# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_coden_Cambridge 440 _publ_contact_author_name 'Prof Michael Veith' _publ_contact_author_address ; Inorganic Chemistry Saarland University P.O. 15 11 50 Saarbrucken 66041 GERMANY ; _publ_contact_author_phone '0681 302 2265' _publ_contact_author_fax '0681 302 3995' _publ_contact_author_email veith@mx.uni-saarland.de _publ_requested_journal 'New J. Chem.' # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, Solid-State Molecular Structure and Solution Dynamics of new Alkoxy Stannylene-Transition Metal Complexes ; loop_ _publ_author_name _publ_author_address 'Veith, Michael' ; Institut fur Anorganische Chemie Universitat des Saarlandes Postfach 151150 66041 Saarbrucken Deutschland ; 'Ehses, Markus' ; Institut fur Anorganische Chemie Universitat des Saarlandes Postfach 151150 66041 Saarbrucken Deutschland ; 'Huch, Volker' ; Institut fur Anorganische Chemie Universitat des Saarlandes Postfach 151150 66041 Saarbrucken Deutschland ; #================================================================= data_comp_2b _database_code_depnum_ccdc_archive 'CCDC 256747' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H36 O9 Sn1 W' _chemical_formula_weight 853.73 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' 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 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 10.212(2) _cell_length_b 16.968(3) _cell_length_c 17.657(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.45(3) _cell_angle_gamma 90.00 _cell_volume 3058.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 5.411 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'Image Plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17039 _diffrn_reflns_av_R_equivalents 0.3516 _diffrn_reflns_av_sigmaI/netI 0.1985 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 24.20 _reflns_number_total 4610 _reflns_number_gt 3842 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4610 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.2410 _refine_ls_wR_factor_gt 0.2340 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.093 _refine_ls_shift/su_mean 0.004 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 0.51733(6) 0.20661(4) 0.21816(3) 0.0284(3) Uani 1 1 d . . . Sn1 Sn 0.48542(9) 0.30596(5) 0.33727(5) 0.0208(3) Uani 1 1 d . . . Sn2 Sn 0.30790(10) 0.25643(6) 0.48745(5) 0.0309(3) Uani 1 1 d . . . O1 O 0.2970(10) 0.3149(6) 0.3797(6) 0.030(2) Uani 1 1 d . . . O2 O 0.5029(10) 0.2696(6) 0.4495(6) 0.029(2) Uani 1 1 d . . . O3 O 0.3057(15) 0.1562(8) 0.4298(8) 0.060(4) Uani 1 1 d . . . O4 O 0.5351(12) 0.4157(6) 0.3587(7) 0.042(3) Uani 1 1 d . . . O5 O 0.4429(18) 0.3467(9) 0.1046(9) 0.074(5) Uani 1 1 d . . . O6 O 0.2177(14) 0.1613(10) 0.2340(8) 0.068(4) Uani 1 1 d . . . O7 O 0.8206(15) 0.2482(12) 0.2116(12) 0.084(6) Uani 1 1 d . . . O8 O 0.589(3) 0.0636(10) 0.3281(11) 0.113(8) Uani 1 1 d . . . O9 O 0.5368(16) 0.0973(10) 0.0737(7) 0.070(4) Uani 1 1 d . . . C1 C 0.1930(15) 0.3687(12) 0.3559(12) 0.050(5) Uani 1 1 d . . . C2 C 0.2074(19) 0.3838(18) 0.2707(11) 0.077(8) Uani 1 1 d . . . H2A H 0.2002 0.3348 0.2437 0.115 Uiso 1 1 calc R . . H2B H 0.2914 0.4070 0.2620 0.115 Uiso 1 1 calc R . . H2C H 0.1396 0.4190 0.2531 0.115 Uiso 1 1 calc R . . C3 C 0.0636(18) 0.3255(18) 0.3720(16) 0.082(8) Uani 1 1 d . . . H3A H 0.0595 0.2774 0.3434 0.123 Uiso 1 1 calc R . . H3B H -0.0091 0.3586 0.3576 0.123 Uiso 1 1 calc R . . H3C H 0.0600 0.3136 0.4251 0.123 Uiso 1 1 calc R . . C4 C 0.201(2) 0.4438(13) 0.3989(14) 0.070(6) Uani 1 1 d . . . H4A H 0.1925 0.4333 0.4519 0.105 Uiso 1 1 calc R . . H4B H 0.1326 0.4785 0.3818 0.105 Uiso 1 1 calc R . . H4C H 0.2847 0.4682 0.3907 0.105 Uiso 1 1 calc R . . C5 C 0.6263(17) 0.2545(11) 0.4941(10) 0.045(5) Uani 1 1 d . . . C6 C 0.738(3) 0.235(2) 0.4414(17) 0.110(12) Uani 1 1 d . . . H6A H 0.7473 0.2767 0.4051 0.165 Uiso 1 1 calc R . . H6B H 0.7197 0.1865 0.4155 0.165 Uiso 1 1 calc R . . H6C H 0.8184 0.2299 0.4707 0.165 Uiso 1 1 calc R . . C7 C 0.676(5) 0.331(2) 0.528(3) 0.20(3) Uani 1 1 d . . . H7A H 0.6930 0.3676 0.4887 0.307 Uiso 1 1 calc R . . H7B H 0.7547 0.3208 0.5573 0.307 Uiso 1 1 calc R . . H7C H 0.6105 0.3520 0.5608 0.307 Uiso 1 1 calc R . . C8 C 0.599(2) 0.197(2) 0.5521(17) 0.122(16) Uani 1 1 d . . . H8A H 0.5774 0.1478 0.5290 0.183 Uiso 1 1 calc R . . H8B H 0.5269 0.2154 0.5813 0.183 Uiso 1 1 calc R . . H8C H 0.6751 0.1913 0.5847 0.183 Uiso 1 1 calc R . . C9 C 0.231(2) 0.0840(11) 0.4523(12) 0.057(5) Uani 1 1 d . . . C10 C 0.088(2) 0.1006(15) 0.4324(13) 0.071(6) Uani 1 1 d . . . H10A H 0.0781 0.1107 0.3790 0.107 Uiso 1 1 calc R . . H10B H 0.0590 0.1458 0.4601 0.107 Uiso 1 1 calc R . . H10C H 0.0355 0.0558 0.4454 0.107 Uiso 1 1 calc R . . C11 C 0.247(3) 0.0643(15) 0.5335(15) 0.092(10) Uani 1 1 d . . . H11A H 0.3376 0.0538 0.5453 0.139 Uiso 1 1 calc R . . H11B H 0.1958 0.0185 0.5446 