# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1554 #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name ; Dr Robin G. Pritchard ; _publ_contact_author_address ; Department of Chemistry University of Manchester Institute of Science and Technology PO Box 88 Manchester M60 1QD England ; _publ_contact_author_phone '0161 200 4568' _publ_contact_author_fax '0161 236 7677' _publ_contact_author_email 'Robin.Pritchard@UMIST.AC.UK' _publ_requested_journal 'Chem. Soc., Dalton Trans.' _publ_author_name 'Godfrey, McAuliffe, Pritchard, Thompson, Cross' _publ_section_title 'Paper ref. 9/03974K' data_t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H21 I4 P' _chemical_formula_weight 667.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.072(5) _cell_length_b 11.309(7) _cell_length_c 31.994(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.88(3) _cell_angle_gamma 90.00 _cell_volume 5446(4) _cell_formula_units_Z 12 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3624 _exptl_absorpt_coefficient_mu 6.929 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.2303 _exptl_absorpt_correction_T_max 0.3379 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9830 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 24.99 _reflns_number_total 9438 _reflns_number_gt 6335 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1112P)^2^+179.7100P] 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 9438 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1068 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2186 _refine_ls_wR_factor_gt 0.1896 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.66882(8) 0.90718(11) 0.34079(4) 0.0498(3) Uani 1 d . . . I2 I 0.29015(8) 0.08462(11) 0.34040(4) 0.0528(3) Uani 1 d . . . I3 I 0.69260(7) 0.40990(10) 0.50191(4) 0.0501(3) Uani 1 d . . . I4 I 0.66228(9) 0.58226(12) 0.34637(4) 0.0572(3) Uani 1 d . . . I5 I 0.48045(9) 0.49681(10) 0.34540(4) 0.0523(3) Uani 1 d . . . I6 I 0.29744(9) 0.41010(12) 0.33919(4) 0.0573(3) Uani 1 d . . . I7 I 0.68402(8) 0.08152(11) 0.50035(4) 0.0543(3) Uani 1 d . . . I8 I 0.5000 0.0000 0.5000 0.0496(4) Uani 1 d S . . I9 I 1.05787(9) 1.26167(12) 0.31920(5) 0.0639(4) Uani 1 d . . . I10 I 0.97837(7) 1.49301(11) 0.31983(4) 0.0483(3) Uani 1 d . . . I11 I 0.89790(8) 1.72536(12) 0.32280(4) 0.0564(3) Uani 1 d . . . I12 I 1.0000 1.0000 0.5000 0.0385(3) Uani 1 d S . . I13 I 1.07661(8) 0.76693(11) 0.49928(4) 0.0492(3) Uani 1 d . . . P1 P 0.7081(3) 1.1109(4) 0.33675(13) 0.0406(10) Uani 1 d . . . P2 P 0.2529(3) -0.1209(4) 0.33640(13) 0.0401(9) Uani 1 d . . . P3 P 0.7330(3) 0.6140(4) 0.50171(13) 0.0357(9) Uani 1 d . . . C1 C 0.7816(12) 1.1400(16) 0.3832(5) 0.050(4) Uani 1 d . . . H1 H 0.7482 1.1184 0.4079 0.060 Uiso 1 calc R . . C2 C 0.8009(17) 1.2746(17) 0.3863(7) 0.074(7) Uani 1 d . . . H2A H 0.7452 1.3179 0.3849 0.111 Uiso 1 calc R . . H2B H 0.8363 1.2986 0.3633 0.111 Uiso 1 calc R . . H2C H 0.8331 1.2915 0.4126 0.111 Uiso 1 calc R . . C3 C 0.8653(12) 1.0680(19) 0.3851(6) 0.057(5) Uani 1 d . . . H3A H 0.8504 0.9847 0.3831 0.085 Uiso 1 calc R . . H3B H 0.8981 1.0828 0.4115 0.085 Uiso 1 calc R . . H3C H 0.9015 1.0899 0.3621 0.085 Uiso 1 calc R . . C4 C 0.7542(12) 1.1319(15) 0.2858(5) 0.045(4) Uani 1 d . . . H4 H 0.7077 1.1071 0.2646 0.054 Uiso 1 calc R . . C5 C 0.7730(14) 1.2633(15) 0.2777(7) 0.059(5) Uani 1 d . . . H5A H 0.7200 1.3093 0.2821 0.089 Uiso 1 calc R . . H5B H 0.7902 1.2735 0.2491 0.089 