Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _audit_creation_method Xtal3.6 _audit_creation_date 03-07-31 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_coden_Cambridge 222 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Murray Baker' _publ_contact_author_address ; Department of Chemistry M313 University of Western Australia 35 Stirling Highway Crawley WA 6009 AUSTRALIA ; _publ_contact_author_email MVB@CHEM.UWA.EDU.AU _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; Synthetic, structural and spectroscopic studies of (pseudo)halo(1,3-di-tert-butylimidazol-2-ylidine)gold complexes ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name 'Murray Baker' 'Peter J. Barnard' 'Simon K. Brayshaw' 'James L. Hickey' 'Brian W. Skelton' 'Allan H. White' _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_jlh104 _database_code_depnum_ccdc_archive 'CCDC 247531' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C11 H20 Au1 Cl1 N2' _chemical_formula_moiety ? _chemical_formula_weight 412.71 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.1345(8) _cell_length_b 11.7348(9) _cell_length_c 11.0707(8) _cell_angle_alpha 90.00000 _cell_angle_beta 107.605(2) _cell_angle_gamma 90.00000 _cell_volume 1378.76(18) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8422 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 37.3 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 10.838 _exptl_crystal_description bar _exptl_crystal_size_max .26 _exptl_crystal_size_mid .06 _exptl_crystal_size_min .05 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .53 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 14240 _reflns_number_total 3611 _reflns_Friedel_coverage 0 _reflns_number_gt 3319 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 37.5 _diffrn_reflns_theta_full 37.5 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full .99 _diffrn_reflns_av_R_equivalents .030 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .02 _refine_ls_wR_factor_ref .024 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_number_reflns 3319 _refine_ls_number_parameters 70 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .007 _refine_diff_density_min -1.07 _refine_diff_density_max 2.374 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 44 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 80 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 4 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 4 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .50000 .285066(8) .25000 .02132(4) Uani ? ? 1.00000 ? ? Cl .50000 .09127(6) .25000 .0327(3) Uani ? ? 1.00000 ? ? C1 .50000 .4570(2) .25000 .0240(9) Uani ? ? 1.00000 ? ? N2 .41080(15) .52433(13) .17529(15) .0256(6) Uani ? ? 1.00000 ? ? C21 .29418(17) .48559(17) .07242(18) .0270(7) Uani ? ? 1.00000 ? ? C22 .21371(18) .4102(2) .1299(2) .0328(8) Uani ? ? 1.00000 ? ? C23 .33535(19) .4218(2) -.02836(18) .0310(8) Uani ? ? 1.00000 ? ? C24 .2173(2) .5901(2) .0135(2) .0386(9) Uani ? ? 1.00000 ? ? C3 .4446(2) .63658(17) .2037(2) .0312(8) Uani ? ? 1.00000 ? ? H22a .18949 .45143 .19260 .04900 Uiso ? ? 1.00000 ? ? H22b .26088 .34465 .16804 .04900 Uiso ? ? 1.00000 ? ? H22c .14036 .38605 .06534 .04900 Uiso ? ? 1.00000 ? ? H23a .38558 .47073 -.06306 .04600 Uiso ? ? 1.00000 ? ? H23b .26360 .39803 -.09544 .04600 Uiso ? ? 1.00000 ? ? H23c .38412 .35663 .00726 .04600 Uiso ? ? 1.00000 ? ? H24a .26688 .63816 -.02308 .05900 Uiso ? ? 1.00000 ? ? H24b .19384 .63205 .07591 .05900 Uiso ? ? 1.00000 ? ? H24c .14373 .56742 -.05175 .05900 Uiso ? ? 1.00000 ? ? H3 .39723 .70233 .16470 .03900 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .01920(4) .02023(5) .02134(5) .00000 .00133(3) .00000 Cl .0260(3) .0230(3) .0401(3) .00000 -.0037(2) .00000 C1 .0248(10) .0213(11) .0223(10) .00000 .0017(8) .00000 N2 .0260(7) .0204(6) .0244(7) .0012(5) -.0012(5) -.0003(5) C21 .0228(7) .0263(8) .0254(8) .0021(6) -.0026(6) -.0000(6) C22 .0229(8) .0338(10) .0378(10) .0003(7) .0032(7) -.0007(8) C23 .0292(8) .0347(10) .0230(8) -.0002(7) -.0013(6) -.0028(7) C24 .0349(10) .0289(10) .0393(11) .0049(7) -.0081(8) .0016(8) C3 .0339(9) .0200(8) .0313(9) .0004(7) -.0029(7) .0004(7) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au Cl . . 2.2742(7) ? Au C1 . . 2.018(3) ? C1 N2 . . 1.341(2) ? C1 N2 . '2 655' 1.341(2) ? N2 C21 . . 1.515(2) ? N2 C3 . . 1.380(2) ? C21 C22 . . 1.528(3) ? C21 C23 . . 1.525(3) ? C21 C24 . . 1.524(3) ? C22 H22a . . .949 ? C22 H22b . . .955 ? C22 H22c . . .9517 ? C23 H23a . . .959 ? C23 H23b . . .9532 ? C23 H23c . . .952 ? C24 H24a . . .960 ? C24 H24b . . .948 ? C24 H24c . . .952 ? C3 H3 . . .960 ? C3 C3 . '2 655' 1.344(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Cl Au C1 . . . 180.0000 ? Au C1 N2 . . . 126.10(11) ? Au C1 N2 . . '2 655' 126.10(11) ? N2 C1 N2 . . '2 655' 107.8(2) ? C1 N2 C21 . . . 126.41(16) ? C1 N2 C3 . . . 108.76(15) ? C21 N2 C3 . . . 124.79(15) ? N2 C21 C22 . . . 109.73(16) ? N2 C21 C23 . . . 108.56(16) ? N2 C21 C24 . . . 108.84(16) ? C22 C21 C23 . . . 111.38(17) ? C22 C21 C24 . . . 108.66(18) ? C23 C21 C24 . . . 109.62(17) ? C21 C22 H22a . . . 110.0 ? C21 C22 H22b . . . 109.7 ? C21 C22 H22c . . . 109.7 ? H22a C22 H22b . . . 109.1 ? H22a C22 H22c . . . 109.4 ? H22b C22 H22c . . . 108.9 ? C21 C23 H23a . . . 109.9 ? C21 C23 H23b . . . 110.3 ? C21 C23 H23c . . . 110.58 ? H23a C23 H23b . . . 108.4 ? H23a C23 H23c . . . 108.6 ? H23b C23 H23c . . . 109.1 ? C21 C24 H24a . . . 109.5 ? C21 C24 H24b . . . 110.4 ? C21 C24 H24c . . . 110.1 ? H24a C24 H24b . . . 108.8 ? H24a C24 H24c . . . 108.5 ? H24b C24 H24c . . . 109.5 ? N2 C3 H3 . . . 126.11 ? N2 C3 C3 . . '2 655' 107.34(17) ? H3 C3 C3 . . '2 655' 126.6 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 784 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -18 _reflns_limit_l_max 18 _reflns_number_observed ? _reflns_d_resolution_high .584 _reflns_d_resolution_low 7.859 _diffrn_reflns_av_sigmaI/netI .025 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .024 _refine_ls_wR_factor_all .024 _refine_ls_goodness_of_fit_all 1.015 _refine_ls_shift/su_mean .0002 #===END data_sbz006 _database_code_depnum_ccdc_archive 'CCDC 247532' _audit_creation_method Xtal3.6 _audit_creation_date 04-01-01 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C15 H28 Au1 Br1 N2 O1' _chemical_formula_moiety 'C11 H20 Au1 Br1 N2, C4 H8 O' _chemical_formula_weight 529.27 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_b_c_a _symmetry_space_group_name_Hall -p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,+z +x,1/2-y,1/2+z _cell_length_a 16.799(4) _cell_length_b 12.289(3) _cell_length_c 17.633(4) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 3640.2(15) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5231 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.04 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 10.277 _exptl_crystal_description slab _exptl_crystal_size_max .12 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .06 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .36 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 26197 _reflns_number_total 3217 _reflns_Friedel_coverage 0 _reflns_number_gt 2117 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 25.07 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .09 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .048 _refine_ls_wR_factor_ref .059 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_number_reflns 2117 _refine_ls_number_parameters 181 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .001 _refine_diff_density_min -2.369 _refine_diff_density_max 2.268 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 120 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 224 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 8 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 8 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 8 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .09232(3) .68487(4) .38610(2) .0202(3) Uani ? ? 1.00000 ? ? Br .08182(8) .54749(10) .28999(7) .0288(7) Uani ? ? 1.00000 ? ? C1 .1000(7) .8007(10) .4636(8) .025(7) Uani ? ? 1.00000 ? ? N2 .1299(6) .9037(8) .4563(6) .023(6) Uani ? ? 1.00000 ? ? C21 .1693(8) .9478(10) .3860(7) .028(7) Uani ? ? 1.00000 ? ? C22 .1053(8) .9502(10) .3240(7) .030(8) Uani ? ? 1.00000 ? ? C23 .2395(9) .8756(10) .3635(8) .037(9) Uani ? ? 1.00000 ? ? C24 .1966(9) 1.0622(10) .4011(8) .033(8) Uani ? ? 1.00000 ? ? C3 .1220(8) .9611(10) .5234(6) .023(7) Uani ? ? 1.00000 ? ? C4 .0885(8) .8930(10) .5757(7) .026(7) Uani ? ? 1.00000 ? ? N5 .0761(6) .7942(7) .5385(6) .022(6) Uani ? ? 1.00000 ? ? C51 .0405(8) .6961(9) .5758(7) .022(7) Uani ? ? 1.00000 ? ? C52 -.0336(8) .6600(10) .5350(7) .028(8) Uani ? ? 1.00000 ? ? C53 .1020(8) .6048(10) .5761(9) .032(8) Uani ? ? 1.00000 ? ? C54 .0197(9) .7261(11) .6571(7) .033(8) Uani ? ? 1.00000 ? ? O01 -.1680(6) .7989(7) .4173(5) .038(6) Uani ? ? 1.00000 ? ? C02 -.1239(11) .8134(12) .3474(9) .048(10) Uani ? ? 1.00000 ? ? C03 -.1420(9) .7169(13) .2979(8) .042(9) Uani ? ? 1.00000 ? ? C04 -.2233(10) .6718(11) .3304(9) .050(10) Uani ? ? 1.00000 ? ? C05 -.2093(9) .7020(10) .4132(8) .034(8) Uani ? ? 1.00000 ? ? H22a .06143 .99600 .33935 .04600 Uiso ? ? 1.00000 ? ? H22b .08507 .87959 .31384 .04600 Uiso ? ? 1.00000 ? ? H22c .12652 .97995 .27795 .04600 Uiso ? ? 1.00000 ? ? H23a .27886 .87505 .40304 .05000 Uiso ? ? 1.00000 ? ? H23b .26423 .90348 .31846 .05000 Uiso ? ? 1.00000 ? ? H23c .22277 .80311 .35435 .05000 Uiso ? ? 1.00000 ? ? H24a .23615 1.06463 .43987 .04700 Uiso ? ? 1.00000 ? ? H24b .15223 1.10680 .41788 .04700 Uiso ? ? 1.00000 ? ? H24c .21764 1.09501 .35632 .04700 Uiso ? ? 1.00000 ? ? H3 .13651 1.03500 .53186 .02800 Uiso ? ? 1.00000 ? ? H4 .07863 .90954 .62798 .03400 Uiso ? ? 1.00000 ? ? H52a -.07275 .71574 .53438 .03800 Uiso ? ? 1.00000 ? ? H52b -.05572 .59649 .55825 .03800 Uiso ? ? 1.00000 ? ? H52c -.02122 .64146 .48290 .03800 Uiso ? ? 1.00000 ? ? H53a .15088 .63000 .60245 .04600 Uiso ? ? 1.00000 ? ? H53b .11913 .58705 .52545 .04600 Uiso ? ? 1.00000 ? ? H53c .08463 .54208 .60080 .04600 Uiso ? ? 1.00000 ? ? H54a .06596 .74971 .68436 .04900 Uiso ? ? 1.00000 ? ? H54b -.00250 .66499 .68372 .04900 Uiso ? ? 1.00000 ? ? H54c -.01875 .78396 .65870 .04900 Uiso ? ? 1.00000 ? ? H02a -.06794 .82047 .35634 .06100 Uiso ? ? 1.00000 ? ? H02b -.14034 .88083 .32151 .06100 Uiso ? ? 1.00000 ? ? H03a -.10089 .66354 .30174 .05300 Uiso ? ? 1.00000 ? ? H03b -.14689 .73697 .24517 .05300 Uiso ? ? 1.00000 ? ? H04a -.22981 .59521 .32161 .06100 Uiso ? ? 1.00000 ? ? H04b -.26877 .70803 .30816 .06100 Uiso ? ? 1.00000 ? ? H05a -.26099 .70881 .43840 .04300 Uiso ? ? 1.00000 ? ? H05b -.18149 .64458 .43799 .04300 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .0318(3) .0148(3) .0140(3) -.0012(2) -.0003(2) -.0013(2) Br .0527(9) .0186(6) .0151(6) -.0007(6) -.0021(6) -.0035(5) C1 .022(7) .021(7) .031(8) .008(6) .004(6) .009(6) N2 .033(7) .011(5) .024(6) -.002(5) .001(5) .001(5) C21 .037(8) .020(7) .027(8) -.004(6) .003(7) .006(6) C22 .056(10) .014(6) .020(7) -.012(6) -.008(6) .006(5) C23 .052(11) .022(7) .036(9) -.000(7) .021(7) .007(6) C24 .048(9) .022(7) .030(8) -.007(7) .007(7) .007(6) C3 .046(8) .017(6) .006(6) .003(6) .006(6) -.002(5) C4 .049(9) .027(7) .002(6) -.002(7) -.001(6) .000(5) N5 .044(7) .007(5) .016(5) -.002(5) -.004(5) .002(4) C51 .032(7) .018(7) .017(7) -.011(6) .002(6) .001(6) C52 .034(8) .025(7) .024(7) -.003(6) -.002(6) .003(5) C53 .044(10) .013(6) .038(8) -.002(6) -.003(7) .006(6) C54 .059(11) .032(7) .008(7) -.002(7) .008(7) -.006(6) O01 .066(8) .020(5) .028(5) -.005(5) .001(5) -.009(4) C02 .073(11) .037(9) .035(9) -.027(9) .014(9) -.002(8) C03 .035(9) .066(11) .025(8) -.011(8) .009(7) -.010(7) C04 .065(11) .037(9) .048(10) .006(9) -.015(9) -.019(8) C05 .039(9) .031(8) .032(8) -.004(7) .008(7) -.004(6) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au Br . . 2.3987(13) ? Au C1 . . 1.977(13) ? C1 N2 . . 1.368(15) ? C1 N5 . . 1.384(16) ? N2 C21 . . 1.507(16) ? N2 C3 . . 1.383(15) ? C21 C22 . . 1.534(18) ? C21 C23 . . 1.53(2) ? C21 C24 . . 1.503(18) ? C22 H22a . . .966 ? C22 H22b . . .949 ? C22 H22c . . .959 ? C23 H23a . . .962 ? C23 H23b . . .960 ? C23 H23c . . .947 ? C24 H24a . . .953 ? C24 H24b . . .972 ? C24 H24c . . .955 ? C3 C4 . . 1.367(17) ? C3 H3 . . .952 ? C4 N5 . . 1.396(15) ? C4 H4 . . .958 ? N5 C51 . . 1.497(15) ? C51 C52 . . 1.505(19) ? C51 C53 . . 1.525(18) ? C51 C54 . . 1.521(18) ? C52 H52a . . .950 ? C52 H52b . . .956 ? C52 H52c . . .969 ? C53 H53a . . .993 ? C53 H53b . . .964 ? C53 H53c . . .932 ? C54 H54a . . .958 ? C54 H54b . . .961 ? C54 H54c . . .961 ? O01 C02 . . 1.45(2) ? O01 C05 . . 1.380(16) ? C02 C03 . . 1.50(2) ? C02 H02a . . .957 ? C02 H02b . . .986 ? C03 C04 . . 1.58(2) ? C03 H03a . . .954 ? C03 H03b . . .966 ? C04 C05 . . 1.52(2) ? C04 H04a . . .960 ? C04 H04b . . .967 ? C05 H05a . . .978 ? C05 H05b . . .952 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Br Au C1 . . . 178.6(4) ? Au C1 N2 . . . 128.7(9) ? Au C1 N5 . . . 126.8(9) ? N2 C1 N5 . . . 104.5(10) ? C1 N2 C21 . . . 124.9(10) ? C1 N2 C3 . . . 110.9(10) ? C21 N2 C3 . . . 124.2(10) ? N2 C21 C22 . . . 106.6(10) ? N2 C21 C23 . . . 110.1(10) ? N2 C21 C24 . . . 108.9(10) ? C22 C21 C23 . . . 111.5(11) ? C22 C21 C24 . . . 108.8(10) ? C23 C21 C24 . . . 110.7(11) ? C21 C22 H22a . . . 110.2 ? C21 C22 H22b . . . 111.6 ? C21 C22 H22c . . . 110.5 ? H22a C22 H22b . . . 108.2 ? H22a C22 H22c . . . 107.4 ? H22b C22 H22c . . . 108.8 ? C21 C23 H23a . . . 110.3 ? C21 C23 H23b . . . 110.0 ? C21 C23 H23c . . . 111.2 ? H23a C23 H23b . . . 107.7 ? H23a C23 H23c . . . 108.7 ? H23b C23 H23c . . . 108.9 ? C21 C24 H24a . . . 111.7 ? C21 C24 H24b . . . 110.3 ? C21 C24 H24c . . . 111.1 ? H24a C24 H24b . . . 107.4 ? H24a C24 H24c . . . 108.8 ? H24b C24 H24c . . . 107.3 ? N2 C3 C4 . . . 107.8(10) ? N2 C3 H3 . . . 126.6 ? C4 C3 H3 . . . 125.6 ? C3 C4 N5 . . . 106.1(10) ? C3 C4 H4 . . . 126.3 ? N5 C4 H4 . . . 127.5 ? C1 N5 C4 . . . 110.7(9) ? C1 N5 C51 . . . 125.6(9) ? C4 N5 C51 . . . 123.7(10) ? N5 C51 C52 . . . 110.9(10) ? N5 C51 C53 . . . 108.9(10) ? N5 C51 C54 . . . 108.1(10) ? C52 C51 C53 . . . 110.2(10) ? C52 C51 C54 . . . 109.4(11) ? C53 C51 C54 . . . 109.3(11) ? C51 C52 H52a . . . 111.4 ? C51 C52 H52b . . . 