# ic981001j.cif data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Dr. Daniel Rabinovich Department of Chemistry University of North Carolina at Charlotte 9201 University City Blvd. Charlotte, NC 28223 USA ; _publ_contact_author_phone '+704 547 4442' _publ_contact_author_fax '+704 547 3151' _publ_contact_author_email DRabinov@email.uncc.edu _publ_requested_journal 'Inorganic Chemistry' # 2. TITLE AND AUTHOR LIST _publ_section_title ; Tris[(alkylthio)methyl]silanes: Synthesis and Structures of Chromium, Molybdenum, and Tungsten Complexes with a Tripodal Thioether Ligand ; loop_ _publ_author_name _publ_author_address 'Yim, H. M.' ; Department of Chemistry The University of North Carolina at Charlotte 9201 University City Blvd. Charlotte, NC 28223 ; 'Tran, L. M.' ; Department of Chemistry The University of North Carolina at Charlotte 9201 University City Blvd. Charlotte, NC 28223 ; 'Dobbin, E. D.' ; Department of Chemistry The University of North Carolina at Charlotte 9201 University City Blvd. Charlotte, NC 28223 ; 'Liable-Sands, L. M.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Incarvito C. D.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Lam, K. -C.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Rheingold, A. L.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; # 3. Results data_drab03 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H18 Mo O3 S3 Si' _chemical_formula_weight 406.45 _chemical_melting_point ? _chemical_compound_source ? 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.34630(6) _cell_length_b 15.2747(2) _cell_length_c 27.1865(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.8987(9) _cell_angle_gamma 90.00 _cell_volume 3465.44(10) _cell_formula_units_Z 8 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 7801 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method ? _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 1.184 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 'Siemens P4/CCD' _diffrn_measurement_method 'phi, omega' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19659 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.91 _reflns_number_total 7793 _reflns_number_observed 6722 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-5.03 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXL-5.03 (Sheldrick, 1994)' _computing_molecular_graphics XP _computing_publication_material XCIF _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 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 'idealized contributions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7789 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_obs 0.0260 _refine_ls_wR_factor_all 0.0634 _refine_ls_wR_factor_obs 0.0603 _refine_ls_goodness_of_fit_all 1.064 _refine_ls_goodness_of_fit_obs 1.103 _refine_ls_restrained_S_all 1.073 _refine_ls_restrained_S_obs 1.103 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1A Mo 0.41359(2) 0.903196(10) 0.258558(6) 0.02198(5) Uani 1 d . . S11A S 0.61305(7) 1.01163(3) 0.30229(2) 0.02763(11) Uani 1 d . . S21A S 0.40573(6) 1.01019(3) 0.18310(2) 0.02672(11) Uani 1 d . . S31A S 0.66465(6) 0.83605(3) 0.21552(2) 0.02421(11) Uani 1 d . . Si1A Si 0.77412(7) 1.02934(3) 0.19965(2) 0.02647(12) Uani 1 d . . O1A O 0.1095(2) 0.99226(12) 0.30419(7) 0.0505(5) Uani 1 d . . O2A O 0.4027(2) 0.76567(11) 0.34477(6) 0.0463(4) Uani 1 d . . O3A O 0.1665(2) 0.77725(10) 0.20542(7) 0.0453(4) Uani 1 d . . C1A C 0.2234(3) 0.95934(14) 0.28713(8) 0.0313(5) Uani 1 d . . C2A C 0.4107(2) 0.81866(14) 0.31366(8) 0.0294(5) Uani 1 d . . C3A C 0.2623(2) 0.82284(12) 0.22479(8) 0.0287(4) Uani 1 d . . C4A C 0.9472(3) 1.09429(15) 0.17452(9) 0.0385(5) Uani 1 d . . H4AA H 1.0350(3) 1.09544(15) 0.19887(9) 0.058 Uiso 1 calc R . H4AB H 0.9120(3) 1.15427(15) 0.16749(9) 0.058 Uiso 1 calc R . H4AC H 0.9843(3) 1.06684(15) 0.14418(9) 0.058 Uiso 1 calc R . C11A C 0.7047(3) 1.08597(13) 0.25811(8) 0.0322(5) Uani 1 d . . H11A H 0.7978(3) 1.11500(13) 0.27413(8) 0.039 Uiso 1 calc R . H11B H 0.6262(3) 1.13201(13) 0.24903(8) 0.039 Uiso 1 calc R . C12A C 0.5064(3) 1.09104(15) 0.34004(9) 0.0429(6) Uani 1 d . . H12A H 0.4497(3) 1.06025(15) 0.36617(9) 0.064 Uiso 1 calc R . H12B H 0.4290(3) 1.12315(15) 0.31943(9) 0.064 Uiso 1 calc R . H12C H 0.5833(3) 1.13226(15) 0.35474(9) 0.064 Uiso 1 calc R . C21A C 0.6005(2) 1.02575(14) 0.15326(8) 0.0295(4) Uani 