Uiso 1 calc R . . H5C H 0.8208 1.2901 0.2969 0.089 Uiso 1 calc R . . C6 C 0.8348(13) 1.0545(19) 0.2795(6) 0.059(5) Uani 1 d . . . H6A H 0.8200 0.9726 0.2849 0.088 Uiso 1 calc R . . H6B H 0.8833 1.0790 0.2986 0.088 Uiso 1 calc R . . H6C H 0.8526 1.0625 0.2509 0.088 Uiso 1 calc R . . C7 C 0.6089(11) 1.1987(13) 0.3388(5) 0.041(4) Uani 1 d . . . H7 H 0.6269 1.2828 0.3375 0.049 Uiso 1 calc R . . C8 C 0.5425(12) 1.1761(19) 0.3021(6) 0.060(5) Uani 1 d . . . H8A H 0.5713 1.1886 0.2760 0.090 Uiso 1 calc R . . H8B H 0.4928 1.2301 0.3037 0.090 Uiso 1 calc R . . H8C H 0.5213 1.0953 0.3033 0.090 Uiso 1 calc R . . C9 C 0.5654(15) 1.180(2) 0.3806(7) 0.080(7) Uani 1 d . . . H9A H 0.6086 1.1945 0.4035 0.121 Uiso 1 calc R . . H9B H 0.5442 1.0989 0.3822 0.121 Uiso 1 calc R . . H9C H 0.5158 1.2338 0.3825 0.121 Uiso 1 calc R . . C10 C 0.1974(11) -0.1494(17) 0.2852(5) 0.048(4) Uani 1 d . . . H10 H 0.2394 -0.1222 0.2644 0.057 Uiso 1 calc R . . C11 C 0.1131(13) -0.076(2) 0.2768(6) 0.073(7) Uani 1 d . . . H11A H 0.1256 0.0061 0.2828 0.109 Uiso 1 calc R . . H11B H 0.0672 -0.1043 0.2945 0.109 Uiso 1 calc R . . H11C H 0.0930 -0.0848 0.2477 0.109 Uiso 1 calc R . . C12 C 0.1837(18) -0.277(2) 0.2767(7) 0.086(8) Uani 1 d . . . H12A H 0.2390 -0.3196 0.2824 0.129 Uiso 1 calc R . . H12B H 0.1644 -0.2884 0.2475 0.129 Uiso 1 calc R . . H12C H 0.1387 -0.3079 0.2944 0.129 Uiso 1 calc R . . C13 C 0.1881(12) -0.1517(16) 0.3811(5) 0.048(4) Uani 1 d . . . H13 H 0.2268 -0.1334 0.4062 0.058 Uiso 1 calc R . . C14 C 0.1656(17) -0.2895(19) 0.3835(8) 0.081(7) Uani 1 d . . . H14A H 0.2199 -0.3350 0.3820 0.121 Uiso 1 calc R . . H14B H 0.1249 -0.3108 0.3603 0.121 Uiso 1 calc R . . H14C H 0.1383 -0.3064 0.4097 0.121 Uiso 1 calc R . . C15 C 0.1067(12) -0.0717(19) 0.3832(6) 0.058(5) Uani 1 d . . . H15A H 0.1250 0.0103 0.3816 0.088 Uiso 1 calc R . . H15B H 0.0786 -0.0852 0.4094 0.088 Uiso 1 calc R . . H15C H 0.0650 -0.0897 0.3600 0.088 Uiso 1 calc R . . C16 C 0.3556(12) -0.2072(18) 0.3401(6) 0.052(4) Uani 1 d . . . H16 H 0.3395 -0.2920 0.3383 0.062 Uiso 1 calc R . . C17 C 0.4058(13) -0.1870(19) 0.3818(7) 0.064(5) Uani 1 d . . . H17A H 0.3676 -0.2059 0.4044 0.096 Uiso 1 calc R . . H17B H 0.4238 -0.1048 0.3840 0.096 Uiso 1 calc R . . H17C H 0.4580 -0.2372 0.3837 0.096 Uiso 1 calc R . . C18 C 0.4125(14) -0.179(2) 0.3041(7) 0.074(6) Uani 1 d . . . H18A H 0.3788 -0.1928 0.2779 0.110 Uiso 1 calc R . . H18B H 0.4647 -0.2292 0.3054 0.110 Uiso 1 calc R . . H18C H 0.4307 -0.0967 0.3056 0.110 Uiso 1 calc R . . C19 C 0.7865(10) 0.6421(15) 0.4528(5) 0.039(4) Uani 1 d . . . H19 H 0.7427 0.6209 0.4299 0.047 Uiso 1 calc R . . C20 C 0.8696(11) 0.5632(16) 0.4472(5) 0.047(4) Uani 1 d . . . H20A H 0.8540 0.4809 0.4510 0.071 Uiso 1 calc R . . H20B H 0.9162 0.5853 0.4677 0.071 Uiso 1 calc R . . H20C H 0.8905 0.5743 0.4193 0.071 Uiso 1 calc R . . C21 C 0.8089(14) 0.7707(16) 0.4470(6) 0.056(5) Uani 1 d . . . H21A H 0.7563 0.8184 0.4506 0.085 Uiso 1 calc R . . H21B H 0.8295 0.7827 0.4191 0.085 Uiso 1 calc R . . H21C H 0.8552 0.7937 0.4675 0.085 Uiso 1 calc R . . C22 C 0.7999(11) 0.6427(16) 0.5498(5) 0.044(4) Uani 1 d . . . H22 H 0.7618 0.6200 0.5728 0.053 Uiso 1 calc R . . C23 C 0.8842(12) 0.5638(18) 0.5555(5) 0.052(5) Uani 1 d . . . H23A H 0.8680 0.4817 0.5508 0.078 Uiso 1 calc R . . H23B H 0.9098 0.5729 0.5838 0.078 Uiso 1 calc R . . H23C H 0.9273 0.5876 0.5356 0.078 Uiso 1 calc R . . C24 C 0.8202(15) 0.7702(17) 0.5567(6) 0.062(5) Uani 