Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Maxence Vennat' ; Laboratoire des Systemes Interfaciaux a l'Echelle Nanometrique Universite Pierre et Marie Curie/CNRS,case 196 4, place Jussieu, 75252 Paris cedex 05, France ; 'Jean-Marie Bregeault' ; Laboratoire des Systemes Interfaciaux a l'Echelle Nanometrique Universite Pierre et Marie Curie/CNRS,case 196 4, place Jussieu, 75252 Paris cedex 05, France ; 'Patrick Herson' ;Laboratoire de Chimie Inorganique et Materiaux Moleculaires Universite Pierre et Marie Curie, case 42, 4 place Jussieu 75252 Paris cedex 05, France ; _publ_contac_author_name 'Professor Jean-Marie Bregeault' _publ_contact_author_address ; Laboratoire des Systemes Interfaciaux a l'Echelle Nanometrique Universite Pierre et Marie Curie/CNRS,case 196 4, place Jussieu, 75252 Paris cedex 05, France ; _publ_contact_author_email bregeaul@ccr.jussieu.fr _publ_contact_author_fax 33(0)1.44.27.55.36 _publ_contact_author_phone 33(0)1.44.27.36.27 _publ_contact_author_name 'J.M. Bregeault' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_section_title ; Mixed crystals containing the dioxo complex [{PPh3SiO}2VO2]- and novel pentacoordinated oxoperoxo complex [{PPh3SiO}2VO(O2)]-:X-ray crystal structure and assessment as oxidation catalysts ; data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 222221' _audit_creation_date 03-14-10 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 22.362(8) _cell_angle_alpha 90 _cell_length_b 11.270(6) _cell_angle_beta 119.00(2) _cell_length_c 23.069(6) _cell_angle_gamma 90 _cell_volume 5085(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'V ' 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780 1.2199 International_Tables_Vol_IV_Table_2.2B 'Si ' 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C60 H50 O4.43 P1 Si2 V1 ' _chemical_formula_moiety ' (C36 H30 O4.43 Si2 V1)-, (C24 H30 P1)+ ' _chemical_compound_source ; ? ; _chemical_formula_weight 980.02 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 13.2 _cell_measurement_temperature 295 _exptl_crystal_description ' stick ' _exptl_crystal_colour ' dark violet ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2045.732 _exptl_absorpt_coefficient_mu 0.322 # Sheldrick geometric definitions 0.95 0.97 _diffrn_measurement_device_type ; Enraf-Nonius CAD4 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; Cad4 Express, (Enraf-Nonius, 1989) ; _computing_data_reduction ; RC93 (Watkin, Prout & Lilley, 1994) ; _computing_cell_refinement ; Cad4 Express, (Enraf-Nonius, 1989) ; _computing_structure_solution ; SHELXS 86 (Sheldrick, 1986) ; _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; Azimutal absorption correction (North et al, 1968) ; _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 3600 _diffrn_standards_number 2 _diffrn_standards_decay_% 6.46 _diffrn_ambient_temperature 295 _diffrn_ambient_pressure 1 _diffrn_reflns_number 9714 _reflns_number_total 8949 _diffrn_reflns_av_R_equivalents 0.06 # Number of reflections with Friedels Law is 8949 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8920 _diffrn_reflns_theta_min 1.041 _diffrn_reflns_theta_max 24.972 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.972 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -26 