# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'RSC Advances' _journal_coden_Cambridge 1500 _publ_contact_author_name 'Breu, Josef' _publ_contact_author_email josef.breu@uni-bayreuth.de _publ_section_title ; Single Crystal Structure Refinement of One- and Two-layer Hydrate of Sodium-Fluorohectorite ; loop_ _publ_author_name H.Kalo W.Milius J.Breu # Attachment '- 1WL.CIF' data_h-1wlc _database_code_depnum_ccdc_archive 'CCDC 869127' #TrackingRef '- 1WL.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'hydrate sodium fluorohectorite' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'F2 Li0.70 Mg2.15 Na0.70 O12 Si4' _chemical_formula_weight 415.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 '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' F F 0.0171 0.0103 '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' Mg Mg 0.0486 0.0363 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 5.2434(10) _cell_length_b 9.0891(18) _cell_length_c 12.165(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.92(3) _cell_angle_gamma 90.00 _cell_volume 578.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1409 _cell_measurement_theta_min 3.36 _cell_measurement_theta_max 25.90 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 411 _exptl_absorpt_coefficient_mu 0.751 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 1' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2006 _diffrn_reflns_av_R_equivalents 0.1808 _diffrn_reflns_av_sigmaI/netI 0.1391 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 25.90 _reflns_number_total 597 _reflns_number_gt 384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS 1' _computing_cell_refinement 'STOE CELL' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 597 _refine_ls_number_parameters 61 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1444 _refine_ls_R_factor_gt 0.1085 _refine_ls_wR_factor_ref 0.3184 _refine_ls_wR_factor_gt 0.2881 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.20395(14) 0.16672(8) 0.22352(7) 0.0263(2) Uani 1 1 d . . . Mg1 Mg 0.0000 0.33409(18) 0.0000 0.0282(5) Uani 0.725(3) 2 d SP . . Li1 Li 0.0000 0.33409(18) 0.0000 0.0282(5) Uani 0.275(3) 2 d SP . . Mg2 Mg 0.0000 0.0000 0.0000 0.0273(6) Uani 0.744(3) 4 d SP . . Li2 Li 0.0000 0.0000 0.0000 0.0273(6) Uani 0.256(3) 4 d SP . . F F 0.1826(4) 0.5000 0.08441(18) 0.0284(6) Uani 1 2 d S . . O1 O 0.1825(3) 0.16751(19) 0.09304(15) 0.0243(5) Uani 1 1 d . . . O3 O 0.2085(5) 0.0000 0.2769(2) 0.0222(7) Uani 1 2 d S . . O2 O -0.0353(3) 0.2511(2) 0.27784(15) 0.0261(5) Uani 1 1 d . . . Na Na -0.2633(12) 0.0000 0.4328(6) 0.077(3) Uani 0.35 2 d SPD . . OW2 O -0.5000 -0.2102(9) 0.5000 0.57(4) Uiso 0.80 2 d SPD . . OW3 O 0.2096 0.0000 