#------------------------------------------------------------------------------ #$Date: 2015-01-07 18:25:02 +0200 (Wed, 07 Jan 2015) $ #$Revision: 129439 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/00/40/1004001.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_1004001 _publ_contact_author ; Prof. Francis J. DiSalvo Department of Chemistry and Chemical Biology Cornell University Ithaca, NY 14853 ; _publ_contact_email fjd3@cornell.edu _publ_contact_author_fax '607-255-4137' _publ_contact_author_phone '607-255-7238' 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_page_first 2666 _journal_page_last 2674 _journal_volume 40 _journal_year 2001 _chemical_formula_moiety 'W6 S8 (PC12H27)6' _chemical_formula_sum 'C72 H162 P6 S8 W6' _chemical_formula_weight 2573.42 _chemical_melting_point ? _chemical_name_common 'Tungsten sulfide cluster with tri-n-' _chemical_name_systematic ; octakis(mu!3$-sulfido)-hexakis(tri-n-butylphosphine) -hexa-tungsten ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 103.3240(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 24.6648(12) _cell_length_b 19.8619(9) _cell_length_c 20.1365(10) _cell_measurement_reflns_used ? _cell_measurement_temperature 163(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 9599.1(8) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'BRUKER SMART' _computing_data_reduction SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 163(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.927 _diffrn_measured_fraction_theta_max 0.927 _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 67732 _diffrn_reflns_theta_full 33.22 _diffrn_reflns_theta_max 33.22 _diffrn_reflns_theta_min 1.56 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 7.469 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.529617 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ? _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description block _exptl_crystal_F_000 5024 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.983 _refine_diff_density_min -1.718 _refine_diff_density_rms 0.396 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 581 _refine_ls_number_reflns 17073 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0250 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.0590 _reflns_number_gt 13885 _reflns_number_total 17073 _reflns_threshold_expression >2sigma(I) _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 1004001 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 0.221998(5) 0.661077(5) 0.487536(5) 0.01761(3) Uani 1 1 d . . . W2 W 0.318507(5) 0.720290(5) 0.483260(5) 0.01700(3) Uani 1 1 d . . . W3 W 0.277213(5) 0.732942(5) 0.594292(5) 0.01748(3) Uani 1 1 d . . . S1 S 0.31176(3) 0.62583(3) 0.55952(4) 0.02175(14) Uani 1 1 d . . . S2 S 0.26217(3) 0.65700(3) 0.38643(4) 0.02124(14) Uani 1 1 d . . . S3 S 0.13662(3) 0.71088(4) 0.41763(4) 0.02330(14) Uani 1 1 d . . . S4 S 0.18644(3) 0.68070(4) 0.59069(4) 0.02235(14) Uani 1 1 d . . . P1 P 0.18736(4) 0.54149(4) 0.47100(4) 0.02516(16) Uani 1 1 d . . . P2 P 0.41114(3) 0.68164(4) 0.46487(4) 0.02415(15) Uani 1 1 d . . . P3 P 0.31241(4) 0.70392(5) 0.71849(4) 0.03089(19) Uani 1 1 d . . . C101 C 0.1333(4) 0.5201(4) 0.5175(5) 0.0234(16) Uani 0.533(8) 1 d P A 1 H10A H 0.1237 0.4719 