# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Robert Less' _publ_contact_author_email RJL1003@CAM.AC.UK _publ_section_title ; Formation of a New Class of 7? Radicals via Sterically-Induced P-P Bond Cleavage of the Dimers [(CH)2(NR)2P]2 ; loop_ _publ_author_name 'Robert Less' 'Ruth Edge' 'Eric McInnes' 'Kristine Muther' 'Vesal Naseri' 'Jeremy M Rawson' ; D.S.Wright ; # Attachment '1a.cif' data_dw0833 _database_code_depnum_ccdc_archive 'CCDC 707574' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 N4 P2' _chemical_formula_sum 'C20 H40 N4 P2' _chemical_formula_weight 398.50 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3138(1) _cell_length_b 9.8033(2) _cell_length_c 10.3563(2) _cell_angle_alpha 73.7030(8) _cell_angle_beta 72.8375(8) _cell_angle_gamma 87.2143(9) _cell_volume 587.45(2) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8964 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 32.03 _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 218 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_reflns_number 12404 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 32.04 _reflns_number_total 4070 _reflns_number_gt 3776 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0360P)^2^+0.1241P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4070 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 P1 P 0.61737(3) 0.413034(19) 0.522368(19) 0.01896(6) Uani 1 1 d . . . N1 N 0.41003(11) 0.29205(7) 0.64188(7) 0.02213(12) Uani 1 1 d . . . N2 N 0.61805(11) 0.35168(7) 0.38012(7) 0.02198(12) Uani 1 1 d . . . C1 C 0.31433(13) 0.23265(8) 0.56063(9) 0.02501(15) Uani 1 1 d . . . H1A H 0.1815 0.1752 0.6009 0.030 Uiso 1 1 calc R . . C2 C 0.42473(13) 0.26348(9) 0.42344(9) 0.02490(15) Uani 1 1 d . . . H2A H 0.3766 0.2285 0.3596 0.030 Uiso 1 1 calc R . . C3 C 0.43874(15) 0.19493(9) 0.77472(8) 0.02657(15) Uani 1 1 d . . . C4 C 0.21448(18) 0.12138(11) 0.86506(10) 0.0382(2) Uani 1 1 d . . . H4A H 0.1019 0.1931 0.8757 0.057 Uiso 1 1 calc R . . H4B H 0.2256 0.0675 0.9580 0.057 Uiso 1 1 calc R . . H4C H 0.1723 0.0564 0.8194 0.057 Uiso 1 1 calc R . . C5 C 0.60846(18) 0.08275(11) 0.74321(11) 0.0396(2) Uani 1 1 d . . . H5A H 0.7550 0.1293 0.6925 0.059 Uiso 1 1 calc R . . H5B H 0.5647 0.0323 0.6852 0.059 Uiso 1 1 calc R . . H5C H 0.6143 0.0148 0.8317 0.059 Uiso 1 1 calc R . . C6 C 0.5138(2) 0.28419(12) 0.85318(11) 0.0456(3) Uani 1 1 d . . . H6A H 0.4038 0.3556 0.8720 0.068 Uiso 1 1 calc R . . H6B H 0.6572 0.3319 0.7956 0.068 Uiso 1 1 calc R . . H6C H 0.5287 0.2225 0.9424 0.068 Uiso 1 1 calc R . . C7 C 0.82183(14) 0.31539(9) 0.28111(9) 0.02629(15) Uani 1 1 d . . . C8 C 0.7668(2) 0.31183(13) 0.14757(10) 0.0418(2) Uani 1 1 d . . . H8A H 0.7020 0.4017 0.1102 0.063 Uiso 1 1 calc R . . H8B H 0.6604 0.2330 0.1701 0.063 Uiso 1 1 calc R . . H8C H 0.9027 0.2985 0.0770 0.063 Uiso 1 1 calc R . . C9 C 0.99996(16) 0.43140(11) 0.24413(11) 0.0359(2) Uani 1 1 d . . . H9A H 0.9439 0.5240 0.2051 0.054 Uiso 1 1 calc R . . H9B H 1.1326 0.4125 0.1744 0.054 Uiso 1 1 calc R . . H9C H 1.0377 0.4322 0.3292 0.054 Uiso 1 1 calc R . . C10 C 0.90344(16) 0.17064(10) 0.34742(11) 0.03511(19) Uani 1 1 d . . . H10A H 0.7837 0.0983 0.3778 0.053 Uiso 1 1 calc R . . H10B H 0.9484 0.1754 0.4289 0.053 Uiso 1 1 calc R . . H10C H 1.0305 0.1455 0.2780 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.02147(9) 