#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/50/79/1507937.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_1507937 loop_ _publ_author_name 'Serpell, Christopher J.' 'Cookson, James' 'Ozkaya, Dogan' 'Beer, Paul D.' _publ_section_title ; Core@shell bimetallic nanoparticle synthesis via anion coordination. ; _journal_issue 6 _journal_name_full 'Nature chemistry' _journal_page_first 478 _journal_page_last 483 _journal_paper_doi 10.1038/nchem.1030 _journal_volume 3 _journal_year 2011 _chemical_formula_moiety 'C16 H36 N, Au Cl4' _chemical_formula_sum 'C16 H36 Au Cl4 N' _chemical_formula_weight 581.25 _chemical_melting_point 421 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 10-07-01 _audit_creation_method CRYSTALS_ver_14.07 _cell_angle_alpha 90 _cell_angle_beta 107.0733(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.7634(3) _cell_length_b 8.8165(2) _cell_length_c 18.1140(4) _cell_measurement_reflns_used 5329 _cell_measurement_temperature 150 _cell_measurement_theta_max 27 _cell_measurement_theta_min 5 _cell_volume 2253.84(9) _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device Area _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 24962 _diffrn_reflns_theta_full 26.936 _diffrn_reflns_theta_max 27.486 _diffrn_reflns_theta_min 5.190 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.999 _exptl_absorpt_correction_T_max 0.28 _exptl_absorpt_correction_T_min 0.23 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1144 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.180 _refine_diff_density_max 1.42 _refine_diff_density_min -1.81 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.9366 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 5138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0292 _refine_ls_shift/su_max 0.0008115 _refine_ls_shift/su_mean 0.0000173 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 8.66 12.1 6.25 1.81 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0880 _refine_ls_wR_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.0880 _reflns_limit_h_max 18 _reflns_limit_h_min -19 _reflns_limit_k_max 11 _reflns_limit_k_min 0 _reflns_limit_l_max 23 _reflns_limit_l_min 0 _reflns_number_gt 3829 _reflns_number_total 5138 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 2.24 _oxford_diffrn_Wilson_scale 82.26 _oxford_refine_ls_r_factor_ref 0.0515 _oxford_refine_ls_scale 0.11230(3) _oxford_reflns_number_all 5138 _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _oxford_structure_analysis_title 031CJS10 _cod_data_source_file nchem.1030-s2.cif _cod_data_source_block TBAAuCl4 _cod_original_sg_symbol_H-M 'P 21/n ' _cod_original_formula_sum 'C16 H36 Au1 Cl4 N1' _cod_database_code 1507937 