# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- DLeznoff DT-ART-09-2011-011741 Revised CIF.cif' #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Daniel B. Leznoff' _publ_contact_author_address ; Leznoff, Daniel B. Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; _publ_contact_author_phone +1-778-782-4887 _publ_contact_author_fax +1-778-782-3765 _publ_contact_author_email dleznoff@sfu.ca #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; INSERT TITLE ; # 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 J.S.Ovens ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; K.N.Truong ; 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 ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; ## -------------------REFERENCES ----------------------## _publ_section_references ; 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 #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 ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _exptl_absorpt_process_details ; Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_KAuCl2CN2 _database_code_depnum_ccdc_archive 'CCDC 844807' #TrackingRef '- DLeznoff DT-ART-09-2011-011741 Revised CIF.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C2 H2 Au1 Cl2 K1 N2 O1' _chemical_formula_moiety 'C2 H2 Au1 Cl2 K1 N2 O1' _chemical_formula_weight 377.02 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 #------------------------------------------------ _cell_length_a 17.345(10) _cell_length_b 7.712(4) _cell_length_c 6.126(3) _cell_angle_alpha 90 _cell_angle_beta 101.399(6) _cell_angle_gamma 90 _cell_volume 803.3(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2733 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.06 _cell_measurement_temperature 296(2) _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.23 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 3.100 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 19.420 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3624 _exptl_absorpt_correction_T_max 0.7457 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 4668 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_min 2.396 _diffrn_reflns_theta_max 28.409 _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 26.988 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 671 _refine_ls_number_restraints 0 _refine_ls_number_parameters 45 _oxford_refine_ls_R_factor_ref 0.0191 _refine_ls_wR_factor_ref 0.0269 _refine_ls_goodness_of_fit_ref 0.9723 # The values computed from all data _oxford_reflns_number_all 950 _refine_ls_R_factor_all 0.0304 _refine_ls_wR_factor_all 0.0330 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 678 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_gt 0.0270 _reflns_number_total 950 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_shift/su_max 0.0000774 _refine_diff_density_min -0.66 _refine_diff_density_max 0.70 _reflns_limit_h_min -22 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 10 _reflns_limit_l_min 0 _reflns_limit_l_max 8 _oxford_refine_ls_scale 0.0866(2) _oxford_diffrn_Wilson_B_factor 2.79 _oxford_diffrn_Wilson_scale 141.76 # Number of reflections with Friedels Law is 950 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 1005 #--------------------------------------------------------- _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 notdet # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment none # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 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' 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' 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' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 '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' 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' 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' #============================================================================== # 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 # TODO check _oxford_atom_site_special_shape 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 0.2500 0.7500 0.5000 0.0351 1.0000 Uani S . . . . . K1 K 0.5000 0.8164(4) 0.2500 0.0675 1.0000 Uani S T . . . . Cl1 Cl 0.31798(11) 0.6462(2) 0.2417(3) 0.0599 1.0000 Uani . . . . . . N1 N 0.4069(4) 0.8753(8) 0.7958(10) 0.0649 1.0000 Uani . . . . . . C1 C 0.3526(4) 0.8339(8) 0.6925(9) 0.0405 1.0000 Uani . . . . . . O1 O 0.0000 0.0000 0.0000 0.1907 1.0000 Uani S . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03313(19) 0.03411(18) 0.03595(18) 0.00083(13) 0.00153(12) -0.00277(13) K1 0.0584(15) 0.0481(11) 0.0836(17) 0.0000 -0.0160(12) 0.0000 Cl1 0.0555(10) 0.0647(11) 0.0613(10) -0.0101(8) 0.0158(8) -0.0038(8) N1 0.053(4) 0.071(4) 0.068(4) -0.005(3) 0.006(3) -0.011(3) C1 0.044(4) 0.039(4) 0.036(3) -0.002(3) 0.002(3) -0.003(3) O1 0.136(10) 0.132(9) 0.277(13) -0.112(11) -0.024(9) 0.016(8) 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 4_566 2.036(6) yes Au1 . Cl1 4_566 2.2963(18) yes Au1 . Cl1 . 2.2963(18) yes Au1 . C1 . 2.036(6) yes Cl1 . Cl1 4_565 3.760(4) yes Cl1 . Cl1 6_564 3.803(3) yes Cl1 . Cl1 6_565 3.803(3) yes K1 . N1 2_676 2.919(6) yes K1 . N1 6_574 2.919(6) yes K1 . N1 5_656 2.963(6) yes K1 . N1 1_554 2.963(6) yes K1 . Cl1 5_655 3.410(3) yes K1 . Cl1 . 3.410(3) yes N1 . C1 . 1.074(7) yes 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 4_566 Au1 . Cl1 4_566 90.06(17) yes C1 4_566 Au1 . Cl1 . 89.94(17) yes Cl1 4_566 Au1 . Cl1 . 179.995 yes C1 4_566 Au1 . C1 . 179.994 yes Cl1 4_566 Au1 . C1 . 