1 d . . . H24A H 0.7660 0.8160 0.5529 0.092 Uiso 1 calc R . . H24B H 0.8626 0.7961 0.5368 0.092 Uiso 1 calc R . . H24C H 0.8454 0.7815 0.5849 0.092 Uiso 1 calc R . . C25 C 0.6340(12) 0.7012(16) 0.5019(5) 0.046(4) Uani 1 d . . . H25 H 0.6515 0.7856 0.5015 0.055 Uiso 1 calc R . . C26 C 0.5824(13) 0.680(2) 0.5404(6) 0.064(5) Uani 1 d . . . H26A H 0.6204 0.6952 0.5652 0.096 Uiso 1 calc R . . H26B H 0.5619 0.5991 0.5407 0.096 Uiso 1 calc R . . H26C H 0.5318 0.7333 0.5401 0.096 Uiso 1 calc R . . C27 C 0.5738(11) 0.6776(16) 0.4637(6) 0.052(5) Uani 1 d . . . H27A H 0.6062 0.6907 0.4387 0.079 Uiso 1 calc R . . H27B H 0.5231 0.7305 0.4636 0.079 Uiso 1 calc R . . H27C H 0.5532 0.5963 0.4642 0.079 Uiso 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 I1 0.0462(6) 0.0471(6) 0.0566(7) 0.0027(5) 0.0075(5) 0.0010(5) I2 0.0510(7) 0.0492(7) 0.0587(8) 0.0002(6) 0.0071(5) -0.0015(5) I3 0.0396(6) 0.0440(6) 0.0668(8) 0.0015(6) 0.0038(5) -0.0020(5) I4 0.0632(8) 0.0631(8) 0.0438(7) -0.0023(6) -0.0108(6) -0.0042(6) I5 0.0729(8) 0.0434(6) 0.0403(6) -0.0016(5) 0.0000(5) 0.0031(6) I6 0.0654(8) 0.0590(8) 0.0486(7) 0.0005(6) 0.0146(6) -0.0069(6) I7 0.0542(7) 0.0568(7) 0.0519(7) 0.0011(6) 0.0040(5) -0.0059(6) I8 0.0597(10) 0.0420(9) 0.0471(9) -0.0010(7) 0.0030(7) 0.0022(7) I9 0.0568(8) 0.0608(8) 0.0737(9) 0.0037(7) -0.0005(6) 0.0081(6) I10 0.0387(6) 0.0600(7) 0.0457(6) 0.0030(5) -0.0016(5) -0.0036(5) I11 0.0468(7) 0.0652(8) 0.0573(7) 0.0005(6) 0.0039(5) 0.0085(6) I12 0.0329(7) 0.0477(8) 0.0348(7) 0.0000(7) 0.0005(5) -0.0001(6) I13 0.0462(6) 0.0510(7) 0.0500(7) 0.0000(5) -0.0006(5) 0.0087(5) P1 0.038(2) 0.052(3) 0.031(2) -0.0024(19) -0.0013(17) 0.0065(19) P2 0.045(2) 0.042(2) 0.033(2) -0.0003(18) 0.0008(18) 0.0046(18) P3 0.038(2) 0.037(2) 0.032(2) -0.0041(17) 0.0007(16) 0.0009(17) C1 0.065(11) 0.048(10) 0.037(9) -0.003(8) -0.006(8) -0.006(9) C2 0.119(19) 0.043(11) 0.058(13) 0.009(10) -0.026(12) -0.024(12) C3 0.054(11) 0.078(14) 0.036(10) -0.004(9) -0.017(8) 0.004(10) C4 0.057(10) 0.049(10) 0.028(8) 0.007(7) -0.005(7) -0.013(8) C5 0.074(13) 0.038(10) 0.065(13) 0.020(9) 0.005(10) -0.016(9) C6 0.061(12) 0.075(13) 0.042(10) 0.001(10) 0.021(9) 0.006(10) C7 0.061(10) 0.021(7) 0.039(9) -0.003(7) -0.001(8) 0.005(7) C8 0.044(10) 0.065(13) 0.069(13) 0.002(11) -0.011(9) 0.002(9) C9 0.068(14) 0.12(2) 0.058(13) 0.022(14) 0.035(11) 0.024(14) C10 0.049(10) 0.063(11) 0.031(9) -0.003(8) -0.002(7) -0.007(9) C11 0.057(12) 0.12(2) 0.041(11) 0.009(12) -0.015(9) 0.028(12) C12 0.105(19) 0.096(18) 0.054(13) -0.014(13) -0.017(13) -0.037(15) C13 0.058(11) 0.051(10) 0.036(9) -0.007(8) 0.011(8) 0.014(8) C14 0.111(19) 0.056(13) 0.079(16) 0.038(12) 0.040(14) 0.012(12) C15 0.058(11) 0.074(14) 0.044(11) 0.008(10) 0.018(9) 0.016(10) C16 0.055(11) 0.056(11) 0.043(10) 0.000(9) -0.009(8) 0.015(9) C17 0.058(12) 0.060(12) 0.072(14) -0.014(11) -0.008(10) 0.017(10) C18 0.058(13) 0.080(16) 0.083(16) 0.004(13) 0.012(11) -0.003(11) C19 0.036(8) 0.051(10) 0.028(8) -0.007(7) 0.000(6) 0.008(7) C20 0.043(9) 0.060(11) 0.039(9) -0.012(8) 0.008(7) 0.008(8) C21 0.081(14) 0.051(11) 0.039(9) 0.008(8) 0.014(9) 0.033(10) C22 0.048(9) 0.054(10) 0.029(8) 0.003(8) 0.004(7) 0.003(8) C23 0.057(11) 0.070(12) 0.027(8) -0.015(8) -0.007(7) 0.009(9) C24 0.080(14) 0.058(12) 0.045(11) -0.007(9) -0.012(10) -0.010(10) C25 0.056(10) 0.052(10) 0.031(8) 0.002(8) 0.006(7) 0.014(8) C26 0.061(12) 0.071(14) 0.062(13) 0.005(11) 0.024(10) 0.018(10) C27 