# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Ulrich Kortz' _publ_contact_author_email U.KORTZ@JACOBS-UNIVERSITY.DE _publ_section_title ; The first 3-dimensional assemblies of organotin-functionalized polyanions ; loop_ _publ_author_name 'Ulrich Kortz' 'Michael H. Dickman' 'Luis Fernando Piedra-Garza' 'Santiago Reinoso' 'Michael Sanguineti' # Attachment 'G-1_Rxn08-02_uk.cif' data_0802 _database_code_depnum_ccdc_archive 'CCDC 729710' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H52 N6 As Na O45 Sn3 W9' _chemical_formula_weight 3061.2 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 17.6040(9) _cell_length_b 17.6040(9) _cell_length_c 17.6040(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5455.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1091 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 18.42 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 3.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5536 _exptl_absorpt_coefficient_mu 20.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0512 _exptl_absorpt_correction_T_max 0.2543 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75800 _diffrn_reflns_av_R_equivalents 0.2948 _diffrn_reflns_av_sigmaI/netI 0.0873 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 24.09 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.09 _diffrn_measured_fraction_theta_full 0.986 _reflns_number_total 2850 _reflns_number_gt 2122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0470P)^2^+80.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_ls_number_reflns 2850 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.704 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.270 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 W1 W 0.18285(6) 0.91307(6) 0.96760(6) 0.0329(3) Uani 1 1 d . . . W2 W 0.12651(6) 1.08789(6) 0.86390(6) 0.0326(3) Uani 1 1 d . . . W3 W 0.00600(6) 0.91295(6) 0.84960(6) 0.0352(3) Uani 1 1 d . . . O1T O 0.2458(9) 0.8620(10) 0.9149(9) 0.037(4) Uiso 1 1 d . . . O1A O 0.0919(11) 0.8861(10) 0.9063(11) 0.048(5) Uiso 1 1 d . . . O2T O 0.1761(9) 1.0093(9) 0.9154(9) 0.031(4) Uiso 1 1 d . . . O2A O 0.3262(9) 0.9115(9) 1.2777(9) 0.033(4) Uiso 1 1 d . . . O3T O 0.0248(10) 0.8652(10) 0.7685(10) 0.045(5) Uiso 1 1 d . . . O3A O -0.0459(10) 0.8327(10) 0.9064(10) 0.041(5) Uiso 1 1 d . . . O1S1 O 0.2527(9) 0.9590(9) 1.0367(9) 0.035(4) Uiso 1 1 d . . . O1A1 O -0.0349(8) 0.9651(8) 0.9651(8) 0.020(6) Uiso 1 3 d S . . O12 O 0.1540(9) 0.8403(9) 1.0427(9) 0.037(4) Uiso 1 1 d . . . O2S1 O 0.1632(9) 0.9109(10) 1.1765(9) 0.040(4) Uiso 1 1 d . . . O2A1 O 0.0960(8) 0.9673(9) 1.0521(8) 0.028(4) Uiso 1 1 d . . . O23 O 0.0537(9) 1.0048(9) 0.8352(9) 0.035(4) Uiso 1 1 d . . . O3S1 O 0.4052(12) 0.9558(12) 1.1062(12) 0.067(6) Uiso 1 1 d . . . As1 As 0.02129(13) 1.02129(13) 1.02129(13) 0.0239(9) Uani 1 3 d S . . Sn1 Sn 0.28135(10) 0.93564(10) 1.15073(10) 