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _refine_diff_density_min -0.31 _refine_diff_density_max 0.93 _refine_ls_number_reflns 5459 _refine_ls_number_parameters 632 #_refine_ls_R_factor_ref 0.0512 _refine_ls_wR_factor_ref 0.0636 _refine_ls_goodness_of_fit_ref 1.0150 #_reflns_number_all 8949 _refine_ls_R_factor_all 0.0941 _refine_ls_wR_factor_all 0.0657 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5459 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_gt 0.0636 _refine_ls_shift/su_max 0.000463 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 11.0 3.50 8.99 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Enraf-Nonius, (1989) Cad4 Express. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_attached_hydrogens V1 V 0.82910(3) 0.59172(5) 0.05771(3) 0.0365 1.0000 Uani . Si1 Si 0.94210(5) 0.80662(9) 0.13776(5) 0.0412 1.0000 Uani . Si2 Si 0.71010(5) 0.59331(9) 0.10192(5) 0.0413 1.0000 Uani . P1 P 0.58884(4) 0.15751(8) -0.25441(4) 0.0389 1.0000 Uani . O11 O 0.90456(12) 0.6829(2) 0.10534(12) 0.0499 1.0000 Uani . O12 O 0.78438(12) 0.5962(2) 0.10630(12) 0.0483 1.0000 Uani . C101 C 0.96806(18) 0.8049(3) 0.22857(17) 0.0465 1.0000 Uani . C102 C 1.0183(2) 0.8797(4) 0.2739(2) 0.0638 1.0000 Uani . C103 C 1.0347(3) 0.8796(5) 0.3404(2) 0.0803 1.0000 Uani . C104 C 1.0029(3) 0.8025(5) 0.3617(2) 0.0810 1.0000 Uani . C105 C 0.9536(3) 0.7256(5) 0.3185(2) 0.0773 1.0000 Uani . C106 C 0.9362(2) 0.7288(4) 0.2517(2) 0.0581 1.0000 Uani . C107 C 1.02111(18) 0.8207(3) 0.12898(17) 0.0463 1.0000 Uani . C108 C 1.0711(2) 0.7342(4) 0.1553(2) 0.0615 1.0000 Uani . C109 C 1.1281(2) 0.7393(5) 0.1470(3) 0.0819 1.0000 Uani . C110 C 1.1363(2) 0.8300(6) 0.1124(3) 0.0850 1.0000 Uani . C111 C 1.0886(3) 0.9181(5) 0.0872(3) 0.0819 1.0000 Uani . C112 C 1.0310(2) 0.9135(4) 0.0958(2) 0.0629 1.0000 Uani . C113 C 0.88680(18) 0.9386(3) 0.09626(18) 0.0457 1.0000 Uani . C114 C 0.8371(2) 0.9366(4) 0.0306(2) 0.0610 1.0000 Uani . C115 C 0.8006(3) 1.0374(4) -0.0008(2) 0.0770 1.0000 Uani . C116 C 0.8136(2) 1.1431(4) 0.0324(2) 0.0633 1.0000 Uani . C117 C 0.8614(3) 1.1471(4) 0.0967(3) 0.0750 1.0000 Uani . C118 C 0.8972(2) 1.0455(4) 0.1290(2) 0.0723 1.0000 Uani . C221 C 0.65810(19) 0.4686(3) 0.04652(18) 0.0485 1.0000 Uani . C222 C 0.6886(2) 0.3612(4) 0.0483(3) 0.0714 1.0000 Uani . C223 C 0.6511(3) 0.2662(5) 0.0096(3) 0.0877 1.0000 Uani . C224 C 0.5825(3) 0.2792(5) -0.0325(3) 0.0841 1.0000 Uani . C225 C 0.5522(3) 0.3840(6) -0.0359(3) 0.0965 1.0000 Uani . C226 C 0.5892(2) 0.4785(4) 0.0031(2) 0.0732 1.0000 Uani . C227 C 0.66406(18) 0.7380(3) 0.07138(18) 0.0479 1.0000 Uani . C228 C 0.6711(3) 0.8092(4) 0.0267(3) 0.0769 1.0000 Uani . C229 C 0.6362(3) 0.9154(5) 0.0051(3) 0.0952 1.0000 Uani . C230 C 0.5948(3) 0.9530(4) 0.0286(3) 0.0782 1.0000 Uani . C231 C 0.5870(3) 0.8869(4) 0.0735(3) 0.0794 1.0000 Uani . C232 C 0.6215(2) 0.7796(4) 0.0947(2) 0.0662 1.0000 Uani . C233 C 0.72200(18) 0.5662(3) 0.18709(18) 0.0473 1.0000 Uani . C234 C 0.7670(2) 0.6349(5) 0.2398(2) 0.0676 1.0000 Uani . C235 C 0.7759(3) 0.6194(6) 0.3035(2) 0.0902 1.0000 Uani . C236 C 0.7384(3) 0.5371(6) 0.3147(3) 0.0868 1.0000 Uani . C237 C 0.6919(4) 0.4706(5) 0.2632(3) 0.0913 1.0000 Uani . C238 C 0.6842(3) 0.4840(4) 0.2005(2) 0.0718 1.0000 Uani . C301 C 0.51122(17) 