0.039(9) 0.041(10) 0.076(13) 0.000(9) -0.008(9) 0.008(7) _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 I1 P1 2.383(5) . ? I2 P2 2.393(5) . ? I3 P3 2.387(4) . ? I4 I5 2.905(2) . ? I5 I6 2.925(2) . ? I7 I8 2.9222(15) . ? I8 I7 2.9222(15) 3_656 ? I9 I10 2.878(2) . ? I10 I11 2.898(2) . ? I12 I13 2.8782(19) 3_776 ? I12 I13 2.8782(19) . ? P1 C7 1.798(16) . ? P1 C4 1.819(16) . ? P1 C1 1.837(17) . ? P2 C13 1.806(17) . ? P2 C16 1.829(18) . ? P2 C10 1.830(16) . ? P3 C25 1.789(17) . ? P3 C19 1.823(16) . ? P3 C22 1.826(16) . ? C1 C3 1.50(3) . ? C1 C2 1.55(2) . ? C4 C6 1.52(3) . ? C4 C5 1.54(2) . ? C7 C8 1.53(2) . ? C7 C9 1.53(2) . ? C10 C12 1.49(3) . ? C10 C11 1.53(3) . ? C13 C15 1.53(2) . ? C13 C14 1.60(3) . ? C16 C18 1.51(3) . ? C16 C17 1.52(3) . ? C19 C21 1.51(2) . ? C19 C20 1.56(2) . ? C22 C24 1.49(2) . ? C22 C23 1.56(2) . ? C25 C26 1.51(2) . ? C25 C27 1.51(2) . ? 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 I4 I5 I6 176.72(6) . . ? I7 I8 I7 180.0 . 3_656 ? I9 I10 I11 178.50(6) . . ? I13 I12 I13 180.0 3_776 . ? C7 P1 C4 108.4(8) . . ? C7 P1 C1 109.9(8) . . ? C4 P1 C1 117.3(8) . . ? C7 P1 I1 108.8(6) . . ? C4 P1 I1 106.4(6) . . ? C1 P1 I1 105.7(6) . . ? C13 P2 C16 109.6(8) . . ? C13 P2 C10 115.7(9) . . ? C16 P2 C10 108.2(8) . . ? C13 P2 I2 106.2(6) . . ? C16 P2 I2 108.6(7) . . ? C10 P2 I2 108.3(6) . . ? C25 P3 C19 108.2(7) . . ? C25 P3 C22 108.9(8) . . ? C19 P3 C22 116.3(8) . . ? C25 P3 I3 108.7(7) . . ? C19 P3 I3 107.1(6) . . ? C22 P3 I3 107.4(6) . . ? C3 C1 C2 112.1(17) . . ? C3 C1 P1 114.1(12) . . ? C2 C1 P1 109.4(13) . . ? C6 C4 C5 112.2(16) . . ? C6 C4 P1 112.8(12) . . ? C5 C4 P1 111.0(13) . . ? C8 C7 C9 110.8(17) . . ? C8 C7 P1 113.2(12) . . ? C9 C7 P1 110.3(13) . . ? C12 C10 C11 112.7(18) . . ? C12 C10 P2 112.9(14) . . ? C11 C10 P2 113.6(13) . . ? C15 C13 C14 113.7(17) . . ? C15 C13 P2 112.9(13) . . ? C14 C13 P2 110.5(12) . . ? C18 C16 C17 111.3(18) . . ? C18 C16 P2 110.4(14) . . ? C17 C16 P2 111.1(13) . . ? C21 C19 C20 110.6(14) . . ? C21 C19 P3 112.7(11) . . ? C20 C19 P3 113.1(11) . . ? C24 C22 C23 112.2(16) . . ? C24 C22 P3 113.4(12) . . ? C23 C22 P3 114.2(11) . . ? C26 C25 C27 108.7(17) . . ? C26 C25 P3 112.4(13) . . ? C27 C25 P3 111.5(12) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.873 _refine_diff_density_min -1.924 _refine_diff_density_rms 0.350 #===END data_gt4b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H84 I8 N6 P2' _chemical_formula_weight 1678.23 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' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 16.913(3) _cell_length_b 9.7437(15) _cell_length_c 35.602(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.02(2) _cell_angle_gamma 90.00 _cell_volume 5852.6(19) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 4.322 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10630 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1238 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 24.98 _reflns_number_total 10630 _reflns_number_gt 4857 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+1.0355P] 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 10630 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1768 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1631 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 1.113 _refine_ls_shift/su_mean 0.037 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.65867(7) 0.05714(12) 0.14177(3) 0.0562(3) Uani 