Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global #============================================================================== # (Publishing Staff Use Only) _journal_coden_Cambridge 222 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Murray Baker' _publ_contact_author_address ; Department of Chemistry University of Western Australia School of Biomedical and Chemical S Crawley WA 6009 AUSTRALIA ; _publ_contact_author_email MVB@CHEM.UWA.EDU.AU _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'Dalton Transactions' _publ_requested_category ? _publ_section_title ; Dinuclear gold(I) complexes of bridging bidentate carbene ligands: synthesis, structure and spectroscopic characterisation ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name 'Murray Baker' 'Peter J. Barnard' 'Susan Berners-Price' 'Brian W. Skelton' 'Allan H. White' _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_pb125 _database_code_depnum_ccdc_archive 'CCDC 227412' _audit_creation_method Xtal3.6 _audit_creation_date 03-10-10 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C44 H44 Au2 Br2 N8 O2' _chemical_formula_moiety 'C44 H40 Au2 N8, 2(H2O), 2(Br)' _chemical_formula_weight 1270.61 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 8.6625(6) _cell_length_b 10.4771(8) _cell_length_c 11.7300(8) _cell_angle_alpha 100.856(2) _cell_angle_beta 91.948(2) _cell_angle_gamma 84.965(2) _cell_volume 1041.3(1) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 2.026 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5541 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 37.9 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 9.003 _exptl_crystal_description bar _exptl_crystal_size_max .22 _exptl_crystal_size_mid .09 _exptl_crystal_size_min .05 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .49 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 21521 _reflns_number_total 10675 _reflns_Friedel_coverage 0 _reflns_number_gt 9035 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.5 _diffrn_reflns_theta_full 37.3 _diffrn_measured_fraction_theta_max .99 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .040 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .042 _refine_ls_wR_factor_ref .053 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_number_reflns 9035 _refine_ls_number_parameters 262 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .002 _refine_diff_density_min -3.729 _refine_diff_density_max 4.423 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 44 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 44 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 2 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 2 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 2 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .78683(2) .530810(10) .536490(10) .01539(6) Uani ? ? 1.00000 ? ? Br -.10493(5) -.05161(5) .78646(4) .02610(19) Uani ? ? 1.00000 ? ? C11 .7262(5) .1902(3) .5066(3) .0179(14) Uani ? ? 1.00000 ? ? C12 .5793(4) .1968(3) .5463(3) .0142(12) Uani ? ? 1.00000 ? ? C13 .4637(5) .1606(4) .4699(3) .0182(14) Uani ? ? 1.00000 ? ? C14 .4910(5) .1145(4) .3521(3) .0208(16) Uani ? ? 1.00000 ? ? C15 .6437(5) .1092(4) .3096(3) .0213(16) Uani ? ? 1.00000 ? ? C16 .7598(5) .1470(4) .3898(4) .0198(15) Uani ? ? 1.00000 ? ? C1 .8585(5) .2222(4) .5918(4) .0207(15) Uani ? ? 1.00000 ? ? N21 .8141(4) .3253(3) .6892(3) .0173(12) Uani ? ? 1.00000 ? ? C22 .7849(4) .4523(3) .6806(3) .0162(13) Uani ? ? 1.00000 ? ? N23 .7436(4) .5121(3) .7891(3) .0168(12) Uani ? ? 1.00000 ? ? C24 .7452(5) .4241(4) .8631(4) .0211(16) Uani ? ? 1.00000 ? ? C25 .7903(5) .3058(4) .7994(4) .0213(16) Uani ? ? 1.00000 ? ? C2 .7055(5) .6526(4) .8253(4) .0202(15) Uani ? ? 1.00000 ? ? C31 .2729(4) .6541(4) .8283(3) .0170(14) Uani ? ? 1.00000 ? ? C32 .4246(4) .6185(3) .7998(3) .0152(13) Uani ? ? 1.00000 ? ? C33 .5390(4) .6853(4) .8615(3) .0176(14) Uani ? ? 1.00000 ? ? C34 .5048(5) .7874(4) .9538(3) .0198(15) Uani ? ? 1.00000 ? ? C35 .3498(5) .8233(4) .9825(3) .0208(16) Uani ? ? 1.00000 ? ? C36 .2335(5) .7561(4) .9200(3) .0197(15) Uani ? ? 1.00000 ? ? C3 .1460(5) .5855(4) .7562(4) .0202(15) Uani ? ? 1.00000 ? ? N41 .1884(4) .4468(3) .7181(3) .0173(12) Uani ? ? 1.00000 ? ? C42 .2212(4) .3885(3) .6067(3) .0155(13) Uani ? ? 1.00000 ? ? N43 .2608(4) .2622(3) .6124(3) .0176(13) Uani ? ? 1.00000 ? ? C44 .2514(5) .2412(4) .7248(4) .0225(17) Uani ? ? 1.00000 ? ? C45 .2061(5) .3574(4) .7910(3) .0217(16) Uani ? ? 1.00000 ? ? C4 .3005(5) .1602(4) .5119(4) .0199(15) Uani ? ? 1.00000 ? ? O01 .8594(5) -.1314(4) 1.0484(3) .0346(18) Uani ? ? 1.00000 ? ? H12 .55853 .22660 .62694 .01700 Uiso ? ? 1.00000 ? ? H14 .40703 .08684 .30073 .02600 Uiso ? ? 1.00000 ? ? H15 .66700 .08113 .22820 .02600 Uiso ? ? 1.00000 ? ? H16 .86483 .14279 .36520 .02400 Uiso ? ? 1.00000 ? ? H1a .93961 .25018 .55186 .02500 Uiso ? ? 1.00000 ? ? H1b .89522 .14652 .62080 .02500 Uiso ? ? 1.00000 ? ? H24 .71875 .44265 .94285 .02700 Uiso ? ? 1.00000 ? ? H25 .80020 .22550 .82543 .02700 Uiso ? ? 1.00000 ? ? H2a .77107 .68450 .88958 .02700 Uiso ? ? 1.00000 ? ? H2b .72421 .69472 .76259 .02700 Uiso ? ? 1.00000 ? ? H32 .44972 .54830 .73747 .01900 Uiso ? ? 1.00000 ? ? H34 .58560 .83228 .99630 .02500 Uiso ? ? 1.00000 ? ? H35 .32380 .89406 1.04372 .02600 Uiso ? ? 1.00000 ? ? H36 .12696 .77933 .93957 .02400 Uiso ? ? 1.00000 ? ? H3a .05501 .59572 .80182 .02500 Uiso ? ? 1.00000 ? ? H3b .12375 .62484 .68991 .02500 Uiso ? ? 1.00000 ? ? H44 .27566 .15981 .75097 .02800 Uiso ? ? 1.00000 ? ? H45 .18922 .37432 .87285 .02800 Uiso ? ? 1.00000 ? ? H4a .28737 .07782 .53166 .02600 Uiso ? ? 1.00000 ? ? H4b .22944 .17288 .44976 .02600 Uiso ? ? 1.00000 ? ? H01a .85188 -.08444 .98939 .05200 Uiso ? ? 1.00000 ? ? H01b .89814 -.08215 1.11517 .05200 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .01484(6) .01570(6) .01581(6) -.00257(4) -.00035(4) .00292(4) Br .02459(19) .0280(2) .02443(19) -.00244(15) -.00015(15) .00147(15) C11 .0192(15) .0129(14) .0211(16) -.0018(11) .0017(12) .0013(12) C12 .0132(13) .0137(13) .0153(14) -.0013(10) .0009(10) .0012(11) C13 .0203(15) .0153(14) .0194(16) -.0023(12) .0002(12) .0036(12) C14 .0241(17) .0198(16) .0175(16) -.0011(13) -.0019(13) .0017(13) C15 .0292(19) .0160(15) .0167(16) -.0021(13) -.0051(13) -.0010(12) C16 .0209(16) .0176(15) .0208(17) -.0004(12) .0047(13) .0033(13) C1 .0171(15) .0191(16) .0241(18) .0003(12) .0011(13) .0001(13) N21 .0181(13) .0158(13) .0173(13) -.0010(10) -.0003(10) .0016(10) C22 .0138(13) .0149(14) .0194(15) -.0024(11) -.0021(11) .0020(12) N23 .0160(12) .0156(13) .0183(13) -.0027(10) -.0012(10) .0018(10) C24 .0245(17) .0204(16) .0183(16) .0007(13) .0019(13) .0045(13) C25 .0254(18) .0197(16) .0188(16) .0010(13) .0001(13) .0049(13) C2 .0183(15) .0162(15) .0243(18) -.0033(12) .0026(13) -.0021(13) C31 .0164(14) .0163(14) .0176(15) -.0002(11) .0017(11) .0014(12) C32 .0129(13) .0145(13) .0168(14) -.0004(10) .0007(10) -.0005(11) C33 .0191(15) .0157(14) .0169(15) -.0017(11) .0012(12) .0003(12) C34 .0210(16) .0182(15) .0188(16) -.0024(12) .0005(12) -.0004(13) C35 .0249(17) .0191(16) .0170(16) -.0023(13) .0024(13) -.0012(13) C36 .0187(15) .0197(16) .0196(16) .0018(12) .0034(12) .0018(13) C3 .0159(14) .0200(16) .0228(17) .0008(12) -.0015(12) .0002(13) N41 .0166(13) .0177(13) .0167(13) -.0026(10) -.0001(10) .0007(11) C42 .0129(13) .0154(14) .0180(15) -.0013(10) .0007(11) .0027(11) N43 .0166(13) .0172(13) .0191(14) -.0045(10) -.0003(10) .0025(11) C44 .0259(18) .0214(17) .0214(17) -.0038(14) -.0013(14) .0068(14) C45 .0251(18) .0238(17) .0167(16) -.0041(14) -.0005(13) .0040(13) C4 .0202(16) .0157(15) .0219(17) -.0037(12) -.0002(13) -.0022(13) O01 .0312(17) .040(2) .036(2) -.0159(15) -.0067(15) .0099(16) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C22 . . 2.016(4) ? Au C42 . '2 666' 2.014(4) ? C11 C12 . . 1.361(5) ? C11 C16 . . 1.392(6) ? C11 C1 . . 1.512(6) ? C12 C13 . . 1.351(5) ? C12 H12 . . .957 ? C13 C14 . . 1.396(6) ? C13 C4 . . 1.514(6) ? C14 C15 . . 1.422(6) ? C14 H14 . . .958 ? C15 C16 . . 1.385(6) ? C15 H15 . . .967 ? C16 H16 . . .959 ? C1 N21 . . 1.454(5) ? C1 H1a . . .954 ? C1 H1b . . .947 ? N21 C22 . . 1.354(5) ? N21 C25 . . 1.372(6) ? C22 N23 . . 1.353(5) ? N23 C24 . . 1.379(6) ? N23 C2 . . 1.465(5) ? C24 C25 . . 1.353(5) ? C24 H24 . . .951 ? C25 H25 . . .943 ? C2 C33 . . 1.509(6) ? C2 H2a . . .955 ? C2 H2b . . .951 ? C31 C32 . . 1.369(5) ? C31 C36 . . 1.394(5) ? C31 C3 . . 1.513(5) ? C32 C33 . . 1.371(5) ? C32 H32 . . .950 ? C33 C34 . . 1.391(5) ? C34 C35 . . 1.396(6) ? C34 H34 . . .952 ? C35 C36 . . 1.388(6) ? C35 H35 . . .948 ? C36 H36 . . .958 ? C3 N41 . . 1.456(5) ? C3 H3a . . .954 ? C3 H3b . . .953 ? N41 C42 . . 1.362(5) ? N41 C45 . . 1.379(6) ? C42 N43 . . 1.351(5) ? N43 C44 . . 1.383(6) ? N43 C4 . . 1.463(5) ? C44 C45 . . 1.349(6) ? C44 H44 . . .963 ? C45 H45 . . .957 ? C4 H4a . . .951 ? C4 H4b . . .959 ? O01 H01a . . .919 ? O01 H01b . . .924 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C22 Au C42 . . '2 666' 177.48(14) ? C12 C11 C16 . . . 121.6(4) ? C12 C11 C1 . . . 119.7(4) ? C16 C11 C1 . . . 118.6(4) ? C11 C12 C13 . . . 