110.9 ? C51 C52 H52c . . . 110.2 ? H52a C52 H52b . . . 109.0 ? H52a C52 H52c . . . 107.9 ? H52b C52 H52c . . . 107.4 ? C51 C53 H53a . . . 109.4 ? C51 C53 H53b . . . 111.4 ? C51 C53 H53c . . . 113.5 ? H53a C53 H53b . . . 104.9 ? H53a C53 H53c . . . 107.4 ? H53b C53 H53c . . . 109.8 ? C51 C54 H54a . . . 111.0 ? C51 C54 H54b . . . 111.1 ? C51 C54 H54c . . . 111.2 ? H54a C54 H54b . . . 107.9 ? H54a C54 H54c . . . 107.9 ? H54b C54 H54c . . . 107.7 ? C02 O01 C05 . . . 108.6(10) ? O01 C02 C03 . . . 107.1(12) ? O01 C02 H02a . . . 112.0 ? O01 C02 H02b . . . 110.7 ? C03 C02 H02a . . . 111.4 ? C03 C02 H02b . . . 109.7 ? H02a C02 H02b . . . 105.9 ? C02 C03 C04 . . . 103.9(12) ? C02 C03 H03a . . . 110.8 ? C02 C03 H03b . . . 112.1 ? C04 C03 H03a . . . 111.0 ? C04 C03 H03b . . . 111.3 ? H03a C03 H03b . . . 107.7 ? C03 C04 C05 . . . 97.4(12) ? C03 C04 H04a . . . 112.6 ? C03 C04 H04b . . . 112.0 ? C05 C04 H04a . . . 114.2 ? C05 C04 H04b . . . 113.4 ? H04a C04 H04b . . . 107.2 ? O01 C05 C04 . . . 109.7(11) ? O01 C05 H05a . . . 110.3 ? O01 C05 H05b . . . 111.6 ? C04 C05 H05a . . . 108.6 ? C04 C05 H05b . . . 109.6 ? H05a C05 H05b . . . 106.9 ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2032 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .839 _reflns_d_resolution_low 8.801 _diffrn_reflns_av_sigmaI/netI .119 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .098 _refine_ls_wR_factor_all .069 _refine_ls_goodness_of_fit_all 1.012 _refine_ls_shift/su_mean .00007 #===END data_sbx006 _database_code_depnum_ccdc_archive 'CCDC 247533' _audit_creation_method Xtal3.6 _audit_creation_date 03-12-28 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C12 H21 Au1 Br1 Cl3 N2' _chemical_formula_moiety 'C11 H20 Au1 Br1 N2, C H Cl3' _chemical_formula_weight 576.54 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_b_c_a _symmetry_space_group_name_Hall -p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,+z +x,1/2-y,1/2+z _cell_length_a 15.583(2) _cell_length_b 12.6100(10) _cell_length_c 18.461(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 3627.6(7) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 2.111 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5654 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 34.02 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 10.745 _exptl_crystal_description prism _exptl_crystal_size_max .16 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .54 _exptl_absorpt_correction_T_max 1. _diffrn_reflns_number 64933 _reflns_number_total 8007 _reflns_Friedel_coverage 0 _reflns_number_gt 5047 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 35.08 _diffrn_reflns_theta_full 35.08 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .081 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .035 _refine_ls_wR_factor_ref .043 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_number_reflns 5047 _refine_ls_number_parameters 172 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .004 _refine_diff_density_min -1.545 _refine_diff_density_max 1.608 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 96 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 168 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 8 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 8 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 24 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .090615(11) .695856(12) .400665(9) .01721(8) Uani ? ? 1.00000 ? ? Br .06604(3) .58175(4) .29874(3) .0238(2) Uani ? ? 1.00000 ? ? C1 .1060(3) .7946(3) .4843(2) .017(2) Uani ? ? 1.00000 ? ? N2 .1289(2) .8992(3) .4802(2) .0178(17) Uani ? ? 1.00000 ? ? C21 .1545(3) .9566(4) .4122(2) .022(2) Uani ? ? 1.00000 ? ? C22 .0833(4) .9503(4) .3566(3) .032(3) Uani ? ? 1.00000 ? ? C23 .2375(4) .9106(5) .3847(3) .036(3) Uani ? ? 1.00000 ? ? C24 .1672(4) 1.0741(4) .4302(3) .034(3) Uani ? ? 1.00000 ? ? C3 .1287(3) .9424(4) .5493(2) .023(2) Uani ? ? 1.00000 ? ? C4 .1069(3) .8658(4) .5954(2) .023(2) Uani ? ? 1.00000 ? ? N5 .0928(2) .7755(3) .5554(2) .0195(18) Uani ? ? 1.00000 ? ? C51 .0645(3) .6712(4) .5874(2) .022(2) Uani ? ? 1.00000 ? ? C52 -.0247(3) .6460(4) .5595(3) .031(3) Uani ? ? 1.00000 ? ? C53 .1277(4) .5832(4) .5667(3) .030(3) Uani ? ? 1.00000 ? ? C54 .0625(5) .6812(4) .6695(3) .039(3) Uani ? ? 1.00000 ? ? Cl1 -.17184(11) .72799(12) .41663(8) .0408(8) Uani ? ? 1.00000 ? ? Cl2 -.22114(11) .65099(14) .27538(8) .0483(9) Uani ? ? 1.00000 ? ? Cl3 -.13608(11) .85277(13) .28918(9) .0504(9) Uani ? ? 1.00000 ? ? C0 -.1447(4) .7236(4) .3242(3) .032(3) Uani ? ? 1.00000 ? ? H22a .03190 .97967 .37565 .04800 Uiso ? ? 1.00000 ? ? H22b .07296 .87757 .34409 .04800 Uiso ? ? 1.00000 ? ? H22c .09926 .98775 .31402 .04800 Uiso ? ? 1.00000 ? ? H23a .28103 .91556 .42129 .05400 Uiso ? ? 1.00000 ? ? H23b .25628 .94738 .34285 .05400 Uiso ? ? 1.00000 ? ? H23c .22998 .83720 .37292 .05400 Uiso ? ? 1.00000 ? ? H24a .21207 1.08173 .46570 .05200 Uiso ? ? 1.00000 ? ? H24b .11593 1.10335 .44966 .05200 Uiso ? ? 1.00000 ? ? H24c .18322 1.11230 .38803 .05200 Uiso ? ? 1.00000 ? ? H3 .14188 1.01494 .56142 .02800 Uiso ? ? 1.00000 ? ? H4 .10222 .87213 .64678 .02900 Uiso ? ? 1.00000 ? ? H52a -.06422 .70148 .57244 .04800 Uiso ? ? 1.00000 ? ? H52b -.04515 .58106 .57846 .04800 Uiso ? ? 1.00000 ? ? H52c -.02422 .64135 .50737 .04800 Uiso ? ? 1.00000 ? ? H53a .18432 .59992 .58439 .04500 Uiso ? ? 1.00000 ? ? H53b .13165 .57740 .51476 .04500 Uiso ? ? 1.00000 ? ? H53c .11072 .51710 .58585 .04500 Uiso ? ? 1.00000 ? ? H54a .11707 .69681 .68784 .05900 Uiso ? ? 1.00000 ? ? H54b .04164 .61661 .69034 .05900 Uiso ? ? 1.00000 ? ? H54c .02316 .73701 .68301 .05900 Uiso ? ? 1.00000 ? ? H0 -.08941 .68844 .31948 .04100 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .02093(8) .01634(7) .01436(7) -.00142(6) .00029(6) -.00123(6) Br .0346(3) .0194(2) .0174(2) -.00237(18) .00053(19) -.00244(17) C1 .016(2) .021(2) .0153(18) -.0003(16) .0020(14) .0004(15) N2 .0176(18) .0187(17) .0173(16) -.0027(14) .0000(14) -.0018(13) C21 .027(2) .022(2) .018(2) .0013(19) .0016(17) .0037(16) C22 .041(3) .027(2) .028(3) -.002(2) -.005(2) .006(2) C23 .033(3) .031(3) .046(3) -.002(2) .019(2) .011(2) C24 .053(4) .022(2) .027(3) -.010(2) .000(2) -.001(2) C3 .031(3) .020(2) .018(2) -.0027(19) .0033(19) -.0051(16) C4 .037(3) .019(2) .0144(19) -.0047(18) .0002(18) -.0039(16) N5 .022(2) .0197(16) .0164(17) -.0032(15) .0008(15) .0022(14) C51 .028(2) .0185(19) .020(2) -.0081(18) -.0008(18) .0025(16) C52 .029(3) .029(3) .036(3) -.007(2) -.001(2) .008(2) C53 .030(3) .024(2) .037(3) .002(2) -.004(2) .006(2) C54 .064(4) .034(3) .020(2) -.018(3) .002(3) .005(2) Cl1 .0492(9) .0437(8) .0295(7) .0040(7) -.0097(6) -.0012(6) Cl2 .0501(9) .0568(9) .0380(8) -.0150(8) .0065(7) -.0223(7) Cl3 .0540(10) .0463(9) .0509(9) -.0113(8) -.0086(8) .0125(7) C0 .029(3) .033(3) .034(3) .006(2) .002(2) -.001(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au Br . . 2.3994(5) ? Au C1 . . 1.999(4) ? C1 N2 . . 1.368(6) ? C1 N5 . . 1.350(6) ? N2 C21 . . 1.502(6) ? N2 C3 . . 1.387(6) ? C21 C22 . . 1.513(7) ? C21 C23 . . 1.507(8) ? C21 C24 . . 1.532(7) ? C22 H22a . . .950 ? C22 H22b . . .960 ? C22 H22c . . .950 ? C23 H23a . . .959 ? C23 H23b . . .947 ? C23 H23c . . .958 ? C24 H24a . . .963 ? C24 H24b . . .950 ? C24 H24c . . .948 ? C3 C4 . . 1.332(6) ? C3 H3 . . .964 ? C4 N5 . . 1.375(6) ? C4 H4 . . .954 ? N5 C51 . . 1.508(6) ? C51 C52 . . 1.515(8) ? C51 C53 . . 1.532(7) ? C51 C54 . . 1.520(7) ? C52 H52a . . .962 ? C52 H52b . . .946 ? C52 H52c . . .965 ? C53 H53a . . .964 ? C53 H53b . . .964 ? C53 H53c . . .943 ? C54 H54a . . .936 ? C54 H54b . . .957 ? C54 H54c . . .967 ? Cl1 C0 . . 1.760(6) ? Cl2 C0 . . 1.752(6) ? Cl3 C0 . . 1.757(6) ? C0 H0 . . .973 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Br Au C1 . . . 177.30(13) ? Au C1 N2 . . . 126.1(3) ? Au C1 N5 . . . 128.4(3) ? N2 C1 N5 . . . 105.5(4) ? C1 N2 C21 . . . 125.4(4) ? C1 N2 C3 . . . 109.1(4) ? C21 N2 C3 . . . 125.4(4) ? N2 C21 C22 . . . 110.3(4) ? N2 C21 C23 . . . 108.9(4) ? N2 C21 C24 . . . 108.7(4) ? C22 C21 C23 . . . 112.4(4) ? C22 C21 C24 . . . 107.0(4) ? C23 C21 C24 . . . 109.5(4) ? C21 C22 H22a . . . 110.3 ? C21 C22 H22b . . . 109.6 ? C21 C22 H22c . . . 110.1 ? H22a C22 H22b . . . 108.7 ? H22a C22 H22c . . . 109.5 ? H22b C22 H22c . . . 108.6 ? C21 C23 H23a . . . 110.2 ? C21 C23 H23b . . . 110.6 ? C21 C23 H23c . . . 110.1 ? H23a C23 H23b . . . 108.9 ? H23a C23 H23c . . . 108.1 ? H23b C23 H23c . . . 109.0 ? C21 C24 H24a . . . 109.7 ? C21 C24 H24b . . . 110.4 ? C21 C24 H24c . . . 110.4 ? H24a C24 H24b . . . 108.3 ? H24a C24 H24c . . . 108.5 ? H24b C24 H24c . . . 109.6 ? N2 C3 C4 . . . 107.7(4) ? N2 C3 H3 . . . 125.9 ? C4 C3 H3 . . . 126.4 ? C3 C4 N5 . . . 107.3(4) ? C3 C4 H4 . . . 126.4 ? N5 C4 H4 . . . 126.3 ? C1 N5 C4 . . . 110.5(4) ? C1 N5 C51 . . . 125.6(4) ? C4 N5 C51 . . . 123.9(4) ? N5 C51 C52 . . . 108.5(4) ? N5 C51 C53 . . . 110.2(4) ? N5 C51 C54 . . . 108.9(4) ? C52 C51 C53 . . . 110.7(4) ? C52 C51 C54 . . . 109.8(5) ? C53 C51 C54 . . . 108.7(4) ? C51 C52 H52a . . . 110.5 ? C51 C52 H52b . . . 111.4 ? C51 C52 H52c . . . 110.2 ? H52a C52 H52b . . . 108.7 ? H52a C52 H52c . . . 107.2 ? H52b C52 H52c . . . 108.6 ? C51 C53 H53a . . . 110.3 ? C51 C53 H53b . . . 110.2 ? C51 C53 H53c . . . 111.5 ? H53a C53 H53b . . . 107.1 ? H53a C53 H53c . . . 108.8 ? H53b C53 H53c . . . 108.8 ? C51 C54 H54a . . . 111.1 ? C51 C54 H54b . . . 109.7 ? C51 C54 H54c . . . 109.3 ? H54a C54 H54b . . . 110.0 ? H54a C54 H54c . . . 109.2 ? H54b C54 H54c . . . 107.5 ? Cl1 C0 Cl2 . . . 110.6(3) ? Cl1 C0 Cl3 . . . 110.2(3) ? Cl1 C0 H0 . . . 108.3 ? Cl2 C0 Cl3 . . . 110.3(3) ? Cl2 C0 H0 . . . 108.6 ? Cl3 C0 H0 . . . 108.8 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Au N2 3.014(4) . . ? Au C21 3.442(5) . . ? Au C22 3.312(5) . . ? Au C23 3.558(6) . . ? Au N5 3.028(4) . . ? Au C51 3.486(5) . . ? Au C52 3.496(6) . . ? Au C53 3.428(6) . . ? Au Cl1 4.1204(18) . . ? Au Cl2 4.4145(17) . 6 ? Au Cl3 4.5421(18) . . ? Au H22b 2.5332(2) . . ? Au H23c 2.8558(3) . . ? Au H52c 2.7487(3) . . ? Au H53b 2.6602(3) . . ? Au H0 3.1820(4) . . ? Br Cl2 3.6923(18) . 6 ? Br Cl3 3.4875(18) . '4 545' ? Br H4 2.9199(5) . '8 564' ? Br H52b 3.0758(5) . '5 566' ? Br H54b 3.0188(5) . '5 566' ? Br H0 2.7973(6) . . ? C1 C21 2.552(6) . . ? C1 C3 2.243(6) . . ? C1 C4 2.239(6) . . ? C1 C51 2.543(6) . . ? C1 Cl1 3.925(5) . '3 566' ? N2 C22 2.475(7) . . ? N2 C23 2.449(7) . . ? N2 C24 2.465(6) . . ? N2 C4 2.196(6) . . ? N2 N5 2.163(5) . . ? N2 H22a 2.653(4) . . ? N2 H22b 2.674(4) . . ? N2 H23a 2.617(4) . . ? N2 H23c 2.649(4) . . ? N2 H24a 2.655(4) . . ? N2 H24b 2.643(4) . . ? N2 H3 2.102(4) . . ? C21 C3 2.568(6) . . ? C21 H22a 2.046(5) . . ? C21 H22b 2.047(5) . . ? C21 H22c 2.045(5) . . ? C21 H23a 2.046(5) . . ? C21 H23b 2.043(5) . . ? C21 H23c 2.044(5) . . ? C21 H24a 2.066(5) . . ? C21 H24b 2.065(5) . . ? C21 H24c 2.063(5) . . ? C22 C23 2.509(8) . . ? C22 C24 2.447(8) . . ? C22 Cl3 3.841(6) . . ? C22 H24b 2.633(5) . . ? C22 H24c 2.633(6) . . ? C23 C24 2.482(8) . . ? C23 Cl3 3.836(6) . 6 ? C23 H24a 2.655(6) . . ? C23 H24c 2.681(6) . . ? C24 C3 2.820(7) . . ? C24 Cl1 3.772(5) . '5 576' ? C24 H22a 2.622(6) . . ? C24 H22c 2.628(5) . . ? C24 H23a 2.678(6) . . ? C24 H23b 2.661(5) . . ? C24 H3 2.566(5) . . ? C3 N5 2.181(6) . . ? C3 Cl1 3.830(5) . '3 566' ? C3 H24a 2.675(5) . . ? C3 H4 2.048(5) . . ? C4 C51 2.545(7) . . ? C4 C54 2.787(7) . . ? C4 Cl1 3.652(6) . '3 566' ? C4 Cl2 3.594(5) . '3 566' ? C4 H3 2.057(5) . . ? C4 H54c 2.636(5) . . ? N5 C52 2.454(7) . . ? N5 C53 2.493(6) . . ? N5 C54 2.465(7) . . ? N5 Cl1 3.704(4) . '3 566' ? N5 H4 2.087(4) . . ? N5 H52a 2.637(4) . . ? N5 H52c 2.640(4) . . ? N5 H53a 2.687(4) . . ? N5 H53b 2.677(4) . . ? N5 H54a 2.666(4) . . ? N5 H54c 2.639(4) . . ? C51 H52a 2.060(5) . . ? C51 H52b 2.058(5) . . ? C51 H52c 2.058(5) . . ? C51 H53a 2.074(5) . . ? C51 H53b 2.073(5) . . ? C51 H53c 2.073(5) . . ? C51 H54a 2.052(5) . . ? C51 H54b 2.052(5) . . ? C51 H54c 2.053(5) . . ? C52 C53 2.506(8) . . ? C52 C54 2.482(8) . . ? C52 Cl1 3.645(6) . . ? C52 H54b 2.653(6) . . ? C52 H54c 2.659(6) . . ? C53 C54 2.481(8) . . ? C53 Cl1 3.940(6) . '3 566' ? C53 H54a 2.660(5) . . ? C53 H54b 2.680(6) . . ? C54 Cl3 3.826(7) . '8 565' ? C54 H4 2.521(6) . . ? C54 H52a 2.679(6) . . ? C54 H52b 2.689(6) . . ? C54 H53a 2.668(6) . . ? C54 H53c 2.689(6) . . ? Cl1 Cl2 2.887(2) . . ? Cl1 Cl3 2.885(2) . . ? Cl1 H23a 3.5733(15) . '3 466' ? Cl1 H24a 3.2968(15) . '5 576' ? Cl1 H24b 3.3727(15) . '5 576' ? Cl1 H3 3.3001(16) . '5 576' ? Cl1 H52a 3.3462(15) . . ? Cl1 H52c 3.0481(16) . . ? Cl1 H53a 3.1200(17) . '3 466' ? Cl1 H53c 3.2343(16) . '5 566' ? Cl1 H0 2.2617(15) . . ? Cl2 Cl3 2.880(2) . . ? Cl2 Cl3 4.377(2) . '7 445' ? Cl2 H22c 3.2509(17) . '4 545' ? Cl2 H23b 3.4141(17) . '4 545' ? Cl2 H24c 3.1125(16) . '4 545' ? Cl2 H4 3.1188(17) . '3 466' ? Cl2 H54a 3.2405(17) . '3 466' ? Cl2 H0 2.2582(17) . . ? Cl3 H22a 3.4585(18) . . ? Cl3 H22b 3.4258(18) . . ? Cl3 H23b 3.1902(17) . '6 455' ? Cl3 H3 3.2247(17) . '5 576' ? Cl3 H54b 3.3388(18) . '8 564' ? Cl3 H54c 3.3586(18) . '8 564' ? Cl3 H0 2.2662(17) . . ? H22a H22b 1.55128(9) . . ? H22a H22c 1.55134(13) . . ? H22b H22c 1.55128(10) . . ? H23a H23b 1.55135(15) . . ? H23a H23c 1.55132(9) . . ? H23b H23c 1.55128(10) . . ? H24a H24b 1.55128(19) . . ? H24a H24c 1.55135(14) . . ? H24a H3 2.24238(17) . . ? H24b H24c 1.55137(13) . . ? H24b H3 2.3798(2) . . ? H4 H54a 2.34855(17) . . ? H4 H54c 2.20642(14) . . ? H52a H52b 1.55129(12) . . ? H52a H52c 1.55128(11) . . ? H52b H52c 1.55137(12) . . ? H53a H53b 1.55133(13) . . ? H53a H53c 1.55139(12) . . ? H53b H53c 1.55143(12) . . ? H54a H54b 1.55130(13) . . ? H54a H54c 1.55128(18) . . ? H54b H54c 1.55123(12) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2176 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _reflns_number_observed ? _reflns_d_resolution_high .618 _reflns_d_resolution_low 9.213 _diffrn_reflns_av_sigmaI/netI .112 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .081 _refine_ls_wR_factor_all .049 _refine_ls_goodness_of_fit_all .954 _refine_ls_shift/su_mean .0002 #===END data_sb6010 _database_code_depnum_ccdc_archive 'CCDC 247534' _audit_creation_method Xtal3.6 _audit_creation_date 04-01-19 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C11 H20 Au1 I1 N2' _chemical_formula_moiety 'C11 H20 Au1 I1 N2' _chemical_formula_weight 504.2 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.052(2) _cell_length_b 10.236(2) _cell_length_c 14.105(3) _cell_angle_alpha 90.00000 _cell_angle_beta 110.776(3) _cell_angle_gamma 90.00000 _cell_volume 1491.9(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.245 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5711 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.66 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 11.906 _exptl_crystal_description chip _exptl_crystal_size_max .11 _exptl_crystal_size_mid .07 _exptl_crystal_size_min .03 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .40 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 13622 _reflns_number_total 3036 _reflns_Friedel_coverage 0 _reflns_number_gt 2549 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .062 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .063 _refine_ls_wR_factor_ref .1 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_number_reflns 2549 _refine_ls_number_parameters 136 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .01 _refine_diff_density_min -4.266 _refine_diff_density_max 6.695 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 44 .002 .002 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 80 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Au ? 