0.5093 0.028 Uiso 0.533(8) 1 calc PR A 1 H10B H 0.1495 0.5255 0.5669 0.028 Uiso 0.533(8) 1 calc PR A 1 C102 C 0.0800(3) 0.5605(3) 0.4994(4) 0.0297(15) Uani 0.533(8) 1 d P A 1 H10C H 0.0610 0.5508 0.4514 0.036 Uiso 0.533(8) 1 calc PR A 1 H10Z H 0.0895 0.6090 0.5026 0.036 Uiso 0.533(8) 1 calc PR A 1 C103 C 0.0396(3) 0.5458(4) 0.5453(4) 0.046(2) Uani 0.533(8) 1 d P A 1 H10D H 0.0044 0.5707 0.5277 0.056 Uiso 0.533(8) 1 calc PR A 1 H10E H 0.0308 0.4971 0.5433 0.056 Uiso 0.533(8) 1 calc PR A 1 C104 C 0.0624(4) 0.5650(6) 0.6156(6) 0.061(3) Uani 0.533(8) 1 d P A 1 H10F H 0.0352 0.5551 0.6429 0.091 Uiso 0.533(8) 1 calc PR A 1 H10G H 0.0708 0.6133 0.6179 0.091 Uiso 0.533(8) 1 calc PR A 1 H10H H 0.0967 0.5395 0.6336 0.091 Uiso 0.533(8) 1 calc PR A 1 C11' C 0.1512(5) 0.5088(7) 0.5335(7) 0.038(3) Uani 0.467(8) 1 d P A 2 H11H H 0.1430 0.4605 0.5240 0.046 Uiso 0.467(8) 1 calc PR A 2 H11I H 0.1763 0.5122 0.5795 0.046 Uiso 0.467(8) 1 calc PR A 2 C12' C 0.0974(5) 0.5450(5) 0.5340(6) 0.050(3) Uani 0.467(8) 1 d P A 2 H12A H 0.0694 0.5362 0.4910 0.060 Uiso 0.467(8) 1 calc PR A 2 H12Z H 0.1039 0.5942 0.5384 0.060 Uiso 0.467(8) 1 calc PR A 2 C13' C 0.0750(5) 0.5158(5) 0.6005(5) 0.090(5) Uani 0.467(8) 1 d P A 2 H13A H 0.0616 0.4689 0.5925 0.03(2) Uiso 0.467(8) 1 calc PR A 2 H13B H 0.1051 0.5172 0.6426 0.25(11) Uiso 0.467(8) 1 calc PR A 2 C14' C 0.0282(5) 0.5624(5) 0.6060(5) 0.082(5) Uani 0.467(8) 1 d PR A 2 H14A H 0.0124 0.5484 0.6443 0.099 Uiso 0.467(8) 1 calc PR A 2 H14B H -0.0008 0.5607 0.5636 0.099 Uiso 0.467(8) 1 calc PR A 2 H14C H 0.0425 0.6085 0.6137 0.099 Uiso 0.467(8) 1 calc PR A 2 C105 C 0.15063(15) 0.51964(15) 0.38377(17) 0.0318(7) Uani 1 1 d . A . H10I H 0.1173 0.5488 0.3710 0.038 Uiso 1 1 calc R . . H10Y H 0.1752 0.5310 0.3529 0.038 Uiso 1 1 calc R . . C106 C 0.13194(17) 0.44700(17) 0.37022(19) 0.0426(9) Uani 1 1 d . . . H10J H 0.1652 0.4175 0.3806 0.051 Uiso 1 1 calc R A . H10K H 0.1080 0.4346 0.4016 0.051 Uiso 1 1 calc R . . C107 C 0.10028(19) 0.4340(2) 0.2979(2) 0.0516(11) Uani 1 1 d . A . H10L H 0.0659 0.4615 0.2883 0.062 Uiso 1 1 calc R . . H10M H 0.1233 0.4487 0.2663 0.062 Uiso 1 1 calc R . . C108 C 0.0847(2) 0.3611(2) 0.2838(2) 0.0760(18) Uani 1 1 d . . . H10N H 0.0642 0.3561 0.2362 0.114 Uiso 1 1 calc R A . H10O H 0.0611 0.3463 0.3141 0.114 Uiso 1 1 calc R . . H10P H 0.1185 0.3336 0.2919 0.114 Uiso 1 1 calc R . . C109 C 0.24167(15) 0.47756(15) 0.49410(17) 0.0333(8) Uani 1 1 d . A . H10Q H 0.2599 0.4831 0.5430 0.040 Uiso 1 1 calc R . . H10R H 0.2237 0.4327 0.4886 0.040 Uiso 1 1 calc R . . C110 C 0.28632(15) 0.47870(16) 0.45350(17) 0.0333(8) Uani 1 1 d . . . H11A H 0.2982 0.5258 0.4491 0.040 Uiso 1 1 calc R A . H11B H 0.2706 0.4611 0.4071 0.040 Uiso 1 1 calc R . . C111 C 0.33680(18) 0.4367(2) 0.4873(2) 0.0528(11) Uani 1 1 d . A . H11C H 0.3520 0.4539 0.5340 0.063 Uiso 1 1 calc R . . H11D H 0.3248 0.3896 0.4912 0.063 Uiso 1 1 calc R . . C112 C 0.38193(18) 0.4376(2) 0.4487(3) 0.0576(12) Uani 1 1 d . . . H11E H 0.4133 0.4099 0.4728 0.086 Uiso 1 1 calc R A . H11F H 0.3946 0.4839 0.4454 0.086 Uiso 1 1 calc R . . H11G H 0.3675 0.4194 0.4028 0.086 Uiso 1 1 calc R . . C201 C 0.4087(5) 0.6477(5) 0.3791(6) 0.0270(17) Uani 0.734(12) 1 d P B 1 H20A H 0.4459 0.6295 0.3784 0.032 Uiso 0.734(12) 1 calc PR B 1 H20B