118.9(3) ? C11 C12 H12 . . . 120.3 ? C13 C12 H12 . . . 120.7 ? C12 C13 C14 . . . 122.0(4) ? C12 C13 C4 . . . 120.3(3) ? C14 C13 C4 . . . 117.6(3) ? C13 C14 C15 . . . 119.5(4) ? C13 C14 H14 . . . 119.8 ? C15 C14 H14 . . . 120.6 ? C14 C15 C16 . . . 117.2(4) ? C14 C15 H15 . . . 122.2 ? C16 C15 H15 . . . 120.6 ? C11 C16 C15 . . . 120.8(4) ? C11 C16 H16 . . . 119.3 ? C15 C16 H16 . . . 120.0 ? C11 C1 N21 . . . 112.8(3) ? C11 C1 H1a . . . 108.4 ? C11 C1 H1b . . . 109.3 ? N21 C1 H1a . . . 108.2 ? N21 C1 H1b . . . 108.6 ? H1a C1 H1b . . . 109.4 ? C1 N21 C22 . . . 123.7(4) ? C1 N21 C25 . . . 124.5(4) ? C22 N21 C25 . . . 111.7(3) ? Au C22 N21 . . . 127.7(3) ? Au C22 N23 . . . 128.2(3) ? N21 C22 N23 . . . 104.0(3) ? C22 N23 C24 . . . 111.4(3) ? C22 N23 C2 . . . 124.8(4) ? C24 N23 C2 . . . 123.8(3) ? N23 C24 C25 . . . 106.4(4) ? N23 C24 H24 . . . 126.8 ? C25 C24 H24 . . . 126.8 ? N21 C25 C24 . . . 106.5(4) ? N21 C25 H25 . . . 126.9 ? C24 C25 H25 . . . 126.6 ? N23 C2 C33 . . . 112.4(3) ? N23 C2 H2a . . . 108.9 ? N23 C2 H2b . . . 108.8 ? C33 C2 H2a . . . 108.5 ? C33 C2 H2b . . . 109.2 ? H2a C2 H2b . . . 108.9 ? C32 C31 C36 . . . 121.0(3) ? C32 C31 C3 . . . 119.5(3) ? C36 C31 C3 . . . 119.5(3) ? C31 C32 C33 . . . 119.4(3) ? C31 C32 H32 . . . 120.0 ? C33 C32 H32 . . . 120.6 ? C2 C33 C32 . . . 119.6(3) ? C2 C33 C34 . . . 118.8(3) ? C32 C33 C34 . . . 121.5(4) ? C33 C34 C35 . . . 118.8(4) ? C33 C34 H34 . . . 120.5 ? C35 C34 H34 . . . 120.7 ? C34 C35 C36 . . . 119.9(3) ? C34 C35 H35 . . . 120.2 ? C36 C35 H35 . . . 119.9 ? C31 C36 C35 . . . 119.4(4) ? C31 C36 H36 . . . 120.1 ? C35 C36 H36 . . . 120.5 ? C31 C3 N41 . . . 112.3(3) ? C31 C3 H3a . . . 108.7 ? C31 C3 H3b . . . 109.1 ? N41 C3 H3a . . . 108.6 ? N41 C3 H3b . . . 109.2 ? H3a C3 H3b . . . 108.9 ? C3 N41 C42 . . . 124.8(4) ? C3 N41 C45 . . . 124.4(3) ? C42 N41 C45 . . . 110.8(3) ? N41 C42 N43 . . . 104.6(3) ? N41 C42 Au . . '2 666' 128.6(3) ? N43 C42 Au . . '2 666' 126.8(3) ? C42 N43 C44 . . . 111.0(3) ? C42 N43 C4 . . . 124.3(4) ? C44 N43 C4 . . . 124.6(4) ? N43 C44 C45 . . . 106.7(4) ? N43 C44 H44 . . . 126.5 ? C45 C44 H44 . . . 126.8 ? N41 C45 C44 . . . 106.9(4) ? N41 C45 H45 . . . 126.6 ? C44 C45 H45 . . . 126.5 ? C13 C4 N43 . . . 113.8(3) ? C13 C4 H4a . . . 109.4 ? C13 C4 H4b . . . 108.3 ? N43 C4 H4a . . . 108.5 ? N43 C4 H4b . . . 108.0 ? H4a C4 H4b . . . 108.6 ? H01a O01 H01b . . . 110.2 ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 608 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min -19 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .584 _reflns_d_resolution_low 11.492 _diffrn_reflns_av_sigmaI/netI .057 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .053 _refine_ls_wR_factor_all .056 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_shift/su_mean .00009 #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_pb1p36 _database_code_depnum_ccdc_archive 'CCDC 227413' _audit_creation_method Xtal3.6 _audit_creation_date 02-09-01 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C48 H46 Au2 Br2 N10' _chemical_formula_moiety 'C44 H40 Au2 N8, 2(C2 H3 N), 2Br' _chemical_formula_weight 1316.71 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_c_a_21 _symmetry_space_group_name_Hall p_2c_-2ac loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,1/2+z 1/2-x,+y,1/2+z 1/2+x,-y,+z _cell_length_a 14.5840(10) _cell_length_b 12.3369(9) _cell_length_c 24.899(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 4479.9(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.952 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 24.5 _cell_measurement_temperature 293(2) _exptl_absorpt_coefficient_mu 8.373 _exptl_crystal_description plate _exptl_crystal_size_max .32 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .11 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .42 _exptl_absorpt_correction_T_max .78 _diffrn_reflns_number 93581 _reflns_number_total 12009 _reflns_Friedel_coverage 0 _reflns_number_gt 9299 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.56 _diffrn_reflns_theta_full 37.56 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .032 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .032 _refine_ls_wR_factor_ref .029 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_number_reflns 9299 _refine_ls_number_parameters 558 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .007 _refine_diff_density_min -2.038 _refine_diff_density_max 2.898 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 192 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 184 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 8 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 8 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 40 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au1 .375330(12) .645413(14) .50000 .01332(7) Uani ? ? 1.00000 ? ? Au2 .303887(12) .859928(14) .455927(10) .01335(7) Uani ? ? 1.00000 ? ? Br1 .64325(4) .72197(5) .61212(3) .0201(3) Uani ? ? 1.00000 ? ? Br2 .03469(4) .78763(5) .34054(3) .0250(3) Uani ? ? 1.00000 ? ? C111 .6498(4) .8070(5) .4388(2) .019(3) Uani ? ? 1.00000 ? ? C112 .6219(4) .8994(5) .4114(2) .019(3) Uani ? ? 1.00000 ? ? C113 .6852(4) .9597(5) .3818(3) .023(3) Uani ? ? 1.00000 ? ? C114 .7769(4) .9291(5) .3805(3) .024(3) Uani ? ? 1.00000 ? ? C115 .8058(4) .8385(5) .4092(3) .025(3) Uani ? ? 1.00000 ? ? C116 .7423(4) .7791(5) .4384(3) .024(3) Uani ? ? 1.00000 ? ? C11 .5858(4) .7335(5) .4697(2) .020(3) Uani ? ? 1.00000 ? ? N121 .5482(3) .6444(3) .43617(18) .0141(18) Uani ? ? 1.00000 ? ? C122 .4638(3) .6040(4) .4423(2) .013(2) Uani ? ? 1.00000 ? ? N123 .4563(3) .5242(4) .4051(2) .017(2) Uani ? ? 1.00000 ? ? C124 .5368(4) .5143(5) .3765(2) .019(3) Uani ? ? 1.00000 ? ? C125 .5952(4) .5888(5) .3957(2) .021(3) Uani ? ? 1.00000 ? ? C12 .3722(4) .4606(5) .3951(3) .023(3) Uani ? ? 1.00000 ? ? C131 .2864(4) .5771(5) .3253(3) .020(3) Uani ? ? 1.00000 ? ? C132 .3299(4) .4798(4) .3401(3) .020(3) Uani ? ? 1.00000 ? ? C133 .3337(4) .3940(5) .3037(3) .023(3) Uani ? ? 1.00000 ? ? C134 .2946(4) .4030(5) .2524(3) .027(3) Uani ? ? 1.00000 ? ? C135 .2540(4) .4992(5) .2374(3) .028(3) Uani ? ? 1.00000 ? ? C136 .2487(4) .5856(5) .2740(3) .027(3) Uani ? ? 1.00000 ? ? C13 .2798(4) .6748(5) .3611(3) .023(3) Uani ? ? 1.00000 ? ? N141 .3625(3) .7447(4) .3571(2) .018(2) Uani ? ? 1.00000 ? ? C142 .3838(4) .8193(5) .3949(3) .015(3) Uani ? ? 1.00000 ? ? N143 .4667(3) .8593(4) .3791(2) .017(2) Uani ? ? 1.00000 ? ? C144 .4942(4) .8100(5) .3321(2) .020(3) Uani ? ? 1.00000 ? ? C145 .4283(4) .7395(5) .3180(2) .022(3) Uani ? ? 1.00000 ? ? C14 .5226(4) .9362(5) .4104(3) .023(3) Uani ? ? 1.00000 ? ? C21 .3021(4) 1.0465(5) .5623(3) .017(3) Uani ? ? 1.00000 ? ? C211 .3498(4) 1.0324(4) .6158(2) .018(2) Uani ? ? 1.00000 ? ? C212 .3944(4) .9355(5) .6320(3) .022(3) Uani ? ? 1.00000 ? ? C213 .4401(4) .9332(5) .6810(3) .029(3) Uani ? ? 1.00000 ? ? C214 .4438(5) 1.0223(6) .7140(3) .034(4) Uani ? ? 1.00000 ? ? C215 .4025(5) 1.1181(5) .6978(3) .029(3) Uani ? ? 1.00000 ? ? C216 .3558(4) 1.1219(4) .6501(3) .022(3) Uani ? ? 1.00000 ? ? C22 .0968(4) .7625(4) .4916(2) .020(3) Uani ? ? 1.00000 ? ? N221 .2211(3) .9772(4) .5543(2) .017(2) Uani ? ? 1.00000 ? ? C222 .2147(4) .8986(4) .5172(2) .016(2) Uani ? ? 1.00000 ? ? N223 .1311(3) .8536(4) .52486(18) .0158(19) Uani ? ? 1.00000 ? ? C224 .0854(4) .9049(4) .5659(2) .020(3) Uani ? ? 1.00000 ? ? C225 .1411(4) .9839(5) .5850(3) .024(3) Uani ? ? 1.00000 ? ? C231 .0631(4) .5979(4) .5518(2) .018(2) Uani ? ? 1.00000 ? ? C232 .0322(4) .6894(5) .5225(2) .018(2) Uani ? ? 1.00000 ? ? C233 -.0596(4) .7142(5) .5229(2) .022(3) Uani ? ? 1.00000 ? ? C234 -.1230(4) .6540(5) .5532(3) .023(3) Uani ? ? 1.00000 ? ? C235 -.0929(4) .5671(5) .5826(3) .024(3) Uani ? ? 1.00000 ? ? C236 .0005(4) .5374(4) .5814(2) .020(3) Uani ? ? 1.00000 ? ? C23 .1629(4) .5635(4) .5543(2) .020(3) Uani ? ? 1.00000 ? ? N241 .2182(3) .6433(4) .5836(2) .017(2) Uani ? ? 1.00000 ? ? C242 .2973(4) .6872(5) .5661(3) .015(3) Uani ? ? 1.00000 ? ? N243 .3202(3) .7631(4) .6032(2) .016(2) Uani ? ? 1.00000 ? ? C244 .2562(4) .7664(5) .6440(2) .020(3) Uani ? ? 1.00000 ? ? C245 .1923(4) .6900(5) .6321(2) .021(3) Uani ? ? 1.00000 ? ? C24 .3992(4) .8359(5) .5965(3) .020(3) Uani ? ? 1.00000 ? ? N011 .4952(5) .4118(6) .7207(3) .052(4) Uani ? ? 1.00000 ? ? C012 .4851(5) .5018(6) .7171(3) .032(4) Uani ? ? 1.00000 ? ? C013 .4711(5) .6181(6) .7113(3) .033(4) Uani ? ? 1.00000 ? ? N021 .2955(5) .9079(6) .2512(3) .051(4) Uani ? ? 1.00000 ? ? C022 .3118(5) .9989(6) .2483(3) .036(4) Uani ? ? 1.00000 ? ? C023 .3329(5) 1.1151(6) .2471(3) .035(4) Uani ? ? 1.00000 ? ? H113 .66395 1.02368 .36204 .02900 Uiso ? ? 1.00000 ? ? H114 .82062 .96955 .35950 .03000 Uiso ? ? 1.00000 ? ? H115 .86923 .81849 .40905 .03200 Uiso ? ? 1.00000 ? ? H116 .76253 .71859 .45849 .03000 Uiso ? ? 1.00000 ? ? H11a .53593 .77551 .48358 .02600 Uiso ? ? 1.00000 ? ? H11b .61851 .70293 .49934 .02600 Uiso ? ? 1.00000 ? ? H124 .54696 .46382 .34737 .02400 Uiso ? ? 1.00000 ? ? H125 .65681 .60217 .38388 .02700 Uiso ? ? 1.00000 ? ? H12a .32782 .48002 .42160 .02800 Uiso ? ? 1.00000 ? ? H12b .38558 .38556 .39822 .02800 Uiso ? ? 