# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Sally Freeman' 'Christopher J. Barker' 'Elena V. Bichenkova' 'Alexander Blake' 'Richard Bryce' 'Alvaro Diaz' 'Laura Etchells' 'Carlos Kremer' 'David Mansell' 'Nicholas Rattray' 'C. Schwalbe' _publ_contact_author_name 'Dr Sally Freeman ' _publ_contact_author_email SALLY.FREEMAN@MANCHESTER.AC.UK _publ_section_title ; Fluorescent probe: Complexation of Fe3+ with the myo-inositol 1,2,3-trisphosphate motif ; # Attachment 'inopyr.cif' #Fluorescent probe: #Complexation of Fe3+ with the myo-inositol 1,2,3-trisphosphate motif data_inopyr _database_code_depnum_ccdc_archive 'CCDC 690016' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H40 O8 Si, C H Cl3' _chemical_formula_sum 'C48 H41 Cl3 O8 Si' _chemical_formula_weight 880.25 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1679(9) _cell_length_b 11.6838(9) _cell_length_c 16.9249(13) _cell_angle_alpha 72.420(2) _cell_angle_beta 81.387(2) _cell_angle_gamma 87.634(2) _cell_volume 2081.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4524 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.0 _exptl_crystal_description sphenoid _exptl_crystal_colour yellow _exptl_crystal_size_min 0.34 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_max 0.90 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.306 _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 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18993 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.45 _reflns_number_total 9307 _reflns_number_gt 6716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP(Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick,2008);PLATON(Spek,2003)' _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^)+(0.0433P)^2^+0.1286P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9307 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Si1 Si 0.22218(4) 0.48299(4) 0.84222(3) 0.02666(11) Uani 1 1 d . . . O1 O 0.50445(10) 0.20716(11) 0.85636(7) 0.0351(3) Uani 1 1 d . . . O2 O 0.34214(9) 0.40225(10) 0.87396(6) 0.0278(2) Uani 1 1 d . . . O3 O 0.56543(10) 0.31180(11) 0.93986(7) 0.0337(3) Uani 1 1 d . . . O4 O 0.67477(9) 0.56886(11) 0.76345(7) 0.0297(3) Uani 1 1 d . . . O5 O 0.70938(10) 0.24372(12) 0.84950(8) 0.0390(3) Uani 1 1 d . . . O6 O 0.59170(9) 0.44491(11) 0.66371(7) 0.0318(3) Uani 1 1 d . . . O7 O 0.87663(10) 0.58291(13) 0.75631(7) 0.0441(3) Uani 1 1 d . . . O8 O 0.76752(11) 0.41177(13) 0.59214(8) 0.0464(3) Uani 1 1 d . . . C1 C 0.49084(14) 0.31503(15) 0.78976(10) 0.0290(3) Uani 1 1 d . . . H1 H 0.4258 0.3035 0.7582 0.035 Uiso 1 1 calc R . . C2 C 0.45858(12) 0.42019(14) 0.82483(9) 0.0242(3) Uani 1 1 d . . . H2 H 0.4593 0.4965 0.7777 0.029 Uiso 1 1 calc R . . C3 C 0.55471(13) 0.42630(16) 0.87857(10) 0.0279(3) Uani 1 1 d . . . H3 H 0.5329 0.4893 0.9071 0.034 Uiso 1 1 calc R . . C4 C 0.67928(13) 0.45375(16) 0.82516(10) 0.0291(4) Uani 1 1 d . . . H4 H 0.7419 0.4549 0.8614 0.035 Uiso 1 1 calc R . . C5 C 0.70824(14) 0.35515(16) 0.78317(10) 0.0312(4) Uani 1 1 d . . . H5 H 0.7892 0.3702 0.7474 0.037 Uiso 1 1 calc R . . C6 C 0.61147(14) 0.33965(16) 0.73156(10) 0.0305(4) Uani 1 1 d . . . H6 H 