#------------------------------------------------------------------------------ #$Date: 2012-11-18 10:43:14 +0200 (Sun, 18 Nov 2012) $ #$Revision: 68669 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/00/2000044.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_2000044 _publ_contact_author ; Prof. Francis J. DiSalvo Department of Chemistry and Chemical Biology Cornell University Ithaca, NY 14853, USA ; _publ_contact_author_email fjd3@cornell.edu _publ_contact_author_fax '607-255-4137' _publ_contact_author_phone '607-255-7238' loop_ _publ_author_name 'Song Jin' 'Jennifer Adamchuk' 'Bosong Xiang' 'Francis J. DiSalvo' _publ_author_address ; Department of Chemistry and Chemical Biology Cornell University Ithaca, NY 14853 ; _publ_section_title ; The Dean-Evans Relation in 31P NMR Spectroscopy and Its Application to the Chemistry of Octahedral Tungsten Sulfide Clusters ; _journal_name_full 'Journal of the American Chemical Society' _journal_volume 124 _journal_page_first 9229 _journal_page_last 9240 _journal_year 2002 _chemical_formula_sum 'C42 H86 N2 P4 S8 W6' _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cell_volume 6169.267 _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 2.264 _exptl_crystal_description 'wedge' _diffrn_ambient_temperature 173 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_gt 0.0388 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2+x,1/2-y,1/2+z 3 -x,-y,-z 4 -1/2-x,-1/2+y,-1/2-z _cell_length_a 15.8389(12) _cell_length_b 19.4806(14) _cell_length_c 20.0882(15) _cell_angle_alpha 90 _cell_angle_beta 95.542(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 N 0.68 P 1.05 S 1.02 W 1.37 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 0.79378(2) 0.440604(16) -0.130423(17) 0.02834(9) Uani 1 1 d . . . W2 W 0.68653(2) 0.378179(16) -0.220791(17) 0.03014(9) Uani 1 1 d . . . W3 W 0.74921(2) 0.309957(16) -0.111001(18) 0.03018(9) Uani 1 1 d . A . W4 W 0.58603(2) 0.345516(16) -0.126107(18) 0.03112(9) Uani 1 1 d . A . W5 W 0.69452(2) 0.408753(15) -0.034709(17) 0.02722(9) Uani 1 1 d . . . W6 W 0.63056(2) 0.476234(15) -0.142303(17) 0.02738(9) Uani 1 1 d . . . S7 S 0.83629(13) 0.34502(11) -0.19967(11) 0.0350(5) Uani 1 1 d . . . S8 S 0.54350(13) 0.43835(10) -0.05391(11) 0.0322(5) Uani 1 1 d . . . S9 S 0.65191(14) 0.28848(10) -0.02501(11) 0.0361(5) Uani 1 1 d . . . S10 S 0.72532(13) 0.50003(10) -0.22934(11) 0.0339(5) Uani 1 1 d . . . S11 S 0.73433(13) 0.52716(10) -0.05825(10) 0.0307(5) Uani 1 1 d . . . S12 S 