Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Russell Morris' 'Ivor Bull' 'Philip Lightfoot' 'Luis Villaescusa' 'Paul S. Wheatley' _publ_contact_author_name 'Prof Russell Morris' _publ_contact_author_address ; Department of Chemistry University of St Andrews Purdie Building North Haugh St Andrews KY169ST UNITED KINGDOM ; _publ_contact_author_email REM1@ST-AND.AC.UK _publ_section_title ; The location of fluoride and organic guests in 'as-made' pure silica zeolites FER and CHA. ; data_CHA _database_code_CSD 201658 _audit_creation_date 2002-02-18T16:31:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C39 H24 F3 N3 O72 Si36' _chemical_formula_structural 'C39 H24 F3 N3 O72 Si36' _chemical_formula_sum 'C39 H24 F3 N3 O72 Si36' _chemical_formula_weight 2754.85 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 m' _symmetry_space_group_name_Hall '-R 3 m' _symmetry_Int_Tables_number 166 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 13.4902(10) _cell_length_b 13.4902(9) _cell_length_c 14.7578(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2325.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 30.09 _cell_measurement_wavelength 0.6984 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.967 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1386 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.61 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6984 _diffrn_radiation_type synchrotron _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_unetI/netI 0.0169 _diffrn_reflns_number 3220 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 30.09 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 0.926 _diffrn_measured_fraction_theta_max 0.926 _reflns_number_total 809 _reflns_number_gt 756 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0877P)^2^+22.5326P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 809 _refine_ls_number_parameters 58 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1689 _refine_ls_wR_factor_gt 0.1658 _refine_ls_goodness_of_fit_ref 1.17 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.005 _refine_diff_density_max 0.686 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.139 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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_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 Si1 Si 0.43743(4) 0.10387(4) 0.72936(3) 0.01129(13) Uani 1 1 d . . . O1 O 0.54681(10) 0.0936(2) 0.70241(15) 0.0174(4) Uani 1 2 d S . . O2 O 0.3333 0.01383(16) 0.6667 0.0161(4) Uani 1 2 d S . . O3 O 0.4610(2) 0.23050(11) 0.70828(17) 0.0224(5) Uani 1 2 d S . . O4 O 0.40075(17) 0.06741(17) 0.8333 0.0189(5) Uani 1 2 d S . . F1 F 0.5674(13) 0.3419(13) 0.8034(10) 0.021(3) Uiso 0.08 1 d P . . C1 C 0.3333 -0.3333 0.6467(3) 0.039(3) Uiso 0.50 6 d SPD . . C2 C 0.2694(4) -0.2694(4) 0.7846(4) 0.164(11) Uiso 0.50 2 d SPD . . C3 C 0.3942(5) -0.2116(10) 0.8192(5) 0.091(5) Uiso 0.50 2 d SPD . . C4 C 0.2704(3) -0.2704(3) 0.6788(4) 0.088(5) Uiso 0.50 2 d SPD . . N1 N 0.3333 -0.3333 0.5439(4) 0.097(8) Uiso 0.50 6 d SPD . . C5 C 0.3811(5) -0.4067(5) 0.5101(5) 0.115(8) Uiso 0.25 1 d PD . . 