1.00000 ? ? H133 .36358 .32786 .31371 .02800 Uiso ? ? 1.00000 ? ? H134 .29627 .34266 .22826 .03300 Uiso ? ? 1.00000 ? ? H135 .22949 .50859 .20192 .03600 Uiso ? ? 1.00000 ? ? H136 .21883 .65256 .26353 .03300 Uiso ? ? 1.00000 ? ? H13a .27245 .65097 .39771 .03100 Uiso ? ? 1.00000 ? ? H13b .22646 .71600 .35169 .03100 Uiso ? ? 1.00000 ? ? H144 .55007 .82518 .31342 .02500 Uiso ? ? 1.00000 ? ? H145 .42696 .69518 .28614 .02700 Uiso ? ? 1.00000 ? ? H14a .51912 1.00585 .39313 .03000 Uiso ? ? 1.00000 ? ? H14b .49930 .94167 .44544 .03000 Uiso ? ? 1.00000 ? ? H21a .34477 1.03226 .53412 .02100 Uiso ? ? 1.00000 ? ? H21b .28279 1.12088 .55933 .02100 Uiso ? ? 1.00000 ? ? H213 .46974 .86732 .69173 .03500 Uiso ? ? 1.00000 ? ? H214 .47537 1.01796 .74802 .04400 Uiso ? ? 1.00000 ? ? H215 .40536 1.18239 .71948 .03800 Uiso ? ? 1.00000 ? ? H216 .32702 1.18792 .63936 .02800 Uiso ? ? 1.00000 ? ? H22a .14748 .72154 .47846 .02400 Uiso ? ? 1.00000 ? ? H22b .06426 .79149 .46100 .02400 Uiso ? ? 1.00000 ? ? H224 .02513 .88713 .57892 .02500 Uiso ? ? 1.00000 ? ? H225 .12841 1.03434 .61315 .02900 Uiso ? ? 1.00000 ? ? H233 -.08093 .77570 .50168 .02700 Uiso ? ? 1.00000 ? ? H234 -.18632 .67420 .55275 .02800 Uiso ? ? 1.00000 ? ? H235 -.13529 .52571 .60421 .03000 Uiso ? ? 1.00000 ? ? H236 .02129 .47436 .60041 .02600 Uiso ? ? 1.00000 ? ? H23a .18617 .55671 .51847 .02600 Uiso ? ? 1.00000 ? ? H23b .16707 .49521 .57165 .02600 Uiso ? ? 1.00000 ? ? H244 .25664 .81383 .67437 .02500 Uiso ? ? 1.00000 ? ? H245 .14019 .67118 .65356 .02700 Uiso ? ? 1.00000 ? ? H24a .45420 .79679 .60456 .02600 Uiso ? ? 1.00000 ? ? H24b .40220 .85828 .55955 .02600 Uiso ? ? 1.00000 ? ? H013a .52414 .65140 .69643 .05200 Uiso ? ? 1.00000 ? ? H013b .45993 .64970 .74610 .05200 Uiso ? ? 1.00000 ? ? H013c .41966 .63299 .68867 .05200 Uiso ? ? 1.00000 ? ? H023a .29609 1.15250 .27274 .05400 Uiso ? ? 1.00000 ? ? H023b .32122 1.14404 .21235 .05400 Uiso ? ? 1.00000 ? ? H023c .39606 1.12660 .25577 .05400 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au1 .01381(7) .01339(7) .01276(8) .00080(7) .00133(7) .00032(10) Au2 .01410(7) .01356(7) .01238(8) .00140(7) .00146(7) -.00011(10) Br1 .0203(3) .0208(2) .0193(3) -.0026(2) .0008(2) -.0001(2) Br2 .0202(3) .0251(3) .0298(3) -.0006(2) -.0019(2) -.0041(3) C111 .018(3) .019(3) .019(3) -.006(2) .000(2) -.005(2) C112 .020(3) .021(2) .017(3) -.006(2) .003(2) -.007(2) C113 .026(3) .023(3) .021(3) -.004(2) .001(2) -.001(2) C114 .024(3) .022(3) .025(3) -.008(2) .004(2) -.007(2) C115 .016(3) .024(3) .036(4) -.006(2) -.000(2) -.007(3) C116 .016(3) .026(3) .029(3) -.002(2) -.007(2) -.002(2) C11 .020(2) .022(2) .018(3) -.003(2) .001(2) -.003(2) N121 .0132(18) .0133(18) .016(2) -.0018(17) .0017(16) -.0014(17) C122 .015(2) .012(2) .012(2) .0008(17) -.0021(17) .0019(17) N123 .021(2) .015(2) .015(2) .0006(17) .0033(18) -.0020(17) C124 .017(3) .024(3) .017(3) -.001(2) .005(2) -.006(2) C125 .016(2) .029(3) .019(3) .004(2) .004(2) -.001(2) C12 .023(3) .018(3) .026(4) -.006(2) -.001(2) -.000(2) C131 .016(2) .021(3) .021(3) -.003(2) -.000(2) -.005(2) C132 .013(2) .021(3) .024(3) -.007(2) -.002(2) -.004(2) C133 .023(3) .017(2) .029(3) .000(2) -.001(3) -.002(2) C134 .027(3) .029(3) .024(3) -.000(2) -.000(2) -.009(3) C135 .027(3) .030(3) .027(3) -.002(3) -.006(3) -.006(3) C136 .021(3) .029(3) .031(3) .002(2) -.009(2) -.001(3) C13 .016(3) .022(3) .029(3) .002(2) -.000(2) -.005(2) N141 .019(2) .020(2) .014(2) .0034(18) .0009(18) .0002(18) C142 .017(3) .014(2) .013(3) .0024(18) -.002(2) -.000(2) N143 .018(2) .018(2) .015(2) -.0011(18) .0018(16) -.0013(19) C144 .021(3) .025(3) .016(3) .001(2) .006(2) -.003(2) C145 .024(3) .025(3) .018(3) .004(2) .003(2) -.005(2) C14 .018(3) .020(3) .032(3) .000(2) -.000(2) -.006(2) C21 .017(3) .019(2) .016(3) -.0010(18) .003(2) -.003(2) C211 .015(2) .019(2) .019(3) .0005(19) .002(2) -.000(2) C212 .017(2) .023(3) .026(3) .002(2) -.000(2) -.008(2) C213 .028(3) .027(3) .031(3) .005(2) -.013(3) -.004(3) C214 .034(3) .038(4) .030(4) .005(3) -.014(3) -.011(3) C215 .034(3) .027(3) .027(3) .005(3) -.003(3) -.011(3) C216 .024(3) .019(2) .022(3) .001(2) .000(2) -.003(2) C22 .021(3) .022(2) .015(3) -.004(2) -.002(2) -.002(2) N221 .013(2) .020(2) .018(2) -.0006(16) .0012(17) -.0007(18) C222 .016(2) .016(2) .017(3) .0030(18) -.000(2) .0006(19) N223 .018(2) .0171(19) .0122(19) -.0001(17) .0037(16) -.0009(17) C224 .020(3) .019(2) .021(3) .001(2) .006(2) -.004(2) C225 .025(3) .016(2) .031(3) .003(2) .006(2) -.002(2) C231 .021(3) .020(2) .014(2) -.004(2) -.003(2) .000(2) C232 .019(3) .024(3) .011(2) -.001(2) -.000(2) -.005(2) C233 .022(3) .022(3) .021(3) .001(2) -.002(2) -.006(2) C234 .017(3) .027(3) .024(3) .002(2) -.000(2) -.006(3) C235 .021(3) .028(3) .023(3) -.008(2) .002(2) -.008(2) C236 .021(3) .019(2) .020(3) -.005(2) .003(2) -.005(2) C23 .018(2) .016(2) .025(3) -.003(2) .003(2) -.002(2) N241 .018(2) .0150(19) .019(2) .0006(17) -.0008(16) .0018(19) C242 .017(3) .015(2) .013(3) .0028(18) .002(2) .005(2) N243 .015(2) .015(2) .018(2) -.0017(16) .0002(18) -.0035(17) C244 .021(3) .024(3) .014(3) .004(2) .003(2) .001(2) C245 .019(3) .025(3) .019(3) .001(2) .004(2) -.002(2) C24 .015(2) .021(3) .023(3) .003(2) -.000(2) -.003(2) N011 .063(5) .051(4) .041(4) .010(4) -.021(4) .007(3) C012 .038(4) .038(3) .021(3) .002(3) -.005(3) .005(3) C013 .034(4) .037(4) .029(4) -.001(3) .004(3) .004(3) N021 .066(5) .040(4) .047(4) .001(3) -.016(4) -.009(3) C022 .044(4) .040(4) .023(3) .003(3) -.010(3) -.005(3) C023 .043(4) .032(3) .030(4) -.002(3) -.004(3) .001(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au1 Au2 . . 3.0485(3) ? Au1 C122 . . 1.997(5) ? Au1 C242 . . 2.066(6) ? Au2 C142 . . 1.979(6) ? Au2 C222 . . 2.061(5) ? C111 C112 . . 1.389(8) ? C111 C116 . . 1.392(8) ? C111 C11 . . 1.511(8) ? C112 C113 . . 1.396(8) ? C112 C14 . . 1.519(8) ? C113 C114 . . 1.390(9) ? C113 H113 . . .981 ? C114 C115 . . 1.392(9) ? C114 H114 . . .964 ? C115 C116 . . 1.386(9) ? C115 H115 . . .958 ? C116 H116 . . .946 ? C11 N121 . . 1.486(7) ? C11 H11a . . .957 ? C11 H11b . . .956 ? N121 C122 . . 1.337(7) ? N121 C125 . . 1.398(7) ? C122 N123 . . 1.356(7) ? N123 C124 . . 1.378(7) ? N123 C12 . . 1.477(7) ? C124 C125 . . 1.341(8) ? C124 H124 . . .968 ? C125 H125 . . .960 ? C12 C132 . . 1.520(9) ? C12 H12a . . .955 ? C12 H12b . . .950 ? C131 C132 . . 1.408(8) ? C131 C136 . . 1.394(9) ? C131 C13 . . 1.501(9) ? C132 C133 . . 1.394(9) ? C133 C134 . . 1.404(10) ? C133 H133 . . .958 ? C134 C135 . . 1.378(9) ? C134 H134 . . .957 ? C135 C136 . . 1.406(9) ? C135 H135 . . .960 ? C136 H136 . . .969 ? C13 N141 . . 1.486(8) ? C13 H13a . . .965 ? C13 H13b . . .959 ? N141 C142 . . 1.352(8) ? N141 C145 . . 1.369(8) ? C142 N143 . . 1.363(7) ? N143 C144 . . 1.378(8) ? N143 C14 . . 1.473(8) ? C144 C145 . . 1.344(8) ? C144 H144 . . .957 ? C145 H145 . . .963 ? C14 H14a . . .962 ? C14 H14b . . .940 ? C21 C211 . . 1.515(9) ? C21 N221 . . 1.471(7) ? C21 H21a . . .953 ? C21 H21b . . .963 ? C211 C212 . . 1.419(8) ? C211 C216 . . 1.398(8) ? C212 C213 . . 1.391(9) ? C212 C24 . . 1.515(9) ? C213 C214 . . 1.374(10) ? C213 H213 . . .958 ? C214 C215 . . 1.387(10) ? C214 H214 . . .964 ? C215 C216 . . 1.371(10) ? C215 H215 . . .960 ? C216 H216 . . .954 ? C22 N223 . . 1.483(7) ? C22 C232 . . 1.515(8) ? C22 H22a . . .954 ? C22 H22b . . .965 ? N221 C222 . . 1.342(7) ? N221 C225 . . 1.398(8) ? C222 N223 . . 1.354(7) ? N223 C224 . . 1.374(7) ? C224 C225 . . 1.355(8) ? C224 H224 . . .962 ? C225 H225 . . .955 ? C231 C232 . . 1.417(8) ? C231 C236 . . 1.391(8) ? C231 C23 . . 1.518(8) ? C232 C233 . . 1.374(8) ? C233 C234 . . 1.405(9) ? C233 H233 . . .976 ? C234 C235 . . 1.371(9) ? C234 H234 . . .956 ? C235 C236 . . 1.411(8) ? C235 H235 . . .965 ? C236 H236 . . .959 ? C23 N241 . . 1.467(7) ? C23 H23a . . .958 ? C23 H23b . . .948 ? N241 C242 . . 1.348(7) ? N241 C245 . . 1.391(8) ? C242 N243 . . 1.356(8) ? N243 C244 . . 1.379(8) ? N243 C24 . . 1.471(7) ? C244 C245 . . 1.358(8) ? C244 H244 . . .957 ? C245 H245 . . .957 ? C24 H24a . . .957 ? C24 H24b . . .961 ? N011 C012 . . 1.124(11) ? C012 C013 . . 1.456(11) ? C013 H013a . . .952 ? C013 H013b . . .963 ? C013 H013c . . .956 ? N021 C022 . . 1.150(11) ? C022 C023 . . 1.466(11) ? C023 H023a . . .952 ? C023 H023b . . .952 ? C023 H023c . . .957 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C122 Au1 C242 . . . 173.0(2) ? C142 Au2 C222 . . . 176.9(2) ? C112 C111 C116 . . . 118.8(5) ? C112 C111 C11 . . . 124.2(5) ? C116 C111 C11 . . . 117.0(5) ? C111 C112 C113 . . . 120.2(5) ? C111 C112 C14 . . . 122.2(5) ? C113 C112 C14 . . . 117.5(5) ? C112 C113 C114 . . . 120.3(6) ? C112 C113 H113 . . . 119.0 ? C114 C113 H113 . . . 120.7 ? C113 C114 C115 . . . 119.7(6) ? C113 C114 H114 . . . 120.6 ? C115 C114 H114 . . . 119.6 ? C114 C115 C116 . . . 119.5(5) ? C114 C115 H115 . . . 119.8 ? C116 C115 H115 . . . 120.7 ? C111 C116 C115 . . . 121.4(6) ? C111 C116 H116 . . . 119.5 ? C115 C116 H116 . . . 119.1 ? C111 C11 N121 . . . 112.7(5) ? C111 C11 H11a . . . 109.2 ? C111 C11 H11b . . . 108.7 ? N121 C11 H11a . . . 108.9 ? N121 C11 H11b . . . 109.0 ? H11a C11 H11b . . . 108.3 ? C11 N121 C122 . . . 