0.64637(14) 0.25978(10) -0.19712(12) 0.0405(6) Uani 1 1 d . . . S13 S 0.84401(13) 0.37482(10) -0.02983(11) 0.0326(5) Uani 1 1 d . . . S14 S 0.53654(13) 0.41339(10) -0.22550(11) 0.0346(5) Uani 1 1 d . . . P1 P 0.93639(15) 0.49718(12) -0.13450(13) 0.0406(6) Uani 1 1 d . . . P2 P 0.68588(15) 0.35702(12) -0.34450(12) 0.0427(6) Uani 1 1 d . . . P3 P 0.82534(18) 0.19960(13) -0.08107(14) 0.0513(7) Uani 1 1 d . . . P4 P 0.44499(17) 0.28263(14) -0.12930(16) 0.0582(8) Uani 1 1 d D . . N5 N 0.7033(4) 0.4279(3) 0.0769(3) 0.0300(16) Uani 1 1 d . . . N6 N 0.5603(4) 0.5766(3) -0.1578(3) 0.0307(16) Uani 1 1 d . . . C11 C 0.9582(7) 0.5392(5) -0.2110(6) 0.072(3) Uani 1 1 d . . . H11A H 0.9164 0.5766 -0.2201 0.087 Uiso 1 1 calc R . . H11B H 1.0150 0.5606 -0.2038 0.087 Uiso 1 1 calc R . . C12 C 0.9560(7) 0.4952(6) -0.2710(5) 0.082(4) Uani 1 1 d . . . H12A H 0.9686 0.5230 -0.3095 0.122 Uiso 1 1 calc R . . H12B H 0.8995 0.4747 -0.2799 0.122 Uiso 1 1 calc R . . H12C H 0.9984 0.4587 -0.2635 0.122 Uiso 1 1 calc R . . C13 C 1.0228(6) 0.4318(5) -0.1183(5) 0.059(3) Uani 1 1 d . . . H13A H 1.0155 0.4095 -0.0749 0.071 Uiso 1 1 calc R . . H13B H 1.0140 0.3959 -0.1532 0.071 Uiso 1 1 calc R . . C14 C 1.1119(6) 0.4553(5) -0.1164(6) 0.075(4) Uani 1 1 d . . . H14A H 1.1500 0.4160 -0.1078 0.112 Uiso 1 1 calc R . . H14B H 1.1231 0.4893 -0.0807 0.112 Uiso 1 1 calc R . . H14C H 1.1214 0.4761 -0.1594 0.112 Uiso 1 1 calc R . . C15 C 0.9634(7) 0.5587(5) -0.0692(6) 0.075(4) Uani 1 1 d . . . H15A H 0.9450 0.5407 -0.0269 0.090 Uiso 1 1 calc R . . H15B H 1.0259 0.5638 -0.0631 0.090 Uiso 1 1 calc R . . C16 C 0.9246(7) 0.6276(5) -0.0824(7) 0.094(5) Uani 1 1 d . . . H16A H 0.9422 0.6584 -0.0450 0.141 Uiso 1 1 calc R . . H16B H 0.8627 0.6234 -0.0872 0.141 Uiso 1 1 calc R . . H16C H 0.9435 0.6465 -0.1237 0.141 Uiso 1 1 calc R . . C21 C 0.7699(6) 0.4011(5) -0.3838(5) 0.055(3) Uani 1 1 d . . . H21A H 0.7682 0.4502 -0.3714 0.066 Uiso 1 1 calc R . . H21B H 0.8250 0.3827 -0.3640 0.066 Uiso 1 1 calc R . . C22 C 0.7689(8) 0.3969(6) -0.4601(6) 0.094(4) Uani 1 1 d . . . H22A H 0.8174 0.4222 -0.4744 0.141 Uiso 1 1 calc R . . H22B H 0.7161 0.4170 -0.4810 0.141 Uiso 1 1 calc R . . H22C H 0.7724 0.3487 -0.4736 0.141 Uiso 1 1 calc R . . C23 C 0.6957(6) 0.2687(4) -0.3709(5) 0.056(3) Uani 1 1 d . . . H23A H 0.6481 0.2422 -0.3552 0.067 Uiso 1 1 calc R . . H23B H 0.6891 0.2676 -0.4204 0.067 Uiso 1 1 calc R . . C24 C 0.7780(6) 0.2325(5) -0.3468(6) 0.079(4) Uani 1 1 d . . . H24A H 0.7763 0.1852 -0.3636 0.119 Uiso 1 1 