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 Si1 0.0128(2) 0.0126(2) 0.0108(3) 0.00081(15) 0.00083(16) 0.00808(14) O1 0.0124(6) 0.0221(11) 0.0210(9) -0.0004(8) -0.0002(4) 0.0110(5) O2 0.0145(9) 0.0177(7) 0.0152(8) -0.0030(4) -0.0060(7) 0.0072(5) O3 0.0262(11) 0.0122(6) 0.0334(11) 0.0061(5) 0.0122(10) 0.0131(6) O4 0.0219(5) 0.0219(5) 0.0089(8) -0.0006(4) 0.0006(4) 0.0082(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si1 O1 1.5995(8) . ? Si1 O3 1.6041(8) . ? Si1 O4 1.6117(9) . ? Si1 O2 1.6117(9) . ? Si1 F1 2.021(16) 24 ? O1 Si1 1.5995(8) 23_655 ? O2 Si1 1.6117(8) 12_556 ? O3 Si1 1.6041(8) 24 ? O4 Si1 1.6117(9) 16_546 ? C1 C4 1.474(7) 25_546 ? C1 C4 1.474(7) 26_556 ? C1 C4 1.474(7) 27_446 ? C1 N1 1.517(7) . ? C1 C4 1.544(7) . ? C1 C4 1.544(7) 3_655 ? C1 C4 1.544(7) 2_545 ? C2 N1 1.496(9) 25_546 ? C2 C3 1.546(6) 2_545 ? C2 C3 1.546(6) . ? C2 C4 1.561(7) . ? C3 C5 1.273(8) 11_446 ? C3 C5 1.272(8) 25_546 ? C3 N1 1.488(11) 25_546 ? C3 C2 1.546(6) 3_655 ? C3 C5 1.572(9) 27_446 ? C3 C5 1.571(9) 10_546 ? C4 C1 1.474(7) 25_546 ? C4 C4 1.512(7) 26_556 ? C4 C4 1.512(7) 27_446 ? N1 C2 1.496(9) 25_546 ? N1 C2 1.496(9) 26_556 ? N1 C2 1.496(9) 27_446 ? N1 C3 1.488(11) 26_556 ? N1 C3 1.488(11) 25_546 ? N1 C3 1.488(11) 27_446 ? N1 C5 1.510(7) 3_655 ? N1 C5 1.510(7) 23_655 ? N1 C5 1.510(7) 24_545 ? N1 C5 1.510(7) 2_545 ? N1 C5 1.510(7) 22 ? N1 C5 1.510(7) . ? C5 C3 1.572(9) 26_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 Si1 O3 110.10(12) . . ? O1 Si1 O4 111.48(9) . . ? O3 Si1 O4 112.13(10) . . ? O1 Si1 O2 106.61(10) . . ? O3 Si1 O2 108.98(12) . . ? O4 Si1 O2 107.32(9) . . ? O1 Si1 F1 75.0(4) . 24 ? O3 Si1 F1 67.1(5) . 24 ? O4 Si1 F1 75.1(4) . 24 ? O2 Si1 F1 176.0(5) . 24 ? Si1 O1 Si1 149.90(16) 23_655 . ? Si1 O2 Si1 142.93(15) . 12_556 ? Si1 O3 Si1 149.98(17) . 24 ? Si1 O4 Si1 144.34(16) 16_546 . ? #==END data_FER _database_code_CSD 201659 _audit_creation_date 2003-04-30T16:15:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C20 H24 F4 N4 O72 Si36' _chemical_formula_weight 2559.67 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_space_group_name_H-M 'P n n m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 7.3952(15) _cell_length_b 14.099(3) _cell_length_c 18.761(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1956.1(7) _cell_formula_units_Z 1 _cell_measurement_temperature 210(2) _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 30.37 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.6942 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.6942 _diffrn_radiation_type Synchrotron _diffrn_radiation_monochromator Silicon _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_unetI/netI 0.0289 _diffrn_reflns_number 12895 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 30.37 _diffrn_reflns_theta_full 30.37 _diffrn_measured_fraction_theta_full 0.934 _diffrn_measured_fraction_theta_max 0.934 _reflns_number_total 2839 _reflns_number_gt 2338 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0911P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2839 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.016 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.212 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Si1 Si 0.21861(8) 0.19882(4) 0.16977(3) 0.00939(16) Uani 1 1 d . . . Si2 Si -0.19285(8) 0.20603(4) 0.18077(3) 0.00931(16) Uani 1 1 d . . . Si3 Si 0.5 0.5 0.15360(5) 0.00714(19) Uani 1 2 d S . . Si4 Si 0.51059(8) 0.29998(4) 0.08356(3) 0.00880(17) Uani 1 1 d . . . Si5 Si 0.29251(8) -0.00096(4) 0.22603(4) 0.00778(16) Uani 1 1 d . . . O1 O 0.5 0 0.24990(14) 0.0156(5) Uani 1 2 d S . . O2 O 0.5430(4) 0.28887(19) 0 0.0219(6) Uani 1 2 d S . . O3 O 0.2523(2) 0.08651(12) 0.17356(9) 0.0166(4) Uani 1 1 d . . . O4 O 0.0109(2) 0.21994(14) 0.15335(11) 0.0178(4) Uani 1 1 d . . . O5 O 0.3332(2) 0.24106(13) 0.10439(10) 0.0191(4) Uani 1 1 d . . . O6 O -0.2469(3) 0.09586(12) 0.18293(10) 0.0208(4) Uani 1 1 d . . . O7 O 0.4845(2) 0.40899(14) 0.10316(12) 0.0235(4) Uani 1 1 d . . . O8 O -0.3181(2) 0.25805(14) 0.12412(11) 0.0227(4) Uani 1 1 d . . . O9 O 0.3248(3) 0.50830(15) 0.20257(11) 0.0259(5) Uani 1 1 d . . . O10 O 0.2849(3) 0.24832(14) 0.24165(11) 0.0297(5) Uani 1 1 d . . . C1 C 1.0039(5) 0.4023(4) 0 0.0325(10) Uani 1 2 d S . . H1 H 1.0075 0.3349 0 0.039 Uiso 2 2 calc SPR . . C2 C 0.4987(4) -0.0490(3) 0.43694(18) 0.0341(7) Uani 1 1 d . . . H2 H 0.4988 -0.0826 0.3931 0.041 Uiso 1 1 calc R . . C3 C 0.0867(18) 0.0785(6) 0 0.081(3) Uani 1 2 d S . . H3 H 0.1479 0.1377 0 0.097 Uiso 2 2 calc SPR . . C4 C 0.1921(17) -0.0030(10) 0 0.114(5) Uani 1 2 d S . . H4 H 0.3206 -0.0035 0 0.137 Uiso 2 2 calc SPR . . C5 C -0.0892(19) 0.0801(9) 0 0.116(4) Uani 1 2 d S . . H5 H -0.1475 0.1402 0 0.139 Uiso 2 2 calc SPR . . F1 F 0.475(2) 0.3391(16) 0.2422(12) 0.101(6) Uiso 0.2 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 Si1 0.0066(3) 0.0079(3) 0.0137(3) -0.0004(2) -0.0021(2) 0.0010(2) Si2 0.0067(3) 0.0068(3) 0.0144(3) -0.0007(2) 0.0037(2) -0.0007(2) Si3 0.0051(4) 0.0073(4) 0.0090(4) 0 0 0.0001(3) Si4 0.0081(3) 0.0075(3) 0.0108(3) -0.0003(2) 0.00014(19) -0.0012(2) Si5 0.0040(3) 0.0087(3) 0.0106(3) 0.00102(19) -0.0001(2) -0.00016(19) O1 0.0033(10) 0.0293(14) 0.0143(12) 0 0 0.0014(8) O2 0.0306(14) 0.0217(14) 0.0135(12) 0 0 -0.0010(11) O3 0.0221(8) 0.0096(8) 0.0181(9) 0.0021(6) -0.0049(7) 0.0037(7) O4 0.0059(7) 0.0210(9) 0.0264(10) 0.0054(8) 0.0030(6) 0.0025(6) O5 0.0091(7) 0.0212(9) 0.0271(10) 0.0054(7) 0.0025(7) -0.0048(7) O6 0.0316(10) 0.0086(8) 0.0223(9) -0.0005(6) 