#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200425.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2200425 loop_ _publ_author_name 'Quach, Tan D.' 'Batey, Robert A.' 'Lough, Alan J.' _publ_section_title ; Tetra-n-butylammonium phenyltrifluoroborate ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o688 _journal_page_last o689 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C16 H36 N 1+, C6 H5 B F3 1-' _chemical_formula_moiety 'C16 H36 N 1+, C6 H5 B F3 1-' _chemical_formula_sum 'C22 H41 B F3 N' _chemical_formula_weight 387.37 _chemical_name_systematic ; Tetra-n-butylammonium Phenyltrifluoroborate ; _space_group_IT_number 60 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.5626(6) _cell_length_b 17.1534(7) _cell_length_c 20.3567(7) _cell_measurement_reflns_used 20559 _cell_measurement_temperature 150.0(10) _cell_measurement_theta_max 25.40 _cell_measurement_theta_min 2.55 _cell_volume 4735.9(3) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_data_reduction DENZO-SMN _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick 1999)' _diffrn_ambient_temperature 150.0(10) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full .995 _diffrn_measured_fraction_theta_max .995 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans, and \w scans with \f offsets' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .029 _diffrn_reflns_av_sigmaI/netI .0536 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 20559 _diffrn_reflns_theta_full 25.37 _diffrn_reflns_theta_max 25.37 _diffrn_reflns_theta_min 2.58 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu .078 _exptl_absorpt_correction_T_max .9741 _exptl_absorpt_correction_T_min .9696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(DENZO-SMN; Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1696 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .34 _refine_diff_density_max .190 _refine_diff_density_min -.188 _refine_ls_extinction_coef none _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 248 _refine_ls_number_reflns 4341 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all .0928 _refine_ls_R_factor_gt .0513 _refine_ls_shift/su_max .002 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0564P)^2^+1.1252P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1299 _reflns_number_gt 2858 _reflns_number_total 4341 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cf6090.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200425 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' 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_refinement_flags _atom_site_occupancy _atom_site_type_symbol F1 .59931(8) .57296(6) .92620(5) .0474(3) Uani d . 1 F F2 .75843(9) .59224(6) .95963(5) .0508(3) Uani d . 1 F F3 .65065(8) .69422(6) .95535(5) .0415(3) Uani d . 1 F C1 .71260(14) .64185(10) .84841(9) .0343(5) Uani d . 