#------------------------------------------------------------------------------ #$Date: 2008-04-03 13:11:48 +0300 (Thu, 03 Apr 2008) $ #$Revision: 326 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2217426.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_2217426 loop_ _publ_author_name 'Cunha-Silva, Luis' 'Brand\~ao, Paula' 'Rocha, Jo\~ao' 'Almeida Paz, Filipe A.' _publ_section_title ; The dehydrated copper silicate Na~2~[Cu~2~Si~4~O~11~]: a three-dimensional microporous framework with a linear Si--O--Si linkage ; _journal_coeditor_code BR2065 _journal_issue 2 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i13 _journal_page_last i14 _journal_volume 64 _journal_year 2008 _chemical_formula_iupac 'Na2 (Cu2 O11 Si4)' _chemical_formula_moiety '2(Na +), Cu2 O11 Si4 2-' _chemical_formula_structural 'Na2 Cu2 (Si4 O11)' _chemical_formula_sum 'Cu2 Na2 O11 Si4' _chemical_formula_weight 461.44 _chemical_name_systematic ; disodium dicopper undecaoxide tetrasilicate ; _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'SHELXTL, manual editing plus enCIFer' _cell_angle_alpha 96.390(7) _cell_angle_beta 97.281(7) _cell_angle_gamma 100.461(7) _cell_formula_units_Z 1 _cell_length_a 5.190(2) _cell_length_b 6.299(3) _cell_length_c 8.196(4) _cell_measurement_reflns_used 758 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 58.11 _cell_measurement_theta_min 8.09 _cell_volume 258.9(2) _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT-Plus (Bruker, 2003)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2007)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker SMART CCD 1000' _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 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1587 _diffrn_reflns_theta_full 26.35 _diffrn_reflns_theta_max 26.35 _diffrn_reflns_theta_min 3.89 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.709 _exptl_absorpt_correction_T_max 0.8340 _exptl_absorpt_correction_T_min 0.6274 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (TWINABS; Sheldrick, 2002) ; _exptl_crystal_colour Black _exptl_crystal_density_diffrn 2.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 224 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.397 _refine_diff_density_min -1.579 _refine_ls_extinction_coef no _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_matrix_type full _refine_ls_number_parameters 88 _refine_ls_number_reflns 1043 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0421 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0809P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1116 _refine_ls_wR_factor_ref 0.1190 _reflns_number_gt 782 _reflns_number_total 1043 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file br2065.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 Cu Cu1 0.70666(10) -0.10891(9) 0.93472(8) 0.0096(3) Uani d . 1 Na Na1 0.8700(4) 0.3540(3) 1.1990(3) 0.0235(6) Uani d . 1 Si Si1 1.0175(2) 0.1358(2) 0.67930(18) 0.0087(4) Uani d . 1 Si Si2 0.5954(3) 0.3456(2) 0.80969(18) 0.0089(4) Uani d . 1 O O1 1.0000 0.0000 0.5000 0.0217(13) Uani d S 1 O O2 1.0064(7) -0.0190(6) 0.8196(5) 0.0127(8) Uani d . 1 O O3 0.7804(6) 0.2736(6) 0.6719(5) 0.0126(8) Uani d . 1 O O4 0.2923(6) 0.3209(5) 0.7137(5) 0.0144(8) Uani d . 1 O O5 0.7200(7) 0.5899(6) 0.8873(5) 0.0170(9) Uani d . 