calc R . . H24B H 0.7850 0.2321 -0.2978 0.119 Uiso 1 1 calc R . . H24C H 0.8258 0.2568 -0.3636 0.119 Uiso 1 1 calc R . . C25 C 0.5889(6) 0.3828(5) -0.3944(5) 0.062(3) Uani 1 1 d . . . H25A H 0.5915 0.3662 -0.4407 0.074 Uiso 1 1 calc R . . H25B H 0.5403 0.3599 -0.3763 0.074 Uiso 1 1 calc R . . C26 C 0.5725(6) 0.4618(5) -0.3963(5) 0.062(3) Uani 1 1 d . . . H26A H 0.5191 0.4713 -0.4236 0.093 Uiso 1 1 calc R . . H26B H 0.6192 0.4849 -0.4157 0.093 Uiso 1 1 calc R . . H26C H 0.5688 0.4787 -0.3507 0.093 Uiso 1 1 calc R . . C31 C 0.7616(14) 0.1196(11) -0.1087(15) 0.055(7) Uani 0.511(12) 1 d P A 1 H31A H 0.7495 0.1213 -0.1580 0.066 Uiso 0.511(12) 1 calc PR A 1 H31B H 0.7979 0.0790 -0.0981 0.066 Uiso 0.511(12) 1 calc PR A 1 C32 C 0.6730(12) 0.1075(10) -0.0770(14) 0.077(8) Uani 0.511(12) 1 d P A 1 H32A H 0.6469 0.0648 -0.0946 0.115 Uiso 0.511(12) 1 calc PR A 1 H32B H 0.6348 0.1461 -0.0889 0.115 Uiso 0.511(12) 1 calc PR A 1 H32C H 0.6836 0.1044 -0.0282 0.115 Uiso 0.511(12) 1 calc PR A 1 C33 C 0.826(3) 0.166(2) -0.0074(16) 0.069(11) Uani 0.511(12) 1 d P A 1 H33A H 0.7670 0.1532 -0.0008 0.082 Uiso 0.511(12) 1 calc PR A 1 H33B H 0.8590 0.1226 -0.0076 0.082 Uiso 0.511(12) 1 calc PR A 1 C34 C 0.8619(16) 0.2077(10) 0.0545(11) 0.065(7) Uani 0.511(12) 1 d P A 1 H34A H 0.8568 0.1808 0.0951 0.097 Uiso 0.511(12) 1 calc PR A 1 H34B H 0.8297 0.2505 0.0567 0.097 Uiso 0.511(12) 1 calc PR A 1 H34C H 0.9217 0.2184 0.0509 0.097 Uiso 0.511(12) 1 calc PR A 1 C35 C 0.9225(14) 0.1814(11) -0.1017(13) 0.048(7) Uani 0.511(12) 1 d P A 1 H35A H 0.9389 0.1350 -0.0848 0.057 Uiso 0.511(12) 1 calc PR A 1 H35B H 0.9214 0.1804 -0.1511 0.057 Uiso 0.511(12) 1 calc PR A 1 C36 C 0.9888(15) 0.2325(14) -0.0741(15) 0.059(8) Uani 0.511(12) 1 d P A 1 H36A H 1.0443 0.2191 -0.0875 0.089 Uiso 0.511(12) 1 calc PR A 1 H36B H 0.9910 0.2331 -0.0251 0.089 Uiso 0.511(12) 1 calc PR A 1 H36C H 0.9739 0.2783 -0.0916 0.089 Uiso 0.511(12) 1 calc PR A 1 C31' C 0.8073(16) 0.1324(10) -0.1407(11) 0.057(7) Uani 0.489(12) 1 d P A 2 H31C H 0.8059 0.1511 -0.1867 0.068 Uiso 0.489(12) 1 calc PR A 2 H31D H 0.8532 0.0979 -0.1345 0.068 Uiso 0.489(12) 1 calc PR A 2 C32' C 0.7208(17) 0.0990(11) -0.1298(14) 0.062(7) Uani 0.489(12) 1 d P A 2 H32D H 0.7085 0.0622 -0.1626 0.093 Uiso 0.489(12) 1 calc PR A 2 H32E H 0.6760 0.1337 -0.1354 0.093 Uiso 0.489(12) 1 calc PR A 2 H32F H 0.7233 0.0798 -0.0846 0.093 Uiso 0.489(12) 1 calc PR A 2 C33' C 0.836(2) 0.1839(16) 0.0153(13) 0.034(7) Uani 0.489(12) 1 d P A 2 H33C H 0.8740 0.2195 0.0366 0.040 