Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 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 - M313 The University of Western Australia 35 Stirling Highway 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 ; Cationic, linear Au(I) N-heterocyclic carbene complexes: synthesis, structure and anti-mitochondrial activity ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name 'Murray Baker' 'Peter J. Barnard' 'Susan Berners-Price' 'Simon K. Brayshaw' 'James L. Hickey' '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. Program 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 ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_1.PF6 _database_code_depnum_ccdc_archive 'CCDC 298906' _audit_creation_method Xtal3.6 _audit_creation_date 03-09-24 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C10 H16 Au1 F6 N4 P1' _chemical_formula_moiety 'C10 H16 Au1 N4, F6 P1' _chemical_formula_weight 534.19 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.302(6) _cell_length_b 21.388(11) _cell_length_c 6.973(4) _cell_angle_alpha 90.00000 _cell_angle_beta 112.567(9) _cell_angle_gamma 90.00000 _cell_volume 1556.5(15) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.28 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 2940 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 32.8 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 9.617 _exptl_crystal_description bar _exptl_crystal_size_max .55 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .07 _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 .58 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 7700 _reflns_number_total 2666 _reflns_Friedel_coverage 0 _reflns_number_gt 1647 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 32.21 _diffrn_reflns_theta_full 32.2 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .053 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .05 _refine_ls_wR_factor_ref .069 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_number_reflns 1647 _refine_ls_number_parameters 102 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .001 _refine_diff_density_min -3.093 _refine_diff_density_max 5.243 _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 64 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' F ? 0 24 .014 .01 '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' P ? 0 4 .09 .095 '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 .50000 .50000 .50000 .0243(2) Uani ? ? 1.00000 ? ? C1 .4145(9) .5846(3) .4568(12) .023(3) Uani ? ? 1.00000 ? ? N2 .4698(8) .6416(4) .4807(11) .026(4) Uani ? ? 1.00000 ? ? C21 .6061(12) .6507(5) .5502(16) .034(5) Uani ? ? 1.00000 ? ? C3 .3799(11) .6886(4) .4315(15) .032(4) Uani ? ? 1.00000 ? ? C4 .2646(10) .6610(3) .3761(13) .026(4) Uani ? ? 1.00000 ? ? N5 .2880(8) .5964(3) .3937(11) .026(3) Uani ? ? 1.00000 ? ? C51 .1863(10) .5492(4) .3501(17) .036(5) Uani ? ? 1.00000 ? ? P .00000 .64485(13) .75000 .0233(13) Uani ? ? 1.00000 ? ? F1 .1042(7) .5927(3) .8501(12) .059(4) Uani ? ? 1.00000 ? ? F2 .1043(6) .6983(2) .8548(9) .047(3) Uani ? ? 1.00000 ? ? F3 .0356(8) .6452(4) .5482(11) .060(4) Uani ? ? 1.00000 ? ? H21a .64365 .62229 .48619 .05000 Uiso ? ? 1.00000 ? ? H21b .64673 .64700 .69722 .05000 Uiso ? ? 1.00000 ? ? H21c .62193 .69234 .51739 .05000 Uiso ? ? 1.00000 ? ? H3 .39564 .73301 .43135 .04200 Uiso ? ? 1.00000 ? ? H4 .17931 .68066 .33356 .03300 Uiso ? ? 1.00000 ? ? H51a .16000 .54725 .46550 .05100 Uiso ? ? 1.00000 ? ? H51b .21790 .50931 .33284 .05100 Uiso ? ? 1.00000 ? ? H51c .11466 .55986 .22744 .05100 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 .0341(3) .0201(2) .0243(2) .0035(2) .0175(2) .0018(2) C1 .030(5) .024(4) .019(4) .001(3) .015(4) .002(3) N2 .036(6) .021(3) .028(4) .004(3) .020(4) .006(3) C21 .049(7) .034(5) .029(5) -.004(5) .028(5) .002(4) C3 .057(7) .022(4) .030(5) .006(4) .032(5) .001(3) C4 .034(5) .024(4) .024(4) .011(4) .017(4) .003(3) N5 .039(5) .017(3) .031(4) -.003(3) .023(4) .001(3) C51 .040(6) .028(4) .048(6) .003(4) .025(5) .006(4) P .0341(18) .0162(12) .0283(16) .00000 .0216(15) .00000 F1 .061(5) .035(3) .081(5) .017(3) .026(4) .012(3) F2 .061(4) .032(3) .042(3) -.013(3) .014(3) -.002(3) F3 .101(7) .059(5) .045(4) -.009(4) .056(4) -.009(4) # 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 C1 . . 2.018(8) ? Au C1 . '3 666' 2.018(8) ? C1 N2 . . 1.351(12) ? C1 N5 . . 1.349(13) ? N2 C21 . . 1.439(15) ? N2 C3 . . 1.377(13) ? C21 H21a . . .945 ? C21 H21b . . .952 ? C21 H21c . . .954 ? C3 C4 . . 1.346(15) ? C3 H3 . . .966 ? C4 N5 . . 1.403(10) ? C4 H4 . . .988 ? N5 C51 . . 1.471(12) ? C51 H51a . . .959 ? C51 H51b . . .950 ? C51 H51c . . .953 ? P F1 . . 1.577(6) ? P F2 . . 1.603(6) ? P F3 . . 1.605(9) ? P F1 . '2 556' 1.577(6) ? P F2 . '2 556' 1.603(6) ? P F3 . '2 556' 1.605(9) ? 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 C1 Au C1 . . '3 666' 180.0000 ? Au C1 N2 . . . 128.2(7) ? Au C1 N5 . . . 127.1(6) ? N2 C1 N5 . . . 104.7(7) ? C1 N2 C21 . . . 123.2(8) ? C1 N2 C3 . . . 111.5(8) ? C21 N2 C3 . . . 125.2(8) ? N2 C21 H21a . . . 111.8 ? N2 C21 H21b . . . 111.3 ? N2 C21 H21c . . . 108.7 ? H21a C21 H21b . . . 109.7 ? H21a C21 H21c . . . 109.1 ? H21b C21 H21c . . . 106.1 ? N2 C3 C4 . . . 106.9(8) ? N2 C3 H3 . . . 126.9 ? C4 C3 H3 . . . 126.1 ? C3 C4 N5 . . . 106.2(8) ? C3 C4 H4 . . . 128.7 ? N5 C4 H4 . . . 125.1 ? C1 N5 C4 . . . 110.7(7) ? C1 N5 C51 . . . 125.8(7) ? C4 N5 C51 . . . 123.5(8) ? N5 C51 H51a . . . 109.0 ? N5 C51 H51b . . . 109.9 ? N5 C51 H51c . . . 110.4 ? H51a C51 H51b . . . 108.7 ? H51a C51 H51c . . . 109.5 ? H51b C51 H51c . . . 109.4 ? F1 P F2 . . . 90.5(3) ? F1 P F3 . . . 89.8(5) ? F1 P F1 . . '2 556' 90.0(3) ? F1 P F2 . . '2 556' 178.8(5) ? F1 P F3 . . '2 556' 90.6(5) ? F2 P F3 . . . 90.5(4) ? F2 P F1 . . '2 556' 178.8(4) ? F2 P F2 . . '2 556' 89.0(3) ? F2 P F3 . . '2 556' 89.1(4) ? F3 P F1 . . '2 556' 90.6(5) ? F3 P F2 . . '2 556' 89.1(4) ? F3 P F3 . . '2 556' 179.5(5) ? F1 P F2 '2 556' . '2 556' 90.5(3) ? F1 P F3 '2 556' . '2 556' 89.8(5) ? F2 P F3 '2 556' . '2 556' 90.5(4) ? _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 1008 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 16 _reflns_limit_k_min 0 _reflns_limit_k_max 32 _reflns_limit_l_min -10 _reflns_limit_l_max 9 _reflns_number_observed ? _reflns_d_resolution_high .667 _reflns_d_resolution_low 10.671 _diffrn_reflns_av_sigmaI/netI .115 _diffrn_reflns_theta_min 1.9 _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 .083 _refine_ls_wR_factor_all .077 _refine_ls_goodness_of_fit_all .94 _refine_ls_shift/su_mean .0002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-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 block for single structure (one for each study in the paper) #======================================================================= data_2.pf6 _database_code_depnum_ccdc_archive 'CCDC 298907' _audit_creation_method Xtal3.6 _audit_creation_date 03-10-06 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C12 H20 Au1 F6 N4 P1' _chemical_formula_moiety ? _chemical_formula_weight 562.25 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C_m_c_a _symmetry_space_group_name_Hall -c_2ac_2 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z +x,-y,-z 1/2-x,+y,1/2-z -x,-y,-z 1/2+x,+y,1/2-z -x,+y,+z 1/2+x,-y,1/2+z 1/2+x,1/2+y,+z -x,1/2-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2-x,1/2-y,-z +x,1/2+y,1/2-z 1/2-x,1/2+y,+z +x,1/2-y,1/2+z _cell_length_a 15.221(5) _cell_length_b 21.319(6) _cell_length_c 10.959(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 3556.2(18) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 2.1 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 2768 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 23.36 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 8.424 _exptl_crystal_description cuboid _exptl_crystal_size_max .13 _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 .63 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 11785 _reflns_number_total 1601 _reflns_Friedel_coverage 0 _reflns_number_gt 1160 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .070 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .108 _refine_ls_wR_factor_ref .164 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_number_reflns 1160 _refine_ls_number_parameters 117 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .0001 _refine_diff_density_min -4.445 _refine_diff_density_max 4.393 _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 96 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 160 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' F ? 0 48 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 32 .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 .11581(9) .50000 .50000 .0885(12) Uani ? ? 1.00000 ? ? C1 .1175(13) .5707(17) .615(2) .09(2) Uani ? ? 1.00000 ? ? N2 .1165(14) .6338(15) .591(2) .11(2) Uani ? ? 