0.139 Uiso 1 1 calc R . . H11C H 0.2179 0.1079 0.5635 0.139 Uiso 1 1 calc R . . C12 C 0.279(4) 0.0215(11) 0.3961(19) 0.107(11) Uani 1 1 d . . . H12A H 0.3687 0.0090 0.4074 0.160 Uiso 1 1 calc R . . H12B H 0.2704 0.0417 0.3455 0.160 Uiso 1 1 calc R . . H12C H 0.2264 -0.0253 0.4005 0.160 Uiso 1 1 calc R . . C13 C 0.6141(18) 0.4702(10) 0.3242(13) 0.053(5) Uani 1 1 d . . . C14 C 0.748(2) 0.4393(18) 0.321(3) 0.134(17) Uani 1 1 d . . . H14A H 0.7488 0.3938 0.2891 0.201 Uiso 1 1 calc R . . H14B H 0.7774 0.4248 0.3715 0.201 Uiso 1 1 calc R . . H14C H 0.8045 0.4790 0.3017 0.201 Uiso 1 1 calc R . . C15 C 0.543(3) 0.501(3) 0.2437(17) 0.17(2) Uani 1 1 d . . . H15A H 0.5305 0.4565 0.2102 0.256 Uiso 1 1 calc R . . H15B H 0.5978 0.5391 0.2202 0.256 Uiso 1 1 calc R . . H15C H 0.4596 0.5238 0.2541 0.256 Uiso 1 1 calc R . . C16 C 0.637(6) 0.536(2) 0.375(3) 0.21(3) Uani 1 1 d . . . H16A H 0.5562 0.5628 0.3836 0.317 Uiso 1 1 calc R . . H16B H 0.6986 0.5716 0.3534 0.317 Uiso 1 1 calc R . . H16C H 0.6724 0.5166 0.4227 0.317 Uiso 1 1 calc R . . C17 C 0.469(2) 0.2933(12) 0.1450(11) 0.059(7) Uani 1 1 d . . . C18 C 0.3286(18) 0.1775(11) 0.2286(9) 0.044(4) Uani 1 1 d . . . C19 C 0.705(2) 0.2319(11) 0.2144(10) 0.047(5) Uani 1 1 d . . . C20 C 0.564(2) 0.1182(14) 0.2903(10) 0.058(5) Uani 1 1 d . . . C21 C 0.5201(16) 0.1379(10) 0.1331(9) 0.039(4) 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 W1 0.0361(4) 0.0415(4) 0.0082(4) -0.0028(2) 0.0117(3) 0.0016(3) Sn1 0.0225(5) 0.0306(5) 0.0094(5) 0.0001(3) 0.0043(4) 0.0032(4) Sn2 0.0390(6) 0.0451(6) 0.0092(5) -0.0011(4) 0.0126(5) 0.0025(5) O1 0.025(5) 0.032(5) 0.031(6) 0.003(5) -0.009(5) 0.009(5) O2 0.027(5) 0.043(5) 0.016(5) 0.006(5) -0.012(4) 0.006(5) O3 0.084(9) 0.058(7) 0.039(7) -0.017(7) 0.018(7) -0.028(8) O4 0.057(7) 0.033(5) 0.038(7) 0.000(5) 0.022(6) -0.002(6) O5 0.097(12) 0.082(9) 0.041(8) 0.028(8) -0.013(8) 0.002(10) O6 0.058(8) 0.104(12) 0.041(8) -0.001(8) 0.014(7) -0.037(9) O7 0.045(9) 0.106(13) 0.101(15) -0.028(12) 0.015(8) -0.007(9) O8 0.21(2) 0.068(9) 0.067(11) 0.034(9) 0.030(13) 0.073(13) O9 0.102(11) 0.090(10) 0.021(6) -0.028(7) 0.034(7) -0.015(10) C1 0.016(7) 0.068(11) 0.065(13) 0.023(10) -0.004(8) 0.019(9) C2 0.039(9) 0.15(2) 0.041(11) 0.037(14) -0.012(9) 0.022(14) C3 0.025(9) 0.13(2) 0.091(19) 0.035(18) -0.010(11) 0.007(14) C4 0.076(14) 0.067(13) 0.070(15) 0.007(12) 0.040(12) 0.021(12) C5 0.034(9) 0.069(11) 0.030(9) 0.009(9) -0.027(8) 0.004(9) C6 0.076(17) 0.17(3) 0.08(2) -0.01(2) -0.019(16) 0.08(2) C7 0.30(6) 0.12(2) 0.19(5) -0.03(3) -0.20(5) -0.01(3) C8 0.050(12) 0.23(4) 0.09(2) 0.13(3) 0.013(14) 0.017(19) C9 0.074(13) 0.052(10) 0.045(11) 0.006(9) 0.012(10) -0.034(11) C10 0.067(13) 0.087(15) 0.060(14) 0.000(13) 0.008(12) -0.032(14) C11 0.11(2) 0.072(14) 0.09(2) 0.044(15) -0.007(17) -0.041(16) C12 0.17(3) 0.027(9) 0.13(3) -0.023(13) 0.03(2) -0.018(15) C13 0.044(10) 0.039(8) 0.075(14) 0.015(10) -0.012(10) -0.013(9) C14 0.051(14) 0.090(18) 0.26(5) 0.06(3) 0.049(19) -0.001(15) C15 0.12(2) 0.33(7) 0.062(19) 0.09(3) 0.034(19) 0.01(4) C16 0.34(7) 0.12(3) 0.17(4) -0.08(3) 0.14(4) -0.17(4) C17 0.054(12) 0.083(14) 0.037(11) -0.019(10) -0.044(10) -0.011(10) C18 0.046(10) 0.066(10) 0.018(8) 0.009(8) -0.009(8) -0.019(10) C19 0.069(13) 0.050(9) 0.023(9) -0.002(8) 0.025(9) 0.027(10) C20 0.071(13) 0.087(14) 0.016(8) -0.008(10) 0.010(9) -0.012(12) C21 0.042(8) 0.050(9) 0.026(8) -0.008(7) 0.023(7) -0.013(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 C21 1.902(16) . ? W1 C19 1.97(2) . ? W1 C18 2.002(19) . ? W1 C17 2.01(2) . ? W1 C20 2.02(2) . ? W1 Sn1 2.7213(11) . ? Sn1 O4 1.964(11) . ? Sn1 O2 2.079(10) . ? Sn1 O1 2.088(11) . ? Sn2 O3 1.982(12) . ? Sn2 O2 2.129(11) . ? Sn2 O1 2.147(10) . ? O1 C1 1.454(18) . ? O2 C5 1.491(16) . ? O3 C9 1.50(2) . ? O4 C13 1.38(2) . ? O5 C17 1.18(2) . ? O6 C18 1.17(2) . ? O7 C19 1.21(3) . ? O8 C20 1.17(3) . ? O9 C21 1.27(2) . ? C1 C4 1.48(3) . ? C1 C2 1.54(3) . ? C1 C3 1.54(3) . ? C5 C8 1.44(3) . ? C5 C7 1.51(3) . ? C5 C6 1.53(4) . ? C9 C11 1.48(3) . ? C9 C10 1.52(3) . ? C9 C12 1.54(3) . ? C13 C16 1.45(4) . ? C13 C14 1.46(3) . ? C13 C15 1.66(3) . ? 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 C21 W1 C19 94.2(7) . . ? C21 W1 C18 87.4(7) . . ? C19 W1 C18 176.2(6) . . ? C21 W1 C17 87.1(8) . . ? C19 W1 C17 92.4(8) . . ? C18 W1 C17 91.1(8) . . ? C21 W1 C20 92.0(8) . . ? C19 W1 C20 88.2(8) . . ? C18 W1 C20 88.4(8) . . ? C17 W1 C20 179.0(7) . . ? C21 W1 Sn1 173.9(5) . . ? C19 W1 Sn1 91.5(5) . . ? C18 W1 Sn1 87.0(5) . . ? C17 W1 Sn1 90.6(6) . . ? C20 W1 Sn1 90.2(6) . . ? O4 Sn1 O2 94.7(4) . . ? O4 Sn1 O1 95.6(5) . . ? O2 Sn1 O1 74.8(4) . . ? O4 Sn1 W1 134.5(4) . . ? O2 Sn1 W1 122.9(3) . . ? O1 Sn1 W1 116.9(3) . . ? O3 Sn2 O2 85.8(5) . . ? O3 Sn2 O1 86.6(5) . . ? O2 Sn2 O1 72.6(4) . . ? C1 O1 Sn1 128.0(10) . . ? C1 O1 Sn2 124.5(11) . . ? Sn1 O1 Sn2 104.9(4) . . ? C5 O2 Sn1 127.2(11) . . ? C5 