#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1004002.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_final _audit_creation_method SHELXL-97 _chemical_name_systematic ; octakis(mu!3$-sulfido)-hexakis(triphenylphophine) -hexa-tungsten-(benzene)solvate ; _chemical_name_common 'Tungsten sulfide cluster with' _chemical_melting_point 'not measured' _chemical_formula_moiety W6S8(PC18H15)6(C6H6) _chemical_formula_sum 'C114 H96 P6 S8 W6' _chemical_formula_weight 3011.31 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _publ_author_name Jin, Song., Zhou, Ran., Scheuer, Ellen. M., Adamchuk, Jennifer., Rayburn, Lori. L., DiSalvo, Francis. J. ; _journal_name_full ; Inorganic Chemistry ; _journal_volume 40 _journal_year 2001 _journal_page_first 2666 _journal_page_last 2674 ; _cell_length_a 14.6107(6) _cell_length_b 16.6282(7) _cell_length_c 21.2344(9) _cell_angle_alpha 96.3869(9) _cell_angle_beta 93.7166(10) _cell_angle_gamma 92.1225(10) _cell_volume 5111.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'NOT MEASURED' _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2884 _exptl_absorpt_coefficient_mu 7.031 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.246069 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; Absorption correction was done with SADABS beta Version. This program only gives ratios of max and min absorptions. ; _diffrn_ambient_temperature 446(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_% 0 _diffrn_reflns_number 39842 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.10 _reflns_number_total 21993 _reflns_number_gt 14342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'Bruker SAINT Plus' _computing_data_reduction SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0369P)^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 21993 _refine_ls_number_parameters 1122 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.965 _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 W1 W 1.207180(19) 0.134264(16) 0.235630(12) 0.01473(7) Uani 1 1 d . . . W2 W 1.137859(19) 0.278979(17) 0.222396(13) 0.01587(7) Uani 1 1 d . . . W3 W 1.297096(19) 0.241117(17) 0.173198(13) 0.01492(7) Uani 1 1 d . . . W4 W 1.364660(19) 0.208695(17) 0.287555(12) 0.01513(7) Uani 1 1 d . . . W5 W 1.205463(19) 0.247094(17) 0.336632(13) 0.01579(7) Uani 1 1 d . . . W6 W 1.29539(2) 0.353617(17) 0.274001(13) 0.01641(7) Uani 1 1 d . . . S7 S 1.06549(12) 0.17784(11) 0.28183(8) 0.0207(4) Uani 1 1 d . . . S8 S 1.35314(13) 0.31549(11) 0.37662(8) 0.0207(4) Uani 1 1 d . . . S9 S 1.15005(12) 0.17230(11) 0.13304(8) 0.0186(4) Uani 1 1 d . . . S10 S 1.43692(12) 0.30998(11) 0.22855(8) 0.0214(4) Uani 1 1 d . . . S11 S 1.14517(13) 0.37850(11) 0.31649(9) 0.0223(4) Uani 1 1 d . . . S12 S 1.35807(12) 0.11076(10) 0.19325(8) 0.0184(4) Uani 1 1 d . . . S13 S 1.27221(13) 0.11612(11) 0.34220(8) 0.0211(4) Uani 1 1 d . . . S14 S 1.22983(13) 0.37169(11) 0.16821(8) 0.0211(4) Uani 1 1 d . . . P1 P 1.13748(13) -0.01192(11) 0.20759(9) 0.0199(4) Uani 1 1 d . . . P2 P 0.99369(13) 