#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2005340.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_2005340 loop_ _publ_author_name 'Chevrier, G.' 'Goukassov, A.' _publ_section_title ; The Hydrogen-Bonding System in Deuterated Copper Fluorosilicate Tetrahydrate: a Neutron Diffraction Study ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2121 _journal_page_last 2123 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac 'Cu Si F6 , 4D2 O' _chemical_formula_moiety 'Cu F6 Si , 4D2 O ' _chemical_formula_sum 'Cu D8 F6 O4 Si' _chemical_formula_weight 285.7 _chemical_name_systematic ' Deuterated copper flurosilicate tetrahydrate' _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 90.00000 _cell_angle_beta 105.160(10) _cell_angle_gamma 90.00000 _cell_formula_units_Z 2 _cell_length_a 5.33(2) _cell_length_b 9.60(5) _cell_length_c 7.18(5) _cell_measurement_reflns_used 17 _cell_measurement_temperature 296 _cell_measurement_theta_max 36.5 _cell_measurement_theta_min 12.5 _cell_volume 355(3) _diffrn_measurement_device '4-circle 6T2 at Orphee reactor' _diffrn_measurement_method ; unique set between 45 and 120\%. \w scans between 2\q = 2 and 45\%, \w--\q scans between 2\q = 45 and 60\% and \w--2\q scans between 2\q = 60 and 120\% ; _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.520(2) _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 2 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 759 _diffrn_reflns_theta_max 60.0 _diffrn_standards_decay_% <0.5 _diffrn_standards_interval_time 120 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.0683(estimated) _exptl_absorpt_correction_type none _exptl_crystal_colour blue _exptl_crystal_density_diffrn 2.679 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 10.891 _exptl_crystal_size_max 4.00 _exptl_crystal_size_mid 3.50 _exptl_crystal_size_min 3.00 _refine_diff_density_max '0.65 fm \%A^-3^' _refine_diff_density_min '-0.75 fm \%A^-3^' _refine_ls_extinction_coef ' G~eq~ = 0.113(5)' _refine_ls_extinction_method ' type 2 anisotropic extinction (Coppens & Hamilton, 1970)' _refine_ls_goodness_of_fit_obs 5.713 _refine_ls_hydrogen_treatment 'D-atoms refined' _refine_ls_number_parameters 101 _refine_ls_number_reflns 433 _refine_ls_R_factor_obs 0.0647 _refine_ls_shift/esd_max 0.00007 _refine_ls_structure_factor_coef F^2^ _refine_ls_weighting_scheme 'w = 1/\s^2^(F^2^)' _refine_ls_wR_factor_obs 0.0465 _reflns_number_observed 433 _reflns_number_total 571 _reflns_observed_criterion F^2^>2.5\s(F^2^) _[local]_cod_data_source_file br1141.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _[local]_cod_chemical_formula_sum_orig 'Cu D8 F6 Si O4' _cod_original_cell_volume 354.