89.94(17) yes Cl1 . Au1 . C1 . 90.06(17) yes Au1 . Cl1 . Cl1 4_565 93.82(8) yes Au1 . Cl1 . Cl1 6_564 147.51(6) yes Cl1 4_565 Cl1 . Cl1 6_564 73.62(5) yes Au1 . Cl1 . Cl1 6_565 64.53(4) yes Cl1 4_565 Cl1 . Cl1 6_565 141.91(6) yes Cl1 6_564 Cl1 . Cl1 6_565 107.30(10) yes N1 2_676 K1 . N1 6_574 70.9(2) yes N1 2_676 K1 . N1 5_656 75.88(16) yes N1 6_574 K1 . N1 5_656 89.65(19) yes N1 2_676 K1 . N1 1_554 89.65(19) yes N1 6_574 K1 . N1 1_554 75.88(16) yes N1 5_656 K1 . N1 1_554 162.3(3) yes N1 2_676 K1 . Cl1 5_655 77.69(14) yes N1 6_574 K1 . Cl1 5_655 147.18(14) yes N1 5_656 K1 . Cl1 5_655 73.38(13) yes N1 1_554 K1 . Cl1 5_655 113.84(12) yes N1 2_676 K1 . Cl1 . 147.18(14) yes N1 6_574 K1 . Cl1 . 77.69(14) yes N1 5_656 K1 . Cl1 . 113.84(12) yes N1 1_554 K1 . Cl1 . 73.38(13) yes Cl1 5_655 K1 . Cl1 . 134.72(12) yes Au1 . Cl1 . K1 . 117.09(8) yes K1 6_575 N1 . K1 5_656 90.35(19) yes K1 6_575 N1 . C1 . 128.6(6) yes K1 5_656 N1 . C1 . 139.4(5) yes Au1 . C1 . N1 . 178.7(6) yes data_KAuBr2CN2 _database_code_depnum_ccdc_archive 'CCDC 844808' #TrackingRef '- DLeznoff DT-ART-09-2011-011741 Revised CIF.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C2 H4 Au1 Br2 K1 N2 O2' _chemical_formula_moiety 'C2 H4 Au1 Br2 K1 N2 O2' _chemical_formula_weight 483.94 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 c 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z x,-y,z+1/2 x+1/2,-y+1/2,z+1/2 #------------------------------------------------ _cell_length_a 21.332(4) _cell_length_b 4.2229(9) _cell_length_c 13.474(3) _cell_angle_alpha 90 _cell_angle_beta 117.087(2) _cell_angle_gamma 90 _cell_volume 1080.7(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4034 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 28.07 _cell_measurement_temperature 150(2) _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.19 _exptl_crystal_density_diffrn 2.950 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 840.000 _exptl_absorpt_coefficient_mu 21.349 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3103 _exptl_absorpt_correction_T_max 0.7456 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _diffrn_reflns_number 1260 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_min 2.145 _diffrn_reflns_theta_max 28.106 _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 26.982 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 1060 _refine_ls_number_restraints 34 _refine_ls_number_parameters 102 _oxford_refine_ls_R_factor_ref 0.0467 _refine_ls_wR_factor_ref 0.0643 _refine_ls_goodness_of_fit_ref 1.1468 # The values computed from all data _oxford_reflns_number_all 1260 _refine_ls_R_factor_all 0.0563 _refine_ls_wR_factor_all 0.0813 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1087 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_gt 0.0655 _reflns_number_total 1260 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_shift/su_max 0.0001124 _refine_diff_density_min -1.55 _refine_diff_density_max 3.66 _reflns_limit_h_min -27 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 5 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_refine_ls_scale 0.0671(10) _oxford_diffrn_Wilson_B_factor 1.54 _oxford_diffrn_Wilson_scale 577.73 # Number of reflections with Friedels Law is 1260 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 1318 #--------------------------------------------------------- _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 notdet # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment none # none if no extinction, _refine_ls_extinction_method None # twinning data loop_ _oxford_twin_element_scale_factors 0.86(3) 0.14(3) _refine_special_details ; Twin law: 0.978 0.000 1.485 0.000 -1.000 0.000 0.029 0.000 -0.978 (obtained through rotax analysis in Crystals software) ; #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 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' 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' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 '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' 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' 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' #============================================================================== # 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 # TODO check _oxford_atom_site_special_shape 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 0.56294(18) 0.7514(4) 0.4922(3) 0.0194 1.0000 Uani D U . . . . Br1 Br 0.5726(3) 1.0820(8) 0.6468(5) 0.0384 1.0000 Uani . . . . . . Br2 Br 0.5555(3) 0.4152(9) 0.3405(5) 0.0307 1.0000 Uani . . . . . . K1 K 0.2863(11) 0.312(6) 0.275(2) 0.0507 0.45(3) Uani . . P . 1 . K2 K 0.3439(6) 0.305(4) 0.2166(10) 0.0239 0.55(3) Uani . . P . 2 . O1 O 0.2364(12) 0.275(5) -0.105(2) 0.0467 1.0000 Uani . . . . . . O2 O 0.394(2) -0.094(8) 0.112(3) 0.0950 1.0000 Uani . . . . . . N1 N 0.7279(7) 0.648(7) 0.599(2) 0.0341 1.0000 Uani D U . . . . N2 N 0.3964(7) 0.758(5) 0.373(2) 0.0379 1.0000 Uani D U . . . . C1 C 0.6667(5) 0.708(7) 0.560(3) 0.0269 1.0000 Uani D U . . . . C2 C 0.4587(5) 0.770(7) 0.417(3) 0.0316 1.0000 Uani D U . . . . 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 0.0250(4) 0.0178(3) 0.0183(3) 0.00060(19) 0.0124(3) 0.0009(2) Br1 0.079(4) 0.0123(14) 0.034(2) 0.0006(15) 0.034(3) 0.0150(13) Br2 0.050(2) 0.031(2) 0.0160(14) -0.0022(15) 0.0196(18) -0.0130(13) K1 0.042(12) 0.023(9) 0.073(17) 0.010(11) 0.014(12) -0.016(9) K2 0.025(7) 0.036(7) 0.015(6) 0.001(5) 0.013(5) -0.003(6) O1 0.039(11) 0.053(14) 0.058(14) 0.013(10) 0.029(11) 0.002(9) O2 0.19(3) 0.057(15) 0.090(18) -0.013(17) 0.11(2) -0.05(2) N1 0.032(7) 0.044(9) 0.028(9) 0.007(9) 0.014(7) 0.013(7) N2 0.037(8) 0.033(10) 0.033(10) -0.006(7) 0.006(8) 0.005(7) C1 0.030(5) 0.038(7) 0.019(7) 0.005(6) 0.017(6) 0.008(6) C2 0.033(6) 0.030(7) 0.027(8) 0.004(6) 0.010(6) -0.001(6) 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 . Br1 . 