0.34899(12) 0.18684(9) 0.0218(4) Uani 1 1 d . . . P3 P 1.34553(13) 0.25070(11) 0.06013(8) 0.0193(4) Uani 1 1 d . . . P4 P 1.50839(13) 0.13593(11) 0.32052(8) 0.0191(4) Uani 1 1 d . . . P5 P 1.15342(13) 0.23956(12) 0.44904(8) 0.0206(4) Uani 1 1 d . A . P6 P 1.36043(14) 0.50109(11) 0.29664(9) 0.0218(4) Uani 1 1 d . . . C101 C 1.0385(5) -0.0229(4) 0.1492(3) 0.0242(17) Uani 1 1 d . . . C102 C 0.9613(6) 0.0202(5) 0.1607(4) 0.045(2) Uani 1 1 d . . . H10A H 0.9614 0.0579 0.1965 0.054 Uiso 1 1 calc R . . C103 C 0.8851(7) 0.0079(6) 0.1200(5) 0.056(3) Uani 1 1 d . . . H10B H 0.8320 0.0339 0.1304 0.068 Uiso 1 1 calc R . . C104 C 0.8844(7) -0.0418(6) 0.0641(5) 0.052(3) Uani 1 1 d . . . H10C H 0.8321 -0.0492 0.0363 0.062 Uiso 1 1 calc R . . C105 C 0.9601(7) -0.0789(7) 0.0508(5) 0.066(3) Uani 1 1 d . . . H10D H 0.9617 -0.1107 0.0120 0.079 Uiso 1 1 calc R . . C106 C 1.0375(6) -0.0719(6) 0.0930(4) 0.049(3) Uani 1 1 d . . . H10E H 1.0890 -0.1007 0.0829 0.058 Uiso 1 1 calc R . . C107 C 1.0948(6) -0.0628(5) 0.2738(4) 0.0289(19) Uani 1 1 d . . . C108 C 1.1513(6) -0.0620(5) 0.3282(4) 0.034(2) Uani 1 1 d . . . H10F H 1.2091 -0.0360 0.3307 0.040 Uiso 1 1 calc R . . C109 C 1.1232(7) -0.0995(5) 0.3792(4) 0.045(3) Uani 1 1 d . . . H10G H 1.1621 -0.0977 0.4159 0.054 Uiso 1 1 calc R . . C110 C 1.0394(7) -0.1389(6) 0.3764(5) 0.052(3) Uani 1 1 d . . . H11A H 1.0207 -0.1637 0.4108 0.062 Uiso 1 1 calc R . . C111 C 0.9835(7) -0.1413(6) 0.3226(5) 0.057(3) Uani 1 1 d . . . H11B H 0.9266 -0.1689 0.3202 0.068 Uiso 1 1 calc R . . C112 C 1.0097(6) -0.1033(5) 0.2710(4) 0.045(2) Uani 1 1 d . . . H11C H 0.9702 -0.1052 0.2346 0.054 Uiso 1 1 calc R . . C113 C 1.2154(5) -0.0867(4) 0.1741(3) 0.0219(16) Uani 1 1 d . . . C114 C 1.2191(6) -0.1642(5) 0.1919(4) 0.036(2) Uani 1 1 d . . . H11D H 1.1794 -0.1804 0.2210 0.043 Uiso 1 1 calc R . . C115 C 1.2810(7) -0.2181(5) 0.1671(4) 0.045(3) Uani 1 1 d . . . H11E H 1.2822 -0.2701 0.1793 0.054 Uiso 1 1 calc R . . C116 C 1.3405(6) -0.1948(5) 0.1245(4) 0.039(2) Uani 1 1 d . . . H11F H 1.3834 -0.2303 0.1087 0.047 Uiso 1 1 calc R . . C117 C 1.3366(6) -0.1191(5) 0.1054(4) 0.040(2) Uani 1 1 d . . . H11G H 1.3766 -0.1033 0.0763 0.048 Uiso 1 1 calc R . . C118 C 1.2732(6) -0.0661(5) 0.1294(4) 0.0309(19) Uani 1 1 d . . . H11H H 1.2697 -0.0154 0.1149 0.037 Uiso 1 1 calc R . . C201 C 0.8944(5) 0.3513(4) 0.2365(3) 0.0251(17) Uani 1 1 d D . . C202 C 0.8110(5) 0.3766(5) 0.2119(4) 0.038(2) Uani 1 1 d D . . H20A H 0.8062 0.3933 0.1715 0.045 Uiso 1 1 calc R . . C203 C 0.7345(6) 0.3767(6) 0.2481(4) 0.047(3) Uani 1 1 d D . . H20B H 0.6791 0.3948 0.2323 0.056 Uiso 1 1 calc R . . C204 C 0.7413(6) 0.3502(5) 0.3069(4) 0.039(2) Uani 1 1 d D . . H20C H 0.6895 0.3472 0.3299 0.047 Uiso 1 1 calc R . . C205 C 0.8246(6) 0.3280(5) 0.3322(4) 0.040(2) Uani 1 1 d D . . H20D H 0.8296 0.3130 0.3731 0.048 Uiso 1 1 calc R . . C206 C 0.9015(5) 0.3282(5) 0.2963(3) 0.0293(18) Uani 1 1 d D . . H20E H 0.9576 0.3125 0.3131 0.035 Uiso 1 1 calc R . . C207 C 1.0173(6) 0.4566(5) 0.1817(4) 0.042(2) Uani 1 1 d D . . C208 C 1.0621(6) 0.4799(6) 0.1292(5) 0.060(3) Uani 1 1 d D . . H20F H 1.0775 0.4415 0.0968 0.072 Uiso 1 1 calc R . . C209 C 1.0824(7) 0.5612(7) 0.1274(7) 0.099(6) Uani 1 1 d D . . H20G H 1.1090 0.5768 0.0918 0.119 Uiso 1 1 calc R . . C210 C 1.0658(8) 0.6194(7) 0.1742(8) 0.112(7) Uani 1 1 d D . . H21A H 1.0832 0.6734 0.1721 0.134 Uiso 1 1 calc R . . C211 C 1.0224(8) 0.5963(6) 0.2251(7) 0.093(5) Uani 1 1 d D . . H21B H 1.0069 0.6352 0.2572 0.112 Uiso 1 1 calc R . . C212 C 1.0016(7) 0.5150(5) 0.2287(5) 0.052(3) Uani 1 1 d D . . H21C H 0.9760 0.5001 0.2649 0.062 Uiso 1 1 calc R . . C213 C 0.9385(5) 0.3094(5) 0.1088(3) 0.0279(18) Uani 1 1 d . . . C214 C 0.9303(5) 0.2248(6) 0.0949(4) 0.034(2) Uani 1 1 d . . . H21D H 0.9559 0.1922 0.1236 0.041 Uiso 1 1 calc R . . C215 C 0.8852(6) 0.1897(7) 0.0397(4) 0.050(3) Uani 1 1 d . . . H21E H 0.8795 0.1336 0.0316 0.060 Uiso 1 1 calc R . . C216 C 0.8487(7) 0.2359(8) -0.0034(4) 0.062(3) Uani 1 1 d . . . H21F H 0.8189 0.2112 -0.0410 0.075 Uiso 1 1 calc R . . C217 C 0.8554(6) 0.3177(8) 0.0079(5) 0.058(3) Uani 1 1 d . . . H21G H 0.8298 0.3488 -0.0219 0.070 Uiso 1 1 calc R . . C218 C 0.9014(5) 0.3566(6) 0.0652(4) 0.042(2) Uani 1 1 d . . . H21H H 0.9062 0.4128 0.0730 0.051 Uiso 1 1 calc R . . C301 C 1.2699(5) 0.3139(4) 0.0162(3) 0.0246(17) Uani 1 1 d . . . C302 C 1.2989(7) 0.3843(5) -0.0057(5) 0.057(3) Uani 1 1 d . . . H30A H 1.3603 0.4019 0.0001 0.069 Uiso 1 1 calc R . . C303 C 1.2337(8) 0.4299(6) -0.0373(6) 0.080(4) Uani 1 1 d . . . H30B H 1.2527 0.4778 -0.0524 0.096 Uiso 1 1 calc R . . C304 C 1.1445(7) 0.4043(6) -0.0457(5) 0.065(3) Uani 1 1 d . . . H30C H 1.1020 0.4355 -0.0653 0.078 Uiso 1 1 calc R . . C305 C 1.1170(6) 0.3339(6) -0.0258(4) 0.048(3) Uani 1 1 d . . . H30D H 1.0560 0.3155 -0.0336 0.057 Uiso 1 1 calc R . . C306 C 1.1780(6) 0.2885(5) 0.0060(4) 0.037(2) Uani 1 1 d . . . H30E H 1.1575 0.2408 0.0206 0.044 Uiso 1 1 calc R . . C307 C 1.3503(5) 0.1605(5) 0.0034(3) 0.0243(17) Uani 1 1 d . . . C308 C 1.3717(7) 0.0868(5) 0.0234(4) 0.049(3) Uani 1 1 d . . . H30F H 1.3795 0.0811 0.0665 0.059 Uiso 1 1 calc R . . C309 C 1.3813(9) 0.0219(6) -0.0218(5) 0.071(4) Uani 1 1 d . . . H30G H 1.3944 -0.0277 -0.0078 0.085 Uiso 1 1 calc R . . C310 C 1.3729(7) 0.0258(6) -0.0849(4) 0.050(3) Uani 1 1 d . . . H31A H 1.3807 -0.0197 -0.1134 0.060 Uiso 1 1 calc R . . C311 C 1.3526(7) 0.0988(6) -0.1063(4) 0.046(2) Uani 1 1 d . . . H31B H 1.3477 0.1036 -0.1496 0.055 Uiso 1 1 calc R . . C312 C 1.3396(6) 0.1646(5) -0.0626(4) 0.036(2) Uani 1 1 d . . . H31C H 1.3234 0.2132 -0.0772 0.044 Uiso 1 1 calc R . . C313 C 1.4599(5) 0.2978(5) 0.0589(3) 0.0238(17) Uani 1 1 d . . . C314 C 1.4818(5) 0.3729(5) 0.0905(4) 0.0308(19) Uani 1 1 d . . . H31D H 1.4361 0.4013 0.1105 0.037 Uiso 1 1 calc R . . C315 C 1.5692(6) 0.4079(5) 0.0938(4) 0.036(2) Uani 1 1 d . . . H31E H 1.5814 0.4600 0.1143 0.044 Uiso 1 1 calc R . . C316 C 1.6384(6) 0.3652(6) 0.0664(4) 0.041(2) Uani 1 1 d . . . H31F H 1.6978 0.3881 0.0690 0.049 Uiso 1 1 calc R . . C317 C 1.6195(6) 0.2891(5) 0.0353(4) 