# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1641 #cif for paper no. B001304H #=============================================================================== data_global #=============================================================================== _audit_creation_date 28-01-00 # 1. SUBMISSION DETAILS _publ_contact_author ;Louis Ricard, Labo DCPH, Ecole Polytechnique Route de Saclay 91128 Palaiseau France ; _publ_contact_author_phone '01-69-33-45-72' _publ_contact_author_fax '01-69-33-39-90' _publ_contact_author_email ricard@neptune.polytechnique.fr _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Chem. Comm.. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The Unexpected Head-to-head Dimerisation of Phosphirenes. ; # 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 Tran Huy Ngoc Hoa, Ricard Louis, and Mathey Francois _publ_author_address ; Laboratoire Heteroelements et Coordination, CNRS UMR 7653, DCPH Ecole Polytechnique, F-91128 Palaiseau Cedex France ; #=============================================================================== # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). An highly disordered CH2Cl2 molecule was detected in the elementary cell at (0,1/2,0). This was taken into account by back-Fourier transformation of all density found in the disordered solvent area with the program SQUEEZE (Sluis & Spek, 1990). ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. #=============================================================================== data_p2c4 # compound 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40H30P2*1/2CH2Cl2' _chemical_formula_weight 615.04 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.069(5) _cell_length_b 12.180(5) _cell_length_c 22.035(5) _cell_angle_alpha 97.030(5) _cell_angle_beta 92.580(5) _cell_angle_gamma 96.690(5) _cell_volume 1602.7(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 637 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 642 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9522 _exptl_absorpt_correction_T_max 0.9615 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14341 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 30.01 _reflns_number_total 9228 _reflns_number_gt 7333 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0807P)^2^+0.4111P] 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 9228 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1472 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _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 P1 P 1.01220(6) 0.09062(3) 0.325546(17) 0.02168(10) Uani 1 1 d . . . P2 P 0.65523(6) 0.04322(3) 0.303438(16) 0.02102(10) Uani 1 1 d . . . C1 C 0.9977(2) 0.22879(11) 0.29925(6) 0.0204(3) Uani 1 1 d . . . C2 C 0.9070(2) 0.23340(11) 0.24227(6) 0.0206(3) Uani 1 1 d . . . C3 C 0.8096(2) 0.13201(11) 0.20025(6) 0.0195(3) Uani 1 1 d . . . C4 C 0.6946(2) 0.04294(11) 0.22048(6) 0.0192(3) Uani 1 1 d . . . C5 C 1.0202(3) 0.12328(12) 0.40901(7) 0.0247(3) Uani 1 1 d . . . C6 C 1.2055(3) 0.09754(14) 0.44176(8) 0.0336(4) Uani 1 1 d . . . H6 H 1.3190 0.0647 0.4204 0.040 Uiso 1 1 calc R . . C7 C 1.2254(4) 0.11953(16) 0.50547(9) 0.0440(5) Uani 1 1 d . . . H7 H 1.3522 0.1019 