#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007235.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_2007235 loop_ _publ_author_name 'Montserrat, N.' 'Moreno, V.' 'Solans, X.' 'Font-Bard\'ia, M.' _publ_section_title ; A New Phase of Sodium Succinate Hexahydrate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 578 _journal_page_last 580 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '2Na + , C4 H4 O4 2- , 6H2 O' _chemical_formula_moiety 'Na2(C4H4O4) . 6 H2O' _chemical_formula_sum 'C4 H16 Na2 O10' _chemical_formula_weight 270.15 _chemical_name_systematic ' \b-Sodium succinate hexahydrate' _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' _cell_angle_alpha 90.00 _cell_angle_beta 102.614(13) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.9033(8) _cell_length_b 6.300(3) _cell_length_c 10.717(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 12 _cell_volume 586.6(3) _computing_cell_refinement 'CAD-4/PC V2.0' _computing_data_collection 'CAD-4/PC V2.0 (Kretschmar, 1996)' _computing_data_reduction 'CFEO (Solans, 1978)' _computing_molecular_graphics 'ORTEP (Johnson, 1976; Brueggermann & Schmid, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1812 _diffrn_reflns_theta_max 29.95 _diffrn_reflns_theta_min 2.34 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time '120 min.' _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.209 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 284 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.239 _refine_diff_density_min -0.193 _refine_ls_extinction_coef 1.30(4) _refine_ls_extinction_method SHELXL93_(Sheldrick,_1993) _refine_ls_goodness_of_fit_all 1.059 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_hydrogen_treatment 'H atoms: see text' _refine_ls_matrix_type full _refine_ls_number_parameters 112 _refine_ls_number_reflns 1716 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.456 _refine_ls_restrained_S_obs 1.080 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_obs 0.0289 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.0332P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1076 _refine_ls_wR_factor_obs 0.0746 _reflns_number_observed 1467 _reflns_number_total 1716 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file jz1231.cif _[local]_cod_data_source_block virbc1 _[local]_cod_cif_authors_sg_H-M P21/c _[local]_cod_chemical_formula_sum_orig 'Na2 C4 H16 O10' _cod_database_code 2007235 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_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 Na 0.0280(2) 0.0275(2) 0.0317(2) 0.00266(12) 0.00730(13) 0.00138(12) O1 0.0257(3) 0.0285(3) 0.0379(3) 0.0009(2) 0.0047(2) -0.0044(2) O2 0.0251(3) 0.0354(3) 0.0384(3) 0.0041(2) 0.0046(2) -0.0091(2) O3 0.0275(3) 0.0390(4) 0.0463(4) -0.0058(3) 0.0094(3) -0.0106(3) O4 0.0303(3) 0.0303(3) 0.0427(4) 0.0043(2) 0.0058(2) -0.0053(3) O5 0.0303(3) 0.0296(3) 0.0306(3) -0.0012(2) 0.0060(2) -0.0010(2) C1 0.0263(4) 0.0247(4) 0.0287(3) 0.0085(2) 0.0076(3) 0.0016(3) C2 0.0246(11) 0.045(2) 0.0379(11) 0.0120(9) 0.0014(8) -0.0169(12) C2' 0.0280(11) 0.0310(12) 0.0286(8) 0.0117(8) 0.0114(8) 0.0049(9) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Na 0.90977(4) 0.00010(5) 0.13159(3) 0.02892(14) Uani d . 1 . Na O1 0.81083(7) 0.32593(10) 0.02824(6) 0.0311(2) Uani d . 1 . O O2 0.61564(7) 0.22614(11) -0.12564(6) 0.0333(2) Uani d . 1 . O O3 0.67995(8) -0.06464(12) 0.20910(7) 0.0374(2) Uani d . 1 . O O4 0.83393(7) -0.09879(11) -0.10539(7) 0.0348(2) Uani d . 1 . O O5 1.00138(7) -0.35940(10) 0.15629(6) 0.0302(2) Uani d . 1 . O C1 0.67015(9) 0.32362(12) -0.02337(7) 0.0263(2) Uani d . 1 . C H3 0.5954(17) -0.119(3) 0.1785(15) 0.046(3) Uiso d . 1 . H H3A 0.6645(16) 0.049(3) 0.2465(16) 0.049(4) Uiso d . 1 . H H4 0.7602(17) -0.005(2) -0.1234(15) 0.041(3) Uiso d . 1 . H H4A 0.7975(16) -0.194(3) -0.1530(15) 0.044(3) Uiso d . 