0.0347(5) Uani 1 1 d . . . C1S1 C 0.2783(17) 1.0479(16) 1.1882(16) 0.049(8) Uiso 1 1 d . . . H1S1 H 0.2393 1.0759 1.1601 0.074 Uiso 1 1 calc R . . H1S2 H 0.3279 1.0717 1.1797 0.074 Uiso 1 1 calc R . . H1S3 H 0.2664 1.0490 1.2426 0.074 Uiso 1 1 calc R . . C2S1 C 0.3071(16) 0.8190(16) 1.1373(17) 0.052(8) Uiso 1 1 d . . . H2S1 H 0.2744 0.7972 1.0978 0.078 Uiso 1 1 calc R . . H2S2 H 0.2985 0.7924 1.1854 0.078 Uiso 1 1 calc R . . H2S3 H 0.3605 0.8133 1.1223 0.078 Uiso 1 1 calc R . . C1G1 C 0.2246(14) 0.7246(14) 0.7754(14) 0.031(10) Uiso 1 3 d S . . N1G1 N 0.2793(12) 0.7205(13) 0.8254(12) 0.043(6) Uiso 1 1 d . . . H1G1 H 0.3134 0.6841 0.8221 0.052 Uiso 1 1 calc R . . H1G2 H 0.2820 0.7542 0.8622 0.052 Uiso 1 1 calc R . . O1W O 0.319(3) 0.102(3) -0.013(3) 0.200(19) Uiso 1 1 d . . . O2W O 0.4614(18) 0.1007(17) 0.1069(17) 0.115(10) Uiso 1 1 d . . . O3W O 0.502(3) 0.815(3) 0.175(3) 0.134(18) Uiso 0.67 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 W1 0.0339(6) 0.0340(6) 0.0308(6) -0.0023(5) 0.0009(5) 0.0056(5) W2 0.0346(6) 0.0351(6) 0.0280(6) 0.0025(5) 0.0045(5) 0.0017(5) W3 0.0376(7) 0.0374(6) 0.0306(6) -0.0065(5) -0.0028(5) -0.0003(5) As1 0.0239(9) 0.0239(9) 0.0239(9) -0.0012(10) -0.0012(10) -0.0012(10) Sn1 0.0365(11) 0.0335(11) 0.0342(11) -0.0028(8) -0.0016(8) 0.0012(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 W1 O1T 1.701(17) . ? W1 O1S1 1.908(16) . ? W1 O12 1.911(16) . ? W1 O2T 1.931(16) . ? W1 O1A 1.989(19) . ? W1 O2A1 2.337(15) . ? W2 O2A 1.730(16) 2_574 ? W2 O2S1 1.793(17) 5_465 ? W2 O2T 1.870(16) . ? W2 O12 1.924(17) 5_465 ? W2 O23 2.010(16) . ? W2 O2A1 2.247(15) 5_465 ? W3 O3T 1.690(18) . ? W3 O23 1.840(16) . ? W3 O1A 1.871(19) . ? W3 O3A 1.920(17) 5_465 ? W3 O3A 1.958(17) . ? W3 O1A1 2.343(13) . ? O2A W2 1.730(15) 2_575 ? O2A Sn1 2.409(16) . ? O3A W3 1.920(17) 9_456 ? O1S1 Sn1 2.111(16) . ? O1A1 As1 1.71(2) . ? O1A1 W3 2.343(13) 9_456 ? O1A1 W3 2.343(13) 5_465 ? O12 W2 1.924(17) 9_456 ? O2S1 W2 1.793(17) 9_456 ? O2S1 Sn1 2.173(17) . ? O2A1 As1 1.711(15) . ? O2A1 W2 2.247(15) 9_456 ? O3S1 Sn1 2.34(2) . ? As1 O2A1 1.711(15) 9_456 ? As1 O2A1 1.711(15) 5_465 ? Sn1 C1S1 2.08(3) . ? Sn1 C2S1 2.12(3) . ? C1S1 H1S1 0.9800 . ? C1S1 H1S2 0.9800 . ? C1S1 H1S3 0.9800 . ? C2S1 H2S1 0.9800 . ? C2S1 H2S2 0.9800 . ? C2S1 H2S3 0.9800 . ? C1G1 N1G1 1.31(2) 11_466 ? C1G1 N1G1 1.31(2) . ? C1G1 N1G1 1.31(2) 8_656 ? N1G1 H1G1 0.8800 . ? N1G1 H1G2 0.8800 . ? 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 O1T W1 O1S1 98.7(7) . . ? O1T W1 O12 101.3(8) . . ? O1S1 W1 O12 90.8(7) . . ? O1T W1 O2T 104.1(7) . . ? O1S1 W1 O2T 88.4(7) . . ? O12 W1 O2T 154.4(7) . . ? O1T W1 O1A 95.9(8) . . ? O1S1 W1 O1A 164.9(7) . . ? O12 W1 O1A 90.1(7) . . ? O2T W1 O1A 84.3(7) . . ? O1T W1 O2A1 171.4(7) . . ? O1S1 W1 O2A1 80.9(6) . . ? O12 W1 O2A1 70.1(6) . . ? O2T W1 O2A1 84.5(6) . . ? O1A W1 O2A1 85.2(7) . . ? O2A W2 O2S1 99.4(8) 2_574 5_465 ? O2A W2 O2T 101.9(7) 2_574 . ? O2S1 W2 O2T 95.4(7) 5_465 . ? O2A W2 O12 100.1(7) 2_574 5_465 ? O2S1 W2 O12 91.6(7) 5_465 5_465 ? O2T W2 O12 155.5(7) . 