#------------------------------------------------------------------------------ #$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/95/2209573.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_2209573 loop_ _publ_author_name 'J. Suresh' 'R. V. Krishnakumar' 'S. Natarajan' _publ_section_title ; L-Argininium trifluoroacetate ; _journal_coeditor_code KJ2012 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o3127 _journal_page_last o3129 _journal_paper_doi 10.1107/S1600536806024743 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac 'C6 H15 N4 O2 +, C2 F3 O2 -' _chemical_formula_moiety 'C6 H15 N4 O2 +, C2 F3 O2 -' _chemical_formula_sum 'C8 H15 F3 N4 O4' _chemical_formula_weight 288.24 _chemical_name_systematic ; L-argininium trifluoroacetic acid ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.0 _cell_angle_beta 106.7700(10) _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 10.5860(6) _cell_length_b 5.6880(4) _cell_length_c 10.8780(7) _cell_measurement_reflns_used 1223 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 2 _cell_volume 627.14(7) _computing_cell_refinement 'CAD-4 EXPRESS' _computing_data_collection 'CAD-4 EXPRESS (Enraf--Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1996)' _computing_molecular_graphics 'PLATON (Spek, 2003) and MERCURY (Macrae et al., 2006)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Nonius MACH3 four-circle' _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 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 1539 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.01 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 300 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.303 _refine_diff_density_min -0.376 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 1223 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0595 _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^)+(0.1263P)^2^+0.0434P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1442 _refine_ls_wR_factor_ref 0.1505 _reflns_number_gt 1097 _reflns_number_total 1223 _reflns_threshold_expression I>2\s(I) _cod_data_source_file kj2012.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2209573 _cod_database_fobs_code 2209573 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _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 O O1 0.5373(2) 0.2646(5) 0.4198(3) 0.0404(7) Uani d . 1 O O2 0.7427(3) 0.1263(5) 0.4699(3) 0.0409(7) Uani d . 1 N N2 1.1220(3) 0.4209(7) 0.2830(3) 0.0377(8) Uani d . 1 H H2A 1.1841 0.4932 0.3388 0.045 Uiso calc R 1 N N3 1.2801(3) 0.1560(8) 0.2699(3) 0.0438(9) Uani d . 