data_sad1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 Ca O11 Si3 Sn' _chemical_formula_weight 421.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' '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' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 14.4783(12) _cell_length_b 11.5879(10) _cell_length_c 5.2292(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 877.32(12) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description grain _exptl_crystal_colour No _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 3.961 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7595 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 33.50 _reflns_number_total 1652 _reflns_number_gt 1531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+5.6610P] 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 1652 _refine_ls_number_parameters 84 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.224 _refine_ls_restrained_S_all 1.224 _refine_ls_shift/su_max 0.001 _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 Ca1 Ca 0.40211(7) 0.7500 1.2500 0.01227(19) Uani 1 2 d S . . Sn1 Sn 0.5000 1.0000 1.0000 0.00821(10) Uani 1 2 d S . . Si1 Si 0.56434(9) 0.7500 0.7500 0.0064(2) Uani 1 2 d S . . Si2 Si 0.64236(6) 0.96853(8) 0.50250(17) 0.00628(17) Uani 1 1 d . . . O1 O 0.7500 1.0000 0.5464(8) 0.0126(7) Uani 1 2 d S . . O2 O 0.63018(18) 0.8336(2) 0.5818(5) 0.0115(5) Uani 1 1 d . . . O3 O 0.57856(17) 1.0474(2) 0.6864(5) 0.0086(4) Uani 1 1 d . . . O4 O 0.50114(18) 0.8265(2) 0.9371(5) 0.0105(5) Uani 1 1 d . . . O5 O 0.38039(17) 1.0120(2) 0.7964(5) 0.0104(5) Uani 1 1 d . . . O6 O 0.2871(2) 0.8197(3) 0.9776(7) 0.0242(7) Uani 1 1 d D . . H1 H 0.318(5) 0.882(4) 0.924(15) 0.05(2) Uiso 1 1 d D . . H2 H 0.227(2) 0.834(10) 0.994(18) 0.08(3) Uiso 1 1 d 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 Ca1 0.0179(4) 0.0081(4) 0.0108(4) 0.0015(3) 0.000 0.000 Sn1 0.00978(15) 0.00692(16) 0.00793(16) -0.00044(10) 0.00068(11) -0.00018(10) Si1 0.0083(5) 0.0044(5) 0.0064(5) -0.0005(4) 0.000 0.000 Si2 0.0069(4) 0.0059(4) 0.0060(4) 0.0006(3) 0.0007(3) -0.0004(3) O1 0.0060(14) 0.0195(19) 0.0123(16) 0.000 0.000 -0.0041(12) O2 0.0116(11) 0.0057(10) 0.0172(12) 0.0021(9) 0.0060(9) 0.0005(8) O3 0.0118(10) 0.0065(10) 0.0075(10) -0.0006(8) 0.0018(8) 0.0004(8) O4 0.0148(11) 0.0050(10) 0.0116(11) -0.0021(9) 0.0048(9) 0.0000(8) O5 0.0089(10) 0.0161(12) 0.0063(10) 0.0006(8) -0.0013(8) -0.0012(9) O6 0.0173(14) 0.0277(17) 0.0277(16) 0.0061(13) -0.0030(12) -0.0058(13) _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 