5_465 ? O2A W2 O23 95.2(7) 2_574 . ? O2S1 W2 O23 165.2(7) 5_465 . ? O2T W2 O23 83.2(7) . . ? O12 W2 O23 84.1(6) 5_465 . ? O2A W2 O2A1 171.9(7) 2_574 5_465 ? O2S1 W2 O2A1 82.2(7) 5_465 5_465 ? O2T W2 O2A1 85.8(6) . 5_465 ? O12 W2 O2A1 71.9(6) 5_465 5_465 ? O23 W2 O2A1 83.0(6) . 5_465 ? O3T W3 O23 103.4(8) . . ? O3T W3 O1A 99.6(9) . . ? O23 W3 O1A 85.8(8) . . ? O3T W3 O3A 103.6(8) . 5_465 ? O23 W3 O3A 93.6(7) . 5_465 ? O1A W3 O3A 156.3(8) . 5_465 ? O3T W3 O3A 99.4(8) . . ? O23 W3 O3A 156.6(7) . . ? O1A W3 O3A 85.5(8) . . ? O3A W3 O3A 85.8(10) 5_465 . ? O3T W3 O1A1 171.1(8) . . ? O23 W3 O1A1 85.2(6) . . ? O1A W3 O1A1 83.4(7) . . ? O3A W3 O1A1 72.9(6) 5_465 . ? O3A W3 O1A1 72.3(6) . . ? W3 O1A W1 151.6(10) . . ? W2 O2T W1 155.3(9) . . ? W2 O2A Sn1 166.0(9) 2_575 . ? W3 O3A W3 122.0(9) 9_456 . ? W1 O1S1 Sn1 132.7(8) . . ? As1 O1A1 W3 123.3(5) . 9_456 ? As1 O1A1 W3 123.3(5) . 5_465 ? W3 O1A1 W3 92.7(7) 9_456 5_465 ? As1 O1A1 W3 123.3(5) . . ? W3 O1A1 W3 92.7(7) 9_456 . ? W3 O1A1 W3 92.7(7) 5_465 . ? W1 O12 W2 123.1(9) . 9_456 ? W2 O2S1 Sn1 134.3(9) 9_456 . ? As1 O2A1 W2 125.9(8) . 9_456 ? As1 O2A1 W1 121.8(8) . . ? W2 O2A1 W1 94.7(6) 9_456 . ? W3 O23 W2 153.6(9) . . ? O2A1 As1 O2A1 111.0(5) 9_456 5_465 ? O2A1 As1 O2A1 111.0(5) 9_456 . ? O2A1 As1 O2A1 111.0(5) 5_465 . ? O2A1 As1 O1A1 107.9(5) 9_456 . ? O2A1 As1 O1A1 107.9(5) 5_465 . ? O2A1 As1 O1A1 107.8(5) . . ? C1S1 Sn1 O1S1 96.4(9) . . ? C1S1 Sn1 C2S1 163.9(11) . . ? O1S1 Sn1 C2S1 97.7(9) . . ? C1S1 Sn1 O2S1 95.7(9) . . ? O1S1 Sn1 O2S1 90.5(6) . . ? C2S1 Sn1 O2S1 91.9(9) . . ? C1S1 Sn1 O3S1 89.2(10) . . ? O1S1 Sn1 O3S1 82.8(7) . . ? C2S1 Sn1 O3S1 84.9(10) . . ? O2S1 Sn1 O3S1 172.1(7) . . ? C1S1 Sn1 O2A 83.2(9) . . ? O1S1 Sn1 O2A 174.6(6) . . ? C2S1 Sn1 O2A 82.1(9) . . ? O2S1 Sn1 O2A 94.9(6) . . ? O3S1 Sn1 O2A 91.8(7) . . ? Sn1 C1S1 H1S1 109.5 . . ? Sn1 C1S1 H1S2 109.5 . . ? H1S1 C1S1 H1S2 109.5 . . ? Sn1 C1S1 H1S3 109.5 . . ? H1S1 C1S1 H1S3 109.5 . . ? H1S2 C1S1 H1S3 109.5 . . ? Sn1 C2S1 H2S1 109.5 . . ? Sn1 C2S1 H2S2 109.5 . . ? H2S1 C2S1 H2S2 109.5 . . ? Sn1 C2S1 H2S3 109.5 . . ? H2S1 C2S1 H2S3 109.5 . . ? H2S2 C2S1 H2S3 109.5 . . ? N1G1 C1G1 N1G1 119.99(4) 11_466 . ? N1G1 C1G1 N1G1 120.00(4) 11_466 8_656 ? N1G1 C1G1 N1G1 119.99(5) . 8_656 ? C1G1 N1G1 H1G1 120.0 . . ? C1G1 N1G1 H1G2 120.0 . . ? H1G1 N1G1 H1G2 120.0 . . ? # Attachment 'G-2_SR154_uk.cif' data_psn _database_code_depnum_ccdc_archive 'CCDC 729711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H54 N6 Na O46 P Sn3 W9' _chemical_formula_weight 3035.3 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 17.5942(3) _cell_length_b 17.5942(3) _cell_length_c 17.5942(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5446.39(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3569 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 20.97 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 3.