Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Carl Redshaw' _publ_contact_author_address ; School of Chemistry and Pharmacy University of East Anglia Norwich Norfolk NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email CARL.REDSHAW@UEA.AC.UK _publ_section_title ; Variable solid state aggregations in a series of (isocyanide)gold(I) halides with the novel trimethylamine-isocyanoborane adduct ; loop_ _publ_author_name 'Carl Redshaw' 'Mark Elsegood' 'Simon Humphrey' 'William C. Kaska' 'Hans-Georg Mack' 'Hermann A. Mayer' ; K.J.H.Young ; data_new _database_code_depnum_ccdc_archive 'CCDC 247203' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H22 Au2 B2 Cl2 N4' _chemical_formula_sum 'C8 H22 Au2 B2 Cl2 N4' _chemical_formula_weight 660.75 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.3771(2) _cell_length_b 15.5012(4) _cell_length_c 18.6225(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1840.88(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 24436 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 16.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.247 _exptl_absorpt_correction_T_max 0.397 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 12711 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4165 _reflns_number_gt 3433 _reflns_threshold_expression I>2\s(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement '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^)+(0.0432P)^2^+36.4370P] 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 0.00080(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 4165 _refine_ls_number_parameters 195 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.931 _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 0.11743(9) 0.93760(3) 0.84037(3) 0.04278(18) Uani 1 1 d . . . Au2 Au 0.61856(9) 0.95355(3) 0.84216(3) 0.04077(17) Uani 1 1 d . . . Cl1 Cl 0.1218(7) 0.9964(3) 0.7286(2) 0.0547(9) Uani 1 1 d . . . Cl2 Cl 0.6217(8) 1.0469(2) 0.9361(3) 0.0611(10) Uani 1 1 d . . . C1 C 0.104(3) 0.8896(9) 0.9362(10) 0.052(4) Uani 1 1 d . . . N1 N 0.091(2) 0.8630(8) 0.9933(8) 0.056(3) Uani 1 1 d . . . B1 B 0.070(3) 0.8293(11) 1.0710(11) 0.050(4) Uani 1 1 d . . . H1A H 0.2025 0.8385 1.0974 0.060 Uiso 1 1 calc R . . H1B H 0.0382 0.7668 1.0707 0.060 Uiso 1 1 calc R . . N2 N -0.1173(19) 0.8814(6) 1.1089(6) 0.037(2) Uani 1 1 d . . . C2 C -0.116(4) 0.8530(12) 1.1843(9) 0.073(6) Uani 1 1 d . . . H2A H -0.2290 0.8822 1.2105 0.109 Uiso 1 1 calc R . . H2B H 0.0190 0.8673 1.2062 0.109 Uiso 1 1 calc R . . H2C H -0.1381 0.7904 