#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2214425.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_2214425 loop_ _publ_author_name 'Ballirano, Paolo' 'Belardi, Girolamo' 'Bosi, Ferdinando' _publ_section_title ; Redetermination of the Tutton's salt Cs~2~[Cu(H~2~O)~6~](SO~4~)~2~ ; _journal_coeditor_code WM2127 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i164 _journal_page_last i165 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac 'Cs2 [Cu (H2 O)6] (S O4)2' _chemical_formula_structural 'Cs2 [Cu (H2 O)6] (S O4)2' _chemical_formula_sum 'Cs2 Cu H12 O14 S2' _chemical_formula_weight 629.61 _chemical_name_common 'Caesium hexaaquacopper sulfate' _chemical_name_systematic ; Dicaesium hexaaquacopper(II) bis[sulfate(VI)] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _cell_angle_alpha 90.00 _cell_angle_beta 106.199(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.4383(6) _cell_length_b 12.7605(12) _cell_length_c 6.3130(6) _cell_measurement_reflns_used 58 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.5 _cell_measurement_theta_min 4.0 _cell_volume 730.14(11) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_data_reduction XSCANS _computing_molecular_graphics 'ATOMS (Dowty, 2003)' _computing_publication_material ; PARST (Nardelli, 1982) and publCIF (Westrip, 2007) ; _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method \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 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3436 _diffrn_reflns_reduction_process 'LP correction applied' _diffrn_reflns_theta_full 35.03 _diffrn_reflns_theta_max 35.03 _diffrn_reflns_theta_min 2.76 _diffrn_standards_decay_% 1 _diffrn_standards_interval_count 47 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 6.757 _exptl_absorpt_correction_T_max 0.584 _exptl_absorpt_correction_T_min 0.226 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 2.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 613.8 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 1.530 _refine_diff_density_min -2.571 _refine_ls_extinction_coef 0.080(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 109 _refine_ls_number_reflns 3208 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.091 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0335 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.5369P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0847 _refine_ls_wR_factor_ref 0.0805 _reflns_number_gt 2728 _reflns_number_total 3208 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wm2127.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/a' _cod_database_code 2214425 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' 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 Cu Cu 0.0000 0.0000 0.0000 0.01692(10) Uani d S 1 Cs Cs 0.11407(2) 0.354561(15) 0.35562(3) 0.02654(8) Uani d . 