1 1 d . . . I2 I 0.61965(9) -0.14445(13) 0.02447(3) 0.0809(4) Uani 1 1 d . . . I3 I 0.73173(8) -0.35080(11) 0.00298(3) 0.0611(3) Uani 1 1 d . . . I4 I 0.84851(8) -0.55533(13) -0.01454(3) 0.0714(4) Uani 1 1 d . . . I5 I 0.15530(7) 0.76995(12) 0.14269(3) 0.0573(3) Uani 1 1 d . . . I6 I -0.00655(9) 0.52105(13) 0.17914(4) 0.0833(4) Uani 1 1 d . . . I7 I -0.00942(8) 0.68303(12) 0.24719(3) 0.0659(4) Uani 1 1 d . . . I8 I -0.00898(12) 0.84806(19) 0.31430(4) 0.1184(7) Uani 1 1 d . . . P1 P 0.7994(2) 0.0578(4) 0.13114(10) 0.0376(9) Uani 1 1 d . . . P2 P 0.2953(2) 0.8017(4) 0.13102(10) 0.0368(9) Uani 1 1 d . . . N1 N 0.8221(7) -0.0939(11) 0.1192(3) 0.044(3) Uani 1 1 d . . . N2 N 0.8115(7) 0.1694(12) 0.0986(3) 0.043(3) Uani 1 1 d . . . N3 N 0.8463(7) 0.1042(12) 0.1697(3) 0.044(3) Uani 1 1 d . . . N4 N 0.3395(7) 0.8478(12) 0.1706(3) 0.046(3) Uani 1 1 d . . . N5 N 0.3002(7) 0.9175(11) 0.0994(3) 0.043(3) Uani 1 1 d . . . N6 N 0.3254(7) 0.6538(13) 0.1185(3) 0.047(3) Uani 1 1 d . . . C1 C 0.8592(8) -0.1267(14) 0.0846(4) 0.036(3) Uani 1 1 d . . . H1A H 0.8671 -0.0417 0.0706 0.043 Uiso 1 1 calc R . . H1B H 0.8235 -0.1856 0.0689 0.043 Uiso 1 1 calc R . . C2 C 0.9379(10) -0.1984(17) 0.0916(4) 0.059(5) Uani 1 1 d . . . H2A H 0.9302 -0.2835 0.1056 0.071 Uiso 1 1 calc R . . H2B H 0.9739 -0.1395 0.1072 0.071 Uiso 1 1 calc R . . C3 C 0.9751(10) -0.232(2) 0.0554(4) 0.072(5) Uani 1 1 d . . . H3A H 0.9411 -0.2946 0.0406 0.108 Uiso 1 1 calc R . . H3B H 1.0265 -0.2738 0.0611 0.108 Uiso 1 1 calc R . . H3C H 0.9815 -0.1479 0.0412 0.108 Uiso 1 1 calc R . . C4 C 0.8019(10) -0.2120(14) 0.1429(4) 0.050(4) Uani 1 1 d . . . H4A H 0.7778 -0.1772 0.1653 0.060 Uiso 1 1 calc R . . H4B H 0.8510 -0.2594 0.1515 0.060 Uiso 1 1 calc R . . C5 C 0.7466(11) -0.3137(15) 0.1236(4) 0.060(5) Uani 1 1 d . . . H5A H 0.6987 -0.2661 0.1134 0.072 Uiso 1 1 calc R . . H5B H 0.7721 -0.3550 0.1024 0.072 Uiso 1 1 calc R . . C6 C 0.7238(14) -0.4242(18) 0.1496(6) 0.103(8) Uani 1 1 d . . . H6A H 0.7711 -0.4686 0.1607 0.154 Uiso 1 1 calc R . . H6B H 0.6910 -0.4913 0.1357 0.154 Uiso 1 1 calc R . . H6C H 0.6943 -0.3847 0.1694 0.154 Uiso 1 1 calc R . . C7 C 0.7558(9) 0.1679(14) 0.0636(4) 0.041(4) Uani 1 1 d . . . H7A H 0.7869 0.1675 0.0414 0.050 Uiso 1 1 calc R . . H7B H 0.7244 0.0832 0.0632 0.050 Uiso 1 1 calc R . . C8 C 0.7008(9) 0.2882(15) 0.0613(4) 0.047(4) Uani 1 1 d . . . H8A H 0.7316 0.3735 0.0627 0.057 Uiso 1 1 calc R . . H8B H 0.6671 0.2864 0.0826 0.057 Uiso 1 1 calc R . . C9 C 0.6480(9) 0.2837(15) 0.0234(4) 0.052(4) Uani 1 1 d . . . H9A H 0.6810 0.2971 0.0025 0.078 Uiso 1 1 calc R . . H9B H 0.6085 0.3559 0.0234 0.078 Uiso 1 1 calc R . . H9C H 0.6218 0.1954 0.0210 0.078 Uiso 1 1 calc R . . C10 C 0.8767(10) 0.2670(15) 0.0994(4) 0.054(4) Uani 1 1 d . . . H10A H 0.8962 0.2822 0.1257 0.065 Uiso 1 1 calc R . . H10B H 0.8567 0.3548 0.0893 0.065 Uiso 1 1 calc R . . C11 C 0.9458(10) 0.2215(17) 0.0772(4) 0.057(4) Uani 1 1 d . . . H11A H 0.9684 0.1366 0.0881 0.068 Uiso 1 1 calc R . . H11B H 0.9266 0.2025 0.0511 0.068 Uiso 1 1 calc R . . C12 C 1.0084(10) 0.329(2) 0.0777(5) 0.082(6) Uani 1 1 d . . . H12A H 0.9845 0.4167 0.0706 0.123 Uiso 1 1 calc R . . H12B H 1.0472 0.3049 0.0600 0.123 Uiso 1 1 calc R . . H12C H 1.0343 0.3358 0.1028 0.123 Uiso 1 1 calc R . . C13 C 0.8169(10) 0.2257(15) 0.1897(4) 0.053(4) Uani 1 1 d . . . H13A H 0.7783 0.2737 0.1726 0.064 Uiso 1 1 calc R . . H13B H 0.8616 0.2883 0.1952 0.064 Uiso 1 1 calc