0.037(2) Uani 1 1 d . . . H31G H 1.6663 0.2602 0.0170 0.045 Uiso 1 1 calc R . . C318 C 1.5312(5) 0.2548(5) 0.0308(4) 0.0288(18) Uani 1 1 d . . . H31H H 1.5188 0.2034 0.0093 0.035 Uiso 1 1 calc R . . C401 C 1.6116(5) 0.1458(4) 0.2764(3) 0.0224(16) Uani 1 1 d . . . C402 C 1.6046(6) 0.1713(4) 0.2163(3) 0.0282(18) Uani 1 1 d . . . H40A H 1.5477 0.1839 0.1986 0.034 Uiso 1 1 calc R . . C403 C 1.6828(6) 0.1782(5) 0.1823(4) 0.037(2) Uani 1 1 d . . . H40B H 1.6782 0.1936 0.1414 0.044 Uiso 1 1 calc R . . C404 C 1.7670(6) 0.1617(5) 0.2104(4) 0.040(2) Uani 1 1 d . . . H40C H 1.8196 0.1688 0.1887 0.048 Uiso 1 1 calc R . . C405 C 1.7753(6) 0.1349(5) 0.2696(4) 0.039(2) Uani 1 1 d . . . H40D H 1.8321 0.1222 0.2873 0.046 Uiso 1 1 calc R . . C406 C 1.6960(6) 0.1274(5) 0.3024(4) 0.035(2) Uani 1 1 d . . . H40E H 1.7004 0.1097 0.3425 0.041 Uiso 1 1 calc R . . C407 C 1.4880(5) 0.0246(5) 0.3114(3) 0.0247(17) Uani 1 1 d . . . C408 C 1.4361(5) -0.0139(5) 0.3518(4) 0.0322(19) Uani 1 1 d . . . H40F H 1.4139 0.0160 0.3868 0.039 Uiso 1 1 calc R . . C409 C 1.4166(6) -0.0967(5) 0.3411(4) 0.035(2) Uani 1 1 d . . . H40G H 1.3814 -0.1214 0.3691 0.042 Uiso 1 1 calc R . . C410 C 1.4480(6) -0.1429(6) 0.2899(4) 0.044(2) Uani 1 1 d . . . H41A H 1.4346 -0.1984 0.2828 0.053 Uiso 1 1 calc R . . C411 C 1.5002(7) -0.1042(5) 0.2493(4) 0.044(2) Uani 1 1 d . . . H41B H 1.5224 -0.1345 0.2145 0.053 Uiso 1 1 calc R . . C412 C 1.5199(6) -0.0231(5) 0.2588(4) 0.0309(19) Uani 1 1 d . . . H41C H 1.5548 0.0012 0.2304 0.037 Uiso 1 1 calc R . . C413 C 1.5565(5) 0.1604(5) 0.4018(3) 0.0245(17) Uani 1 1 d . . . C414 C 1.5902(6) 0.1029(6) 0.4399(3) 0.036(2) Uani 1 1 d . . . H41D H 1.5825 0.0481 0.4251 0.043 Uiso 1 1 calc R . . C415 C 1.6348(6) 0.1262(6) 0.4991(4) 0.040(2) Uani 1 1 d . . . H41E H 1.6546 0.0874 0.5246 0.048 Uiso 1 1 calc R . . C416 C 1.6496(6) 0.2072(6) 0.5197(4) 0.039(2) Uani 1 1 d . . . H41F H 1.6805 0.2232 0.5590 0.046 Uiso 1 1 calc R . . C417 C 1.6188(6) 0.2650(6) 0.4824(4) 0.041(2) Uani 1 1 d . . . H41G H 1.6304 0.3198 0.4961 0.049 Uiso 1 1 calc R . . C418 C 1.5706(5) 0.2414(5) 0.4246(4) 0.0314(19) Uani 1 1 d . . . H41H H 1.5474 0.2805 0.4006 0.038 Uiso 1 1 calc R . . C501 C 1.2261(5) 0.1829(5) 0.4999(3) 0.0269(18) Uani 1 1 d . . . C502 C 1.3212(5) 0.1903(5) 0.4994(4) 0.0311(19) Uani 1 1 d . . . H50A H 1.3469 0.2203 0.4700 0.037 Uiso 1 1 calc R . . C503 C 1.3794(6) 0.1539(6) 0.5417(4) 0.042(2) Uani 1 1 d . . . H50B H 1.4428 0.1596 0.5405 0.050 Uiso 1 1 calc R . . C504 C 1.3414(6) 0.1097(5) 0.5848(4) 0.041(2) Uani 1 1 d . . . H50C H 1.3795 0.0860 0.6136 0.049 Uiso 1 1 calc R . . C505 C 1.2480(7) 0.0999(5) 0.5863(5) 0.048(3) Uani 1 1 d . . . H50D H 1.2232 0.0697 0.6159 0.057 Uiso 1 1 calc R . . C506 C 1.1907(5) 0.1349(5) 0.5436(4) 0.034(2) Uani 1 1 d . . . H50E H 1.1275 0.1263 0.5439 0.041 Uiso 1 1 calc R . . C507 C 1.0412(5) 0.1872(5) 0.4475(3) 0.0223(17) Uani 1 1 d . . . C508 C 0.9628(5) 0.2267(5) 0.4624(4) 0.0316(19) Uani 1 1 d . . . H50F H 0.9673 0.2820 0.4756 0.038 Uiso 1 1 calc R . . C509 C 0.8765(6) 