0.5274 0.053 Uiso 1 1 calc R . . C8 C 1.0606(4) 0.16702(16) 0.53660(8) 0.0466(5) Uani 1 1 d . . . H8 H 1.0742 0.1820 0.5800 0.056 Uiso 1 1 calc R . . C9 C 0.8762(4) 0.19281(15) 0.50486(8) 0.0412(4) Uani 1 1 d . . . H9 H 0.7633 0.2256 0.5265 0.049 Uiso 1 1 calc R . . C10 C 0.8551(3) 0.17098(13) 0.44115(7) 0.0318(3) Uani 1 1 d . . . H10 H 0.7276 0.1887 0.4195 0.038 Uiso 1 1 calc R . . C11 C 1.0845(3) 0.32809(11) 0.34337(7) 0.0228(3) Uani 1 1 d . . . C12 C 1.2992(3) 0.33803(13) 0.37039(7) 0.0279(3) Uani 1 1 d . . . H12 H 1.3934 0.2831 0.3585 0.034 Uiso 1 1 calc R . . C13 C 1.3770(3) 0.42709(14) 0.41444(8) 0.0354(4) Uani 1 1 d . . . H13 H 1.5242 0.4334 0.4322 0.043 Uiso 1 1 calc R . . C14 C 1.2391(3) 0.50727(14) 0.43261(8) 0.0384(4) Uani 1 1 d . . . H14 H 1.2915 0.5679 0.4631 0.046 Uiso 1 1 calc R . . C15 C 1.0254(3) 0.49841(13) 0.40608(8) 0.0346(4) Uani 1 1 d . . . H15 H 0.9314 0.5532 0.4183 0.042 Uiso 1 1 calc R . . C16 C 0.9484(3) 0.40962(12) 0.36172(7) 0.0278(3) Uani 1 1 d . . . H16 H 0.8018 0.4042 0.3436 0.033 Uiso 1 1 calc R . . C17 C 0.8958(2) 0.34190(11) 0.21775(7) 0.0216(3) Uani 1 1 d . . . C18 C 1.0826(3) 0.42070(12) 0.21844(7) 0.0252(3) Uani 1 1 d . . . H18 H 1.2214 0.4061 0.2354 0.030 Uiso 1 1 calc R . . C19 C 1.0676(3) 0.52025(13) 0.19463(8) 0.0318(3) Uani 1 1 d . . . H19 H 1.1956 0.5734 0.1953 0.038 Uiso 1 1 calc R . . C20 C 0.8654(3) 0.54184(14) 0.16994(9) 0.0396(4) Uani 1 1 d . . . H20 H 0.8551 0.6099 0.1536 0.047 Uiso 1 1 calc R . . C21 C 0.6791(3) 0.46502(15) 0.16892(10) 0.0399(4) Uani 1 1 d . . . H21 H 0.5406 0.4802 0.1521 0.048 Uiso 1 1 calc R . . C22 C 0.6943(3) 0.36516(13) 0.19263(8) 0.0303(3) Uani 1 1 d . . . H22 H 0.5658 0.3122 0.1916 0.036 Uiso 1 1 calc R . . C23 C 0.8461(2) 0.13605(11) 0.13372(6) 0.0211(3) Uani 1 1 d . . . C24 C 1.0609(3) 0.16178(15) 0.11556(7) 0.0302(3) Uani 1 1 d . . . H24 H 1.1817 0.1780 0.1455 0.036 Uiso 1 1 calc R . . C25 C 1.1004(3) 0.16396(19) 0.05380(8) 0.0416(5) Uani 1 1 d . . . H25 H 1.2476 0.1809 0.0418 0.050 Uiso 1 1 calc R . . C26 C 0.9251(3) 0.14138(17) 0.01005(8) 0.0390(4) Uani 1 1 d . . . H26 H 0.9522 0.1422 -0.0320 0.047 Uiso 1 1 calc R . . C27 C 0.7100(3) 0.11762(14) 0.02746(7) 0.0303(3) Uani 1 1 d . . . H27 H 0.5893 0.1035 -0.0025 0.036 Uiso 1 1 calc R . . C28 C 0.6713(3) 0.11446(12) 0.08892(7) 0.0246(3) Uani 1 1 d . . . H28 H 0.5237 0.0974 0.1006 0.030 Uiso 1 1 calc R . . C29 C 0.5938(2) -0.05881(11) 0.17999(6) 0.0212(3) Uani 1 1 d . . . C30 C 0.7205(3) -0.11801(12) 0.13966(7) 0.0254(3) Uani 1 1 d . . . H30 H 0.8714 -0.0902 0.1357 0.030 Uiso 1 1 calc R . . C31 C 0.6294(3) -0.21730(13) 0.10499(7) 0.0326(4) Uani 1 1 d . . . H31 H 0.7179 -0.2570 0.0777 0.039 Uiso 1 1 calc R . . C32 C 0.4089(3) -0.25847(13) 0.11034(8) 0.0368(4) Uani 1 1 d . . . H32 H 0.3466 -0.3267 0.0870 0.044 Uiso 1 1 calc R . . C33 C 0.2805(3) -0.19988(13) 0.14973(8) 0.0338(4) Uani 1 1 d . . . H33 H 0.1292 -0.2275 0.1531 0.041 Uiso 1 1 calc R . . C34 C 0.3718(3) -0.10055(12) 0.18446(7) 0.0258(3) Uani 1 1 d . . . H34 H 0.2823 -0.0608 0.2114 0.031 Uiso 1 1 calc R . . C35 C 0.6274(3) -0.10639(11) 0.31097(6) 0.0225(3) Uani 1 1 d . . . C36 C 0.7861(3) -0.17640(13) 0.29343(7) 0.0285(3) Uani 1 1 d . . . H36 H 0.9196 -0.1468 