Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm #============================================================================= # 1. SUBMISSION DETAILS _journal_coden_Cambridge 1350 _publ_contact_author_name 'Daniel B. Leznoff' _publ_contact_author_address ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; _publ_contact_author_phone 604-291-4887 _publ_contact_author_fax 604-291-3765 _publ_contact_author_email dleznoff@sfu.ca _publ_section_title ; Preparation and characterization of two chiral Au(CN)2-based coordination polymers containing (1R,2R)-N,N'-Dimethylcyclohexanediamine ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address A.R.Geisheimer ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; M.J.Katz ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; R.J.Batchelor ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; D.B.Leznoff ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; _publ_section_references ; Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. # CRYSTALS # Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. #ORTEP-3 version 1.073 # Farrugia, L.J., (1997) J. Appl. Cryst. 30, 565. # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # SHELXS 86 # Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. ; data_{Cu(C8H18N2)[Au(CN)2]2} _database_code_depnum_ccdc_archive 'CCDC 646319' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C12 H18 Au2 Cu1 N6' _chemical_formula_moiety 'C12 H18 Au2 Cu1 N6' _chemical_formula_weight 703.80 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z #------------------------------------------------ _cell_length_a 8.3621(4) _cell_length_b 11.0698(5) _cell_length_c 9.8203(5) _cell_angle_alpha 90 _cell_angle_beta 101.459(3) _cell_angle_gamma 90 _cell_volume 890.91(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5280 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 26.40 _cell_measurement_temperature 293 _exptl_crystal_description 'plate ' _exptl_crystal_colour Blue _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_max 0.3 _exptl_crystal_density_diffrn 2.623 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 638 _exptl_absorpt_coefficient_mu 17.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.06540 _exptl_absorpt_correction_T_max 0.24444 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area Detector' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w\f _diffrn_ambient_temperature 293 _diffrn_reflns_number 11576 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_min 2.116 _diffrn_reflns_theta_max 26.419 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.891 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_decay_% ? #========================================================================== # 8. REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 3555 _reflns_number_gt 2842 _reflns_threshold_expression I>2.5\s(I _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.0558 _refine_ls_number_reflns 2842 _refine_ls_number_restraints 1 _refine_ls_number_parameters 192 _refine_ls_goodness_of_fit_ref 0.9877 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.00P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_shift/su_max 0.000267 _refine_diff_density_max 2.48 _refine_diff_density_min -1.14 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 12 #_refine_ls_R_factor_ref 0.0434 #_reflns_number_all 3555 _refine_ls_R_factor_all 0.0536 _refine_ls_wR_factor_all 0.0600 # Number of reflections with Friedels Law is 1911 # Number of reflections without Friedels Law is 3555 # Theoretical number of reflections is about 1831 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method None _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_abs_structure_details 'Flack (1983), 1644 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad #========================================================== # 9. General computing _computing_data_collection ; Bruker SMART ; _computing_cell_refinement ; Bruker SMART ; _computing_data_reduction ; Bruker SAINT ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _computing_structure_refinement ; Crystals ; #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956 12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Au1 Au 0.97964(7) 0.2338(2) -0.79519(7) 0.0484 1.0000 Uani . . . . . . Au2 Au 0.00706(9) -0.0136(2) -0.97295(8) 0.0510 1.0000 Uani . . . . . . Cu1 Cu 0.43120(19) 0.2254(3) -1.1606(2) 0.0396 1.0000 Uani . . . . . . N1 N 0.6308(16) 0.2505(16) -0.9790(17) 0.0561 1.0000 Uani . . . . . . N2 N 1.3101(18) 0.222(2) -0.5847(19) 0.0737 1.0000 Uani . . . . . . N3 N 0.289(2) 0.1114(14) -1.0841(19) 0.0505 1.0000 Uani . . . . . . N4 N -0.280(2) -0.1461(15) -0.878(2) 0.0590 1.0000 Uani . . . . . . N5 N 0.5673(17) 0.0914(12) -1.2245(17) 0.0459 1.0000 Uani . . . . . . N6 N 0.5219(17) 0.3269(13) -1.2984(17) 0.0495 1.0000 Uani . . . . . . C1 C 0.7575(18) 0.2448(19) -0.9101(16) 0.0425 1.0000 Uani . . . . . . C2 C 1.196(2) 0.228(2) -0.6660(19) 0.0557 1.0000 Uani . . . . . . C3 C 0.190(3) 0.0648(17) -1.043(2) 0.0515 1.0000 Uani . . . . . . C4 C -0.179(2) -0.0930(19) -0.908(3) 0.0586 1.0000 Uani . . . . . . C5 C 0.6529(18) 0.1408(15) -1.3331(18) 0.0393 1.0000 Uani . . . . . . C6 C 0.808(3) 0.074(2) -1.343(3) 0.0735 1.0000 Uani . . . . . . C7 C 0.896(3) 0.129(2) -1.446(3) 0.0755 1.0000 Uani . . . . . . C8 C 0.919(3) 0.259(3) -1.419(3) 0.0920 1.0000 Uani . . . . . . C9 C 0.759(3) 0.326(2) -1.421(3) 0.0745 1.0000 Uani . . . . . . C10 C 0.681(2) 0.2706(15) -1.309(2) 0.0490 1.0000 Uani . . . . . . C11 C 0.474(3) -0.023(2) -1.269(3) 0.0971 1.0000 Uani . . . . . . C12 C 0.525(3) 0.4564(18) -1.278(3) 0.0731 1.0000 Uani . . . . . . H50 H 0.6484 0.0717 -1.1483 0.047(16) 1.0000 Uiso R . . . . . H51 H 0.5764 0.1320 -1.4248 0.039(16) 1.0000 Uiso R . . . . . H60 H 0.4534 0.3138 -1.3839 0.051(16) 1.0000 Uiso R . . . . . H61 H 0.7791 -0.0113 -1.3725 0.083(16) 1.0000 Uiso R . . . . . H62 H 0.8817 0.0735 -1.2494 0.083(16) 1.0000 Uiso R . . . . . H71 H 0.8312 0.1168 -1.5421 0.088(16) 1.0000 Uiso R . . . . . H72 H 1.0048 0.0891 -1.4374 0.088(16) 1.0000 Uiso R . . . . . H81 H 0.9734 0.2949 -1.4918 0.102(16) 1.0000 Uiso R . . . . . H82 H 0.9909 0.2706 -1.3255 0.102(16) 1.0000 Uiso R . . . . . H91 H 0.6861 0.3164 -1.5140 0.085(16) 1.0000 Uiso R . . . . . H92 H 0.7809 0.4139 -1.4014 0.085(16) 1.0000 Uiso R . . . . . H101 H 0.7577 0.2810 -1.2172 0.051(16) 1.0000 Uiso R . . . . . H111 H 0.4201 -0.0512 -1.1930 0.121(16) 1.0000 Uiso R . . . . . H112 H 0.5517 -0.0861 -1.2892 0.121(16) 1.0000 Uiso R . . . . . H113 H 0.3897 -0.0071 -1.3548 0.121(16) 1.0000 Uiso R . . . . . H121 H 0.4126 0.4850 -1.2722 0.083(16) 1.0000 Uiso R . . . . . H122 H 0.5610 0.4971 -1.3572 0.083(16) 1.0000 Uiso R . . . . . H123 H 0.6019 0.4765 -1.1892 0.083(16) 1.0000 Uiso 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 0.0370(3) 0.0534(3) 0.0522(4) -0.0053(3) 0.0029(3) -0.0007(4) Au2 0.0330(3) 0.0468(3) 0.0763(5) 0.0108(5) 0.0186(3) -0.0037(3) Cu1 0.0266(7) 0.0346(9) 0.0598(13) -0.0003(10) 0.0138(8) 0.0012(10) N1 0.035(7) 0.056(11) 0.077(12) -0.004(8) 0.011(7) -0.003(8) N2 0.049(8) 0.093(13) 0.069(11) 0.007(13) -0.012(8) 0.021(12) N3 0.046(10) 0.047(9) 0.064(11) 0.005(7) 0.025(8) -0.006(8) N4 0.038(9) 0.057(11) 0.086(14) 0.010(9) 0.023(9) 0.000(8) N5 0.035(7) 0.039(8) 0.066(11) 0.007(7) 0.014(7) 0.007(6) N6 0.044(8) 0.045(8) 0.059(11) -0.003(7) 0.009(7) -0.009(6) C1 0.043(8) 0.050(10) 0.032(9) -0.015(8) 0.001(7) -0.008(9) C2 0.056(10) 0.057(10) 0.056(12) -0.016(11) 0.016(9) 0.002(12) C3 0.047(11) 0.041(10) 0.075(14) -0.005(9) 0.034(10) -0.005(8) C4 0.035(10) 0.056(12) 0.093(17) 0.007(10) 0.033(11) 0.003(9) C5 0.022(7) 0.061(11) 0.035(10) -0.007(8) 0.006(6) 0.004(7) C6 0.055(13) 0.097(17) 0.074(17) 0.004(13) 0.026(11) 0.029(12) C7 0.046(12) 0.13(2) 0.065(16) -0.014(14) 0.033(11) -0.004(12) C8 0.047(12) 0.16(3) 0.071(17) -0.006(17) 0.017(11) -0.010(16) C9 0.076(16) 0.069(15) 0.087(19) 0.019(13) 0.037(14) -0.006(12) C10 0.030(8) 0.058(12) 0.061(13) 0.006(8) 0.015(8) -0.001(7) C11 0.10(2) 0.044(13) 0.17(3) -0.049(17) 0.082(18) -0.019(14) C12 0.067(14) 0.049(13) 0.107(19) 0.013(11) 0.027(12) 0.002(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Au1 . Au2 1_655 3.2799(13) yes Au1 . Au2 2_653 3.6219(13) yes Au1 . C1 . 1.976(15) yes Au1 . C2 . 1.995(18) yes Au2 . C3 . 1.996(19) yes Au2 . C4 . 2.00(2) yes Cu1 . N4 2_553 1.993(18) yes Cu1 . N1 . 2.205(15) yes Cu1 . N3 . 1.980(16) yes Cu1 . N5 . 2.043(14) yes Cu1 . N6 . 2.020(15) yes N1 . C1 . 1.14(2) yes N2 . C2 . 1.12(2) yes N3 . C3 . 1.12(2) yes N4 . C4 . 1.11(2) yes N5 . C5 . 1.50(2) yes N5 . C11 . 1.50(3) yes N5 . H50 . 0.930 no N6 . C10 . 1.49(2) yes N6 . C12 . 1.45(3) yes N6 . H60 . 0.930 no C5 . C6 . 1.52(2) yes C5 . C10 . 1.47(2) yes C5 . H51 . 1.000 no C6 . C7 . 1.49(3) yes C6 . H61 . 1.000 no C6 . H62 . 1.000 no C7 . C8 . 1.47(4) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C8 . C9 . 1.52(3) yes C8 . H81 . 1.000 no C8 . H82 . 1.000 no C9 . C10 . 1.52(3) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C10 . H101 . 1.000 no C11 . H111 . 1.000 no C11 . H112 . 1.000 no C11 . H113 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Au2 1_655 Au1 . Au2 2_653 107.21(2) yes Au2 1_655 Au1 . C1 . 84.5(5) yes Au2 2_653 Au1 . C1 . 74.7(6) yes Au2 1_655 Au1 . C2 . 99.2(6) yes Au2 2_653 Au1 . C2 . 106.8(7) yes C1 . Au1 . C2 . 175.2(7) yes Au1 1_455 Au2 . Au1 2_643 173.40(3) yes Au1 1_455 Au2 . C3 . 87.7(6) yes Au1 2_643 Au2 . C3 . 89.8(6) yes Au1 1_455 Au2 . C4 . 93.3(6) yes Au1 2_643 Au2 . C4 . 89.0(7) yes C3 . Au2 . C4 . 178.3(10) yes N4 2_553 Cu1 . N1 . 99.4(7) yes N4 2_553 Cu1 . N3 . 86.0(6) yes N1 . Cu1 . N3 . 100.9(7) yes N4 2_553 Cu1 . N5 . 172.7(7) yes N1 . Cu1 . N5 . 87.8(6) yes N3 . Cu1 . N5 . 