1 d . . H21A H 0.5981(2) 1.08112(14) 0.13433(8) 0.035 Uiso 1 calc R . H21B H 0.6182(2) 0.97723(14) 0.12981(8) 0.035 Uiso 1 calc R . C22A C 0.2958(3) 0.9542(2) 0.13363(9) 0.0460(6) Uani 1 d . . H22A H 0.1867(3) 0.9413(2) 0.14433(9) 0.069 Uiso 1 calc R . H22B H 0.3505(3) 0.8994(2) 0.12558(9) 0.069 Uiso 1 calc R . H22C H 0.2912(3) 0.9919(2) 0.10447(9) 0.069 Uiso 1 calc R . C31A C 0.8352(2) 0.91244(13) 0.21615(8) 0.0287(4) Uani 1 d . . H31A H 0.9159(2) 0.89186(13) 0.19246(8) 0.034 Uiso 1 calc R . H31B H 0.8860(2) 0.91222(13) 0.24931(8) 0.034 Uiso 1 calc R . C32A C 0.7523(3) 0.74595(14) 0.25160(9) 0.0374(5) Uani 1 d . . H32A H 0.6734(3) 0.69880(14) 0.25462(9) 0.056 Uiso 1 calc R . H32B H 0.7828(3) 0.76726(14) 0.28442(9) 0.056 Uiso 1 calc R . H32C H 0.8474(3) 0.72367(14) 0.23501(9) 0.056 Uiso 1 calc R . Mo1B Mo 1.09005(2) 1.271848(10) 0.488992(6) 0.02125(5) Uani 1 d . . S11B S 0.84167(6) 1.33174(3) 0.53656(2) 0.02398(10) Uani 1 d . . S21B S 1.08846(6) 1.14852(3) 0.55571(2) 0.02841(11) Uani 1 d . . S31B S 0.88035(6) 1.18689(3) 0.43582(2) 0.02568(11) Uani 1 d . . Si1B Si 0.72118(7) 1.13941(4) 0.53358(2) 0.02853(13) Uani 1 d . . O1B O 1.3402(2) 1.38663(10) 0.54863(7) 0.0481(5) Uani 1 d . . O2B O 1.1039(2) 1.41511(12) 0.40576(7) 0.0513(5) Uani 1 d . . O3B O 1.3905(2) 1.18494(13) 0.43996(7) 0.0542(5) Uani 1 d . . C1B C 1.2436(3) 1.34419(13) 0.52744(8) 0.0296(5) Uani 1 d . . C2B C 1.0967(3) 1.36169(14) 0.43704(8) 0.0310(5) Uani 1 d . . C3B C 1.2772(3) 1.21762(14) 0.45819(8) 0.0312(5) Uani 1 d . . C4B C 0.5452(3) 1.07256(14) 0.55421(10) 0.0396(6) Uani 1 d . . H4BA H 0.5768(3) 1.01093(14) 0.55688(10) 0.059 Uiso 1 calc R . H4BB H 0.4572(3) 1.07831(14) 0.53016(10) 0.059 Uiso 1 calc R . H4BC H 0.5101(3) 1.09363(14) 0.58633(10) 0.059 Uiso 1 calc R . C11B C 0.6670(2) 1.25994(13) 0.52775(8) 0.0285(4) Uani 1 d . . H11C H 0.6191(2) 1.27067(13) 0.49476(8) 0.034 Uiso 1 calc R . H11D H 0.5855(2) 1.27464(13) 0.55252(8) 0.034 Uiso 1 calc R . C12B C 0.7644(3) 1.43185(13) 0.50822(10) 0.0430(6) Uani 1 d . . H12D H 0.8465(3) 1.47763(13) 0.51012(10) 0.065 Uiso 1 calc R . H12E H 0.6688(3) 1.45120(13) 0.52567(10) 0.065 Uiso 1 calc R . H12F H 0.7363(3) 1.42046(13) 0.47367(10) 0.065 Uiso 1 calc R . C21B C 0.8895(3) 1.12958(15) 0.58152(9) 0.0358(5) Uani 1 d . . H21C H 0.8712(3) 1.17253(15) 0.60811(9) 0.043 Uiso 1 calc R . H21D H 0.8867(3) 1.07033(15) 0.59624(9) 0.043 Uiso 1 calc R . C22B C 1.1949(3) 1.1873(2) 0.61085(9) 0.0469(6) Uani 1 d . . H22D H 1.3063(3) 1.2005(2) 0.60277(9) 0.070 Uiso 1 calc R . H22E H 1.1925(3) 1.1418(2) 0.63626(9) 0.070 Uiso 1 calc R . H22F H 1.1429(3) 1.2403(2) 0.62306(9) 0.070 Uiso 1 calc R . C31B C 0.7923(3) 1.09779(13) 0.47138(9) 0.0338(5) Uani 1 d . . H31C H 0.8729(3) 1.05102(13) 0.47657(9) 0.041 Uiso 1 calc R . H31D H 0.7005(3) 1.07251(13) 0.45276(9) 0.041 Uiso 1 calc R . C32B C 0.9816(3) 1.1267(2) 0.38730(9) 0.0416(6) Uani 1 d . . H32D H 1.0346(3) 1.1681(2) 0.36535(9) 0.062 Uiso 1 calc R . H32E H 0.9028(3) 1.0923(2) 0.36846(9) 0.062 Uiso 1 calc R . H32F H 1.0617(3) 1.0874(2) 0.40206(9) 0.062 Uiso 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 Mo1A 0.02343(9) 0.02236(8) 0.02017(9) 0.00001(6) 0.00060(7) -0.00005(6) S11A 0.0366(3) 0.0246(2) 0.0216(3) -0.0024(2) -0.0029(2) -0.0002(2) S21A 0.0265(3) 0.0268(2) 0.0268(3) 0.0030(2) -0.0015(2) 0.0024(2) S31A 0.0267(2) 0.0225(2) 0.0234(3) -0.0016(2) -0.0011(2) 0.0006(2) Si1A 0.0267(3) 0.0246(3) 0.0281(3) 0.0013(2) 0.0015(2) -0.0026(2) O1A 0.0376(10) 0.0678(12) 0.0462(11) -0.0151(9) 0.0088(8) 0.0134(9) O2A 0.0575(12) 0.0439(9) 0.0377(10) 0.0142(8) 0.0038(8) -0.0042(8) O3A 0.0390(9) 0.0281(8) 0.0682(13) -0.0011(8) -0.0185(9) -0.0032(7) C1A 0.0302(11) 0.0356(11) 0.0280(12) -0.0030(9) -0.0006(9) 0.0006(9) C2A 0.0282(11) 0.0321(10) 0.0280(12) -0.0002(9) 0.0014(9) -0.0009(8) C3A 0.0272(10) 0.0227(9) 0.0362(12) 0.0038(9) -0.0001(9) 0.0029(8) C4A 0.0353(12) 0.0381(12) 0.0422(14) 0.0040(10) 0.0051(11) -0.0111(10) C11A 0.0416(13) 0.0245(9) 0.0307(12) -0.0027(9) 0.0023(10) -0.0064(9) C12A 0.064(2) 0.0371(12) 0.0283(13) -0.0084(10) 0.0076(12) 0.0041(11) C21A 0.0292(11) 0.0335(10) 0.0259(11) 0.0058(9) 0.0022(9) 0.0010(9) C22A 0.053(2) 0.0538(14) 0.0304(13) 0.0096(11) -0.0170(11) -0.0154(12) C31A 0.0240(10) 0.0299(10) 0.0322(12) -0.0005(9) -0.0004(9) -0.0018(8) C32A 0.0423(14) 0.0275(10) 0.0423(14) 0.0075(10) 0.0001(11) 0.0056(9) Mo1B 0.02289(9) 0.02072(8) 