# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/208 data_wtwong493-TCLau020 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Dec 14 17:05:15 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Marrearch Image Plate' _computing_cell_refinement 'Marrearch Image Plate' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 8.140(1) _cell_length_b 16.191(1) _cell_length_c 14.008(2) _cell_angle_alpha 90 _cell_angle_beta 105.90(2) _cell_angle_gamma 90 _cell_volume 1775.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.220 _exptl_crystal_density_diffrn 2.629 _exptl_crystal_density_meas ? _chemical_formula_weight 702.94 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H18 Au2 N8 Ni ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1280.00 _exptl_absorpt_coefficient_mu 17.597 _exptl_absorpt_correction_type 'Interimage Scaling' #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Image Plate' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 17070 _reflns_number_total 3149 _reflns_number_observed 1836 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.52 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Au 0 8 -2.013 8.802 'International Tables' Ni 0 4 0.339 1.112 'International Tables' N 0 32 0.006 0.003 'International Tables' C 0 40 0.003 0.002 'International Tables' H 0 72 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Au(1) 0.24764(9) 0.04008(5) 0.25063(6) 0.0400(2) Uij ? ? Au(2) 0.0000 0.0000 0.0000 0.0426(4) Uij ? ? Au(3) 0.0000 -0.5000 0.0000 0.0417(3) Uij ? ? Ni(1) 0.6558(2) -0.2115(1) 0.2722(1) 0.0297(6) Uij ? ? N(1) 0.634(1) -0.1956(10) 0.1209(9) 0.039(4) Uij ? ? N(2) 0.846(2) -0.303(1) 0.290(1) 0.052(5) Uij ? ? N(3) 0.708(2) -0.191(1) 0.4284(10) 0.048(5) Uij ? ? N(4) 0.860(2) -0.129(1) 0.2884(10) 0.040(4) Uij ? ? N(5) 0.474(2) -0.116(1) 0.2590(10) 0.042(5) Uij ? ? N(6) 0.473(2) -0.3019(9) 0.255(1) 0.045(5) Uij ? ? N(7) -0.293(2) 0.121(1) 0.012(1) 0.064(6) Uij ? ? N(8) -0.188(2) -0.350(1) 0.059(1) 0.076(7) Uij ? ? C(1) 0.758(2) -0.135(1) 0.106(1) 0.056(7) Uij ? ? C(2) 0.817(2) -0.079(1) 0.195(1) 0.053(6) Uij ? ? C(3) 1.025(2) -0.179(1) 0.300(1) 0.057(7) Uij ? ? C(4) 1.014(2) -0.263(1) 0.337(2) 0.059(7) Uij ? ? C(5) 0.867(2) -0.079(1) 0.378(1) 0.051(6) Uij ? ? C(6) 0.847(2) -0.132(1) 0.462(1) 0.045(6) Uij ? ? C(7) 0.386(2) -0.061(1) 0.253(1) 0.036(5) Uij ? ? C(8) 0.107(2) 0.141(1) 0.248(1) 0.039(5) Uij ? ? C(9) -0.186(2) 0.076(1) 0.007(1) 0.052(7) Uij ? ? C(10) -0.123(2) -0.404(1) 0.035(1) 0.051(7) Uij ? ? H(1) 0.8534 -0.1626 0.0947 0.0670 Uij ? ? H(2) 0.7053 -0.1019 0.0492 0.0670 Uij ? ? H(3) 0.7283 -0.0414 0.1959 0.0639 Uij ? ? H(4) 0.9152 -0.0499 0.1901 0.0639 Uij ? ? H(5) 1.0481 -0.1822 0.2372 0.0687 Uij ? ? H(6) 1.1162 -0.1507 0.3454 0.0687 Uij ? ? H(7) 1.0298 -0.2609 0.4068 0.0711 Uij ? ? H(8) 1.1024 -0.2958 0.3236 0.0711 Uij ? ? H(9) 0.9734 -0.0514 0.3984 0.0616 Uij ? ? H(10) 0.7769 -0.0396 0.3627 0.0616 Uij ? ? H(11) 0.8232 -0.0974 0.5113 0.0540 Uij ? ? H(12) 0.9503 -0.1610 0.4889 0.0540 Uij ? ? H(13) 0.6520 -0.2410 0.0966 0.0472 Uij ? ? H(14) 0.5347 -0.1793 0.0922 0.0472 Uij ? ? H(15) 0.8277 -0.3410 0.3258 0.0625 Uij ? ? H(16) 0.8461 -0.3220 0.2339 0.0625 Uij ? ? H(17) 0.6196 -0.1726 0.4410 0.0577 Uij ? ? H(18) 0.7357 -0.2361 0.4585 0.0577 Uij ? ? 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(1) 0.0366(4) 0.0337(4) 0.0498(4) 0.0065(3) 0.0119(3) -0.0021(4) Au(2) 0.0535(6) 0.0404(8) 0.0382(7) 0.0062(5) 0.0200(5) 0.0071(6) Au(3) 0.0492(6) 0.0428(8) 0.0386(7) 0.0075(5) 0.0211(5) 0.0068(6) Ni(1) 0.030(1) 0.032(1) 0.027(1) -0.0004(10) 0.0078(8) -0.001(1) N(1) 0.040(8) 0.05(1) 0.027(8) 0.003(7) 0.004(6) 0.001(7) N(2) 0.07(1) 0.05(1) 0.033(9) 0.013(9) 0.014(8) 0.007(8) N(3) 0.051(9) 0.07(1) 0.028(8) 0.015(8) 0.014(7) -0.002(8) N(4) 0.044(8) 0.04(1) 0.034(9) -0.007(7) 0.012(6) -0.009(8) N(5) 0.037(8) 0.05(1) 0.034(9) 0.012(8) 0.003(6) -0.002(8) N(6) 0.058(10) 0.027(9) 0.05(1) -0.011(8) 0.017(7) 0.005(8) N(7) 0.06(1) 0.07(1) 0.05(1) 0.02(1) -0.008(8) -0.02(1) N(8) 0.08(1) 0.10(2) 0.05(1) 0.03(1) 0.008(9) -0.02(1) C(1) 0.06(1) 0.09(2) 0.02(1) -0.03(1) 0.010(8) -0.01(1) C(2) 0.06(1) 0.04(1) 0.05(1) -0.02(1) 0.008(10) 0.01(1) C(3) 0.06(1) 0.08(2) 0.04(1) -0.02(1) 0.012(9) -0.01(1) C(4) 0.05(1) 0.08(2) 0.05(1) 0.00(1) 0.012(10) -0.01(1) C(5) 0.05(1) 0.04(1) 0.05(1) -0.008(10) 0.000(9) -0.02(1) C(6) 0.05(1) 0.06(1) 0.018(9) -0.011(10) 0.000(8) -0.002(9) C(7) 0.027(9) 0.05(1) 0.03(1) 0.014(8) 0.011(7) 0.001(9) C(8) 0.039(9) 0.03(1) 0.05(1) -0.002(8) 0.019(8) 0.002(9) C(9) 0.06(1) 0.06(2) 0.04(1) -0.01(1) 0.009(9) 0.01(1) C(10) 0.05(1) 0.07(2) 0.03(1) 0.02(1) 0.010(9) 0.01(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1836 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0569 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0666 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.315 _refine_ls_shift/esd_max 0.0140 _refine_ls_shift/esd_mean ? _refine_diff_density_min -4.20 _refine_diff_density_max 2.92 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;