0.2773 0.034 Uiso 1 1 calc R . . C37 C 0.7496(3) -0.28953(13) 0.29949(8) 0.0356(4) Uani 1 1 d . . . H37 H 0.8585 -0.3367 0.2876 0.043 Uiso 1 1 calc R . . C38 C 0.5553(3) -0.33339(14) 0.32283(9) 0.0392(4) Uani 1 1 d . . . H38 H 0.5307 -0.4106 0.3267 0.047 Uiso 1 1 calc R . . C39 C 0.3972(3) -0.26496(14) 0.34050(8) 0.0373(4) Uani 1 1 d . . . H39 H 0.2640 -0.2951 0.3566 0.045 Uiso 1 1 calc R . . C40 C 0.4333(3) -0.15172(13) 0.33468(7) 0.0292(3) Uani 1 1 d . . . H40 H 0.3243 -0.1049 0.3470 0.035 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 P1 0.0275(2) 0.01911(17) 0.01775(18) 0.00194(13) -0.00046(14) 0.00122(14) P2 0.0267(2) 0.01834(17) 0.01730(18) 0.00145(13) 0.00258(14) 0.00006(13) C1 0.0214(6) 0.0184(6) 0.0205(6) 0.0019(5) 0.0018(5) -0.0002(5) C2 0.0212(6) 0.0198(6) 0.0201(6) 0.0028(5) 0.0018(5) -0.0003(5) C3 0.0206(6) 0.0208(6) 0.0167(6) 0.0016(5) -0.0006(5) 0.0020(5) C4 0.0207(6) 0.0198(6) 0.0167(6) 0.0007(5) -0.0002(5) 0.0029(5) C5 0.0354(8) 0.0190(6) 0.0184(6) 0.0034(5) -0.0017(6) -0.0013(6) C6 0.0426(9) 0.0302(8) 0.0267(8) 0.0064(6) -0.0074(7) -0.0001(7) C7 0.0595(12) 0.0408(9) 0.0284(9) 0.0085(7) -0.0160(8) -0.0041(9) C8 0.0793(15) 0.0381(9) 0.0175(7) 0.0027(7) -0.0053(8) -0.0087(9) C9 0.0656(13) 0.0317(8) 0.0243(8) -0.0016(7) 0.0086(8) 0.0016(8) C10 0.0459(10) 0.0262(7) 0.0228(7) 0.0024(6) 0.0027(7) 0.0027(7) C11 0.0292(7) 0.0191(6) 0.0188(6) 0.0035(5) 0.0005(5) -0.0035(5) C12 0.0311(8) 0.0256(7) 0.0258(7) 0.0047(6) -0.0023(6) -0.0018(6) C13 0.0395(9) 0.0338(8) 0.0285(8) 0.0037(7) -0.0097(7) -0.0096(7) C14 0.0590(12) 0.0265(8) 0.0242(8) -0.0028(6) -0.0038(8) -0.0087(8) C15 0.0506(10) 0.0233(7) 0.0285(8) -0.0012(6) 0.0053(7) 0.0023(7) C16 0.0337(8) 0.0239(7) 0.0247(7) 0.0014(6) 0.0018(6) 0.0009(6) C17 0.0258(7) 0.0188(6) 0.0198(6) 0.0016(5) 0.0021(5) 0.0011(5) C18 0.0269(7) 0.0246(7) 0.0242(7) 0.0058(6) 0.0023(6) -0.0004(6) C19 0.0378(9) 0.0243(7) 0.0334(8) 0.0077(6) 0.0055(7) -0.0021(6) C20 0.0477(11) 0.0259(8) 0.0485(11) 0.0147(7) 0.0023(8) 0.0081(7) C21 0.0359(9) 0.0330(8) 0.0538(12) 0.0142(8) -0.0030(8) 0.0099(7) C22 0.0286(8) 0.0252(7) 0.0377(9) 0.0073(6) 0.0008(7) 0.0030(6) C23 0.0263(7) 0.0195(6) 0.0178(6) 0.0027(5) 0.0009(5) 0.0044(5) C24 0.0247(7) 0.0444(9) 0.0228(7) 0.0089(7) 0.0010(6) 0.0058(7) C25 0.0294(9) 0.0730(13) 0.0278(8) 0.0180(9) 0.0102(7) 0.0142(9) C26 0.0432(10) 0.0584(11) 0.0195(7) 0.0108(7) 0.0066(7) 0.0159(9) C27 0.0359(9) 0.0343(8) 0.0205(7) 0.0056(6) -0.0047(6) 0.0046(7) C28 0.0256(7) 0.0271(7) 0.0208(7) 0.0053(5) -0.0019(5) 0.0009(6) C29 0.0263(7) 0.0183(6) 0.0185(6) 0.0041(5) -0.0031(5) 0.0009(5) C30 0.0333(8) 0.0226(6) 0.0204(7) 0.0020(5) 0.0002(6) 0.0050(6) C31 0.0530(10) 0.0227(7) 0.0221(7) -0.0006(6) -0.0013(7) 0.0089(7) C32 0.0552(11) 0.0200(7) 0.0313(8) -0.0007(6) -0.0155(8) -0.0004(7) C33 0.0345(9) 0.0243(7) 0.0399(9) 0.0060(7) -0.0120(7) -0.0044(6) C34 0.0263(7) 0.0217(6) 0.0288(8) 0.0046(6) -0.0022(6) 0.0007(6) C35 0.0315(8) 0.0192(6) 0.0157(6) 0.0021(5) 0.0008(5) -0.0010(5) C36 0.0359(8) 0.0258(7) 0.0233(7) 0.0025(6) 0.0011(6) 0.0026(6) C37 0.0536(11) 0.0239(7) 0.0292(8) -0.0001(6) -0.0008(7) 0.0096(7) C38 0.0609(12) 0.0211(7) 0.0344(9) 0.0061(6) -0.0019(8) -0.0009(7) C39 0.0489(10) 0.0280(8) 