R . . C14 C 0.7792(10) 0.1980(16) 0.2254(4) 0.056(4) Uani 1 1 d . . . H14A H 0.8182 0.1569 0.2437 0.067 Uiso 1 1 calc R . . H14B H 0.7357 0.1323 0.2206 0.067 Uiso 1 1 calc R . . C15 C 0.7477(12) 0.3277(18) 0.2413(4) 0.076(6) Uani 1 1 d . . . H15A H 0.7911 0.3911 0.2470 0.114 Uiso 1 1 calc R . . H15B H 0.7219 0.3069 0.2641 0.114 Uiso 1 1 calc R . . H15C H 0.7097 0.3690 0.2230 0.114 Uiso 1 1 calc R . . C16 C 0.9098(9) 0.0227(17) 0.1894(4) 0.054(4) Uani 1 1 d . . . H16A H 0.9097 -0.0712 0.1796 0.065 Uiso 1 1 calc R . . H16B H 0.9027 0.0192 0.2165 0.065 Uiso 1 1 calc R . . C17 C 1.002(2) 0.108(3) 0.1807(10) 0.21(3) Uani 1 1 d . . . H17A H 1.0220 0.0814 0.1567 0.253 Uiso 1 1 calc R . . H17B H 0.9974 0.2086 0.1821 0.253 Uiso 1 1 calc R . . C18 C 1.037(3) 0.062(3) 0.2063(8) 0.207(19) Uani 1 1 d . . . H18A H 1.0100 -0.0186 0.2150 0.310 Uiso 1 1 calc R . . H18B H 1.0427 0.1290 0.2264 0.310 Uiso 1 1 calc R . . H18C H 1.0896 0.0354 0.1992 0.310 Uiso 1 1 calc R . . C19 C 0.3102(10) 0.9686(15) 0.1904(4) 0.056(5) Uani 1 1 d . . . H19A H 0.2678 1.0125 0.1745 0.067 Uiso 1 1 calc R . . H19B H 0.3534 1.0351 0.1946 0.067 Uiso 1 1 calc R . . C20 C 0.2785(13) 0.9308(19) 0.2283(4) 0.085(7) Uani 1 1 d . . . H20A H 0.2319 0.8715 0.2242 0.102 Uiso 1 1 calc R . . H20B H 0.3191 0.8803 0.2437 0.102 Uiso 1 1 calc R . . C21 C 0.2563(16) 1.060(2) 0.2487(5) 0.109(8) Uani 1 1 d . . . H21A H 0.2975 1.1283 0.2468 0.163 Uiso 1 1 calc R . . H21B H 0.2505 1.0390 0.2750 0.163 Uiso 1 1 calc R . . H21C H 0.2066 1.0953 0.2374 0.163 Uiso 1 1 calc R . . C22 C 0.4106(9) 0.7790(18) 0.1876(4) 0.058(5) Uani 1 1 d . . . H22A H 0.4051 0.7702 0.2147 0.069 Uiso 1 1 calc R . . H22B H 0.4125 0.6861 0.1772 0.069 Uiso 1 1 calc R . . C23 C 0.4858(11) 0.8468(18) 0.1821(5) 0.066(5) Uani 1 1 d . . . H23A H 0.4810 0.9444 0.1881 0.080 Uiso 1 1 calc R . . H23B H 0.4969 0.8396 0.1555 0.080 Uiso 1 1 calc R . . C24 C 0.5541(11) 0.787(2) 0.2059(6) 0.093(7) Uani 1 1 d . . . H24A H 0.5387 0.7731 0.2314 0.140 Uiso 1 1 calc R . . H24B H 0.5988 0.8495 0.2064 0.140 Uiso 1 1 calc R . . H24C H 0.5691 0.6997 0.1954 0.140 Uiso 1 1 calc R . . C25 C 0.3560(10) 1.0317(15) 0.1020(5) 0.055(5) Uani 1 1 d . . . H25A H 0.3729 1.0463 0.1286 0.066 Uiso 1 1 calc R . . H25B H 0.3282 1.1148 0.0929 0.066 Uiso 1 1 calc R . . C26 C 0.4287(10) 1.0144(18) 0.0805(4) 0.060(5) Uani 1 1 d . . . H26A H 0.4128 0.9838 0.0549 0.072 Uiso 1 1 calc R . . H26B H 0.4625 0.9432 0.0926 0.072 Uiso 1 1 calc R . . C27 C 0.4755(10) 1.146(2) 0.0786(5) 0.079(6) Uani 1 1 d . . . H27A H 0.4424 1.2163 0.0665 0.119 Uiso 1 1 calc R . . H27B H 0.5214 1.1301 0.0643 0.119 Uiso 1 1 calc R . . H27C H 0.4928 1.1748 0.1039 0.119 Uiso 1 1 calc R . . C28 C 0.2472(8) 0.9114(14) 0.0643(4) 0.040(4) Uani 1 1 d . . . H28A H 0.2796 0.9200 0.0426 0.048 Uiso 1 1 calc R . . H28B H 0.2216 0.8212 0.0627 0.048 Uiso 1 1 calc R . . C29 C 0.1854(10) 1.0178(17) 0.0614(4) 0.054(4) Uani 1 1 d . . . H29A H 0.2105 1.1080 0.0649 0.065 Uiso 1 1 calc R . . H29B H 0.1500 1.0046 0.0817 0.065 Uiso 1 1 calc R . . C30 C 0.1364(9) 1.0163(17) 0.0237(4) 0.057(5) Uani 1 1 d . . . H30A H 0.1709 1.0318 0.0034 0.086 Uiso 1 1 calc R . . H30B H 0.0967 1.0882 0.0234 0.086 Uiso 1 1 calc R . . H30C H 0.1105 0.9279 0.0202 0.086 Uiso 1 1 calc R . . C31 C 0.3056(11) 0.5339(15) 0.1398(4) 0.058(5) Uani 1 1 d . . . H31A H 0.2796 0.5643 0.1621 0.069 Uiso 1 1 calc R . . H31B H 0.3549 0.4878 0.1486 0.069 Uiso 1 1 calc R . . C32 