1 C C2 .64272(17) .64701(12) .79801(10) .0477(6) Uani d . 1 C H2A .5755 .6374 .8083 .057 Uiso calc R 1 H C3 .6668(2) .66524(14) .73437(11) .0594(7) Uani d . 1 C H3A .6169 .6673 .7017 .071 Uiso calc R 1 H C4 .7628(2) .68042(13) .71811(11) .0582(7) Uani d . 1 C H4A .7794 .6948 .6744 .070 Uiso calc R 1 H C5 .83502(18) .67485(13) .76501(12) .0558(6) Uani d . 1 C H5A .9019 .6845 .7538 .067 Uiso calc R 1 H C6 .80956(16) .65481(11) .82970(10) .0445(5) Uani d . 1 C H6A .8603 .6500 .8616 .053 Uiso calc R 1 H B1 .68074(17) .62465(13) .92269(11) .0370(5) Uani d . 1 B N1 .65083(11) .35374(8) .95923(7) .0317(4) Uani d . 1 N C7 .55031(14) .39006(11) .94591(9) .0352(5) Uani d . 1 C H7A .5171 .3986 .9886 .042 Uiso calc R 1 H H7B .5609 .4419 .9257 .042 Uiso calc R 1 H C8 .48082(15) .34400(12) .90189(11) .0488(6) Uani d . 1 C H8A .4598 .2958 .9247 .059 Uiso calc R 1 H H8B .5156 .3288 .8611 .059 Uiso calc R 1 H C9 .39061(15) .39282(14) .88469(11) .0522(6) Uani d . 1 C H9A .3419 .3591 .8623 .063 Uiso calc R 1 H H9B .3601 .4117 .9259 .063 Uiso calc R 1 H C10 .41242(19) .46196(15) .84130(12) .0707(7) Uani d . 1 C H10A .3506 .4881 .8297 .106 Uiso calc R 1 H H10B .4455 .4442 .8012 .106 Uiso calc R 1 H H10C .4553 .4985 .8648 .106 Uiso calc R 1 H C11 .64050(15) .27316(10) .98920(9) .0362(5) Uani d . 1 C H11A .6035 .2400 .9580 .043 Uiso calc R 1 H H11B .7072 .2504 .9938 .043 Uiso calc R 1 H C12 .58977(14) .26878(11) 1.05540(9) .0376(5) Uani d . 1 C H12A .5254 .2959 1.0532 .045 Uiso calc R 1 H H12B .6307 .2952 1.0889 .045 Uiso calc R 1 H C13 .57400(17) .18434(12) 1.07489(11) .0522(6) Uani d . 1 C H13A .5366 .1578 1.0396 .063 Uiso calc R 1 H H13B .6390 .1584 1.0785 .063 Uiso calc R 1 H C14 .51968(19) .17450(13) 1.13854(11) .0595(7) Uani d . 1 C H14A .5085 .1189 1.1468 .089 Uiso calc R 1 H H14B .4562 .2016 1.1360 .089 Uiso calc R 1 H H14C .5589 .1966 1.1744 .089 Uiso calc R 1 H C15 .70366(14) .40930(10) 1.00524(9) .0330(4) Uani d . 1 C H15A .6640 .4143 1.0458 .040 Uiso calc R 1 H H15B .7058 .4613 .9842 .040 Uiso calc R 1 H C16 .80804(14) .38684(12) 1.02447(9) .0387(5) Uani d . 1 C H16A .8502 .3848 .9848 .046 Uiso calc R 1 H H16B .8079 .3345 1.0450 .046 Uiso calc R 1 H C17 .84916(16) .44636(12) 1.07262(10) .0473(5) Uani d . 1 C H17A .8059 .4486 1.1117 .057 Uiso calc R 1 H H17B .8486 .4985 1.0517 .057 Uiso calc R 1 H C18 .95382(17) .42737(15) 1.09446(12) .0637(7) Uani d . 1 C H18A .9754 .4656 1.1272 .095 Uiso calc R 1 H H18B .9981 .4292 1.0564 .095 Uiso calc R 1 H H18C .9554 .3751 1.1138 .095 Uiso calc R 1 H C19 .70862(15) .34332(10) .89591(9) .0349(5) Uani d . 1 C H19A .7698 .3144 .9064 .042 Uiso calc R 1 H H19B .6691 .3101 .8661 .042 Uiso calc R 1 H C20 .73718(15) .41645(11) .85871(9) .0383(5) Uani d . 1 C H20A .7891 .4449 .8831 .046 Uiso calc R 1 H H20B .6792 .4511 .8543 .046 Uiso calc R 1 H C21 .77516(15) .39356(11) .79091(9) .0407(5) Uani d . 