0.6328 0.2702 0.7093 0.037 Uiso 1 1 calc R . . C7 C 0.59595(14) 0.22107(17) 0.90113(11) 0.0366(4) Uani 1 1 d . . . H7 H 0.6023 0.1438 0.9464 0.044 Uiso 1 1 calc R . . C8 C 0.23581(16) 0.5266(2) 0.72580(11) 0.0447(5) Uani 1 1 d . . . H8A H 0.3010 0.5859 0.7010 0.067 Uiso 1 1 calc R . . H8B H 0.1593 0.5614 0.7081 0.067 Uiso 1 1 calc R . . H8C H 0.2544 0.4554 0.7071 0.067 Uiso 1 1 calc R . . C9 C 0.08920(15) 0.38425(18) 0.89112(12) 0.0406(4) Uani 1 1 d . . . H9A H 0.1006 0.3091 0.8765 0.061 Uiso 1 1 calc R . . H9B H 0.0162 0.4246 0.8707 0.061 Uiso 1 1 calc R . . H9C H 0.0803 0.3667 0.9521 0.061 Uiso 1 1 calc R . . C10 C 0.21555(14) 0.62109(16) 0.87782(11) 0.0319(4) Uani 1 1 d . . . C11 C 0.09748(17) 0.68906(19) 0.85769(13) 0.0461(5) Uani 1 1 d . . . H11A H 0.0949 0.7627 0.8742 0.069 Uiso 1 1 calc R . . H11B H 0.0279 0.6381 0.8886 0.069 Uiso 1 1 calc R . . H11C H 0.0944 0.7097 0.7974 0.069 Uiso 1 1 calc R . . C12 C 0.21604(18) 0.5839(2) 0.97305(12) 0.0456(5) Uani 1 1 d . . . H12A H 0.2913 0.5412 0.9865 0.068 Uiso 1 1 calc R . . H12B H 0.1467 0.5311 1.0014 0.068 Uiso 1 1 calc R . . H12C H 0.2105 0.6556 0.9919 0.068 Uiso 1 1 calc R . . C13 C 0.32400(17) 0.70486(19) 0.83454(14) 0.0496(5) Uani 1 1 d . . . H13A H 0.3247 0.7292 0.7738 0.074 Uiso 1 1 calc R . . H13B H 0.3993 0.6626 0.8483 0.074 Uiso 1 1 calc R . . H13C H 0.3172 0.7762 0.8539 0.074 Uiso 1 1 calc R . . C14 C 0.78478(14) 0.62295(17) 0.72810(10) 0.0304(4) Uani 1 1 d . . . C15 C 0.77351(13) 0.72727(15) 0.65464(10) 0.0278(3) Uani 1 1 d . . . C16 C 0.87196(13) 0.76423(15) 0.58903(10) 0.0252(3) Uani 1 1 d . . . C17 C 0.98635(13) 0.70277(15) 0.58773(10) 0.0276(3) Uani 1 1 d . . . H17 H 0.9984 0.6341 0.6332 0.033 Uiso 1 1 calc R . . C18 C 1.07718(14) 0.74089(16) 0.52299(10) 0.0286(3) Uani 1 1 d . . . H18 H 1.1516 0.6985 0.5244 0.034 Uiso 1 1 calc R . . C19 C 1.06417(13) 0.84271(15) 0.45294(10) 0.0264(3) Uani 1 1 d . . . C20 C 1.15709(14) 0.88239(16) 0.38528(10) 0.0326(4) Uani 1 1 d . . . H20 H 1.2318 0.8404 0.3856 0.039 Uiso 1 1 calc R . . C21 C 1.14173(16) 0.98155(17) 0.31825(11) 0.0361(4) Uani 1 1 d . . . H21 H 1.2060 1.0077 0.2732 0.043 Uiso 1 1 calc R . . C22 C 1.03285(16) 1.04300(16) 0.31641(11) 0.0350(4) Uani 1 1 d . . . H22 H 1.0235 1.1114 0.2701 0.042 Uiso 1 1 calc R . . C23 C 0.93638(14) 1.00595(15) 0.38160(10) 0.0294(4) Uani 1 1 d . . . C24 C 0.82148(15) 1.06547(16) 0.38050(11) 0.0338(4) Uani 1 1 d . . . H24 H 0.8098 1.1331 0.3342 0.041 Uiso 1 1 calc R . . C25 C 0.72952(15) 1.02747(16) 0.44383(11) 0.0342(4) Uani 1 1 d . . . H25 H 0.6544 1.0687 0.4411 0.041 Uiso 1 1 calc R . . C26 C 0.74270(14) 0.92597(15) 0.51529(10) 0.0282(3) Uani 1 1 d . . . C27 C 0.64803(14) 0.88529(17) 0.58132(11) 0.0339(4) Uani 1 1 d . . . H27 H 0.5724 0.9256 0.5793 0.041 Uiso 1 1 calc R . . C28 C 0.66285(14) 0.78800(16) 0.64889(11) 0.0321(4) Uani 1 1 d . . . H28 H 0.5969 0.7614 0.6925 0.039 Uiso 1 1 calc R . . C29 C 0.85545(13) 0.86461(15) 0.51914(10) 0.0252(3) Uani 1 1 d . . . C30 C 0.95228(13) 0.90490(15) 0.45118(10) 0.0259(3) Uani 1 1 d . . . C31 C 0.67695(14) 0.47187(16) 0.59455(10) 0.0309(4) Uani 1 1 d . . . C32 C 0.64261(14) 0.57740(16) 0.52809(10) 0.0291(4) Uani 