0.1859(6) 0.4581(4) 0.046(2) Uani 1 1 d . . . H50G H 0.8241 0.2136 0.4678 0.055 Uiso 1 1 calc R . . C510 C 0.8715(6) 0.1039(5) 0.4392(4) 0.035(2) Uani 1 1 d . . . H51A H 0.8153 0.0753 0.4376 0.042 Uiso 1 1 calc R . . C511 C 0.9471(6) 0.0644(5) 0.4228(4) 0.043(2) Uani 1 1 d . . . H51B H 0.9416 0.0093 0.4086 0.051 Uiso 1 1 calc R . . C512 C 1.0348(3) 0.1048(3) 0.4268(2) 0.035(2) Uani 1 1 d . . . H51C H 1.0866 0.0770 0.4159 0.042 Uiso 1 1 calc R . . C601 C 1.4573(3) 0.5201(3) 0.3557(2) 0.0272(18) Uani 1 1 d R . . C602 C 1.5192(3) 0.4625(3) 0.3644(2) 0.038(2) Uani 1 1 d R . . H60A H 1.5131 0.4131 0.3388 0.045 Uiso 1 1 calc R . . C603 C 1.5918(6) 0.4762(6) 0.4109(4) 0.050(3) Uani 1 1 d . . . H60B H 1.6333 0.4358 0.4157 0.061 Uiso 1 1 calc R . . C604 C 1.6031(7) 0.5471(7) 0.4491(5) 0.058(3) Uani 1 1 d . . . H60C H 1.6503 0.5548 0.4811 0.070 Uiso 1 1 calc R . . C605 C 1.5435(8) 0.6075(7) 0.4399(5) 0.073(4) Uani 1 1 d . . . H60D H 1.5515 0.6575 0.4645 0.088 Uiso 1 1 calc R . . C606 C 1.4715(7) 0.5937(6) 0.3937(5) 0.052(3) Uani 1 1 d . . . H60E H 1.4314 0.6349 0.3880 0.062 Uiso 1 1 calc R . . C607 C 1.3989(6) 0.5462(4) 0.2274(4) 0.0282(18) Uani 1 1 d . . . C608 C 1.3376(6) 0.5505(4) 0.1745(4) 0.0288(18) Uani 1 1 d . . . H60F H 1.2767 0.5325 0.1755 0.035 Uiso 1 1 calc R . . C609 C 1.3664(7) 0.5813(5) 0.1211(4) 0.039(2) Uani 1 1 d . . . H60G H 1.3253 0.5829 0.0859 0.047 Uiso 1 1 calc R . . C610 C 1.4572(7) 0.6100(5) 0.1197(4) 0.047(3) Uani 1 1 d . . . H61A H 1.4768 0.6306 0.0836 0.056 Uiso 1 1 calc R . . C611 C 1.5156(7) 0.6076(6) 0.1701(5) 0.054(3) Uani 1 1 d . . . H61B H 1.5758 0.6274 0.1690 0.065 Uiso 1 1 calc R . . C612 C 1.4890(6) 0.5762(5) 0.2245(4) 0.040(2) Uani 1 1 d . . . H61C H 1.5312 0.5752 0.2591 0.048 Uiso 1 1 calc R . . C613 C 1.2795(5) 0.5750(4) 0.3294(3) 0.0260(18) Uani 1 1 d . . . C614 C 1.2372(6) 0.5553(5) 0.3825(4) 0.039(2) Uani 1 1 d . . . H61D H 1.2501 0.5077 0.3998 0.046 Uiso 1 1 calc R . . C615 C 1.1744(7) 0.6086(6) 0.4097(5) 0.057(3) Uani 1 1 d . . . H61E H 1.1442 0.5950 0.4446 0.069 Uiso 1 1 calc R . . C616 C 1.1569(7) 0.6797(6) 0.3859(5) 0.053(3) Uani 1 1 d . . . H61F H 1.1165 0.7155 0.4048 0.063 Uiso 1 1 calc R . . C617 C 1.2006(7) 0.6973(6) 0.3334(4) 0.051(3) Uani 1 1 d . . . H61G H 1.1886 0.7456 0.3168 0.061 Uiso 1 1 calc R . . C618 C 1.2631(4) 0.6450(4) 0.3037(2) 0.039(2) Uani 1 1 d . . . H61H H 1.2918 0.6579 0.2681 0.047 Uiso 1 1 calc R . . C1S C 1.3085(4) 0.2828(4) 0.7029(2) 0.116(5) Uiso 1 1 d R . . H1SA H 1.3447 0.2731 0.6686 0.139 Uiso 1 1 calc R . . C2S C 1.2827(4) 0.2195(4) 0.7365(2) 0.118(5) Uiso 1 1 d R . . H2SA H 1.3015 0.1675 0.7247 0.142 Uiso 1 1 calc R . . C3S C 1.2287(4) 0.2340(4) 0.7878(2) 0.131(6) Uiso 1 1 d R . . H3SA H 1.2114 0.1917 0.8103 0.157 Uiso 1 1 calc R . . C4S C 1.2006(4) 0.3118(4) 0.8054(2) 0.135(6) Uiso 1 1 d R . . H4SA H 1.1645 0.3215 0.8397 0.162 Uiso 1 1 calc R . . C5S C 1.2264(4) 0.3750(4) 0.7717(2) 0.144(7) Uiso 1 1 d R . . H5SA H 1.2076 0.4271 0.7835 0.172 Uiso 1 1 calc R . . C6S C 1.2804(4) 0.3605(4) 0.7205(2) 