O6 2.335(3) . ? Ca1 O6 2.335(4) 4_567 ? Ca1 O4 2.349(3) 4_567 ? Ca1 O4 2.349(3) . ? Ca1 O3 2.388(2) 5_677 ? Ca1 O3 2.388(2) 8_656 ? Ca1 Sn1 3.4800(5) . ? Ca1 Sn1 3.4800(5) 4_567 ? Ca1 Si1 3.5147(11) 1_556 ? Ca1 Si1 3.5147(11) . ? Ca1 Si2 3.5677(10) 8_656 ? Ca1 Si2 3.5677(10) 5_677 ? Sn1 O4 2.037(3) 5_677 ? Sn1 O4 2.037(3) . ? Sn1 O5 2.038(3) . ? Sn1 O5 2.038(3) 5_677 ? Sn1 O3 2.070(2) 5_677 ? Sn1 O3 2.070(2) . ? Sn1 Ca1 3.4800(5) 5_677 ? Si1 O4 1.606(3) 4_566 ? Si1 O4 1.606(3) . ? Si1 O2 1.619(3) . ? Si1 O2 1.619(3) 4_566 ? Si1 Ca1 3.5147(11) 1_554 ? Si2 O5 1.613(3) 5_676 ? Si2 O3 1.616(3) . ? Si2 O1 1.6169(11) . ? Si2 O2 1.627(3) . ? Si2 Ca1 3.5677(10) 5_677 ? O1 Si2 1.6169(11) 2_675 ? O3 Ca1 2.388(2) 5_677 ? O5 Si2 1.613(3) 5_676 ? 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 O6 Ca1 O6 89.05(17) . 4_567 ? O6 Ca1 O4 172.10(11) . 4_567 ? O6 Ca1 O4 83.10(11) 4_567 4_567 ? O6 Ca1 O4 83.10(11) . . ? O6 Ca1 O4 172.10(11) 4_567 . ? O4 Ca1 O4 104.77(14) 4_567 . ? O6 Ca1 O3 80.12(11) . 5_677 ? O6 Ca1 O3 109.79(11) 4_567 5_677 ? O4 Ca1 O3 101.69(9) 4_567 5_677 ? O4 Ca1 O3 69.78(9) . 5_677 ? O6 Ca1 O3 109.79(11) . 8_656 ? O6 Ca1 O3 80.12(11) 4_567 8_656 ? O4 Ca1 O3 69.78(9) 4_567 8_656 ? O4 Ca1 O3 101.69(9) . 8_656 ? O3 Ca1 O3 166.54(13) 5_677 8_656 ? O6 Ca1 Sn1 76.90(8) . . ? O6 Ca1 Sn1 143.84(9) 4_567 . ? O4 Ca1 Sn1 109.10(7) 4_567 . ? O4 Ca1 Sn1 34.48(6) . . ? O3 Ca1 Sn1 35.51(6) 5_677 . ? O3 Ca1 Sn1 135.93(7) 8_656 . ? O6 Ca1 Sn1 143.84(9) . 4_567 ? O6 Ca1 Sn1 76.90(8) 4_567 4_567 ? O4 Ca1 Sn1 34.48(6) 4_567 4_567 ? O4 Ca1 Sn1 109.10(7) . 4_567 ? O3 Ca1 Sn1 135.93(7) 5_677 4_567 ? O3 Ca1 Sn1 35.51(6) 8_656 4_567 ? Sn1 Ca1 Sn1 131.93(3) . 4_567 ? O6 Ca1 Si1 158.48(9) . 1_556 ? O6 Ca1 Si1 91.30(9) 4_567 1_556 ? O4 Ca1 Si1 22.18(6) 4_567 1_556 ? O4 Ca1 Si1 96.33(8) . 1_556 ? O3 Ca1 Si1 79.52(6) 5_677 1_556 ? O3 Ca1 Si1 91.45(6) 8_656 1_556 ? Sn1 Ca1 Si1 90.42(2) . 1_556 ? Sn1 Ca1 Si1 56.521(11) 4_567 1_556 ? O6 Ca1 Si1 91.30(9) . . ? O6 Ca1 Si1 158.48(9) 4_567 . ? O4 Ca1 Si1 96.33(8) 4_567 . ? O4 Ca1 Si1 22.18(6) . . ? O3 Ca1 Si1 91.45(6) 5_677 . ? O3 Ca1 Si1 79.52(6) 8_656 . ? Sn1 Ca1 Si1 56.521(10) . . ? Sn1 Ca1 Si1 90.42(2) 4_567 . ? Si1 Ca1 Si1 96.13(4) 1_556 . ? O6 Ca1 Si2 88.06(9) . 8_656 ? O6 Ca1 Si2 77.09(10) 4_567 8_656 ? O4 Ca1 Si2 91.02(6) 4_567 8_656 ? O4 Ca1 Si2 101.68(7) . 8_656 ? O3 Ca1 Si2 166.08(6) 5_677 8_656 ? O3 Ca1 Si2 21.83(6) 8_656 8_656 ? Sn1 Ca1 Si2 134.291(18) . 