0.0336(9) 0.0082(7) 0.0063(8) -0.0078(7) C40 0.0357(8) 0.0264(7) 0.0249(7) 0.0046(6) 0.0045(6) -0.0011(6) _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 P1 C5 1.8307(16) . ? P1 C1 1.8558(15) . ? P1 P2 2.1929(18) . ? P2 C35 1.8388(16) . ? P2 C4 1.8537(15) . ? C1 C2 1.358(2) . ? C1 C11 1.484(2) . ? C2 C3 1.494(2) . ? C2 C17 1.4951(19) . ? C3 C4 1.3539(19) . ? C3 C23 1.4983(19) . ? C4 C29 1.486(2) . ? C5 C10 1.394(2) . ? C5 C6 1.395(2) . ? C6 C7 1.394(2) . ? C6 H6 0.9500 . ? C7 C8 1.380(3) . ? C7 H7 0.9500 . ? C8 C9 1.381(3) . ? C8 H8 0.9500 . ? C9 C10 1.394(2) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.393(2) . ? C11 C16 1.398(2) . ? C12 C13 1.387(2) . ? C12 H12 0.9500 . ? C13 C14 1.392(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.393(2) . ? C17 C18 1.396(2) . ? C18 C19 1.390(2) . ? C18 H18 0.9500 . ? C19 C20 1.386(3) . ? C19 H19 0.9500 . ? C20 C21 1.379(3) . ? C20 H20 0.9500 . ? C21 C22 1.392(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.393(2) . ? C23 C28 1.395(2) . ? C24 C25 1.395(2) . ? C24 H24 0.9500 . ? C25 C26 1.382(3) . ? C25 H25 0.9500 . ? C26 C27 1.385(3) . ? C26 H26 0.9500 . ? C27 C28 1.389(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.391(2) . ? C29 C34 1.396(2) . ? C30 C31 1.390(2) . ? C30 H30 0.9500 . ? C31 C32 1.388(3) . ? C31 H31 0.9500 . ? C32 C33 1.382(3) . ? C32 H32 0.9500 . ? C33 C34 1.391(2) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.393(2) . ? C35 C36 1.396(2) . ? C36 C37 1.394(2) . ? C36 H36 0.9500 . ? C37 C38 1.384(3) . ? C37 H37 0.9500 . ? C38 C39 1.381(3) . ? C38 H38 0.9500 . ? C39 C40 1.394(2) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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 C5 P1 C1 102.72(7) . . ? C5 P1 P2 101.40(6) . . ? C1 P1 P2 91.11(5) . . ? C35 P2 C4 102.02(6) . . ? C35 P2 P1 101.17(5) . . ? C4 P2 P1 91.24(5) . . ? C2 C1 C11 124.28(12) . . ? C2 C1 P1 119.01(10) . . ? C11 C1 P1 116.70(10) . . ? C1 C2 C3 122.94(12) . . ? C1 C2 C17 121.62(13) . . ? C3 C2 C17 115.43(12) . . ? C4 C3 C2 122.65(12) . . ? C4 C3 C23 122.09(13) . . ? C2 C3 C23 115.26(11) . . ? C3 C4 C29 124.12(12) . . ? C3 C4 P2 119.95(11) . . ? C29 C4 P2 115.93(10) . . ? C10 C5 C6 118.84(15) . . ? C10 C5 P1 124.46(12) . . ? C6 C5 P1 116.70(13) . . ? C7 C6 C5 120.60(18) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 119.85(18) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 120.24(17) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 120.21(18) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C5 120.26(17) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? C12 C11 C16 118.65(14) . . ? C12 C11 C1 120.43(13) . . ? C16 C11 C1 120.78(14) . . ? C13 C12 C11 120.82(16) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 119.94(17) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 119.82(16) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.14(16) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.63(16) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C22 C17 C18 118.58(14) . . ? C22 C17 C2 119.45(13) . . ? C18 C17 C2 121.96(13) . . ? C19 C18 C17 120.63(15) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 119.86(15) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 