#------------------------------------------------------------------------------ #$Date: 2017-01-09 12:55:22 +0200 (Mon, 09 Jan 2017) $ #$Revision: 190295 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/48/4304874.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_4304874 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, (As F6), 0.5(C3 H6 O)' _chemical_formula_sum 'C7.5 H19 As Au F6 N4 O0.5' _chemical_formula_weight 559.16 _chemical_name_common '[Au(C(NHCH3)2)2](AsF6).0.5CO(CH3)2' _chemical_name_systematic ? _space_group_IT_number 136 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4n 2n' _symmetry_space_group_name_H-M 'P 42/m n m' _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 4 _cell_length_a 15.6093(8) _cell_length_b 15.6093(8) _cell_length_c 6.4275(5) _cell_measurement_reflns_used 981 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 28.3 _cell_measurement_theta_min 2.61 _cell_volume 1566.06(17) _computing_cell_refinement SMART _computing_data_collection 'SMART 5.054 (Bruker, 2002)' _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _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 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0140 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 18143 _diffrn_reflns_theta_full 28.29 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_min 1.85 _exptl_absorpt_coefficient_mu 11.550 _exptl_absorpt_correction_T_max 0.360 _exptl_absorpt_correction_T_min 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1048 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.459 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.215 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.313 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 1113 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.313 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0168 _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^)+(0.0198P)^2^+1.3644P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.0483 _reflns_number_gt 981 _reflns_number_total 1113 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ic702481v-file003.cif _cod_data_source_block dp74 _cod_depositor_comments ; Changing the _chemical_formula_sum data item value from 'C7.5 H19 A2 As F6 N4 O0.5' to 'C7.5 H19 As Au F6 N4 O0.5'. Antanas Vaitkus, 2017-01-09 ; _cod_original_formula_sum 'C7.5 H19 As A2 F6 N4 O0.5' _cod_database_code 4304874 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' '-x, -y, -z' 'x, y, -z' 'y-1/2, -x-1/2, -z-1/2' '-y-1/2, x-1/2, -z-1/2' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y, -x, z' 'y, x, z' 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 Au1 Au 0.5000 0.0000 0.5000 0.01298(8) Uani 1 4 d S . . N1 N 0.51260(19) 0.1875(2) 0.5000 0.0190(6) Uani 1 2 d S . . H1 H 0.5673 0.1739 0.5000 0.023 Uiso 1 2 calc SR . . N2 N 0.37451(19) 0.14474(19) 0.5000 0.0167(6) Uani 1 2 d S . . H2 H 0.3622 0.1998 0.5000 0.020 Uiso 1 2 calc SR . . C1 C 0.4909(2) 0.2788(3) 0.5000 0.0239(8) Uani 1 2 d S . . H1A H 0.5421 0.3128 0.5000 0.029 Uiso 1 2 d SR . . H1B H 0.4573 0.2921 0.6209 0.029 Uiso 1 1 d R . . C2 C 0.3028(2) 0.0848(2) 0.5000 0.0211(7) Uani 1 2 d S . . H2A H 0.3200 0.0257 0.5000 0.025 Uiso 1 2 d SR . . H2B H 