0.1687(3) -0.24988(16) 0.0426 1.0000 Uani . C302 C 0.5006(2) 0.2666(4) -0.21938(19) 0.0561 1.0000 Uani . C303 C 0.4396(2) 0.2768(4) -0.2182(2) 0.0690 1.0000 Uani . C304 C 0.3901(2) 0.1903(5) -0.2469(2) 0.0686 1.0000 Uani . C305 C 0.4004(2) 0.0935(4) -0.2774(2) 0.0635 1.0000 Uani . C306 C 0.4608(2) 0.0835(4) -0.2787(2) 0.0563 1.0000 Uani . C307 C 0.63618(18) 0.0287(3) -0.21020(16) 0.0426 1.0000 Uani . C308 C 0.6124(2) -0.0504(4) -0.1818(2) 0.0678 1.0000 Uani . C309 C 0.6523(3) -0.1478(5) -0.1470(3) 0.0860 1.0000 Uani . C310 C 0.7142(3) -0.1650(4) -0.1424(2) 0.0727 1.0000 Uani . C311 C 0.7386(3) -0.0863(5) -0.1702(3) 0.0863 1.0000 Uani . C312 C 0.7010(2) 0.0113(4) -0.2034(2) 0.0710 1.0000 Uani . C313 C 0.64050(17) 0.2858(3) -0.21658(17) 0.0420 1.0000 Uani . C314 C 0.6812(2) 0.2900(4) -0.14778(19) 0.0598 1.0000 Uani . C315 C 0.7169(3) 0.3917(4) -0.1183(2) 0.0723 1.0000 Uani . C316 C 0.7130(2) 0.4880(4) -0.1559(2) 0.0685 1.0000 Uani . C317 C 0.6729(2) 0.4848(4) -0.2234(2) 0.0665 1.0000 Uani . C318 C 0.6367(2) 0.3837(4) -0.2544(2) 0.0548 1.0000 Uani . C319 C 0.56880(19) 0.1498(3) -0.33957(17) 0.0465 1.0000 Uani . C320 C 0.5075(3) 0.1759(9) -0.3882(3) 0.1391 1.0000 Uani . C321 C 0.4937(4) 0.1766(11) -0.4541(3) 0.1577 1.0000 Uani . C322 C 0.5402(3) 0.1486(6) -0.4707(2) 0.0899 1.0000 Uani . C323 C 0.6005(4) 0.1198(11) -0.4225(3) 0.1647 1.0000 Uani . C324 C 0.6143(3) 0.120(1) -0.3576(3) 0.1546 1.0000 Uani . O1 O 0.84920(19) 0.4549(3) 0.05422(16) 0.0871 1.0000 Uani . O2 O 0.7463(4) 0.6135(9) -0.0181(4) 0.0669 0.4291 Uani . O3 O 0.8072(7) 0.6467(15) -0.0229(8) 0.0664 0.4291 Uani . O4 O 0.7828(5) 0.6465(9) -0.0160(4) 0.0553 0.5709 Uani . H1021 H 1.0432 0.9338 0.2581 0.113(3) 1.0000 Uiso . H1031 H 1.0695 0.9371 0.3721 0.113(3) 1.0000 Uiso . H1041 H 1.0153 0.8026 0.4102 0.113(3) 1.0000 Uiso . H1051 H 0.9302 0.6670 0.3343 0.113(3) 1.0000 Uiso . H1061 H 0.8992 0.6748 0.2193 0.113(3) 1.0000 Uiso . H1081 H 1.0666 0.6683 0.1823 0.113(3) 1.0000 Uiso . H1091 H 1.1633 0.6738 0.1652 0.113(3) 1.0000 Uiso . H1101 H 1.1781 0.8329 0.1075 0.113(3) 1.0000 Uiso . H1111 H 1.0945 0.9851 0.0615 0.113(3) 1.0000 Uiso . H1121 H 0.9966 0.9789 0.0771 0.113(3) 1.0000 Uiso . H1141 H 0.8270 0.8605 0.0050 0.113(3) 1.0000 Uiso . H1151 H 0.7639 1.0336 -0.0484 0.113(3) 1.0000 Uiso . H1161 H 0.7877 1.2171 0.0090 0.113(3) 1.0000 Uiso . H1171 H 0.8703 1.2235 0.1217 0.113(3) 1.0000 Uiso . H1181 H 0.9317 1.0501 0.1773 0.113(3) 1.0000 Uiso . H2221 H 0.7396 0.3525 0.0786 0.113(3) 1.0000 Uiso . H2231 H 0.6738 0.1866 0.0121 0.113(3) 1.0000 Uiso . H2241 H 0.5545 0.2105 -0.0605 0.113(3) 1.0000 Uiso . H2251 H 0.5020 0.3929 -0.0676 0.113(3) 1.0000 Uiso . H2261 H 0.5655 0.5565 0.0006 0.113(3) 1.0000 Uiso . H2281 H 0.7018 0.7830 0.0084 0.113(3) 1.0000 Uiso . H2291 H 0.6424 0.9649 -0.0280 0.113(3) 1.0000 Uiso . H2301 H 0.5694 1.0301 0.0125 0.113(3) 1.0000 Uiso . H2311 H 0.5565 0.9159 0.0918 0.113(3) 1.0000 Uiso . H2321 H 0.6155 0.7313 0.1285 0.113(3) 1.0000 Uiso . H2341 H 0.7947 0.6983 0.2323 0.113(3) 1.0000 Uiso . H2351 H 0.8096 0.6712 0.3413 0.113(3) 1.0000 Uiso . H2361 H 0.7447 0.5245 0.3607 0.113(3) 1.0000 Uiso . H2371 H 0.6627 0.4125 0.2712 0.113(3) 1.0000 Uiso . H2381 H 0.6500 0.4326 0.1633 0.113(3) 1.0000 Uiso . H3021 H 0.5374 0.3282 -0.1977 