data_vc1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H88 O20 P4 Sn6' _chemical_formula_weight 1965.32 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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 16.9713(7) _cell_length_b 15.6743(6) _cell_length_c 14.2523(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.5550(10) _cell_angle_gamma 90.00 _cell_volume 3652.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7846 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 29.9 _exptl_crystal_description 'block, cut' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 2.174 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.5575 _exptl_absorpt_correction_T_max 0.6948 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14858 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5373 _reflns_number_gt 4473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, 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^)+(0.0300P)^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 5373 _refine_ls_number_parameters 235 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.665762(15) 0.5000 0.382274(17) 0.02726(7) Uani 1 2 d S . . Sn2 Sn 0.488038(10) 0.607488(11) 0.324346(12) 0.02498(5) Uani 1 1 d . . . P1 P 0.62936(4) 0.35041(4) 0.52281(5) 0.02780(14) Uani 1 1 d . . . H1 H 0.6666(17) 0.2846(16) 0.5560(19) 0.031(7) Uiso 1 1 d . . . O1 O 0.60127(11) 0.59279(11) 0.27852(13) 0.0292(4) Uani 1 1 d . A . O2 O 0.42874(15) 0.5000 0.23882(17) 0.0287(5) Uani 1 2 d S . . O3 O 0.54518(14) 0.5000 0.39245(16) 0.0243(5) Uani 1 2 d S . . O4 O 0.69040(11) 0.40561(12) 0.48884(13) 0.0328(4) Uani 1 1 d . A . O5 O 0.55869(11) 0.67851(11) 0.43880(12) 0.0295(4) Uani 1 1 d . . . O6 O 0.39629(11) 0.60719(11) 0.39454(13) 0.0307(4) Uani 1 1 d . . . C1 C 0.43943(18) 0.70323(17) 0.2202(2) 0.0358(6) Uani 1 1 d D A . H1A H 0.4705 0.7036 0.1713 0.043 Uiso 1 1 calc R . . H1B H 0.3827 0.6884 0.1869 0.043 Uiso 1 1 calc R . . C2 C 0.4409(3) 0.79211(19) 0.2619(3) 0.0597(10) Uani 1 1 d D . . H2A H 0.4958 0.8038 0.3038 0.072 Uiso 1 1 calc R A . H2B H 0.4026 0.7946 0.3025 0.072 Uiso 1 1 calc R . . C3 C 0.4183(3) 0.8607(2) 0.1843(3) 0.0673(11) Uani 1 1 d D A . H3A H 0.3660 0.8458 0.1381 0.081 Uiso 1 1 calc R . . H3B H 0.4109 0.9150 0.2150 0.081 Uiso 1 1 calc R . . C4 C 0.4816(3) 0.8717(3) 0.1300(4) 0.108(2) Uani 1 1 d D . . H4A H 0.5311 0.8948 