#------------------------------------------------------------------------------ #$Date: 2008-04-05 11:13:02 +0300 (Sat, 05 Apr 2008) $ #$Revision: 340 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2102815.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_2102815 loop_ _publ_author_name 'Weller, Mark T.' 'Henry, Paul F.' 'Light, Mark E.' _publ_section_title ; Rapid structure determination of the hydrogen-containing compound Cs~2~C~2~O~4~·H~2~O by joint single-crystal X-ray and powder neutron diffraction ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 426 _journal_page_last 432 _journal_volume 63 _journal_year 2007 _chemical_formula_sum 'C2 H2 Cs2 O5' _chemical_formula_weight 371.86 _chemical_name_systematic ; ? ; _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _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 107.189(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.0748(5) _cell_length_b 6.6473(3) _cell_length_c 11.2997(6) _cell_measurement_reflns_used 869 _cell_measurement_temperature 289(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.02 _cell_volume 722.94(6) _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 289(2) _diffrn_detector_area_resol_mean 9.091 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4032 _diffrn_reflns_theta_full 27.31 _diffrn_reflns_theta_max 27.31 _diffrn_reflns_theta_min 3.73 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 10.040 _exptl_absorpt_correction_T_max 0.5005 _exptl_absorpt_correction_T_min 0.2060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 3.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 656 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.956 _refine_diff_density_min -0.904 _refine_ls_extinction_coef 0.0034(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 47 _refine_ls_number_reflns 809 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.168 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0249 _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^)+(0.0142P)^2^+1.8270P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.0536 _reflns_number_gt 700 _reflns_number_total 809 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file bk5052.cif 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_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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cs Cs1 0.87244(3) 0.30550(4) 0.37345(2) 0.02732(16) Uani d . 1 O O1 0.6398(3) 0.2709(6) 0.0934(3) 0.0335(8) Uani d . 1 O O2 0.8242(3) 0.4550(5) 0.0942(3) 0.0303(7) Uani d . 1 O O3 1.0000 -0.0535(9) 0.2500 0.074(2) Uani d S 1 H H1 0.968(6) -0.128(9) 0.291(5) 0.050(18) Uiso d . 