Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_compound_1 _database_code_CSD 173686 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Colacio,Enrique' 'Kivekas, Raikko' 'Lloret, F.' 'Ruiz, Jose' 'Suarez-Varela, Jose' 'Sundberg, Markku R.' _publ_requested_journal 'Chemical Communications' _publ_contact_author_name 'Prof ENRIQUE COLACIO' _publ_contact_author_address ; Inorganic Chemistry University og Granada Fuentenueva s/n Granada 18071 SPAIN ; _publ_contact_author_phone '+34 958 243236' _publ_contact_author_fax '+34 958 248526' _publ_contact_author_email 'ECOLACIO@UGR.ES' _publ_section_title ; Aurophilicity as cofactor in crystal engineering. Dicyanoaurate(I) anion as building block in a novel Co(II)-Au(I) bimetallic assembly ; _publ_contact_letter ; Please consider this CIF submission as crystallographic information file for compound AuCNCo. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C10 H14 Au2 Co N6 O2' _chemical_formula_sum 'C10 H14 Au2 Co N6 O2' _chemical_formula_weight 703.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.375(2) _cell_length_b 14.054(5) _cell_length_c 15.077(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.75(2) _cell_angle_gamma 90.00 _cell_volume 1772.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.70 _cell_measurement_theta_max 14.92 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 17.447 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_process_details 'North, Phillips & Mathews 1968' _exptl_absorpt_correction_T_min 0.0471 _exptl_absorpt_correction_T_max 0.0775 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method '\w--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 3418 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.24 _reflns_number_total 3189 _reflns_number_gt 2374 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_cell_refinement ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_data_reduction ; Texsan Process (Molecular Structure Corporation, 1993) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Electron density synthesis with coefficients Fo-Fc Highest peak 3.38 at 0.3923 0.2742 0.0309 [ 1.07 A from AU1 ] Deepest hole -2.81 at 0.4376 0.7354 0.0266 [ 0.87 A from AU2 ] ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+16.7265P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3189 _refine_ls_number_parameters 194 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1544 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.26521(6) 0.27359(4) 0.03455(3) 0.0213(2) Uani 1 d . . . Au2 Au 0.36851(6) 0.72842(4) -0.50153(3) 0.0210(2) Uani 1 d . . . Co Co 0.3137(2) 0.50010(12) -0.23327(10) 0.0131(4) Uani 1 d . . . O1 O 0.5539(12) 0.4683(8) -0.2040(7) 0.031(2) Uani 1 d . . . O2 O 0.0747(11) 0.5399(7) -0.2574(6) 0.023(2) Uani 1 d . . . N1 N 0.2624(15) 0.4148(9) -0.1246(8) 0.028(3) Uani 1 d . . . N2 N 0.3641(14) 0.5828(9) -0.3459(7) 0.023(3) Uani 1 d . . . N3 N 0.2858(15) 0.3821(8) -0.3170(7) 0.022(3) Uani 1 d . . . N4 N 0.3399(15) 0.6184(8) -0.1503(7) 0.021(3) Uani 1 d . . . N5 N 0.7746(15) 0.3838(10) -0.1699(8) 0.030(3) Uani 1 d U . . N6 N -0.1525(15) 0.5581(11) -0.3417(8) 0.031(3) Uani 1 d . . . C1 C 0.2610(16) 0.3655(11) -0.0635(9) 0.023(3) Uani 1 d U . . C2 C 0.3690(15) 0.6365(11) -0.4043(9) 0.020(3) Uani 1 d U . . C3 C 0.2700(15) 0.3222(10) -0.3705(8) 0.017(3) Uani 1 d U . . C4 C 0.3512(17) 0.6775(11) -0.0956(10) 0.026(3) Uani 1 d . . . C5 C 0.6416(19) 0.3966(12) -0.2149(11) 0.034(4) Uani 1 d . . . H5 H 0.6082 0.3503 -0.2578 0.041 Uiso 1 calc R . . C6 C 0.832(2) 0.4477(13) -0.0999(11) 0.036(4) Uani 1 d . . . H6A H 0.9230 0.4841 -0.1200 0.054 Uiso 1 calc R . . H6B H 0.8646 0.4107 -0.0471 0.054 Uiso 1 calc R . . H6C H 0.7458 0.4916 -0.0854 0.054 Uiso 1 calc R . . C7 C 0.880(2) 0.3053(12) -0.1936(12) 0.039(4) Uani 1 d . . . H7A H 0.8189 0.2586 -0.2295 0.058 Uiso 1 calc R . . H7B H 0.9241 0.2748 -0.1393 0.058 Uiso 1 calc R . . H7C H 0.9676 0.3302 -0.2277 0.058 Uiso 1 calc R . . C8 C -0.0130(16) 0.5185(11) -0.3218(9) 0.022(3) Uani 1 d . . . H8 H 0.0223 0.4700 -0.3601 0.027 Uiso 1 calc R . . C9 C -0.2149(19) 0.6359(12) -0.2895(11) 0.033(4) Uani 1 d . . . H9A H -0.3194 0.6180 -0.2681 0.049 Uiso 1 calc R . . H9B H -0.2265 0.6930 -0.3266 0.049 Uiso 1 calc R . . H9C H -0.1408 0.6491 -0.2387 0.049 Uiso 1 calc R . . C10 C -0.2473(19) 0.5216(14) -0.4161(11) 0.039(4) Uani 1 d . . . H10A H -0.1989 0.4629 -0.4373 0.058 Uiso 1 calc R . . H10B H -0.2520 0.5689 -0.4639 0.058 Uiso 1 calc R . . H10C H -0.3557 0.5082 -0.3978 0.058 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0344(4) 0.0144(3) 0.0147(3) 0.0078(2) -0.0020(2) -0.0009(2) Au2 0.0319(4) 0.0160(3) 0.0150(3) 0.0085(2) -0.0007(2) 0.0025(2) Co 0.0223(9) 0.0086(9) 0.0079(8) 0.0006(7) -0.0031(6) 0.0011(7) O1 0.024(5) 0.025(6) 0.044(7) 0.002(5) 0.000(5) 0.001(5) O2 0.025(5) 0.018(5) 0.024(5) 0.003(4) -0.008(4) -0.004(4) N1 0.042(8) 0.020(7) 0.020(6) -0.001(6) -0.001(5) -0.010(6) N2 0.030(7) 0.024(7) 0.016(6) 0.007(5) -0.006(5) 0.008(5) N3 0.041(7) 0.010(6) 0.016(6) 0.001(5) -0.001(5) 0.003(5) N4 0.039(7) 0.008(6) 0.017(6) -0.004(5) -0.003(5) 0.001(5) N5 0.027(6) 0.032(6) 0.030(6) 0.015(5) -0.009(5) -0.001(5) N6 0.030(7) 0.043(9) 0.020(6) -0.008(6) 0.000(5) -0.001(6) C1 0.020(6) 0.024(6) 0.025(6) -0.003(6) -0.009(5) -0.007(5) C2 0.016(6) 0.023(6) 0.021(6) 0.002(5) -0.007(5) 0.004(5) C3 0.020(4) 0.016(5) 0.014(4) -0.005(4) -0.001(4) 0.004(4) C4 0.026(8) 0.016(8) 0.037(9) 0.010(7) -0.004(6) -0.002(6) C5 0.039(10) 0.026(9) 0.038(9) 0.008(7) 0.006(7) 0.015(7) C6 0.041(10) 0.030(10) 0.036(9) -0.002(8) 0.002(7) 0.000(8) C7 0.046(11) 0.016(8) 0.054(11) 0.007(8) 0.003(9) 0.004(7) C8 0.020(7) 0.026(8) 0.021(7) -0.002(6) 0.002(6) -0.004(6) C9 0.032(8) 0.019(8) 0.049(10) 0.002(8) 0.010(7) 0.004(7) C10 0.028(9) 0.043(11) 0.043(10) -0.010(9) -0.008(7) -0.002(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C3 1.964(13) 4_566 ? Au1 C1 1.963(15) . ? Au1 Au2 3.1949(10) 2_644 ? Au2 C4 1.939(16) 4_575 ? Au2 C2 1.953(14) . ? Au2 Au1 3.1949(10) 2_654 ? Co N4 2.086(11) . ? Co O1 2.088(10) . ? Co N3 2.090(12) . ? Co N1 2.091(12) . ? Co O2 2.093(10) . ? Co N2 2.116(12) . ? O1 C5 1.263(19) . ? O2 C8 1.227(16) . ? N1 C1 1.152(19) . ? N2 C2 1.163(18) . ? N3 C3 1.170(17) . ? N4 C4 1.172(19) . ? N5 C5 1.29(2) . ? N5 C6 1.45(2) . ? N5 C7 1.47(2) . ? N6 C8 1.316(19) . ? N6 C10 1.44(2) . ? N6 C9 1.46(2) . ? C3 Au1 1.964(13) 4_565 ? C4 Au2 1.939(16) 4_576 ? C5 H5 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Au1 C1 177.9(6) 4_566 . ? C3 Au1 Au2 89.5(4) 4_566 2_644 ? C1 Au1 Au2 89.8(4) . 2_644 ? C4 Au2 C2 175.5(6) 4_575 . ? C4 Au2 Au1 77.8(4) 4_575 2_654 ? C2 Au2 Au1 106.3(4) . 2_654 ? N4 Co O1 88.3(5) . . ? N4 Co N3 179.5(4) . . ? O1 Co N3 92.1(5) . . ? N4 Co N1 90.4(5) . . ? O1 Co N1 86.8(5) . . ? N3 Co N1 89.8(5) . . ? N4 Co O2 87.9(4) . . ? O1 Co O2 176.3(4) . . ? N3 Co O2 91.7(4) . . ? N1 Co O2 93.4(4) . . ? N4 Co N2 91.4(5) . . ? O1 Co N2 93.4(4) . . ? N3 Co N2 88.4(5) . . ? N1 Co N2 178.2(5) . . ? O2 Co N2 86.5(4) . . ? C5 O1 Co 134.8(12) . . ? C8 O2 Co 127.1(10) . . ? C1 N1 Co 168.7(12) . . ? C2 N2 Co 168.6(11) . . ? C3 N3 Co 173.5(11) . . ? C4 N4 Co 172.0(11) . . ? C5 N5 C6 122.9(15) . . ? C5 N5 C7 119.5(15) . . ? C6 N5 C7 117.5(13) . . ? C8 N6 C10 118.6(14) . . ? C8 N6 C9 122.1(13) . . ? C10 N6 C9 119.3(14) . . ? N1 C1 Au1 175.5(14) . . ? N2 C2 Au2 177.7(12) . . ? N3 C3 Au1 173.8(12) . 4_565 ? N4 C4 Au2 177.8(13) . 4_576 ? O1 C5 N5 122.4(17) . . ? O1 C5 H5 118.8 . . ? N5 C5 H5 118.8 . . ? N5 C6 H6A 109.5 . . ? N5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N5 C7 H7A 109.5 . . ? N5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 C8 N6 124.6(14) . . ? O2 C8 H8 117.7 . . ? N6 C8 H8 117.7 . . ? N6 C9 H9A 109.5 . . ? N6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N6 C10 H10A 109.5 . . ? N6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 3.379 _refine_diff_density_min -2.811 _refine_diff_density_rms 0.392 #===END