1.1863 0.109 Uiso 1 1 calc R . . C3 C -0.324(2) 0.8625(10) 1.0744(10) 0.054(4) Uani 1 1 d . . . H3A H -0.3199 0.8807 1.0241 0.081 Uiso 1 1 calc R . . H3B H -0.4348 0.8938 1.0997 0.081 Uiso 1 1 calc R . . H3C H -0.3516 0.8004 1.0769 0.081 Uiso 1 1 calc R . . C4 C -0.086(3) 0.9762(9) 1.1049(9) 0.055(4) Uani 1 1 d . . . H4A H -0.2193 1.0055 1.1143 0.083 Uiso 1 1 calc R . . H4B H -0.0355 0.9917 1.0569 0.083 Uiso 1 1 calc R . . H4C H 0.0177 0.9939 1.1409 0.083 Uiso 1 1 calc R . . C5 C 0.625(3) 0.8745(9) 0.7593(9) 0.047(3) Uani 1 1 d . . . N3 N 0.630(2) 0.8331(8) 0.7103(7) 0.048(3) Uani 1 1 d . . . B2 B 0.637(3) 0.7764(13) 0.6456(13) 0.066(6) Uani 1 1 d . A . H2D H 0.5779 0.8080 0.6041 0.079 Uiso 1 1 calc R . . H2E H 0.5483 0.7249 0.6541 0.079 Uiso 1 1 calc R . . N4 N 0.867(2) 0.7463(6) 0.6270(6) 0.043(2) Uani 1 1 d DU . . C6 C 1.038(7) 0.811(3) 0.631(3) 0.056(11) Uani 0.33(5) 1 d PDU A 1 H6A H 1.0149 0.8557 0.5945 0.084 Uiso 0.33(5) 1 calc PR A 1 H6B H 1.1731 0.7825 0.6218 0.084 Uiso 0.33(5) 1 calc PR A 1 H6C H 1.0399 0.8373 0.6786 0.084 Uiso 0.33(5) 1 calc PR A 1 C7 C 0.909(9) 0.679(3) 0.678(2) 0.051(10) Uani 0.33(5) 1 d PDU A 1 H7A H 0.7937 0.6370 0.6775 0.077 Uiso 0.33(5) 1 calc PR A 1 H7B H 0.9218 0.7037 0.7262 0.077 Uiso 0.33(5) 1 calc PR A 1 H7C H 1.0402 0.6496 0.6653 0.077 Uiso 0.33(5) 1 calc PR A 1 C8 C 0.867(11) 0.704(3) 0.5545(14) 0.041(8) Uani 0.33(5) 1 d PDU A 1 H8A H 0.8584 0.7485 0.5172 0.061 Uiso 0.33(5) 1 calc PR A 1 H8B H 0.7465 0.6654 0.5507 0.061 Uiso 0.33(5) 1 calc PR A 1 H8C H 0.9970 0.6711 0.5484 0.061 Uiso 0.33(5) 1 calc PR A 1 C6X C 0.983(5) 0.8225(13) 0.599(2) 0.057(7) Uani 0.67(5) 1 d PDU A 2 H6X1 H 0.9753 0.8697 0.6337 0.085 Uiso 0.67(5) 1 calc PR A 2 H6X2 H 0.9191 0.8411 0.5534 0.085 Uiso 0.67(5) 1 calc PR A 2 H6X3 H 1.1297 0.8070 0.5905 0.085 Uiso 0.67(5) 1 calc PR A 2 C7X C 0.984(5) 0.7149(19) 0.6884(13) 0.055(6) Uani 0.67(5) 1 d PDU A 2 H7X1 H 0.9795 0.7578 0.7270 0.083 Uiso 0.67(5) 1 calc PR A 2 H7X2 H 1.1305 0.7048 0.6744 0.083 Uiso 0.67(5) 1 calc PR A 2 H7X3 H 0.9224 0.6607 0.7053 0.083 Uiso 0.67(5) 1 calc PR A 2 C8X C 0.859(6) 0.6765(17) 0.5718(15) 0.054(6) Uani 0.67(5) 1 d PDU A 2 H8X1 H 0.7808 0.6272 0.5909 0.080 Uiso 0.67(5) 1 calc PR A 2 H8X2 H 1.0021 0.6584 0.5598 0.080 Uiso 0.67(5) 1 calc PR A 2 H8X3 H 0.7892 0.6982 0.5286 0.080 Uiso 0.67(5) 1 calc PR 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 0.0349(3) 0.0457(3) 0.0478(4) -0.0016(2) 0.0052(4) -0.0001(2) Au2 0.0341(3) 0.0450(3) 0.0431(3) 0.0011(2) 0.0009(3) 0.0047(2) Cl1 0.046(2) 0.064(2) 