1 O O6 0.5974(6) 0.1760(5) 0.9452(5) 0.0107(8) 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 Cu1 0.0054(4) 0.0083(4) 0.0159(4) 0.0011(2) 0.0051(2) 0.0018(2) Na1 0.0137(11) 0.0161(12) 0.0396(16) 0.0021(9) 0.0072(10) -0.0030(10) Si1 0.0048(7) 0.0096(7) 0.0124(8) 0.0018(5) 0.0034(5) 0.0009(5) Si2 0.0040(6) 0.0078(7) 0.0155(8) 0.0013(5) 0.0042(5) 0.0018(5) O1 0.020(3) 0.024(3) 0.021(3) 0.006(2) 0.007(2) -0.006(2) O2 0.0078(17) 0.0137(18) 0.018(2) 0.0033(13) 0.0040(14) 0.0045(14) O3 0.0057(16) 0.0169(19) 0.018(2) 0.0068(14) 0.0049(14) 0.0018(14) O4 0.0063(16) 0.0140(18) 0.023(2) 0.0017(14) 0.0014(14) 0.0061(15) O5 0.0145(18) 0.0100(18) 0.028(2) 0.0000(14) 0.0129(16) 0.0016(15) O6 0.0082(16) 0.0111(17) 0.016(2) 0.0039(13) 0.0061(14) 0.0050(14) 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 Cu1 O5 1_545 1.909(3) yes Cu1 O2 . 1.950(4) yes Cu1 O6 2_657 1.970(4) yes Cu1 O6 . 1.974(3) yes Cu1 O2 2_757 2.316(4) yes Cu1 Cu1 2_657 2.9921(13) no Cu1 Cu1 2_757 3.1031(15) no Cu1 Si2 2_657 3.1221(19) no Cu1 Si1 . 3.1673(19) no Si1 O2 . 1.588(4) no Si1 O1 . 1.5991(14) no Si1 O3 . 1.629(3) no Si1 O4 1_655 1.642(4) no Si2 O5 . 1.583(4) no Si2 O6 . 1.625(4) no Si2 O4 . 1.639(3) no Si2 O3 . 1.650(4) no Si2 Cu1 2_657 3.1221(19) no O1 Si1 2_756 1.5991(14) no O2 Cu1 2_757 2.316(4) no O4 Si1 1_455 1.642(4) no O5 Cu1 1_565 1.909(3) no O6 Cu1 2_657 1.970(4) no 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 Cu1 O2 1_545 . 92.49(15) no O5 Cu1 O6 1_545 2_657 91.91(15) no O2 Cu1 O6 . 2_657 175.60(13) no O5 Cu1 O6 1_545 . 164.27(15) no O2 Cu1 O6 . . 94.42(14) no O6 Cu1 O6 2_657 . 81.32(16) no O5 Cu1 O2 1_545 2_757 105.60(16) no O2 Cu1 O2 . 2_757 87.05(15) no O6 Cu1 O2 2_657 2_757 91.76(14) no O6 Cu1 O2 . 2_757 88.87(14) no O5 Cu1 Cu1 1_545 2_657 131.06(12) no O2 Cu1 Cu1 . 2_657 135.03(10) no O6 Cu1 Cu1 2_657 2_657 40.70(10) no O6 Cu1 Cu1 . 2_657 40.62(10) no O2 Cu1 Cu1 2_757 2_657 90.41(9) no O5 Cu1 Cu1 1_545 2_757 103.18(12) no O2 Cu1 Cu1 . 2_757 48.19(11) no O6 Cu1 Cu1 2_657 2_757 130.50(11) no O6 Cu1 Cu1 . 2_757 91.93(10) no O2 Cu1 Cu1 2_757 2_757 38.86(9) no Cu1 Cu1 Cu1 2_657 2_757 116.74(4) no O5 Cu1 Si2 1_545 2_657 73.75(12) no O2 Cu1 Si2 . 2_657 156.11(11) no O6 Cu1 Si2 2_657 2_657 26.72(10) no O6 Cu1 Si2 . 2_657 103.96(11) no O2 Cu1 Si2 2_757 2_657 78.31(10) no Cu1 Cu1 Si2 2_657 2_657 64.59(4) no Cu1 Cu1 Si2 2_757 2_657 115.04(5) no O5 Cu1 Si1 1_545 . 106.73(13) no O2 Cu1 Si1 . . 23.68(11) no O6 Cu1 Si1 2_657 . 153.39(10) no O6 Cu1 Si1 . . 75.74(11) no O2 Cu1 Si1 2_757 . 100.98(10) no Cu1 Cu1 Si1 2_657 . 115.23(4) no Cu1 Cu1 Si1 2_757 . 64.33(4) no Si2 Cu1 Si1 2_657 . 179.25(4) no O2 Si1 O1 . . 111.33(15) no O2 Si1 O3 . . 112.6(2) no O1 Si1 O3 . . 108.16(15) no O2 Si1 O4 . 1_655 111.48(19) no O1 Si1 O4 . 1_655 108.08(16) no O3 Si1 O4 . 1_655 104.92(18) no O1 Si1 Cu1 . . 115.96(7) no O3 Si1 Cu1 . . 84.08(15) no O4 Si1 Cu1 1_655 . 129.55(15) no O5 Si2 O6 . . 113.2(2) no O5 Si2 O4 . . 111.75(19) no O6 Si2 O4 . . 109.3(2) no O5 Si2 O3 . . 107.1(2) no O6 Si2 O3 . . 107.00(19) no O4 Si2 O3 . . 108.15(19) no O5 Si2 Cu1 . 2_657 109.62(16) no O4 Si2 Cu1 . 2_657 81.61(15) no O3 Si2 Cu1 . 2_657 134.72(14) no Si1 O1 Si1 2_756 . 180.0 no Si1 O2 Cu1 . . 126.8(2) no Si1 O2 Cu1 . 2_757 116.29(18) no Cu1 O2 Cu1 . 2_757 92.95(15) no Si1 O3 Si2 . . 132.7(3) no Si2 O4 Si1 . 1_455 137.0(2) no Si2 O5 Cu1 . 1_565 152.9(2) no Si2 O6 Cu1 . 2_657 120.24(18) no Si2 O6 Cu1 . . 130.3(2) no Cu1 O6 Cu1 2_657 . 98.68(16) no