Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_structure _database_code_CSD 170528 _audit_creation_date 01-04-11 _audit_creation_method 'SHELXL-97 and manual editing' _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Dietzel, Pascal D. C.' ; Max-Planck-Institut fur Festkorperforschung Heisenbergstr. 1 D-70569 Stuttgart Germany ; 'Jansen, Martin' ; Max-Planck-Institut fur Festkorperforschung Heisenbergstr. 1 D-70569 Stuttgart Germany ; _publ_contact_author_name 'Prof Martin Jansen' _publ_contact_author_address ; Max-Planck-Institut fur Festkorperforschung Heisenbergstr. 1 D-70569 Stuttgart Germany ; _publ_contact_author_email 'martin@jansen.mpi-stuttgart.mpg.de' _publ_contact_author_phone '+49-711-6891501' _publ_contact_author_fax '+49-711-6891502' _publ_requested_journal 'Chem. Commun.' _publ_section_title ; Synthesis and Crystal Structure Determination of Tetramethylammonium Auride ; _chemical_name_systematic 'tetramethylammonium auride' _chemical_formula_sum 'C4 H12 Au N' _chemical_formula_weight 271.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0015 0.0009 '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' 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -0.7638 5.9978 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n m m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z' '-y, -x, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z' '-x-1/2, y, z' '-y-1/2, -x-1/2, z' 'y, x, z' _cell_length_a 7.599(3) _cell_length_b 7.599(3) _cell_length_c 5.433(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 313.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 3190 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 25.6 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.034 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 244 _exptl_absorpt_coefficient_mu 12.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.532 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details 'Blessing, R.H., Acta Cryst. 1995, A51, 33' _exptl_special_details ? _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.56085 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2395 _diffrn_reflns_av_R_equivalents 'see _refine_special_details' _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 23.45 _reflns_number_total 296 _reflns_number_gt 278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software, Darmstadt 1998' _computing_cell_refinement 'Stoe IPDS software, Darmstadt 1998' _computing_data_reduction 'Stoe IPDS software, Darmstadt 1998' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Crystal Impact, 2000)' _computing_publication_material 'CIFTAB (Sheldrick 1993)' _refine_special_details ; The refinement is based on data from a crystal twinned by reticular merohedry (twin law -0.5 -0.5 1 0.5 0.5 1 -0.5 0.5 0, BASF 0.352(1)). A total of 7722 reflections was measured up to 2theta = 52.1 with 4773 belonging to the first domain, and 4774 to the second domain. The data of the domains was individually corrected for absorption and merged in space group P-1 with R(int) = 0.0501 and 0.0705, respectively. These datasets with 2231 and 2235 intensities respectively were combined. The resulting dataset contained 3619 reflections independent for P-1. It was processed in SHELX by using the HKLF 5 command. The dataset was cut-off at 2theta = 47 to give 2395 reflections. 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^)+(0.0629P)^2^+8.0501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary vecmap _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2395 _refine_ls_number_parameters 20 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 0.7500 0.7500 0.36566(8) 0.01677(12) Uani 1 8 d S . . N N 0.7500 1.2500 1.0000 0.0163(18) Uani 1 8 d S . . C C 0.7500 1.0912(7) 0.8420(11) 0.0194(10) Uani 1 2 d SD . . H1 H 0.854(5) 1.088(9) 0.735(10) 0.024(14) Uiso 1 1 d D . . H2 H 0.7500 0.997(14) 0.955(18) 0.03(2) 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 Au 0.01707(14) 0.01707(14) 0.01618(19) 0.000 0.000 0.000 N 0.016(3) 0.016(3) 0.016(5) 0.000 0.000 0.000 C 0.022(2) 0.013(2) 0.023(3) 0.0009(18) 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 N C 1.481(6) . ? N C 1.481(6) 12_767 ? N C 1.481(6) 2_675 ? N C 1.481(6) 11_577 ? C H1 0.982(19) . ? C H2 0.94(11) . ? 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 N C 109.6(2) . 12_767 ? C N C 109.1(5) . 2_675 ? C N C 109.6(2) 12_767 2_675 ? C N C 109.6(2) . 11_577 ? C N C 109.1(5) 12_767 11_577 ? C N C 109.6(2) 2_675 11_577 ? N C H1 111(4) . . ? N C H2 104(6) . . ? H1 C H2 111(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.45 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 4.223 _refine_diff_density_min -3.690 _refine_diff_density_rms 0.327