# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof Dietrich Gudat' _publ_contact_author_email GUDAT@IAC.UNI-STUTTGART.DE _publ_section_title ; Pyrido-annellated Diazaphospholenes and Phospholenium Ions ; loop_ _publ_author_name 'Dietrich Gudat' 'Zoltan Benko' 'Sebastian Burck' 'Martin Nieger' L.Nyulaszi 'Nicholas Shore' # Attachment 'dalton_2008_rev2.cif' data_dg017_hy_compound_2a _database_code_depnum_ccdc_archive 'CCDC 680282' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-(2,6-Diisopropylphenyl)-(1,5-a]-pyridine-[1,3,2]- diazaphospholenium-triflate ; _chemical_name_common ;3-(2,6-Diisopropylphenyl)-(1,5-a)-pyridine-(1,3,2)- diazaphospholenium-triflate ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 N2 P, C F3 S O3 ' _chemical_formula_sum 'C19 H22 F3 N2 O3 P S' _chemical_formula_weight 446.42 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R 3 c r' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' 'y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, y+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 16.983(2) _cell_length_b 16.983(2) _cell_length_c 16.983(2) _cell_angle_alpha 57.30(1) _cell_angle_beta 57.30(1) _cell_angle_gamma 57.30(1) _cell_volume 3248.3(7) _cell_formula_units_Z 6 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 392 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.271 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 40 mm, 60 sec./deg., 1 deg., 8 sets, 742 frames scaling using SADABS, T-ratio=0.8060, SADABS is used for scaling, but no spherical absorption correction was applied, as for this weakly absorbing compound the effects of scaling are larger than the effects of absorption ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44464 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3809 _reflns_number_gt 3575 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DIRAX _computing_data_reduction EVALCCD _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The crystal is a racemic twin, x = 0.44(9). ; _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^)+(0.0610P)^2^+2.5197P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.44(9) _refine_ls_number_reflns 3809 _refine_ls_number_parameters 263 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.089 _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 0.47139(6) 0.18216(6) 0.52870(6) 0.02371(18) Uani 1 1 d . . . N2 N 0.58982(18) 0.12963(19) 0.45673(19) 0.0208(6) Uani 1 1 d . . . C3 C 0.6358(2) 0.0273(2) 0.5022(2) 0.0207(6) Uani 1 1 d . . . C4 C 0.5714(2) -0.0080(2) 0.5982(2) 0.0248(6) Uani 1 1 d . . . H4 H 0.5866 -0.0753 0.6427 0.030 Uiso 1 1 calc R . . N5 N 0.48315(18) 0.06815(18) 0.61934(17) 0.0176(5) Uani 1 1 d . . . C6 C 0.6399(2) 0.1819(3) 0.3589(2) 0.0253(7) Uani 1 1 d . . . H6 H 0.6087 0.2513 0.3281 0.030 Uiso 1 1 calc R . . C7 C 0.7339(2) 0.1314(3) 0.3091(2) 0.0295(7) Uani 1 1 d . . . H7 H 0.7684 0.1661 0.2427 0.035 Uiso 1 1 calc R . . C8 C 0.7820(2) 0.0272(3) 0.3547(3) 0.0327(8) Uani 1 1 d . . . H8 H 0.8481 -0.0062 0.3188 0.039 Uiso 1 1 calc R . . C9 C 0.7346(2) -0.0239(3) 0.4478(3) 0.0287(7) Uani 1 1 d . . . H9 H 0.7665 -0.0934 0.4773 0.034 Uiso 1 1 calc R . . C10 C 0.3995(2) 0.0560(2) 0.7147(2) 0.0164(5) Uani 1 1 d . . . C11 C 0.3966(2) 0.0702(2) 0.7897(2) 0.0215(6) Uani 1 1 d . . . C12 C 0.3124(2) 0.0633(2) 0.8786(2) 0.0257(7) Uani 1 1 d . . . H12 H 0.3063 0.0736 0.9316 0.031 Uiso 1 1 calc R . . C13 C 0.2385(2) 0.0416(2) 0.8891(2) 0.0266(7) Uani 1 1 d . . . H13 H 0.1821 0.0376 0.9492 0.032 Uiso 1 1 calc R . . C14 C 0.2459(2) 0.0259(2) 0.8134(2) 0.0236(6) Uani 1 1 d . . . H14 H 0.1950 0.0101 0.8226 0.028 Uiso 1 1 calc R . . C15 C 0.3270(2) 0.0328(2) 0.7232(2) 0.0216(6) Uani 1 1 d . . . C16 C 0.3329(2) 0.0152(3) 0.6406(2) 0.0289(7) Uani 1 1 d . . . H16 H 0.3888 0.0352 0.5792 0.035 Uiso 1 1 calc R . . C17 C 0.2384(3) 0.0776(3) 0.6147(3) 0.0428(9) Uani 1 1 d . . . H17A H 0.2470 0.0637 0.5610 0.064 Uiso 1 1 calc R . . H17B H 0.2257 0.1487 0.5925 0.064 Uiso 1 1 calc R . . H17C H 0.1818 0.0606 0.6738 0.064 Uiso 1 1 calc R . . C18 C 0.3597(3) -0.0971(3) 0.6693(4) 0.0507(11) Uani 1 1 d . . . H18A H 0.4211 -0.1354 0.6851 0.076 Uiso 1 1 calc R . . H18B H 0.3701 -0.1087 0.6133 0.076 Uiso 1 1 calc R . . H18C H 0.3050 -0.1186 0.7279 0.076 Uiso 1 1 calc R . . C19 C 0.4779(2) 0.0939(3) 0.7779(2) 0.0277(7) Uani 1 1 d . . . H19 H 0.5376 0.0774 0.7194 0.033 Uiso 1 1 calc R . . C20 C 0.4440(3) 0.2059(3) 0.7549(3) 0.0436(9) Uani 1 1 d . . . H20A H 0.4972 0.2198 0.7473 0.065 Uiso 1 1 calc R . . H20B H 0.3837 0.2249 0.8099 0.065 Uiso 1 1 calc R . . H20C H 0.4295 0.2446 0.6929 0.065 Uiso 1 1 calc R . . C21 C 0.5097(3) 0.0312(3) 0.8693(3) 0.0406(9) Uani 1 1 d . . . H21A H 0.5622 0.0484 0.8583 0.061 Uiso 1 1 calc R . . H21B H 0.5352 -0.0399 0.8800 0.061 Uiso 1 1 calc R . . H21C H 0.4520 0.0447 0.9283 0.061 Uiso 1 1 calc R . . S1 S 0.44754(3) 0.44754(3) 0.44754(3) 0.0211(3) Uani 1 3 d S . . O1 O 0.53188(19) 0.35975(18) 0.42808(19) 0.0363(6) Uani 1 1 d . . . C1T C 0.49071(12) 0.49071(12) 0.49071(12) 0.0225(11) Uani 1 3 d S . . F1 F 0.42376(14) 0.57670(13) 0.50578(13) 0.0295(4) Uani 1 1 d . . . S2 S 0.34103(3) 0.34103(3) 0.34103(3) 0.0239(3) Uani 1 3 d S . . O2 O 0.44247(18) 0.27191(19) 0.33161(19) 0.0353(6) Uani 1 1 d . . . C2T C 0.29718(15) 0.29718(15) 0.29718(15) 0.0351(14) Uani 1 3 d S . . F2 F 0.2932(2) 0.20652(18) 0.3584(2) 0.0562(7) Uani 1 1 d . . . S3 S 0.19565(4) 0.19565(4) 0.19565(4) 0.0326(3) Uani 1 3 d S . . O3 O 0.2604(2) 0.1043(2) 0.2447(2) 0.0564(8) Uani 1 1 d . . . C3T C 0.1543(3) 0.1543(3) 0.1543(3) 0.079(3) Uani 1 3 d S . . F3 F 0.2293(4) 0.1034(4) 0.0916(3) 0.1106(14) 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 P1 0.0196(4) 0.0227(4) 0.0203(4) -0.0058(3) -0.0041(3) -0.0073(3) N2 0.0189(13) 0.0252(13) 0.0212(13) -0.0081(10) -0.0069(11) -0.0096(10) C3 0.0163(14) 0.0287(16) 0.0257(15) -0.0123(13) -0.0073(12) -0.0102(12) C4 0.0216(15) 0.0357(18) 0.0231(15) -0.0128(14) -0.0070(12) -0.0118(13) N5 0.0169(12) 0.0205(12) 0.0159(12) -0.0059(10) -0.0048(9) -0.0084(10) C6 0.0264(16) 0.0318(17) 