(8) _cod_database_code 2005340 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,1/2+y,1/2-z x,1/2-y,1/2+z 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 _atom_site_aniso_type_symbol Cu .020(2) .017(2) .020(2) .0003(17) .0134(17) .0013(16) Cu Si .004(3) .011(3) .010(3) -.001(3) .003(2) -.000(3) Si F1 .029(2) .022(2) .037(3) -.0100(19) .018(2) .0025(18) F F2 .037(3) .023(2) .024(2) -.0002(18) .0193(19) -.0053(18) F F3 .030(3) .038(3) .021(3) .0033(17) .0008(18) .0012(17) F O1 .028(3) .022(3) .030(3) -.005(2) .013(2) .002(2) O O2 .024(2) .029(3) .023(3) .008(2) .0145(19) -.002(2) O D11 .043(4) .035(3) .040(4) -.004(3) .029(3) -.003(3) D D12 .051(4) .036(4) .043(5) -.021(3) .023(3) -.012(3) D D21 .050(3) .034(3) .034(4) .013(3) .027(3) -.000(3) D D22 .042(3) .020(3) .042(4) .012(3) .018(3) .007(3) D 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_type_symbol Cu 0.0000 0.0000 0.0000 0.0176(9) Uani Cu Si 0.5000 0.0000 0.5000 0.0083(13) Uani Si F1 0.7311(7) 0.1050(4) 0.4529(6) 0.0274(11) Uani F F2 0.3893(8) 0.1334(4) 0.6110(5) 0.0255(10) Uani F F3 0.2981(7) 0.0471(4) 0.2921(5) 0.0305(11) Uani F O1 0.1260(8) 0.1582(5) -0.1203(7) 0.0257(12) Uani O O2 -0.2393(7) 0.1269(5) 0.0790(7) 0.0236(12) Uani O D11 0.2204(10) 0.1406(5) -0.2153(8) 0.0361(15) Uani D D12 0.2198(11) 0.2301(6) -0.0398(8) 0.0414(17) Uani D D21 -0.2500(10) 0.1226(5) 0.2092(10) 0.0364(15) Uani D D22 -0.2427(10) 0.2232(5) 0.0437(7) 0.0336(16) Uani D loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0.7689 0.0000 ' Delapalme (1985)' Si 0.4150 0.0000 ' Delapalme (1985)' F 0.5650 0.0000 ' Delapalme (1985)' D 0.6670 0.0000 ' Delapalme (1985)' O 0.5805 0.0000 ' Delapalme (1985)' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu O1 1_555 180.0 no O2 Cu O2 1_555 180.0 no F3 Cu F3 1_555 180.0 no O1 Cu O2 1_555 88.3(5) yes O1 Cu O2 2_555 91.7(7) yes O1 Cu F3 1_555 90.8(8) yes O1 Cu F3 2_555 89.2(6) yes O2 Cu F3 1_555 87.8(6) yes O2 Cu F3 2_555 92.2(8) yes F1 Si F1 1_555 180.0 no F2 Si F2 1_555 180.0 no F3 Si F3 1_555 180.0 no F1 Si F2 1_555 90.3(6) yes F1 Si F2 2_656 89.7(7) yes F1 Si F3 1_555 89.6(6) yes F1 Si F3 2_656 90.4(7) yes F2 Si F3 1_555 89.6(8) yes F2 Si F3 2_656 90.4(6) yes D11 O1 D12 1_555 105.5(13) yes D21 O2 D22 1_555 107.4(15) yes Cu O1 D11 1_555 118.8(12) no Cu O1 D12 1_555 118.8(13) no Cu O2 D21 1_555 118.0(12) no Cu O2 D22 1_555 119.6(13) no Cu F3 Si 1_555 153(4) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu O1 1_555 1_555 1.951(8) yes Cu O2 1_555 1_555 1.952(7) yes Cu F3 1_555 1_555 2.320(13) yes O1 O2 1_555 1_555 2.718(11) no O1 O2 1_555 2_555 2.800(15) no O1 F3 1_555 1_555 3.05(2) no O2 F3 1_555 1_555 2.974(12) no O1 F3 1_555 2_555 3.009(11) no O2 F3 1_555 2_555 3.089(17) no Si F1 1_555 1_555 1.693(6) yes Si F2 1_555 1_555 1.693(7) yes Si F3 1_555 1_555 1.658(10) yes F1 F2 1_555 1_555 2.401(9) no F1 F2 1_555 2_656 2.388(12) no F1 F3 1_555 1_555 2.361(10) no F2 F3 1_555 1_555 2.362(15) no F1 F3 1_555 2_656 2.378(12) no F2 F3 1_555 2_656 2.378(9) no O1 D11 1_555 1_555 0.962(8) yes O1 D12 1_555 1_555 0.953(8) yes O1 D22 1_555 1_555 2.617(10) no O2 D21 1_555 1_555 0.952(10) yes O2 D22 1_555 1_555 0.957(8) yes O2 D12 1_555 1_555 2.965(12) no