#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/37/2103785.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_2103785 loop_ _publ_author_name 'Clemente, Dore Augusto' 'Marzotto, Armando' _publ_section_title ; 22 Space-group changes ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 43 _journal_page_last 50 _journal_paper_doi 10.1107/S0108768102022668 _journal_volume 59 _journal_year 2003 _chemical_formula_sum 'C5 H15 N2 Na O9' _chemical_formula_weight 270.18 _chemical_name_systematic ;catena-(mu!2$-Aqua)bis(diaqua-(mu!3$-beta-N-oxalyl-L-alpha,beta-diaminopropionic acid)-sodium) trihydrate ; _space_group_IT_number 20 _symmetry_space_group_name_Hall 'C 2c 2' _symmetry_space_group_name_H-M 'C 2 2 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 9.453(2) _cell_length_b 17.812(2) _cell_length_c 13.475(2) _cell_measurement_temperature 293(2) _cell_volume 2268.9(6) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.274 _diffrn_measured_fraction_theta_max 0.274 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.0133 _diffrn_reflns_av_sigmaI/netI 0.1091 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 18110 _diffrn_reflns_theta_full 67.67 _diffrn_reflns_theta_max 67.67 _diffrn_reflns_theta_min 2.29 _exptl_absorpt_coefficient_mu 0.181 _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _refine_diff_density_max 0.084 _refine_diff_density_min -0.213 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.246 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 113 _refine_ls_number_reflns 5671 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.246 _refine_ls_R_factor_all 0.0098 _refine_ls_R_factor_gt 0.0093 _refine_ls_shift/su_max 3.198 _refine_ls_shift/su_mean 0.028 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0565 _reflns_number_gt 4802 _reflns_number_total 5671 _reflns_threshold_expression >2sigma(I) _cod_data_source_file an0613.cif _cod_data_source_block yakvip _cod_database_code 2103785 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, -y+1/2, z+1/2' '-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 Na1 0.46230(2) -0.130200(8) -0.088100(15) 0.02000(3) Uiso d . 1 Na N1 0.53650(4) -0.379200(17) 0.11550(3) 0.02000(5) Uiso d . 1 N H13 0.6197(9) -0.3554(5) 0.1107(7) 0.0200(16) Uiso d . 1 H N2 0.45060(4) -0.338300(16) -0.07680(3) 0.02000(5) Uiso d . 1 N H1 0.5118(9) -0.2966(5) -0.0634(6) 0.0200(16) Uiso d . 1 H H2 0.4028(9) -0.3303(4) -0.1389(6) 0.0200(17) Uiso d . 1 H H3 0.5056(9) -0.3835(4) -0.0806(6) 0.0200(16) Uiso d . 1 H O1 0.78280(3) -0.449700(15) 0.14750(3) 0.02000(4) Uiso d . 1 O O2 0.68190(3) -0.559500(15) 0.11080(3) 0.02000(4) Uiso d . 1 O O3 0.42420(3) -0.491600(15) 0.12270(3) 0.02000(5) Uiso d . 1 O O4 0.12600(3) -0.279900(15) 0.03880(3) 0.02000(4) Uiso d . 1 O O5 0.27360(3) -0.220900(14) -0.06470(3) 0.02000(4) Uiso d . 1 O C1 0.67960(4) -0.490300(18) 0.12760(4) 0.02000(5) Uiso d . 1 C C2 0.53260(4) -0.453400(19) 0.12160(3) 0.02000(5) Uiso d . 1 C C3 0.41030(5) -0.333100(19) 0.10470(4) 0.02000(5) Uiso d . 1 C H7 0.4419(8) -0.2783(5) 0.1174(7) 0.0200(17) Uiso d . 1 H H8 0.3425(9) -0.3473(5) 0.1533(6) 0.0200(17) Uiso d . 1 H C4 0.34080(4) -0.339700(19) 0.00240(4) 0.02000(6) Uiso d . 1 C H9 0.2876(8) -0.3890(4) -0.0064(6) 0.0200(17) Uiso d . 1 H C5 0.23740(4) -0.27410(2) -0.01060(4) 0.02000(5) Uiso d . 1 C O11 0.80390(3) -0.181500(15) 0.25850(3) 0.02000(5) Uiso d . 1 O O12 0.46930(3) -0.088300(15) 0.08200(3) 0.02000(5) Uiso d . 1 O H16 0.3743(9) -0.0718(4) 0.0807(6) 0.0200(17) Uiso d . 1 H H17 0.5124(9) -0.0450(4) 0.0945(6) 0.0200(16) Uiso d . 1 H O14 0.0000 -0.31080(2) 0.2500 0.02000(6) Uiso d S 1 O O15 0.63510(3) -0.033400(16) -0.14920(3) 0.02000(4) Uiso d . 1 O H20 0.7289(16) -0.0273(9) -0.1345(12) 0.020(3) Uiso d P 0.50 H H21 0.6519(17) -0.0227(9) -0.2164(13) 0.020(3) Uiso d P 0.50 H O18 -0.5000 -0.17990(2) 0.2500 0.02000(6) Uiso d S 1 O loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Na Na 0.0362 0.0249 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 O4 Na1 O1 6_545 6_445 173.443(13) O4 Na1 O12 6_545 . 85.599(14) O1 Na1 O12 6_445 . 98.964(14) O4 Na1 O5 6_545 . 89.633(17) O1 Na1 O5 6_445 . 85.231(17) O12 Na1 O5 . . 95.894(13) O4 Na1 O14 6_545 6_545 82.067(13) O1 Na1 O14 6_445 6_545 93.523(14) O12 Na1 O14 . 6_545 167.446(12) O5 Na1 O14 . 6_545 86.389(13) O4 Na1 O15 6_545 . 97.675(18) O1 Na1 O15 6_445 . 86.696(17) O12 Na1 O15 . . 94.658(14) O5 Na1 O15 . . 167.593(15) O14 Na1 O15 6_545 . 84.719(13) C2 N1 C3 . . 123.11(3) C1 O1 Na1 . 6_545 147.50(3) C5 O4 Na1 . 6_445 140.37(3) C5 O5 Na1 . . 141.77(3) O1 C1 O2 . . 126.67(4) O1 C1 C2 . . 118.11(3) O2 C1 C2 . . 115.22(3) O3 C2 N1 . . 125.15(4) O3 C2 C1 . . 121.01(3) N1 C2 C1 . . 113.84(3) N1 C3 C4 . . 113.47(3) N2 C4 C3 . . 110.17(4) N2 C4 C5 . . 110.47(4) C3 C4 C5 . . 108.53(3) O5 C5 O4 . . 127.37(4) O5 C5 C4 . . 118.18(4) O4 C5 C4 . . 114.40(4) Na1 O14 Na1 6_445 7_545 129.146(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Na1 O4 6_545 2.3238(4) Na1 O1 6_445 2.3548(4) Na1 O12 . 2.4114(5) Na1 O5 . 2.4272(4) Na1 O14 6_545 2.4476(4) Na1 O15 . 2.5138(4) N1 C2 . 1.3247(5) N1 C3 . 1.4555(6) N2 C4 . 1.4889(7) O1 C1 . 1.2436(5) O1 Na1 6_545 2.3548(4) O2 C1 . 1.2534(4) O3 C2 . 1.2301(5) O4 C5 . 1.2501(5) O4 Na1 6_445 2.3238(4) O5 C5 . 1.2436(5) C1 C2 . 1.5393(6) C3 C4 . 1.5316(7) C4 C5 . 1.5334(5) O14 Na1 6_445 2.4476(4) O14 Na1 7_545 2.4476(4)