# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2002 data_global #============================================================================== _audit_creation_date '2000-11-27' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== _journal_coden_Cambridge 207 loop_ _publ_author_name 'Thiemann, Thies' 'Arima, Kazuya' 'Gorohmaru, Hideki' 'Mataka, Shuntaro' 'Tabuchi, Yumiko' 'Tanaka, Yasuko' 'Umeno, Kuniharu' 'Wang, Jian' 'Watanabe, Masataka' _publ_contact_author_name 'Prof Thies Thiemann' _publ_contact_author_address ; Institute of Advanced Material Study Kyushu University 6-1 Kasuga-koh-en Kasuga-shi Fukuoka 816-8580 JAPAN ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+81-92-583-7812' _publ_contact_author_fax '+81-92-583-7811' _publ_contact_author_email thies@cm.kyushu-u.ac.jp _publ_requested_journal 'Perkin Transactions 1' _publ_section_title ; Elongated Phosphoranes by C-C coupling of Haloaroylmethylidenetriphenylphosphoranes synthesis and applications ; _publ_section_references ; Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Sheldrick, G.M. (1997). SHELXL-97 Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1994). J. Appl. Cryst., 26, 343. ; data__4l _database_code_CSD 182734 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version1.06(MSC,1997-1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'teXsan for Windows version1.06(MSC,1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 21.492(1) _cell_length_b 8.0545(4) _cell_length_c 15.4024(9) _cell_angle_alpha 90.0(5) _cell_angle_beta 96.1(8) _cell_angle_gamma 90.0(6) _cell_volume 2651(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183.2 _cell_measurement_reflns_used 12140 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 506.58 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H27 O P ' _chemical_formula_moiety 'C36 H27 O P ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1064.00 _exptl_absorpt_coefficient_mu 0.132 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9492 _exptl_absorpt_correction_T_max 0.9934 _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 183.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXIS-RAPID' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w/2\q _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 6425 _reflns_number_total 6007 _reflns_number_gt 3186 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01250 _diffrn_orient_matrix_UB_12 -0.03798 _diffrn_orient_matrix_UB_13 0.06118 _diffrn_orient_matrix_UB_21 0.04139 _diffrn_orient_matrix_UB_22 -0.03706 _diffrn_orient_matrix_UB_23 -0.01715 _diffrn_orient_matrix_UB_31 0.01790 _diffrn_orient_matrix_UB_32 0.11224 _diffrn_orient_matrix_UB_33 0.01504 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 144 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 108 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 4 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.31747(4) -0.06414(11) 0.63053(6) 0.0250(2) Uani 1 1 d . . . O1 O 0.32403(11) 0.2274(3) 0.51988(19) 0.0414(7) Uani 1 1 d . . . C1 C 0.02235(17) 0.6296(5) 0.3653(3) 0.0362(9) Uani 1 1 d . . . C2 C 0.07733(18) 0.6695(5) 0.4133(3) 0.0368(9) Uani 1 1 d . . . C3 C 0.0900(2) 0.8377(5) 0.4359(3) 0.0481(11) Uani 1 1 d . . . C4 C 0.0458(2) 0.9594(5) 0.4136(3) 0.0523(11) Uani 1 1 d . . . C5 C -0.01036(17) 0.9190(5) 0.3655(2) 0.0384(9) Uani 1 1 d . . . C6 C -0.0576(2) 1.0432(5) 0.3413(3) 0.0482(11) Uani 1 1 d . . . C7 C -0.11071(18) 1.0035(6) 0.2918(3) 0.0444(10) Uani 1 1 d . . . C8 C -0.12095(18) 0.8395(6) 0.2608(3) 0.0475(11) Uani 1 1 d . . . C9 C -0.07726(18) 0.7173(5) 0.2839(3) 0.0456(10) Uani 1 1 d . . . C10 C -0.02293(17) 0.7556(5) 0.3377(2) 0.0348(8) Uani 1 1 d . . . C11 C 0.12460(16) 0.5401(4) 0.4406(2) 0.0316(8) Uani 1 1 d . . . C12 C 0.10858(16) 0.3947(4) 0.4832(2) 0.0331(8) Uani 1 1 d . . . C13 C 0.15402(16) 0.2784(4) 0.5118(2) 0.0322(8) Uani 1 1 d . . . C14 C 0.21659(15) 0.3025(4) 0.4978(2) 0.0263(7) Uani 1 1 d . . . C15 C 0.23185(16) 0.4456(4) 0.4528(2) 0.0318(8) Uani 1 1 d . . . C16 C 0.18697(17) 0.5625(4) 0.4259(2) 0.0346(8) Uani 1 1 d . . . C17 C 0.26876(16) 0.1870(4) 0.5326(2) 0.0289(8) Uani 1 1 d . . . C18 C 0.25535(14) 0.0455(4) 0.5783(2) 0.0292(8) Uani 1 1 d . . . C19 C 0.36873(14) 0.0602(4) 0.7050(2) 0.0266(7) Uani 1 1 d . . . C20 C 0.43281(16) 0.0292(4) 0.7191(2) 0.0325(8) Uani 1 1 d . . . C21 C 0.46946(17) 0.1183(5) 0.7825(3) 0.0403(9) Uani 1 1 d . . . C22 C 0.44277(19) 0.2356(5) 0.8324(3) 0.0412(9) Uani 1 1 d . . . C23 C 0.3793(2) 0.2675(5) 0.8178(3) 0.0491(11) Uani 1 1 d . . . C24 C 0.34310(18) 0.1803(5) 0.7545(3) 0.0431(10) Uani 1 1 d . . . C25 C 0.36823(15) -0.1721(4) 0.5620(2) 0.0268(7) Uani 1 1 d . . . C26 C 0.36943(16) -0.3448(4) 0.5580(3) 0.0317(8) Uani 1 1 d . . . C27 C 0.40763(17) -0.4249(5) 0.5036(3) 0.0374(9) Uani 1 1 d . . . C28 C 0.44507(17) -0.3342(5) 0.4538(3) 0.0390(9) Uani 1 1 d . . . C29 C 0.44388(16) -0.1613(5) 0.4562(2) 0.0351(9) Uani 1 1 d . . . C30 C 0.40615(16) -0.0804(4) 0.5108(2) 0.0307(8) Uani 1 1 d . . . C31 C 