Uiso 0.489(12) 1 calc PR A 2 H33D H 0.7794 0.1907 0.0314 0.040 Uiso 0.489(12) 1 calc PR A 2 C34' C 0.8675(14) 0.1172(9) 0.0385(11) 0.064(7) Uani 0.489(12) 1 d P A 2 H34D H 0.8706 0.1156 0.0874 0.096 Uiso 0.489(12) 1 calc PR A 2 H34E H 0.9242 0.1098 0.0241 0.096 Uiso 0.489(12) 1 calc PR A 2 H34F H 0.8291 0.0812 0.0196 0.096 Uiso 0.489(12) 1 calc PR A 2 C35' C 0.949(2) 0.2160(14) -0.0911(13) 0.052(9) Uani 0.489(12) 1 d P A 2 H35C H 0.9534 0.2345 -0.1365 0.062 Uiso 0.489(12) 1 calc PR A 2 H35D H 0.9695 0.2520 -0.0587 0.062 Uiso 0.489(12) 1 calc PR A 2 C36' C 1.0071(16) 0.1547(12) -0.0810(11) 0.086(9) Uani 0.489(12) 1 d P A 2 H36D H 1.0654 0.1689 -0.0867 0.129 Uiso 0.489(12) 1 calc PR A 2 H36E H 0.9892 0.1192 -0.1140 0.129 Uiso 0.489(12) 1 calc PR A 2 H36F H 1.0047 0.1364 -0.0359 0.129 Uiso 0.489(12) 1 calc PR A 2 C41 C 0.4516(14) 0.1893(7) -0.1204(9) 0.098(8) Uiso 0.70(2) 1 d PD B 1 H41A H 0.3985 0.1674 -0.1399 0.118 Uiso 0.70(2) 1 calc PR B 1 H41B H 0.4994 0.1710 -0.1433 0.118 Uiso 0.70(2) 1 calc PR B 1 C42 C 0.4662(12) 0.1748(10) -0.0422(8) 0.095(7) Uiso 0.70(2) 1 d PD B 1 H42A H 0.4684 0.1251 -0.0343 0.143 Uiso 0.70(2) 1 calc PR B 1 H42B H 0.4193 0.1946 -0.0201 0.143 Uiso 0.70(2) 1 calc PR B 1 H42C H 0.5197 0.1957 -0.0239 0.143 Uiso 0.70(2) 1 calc PR B 1 C41' C 0.4365(17) 0.1997(10) -0.0886(16) 0.034(8) Uiso 0.30(2) 1 d PD B 2 H41C H 0.4173 0.2108 -0.0444 0.041 Uiso 0.30(2) 1 calc PR B 2 H41D H 0.3877 0.1770 -0.1142 0.041 Uiso 0.30(2) 1 calc PR B 2 C42' C 0.503(2) 0.1416(15) -0.074(2) 0.077(14) Uiso 0.30(2) 1 d PD B 2 H42D H 0.4759 0.1029 -0.0530 0.115 Uiso 0.30(2) 1 calc PR B 2 H42E H 0.5501 0.1587 -0.0438 0.115 Uiso 0.30(2) 1 calc PR B 2 H42F H 0.5233 0.1265 -0.1160 0.115 Uiso 0.30(2) 1 calc PR B 2 C43 C 0.3705(7) 0.3220(6) -0.0725(7) 0.094(4) Uani 1 1 d D B . H43A H 0.3982 0.3200 -0.0262 0.113 Uiso 1 1 calc R . . H43B H 0.3639 0.3712 -0.0845 0.113 Uiso 1 1 calc R . . C44 C 0.2830(7) 0.2917(7) -0.0722(8) 0.124(6) Uani 1 1 d D . . H44A H 0.2515 0.3168 -0.0403 0.186 Uiso 1 1 calc R B . H44B H 0.2876 0.2433 -0.0591 0.186 Uiso 1 1 calc R . . H44C H 0.2529 0.2953 -0.1171 0.186 Uiso 1 1 calc R . . C45 C 0.3774(7) 0.2861(7) -0.2085(6) 0.097(5) Uani 1 1 d D B . H45A H 0.3236 0.2617 -0.2033 0.116 Uiso 1 1 calc R . . H45B H 0.3636 0.3346 -0.2195 0.116 Uiso 1 1 calc R . . C46 C 0.4203(8) 0.2533(7) -0.2668(6) 0.102(5) Uani 1 1 d D . . H46A H 0.3820 0.2565 -0.3081 0.153 Uiso 1 1 calc R B . H46B H 0.4329 0.2050 -0.2567 0.153 Uiso 1 1 calc R . . H46C H 0.4731 