2.438(5) yes Au1 . Br2 . 2.434(5) yes Au1 . C1 . 1.982(9) yes Au1 . C2 . 1.981(9) yes Br1 . Br2 3_565 3.494(5) yes Br1 . Br2 3_575 3.508(4) yes K1 . N1 4_454 2.88(4) yes K1 . N1 4_464 3.11(4) yes K1 . N2 1_545 3.15(3) yes K1 . N2 . 2.82(3) yes K2 . N1 4_454 2.95(2) yes K2 . N2 1_545 2.98(3) yes K2 . N1 4_464 3.22(3) yes K2 . N2 . 2.69(3) yes N1 . C1 . 1.190(9) yes N2 . C2 . 1.185(9) yes 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 Br1 . Au1 . Br2 . 178.8(3) yes Br1 . Au1 . C1 . 91.1(9) yes Br2 . Au1 . C1 . 87.9(10) yes Br1 . Au1 . C2 . 93.0(12) yes Br2 . Au1 . C2 . 88.0(12) yes C1 . Au1 . C2 . 175.8(18) yes Au1 . Br1 . Br2 3_565 107.29(16) yes Au1 . Br1 . Br2 3_575 170.11(16) yes Br2 3_565 Br1 . Br2 3_575 74.17(4) yes Au1 . Br2 . Br1 3_564 171.26(15) yes Au1 . Br2 . Br1 3_574 106.40(17) yes Br1 3_564 Br2 . Br1 3_574 74.17(4) yes N1 4_454 K1 . N1 4_464 89.6(10) yes N1 4_454 K1 . N2 1_545 78.7(9) yes N1 4_464 K1 . N2 1_545 145.9(13) yes N1 4_454 K1 . N2 . 142.5(13) yes N1 4_464 K1 . N2 . 80.1(8) yes N2 1_545 K1 . N2 . 89.8(7) yes N1 4_454 K2 . N2 1_545 80.3(8) yes N1 4_454 K2 . N1 4_464 86.1(5) yes N2 1_545 K2 . N1 4_464 149.3(8) yes N1 4_454 K2 . N2 . 146.2(10) yes N2 1_545 K2 . N2 . 96.2(10) yes N1 4_464 K2 . N2 . 80.1(6) yes K1 4_555 N1 . K1 4_565 89.6(10) yes K1 4_555 N1 . C1 . 119(2) yes K1 4_565 N1 . C1 . 99(2) yes K1 . N2 . K1 1_565 89.8(7) yes K1 . N2 . C2 . 140.0(20) yes K1 1_565 N2 . C2 . 129.2(20) yes N1 . C1 . Au1 . 173(3) yes N2 . C2 . Au1 . 175(2) yes data_KAuI2CN2 _database_code_depnum_ccdc_archive 'CCDC 844809' #TrackingRef '- DLeznoff DT-ART-09-2011-011741 Revised CIF.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C3 H1 Au1.5 I3 K1.5 N3 O0.5' _chemical_formula_moiety 'C3 H1 Au1.5 I3 K1.5 N3 O0.5' _chemical_formula_weight 821.87 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 #------------------------------------------------ _cell_length_a 4.3182(3) _cell_length_b 24.4306(18) _cell_length_c 13.312(1) _cell_angle_alpha 90 _cell_angle_beta 90.850(1) _cell_angle_gamma 90 _cell_volume 1404.21(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5611 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.38 _cell_measurement_temperature 296(2) _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.42 _exptl_crystal_density_diffrn 3.883 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 22.682 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4019 _exptl_absorpt_correction_T_max 0.7457 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 16403 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_theta_min 1.667 _diffrn_reflns_theta_max 28.464 _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.041 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2253 _refine_ls_number_restraints 0 _refine_ls_number_parameters 124 _oxford_refine_ls_R_factor_ref 0.0344 _refine_ls_wR_factor_ref 0.0448 _refine_ls_goodness_of_fit_ref 0.9847 # The values computed from all data _oxford_reflns_number_all 3363 _refine_ls_R_factor_all 0.0622 _refine_ls_wR_factor_all 0.0566 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2375 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_gt 0.0460 _reflns_number_total 3363 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.03P)^2^ + 0.00P] ,where P=(max(Fo,0) + 2Fc)/3 ; _refine_ls_shift/su_max 0.0003845 _refine_diff_density_min -1.14 _refine_diff_density_max 1.57 _reflns_limit_h_min -5 _reflns_limit_h_max 5 _reflns_limit_k_min 0 _reflns_limit_k_max 32 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_refine_ls_scale 0.06050(12) _oxford_diffrn_Wilson_B_factor 2.99 _oxford_diffrn_Wilson_scale 311.38 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 3363 # Theoretical number of reflections is about 7087 #--------------------------------------------------------- _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 notdet # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment none # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 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' 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' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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' 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' 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' #============================================================================== # 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 # TODO check _oxford_atom_site_special_shape 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 0.0000 0.5000 0.5000 0.0378 1.0000 Uani S . . . . . Au2 Au 0.13223(10) 0.211800(19) 0.43425(3) 0.0360 1.0000 Uani . . . . . . I1 I -0.3161(2) 0.40867(4) 0.52465(7) 0.0500 1.0000 Uani . . . . . . I2 I -0.1586(2) 0.15877(4) 0.28847(7) 0.0528 1.0000 Uani . . . . . . I3 I 0.4599(2) 0.26053(4) 0.57622(6) 0.0450 1.0000 Uani . . . . . . K1 K 0.021(2) 0.5082(3) 0.0536(6) 0.0803 0.5000 Uani . . . . . . K2 K -0.3947(7) 0.38164(15) 0.2328(3) 0.0618 1.0000 Uani . . . . . . O1 O 0.511(7) 0.5291(8) 0.1150(16) 0.0960 0.5000 Uani . . . . . . N1 N 0.072(4) 0.4708(6) 0.2736(10) 0.0841 1.0000 Uani . . . . . . N2 N 0.110(3) 0.3193(5) 0.3104(9) 0.0608 1.0000 Uani . . . . . . N3 N 0.129(3) 0.1056(5) 0.5659(10) 0.0724 1.0000 Uani . . . . . . C1 C 0.047(3) 0.4820(6) 0.3581(11) 0.0559 1.0000 Uani . . . . . . C2 C 0.124(3) 0.2805(5) 0.3519(10) 0.0420 1.0000 Uani . . . . . . C3 C 0.133(3) 0.1440(5) 0.5164(10) 0.0464 1.0000 Uani . . . . . . 