# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Charles L. B. Macdonald' 'Michelle Carlesimo' 'Bobby D. Ellis' _publ_contact_author_name 'Charles L. B. Macdonald' _publ_contact_author_address ; Department of Chemistry and Biochemistry The University of Windsor Windsor Ontario N9B 3P4 CANADA ; _publ_contact_author_email cmacd@uwindsor.ca _publ_requested_journal 'Chemical Communications' _publ_section_title ; Stabilised Phosphorus (I) and Arsenic (I) Iodide: Readily-synthesised reagents for low oxidation state main group chemistry ; data_bde311s _database_code_CSD 212868 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'triphosphenium iodide' _chemical_melting_point 149-150 _chemical_formula_moiety '[C26 H24 P3][I1]' _chemical_formula_sum 'C26 H24 I P3' _chemical_formula_weight 556.26 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' I I -0.4742 1.8119 '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 10.1340(5) _cell_length_b 13.5928(7) _cell_length_c 19.7256(10) _cell_angle_alpha 71.9900(10) _cell_angle_beta 81.3070(10) _cell_angle_gamma 68.8530(10) _cell_volume 2407.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 174 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.541 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; crystals were covered in Nujol and placed rapidly into the cold N2 stream ; _diffrn_ambient_temperature 174(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23284 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 27.54 _reflns_number_total 10966 _reflns_number_gt 9345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0352P)^2^+5.3099P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10966 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_restrained_S_all 1.207 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C121 C 0.1692(5) 0.7892(3) 0.2093(2) 0.0239(9) Uani 1 1 d . . . C122 C 0.0687(5) 0.7867(4) 0.1695(3) 0.0310(11) Uani 1 1 d . . . H122 H 0.0938 0.7355 0.1435 0.037 Uiso 1 1 calc R . . C123 C -0.0693(5) 0.8605(4) 0.1683(3) 0.0358(12) Uani 1 1 d . . . H123 H -0.1360 0.8592 0.1412 0.043 Uiso 1 1 calc R . . C124 C -0.1064(6) 0.9356(4) 0.2077(3) 0.0378(12) Uani 1 1 d . . . H124 H -0.1983 0.9849 0.2070 0.045 Uiso 1 1 calc R . . C125 C -0.0081(6) 0.9378(4) 0.2479(3) 0.0408(13) Uani 1 1 d . . . H125 H -0.0337 0.9884 0.2743 0.049 Uiso 1 1 calc R . . C126 C 0.1289(5) 0.8646(4) 0.2490(3) 0.0338(11) Uani 1 1 d . . . H126 H 0.1946 0.8660 0.2766 0.041 Uiso 1 1 calc R . . C212 C 0.7226(5) 0.0737(4) 0.4009(3) 0.0297(10) Uani 1 1 d . . . H212 H 0.6362 0.1276 0.3870 0.036 Uiso 1 1 calc R . . C231 C 1.0010(5) 0.1990(3) 0.1225(2) 0.0219(9) Uani 1 1 d . . . C232 C 1.1469(5) 0.1484(4) 0.1217(3) 0.0285(10) Uani 1 1 d . . . H232 H 1.2005 0.1547 0.1534 0.034 Uiso 1 1 calc R . . C233 C 1.2125(5) 0.0883(4) 0.0730(3) 0.0325(11) Uani 1 1 d . . . H233 H 1.3105 0.0565 0.0709 0.039 Uiso 1 1 calc R . . C234 C 1.1313(6) 0.0756(4) 0.0274(3) 0.0354(12) Uani 1 1 d . . . H234 H 1.1754 0.0338 -0.0043 0.043 Uiso 1 1 calc R . . C235 C 0.9870(6) 0.1241(4) 0.0288(3) 0.0383(12) Uani 1 1 d . . . H235 H 0.9337 0.1151 -0.0018 0.046 Uiso 1 1 calc R . . C236 C 0.9200(5) 0.1869(4) 0.0759(3) 0.0309(11) Uani 1 1 d . . . H236 H 0.8221 0.2205 0.0765 0.037 Uiso 1 1 calc R . . C11 C 0.4333(5) 0.8080(4) 0.1467(3) 0.0298(10) Uani 1 1 d . . . H02A H 0.4438 0.8030 0.0980 0.036 Uiso 1 1 calc R . . H02B H 0.3703 0.8811 0.1469 0.036 Uiso 1 1 calc R . . C12 C 0.5766(5) 0.7903(4) 0.1714(2) 0.0290(10) Uani 1 1 d . . . H00E H 0.5974 0.8584 0.1548 0.035 Uiso 1 1 calc R . . H00F H 0.6497 0.7359 0.1517 0.035 Uiso 1 1 calc R . . C21 C 0.6969(5) 0.3038(4) 0.2805(2) 0.0250(9) Uani 1 1 d . . . H00C H 0.6147 0.2851 0.3045 0.030 Uiso 1 1 calc R . . H00D H 0.6726 0.3829 0.2673 0.030 Uiso 1 1 calc R . . C22 C 0.7418(4) 0.2625(4) 0.2148(2) 0.0242(9) Uani 1 1 d . . . H00A H 0.6725 0.3040 0.1785 0.029 Uiso 1 1 calc R . . H00B H 0.7510 0.1856 0.2266 0.029 Uiso 1 1 calc R . . C111 C 0.3604(4) 0.6042(4) 