0.5000 0.250 Uiso 0.25 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0186(3) 0.0229(3) 0.0376(4) 0.0003(3) 0.0034(3) -0.0009(3) Mg1 0.0182(7) 0.0244(8) 0.0421(9) 0.000 0.0032(7) 0.000 Li1 0.0182(7) 0.0244(8) 0.0421(9) 0.000 0.0032(7) 0.000 Mg2 0.0166(9) 0.0207(10) 0.0445(12) 0.000 0.0016(9) 0.000 Li2 0.0166(9) 0.0207(10) 0.0445(12) 0.000 0.0016(9) 0.000 F 0.0236(10) 0.0301(11) 0.0323(11) 0.000 0.0079(9) 0.000 O1 0.0195(8) 0.0188(9) 0.0344(9) -0.0017(8) 0.0011(8) -0.0008(6) O3 0.0228(11) 0.0147(11) 0.0291(12) 0.000 0.0008(10) 0.000 O2 0.0210(8) 0.0259(9) 0.0314(9) -0.0002(9) 0.0030(7) 0.0027(7) Na 0.051(3) 0.094(5) 0.088(5) 0.000 0.021(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si O1 1.584(2) . ? Si O3 1.6483(12) . ? Si O2 1.647(2) . ? Si O2 1.6553(19) 8 ? Si Mg1 3.2217(12) 7 ? Si Mg2 3.2305(10) . ? Si Mg1 3.2333(13) . ? Mg1 F 2.0276(19) . ? Mg1 F 2.0276(19) 5_565 ? Mg1 O1 2.076(2) 8_455 ? Mg1 O1 2.076(2) 7 ? Mg1 O1 2.084(2) 2 ? Mg1 O1 2.084(2) . ? Mg1 Li1 3.016(3) 5_565 ? Mg1 Mg1 3.016(3) 5_565 ? Mg1 Li2 3.0245(9) 3 ? Mg1 Mg2 3.0245(9) 3 ? Mg1 Li2 3.0245(9) 3_455 ? Mg1 Mg2 3.0245(9) 3_455 ? Mg2 F 2.014(2) 3_445 ? Mg2 F 2.014(2) 7 ? Mg2 O1 2.0898(18) . ? Mg2 O1 2.0898(18) 5 ? Mg2 O1 2.0898(18) 2 ? Mg2 O1 2.0898(18) 6 ? Mg2 Li1 3.0245(9) 7 ? Mg2 Mg1 3.0245(9) 7 ? Mg2 Li1 3.0245(9) 3_445 ? Mg2 Mg1 3.0245(9) 3_445 ? Mg2 Li1 3.0245(9) 7_455 ? Mg2 Mg1 3.0245(9) 7_455 ? F Li2 2.014(2) 3 ? F Mg2 2.014(2) 3 ? F Mg1 2.0276(19) 5_565 ? F Li1 2.0276(19) 5_565 ? O1 Li1 2.076(2) 7 ? O1 Mg1 2.076(2) 7 ? O3 Si 1.6483(12) 6 ? O2 Si 1.6553(19) 8_455 ? Na OW3 0.846(7) 5_556 ? Na OW2 3.059(8) 3 ? Na OW2 3.059(8) 7_446 ? Na OW3 2.558(6) . ? Na OW3 2.935(7) 1_455 ? Na Na 3.064(14) 5_456 ? Na Na 3.112(13) 5_556 ? OW2 Na 3.059(8) 3_445 ? OW2 Na 3.059(8) 7_446 ? OW3 Na 0.846(7) 5_556 ? OW3 Na 2.935(7) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si O3 113.42(11) . . ? O1 Si O2 113.34(10) . . ? O3 Si O2 105.12(12) . . ? O1 Si O2 113.46(10) . 8 ? O3 Si O2 105.56(11) . 8 ? O2 Si O2 105.11(8) . 8 ? O1 Si Mg1 32.79(7) . 7 ? O3 Si Mg1 109.62(9) . 7 ? O2 Si Mg1 139.81(8) . 7 ? O2 Si Mg1 84.58(7) 8 7 ? O1 Si Mg2 33.04(7) . . ? O3 Si Mg2 84.01(8) . . ? O2 Si Mg2 109.79(7) . . ? O2 Si Mg2 139.87(8) 8 . ? Mg1 Si Mg2 55.91(2) 7 . ? O1 Si Mg1 32.67(7) . . ? O3 Si Mg1 139.38(9) . . ? O2 Si Mg1 84.32(7) . . ? O2 Si Mg1 109.88(8) 8 . ? Mg1 Si Mg1 56.09(3) 7 . ? Mg2 Si Mg1 56.04(3) . . ? F Mg1 F 83.90(11) . 5_565 ? F Mg1 O1 95.60(9) . 8_455 ? F Mg1 O1 85.00(8) 5_565 8_455 ? F Mg1 O1 85.00(8) . 7 ? F Mg1 O1 95.60(9) 5_565 7 ? O1 Mg1 O1 179.20(13) 8_455 7 ? F Mg1 O1 177.52(8) . 