# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Louisa Hope-Weeks' _publ_contact_author_email louisa.hope-weeks@ttu.edu _publ_author_name C.Krempner data_2009072401krempnerbrw _database_code_depnum_ccdc_archive 'CCDC 829366' #TrackingRef '2009072401KrempnerBRW.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 Ca O6 Si8' _chemical_formula_weight 631.41 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 16.731(4) _cell_length_b 12.770(3) _cell_length_c 16.848(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3599.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8141 _exptl_absorpt_correction_T_max 0.8858 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16495 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0139 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 24.66 _reflns_number_total 1589 _reflns_number_gt 1365 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0461P)^2^+4.5364P] 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_extinction_coef ? _refine_ls_number_reflns 1589 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.261 _refine_ls_shift/su_mean 0.029 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 Ca1 Ca 0.5000 1.0000 0.0000 0.0399(2) Uani 1 4 d S . . Si1 Si 0.5000 0.79403(7) 0.16156(5) 0.0579(3) Uani 1 2 d S . . Si2 Si 0.5000 0.72662(8) 0.03515(7) 0.0718(4) Uani 0.8054(16) 2 d SP . . Si3 Si 0.60932(5) 0.90299(6) 0.16538(4) 0.0574(3) Uani 0.8054(16) 1 d P . . O2 O 0.5000 0.8213(2) -0.03615(15) 0.0697(9) Uani 0.8054(16) 2 d SP . . O3 O 0.60851(13) 0.99561(15) 0.09258(11) 0.0640(6) Uani 0.8054(16) 1 d P . . C20 C 0.5000 0.7918(7) -0.1199(4) 0.097(3) Uani 0.8054(16) 2 d SP . . C21 C 0.5897(4) 0.6450(6) 0.0141(5) 0.098(3) Uani 0.8054(16) 1 d P . . H21A H 0.5838 0.6116 -0.0380 0.147 Uiso 0.8054(16) 1 calc PR . . H21B H 0.5950 0.5909 0.0550 0.147 Uiso 0.8054(16) 1 calc PR . . H21C H 0.6374 0.6893 0.0141 0.147 Uiso 0.8054(16) 1 calc PR . . C30 C 0.6721(5) 1.0703(7) 0.0869(5) 0.1025(19) Uani 0.8054(16) 1 d P . . C31 C 0.7047(4) 0.8282(5) 0.1514(3) 0.0831(17) Uani 0.8054(16) 1 d P . . H31A H 0.7084 0.8041 0.0963 0.125 Uiso 0.8054(16) 1 calc PR . . H31B H 0.7052 0.7676 0.1871 0.125 Uiso 0.8054(16) 1 calc PR . . H31C H 0.7502 0.8737 0.1634 0.125 Uiso 0.8054(16) 1 calc PR . . C32 C 0.6182(3) 0.9768(5) 0.2610(4) 0.0677(15) Uani 0.8054(16) 1 d P . . H32A H 0.6695 1.0137 0.2625 0.101 Uiso 0.8054(16) 1 calc PR . . H32B H 0.6152 0.9276 0.3056 0.101 Uiso 0.8054(16) 1 calc PR . . H32C H 0.5744 1.0275 0.2650 0.101 Uiso 0.8054(16) 1 calc PR . . Si29 Si 0.5000 0.9630(3) 0.2073(2) 0.0402(11) Uani 0.1946(16) 2 d SP . . Si39 Si 0.60867(18) 0.7832(2) 0.07696(17) 0.0442(9) Uani 0.1946(16) 1 d P . . O29 O 0.5000 1.0528(7) 0.1327(5) 0.040(2) Uani 0.1946(16) 2 d SP . . O39 O 0.6083(4) 0.8781(5) 0.0063(4) 0.0424(17) Uani 0.1946(16) 1 d P . . C209 C 0.5000 1.1596(15) 0.1531(10) 0.058(6) Uani 0.1946(16) 2 d SP . . C219 C 0.5884(12) 0.9970(19) 0.2707(13) 0.047(4) Uani 0.1946(16) 1 d P . . C309 C 0.6732(13) 0.8842(17) -0.0498(13) 0.078(7) Uani 0.1946(16) 1 d P . . C319 C 0.6186(11) 0.650(2) 0.0256(18) 0.049(5) Uani 0.1946(16) 1 d P . . C329 C 0.7040(15) 0.7958(19) 0.1294(14) 0.067(6) Uani 0.1946(16) 1 d P . . H20A H 0.5000 0.847(12) -0.141(10) 0.30(11) Uiso 0.8054(16) 2 d SP . . H20B H 0.539(3) 0.753(4) -0.129(3) 0.13(2) Uiso 0.8054(16) 1 d P . . H30A H 0.667(4) 1.125(4) 0.032(3) 0.09(2) Uiso 0.8054(16) 1 d P . . H30B H 0.675(3) 1.100(4) 0.120(3) 0.10(2) Uiso 0.8054(16) 1 d P . . H30C H 0.715(3) 1.049(5) 0.091(4) 0.14(3) Uiso 0.8054(16) 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 Ca1 0.0614(5) 0.0303(4) 0.0281(4) -0.0050(3) 0.000 0.000 Si1 0.0957(7) 0.0393(5) 0.0387(5) -0.0024(3) 0.000 0.000 Si2 0.1403(12) 0.0317(6) 0.0435(6) -0.0066(4) 0.000 0.000 Si3 0.0801(6) 0.0550(5) 0.0370(4) -0.0014(3) -0.0060(4) 0.0071(4) O2 0.137(3) 0.0336(14) 0.0383(14) -0.0073(11) 0.000 0.000 O3 0.0804(14) 0.0644(12) 0.0473(11) 0.0095(9) -0.0120(10) -0.0138(11) C20 0.200(9) 0.052(4) 0.040(3) -0.018(3) 0.000 0.000 C21 0.177(8) 0.056(3) 0.062(3) -0.007(2) 0.004(5) 0.042(5) C30 0.106(4) 0.118(5) 0.084(4) 0.031(4) -0.033(3) -0.055(4) C31 0.094(3) 0.100(5) 0.056(3) -0.016(3) -0.010(2) 0.021(3) C32 0.091(4) 0.064(3) 0.048(2) -0.0090(19) -0.011(3) 0.009(3) Si29 0.065(3) 0.036(2) 0.0196(17) -0.0032(14) 0.000 0.000 Si39 0.0564(18) 0.0351(15) 0.0410(16) -0.0070(11) -0.0127(12) 0.0146(12) O29 0.067(6) 0.028(5) 0.025(4) -0.008(4) 0.000 0.000 O39 0.037(4) 0.041(4) 0.049(4) 0.000(3) 0.008(3) 0.013(3) C209 0.141(18) 0.019(7) 0.013(6) 0.007(6) 0.000 0.000 C219 0.063(11) 0.049(9) 0.029(7) -0.009(6) -0.023(8) 0.013(8) C309 0.091(12) 0.081(11) 0.061(10) 0.051(9) 0.049(10) 0.052(9) C319 0.044(7) 0.042(8) 0.060(11) -0.026(8) -0.014(6) 0.007(6) C329 0.060(9) 0.075(12) 0.067(13) -0.035(9) -0.032(9) 0.040(8) _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 Ca1 O29 2.335(8) . ? Ca1 O29 2.335(8) 9_675 ? Ca1 O2 2.361(3) . ? Ca1 O2 2.361(3) 9_675 ? Ca1 O39 2.391(6) . ? Ca1 O39 2.391(6) 12_655 ? Ca1 O39 2.391(6) 4_575 ? Ca1 O39 2.391(6) 9_675 ? Ca1 O3 2.394(2) 9_675 ? Ca1 O3 2.394(2) 12_655 ? Ca1 O3 2.394(2) 4_575 ? Ca1 O3 2.394(2) . ? Si1 Si29 2.291(4) . ? Si1 Si2 2.2971(14) . ? Si1 Si3 2.2991(11) 12_655 ? Si1 Si3 2.2991(11) . ? Si1 Si39 2.314(3) 12_655 ? Si1 Si39 2.314(3) . ? Si2 O2 1.705(3) . ? Si2 C21 1.861(7) 12_655 ? Si2 C21 1.861(7) . ? Si2 Si39 2.079(3) 12_655 ? Si2 C319 2.22(2) 12_655 ? Si3 O3 1.704(2) . ? Si3 C32 1.872(6) . ? Si3 C31 1.874(6) . ? O2 C20 1.460(6) . ? O3 C30 1.432(5) . ? C20 C209 0.837(16) 9_675 ? C30 C309 0.853(18) 4_575 ? Si29 O29 1.702(10) . ? Si29 C219 1.88(2) 12_655 ? Si29 C219 1.88(2) . ? Si29 Si3 2.105(2) 12_655 ? Si29 C32 2.181(6) 12_655 ? Si39 O39 1.699(7) . ? Si39 C329 1.83(2) . ? Si39 C319 1.92(3) . ? O29 C209 1.41(2) . ? O39 C309 1.44(2) . ? C209 C20 0.837(16) 9_675 ? C309 C30 0.853(18) 4_575 ? 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 O29 Ca1 O29 180.0 . 9_675 ? O29 Ca1 O2 121.7(2) . . ? O29 Ca1 O2 58.3(2) 9_675 . ? O29 Ca1 O2 58.3(2) . 9_675 ? O29 Ca1 O2 121.7(2) 9_675 9_675 ? O2 Ca1 O2 180.0 . 9_675 ? O29 Ca1 O39 98.4(2) . . ? O29 Ca1 O39 81.6(2) 9_675 . ? O2 Ca1 O39 51.85(17) . . ? O2 Ca1 O39 128.15(17) 9_675 . ? O29 Ca1 O39 98.4(2) . 12_655 ? O29 Ca1 O39 81.6(2) 9_675 12_655 ? O2 Ca1 O39 51.85(17) . 12_655 ? O2 Ca1 O39 128.15(17) 9_675 12_655 ? O39 Ca1 O39 98.5(3) . 12_655 ? O29 Ca1 O39 81.6(2) . 4_575 ? O29 Ca1 O39 98.4(2) 9_675 4_575 ? O2 Ca1 O39 128.15(17) . 4_575 ? O2 Ca1 O39 51.85(17) 9_675 4_575 ? O39 Ca1 O39 81.5(3) . 4_575 ? O39 Ca1 O39 180.000(1) 12_655 4_575 ? O29 Ca1 O39 81.6(2) . 9_675 ? O29 Ca1 O39 98.4(2) 9_675 9_675 ? O2 Ca1 O39 128.15(17) . 9_675 ? O2 Ca1 O39 51.85(17) 9_675 9_675 ? O39 Ca1 O39 179.999(1) . 9_675 ? O39 Ca1 O39 81.5(3) 12_655 9_675 ? O39 Ca1 O39 98.5(3) 4_575 9_675 ? O29 Ca1 O3 128.10(8) . 9_675 ? O29 Ca1 O3 51.90(8) 9_675 9_675 ? O2 Ca1 O3 81.64(6) . 9_675 ? O2 Ca1 O3 98.36(6) 9_675 9_675 ? O39 Ca1 O3 128.21(18) . 9_675 ? O39 Ca1 O3 57.95(18) 12_655 9_675 ? O39 Ca1 O3 122.05(18) 4_575 9_675 ? O39 Ca1 O3 51.79(18) 9_675 9_675 ? O29 Ca1 O3 51.90(8) . 12_655 ? O29 Ca1 O3 128.10(8) 9_675 12_655 ? O2 Ca1 O3 98.36(6) . 12_655 ? O2 Ca1 O3 81.64(6) 9_675 12_655 ? O39 Ca1 O3 122.05(18) . 12_655 ? O39 Ca1 O3 51.79(18) 12_655 12_655 ? O39 Ca1 O3 128.21(18) 4_575 12_655 ? O39 Ca1 O3 57.95(18) 9_675 12_655 ? O3 Ca1 O3 81.38(10) 9_675 12_655 ? O29 Ca1 O3 128.10(8) . 4_575 ? O29 Ca1 O3 51.90(8) 9_675 4_575 ? O2 Ca1 O3 81.64(6) . 4_575 ? O2 Ca1 O3 98.36(6) 9_675 4_575 ? O39 Ca1 O3 57.95(18) . 4_575 ? O39 Ca1 O3 128.21(18) 12_655 4_575 ? O39 Ca1 O3 51.79(18) 4_575 4_575 ? O39 Ca1 O3 122.05(18) 9_675 4_575 ? O3 Ca1 O3 98.62(10) 9_675 4_575 ? O3 Ca1 O3 180.00(9) 12_655 4_575 ? O29 Ca1 O3 51.90(8) . . ? O29 Ca1 O3 128.10(8) 9_675 . ? O2 Ca1 O3 98.36(6) . . ? O2 Ca1 O3 81.64(6) 9_675 . ? O39 Ca1 O3 51.79(18) . . ? O39 Ca1 O3 122.05(18) 12_655 . ? O39 Ca1 O3 57.95(18) 4_575 . ? O39 Ca1 O3 128.21(18) 9_675 . ? O3 Ca1 O3 180.0 9_675 . ? O3 Ca1 O3 98.63(10) 12_655 . ? O3 Ca1 O3 81.37(10) 4_575 . ? Si29 Si1 Si2 131.68(10) . . ? Si29 Si1 Si3 54.60(3) . 