1 C C1 0.7393(5) 0.3148(6) 0.0543(4) 0.0224(9) Uani 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 Cs1 0.02621(19) 0.0275(2) 0.0283(2) -0.00157(11) 0.00824(13) -0.00304(12) O1 0.0317(18) 0.0366(18) 0.037(2) -0.0071(15) 0.0183(16) -0.0071(16) O2 0.0331(16) 0.0273(16) 0.0308(17) -0.0049(14) 0.0102(14) -0.0048(13) O3 0.124(6) 0.029(3) 0.110(6) 0.000 0.095(5) 0.000 C1 0.024(2) 0.021(2) 0.022(2) 0.0055(16) 0.0067(18) 0.0041(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Cs1 O2 6_566 3.116(3) Cs1 O1 8_556 3.120(3) Cs1 O1 4_655 3.123(4) Cs1 O2 2_755 3.131(3) Cs1 O2 4_645 3.149(3) Cs1 O2 . 3.205(3) Cs1 O3 . 3.217(4) Cs1 O1 . 3.343(3) Cs1 C1 . 3.456(4) Cs1 O1 4_645 3.579(4) Cs1 C1 4_645 3.622(4) Cs1 O3 3_455 3.7162(15) Cs1 H1 . 3.26(6) O1 C1 . 1.244(6) O1 Cs1 8_455 3.120(3) O1 Cs1 4_645 3.123(4) O1 Cs1 4_655 3.579(4) O2 C1 . 1.256(5) O2 Cs1 6_565 3.116(3) O2 Cs1 2_755 3.131(3) O2 Cs1 4_655 3.149(3) O3 Cs1 2_755 3.217(4) O3 Cs1 3_545 3.7162(15) O3 Cs1 4_645 3.7162(15) O3 H1 . 0.81(6) C1 C1 7_655 1.566(9) C1 Cs1 4_655 3.622(4) C1 Cs1 4_645 3.733(4) C1 Cs1 6_565 3.738(4) C1 Cs1 8_455 3.743(4) C1 Cs1 2_755 3.753(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 O2 Cs1 O1 6_566 8_556 75.37(9) O2 Cs1 O1 6_566 4_655 51.46(9) O1 Cs1 O1 8_556 4_655 96.95(8) O2 Cs1 O2 6_566 2_755 97.01(7) O1 Cs1 O2 8_556 2_755 51.36(8) O1 Cs1 O2 4_655 2_755 75.12(8) O2 Cs1 O2 6_566 4_645 91.88(8) O1 Cs1 O2 8_556 4_645 102.23(9) O1 Cs1 O2 4_655 4_645 132.11(8) O2 Cs1 O2 2_755 4_645 147.93(11) O2 Cs1 O2 6_566 . 127.99(4) O1 Cs1 O2 8_556 . 132.74(9) O1 Cs1 O2 4_655 . 79.10(8) O2 Cs1 O2 2_755 . 82.83(9) O2 Cs1 O2 4_645 . 115.23(6) O2 Cs1 O3 6_566 . 154.52(7) O1 Cs1 O3 8_556 . 82.14(7) O1 Cs1 O3 4_655 . 145.25(10) O2 Cs1 O3 2_755 . 77.58(8) O2 Cs1 O3 4_645 . 81.21(9) O2 Cs1 O3 . . 76.53(7) O2 Cs1 O1 6_566 . 124.15(8) O1 Cs1 O1 8_556 . 160.33(9) O1 Cs1 O1 4_655 . 98.06(8) O2 Cs1 O1 2_755 . 121.30(8) O2 Cs1 O1 4_645 . 76.69(8) O2 Cs1 O1 . . 39.62(8) O3 Cs1 O1 . . 78.27(6) O2 Cs1 C1 6_566 . 136.21(9) O1 Cs1 C1 8_556 . 144.25(10) O1 Cs1 C1 4_655 . 95.19(9) O2 Cs1 C1 2_755 . 100.40(9) O2 Cs1 C1 4_645 . 94.06(9) O2 Cs1 C1 . . 21.30(8) O3 Cs1 C1 . . 69.05(7) O1 Cs1 C1 . . 20.99(9) O2 Cs1 O1 6_566 4_645 113.90(8) O1 Cs1 O1 8_556 4_645 78.66(10) O1 Cs1 O1 4_655 4_645 165.28(13) O2 Cs1 O1 2_755 4_645 111.45(8) O2 Cs1 O1 4_645 4_645 37.91(8) O2 Cs1 O1 . 4_645 114.27(8) O3 Cs1 O1 . 4_645 48.66(9) O1 Cs1 O1 . 4_645 89.69(9) C1 Cs1 O1 . 4_645 96.43(9) O2 Cs1 C1 6_566 4_645 98.47(9) O1 Cs1 C1 8_556 4_645 85.79(10) O1 Cs1 C1 4_655 4_645 147.07(10) O2 Cs1 C1 2_755 4_645 128.12(9) O2 Cs1 C1 4_645 4_645 19.83(9) O2 Cs1 C1 . 4_645 122.30(9) O3 Cs1 C1 . 4_645 67.68(10) O1 Cs1 C1 . 4_645 88.49(9) C1 Cs1 C1 . 