0 4 -2.688 8.798 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' I ? 0 4 -.726 1.812 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 8 .004 .003 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .45173(5) .48086(5) .73366(4) .0242(3) Uani ? ? 1.00000 ? ? I .68275(8) .56074(11) .82775(6) .0326(5) Uani ? ? 1.00000 ? ? C1 .2675(13) .4204(14) .6666(10) .028(6) Uani ? ? 1.00000 ? ? N2 .2046(9) .3858(10) .5666(7) .020(4) Uani ? ? 1.00000 ? ? C21 .2623(13) .3995(14) .4840(10) .029(6) Uani ? ? 1.00000 ? ? C22 .3758(14) .3095(15) .5050(11) .038(7) Uani ? ? 1.00000 ? ? C23 .2965(15) .5404(14) .4735(12) .035(7) Uani ? ? 1.00000 ? ? C24 .1568(15) .3543(16) .3832(11) .039(7) Uani ? ? 1.00000 ? ? C3 .0823(12) .3417(14) .5538(9) .030(6) Uani ? ? 1.00000 ? ? C4 .0665(11) .3496(14) .6440(9) .027(6) Uani ? ? 1.00000 ? ? N5 .1831(10) .3930(11) .7136(8) .028(5) Uani ? ? 1.00000 ? ? C51 .2060(13) .4081(14) .8255(9) .026(6) Uani ? ? 1.00000 ? ? C52 .3141(14) .3147(14) .8825(10) .034(7) Uani ? ? 1.00000 ? ? C53 .2406(16) .5499(15) .8541(11) .034(7) Uani ? ? 1.00000 ? ? C54 .0832(14) .3719(15) .8441(11) .036(7) Uani ? ? 1.00000 ? ? H22a .35047 .22045 .51167 .05500 Uiso ? ? 1.00000 ? ? H22b .44359 .33103 .56922 .05500 Uiso ? ? 1.00000 ? ? H22c .41233 .31200 .45385 .05500 Uiso ? ? 1.00000 ? ? H23a .21949 .59335 .46084 .05700 Uiso ? ? 1.00000 ? ? H23b .32812 .55273 .42107 .05700 Uiso ? ? 1.00000 ? ? H23c .35938 .57176 .53644 .05700 Uiso ? ? 1.00000 ? ? H24a .08234 .41273 .36741 .05500 Uiso ? ? 1.00000 ? ? H24b .12712 .26867 .38938 .05500 Uiso ? ? 1.00000 ? ? H24c .18622 .35732 .32781 .05500 Uiso ? ? 1.00000 ? ? H3 .01913 .31387 .49020 .03800 Uiso ? ? 1.00000 ? ? H4 -.01112 .32959 .65837 .03200 Uiso ? ? 1.00000 ? ? H52a .28987 .22506 .86338 .05400 Uiso ? ? 1.00000 ? ? H52b .33723 .32172 .95382 .05400 Uiso ? ? 1.00000 ? ? H52c .39118 .33141 .86642 .05400 Uiso ? ? 1.00000 ? ? H53a .17027 .60671 .81533 .05400 Uiso ? ? 1.00000 ? ? H53b .31457 .57505 .83560 .05400 Uiso ? ? 1.00000 ? ? H53c .26062 .56537 .92300 .05400 Uiso ? ? 1.00000 ? ? H54a .01505 .43080 .80891 .05500 Uiso ? ? 1.00000 ? ? H54b .09755 .37652 .91486 .05500 Uiso ? ? 1.00000 ? ? H54c .05733 .28538 .82089 .05500 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .0257(4) .0228(4) .0228(4) -.00311(18) .0068(3) -.00060(18) I .0279(5) .0413(6) .0261(5) -.0063(4) .0066(4) -.0017(4) C1 .034(7) .025(8) .027(6) .001(6) .011(6) -.005(6) N2 .024(5) .014(5) .019(5) -.005(4) .004(4) -.002(4) C21 .035(7) .027(7) .029(6) -.011(6) .016(6) -.014(6) C22 .039(8) .040(9) .050(8) .002(7) .035(7) .003(7) C23 .050(9) .019(7) .044(8) -.014(6) .026(8) -.000(6) C24 .049(9) .032(8) .035(7) -.017(7) .015(7) -.006(6) C3 .027(7) .033(8) .030(7) -.007(6) .008(6) -.006(6) C4 .018(6) .031(7) .029(6) -.008(5) .005(5) -.007(6) N5 .025(5) .031(6) .027(5) .007(5) .010(5) .005(5) C51 .036(7) .025(7) .028(6) .002(6) .024(6) .001(5) C52 .054(9) .020(7) .030(7) -.000(6) .016(7) .001(6) C53 .050(9) .030(8) .029(7) -.001(7) .023(7) -.002(6) C54 .040(8) .038(9) .038(8) .003(7) .021(7) .001(7) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au I . . 2.5583(10) ? Au C1 . . 2.014(13) ? C1 N2 . . 1.380(15) ? C1 N5 . . 1.35(2) ? N2 C21 . . 1.52(2) ? N2 C3 . . 1.375(17) ? C21 C22 . . 1.50(2) ? C21 C23 . . 1.51(2) ? C21 C24 . . 1.555(17) ? C22 H22a . . .968 ? C22 H22b . . .974 ? C22 H22c . . .944 ? C23 H23a . . .971 ? C23 H23b . . .93 ? C23 H23c . . .968 ? C24 H24a . . .977 ? C24 H24b . . .950 ? C24 H24c . . .948 ? C3 C4 . . 1.35(2) ? C3 H3 . . .964 ? C4 N5 . . 1.388(14) ? C4 H4 . . .971 ? N5 C51 . . 1.515(17) ? C51 C52 . . 1.518(18) ? C51 C53 . . 1.52(2) ? C51 C54 . . 1.52(2) ? C52 H52a . . .967 ? C52 H52b . . .948 ? C52 H52c . . .972 ? C53 H53a . . .969 ? C53 H53b . . .977 ? C53 H53c . . .931 ? C54 H54a . . .955 ? C54 H54b . . .955 ? C54 H54c . . .952 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published I Au C1 . . . 176.8(4) ? Au C1 N2 . . . 128.2(11) ? Au C1 N5 . . . 126.3(9) ? N2 C1 N5 . . . 105.3(11) ? C1 N2 C21 . . . 124.3(10) ? C1 N2 C3 . . . 109.5(11) ? C21 N2 C3 . . . 126.2(9) ? N2 C21 C22 . . . 110.0(11) ? N2 C21 C23 . . . 110.5(12) ? N2 C21 C24 . . . 106.9(11) ? C22 C21 C23 . . . 112.6(13) ? C22 C21 C24 . . . 107.6(12) ? C23 C21 C24 . . . 109.1(11) ? C21 C22 H22a . . . 110.3 ? C21 C22 H22b . . . 111.0 ? C21 C22 H22c . . . 112.8 ? H22a C22 H22b . . . 106.0 ? H22a C22 H22c . . . 108.4 ? H22b C22 H22c . . . 108.0 ? C21 C23 H23a . . . 108.5 ? C21 C23 H23b . . . 112.6 ? C21 C23 H23c . . . 110.5 ? H23a C23 H23b . . . 109.2 ? H23a C23 H23c . . . 106.3 ? H23b C23 H23c . . . 109.5 ? C21 C24 H24a . . . 108.9 ? C21 C24 H24b . . . 111.2 ? C21 C24 H24c . . . 112.2 ? H24a C24 H24b . . . 107.2 ? H24a C24 H24c . . . 107.4 ? H24b C24 H24c . . . 109.6 ? N2 C3 C4 . . . 107.9(10) ? N2 C3 H3 . . . 125.0 ? C4 C3 H3 . . . 127.1 ? C3 C4 N5 . . . 106.8(12) ? C3 C4 H4 . . . 127.3 ? N5 C4 H4 . . . 125.9 ? C1 N5 C4 . . . 110.4(11) ? C1 N5 C51 . . . 126.9(10) ? C4 N5 C51 . . . 122.7(12) ? N5 C51 C52 . . . 107.3(12) ? N5 C51 C53 . . . 107.9(11) ? N5 C51 C54 . . . 109.0(10) ? C52 C51 C53 . . . 112.6(10) ? C52 C51 C54 . . . 109.8(12) ? C53 C51 C54 . . . 110.1(13) ? C51 C52 H52a . . . 111.2 ? C51 C52 H52b . . . 112.3 ? C51 C52 H52c . . . 110.8 ? H52a C52 H52b . . . 108.2 ? H52a C52 H52c . . . 106.3 ? H52b C52 H52c . . . 107.8 ? C51 C53 H53a . . . 110.4 ? C51 C53 H53b . . . 109.6 ? C51 C53 H53c . . . 112.6 ? H53a C53 H53b . . . 105.7 ? H53a C53 H53c . . . 109.5 ? H53b C53 H53c . . . 108.8 ? C51 C54 H54a . . . 110.2 ? C51 C54 H54b . . . 110.0 ? C51 C54 H54c . . . 110.2 ? H54a C54 H54b . . . 108.6 ? H54a C54 H54c . . . 108.9 ? H54b C54 H54c . . . 108.9 ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 928 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min -17 _reflns_limit_l_max 16 _reflns_number_observed ? _reflns_d_resolution_high .8 _reflns_d_resolution_low 10.026 _diffrn_reflns_av_sigmaI/netI .065 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .078 _refine_ls_wR_factor_all .108 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_shift/su_mean .002 #===END data_sb6004 _database_code_depnum_ccdc_archive 'CCDC 247535' _audit_creation_method Xtal3.6 _audit_creation_date 03-12-22 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C12 H20 Au1 N3 S1' _chemical_formula_moiety 'C12 H20 Au1 N3 S1' _chemical_formula_weight 435.38 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 6.7689(6) _cell_length_b 15.0730(10) _cell_length_c 14.4970(10) _cell_angle_alpha 90.00000 _cell_angle_beta 90.803(2) _cell_angle_gamma 90.00000 _cell_volume 1478.9(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8869 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 37.4 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 10.072 _exptl_crystal_description cuboid _exptl_crystal_size_max .12 _exptl_crystal_size_mid .11 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .65 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 29467 _reflns_number_total 7777 _reflns_Friedel_coverage 0 _reflns_number_gt 5820 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.6 _diffrn_reflns_theta_full 37.6 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .056 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .039 _refine_ls_wR_factor_ref .045 _refine_ls_goodness_of_fit_ref 1.16 _refine_ls_number_reflns 5820 _refine_ls_number_parameters 154 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .003 _refine_diff_density_min -3.116 _refine_diff_density_max 3.208 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 48 .002 .002 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 80 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Au ? 0 4 -2.688 8.798 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 12 .004 .003 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' S ? 0 4 .11 .124 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .23033(2) .177388(9) 1.074735(9) .01704(7) Uani ? ? 1.00000 ? ? C1 .0940(6) .1948(2) .9507(2) .0170(15) Uani ? ? 1.00000 ? ? N2 .1244(5) .1499(2) .8712(2) .0188(14) Uani ? ? 1.00000 ? ? C21 .2721(6) .0762(3) .8574(3) .0206(17) Uani ? ? 1.00000 ? ? C22 .2065(8) -.0038(3) .9129(4) .033(2) Uani ? ? 1.00000 ? ? C23 .4783(6) .1089(3) .8863(3) .031(2) Uani ? ? 1.00000 ? ? C24 .2770(7) .0532(3) .7547(3) .033(2) Uani ? ? 1.00000 ? ? C3 .0012(6) .1821(3) .8029(3) .0218(17) Uani ? ? 1.00000 ? ? C4 -.1061(6) .2478(3) .8394(3) .0213(17) Uani ? ? 1.00000 ? ? N5 -.0493(5) .2561(2) .9309(2) .0176(14) Uani ? ? 1.00000 ? ? C51 -.1289(6) .3231(2) .9971(3) .0201(16) Uani ? ? 1.00000 ? ? C52 -.2320(6) .2749(3) 1.0764(3) .0242(19) Uani ? ? 1.00000 ? ? C53 .0404(7) .3819(3) 1.0320(3) .0246(18) Uani ? ? 1.00000 ? ? C54 -.2818(8) .3810(3) .9466(3) .032(2) Uani ? ? 1.00000 ? ? S .39639(17) .16727(7) 1.21459(7) .0240(5) Uani ? ? 1.00000 ? ? C .2713(7) .0864(3) 1.2683(3) .029(2) Uani ? ? 1.00000 ? ? N .1959(7) .0294(4) 1.3081(3) .049(3) Uani ? ? 1.00000 ? ? H22a .07942 -.02215 .89285 .05300 Uiso ? ? 1.00000 ? ? H22b .20509 .01060 .97644 .05300 Uiso ? ? 1.00000 ? ? H22c .29827 -.05142 .90356 .05300 Uiso ? ? 1.00000 ? ? H23a .51273 .15935 .84985 .04900 Uiso ? ? 1.00000 ? ? H23b .57265 .06329 .87654 .04900 Uiso ? ? 1.00000 ? ? H23c .47947 .12531 .94942 .04900 Uiso ? ? 1.00000 ? ? H24a .31671 .10309 .72017 .05100 Uiso ? ? 1.00000 ? ? H24b .14847 .03475 .73432 .05100 Uiso ? ? 1.00000 ? ? H24c .36733 .00555 .74515 .05100 Uiso ? ? 1.00000 ? ? H3 -.00685 .16029 .74089 .02800 Uiso ? ? 1.00000 ? ? H4 -.20381 .28289 .80767 .02800 Uiso ? ? 1.00000 ? ? H52a -.33553 .23891 1.05217 .03800 Uiso ? ? 1.00000 ? ? H52b -.28446 .31704 1.11796 .03800 Uiso ? ? 1.00000 ? ? H52c -.13859 .23832 1.10820 .03800 Uiso ? ? 1.00000 ? ? H53a .10039 .41108 .98113 .03900 Uiso ? ? 1.00000 ? ? H53b .13626 .34689 1.06331 .03900 Uiso ? ? 1.00000 ? ? H53c -.00961 .42560 1.07307 .03900 Uiso ? ? 1.00000 ? ? H54a -.21675 .41241 .89670 .05000 Uiso ? ? 1.00000 ? ? H54b -.33249 .42464 .98743 .05000 Uiso ? ? 1.00000 ? ? H54c -.38399 .34661 .92159 .05000 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .01966(7) .01883(7) .01258(6) .00172(5) -.00196(4) -.00016(5) C1 .0191(16) .0198(16) .0120(14) .0018(12) -.0017(12) .0018(11) N2 .0172(14) .0240(14) .0151(13) .0002(12) -.0003(11) -.0001(11) C21 .0185(17) .0231(17) .0202(17) .0005(13) -.0014(13) -.0038(13) C22 .043(3) .023(2) .033(2) .0050(19) .011(2) .0036(17) C23 .0199(19) .040(3) .033(2) .0043(17) -.0000(16) -.009(2) C24 .036(2) .043(3) .020(2) .013(2) -.0023(17) -.0078(18) C3 .0241(18) .0278(19) .0135(14) .0026(15) -.0019(13) -.0002(13) C4 .0244(18) .0243(18) .0152(15) .0026(14) -.0032(13) .0005(13) N5 .0202(15) .0186(14) .0140(13) .0019(11) .0008(11) .0000(10) C51 .0245(17) .0183(15) .0175(15) .0016(14) .0009(13) -.0014(13) C52 .0214(19) .027(2) .024(2) .0002(14) .0027(15) -.0014(15) C53 .033(2) .0157(16) .0249(19) -.0017(15) .0008(16) -.0008(14) C54 .038(2) .033(2) .026(2) .014(2) -.0031(18) -.0026(18) S .0249(5) .0295(5) .0172(4) -.0006(4) -.0056(3) .0016(3) C .026(2) .042(3) .0196(18) .0017(18) -.0005(15) -.0015(17) N .040(3) .077(4) .031(2) -.014(2) .0050(19) .012(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C1 . . 2.026(4) ? Au S . . 2.3095(11) ? C1 N2 . . 1.355(5) ? C1 N5 . . 1.367(5) ? N2 C21 . . 1.509(5) ? N2 C3 . . 1.375(5) ? C21 C22 . . 1.520(6) ? C21 C23 . . 1.533(6) ? C21 C24 . . 1.530(6) ? C22 H22a . . .945 ? C22 H22b . . .947 ? C22 H22c . . .960 ? C23 H23a . . .957 ? C23 H23b . . .950 ? C23 H23c . . .947 ? C24 H24a . . .945 ? C24 H24b . . .956 ? C24 H24c . . .954 ? C3 C4 . . 1.341(6) ? C3 H3 . . .959 ? C4 N5 . . 1.382(5) ? C4 H4 . . .959(4) ? N5 C51 . . 1.499(5) ? C51 C52 . . 1.536(6) ? C51 C53 . . 1.529(6) ? C51 C54 . . 1.532(6) ? C52 H52a . . .950 ? C52 H52b . . .948 ? C52 H52c . . .953 ? C53 H53a . . .955 ? C53 H53b . . .947 ? C53 H53c . . .953 ? C54 H54a . . .975 ? C54 H54b . . .952 ? C54 H54c . . .933 ? S C . . 1.681(5) ? C N . . 1.158(7) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C1 Au S . . . 175.90(11) ? Au C1 N2 . . . 128.1(3) ? Au C1 N5 . . . 125.9(3) ? N2 C1 N5 . . . 106.0(3) ? C1 N2 C21 . . . 126.1(3) ? C1 N2 C3 . . . 109.7(3) ? C21 N2 C3 . . . 124.1(3) ? N2 C21 C22 . . . 108.3(3) ? N2 C21 C23 . . . 109.2(3) ? N2 C21 C24 . . . 108.6(3) ? C22 C21 C23 . . . 112.5(4) ? C22 C21 C24 . . . 110.2(4) ? C23 C21 C24 . . . 107.9(4) ? C21 C22 H22a . . . 109.9 ? C21 C22 H22b . . . 109.9 ? C21 C22 H22c . . . 108.9 ? H22a C22 H22b . . . 110.2 ? H22a C22 H22c . . . 109.0 ? H22b C22 H22c . . . 108.9 ? C21 C23 H23a . . . 109.4 ? C21 C23 H23b . . . 109.7 ? C21 C23 H23c . . . 110.1 ? H23a C23 H23b . . . 108.8 ? H23a C23 H23c . . . 109.1 ? H23b C23 H23c . . . 109.7 ? C21 C24 H24a . . . 110.2 ? C21 C24 H24b . . . 109.5 ? C21 C24 H24c . . . 109.5 ? H24a C24 H24b . . . 109.4 ? H24a C24 H24c . . . 109.6 ? H24b C24 H24c . . . 108.6 ? N2 C3 C4 . . . 107.7(3) ? N2 C3 H3 . . . 125.5 ? C4 C3 H3 . . . 