1 1 d . . . C33 C 0.72594(13) 0.63558(15) 0.45600(10) 0.0273(3) Uani 1 1 d . . . C34 C 0.85127(13) 0.60049(16) 0.44229(10) 0.0296(4) Uani 1 1 d . . . H34 H 0.8813 0.5348 0.4829 0.036 Uiso 1 1 calc R . . C35 C 0.92649(14) 0.65955(16) 0.37261(11) 0.0317(4) Uani 1 1 d . . . H35 H 1.0084 0.6344 0.3660 0.038 Uiso 1 1 calc R . . C36 C 0.88737(14) 0.75820(16) 0.30863(10) 0.0308(4) Uani 1 1 d . . . C37 C 0.96420(16) 0.81947(17) 0.23607(11) 0.0381(4) Uani 1 1 d . . . H37 H 1.0463 0.7953 0.2283 0.046 Uiso 1 1 calc R . . C38 C 0.92280(17) 0.91436(18) 0.17564(12) 0.0424(4) Uani 1 1 d . . . H38 H 0.9761 0.9539 0.1264 0.051 Uiso 1 1 calc R . . C39 C 0.80385(17) 0.95237(18) 0.18637(12) 0.0406(4) Uani 1 1 d . . . H39 H 0.7762 1.0178 0.1444 0.049 Uiso 1 1 calc R . . C40 C 0.72418(15) 0.89529(16) 0.25844(11) 0.0338(4) Uani 1 1 d . . . C41 C 0.60104(16) 0.93500(17) 0.27188(12) 0.0370(4) Uani 1 1 d . . . H41 H 0.5729 1.0019 0.2312 0.044 Uiso 1 1 calc R . . C42 C 0.52540(15) 0.87850(17) 0.34134(12) 0.0353(4) Uani 1 1 d . . . H42 H 0.4447 0.9066 0.3486 0.042 Uiso 1 1 calc R . . C43 C 0.56298(14) 0.77719(16) 0.40459(11) 0.0312(4) Uani 1 1 d . . . C44 C 0.48440(14) 0.71717(17) 0.47665(11) 0.0341(4) Uani 1 1 d . . . H44 H 0.4031 0.7437 0.4844 0.041 Uiso 1 1 calc R . . C45 C 0.52333(14) 0.62045(17) 0.53628(11) 0.0326(4) Uani 1 1 d . . . H45 H 0.4680 0.5815 0.5845 0.039 Uiso 1 1 calc R . . C46 C 0.68469(13) 0.73522(15) 0.39408(10) 0.0278(3) Uani 1 1 d . . . C47 C 0.76456(14) 0.79658(15) 0.32035(10) 0.0287(3) Uani 1 1 d . . . Cl1 Cl 0.42107(5) 0.07991(6) 1.10110(4) 0.06001(16) Uani 1 1 d . A . Cl2 Cl 0.23034(12) 0.25517(16) 1.11143(9) 0.0545(4) Uani 0.760(9) 1 d P A 1 Cl3 Cl 0.21611(19) 0.08715(17) 1.01903(12) 0.0686(5) Uani 0.760(9) 1 d P A 1 Cl2P Cl 0.291(2) 0.2752(6) 1.1099(4) 0.127(5) Uani 0.240(9) 1 d P A 2 Cl3P Cl 0.1840(10) 0.1097(13) 1.0489(10) 0.156(5) Uani 0.240(9) 1 d P A 2 C48 C 0.31419(15) 0.17544(17) 1.04926(11) 0.0376(4) Uani 1 1 d . . . H48 H 0.3572 0.2341 0.9978 0.045 Uiso 0.760(9) 1 calc PR A 1 H48P H 0.3506 0.2190 0.9906 0.045 Uiso 0.240(9) 1 calc PR A 2 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 Si1 0.0220(2) 0.0325(3) 0.0246(2) -0.00697(19) -0.00491(16) 0.00264(17) O1 0.0332(6) 0.0274(7) 0.0396(7) -0.0028(5) -0.0053(5) 0.0016(5) O2 0.0218(5) 0.0312(6) 0.0259(6) -0.0036(5) -0.0002(4) 0.0021(4) O3 0.0305(6) 0.0403(7) 0.0239(6) 0.0010(5) -0.0061(5) 0.0007(5) O4 0.0234(5) 0.0332(7) 0.0286(6) -0.0034(5) -0.0030(4) -0.0036(5) O5 0.0296(6) 0.0383(7) 0.0379(7) 0.0031(6) -0.0030(5) 0.0100(5) O6 0.0312(6) 0.0380(7) 0.0245(6) -0.0085(5) -0.0029(5) 0.0082(5) O7 0.0261(6) 0.0624(9) 0.0335(7) 0.0041(6) -0.0095(5) -0.0062(6) O8 0.0424(7) 0.0473(9) 0.0385(7) -0.0040(6) 0.0051(6) 0.0194(6) C1 0.0274(8) 0.0291(9) 0.0296(8) -0.0070(7) -0.0063(6) 0.0029(7) C2 0.0216(7) 0.0269(9) 0.0213(7) -0.0039(6) -0.0017(6) 0.0019(6) C3 0.0269(7) 0.0330(9) 0.0219(8) -0.0050(7) -0.0033(6) -0.0010(7) C4 0.0223(7) 0.0371(10) 0.0243(8) -0.0027(7) -0.0052(6) -0.0010(7) C5 0.0241(7) 0.0343(10) 0.0278(8) -0.0001(7) -0.0015(6) 0.0051(7) C6 0.0318(8) 0.0295(9) 0.0289(8) -0.0086(7) -0.0031(7) 0.0070(7) C7 0.0310(8) 0.0344(10) 