1.00000 ? ? C21 .109(3) .657(2) .477(4) .16(4) Uani ? ? 1.00000 ? ? C22 .188(3) .6690(19) .427(3) .14(3) Uani ? ? 1.00000 ? ? C3 .123(2) .6720(14) .691(4) .12(2) Uani ? ? 1.00000 ? ? C4 .131(2) .632(2) .786(4) .14(3) Uani ? ? 1.00000 ? ? N5 .1260(14) .5727(11) .738(2) .113(18) Uani ? ? 1.00000 ? ? C51 .133(3) .5171(16) .825(3) .20(4) Uani ? ? 1.00000 ? ? P .00000 .6517(3) .1201(6) .070(5) Uani ? ? 1.00000 ? ? F1 .00000 .5959(8) .0252(12) .085(12) Uani ? ? 1.00000 ? ? F2 .1035(13) .6524(10) .1206(18) .145(17) Uani ? ? 1.00000 ? ? F3 .00000 .7072(8) .2168(14) .134(17) Uani ? ? 1.00000 ? ? F4 .00000 .6982(10) .0101(14) .15(3) Uani ? ? 1.00000 ? ? F5 .00000 .6049(7) .2293(12) .088(11) Uani ? ? 1.00000 ? ? H21a .07174 .69431 .48161 .15500 Uiso ? ? 1.00000 ? ? H21b .07480 .62682 .42884 .15500 Uiso ? ? 1.00000 ? ? H22a .17851 .68687 .34792 .17400 Uiso ? ? 1.00000 ? ? H22b .21859 .63116 .41999 .17400 Uiso ? ? 1.00000 ? ? H22c .21723 .69772 .47715 .17400 Uiso ? ? 1.00000 ? ? H3 .12037 .71835 .70108 .15400 Uiso ? ? 1.00000 ? ? H4 .13163 .64727 .86184 .13800 Uiso ? ? 1.00000 ? ? H51a .13664 .53400 .90746 .29400 Uiso ? ? 1.00000 ? ? H51b .19013 .49736 .81031 .29400 Uiso ? ? 1.00000 ? ? H51c .08701 .48932 .81874 .29400 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 .0610(11) .1121(13) .0923(13) .00000 .00000 -.0549(8) C1 .044(14) .17(3) .061(16) -.013(14) -.001(9) -.021(17) N2 .12(2) .14(2) .073(17) .003(15) -.041(12) -.034(16) C21 .22(6) .11(3) .14(4) .07(3) -.08(4) -.07(3) C22 .16(3) .20(4) .047(17) -.01(3) -.012(18) .02(2) C3 .13(2) .10(2) .12(3) -.020(16) .03(2) -.07(2) C4 .16(3) .16(3) .10(3) -.08(2) .06(2) -.08(2) N5 .098(16) .134(19) .11(2) -.036(13) .052(13) -.048(16) C51 .36(7) .15(3) .09(3) -.14(4) .14(4) -.04(2) P .119(7) .067(4) .024(4) .00000 .00000 -.002(3) F1 .146(19) .081(10) .028(7) .00000 .00000 -.014(6) F2 .127(16) .20(2) .107(14) -.050(13) .000(11) .004(14) F3 .28(3) .075(10) .042(10) .00000 .00000 -.009(8) F4 .33(5) .079(12) .043(11) .00000 .00000 .013(8) F5 .153(17) .086(9) .026(7) .00000 .00000 .007(7) # 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 C1 . . 1.96(3) ? Au C1 . '3 566' 1.96(3) ? Au Au . '5 566' 3.525(2) ? C1 N2 . . 1.37(5) ? C1 N5 . . 1.36(3) ? N2 C21 . . 1.35(6) ? N2 C3 . . 1.37(5) ? C21 C22 . . 1.35(7) ? C21 H21a . . .98 ? C21 H21b . . .98 ? C22 H22a . . .95 ? C22 H22b . . .93 ? C22 H22c . . .93 ? C3 C4 . . 1.35(5) ? C3 H3 . . 1.00 ? C4 N5 . . 1.37(5) ? C4 H4 . . .90 ? N5 C51 . . 1.52(4) ? C51 H51a . . .97 ? C51 H51b . . .98 ? C51 H51c . . .92 ? P F1 . . 1.579(17) ? P F2 . . 1.58(2) ? P F3 . . 1.590(17) ? P F4 . . 1.56(2) ? P F5 . . 1.558(15) ? P F2 . 7 1.58(2) ? 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 C1 Au C1 . . '3 566' 178.5(8) ? C1 Au Au . . '5 566' 90.7(6) ? C1 Au Au '3 566' . '5 566' 90.7(6) ? Au C1 N2 . . . 129(2) ? Au C1 N5 . . . 131(3) ? N2 C1 N5 . . . 99(3) ? C1 N2 C21 . . . 122(3) ? C1 N2 C3 . . . 116(3) ? C21 N2 C3 . . . 122(3) ? N2 C21 C22 . . . 112(4) ? N2 C21 H21a . . . 107 ? N2 C21 H21b . . . 108 ? C22 C21 H21a . . . 112 ? C22 C21 H21b . . . 113 ? H21a C21 H21b . . . 105 ? C21 C22 H22a . . . 108 ? C21 C22 H22b . . . 108 ? C21 C22 H22c . . . 108 ? H22a C22 H22b . . . 111 ? H22a C22 H22c . . . 110 ? H22b C22 H22c . . . 112 ? N2 C3 C4 . . . 104(3) ? N2 C3 H3 . . . 133 ? C4 C3 H3 . . . 123 ? C3 C4 N5 . . . 107(3) ? C3 C4 H4 . . . 120 ? N5 C4 H4 . . . 133 ? C1 N5 C4 . . . 114(3) ? C1 N5 C51 . . . 127(3) ? C4 N5 C51 . . . 119(3) ? N5 C51 H51a . . . 107 ? N5 C51 H51b . . . 107 ? N5 C51 H51c . . . 114 ? H51a C51 H51b . . . 105 ? H51a C51 H51c . . . 111 ? H51b C51 H51c . . . 113 ? F1 P F2 . . . 90.6(8) ? F1 P F3 . . . 179.4(9) ? F1 P F4 . . . 88.3(9) ? F1 P F5 . . . 91.4(8) ? F1 P F2 . . 7 90.6(8) ? F2 P F3 . . . 89.4(8) ? F2 P F4 . . . 89.8(8) ? F2 P F5 . . . 90.2(8) ? F2 P F2 . . 7 178.8(12) ? F3 P F4 . . . 92.3(10) ? F3 P F5 . . . 87.9(8) ? F3 P F2 . . 7 89.4(8) ? F4 P F5 . . . 179.7(5) ? F4 P F2 . . 7 89.8(8) ? F5 P F2 . . 7 90.2(8) ? 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 2144 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 25 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _reflns_number_observed ? _reflns_d_resolution_high .842 _reflns_d_resolution_low 10.637 _diffrn_reflns_av_sigmaI/netI .074 _diffrn_reflns_theta_min 1.91 _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 1 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .133 _refine_ls_wR_factor_all .187 _refine_ls_goodness_of_fit_all 1.138 _refine_ls_shift/su_mean .00003 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-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 block for single structure (one for each study in the paper) #======================================================================= data_3.cl _database_code_depnum_ccdc_archive 'CCDC 298908' _audit_creation_method Xtal3.6 _audit_creation_date 05-10-05 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C18 H32 Au1 Cl1 N4' _chemical_formula_moiety 'C18 H32 Au1 N4, Cl' _chemical_formula_weight 536.9 _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 10.692(2) _cell_length_b 10.855(2) _cell_length_c 10.818(2) _cell_angle_alpha 90.00000 _cell_angle_beta 118.252(2) _cell_angle_gamma 90.00000 _cell_volume 1106.0(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4977 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 33.31 _cell_measurement_temperature 170 _exptl_absorpt_coefficient_mu 6.778 _exptl_crystal_description plate _exptl_crystal_size_max .34 _exptl_crystal_size_mid .18 _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 .66 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 18513 _reflns_number_total 4126 _reflns_Friedel_coverage 0 _reflns_number_gt 3039 _reflns_threshold_expression 'I > 2.00 sig(I)' _diffrn_reflns_theta_max 33.3 _diffrn_reflns_theta_full 33.3 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .032 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _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 Fsqd _refine_ls_R_factor_gt .017 _refine_ls_wR_factor_gt .037 _refine_ls_goodness_of_fit_gt .96 _refine_ls_number_reflns 4126 _refine_ls_number_parameters 112 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .002 _refine_diff_density_min -1.012 _refine_diff_density_max 1.25 _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 64 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' Cl ? 0 2 .132 .159 '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' 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 .00000 .00000 .50000 .01466(4) Uani ? ? 1.00000 ? ? Cl .00000 .00000 .00000 .0266(3) Uani ? ? 1.00000 ? ? C1 .1470(2) .1364(2) .5704(2) .0200(8) Uani ? ? 1.00000 ? ? N2 .2051(2) .1953(2) .4986(2) .0220(7) Uani ? ? 1.00000 ? ? C21 .1847(3) .1570(2) .3587(2) .0238(9) Uani ? ? 1.00000 ? ? C22 .3026(4) .0686(3) .3752(3) .0363(13) Uani ? ? 1.00000 ? ? C23 .1762(4) .2697(3) .2712(3) .0371(13) Uani ? ? 1.00000 ? ? C3 .2989(3) .2858(3) .5807(3) .0302(11) Uani ? ? 1.00000 ? ? C4 .2966(3) .2843(3) .7057(3) .0344(12) Uani ? ? 1.00000 ? ? N5 .2046(2) .1911(2) .6983(2) .0260(8) Uani ? ? 1.00000 ? ? C51 .1738(3) .1585(3) .8139(3) .0301(11) Uani ? ? 1.00000 ? ? C52 .3088(4) .1189(4) .9423(4) .0504(17) Uani ? ? 1.00000 ? ? C53 .1025(5) .2665(4) .8460(4) .056(2) Uani ? ? 1.00000 ? ? H21 .09734 .11401 .30990 .03000 Uiso ? ? 1.00000 ? ? H22a .30405 -.00006 .43026 .05400 Uiso ? ? 1.00000 ? ? H22b .39149 .10991 .42025 .05400 Uiso ? ? 1.00000 ? ? H22c .28582 .04097 .28528 .05400 Uiso ? ? 1.00000 ? ? H23a .10168 .32188 .26380 .05600 Uiso ? ? 1.00000 ? ? H23b .15801 .24422 .18022 .05600 Uiso ? ? 1.00000 ? ? H23c .26368 .31316 .31519 .05600 Uiso ? ? 1.00000 ? ? H3 .35390 .33836 .55514 .03800 Uiso ? ? 1.00000 ? ? H4 .34834 .33731 .78333 .04300 Uiso ? ? 1.00000 ? ? H51 .10978 .09086 .78593 .03800 Uiso ? ? 1.00000 ? ? H52a .35021 .05171 .91842 .07600 Uiso ? ? 1.00000 ? ? H52b .28700 .09438 1.01417 .07600 Uiso ? ? 1.00000 ? ? H52c .37373 .18584 .97449 .07600 Uiso ? ? 1.00000 ? ? H53a .01847 .28870 .76344 .08400 Uiso ? ? 1.00000 ? ? H53b .16556 .33468 .87738 .08400 Uiso ? ? 1.00000 ? ? H53c .07884 .24322 .91706 .08400 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 .01384(5) .01500(5) .01351(5) -.00251(3) .00513(4) .00045(3) Cl .0250(4) .0257(4) .0336(4) .0033(3) .0175(3) -.0028(3) C1 .0179(9) .0221(10) .0201(9) -.0037(8) .0090(8) -.0013(7) N2 .0216(9) .0233(9) .0233(9) -.0064(7) .0124(7) -.0027(7) C21 .0280(11) .0255(11) .0202(10) -.0064(9) .0132(9) -.0016(8) C22 .0425(16) .0347(15) .0399(15) .0060(12) .0263(13) -.0011(12) C23 .0458(16) .0371(15) .0289(13) -.0084(13) .0181(12) .0037(11) C3 .0324(12) .0310(13) .0292(12) -.0168(10) .0163(10) -.0086(10) C4 .0381(14) .0383(15) .0298(13) -.0214(12) .0186(11) -.0130(11) N5 .0274(10) .0304(11) .0236(9) -.0119(8) .0149(8) -.0079(8) C51 .0366(13) .0357(14) .0226(11) -.0070(11) .0177(10) -.0023(10) C52 .0356(16) .074(3) .0349(16) -.0109(16) .0108(13) .0150(16) C53 .085(3) .053(2) .054(2) .007(2) .053(2) -.0003(17) # 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 Au C1 . . 