1 C H21A .8233 .3505 .7956 .049 Uiso calc R 1 H H21B .7194 .3741 .7642 .049 Uiso calc R 1 H C22 .82409(17) .46097(12) .75513(10) .0477(6) Uani d . 1 C H22A .8425 .4444 .7107 .072 Uiso calc R 1 H H22B .8833 .4771 .7792 .072 Uiso calc R 1 H H22C .7780 .5049 .7525 .072 Uiso calc R 1 H 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 F1 .0499(7) .0383(6) .0540(7) -.0113(6) .0078(6) -.0029(5) F2 .0560(8) .0495(7) .0470(7) .0081(6) -.0111(6) .0052(5) F3 .0443(7) .0352(6) .0450(6) -.0030(5) .0054(5) -.0075(5) C1 .0343(12) .0256(10) .0430(11) .0018(9) -.0019(9) -.0051(8) C2 .0443(13) .0527(13) .0460(12) .0073(11) -.0022(11) .0017(10) C3 .0674(18) .0640(16) .0468(14) .0106(13) -.0039(13) .0071(11) C4 .082(2) .0487(14) .0439(13) -.0030(13) .0106(14) -.0008(11) C5 .0507(15) .0514(14) .0654(16) -.0117(11) .0222(13) -.0180(12) C6 .0390(13) .0423(12) .0522(13) -.0021(10) .0016(11) -.0150(10) B1 .0363(13) .0321(12) .0426(12) -.0013(11) -.0024(11) -.0022(10) N1 .0345(9) .0292(8) .0313(8) .0017(7) .0005(7) -.0029(6) C7 .0327(11) .0350(11) .0378(10) .0042(9) -.0021(9) -.0003(9) C8 .0441(13) .0467(12) .0556(13) -.0024(11) -.0109(11) -.0066(10) C9 .0360(13) .0683(15) .0523(13) -.0014(11) -.0098(11) -.0015(12) C10 .0569(16) .0831(18) .0722(17) .0013(14) -.0238(14) .0140(14) C11 .0404(12) .0291(10) .0390(11) .0015(9) .0004(9) .0000(9) C12 .0380(12) .0371(11) .0378(11) .0023(9) .0005(9) .0028(9) C13 .0563(15) .0444(13) .0559(13) -.0035(11) .0094(12) .0061(10) C14 .0649(17) .0516(14) .0619(15) -.0007(12) .0111(13) .0165(11) C15 .0364(11) .0303(10) .0324(10) .0007(9) -.0008(9) -.0016(8) C16 .0379(12) .0408(11) .0375(10) .0043(10) -.0023(9) -.0031(9) C17 .0470(14) .0493(13) .0456(12) .0036(11) -.0089(10) -.0074(10) C18 .0480(15) .0769(17) .0661(15) .0044(13) -.0167(13) -.0165(13) C19 .0382(11) .0329(10) .0337(10) .0030(9) .0031(9) -.0047(8) C20 .0455(13) .0355(11) .0338(10) .0020(10) .0020(9) -.0018(8) C21 .0488(14) .0401(11) .0331(10) .0067(10) .0001(9) -.0011(9) C22 .0531(14) .0530(13) .0370(11) .0048(11) .0067(10) .0030(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 '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 C6 C1 C2 115.51(18) C6 C1 B1 123.03(18) C2 C1 B1 121.43(18) C3 C2 C1 123.0(2) C3 C2 H2A 118.5 C1 C2 H2A 118.5 C4 C3 C2 119.9(2) C4 C3 H3A 120.1 C2 C3 H3A 120.1 C3 C4 C5 119.9(2) C3 C4 H4A 120.1 C5 C4 H4A 120.1 C4 C5 C6 119.6(2) C4 C5 H5A 120.2 C6 C5 H5A 120.2 C1 C6 C5 122.0(2) C1 C6 H6A 119.0 C5 C6 H6A 119.0 F2 B1 F1 107.99(16) F2 B1 F3 107.19(16) F1 B1 F3 106.08(16) F2 B1 C1 112.03(17) F1 B1 C1 111.91(16) F3 B1 C1 111.33(16) C15 N1 C11 111.58(13) C15 N1 C19 110.75(14) C11 N1 C19 106.36(13) C15 N1 C7 106.01(13) C11 N1 C7 111.19(14) C19 N1 C7 111.03(13) C8 C7 N1 116.54(15) C8 C7 H7A 108.2 N1 C7 H7A 108.2 C8 C7 H7B 108.2 N1 C7 H7B 108.2 H7A C7 H7B 107.3 C7 C8 C9 110.32(17) C7 C8 H8A 109.6 C9 C8 H8A 109.6 C7 C8 H8B 109.6 C9 C8 H8B 109.6 H8A C8 H8B 108.1 C10 C9 C8 