0.1734 0.162 Uiso 1 1 calc R A . H4B H 0.4614 0.9107 0.0760 0.162 Uiso 1 1 calc R . . H4C H 0.4934 0.8169 0.1053 0.162 Uiso 1 1 calc R . . C5 C 0.7792(3) 0.5040(18) 0.3454(3) 0.0377(17) Uani 0.50 1 d PD A -1 H5A H 0.7715 0.4793 0.2804 0.045 Uiso 0.50 1 calc PR A -1 H5B H 0.7953 0.5638 0.3422 0.045 Uiso 0.50 1 calc PR A -1 C6 C 0.8484(4) 0.4566(4) 0.4168(5) 0.0531(17) Uani 0.50 1 d PD A -1 H6A H 0.8951 0.4506 0.3892 0.064 Uiso 0.50 1 calc PR A -1 H6B H 0.8300 0.3994 0.4290 0.064 Uiso 0.50 1 calc PR A -1 C7 C 0.8752(4) 0.5087(14) 0.5164(4) 0.072(4) Uani 0.50 1 d PD A -1 H7A H 0.9070 0.5595 0.5100 0.087 Uiso 0.50 1 calc PR A -1 H7B H 0.8278 0.5255 0.5390 0.087 Uiso 0.50 1 calc PR A -1 C8 C 0.9270(11) 0.4434(11) 0.5829(11) 0.241(10) Uiso 0.50 1 d PD A -1 H8A H 0.9462 0.4669 0.6480 0.362 Uiso 0.50 1 calc PR A -1 H8B H 0.9736 0.4285 0.5589 0.362 Uiso 0.50 1 calc PR A -1 H8C H 0.8946 0.3927 0.5847 0.362 Uiso 0.50 1 calc PR A -1 C1A C 0.63449(16) 0.65106(17) 0.22728(19) 0.0314(6) Uani 1 1 d . . . C2A C 0.6774(2) 0.7203(2) 0.2726(2) 0.0464(8) Uani 1 1 d . A . H2A H 0.6857 0.7281 0.3400 0.056 Uiso 1 1 calc R . . C3A C 0.7085(2) 0.7788(2) 0.2188(3) 0.0567(9) Uani 1 1 d . . . H3A H 0.7376 0.8266 0.2499 0.068 Uiso 1 1 calc R A . C4A C 0.6972(2) 0.7673(2) 0.1209(3) 0.0535(9) Uani 1 1 d . A . H4A H 0.7189 0.8068 0.0849 0.064 Uiso 1 1 calc R . . C5A C 0.6548(3) 0.6991(2) 0.0761(3) 0.0617(10) Uani 1 1 d . . . H5A H 0.6467 0.6916 0.0087 0.074 Uiso 1 1 calc R A . C6A C 0.6226(2) 0.6393(2) 0.1291(2) 0.0511(8) Uani 1 1 d . A . H6A H 0.5933 0.5917 0.0977 0.061 Uiso 1 1 calc R . . C1B C 0.3519(2) 0.5000 0.1735(3) 0.0316(8) Uani 1 2 d S . . C2B C 0.3448(3) 0.5000 0.0751(3) 0.0515(12) Uani 1 2 d S A . H2B H 0.3924 0.5000 0.0533 0.062 Uiso 1 2 calc SR . . C3B C 0.2699(4) 0.5000 0.0082(4) 0.0715(17) Uani 1 2 d S . . H3B H 0.2662 0.5000 -0.0588 0.086 Uiso 1 2 calc SR A . C4B C 0.2021(4) 0.5000 0.0389(5) 0.0708(18) Uani 1 2 d S A . H4B H 0.1508 0.5000 -0.0071 0.085 Uiso 1 2 calc SR . . C5B C 0.2060(3) 0.5000 0.1369(5) 0.0650(16) Uani 1 2 d S . . H5B H 0.1578 0.5000 0.1573 0.078 Uiso 1 2 calc SR A . C6B C 0.2828(3) 0.5000 0.2059(4) 0.0456(11) Uani 1 2 d S A . H6B H 0.2866 0.5000 0.2730 0.055 Uiso 1 2 calc SR . . 