12_655 ? Si2 Si1 Si3 104.64(3) . 12_655 ? Si29 Si1 Si3 54.60(3) . . ? Si2 Si1 Si3 104.64(3) . . ? Si3 Si1 Si3 105.42(6) 12_655 . ? Si29 Si1 Si39 105.29(9) . 12_655 ? Si2 Si1 Si39 53.60(7) . 12_655 ? Si3 Si1 Si39 55.14(7) 12_655 12_655 ? Si3 Si1 Si39 132.72(8) . 12_655 ? Si29 Si1 Si39 105.29(9) . . ? Si2 Si1 Si39 53.60(7) . . ? Si3 Si1 Si39 132.72(8) 12_655 . ? Si3 Si1 Si39 55.14(7) . . ? Si39 Si1 Si39 103.55(14) 12_655 . ? O2 Si2 C21 105.2(3) . 12_655 ? O2 Si2 C21 105.2(3) . . ? C21 Si2 C21 107.4(5) 12_655 . ? O2 Si2 Si39 89.56(10) . 12_655 ? C21 Si2 Si39 63.5(2) 12_655 12_655 ? C21 Si2 Si39 164.6(3) . 12_655 ? O2 Si2 C319 105.2(9) . 12_655 ? C21 Si2 C319 10.9(7) 12_655 12_655 ? C21 Si2 C319 117.4(5) . 12_655 ? Si39 Si2 C319 52.8(6) 12_655 12_655 ? O2 Si2 Si1 112.80(10) . . ? C21 Si2 Si1 112.8(2) 12_655 . ? C21 Si2 Si1 112.8(2) . . ? Si39 Si2 Si1 63.62(8) 12_655 . ? C319 Si2 Si1 103.4(7) 12_655 . ? O3 Si3 C32 105.7(2) . . ? O3 Si3 C31 105.7(2) . . ? C32 Si3 C31 107.3(2) . . ? O3 Si3 Si1 113.18(8) . . ? C32 Si3 Si1 113.0(2) . . ? C31 Si3 Si1 111.4(2) . . ? C20 O2 Si2 119.8(4) . . ? C20 O2 Ca1 119.9(4) . . ? Si2 O2 Ca1 120.24(13) . . ? C30 O3 Si3 120.3(3) . . ? C30 O3 Ca1 120.3(3) . . ? Si3 O3 Ca1 119.42(10) . . ? C209 C20 O2 117.0(12) 9_675 . ? C309 C30 O3 121.2(12) 4_575 . ? O29 Si29 C219 105.3(8) . 12_655 ? O29 Si29 C219 105.3(8) . . ? C219 Si29 C219 104.1(12) 12_655 . ? O29 Si29 Si3 89.83(18) . 12_655 ? C219 Si29 Si3 65.8(5) 12_655 12_655 ? C219 Si29 Si3 163.9(8) . 12_655 ? O29 Si29 C32 104.6(2) . 12_655 ? C219 Si29 C32 14.2(6) 12_655 12_655 ? C219 Si29 C32 117.4(6) . 12_655 ? Si3 Si29 C32 51.75(13) 12_655 12_655 ? O29 Si29 Si1 112.7(3) . . ? C219 Si29 Si1 114.2(6) 12_655 . ? C219 Si29 Si1 114.2(6) . . ? Si3 Si29 Si1 62.89(9) 12_655 . ? C32 Si29 Si1 102.44(18) 12_655 . ? O39 Si39 C329 106.2(11) . . ? O39 Si39 C319 108.5(10) . . ? C329 Si39 C319 102.7(8) . . ? O39 Si39 Si1 112.7(3) . . ? C329 Si39 Si1 112.4(8) . . ? C319 Si39 Si1 113.5(8) . . ? C209 O29 Si29 118.2(9) . . ? C209 O29 Ca1 121.0(9) . . ? Si29 O29 Ca1 120.9(5) . . ? C309 O39 Si39 119.7(9) . . ? C309 O39 Ca1 120.5(8) . . ? Si39 O39 Ca1 119.9(4) . . ? C20 C209 O29 123.8(15) 9_675 . ? C30 C309 O39 120.0(17) 4_575 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.66 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.265 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.040 # Attachment '2010060201BRWCK_0m.cif' data_2010060201brwck_0m _database_code_depnum_ccdc_archive 'CCDC 829367' #TrackingRef '2010060201BRWCK_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 Ba O6 Si8' _chemical_formula_weight 728.62876 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 21.499(5) _cell_length_b 17.291(4) _cell_length_c 26.008(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.524(2) _cell_angle_gamma 90.00 _cell_volume 9506(4) _cell_formula_units_Z 10 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelipiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3780 _exptl_absorpt_coefficient_mu 1.525 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5877 _exptl_absorpt_correction_T_max 0.6980 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 113473 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 28.83 _reflns_number_total 23539 _reflns_number_gt 16807 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0591P)^2^+28.5851P] 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_extinction_coef ? _refine_ls_number_reflns 23539 _refine_ls_number_parameters 790 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.003 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 Ba1 Ba 1.0000 0.0000 1.0000 0.02258(7) Uani 1 2 d S . . Si11 Si 0.88074(5) 0.16226(6) 0.98378(5) 0.0382(3) Uani 1 1 d . . . Si12 Si 0.98173(6) 0.21010(6) 1.01501(5) 0.0350(3) Uani 1 1 d . . . Si13 Si 0.88081(6) 0.10552(7) 0.90418(5) 0.0415(3) Uani 1 1 d . . . Si14 Si 0.85230(6) 0.07003(7) 1.03970(5) 0.0411(3) Uani 1 1 d . . . O12 O 1.03667(14) 0.14017(16) 1.03212(14) 0.0482(8) Uani 1 1 d . . . O13 O 0.93974(16) 0.0395(2) 0.90460(12) 0.0541(9) Uani 1 1 d . . . O14 O 0.89886(15) -0.00950(17) 1.04653(14) 0.0511(9) Uani 1 1 d . . . C12 C 1.1011(3) 0.1557(3) 1.0573(3) 0.088(2) Uani 1 1 d . . . H12A H 1.1175 0.1998 1.0401 0.132 Uiso 1 1 calc R . . H12B H 1.1273 0.1101 1.0546 0.132 Uiso 1 1 calc R . . H12C H 1.1022 0.1680 1.0942 0.132 Uiso 1 1 calc R . . C13 C 0.9502(4) 0.0027(4) 0.8575(2) 0.098(3) Uani 1 1 d . . . H13A H 0.9099 -0.0164 0.8379 0.147 Uiso 1 1 calc R . . H13B H 0.9795 -0.0407 0.8664 0.147 Uiso 1 1 calc R . . H13C H 0.9684 0.0401 0.8361 0.147 Uiso 1 1 calc R . . C14 C 0.8877(3) -0.0747(3) 1.0782(3) 0.088(2) Uani 1 1 d . . . H14D H 0.8799 -0.0564 1.1121 0.132 Uiso 1 1 calc R . . H14E H 0.9249 -0.1086 1.0836 0.132 Uiso 1 1 calc R . . H14F H 0.8508 -0.1036 1.0603 0.132 Uiso 1 1 calc R . . C121 C 1.0116(2) 0.2711(3) 0.9653(2) 0.0511(12) Uani 1 1 d . . . H12D H 1.0532 0.2923 0.9806 0.077 Uiso 1 1 calc R . . H12E H 0.9820 0.3136 0.9545 0.077 Uiso 1 1 calc R . . H12F H 1.0154 0.2394 0.9348 0.077 Uiso 1 1 calc R . . C122 C 0.9843(3) 0.2708(3) 1.0745(2) 0.0637(15) Uani 1 1 d . . . H12G H 0.9729 0.2392 1.1027 0.095 Uiso 1 1 calc R . . H12H H 0.9543 0.3137 1.0666 0.095 Uiso 1 1 calc R . . H12I H 1.0271 0.2914 1.0856 0.095 Uiso 1 1 calc R . . C131 C 0.8052(3) 0.0520(3) 0.8782(2) 0.0664(16) Uani 1 1 d . . . H13D H 0.8070 0.0312 0.8435 0.100 Uiso 1 1 calc R . . H13E H 0.7693 0.0875 0.8758 0.100 Uiso 1 1 calc R . . H13F H 0.8000 0.0094 0.9019 0.100 Uiso 1 1 calc R . . C132 C 0.8930(3) 0.1792(3) 0.8539(2) 0.0636(15) Uani 1 1 d . . . H13G H 0.9318 0.2085 0.8667 0.095 Uiso 1 1 calc R . . H13H H 0.8568 0.2146 0.8476 0.095 Uiso 1 1 calc R . . H13I H 0.8969 0.1529 0.8213 0.095 Uiso 1 1 calc R . . C141 C 0.8548(3) 0.1091(4) 1.1069(2) 0.083(2) Uani 1 1 d . . . H14A H 0.8386 0.0700 1.1284 0.124 Uiso 1 1 calc R . . H14B H 0.8285 0.1557 1.1051 0.124 Uiso 1 1 calc R . . H14C H 0.8985 0.1220 1.1226 0.124 Uiso 1 1 calc R . . C142 C 0.7695(2) 0.0332(4) 1.0152(3) 0.0729(18) Uani 1 1 d . . . H14G H 0.7676 0.0083 0.9812 0.109 Uiso 1 1 calc R . . H14H H 0.7397 0.0767 1.0117 0.109 Uiso 1 1 calc R . . H14I H 0.7581 -0.0043 1.0402 0.109 Uiso 1 1 calc R . . Ba2 Ba 0.591117(10) 0.001999(12) 0.208043(8) 0.02405(6) Uani 1 1 d . . . Si21 Si 0.70895(5) -0.15918(6) 0.24441(5) 0.0339(2) Uani 1 1 d . . . Si22 Si 0.75860(5) -0.04118(7) 0.26245(5) 0.0406(3) Uani 1 1 d . . . Si23 Si 0.62999(5) -0.17053(6) 0.29324(4) 0.0334(2) Uani 1 1 d . . . Si24 Si 0.66659(6) -0.16642(7) 0.15654(5) 0.0369(3) Uani 1 1 d . . . Si25 Si 0.46874(5) 0.16394(6) 0.17145(5) 0.0342(2) Uani 1 1 d . . . Si26 Si 0.51255(6) 0.17147(7) 0.25907(5) 0.0410(3) Uani 1 1 d . . . Si27 Si 0.41970(5) 0.04489(7) 0.15628(5) 0.0415(3) Uani 1 1 d . . . Si28 Si 0.54689(6) 0.17250(7) 0.12166(5) 0.0374(3) Uani 1 1 d . . . O22 O 0.71299(14) 0.03578(17) 0.23927(15) 0.0538(9) Uani 1 1 d . . . O23 O 0.57651(15) -0.09721(18) 0.28426(12) 0.0469(8) Uani 1 1 d . . . O24 O 0.60739(17) -0.1016(2) 0.13569(12) 0.0552(9) Uani 1 1 d . . . O26 O 0.57433(18) 0.1108(2) 0.27761(13) 0.0636(11) Uani 1 1 d . . . O27 O 0.46933(14) -0.03062(17) 0.17434(15) 0.0530(9) Uani 1 1 d . . . O28 O 0.60089(17) 0.10022(19) 0.13121(14) 0.0579(10) Uani 1 1 d . . . C22 C 0.7369(3) 0.1142(3) 0.2437(3) 0.093(3) Uani 1 1 d . . . H22D H 0.7498 0.1277 0.2807 0.139 Uiso 1 1 calc R . . H22E H 0.7037 0.1497 0.2271 0.139 Uiso 1 1 calc R . . H22F H 0.7734 0.1182 0.2261 0.139 Uiso 1 1 calc R . . C23 C 0.5252(3) -0.0928(4) 0.3125(3) 0.080(2) Uani 1 1 d . . . H23D H 0.4991 -0.1395 0.3057 0.120 Uiso 1 1 calc R . . H23E H 0.4994 -0.0472 0.3010 0.120 Uiso 1 1 calc R . . H23F H 0.5421 -0.0888 0.3500 0.120 Uiso 1 1 calc