2 ? F Mg1 O1 94.69(7) 5_565 2 ? O1 Mg1 O1 86.29(8) 8_455 2 ? O1 Mg1 O1 93.12(8) 7 2 ? F Mg1 O1 94.69(7) . . ? F Mg1 O1 177.52(8) 5_565 . ? O1 Mg1 O1 93.12(8) 8_455 . ? O1 Mg1 O1 86.29(8) 7 . ? O1 Mg1 O1 86.79(12) 2 . ? F Mg1 Li1 41.95(5) . 5_565 ? F Mg1 Li1 41.95(5) 5_565 5_565 ? O1 Mg1 Li1 90.40(7) 8_455 5_565 ? O1 Mg1 Li1 90.40(7) 7 5_565 ? O1 Mg1 Li1 136.61(6) 2 5_565 ? O1 Mg1 Li1 136.61(6) . 5_565 ? F Mg1 Mg1 41.95(5) . 5_565 ? F Mg1 Mg1 41.95(5) 5_565 5_565 ? O1 Mg1 Mg1 90.40(7) 8_455 5_565 ? O1 Mg1 Mg1 90.40(7) 7 5_565 ? O1 Mg1 Mg1 136.61(6) 2 5_565 ? O1 Mg1 Mg1 136.61(6) . 5_565 ? Li1 Mg1 Mg1 0.0 5_565 5_565 ? F Mg1 Li2 41.39(6) . 3 ? F Mg1 Li2 90.49(7) 5_565 3 ? O1 Mg1 Li2 136.96(7) 8_455 3 ? O1 Mg1 Li2 43.63(5) 7 3 ? O1 Mg1 Li2 136.75(6) 2 3 ? O1 Mg1 Li2 89.79(5) . 3 ? Li1 Mg1 Li2 60.09(3) 5_565 3 ? Mg1 Mg1 Li2 60.09(3) 5_565 3 ? F Mg1 Mg2 41.39(6) . 3 ? F Mg1 Mg2 90.49(7) 5_565 3 ? O1 Mg1 Mg2 136.96(7) 8_455 3 ? O1 Mg1 Mg2 43.63(5) 7 3 ? O1 Mg1 Mg2 136.75(6) 2 3 ? O1 Mg1 Mg2 89.79(5) . 3 ? Li1 Mg1 Mg2 60.09(3) 5_565 3 ? Mg1 Mg1 Mg2 60.09(3) 5_565 3 ? Li2 Mg1 Mg2 0.0 3 3 ? F Mg1 Li2 90.49(7) . 3_455 ? F Mg1 Li2 41.39(6) 5_565 3_455 ? O1 Mg1 Li2 43.63(5) 8_455 3_455 ? O1 Mg1 Li2 136.96(7) 7 3_455 ? O1 Mg1 Li2 89.79(5) 2 3_455 ? O1 Mg1 Li2 136.75(6) . 3_455 ? Li1 Mg1 Li2 60.09(3) 5_565 3_455 ? Mg1 Mg1 Li2 60.09(3) 5_565 3_455 ? Li2 Mg1 Li2 120.19(5) 3 3_455 ? Mg2 Mg1 Li2 120.19(5) 3 3_455 ? F Mg1 Mg2 90.49(7) . 3_455 ? F Mg1 Mg2 41.39(6) 5_565 3_455 ? O1 Mg1 Mg2 43.63(5) 8_455 3_455 ? O1 Mg1 Mg2 136.96(7) 7 3_455 ? O1 Mg1 Mg2 89.79(5) 2 3_455 ? O1 Mg1 Mg2 136.75(6) . 3_455 ? Li1 Mg1 Mg2 60.09(3) 5_565 3_455 ? Mg1 Mg1 Mg2 60.09(3) 5_565 3_455 ? Li2 Mg1 Mg2 120.19(5) 3 3_455 ? Mg2 Mg1 Mg2 120.19(5) 3 3_455 ? Li2 Mg1 Mg2 0.0 3_455 3_455 ? F Mg2 F 180.00(10) 3_445 7 ? F Mg2 O1 95.03(7) 3_445 . ? F Mg2 O1 84.97(7) 7 . ? F Mg2 O1 84.97(7) 3_445 5 ? F Mg2 O1 95.03(7) 7 5 ? O1 Mg2 O1 180.00(11) . 5 ? F Mg2 O1 84.97(7) 3_445 2 ? F Mg2 O1 95.03(7) 7 2 ? O1 Mg2 O1 86.47(10) . 2 ? O1 Mg2 O1 93.53(10) 5 2 ? F Mg2 O1 95.03(7) 3_445 6 ? F Mg2 O1 84.97(7) 7 6 ? O1 Mg2 O1 93.53(10) . 6 ? O1 Mg2 O1 86.47(10) 5 6 ? O1 Mg2 O1 180.00(9) 2 6 ? F Mg2 Li1 138.28(4) 3_445 7 ? F Mg2 Li1 41.72(4) 7 7 ? O1 Mg2 Li1 43.26(6) . 7 ? O1 Mg2 Li1 136.74(6) 5 7 ? O1 Mg2 Li1 90.10(6) 2 7 ? O1 Mg2 Li1 89.90(6) 6 7 ? F Mg2 Mg1 138.28(4) 3_445 7 ? F Mg2 Mg1 41.72(4) 7 7 ? O1 Mg2 Mg1 43.26(6) . 7 ? O1 Mg2 Mg1 136.74(6) 5 7 ? O1 Mg2 Mg1 90.10(6) 2 7 ? O1 Mg2 Mg1 89.90(6) 6 7 ? Li1 Mg2 Mg1 0.00(5) 7 7 ? F Mg2 Li1 41.72(4) 3_445 3_445 ? F Mg2 Li1 138.28(4) 7 3_445 ? O1 Mg2 Li1 136.74(6) . 3_445 ? O1 Mg2 Li1 43.26(6) 5 3_445 ? O1 Mg2 Li1 89.90(6) 2 3_445 ? O1 Mg2 Li1 90.10(6) 6 3_445 ? Li1 Mg2 Li1 180.00(5) 7 3_445 ? Mg1 Mg2 Li1 180.00(5) 7 3_445 ? F Mg2 Mg1 41.72(4) 3_445 3_445 ? F Mg2 Mg1 138.28(4) 7 3_445 ? O1 Mg2 Mg1 136.74(6) . 