2.027(2) ? Au C1 . '3 556' 2.027(2) ? C1 N2 . . 1.362(4) ? C1 N5 . . 1.356(3) ? N2 C21 . . 1.482(4) ? N2 C3 . . 1.385(3) ? C21 C22 . . 1.526(5) ? C21 C23 . . 1.523(4) ? C21 H21 . . .950 ? C22 H22a . . .950 ? C22 H22b . . .950 ? C22 H22c . . .950 ? C23 H23a . . .950 ? C23 H23b . . .950 ? C23 H23c . . .950 ? C3 C4 . . 1.364(5) ? C3 H3 . . .950 ? C4 N5 . . 1.386(4) ? C4 H4 . . .950 ? N5 C51 . . 1.479(5) ? C51 C52 . . 1.516(4) ? C51 C53 . . 1.525(6) ? C51 H51 . . .950 ? C52 H52a . . .950 ? C52 H52b . . .950 ? C52 H52c . . .950 ? C53 H53a . . .950 ? C53 H53b . . .950 ? C53 H53c . . .950 ? 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 C1 Au C1 . . '3 556' 180.0000 ? Au C1 N2 . . . 127.61(17) ? Au C1 N5 . . . 126.9(2) ? N2 C1 N5 . . . 105.5(2) ? C1 N2 C21 . . . 124.4(2) ? C1 N2 C3 . . . 110.7(2) ? C21 N2 C3 . . . 124.5(3) ? N2 C21 C22 . . . 110.1(2) ? N2 C21 C23 . . . 110.2(2) ? N2 C21 H21 . . . 109.6 ? C22 C21 C23 . . . 112.4(3) ? C22 C21 H21 . . . 107.3 ? C23 C21 H21 . . . 107.2 ? C21 C22 H22a . . . 109.5 ? C21 C22 H22b . . . 109.5 ? C21 C22 H22c . . . 109.5 ? H22a C22 H22b . . . 109.5 ? H22a C22 H22c . . . 109.5 ? H22b C22 H22c . . . 109.5 ? C21 C23 H23a . . . 109.4 ? C21 C23 H23b . . . 109.5 ? C21 C23 H23c . . . 109.5 ? H23a C23 H23b . . . 109.5 ? H23a C23 H23c . . . 109.5 ? H23b C23 H23c . . . 109.5 ? N2 C3 C4 . . . 106.3(3) ? N2 C3 H3 . . . 126.8 ? C4 C3 H3 . . . 126.9 ? C3 C4 N5 . . . 107.2(2) ? C3 C4 H4 . . . 126.4 ? N5 C4 H4 . . . 126.4 ? C1 N5 C4 . . . 110.2(3) ? C1 N5 C51 . . . 125.6(2) ? C4 N5 C51 . . . 124.2(2) ? N5 C51 C52 . . . 110.2(3) ? N5 C51 C53 . . . 110.1(3) ? N5 C51 H51 . . . 109.4 ? C52 C51 C53 . . . 111.8(3) ? C52 C51 H51 . . . 107.6 ? C53 C51 H51 . . . 107.7 ? C51 C52 H52a . . . 109.4 ? C51 C52 H52b . . . 109.5 ? C51 C52 H52c . . . 109.5 ? H52a C52 H52b . . . 109.5 ? H52a C52 H52c . . . 109.5 ? H52b C52 H52c . . . 109.5 ? C51 C53 H53a . . . 109.5 ? C51 C53 H53b . . . 109.5 ? C51 C53 H53c . . . 109.5 ? H53a C53 H53b . . . 109.5 ? H53a C53 H53c . . . 109.5 ? H53b C53 H53c . . . 109.5 ? _exptl_crystal_F_000 528 _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -16 _reflns_limit_l_max 14 _reflns_number_observed ? _reflns_d_resolution_high .644 _reflns_d_resolution_low 9.213 _diffrn_reflns_av_sigmaI/netI .032 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 170 _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 .026 _refine_ls_wR_factor_ref .047 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_shift/su_mean .0003 #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## #============================================================================== #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_4.pf6 _database_code_depnum_ccdc_archive 'CCDC 298909' _audit_creation_method Xtal3.6 _audit_creation_date 03-10-15 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C22 H40 Au1 F6 N4 P1' _chemical_formula_moiety ? _chemical_formula_weight 702.52 _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 14.007(8) _cell_length_b 14.365(8) _cell_length_c 14.370(8) _cell_angle_alpha 89.345(10) _cell_angle_beta 84.748(10) _cell_angle_gamma 76.273(10) _cell_volume 2797(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4366 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 29.22 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 5.374 _exptl_crystal_description prism _exptl_crystal_size_max .13 _exptl_crystal_size_mid .12 _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 .69 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 32862 _reflns_number_total 15655 _reflns_Friedel_coverage 0 _reflns_number_gt 8656 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 30.1 _diffrn_reflns_theta_full 30.1 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .053 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _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 .077 _refine_ls_wR_factor_ref .117 _refine_ls_goodness_of_fit_ref 1.14 _refine_ls_number_reflns 8656 _refine_ls_number_parameters 354 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .004 _refine_diff_density_min -4.013 _refine_diff_density_max 3.71 _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 88 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 160 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' F ? 0 24 .014 .01 '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' P ? 0 4 .09 .095 '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 .50000 .50000 .50000 .0295(4) Uani ? ? 1.00000 ? ? Au2 .00000 .50000 .00000 .0707(8) Uani ? ? 1.00000 ? ? Au3 .26300(4) .18089(4) .26794(4) .0429(4) Uani ? ? 1.00000 ? ? C11 .5228(8) .5167(8) .3600(8) .028(2) Uiso ? ? 1.00000 ? ? N12 .5852(9) .4563(8) .2994(8) .043(3) Uiso ? ? 1.00000 ? ? C121 .6414(13) .3635(12) .3233(12) .059(4) Uiso ? ? 1.00000 ? ? C122 .5652(16) .2926(15) .3323(14) .073(5) Uiso ? ? 1.00000 ? ? C123 .6137(19) .1944(17) .3531(16) .093(7) Uiso ? ? 1.00000 ? ? C124 .537(2) .1324(17) .3724(17) .094(7) Uiso ? ? 1.00000 ? ? C13 .5785(12) .4928(11) .2096(11) .050(4) Uiso ? ? 1.00000 ? ? C14 .5154(12) .5793(11) .2153(11) .050(4) Uiso ? ? 1.00000 ? ? N15 .4780(8) .5913(7) .3093(7) .036(2) Uiso ? ? 1.00000 ? ? C151 .4002(11) .6744(10) .3456(10) .044(3) Uiso ? ? 1.00000 ? ? C152 .4391(13) .7581(12) .3672(12) .061(4) Uiso ? ? 1.00000 ? ? C153 .4876(14) .7990(13) .2840(13) .067(5) Uiso ? ? 1.00000 ? ? C154 .514(2) .893(2) .3180(19) .108(8) Uiso ? ? 1.00000 ? ? C21 .0054(14) .4992(14) .1423(13) .067(5) Uiso ? ? 1.00000 ? ? N22 -.0296(11) .4361(10) .2012(10) .062(4) Uiso ? ? 1.00000 ? ? C221 -.0791(14) .3647(13) .1787(13) .064(5) Uiso ? ? 1.00000 ? ? C222 -.0058(13) .2656(12) .1711(12) .057(4) Uiso ? ? 1.00000 ? ? C223 -.0637(19) .1878(18) .1546(17) .093(7) Uiso ? ? 1.00000 ? ? C224 -.003(3) .094(3) .133(3) .155(13) Uiso ? ? 1.00000 ? ? C23 -.0152(16) .4574(15) .2870(14) .074(5) Uiso ? ? 1.00000 ? ? C24 .0328(15) .5276(14) .2884(14) .073(5) Uiso ? ? 1.00000 ? ? N25 .0447(13) .5509(12) .1957(12) .076(4) Uiso ? ? 1.00000 ? ? C251 .0937(18) .6260(17) .1597(16) .088(6) Uiso ? ? 1.00000 ? ? C252 .030(3) .711(3) .122(3) .173(15) Uiso ? ? 1.00000 ? ? C253 -.026(4) .762(4) .209(3) .196(13) Uiso ? ? 1.00000 ? ? C254 -.108(4) .835(4) .176(4) .235(16) Uiso ? ? 1.00000 ? ? C31 .2371(10) .0490(9) .2647(9) .040(3) Uiso ? ? 1.00000 ? ? N32 .1792(9) .0110(8) .3306(8) .045(3) Uiso ? ? 1.00000 ? ? C321 .1403(13) .0566(15) .4215(14) .084(6) Uiso ? ? 1.00000 ? ? C322 .2247(13) .0168(13) .5013(13) .075(5) Uiso ? ? 1.00000 ? ? C323 .188(2) .0590(16) .5887(19) .124(10) Uiso ? ? 1.00000 ? ? C324 .119(3) -.001(3) .641(2) .193(17) Uiso ? ? 1.00000 ? ? C33 .1763(12) -.0795(12) .3013(11) .054(4) Uiso ? ? 1.00000 ? ? C34 .2279(13) -.0937(12) .2205(12) .056(4) Uiso ? ? 1.00000 ? ? N35 .2663(8) -.0185(8) .1996(8) .041(3) Uiso ? ? 1.00000 ? ? C351 .3331(10) -.0120(12) .1153(11) .055(4) Uiso ? ? 1.00000 ? ? C352 .2779(13) .0102(17) .0338(14) .092(7) Uiso ? ? 1.00000 ? ? C353 .350(2) .030(2) -.050(2) .145(12) Uiso ? ? 1.00000 ? ? C354 .387(3) -.050(3) -.098(3) .21(2) Uiso ? ? 1.00000 ? ? C41 .2879(11) .3152(11) .2674(11) .049(4) Uiso ? ? 1.00000 ? ? N42 .3360(11) .3539(10) .1986(10) .061(4) Uiso ? ? 1.00000 ? ? C421 .391(2) .2970(17) .114(2) .116(9) Uiso ? ? 1.00000 ? ? C422 .364(3) .349(3) .027(2) .26(3) Uiso ? ? 1.00000 ? ? C423 .263(2) .352(3) .016(2) .196(14) Uiso ? ? 1.00000 ? ? C424 .249(3) .363(4) -.087(3) .216(15) Uiso ? ? 1.00000 ? ? C43 .3321(16) .4479(15) .2257(15) .078(6) Uiso ? ? 1.00000 ? ? C44 .2859(15) .4617(14) .3056(14) .070(5) Uiso ? ? 1.00000 ? ? N45 .2599(11) .3798(10) .3349(10) .062(4) Uiso ? ? 1.00000 ? ? C451 .2057(12) .3703(17) .4225(15) .087(6) Uiso ? ? 1.00000 ? ? C452 .2755(16) .340(2) .4946(16) .148(12) Uiso ? ? 1.00000 ? ? C453 .216(2) .331(3) .590(2) .183(16) Uiso ? ? 1.00000 ? ? C454 .259(3) .373(3) .663(2) .172(15) Uiso ? ? 1.00000 ? ? P1 -.1185(3) .2914(3) .5112(3) .052(3) Uani ? ? 1.00000 ? ? F11 -.0839(9) .2679(10) .4031(7) .089(10) Uani ? ? 1.00000 ? ? F12 -.1958(10) .3886(8) .4880(9) .095(11) Uani ? ? 1.00000 ? ? F13 -.1507(8) .3123(8) .6191(6) .072(8) Uani ? ? 1.00000 ? ? F14 -.0466(9) .1959(12) .5373(8) .127(12) Uani ? ? 1.00000 ? ? F15 -.0424(11) .3554(14) .5180(7) .139(17) Uani ? ? 1.00000 ? ? F16 -.2054(8) .2380(7) .5085(7) .067(8) Uani ? ? 1.00000 ? ? P2 .6673(3) .3092(3) -.0142(3) .048(3) Uani ? ? 1.00000 ? ? F21 .7377(8) .3709(8) .0235(7) .069(8) Uani ? ? 1.00000 ? ? F22 .6976(7) .3332(8) -.1186(6) .062(7) Uani ? ? 1.00000 ? ? F23 .5953(9) .2476(6) -.0521(7) .071(8) Uani ? ? 1.00000 ? ? F24 .6355(10) .2810(8) .0919(6) .079(9) Uani ? ? 1.00000 ? ? F25 .7578(10) .2180(8) -.0241(9) .111(12) Uani ? ? 1.00000 ? ? F26 .5769(7) .4002(6) -.0063(6) .059(7) Uani ? ? 