0.02016(9) -0.00247(6) 0.00081(7) -0.00036(6) S11B 0.0285(3) 0.0206(2) 0.0228(3) -0.0025(2) 0.0008(2) 0.0007(2) S21B 0.0334(3) 0.0261(2) 0.0257(3) 0.0008(2) -0.0008(2) 0.0081(2) S31B 0.0291(3) 0.0260(2) 0.0219(3) -0.0033(2) 0.0002(2) -0.0022(2) Si1B 0.0324(3) 0.0217(3) 0.0316(3) 0.0024(2) 0.0061(3) -0.0037(2) O1B 0.0403(10) 0.0367(8) 0.0668(13) -0.0197(9) -0.0161(9) -0.0009(7) O2B 0.0559(12) 0.0531(10) 0.0449(11) 0.0220(9) 0.0024(9) -0.0112(9) O3B 0.0352(10) 0.0732(12) 0.0544(12) -0.0252(10) 0.0077(8) 0.0107(9) C1B 0.0303(11) 0.0244(9) 0.0340(12) -0.0050(9) -0.0010(9) 0.0048(8) C2B 0.0281(11) 0.0344(11) 0.0304(12) -0.0007(9) 0.0013(9) -0.0043(9) C3B 0.0307(11) 0.0354(11) 0.0274(12) -0.0088(9) -0.0008(9) -0.0021(9) C4B 0.0423(14) 0.0311(11) 0.0458(15) 0.0018(10) 0.0125(11) -0.0092(10) C11B 0.0268(11) 0.0258(9) 0.0331(12) 0.0013(9) 0.0022(9) -0.0004(8) C12B 0.0477(15) 0.0221(10) 0.060(2) 0.0073(11) 0.0083(13) 0.0055(10) C21B 0.0417(13) 0.0341(11) 0.0318(12) 0.0108(10) 0.0069(10) 0.0029(10) C22B 0.050(2) 0.057(2) 0.0326(13) -0.0009(12) -0.0148(11) 0.0116(12) C31B 0.0413(13) 0.0230(9) 0.0372(13) -0.0045(9) 0.0042(10) -0.0068(9) C32B 0.0485(14) 0.0481(13) 0.0284(13) -0.0139(11) 0.0066(11) -0.0016(11) _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 Mo1A C1A 1.974(2) . ? Mo1A C2A 1.978(2) . ? Mo1A C3A 1.977(2) . ? Mo1A S11A 2.6204(5) . ? Mo1A S21A 2.6229(5) . ? Mo1A S31A 2.6246(5) . ? S11A C12A 1.829(2) . ? S11A C11A 1.829(2) . ? S21A C22A 1.828(2) . ? S21A C21A 1.844(2) . ? S31A C32A 1.835(2) . ? S31A C31A 1.841(2) . ? Si1A C4A 1.889(2) . ? Si1A C21A 1.907(2) . ? Si1A C11A 1.908(2) . ? Si1A C31A 1.909(2) . ? O1A C1A 1.177(3) . ? O2A C2A 1.173(3) . ? O3A C3A 1.178(2) . ? Mo1B C3B 1.966(2) . ? Mo1B C2B 1.971(2) . ? Mo1B C1B 1.978(2) . ? Mo1B S31B 2.5996(5) . ? Mo1B S21B 2.6154(5) . ? Mo1B S11B 2.6251(5) . ? S11B C12B 1.826(2) . ? S11B C11B 1.837(2) . ? S21B C22B 1.829(2) . ? S21B C21B 1.835(2) . ? S31B C32B 1.826(2) . ? S31B C31B 1.830(2) . ? Si1B C4B 1.881(2) . ? Si1B C11B 1.902(2) . ? Si1B C21B 1.908(2) . ? Si1B C31B 1.910(2) . ? O1B C1B 1.178(3) . ? O2B C2B 1.181(3) . ? O3B C3B 1.185(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A Mo1A C2A 88.07(9) . . ? C1A Mo1A C3A 86.60(9) . . ? C2A Mo1A C3A 86.05(8) . . ? C1A Mo1A S11A 93.21(6) . . ? C2A Mo1A S11A 94.82(6) . . ? C3A Mo1A S11A 179.10(6) . . ? C1A Mo1A S21A 91.53(7) . . ? C2A Mo1A S21A 176.94(6) . . ? C3A Mo1A S21A 90.90(6) . . ? S11A Mo1A S21A 88.22(2) . . ? C1A Mo1A S31A 176.09(7) . . ? C2A Mo1A S31A 95.84(6) . . ? C3A Mo1A S31A 93.39(6) . . ? S11A Mo1A S31A 86.75(2) . . ? S21A Mo1A S31A 84.56(2) . . ? C12A S11A C11A 99.73(11) . . ? C12A S11A Mo1A 111.25(9) . . ? C11A S11A Mo1A 111.32(7) . . ? C22A S21A C21A 99.93(11) . . ? C22A S21A Mo1A 106.86(8) . . ? C21A S21A Mo1A 114.40(7) . . ? C32A S31A C31A 99.71(10) . . ? C32A S31A Mo1A 111.66(8) . . ? C31A S31A Mo1A 111.78(7) . . ? C4A Si1A C21A 110.70(11) . . ? C4A Si1A C11A 107.89(10) . . ? C21A Si1A C11A 109.06(10) . . ? C4A Si1A C31A 111.92(10) . . ? C21A Si1A C31A 109.03(9) . . ? C11A Si1A C31A 108.18(10) . . ? O1A C1A Mo1A 179.5(2) . . ? O2A C2A Mo1A 176.1(2) . . ? O3A C3A Mo1A 177.0(2) . . ? S11A C11A Si1A 113.65(10) . . ? S21A C21A Si1A 112.26(11) . . ? S31A C31A Si1A 112.77(11) . . ? C3B Mo1B C2B 87.52(9) . . ? C3B Mo1B C1B 87.02(9) . . ? C2B Mo1B C1B 87.97(9) . . ? C3B Mo1B S31B 94.89(6) . . ? C2B Mo1B S31B 88.58(6) . . ? C1B Mo1B S31B 175.98(6) . . ? C3B Mo1B S21B 90.26(7) . . ? C2B Mo1B S21B 177.67(7) . . ? C1B Mo1B S21B 92.65(6) . . ? S31B Mo1B S21B 90.88(2) . . ? C3B Mo1B S11B 174.33(7) . . ? C2B Mo1B S11B 98.14(7) . . ? C1B Mo1B S11B 93.16(6) . . ? S31B Mo1B S11B 85.29(2) . . ? S21B Mo1B S11B 84.07(2) . . ? C12B S11B C11B 99.82(10) . . ? C12B S11B Mo1B 111.14(9) . . ? C11B S11B Mo1B 111.04(7) . . ? C22B S21B C21B 99.69(12) . . ? C22B S21B Mo1B 109.12(9) . . ? C21B S21B Mo1B 113.15(7) . . ? C32B S31B C31B 101.62(11) . . ? C32B S31B Mo1B 109.75(8) . . ? C31B S31B Mo1B 110.49(8) . . ? C4B Si1B C11B 111.38(10) . . ? C4B Si1B C21B 108.89(11) . . ? C11B Si1B C21B 107.74(10) . . ? C4B Si1B C31B 109.76(10) . . ? C11B Si1B C31B 108.98(10) . . ? C21B Si1B C31B 110.06(11) . . ? O1B C1B Mo1B 176.9(2) . . ? O2B C2B Mo1B 178.6(2) . . ? O3B C3B Mo1B 179.5(2) . . ? S11B C11B Si1B 112.32(11) . . ? S21B C21B Si1B 112.80(12) . . ? S31B C31B Si1B 110.68(10) . . ? _refine_diff_density_max 