0.0200(15) -0.0061(13) -0.0054(13) -0.0170(14) C7 0.0280(17) 0.0433(19) 0.0235(16) -0.0134(14) -0.0012(14) -0.0223(15) C8 0.0180(15) 0.050(2) 0.0372(18) -0.0317(17) 0.0014(14) -0.0105(15) C9 0.0229(16) 0.0326(18) 0.0346(19) -0.0168(15) -0.0097(15) -0.0075(14) C10 0.0149(13) 0.0143(13) 0.0158(13) -0.0030(11) -0.0056(11) -0.0047(11) C11 0.0216(15) 0.0204(15) 0.0184(14) -0.0032(12) -0.0078(12) -0.0078(12) C12 0.0269(16) 0.0295(17) 0.0162(14) -0.0053(13) -0.0065(12) -0.0110(13) C13 0.0196(15) 0.0215(16) 0.0200(15) -0.0011(12) -0.0037(12) -0.0059(12) C14 0.0203(15) 0.0233(15) 0.0223(16) -0.0015(12) -0.0064(12) -0.0122(12) C15 0.0220(15) 0.0198(14) 0.0227(15) -0.0041(12) -0.0102(12) -0.0081(12) C16 0.0307(17) 0.042(2) 0.0275(17) -0.0142(14) -0.0051(14) -0.0233(16) C17 0.049(2) 0.050(2) 0.042(2) -0.0113(18) -0.0252(18) -0.0199(19) C18 0.057(3) 0.043(2) 0.076(3) -0.031(2) -0.036(2) -0.009(2) C19 0.0250(16) 0.0405(19) 0.0261(16) -0.0167(15) -0.0068(13) -0.0134(14) C20 0.058(2) 0.042(2) 0.048(2) -0.0100(18) -0.024(2) -0.0271(19) C21 0.0327(19) 0.054(2) 0.044(2) -0.0179(19) -0.0218(17) -0.0108(17) S1 0.0213(3) 0.0213(3) 0.0213(3) -0.0076(2) -0.0076(2) -0.0076(2) O1 0.0368(14) 0.0269(12) 0.0444(15) -0.0186(11) -0.0103(11) -0.0087(11) C1T 0.0204(14) 0.0204(14) 0.0204(14) -0.0059(9) -0.0059(9) -0.0059(9) F1 0.0294(10) 0.0224(9) 0.0301(10) -0.0137(8) -0.0072(8) -0.0041(8) S2 0.0233(4) 0.0233(4) 0.0233(4) -0.0078(2) -0.0078(2) -0.0078(2) O2 0.0322(13) 0.0360(13) 0.0376(13) -0.0154(11) -0.0158(11) -0.0059(11) C2T 0.0352(18) 0.0352(18) 0.0352(18) -0.0124(11) -0.0124(11) -0.0124(11) F2 0.0797(18) 0.0421(13) 0.0637(16) -0.0092(12) -0.0331(14) -0.0326(13) S3 0.0284(4) 0.0284(4) 0.0284(4) -0.0075(2) -0.0075(2) -0.0075(2) O3 0.0447(17) 0.0527(18) 0.0370(15) -0.0069(13) -0.0163(13) -0.0038(14) C3T 0.053(2) 0.053(2) 0.053(2) -0.0041(19) -0.0041(19) -0.0041(19) F3 0.132(3) 0.128(3) 0.094(3) -0.081(2) -0.040(2) -0.016(3) _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 N5 1.689(2) . ? P1 N2 1.708(3) . ? P1 O1 2.992(3) . ? P1 O2 3.037(3) . ? N2 C3 1.401(4) . ? N2 C6 1.402(4) . ? C3 C4 1.392(4) . ? C3 C9 1.429(4) . ? C4 N5 1.369(4) . ? C4 H4 0.9500 . ? N5 C10 1.467(3) . ? C6 C7 1.358(5) . ? C6 H6 0.9500 . ? C7 C8 1.428(5) . ? C7 H7 0.9500 . ? C8 C9 1.340(5) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.392(4) . ? C10 C15 1.400(4) . ? C11 C12 1.412(4) . ? C11 C19 1.522(4) . ? C12 C13 1.390(5) . ? C12 H12 0.9500 . ? C13 C14 1.379(5) . ? C13 H13 0.9500 . ? C14 C15 1.400(4) . ? C14 H14 0.9500 . ? C15 C16 1.527(4) . ? C16 C17 1.521(5) . ? C16 C18 1.543(5) . ? C16 H16 1.0000 . ? 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 C21 1.529(5) . ? C19 C20 1.537(5) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? S1 O1 1.448(2) 2 ? S1 O1 1.448(2) 3 ? S1 O1 1.448(2) . ? S1 C1T 1.832(5) . ? C1T F1 1.337(3) . ? C1T F1 1.337(3) 3 ? C1T F1 1.337(3) 2 ? S2 O2 1.446(2) 2 ? S2 O2 1.446(2) . ? S2 O2 1.446(2) 3 ? S2 C2T 1.860(6) . ? C2T F2 1.328(3) 3 ? C2T F2 1.328(3) . ? C2T F2 1.328(3) 2 ? S3 O3 1.435(3) 3 ? S3 O3 1.435(3) 2 ? S3 O3 1.435(3) . ? S3 C3T 1.756(13) . ? C3T F3 1.357(6) 2 ? C3T F3 1.357(6) . ? C3T F3 1.357(6) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 P1 N2 87.52(12) . . ? N5 P1 O1 143.24(10) . . ? N2 P1 O1 83.90(10) . . ? N5 P1 O2 133.40(10) . . ? N2 P1 O2 79.67(10) . . ? O1 P1 O2 79.90(7) . . ? C3 N2 C6 120.6(3) . . ? C3 N2 P1 115.0(2) . . ? C6 N2 P1 124.4(2) . . ? C4 C3 N2 110.2(3) . . ? C4 C3 C9 130.5(3) . . ? N2 C3 C9 119.3(3) . . ? N5 C4 C3 110.3(3) . . ? N5 C4 H4 124.9 . . ? C3 C4 H4 124.9 . . ? C4 N5 C10 124.0(2) . . ? C4 N5 P1 117.1(2) . . ? C10 N5 P1 118.95(19) . . ? C7 C6 N2 118.8(3) . . ? C7 C6 H6 120.6 . . ? N2 C6 H6 120.6 . . ? C6 C7 C8 121.2(3) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C3 119.4(3) . . ? C8 C9 H9 120.3 . . ? C3 C9 H9 120.3 . . ? C11 C10 C15 124.5(3) . . ? C11 C10 N5 117.8(2) . . ? C15 C10 N5 117.7(2) . . ? C10 C11 C12 116.3(3) . . ? C10 C11 C19 122.8(3) . . ? C12 C11 C19 120.8(3) . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 121.2(3) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C10 116.4(3) . . ? C14 C15 C16 119.9(3) . . ? C10 C15 C16 123.6(3) . . ? C17 C16 C15 113.2(3) . . ? C17 C16 C18 111.2(3) . . ? C15 C16 C18 109.9(3) . . ? C17 C16 H16 107.4 . . ? C15 C16 H16 107.4 . . ? C18 C16 H16 107.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C11 C19 C21 112.2(3) . . ? C11 C19 C20 110.6(3) . . ? C21 C19 C20 110.7(3) . . ? C11 C19 H19 107.7 . . ? C21 C19 H19 107.7 . . ? C20 C19 H19 107.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 S1 O1 115.14(8) 2 3 ? O1 S1 O1 115.14(8) 2 . ? O1 S1 O1 115.14(8) 3 . ? O1 S1 C1T 102.93(11) 2 . ? O1 S1 C1T 102.93(11) 3 . ? O1 S1 C1T 102.93(11) . . ? S1 O1 P1 111.98(13) . . ? F1 C1T F1 107.7(2) . 3 ? F1 C1T F1 107.7(2) . 2 ? F1 C1T F1 107.7(2) 3 2 ? F1 C1T S1 111.2(2) . . ? F1 C1T S1 111.2(2) 3 . ? F1 C1T S1 111.2(2) 2 . ? O2 S2 O2 115.14(8) 2 . ? O2 S2 O2 115.14(8) 2 3 ? O2 S2 O2 115.14(8) . 3 ? O2 S2 C2T 102.94(11) 2 . ? O2 S2 C2T 102.94(11) . . ? O2 S2 C2T 102.94(11) 3 . ? S2 O2 P1 109.30(13) . . ? F2 C2T F2 108.0(3) 3 . ? F2 C2T F2 108.0(3) 3 2 ? F2 C2T F2 108.0(3) . 2 ? F2 C2T S2 110.9(3) 3 . ? F2 C2T S2 110.9(3) . . ? F2 C2T S2 110.9(3) 2 . ? O3 S3 O3 115.22(11) 3 2 ? O3 S3 O3 115.22(11) 3 . ? O3 S3 O3 115.22(11) 2 . ? O3 S3 C3T 102.82(16) 3 . ? O3 S3 C3T 102.82(16) 2 . ? O3 S3 C3T 102.82(16) . . ? F3 C3T F3 105.0(6) 2 . ? F3 C3T F3 105.0(6) 2 3 ? F3 C3T F3 105.0(6) . 3 ? F3 C3T S3 113.7(5) 2 . ? F3 C3T S3 113.7(5) . . ? F3 C3T S3 113.7(5) 3 . ? 