93.8(6) yes N4 2_553 Cu1 . N6 . 94.0(7) yes N1 . Cu1 . N6 . 98.4(6) yes N3 . Cu1 . N6 . 160.4(7) yes N5 . Cu1 . N6 . 83.8(6) yes Cu1 . N1 . C1 . 159.7(16) yes Cu1 . N3 . C3 . 167.1(17) yes Cu1 2_543 N4 . C4 . 166.3(19) yes Cu1 . N5 . C5 . 109.1(10) yes Cu1 . N5 . C11 . 114.3(12) yes C5 . N5 . C11 . 113.0(16) yes Cu1 . N5 . H50 . 106.5 no C5 . N5 . H50 . 106.5 no C11 . N5 . H50 . 106.9 no Cu1 . N6 . C10 . 105.8(11) yes Cu1 . N6 . C12 . 117.0(14) yes C10 . N6 . C12 . 115.7(15) yes Cu1 . N6 . H60 . 105.8 no C10 . N6 . H60 . 105.8 no C12 . N6 . H60 . 105.7 no Au1 . C1 . N1 . 178.4(16) yes Au1 . C2 . N2 . 173.9(19) yes Au2 . C3 . N3 . 177.9(19) yes Au2 . C4 . N4 . 174(2) yes N5 . C5 . C6 . 113.7(15) yes N5 . C5 . C10 . 109.0(14) yes C6 . C5 . C10 . 112.1(16) yes N5 . C5 . H51 . 107.1 no C6 . C5 . H51 . 107.2 no C10 . C5 . H51 . 107.3 no C5 . C6 . C7 . 112.7(19) yes C5 . C6 . H61 . 108.5 no C7 . C6 . H61 . 108.3 no C5 . C6 . H62 . 108.7 no C7 . C6 . H62 . 109.2 no H61 . C6 . H62 . 109.5 no C6 . C7 . C8 . 110(2) yes C6 . C7 . H71 . 109.8 no C8 . C7 . H71 . 109.2 no C6 . C7 . H72 . 108.9 no C8 . C7 . H72 . 109.3 no H71 . C7 . H72 . 109.5 no C7 . C8 . C9 . 113(2) yes C7 . C8 . H81 . 108.6 no C9 . C8 . H81 . 108.8 no C7 . C8 . H82 . 108.7 no C9 . C8 . H82 . 108.4 no H81 . C8 . H82 . 109.5 no C8 . C9 . C10 . 107.3(20) yes C8 . C9 . H91 . 109.7 no C10 . C9 . H91 . 110.3 no C8 . C9 . H92 . 110.2 no C10 . C9 . H92 . 109.9 no H91 . C9 . H92 . 109.5 no C9 . C10 . N6 . 113.5(16) yes C9 . C10 . C5 . 110.9(17) yes N6 . C10 . C5 . 107.5(14) yes C9 . C10 . H101 . 108.4 no N6 . C10 . H101 . 108.1 no C5 . C10 . H101 . 108.2 no N5 . C11 . H111 . 109.3 no N5 . C11 . H112 . 109.2 no H111 . C11 . H112 . 109.5 no N5 . C11 . H113 . 109.9 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no N6 . C12 . H121 . 109.4 no N6 . C12 . H122 . 109.6 no H121 . C12 . H122 . 109.5 no N6 . C12 . H123 . 109.4 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no #=============================================================================== data_{Cu(C8H18N2)[Au(CN)2](ClO4)} _database_code_depnum_ccdc_archive 'CCDC 646320' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C10 H18 Au1 Cl1 Cu1 N4 O4' _chemical_formula_moiety 'C10 H18 Au1 Cl1 Cu1 N4 O4' _chemical_formula_weight 554.24 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21 ' 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 -x,y,-z+1/2 -x+1/2,y+1/2,-z+1/2 -x,-y,z+1/2 -x+1/2,-y+1/2,z+1/2 #------------------------------------------------ _cell_length_a 7.2413(2) _cell_length_b 17.2528(5) _cell_length_c 12.9833(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1622.04(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1210 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 24.56 _cell_measurement_temperature 293 _exptl_crystal_description 'needle ' _exptl_crystal_colour Blue _exptl_crystal_size_min 0.1 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_max 0.5 _exptl_crystal_density_diffrn 2.269 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 10.