H 0.3820 0.6096 0.3707 0.032 Uiso 0.734(12) 1 calc PR B 1 C202 C 0.3920(3) 0.6979(3) 0.3214(3) 0.0305(12) Uani 0.734(12) 1 d P B 1 H20C H 0.3598 0.7242 0.3289 0.037 Uiso 0.734(12) 1 calc PR B 1 H20D H 0.4232 0.7297 0.3235 0.037 Uiso 0.734(12) 1 calc PR B 1 C203 C 0.3766(3) 0.6683(3) 0.2508(3) 0.0493(19) Uani 0.734(12) 1 d P B 1 H20E H 0.3465 0.6349 0.2490 0.059 Uiso 0.734(12) 1 calc PR B 1 H20F H 0.3617 0.7046 0.2179 0.059 Uiso 0.734(12) 1 calc PR B 1 C204 C 0.4236(6) 0.6351(7) 0.2287(5) 0.174(8) Uani 0.734(12) 1 d P B 1 H20G H 0.4104 0.6172 0.1825 0.261 Uiso 0.734(12) 1 calc PR B 1 H20H H 0.4380 0.5981 0.2601 0.261 Uiso 0.734(12) 1 calc PR B 1 H20I H 0.4532 0.6680 0.2292 0.261 Uiso 0.734(12) 1 calc PR B 1 C21' C 0.4144(14) 0.6309(13) 0.3902(18) 0.027(4) Uani 0.266(12) 1 d P B 2 H21F H 0.4516 0.6094 0.3977 0.032 Uiso 0.266(12) 1 calc PR B 2 H21G H 0.3862 0.5946 0.3849 0.032 Uiso 0.266(12) 1 calc PR B 2 C22' C 0.4042(8) 0.6725(11) 0.3247(9) 0.037(4) Uani 0.266(12) 1 d P B 2 H22A H 0.3672 0.6942 0.3176 0.044 Uiso 0.266(12) 1 calc PR B 2 H22B H 0.4325 0.7087 0.3303 0.044 Uiso 0.266(12) 1 calc PR B 2 C23' C 0.4065(8) 0.6313(9) 0.2611(9) 0.050(5) Uani 0.266(12) 1 d P B 2 H23A H 0.4412 0.6045 0.2713 0.060 Uiso 0.266(12) 1 calc PR B 2 H23B H 0.3749 0.5992 0.2525 0.060 Uiso 0.266(12) 1 calc PR B 2 C24' C 0.4045(10) 0.6679(14) 0.2005(10) 0.083(8) Uani 0.266(12) 1 d P B 2 H24A H 0.4035 0.6365 0.1627 0.099 Uiso 0.266(12) 1 calc PR B 2 H24B H 0.4376 0.6965 0.2063 0.099 Uiso 0.266(12) 1 calc PR B 2 H24C H 0.3710 0.6962 0.1904 0.099 Uiso 0.266(12) 1 calc PR B 2 C205 C 0.44569(15) 0.61636(17) 0.52372(18) 0.0344(7) Uani 1 1 d . B . H20J H 0.4201 0.5776 0.5208 0.041 Uiso 1 1 calc R . . H20K H 0.4790 0.6007 0.5085 0.041 Uiso 1 1 calc R . . C206 C 0.46383(18) 0.6381(2) 0.59829(19) 0.0463(10) Uani 1 1 d . . . H20L H 0.4302 0.6485 0.6153 0.056 Uiso 0.52(2) 1 calc PR B 1 H20M H 0.4858 0.6801 0.6007 0.056 Uiso 0.52(2) 1 calc PR B 1 H20R H 0.5004 0.6610 0.6056 0.056 Uiso 0.48(2) 1 calc PR B 2 H20S H 0.4366 0.6709 0.6083 0.056 Uiso 0.48(2) 1 calc PR B 2 C207 C 0.4992(5) 0.5848(7) 0.6465(6) 0.057(3) Uani 0.52(2) 1 d P B 1 H20N H 0.5321 0.5718 0.6290 0.068 Uiso 0.52(2) 1 calc PR B 1 H20X H 0.5126 0.6040 0.6928 0.068 Uiso 0.52(2) 1 calc PR B 1 C208 C 0.4622(7) 0.5219(6) 0.6497(6) 0.068(4) Uani 0.52(2) 1 d P B 1 H20P H 0.4834 0.4890 0.6817 0.102 Uiso 0.52(2) 1 calc PR B 1 H20Q H 0.4510 0.5016 0.6042 0.102 Uiso 0.52(2) 1 calc PR B 1 H20R H 0.4289 0.5355 0.6651 0.102 Uiso 0.52(2) 1 calc PR B 1 C27' C 0.4685(12) 0.5791(9) 0.6475(7) 0.090(7) Uani 0.48(2) 1 d P B 2 H27A H 0.4817 0.5976 0.6941 0.108 Uiso 0.48(2) 1 calc PR B 2 H27B H 0.4302 0.5623 0.6443 0.108 Uiso 0.48(2) 1 calc PR B 2 C28' C 0.5010(12) 0.5240(8) 0.6425(8) 0.117(9) Uani 0.48(2) 1 d P B 2 H28A H 0.4951 0.4893 0.6747 0.175 Uiso 0.48(2) 1 calc PR B 2 H28B H 0.5404 0.5374 0.6534 0.175 Uiso 0.48(2) 1 calc PR B 2 H28C H 0.4909 0.5061 0.5960 0.175 Uiso 0.48(2) 1 calc PR B 2 C209 C 0.46358(13) 0.74862(16) 0.47293(18) 0.0300(7) Uani 1 1 d . B . H20O H 0.4489 0.7834 0.4382 0.036 Uiso 1 1 calc R . . H20W H 0.4675 0.7699 0.5182 0.036 Uiso 1 1 calc R . . C210 C 0.52155(15) 0.72880(19) 0.4654(2) 0.0405(8) Uani 1 1 d . . . H20S H 0.5375 0.6958 0.5014 0.049 Uiso 1 1 calc R B . H20T