0.121(6) Uiso 1 1 d R . . H6SA H 1.2977 0.4029 0.6980 0.146 Uiso 1 1 calc R . . C513 C 1.1372(5) 0.3324(5) 0.5028(3) 0.0295(18) Uiso 1 1 d D . . C514 C 1.1361(5) 0.3279(4) 0.5648(3) 0.070(4) Uiso 0.746(11) 1 d PD A 1 H51D H 1.1428 0.2781 0.5803 0.084 Uiso 0.746(11) 1 calc PR A 1 C515 C 1.1249(5) 0.3965(4) 0.6068(3) 0.087(6) Uiso 0.746(11) 1 d PRD A 1 H51E H 1.1290 0.3934 0.6504 0.104 Uiso 0.746(11) 1 calc PR A 1 C524 C 1.0942(5) 0.3140(4) 0.5618(3) 0.032(8) Uiso 0.254(11) 1 d PRD A 2 H52A H 1.0732 0.2635 0.5711 0.039 Uiso 0.254(11) 1 calc PR A 2 C525 C 1.0914(5) 0.3943(4) 0.6034(3) 0.021(7) Uiso 0.254(11) 1 d PRD A 2 H52C H 1.0776 0.3925 0.6453 0.025 Uiso 0.254(11) 1 calc PR A 2 C516 C 1.1076(5) 0.4699(4) 0.5837(3) 0.100(5) Uiso 1 1 d RD . . H51F H 1.1002 0.5159 0.6118 0.120 Uiso 1 1 calc R A 1 C517 C 1.1015(5) 0.4746(4) 0.5187(3) 0.208(14) Uiso 0.746(11) 1 d PRD A 1 H51G H 1.0900 0.5237 0.5032 0.250 Uiso 0.746(11) 1 calc PR A 1 C518 C 1.1127(5) 0.4059(4) 0.4767(3) 0.108(7) Uiso 0.746(11) 1 d PRD A 1 H51H H 1.1046 0.4072 0.4330 0.130 Uiso 0.746(11) 1 calc PR A 1 C527 C 1.1692(14) 0.4731(11) 0.5364(8) 0.010(5) Uiso 0.254(11) 1 d PD A 2 H52D H 1.2051 0.5197 0.5335 0.012 Uiso 0.254(11) 1 calc PR A 2 C528 C 1.1748(13) 0.4030(8) 0.4932(8) 0.001(5) Uiso 0.254(11) 1 d PD A 2 H52E H 1.2059 0.4067 0.4567 0.001 Uiso 0.254(11) 1 calc PR A 2 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 0.01276(16) 0.01434(14) 0.01629(13) -0.00278(12) 0.00187(11) 0.00220(11) W2 0.01109(16) 0.01577(14) 0.02002(14) -0.00184(12) 0.00081(11) 0.00305(11) W3 0.01142(16) 0.01525(14) 0.01750(13) -0.00195(12) 0.00209(11) 0.00243(11) W4 0.01068(16) 0.01748(15) 0.01641(13) -0.00297(12) 0.00176(11) 0.00308(11) W5 0.01122(16) 0.01789(15) 0.01733(13) -0.00376(12) 0.00264(11) 0.00267(11) W6 0.01257(16) 0.01500(14) 0.02049(14) -0.00378(12) 0.00133(11) 0.00204(11) S7 0.0129(10) 0.0235(10) 0.0250(9) -0.0002(8) 0.0025(7) -0.0013(7) S8 0.0163(10) 0.0246(10) 0.0190(8) -0.0049(8) -0.0023(7) -0.0016(8) S9 0.0157(10) 0.0194(9) 0.0194(8) -0.0019(8) -0.0024(7) 0.0001(7) S10 0.0134(10) 0.0244(10) 0.0253(9) -0.0030(8) 0.0044(7) -0.0001(7) S11 0.0169(11) 0.0197(9) 0.0292(9) -0.0037(8) 0.0017(8) 0.0070(7) S12 0.0179(10) 0.0181(9) 0.0184(8) -0.0038(8) 0.0027(7) 0.0060(7) S13 0.0210(11) 0.0228(10) 0.0194(8) 0.0022(8) 0.0021(7) 0.0010(8) S14 0.0214(11) 0.0169(9) 0.0250(9) 0.0017(8) 0.0019(7) 0.0025(7) P1 0.0199(11) 0.0168(9) 0.0226(9) -0.0022(8) 0.0061(8) -0.0004(8) P2 0.0151(11) 0.0233(10) 0.0280(10) 0.0045(9) 0.0025(8) 0.0054(8) P3 0.0166(11) 0.0209(10) 0.0202(9) -0.0013(8) 0.0053(7) 0.0034(8) P4 0.0138(11) 0.0251(10) 0.0178(9) -0.0012(8) 0.0013(7) 0.0031(8) P5 0.0147(11) 0.0264(10) 0.0198(9) -0.0039(9) 0.0041(7) 0.0016(8) P6 0.0208(11) 0.0157(9) 0.0281(10) -0.0042(9) 0.0051(8) 0.0017(8) C101 0.022(5) 0.019(4) 0.030(4) -0.004(3) 0.005(3) -0.001(3) C102 0.030(6) 0.041(5) 0.057(6) -0.026(5) -0.007(4) 0.011(4) C103 0.028(6) 0.049(6) 0.082(7) -0.029(6) -0.013(5) 0.014(5) C104 0.028(6) 0.067(7) 0.056(6) -0.013(6) -0.007(5) 