0.28426(14) -0.2212(4) 0.6950(2) 0.0256(7) Uani 1 1 d . . . C32 C 0.30645(16) -0.2488(5) 0.7828(2) 0.0330(8) Uani 1 1 d . . . C33 C 0.27920(18) -0.3715(5) 0.8308(3) 0.0402(9) Uani 1 1 d . . . C34 C 0.23109(18) -0.4665(5) 0.7916(3) 0.0424(10) Uani 1 1 d . . . C35 C 0.20912(17) -0.4421(5) 0.7045(3) 0.0403(9) Uani 1 1 d . . . C36 C 0.23565(16) -0.3188(5) 0.6562(3) 0.0349(8) Uani 1 1 d . . . H1 H 0.0117 0.5132 0.3455 0.026 Uiso 1 1 d . . . H2 H -0.0507 1.1524 0.3644 0.026 Uiso 1 1 d . . . H3 H -0.1435 1.0823 0.2647 0.026 Uiso 1 1 d . . . H4 H -0.0889 0.5908 0.2663 0.026 Uiso 1 1 d . . . H5 H 0.0625 0.3880 0.4957 0.026 Uiso 1 1 d . . . H6 H 0.1412 0.1748 0.5402 0.026 Uiso 1 1 d . . . H7 H 0.2771 0.4575 0.4412 0.026 Uiso 1 1 d . . . H8 H 0.1997 0.6688 0.3955 0.026 Uiso 1 1 d . . . H9 H 0.2138 0.0138 0.5838 0.026 Uiso 1 1 d . . . H10 H 0.4528 -0.0664 0.6877 0.026 Uiso 1 1 d . . . H11 H 0.5129 0.0840 0.7923 0.026 Uiso 1 1 d . . . H12 H 0.4723 0.2858 0.8830 0.026 Uiso 1 1 d . . . H13 H 0.2998 0.2115 0.7408 0.026 Uiso 1 1 d . . . H14 H 0.3466 -0.4222 0.5999 0.026 Uiso 1 1 d . . . H15 H 0.4027 -0.5622 0.5053 0.026 Uiso 1 1 d . . . H16 H 0.4701 -0.3792 0.4093 0.026 Uiso 1 1 d . . . H17 H 0.4721 -0.1058 0.4209 0.026 Uiso 1 1 d . . . H18 H 0.4026 0.0288 0.5055 0.026 Uiso 1 1 d . . . H19 H 0.3408 -0.1771 0.8165 0.026 Uiso 1 1 d . . . H20 H 0.2086 -0.5530 0.8240 0.026 Uiso 1 1 d . . . H21 H 0.1417 0.8741 0.4740 0.026 Uiso 1 1 d . . . H22 H -0.1679 0.8078 0.2265 0.026 Uiso 1 1 d . . . H23 H 0.3546 0.3605 0.8628 0.026 Uiso 1 1 d . . . H24 H 0.2944 -0.3806 0.9036 0.026 Uiso 1 1 d . . . H25 H 0.1681 -0.5275 0.6711 0.026 Uiso 1 1 d . . . H26 H 0.2099 -0.2681 0.5887 0.026 Uiso 1 1 d . . . H27 H 0.0557 1.1157 0.4174 0.026 Uiso 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 0.0231(4) 0.0269(4) 0.0246(5) -0.0020(4) 0.0005(3) 0.0003(4) O1 0.0274(13) 0.0415(15) 0.0564(19) 0.0134(14) 0.0097(12) 0.0028(11) C1 0.037(2) 0.041(2) 0.032(2) 0.0019(17) 0.0070(17) 0.0042(16) C2 0.043(2) 0.040(2) 0.028(2) 0.0032(17) 0.0023(17) 0.0052(17) C3 0.052(3) 0.037(2) 0.051(3) -0.001(2) -0.012(2) 0.0087(19) C4 0.060(3) 0.044(2) 0.049(3) -0.005(2) -0.013(2) 0.007(2) C5 0.040(2) 0.045(2) 0.029(2) -0.0003(18) 0.0035(16) 0.0024(18) C6 0.056(3) 0.048(3) 0.042(2) 0.004(2) 0.007(2) 0.015(2) C7 0.033(2) 0.062(3) 0.039(2) 0.016(2) 0.0061(19) 0.0103(19) C8 0.034(2) 0.056(3) 0.054(3) 0.018(2) 0.010(2) 0.006(2) C9 0.035(2) 0.057(3) 0.044(3) 0.005(2) 0.0023(19) -0.0036(19) C10 0.036(2) 0.040(2) 0.030(2) 0.0042(17) 