H 0.5181 0.7063 0.4207 0.049 Uiso 1 1 calc R . . C211 C 0.56111(17) 0.7870(2) 0.4700(2) 0.0517(11) Uani 1 1 d . B . H21A H 0.5650 0.8093 0.5149 0.062 Uiso 1 1 calc R . . H21B H 0.5452 0.8203 0.4342 0.062 Uiso 1 1 calc R . . C212 C 0.61794(18) 0.7662(3) 0.4618(3) 0.0619(13) Uani 1 1 d . . . H21C H 0.6419 0.8060 0.4652 0.093 Uiso 1 1 calc R B . H21D H 0.6145 0.7450 0.4170 0.093 Uiso 1 1 calc R . . H21E H 0.6343 0.7341 0.4977 0.093 Uiso 1 1 calc R . . C301 C 0.3311(6) 0.6203(6) 0.7393(5) 0.033(2) Uani 0.64(3) 1 d P C 1 H30A H 0.3577 0.6049 0.7123 0.040 Uiso 0.64(3) 1 calc PR C 1 H30B H 0.3500 0.6173 0.7883 0.040 Uiso 0.64(3) 1 calc PR C 1 C302 C 0.2795(7) 0.5741(5) 0.7247(6) 0.039(3) Uani 0.64(3) 1 d P C 1 H30C H 0.2536 0.5894 0.7526 0.047 Uiso 0.64(3) 1 calc PR C 1 H30D H 0.2601 0.5788 0.6761 0.047 Uiso 0.64(3) 1 calc PR C 1 C303 C 0.2925(9) 0.5014(5) 0.7395(5) 0.051(4) Uani 0.64(3) 1 d P C 1 H30E H 0.3132 0.4967 0.7876 0.062 Uiso 0.64(3) 1 calc PR C 1 H30F H 0.3171 0.4854 0.7102 0.062 Uiso 0.64(3) 1 calc PR C 1 C304 C 0.2418(9) 0.4574(5) 0.7277(7) 0.062(4) Uani 0.64(3) 1 d P C 1 H30G H 0.2530 0.4105 0.7383 0.093 Uiso 0.64(3) 1 calc PR C 1 H30H H 0.2215 0.4607 0.6799 0.093 Uiso 0.64(3) 1 calc PR C 1 H30I H 0.2176 0.4721 0.7573 0.093 Uiso 0.64(3) 1 calc PR C 1 C31' C 0.3148(7) 0.6045(8) 0.7326(7) 0.016(2) Uani 0.36(3) 1 d P C 2 H31H H 0.3410 0.5852 0.7071 0.019 Uiso 0.36(3) 1 calc PR C 2 H31Z H 0.3304 0.5955 0.7816 0.019 Uiso 0.36(3) 1 calc PR C 2 C32' C 0.2585(8) 0.5665(9) 0.7105(9) 0.026(3) Uani 0.36(3) 1 d P C 2 H32A H 0.2437 0.5714 0.6607 0.031 Uiso 0.36(3) 1 calc PR C 2 H32B H 0.2311 0.5861 0.7340 0.031 Uiso 0.36(3) 1 calc PR C 2 C33' C 0.2674(8) 0.4899(7) 0.7294(9) 0.032(3) Uani 0.36(3) 1 d P C 2 H33A H 0.2948 0.4707 0.7057 0.038 Uiso 0.36(3) 1 calc PR C 2 H33B H 0.2827 0.4854 0.7791 0.038 Uiso 0.36(3) 1 calc PR C 2 C34' C 0.2131(9) 0.4505(7) 0.7093(8) 0.039(4) Uani 0.36(3) 1 d P C 2 H34A H 0.2202 0.4030 0.7214 0.058 Uiso 0.36(3) 1 calc PR C 2 H34B H 0.1980 0.4544 0.6600 0.058 Uiso 0.36(3) 1 calc PR C 2 H34C H 0.1862 0.4687 0.7335 0.058 Uiso 0.36(3) 1 calc PR C 2 C305 C 0.3817(3) 0.7501(4) 0.7583(4) 0.0340(18) Uani 0.610(10) 1 d P C 1 H30J H 0.3969 0.7315 0.8045 0.041 Uiso 0.610(10) 1 calc PR C 1 H30K H 0.4089 0.7402 0.7303 0.041 Uiso 0.610(10) 1 calc PR C 1 C306 C 0.3768(3) 0.8273(4) 0.7643(4) 0.0363(16) Uani 0.610(10) 1 d P C 1 H30L H 0.3510 0.8444 0.7225 0.044 Uiso 0.610(10) 1 calc PR C 1 H30Z H 0.3602 0.8376 0.8035 0.044 Uiso 0.610(10) 1 calc PR C 1 C307 C 0.4315(3) 0.8638(4) 0.7736(4) 0.058(2) Uani 0.610(10) 1 d P C 1 H30M H 0.4474 0.8546 0.7337 0.069 Uiso 0.610(10) 1 calc PR C 1 H30N H 0.4246 0.9128 0.7748 0.069 Uiso 0.610(10) 1 calc PR C 1 C308 C 0.4733(4) 0.8442(6) 0.8373(5) 0.092(4) Uani 0.610(10) 1 d P C 1 H30O H 0.5075 0.8704 0.8408 0.138 Uiso 0.610(10) 1 calc PR C 1 H30P H 0.4818 0.7961 0.8356 0.138 Uiso 0.610(10) 1 calc PR C 1 H30Q H 0.4579 0.8532 0.8772 0.138 Uiso 0.610(10) 1 calc PR C 1 C35' C 0.3787(5) 0.7217(5) 0.7626(6) 0.025(2) Uani 0.390(10) 1 d P C 2 H35A H 0.3867 0.6972 0.8066 0.030 Uiso 0.390(10) 1 calc PR C 2 H35B H 0.4055 0.7063 0.7361 0.030 Uiso 0.390(10) 1 calc PR C 2 C36' C 0.3862(4) 0.7979(5) 0.7763(5) 0.0246(19) Uani 0.390(10) 1 d P C 2 H36A H 0.3767 0.8222 0.7322 