#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2203360.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_2203360 loop_ _publ_author_name 'Zhang, Jian' 'Kang, Yao' 'Wen, Yi-Hang' 'Li, Zhao-Ji' 'Qin, Ye-Yan' 'Yao, Yuan-Gen' _publ_section_title ; Bis(melaminium) terephthalate dihydrate ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o462 _journal_page_last o463 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '2C3 H7 N6 1+, C8 H4 O4 2-, 2H2 O' _chemical_formula_moiety '2C3 H7 N6 1+, C8 H4 O4 2-, 2H2 O' _chemical_formula_sum 'C14 H22 N12 O6' _chemical_formula_weight 454.44 _chemical_name_systematic ; Bis(melaminium) terephthalate dihydrate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 93.33(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.809(4) _cell_length_b 20.164(10) _cell_length_c 7.062(6) _cell_measurement_reflns_used 1132 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.11 _cell_measurement_theta_min 2.02 _cell_volume 968.0(11) _computing_cell_refinement 'SMART and SAINT (Siemens,1994)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction 'XPREP in SHELXTL (Siemens, 1994)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution SHELXTL _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method '\f and \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 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_number 3095 _diffrn_reflns_theta_full 25.11 _diffrn_reflns_theta_max 25.11 _diffrn_reflns_theta_min 2.02 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_correction_T_min 0.975 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 476 _exptl_crystal_size_max .20 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .15 _refine_diff_density_max 0.269 _refine_diff_density_min -0.258 _refine_ls_extinction_coef 0.009(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 154 _refine_ls_number_reflns 1691 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_gt 0.0669 _refine_ls_shift/su_max 0.170 _refine_ls_shift/su_mean 0.010 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0718P)^2^+1.0433P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1511 _refine_ls_wR_factor_ref 0.1741 _reflns_number_gt 1215 _reflns_number_total 1691 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wn6215.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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_original_cell_volume 967.9(11) _cod_database_code 2203360 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 N3 0.2912(4) 0.69529(13) 0.4061(4) 0.0308(7) Uani d . 1 N H3A 0.3021 0.7378 0.4113 0.037 Uiso calc R 1 H O2 0.3209(3) 0.82958(11) 0.4212(4) 0.0395(7) Uani d . 1 O O1 0.6320(4) 0.82430(11) 0.5293(4) 0.0412(7) Uani d . 1 O N2 0.4269(4) 0.59022(13) 0.4708(4) 0.0316(7) Uani d . 1 N N1 0.0989(4) 0.60209(14) 0.3276(4) 0.0353(7) Uani d . 1 N N6 0.6065(4) 0.68518(14) 0.5335(4) 0.0384(8) Uani d . 1 N H6A 0.7058 0.6619 0.5750 0.046 Uiso calc R 1 H H6B 0.6142 0.7277 0.5326 0.046 Uiso calc R 1 H N5 0.2329(5) 0.50096(14) 0.3999(5) 0.0435(8) Uani d . 1 N H5A 0.3279 0.4763 0.4439 0.052 Uiso calc R 1 H H5B 0.1247 0.4832 0.3561 0.052 Uiso calc R 1 H C4 0.4895(5) 0.93072(15) 0.4904(5) 0.0292(8) Uani d . 1 C C3 0.4425(5) 0.65558(15) 0.4710(5) 0.0275(8) Uani d . 1 C C2 0.2532(5) 0.56633(16) 0.3997(5) 0.0302(8) Uani d . 1 C N4 -0.0197(4) 0.70654(15) 0.2662(4) 0.0421(9) Uani d . 1 N H4A -0.1284 0.6901 0.2191 0.050 Uiso calc R 1 H H4B -0.0033 0.7488 0.2700 0.050 Uiso calc R 1 H C5 0.3396(5) 0.97024(17) 0.4089(5) 0.0350(9) Uani d . 