123.4(4) ? C11 N121 C125 . . . 126.0(4) ? C122 N121 C125 . . . 110.5(4) ? Au1 C122 N121 . . . 125.6(4) ? Au1 C122 N123 . . . 128.7(4) ? N121 C122 N123 . . . 105.4(4) ? C122 N123 C124 . . . 110.4(4) ? C122 N123 C12 . . . 124.6(5) ? C124 N123 C12 . . . 125.0(5) ? N123 C124 C125 . . . 107.2(5) ? N123 C124 H124 . . . 125.1 ? C125 C124 H124 . . . 127.6 ? N121 C125 C124 . . . 106.4(5) ? N121 C125 H125 . . . 126.5 ? C124 C125 H125 . . . 127.1 ? N123 C12 C132 . . . 114.0(5) ? N123 C12 H12a . . . 108.2 ? N123 C12 H12b . . . 109.4 ? C132 C12 H12a . . . 108.0 ? C132 C12 H12b . . . 108.0 ? H12a C12 H12b . . . 109.1 ? C132 C131 C136 . . . 118.8(6) ? C132 C131 C13 . . . 123.9(6) ? C136 C131 C13 . . . 117.2(5) ? C12 C132 C131 . . . 123.4(5) ? C12 C132 C133 . . . 116.8(5) ? C131 C132 C133 . . . 119.7(6) ? C132 C133 C134 . . . 121.0(6) ? C132 C133 H133 . . . 119.8 ? C134 C133 H133 . . . 119.2 ? C133 C134 C135 . . . 119.3(6) ? C133 C134 H134 . . . 120.0 ? C135 C134 H134 . . . 120.7 ? C134 C135 C136 . . . 120.1(6) ? C134 C135 H135 . . . 120.9 ? C136 C135 H135 . . . 119.0 ? C131 C136 C135 . . . 121.0(6) ? C131 C136 H136 . . . 119.2 ? C135 C136 H136 . . . 119.7 ? C131 C13 N141 . . . 112.1(5) ? C131 C13 H13a . . . 108.9 ? C131 C13 H13b . . . 109.4 ? N141 C13 H13a . . . 109.3 ? N141 C13 H13b . . . 109.6 ? H13a C13 H13b . . . 107.5 ? C13 N141 C142 . . . 122.3(5) ? C13 N141 C145 . . . 126.0(5) ? C142 N141 C145 . . . 111.6(5) ? Au2 C142 N141 . . . 124.9(4) ? Au2 C142 N143 . . . 130.7(4) ? N141 C142 N143 . . . 104.4(5) ? C142 N143 C144 . . . 110.1(5) ? C142 N143 C14 . . . 124.8(5) ? C144 N143 C14 . . . 124.8(5) ? N143 C144 C145 . . . 107.5(5) ? N143 C144 H144 . . . 125.1 ? C145 C144 H144 . . . 127.4 ? N141 C145 C144 . . . 106.4(5) ? N141 C145 H145 . . . 126.8 ? C144 C145 H145 . . . 126.8 ? C112 C14 N143 . . . 110.2(5) ? C112 C14 H14a . . . 108.9 ? C112 C14 H14b . . . 110.5 ? N143 C14 H14a . . . 108.1 ? N143 C14 H14b . . . 109.7 ? H14a C14 H14b . . . 109.3 ? C211 C21 N221 . . . 114.9(5) ? C211 C21 H21a . . . 109.0 ? C211 C21 H21b . . . 108.1 ? N221 C21 H21a . . . 108.5 ? N221 C21 H21b . . . 108.0 ? H21a C21 H21b . . . 108.1 ? C21 C211 C212 . . . 123.9(5) ? C21 C211 C216 . . . 118.3(5) ? C212 C211 C216 . . . 117.6(5) ? C211 C212 C213 . . . 119.1(6) ? C211 C212 C24 . . . 122.6(6) ? C213 C212 C24 . . . 118.2(5) ? C212 C213 C214 . . . 121.8(6) ? C212 C213 H213 . . . 118.5 ? C214 C213 H213 . . . 119.6 ? C213 C214 C215 . . . 119.4(6) ? C213 C214 H214 . . . 120.0 ? C215 C214 H214 . . . 120.7 ? C214 C215 C216 . . . 119.9(6) ? C214 C215 H215 . . . 121.4 ? C216 C215 H215 . . . 118.7 ? C211 C216 C215 . . . 122.2(5) ? C211 C216 H216 . . . 118.4 ? C215 C216 H216 . . . 119.4 ? N223 C22 C232 . . . 112.1(5) ? N223 C22 H22a . . . 109.4 ? N223 C22 H22b . . . 109.0 ? C232 C22 H22a . . . 109.9 ? C232 C22 H22b . . . 108.4 ? H22a C22 H22b . . . 107.9 ? C21 N221 C222 . . . 124.7(5) ? C21 N221 C225 . . . 124.2(5) ? C222 N221 C225 . . . 111.1(4) ? Au2 C222 N221 . . . 129.2(4) ? Au2 C222 N223 . . . 125.3(4) ? N221 C222 N223 . . . 105.2(5) ? C22 N223 C222 . . . 122.4(5) ? C22 N223 C224 . . . 126.9(4) ? C222 N223 C224 . . . 110.6(5) ? N223 C224 C225 . . . 107.6(5) ? N223 C224 H224 . . . 126.1 ? C225 C224 H224 . . . 126.4 ? N221 C225 C224 . . . 105.4(5) ? N221 C225 H225 . . . 126.9 ? C224 C225 H225 . . . 127.6 ? C232 C231 C236 . . . 119.4(5) ? C232 C231 C23 . . . 123.3(5) ? C236 C231 C23 . . . 117.2(5) ? C22 C232 C231 . . . 122.6(5) ? C22 C232 C233 . . . 118.5(5) ? C231 C232 C233 . . . 118.9(5) ? C232 C233 C234 . . . 121.9(5) ? C232 C233 H233 . . . 118.6 ? C234 C233 H233 . . . 119.5 ? C233 C234 C235 . . . 119.3(5) ? C233 C234 H234 . . . 119.4 ? C235 C234 H234 . . . 121.3 ? C234 C235 C236 . . . 120.0(6) ? C234 C235 H235 . . . 120.4 ? C236 C235 H235 . . . 119.5 ? C231 C236 C235 . . . 120.4(5) ? C231 C236 H236 . . . 119.3 ? C235 C236 H236 . . . 120.3 ? C231 C23 N241 . . . 111.0(4) ? C231 C23 H23a . . . 109.0 ? C231 C23 H23b . . . 109.2 ? N241 C23 H23a . . . 109.1 ? N241 C23 H23b . . . 109.5 ? H23a C23 H23b . . . 108.9 ? C23 N241 C242 . . . 125.4(5) ? C23 N241 C245 . . . 124.2(5) ? C242 N241 C245 . . . 110.3(5) ? Au1 C242 N241 . . . 129.0(4) ? Au1 C242 N243 . . . 125.4(4) ? N241 C242 N243 . . . 105.5(5) ? C242 N243 C244 . . . 110.9(5) ? C242 N243 C24 . . . 122.5(5) ? C244 N243 C24 . . . 126.5(5) ? N243 C244 C245 . . . 106.5(5) ? N243 C244 H244 . . . 126.6 ? C245 C244 H244 . . . 126.9 ? N241 C245 C244 . . . 106.9(5) ? N241 C245 H245 . . . 126.8 ? C244 C245 H245 . . . 126.4 ? C212 C24 N243 . . . 113.2(5) ? C212 C24 H24a . . . 109.0 ? C212 C24 H24b . . . 109.1 ? N243 C24 H24a . . . 108.9 ? N243 C24 H24b . . . 108.6 ? H24a C24 H24b . . . 107.9 ? N011 C012 C013 . . . 178.8(8) ? C012 C013 H013a . . . 110.4 ? C012 C013 H013b . . . 109.6 ? C012 C013 H013c . . . 111.0 ? H013a C013 H013b . . . 108.2 ? H013a C013 H013c . . . 108.9 ? H013b C013 H013c . . . 108.7 ? N021 C022 C023 . . . 177.5(8) ? C022 C023 H023a . . . 110.0 ? C022 C023 H023b . . . 110.3 ? C022 C023 H023c . . . 110.0 ? H023a C023 H023b . . . 109.1 ? H023a C023 H023c . . . 108.7 ? H023b C023 H023c . . . 108.7 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2528 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 42 _reflns_number_observed ? _reflns_d_resolution_high .583 _reflns_d_resolution_low 12.419 _diffrn_reflns_av_sigmaI/netI .074 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .05 _refine_ls_wR_factor_all .031 _refine_ls_goodness_of_fit_all .957 _refine_ls_shift/su_mean .0001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_pch1b _database_code_depnum_ccdc_archive 'CCDC 227414' _audit_creation_method Xtal3.6 _audit_creation_date 03-03-13 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C40 H40 Au2 Br2 N12 O2' _chemical_formula_moiety 'C40 H36 Au2 N12, 2 (H2 O), 2(Br)' _chemical_formula_weight 1274.58 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 8.5150(10) _cell_length_b 11.008(2) _cell_length_c 11.847(2) _cell_angle_alpha 97.120(3) _cell_angle_beta 102.365(3) _cell_angle_gamma 97.137(3) _cell_volume 1063.2(3) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5352 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 33.42 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 8.821 _exptl_crystal_description prism _exptl_crystal_size_max .17 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .65 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 18577 _reflns_number_total 4846 _reflns_Friedel_coverage 0 _reflns_number_gt 4219 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .051 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .032 _refine_ls_wR_factor_ref .04 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_number_reflns 4219 _refine_ls_number_parameters 262 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .005 _refine_diff_density_min -1.561 _refine_diff_density_max 1.521 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 40 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 40 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 2 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 2 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 2 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .81079(2) .53196(2) .547960(17) .02027(10) Uani ? ? 1.00000 ? ? Br .07973(7) -.04197(6) .77867(5) .0322(3) Uani ? ? 1.00000 ? ? C11 .6600(7) .1979(5) .5361(5) .024(2) Uani ? ? 1.00000 ? ? N12 .5199(6) .2091(4) .5711(4) .0225(19) Uani ? ? 1.00000 ? ? C13 .3769(7) .1669(5) .4907(5) .022(2) Uani ? ? 1.00000 ? ? C14 .3690(7) .1138(6) .3758(5) .029(2) Uani ? ? 1.00000 ? ? C15 .5153(8) .1007(6) .3404(5) .030(3) Uani ? ? 1.00000 ? ? C16 .6627(8) .1451(6) .4227(5) .031(3) Uani ? ? 1.00000 ? ? C1 .8198(7) .2388(5) .6263(5) .028(2) Uani ? ? 1.00000 ? ? N21 .8169(5) .3416(4) .7166(4) .0224(19) Uani ? ? 1.00000 ? ? C22 .8260(6) .4643(5) .7010(5) .022(2) Uani ? ? 1.00000 ? ? N23 .8301(6) .5278(4) .8090(4) .0236(19) Uani ? ? 1.00000 ? ? C24 .8200(7) .4455(6) .8893(5) .029(3) Uani ? ? 1.00000 ? ? C25 .8122(8) .3289(6) .8319(5) .030(3) Uani ? ? 1.00000 ? ? C2 .8393(7) .6626(5) .8369(5) .027(2) Uani ? ? 1.00000 ? ? C31 .4049(7) .6682(5) .8244(5) .023(2) Uani ? ? 1.00000 ? ? N32 .5429(6) .6368(4) .8000(4) .0227(19) Uani ? ? 1.00000 ? ? C33 .6866(6) .6983(5) .8692(4) .020(2) Uani ? ? 1.00000 ? ? C34 .6954(7) .7906(5) .9636(5) .028(2) Uani ? ? 1.00000 ? ? C35 .5520(8) .8233(5) .9867(5) .031(3) Uani ? ? 1.00000 ? ? C36 .4022(8) .7599(5) .9158(5) .028(2) Uani ? ? 1.00000 ? ? C3 .2475(7) .6005(5) .7422(5) .027(2) Uani ? ? 1.00000 ? ? N41 .2505(5) .4658(4) .7162(4) .0213(18) Uani ? ? 1.00000 ? ? C42 .2225(6) .4000(5) .6066(4) .020(2) Uani ? ? 1.00000 ? ? N43 .2359(5) .2820(4) .6244(4) .0213(18) Uani ? ? 1.00000 ? ? C44 .2702(7) .2722(6) .7432(5) .027(2) Uani ? ? 1.00000 ? ? C45 .2798(7) .3877(6) .7999(5) .028(2) Uani ? ? 1.00000 ? ? C4 .2197(7) .1761(5) .5304(5) .024(2) Uani ? ? 1.00000 ? ? O01 .8386(7) .0836(5) .9375(4) .051(3) Uani ? ? 1.00000 ? ? H14 .26505 .08731 .32164 .03700 Uiso ? ? 1.00000 ? ? H15 .51509 .06227 .26218 .04200 Uiso ? ? 1.00000 ? ? H16 .76529 .13980 .40156 .04000 Uiso ? ? 