0.030 Uiso 0.390(10) 1 calc PR C 2 H36B H 0.3598 0.8127 0.8037 0.030 Uiso 0.390(10) 1 calc PR C 2 C37' C 0.4451(4) 0.8163(5) 0.8137(6) 0.046(3) Uani 0.390(10) 1 d P C 2 H37A H 0.4554 0.7898 0.8564 0.055 Uiso 0.390(10) 1 calc PR C 2 H37B H 0.4712 0.8041 0.7849 0.055 Uiso 0.390(10) 1 calc PR C 2 C38' C 0.4515(6) 0.8908(6) 0.8310(8) 0.067(4) Uani 0.390(10) 1 d P C 2 H38A H 0.4901 0.9000 0.8552 0.100 Uiso 0.390(10) 1 calc PR C 2 H38B H 0.4263 0.9032 0.8601 0.100 Uiso 0.390(10) 1 calc PR C 2 H38C H 0.4424 0.9173 0.7888 0.100 Uiso 0.390(10) 1 calc PR C 2 C309 C 0.26647(14) 0.72969(16) 0.77369(15) 0.0286(7) Uani 1 1 d . C . H30R H 0.2629 0.7793 0.7715 0.034 Uiso 1 1 calc R . . H30S H 0.2290 0.7106 0.7547 0.034 Uiso 1 1 calc R . . C310 C 0.28445(17) 0.70919(19) 0.84890(17) 0.0401(9) Uani 1 1 d . . . H31A H 0.2864 0.6595 0.8518 0.048 Uiso 1 1 calc R C . H31B H 0.3223 0.7269 0.8681 0.048 Uiso 1 1 calc R . . C311 C 0.24542(17) 0.73457(19) 0.89221(18) 0.0403(9) Uani 1 1 d . C . H31C H 0.2070 0.7199 0.8709 0.048 Uiso 1 1 calc R . . H31D H 0.2562 0.7135 0.9379 0.048 Uiso 1 1 calc R . . C312 C 0.24594(19) 0.8098(2) 0.9005(2) 0.0477(10) Uani 1 1 d . . . H31E H 0.2202 0.8227 0.9288 0.072 Uiso 1 1 calc R C . H31F H 0.2343 0.8311 0.8556 0.072 Uiso 1 1 calc R . . H31G H 0.2837 0.8247 0.9225 0.072 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 0.01963(6) 0.01538(5) 0.01926(5) -0.00059(4) 0.00741(4) -0.00143(4) W2 0.01750(6) 0.01722(5) 0.01737(5) -0.00004(4) 0.00626(4) 0.00013(4) W3 0.01970(6) 0.01794(5) 0.01551(5) 0.00054(4) 0.00549(4) 0.00091(4) S1 0.0252(4) 0.0197(3) 0.0216(3) 0.0028(2) 0.0080(3) 0.0040(3) S2 0.0242(4) 0.0207(3) 0.0198(3) -0.0031(2) 0.0072(3) -0.0006(2) S3 0.0191(4) 0.0270(3) 0.0234(3) -0.0045(3) 0.0041(3) -0.0019(3) S4 0.0260(4) 0.0206(3) 0.0233(3) 0.0013(2) 0.0114(3) -0.0020(3) P1 0.0318(5) 0.0181(3) 0.0286(4) -0.0015(3) 0.0133(3) -0.0041(3) P2 0.0211(4) 0.0261(4) 0.0270(4) -0.0009(3) 0.0091(3) 0.0022(3) P3 0.0338(5) 0.0426(5) 0.0170(4) 0.0040(3) 0.0075(3) 0.0157(4) C101 0.017(5) 0.019(3) 0.039(5) 0.003(3) 0.016(3) 0.001(3) C102 0.028(4) 0.031(3) 0.034(4) 0.000(3) 0.014(3) -0.003(3) C103 0.044(5) 0.042(4) 0.063(5) 0.006(4) 0.032(4) 0.000(3) C104 0.048(6) 0.069(6) 0.075(7) -0.005(5) 0.035(6) -0.007(5) C11' 0.028(7) 0.038(6) 0.050(7) 0.000(4) 0.011(5) -0.005(4) C12' 0.045(6) 0.042(5) 0.057(7) 0.001(4) 0.000(5) -0.019(4) C13' 0.087(10) 0.124(13) 0.062(8) -0.050(8) 0.025(7) -0.003(9) C14' 0.136(15) 0.066(8) 0.061(8) -0.006(6) 0.054(10) -0.011(10) C105 0.034(2) 0.0225(14) 0.0368(18) -0.0027(12) 0.0032(14) -0.0031(12) C106 0.052(2) 0.0265(16) 0.043(2) -0.0046(14) -0.0026(17) -0.0082(15) C107 0.062(3) 0.042(2) 0.044(2) -0.0078(17) -0.0041(19) -0.0134(19) C108 0.111(5) 0.046(3) 0.052(3) -0.016(2) -0.019(3) -0.012(3) C109 0.046(2) 0.0196(14) 0.0322(17) 0.0040(12) 0.0040(14) -0.0018(13) C110 0.037(2) 0.0243(15) 0.0360(18) -0.0045(13) 0.0030(14) 0.0078(13) C111 0.044(3) 0.043(2) 0.069(3) 0.015(2) 0.006(2) 0.0122(18) C112 0.042(3) 0.047(2) 0.081(3) -0.011(2) 0.007(2) 0.0113(19) C201 0.030(3) 0.025(5) 0.029(4) 0.001(3) 0.012(3) 0.007(3) C202 0.033(3) 0.033(3) 0.027(2) 0.000(2) 0.011(2) 0.005(2) C203 0.069(5) 0.046(3) 0.029(3) -0.004(2) 0.004(3) 0.015(3) C204 0.228(16) 0.261(17) 0.042(6) 0.027(8) 0.049(8) 