0.507 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.077 data_drab04 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 O3 S3 Si W' _chemical_formula_weight 494.36 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' 'Si' 'Si' 0.0817 0.0704 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1582(2) _cell_length_b 14.9903(2) _cell_length_c 26.7268(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.6568(8) _cell_angle_gamma 90.00 _cell_volume 3268.30(9) _cell_formula_units_Z 8 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 7821 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 7.522 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 'Siemen's P4/CCD' _diffrn_measurement_method SMART _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15140 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0963 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.47 _reflns_number_total 7476 _reflns_number_gt 5201 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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 'idealized contributions' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00015(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7476 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 0.871 _refine_ls_restrained_S_all 0.871 _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 W1A W 0.41150(3) 0.90116(2) 0.258787(10) 0.02147(9) Uani 1 1 d . . . S11A S 0.6098(2) 1.00996(14) 0.30202(7) 0.0261(4) Uani 1 1 d . . . S21A S 0.4038(2) 1.00802(14) 0.18366(7) 0.0252(4) Uani 1 1 d . . . S31A S 0.6635(2) 0.83476(13) 0.21574(6) 0.0225(4) Uani 1 1 d . . . Si1A Si 0.7745(2) 1.02835(15) 0.19918(7) 0.0244(5) Uani 1 1 d . . . O1A O 0.1047(6) 0.9923(4) 0.3043(2) 0.0418(15) Uani 1 1 d . . . O2A O 0.4075(7) 0.7635(4) 0.3456(2) 0.0360(14) Uani 1 1 d . . . O3A O 0.1670(6) 0.7747(4) 0.2043(2) 0.0374(14) Uani 1 1 d . . . C1A C 0.2203(8) 0.9578(6) 0.2875(3) 0.0285(18) Uani 1 1 d . . . C2A C 0.4120(8) 0.8170(6) 0.3137(3) 0.0263(17) Uani 1 1 d . . . C3A C 0.2594(8) 0.8217(5) 0.2251(3) 0.0243(16) Uani 1 1 d . . . C4A C 0.9461(9) 1.0947(6) 0.1742(3) 0.038(2) Uani 1 1 d . . . H4AA H 0.9861 1.0667 0.1435 0.058 Uiso 1 1 calc R . . H4AB H 1.0350 1.0971 0.1991 0.058 Uiso 1 1 calc R . . H4AC H 0.9081 1.1553 0.1667 0.058 Uiso 1 1 calc R . . C11A C 0.7015(9) 1.0850(5) 0.2579(3) 0.0286(18) Uani 1 1 d . . . H11A H 0.7957 1.1153 0.2742 0.034 Uiso 1 1 calc R . . H11B H 0.6203 1.1314 0.2485 0.034 Uiso 1 1 calc R . . C12A C 0.5023(10) 1.0905(6) 0.3392(3) 0.041(2) Uani 1 1 d . . . H12A H 0.5814 1.1310 0.3552 0.062 Uiso 1 1 calc R . . H12B H 0.4396 1.0595 0.3651 0.062 Uiso 1 1 calc R . . H12C H 0.4272 1.1247 0.3178 0.062 Uiso 1 1 calc R . . C21A C 0.5987(8) 1.0240(6) 0.1536(3) 0.0273(17) Uani 1 1 d . . . H21A H 0.5954 1.0803 0.1343 0.033 Uiso 1 1 calc R . . H21B H 0.6168 0.9745 0.1298 0.033 Uiso 1 1 calc R . . C22A C 0.2925(9) 0.9530(7) 0.1346(3) 0.045(2) Uani 1 1 d . . . H22A H 0.2869 0.9919 0.1052 0.067 Uiso 1 1 calc R . . H22B H 0.1813 0.9397 0.1459 0.067 Uiso 1 1 calc R . . H22C H 0.3483 0.8973 0.1259 0.067 Uiso 1 1 calc R . . C31A C 0.8363(8) 0.9112(5) 0.2160(3) 0.0256(17) Uani 1 1 d . . . H31A H 0.9188 0.8900 0.1919 0.031 Uiso 1 1 calc R . . H31B H 0.8881 0.9113 0.2497 0.031 Uiso 1 1 calc R . . C32A C 0.7493(9) 0.7457(5) 0.2521(3) 0.0316(19) Uani 1 1 d . . . H32A H 0.8451 0.7214 0.2350 0.047 Uiso 1 1 calc R . . H32B H 0.6672 0.6986 0.2561 0.047 Uiso 1 1 calc R . . H32C H 0.7827 0.7682 0.2851 0.047 Uiso 1 1 calc R . . W1B W 1.09006(3) 1.27239(2) 0.489435(11) 0.02069(9) Uani 1 1 d . . . S11B S 0.8406(2) 1.33212(13) 0.53666(6) 0.0217(4) Uani 1 1 d . . . S21B S 1.0860(2) 1.14928(14) 0.55572(7) 0.0248(4) Uani 1 1 d . . . S31B S 0.8808(2) 1.18803(14) 0.43633(6) 0.0234(4) Uani 1 1 d . . . Si1B Si 0.7167(2) 1.13962(15) 0.53357(8) 0.0254(5) Uani 1 1 d . . . O1B O 1.3371(6) 1.3870(4) 0.5509(2) 0.0377(14) Uani 1 1 d . . . O2B O 1.1032(7) 1.4168(4) 0.4062(2) 0.0432(16) Uani 1 1 d . . . O3B O 1.3923(6) 1.1824(5) 0.4409(2) 0.0449(16) Uani 1 1 d . . . C1B C 1.2422(8) 1.3445(5) 0.5290(3) 0.0267(17) Uani 1 1 d . . . C2B C 1.0979(8) 1.3628(5) 0.4372(3) 0.0247(16) Uani 1 1 d . . . C3B C 1.2792(8) 1.2165(5) 0.4585(3) 0.0258(17) Uani 1 1 d . . . C4B C 0.5383(8) 1.0733(6) 0.5540(3) 0.0325(19) Uani 1 1 d . . . H4BA H 0.5000 1.0959 0.5863 0.049 Uiso 1 1 calc R . . H4BB H 0.5705 1.0106 0.5576 0.049 