R . . C24 C 0.5729(4) -0.1028(4) 0.0832(2) 0.108(3) Uani 1 1 d . . . H24D H 0.6026 -0.1041 0.0588 0.162 Uiso 1 1 calc R . . H24E H 0.5466 -0.0562 0.0768 0.162 Uiso 1 1 calc R . . H24F H 0.5458 -0.1487 0.0781 0.162 Uiso 1 1 calc R . . C26 C 0.6111(4) 0.1119(5) 0.3293(2) 0.125(4) Uani 1 1 d . . . H26A H 0.5836 0.1021 0.3547 0.188 Uiso 1 1 calc R . . H26B H 0.6313 0.1626 0.3361 0.188 Uiso 1 1 calc R . . H26C H 0.6438 0.0717 0.3324 0.188 Uiso 1 1 calc R . . C27 C 0.4487(3) -0.1097(3) 0.1698(3) 0.087(2) Uani 1 1 d . . . H27D H 0.4211 -0.1200 0.1951 0.130 Uiso 1 1 calc R . . H27E H 0.4856 -0.1440 0.1768 0.130 Uiso 1 1 calc R . . H27F H 0.4253 -0.1191 0.1343 0.130 Uiso 1 1 calc R . . C28 C 0.6520(3) 0.0954(4) 0.1024(3) 0.099(3) Uani 1 1 d . . . H28A H 0.6347 0.0928 0.0649 0.149 Uiso 1 1 calc R . . H28B H 0.6771 0.0489 0.1130 0.149 Uiso 1 1 calc R . . H28C H 0.6790 0.1412 0.1097 0.149 Uiso 1 1 calc R . . C221 C 0.7830(3) -0.0247(3) 0.3344(2) 0.0609(14) Uani 1 1 d . . . H22A H 0.8075 0.0233 0.3404 0.091 Uiso 1 1 calc R . . H22B H 0.8089 -0.0682 0.3501 0.091 Uiso 1 1 calc R . . H22C H 0.7452 -0.0204 0.3504 0.091 Uiso 1 1 calc R . . C222 C 0.8307(2) -0.0341(4) 0.2324(3) 0.0739(18) Uani 1 1 d . . . H22G H 0.8185 -0.0368 0.1942 0.111 Uiso 1 1 calc R . . H22H H 0.8593 -0.0770 0.2447 0.111 Uiso 1 1 calc R . . H22I H 0.8521 0.0151 0.2423 0.111 Uiso 1 1 calc R . . C231 C 0.5830(2) -0.2612(3) 0.27731(19) 0.0478(11) Uani 1 1 d . . . H23A H 0.5525 -0.2663 0.3009 0.072 Uiso 1 1 calc R . . H23B H 0.6116 -0.3058 0.2817 0.072 Uiso 1 1 calc R . . H23C H 0.5604 -0.2589 0.2410 0.072 Uiso 1 1 calc R . . C232 C 0.6647(2) -0.1701(3) 0.36502(17) 0.0508(12) Uani 1 1 d . . . H23G H 0.6789 -0.1177 0.3758 0.076 Uiso 1 1 calc R . . H23H H 0.7007 -0.2057 0.3718 0.076 Uiso 1 1 calc R . . H23I H 0.6325 -0.1867 0.3849 0.076 Uiso 1 1 calc R . . C241 C 0.7289(3) -0.1462(3) 0.1165(2) 0.0623(15) Uani 1 1 d . . . H24A H 0.7109 -0.1529 0.0793 0.093 Uiso 1 1 calc R . . H24B H 0.7643 -0.1822 0.1265 0.093 Uiso 1 1 calc R . . H24C H 0.7441 -0.0930 0.1228 0.093 Uiso 1 1 calc R . . C242 C 0.6311(2) -0.2636(3) 0.1376(2) 0.0515(12) Uani 1 1 d . . . H24G H 0.5926 -0.2701 0.1524 0.077 Uiso 1 1 calc R . . H24H H 0.6616 -0.3041 0.1512 0.077 Uiso 1 1 calc R . . H24I H 0.6206 -0.2674 0.0994 0.077 Uiso 1 1 calc R . . C261 C 0.5435(3) 0.2706(3) 0.2784(2) 0.0685(16) Uani 1 1 d . . . H26D H 0.5592 0.2721 0.3162 0.103 Uiso 1 1 calc R . . H26E H 0.5094 0.3085 0.2691 0.103 Uiso 1 1 calc R . . H26F H 0.5780 0.2831 0.2599 0.103 Uiso 1 1 calc R . . C262 C 0.4542(3) 0.1451(3) 0.3017(2) 0.0709(17) Uani 1 1 d . . . H26G H 0.4447 0.0898 0.2982 0.106 Uiso 1 1 calc R . . H26H H 0.4152 0.1749 0.2909 0.106 Uiso 1 1 calc R . . H26I H 0.4722 0.1570 0.3382 0.106 Uiso 1 1 calc R . . C271 C 0.3533(2) 0.0324(3) 0.1937(3) 0.0689(17) Uani 1 1 d . . . H27A H 0.3311 -0.0162 0.1833 0.103 Uiso 1 1 calc R . . H27B H 0.3237 0.0757 0.1861 0.103 Uiso 1 1 calc R . . H27C H 0.3706 0.0311 0.2313 0.103 Uiso 1 1 calc R . . C272 C 0.3854(3) 0.0289(4) 0.0857(2) 0.0704(17) Uani 1 1 d . . . H27G H 0.4196 0.0263 0.0655 0.106 Uiso 1 1 calc R . . H27H H 0.3570 0.0718 0.0728 0.106 Uiso 1 1 calc R . . H27I H 0.3616 -0.0198 0.0818 0.106 Uiso 1 1 calc R . . C281 C 0.5946(2) 0.2631(3) 0.1339(2) 0.0527(13) Uani 1 1 d . . . H28D H 0.6164 0.2643 0.1704 0.079 Uiso 1 1 calc R . . H28E H 0.5665 0.3080 0.1268 0.079 Uiso 1 1 calc R . . H28F H 0.6259 0.2645 0.1108 0.079 Uiso 1 1 calc R . . C282 C 0.5104(3) 0.1673(3) 0.05021(19) 0.0645(15) Uani 1 1 d . . . H28P H 0.5433 0.1744 0.0291 0.097 Uiso 1 1 calc R . . H28Q H 0.4785 0.2081 0.0418 0.097 Uiso 1 1 calc R . . H28R H 0.4903 0.1167 0.0425 0.097 Uiso 1 1 calc R . . Ba3 Ba 0.194405(9) 0.007726(12) 0.401063(8) 0.02211(6) Uani 1 1 d . . . Si31 Si 0.31573(5) -0.14241(6) 0.44294(4) 0.0287(2) Uani 1 1 d . . . Si32 Si 0.23462(5) -0.16003(7) 0.48874(4) 0.0332(2) Uani 1 1 d . . . Si33 Si 0.36149(5) -0.02223(6) 0.46035(5) 0.0337(2) Uani 1 1 d . . . Si34 Si 0.27862(5) -0.15641(6) 0.35468(4) 0.0330(2) Uani 1 1 d . . . Si35 Si 0.07171(5) 0.16337(6) 0.35949(4) 0.0282(2) Uani 1 1 d . . . Si36 Si 0.11085(5) 0.17366(6) 0.44771(4) 0.0330(2) Uani 1 1 d . . . Si37 Si 0.02618(5) 0.04272(7) 0.34240(5) 0.0338(2) Uani 1 1 d . . . Si38 Si 0.15189(5) 0.17455(6) 0.31189(4) 0.0322(2) Uani 1 1 d . . . O32 O 0.17723(15) -0.0914(2) 0.47640(13) 0.0516(9) Uani 1 1 d . . . O33 O 0.31226(14) 0.05173(16) 0.43804(15) 0.0512(9) Uani 1 1 d . . . O34 O 0.21825(16) -0.0958(2) 0.33093(12) 0.0535(9) Uani 1 1 d . . . O36 O 0.17026(17) 0.1117(2) 0.47069(12) 0.0593(10) Uani 1 1 d . . . O37 O 0.07590(13) -0.03161(16) 0.36356(14) 0.0488(9) Uani 1 1 d . . . O38 O 0.20507(17) 0.10139(19) 0.32132(14) 0.0575(10) Uani 1 1 d . . . C32 C 0.1240(3) -0.0911(4) 0.5024(3) 0.096(3) Uani 1 1 d . . . H32A H 0.1006 -0.1397 0.4952 0.145 Uiso 1 1 calc R . . H32B H 0.0962 -0.0476 0.4896 0.145 Uiso 1 1 calc R . . H32C H 0.1387 -0.0857 0.5402 0.145 Uiso 1 1 calc R . . C33 C 0.3319(3) 0.1313(3) 0.4449(3) 0.090(3) Uani 1 1 d . . . H33A H 0.3511 0.1402 0.4816 0.135 Uiso 1 1 calc R . . H33B H 0.2950 0.1651 0.4352 0.135 Uiso 1 1 calc R . . H33C H 0.3628 0.1426 0.4226 0.135 Uiso 1 1 calc R . . C34 C 0.1858(4) -0.1010(5) 0.2778(2) 0.107(3) Uani 1 1 d . . . H34A H 0.1570 -0.0569 0.2697 0.160 Uiso 1 1 calc R . . H34B H 0.1614 -0.1492 0.2729 0.160 Uiso 1 1 calc R . . H34C H 0.2166 -0.1006 0.2543 0.160 Uiso 1 1 calc R . . C36 C 0.2020(4) 0.1125(5) 0.5243(2) 0.119(4) Uani 1 1 d . . . H36A H 0.2302 0.1575 0.5303 0.178 Uiso 1 1 calc R . . H36B H 0.2268 0.0651 0.5320 0.178 Uiso 1 1 calc R . . H36C H 0.1706 0.1157 0.5472 0.178 Uiso 1 1 calc R . . C37 C 0.0568(3) -0.1116(3) 0.3582(3) 0.087(2) Uani 1 1 d . . . H37D H 0.0243 -0.1216 0.3794 0.131 Uiso 1 1 calc R . . H37E H 0.0935 -0.1449 0.3702 0.131 Uiso 1 1 calc R . . H37F H 0.0395 -0.1228 0.3215 0.131 Uiso 1 1 calc R . . C38 C 0.2576(3) 0.0977(4) 0.2942(3) 0.105(3) Uani 1 1 d . . . H38A H 0.2420 0.0866 0.2571 0.157 Uiso 1 1 calc R . . H38B H 0.2866 0.0567 0.3094 0.157 Uiso 1 1 calc R . . H38C H 0.2799 0.1474 0.2976 0.157 Uiso 1 1 calc R . . C321 C 0.1938(3) -0.2547(3) 0.4735(2) 0.0566(14) Uani 1 1 d . . . H32D H 0.1629 -0.2623 0.4965 0.085 Uiso 1 1 calc R . . H32E H 0.2251 -0.2965 0.4791 0.085 Uiso 1 1 calc R . . H32F H 0.1721 -0.2550 0.4370 0.085 Uiso 1 1 calc R . . C322 C 0.2651(3) -0.1556(3) 0.56090(17) 0.0545(13) Uani 1 1 d . . . H32G H 0.2811 -0.1035 0.5704 0.082 Uiso 1 1 calc R . . H32H H 0.2993 -0.1932 0.5704 0.082 Uiso 1 1 calc R . . H32I H 0.2307 -0.1677 0.5797 0.082 Uiso 1 1 calc R . . C331 C 0.4328(2) -0.0100(3) 0.4296(2) 0.0592(14) Uani 1 1 d . . . H33D H 0.4199 -0.0082 0.3915 0.089 Uiso 1 1 calc R . . H33E H 0.4617 -0.0536 0.4393 0.089 Uiso 1 1 calc R . . H33F H 0.4543 0.0384 0.4418 0.089 Uiso 1 1 calc R . . C332 C 0.3867(2) -0.0059(3) 0.5324(2) 0.0543(13) Uani 1 1 d . . . H33G H 0.4108 0.0424 0.5383 0.081 Uiso 1 1 calc R . . H33H H 0.4133 -0.0491 0.5477 0.081 Uiso 1 1 calc R . . H33I H 0.3492 -0.0025 0.5488 0.081 Uiso 1 1 calc R . . C341 C 0.3423(3) -0.1349(3) 0.31652(19) 0.0540(13) Uani 1 1 d . . . H34P H 0.3268 -0.1458 0.2794 0.081 Uiso 1 1 calc R . . H32Q H 0.3793 -0.1674 0.3293 0.081 Uiso 1 1 calc R . . H30R H 0.3543 -0.0803 0.3208 0.081 Uiso 1 1 calc R . . C342 C 0.2475(2) -0.2560(3) 0.3377(2) 0.0513(12) Uani 1 1 d . . . H34D H 0.2075 -0.2630 0.3501 0.077 Uiso 1 1 calc R . . H34E H 0.2783 -0.2943 0.3545 0.077 Uiso 1 1 calc R . . H34F H 0.2405 -0.2630 0.2997 0.077 Uiso 1 1 calc R . . C361 C 0.1434(2) 0.2721(3) 0.4663(2) 0.0521(12) Uani 1 1 d . . . H36D H 0.1571 0.2748 0.5044 0.078 Uiso 1 1 calc R . . H36E H 0.1106 0.3111 0.4552 0.078 Uiso 1 1 calc R . . H36F H 0.1796 0.2821 0.4492 0.078 Uiso 1 1 calc R . . C362 C 0.0468(3) 0.1516(3) 0.48593(19) 0.0552(13) Uani 1 1 d . . . H36G H 0.0347 0.0970 0.4813 0.083 Uiso 1 1 calc R . . H36H H 0.0099 0.1842 0.4733 0.083 Uiso 1 1 calc R . . H36I H 0.0623 0.1621 0.5231 0.083 Uiso 1 1 calc R . . C371 C 0.0007(2) 0.0260(3) 0.2704(2) 0.0566(13) Uani 1 1 d . . . H37A H 0.0378 0.0276 0.2534 0.085 Uiso 1 1 calc R . . H37B H -0.0292 0.0664 0.2556 0.085 Uiso 1 1 calc R . . H37C H -0.0197 -0.0247 0.2645 0.085 Uiso 1 1 calc R . . C372 C -0.0437(2) 0.0273(3) 0.3744(2) 0.0610(15) Uani 1 1 d . . . H21G H -0.0649 -0.0210 0.3617 0.092 Uiso 1 1 calc R . . H19G H -0.0733 0.0706 0.3660 0.092 Uiso 1 1 calc R . . H17G H -0.0297 0.0242 0.4124 0.092 Uiso 1 1 calc R . . C381 C 0.1182(3) 0.1757(3) 0.24014(18) 0.0574(14) Uani 1 1 d . . . H28G H 0.1523 0.1842 0.2204 0.086 Uiso 1 1 calc R . . H26X H 0.0871 0.2175 0.2326 0.086 Uiso 1 1 calc R . . H24X H 0.0976 0.1261 0.2299 0.086 Uiso 1 1 calc R . . C382 C 0.2000(2) 0.2638(3) 0.32753(19) 0.0445(11) Uani 1 1 d . . . H38D H 0.2212 0.2624 0.3642 0.067 Uiso 1 1 calc R . . H38E H 0.1724 0.3093 0.3216 0.067 Uiso 1 1 calc R . . H38F H 0.2318 0.2668 0.3050 0.067 Uiso 1 1 calc R . . 