O2 Sn2 126.9(10) . . ? Sn1 O2 Sn2 105.8(3) . . ? C9 O3 Sn2 124.2(13) . . ? C13 O4 Sn1 134.5(12) . . ? O1 C1 C4 111.0(15) . . ? O1 C1 C2 107.4(16) . . ? C4 C1 C2 110.6(19) . . ? O1 C1 C3 105.8(15) . . ? C4 C1 C3 111(2) . . ? C2 C1 C3 111.3(17) . . ? C8 C5 O2 108.4(15) . . ? C8 C5 C7 111(3) . . ? O2 C5 C7 109.5(18) . . ? C8 C5 C6 117(2) . . ? O2 C5 C6 110.6(15) . . ? C7 C5 C6 100(3) . . ? C11 C9 O3 113.4(16) . . ? C11 C9 C10 110(2) . . ? O3 C9 C10 106.2(17) . . ? C11 C9 C12 116(2) . . ? O3 C9 C12 102.7(17) . . ? C10 C9 C12 107(2) . . ? O4 C13 C16 109(2) . . ? O4 C13 C14 109.3(17) . . ? C16 C13 C14 99(3) . . ? O4 C13 C15 109.8(19) . . ? C16 C13 C15 111(3) . . ? C14 C13 C15 118(3) . . ? O5 C17 W1 176.9(13) . . ? O6 C18 W1 179.1(17) . . ? O7 C19 W1 179.3(19) . . ? O8 C20 W1 175.5(17) . . ? O9 C21 W1 171.8(14) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 24.20 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 4.395 _refine_diff_density_min -4.938 _refine_diff_density_rms 0.501 #===END data_comp_2a _database_code_depnum_ccdc_archive 'CCDC 256748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H36 Cr O9 Sn2' _chemical_formula_weight 721.88 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 10.238(2) _cell_length_b 17.010(3) _cell_length_c 17.600(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.03(3) _cell_angle_gamma 90.00 _cell_volume 3064.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 2.004 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2456 _exptl_absorpt_correction_T_max 0.9967 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe AED2' _diffrn_measurement_method ; Scan width (omega) = 1.00 - 1.15, scan ratio 2theta:omega = 1.00 I(Net) and sigma(I) calculated according to Blessing (1987) ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 7.2 _diffrn_reflns_number 4903 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 24.19 _reflns_number_total 4903 _reflns_number_gt 3611 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0969P)^2^+6.8551P] 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 4903 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 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 Sn1 Sn 0.01592(6) 0.80325(4) 0.66479(3) 0.0502(2) Uani 1 1 d . . . Sn2 Sn 0.19144(8) 0.75491(4) 0.51222(4) 0.0662(3) Uani 1 1 d . . . Cr1 Cr -0.01117(17) 0.70789(10) 0.77708(9) 0.0614(4) Uani 1 1 d . . . O1 O 0.2014(6) 0.8155(4) 0.6201(4) 0.0576(16) Uani 1 1 d . . . O2 O -0.0058(6) 0.7665(4) 0.5531(4) 0.0590(16) Uani 1 1 d . . . O3 O 0.1977(8) 0.6538(4) 0.5659(4) 0.078(2) Uani 1 1 d . . . O4 O -0.0355(8) 0.9116(4) 0.6428(5) 0.082(2) Uani 1 1 d . . . C1 C 0.3046(11) 0.8686(7) 0.6430(8) 0.087(4) Uani 1 1 d . . . C2 C 0.2939(15) 0.8869(10) 0.7263(8) 0.120(6) Uani 1 1 d . . . H2A H 0.2117 0.9120 0.7354 0.180 Uiso 1 1 calc R . . H2B H 0.3638 0.9213 0.7417 0.180 Uiso 1 1 calc R . . H2C H 0.2994 0.8390 0.7550 0.180 Uiso 1 1 calc R . . C3 C 0.4318(12) 0.8258(12) 0.6279(11) 0.141(7) Uani 1 1 d . . . H3A H 0.4396 0.8170 0.5743 0.211 Uiso 1 1 calc R . . H3B H 0.4322 0.7762 0.6539 0.211 Uiso 1 1 calc R . . H3C H 0.5040 0.8571 0.6459 0.211 Uiso 1 1 calc R . . C4 C 0.2888(17) 0.9422(9) 0.5960(10) 0.134(6) Uani 1 1 d . . . H4A H 0.2090 0.9681 0.6091 0.201 Uiso 1 1 calc R . . H4B H 0.2862 0.9286 0.5431 0.201 Uiso 1 1 calc R . . H4C H 0.3613 0.9768 0.6060 0.201 Uiso 1 1 calc R . . C5 C -0.1231(12) 0.7542(7) 0.5080(7) 0.075(3) Uani 1 1 d . . . C6 C -0.2350(15) 0.7373(13) 0.5615(10) 0.157(9) Uani 1 1 d . . . H6A H -0.2445 0.7804 0.5961 0.235 Uiso 1 1 calc R . . H6B H -0.2165 0.6901 0.5897 0.235 Uiso 1 1 calc R . . H6C H -0.3146 0.7306 0.5325 0.235 Uiso 1 1 calc R . . C7 C -0.0960(17) 0.6880(13) 0.4548(12) 0.171(10) Uani 1 1 d . . . H7A H -0.0771 0.6412 0.4835 0.256 Uiso 1 1 calc R . . H7B H -0.0223 0.7010 0.4243 0.256 Uiso 1 1 calc R . . H7C H -0.1710 0.6791 0.4225 0.256 Uiso 1 1 calc R . . C8 C -0.149(2) 0.8290(11) 0.4671(12) 0.173(10) Uani 1 1 d . . . H8A H -0.1654 0.8700 0.5032 0.260 Uiso 1 1 calc R . . H8B H -0.2245 0.8228 0.4343 0.260 Uiso 1 1 calc R . . H8C H -0.0749 0.8426 0.4374 0.260 Uiso 1 1 calc R . . C9 C 0.2732(14) 0.5869(8) 0.5486(8) 0.088(4) Uani 1 1 d . . . C10 C 0.2498(18) 0.5653(11) 0.4670(9) 0.134(7) Uani 1 1 d . . . H10A H 0.1588 0.5540 0.4587 0.200 Uiso 1 1 calc R . . H10B H 0.3008 0.5198 0.4549 0.200 Uiso 1 1 calc R . . H10C H 0.2748 0.6084 0.4352 0.200 Uiso 1 1 calc R . . C11 C 0.228(2) 0.5227(9) 0.6014(11) 0.149(7) Uani 1 1 d . . . H11A H 0.1379 0.5111 0.5908 0.224 Uiso 1 1 calc R . . H11B H 0.2383 0.5399 0.6531 0.224 Uiso 1 1 calc R . . H11C H 0.2796 0.4763 0.5937 0.224 Uiso 1 1 calc R . . C12 C 0.4120(17) 0.6040(12) 0.5649(11) 0.145(7) Uani 1 1 d . . . H12A H 0.4412 0.6448 0.5315 0.218 Uiso 1 1 calc R . . H12B H 0.4629 0.5574 0.5572 0.218 Uiso 1 1 calc R . . H12C H 0.4222 0.6211 0.6167 0.218 Uiso 1 1 