0.2778 -0.2728 0.153 Uiso 1 1 calc R . . C51 C 0.7577(5) 0.3939(4) 0.1196(4) 0.033(2) Uani 1 1 d . . . H51A H 0.7930 0.3601 0.1025 0.040 Uiso 1 1 calc R . . C52 C 0.7647(5) 0.4056(4) 0.1863(4) 0.040(2) Uani 1 1 d . . . H52A H 0.8050 0.3797 0.2141 0.048 Uiso 1 1 calc R . . C53 C 0.7151(5) 0.4540(4) 0.2161(4) 0.036(2) Uani 1 1 d . C . C54 C 0.6589(5) 0.4884(4) 0.1718(4) 0.039(2) Uani 1 1 d . . . H54A H 0.6224 0.5222 0.1876 0.047 Uiso 1 1 calc R . . C55 C 0.6550(5) 0.4740(4) 0.1033(4) 0.037(2) Uani 1 1 d . . . H55A H 0.6153 0.4988 0.0740 0.045 Uiso 1 1 calc R . . C56 C 0.7233(6) 0.4690(5) 0.2906(5) 0.048(2) Uani 1 1 d . . . C57 C 0.6643(18) 0.5161(17) 0.3130(12) 0.114(16) Uani 0.55(2) 1 d P C 1 H57A H 0.6708 0.5607 0.2915 0.171 Uiso 0.55(2) 1 calc PR C 1 H57B H 0.6744 0.5212 0.3616 0.171 Uiso 0.55(2) 1 calc PR C 1 H57C H 0.6066 0.4989 0.3013 0.171 Uiso 0.55(2) 1 calc PR C 1 C58 C 0.7066(15) 0.3972(12) 0.3270(10) 0.077(9) Uani 0.55(2) 1 d P C 1 H58A H 0.6986 0.3607 0.2934 0.116 Uiso 0.55(2) 1 calc PR C 1 H58B H 0.6556 0.4011 0.3507 0.116 Uiso 0.55(2) 1 calc PR C 1 H58C H 0.7554 0.3862 0.3589 0.116 Uiso 0.55(2) 1 calc PR C 1 C59 C 0.8153(14) 0.4868(13) 0.3137(10) 0.072(8) Uani 0.55(2) 1 d P C 1 H59A H 0.8309 0.5296 0.2923 0.108 Uiso 0.55(2) 1 calc PR C 1 H59B H 0.8524 0.4497 0.3011 0.108 Uiso 0.55(2) 1 calc PR C 1 H59C H 0.8218 0.4925 0.3624 0.108 Uiso 0.55(2) 1 calc PR C 1 C57' C 0.6342(19) 0.4588(16) 0.3162(14) 0.078(11) Uani 0.45(2) 1 d P C 2 H57D H 0.5997 0.5000 0.3065 0.118 Uiso 0.45(2) 1 calc PR C 2 H57E H 0.6408 0.4507 0.3646 0.118 Uiso 0.45(2) 1 calc PR C 2 H57F H 0.6060 0.4192 0.2936 0.118 Uiso 0.45(2) 1 calc PR C 2 C58' C 0.789(2) 0.4347(16) 0.3293(14) 0.086(11) Uani 0.45(2) 1 d P C 2 H58D H 0.8415 0.4609 0.3291 0.129 Uiso 0.45(2) 1 calc PR C 2 H58E H 0.7965 0.3889 0.3106 0.129 Uiso 0.45(2) 1 calc PR C 2 H58F H 0.7739 0.4303 0.3754 0.129 Uiso 0.45(2) 1 calc PR C 2 C59' C 0.741(3) 0.5495(12) 0.2995(13) 0.101(15) Uani 0.45(2) 1 d P C 2 H59D H 0.7468 0.5703 0.2557 0.151 Uiso 0.45(2) 1 calc PR C 2 H59E H 0.7942 0.5563 0.3284 0.151 Uiso 0.45(2) 1 calc PR C 2 H59F H 0.6944 0.5711 0.3200 0.151 Uiso 0.45(2) 1 calc PR C 2 C61 C 0.5274(5) 0.6083(4) -0.1074(5) 0.038(2) Uani 1 1 d . . . H61A H 0.5345 0.5880 -0.0642 0.046 Uiso 1 1 calc R . . C62 C 0.4832(6) 0.6697(4) -0.1153(5) 0.044(2) Uani 1 1 d . . . H62A H 0.4603 0.6894 -0.0777 0.053 Uiso 1 1 calc R . . C63 C 0.4714(5) 0.7031(4) -0.1762(4) 0.037(2) Uani 1 1 d . . . C64 C 0.5064(6) 0.6678(4) -0.2271(5) 