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 Ba1 0.02202(14) 0.01678(13) 0.02884(15) -0.00192(11) 0.00436(11) -0.00050(11) Si11 0.0307(6) 0.0257(5) 0.0590(8) 0.0033(5) 0.0104(5) 0.0005(4) Si12 0.0385(6) 0.0218(5) 0.0448(7) -0.0039(5) 0.0077(5) -0.0026(4) Si13 0.0373(7) 0.0415(7) 0.0407(7) 0.0089(5) -0.0065(5) -0.0070(5) Si14 0.0377(6) 0.0337(6) 0.0579(8) -0.0016(5) 0.0244(6) 0.0010(5) O12 0.0381(17) 0.0223(14) 0.076(2) -0.0047(14) -0.0104(16) -0.0027(12) O13 0.063(2) 0.066(2) 0.0303(16) -0.0088(15) 0.0016(15) 0.0152(18) O14 0.0519(19) 0.0355(16) 0.076(2) 0.0172(16) 0.0386(18) 0.0102(14) C12 0.052(3) 0.040(3) 0.147(6) -0.001(3) -0.047(4) -0.010(2) C13 0.123(6) 0.127(6) 0.039(3) -0.031(4) 0.002(3) 0.030(5) C14 0.102(5) 0.053(3) 0.129(6) 0.043(4) 0.078(5) 0.021(3) C121 0.037(2) 0.046(3) 0.069(3) 0.012(2) 0.007(2) -0.010(2) C122 0.085(4) 0.046(3) 0.064(4) -0.024(3) 0.024(3) -0.010(3) C131 0.058(3) 0.065(4) 0.065(4) 0.013(3) -0.018(3) -0.020(3) C132 0.071(4) 0.066(3) 0.047(3) 0.018(3) -0.008(3) -0.022(3) C141 0.124(6) 0.069(4) 0.070(4) -0.015(3) 0.052(4) -0.010(4) C142 0.043(3) 0.070(4) 0.113(5) 0.018(4) 0.031(3) -0.008(3) Ba2 0.02341(10) 0.02167(11) 0.02653(11) 0.00278(8) 0.00311(8) 0.00022(8) Si21 0.0290(6) 0.0302(6) 0.0421(6) 0.0022(5) 0.0054(5) 0.0007(4) Si22 0.0234(5) 0.0393(6) 0.0559(8) 0.0018(6) -0.0013(5) -0.0046(5) Si23 0.0368(6) 0.0305(6) 0.0325(6) 0.0079(5) 0.0051(5) -0.0015(5) Si24 0.0448(7) 0.0313(6) 0.0374(6) -0.0069(5) 0.0145(5) 0.0021(5) Si25 0.0318(6) 0.0279(5) 0.0428(7) 0.0052(5) 0.0060(5) 0.0016(4) Si26 0.0530(8) 0.0310(6) 0.0413(7) -0.0042(5) 0.0150(6) 0.0075(5) Si27 0.0236(6) 0.0386(6) 0.0592(8) 0.0043(6) -0.0007(5) -0.0041(5) Si28 0.0413(7) 0.0331(6) 0.0386(6) 0.0136(5) 0.0098(5) 0.0030(5) O22 0.0313(16) 0.0284(15) 0.094(3) 0.0042(16) -0.0105(17) -0.0080(13) O23 0.0494(19) 0.0474(18) 0.0516(19) 0.0223(15) 0.0294(16) 0.0141(15) O24 0.074(2) 0.055(2) 0.0317(17) -0.0099(15) -0.0032(16) 0.0240(18) O26 0.081(3) 0.069(2) 0.0330(18) -0.0125(16) -0.0091(17) 0.039(2) O27 0.0293(16) 0.0292(16) 0.093(3) 0.0059(16) -0.0085(16) -0.0074(12) O28 0.068(2) 0.051(2) 0.067(2) 0.0302(17) 0.0453(19) 0.0226(17) C22 0.061(4) 0.037(3) 0.164(7) 0.009(4) -0.022(4) -0.024(3) C23 0.077(4) 0.085(4) 0.094(5) 0.047(4) 0.059(4) 0.031(3) C24 0.147(7) 0.116(6) 0.042(3) -0.027(4) -0.033(4) 0.066(5) C26 0.167(8) 0.148(7) 0.038(3) -0.032(4) -0.039(4) 0.092(6) C27 0.062(4) 0.034(3) 0.152(7) 0.005(3) -0.013(4) -0.020(3) C28 0.112(5) 0.093(5) 0.121(6) 0.055(4) 0.095(5) 0.050(4) C221 0.053(3) 0.063(3) 0.060(3) -0.007(3) -0.007(3) -0.015(3) C222 0.037(3) 0.083(4) 0.106(5) 0.003(4) 0.024(3) -0.016(3) C231 0.049(3) 0.048(3) 0.045(3) 0.009(2) 0.005(2) -0.013(2) C232 0.064(3) 0.053(3) 0.034(2) 0.006(2) 0.004(2) -0.011(2) C241 0.083(4) 0.053(3) 0.061(3) -0.013(3) 0.041(3) -0.015(3) C242 0.057(3) 0.042(3) 0.060(3) -0.019(2) 0.019(3) -0.007(2) C261 0.092(5) 0.044(3) 0.068(4) -0.018(3) 0.010(3) -0.010(3) C262 0.108(5) 0.056(3) 0.061(4) -0.010(3) 0.048(3) -0.003(3) C271 0.042(3) 0.067(4) 0.102(5) 0.002(3) 0.021(3) -0.015(3) C272 0.059(4) 0.072(4) 0.068(4) -0.005(3) -0.020(3) -0.015(3) C281 0.047(3) 0.045(3) 0.069(3) 0.016(2) 0.018(3) -0.003(2) C282 0.078(4) 0.075(4) 0.040(3) 0.016(3) 0.009(3) -0.018(3) Ba3 0.01893(10) 0.02253(10) 0.02500(11) -0.00078(8) 0.00433(8) 0.00022(8) Si31 0.0247(5) 0.0262(5) 0.0340(6) 0.0000(4) 0.0018(4) 0.0010(4) Si32 0.0346(6) 0.0331(6) 0.0316(6) 0.0092(5) 0.0057(5) -0.0028(5) Si33 0.0194(5) 0.0295(5) 0.0492(7) -0.0012(5) -0.0020(5) -0.0021(4) Si34 0.0350(6) 0.0322(6) 0.0325(6) -0.0092(5) 0.0080(5) 0.0056(5) Si35 0.0239(5) 0.0267(5) 0.0342(6) -0.0025(4) 0.0056(4) 0.0006(4) Si36 0.0352(6) 0.0327(6) 0.0326(6) -0.0095(5) 0.0099(5) 0.0063(5) Si37 0.0186(5) 0.0320(6) 0.0490(7) -0.0046(5) 0.0013(5) -0.0027(4) Si38 0.0369(6) 0.0272(5) 0.0351(6) 0.0068(4) 0.0138(5) 0.0031(4) O32 0.0470(19) 0.059(2) 0.057(2) 0.0262(17) 0.0328(16) 0.0154(16) O33 0.0280(15) 0.0252(15) 0.091(3) 0.0005(16) -0.0129(16) -0.0049(12) O34 0.063(2) 0.061(2) 0.0300(16) -0.0166(15) -0.0075(15) 0.0298(18) O36 0.070(2) 0.070(2) 0.0314(17) -0.0178(16) -0.0097(16) 0.0367(19) O37 0.0264(15) 0.0237(14) 0.090(3) -0.0020(15) -0.0072(16) -0.0066(12) O38 0.066(2) 0.0484(19) 0.073(2) 0.0304(17) 0.0522(19) 0.0292(17) C32 0.072(4) 0.129(6) 0.107(5) 0.063(5) 0.067(4) 0.040(4) C33 0.045(3) 0.029(3) 0.179(8) 0.006(4) -0.025(4) -0.010(2) C34 0.131(6) 0.134(6) 0.037(3) -0.032(4) -0.033(4) 0.081(5) C36 0.150(7) 0.151(7) 0.036(3) -0.035(4) -0.036(4) 0.094(6) C37 0.050(3) 0.032(3) 0.166(7) 0.000(3) -0.019(4) -0.016(2) C38 0.116(6) 0.091(5) 0.141(6) 0.067(5) 0.111(5) 0.063(4) C321 0.057(3) 0.058(3) 0.052(3) 0.013(2) 0.002(2) -0.024(3) C322 0.074(4) 0.061(3) 0.028(2) 0.004(2) 0.009(2) -0.015(3) C331 0.035(2) 0.057(3) 0.087(4) 0.001(3) 0.017(3) -0.015(2) C332 0.042(3) 0.058(3) 0.058(3) -0.016(2) -0.004(2) -0.009(2) C341 0.069(3) 0.054(3) 0.047(3) -0.013(2) 0.030(3) -0.004(3) C342 0.052(3) 0.047(3) 0.056(3) -0.026(2) 0.012(2) -0.005(2) C361 0.057(3) 0.049(3) 0.051(3) -0.024(2) 0.013(2) -0.008(2) C362 0.070(3) 0.056(3) 0.047(3) -0.013(2) 0.030(3) -0.004(3) C371 0.049(3) 0.064(3) 0.051(3) -0.016(3) -0.008(2) -0.015(3) C372 0.036(3) 0.058(3) 0.093(4) -0.005(3) 0.022(3) -0.012(2) C381 0.076(4) 0.061(3) 0.037(3) 0.005(2) 0.017(2) -0.024(3) C382 0.031(2) 0.046(3) 0.057(3) 0.013(2) 0.008(2) -0.0046(19) _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 Ba1 O12 2.637(3) 3_757 ? Ba1 O12 2.637(3) . ? Ba1 O13 2.670(3) . ? Ba1 O13 2.670(3) 3_757 ? Ba1 O14 2.680(3) 3_757 ? Ba1 O14 2.680(3) . ? Ba1 Si12 3.6825(13) 3_757 ? Ba1 Si12 3.6825(13) . ? Ba1 Si13 3.7111(13) 3_757 ? Ba1 Si13 3.7112(13) . ? Ba1 Si14 3.7168(13) . ? Ba1 Si14 3.7168(13) 3_757 ? Si11 Si13 2.2911(19) . ? Si11 Si14 2.3147(17) . ? Si11 Si12 2.3267(17) . ? Si12 O12 1.692(3) . ? Si12 C122 1.862(5) . ? Si12 C121 1.870(5) . ? Si13 O13 1.703(4) . ? Si13 C132 1.877(5) . ? Si13 C131 1.885(5) . ? Si14 O14 1.691(3) . ? Si14 C141 1.866(6) . ? Si14 C142 1.889(5) . ? O12 C12 1.446(5) . ? O13 C13 1.434(6) . ? O14 C14 1.442(6) . ? Ba2 O28 2.660(3) . ? Ba2 O22 2.663(3) . ? Ba2 O27 2.665(3) . ? Ba2 O24 2.667(3) . ? Ba2 O26 2.679(3) . ? Ba2 O23 2.683(3) . ? Ba2 Si22 3.6965(14) . ? Ba2 Si24 3.7016(12) . ? Ba2 Si23 3.7191(12) . ? Ba2 Si28 3.7233(12) . ? Ba2 Si26 3.7443(13) . ? Ba2 Si27 3.7593(14) . ? Si21 Si24 2.3037(18) . ? Si21 Si23 2.3066(16) . ? Si21 Si22 2.3109(17) . ? Si22 O22 1.697(3) . ? Si22 C222 1.863(5) . ? Si22 C221 1.870(5) . ? Si23 O23 1.699(3) . ? Si23 C231 1.870(5) . ? Si23 C232 1.880(5) . ? Si24 O24 1.708(3) . ? Si24 C242 1.873(5) . ? Si24 C241 1.874(5) . ? Si25 Si26 2.3049(18) . ? Si25 Si28 2.3058(17) . ? Si25 Si27 2.3138(17) . ? Si26 O26 1.692(3) . ? Si26 C261 1.874(5) . ? Si26 C262 1.875(5) . ? Si27 O27 1.697(3) . ? Si27 C272 1.870(6) . ? Si27 C271 1.881(5) . ? Si28 O28 1.693(3) . ? Si28 C281 1.867(5) . ? Si28 C282 1.883(5) . ? O22 C22 1.447(5) . ? O23 C23 1.433(5) . ? O24 C24 1.429(6) . ? O26 C26 1.429(6) . ? O27 C27 1.437(5) . ? O28 C28 1.441(6) . ? Ba3 O37 2.645(3) . ? Ba3 O33 2.652(3) . ? Ba3 O36 2.669(3) . ? Ba3 O34 2.671(3) . ? Ba3 O38 2.674(3) . ? Ba3 O32 2.679(3) . ? Ba3 Si33 3.6778(13) . ? Ba3 Si34 3.6860(12) . ? Ba3 Si32 3.6934(12) . ? Ba3 Si31 3.7003(12) . ? Ba3 Si36 3.7051(12) . ? Ba3 Si37 3.7094(13) . ? Si31 Si34 2.3012(16) . ? Si31 Si32 2.3045(16) . ? Si31 Si33 2.3083(16) . ? Si32 O32 1.700(3) . ? Si32 C321 1.865(5) . ? Si32 C322 1.873(5) . ? Si33 O33 1.693(3) . ? Si33 C331 1.867(5) . ? Si33 C332 1.874(5) . ? Si34 O34 1.695(3) . ? Si34 C341 1.869(5) . ? Si34 C342 1.871(5) . ? Si35 Si36 2.3020(16) . ? Si35 Si38 2.3068(15) . ? Si35 Si37 2.3128(15) . ? Si36 O36 1.691(3) . ? Si36 C361 1.871(5) . ? Si36 C362 1.879(5) . ? Si37 O37 1.698(3) . ? Si37 C372 1.865(5) . ? Si37 C371 1.876(5) . ? Si38 O38 1.693(3) . ? Si38 C382 1.862(4) . ? Si38 C381 1.874(5) . ? O32 C32 1.432(5) . ? O33 C33 1.440(5) . ? O34 C34 1.434(6) . ? O36 C36 1.436(6) . ? O37 C37 1.443(5) . ? O38 C38 1.437(5) . ? 