C 0.2527(11) 0.4307(15) 0.1191(4) 0.062(5) Uani 1 1 d . . . H32A H 0.2806 0.3893 0.0987 0.074 Uiso 1 1 calc R . . H32B H 0.2050 0.4764 0.1080 0.074 Uiso 1 1 calc R . . C33 C 0.2295(12) 0.3194(16) 0.1464(5) 0.074(6) Uani 1 1 d . . . H33A H 0.2767 0.2852 0.1604 0.111 Uiso 1 1 calc R . . H33B H 0.2036 0.2447 0.1324 0.111 Uiso 1 1 calc R . . H33C H 0.1936 0.3576 0.1638 0.111 Uiso 1 1 calc R . . C34 C 0.3655(10) 0.6304(15) 0.0830(4) 0.049(4) Uani 1 1 d . . . H34A H 0.3691 0.7173 0.0693 0.059 Uiso 1 1 calc R . . H34B H 0.3341 0.5662 0.0668 0.059 Uiso 1 1 calc R . . C35 C 0.4490(12) 0.572(2) 0.0919(5) 0.089(7) Uani 1 1 d . . . H35A H 0.4816 0.6387 0.1065 0.107 Uiso 1 1 calc R . . H35B H 0.4458 0.4882 0.1070 0.107 Uiso 1 1 calc R . . C36 C 0.4863(14) 0.540(2) 0.0561(7) 0.118(9) Uani 1 1 d . . . H36A H 0.4551 0.4707 0.0422 0.177 Uiso 1 1 calc R . . H36B H 0.5396 0.5053 0.0619 0.177 Uiso 1 1 calc R . . H36C H 0.4885 0.6224 0.0411 0.177 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 I1 0.0409(7) 0.0699(7) 0.0586(6) 0.0091(6) 0.0090(5) -0.0029(6) I2 0.1093(12) 0.0571(7) 0.0744(8) -0.0067(6) -0.0082(8) -0.0018(8) I3 0.0872(10) 0.0512(6) 0.0444(6) 0.0011(5) 0.0016(6) -0.0227(7) I4 0.0728(9) 0.0766(8) 0.0663(7) 0.0001(6) 0.0159(7) -0.0124(8) I5 0.0389(6) 0.0745(8) 0.0592(6) 0.0069(6) 0.0088(5) 0.0006(6) I6 0.0851(11) 0.0691(8) 0.0981(10) -0.0100(7) 0.0234(8) -0.0230(8) I7 0.0600(8) 0.0584(7) 0.0767(8) 0.0124(6) -0.0137(6) -0.0078(6) I8 0.1381(16) 0.1337(14) 0.0824(10) -0.0238(10) 0.0008(10) -0.0659(13) P1 0.040(2) 0.037(2) 0.036(2) 0.0009(17) 0.0063(18) -0.002(2) P2 0.035(2) 0.039(2) 0.037(2) -0.0028(17) 0.0043(18) 0.0038(19) N1 0.054(9) 0.037(7) 0.041(7) 0.003(6) 0.011(6) -0.005(7) N2 0.049(8) 0.046(7) 0.036(6) 0.003(6) 0.008(6) -0.008(7) N3 0.038(8) 0.042(7) 0.051(7) 0.000(6) 0.000(6) -0.003(6) N4 0.045(8) 0.040(7) 0.051(7) -0.003(6) -0.001(6) 0.005(7) N5 0.054(9) 0.035(7) 0.040(7) -0.001(5) 0.007(6) -0.003(7) N6 0.048(8) 0.053(8) 0.039(7) 0.007(6) 0.007(6) 0.005(7) C1 0.021(8) 0.040(8) 0.045(8) 0.006(7) -0.001(7) -0.010(7) C2 0.064(13) 0.048(10) 0.066(11) 0.001(8) 0.005(9) 0.008(10) C3 0.046(11) 0.111(15) 0.059(10) -0.005(11) 0.001(9) 0.025(12) C4 0.067(12) 0.037(9) 0.044(9) 0.003(7) -0.009(8) 0.003(9) C5 0.077(13) 0.043(9) 0.062(10) 0.014(8) 0.022(9) -0.025(10) C6 0.14(2) 0.055(12) 0.119(17) -0.014(11) 0.039(15) -0.066(14) C7 0.047(10) 0.040(9) 0.038(8) 0.001(7) 0.009(7) 0.000(8) C8 0.043(10) 0.050(9) 0.051(9) 0.009(7) 0.017(8) 0.019(8) C9 0.051(11) 0.036(9) 0.070(11) 0.027(8) 0.005(9) 0.015(8) C10 0.067(12) 0.040(9) 0.058(10) 0.003(8) 0.007(9) -0.017(9) C11 0.052(11) 0.066(11) 0.053(9) 0.003(9) 0.011(8) -0.012(10) C12 0.047(12) 0.087(14) 0.114(15) 0.004(12) 0.021(11) -0.034(11) C13 0.061(12) 0.040(9) 0.058(10) -0.005(8) 0.008(9) 0.007(9) C14 0.060(12) 0.051(10) 0.057(10) 0.000(8) 0.003(9) 0.017(9) C15 0.093(15) 0.086(14) 0.047(10) -0.018(10) -0.002(10) 0.018(13) C16 0.048(11) 0.058(11) 0.055(9) 0.003(8) 0.000(8) 0.012(10) C17 0.31(5) 0.060(16) 0.23(4) -0.01(2) -0.22(4) 0.04(2) C18 0.43(6) 0.10(2) 0.10(2) -0.04(2) 0.05(3) -0.08(3) C19 0.067(12) 0.052(10) 0.045(9) -0.015(8) -0.013(8) 0.020(10) C20 0.126(19) 0.083(14) 0.044(10) -0.028(10) -0.006(11) 0.021(14) C21 0.16(2) 0.103(16) 0.060(11) -0.025(12) 0.009(13) 0.044(18) C22 0.042(11) 0.076(12) 0.054(10) 0.011(9) -0.010(8) 0.012(10) C23 0.064(13) 0.064(12) 0.068(11) -0.002(10) -0.022(10) 0.019(11) C24 0.042(12) 