1.00000 ? ? H1a .90353 .26325 .58752 .03800 Uiso ? ? 1.00000 ? ? H1b .84857 .16970 .66449 .03800 Uiso ? ? 1.00000 ? ? H24 .81883 .46817 .97066 .03800 Uiso ? ? 1.00000 ? ? H25 .80593 .25309 .86336 .03800 Uiso ? ? 1.00000 ? ? H2a .85678 .69960 .77144 .03500 Uiso ? ? 1.00000 ? ? H2b .93066 .69307 .90172 .03500 Uiso ? ? 1.00000 ? ? H34 .79902 .83111 1.01085 .03500 Uiso ? ? 1.00000 ? ? H35 .55389 .88701 1.04986 .04000 Uiso ? ? 1.00000 ? ? H36 .29927 .77975 .92995 .03600 Uiso ? ? 1.00000 ? ? H3a .22973 .63426 .67064 .03500 Uiso ? ? 1.00000 ? ? H3b .15800 .61293 .77769 .03500 Uiso ? ? 1.00000 ? ? H44 .28428 .19869 .77678 .03500 Uiso ? ? 1.00000 ? ? H45 .30391 .41255 .88363 .03500 Uiso ? ? 1.00000 ? ? H4a .18634 .10121 .55845 .03300 Uiso ? ? 1.00000 ? ? H4b .13594 .18486 .46493 .03300 Uiso ? ? 1.00000 ? ? H01a .88781 .03102 .89362 .07600 Uiso ? ? 1.00000 ? ? H01b .88159 .08525 1.01641 .07600 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .01884(11) .02046(12) .02080(11) .00260(8) .00323(8) .00341(7) Br .0321(3) .0335(3) .0284(3) .0003(3) .0091(2) -.0031(2) C11 .027(3) .017(3) .031(3) .007(2) .009(2) .003(2) N12 .024(2) .020(2) .024(2) .007(2) .005(2) .0032(18) C13 .028(3) .012(2) .026(3) .002(2) .007(2) .003(2) C14 .030(3) .025(3) .030(3) .001(2) .005(2) .001(2) C15 .043(4) .025(3) .026(3) .010(3) .014(3) .002(2) C16 .036(3) .024(3) .041(3) .011(3) .023(3) .006(3) C1 .020(3) .021(3) .043(3) .004(2) .007(2) .002(2) N21 .014(2) .025(2) .028(2) .0053(18) .0015(18) .006(2) C22 .014(2) .023(3) .028(3) .001(2) .005(2) .004(2) N23 .021(2) .024(2) .025(2) .003(2) .0035(19) .0039(19) C24 .027(3) .040(4) .023(3) .010(3) .006(2) .008(2) C25 .035(3) .030(3) .033(3) .011(3) .016(3) .017(3) C2 .024(3) .023(3) .030(3) .001(2) .003(2) .002(2) C31 .027(3) .018(3) .027(3) .007(2) .009(2) .005(2) N32 .023(2) .023(2) .021(2) .005(2) .0061(19) -.0000(18) C33 .022(3) .017(3) .020(2) .003(2) .003(2) .004(2) C34 .031(3) .023(3) .022(3) -.001(2) -.003(2) .002(2) C35 .048(4) .019(3) .025(3) .010(3) .005(3) -.003(2) C36 .038(3) .021(3) .031(3) .014(3) .016(3) .003(2) C3 .023(3) .027(3) .032(3) .011(2) .009(2) .002(2) N41 .021(2) .025(2) .020(2) .0071(19) .0072(18) .0029(18) C42 .014(2) .022(3) .024(3) .000(2) .004(2) .000(2) N43 .018(2) .024(2) .024(2) .0045(18) .0069(18) .0032(18) C44 .024(3) .034(3) .025(3) .005(2) .006(2) .008(2) C45 .030(3) .032(3) .025(3) .005(3) .011(2) .003(2) C4 .025(3) .022(3) .022(3) -.003(2) .003(2) -.003(2) O01 .076(4) .047(3) .053(3) .039(3) .035(3) .028(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C22 . . 2.029(6) ? Au C42 . '2 666' 2.040(6) ? C11 N12 . . 1.359(8) ? C11 C16 . . 1.403(9) ? C11 C1 . . 1.517(7) ? N12 C13 . . 1.364(6) ? C13 C14 . . 1.396(8) ? C13 C4 . . 1.522(9) ? C14 C15 . . 1.416(10) ? C14 H14 . . .963 ? C15 C16 . . 1.403(8) ? C15 H15 . . .969 ? C16 H16 . . .965 ? C1 N21 . . 1.464(8) ? C1 H1a . . .957 ? C1 H1b . . .963 ? N21 C22 . . 1.381(8) ? N21 C25 . . 1.399(8) ? C22 N23 . . 1.370(7) ? N23 C24 . . 1.401(8) ? N23 C2 . . 1.468(8) ? C24 C25 . . 1.363(9) ? C24 H24 . . .967 ? C25 H25 . . .956 ? C2 C33 . . 1.515(9) ? C2 H2a . . .950 ? C2 H2b . . .961 ? C31 N32 . . 1.343(8) ? C31 C36 . . 1.393(8) ? C31 C3 . . 1.522(7) ? N32 C33 . . 1.362(6) ? C33 C34 . . 1.397(7) ? C34 C35 . . 1.387(10) ? C34 H34 . . .959 ? C35 C36 . . 1.412(8) ? C35 H35 . . .956 ? C36 H36 . . .972 ? C3 N41 . . 1.481(8) ? C3 H3a . . .957 ? C3 H3b . . .962 ? N41 C42 . . 1.364(7) ? N41 C45 . . 1.393(8) ? C42 N43 . . 1.356(7) ? N43 C44 . . 1.395(7) ? N43 C4 . . 1.480(7) ? C44 C45 . . 1.347(9) ? C44 H44 . . .954 ? C45 H45 . . .966 ? C4 H4a . . .959 ? C4 H4b . . .959 ? O01 H01a . . .927 ? O01 H01b . . .925 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C22 Au C42 . . '2 666' 175.7(2) ? N12 C11 C16 . . . 123.0(5) ? N12 C11 C1 . . . 117.9(5) ? C16 C11 C1 . . . 119.0(6) ? C11 N12 C13 . . . 117.4(5) ? N12 C13 C14 . . . 123.2(6) ? N12 C13 C4 . . . 117.6(5) ? C14 C13 C4 . . . 119.2(5) ? C13 C14 C15 . . . 119.2(5) ? C13 C14 H14 . . . 120.1 ? C15 C14 H14 . . . 120.7 ? C14 C15 C16 . . . 117.8(5) ? C14 C15 H15 . . . 121.7 ? C16 C15 H15 . . . 120.5 ? C11 C16 C15 . . . 119.5(6) ? C11 C16 H16 . . . 120.1 ? C15 C16 H16 . . . 120.5 ? C11 C1 N21 . . . 114.3(5) ? C11 C1 H1a . . . 109.1 ? C11 C1 H1b . . . 109.0 ? N21 C1 H1a . . . 108.4 ? N21 C1 H1b . . . 108.0 ? H1a C1 H1b . . . 107.8 ? C1 N21 C22 . . . 124.7(5) ? C1 N21 C25 . . . 124.3(5) ? C22 N21 C25 . . . 111.0(5) ? Au C22 N21 . . . 127.1(4) ? Au C22 N23 . . . 127.9(4) ? N21 C22 N23 . . . 104.7(5) ? C22 N23 C24 . . . 110.5(5) ? C22 N23 C2 . . . 125.2(5) ? C24 N23 C2 . . . 124.3(5) ? N23 C24 C25 . . . 107.5(5) ? N23 C24 H24 . . . 125.8 ? C25 C24 H24 . . . 126.7 ? N21 C25 C24 . . . 106.3(5) ? N21 C25 H25 . . . 126.2 ? C24 C25 H25 . . . 127.5 ? N23 C2 C33 . . . 112.3(5) ? N23 C2 H2a . . . 109.1 ? N23 C2 H2b . . . 108.3 ? C33 C2 H2a . . . 109.5 ? C33 C2 H2b . . . 109.0 ? H2a C2 H2b . . . 108.5 ? N32 C31 C36 . . . 123.4(5) ? N32 C31 C3 . . . 115.8(5) ? C36 C31 C3 . . . 120.7(6) ? C31 N32 C33 . . . 117.7(5) ? C2 C33 N32 . . . 116.0(4) ? C2 C33 C34 . . . 121.1(4) ? N32 C33 C34 . . . 122.9(5) ? C33 C34 C35 . . . 118.8(5) ? C33 C34 H34 . . . 120.4 ? C35 C34 H34 . . . 120.8 ? C34 C35 C36 . . . 118.9(5) ? C34 C35 H35 . . . 120.9 ? C36 C35 H35 . . . 120.2 ? C31 C36 C35 . . . 118.4(6) ? C31 C36 H36 . . . 120.5 ? C35 C36 H36 . . . 121.1 ? C31 C3 N41 . . . 111.8(5) ? C31 C3 H3a . . . 109.7 ? C31 C3 H3b . . . 109.1 ? N41 C3 H3a . . . 109.4 ? N41 C3 H3b . . . 109.0 ? H3a C3 H3b . . . 107.9 ? C3 N41 C42 . . . 124.7(5) ? C3 N41 C45 . . . 125.1(4) ? C42 N41 C45 . . . 110.3(5) ? N41 C42 N43 . . . 104.5(5) ? N41 C42 Au . . '2 666' 127.3(4) ? N43 C42 Au . . '2 666' 128.0(4) ? C42 N43 C44 . . . 111.8(5) ? C42 N43 C4 . . . 124.7(5) ? C44 N43 C4 . . . 123.5(5) ? N43 C44 C45 . . . 105.7(5) ? N43 C44 H44 . . . 126.9 ? C45 C44 H44 . . . 127.5 ? N41 C45 C44 . . . 107.8(5) ? N41 C45 H45 . . . 125.9 ? C44 C45 H45 . . . 126.3 ? C13 C4 N43 . . . 112.8(4) ? C13 C4 H4a . . . 109.5 ? C13 C4 H4b . . . 109.1 ? N43 C4 H4a . . . 108.5 ? N43 C4 H4b . . . 108.7 ? H4a C4 H4b . . . 108.0 ? H01a O01 H01b . . . 110.0 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 608 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min -15 _reflns_limit_l_max 14 _reflns_number_observed ? _reflns_d_resolution_high .769 _reflns_d_resolution_low 10.767 _diffrn_reflns_av_sigmaI/netI .05 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .039 _refine_ls_wR_factor_all .042 _refine_ls_goodness_of_fit_all .995 _refine_ls_shift/su_mean .0002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_p1130 _database_code_depnum_ccdc_archive 'CCDC 227415' _audit_creation_method Xtal3.6 _audit_creation_date 03-05-07 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C32 H44 Au2 Br2 N8 O4' _chemical_formula_moiety 'C32 H36 Au2 N8, 4(H2 O), 2(Br)' _chemical_formula_weight 1158.5 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.6088(6) _cell_length_b 8.4127(5) _cell_length_c 19.9930(10) _cell_angle_alpha 90.00000 _cell_angle_beta 101.0040(10) _cell_angle_gamma 90.00000 _cell_volume 1916.64(18) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 10026 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 37.53 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 9.776 _exptl_crystal_description bar _exptl_crystal_size_max .19 _exptl_crystal_size_mid .09 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .50 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 40102 _reflns_number_total 8228 _reflns_Friedel_coverage 0 _reflns_number_gt 6097 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 34.65 _diffrn_reflns_theta_full 34.65 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .063 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .044 _refine_ls_wR_factor_ref .062 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_number_reflns 6097 _refine_ls_number_parameters 217 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .005 _refine_diff_density_min -3.252 _refine_diff_density_max 3.675 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 64 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 88 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 4 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 4 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 8 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .459034(16) .77573(3) .488363(10) .01828(9) Uani ? ? 1.00000 ? ? Br .09504(6) .43254(9) .70373(3) .0373(3) Uani ? ? 1.00000 ? ? C1 .3008(6) .7352(9) .6178(3) .034(3) Uani ? ? 1.00000 ? ? N21 .2401(4) .7157(6) .5477(3) .024(2) Uani ? ? 1.00000 ? ? C22 .2896(5) .7312(7) .4919(3) .019(2) Uani ? ? 1.00000 ? ? N23 .2002(4) .7085(5) .4383(2) .0186(18) Uani ? ? 1.00000 ? ? C24 .0962(5) .6773(8) .4604(3) .027(2) Uani ? ? 1.00000 ? ? C25 .1221(5) .6816(9) .5290(3) .032(3) Uani ? ? 1.00000 ? ? C2 .2122(5) .7077(6) .3674(3) .021(2) Uani ? ? 1.00000 ? ? C31 .3157(5) .2807(6) .3613(3) .019(2) Uani ? ? 1.00000 ? ? C32 .2610(5) .4172(7) .3795(3) .020(2) Uani ? ? 1.00000 ? ? C33 .2735(4) .5618(6) .3479(2) .0170(19) Uani ? ? 