Uiso 1 1 calc R . . H4BC H 0.4499 1.0782 0.5291 0.049 Uiso 1 1 calc R . . C11B C 0.6640(8) 1.2610(5) 0.5275(3) 0.0248(17) Uani 1 1 d . . . H11C H 0.6165 1.2720 0.4938 0.030 Uiso 1 1 calc R . . H11D H 0.5799 1.2764 0.5524 0.030 Uiso 1 1 calc R . . C12B C 0.7643(9) 1.4324(6) 0.5079(3) 0.0348(19) Uani 1 1 d . . . H12D H 0.6694 1.4541 0.5265 0.052 Uiso 1 1 calc R . . H12E H 0.7314 1.4198 0.4732 0.052 Uiso 1 1 calc R . . H12F H 0.8505 1.4780 0.5083 0.052 Uiso 1 1 calc R . . C21B C 0.8842(8) 1.1295(6) 0.5815(3) 0.0308(18) Uani 1 1 d . . . H21C H 0.8646 1.1729 0.6087 0.037 Uiso 1 1 calc R . . H21D H 0.8813 1.0689 0.5962 0.037 Uiso 1 1 calc R . . C22B C 1.1910(9) 1.1882(7) 0.6111(3) 0.044(2) Uani 1 1 d . . . H22D H 1.1898 1.1414 0.6367 0.066 Uiso 1 1 calc R . . H22E H 1.1357 1.2415 0.6238 0.066 Uiso 1 1 calc R . . H22F H 1.3046 1.2030 0.6029 0.066 Uiso 1 1 calc R . . C31B C 0.7902(9) 1.0981(5) 0.4714(3) 0.0288(17) Uani 1 1 d . . . H31C H 0.8723 1.0503 0.4767 0.035 Uiso 1 1 calc R . . H31D H 0.6969 1.0727 0.4521 0.035 Uiso 1 1 calc R . . C32B C 0.9845(9) 1.1290(6) 0.3873(3) 0.034(2) Uani 1 1 d . . . H32D H 0.9039 1.0965 0.3669 0.051 Uiso 1 1 calc R . . H32E H 1.0627 1.0867 0.4021 0.051 Uiso 1 1 calc R . . H32F H 1.0432 1.1717 0.3663 0.051 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 W1A 0.02126(14) 0.02325(18) 0.01989(15) 0.00023(13) 0.00038(10) 0.00012(12) S11A 0.0325(9) 0.0241(11) 0.0216(9) -0.0016(8) -0.0012(7) -0.0001(8) S21A 0.0216(8) 0.0291(12) 0.0248(9) 0.0027(8) -0.0012(7) 0.0022(8) S31A 0.0232(8) 0.0215(10) 0.0227(9) -0.0007(8) -0.0008(6) 0.0005(8) Si1A 0.0224(9) 0.0240(12) 0.0267(11) 0.0015(9) 0.0022(8) -0.0036(9) O1A 0.034(3) 0.055(5) 0.037(3) -0.012(3) 0.003(2) 0.012(3) O2A 0.045(3) 0.036(4) 0.028(3) 0.007(3) 0.003(2) 0.000(3) O3A 0.034(3) 0.026(3) 0.052(4) -0.001(3) -0.017(3) 0.001(3) C1A 0.024(4) 0.039(5) 0.022(4) 0.005(4) -0.003(3) -0.008(4) C2A 0.027(4) 0.031(5) 0.022(4) -0.002(4) 0.001(3) 0.001(3) C3A 0.023(3) 0.021(4) 0.028(4) -0.001(3) -0.002(3) 0.001(3) C4A 0.031(4) 0.046(6) 0.038(5) 0.004(4) 0.003(3) -0.002(4) C11A 0.033(4) 0.026(5) 0.026(4) 0.001(3) 0.000(3) -0.009(3) C12A 0.058(5) 0.035(6) 0.031(5) 0.000(4) 0.008(4) 0.013(4) C21A 0.029(4) 0.028(5) 0.025(4) 0.004(3) 0.000(3) -0.001(3) C22A 0.044(5) 0.057(7) 0.032(5) 0.009(5) -0.014(4) -0.010(5) C31A 0.025(4) 0.020(4) 0.031(4) -0.001(3) -0.003(3) -0.004(3) C32A 0.041(5) 0.025(5) 0.029(4) 0.005(3) -0.004(3) 0.002(3) W1B 0.02043(14) 0.02140(17) 0.02024(15) -0.00182(14) 0.00049(10) -0.00029(13) S11B 0.0239(8) 0.0193(10) 0.0219(9) -0.0015(8) 0.0010(6) 0.0011(7) S21B 0.0257(9) 0.0248(11) 0.0237(9) 0.0002(8) -0.0012(7) 0.0055(8) S31B 0.0233(8) 0.0260(11) 0.0209(9) -0.0014(8) -0.0003(7) -0.0021(8) Si1B 0.0258(10) 0.0217(12) 0.0286(11) 0.0016(10) 0.0033(8) -0.0023(9) O1B 0.034(3) 0.024(3) 0.055(4) -0.011(3) -0.011(3) -0.002(3) O2B 0.044(3) 0.039(4) 0.047(4) 0.020(3) -0.002(3) -0.008(3) O3B 0.031(3) 0.060(5) 0.044(3) -0.016(3) 0.011(3) 0.008(3) C1B 0.025(4) 0.025(5) 0.030(4) -0.006(4) -0.004(3) 0.007(3) C2B 0.024(3) 0.025(4) 0.025(4) -0.001(4) -0.001(3) -0.008(3) C3B 0.029(4) 0.022(5) 0.027(4) -0.006(3) 0.001(3) -0.008(3) C4B 0.031(4) 0.029(5) 0.037(5) -0.004(4) 0.008(3) -0.006(4) C11B 0.024(4) 0.022(4) 0.028(4) 0.006(3) 0.005(3) 0.004(3) C12B 0.037(4) 0.022(5) 0.046(5) -0.001(4) 0.005(4) 0.007(4) C21B 0.030(4) 0.027(5) 0.035(4) 0.015(4) 0.005(3) -0.004(3) C22B 0.040(4) 0.058(7) 0.033(5) -0.002(5) -0.011(3) 0.012(5) C31B 0.032(4) 0.017(4) 0.037(4) -0.004(4) 0.005(3) -0.006(3) C32B 0.041(4) 0.043(6) 0.019(4) -0.010(4) 0.001(3) -0.001(4) _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 W1A C3A 1.935(7) . ? W1A C2A 1.935(8) . ? W1A C1A 1.942(8) . ? W1A S11A 2.5630(19) . ? W1A S31A 2.5679(17) . ? W1A S21A 2.5688(19) . ? S11A C12A 1.799(8) . ? S11A C11A 1.800(7) . ? S21A C22A 1.787(8) . ? S21A C21A 1.805(7) . ? S31A C32A 1.789(7) . ? S31A C31A 1.817(7) . ? Si1A C4A 1.848(8) . ? Si1A C21A 1.871(7) . ? Si1A C31A 1.880(8) . ? Si1A C11A 1.886(7) . ? O1A C1A 1.170(8) . ? O2A C2A 1.171(9) . ? O3A C3A 1.168(8) . ? W1B C2B 1.948(8) . ? W1B C3B 1.948(7) . ? W1B C1B 1.949(7) . ? W1B S31B 2.5441(17) . ? W1B S21B 2.5587(19) . ? W1B S11B 2.5679(17) . ? S11B C12B 1.797(8) . ? S11B C11B 1.807(7) . ? S21B C22B 1.799(8) . ? S21B C21B 1.816(7) . ? S31B C32B 1.800(7) . ? S31B C31B 1.805(8) . ? Si1B C4B 1.851(7) . ? Si1B C21B 1.868(7) . ? Si1B C11B 1.876(8) . ? Si1B C31B 1.880(7) . ? O1B C1B 1.157(8) . ? O2B C2B 1.159(9) . ? O3B C3B 1.161(8) . ? 