0.1613(2) 0.0233(9) Uani 1 1 d . . . C112 C 0.3562(5) 0.6291(4) 0.0874(3) 0.0304(10) Uani 1 1 d . . . H112 H 0.3515 0.6988 0.0586 0.037 Uiso 1 1 calc R . . C113 C 0.3591(5) 0.5481(4) 0.0573(3) 0.0355(12) Uani 1 1 d . . . H113 H 0.3553 0.5640 0.0081 0.043 Uiso 1 1 calc R . . C114 C 0.3677(6) 0.4436(5) 0.1002(3) 0.0399(13) Uani 1 1 d . . . H114 H 0.3728 0.3893 0.0797 0.048 Uiso 1 1 calc R . . C115 C 0.3687(5) 0.4204(4) 0.1736(3) 0.0353(12) Uani 1 1 d . . . H115 H 0.3713 0.3511 0.2023 0.042 Uiso 1 1 calc R . . C116 C 0.3659(5) 0.5000(4) 0.2045(3) 0.0288(10) Uani 1 1 d . . . H116 H 0.3677 0.4840 0.2538 0.035 Uiso 1 1 calc R . . C131 C 0.7553(5) 0.6814(4) 0.2953(2) 0.0252(9) Uani 1 1 d . . . C132 C 0.8071(5) 0.7207(4) 0.3389(3) 0.0298(10) Uani 1 1 d . . . H132 H 0.7470 0.7777 0.3570 0.036 Uiso 1 1 calc R . . C133 C 0.9488(6) 0.6748(4) 0.3554(3) 0.0352(12) Uani 1 1 d . . . H133 H 0.9836 0.7007 0.3849 0.042 Uiso 1 1 calc R . . C134 C 1.0377(5) 0.5907(4) 0.3280(3) 0.0335(11) Uani 1 1 d . . . H134 H 1.1328 0.5605 0.3389 0.040 Uiso 1 1 calc R . . C135 C 0.9871(5) 0.5510(4) 0.2848(3) 0.0347(11) Uani 1 1 d . . . H135 H 1.0481 0.4942 0.2667 0.042 Uiso 1 1 calc R . . C136 C 0.8462(5) 0.5951(4) 0.2682(3) 0.0301(10) Uani 1 1 d . . . H136 H 0.8119 0.5679 0.2393 0.036 Uiso 1 1 calc R . . C141 C 0.4925(5) 0.8592(4) 0.3055(3) 0.0259(10) Uani 1 1 d . . . C142 C 0.4331(6) 0.8404(4) 0.3745(3) 0.0377(12) Uani 1 1 d . . . H142 H 0.4332 0.7702 0.3998 0.045 Uiso 1 1 calc R . . C143 C 0.3739(6) 0.9257(5) 0.4055(3) 0.0442(14) Uani 1 1 d . . . H143 H 0.3357 0.9125 0.4520 0.053 Uiso 1 1 calc R . . C144 C 0.3712(6) 1.0289(5) 0.3685(3) 0.0420(13) Uani 1 1 d . . . H144 H 0.3311 1.0861 0.3897 0.050 Uiso 1 1 calc R . . C145 C 0.4277(6) 1.0490(4) 0.2997(3) 0.0453(14) Uani 1 1 d . . . H145 H 0.4247 1.1200 0.2745 0.054 Uiso 1 1 calc R . . C146 C 0.4892(6) 0.9646(4) 0.2675(3) 0.0357(12) Uani 1 1 d . . . H146 H 0.5276 0.9784 0.2211 0.043 Uiso 1 1 calc R . . C211 C 0.8469(5) 0.0997(3) 0.3857(2) 0.0207(9) Uani 1 1 d . . . C213 C 0.7286(6) -0.0338(4) 0.4371(3) 0.0350(11) Uani 1 1 d . . . H213 H 0.6458 -0.0514 0.4474 0.042 Uiso 1 1 calc R . . C214 C 0.8565(6) -0.1135(4) 0.4576(3) 0.0328(11) Uani 1 1 d . . . H214 H 0.8600 -0.1850 0.4818 0.039 Uiso 1 1 calc R . . C215 C 0.9792(6) -0.0878(4) 0.4424(3) 0.0373(12) Uani 1 1 d . . . H215 H 1.0654 -0.1421 0.4563 0.045 Uiso 1 1 calc R . . C216 C 0.9752(5) 0.0185(4) 0.4066(3) 0.0320(11) Uani 1 1 d . . . H216 H 1.0585 0.0353 0.3965 0.038 Uiso 1 1 calc R . . C221 C 0.8202(5) 0.3117(3) 0.4045(2) 0.0219(9) Uani 1 1 d . . . C222 C 0.6912(5) 0.3338(4) 0.4441(3) 0.0330(11) Uani 1 1 d . . . H222 H 0.6207 0.3094 0.4372 0.040 Uiso 1 1 calc R . . C223 C 0.6694(6) 0.3924(4) 0.4936(3) 0.0399(13) Uani 1 1 d . . . H223 H 0.5842 0.4071 0.5203 0.048 Uiso 1 1 calc R . . C224 C 0.7740(7) 0.4291(4) 0.5036(3) 0.0417(14) Uani 1 1 d . . . H224 H 0.7582 0.4697 0.5361 0.050 Uiso 1 1 calc R . . C225 C 0.9018(6) 0.4057(4) 0.4653(3) 0.0383(12) Uani 1 1 d . . . H225 H 0.9723 0.4293 0.4729 0.046 Uiso 1 1 calc R . . C226 C 0.9262(5) 0.3470(4) 0.4154(2) 0.0289(10) Uani 1 1 d . . . H226 H 1.0123 0.3317 0.3895 0.035 Uiso 1 1 calc R . . C241 C 0.8807(5) 0.4223(3) 0.1301(2) 0.0211(9) Uani 1 1 d . . . C242 C 0.9945(6) 0.4609(4) 0.1151(3) 0.0355(12) Uani 1 1 d . . . H242 H 1.0825 0.4151 0.1330 0.043 Uiso 1 1 calc R . . C243 C 0.9778(6) 0.5678(4) 0.0736(3) 0.0425(13) Uani 1 1 d . . . H243 H 1.0542 0.5934 0.0639 0.051 Uiso 1 1 calc R . . C244 C 0.8478(6) 0.6356(4) 0.0467(3) 0.0395(13) Uani 1 1 d . . . H244 H 0.8366 0.7068 0.0185 0.047 Uiso 1 1 calc R . . C245 C 0.7340(6) 0.5979(4) 0.0616(3) 0.0327(11) Uani 1 1 d . . . H245 H 0.6464 0.6442 0.0436 0.039 Uiso 1 1 calc R . . C246 C 0.7492(5) 0.4916(4) 0.1033(2) 0.0271(10) Uani 1 1 d . . . H246 H 0.6721 0.4669 0.1133 0.033 Uiso 1 1 calc R . . I1 I 0.33762(3) 0.31078(3) 0.400515(19) 0.03462(10) Uani 1 1 d . . . P11 P 0.46723(14) 0.62649(10) 0.29904(7) 0.0295(3) Uani 1 1 d . . . P12 P 