1.00000 ? ? H121a .66854 .36676 .38106 .07300 Uiso ? ? 1.00000 ? ? H121b .69325 .34057 .27575 .07300 Uiso ? ? 1.00000 ? ? H122a .53651 .29292 .27480 .09100 Uiso ? ? 1.00000 ? ? H122b .51492 .31602 .38093 .09100 Uiso ? ? 1.00000 ? ? H123a .64859 .19432 .40656 .11600 Uiso ? ? 1.00000 ? ? H123b .65842 .16800 .30115 .11600 Uiso ? ? 1.00000 ? ? H124a .56980 .06879 .38581 .14200 Uiso ? ? 1.00000 ? ? H124b .50151 .13238 .31893 .14200 Uiso ? ? 1.00000 ? ? H124c .49168 .15870 .42434 .14200 Uiso ? ? 1.00000 ? ? H13 .61266 .46181 .15394 .06200 Uiso ? ? 1.00000 ? ? H14 .49953 .62320 .16587 .06300 Uiso ? ? 1.00000 ? ? H151a .36760 .65599 .40119 .05500 Uiso ? ? 1.00000 ? ? H151b .35442 .69255 .30007 .05500 Uiso ? ? 1.00000 ? ? H152a .48641 .73876 .41121 .07600 Uiso ? ? 1.00000 ? ? H152b .38576 .80669 .39397 .07600 Uiso ? ? 1.00000 ? ? H153a .44329 .81422 .23666 .08400 Uiso ? ? 1.00000 ? ? H153b .54560 .75408 .26002 .08400 Uiso ? ? 1.00000 ? ? H154a .54537 .92059 .26681 .16100 Uiso ? ? 1.00000 ? ? H154b .55846 .87716 .36548 .16100 Uiso ? ? 1.00000 ? ? H154c .45615 .93730 .34212 .16100 Uiso ? ? 1.00000 ? ? H221a -.10641 .37949 .12067 .08100 Uiso ? ? 1.00000 ? ? H221b -.13050 .36317 .22625 .08100 Uiso ? ? 1.00000 ? ? H222a .02558 .25255 .22734 .07200 Uiso ? ? 1.00000 ? ? H222b .04272 .26501 .12020 .07200 Uiso ? ? 1.00000 ? ? H223a -.10270 .20768 .10395 .11700 Uiso ? ? 1.00000 ? ? H223b -.10576 .18406 .20963 .11700 Uiso ? ? 1.00000 ? ? H224a -.04307 .05105 .12435 .23300 Uiso ? ? 1.00000 ? ? H224b .03628 .07282 .18375 .23300 Uiso ? ? 1.00000 ? ? H224c .03934 .09644 .07807 .23300 Uiso ? ? 1.00000 ? ? H23 -.03621 .42643 .34134 .09200 Uiso ? ? 1.00000 ? ? H24 .05373 .55473 .34073 .09100 Uiso ? ? 1.00000 ? ? H251a .14309 .59794 .11184 .11000 Uiso ? ? 1.00000 ? ? H251b .12382 .64660 .20981 .11000 Uiso ? ? 1.00000 ? ? H252a -.01406 .69322 .08251 .21200 Uiso ? ? 1.00000 ? ? H252b .06824 .74828 .08711 .21200 Uiso ? ? 1.00000 ? ? H253a .01780 .79373 .23966 .25100 Uiso ? ? 1.00000 ? ? H253b -.04506 .71815 .25210 .25100 Uiso ? ? 1.00000 ? ? H254a -.14403 .86519 .22949 .36100 Uiso ? ? 1.00000 ? ? H254b -.14603 .79663 .14744 .36100 Uiso ? ? 1.00000 ? ? H254c -.08316 .87221 .13499 .36100 Uiso ? ? 1.00000 ? ? H321a .07981 .04019 .44159 .10400 Uiso ? ? 1.00000 ? ? H321b .12906 .12421 .41595 .10400 Uiso ? ? 1.00000 ? ? H322a .28469 .03386 .48125 .09400 Uiso ? ? 1.00000 ? ? H322b .23623 -.05086 .50603 .09400 Uiso ? ? 1.00000 ? ? H323a .15059 .12288 .58021 .15600 Uiso ? ? 1.00000 ? ? H323b .24080 .06042 .62468 .15600 Uiso ? ? 1.00000 ? ? H324a .09383 .02792 .69988 .29100 Uiso ? ? 1.00000 ? ? H324b .15603 -.06429 .64896 .29100 Uiso ? ? 1.00000 ? ? H324c .06582 -.00182 .60449 .29100 Uiso ? ? 1.00000 ? ? H33 .14357 -.12271 .33360 .06700 Uiso ? ? 1.00000 ? ? H34 .23682 -.14910 .18219 .07000 Uiso ? ? 1.00000 ? ? H351a .38001 -.07162 .10523 .07000 Uiso ? ? 1.00000 ? ? H351b .36659 .03699 .12443 .07000 Uiso ? ? 1.00000 ? ? H352a .22529 .06506 .04639 .11500 Uiso ? ? 1.00000 ? ? H352b .25222 -.04271 .01870 .11500 Uiso ? ? 1.00000 ? ? H353a .40158 .05348 -.02680 .18100 Uiso ? ? 1.00000 ? ? H353b .31458 .07763 -.08936 .18100 Uiso ? ? 1.00000 ? ? H354a .43675 -.03942 -.14409 .31400 Uiso ? ? 1.00000 ? ? H354b .33645 -.06783 -.12728 .31400 Uiso ? ? 1.00000 ? ? H354c .41544 -.09839 -.05682 .31400 Uiso ? ? 1.00000 ? ? H421a .37563 .23606 .11364 .14400 Uiso ? ? 1.00000 ? ? H421b .46039 .28800 .11827 .14400 Uiso ? ? 1.00000 ? ? H422a .40427 .31532 -.02485 .32400 Uiso ? ? 1.00000 ? ? H422b .37292 .41155 .03037 .32400 Uiso ? ? 1.00000 ? ? H423a .22153 .40480 .05024 .24500 Uiso ? ? 1.00000 ? ? H423b .24695 .29420 .03839 .24500 Uiso ? ? 1.00000 ? ? H424a .18176 .36528 -.09597 .32300 Uiso ? ? 1.00000 ? ? H424b .29032 .30963 -.12044 .32300 Uiso ? ? 1.00000 ? ? H424c .26491 .42023 -.10858 .32300 Uiso ? ? 1.00000 ? ? H43 .35975 .49328 .19065 .09800 Uiso ? ? 1.00000 ? ? H44 .27110 .52020 .33993 .08700 Uiso ? ? 1.00000 ? ? H451a .16851 .32356 .41669 .10800 Uiso ? ? 1.00000 ? ? H451b .16240 .43001 .44044 .10800 Uiso ? ? 1.00000 ? ? H452a .31361 .38559 .49974 .18700 Uiso ? ? 1.00000 ? ? H452b .31812 .27916 .47734 .18700 Uiso ? ? 1.00000 ? ? H453a .21971 .26543 .60324 .22900 Uiso ? ? 1.00000 ? ? H453b .14953 .36442 .58785 .22900 Uiso ? ? 1.00000 ? ? H454a .22365 .36763 .72159 .26000 Uiso ? ? 1.00000 ? ? H454b .25613 .43817 .64981 .26000 Uiso ? ? 1.00000 ? ? H454c .32631 .33918 .66520 .26000 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 .0327(4) .0331(3) .0218(3) -.0085(3) .0052(2) -.0054(2) Au2 .0402(5) .0616(6) .1096(9) -.0165(4) .0048(5) .0324(6) Au3 .0482(3) .0334(3) .0417(3) -.0046(2) .0105(2) .0016(2) P1 .043(2) .076(3) .037(2) -.016(2) .0002(16) .0165(19) F11 .103(9) .131(10) .043(6) -.056(8) .012(5) .006(6) F12 .109(10) .065(7) .115(10) -.021(7) -.043(8) .023(7) F13 .078(7) .091(7) .042(5) -.023(6) .022(5) -.005(5) F14 .076(8) .176(14) .078(8) .065(9) .019(6) .036(8) F15 .138(13) .28(2) .042(6) -.145(15) -.008(7) .019(9) F16 .076(7) .063(6) .070(7) -.036(5) .007(5) -.009(5) P2 .067(3) .0402(19) .0309(18) -.0014(18) -.0081(17) -.0059(14) F21 .064(6) .078(7) .066(6) -.013(5) -.022(5) -.022(5) F22 .050(5) .103(7) .031(4) -.014(5) .001(4) .000(4) F23 .116(9) .048(5) .053(6) -.026(6) -.014(5) -.005(4) F24 .133(10) .074(7) .029(5) -.023(7) -.008(5) .004(4) F25 .134(12) .080(8) .095(9) .049(8) -.065(8) -.051(7) F26 .063(6) .059(5) .046(5) .003(4) -.002(4) -.011(4) # 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 . . 2.028(11) ? Au1 C11 . '2 666' 2.028(11) ? Au2 C21 . . 2.05(2) ? Au2 C21 . '2 565' 2.05(2) ? Au3 C31 . . 2.014(15) ? Au3 C41 . . 2.041(17) ? C11 N12 . . 1.339(15) ? C11 N15 . . 1.349(15) ? N12 C121 . . 1.43(2) ? N12 C13 . . 1.39(2) ? C121 C122 . . 1.64(3) ? C121 H121a . . .951 ? C121 H121b . . .950 ? C122 C123 . . 1.45(3) ? C122 H122a . . .95 ? C122 H122b . . .95 ? C123 C124 . . 1.56(4) ? C123 H123a . . .95 ? C123 H123b . . .95 ? C124 H124a . . .95 ? C124 H124b . . .95 ? C124 H124c . . .95 ? C13 C14 . . 1.34(2) ? C13 H13 . . .951 ? C14 N15 . . 1.401(18) ? C14 H14 . . .951 ? N15 C151 . . 1.476(16) ? C151 C152 . . 1.48(3) ? C151 H151a . . .950 ? C151 H151b . . .949 ? C152 C153 . . 1.50(3) ? C152 H152a . . .949 ? C152 H152b . . .949 ? C153 C154 . . 1.58(4) ? C153 H153a . . .95 ? C153 H153b . . .949 ? C154 H154a . . .95 ? C154 H154b . . .95 ? C154 H154c . . .95 ? C21 N22 . . 1.38(3) ? C21 N25 . . 1.31(3) ? N22 C221 . . 1.42(3) ? N22 C23 . . 1.32(3) ? C221 C222 . . 1.54(2) ? C221 H221a . . .95 ? C221 H221b . . .95 ? C222 C223 . . 1.56(4) ? C222 H222a . . .951 ? C222 H222b . . .950 ? C223 C224 . . 1.43(4) ? C223 H223a . . .95 ? C223 H223b . . .95 ? C224 H224a . . .95 ? C224 H224b . . .95 ? C224 H224c . . .95 ? C23 C24 . . 1.34(3) ? C23 H23 . . .95 ? C24 N25 . . 1.38(3) ? C24 H24 . . .95 ? N25 C251 . . 1.48(3) ? C251 C252 . . 1.46(5) ? C251 H251a . . .95 ? C251 H251b . . .95 ? C252 C253 . . 1.52(6) ? C252 H252a . . .95 ? C252 H252b . . .96 ? C253 C254 . . 1.46(7) ? C253 H253a . . .98 ? C253 H253b . . .95 ? C254 H254a . . .93 ? C254 H254b . . .97 ? C254 H254c . . .90 ? C31 N32 . . 1.382(19) ? C31 N35 . . 1.321(17) ? N32 C321 . . 1.47(2) ? N32 C33 . . 1.38(2) ? C321 C322 . . 1.72(3) ? C321 H321a . . .95 ? C321 H321b . . .95 ? C322 C323 . . 1.40(3) ? C322 H322a . . .95 ? C322 H322b . . .95 ? C323 C324 . . 1.57(5) ? C323 H323a . . .95 ? C323 H323b . . .95 ? C324 H324a . . .95 ? C324 H324b . . .95 ? C324 H324c . . .95 ? C33 C34 . . 1.30(2) ? C33 H33 . . .949 ? C34 N35 . . 1.34(2) ? C34 H34 . . .951 ? N35 C351 . . 1.477(19) ? C351 C352 . . 1.45(3) ? C351 H351a . . .950 ? C351 H351b . . .950 ? C352 C353 . . 1.57(4) ? C352 H352a . . .95 ? C352 H352b . . .95 ? C353 C354 . . 1.32(5) ? C353 H353a . . .95 ? C353 H353b . . .95 ? C354 H354a . . .95 ? C354 H354b . . .94 ? C354 H354c . . .95 ? C41 N42 . . 1.34(2) ? C41 N45 . . 1.32(2) ? N42 C421 . . 1.51(3) ? N42 C43 . . 1.40(3) ? C421 C422 . . 1.48(4) ? C421 H421a . . .95 ? C421 H421b . . .95 ? C422 C423 . . 1.43(5) ? C422 H422a . . .95 ? C422 H422b . . .94 ? C423 C424 . . 1.51(6) ? C423 H423a . . .95 ? C423 H423b . . .96 ? C424 H424a . . .95 ? C424 H424b . . .95 ? C424 H424c . . .94 ? C43 C44 . . 1.26(3) ? C43 H43 . . .95 ? C44 N45 . . 1.36(3) ? C44 H44 . . .95 ? N45 C451 . . 1.43(2) ? C451 C452 . . 1.48(3) ? C451 H451a . . .95 ? C451 H451b . . .95 ? C452 C453 . . 1.56(4) ? C452 H452a . . .95 ? C452 H452b . . .95 ? C453 C454 . . 1.45(5) ? C453 H453a . . .95 ? C453 H453b . . .94 ? C454 H454a . . .95 ? C454 H454b . . .95 ? C454 H454c . . .95 ? P1 F11 . . 1.599(10) ? P1 F12 . . 1.603(12) ? P1 F13 . . 1.587(10) ? P1 F14 . . 1.562(15) ? P1 F15 . . 1.57(2) ? P1 F16 . . 1.589(13) ? P2 F21 . . 1.604(13) ? P2 F22 . . 1.577(9) ? P2 F23 . . 1.622(13) ? P2 F24 . . 1.623(10) ? P2 F25 . . 1.590(12) ? P2 F26 . . 1.586(9) ? 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 C11 . . '2 666' 180.0000 ? C21 Au2 C21 . . '2 565' 180.0000 ? C31 Au3 C41 . . . 