0.113(3) 1.0000 Uiso . H3031 H 0.4310 0.3482 -0.1967 0.113(3) 1.0000 Uiso . H3041 H 0.3463 0.1970 -0.2446 0.113(3) 1.0000 Uiso . H3051 H 0.3637 0.0310 -0.2991 0.113(3) 1.0000 Uiso . H3061 H 0.4688 0.0124 -0.3005 0.113(3) 1.0000 Uiso . H3081 H 0.5664 -0.0380 -0.1856 0.113(3) 1.0000 Uiso . H3091 H 0.6352 -0.2053 -0.1252 0.113(3) 1.0000 Uiso . H3101 H 0.7426 -0.2371 -0.1186 0.113(3) 1.0000 Uiso . H3111 H 0.7852 -0.0987 -0.1664 0.113(3) 1.0000 Uiso . H3121 H 0.7201 0.0706 -0.2231 0.113(3) 1.0000 Uiso . H3141 H 0.6838 0.2187 -0.1198 0.113(3) 1.0000 Uiso . H3151 H 0.7458 0.3950 -0.0689 0.113(3) 1.0000 Uiso . H3161 H 0.7392 0.5628 -0.1341 0.113(3) 1.0000 Uiso . H3171 H 0.6703 0.5565 -0.2502 0.113(3) 1.0000 Uiso . H3181 H 0.6077 0.3805 -0.3043 0.113(3) 1.0000 Uiso . H3201 H 0.4688 0.1908 -0.3778 0.113(3) 1.0000 Uiso . H3211 H 0.4458 0.1983 -0.4897 0.113(3) 1.0000 Uiso . H3221 H 0.5291 0.1498 -0.5187 0.113(3) 1.0000 Uiso . H3231 H 0.6380 0.0980 -0.4332 0.113(3) 1.0000 Uiso . H3241 H 0.6598 0.0881 -0.3226 0.113(3) 1.0000 Uiso . 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 V1 0.0375(3) 0.0353(3) 0.0368(3) -0.0027(2) 0.0180(2) -0.0012(2) Si1 0.0391(5) 0.0421(5) 0.0438(5) -0.0042(4) 0.0212(4) -0.0056(4) Si2 0.0389(5) 0.0436(5) 0.0445(5) 0.0048(4) 0.0227(4) 0.0002(4) P1 0.0401(5) 0.0393(5) 0.0353(4) 0.0002(4) 0.0167(4) -0.0026(4) O11 0.0467(14) 0.0490(14) 0.0554(15) -0.0107(12) 0.0259(12) -0.0133(11) O12 0.0431(13) 0.0562(15) 0.0503(14) 0.0022(12) 0.0263(11) -0.0017(12) C101 0.0433(19) 0.051(2) 0.0457(19) -0.0012(16) 0.0219(16) 0.0041(16) C102 0.063(3) 0.072(3) 0.055(2) -0.007(2) 0.028(2) -0.013(2) C103 0.080(3) 0.094(4) 0.057(3) -0.015(3) 0.026(2) -0.008(3) C104 0.091(4) 0.105(4) 0.047(2) 0.003(3) 0.034(3) 0.013(3) C105 0.083(3) 0.095(4) 0.067(3) 0.010(3) 0.047(3) -0.002(3) C106 0.062(2) 0.060(2) 0.059(2) 0.0005(19) 0.035(2) -0.001(2) C107 0.0409(18) 0.053(2) 0.0477(19) -0.0062(16) 0.0233(16) -0.0097(16) C108 0.054(2) 0.067(3) 0.066(3) 0.011(2) 0.031(2) 0.007(2) C109 0.060(3) 0.097(4) 0.096(4) 0.010(3) 0.044(3) 0.012(3) C110 0.051(3) 0.122(5) 0.095(4) 0.008(3) 0.046(3) -0.002(3) C111 0.068(3) 0.107(4) 0.083(3) 0.017(3) 0.046(3) -0.015(3) C112 0.052(2) 0.071(3) 0.065(3) 0.010(2) 0.028(2) -0.004(2) C113 0.0461(19) 0.047(2) 0.0475(19) -0.0036(16) 0.0257(17) -0.0027(16) C114 0.067(3) 0.048(2) 0.053(2) -0.0021(18) 0.017(2) -0.0020(19) C115 0.087(3) 0.063(3) 0.055(3) 0.008(2) 0.014(2) 0.003(2) C116 0.071(3) 0.056(2) 0.069(3) 0.006(2) 0.039(2) 0.005(2) C117 0.086(3) 0.053(3) 0.082(3) -0.013(2) 0.038(3) 0.007(2) C118 0.076(3) 0.060(3) 0.059(3) -0.014(2) 0.016(2) 0.007(2) C221 0.047(2) 0.051(2) 0.050(2) 0.0033(17) 0.0256(17) -0.0019(17) C222 0.058(3) 0.052(2) 0.099(4) -0.010(2) 0.034(3) -0.007(2) C223 0.088(4) 0.061(3) 0.119(4) -0.016(3) 0.054(3) -0.015(3) C224 0.093(4) 0.073(3) 0.079(3) -0.018(3) 0.036(3) -0.026(3) C225 0.066(3) 0.096(4) 0.086(4) -0.006(3) 0.004(3) -0.014(3) C226 0.059(3) 0.071(3) 0.067(3) -0.005(2) 0.014(2) -0.002(2) C227 0.0436(18) 0.049(2) 0.050(2) 0.0013(16) 0.0220(16) -0.0025(16) C228 0.095(4) 0.070(3) 0.088(3) 0.027(3) 0.062(3) 0.025(3) C229 0.125(5) 0.073(3) 0.109(4) 0.045(3) 0.073(4) 0.032(3) C230 0.071(3) 0.054(3) 0.101(4) 0.018(3) 0.035(3) 0.019(2) C231 0.072(3) 0.066(3) 