1 . H H5 0.9333(18) -0.447(2) 0.1211(14) 0.041(3) Uiso d . 1 . H H5A 1.0604(14) -0.349(2) 0.1082(13) 0.038(3) Uiso d . 1 . H C2 0.5811(3) 0.4836(5) 0.0373(3) 0.0368(6) Uani d P 0.50 1 C H2A 0.5783(3) 0.4360(5) 0.1228(3) 0.57(16) Uiso calc PR 0.50 1 H H2B 0.6350(3) 0.6184(5) 0.0450(3) 0.080(11) Uiso calc PR 0.50 1 H C2' 0.5438(3) 0.4106(4) 0.0409(2) 0.0284(5) Uani d P 0.50 2 C H2'A 0.4732(3) 0.2975(4) 0.0502(2) 0.056(8) Uiso calc PR 0.50 2 H H2'B 0.5902(3) 0.4641(4) 0.1254(2) 0.026(5) Uiso calc PR 0.50 2 H loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 ' 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 O5 Na O3 . . 95.51(3) yes O5 Na O1 . . 159.45(3) yes O3 Na O1 . . 92.87(3) yes O5 Na O5 . 2_755 102.06(2) yes O3 Na O5 . 2_755 82.24(3) yes O1 Na O5 . 2_755 97.63(3) yes O5 Na O4 . 3_755 87.10(3) yes O3 Na O4 . 3_755 166.05(3) yes O1 Na O4 . 3_755 89.27(3) yes O5 Na O4 2_755 3_755 83.81(3) yes O5 Na O4 . . 83.66(3) yes O3 Na O4 . . 103.98(3) yes O1 Na O4 . . 76.12(3) yes O5 Na O4 2_755 . 171.24(3) yes O4 Na O4 3_755 . 89.92(3) yes O5 Na Na . 3_755 83.41(2) ? O3 Na Na . 3_755 147.56(3) ? O1 Na Na . 3_755 79.50(2) ? O5 Na Na 2_755 3_755 129.82(2) ? O4 Na Na 3_755 3_755 46.32(2) ? O4 Na Na . 3_755 43.60(2) ? O5 Na Na . 2_755 124.92(3) ? O3 Na Na . 2_755 99.36(2) ? O1 Na Na . 2_755 71.78(3) ? O5 Na Na 2_755 2_755 30.48(2) ? O4 Na Na 3_755 2_755 68.25(2) ? O4 Na Na . 2_755 140.92(2) ? Na Na Na 3_755 2_755 107.81(2) ? O5 Na Na . 2_745 30.54(2) ? O3 Na Na . 2_745 84.54(2) ? O1 Na Na . 2_745 169.92(2) ? O5 Na Na 2_755 2_745 72.39(3) ? O4 Na Na 3_755 2_745 90.97(2) ? O4 Na Na . 2_745 113.95(3) ? Na Na Na 3_755 2_745 107.78(2) ? Na Na Na 2_755 2_745 98.98(3) ? O5 Na H5A . . 18.1(3) ? O3 Na H5A . . 112.5(3) ? O1 Na H5A . . 144.8(3) ? O5 Na H5A 2_755 . 109.3(3) ? O4 Na H5A 3_755 . 72.0(3) ? O4 Na H5A . . 74.3(3) ? Na Na H5A 3_755 . 65.9(3) ? Na Na H5A 2_755 . 124.0(3) ? Na Na H5A 2_745 . 44.0(3) ? C1 O1 Na . . 115.03(5) ? Na O3 H3 . . 134.6(10) ? Na O3 H3A . . 105.0(10) ? H3 O3 H3A . . 108.1(14) ? Na O4 Na 3_755 . 90.08(3) ? Na O4 H4 3_755 . 118.5(9) ? Na O4 H4 . . 94.4(10) ? Na O4 H4A 3_755 . 111.9(10) ? Na O4 H4A . . 142.3(11) ? H4 O4 H4A . . 100.6(13) ? Na O5 Na . 2_745 118.98(3) ? Na O5 H5 . . 111.9(9) ? Na O5 H5 2_745 . 103.8(10) ? Na O5 H5A . . 95.9(9) ? Na O5 H5A 2_745 . 120.2(9) ? H5 O5 H5A . . 105.7(14) ? O1 C1 O2 . . 123.25(7) ? O1 C1 C2 . . 111.67(11) ? O2 C1 C2 . . 124.10(11) ? O1 C1 C2' . . 123.67(13) ? O2 C1 C2' . . 112.49(13) ? C2 C2 C1 3_665 . 113.3(3) ? C2 C2 H2A 3_665 . 108.9(3) ? C1 C2 H2A . . 108.91(14) ? C2 C2 H2B 3_665 . 108.9(3) ? C1 C2 H2B . . 108.91(14) ? H2A C2 H2B . . 107.7 ? C2' C2' C1 3_665 . 109.6(2) ? C2' C2' H2'A 3_665 . 109.7(2) ? C1 C2' H2'A . . 109.75(11) ? C2' C2' H2'B 3_665 . 109.7(2) ? C1 C2' H2'B . . 109.75(11) ? H2'A C2' H2'B . . 108.2 ? 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 Na O5 . 2.4022(12) yes Na O3 . 2.4054(8) yes Na O1 . 2.4063(11) yes Na O5 2_755 2.4066(8) yes Na O4 3_755 2.4397(8) yes Na O4 . 2.5584(9) yes Na Na 3_755 3.5377(9) yes Na Na 2_755 4.1430(13) yes Na Na 2_745 4.1430(13) yes Na H5A . 2.615(13) ? O1 C1 . 1.2540(10) yes O2 C1 . 1.2576(11) yes O3 H3 . 0.83(2) ? O3 H3A . 0.84(2) ? O4 Na 3_755 2.4397(8) no O4 H4 . 0.875(15) ? O4 H4A . 0.81(2) ? O5 Na 2_745 2.4066(8) ? O5 H5 . 0.84(2) ? O5 H5A . 0.815(13) ? C1 C2 . 1.513(3) yes C1 C2' . 1.542(2) yes C2 C2 3_665 1.504(5) yes C2 H2A . 0.97 ? C2 H2B . 0.97 ? C2' C2' 3_665 1.533(5) yes C2' H2'A . 0.97 ? C2' H2'B . 0.97 ? 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 H3 O2 3_655 0.827(16) 1.960(16) 2.7808(16) 171.7(16) yes O3 H3A O2 4_566 0.846(18) 2.082(18) 2.9078(17) 165.1(16) yes O4 H4 O2 . 0.873(14) 1.940(14) 2.7983(16) 167.3(15) yes O4 H4A O3 4_555 0.808(17) 2.217(17) 3.0229(18) 174.8(16) yes O5 H5 O1 1_545 0.845(15) 1.937(14) 2.7703(16) 168.5(15) yes O5 H5A O1 3_755 0.815(13) 2.051(13) 2.8627(16) 174.0(13) yes