126.8 ? C3 C4 N5 . . . 107.5(3) ? C3 C4 H4 . . . 126.3 ? N5 C4 H4 . . . 126.2 ? C1 N5 C4 . . . 109.1(3) ? C1 N5 C51 . . . 125.6(3) ? C4 N5 C51 . . . 125.3(3) ? N5 C51 C52 . . . 109.4(3) ? N5 C51 C53 . . . 109.1(3) ? N5 C51 C54 . . . 109.0(3) ? C52 C51 C53 . . . 111.8(3) ? C52 C51 C54 . . . 108.4(3) ? C53 C51 C54 . . . 109.1(3) ? C51 C52 H52a . . . 109.5 ? C51 C52 H52b . . . 109.7 ? C51 C52 H52c . . . 109.3 ? H52a C52 H52b . . . 109.7 ? H52a C52 H52c . . . 109.2 ? H52b C52 H52c . . . 109.4 ? C51 C53 H53a . . . 109.6 ? C51 C53 H53b . . . 110.0 ? C51 C53 H53c . . . 109.6 ? H53a C53 H53b . . . 109.3 ? H53a C53 H53c . . . 108.8 ? H53b C53 H53c . . . 109.5 ? C51 C54 H54a . . . 108.8 ? C51 C54 H54b . . . 110.1 ? C51 C54 H54c . . . 111.2 ? H54a C54 H54b . . . 107.2 ? H54a C54 H54c . . . 108.8 ? H54b C54 H54c . . . 110.7 ? Au S C . . . 102.26(16) ? S C N . . . 175.8(4) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 832 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min -24 _reflns_limit_l_max 24 _reflns_number_observed ? _reflns_d_resolution_high .582 _reflns_d_resolution_low 10.426 _diffrn_reflns_av_sigmaI/netI .075 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .062 _refine_ls_wR_factor_all .049 _refine_ls_goodness_of_fit_all 1.09 _refine_ls_shift/su_mean .0005 #===END data_sb6008 _database_code_depnum_ccdc_archive 'CCDC 247536' _audit_creation_method Xtal3.6 _audit_creation_date 04-01-01 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C12 H20 Au1 N3 Se1' _chemical_formula_moiety 'C12 H20 Au1 N3 Se1' _chemical_formula_weight 482.24 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 7.6181(9) _cell_length_b 9.8300(10) _cell_length_c 10.8300(10) _cell_angle_alpha 81.402(3) _cell_angle_beta 82.135(3) _cell_angle_gamma 75.279(3) _cell_volume 771.42(14) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4925 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 32.4 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 11.879 _exptl_crystal_description block _exptl_crystal_size_max .14 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .11 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .43 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 15225 _reflns_number_total 5378 _reflns_Friedel_coverage 0 _reflns_number_gt 4222 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 32.2 _diffrn_reflns_theta_full 32.2 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .072 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .056 _refine_ls_wR_factor_ref .068 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_number_reflns 4222 _refine_ls_number_parameters 154 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .001 _refine_diff_density_min -4.776 _refine_diff_density_max 6.801 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 24 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 40 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 2 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 6 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Se ? 0 2 -.178 2.223 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .73776(4) .94363(3) .27379(3) .0188(2) Uani ? ? 1.00000 ? ? C1 .9496(10) .7919(8) .2029(7) .017(5) Uani ? ? 1.00000 ? ? N2 .9701(8) .7554(7) .0849(6) .016(4) Uani ? ? 1.00000 ? ? C21 .8316(10) .7927(9) -.0065(7) .021(5) Uani ? ? 1.00000 ? ? C22 .7771(12) .9548(10) -.0416(9) .029(6) Uani ? ? 1.00000 ? ? C23 .6638(11) .7387(10) .0530(9) .028(6) Uani ? ? 1.00000 ? ? C24 .9118(12) .7241(11) -.1271(9) .033(7) Uani ? ? 1.00000 ? ? C3 1.1429(10) .6657(9) .0639(7) .021(5) Uani ? ? 1.00000 ? ? C4 1.2235(11) .6485(9) .1701(8) .024(5) Uani ? ? 1.00000 ? ? N5 1.1030(9) .7267(7) .2561(6) .020(4) Uani ? ? 1.00000 ? ? C51 1.1443(11) .7409(9) .3848(7) .023(5) Uani ? ? 1.00000 ? ? C52 1.1740(14) .8886(12) .3831(9) .037(7) Uani ? ? 1.00000 ? ? C53 .9898(14) .7122(12) .4814(9) .038(7) Uani ? ? 1.00000 ? ? C54 1.3201(15) .6305(13) .4158(9) .041(7) Uani ? ? 1.00000 ? ? Se .49179(11) 1.12514(9) .35709(8) .0230(5) Uani ? ? 1.00000 ? ? C .5690(11) 1.2776(9) .2699(8) .025(5) Uani ? ? 1.00000 ? ? N .6096(12) 1.3790(10) .2191(9) .041(6) Uani ? ? 1.00000 ? ? H22a .88014 .98899 -.07694 .04600 Uiso ? ? 1.00000 ? ? H22b .72815 .99884 .03470 .04600 Uiso ? ? 1.00000 ? ? H22c .68616 .97895 -.09675 .04600 Uiso ? ? 1.00000 ? ? H23a .69787 .63839 .07551 .04000 Uiso ? ? 1.00000 ? ? H23b .57288 .76146 -.00212 .04000 Uiso ? ? 1.00000 ? ? H23c .61487 .78134 .12933 .04000 Uiso ? ? 1.00000 ? ? H24a .94800 .62307 -.10640 .05100 Uiso ? ? 1.00000 ? ? H24b 1.01783 .75657 -.16310 .05100 Uiso ? ? 1.00000 ? ? H24c .82491 .74625 -.18519 .05100 Uiso ? ? 1.00000 ? ? H3 1.19233 .62506 -.01147 .02700 Uiso ? ? 1.00000 ? ? H4 1.34374 .59309 .18400 .03100 Uiso ? ? 1.00000 ? ? H52a 1.27396 .90087 .31988 .05500 Uiso ? ? 1.00000 ? ? H52b 1.20475 .90037 .46146 .05500 Uiso ? ? 1.00000 ? ? H52c 1.06834 .95826 .36119 .05500 Uiso ? ? 1.00000 ? ? H53a .97649 .61802 .47880 .05700 Uiso ? ? 1.00000 ? ? H53b .87862 .77760 .46251 .05700 Uiso ? ? 1.00000 ? ? H53c 1.01504 .71970 .56278 .05700 Uiso ? ? 1.00000 ? ? H54a 1.30353 .53783 .41806 .06000 Uiso ? ? 1.00000 ? ? H54b 1.35208 .64187 .49492 .06000 Uiso ? ? 1.00000 ? ? H54c 1.41742 .64367 .35271 .06000 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .02143(14) .01803(16) .01605(14) -.00155(10) -.00058(9) -.00555(10) C1 .021(3) .014(3) .018(3) -.009(3) -.002(3) .002(3) N2 .018(3) .015(3) .015(3) -.001(2) .000(2) -.005(2) C21 .021(3) .023(4) .021(4) -.007(3) -.005(3) -.004(3) C22 .036(4) .021(4) .028(4) -.006(3) -.010(3) .005(3) C23 .026(4) .029(5) .031(4) -.011(3) -.002(3) -.005(4) C24 .031(4) .043(6) .028(4) -.007(4) -.008(3) -.015(4) C3 .019(3) .023(4) .019(3) .000(3) .002(3) -.010(3) C4 .026(4) .021(4) .025(4) .001(3) -.001(3) -.012(3) N5 .023(3) .022(3) .013(3) -.003(2) .001(2) -.005(2) C51 .031(4) .017(4) .016(3) .001(3) -.004(3) -.003(3) C52 .048(5) .043(6) .024(4) -.011(5) -.014(4) -.010(4) C53 .041(5) .047(6) .018(4) -.004(4) .002(3) .002(4) C54 .045(5) .047(6) .023(4) .009(5) -.012(4) -.007(4) Se .0234(3) .0229(4) .0205(4) -.0009(3) .0017(3) -.0072(3) C .031(4) .022(4) .017(4) .004(3) -.000(3) -.007(3) N .043(5) .031(5) .038(5) -.003(4) .012(4) .002(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C1 . . 2.049(7) ? Au Se . . 2.4142(8) ? C1 N2 . . 1.357(10) ? C1 N5 . . 1.342(10) ? N2 C21 . . 1.486(10) ? N2 C3 . . 1.396(9) ? C21 C22 . . 1.543(12) ? C21 C23 . . 1.532(12) ? C21 C24 . . 1.539(13) ? C22 H22a . . .943 ? C22 H22b . . .975 ? C22 H22c . . .938 ? C23 H23a . . .956 ? C23 H23b . . .939 ? C23 H23c . . .968 ? C24 H24a . . .961 ? C24 H24b . . .956 ? C24 H24c . . .938 ? C3 C4 . . 1.345(12) ? C3 H3 . . .951 ? C4 N5 . . 1.387(10) ? C4 H4 . . .959 ? N5 C51 . . 1.504(11) ? C51 C52 . . 1.522(15) ? C51 C53 . . 1.517(13) ? C51 C54 . . 1.536(13) ? C52 H52a . . .971 ? C52 H52b . . .941 ? C52 H52c . . .947 ? C53 H53a . . .962 ? C53 H53b . . .951 ? C53 H53c . . .945 ? C54 H54a . . .947 ? C54 H54b . . .952 ? C54 H54c . . .958 ? Se C . . 1.832(9) ? C N . . 1.157(13) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C1 Au Se . . . 179.0(3) ? Au C1 N2 . . . 124.9(5) ? Au C1 N5 . . . 126.7(6) ? N2 C1 N5 . . . 107.8(6) ? C1 N2 C21 . . . 127.5(6) ? C1 N2 C3 . . . 108.5(6) ? C21 N2 C3 . . . 123.9(7) ? N2 C21 C22 . . . 110.1(8) ? N2 C21 C23 . . . 108.8(6) ? N2 C21 C24 . . . 109.7(6) ? C22 C21 C23 . . . 110.0(6) ? C22 C21 C24 . . . 108.2(7) ? C23 C21 C24 . . . 110.0(8) ? C21 C22 H22a . . . 110.4 ? C21 C22 H22b . . . 108.6 ? C21 C22 H22c . . . 110.3 ? H22a C22 H22b . . . 108.0 ? H22a C22 H22c . . . 111.1 ? H22b C22 H22c . . . 108.4 ? C21 C23 H23a . . . 109.9 ? C21 C23 H23b . . . 111.0 ? C21 C23 H23c . . . 109.6 ? H23a C23 H23b . . . 109.9 ? H23a C23 H23c . . . 107.4 ? H23b C23 H23c . . . 108.9 ? C21 C24 H24a . . . 109.1 ? C21 C24 H24b . . . 109.8 ? C21 C24 H24c . . . 110.4 ? H24a C24 H24b . . . 108.0 ? H24a C24 H24c . . . 109.5 ? H24b C24 H24c . . . 109.9 ? N2 C3 C4 . . . 106.8(7) ? N2 C3 H3 . . . 125.8 ? C4 C3 H3 . . . 127.3 ? C3 C4 N5 . . . 108.1(7) ? C3 C4 H4 . . . 126.3 ? N5 C4 H4 . . . 125.6 ? C1 N5 C4 . . . 108.7(7) ? C1 N5 C51 . . . 126.4(6) ? C4 N5 C51 . . . 124.8(6) ? N5 C51 C52 . . . 108.2(7) ? N5 C51 C53 . . . 109.6(8) ? N5 C51 C54 . . . 108.9(7) ? C52 C51 C53 . . . 112.5(8) ? C52 C51 C54 . . . 109.1(9) ? C53 C51 C54 . . . 108.4(7) ? C51 C52 H52a . . . 108.8 ? C51 C52 H52b . . . 110.8 ? C51 C52 H52c . . . 110.3 ? H52a C52 H52b . . . 108.4 ? H52a C52 H52c . . . 108.0 ? H52b C52 H52c . . . 110.5 ? C51 C53 H53a . . . 109.3 ? C51 C53 H53b . . . 109.9 ? C51 C53 H53c . . . 110.4 ? H53a C53 H53b . . . 108.4 ? H53a C53 H53c . . . 108.9 ? H53b C53 H53c . . . 109.9 ? C51 C54 H54a . . . 110.2 ? C51 C54 H54b . . . 109.9 ? C51 C54 H54c . . . 109.4 ? H54a C54 H54b . . . 109.6 ? H54a C54 H54c . . . 109.1 ? H54b C54 H54c . . . 108.7 ? Au Se C . . . 97.0(2) ? Se C N . . . 175.9(8) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 452 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min -15 _reflns_limit_l_max 16 _reflns_number_observed ? _reflns_d_resolution_high .667 _reflns_d_resolution_low 10.628 _diffrn_reflns_av_sigmaI/netI .087 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .073 _refine_ls_wR_factor_all .073 _refine_ls_goodness_of_fit_all .959 _refine_ls_shift/su_mean .0001 #===END data_sb6007 _database_code_depnum_ccdc_archive 'CCDC 247537' _audit_creation_method Xtal3.6 _audit_creation_date 04-01-08 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C11 H20 Au1 N5' _chemical_formula_moiety 'C11 H20 Au1 N5' _chemical_formula_weight 419.33 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 12.0971(6) _cell_length_b 11.0236(6) _cell_length_c 10.9938(6) _cell_angle_alpha 90.00000 _cell_angle_beta 103.8980(10) _cell_angle_gamma 90.00000 _cell_volume 1423.14(13) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5794 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 37.4 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 10.326 _exptl_crystal_description rhom _exptl_crystal_size_max .18 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .14 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .65 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 28477 _reflns_number_total 7218 _reflns_Friedel_coverage 0 _reflns_number_gt 5716 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.5 _diffrn_reflns_theta_full 37.5 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .042 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .029 _refine_ls_wR_factor_ref .048 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_number_reflns 5716 _refine_ls_number_parameters 154 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .002 _refine_diff_density_min -1.307 _refine_diff_density_max 2.703 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 44 .002 .002 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 80 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Au ? 0 4 -2.688 8.798 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 20 .004 .003 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .727619(10) .517468(12) .380727(11) .01885(6) Uani ? ? 1.00000 ? ? C1 .7220(3) .6979(3) .3689(3) .0183(13) Uani ? ? 1.00000 ? ? N2 .8020(3) .7735(3) .3412(3) .0209(11) Uani ? ? 1.00000 ? ? C21 .9092(3) .7365(4) .3045(3) .0258(15) Uani ? ? 1.00000 ? ? C22 .8762(3) .6665(4) .1820(3) .0312(17) Uani ? ? 1.00000 ? ? C23 .9822(3) .6568(5) .4069(4) .0338(18) Uani ? ? 1.00000 ? ? C24 .9753(4) .8485(5) .2897(5) .045(2) Uani ? ? 1.00000 ? ? C3 .7680(3) .8924(3) .3499(3) .0258(15) Uani ? ? 1.00000 ? ? C4 .6668(3) .8915(3) .3814(3) .0236(14) Uani ? ? 1.00000 ? ? N5 .6396(2) .7709(3) .3924(2) .0191(10) Uani ? ? 1.00000 ? ? C51 .5332(3) .7283(3) .4289(3) .0203(12) Uani ? ? 1.00000 ? ? C52 .4648(3) .6479(4) .3246(3) .0261(15) Uani ? ? 1.00000 ? ? C53 .5675(3) .6622(4) .5530(3) .0229(13) Uani ? ? 1.00000 ? ? C54 .4615(3) .8382(4) .4439(4) .0316(17) Uani ? ? 1.00000 ? ? N01 .7251(3) .3328(4) .4018(4) .0359(17) Uani ? ? 1.00000 ? ? N02 .7795(3) .2611(3) .3672(3) .0295(15) Uani ? ? 1.00000 ? ? N03 .8283(3) .1803(4) .3392(5) .053(2) Uani ? ? 1.00000 ? ? H22a .83002 .71603 .11841 .04500 Uiso ? ? 1.00000 ? ? H22b .83306 .59565 .19224 .04500 Uiso ? ? 1.00000 ? ? H22c .94204 .64187 .15613 .04500 Uiso ? ? 1.00000 ? ? H23a 1.00245 .70182 .48406 .04900 Uiso ? ? 1.00000 ? ? H23b 1.04980 .63279 .38449 .04900 Uiso ? ? 1.00000 ? ? H23c .94082 .58658 .42061 .04900 Uiso ? ? 1.00000 ? ? H24a .99602 .89300 .36509 .07100 Uiso ? ? 1.00000 ? ? H24b .92962 .90072 .22579 .07100 Uiso ? ? 1.00000 ? ? H24c 1.04260 .82810 .26249 .07100 Uiso ? ? 1.00000 ? ? H3 .80926 .96327 .33608 .03200 Uiso ? ? 1.00000 ? ? H4 .62246 .95986 .39208 .02900 Uiso ? ? 1.00000 ? ? H52a .44501 .69315 .24780 .04000 Uiso ? ? 1.00000 ? ? H52b .39703 .62113 .34499 .04000 Uiso ? ? 1.00000 ? ? H52c .50926 .57987 .31275 .04000 Uiso ? ? 1.00000 ? ? H53a .60929 .71550 .61604 .03500 Uiso ? ? 1.00000 ? ? H53b .61330 .59404 .54596 .03500 Uiso ? ? 1.00000 ? ? H53c .50108 .63530 .57820 .03500 Uiso ? ? 1.00000 ? ? H54a .50234 .88939 .50868 .04700 Uiso ? ? 1.00000 ? ? H54b .39248 .81276 .46417 .04700 Uiso ? ? 1.00000 ? ? H54c .44212 .88330 .36731 .04700 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .01875(7) .01246(7) .02453(7) .00019(4) .00363(4) -.00097(4) C1 .0194(13) .0157(15) .0203(13) .0011(10) .0057(11) -.0009(9) N2 .0246(13) .0152(12) .0243(13) -.0026(10) .0089(10) .0005(9) C21 .0269(15) .0256(18) .0270(15) -.0046(13) .0106(13) -.0023(13) C22 .0340(18) .037(2) .0247(16) .0050(16) .0104(14) -.0002(14) C23 .0203(15) .046(3) .0327(18) .0013(15) .0015(13) .0002(17) C24 .048(3) .028(2) .069(3) -.008(2) .035(2) -.002(2) C3 .0342(17) .0159(16) .0284(16) -.0014(13) .0094(13) .0014(12) C4 .0324(16) .0143(15) .0258(14) .0009(12) .0103(12) .0015(11) N5 .0201(11) .0151(12) .0222(12) -.0000(9) .0057(9) .0011(9) C51 .0182(12) .0181(14) .0248(14) .0006(10) .0058(10) .0014(11) C52 .0225(14) .0245(18) .0302(16) -.0012(12) .0045(12) .0027(13) C53 .0240(14) .0238(16) .0232(14) -.0014(12) .0101(11) .0027(12) C54 .0319(18) .0233(18) .045(2) .0060(14) .0201(16) .0043(15) N01 .0321(18) .0178(17) .058(2) -.0087(12) .0109(16) .0037(15) N02 .0235(14) .0199(16) .045(2) -.0064(12) .0086(14) -.0000(14) N03 .0302(18) .022(2) .110(4) -.0017(15) .022(2) -.011(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C1 . . 