# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2027 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Prof. Dr. H. Schmidbaur, Dr. A. Schier Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstra\"se 4 D-85747 Garching Germany ; _publ_contact_author_phone '++49 89 2891-3130' _publ_contact_author_fax '++49 89 2891-3125' _publ_contact_author_email 'Annette.Schier@lrz.tum.de' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; please consider this CIF submission for publication in "J. Chem. Soc., Dalton Trans.". Date of submission: May 20000. ; #============================================================================ # 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_name_full ? _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 ; The Solid State Aggregation of Two Gold(I) Nitrate Complexes ; loop_ _publ_author_name _publ_author_address 'T. Mathieson' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstra\"se 4 D-85747 Garching Germany ; 'A. Schier' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstra\"se 4 D-85747 Garching Germany ; 'Hubert Schmidbaur' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstra\"se 4 D-85747 Garching Germany ; #============================================================================== data_TREV3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 Au N O3 P' _chemical_formula_weight 335.05 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' 'P' 'P' 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M P(-1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.052(1) _cell_length_b 10.436(2) _cell_length_c 13.422(1) _cell_angle_alpha 78.12(1) _cell_angle_beta 75.62(1) _cell_angle_gamma 74.97(1) _cell_volume 1172.6(3) _cell_formula_units_Z 6 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 17 _cell_measurement_theta_max 24 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 18.967 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.503 _exptl_absorpt_correction_T_max 0.997 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'Enraf Nonius CAD4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600s _diffrn_standards_decay_% 1.7% _diffrn_reflns_number 5398 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.03 _reflns_number_total 5112 _reflns_number_gt 4501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius CAD4' _computing_cell_refinement 'Enraf Nonius CAD4' _computing_data_reduction 'Enraf Nonius SDP-PLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0465P)^2^+8.6998P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00317(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5112 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _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 0.96401(3) 0.16320(3) 0.28753(2) 0.02892(10) Uani 1 1 d . . . Au2 Au 0.62797(3) 0.26081(3) 0.18865(2) 0.02726(9) Uani 1 1 d . . . Au3 Au 1.34200(3) 0.11807(3) 0.19578(2) 0.02339(9) Uani 1 1 d . . . P1 P 0.9440(2) 0.35781(19) 0.33721(14) 0.0241(4) Uani 1 1 d . . . P2 P 0.7515(2) 