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.17016 _exptl_absorpt_correction_T_max 0.34895 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area Detector' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w\f _diffrn_ambient_temperature 293 _diffrn_reflns_number 4494 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_min 2.835 _diffrn_reflns_theta_max 28.376 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.808 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_decay_% ? #========================================================================== # 8. REFINEMENT DATA # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_number_total 2004 _reflns_number_gt 1207 _reflns_threshold_expression I>2.5\s(I _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0254 _refine_ls_number_reflns 1207 _refine_ls_number_parameters 99 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.7832 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.00P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_shift/su_max 0.000337 _refine_diff_density_max 0.59 _refine_diff_density_min -0.84 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 17 #_refine_ls_R_factor_ref 0.0278 #_reflns_number_all 2004 _refine_ls_R_factor_all 0.0554 _refine_ls_wR_factor_all 0.0333 # Number of reflections with Friedels Law is 1161 # Number of reflections without Friedels Law is 2004 # Theoretical number of reflections is about 1012 #--------------------------------------------------------- _chemical_name_systematic ; ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr # none if no extinction, _refine_ls_extinction_method None _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_abs_structure_details 'Flack (1983), 843 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad #========================================================== # 9. General computing _computing_data_collection ; Bruker SMART ; _computing_cell_refinement ; Bruker SMART ; _computing_data_reduction ; Bruker SAINT ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _computing_structure_refinement ; Crystals ; #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956 12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4' #============================================================================== # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Au1 Au 0.51150(8) 0.5000 0.5000 0.0468 1.0000 Uani S T . . . . Cu1 Cu 0.5000 0.72630(7) 0.7500 0.0333 1.0000 Uani S T . . . . Cl1 Cl 0.0000 0.77510(16) 0.7500 0.0431 1.0000 Uani S T . . . . O1 O 0.1541(7) 0.7279(3) 0.7236(6) 0.0714 1.0000 Uani . . . . . . O2 O 0.0476(11) 0.8232(4) 0.8350(4) 0.0716 1.0000 Uani . . . . . . N1 N 0.5096(15) 0.6446(3) 0.6439(4) 0.0461 1.0000 Uani . . . . . . N2 N 0.4769(10) 0.8126(3) 0.8541(4) 0.0337 1.0000 Uani . . . . . . C1 C 0.5098(16) 0.5917(4) 0.5902(5) 0.0465 1.0000 Uani . . . . . . C2 C 0.5342(10) 0.8863(3) 0.8054(4) 0.0302 1.0000 Uani . . . . . . C3 C 0.472(2) 0.9583(4) 0.8606(6) 0.0641 1.0000 Uani . . . . . . C4 C 0.529(3) 1.0312(4) 0.8050(7) 0.0848 1.0000 Uani . . . . . . C5 C 0.5606(13) 0.8012(5) 0.9558(5) 0.0648 1.0000 Uani . . . . . . H20 H 0.3509 0.8178 0.8662 0.041(9) 1.0000 Uiso R . . . . . H21 H 0.6723 0.8865 0.8034 0.040(9) 1.0000 Uiso R . . . . . H31 H 0.5295 0.9586 0.9307 0.079(9) 1.0000 Uiso R . . . . . H32 H 0.3345 0.9569 0.8676 0.079(9) 1.0000 Uiso R . . . . . H41 H 0.4677 1.0762 0.8397 0.109(9) 1.0000 Uiso R . . . . . H42 H 0.6661 1.0373 