178.3(6) ? Au1 C11 N12 . . . 127.1(8) ? Au1 C11 N15 . . . 126.7(8) ? N12 C11 N15 . . . 106.2(10) ? C11 N12 C121 . . . 124.4(12) ? C11 N12 C13 . . . 109.7(10) ? C121 N12 C13 . . . 125.6(12) ? N12 C121 C122 . . . 106.8(14) ? N12 C121 H121a . . . 110.1 ? N12 C121 H121b . . . 110.1 ? C122 C121 H121a . . . 110.1 ? C122 C121 H121b . . . 110.2 ? H121a C121 H121b . . . 109.4 ? C121 C122 C123 . . . 112.7(18) ? C121 C122 H122a . . . 108.7 ? C121 C122 H122b . . . 108.8 ? C123 C122 H122a . . . 109 ? C123 C122 H122b . . . 109 ? H122a C122 H122b . . . 109 ? C122 C123 C124 . . . 111(2) ? C122 C123 H123a . . . 109 ? C122 C123 H123b . . . 109 ? C124 C123 H123a . . . 109 ? C124 C123 H123b . . . 109 ? H123a C123 H123b . . . 110 ? C123 C124 H124a . . . 109 ? C123 C124 H124b . . . 109 ? C123 C124 H124c . . . 109 ? H124a C124 H124b . . . 110 ? H124a C124 H124c . . . 110 ? H124b C124 H124c . . . 109 ? N12 C13 C14 . . . 108.1(13) ? N12 C13 H13 . . . 126.0 ? C14 C13 H13 . . . 126.0 ? C13 C14 N15 . . . 105.5(13) ? C13 C14 H14 . . . 127.2 ? N15 C14 H14 . . . 127.3 ? C11 N15 C14 . . . 110.4(10) ? C11 N15 C151 . . . 125.9(10) ? C14 N15 C151 . . . 123.8(11) ? N15 C151 C152 . . . 113.0(13) ? N15 C151 H151a . . . 108.5 ? N15 C151 H151b . . . 108.6 ? C152 C151 H151a . . . 108.5 ? C152 C151 H151b . . . 108.6 ? H151a C151 H151b . . . 109.5 ? C151 C152 C153 . . . 114.5(15) ? C151 C152 H152a . . . 108.1 ? C151 C152 H152b . . . 108.0 ? C153 C152 H152a . . . 108.3 ? C153 C152 H152b . . . 108.3 ? H152a C152 H152b . . . 109.7 ? C152 C153 C154 . . . 107.4(17) ? C152 C153 H153a . . . 109.9 ? C152 C153 H153b . . . 110.0 ? C154 C153 H153a . . . 109.8 ? C154 C153 H153b . . . 110 ? H153a C153 H153b . . . 109.5 ? C153 C154 H154a . . . 109 ? C153 C154 H154b . . . 109 ? C153 C154 H154c . . . 110 ? H154a C154 H154b . . . 109 ? H154a C154 H154c . . . 110 ? H154b C154 H154c . . . 110 ? Au2 C21 N22 . . . 124.0(15) ? Au2 C21 N25 . . . 130.1(15) ? N22 C21 N25 . . . 105.8(16) ? C21 N22 C221 . . . 128.5(16) ? C21 N22 C23 . . . 107.2(18) ? C221 N22 C23 . . . 124.1(17) ? N22 C221 C222 . . . 110.0(16) ? N22 C221 H221a . . . 109.4 ? N22 C221 H221b . . . 109.4 ? C222 C221 H221a . . . 109.3 ? C222 C221 H221b . . . 109.3 ? H221a C221 H221b . . . 109 ? C221 C222 C223 . . . 108.9(16) ? C221 C222 H222a . . . 109.7 ? C221 C222 H222b . . . 109.7 ? C223 C222 H222a . . . 109.6 ? C223 C222 H222b . . . 109.7 ? H222a C222 H222b . . . 109.3 ? C222 C223 C224 . . . 115(3) ? C222 C223 H223a . . . 108 ? C222 C223 H223b . . . 108 ? C224 C223 H223a . . . 108 ? C224 C223 H223b . . . 108 ? H223a C223 H223b . . . 109 ? C223 C224 H224a . . . 109 ? C223 C224 H224b . . . 109 ? C223 C224 H224c . . . 109 ? H224a C224 H224b . . . 110 ? H224a C224 H224c . . . 110 ? H224b C224 H224c . . . 110 ? N22 C23 C24 . . . 111.8(19) ? N22 C23 H23 . . . 124 ? C24 C23 H23 . . . 124 ? C23 C24 N25 . . . 103.2(19) ? C23 C24 H24 . . . 128 ? N25 C24 H24 . . . 128 ? C21 N25 C24 . . . 111.8(19) ? C21 N25 C251 . . . 123.6(18) ? C24 N25 C251 . . . 125(2) ? N25 C251 C252 . . . 116(3) ? N25 C251 H251a . . . 108 ? N25 C251 H251b . . . 108 ? C252 C251 H251a . . . 108 ? C252 C251 H251b . . . 108 ? H251a C251 H251b . . . 110 ? C251 C252 C253 . . . 103(3) ? C251 C252 H252a . . . 111 ? C251 C252 H252b . . . 110 ? C253 C252 H252a . . . 111 ? C253 C252 H252b . . . 112 ? H252a C252 H252b . . . 109 ? C252 C253 C254 . . . 106(4) ? C252 C253 H253a . . . 108 ? C252 C253 H253b . . . 110 ? C254 C253 H253a . . . 110 ? C254 C253 H253b . . . 115 ? H253a C253 H253b . . . 107 ? C253 C254 H254a . . . 106 ? C253 C254 H254b . . . 103 ? C253 C254 H254c . . . 108 ? H254a C254 H254b . . . 110 ? H254a C254 H254c . . . 116 ? H254b C254 H254c . . . 113 ? Au3 C31 N32 . . . 126.3(9) ? Au3 C31 N35 . . . 129.2(11) ? N32 C31 N35 . . . 104.4(12) ? C31 N32 C321 . . . 123.6(14) ? C31 N32 C33 . . . 108.7(12) ? C321 N32 C33 . . . 127.2(14) ? N32 C321 C322 . . . 109.0(12) ? N32 C321 H321a . . . 109.5 ? N32 C321 H321b . . . 109.6 ? C322 C321 H321a . . . 109.6 ? C322 C321 H321b . . . 109.7 ? H321a C321 H321b . . . 109.4 ? C321 C322 C323 . . . 109.4(16) ? C321 C322 H322a . . . 109.3 ? C321 C322 H322b . . . 109.4 ? C323 C322 H322a . . . 110 ? C323 C322 H322b . . . 109.5 ? H322a C322 H322b . . . 109.6 ? C322 C323 C324 . . . 109(2) ? C322 C323 H323a . . . 109 ? C322 C323 H323b . . . 109 ? C324 C323 H323a . . . 110 ? C324 C323 H323b . . . 110 ? H323a C323 H323b . . . 109 ? C323 C324 H324a . . . 109 ? C323 C324 H324b . . . 109 ? C323 C324 H324c . . . 109 ? H324a C324 H324b . . . 110 ? H324a C324 H324c . . . 109 ? H324b C324 H324c . . . 110 ? N32 C33 C34 . . . 106.1(15) ? N32 C33 H33 . . . 126.9 ? C34 C33 H33 . . . 127.0 ? C33 C34 N35 . . . 109.7(15) ? C33 C34 H34 . . . 125.1 ? N35 C34 H34 . . . 125.2 ? C31 N35 C34 . . . 110.9(12) ? C31 N35 C351 . . . 124.5(13) ? C34 N35 C351 . . . 124.5(12) ? N35 C351 C352 . . . 110.7(12) ? N35 C351 H351a . . . 109.2 ? N35 C351 H351b . . . 109.2 ? C352 C351 H351a . . . 109.2 ? C352 C351 H351b . . . 109.1 ? H351a C351 H351b . . . 109.4 ? C351 C352 C353 . . . 108.4(18) ? C351 C352 H352a . . . 109.7 ? C351 C352 H352b . . . 110 ? C353 C352 H352a . . . 110 ? C353 C352 H352b . . . 110 ? H352a C352 H352b . . . 109.6 ? C352 C353 C354 . . . 109(3) ? C352 C353 H353a . . . 109 ? C352 C353 H353b . . . 109 ? C354 C353 H353a . . . 110 ? C354 C353 H353b . . . 110 ? H353a C353 H353b . . . 109 ? C353 C354 H354a . . . 109 ? C353 C354 H354b . . . 109 ? C353 C354 H354c . . . 109 ? H354a C354 H354b . . . 110 ? H354a C354 H354c . . . 110 ? H354b C354 H354c . . . 110 ? Au3 C41 N42 . . . 126.3(11) ? Au3 C41 N45 . . . 126.5(12) ? N42 C41 N45 . . . 107.2(15) ? C41 N42 C421 . . . 122.9(16) ? C41 N42 C43 . . . 107.2(14) ? C421 N42 C43 . . . 129.7(17) ? N42 C421 C422 . . . 110(2) ? N42 C421 H421a . . . 109 ? N42 C421 H421b . . . 109 ? C422 C421 H421a . . . 109 ? C422 C421 H421b . . . 109 ? H421a C421 H421b . . . 109 ? C421 C422 C423 . . . 109(3) ? C421 C422 H422a . . . 109 ? C421 C422 H422b . . . 110 ? C423 C422 H422a . . . 109 ? C423 C422 H422b . . . 110 ? H422a C422 H422b . . . 110 ? C422 C423 C424 . . . 108(3) ? C422 C423 H423a . . . 110 ? C422 C423 H423b . . . 110 ? C424 C423 H423a . . . 110 ? C424 C423 H423b . . . 110 ? H423a C423 H423b . . . 109 ? C423 C424 H424a . . . 109 ? C423 C424 H424b . . . 109 ? C423 C424 H424c . . . 110 ? H424a C424 H424b . . . 109 ? H424a C424 H424c . . . 110 ? H424b C424 H424c . . . 110 ? N42 C43 C44 . . . 108(2) ? N42 C43 H43 . . . 126 ? C44 C43 H43 . . . 126 ? C43 C44 N45 . . . 109.5(18) ? C43 C44 H44 . . . 125 ? N45 C44 H44 . . . 125.2 ? C41 N45 C44 . . . 108.4(15) ? C41 N45 C451 . . . 127.1(17) ? C44 N45 C451 . . . 124.4(16) ? N45 C451 C452 . . . 109.4(15) ? N45 C451 H451a . . . 110 ? N45 C451 H451b . . . 110 ? C452 C451 H451a . . . 109 ? C452 C451 H451b . . . 109 ? H451a C451 H451b . . . 109.5 ? C451 C452 C453 . . . 109.2(19) ? C451 C452 H452a . . . 110 ? C451 C452 H452b . . . 110 ? C453 C452 H452a . . . 110 ? C453 C452 H452b . . . 110 ? H452a C452 H452b . . . 109 ? C452 C453 C454 . . . 109(3) ? C452 C453 H453a . . . 109 ? C452 C453 H453b . . . 110 ? C454 C453 H453a . . . 109 ? C454 C453 H453b . . . 110 ? H453a C453 H453b . . . 110 ? C453 C454 H454a . . . 109 ? C453 C454 H454b . . . 109 ? C453 C454 H454c . . . 110 ? H454a C454 H454b . . . 109 ? H454a C454 H454c . . . 109 ? H454b C454 H454c . . . 110 ? F11 P1 F12 . . . 92.6(7) ? F11 P1 F13 . . . 178.5(6) ? F11 P1 F14 . . . 89.4(6) ? F11 P1 F15 . . . 92.1(7) ? F11 P1 F16 . . . 91.7(7) ? F12 P1 F13 . . . 88.9(6) ? F12 P1 F14 . . . 177.4(7) ? F12 P1 F15 . . . 86.2(8) ? F12 P1 F16 . . . 87.8(7) ? F13 P1 F14 . . . 89.1(6) ? F13 P1 F15 . . . 88.0(6) ? F13 P1 F16 . . . 88.4(6) ? F14 P1 F15 . . . 95.4(9) ? F14 P1 F16 . . . 90.5(7) ? F15 P1 F16 . . . 173.1(7) ? F21 P2 F22 . . . 91.0(6) ? F21 P2 F23 . . . 179.5(6) ? F21 P2 F24 . . . 90.7(6) ? F21 P2 F25 . . . 89.7(7) ? F21 P2 F26 . . . 90.7(5) ? F22 P2 F23 . . . 89.1(6) ? F22 P2 F24 . . . 178.1(7) ? F22 P2 F25 . . . 87.5(6) ? F22 P2 F26 . . . 91.7(5) ? F23 P2 F24 . . . 89.2(6) ? F23 P2 F25 . . . 90.8(7) ? F23 P2 F26 . . . 88.8(6) ? F24 P2 F25 . . . 91.6(6) ? F24 P2 F26 . . . 89.2(5) ? F25 P2 F26 . . . 179.0(6) ? 