1.993(4) ? Au N01 . . 2.050(4) ? C1 N2 . . 1.366(5) ? C1 N5 . . 1.354(5) ? N2 C21 . . 1.503(5) ? N2 C3 . . 1.384(5) ? C21 C22 . . 1.521(5) ? C21 C23 . . 1.531(5) ? C21 C24 . . 1.501(7) ? C22 H22a . . .954 ? C22 H22b . . .961 ? C22 H22c . . .947 ? C23 H23a . . .962 ? C23 H23b . . .947 ? C23 H23c . . .953 ? C24 H24a . . .944 ? C24 H24b . . .972 ? C24 H24c . . .959 ? C3 C4 . . 1.350(6) ? C3 H3 . . .959 ? C4 N5 . . 1.381(5) ? C4 H4 . . .949 ? N5 C51 . . 1.512(5) ? C51 C52 . . 1.525(5) ? C51 C53 . . 1.514(5) ? C51 C54 . . 1.522(6) ? C52 H52a . . .960 ? C52 H52b . . .948 ? C52 H52c . . .950 ? C53 H53a . . .956 ? C53 H53b . . .948 ? C53 H53c . . .958 ? C54 H54a . . .949 ? C54 H54b . . .957 ? C54 H54c . . .957 ? N01 N02 . . 1.151(6) ? N02 N03 . . 1.150(6) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C1 Au N01 . . . 175.63(16) ? Au C1 N2 . . . 127.5(3) ? Au C1 N5 . . . 126.6(3) ? N2 C1 N5 . . . 105.8(3) ? C1 N2 C21 . . . 126.6(3) ? C1 N2 C3 . . . 108.9(3) ? C21 N2 C3 . . . 124.5(3) ? N2 C21 C22 . . . 108.4(3) ? N2 C21 C23 . . . 109.9(3) ? N2 C21 C24 . . . 108.8(4) ? C22 C21 C23 . . . 110.0(3) ? C22 C21 C24 . . . 110.7(4) ? C23 C21 C24 . . . 108.9(3) ? C21 C22 H22a . . . 109.9 ? C21 C22 H22b . . . 110.0 ? C21 C22 H22c . . . 110.5 ? H22a C22 H22b . . . 108.2 ? H22a C22 H22c . . . 109.3 ? H22b C22 H22c . . . 108.8 ? C21 C23 H23a . . . 109.4 ? C21 C23 H23b . . . 110.5 ? C21 C23 H23c . . . 110.5 ? H23a C23 H23b . . . 108.7 ? H23a C23 H23c . . . 108.2 ? H23b C23 H23c . . . 109.5 ? C21 C24 H24a . . . 111.6 ? C21 C24 H24b . . . 109.9 ? C21 C24 H24c . . . 110.9 ? H24a C24 H24b . . . 108.1 ? H24a C24 H24c . . . 109.2 ? H24b C24 H24c . . . 106.9 ? N2 C3 C4 . . . 108.3(3) ? N2 C3 H3 . . . 125.8 ? C4 C3 H3 . . . 125.9 ? C3 C4 N5 . . . 106.2(3) ? C3 C4 H4 . . . 126.9 ? N5 C4 H4 . . . 126.9 ? C1 N5 C4 . . . 110.7(3) ? C1 N5 C51 . . . 125.3(3) ? C4 N5 C51 . . . 123.9(3) ? N5 C51 C52 . . . 108.9(3) ? N5 C51 C53 . . . 108.8(2) ? N5 C51 C54 . . . 108.9(3) ? C52 C51 C53 . . . 112.3(3) ? C52 C51 C54 . . . 108.9(3) ? C53 C51 C54 . . . 109.0(3) ? C51 C52 H52a . . . 109.6 ? C51 C52 H52b . . . 110.3 ? C51 C52 H52c . . . 109.8 ? H52a C52 H52b . . . 108.8 ? H52a C52 H52c . . . 108.6 ? H52b C52 H52c . . . 109.7 ? C51 C53 H53a . . . 109.9 ? C51 C53 H53b . . . 110.3 ? C51 C53 H53c . . . 110.0 ? H53a C53 H53b . . . 109.2 ? H53a C53 H53c . . . 108.3 ? H53b C53 H53c . . . 109.0 ? C51 C54 H54a . . . 110.4 ? C51 C54 H54b . . . 110.1 ? C51 C54 H54c . . . 110.1 ? H54a C54 H54b . . . 108.9 ? H54a C54 H54c . . . 108.9 ? H54b C54 H54c . . . 108.3 ? Au N01 N02 . . . 128.3(4) ? N01 N02 N03 . . . 172.6(5) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 800 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -18 _reflns_limit_l_max 18 _reflns_number_observed ? _reflns_d_resolution_high .584 _reflns_d_resolution_low 11.715 _diffrn_reflns_av_sigmaI/netI .05 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .044 _refine_ls_wR_factor_all .053 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_shift/su_mean .0008 #===END data_sb6012 _database_code_depnum_ccdc_archive 'CCDC 247538' _audit_creation_method Xtal3.6 _audit_creation_date 04-04-06 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C12 H20 Au1 N3 O1' _chemical_formula_moiety 'C12 H20 Au1 N3 O1' _chemical_formula_weight 419.28 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 11.6800(10) _cell_length_b 11.3460(10) _cell_length_c 10.9510(10) _cell_angle_alpha 90.00000 _cell_angle_beta 101.574(2) _cell_angle_gamma 90.00000 _cell_volume 1421.7(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6687 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 37.41 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 10.337 _exptl_crystal_description bar _exptl_crystal_size_max .19 _exptl_crystal_size_mid .11 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .44 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 28337 _reflns_number_total 7382 _reflns_Friedel_coverage 0 _reflns_number_gt 6120 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.51 _diffrn_reflns_theta_full 37.51 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .038 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .023 _refine_ls_wR_factor_ref .036 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_number_reflns 6120 _refine_ls_number_parameters 154 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .007 _refine_diff_density_min -2.419 _refine_diff_density_max 1.517 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 48 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 80 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 4 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .731053(7) .522947(7) .370044(8) .01540(4) Uani ? ? 1.00000 ? ? C1 .72823(19) .6979(2) .3662(2) .0148(9) Uani ? ? 1.00000 ? ? N2 .8115(2) .77045(19) .3374(2) .0170(8) Uani ? ? 1.00000 ? ? C21 .9224(2) .7322(2) .2972(2) .0205(10) Uani ? ? 1.00000 ? ? C22 .8882(3) .6667(3) .1725(3) .0264(12) Uani ? ? 1.00000 ? ? C23 .9940(2) .6547(3) .3962(3) .0276(12) Uani ? ? 1.00000 ? ? C24 .9934(3) .8419(3) .2809(4) .0388(16) Uani ? ? 1.00000 ? ? C3 .7796(2) .8868(2) .3488(3) .0210(10) Uani ? ? 1.00000 ? ? C4 .6753(2) .8865(2) .3835(2) .0205(10) Uani ? ? 1.00000 ? ? N5 .64444(18) .76994(18) .3941(2) .0161(8) Uani ? ? 1.00000 ? ? C51 .5354(2) .7301(2) .4351(2) .0182(9) Uani ? ? 1.00000 ? ? C52 .4633(2) .6515(3) .3330(3) .0239(11) Uani ? ? 1.00000 ? ? C53 .5691(2) .6651(3) .5577(3) .0231(11) Uani ? ? 1.00000 ? ? C54 .4631(3) .8382(3) .4535(3) .0287(12) Uani ? ? 1.00000 ? ? N .7345(2) .3481(3) .3759(3) .0279(12) Uani ? ? 1.00000 ? ? C .7737(2) .2525(2) .3787(3) .0255(12) Uani ? ? 1.00000 ? ? O .8091(2) .1543(2) .3804(3) .0494(14) Uani ? ? 1.00000 ? ? H22a .84297 .71776 .11198 .04500 Uiso ? ? 1.00000 ? ? H22b .84230 .59929 .18257 .04500 Uiso ? ? 1.00000 ? ? H22c .95606 .64276 .14436 .04500 Uiso ? ? 1.00000 ? ? H23a 1.01358 .69768 .47225 .04900 Uiso ? ? 1.00000 ? ? H23b 1.06300 .63075 .37061 .04900 Uiso ? ? 1.00000 ? ? H23c .94924 .58729 .40882 .04900 Uiso ? ? 1.00000 ? ? H24a 1.01458 .88223 .35815 .07100 Uiso ? ? 1.00000 ? ? H24b .94751 .89300 .22119 .07100 Uiso ? ? 1.00000 ? ? H24c 1.06190 .81989 .25229 .07100 Uiso ? ? 1.00000 ? ? H3 .82284 .95422 .33448 .03200 Uiso ? ? 1.00000 ? ? H4 .63152 .95373 .39824 .02900 Uiso ? ? 1.00000 ? ? H52a .44384 .69494 .25746 .04000 Uiso ? ? 1.00000 ? ? H52b .39392 .62698 .35808 .04000 Uiso ? ? 1.00000 ? ? H52c .50815 .58431 .32035 .04000 Uiso ? ? 1.00000 ? ? H53a .61333 .71595 .61824 .03500 Uiso ? ? 1.00000 ? ? H53b .61475 .59799 .54692 .03500 Uiso ? ? 1.00000 ? ? H53c .50051 .64066 .58465 .03500 Uiso ? ? 1.00000 ? ? H54a .50646 .88707 .51647 .04700 Uiso ? ? 1.00000 ? ? H54b .39294 .81353 .47821 .04700 Uiso ? ? 1.00000 ? ? H54c .44355 .88090 .37768 .04700 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .01457(5) .01105(4) .02032(5) .00009(3) .00287(3) -.00080(3) C1 .0158(10) .0130(9) .0151(9) -.0002(7) .0023(8) .0007(7) N2 .0211(9) .0136(8) .0168(9) -.0019(7) .0052(7) -.0003(7) C21 .0203(11) .0212(11) .0221(11) -.0025(9) .0088(9) -.0022(9) C22 .0302(13) .0317(14) .0188(11) .0025(11) .0087(10) -.0018(10) C23 .0171(11) .0376(15) .0267(13) .0007(11) .0007(10) -.0024(12) C24 .0338(16) .0306(15) .060(2) -.0127(13) .0281(16) -.0069(16) C3 .0274(12) .0144(9) .0218(11) -.0025(9) .0066(9) .0008(9) C4 .0275(12) .0140(9) .0214(11) .0010(9) .0085(9) .0013(8) N5 .0186(9) .0125(8) .0176(9) .0006(7) .0042(7) .0003(7) C51 .0175(10) .0179(10) .0198(10) .0022(8) .0053(8) .0029(8) C52 .0192(11) .0252(12) .0264(13) .0003(9) .0023(9) .0013(10) C53 .0245(12) .0259(12) .0205(11) .0006(10) .0080(10) .0047(10) C54 .0288(13) .0243(12) .0364(15) .0078(11) .0150(12) .0011(12) N .0211(11) .0163(10) .0458(17) -.0002(8) .0055(11) -.0013(10) C .0157(12) .0181(11) .0416(17) -.0009(9) .0028(11) -.0040(11) O .0385(14) .0170(10) .088(2) .0080(10) .0011(14) -.0081(13) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C1 . . 1.986(3) ? Au N . . 1.985(3) ? C1 N2 . . 1.358(3) ? C1 N5 . . 1.356(3) ? N2 C21 . . 1.513(4) ? N2 C3 . . 1.384(4) ? C21 C22 . . 1.536(4) ? C21 C23 . . 1.511(4) ? C21 C24 . . 1.527(5) ? C22 H22a . . .955 ? C22 H22b . . .953 ? C22 H22c . . .946 ? C23 H23a . . .952 ? C23 H23b . . .945 ? C23 H23c . . .952 ? C24 H24a . . .950 ? C24 H24b . . .954 ? C24 H24c . . .949 ? C3 C4 . . 1.347(4) ? C3 H3 . . .948 ? C4 N5 . . 1.381(3) ? C4 H4 . . .950 ? N5 C51 . . 1.502(4) ? C51 C52 . . 1.542(4) ? C51 C53 . . 1.512(4) ? C51 C54 . . 1.525(4) ? C52 H52a . . .950 ? C52 H52b . . .949 ? C52 H52c . . .950 ? C53 H53a . . .950 ? C53 H53b . . .950 ? C53 H53c . . .950 ? C54 H54a . . .948 ? C54 H54b . . .955 ? C54 H54c . . .949 ? N C . . 1.175(4) ? C O . . 1.188(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C1 Au N . . . 179.36(9) ? Au C1 N2 . . . 126.93(18) ? Au C1 N5 . . . 127.40(18) ? N2 C1 N5 . . . 105.7(2) ? C1 N2 C21 . . . 126.0(2) ? C1 N2 C3 . . . 109.8(2) ? C21 N2 C3 . . . 124.2(2) ? N2 C21 C22 . . . 108.2(2) ? N2 C21 C23 . . . 109.9(2) ? N2 C21 C24 . . . 108.5(2) ? C22 C21 C23 . . . 111.4(2) ? C22 C21 C24 . . . 109.9(3) ? C23 C21 C24 . . . 108.9(2) ? C21 C22 H22a . . . 109.5 ? C21 C22 H22b . . . 109.7 ? C21 C22 H22c . . . 110.0 ? H22a C22 H22b . . . 108.8 ? H22a C22 H22c . . . 109.4 ? H22b C22 H22c . . . 109.5 ? C21 C23 H23a . . . 109.3 ? C21 C23 H23b . . . 109.7 ? C21 C23 H23c . . . 109.3 ? H23a C23 H23b . . . 109.7 ? H23a C23 H23c . . . 109.1 ? H23b C23 H23c . . . 109.8 ? C21 C24 H24a . . . 109.8 ? C21 C24 H24b . . . 109.4 ? C21 C24 H24c . . . 109.7 ? H24a C24 H24b . . . 109.2 ? H24a C24 H24c . . . 109.5 ? H24b C24 H24c . . . 109.2 ? N2 C3 C4 . . . 107.4(2) ? N2 C3 H3 . . . 126.4 ? C4 C3 H3 . . . 126.3 ? C3 C4 N5 . . . 107.0(2) ? C3 C4 H4 . . . 126.4 ? N5 C4 H4 . . . 126.6 ? C1 N5 C4 . . . 110.2(2) ? C1 N5 C51 . . . 125.4(2) ? C4 N5 C51 . . . 124.3(2) ? N5 C51 C52 . . . 109.2(2) ? N5 C51 C53 . . . 109.1(2) ? N5 C51 C54 . . . 108.8(2) ? C52 C51 C53 . . . 111.6(2) ? C52 C51 C54 . . . 108.9(2) ? C53 C51 C54 . . . 109.1(2) ? C51 C52 H52a . . . 109.4 ? C51 C52 H52b . . . 109.5 ? C51 C52 H52c . . . 109.4 ? H52a C52 H52b . . . 109.6 ? H52a C52 H52c . . . 109.4 ? H52b C52 H52c . . . 109.6 ? C51 C53 H53a . . . 109.4 ? C51 C53 H53b . . . 109.5 ? C51 C53 H53c . . . 109.4 ? H53a C53 H53b . . . 109.5 ? H53a C53 H53c . . . 109.5 ? H53b C53 H53c . . . 109.5 ? C51 C54 H54a . . . 109.7 ? C51 C54 H54b . . . 109.3 ? C51 C54 H54c . . . 109.7 ? H54a C54 H54b . . . 109.2 ? H54a C54 H54c . . . 109.7 ? H54b C54 H54c . . . 109.2 ? Au N C . . . 158.2(2) ? N C O . . . 177.5(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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 800 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min -18 _reflns_limit_l_max 18 _reflns_number_observed ? _reflns_d_resolution_high .584 _reflns_d_resolution_low 11.416 _diffrn_reflns_av_sigmaI/netI .042 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .033 _refine_ls_wR_factor_all .039 _refine_ls_goodness_of_fit_all .991 _refine_ls_shift/su_mean .0004 #===END data_sb6013 _database_code_depnum_ccdc_archive 'CCDC 247539' _audit_creation_method Xtal3.6 _audit_creation_date 04-01-02 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C13 H23 Au1 N2 O2' _chemical_formula_moiety 'C13 H23 Au1 N2 O2' _chemical_formula_weight 436.35 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 13.1458(8) _cell_length_b 9.7248(6) _cell_length_c 11.3223(7) _cell_angle_alpha 90.00000 _cell_angle_beta 91.456(2) _cell_angle_gamma 90.00000 _cell_volume 1446.98(15) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.003 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5229 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 37.32 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 10.164 _exptl_crystal_description prism _exptl_crystal_size_max .12 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .07 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .56 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 28862 _reflns_number_total 7566 _reflns_Friedel_coverage 0 _reflns_number_gt 5926 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.53 _diffrn_reflns_theta_full 37.53 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .039 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .028 _refine_ls_wR_factor_ref .033 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_number_reflns 5926 _refine_ls_number_parameters 163 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .003 _refine_diff_density_min -1.953 _refine_diff_density_max 1.936 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 52 .002 .002 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 92 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Au ? 0 4 -2.688 8.798 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 8 .004 .003 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' O ? 0 8 .008 .006 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .284084(7) .546452(9) .383293(8) .01533(5) Uani ? ? 1.00000 ? ? C1 .2668(2) .7338(3) .4487(2) .0144(10) Uani ? ? 1.00000 ? ? N2 .18681(16) .8189(2) .4217(2) .0149(9) Uani ? ? 1.00000 ? ? C21 .0929(2) .7805(3) .3500(2) .0190(11) Uani ? ? 1.00000 ? ? C22 .0432(2) .6549(4) .4053(3) .0276(15) Uani ? ? 1.00000 ? ? C23 .1219(2) .7527(3) .2225(2) .0245(13) Uani ? ? 1.00000 ? ? C24 .0186(3) .9006(4) .3517(3) .0324(16) Uani ? ? 1.00000 ? ? C3 .2052(2) .9466(3) .4716(2) .0167(10) Uani ? ? 1.00000 ? ? C4 .2954(2) .9406(2) .5304(2) .0151(10) Uani ? ? 1.00000 ? ? N5 .33267(16) .8090(2) .51621(18) .0136(9) Uani ? ? 1.00000 ? ? C51 .4312(2) .7582(3) .5701(2) .0144(10) Uani ? ? 1.00000 ? ? C52 .4093(2) .6371(3) .6511(2) .0206(12) Uani ? ? 1.00000 ? ? C53 .5034(2) .7157(3) .4724(2) .0194(11) Uani ? ? 1.00000 ? ? C54 .4809(2) .8721(3) .6437(2) .0180(11) Uani ? ? 1.00000 ? ? O11 .30614(16) .3662(2) .2954(2) .0238(10) Uani ? ? 1.00000 ? ? C11 .2347(2) .2732(3) .2952(3) .0205(12) Uani ? ? 1.00000 ? ? O12 .16151(19) .2717(2) .3616(2) .0315(12) Uani ? ? 1.00000 ? ? C12 .2473(3) .1641(3) .2021(3) .0310(16) Uani ? ? 1.00000 ? ? H22a .02552 .67265 .48414 .04100 Uiso ? ? 1.00000 ? ? H22b .08995 .57834 .40470 .04100 Uiso ? ? 