0.24977(19) 0.02465(14) 0.0244(4) Uani 1 1 d . . . P3 P 1.4236(2) -0.05722(17) 0.30888(13) 0.0208(3) Uani 1 1 d . . . C11 C 0.8189(10) 0.3769(10) 0.4620(7) 0.040(2) Uani 1 1 d . . . H11A H 0.8149 0.4648 0.4792 0.061 Uiso 1 1 calc R . . H11B H 0.8599 0.3060 0.5148 0.061 Uiso 1 1 calc R . . H11C H 0.7135 0.3705 0.4603 0.061 Uiso 1 1 calc R . . C12 C 1.1257(10) 0.3851(10) 0.3494(8) 0.042(2) Uani 1 1 d . . . H12A H 1.1080 0.4728 0.3713 0.063 Uiso 1 1 calc R . . H12B H 1.1992 0.3830 0.2822 0.063 Uiso 1 1 calc R . . H12C H 1.1693 0.3145 0.4014 0.063 Uiso 1 1 calc R . . C13 C 0.8686(14) 0.4991(10) 0.2494(8) 0.050(2) Uani 1 1 d . . . H13A H 0.8624 0.5820 0.2753 0.075 Uiso 1 1 calc R . . H13B H 0.7641 0.4945 0.2442 0.075 Uiso 1 1 calc R . . H13C H 0.9380 0.4983 0.1806 0.075 Uiso 1 1 calc R . . C21 C 0.9499(9) 0.2645(9) 0.0022(7) 0.0365(18) Uani 1 1 d . . . H21A H 0.9996 0.2584 -0.0709 0.055 Uiso 1 1 calc R . . H21B H 1.0064 0.1919 0.0469 0.055 Uiso 1 1 calc R . . H21C H 0.9525 0.3513 0.0182 0.055 Uiso 1 1 calc R . . C22 C 0.6736(9) 0.3734(8) -0.0745(6) 0.0327(16) Uani 1 1 d . . . H22A H 0.7379 0.3568 -0.1429 0.049 Uiso 1 1 calc R . . H22B H 0.6743 0.4630 -0.0631 0.049 Uiso 1 1 calc R . . H22C H 0.5662 0.3680 -0.0715 0.049 Uiso 1 1 calc R . . C23 C 0.7609(11) 0.0887(8) -0.0086(7) 0.0369(18) Uani 1 1 d . . . H23A H 0.8157 0.0850 -0.0811 0.055 Uiso 1 1 calc R . . H23B H 0.6547 0.0759 0.0001 0.055 Uiso 1 1 calc R . . H23C H 0.8174 0.0177 0.0372 0.055 Uiso 1 1 calc R . . C31 C 1.3218(10) -0.0366(8) 0.4398(6) 0.0328(17) Uani 1 1 d . . . H31A H 1.3599 -0.1158 0.4878 0.049 Uiso 1 1 calc R . . H31B H 1.2094 -0.0263 0.4452 0.049 Uiso 1 1 calc R . . H31C H 1.3405 0.0434 0.4577 0.049 Uiso 1 1 calc R . . C32 C 1.4044(9) -0.2157(8) 0.2866(6) 0.0308(16) Uani 1 1 d . . . H32A H 1.4427 -0.2871 0.3401 0.046 Uiso 1 1 calc R . . H32B H 1.4657 -0.2338 0.2178 0.046 Uiso 1 1 calc R . . H32C H 1.2941 -0.2125 0.2899 0.046 Uiso 1 1 calc R . . C33 C 1.6267(8) -0.0848(8) 0.3107(7) 0.0325(17) Uani 1 1 d . . . H33A H 1.6552 -0.1639 0.3616 0.049 Uiso 1 1 calc R . . H33B H 1.6465 -0.0061 0.3298 0.049 Uiso 1 1 calc R . . H33C H 1.6895 -0.0996 0.2415 0.049 Uiso 1 1 calc R . . O11 O 0.9808(7) -0.0135(6) 0.2310(5) 0.0395(14) Uani 1 1 d . . . O12 O 1.0093(7) -0.2304(7) 0.2700(6) 0.0519(18) Uani 1 1 d . . . O13 O 0.9762(8) -0.1112(7) 0.3917(5) 0.0494(16) Uani 1 1 d . . . O21 O 0.5268(7) 0.2408(6) 0.3476(4) 0.0368(13) Uani 1 1 d . . . O22 O 0.4182(8) 0.3396(7) 0.4813(4) 0.0443(15) Uani 1 1 d . . . O23 O 0.4705(9) 0.4579(6) 0.3316(5) 0.0496(16) Uani 1 1 d . . . O31 O 1.2590(7) 0.2963(6) 0.1013(4) 0.0349(13) Uani 1 1 d . . . O32 O 1.2647(8) 0.3974(6) -0.0559(5) 0.0449(15) Uani 1 1 d . . . O33 O 1.3696(8) 0.1856(7) -0.0286(5) 0.0443(15) Uani 1 1 d . . . N1 N 0.9882(7) -0.1207(7) 0.2997(6) 0.0340(15) Uani 1 1 d . . . N2 N 0.4703(7) 0.3506(7) 0.3879(5) 0.0280(13) Uani 1 1 d . . . N3 N 1.2983(7) 0.2914(7) 0.0025(5) 0.0298(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03069(16) 0.03249(17) 