0.8096 0.109(9) 1.0000 Uiso R . . . . . H51 H 0.5165 0.7512 0.9858 0.081(9) 1.0000 Uiso R . . . . . H52 H 0.5251 0.8449 1.0023 0.081(9) 1.0000 Uiso R . . . . . H53 H 0.6981 0.7998 0.9484 0.081(9) 1.0000 Uiso 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 0.0591(3) 0.03280(18) 0.0485(2) -0.0157(3) 0.0000 0.0000 Cu1 0.0497(11) 0.0225(6) 0.0278(6) 0.0000 -0.0023(16) 0.0000 Cl1 0.031(2) 0.0448(17) 0.0530(17) 0.0000 0.001(3) 0.0000 O1 0.037(3) 0.056(4) 0.121(8) -0.022(4) 0.004(4) 0.017(3) O2 0.078(6) 0.083(5) 0.054(4) -0.028(3) 0.003(4) -0.002(5) N1 0.062(5) 0.030(3) 0.046(3) -0.013(3) 0.000(6) -0.005(6) N2 0.045(4) 0.030(3) 0.026(3) 0.000(2) 0.002(4) -0.001(4) C1 0.051(5) 0.038(4) 0.051(4) -0.007(3) -0.006(6) -0.002(6) C2 0.034(5) 0.023(3) 0.034(3) 0.000(3) -0.001(4) -0.004(3) C3 0.099(9) 0.044(5) 0.050(5) -0.014(4) -0.011(8) 0.009(7) C4 0.141(13) 0.026(4) 0.088(7) -0.006(4) -0.032(10) -0.013(7) C5 0.115(9) 0.054(5) 0.026(4) -0.001(4) -0.015(5) -0.006(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Au1 . C1 3_566 1.969(7) yes Au1 . C1 . 1.969(7) yes Cu1 . O1 5_656 2.528(5) yes Cu1 . N2 5_656 2.018(5) yes Cu1 . N1 5_656 1.973(5) yes Cu1 . O1 . 2.528(5) yes Cu1 . N1 . 1.973(5) yes Cu1 . N2 . 2.018(5) yes Cl1 . O1 5_556 1.424(5) yes Cl1 . O2 5_556 1.423(6) yes Cl1 . O1 . 1.424(5) yes Cl1 . O2 . 1.423(6) yes N1 . C1 . 1.147(7) yes N2 . C2 . 1.479(7) yes N2 . C5 . 1.466(8) yes N2 . H20 . 0.930 no C2 . C2 5_656 1.521(12) yes C2 . C3 . 1.504(10) yes C2 . H21 . 1.000 no C3 . C4 . 1.509(12) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . C4 5_656 1.489(18) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 3_566 Au1 . C1 . 179.3(7) yes O1 5_656 Cu1 . N2 5_656 90.0(3) yes O1 5_656 Cu1 . N1 5_656 87.0(3) yes N2 5_656 Cu1 . N1 5_656 176.5(3) yes O1 5_656 Cu1 . O1 . 178.8(3) yes N2 5_656 Cu1 . O1 . 89.1(3) yes N1 5_656 Cu1 . O1 . 93.9(4) yes O1 5_656 Cu1 . N1 . 93.9(4) yes N2 5_656 Cu1 . N1 . 93.3(2) yes N1 5_656 Cu1 . N1 . 88.7(3) yes O1 . Cu1 . N1 . 87.0(3) yes O1 5_656 Cu1 . N2 . 89.1(3) yes N2 5_656 Cu1 . N2 . 84.9(3) yes N1 5_656 Cu1 . N2 . 93.3(2) yes O1 . Cu1 . N2 . 90.0(3) yes N1 . Cu1 . N2 . 176.5(3) yes O1 5_556 Cl1 . O2 5_556 109.3(4) yes O1 5_556 Cl1 . O1 . 110.2(5) yes O2 5_556 Cl1 . O1 . 109.7(4) yes O1 5_556 Cl1 . O2 . 109.7(4) yes O2 5_556 Cl1 . O2 . 108.7(6) yes O1 . Cl1 . O2 . 109.3(4) yes Cu1 . O1 . Cl1 . 138.6(4) yes Cu1 . N1 . C1 . 172.8(6) yes Cu1 . N2 . C2 . 108.9(4) yes Cu1 . N2 . C5 . 118.0(5) yes C2 . N2 . C5 . 112.6(6) yes Cu1 . N2 . H20 . 105.4 no C2 . N2 . H20 . 105.4 no C5 . N2 . H20 . 105.4 no Au1 . C1 . N1 . 179.1(7) yes C2 5_656 C2 . N2 . 108.2(4) yes C2 5_656 C2 . C3 . 110.7(6) yes N2 . C2 . C3 . 115.0(6) yes C2 5_656 C2 . H21 . 107.5 no N2 . C2 . H21 . 107.2 no C3 . C2 . H21 . 107.9 no C2 . C3 . C4 . 112.3(9) yes C2 . C3 . H31 . 108.3 no C4 . C3 . H31 . 108.4 no C2 . C3 . H32 . 108.8 no C4 . C3 . H32 . 109.6 no H31 . C3 . H32 . 109.5 no C3 . C4 . C4 5_656 112.4(11) yes C3 . C4 . H41 . 108.0 no C4 5_656 C4 . H41 . 107.8 no C3 . C4 . H42 . 109.3 no C4 5_656 C4 . H42 . 109.7 no H41 . C4 . H42 . 109.5 no N2 . C5 . H51 . 109.5 no N2 . C5 . H52 . 109.7 no H51 . C5 . H52 . 109.5 no N2 . C5 . H53 . 109.2 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no