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5080 _exptl_absorpt_coefficient_mu 20.397 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.0530 _exptl_absorpt_correction_T_max 0.1899 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50041 _diffrn_reflns_av_R_equivalents 0.1174 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 26.44 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 3760 _reflns_number_gt 3236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0370P)^2^+67.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(16) _refine_ls_number_reflns 3760 _refine_ls_number_parameters 114 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.923 _refine_diff_density_min -1.117 _refine_diff_density_rms 0.273 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 W1 W 0.56846(4) 0.78279(4) 0.83650(4) 0.02554(16) Uani 1 1 d . . . W2 W 0.66191(4) 0.62328(4) 0.88445(4) 0.02478(16) Uani 1 1 d . . . W3 W 0.83576(4) 0.74384(4) 0.90069(4) 0.02776(17) Uani 1 1 d . . . P P 0.7307(2) 0.7307(2) 0.7307(2) 0.0173(13) Uani 1 3 d S . . Sn Sn 0.46891(6) 0.60029(6) 0.81299(6) 0.0259(3) Uani 1 1 d . . . C1 C 0.4470(10) 0.6112(10) 0.9306(9) 0.033(4) Uiso 1 1 d . . . H1A H 0.4874 0.5860 0.9594 0.049 Uiso 1 1 calc R . . H1B H 0.3981 0.5875 0.9427 0.049 Uiso 1 1 calc R . . H1C H 0.4453 0.6652 0.9443 0.049 Uiso 1 1 calc R . . C2 C 0.4664(11) 0.5548(10) 0.7044(10) 0.038(4) Uiso 1 1 d . . . H2A H 0.4135 0.5472 0.6887 0.056 Uiso 1 1 calc R . . H2B H 0.4931 0.5060 0.7041 0.056 Uiso 1 1 calc R . . H2C H 0.4914 0.5899 0.6690 0.056 Uiso 1 1 calc R . . O1T O 0.5027(6) 0.8349(6) 0.8874(6) 0.030(3) Uiso 1 1 d . . . O1A O 0.6544(6) 0.8442(6) 0.8637(6) 0.030(3) Uiso 1 1 d . . . O1SN O 0.3469(7) 0.6476(7) 0.7943(7) 0.038(3) Uiso 1 1 d . . . O1P O 0.6640(6) 0.7035(6) 0.7792(6) 0.024(2) Uiso 1 1 d . . . O1S O 0.5024(6) 0.7112(6) 0.7899(6) 0.030(3) Uiso 1 1 d . . . O2A O 0.7411(6) 0.5721(6) 0.8354(6) 0.027(2) Uiso 1 1 d . . . O2S O 0.5874(6) 0.5757(6) 0.8318(6) 0.028(2) Uiso 1 1 d . . . O2T O 0.6571(6) 0.5751(6) 0.9696(6) 0.031(3) Uiso 1 1 d . . . O2P O 0.7825(6) 0.7825(6) 0.7825(6) 0.028(4) Uiso 1 3 d S . . O3T O 0.8834(7) 0.7272(7) 0.9828(6) 0.033(3) Uiso 1 1 d . . . O3A O 0.7939(6) 0.8428(6) 0.9167(6) 0.026(2) Uiso 1 1 d . . . O12 O 0.5955(6) 0.7089(6) 0.9097(6) 0.026(2) Uiso 1 1 d . . . O23 O 0.7439(6) 0.6954(6) 0.9170(6) 0.026(2) Uiso 1 1 d . . . C1G C 0.5273(9) 0.9727(9) 1.0273(9) 0.025(6) Uiso 1 3 d S . . N1G N 0.4710(8) 0.9229(8) 1.0294(9) 0.038(4) Uiso 1 1 d . . . H1G1 H 0.4351 0.9272 1.0640 0.045 Uiso 1 1 calc R . . H1G2 H 0.4695 0.8854 0.9963 0.045 Uiso 1 1 calc R . . O1W O 0.4488(8) 0.7471(8) 0.6457(8) 0.055(4) Uiso 1 1 d . . . O2W O 0.2904(8) 0.6392(8) 0.6521(8) 0.054(4) Uiso 1 1 d . . . O3W O 0.3202(10) 0.8202(10) 0.6798(10) 0.083(9) Uiso 1 3 d S . . 