0.35374(13) 0.70696(9) 0.20356(6) 0.0237(2) Uani 1 1 d . . . P13 P 0.57430(13) 0.74338(10) 0.26876(6) 0.0241(2) Uani 1 1 d . . . P21 P 1.03321(13) 0.23899(11) 0.27333(7) 0.0296(3) Uani 1 1 d . . . P22 P 0.84596(12) 0.23807(9) 0.33914(6) 0.0207(2) Uani 1 1 d . . . P23 P 0.91242(12) 0.28103(9) 0.18291(6) 0.0206(2) Uani 1 1 d . . . I2 I 0.56469(4) 0.13896(3) 0.075367(18) 0.03561(10) 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 C121 0.024(2) 0.020(2) 0.025(2) -0.0031(17) -0.0002(18) -0.0071(18) C122 0.035(3) 0.030(2) 0.031(3) -0.011(2) 0.001(2) -0.012(2) C123 0.024(3) 0.043(3) 0.037(3) -0.009(2) -0.003(2) -0.008(2) C124 0.028(3) 0.030(3) 0.043(3) -0.004(2) -0.003(2) 0.000(2) C125 0.042(3) 0.030(3) 0.047(3) -0.019(2) 0.000(3) -0.004(2) C126 0.035(3) 0.029(2) 0.039(3) -0.013(2) -0.006(2) -0.008(2) C212 0.026(2) 0.025(2) 0.034(3) -0.007(2) 0.001(2) -0.0056(19) C231 0.026(2) 0.0166(19) 0.023(2) -0.0047(17) 0.0030(17) -0.0094(17) C232 0.028(2) 0.027(2) 0.029(2) -0.0048(19) -0.0038(19) -0.009(2) C233 0.028(3) 0.020(2) 0.039(3) -0.004(2) 0.006(2) -0.0024(19) C234 0.050(3) 0.023(2) 0.037(3) -0.015(2) 0.010(2) -0.016(2) C235 0.053(4) 0.036(3) 0.036(3) -0.016(2) -0.001(2) -0.023(3) C236 0.029(3) 0.029(2) 0.039(3) -0.013(2) 0.000(2) -0.012(2) C11 0.037(3) 0.029(2) 0.025(2) -0.0037(19) 0.001(2) -0.018(2) C12 0.037(3) 0.032(2) 0.017(2) -0.0079(19) -0.0001(19) -0.010(2) C21 0.022(2) 0.025(2) 0.027(2) -0.0031(18) -0.0042(18) -0.0078(18) C22 0.018(2) 0.027(2) 0.028(2) -0.0054(19) -0.0001(17) -0.0096(18) C111 0.019(2) 0.023(2) 0.028(2) -0.0117(18) -0.0005(18) -0.0037(18) C112 0.029(3) 0.033(3) 0.030(3) -0.012(2) 0.002(2) -0.010(2) C113 0.029(3) 0.045(3) 0.034(3) -0.021(2) 0.002(2) -0.007(2) C114 0.031(3) 0.041(3) 0.053(3) -0.030(3) -0.002(2) -0.004(2) C115 0.028(3) 0.028(2) 0.053(3) -0.015(2) -0.007(2) -0.008(2) C116 0.027(2) 0.030(2) 0.032(3) -0.013(2) -0.001(2) -0.008(2) C131 0.028(2) 0.020(2) 0.028(2) -0.0048(18) -0.0033(19) -0.0095(18) C132 0.032(3) 0.028(2) 0.029(2) -0.010(2) -0.005(2) -0.007(2) C133 0.041(3) 0.034(3) 0.033(3) -0.007(2) -0.012(2) -0.013(2) C134 0.028(3) 0.031(3) 0.034(3) 0.001(2) -0.008(2) -0.006(2) C135 0.032(3) 0.026(2) 0.040(3) -0.008(2) 0.000(2) -0.004(2) C136 0.034(3) 0.034(3) 0.029(3) -0.016(2) 0.001(2) -0.014(2) C141 0.023(2) 0.023(2) 0.033(3) -0.0100(19) -0.0053(19) -0.0063(18) C142 0.049(3) 0.031(3) 0.036(3) -0.011(2) 0.006(2) -0.019(2) C143 0.046(3) 0.049(3) 0.047(3) -0.028(3) 0.007(3) -0.018(3) C144 0.034(3) 0.039(3) 0.061(4) -0.031(3) -0.005(3) -0.006(2) C145 0.051(4) 0.023(3) 0.058(4) -0.007(2) -0.009(3) -0.009(2) C146 0.041(3) 0.030(3) 0.039(3) -0.011(2) -0.001(2) -0.015(2) C211 0.029(2) 0.0169(19) 0.017(2) -0.0063(16) 0.0003(17) -0.0077(17) C213 0.039(3) 0.030(3) 0.038(3) -0.009(2) 0.003(2) -0.017(2) C214 0.049(3) 0.024(2) 0.025(2) -0.0055(19) -0.002(2) -0.013(2) C215 0.034(3) 0.027(2) 0.041(3) 0.000(2) -0.010(2) -0.004(2) C216 0.030(3) 0.030(2) 0.035(3) -0.003(2) -0.006(2) -0.011(2) C221 0.029(2) 0.018(2) 0.017(2) -0.0041(16) -0.0046(17) -0.0058(18) C222 0.028(3) 0.030(3) 0.038(3) -0.010(2) -0.005(2) -0.005(2) C223 0.043(3) 0.038(3) 0.030(3) -0.015(2) 0.004(2) -0.001(2) C224 0.069(4) 0.027(3) 0.030(3) -0.010(2) -0.011(3) -0.012(3) C225 0.055(4) 0.035(3) 0.032(3) -0.006(2) -0.008(2) -0.022(3) C226 0.035(3) 0.029(2) 0.024(2) -0.0032(19) -0.003(2) -0.014(2) C241 0.030(2) 0.018(2) 0.014(2) -0.0054(16) -0.0010(17) -0.0061(17) C242 0.034(3) 0.028(2) 0.044(3) -0.006(2) 0.000(2) -0.013(2) C243 0.047(3) 0.033(3) 0.050(3) -0.009(2) 0.006(3) -0.022(3) C244 0.057(4) 0.025(2) 0.031(3) -0.006(2) 0.008(2) -0.011(2) C245 0.040(3) 0.024(2) 0.026(2) -0.0049(19) -0.008(2) 0.000(2) C246 0.029(2) 0.027(2) 0.026(2) -0.0084(19) -0.0029(19) -0.0084(19) I1 0.02377(17) 0.02615(16) 0.0500(2) -0.00864(14) 0.00426(14) -0.00768(13) P11 0.0383(7) 0.0258(6) 0.0256(6) -0.0023(5) -0.0062(5) -0.0144(5) P12 0.0245(6) 0.0224(5) 0.0253(6) -0.0072(5) -0.0018(5) -0.0082(5) P13 0.0263(6) 0.0246(6) 