0.054(2) 0.0092(16) -0.001(2) -0.003(2) Cl2 0.061(2) 0.060(2) 0.062(2) -0.0172(18) -0.010(2) 0.018(2) C1 0.041(8) 0.049(8) 0.068(11) 0.012(7) 0.024(9) 0.008(7) N1 0.036(7) 0.052(7) 0.079(10) -0.001(7) 0.022(7) 0.003(5) B1 0.050(11) 0.045(9) 0.055(11) -0.002(8) 0.010(8) 0.006(7) N2 0.027(5) 0.040(5) 0.045(6) -0.003(4) -0.006(6) 0.002(5) C2 0.090(14) 0.077(11) 0.051(10) 0.022(8) 0.039(11) 0.032(11) C3 0.042(9) 0.053(9) 0.067(11) -0.006(8) -0.002(8) -0.013(7) C4 0.058(10) 0.042(8) 0.066(10) -0.015(7) 0.000(8) -0.021(7) C5 0.036(7) 0.042(7) 0.063(10) 0.002(7) 0.001(8) 0.002(7) N3 0.039(7) 0.054(7) 0.050(7) 0.002(6) -0.002(7) 0.010(6) B2 0.042(10) 0.070(11) 0.086(16) -0.015(11) -0.024(11) -0.014(9) N4 0.039(6) 0.038(5) 0.051(6) 0.002(4) 0.000(5) -0.003(5) C6 0.06(2) 0.041(17) 0.07(2) 0.002(15) 0.000(19) -0.015(14) C7 0.06(2) 0.056(18) 0.040(14) 0.014(13) 0.009(17) -0.012(16) C8 0.048(19) 0.030(18) 0.043(10) 0.013(10) -0.002(18) 0.000(19) C6X 0.056(15) 0.045(10) 0.069(18) 0.010(9) 0.007(12) -0.002(9) C7X 0.057(16) 0.047(14) 0.061(11) 0.008(8) -0.004(9) 0.014(11) C8X 0.060(14) 0.044(11) 0.057(12) -0.005(9) 0.011(13) 0.008(13) _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 C1 1.936(17) . ? Au1 Cl1 2.273(4) . ? Au1 Au2 3.1911(8) 1_455 ? Au1 Au2 3.2055(8) . ? Au2 C5 1.972(16) . ? Au2 Cl2 2.270(4) . ? Au2 Au1 3.1911(8) 1_655 ? C1 N1 1.14(2) . ? N1 B1 1.54(2) . ? B1 N2 1.60(2) . ? N2 C2 1.471(19) . ? N2 C4 1.485(17) . ? N2 C3 1.494(19) . ? C5 N3 1.115(18) . ? N3 B2 1.49(2) . ? B2 N4 1.58(2) . ? N4 C7 1.44(3) . ? N4 C7X 1.45(2) . ? N4 C6 1.48(2) . ? N4 C6X 1.489(17) . ? N4 C8X 1.493(17) . ? N4 C8 1.50(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 C1 Au1 Cl1 177.8(5) . . ? C1 Au1 Au2 88.5(5) . 1_455 ? Cl1 Au1 Au2 89.47(12) . 1_455 ? C1 Au1 Au2 93.8(5) . . ? Cl1 Au1 Au2 88.07(12) . . ? Au2 Au1 Au2 171.05(2) 1_455 . ? C5 Au2 Cl2 177.9(5) . . ? C5 Au2 Au1 85.5(5) . 1_655 ? Cl2 Au2 Au1 92.79(13) . 1_655 ? C5 Au2 Au1 88.0(5) . . ? Cl2 Au2 Au1 93.78(13) . . ? Au1 Au2 Au1 171.05(2) 1_655 . ? N1 C1 Au1 177.9(14) . . ? C1 N1 B1 178.5(15) . . ? N1 B1 N2 107.8(12) . . ? C2 N2 C4 110.1(13) . . ? C2 N2 C3 110.8(15) . . ? C4 N2 C3 107.0(11) . . ? C2 N2 B1 105.4(12) . . ? C4 N2 B1 112.1(12) . . ? C3 N2 B1 111.5(12) . . ? N3 C5 Au2 176.7(14) . . ? C5 N3 B2 179.0(16) . . ? N3 B2 N4 112.3(13) . . ? C7 N4 C7X 30.6(18) . . ? C7 N4 C6 109(2) . . ? C7X N4 C6 79(2) . . ? C7 N4 C6X 136(2) . . ? C7X N4 C6X 106.9(15) . . ? C6 N4 C6X 28(2) . . ? C7 N4 C8X 86(2) . . ? C7X N4 C8X 108.5(14) . . ? C6 N4 C8X 123(3) . . ? C6X N4 C8X 110.4(17) . . ? C7 N4 C8 106.2(19) . . ? C7X N4 C8 124(2) . . ? C6 N4 C8 110(2) . . ? C6X N4 C8 92(2) . . ? C8X N4 C8 20.7(15) . . ? C7 N4 B2 104(2) . . ? C7X N4 B2 113.9(16) . . ? C6 N4 B2 118(3) . . ? C6X N4 B2 107.7(15) . . ? C8X N4 B2 109.4(17) . . ? C8 N4 B2 109(3) . . ? 