1.00000 ? ? H22c -.01621 .62901 .36034 .04100 Uiso ? ? 1.00000 ? ? H23a .15323 .83182 .18912 .03800 Uiso ? ? 1.00000 ? ? H23b .06369 .72860 .17578 .03800 Uiso ? ? 1.00000 ? ? H23c .16985 .67793 .22013 .03800 Uiso ? ? 1.00000 ? ? H24a .04919 .97978 .31743 .04700 Uiso ? ? 1.00000 ? ? H24b .00100 .92085 .43039 .04700 Uiso ? ? 1.00000 ? ? H24c -.04121 .87762 .30669 .04700 Uiso ? ? 1.00000 ? ? H3 .16191 1.02508 .46469 .02100 Uiso ? ? 1.00000 ? ? H4 .32767 1.01391 .57335 .01900 Uiso ? ? 1.00000 ? ? H52a .36452 .66459 .71125 .03100 Uiso ? ? 1.00000 ? ? H52b .47100 .60385 .68650 .03100 Uiso ? ? 1.00000 ? ? H52c .37815 .56433 .60625 .03100 Uiso ? ? 1.00000 ? ? H53a .51629 .79256 .42270 .03000 Uiso ? ? 1.00000 ? ? H53b .47291 .64429 .42607 .03000 Uiso ? ? 1.00000 ? ? H53c .56576 .68380 .50634 .03000 Uiso ? ? 1.00000 ? ? H54a .49527 .94895 .59423 .02700 Uiso ? ? 1.00000 ? ? H54b .54279 .83980 .67897 .02700 Uiso ? ? 1.00000 ? ? H54c .43629 .90053 .70366 .02700 Uiso ? ? 1.00000 ? ? H12a .31232 .12101 .21151 .04700 Uiso ? ? 1.00000 ? ? H12b .24199 .20359 .12530 .04700 Uiso ? ? 1.00000 ? ? H12c .19608 .09545 .20934 .04700 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .01522(5) .01178(4) .01888(5) .00020(3) -.00166(3) -.00329(3) C1 .0145(10) .0149(10) .0137(9) .0006(8) -.0003(8) -.0018(8) N2 .0118(9) .0152(9) .0177(9) .0008(7) -.0018(7) -.0012(7) C21 .0129(11) .0258(13) .0180(11) .0024(9) -.0042(9) -.0052(10) C22 .0213(14) .0380(18) .0232(13) -.0088(13) -.0014(11) -.0011(12) C23 .0228(14) .0335(16) .0168(11) .0015(12) -.0049(10) -.0027(11) C24 .0187(14) .0378(18) .0403(18) .0102(13) -.0102(13) -.0138(15) C3 .0155(11) .0153(11) .0194(11) .0033(9) -.0015(8) -.0034(9) C4 .0146(10) .0128(10) .0180(10) .0001(8) -.0011(8) -.0023(8) N5 .0147(9) .0107(8) .0153(8) .0011(7) -.0012(7) -.0015(7) C51 .0132(10) .0147(10) .0152(10) .0020(8) -.0024(8) -.0003(8) C52 .0230(13) .0184(11) .0203(11) -.0013(10) -.0009(9) .0049(10) C53 .0180(12) .0220(12) .0181(11) .0026(10) -.0009(9) -.0020(9) C54 .0182(11) .0186(11) .0168(10) -.0019(9) -.0046(9) -.0020(9) O11 .0208(10) .0170(9) .0336(11) .0002(8) -.0006(8) -.0094(8) C11 .0184(12) .0133(11) .0296(13) .0036(9) -.0034(10) -.0017(10) O12 .0278(12) .0245(11) .0427(13) -.0012(9) .0086(10) -.0056(10) C12 .0255(15) .0242(15) .0433(18) -.0005(12) -.0006(13) -.0157(13) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C1 . . 1.982(3) ? Au O11 . . 2.040(2) ? C1 N2 . . 1.367(3) ? C1 N5 . . 1.354(3) ? N2 C21 . . 1.508(3) ? N2 C3 . . 1.382(3) ? C21 C22 . . 1.527(4) ? C21 C23 . . 1.526(4) ? C21 C24 . . 1.523(5) ? C22 H22a . . .944 ? C22 H22b . . .966 ? C22 H22c . . .954 ? C23 H23a . . .955 ? C23 H23b . . .948 ? C23 H23c . . .963 ? C24 H24a . . .956 ? C24 H24b . . .947 ? C24 H24c . . .953 ? C3 C4 . . 1.346(4) ? C3 H3 . . .955 ? C4 N5 . . 1.381(3) ? C4 H4 . . .956 ? N5 C51 . . 1.501(3) ? C51 C52 . . 1.524(4) ? C51 C53 . . 1.532(4) ? C51 C54 . . 1.524(4) ? C52 H52a . . .950 ? C52 H52b . . .953 ? C52 H52c . . .956 ? C53 H53a . . .954 ? C53 H53b . . .952 ? C53 H53c . . .949 ? C54 H54a . . .956 ? C54 H54b . . .950 ? C54 H54c . . .949 ? O11 C11 . . 1.304(3) ? C11 O12 . . 1.237(4) ? C11 C12 . . 1.507(4) ? C12 H12a . . .956 ? C12 H12b . . .951 ? C12 H12c . . .953 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C1 Au O11 . . . 172.40(10) ? Au C1 N2 . . . 124.62(18) ? Au C1 N5 . . . 129.03(19) ? N2 C1 N5 . . . 106.0(2) ? C1 N2 C21 . . . 125.8(2) ? C1 N2 C3 . . . 109.1(2) ? C21 N2 C3 . . . 125.1(2) ? N2 C21 C22 . . . 109.3(2) ? N2 C21 C23 . . . 109.5(2) ? N2 C21 C24 . . . 108.6(2) ? C22 C21 C23 . . . 111.5(2) ? C22 C21 C24 . . . 109.1(2) ? C23 C21 C24 . . . 108.9(2) ? C21 C22 H22a . . . 111.1 ? C21 C22 H22b . . . 109.5 ? C21 C22 H22c . . . 110.2 ? H22a C22 H22b . . . 108.6 ? H22a C22 H22c . . . 109.6 ? H22b C22 H22c . . . 107.8 ? C21 C23 H23a . . . 110.6 ? C21 C23 H23b . . . 110.7 ? C21 C23 H23c . . . 109.8 ? H23a C23 H23b . . . 109.2 ? H23a C23 H23c . . . 107.9 ? H23b C23 H23c . . . 108.5 ? C21 C24 H24a . . . 109.7 ? C21 C24 H24b . . . 110.1 ? C21 C24 H24c . . . 109.6 ? H24a C24 H24b . . . 109.2 ? H24a C24 H24c . . . 108.7 ? H24b C24 H24c . . . 109.5 ? N2 C3 C4 . . . 107.8(2) ? N2 C3 H3 . . . 125.9 ? C4 C3 H3 . . . 126.3 ? C3 C4 N5 . . . 107.0(2) ? C3 C4 H4 . . . 126.4 ? N5 C4 H4 . . . 126.6 ? C1 N5 C4 . . . 110.0(2) ? C1 N5 C51 . . . 125.7(2) ? C4 N5 C51 . . . 124.2(2) ? N5 C51 C52 . . . 108.9(2) ? N5 C51 C53 . . . 109.8(2) ? N5 C51 C54 . . . 109.7(2) ? C52 C51 C53 . . . 110.8(2) ? C52 C51 C54 . . . 108.5(2) ? C53 C51 C54 . . . 109.0(2) ? C51 C52 H52a . . . 110.1 ? C51 C52 H52b . . . 110.1 ? C51 C52 H52c . . . 109.7 ? H52a C52 H52b . . . 109.3 ? H52a C52 H52c . . . 108.9 ? H52b C52 H52c . . . 108.7 ? C51 C53 H53a . . . 109.7 ? C51 C53 H53b . . . 109.6 ? C51 C53 H53c . . . 109.9 ? H53a C53 H53b . . . 109.0 ? H53a C53 H53c . . . 109.2 ? H53b C53 H53c . . . 109.4 ? C51 C54 H54a . . . 109.6 ? C51 C54 H54b . . . 109.9 ? C51 C54 H54c . . . 109.8 ? H54a C54 H54b . . . 108.9 ? H54a C54 H54c . . . 109.0 ? H54b C54 H54c . . . 109.5 ? Au O11 C11 . . . 119.06(19) ? O11 C11 O12 . . . 125.3(3) ? O11 C11 C12 . . . 113.4(3) ? O12 C11 C12 . . . 121.2(3) ? C11 C12 H12a . . . 110.1 ? C11 C12 H12b . . . 110.4 ? C11 C12 H12c . . . 110.1 ? H12a C12 H12b . . . 108.9 ? H12a C12 H12c . . . 108.3 ? H12b C12 H12c . . . 109.0 ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 840 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -19 _reflns_limit_l_max 19 _reflns_number_observed ? _reflns_d_resolution_high .583 _reflns_d_resolution_low 13.107 _diffrn_reflns_av_sigmaI/netI .056 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .045 _refine_ls_wR_factor_all .035 _refine_ls_goodness_of_fit_all .981 _refine_ls_shift/su_mean .0001 #===END data_sb6016 _database_code_depnum_ccdc_archive 'CCDC 247540' _audit_creation_method Xtal3.6 _audit_creation_date 04-01-09 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C11 H20 Au1 N3 O3' _chemical_formula_moiety 'C11 H20 Au1 N3 O3' _chemical_formula_weight 439.31 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 6.9558(10) _cell_length_b 14.226(2) _cell_length_c 14.223(2) _cell_angle_alpha 90.00000 _cell_angle_beta 97.402(4) _cell_angle_gamma 90.00000 _cell_volume 1395.7(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.091 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6153 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 37.43 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 10.545 _exptl_crystal_description brick _exptl_crystal_size_max .18 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .52 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 27135 _reflns_number_total 7075 _reflns_Friedel_coverage 0 _reflns_number_gt 5739 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.6 _diffrn_reflns_theta_full 37.6 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .046 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .032 _refine_ls_wR_factor_ref .047 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_number_reflns 5739 _refine_ls_number_parameters 163 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .008 _refine_diff_density_min -2.923 _refine_diff_density_max 2.791 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 44 .002 .002 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 80 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Au ? 0 4 -2.688 8.798 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 12 .004 .003 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' O ? 0 12 .008 .006 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .28561(2) .176820(10) .587480(10) .01381(6) Uani ? ? 1.00000 ? ? C1 .4067(5) .1953(2) .4708(2) .0130(11) Uani ? ? 1.00000 ? ? N2 .5507(4) .25634(18) .45836(18) .0127(10) Uani ? ? 1.00000 ? ? C21 .6430(5) .3253(2) .5309(3) .0158(12) Uani ? ? 1.00000 ? ? C22 .7465(5) .2710(3) .6165(3) .0219(14) Uani ? ? 1.00000 ? ? C23 .4865(5) .3900(2) .5595(2) .0179(13) Uani ? ? 1.00000 ? ? C24 .7915(6) .3838(3) .4875(3) .0260(16) Uani ? ? 1.00000 ? ? C3 .5998(5) .2490(2) .3682(2) .0180(13) Uani ? ? 1.00000 ? ? C4 .4836(5) .1817(2) .3236(3) .0190(14) Uani ? ? 1.00000 ? ? N5 .3653(4) .1498(2) .38651(19) .0140(10) Uani ? ? 1.00000 ? ? C51 .2057(5) .0795(3) .3631(3) .0192(14) Uani ? ? 1.00000 ? ? C52 .2406(6) -.0059(3) .4266(3) .0289(18) Uani ? ? 1.00000 ? ? C53 .0127(5) .1275(3) .3732(3) .0229(15) Uani ? ? 1.00000 ? ? C54 .2034(6) .0484(4) .2603(3) .036(2) Uani ? ? 1.00000 ? ? N0 .2264(5) .1087(2) .7732(2) .0232(14) Uani ? ? 1.00000 ? ? O1 .1505(4) .16796(19) .7075(2) .0241(13) Uani ? ? 1.00000 ? ? O2 .3572(6) .0574(3) .7544(3) .054(2) Uani ? ? 1.00000 ? ? O3 .1602(5) .1097(3) .8488(2) .0374(16) Uani ? ? 1.00000 ? ? H22a .84352 .23118 .59630 .03400 Uiso ? ? 1.00000 ? ? H22b .65592 .23370 .64459 .03400 Uiso ? ? 1.00000 ? ? H22c .80667 .31420 .66241 .03400 Uiso ? ? 1.00000 ? ? H23a .42499 .42212 .50518 .02800 Uiso ? ? 1.00000 ? ? H23b .54351 .43432 .60454 .02800 Uiso ? ? 1.00000 ? ? H23c .39277 .35382 .58673 .02800 Uiso ? ? 1.00000 ? ? H24a .73022 .41841 .43411 .04100 Uiso ? ? 1.00000 ? ? H24b .88833 .34431 .46699 .04100 Uiso ? ? 1.00000 ? ? H24c .85192 .42744 .53306 .04100 Uiso ? ? 1.00000 ? ? H3 .69716 .28422 .34227 .02300 Uiso ? ? 1.00000 ? ? H4 .48361 .16073 .25991 .02400 Uiso ? ? 1.00000 ? ? H52a .36170 -.03378 .41933 .04500 Uiso ? ? 1.00000 ? ? H52b .13987 -.05046 .41203 .04500 Uiso ? ? 1.00000 ? ? H52c .24290 .01313 .49169 .04500 Uiso ? ? 1.00000 ? ? H53a -.00525 .18029 .33162 .03400 Uiso ? ? 1.00000 ? ? H53b .01094 .14810 .43655 .03400 Uiso ? ? 1.00000 ? ? H53c -.09209 .08451 .35689 .03400 Uiso ? ? 1.00000 ? ? H54a .18077 .10271 .21940 .05500 Uiso ? ? 1.00000 ? ? H54b .10206 .00470 .24324 .05500 Uiso ? ? 1.00000 ? ? H54c .32385 .02163 .25089 .05500 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .01480(6) .01525(6) .01148(6) .00008(4) .00208(4) .00133(4) C1 .0142(12) .0108(11) .0141(13) .0018(9) .0018(10) -.0003(9) N2 .0137(10) .0129(11) .0118(10) -.0006(8) .0024(8) .0000(8) C21 .0166(13) .0129(13) .0176(14) -.0006(10) .0014(10) -.0030(10) C22 .0200(14) .0233(16) .0203(15) .0008(12) -.0056(12) .0003(12) C23 .0244(15) .0123(13) .0172(13) .0022(11) .0035(11) -.0001(10) C24 .0262(17) .0224(17) .0311(19) -.0110(14) .0103(14) -.0078(14) C3 .0204(14) .0211(15) .0132(13) .0007(11) .0053(11) -.0006(11) C4 .0183(14) .0258(17) .0134(13) .0020(12) .0042(11) -.0027(11) N5 .0128(11) .0162(11) .0131(11) .0016(9) .0021(8) -.0024(9) C51 .0138(13) .0210(15) .0223(15) -.0003(11) .0000(11) -.0069(12) C52 .0234(17) .0180(16) .044(2) -.0024(13) -.0024(16) -.0026(15) C53 .0120(13) .032(2) .0248(17) .0001(12) .0025(11) -.0010(14) C54 .0248(18) .051(3) .034(2) -.0120(18) .0090(16) -.025(2) N0 .0245(14) .0256(16) .0191(13) -.0064(12) .0013(11) .0051(12) O1 .0219(13) .0350(16) .0163(12) .0068(10) .0060(10) .0070(10) O2 .071(3) .049(2) .045(2) .036(2) .022(2) .0265(18) O3 .0409(17) .056(2) .0159(12) -.0104(16) .0044(12) .0073(14) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C1 . . 1.973(3) ? Au O1 . . 2.056(3) ? Au O2 . . 2.909(4) ? C1 N2 . . 1.354(4) ? C1 N5 . . 1.360(4) ? N2 C21 . . 1.506(4) ? N2 C3 . . 1.372(4) ? C21 C22 . . 1.539(5) ? C21 C23 . . 1.521(5) ? C21 C24 . . 1.519(5) ? C22 H22a . . .953 ? C22 H22b . . .950 ? C22 H22c . . .954 ? C23 H23a . . .950 ? C23 H23b . . .948 ? C23 H23c . . .951 ? C24 H24a . . .958 ? C24 H24b . . .951 ? C24 H24c . . .955 ? C3 C4 . . 1.357(5) ? C3 H3 . . .954 ? C4 N5 . . 1.369(5) ? C4 H4 . . .954 ? N5 C51 . . 1.499(4) ? C51 C52 . . 1.514(6) ? C51 C53 . . 1.529(5) ? C51 C54 . . 1.526(6) ? C52 H52a . . .949 ? C52 H52b . . .948 ? C52 H52c . . .962 ? C53 H53a . . .954 ? C53 H53b . . .950 ? C53 H53c . . .957 ? C54 H54a . . .967 ? C54 H54b . . .948 ? C54 H54c . . .946 ? N0 O1 . . 1.317(4) ? N0 O2 . . 1.223(6) ? N0 O3 . . 1.223(5) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C1 Au O1 . . . 175.50(12) ? C1 Au O2 . . . 135.85(13) ? O1 Au O2 . . . 48.34(12) ? Au C1 N2 . . . 126.7(2) ? Au C1 N5 . . . 127.8(2) ? N2 C1 N5 . . . 105.5(3) ? C1 N2 C21 . . . 125.8(3) ? C1 N2 C3 . . . 110.5(3) ? C21 N2 C3 . . . 123.6(3) ? N2 C21 C22 . . . 109.2(2) ? N2 C21 C23 . . . 108.7(3) ? N2 C21 C24 . . . 109.3(3) ? C22 C21 C23 . . . 111.8(3) ? C22 C21 C24 . . . 108.8(3) ? C23 C21 C24 . . . 108.9(3) ? C21 C22 H22a . . . 109.7 ? C21 C22 H22b . . . 110.2 ? C21 C22 H22c . . . 109.7 ? H22a C22 H22b . . . 109.2 ? H22a C22 H22c . . . 108.9 ? H22b C22 H22c . . . 109.1 ? C21 C23 H23a . . . 109.7 ? C21 C23 H23b . . . 109.4 ? C21 C23 H23c . . . 109.4 ? H23a C23 H23b . . . 109.6 ? H23a C23 H23c . . . 109.3 ? H23b C23 H23c . . . 109.5 ? C21 C24 H24a . . . 110.3 ? C21 C24 H24b . . . 110.3 ? C21 C24 H24c . . . 110.1 ? H24a C24 H24b . . . 108.7 ? H24a C24 H24c . . . 108.4 ? H24b C24 H24c . . . 109.0 ? N2 C3 C4 . . . 106.6(3) ? N2 C3 H3 . . . 126.6 ? C4 C3 H3 . . . 126.8 ? C3 C4 N5 . . . 107.5(3) ? C3 C4 H4 . . . 126.3 ? N5 C4 H4 . . . 126.2 ? C1 N5 C4 . . . 110.0(3) ? C1 N5 C51 . . . 125.4(3) ? C4 N5 C51 . . . 124.5(3) ? N5 C51 C52 . . . 110.2(3) ? N5 C51 C53 . . . 108.4(3) ? N5 C51 C54 . . . 108.8(3) ? C52 C51 C53 . . . 112.2(3) ? C52 C51 C54 . . . 108.7(3) ? C53 C51 C54 . . . 108.5(3) ? C51 C52 H52a . . . 110.3 ? C51 C52 H52b . . . 110.4 ? C51 C52 H52c . . . 109.3 ? H52a C52 H52b . . . 109.7 ? H52a C52 H52c . . . 108.5 ? H52b C52 H52c . . . 108.6 ? C51 C53 H53a . . . 109.9 ? C51 C53 H53b . . . 110.2 ? C51 C53 H53c . . . 110.1 ? H53a C53 H53b . . . 109.1 ? H53a C53 H53c . . . 108.6 ? H53b C53 H53c . . . 108.9 ? C51 C54 H54a . . . 109.0 ? C51 C54 H54b . . . 110.5 ? C51 C54 H54c . . . 110.7 ? H54a C54 H54b . . . 108.2 ? H54a C54 H54c . . . 108.4 ? H54b C54 H54c . . . 110.0 ? O1 N0 O2 . . . 117.9(3) ? O1 N0 O3 . . . 117.0(3) ? O2 N0 O3 . . . 125.0(4) ? Au O1 N0 . . . 116.3(2) ? Au O2 N0 . . . 