0.113(4) 0.011(3) 0.055(3) 0.020(2) C232 0.063(2) 0.062(3) 0.086(3) 0.011(2) 0.045(2) 0.007(2) C233 0.0433(18) 0.052(2) 0.051(2) 0.0094(17) 0.0260(17) 0.0069(16) C234 0.063(3) 0.086(3) 0.064(3) -0.003(2) 0.038(2) -0.012(2) C235 0.071(3) 0.146(5) 0.055(3) -0.010(3) 0.033(2) -0.003(3) C236 0.102(4) 0.110(4) 0.063(3) 0.025(3) 0.051(3) 0.026(4) C237 0.135(5) 0.078(3) 0.098(4) 0.015(3) 0.086(4) -0.003(3) C238 0.097(3) 0.060(3) 0.074(3) 0.001(2) 0.054(3) -0.013(2) C301 0.0414(18) 0.046(2) 0.0401(18) 0.0017(15) 0.0191(16) -0.0032(15) C302 0.061(2) 0.058(2) 0.053(2) -0.0060(18) 0.0300(19) 0.0001(19) C303 0.071(3) 0.080(3) 0.065(3) -0.017(2) 0.040(2) 0.003(2) C304 0.048(2) 0.101(4) 0.062(3) 0.003(2) 0.030(2) 0.006(2) C305 0.048(2) 0.072(3) 0.069(3) -0.010(2) 0.027(2) -0.006(2) C306 0.051(2) 0.053(2) 0.064(2) -0.0121(19) 0.0279(19) -0.0057(18) C307 0.0488(19) 0.0373(18) 0.0373(17) -0.0031(14) 0.0173(15) -0.0022(15) C308 0.065(3) 0.071(3) 0.066(3) 0.023(2) 0.031(2) -0.003(2) C309 0.103(4) 0.063(3) 0.076(3) 0.026(3) 0.030(3) -0.013(3) C310 0.089(4) 0.045(2) 0.058(3) 0.0051(19) 0.015(2) 0.012(2) C311 0.088(4) 0.080(3) 0.097(4) 0.025(3) 0.049(3) 0.032(3) C312 0.071(3) 0.070(3) 0.084(3) 0.031(2) 0.046(3) 0.020(2) C313 0.0419(18) 0.0382(17) 0.0431(18) -0.0002(14) 0.0185(15) -0.0027(15) C314 0.066(2) 0.051(2) 0.046(2) -0.0039(18) 0.0150(19) -0.010(2) C315 0.075(3) 0.061(3) 0.058(3) -0.011(2) 0.014(2) -0.013(2) C316 0.063(3) 0.050(2) 0.083(3) -0.015(2) 0.028(2) -0.011(2) C317 0.073(3) 0.047(2) 0.084(3) 0.000(2) 0.041(3) -0.010(2) C318 0.053(2) 0.053(2) 0.057(2) 0.0072(18) 0.0253(18) -0.0033(18) C319 0.051(2) 0.0464(19) 0.0383(18) 0.0023(15) 0.0191(17) -0.0050(17) C320 0.073(4) 0.285(11) 0.051(3) 0.029(5) 0.024(3) 0.054(5) C321 0.094(5) 0.307(12) 0.045(3) 0.029(5) 0.013(3) 0.052(6) C322 0.111(4) 0.119(4) 0.043(3) 0.003(3) 0.039(3) -0.013(4) C323 0.105(5) 0.345(14) 0.053(3) 0.018(5) 0.046(3) 0.064(7) C324 0.081(4) 0.336(13) 0.053(3) 0.026(5) 0.038(3) 0.074(6) O1 0.103(3) 0.0554(19) 0.076(2) -0.0046(16) 0.0222(19) 0.0292(18) O2 0.053(5) 0.086(6) 0.052(4) -0.004(4) 0.018(4) 0.007(4) O3 0.067(8) 0.070(5) 0.064(6) 0.004(4) 0.033(5) -0.001(6) O4 0.057(7) 0.059(4) 0.040(3) 0.004(3) 0.017(5) -0.005(5) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag V1 . O11 . 1.820(2) yes V1 . O12 . 1.829(2) yes V1 . O1 . 1.619(3) yes V1 . O2 . 1.846(8) yes V1 . O3 . 1.787(15) yes V1 . O4 . 1.624(9) yes Si1 . O11 . 1.612(2) yes Si1 . C101 . 1.883(4) yes Si1 . C107 . 1.880(4) yes Si1 . C113 . 1.873(4) yes Si2 . O12 . 1.615(2) yes Si2 . C221 . 1.876(4) yes Si2 . C227 . 1.874(4) yes Si2 . C233 . 1.876(4) yes P1 . C301 . 1.793(3) yes P1 . C307 . 1.794(3) yes P1 . C313 . 1.792(3) yes P1 . C319 . 1.793(3) yes C101 . C102 . 1.389(6) yes C101 . C106 . 1.377(6) yes C102 . C103 . 1.394(6) yes C102 . H1021 . 1.006 no C103 . C104 . 1.358(8) yes C103 . H1031 . 1.004 no C104 . C105 . 1.376(7) yes C104 . H1041 . 1.013 no C105 . C106 . 1.396(6) yes C105 . H1051 . 1.013 no C106 . H1061 . 1.007 no C107 . C108 . 1.381(6) yes C107 . C112 . 1.375(6) yes C108 . C109 . 1.379(6) yes C108 . H1081 . 1.004 no C109 . C110 . 1.363(8) yes C109 . H1091 . 1.009 no C110 . C111 . 1.364(8) yes C110 . H1101 . 0.995 no C111 . C112 . 1.396(6) yes C111 . H1111 . 