#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2217427.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_2217427 loop_ _publ_author_name 'Zhu, Bao-Yong' 'Cui, De-Liang' 'Jing, Hai-Peng' _publ_section_title ; Melaminium sulfate ; _journal_coeditor_code BT2656 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o351 _journal_volume 64 _journal_year 2008 _chemical_formula_iupac 'C3 H8 N6 2+, S O4 2-' _chemical_formula_moiety 'C3 H8 N6 2+, S O4 2-' _chemical_formula_sum 'C3 H8 N6 O4 S' _chemical_formula_weight 224.21 _chemical_name_systematic ; Melaminium sulfate ; _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 _cell_angle_alpha 90.00 _cell_angle_beta 129.7390(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 18.5787(3) _cell_length_b 8.6272(2) _cell_length_c 12.7945(4) _cell_measurement_reflns_used 2920 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.76 _cell_volume 1576.94(7) _computing_cell_refinement 'APEX2 (Bruker, 2005)' _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_data_reduction 'APEX2 (Bruker, 2005)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX2 CCD' _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 0.0129 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 3793 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 2.76 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_T_max 0.8996 _exptl_absorpt_correction_T_min 0.8785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(APEX2; Bruker, 2005)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.889 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 928 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _refine_diff_density_max 0.479 _refine_diff_density_min -0.454 _refine_ls_extinction_coef 0.0037(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 1794 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.998 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0312 _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^)+(0.041P)^2^+3.6165P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0864 _refine_ls_wR_factor_ref 0.0885 _reflns_number_gt 1672 _reflns_number_total 1794 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt2656.cif _[local]_cod_data_source_block I _[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. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2217427 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_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 S S1 0.65733(3) 0.06360(5) 0.27385(4) 0.02105(15) Uani d . 1 O O2 0.63929(12) 0.11467(16) 0.36667(16) 0.0369(4) Uani d . 1 O O4 0.70593(10) -0.08710(15) 0.32413(17) 0.0348(4) Uani d . 1 C C2 0.84604(12) 0.9717(2) 0.65207(17) 0.0210(3) Uani d . 1 N N5 0.86032(10) 0.82418(17) 0.63479(15) 0.0215(3) Uani d . 1 N N3 0.95352(12) 1.16685(18) 0.54108(18) 0.0312(4) Uani d . 1 H H3A 0.9834 1.1488 0.5118 0.037 Uiso calc R 1 H H3B 0.9448 1.2607 0.5534 0.037 Uiso calc R 1 O O3 0.71951(10) 0.17704(15) 0.28119(15) 0.0309(3) Uani d . 1 N N2 0.80592(11) 1.00382(18) 0.70342(17) 0.0277(3) Uani d . 1 H H2A 0.7879 0.9301 0.7272 0.033 Uiso calc R 1 H H2B 0.7974 1.0988 0.7136 0.033 Uiso calc R 1 C C3 0.92125(12) 1.0513(2) 0.56700(18) 0.0222(3) Uani d . 1 N N4 0.93490(11) 0.90603(17) 0.54780(16) 0.0236(3) Uani d . 1 N N1 0.91024(13) 0.64908(18) 0.55885(18) 0.0317(4) Uani d . 