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 C1 Au1 Au2 C5 119.2(6) . . . . ? Cl1 Au1 Au2 C5 -62.0(4) . . . . ? Au2 Au1 Au2 C5 -136.1(5) 1_455 . . . ? C1 Au1 Au2 Cl2 -61.9(5) . . . . ? Cl1 Au1 Au2 Cl2 116.99(15) . . . . ? Au2 Au1 Au2 Cl2 42.9(3) 1_455 . . . ? C1 Au1 Au2 Au1 75.3(5) . . . 1_655 ? Cl1 Au1 Au2 Au1 -105.9(2) . . . 1_655 ? Au2 Au1 Au2 Au1 180.0 1_455 . . 1_655 ? Cl1 Au1 C1 N1 -16(58) . . . . ? Au2 Au1 C1 N1 -39(46) 1_455 . . . ? Au2 Au1 C1 N1 132(46) . . . . ? Au1 C1 N1 B1 -15(100) . . . . ? C1 N1 B1 N2 18(69) . . . . ? N1 B1 N2 C2 -174.6(15) . . . . ? N1 B1 N2 C4 -54.7(17) . . . . ? N1 B1 N2 C3 65.1(16) . . . . ? Cl2 Au2 C5 N3 -53(37) . . . . ? Au1 Au2 C5 N3 -89(28) 1_655 . . . ? Au1 Au2 C5 N3 97(28) . . . . ? Au2 C5 N3 B2 161(91) . . . . ? C5 N3 B2 N4 -68(100) . . . . ? N3 B2 N4 C7 78(3) . . . . ? N3 B2 N4 C7X 47(2) . . . . ? N3 B2 N4 C6 -43(4) . . . . ? N3 B2 N4 C6X -71(2) . . . . ? N3 B2 N4 C8X 168.6(19) . . . . ? N3 B2 N4 C8 -169(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.320 _refine_diff_density_min -2.221 _refine_diff_density_rms 0.499 data_cr71 _database_code_depnum_ccdc_archive 'CCDC 247204' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H11 Au B Br N2' _chemical_formula_sum 'C4 H11 Au B Br N2' _chemical_formula_weight 374.83 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' B B 0.0013 0.0007 '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' Br Br -0.2901 2.4595 '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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.4334(3) _cell_length_b 15.8549(7) _cell_length_c 18.7149(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1908.94(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7728 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 29.00 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 19.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.041 _exptl_absorpt_correction_T_max 0.696 _exptl_absorpt_process_details 'SADABS v.2.03, Sheldrick, G.M. (2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16755 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 29.00 _reflns_number_total 4648 _reflns_number_gt 4088 