1.00000 ? ? C34 .3410(5) .5688(7) .2977(3) .022(2) Uani ? ? 1.00000 ? ? C35 .3958(5) .4347(8) .2799(3) .025(2) Uani ? ? 1.00000 ? ? C36 .3844(5) .2904(7) .3115(3) .022(2) Uani ? ? 1.00000 ? ? C3 .2982(5) .1232(7) .3944(3) .023(2) Uani ? ? 1.00000 ? ? N41 .2838(4) .1387(5) .4643(2) .0197(18) Uani ? ? 1.00000 ? ? C42 .3720(4) .1797(7) .5170(3) .020(2) Uani ? ? 1.00000 ? ? N43 .3205(4) .1872(7) .5718(3) .026(2) Uani ? ? 1.00000 ? ? C44 .2032(5) .1488(9) .5538(3) .031(3) Uani ? ? 1.00000 ? ? C45 .1803(5) .1184(8) .4869(3) .026(2) Uani ? ? 1.00000 ? ? C4 .3815(7) .2302(10) .6405(3) .038(3) Uani ? ? 1.00000 ? ? O01 .9871(4) .8079(7) .6616(3) .040(3) Uani ? ? 1.00000 ? ? O02 .6513(4) .4551(7) .2091(3) .037(2) Uani ? ? 1.00000 ? ? H1a .30394 .84658 .62912 .05200 Uiso ? ? 1.00000 ? ? H1b .37848 .69619 .62287 .05200 Uiso ? ? 1.00000 ? ? H1c .26007 .68103 .64762 .05200 Uiso ? ? 1.00000 ? ? H4a .46134 .25514 .64039 .05700 Uiso ? ? 1.00000 ? ? H4b .34480 .31996 .65689 .05700 Uiso ? ? 1.00000 ? ? H4c .37922 .14329 .67060 .05700 Uiso ? ? 1.00000 ? ? H01a 1.01022 .71154 .68207 .06100 Uiso ? ? 1.00000 ? ? H01b 1.03399 .88829 .68310 .06100 Uiso ? ? 1.00000 ? ? H02a .59719 .37236 .20481 .05500 Uiso ? ? 1.00000 ? ? H02b .69752 .43538 .25110 .05500 Uiso ? ? 1.00000 ? ? H24 .02143 .65698 .43263 .03300 Uiso ? ? 1.00000 ? ? H25 .06895 .66414 .55909 .03900 Uiso ? ? 1.00000 ? ? H2a .25576 .79884 .35911 .02700 Uiso ? ? 1.00000 ? ? H2b .13598 .71246 .33961 .02700 Uiso ? ? 1.00000 ? ? H32 .21456 .41129 .41382 .02400 Uiso ? ? 1.00000 ? ? H34 .34938 .66695 .27544 .02700 Uiso ? ? 1.00000 ? ? H35 .44218 .44096 .24550 .03100 Uiso ? ? 1.00000 ? ? H36 .42331 .19838 .29914 .02800 Uiso ? ? 1.00000 ? ? H3a .36477 .05787 .39328 .02800 Uiso ? ? 1.00000 ? ? H3b .23014 .07345 .36889 .02800 Uiso ? ? 1.00000 ? ? H44 .14841 .14429 .58369 .03900 Uiso ? ? 1.00000 ? ? H45 .10656 .08855 .46020 .03300 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .01418(9) .02103(10) .01969(10) .00034(7) .00339(6) .00085(7) Br .0339(3) .0419(4) .0334(3) -.0059(3) -.0006(3) -.0009(3) C1 .026(3) .055(4) .020(3) -.003(3) .003(2) -.005(3) N21 .017(2) .035(3) .022(2) .0021(18) .0058(16) -.0030(18) C22 .018(2) .019(2) .022(2) .0013(18) .0044(17) -.0006(18) N23 .0160(18) .018(2) .022(2) .0000(14) .0031(15) -.0042(15) C24 .015(2) .039(3) .028(3) -.004(2) .0049(19) -.006(2) C25 .023(3) .048(4) .027(3) -.005(3) .009(2) -.002(3) C2 .027(2) .016(3) .022(2) -.0011(18) .007(2) .0011(17) C31 .017(2) .020(2) .020(2) .0008(18) .0017(17) -.0021(18) C32 .020(2) .023(2) .017(2) .0002(18) .0068(17) .0001(17) C33 .018(2) .019(2) .0136(19) -.0019(17) .0007(15) -.0007(16) C34 .021(2) .029(3) .015(2) -.004(2) .0024(17) .0010(18) C35 .020(2) .039(3) .016(2) -.000(2) .0052(18) -.001(2) C36 .019(2) .026(3) .022(2) .0028(18) .0038(18) -.0053(19) C3 .026(2) .015(2) .027(2) -.0001(19) .003(2) -.0022(19) N41 .0158(18) .018(2) .025(2) -.0009(15) .0025(15) .0031(16) C42 .017(2) .022(2) .022(2) .0013(18) .0056(17) .0042(19) N43 .017(2) .037(3) .024(2) -.0048(19) .0036(17) .004(2) C44 .020(2) .046(4) .029(3) -.004(2) .009(2) .007(3) C45 .016(2) .032(3) .029(3) -.004(2) .003(2) .005(2) C4 .033(3) .060(5) .021(3) -.017(3) .006(2) -.000(3) O01 .028(2) .050(3) .039(3) .003(2) -.003(2) -.003(2) O02 .029(2) .043(3) .039(3) .005(2) .004(2) .003(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C22 . . 2.017(6) ? Au C42 . '3 666' 2.019(5) ? C1 N21 . . 1.454(8) ? C1 H1a . . .963 ? C1 H1b . . .947 ? C1 H1c . . .946 ? N21 C22 . . 1.354(8) ? N21 C25 . . 1.379(8) ? C22 N23 . . 1.355(7) ? N23 C24 . . 1.388(8) ? N23 C2 . . 1.451(8) ? C24 C25 . . 1.348(9) ? C24 H24 . . .952 ? C25 H25 . . .952 ? C2 C33 . . 1.506(8) ? C2 H2a . . .950 ? C2 H2b . . .952 ? C31 C32 . . 1.393(8) ? C31 C36 . . 1.393(8) ? C31 C3 . . 1.512(8) ? C32 C33 . . 1.391(8) ? C32 H32 . . .952 ? C33 C34 . . 1.387(8) ? C34 C35 . . 1.375(9) ? C34 H34 . . .952 ? C35 C36 . . 1.386(9) ? C35 H35 . . .952 ? C36 H36 . . .952 ? C3 N41 . . 1.445(8) ? C3 H3a . . .952 ? C3 H3b . . .951 ? N41 C42 . . 1.366(6) ? N41 C45 . . 1.373(8) ? C42 N43 . . 1.346(8) ? N43 C44 . . 1.379(8) ? N43 C4 . . 1.466(8) ? C44 C45 . . 1.338(9) ? C44 H44 . . .952 ? C45 H45 . . .952 ? C4 H4a . . .951 ? C4 H4b . . .955 ? C4 H4c . . .951 ? O01 H01a . . .924 ? O01 H01b . . .921 ? O02 H02a . . .931 ? O02 H02b . . .921 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C22 Au C42 . . '3 666' 179.0(2) ? N21 C1 H1a . . . 109.0 ? N21 C1 H1b . . . 109.9 ? N21 C1 H1c . . . 110.2 ? H1a C1 H1b . . . 108.7 ? H1a C1 H1c . . . 108.8 ? H1b C1 H1c . . . 110.2 ? C1 N21 C22 . . . 125.4(5) ? C1 N21 C25 . . . 123.9(6) ? C22 N21 C25 . . . 110.7(5) ? Au C22 N21 . . . 128.1(4) ? Au C22 N23 . . . 127.1(4) ? N21 C22 N23 . . . 104.9(5) ? C22 N23 C24 . . . 110.8(5) ? C22 N23 C2 . . . 124.9(5) ? C24 N23 C2 . . . 124.2(4) ? N23 C24 C25 . . . 106.3(5) ? N23 C24 H24 . . . 126.8 ? C25 C24 H24 . . . 126.9 ? N21 C25 C24 . . . 107.4(6) ? N21 C25 H25 . . . 126.3 ? C24 C25 H25 . . . 126.4 ? N23 C2 C33 . . . 113.2(4) ? N23 C2 H2a . . . 108.6 ? N23 C2 H2b . . . 108.5 ? C33 C2 H2a . . . 108.6 ? C33 C2 H2b . . . 108.5 ? H2a C2 H2b . . . 109.3 ? C32 C31 C36 . . . 119.3(5) ? C32 C31 C3 . . . 120.2(5) ? C36 C31 C3 . . . 120.5(5) ? C31 C32 C33 . . . 120.7(5) ? C31 C32 H32 . . . 119.6 ? C33 C32 H32 . . . 119.7 ? C2 C33 C32 . . . 120.0(5) ? C2 C33 C34 . . . 120.8(5) ? C32 C33 C34 . . . 119.2(5) ? C33 C34 C35 . . . 120.4(5) ? C33 C34 H34 . . . 119.8 ? C35 C34 H34 . . . 119.8 ? C34 C35 C36 . . . 120.8(6) ? C34 C35 H35 . . . 119.6 ? C36 C35 H35 . . . 119.6 ? C31 C36 C35 . . . 119.6(5) ? C31 C36 H36 . . . 120.2 ? C35 C36 H36 . . . 120.2 ? C31 C3 N41 . . . 113.2(5) ? C31 C3 H3a . . . 108.6 ? C31 C3 H3b . . . 108.6 ? N41 C3 H3a . . . 108.6 ? N41 C3 H3b . . . 108.7 ? H3a C3 H3b . . . 109.2 ? C3 N41 C42 . . . 124.1(5) ? C3 N41 C45 . . . 125.3(4) ? C42 N41 C45 . . . 110.6(5) ? N41 C42 N43 . . . 104.8(5) ? N41 C42 Au . . '3 666' 126.8(4) ? N43 C42 Au . . '3 666' 128.4(4) ? C42 N43 C44 . . . 110.4(5) ? C42 N43 C4 . . . 124.3(5) ? C44 N43 C4 . . . 125.3(6) ? N43 C44 C45 . . . 107.6(6) ? N43 C44 H44 . . . 126.2 ? C45 C44 H44 . . . 126.2 ? N41 C45 C44 . . . 106.6(5) ? N41 C45 H45 . . . 126.7 ? C44 C45 H45 . . . 126.7 ? N43 C4 H4a . . . 110.4 ? N43 C4 H4b . . . 110.4 ? N43 C4 H4c . . . 109.7 ? H4a C4 H4b . . . 109.0 ? H4a C4 H4c . . . 108.4 ? H4b C4 H4c . . . 108.8 ? H01a O01 H01b . . . 110.0 ? H02a O02 H02b . . . 102.4 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1104 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -31 _reflns_limit_l_max 31 _reflns_number_observed ? _reflns_d_resolution_high .625 _reflns_d_resolution_low 10.766 _diffrn_reflns_av_sigmaI/netI .076 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .071 _refine_ls_wR_factor_all .068 _refine_ls_goodness_of_fit_all .987 _refine_ls_shift/su_mean .0001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_p128 _database_code_depnum_ccdc_archive 'CCDC 227416' _audit_creation_method Xtal3.6 _audit_creation_date 03-05-08 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C30 H34 Au2 Br2 N10' _chemical_formula_moiety 'C30 H34 Au2 N10, 2(Br)' _chemical_formula_weight 1088.41 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 8.2070(10) _cell_length_b 10.8870(10) _cell_length_c 11.2330(10) _cell_angle_alpha 113.735(3) _cell_angle_beta 102.869(3) _cell_angle_gamma 100.632(3) _cell_volume 852.38(15) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 2.12 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 3669 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 33.8 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 10.977 _exptl_crystal_description blade _exptl_crystal_size_max .12 _exptl_crystal_size_mid .09 _exptl_crystal_size_min .02 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .63 _exptl_absorpt_correction_T_max 1.0 _diffrn_reflns_number 14290 _reflns_number_total 5990 _reflns_Friedel_coverage 0 _reflns_number_gt 4261 _reflns_threshold_expression 'F > .00 sig(F )' _diffrn_reflns_theta_max 32.21 _diffrn_reflns_theta_full 32.1 _diffrn_measured_fraction_theta_max .99 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .068 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .053 _refine_ls_wR_factor_ref .058 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_number_reflns 4261 _refine_ls_number_parameters 199 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .002 _refine_diff_density_min -2.743 _refine_diff_density_max 3.462 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 30 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 34 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 2 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 2 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 10 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au .75120(4) .51219(3) .46801(4) .01933(12) Uani ? ? 1.00000 ? ? Br .82305(12) .81128(10) .18286(10) .0300(4) Uani ? ? 1.00000 ? ? C1 .8364(15) .5755(12) .8051(12) .042(5) Uani ? ? 1.00000 ? ? N21 .8169(10) .6929(8) .7735(8) .025(3) Uani ? ? 1.00000 ? ? C22 .7893(10) .6823(9) .6476(9) .021(3) Uani ? ? 