10_556 ? O1 N3 O1 12(2) . 10_556 ? O2 N3 O1 129.1(8) . 10_556 ? N3 N3 O1 52.7(10) 10_556 10_556 ? O1 N3 O1 100.5(18) 4_556 10_556 ? O1 O1 N3 115.2(12) 10_556 . ? O1 O1 N3 52.7(10) 10_556 10_556 ? N3 O1 N3 62.5(9) . 10_556 ? N2 O2 N3 119.1(13) 10_556 . ? 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 N1 Au1 Au2 N2 60.5(3) 9_655 . . 9 ? N1 Au1 Au2 N2 -119.5(3) . . . 9 ? Au2 Au1 Au2 N2 0.0 1_655 . . 9 ? N1 Au1 Au2 N2 -119.5(3) 9_655 . . . ? N1 Au1 Au2 N2 60.5(3) . . . . ? Au2 Au1 Au2 N2 0.0 1_655 . . . ? N1 Au1 Au2 N2 -60.5(3) 9_655 . . 10 ? N1 Au1 Au2 N2 119.5(3) . . . 10 ? Au2 Au1 Au2 N2 0.0 1_655 . . 10 ? N1 Au1 Au2 N2 119.5(3) 9_655 . . 2 ? N1 Au1 Au2 N2 -60.5(3) . . . 2 ? Au2 Au1 Au2 N2 0.0 1_655 . . 2 ? N1 Au1 Au2 Au1 0.0 9_655 . . 1_455 ? N1 Au1 Au2 Au1 0.0 . . . 1_455 ? Au2 Au1 Au2 Au1 0.0 1_655 . . 1_455 ? N2 Au2 N2 O2 0.0(6) 9 . . 10_556 ? N2 Au2 N2 O2 180.000(3) 10 . . 10_556 ? N2 Au2 N2 O2 0.000(3) 2 . . 10_556 ? Au1 Au2 N2 O2 90.000(3) 1_455 . . 10_556 ? Au1 Au2 N2 O2 -90.000(2) . . . 10_556 ? O1 N3 O1 O1 32.1(16) 11 . . 10_556 ? O2 N3 O1 O1 -148.9(10) . . . 10_556 ? N3 N3 O1 O1 0.000(11) 10_556 . . 10_556 ? O1 N3 O1 O1 25.2(11) 4_556 . . 10_556 ? O1 N3 O1 N3 32.1(16) 11 . . 10_556 ? O2 N3 O1 N3 -148.9(10) . . . 10_556 ? O1 N3 O1 N3 25.2(10) 4_556 . . 10_556 ? O1 N3 O1 N3 0.000(16) 10_556 . . 10_556 ? O1 N3 O2 N2 89.5(11) 11 . . 10_556 ? O1 N3 O2 N2 -89.5(11) . . . 10_556 ? N3 N3 O2 N2 180.000(5) 10_556 . . 10_556 ? O1 N3 O2 N2 97.6(13) 4_556 . . 10_556 ? O1 N3 O2 N2 -97.6(13) 10_556 . . 10_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.030 _refine_diff_density_min -2.730 _refine_diff_density_rms 0.303 data_Au(NH3)2ClO4 _database_code_depnum_ccdc_archive 'CCDC 608549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Au(NH3)2ClO4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H12 Au2 Cl2 N4 O8' _chemical_formula_weight 660.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6791(10) _cell_length_b 7.9129(10) _cell_length_c 11.5690(16) _cell_angle_alpha 72.624(8) _cell_angle_beta 73.946(7) _cell_angle_gamma 66.513(13) _cell_volume 605.27(14) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 182 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 24.684 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.1296 _exptl_absorpt_correction_T_max 0.6381 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6697 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2980 _reflns_number_gt 2662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0666P)^2^+0.9599P] 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 0.0018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2980 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Au1 Au 0.0000 0.5000 0.0000 0.00759(15) Uani 1 2 d S . . Au2 Au 0.0000 0.0000 0.5000 0.01175(15) Uani 1 2 d S . . Au3 Au 0.01965(5) 0.24503(3) 