0.0231(6) -0.0081(5) -0.0009(5) -0.0094(5) P21 0.0201(6) 0.0415(7) 0.0241(6) -0.0052(5) -0.0031(5) -0.0093(5) P22 0.0222(6) 0.0204(5) 0.0194(5) -0.0046(4) -0.0015(4) -0.0074(4) P23 0.0188(5) 0.0210(5) 0.0200(5) -0.0037(4) -0.0013(4) -0.0056(4) I2 0.03093(18) 0.03606(18) 0.03379(18) 0.00030(14) -0.00379(13) -0.01162(14) _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 C121 C126 1.387(7) . ? C121 C122 1.393(6) . ? C121 P12 1.807(5) . ? C122 C123 1.396(7) . ? C123 C124 1.382(8) . ? C124 C125 1.377(8) . ? C125 C126 1.385(7) . ? C212 C211 1.394(6) . ? C212 C213 1.397(6) . ? C231 C232 1.388(6) . ? C231 C236 1.403(6) . ? C231 P23 1.801(4) . ? C232 C233 1.390(7) . ? C233 C234 1.392(7) . ? C234 C235 1.370(8) . ? C235 C236 1.390(7) . ? C11 C12 1.515(7) . ? C11 P12 1.835(5) . ? C12 P13 1.827(5) . ? C21 C22 1.512(6) . ? C21 P22 1.826(4) . ? C22 P23 1.826(4) . ? C111 C112 1.395(6) . ? C111 C116 1.395(6) . ? C111 P12 1.813(4) . ? C112 C113 1.393(7) . ? C113 C114 1.389(8) . ? C114 C115 1.383(8) . ? C115 C116 1.387(7) . ? C131 C132 1.387(6) . ? C131 C136 1.403(6) . ? C131 P13 1.803(5) . ? C132 C133 1.387(7) . ? C133 C134 1.379(7) . ? C134 C135 1.378(7) . ? C135 C136 1.381(7) . ? C141 C146 1.386(7) . ? C141 C142 1.389(7) . ? C141 P13 1.809(5) . ? C142 C143 1.381(7) . ? C143 C144 1.359(8) . ? C144 C145 1.375(8) . ? C145 C146 1.388(7) . ? C211 C216 1.387(6) . ? C211 P22 1.818(4) . ? C213 C214 1.376(7) . ? C214 C215 1.377(7) . ? C215 C216 1.387(7) . ? C221 C226 1.392(6) . ? C221 C222 1.400(7) . ? C221 P22 1.800(4) . ? C222 C223 1.390(7) . ? C223 C224 1.384(8) . ? C224 C225 1.380(8) . ? C225 C226 1.391(7) . ? C241 C242 1.390(7) . ? C241 C246 1.393(6) . ? C241 P23 1.815(4) . ? C242 C243 1.393(7) . ? C243 C244 1.378(8) . ? C244 C245 1.381(8) . ? C245 C246 1.389(6) . ? P11 P13 2.1260(17) . ? P11 P12 2.1305(17) . ? P21 P23 2.1286(16) . ? P21 P22 2.1328(17) . ? 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 C126 C121 C122 118.9(4) . . ? C126 C121 P12 119.2(4) . . ? C122 C121 P12 121.6(4) . . ? C121 C122 C123 120.4(5) . . ? C124 C123 C122 119.5(5) . . ? C125 C124 C123 120.4(5) . . ? C124 C125 C126 120.1(5) . . ? C125 C126 C121 120.7(5) . . ? C211 C212 C213 119.7(4) . . ? C232 C231 C236 120.1(4) . . ? C232 C231 P23 121.0(4) . . ? C236 C231 P23 118.8(3) . . ? C231 C232 C233 119.6(5) . . ? C232 C233 C234 120.0(5) . . ? C235 C234 C233 120.6(5) . . ? C234 C235 C236 120.2(5) . . ? C235 C236 C231 119.5(5) . . ? C12 C11 P12 112.1(3) . . ? C11 C12 P13 109.1(3) . . ? C22 C21 P22 107.3(3) . . ? C21 C22 P23 106.4(3) . . ? C112 C111 C116 120.5(4) . . ? C112 C111 P12 121.0(3) . . ? C116 C111 P12 118.5(3) . . ? C113 C112 C111 119.0(5) . . ? C114 C113 C112 120.4(5) . . ? C115 C114 C113 120.1(5) . . ? C114 C115 C116 120.2(5) . . ? C115 C116 C111 119.7(5) . . ? C132 C131 C136 119.9(4) . . ? C132 C131 P13 121.3(4) . . ? C136 C131 P13 118.7(4) . . ? C131 C132 C133 119.9(5) . . ? C134 C133 C132 119.9(5) . . ? C135 C134 C133 120.6(5) . . ? C134 C135 C136 120.3(5) . . ? C135 C136 C131 119.4(5) . . ? C146 C141 C142 119.6(5) . . ? C146 C141 P13 122.3(4) . . ? C142 C141 P13 118.1(4) . . ? C143 C142 C141 120.0(5) . . ? C144 C143 C142 120.4(6) . . ? C143 C144 C145 120.1(5) . . ? C144 C145 C146 120.7(5) . . ? C141 C146 C145 119.2(5) . . ? C216 C211 C212 119.6(4) . . ? C216 C211 P22 118.7(3) . . ? C212 C211 P22 121.7(3) . . ? C214 C213 C212 120.2(5) . . ? C213 C214 C215 120.1(5) . . ? C214 C215 C216 120.5(5) . . ? C215 C216 C211 120.0(5) . . ? C226 C221 C222 120.3(4) . . ? C226 C221 P22 120.6(4) . . ? C222 C221 P22 119.0(4) . . ? C223 C222 C221 119.4(5) . . ? C224 C223 C222 120.3(5) . . ? C225 C224 C223 120.1(5) . . ? C224 C225 C226 120.7(5) . . ? C225 C226 C221 119.2(5) . . ? C242 C241 C246 119.4(4) . . ? C242 C241 P23 117.7(3) . . ? C246 C241 P23 122.9(3) . . ? C241 C242 C243 120.4(5) . . ? C244 C243 C242 119.8(5) . . ? C243 C244 C245 120.0(5) . . ? C244 C245 C246 120.7(5) . . ? C245 C246 C241 119.6(5) . . ? P13 P11 P12 89.35(6) . . ? C121 