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 N5 P1 N2 C3 0.17(19) . . . . ? O1 P1 N2 C3 144.37(18) . . . . ? O2 P1 N2 C3 -134.82(19) . . . . ? N5 P1 N2 C6 179.7(2) . . . . ? O1 P1 N2 C6 -36.1(2) . . . . ? O2 P1 N2 C6 44.7(2) . . . . ? C6 N2 C3 C4 -179.4(3) . . . . ? P1 N2 C3 C4 0.2(3) . . . . ? C6 N2 C3 C9 -0.2(4) . . . . ? P1 N2 C3 C9 179.4(2) . . . . ? N2 C3 C4 N5 -0.6(3) . . . . ? C9 C3 C4 N5 -179.6(3) . . . . ? C3 C4 N5 C10 -179.7(3) . . . . ? C3 C4 N5 P1 0.7(3) . . . . ? N2 P1 N5 C4 -0.5(2) . . . . ? O1 P1 N5 C4 -76.9(3) . . . . ? O2 P1 N5 C4 72.7(2) . . . . ? N2 P1 N5 C10 179.9(2) . . . . ? O1 P1 N5 C10 103.5(2) . . . . ? O2 P1 N5 C10 -106.9(2) . . . . ? C3 N2 C6 C7 -0.1(4) . . . . ? P1 N2 C6 C7 -179.6(2) . . . . ? N2 C6 C7 C8 -0.3(4) . . . . ? C6 C7 C8 C9 0.9(5) . . . . ? C7 C8 C9 C3 -1.2(5) . . . . ? C4 C3 C9 C8 179.8(3) . . . . ? N2 C3 C9 C8 0.8(4) . . . . ? C4 N5 C10 C11 90.5(3) . . . . ? P1 N5 C10 C11 -89.9(3) . . . . ? C4 N5 C10 C15 -90.7(3) . . . . ? P1 N5 C10 C15 88.9(3) . . . . ? C15 C10 C11 C12 -2.0(4) . . . . ? N5 C10 C11 C12 176.7(3) . . . . ? C15 C10 C11 C19 179.1(3) . . . . ? N5 C10 C11 C19 -2.2(4) . . . . ? C10 C11 C12 C13 1.1(4) . . . . ? C19 C11 C12 C13 -180.0(3) . . . . ? C11 C12 C13 C14 0.4(5) . . . . ? C12 C13 C14 C15 -1.0(5) . . . . ? C13 C14 C15 C10 0.2(5) . . . . ? C13 C14 C15 C16 -179.8(3) . . . . ? C11 C10 C15 C14 1.4(4) . . . . ? N5 C10 C15 C14 -177.3(3) . . . . ? C11 C10 C15 C16 -178.6(3) . . . . ? N5 C10 C15 C16 2.7(4) . . . . ? C14 C15 C16 C17 51.8(4) . . . . ? C10 C15 C16 C17 -128.2(3) . . . . ? C14 C15 C16 C18 -73.3(4) . . . . ? C10 C15 C16 C18 106.7(3) . . . . ? C10 C11 C19 C21 -134.4(3) . . . . ? C12 C11 C19 C21 46.7(4) . . . . ? C10 C11 C19 C20 101.3(3) . . . . ? C12 C11 C19 C20 -77.5(4) . . . . ? O1 S1 O1 P1 -120.05(10) 2 . . . ? O1 S1 O1 P1 17.6(2) 3 . . . ? C1T S1 O1 P1 128.77(9) . . . . ? N5 P1 O1 S1 -113.11(19) . . . . ? N2 P1 O1 S1 169.34(17) . . . . ? O2 P1 O1 S1 88.79(15) . . . . ? O1 S1 C1T F1 55.61(13) 2 . . . ? O1 S1 C1T F1 -64.39(13) 3 . . . ? O1 S1 C1T F1 175.61(13) . . . . ? O1 S1 C1T F1 -64.39(13) 2 . . 3 ? O1 S1 C1T F1 175.61(13) 3 . . 3 ? O1 S1 C1T F1 55.61(13) . . . 3 ? O1 S1 C1T F1 175.61(13) 2 . . 2 ? O1 S1 C1T F1 55.61(13) 3 . . 2 ? O1 S1 C1T F1 -64.39(13) . . . 2 ? O2 S2 O2 P1 121.25(11) 2 . . . ? O2 S2 O2 P1 -16.3(2) 3 . . . ? C2T S2 O2 P1 -127.55(8) . . . . ? N5 P1 O2 S2 107.15(18) . . . . ? N2 P1 O2 S2 -176.33(16) . . . . ? O1 P1 O2 S2 -90.75(14) . . . . ? O2 S2 C2T F2 -54.82(17) 2 . . 3 ? O2 S2 C2T F2 -174.82(17) . . . 3 ? O2 S2 C2T F2 65.18(17) 3 . . 3 ? O2 S2 C2T F2 -174.82(17) 2 . . . ? O2 S2 C2T F2 65.18(17) . . . . ? O2 S2 C2T F2 -54.82(17) 3 . . . ? O2 S2 C2T F2 65.18(17) 2 . . 2 ? O2 S2 C2T F2 -54.82(17) . . . 2 ? O2 S2 C2T F2 -174.82(17) 3 . . 2 ? O3 S3 C3T F3 60.8(3) 3 . . 2 ? O3 S3 C3T F3 -59.2(3) 2 . . 2 ? O3 S3 C3T F3 -179.2(3) . . . 2 ? O3 S3 C3T F3 -179.2(3) 3 . . . ? O3 S3 C3T F3 60.8(3) 2 . . . ? O3 S3 C3T F3 -59.2(3) . . . . ? O3 S3 C3T F3 -59.2(3) 3 . . 3 ? O3 S3 C3T F3 -179.2(3) 2 . . 3 ? O3 S3 C3T F3 60.8(3) . . . 3 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C6 H6 O1 0.95 2.52 3.064(4) 116.2 . C4 H4 O3 0.95 2.30 3.244(5) 170.1 4_545 C9 H9 O3 0.95 2.42 3.289(5) 151.1 5_545 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.848 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.055 #============================================================================== data_dg006_hy_compound_2b_otf _database_code_depnum_ccdc_archive 'CCDC 680283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-Tert.-butyl-[1,5-a]-pyridine-[1,3,2]-diazaphospholenium- triflate ; _chemical_name_common ;3-Tert.-butyl-(1,5-a)-pyridine-(1,3,2)-diazaphospholenium- triflate ; _chemical_melting_point ? _chemical_formula_moiety 'C10 H14 N2 P, C F3 S O3' _chemical_formula_sum 'C11 H14 F3 N2 O3 P S' _chemical_formula_weight 342.27 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.492(2) _cell_length_b 10.685(1) _cell_length_c 15.309(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3024.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 162 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.362 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 40 mm, 60 sec./deg., 1 deg., 5 sets, 838 frames scaling using SADABS, T-ratio=0.8263 SADABS is used for scaling, but no spherical absorption correction was applied, as for this weakly absorbing compound the effects of scaling are larger than the effects of absorption ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53188 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6883 _reflns_number_gt 6107 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DIRAX/Collect _computing_data_reduction EVALCCD _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. One SO3CF3 anion and one cation disordered (0.6 : 0.4). Use of restraints for geometry (SADI, SAME) and restraints (SIMU) and constraints (EADP) for displacement parameters of disordered anion and cation. The 'non-disordered' anion and cation were used as a 'model'. The displacement parameters of the ordered atoms of the disordered cation are significantly higher than the equivalent isotropic displacement parameters of the comparable atomsin the ordered cation (approx. by 50%). The core of the cation is disordered. The higher displacement parameters of the ordered atoms indicates, that also this atoms might be affected by the disorder, which could result in anomalous anisotropic displacement parameters. Therefor also this ordered atoms are refined isotropically. The Flack parameter is x = 0.17(11). One anion and one cation are disordered. So the model used in the refinement has some errors. Also the effects of anomalous scattering are, even if they are significan, small usind Mo-Ka radiation. Both, small effects of anomalous scattering and errors in the refined model are the reason for the large s.u.'s of the Flack parameter. Such large s.u.'s are wellknown. It's not a racemic twin and the value is (using the errors) is close to the expected value of 0 for the correct absolute structure. Using crystalographic experience the determination of the absolut structure is correct. More background information could be also find in following paper and references citated therein: R.W.W. Hooft, L.H. Straver, A.L. Spek J. Appl. Cryst. (2008), 41, 96-103 ; _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^)+(0.0592P)^2^+8.5802P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.17(11) _refine_ls_number_reflns 6883 _refine_ls_number_parameters 310 _refine_ls_number_restraints 303 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1497 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.095 _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 S1 S 0.51024(4) 0.77776(8) 0.10706(6) 0.01720(18) Uani 1 1 d D . . O1 O 0.5173(2) 0.8601(3) 0.1811(2) 0.0374(8) Uani 1 1 d D . . O2 O 0.51924(19) 0.8379(3) 0.02358(18) 0.0315(7) Uani 1 1 d D . . O3 O 0.54625(16) 0.6590(2) 0.1166(2) 0.0322(7) Uani 1 1 d D . . C1 C 0.4149(2) 0.7349(4) 0.1067(3) 0.0400(10) Uani 1 1 d D . . F1 F 0.3967(2) 0.6739(4) 0.1804(3) 0.0717(12) Uani 1 1 d D . . F2 F 0.37308(17) 0.8360(4) 0.0997(4) 0.0770(12) Uani 1 1 d D . . F3 F 0.39886(19) 0.6604(3) 0.0396(3) 0.0636(10) Uani 1 1 d D . . P1 P 0.52941(6) 0.38435(9) 0.05034(7) 0.0218(2) Uani 1 1 d D . . N2 N 0.51934(18) 0.2339(3) 0.0182(2) 0.0177(6) Uani 1 1 d D . . C3 C 0.5224(2) 0.1478(4) 0.0830(3) 0.0214(8) Uani 1 1 d D . . H3 H 0.5192 0.0601 0.0739 0.026 Uiso 1 1 calc R . . C4 C 0.5308(2) 0.2035(3) 0.1643(2) 0.0180(7) Uani 1 1 d D . . N5 N 0.53608(17) 0.3325(3) 0.1557(2) 0.0170(6) Uani 1 1 d D . . C6 C 0.5085(2) 0.1957(4) -0.0765(3) 0.0225(8) Uani 1 1 d . . . C7 C 0.4935(3) 0.3155(4) -0.1298(3) 0.0364(11) Uani 1 1 d . . . H7A H 0.4498 0.3564 -0.1075 0.055 Uiso 1 1 calc R . . H7B H 0.4865 0.2934 -0.1914 0.055 Uiso 1 1 calc R . . H7C H 0.5347 0.3727 -0.1245 0.055 Uiso 1 1 calc R . . C8 C 0.4420(3) 0.1109(4) -0.0814(3) 0.0325(10) Uani 1 1 d . . . H8A H 0.3994 0.1568 -0.0606 0.049 Uiso 1 1 calc R . . H8B H 0.4497 0.0370 -0.0446 0.049 Uiso 1 1 calc R . . H8C H 0.4343 0.0846 -0.1420 0.049 Uiso 1 1 calc R . . C9 C 0.5763(3) 0.1295(5) -0.1068(3) 0.0375(11) Uani 1 1 d . . . H9A H 0.6176 0.1865 -0.1021 0.056 Uiso 1 1 calc R . . H9B H 0.5704 0.1034 -0.1678 0.056 Uiso 1 1 calc R . . H9C H 0.5847 0.0557 -0.0702 0.056 Uiso 1 1 calc R . . C10 C 0.5452(2) 0.4088(4) 0.2292(2) 0.0223(8) Uani 1 1 d . . . H10 H 0.5500 0.4968 0.2230 0.027 Uiso 1 1 calc R . . C11 C 0.5473(2) 0.3549(4) 0.3101(3) 0.0266(9) Uani 1 1 d . . . H11 H 0.5536 0.4059 0.3604 0.032 Uiso 1 1 calc R . . C12 C 0.5402(2) 0.2226(4) 0.3198(3) 0.0261(9) Uani 1 1 d . . . H12 H 0.5406 0.1866 0.3766 0.031 Uiso 1 1 calc R . . C13 C 0.5328(2) 0.1481(4) 0.2489(3) 0.0239(8) Uani 1 1 d . . . H13 H 0.5290 0.0599 0.2554 0.029 Uiso 1 1 calc R . . S1' S 0.22518(11) 0.28543(19) 0.09460(13) 0.0287(3) Uiso 0.60 1 d PD A 1 O1' O 0.1901(4) 0.4042(6) 0.0812(5) 0.0633(18) Uiso 0.60 1 d PDU A 1 O2' O 0.2101(4) 0.2216(6) 0.1775(4) 0.0415(12) Uiso 0.60 1 d PDU A 1 O3' O 0.2233(4) 0.2013(6) 0.0205(4) 0.0491(13) Uiso 0.60 1 d PDU A 1 C1' C 0.3193(3) 0.3343(5) 0.1033(4) 0.0293(11) Uiso 0.60 1 d PD A 1 F1' F 0.3625(3) 0.2375(5) 0.1205(4) 0.0540(13) Uiso 0.60 1 d PDU A 1 F2' F 0.3304(3) 0.4166(5) 0.1670(4) 0.0555(12) Uiso 0.60 1 d PDU A 1 F3' F 0.3404(4) 0.3943(6) 0.0318(4) 0.0542(13) Uiso 0.60 1 d PDU A 1 S1A S 0.22542(18) 0.2939(3) 0.1241(2) 0.0287(3) Uiso 0.40 1 d PD B 2 O1A O 0.2184(7) 0.1938(10) 0.1868(7) 0.0633(18) Uiso 0.40 1 d PDU B 2 O2A O 0.2000(5) 0.2657(8) 0.0361(4) 0.0415(12) Uiso 0.40 1 d PDU B 2 O3A O 0.2065(5) 0.4176(6) 0.1543(6) 0.0491(13) Uiso 0.40 1 d PDU B 2 C1A C 0.3231(3) 0.2990(7) 0.1071(5) 0.0293(11) Uiso 0.40 1 d PD B 2 F1A F 0.3462(5) 0.3583(9) 0.0350(6) 0.0540(13) Uiso 0.40 1 d PDU B 2 F2A F 0.3500(4) 0.1845(7) 0.0928(6) 0.0555(12) Uiso 0.40 1 d PDU B 2 F3A F 0.3551(4) 0.3479(8) 0.1774(5) 0.0542(13) Uiso 0.40 1 d PDU B 2 P1' P 0.20084(12) 0.6651(2) 0.06314(14) 0.0311(4) Uiso 0.60 1 d PDU C 1 N2' N 0.2043(2) 0.8113(3) 0.0221(2) 0.0260(7) Uiso 1 1 d DU . . C3' C 0.2132(5) 0.9007(8) 0.0794(5) 0.0334(15) Uiso 0.60 1 d PDU C 1 H3' H 0.2180 0.9864 0.0638 0.040 Uiso 0.60 1 calc PR C 1 C4' C 0.2151(7) 0.8597(9) 0.1635(6) 0.0258(17) Uiso 0.60 1 d PDU C 1 N5' N 0.2113(7) 0.7288(8) 0.1629(6) 0.0302(17) Uiso 0.60 1 d PDU C 1 C6' C 0.2023(3) 0.8244(5) -0.0772(3) 0.0356(10) Uiso 1 1 d . C . C7' C 0.2778(3) 0.8639(6) -0.1057(4) 0.0531(15) Uiso 1 1 d . . . H7'1 H 0.2906 0.9429 -0.0772 0.080 Uiso 1 1 calc R C . H7'2 H 0.2786 0.8750 -0.1692 0.080 Uiso 1 1 calc R . . H7'3 H 0.3126 0.7991 -0.0890 0.080 Uiso 1 1 calc R . . C8' C 0.1471(3) 0.9248(5) -0.1008(4) 0.0421(12) Uiso 1 1 d . . . H8'1 H 0.0990 0.8984 -0.0812 0.063 Uiso 1 1 calc R C . H8'2 H 0.1467 0.9369 -0.1642 0.063 Uiso 1 1 calc R . . H8'3 H 0.1602 1.0035 -0.0720 0.063 Uiso 1 1 calc R . . C9' C 0.1787(4) 0.7003(7) -0.1167(5) 0.0656(18) Uiso 1 1 d . . . H9'1 H 0.1304 0.6786 -0.0951 0.098 Uiso 1 1 calc R C . H9'2 H 0.2131 0.6348 -0.1000 0.098 Uiso 1 1 calc R . . H9'3 H 0.1774 0.7077 -0.1805 0.098 Uiso 1 1 calc R . . C10' C 0.2160(3) 0.6656(5) 0.2413(4) 0.0414(12) Uiso 1 1 d . . . H10' H 0.2130 0.5769 0.2414 0.050 Uiso 0.60 1 calc PR C 1 H10A H 0.2124 0.5771 0.2371 0.050 Uiso 0.40 1 calc PR C 2 C11' C 0.2249(3) 0.7276(5) 0.3193(4) 0.0452(12) Uiso 1 1 d . C . H11' H 0.2286 0.6808 0.3719 0.054 Uiso 1 1 calc R . . C12' C 0.2288(3) 0.8597(5) 0.3225(4) 0.0427(12) Uiso 1 1 d . . . H12' H 0.2355 0.9008 0.3770 0.051 Uiso 1 1 calc R C . C13' C 0.2229(3) 0.9284(5) 0.2477(3) 0.0388(11) Uiso 1 1 d . C . H13' H 0.2238 1.0173 0.2492 0.047 Uiso 0.60 1 calc PR D 1 H13A H 0.2249 1.0171 0.2510 0.047 Uiso 0.40 1 calc PR D 2 P1A P 0.20825(18) 0.9504(3) 0.0763(2) 0.0311(4) Uiso 0.40 1 d PDU C 2 C3A C 0.2069(7) 0.7016(11) 0.0814(7) 0.0334(15) Uiso 0.40 1 d PDU C 2 H3A H 0.2050 0.6161 0.0645 0.040 Uiso 0.40 1 calc PR C 2 C4A C 0.2126(12) 0.7472(13) 0.1664(9) 0.0258(17) Uiso 0.40 1 d PDU C 2 N5A N 0.2147(10) 0.8755(12) 0.1724(7) 0.0302(17) Uiso 0.40 1 d PDU C 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 S1 0.0181(4) 0.0166(4) 0.0168(4) 0.0024(4) 0.0001(4) -0.0002(3) O1 0.057(2) 0.0275(16) 0.0274(17) -0.0041(14) 0.0018(16) -0.0062(15) O2 0.0406(19) 0.0343(17) 0.0194(15) 0.0097(13) 0.0003(13) -0.0061(14) O3 0.0328(15) 0.0127(13) 0.051(2) 0.0027(14) -0.0027(15) 0.0030(11) C1 0.025(2) 0.047(3) 0.048(3) 0.007(3) 0.000(3) -0.001(2) F1 0.044(2) 0.102(3) 0.069(2) 0.024(2) 0.0169(18) -0.031(2) F2 0.0306(16) 0.077(2) 0.124(4) 0.007(3) 0.001(2) 0.0219(17) F3 0.051(2) 0.068(2) 