0.046(2) Uani 1 1 d . . . H64A H 0.5004 0.6864 -0.2710 0.055 Uiso 1 1 calc R . . C65 C 0.5482(6) 0.6089(4) -0.2163(5) 0.048(3) Uani 1 1 d . . . H65A H 0.5712 0.5882 -0.2534 0.057 Uiso 1 1 calc R . . C66 C 0.4251(5) 0.7702(4) -0.1857(5) 0.041(2) Uani 1 1 d . . . C67 C 0.3373(6) 0.7666(5) -0.1620(5) 0.066(3) Uani 1 1 d . . . H67A H 0.3416 0.7506 -0.1155 0.099 Uiso 1 1 calc R . . H67B H 0.3023 0.7345 -0.1902 0.099 Uiso 1 1 calc R . . H67C H 0.3113 0.8122 -0.1648 0.099 Uiso 1 1 calc R . . C68 C 0.4145(8) 0.7944(6) -0.2591(6) 0.093(5) Uani 1 1 d . . . H68A H 0.4703 0.7976 -0.2760 0.140 Uiso 1 1 calc R . . H68B H 0.3870 0.8395 -0.2617 0.140 Uiso 1 1 calc R . . H68C H 0.3794 0.7613 -0.2861 0.140 Uiso 1 1 calc R . . C69 C 0.4768(8) 0.8246(5) -0.1467(7) 0.106(5) Uani 1 1 d . . . H69A H 0.5330 0.8276 -0.1629 0.160 Uiso 1 1 calc R . . H69B H 0.4827 0.8125 -0.0991 0.160 Uiso 1 1 calc R . . H69C H 0.4480 0.8690 -0.1528 0.160 Uiso 1 1 calc R . . 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 0.02168(18) 0.03204(17) 0.0310(2) -0.00988(14) 0.00090(15) -0.00103(13) W2 0.02254(19) 0.03381(18) 0.0333(2) -0.01190(15) -0.00133(15) 0.00100(14) W3 0.02413(19) 0.02918(17) 0.0364(2) -0.00971(15) -0.00109(15) 0.00393(14) W4 0.02193(18) 0.02978(17) 0.0410(2) -0.00555(15) -0.00010(16) -0.00038(14) W5 0.02297(18) 0.02728(16) 0.0312(2) -0.00560(14) 0.00175(15) 0.00274(13) W6 0.02347(18) 0.02829(17) 0.0302(2) -0.00486(14) 0.00190(15) 0.00235(13) S7 0.0247(12) 0.0435(12) 0.0361(13) -0.0139(10) -0.0012(10) 0.0039(9) S8 0.0267(12) 0.0331(10) 0.0370(13) 0.0011(9) 0.0044(10) 0.0046(9) S9 0.0327(13) 0.0299(10) 0.0447(14) -0.0020(10) -0.0008(11) 0.0032(9) S10 0.0292(12) 0.0402(12) 0.0321(13) -0.0069(9) 0.0018(10) -0.0011(9) S11 0.0335(12) 0.0291(10) 0.0292(12) -0.0071(9) 0.0017(10) -0.0010(9) S12 0.0340(13) 0.0333(11) 0.0524(15) -0.0145(10) -0.0044(11) -0.0002(10) S13 0.0251(11) 0.0380(11) 0.0343(13) -0.0087(10) 0.0002(9) 0.0013(9) S14 0.0263(12) 0.0377(11) 0.0390(13) -0.0051(10) -0.0008(10) 0.0001(9) P1 0.0307(13) 0.0463(13) 0.0447(15) -0.0139(11) 0.0024(11) -0.0059(11) P2 0.0374(14) 0.0527(15) 0.0370(15) -0.0172(12) -0.0016(11) -0.0035(11) P3 0.0568(18) 0.0427(14) 0.0504(17) -0.0167(12) -0.0155(14) 0.0191(13) P4 0.0357(16) 0.0602(17) 0.076(2) 0.0076(15) -0.0078(14) -0.0168(13) N5 0.022(4) 0.027(3) 0.040(4) -0.004(3) 0.000(3) 0.002(3) N6 0.025(4) 0.037(4) 0.031(4) -0.001(3) 0.005(3) 0.001(3) C11 0.055(7) 0.069(7) 0.095(10) 0.000(7) 0.013(7) -0.020(6) C12 0.076(9) 0.102(9) 