77.1(2) ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 840 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min -24 _reflns_limit_l_max 24 _reflns_number_observed ? _reflns_d_resolution_high .582 _reflns_d_resolution_low 9.996 _diffrn_reflns_av_sigmaI/netI .051 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .045 _refine_ls_wR_factor_all .051 _refine_ls_goodness_of_fit_all 1.062 _refine_ls_shift/su_mean .001 #===END data_sb5022 _database_code_depnum_ccdc_archive 'CCDC 247541' _audit_creation_method Xtal3.6 _audit_creation_date 04-02-23 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C12 H23 Au1 N2' _chemical_formula_moiety 'C12 H23 Au1 N2' _chemical_formula_weight 392.34 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 20.434(4) _cell_length_b 10.082(2) _cell_length_c 13.601(4) _cell_angle_alpha 90.00000 _cell_angle_beta 102.497(5) _cell_angle_gamma 90.00000 _cell_volume 2735.6(11) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5985 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 34.87 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 10.73 _exptl_crystal_description brisk _exptl_crystal_size_max .14 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .06 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .70 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 48276 _reflns_number_total 12086 _reflns_Friedel_coverage 0 _reflns_number_gt 9701 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 35.13 _diffrn_reflns_theta_full 35.13 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .043 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .028 _refine_ls_wR_factor_ref .041 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_number_reflns 9701 _refine_ls_number_parameters 271 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .004 _refine_diff_density_min -1.915 _refine_diff_density_max 3.303 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 96 .002 .002 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 184 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Au ? 0 8 -2.688 8.798 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 16 .004 .003 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au1 .627526(7) .484397(15) .698121(11) .02658(6) Uani ? ? 1.00000 ? ? Au2 .909783(6) .949388(12) .641907(9) .01941(5) Uani ? ? 1.00000 ? ? C1 .6846(2) .5461(4) .5965(3) .0316(17) Uani ? ? 1.00000 ? ? C11 .57294(17) .4264(3) .8005(3) .0226(13) Uani ? ? 1.00000 ? ? N12 .50619(14) .4067(3) .7865(2) .0233(12) Uani ? ? 1.00000 ? ? C121 .45735(18) .4140(4) .6868(3) .0268(14) Uani ? ? 1.00000 ? ? C122 .4781(2) .3139(4) .6160(3) .0341(18) Uani ? ? 1.00000 ? ? C123 .4584(2) .5550(4) .6454(4) .038(2) Uani ? ? 1.00000 ? ? C124 .3873(2) .3804(5) .7004(3) .039(2) Uani ? ? 1.00000 ? ? C13 .4889(2) .3753(4) .8762(3) .0303(16) Uani ? ? 1.00000 ? ? C14 .5446(2) .3744(4) .9472(3) .0308(16) Uani ? ? 1.00000 ? ? N15 .59678(16) .4049(3) .9009(2) .0261(13) Uani ? ? 1.00000 ? ? C151 .6694(2) .4111(4) .9547(3) .0309(16) Uani ? ? 1.00000 ? ? C152 .7086(2) .3101(5) .9059(4) .039(2) Uani ? ? 1.00000 ? ? C153 .6956(2) .5519(4) .9478(4) .041(2) Uani ? ? 1.00000 ? ? C154 .6760(3) .3720(5) 1.0650(3) .046(2) Uani ? ? 1.00000 ? ? C2 .8850(2) 1.0090(4) .4934(3) .0248(14) Uani ? ? 1.00000 ? ? C21 .94045(16) .8887(3) .7880(2) .0191(12) Uani ? ? 1.00000 ? ? N22 .90358(14) .8626(3) .8572(2) .0207(11) Uani ? ? 1.00000 ? ? C221 .82952(16) .8827(3) .8417(3) .0225(13) Uani ? ? 1.00000 ? ? C222 .79442(18) .7887(4) .7592(3) .0310(16) Uani ? ? 1.00000 ? ? C223 .8131(2) 1.0268(4) .8161(3) .0298(16) Uani ? ? 1.00000 ? ? C224 .80711(19) .8493(4) .9397(3) .0295(16) Uani ? ? 1.00000 ? ? C23 .94377(18) .8171(4) .9456(3) .0265(15) Uani ? ? 1.00000 ? ? C24 1.00680(18) .8148(4) .9310(2) .0263(15) Uani ? ? 1.00000 ? ? N25 1.00457(13) .8597(3) .8356(2) .0197(11) Uani ? ? 1.00000 ? ? C251 1.06525(15) .8784(3) .7908(2) .0209(12) Uani ? ? 1.00000 ? ? C252 1.05863(17) .7887(3) .6988(3) .0247(14) Uani ? ? 1.00000 ? ? C253 1.0710(2) 1.0239(3) .7639(3) .0255(14) Uani ? ? 1.00000 ? ? C254 1.12768(17) .8362(4) .8683(3) .0291(16) Uani ? ? 1.00000 ? ? H122a .47722 .22724 .64364 .05100 Uiso ? ? 1.00000 ? ? H122b .52242 .33283 .60844 .05100 Uiso ? ? 1.00000 ? ? H122c .44821 .31744 .55218 .05100 Uiso ? ? 1.00000 ? ? H123a .44523 .61542 .69004 .05500 Uiso ? ? 1.00000 ? ? H123b .42824 .55939 .58124 .05500 Uiso ? ? 1.00000 ? ? H123c .50245 .57478 .63749 .05500 Uiso ? ? 1.00000 ? ? H124a .37332 .44185 .74485 .05800 Uiso ? ? 1.00000 ? ? H124b .38768 .29305 .72956 .05800 Uiso ? ? 1.00000 ? ? H124c .35614 .38061 .63771 .05800 Uiso ? ? 1.00000 ? ? H13 .44455 .35755 .88626 .03700 Uiso ? ? 1.00000 ? ? H14 .54798 .35539 1.01667 .03900 Uiso ? ? 1.00000 ? ? H152a .69120 .22332 .91304 .05900 Uiso ? ? 1.00000 ? ? H152b .75438 .31237 .94159 .05900 Uiso ? ? 1.00000 ? ? H152c .70489 .33117 .83863 .05900 Uiso ? ? 1.00000 ? ? H153a .67074 .61231 .97773 .06200 Uiso ? ? 1.00000 ? ? H153b .69240 .57459 .87884 .06200 Uiso ? ? 1.00000 ? ? H153c .74189 .55579 .98179 .06200 Uiso ? ? 1.00000 ? ? H154a .65044 .43710 1.09427 .06900 Uiso ? ? 1.00000 ? ? H154b .72091 .37720 1.09838 .06900 Uiso ? ? 1.00000 ? ? H154c .65769 .28830 1.06961 .06900 Uiso ? ? 1.00000 ? ? H1a .67010 .50288 .53339 .04800 Uiso ? ? 1.00000 ? ? H1b .73074 .52789 .62206 .04800 Uiso ? ? 1.00000 ? ? H1c .67915 .63970 .58548 .04800 Uiso ? ? 1.00000 ? ? H222a .80655 .69886 .77919 .04700 Uiso ? ? 1.00000 ? ? H222b .80786 .80679 .69834 .04700 Uiso ? ? 1.00000 ? ? H222c .74742 .79790 .75016 .04700 Uiso ? ? 1.00000 ? ? H223a .83612 1.08235 .86879 .04600 Uiso ? ? 1.00000 ? ? H223b .76619 1.04046 .80698 .04600 Uiso ? ? 1.00000 ? ? H223c .82663 1.04934 .75518 .04600 Uiso ? ? 1.00000 ? ? H224a .82865 .90812 .99227 .04400 Uiso ? ? 1.00000 ? ? H224b .81894 .76081 .95938 .04400 Uiso ? ? 1.00000 ? ? H224c .75995 .86013 .93003 .04400 Uiso ? ? 1.00000 ? ? H23 .92901 .79185 1.00611 .03400 Uiso ? ? 1.00000 ? ? H24 1.04621 .78572 .97876 .03300 Uiso ? ? 1.00000 ? ? H252a 1.05506 .69901 .71844 .03800 Uiso ? ? 1.00000 ? ? H252b 1.09682 .79906 .67073 .03800 Uiso ? ? 1.00000 ? ? H252c 1.01944 .81263 .65042 .03800 Uiso ? ? 1.00000 ? ? H253a 1.07483 1.07621 .82348 .03900 Uiso ? ? 1.00000 ? ? H253b 1.03189 1.05011 .71643 .03900 Uiso ? ? 1.00000 ? ? H253c 1.10927 1.03654 .73672 .03900 Uiso ? ? 1.00000 ? ? H254a 1.13298 .89003 .92530 .04300 Uiso ? ? 1.00000 ? ? H254b 1.16587 .84491 .83821 .04300 Uiso ? ? 1.00000 ? ? H254c 1.12343 .74562 .88539 .04300 Uiso ? ? 1.00000 ? ? H2a .86097 1.09069 .48747 .03700 Uiso ? ? 1.00000 ? ? H2b .85806 .94362 .45327 .03700 Uiso ? ? 1.00000 ? ? H2c .92473 1.02214 .46876 .03700 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au1 .02141(7) .03453(7) .02358(7) -.00592(5) .00439(5) .00057(5) Au2 .01948(6) .02211(6) .01643(6) .00115(4) .00339(4) .00065(4) C1 .0266(18) .048(2) .0204(16) -.0121(16) .0055(13) -.0003(14) C11 .0212(15) .0223(14) .0245(15) -.0015(11) .0056(12) -.0004(11) N12 .0197(13) .0261(13) .0248(13) -.0016(10) .0058(10) -.0024(11) C121 .0207(15) .0285(16) .0297(17) -.0014(13) .0026(13) -.0053(13) C122 .032(2) .036(2) .0318(19) -.0023(16) .0019(15) -.0088(16) C123 .032(2) .033(2) .042(2) -.0007(16) -.0057(17) .0012(17) C124 .0240(18) .052(3) .042(2) -.0068(17) .0097(16) -.007(2) C13 .0291(18) .0332(18) .0321(18) -.0038(14) .0146(15) -.0045(15) C14 .036(2) .0320(17) .0263(17) -.0012(15) .0114(15) -.0038(14) N15 .0275(15) .0251(14) .0260(14) -.0024(11) .0063(11) -.0019(11) C151 .0309(18) .0318(17) .0265(17) -.0016(15) -.0014(14) -.0030(14) C152 .027(2) .039(2) .048(2) .0037(16) -.0017(17) -.0009(19) C153 .037(2) .033(2) .045(3) -.0087(17) -.0065(19) -.0024(18) C154 .052(3) .054(3) .0252(19) -.002(2) -.0038(18) .0007(19) C2 .0283(17) .0265(16) .0193(14) -.0013(13) .0042(13) .0010(12) C21 .0181(13) .0215(13) .0177(13) -.0012(10) .0040(10) -.0014(10) N22 .0198(12) .0231(12) .0194(12) -.0014(10) .0049(10) .0008(10) C221 .0190(14) .0252(14) .0239(15) .0008(11) .0059(12) -.0007(12) C222 .0212(16) .039(2) .0314(18) -.0023(14) .0026(14) -.0067(15) C223 .0271(18) .0275(16) .037(2) .0068(13) .0123(15) .0014(14) C224 .0255(17) .0337(18) .0332(18) .0007(14) .0151(14) -.0000(15) C23 .0249(16) .0362(18) .0187(14) .0022(13) .0054(12) .0061(13) C24 .0254(16) .0342(17) .0185(14) -.0003(13) .0028(12) .0079(13) N25 .0173(12) .0223(12) .0201(12) -.0010(9) .0055(9) .0020(9) C251 .0159(13) .0241(14) .0230(14) -.0013(11) .0049(11) .0010(11) C252 .0236(15) .0241(15) .0284(16) .0009(12) .0099(13) -.0025(12) C253 .0265(17) .0223(14) .0278(17) -.0038(12) .0059(14) .0017(12) C254 .0182(15) .0352(18) .0323(18) -.0022(13) .0023(13) .0049(15) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au1 C1 . . 2.088(4) ? Au1 C11 . . 2.049(4) ? Au2 C2 . . 2.063(4) ? Au2 C21 . . 2.044(3) ? C1 H1a . . .951 ? C1 H1b . . .949 ? C1 H1c . . .958 ? C11 N12 . . 1.351(5) ? C11 N15 . . 1.364(5) ? N12 C121 . . 1.502(4) ? N12 C13 . . 1.377(5) ? C121 C122 . . 1.518(6) ? C121 C123 . . 1.531(6) ? C121 C124 . . 1.520(6) ? C122 H122a . . .953 ? C122 H122b . . .952 ? C122 H122c . . .948 ? C123 H123a . . .940 ? C123 H123b . . .954 ? C123 H123c . . .950 ? C124 H124a . . .952 ? C124 H124b . . .966 ? C124 H124c . . .948 ? C13 C14 . . 1.323(5) ? C13 H13 . . .963 ? C14 N15 . . 1.386(6) ? C14 H14 . . .952 ? N15 C151 . . 1.508(5) ? C151 C152 . . 1.532(6) ? C151 C153 . . 1.527(6) ? C151 C154 . . 1.529(6) ? C152 H152a . . .957 ? C152 H152b . . .956 ? C152 H152c . . .927 ? C153 H153a . . .940 ? C153 H153b . . .954 ? C153 H153c . . .959 ? C154 H154a . . .975 ? C154 H154b . . .934 ? C154 H154c . . .930 ? C2 H2a . . .954 ? C2 H2b . . .952 ? C2 H2c . . .952 ? C21 N22 . . 1.352(5) ? C21 N25 . . 1.362(4) ? N22 C221 . . 1.496(4) ? N22 C23 . . 1.379(4) ? C221 C222 . . 1.525(5) ? C221 C223 . . 1.515(5) ? C221 C224 . . 1.537(6) ? C222 H222a . . .962 ? C222 H222b . . .944 ? C222 H222c . . .946 ? C223 H223a . . .949 ? C223 H223b . . .950 ? C223 H223c . . .956 ? C224 H224a . . .960 ? C224 H224b . . .948 ? C224 H224c . . .950 ? C23 C24 . . 1.345(5) ? C23 H23 . . .970 ? C24 N25 . . 1.365(4) ? C24 H24 . . .964 ? N25 C251 . . 1.507(5) ? C251 C252 . . 1.527(5) ? C251 C253 . . 1.522(5) ? C251 C254 . . 1.529(4) ? C252 H252a . . .950 ? C252 H252b . . .946 ? C252 H252c . . .951 ? C253 H253a . . .956 ? C253 H253b . . .950 ? C253 H253c . . .942 ? C254 H254a . . .934 ? C254 H254b . . .960 ? C254 H254c . . .951 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C1 Au1 C11 . . . 178.64(13) ? C2 Au2 C21 . . . 176.36(15) ? Au1 C1 H1a . . . 110.5 ? Au1 C1 H1b . . . 110.6 ? Au1 C1 H1c . . . 109.5 ? H1a C1 H1b . . . 109.5 ? H1a C1 H1c . . . 107.9 ? H1b C1 H1c . . . 108.7 ? Au1 C11 N12 . . . 128.9(3) ? Au1 C11 N15 . . . 126.6(3) ? N12 C11 N15 . . . 104.4(3) ? C11 N12 C121 . . . 125.0(3) ? C11 N12 C13 . . . 110.7(3) ? C121 N12 C13 . . . 124.3(3) ? N12 C121 C122 . . . 108.5(3) ? N12 C121 C123 . . . 108.6(3) ? N12 C121 C124 . . . 109.8(3) ? C122 C121 C123 . . . 110.8(4) ? C122 C121 C124 . . . 109.2(3) ? C123 C121 C124 . . . 109.9(3) ? C121 C122 H122a . . . 109.1 ? C121 C122 H122b . . . 109.8 ? C121 C122 H122c . . . 110.0 ? H122a C122 H122b . . . 109.1 ? H122a C122 H122c . . . 109.4 ? H122b C122 H122c . . . 109.5 ? C121 C123 H123a . . . 109.6 ? C121 C123 H123b . . . 108.8 ? C121 C123 H123c . . . 109.1 ? H123a C123 H123b . . . 109.9 ? H123a C123 H123c . . . 110.3 ? H123b C123 H123c . . . 109.1 ? C121 C124 H124a . . . 110.7 ? C121 C124 H124b . . . 109.3 ? C121 C124 H124c . . . 111.0 ? H124a C124 H124b . . . 108.0 ? H124a C124 H124c . . . 109.5 ? H124b C124 H124c . . . 108.4 ? N12 C13 C14 . . . 107.7(4) ? N12 C13 H13 . . . 126.8 ? C14 C13 H13 . . . 125.5 ? C13 C14 N15 . . . 106.9(3) ? C13 C14 H14 . . . 126.4 ? N15 C14 H14 . . . 126.7 ? C11 N15 C14 . . . 110.3(3) ? C11 N15 C151 . . . 125.5(3) ? C14 N15 C151 . . . 124.2(3) ? N15 C151 C152 . . . 108.3(3) ? N15 C151 C153 . . . 109.2(3) ? N15 C151 C154 . . . 109.5(4) ? C152 C151 C153 . . . 111.6(4) ? C152 C151 C154 . . . 108.1(4) ? C153 C151 C154 . . . 110.0(4) ? C151 C152 H152a . . . 108.8 ? C151 C152 H152b . . . 108.0 ? C151 C152 H152c . . . 109.6 ? H152a C152 H152b . . . 108.4 ? H152a C152 H152c . . . 110.9 ? H152b C152 H152c . . . 111.0 ? C151 C153 H153a . . . 110.3 ? C151 C153 H153b . . . 109.4 ? C151 C153 H153c . . . 109.3 ? H153a C153 H153b . . . 110.0 ? H153a C153 H153c . . . 109.5 ? H153b C153 H153c . . . 108.3 ? C151 C154 H154a . . . 106.6 ? C151 C154 H154b . . . 109.3 ? C151 C154 H154c . . . 110.4 ? H154a C154 H154b . . . 108.7 ? H154a C154 H154c . . . 109.0 ? H154b C154 H154c . . . 112.7 ? Au2 C2 H2a . . . 110.3 ? Au2 C2 H2b . . . 110.4 ? Au2 C2 H2c . . . 109.8 ? H2a C2 H2b . . . 109.0 ? H2a C2 H2c . . . 108.2 ? H2b C2 H2c . . . 109.0 ? Au2 C21 N22 . . . 129.4(2) ? Au2 C21 N25 . . . 126.0(3) ? N22 C21 N25 . . . 104.6(3) ? C21 N22 C221 . . . 125.1(3) ? C21 N22 C23 . . . 110.8(3) ? C221 N22 C23 . . . 124.2(3) ? N22 C221 C222 . . . 108.7(3) ? N22 C221 C223 . . . 109.2(3) ? N22 C221 C224 . . . 109.3(3) ? C222 C221 C223 . . . 112.5(3) ? C222 C221 C224 . . . 108.8(3) ? C223 C221 C224 . . . 108.4(3) ? C221 C222 H222a . . . 109.0 ? C221 C222 H222b . . . 110.2 ? C221 C222 H222c . . . 109.7 ? H222a C222 H222b . . . 108.9 ? H222a C222 H222c . . . 108.7 ? H222b C222 H222c . . . 110.3 ? C221 C223 H223a . . . 110.1 ? C221 C223 H223b . . . 109.6 ? C221 C223 H223c . . . 109.6 ? H223a C223 H223b . . . 109.5 ? H223a C223 H223c . . . 109.0 ? H223b C223 H223c . . . 108.9 ? C221 C224 H224a . . . 109.7 ? C221 C224 H224b . . . 110.2 ? C221 C224 H224c . . . 109.8 ? H224a C224 H224b . . . 108.9 ? H224a C224 H224c . . . 108.6 ? H224b C224 H224c . . . 109.6 ? N22 C23 C24 . . . 106.6(3) ? N22 C23 H23 . . . 126.2 ? C24 C23 H23 . . . 127.2 ? C23 C24 N25 . . . 107.4(3) ? C23 C24 H24 . . . 126.3 ? N25 C24 H24 . . . 126.3 ? C21 N25 C24 . . . 110.7(3) ? C21 N25 C251 . . . 124.9(3) ? C24 N25 C251 . . . 124.3(3) ? N25 C251 C252 . . . 108.8(3) ? N25 C251 C253 . . . 109.4(3) ? N25 C251 C254 . . . 108.9(3) ? C252 C251 C253 . . . 111.8(3) ? C252 C251 C254 . . . 108.2(3) ? C253 C251 C254 . . . 109.7(3) ? C251 C252 H252a . . . 109.4 ? C251 C252 H252b . . . 109.3 ? C251 C252 H252c . . . 109.2 ? H252a C252 H252b . . . 109.8 ? H252a C252 H252c . . . 109.4 ? H252b C252 H252c . . . 109.8 ? C251 C253 H253a . . . 108.9 ? C251 C253 H253b . . . 109.5 ? C251 C253 H253c . . . 109.8 ? H253a C253 H253b . . . 108.9 ? H253a C253 H253c . . . 109.6 ? H253b C253 H253c . . . 110.1 ? C251 C254 H254a . . . 109.9 ? C251 C254 H254b . . . 108.4 ? C251 C254 H254c . . . 109.2 ? H254a C254 H254b . . . 110.0 ? H254a C254 H254c . . . 110.8 ? H254b C254 H254c . . . 