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 O12 Ba1 O12 179.997(1) 3_757 . ? O12 Ba1 O13 82.80(10) 3_757 . ? O12 Ba1 O13 97.20(10) . . ? O12 Ba1 O13 97.20(10) 3_757 3_757 ? O12 Ba1 O13 82.80(10) . 3_757 ? O13 Ba1 O13 179.999(1) . 3_757 ? O12 Ba1 O14 97.68(10) 3_757 3_757 ? O12 Ba1 O14 82.32(10) . 3_757 ? O13 Ba1 O14 82.00(11) . 3_757 ? O13 Ba1 O14 98.00(11) 3_757 3_757 ? O12 Ba1 O14 82.32(10) 3_757 . ? O12 Ba1 O14 97.68(10) . . ? O13 Ba1 O14 98.00(11) . . ? O13 Ba1 O14 81.99(11) 3_757 . ? O14 Ba1 O14 179.999(1) 3_757 . ? O12 Ba1 Si12 24.65(7) 3_757 3_757 ? O12 Ba1 Si12 155.35(7) . 3_757 ? O13 Ba1 Si12 101.37(8) . 3_757 ? O13 Ba1 Si12 78.63(8) 3_757 3_757 ? O14 Ba1 Si12 84.35(7) 3_757 3_757 ? O14 Ba1 Si12 95.65(7) . 3_757 ? O12 Ba1 Si12 155.35(7) 3_757 . ? O12 Ba1 Si12 24.65(7) . . ? O13 Ba1 Si12 78.63(8) . . ? O13 Ba1 Si12 101.37(8) 3_757 . ? O14 Ba1 Si12 95.65(7) 3_757 . ? O14 Ba1 Si12 84.35(7) . . ? Si12 Ba1 Si12 180.0 3_757 . ? O12 Ba1 Si13 83.72(7) 3_757 3_757 ? O12 Ba1 Si13 96.28(7) . 3_757 ? O13 Ba1 Si13 155.27(7) . 3_757 ? O13 Ba1 Si13 24.73(7) 3_757 3_757 ? O14 Ba1 Si13 79.38(8) 3_757 3_757 ? O14 Ba1 Si13 100.62(8) . 3_757 ? Si12 Ba1 Si13 60.80(3) 3_757 3_757 ? Si12 Ba1 Si13 119.19(3) . 3_757 ? O12 Ba1 Si13 96.28(7) 3_757 . ? O12 Ba1 Si13 83.72(7) . . ? O13 Ba1 Si13 24.73(7) . . ? O13 Ba1 Si13 155.27(7) 3_757 . ? O14 Ba1 Si13 100.62(8) 3_757 . ? O14 Ba1 Si13 79.38(8) . . ? Si12 Ba1 Si13 119.20(3) 3_757 . ? Si12 Ba1 Si13 60.81(3) . . ? Si13 Ba1 Si13 180.00(3) 3_757 . ? O12 Ba1 Si14 99.57(7) 3_757 . ? O12 Ba1 Si14 80.43(7) . . ? O13 Ba1 Si14 83.14(8) . . ? O13 Ba1 Si14 96.86(8) 3_757 . ? O14 Ba1 Si14 155.56(6) 3_757 . ? O14 Ba1 Si14 24.44(6) . . ? Si12 Ba1 Si14 117.64(3) 3_757 . ? Si12 Ba1 Si14 62.36(3) . . ? Si13 Ba1 Si14 119.59(3) 3_757 . ? Si13 Ba1 Si14 60.41(3) . . ? O12 Ba1 Si14 80.43(7) 3_757 3_757 ? O12 Ba1 Si14 99.57(7) . 3_757 ? O13 Ba1 Si14 96.86(8) . 3_757 ? O13 Ba1 Si14 83.14(8) 3_757 3_757 ? O14 Ba1 Si14 24.44(6) 3_757 3_757 ? O14 Ba1 Si14 155.56(6) . 3_757 ? Si12 Ba1 Si14 62.36(3) 3_757 3_757 ? Si12 Ba1 Si14 117.64(3) . 3_757 ? Si13 Ba1 Si14 60.41(3) 3_757 3_757 ? Si13 Ba1 Si14 119.59(3) . 3_757 ? Si14 Ba1 Si14 180.0 . 3_757 ? Si13 Si11 Si14 108.45(7) . . ? Si13 Si11 Si12 108.25(6) . . ? Si14 Si11 Si12 111.25(7) . . ? Si13 Si11 Ba1 70.73(4) . . ? Si14 Si11 Ba1 70.70(4) . . ? Si12 Si11 Ba1 69.73(4) . . ? O12 Si12 C122 105.7(2) . . ? O12 Si12 C121 105.8(2) . . ? C122 Si12 C121 107.1(2) . . ? O12 Si12 Si11 113.57(11) . . ? C122 Si12 Si11 112.0(2) . . ? C121 Si12 Si11 112.09(16) . . ? O12 Si12 Ba1 40.54(10) . . ? C122 Si12 Ba1 131.04(19) . . ? C121 Si12 Ba1 115.24(17) . . ? Si11 Si12 Ba1 73.92(4) . . ? O13 Si13 C132 105.1(2) . . ? O13 Si13 C131 105.4(2) . . ? C132 Si13 C131 107.8(2) . . ? O13 Si13 Si11 113.84(12) . . ? C132 Si13 Si11 111.20(19) . . ? C131 Si13 Si11 113.0(2) . . ? O13 Si13 Ba1 40.96(10) . . ? C132 Si13 Ba1 129.32(18) . . ? C131 Si13 Ba1 116.33(18) . . ? Si11 Si13 Ba1 73.63(4) . . ? O14 Si14 C141 106.3(3) . . ? O14 Si14 C142 105.4(2) . . ? C141 Si14 C142 107.5(3) . . ? O14 Si14 Si11 114.02(12) . . ? C141 Si14 Si11 112.0(2) . . ? C142 Si14 Si11 111.2(2) . . ? O14 Si14 Ba1 40.96(10) . . ? C141 Si14 Ba1 119.9(2) . . ? C142 Si14 Ba1 126.7(2) . . ? Si11 Si14 Ba1 73.30(4) . . ? C12 O12 Si12 123.5(3) . . ? C12 O12 Ba1 121.4(3) . . ? Si12 O12 Ba1 114.81(14) . . ? C13 O13 Si13 121.6(4) . . ? C13 O13 Ba1 123.7(3) . . ? Si13 O13 Ba1 114.31(15) . . ? C14 O14 Si14 122.6(3) . . ? C14 O14 Ba1 122.6(3) . . ? Si14 O14 Ba1 114.60(14) . . ? O28 Ba2 O22 83.15(11) . . ? O28 Ba2 O27 95.49(11) . . ? O22 Ba2 O27 178.54(11) . . ? O28 Ba2 O24 81.97(11) . . ? O22 Ba2 O24 96.55(11) . . ? O27 Ba2 O24 82.73(11) . . ? O28 Ba2 O26 95.62(12) . . ? O22 Ba2 O26 83.48(12) . . ? O27 Ba2 O26 97.19(12) . . ? O24 Ba2 O26 177.57(11) . . ? O28 Ba2 O23 177.83(10) . . ? O22 Ba2 O23 99.00(10) . . ? O27 Ba2 O23 82.37(10) . . ? O24 Ba2 O23 98.04(11) . . ? O26 Ba2 O23 84.35(11) . . ? O28 Ba2 Si22 102.21(8) . . ? O22 Ba2 Si22 24.77(7) . . ? O27 Ba2 Si22 155.91(7) . . ? O24 Ba2 Si22 83.70(8) . . ? O26 Ba2 Si22 97.19(8) . . ? O23 Ba2 Si22 79.94(7) . . ? O28 Ba2 Si24 97.50(7) . . ? O22 Ba2 Si24 79.11(8) . . ? O27 Ba2 Si24 100.59(8) . . ? O24 Ba2 Si24 24.99(7) . . ? O26 Ba2 Si24 156.72(7) . . ? O23 Ba2 Si24 83.25(7) . . ? Si22 Ba2 Si24 61.24(3) . . ? O28 Ba2 Si23 156.89(7) . . ? O22 Ba2 Si23 83.84(7) . . ? O27 Ba2 Si23 97.27(7) . . ? O24 Ba2 Si23 80.64(8) . . ? O26 Ba2 Si23 101.77(8) . . ? O23 Ba2 Si23 24.61(6) . . ? Si22 Ba2 Si23 60.84(3) . . ? Si24 Ba2 Si23 61.24(3) . . ? O28 Ba2 Si28 24.16(7) . . ? O22 Ba2 Si28 97.99(7) . . ? O27 Ba2 Si28 80.90(7) . . ? O24 Ba2 Si28 99.09(8) . . ? O26 Ba2 Si28 78.50(8) . . ? O23 Ba2 Si28 154.24(7) . . ? Si22 Ba2 Si28 120.96(3) . . ? Si24 Ba2 Si28 119.02(3) . . ? Si23 Ba2 Si28 178.17(3) . . ? O28 Ba2 Si26 82.48(7) . . ? O22 Ba2 Si26 101.69(8) . . ? O27 Ba2 Si26 78.61(8) . . ? O24 Ba2 Si26 154.36(7) . . ? O26 Ba2 Si26 23.97(7) . . ? O23 Ba2 Si26 96.74(7) . . ? Si22 Ba2 Si26 119.56(3) . . ? Si24 Ba2 Si26 179.19(3) . . ? Si23 Ba2 Si26 118.91(3) . . ? Si28 Ba2 Si26 60.80(3) . . ? O28 Ba2 Si27 79.15(8) . . ? O22 Ba2 Si27 155.75(7) . . ? O27 Ba2 Si27 23.65(7) . . ? O24 Ba2 Si27 97.25(8) . . ? O26 Ba2 Si27 81.91(8) . . ? O23 Ba2 Si27 98.70(7) . . ? Si22 Ba2 Si27 178.46(3) . . ? Si24 Ba2 Si27 119.44(3) . . ? Si23 Ba2 Si27 118.07(3) . . ? Si28 Ba2 Si27 60.14(3) . . ? Si26 Ba2 Si27 59.76(3) . . ? Si24 Si21 Si23 110.13(6) . . ? Si24 Si21 Si22 109.49(6) . . ? Si23 Si21 Si22 108.81(6) . . ? Si24 Si21 Ba2 70.46(4) . . ? Si23 Si21 Ba2 70.89(4) . . ? Si22 Si21 Ba2 70.27(4) . . ? O22 Si22 C222 105.7(2) . . ? O22 Si22 C221 105.9(2) . . ? C222 Si22 C221 107.9(3) . . ? O22 Si22 Si21 113.88(12) . . ? C222 Si22 Si21 111.2(2) . . ? C221 Si22 Si21 111.87(18) . . ? O22 Si22 Ba2 41.10(10) . . ? C222 Si22 Ba2 130.7(2) . . ? C221 Si22 Ba2 115.30(19) . . ? Si21 Si22 Ba2 73.68(4) . . ? O23 Si23 C231 105.7(2) . . ? O23 Si23 C232 105.6(2) . . ? C231 Si23 C232 108.9(2) . . ? O23 Si23 Si21 114.11(11) . . ? C231 Si23 Si21 111.80(17) . . ? C232 Si23 Si21 110.39(17) . . ? O23 Si23 Ba2 41.11(10) . . ? C231 Si23 Ba2 119.15(15) . . ? C232 Si23 Ba2 126.44(16) . . ? Si21 Si23 Ba2 73.24(4) . . ? O24 Si24 C242 105.1(2) . . ? O24 Si24 C241 105.6(2) . . ? C242 Si24 C241 108.6(2) . . ? O24 Si24 Si21 114.58(12) . . ? C242 Si24 Si21 112.17(18) . . ? C241 Si24 Si21 110.4(2) . . ? O24 Si24 Ba2 41.26(10) . . ? C242 Si24 Ba2 128.06(16) . . ? C241 Si24 Ba2 117.37(17) . . ? Si21 Si24 Ba2 73.64(4) . . ? Si26 Si25 Si28 110.09(7) . . ? Si26 Si25 Si27 108.06(6) . . ? Si28 Si25 Si27 108.51(7) . . ? O26 Si26 C261 105.6(3) . . ? O26 Si26 C262 104.8(3) . . ? C261 Si26 C262 107.9(3) . . ? O26 Si26 Si25 113.86(12) . . ? C261 Si26 Si25 112.2(2) . . ? C262 Si26 Si25 111.9(2) . . ? O26 Si26 Ba2 40.03(11) . . ? C261 Si26 Ba2 