0.007(5) C105 0.044(8) 0.092(9) 0.050(6) -0.040(6) -0.007(5) 0.008(6) C106 0.023(5) 0.072(7) 0.044(5) -0.030(5) 0.006(4) 0.015(5) C107 0.033(5) 0.022(4) 0.032(4) -0.003(4) 0.015(4) 0.007(3) C108 0.047(6) 0.023(4) 0.030(4) 0.001(4) 0.007(4) 0.006(4) C109 0.072(8) 0.030(5) 0.036(5) 0.008(4) 0.013(5) 0.013(5) C110 0.052(7) 0.058(7) 0.056(6) 0.027(6) 0.034(5) 0.031(5) C111 0.036(6) 0.065(7) 0.076(7) 0.028(6) 0.020(5) -0.001(5) C112 0.026(5) 0.055(6) 0.058(6) 0.022(5) 0.012(4) -0.001(4) C113 0.020(4) 0.026(4) 0.019(3) -0.003(3) 0.002(3) 0.003(3) C114 0.050(6) 0.029(5) 0.031(4) 0.001(4) 0.015(4) 0.012(4) C115 0.080(8) 0.030(5) 0.027(4) -0.002(4) 0.003(4) 0.029(5) C116 0.036(6) 0.044(5) 0.034(5) -0.017(4) 0.002(4) 0.021(4) C117 0.044(6) 0.032(5) 0.040(5) -0.016(4) 0.016(4) 0.002(4) C118 0.038(5) 0.018(4) 0.036(4) -0.008(4) 0.012(4) -0.004(3) C201 0.017(4) 0.022(4) 0.036(4) -0.002(4) 0.007(3) 0.003(3) C202 0.028(5) 0.055(6) 0.031(4) 0.004(4) 0.009(4) 0.017(4) C203 0.013(5) 0.074(7) 0.055(6) 0.000(6) 0.013(4) 0.014(4) C204 0.025(5) 0.045(5) 0.043(5) -0.016(5) 0.019(4) 0.000(4) C205 0.039(6) 0.042(5) 0.042(5) 0.006(4) 0.020(4) 0.008(4) C206 0.021(5) 0.032(5) 0.035(4) -0.002(4) 0.007(3) 0.009(3) C207 0.016(5) 0.035(5) 0.077(7) 0.022(5) -0.005(4) -0.001(4) C208 0.033(6) 0.064(7) 0.095(8) 0.053(7) 0.005(5) 0.009(5) C209 0.038(7) 0.078(9) 0.194(17) 0.097(12) -0.027(8) -0.015(7) C210 0.037(8) 0.033(7) 0.26(2) 0.050(11) -0.046(10) -0.023(6) C211 0.043(8) 0.041(7) 0.186(16) -0.002(9) -0.036(9) -0.007(6) C212 0.041(6) 0.026(5) 0.086(8) -0.006(5) -0.006(5) 0.005(4) C213 0.016(4) 0.048(5) 0.021(4) 0.005(4) 0.005(3) 0.004(4) C214 0.013(4) 0.058(6) 0.031(4) -0.003(4) 0.004(3) 0.007(4) C215 0.025(5) 0.093(8) 0.027(4) -0.023(5) 0.005(4) 0.015(5) C216 0.030(6) 0.123(11) 0.029(5) -0.021(7) 0.002(4) 0.025(7) C217 0.015(5) 0.124(11) 0.043(6) 0.034(7) 0.003(4) 0.022(6) C218 0.019(5) 0.074(7) 0.040(5) 0.019(5) 0.010(4) 0.020(4) C301 0.026(5) 0.023(4) 0.024(4) -0.005(3) 0.009(3) 0.010(3) C302 0.044(6) 0.038(6) 0.088(8) 0.025(6) -0.032(6) -0.012(5) C303 0.070(9) 0.040(6) 0.128(11) 0.038(7) -0.048(8) -0.006(6) C304 0.055(8) 0.047(6) 0.088(8) 0.007(6) -0.035(6) 0.022(5) C305 0.024(6) 0.080(8) 0.039(5) 0.007(5) -0.001(4) 0.016(5) C306 0.039(6) 0.042(5) 0.032(4) 0.014(4) 0.004(4) 0.003(4) C307 0.016(4) 0.032(4) 0.025(4) -0.004(4) 0.009(3) 0.001(3) C308 0.096(9) 0.019(4) 0.033(5) -0.002(4) 0.015(5) 0.003(5) C309 0.149(12) 0.026(5) 0.041(6) -0.002(5) 0.025(7) 0.022(6) C310 0.073(8) 0.041(6) 0.034(5) -0.022(5) 0.017(5) -0.001(5) C311 0.061(7) 0.055(6) 0.020(4) -0.011(4) 0.006(4) 0.010(5) C312 0.048(6) 0.032(5) 0.026(4) -0.007(4) -0.003(4) 0.008(4) C313 0.025(5) 0.029(4) 0.018(3) 0.004(3) 0.003(3) 0.005(3) C314 0.026(5) 0.030(5) 0.038(4) 0.005(4) 0.005(4) 0.008(4) C315 0.031(5) 0.030(5) 0.047(5) -0.001(4) 0.004(4) -0.005(4) C316 0.019(5) 0.057(6) 0.050(5) 0.015(5) 0.007(4) -0.001(4) C317 0.023(5) 0.047(6) 0.043(5) 0.001(5) 0.015(4) 0.004(4) C318 0.020(5) 0.030(4) 0.034(4) -0.007(4) 