P12 C111 106.2(2) . . ? C121 P12 C11 102.3(2) . . ? C111 P12 C11 112.7(2) . . ? C121 P12 P11 118.84(16) . . ? C111 P12 P11 108.52(15) . . ? C11 P12 P11 108.25(17) . . ? C131 P13 C141 107.3(2) . . ? C131 P13 C12 107.9(2) . . ? C141 P13 C12 110.0(2) . . ? C131 P13 P11 111.31(15) . . ? C141 P13 P11 114.10(16) . . ? C12 P13 P11 106.00(17) . . ? P23 P21 P22 88.45(6) . . ? C221 P22 C211 108.19(19) . . ? C221 P22 C21 109.3(2) . . ? C211 P22 C21 107.8(2) . . ? C221 P22 P21 112.18(16) . . ? C211 P22 P21 112.19(15) . . ? C21 P22 P21 107.13(16) . . ? C231 P23 C241 105.46(19) . . ? C231 P23 C22 110.2(2) . . ? C241 P23 C22 108.6(2) . . ? C231 P23 P21 112.19(16) . . ? C241 P23 P21 112.36(15) . . ? C22 P23 P21 108.04(15) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.450 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.111 data_p21-p21c _database_code_CSD 212869 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'triphosphenium tetraphenylborate' _chemical_melting_point 142-3 _chemical_formula_moiety '[C26 H24 P3][C24 H20 B]' _chemical_formula_sum 'C50 H44 B P3' _chemical_formula_weight 748.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9875(6) _cell_length_b 17.5408(6) _cell_length_c 20.9570(9) _cell_angle_alpha 90.00 _cell_angle_beta 113.179(15) _cell_angle_gamma 90.00 _cell_volume 4050.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 174(2) _cell_measurement_reflns_used 8052 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.182 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; crystals were covered in Nujol and placed rapidly into the cold N2 stream ; _diffrn_ambient_temperature 174(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29472 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.51 _reflns_number_total 9065 _reflns_number_gt 7146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0000P)^2^+11.1148P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9065 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1414 _refine_ls_R_factor_gt 0.1190 _refine_ls_wR_factor_ref 0.2253 _refine_ls_wR_factor_gt 0.2134 _refine_ls_goodness_of_fit_ref 1.399 _refine_ls_restrained_S_all 1.399 _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 P11 P 0.19432(12) 0.29409(7) 0.30068(7) 0.0298(3) Uani 1 1 d . . . P12 P 0.12385(13) 0.18841(8) 0.25038(7) 0.0352(3) Uani 1 1 d . . . P13 P 0.12933(13) 0.23848(8) 0.15948(7) 0.0340(3) Uani 1 1 d . . . C14 C 0.2659(5) 0.2962(3) 0.1889(3) 0.0374(12) Uani 1 1 d . . . H14A H 0.336(3) 0.2641(13) 0.2030(6) 0.045 Uiso 1 1 calc R . . H14B H 0.2660(5) 0.3285(13) 0.1520(14) 0.045 Uiso 1 1 calc R . . C15 C 0.2683(5) 0.3444(3) 0.2500(3) 0.0378(12) Uani 1 1 d . . . H15A H 0.2265(16) 0.3924(19) 0.2329(7) 0.045 Uiso 1 1 calc R . . H15B H 0.352(3) 0.3559(6) 0.2801(12) 0.045 Uiso 1 1 calc R . . C111 C 0.3046(4) 0.2767(3) 0.3875(3) 0.0306(10) Uani 1 1 d . . . C112 C 0.3093(5) 0.3189(4) 0.4439(3) 0.0464(14) Uani 1 1 d . . . H112 H 0.248(4) 0.363(3) 0.4372(5) 0.056 Uiso 1 1 calc R . . C113 C 0.3955(6) 0.3034(4) 0.5093(3) 0.0600(19) Uani 1 1 d . . . H113 H 0.3985(6) 0.334(2) 0.549(3) 0.072 Uiso 1 1 calc R . . C114 C 0.4773(6) 0.2449(4) 0.5187(3) 0.0560(17) Uani 1 1 d . . . H114 H 0.541(4) 0.2332(9) 0.568(3) 0.067 Uiso 1 1 calc R . . C115 C 0.4743(6) 0.2023(4) 0.4630(3) 0.0592(19) Uani 1 1 d . . . H115 H 0.531(4) 0.161(3) 0.4696(6) 0.071 Uiso 1 1 calc R . . C116 C 0.3890(5) 0.2193(3) 0.3969(3) 0.0451(14) Uani 1 1 d . . . H116 H 0.3886(5) 0.1934(18) 0.361(3) 0.054 Uiso 1 1 calc R . . C121 C 0.0823(5) 0.3591(3) 0.3066(3) 0.0336(11) Uani 1 1 d . . . C122 C -0.0335(5) 0.3329(4) 0.2954(3) 0.0414(13) Uani 1 1 d . . . H122 H -0.0516(12) 0.280(3) 0.2875(6) 0.050 Uiso 1 1 calc R . . C123 C -0.1223(6) 0.3826(4) 0.2955(3) 0.0542(17) Uani 1 1 d . . . H123 H -0.195(6) 0.3650(14) 0.2892(6) 0.065 Uiso 1 1 calc R . . C124 C -0.0980(6) 0.4592(4) 0.3054(3) 0.0542(17) Uani 1 1 d . . . H124 H -0.156(5) 0.491(3) 0.3041(3) 0.065 Uiso 1 1 calc R . . C125 C 0.0177(6) 0.4868(4) 