120.30(15) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.82(16) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C17 120.81(15) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? C24 C23 C28 118.53(14) . . ? C24 C23 C3 119.38(13) . . ? C28 C23 C3 122.09(13) . . ? C23 C24 C25 120.61(15) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 119.97(16) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.12(16) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 119.82(15) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C23 120.93(15) . . ? C27 C28 H28 119.5 . . ? C23 C28 H28 119.5 . . ? C30 C29 C34 118.57(14) . . ? C30 C29 C4 121.13(14) . . ? C34 C29 C4 120.19(13) . . ? C31 C30 C29 120.91(16) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C32 C31 C30 119.94(16) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 119.77(15) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.26(16) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C29 120.55(15) . . ? C33 C34 H34 119.7 . . ? C29 C34 H34 119.7 . . ? C40 C35 C36 118.76(14) . . ? C40 C35 P2 117.22(11) . . ? C36 C35 P2 124.02(12) . . ? C37 C36 C35 120.32(16) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C38 C37 C36 120.21(16) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C39 C38 C37 120.05(15) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 119.92(16) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C35 C40 C39 120.74(16) . . ? C35 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.878 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.065 data_wpsi # compound 4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H30 O5 P2 Si2 W' _chemical_formula_weight 736.48 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' 'P' 'P' 0.1023 0.0942 '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 'P 21/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 12.6004(3) _cell_length_b 12.2493(3) _cell_length_c 20.1311(5) _cell_angle_alpha 90.000 _cell_angle_beta 96.1640(10) _cell_angle_gamma 90.000 _cell_volume 3089.19(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 601 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'cube' _exptl_crystal_colour 'pale yellow' _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 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 3.953 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5052 _exptl_absorpt_correction_T_max 0.5052 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16625 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 30.03 _reflns_number_total 8897 _reflns_number_gt 8030 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0398P)^2^+0.6365P] 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 8897 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.221 _refine_ls_restrained_S_all 1.221 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.200261(8) -0.450536(8) 0.135686(5) 0.01551(5) Uani 1 1 d . . . P1 P 0.43093(6) -0.24139(6) 0.14693(4) 0.01612(14) Uani 1 1 d . . . P2 P 0.26165(5) -0.26273(6) 0.10442(3) 0.01354(13) Uani 1 1 d . . . Si1 Si 0.65063(6) -0.30562(7) 0.09581(4) 0.02039(17) Uani 1 1 d . . . Si2 Si 0.13769(6) -0.19304(7) -0.04108(4) 0.01850(16) Uani 