130.6(2) . . ? C262 Si26 Ba2 114.41(18) . . ? Si25 Si26 Ba2 74.62(4) . . ? O27 Si27 C272 105.9(2) . . ? O27 Si27 C271 105.4(2) . . ? C272 Si27 C271 106.9(3) . . ? O27 Si27 Si25 113.16(12) . . ? C272 Si27 Si25 112.6(2) . . ? C271 Si27 Si25 112.3(2) . . ? O27 Si27 Ba2 39.06(10) . . ? C272 Si27 Ba2 120.5(2) . . ? C271 Si27 Ba2 125.3(2) . . ? Si25 Si27 Ba2 74.22(4) . . ? O28 Si28 C281 104.7(2) . . ? O28 Si28 C282 105.1(2) . . ? C281 Si28 C282 109.0(2) . . ? O28 Si28 Si25 114.88(12) . . ? C281 Si28 Si25 113.08(17) . . ? C282 Si28 Si25 109.64(19) . . ? O28 Si28 Ba2 40.02(10) . . ? C281 Si28 Ba2 119.33(17) . . ? C282 Si28 Ba2 124.89(19) . . ? Si25 Si28 Ba2 75.06(4) . . ? C22 O22 Si22 122.2(3) . . ? C22 O22 Ba2 123.0(3) . . ? Si22 O22 Ba2 114.14(14) . . ? C23 O23 Si23 122.3(3) . . ? C23 O23 Ba2 123.3(3) . . ? Si23 O23 Ba2 114.28(13) . . ? C24 O24 Si24 121.4(3) . . ? C24 O24 Ba2 124.8(3) . . ? Si24 O24 Ba2 113.75(15) . . ? C26 O26 Si26 122.0(3) . . ? C26 O26 Ba2 121.6(3) . . ? Si26 O26 Ba2 116.00(16) . . ? C27 O27 Si27 122.7(3) . . ? C27 O27 Ba2 119.9(3) . . ? Si27 O27 Ba2 117.29(14) . . ? C28 O28 Si28 122.3(3) . . ? C28 O28 Ba2 121.8(3) . . ? Si28 O28 Ba2 115.82(14) . . ? O37 Ba3 O33 178.22(9) . . ? O37 Ba3 O36 97.46(11) . . ? O33 Ba3 O36 81.49(11) . . ? O37 Ba3 O34 82.42(11) . . ? O33 Ba3 O34 98.63(11) . . ? O36 Ba3 O34 179.67(10) . . ? O37 Ba3 O38 94.76(11) . . ? O33 Ba3 O38 84.02(11) . . ? O36 Ba3 O38 99.97(12) . . ? O34 Ba3 O38 79.73(11) . . ? O37 Ba3 O32 81.55(11) . . ? O33 Ba3 O32 99.70(11) . . ? O36 Ba3 O32 82.22(12) . . ? O34 Ba3 O32 98.06(12) . . ? O38 Ba3 O32 175.96(11) . . ? O37 Ba3 Si33 156.86(6) . . ? O33 Ba3 Si33 24.92(6) . . ? O36 Ba3 Si33 96.11(7) . . ? O34 Ba3 Si33 84.11(7) . . ? O38 Ba3 Si33 101.24(8) . . ? O32 Ba3 Si33 81.83(7) . . ? O37 Ba3 Si34 100.31(7) . . ? O33 Ba3 Si34 81.12(7) . . ? O36 Ba3 Si34 155.32(7) . . ? O34 Ba3 Si34 24.99(7) . . ? O38 Ba3 Si34 95.49(7) . . ? O32 Ba3 Si34 83.59(7) . . ? Si33 Ba3 Si34 61.85(3) . . ? O37 Ba3 Si32 97.29(7) . . ? O33 Ba3 Si32 84.32(7) . . ? O36 Ba3 Si32 99.36(8) . . ? O34 Ba3 Si32 80.96(8) . . ? O38 Ba3 Si32 155.64(6) . . ? O32 Ba3 Si32 25.05(7) . . ? Si33 Ba3 Si32 61.96(3) . . ? Si34 Ba3 Si32 61.56(3) . . ? O37 Ba3 Si31 120.52(6) . . ? O33 Ba3 Si31 61.26(6) . . ? O36 Ba3 Si31 119.13(7) . . ? O34 Ba3 Si31 61.19(7) . . ? O38 Ba3 Si31 119.84(7) . . ? O32 Ba3 Si31 61.30(7) . . ? Si33 Ba3 Si31 36.46(2) . . ? Si34 Ba3 Si31 36.31(3) . . ? Si32 Ba3 Si31 36.32(3) . . ? O37 Ba3 Si36 80.09(7) . . ? O33 Ba3 Si36 98.47(7) . . ? O36 Ba3 Si36 24.53(7) . . ? O34 Ba3 Si36 155.16(7) . . ? O38 Ba3 Si36 84.28(7) . . ? O32 Ba3 Si36 96.66(7) . . ? Si33 Ba3 Si36 117.82(3) . . ? Si34 Ba3 Si36 179.56(3) . . ? Si32 Ba3 Si36 118.61(3) . . ? Si31 Ba3 Si36 143.59(3) . . ? O37 Ba3 Si37 24.38(6) . . ? O33 Ba3 Si37 153.84(6) . . ? O36 Ba3 Si37 82.72(7) . . ? O34 Ba3 Si37 97.05(7) . . ? O38 Ba3 Si37 78.32(8) . . ? O32 Ba3 Si37 98.68(7) . . ? Si33 Ba3 Si37 178.65(3) . . ? Si34 Ba3 Si37 119.43(3) . . ? Si32 Ba3 Si37 118.87(3) . . ? Si31 Ba3 Si37 144.83(3) . . ? Si36 Ba3 Si37 60.90(3) . . ? Si34 Si31 Si32 110.15(6) . . ? Si34 Si31 Si33 110.37(6) . . ? Si32 Si31 Si33 110.69(6) . . ? Si34 Si31 Ba3 71.51(4) . . ? Si32 Si31 Ba3 71.68(4) . . ? Si33 Si31 Ba3 71.24(4) . . ? O32 Si32 C321 106.0(2) . . ? O32 Si32 C322 105.6(2) . . ? C321 Si32 C322 108.3(2) . . ? O32 Si32 Si31 113.69(11) . . ? C321 Si32 Si31 112.16(19) . . ? C322 Si32 Si31 110.70(17) . . ? O32 Si32 Ba3 41.84(10) . . ? C321 Si32 Ba3 120.69(17) . . ? C322 Si32 Ba3 125.87(17) . . ? Si31 Si32 Ba3 72.00(4) . . ? O33 Si33 C331 106.1(2) . . ? O33 Si33 C332 106.1(2) . . ? C331 Si33 C332 107.5(2) . . ? O33 Si33 Si31 113.29(11) . . ? C331 Si33 Si31 111.85(18) . . ? C332 Si33 Si31 111.53(17) . . ? O33 Si33 Ba3 41.29(10) . . ? C331 Si33 Ba3 128.32(19) . . ? C332 Si33 Ba3 118.70(17) . . ? Si31 Si33 Ba3 72.30(4) . . ? O34 Si34 C341 105.7(2) . . ? O34 Si34 C342 105.5(2) . . ? C341 Si34 C342 108.8(2) . . ? O34 Si34 Si31 113.66(11) . . ? C341 Si34 Si31 110.77(17) . . ? C342 Si34 Si31 112.06(17) . . ? O34 Si34 Ba3 41.72(10) . . ? C341 Si34 Ba3 118.17(16) . . ? C342 Si34 Ba3 127.60(16) . . ? Si31 Si34 Ba3 72.18(4) . . ? Si36 Si35 Si38 110.83(6) . . ? Si36 Si35 Si37 109.03(6) . . ? Si38 Si35 Si37 107.70(6) . . ? Si36 Si35 Ba3 70.21(4) . . ? Si38 Si35 Ba3 70.29(4) . . ? Si37 Si35 Ba3 70.25(4) . . ? O36 Si36 C361 105.2(2) . . ? O36 Si36 C362 105.3(2) . . ? C361 Si36 C362 108.9(2) . . ? O36 Si36 Si35 114.73(11) . . ? C361 Si36 Si35 112.32(17) . . ? C362 Si36 Si35 109.98(18) . . ? O36 Si36 Ba3 40.94(10) . . ? C361 Si36 Ba3 127.47(16) . . ? C362 Si36 Ba3 117.53(16) . . ? Si35 Si36 Ba3 74.01(4) . . ? O37 Si37 C372 104.9(2) . . ? O37 Si37 C371 105.0(2) . . ? C372 Si37 C371 108.2(3) . . ? O37 Si37 Si35 113.65(11) . . ? C372 Si37 Si35 112.99(18) . . ? C371 Si37 Si35 111.52(18) . . ? O37 Si37 Ba3 40.03(9) . . ? C372 Si37 Ba3 126.7(2) . . ? C371 Si37 Ba3 118.06(18) . . ? Si35 Si37 Ba3 73.82(4) . . ? O38 Si38 C382 104.7(2) . . ? O38 Si38 C381 106.3(2) . . ? C382 Si38 C381 107.9(2) . . ? O38 Si38 Si35 114.26(11) . . ? C382 Si38 Si35 113.10(16) . . ? C381 Si38 Si35 110.15(18) . . ? O38 Si38 Ba3 41.02(10) . . ? C382 Si38 Ba3 116.39(15) . . ? C381 Si38 Ba3 129.59(17) . . ? Si35 Si38 Ba3 73.87(4) . . ? C32 O32 Si32 121.9(3) . . ? C32 O32 Ba3 124.9(3) . . ? Si32 O32 Ba3 113.11(14) . . ? C33 O33 Si33 121.9(3) . . ? C33 O33 Ba3 123.9(3) . . ? Si33 O33 Ba3 113.79(14) . . ? C34 O34 Si34 121.2(3) . . ? C34 O34 Ba3 125.5(3) . . ? Si34 O34 Ba3 113.29(14) . . ? C36 O36 Si36 122.0(3) . . ? C36 O36 Ba3 123.3(3) . . ? Si36 O36 Ba3 114.53(15) . . ? C37 O37 Si37 122.9(3) . . ? C37 O37 Ba3 121.3(3) . . ? Si37 O37 Ba3 115.59(13) . . ? C38 O38 Si38 122.1(3) . . ? C38 O38 Ba3 122.7(3) . . ? Si38 O38 Ba3 114.44(14) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.83 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 4.389 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.148 # Attachment 'CKSrCmcaBRW.cif' data_cksrcmcabrw _database_code_depnum_ccdc_archive 'CCDC 829368' #TrackingRef 'CKSrCmcaBRW.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 O6 Si8 Sr' _chemical_formula_weight 678.92 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x+1/2, y, -z+1/2' '-x+1/2, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1, y+1/2, -z+1/2' '-x+1, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, z' 'x-1/2, -y, z-1/2' 'x-1/2, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z-1/2' 'x, y+1/2, -z-1/2' _cell_length_a 16.8439(16) _cell_length_b 12.8565(12) _cell_length_c 16.9429(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3669.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 3.196 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3908 _exptl_absorpt_correction_T_max 0.6305 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13774 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 22.57 _reflns_number_total 1259 _reflns_number_gt 1044 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0453P)^2^+11.5346P] 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_extinction_coef ? _refine_ls_number_reflns 1259 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.006 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 Sr1 Sr 0.5000 0.5000 0.5000 0.0392(3) Uani 1 4 d S . . Si1 Si 0.5000 0.70057(12) 0.65784(9) 0.0591(5) Uani 1 2 d S . . Si2 Si 0.5000 0.77559(15) 0.53410(13) 0.0748(8) Uani 0.824(3) 2 d SP . . Si3 Si 0.61070(10) 0.59713(11) 0.66614(8) 0.0582(5) Uani 0.824(3) 1 d P . . O2 O 0.5000 0.6867(4) 0.4602(3) 0.0737(17) Uani 0.824(3) 2 d SP . . O3 O 0.6145(2) 0.5032(3) 0.5959(2) 0.0677(11) Uani 0.824(3) 1 d P . . C20 C 0.5000 0.7182(10) 0.3792(7) 0.106(5) Uani 0.824(3) 2 d SP . . C21 C 0.5889(8) 0.8583(10) 0.5159(7) 0.108(5) Uani 0.824(3) 1 d P . . H21A H 0.6363 0.8142 0.5130 0.162 Uiso 0.824(3) 1 calc PR . . H21B H 0.5948 0.9083 0.5591 0.162 Uiso 0.824(3) 1 calc