#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/64/2016408.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_2016408 loop_ _publ_author_name 'Lennartson, Anders ' 'H\%akansson, Mikael' _publ_section_title ; Investigation of commercial sodium cacodylate trihydrate: penta-\m-aqua-disodium(I) bis(dimethylarsenate) and di-\m-aqua-bis[triaquasodium(I)] bis(dimethylarsenate) ; _journal_coeditor_code SF3063 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m13 _journal_page_last m16 _journal_volume 64 _journal_year 2008 _chemical_formula_iupac '[Na2 (H2 O1)8] (C2 H6 As O2)2' _chemical_formula_moiety 'H16 Na2 O8 2+, 2(C2 H6 As O2 -)' _chemical_formula_sum 'C4 H28 As2 Na2 O12' _chemical_formula_weight 464.08 _chemical_name_common 'sodium cacodylate tetrahydrate' _chemical_name_systematic 'di-\m-aqua-bis[triaquasodium(I)] bis(dimethylarsenate)' _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 90.00 _cell_angle_beta 109.907(8) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.516(3) _cell_length_b 8.838(2) _cell_length_c 19.635(5) _cell_measurement_reflns_used 5714 _cell_measurement_temperature 303(2) _cell_measurement_theta_max 25.50 _cell_measurement_theta_min 2.21 _cell_volume 1879.0(8) _computing_cell_refinement 'CrystalClear (Rigaku, 2000)' _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_data_reduction 'CrystalClear (Rigaku, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _diffrn_ambient_temperature 303(2) _diffrn_detector_area_resol_mean 105 _diffrn_measured_fraction_theta_full 0.941 _diffrn_measured_fraction_theta_max 0.944 _diffrn_measurement_device_type 'Rigaku R-AXIS IIc image-plate system' _diffrn_measurement_method \f _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 5714 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 2.21 _diffrn_standards_decay_% 'not measured' _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.646 _exptl_absorpt_correction_T_max 0.696 _exptl_absorpt_correction_T_min 0.373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.278 _refine_diff_density_min -0.195 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 125 _refine_ls_number_reflns 1652 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.0202 _refine_ls_R_factor_gt 0.0177 _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^)+(0.0278P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0438 _reflns_number_gt 1517 _reflns_number_total 1652 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file sf3063.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'not measured' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value 'not measured' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1879.1(8) _cod_database_code 2016408 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 C C1 0.1060(2) 1.04565(19) 0.17722(11) 0.0425(4) Uani d . 1 H H1A 0.1371 1.1313 0.1588 0.064 Uiso calc R 1 H H1B 0.1294 1.0538 0.2289 0.064 Uiso calc R 1 H H1C 0.0176 1.0430 0.1561 0.064 Uiso calc R 1 C C2 0.34923(17) 0.8666(2) 0.19694(11) 0.0383(4) Uani d . 1 H H2A 0.3817 0.9539 0.1805 0.057 Uiso calc R 1 H H2B 0.3832 0.7767 0.1837 0.057 Uiso calc R 1 H H2C 0.3711 0.8706 0.2487 0.057 Uiso calc R 1 O O1 0.11507(11) 0.71695(12) 0.18493(6) 0.0275(2) Uani d . 1 O O2 0.13842(10) 0.85626(10) 0.06215(6) 0.0243(2) Uani d . 1 O O3 0.13255(14) 0.76248(17) 0.33138(8) 0.0424(3) Uani d . 1 O O4 0.33169(13) 1.08614(14) 0.50682(8) 0.0355(3) Uani d . 