0.3176(3) 0.0479(15) Uani 1 1 d . . . H125 H 0.0355(13) 0.542(4) 0.3259(6) 0.058 Uiso 1 1 calc R . . C126 C 0.1078(5) 0.4370(3) 0.3182(3) 0.0393(12) Uani 1 1 d . . . H126 H 0.187(5) 0.4558(12) 0.3264(6) 0.047 Uiso 1 1 calc R . . C131 C 0.1368(5) 0.1656(3) 0.1013(3) 0.0391(12) Uani 1 1 d . . . C132 C 0.2340(6) 0.1145(4) 0.1232(3) 0.0491(15) Uani 1 1 d . . . H132 H 0.303(4) 0.1205(5) 0.173(3) 0.059 Uiso 1 1 calc R . . C133 C 0.2402(7) 0.0565(4) 0.0807(4) 0.0606(18) Uani 1 1 d . . . H133 H 0.306(5) 0.022(3) 0.0965(13) 0.073 Uiso 1 1 calc R . . C134 C 0.1506(7) 0.0490(4) 0.0149(4) 0.0590(19) Uani 1 1 d . . . H134 H 0.1550(8) 0.007(3) -0.016(2) 0.071 Uiso 1 1 calc R . . C135 C 0.0552(7) 0.0996(4) -0.0079(4) 0.0592(18) Uani 1 1 d . . . H135 H -0.004(5) 0.0945(5) -0.052(3) 0.071 Uiso 1 1 calc R . . C136 C 0.0475(6) 0.1577(4) 0.0343(3) 0.0472(14) Uani 1 1 d . . . H136 H -0.020(4) 0.193(2) 0.0175(11) 0.057 Uiso 1 1 calc R . . C141 C 0.0033(5) 0.2998(3) 0.1109(2) 0.0342(11) Uani 1 1 d . . . C142 C -0.1030(5) 0.2961(4) 0.1229(3) 0.0462(14) Uani 1 1 d . . . H142 H -0.1086(6) 0.264(2) 0.156(2) 0.055 Uiso 1 1 calc R . . C143 C -0.1997(6) 0.3419(4) 0.0845(3) 0.0578(18) Uani 1 1 d . . . H143 H -0.274(5) 0.3387(5) 0.0917(6) 0.069 Uiso 1 1 calc R . . C144 C -0.1919(6) 0.3920(4) 0.0359(3) 0.0492(15) Uani 1 1 d . . . H144 H -0.263(5) 0.426(2) 0.0086(18) 0.059 Uiso 1 1 calc R . . C145 C -0.0859(6) 0.3961(3) 0.0246(3) 0.0456(14) Uani 1 1 d . . . H145 H -0.0801(7) 0.433(2) -0.012(2) 0.055 Uiso 1 1 calc R . . C146 C 0.0110(6) 0.3514(3) 0.0618(3) 0.0411(13) Uani 1 1 d . . . H146 H 0.088(5) 0.3554(4) 0.0539(5) 0.049 Uiso 1 1 calc R . . C151 C 0.8632(5) 0.1160(3) 0.3373(3) 0.0323(11) Uani 1 1 d . . . C152 C 0.9371(5) 0.1726(3) 0.3799(3) 0.0386(12) Uani 1 1 d . . . H152 H 0.896(2) 0.223(3) 0.3899(6) 0.046 Uiso 1 1 calc R . . C153 C 1.0643(6) 0.1663(4) 0.4103(3) 0.0504(16) Uani 1 1 d . . . H153 H 1.119(3) 0.213(3) 0.4431(19) 0.060 Uiso 1 1 calc R . . C154 C 1.1222(6) 0.1025(4) 0.3999(3) 0.0559(18) Uani 1 1 d . . . H154 H 1.210(6) 0.0979(6) 0.4209(15) 0.067 Uiso 1 1 calc R . . C155 C 1.0513(6) 0.0458(4) 0.3588(3) 0.0538(17) Uani 1 1 d . . . H155 H 1.089(3) 0.001(3) 0.3512(7) 0.065 Uiso 1 1 calc R . . C156 C 0.9264(5) 0.0530(3) 0.3283(3) 0.0420(13) Uani 1 1 d . . . H156 H 0.880(3) 0.011(3) 0.2986(19) 0.050 Uiso 1 1 calc R . . C161 C 0.6799(5) 0.0922(3) 0.2170(3) 0.0338(11) Uani 1 1 d . . . C162 C 0.7375(5) 0.1278(4) 0.1781(3) 0.0450(14) Uani 1 1 d . . . H162 H 0.799(4) 0.170(3) 0.2005(14) 0.054 Uiso 1 1 calc R . . C163 C 0.7127(6) 0.1075(4) 0.1095(3) 0.0539(17) Uani 1 1 d . . . H163 H 0.749(3) 0.1313(19) 0.0860(18) 0.065 Uiso 1 1 calc R . . C164 C 0.6304(6) 0.0496(4) 0.0783(3) 0.0528(16) Uani 1 1 d . . . H164 H 0.6121(13) 0.0345(10) 0.029(3) 0.063 Uiso 1 1 calc R . . C165 C 0.5743(5) 0.0130(4) 0.1153(3) 0.0479(15) Uani 1 1 d . . . H165 H 0.516(4) -0.030(3) 0.0932(14) 0.058 Uiso 1 1 calc R . . C166 C 0.5976(5) 0.0351(3) 0.1836(3) 0.0377(12) Uani 1 1 d . . . H166 H 0.555(3) 0.0094(15) 0.2086(15) 0.045 Uiso 1 1 calc R . . C171 C 0.6497(5) 0.0607(3) 0.3353(3) 0.0325(11) Uani 1 1 d . . . C172 C 0.5262(6) 0.0713(3) 0.3232(3) 0.0448(14) Uani 1 1 d . . . H172 H 0.477(3) 0.115(3) 0.289(2) 0.054 Uiso 1 1 calc R . . C173 C 0.4672(7) 0.0254(4) 0.3545(4) 0.0559(18) Uani 1 1 d . . . H173 H 0.387(6) 0.0342(8) 0.3455(8) 0.067 Uiso 1 1 calc R . . C174 C 0.5277(7) -0.0330(4) 0.3990(3) 0.0540(17) Uani 1 1 d . . . H174 H 0.480(3) -0.070(2) 0.4248(15) 0.065 Uiso 1 1 calc R . . C175 C 0.6476(7) -0.0453(3) 0.4110(3) 0.0498(16) Uani 1 1 d . . . H175 H 0.692(3) -0.087(3) 0.442(2) 0.060 Uiso 1 1 calc R . . C176 C 0.7075(5) 0.0007(3) 0.3791(3) 0.0358(12) Uani 1 1 d . . . H176 H 0.799(5) -0.0108(7) 0.3887(6) 0.043 Uiso 1 1 calc R . . C181 C 0.6647(5) 0.2054(3) 0.3021(3) 0.0373(12) Uani 1 1 d . . . C182 C 0.6790(6) 0.2365(3) 0.3670(4) 0.0537(16) Uani 1 1 d . . . H182 H 0.720(2) 0.199(2) 0.416(3) 0.064 Uiso 1 1 calc R . . C183 C 0.6454(7) 0.3101(4) 