0.182(14) C21' 0.033(12) 0.014(10) 0.036(13) 0.001(7) 0.014(9) -0.001(7) C22' 0.029(9) 0.042(11) 0.040(9) 0.001(8) 0.010(6) 0.015(7) C23' 0.043(11) 0.056(11) 0.054(11) 0.019(8) 0.018(8) -0.004(8) C24' 0.072(16) 0.14(2) 0.035(11) -0.016(12) 0.013(10) 0.008(14) C205 0.0283(19) 0.0326(17) 0.044(2) 0.0031(14) 0.0112(14) 0.0087(13) C206 0.046(3) 0.048(2) 0.040(2) 0.0087(17) 0.0001(17) 0.0079(18) C207 0.018(5) 0.090(8) 0.063(6) 0.035(5) 0.010(4) 0.015(5) C208 0.071(9) 0.061(7) 0.077(7) 0.042(5) 0.027(6) 0.030(6) C27' 0.117(18) 0.095(12) 0.054(7) 0.026(7) 0.012(9) 0.053(12) C28' 0.15(2) 0.101(12) 0.108(12) 0.051(9) 0.047(12) 0.087(13) C209 0.0201(16) 0.0326(16) 0.0385(18) -0.0018(13) 0.0093(13) -0.0007(12) C210 0.0266(19) 0.049(2) 0.049(2) 0.0014(17) 0.0169(16) 0.0019(15) C211 0.028(2) 0.061(3) 0.070(3) 0.010(2) 0.0203(19) -0.0047(18) C212 0.028(2) 0.091(4) 0.069(3) 0.023(3) 0.015(2) -0.001(2) C301 0.042(6) 0.030(5) 0.029(3) 0.004(3) 0.011(4) 0.005(4) C302 0.062(9) 0.031(4) 0.025(4) 0.009(3) 0.014(5) 0.019(5) C303 0.091(11) 0.027(4) 0.036(4) 0.007(3) 0.015(5) 0.007(5) C304 0.109(13) 0.032(4) 0.055(6) 0.006(4) 0.035(7) 0.004(6) C31' 0.017(6) 0.011(5) 0.017(4) 0.003(3) 0.001(4) -0.003(4) C32' 0.031(8) 0.024(5) 0.021(6) 0.002(4) 0.002(5) 0.002(5) C33' 0.037(9) 0.015(5) 0.041(7) 0.007(4) 0.004(6) -0.006(5) C34' 0.052(10) 0.030(5) 0.035(7) 0.004(4) 0.012(6) -0.016(6) C305 0.030(4) 0.049(5) 0.022(3) 0.008(4) 0.003(2) 0.007(4) C306 0.034(4) 0.039(4) 0.034(3) -0.004(3) 0.004(3) 0.000(3) C307 0.046(5) 0.064(5) 0.056(5) 0.001(4) -0.004(3) -0.009(4) C308 0.069(7) 0.116(10) 0.071(7) 0.003(6) -0.026(5) -0.023(6) C35' 0.029(5) 0.026(5) 0.021(4) 0.007(4) 0.007(3) 0.002(4) C36' 0.028(5) 0.016(4) 0.028(4) -0.005(4) 0.003(3) 0.002(3) C37' 0.019(5) 0.047(6) 0.070(8) -0.022(5) 0.006(5) -0.007(4) C38' 0.050(8) 0.044(7) 0.104(12) -0.030(7) 0.013(7) -0.019(6) C309 0.0320(18) 0.0340(16) 0.0211(14) 0.0019(12) 0.0085(12) 0.0095(13) C310 0.051(2) 0.051(2) 0.0215(16) 0.0055(14) 0.0145(15) 0.0200(18) C311 0.048(2) 0.053(2) 0.0233(16) 0.0026(15) 0.0155(15) 0.0113(17) C312 0.058(3) 0.053(2) 0.035(2) -0.0089(17) 0.0165(18) 0.006(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 S1 2.4522(7) . ? W1 S3 2.4553(7) . ? W1 S2 2.4624(7) . ? W1 S4 2.4649(7) . ? W1 P1 2.5202(8) . ? W1 W2 2.67417(19) . ? W1 W3 2.67604(17) 7_566 ? W1 W3 2.67655(17) . ? W1 W2 2.67701(18) 7_566 ? W2 S4 2.4527(7) 7_566 ? W2 S1 2.4543(7) . ? W2 S3 2.4614(7) 7_566 ? W2 S2 2.4626(7) . ? W2 P2 2.5172(8) . ? W2 W3 2.67374(19) . ? W2 W1 2.67702(18) 7_566 ? W2 W3 2.67884(18) 7_566 ? W3 S1 2.4530(7) . ? W3 S4 2.4535(8) . ? W3 S2 2.4590(7) 7_566 ? W3 S3 2.4607(8) 7_566 ? W3 P3 2.5179(8) . ? W3 W1 2.67599(18) 7_566 ? W3 W2 2.67882(18) 7_566 ? S2 W3 2.4591(7) 7_566 ? S3 W3 2.4607(8) 7_566 ? S3 W2 2.4614(7) 7_566 ? S4 W2 2.4528(7) 7_566 ? P1 C11' 1.822(15) . ? P1 C109 1.826(3) . ? P1 C105 1.833(3) . ? P1 C101 1.847(10) . ? P2 C21' 1.83(4) . ? P2 C205 1.829(3) . ? P2 C209 1.836(3) . ? P2 C201 1.842(13) . ? P3 C35' 1.709(12) . ? P3 C301 1.749(11) . ? P3 C309 1.834(3) . ? P3 C305 1.943(9) . ? P3 C31' 1.994(15) . ? C101 C102 1.511(10) . ? C102 C103 1.535(10) . ? C103 C104 1.450(14) . ? C11' C12' 1.511(14) . ? C12' C13' 1.668(13) . ? C13' C14' 1.5039 . ? C105 C106 1.520(4) . ? C106 