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 1392 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 19 _reflns_limit_k_min -19 _reflns_limit_k_max 20 _reflns_limit_l_min -20 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .708 _reflns_d_resolution_low 14.268 _diffrn_reflns_av_sigmaI/netI .188 _diffrn_reflns_theta_min 1.42 _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 30 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .149 _refine_ls_wR_factor_all .14 _refine_ls_goodness_of_fit_all 1.013 _refine_ls_shift/su_mean .0004 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-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 block for single structure (one for each study in the paper) #======================================================================= data_5.pf6 _database_code_depnum_ccdc_archive 'CCDC 298910' _audit_creation_method Xtal3.6 _audit_creation_date 03-06-23 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C22 H40 Au1 F6 N4 P1' _chemical_formula_moiety ? _chemical_formula_weight 702.52 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 9.7407(6) _cell_length_b 22.1350(10) _cell_length_c 12.4258(7) _cell_angle_alpha 90.00000 _cell_angle_beta 92.6420(10) _cell_angle_gamma 90.00000 _cell_volume 2676.3(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8409 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 37.48 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 5.616 _exptl_crystal_description slab _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour colorless _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 .44 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 54936 _reflns_number_total 14051 _reflns_Friedel_coverage 0 _reflns_number_gt 11885 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.5 _diffrn_reflns_theta_full 37.5 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full .99 _diffrn_reflns_av_R_equivalents .043 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .036 _refine_ls_wR_factor_ref .061 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_number_reflns 11885 _refine_ls_number_parameters 307 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .009 _refine_diff_density_min -2.941 _refine_diff_density_max 4.484 _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 88 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 160 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' F ? 0 24 .014 .01 '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' P ? 0 4 .09 .095 '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 .772472(10) .128559(5) .527183(8) .01565(5) Uani ? ? 1.00000 ? ? C11 .7390(3) .12755(11) .6879(2) .0149(10) Uani ? ? 1.00000 ? ? N12 .6385(3) .15688(12) .7402(2) .0183(10) Uani ? ? 1.00000 ? ? C121 .5374(3) .20270(14) .6945(3) .0203(12) Uani ? ? 1.00000 ? ? C122 .6027(4) .24191(19) .6113(4) .038(2) Uani ? ? 1.00000 ? ? C123 .4137(4) .16875(18) .6466(3) .0313(17) Uani ? ? 1.00000 ? ? C124 .4928(4) .24370(19) .7854(3) .0336(18) Uani ? ? 1.00000 ? ? C13 .6349(4) .13586(17) .8444(3) .0256(15) Uani ? ? 1.00000 ? ? C14 .7347(4) .09448(17) .8587(3) .0254(14) Uani ? ? 1.00000 ? ? N15 .7991(3) .08974(12) .7626(2) .0178(10) Uani ? ? 1.00000 ? ? C151 .9274(3) .05295(14) .7485(3) .0212(12) Uani ? ? 1.00000 ? ? C152 1.0419(3) .09627(17) .7230(3) .0262(14) Uani ? ? 1.00000 ? ? C153 .9028(4) .00611(17) .6590(3) .0327(17) Uani ? ? 1.00000 ? ? C154 .9659(4) .02018(18) .8532(3) .0318(17) Uani ? ? 1.00000 ? ? C21 .7969(3) .12474(13) .3657(3) .0178(11) Uani ? ? 1.00000 ? ? N22 .7248(3) .08890(13) .2937(2) .0199(10) Uani ? ? 1.00000 ? ? C221 .6074(3) .04815(14) .3191(2) .0208(12) Uani ? ? 1.00000 ? ? C222 .4869(3) .08739(17) .3515(3) .0250(14) Uani ? ? 1.00000 ? ? C223 .6517(4) .00463(16) .4085(3) .0250(14) Uani ? ? 1.00000 ? ? C224 .5653(4) .01133(19) .2181(3) .0310(17) Uani ? ? 1.00000 ? ? C23 .7695(4) .09833(17) .1912(3) .0270(15) Uani ? ? 1.00000 ? ? C24 .8725(4) .13949(18) .1992(3) .0292(16) Uani ? ? 1.00000 ? ? N25 .8874(3) .15605(12) .3059(2) .0199(10) Uani ? ? 1.00000 ? ? C251 .9912(3) .20097(15) .3489(3) .0241(13) Uani ? ? 1.00000 ? ? C252 .9203(4) .24933(18) .4136(4) .0342(18) Uani ? ? 1.00000 ? ? C253 1.1016(4) .1678(2) .4165(4) .042(2) Uani ? ? 1.00000 ? ? C254 1.0579(5) .2321(2) .2544(4) .036(2) Uani ? ? 1.00000 ? ? P .27439(8) .37518(4) .52735(6) .0211(4) Uani ? ? 1.00000 ? ? F1 .1106(3) .37293(10) .5112(3) .0322(12) Uani ? ? 1.00000 ? ? F2 .2592(3) .38791(15) .6522(2) .0389(13) Uani ? ? 1.00000 ? ? F3 .4396(3) .37678(12) .5438(3) .0356(13) Uani ? ? 1.00000 ? ? F4 .2893(4) .36252(16) .4018(2) .0456(16) Uani ? ? 1.00000 ? ? F5 .2726(3) .44637(14) .5051(3) .0421(14) Uani ? ? 1.00000 ? ? F6 .2761(3) .30406(14) .5489(3) .0440(15) Uani ? ? 1.00000 ? ? H122a .67988 .26211 .64359 .05800 Uiso ? ? 1.00000 ? ? H122b .53795 .27031 .58350 .05800 Uiso ? ? 1.00000 ? ? H122c .63232 .21693 .55398 .05800 Uiso ? ? 1.00000 ? ? H123a .37470 .14463 .70053 .04700 Uiso ? ? 1.00000 ? ? H123b .44125 .14341 .58951 .04700 Uiso ? ? 1.00000 ? ? H123c .34687 .19679 .61902 .04700 Uiso ? ? 1.00000 ? ? H124a .45138 .22007 .83948 .05300 Uiso ? ? 1.00000 ? ? H124b .42902 .27286 .75843 .05300 Uiso ? ? 1.00000 ? ? H124c .57133 .26381 .81750 .05300 Uiso ? ? 1.00000 ? ? H13 .57147 .14813 .89659 .03200 Uiso ? ? 1.00000 ? ? H14 .75711 .07280 .92324 .03200 Uiso ? ? 1.00000 ? ? H152a 1.05484 .12484 .77947 .04000 Uiso ? ? 1.00000 ? ? H152b 1.01861 .11701 .65738 .04000 Uiso ? ? 1.00000 ? ? H152c 1.12484 .07434 .71499 .04000 Uiso ? ? 1.00000 ? ? H153a .83084 -.02042 .67699 .05000 Uiso ? ? 1.00000 ? ? H153b .98474 -.01661 .65064 .05000 Uiso ? ? 1.00000 ? ? H153c .87851 .02605 .59303 .05000 Uiso ? ? 1.00000 ? ? H154a .89470 -.00731 .86971 .04800 Uiso ? ? 1.00000 ? ? H154b .97926 .04835 .90980 .04800 Uiso ? ? 1.00000 ? ? H154c 1.04885 -.00204 .84480 .04800 Uiso ? ? 1.00000 ? ? H222a .46163 .11426 .29433 .03800 Uiso ? ? 1.00000 ? ? H222b .51337 .11020 .41407 .03800 Uiso ? ? 1.00000 ? ? H222c .41111 .06238 .36656 .03800 Uiso ? ? 1.00000 ? ? H223a .72684 -.01915 .38629 .03800 Uiso ? ? 1.00000 ? ? H223b .57733 -.02120 .42409 .03800 Uiso ? ? 1.00000 ? ? H223c .67959 .02662 .47160 .03800 Uiso ? ? 1.00000 ? ? H224a .63979 -.01325 .19758 .04900 Uiso ? ? 1.00000 ? ? H224b .53928 .03773 .16013 .04900 Uiso ? ? 1.00000 ? ? H224c .48897 -.01408 .23258 .04900 Uiso ? ? 1.00000 ? ? H23 .73460 .07951 .12708 .03400 Uiso ? ? 1.00000 ? ? H24 .92465 .15398 .14159 .03600 Uiso ? ? 1.00000 ? ? H252a .85167 .26897 .36914 .05200 Uiso ? ? 1.00000 ? ? H252b .98539 .27829 .43990 .05200 Uiso ? ? 1.00000 ? ? H252c .87727 .23125 .47337 .05200 Uiso ? ? 1.00000 ? ? H253a 1.14309 .13785 .37298 .06300 Uiso ? ? 1.00000 ? ? H253b 1.06127 .14840 .47552 .06300 Uiso ? ? 1.00000 ? ? H253c 1.16939 .19544 .44205 .06300 Uiso ? ? 1.00000 ? ? H254a 1.10406 .20339 .21261 .05500 Uiso ? ? 1.00000 ? ? H254b 1.12332 .26142 .28168 .05500 Uiso ? ? 1.00000 ? ? H254c .98973 .25222 .21071 .05500 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 .01841(6) .01472(5) .01391(5) -.00016(3) .00181(3) -.00129(3) C11 .0189(11) .0117(10) .0142(10) .0010(8) .0015(8) -.0011(7) N12 .0216(11) .0169(10) .0167(9) .0014(8) .0040(8) -.0006(8) C121 .0215(12) .0164(12) .0234(12) .0024(9) .0046(10) -.0018(10) C122 .0331(18) .0276(17) .054(3) .0103(14) .0175(17) .0171(17) C123 .0307(17) .0256(16) .0369(18) .0019(13) -.0073(14) -.0046(14) C124 .0366(19) .0276(17) .037(2) .0076(14) .0045(15) -.0130(15) C13 .0300(16) .0311(17) .0163(12) .0017(12) .0080(11) .0012(11) C14 .0310(15) .0300(16) .0154(11) .0002(12) .0032(10) .0036(11) N15 .0213(10) .0167(10) .0153(9) .0006(8) .0000(8) .0008(8) C151 .0208(12) .0161(12) .0262(13) .0005(9) -.0042(10) -.0013(10) C152 .0199(13) .0270(15) .0316(16) .0004(11) .0004(11) .0022(12) C153 .0339(18) .0223(15) .041(2) .0064(13) -.0092(15) -.0132(14) C154 .0336(18) .0256(16) .0352(18) .0016(13) -.0085(14) .0104(14) C21 .0189(11) .0186(12) .0160(11) -.0001(9) .0005(9) -.0006(8) N22 .0255(12) .0207(11) .0137(9) -.0010(9) .0022(8) -.0030(8) C221 .0260(13) .0190(12) .0171(11) -.0033(10) -.0003(10) -.0022(9) C222 .0212(13) .0275(15) .0264(14) .0001(11) .0016(11) -.0014(12) C223 .0292(15) .0216(14) .0242(14) -.0038(11) .0018(11) .0011(11) C224 .040(2) .0303(17) .0225(14) -.0083(14) -.0019(13) -.0076(12) C23 .0380(18) .0296(16) .0138(11) -.0030(13) .0067(11) -.0028(11) C24 .039(2) .0285(16) .0203(14) -.0049(14) .0103(13) .0002(12) N25 .0221(11) .0182(11) .0197(10) -.0007(8) .0055(8) -.0012(8) C251 .0234(13) .0199(13) .0295(15) -.0032(10) .0080(11) -.0003(11) C252 .0351(18) .0251(16) .044(2) -.0077(13) .0182(16) -.0118(15) C253 .0306(19) .035(2) .058(3) -.0081(15) -.0092(18) .012(2) C254 .040(2) .0283(18) .042(2) -.0090(15) .0211(17) .0011(15) P .0213(4) .0244(4) .0174(4) .0031(3) .0004(3) -.0003(2) F1 .0248(11) .0361(14) .0355(14) .0010(8) -.0021(9) -.0008(9) F2 .0409(14) .0586(17) .0176(9) -.0010(13) .0049(9) -.0056(11) F3 .0225(10) .0492(16) .0351(13) .0047(9) .0014(9) -.0012(10) F4 .0442(16) .076(2) .0169(10) .0116(14) .0034(10) -.0096(11) F5 .0408(15) .0289(13) .0578(15) .0025(10) .0139(12) .0107(12) F6 .0450(16) .0259(13) .0609(17) .0072(10) .0007(13) .0041(12) # 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 C11 . . 2.038(3) ? Au C21 . . 2.033(3) ? C11 N12 . . 1.364(4) ? C11 N15 . . 1.362(4) ? N12 C121 . . 1.507(4) ? N12 C13 . . 1.378(4) ? C121 C122 . . 1.512(6) ? C121 C123 . . 1.517(5) ? C121 C124 . . 