0.073(2) 0.000(2) -0.0305(19) -0.0227(18) P1 0.0316(5) 0.0153(4) 0.0186(4) 0.0001(4) -0.0009(4) -0.0014(4) N2 0.0212(16) 0.0164(15) 0.0155(14) -0.0044(12) -0.0006(12) 0.0028(12) C3 0.0250(19) 0.0161(18) 0.0230(19) 0.0029(15) -0.0015(14) 0.0014(15) C4 0.0161(17) 0.0186(17) 0.0194(18) 0.0041(15) 0.0034(14) 0.0010(14) N5 0.0184(15) 0.0156(15) 0.0170(16) 0.0015(12) -0.0013(12) 0.0008(12) C6 0.026(2) 0.0225(19) 0.0187(19) -0.0042(16) -0.0043(15) 0.0032(16) C7 0.061(3) 0.027(2) 0.021(2) -0.0001(18) -0.005(2) -0.001(2) C8 0.034(2) 0.032(2) 0.031(2) -0.0009(19) -0.0104(19) -0.0051(19) C9 0.031(2) 0.055(3) 0.026(2) -0.014(2) 0.0010(18) 0.008(2) C10 0.032(2) 0.0179(18) 0.0171(18) -0.0020(15) -0.0020(15) 0.0006(15) C11 0.032(2) 0.029(2) 0.0182(18) -0.0059(16) -0.0006(16) 0.0049(18) C12 0.031(2) 0.030(2) 0.0174(18) 0.0061(16) 0.0001(16) 0.0039(18) C13 0.030(2) 0.0200(19) 0.021(2) 0.0036(15) 0.0016(16) 0.0013(16) _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 S1 O2 1.440(3) . ? S1 O3 1.441(3) . ? S1 O1 1.441(3) . ? S1 C1 1.821(4) . ? C1 F3 1.333(5) . ? C1 F2 1.333(5) . ? C1 F1 1.346(5) . ? P1 N2 1.691(3) . ? P1 N5 1.710(3) . ? N2 C3 1.354(5) . ? N2 C6 1.519(5) . ? C3 C4 1.388(5) . ? C3 H3 0.9500 . ? C4 N5 1.388(5) . ? C4 C13 1.425(5) . ? N5 C10 1.400(5) . ? C6 C9 1.512(6) . ? C6 C8 1.529(6) . ? C6 C7 1.543(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? 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 C11 1.367(6) . ? C10 H10 0.9500 . ? C11 C12 1.427(6) . ? C11 H11 0.9500 . ? C12 C13 1.354(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? S1' O1' 1.440(5) . ? S1' O3' 1.449(5) . ? S1' O2' 1.467(5) . ? S1' C1' 1.821(5) . ? C1' F3' 1.327(6) . ? C1' F2' 1.329(6) . ? C1' F1' 1.333(6) . ? S1A O3A 1.444(6) . ? S1A O1A 1.444(6) . ? S1A O2A 1.459(6) . ? S1A C1A 1.826(6) . ? C1A F3A 1.334(7) . ? C1A F2A 1.339(7) . ? C1A F1A 1.343(7) . ? P1' N5' 1.684(9) . ? P1' N2' 1.686(4) . ? N2' C3' 1.307(9) . ? N2' C3A 1.483(11) . ? N2' C6' 1.526(6) . ? N2' P1A 1.704(5) . ? C3' C4' 1.361(11) . ? C3' H3' 0.9500 . ? C4' N5' 1.400(9) . ? C4' C13' 1.490(10) . ? N5' C10' 1.379(10) . ? C6' C9' 1.521(9) . ? C6' C7' 1.522(8) . ? C6' C8' 1.523(7) . ? C7' H7'1 0.9800 . ? C7' H7'2 0.9800 . ? C7' H7'3 0.9800 . ? C8' H8'1 0.9800 . ? C8' H8'2 0.9800 . ? C8' H8'3 0.9800 . ? C9' H9'1 0.9800 . ? C9' H9'2 0.9800 . ? C9' H9'3 0.9800 . ? C10' C11' 1.375(8) . ? C10' C4A 1.441(15) . ? C10' H10' 0.9500 . ? C10' H10A 0.9500 . ? C11' C12' 1.415(8) . ? C11' H11' 0.9500 . ? C12' C13' 1.365(7) . ? C12' H12' 0.9500 . ? C13' N5A 1.292(12) . ? C13' H13' 0.9500 . ? C13' H13A 0.9500 . ? P1A N5A 1.679(11) . ? C3A C4A 1.394(15) . ? C3A H3A 0.9500 . ? C4A N5A 1.375(13) . ? 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 S1 O3 115.5(2) . . ? O2 S1 O1 114.52(19) . . ? O3 S1 O1 114.6(2) . . ? O2 S1 C1 102.8(2) . . ? O3 S1 C1 103.08(18) . . ? O1 S1 C1 104.1(2) . . ? F3 C1 F2 107.1(4) . . ? F3 C1 F1 107.5(4) . . ? F2 C1 F1 108.4(4) . . ? F3 C1 S1 111.6(3) . . ? F2 C1 S1 111.0(3) . . ? F1 C1 S1 111.2(3) . . ? N2 P1 N5 88.53(15) . . ? C3 N2 C6 121.5(3) . . ? C3 N2 P1 115.3(3) . . ? C6 N2 P1 123.2(3) . . ? N2 C3 C4 111.7(3) . . ? N2 C3 H3 124.1 . . ? C4 C3 H3 124.1 . . ? N5 C4 C3 110.4(3) . . ? N5 C4 C13 119.8(3) . . ? C3 C4 C13 129.8(3) . . ? C4 N5 C10 120.7(3) . . ? C4 N5 P1 113.9(3) . . ? C10 N5 P1 125.3(3) . . ? C9 C6 N2 108.0(3) . . ? C9 C6 C8 112.0(4) . . ? N2 C6 C8 108.2(3) . . ? C9 C6 C7 112.0(4) . . ? N2 C6 C7 107.8(3) . . ? C8 C6 C7 108.7(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N5 119.1(4) . . ? C11 C10 H10 120.4 . . ? N5 C10 H10 120.4 . . ? C10 C11 C12 120.6(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 120.6(4) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C4 119.2(4) . . ? C12 C13 H13 120.4 . . ? C4 C13 H13 120.4 . . ? O1' S1' O3' 115.1(4) . . ? O1' S1' O2' 116.6(4) . . ? O3' S1' O2' 112.6(4) . . ? O1' S1' C1' 100.9(4) . . ? O3' S1' C1' 105.0(3) . . ? O2' S1' C1' 104.6(4) . . ? F3' C1' F2' 103.9(5) . . ? F3' C1' F1' 111.2(5) . . ? F2' C1' F1' 106.0(5) . . ? F3' C1' S1' 111.1(5) . . ? F2' C1' S1' 113.0(4) . . ? F1' C1' S1' 111.4(4) . . ? O3A S1A O1A 116.3(6) . . ? O3A S1A O2A 114.0(5) . . ? O1A S1A O2A 115.7(6) . . ? O3A S1A C1A 105.0(5) . . ? O1A S1A C1A 101.9(6) . . ? O2A S1A C1A 101.2(4) . . ? F3A C1A F2A 108.9(7) . . ? F3A C1A F1A 109.7(7) . . ? F2A C1A F1A 100.3(7) . . ? F3A C1A S1A 109.6(6) . . ? F2A C1A S1A 111.3(5) . . ? F1A C1A S1A 116.5(6) . . ? N5' P1' N2' 87.6(3) . . ? C3' N2' C3A 99.3(7) . . ? C3' N2' C6' 127.2(5) . . ? C3A N2' C6' 133.0(5) . . ? C3' N2' P1' 115.6(5) . . ? C3A N2' P1' 16.4(5) . . ? C6' N2' P1' 117.1(3) . . ? C3' N2' P1A 14.2(4) . . ? C3A N2' P1A 112.9(5) . . ? C6' N2' P1A 114.0(3) . . ? P1' N2' P1A 128.9(3) . . ? N2' C3' C4' 113.8(8) . . ? N2' C3' H3' 123.1 . . ? C4' C3' H3' 123.1 . . ? C3' C4' N5' 108.3(8) . . ? C3' C4' C13' 131.4(8) . . ? N5' C4' C13' 120.2(8) . . ? C10' N5' C4' 118.7(8) . . ? C10' N5' P1' 126.8(6) . . ? C4' N5' P1' 114.6(7) . . ? C9' C6' C7' 113.0(5) . . ? C9' C6' C8' 109.1(5) . . ? C7' C6' C8' 110.6(4) . . ? C9' C6' N2' 108.9(4) . . ? C7' C6' N2' 106.7(4) . . ? C8' C6' N2' 108.5(4) . . ? C6' C7' H7'1 109.5 . . ? C6' C7' H7'2 109.5 . . ? H7'1 C7' H7'2 109.5 . . ? C6' C7' H7'3 109.5 . . ? H7'1 C7' H7'3 109.5 . . ? H7'2 C7' H7'3 109.5 . . ? C6' C8' H8'1 109.5 . . ? C6' C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C6' C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C6' C9' H9'1 109.5 . . ? C6' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C6' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C11' C10' N5' 121.8(6) . . ? C11' C10' C4A 113.9(7) . . ? N5' C10' C4A 7.9(8) . . ? C11' C10' H10' 119.1 . . ? N5' C10' H10' 119.1 . . ? C4A C10' H10' 127.0 . . ? C11' C10' H10A 123.1 . . ? N5' C10' H10A 115.1 . . ? C4A C10' H10A 123.1 . . ? H10' C10' H10A 4.0 . . ? C10' C11' C12' 121.1(6) . . ? C10' C11' H11' 119.4 . . ? C12' C11' H11' 119.4 . . ? C13' C12' C11' 120.2(5) . . ? C13' C12' H12' 119.9 . . ? C11' C12' H12' 119.9 . . ? N5A C13' C12' 121.5(7) . . ? N5A C13' C4' 3.7(9) . . ? C12' C13' C4' 117.9(6) . . ? N5A C13' H13' 117.5 . . ? C12' C13' H13' 121.0 . . ? C4' C13' H13' 121.0 . . ? N5A C13' H13A 119.2 . . ? C12' C13' H13A 119.2 . . ? C4' C13' H13A 122.8 . . ? H13' C13' H13A 2.1 . . ? N5A P1A N2' 90.8(5) . . ? C4A C3A N2' 107.3(9) . . ? C4A C3A H3A 126.3 . . ? N2' C3A H3A 126.3 . . ? N5A C4A C3A 114.4(12) . . ? N5A C4A C10' 123.3(12) . . ? C3A C4A C10' 122.3(11) . . ? C13' N5A C4A 120.0(11) . . ? C13' N5A P1A 125.5(9) . . ? C4A N5A P1A 114.5(10) . . ? 