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 0.0438(4) 0.0332(4) 0.0362(4) 0.0000(3) -0.0019(3) -0.0032(3) Au2 0.0404(3) 0.0337(3) 0.0339(3) 0.00273(19) -0.00162(18) -0.0030(2) I1 0.0514(5) 0.0404(5) 0.0580(6) 0.0078(4) -0.0037(4) -0.0099(4) I2 0.0558(5) 0.0591(6) 0.0431(5) -0.0003(4) -0.0135(4) -0.0111(4) I3 0.0462(5) 0.0444(5) 0.0443(5) -0.0048(4) -0.0031(4) -0.0090(4) K1 0.092(5) 0.059(4) 0.090(5) 0.026(4) 0.016(5) 0.027(4) K2 0.0543(19) 0.069(2) 0.061(2) 0.0069(17) -0.0086(15) -0.0045(16) O1 0.21(3) 0.028(10) 0.047(13) 0.000(9) 0.049(16) -0.006(14) N1 0.144(15) 0.065(9) 0.043(8) 0.002(7) -0.001(8) -0.025(9) N2 0.085(9) 0.046(7) 0.052(7) 0.012(6) 0.002(6) 0.011(6) N3 0.113(12) 0.043(7) 0.060(8) 0.002(7) -0.006(8) -0.005(7) C1 0.063(9) 0.064(9) 0.041(8) 0.005(7) 0.001(7) -0.014(8) C2 0.044(7) 0.034(7) 0.049(8) 0.004(6) 0.006(6) 0.000(5) C3 0.060(8) 0.039(7) 0.039(7) 0.004(6) -0.011(6) -0.006(6) 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 2_566 1.953(15) yes Au1 . I1 2_566 2.6387(8) yes Au1 . I1 2_466 3.7118(9) yes Au1 . I1 1_655 3.7118(9) yes Au1 . I1 . 2.6387(8) yes Au1 . C1 . 1.953(15) yes Au2 . I3 1_455 3.6852(10) yes Au2 . I2 . 2.6361(10) yes Au2 . I3 . 2.6291(9) yes Au2 . C2 . 2.005(13) yes Au2 . C3 . 1.985(13) yes I1 . I3 1_455 3.8111(12) yes I1 . I2 4_555 3.9296(12) yes I1 . K2 . 3.951(4) yes I3 . K2 4_655 4.094(4) yes I2 . I3 4_454 3.8009(12) yes K1 . O1 1_455 2.41(3) yes K1 . N3 4_554 2.824(15) yes K1 . N3 3_555 2.929(14) yes K1 . K1 2_565 1.490(18) yes K1 . O1 . 2.31(3) yes K1 . N1 . 3.074(15) yes K2 . N2 1_455 2.834(13) yes K2 . N3 4_454 3.021(14) yes K2 . N3 4_554 3.209(15) yes K2 . N1 1_455 3.223(17) yes K2 . N1 . 3.012(15) yes K2 . N2 . 2.840(13) yes N1 . C1 . 1.163(17) yes N2 . C2 . 1.098(15) yes N3 . C3 . 1.146(16) yes 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 2_566 Au1 . I1 2_566 89.5(4) yes C1 2_566 Au1 . I1 2_466 81.8(4) yes I1 2_566 Au1 . I1 2_466 83.86(2) yes C1 2_566 Au1 . I1 1_655 98.2(4) yes I1 2_566 Au1 . I1 1_655 96.14(2) yes I1 2_466 Au1 . I1 1_655 179.997 yes C1 2_566 Au1 . I1 . 90.5(4) yes I1 2_566 Au1 . I1 . 179.996 yes I1 2_466 Au1 . I1 . 96.14(2) yes I1 1_655 Au1 . I1 . 83.86(2) yes C1 2_566 Au1 . C1 . 179.994 yes I1 2_566 Au1 . C1 . 90.5(4) yes I1 2_466 Au1 . C1 . 98.2(4) yes I1 1_655 Au1 . C1 . 81.8(4) yes I1 . Au1 . C1 . 89.5(4) yes I3 1_455 Au2 . I2 . 99.56(3) yes I3 1_455 Au2 . I3 . 84.53(3) yes I2 . Au2 . I3 . 175.69(3) yes I3 1_455 Au2 . C2 . 90.1(3) yes I2 . Au2 . C2 . 90.3(4) yes I3 . Au2 . C2 . 91.1(4) yes I3 1_455 Au2 . C3 . 88.9(4) yes I2 . Au2 . C3 . 89.6(4) yes I3 . Au2 . C3 . 89.2(4) yes C2 . Au2 . C3 . 179.0(5) yes Au1 . I1 . Au1 1_455 83.86(2) yes Au1 . I1 . I3 1_455 163.43(4) yes Au1 1_455 I1 . I3 1_455 112.53(3) yes Au1 . I1 . I2 4_555 112.49(3) yes Au1 1_455 I1 . I2 4_555 117.26(3) yes I3 1_455 I1 . I2 4_555 58.79(2) yes Au1 . I1 . K2 . 93.22(6) yes Au1 1_455 I1 . K2 . 87.54(5) yes I3 1_455 I1 . K2 . 90.01(6) yes I2 4_555 I1 . K2 . 145.09(6) yes Au2 . I2 . I3 4_454 119.26(3) yes Au2 . I2 . I1 4_554 159.77(4) yes I3 4_454 I2 . I1 4_554 59.05(2) yes Au2 . I3 . Au2 1_655 84.53(2) yes Au2 . I3 . I2 4_655 172.75(4) yes Au2 1_655 I3 . I2 4_655 102.28(3) yes Au2 . I3 . I1 1_655 115.84(3) yes Au2 1_655 I3 . I1 1_655 90.60(3) yes I2 4_655 I3 . I1 1_655 62.16(2) yes O1 1_455 K1 . N3 4_554 109.8(6) yes O1 1_455 K1 . N3 3_555 79.5(6) yes N3 4_554 K1 . N3 3_555 150.0(4) yes O1 1_455 K1 . K1 2_565 106.4(10) yes N3 4_554 K1 . K1 2_565 78.9(6) yes N3 3_555 K1 . K1 2_565 71.1(6) yes O1 1_455 K1 . O1 . 131.9(10) yes N3 4_554 K1 . O1 . 92.7(6) yes N3 3_555 K1 . O1 . 102.0(6) yes K1 2_565 K1 . O1 . 119.7(9) yes O1 1_455 K1 . N1 . 78.0(7) yes N3 4_554 K1 . N1 . 69.0(4) yes N3 3_555 K1 . N1 . 140.5(5) yes K1 2_565 K1 . N1 . 146.9(7) yes O1 . K1 . N1 . 71.1(6) yes N2 1_455 K2 . N3 4_454 79.3(4) yes N2 1_455 K2 . N3 4_554 148.0(4) yes N3 4_454 K2 . N3 4_554 87.7(3) yes N2 1_455 K2 . N1 1_455 75.9(4) yes N3 4_454 K2 . N1 1_455 64.8(4) yes N3 4_554 K2 . N1 1_455 124.3(3) yes N2 1_455 K2 . I1 . 77.6(3) yes N3 4_454 K2 . I1 . 138.9(3) yes N3 4_554 K2 . I1 . 127.8(3) yes N1 1_455 K2 . I1 . 76.8(3) yes N2 1_455 K2 . N1 . 146.1(4) yes N3 4_454 K2 . N1 . 120.3(4) yes N3 4_554 K2 . N1 . 65.1(4) yes N1 1_455 K2 . N1 . 87.6(4) yes I1 . K2 . N1 . 69.8(3) yes N2 1_455 K2 . N2 . 99.1(4) yes N3 4_454 K2 . N2 . 146.4(4) yes N3 4_554 K2 . N2 . 76.1(3) yes N1 1_455 K2 . N2 . 148.0(4) yes I1 . K2 . N2 . 71.2(3) yes N1 . K2 . N2 . 79.3(4) yes K1 . O1 . K1 1_655 131.9(10) yes K2 . N1 . K1 . 90.3(4) yes K2 . N1 . K2 1_655 87.6(4) yes K1 . N1 . K2 1_655 94.7(4) yes K2 . N1 . C1 . 105.8(11) yes K1 . N1 . C1 . 147.7(13) yes K2 1_655 N1 . C1 . 113.5(13) yes K2 1_655 N2 . K2 . 99.1(4) yes K2 1_655 N2 . C2 . 127.6(11) yes K2 . N2 . C2 . 133.0(11) yes K1 4_555 N3 . K1 3_545 30.0(4) yes K1 4_555 N3 . K2 4_655 104.7(5) yes K1 3_545 N3 . K2 4_655 128.7(5) yes K1 4_555 N3 . K2 4_555 91.1(4) yes K1 3_545 N3 . K2 4_555 107.6(5) yes K2 4_655 N3 . K2 4_555 87.7(3) yes K1 4_555 N3 . C3 . 140.9(11) yes K1 3_545 N3 . C3 . 111.0(10) yes K2 4_655 N3 . C3 . 108.8(10) yes K2 4_555 N3 . C3 . 109.5(11) yes N1 . C1 . Au1 . 179.2(13) yes Au2 . C2 . N2 . 