0.0114(16) 0.0003(17) C11 0.0336(18) 0.0344(19) 0.0256(19) 0.0017(15) -0.0016(15) 0.0075(15) C12 0.0274(18) 0.041(2) 0.031(2) 0.0034(16) 0.0018(15) 0.0041(15) C13 0.0329(18) 0.0293(18) 0.034(2) 0.0056(16) 0.0031(16) 0.0023(15) C14 0.0292(17) 0.0274(16) 0.0218(18) -0.0003(14) -0.0002(14) 0.0039(14) C15 0.0311(18) 0.0324(18) 0.031(2) 0.0039(16) -0.0008(15) -0.0012(16) C16 0.0387(19) 0.0316(18) 0.032(2) 0.0078(17) -0.0010(16) -0.0016(17) C17 0.0300(18) 0.0308(18) 0.0256(19) -0.0018(15) 0.0006(15) 0.0021(14) C18 0.0220(16) 0.0316(18) 0.032(2) 0.0021(15) -0.0049(14) 0.0005(14) C19 0.0278(16) 0.0246(16) 0.0265(18) -0.0013(15) -0.0006(14) -0.0053(14) C20 0.0306(18) 0.0363(19) 0.030(2) -0.0023(16) 0.0012(15) -0.0019(15) C21 0.032(2) 0.049(2) 0.038(2) 0.0022(19) -0.0049(17) -0.0119(17) C22 0.053(2) 0.038(2) 0.031(2) -0.0060(18) -0.0016(18) -0.0160(19) C23 0.056(3) 0.044(2) 0.045(3) -0.018(2) -0.002(2) -0.001(2) C24 0.037(2) 0.042(2) 0.049(3) -0.017(2) -0.0018(19) 0.0055(18) C25 0.0221(16) 0.0322(18) 0.0251(18) -0.0041(15) -0.0024(14) 0.0015(14) C26 0.0295(18) 0.0299(18) 0.035(2) -0.0017(16) -0.0004(15) 0.0011(15) C27 0.0345(19) 0.0353(19) 0.042(2) -0.0105(18) 0.0013(17) 0.0029(17) C28 0.032(2) 0.050(2) 0.035(2) -0.0105(19) 0.0038(17) 0.0053(18) C29 0.0260(18) 0.048(2) 0.032(2) -0.0006(18) 0.0043(15) 0.0038(17) C30 0.0330(18) 0.0308(18) 0.0276(19) 0.0004(16) 0.0002(15) 0.0048(15) C31 0.0243(16) 0.0267(17) 0.0260(18) -0.0004(14) 0.0031(14) 0.0029(13) C32 0.0329(19) 0.0372(19) 0.027(2) -0.0006(17) -0.0033(15) 0.0039(16) C33 0.047(2) 0.045(2) 0.029(2) 0.0056(17) 0.0039(18) 0.0062(18) C34 0.050(2) 0.035(2) 0.045(3) 0.0082(18) 0.017(2) -0.0046(18) C35 0.043(2) 0.039(2) 0.040(2) -0.0022(19) 0.0080(18) -0.0093(18) C36 0.0309(18) 0.042(2) 0.032(2) -0.0007(17) 0.0041(16) -0.0062(16) #============================================================================== # REFINEMENT DATA _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^)+(0.0976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0033(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6007 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.2004 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_min -0.36 _refine_diff_density_max 0.50 #============================================================================== # MOLECULAR GEOMETRY _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 C18 1.727(12) . ? P1 C31 1.802(10) . ? P1 C19 1.806(13) . ? P1 C25 1.818(11) . ? O1 C17 1.267(6) . ? C1 C2 1.364(10) . ? C1 C10 