0.02727(15) -0.01119(11) -0.00075(11) -0.01310(12) Au2 0.02933(16) 0.02540(15) 0.02551(15) -0.00575(10) -0.00030(11) -0.00699(11) Au3 0.02597(15) 0.02227(14) 0.02091(14) -0.00030(10) -0.00742(10) -0.00338(10) P1 0.0264(9) 0.0256(9) 0.0232(8) -0.0040(7) -0.0094(7) -0.0062(7) P2 0.0226(8) 0.0243(9) 0.0267(9) -0.0068(7) -0.0014(7) -0.0070(7) P3 0.0222(8) 0.0204(8) 0.0189(8) -0.0009(6) -0.0053(6) -0.0039(6) C11 0.035(4) 0.052(5) 0.032(4) -0.013(4) -0.006(3) -0.001(4) C12 0.029(4) 0.049(5) 0.058(6) -0.030(4) -0.012(4) -0.007(4) C13 0.077(7) 0.038(5) 0.044(5) 0.013(4) -0.033(5) -0.026(5) C21 0.027(4) 0.047(5) 0.035(4) -0.006(4) -0.007(3) -0.009(4) C22 0.032(4) 0.034(4) 0.033(4) -0.003(3) -0.009(3) -0.010(3) C23 0.045(5) 0.028(4) 0.035(4) -0.012(3) 0.007(3) -0.011(3) C31 0.038(4) 0.033(4) 0.024(4) -0.006(3) -0.008(3) 0.002(3) C32 0.032(4) 0.026(4) 0.033(4) -0.006(3) -0.004(3) -0.005(3) C33 0.018(3) 0.035(4) 0.042(4) 0.001(3) -0.006(3) -0.007(3) O11 0.038(3) 0.043(3) 0.043(3) -0.019(3) 0.002(3) -0.017(3) O12 0.036(3) 0.041(4) 0.086(5) -0.039(4) -0.003(3) -0.007(3) O13 0.058(4) 0.038(4) 0.051(4) -0.013(3) -0.020(3) 0.005(3) O21 0.044(3) 0.027(3) 0.032(3) -0.007(2) 0.001(2) -0.001(2) O22 0.046(4) 0.053(4) 0.026(3) -0.013(3) -0.001(2) 0.005(3) O23 0.066(5) 0.027(3) 0.051(4) -0.004(3) -0.004(3) -0.010(3) O31 0.046(3) 0.028(3) 0.026(3) 0.006(2) -0.015(2) -0.001(2) O32 0.053(4) 0.042(3) 0.041(3) 0.019(3) -0.027(3) -0.016(3) O33 0.047(4) 0.043(4) 0.038(3) -0.009(3) 0.000(3) -0.008(3) N1 0.015(3) 0.039(4) 0.052(4) -0.022(3) -0.006(3) -0.002(3) N2 0.023(3) 0.030(3) 0.030(3) -0.005(3) -0.006(2) -0.003(2) N3 0.025(3) 0.037(4) 0.031(3) 0.005(3) -0.014(3) -0.014(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 Au1 O11 2.090(6) . ? Au1 P1 2.2158(19) . ? Au1 Au3 3.2795(6) . ? Au2 O21 2.093(6) . ? Au2 P2 2.2190(18) . ? Au2 Au3 3.2783(5) 1_455 ? Au3 O31 2.100(5) . ? Au3 P3 2.2156(17) . ? Au3 Au2 3.2783(6) 1_655 ? P1 C13 1.786(9) . ? P1 C11 1.790(8) . ? P1 C12 1.791(8) . ? P2 C21 1.787(8) . ? P2 C22 1.794(8) . ? P2 C23 1.802(8) . ? P3 C33 1.791(7) . ? P3 C31 1.798(8) . ? P3 C32 1.798(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O11 N1 1.293(10) . ? O12 N1 1.241(9) . ? O13 N1 1.235(9) . ? O21 N2 1.296(8) . ? O22 N2 1.217(9) . ? O23 N2 1.215(9) . ? O31 N3 1.293(8) . ? O32 N3 1.232(8) . ? O33 N3 1.224(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 O11 Au1 P1 176.23(19) . . ? O11 Au1 Au3 85.67(16) . . ? P1 Au1 Au3 94.18(5) . . ? O21 Au2 P2 171.46(16) . . ? O21 Au2 Au3 78.85(17) . 1_455 ? P2 Au2 Au3 99.30(5) . 1_455 ? O31 Au3 P3 173.98(16) . . ? O31 Au3 Au2 84.32(17) . 1_655 ? P3 Au3 Au2 93.48(5) . 1_655 ? O31 Au3 Au1 78.78(17) . . ? P3 Au3 Au1 99.40(5) . . ? Au2 Au3 Au1 138.383(13) 1_655 . ? C13 P1 C11 105.7(5) . . ? C13 P1 C12 105.3(5) . . ? C11 P1 C12 104.2(4) . . ? C13 P1 Au1 113.1(3) . . ? C11 P1 Au1 113.6(3) . . ? C12 P1 Au1 114.0(3) . . ? C21 P2 C22 103.6(4) . . ? C21 P2 C23 105.6(4) . . ? C22 P2 C23 106.3(4) . . ? C21 P2 Au2 112.5(3) . . ? C22 P2 Au2 117.7(3) . . ? C23 P2 Au2 110.2(3) . . ? C33 P3 C31 105.3(4) . . ? C33 P3 C32 103.5(4) . . ? C31 P3 C32 107.2(4) . . ? C33 P3 Au3 113.7(3) . . ? C31 P3 Au3 111.4(3) . . ? C32 P3 Au3 115.0(3) . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P2 C23 H23A 109.5 . . ? P2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P3 C31 H31A 109.5 . . ? P3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? P3 C32 H32A 109.5 . . ? P3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P3 C33 H33A 109.5 . . ? P3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? P3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N1 O11 Au1 115.1(5) . . ? N2 O21 Au2 116.8(5) . . ? N3 O31 Au3 114.9(5) . . ? O13 N1 O12 122.2(8) . . ? O13 N1 O11 119.4(7) . . ? O12 N1 O11 118.4(7) . . ? O23 N2 O22 123.6(7) . . ? O23 N2 O21 119.2(7) . . ? O22 N2 O21 117.3(7) . . ? O33 N3 O32 123.4(7) . . ? O33 N3 O31 119.8(6) . . ? O32 N3 O31 116.8(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.057 _refine_diff_density_min -2.092 _refine_diff_density_rms 0.223 data_trev8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5.50 H10 Au Cl N2 O3' _chemical_formula_weight 384.57 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.7432(9) _cell_length_b 7.7740(3) _cell_length_c 10.5128(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.945(2) _cell_angle_gamma 90.00 _cell_volume 2041.21(11) _cell_formula_units_Z 8 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 14.652 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'Nonius DIP2020' _diffrn_measurement_method 'phi-oscillation, 360 images, 1, 0.4/min, 300 s/image' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3779 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 26.45 _reflns_number_total 1986 _reflns_number_gt 1911 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement ? _computing_data_reduction SCALEPACK _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0967P)^2^+10.9327P] 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 'riding (t-Bu), fixed (CHCl2)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1986 _refine_ls_number_parameters 114 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _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 Au Au -0.003302(11) 0.16228(3) 0.59268(3) 0.0239(2) Uani 1 1 d . . . N1 N 0.1173(3) 0.2220(9) 0.6938(7) 0.0257(15) Uani 1 1 d . . . C1 C 0.1758(3) 0.2428(10) 0.7338(8) 0.0225(16) Uani 1 1 d . . . C11 C 0.1877(4) 0.2447(12) 0.6030(9) 0.0322(19) Uani 1 1 d . . . H11A H 0.1704 0.3447 0.5480 0.048 Uiso 1 1 calc R . . H11B H 0.1740 0.1391 0.5515 0.048 Uiso 1 1 calc R . . H11C H 0.2265 0.2517 0.6251 0.048 Uiso 1 1 calc R . . C12 C 0.2017(4) 0.0882(10) 0.8252(9) 0.0284(17) Uani 1 1 d . . . H12A H 0.1915 -0.0183 0.7722 0.043 Uiso 1 1 calc R . . H12B H 0.1894 0.0838 0.9024 0.043 Uiso 1 1 calc R . . H12C H 0.2408 0.1006 0.8590 0.043 Uiso 1 1 calc R . . C13 C 0.1909(4) 0.4115(11) 0.8129(9) 0.0302(18) Uani 1 1 d . . . H13A H 0.1739 0.5078 0.7528 0.045 Uiso 1 1 calc R . . H13B