0.0078(8) -0.0054(7) O7 0.0346(11) 0.0108(8) 0.0252(10) -0.0069(7) -0.0011(8) 0.0001(7) O8 0.0103(8) 0.0304(11) 0.0273(10) 0.0108(8) -0.0049(7) 0.0004(7) O9 0.0081(7) 0.0524(14) 0.0172(9) 0.0018(8) 0.0053(7) 0.0027(7) O10 0.0379(11) 0.0275(11) 0.0238(11) -0.0126(8) -0.0115(9) 0.0078(9) C1 0.040(2) 0.026(2) 0.032(2) 0 0 -0.0007(17) C2 0.0377(17) 0.0418(19) 0.0227(15) -0.0084(14) -0.0008(12) 0.0015(14) C3 0.144(9) 0.077(5) 0.020(3) 0 0 -0.038(6) C4 0.107(8) 0.214(16) 0.020(3) 0 0 -0.040(9) C5 0.146(11) 0.180(13) 0.022(3) 0 0 -0.018(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si1 O4 1.5949(17) . ? Si1 O10 1.5956(19) . ? Si1 O3 1.6045(18) . ? Si1 O5 1.6052(18) . ? Si2 O8 1.5893(18) . ? Si2 O10 1.600(2) 4_455 ? Si2 O4 1.6040(17) . ? Si2 O6 1.6043(18) . ? Si2 F1 2.01(2) 4_455 ? Si3 O9 1.5925(19) 2_665 ? Si3 O9 1.5925(19) . ? Si3 O7 1.598(2) . ? Si3 O7 1.598(2) 2_665 ? Si4 O8 1.5916(18) 1_655 ? Si4 O7 1.592(2) . ? Si4 O2 1.5936(9) . ? Si4 O5 1.6014(17) . ? Si5 O1 1.5985(10) . ? Si5 O6 1.5994(19) 2 ? Si5 O9 1.601(2) 3_545 ? Si5 O3 1.6058(18) . ? O1 Si5 1.5985(10) 2_655 ? O2 Si4 1.5936(9) 6 ? O6 Si5 1.5994(19) 2 ? O8 Si4 1.5916(18) 1_455 ? O9 Si5 1.601(2) 3 ? O10 Si2 1.600(2) 4 ? C1 C2 1.368(4) 3_655 ? C1 C2 1.368(4) 8_765 ? C2 C1 1.368(4) 3_645 ? C2 C2 1.381(7) 2_655 ? C3 C5 1.301(15) . ? C3 C4 1.389(12) . ? C4 C5 1.327(13) 5 ? C5 C4 1.327(13) 5 ? F1 Si2 2.01(2) 4 ? 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 O4 Si1 O10 112.19(11) . . ? O4 Si1 O3 110.02(10) . . ? O10 Si1 O3 110.27(10) . . ? O4 Si1 O5 106.95(10) . . ? O10 Si1 O5 108.74(11) . . ? O3 Si1 O5 108.54(10) . . ? O8 Si2 O10 111.27(12) . 4_455 ? O8 Si2 O4 106.05(10) . . ? O10 Si2 O4 109.83(11) 4_455 . ? O8 Si2 O6 108.58(11) . . ? O10 Si2 O6 109.93(10) 4_455 . ? O4 Si2 O6 111.13(10) . . ? O8 Si2 F1 171.0(6) . 4_455 ? O10 Si2 F1 62.3(6) 4_455 4_455 ? O4 Si2 F1 71.9(5) . 4_455 ? O6 Si2 F1 80.1(6) . 4_455 ? O9 Si3 O9 109.53(16) 2_665 . ? O9 Si3 O7 109.94(10) 2_665 . ? O9 Si3 O7 110.00(10) . . ? O9 Si3 O7 110.00(10) 2_665 2_665 ? O9 Si3 O7 109.94(10) . 2_665 ? O7 Si3 O7 107.41(16) . 2_665 ? O8 Si4 O7 110.17(11) 1_655 . ? O8 Si4 O2 108.30(13) 1_655 . ? O7 Si4 O2 109.90(13) . . ? O8 Si4 O5 110.05(10) 1_655 . ? O7 Si4 O5 110.18(10) . . ? O2 Si4 O5 108.20(13) . . ? O1 Si5 O6 110.57(9) . 2 ? O1 Si5 O9 106.57(12) . 3_545 ? O6 Si5 O9 112.13(11) 2 3_545 ? O1 Si5 O3 110.06(9) . . ? O6 Si5 O3 107.07(11) 2 . ? O9 Si5 O3 110.48(11) 3_545 . ? Si5 O1 Si5 147.46(19) . 2_655 ? Si4 O2 Si4 159.3(2) 6 . ? Si1 O3 Si5 144.47(12) . . ? Si1 O4 Si2 145.07(14) . . ? Si4 O5 Si1 144.23(13) . . ? Si5 O6 Si2 151.08(14) 2 . ? Si4 O7 Si3 154.55(15) . . ? Si2 O8 Si4 162.75(13) . 1_455 ? Si3 O9 Si5 156.55(15) . 3 ? Si1 O10 Si2 167.52(17) . 4 ? C2 C1 C2 119.7(5) 3_655 8_765 ? C1 C2 C2 120.2(2) 3_645 2_655 ? C5 C3 C4 125.2(9) . . ? C5 C4 C3 110.9(11) 5 . ? C3 C5 C4 124.0(12) . 5 ? #==END