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 W1 0.0268(4) 0.0257(3) 0.0241(3) -0.0006(3) 0.0023(3) 0.0016(3) W2 0.0253(3) 0.0260(3) 0.0230(3) 0.0020(3) 0.0004(3) 0.0004(3) W3 0.0287(3) 0.0291(4) 0.0254(3) -0.0012(3) -0.0048(3) -0.0016(3) P 0.0173(13) 0.0173(13) 0.0173(13) 0.0007(15) 0.0007(15) 0.0007(15) Sn 0.0263(6) 0.0262(6) 0.0252(6) -0.0017(5) 0.0011(5) -0.0003(5) _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 W1 O1T 1.727(11) . ? W1 O12 1.891(10) . ? W1 O1S 1.900(11) . ? W1 O2A 1.918(11) 9 ? W1 O1A 1.919(11) . ? W1 O1P 2.406(11) . ? W2 O2T 1.723(11) . ? W2 O2S 1.810(11) . ? W2 O2A 1.870(11) . ? W2 O12 1.957(11) . ? W2 O23 2.005(11) . ? W2 O1P 2.329(10) . ? W3 O3T 1.695(12) . ? W3 O23 1.850(11) . ? W3 O3A 1.912(11) . ? W3 O1A 1.925(11) 5 ? W3 O3A 1.959(11) 5 ? W3 O2P 2.380(11) . ? P O1P 1.528(11) 5 ? P O1P 1.528(11) . ? P O1P 1.528(11) 9 ? P O2P 1.58(2) . ? Sn C2 2.072(18) . ? Sn O1S 2.078(11) . ? Sn C1 2.114(16) . ? Sn O2S 2.154(11) . ? Sn O1SN 2.325(12) . ? Sn O2T 2.483(11) 10_646 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O1A W3 1.925(11) 9 ? O2A W1 1.918(11) 5 ? O2T Sn 2.483(11) 7_665 ? O2P W3 2.380(11) 5 ? O2P W3 2.380(11) 9 ? O3A W3 1.959(11) 9 ? C1G N1G 1.323(15) 6_467 ? C1G N1G 1.323(15) 12_675 ? C1G N1G 1.323(15) . ? N1G H1G1 0.8800 . ? N1G H1G2 0.8800 . ? 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 O1T W1 O12 100.4(5) . . ? O1T W1 O1S 99.6(5) . . ? O12 W1 O1S 89.5(5) . . ? O1T W1 O2A 102.7(5) . 9 ? O12 W1 O2A 156.9(5) . 9 ? O1S W1 O2A 87.9(5) . 9 ? O1T W1 O1A 95.7(5) . . ? O12 W1 O1A 91.1(5) . . ? O1S W1 O1A 164.3(5) . . ? O2A W1 O1A 85.4(5) 9 . ? O1T W1 O1P 173.5(5) . . ? O12 W1 O1P 73.2(4) . . ? O1S W1 O1P 82.1(4) . . ? O2A W1 O1P 83.7(4) 9 . ? O1A W1 O1P 83.1(4) . . ? O2T W2 O2S 100.5(5) . . ? O2T W2 O2A 101.6(5) . . ? O2S W2 O2A 94.7(5) . . ? O2T W2 O12 98.7(5) . . ? O2S W2 O12 92.3(5) . . ? O2A W2 O12 156.9(4) . . ? O2T W2 O23 95.6(5) . . ? O2S W2 O23 163.7(5) . . ? O2A W2 O23 84.3(4) . . ? O12 W2 O23 83.0(4) . . ? O2T W2 O1P 171.9(5) . . ? O2S W2 O1P 83.4(4) . . ? O2A W2 O1P 85.0(4) . . ? O12 W2 O1P 74.0(4) . . ? O23 W2 O1P 80.4(4) . . ? O3T W3 O23 102.7(5) . . ? O3T W3 O3A 102.9(5) . . ? O23 W3 O3A 93.5(5) . . ? O3T W3 O1A 99.9(5) . 5 ? O23 W3 O1A 85.8(5) . 5 ? O3A W3 O1A 156.8(5) . 5 ? O3T W3 O3A 99.3(5) . 5 ? O23 W3 O3A 157.3(5) . 5 ? O3A W3 O3A 87.0(6) . 5 ? O1A W3 O3A 85.0(5) 5 5 ? O3T W3 O2P 171.3(5) . . ? O23 W3 O2P 85.6(4) . . ? O3A W3 O2P 73.5(4) . . ? O1A W3 O2P 83.3(4) 5 . ? O3A W3 O2P 72.8(4) 5 . ? O1P P O1P 111.3(4) 5 . ? O1P P O1P 111.3(4) 5 9 ? O1P P O1P 111.3(4) . 9 ? O1P P O2P 107.6(5) 5 . ? O1P P O2P 107.6(5) . . ? O1P P O2P 107.6(5) 9 . ? C2 Sn O1S 100.8(6) . . ? C2 Sn C1 159.1(7) . . ? O1S Sn C1 99.1(6) . . ? C2 Sn O2S 94.9(6) . . ? O1S Sn O2S 86.8(4) . . ? C1 Sn O2S 92.5(6) . . ? C2 Sn O1SN 89.3(6) . . ? O1S Sn O1SN 84.1(4) . . ? C1 Sn O1SN 86.4(6) . . ? O2S Sn O1SN 170.6(4) . . ? C2 Sn O2T 80.3(6) . 