H 0.2298 0.4259 0.8463 0.045 Uiso 1 1 calc R . . H13C H 0.1786 0.4091 0.8902 0.045 Uiso 1 1 calc R . . N2 N -0.1132(3) 0.2603(10) 0.4728(8) 0.0263(15) Uani 1 1 d . . . O1 O -0.0903(3) 0.3993(8) 0.4908(9) 0.0448(18) Uani 1 1 d . . . O2 O -0.1613(3) 0.2406(9) 0.4162(7) 0.0343(14) Uani 1 1 d . . . O3 O -0.0837(2) 0.1205(9) 0.5178(7) 0.0270(12) Uani 1 1 d . . . C C 0.0722(3) 0.1976(12) 0.6562(9) 0.0213(16) Uani 1 1 d . . . Cl1 Cl -0.05819(13) -0.2434(4) 0.7072(3) 0.0543(7) Uani 1 1 d . . . C01 C 0.0000 -0.372(2) 0.7500 0.056(5) Uani 1 2 d S . . H01A H -0.0022 -0.4455 0.6742 0.067 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.0234(3) 0.0165(3) 0.0309(3) -0.00133(9) 0.00871(19) 0.00064(9) N1 0.030(4) 0.019(3) 0.027(4) -0.005(3) 0.009(3) 0.001(3) C1 0.021(4) 0.017(4) 0.027(4) 0.000(3) 0.005(3) 0.001(3) C11 0.040(5) 0.030(5) 0.026(4) -0.001(3) 0.012(4) -0.005(4) C12 0.032(4) 0.022(4) 0.028(4) 0.004(3) 0.007(3) 0.003(3) C13 0.038(5) 0.022(4) 0.027(4) -0.004(3) 0.007(3) -0.006(3) N2 0.023(4) 0.026(4) 0.030(4) 0.000(3) 0.009(3) 0.007(3) O1 0.035(4) 0.012(3) 0.072(5) -0.002(3) 0.000(3) -0.001(3) O2 0.030(4) 0.032(3) 0.039(4) 0.001(3) 0.010(3) 0.000(3) O3 0.022(3) 0.021(3) 0.033(3) 0.002(3) 0.003(2) 0.004(3) C 0.016(4) 0.027(4) 0.020(4) 0.000(3) 0.006(3) -0.001(3) Cl1 0.0626(18) 0.0496(16) 0.0448(15) -0.0057(12) 0.0118(13) -0.0038(13) C01 0.086(14) 0.030(7) 0.037(8) 0.000 0.006(8) 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 Au C 1.907(8) . ? Au O3 2.033(6) . ? Au Au 3.2312(5) 5_556 ? Au Au 3.2488(6) 2_556 ? N1 C 1.142(11) . ? N1 C1 1.477(11) . ? C1 C11 1.519(12) . ? C1 C13 1.527(11) . ? C1 C12 1.541(11) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? N2 O2 1.219(10) . ? N2 O1 1.223(11) . ? N2 O3 1.327(10) . ? Cl1 C01 1.765(10) . ? C01 Cl1 1.765(10) 2_556 ? C01 H01A 0.9666 . ? 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 C Au O3 177.6(3) . . ? C Au Au 92.5(3) . 5_556 ? O3 Au Au 85.39(19) . 5_556 ? C Au Au 88.7(3) . 2_556 ? O3 Au Au 93.43(19) . 2_556 ? Au Au Au 128.259(10) 5_556 2_556 ? C N1 C1 175.2(8) . . ? N1 C1 C11 106.7(7) . . ? N1 C1 C13 107.2(7) . . ? C11 C1 C13 112.6(7) . . ? N1 C1 C12 106.7(7) . . ? C11 C1 C12 112.2(7) . . ? C13 C1 C12 111.0(7) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 N2 O1 124.7(8) . . ? O2 N2 O3 117.4(7) . . ? O1 N2 O3 117.9(7) . . ? N2 O3 Au 114.8(5) . . ? N1 C Au 178.7(8) . . ? Cl1 C01 Cl1 111.3(9) 2_556 . ? Cl1 C01 H01A 109.6 2_556 . ? Cl1 C01 H01A 109.6 . . ? 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 C N1 C1 C11 41(10) . . . . ? C N1 C1 C13 162(10) . . . . ? C N1 C1 C12 -79(10) . . . . ? O2 N2 O3 Au 173.8(6) . . . . ? O1 N2 O3 Au -6.0(10) . . . . ? C Au O3 N2 -104(7) . . . . ? Au Au O3 N2 -132.6(6) 5_556 . . . ? Au Au O3 N2 99.3(5) 2_556 . . . ? C1 N1 C Au -124(34) . . . . ? O3 Au C N1 105(37) . . . . ? Au Au C N1 134(37) 5_556 . . . ? Au Au C N1 -98(37) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 4.952 _refine_diff_density_min -6.308 _refine_diff_density_rms 0.480