0.007(3) -0.002(3) C401 0.021(5) 0.022(4) 0.023(4) -0.004(3) 0.005(3) -0.001(3) C402 0.030(5) 0.027(4) 0.029(4) 0.001(4) 0.009(3) 0.004(3) C403 0.046(6) 0.030(5) 0.036(5) -0.001(4) 0.020(4) 0.007(4) C404 0.033(6) 0.033(5) 0.053(6) -0.013(5) 0.028(4) -0.010(4) C405 0.015(5) 0.050(6) 0.048(5) -0.014(5) 0.013(4) 0.005(4) C406 0.027(5) 0.044(5) 0.035(4) 0.004(4) 0.010(4) 0.006(4) C407 0.018(4) 0.028(4) 0.028(4) 0.010(4) -0.007(3) 0.003(3) C408 0.029(5) 0.034(5) 0.034(4) 0.004(4) 0.002(4) 0.005(4) C409 0.040(6) 0.030(5) 0.035(5) 0.009(4) 0.001(4) -0.003(4) C410 0.041(6) 0.036(5) 0.053(6) 0.003(5) -0.006(4) -0.003(4) C411 0.063(7) 0.031(5) 0.034(5) -0.013(4) 0.006(4) 0.004(4) C412 0.040(5) 0.026(4) 0.027(4) -0.003(4) 0.012(4) 0.005(4) C413 0.011(4) 0.036(4) 0.026(4) -0.004(4) 0.001(3) 0.009(3) C414 0.034(5) 0.051(6) 0.023(4) 0.002(4) 0.004(3) 0.016(4) C415 0.030(5) 0.057(6) 0.033(5) 0.003(5) 0.004(4) 0.005(4) C416 0.020(5) 0.064(6) 0.029(4) -0.006(5) 0.002(3) 0.003(4) C417 0.027(5) 0.048(6) 0.043(5) -0.006(5) 0.004(4) -0.006(4) C418 0.020(5) 0.041(5) 0.032(4) -0.005(4) 0.002(3) 0.011(4) C501 0.022(5) 0.031(4) 0.027(4) -0.004(4) 0.006(3) 0.008(3) C502 0.010(4) 0.049(5) 0.034(4) 0.004(4) 0.003(3) -0.003(4) C503 0.032(6) 0.060(6) 0.032(4) 0.000(5) 0.002(4) 0.009(5) C504 0.042(6) 0.034(5) 0.045(5) -0.004(4) -0.005(4) 0.009(4) C505 0.042(6) 0.041(6) 0.063(6) 0.020(5) -0.002(5) 0.006(4) C506 0.014(4) 0.042(5) 0.045(5) 0.004(4) 0.001(4) 0.001(4) C507 0.014(4) 0.038(5) 0.014(3) -0.001(3) 0.004(3) -0.001(3) C508 0.022(5) 0.036(5) 0.040(5) 0.008(4) 0.013(4) 0.007(4) C509 0.018(5) 0.063(7) 0.057(6) 0.007(6) 0.009(4) 0.007(4) C510 0.017(5) 0.051(6) 0.035(4) 0.003(4) -0.001(3) -0.011(4) C511 0.035(6) 0.027(5) 0.059(6) -0.021(5) 0.006(4) -0.009(4) C512 0.018(5) 0.037(5) 0.047(5) -0.014(4) 0.005(4) -0.005(4) C601 0.027(5) 0.024(4) 0.029(4) -0.002(4) 0.002(3) -0.005(3) C602 0.018(5) 0.038(5) 0.052(5) -0.010(5) -0.001(4) -0.001(4) C603 0.038(6) 0.048(6) 0.059(6) -0.014(5) -0.017(5) 0.009(5) C604 0.042(7) 0.064(7) 0.061(7) -0.021(6) -0.017(5) 0.001(5) C605 0.062(9) 0.056(7) 0.085(8) -0.056(6) -0.025(6) 0.014(6) C606 0.041(6) 0.033(5) 0.071(7) -0.024(5) -0.021(5) 0.007(4) C607 0.029(5) 0.015(4) 0.040(4) -0.004(4) 0.004(4) 0.007(3) C608 0.036(5) 0.017(4) 0.034(4) 0.001(4) 0.005(4) 0.004(3) C609 0.058(7) 0.022(4) 0.038(5) 0.001(4) 0.002(4) 0.011(4) C610 0.055(7) 0.040(5) 0.051(6) 0.013(5) 0.022(5) 0.008(5) C611 0.036(6) 0.066(7) 0.065(7) 0.020(6) 0.020(5) 0.005(5) C612 0.026(5) 0.045(5) 0.051(5) 0.013(5) 0.012(4) 0.002(4) C613 0.022(5) 0.026(4) 0.028(4) -0.009(4) 0.005(3) -0.003(3) C614 0.049(6) 0.017(4) 0.050(5) -0.003(4) 0.023(5) -0.001(4) C615 0.058(8) 0.044(6) 0.065(7) -0.026(6) 0.037(6) -0.018(5) C616 0.036(6) 0.044(6) 0.073(7) -0.022(6) 0.013(5) 0.015(5) C617 0.066(8) 0.042(6) 0.044(5) -0.004(5) -0.003(5) 0.033(5) C618 0.054(6) 0.035(5) 0.031(4) 0.003(4) 0.007(4) 0.017(4) _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.828 _refine_diff_density_min -1.731 _refine_diff_density_rms 0.182