0.2682 0.0954 0.3794 0.025 Uiso 1 1 d R . . C3 C 0.4561(2) 0.1232(2) 0.5000 0.0158(6) Uani 1 2 d S . . As1 As 0.28302(2) 0.28302(2) 0.0000 0.01278(11) Uani 1 4 d S . . F1 F 0.28317(15) 0.28317(15) 0.2672(3) 0.0358(6) Uani 1 2 d S . . F2 F 0.20421(13) 0.36064(13) 0.0000 0.0226(5) Uani 1 2 d S . . F3 F 0.36030(14) 0.36030(14) 0.0000 0.0406(10) Uani 1 4 d S . . F4 F 0.20549(15) 0.20549(15) 0.0000 0.0425(10) Uani 1 4 d S . . O1 O 0.0000 0.0000 0.144(3) 0.067(4) Uani 0.50 4 d SP . . C7 C 0.0000 0.0000 0.330(3) 0.039(4) Uani 0.50 4 d SP . . C8 C 0.0573(4) 0.0573(4) 0.447(2) 0.045(4) Uani 0.50 2 d SP . . H8A H 0.1034 0.0351 0.5001 0.054 Uiso 0.50 2 d SPR . . H8B H 0.0256 0.0833 0.5597 0.054 Uiso 0.25 1 d PR . . H8C H 0.0739 0.1037 0.3556 0.054 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01379(11) 0.01274(11) 0.01239(12) 0.000 0.000 0.00407(6) N1 0.0161(14) 0.0159(15) 0.0249(17) 0.000 0.000 0.0021(11) N2 0.0154(14) 0.0131(14) 0.0214(16) 0.000 0.000 0.0031(10) C1 0.0186(17) 0.0167(18) 0.036(2) 0.000 0.000 0.0008(14) C2 0.0183(18) 0.0211(18) 0.0241(18) 0.000 0.000 0.0000(13) C3 0.0187(17) 0.0170(16) 0.0116(15) 0.000 0.000 0.0033(12) As1 0.01134(14) 0.01134(14) 0.0157(2) 0.000 0.000 0.00321(19) F1 0.0451(10) 0.0451(10) 0.0171(11) 0.0001(8) 0.0001(8) 0.0295(15) F2 0.0214(11) 0.0222(11) 0.0243(11) 0.000 0.000 0.0125(8) F3 0.0217(11) 0.0217(11) 0.078(3) 0.000 0.000 -0.0084(13) F4 0.0224(11) 0.0224(11) 0.083(3) 0.000 0.000 -0.0077(13) O1 0.056(5) 0.056(5) 0.089(11) 0.000 0.000 0.004(5) C7 0.024(4) 0.024(4) 0.069(12) 0.000 0.000 0.007(4) C8 0.028(2) 0.028(2) 0.079(14) 0.001(3) 0.001(3) 0.002(3) 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' O O 0.0106 0.0060 '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' 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 C3 Au1 C3 180.0 . 9_656 ? C3 Au1 Au1 90.0 . 3_544 ? Au1 Au1 Au1 180.0 3_544 3_545 ? C3 N1 C1 125.3(3) . . ? C3 N1 H1 117.3 . . ? C1 N1 H1 117.3 . . ? C3 N2 C2 125.3(3) . . ? C3 N2 H2 117.3 . . ? C2 N2 H2 117.3 . . ? N1 C1 H1A 110.1 . . ? N1 C1 H1B 109.6 . . ? H1A C1 H1B 109.6 . . ? N2 C2 H2A 113.7 . . ? N2 C2 H2B 108.8 . . ? H2A C2 H2B 108.9 . . ? N2 C3 N1 116.6(3) . . ? N2 C3 Au1 124.3(3) . . ? N1 C3 Au1 119.1(3) . . ? F3 As1 F4 180.00(10) . . ? F3 As1 F1 89.89(12) . . ? F4 As1 F1 90.11(12) . . ? F1 As1 F1 179.8(3) 10 . ? F3 As1 F2 90.44(7) . . ? F4 As1 F2 89.56(7) . . ? F1 As1 F2 90.00(8) . . ? F2 As1 F2 179.12(15) 7 . ? O1 C7 C8 120.7(9) . . ? O1 C7 C8 120.7(9) . 2 ? C8 C7 C8 118.6(17) . 2 ? C7 C8 H8A 117.5 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.4 . . ? C7 C8 H8C 107.9 . . ? H8A C8 H8C 108.2 . . ? H8B C8 H8C 106.1 . . ? 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 Au1 C3 2.042(3) . ? Au1 Au1 3.2138(3) 3_544 ? N1 C3 1.335(5) . ? N1 C1 1.466(5) . ? N1 H1 0.8800 . ? N2 C3 1.318(4) . ? N2 C2 1.459(4) . ? N2 H2 0.8800 . ? C1 H1A 0.9599 . ? C1 H1B 0.9600 . ? C2 H2A 0.9599 . ? C2 H2B 0.9601 . ? As1 F3 1.706(3) . ? As1 F4 1.711(3) . ? As1 F1 1.717(2) . ? As1 F2 1.7266(19) . ? O1 C7 1.20(3) . ? C7 C8 1.470(14) . ? C8 H8A 0.8677 . ? C8 H8B 0.9654 . ? C8 H8C 0.9696 . ? 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 H1 F2 0.88 2.20 3.084(4) 180 13_666 N2 H2 F1 0.88 2.34 2.990(3) 131 .