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0435P)^2^+0.5875P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.503(16) _refine_ls_number_reflns 4648 _refine_ls_number_parameters 195 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.047 _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 0.88096(4) 0.064679(16) 0.153200(14) 0.03421(8) Uani 1 1 d . . . Au2 Au 0.37999(4) 0.050447(15) 0.159581(13) 0.03224(8) Uani 1 1 d . . . Br1 Br 0.87324(12) 0.00419(5) 0.26998(4) 0.04392(18) Uani 1 1 d . . . Br2 Br 0.37747(13) -0.04746(5) 0.06255(5) 0.0504(2) Uani 1 1 d . . . C1 C 0.8959(11) 0.1121(5) 0.0572(4) 0.0382(17) Uani 1 1 d . . . N1 N 0.9137(9) 0.1384(4) 0.0002(4) 0.0403(14) Uani 1 1 d . . . B1 B 0.9394(13) 0.1738(6) -0.0751(5) 0.041(2) Uani 1 1 d . . . H1A H 0.9687 0.2350 -0.0731 0.049 Uiso 1 1 calc R . . H1B H 0.8104 0.1650 -0.1030 0.049 Uiso 1 1 calc R . . N2 N 1.1274(9) 0.1254(3) -0.1116(3) 0.0346(13) Uani 1 1 d . . . C2 C 1.1365(16) 0.1535(6) -0.1873(5) 0.059(2) Uani 1 1 d . . . H2A H 1.2559 0.1271 -0.2109 0.088 Uiso 1 1 calc R . . H2B H 1.1512 0.2150 -0.1890 0.088 Uiso 1 1 calc R . . H2C H 1.0083 0.1368 -0.2118 0.088 Uiso 1 1 calc R . . C3 C 1.3291(12) 0.1456(6) -0.0755(5) 0.053(2) Uani 1 1 d . . . H3A H 1.3229 0.1277 -0.0254 0.080 Uiso 1 1 calc R . . H3B H 1.3540 0.2066 -0.0777 0.080 Uiso 1 1 calc R . . H3C H 1.4425 0.1159 -0.0997 0.080 Uiso 1 1 calc R . . C4 C 1.1003(12) 0.0317(5) -0.1102(4) 0.0400(16) Uani 1 1 d . . . H4A H 1.2175 0.0048 -0.1347 0.060 Uiso 1 1 calc R . . H4B H 0.9704 0.0166 -0.1344 0.060 Uiso 1 1 calc R . . H4C H 1.0952 0.0122 -0.0605 0.060 Uiso 1 1 calc R . . C5 C 0.3747(11) 0.1265(4) 0.2426(4) 0.0333(15) Uani 1 1 d . . . N3 N 0.3699(10) 0.1675(4) 0.2921(3) 0.0376(13) Uani 1 1 d . . . B2 B 0.3709(16) 0.2150(8) 0.3615(6) 0.065(3) Uani 1 1 d . A . H2D H 0.4746 0.2610 0.3594 0.078 Uiso 1 1 calc R . . H2E H 0.4099 0.1765 0.4009 0.078 Uiso 1 1 calc R . . N4 N 0.1453(9) 0.2534(3) 0.3760(3) 0.0329(13) Uani 1 1 d D . . C6 C -0.025(2) 0.1928(11) 0.3739(10) 0.050(5) Uani 0.62(2) 1 d PD A 1 H6A H -0.0016 0.1489 0.4098 0.075 Uiso 0.62(2) 1 calc PR A 1 H6B H -0.0318 0.1670 0.3263 0.075 Uiso 0.62(2) 1 calc PR A 1 H6C H -0.1563 0.2218 0.3840 0.075 Uiso 0.62(2) 1 calc PR A 1 C7 C 0.128(3) 0.3240(9) 0.3253(7) 0.050(5) Uani 0.62(2) 1 d PD A 1 H7A H 0.2488 0.3612 0.3305 0.075 Uiso 0.62(2) 1 calc PR A 1 H7B H 0.0007 0.3559 0.3352 0.075 Uiso 0.62(2) 1 calc PR A 1 H7C H 0.1232 0.3020 0.2764 0.075 Uiso 0.62(2) 1 calc PR A 1 C8 C 0.153(2) 0.2912(10) 0.4499(6) 0.035(3) Uani 0.62(2) 1 d PD A 1 H8A H 0.1622 0.2459 0.4855 0.053 Uiso 0.62(2) 