1.008 no C112 . H1121 . 1.000 no C113 . C114 . 1.377(5) yes C113 . C118 . 1.381(6) yes C114 . C115 . 1.382(6) yes C114 . H1141 . 1.003 no C115 . C116 . 1.370(7) yes C115 . H1151 . 1.004 no C116 . C117 . 1.344(6) yes C116 . H1161 . 1.010 no C117 . C118 . 1.389(7) yes C117 . H1171 . 1.000 no C118 . H1181 . 1.003 no C221 . C222 . 1.381(6) yes C221 . C226 . 1.375(6) yes C222 . C223 . 1.387(7) yes C222 . H2221 . 1.012 no C223 . C224 . 1.368(8) yes C223 . H2231 . 1.018 no C224 . C225 . 1.344(8) yes C224 . H2241 . 1.008 no C225 . C226 . 1.382(7) yes C225 . H2251 . 1.004 no C226 . H2261 . 1.014 no C227 . C228 . 1.375(6) yes C227 . C232 . 1.383(6) yes C228 . C229 . 1.383(7) yes C228 . H2281 . 1.007 no C229 . C230 . 1.349(8) yes C229 . H2291 . 1.007 no C230 . C231 . 1.352(7) yes C230 . H2301 . 1.006 no C231 . C232 . 1.389(6) yes C231 . H2311 . 1.014 no C232 . H2321 . 1.012 no C233 . C234 . 1.380(6) yes C233 . C238 . 1.387(6) yes C234 . C235 . 1.396(7) yes C234 . H2341 . 1.015 no C235 . C236 . 1.357(8) yes C235 . H2351 . 1.015 no C236 . C237 . 1.363(8) yes C236 . H2361 . 1.009 no C237 . C238 . 1.379(7) yes C237 . H2371 . 1.002 no C238 . H2381 . 1.010 no C301 . C302 . 1.390(5) yes C301 . C306 . 1.381(5) yes C302 . C303 . 1.381(6) yes C302 . H3021 . 1.005 no C303 . C304 . 1.379(7) yes C303 . H3031 . 1.010 no C304 . C305 . 1.377(6) yes C304 . H3041 . 1.010 no C305 . C306 . 1.370(6) yes C305 . H3051 . 1.011 no C306 . H3061 . 1.008 no C307 . C308 . 1.359(5) yes C307 . C312 . 1.392(6) yes C308 . C309 . 1.396(7) yes C308 . H3081 . 0.998 no C309 . C310 . 1.349(8) yes C309 . H3091 . 1.002 no C310 . C311 . 1.356(8) yes C310 . H3101 . 1.013 no C311 . C312 . 1.371(6) yes C311 . H3111 . 1.012 no C312 . H3121 . 1.012 no C313 . C314 . 1.396(5) yes C313 . C318 . 1.383(5) yes C314 . C315 . 1.374(6) yes C314 . H3141 . 1.013 no C315 . C316 . 1.366(7) yes C315 . H3151 . 1.002 no C316 . C317 . 1.368(6) yes C316 . H3161 . 1.010 no C317 . C318 . 1.380(6) yes C317 . H3171 . 1.002 no C318 . H3181 . 1.011 no C319 . C320 . 1.317(6) yes C319 . C324 . 1.316(7) yes C320 . C321 . 1.396(8) yes C320 . H3201 . 1.019 no C321 . C322 . 1.309(9) yes C321 . H3211 . 1.015 no C322 . C323 . 1.305(9) yes C322 . H3221 . 1.011 no C323 . C324 . 1.376(7) yes C323 . H3231 . 1.013 no C324 . H3241 . 1.009 no O2 . O3 . 1.467(8) yes O2 . O4 . 0.88(1) yes O3 . O4 . 0.639(9) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O11 . V1 . O12 . 103.69(11) yes O11 . V1 . O1 . 111.68(16) yes O12 . V1 . O1 . 107.70(17) yes O11 . V1 . O2 . 135.0(3) yes O12 . V1 . O2 . 89.0(3) yes O1 . V1 . O2 . 104.7(3) yes O11 . V1 . O3 . 98.0(5) yes O12 . V1 . O3 . 132.3(4) yes O1 . V1 . O3 . 102.7(5) yes O2 . V1 . O3 . 47.6(3) yes O11 . V1 . O4 . 110.6(4) yes O12 . V1 . O4 . 111.7(3) yes O1 . V1 . O4 . 111.2(4) yes O2 . V1 . O4 . 28.3(3) yes O3 . V1 . O4 . 20.9(4) yes O11 . Si1 . C101 . 108.51(15) yes O11 . Si1 . C107 . 109.15(15) yes C101 . Si1 . C107 . 108.77(16) yes O11 . Si1 . C113 . 112.53(15) yes C101 . Si1 . C113 . 110.35(16) yes C107 . Si1 . C113 . 107.46(17) yes O12 . Si2 . C221 . 109.67(15) yes O12 . Si2 . C227 . 111.54(15) yes C221 . Si2 . C227 . 110.46(17) yes O12 . Si2 . C233 . 108.58(14) yes C221 . Si2 . C233 . 108.53(17) yes C227 . Si2 . C233 . 107.97(17) yes C301 . P1 . C307 . 