calc R . . C13 C -0.1156(15) 0.9674(7) 0.6813(9) 0.094(4) Uani 1 1 d . . . C14 C -0.242(2) 0.9357(14) 0.696(2) 0.29(2) Uani 1 1 d . . . H14A H -0.2325 0.8870 0.7227 0.435 Uiso 1 1 calc R . . H14B H -0.2872 0.9267 0.6483 0.435 Uiso 1 1 calc R . . H14C H -0.2903 0.9722 0.7257 0.435 Uiso 1 1 calc R . . C15 C -0.129(3) 1.0307(14) 0.6321(17) 0.29(2) Uani 1 1 d . . . H15A H -0.0447 1.0529 0.6228 0.435 Uiso 1 1 calc R . . H15B H -0.1840 1.0697 0.6546 0.435 Uiso 1 1 calc R . . H15C H -0.1678 1.0132 0.5850 0.435 Uiso 1 1 calc R . . C16 C -0.055(3) 0.9934(18) 0.7513(16) 0.30(2) Uani 1 1 d . . . H16A H 0.0324 1.0113 0.7415 0.444 Uiso 1 1 calc R . . H16B H -0.0510 0.9505 0.7867 0.444 Uiso 1 1 calc R . . H16C H -0.1045 1.0357 0.7723 0.444 Uiso 1 1 calc R . . C17 C 0.1665(13) 0.6810(8) 0.7676(6) 0.079(3) Uani 1 1 d . . . C18 C -0.1898(13) 0.7331(8) 0.7825(7) 0.083(3) Uani 1 1 d . . . C19 C -0.0195(13) 0.6433(8) 0.8598(7) 0.086(4) Uani 1 1 d . . . C20 C 0.0354(12) 0.7895(8) 0.8430(7) 0.078(3) Uani 1 1 d . . . C21 C -0.0538(12) 0.6250(8) 0.7097(7) 0.079(3) Uani 1 1 d . . . O5 O 0.2729(11) 0.6640(7) 0.7638(5) 0.117(4) Uani 1 1 d . . . O6 O -0.2965(11) 0.7454(7) 0.7873(7) 0.127(4) Uani 1 1 d . . . O7 O -0.0273(12) 0.6033(7) 0.9121(6) 0.130(4) Uani 1 1 d . . . O8 O 0.0611(11) 0.8376(6) 0.8865(6) 0.117(4) Uani 1 1 d . . . O9 O -0.0831(12) 0.5739(6) 0.6737(7) 0.132(4) 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 Sn1 0.0439(4) 0.0625(4) 0.0441(4) -0.0011(3) 0.0002(3) -0.0026(3) Sn2 0.0697(5) 0.0854(5) 0.0438(4) 0.0011(3) 0.0132(3) -0.0046(4) Cr1 0.0617(10) 0.0815(11) 0.0411(9) 0.0048(7) 0.0083(7) -0.0004(8) O1 0.040(4) 0.079(4) 0.054(4) -0.005(3) 0.002(3) -0.012(3) O2 0.048(4) 0.077(4) 0.051(4) -0.010(3) -0.007(3) -0.002(3) O3 0.091(6) 0.079(5) 0.064(5) 0.000(4) 0.028(4) 0.016(4) O4 0.089(6) 0.066(4) 0.089(6) 0.003(4) -0.007(4) 0.011(4) C1 0.056(7) 0.089(8) 0.116(11) -0.020(7) -0.004(7) -0.020(6) C2 0.107(12) 0.165(14) 0.088(11) -0.062(10) -0.014(8) -0.027(10) C3 0.044(8) 0.221(19) 0.157(16) -0.056(14) -0.010(9) -0.035(10) C4 0.145(16) 0.112(12) 0.145(16) -0.009(11) 0.031(12) -0.061(11) C5 0.070(8) 0.092(8) 0.064(7) -0.013(6) -0.031(6) 0.007(6) C6 0.068(10) 0.30(3) 0.101(13) -0.005(15) -0.014(9) -0.058(13) C7 0.099(13) 0.23(2) 0.178(19) -0.135(17) -0.048(12) 0.015(13) C8 0.20(2) 0.151(16) 0.161(19) 0.018(14) -0.095(17) 0.024(15) C9 0.085(10) 0.092(9) 0.087(9) -0.015(7) 0.013(7) 0.019(7) C10 0.163(17) 0.144(14) 0.093(12) -0.045(10) -0.003(11) 0.042(12) C11 0.20(2) 0.083(10) 0.163(18) 0.008(11) 0.007(15) 0.049(11) C12 0.116(15) 0.180(18) 0.141(17) -0.018(14) 0.007(12) 0.050(13) C13 0.101(11) 0.070(7) 0.110(11) -0.010(7) -0.019(8) 0.026(7) C14 0.133(19) 0.19(2) 0.56(6) -0.19(3) 0.18(3) -0.026(16) C15 0.40(5) 0.17(2) 0.30(4) 0.10(2) 0.15(3) 0.20(3) C16 0.28(3) 0.33(4) 0.27(3) -0.24(3) -0.17(3) 0.18(3) C17 0.076(8) 0.110(9) 0.052(7) 0.012(6) 0.005(6) 0.021(7) C18 0.066(8) 0.120(10) 0.063(7) 0.013(7) 0.023(6) -0.006(7) C19 0.094(10) 0.103(9) 0.062(7) 0.016(7) 0.019(6) 0.005(7) C20 0.057(7) 0.114(9) 0.064(7) -0.010(7) -0.001(5) 0.012(6) C21 0.084(9) 0.090(8) 0.065(8) 0.000(6) 0.019(6) -0.016(7) O5 0.100(8) 0.166(9) 0.084(7) -0.008(6) -0.008(6) 0.051(7) O6 0.078(8) 0.186(11) 0.117(9) 0.034(7) 0.020(6) 0.004(7) O7 0.144(10) 0.155(9) 0.091(8) 0.052(7) 0.031(7) 0.012(7) O8 0.123(9) 0.137(8) 0.090(7) -0.046(6) -0.017(6) 0.011(6) O9 0.165(11) 0.109(7) 0.123(9) -0.034(7) 0.030(8) -0.048(7) _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 Sn1 O4 1.953(7) . ? Sn1 O2 2.071(6) . ? Sn1 O1 2.079(6) . ? Sn1 Cr1 2.5754(17) . ? Sn2 O3 1.962(7) . ? Sn2 O1 2.162(6) . ? Sn2 O2 2.165(7) . ? Cr1 C19 1.826(13) . ? Cr1 C20 1.867(13) . ? Cr1 C18 1.883(14) . ? Cr1 C17 1.886(14) . ? Cr1 C21 1.889(13) . ? O1 C1 1.442(12) . ? O2 C5 1.444(11) . ? O3 C9 1.413(14) . ? O4 C13 1.433(15) . ? C1 C2 1.505(18) . ? C1 C4 1.51(2) . ? C1 C3 1.520(19) . ? C5 C8 1.48(2) . ? C5 C7 1.494(18) . ? C5 C6 1.52(2) . ? C9 C12 1.47(2) . ? C9 C10 1.497(18) . ? C9 C11 1.51(2) . ? C13 C15 1.39(2) . ? C13 C14 1.43(2) . ? C13 C16 1.44(2) . ? C17 O5 1.130(14) . ? C18 O6 1.117(15) . ? C19 O7 1.149(14) . ? C20 O8 1.147(14) . ? C21 O9 1.113(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Sn1 O2 94.1(3) . . ? O4 Sn1 O1 94.3(3) . . ? O2 Sn1 O1 75.8(3) . . ? O4 Sn1 Cr1 135.6(3) . . ? O2 Sn1 Cr1 121.82(19) . . ? O1 Sn1 Cr1 117.70(19) . . ? O3 Sn2 O1 89.6(3) . . ? O3 Sn2 O2 86.7(3) . . ? O1 Sn2 O2 72.2(2) . . ? C19 Cr1 C20 88.1(6) . . ? C19 Cr1 C18 92.1(6) . . ? C20 Cr1 C18 92.1(6) . . ? C19 Cr1 C17 89.1(5) . . ? C20 Cr1 C17 89.9(5) . . ? C18 Cr1 C17 177.7(5) . . ? C19 Cr1 C21 92.2(6) . . ? C20 Cr1 C21 178.5(5) . . ? C18 Cr1 C21 89.3(6) . . ? C17 Cr1 C21 88.6(6) . . ? C19 Cr1 Sn1 175.8(5) . . ? C20 Cr1 Sn1 88.8(4) . . ? C18 Cr1 Sn1 90.8(4) . . ? C17 Cr1 Sn1 88.1(4) . . ? C21 Cr1 Sn1 90.9(4) . . ? C1 O1 Sn1 128.8(7) . . ? C1 