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 O2 S1 C1 F3 58.6(3) . . . . ? O3 S1 C1 F3 -61.7(4) . . . . ? O1 S1 C1 F3 178.3(3) . . . . ? O2 S1 C1 F2 -60.7(4) . . . . ? O3 S1 C1 F2 178.9(4) . . . . ? O1 S1 C1 F2 59.0(4) . . . . ? O2 S1 C1 F1 178.6(3) . . . . ? O3 S1 C1 F1 58.2(4) . . . . ? O1 S1 C1 F1 -61.7(4) . . . . ? N5 P1 N2 C3 -1.3(3) . . . . ? N5 P1 N2 C6 179.4(3) . . . . ? C6 N2 C3 C4 -178.5(3) . . . . ? P1 N2 C3 C4 2.2(4) . . . . ? N2 C3 C4 N5 -2.0(5) . . . . ? N2 C3 C4 C13 176.6(4) . . . . ? C3 C4 N5 C10 -179.7(3) . . . . ? C13 C4 N5 C10 1.6(6) . . . . ? C3 C4 N5 P1 1.0(4) . . . . ? C13 C4 N5 P1 -177.7(3) . . . . ? N2 P1 N5 C4 0.1(3) . . . . ? N2 P1 N5 C10 -179.2(3) . . . . ? C3 N2 C6 C9 -69.2(5) . . . . ? P1 N2 C6 C9 110.1(4) . . . . ? C3 N2 C6 C8 52.2(5) . . . . ? P1 N2 C6 C8 -128.5(3) . . . . ? C3 N2 C6 C7 169.7(4) . . . . ? P1 N2 C6 C7 -11.1(5) . . . . ? C4 N5 C10 C11 -1.4(6) . . . . ? P1 N5 C10 C11 177.8(3) . . . . ? N5 C10 C11 C12 -0.1(6) . . . . ? C10 C11 C12 C13 1.4(7) . . . . ? C11 C12 C13 C4 -1.2(7) . . . . ? N5 C4 C13 C12 -0.2(6) . . . . ? C3 C4 C13 C12 -178.7(4) . . . . ? O1' S1' C1' F3' -58.5(5) . . . . ? O3' S1' C1' F3' 61.4(5) . . . . ? O2' S1' C1' F3' -179.9(5) . . . . ? O1' S1' C1' F2' 57.8(6) . . . . ? O3' S1' C1' F2' 177.7(5) . . . . ? O2' S1' C1' F2' -63.6(6) . . . . ? O1' S1' C1' F1' 176.9(5) . . . . ? O3' S1' C1' F1' -63.2(6) . . . . ? O2' S1' C1' F1' 55.5(6) . . . . ? O3A S1A C1A F3A 49.1(7) . . . . ? O1A S1A C1A F3A -72.6(8) . . . . ? O2A S1A C1A F3A 167.9(7) . . . . ? O3A S1A C1A F2A 169.7(7) . . . . ? O1A S1A C1A F2A 48.0(8) . . . . ? O2A S1A C1A F2A -71.5(7) . . . . ? O3A S1A C1A F1A -76.2(8) . . . . ? O1A S1A C1A F1A 162.2(8) . . . . ? O2A S1A C1A F1A 42.7(8) . . . . ? N5' P1' N2' C3' 0.4(7) . . . . ? N5' P1' N2' C3A 8(2) . . . . ? N5' P1' N2' C6' 176.2(5) . . . . ? N5' P1' N2' P1A -5.2(6) . . . . ? C3A N2' C3' C4' -4.6(11) . . . . ? C6' N2' C3' C4' -177.9(8) . . . . ? P1' N2' C3' C4' -2.6(10) . . . . ? P1A N2' C3' C4' 159(2) . . . . ? N2' C3' C4' N5' 3.7(14) . . . . ? N2' C3' C4' C13' -178.9(10) . . . . ? C3' C4' N5' C10' 176.8(10) . . . . ? C13' C4' N5' C10' -1.0(18) . . . . ? C3' C4' N5' P1' -3.4(15) . . . . ? C13' C4' N5' P1' 178.8(8) . . . . ? N2' P1' N5' C10' -178.5(11) . . . . ? N2' P1' N5' C4' 1.8(10) . . . . ? C3' N2' C6' C9' -170.9(6) . . . . ? C3A N2' C6' C9' 18.3(10) . . . . ? P1' N2' C6' C9' 13.9(6) . . . . ? P1A N2' C6' C9' -164.9(4) . . . . ? C3' N2' C6' C7' 66.9(7) . . . . ? C3A N2' C6' C7' -104.0(9) . . . . ? P1' N2' C6' C7' -108.3(4) . . . . ? P1A N2' C6' C7' 72.9(5) . . . . ? C3' N2' C6' C8' -52.3(7) . . . . ? C3A N2' C6' C8' 136.9(8) . . . . ? P1' N2' C6' C8' 132.5(4) . . . . ? P1A N2' C6' C8' -46.3(5) . . . . ? C4' N5' C10' C11' -0.6(15) . . . . ? P1' N5' C10' C11' 179.7(7) . . . . ? C4' N5' C10' C4A -2(9) . . . . ? P1' N5' C10' C4A 178(11) . . . . ? N5' C10' C11' C12' 0.8(11) . . . . ? C4A C10' C11' C12' 1.1(12) . . . . ? C10' C11' C12' C13' 0.7(9) . . . . ? C11' C12' C13' N5A -0.9(12) . . . . ? C11' C12' C13' C4' -2.2(10) . . . . ? C3' C4' C13' N5A 22(18) . . . . ? N5' C4' C13' N5A -161(20) . . . . ? C3' C4' C13' C12' -174.8(11) . . . . ? N5' C4' C13' C12' 2.4(15) . . . . ? C3' N2' P1A N5A -16.2(19) . . . . ? C3A N2' P1A N5A 1.1(9) . . . . ? C6' N2' P1A N5A -176.4(7) . . . . ? P1' N2' P1A N5A 4.9(7) . . . . ? C3' N2' C3A C4A 3.7(12) . . . . ? C6' N2' C3A C4A 176.3(10) . . . . ? P1' N2' C3A C4A -170(3) . . . . ? P1A N2' C3A C4A -0.6(13) . . . . ? N2' C3A C4A N5A 0(2) . . . . ? N2' C3A C4A C10' 179.7(14) . . . . ? C11' C10' C4A N5A -3(2) . . . . ? N5' C10' C4A N5A 176(12) . . . . ? C11' C10' C4A C3A 177.1(14) . . . . ? N5' C10' C4A C3A -5(8) . . . . ? C12' C13' N5A C4A -1(2) . . . . ? C4' C13' N5A C4A 16(18) . . . . ? C12' C13' N5A P1A -179.0(9) . . . . ? C4' C13' N5A P1A -162(21) . . . . ? C3A C4A N5A C13' -177.2(15) . . . . ? C10' C4A N5A C13' 3(3) . . . . ? C3A C4A N5A P1A 1(2) . . . . ? C10' C4A N5A P1A -178.9(13) . . . . ? N2' P1A N5A C13' 177.0(15) . . . . ? N2' P1A N5A C4A -1.3(16) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.002 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.089 #============================================================================== data_dg022_hy_compound_3a _database_code_depnum_ccdc_archive 'CCDC 680284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-(2,6-Diisopropylphenyl)-[1,5-a]pyridine-2-hexamethyldisilazyl- [1,3,2]-diazaphospholene ; _chemical_name_common ; 3-(2,6-Diisopropylphenyl)-(1,5-a)pyridine-2- hexamethyldisilazyl-(1,3,2)-diazaphospholene ; _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 N3 P Si2' _chemical_formula_sum 'C24 H40 N3 P Si2' _chemical_formula_weight 457.74 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' N N 0.0061 0.0033 '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' _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 10.2893(3) _cell_length_b 10.4169(4) _cell_length_c 13.7477(6) _cell_angle_alpha 72.889(2) _cell_angle_beta 87.454(2) _cell_angle_gamma 71.054(2) _cell_volume 1329.87(9) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4774 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description nlocks _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.209 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 30 mm, 30 sec./deg., 2 deg., 4 sets, 176 frames, mos.= 0.706(2) deg. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 2 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14747 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4681 _reflns_number_gt 3829 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0437P)^2^+0.5602P] 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 4681 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0874 _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 0.09225(4) 0.57652(5) 0.20750(3) 0.01626(13) Uani 1 1 d . . . N2 N 0.11877(14) 0.58961(15) 0.07949(11) 0.0182(3) Uani 1 1 d . . . C3 C 0.11074(17) 0.72799(19) 0.01642(13) 0.0186(4) Uani 1 1 d . . . C4 C 0.08804(17) 0.81906(19) 0.07176(13) 0.0185(4) Uani 1 1 d . . . H4 H 0.0816 0.9161 0.0441 0.022 Uiso 1 1 calc R . . N5 N 0.07484(14) 0.75415(15) 0.17589(11) 0.0165(3) Uani 1 1 d . . . C6 C 0.15012(17) 0.4766(2) 0.03930(15) 0.0228(4) Uani 1 1 d . . . H6 H 0.1552 0.3850 0.0826 0.027 Uiso 1 1 calc R . . C7 C 0.17344(18) 0.4942(2) -0.05987(16) 0.0288(5) Uani 1 1 d . . . H7 H 0.1978 0.4150 -0.0858 0.035 Uiso 1 1 calc R . . C8 C 0.16153(19) 0.6333(2) -0.12675(15) 0.0299(5) Uani 1 1 d . . . H8 H 0.1744 0.6462 -0.1974 0.036 Uiso 1 1 calc R . . C9 C 0.13233(18) 0.7451(2) -0.09007(14) 0.0247(4) Uani 1 1 d . . . H9 H 0.1259 0.8361 -0.1349 0.030 Uiso 1 1 calc R . . C10 C -0.00244(17) 0.83990(18) 0.23757(13) 0.0173(4) Uani 1 1 d . . . C11 C -0.14675(17) 0.87766(18) 0.23499(13) 0.0185(4) Uani 1 1 d . . . C12 C -0.21774(19) 0.96050(19) 0.29606(14) 0.0233(4) Uani 1 1 d . . . H12 H -0.3150 0.9850 0.2969 0.028 Uiso 1 1 calc R . . C13 C -0.1495(2) 1.0077(2) 0.35525(14) 0.0256(4) Uani 1 1 d . . . H13 H -0.2000 1.0650 0.3956 0.031 Uiso 1 1 calc R . . C14 C -0.0080(2) 0.9715(2) 0.35574(15) 0.0254(4) Uani 1 1 d . . . H14 H 0.0379 1.0051 0.3963 0.031 Uiso 1 1 calc R . . C15 C 0.06864(18) 0.88665(19) 0.29801(14) 0.0212(4) Uani 1 1 d . . . C16 C 0.22366(19) 0.8529(2) 0.29579(16) 0.0295(5) Uani 1 1 d . . . H16 H 0.2619 0.7665 0.2723 0.035 Uiso 1 1 calc R . . C17 C 0.2933(2) 0.8206(2) 0.40014(17) 0.0391(5) Uani 1 1 d . . . H17A H 0.3928 0.7991 0.3939 0.059 Uiso 1 1 calc R . . H17B H 0.2749 0.7387 0.4479 0.059 Uiso 1 1 calc R . . H17C H 0.2569 0.9034 0.4255 0.059 Uiso 1 1 calc R . . C18 C 0.2591(2) 0.9748(3) 0.21859(18) 0.0433(6) Uani 1 1 d . . . H18A H 0.3593 0.9516 0.2176 0.065 Uiso 1 1 calc R . . H18B H 0.2192 1.0622 0.2381 0.065 Uiso 1 1 calc R . . H18C H 0.2214 0.9887 0.1506 0.065 Uiso 1 1 calc R . . C19 C -0.22743(17) 0.83556(19) 0.16667(14) 0.0213(4) Uani 1 1 d . . . H19 H -0.1602 0.7824 0.1258 0.026 Uiso 1 1 calc R . . C20 C -0.32893(19) 0.9659(2) 0.09186(16) 0.0309(5) Uani 1 1 d . . . H20A H -0.3788 0.9350 0.0490 0.046 Uiso 1 1 calc R . . H20B H -0.2784 1.0246 0.0488 0.046 Uiso 1 1 calc R . . H20C H -0.3945 1.0217 0.1300 0.046 Uiso 1 1 calc R . . C21 C -0.3022(2) 0.7362(2) 0.22986(16) 0.0298(5) Uani 1 1 d . . . H21A H -0.3530 0.7105 0.1841 0.045 Uiso 1 1 calc R . . H21B H -0.3666 0.7845 0.2726 0.045 Uiso 1 1 calc R . . H21C H -0.2348 0.6501 0.2733 0.045 Uiso 1 1 calc R . . N1 N 0.24817(14) 0.46854(15) 0.26737(11) 0.0179(3) Uani 1 1 d . . . Si1 Si 0.41566(5) 0.45844(5) 0.22465(4) 0.02090(14) Uani 1 1 d . . . C22 C 0.42163(18) 0.6078(2) 0.11258(15) 0.0261(4) Uani 1 1 d . . . H22A H 0.3840 0.6975 0.1294 0.039 Uiso 1 1 calc R . . H22B H 0.3669 0.6105 0.0550 0.039 Uiso 1 1 calc R . . H22C H 0.5172 0.5943 0.0941 0.039 Uiso 1 1 calc R . . C23 C 0.5248(2) 0.4599(2) 0.32956(16) 0.0326(5) Uani 1 1 d . . . H23A H 0.5247 0.3825 0.3908 0.049 Uiso 1 1 calc R . . H23B H 0.4875 0.5510 0.3444 0.049 Uiso 1 1 calc R . . H23C H 0.6192 0.4470 0.3083 0.049 Uiso 1 1 calc R . . C24 C 0.4890(2) 0.2931(2) 0.18615(18) 0.0346(5) Uani 1 1 d . . . H24A H 0.4879 0.2109 0.2433 0.052 Uiso 1 1 calc R . . H24B H 0.5840 0.2826 0.1671 0.052 Uiso 1 1 calc R . . H24C H 0.4338 0.2988 0.1278 0.052 Uiso 1 1 calc R . . Si2 Si 0.22425(5) 0.35654(5) 0.38754(4) 0.02320(14) Uani 1 1 d . . . C25 C 0.0697(2) 0.3016(2) 0.38224(16) 0.0312(5) Uani 1 1 d . . . H25A H 0.0806 0.2504 0.3313 0.047 Uiso 1 1 calc R . . H25B H -0.0126 0.3861 0.3634 0.047 Uiso 1 1 calc R . . H25C H 0.0600 0.2394 0.4492 0.047 Uiso 1 1 calc R . . C26 C 0.3715(2) 0.1865(2) 0.42925(18) 0.0386(5) Uani 1 1 d . . . H26A H 0.3825 0.1359 0.3780 0.058 Uiso 1 1 calc R . . H26B H 0.3531 0.1272 0.4947 0.058 Uiso 1 1 calc R . . H26C H 0.4561 0.2075 0.4369 0.058 Uiso 1 1 calc R . . C27 C 0.2026(2) 0.4526(3) 0.48457(16) 0.0405(5) Uani 1 1 d . . . H27A H 0.2835 0.4815 0.4879 0.061 Uiso 1 1 calc R . . H27B H 0.1927 0.3899 0.5513 0.061 Uiso 1 1 calc R . . H27C H 0.1202 0.5370 0.4658 0.061 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 0.0146(2) 0.0151(2) 0.0187(3) -0.00405(19) 0.00194(17) -0.00528(18) N2 0.0161(7) 0.0196(8) 0.0208(8) -0.0077(7) 0.0019(6) -0.0069(6) C3 0.0142(8) 0.0212(10) 0.0180(10) -0.0022(8) -0.0007(7) -0.0055(7) C4 0.0169(8) 0.0177(9) 0.0177(10) -0.0012(8) 0.0016(7) -0.0051(7) N5 0.0175(7) 0.0152(8) 0.0150(8) -0.0035(6) 0.0015(6) -0.0041(6) C6 0.0150(9) 0.0266(10) 0.0329(11) -0.0166(9) 0.0031(7) -0.0081(8) C7 0.0192(9) 0.0408(13) 0.0365(12) -0.0264(10) 0.0057(8) -0.0101(9) C8 0.0202(10) 0.0518(14) 0.0224(11) -0.0177(10) 0.0036(8) -0.0121(9) C9 0.0207(9) 0.0336(11) 0.0177(10) -0.0054(9) 0.0000(7) -0.0081(8) C10 0.0215(9) 0.0126(9) 0.0160(9) -0.0026(7) 0.0019(7) -0.0049(7) C11 0.0218(9) 0.0137(9) 0.0171(9) -0.0012(7) 0.0021(7) -0.0053(7) C12 0.0225(9) 0.0207(10) 0.0231(10) -0.0048(8) 0.0066(8) -0.0047(8) C13 0.0342(11) 0.0212(10) 0.0211(10) -0.0091(8) 0.0087(8) -0.0070(8) C14 0.0359(11) 0.0235(10) 0.0210(10) -0.0087(8) 0.0015(8) -0.0131(9) C15 0.0265(10) 0.0178(9) 0.0192(10) -0.0048(8) 0.0011(7) -0.0077(8) C16 0.0251(10) 0.0355(12) 0.0349(12) -0.0192(10) -0.0006(8) -0.0110(9) C17 0.0367(12) 0.0424(13) 0.0413(14) -0.0132(11) -0.0108(10) -0.0146(10) C18 0.0350(12) 0.0678(17) 0.0375(14) -0.0176(12) 0.0085(10) -0.0294(12) C19 0.0161(9) 0.0235(10) 0.0247(10) -0.0088(8) 0.0036(7) -0.0059(7) C20 0.0248(10) 0.0334(12) 0.0309(12) -0.0064(10) -0.0031(8) -0.0068(9) C21 0.0287(10) 0.0333(12) 0.0325(12) -0.0112(10) 0.0042(9) -0.0157(9) N1 0.0164(7) 0.0154(8) 0.0191(8) -0.0025(6) 0.0005(6) -0.0039(6) Si1 0.0148(2) 0.0210(3) 0.0241(3) -0.0040(2) 0.00014(19) -0.0044(2) C22 0.0166(9) 0.0320(11) 