1.527(5) ? C122 H122a . . .948 ? C122 H122b . . .944 ? C122 H122c . . .957 ? C123 H123a . . .950 ? C123 H123b . . .952 ? C123 H123c . . .952 ? C124 H124a . . .955 ? C124 H124b . . .946 ? C124 H124c . . .956 ? C13 C14 . . 1.341(5) ? C13 H13 . . .955 ? C14 N15 . . 1.379(4) ? C14 H14 . . .951 ? N15 C151 . . 1.508(4) ? C151 C152 . . 1.516(5) ? C151 C153 . . 1.532(5) ? C151 C154 . . 1.521(5) ? C152 H152a . . .949 ? C152 H152b . . .954 ? C152 H152c . . .952 ? C153 H153a . . .949 ? C153 H153b . . .953 ? C153 H153c . . .951 ? C154 H154a . . .952 ? C154 H154b . . .944 ? C154 H154c . . .956 ? C21 N22 . . 1.366(4) ? C21 N25 . . 1.367(4) ? N22 C221 . . 1.502(4) ? N22 C23 . . 1.380(4) ? C221 C222 . . 1.529(5) ? C221 C223 . . 1.517(5) ? C221 C224 . . 1.537(5) ? C222 H222a . . .950 ? C222 H222b . . .953 ? C222 H222c . . .948 ? C223 H223a . . .952 ? C223 H223b . . .950 ? C223 H223c . . .952 ? C224 H224a . . .951 ? C224 H224b . . .952 ? C224 H224c . . .956 ? C23 C24 . . 1.356(6) ? C23 H23 . . .948 ? C24 N25 . . 1.377(5) ? C24 H24 . . .952 ? N25 C251 . . 1.499(4) ? C251 C252 . . 1.523(5) ? C251 C253 . . 1.522(6) ? C251 C254 . . 1.532(6) ? C252 H252a . . .953 ? C252 H252b . . .949 ? C252 H252c . . .957 ? C253 H253a . . .957 ? C253 H253b . . .950 ? C253 H253c . . .944 ? C254 H254a . . .947 ? C254 H254b . . .960 ? C254 H254c . . .949 ? P F1 . . 1.599(3) ? P F2 . . 1.590(3) ? P F3 . . 1.613(3) ? P F4 . . 1.598(3) ? P F5 . . 1.600(3) ? P F6 . . 1.597(3) ? 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 Au C21 . . . 176.11(11) ? Au C11 N12 . . . 127.8(2) ? Au C11 N15 . . . 126.2(2) ? N12 C11 N15 . . . 105.3(3) ? C11 N12 C121 . . . 127.7(3) ? C11 N12 C13 . . . 109.7(3) ? C121 N12 C13 . . . 122.5(3) ? N12 C121 C122 . . . 110.8(3) ? N12 C121 C123 . . . 107.9(3) ? N12 C121 C124 . . . 108.9(3) ? C122 C121 C123 . . . 111.5(3) ? C122 C121 C124 . . . 107.9(3) ? C123 C121 C124 . . . 109.7(3) ? C121 C122 H122a . . . 109.4 ? C121 C122 H122b . . . 109.7 ? C121 C122 H122c . . . 109.2 ? H122a C122 H122b . . . 110.1 ? H122a C122 H122c . . . 109.1 ? H122b C122 H122c . . . 109.4 ? C121 C123 H123a . . . 109.7 ? C121 C123 H123b . . . 109.8 ? C121 C123 H123c . . . 109.6 ? H123a C123 H123b . . . 109.3 ? H123a C123 H123c . . . 109.3 ? H123b C123 H123c . . . 109.1 ? C121 C124 H124a . . . 109.8 ? C121 C124 H124b . . . 110.3 ? C121 C124 H124c . . . 109.6 ? H124a C124 H124b . . . 109.3(4) ? H124a C124 H124c . . . 108.5 ? H124b C124 H124c . . . 109.2 ? N12 C13 C14 . . . 107.8(3) ? N12 C13 H13 . . . 125.9 ? C14 C13 H13 . . . 126.3 ? C13 C14 N15 . . . 107.1(3) ? C13 C14 H14 . . . 126.3 ? N15 C14 H14 . . . 126.6 ? C11 N15 C14 . . . 110.2(3) ? C11 N15 C151 . . . 125.8(3) ? C14 N15 C151 . . . 123.6(3) ? N15 C151 C152 . . . 107.7(3) ? N15 C151 C153 . . . 110.3(3) ? N15 C151 C154 . . . 109.4(3) ? C152 C151 C153 . . . 111.6(3) ? C152 C151 C154 . . . 109.0(3) ? C153 C151 C154 . . . 108.8(3) ? C151 C152 H152a . . . 109.9 ? C151 C152 H152b . . . 109.6 ? C151 C152 H152c . . . 109.6 ? H152a C152 H152b . . . 109.2 ? H152a C152 H152c . . . 109.4 ? H152b C152 H152c . . . 109.0 ? C151 C153 H153a . . . 109.9 ? C151 C153 H153b . . . 109.4 ? C151 C153 H153c . . . 109.6 ? H153a C153 H153b . . . 109.3 ? H153a C153 H153c . . . 109.5 ? H153b C153 H153c . . . 109.1 ? C151 C154 H154a . . . 109.6 ? C151 C154 H154b . . . 110.0 ? C151 C154 H154c . . . 109.2 ? H154a C154 H154b . . . 109.8 ? H154a C154 H154c . . . 108.8 ? H154b C154 H154c . . . 109.5 ? Au C21 N22 . . . 126.2(2) ? Au C21 N25 . . . 128.5(2) ? N22 C21 N25 . . . 105.2(3) ? C21 N22 C221 . . . 125.7(3) ? C21 N22 C23 . . . 110.0(3) ? C221 N22 C23 . . . 124.1(3) ? N22 C221 C222 . . . 108.4(3) ? N22 C221 C223 . . . 110.0(3) ? N22 C221 C224 . . . 108.9(3) ? C222 C221 C223 . . . 111.4(3) ? C222 C221 C224 . . . 109.7(3) ? C223 C221 C224 . . . 108.5(3) ? C221 C222 H222a . . . 109.6 ? C221 C222 H222b . . . 109.5 ? C221 C222 H222c . . . 109.5 ? H222a C222 H222b . . . 109.2 ? H222a C222 H222c . . . 109.6 ? H222b C222 H222c . . . 109.4 ? C221 C223 H223a . . . 109.6 ? C221 C223 H223b . . . 109.7 ? C221 C223 H223c . . . 109.8 ? H223a C223 H223b . . . 109.3 ? H223a C223 H223c . . . 109.1 ? H223b C223 H223c . . . 109.3 ? C221 C224 H224a . . . 110.1 ? C221 C224 H224b . . . 110.1 ? C221 C224 H224c . . . 109.8 ? H224a C224 H224b . . . 109.2 ? H224a C224 H224c . . . 108.9 ? H224b C224 H224c . . . 108.8 ? N22 C23 C24 . . . 107.3(3) ? N22 C23 H23 . . . 126.4 ? C24 C23 H23 . . . 126.3 ? C23 C24 N25 . . . 107.1(3) ? C23 C24 H24 . . . 126.2 ? N25 C24 H24 . . . 126.8 ? C21 N25 C24 . . . 110.3(3) ? C21 N25 C251 . . . 125.7(3) ? C24 N25 C251 . . . 124.0(3) ? N25 C251 C252 . . . 109.8(3) ? N25 C251 C253 . . . 108.9(3) ? N25 C251 C254 . . . 109.2(3) ? C252 C251 C253 . . . 111.9(3) ? C252 C251 C254 . . . 107.9(3) ? C253 C251 C254 . . . 109.0(3) ? C251 C252 H252a . . . 109.7 ? C251 C252 H252b . . . 110.1 ? C251 C252 H252c . . . 109.9 ? H252a C252 H252b . . . 109.3 ? H252a C252 H252c . . . 108.7 ? H252b C252 H252c . . . 109.0 ? C251 C253 H253a . . . 109.2 ? C251 C253 H253b . . . 109.7 ? C251 C253 H253c . . . 109.7 ? H253a C253 H253b . . . 108.9 ? H253a C253 H253c . . . 109.4 ? H253b C253 H253c . . . 110.0 ? C251 C254 H254a . . . 110.3 ? C251 C254 H254b . . . 109.3 ? C251 C254 H254c . . . 109.8 ? H254a C254 H254b . . . 108.9 ? H254a C254 H254c . . . 109.8 ? H254b C254 H254c . . . 108.7 ? F1 P F2 . . . 89.48(16) ? F1 P F3 . . . 179.47(14) ? F1 P F4 . . . 90.39(17) ? F1 P F5 . . . 90.36(13) ? F1 P F6 . . . 89.60(13) ? F2 P F3 . . . 90.57(16) ? F2 P F4 . . . 179.8(2) ? F2 P F5 . . . 89.63(17) ? F2 P F6 . . . 90.66(17) ? F3 P F4 . . . 89.57(17) ? F3 P F5 . . . 90.17(14) ? F3 P F6 . . . 89.87(14) ? F4 P F5 . . . 90.25(17) ? F4 P F6 . . . 89.46(17) ? F5 P F6 . . . 179.7(2) ? 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 direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _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 1392 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 16 _reflns_limit_k_min 0 _reflns_limit_k_max 37 _reflns_limit_l_min -21 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .583 _reflns_d_resolution_low 10.803 _diffrn_reflns_av_sigmaI/netI .044 _diffrn_reflns_theta_min 1.88 _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 .047 _refine_ls_wR_factor_all .065 _refine_ls_goodness_of_fit_all 1.075 _refine_ls_shift/su_mean .0005 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-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 block for single structure (one for each study in the paper) #======================================================================= data_6.pf6 _database_code_depnum_ccdc_archive 'CCDC 298911' _audit_creation_method Xtal3.6 _audit_creation_date 03-06-24 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C30 H48 Au1 F6 N4 P1' _chemical_formula_moiety ? _chemical_formula_weight 806.67 _chemical_melting_point ? _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P_43_2_2 _symmetry_space_group_name_Hall p_4cw_2c loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z +x,-y,1/2-z -x,-y,1/2+z -x,+y,-z +y,+x,1/4-z +y,-x,1/4+z -y,+x,3/4+z -y,-x,3/4-z _cell_length_a 14.2018(8) _cell_length_b 14.2018(8) _cell_length_c 16.8340(10) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 3395.3(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8344 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.14 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 4.438 _exptl_crystal_description polyhedron _exptl_crystal_size_max .29 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .16 _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 .73 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 54843 _reflns_number_total 3560 _reflns_Friedel_coverage .99 _reflns_number_gt 3036 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 32.5 _diffrn_reflns_theta_full 32.5 _diffrn_measured_fraction_theta_max .99 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .058 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .049 _refine_ls_wR_factor_ref .08 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_number_reflns 3016 _refine_ls_number_parameters 194 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .002 _refine_diff_density_min -3.157 _refine_diff_density_max 2.429 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack xabs refined' _refine_ls_abs_structure_Flack .28(3) # 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 ? 0 120 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 192 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' F ? 0 24 .014 .01 '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' P ? 0 4 .09 .095 '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 .50000 .76908(3) .50000 .0298(2) Uani ? ? 1.00000 ? ? C11 .50000 .6304(8) .50000 .035(6) Uani ? ? 1.00000 ? ? N12 .5755(6) .5697(6) .4969(9) .038(4) Uani ? ? 1.00000 ? ? C121 .6736(8) .6033(8) .4917(8) .040(5) Uani ? ? 1.00000 ? ? C122 .7067(9) .6103(10) .4044(9) .045(6) Uani ? ? 