1 1 d . . . O1 O 0.2732(2) -0.4039(3) 0.28944(13) 0.0421(7) Uani 1 1 d . . . O2 O 0.4268(2) -0.5573(2) 0.12068(17) 0.0378(7) Uani 1 1 d . . . O3 O 0.1200(2) -0.5062(2) -0.01582(12) 0.0322(5) Uani 1 1 d . . . O4 O -0.03511(19) -0.3702(2) 0.15301(14) 0.0362(6) Uani 1 1 d . . . O5 O 0.1334(2) -0.6860(2) 0.17694(16) 0.0414(7) Uani 1 1 d . . . C1 C 0.5013(2) -0.2843(2) 0.07719(15) 0.0176(5) Uani 1 1 d . . . C2 C 0.4536(2) -0.3032(2) 0.01491(15) 0.0188(5) Uani 1 1 d . . . H2 H 0.4954 -0.3417 -0.0139 0.023 Uiso 1 1 calc R . . C3 C 0.3463(2) -0.2728(2) -0.01431(14) 0.0183(5) Uani 1 1 d . . . H3 H 0.3355 -0.2761 -0.0617 0.022 Uiso 1 1 calc R . . C4 C 0.2602(2) -0.2406(2) 0.01518(13) 0.0146(5) Uani 1 1 d . . . C5 C 0.4542(2) -0.0941(2) 0.14905(14) 0.0169(5) Uani 1 1 d . . . C6 C 0.4409(3) -0.0405(3) 0.20893(18) 0.0263(7) Uani 1 1 d . . . H6 H 0.4241 -0.0811 0.2466 0.032 Uiso 1 1 calc R . . C7 C 0.4523(3) 0.0719(3) 0.2133(2) 0.0372(9) Uani 1 1 d . . . H7 H 0.4433 0.1083 0.2539 0.045 Uiso 1 1 calc R . . C8 C 0.4766(3) 0.1306(3) 0.1588(2) 0.0379(9) Uani 1 1 d . . . H8 H 0.4840 0.2076 0.1621 0.046 Uiso 1 1 calc R . . C9 C 0.4903(3) 0.0798(3) 0.0996(2) 0.0355(8) Uani 1 1 d . . . H9 H 0.5070 0.1214 0.0623 0.043 Uiso 1 1 calc R . . C10 C 0.4795(3) -0.0332(3) 0.09458(17) 0.0253(7) Uani 1 1 d . . . H10 H 0.4894 -0.0688 0.0538 0.030 Uiso 1 1 calc R . . C11 C 0.2003(2) -0.1427(3) 0.13793(13) 0.0160(5) Uani 1 1 d . . . C12 C 0.2130(3) -0.0402(2) 0.11000(16) 0.0199(6) Uani 1 1 d . . . H12 H 0.2489 -0.0337 0.0711 0.024 Uiso 1 1 calc R . . C13 C 0.1737(3) 0.0526(2) 0.13836(17) 0.0242(7) Uani 1 1 d . . . H13 H 0.1822 0.1221 0.1186 0.029 Uiso 1 1 calc R . . C14 C 0.1222(3) 0.0439(3) 0.19563(19) 0.0294(8) Uani 1 1 d . . . H14 H 0.0959 0.1075 0.2154 0.035 Uiso 1 1 calc R . . C15 C 0.1092(3) -0.0573(3) 0.22390(18) 0.0298(8) Uani 1 1 d . . . H15 H 0.0734 -0.0633 0.2630 0.036 Uiso 1 1 calc R . . C16 C 0.1482(3) -0.1504(3) 0.19550(15) 0.0217(6) Uani 1 1 d . . . H16 H 0.1394 -0.2197 0.2154 0.026 Uiso 1 1 calc R . . C17 C 0.7032(3) -0.2217(3) 0.1693(2) 0.0336(8) Uani 1 1 d . . . H17A H 0.6649 -0.2403 0.2076 0.050 Uiso 1 1 calc R . . H17B H 0.6930 -0.1441 0.1586 0.050 Uiso 1 1 calc R . . H17C H 0.7795 -0.2366 0.1803 0.050 Uiso 1 1 calc R . . C18 C 0.7143(3) -0.2591(3) 0.02132(19) 0.0327(8) Uani 1 1 d . . . H18A H 0.7921 -0.2641 0.0307 0.049 Uiso 1 1 calc R . . H18B H 0.6939 -0.1833 0.0110 0.049 Uiso 1 1 calc R . . H18C H 0.6903 -0.3056 -0.0170 0.049 Uiso 1 1 calc R . . C19 C 0.6767(3) -0.4538(3) 0.1122(2) 0.0339(8) Uani 1 1 d . . . H19A H 0.7532 -0.4652 0.1246 0.051 Uiso 1 1 calc R . . H19B H 0.6536 -0.4957 0.0718 0.051 Uiso 1 1 calc R . . H19C H 0.6370 -0.4781 0.1487 0.051 Uiso 1 1 calc R . . C20 C 0.1526(3) -0.0466(3) -0.0642(2) 0.0326(8) Uani 1 1 d . . . H20A H 0.0996 -0.0282 -0.1018 0.049 Uiso 1 1 calc R . . H20B H 0.2245 -0.0344 -0.0772 0.049 Uiso 1 1 calc R . . H20C H 0.1417 -0.0003 -0.0259 0.049 Uiso 1 1 calc R . . C21 C 0.0136(2) -0.2142(3) 0.00026(18) 0.0298(7) Uani 1 1 d . . . H21A H -0.0487 -0.1930 -0.0305 0.045 Uiso 1 1 calc R . . H21B H 0.0166 -0.1694 0.0407 0.045 Uiso 1 1 calc R . . H21C H 0.0076 -0.2914 0.0122 0.045 Uiso 1 1 calc R . . C22 C 0.1308(3) -0.2756(3) -0.11922(16) 