0.0264(11) -0.0028(9) 0.0014(8) -0.0090(8) C23 0.0252(10) 0.0369(12) 0.0324(12) -0.0015(10) -0.0040(8) -0.0130(9) C24 0.0219(10) 0.0315(12) 0.0477(14) -0.0133(10) 0.0076(9) -0.0044(9) Si2 0.0263(3) 0.0197(3) 0.0206(3) -0.0004(2) 0.0007(2) -0.0084(2) C25 0.0349(11) 0.0269(11) 0.0301(12) -0.0002(9) 0.0049(9) -0.0155(9) C26 0.0359(12) 0.0260(12) 0.0408(14) 0.0086(10) -0.0031(10) -0.0088(9) C27 0.0570(14) 0.0447(14) 0.0239(12) -0.0096(11) 0.0054(10) -0.0229(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 P1 N1 1.7080(14) . ? P1 N5 1.7213(15) . ? P1 N2 1.7408(15) . ? N2 C6 1.384(2) . ? N2 C3 1.425(2) . ? C3 C4 1.341(3) . ? C3 C9 1.438(3) . ? C4 N5 1.413(2) . ? C4 H4 0.9500 . ? N5 C10 1.440(2) . ? C6 C7 1.342(3) . ? C6 H6 0.9500 . ? C7 C8 1.439(3) . ? C7 H7 0.9500 . ? C8 C9 1.344(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.406(2) . ? C10 C15 1.409(2) . ? C11 C12 1.395(3) . ? C11 C19 1.520(2) . ? C12 C13 1.381(3) . ? C12 H12 0.9500 . ? C13 C14 1.380(3) . ? C13 H13 0.9500 . ? C14 C15 1.392(3) . ? C14 H14 0.9500 . ? C15 C16 1.519(3) . ? C16 C17 1.528(3) . ? C16 C18 1.531(3) . ? C16 H16 1.0000 . ? 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 C20 1.532(3) . ? C19 C21 1.532(3) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? N1 Si1 1.7761(14) . ? N1 Si2 1.7796(15) . ? Si1 C22 1.8551(19) . ? Si1 C24 1.864(2) . ? Si1 C23 1.873(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Si2 C27 1.856(2) . ? Si2 C25 1.8673(19) . ? Si2 C26 1.870(2) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 N1 P1 N5 112.87(7) . . ? N1 P1 N2 103.48(7) . . ? N5 P1 N2 86.99(7) . . ? C6 N2 C3 120.70(16) . . ? C6 N2 P1 124.51(13) . . ? C3 N2 P1 114.76(12) . . ? C4 C3 N2 110.82(15) . . ? C4 C3 C9 131.91(17) . . ? N2 C3 C9 117.23(16) . . ? C3 C4 N5 112.25(16) . . ? C3 C4 H4 123.9 . . ? N5 C4 H4 123.9 . . ? C4 N5 C10 119.59(14) . . ? C4 N5 P1 115.15(12) . . ? C10 N5 P1 120.37(11) . . ? C7 C6 N2 121.07(18) . . ? C7 C6 H6 119.5 . . ? N2 C6 H6 119.5 . . ? C6 C7 C8 119.88(18) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.54(18) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C3 120.53(19) . . ? C8 C9 H9 119.7 . . ? C3 C9 H9 119.7 . . ? C11 C10 C15 121.32(16) . . ? C11 C10 N5 119.71(15) . . ? C15 C10 N5 118.96(15) . . ? C12 C11 C10 117.93(16) . . ? C12 C11 C19 119.26(16) . . ? C10 C11 C19 122.79(15) . . ? C13 C12 C11 121.37(17) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 119.98(17) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 121.27(17) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C10 118.12(16) . . ? C14 C15 C16 120.67(16) . . ? C10 C15 C16 121.13(16) . . ? C15 C16 C17 113.27(17) . . ? C15 C16 C18 110.27(17) . . ? C17 C16 C18 110.04(17) . . ? C15 C16 H16 107.7 . . ? C17 C16 H16 107.7 . . ? C18 C16 H16 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C11 C19 C20 111.64(15) . . ? C11 C19 C21 111.11(15) . . ? C20 C19 C21 110.69(15) . . ? C11 C19 H19 107.7 . . ? C20 C19 H19 107.7 . . ? C21 C19 H19 107.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P1 N1 Si1 128.91(9) . . ? P1 N1 Si2 109.98(8) . . ? Si1 N1 Si2 121.10(8) . . ? N1 Si1 C22 114.66(8) . . ? N1 Si1 C24 108.63(8) . . ? C22 Si1 C24 106.56(10) . . ? N1 Si1 C23 109.13(8) . . ? C22 Si1 C23 106.40(9) . . ? C24 Si1 C23 111.47(10) . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 Si2 C27 109.32(9) . . ? N1 Si2 C25 111.50(8) . . ? C27 Si2 C25 109.04(10) . . ? N1 Si2 C26 112.16(9) . . ? C27 Si2 C26 109.62(11) . . ? C25 Si2 C26 105.09(10) . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? 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 N1 P1 N2 C6 63.74(14) . . . . ? N5 P1 N2 C6 176.55(14) . . . . ? N1 P1 N2 C3 -114.11(12) . . . . ? N5 P1 N2 C3 -1.30(11) . . . . ? C6 N2 C3 C4 -176.01(15) . . . . ? P1 N2 C3 C4 1.93(18) . . . . ? C6 N2 C3 C9 1.8(2) . . . . ? P1 N2 C3 C9 179.77(12) . . . . ? N2 C3 C4 N5 -1.56(19) . . . . ? C9 C3 C4 N5 -178.98(16) . . . . ? C3 C4 N5 C10 -154.73(15) . . . . ? C3 C4 N5 P1 0.62(18) . . . . ? N1 P1 N5 C4 103.76(12) . . . . ? N2 P1 N5 C4 0.40(11) . . . . ? N1 P1 N5 C10 -101.10(13) . . . . ? N2 P1 N5 C10 155.54(13) . . . . ? C3 N2 C6 C7 -0.1(2) . . . . ? P1 N2 C6 C7 -177.87(13) . . . . ? N2 C6 C7 C8 -2.0(3) . . . . ? C6 C7 C8 C9 2.5(3) . . . . ? C7 C8 C9 C3 -0.8(3) . . . . ? C4 C3 C9 C8 175.97(18) . . . . ? N2 C3 C9 C8 -1.3(2) . . . . ? C4 N5 C10 C11 81.8(2) . . . . ? P1 N5 C10 C11 -72.25(19) . . . . ? C4 N5 C10 C15 -96.97(19) . . . . ? P1 N5 C10 C15 108.98(16) . . . . ? C15 C10 C11 C12 -1.4(3) . . . . ? N5 C10 C11 C12 179.84(15) . . . . ? C15 C10 C11 C19 176.79(17) . . . . ? N5 C10 C11 C19 -1.9(3) . . . . ? C10 C11 C12 C13 1.8(3) . . . . ? C19 C11 C12 C13 -176.52(17) . . . . ? C11 C12 C13 C14 -0.8(3) . . . . ? C12 C13 C14 C15 -0.5(3) . . . . ? C13 C14 C15 C10 0.8(3) . . . . ? C13 C14 C15 C16 177.38(18) . . . . ? C11 C10 C15 C14 0.2(3) . . . . ? N5 C10 C15 C14 178.90(16) . . . . ? C11 C10 C15 C16 -176.35(17) . . . . ? N5 C10 C15 C16 2.4(3) . . . . ? C14 C15 C16 C17 41.1(3) . . . . ? C10 C15 C16 C17 -142.43(18) . . . . ? C14 C15 C16 C18 -82.7(2) . . . . ? C10 C15 C16 C18 93.8(2) . . . . ? C12 C11 C19 C20 58.3(2) . . . . ? C10 C11 C19 C20 -119.91(18) . . . . ? C12 C11 C19 C21 -65.8(2) . . . . ? C10 C11 C19 C21 115.98(19) . . . . ? N5 P1 N1 Si1 -56.66(13) . . . . ? N2 P1 N1 Si1 35.77(12) . . . . ? N5 P1 N1 Si2 123.54(8) . . . . ? N2 P1 N1 Si2 -144.03(8) . . . . ? P1 N1 Si1 C22 13.01(14) . . . . ? Si2 N1 Si1 C22 -167.21(10) . . . . ? P1 N1 Si1 C24 -106.06(13) . . . . ? Si2 N1 Si1 C24 73.72(12) . . . . ? P1 N1 Si1 C23 132.23(12) . . . . ? Si2 N1 Si1 C23 -47.99(12) . . . . ? P1 N1 Si2 C27 -84.85(11) . . . . ? Si1 N1 Si2 C27 95.33(12) . . . . ? P1 N1 Si2 C25 35.79(11) . . . . ? Si1 N1 Si2 C25 -144.02(10) . . . . ? P1 N1 Si2 C26 153.35(10) . . . . ? Si1 N1 Si2 C26 -26.47(13) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.303 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.048 #============================================================================== #_eof # End of Crystallographic Information File