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn Au1 Au 0.002532(15) 0.62618(3) 0.225019(12) 0.0273 1.0000 Uani . Cl2 Cl 0.05017(11) 0.79125(19) 0.14747(9) 0.0381 1.0000 Uani . Cl3 Cl -0.14155(11) 0.60538(19) 0.13459(10) 0.0402 1.0000 Uani . Cl4 Cl -0.04498(16) 0.4640(2) 0.30392(13) 0.0597 1.0000 Uani . Cl5 Cl 0.14729(13) 0.6470(3) 0.31356(10) 0.0548 1.0000 Uani . N6 N 0.3009(3) 0.3768(5) 0.5535(2) 0.0213 1.0000 Uani . C7 C 0.4021(3) 0.3771(7) 0.5481(3) 0.0223 1.0000 Uani . C8 C 0.4617(4) 0.2389(6) 0.5783(3) 0.0265 1.0000 Uani . C9 C 0.5619(4) 0.2628(7) 0.5723(3) 0.0291 1.0000 Uani . C10 C 0.6248(4) 0.1249(9) 0.5983(4) 0.0436 1.0000 Uani . C11 C 0.2425(4) 0.2516(6) 0.5058(3) 0.0244 1.0000 Uani . C12 C 0.2293(4) 0.2539(7) 0.4192(3) 0.0307 1.0000 Uani . C13 C 0.1606(4) 0.1306(8) 0.3794(3) 0.0335 1.0000 Uani . C14 C 0.1464(6) 0.1275(11) 0.2928(4) 0.0515 1.0000 Uani . C15 C 0.2605(4) 0.5341(6) 0.5248(3) 0.0215 1.0000 Uani . C16 C 0.1588(4) 0.5585(7) 0.5223(4) 0.0281 1.0000 Uani . C17 C 0.1343(4) 0.7260(7) 0.5107(4) 0.0333 1.0000 Uani . C18 C 0.0300(5) 0.7558(8) 0.5031(4) 0.0382 1.0000 Uani . C19 C 0.3005(4) 0.3510(6) 0.6358(3) 0.0231 1.0000 Uani . C20 C 0.3538(4) 0.4671(7) 0.6946(3) 0.0313 1.0000 Uani . C21 C 0.3389(5) 0.4370(8) 0.7728(3) 0.0382 1.0000 Uani . C22 C 0.3870(5) 0.5529(9) 0.8325(4) 0.0414 1.0000 Uani . H71 H 0.4354 0.4648 0.5779 0.0294 1.0000 Uiso R H72 H 0.3985 0.3897 0.4940 0.0293 1.0000 Uiso R H81 H 0.4649 0.2237 0.6317 0.0359 1.0000 Uiso R H82 H 0.4332 0.1507 0.5479 0.0361 1.0000 Uiso R H91 H 0.5900 0.3532 0.6040 0.0370 1.0000 Uiso R H92 H 0.5593 0.2838 0.5196 0.0376 1.0000 Uiso R H101 H 0.6901 0.1453 0.5985 0.0711 1.0000 Uiso R H102 H 0.6240 0.0965 0.6498 0.0709 1.0000 Uiso R H103 H 0.5977 0.0431 0.5638 0.0714 1.0000 Uiso R H111 H 0.2749 0.1565 0.5266 0.0336 1.0000 Uiso R H112 H 0.1805 0.2564 0.5150 0.0336 1.0000 Uiso R H121 H 0.2887 0.2380 0.4093 0.0392 1.0000 Uiso R H122 H 0.2054 0.3532 0.3980 0.0392 1.0000 Uiso R H131 H 0.1838 0.0309 0.4012 0.0445 1.0000 Uiso R H132 H 0.1001 0.1476 0.3884 0.0440 1.0000 Uiso R H141 H 0.1041 0.0464 0.2694 0.0768 1.0000 Uiso R H142 H 0.2079 0.1128 0.2857 0.0773 1.0000 Uiso R H143 H 0.1196 0.2231 0.2710 0.0770 1.0000 Uiso R H151 H 0.2993 0.6074 0.5596 0.0300 1.0000 Uiso R H152 H 0.2686 0.5447 0.4736 0.0302 1.0000 Uiso R H161 H 0.1486 0.5239 0.5701 0.0370 1.0000 Uiso R H162 H 0.1184 0.5038 0.4794 0.0371 1.0000 Uiso R H171 H 0.1734 0.7820 0.5554 0.0405 1.0000 Uiso R H172 H 0.1476 0.7649 0.4653 0.0406 1.0000 Uiso R H181 H 0.0191 0.8642 0.5035 0.0620 1.0000 Uiso R H182 H 0.0150 0.7098 0.5467 0.0617 1.0000 Uiso R H183 H -0.0084 0.7140 0.4555 0.0621 1.0000 Uiso R H191 H 0.3262 0.2490 0.6500 0.0334 1.0000 Uiso