110.18(16) yes C301 . P1 . C313 . 109.17(16) yes C307 . P1 . C313 . 108.21(16) yes C301 . P1 . C319 . 109.43(17) yes C307 . P1 . C319 . 110.40(17) yes C313 . P1 . C319 . 109.42(17) yes V1 . O11 . Si1 . 152.90(17) yes V1 . O12 . Si2 . 144.34(16) yes Si1 . C101 . C102 . 122.1(3) yes Si1 . C101 . C106 . 119.9(3) yes C102 . C101 . C106 . 118.0(4) yes C101 . C102 . C103 . 120.9(4) yes C101 . C102 . H1021 . 118.875 no C103 . C102 . H1021 . 120.207 no C102 . C103 . C104 . 119.6(4) yes C102 . C103 . H1031 . 119.920 no C104 . C103 . H1031 . 120.441 no C103 . C104 . C105 . 121.1(4) yes C103 . C104 . H1041 . 119.181 no C105 . C104 . H1041 . 119.679 no C104 . C105 . C106 . 118.8(4) yes C104 . C105 . H1051 . 121.433 no C106 . C105 . H1051 . 119.812 no C101 . C106 . C105 . 121.6(4) yes C101 . C106 . H1061 . 118.844 no C105 . C106 . H1061 . 119.588 no Si1 . C107 . C108 . 119.7(3) yes Si1 . C107 . C112 . 122.5(3) yes C108 . C107 . C112 . 117.8(3) yes C107 . C108 . C109 . 121.0(4) yes C107 . C108 . H1081 . 119.501 no C109 . C108 . H1081 . 119.471 no C108 . C109 . C110 . 120.6(5) yes C108 . C109 . H1091 . 119.917 no C110 . C109 . H1091 . 119.489 no C109 . C110 . C111 . 119.7(4) yes C109 . C110 . H1101 . 119.503 no C111 . C110 . H1101 . 120.696 no C110 . C111 . C112 . 119.8(4) yes C110 . C111 . H1111 . 119.916 no C112 . C111 . H1111 . 120.259 no C107 . C112 . C111 . 121.0(4) yes C107 . C112 . H1121 . 120.292 no C111 . C112 . H1121 . 118.674 no Si1 . C113 . C114 . 122.0(3) yes Si1 . C113 . C118 . 121.2(3) yes C114 . C113 . C118 . 116.7(4) yes C113 . C114 . C115 . 121.3(4) yes C113 . C114 . H1141 . 119.547 no C115 . C114 . H1141 . 119.150 no C114 . C115 . C116 . 120.7(4) yes C114 . C115 . H1151 . 120.073 no C116 . C115 . H1151 . 119.225 no C115 . C116 . C117 . 119.1(4) yes C115 . C116 . H1161 . 120.572 no C117 . C116 . H1161 . 120.309 no C116 . C117 . C118 . 120.5(4) yes C116 . C117 . H1171 . 119.603 no C118 . C117 . H1171 . 119.914 no C113 . C118 . C117 . 121.7(4) yes C113 . C118 . H1181 . 119.242 no C117 . C118 . H1181 . 119.069 no Si2 . C221 . C222 . 120.2(3) yes Si2 . C221 . C226 . 122.8(3) yes C222 . C221 . C226 . 117.1(4) yes C221 . C222 . C223 . 121.5(4) yes C221 . C222 . H2221 . 118.730 no C223 . C222 . H2221 . 119.796 no C222 . C223 . C224 . 119.6(5) yes C222 . C223 . H2231 . 120.926 no C224 . C223 . H2231 . 119.443 no C223 . C224 . C225 . 119.7(5) yes C223 . C224 . H2241 . 120.362 no C225 . C224 . H2241 . 119.940 no C224 . C225 . C226 . 120.9(5) yes C224 . C225 . H2251 . 118.947 no C226 . C225 . H2251 . 120.169 no C221 . C226 . C225 . 121.2(5) yes C221 . C226 . H2261 . 118.761 no C225 . C226 . H2261 . 120.011 no Si2 . C227 . C228 . 123.2(3) yes Si2 . C227 . C232 . 120.4(3) yes C228 . C227 . C232 . 116.4(4) yes C227 . C228 . C229 . 121.6(5) yes C227 . C228 . H2281 . 119.440 no C229 . C228 . H2281 . 118.917 no C228 . C229 . C230 . 120.3(5) yes C228 . C229 . H2291 . 119.360 no C230 . C229 . H2291 . 120.327 no C229 . C230 . C231 . 120.2(4) yes C229 . C230 . H2301 . 119.708 no C231 . C230 . H2301 . 120.077 no C230 . C231 . C232 . 119.6(4) yes C230 . C231 . H2311 . 120.136 no C232 . C231 . H2311 . 120.272 no C227 . C232 . C231 . 121.8(4) yes C227 . C232 . H2321 . 119.440 no C231 . C232 . H2321 . 