1 calc PR A 1 H8B H 0.0276 0.3245 0.4584 0.053 Uiso 0.62(2) 1 calc PR A 1 H8C H 0.2759 0.3276 0.4540 0.053 Uiso 0.62(2) 1 calc PR A 1 C6X C 0.037(4) 0.1772(11) 0.4038(15) 0.042(6) Uani 0.38(2) 1 d PD A 2 H6X1 H 0.0465 0.1317 0.3685 0.063 Uiso 0.38(2) 1 calc PR A 2 H6X2 H -0.1091 0.1906 0.4128 0.063 Uiso 0.38(2) 1 calc PR A 2 H6X3 H 0.1032 0.1591 0.4484 0.063 Uiso 0.38(2) 1 calc PR A 2 C7X C 0.013(3) 0.2795(17) 0.3114(9) 0.045(7) Uani 0.38(2) 1 d PD A 2 H7X1 H 0.0218 0.2357 0.2745 0.068 Uiso 0.38(2) 1 calc PR A 2 H7X2 H 0.0658 0.3328 0.2921 0.068 Uiso 0.38(2) 1 calc PR A 2 H7X3 H -0.1316 0.2865 0.3262 0.068 Uiso 0.38(2) 1 calc PR A 2 C8X C 0.132(4) 0.3233(13) 0.4273(12) 0.043(6) Uani 0.38(2) 1 d PD A 2 H8X1 H 0.2088 0.3720 0.4088 0.064 Uiso 0.38(2) 1 calc PR A 2 H8X2 H 0.1919 0.3058 0.4731 0.064 Uiso 0.38(2) 1 calc PR A 2 H8X3 H -0.0142 0.3389 0.4343 0.064 Uiso 0.38(2) 1 calc PR 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 0.03022(15) 0.03524(14) 0.03717(16) -0.00138(12) 0.00530(15) 0.00085(12) Au2 0.02887(14) 0.03743(14) 0.03042(15) 0.00009(11) 0.00139(14) 0.00555(12) Br1 0.0352(4) 0.0543(4) 0.0422(4) 0.0057(3) 0.0008(4) -0.0036(4) Br2 0.0528(5) 0.0541(5) 0.0445(4) -0.0145(3) -0.0095(4) 0.0181(4) C1 0.027(4) 0.036(4) 0.052(5) -0.010(3) 0.010(4) 0.008(3) N1 0.038(3) 0.040(3) 0.043(4) -0.002(3) 0.003(3) 0.009(3) B1 0.034(4) 0.046(5) 0.043(5) 0.005(4) 0.008(4) 0.010(4) N2 0.028(3) 0.037(3) 0.039(3) 0.005(2) 0.005(3) 0.004(3) C2 0.059(6) 0.069(6) 0.049(5) 0.018(4) 0.017(5) 0.013(5) C3 0.039(5) 0.048(5) 0.072(6) -0.012(4) 0.000(4) -0.005(4) C4 0.041(4) 0.035(3) 0.045(4) -0.010(3) -0.006(4) -0.003(3) C5 0.022(3) 0.040(4) 0.038(4) 0.004(3) 0.006(3) -0.004(3) N3 0.031(3) 0.046(3) 0.036(3) -0.007(3) 0.003(3) 0.000(3) B2 0.035(5) 0.086(8) 0.074(7) -0.032(6) -0.001(6) 0.010(6) N4 0.033(3) 0.036(3) 0.029(3) 0.000(2) 0.005(3) 0.002(3) C6 0.028(8) 0.082(12) 0.039(10) -0.023(9) -0.007(6) -0.012(8) C7 0.056(10) 0.058(9) 0.037(7) 0.019(6) 0.012(7) 0.025(8) C8 0.043(8) 0.030(7) 0.033(7) -0.006(6) -0.002(6) 0.006(6) C6X 0.026(12) 0.058(14) 0.043(16) -0.006(12) 0.012(11) -0.008(10) C7X 0.029(12) 0.062(16) 0.044(13) 0.007(12) 0.005(10) 0.012(11) C8X 0.057(14) 0.033(12) 0.039(13) 0.007(10) -0.014(12) 0.004(12) _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 C1 1.949(8) . ? Au1 Br1 2.3871(8) . ? Au1 Au2 3.2206(4) 1_655 ? Au1 Au2 3.2331(4) . ? Au2 C5 1.967(8) . ? Au2 Br2 2.3890(9) . ? Au2 Au1 3.2206(4) 1_455 ? C1 N1 1.152(10) . ? N1 B1 1.526(11) . ? B1 N2 1.586(10) . ? N2 C2 1.486(10) . ? N2 C3 1.497(10) . ? N2 C4 1.497(9) . ? C5 N3 1.132(9) . ? N3 B2 1.501(12) . ? B2 N4 1.597(12) . ? N4 C6 1.458(11) . ? N4 C8X 1.469(13) . ? N4 C7 1.473(12) . ? N4 C6X 1.487(14) . ? N4 C8 1.508(10) . ? N4 C7X 1.535(16) . ? 