3_445 ? O1 Mg2 Mg1 43.26(6) 5 3_445 ? O1 Mg2 Mg1 89.90(6) 2 3_445 ? O1 Mg2 Mg1 90.10(6) 6 3_445 ? Li1 Mg2 Mg1 180.00(5) 7 3_445 ? Mg1 Mg2 Mg1 180.00(5) 7 3_445 ? Li1 Mg2 Mg1 0.00(5) 3_445 3_445 ? F Mg2 Li1 41.72(4) 3_445 7_455 ? F Mg2 Li1 138.28(4) 7 7_455 ? O1 Mg2 Li1 90.10(6) . 7_455 ? O1 Mg2 Li1 89.90(6) 5 7_455 ? O1 Mg2 Li1 43.26(6) 2 7_455 ? O1 Mg2 Li1 136.74(6) 6 7_455 ? Li1 Mg2 Li1 120.19(5) 7 7_455 ? Mg1 Mg2 Li1 120.19(5) 7 7_455 ? Li1 Mg2 Li1 59.81(5) 3_445 7_455 ? Mg1 Mg2 Li1 59.81(5) 3_445 7_455 ? F Mg2 Mg1 41.72(4) 3_445 7_455 ? F Mg2 Mg1 138.28(4) 7 7_455 ? O1 Mg2 Mg1 90.10(6) . 7_455 ? O1 Mg2 Mg1 89.90(6) 5 7_455 ? O1 Mg2 Mg1 43.26(6) 2 7_455 ? O1 Mg2 Mg1 136.74(6) 6 7_455 ? Li1 Mg2 Mg1 120.19(5) 7 7_455 ? Mg1 Mg2 Mg1 120.19(5) 7 7_455 ? Li1 Mg2 Mg1 59.81(5) 3_445 7_455 ? Mg1 Mg2 Mg1 59.81(5) 3_445 7_455 ? Li1 Mg2 Mg1 0.00(5) 7_455 7_455 ? Li2 F Mg2 0.0 3 3 ? Li2 F Mg1 96.89(8) 3 . ? Mg2 F Mg1 96.89(8) 3 . ? Li2 F Mg1 96.89(8) 3 5_565 ? Mg2 F Mg1 96.89(8) 3 5_565 ? Mg1 F Mg1 96.10(11) . 5_565 ? Li2 F Li1 96.89(8) 3 5_565 ? Mg2 F Li1 96.89(8) 3 5_565 ? Mg1 F Li1 96.10(11) . 5_565 ? Mg1 F Li1 0.0 5_565 5_565 ? Si O1 Li1 122.81(11) . 7 ? Si O1 Mg1 122.81(11) . 7 ? Li1 O1 Mg1 0.00(9) 7 7 ? Si O1 Mg1 123.11(11) . . ? Li1 O1 Mg1 93.71(8) 7 . ? Mg1 O1 Mg1 93.71(8) 7 . ? Si O1 Mg2 122.55(10) . . ? Li1 O1 Mg2 93.11(8) 7 . ? Mg1 O1 Mg2 93.11(8) 7 . ? Mg1 O1 Mg2 93.37(8) . . ? Si O3 Si 133.66(17) 6 . ? Si O2 Si 132.92(13) . 8_455 ? OW3 Na OW2 68.13(19) 5_556 3 ? OW3 Na OW2 68.13(19) 5_556 7_446 ? OW2 Na OW2 118.9(3) 3 7_446 ? OW3 Na OW3 55.9(4) 5_556 . ? OW2 Na OW3 60.30(13) 3 . ? OW2 Na OW3 60.30(13) 7_446 . ? OW3 Na OW3 89.3(5) 5_556 1_455 ? OW2 Na OW3 110.00(16) 3 1_455 ? OW2 Na OW3 110.00(16) 7_446 1_455 ? OW3 Na OW3 145.3(3) . 1_455 ? OW3 Na Na 73.3(5) 5_556 5_456 ? OW2 Na Na 103.0(2) 3 5_456 ? OW2 Na Na 103.0(2) 7_446 5_456 ? OW3 Na Na 129.2(4) . 5_456 ? OW3 Na Na 16.03(13) 1_455 5_456 ? OW3 Na Na 42.9(3) 5_556 5_556 ? OW2 Na Na 59.43(13) 3 5_556 ? OW2 Na Na 59.43(13) 7_446 5_556 ? OW3 Na Na 13.02(11) . 5_556 ? OW3 Na Na 132.2(4) 1_455 5_556 ? Na Na Na 116.2(5) 5_456 5_556 ? Na OW2 Na 61.1(3) 3_445 7_446 ? Na OW3 Na 124.1(4) 5_556 . ? Na OW3 Na 90.7(5) 5_556 1_655 ? Na OW3 Na 145.3(3) . 1_655 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.579 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.256 # Attachment '- 2WL.CIF' data_h-2wl2 _database_code_depnum_ccdc_archive 'CCDC 869128' #TrackingRef '- 2WL.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'hydrate sodium fluorohectorite' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'F2 Li0.70 Mg2.15 Na0.70 O14 Si4' _chemical_formula_weight 447.