O1 Sn2 124.5(7) . . ? Sn1 O1 Sn2 104.8(2) . . ? C5 O2 Sn1 129.8(7) . . ? C5 O2 Sn2 125.2(7) . . ? Sn1 O2 Sn2 105.0(3) . . ? C9 O3 Sn2 128.0(7) . . ? C13 O4 Sn1 133.3(8) . . ? O1 C1 C2 109.6(11) . . ? O1 C1 C4 107.3(11) . . ? C2 C1 C4 110.8(13) . . ? O1 C1 C3 106.0(10) . . ? C2 C1 C3 110.3(13) . . ? C4 C1 C3 112.7(14) . . ? O2 C5 C8 106.5(11) . . ? O2 C5 C7 106.9(10) . . ? C8 C5 C7 112.2(16) . . ? O2 C5 C6 108.3(10) . . ? C8 C5 C6 109.3(15) . . ? C7 C5 C6 113.3(14) . . ? O3 C9 C12 109.1(12) . . ? O3 C9 C10 109.0(12) . . ? C12 C9 C10 111.9(13) . . ? O3 C9 C11 106.0(11) . . ? C12 C9 C11 109.1(14) . . ? C10 C9 C11 111.5(14) . . ? C15 C13 C14 109(2) . . ? C15 C13 O4 105.7(15) . . ? C14 C13 O4 111.2(12) . . ? C15 C13 C16 109(2) . . ? C14 C13 C16 110(2) . . ? O4 C13 C16 111.4(13) . . ? O5 C17 Cr1 178.1(11) . . ? O6 C18 Cr1 177.3(13) . . ? O7 C19 Cr1 178.6(13) . . ? O8 C20 Cr1 176.5(12) . . ? O9 C21 Cr1 175.5(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.19 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.868 _refine_diff_density_min -1.413 _refine_diff_density_rms 0.154 #===END data_comp_3b _database_code_depnum_ccdc_archive 'CCDC 256749' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 Cr2 O14 Sn2' _chemical_formula_weight 913.93 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' Cr Cr 0.3209 0.6236 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 12.599(3) _cell_length_b 11.177(2) _cell_length_c 13.217(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.24(3) _cell_angle_gamma 90.00 _cell_volume 1853.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.959 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8044 _exptl_absorpt_correction_T_max 0.9964 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe AED2' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4.0 _diffrn_reflns_number 3460 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0126 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.09 _reflns_number_total 3460 _reflns_number_gt 3204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (Stoe, 1996)' _computing_cell_refinement 'STADI4 (Stoe, 1996)' _computing_data_reduction 'X-RED (Stoe, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0435P)^2^+3.2498P] 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 3460 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.159 _refine_ls_shift/su_mean 0.007 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 Sn1 Sn 0.72178(3) 0.2500 0.85208(2) 0.03347(12) Uani 1 2 d S . . Sn2 Sn 0.78460(3) 0.2500 0.61122(3) 0.03604(12) Uani 1 2 d S . . Cr1 Cr 0.87414(7) 0.2500 0.99741(6) 0.0392(2) Uani 1 2 d S . . Cr2 Cr 0.68931(8) 0.2500 0.42635(7) 0.0540(3) Uani 1 2 d S . . O1 O 0.7380(2) 0.1369(2) 0.72701(18) 0.0382(6) Uani 1 1 d . . . O2 O 0.5658(3) 0.2500 0.8259(3) 0.0530(11) Uani 1 2 d S . . O3 O 0.9312(3) 0.2500 0.6758(3) 0.0522(10) Uani 1 2 d S . . C1 C 0.7120(4) 0.0093(4) 0.7199(3) 0.0495(10) Uani 1 1 d . . . C2 C 0.7109(5) -0.0400(4) 0.8261(4) 0.0657(13) Uani 1 1 d . . . H2A H 0.6558 -0.0013 0.8597 0.099 Uiso 1 1 calc R . . H2B H 0.7787 -0.0255 0.8634 0.099 Uiso 1 1 calc R . . H2C H 0.6976 -0.1245 0.8228 0.099 Uiso 1 1 calc R . . C3 C 0.6015(4) -0.0025(5) 0.6634(4) 0.0729(15) Uani 1 1 d . . . H3A H 0.6024 0.0300 0.5963 0.109 Uiso 1 1 calc R . . H3B H 0.5508 0.0406 0.6994 0.109 Uiso 1 1 calc R . . H3C H 0.5818 -0.0854 0.6590 0.109 Uiso 1 1 calc R . . C4 C 0.7987(5) -0.0507(4) 0.6658(4) 0.0700(14) Uani 1 1 d . . . H4A H 0.7989 -0.0183 0.5985 0.105 Uiso 1 1 calc R . . H4B H 0.7855 -0.1352 0.6616 0.105 Uiso 1 1 calc R . . H4C H 0.8667 -0.0366 0.7029 0.105 Uiso 1 1 calc R . . C5 C 0.4807(5) 0.2500 0.8894(5) 0.0572(16) Uani 1 2 d S . . C6 C 0.3899(9) 0.2500 0.8354(11) 0.39(3) Uani 1 2 d S . . H6A H 0.3885 0.3134 0.7863 0.592 Uiso 0.50 1 calc PR . . H6B H 0.3337 0.2619 0.8788 0.592 Uiso 0.50 1 calc PR . . H6C H 0.3799 0.1747 0.8009 0.592 Uiso 0.50 1 calc PR . . C7 C 1.1181(6) 0.2500 0.7171(7) 0.102(4) Uani 1 2 d S . . H7A H 1.1130 0.3211 0.7571 0.153 Uiso 0.50 1 calc PR . . H7B H 1.1861 0.2479 0.6899 0.153 Uiso 1 2 calc SR . . H7C H 1.1108 0.1809 0.7591 0.153 Uiso 0.50 1 calc PR . . C8 C 0.4927(10) 0.1535(13) 0.9614(10) 0.279(10) Uani 1 1 d . . . H8A H 0.5620 0.1578 0.9982 0.418 Uiso 1 1 calc R . . H8B H 0.4853 0.0785 0.9261 0.418 Uiso 1 1 calc R . . H8C H 0.4389 0.1597 1.0081 0.418 Uiso 1 1 calc R . . C9 C 1.0305(5) 0.2500 0.6310(5) 0.0544(16) Uani 1 2 d S . . C10 C 1.0364(5) 0.1410(8) 0.5661(6) 0.118(3) Uani 1 1 d . . . H10A H 1.0336 0.0708 0.6075 0.177 Uiso 1 1 calc R . . H10B H 1.1019 0.1418 0.5344 0.177 Uiso 1 1 calc R . . H10C H 0.9773 0.1407 0.5148 0.177 Uiso 1 1 calc R . . O4 O 1.0622(4) 0.2500 1.1541(4) 0.0839(17) Uani 1 2 d S . . O5 O 0.9888(3) 0.0588(3) 0.8865(3) 0.0773(11) Uani 1 1 d . . . O6 O 0.7674(4) 0.0618(5) 1.1179(3) 0.1007(15) Uani 1 1 d . . . O7 O 0.4770(4) 