176.4(12) yes Au2 . C3 . N3 . 178.2(13) yes data_KAu1Au3Br _database_code_depnum_ccdc_archive 'CCDC 844810' #TrackingRef '- DLeznoff DT-ART-09-2011-011741 Revised CIF.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C6 H2 Au3 Br2 K3 N6 O1' _chemical_formula_moiety 'C6 H2 Au3 Br2 K3 N6 O1' _chemical_formula_weight 1042.12 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 8.1153(16) _cell_length_b 10.1791(16) _cell_length_c 12.875(3) _cell_angle_alpha 70.416(2) _cell_angle_beta 88.834(2) _cell_angle_gamma 70.991(1) _cell_volume 942.7(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5232 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.11 _cell_measurement_temperature 296(2) _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 3.664 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 28.190 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4323 _exptl_absorpt_correction_T_max 0.7457 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 10973 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_theta_min 1.687 _diffrn_reflns_theta_max 28.422 _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.580 _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 -17 _diffrn_reflns_limit_l_max 16 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2960 _refine_ls_number_restraints 0 _refine_ls_number_parameters 190 _oxford_refine_ls_R_factor_ref 0.0328 _refine_ls_wR_factor_ref 0.0436 _refine_ls_goodness_of_fit_ref 1.0811 # The values computed from all data _oxford_reflns_number_all 4332 _refine_ls_R_factor_all 0.0540 _refine_ls_wR_factor_all 0.0644 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3055 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_gt 0.0442 _reflns_number_total 4332 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_shift/su_max 0.0013129 _refine_diff_density_min -1.16 _refine_diff_density_max 1.59 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -12 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_refine_ls_scale 0.05353(10) _oxford_diffrn_Wilson_B_factor 3.20 _oxford_diffrn_Wilson_scale 501.89 # Number of reflections with Friedels Law is 4332 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4728 #--------------------------------------------------------- _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 notdet # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment none # none if no extinction, _refine_ls_extinction_method None #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 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' 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' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 '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' 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' 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' #============================================================================== # 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 # TODO check _oxford_atom_site_special_shape 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 0.76416(5) 0.96243(5) 0.50449(3) 0.0372 1.0000 Uani . . . . . . Au2 Au 0.58133(6) 0.59123(4) 0.89290(4) 0.0442 1.0000 Uani . . . . . . Au3 Au 0.91117(6) 0.40614(5) 1.10745(4) 0.0470 1.0000 Uani . . . . . . Br1 Br 0.83876(16) 1.12939(13) 0.33934(9) 0.0497 1.0000 Uani . . . . . . Br2 Br 0.68650(17) 0.79550(14) 0.66703(10) 0.0552 1.0000 Uani . . . . . . K1 K 1.0865(3) 0.1125(3) 0.8393(2) 0.0486 1.0000 Uani . . . . . . K2 K 0.5896(3) 0.1040(3) 0.8441(2) 0.0466 1.0000 Uani . . . . . . K3 K 0.7137(4) 0.5013(3) 0.5737(2) 0.0608 1.0000 Uani . . . . . . O1 O 0.6379(11) 0.4654(9) 0.3840(6) 0.0636 1.0000 Uani . . . . . . N11 N 0.6023(18) 1.2156(14) 0.6005(10) 0.0803 1.0000 Uani . . . . . . N12 N 0.9316(16) 0.7006(13) 0.4167(11) 0.0748 1.0000 Uani . . . . . . N21 N 0.4175(13) 0.8956(11) 0.9273(8) 0.0500 1.0000 Uani . . . . . . N22 N 0.7498(13) 0.3249(11) 0.8114(9) 0.0524 1.0000 Uani . . . . . . N31 N 0.7425(13) 0.6816(11) 1.1791(9) 0.0556 1.0000 Uani . . . . . . N32 N 1.0779(13) 0.1062(11) 1.0701(8) 0.0498 1.0000 Uani . . . . . . C11 C 0.6596(16) 1.1245(13) 0.5651(10) 0.0526 1.0000 Uani . . . . . . C12 C 0.8685(18) 0.7961(15) 0.4485(11) 0.0558 1.0000 Uani . . . . . . C21 C 0.4771(16) 0.7834(13) 0.9182(9) 0.0466 1.0000 Uani . . . . . . C22 C 0.6890(15) 0.4181(12) 0.8471(10) 0.0459 1.0000 Uani . . . . . . C31 C 0.8089(15) 0.5824(12) 1.1480(10) 0.0501 1.0000 Uani . . . . . . C32 C 1.0179(15) 0.2200(12) 1.0804(9) 0.0443 1.0000 Uani . . . . . . 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 0.0381(2) 0.0423(3) 0.0320(2) -0.01280(18) 0.00830(18) -0.01512(18) Au2 0.0601(3) 0.0334(2) 0.0379(3) -0.01237(19) 0.0117(2) -0.0147(2) Au3 0.0588(3) 0.0369(3) 0.0438(3) -0.0151(2) 0.0110(2) -0.0134(2) Br1 0.0558(7) 0.0533(7) 0.0370(7) -0.0092(5) 0.0134(6) -0.0218(6) Br2 0.0664(9) 0.0608(8) 0.0410(7) -0.0109(6) 0.0142(6) -0.0324(7) K1 0.0429(14) 0.0456(15) 0.0542(16) -0.0139(12) 0.0084(12) -0.0149(11) K2 0.0421(14) 0.0495(15) 0.0473(15) -0.0141(11) 0.0105(12) -0.0175(11) K3 0.0619(19) 0.0610(18) 0.0586(19) -0.0217(14) 0.0126(15) -0.0191(14) O1 0.080(6) 0.052(5) 0.042(5) -0.008(4) 0.015(5) -0.010(5) N11 0.118(11) 0.068(8) 0.056(8) -0.030(7) 0.039(8) -0.025(8) N12 0.073(8) 0.072(8) 0.091(10) -0.043(8) 0.030(7) -0.025(7) N21 0.051(6) 0.052(6) 0.049(6) -0.019(5) 0.011(5) -0.018(5) N22 0.050(6) 0.046(6) 0.071(8) -0.029(5) 0.013(5) -0.021(5) N31 0.058(7) 0.044(6) 0.068(8) -0.020(5) 0.014(6) -0.020(5) N32 0.055(6) 0.047(6) 0.045(6) -0.011(5) 0.014(5) -0.019(5) C11 0.057(8) 0.047(7) 0.048(7) -0.011(6) 0.022(6) -0.018(6) C12 0.063(8) 0.059(8) 0.058(9) -0.030(7) 0.014(7) -0.028(7) C21 0.055(7) 0.044(7) 0.043(7) -0.018(5) 0.017(6) -0.015(5) C22 0.053(7) 0.028(6) 0.053(7) -0.010(5) 0.003(6) -0.013(5) C31 0.054(7) 0.035(6) 0.063(8) -0.014(6) 0.022(6) -0.021(5) C32 0.053(7) 0.037(6) 0.038(7) -0.012(5) 0.014(5) -0.010(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 . Br1 . 