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 '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' F F 0.0171 0.0103 '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' Mg Mg 0.0486 0.0363 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 5.2432(10) _cell_length_b 9.0870(18) _cell_length_c 15.064(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.42(3) _cell_angle_gamma 90.00 _cell_volume 713.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1743 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 25.93 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 443 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STEO IPDS 1' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2477 _diffrn_reflns_av_R_equivalents 0.2261 _diffrn_reflns_av_sigmaI/netI 0.1511 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.93 _reflns_number_total 734 _reflns_number_gt 426 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STEO IPDS 1' _computing_cell_refinement 'STEO CELL' _computing_data_reduction 'STEO X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 734 _refine_ls_number_parameters 73 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1611 _refine_ls_R_factor_gt 0.1150 _refine_ls_wR_factor_ref 0.3223 _refine_ls_wR_factor_gt 0.2787 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.10636(15) 0.16707(7) 0.81766(6) 0.0263(2) Uani 1 1 d . . . Mg1 Mg 0.0000 0.0000 1.0000 0.0220(6) Uani 0.703(3) 4 d SP . . Li1 Li 0.0000 0.0000 1.0000 0.0220(6) Uani 0.297(3) 4 d SP . . Mg2 Mg 0.0000 0.33361(14) 1.0000 0.0252(4) Uani 0.767(2) 2 d SP . . Li2 Li 0.0000 0.33361(14) 1.0000 0.0252(4) Uani 0.233(3) 2 d SP . . O1 O 0.1413(3) 0.16780(17) 0.92345(13) 0.0264(5) Uani 1 1 d . . . O5 O 0.3413(3) 0.24843(18) 0.77487(13) 0.0284(5) Uani 1 1 d . . . F F -0.3542(4) 0.0000 0.93276(15) 0.0302(6) Uani 1 2 d S . . O3 O 0.0852(5) 0.0000 0.77472(18) 0.0292(8) Uani 1 2 d S . . Na Na 0.5000 0.3318(12) 0.5000 0.125(5) Uani 0.35 2 d SP . . OW1 O -0.210(4) 0.0000 0.5880(9) 0.549(15) Uani 1 2 d S . . OW2 O -0.134(3) 0.353(2) 0.5917(7) 0.321(11) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0213(3) 0.0097(3) 0.0487(4) -0.0008(3) 0.0073(3) -0.0003(3) Mg1 0.0199(10) 0.0065(9) 0.0402(12) 0.000 0.0064(9) 0.000 Li1 0.0199(10) 0.0065(9) 0.0402(12) 0.000 0.0064(9) 0.000 Mg2 0.0151(7) 0.0067(6) 0.0543(9) 0.000 0.0068(6) 0.000 Li2 0.0151(7) 0.0067(6) 0.0543(9) 0.000 0.0068(6) 0.000 O1 0.0147(8) 0.0083(8) 0.0582(11) 0.0005(7) 0.0124(8) 0.0002(6) O5 0.0186(9) 0.0105(8) 0.0573(11) -0.0010(8) 0.0090(8) 0.0016(7) F 0.0233(10) 0.0129(9) 0.0555(13) 0.000 0.0088(10) 0.000 O3 0.0258(13) 0.0136(11) 0.0493(15) 0.000 0.0085(12) 0.000 Na 0.162(10) 0.105(8) 0.116(7) 0.000 0.049(6) 0.000 OW1 