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 0.02500(13) 0.03416(14) 0.02400(12) 0.000 0.00895(9) 0.000 Sn2 0.02803(9) 0.02599(9) 0.02119(9) 0.00166(7) 0.00707(6) 0.00010(7) P1 0.0293(3) 0.0298(3) 0.0247(3) 0.0029(3) 0.0080(3) 0.0052(3) O1 0.0300(10) 0.0328(10) 0.0267(9) 0.0047(7) 0.0109(7) -0.0018(7) O2 0.0318(14) 0.0284(13) 0.0233(12) 0.000 0.0027(10) 0.000 O3 0.0263(13) 0.0258(12) 0.0221(12) 0.000 0.0086(10) 0.000 O4 0.0271(10) 0.0440(11) 0.0282(10) 0.0042(8) 0.0087(7) 0.0029(8) O5 0.0337(10) 0.0282(9) 0.0263(9) -0.0014(7) 0.0080(7) -0.0040(8) O6 0.0306(10) 0.0379(10) 0.0249(9) -0.0034(8) 0.0098(7) -0.0028(8) C1 0.0406(16) 0.0347(15) 0.0327(15) 0.0089(12) 0.0109(12) 0.0048(12) C2 0.086(3) 0.0332(17) 0.058(2) 0.0060(16) 0.016(2) 0.0063(17) C3 0.074(3) 0.0404(19) 0.088(3) 0.023(2) 0.023(2) 0.0163(18) C4 0.091(4) 0.082(3) 0.164(6) 0.074(4) 0.057(4) 0.017(3) C5 0.033(2) 0.050(4) 0.034(2) 0.004(8) 0.0165(18) 0.012(8) C6 0.034(3) 0.062(4) 0.066(4) 0.003(3) 0.017(3) 0.001(3) C7 0.040(3) 0.120(10) 0.050(3) -0.020(8) 0.001(2) 0.031(8) C1A 0.0317(14) 0.0344(14) 0.0312(14) 0.0085(11) 0.0140(11) 0.0009(11) C2A 0.0509(19) 0.0511(19) 0.0360(16) 0.0048(14) 0.0093(14) -0.0157(15) C3A 0.056(2) 0.050(2) 0.064(2) 0.0080(17) 0.0167(18) -0.0205(17) C4A 0.053(2) 0.053(2) 0.063(2) 0.0214(18) 0.0297(18) -0.0016(16) C5A 0.091(3) 0.065(2) 0.0405(19) 0.0087(18) 0.037(2) -0.007(2) C6A 0.076(2) 0.0466(18) 0.0361(17) -0.0017(14) 0.0234(17) -0.0091(17) C1B 0.034(2) 0.0258(18) 0.0294(19) 0.000 -0.0012(15) 0.000 C2B 0.058(3) 0.060(3) 0.029(2) 0.000 0.001(2) 0.000 C3B 0.075(4) 0.075(4) 0.044(3) 0.000 -0.019(3) 0.000 C4B 0.057(4) 0.051(3) 0.075(4) 0.000 -0.031(3) 0.000 C5B 0.033(3) 0.045(3) 0.107(5) 0.000 0.003(3) 0.000 C6B 0.035(2) 0.035(2) 0.065(3) 0.000 0.011(2) 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 O4 2.0809(18) 6_565 ? Sn1 O4 2.0809(18) . ? Sn1 O3 2.090(2) . ? Sn1 C5 2.129(5) . ? Sn1 C5 2.129(5) 6_565 ? Sn1 O1 2.1522(18) 6_565 ? Sn1 O1 2.1522(18) . ? Sn2 O3 2.0534(14) . ? Sn2 O6 2.0641(17) . ? Sn2 O5 2.0710(17) . ? Sn2 C1 2.116(3) . ? Sn2 O2 2.1632(15) . ? Sn2 O1 2.2013(17) . ? P1 O6 1.5146(18) 5_666 ? P1 O5 1.5189(19) 6_565 ? P1 O4 1.5248(19) . ? O1 C1A 1.380(3) . ? O2 C1B 1.384(4) . ? O2 Sn2 2.1632(15) 6_565 ? O3 Sn2 2.0534(14) 6_565 ? O5 P1 1.5189(19) 6_565 ? O6 P1 1.5146(18) 5_666 ? C1 C2 1.512(4) . ? C2 C3 1.517(4) . ? C3 C4 1.493(5) . ? C5 C6 1.526(13) . ? C6 C7 1.593(12) . ? C7 C8 1.508(14) . ? C1A C2A 1.368(4) . ? C1A C6A 1.372(4) . ? C2A C3A 1.388(4) . ? C3A C4A 1.370(5) . ? C4A C5A 1.351(5) . ? C5A C6A 1.403(4) . ? C1B C6B 1.371(6) . ? C1B C2B 1.376(6) . ? C2B C3B 1.369(7) . ? C3B C4B 1.336(9) . ? C4B C5B 1.380(8) . ? C5B C6B 1.406(7) . ? 