0.072(9) -0.018(7) 0.037(7) -0.013(7) C13 0.033(6) 0.082(8) 0.063(7) -0.012(6) 0.003(5) -0.002(5) C14 0.042(7) 0.066(7) 0.115(11) -0.002(7) 0.004(7) -0.011(6) C15 0.084(9) 0.058(7) 0.080(9) -0.026(6) -0.005(7) 0.000(6) C16 0.058(8) 0.043(6) 0.175(15) 0.018(8) -0.015(9) 0.010(6) C21 0.042(6) 0.078(7) 0.047(6) -0.022(5) 0.012(5) -0.014(5) C22 0.097(10) 0.126(11) 0.064(9) -0.023(8) 0.031(8) -0.015(9) C23 0.052(7) 0.048(6) 0.064(7) -0.030(5) -0.012(5) 0.000(5) C24 0.061(8) 0.071(7) 0.103(10) -0.050(7) -0.009(7) 0.024(6) C25 0.043(6) 0.084(8) 0.055(7) -0.034(6) -0.012(5) -0.007(6) C26 0.057(7) 0.060(7) 0.065(8) 0.003(6) -0.009(6) 0.008(5) C31 0.033(15) 0.032(12) 0.09(2) -0.020(12) -0.023(14) 0.010(10) C32 0.042(14) 0.048(12) 0.13(2) -0.020(14) -0.015(14) 0.000(10) C33 0.08(2) 0.08(2) 0.05(2) -0.018(16) -0.008(18) 0.037(18) C34 0.10(2) 0.052(14) 0.039(14) -0.004(11) -0.002(14) 0.017(13) C35 0.039(14) 0.046(13) 0.059(16) 0.004(13) 0.015(12) 0.035(12) C36 0.046(17) 0.050(14) 0.08(2) -0.027(14) 0.019(15) -0.004(13) C31' 0.081(19) 0.046(12) 0.047(14) -0.007(10) 0.026(13) 0.005(12) C32' 0.07(2) 0.042(14) 0.07(2) -0.006(12) 0.000(16) 0.001(13) C33' 0.025(12) 0.06(2) 0.017(16) 0.007(14) -0.002(12) 0.002(12) C34' 0.075(17) 0.051(13) 0.063(16) 0.035(11) -0.008(13) 0.009(11) C35' 0.09(3) 0.038(17) 0.024(14) 0.003(13) -0.012(15) 0.007(17) C36' 0.11(2) 0.11(2) 0.043(15) -0.019(14) 0.015(15) 0.037(17) C43 0.061(8) 0.093(10) 0.129(13) 0.003(9) 0.013(8) -0.033(7) C44 0.073(10) 0.124(12) 0.182(17) 0.041(12) 0.043(11) 0.009(9) C45 0.057(8) 0.123(12) 0.109(12) 0.010(9) -0.004(8) -0.045(8) C46 0.082(10) 0.128(12) 0.093(11) -0.037(9) -0.010(8) -0.045(9) C51 0.035(5) 0.034(4) 0.031(5) 0.003(4) 0.010(4) 0.007(4) C52 0.038(5) 0.040(5) 0.041(6) 0.005(4) 0.001(4) 0.009(4) C53 0.022(5) 0.048(5) 0.037(5) -0.002(4) 0.007(4) -0.001(4) C54 0.030(5) 0.044(5) 0.043(6) -0.005(4) 0.001(4) 0.015(4) C55 0.027(5) 0.037(5) 0.046(6) -0.013(4) -0.003(4) 0.014(4) C56 0.042(6) 0.063(6) 0.038(6) -0.006(5) -0.001(5) 0.011(5) C57 0.11(3) 0.17(4) 0.050(17) -0.05(2) -0.013(18) 0.09(3) C58 0.078(19) 0.12(2) 0.034(12) 0.010(12) -0.001(11) -0.006(15) C59 0.074(17) 0.09(2) 0.045(13) 0.004(12) -0.024(11) -0.021(14) C57' 0.11(3) 0.09(2) 0.045(17) -0.019(17) 0.025(16) -0.02(2) C58' 0.10(3) 0.09(2) 0.06(2) -0.011(18) -0.004(18) 0.02(2) C59' 0.21(5) 0.049(16) 0.045(17) -0.028(13) 0.01(2) -0.03(2) C61 0.042(6) 0.024(4) 0.049(6) 0.018(4) 0.011(5) 0.004(4) C62 0.044(6) 0.043(5) 0.046(6) 0.009(4) 0.013(5) 