0.87(3) 0.42(3) 0.259(10) 0.000 -0.336(12) 0.000 OW2 0.262(14) 0.63(3) 0.068(5) 0.105(8) 0.024(7) 0.165(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si O1 1.584(2) . ? Si O5 1.630(2) . ? Si O3 1.6491(13) . ? Si O5 1.6541(19) 8_455 ? Si Mg2 3.2387(11) . ? Si Mg1 3.2410(10) . ? Si Mg2 3.2461(13) 7_557 ? Mg1 F 2.013(2) . ? Mg1 F 2.013(2) 5_557 ? Mg1 O1 2.0963(18) 6 ? Mg1 O1 2.0963(18) 2_557 ? Mg1 O1 2.0963(18) . ? Mg1 O1 2.0963(18) 5_557 ? Mg1 Li2 3.0263(8) 7_557 ? Mg1 Li2 3.0263(8) 3_445 ? Mg1 Mg2 3.0263(8) 7_557 ? Mg1 Mg2 3.0263(8) 3_445 ? Mg1 Li2 3.0263(8) 7_457 ? Mg1 Li2 3.0263(8) 3_545 ? Mg2 F 2.0174(18) 7_457 ? Mg2 F 2.0174(18) 3 ? Mg2 O1 2.083(2) . ? Mg2 O1 2.083(2) 2_557 ? Mg2 O1 2.0935(19) 8_455 ? Mg2 O1 2.0935(19) 7_557 ? Mg2 Li2 3.024(3) 5_567 ? Mg2 Mg2 3.024(3) 5_567 ? Mg2 Li1 3.0263(8) 3 ? Mg2 Mg1 3.0263(8) 3 ? Mg2 Mg1 3.0263(8) 3_455 ? Mg2 Li1 3.0263(8) 3_455 ? O1 Li2 2.0935(19) 7_557 ? O1 Mg2 2.0935(19) 7_557 ? O5 Si 1.6541(19) 8 ? F Li2 2.0174(18) 7_457 ? F Mg2 2.0174(18) 7_457 ? F Mg2 2.0174(18) 3_445 ? F Li2 2.0174(18) 3_445 ? O3 Si 1.6491(13) 6 ? Na OW1 2.372(16) 3 ? Na OW1 2.372(16) 7_556 ? Na OW2 2.243(15) 1_655 ? Na OW2 2.243(15) 2_556 ? Na OW2 2.335(19) 7_556 ? Na OW2 2.335(19) 8 ? Na Na 3.014(10) 7_556 ? Na Na 3.014(10) 7_656 ? Na Na 3.06(2) 5_666 ? OW1 Na 2.372(16) 7_556 ? OW1 Na 2.372(16) 3_445 ? OW2 Na 2.243(15) 1_455 ? OW2 Na 2.335(19) 7_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si O5 112.87(10) . . ? O1 Si O3 113.19(11) . . ? O5 Si O3 106.45(12) . . ? O1 Si O5 112.81(11) . 8_455 ? O5 Si O5 105.94(8) . 8_455 ? O3 Si O5 104.93(11) . 8_455 ? O1 Si Mg2 32.44(6) . . ? O5 Si Mg2 109.44(7) . . ? O3 Si Mg2 138.80(10) . . ? O5 Si Mg2 84.07(8) 8_455 . ? O1 Si Mg1 32.92(6) . . ? O5 Si Mg1 139.19(8) . . ? O3 Si Mg1 83.73(9) . . ? O5 Si Mg1 109.33(8) 8_455 . ? Mg2 Si Mg1 55.79(3) . . ? O1 Si Mg2 32.60(7) . 7_557 ? O5 Si Mg2 84.17(7) . 7_557 ? O3 Si Mg2 109.80(9) . 7_557 ? O5 Si Mg2 139.25(8) 8_455 7_557 ? Mg2 Si Mg2 55.71(3) . 7_557 ? Mg1 Si Mg2 55.62(2) . 7_557 ? F Mg1 F 180.0 . 5_557 ? F Mg1 O1 94.93(7) . 6 ? F Mg1 O1 85.07(7) 5_557 6 ? F Mg1 O1 85.07(7) . 2_557 ? F Mg1 O1 94.93(7) 5_557 2_557 ? O1 Mg1 O1 180.000(1) 6 2_557 ? F Mg1 O1 94.93(7) . . ? F Mg1 O1 85.07(7) 5_557 . ? O1 Mg1 O1 93.34(10) 6 . ? O1 Mg1 O1 86.66(10) 2_557 . ? F Mg1 O1 85.07(7) . 5_557 ? F Mg1 O1 94.93(7) 5_557 5_557 ? O1 Mg1 O1 86.66(10) 6 5_557 ? O1 Mg1 O1 93.34(10) 2_557 5_557 ? O1 Mg1 O1 180.000(1) . 5_557 ? F Mg1 Li2 138.61(5) . 7_557 ? F Mg1 Li2 41.39(5) 5_557 7_557 ? O1 Mg1 Li2 90.23(5) 6 7_557 ? O1 Mg1 Li2 89.77(5) 2_557 7_557 ? O1 Mg1 Li2 43.72(5) . 7_557 ? O1 Mg1 Li2 136.28(5) 5_557 7_557 ? F Mg1 Li2 41.39(5) . 