PR . . H21C H 0.5823 0.8957 0.4659 0.162 Uiso 0.824(3) 1 calc PR . . C30 C 0.6786(4) 0.4267(6) 0.5913(4) 0.112(3) Uani 0.824(3) 1 d P . . H30A H 0.7297 0.4628 0.5883 0.168 Uiso 0.824(3) 1 calc PR . . H30B H 0.6715 0.3836 0.5441 0.168 Uiso 0.824(3) 1 calc PR . . H30C H 0.6774 0.3824 0.6383 0.168 Uiso 0.824(3) 1 calc PR . . C31 C 0.7027(7) 0.6758(10) 0.6543(6) 0.087(3) Uani 0.824(3) 1 d P . . H31A H 0.7488 0.6341 0.6699 0.131 Uiso 0.824(3) 1 calc PR . . H31B H 0.6994 0.7378 0.6878 0.131 Uiso 0.824(3) 1 calc PR . . H31C H 0.7082 0.6969 0.5990 0.131 Uiso 0.824(3) 1 calc PR . . C32 C 0.6172(6) 0.5277(7) 0.7626(6) 0.069(3) Uani 0.824(3) 1 d P . . H32A H 0.5733 0.4780 0.7670 0.104 Uiso 0.824(3) 1 calc PR . . H32B H 0.6139 0.5783 0.8058 0.104 Uiso 0.824(3) 1 calc PR . . H32C H 0.6679 0.4904 0.7658 0.104 Uiso 0.824(3) 1 calc PR . . Si29 Si 0.5000 0.5318(6) 0.7095(4) 0.043(2) Uani 0.176(3) 2 d SP . . Si39 Si 0.6100(4) 0.7161(4) 0.5784(4) 0.048(2) Uani 0.176(3) 1 d P . . O29 O 0.5000 0.4400(14) 0.6373(10) 0.049(6) Uani 0.176(3) 2 d SP . . O39 O 0.6133(8) 0.6265(11) 0.5056(8) 0.047(4) Uani 0.176(3) 1 d P . . H20B H 0.543(5) 0.764(7) 0.371(6) 0.18(4) Uiso 0.824(3) 1 d P . . C209 C 0.5000 0.325(3) 0.6559(14) 0.100(10) Uani 0.351(5) 2 d SP . . C219 C 0.590(3) 0.498(3) 0.771(2) 0.047(10) Uani 0.176(3) 1 d P . . C319 C 0.616(2) 0.849(4) 0.532(2) 0.037(8) Uani 0.176(3) 1 d P . . C329 C 0.709(3) 0.701(4) 0.628(2) 0.054(10) Uani 0.176(3) 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 Sr1 0.0630(5) 0.0286(4) 0.0262(4) 0.0047(3) 0.000 0.000 Si1 0.0995(14) 0.0384(9) 0.0393(9) 0.0031(7) 0.000 0.000 Si2 0.146(2) 0.0317(11) 0.0469(12) 0.0086(9) 0.000 0.000 Si3 0.0811(11) 0.0557(9) 0.0377(8) 0.0001(6) -0.0056(7) -0.0049(8) O2 0.149(5) 0.035(3) 0.038(3) 0.012(2) 0.000 0.000 O3 0.084(3) 0.070(2) 0.049(2) -0.0129(17) -0.0139(18) 0.015(2) C20 0.231(17) 0.053(7) 0.033(6) 0.014(5) 0.000 0.000 C21 0.204(15) 0.052(6) 0.069(7) 0.017(4) -0.005(7) -0.035(8) C30 0.098(5) 0.137(7) 0.102(5) -0.016(5) -0.030(4) 0.061(5) C31 0.101(7) 0.107(9) 0.054(6) 0.021(5) -0.005(5) -0.035(6) C32 0.096(7) 0.058(6) 0.054(5) 0.009(4) -0.010(5) -0.007(5) Si29 0.076(6) 0.036(5) 0.015(4) 0.005(3) 0.000 0.000 Si39 0.069(5) 0.033(3) 0.043(4) 0.013(3) -0.022(3) -0.017(3) O29 0.100(17) 0.025(11) 0.023(10) 0.002(8) 0.000 0.000 O39 0.038(8) 0.047(9) 0.055(9) 0.005(7) -0.004(7) -0.018(6) C209 0.18(3) 0.10(2) 0.027(13) 0.004(13) 0.000 0.000 C219 0.09(3) 0.029(16) 0.018(13) 0.019(10) -0.032(16) -0.033(14) C319 0.046(14) 0.047(17) 0.018(13) 0.034(12) 0.010(12) -0.003(12) C329 0.047(16) 0.07(2) 0.04(2) 0.023(18) -0.017(16) -0.056(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 Sr1 O29 2.451(17) . ? Sr1 O29 2.452(17) 9_666 ? Sr1 O2 2.493(4) 9_666 ? Sr1 O2 2.493(4) . ? Sr1 O39 2.509(13) . ? Sr1 O39 2.509(13) 9_666 ? Sr1 O39 2.509(13) 10_655 ? Sr1 O39 2.509(13) 2_566 ? Sr1 O3 2.521(4) . ? Sr1 O3 2.521(4) 9_666 ? Sr1 O3 2.521(4) 10_655 ? Sr1 O3 2.521(4) 2_566 ? Si1 Si3 2.2946(18) 10_655 ? Si1 Si3 2.2946(18) . ? Si1 Si39 2.298(7) 10_655 ? Si1 Si39 2.298(7) . ? Si1 Si2 2.308(3) . ? Si1 Si29 2.339(8) . ? Si2 O2 1.695(5) . ? Si2 C21 1.861(13) 10_655 ? Si2 C21 1.861(13) . ? Si2 Si39 2.140(6) 10_655 ? Si2 C319 2.16(4) 10_655 ? Si3 O3 1.697(3) . ? Si3 C31 1.861(10) . ? Si3 C32 1.866(9) . ? O2 C20 1.431(11) . ? O3 C30 1.463(7) . ? C20 C209 0.81(2) 9_666 ? Si29 O29 1.699(19) . ? Si29 C219 1.90(4) 10_655 ? Si29 C219 1.90(4) . ? Si29 C32 2.171(11) 10_655 ? Si29 Si3 2.173(4) 10_655 ? Si39 O39 1.688(16) . ? Si39 C319 1.88(4) . ? Si39 C329 1.88(4) . ? O29 C209 1.51(4) . ? C209 C20 0.81(2) 9_666 ? 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 O29 Sr1 O29 179.999(1) . 9_666 ? O29 Sr1 O2 56.0(4) . 9_666 ? O29 Sr1 O2 124.0(4) 9_666 9_666 ? O29 Sr1 O2 124.0(4) . . ? O29 Sr1 O2 56.0(4) 9_666 . ? O2 Sr1 O2 180.0 9_666 . ? O29 Sr1 O39 99.7(4) . . ? O29 Sr1 O39 80.3(4) 9_666 . ? O2 Sr1 O39 127.9(3) 9_666 . ? O2 Sr1 O39 52.1(3) . . ? O29 Sr1 O39 80.3(4) . 9_666 ? O29 Sr1 O39 99.7(4) 9_666 9_666 ? O2 Sr1 O39 52.1(3) 9_666 9_666 ? O2 Sr1 O39 127.9(3) . 9_666 ? O39 Sr1 O39 179.999(1) . 9_666 ? O29 Sr1 O39 99.7(4) . 10_655 ? O29 Sr1 O39 80.3(4) 9_666 10_655 ? O2 Sr1 O39 127.9(3) 9_666 10_655 ? O2 Sr1 O39 52.1(3) . 10_655 ? O39 Sr1 O39 99.0(7) . 10_655 ? O39 Sr1 O39 81.0(7) 9_666 10_655 ? O29 Sr1 O39 80.3(4) . 2_566 ? O29 Sr1 O39 99.7(4) 9_666 2_566 ? O2 Sr1 O39 52.1(3) 9_666 2_566 ? O2 Sr1 O39 127.9(3) . 2_566 ? O39 Sr1 O39 81.0(7) . 2_566 ? O39 Sr1 O39 99.0(7) 9_666 2_566 ? O39 Sr1 O39 180.000(2) 10_655 2_566 ? O29 Sr1 O3 52.67(15) . . ? O29 Sr1 O3 127.33(15) 9_666 . ? O2 Sr1 O3 80.88(11) 9_666 . ? O2 Sr1 O3 99.12(11) . . ? O39 Sr1 O3 51.9(3) . . ? O39 Sr1 O3 128.1(3) 9_666 . ? O39 Sr1 O3 123.1(3) 10_655 . ? O39 Sr1 O3 56.9(3) 2_566 . ? O29 Sr1 O3 127.33(15) . 9_666 ? O29 Sr1 O3 52.67(15) 9_666 9_666 ? O2 Sr1 O3 99.12(11) 9_666 9_666 ? O2 Sr1 O3 80.88(11) . 9_666 ? O39 Sr1 O3 128.1(3) . 9_666 ? O39 Sr1 O3 51.9(3) 9_666 9_666 ? O39 Sr1 O3 56.9(3) 10_655 9_666 ? O39 Sr1 O3 123.1(3) 2_566 9_666 ? O3 Sr1 O3 180.0 . 9_666 ? O29 Sr1 O3 52.67(15) . 10_655 ? O29 Sr1 O3 127.33(15) 9_666 10_655 ? O2 Sr1 O3 80.88(11) 9_666 10_655 ? O2 Sr1 O3 99.12(11) . 10_655 ? O39 Sr1 O3 123.1(3) . 10_655 ? O39 Sr1 O3 56.9(3) 9_666 10_655 ? O39 Sr1 O3 51.9(3) 10_655 10_655 ? O39 Sr1 O3 128.1(3) 2_566 10_655 ? O3 Sr1 O3 99.75(17) . 10_655 ? O3 Sr1 O3 80.25(17) 9_666 10_655 ? O29 Sr1 O3 127.33(15) . 2_566 ? O29 Sr1 O3 52.67(15) 9_666 2_566 ? O2 Sr1 O3 99.12(11) 9_666 2_566 ? O2 Sr1 O3 80.88(11) . 2_566 ? O39 Sr1 O3 56.9(3) . 2_566 ? O39 Sr1 O3 123.1(3) 9_666 2_566 ? O39 Sr1 O3 128.1(3) 10_655 2_566 ? O39 Sr1 O3 51.9(3) 2_566 2_566 ? O3 Sr1 O3 80.25(17) . 2_566 ? O3 Sr1 O3 99.75(17) 9_666 2_566 ? O3 Sr1 O3 180.0 10_655 2_566 ? Si3 Si1 Si3 108.71(10) 10_655 . ? Si3 Si1 Si39 55.35(15) 10_655 10_655 ? Si3 Si1 Si39 137.84(16) . 10_655 ? Si3 Si1 Si39 137.84(16) 10_655 . ? Si3 Si1 Si39 55.35(15) . . ? Si39 Si1 Si39 107.4(3) 10_655 . ? Si3 Si1 Si2 107.33(6) 10_655 . ? Si3 Si1 Si2 107.33(6) . . ? Si39 Si1 Si2 55.36(14) 10_655 . ? Si39 Si1 Si2 55.36(14) . . ? Si3 Si1 Si29 55.91(6) 10_655 . ? Si3 Si1 Si29 55.91(6) . . ? Si39 Si1 Si29 107.44(18) 10_655 . ? Si39 Si1 Si29 107.44(18) . . ? Si2 Si1 Si29 136.7(2) . . ? O2 Si2 C21 105.2(4) . 10_655 ? O2 Si2 C21 105.2(4) . . ? C21 Si2 C21 107.0(8) 10_655 . ? O2 Si2 Si39 91.0(2) . 10_655 ? C21 Si2 Si39 64.3(4) 10_655 10_655 ? C21 Si2 Si39 163.4(5) . 10_655 ? O2 Si2 C319 106.4(13) . 10_655 ? C21 Si2 C319 12.9(11) 10_655 10_655 ? C21 Si2 C319 118.2(10) . 10_655 ? Si39 Si2 C319 51.8(11) 10_655 10_655 ? O2 Si2 Si1 112.90(18) . . ? C21 Si2 Si1 112.9(3) 10_655 . ? C21 Si2 Si1 112.9(3) . . ? Si39 Si2 Si1 62.10(18) 10_655 . ? C319 Si2 Si1 101.3(9) 10_655 . ? O3 Si3 C31 106.3(4) . . ? O3 Si3 C32 105.8(4) . . ? C31 Si3 C32 107.8(4) . . ? O3 Si3 Si1 113.56(15) . . ? C31 Si3 Si1 110.8(4) . . ? C32 Si3 Si1 112.3(4) . . ? C20 O2 Si2 121.2(6) . . ? C20 O2 Sr1 122.1(6) . . ? Si2 O2 Sr1 116.7(2) . . ? C30 O3 Si3 122.9(4) . . ? C30 O3 Sr1 121.3(3) . . ? Si3 O3 Sr1 115.79(18) . . ? C209 C20 O2 120(2) 9_666 . ? O29 Si29 C219 103.8(16) . 10_655 ? O29 Si29 C219 103.8(15) . . ? C219 Si29 C219 107(2) 10_655 . ? O29 Si29 C32 106.4(4) . 10_655 ? C219 Si29 C32 15.4(9) 10_655 10_655 ? C219 Si29 C32 119.7(13) . 10_655 ? O29 Si29 Si3 91.5(4) . 10_655 ? C219 Si29 Si3 65.6(10) 10_655 10_655 ? C219 Si29 Si3 164.4(16) . 