8_656 ? Sn1 Ca1 Si2 56.543(15) 4_567 8_656 ? Si1 Ca1 Si2 112.98(2) 1_556 8_656 ? Si1 Ca1 Si2 81.416(18) . 8_656 ? O6 Ca1 Si2 77.09(10) . 5_677 ? O6 Ca1 Si2 88.06(9) 4_567 5_677 ? O4 Ca1 Si2 101.68(7) 4_567 5_677 ? O4 Ca1 Si2 91.02(6) . 5_677 ? O3 Ca1 Si2 21.83(6) 5_677 5_677 ? O3 Ca1 Si2 166.08(6) 8_656 5_677 ? Sn1 Ca1 Si2 56.543(16) . 5_677 ? Sn1 Ca1 Si2 134.291(18) 4_567 5_677 ? Si1 Ca1 Si2 81.416(18) 1_556 5_677 ? Si1 Ca1 Si2 112.98(2) . 5_677 ? Si2 Ca1 Si2 159.21(5) 8_656 5_677 ? O4 Sn1 O4 180.0 5_677 . ? O4 Sn1 O5 90.59(11) 5_677 . ? O4 Sn1 O5 89.41(11) . . ? O4 Sn1 O5 89.41(11) 5_677 5_677 ? O4 Sn1 O5 90.59(11) . 5_677 ? O5 Sn1 O5 180.000(1) . 5_677 ? O4 Sn1 O3 97.44(10) 5_677 5_677 ? O4 Sn1 O3 82.56(10) . 5_677 ? O5 Sn1 O3 88.00(10) . 5_677 ? O5 Sn1 O3 92.00(10) 5_677 5_677 ? O4 Sn1 O3 82.56(10) 5_677 . ? O4 Sn1 O3 97.44(10) . . ? O5 Sn1 O3 92.00(10) . . ? O5 Sn1 O3 88.00(10) 5_677 . ? O3 Sn1 O3 180.000(1) 5_677 . ? O4 Sn1 Ca1 139.26(7) 5_677 . ? O4 Sn1 Ca1 40.74(7) . . ? O5 Sn1 Ca1 84.65(7) . . ? O5 Sn1 Ca1 95.35(7) 5_677 . ? O3 Sn1 Ca1 42.08(7) 5_677 . ? O3 Sn1 Ca1 137.92(7) . . ? O4 Sn1 Ca1 40.74(7) 5_677 5_677 ? O4 Sn1 Ca1 139.26(7) . 5_677 ? O5 Sn1 Ca1 95.35(7) . 5_677 ? O5 Sn1 Ca1 84.65(7) 5_677 5_677 ? O3 Sn1 Ca1 137.92(7) 5_677 5_677 ? O3 Sn1 Ca1 42.08(7) . 5_677 ? Ca1 Sn1 Ca1 180.0 . 5_677 ? O4 Si1 O4 110.6(2) 4_566 . ? O4 Si1 O2 109.56(15) 4_566 . ? O4 Si1 O2 109.63(13) . . ? O4 Si1 O2 109.63(13) 4_566 4_566 ? O4 Si1 O2 109.56(15) . 4_566 ? O2 Si1 O2 107.9(2) . 4_566 ? O4 Si1 Ca1 33.50(10) 4_566 1_554 ? O4 Si1 Ca1 94.16(11) . 1_554 ? O2 Si1 Ca1 89.39(10) . 1_554 ? O2 Si1 Ca1 142.89(9) 4_566 1_554 ? O4 Si1 Ca1 94.16(11) 4_566 . ? O4 Si1 Ca1 33.50(10) . . ? O2 Si1 Ca1 142.89(9) . . ? O2 Si1 Ca1 89.39(10) 4_566 . ? Ca1 Si1 Ca1 96.13(4) 1_554 . ? O5 Si2 O3 112.37(14) 5_676 . ? O5 Si2 O1 107.62(17) 5_676 . ? O3 Si2 O1 109.81(14) . . ? O5 Si2 O2 111.08(15) 5_676 . ? O3 Si2 O2 109.23(14) . . ? O1 Si2 O2 106.56(12) . . ? O5 Si2 Ca1 100.75(10) 5_676 5_677 ? O3 Si2 Ca1 33.32(9) . 5_677 ? O1 Si2 Ca1 85.19(6) . 5_677 ? O2 Si2 Ca1 140.03(11) . 5_677 ? Si2 O1 Si2 163.7(3) . 2_675 ? Si1 O2 Si2 141.04(17) . . ? Si2 O3 Sn1 129.46(14) . . ? Si2 O3 Ca1 124.86(14) . 5_677 ? Sn1 O3 Ca1 102.41(10) . 5_677 ? Si1 O4 Sn1 130.34(15) . . ? Si1 O4 Ca1 124.32(14) . . ? Sn1 O4 Ca1 104.78(11) . . ? Si2 O5 Sn1 133.58(15) 5_676 . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 33.50 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.030 _refine_diff_density_min -1.425 _refine_diff_density_rms 0.198