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 O4 90.63(10) 6_565 . ? O4 Sn1 O3 87.60(7) 6_565 . ? O4 Sn1 O3 87.60(7) . . ? O4 Sn1 C5 98.1(6) 6_565 . ? O4 Sn1 C5 100.6(5) . . ? O3 Sn1 C5 169.91(18) . . ? O4 Sn1 C5 100.6(5) 6_565 6_565 ? O4 Sn1 C5 98.1(6) . 6_565 ? O3 Sn1 C5 169.91(18) . 6_565 ? C5 Sn1 C5 3.4(15) . 6_565 ? O4 Sn1 O1 161.38(7) 6_565 6_565 ? O4 Sn1 O1 89.24(7) . 6_565 ? O3 Sn1 O1 73.78(6) . 6_565 ? C5 Sn1 O1 100.2(5) . 6_565 ? C5 Sn1 O1 97.9(5) 6_565 6_565 ? O4 Sn1 O1 89.24(7) 6_565 . ? O4 Sn1 O1 161.38(7) . . ? O3 Sn1 O1 73.78(6) . . ? C5 Sn1 O1 97.9(5) . . ? C5 Sn1 O1 100.2(5) 6_565 . ? O1 Sn1 O1 85.03(10) 6_565 . ? O3 Sn2 O6 95.22(8) . . ? O3 Sn2 O5 88.19(7) . . ? O6 Sn2 O5 88.40(7) . . ? O3 Sn2 C1 163.58(9) . . ? O6 Sn2 C1 97.97(9) . . ? O5 Sn2 C1 101.87(9) . . ? O3 Sn2 O2 73.54(8) . . ? O6 Sn2 O2 88.51(8) . . ? O5 Sn2 O2 161.10(7) . . ? C1 Sn2 O2 97.02(9) . . ? O3 Sn2 O1 73.45(8) . . ? O6 Sn2 O1 167.31(7) . . ? O5 Sn2 O1 85.57(7) . . ? C1 Sn2 O1 94.20(9) . . ? O2 Sn2 O1 93.59(8) . . ? O6 P1 O5 114.40(10) 5_666 6_565 ? O6 P1 O4 111.07(11) 5_666 . ? O5 P1 O4 112.28(10) 6_565 . ? C1A O1 Sn1 127.29(16) . . ? C1A O1 Sn2 126.91(15) . . ? Sn1 O1 Sn2 100.98(7) . . ? C1B O2 Sn2 126.22(8) . . ? C1B O2 Sn2 126.22(8) . 6_565 ? Sn2 O2 Sn2 102.31(10) . 6_565 ? Sn2 O3 Sn2 110.27(11) 6_565 . ? Sn2 O3 Sn1 108.32(7) 6_565 . ? Sn2 O3 Sn1 108.32(7) . . ? P1 O4 Sn1 127.91(11) . . ? P1 O5 Sn2 128.94(10) 6_565 . ? P1 O6 Sn2 141.95(11) 5_666 . ? C2 C1 Sn2 114.5(2) . . ? C1 C2 C3 113.1(3) . . ? C4 C3 C2 112.5(3) . . ? C6 C5 Sn1 114.0(7) . . ? C5 C6 C7 109.3(10) . . ? C8 C7 C6 101.1(12) . . ? C2A C1A C6A 120.2(3) . . ? C2A C1A O1 121.0(2) . . ? C6A C1A O1 118.8(3) . . ? C1A C2A C3A 119.8(3) . . ? C4A C3A C2A 120.4(3) . . ? C5A C4A C3A 119.8(3) . . ? C4A C5A C6A 120.6(3) . . ? C1A C6A C5A 119.2(3) . . ? C6B C1B C2B 119.6(4) . . ? C6B C1B O2 120.7(4) . . ? C2B C1B O2 119.6(4) . . ? C3B C2B C1B 121.4(5) . . ? C4B C3B C2B 119.4(5) . . ? C3B C4B C5B 121.3(5) . . ? C4B C5B C6B 119.5(5) . . ? C1B C6B C5B 118.7(5) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.125 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.111