10_646 ? O1S Sn O2T 178.0(4) . 10_646 ? C1 Sn O2T 79.6(5) . 10_646 ? O2S Sn O2T 94.8(4) . 10_646 ? O1SN Sn O2T 94.2(4) . 10_646 ? Sn C1 H1A 109.5 . . ? Sn C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sn C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sn C2 H2A 109.5 . . ? Sn C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sn C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? W1 O1A W3 150.6(6) . 9 ? P O1P W2 130.2(6) . . ? P O1P W1 126.1(6) . . ? W2 O1P W1 90.4(4) . . ? W1 O1S Sn 135.4(6) . . ? W2 O2A W1 153.0(6) . 5 ? W2 O2S Sn 133.4(6) . . ? W2 O2T Sn 161.5(6) . 7_665 ? P O2P W3 124.5(4) . 5 ? P O2P W3 124.5(4) . 9 ? W3 O2P W3 91.0(5) 5 9 ? P O2P W3 124.5(4) . . ? W3 O2P W3 91.0(5) 5 . ? W3 O2P W3 91.0(5) 9 . ? W3 O3A W3 122.7(6) . 9 ? W1 O12 W2 121.6(6) . . ? W3 O23 W2 151.1(6) . . ? N1G C1G N1G 119.89(16) 6_467 12_675 ? N1G C1G N1G 119.89(16) 6_467 . ? N1G C1G N1G 119.89(16) 12_675 . ? C1G N1G H1G1 120.0 . . ? C1G N1G H1G2 120.0 . . ? H1G1 N1G H1G2 120.0 . . ? # Attachment 'G-3_MS01_uk.cif' data_sisn _database_code_depnum_ccdc_archive 'CCDC 729712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H56 N6 Na2 O47 Si Sn3 W9' _chemical_formula_weight 3073.4 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 17.5199(4) _cell_length_b 17.5199(4) _cell_length_c 17.5199(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5377.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2348 _cell_measurement_theta_min 3.68 _cell_measurement_theta_max 22.96 _exptl_crystal_description tetrahedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 3.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5672 _exptl_absorpt_coefficient_mu 20.675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0135 _exptl_absorpt_correction_T_max 0.0997 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53126 _diffrn_reflns_av_R_equivalents 0.1406 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.61 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 4176 _reflns_number_gt 3342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0760P)^2^+22.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(2) _refine_ls_number_reflns 4176 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.794 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.326 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 W1 W 0.58987(5) 0.12966(5) 1.12819(5) 0.0399(2) Uani 1 1 d . . . W2 W 0.67919(5) 0.08765(5) 0.96927(5) 0.0415(2) Uani 1 1 d . . . W3 W 0.50436(5) 0.08388(5) 0.84882(5) 0.0422(2) Uani 1 1 d . . . Si Si 0.5192(3) -0.0192(3) 1.0192(3) 0.0341(18) Uani 1 3 d S . . Sn Sn 0.78520(8) 0.06395(8) 1.15501(8) 0.0422(3) Uani 1 1 d . . . C1 C 0.8064(13) 0.1806(13) 1.1433(13) 0.051(5) Uiso 1 1 d . . . H1A H 0.7698 0.2094 1.1743 0.076 