0.3748(5) 0.067(2) Uani 1 1 d . . . H183 H 0.6600(13) 0.3308(15) 0.424(3) 0.080 Uiso 1 1 calc R . . C184 C 0.5930(6) 0.3557(4) 0.3179(5) 0.070(3) Uani 1 1 d . . . H184 H 0.5720(19) 0.404(4) 0.3231(7) 0.084 Uiso 1 1 calc R . . C185 C 0.5719(5) 0.3280(4) 0.2529(5) 0.065(2) Uani 1 1 d . . . H185 H 0.532(3) 0.360(2) 0.212(3) 0.077 Uiso 1 1 calc R . . C186 C 0.6083(5) 0.2530(3) 0.2449(4) 0.0504(16) Uani 1 1 d . . . H186 H 0.5929(11) 0.2333(13) 0.197(3) 0.061 Uiso 1 1 calc R . . B1 B 0.7147(5) 0.1189(3) 0.2978(3) 0.0319(12) 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 P11 0.0246(6) 0.0305(6) 0.0325(6) 0.0006(5) 0.0093(5) -0.0022(5) P12 0.0394(8) 0.0323(7) 0.0309(7) 0.0027(5) 0.0106(6) -0.0087(6) P13 0.0349(7) 0.0357(7) 0.0296(6) 0.0018(5) 0.0108(6) -0.0068(6) C14 0.039(3) 0.037(3) 0.037(3) 0.000(2) 0.017(2) -0.006(2) C15 0.036(3) 0.036(3) 0.045(3) 0.000(2) 0.019(2) -0.009(2) C111 0.028(2) 0.027(2) 0.035(3) -0.0015(19) 0.010(2) -0.0014(19) C112 0.042(3) 0.047(3) 0.042(3) -0.007(3) 0.008(3) 0.013(3) C113 0.053(4) 0.076(5) 0.033(3) -0.013(3) -0.003(3) 0.018(3) C114 0.051(4) 0.065(4) 0.038(3) 0.001(3) 0.002(3) 0.012(3) C115 0.049(4) 0.065(4) 0.049(4) -0.002(3) 0.004(3) 0.029(3) C116 0.040(3) 0.053(4) 0.035(3) -0.003(2) 0.006(2) 0.015(3) C121 0.027(3) 0.039(3) 0.035(3) 0.009(2) 0.013(2) 0.002(2) C122 0.029(3) 0.049(3) 0.047(3) 0.006(3) 0.016(2) -0.002(2) C123 0.030(3) 0.079(5) 0.060(4) 0.008(3) 0.024(3) 0.006(3) C124 0.043(4) 0.066(4) 0.058(4) 0.013(3) 0.025(3) 0.022(3) C125 0.054(4) 0.039(3) 0.059(4) 0.011(3) 0.031(3) 0.016(3) C126 0.031(3) 0.044(3) 0.048(3) 0.008(2) 0.020(2) 0.003(2) C131 0.042(3) 0.041(3) 0.036(3) -0.001(2) 0.016(2) -0.008(2) C132 0.055(4) 0.052(4) 0.043(3) 0.000(3) 0.022(3) -0.002(3) C133 0.070(5) 0.056(4) 0.067(5) 0.000(3) 0.038(4) 0.006(4) C134 0.079(5) 0.050(4) 0.065(4) -0.015(3) 0.046(4) -0.016(4) C135 0.073(5) 0.058(4) 0.048(4) -0.011(3) 0.026(4) -0.015(4) C136 0.044(3) 0.047(3) 0.045(3) -0.006(3) 0.012(3) -0.009(3) C141 0.041(3) 0.034(3) 0.025(2) 0.001(2) 0.010(2) -0.010(2) C142 0.033(3) 0.054(4) 0.043(3) 0.010(3) 0.006(2) -0.010(3) C143 0.033(3) 0.070(5) 0.058(4) 0.016(3) 0.005(3) -0.002(3) C144 0.043(3) 0.049(4) 0.042(3) 0.002(3) 0.002(3) 0.004(3) C145 0.055(4) 0.042(3) 0.038(3) 0.007(2) 0.016(3) 0.001(3) C146 0.047(3) 0.041(3) 0.036(3) 0.004(2) 0.017(3) -0.005(3) C151 0.039(3) 0.028(2) 0.030(2) 0.000(2) 0.014(2) -0.002(2) C152 0.042(3) 0.037(3) 0.041(3) -0.003(2) 0.020(3) -0.009(2) C153 0.043(3) 0.066(4) 0.038(3) 0.001(3) 0.011(3) -0.023(3) C154 0.035(3) 0.090(5) 0.038(3) 0.018(3) 0.009(3) 0.000(3) C155 0.043(4) 0.064(4) 0.058(4) 0.023(3) 0.023(3) 0.019(3) C156 0.041(3) 0.039(3) 0.045(3) 0.005(2) 0.017(3) 0.009(2) C161 0.035(3) 0.032(3) 0.034(3) 0.006(2) 0.013(2) 0.001(2) C162 0.041(3) 0.057(4) 0.034(3) 0.004(3) 0.012(2) -0.011(3) C163 0.058(4) 0.073(5) 0.036(3) 0.003(3) 0.024(3) -0.015(3) C164 0.048(4) 0.073(5) 0.029(3) -0.003(3) 0.007(3) -0.003(3) C165 0.032(3) 0.067(4) 0.039(3) -0.006(3) 0.007(2) -0.007(3) C166 0.029(3) 0.048(3) 0.038(3) 0.002(2) 0.015(2) -0.003(2) C171 0.041(3) 0.028(2) 0.030(2) -0.0044(19) 0.016(2) -0.002(2) C172 0.052(4) 0.036(3) 0.057(4) 0.009(3) 0.032(3) 0.005(3) C173 0.063(4) 0.048(4) 0.078(5) -0.007(3) 0.050(4) -0.007(3) C174 0.081(5) 0.039(3) 0.064(4) -0.005(3) 0.052(4) -0.012(3) C175 0.080(5) 0.034(3) 0.038(3) -0.001(2) 0.026(3) -0.009(3) C176 0.051(3) 0.025(2) 0.033(3) -0.001(2) 0.019(2) -0.003(2) C181 0.031(3) 0.030(3) 0.053(3) 0.001(2) 0.019(2) 0.000(2) C182 0.062(4) 0.037(3) 0.070(4) -0.007(3) 0.034(4) 0.007(3) C183 0.071(5) 0.039(4) 0.109(6) -0.006(4) 0.055(5) 0.003(3) C184 0.038(4) 0.036(3) 0.139(8) -0.002(4) 0.038(5) 0.003(3) C185 0.023(3) 0.047(4) 0.109(6) 0.026(4) 0.011(3) -0.001(3) C186 0.030(3) 0.038(3) 0.075(4) 0.011(3) 0.012(3) -0.003(2) B1 0.031(3) 0.028(3) 0.036(3) 0.000(2) 0.012(2) 0.003(2) _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 P11 C121 1.802(5) . ? P11 C111 1.804(5) . ? P11 C15 1.852(5) . ? P11 P12 