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 C3A W1A C2A 87.0(3) . . ? C3A W1A C1A 86.5(3) . . ? C2A W1A C1A 88.8(3) . . ? C3A W1A S11A 178.4(2) . . ? C2A W1A S11A 94.4(2) . . ? C1A W1A S11A 92.8(2) . . ? C3A W1A S31A 93.7(2) . . ? C2A W1A S31A 95.3(2) . . ? C1A W1A S31A 175.9(2) . . ? S11A W1A S31A 86.81(6) . . ? C3A W1A S21A 90.6(2) . . ? C2A W1A S21A 177.5(2) . . ? C1A W1A S21A 91.4(2) . . ? S11A W1A S21A 88.01(6) . . ? S31A W1A S21A 84.49(6) . . ? C12A S11A C11A 98.8(4) . . ? C12A S11A W1A 111.5(3) . . ? C11A S11A W1A 111.5(2) . . ? C22A S21A C21A 100.2(4) . . ? C22A S21A W1A 107.0(3) . . ? C21A S21A W1A 114.6(2) . . ? C32A S31A C31A 99.8(3) . . ? C32A S31A W1A 110.9(3) . . ? C31A S31A W1A 112.3(2) . . ? C4A Si1A C21A 111.2(3) . . ? C4A Si1A C31A 112.7(4) . . ? C21A Si1A C31A 108.9(3) . . ? C4A Si1A C11A 107.8(4) . . ? C21A Si1A C11A 108.0(3) . . ? C31A Si1A C11A 107.9(3) . . ? O1A C1A W1A 179.3(7) . . ? O2A C2A W1A 176.8(7) . . ? O3A C3A W1A 179.1(7) . . ? S11A C11A Si1A 113.7(4) . . ? S21A C21A Si1A 112.8(4) . . ? S31A C31A Si1A 112.5(4) . . ? C2B W1B C3B 87.8(3) . . ? C2B W1B C1B 88.7(3) . . ? C3B W1B C1B 88.1(3) . . ? C2B W1B S31B 88.5(2) . . ? C3B W1B S31B 94.5(2) . . ? C1B W1B S31B 176.1(2) . . ? C2B W1B S21B 177.6(2) . . ? C3B W1B S21B 90.0(2) . . ? C1B W1B S21B 92.1(2) . . ? S31B W1B S21B 90.79(6) . . ? C2B W1B S11B 98.2(2) . . ? C3B W1B S11B 173.9(2) . . ? C1B W1B S11B 92.5(2) . . ? S31B W1B S11B 85.25(6) . . ? S21B W1B S11B 83.94(6) . . ? C12B S11B C11B 99.4(4) . . ? C12B S11B W1B 110.7(3) . . ? C11B S11B W1B 111.2(2) . . ? C22B S21B C21B 99.6(4) . . ? C22B S21B W1B 109.0(3) . . ? C21B S21B W1B 113.5(2) . . ? C32B S31B C31B 102.1(4) . . ? C32B S31B W1B 109.4(3) . . ? C31B S31B W1B 111.0(3) . . ? C4B Si1B C21B 109.0(3) . . ? C4B Si1B C11B 111.5(3) . . ? C21B Si1B C11B 107.7(4) . . ? C4B Si1B C31B 110.1(3) . . ? C21B Si1B C31B 109.9(3) . . ? C11B Si1B C31B 108.6(3) . . ? O1B C1B W1B 177.2(7) . . ? O2B C2B W1B 179.6(7) . . ? O3B C3B W1B 178.8(7) . . ? S11B C11B Si1B 112.3(4) . . ? S21B C21B Si1B 112.7(4) . . ? S31B C31B Si1B 110.4(4) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 28.47 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 1.201 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.243 data_drab06 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 Cr O3 S3 Si' _chemical_formula_weight 362.51 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1658(2) _cell_length_b 15.0563(2) _cell_length_c 26.5791(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.3653(6) _cell_angle_gamma 90.00 _cell_volume 3267.74(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.153 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12246 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5611 _reflns_number_gt 4670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5611 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1503 _refine_ls_goodness_of_fit_ref 1.255 _refine_ls_restrained_S_all 1.255 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1A Cr 0.41569(8) 0.77226(5) 0.48832(2) 0.0203(2) Uani 1 1 d . . . Cr1B Cr 0.07883(8) 0.40875(5) 0.25767(2) 0.0219(2) Uani 1 1 d . . . Si1A Si 0.77867(14) 0.63666(9) 0.53256(4) 0.0252(3) Uani 1 1 d . . . S11A S 0.40916(13) 0.65107(8) 0.55010(4) 0.0250(3) Uani 1 1 d . . . S21A S 0.61144(13) 0.69355(8) 0.43573(4) 0.0238(3) Uani 1 1 d . . . S31A S 0.65431(12) 0.82843(7) 0.53573(4) 0.0222(3) Uani 1 1 d . . . O1A O 0.1157(4) 0.6942(3) 0.43965(13) 0.0476(10) Uani 1 1 d . . . O2A O 0.1767(4) 0.8844(2) 0.54573(14) 0.0398(9) Uani 1 1 d . . . O3A O 0.4021(4) 0.9143(3) 0.40913(13) 0.0438(9) Uani 1 1 d . . . C1A C 0.2333(6) 0.7244(3) 0.45823(17) 0.0303(11) Uani 1 1 d . . . C2A C 0.2747(5) 0.8411(3) 0.52468(17) 0.0276(10) Uani 1 1 d . . . C3A C 0.4127(5) 0.8581(3) 0.44001(17) 0.0289(10) Uani 1 1 d . . . C4A C 0.9543(6) 0.5676(3) 0.55346(18) 0.0338(11) Uani 1 1 d . . . H4AA H 0.9912 0.5874 0.5868 0.051 Uiso 1 1 calc R . . H4AB H 1.0441 0.5737 0.5294 0.051 Uiso 1 1 calc R . . H4AC H 0.9204 0.5053 0.5552 0.051 Uiso 1 1 calc R . . C11A C 0.6064(5) 0.6259(4) 0.57884(17) 0.0330(11) Uani 1 1 d . . . H11A H 0.6045 0.5645 0.5923 0.040 Uiso 1 1 calc R . . H11B H 0.6260 0.6668 0.6074 0.040 Uiso 1 1 calc R . . C12A C 0.3008(6) 