1 S S 0.37975(7) 0.14584(5) 0.73909(10) 0.01703(11) Uani d . 1 O O1 0.3992(3) 0.24027(18) 0.6156(4) 0.0273(4) Uani d . 1 O O2 0.5138(3) 0.0821(2) 0.7893(5) 0.0314(5) Uani d . 1 O O3 0.2560(2) 0.08353(19) 0.6000(3) 0.0250(4) Uani d . 1 O O4 0.3439(3) 0.1767(2) 0.9448(4) 0.0280(4) Uani d . 1 O OW1 0.1450(3) 0.1085(2) 0.1577(4) 0.0252(4) Uani d . 1 O OW2 -0.1908(3) 0.1109(2) 0.0139(4) 0.0297(5) Uani d . 1 O OW3 -0.0002(2) -0.06342(18) 0.2836(3) 0.0205(3) Uani d . 1 H H11 0.184(7) 0.093(5) 0.277(11) 0.050 Uiso d . 1 H H12 0.199(7) 0.122(5) 0.094(11) 0.050 Uiso d . 1 H H21 -0.281(7) 0.099(5) -0.063(10) 0.050 Uiso d . 1 H H22 -0.181(7) 0.166(5) -0.017(11) 0.050 Uiso d . 1 H H31 -0.071(7) -0.051(5) 0.310(11) 0.050 Uiso d . 1 H H32 0.034(7) -0.113(5) 0.308(10) 0.050 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 Cu 0.01750(19) 0.0183(2) 0.01490(17) -0.00407(15) 0.00436(13) 0.00055(14) Cs 0.02807(11) 0.02663(11) 0.02645(10) 0.00196(6) 0.01012(7) 0.00193(6) S 0.0157(2) 0.0182(2) 0.0169(2) -0.00196(19) 0.00399(18) 0.00030(19) O1 0.0344(11) 0.0214(9) 0.0283(10) -0.0026(8) 0.0124(9) 0.0051(8) O2 0.0188(9) 0.0314(12) 0.0407(12) 0.0036(8) 0.0031(8) 0.0038(10) O3 0.0203(8) 0.0315(11) 0.0219(8) -0.0090(8) 0.0039(7) -0.0048(8) O4 0.0334(11) 0.0330(11) 0.0197(8) -0.0064(9) 0.0112(8) -0.0049(8) OW1 0.0259(10) 0.0295(11) 0.0197(8) -0.0102(8) 0.0055(7) -0.0012(7) OW2 0.0231(10) 0.0280(11) 0.0390(12) 0.0030(9) 0.0101(9) 0.0051(10) OW3 0.0218(9) 0.0220(9) 0.0197(8) 0.0005(7) 0.0089(7) 0.0030(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O1- 0.0080 0.0060 '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' Cu Cu2+ 0.2630 1.2660 '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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 1 0 4 0 0 0 3 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 OW3 Cu OW3 . 3 180.00(17) ? OW3 Cu OW1 . . 90.34(9) ? OW3 Cu OW1 3 . 89.66(9) ? OW3 Cu OW1 . 3 89.66(9) ? OW3 Cu OW1 3 3 90.34(9) ? OW1 Cu OW1 . 3 180.00(16) ? OW3 Cu OW2 . 3 88.94(9) ? OW3 Cu OW2 3 3 91.06(9) ? OW1 Cu OW2 . 3 90.60(10) ? OW1 Cu OW2 3 3 89.40(10) ? OW3 Cu OW2 . . 91.06(9) ? OW3 Cu OW2 3 . 88.94(9) ? OW1 Cu OW2 . . 89.40(10) ? OW1 Cu OW2 3 . 90.60(10) ? OW2 Cu OW2 3 . 180.00(17) ? O1 Cs O4 . 4_564 140.29(7) ? O1 Cs O3 . 2_556 97.49(6) ? O4 Cs O3 4_564 2_556 113.63(6) ? O1 Cs O2 . 2_556 141.84(6) ? O4 Cs O2 4_564 2_556 73.76(6) ? O3 Cs O2 2_556 2_556 44.43(6) ? O1 Cs O1 . 4_565 97.59(5) ? O4 Cs O1 4_564 4_565 83.64(6) ? O3 Cs O1 2_556 4_565 126.51(6) ? O2 Cs O1 2_556 4_565 104.49(6) ? O1 Cs OW2 . 4_665 81.11(6) ? O4 Cs OW2 4_564 4_665 87.04(6) ? O3 Cs OW2 2_556 4_665 69.69(6) ? O2 Cs OW2 2_556 4_665 85.68(7) ? O1 Cs OW2 4_565 4_665 163.61(6) ? O1 Cs O2 . 