0.0351(9) 0.0032(8) -0.0053(7) 0.0055(7) C8 0.0385(9) 0.0660(14) 0.0318(9) -0.0157(10) -0.0130(8) 0.0121(9) C9 0.0279(8) 0.0451(12) 0.0492(11) -0.0143(9) -0.0056(8) -0.0023(8) C10 0.0318(8) 0.0294(9) 0.0335(9) -0.0077(7) -0.0068(7) 0.0054(7) C11 0.0432(10) 0.0392(12) 0.0533(12) -0.0098(10) -0.0111(9) 0.0139(9) C12 0.0534(11) 0.0517(13) 0.0403(11) -0.0243(10) -0.0143(9) 0.0113(10) C13 0.0432(10) 0.0344(11) 0.0689(14) -0.0125(10) -0.0070(10) -0.0007(9) C14 0.0247(8) 0.0383(10) 0.0268(8) -0.0078(7) -0.0021(6) -0.0057(7) C15 0.0245(7) 0.0302(9) 0.0299(8) -0.0091(7) -0.0063(6) -0.0026(6) C16 0.0243(7) 0.0258(8) 0.0268(8) -0.0081(7) -0.0063(6) -0.0028(6) C17 0.0264(7) 0.0269(9) 0.0281(8) -0.0045(7) -0.0077(6) 0.0014(6) C18 0.0245(7) 0.0313(9) 0.0310(8) -0.0100(7) -0.0060(6) 0.0029(6) C19 0.0261(7) 0.0276(9) 0.0268(8) -0.0090(7) -0.0061(6) -0.0014(6) C20 0.0283(8) 0.0366(10) 0.0334(9) -0.0119(8) -0.0033(7) -0.0005(7) C21 0.0370(9) 0.0403(11) 0.0282(9) -0.0077(8) 0.0001(7) -0.0059(8) C22 0.0452(10) 0.0304(10) 0.0271(8) -0.0031(7) -0.0085(7) -0.0042(8) C23 0.0342(8) 0.0290(9) 0.0273(8) -0.0092(7) -0.0100(7) -0.0015(7) C24 0.0403(9) 0.0270(9) 0.0334(9) -0.0032(7) -0.0152(7) 0.0015(7) C25 0.0318(8) 0.0309(10) 0.0434(10) -0.0119(8) -0.0158(8) 0.0062(7) C26 0.0278(8) 0.0259(9) 0.0337(9) -0.0106(7) -0.0098(7) 0.0009(6) C27 0.0222(7) 0.0374(10) 0.0454(10) -0.0163(8) -0.0077(7) 0.0039(7) C28 0.0241(8) 0.0349(10) 0.0366(9) -0.0108(8) -0.0012(7) -0.0033(7) C29 0.0252(7) 0.0251(8) 0.0285(8) -0.0108(7) -0.0080(6) -0.0002(6) C30 0.0283(7) 0.0259(9) 0.0261(8) -0.0088(7) -0.0088(6) -0.0022(6) C31 0.0303(8) 0.0363(10) 0.0278(8) -0.0136(8) -0.0020(7) 0.0032(7) C32 0.0295(8) 0.0347(10) 0.0276(8) -0.0154(7) -0.0069(7) 0.0045(7) C33 0.0279(7) 0.0314(9) 0.0279(8) -0.0152(7) -0.0086(6) 0.0034(7) C34 0.0277(8) 0.0340(10) 0.0309(9) -0.0135(7) -0.0098(7) 0.0060(7) C35 0.0255(8) 0.0369(10) 0.0364(9) -0.0155(8) -0.0071(7) 0.0038(7) C36 0.0310(8) 0.0329(10) 0.0328(9) -0.0150(8) -0.0073(7) -0.0003(7) C37 0.0364(9) 0.0393(11) 0.0399(10) -0.0150(9) -0.0021(8) -0.0026(8) C38 0.0466(10) 0.0405(11) 0.0362(10) -0.0078(9) -0.0002(8) -0.0058(9) C39 0.0517(11) 0.0339(10) 0.0352(10) -0.0063(8) -0.0108(8) -0.0022(8) C40 0.0389(9) 0.0314(10) 0.0360(9) -0.0136(8) -0.0125(7) -0.0007(7) C41 0.0432(9) 0.0301(10) 0.0415(10) -0.0102(8) -0.0208(8) 0.0057(8) C42 0.0324(8) 0.0349(10) 0.0455(10) -0.0175(8) -0.0178(8) 0.0089(7) C43 0.0298(8) 0.0353(10) 0.0350(9) -0.0171(8) -0.0120(7) 0.0044(7) C44 0.0265(8) 0.0430(11) 0.0370(9) -0.0175(8) -0.0090(7) 0.0091(7) C45 0.0290(8) 0.0408(10) 0.0299(9) -0.0144(8) -0.0037(7) 0.0052(7) C46 0.0286(8) 0.0308(9) 0.0298(8) -0.0150(7) -0.0105(7) 0.0029(7) C47 0.0317(8) 0.0281(9) 0.0301(8) -0.0119(7) -0.0097(7) 0.0008(7) Cl1 0.0526(3) 0.0569(4) 0.0551(3) 0.0072(3) -0.0136(2) 0.0147(3) Cl2 0.0632(8) 0.0553(7) 0.0390(5) -0.0105(4) -0.0018(4) 0.0200(4) Cl3 0.0691(9) 0.0628(7) 0.0829(9) -0.0248(7) -0.0308(7) -0.0073(6) Cl2P 0.236(13) 0.061(3) 0.069(2) -0.025(2) 0.031(5) 0.033(5) Cl3P 0.079(4) 0.156(8) 0.172(8) 0.060(6) -0.039(5) -0.065(4) C48 0.0389(9) 0.0349(10) 0.0323(9) -0.0011(8) -0.0048(7) 