1.439(10) . ? C1 H1 1.005(5) . ? C2 C3 1.418(7) . ? C2 C11 1.485(10) . ? C3 C4 1.382(10) . ? C3 H21 1.235(9) . ? C4 C5 1.387(11) . ? C4 H27 1.277(5) . ? C5 C10 1.401(7) . ? C5 C6 1.445(10) . ? C6 C7 1.343(11) . ? C6 H2 0.954(6) . ? C7 C8 1.414(8) . ? C7 H3 1.006(8) . ? C8 C9 1.381(10) . ? C8 H22 1.117(8) . ? C9 C10 1.393(11) . ? C9 H4 1.077(6) . ? C11 C16 1.395(6) . ? C11 C12 1.403(8) . ? C12 C13 1.390(10) . ? C12 H5 1.030(4) . ? C13 C14 1.398(6) . ? C13 H6 0.995(6) . ? C14 C15 1.402(8) . ? C14 C17 1.511(11) . ? C15 C16 1.380(10) . ? C15 H7 1.012(4) . ? C16 H8 1.026(6) . ? C17 C18 1.386(8) . ? C18 H9 0.941(4) . ? C19 C24 1.382(9) . ? C19 C20 1.394(6) . ? C20 C21 1.388(11) . ? C20 H10 1.027(6) . ? C21 C22 1.381(9) . ? C21 H11 0.970(5) . ? C22 C23 1.382(7) . ? C22 H12 1.033(8) . ? C23 C24 1.374(11) . ? C23 H23 1.185(8) . ? C24 H13 0.965(5) . ? C25 C26 1.393(5) . ? C25 C30 1.402(10) . ? C26 C27 1.392(10) . ? C26 H14 1.055(7) . ? C27 C28 1.378(10) . ? C27 H15 1.112(4) . ? C28 C29 1.393(5) . ? C28 H16 0.984(7) . ? C29 C30 1.391(10) . ? C29 H17 0.966(7) . ? C30 H18 0.886(4) . ? C31 C36 1.391(10) . ? C31 C32 1.403(8) . ? C32 C33 1.399(9) . ? C32 H19 1.033(8) . ? C33 C34 1.374(11) . ? C33 H24 1.137(6) . ? C34 C35 1.389(9) . ? C34 H20 1.009(7) . ? C35 C36 1.398(9) . ? C35 H25 1.191(9) . ? C36 H26 1.196(8) . ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 P1 C31 106.5(4) . . ? C18 P1 C19 113.7(4) . . ? C31 P1 C19 106.9(4) . . ? C18 P1 C25 117.1(3) . . ? C31 P1 C25 106.4(4) . . ? C19 P1 C25 105.7(3) . . ? C2 C1 C10 120.9(5) . . ? C2 C1 H1 122.7(6) . . ? C10 C1 H1 116.3(5) . . ? C1 C2 C3 119.4(6) . . ? C1 C2 C11 121.0(5) . . ? C3 C2 C11 119.6(5) . . ? C4 C3 C2 120.6(6) . . ? C4 C3 H21 120.6(5) . . ? C2 C3 H21 118.9(6) . . ? C3 C4 C5 120.1(5) . . ? C3 C4 H27 125.6(5) . . ? C5 C4 H27 112.8(7) . . ? C4 C5 C10 120.8(6) . . ? C4 C5 C6 121.5(5) . . ? C10 C5 C6 117.7(6) . . ? C7 C6 C5 120.8(5) . . ? C7 C6 H2 121.3(7) . . ? C5 C6 H2 117.7(6) . . ? C6 C7 C8 120.5(6) . . ? C6 C7 H3 127.0(6) . . ? C8 C7 H3 111.8(6) . . ? C9 C8 C7 120.1(6) . . ? C9 C8 H22 120.9(5) . . ? C7 C8 H22 118.3(7) . . ? C8 C9 C10 120.0(6) . . ? C8 C9 H4 118.4(5) . . ? C10 C9 H4 121.1(6) . . ? C9 C10 C5 120.8(6) . . ? C9 C10 C1 121.2(5) . . ? C5 C10 C1 118.0(5) . . ? C16 C11 C12 118.2(6) . . ? C16 C11 C2 120.2(5) . . ? C12 C11 C2 121.6(4) . . ? C13 C12 C11 120.8(4) . . ? C13 C12 H5 124.2(5) . . ? C11 C12 H5 114.8(7) . . ? C12 C13 C14 120.8(5) . . ? C12 C13 H6 119.1(4) . . ? C14 C13 H6 120.0(6) . . ? C13 C14 C15 118.0(6) . . ? C13 C14 C17 123.3(4) . . ? C15 C14 C17 118.6(4) . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H7 122.4(5) . . ? C14 C15 H7 116.4(7) . . ? C15 C16 C11 121.0(5) . . ? C15 C16 H8 119.6(4) . . ? C11 C16 H8 119.3(6) . . ? O1 C17 C18 122.6(6) . . ? O1 C17 C14 117.3(4) . . ? C18 C17 C14 120.0(5) . . ? C17 C18 P1 117.7(5) . . ? C17 C18 H9 121.3(7) . . ? P1 C18 H9 120.9(4) . . ? C24 C19 C20 118.9(6) . . ? C24 C19 P1 119.1(4) . . ? C20 C19 P1 121.7(5) . . ? C21 C20 C19 119.7(6) . . ? C21 C20 H10 119.0(5) . . ? C19 C20 H10 121.1(6) . . ? C22 C21 C20 120.5(4) . . ? C22 C21 H11 123.9(7) . . ? C20 C21 H11 115.3(6) . . ? C21 C22 C23 119.8(6) . . ? C21 C22 H12 115.4(5) . . ? C23 C22 H12 124.5(6) . . ? C24 C23 C22 119.7(6) . . ? C24 C23 H23 118.9(5) . . ? C22 C23 H23 121.2(6) . . ? C23 C24 C19 121.4(5) . . ? C23 C24 H13 118.8(6) . . ? C19 C24 H13 119.5(7) . . ? C26 C25 C30 119.1(5) . . ? C26 C25 P1 121.2(5) . . ? C30 C25 P1 119.7(4) . . ? C27 C26 C25 120.3(6) . . ? C27 C26 H14 115.9(5) . . ? C25 C26 H14 123.5(5) . . ? C28 C27 C26 120.4(5) . . ? C28 C27 H15 127.1(5) . . ? C26 C27 H15 112.5(6) . . ? C27 C28 C29 120.1(5) . . ? C27 C28 H16 125.9(5) . . ? C29 C28 H16 113.5(6) . . ? C30 C29 C28 119.9(6) . . ? C30 C29 H17 124.4(5) . . ? C28 C29 H17 115.7(6) . . ? C29 C30 C25 120.2(4) . . ? C29 C30 H18 117.4(6) . . ? C25 C30 H18 121.7(5) . . ? C36 C31 C32 119.2(6) . . ? C36 C31 P1 118.9(5) . . ? C32 C31 P1 121.9(5) . . ? C33 C32 C31 120.2(6) . . ? C33 C32 H19 116.5(5) . . ? C31 C32 H19 123.2(6) . . ? C34 C33 C32 119.9(5) . . ? C34 C33 H24 121.5(7) . . ? C32 C33 H24 118.3(6) . . ? C33 C34 C35 120.6(6) . . ? C33 C34 H20 123.0(5) . . ? C35 C34 H20 116.3(6) . . ? C34 C35 C36 119.9(6) . . ? C34 C35 H25 119.7(6) . . ? C36 C35 H25 120.3(5) . . ? C31 C36 C35 120.2(5) . . ? C31 C36 H26 116.0(6) . . ? C35 C36 H26 121.9(5) . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? # -- ENTER NON-BONDED CONTACTS HERE, ONE PER LINE -- # e.g. O1 N1 2.841(1) . . yes #------------------------------------------------------------------------------ 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 C10 C1 C2 C3 -0.2(6) . . . . ? C10 C1 C2 C11 -179.0(3) . . . . ? C1 C2 C3 C4 3.3(7) . . . . ? C11 C2 C3 C4 -177.9(4) . . . . ? C2 C3 C4 C5 -2.7(7) . . . . ? C3 C4 C5 C10 -1.0(7) . . . . ? C3 C4 C5 C6 179.8(4) . . . . ? C4 C5 C6 C7 177.4(4) . . . . ? C10 C5 C6 C7 -1.8(6) . . . . ? C5 C6 C7 C8 -1.4(6) . . . . ? C6 C7 C8 C9 2.5(6) . . . . ? C7 C8 C9 C10 -0.2(6) . . . . ? C8 C9 C10 