118.751 no Si2 . C233 . C234 . 120.2(3) yes Si2 . C233 . C238 . 123.4(3) yes C234 . C233 . C238 . 116.2(4) yes C233 . C234 . C235 . 121.9(4) yes C233 . C234 . H2341 . 119.325 no C235 . C234 . H2341 . 118.793 no C234 . C235 . C236 . 120.0(5) yes C234 . C235 . H2351 . 119.873 no C236 . C235 . H2351 . 120.077 no C235 . C236 . C237 . 119.4(5) yes C235 . C236 . H2361 . 120.690 no C237 . C236 . H2361 . 119.934 no C236 . C237 . C238 . 120.6(5) yes C236 . C237 . H2371 . 119.173 no C238 . C237 . H2371 . 120.215 no C233 . C238 . C237 . 121.8(5) yes C233 . C238 . H2381 . 119.025 no C237 . C238 . H2381 . 119.138 no P1 . C301 . C302 . 119.6(3) yes P1 . C301 . C306 . 120.7(3) yes C302 . C301 . C306 . 119.7(3) yes C301 . C302 . C303 . 119.3(4) yes C301 . C302 . H3021 . 119.981 no C303 . C302 . H3021 . 120.740 no C302 . C303 . C304 . 120.1(4) yes C302 . C303 . H3031 . 119.923 no C304 . C303 . H3031 . 119.928 no C303 . C304 . C305 . 120.7(4) yes C303 . C304 . H3041 . 119.731 no C305 . C304 . H3041 . 119.533 no C304 . C305 . C306 . 119.1(4) yes C304 . C305 . H3051 . 120.637 no C306 . C305 . H3051 . 120.222 no C301 . C306 . C305 . 121.1(4) yes C301 . C306 . H3061 . 119.455 no C305 . C306 . H3061 . 119.469 no P1 . C307 . C308 . 122.9(3) yes P1 . C307 . C312 . 118.2(3) yes C308 . C307 . C312 . 118.8(4) yes C307 . C308 . C309 . 120.1(4) yes C307 . C308 . H3081 . 119.530 no C309 . C308 . H3081 . 120.323 no C308 . C309 . C310 . 120.2(4) yes C308 . C309 . H3091 . 120.224 no C310 . C309 . H3091 . 119.542 no C309 . C310 . C311 . 120.2(4) yes C309 . C310 . H3101 . 120.559 no C311 . C310 . H3101 . 119.280 no C310 . C311 . C312 . 120.6(5) yes C310 . C311 . H3111 . 120.253 no C312 . C311 . H3111 . 119.148 no C307 . C312 . C311 . 120.0(4) yes C307 . C312 . H3121 . 119.914 no C311 . C312 . H3121 . 120.090 no P1 . C313 . C314 . 119.5(3) yes P1 . C313 . C318 . 120.6(3) yes C314 . C313 . C318 . 119.8(3) yes C313 . C314 . C315 . 119.6(4) yes C313 . C314 . H3141 . 120.046 no C315 . C314 . H3141 . 120.366 no C314 . C315 . C316 . 120.3(4) yes C314 . C315 . H3151 . 119.612 no C316 . C315 . H3151 . 120.052 no C315 . C316 . C317 . 120.4(4) yes C315 . C316 . H3161 . 120.117 no C317 . C316 . H3161 . 119.433 no C316 . C317 . C318 . 120.5(4) yes C316 . C317 . H3171 . 119.395 no C318 . C317 . H3171 . 120.103 no C313 . C318 . C317 . 119.4(4) yes C313 . C318 . H3181 . 119.846 no C317 . C318 . H3181 . 120.785 no P1 . C319 . C320 . 121.8(4) yes P1 . C319 . C324 . 122.5(3) yes C320 . C319 . C324 . 115.7(4) yes C319 . C320 . C321 . 121.2(6) yes C319 . C320 . H3201 . 119.176 no C321 . C320 . H3201 . 119.549 no C320 . C321 . C322 . 122.0(6) yes C320 . C321 . H3211 . 118.101 no C322 . C321 . H3211 . 119.861 no C321 . C322 . C323 . 116.7(5) yes C321 . C322 . H3221 . 120.699 no C323 . C322 . H3221 . 122.609 no C322 . C323 . C324 . 121.4(6) yes C322 . C323 . H3231 . 119.232 no C324 . C323 . H3231 . 119.332 no C319 . C324 . C323 . 122.9(5) yes C319 . C324 . H3241 . 118.276 no C323 . C324 . H3241 . 118.483 no V1 . O2 . O3 . 64.1(8) yes V1 . O2 . O4 . 61.6(7) yes O3 . O2 . O4 . 12.3(12) yes V1 . O3 . O2 . 68.3(7) yes V1 . O3 . O4 . 65.0(20) yes O2 . O3 . O4 . 17.0(17) yes V1 . O4 . O2 . 90.1(8) yes V1 . O4 . O3 . 94.1(22) yes O2 . O4 . O3 . 150.7(28) yes