0.2500 0.5182(5) 0.0790(16) Uani 1 2 d S . . O8 O 0.6871(4) -0.0203(5) 0.4047(4) 0.1063(16) Uani 1 1 d . . . O9 O 0.8942(6) 0.2500 0.3231(5) 0.165(5) Uani 1 2 d S . . O10 O 0.5640(6) 0.2500 0.2229(4) 0.121(3) Uani 1 2 d S . . C11 C 0.9898(5) 0.2500 1.0955(5) 0.0556(16) Uani 1 2 d S . . C12 C 0.9439(3) 0.1310(4) 0.9261(3) 0.0511(10) Uani 1 1 d . . . C13 C 0.8062(4) 0.1319(5) 1.0707(4) 0.0590(12) Uani 1 1 d . . . C14 C 0.6128(6) 0.2500 0.3000(6) 0.082(3) Uani 1 2 d S . . C15 C 0.6898(4) 0.0806(6) 0.4169(4) 0.0727(15) Uani 1 1 d . . . C16 C 0.8181(7) 0.2500 0.3641(6) 0.097(3) Uani 1 2 d S . . C17 C 0.5575(6) 0.2500 0.4868(5) 0.0544(16) Uani 1 2 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 Sn1 0.0381(2) 0.0322(2) 0.02918(19) 0.000 -0.00199(14) 0.000 Sn2 0.0369(2) 0.0411(2) 0.0296(2) 0.000 0.00026(14) 0.000 Cr1 0.0432(5) 0.0401(5) 0.0326(4) 0.000 -0.0054(4) 0.000 Cr2 0.0498(6) 0.0803(8) 0.0308(5) 0.000 -0.0032(4) 0.000 O1 0.0499(15) 0.0292(13) 0.0356(13) -0.0046(10) 0.0041(11) -0.0047(11) O2 0.036(2) 0.082(3) 0.040(2) 0.000 0.0024(17) 0.000 O3 0.034(2) 0.075(3) 0.047(2) 0.000 0.0010(17) 0.000 C1 0.066(3) 0.031(2) 0.052(2) -0.0066(18) 0.006(2) -0.0081(19) C2 0.099(4) 0.035(2) 0.063(3) 0.005(2) 0.014(3) -0.012(2) C3 0.077(3) 0.065(3) 0.075(3) -0.011(3) -0.003(3) -0.029(3) C4 0.102(4) 0.042(3) 0.068(3) -0.007(2) 0.015(3) 0.017(3) C5 0.046(3) 0.074(5) 0.054(4) 0.000 0.018(3) 0.000 C6 0.051(6) 1.03(8) 0.110(11) 0.000 0.028(7) 0.000 C7 0.043(4) 0.176(11) 0.088(6) 0.000 0.002(4) 0.000 C8 0.229(12) 0.34(2) 0.296(17) 0.197(15) 0.201(13) 0.117(13) C9 0.037(3) 0.076(5) 0.051(4) 0.000 0.009(3) 0.000 C10 0.073(4) 0.149(7) 0.132(6) -0.058(6) 0.012(4) 0.025(4) O4 0.070(3) 0.098(4) 0.076(3) 0.000 -0.037(3) 0.000 O5 0.090(3) 0.067(2) 0.074(2) -0.005(2) 0.010(2) 0.029(2) O6 0.104(3) 0.098(3) 0.101(3) 0.047(3) 0.016(3) -0.018(3) O7 0.057(3) 0.091(4) 0.090(4) 0.000 0.016(3) 0.000 O8 0.128(4) 0.089(3) 0.095(3) -0.040(3) -0.022(3) 0.026(3) O9 0.088(5) 0.348(15) 0.063(4) 0.000 0.032(4) 0.000 O10 0.125(6) 0.184(8) 0.046(3) 0.000 -0.030(3) 0.000 C11 0.058(4) 0.058(4) 0.048(4) 0.000 -0.008(3) 0.000 C12 0.053(2) 0.052(3) 0.047(2) 0.004(2) -0.0029(19) 0.006(2) C13 0.059(3) 0.063(3) 0.053(3) 0.013(2) -0.003(2) -0.001(2) C14 0.067(5) 0.130(8) 0.048(4) 0.000 -0.007(4) 0.000 C15 0.073(3) 0.093(5) 0.050(3) -0.022(3) -0.008(2) 0.013(3) C16 0.069(5) 0.184(11) 0.040(4) 0.000 0.009(4) 0.000 C17 0.061(4) 0.057(4) 0.044(3) 0.000 -0.009(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O2 1.964(4) . ? Sn1 O1 2.106(2) 4_565 ? Sn1 O1 2.106(2) . ? Sn1 Cr1 2.5886(12) . ? Sn2 O3 1.963(4) . ? Sn2 O1 2.110(3) . ? Sn2 O1 2.110(3) 4_565 ? Sn2 Cr2 2.6222(12) . ? Cr1 C11 1.860(6) . ? Cr1 C13 1.888(5) . ? Cr1 C13 1.888(5) 4_565 ? Cr1 C12 1.892(5) 4_565 ? Cr1 C12 1.892(5) . ? Cr2 C14 1.851(7) . ? Cr2 C16 1.885(9) . ? Cr2 C15 1.898(7) . ? Cr2 C15 1.898(7) 4_565 ? Cr2 C17 1.907(7) . ? O1 C1 1.464(5) . ? O2 C5 1.421(7) . ? O3 C9 1.432(7) . ? C1 C2 1.509(6) . ? C1 C4 1.517(6) . ? C1 C3 1.524(7) . ? C5 C6 1.293(14) . ? C5 C8 1.437(11) 4_565 ? C5 C8 1.437(11) . ? C7 C9 1.511(10) . ? C9 C10 1.495(8) 4_565 ? C9 C10 1.495(8) . ? O4 C11 1.141(8) . ? O5 C12 1.140(5) . ? O6 C13 1.139(6) . ? O7 C17 1.131(8) . ? O8 C15 1.139(8) . ? O9 C16 1.143(10) . ? O10 C14 1.141(9) . ? 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 O2 Sn1 O1 91.64(12) . 4_565 ? O2 Sn1 O1 91.64(12) . . ? O1 Sn1 O1 73.81(14) 4_565 . ? O2 Sn1 Cr1 142.47(12) . . ? O1 Sn1 Cr1 117.65(7) 4_565 . ? O1 Sn1 Cr1 117.65(7) . . ? O3 Sn2 O1 89.89(12) . . ? O3 Sn2 O1 89.89(12) . 4_565 ? O1 Sn2 O1 73.65(13) . 4_565 ? O3 Sn2 Cr2 137.53(12) . . ? O1 Sn2 Cr2 122.81(7) . . ? O1 Sn2 Cr2 122.81(7) 4_565 . ? C11 Cr1 C13 90.3(2) . . ? C11 Cr1 C13 90.3(2) . 4_565 ? C13 Cr1 C13 88.7(3) . 4_565 ? C11 Cr1 C12 88.7(2) . 4_565 ? C13 Cr1 C12 179.0(2) . 4_565 ? C13 Cr1 C12 91.0(2) 4_565 4_565 ? C11 Cr1 C12 88.7(2) . . ? C13 Cr1 C12 91.0(2) . . ? C13 Cr1 C12 179.0(2) 4_565 . ? C12 Cr1 C12 89.3(3) 4_565 . ? C11 Cr1 Sn1 176.3(2) . . ? C13 Cr1 Sn1 92.31(14) . . ? C13 Cr1 Sn1 92.31(14) 4_565 . ? C12 Cr1 Sn1 88.69(13) 4_565 . ? C12 Cr1 Sn1 88.69(13) . . ? C14 Cr2 C16 90.2(4) . . ? C14 Cr2 C15 86.86(15) . . ? C16 Cr2 C15 87.88(18) . . ? C14 Cr2 C15 86.86(15) . 4_565 ? C16 Cr2 C15 87.88(18) . 4_565 ? C15 Cr2 C15 172.4(3) . 4_565 ? C14 Cr2 C17 88.6(3) . . ? C16 Cr2 C17 178.9(3) . . ? C15 Cr2 C17 92.06(18) . . ? C15 Cr2 C17 92.06(18) 4_565 . ? C14 Cr2 Sn2 175.9(3) . . ? C16 Cr2 Sn2 93.9(2) . . ? C15 Cr2 Sn2 93.28(15) . . ? C15 Cr2 Sn2 93.28(15) 4_565 . ? C17 Cr2 Sn2 87.24(19) . . ? C1 O1 Sn1 126.7(2) . . ? C1 O1 Sn2 127.8(2) . . ? Sn1 O1 Sn2 105.24(11) . . ? C5 O2 Sn1 133.8(4) . . ? C9 O3 Sn2 130.1(4) . . ? O1 C1 C2 108.5(3) . . ? O1 C1 C4 107.1(4) . . ? C2 C1 C4 110.2(4) . . ? O1 C1 C3 107.7(4) . . ? C2 C1 C3 109.8(4) . . ? C4 C1 C3 113.3(4) . . ? C6 C5 O2 110.6(8) . . ? C6 C5 C8 113.6(8) . 