1.00000 ? ? N23 .7942(9) .8139(7) .6652(8) .020(3) Uani ? ? 1.00000 ? ? C24 .8242(11) .9035(9) .8016(10) .026(3) Uani ? ? 1.00000 ? ? C25 .8397(12) .8268(10) .8722(10) .030(4) Uani ? ? 1.00000 ? ? C2 .7563(11) .8527(9) .5545(10) .023(3) Uani ? ? 1.00000 ? ? C31 .2938(11) .8086(9) .5258(10) .024(3) Uani ? ? 1.00000 ? ? N32 .4667(9) .8311(7) .5784(8) .021(3) Uani ? ? 1.00000 ? ? C33 .5628(10) .8321(9) .4969(10) .022(3) Uani ? ? 1.00000 ? ? C34 .4949(11) .8147(10) .3639(10) .026(3) Uani ? ? 1.00000 ? ? C35 .3145(12) .7948(10) .3110(10) .028(3) Uani ? ? 1.00000 ? ? C36 .2137(11) .7909(10) .3961(11) .030(4) Uani ? ? 1.00000 ? ? C3 .1828(11) .8115(10) .6182(10) .025(3) Uani ? ? 1.00000 ? ? N41 .2557(9) .7806(8) .7307(8) .022(3) Uani ? ? 1.00000 ? ? C42 .2874(10) .6560(9) .7122(9) .022(3) Uani ? ? 1.00000 ? ? N43 .3514(10) .6722(8) .8420(8) .026(3) Uani ? ? 1.00000 ? ? C44 .3618(13) .8028(11) .9377(10) .034(4) Uani ? ? 1.00000 ? ? C45 .3014(13) .8721(10) .8689(11) .033(4) Uani ? ? 1.00000 ? ? C4 .3961(14) .5628(11) .8745(11) .037(4) Uani ? ? 1.00000 ? ? H1a .82915 .59499 .89439 .06300 Uiso ? ? 1.00000 ? ? H1b .94472 .55792 .80100 .06300 Uiso ? ? 1.00000 ? ? H1c .74253 .49204 .74090 .06300 Uiso ? ? 1.00000 ? ? H24 .83277 1.00169 .83924 .03000 Uiso ? ? 1.00000 ? ? H25 .86159 .85860 .96855 .03800 Uiso ? ? 1.00000 ? ? H2a .79373 .79581 .48120 .03000 Uiso ? ? 1.00000 ? ? H2b .82082 .94924 .58770 .03000 Uiso ? ? 1.00000 ? ? H34 .56904 .81580 .30919 .03300 Uiso ? ? 1.00000 ? ? H35 .26222 .78206 .21917 .03500 Uiso ? ? 1.00000 ? ? H36 .08973 .77764 .36517 .03700 Uiso ? ? 1.00000 ? ? H3a .06868 .74306 .56233 .03100 Uiso ? ? 1.00000 ? ? H3b .16670 .90243 .65692 .03100 Uiso ? ? 1.00000 ? ? H44 .40507 .83798 1.03553 .04300 Uiso ? ? 1.00000 ? ? H45 .29102 .96563 .90788 .04200 Uiso ? ? 1.00000 ? ? H4a .51353 .59703 .93744 .05700 Uiso ? ? 1.00000 ? ? H4b .38801 .48213 .79290 .05700 Uiso ? ? 1.00000 ? ? H4c .31891 .53335 .91642 .05700 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .01710(15) .01580(15) .02535(18) .00422(10) .00867(11) .00925(12) Br .0279(4) .0331(5) .0306(5) .0074(4) .0096(4) .0170(4) C1 .052(7) .042(7) .045(7) .015(5) .021(5) .031(6) N21 .028(4) .024(4) .028(4) .008(3) .011(3) .014(3) C22 .017(4) .020(4) .028(5) .007(3) .009(3) .010(4) N23 .016(3) .020(4) .029(4) .008(3) .013(3) .012(3) C24 .022(4) .021(4) .029(5) .006(3) .011(4) .006(4) C25 .029(5) .027(5) .030(5) .007(4) .008(4) .011(4) C2 .020(4) .021(4) .035(5) .009(3) .016(4) .017(4) C31 .018(4) .021(4) .038(5) .008(3) .012(4) .015(4) N32 .017(3) .021(4) .032(4) .009(3) .011(3) .015(3) C33 .016(4) .016(4) .039(5) .006(3) .016(3) .014(4) C34 .026(4) .027(5) .039(5) .009(3) .021(4) .021(4) C35 .035(5) .027(5) .033(5) .008(4) .009(4) .027(4) C36 .018(4) .026(5) .049(6) .010(3) .011(4) .021(4) C3 .015(4) .029(5) .035(5) .011(3) .010(3) .015(4) N41 .018(3) .022(4) .029(4) .007(3) .014(3) .010(3) C42 .018(4) .024(5) .022(4) .001(3) .007(3) .011(4) N43 .028(4) .023(4) .026(4) .000(3) .009(3) .012(3) C44 .032(5) .033(6) .028(5) -.000(4) .010(4) .011(4) C45 .039(5) .024(5) .034(5) .004(4) .023(4) .007(4) C4 .042(6) .034(6) .033(6) .001(4) .008(4) .020(5) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au C22 . . 2.024(8) ? Au C42 . '2 666' 2.017(8) ? C1 N21 . . 1.484(18) ? C1 H1a . . .957 ? C1 H1b . . .950 ? C1 H1c . . .952 ? N21 C22 . . 1.334(14) ? N21 C25 . . 1.376(12) ? C22 N23 . . 1.357(13) ? N23 C24 . . 1.378(12) ? N23 C2 . . 1.457(15) ? C24 C25 . . 1.368(18) ? C24 H24 . . .960 ? C25 H25 . . .955 ? C2 C33 . . 1.511(12) ? C2 H2a . . .963 ? C2 H2b . . .956 ? C31 N32 . . 1.343(11) ? C31 C36 . . 1.376(16) ? C31 C3 . . 1.521(16) ? N32 C33 . . 1.337(14) ? C33 C34 . . 1.394(16) ? C34 C35 . . 1.407(13) ? C34 H34 . . .958 ? C35 C36 . . 1.404(17) ? C35 H35 . . .966 ? C36 H36 . . .961 ? C3 N41 . . 1.466(15) ? C3 H3a . . .965 ? C3 H3b . . .955 ? N41 C42 . . 1.371(14) ? N41 C45 . . 1.378(12) ? C42 N43 . . 1.360(13) ? N43 C44 . . 1.367(12) ? N43 C4 . . 1.462(17) ? C44 C45 . . 1.361(19) ? C44 H44 . . .958 ? C45 H45 . . .962 ? C4 H4a . . .959 ? C4 H4b . . .959 ? C4 H4c . . .951 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C22 Au C42 . . '2 666' 179.3(5) ? N21 C1 H1a . . . 111.1 ? N21 C1 H1b . . . 111.7 ? N21 C1 H1c . . . 109.6 ? H1a C1 H1b . . . 108.9 ? H1a C1 H1c . . . 106.5 ? H1b C1 H1c . . . 108.9 ? C1 N21 C22 . . . 123.2(8) ? C1 N21 C25 . . . 123.6(10) ? C22 N21 C25 . . . 113.0(10) ? Au C22 N21 . . . 129.2(8) ? Au C22 N23 . . . 126.3(8) ? N21 C22 N23 . . . 104.5(7) ? C22 N23 C24 . . . 110.4(9) ? C22 N23 C2 . . . 125.1(7) ? C24 N23 C2 . . . 124.3(8) ? N23 C24 C25 . . . 107.4(8) ? N23 C24 H24 . . . 125.8 ? C25 C24 H24 . . . 126.8 ? N21 C25 C24 . . . 104.7(9) ? N21 C25 H25 . . . 127.4 ? C24 C25 H25 . . . 127.9 ? N23 C2 C33 . . . 112.0(9) ? N23 C2 H2a . . . 109.3 ? N23 C2 H2b . . . 109.7 ? C33 C2 H2a . . . 108.7 ? C33 C2 H2b . . . 109.1 ? H2a C2 H2b . . . 107.9 ? N32 C31 C36 . . . 123.7(10) ? N32 C31 C3 . . . 117.9(9) ? C36 C31 C3 . . . 118.3(8) ? C31 N32 C33 . . . 117.0(9) ? C2 C33 N32 . . . 117.0(9) ? C2 C33 C34 . . . 119.0(10) ? N32 C33 C34 . . . 124.0(8) ? C33 C34 C35 . . . 118.6(10) ? C33 C34 H34 . . . 120.9 ? C35 C34 H34 . . . 120.5 ? C34 C35 C36 . . . 117.1(10) ? C34 C35 H35 . . . 121.1 ? C36 C35 H35 . . . 121.7 ? C31 C36 C35 . . . 119.6(9) ? C31 C36 H36 . . . 119.8 ? C35 C36 H36 . . . 120.6 ? C31 C3 N41 . . . 114.9(8) ? C31 C3 H3a . . . 108.6 ? C31 C3 H3b . . . 108.9 ? N41 C3 H3a . . . 108.0 ? N41 C3 H3b . . . 108.5 ? H3a C3 H3b . . . 107.8 ? C3 N41 C42 . . . 124.3(7) ? C3 N41 C45 . . . 124.9(9) ? C42 N41 C45 . . . 110.8(9) ? N41 C42 N43 . . . 104.5(7) ? N41 C42 Au . . '2 666' 127.3(7) ? N43 C42 Au . . '2 666' 128.2(8) ? C42 N43 C44 . . . 110.8(10) ? C42 N43 C4 . . . 124.6(8) ? C44 N43 C4 . . . 124.6(9) ? N43 C44 C45 . . . 107.7(9) ? N43 C44 H44 . . . 125.3 ? C45 C44 H44 . . . 126.9 ? N41 C45 C44 . . . 106.1(9) ? N41 C45 H45 . . . 126.5 ? C44 C45 H45 . . . 127.4 ? N43 C4 H4a . . . 111.0 ? N43 C4 H4b . . . 110.9 ? N43 C4 H4c . . . 110.6 ? H4a C4 H4b . . . 108.0 ? H4a C4 H4c . . . 107.7 ? H4b C4 H4c . . . 108.5 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 512 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min -16 _reflns_limit_l_max 16 _reflns_number_observed ? _reflns_d_resolution_high .667 _reflns_d_resolution_low 9.688 _diffrn_reflns_av_sigmaI/netI .123 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .089 _refine_ls_wR_factor_all .063 _refine_ls_goodness_of_fit_all 1.066 _refine_ls_shift/su_mean .00008 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_p11p23 _database_code_depnum_ccdc_archive 'CCDC 227417' _audit_creation_method Xtal3.6 _audit_creation_date 02-08-30 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C18 H24 Au2 I2 N8' _chemical_formula_moiety 'C18 H24 Au2 N8, 2(I)' _chemical_formula_weight 1000.19 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 7.7760(10) _cell_length_b 12.487(2) _cell_length_c 13.911(2) _cell_angle_alpha 69.544(3) _cell_angle_beta 81.978(3) _cell_angle_gamma 88.246(3) _cell_volume 1252.9(3) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.651 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4804 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 34.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 14.181 _exptl_crystal_description prism _exptl_crystal_size_max .15 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .07 _exptl_crystal_size_rad ? _exptl_crystal_colour dark _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .57 _exptl_absorpt_correction_T_max .86 _diffrn_reflns_number 25855 _reflns_number_total 12877 _reflns_Friedel_coverage 0 _reflns_number_gt 7646 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.7 _diffrn_reflns_theta_full 37.2 _diffrn_measured_fraction_theta_max .96 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .055 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .049 _refine_ls_wR_factor_ref .047 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_number_reflns 7646 _refine_ls_number_parameters 271 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .009 _refine_diff_density_min -4.026 _refine_diff_density_max 3.061 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 36 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 48 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 4 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' I ? 0 4 -.726 1.812 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au1 .48644(4) .62578(2) .34612(2) .01968(19) Uani ? ? 1.00000 ? ? Au2 .70789(4) .72087(2) .08970(2) .0221(2) Uani ? ? 1.00000 ? ? I1 .11716(6) .65581(4) .23080(4) .0219(3) Uani ? ? 1.00000 ? ? I2 .99275(7) 1.12443(4) .32295(4) .0264(4) Uani ? ? 1.00000 ? ? C11 .4804(9) .4589(6) .3602(5) .019(5) Uani ? ? 1.00000 ? ? N12 .6035(8) .3979(5) .3221(5) .019(4) Uani ? ? 1.00000 ? ? C13 .5454(11) .2864(6) .3470(6) .026(5) Uani ? ? 1.00000 ? ? C14 .3894(11) .2768(7) .4026(7) .029(6) Uani ? ? 1.00000 ? ? N15 .3510(8) .3830(5) .4094(5) .023(4) Uani ? ? 1.00000 ? ? C151 .1934(10) .4093(8) .4694(6) .033(6) Uani ? ? 