0.0277(7) Uani 1 1 d . . . H22A H 0.1229 -0.3530 -0.1083 0.042 Uiso 1 1 calc R . . H22B H 0.1965 -0.2653 -0.1405 0.042 Uiso 1 1 calc R . . H22C H 0.0694 -0.2520 -0.1499 0.042 Uiso 1 1 calc R . . C23 C 0.2484(3) -0.4190(3) 0.23420(16) 0.0236(6) Uani 1 1 d . . . C24 C 0.3481(3) -0.5147(3) 0.12539(16) 0.0228(6) Uani 1 1 d . . . C25 C 0.1501(2) -0.4854(3) 0.03825(16) 0.0212(6) Uani 1 1 d . . . C26 C 0.0491(2) -0.3960(3) 0.14687(15) 0.0220(6) Uani 1 1 d . . . C27 C 0.1575(3) -0.6008(3) 0.16184(18) 0.0265(7) Uani 1 1 d . . . 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 0.01536(8) 0.01056(8) 0.02121(7) 0.00070(4) 0.00479(5) -0.00110(4) P1 0.0148(3) 0.0141(3) 0.0196(3) 0.0006(3) 0.0026(2) -0.0001(3) P2 0.0135(3) 0.0101(3) 0.0177(3) 0.0001(2) 0.0050(2) -0.0002(2) Si1 0.0119(3) 0.0185(4) 0.0308(4) -0.0020(3) 0.0027(3) 0.0006(3) Si2 0.0163(4) 0.0194(4) 0.0198(4) 0.0018(3) 0.0015(3) 0.0014(3) O1 0.0449(16) 0.0564(19) 0.0244(12) -0.0030(12) 0.0008(11) 0.0033(14) O2 0.0264(13) 0.0319(15) 0.0559(19) -0.0079(12) 0.0082(13) 0.0089(10) O3 0.0343(13) 0.0329(14) 0.0293(12) -0.0081(11) 0.0023(10) -0.0008(11) O4 0.0209(11) 0.0442(16) 0.0451(15) 0.0010(12) 0.0114(10) 0.0046(11) O5 0.0416(15) 0.0177(12) 0.0637(19) 0.0113(12) 0.0000(13) -0.0089(11) C1 0.0161(12) 0.0131(12) 0.0243(13) 0.0000(10) 0.0052(10) 0.0010(10) C2 0.0145(12) 0.0164(13) 0.0266(14) -0.0029(11) 0.0077(10) -0.0005(10) C3 0.0171(13) 0.0196(14) 0.0184(12) -0.0024(10) 0.0026(10) -0.0014(11) C4 0.0159(12) 0.0091(12) 0.0190(12) 0.0004(9) 0.0025(9) -0.0014(10) C5 0.0161(12) 0.0125(13) 0.0219(13) -0.0031(10) 0.0014(10) -0.0017(10) C6 0.0295(17) 0.0267(18) 0.0230(15) -0.0072(12) 0.0042(13) -0.0041(13) C7 0.039(2) 0.0280(18) 0.044(2) -0.0199(17) 0.0047(17) -0.0049(16) C8 0.040(2) 0.0164(16) 0.057(2) -0.0111(15) 0.0038(18) -0.0057(14) C9 0.047(2) 0.0163(15) 0.044(2) 0.0044(15) 0.0067(17) -0.0105(16) C10 0.0308(17) 0.0203(15) 0.0258(15) -0.0019(12) 0.0080(13) -0.0068(13) C11 0.0156(13) 0.0127(14) 0.0203(13) -0.0012(9) 0.0042(10) 0.0015(10) C12 0.0203(14) 0.0162(14) 0.0235(14) 0.0018(10) 0.0034(11) 0.0023(10) C13 0.0300(16) 0.0147(16) 0.0276(16) 0.0013(11) 0.0011(13) 0.0041(12) C14 0.040(2) 0.0169(16) 0.0325(18) -0.0047(12) 0.0068(15) 0.0085(13) C15 0.041(2) 0.0227(17) 0.0284(16) -0.0021(12) 0.0155(15) 0.0071(13) C16 0.0276(15) 0.0166(14) 0.0222(13) 0.0003(11) 0.0086(11) 0.0022(12) C17 0.0198(15) 0.037(2) 0.043(2) -0.0114(16) -0.0035(13) 0.0002(14) C18 0.0176(14) 0.037(2) 0.045(2) 0.0038(16) 0.0098(14) -0.0024(14) C19 0.0232(16) 0.0249(19) 0.054(2) 0.0039(15) 0.0077(16) 0.0066(13) C20 0.041(2) 0.0225(18) 0.0328(18) 0.0057(13) -0.0012(16) 0.0022(14) C21 0.0176(14) 0.039(2) 0.0327(17) 0.0030(14) 0.0020(12) 0.0059(13) C22 0.0305(16) 0.0268(17) 0.0248(15) -0.0018(12) -0.0020(12) -0.0015(13) C23 0.0233(15) 0.0221(15) 0.0263(15) 0.0010(12) 0.0070(12) 0.0024(13) C24 0.0222(15) 0.0168(14) 0.0299(15) -0.0027(12) 0.0042(12) -0.0023(12) C25 0.0182(13) 0.0140(14) 0.0320(16) -0.0039(12) 0.0059(11) -0.0009(11) C26 0.0223(14) 0.0196(14) 0.0248(14) 0.0039(11) 0.0066(11) -0.0038(12) C27 0.0226(15) 0.0188(15) 0.0379(17) 0.0027(13) 0.0022(13) -0.0001(12) _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 