4_565 ? O2 C5 C8 110.6(5) . 4_565 ? C6 C5 C8 113.6(8) . . ? O2 C5 C8 110.6(5) . . ? C8 C5 C8 97.3(14) 4_565 . ? O3 C9 C10 109.1(4) . 4_565 ? O3 C9 C10 109.1(4) . . ? C10 C9 C10 109.1(8) 4_565 . ? O3 C9 C7 107.1(5) . . ? C10 C9 C7 111.2(4) 4_565 . ? C10 C9 C7 111.2(4) . . ? O4 C11 Cr1 178.5(7) . . ? O5 C12 Cr1 177.2(4) . . ? O6 C13 Cr1 177.6(5) . . ? O10 C14 Cr2 178.8(8) . . ? O8 C15 Cr2 175.4(5) . . ? O9 C16 Cr2 177.7(7) . . ? O7 C17 Cr2 176.8(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.243 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.102 #===END data_comp_3a _database_code_depnum_ccdc_archive 'CCDC 256750' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 Cr O14 Sn2 W' _chemical_formula_weight 1045.78 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' 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' Cr Cr 0.3209 0.6236 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 12.550(3) _cell_length_b 11.190(2) _cell_length_c 13.390(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.97(3) _cell_angle_gamma 90.00 _cell_volume 1873.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 4.716 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4477 _exptl_absorpt_correction_T_max 0.9913 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe STADI4' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2.8 _diffrn_reflns_number 4522 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4522 _reflns_number_gt 3898 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4522 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1990 _refine_ls_wR_factor_gt 0.1904 _refine_ls_goodness_of_fit_ref 1.707 _refine_ls_restrained_S_all 1.707 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.004 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 Cr1 Cr 0.12523(10) 0.2500 0.50292(9) 0.0192(3) Uani 1 2 d S . . W1 W 0.31154(4) 0.2500 1.07682(4) 0.0575(2) Uani 1 2 d S . . Sn1 Sn 0.21404(5) 0.2500 0.88562(5) 0.0343(2) Uani 1 2 d S . . Sn2 Sn 0.27885(5) 0.2500 0.64772(5) 0.0324(2) Uani 1 2 d S . . O1 O 0.2600(4) 0.1368(5) 0.7714(4) 0.0368(11) Uani 1 1 d . . . O2 O 0.0658(6) 0.2500 0.8210(7) 0.052(2) Uani 1 2 d S . . O3 O 0.4321(6) 0.2500 0.6722(6) 0.051(2) Uani 1 2 d S . . O4 O 0.2330(7) 0.0635(10) 0.3801(8) 0.096(3) Uani 1 1 d . . . O5 O 0.0115(7) 0.0592(7) 0.6146(6) 0.074(2) Uani 1 1 d . . . O6 O -0.0643(9) 0.2500 0.3498(10) 0.086(4) Uani 1 2 d S . . O7 O 0.5337(8) 0.2500 0.9814(10) 0.076(3) Uani 1 2 d S . . O8 O 0.4332(12) 0.2500 1.2846(9) 0.110(6) Uani 1 2 d S . . O9 O 0.0937(11) 0.2500 1.1803(11) 0.138(9) Uani 1 2 d S . . O10 O 0.3103(9) -0.0337(11) 1.0937(10) 0.111(4) Uani 1 1 d . . . C1 C 0.2853(8) 0.0092(8) 0.7805(7) 0.050(2) Uani 1 1 d . . . C2 C 0.1991(10) -0.0501(10) 0.8345(9) 0.073(3) Uani 1 1 d . . . H2A H 0.1984 -0.0165 0.9004 0.110 Uiso 1 1 calc R . . H2B H 0.2131 -0.1343 0.8397 0.110 Uiso 1 1 calc R . . H2C H 0.1309 -0.0373 0.7977 0.110 Uiso 1 1 calc R . . C3 C 0.2871(10) -0.0419(9) 0.6714(8) 0.063(3) Uani 1 1 d . . . H3A H 0.3415 -0.0019 0.6378 0.094 Uiso 1 1 calc R . . H3B H 0.2188 -0.0292 0.6350 0.094 Uiso 1 1 calc R . . H3C H 0.3023 -0.1260 0.6747 0.094 Uiso 1 1 calc R . . C4 C 0.3993(10) 0.0013(12) 0.8338(10) 0.082(4) Uani 1 1 d . . . H4A H 0.4484 0.0428 0.7949 0.123 Uiso 1 1 calc R . . H4B H 0.4202 -0.0810 0.8407 0.123 Uiso 1 1 calc R . . H4C H 0.4002 0.0373 0.8990 0.123 Uiso 1 1 calc R . . C5 C -0.0294(9) 0.2500 0.8688(10) 0.052(3) Uani 1 2 d S . . C6 C -0.1184(12) 0.2500 0.7875(15) 0.107(9) Uani 1 2 d S . . H6A H -0.1200 0.3213 0.7501 0.160 Uiso 1 1 d . . . H6B H -0.1882 0.2500 0.8230 0.160 Uiso 1 2 d S . . C7 C -0.0365(10) 0.1377(16) 0.9296(14) 0.113(6) Uani 1 1 d . . . H7A H -0.0302 0.0694 0.8872 0.169 Uiso 1 1 calc R . . H7B H -0.1041 0.1354 0.9581 0.169 Uiso 1 1 calc R . . H7C H 0.0204 0.1368 0.9825 0.169 Uiso 1 1 calc R . . C8 C 0.5190(10) 0.2500 0.6103(10) 0.053(3) Uani 1 2 d S . . C9 C 0.6147(18) 0.2500 0.668(4) 0.28(4) Uani 1 2 d S . . H9A H 0.6352 0.3176 0.7091 0.420 Uiso 1 1 d . . . H9B H 0.6832 0.2500 0.6220 0.420 Uiso 1 2 d S . . C10 C 0.532(3) 0.147(2) 0.572(3) 0.37(4) Uani 1 1 d . . . H10A H 0.5336 0.0876 0.6237 0.552 Uiso 1 1 calc R . . H10B H 0.5983 0.1459 0.5413 0.552 Uiso 1 1 calc R . . H10C H 0.4740 0.1310 0.5224 0.552 Uiso 1 1 calc R . . C11 C 0.1959(8) 0.1286(12) 0.4291(7) 0.062(3) Uani 1 1 d . . . C12 C 0.0562(7) 0.1278(9) 0.5750(7) 0.053(2) Uani 1 1 d . . . C13 C 0.0082(11) 0.2500 0.4060(11) 0.057(3) Uani 1 2 d S . . C14 C 0.4531(11) 0.2500 1.0126(11) 0.058(3) Uani 1 2 d S . . C15 C 0.3929(12) 0.2500 1.2131(14) 0.080(5) Uani 1 2 d S . . C16 C 0.1695(19) 0.2500 1.1425(14) 0.107(8) Uani 1 2 d S . . C17 C 0.3113(9) 0.0691(15) 1.0851(9) 0.077(4) 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 Cr1 0.0212(6) 0.0220(6) 0.0131(6) 0.000 -0.0055(5) 0.000 W1 0.0501(3) 0.0876(5) 