2.4436(13) yes Au1 . Br2 . 2.4340(14) yes Au1 . C11 . 1.993(12) yes Au1 . C12 . 1.991(12) yes Au2 . Au2 2_667 3.2883(10) yes Au2 . Au3 . 3.4456(9) yes Au2 . Br2 . 3.2420(13) yes Au2 . C21 . 1.997(11) yes Au2 . C22 . 1.973(11) yes Au3 . Au3 2_767 3.3873(10) yes Au3 . C31 . 1.955(11) yes Au3 . C32 . 1.955(11) yes K1 . N31 2_767 2.815(10) yes K1 . N21 1_645 2.821(10) yes K1 . N32 2_757 2.868(10) yes K1 . N12 2_766 3.184(13) yes K1 . N22 . 2.818(10) yes K1 . N32 . 2.951(10) yes K2 . N32 2_757 2.803(10) yes K2 . N31 2_667 2.807(10) yes K2 . N21 1_545 2.818(10) yes K2 . N21 2_667 2.944(10) yes K2 . N11 1_545 2.968(12) yes K2 . N22 . 2.859(10) yes K3 . N12 2_766 2.918(12) yes K3 . N11 1_545 3.228(13) yes K3 . N11 2_676 3.316(13) yes K3 . N12 . 3.282(12) yes K3 . N22 . 2.946(11) yes N11 . C11 . 1.132(15) yes N12 . C12 . 1.144(15) yes N21 . C21 . 1.131(14) yes N22 . C22 . 1.154(13) yes N31 . C31 . 1.174(14) yes N32 . C32 . 1.153(14) yes 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 Br1 . Au1 . Br2 . 179.04(5) yes Br1 . Au1 . C11 . 92.3(3) yes Br2 . Au1 . C11 . 88.1(3) yes Br1 . Au1 . C12 . 89.4(4) yes Br2 . Au1 . C12 . 90.2(4) yes C11 . Au1 . C12 . 178.2(5) yes Au2 2_667 Au2 . Au3 . 72.59(2) yes Au2 2_667 Au2 . Br2 . 172.14(3) yes Au3 . Au2 . Br2 . 115.03(3) yes Au2 2_667 Au2 . C21 . 93.5(3) yes Au3 . Au2 . C21 . 100.5(3) yes Br2 . Au2 . C21 . 83.4(3) yes Au2 2_667 Au2 . C22 . 94.2(3) yes Au3 . Au2 . C22 . 84.0(3) yes Br2 . Au2 . C22 . 88.7(3) yes C21 . Au2 . C22 . 172.0(4) yes Au3 2_767 Au3 . Au2 . 74.31(2) yes Au3 2_767 Au3 . C31 . 91.3(3) yes Au2 . Au3 . C31 . 83.4(4) yes Au3 2_767 Au3 . C32 . 92.4(3) yes Au2 . Au3 . C32 . 100.6(3) yes C31 . Au3 . C32 . 175.1(5) yes Au1 . Br2 . Au2 . 175.60(5) yes N31 2_767 K1 . N21 1_645 85.2(3) yes N31 2_767 K1 . N32 2_757 161.9(3) yes N21 1_645 K1 . N32 2_757 90.1(3) yes N31 2_767 K1 . N12 2_766 72.0(3) yes N21 1_645 K1 . N12 2_766 113.5(3) yes N32 2_757 K1 . N12 2_766 125.6(3) yes N31 2_767 K1 . N22 . 93.5(3) yes N21 1_645 K1 . N22 . 164.5(3) yes N32 2_757 K1 . N22 . 86.4(3) yes N12 2_766 K1 . N22 . 80.6(3) yes N31 2_767 K1 . N32 . 81.9(3) yes N21 1_645 K1 . N32 . 81.3(3) yes N32 2_757 K1 . N32 . 80.1(3) yes N12 2_766 K1 . N32 . 148.2(3) yes N22 . K1 . N32 . 83.2(3) yes N32 2_757 K2 . N31 2_667 163.2(3) yes N32 2_757 K2 . N21 1_545 93.4(3) yes N31 2_667 K2 . N21 1_545 85.4(3) yes N32 2_757 K2 . N21 2_667 81.8(3) yes N31 2_667 K2 . N21 2_667 81.4(3) yes N21 1_545 K2 . N21 2_667 82.5(3) yes N32 2_757 K2 . N11 1_545 105.3(3) yes N31 2_667 K2 . N11 1_545 90.1(3) yes N21 1_545 K2 . N11 1_545 116.8(4) yes N21 2_667 K2 . N11 1_545 158.4(3) yes N32 2_757 K2 . N22 . 86.8(3) yes N31 2_667 K2 . N22 . 90.3(3) yes N21 1_545 K2 . N22 . 165.8(3) yes N21 2_667 K2 . N22 . 83.5(3) yes N11 1_545 K2 . N22 . 76.6(3) yes N12 2_766 K3 . N11 1_545 84.2(3) yes N12 2_766 K3 . N11 2_676 142.1(3) yes N11 1_545 K3 . N11 2_676 104.7(3) yes N12 2_766 K3 . N12 . 73.3(4) yes N11 1_545 K3 . N12 . 140.8(3) yes N11 2_676 K3 . N12 . 77.5(3) yes N12 2_766 K3 . N22 . 83.1(3) yes N11 1_545 K3 . N22 . 71.5(3) yes N11 2_676 K3 . N22 . 134.8(3) yes N12 . K3 . N22 . 134.3(3) yes K2 1_565 N11 . K3 1_565 100.0(3) yes K2 1_565 N11 . K3 2_676 123.8(4) yes K3 1_565 N11 . K3 2_676 75.3(3) yes K2 1_565 N11 . C11 . 113.5(10) yes K3 1_565 N11 . C11 . 129.1(11) yes K3 2_676 N11 . C11 . 111.4(11) yes K3 2_766 N12 . K1 2_766 94.3(3) yes K3 2_766 N12 . K3 . 106.7(4) yes K1 2_766 N12 . K3 . 136.8(4) yes K3 2_766 N12 . C12 . 135.7(11) yes K1 2_766 N12 . C12 . 99.0(11) yes K3 . N12 . C12 . 91.7(10) yes K2 1_565 N21 . K1 1_465 92.0(3) yes K2 1_565 N21 . K2 2_667 97.5(3) yes K1 1_465 N21 . K2 2_667 98.3(3) yes K2 1_565 N21 . C21 . 117.9(9) yes K1 1_465 N21 . C21 . 128.8(9) yes K2 2_667 N21 . C21 . 115.9(9) yes K1 . N22 . K2 . 91.3(3) yes K1 . N22 . K3 . 101.9(3) yes K2 . N22 . K3 . 109.8(3) yes K1 . N22 . C22 . 133.5(9) yes K2 . N22 . C22 . 118.3(9) yes K3 . N22 . C22 . 100.3(8) yes K2 2_667 N31 . K1 2_767 92.4(3) yes K2 2_667 N31 . C31 . 137.8(10) yes K1 2_767 N31 . C31 . 118.5(9) yes K2 2_757 N32 . K1 2_757 91.4(3) yes K2 2_757 N32 . K1 . 98.6(3) yes K1 2_757 N32 . K1 . 99.9(3) yes K2 2_757 N32 . C32 . 127.3(9) yes K1 2_757 N32 . C32 . 118.7(8) yes K1 . N32 . C32 . 115.4(8) yes Au1 . C11 . N11 . 179.0(13) yes Au1 . C12 . N12 . 178.6(13) yes Au2 . C21 . N21 . 176.7(11) yes N22 . C22 . Au2 . 174.3(11) yes N31 . C31 . Au3 . 174.8(10) yes N32 . C32 . Au3 . 176.1(10) yes data_KAu1Au3I _database_code_depnum_ccdc_archive 'CCDC 844811' #TrackingRef '- DLeznoff DT-ART-09-2011-011741 Revised CIF.