0.0041(8) _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 Si1 O2 1.6669(11) . ? Si1 C9 1.8488(18) . ? Si1 C8 1.8643(18) . ? Si1 C10 1.8804(18) . ? O1 C7 1.402(2) . ? O1 C1 1.435(2) . ? O2 C2 1.4211(17) . ? O3 C7 1.412(2) . ? O3 C3 1.437(2) . ? O4 C14 1.3720(18) . ? O4 C4 1.437(2) . ? O5 C7 1.4124(19) . ? O5 C5 1.441(2) . ? O6 C31 1.3580(19) . ? O6 C6 1.442(2) . ? O7 C14 1.213(2) . ? O8 C31 1.210(2) . ? C1 C6 1.527(2) . ? C1 C2 1.527(2) . ? C1 H1 1.0000 . ? C2 C3 1.524(2) . ? C2 H2 1.0000 . ? C3 C4 1.530(2) . ? C3 H3 1.0000 . ? C4 C5 1.527(2) . ? C4 H4 1.0000 . ? C5 C6 1.536(2) . ? C5 H5 1.0000 . ? C6 H6 1.0000 . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C13 1.536(2) . ? C10 C12 1.538(2) . ? C10 C11 1.539(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.472(2) . ? C15 C28 1.401(2) . ? C15 C16 1.419(2) . ? C16 C29 1.421(2) . ? C16 C17 1.440(2) . ? C17 C18 1.356(2) . ? C17 H17 0.9500 . ? C18 C19 1.424(2) . ? C18 H18 0.9500 . ? C19 C20 1.402(2) . ? C19 C30 1.419(2) . ? C20 C21 1.381(3) . ? C20 H20 0.9500 . ? C21 C22 1.386(3) . ? C21 H21 0.9500 . ? C22 C23 1.400(2) . ? C22 H22 0.9500 . ? C23 C30 1.420(2) . ? C23 C24 1.434(2) . ? C24 C25 1.349(2) . ? C24 H24 0.9500 . ? C25 C26 1.436(2) . ? C25 H25 0.9500 . ? C26 C27 1.400(2) . ? C26 C29 1.423(2) . ? C27 C28 1.372(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.434(2) . ? C31 C32 1.478(2) . ? C32 C45 1.406(2) . ? C32 C33 1.424(2) . ? C33 C46 1.424(2) . ? C33 C34 1.447(2) . ? C34 C35 1.354(2) . ? C34 H34 0.9500 . ? C35 C36 1.428(2) . ? C35 H35 0.9500 . ? C36 C37 1.400(2) . ? C36 C47 1.429(2) . ? C37 C38 1.380(3) . ? C37 H37 0.9500 . ? C38 C39 1.387(3) . ? C38 H38 0.9500 . ? C39 C40 1.399(2) . ? C39 H39 0.9500 . ? C40 C47 1.414(2) . ? C40 C41 1.441(2) . ? C41 C42 1.346(3) . ? C41 H41 0.9500 . ? C42 C43 1.432(2) . ? C42 H42 0.9500 . ? C43 C44 1.401(2) . ? C43 C46 1.430(2) . ? C44 C45 1.374(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.430(2) . ? Cl1 C48 1.7471(19) . ? Cl2 C48 1.754(2) . ? Cl3 C48 1.762(2) . ? Cl2P C48 1.759(7) . ? Cl3P C48 1.674(7) . ? C48 H48 1.0000 . ? C48 H48P 1.0000 . ? 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 O2 Si1 C9 105.80(8) . . ? O2 Si1 C8 109.78(7) . . ? C9 Si1 C8 110.58(9) . . ? O2 Si1 C10 108.61(7) . . ? C9 Si1 C10 111.93(8) . . ? C8 Si1 C10 110.03(9) . . ? C7 O1 C1 110.64(12) . . ? C2 O2 Si1 122.35(10) . . ? C7 O3 C3 111.05(12) . . ? C14 O4 C4 115.54(12) . . ? C7 O5 C5 111.11(12) . . ? C31 O6 C6 117.28(12) . . ? O1 C1 C6 107.49(13) . . ? O1 C1 C2 110.37(12) . . ? C6 C1 C2 109.90(13) . . ? O1 C1 H1 109.7 . . ? C6 C1 H1 109.7 . . ? C2 C1 H1 109.7 . . ? O2 C2 C3 110.29(12) . . ? O2 C2 C1 110.28(12) . . ? C3 C2 C1 107.27(13) . . ? O2 C2 H2 109.7 . . ? C3 C2 H2 109.7 . . ? C1 C2 H2 109.7 . . ? O3 C3 C2 110.17(13) . . ? O3 C3 C4 106.10(13) . . ? C2 C3 C4 110.73(12) . . ? O3 C3 H3 109.9 . . ? C2 C3 H3 109.9 . . ? C4 C3 H3 109.9 . . ? O4 C4 C5 110.65(12) . . ? O4 C4 C3 108.65(13) . . ? C5 C4 C3 107.82(13) . . ? O4 C4 H4 109.9 . . ? C5 C4 H4 109.9 . . ? C3 C4 H4 109.9 . . ? O5 C5 C4 106.64(13) . . ? O5 C5 C6 105.79(13) . . ? C4 C5 C6 113.75(13) . . ? O5 C5 H5 110.2 . . ? C4 C5 H5 110.2 . . ? C6 C5 H5 110.2 . . ? O6 