#------------------------------------------------------------------------------ #$Date: 2016-03-22 23:57:47 +0200 (Tue, 22 Mar 2016) $ #$Revision: 179086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/48/4304875.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4304875 loop_ _publ_author_name 'Daniel Rios' 'David M. Pham' 'James C. Fettinger' 'Marilyn M. Olmstead' 'Alan L. Balch' _publ_section_title ; Blue or Green Glowing Crystals of the Cation [Au{C(NHMe)2}2]+. Structural Effects of Anions, Hydrogen Bonding, and Solvate Molecules on the Luminescence of a Two-Coordinate Gold(I) Carbene Complex ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3442 _journal_page_last 3451 _journal_paper_doi 10.1021/ic702481v _journal_volume 47 _journal_year 2008 _chemical_formula_moiety 'C6 H16 Au N4, o.5(C6 H5 Cl), As F6' _chemical_formula_sum 'C9 H18.5 As Au Cl F6 N4' _chemical_formula_weight 585.88 _chemical_name_common '[AuL2]AsF6-0.5PhCl' _chemical_name_systematic ; ? ; _space_group_IT_number 131 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4c 2' _symmetry_space_group_name_H-M 'P 42/m m c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 11.1918(3) _cell_length_b 11.1918(3) _cell_length_c 6.4062(4) _cell_measurement_reflns_used 7489 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 28.30 _cell_measurement_theta_min 2.57 _cell_volume 802.42(6) _computing_cell_refinement SAINT _computing_data_collection 'Apex II 2.0 Rev.2 (Bruker, 2005)' _computing_data_reduction 'SAINT 7.12A (Bruker, 2004)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.085 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 7707 _diffrn_reflns_theta_full 28.30 _diffrn_reflns_theta_max 28.30 _diffrn_reflns_theta_min 1.82 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 549 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.786 _refine_diff_density_min -4.269 _refine_diff_density_rms 0.191 _refine_ls_extinction_coef 0.0021(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 50 _refine_ls_number_reflns 601 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.835 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0257 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+4.9709P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.0819 _reflns_number_gt 598 _reflns_number_total 601 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ic702481v-file004.cif _cod_data_source_block dp93 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 4304875 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x, y, -z' 'x, -y, -z' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' 'x, -y, z' '-x, y, z' '-y, -x, z-1/2' 'y, x, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.0000 0.5000 0.0000 0.0221(3) Uani 1 8 d S . . F1 F 0.0000 0.3471(4) 0.0000 0.0410(15) Uani 1 4 d S . . F2 F 0.0000 0.5000 -0.2667(8) 0.043(2) Uani 1 4 d S . . F3 F 0.1527(7) 0.5000 0.0000 0.064(2) Uani 1 4 d S . . Au1 Au 0.0000 0.0000 0.0000 0.0182(2) Uani 1 8 d S . . N1 N 0.1933(11) 0.1755(11) 0.0000 0.024(2) Uani 0.50 2 d SP A 1 H1A H 0.1305 0.2228 0.0000 0.029 Uiso 0.50 2 calc SPR A 1 C1 C 0.3112(12) 0.2321(12) 0.0000 0.035(3) Uani 0.50 2 d SP A 1 H1B H 0.3079 0.3178 0.0000 0.052 Uiso 0.50 2 d SPR A 1 H1C H 0.3527 0.2050 0.1224 0.052 Uiso 0.50 1 d PR A 1 N2 N 0.2664(6) 0.0000 0.0000 0.0246(14) Uani 1 4 d S . 