114.17(19) C10 C9 H9A 108.7 C8 C9 H9A 108.7 C10 C9 H9B 108.7 C8 C9 H9B 108.7 H9A C9 H9B 107.6 C9 C10 H10A 109.5 C9 C10 H10B 109.5 H10A C10 H10B 109.5 C9 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C12 C11 N1 116.41(14) C12 C11 H11A 108.2 N1 C11 H11A 108.2 C12 C11 H11B 108.2 N1 C11 H11B 108.2 H11A C11 H11B 107.3 C11 C12 C13 110.12(16) C11 C12 H12A 109.6 C13 C12 H12A 109.6 C11 C12 H12B 109.6 C13 C12 H12B 109.6 H12A C12 H12B 108.2 C14 C13 C12 113.74(18) C14 C13 H13A 108.8 C12 C13 H13A 108.8 C14 C13 H13B 108.8 C12 C13 H13B 108.8 H13A C13 H13B 107.7 C13 C14 H14A 109.5 C13 C14 H14B 109.5 H14A C14 H14B 109.5 C13 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 N1 C15 C16 116.13(15) N1 C15 H15A 108.3 C16 C15 H15A 108.3 N1 C15 H15B 108.3 C16 C15 H15B 108.3 H15A C15 H15B 107.4 C15 C16 C17 109.73(16) C15 C16 H16A 109.7 C17 C16 H16A 109.7 C15 C16 H16B 109.7 C17 C16 H16B 109.7 H16A C16 H16B 108.2 C16 C17 C18 112.73(18) C16 C17 H17A 109.0 C18 C17 H17A 109.0 C16 C17 H17B 109.0 C18 C17 H17B 109.0 H17A C17 H17B 107.8 C17 C18 H18A 109.5 C17 C18 H18B 109.5 H18A C18 H18B 109.5 C17 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C20 C19 N1 117.28(14) C20 C19 H19A 108.0 N1 C19 H19A 108.0 C20 C19 H19B 108.0 N1 C19 H19B 108.0 H19A C19 H19B 107.2 C19 C20 C21 109.00(15) C19 C20 H20A 109.9 C21 C20 H20A 109.9 C19 C20 H20B 109.9 C21 C20 H20B 109.9 H20A C20 H20B 108.3 C22 C21 C20 112.67(16) C22 C21 H21A 109.1 C20 C21 H21A 109.1 C22 C21 H21B 109.1 C20 C21 H21B 109.1 H21A C21 H21B 107.8 C21 C22 H22A 109.5 C21 C22 H22B 109.5 H22A C22 H22B 109.5 C21 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag F1 B1 1.418(2) ? F2 B1 1.409(3) ? F3 B1 1.426(2) ? C1 C6 1.387(3) ? C1 C2 1.400(3) ? C1 B1 1.600(3) y C2 C3 1.372(3) ? C2 H2A .950 ? C3 C4 1.368(3) ? C3 H3A .950 ? C4 C5 1.371(3) ? C4 H4A .950 ? C5 C6 1.404(3) ? C5 H5A .950 ? C6 H6A .950 ? N1 C15 1.516(2) ? N1 C11 1.517(2) ? N1 C19 1.519(2) ? N1 C7 1.523(2) ? C7 C8 1.522(3) ? C7 H7A .990 ? C7 H7B .990 ? C8 C9 1.523(3) ? C8 H8A .990 ? C8 H8B .990 ? C9 C10 1.508(3) ? C9 H9A .990 ? C9 H9B .990 ? C10 H10A .980 ? C10 H10B .980 ? C10 H10C .980 ? C11 C12 1.515(2) ? C11 H11A .990 ? C11 H11B .990 ? C12 C13 1.517(3) ? C12 H12A .990 ? C12 H12B .990 ? C13 C14 1.500(3) ? C13 H13A .990 ? C13 H13B .990 ? C14 H14A .980 ? C14 H14B .980 ? C14 H14C .980 ? C15 C16 1.518(3) ? C15 H15A .990 ? C15 H15B .990 ? C16 C17 1.521(3) ? C16 H16A .990 ? C16 H16B .990 ? C17 C18 1.523(3) ? C17 H17A .990 ? C17 H17B .990 ? C18 H18A .980 ? C18 H18B .980 ? C18 H18C .980 ? C19 C20 1.516(3) ? C19 H19A .990 ? C19 H19B .990 ? C20 C21 1.525(3) ? C20 H20A .990 ? C20 H20B .990 ? C21 C22 1.519(3) ? C21 H21A .990 ? C21 H21B .990 ? C22 H22A .980 ? C22 H22B .980 ? C22 H22C .980 ? 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_publ_flag C7 C8 C9 C10 67.5(2) y C11 C12 C13 C14 -177.23(19) y C15 C16 C17 C18 179.70(18) y C19 C20 C21 C22 -168.75(17) y