1.00000 ? ? C1 .7701(9) .4447(6) .2599(6) .021(5) Uani ? ? 1.00000 ? ? C11' .7228(10) .5622(6) .0799(6) .022(5) Uani ? ? 1.00000 ? ? N12' .7655(9) .4637(5) .1511(5) .022(4) Uani ? ? 1.00000 ? ? C13' .7970(12) .3789(7) .1080(7) .033(7) Uani ? ? 1.00000 ? ? C14' .7738(13) .4260(7) .0079(6) .035(7) Uani ? ? 1.00000 ? ? N15' .7285(9) .5382(6) -.0077(5) .028(5) Uani ? ? 1.00000 ? ? C151' .6938(14) .6208(8) -.1089(7) .039(7) Uani ? ? 1.00000 ? ? C21 .4845(10) .7854(6) .3530(5) .020(5) Uani ? ? 1.00000 ? ? N22 .6116(8) .8667(5) .3219(5) .020(4) Uani ? ? 1.00000 ? ? C23 .5583(11) .9606(6) .3510(7) .027(6) Uani ? ? 1.00000 ? ? C24 .3930(11) .9362(7) .3988(6) .028(6) Uani ? ? 1.00000 ? ? N25 .3510(8) .8304(5) .3990(5) .021(4) Uani ? ? 1.00000 ? ? C251 .1841(10) .7744(8) .4455(7) .030(6) Uani ? ? 1.00000 ? ? C2 .7757(10) .8624(6) .2597(6) .021(5) Uani ? ? 1.00000 ? ? C21' .7296(10) .8857(6) .0799(6) .023(5) Uani ? ? 1.00000 ? ? N22' .7714(8) .9280(5) .1511(5) .020(4) Uani ? ? 1.00000 ? ? C23' .8015(12) 1.0434(7) .1092(7) .032(6) Uani ? ? 1.00000 ? ? C24' .7744(13) 1.0759(7) .0080(7) .034(6) Uani ? ? 1.00000 ? ? N25' .7297(9) .9785(5) -.0080(5) .026(5) Uani ? ? 1.00000 ? ? C251' .6952(12) .9774(7) -.1079(6) .032(6) Uani ? ? 1.00000 ? ? H13 .60682 .22768 .32837 .03200 Uiso ? ? 1.00000 ? ? H14 .31736 .20910 .43168 .03700 Uiso ? ? 1.00000 ? ? H151a .19424 .48977 .45772 .05000 Uiso ? ? 1.00000 ? ? H151b .19600 .36872 .54105 .05000 Uiso ? ? 1.00000 ? ? H151c .09061 .39065 .44741 .05000 Uiso ? ? 1.00000 ? ? H1a .85996 .39264 .28421 .02600 Uiso ? ? 1.00000 ? ? H1b .79510 .51572 .26767 .02600 Uiso ? ? 1.00000 ? ? H13' .82844 .30061 .14393 .04000 Uiso ? ? 1.00000 ? ? H14' .78447 .38963 -.04370 .04300 Uiso ? ? 1.00000 ? ? H151'a .60210 .59136 -.13272 .06100 Uiso ? ? 1.00000 ? ? H151'b .79530 .63150 -.15891 .06100 Uiso ? ? 1.00000 ? ? H151'c .65999 .69203 -.10276 .06100 Uiso ? ? 1.00000 ? ? H23 .62537 1.02821 .33970 .03300 Uiso ? ? 1.00000 ? ? H24 .31960 .98382 .42762 .03400 Uiso ? ? 1.00000 ? ? H251a .11968 .82114 .47833 .04500 Uiso ? ? 1.00000 ? ? H251b .20484 .70299 .49620 .04500 Uiso ? ? 1.00000 ? ? H251c .12206 .76615 .39343 .04500 Uiso ? ? 1.00000 ? ? H2a .80149 .78441 .26742 .02700 Uiso ? ? 1.00000 ? ? H2b .86640 .89203 .28410 .02700 Uiso ? ? 1.00000 ? ? H23' .83436 1.09210 .14463 .04000 Uiso ? ? 1.00000 ? ? H24' .78394 1.15212 -.04245 .04100 Uiso ? ? 1.00000 ? ? H251'a .75130 .91412 -.12137 .04800 Uiso ? ? 1.00000 ? ? H251'b .57418 .96674 -.10885 .04800 Uiso ? ? 1.00000 ? ? H251'c .73549 1.04570 -.16314 .04800 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au1 .01902(14) .01920(13) .02025(13) .00072(10) .00126(10) -.00770(10) Au2 .02474(15) .01931(13) .02125(14) .00275(11) -.00119(11) -.00671(11) I1 .0218(2) .0238(2) .0199(2) .00260(18) -.00228(17) -.00760(18) I2 .0250(3) .0290(3) .0265(2) .0059(2) -.0025(2) -.0122(2) C11 .017(3) .019(3) .019(3) -.002(3) -.007(3) -.002(3) N12 .018(3) .017(3) .021(3) .004(2) -.001(2) -.005(2) C13 .029(4) .016(3) .030(4) .002(3) .001(3) -.005(3) C14 .029(4) .019(4) .034(4) -.003(3) -.009(3) .000(3) N15 .018(3) .022(3) .021(3) .002(2) .001(2) .001(2) C151 .018(4) .041(5) .027(4) -.001(3) .008(3) -.001(4) C1 .018(3) .014(3) .028(4) .003(3) -.001(3) -.007(3) C11' .021(4) .022(3) .025(4) -.002(3) -.001(3) -.010(3) N12' .030(4) .018(3) .019(3) .005(2) -.001(2) -.007(2) C13' .045(5) .024(4) .033(4) .004(4) -.002(4) -.014(4) C14' .054(6) .027(4) .023(4) -.004(4) .006(4) -.013(3) N15' .037(4) .031(4) .015(3) -.003(3) .000(3) -.009(3) C151' .058(6) .033(5) .022(4) .001(4) -.007(4) -.003(4) C21 .022(4) .022(3) .018(3) .001(3) -.003(3) -.009(3) N22 .020(3) .018(3) .020(3) .002(2) .000(2) -.006(2) C23 .030(4) .020(3) .034(4) .001(3) .003(3) -.015(3) C24 .038(5) .027(4) .028(4) .007(3) -.005(3) -.019(3) N25 .017(3) .025(3) .025(3) .003(2) -.002(2) -.014(3) C251 .018(4) .047(5) .031(4) -.003(3) .004(3) -.024(4) C2 .021(4) .021(3) .020(3) .000(3) -.000(3) -.005(3) C21' .023(4) .021(3) .019(3) .000(3) .003(3) -.003(3) N22' .021(3) .016(3) .021(3) .000(2) .000(2) -.007(2) C23' .039(5) .023(4) .030(4) -.009(3) .006(4) -.009(3) C24' .051(6) .019(4) .027(4) -.002(4) .003(4) -.005(3) N25' .032(4) .022(3) .018(3) .007(3) .003(3) -.002(3) C251' .044(5) .030(4) .020(4) .003(4) -.000(3) -.006(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au1 C11 . . 2.024(8) ? Au1 C21 . . 2.028(8) ? Au2 C11' . . 2.032(9) ? Au2 C21' . . 2.025(8) ? C11 N12 . . 1.368(10) ? C11 N15 . . 1.339(9) ? N12 C13 . . 1.386(10) ? N12 C1 . . 1.466(9) ? C13 C14 . . 1.329(11) ? C13 H13 . . .954 ? C14 N15 . . 1.384(11) ? C14 H14 . . .958 ? N15 C151 . . 1.480(11) ? C151 H151a . . .960 ? C151 H151b . . .950 ? C151 H151c . . .958 ? C1 N12' . . 1.453(11) ? C1 H1a . . .954 ? C1 H1b . . .959 ? C11' N12' . . 1.349(9) ? C11' N15' . . 1.348(12) ? N12' C13' . . 1.387(13) ? C13' C14' . . 1.345(12) ? C13' H13' . . .971 ? C14' N15' . . 1.383(12) ? C14' H14' . . .969 ? N15' C151' . . 1.480(10) ? C151' H151'a . . .960 ? C151' H151'b . . .956 ? C151' H151'c . . .948 ? C21 N22 . . 1.352(10) ? C21 N25 . . 1.354(10) ? N22 C23 . . 1.403(11) ? N22 C2 . . 1.449(9) ? C23 C24 . . 1.353(12) ? C23 H23 . . .959 ? C24 N25 . . 1.370(12) ? C24 H24 . . .960 ? N25 C251 . . 1.447(10) ? C251 H251a . . .951 ? C251 H251b . . .950 ? C251 H251c . . .960 ? C2 N22' . . 1.449(9) ? C2 H2a . . .960 ? C2 H2b . . .959 ? C21' N22' . . 1.353(12) ? C21' N25' . . 1.359(8) ? N22' C23' . . 1.366(10) ? C23' C24' . . 1.367(13) ? C23' H23' . . .965 ? C24' N25' . . 1.373(12) ? C24' H24' . . .963 ? N25' C251' . . 1.457(12) ? C251' H251'a . . .953 ? C251' H251'b . . .957 ? C251' H251'c . . .952 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C11 Au1 C21 . . . 172.3(3) ? C11' Au2 C21' . . . 170.0(3) ? Au1 C11 N12 . . . 128.9(5) ? Au1 C11 N15 . . . 126.9(6) ? N12 C11 N15 . . . 104.2(6) ? C11 N12 C13 . . . 110.4(6) ? C11 N12 C1 . . . 125.1(6) ? C13 N12 C1 . . . 124.5(7) ? N12 C13 C14 . . . 107.0(7) ? N12 C13 H13 . . . 126.3 ? C14 C13 H13 . . . 126.7 ? C13 C14 N15 . . . 106.9(7) ? C13 C14 H14 . . . 126.3 ? N15 C14 H14 . . . 126.8 ? C11 N15 C14 . . . 111.6(6) ? C11 N15 C151 . . . 123.2(7) ? C14 N15 C151 . . . 125.0(6) ? N15 C151 H151a . . . 108.5 ? N15 C151 H151b . . . 109.0 ? N15 C151 H151c . . . 110.8 ? H151a C151 H151b . . . 108.7 ? H151a C151 H151c . . . 108.4 ? H151b C151 H151c . . . 111.2 ? N12 C1 N12' . . . 111.0(7) ? N12 C1 H1a . . . 109.3 ? N12 C1 H1b . . . 109.3 ? N12' C1 H1a . . . 109.5 ? N12' C1 H1b . . . 109.4 ? H1a C1 H1b . . . 108.4 ? Au2 C11' N12' . . . 128.4(7) ? Au2 C11' N15' . . . 125.7(5) ? N12' C11' N15' . . . 104.6(7) ? C1 N12' C11' . . . 125.6(7) ? C1 N12' C13' . . . 123.4(6) ? C11' N12' C13' . . . 110.9(7) ? N12' C13' C14' . . . 106.7(7) ? N12' C13' H13' . . . 126.3 ? C14' C13' H13' . . . 127.0 ? C13' C14' N15' . . . 106.4(9) ? C13' C14' H14' . . . 127.8 ? N15' C14' H14' . . . 125.9 ? C11' N15' C14' . . . 111.4(6) ? C11' N15' C151' . . . 125.0(7) ? C14' N15' C151' . . . 123.6(8) ? N15' C151' H151'a . . . 109.5 ? N15' C151' H151'b . . . 110.0 ? N15' C151' H151'c . . . 110.6 ? H151'a C151' H151'b . . . 108.2 ? H151'a C151' H151'c . . . 108.9 ? H151'b C151' H151'c . . . 109.7 ? Au1 C21 N22 . . . 130.3(6) ? Au1 C21 N25 . . . 125.2(5) ? N22 C21 N25 . . . 104.4(7) ? C21 N22 C23 . . . 110.9(6) ? C21 N22 C2 . . . 125.0(7) ? C23 N22 C2 . . . 123.9(6) ? N22 C23 C24 . . . 105.9(7) ? N22 C23 H23 . . . 127.1 ? C24 C23 H23 . . . 127.0 ? C23 C24 N25 . . . 107.0(8) ? C23 C24 H24 . . . 126.4 ? N25 C24 H24 . . . 126.6 ? C21 N25 C24 . . . 111.8(6) ? C21 N25 C251 . . . 125.2(7) ? C24 N25 C251 . . . 123.0(7) ? N25 C251 H251a . . . 107.7 ? N25 C251 H251b . . . 107.6 ? N25 C251 H251c . . . 110.5 ? H251a C251 H251b . . . 109.4 ? H251a C251 H251c . . . 109.2 ? H251b C251 H251c . . . 112.4 ? N22 C2 N22' . . . 111.4(6) ? N22 C2 H2a . . . 109.5 ? N22 C2 H2b . . . 109.2 ? N22' C2 H2a . . . 109. ? N22' C2 H2b . . . 109.5 ? H2a C2 H2b . . . 107.9 ? Au2 C21' N22' . . . 129.3(5) ? Au2 C21' N25' . . . 125.4(7) ? N22' C21' N25' . . . 104.7(7) ? C2 N22' C21' . . . 125.4(6) ? C2 N22' C23' . . . 123.2(8) ? C21' N22' C23' . . . 111.4(6) ? N22' C23' C24' . . . 106.5(8) ? N22' C23' H23' . . . 126.5 ? C24' C23' H23' . . . 127.1 ? C23' C24' N25' . . . 106.7(7) ? C23' C24' H24' . . . 126.9 ? N25' C24' H24' . . . 126.4 ? C21' N25' C24' . . . 110.7(7) ? C21' N25' C251' . . . 125.9(7) ? C24' N25' C251' . . . 123.3(6) ? N25' C251' H251'a . . . 109.6 ? N25' C251' H251'b . . . 112.0 ? N25' C251' H251'c . . . 112.1 ? H251'a C251' H251'b . . . 105.7 ? H251'a C251' H251'c . . . 108.5 ? H251'b C251' H251'c . . . 108.7 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 904 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min -21 _reflns_limit_k_max 21 _reflns_limit_l_min -23 _reflns_limit_l_max 23 _reflns_number_observed ? _reflns_d_resolution_high .581 _reflns_d_resolution_low 12.877 _diffrn_reflns_av_sigmaI/netI .16 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .106 _refine_ls_wR_factor_all .055 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_shift/su_mean .0004 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END