1.00000 ? ? C123 .8049(12) .6494(15) .4029(11) .056(9) Uani ? ? 1.00000 ? ? C124 .8722(11) .5909(12) .4515(11) .053(8) Uani ? ? 1.00000 ? ? C125 .8361(12) .5865(13) .5358(11) .057(9) Uani ? ? 1.00000 ? ? C126 .7412(10) .5421(14) .5392(10) .061(9) Uani ? ? 1.00000 ? ? C13 .5448(11) .4766(8) .4993(18) .062(7) Uani ? ? 1.00000 ? ? C21 .50000 .9113(8) .50000 .030(5) Uani ? ? 1.00000 ? ? N22 .5713(6) .9681(7) .4786(6) .035(4) Uani ? ? 1.00000 ? ? C221 .6626(8) .9342(7) .4507(7) .035(5) Uani ? ? 1.00000 ? ? C222 .6758(9) .9503(10) .3622(9) .047(7) Uani ? ? 1.00000 ? ? C223 .7657(12) .9120(9) .3314(10) .056(8) Uani ? ? 1.00000 ? ? C224 .8499(17) .9558(12) .3788(17) .090(13) Uani ? ? 1.00000 ? ? C225 .8347(11) .9389(13) .4702(15) .076(12) Uani ? ? 1.00000 ? ? C226 .7411(9) .9794(12) .4950(17) .063(9) Uani ? ? 1.00000 ? ? C23 .5449(9) 1.0614(8) .4858(7) .039(6) Uani ? ? 1.00000 ? ? P .72511(19) .72509(19) .12500 .0344(13) Uani ? ? 1.00000 ? ? F1 .6508(10) .6508(10) .12500 .18(2) Uani ? ? 1.00000 ? ? F2 .6520(12) .7925(10) .1645(9) .094(10) Uani ? ? 1.00000 ? ? F3 .8004(10) .8004(10) .12500 .16(2) Uani ? ? 1.00000 ? ? F4 .7492(17) .6926(15) .2089(11) .159(18) Uani ? ? 1.00000 ? ? H121 .67405 .66537 .51363 .05000 Uiso ? ? 1.00000 ? ? H122a .66632 .65145 .37524 .05800 Uiso ? ? 1.00000 ? ? H122b .70588 .54982 .38041 .05800 Uiso ? ? 1.00000 ? ? H123a .80549 .71145 .42399 .07500 Uiso ? ? 1.00000 ? ? H123b .82817 .65075 .34980 .07500 Uiso ? ? 1.00000 ? ? H124a .93377 .61939 .45018 .06600 Uiso ? ? 1.00000 ? ? H124b .87624 .52963 .43013 .06600 Uiso ? ? 1.00000 ? ? H125a .83373 .65025 .55651 .07000 Uiso ? ? 1.00000 ? ? H125b .87956 .55193 .56733 .07000 Uiso ? ? 1.00000 ? ? H126a .74381 .48198 .51982 .07200 Uiso ? ? 1.00000 ? ? H126b .72107 .54217 .59430 .07200 Uiso ? ? 1.00000 ? ? H13 .58701 .42371 .49743 .07200 Uiso ? ? 1.00000 ? ? H221 .66759 .86959 .46137 .04200 Uiso ? ? 1.00000 ? ? H222a .67313 1.01793 .34978 .05800 Uiso ? ? 1.00000 ? ? H222b .62307 .92287 .33308 .05800 Uiso ? ? 1.00000 ? ? H223a .77305 .92452 .27563 .07800 Uiso ? ? 1.00000 ? ? H223b .76565 .84476 .33828 .07800 Uiso ? ? 1.00000 ? ? H224a .85231 1.02082 .36665 .11100 Uiso ? ? 1.00000 ? ? H224b .90652 .92618 .36160 .11100 Uiso ? ? 1.00000 ? ? H225a .88577 .97167 .49466 .08800 Uiso ? ? 1.00000 ? ? H225b .83794 .87534 .47854 .08800 Uiso ? ? 1.00000 ? ? H226a .73420 .96766 .55214 .08300 Uiso ? ? 1.00000 ? ? H226b .73984 1.04705 .48902 .08300 Uiso ? ? 1.00000 ? ? H23 .58177 1.11644 .47391 .05100 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 .0363(2) .0270(2) .0261(2) .00000 .0040(3) .00000 C11 .057(7) .023(5) .024(5) .00000 .015(9) .00000 N12 .047(4) .024(3) .042(5) -.000(3) .018(6) -.002(4) C121 .049(5) .035(4) .035(6) .013(4) .003(5) .003(5) C122 .040(6) .044(6) .049(7) .002(5) -.003(5) .009(5) C123 .045(7) .062(10) .060(9) .000(6) .014(6) .019(8) C124 .041(7) .058(8) .060(9) .016(6) -.006(6) .017(7) C125 .054(9) .069(10) .049(8) -.011(8) -.005(7) .008(7) C126 .046(7) .081(10) .057(9) .014(7) .003(6) .036(8) C13 .077(8) .030(5) .078(9) -.003(4) .021(14) .009(7) C21 .034(5) .022(5) .033(6) .00000 .009(9) .00000 N22 .033(4) .032(4) .039(5) -.002(3) .003(3) .009(3) C221 .043(5) .029(4) .033(5) .002(4) .004(4) -.005(4) C222 .044(6) .049(7) .049(7) .005(5) .017(5) -.004(5) C223 .067(8) .036(6) .064(9) .003(6) .027(8) .005(6) C224 .095(14) .045(8) .129(18) -.016(9) .067(14) -.031(10) C225 .043(7) .060(9) .126(19) -.003(6) -.016(8) -.045(10) C226 .046(6) .076(12) .067(10) .004(5) .003(10) -.014(9) C23 .045(5) .031(5) .040(7) -.001(4) -.001(5) -.002(4) P .0280(9) .0280(9) .047(2) -.0002(13) -.0032(10) .0032(10) F1 .19(2) .19(2) .15(2) -.14(3) .09(2) -.09(2) F2 .092(10) .092(10) .097(10) .038(7) .022(8) -.019(8) F3 .131(14) .131(14) .22(3) -.072(16) .096(18) -.096(18) F4 .20(2) .20(2) .083(10) .11(2) -.008(12) -.001(11) # 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 C11 . . 1.970(12) ? Au C21 . . 2.020(11) ? C11 N12 . . 1.376(11) ? C11 N12 . '4 656' 1.376(11) ? N12 C121 . . 1.476(15) ? N12 C13 . . 1.393(14) ? C121 C122 . . 1.55(2) ? C121 C126 . . 1.52(2) ? C121 H121 . . .955 ? C122 C123 . . 1.50(2) ? C122 H122a . . .955 ? C122 H122b . . .950 ? C123 C124 . . 1.51(2) ? C123 H123a . . .95 ? C123 H123b . . .953 ? C124 C125 . . 1.51(3) ? C124 H124a . . .964 ? C124 H124b . . .943 ? C125 C126 . . 1.49(2) ? C125 H125a . . .971 ? C125 H125b . . .950 ? C126 H126a . . .92 ? C126 H126b . . .971 ? C13 H13 . . .962 ? C13 C13 . '4 656' 1.27(2) ? C21 N22 . . 1.344(12) ? C21 N22 . '4 656' 1.344(12) ? N22 C221 . . 1.460(15) ? N22 C23 . . 1.382(15) ? C221 C222 . . 1.52(2) ? C221 C226 . . 1.49(2) ? C221 H221 . . .938 ? C222 C223 . . 1.48(2) ? C222 H222a . . .984 ? C222 H222b . . .976 ? C223 C224 . . 1.57(3) ? C223 H223a . . .961 ? C223 H223b . . .962 ? C224 C225 . . 1.57(4) ? C224 H224a . . .946 ? C224 H224b . . .95 ? C225 C226 . . 1.51(2) ? C225 H225a . . .954 ? C225 H225b . . .915 ? C226 H226a . . .98 ? C226 H226b . . .966 ? C23 H23 . . .962 ? C23 C23 . '4 656' 1.362(18) ? P F1 . . 1.491(15) ? P F2 . . 1.561(16) ? P F3 . . 1.512(15) ? P F4 . . 1.52(2) ? P F2 . 5 1.560(16) ? P F4 . 5 1.52(2) ? 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 Au C21 . . . 180.0000 ? Au C11 N12 . . . 128.7(5) ? Au C11 N12 . . '4 656' 128.7(5) ? N12 C11 N12 . . '4 656' 102.5(9) ? C11 N12 C121 . . . 122.4(8) ? C11 N12 C13 . . . 110.4(9) ? C121 N12 C13 . . . 127.2(10) ? N12 C121 C122 . . . 111.3(11) ? N12 C121 C126 . . . 112.3(11) ? N12 C121 H121 . . . 106.3 ? C122 C121 C126 . . . 110.1(11) ? C122 C121 H121 . . . 107.8 ? C126 C121 H121 . . . 108.7 ? C121 C122 C123 . . . 108.8(12) ? C121 C122 H122a . . . 110.3 ? C121 C122 H122b . . . 110.0 ? C123 C122 H122a . . . 108.9 ? C123 C122 H122b . . . 109.7 ? H122a C122 H122b . . . 109.1 ? C122 C123 C124 . . . 112.1(15) ? C122 C123 H123a . . . 110.1 ? C122 C123 H123b . . . 110.3 ? C124 C123 H123a . . . 107.6 ? C124 C123 H123b . . . 107.5 ? H123a C123 H123b . . . 109 ? C123 C124 C125 . . . 108.6(14) ? C123 C124 H124a . . . 109.3 ? C123 C124 H124b . . . 109.9 ? C125 C124 H124a . . . 110.3 ? C125 C124 H124b . . . 109.9 ? H124a C124 H124b . . . 108.8 ? C124 C125 C126 . . . 111.2(14) ? C124 C125 H125a . . . 108.1 ? C124 C125 H125b . . . 109.1 ? C126 C125 H125a . . . 110.4 ? C126 C125 H125b . . . 110.3 ? H125a C125 H125b . . . 107.6 ? C121 C126 C125 . . . 108.0(14) ? C121 C126 H126a . . . 111.8 ? C121 C126 H126b . . . 108.4 ? C125 C126 H126a . . . 110.2 ? C125 C126 H126b . . . 107.7 ? H126a C126 H126b . . . 110.7 ? N12 C13 H13 . . . 123.1 ? N12 C13 C13 . . '4 656' 108.3(11) ? H13 C13 C13 . . '4 656' 128.6 ? Au C21 N22 . . . 126.9(6) ? Au C21 N22 . . '4 656' 126.9(6) ? N22 C21 N22 . . '4 656' 106.3(10) ? C21 N22 C221 . . . 123.9(9) ? C21 N22 C23 . . . 110.3(9) ? C221 N22 C23 . . . 125.8(10) ? N22 C221 C222 . . . 112.1(10) ? N22 C221 C226 . . . 111.2(11) ? N22 C221 H221 . . . 109.1 ? C222 C221 C226 . . . 109.5(13) ? C222 C221 H221 . . . 109.0 ? C226 C221 H221 . . . 105.7 ? C221 C222 C223 . . . 113.3(12) ? C221 C222 H222a . . . 110.5 ? C221 C222 H222b . . . 109.8 ? C223 C222 H222a . . . 108.5 ? C223 C222 H222b . . . 109.8 ? H222a C222 H222b . . . 104.6 ? C222 C223 C224 . . . 109.5(14) ? C222 C223 H223a . . . 111.6 ? C222 C223 H223b . . . 108.8 ? C224 C223 H223a . . . 109.9 ? C224 C223 H223b . . . 109.5 ? H223a C223 H223b . . . 107.5 ? C223 C224 C225 . . . 109.5(16) ? C223 C224 H224a . . . 108 ? C223 C224 H224b . . . 108 ? C225 C224 H224a . . . 111 ? C225 C224 H224b . . . 110 ? H224a C224 H224b . . . 110 ? C224 C225 C226 . . . 109.5(18) ? C224 C225 H225a . . . 104.1 ? C224 C225 H225b . . . 107 ? C226 C225 H225a . . . 111.4 ? C226 C225 H225b . . . 112.2 ? H225a C225 H225b . . . 112 ? C221 C226 C225 . . . 111.0(17) ? C221 C226 H226a . . . 110.1 ? C221 C226 H226b . . . 111.4 ? C225 C226 H226a . . . 107.1 ? C225 C226 H226b . . . 111.5 ? H226a C226 H226b . . . 106 ? N22 C23 H23 . . . 127.8(12) ? N22 C23 C23 . . '4 656' 106.6(10) ? H23 C23 C23 . . '4 656' 125.6 ? F1 P F2 . . . 87.9(8) ? F1 P F3 . . . 180.00(9) ? F1 P F4 . . . 86.8(9) ? F1 P F2 . . 5 87.9(8) ? F1 P F4 . . 5 86.8(9) ? F2 P F3 . . . 92.1(8) ? F2 P F4 . . . 86.6(10) ? F2 P F2 . . 5 175.7(9) ? F2 P F4 . . 5 93.2(10) ? F3 P F4 . . . 93.2(9) ? F3 P F2 . . 5 92.1(8) ? F3 P F4 . . 5 93.2(9) ? F4 P F2 . . 5 93.2(10) ? F4 P F4 . . 5 173.7(12) ? F2 P F4 5 . 5 86.6(10) ? 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 1616 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 15 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _reflns_number_observed ? _reflns_d_resolution_high .66 _reflns_d_resolution_low 14.162 _diffrn_reflns_av_sigmaI/netI .048 _diffrn_reflns_theta_min 1.43 _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 .063 _refine_ls_wR_factor_all .09 _refine_ls_goodness_of_fit_all 1.176 _refine_ls_shift/su_mean .0003 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end