Uiso 1 1 calc R . . H1B H 0.8010 0.1952 1.0896 0.076 Uiso 1 1 calc R . . H1C H 0.8584 0.1919 1.1605 0.076 Uiso 1 1 calc R . . C2 C 0.7879(13) -0.0506(13) 1.1984(13) 0.052(5) Uiso 1 1 d . . . H2A H 0.7712 -0.0860 1.1585 0.078 Uiso 1 1 calc R . . H2B H 0.7537 -0.0546 1.2425 0.078 Uiso 1 1 calc R . . H2C H 0.8401 -0.0633 1.2141 0.078 Uiso 1 1 calc R . . O1A O 0.5092(7) 0.0799(7) 1.1788(7) 0.036(3) Uiso 1 1 d . . . O1S O 0.6661(8) 0.0808(8) 1.1773(8) 0.043(3) Uiso 1 1 d . . . O1T O 0.5909(9) 0.2164(9) 1.1768(9) 0.051(4) Uiso 1 1 d . . . O1SW O 0.9082(10) 0.0478(10) 1.1081(10) 0.064(4) Uiso 1 1 d . . . O1SI O 0.5894(7) 0.0342(7) 1.0484(7) 0.036(3) Uiso 1 1 d . . . O2T O 0.7470(8) 0.1372(8) 0.9168(8) 0.046(3) Uiso 1 1 d . . . O2S O 0.7520(8) 0.0384(8) 1.0418(8) 0.044(3) Uiso 1 1 d . . . O2SI O 0.4652(8) 0.0348(8) 0.9652(8) 0.040(5) Uiso 1 3 d S . . O3T O 0.5230(9) 0.1321(9) 0.7648(8) 0.049(3) Uiso 1 1 d . . . O3B O 0.4042(8) 0.0430(8) 0.8302(8) 0.045(3) Uiso 1 1 d . . . O3A O 0.5564(8) -0.0064(8) 0.8351(8) 0.043(3) Uiso 1 1 d . . . O12 O 0.6578(9) 0.1611(9) 1.0466(9) 0.050(3) Uiso 1 1 d . . . O23 O 0.5966(8) 0.1130(8) 0.9096(8) 0.045(3) Uiso 1 1 d . . . C1G C 0.2758(11) -0.2242(11) 0.7242(11) 0.039(7) Uiso 1 3 d S . . N1G N 0.2797(11) -0.1725(11) 0.7798(11) 0.054(5) Uiso 1 1 d . . . H1G1 H 0.2455 -0.1358 0.7825 0.065 Uiso 1 1 calc R . . H1G2 H 0.3165 -0.1751 0.8140 0.065 Uiso 1 1 calc R . . O1W O 0.9577(13) -0.0968(13) 1.1028(13) 0.089(6) Uiso 1 1 d . . . O2W O 0.8046(14) -0.1072(14) 1.0058(15) 0.099(7) Uiso 1 1 d . . . O3W O 0.323(2) 0.008(2) 0.691(2) 0.163(13) Uiso 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 W1 0.0432(4) 0.0365(4) 0.0399(4) -0.0020(3) 0.0014(4) -0.0025(3) W2 0.0415(4) 0.0438(4) 0.0391(4) 0.0007(3) 0.0019(3) -0.0054(4) W3 0.0433(4) 0.0445(4) 0.0388(4) 0.0052(4) -0.0011(3) 0.0014(4) Si 0.0341(18) 0.0341(18) 0.0341(18) 0.000(2) 0.000(2) 0.000(2) Sn 0.0438(7) 0.0445(7) 0.0384(7) 0.0030(6) -0.0017(6) -0.0023(6) _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 W1 O1T 1.742(16) . ? W1 O1S 1.805(13) . ? W1 O1A 1.883(13) . ? W1 O12 1.940(16) . ? W1 O3A 2.024(14) 12_565 ? W1 O1SI 2.180(12) . ? W2 O2T 1.734(15) . ? W2 O23 1.840(15) . ? W2 O1A 1.902(13) 6_456 ? W2 O12 1.906(15) . ? W2 O2S 1.996(14) . ? W2 O1SI 2.296(13) . ? W3 O3T 1.728(15) . ? W3 O3A 1.842(14) . ? W3 O3B 1.923(14) . ? W3 O3B 1.974(14) 12_565 ? W3 O23 2.001(14) . ? W3 O2SI 2.317(13) . ? Si O1SI 1.628(13) 6_456 ? Si O1SI 1.628(13) . ? Si O1SI 1.628(13) 12_565 ? Si O2SI 1.64(2) . ? Sn C1 2.09(2) . ? Sn O2S 2.115(14) . ? Sn O1S 2.143(13) . ? Sn C2 2.15(2) . ? Sn O1SW 2.324(18) . ? Sn O1T 2.396(15) 8_746 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O1A W2 1.902(13) 12_565 ? O1T Sn 2.396(15) 11_567 ? O2SI W3 2.317(13) 6_456 ? O2SI W3 2.317(13) 12_565 ? O3B W3 1.974(14) 6_456 ? O3A W1 2.024(14) 6_456 ? C1G N1G 1.332(19) 8_645 ? C1G N1G 1.332(19) 11_556 ? C1G N1G 1.332(19) . ? N1G H1G1 0.8800 . ? N1G H1G2 0.8800 . ? 