4_645 101.56(10) O1 Cs1 C1 4_645 4_645 19.88(9) O2 Cs1 O3 6_566 3_455 78.03(7) O1 Cs1 O3 8_556 3_455 151.44(7) O1 Cs1 O3 4_655 3_455 73.97(10) O2 Cs1 O3 2_755 3_455 143.73(10) O2 Cs1 O3 4_645 3_455 68.28(10) O2 Cs1 O3 . 3_455 73.13(6) O3 Cs1 O3 . 3_455 120.85(8) O1 Cs1 O3 . 3_455 46.71(7) C1 Cs1 O3 . 3_455 64.31(7) O1 Cs1 O3 4_645 3_455 103.15(10) C1 Cs1 O3 4_645 3_455 88.01(11) O2 Cs1 H1 6_566 . 144.0(10) O1 Cs1 H1 8_556 . 79.9(11) O1 Cs1 H1 4_655 . 159.2(10) O2 Cs1 H1 2_755 . 87.3(10) O2 Cs1 H1 4_645 . 68.2(10) O2 Cs1 H1 . . 88.0(10) O3 Cs1 H1 . . 14.3(10) O1 Cs1 H1 . . 81.6(11) C1 Cs1 H1 . . 77.0(10) O1 Cs1 H1 4_645 . 34.4(10) C1 Cs1 H1 4_645 . 53.6(10) O3 Cs1 H1 3_455 . 117.9(11) C1 O1 Cs1 . 8_455 110.6(3) C1 O1 Cs1 . 4_645 109.8(3) Cs1 O1 Cs1 8_455 4_645 83.05(8) C1 O1 Cs1 . . 84.7(3) Cs1 O1 Cs1 8_455 . 164.58(13) Cs1 O1 Cs1 4_645 . 89.78(9) C1 O1 Cs1 . 4_655 82.0(2) Cs1 O1 Cs1 8_455 4_655 101.34(10) Cs1 O1 Cs1 4_645 4_655 165.28(13) Cs1 O1 Cs1 . 4_655 82.46(7) C1 O2 Cs1 . 6_565 110.1(3) C1 O2 Cs1 . 2_755 110.1(2) Cs1 O2 Cs1 6_565 2_755 82.99(7) C1 O2 Cs1 . 4_655 101.9(2) Cs1 O2 Cs1 6_565 4_655 88.12(8) Cs1 O2 Cs1 2_755 4_655 147.93(11) C1 O2 Cs1 . . 90.7(2) Cs1 O2 Cs1 6_565 . 158.81(11) Cs1 O2 Cs1 2_755 . 85.87(7) Cs1 O2 Cs1 4_655 . 91.88(8) Cs1 O3 Cs1 2_755 . 84.25(14) Cs1 O3 Cs1 2_755 3_545 82.04(3) Cs1 O3 Cs1 . 3_545 120.85(8) Cs1 O3 Cs1 2_755 4_645 120.85(8) Cs1 O3 Cs1 . 4_645 82.04(3) Cs1 O3 Cs1 3_545 4_645 150.78(18) Cs1 O3 H1 2_755 . 169(4) Cs1 O3 H1 . . 86(4) Cs1 O3 H1 3_545 . 99(4) Cs1 O3 H1 4_645 . 62(4) O1 C1 O2 . . 125.6(4) O1 C1 C1 . 7_655 117.5(5) O2 C1 C1 . 7_655 116.9(5) O1 C1 Cs1 . . 74.4(3) O2 C1 Cs1 . . 68.0(2) C1 C1 Cs1 7_655 . 135.0(3) O1 C1 Cs1 . 4_655 78.1(2) O2 C1 Cs1 . 4_655 58.3(2) C1 C1 Cs1 7_655 4_655 142.7(3) Cs1 C1 Cs1 . 4_655 80.30(9) O1 C1 Cs1 . 4_645 51.9(2) O2 C1 Cs1 . 4_645 144.3(3) C1 C1 Cs1 7_655 4_645 78.1(3) Cs1 C1 Cs1 . 4_645 78.75(8) Cs1 C1 Cs1 4_655 4_645 129.32(13) O1 C1 Cs1 . 6_565 144.1(3) O2 C1 Cs1 . 6_565 51.6(2) C1 C1 Cs1 7_655 6_565 77.7(3) Cs1 C1 Cs1 . 6_565 119.42(12) Cs1 C1 Cs1 4_655 6_565 72.58(7) Cs1 C1 Cs1 4_645 6_565 155.80(13) O1 C1 Cs1 . 8_455 51.3(2) O2 C1 Cs1 . 8_455 144.4(3) C1 C1 Cs1 7_655 8_455 78.3(3) Cs1 C1 Cs1 . 8_455 125.59(13) Cs1 C1 Cs1 4_655 8_455 89.59(9) Cs1 C1 Cs1 4_645 8_455 67.22(7) Cs1 C1 Cs1 6_565 8_455 107.56(10) O1 C1 Cs1 . 2_755 144.8(3) O2 C1 Cs1 . 2_755 51.6(2) C1 C1 Cs1 7_655 2_755 77.6(3) Cs1 C1 Cs1 . 2_755 73.42(8) Cs1 C1 Cs1 4_655 2_755 109.83(11) Cs1 C1 Cs1 4_645 2_755 107.45(10) Cs1 C1 Cs1 6_565 2_755 67.08(7) Cs1 C1 Cs1 8_455 2_755 155.89(13) 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 H1 O1 4_645 0.81(6) 2.05(5) 2.819(4) 161(6)