0.0338(3) 0.000 -0.0015(2) 0.000 Sn1 0.0322(3) 0.0425(4) 0.0277(4) 0.000 0.0011(3) 0.000 Sn2 0.0340(3) 0.0348(4) 0.0277(4) 0.000 -0.0006(3) 0.000 O1 0.045(3) 0.031(3) 0.034(3) 0.002(2) 0.005(2) 0.006(2) O2 0.031(4) 0.080(7) 0.045(5) 0.000 0.002(3) 0.000 O3 0.033(4) 0.086(7) 0.033(4) 0.000 0.001(3) 0.000 O4 0.098(6) 0.099(7) 0.093(7) -0.035(6) 0.023(5) 0.024(5) O5 0.088(5) 0.063(5) 0.072(5) 0.003(4) 0.013(4) -0.027(4) O6 0.054(6) 0.125(11) 0.073(8) 0.000 -0.029(6) 0.000 O7 0.046(5) 0.087(8) 0.097(9) 0.000 0.016(5) 0.000 O8 0.105(10) 0.193(18) 0.029(6) 0.000 -0.011(6) 0.000 O9 0.057(7) 0.30(3) 0.060(8) 0.000 0.021(6) 0.000 O10 0.120(9) 0.093(8) 0.115(9) 0.052(7) -0.019(7) -0.018(6) C1 0.064(5) 0.034(4) 0.051(5) 0.006(4) 0.003(4) 0.007(4) C2 0.108(9) 0.042(5) 0.073(7) 0.015(5) 0.025(6) -0.019(5) C3 0.104(8) 0.038(5) 0.047(5) -0.007(4) 0.010(5) 0.007(5) C4 0.087(8) 0.076(8) 0.078(8) 0.004(6) -0.013(6) 0.047(7) C5 0.033(5) 0.082(10) 0.044(7) 0.000 0.011(5) 0.000 C6 0.038(7) 0.21(3) 0.068(12) 0.000 -0.001(7) 0.000 C7 0.063(7) 0.138(14) 0.139(14) 0.048(12) 0.018(8) -0.023(8) C8 0.041(6) 0.077(9) 0.044(7) 0.000 0.009(5) 0.000 C9 0.041(11) 0.56(11) 0.24(5) 0.000 0.038(19) 0.000 C10 0.38(5) 0.15(3) 0.64(8) -0.15(4) 0.43(6) -0.07(3) C11 0.055(5) 0.083(8) 0.046(5) -0.007(5) -0.005(4) -0.002(5) C12 0.053(4) 0.059(6) 0.043(5) -0.004(4) -0.009(4) -0.005(4) C13 0.055(7) 0.073(9) 0.043(7) 0.000 0.005(6) 0.000 C14 0.054(7) 0.069(9) 0.047(7) 0.000 -0.014(6) 0.000 C15 0.048(7) 0.129(16) 0.060(10) 0.000 -0.013(7) 0.000 C16 0.103(15) 0.17(3) 0.043(10) 0.000 0.003(10) 0.000 C17 0.062(6) 0.115(11) 0.052(6) 0.024(7) -0.012(5) -0.020(7) _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 Cr1 C13 1.874(14) . ? Cr1 C12 1.923(11) . ? Cr1 C12 1.923(11) 4_565 ? Cr1 C11 1.940(12) . ? Cr1 C11 1.940(12) 4_565 ? Cr1 Sn2 2.6130(16) . ? W1 C15 2.012(17) . ? W1 C17 2.027(17) 4_565 ? W1 C17 2.027(17) . ? W1 C14 2.040(16) . ? W1 C16 2.06(2) . ? W1 Sn1 2.7402(12) . ? Sn1 O2 1.983(8) . ? Sn1 O1 2.105(5) . ? Sn1 O1 2.105(5) 4_565 ? Sn2 O3 1.924(8) . ? Sn2 O1 2.115(5) 4_565 ? Sn2 O1 2.115(5) . ? O1 C1 1.465(10) . ? O2 C5 1.404(14) . ? O3 C8 1.425(15) . ? O4 C11 1.109(14) . ? O5 C12 1.112(12) . ? O6 C13 1.129(17) . ? O7 C14 1.127(18) . ? O8 C15 1.044(19) . ? O9 C16 1.12(3) . ? O10 C17 1.156(18) . ? C1 C2 1.506(14) . ? C1 C4 1.546(15) . ? C1 C3 1.571(14) . ? C5 C6 1.49(2) . ? C5 C7 1.504(17) 4_565 ? C5 C7 1.504(17) . ? C8 C10 1.27(2) . ? C8 C10 1.27(2) 4_565 ? C8 C9 1.37(4) . ? C9 C10 1.96(5) . ? C9 C10 1.96(5) 4_565 ? 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 C13 Cr1 C12 89.3(4) . . ? C13 Cr1 C12 89.3(4) . 4_565 ? C12 Cr1 C12 90.7(6) . 4_565 ? C13 Cr1 C11 90.7(4) . . ? C12 Cr1 C11 90.2(5) . . ? C12 Cr1 C11 179.1(5) 4_565 . ? C13 Cr1 C11 90.7(4) . 4_565 ? C12 Cr1 C11 179.1(5) . 4_565 ? C12 Cr1 C11 90.2(5) 4_565 4_565 ? C11 Cr1 C11 88.9(7) . 4_565 ? C13 Cr1 Sn2 176.0(4) . . ? C12 Cr1 Sn2 87.9(3) . . ? C12 Cr1 Sn2 87.9(3) 4_565 . ? C11 Cr1 Sn2 92.2(3) . . ? C11 Cr1 Sn2 92.2(3) 4_565 . ? C15 W1 C17 87.3(3) . 4_565 ? C15 W1 C17 87.3(3) . . ? C17 W1 C17 173.7(7) 4_565 . ? C15 W1 C14 89.4(6) . . ? C17 W1 C14 91.6(4) 4_565 . ? C17 W1 C14 91.6(4) . . ? C15 W1 C16 90.2(7) . . ? C17 W1 C16 88.3(4) 4_565 . ? C17 W1 C16 88.3(4) . . ? C14 W1 C16 179.6(6) . . ? C15 W1 Sn1 176.1(5) . . ? C17 W1 Sn1 92.8(3) 4_565 . ? C17 W1 Sn1 92.8(3) . . ? C14 W1 Sn1 86.6(4) . . ? C16 W1 Sn1 93.8(5) . . ? O2 Sn1 O1 89.3(3) . . ? O2 Sn1 O1 89.3(3) . 4_565 ? O1 Sn1 O1 74.0(3) . 4_565 ? O2 Sn1 W1 137.2(3) . . ? O1 Sn1 W1 123.41(14) . . ? O1 Sn1 W1 123.41(14) 4_565 . ? O3 Sn2 O1 92.5(2) . 4_565 ? O3 Sn2 O1 92.5(2) . . ? O1 Sn2 O1 73.6(3) 4_565 . ? O3 Sn2 Cr1 142.1(3) . . ? O1 Sn2 Cr1 117.11(15) 4_565 . ? O1 Sn2 Cr1 117.11(15) . . ? C1 O1 Sn1 126.7(5) . . ? C1 O1 Sn2 127.6(5) . . ? Sn1 O1 Sn2 105.3(2) . . ? C5 O2 Sn1 127.2(8) . . ? C8 O3 Sn2 134.8(8) . . ? O1 C1 C2 108.1(8) . . ? O1 C1 C4 106.2(8) . . ? C2 C1 C4 115.3(10) . . ? O1 C1 C3 107.4(7) . . ? C2 C1 C3 110.8(9) . . ? C4 C1 C3 108.7(9) . . ? O2 C5 C6 106.3(11) . . ? O2 C5 C7 109.9(8) . 4_565 ? C6 C5 C7 108.7(9) . 4_565 ? O2 C5 C7 109.9(8) . . ? C6 C5 C7 108.7(9) . . ? C7 C5 C7 113.3(18) 4_565 . ? C10 C8 C10 129(4) . 4_565 ? C10 C8 C9 95(3) . . ? C10 C8 C9 95(3) 4_565 . ? C10 C8 O3 111.4(13) . . ? C10 C8 O3 111.4(13) 4_565 . ? C9 C8 O3 110(2) . . ? C8 C9 C10 40.5(14) . . ? C8 C9 C10 40.5(14) . 4_565 ? C10 C9 C10 72(3) . 4_565 ? C8 C10 C9 44.3(17) . . ? O4 C11 Cr1 174.4(11) . . ? O5 C12 Cr1 176.4(9) . . ? O6 C13 Cr1 178.0(14) . . ? O7 C14 W1 176.9(12) . . ? O8 C15 W1 178.5(17) . . ? O9 C16 W1 178.3(18) . . ? O10 C17 W1 177.3(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.462 _refine_diff_density_min -3.064 _refine_diff_density_rms 0.238 #========================================================================== #_eof # End of Crystallographic Information File