#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2102066.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_2102066 _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M C2/c loop_ _publ_author_name 'Kaduk, James A.' _publ_section_title ; Terephthalate salts: salts of monopositive cations ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 474 _journal_page_last 485 _journal_volume 56 _journal_year 2000 _chemical_formula_sum 'C8 H9 N O4' _chemical_formula_weight 183.16 _chemical_name_systematic ; ? ; _symmetry_cell_setting monoclinic _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 98.04(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 18.924(4) _cell_length_b 3.7967(8) _cell_length_c 11.481(2) _cell_measurement_temperature 293(2) _cell_volume 816.8(3) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .959 _diffrn_measured_fraction_theta_max .959 _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 .0187 _diffrn_reflns_av_sigmaI/netI .0263 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 785 _diffrn_reflns_theta_full 20.01 _diffrn_reflns_theta_max 20.01 _diffrn_reflns_theta_min 3.58 _exptl_absorpt_coefficient_mu .121 _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 384 _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .05 _refine_diff_density_max .106 _refine_diff_density_min -.178 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .995 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 80 _refine_ls_number_reflns 373 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all .994 _refine_ls_R_factor_all .0405 _refine_ls_R_factor_gt .0293 _refine_ls_shift/su_max .243 _refine_ls_shift/su_mean .022 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0755 _reflns_number_gt 307 _reflns_number_total 373 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file bk0069.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 .09478(9) .1447(5) .65460(15) .0429(7) Uani d . 1 O O2 .05923(10) .0337(6) .46591(16) .0454(7) Uani d D 1 O C4 .10757(14) .1194(7) .5524(2) .0307(8) Uani d . 1 C C1 .18055(13) .1862(6) .5232(2) .0246(8) Uani d . 1 C C2 .19949(14) .1088(7) .4134(2) .0287(8) Uani d . 1 C C6 .23173(14) .3281(7) .6095(2) .0295(8) Uani d . 1 C H2A .1644(13) .004(6) .354(2) .031(7) Uiso d . 1 H H6A .2178(12) .383(7) .685(2) .037(7) Uiso d . 1 H N1 .5000 .0908(14) .7500 .0459(10) Uani d S 1 N H1 .5335(19) -.046(10) .721(3) .080(12) Uiso d . 1 H H2 .475(2) .189(12) .688(4) .106(17) Uiso d . 1 H H3 .021(2) .00(2) .496(6) .050(18) Uiso d PD .50 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 O1 .0298(12) .0699(15) .0310(12) -.0041(10) .0114(8) -.0016(10) O2 .0209(12) .0811(16) .0341(12) -.0141(13) .0034(10) .0001(11) C4 .0244(19) .0352(17) .0324(17) -.0015(13) .0038(15) .0018(14) C1 .0197(17) .0289(15) .0250(15) -.0020(13) .0024(15) .0006(13) C2 .0219(18) .0352(16) .0276(15) -.0046(14) -.0015(14) -.0031(14) C6 .029(2) .0373(18) .0231(16) .0007(14) .0065(15) .0002(14) N1 .049(3) .050(3) .042(3) .000 .020(3) .000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance O1 C4 . 1.235(3) O2 C4 . 1.294(3) C4 C1 . 1.488(3) C1 C2 . 1.390(3) C1 C6 . 1.393(3) C2 C6 7_556 1.384(4) C6 C2 7_556 1.384(4) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O1 C4 O2 . . 122.5(2) O1 C4 C1 . . 120.8(2) O2 C4 C1 . . 116.7(2) C2 C1 C6 . . 119.0(2) C2 C1 C4 . . 122.2(2) C6 C1 C4 . . 118.8(2) C1 C2 C6 . 7_556 120.3(2) C2 C6 C1 7_556 . 120.7(2) _cod_database_code 2102066