2.1354(19) . ? P12 P13 2.1221(19) . ? P13 C131 1.792(6) . ? P13 C141 1.807(6) . ? P13 C14 1.814(5) . ? C14 C15 1.526(7) . ? C111 C112 1.377(7) . ? C111 C116 1.384(7) . ? C112 C113 1.380(8) . ? C113 C114 1.378(9) . ? C114 C115 1.375(8) . ? C115 C116 1.392(8) . ? C121 C122 1.391(7) . ? C121 C126 1.401(7) . ? C122 C123 1.376(8) . ? C123 C124 1.375(9) . ? C124 C125 1.394(9) . ? C125 C126 1.385(7) . ? C131 C132 1.397(8) . ? C131 C136 1.399(8) . ? C132 C133 1.373(9) . ? C133 C134 1.381(10) . ? C134 C135 1.377(10) . ? C135 C136 1.376(8) . ? C141 C142 1.394(8) . ? C141 C146 1.401(7) . ? C142 C143 1.379(8) . ? C143 C144 1.375(9) . ? C144 C145 1.384(9) . ? C145 C146 1.363(8) . ? C151 C156 1.394(7) . ? C151 C152 1.395(7) . ? C151 B1 1.642(8) . ? C152 C153 1.407(8) . ? C153 C154 1.380(9) . ? C154 C155 1.369(9) . ? C155 C156 1.383(8) . ? C161 C166 1.387(7) . ? C161 C162 1.405(7) . ? C161 B1 1.645(8) . ? C162 C163 1.395(8) . ? C163 C164 1.387(9) . ? C164 C165 1.369(8) . ? C165 C166 1.402(7) . ? C171 C176 1.389(7) . ? C171 C172 1.412(8) . ? C171 B1 1.659(8) . ? C172 C173 1.394(8) . ? C173 C174 1.383(9) . ? C174 C175 1.374(9) . ? C175 C176 1.413(8) . ? C181 C186 1.396(8) . ? C181 C182 1.412(8) . ? C181 B1 1.646(7) . ? C182 C183 1.382(8) . ? C183 C184 1.365(11) . ? C184 C185 1.374(11) . ? C185 C186 1.417(9) . ? 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 C121 P11 C111 107.9(2) . . ? C121 P11 C15 106.0(2) . . ? C111 P11 C15 109.4(2) . . ? C121 P11 P12 114.98(19) . . ? C111 P11 P12 109.97(17) . . ? C15 P11 P12 108.43(18) . . ? P13 P12 P11 86.44(7) . . ? C131 P13 C141 107.2(3) . . ? C131 P13 C14 110.4(3) . . ? C141 P13 C14 107.6(2) . . ? C131 P13 P12 110.04(19) . . ? C141 P13 P12 115.95(18) . . ? C14 P13 P12 105.58(18) . . ? C15 C14 P13 108.1(4) . . ? C14 C15 P11 111.2(4) . . ? C112 C111 C116 119.1(5) . . ? C112 C111 P11 122.7(4) . . ? C116 C111 P11 118.2(4) . . ? C111 C112 C113 120.5(6) . . ? C114 C113 C112 120.1(6) . . ? C115 C114 C113 120.2(6) . . ? C114 C115 C116 119.5(6) . . ? C111 C116 C115 120.5(6) . . ? C122 C121 C126 119.1(5) . . ? C122 C121 P11 120.0(4) . . ? C126 C121 P11 120.8(4) . . ? C123 C122 C121 120.8(6) . . ? C124 C123 C122 120.1(6) . . ? C123 C124 C125 120.2(6) . . ? C126 C125 C124 120.0(6) . . ? C125 C126 C121 119.8(5) . . ? C132 C131 C136 118.4(6) . . ? C132 C131 P13 119.6(4) . . ? C136 C131 P13 122.1(5) . . ? C133 C132 C131 121.0(6) . . ? C132 C133 C134 120.0(7) . . ? C135 C134 C133 119.9(7) . . ? C136 C135 C134 120.8(7) . . ? C135 C136 C131 120.1(6) . . ? C142 C141 C146 119.5(5) . . ? C142 C141 P13 119.4(4) . . ? C146 C141 P13 121.1(4) . . ? C143 C142 C141 119.0(6) . . ? C144 C143 C142 121.2(7) . . ? C143 C144 C145 119.6(6) . . ? C146 C145 C144 120.4(6) . . ? C145 C146 C141 120.2(6) . . ? C156 C151 C152 114.1(5) . . ? C156 C151 B1 119.8(5) . . ? C152 C151 B1 126.1(5) . . ? C151 C152 C153 122.4(6) . . ? C154 C153 C152 121.0(6) . . ? C155 C154 C153 117.6(6) . . ? C154 C155 C156 121.0(7) . . ? C155 C156 C151 123.9(6) . . ? C166 C161 C162 116.3(5) . . ? C166 C161 B1 124.5(5) . . ? C162 C161 B1 119.2(5) . . ? C163 C162 C161 122.0(6) . . ? C164 C163 C162 119.7(6) . . ? C165 C164 C163 119.6(6) . . ? C164 C165 C166 120.2(6) . . ? C161 C166 C165 122.0(5) . . ? C176 C171 C172 115.8(5) . . ? C176 C171 B1 125.0(5) . . ? C172 C171 B1 119.2(5) . . ? C173 C172 C171 121.9(6) . . ? C174 C173 C172 121.1(6) . . ? C175 C174 C173 118.2(6) . . ? C174 C175 C176 120.9(6) . . ? C171 C176 C175 122.1(6) . . ? C186 C181 C182 115.5(6) . . ? C186 C181 B1 124.6(5) . . ? C182 C181 B1 119.9(5) . . ? C183 C182 C181 122.9(7) . . ? C184 C183 C182 120.0(8) . . ? C183 C184 C185 120.0(7) . . ? C184 C185 C186 120.0(7) . . ? C181 C186 C185 121.4(7) . . ? C151 B1 C161 107.1(4) . . ? C151 B1 C181 110.3(4) . . ? C161 B1 C181 111.6(4) . . ? C151 B1 C171 111.1(4) . . ? C161 B1 C171 109.7(4) . . ? C181 B1 C171 107.0(4) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.406 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.074