4_565 94.88(6) ? O4 Cs O2 4_564 4_565 111.81(6) ? O3 Cs O2 2_556 4_565 83.77(6) ? O2 Cs O2 2_556 4_565 80.69(8) ? O1 Cs O2 4_565 4_565 43.99(6) ? OW2 Cs O2 4_665 4_565 152.24(6) ? O1 Cs OW1 . . 67.15(6) ? O4 Cs OW1 4_564 . 73.24(6) ? O3 Cs OW1 2_556 . 144.36(5) ? O2 Cs OW1 2_556 . 142.85(6) ? O1 Cs OW1 4_565 . 88.33(6) ? OW2 Cs OW1 4_665 . 76.06(6) ? O2 Cs OW1 4_565 . 127.78(6) ? O1 Cs O2 . 4_564 126.34(6) ? O4 Cs O2 4_564 4_564 42.23(6) ? O3 Cs O2 2_556 4_564 82.25(6) ? O2 Cs O2 2_556 4_564 61.70(8) ? O1 Cs O2 4_565 4_564 125.49(6) ? OW2 Cs O2 4_665 4_564 48.26(6) ? O2 Cs O2 4_565 4_564 137.77(8) ? OW1 Cs O2 . 4_564 82.32(6) ? O2 S O1 . . 109.96(15) y O2 S O3 . . 108.73(15) y O1 S O3 . . 108.61(14) y O2 S O4 . . 110.66(16) y O1 S O4 . . 109.77(14) y O3 S O4 . . 109.07(13) y S O1 Cs . . 116.54(12) ? S O1 Cs . 4_665 98.82(11) ? Cs O1 Cs . 4_665 119.34(7) ? S O2 Cs . 2_546 102.10(12) ? S O2 Cs . 4_665 96.71(12) ? Cs O2 Cs 2_546 4_665 99.31(8) ? S O2 Cs . 4_666 93.62(13) ? Cs O2 Cs 2_546 4_666 118.30(8) ? Cs O2 Cs 4_665 4_666 137.77(8) ? S O3 Cs . 2_546 102.83(11) ? S O4 Cs . 4_666 111.17(13) ? Cu OW1 Cs . . 134.36(11) ? Cu OW1 H11 . . 113(5) ? Cs OW1 H11 . . 87(5) ? Cu OW1 H12 . . 112(5) ? Cs OW1 H12 . . 97(5) ? H11 OW1 H12 . . 112(6) ? Cu OW2 Cs . 4_565 134.73(10) ? Cu OW2 H21 . . 122(4) ? Cs OW2 H21 4_565 . 75(4) ? Cu OW2 H22 . . 114(5) ? Cs OW2 H22 4_565 . 101(5) ? H21 OW2 H22 . . 101(6) ? Cu OW3 H31 . . 110(5) ? Cu OW3 H32 . . 117(5) ? H31 OW3 H32 . . 122(7) ? 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 Cu OW3 . 1.965(2) y Cu OW3 3 1.965(2) ? Cu OW1 . 2.005(2) y Cu OW1 3 2.005(2) ? Cu OW2 3 2.311(2) ? Cu OW2 . 2.311(2) y Cs O1 . 3.098(2) y Cs O4 4_564 3.114(2) y Cs O3 2_556 3.151(3) y Cs O2 2_556 3.179(3) y Cs O1 4_565 3.182(2) y Cs OW2 4_665 3.233(3) y Cs O2 4_565 3.239(3) y Cs OW1 . 3.422(3) y Cs O2 4_564 3.528(3) y Cs S 4_565 3.7066(7) ? Cs S 2_556 3.7677(7) ? Cs S 4_564 3.9035(8) ? Cs H11 . 3.47(6) ? S O2 . 1.463(2) y S O1 . 1.474(2) y S O3 . 1.482(2) y S O4 . 1.484(2) y S Cs 4_665 3.7066(7) ? S Cs 2_546 3.7677(7) ? S Cs 4_666 3.9035(8) ? O1 Cs 4_665 3.182(2) ? O2 Cs 2_546 3.179(3) ? O2 Cs 4_665 3.239(3) ? O2 Cs 4_666 3.528(3) ? O3 Cs 2_546 3.151(3) ? O4 Cs 4_666 3.114(2) ? OW1 H11 . 0.77(7) ? OW1 H12 . 0.76(7) ? OW2 Cs 4_565 3.233(3) ? OW2 H21 . 0.87(7) ? OW2 H22 . 0.74(6) ? OW3 H31 . 0.75(7) ? OW3 H32 . 0.70(7) ? 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 OW1 H11 O3 1_555 0.77(7) 1.97(7) 2.714(2) 166(7) y OW1 H12 O4 1_554 0.75(7) 1.99(7) 2.738(4) 173(7) y OW2 H21 O2 1_454 0.87(6) 1.91(7) 2.777(3) 174(7) y OW2 H22 O4 4_564 0.74(6) 2.04(6) 2.779(4) 171(6) y OW3 H31 O3 3_556 0.74(7) 2.02(7) 2.725(3) 155(7) y OW3 H32 O1 2_546 0.71(7) 1.99(6) 2.693(3) 171(6) y