0.003(4) C63 0.032(5) 0.030(4) 0.049(6) 0.011(4) 0.001(4) 0.000(4) C64 0.055(6) 0.048(5) 0.036(6) 0.018(4) 0.014(5) 0.014(5) C65 0.049(6) 0.048(5) 0.049(6) 0.009(5) 0.020(5) 0.013(5) C66 0.035(5) 0.027(4) 0.061(7) 0.010(4) 0.007(5) 0.003(4) C67 0.053(7) 0.069(7) 0.082(8) 0.036(6) 0.033(6) 0.029(5) C68 0.099(10) 0.085(9) 0.101(11) 0.051(8) 0.040(9) 0.043(7) C69 0.089(10) 0.042(7) 0.182(16) 0.003(8) -0.019(10) 0.018(7) 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 S7 2.4569(19) . ? W1 S10 2.459(2) . ? W1 S13 2.459(2) . ? W1 S11 2.4689(19) . ? W1 P1 2.522(2) . ? W1 W2 2.6579(5) . ? W1 W6 2.6651(5) . ? W1 W5 2.6717(5) . ? W1 W3 2.6798(5) . ? W2 S12 2.451(2) . ? W2 S7 2.455(2) . ? W2 S10 2.462(2) . ? W2 S14 2.466(2) . ? W2 P2 2.518(2) . ? W2 W4 2.6723(5) . ? W2 W6 2.6815(4) . ? W2 W3 2.6820(5) . ? W3 S7 2.453(2) . ? W3 S13 2.457(2) . ? W3 S9 2.459(2) . ? W3 S12 2.461(2) . ? W3 P3 2.509(2) . ? W3 W5 2.6570(4) . ? W3 W4 2.6647(5) . ? W4 S12 2.450(2) . ? W4 S8 2.453(2) . ? W4 S9 2.457(2) . ? W4 S14 2.459(2) . ? W4 P4 2.543(2) . ? W4 W6 2.6706(5) . ? W4 W5 2.6892(5) . ? W5 N5 2.263(7) . ? W5 S11 2.4494(19) . ? W5 S13 2.451(2) . ? W5 S9 2.451(2) . ? W5 S8 2.454(2) . ? W5 W6 2.6463(5) . ? W6 N6 2.257(6) . ? W6 S11 2.450(2) . ? W6 S14 2.455(2) . ? W6 S10 2.456(2) . ? W6 S8 2.464(2) . ? P1 C15 1.798(10) . ? P1 C11 1.803(11) . ? P1 C13 1.876(10) . ? P2 C23 1.811(8) . ? P2 C25 1.821(10) . ? P2 C21 1.826(9) . ? P3 C33 1.62(4) . ? P3 C35 1.67(2) . ? P3 C31' 1.78(2) . ? P3 C31 1.91(2) . ? P3 C33' 1.95(3) . ? P3 C35' 2.01(3) . ? P4 C41' 1.821(14) . ? P4 C41 1.829(13) . ? P4 C45 1.831(10) . ? P4 C43 1.882(10) . ? N5 C55 1.324(9) . ? N5 C51 1.331(10) . ? N6 C65 1.329(10) . ? N6 C61 1.335(10) . ? C11 C12 1.478(13) . ? C13 C14 1.480(12) . ? C15 C16 1.490(12) . ? C21 C22 1.534(13) . ? C23 C24 1.520(12) . ? C25 C26 1.560(12) . ? C31 C32 1.61(3) . ? C33 C34 1.55(3) . ? C35 C36 1.51(3) . ? C31' C32' 1.55(3) . ? C33' C34' 1.45(4) . ? C35' C36' 1.51(4) . ? C41 C42 1.591(15) . ? C41' C42' 1.549(17) . ? C43 C44 1.507(12) . ? C45 C46 1.548(12) . ? C51 C52 1.354(11) . ? C52 C53 1.398(10) . ? C53 C54 1.372(11) . ? C53 C56 1.517(12) . ? C54 C55 1.400(11) . ? C56 C58' 1.40(3) . ? C56 C57 1.41(2) . ? C56 C59 1.53(2) . ? C56 C57' 1.56(3) . ? C56 C59' 1.60(2) . ? C56 C58 1.61(2) . ? C61 C62 1.387(10) . ? C62 C63 1.382(11) . ? C63 C64 1.390(11) . ? C63 C66 1.502(10) . ? C64 C65 1.333(11) . ? C66 C69 1.511(14) . ? C66 C67 1.515(11) . ? C66 C68 1.540(13) . ? _cod_database_code 2000044