0.127(19) 0.110(16) 0.027(14) -0.004(11) -0.003(13) C25 0.059(12) 0.030(8) 0.076(11) 0.018(8) -0.004(9) -0.016(9) C26 0.045(11) 0.088(13) 0.050(9) 0.016(9) 0.016(8) -0.007(10) C27 0.043(11) 0.105(15) 0.088(13) 0.029(12) -0.008(10) -0.043(12) C28 0.036(9) 0.044(9) 0.040(8) 0.004(7) 0.006(7) 0.013(8) C29 0.058(12) 0.061(11) 0.044(9) 0.002(8) 0.008(8) 0.001(10) C30 0.044(11) 0.071(11) 0.055(10) 0.006(9) -0.008(8) -0.017(9) C31 0.077(13) 0.047(10) 0.050(9) 0.000(8) 0.012(9) 0.019(10) C32 0.090(14) 0.044(10) 0.050(9) 0.000(8) -0.003(9) -0.008(10) C33 0.099(16) 0.044(10) 0.082(12) 0.000(9) 0.026(11) -0.033(11) C34 0.074(13) 0.032(8) 0.043(8) -0.005(7) 0.016(8) -0.013(9) C35 0.087(17) 0.100(16) 0.083(14) 0.014(12) 0.024(12) 0.052(14) C36 0.10(2) 0.098(17) 0.16(2) 0.012(17) 0.054(18) 0.025(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 I1 P1 2.436(4) . ? I2 I3 2.9024(19) . ? I3 I4 2.9042(19) . ? I5 P2 2.452(4) . ? I6 I7 2.8948(19) . ? I7 I8 2.880(2) . ? P1 N1 1.592(12) . ? P1 N3 1.603(12) . ? P1 N2 1.612(11) . ? P2 N5 1.600(11) . ? P2 N6 1.603(12) . ? P2 N4 1.612(12) . ? N1 C1 1.457(16) . ? N1 C4 1.481(17) . ? N2 C10 1.456(18) . ? N2 C7 1.508(17) . ? N3 C16 1.472(17) . ? N3 C13 1.484(17) . ? N4 C22 1.469(18) . ? N4 C19 1.476(17) . ? N5 C25 1.458(17) . ? N5 C28 1.488(16) . ? N6 C31 1.445(18) . ? N6 C34 1.494(17) . ? C1 C2 1.51(2) . ? C2 C3 1.51(2) . ? C4 C5 1.50(2) . ? C5 C6 1.49(2) . ? C7 C8 1.495(18) . ? C8 C9 1.56(2) . ? C10 C11 1.52(2) . ? C11 C12 1.49(2) . ? C13 C14 1.485(19) . ? C14 C15 1.50(2) . ? C16 C17 1.81(4) . ? C17 C18 1.15(3) . ? C19 C20 1.53(2) . ? C20 C21 1.51(2) . ? C22 C23 1.46(2) . ? C23 C24 1.50(2) . ? C25 C26 1.50(2) . ? C26 C27 1.51(2) . ? C28 C29 1.470(19) . ? C29 C30 1.529(19) . ? C31 C32 1.50(2) . ? C32 C33 1.53(2) . ? C34 C35 1.54(2) . ? C35 C36 1.49(2) . ? 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 I2 I3 I4 176.88(6) . . ? I8 I7 I6 178.57(7) . . ? N1 P1 N3 112.1(6) . . ? N1 P1 N2 112.9(6) . . ? N3 P1 N2 110.2(6) . . ? N1 P1 I1 107.2(5) . . ? N3 P1 I1 107.3(5) . . ? N2 P1 I1 106.7(5) . . ? N5 P2 N6 113.9(6) . . ? N5 P2 N4 112.0(6) . . ? N6 P2 N4 110.9(6) . . ? N5 P2 I5 107.8(5) . . ? N6 P2 I5 105.3(5) . . ? N4 P2 I5 106.4(5) . . ? C1 N1 C4 116.2(11) . . ? C1 N1 P1 123.7(9) . . ? C4 N1 P1 120.0(9) . . ? C10 N2 C7 116.8(11) . . ? C10 N2 P1 124.1(10) . . ? C7 N2 P1 118.9(9) . . ? C16 N3 C13 117.4(12) . . ? C16 N3 P1 123.8(10) . . ? C13 N3 P1 118.3(10) . . ? C22 N4 C19 117.4(12) . . ? C22 N4 P2 123.3(10) . . ? C19 N4 P2 119.3(10) . . ? C25 N5 C28 115.7(11) . . ? C25 N5 P2 124.0(10) . . ? C28 N5 P2 120.3(10) . . ? C31 N6 C34 117.2(11) . . ? C31 N6 P2 119.4(9) . . ? C34 N6 P2 123.0(10) . . ? N1 C1 C2 112.9(11) . . ? C1 C2 C3 111.9(13) . . ? N1 C4 C5 114.4(11) . . ? C6 C5 C4 111.9(14) . . ? C8 C7 N2 112.8(11) . . ? C7 C8 C9 109.9(12) . . ? N2 C10 C11 114.1(12) . . ? C12 C11 C10 111.1(14) . . ? N3 C13 C14 116.3(12) . . ? C13 C14 C15 110.8(13) . . ? N3 C16 C17 106.0(13) . . ? C18 C17 C16 95(4) . . ? N4 C19 C20 112.3(13) . . ? C21 C20 C19 109.7(16) . . ? C23 C22 N4 115.8(13) . . ? C22 C23 C24 113.1(15) . . ? N5 C25 C26 115.6(14) . . ? C25 C26 C27 112.3(15) . . ? C29 C28 N5 114.4(11) . . ? C28 C29 C30 113.1(13) . . ? N6 C31 C32 115.8(13) . . ? C31 C32 C33 109.4(13) . . ? N6 C34 C35 110.2(12) . . ? C36 C35 C34 109.8(16) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.936 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.162