R H192 H 0.2338 0.3522 0.6338 0.0328 1.0000 Uiso R H201 H 0.4229 0.4565 0.7016 0.0415 1.0000 Uiso R H202 H 0.3313 0.5683 0.6768 0.0411 1.0000 Uiso R H211 H 0.3644 0.3379 0.7901 0.0511 1.0000 Uiso R H212 H 0.2733 0.4343 0.7684 0.0515 1.0000 Uiso R H221 H 0.3756 0.5356 0.8810 0.0670 1.0000 Uiso R H222 H 0.4529 0.5520 0.8374 0.0675 1.0000 Uiso R H223 H 0.3624 0.6491 0.8120 0.0673 1.0000 Uiso R 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 0.03282(11) 0.02459(11) 0.02584(11) 0.00228(9) 0.01050(7) 0.00350(10) Cl2 0.0402(8) 0.0392(8) 0.0393(8) 0.0131(7) 0.0186(6) 0.0055(6) Cl3 0.0312(7) 0.0348(8) 0.0497(9) -0.0027(7) 0.0041(6) 0.0035(6) Cl4 0.0693(12) 0.0552(12) 0.0613(12) 0.0283(10) 0.0295(10) -0.0022(10) Cl5 0.0455(9) 0.0685(14) 0.0390(8) 0.0117(9) -0.0052(7) -0.0057(9) N6 0.0192(18) 0.022(2) 0.023(2) -0.0004(19) 0.0079(15) -0.0027(19) C7 0.020(2) 0.025(2) 0.022(2) 0.001(2) 0.0051(17) -0.002(2) C8 0.023(3) 0.021(3) 0.038(3) 0.003(2) 0.012(2) 0.000(2) C9 0.026(3) 0.031(3) 0.033(3) 0.006(2) 0.012(2) -0.002(2) C10 0.027(3) 0.042(4) 0.062(4) 0.010(4) 0.014(3) 0.008(3) C11 0.020(2) 0.021(3) 0.031(3) -0.002(2) 0.006(2) -0.001(2) C12 0.031(3) 0.033(3) 0.028(3) -0.003(2) 0.009(2) -0.006(2) C13 0.029(3) 0.035(3) 0.037(3) -0.014(3) 0.011(2) -0.005(3) C14 0.052(4) 0.060(5) 0.037(3) -0.020(4) 0.004(3) -0.008(4) C15 0.028(3) 0.018(2) 0.020(2) -0.0025(18) 0.009(2) 0.000(2) C16 0.025(3) 0.025(3) 0.036(3) 0.004(2) 0.011(2) 0.005(2) C17 0.029(3) 0.024(3) 0.045(3) -0.003(3) 0.008(3) 0.003(2) C18 0.032(3) 0.035(3) 0.044(4) 0.010(3) 0.006(3) 0.012(3) C19 0.024(2) 0.026(3) 0.020(2) 0.003(2) 0.0075(19) 0.001(2) C20 0.035(3) 0.035(3) 0.025(3) 0.000(2) 0.010(2) -0.007(3) C21 0.050(4) 0.044(4) 0.023(3) -0.001(3) 0.015(3) -0.006(3) C22 0.052(4) 0.046(4) 0.026(3) -0.007(3) 0.011(3) 0.006(3) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956 12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl2 Au1 Cl3 90.01(6) yes Cl2 Au1 Cl4 179.12(8) yes Cl3 Au1 Cl4 90.35(7) yes Cl2 Au1 Cl5 89.25(7) yes Cl3 Au1 Cl5 179.06(7) yes Cl4 Au1 Cl5 90.40(8) yes C7 N6 C11 111.7(4) yes C7 N6 C15 105.4(4) yes C11 N6 C15 111.5(4) yes C7 N6 C19 110.6(4) yes C11 N6 C19 106.8(4) yes C15 N6 C19 110.9(4) yes N6 C7 C8 116.9(4) yes N6 C7 H71 107.8 no C8 C7 H71 106.9 no N6 C7 H72 107.5 no C8 C7 H72 108.2 no H71 C7 H72 109.4 no C7 C8 C9 109.6(4) yes C7 C8 H81 109.2 no C9 C8 H81 109.1 no C7 C8 H82 109.3 no C9 C8 H82 109.6 no H81 C8 H82 110.0 no C8 C9 C10 112.6(5) yes C8 C9 H91 108.4 no C10 C9 H91 110.3 no C8 C9 H92 109.8 no C10 C9 H92 107.8 no H91 C9 H92 107.9 no C9 C10 H101 111.5 no C9 C10 H102 109.1 no H101 C10 H102 109.5 no C9 C10 H103 107.4 no H101 C10 H103 111.1 no H102 C10 H103 108.2 no N6 C11 C12 