3_445 ? F Mg1 Li2 138.61(5) 5_557 3_445 ? O1 Mg1 Li2 89.77(5) 6 3_445 ? O1 Mg1 Li2 90.23(5) 2_557 3_445 ? O1 Mg1 Li2 136.28(5) . 3_445 ? O1 Mg1 Li2 43.72(5) 5_557 3_445 ? Li2 Mg1 Li2 180.0 7_557 3_445 ? F Mg1 Mg2 138.61(5) . 7_557 ? F Mg1 Mg2 41.39(5) 5_557 7_557 ? O1 Mg1 Mg2 90.23(5) 6 7_557 ? O1 Mg1 Mg2 89.77(5) 2_557 7_557 ? O1 Mg1 Mg2 43.72(5) . 7_557 ? O1 Mg1 Mg2 136.28(5) 5_557 7_557 ? Li2 Mg1 Mg2 0.0 7_557 7_557 ? Li2 Mg1 Mg2 180.0 3_445 7_557 ? F Mg1 Mg2 41.39(5) . 3_445 ? F Mg1 Mg2 138.61(5) 5_557 3_445 ? O1 Mg1 Mg2 89.77(5) 6 3_445 ? O1 Mg1 Mg2 90.23(5) 2_557 3_445 ? O1 Mg1 Mg2 136.28(5) . 3_445 ? O1 Mg1 Mg2 43.72(5) 5_557 3_445 ? Li2 Mg1 Mg2 180.0 7_557 3_445 ? Li2 Mg1 Mg2 0.00(4) 3_445 3_445 ? Mg2 Mg1 Mg2 180.0 7_557 3_445 ? F Mg1 Li2 41.39(5) . 7_457 ? F Mg1 Li2 138.61(5) 5_557 7_457 ? O1 Mg1 Li2 136.28(5) 6 7_457 ? O1 Mg1 Li2 43.72(5) 2_557 7_457 ? O1 Mg1 Li2 89.77(5) . 7_457 ? O1 Mg1 Li2 90.23(5) 5_557 7_457 ? Li2 Mg1 Li2 120.05(4) 7_557 7_457 ? Li2 Mg1 Li2 59.95(4) 3_445 7_457 ? Mg2 Mg1 Li2 120.05(4) 7_557 7_457 ? Mg2 Mg1 Li2 59.95(4) 3_445 7_457 ? F Mg1 Li2 138.61(5) . 3_545 ? F Mg1 Li2 41.39(5) 5_557 3_545 ? O1 Mg1 Li2 43.72(5) 6 3_545 ? O1 Mg1 Li2 136.28(5) 2_557 3_545 ? O1 Mg1 Li2 90.23(5) . 3_545 ? O1 Mg1 Li2 89.77(5) 5_557 3_545 ? Li2 Mg1 Li2 59.95(4) 7_557 3_545 ? Li2 Mg1 Li2 120.05(4) 3_445 3_545 ? Mg2 Mg1 Li2 59.95(4) 7_557 3_545 ? Mg2 Mg1 Li2 120.05(4) 3_445 3_545 ? Li2 Mg1 Li2 180.0 7_457 3_545 ? F Mg2 F 82.92(11) 7_457 3 ? F Mg2 O1 176.55(8) 7_457 . ? F Mg2 O1 94.93(7) 3 . ? F Mg2 O1 94.93(7) 7_457 2_557 ? F Mg2 O1 176.55(8) 3 2_557 ? O1 Mg2 O1 87.35(11) . 2_557 ? F Mg2 O1 85.04(8) 7_457 8_455 ? F Mg2 O1 95.49(8) 3 8_455 ? O1 Mg2 O1 92.51(8) . 8_455 ? O1 Mg2 O1 86.98(8) 2_557 8_455 ? F Mg2 O1 95.49(8) 7_457 7_557 ? F Mg2 O1 85.04(8) 3 7_557 ? O1 Mg2 O1 86.98(8) . 7_557 ? O1 Mg2 O1 92.51(8) 2_557 7_557 ? O1 Mg2 O1 179.29(11) 8_455 7_557 ? F Mg2 Li2 41.46(6) 7_457 5_567 ? F Mg2 Li2 41.46(6) 3 5_567 ? O1 Mg2 Li2 136.33(6) . 5_567 ? O1 Mg2 Li2 136.33(6) 2_557 5_567 ? O1 Mg2 Li2 90.35(5) 8_455 5_567 ? O1 Mg2 Li2 90.35(5) 7_557 5_567 ? F Mg2 Mg2 41.46(6) 7_457 5_567 ? F Mg2 Mg2 41.46(6) 3 5_567 ? O1 Mg2 Mg2 136.33(6) . 5_567 ? O1 Mg2 Mg2 136.33(6) 2_557 5_567 ? O1 Mg2 Mg2 90.35(5) 8_455 5_567 ? O1 Mg2 Mg2 90.35(5) 7_557 5_567 ? Li2 Mg2 Mg2 0.0 5_567 5_567 ? F Mg2 Li1 90.15(7) 7_457 3 ? F Mg2 Li1 41.29(6) 3 3 ? O1 Mg2 Li1 89.98(5) . 3 ? O1 Mg2 Li1 136.30(5) 2_557 3 ? O1 Mg2 Li1 136.72(6) 8_455 3 ? O1 Mg2 Li1 43.79(5) 7_557 3 ? Li2 Mg2 Li1 60.03(2) 5_567 3 ? Mg2 Mg2 Li1 60.03(2) 5_567 3 ? F Mg2 Mg1 90.15(7) 7_457 3 ? F Mg2 Mg1 41.29(6) 3 3 ? O1 Mg2 Mg1 89.98(5) . 