C6 C1 105.50(12) . . ? O6 C6 C5 114.51(14) . . ? C1 C6 C5 107.61(13) . . ? O6 C6 H6 109.7 . . ? C1 C6 H6 109.7 . . ? C5 C6 H6 109.7 . . ? O1 C7 O3 110.71(13) . . ? O1 C7 O5 111.40(14) . . ? O3 C7 O5 111.51(14) . . ? O1 C7 H7 107.7 . . ? O3 C7 H7 107.7 . . ? O5 C7 H7 107.7 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C13 C10 C12 108.67(15) . . ? C13 C10 C11 109.19(15) . . ? C12 C10 C11 108.84(15) . . ? C13 C10 Si1 111.62(12) . . ? C12 C10 Si1 109.38(13) . . ? C11 C10 Si1 109.09(12) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O7 C14 O4 120.86(15) . . ? O7 C14 C15 127.53(14) . . ? O4 C14 C15 111.59(13) . . ? C28 C15 C16 120.06(15) . . ? C28 C15 C14 119.18(14) . . ? C16 C15 C14 120.73(14) . . ? C15 C16 C29 118.30(14) . . ? C15 C16 C17 123.62(15) . . ? C29 C16 C17 118.03(14) . . ? C18 C17 C16 121.34(15) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 121.88(14) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C20 C19 C30 118.99(15) . . ? C20 C19 C18 122.40(14) . . ? C30 C19 C18 118.60(14) . . ? C21 C20 C19 121.04(15) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 120.21(16) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 121.10(16) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C30 118.88(15) . . ? C22 C23 C24 122.49(16) . . ? C30 C23 C24 118.63(14) . . ? C25 C24 C23 121.38(16) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 121.43(15) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C27 C26 C29 118.87(15) . . ? C27 C26 C25 122.08(15) . . ? C29 C26 C25 119.05(15) . . ? C28 C27 C26 120.97(15) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C15 121.18(15) . . ? C27 C28 H28 119.4 . . ? C15 C28 H28 119.4 . . ? C16 C29 C26 120.61(14) . . ? C16 C29 C30 120.26(14) . . ? C26 C29 C30 119.13(15) . . ? C19 C30 C23 119.77(14) . . ? C19 C30 C29 119.86(14) . . ? C23 C30 C29 120.37(14) . . ? O8 C31 O6 120.59(16) . . ? O8 C31 C32 127.55(15) . . ? O6 C31 C32 111.86(13) . . ? C45 C32 C33 119.27(16) . . ? C45 C32 C31 118.64(15) . . ? C33 C32 C31 122.09(14) . . ? C32 C33 C46 118.47(14) . . ? C32 C33 C34 123.79(16) . . ? C46 C33 C34 117.73(15) . . ? C35 C34 C33 121.16(16) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 122.47(15) . . ? C34 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C37 C36 C35 122.96(15) . . ? C37 C36 C47 118.98(16) . . ? C35 C36 C47 118.06(15) . . ? C38 C37 C36 121.17(17) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 120.33(18) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C40 120.61(18) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C47 119.79(16) . . ? C39 C40 C41 121.60(17) . . ? C47 C40 C41 118.61(16) . . ? C42 C41 C40 120.80(17) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C43 121.94(16) . . ? C41 C42 H42 119.0 . . ? C43 C42 H42 119.0 . . ? C44 C43 C46 118.59(16) . . ? C44 C43 C42 122.26(15) . . ? C46 C43 C42 119.14(16) . . ? C45 C44 C43 120.85(15) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C32 121.97(16) . . ? C44 C45 H45 119.0 . . ? C32 C45 H45 119.0 . . ? C33 C46 C43 120.84(15) . . ? C33 C46 C47 120.73(14) . . ? C43 C46 C47 118.42(16) . . ? C40 C47 C36 119.10(15) . . ? C40 C47 C46 