2 H2A H 0.3450 0.0000 0.0000 0.029 Uiso 1 4 calc SR . 2 C2 C 0.2630(12) -0.1415(11) 0.0000 0.025(2) Uani 0.50 2 d SP . 2 H2B H 0.3447 -0.1677 0.0000 0.037 Uiso 0.50 2 d SPR . 2 H2C H 0.2234 -0.1713 0.1224 0.037 Uiso 0.50 1 d PR . 2 C3 C 0.1733(9) 0.0578(10) 0.0000 0.020(2) Uani 0.50 2 d SP . . Cl1 Cl 0.5000 0.5000 0.0000 0.100 Uiso 0.50 8 d SP . 1 C4 C 0.5000 0.5000 0.2500 0.100 Uiso 1 8 d S . . H4A H 0.5000 0.5000 0.3998 0.120 Uiso 0.25 2 calc SPR . 2 C5 C 0.5000 0.391(3) 0.116(5) 0.100 Uiso 0.50 2 d SP . 2 H5A H 0.5000 0.3158 0.1844 0.120 Uiso 0.50 2 calc SPR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0407(7) 0.0102(5) 0.0154(5) 0.000 0.000 0.000 F1 0.089(5) 0.012(2) 0.022(2) 0.000 0.000 0.000 F2 0.094(6) 0.021(3) 0.015(3) 0.000 0.000 0.000 F3 0.041(4) 0.058(4) 0.093(6) 0.000 0.000 0.000 Au1 0.0122(2) 0.0302(3) 0.0123(3) 0.000 0.000 0.000 N1 0.018(5) 0.030(5) 0.023(6) 0.000 0.000 0.003(5) C1 0.018(5) 0.029(6) 0.056(9) 0.000 0.000 -0.006(5) N2 0.016(3) 0.042(4) 0.016(3) 0.000 0.000 0.000 C2 0.026(6) 0.026(6) 0.022(5) 0.000 0.000 -0.003(5) C3 0.021(5) 0.027(5) 0.011(4) 0.000 0.000 0.001(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 As1 F2 180.0 9_565 . ? F2 As1 F3 90.000(1) 9_565 9_565 ? F2 As1 F3 90.000(1) . 9_565 ? F2 As1 F3 90.000(1) 9_565 . ? F2 As1 F3 90.000(1) . . ? F3 As1 F3 180.0 9_565 . ? F2 As1 F1 90.0 9_565 9_565 ? F2 As1 F1 90.0 . 9_565 ? F3 As1 F1 90.0 9_565 9_565 ? F3 As1 F1 90.0 . 9_565 ? F2 As1 F1 90.0 9_565 . ? F2 As1 F1 90.0 . . ? F3 As1 F1 90.0 9_565 . ? F3 As1 F1 90.0 . . ? F1 As1 F1 180.0 9_565 . ? C3 Au1 C3 180.0 . 9 ? C3 Au1 C3 36.9(6) . 13 ? C3 Au1 C3 143.1(6) 9 13 ? C3 Au1 C3 143.1(6) . 5 ? C3 Au1 C3 36.9(6) 9 5 ? C3 Au1 C3 180.0 13 5 ? C3 Au1 Au1 90.0 . 3 ? C3 Au1 Au1 90.0 9 3 ? C3 Au1 Au1 90.0 13 3 ? C3 Au1 Au1 90.0 5 3 ? C3 Au1 Au1 90.0 . 3_554 ? C3 Au1 Au1 90.0 9 3_554 ? C3 Au1 Au1 90.0 13 3_554 ? C3 Au1 Au1 90.0 5 3_554 ? Au1 Au1 Au1 180.0 3 3_554 ? C3 N1 C1 125.3(11) . . ? C3 N1 H1A 117.4 . . ? C1 N1 H1A 117.4 . . ? N1 C1 H1B 113.5 . . ? N1 C1 H1C 107.4 . . ? H1B C1 H1C 109.5 . . ? C3 N2 C2 120.4(9) . . ? C3 N2 C2 120.4(9) 13 13 ? C2 N2 C2 177.3(11) . 13 ? C3 N2 H2A 148.2 13 . ? C3 N2 H2A 148.2 . . ? C2 N2 H2A 91.4 . . ? C2 N2 H2A 91.4 13 . ? C3 C2 H2B 154.8 13 . ? N2 C2 H2B 106.4 . . ? C3 C2 H2C 84.2 13 . ? N2 C2 H2C 111.0 . . ? H2B C2 H2C 109.5 . . ? N2 C3 N1 112.2(10) . . ? C3 C3 N1 170.4(7) 13 . ? N2 C3 C2 74.8(8) . 13 ? N2 C3 Au1 129.8(8) . . ? N1 C3 Au1 118.1(8) . . ? C2 C3 Au1 155.4(9) 13 . ? C4 Cl1 C4 180.0 . 