W1 C27 2.004(3) . ? W1 C25 2.041(3) . ? W1 C23 2.048(3) . ? W1 C24 2.052(3) . ? W1 C26 2.054(3) . ? W1 P2 2.5277(7) . ? P1 C1 1.817(3) . ? P1 C5 1.828(3) . ? P1 P2 2.2269(10) . ? P2 C4 1.815(3) . ? P2 C11 1.824(3) . ? Si1 C18 1.864(4) . ? Si1 C17 1.864(4) . ? Si1 C19 1.867(3) . ? Si1 C1 1.896(3) . ? Si2 C22 1.865(3) . ? Si2 C21 1.867(3) . ? Si2 C20 1.868(3) . ? Si2 C4 1.905(3) . ? O1 C23 1.138(4) . ? O2 C24 1.134(4) . ? O3 C25 1.143(4) . ? O4 C26 1.126(4) . ? O5 C27 1.137(4) . ? C1 C2 1.352(4) . ? C2 C3 1.463(4) . ? C2 H2 0.9500 . ? C3 C4 1.351(4) . ? C3 H3 0.9500 . ? C5 C10 1.390(4) . ? C5 C6 1.399(4) . ? C6 C7 1.386(5) . ? C6 H6 0.9500 . ? C7 C8 1.373(6) . ? C7 H7 0.9500 . ? C8 C9 1.372(6) . ? C8 H8 0.9500 . ? C9 C10 1.394(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.392(4) . ? C11 C16 1.395(4) . ? C12 C13 1.387(4) . ? C12 H12 0.9500 . ? C13 C14 1.387(5) . ? C13 H13 0.9500 . ? C14 C15 1.381(5) . ? C14 H14 0.9500 . ? C15 C16 1.389(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 C27 W1 C25 89.72(13) . . ? C27 W1 C23 88.85(14) . . ? C25 W1 C23 178.50(12) . . ? C27 W1 C24 86.99(13) . . ? C25 W1 C24 90.75(12) . . ? C23 W1 C24 89.60(13) . . ? C27 W1 C26 89.47(13) . . ? C25 W1 C26 88.77(12) . . ? C23 W1 C26 90.80(12) . . ? C24 W1 C26 176.43(12) . . ? C27 W1 P2 177.76(9) . . ? C25 W1 P2 91.35(9) . . ? C23 W1 P2 90.10(10) . . ? C24 W1 P2 91.03(9) . . ? C26 W1 P2 92.52(9) . . ? C1 P1 C5 102.34(13) . . ? C1 P1 P2 101.29(10) . . ? C5 P1 P2 105.67(9) . . ? C4 P2 C11 106.67(12) . . ? C4 P2 P1 105.70(9) . . ? C11 P2 P1 100.93(9) . . ? C4 P2 W1 114.23(9) . . ? C11 P2 W1 119.21(9) . . ? P1 P2 W1 108.52(3) . . ? C18 Si1 C17 108.85(18) . . ? C18 Si1 C19 110.82(19) . . ? C17 Si1 C19 110.8(2) . . ? C18 Si1 C1 107.62(14) . . ? C17 Si1 C1 109.98(14) . . ? C19 Si1 C1 108.68(15) . . ? C22 Si2 C21 109.57(16) . . ? C22 Si2 C20 107.95(17) . . ? C21 Si2 C20 110.87(18) . . ? C22 Si2 C4 107.28(14) . . ? C21 Si2 C4 110.89(14) . . ? C20 Si2 C4 110.17(15) . . ? C2 C1 P1 124.1(2) . . ? C2 C1 Si1 119.6(2) . . ? P1 C1 Si1 116.32(16) . . ? C1 C2 C3 129.0(3) . . ? C1 C2 H2 115.5 . . ? C3 C2 H2 115.5 . . ? C4 C3 C2 130.4(3) . . ? C4 C3 H3 114.8 . . ? C2 C3 H3 114.8 . . ? C3 C4 P2 117.9(2) . . ? C3 C4 Si2 117.8(2) . . ? P2 C4 Si2 123.76(15) . . ? C10 C5 C6 119.1(3) . . ? C10 C5 P1 124.1(2) . . ? C6 C5 P1 116.8(2) . . ? C7 C6 C5 120.0(3) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C6 120.0(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.6(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C5 C10 C9 120.2(3) . . ? C5 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C16 118.7(3) . . ? C12 C11 P2 120.4(2) . . ? C16 C11 P2 120.6(2) . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 120.0(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 119.8(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.3(3) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.4(3) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 C23 W1 177.9(3) . . ? O2 C24 W1 175.0(3) . . ? O3 C25 W1 178.4(3) . . ? O4 C26 W1 177.3(3) . . ? O5 C27 W1 179.7(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.914 _refine_diff_density_min -2.088 _refine_diff_density_rms 0.282