1 H H3C 1.3029 0.0285 0.2394 0.053 Uiso calc R 1 H H3D 1.3380 0.2366 0.3257 0.053 Uiso calc R 1 C C2 0.7108(3) 0.5309(7) 0.4195(3) 0.0261(7) Uani d . 1 H H2 0.7752 0.5755 0.5006 0.031 Uiso calc R 1 C C4 0.9141(3) 0.4356(8) 0.3449(3) 0.0356(8) Uani d . 1 H H4A 0.9639 0.4726 0.4326 0.043 Uiso calc R 1 H H4B 0.9034 0.2663 0.3380 0.043 Uiso calc R 1 C C1 0.6600(3) 0.2876(6) 0.4373(3) 0.0267(7) Uani d . 1 C C3 0.7786(3) 0.5522(7) 0.3138(3) 0.0314(8) Uani d . 1 H H3A 0.7883 0.7176 0.2968 0.038 Uiso calc R 1 H H3B 0.7221 0.4824 0.2359 0.038 Uiso calc R 1 N N4 1.0687(3) 0.1024(7) 0.1454(3) 0.0429(9) Uani d . 1 H H4C 0.9869 0.1429 0.1214 0.052 Uiso calc R 1 H H4D 1.0940 -0.0212 0.1136 0.052 Uiso calc R 1 N N1 0.5998(3) 0.7046(6) 0.3937(3) 0.0318(7) Uani d . 1 H H1A 0.6301 0.8472 0.3837 0.048 Uiso calc R 1 H H1B 0.5658 0.7062 0.4596 0.048 Uiso calc R 1 H H1C 0.5376 0.6637 0.3226 0.048 Uiso calc R 1 C C5 0.9896(3) 0.5197(8) 0.2539(3) 0.0378(9) Uani d . 1 H H5A 0.9406 0.4773 0.1668 0.045 Uiso calc R 1 H H5B 0.9959 0.6898 0.2582 0.045 Uiso calc R 1 C C6 1.1545(3) 0.2290(8) 0.2305(3) 0.0325(8) Uani d . 1 F F2 0.2764(4) 0.2887(6) -0.0143(3) 0.0841(12) Uani d . 1 F F1 0.3384(4) 0.5534(7) -0.1197(3) 0.0797(10) Uani d . 1 O O3 0.3711(3) 0.7280(8) 0.1804(3) 0.0569(9) Uani d . 1 O O4 0.1828(3) 0.7411(8) 0.0229(3) 0.0599(9) Uani d . 1 F F3 0.4711(3) 0.4273(10) 0.0537(4) 0.1064(16) Uani d . 1 C C7 0.2965(3) 0.6685(8) 0.0751(3) 0.0398(9) Uani d . 1 C C8 0.3464(4) 0.4837(9) -0.0010(4) 0.0486(10) Uani d . 1 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 O1 0.0213(11) 0.0461(17) 0.0551(14) -0.0060(12) 0.0130(10) 0.0056(13) O2 0.0286(12) 0.0350(15) 0.0620(15) 0.0038(11) 0.0175(11) 0.0113(12) N2 0.0190(13) 0.053(2) 0.0416(14) -0.0073(15) 0.0101(11) -0.0080(15) N3 0.0192(13) 0.067(2) 0.0433(14) 0.0035(16) 0.0052(11) -0.0076(17) C2 0.0143(13) 0.0337(18) 0.0303(14) 0.0045(14) 0.0064(11) 0.0005(14) C4 0.0215(16) 0.048(2) 0.0418(17) 0.0053(17) 0.0163(13) 0.0070(18) C1 0.0204(15) 0.0336(19) 0.0274(14) 0.0014(14) 0.0090(12) 0.0014(13) C3 0.0250(16) 0.037(2) 0.0355(14) 0.0037(16) 0.0133(12) 0.0063(15) N4 0.0224(13) 0.057(2) 0.0455(15) 0.0024(15) 0.0031(12) -0.0084(16) N1 0.0220(13) 0.0335(17) 0.0418(15) 0.0020(13) 0.0122(11) 0.0012(13) C5 0.0281(16) 0.046(2) 0.0460(18) 0.0052(18) 0.0208(14) 0.0049(18) C6 0.0200(15) 0.048(2) 0.0304(14) -0.0039(16) 0.0095(12) 0.0035(16) F2 0.131(3) 0.052(2) 0.085(2) -0.027(2) 0.056(2) -0.0171(17) F1 0.110(3) 0.081(2) 0.0637(15) -0.013(2) 0.0491(16) -0.0042(17) O3 0.0356(14) 0.075(2) 0.0485(14) 0.0120(16) -0.0060(11) -0.0151(17) O4 0.0303(14) 0.073(2) 0.0636(17) 0.0088(16) -0.0073(12) -0.015(2) F3 0.063(2) 0.125(4) 0.116(3) 0.045(2) 0.0026(18) -0.044(3) C7 0.0272(17) 0.046(2) 