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C10 H4 Au5 I2 K5 N10 O2' _chemical_formula_moiety 'C10 H4 Au5 I2 K5 N10 O2' _chemical_formula_weight 1730.34 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------ _cell_length_a 7.3196(6) _cell_length_b 9.8319(8) _cell_length_c 11.5992(9) _cell_angle_alpha 99.936(1) _cell_angle_beta 92.457(1) _cell_angle_gamma 111.249(1) _cell_volume 761.26(11) _cell_formula_units_Z 1 _cell_measurement_reflns_used 5741 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.44 _cell_measurement_temperature 296(2) _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_max 0.45 _exptl_crystal_density_diffrn 3.765 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 26.743 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2560 _exptl_absorpt_correction_T_max 0.7457 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 8751 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_theta_min 2.269 _diffrn_reflns_theta_max 28.474 _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 25.912 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 #========================================================================== # 8. REFINEMENT DATA # The values actually used during refinement # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2746 _refine_ls_number_restraints 0 _refine_ls_number_parameters 161 _oxford_refine_ls_R_factor_ref 0.0391 _refine_ls_wR_factor_ref 0.0549 _refine_ls_goodness_of_fit_ref 1.1557 # The values computed from all data _oxford_reflns_number_all 3540 _refine_ls_R_factor_all 0.0503 _refine_ls_wR_factor_all 0.0675 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2806 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_gt 0.0556 _reflns_number_total 3540 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_shift/su_max 0.0002106 _refine_diff_density_min -2.40 _refine_diff_density_max 1.84 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min -12 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_refine_ls_scale 0.0871(3) _oxford_diffrn_Wilson_B_factor 2.85 _oxford_diffrn_Wilson_scale 164.81 # Number of reflections with Friedels Law is 3540 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3850 #--------------------------------------------------------- _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 notdet # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment none # none if no extinction, _refine_ls_extinction_coef 18.7(14) _refine_ls_extinction_method 'Larson (1970), Equation 22' #========================================================== # 9. General computing _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_structure_solution ; SIR92 (Altomare et al, 1994) CRYSTALS (Watkin, 1988) ; #=================================================================== # 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' 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' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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' 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' 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' #============================================================================== # 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 # TODO check _oxford_atom_site_special_shape 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 0.0000 0.0000 0.0000 0.0326 1.0000 Uani S . . . . . Au2 Au -0.26072(6) 0.01867(5) 0.25268(4) 0.0407 1.0000 Uani . . . . . . Au3 Au -0.5000 0.0000 0.5000 0.0417 1.0000 Uani S . . . . . Au4 Au 0.0000 0.0000 0.5000 0.0446 1.0000 Uani S . . . . . I1 I 0.27989(14) -0.00093(10) 0.14812(10) 0.0680 1.0000 Uani . . . . . . K1 K 0.0000 0.5000 0.5000 0.0432 1.0000 Uani S . . . . . K2 K -0.0085(4) 0.5855(3) 0.1561(3) 0.0483 1.0000 Uani . . . . . . K3 K 0.4536(4) 0.4548(3) 0.3043(3) 0.0483 1.0000 Uani . . . . . . O1 O 0.6994(15) 0.3605(11) -0.0005(10) 0.0724 1.0000 Uani . . . . . . N11 N 0.1475(16) 0.3453(11) 0.0954(10) 0.0499 1.0000 Uani . . . . . . N21 N -0.3293(17) -0.3192(12) 0.1903(11) 0.0549 1.0000 Uani . . . . . . N22 N -0.2238(15) 0.3487(11) 0.2863(10) 0.0504 1.0000 Uani . . . . . . N31 N -0.2631(14) 0.3280(11) 0.6342(9) 0.0443 1.0000 Uani . . . . . . N41 N -0.2494(15) -0.3300(11) 0.5116(11) 0.0522 1.0000 Uani . . . . . . C11 C 0.0893(17) 0.2191(13) 0.0594(11) 0.0410 1.0000 Uani . . . . . . C21 C -0.3010(17) -0.1926(13) 0.2162(11) 0.0433 1.0000 Uani . . . . . . C22 C -0.2306(16) 0.2300(13) 0.2773(12) 0.0439 1.0000 Uani . . . . . . C31 C -0.3452(17) 0.2114(13) 0.5860(12) 0.0428 1.0000 Uani . . . . . . C41 C -0.1573(17) -0.2070(12) 0.5081(11) 0.0459 1.0000 Uani . . . . . . 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 0.0309(3) 0.0233(3) 0.0406(3) 0.0044(2) -0.0021(2) 0.0081(2) Au2 0.0404(3) 0.0315(2) 0.0479(3) 0.00695(19) 0.0016(2) 0.01173(19) Au3 0.0443(4) 0.0256(3) 0.0471(4) 0.0030(3) 0.0058(3) 0.0057(3) Au4 0.0468(4) 0.0274(3) 0.0540(5) 0.0096(3) -0.0025(3) 0.0078(3) I1 0.0629(6) 0.0441(5) 0.0875(8) 0.0035(5) -0.0369(5) 0.0184(4) K1 0.0379(18) 0.045(2) 0.043(2) 0.0096(16) 0.0016(15) 0.0113(15) K2 0.0537(15) 0.0432(14) 0.0491(16) 0.0053(12) 0.0015(12) 0.0216(12) K3 0.0446(14) 0.0442(14) 0.0571(17) 0.0141(13) 0.0070(12) 0.0160(12) O1 0.069(6) 0.063(6) 0.074(7) 0.009(6) -0.021(6) 0.017(5) N11 0.059(6) 0.028(5) 0.054(7) -0.003(5) 0.002(5) 0.013(5) N21 0.063(7) 0.039(6) 0.066(8) 0.022(5) 0.019(6) 0.018(5) N22 0.046(6) 0.038(6) 0.059(7) 0.003(5) -0.006(5) 0.010(5) N31 0.045(5) 0.032(5) 0.043(6) -0.003(4) 0.003(5) 0.004(4) N41 0.040(5) 0.035(5) 0.070(8) 0.013(5) -0.003(5) 0.001(4) C11 0.041(6) 0.039(6) 0.045(7) 0.009(5) 0.003(5) 0.017(5) C21 0.041(6) 0.041(6) 0.047(7) 0.014(5) 0.004(5) 0.012(5) C22 0.034(6) 0.034(6) 0.052(8) 0.001(5) -0.009(5) 0.003(5) C31 0.035(6) 0.036(6) 0.059(8) 0.010(6) 0.007(5) 0.015(5) C41 0.047(7) 0.031(6) 0.052(8) -0.003(5) -0.012(6) 0.013(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 . C11 2_555 1.993(12) yes Au1 . Au2 2_555 3.5796(5) yes Au1 . I1 2_555 2.6204(8) yes Au1 . Au2 . 3.5796(5) yes Au1 . I1 . 