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 O1T W1 O1S 100.0(7) . . ? O1T W1 O1A 100.5(6) . . ? O1S W1 O1A 96.4(6) . . ? O1T W1 O12 96.1(7) . . ? O1S W1 O12 91.8(6) . . ? O1A W1 O12 159.9(6) . . ? O1T W1 O3A 92.6(7) . 12_565 ? O1S W1 O3A 167.2(6) . 12_565 ? O1A W1 O3A 83.8(5) . 12_565 ? O12 W1 O3A 84.2(6) . 12_565 ? O1T W1 O1SI 169.3(6) . . ? O1S W1 O1SI 86.8(5) . . ? O1A W1 O1SI 86.8(5) . . ? O12 W1 O1SI 75.4(6) . . ? O3A W1 O1SI 80.4(5) 12_565 . ? O2T W2 O23 96.7(6) . . ? O2T W2 O1A 102.0(6) . 6_456 ? O23 W2 O1A 87.4(6) . 6_456 ? O2T W2 O12 100.0(7) . . ? O23 W2 O12 94.9(6) . . ? O1A W2 O12 157.4(6) 6_456 . ? O2T W2 O2S 96.7(6) . . ? O23 W2 O2S 165.6(6) . . ? O1A W2 O2S 84.6(6) 6_456 . ? O12 W2 O2S 88.0(6) . . ? O2T W2 O1SI 173.2(6) . . ? O23 W2 O1SI 84.4(5) . . ? O1A W2 O1SI 84.7(5) 6_456 . ? O12 W2 O1SI 73.2(6) . . ? O2S W2 O1SI 82.9(5) . . ? O3T W3 O3A 102.5(7) . . ? O3T W3 O3B 102.1(6) . . ? O3A W3 O3B 96.3(6) . . ? O3T W3 O3B 97.2(6) . 12_565 ? O3A W3 O3B 158.0(6) . 12_565 ? O3B W3 O3B 89.1(8) . 12_565 ? O3T W3 O23 100.2(7) . . ? O3A W3 O23 83.6(6) . . ? O3B W3 O23 157.2(6) . . ? O3B W3 O23 83.3(6) 12_565 . ? O3T W3 O2SI 170.7(7) . . ? O3A W3 O2SI 86.7(6) . . ? O3B W3 O2SI 75.0(5) . . ? O3B W3 O2SI 74.1(5) 12_565 . ? O23 W3 O2SI 82.3(5) . . ? O1SI Si O1SI 112.2(5) 6_456 . ? O1SI Si O1SI 112.2(5) 6_456 12_565 ? O1SI Si O1SI 112.2(5) . 12_565 ? O1SI Si O2SI 106.6(5) 6_456 . ? O1SI Si O2SI 106.6(5) . . ? O1SI Si O2SI 106.6(5) 12_565 . ? C1 Sn O2S 99.4(7) . . ? C1 Sn O1S 93.2(7) . . ? O2S Sn O1S 86.1(5) . . ? C1 Sn C2 161.1(9) . . ? O2S Sn C2 98.1(8) . . ? O1S Sn C2 94.9(7) . . ? C1 Sn O1SW 85.4(8) . . ? O2S Sn O1SW 84.1(6) . . ? O1S Sn O1SW 169.8(6) . . ? C2 Sn O1SW 89.5(8) . . ? C1 Sn O1T 81.4(7) . 8_746 ? O2S Sn O1T 179.2(5) . 8_746 ? O1S Sn O1T 94.1(5) . 8_746 ? C2 Sn O1T 81.1(7) . 8_746 ? O1SW Sn O1T 95.7(6) . 8_746 ? Sn C1 H1A 109.5 . . ? Sn C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sn C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sn C2 H2A 109.5 . . ? Sn C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sn C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? W1 O1A W2 151.7(7) . 12_565 ? W1 O1S Sn 134.3(7) . . ? W1 O1T Sn 162.6(9) . 11_567 ? Si O1SI W1 130.2(7) . . ? Si O1SI W2 124.2(7) . . ? W1 O1SI W2 94.1(5) . . ? W2 O2S Sn 133.0(7) . . ? Si O2SI W3 123.5(5) . 6_456 ? Si O2SI W3 123.5(5) . . ? W3 O2SI W3 92.5(7) 6_456 . ? Si O2SI W3 123.5(5) . 12_565 ? W3 O2SI W3 92.5(7) 6_456 12_565 ? W3 O2SI W3 92.5(7) . 12_565 ? W3 O3B W3 118.4(7) . 6_456 ? W3 O3A W1 152.6(8) . 6_456 ? W2 O12 W1 116.9(8) . . ? W2 O23 W3 151.1(8) . . ? N1G C1G N1G 120.003(9) 8_645 11_556 ? N1G C1G N1G 119.997(9) 8_645 . ? N1G C1G N1G 120.000(9) 11_556 . ? C1G N1G H1G1 120.0 . . ? C1G N1G H1G2 120.0 . . ? H1G1 N1G H1G2 120.0 . . ?