10_655 ? C32 Si29 Si3 50.9(2) 10_655 10_655 ? O29 Si29 Si1 112.1(7) . . ? C219 Si29 Si1 114.7(9) 10_655 . ? C219 Si29 Si1 114.7(9) . . ? C32 Si29 Si1 100.2(3) 10_655 . ? Si3 Si29 Si1 61.00(18) 10_655 . ? O39 Si39 C319 108.3(15) . . ? O39 Si39 C329 103.1(18) . . ? C319 Si39 C329 103.7(16) . . ? O39 Si39 Si1 113.3(5) . . ? C319 Si39 Si1 111.3(11) . . ? C329 Si39 Si1 116.4(12) . . ? C209 O29 Si29 122.0(15) . . ? C209 O29 Sr1 120.3(14) . . ? Si29 O29 Sr1 117.7(9) . . ? Si39 O39 Sr1 116.4(7) . . ? C20 C209 O29 121(3) 9_666 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.57 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.660 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.053 # Attachment 'LJHW_Krempner_9final_0m.cif' data_ljhw_krempner_9_0m _database_code_depnum_ccdc_archive 'CCDC 829369' #TrackingRef 'LJHW_Krempner_9final_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H54 Mg O6 Si8' _chemical_formula_weight 615.64 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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8056(10) _cell_length_b 12.7931(13) _cell_length_c 13.7123(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.4620(10) _cell_angle_gamma 90.00 _cell_volume 1712.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1967 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 21.50 _exptl_crystal_description block/needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9381 _exptl_absorpt_correction_T_max 0.9537 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15332 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 24.08 _reflns_number_total 2727 _reflns_number_gt 2041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0232P)^2^+1.3161P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0006(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2727 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _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 C1 C -0.2108(4) 0.3757(3) 0.2727(3) 0.0488(10) Uani 1 1 d . . . H1A H -0.2640 0.4334 0.2970 0.073 Uiso 1 1 calc R . . H1B H -0.1962 0.3219 0.3235 0.073 Uiso 1 1 calc R . . H1C H -0.2610 0.3455 0.2142 0.073 Uiso 1 1 calc R . . C2 C 0.4031(3) 0.3110(2) 0.0893(3) 0.0444(9) Uani 1 1 d . . . H2A H 0.3619 0.2820 0.0273 0.067 Uiso 1 1 calc R . . H2B H 0.4343 0.2539 0.1336 0.067 Uiso 1 1 calc R . . H2C H 0.4814 0.3551 0.0770 0.067 Uiso 1 1 calc R . . C3 C -0.1714(3) 0.1692(2) 0.0780(2) 0.0406(9) Uani 1 1 d . . . H3A H -0.2386 0.2212 0.0950 0.061 Uiso 1 1 calc R . . H3B H -0.1587 0.1167 0.1301 0.061 Uiso 1 1 calc R . . H3C H -0.2044 0.1351 0.0162 0.061 Uiso 1 1 calc R . . C4 C 0.1005(3) 0.1378(2) 0.0017(2) 0.0315(8) Uani 1 1 d . . . H4A H 0.0463 0.1103 -0.0565 0.047 Uiso 1 1 calc R . . H4B H 0.1264 0.0802 0.0468 0.047 Uiso 1 1 calc R . . H4C H 0.1832 0.1716 -0.0180 0.047 Uiso 1 1 calc R . . C5 C 0.3732(4) 0.4728(3) 0.2424(3) 0.0500(10) Uani 1 1 d . . . H5A H 0.4579 0.4969 0.2171 0.075 Uiso 1 1 calc R . . H5B H 0.3956 0.4308 0.3015 0.075 Uiso 1 1 calc R . . H5C H 0.3183 0.5334 0.2584 0.075 Uiso 1 1 calc R . . C6 C 0.3104(3) 0.5441(3) 0.0181(3) 0.0528(11) Uani 1 1 d . . . H6A H 0.3561 0.5870 0.0707 0.079 Uiso 1 1 calc R . . H6B H 0.2656 0.5897 -0.0328 0.079 Uiso 1 1 calc R . . H6C H 0.3783 0.5003 -0.0104 0.079 Uiso 1 1 calc R . . C7 C -0.1709(4) 0.5936(3) 0.1596(3) 0.0543(11) Uani 1 1 d . . . H7A H -0.2597 0.5646 0.1730 0.081 Uiso 1 1 calc R . . H7B H -0.1829 0.6381 0.1012 0.081 Uiso 1 1 calc R . . H7C H -0.1331 0.6352 0.2158 0.081 Uiso 1 1 calc R . . C8 C -0.1073(4) 0.3022(3) -0.1125(2) 0.0527(11) Uani 1 1 d . . . H8A H -0.0480 0.2535 -0.1440 0.079 Uiso 1 1 calc R . . H8B H -0.1262 0.3633 -0.1548 0.079 Uiso 1 1 calc R . . H8C H -0.1936 0.2673 -0.1019 0.079 Uiso 1 1 calc R . . C9 C 0.0260(4) 0.5102(3) 0.3465(2) 0.0520(10) Uani 1 1 d . . . H9A H 0.1048 0.5503 0.3282 0.078 Uiso 1 1 calc R . . H9B H 0.0544 0.4660 0.4032 0.078 Uiso 1 1 calc R . . H9C H -0.0460 0.5583 0.3632 0.078 Uiso 1 1 calc R . . Mg1 Mg 0.0000 0.5000 0.0000 0.0188(3) Uani 1 2 d S . . O1 O -0.0775(2) 0.50888(15) 0.14283(14) 0.0294(5) Uani 1 1 d . . . O2 O 0.20879(18) 0.47837(14) 0.05741(14) 0.0273(5) Uani 1 1 d . . . O3 O -0.0386(2) 0.33580(14) -0.01818(13) 0.0269(5) Uani 1 1 d . . . Si1 Si -0.04145(10) 0.42590(7) 0.24107(6) 0.0310(2) Uani 1 1 d . . . Si2 Si 0.27293(9) 0.39142(6) 0.14691(7) 0.0294(2) Uani 1 1 d . . . Si3 Si 0.10585(9) 0.29267(6) 0.20986(6) 0.0267(2) Uani 1 1 d . . . Si4 Si -0.00398(8) 0.23553(6) 0.06400(6) 0.0223(2) Uani 1 1 d . . . 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 C1 0.062(3) 0.045(2) 0.044(2) 0.0107(17) 0.028(2) 0.0128(19) C2 0.030(2) 0.033(2) 0.069(3) 0.0115(18) 0.0007(18) 0.0011(16) C3 0.038(2) 0.0333(19) 0.050(2) 0.0047(17) 0.0025(17) -0.0092(16) C4 0.042(2) 0.0267(17) 0.0252(17) -0.0012(14) 0.0012(15) 0.0005(15) C5 0.051(2) 0.032(2) 0.061(3) 0.0035(18) -0.0297(19) -0.0042(17) C6 0.027(2) 0.052(2) 0.077(3) 0.034(2) -0.0023(19) -0.0059(17) C7 0.078(3) 0.047(2) 0.041(2) 0.0120(18) 0.026(2) 0.038(2) C8 0.084(3) 0.033(2) 0.034(2) -0.0004(16) -0.0315(19) -0.0069(19) C9 0.086(3) 0.041(2) 0.029(2) -0.0052(17) 0.0004(19) 0.018(2) Mg1 0.0200(7) 0.0178(7) 0.0183(7) 0.0016(6) -0.0002(6) 0.0006(6) O1 0.0390(13) 0.0250(11) 0.0252(11) 0.0055(9) 0.0089(10) 0.0132(10) O2 0.0167(11) 0.0263(11) 0.0377(13) 0.0114(10) -0.0032(9) -0.0038(9) O3 0.0356(12) 0.0190(11) 0.0235(11) 0.0031(9) -0.0105(9) -0.0031(9) Si1 0.0454(6) 0.0276(5) 0.0207(5) 0.0036(4) 0.0068(4) 0.0072(4) Si2 0.0271(5) 0.0222(5) 0.0361(5) 0.0043(4) -0.0120(4) 0.0008(4) Si3 0.0354(5) 0.0229(5) 0.0206(4) 0.0015(4) -0.0035(4) 0.0034(4) Si4 0.0272(5) 0.0177(4) 0.0216(4) 0.0022(3) -0.0004(3) -0.0017(4) _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 C1 Si1 1.870(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 Si2 1.872(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si4 1.874(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 Si4 1.874(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Si2 1.876(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 O2 1.447(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O1 1.451(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O3 1.465(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 Si1 1.873(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? Mg1 O2 2.1403(18) 3_565 ? Mg1 O2 2.1403(18) . ? Mg1 O3 2.1448(18) 3_565 ? Mg1 O3 2.1448(18) . ? Mg1 O1 2.1701(18) 3_565 ? Mg1 O1 2.1701(18) . ? O1 Si1 1.725(2) . ? O2 Si2 1.730(2) . ? O3 Si4 1.7198(19) . ? Si1 Si3 2.3005(12) . ? Si2 Si3 2.3009(12) . ? Si3 Si4 2.2988(11) . ? 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 Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si2 C2 H2A 109.5 . . ? Si2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si4 C3 H3A 109.5 . . ? Si4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si4 C4 H4A 109.5 . . ? Si4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O2 C6 H6A 109.5 . . ? O2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 Mg1 O2 180.0 3_565 . ? O2 Mg1 O3 93.91(7) 3_565 3_565 ? O2 Mg1 O3 86.09(7) . 3_565 ? O2 Mg1 O3 86.09(7) 3_565 . ? O2 Mg1 O3 93.91(7) . . ? O3 Mg1 O3 180.0 3_565 . ? O2 Mg1 O1 94.57(7) 3_565 3_565 ? O2 Mg1 O1 85.43(7) . 3_565 ? O3 Mg1 O1 94.77(7) 3_565 3_565 ? O3 Mg1 O1 85.23(7) . 3_565 ? O2 Mg1 O1 85.44(7) 3_565 . ? O2 Mg1 O1 94.56(7) . . ? O3 Mg1 O1 85.23(7) 3_565 . ? O3 Mg1 O1 94.77(7) . . ? O1 Mg1 O1 180.0 3_565 . ? C7 O1 Si1 114.92(18) . . ? C7 O1 Mg1 117.53(17) . . ? Si1 O1 Mg1 127.54(10) . . ? C6 O2 Si2 114.95(17) . . ? C6 O2 Mg1 117.13(17) . . ? Si2 O2 Mg1 127.92(10) . . ? C8 O3 Si4 113.90(17) . . ? C8 O3 Mg1 116.83(17) . . ? Si4 O3 Mg1 129.25(10) . . ? O1 Si1 C1 105.81(13) . . ? O1 Si1 C9 106.23(13) . . ? C1 Si1 C9 105.93(17) . . ? O1 Si1 Si3 113.34(8) . . ? C1 Si1 Si3 112.08(11) . . ? C9 Si1 Si3 112.86(12) . . ? O2 Si2 C2 105.71(13) . . ? O2 Si2 C5 105.61(13) . . ? C2 Si2 C5 105.45(16) . . ? O2 Si2 Si3 113.29(7) . . ? C2 Si2 Si3 113.28(11) . . ? C5 Si2 Si3 112.79(13) . . ? Si4 Si3 Si1 98.45(4) . . ? Si4 Si3 Si2 98.02(4) . . ? Si1 Si3 Si2 98.34(4) . . ? O3 Si4 C4 106.34(12) . . ? O3 Si4 C3 106.54(13) . . ? C4 Si4 C3 105.47(14) . . ? O3 Si4 Si3 112.33(7) . . ? C4 Si4 Si3 112.21(10) . . ? C3 Si4 Si3 113.40(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.08 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.301 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.058