3 ? O1 Mg2 Mg1 136.30(5) 2_557 3 ? O1 Mg2 Mg1 136.72(6) 8_455 3 ? O1 Mg2 Mg1 43.79(5) 7_557 3 ? Li2 Mg2 Mg1 60.03(2) 5_567 3 ? Mg2 Mg2 Mg1 60.03(2) 5_567 3 ? Li1 Mg2 Mg1 0.0 3 3 ? F Mg2 Mg1 41.29(6) 7_457 3_455 ? F Mg2 Mg1 90.15(7) 3 3_455 ? O1 Mg2 Mg1 136.30(5) . 3_455 ? O1 Mg2 Mg1 89.98(5) 2_557 3_455 ? O1 Mg2 Mg1 43.79(5) 8_455 3_455 ? O1 Mg2 Mg1 136.72(6) 7_557 3_455 ? Li2 Mg2 Mg1 60.03(2) 5_567 3_455 ? Mg2 Mg2 Mg1 60.03(2) 5_567 3_455 ? Li1 Mg2 Mg1 120.05(4) 3 3_455 ? Mg1 Mg2 Mg1 120.05(4) 3 3_455 ? F Mg2 Li1 41.29(6) 7_457 3_455 ? F Mg2 Li1 90.15(7) 3 3_455 ? O1 Mg2 Li1 136.30(5) . 3_455 ? O1 Mg2 Li1 89.98(5) 2_557 3_455 ? O1 Mg2 Li1 43.79(5) 8_455 3_455 ? O1 Mg2 Li1 136.72(6) 7_557 3_455 ? Li2 Mg2 Li1 60.03(2) 5_567 3_455 ? Mg2 Mg2 Li1 60.03(2) 5_567 3_455 ? Li1 Mg2 Li1 120.05(4) 3 3_455 ? Mg1 Mg2 Li1 120.05(4) 3 3_455 ? Mg1 Mg2 Li1 0.0 3_455 3_455 ? Si O1 Mg2 123.50(10) . . ? Si O1 Li2 123.35(11) . 7_557 ? Mg2 O1 Li2 93.02(8) . 7_557 ? Si O1 Mg2 123.35(11) . 7_557 ? Mg2 O1 Mg2 93.02(8) . 7_557 ? Li2 O1 Mg2 0.00(7) 7_557 7_557 ? Si O1 Mg1 122.84(9) . . ? Mg2 O1 Mg1 93.00(9) . . ? Li2 O1 Mg1 92.49(8) 7_557 . ? Mg2 O1 Mg1 92.49(8) 7_557 . ? Si O5 Si 134.08(13) . 8 ? Mg1 F Li2 97.32(8) . 7_457 ? Mg1 F Mg2 97.32(8) . 7_457 ? Li2 F Mg2 0.0 7_457 7_457 ? Mg1 F Mg2 97.32(8) . 3_445 ? Li2 F Mg2 97.08(11) 7_457 3_445 ? Mg2 F Mg2 97.08(11) 7_457 3_445 ? Mg1 F Li2 97.32(8) . 3_445 ? Li2 F Li2 97.08(11) 7_457 3_445 ? Mg2 F Li2 97.08(11) 7_457 3_445 ? Mg2 F Li2 0.00(5) 3_445 3_445 ? Si O3 Si 134.03(18) . 6 ? OW1 Na OW1 99.8(7) 3 7_556 ? OW1 Na OW2 91.0(7) 3 1_655 ? OW1 Na OW2 82.6(6) 7_556 1_655 ? OW1 Na OW2 82.6(6) 3 2_556 ? OW1 Na OW2 91.0(7) 7_556 2_556 ? OW2 Na OW2 170.0(12) 1_655 2_556 ? OW1 Na OW2 169.8(7) 3 7_556 ? OW1 Na OW2 86.8(5) 7_556 7_556 ? OW2 Na OW2 97.7(5) 1_655 7_556 ? OW2 Na OW2 89.5(6) 2_556 7_556 ? OW1 Na OW2 86.8(5) 3 8 ? OW1 Na OW2 169.8(7) 7_556 8 ? OW2 Na OW2 89.5(6) 1_655 8 ? OW2 Na OW2 97.7(5) 2_556 8 ? OW2 Na OW2 87.8(9) 7_556 8 ? OW1 Na Na 82.0(5) 3 7_556 ? OW1 Na Na 140.8(5) 7_556 7_556 ? OW2 Na Na 136.6(5) 1_655 7_556 ? OW2 Na Na 50.2(5) 2_556 7_556 ? OW2 Na Na 88.0(6) 7_556 7_556 ? OW2 Na Na 47.5(4) 8 7_556 ? OW1 Na Na 140.8(5) 3 7_656 ? OW1 Na Na 82.0(5) 7_556 7_656 ? OW2 Na Na 50.2(5) 1_655 7_656 ? OW2 Na Na 136.6(5) 2_556 7_656 ? OW2 Na Na 47.5(4) 7_556 7_656 ? OW2 Na Na 88.0(6) 8 7_656 ? Na Na Na 120.9(7) 7_556 7_656 ? OW1 Na Na 49.9(4) 3 5_666 ? OW1 Na Na 49.9(4) 7_556 5_666 ? OW2 Na Na 85.0(6) 1_655 5_666 ? OW2 Na Na 85.0(6) 2_556 5_666 ? OW2 Na Na 136.1(5) 7_556 5_666 ? OW2 Na Na 136.1(5) 8 5_666 ? Na Na Na 119.6(3) 7_556 5_666 ? Na Na Na 119.6(3) 7_656 5_666 ? Na OW1 Na 80.2(7) 7_556 3_445 ? Na OW2 Na 82.3(5) 1_455 7_556 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.122 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.255