0.6871(4) 0.60546(18) 0.0382(12) Uani 1 1 d . . . H12A H 0.2984 0.6387 0.6301 0.057 Uiso 1 1 calc R . . H12B H 0.1885 0.7036 0.5962 0.057 Uiso 1 1 calc R . . H12C H 0.3567 0.7386 0.6202 0.057 Uiso 1 1 calc R . . C21A C 0.7051(6) 0.5999(3) 0.46817(16) 0.0291(10) Uani 1 1 d . . . H21A H 0.7987 0.5773 0.4484 0.035 Uiso 1 1 calc R . . H21B H 0.6243 0.5513 0.4717 0.035 Uiso 1 1 calc R . . C22A C 0.5062(6) 0.6382(4) 0.38443(17) 0.0360(12) Uani 1 1 d . . . H22A H 0.5861 0.6068 0.3636 0.054 Uiso 1 1 calc R . . H22B H 0.4481 0.6822 0.3639 0.054 Uiso 1 1 calc R . . H22C H 0.4275 0.5955 0.3980 0.054 Uiso 1 1 calc R . . C31A C 0.8342(5) 0.7572(3) 0.52852(17) 0.0262(10) Uani 1 1 d . . . H31A H 0.9152 0.7715 0.5552 0.031 Uiso 1 1 calc R . . H31B H 0.8856 0.7692 0.4956 0.031 Uiso 1 1 calc R . . C32A C 0.7320(6) 0.9293(3) 0.50734(19) 0.0351(11) Uani 1 1 d . . . H32A H 0.8267 0.9506 0.5267 0.053 Uiso 1 1 calc R . . H32B H 0.6462 0.9748 0.5073 0.053 Uiso 1 1 calc R . . H32C H 0.7652 0.9171 0.4727 0.053 Uiso 1 1 calc R . . Si1B Si -0.28240(14) 0.53256(9) 0.19839(4) 0.0251(3) Uani 1 1 d . . . S11B S -0.10692(14) 0.51182(8) 0.30080(4) 0.0268(3) Uani 1 1 d . . . S21B S -0.16235(12) 0.34152(7) 0.21653(4) 0.0225(3) Uani 1 1 d . . . S31B S 0.08812(13) 0.51043(8) 0.18485(4) 0.0245(3) Uani 1 1 d . . . O1B O 0.0958(4) 0.2773(2) 0.34265(12) 0.0401(9) Uani 1 1 d . . . O2B O 0.3811(4) 0.4912(3) 0.30253(14) 0.0468(10) Uani 1 1 d . . . O3B O 0.3173(4) 0.2835(2) 0.20935(15) 0.0425(9) Uani 1 1 d . . . C1B C 0.0830(5) 0.3297(3) 0.31019(17) 0.0277(10) Uani 1 1 d . . . C2B C 0.2624(5) 0.4615(3) 0.28431(17) 0.0300(11) Uani 1 1 d . . . C3B C 0.2197(5) 0.3314(3) 0.22666(18) 0.0303(10) Uani 1 1 d . . . C4B C -0.4572(6) 0.5980(4) 0.17241(19) 0.0367(12) Uani 1 1 d . . . H4BA H -0.5469 0.5985 0.1967 0.055 Uiso 1 1 calc R . . H4BB H -0.4951 0.5709 0.1409 0.055 Uiso 1 1 calc R . . H4BC H -0.4215 0.6591 0.1659 0.055 Uiso 1 1 calc R . . C11B C -0.2091(6) 0.5883(3) 0.25783(17) 0.0317(11) Uani 1 1 d . . . H11C H -0.1324 0.6366 0.2490 0.038 Uiso 1 1 calc R . . H11D H -0.3040 0.6153 0.2751 0.038 Uiso 1 1 calc R . . C12B C 0.0054(7) 0.5917(4) 0.33816(18) 0.0405(13) Uani 1 1 d . . . H12D H -0.0717 0.6318 0.3549 0.061 Uiso 1 1 calc R . . H12E H 0.0778 0.6262 0.3163 0.061 Uiso 1 1 calc R . . H12F H 0.0711 0.5605 0.3636 0.061 Uiso 1 1 calc R . . C21B C -0.3410(5) 0.4147(3) 0.21478(17) 0.0272(10) Uani 1 1 d . . . H21C H -0.3950 0.4140 0.2480 0.033 Uiso 1 1 calc R . . H21D H -0.4205 0.3922 0.1895 0.033 Uiso 1 1 calc R . . C22B C -0.2467(6) 0.2519(3) 0.25429(17) 0.0318(11) Uani 1 1 d . . . H22D H -0.3422 0.2266 0.2370 0.048 Uiso 1 1 calc R . . H22E H -0.2798 0.2752 0.2871 0.048 Uiso 1 1 calc R . . H22F H -0.1635 0.2057 0.2591 0.048 Uiso 1 1 calc R . . C31B C -0.1058(5) 0.5291(3) 0.15304(16) 0.0274(10) Uani 1 1 d . . . H31C H -0.1247 0.4811 0.1282 0.033 Uiso 1 1 calc R . . H31D H -0.1009 0.5861 0.1345 0.033 Uiso 1 1 calc R . . C32B C 0.1969(6) 0.4548(4) 0.13478(18) 0.0382(12) Uani 1 1 d . . . H32D H 0.2023 0.4939 0.1054 0.057 Uiso 1 1 calc R . . H32E H 0.1391 0.4000 0.1257 0.057 Uiso 1 1 calc R . . H32F H 0.3081 0.4404 0.1462 0.057 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 Cr1A 0.0195(4) 0.0213(4) 0.0200(3) -0.0020(3) -0.0005(3) 0.0005(3) Cr1B 0.0218(4) 0.0241(4) 0.0198(4) 0.0006(3) 0.0000(3) -0.0004(3) Si1A 0.0262(6) 0.0213(7) 0.0282(6) 0.0022(5) -0.0038(5) 0.0029(5) S11A 0.0263(6) 0.0260(6) 0.0228(5) -0.0005(4) 0.0013(4) -0.0063(5) S21A 0.0246(5) 0.0266(6) 0.0202(5) -0.0019(4) 0.0005(4) 0.0012(4) S31A 0.0237(5) 0.0220(6) 0.0210(5) -0.0024(4) 0.0005(4) -0.0001(4) O1A 0.0298(19) 0.069(3) 0.044(2) -0.024(2) -0.0061(16) -0.0104(19) O2A 0.0323(18) 0.032(2) 0.055(2) -0.0155(17) 0.0116(16) -0.0023(16) O3A 0.049(2) 0.045(2) 0.037(2) 0.0131(18) -0.0013(16) 0.0111(18) C1A 0.034(3) 0.030(3) 0.027(2) -0.006(2) 0.004(2) 0.000(2) C2A 0.028(2) 0.023(3) 0.032(2) -0.0024(19) 0.0053(19) -0.0014(19) C3A 0.021(2) 0.037(3) 0.029(2) -0.001(2) -0.0039(18) 0.004(2) C4A 0.033(2) 0.028(3) 0.041(3) -0.002(2) -0.005(2) 0.005(2) C11A 0.030(2) 0.037(3) 0.032(2) 0.007(2) -0.0011(19) -0.006(2) C12A 0.038(3) 0.044(3) 0.033(3) -0.001(2) 0.016(2) -0.008(2) C21A 0.034(2) 0.021(2) 0.032(2) -0.0058(19) -0.0029(19) 0.005(2) C22A 0.036(3) 0.049(3) 0.023(2) -0.008(2) -0.0033(19) 0.003(2) C31A 0.023(2) 0.022(2) 0.034(2) -0.0001(19) -0.0044(18) -0.0006(18) C32A 0.039(3) 