0.247877(18) 0.00884(15) Uani 1 1 d . . . N1 N 0.2769(8) 0.4868(7) -0.0125(5) 0.0127(11) Uani 1 1 d . . . H1A H 0.3128 0.5568 -0.0843 0.019 Uiso 1 1 calc R . . H1B H 0.3561 0.3677 -0.0074 0.019 Uiso 1 1 calc R . . H1C H 0.2817 0.5304 0.0487 0.019 Uiso 1 1 calc R . . N2 N 0.2759(8) -0.0237(8) 0.4980(5) 0.0151(11) Uani 1 1 d . . . H2A H 0.3120 -0.0962 0.5687 0.023 Uiso 1 1 calc R . . H2B H 0.2807 0.0902 0.4889 0.023 Uiso 1 1 calc R . . H2C H 0.3551 -0.0755 0.4357 0.023 Uiso 1 1 calc R . . N3 N 0.1542(9) 0.0139(7) 0.1701(5) 0.0166(12) Uani 1 1 d . . . H3A H 0.1781 0.0512 0.0886 0.025 Uiso 1 1 calc R . . H3B H 0.0782 -0.0549 0.1909 0.025 Uiso 1 1 calc R . . H3C H 0.2648 -0.0552 0.1971 0.025 Uiso 1 1 calc R . . N4 N -0.1148(9) 0.4783(7) 0.3238(5) 0.0174(12) Uani 1 1 d . . . H4A H -0.1293 0.5819 0.2642 0.026 Uiso 1 1 calc R . . H4B H -0.0435 0.4771 0.3732 0.026 Uiso 1 1 calc R . . H4C H -0.2301 0.4774 0.3670 0.026 Uiso 1 1 calc R . . Cl1 Cl 0.6432(2) 0.49825(18) -0.33642(12) 0.0101(3) Uani 1 1 d . . . O1 O 0.7387(10) 0.6135(9) -0.4281(5) 0.0304(14) Uani 1 1 d . . . O2 O 0.4448(9) 0.6115(9) -0.3026(5) 0.0436(16) Uani 1 1 d . . . O3 O 0.7301(9) 0.4251(8) -0.2293(5) 0.0262(13) Uani 1 1 d . . . O4 O 0.6499(13) 0.3483(7) -0.3831(5) 0.052(2) Uani 1 1 d . . . Cl2 Cl 0.3351(2) 0.0202(2) -0.16300(14) 0.0182(4) Uani 1 1 d . . . O5 O 0.3827(13) 0.1430(8) -0.1184(6) 0.054(2) Uani 1 1 d . A . O6A O 0.1242(14) 0.1229(13) -0.1280(10) 0.025(2) Uani 0.50 1 d P A 1 O7A O 0.382(2) -0.1561(13) -0.0917(10) 0.036(3) Uani 0.50 1 d P A 1 O8A O 0.389(2) 0.0501(15) -0.2844(9) 0.033(3) Uani 0.50 1 d P A 1 O6B O 0.2323(18) -0.0984(15) -0.0759(10) 0.022(2) Uani 0.50 1 d P A 2 O7B O 0.5277(15) -0.1163(13) -0.2095(10) 0.028(2) Uani 0.50 1 d P A 2 O8B O 0.2360(18) 0.0944(15) -0.2709(9) 0.022(2) Uani 0.50 1 d P A 2 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 0.0098(2) 0.0060(2) 0.0067(2) -0.00049(15) -0.00446(15) -0.00096(15) Au2 0.0116(2) 0.0171(2) 0.0067(2) 0.00333(16) -0.00577(15) -0.00666(16) Au3 0.0149(2) 0.0064(2) 0.0052(2) -0.00097(13) -0.00453(13) -0.00208(13) N1 0.012(3) 0.009(2) 0.016(2) -0.0023(19) -0.005(2) -0.001(2) N2 0.014(3) 0.021(3) 0.012(2) 0.000(2) -0.007(2) -0.006(2) N3 0.025(3) 0.007(2) 0.016(3) -0.0034(19) -0.007(2) 0.000(2) N4 0.021(3) 0.015(3) 0.016(3) -0.009(2) -0.010(2) 0.003(2) Cl1 0.0140(8) 0.0081(6) 0.0102(6) -0.0015(5) -0.0067(6) -0.0030(5) O1 0.041(4) 0.040(3) 0.015(3) 0.003(2) -0.005(3) -0.026(3) O2 0.013(3) 0.065(4) 0.032(3) -0.010(3) -0.003(2) 0.008(3) O3 0.041(4) 0.024(3) 0.017(3) 0.006(2) -0.020(3) -0.012(3) O4 0.126(7) 0.015(3) 0.036(3) -0.003(2) -0.040(4) -0.030(3) Cl2 0.0121(8) 0.0191(8) 0.0184(7) 0.0053(6) -0.0069(6) -0.0042(6) O5 0.108(7) 0.023(3) 0.036(3) -0.022(3) 0.005(4) -0.028(3) O6A 0.008(5) 0.021(5) 0.047(6) -0.010(4) -0.007(5) -0.003(4) O7A 0.067(10) 0.009(5) 0.027(6) 0.009(4) -0.030(7) -0.002(5) O8A 