#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/49/2204925.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_2204925 loop_ _publ_author_name 'Zhang, Xiu-Lian' 'Chen, Xiao-Ming' 'Ng, Seik Weng' _publ_section_title ; Melaminium di(hydrogen oxalate) ; _journal_issue 1 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first o156 _journal_page_last o157 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac 'C3 H8 N6 2+, 2C2 H O4 -' _chemical_formula_moiety 'C3 H8 N6 2+, 2C2 H O4 -' _chemical_formula_sum 'C7 H10 N6 O8' _chemical_formula_weight 306.21 _chemical_name_systematic ; Melaminium(2+) di(hydrogen oxalate) ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/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 _cell_angle_beta 108.402(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.829(2) _cell_length_b 8.4280(10) _cell_length_c 6.8415(8) _cell_measurement_reflns_used 1045 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 27.3 _cell_measurement_theta_min 3.3 _cell_volume 1139.6(2) _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_collection 'SMART (Bruker, 2002)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _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 0.996 _diffrn_measured_fraction_theta_max 0.97 _diffrn_measurement_device_type 'Bruker APEX 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 0.019 _diffrn_reflns_av_sigmaI/netI 0.024 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_number 3287 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.6 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type none _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 632 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.26 _refine_diff_density_min -0.22 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 117 _refine_ls_number_reflns 1269 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.06 _refine_ls_R_factor_all 0.049 _refine_ls_R_factor_gt 0.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0711P)^2^+0.2079P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.110 _refine_ls_wR_factor_ref 0.116 _reflns_number_gt 1068 _reflns_number_total 1269 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file lh6334.cif _[local]_cod_cif_authors_sg_H-M 'C 2/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. '_exptl_absorpt_correction_type' value 'None' changed to 'none' 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_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2204925 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_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 0.39408(6) 0.33040(10) 0.5019(2) 0.0351(3) Uani d . 1 O O2 0.33277(6) 0.55290(10) 0.4576(2) 0.0347(4) Uani d . 1 O O3 0.28898(6) 0.18790(10) 0.2248(2) 0.0325(3) Uani d D 1 O O4 0.22063(5) 0.36290(10) 0.3048(2) 0.0359(3) Uani d . 1 O N1 0.5000 0.5051(2) 0.7500 0.0294(5) Uani d SD 1 N N2 0.44680(10) 0.7417(2) 0.6298(2) 0.0248(3) Uani d D 1 N N3 0.39420(10) 0.9795(2) 0.5160(2) 0.0272(3) Uani d D 1 N N4 0.5000 0.9864(2) 0.7500 0.0241(4) Uani d S 1 N C1 0.5000 0.6586(2) 0.7500 0.0230(5) Uani d S 1 C C2 0.44746(7) 0.9047(2) 0.6330(2) 0.0219(3) Uani d . 