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 C1 Au1 Br1 178.1(2) . . ? C1 Au1 Au2 90.7(2) . 1_655 ? Br1 Au1 Au2 87.63(2) . 1_655 ? C1 Au1 Au2 96.3(2) . . ? Br1 Au1 Au2 85.26(2) . . ? Au2 Au1 Au2 170.924(12) 1_655 . ? C5 Au2 Br2 176.96(18) . . ? C5 Au2 Au1 88.2(2) . 1_455 ? Br2 Au2 Au1 90.61(2) . 1_455 ? C5 Au2 Au1 90.2(2) . . ? Br2 Au2 Au1 91.38(2) . . ? Au1 Au2 Au1 170.924(12) 1_455 . ? N1 C1 Au1 176.8(7) . . ? C1 N1 B1 179.4(9) . . ? N1 B1 N2 107.6(6) . . ? C2 N2 C3 109.4(7) . . ? C2 N2 C4 108.5(6) . . ? C3 N2 C4 107.8(6) . . ? C2 N2 B1 107.2(6) . . ? C3 N2 B1 111.3(6) . . ? C4 N2 B1 112.5(6) . . ? N3 C5 Au2 177.2(6) . . ? C5 N3 B2 174.6(8) . . ? N3 B2 N4 109.6(7) . . ? C6 N4 C8X 118.1(13) . . ? C6 N4 C7 115.2(9) . . ? C8X N4 C7 81.0(11) . . ? C6 N4 C6X 28.8(9) . . ? C8X N4 C6X 110.9(13) . . ? C7 N4 C6X 143.9(12) . . ? C6 N4 C8 108.3(9) . . ? C8X N4 C8 26.2(8) . . ? C7 N4 C8 107.0(8) . . ? C6X N4 C8 91.1(12) . . ? C6 N4 C7X 74.9(11) . . ? C8X N4 C7X 106.2(11) . . ? C7 N4 C7X 41.0(9) . . ? C6X N4 C7X 103.6(12) . . ? C8 N4 C7X 129.5(10) . . ? C6 N4 B2 115.3(9) . . ? C8X N4 B2 116.9(12) . . ? C7 N4 B2 104.4(9) . . ? C6X N4 B2 100.0(11) . . ? C8 N4 B2 106.0(8) . . ? C7X N4 B2 118.1(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 C1 Au1 Au2 C5 -119.7(3) . . . . ? Br1 Au1 Au2 C5 61.41(19) . . . . ? Au2 Au1 Au2 C5 100.0(2) 1_655 . . . ? C1 Au1 Au2 Br2 62.9(2) . . . . ? Br1 Au1 Au2 Br2 -116.00(3) . . . . ? Au2 Au1 Au2 Br2 -77.43(9) 1_655 . . . ? C1 Au1 Au2 Au1 -39.6(2) . . . 1_455 ? Br1 Au1 Au2 Au1 141.43(9) . . . 1_455 ? Au2 Au1 Au2 Au1 180.0 1_655 . . 1_455 ? Br1 Au1 C1 N1 -7(19) . . . . ? Au2 Au1 C1 N1 22(13) 1_655 . . . ? Au2 Au1 C1 N1 -153(13) . . . . ? Au1 C1 N1 B1 -56(90) . . . . ? C1 N1 B1 N2 71(84) . . . . ? N1 B1 N2 C2 173.9(7) . . . . ? N1 B1 N2 C3 -66.5(8) . . . . ? N1 B1 N2 C4 54.7(9) . . . . ? Br2 Au2 C5 N3 15(18) . . . . ? Au1 Au2 C5 N3 82(14) 1_455 . . . ? Au1 Au2 C5 N3 -107(14) . . . . ? Au2 C5 N3 B2 32(21) . . . . ? C5 N3 B2 N4 -125(8) . . . . ? N3 B2 N4 C6 54.1(13) . . . . ? N3 B2 N4 C8X -160.4(13) . . . . ? N3 B2 N4 C7 -73.4(11) . . . . ? N3 B2 N4 C6X 79.8(14) . . . . ? N3 B2 N4 C8 173.8(9) . . . . ? N3 B2 N4 C7X -31.7(16) . . . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.830 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.198