121.07(15) . . ? C36 C47 C46 119.82(15) . . ? Cl3P C48 Cl1 115.3(4) . . ? Cl3P C48 Cl2 87.2(8) . . ? Cl1 C48 Cl2 112.81(11) . . ? Cl3P C48 Cl2P 111.0(4) . . ? Cl1 C48 Cl2P 99.8(6) . . ? Cl2 C48 Cl2P 23.8(7) . . ? Cl3P C48 Cl3 22.9(8) . . ? Cl1 C48 Cl3 107.81(12) . . ? Cl2 C48 Cl3 109.83(11) . . ? Cl2P C48 Cl3 133.6(7) . . ? Cl3P C48 H48 121.9 . . ? Cl1 C48 H48 108.8 . . ? Cl2 C48 H48 108.8 . . ? Cl2P C48 H48 96.1 . . ? Cl3 C48 H48 108.8 . . ? Cl3P C48 H48P 110.1 . . ? Cl1 C48 H48P 110.1 . . ? Cl2 C48 H48P 119.7 . . ? Cl2P C48 H48P 110.1 . . ? Cl3 C48 H48P 94.6 . . ? H48 C48 H48P 15.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Si1 O2 C2 150.83(12) . . . . ? C8 Si1 O2 C2 31.49(14) . . . . ? C10 Si1 O2 C2 -88.85(12) . . . . ? C7 O1 C1 C6 60.37(16) . . . . ? C7 O1 C1 C2 -59.47(15) . . . . ? Si1 O2 C2 C3 132.94(12) . . . . ? Si1 O2 C2 C1 -108.75(13) . . . . ? O1 C1 C2 O2 -66.07(15) . . . . ? C6 C1 C2 O2 175.56(12) . . . . ? O1 C1 C2 C3 54.07(15) . . . . ? C6 C1 C2 C3 -64.31(16) . . . . ? C7 O3 C3 C2 58.57(15) . . . . ? C7 O3 C3 C4 -61.34(15) . . . . ? O2 C2 C3 O3 66.62(16) . . . . ? C1 C2 C3 O3 -53.51(15) . . . . ? O2 C2 C3 C4 -176.31(13) . . . . ? C1 C2 C3 C4 63.56(17) . . . . ? C14 O4 C4 C5 -81.03(15) . . . . ? C14 O4 C4 C3 160.78(13) . . . . ? O3 C3 C4 O4 -178.90(12) . . . . ? C2 C3 C4 O4 61.56(17) . . . . ? O3 C3 C4 C5 61.14(15) . . . . ? C2 C3 C4 C5 -58.40(17) . . . . ? C7 O5 C5 C4 60.07(16) . . . . ? C7 O5 C5 C6 -61.35(17) . . . . ? O4 C4 C5 O5 -179.32(11) . . . . ? C3 C4 C5 O5 -60.63(15) . . . . ? O4 C4 C5 C6 -63.11(16) . . . . ? C3 C4 C5 C6 55.58(17) . . . . ? C31 O6 C6 C1 -166.82(13) . . . . ? C31 O6 C6 C5 75.04(17) . . . . ? O1 C1 C6 O6 177.19(12) . . . . ? C2 C1 C6 O6 -62.67(15) . . . . ? O1 C1 C6 C5 -60.14(17) . . . . ? C2 C1 C6 C5 60.00(17) . . . . ? O5 C5 C6 O6 176.98(12) . . . . ? C4 C5 C6 O6 60.27(17) . . . . ? O5 C5 C6 C1 60.06(17) . . . . ? C4 C5 C6 C1 -56.65(18) . . . . ? C1 O1 C7 O3 62.88(16) . . . . ? C1 O1 C7 O5 -61.81(18) . . . . ? C3 O3 C7 O1 -62.64(16) . . . . ? C3 O3 C7 O5 61.99(16) . . . . ? C5 O5 C7 O1 63.12(18) . . . . ? C5 O5 C7 O3 -61.12(17) . . . . ? O2 Si1 C10 C13 65.60(14) . . . . ? C9 Si1 C10 C13 -177.96(13) . . . . ? C8 Si1 C10 C13 -54.59(15) . . . . ? O2 Si1 C10 C12 -54.70(13) . . . . ? C9 Si1 C10 C12 61.75(14) . . . . ? C8 Si1 C10 C12 -174.89(12) . . . . ? O2 Si1 C10 C11 -173.65(11) . . . . ? C9 Si1 C10 C11 -57.21(15) . . . . ? C8 Si1 C10 C11 66.16(14) . . . . ? C4 O4 C14 O7 -9.9(2) . . . . ? C4 O4 C14 C15 168.57(13) . . . . ? O7 C14 C15 C28 -156.02(18) . . . . ? O4 C14 C15 C28 25.6(2) . . . . ? O7 C14 C15 C16 25.8(3) . . . . ? O4 C14 C15 C16 -152.51(14) . . . . ? C28 C15 C16 C29 1.1(2) . . . . ? C14 C15 C16 C29 179.21(14) . . . . ? C28 C15 C16 C17 -176.38(15) . . . . ? C14 C15 C16 C17 1.7(2) . . . . ? C15 C16 C17 C18 179.18(15) . . . . ? C29 C16 C17 C18 1.7(2) . . . . ? C16 C17 C18 C19 -0.4(2) . . . . ? C17 C18 C19 C20 -179.45(15) . . . . ? C17 C18 C19 C30 -0.5(2) . . . . ? C30 C19 C20 C21 1.1(2) . . . . ? C18 C19 C20 C21 -179.95(15) . . . . ? C19 C20 C21 C22 -0.7(3) . . . . ? C20 C21 C22 C23 -0.4(3) . . . . ? C21 C22 C23 C30 1.2(2) . . . . ? C21 C22 C23 C24 -178.20(16) . . . . ? C22 C23 C24 C25 179.48(16) . . . . ? C30 C23 C24 C25 0.1(2) . . . . ? C23 C24 C25 C26 0.2(2) . . . . ? C24 C25 C26 C27 -179.80(15) . . . . ? C24 C25 C26 C29 0.1(2) . . . . ? C29 C26 C27 C28 0.0(2) . . . . ? C25 C26 C27 C28 179.94(15) . . . . ? C26 C27 C28 C15 0.9(3) . . . . ? C16 C15 C28 C27 -1.5(2) . . . . ? C14 C15 C28 C27 -179.65(15) . . . . ? C15 C16 C29 C26 -0.2(2) . . . . ? C17 C16 C29 C26 177.44(14) . . . . ? C15 C16 C29 C30 -179.75(13) . . . . ? C17 C16 C29 C30 -2.1(2) . . . . ? C27 C26 C29 C16 -0.4(2) . . . . ? C25 C26 C29 C16 179.69(14) . . . . ? C27 C26 C29 C30 179.21(14) . . . . ? C25 C26 C29 C30 -0.7(2) . . . . ? C20 C19 C30 C23 -0.3(2) . . . . ? C18 C19 C30 C23 -179.28(14) . . . . ? C20 C19 C30 C29 179.01(14) . . . . ? C18 C19 C30 C29 0.0(2) . . . . ? C22 C23 C30 C19 -0.8(2) . . . . ? C24 C23 C30 C19 178.57(14) . . . . ? C22 C23 C30 C29 179.89(14) . . . . ? C24 C23 C30 C29 -0.7(2) . . . . ? C16 C29 C30 C19 1.3(2) . . . . ? C26 C29 C30 C19 -178.25(14) . . . . ? C16 C29 C30 C23 -179.40(14) . . . . ? C26 C29 C30 C23 1.0(2) . . . . ? C6 O6 C31 O8 -2.7(2) . . . . ? C6 O6 C31 C32 176.79(13) . . . . ? O8 C31 C32 C45 167.47(17) . . . . ? O6 C31 C32 C45 -12.0(2) . . . . ? O8 C31 C32 C33 -11.8(3) . . . . ? O6 C31 C32 C33 168.70(13) . . . . ? C45 C32 C33 C46 -0.6(2) . . . . ? C31 C32 C33 C46 178.72(14) . . . . ? C45 C32 C33 C34 178.49(15) . . . . ? C31 C32 C33 C34 -2.2(2) . . . . ? C32 C33 C34 C35 -179.72(15) . . . . ? C46 C33 C34 C35 -0.6(2) . . . . ? C33 C34 C35 C36 -0.6(2) . . . . ? C34 C35 C36 C37 -179.60(16) . . . . ? C34 C35 C36 C47 1.3(2) . . . . ? C35 C36 C37 C38 179.94(16) . . . . ? C47 C36 C37 C38 -1.0(3) . . . . ? C36 C37 C38 C39 1.0(3) . . . . ? C37 C38 C39 C40 0.0(3) . . . . ? C38 C39 C40 C47 -1.1(3) . . . . ? C38 C39 C40 C41 178.50(17) . . . . ? C39 C40 C41 C42 179.55(16) . . . . ? C47 C40 C41 C42 -0.8(2) . . . . ? C40 C41 C42 C43 -0.1(3) . . . . ? C41 C42 C43 C44 -179.34(16) . . . . ? C41 C42 C43 C46 0.5(2) . . . . ? C46 C43 C44 C45 0.3(2) . . . . ? C42 C43 C44 C45 -179.82(15) . . . . ? C43 C44 C45 C32 0.0(3) . . . . ? C33 C32 C45 C44 0.1(2) . . . . ? C31 C32 C45 C44 -179.24(15) . . . . ? C32 C33 C46 C43 1.0(2) . . . . ? C34 C33 C46 C43 -178.16(14) . . . . ? C32 C33 C46 C47 -179.77(13) . . . . ? C34 C33 C46 C47 1.1(2) . . . . ? C44 C43 C46 C33 -0.9(2) . . . . ? C42 C43 C46 C33 179.30(14) . . . . ? C44 C43 C46 C47 179.87(14) . . . . ? C42 C43 C46 C47 0.0(2) . . . . ? C39 C40 C47 C36 1.1(2) . . . . ? C41 C40 C47 C36 -178.51(15) . . . . ? C39 C40 C47 C46 -179.02(15) . . . . ? C41 C40 C47 C46 1.4(2) . . . . ? C37 C36 C47 C40 -0.1(2) . . . . ? C35 C36 C47 C40 179.04(14) . . . . ? C37 C36 C47 C46 -179.95(15) . . . . ? C35 C36 C47 C46 -0.9(2) . . . . ? C33 C46 C47 C40 179.76(14) . . . . ? C43 C46 C47 C40 -1.0(2) . . . . ? C33 C46 C47 C36 -0.3(2) . . . . ? C43 C46 C47 C36 178.92(14) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.380 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.049 # start Validation Reply Form _vrf_PLAT063_ALERT_4_B ; PROBLEM: Crystal Probably too Large for Beam Size Response: A normal-focus tube was used, providing a wide beam. ;