1 C H5C 0.2311 0.9502 0.3464 0.042 Uiso calc R 1 H C8 0.6510(5) 0.96178(16) 0.5811(5) 0.0331(8) Uani d . 1 C H8A 0.7535 0.9364 0.6354 0.040 Uiso calc R 1 H C9 0.4795(5) 0.85639(16) 0.4794(5) 0.0298(8) Uani d . 1 C C1 0.1229(5) 0.66663(16) 0.3330(5) 0.0307(8) Uani d . 1 C OW -0.0553(5) 0.85744(16) 0.2865(5) 0.0517(8) Uani d . 1 O HW1B 0.065(8) 0.854(2) 0.337(6) 0.067(14) Uiso d . 1 H HW1A -0.127(9) 0.859(3) 0.380(8) 0.11(2) Uiso d . 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 N3 0.0289(15) 0.0153(14) 0.0476(18) -0.0010(12) -0.0043(13) -0.0005(12) O2 0.0291(14) 0.0205(13) 0.0680(18) -0.0030(10) -0.0059(12) -0.0004(11) O1 0.0340(14) 0.0195(13) 0.0681(18) 0.0029(11) -0.0139(12) 0.0003(11) N2 0.0306(16) 0.0198(15) 0.0440(17) -0.0025(12) -0.0023(13) 0.0007(12) N1 0.0302(16) 0.0235(16) 0.0512(19) -0.0011(12) -0.0053(13) -0.0037(13) N6 0.0312(17) 0.0203(15) 0.062(2) -0.0030(12) -0.0117(14) 0.0036(14) N5 0.0352(17) 0.0239(16) 0.069(2) -0.0050(13) -0.0130(15) -0.0016(14) C4 0.0289(18) 0.0222(17) 0.0364(19) -0.0019(14) -0.0003(14) 0.0014(14) C3 0.0276(17) 0.0209(17) 0.0335(18) -0.0017(15) -0.0013(14) -0.0002(14) C2 0.0309(18) 0.0232(18) 0.0366(19) -0.0001(15) 0.0020(15) -0.0010(14) N4 0.0319(16) 0.0251(17) 0.067(2) -0.0003(13) -0.0121(15) -0.0001(14) C5 0.031(2) 0.0253(18) 0.047(2) -0.0013(15) -0.0087(16) -0.0005(16) C8 0.0295(19) 0.0217(18) 0.047(2) 0.0016(15) -0.0068(15) -0.0002(15) C9 0.0283(19) 0.0223(17) 0.0386(19) 0.0004(15) -0.0010(14) -0.0009(14) C1 0.0257(18) 0.0258(19) 0.040(2) -0.0008(15) -0.0025(14) -0.0030(15) OW 0.0345(17) 0.057(2) 0.062(2) -0.0017(14) -0.0100(15) -0.0006(15) 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' 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 _geom_angle_publ_flag C1 N3 C3 . 118.8(3) no C1 N3 H3A . 120.6 no C3 N3 H3A . 120.6 no C3 N2 C2 . 115.2(3) no C1 N1 C2 . 115.2(3) no C3 N6 H6A . 120.0 no C3 N6 H6B . 120.0 no H6A N6 H6B . 120.0 no C2 N5 H5A . 120.0 no C2 N5 H5B . 120.0 no H5A N5 H5B . 120.0 no C8 C4 C5 . 118.3(3) no C8 C4 C9 . 120.4(3) no C5 C4 C9 . 121.3(3) no N6 C3 N2 . 121.2(3) no N6 C3 N3 . 117.1(3) no N2 C3 N3 . 121.8(3) no N5 C2 N2 . 116.4(3) no N5 C2 N1 . 116.9(3) no N2 C2 N1 . 126.7(3) no C1 N4 H4A . 120.0 no C1 N4 H4B . 120.0 no H4A N4 H4B . 120.0 no C8 C5 C4 3_676 121.2(3) no C8 C5 H5C 3_676 119.4 no C4 C5 H5C . 119.4 no C5 C8 C4 3_676 120.5(3) no C5 C8 H8A 3_676 119.8 no C4 C8 H8A . 119.8 no O1 C9 O2 . 123.5(3) no O1 C9 C4 . 117.7(3) no O2 C9 C4 . 118.8(3) no N1 C1 N4 . 120.3(3) no N1 C1 N3 . 122.3(3) no N4 C1 N3 . 117.4(3) no HW1B OW HW1A . 105(5) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N3 C1 . 1.358(4) no N3 C3 . 1.363(4) no N3 H3A . 0.8600 no O2 C9 . 1.255(4) no O1 C9 . 1.256(4) no N2 C3 . 1.322(4) no N2 C2 . 1.347(4) no N1 C1 . 1.312(4) no N1 C2 . 1.349(4) no N6 C3 . 1.320(4) no N6 H6A . 0.8600 no N6 H6B . 0.8600 no N5 C2 . 1.325(4) no N5 H5A . 0.8600 no N5 H5B . 0.8600 no C4 C8 . 1.389(5) no C4 C5 . 1.393(5) no C4 C9 . 1.502(5) no N4 C1 . 1.326(4) no N4 H4A . 0.8600 no N4 H4B . 0.8600 no C5 C8 3_676 1.374(5) no C5 H5C . 0.9300 no C8 C5 3_676 1.374(5) no C8 H8A . 0.9300 no OW HW1B . 0.87(5) no OW HW1A . 0.84(6) no 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 _geom_hbond_publ_flag N3 H3A O2 . 0.86 1.86 2.717(4) 179 yes N6 H6A OW 4_676 0.86 2.18 2.959(4) 151 yes N6 H6B O1 . 0.86 1.95 2.811(4) 180 yes N5 H5A N2 3_666 0.86 2.20 3.055(4) 175 yes N4 H4A O1 4_475 0.86 2.07 2.889(4) 159 yes N4 H4B OW . 0.86 2.22 3.056(5) 163 yes OW HW1B O2 . 0.87(5) 1.88(5) 2.738(4) 168(4) yes OW HW1A O1 1_455 0.84(6) 2.13(6) 2.889(5) 151(6) yes