#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/04/4000492.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000492 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm0489385 _journal_year 2004 _chemical_formula_moiety 'C9 H15 N O6' _chemical_formula_sum 'C9 H15 N O6' _chemical_formula_weight 233.22 _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 _cell_angle_alpha 90 _cell_angle_beta 105.215(18) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.6267(10) _cell_length_b 23.134(8) _cell_length_c 8.082(2) _cell_measurement_reflns_used 2666 _cell_measurement_temperature 100 _cell_measurement_theta_max 30.0 _cell_measurement_theta_min 2.5 _cell_volume 1015.1(5) _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean ? _diffrn_measurement_device 'KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method ' \w scans with \k offsets' _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 0.031 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 9980 _diffrn_reflns_theta_max 30.01 _diffrn_reflns_theta_min 2.76 _diffrn_standards_decay_% <2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type none _exptl_crystal_colour color _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description fragment _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 154 _refine_ls_number_reflns 2949 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.076 _refine_ls_R_factor_gt 0.045 _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^)+(0.0453P)^2^+0.1619P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.104 _refine_ls_wR_factor_ref 0.113 _reflns_number_gt 2076 _reflns_number_total 2949 _reflns_threshold_expression I>2\s(I) _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_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4000492 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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.07689(19) 0.63841(5) -0.28525(12) 0.0191(3) Uani 1 1 d . . . O2 O 0.24530(18) 0.58457(5) -0.05540(13) 0.0183(2) Uani 1 1 d . . . O3 O 0.4107(2) 0.44702(5) 0.18305(14) 0.0202(3) Uani 1 1 d . . . H3 H 0.558(3) 0.4378(9) 0.139(2) 0.030 Uiso 1 1 d . . . O4 O 0.58128(18) 0.53146(5) 0.28883(13) 0.0197(3) Uani 1 1 d . . . O5 O 0.83222(19) 0.73063(5) 0.64716(13) 0.0195(2) Uani 1 1 d . . . H5 H 0.923(3) 0.6916(9) 0.670(2) 0.029 Uiso 1 1 d . . . O6 O 0.4673(2) 0.76983(5) 0.53572(14) 0.0233(3) Uani 1 1 d . . . N1 N 0.1767(2) 0.61769(5) 0.26304(14) 0.0135(3) Uani 1 1 d . . . H1N H 0.291(3) 0.6064(8) 0.203(2) 0.016 Uiso 1 1 d . . . C1 C -0.0677(2) 0.62604(7) 0.13211(17) 0.0150(3) Uani 1 1 d . . . H1A H -0.1778 0.6488 0.1848 0.018 Uiso 1 1 calc R . . H1B H -0.1449 0.5878 0.1004 0.018 Uiso 1 1 calc R . . C2 C -0.0454(3) 0.65652(7) -0.02881(17) 0.0147(3) Uani 1 1 d . . . H2A H 0.0331 0.6946 0.0037 0.018 Uiso 1 1 calc R . . H2B H -0.2130 0.6636 -0.1032 0.018 Uiso 1 1 calc R . . C3 C 0.1013(3) 0.62391(7) -0.13135(17) 0.0153(3) Uani 1 1 d . . . C4 C 0.1601(3) 0.56801(7) 0.38046(17) 0.0149(3) Uani 1 1 d . . . H4A H 0.0056 0.5714 0.4165 0.018 Uiso 1 1 calc R . . H4B H 0.2996 0.5702 0.4846 0.018 Uiso 1 1 calc R . . C5 C 0.1653(3) 0.51008(7) 0.29456(18) 0.0151(3) Uani 1 1 d . . . H5A H 0.1320 0.4792 0.3704 0.018 Uiso 1 1 calc R . . H5B H 0.0322 0.5090 0.1866 0.018 Uiso 1 1 calc R . . C6 C 0.4084(3) 0.49787(7) 0.25476(17) 0.0144(3) Uani 1 1 d . . . C7 C 0.2569(3) 0.67289(7) 0.35969(17) 0.0154(3) Uani 1 1 d . . . H7A H 0.1443 0.6815 0.4322 0.019 Uiso 1 1 calc R . . H7B H 0.2439 0.7050 0.2767 0.019 Uiso 1 1 calc R . . C8 C 0.5197(3) 0.67000(7) 0.47252(19) 0.0206(3) Uani 1 1 d . . . H8A H 0.5297 0.6408 0.5635 0.025 Uiso 1 1 calc R . . H8B H 0.6313 0.6578 0.4025 0.025 Uiso 1 1 calc R . . C9 C 0.6021(3) 0.72802(7) 0.55382(18) 0.0163(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0223(5) 0.0222(6) 0.0130(5) 0.0004(4) 0.0047(4) 0.0022(5) O2 0.0201(5) 0.0184(6) 0.0166(5) 0.0007(4) 0.0052(4) 0.0049(4) O3 0.0186(5) 0.0188(6) 0.0247(5) -0.0066(5) 0.0084(4) -0.0009(4) O4 0.0150(5) 0.0201(6) 0.0233(5) -0.0023(4) 0.0038(4) -0.0020(4) O5 0.0187(5) 0.0164(6) 0.0198(5) 0.0020(4) -0.0015(4) -0.0023(4) O6 0.0220(6) 0.0167(6) 0.0290(6) -0.0015(5) 0.0031(5) 0.0009(5) N1 0.0143(6) 0.0144(7) 0.0120(5) -0.0001(5) 0.0035(5) -0.0009(5) C1 0.0123(7) 0.0184(8) 0.0135(6) 0.0007(6) 0.0019(5) -0.0006(6) C2 0.0145(7) 0.0155(8) 0.0135(6) -0.0003(6) 0.0024(5) 0.0015(6) C3 0.0149(7) 0.0146(7) 0.0156(6) -0.0016(6) 0.0027(5) -0.0021(6) C4 0.0176(7) 0.0145(7) 0.0132(6) 0.0021(5) 0.0052(5) -0.0016(6) C5 0.0148(7) 0.0151(8) 0.0156(6) 0.0007(6) 0.0043(5) -0.0018(6) C6 0.0151(7) 0.0162(8) 0.0106(6) 0.0018(5) 0.0009(5) 0.0015(6) C7 0.0179(7) 0.0135(8) 0.0146(6) -0.0003(5) 0.0038(5) -0.0003(6) C8 0.0173(7) 0.0189(8) 0.0228(7) -0.0039(6) 0.0008(6) 0.0007(6) C9 0.0181(7) 0.0170(8) 0.0137(6) 0.0019(5) 0.0042(6) -0.0020(6)