C5 -3.1(6) . . . . ? C8 C9 C10 C1 177.9(4) . . . . ? C4 C5 C10 C9 -175.2(4) . . . . ? C6 C5 C10 C9 4.1(6) . . . . ? C4 C5 C10 C1 3.9(6) . . . . ? C6 C5 C10 C1 -176.8(3) . . . . ? C2 C1 C10 C9 175.7(4) . . . . ? C2 C1 C10 C5 -3.3(5) . . . . ? C1 C2 C11 C16 129.9(5) . . . . ? C3 C2 C11 C16 -48.8(6) . . . . ? C1 C2 C11 C12 -51.5(6) . . . . ? C3 C2 C11 C12 129.8(5) . . . . ? C16 C11 C12 C13 1.7(6) . . . . ? C2 C11 C12 C13 -177.0(4) . . . . ? C11 C12 C13 C14 -0.9(6) . . . . ? C12 C13 C14 C15 -1.1(5) . . . . ? C12 C13 C14 C17 175.7(3) . . . . ? C13 C14 C15 C16 2.4(5) . . . . ? C17 C14 C15 C16 -174.6(3) . . . . ? C14 C15 C16 C11 -1.7(6) . . . . ? C12 C11 C16 C15 -0.4(6) . . . . ? C2 C11 C16 C15 178.3(4) . . . . ? C13 C14 C17 O1 -176.0(3) . . . . ? C15 C14 C17 O1 0.8(5) . . . . ? C13 C14 C17 C18 2.5(5) . . . . ? C15 C14 C17 C18 179.3(3) . . . . ? O1 C17 C18 P1 8.1(5) . . . . ? C14 C17 C18 P1 -170.3(3) . . . . ? C31 P1 C18 C17 172.3(3) . . . . ? C19 P1 C18 C17 54.9(5) . . . . ? C25 P1 C18 C17 -68.9(6) . . . . ? C18 P1 C19 C24 38.1(5) . . . . ? C31 P1 C19 C24 -79.1(6) . . . . ? C25 P1 C19 C24 167.9(3) . . . . ? C18 P1 C19 C20 -147.3(4) . . . . ? C31 P1 C19 C20 95.5(6) . . . . ? C25 P1 C19 C20 -17.5(4) . . . . ? C24 C19 C20 C21 0.3(5) . . . . ? P1 C19 C20 C21 -174.3(3) . . . . ? C19 C20 C21 C22 0.9(6) . . . . ? C20 C21 C22 C23 -1.6(6) . . . . ? C21 C22 C23 C24 1.1(7) . . . . ? C22 C23 C24 C19 0.2(7) . . . . ? C20 C19 C24 C23 -0.9(6) . . . . ? P1 C19 C24 C23 173.9(4) . . . . ? C18 P1 C25 C26 -110.9(6) . . . . ? C31 P1 C25 C26 8.0(4) . . . . ? C19 P1 C25 C26 121.4(6) . . . . ? C18 P1 C25 C30 68.0(6) . . . . ? C31 P1 C25 C30 -173.2(3) . . . . ? C19 P1 C25 C30 -59.8(6) . . . . ? C30 C25 C26 C27 -0.3(6) . . . . ? P1 C25 C26 C27 178.6(3) . . . . ? C25 C26 C27 C28 0.7(6) . . . . ? C26 C27 C28 C29 -1.4(6) . . . . ? C27 C28 C29 C30 1.8(6) . . . . ? C28 C29 C30 C25 -1.4(6) . . . . ? C26 C25 C30 C29 0.7(5) . . . . ? P1 C25 C30 C29 -178.2(3) . . . . ? C18 P1 C31 C36 48.5(5) . . . . ? C19 P1 C31 C36 170.3(3) . . . . ? C25 P1 C31 C36 -77.2(5) . . . . ? C18 P1 C31 C32 -132.2(5) . . . . ? C19 P1 C31 C32 -10.4(3) . . . . ? C25 P1 C31 C32 102.1(5) . . . . ? C36 C31 C32 C33 -1.0(5) . . . . ? P1 C31 C32 C33 179.7(3) . . . . ? C31 C32 C33 C34 0.8(6) . . . . ? C32 C33 C34 C35 0.0(6) . . . . ? C33 C34 C35 C36 -0.6(6) . . . . ? C32 C31 C36 C35 0.4(5) . . . . ? P1 C31 C36 C35 179.8(3) . . . . ? C34 C35 C36 C31 0.3(6) . . . . ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================