0.022(3) 0.045(3) 0.001(2) -0.005(2) -0.005(2) Si1B 0.0237(6) 0.0250(7) 0.0267(6) 0.0021(5) 0.0003(5) 0.0034(5) S11B 0.0332(6) 0.0274(6) 0.0197(5) -0.0023(4) 0.0032(4) -0.0008(5) S21B 0.0238(5) 0.0230(6) 0.0208(5) -0.0007(4) 0.0017(4) -0.0007(4) S31B 0.0233(5) 0.0256(6) 0.0246(5) 0.0012(4) 0.0028(4) -0.0027(4) O1B 0.048(2) 0.039(2) 0.0328(18) 0.0158(16) -0.0075(15) 0.0036(17) O2B 0.0297(19) 0.063(3) 0.048(2) -0.0118(19) -0.0060(16) -0.0089(18) O3B 0.0313(18) 0.024(2) 0.072(3) 0.0014(17) 0.0183(17) 0.0059(15) C1B 0.023(2) 0.029(3) 0.031(2) -0.006(2) -0.0006(18) -0.0035(19) C2B 0.026(2) 0.036(3) 0.028(2) -0.007(2) 0.0041(18) -0.003(2) C3B 0.029(2) 0.025(3) 0.037(3) 0.008(2) -0.0008(19) -0.003(2) C4B 0.030(2) 0.040(3) 0.040(3) 0.001(2) 0.000(2) 0.013(2) C11B 0.041(3) 0.027(3) 0.028(2) -0.0001(19) 0.000(2) 0.007(2) C12B 0.058(3) 0.037(3) 0.026(2) -0.005(2) -0.006(2) -0.005(3) C21B 0.022(2) 0.029(3) 0.031(2) 0.0036(19) 0.0006(18) -0.0044(19) C22B 0.036(3) 0.025(3) 0.035(2) 0.008(2) 0.002(2) -0.003(2) C31B 0.024(2) 0.034(3) 0.024(2) 0.0050(19) -0.0007(17) -0.0030(19) C32B 0.042(3) 0.041(3) 0.031(3) 0.006(2) 0.014(2) 0.013(2) _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 Cr1A C3A 1.822(5) . ? Cr1A C2A 1.830(4) . ? Cr1A C1A 1.833(5) . ? Cr1A S21A 2.4376(12) . ? Cr1A S11A 2.4555(13) . ? Cr1A S31A 2.4634(12) . ? Cr1B C3B 1.836(5) . ? Cr1B C2B 1.834(5) . ? Cr1B C1B 1.834(5) . ? Cr1B S11B 2.4587(13) . ? Cr1B S21B 2.4641(12) . ? Cr1B S31B 2.4694(13) . ? Si1A C4A 1.853(5) . ? Si1A C31A 1.874(5) . ? Si1A C11A 1.881(5) . ? Si1A C21A 1.893(5) . ? S11A C12A 1.805(4) . ? S11A C11A 1.818(5) . ? S21A C22A 1.810(5) . ? S21A C21A 1.819(5) . ? S31A C32A 1.812(5) . ? S31A C31A 1.830(4) . ? O1A C1A 1.169(6) . ? O2A C2A 1.176(5) . ? O3A C3A 1.182(6) . ? Si1B C4B 1.864(5) . ? Si1B C11B 1.883(5) . ? Si1B C31B 1.886(4) . ? Si1B C21B 1.889(5) . ? S11B C12B 1.807(5) . ? S11B C11B 1.820(5) . ? S21B C22B 1.819(5) . ? S21B C21B 1.829(5) . ? S31B C32B 1.810(5) . ? S31B C31B 1.812(4) . ? O1B C1B 1.173(6) . ? O2B C2B 1.170(6) . ? O3B C3B 1.172(6) . ? 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 C3A Cr1A C2A 88.0(2) . . ? C3A Cr1A C1A 87.9(2) . . ? C2A Cr1A C1A 86.6(2) . . ? C3A Cr1A S21A 86.94(14) . . ? C2A Cr1A S21A 174.48(15) . . ? C1A Cr1A S21A 95.33(14) . . ? C3A Cr1A S11A 176.54(15) . . ? C2A Cr1A S11A 92.95(15) . . ? C1A Cr1A S11A 88.79(16) . . ? S21A Cr1A S11A 92.25(4) . . ? C3A Cr1A S31A 97.12(15) . . ? C2A Cr1A S31A 91.93(15) . . ? C1A Cr1A S31A 174.69(15) . . ? S21A Cr1A S31A 86.60(4) . . ? S11A Cr1A S31A 86.19(4) . . ? C3B Cr1B C2B 86.3(2) . . ? C3B Cr1B C1B 85.5(2) . . ? C2B Cr1B C1B 88.6(2) . . ? C3B Cr1B S11B 178.86(15) . . ? C2B Cr1B S11B 92.97(15) . . ? C1B Cr1B S11B 93.61(14) . . ? C3B Cr1B S21B 92.36(15) . . ? C2B Cr1B S21B 176.30(15) . . ? C1B Cr1B S21B 94.71(14) . . ? S11B Cr1B S21B 88.42(4) . . ? C3B Cr1B S31B 91.09(15) . . ? C2B Cr1B S31B 90.28(16) . . ? C1B Cr1B S31B 176.49(14) . . ? S11B Cr1B S31B 89.79(4) . . ? S21B Cr1B S31B 86.29(4) . . ? C4A Si1A C31A 111.9(2) . . ? C4A Si1A C11A 109.6(2) . . ? C31A Si1A C11A 107.7(2) . . ? C4A Si1A C21A 110.3(2) . . ? C31A Si1A C21A 107.9(2) . . ? C11A Si1A C21A 109.4(2) . . ? C12A S11A C11A 99.1(2) . . ? C12A S11A Cr1A 109.54(19) . . ? C11A S11A Cr1A 114.40(16) . . ? C22A S21A C21A 101.3(2) . . ? C22A S21A Cr1A 110.25(16) . . ? C21A S21A Cr1A 112.35(15) . . ? C32A S31A C31A 99.4(2) . . ? C32A S31A Cr1A 110.66(17) . . ? C31A S31A Cr1A 112.23(15) . . ? O1A C1A Cr1A 179.0(4) . . ? O2A C2A Cr1A 175.8(4) . . ? O3A C3A Cr1A 176.5(4) . . ? S11A C11A Si1A 111.8(2) . . ? S21A C21A Si1A 109.4(2) . . ? S31A C31A Si1A 111.5(2) . . ? C4B Si1B C11B 108.3(2) . . ? C4B Si1B C31B 111.4(2) . . ? C11B Si1B C31B 108.0(2) . . ? C4B Si1B C21B 112.8(2) . . ? C11B Si1B C21B 107.7(2) . . ? C31B Si1B C21B 108.5(2) . . ? C12B S11B C11B 98.8(2) . . ? C12B S11B Cr1B 111.35(18) . . ? C11B S11B Cr1B 112.84(15) . . ? C22B S21B C21B 99.0(2) . . ? C22B S21B Cr1B 111.34(17) . . ? C21B S21B Cr1B 113.52(15) . . ? C32B S31B C31B 99.2(2) . . ? C32B S31B Cr1B 107.89(17) . . ? C31B S31B Cr1B 115.53(15) . . ? O1B C1B Cr1B 175.4(4) . . ? O2B C2B Cr1B 176.6(5) . . ? O3B C3B Cr1B 175.4(4) . . ? S11B C11B Si1B 112.8(3) . . ? S21B C21B Si1B 111.6(2) . . ? S31B C31B Si1B 112.0(2) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.553 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.101