C107 1.508(5) . ? C107 C108 1.508(5) . ? C109 C110 1.516(5) . ? C110 C111 1.523(5) . ? C111 C112 1.496(6) . ? C201 C202 1.516(9) . ? C202 C203 1.504(8) . ? C203 C204 1.486(13) . ? C21' C22' 1.53(3) . ? C22' C23' 1.53(3) . ? C23' C24' 1.41(3) . ? C205 C206 1.527(5) . ? C206 C27' 1.521(16) . ? C206 C207 1.561(11) . ? C207 C208 1.557(19) . ? C27' C28' 1.38(3) . ? C209 C210 1.524(5) . ? C210 C211 1.502(5) . ? C211 C212 1.507(6) . ? C301 C302 1.542(11) . ? C302 C303 1.494(12) . ? C303 C304 1.500(12) . ? C31' C32' 1.554(15) . ? C32' C33' 1.57(2) . ? C33' C34' 1.522(15) . ? C305 C306 1.544(9) . ? C306 C307 1.505(10) . ? C307 C308 1.501(12) . ? C35' C36' 1.540(12) . ? C36' C37' 1.520(13) . ? C37' C38' 1.520(15) . ? C309 C310 1.532(4) . ? C310 C311 1.526(5) . ? C311 C312 1.503(5) . ? 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 S1 W1 S3 172.80(2) . . ? S1 W1 S2 89.93(2) . . ? S3 W1 S2 89.69(3) . . ? S1 W1 S4 89.72(3) . . ? S3 W1 S4 89.70(3) . . ? S2 W1 S4 172.36(2) . . ? S1 W1 P1 92.37(3) . . ? S3 W1 P1 94.83(3) . . ? S2 W1 P1 92.78(2) . . ? S4 W1 P1 94.86(3) . . ? S1 W1 W2 57.010(18) . . ? S3 W1 W2 117.167(19) . . ? S2 W1 W2 57.117(17) . . ? S4 W1 W2 116.733(18) . . ? P1 W1 W2 133.43(2) . . ? S1 W1 W3 117.054(18) . 7_566 ? S3 W1 W3 57.117(18) . 7_566 ? S2 W1 W3 57.000(16) . 7_566 ? S4 W1 W3 116.681(17) . 7_566 ? P1 W1 W3 135.265(19) . 7_566 ? W2 W1 W3 60.092(4) . 7_566 ? S1 W1 W3 56.944(17) . . ? S3 W1 W3 117.131(17) . . ? S2 W1 W3 117.027(17) . . ? S4 W1 W3 56.827(18) . . ? P1 W1 W3 134.665(19) . . ? W2 W1 W3 59.960(4) . . ? W3 W1 W3 90.029(6) 7_566 . ? S1 W1 W2 116.950(17) . 7_566 ? S3 W1 W2 57.121(17) . 7_566 ? S2 W1 W2 116.887(17) . 7_566 ? S4 W1 W2 56.801(17) . 7_566 ? P1 W1 W2 136.57(2) . 7_566 ? W2 W1 W2 89.999(5) . 7_566 ? W3 W1 W2 59.930(5) 7_566 7_566 ? W3 W1 W2 60.050(4) . 7_566 ? S4 W2 S1 172.62(3) 7_566 . ? S4 W2 S3 89.84(2) 7_566 7_566 ? S1 W2 S3 90.00(2) . 7_566 ? S4 W2 S2 89.34(2) 7_566 . ? S1 W2 S2 89.88(2) . . ? S3 W2 S2 172.64(3) 7_566 . ? S4 W2 P2 94.30(3) 7_566 . ? S1 W2 P2 93.08(3) . . ? S3 W2 P2 91.99(3) 7_566 . ? S2 W2 P2 95.37(3) . . ? S4 W2 W3 117.201(18) 7_566 . ? S1 W2 W3 56.962(17) . . ? S3 W2 W3 57.086(19) 7_566 . ? S2 W2 W3 117.125(18) . . ? P2 W2 W3 133.254(19) . . ? S4 W2 W1 116.874(19) 7_566 . ? S1 W2 W1 56.936(18) . . ? S3 W2 W1 117.095(19) 7_566 . ? S2 W2 W1 57.110(18) . . ? P2 W2 W1 135.682(19) . . ? W3 W2 W1 60.064(4) . . ? S4 W2 W1 57.237(18) 7_566 7_566 ? S1 W2 W1 116.925(18) . 7_566 ? S3 W2 W1 56.903(18) 7_566 7_566 ? S2 W2 W1 116.886(17) . 7_566 ? P2 W2 W1 134.270(19) . 7_566 ? W3 W2 W1 60.015(4) . 7_566 ? W1 W2 W1 89.999(5) . 7_566 ? S4 W2 W3 56.919(18) 7_566 7_566 ? S1 W2 W3 116.876(18) . 7_566 ? S3 W2 W3 116.829(18) 7_566 7_566 ? S2 W2 W3 56.960(17) . 7_566 ? P2 W2 W3 136.707(19) . 7_566 ? W3 W2 W3 90.029(6) . 7_566 ? W1 W2 W3 59.988(5) . 7_566 ? W1 W2 W3 59.966(4) 7_566 7_566 ? S1 W3 S4 89.97(3) . . ? S1 W3 S2 172.70(2) . 7_566 ? S4 W3 S2 89.40(2) . 7_566 ? S1 W3 S3 90.04(3) . 7_566 ? S4 W3 S3 172.61(2) . 7_566 ? S2 W3 S3 89.65(3) 7_566 7_566 ? S1 W3 P3 91.27(3) . . ? S4 W3 P3 92.06(3) . . ? S2 W3 P3 96.03(3) 7_566 . ? S3 W3 P3 95.33(3) 7_566 . ? S1 W3 W2 57.008(17) . . ? S4 W3 W2 117.156(17) . . ? S2 W3 W2 117.132(17) 7_566 . ? S3 W3 W2 57.109(17) 7_566 . ? P3 W3 W2 134.31(2) . . ? S1 W3 W1 117.009(18) . 