9_665 ? C5 C4 C5 110(3) 12_656 11_566 ? C5 C4 C5 109.3(13) 12_656 . ? C5 C4 C5 109.3(13) 11_566 . ? C5 C4 C5 109.4(13) 12_656 2_665 ? C5 C4 C5 109.4(13) 11_566 2_665 ? C5 C4 C5 110(3) . 2_665 ? C5 C4 Cl1 54.9(13) 12_656 3_655 ? C5 C4 Cl1 54.9(13) 11_566 3_655 ? C5 C4 Cl1 125.1(13) . 3_655 ? C5 C4 Cl1 125.1(13) 2_665 3_655 ? C5 C4 Cl1 125.1(13) 12_656 . ? C5 C4 Cl1 125.1(13) 11_566 . ? C5 C4 Cl1 54.9(13) . . ? C5 C4 Cl1 54.9(13) 2_665 . ? Cl1 C4 Cl1 180.0 3_655 . ? C5 C5 C4 125.1(13) 10 . ? C5 C5 H5A 117.4 10 . ? C4 C5 H5A 117.4 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 F2 1.708(5) 9_565 ? As1 F2 1.708(5) . ? As1 F3 1.709(7) 9_565 ? As1 F3 1.709(7) . ? As1 F1 1.711(5) 9_565 ? As1 F1 1.711(5) . ? Au1 C3 2.044(11) . ? Au1 C3 2.044(11) 9 ? Au1 C3 2.044(11) 13 ? Au1 C3 2.044(11) 5 ? Au1 Au1 3.2031(2) 3 ? Au1 Au1 3.2031(2) 3_554 ? N1 C3 1.337(16) . ? N1 C1 1.464(17) . ? N1 H1A 0.8800 . ? C1 H1B 0.9599 . ? C1 H1C 0.9601 . ? N2 C3 1.226(12) 13 ? N2 C3 1.226(12) . ? N2 C2 1.584(12) . ? N2 C2 1.584(12) 13 ? N2 H2A 0.8800 . ? C2 C3 1.374(17) 13 ? C2 H2B 0.9601 . ? C2 H2C 0.9601 . ? C3 C3 1.29(2) 13 ? C3 C2 1.374(17) 13 ? Cl1 C4 1.6015 . ? Cl1 C4 1.6016 9_665 ? C4 C5 1.49(3) 12_656 ? C4 C5 1.49(3) 11_566 ? C4 C5 1.49(3) . ? C4 C5 1.49(3) 2_665 ? C4 Cl1 1.6015 3_655 ? C4 H4A 0.95 . ? C5 C5 1.49(6) 10 ? C5 H5A 0.9500 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A F1 0.88 2.02 2.893(12) 173.4 . N2 H2A F2 0.88 2.29 3.012(7) 139.2 3_655 N2 H2A F2 0.88 2.29 3.012(7) 139.2 11 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N2 C2 C3 0.0 . . . 13 ? C2 N2 C2 C3 -0.009(4) 13 . . 13 ? C2 N2 C3 C3 0.0 . . . 13 ? C2 N2 C3 C3 180.0 13 . . 13 ? C3 N2 C3 N1 180.0 13 . . . ? C2 N2 C3 N1 180.0 . . . . ? C2 N2 C3 N1 0.0 13 . . . ? C3 N2 C3 C2 180.0 13 . . 13 ? C2 N2 C3 C2 180.0 . . . 13 ? C3 N2 C3 Au1 0.0 13 . . . ? C2 N2 C3 Au1 0.0 . . . . ? C2 N2 C3 Au1 180.0 13 . . . ? C1 N1 C3 N2 0.0 . . . . ? C1 N1 C3 C3 0.0 . . . 13 ? C1 N1 C3 C2 0.0 . . . 13 ? C1 N1 C3 Au1 180.0 . . . . ? C3 Au1 C3 N2 -125(4) 9 . . . ? C3 Au1 C3 N2 0.0 13 . . . ? C3 Au1 C3 N2 180.0 5 . . . ? Au1 Au1 C3 N2 90.0 3 . . . ? Au1 Au1 C3 N2 -90.0 3_554 . . . ? C3 Au1 C3 C3 -125(4) 9 . . 13 ? C3 Au1 C3 C3 180.0 5 . . 13 ? Au1 Au1 C3 C3 90.0 3 . . 13 ? Au1 Au1 C3 C3 -90.0 3_554 . . 13 ? C3 Au1 C3 N1 55(4) 9 . . . ? C3 Au1 C3 N1 180.0 13 . . . ? C3 Au1 C3 N1 0.0 5 . . . ? Au1 Au1 C3 N1 -90.0 3 . . . ? Au1 Au1 C3 N1 90.0 3_554 . . . ? C3 Au1 C3 C2 55(4) 9 . . 13 ? C3 Au1 C3 C2 180.0 13 . . 13 ? C3 Au1 C3 C2 0.0 5 . . 13 ? Au1 Au1 C3 C2 -90.0 3 . . 13 ? Au1 Au1 C3 C2 90.0 3_554 . . 13 ? C4 Cl1 C4 C5 89(19) 9_665 . . 12_656 ? C4 Cl1 C4 C5 -91(21) 9_665 . . 11_566 ? C4 Cl1 C4 C5 -1(19) 9_665 . . . ? C4 Cl1 C4 C5 179(21) 9_665 . . 2_665 ? C4 Cl1 C4 Cl1 -1.7 9_665 . . 3_655 ? C5 C4 C5 C5 -119.9(8) 12_656 . . 10 ? C5 C4 C5 C5 119.9(8) 11_566 . . 10 ? C5 C4 C5 C5 0.000(7) 2_665 . . 10 ? Cl1 C4 C5 C5 180.000(4) 3_655 . . 10 ? Cl1 C4 C5 C5 0.000(4) . . . 10 ?