117.4(5) yes N6 C11 H111 105.9 no C12 C11 H111 107.8 no N6 C11 H112 106.1 no C12 C11 H112 109.4 no H111 C11 H112 110.2 no C11 C12 C13 110.3(5) yes C11 C12 H121 110.2 no C13 C12 H121 109.1 no C11 C12 H122 109.8 no C13 C12 H122 109.9 no H121 C12 H122 107.7 no C12 C13 C14 112.0(6) yes C12 C13 H131 110.1 no C14 C13 H131 109.0 no C12 C13 H132 109.3 no C14 C13 H132 108.9 no H131 C13 H132 107.4 no C13 C14 H141 110.1 no C13 C14 H142 106.9 no H141 C14 H142 110.9 no C13 C14 H143 108.8 no H141 C14 H143 109.4 no H142 C14 H143 110.6 no N6 C15 C16 115.0(4) yes N6 C15 H151 106.7 no C16 C15 H151 108.6 no N6 C15 H152 105.4 no C16 C15 H152 111.0 no H151 C15 H152 110.0 no C15 C16 C17 109.7(5) yes C15 C16 H161 110.1 no C17 C16 H161 109.6 no C15 C16 H162 109.3 no C17 C16 H162 108.1 no H161 C16 H162 110.0 no C16 C17 C18 111.8(5) yes C16 C17 H171 108.5 no C18 C17 H171 108.8 no C16 C17 H172 111.4 no C18 C17 H172 108.3 no H171 C17 H172 107.9 no C17 C18 H181 109.5 no C17 C18 H182 108.6 no H181 C18 H182 109.2 no C17 C18 H183 109.3 no H181 C18 H183 109.3 no H182 C18 H183 111.0 no N6 C19 C20 116.1(4) yes N6 C19 H191 106.5 no C20 C19 H191 110.6 no N6 C19 H192 104.9 no C20 C19 H192 109.2 no H191 C19 H192 109.2 no C19 C20 C21 110.5(5) yes C19 C20 H201 109.0 no C21 C20 H201 106.8 no C19 C20 H202 109.2 no C21 C20 H202 109.9 no H201 C20 H202 111.4 no C20 C21 C22 112.6(6) yes C20 C21 H211 108.0 no C22 C21 H211 109.0 no C20 C21 H212 110.4 no C22 C21 H212 109.4 no H211 C21 H212 107.2 no C21 C22 H221 112.3 no C21 C22 H222 108.4 no H221 C22 H222 111.3 no C21 C22 H223 106.2 no H221 C22 H223 110.5 no H222 C22 H223 107.9 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Au1 Cl2 2.2730(15) yes Au1 Cl3 2.2794(15) yes Au1 Cl4 2.2734(17) yes Au1 Cl5 2.2717(17) yes N6 C7 1.527(6) yes N6 C11 1.507(7) yes N6 C15 1.538(7) yes N6 C19 1.509(6) yes C7 C8 1.508(7) yes C7 H71 0.988 no C7 H72 0.972 no C8 C9 1.530(7) yes C8 H81 0.964 no C8 H82 0.974 no C9 C10 1.518(9) yes C9 H91 0.999 no C9 H92 0.962 no C10 H101 0.980 no C10 H102 0.969 no C10 H103 0.962 no C11 C12 1.522(8) yes C11 H111 0.984 no C11 H112 0.979 no C12 C13 1.518(8) yes C12 H121 0.955 no C12 H122 0.979 no C13 C14 1.519(9) yes C13 H131 0.983 no C13 H132 0.966 no C14 H141 0.962 no C14 H142 0.963 no C14 H143 0.966 no C15 C16 1.505(7) yes C15 H151 0.965 no C15 H152 0.975 no C16 C17 1.520(8) yes C16 H161 0.971 no C16 H162 0.959 no C17 C18 1.528(8) yes C17 H171 0.977 no C17 H172 0.963 no C18 H181 0.969 no C18 H182 0.969 no C18 H183 0.956 no C19 C20 1.520(8) yes C19 H191 0.980 no C19 H192 0.976 no C20 C21 1.519(8) yes C20 H201 0.995 no C20 H202 0.974 no C21 C22 1.504(9) yes C21 H211 0.966 no C21 H212 0.948 no C22 H221 0.954 no C22 H222 0.951 no C22 H223 0.953 no