0.052(9) 0.030(6) 0.018(5) -0.002(4) 0.003(6) -0.021(6) O6B 0.028(7) 0.023(5) 0.016(5) 0.000(4) -0.002(5) -0.014(5) O7B 0.016(5) 0.016(5) 0.044(6) -0.016(4) -0.007(5) 0.010(4) O8B 0.027(7) 0.026(5) 0.013(5) 0.010(4) -0.017(5) -0.009(5) _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 Au1 N1 2.053(5) 2_565 ? Au1 N1 2.053(5) . ? Au1 Au3 2.9762(5) . ? Au1 Au3 2.9762(5) 2_565 ? Au2 N2 2.045(5) . ? Au2 N2 2.045(5) 2_556 ? Au2 Au3 2.9836(5) 2_556 ? Au2 Au3 2.9836(5) . ? Au3 N3 2.045(5) . ? Au3 N4 2.048(5) . ? Cl1 O4 1.421(5) . ? Cl1 O1 1.422(6) . ? Cl1 O3 1.427(5) . ? Cl1 O2 1.438(6) . ? Cl2 O8A 1.326(10) . ? Cl2 O7A 1.354(9) . ? Cl2 O5 1.425(6) . ? Cl2 O6B 1.451(11) . ? Cl2 O8B 1.488(10) . ? Cl2 O6A 1.494(10) . ? Cl2 O7B 1.509(10) . ? 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 N1 Au1 N1 180.0(4) 2_565 . ? N1 Au1 Au3 90.73(14) 2_565 . ? N1 Au1 Au3 89.27(14) . . ? N1 Au1 Au3 89.27(14) 2_565 2_565 ? N1 Au1 Au3 90.73(14) . 2_565 ? Au3 Au1 Au3 180.0 . 2_565 ? N2 Au2 N2 180.0 . 2_556 ? N2 Au2 Au3 90.83(14) . 2_556 ? N2 Au2 Au3 89.17(14) 2_556 2_556 ? N2 Au2 Au3 89.17(14) . . ? N2 Au2 Au3 90.83(14) 2_556 . ? Au3 Au2 Au3 180.0 2_556 . ? N3 Au3 N4 179.36(18) . . ? N3 Au3 Au1 90.78(14) . . ? N4 Au3 Au1 88.59(15) . . ? N3 Au3 Au2 91.16(15) . . ? N4 Au3 Au2 89.47(15) . . ? Au1 Au3 Au2 174.741(13) . . ? O4 Cl1 O1 110.2(4) . . ? O4 Cl1 O3 110.3(3) . . ? O1 Cl1 O3 110.3(4) . . ? O4 Cl1 O2 109.0(5) . . ? O1 Cl1 O2 108.8(4) . . ? O3 Cl1 O2 108.4(4) . . ? O8A Cl2 O7A 121.5(8) . . ? O8A Cl2 O5 108.7(6) . . ? O7A Cl2 O5 111.4(6) . . ? O8A Cl2 O6B 132.7(7) . . ? O7A Cl2 O6B 43.3(7) . . ? O5 Cl2 O6B 118.5(5) . . ? O8A Cl2 O8B 43.9(7) . . ? O7A Cl2 O8B 128.3(7) . . ? O5 Cl2 O8B 120.2(5) . . ? O6B Cl2 O8B 103.9(7) . . ? O8A Cl2 O6A 110.7(7) . . ? O7A Cl2 O6A 109.1(8) . . ? O5 Cl2 O6A 91.3(5) . . ? O6B Cl2 O6A 66.5(6) . . ? O8B Cl2 O6A 68.3(6) . . ? O8A Cl2 O7B 64.8(7) . . ? O7A Cl2 O7B 65.1(7) . . ? O5 Cl2 O7B 104.5(5) . . ? O6B Cl2 O7B 104.6(6) . . ? O8B Cl2 O7B 102.9(6) . . ? O6A Cl2 O7B 164.1(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 N1 Au1 Au3 N3 96.3(2) 2_565 . . . ? N1 Au1 Au3 N3 -83.7(2) . . . . ? Au3 Au1 Au3 N3 -130(100) 2_565 . . . ? N1 Au1 Au3 N4 -83.8(2) 2_565 . . . ? N1 Au1 Au3 N4 96.2(2) . . . . ? Au3 Au1 Au3 N4 50(100) 2_565 . . . ? N1 Au1 Au3 Au2 -15.34(16) 2_565 . . . ? N1 Au1 Au3 Au2 164.66(16) . . . . ? Au3 Au1 Au3 Au2 118(100) 2_565 . . . ? N2 Au2 Au3 N3 83.7(2) . . . . ? N2 Au2 Au3 N3 -96.3(2) 2_556 . . . ? Au3 Au2 Au3 N3 117(100) 2_556 . . . ? N2 Au2 Au3 N4 -96.3(2) . . . . ? N2 Au2 Au3 N4 83.7(2) 2_556 . . . ? Au3 Au2 Au3 N4 -63(100) 2_556 . . . ? N2 Au2 Au3 Au1 -164.68(17) . . . . ? N2 Au2 Au3 Au1 15.32(17) 2_556 . . . ? Au3 Au2 Au3 Au1 -131(100) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 5.501 _refine_diff_density_min -5.713 _refine_diff_density_rms 0.467