1 O O5 0.37936(13) 0.64835(14) 0.50201(7) 0.0277(3) Uani d . 1 O O6 0.41984(15) 0.94080(17) 0.38455(9) 0.0394(3) Uani d . 1 Na Na1 0.27390(6) 0.86194(6) 0.43443(4) 0.02757(16) Uani d . 1 As As1 0.173618(13) 0.863667(15) 0.153124(7) 0.01910(8) Uani d . 1 H H3A 0.137(2) 0.746(3) 0.2950(14) 0.055(8) Uiso d . 1 H H3B 0.068(3) 0.753(3) 0.3327(13) 0.055(8) Uiso d . 1 H H4A 0.276(3) 1.109(3) 0.5193(16) 0.058(8) Uiso d . 1 H H4B 0.342(2) 1.162(3) 0.4851(15) 0.060(8) Uiso d . 1 H H5A 0.371(2) 0.570(3) 0.4824(12) 0.038(6) Uiso d . 1 H H5B 0.449(2) 0.658(2) 0.5194(13) 0.037(6) Uiso d . 1 H H6A 0.411(2) 1.013(3) 0.3684(13) 0.043(7) Uiso d . 1 H H6B 0.492(3) 0.940(3) 0.4146(16) 0.068(8) 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 C1 0.0568(12) 0.0292(8) 0.0532(11) 0.0011(8) 0.0339(10) -0.0085(8) C2 0.0247(9) 0.0536(12) 0.0328(9) -0.0058(7) 0.0049(7) 0.0064(7) O1 0.0321(6) 0.0273(5) 0.0286(6) -0.0053(5) 0.0173(5) -0.0002(4) O2 0.0264(6) 0.0286(6) 0.0187(5) 0.0019(4) 0.0087(5) 0.0001(4) O3 0.0286(8) 0.0722(10) 0.0284(7) -0.0055(6) 0.0124(6) -0.0105(6) O4 0.0425(8) 0.0281(6) 0.0454(7) 0.0008(6) 0.0273(6) 0.0016(6) O5 0.0216(7) 0.0292(7) 0.0309(6) 0.0001(5) 0.0072(5) -0.0046(5) O6 0.0408(9) 0.0373(8) 0.0465(8) 0.0009(6) 0.0234(7) 0.0092(7) Na1 0.0288(4) 0.0281(3) 0.0274(3) 0.0001(2) 0.0116(3) 0.0005(2) As1 0.01939(11) 0.02204(11) 0.01779(11) -0.00102(5) 0.00883(7) -0.00146(5) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 As1 C1 H1A . . 109.5 As1 C1 H1B . . 109.5 H1A C1 H1B . . 109.5 As1 C1 H1C . . 109.5 H1A C1 H1C . . 109.5 H1B C1 H1C . . 109.5 As1 C2 H2A . . 109.5 As1 C2 H2B . . 109.5 H2A C2 H2B . . 109.5 As1 C2 H2C . . 109.5 H2A C2 H2C . . 109.5 H2B C2 H2C . . 109.5 Na1 O3 H3A . . 131(2) Na1 O3 H3B . . 115.0(19) H3A O3 H3B . . 114(3) Na1 O4 H4A . . 108.0(18) Na1 O4 H4B . . 115(2) H4A O4 H4B . . 103(2) Na1 O5 Na1 . 7_566 89.66(5) Na1 O5 H5A . . 118.1(16) Na1 O5 H5A 7_566 . 103.1(16) Na1 O5 H5B . . 114.9(15) Na1 O5 H5B 7_566 . 126.6(17) H5A O5 H5B . . 105(2) Na1 O6 H6A . . 116.2(19) Na1 O6 H6B . . 112.8(19) H6A O6 H6B . . 107(3) O3 Na1 O6 . . 98.10(7) O3 Na1 O5 . . 105.12(6) O6 Na1 O5 . . 99.64(6) O3 Na1 O4 . . 144.03(6) O6 Na1 O4 . . 84.68(6) O5 Na1 O4 . . 109.75(6) O3 Na1 O5 . 7_566 90.97(6) O6 Na1 O5 . 7_566 164.22(5) O5 Na1 O5 . 7_566 90.34(5) O4 Na1 O5 . 7_566 80.43(5) O3 Na1 Na1 . 7_566 101.16(5) O6 Na1 Na1 . 7_566 144.33(6) O5 Na1 Na1 . 7_566 46.33(4) O4 Na1 Na1 . 7_566 96.58(5) O5 Na1 Na1 7_566 7_566 44.01(3) O1 As1 O2 . . 112.39(5) O1 As1 C2 . . 109.94(7) O2 As1 C2 . . 108.19(8) O1 As1 C1 . . 107.96(8) O2 As1 C1 . . 108.77(7) C2 As1 C1 . . 109.56(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 As1 1.9152(17) C1 H1A 0.9600 C1 H1B 0.9600 C1 H1C 0.9600 C2 As1 1.9095(19) C2 H2A 0.9600 C2 H2B 0.9600 C2 H2C 0.9600 O1 As1 1.6771(10) O2 As1 1.6931(12) O3 Na1 2.2965(16) O3 H3A 0.75(3) O3 H3B 0.75(3) O4 Na1 2.3969(15) O4 H4A 0.78(3) O4 H4B 0.82(3) O5 Na1 2.3878(14) O5 H5A 0.78(2) O5 H5B 0.76(2) O6 Na1 2.3218(15) O6 H6A 0.71(2) O6 H6B 0.84(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 O3 H3A O1 . 0.75(3) 2.104 2.842(2) 168.65 O3 H3B O1 2_555 0.75(3) 2.045 2.788(2) 168.71 O4 H4A O2 6_576 0.78(3) 2.059 2.835(2) 171.69 O4 H4B O2 4_555 0.82(3) 2.005 2.823(2) 175.19 O5 H5A O2 4_545 0.78(2) 2.070 2.849(2) 175.02 O5 H5B O2 8_566 0.76(2) 2.061 2.810(2) 169.77 O6 H6A O1 4_555 0.71(2) 2.053 2.758(2) 176.06 O6 H6B O4 5_676 0.84(3) 2.101 2.939(2) 173.91