7_566 ? S4 W3 W1 116.778(17) . 7_566 ? S2 W3 W1 57.122(17) 7_566 7_566 ? S3 W3 W1 56.924(17) 7_566 7_566 ? P3 W3 W1 137.89(2) . 7_566 ? W2 W3 W1 60.053(5) . 7_566 ? S1 W3 W1 56.916(18) . . ? S4 W3 W1 57.235(17) . . ? S2 W3 W1 117.029(17) 7_566 . ? S3 W3 W1 117.030(17) 7_566 . ? P3 W3 W1 132.13(2) . . ? W2 W3 W1 59.976(5) . . ? W1 W3 W1 89.970(6) 7_566 . ? S1 W3 W2 116.855(18) . 7_566 ? S4 W3 W2 56.894(17) . 7_566 ? S2 W3 W2 57.085(17) 7_566 7_566 ? S3 W3 W2 116.800(18) 7_566 7_566 ? P3 W3 W2 135.58(2) . 7_566 ? W2 W3 W2 89.970(5) . 7_566 ? W1 W3 W2 59.918(4) 7_566 7_566 ? W1 W3 W2 59.983(4) . 7_566 ? W1 S1 W3 66.140(18) . . ? W1 S1 W2 66.054(17) . . ? W3 S1 W2 66.030(18) . . ? W3 S2 W1 65.878(18) 7_566 . ? W3 S2 W2 65.953(17) 7_566 . ? W1 S2 W2 65.773(18) . . ? W1 S3 W3 65.960(19) . 7_566 ? W1 S3 W2 65.977(18) . 7_566 ? W3 S3 W2 65.803(18) 7_566 7_566 ? W2 S4 W3 66.186(18) 7_566 . ? W2 S4 W1 65.962(18) 7_566 . ? W3 S4 W1 65.938(19) . . ? C11' P1 C109 91.3(4) . . ? C11' P1 C105 111.4(4) . . ? C109 P1 C105 104.53(15) . . ? C11' P1 C101 16.7(3) . . ? C109 P1 C101 106.5(3) . . ? C105 P1 C101 100.1(3) . . ? C11' P1 W1 116.7(4) . . ? C109 P1 W1 114.53(11) . . ? C105 P1 W1 115.29(10) . . ? C101 P1 W1 114.4(3) . . ? C21' P2 C205 92.3(7) . . ? C21' P2 C209 108.0(11) . . ? C205 P2 C209 104.05(16) . . ? C21' P2 C201 12.8(7) . . ? C205 P2 C201 104.9(2) . . ? C209 P2 C201 102.6(4) . . ? C21' P2 W2 120.2(11) . . ? C205 P2 W2 115.09(12) . . ? C209 P2 W2 114.26(11) . . ? C201 P2 W2 114.5(4) . . ? C35' P3 C301 84.5(6) . . ? C35' P3 C309 106.1(5) . . ? C301 P3 C309 106.6(4) . . ? C35' P3 C305 16.7(3) . . ? C301 P3 C305 101.0(6) . . ? C309 P3 C305 103.0(3) . . ? C35' P3 C31' 97.9(6) . . ? C301 P3 C31' 13.5(5) . . ? C309 P3 C31' 101.1(5) . . ? C305 P3 C31' 114.5(5) . . ? C35' P3 W3 122.6(4) . . ? C301 P3 W3 117.8(4) . . ? C309 P3 W3 114.74(10) . . ? C305 P3 W3 111.8(2) . . ? C31' P3 W3 111.1(4) . . ? C102 C101 P1 116.4(6) . . ? C101 C102 C103 113.8(7) . . ? C104 C103 C102 112.2(7) . . ? C12' C11' P1 113.8(8) . . ? C11' C12' C13' 107.0(9) . . ? C14' C13' C12' 104.3(6) . . ? C106 C105 P1 117.3(2) . . ? C107 C106 C105 113.8(3) . . ? C108 C107 C106 113.5(4) . . ? C110 C109 P1 115.7(2) . . ? C109 C110 C111 111.8(3) . . ? C112 C111 C110 113.1(4) . . ? C202 C201 P2 115.0(6) . . ? C203 C202 C201 115.6(6) . . ? C204 C203 C202 114.3(7) . . ? C22' C21' P2 112.5(16) . . ? C23' C22' C21' 113.7(19) . . ? C24' C23' C22' 116.6(18) . . ? C206 C205 P2 115.0(2) . . ? C27' C206 C205 112.5(7) . . ? C27' C206 C207 29.0(9) . . ? C205 C206 C207 114.5(6) . . ? C208 C207 C206 108.7(10) . . ? C28' C27' C206 122(2) . . ? C210 C209 P2 117.5(2) . . ? C211 C210 C209 113.9(3) . . ? C210 C211 C212 112.9(4) . . ? C302 C301 P3 111.0(7) . . ? C303 C302 C301 114.0(8) . . ? C302 C303 C304 113.5(8) . . ? C32' C31' P3 116.4(10) . . ? C31' C32' C33' 109.6(11) . . ? C34' C33' C32' 111.7(12) . . ? C306 C305 P3 115.0(5) . . ? C307 C306 C305 113.8(7) . . ? C308 C307 C306 113.7(7) . . ? C36' C35' P3 110.9(7) . . ? C37' C36' C35' 112.7(9) . . ? C38' C37' C36' 112.7(9) . . ? C310 C309 P3 116.5(2) . . ? C311 C310 C309 113.6(3) . . ? C312 C311 C310 113.7(3) . . ? #===END _journal_paper_doi 10.1021/ic001314q