108.5 ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1504 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 33 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -21 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .618 _reflns_d_resolution_low 9.955 _diffrn_reflns_av_sigmaI/netI .052 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .041 _refine_ls_wR_factor_all .044 _refine_ls_goodness_of_fit_all .984 _refine_ls_shift/su_mean .0004 #===END ######################################## data_sb5170 _database_code_depnum_ccdc_archive 'CCDC 247542' _audit_creation_method Xtal3.6 _audit_creation_date 04-01-01 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C12 H20 Au1 N3' _chemical_formula_moiety 'C12 H20 Au1 N3' _chemical_formula_weight 403.32 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 12.6785(8) _cell_length_b 12.6643(8) _cell_length_c 17.5200(10) _cell_angle_alpha 90.00000 _cell_angle_beta 92.900(2) _cell_angle_gamma 90.00000 _cell_volume 2809.5(3) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6405 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 33.8 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 10.453 _exptl_crystal_description prism _exptl_crystal_size_max .32 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .11 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .45 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 56296 _reflns_number_total 12031 _reflns_Friedel_coverage 0 _reflns_number_gt 8969 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 34.6 _diffrn_reflns_theta_full 34.6 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .088 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .048 _refine_ls_wR_factor_ref .067 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_number_reflns 8969 _refine_ls_number_parameters 289 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .004 _refine_diff_density_min -3.881 _refine_diff_density_max 8.323 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 96 .002 .002 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 160 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Au ? 0 8 -2.688 8.798 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 24 .004 .003 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au1 .888185(18) .403855(16) .632736(13) .01786(11) Uani ? ? 1.00000 ? ? Au2 .624255(17) .684799(17) .401963(12) .01654(10) Uani ? ? 1.00000 ? ? C11 .8864(5) .5502(4) .6773(3) .018(2) Uani ? ? 1.00000 ? ? N12 .9696(4) .6165(4) .6926(3) .016(2) Uani ? ? 1.00000 ? ? C121 1.0837(5) .5903(5) .6837(4) .020(3) Uani ? ? 1.00000 ? ? C122 1.1017(6) .5570(6) .6029(4) .033(4) Uani ? ? 1.00000 ? ? C123 1.1128(6) .5035(7) .7412(5) .043(4) Uani ? ? 1.00000 ? ? C124 1.1523(6) .6865(6) .7034(5) .034(4) Uani ? ? 1.00000 ? ? C13 .9349(5) .7114(5) .7215(3) .020(3) Uani ? ? 1.00000 ? ? C14 .8285(5) .7043(5) .7245(4) .023(3) Uani ? ? 1.00000 ? ? N15 .7988(4) .6058(3) .6983(3) .016(2) Uani ? ? 1.00000 ? ? C151 .6883(5) .5626(5) .6939(3) .019(3) Uani ? ? 1.00000 ? ? C152 .6564(5) .5371(5) .6117(4) .025(3) Uani ? ? 1.00000 ? ? C153 .6836(5) .4649(5) .7447(4) .027(3) Uani ? ? 1.00000 ? ? C154 .6135(5) .6480(6) .7239(4) .028(3) Uani ? ? 1.00000 ? ? C1 .8870(5) .2584(5) .5869(4) .025(3) Uani ? ? 1.00000 ? ? N1 .8831(5) .1791(5) .5617(5) .040(4) Uani ? ? 1.00000 ? ? C21 .6270(5) .7900(5) .4882(3) .019(2) Uani ? ? 1.00000 ? ? N22 .7137(4) .8367(4) .5241(3) .019(2) Uani ? ? 1.00000 ? ? C221 .8256(4) .8293(5) .4990(3) .017(2) Uani ? ? 1.00000 ? ? C222 .8280(5) .8718(6) .4196(4) .025(3) Uani ? ? 1.00000 ? ? C223 .8597(5) .7127(5) .5028(4) .025(3) Uani ? ? 1.00000 ? ? C224 .8969(5) .8930(5) .5532(4) .024(3) Uani ? ? 1.00000 ? ? C23 .6830(5) .8965(5) .5859(4) .024(3) Uani ? ? 1.00000 ? ? C24 .5779(6) .8866(5) .5886(4) .026(3) Uani ? ? 1.00000 ? ? N25 .5432(4) .8243(4) .5272(3) .019(2) Uani ? ? 1.00000 ? ? C251 .4299(5) .7947(6) .5080(4) .025(3) Uani ? ? 1.00000 ? ? C252 .4036(6) .8144(7) .4233(5) .034(4) Uani ? ? 1.00000 ? ? C253 .4113(6) .6806(6) .5279(5) .035(4) Uani ? ? 1.00000 ? ? C254 .3587(6) .8667(7) .5534(5) .036(4) Uani ? ? 1.00000 ? ? C2 .6178(5) .5772(5) .3150(4) .020(3) Uani ? ? 1.00000 ? ? N2 .6117(5) .5213(5) .2681(4) .036(3) Uani ? ? 1.00000 ? ? H122a 1.08262 .61369 .56878 .05200 Uiso ? ? 1.00000 ? ? H122b 1.06014 .49696 .58932 .05200 Uiso ? ? 1.00000 ? ? H122c 1.17435 .54085 .59807 .05200 Uiso ? ? 1.00000 ? ? H123a 1.09937 .52594 .79116 .06800 Uiso ? ? 1.00000 ? ? H123b 1.18499 .48535 .73816 .06800 Uiso ? ? 1.00000 ? ? H123c 1.07078 .44145 .72941 .06800 Uiso ? ? 1.00000 ? ? H124a 1.14148 .70984 .75437 .05200 Uiso ? ? 1.00000 ? ? H124b 1.13277 .74413 .66928 .05200 Uiso ? ? 1.00000 ? ? H124c 1.22453 .67131 .69857 .05200 Uiso ? ? 1.00000 ? ? H13 .97713 .77074 .73591 .02500 Uiso ? ? 1.00000 ? ? H14 .78256 .75614 .74237 .03000 Uiso ? ? 1.00000 ? ? H152a .65948 .59996 .58170 .04000 Uiso ? ? 1.00000 ? ? H152b .58598 .51068 .60824 .04000 Uiso ? ? 1.00000 ? ? H152c .70282 .48611 .59264 .04000 Uiso ? ? 1.00000 ? ? H153a .70452 .48464 .79610 .04000 Uiso ? ? 1.00000 ? ? H153b .73117 .41348 .72762 .04000 Uiso ? ? 1.00000 ? ? H153c .61433 .43804 .74322 .04000 Uiso ? ? 1.00000 ? ? H154a .63338 .66553 .77554 .04500 Uiso ? ? 1.00000 ? ? H154b .54269 .62543 .72022 .04500 Uiso ? ? 1.00000 ? ? H154c .61964 .71161 .69360 .04500 Uiso ? ? 1.00000 ? ? H222a .80615 .94461 .41954 .03900 Uiso ? ? 1.00000 ? ? H222b .78209 .83326 .38609 .03900 Uiso ? ? 1.00000 ? ? H222c .89813 .86872 .40259 .03900 Uiso ? ? 1.00000 ? ? H223a .85791 .68790 .55353 .03700 Uiso ? ? 1.00000 ? ? H223b .93080 .70721 .48641 .03700 Uiso ? ? 1.00000 ? ? H223c .81476 .67175 .46991 .03700 Uiso ? ? 1.00000 ? ? H224a .89630 .86712 .60291 .03800 Uiso ? ? 1.00000 ? ? H224b .87395 .96580 .55217 .03800 Uiso ? ? 1.00000 ? ? H224c .96783 .89196 .53592 .03800 Uiso ? ? 1.00000 ? ? H23 .72789 .93560 .62008 .03000 Uiso ? ? 1.00000 ? ? H24 .53437 .91907 .62510 .03200 Uiso ? ? 1.00000 ? ? H252a .41692 .88583 .41065 .05000 Uiso ? ? 1.00000 ? ? H252b .33199 .79761 .40996 .05000 Uiso ? ? 1.00000 ? ? H252c .44756 .77029 .39244 .05000 Uiso ? ? 1.00000 ? ? H253a .42738 .67094 .58105 .05100 Uiso ? ? 1.00000 ? ? H253b .45442 .63681 .49928 .05100 Uiso ? ? 1.00000 ? ? H253c .33884 .66413 .51680 .05100 Uiso ? ? 1.00000 ? ? H254a .37197 .85696 .60761 .05700 Uiso ? ? 1.00000 ? ? H254b .28554 .85248 .54177 .05700 Uiso ? ? 1.00000 ? ? H254c .37171 .93947 .54215 .05700 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au1 .02716(12) .00814(10) .01834(11) .00055(7) .00185(8) -.00060(7) Au2 .02508(11) .01355(10) .01111(10) .00094(7) .00205(7) -.00312(7) C11 .031(3) .008(2) .014(2) -.0014(19) .001(2) .0020(18) N12 .025(2) .009(2) .014(2) -.0034(16) .0015(17) .0015(16) C121 .028(3) .014(3) .018(3) -.001(2) .000(2) .002(2) C122 .031(3) .039(4) .029(3) -.003(3) .012(3) -.010(3) C123 .030(3) .051(5) .048(5) .008(3) .001(3) .032(4) C124 .038(4) .024(3) .039(4) -.006(3) .004(3) -.008(3) C13 .032(3) .010(2) .018(3) -.002(2) .002(2) -.000(2) C14 .039(3) .011(2) .019(3) -.000(2) .000(2) -.006(2) N15 .024(2) .010(2) .014(2) -.0001(15) .0034(17) .0011(16) C151 .029(3) .013(2) .017(2) -.004(2) .001(2) -.001(2) C152 .030(3) .023(3) .022(3) -.001(2) -.002(2) -.004(2) C153 .036(3) .022(3) .022(3) -.006(2) .004(2) .007(2) C154 .025(3) .024(3) .035(4) .002(2) .005(3) -.011(3) C1 .021(3) .021(3) .032(3) .002(2) .006(2) .001(3) N1 .041(4) .025(3) .055(5) -.004(3) .013(3) -.012(3) C21 .028(3) .013(2) .016(2) .001(2) .003(2) -.005(2) N22 .026(2) .016(2) .014(2) .0030(18) .0006(17) -.0026(17) C221 .022(2) .016(3) .014(2) .001(2) .0016(19) .002(2) C222 .029(3) .031(3) .016(3) .007(3) .003(2) .006(2) C223 .030(3) .016(3) .027(3) .008(2) -.003(2) -.001(2) C224 .034(3) .021(3) .018(3) -.004(2) -.002(2) -.002(2) C23 .040(3) .018(3) .013(2) .001(2) .002(2) -.009(2) C24 .039(3) .017(3) .022(3) .005(2) .005(3) -.009(2) N25 .027(2) .014(2) .017(2) .0034(17) .0046(18) -.0032(17) C251 .022(3) .030(3) .023(3) .004(2) .002(2) -.008(3) C252 .028(3) .048(5) .027(3) .006(3) -.002(3) .001(3) C253 .031(3) .037(4) .037(4) -.003(3) .005(3) .001(3) C254 .035(4) .043(4) .032(4) .012(3) .009(3) -.011(3) C2 .026(3) .019(3) .016(3) -.001(2) .006(2) .004(2) N2 .040(3) .038(4) .031(3) -.004(3) .004(3) -.016(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au1 C11 . . 2.011(6) ? Au1 C1 . . 2.009(7) ? Au2 C21 . . 2.013(6) ? Au2 C2 . . 2.043(6) ? C11 N12 . . 1.365(7) ? C11 N15 . . 1.381(8) ? N12 C121 . . 1.500(8) ? N12 C13 . . 1.384(8) ? C121 C122 . . 1.506(10) ? C121 C123 . . 1.524(11) ? C121 C124 . . 1.526(10) ? C122 H122a . . .957 ? C122 H122b . . .949 ? C122 H122c . . .951 ? C123 H123a . . .944 ? C123 H123b . . .948 ? C123 H123c . . .966 ? C124 H124a . . .957 ? C124 H124b . . .969 ? C124 H124c . . .943 ? C13 C14 . . 1.355(9) ? C13 H13 . . .950 ? C14 N15 . . 1.376(8) ? C14 H14 . . .941 ? N15 C151 . . 1.501(8) ? C151 C152 . . 1.511(9) ? C151 C153 . . 1.527(9) ? C151 C154 . . 1.549(9) ? C152 H152a . . .957 ? C152 H152b . . .952 ? C152 H152c . . .946 ? C153 H153a . . .960 ? C153 H153b . . .946 ? C153 H153c . . .941 ? C154 H154a . . .953 ? C154 H154b . . .941 ? C154 H154c . . .971 ? C1 N1 . . 1.098(10) ? C21 N22 . . 1.372(8) ? C21 N25 . . 1.363(8) ? N22 C221 . . 1.510(8) ? N22 C23 . . 1.392(8) ? C221 C222 . . 1.494(9) ? C221 C223 . . 1.539(9) ? C221 C224 . . 1.510(9) ? C222 H222a . . .963 ? C222 H222b . . .941 ? C222 H222c . . .953 ? C223 H223a . . .943 ? C223 H223b . . .962 ? C223 H223c . . .945 ? C224 H224a . . .931 ? C224 H224b . . .967 ? C224 H224c . . .964 ? C23 C24 . . 1.342(10) ? C23 H23 . . .945 ? C24 N25 . . 1.388(8) ? C24 H24 . . .958 ? N25 C251 . . 1.506(8) ? C251 C252 . . 1.525(10) ? C251 C253 . . 1.508(11) ? C251 C254 . . 1.534(11) ? C252 H252a . . .948 ? C252 H252b . . .950 ? C252 H252c . . .973 ? C253 H253a . . .951 ? C253 H253b . . .941 ? C253 H253c . . .952 ? C254 H254a . . .964 ? C254 H254b . . .956 ? C254 H254c . . .959 ? C2 N2 . . 1.085(9) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C11 Au1 C1 . . . 178.7(2) ? C21 Au2 C2 . . . 178.6(3) ? Au1 C11 N12 . . . 128.3(4) ? Au1 C11 N15 . . . 126.8(4) ? N12 C11 N15 . . . 104.9(5) ? C11 N12 C121 . . . 125.7(5) ? C11 N12 C13 . . . 110.4(5) ? C121 N12 C13 . . . 123.8(5) ? N12 C121 C122 . . . 110.6(5) ? N12 C121 C123 . . . 107.1(5) ? N12 C121 C124 . . . 110.0(5) ? C122 C121 C123 . . . 112.1(6) ? C122 C121 C124 . . . 108.9(6) ? C123 C121 C124 . . . 108.0(6) ? C121 C122 H122a . . . 109.3 ? C121 C122 H122b . . . 110.5 ? C121 C122 H122c . . . 109.7 ? H122a C122 H122b . . . 109.0 ? H122a C122 H122c . . . 108.8 ? H122b C122 H122c . . . 109.5 ? C121 C123 H123a . . . 110.3 ? C121 C123 H123b . . . 109.9 ? C121 C123 H123c . . . 109.5 ? H123a C123 H123b . . . 110.2 ? H123a C123 H123c . . . 108.7 ? H123b C123 H123c . . . 108.3 ? C121 C124 H124a . . . 110.5 ? C121 C124 H124b . . . 109.6 ? C121 C124 H124c . . . 111.2 ? H124a C124 H124b . . . 107.4 ? H124a C124 H124c . . . 109.5 ? H124b C124 H124c . . . 108.5 ? N12 C13 C14 . . . 107.0(5) ? N12 C13 H13 . . . 126.8 ? C14 C13 H13 . . . 126.2 ? C13 C14 N15 . . . 107.6(5) ? C13 C14 H14 . . . 127.0 ? N15 C14 H14 . . . 125.4 ? C11 N15 C14 . . . 110.0(5) ? C11 N15 C151 . . . 124.1(4) ? C14 N15 C151 . . . 126.0(5) ? N15 C151 C152 . . . 109.4(5) ? N15 C151 C153 . . . 109.2(5) ? N15 C151 C154 . . . 108.3(5) ? C152 C151 C153 . . . 111.4(5) ? C152 C151 C154 . . . 109.5(5) ? C153 C151 C154 . . . 109.0(5) ? C151 C152 H152a . . . 109.2 ? C151 C152 H152b . . . 110.0 ? C151 C152 H152c . . . 109.9 ? H152a C152 H152b . . . 108.7 ? H152a C152 H152c . . . 109.3 ? H152b C152 H152c . . . 109.7 ? C151 C153 H153a . . . 108.6 ? C151 C153 H153b . . . 109.2 ? C151 C153 H153c . . . 110.0 ? H153a C153 H153b . . . 109.0 ? H153a C153 H153c . . . 109.4 ? H153b C153 H153c . . . 110.6 ? C151 C154 H154a . . . 110.3 ? C151 C154 H154b . . . 111.3 ? C151 C154 H154c . . . 109.0 ? H154a C154 H154b . . . 110.0 ? H154a C154 H154c . . . 107.5 ? H154b C154 H154c . . . 108.5 ? Au1 C1 N1 . . . 177.9(6) ? Au2 C21 N22 . . . 127.7(4) ? Au2 C21 N25 . . . 127.1(4) ? N22 C21 N25 . . . 105.1(5) ? C21 N22 C221 . . . 125.6(5) ? C21 N22 C23 . . . 110.0(5) ? C221 N22 C23 . . . 124.3(5) ? N22 C221 C222 . . . 108.2(5) ? N22 C221 C223 . . . 108.3(5) ? N22 C221 C224 . . . 109.0(5) ? C222 C221 C223 . . . 111.6(5) ? C222 C221 C224 . . . 110.7(5) ? C223 C221 C224 . . . 109.1(5) ? C221 C222 H222a . . . 109.1 ? C221 C222 H222b . . . 110.6 ? C221 C222 H222c . . . 109.8 ? H222a C222 H222b . . . 109.1 ? H222a C222 H222c . . . 108.2 ? H222b C222 H222c . . . 110.0 ? C221 C223 H223a . . . 109.8 ? C221 C223 H223b . . . 108.7 ? C221 C223 H223c . . . 109.9 ? H223a C223 H223b . . . 109.0 ? H223a C223 H223c . . . 110.5 ? H223b C223 H223c . . . 108.9 ? C221 C224 H224a . . . 111.6 ? C221 C224 H224b . . . 109.2 ? C221 C224 H224c . . . 109.5 ? H224a C224 H224b . . . 109.6 ? H224a C224 H224c . . . 109.9 ? H224b C224 H224c . . . 107.0 ? N22 C23 C24 . . . 107.1(6) ? N22 C23 H23 . . . 126.5 ? C24 C23 H23 . . . 126.4 ? C23 C24 N25 . . . 107.6(6) ? C23 C24 H24 . . . 126.2 ? N25 C24 H24 . . . 126.2 ? C21 N25 C24 . . . 110.2(5) ? C21 N25 C251 . . . 124.6(5) ? C24 N25 C251 . . . 125.2(5) ? N25 C251 C252 . . . 109.6(5) ? N25 C251 C253 . . . 110.3(5) ? N25 C251 C254 . . . 108.4(5) ? C252 C251 C253 . . . 110.7(6) ? C252 C251 C254 . . . 107.6(6) ? C253 C251 C254 . . . 110.3(6) ? C251 C252 H252a . . . 110.5 ? C251 C252 H252b . . . 111.2 ? C251 C252 H252c . . . 110.1 ? H252a C252 H252b . . . 109.6 ? H252a C252 H252c . . . 107.7 ? H252b C252 H252c . . . 107.6 ? C251 C253 H253a . . . 108.7 ? C251 C253 H253b . . . 109.8 ? C251 C253 H253c . . . 108.9 ? H253a C253 H253b . . . 110.1 ? H253a C253 H253c . . . 109.2 ? H253b C253 H253c . . . 110.0 ? C251 C254 H254a . . . 110.9 ? C251 C254 H254b . . . 111.6 ? C251 C254 H254c . . . 110.7 ? H254a C254 H254b . . . 107.8 ? H254a C254 H254c . . . 107.6 ? H254b C254 H254c . . . 108.2 ? Au2 C2 N2 . . . 177.9(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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1536 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -28 _reflns_limit_l_max 27 _reflns_number_observed ? _reflns_d_resolution_high .625 _reflns_d_resolution_low 12.63 _diffrn_reflns_av_sigmaI/netI .091 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .076 _refine_ls_wR_factor_all .075 _refine_ls_goodness_of_fit_all .989 _refine_ls_shift/su_mean .0003 #===END