2.6204(8) yes Au1 . C11 . 1.993(12) yes Au2 . I1 1_455 3.4518(10) yes Au2 . Au3 . 3.4220(5) yes Au2 . Au4 . 3.4454(5) yes Au2 . C21 . 1.955(12) yes Au2 . C22 . 1.976(12) yes Au3 . C31 2_456 2.020(12) yes Au3 . Au4 1_455 3.6598(3) yes Au3 . Au4 . 3.6598(3) yes Au3 . C31 . 2.020(12) yes Au4 . C41 2_556 1.963(12) yes Au4 . C41 . 1.963(12) yes K1 . N22 2_566 2.767(11) yes K1 . N31 2_566 2.792(10) yes K1 . N41 1_565 2.881(11) yes K1 . N41 2_556 2.881(11) yes K1 . N22 . 2.767(11) yes K1 . N31 . 2.792(10) yes K2 . N21 1_565 2.845(12) yes K2 . N31 2_566 2.871(11) yes K2 . N11 2_565 3.307(12) yes K2 . N11 . 2.971(10) yes K2 . N22 . 2.990(11) yes K3 . N21 1_665 2.801(10) yes K3 . N41 2_556 2.855(12) yes K3 . N22 1_655 2.908(10) yes K3 . N31 2_566 2.955(10) yes K3 . N41 1_665 3.074(11) yes K3 . N11 . 2.990(11) yes N11 . C11 . 1.148(14) yes N21 . C21 . 1.166(15) yes N22 . C22 . 1.137(14) yes N31 . C31 . 1.113(14) yes N41 . C41 . 1.160(14) yes 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 C11 2_555 Au1 . Au2 2_555 78.1(3) yes C11 2_555 Au1 . I1 2_555 88.3(3) yes Au2 2_555 Au1 . I1 2_555 85.02(3) yes C11 2_555 Au1 . Au2 . 101.9(3) yes Au2 2_555 Au1 . Au2 . 179.997 yes I1 2_555 Au1 . Au2 . 94.98(3) yes C11 2_555 Au1 . I1 . 91.7(3) yes Au2 2_555 Au1 . I1 . 94.98(3) yes I1 2_555 Au1 . I1 . 179.996 yes Au2 . Au1 . I1 . 85.02(3) yes C11 2_555 Au1 . C11 . 179.994 yes Au2 2_555 Au1 . C11 . 101.9(3) yes I1 2_555 Au1 . C11 . 91.7(3) yes Au2 . Au1 . C11 . 78.1(3) yes I1 . Au1 . C11 . 88.3(3) yes I1 1_455 Au2 . Au1 . 105.86(2) yes I1 1_455 Au2 . Au3 . 77.89(2) yes Au1 . Au2 . Au3 . 173.184(14) yes I1 1_455 Au2 . Au4 . 142.08(2) yes Au1 . Au2 . Au4 . 111.276(13) yes Au3 . Au2 . Au4 . 64.405(10) yes I1 1_455 Au2 . C21 . 100.0(3) yes Au1 . Au2 . C21 . 78.4(4) yes Au3 . Au2 . C21 . 95.5(4) yes Au4 . Au2 . C21 . 80.5(4) yes I1 1_455 Au2 . C22 . 76.8(3) yes Au1 . Au2 . C22 . 99.4(4) yes Au3 . Au2 . C22 . 87.0(4) yes Au4 . Au2 . C22 . 103.9(4) yes C21 . Au2 . C22 . 175.6(5) yes Au2 . Au3 . Au2 2_456 179.997 yes Au2 . Au3 . C31 2_456 83.1(3) yes Au2 2_456 Au3 . C31 2_456 96.9(3) yes Au2 . Au3 . Au4 1_455 121.892(9) yes Au2 2_456 Au3 . Au4 1_455 58.108(9) yes C31 2_456 Au3 . Au4 1_455 80.4(3) yes Au2 . Au3 . Au4 . 58.108(9) yes Au2 2_456 Au3 . Au4 . 121.892(9) yes C31 2_456 Au3 . Au4 . 99.6(3) yes Au4 1_455 Au3 . Au4 . 179.997 yes Au2 . Au3 . C31 . 96.9(3) yes Au2 2_456 Au3 . C31 . 83.1(3) yes C31 2_456 Au3 . C31 . 179.994 yes Au4 1_455 Au3 . C31 . 99.6(3) yes Au4 . Au3 . C31 . 80.4(3) yes Au2 2_556 Au4 . Au2 . 179.997 yes Au2 2_556 Au4 . C41 2_556 97.8(3) yes Au2 . Au4 . C41 2_556 82.2(3) yes Au2 2_556 Au4 . Au3 1_655 57.487(9) yes Au2 . Au4 . Au3 1_655 122.513(9) yes C41 2_556 Au4 . Au3 1_655 77.7(3) yes Au2 2_556 Au4 . Au3 . 122.513(9) yes Au2 . Au4 . Au3 . 57.487(9) yes C41 2_556 Au4 . Au3 . 102.3(3) yes Au3 1_655 Au4 . Au3 . 179.997 yes Au2 2_556 Au4 . C41 . 82.2(3) yes Au2 . Au4 . C41 . 97.8(3) yes C41 2_556 Au4 . C41 . 179.994 yes Au3 1_655 Au4 . C41 . 102.3(3) yes Au3 . Au4 . C41 . 77.7(3) yes Au2 1_655 I1 . Au1 . 158.74(5) yes N22 2_566 K1 . N31 2_566 94.8(3) yes N22 2_566 K1 . N41 1_565 95.4(3) yes N31 2_566 K1 . N41 1_565 94.8(3) yes N22 2_566 K1 . N41 2_556 84.6(3) yes N31 2_566 K1 . N41 2_556 85.2(3) yes N41 1_565 K1 . N41 2_556 179.996 yes N22 2_566 K1 . N22 . 179.996 yes N31 2_566 K1 . N22 . 85.2(3) yes N41 1_565 K1 . N22 . 84.6(3) yes N41 2_556 K1 . N22 . 95.4(3) yes N22 2_566 K1 . N31 . 85.2(3) yes N31 2_566 K1 . N31 . 179.996 yes N41 1_565 K1 . N31 . 85.2(3) yes N41 2_556 K1 . N31 . 94.8(3) yes N22 . K1 . N31 . 94.8(3) yes N21 1_565 K2 . N31 2_566 112.3(3) yes N21 1_565 K2 . N11 2_565 71.8(3) yes N31 2_566 K2 . N11 2_565 150.0(3) yes N21 1_565 K2 . N11 . 150.9(3) yes N31 2_566 K2 . N11 . 83.7(3) yes N11 2_565 K2 . N11 . 106.9(3) yes N21 1_565 K2 . N22 . 84.8(3) yes N31 2_566 K2 . N22 . 79.8(3) yes N11 2_565 K2 . N22 . 129.8(3) yes N11 . K2 . N22 . 73.9(3) yes N21 1_665 K3 . N41 2_556 156.7(3) yes N21 1_665 K3 . N22 1_655 87.2(3) yes N41 2_556 K3 . N22 1_655 104.7(3) yes N21 1_665 K3 . N31 2_566 79.1(3) yes N41 2_556 K3 . N31 2_566 82.8(3) yes N22 1_655 K3 . N31 2_566 156.9(3) yes N21 1_665 K3 . N41 1_665 79.8(3) yes N41 2_556 K3 . N41 1_665 82.9(3) yes N22 1_655 K3 . N41 1_665 78.9(3) yes N31 2_566 K3 . N41 1_665 80.4(3) yes N21 1_665 K3 . N11 . 87.3(3) yes N41 2_556 K3 . N11 . 104.6(3) yes N22 1_655 K3 . N11 . 116.2(3) yes N31 2_566 K3 . N11 . 82.0(3) yes N41 1_665 K3 . N11 . 159.8(3) yes K2 . N11 . K3 . 95.5(3) yes K2 . N11 . K2 2_565 73.1(3) yes K3 . N11 . K2 2_565 145.3(4) yes K2 . N11 . C11 . 139.0(9) yes K3 . N11 . C11 . 114.9(9) yes K2 2_565 N11 . C11 . 92.9(9) yes K3 1_445 N21 . K2 1_545 96.6(3) yes K3 1_445 N21 . C21 . 127.2(10) yes K2 1_545 N21 . C21 . 120.4(9) yes K1 . N22 . K3 1_455 100.1(3) yes K1 . N22 . K2 . 94.2(3) yes K3 1_455 N22 . K2 . 91.3(3) yes K1 . N22 . C22 . 105.1(9) yes K3 1_455 N22 . C22 . 128.4(9) yes K2 . N22 . C22 . 130.1(10) yes K1 . N31 . K2 2_566 96.3(3) yes K1 . N31 . K3 2_566 94.2(3) yes K2 2_566 N31 . K3 2_566 98.4(3) yes K1 . N31 . C31 . 112.7(9) yes K2 2_566 N31 . C31 . 125.2(10) yes K3 2_566 N31 . C31 . 123.0(9) yes K3 2_556 N41 . K1 2_556 94.5(3) yes K3 2_556 N41 . K3 1_445 97.1(3) yes K1 2_556 N41 . K3 1_445 93.8(3) yes K3 2_556 N41 . C41 . 130.3(10) yes K1 2_556 N41 . C41 . 110.2(9) yes K3 1_445 N41 . C41 . 122.3(9) yes Au1 . C11 . N11 . 177.4(11) yes N21 . C21 . Au2 . 177.4(12) yes Au2 . C22 . N22 . 175.5(10) yes Au3 . C31 . N31 . 178.7(10) yes N41 . C41 . Au4 . 179.2(12) yes