1 H H1A 0.9372 0.6259 0.5259 0.038 Uiso calc R 1 H H1B 0.8889 0.5768 0.5787 0.038 Uiso calc R 1 O O1 0.56934(11) 0.0514(2) 0.13681(16) 0.0440(4) Uani d . 1 N N6 0.87638(11) 1.08607(18) 0.61675(16) 0.0232(3) Uani d . 1 C C1 0.90174(12) 0.7934(2) 0.57868(17) 0.0219(3) Uani d . 1 H H6 0.8684(18) 1.183(3) 0.626(2) 0.042(7) Uiso d . 1 H H5 0.8388(18) 0.749(3) 0.651(3) 0.044(7) Uiso 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 S1 0.0277(2) 0.0160(2) 0.0288(2) 0.00029(15) 0.0224(2) 0.00143(15) O2 0.0657(10) 0.0212(7) 0.0574(9) -0.0009(7) 0.0549(9) -0.0015(6) O4 0.0425(8) 0.0182(6) 0.0605(10) 0.0067(6) 0.0408(8) 0.0085(6) C2 0.0228(8) 0.0197(8) 0.0233(8) -0.0007(6) 0.0160(7) -0.0004(6) N5 0.0284(7) 0.0166(7) 0.0289(7) -0.0010(6) 0.0226(7) 0.0004(6) N3 0.0438(9) 0.0183(7) 0.0528(10) -0.0030(7) 0.0407(9) -0.0011(7) O3 0.0416(8) 0.0189(6) 0.0502(8) -0.0047(5) 0.0377(7) -0.0022(6) N2 0.0395(9) 0.0202(7) 0.0418(9) -0.0002(6) 0.0345(8) -0.0006(6) C3 0.0246(8) 0.0201(8) 0.0274(8) -0.0013(6) 0.0191(7) -0.0010(6) N4 0.0296(8) 0.0185(7) 0.0345(8) -0.0010(6) 0.0259(7) -0.0010(6) N1 0.0519(10) 0.0172(7) 0.0516(10) -0.0016(7) 0.0449(9) -0.0018(7) O1 0.0361(8) 0.0554(10) 0.0329(8) -0.0085(7) 0.0185(7) 0.0045(7) N6 0.0320(8) 0.0156(7) 0.0330(8) -0.0002(6) 0.0259(7) -0.0012(6) C1 0.0254(8) 0.0194(8) 0.0262(8) -0.0003(6) 0.0188(7) -0.0007(6) 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' S S 0.1246 0.1234 '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 O1 S1 O3 111.02(9) n O1 S1 O4 111.51(10) n O3 S1 O4 108.77(8) n O1 S1 O2 109.36(10) n O3 S1 O2 108.65(8) n O4 S1 O2 107.42(9) n N2 C2 N5 121.41(16) ? N2 C2 N6 120.69(16) ? N5 C2 N6 117.88(15) n C2 N5 C1 120.25(15) n C2 N5 H5 120.6(18) ? C1 N5 H5 118.9(19) ? C3 N3 H3A 120.0 ? C3 N3 H3B 120.0 ? H3A N3 H3B 120.0 ? C2 N2 H2A 120.0 ? C2 N2 H2B 120.0 ? H2A N2 H2B 120.0 ? N3 C3 N4 119.80(16) ? N3 C3 N6 117.71(16) ? N4 C3 N6 122.46(16) n C3 N4 C1 116.79(15) n C1 N1 H1A 120.0 ? C1 N1 H1B 120.0 ? H1A N1 H1B 120.0 ? C2 N6 C3 120.35(15) n C2 N6 H6 120.8(17) ? C3 N6 H6 118.8(17) ? N1 C1 N4 120.09(16) ? N1 C1 N5 117.76(16) ? N4 C1 N5 122.13(15) n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S1 O1 1.4470(10) n S1 O3 1.4710(10) n S1 O4 1.4750(10) n S1 O2 1.4920(10) n C2 N2 1.300(2) ? C2 N5 1.347(2) n C2 N6 1.350(2) n N5 C1 1.373(2) n N5 H5 0.85(3) ? N3 C3 1.310(2) ? N3 H3A 0.8600 ? N3 H3B 0.8600 ? N2 H2A 0.8600 ? N2 H2B 0.8600 ? C3 N4 1.333(2) n C3 N6 1.367(2) n N4 C1 1.338(2) n N1 C1 1.300(2) ? N1 H1A 0.8600 ? N1 H1B 0.8600 ? N6 H6 0.87(3) ? 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 N6 H6 O2 7_666 0.87(3) 1.76(3) 2.622(2) 171(3) N5 H5 O4 7_656 0.85(3) 1.76(3) 2.608(2) 176(3) N3 H3B O2 7_666 0.86 2.59 3.244(2) 134.1 N3 H3B O1 8_566 0.86 2.44 2.944(2) 117.9 N3 H3A N4 5_776 0.86 2.14 3.000(2) 175.7 N2 H2B O3 7_666 0.86 1.97 2.822(2) 172.1 N2 H2A O3 6_566 0.86 2.02 2.836(2) 159.0 N1 H1B O2 7_656 0.86 1.99 2.838(2) 168.6 N1 H1A O1 8_556 0.86 2.43 2.992(2) 123.1 N1 H1A O1 4_655 0.86 2.11 2.887(2) 150.7 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 N2 C2 N5 C1 179.14(16) N6 C2 N5 C1 -2.1(2) N3 C3 N4 C1 178.76(17) N6 C3 N4 C1 0.5(3) N2 C2 N6 C3 177.84(17) N5 C2 N6 C3 -0.9(3) N3 C3 N6 C2 -176.50(17) N4 C3 N6 C2 1.8(3) C3 N4 C1 N1 178.06(18) C3 N4 C1 N5 -3.6(3) C2 N5 C1 N1 -177.10(17) C2 N5 C1 N4 4.6(3)