1 C C3 0.34060(10) 0.4069(2) 0.4346(2) 0.0256(4) Uani d . 1 C C4 0.27650(10) 0.3165(2) 0.3126(2) 0.0253(4) Uani d . 1 C H3o 0.2510(10) 0.141(2) 0.164(3) 0.062(7) Uiso d D 1 H H1 0.4650(10) 0.458(2) 0.672(3) 0.034(5) Uiso d D 1 H H2 0.4120(10) 0.688(2) 0.567(3) 0.034(5) Uiso d D 1 H H3a 0.3930(10) 1.0800(10) 0.517(3) 0.032(5) Uiso d D 1 H H3b 0.3600(10) 0.930(2) 0.437(3) 0.040(5) Uiso d 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 O1 0.0217(6) 0.0237(6) 0.0496(8) 0.0022(4) -0.0036(5) -0.0034(5) O2 0.0281(6) 0.0198(6) 0.0458(8) 0.0013(5) -0.0032(5) -0.0047(5) O3 0.0269(7) 0.0224(6) 0.0417(7) -0.0029(5) 0.0016(5) -0.0070(5) O4 0.0215(6) 0.0305(7) 0.0482(8) 0.0036(5) 0.0002(5) -0.0008(5) N1 0.0230(10) 0.0210(10) 0.0350(10) 0.000 -0.0040(10) 0.000 N2 0.0170(10) 0.0210(10) 0.0300(10) -0.0030(10) -0.0020(10) 0.0000(10) N3 0.0190(10) 0.0240(10) 0.0320(10) 0.0010(10) -0.0030(10) 0.0020(10) N4 0.0180(10) 0.0210(10) 0.0290(10) 0.000 0.0010(10) 0.000 C1 0.0200(10) 0.0220(10) 0.0240(10) 0.000 0.0040(10) 0.000 C2 0.0180(10) 0.0240(10) 0.0230(10) 0.0000(10) 0.0050(10) 0.0010(10) C3 0.0230(10) 0.0210(10) 0.0290(10) 0.0000(10) 0.0030(10) 0.0020(10) C4 0.0240(10) 0.0180(10) 0.0280(10) 0.0030(10) 0.0000(10) 0.0050(10) 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_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 N2 C2 . . 120.50(10) yes C2 N4 C2 6_657 . 117.5(2) yes N1 C1 N2 . . 121.30(10) yes N1 C1 N2 . 6_657 121.30(10) yes N2 C1 N2 . 6_657 117.4(2) yes N2 C2 N3 . . 118.00(10) yes N2 C2 N4 . . 122.00(10) yes N3 C2 N4 . . 119.90(10) yes O1 C3 O2 . . 126.80(10) yes O1 C3 C4 . . 117.90(10) yes O2 C3 C4 . . 115.40(10) yes O3 C4 O4 . . 125.1(2) yes O3 C4 C3 . . 113.40(10) yes O4 C4 C3 . . 121.50(10) yes C4 O3 H3o . . 109(2) no C1 N1 H1 . . 118.0(10) no C1 N2 H2 . . 116.0(10) no C2 N2 H2 . . 123.0(10) no C2 N3 H3a . . 120.0(10) no C2 N3 H3b . . 122.0(10) no H3a N3 H3b . . 118(2) 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 O1 C3 . 1.242(2) yes O2 C3 . 1.257(2) yes O3 C4 . 1.305(2) yes O4 C4 . 1.214(2) yes C1 N1 . 1.294(3) yes C1 N2 . 1.349(2) yes C1 N2 6_657 1.349(2) no C2 N2 . 1.374(2) yes C2 N3 . 1.308(2) yes C2 N4 . 1.326(2) yes N4 C2 6_657 1.326(2) no C3 C4 . 1.535(2) yes O3 H3o . 0.860(10) no N1 H1 . 0.850(10) no N2 H2 . 0.860(10) no N3 H3a . 0.850(10) no N3 H3b . 0.860(10) 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 O3 H3o O2 8_546 0.860(10) 1.840(10) 2.699(2) 176(2) yes N1 H1 O1 . 0.850(10) 1.900(10) 2.748(2) 173(2) yes N2 H2 O2 . 0.860(10) 1.940(10) 2.792(2) 173(2) yes N3 H3a O1 1_565 0.850(10) 2.110(10) 2.959(2) 175(2) yes N3 H3b O4 8_556 0.860(10) 2.030(10) 2.861(2) 164(2) yes 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 C1 N2 C2 . . 179.50(10) no N2 C1 N2 C2 6_657 . -0.50(10) no N3 C2 N2 C1 . . -178.90(10) no N4 C2 N2 C1 . . 1.1(2) no N3 C2 N4 C2 . 6_657 179.4(2) no N2 C2 N4 C2 . 6_657 -0.50(10) no O1 C3 C4 O4 . . 153.4(2) no O2 C3 C4 O4 . . -25.8(2) no O1 C3 C4 O3 . . -25.6(2) no O2 C3 C4 O3 . . 155.30(10) no