0.0405(17) -0.0005(18) 0.0015(13) -0.0007(17) C8 0.046(2) 0.045(2) 0.053(2) 0.000(2) 0.0121(18) -0.0016(19) 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0000 '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_publ_flag C6 N2 C5 125.3(3) y C6 N2 H2A 117.3 ? C5 N2 H2A 117.3 ? C6 N3 H3C 120.0 ? C6 N3 H3D 120.0 ? H3C N3 H3D 120.0 ? N1 C2 C1 109.7(2) y N1 C2 C3 108.7(3) y C1 C2 C3 115.5(3) y N1 C2 H2 107.5 ? C1 C2 H2 107.5 ? C3 C2 H2 107.5 ? C5 C4 C3 110.9(3) y C5 C4 H4A 109.5 ? C3 C4 H4A 109.5 ? C5 C4 H4B 109.5 ? C3 C4 H4B 109.5 ? H4A C4 H4B 108.1 ? O2 C1 O1 125.0(3) y O2 C1 C2 117.5(3) y O1 C1 C2 117.5(3) y C2 C3 C4 114.5(3) y C2 C3 H3A 108.6 ? C4 C3 H3A 108.6 ? C2 C3 H3B 108.6 ? C4 C3 H3B 108.6 ? H3A C3 H3B 107.6 ? C6 N4 H4C 120.0 ? C6 N4 H4D 120.0 ? H4C N4 H4D 120.0 ? C2 N1 H1A 109.5 ? C2 N1 H1B 109.5 ? H1A N1 H1B 109.5 ? C2 N1 H1C 109.5 ? H1A N1 H1C 109.5 ? H1B N1 H1C 109.5 ? N2 C5 C4 113.0(3) y N2 C5 H5A 109.0 ? C4 C5 H5A 109.0 ? N2 C5 H5B 109.0 ? C4 C5 H5B 109.0 ? H5A C5 H5B 107.8 ? N4 C6 N2 123.0(3) ? N4 C6 N3 118.6(4) ? N2 C6 N3 118.4(3) ? O3 C7 O4 127.4(4) ? O3 C7 C8 117.6(4) ? O4 C7 C8 115.0(3) ? F2 C8 F3 107.6(5) ? F2 C8 F1 105.5(4) ? F3 C8 F1 106.6(4) ? F2 C8 C7 111.6(4) ? F3 C8 C7 112.4(4) ? F1 C8 C7 112.8(4) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 C1 1.264(4) y O2 C1 1.247(4) y N2 C6 1.322(6) y N2 C5 1.458(4) y N2 H2A 0.8600 ? N3 C6 1.340(5) y N3 H3C 0.8600 ? N3 H3D 0.8600 ? C2 N1 1.498(4) y C2 C1 1.517(5) y C2 C3 1.525(4) y C2 H2 0.9800 ? C4 C5 1.518(5) y C4 C3 1.526(5) y C4 H4A 0.9700 ? C4 H4B 0.9700 ? C3 H3A 0.9700 ? C3 H3B 0.9700 ? N4 C6 1.310(5) y N4 H4C 0.8600 ? N4 H4D 0.8600 ? N1 H1A 0.8900 ? N1 H1B 0.8900 ? N1 H1C 0.8900 ? C5 H5A 0.9700 ? C5 H5B 0.9700 ? F2 C8 1.319(6) y F1 C8 1.330(6) y O3 C7 1.236(5) y O4 C7 1.244(5) y F3 C8 1.321(5) y C7 C8 1.524(6) y loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1A O2 1_565 0.89 2.04 2.829(4) 147 N1 H1B O1 2_656 0.89 1.96 2.835(4) 167 N1 H1C O3 . 0.89 2.01 2.832(4) 152 N2 H2A O2 2_756 0.86 2.14 2.902(4) 148 N3 H3C O3 1_645 0.86 2.03 2.888(6) 175 N3 H3D O1 1_655 0.86 2.07 2.808(4) 144 N4 H4C O4 2_645 0.86 2.09 2.872(4) 151 N4 H4D O4 1_645 0.86 2.05 2.896(5) 166 C5 H5A O4 2_645 0.97 2.49 3.426(5) 161 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 N1 C2 C1 O2 -174.3(3) y C3 C2 C1 O2 62.5(4) y N1 C2 C1 O1 4.7(4) y C3 C2 C1 O1 -118.6(3) y N1 C2 C3 C4 164.5(3) y C1 C2 C3 C4 -71.7(4) y C5 C4 C3 C2 -164.5(3) y C6 N2 C5 C4 93.6(4) y C3 C4 C5 N2 177.6(3) y C5 N2 C6 N4 -0.8(6) y C5 N2 C6 N3 -178.1(3) y O3 C7 C8 F2 115.2(5) ? O4 C7 C8 F2 -64.3(6) ? O3 C7 C8 F3 -5.7(7) ? O4 C7 C8 F3 174.7(5) ? O3 C7 C8 F1 -126.3(5) ? O4 C7 C8 F1 54.2(6) ?