0.01645(9) 0.01957(9) -0.00489(6) -0.00695(6) -0.00001(6) N1 0.0256(3) 0.0186(3) 0.0205(3) -0.0017(2) -0.0075(2) -0.0022(2) N2 0.0228(3) 0.0228(3) 0.0224(3) -0.0103(2) -0.0059(2) 0.0012(2) C1 0.0239(3) 0.0221(3) 0.0296(4) -0.0059(3) -0.0095(3) -0.0029(3) C2 0.0250(3) 0.0247(3) 0.0296(4) -0.0116(3) -0.0110(3) 0.0003(3) C3 0.0330(4) 0.0220(3) 0.0212(3) -0.0003(3) -0.0077(3) -0.0012(3) C4 0.0399(5) 0.0365(5) 0.0264(4) 0.0005(3) 0.0002(3) -0.0055(4) C5 0.0402(5) 0.0341(5) 0.0365(5) 0.0015(4) -0.0114(4) 0.0104(4) C6 0.0722(8) 0.0385(5) 0.0305(5) -0.0022(4) -0.0266(5) -0.0098(5) C7 0.0280(4) 0.0258(3) 0.0240(3) -0.0102(3) -0.0036(3) 0.0034(3) C8 0.0515(6) 0.0503(6) 0.0259(4) -0.0185(4) -0.0080(4) 0.0065(5) C9 0.0300(4) 0.0331(4) 0.0359(5) -0.0080(4) 0.0024(3) -0.0035(3) C10 0.0329(4) 0.0283(4) 0.0439(5) -0.0139(4) -0.0085(4) 0.0085(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 N1 1.7388(11) . ? P1 N2 1.7394(8) . ? P1 P1 2.2439(8) 2_666 ? N1 C1 1.4217(10) . ? N1 C3 1.4924(11) . ? N2 C2 1.4144(11) . ? N2 C7 1.4884(11) . ? C1 C2 1.3383(13) . ? C3 C6 1.5223(14) . ? C3 C4 1.5293(14) . ? C3 C5 1.5312(14) . ? C7 C9 1.5267(14) . ? C7 C10 1.5302(13) . ? C7 C8 1.5319(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 N2 94.28(4) . . ? N1 P1 P1 94.33(4) . 2_666 ? N2 P1 P1 94.24(4) . 2_666 ? C1 N1 C3 117.51(7) . . ? C1 N1 P1 106.31(6) . . ? C3 N1 P1 122.41(6) . . ? C2 N2 C7 118.74(7) . . ? C2 N2 P1 106.59(6) . . ? C7 N2 P1 124.11(6) . . ? C2 C1 N1 115.22(7) . . ? C1 C2 N2 115.34(7) . . ? N1 C3 C6 108.29(7) . . ? N1 C3 C4 108.47(8) . . ? C6 C3 C4 109.10(9) . . ? N1 C3 C5 110.85(7) . . ? C6 C3 C5 110.57(9) . . ? C4 C3 C5 109.51(8) . . ? N2 C7 C9 108.26(7) . . ? N2 C7 C10 110.85(8) . . ? C9 C7 C10 110.16(8) . . ? N2 C7 C8 108.28(8) . . ? C9 C7 C8 109.47(8) . . ? C10 C7 C8 109.77(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 32.04 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.313 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.039 # Attachment '1b.cif' data_dw0827 _database_code_depnum_ccdc_archive 'CCDC 707575' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 N4 P2' _chemical_formula_sum 'C40 H48 N4 P2' _chemical_formula_weight 646.76 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6059(3) _cell_length_b 10.2485(4) _cell_length_c 10.8287(4) _cell_angle_alpha 85.8725(16) _cell_angle_beta 74.5382(17) _cell_angle_gamma 73.0208(14) _cell_volume 880.36(6) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6684 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 346 _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.962 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 9748 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3565 _reflns_number_gt 2504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.8548P] 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 3565 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.08215(9) 0.07014(7) 0.00620(7) 0.0227(2) Uani 1 1 d . . . N1 N -0.0702(3) 0.2249(2) 0.0146(2) 0.0248(5) Uani 1 1 d . . . N2 N 0.0454(3) 0.0709(2) 0.1710(2) 0.0271(5) Uani 1 1 d . . . C1 C -0.1741(4) 0.2474(3) 0.1407(3) 0.0285(7) Uani 1 1 d . . . H1 H -0.275(4) 0.316(3) 0.159(3) 0.027(8) Uiso 1 1 d . . . C2 C -0.1119(4) 0.1637(3) 0.2259(3) 0.0280(6) Uani 1 1 d . . . H2 H -0.158(4) 0.163(3) 0.317(3) 0.030(8) Uiso 1 1 d . . . C11 C -0.0900(3) 0.3252(3) -0.0838(2) 0.0232(6) Uani 1 1 d . . . C12 C -0.2400(3) 0.3635(3) -0.1218(3) 0.0257(6) Uani 1 1 d . . . C121 C -0.3815(4) 0.3012(3) -0.0655(3) 0.0354(7) Uani 1 1 d . . . H12A H -0.3364 0.2098 -0.0335 0.053 Uiso 1 1 calc R . . H12B H -0.4376 0.2946 -0.1316 0.053 Uiso 1 1 calc R . . H12C H -0.4626 0.3585 0.0053 0.053 Uiso 1 1 calc R . . C13 C -0.2580(4) 0.4622(3) -0.2172(3) 0.0303(7) Uani 1 1 d . . . H13 H -0.3605 0.4895 -0.2423 0.036 Uiso 1 1 calc R . . C14 C -0.1325(4) 0.5213(3) -0.2762(3) 0.0321(7) Uani 1 1 d . . . C141 C -0.1542(5) 0.6264(3) -0.3807(3) 0.0471(9) Uani 1 1 d . . . H14A H -0.2710 0.6838 -0.3612 0.071 Uiso 1 1 calc R . . H14B H -0.1264 0.5799 -0.4630 0.071 Uiso 1 1 calc R . . H14C H -0.0792 0.6835 -0.3854 0.071 Uiso 1 1 calc R . . C15 C 0.0157(4) 0.4807(3) -0.2367(3) 0.0295(7) Uani 1 1 d . . . H15 H 0.1038 0.5200 -0.2766 0.035 Uiso 1 1 calc R . . C16 C 0.0395(4) 0.3848(3) -0.1413(3) 0.0254(6) Uani 1 1 d . . . C161 C 0.1992(4) 0.3505(3) -0.0996(3) 0.0334(7) Uani 1 1 d . . . H16A H 0.1725 0.3577 -0.0061 0.050 Uiso 1 1 calc R . . H16B H 0.2636 0.4143 -0.1388 0.050 Uiso 1 1 calc R . . H16C H 0.2659 0.2572 -0.1266 0.050 Uiso 1 1 calc R . . C21 C 0.1545(4) -0.0050(3) 0.2462(2) 0.0244(6) Uani 1 1 d . . . C22 C 0.1033(4) -0.1009(3) 0.3347(2) 0.0269(6) Uani 1 1 d . . . C221 C -0.0661(4) -0.1250(3) 0.3577(3) 0.0328(7) Uani 1 1 d . . . H22A H -0.1086 -0.0989 0.2814 0.049 Uiso 1 1 calc R . . H22B H -0.1442 -0.0700 0.4311 0.049 Uiso 1 1 calc R . . H22C H -0.0559 -0.2218 0.3756 0.049 Uiso 1 1 calc R . . C23 C 0.2156(4) -0.1760(3) 0.4034(3) 0.0323(7) Uani 1 1 d . . . H23 H 0.1821 -0.2413 0.4633 0.039 Uiso 1 1 calc R . . C24 C 0.3733(4) -0.1594(3) 0.3881(3) 0.0374(8) Uani 1 1 d . . . C241 C 0.4947(5) -0.2427(4) 0.4627(3) 0.0587(11) Uani 1 1 d . . . H24A H 0.4614 -0.3246 0.4963 0.088 Uiso 1 1 calc R . . H24B H 0.4924 -0.1879 0.5340 0.088 Uiso 1 1 calc R . . H24C H 0.6086 -0.2694 0.4060 0.088 Uiso 1 1 calc R . . C25 C 0.4187(4) -0.0614(3) 0.3020(3) 0.0338(7) Uani 1 1 d . . . H25 H 0.5256 -0.0471 0.2917 0.041 Uiso 1 1 calc R . . C26 C 0.3128(4) 0.0161(3) 0.2305(3) 0.0283(6) Uani 1 1 d . . . C261 C 0.3684(4) 0.1220(3) 0.1399(3) 0.0378(8) Uani 1 1 d . . . H26A H 0.2793 0.2087 0.1549 0.057 Uiso 1 1 calc R . . H26B H 0.3911 0.0919 0.0514 0.057 Uiso 1 1 calc R . . H26C H 0.4708 0.1342 0.1546 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0243(4) 0.0216(4) 0.0219(4) 0.0041(3) -0.0057(3) -0.0069(3) N1 0.0240(13) 0.0221(11) 0.0231(12) 0.0063(9) -0.0024(10) -0.0033(10) N2 0.0273(13) 0.0309(13) 0.0209(12) 0.0045(10) -0.0076(10) -0.0047(10) C1 0.0270(16) 0.0278(15) 0.0264(15) -0.0003(12) -0.0021(13) -0.0054(13) C2 0.0265(16) 0.0329(16) 0.0212(14) -0.0002(12) -0.0028(12) -0.0066(13) C11 0.0250(15) 0.0192(13) 0.0239(14) 0.0018(11) -0.0061(12) -0.0046(11) C12 0.0247(15) 0.0249(14) 0.0255(14) -0.0008(12) -0.0053(12) -0.0049(12) C121 0.0302(17) 0.0360(17) 0.0397(17) -0.0001(14) -0.0087(14) -0.0092(14) C13 0.0283(16) 0.0303(15) 0.0311(16) -0.0002(13) -0.0125(13) -0.0018(13) C14 0.0410(19) 0.0245(15) 0.0264(15) 0.0031(12) -0.0067(14) -0.0050(13) C141 0.059(2) 0.0395(19) 0.0359(18) 0.0140(15) -0.0117(17) -0.0065(17) C15 0.0341(17) 0.0254(15) 0.0287(15) 0.0032(12) -0.0043(13) -0.0123(13) C16 0.0285(16) 0.0219(14) 0.0265(15) 0.0021(12) -0.0073(12) -0.0085(12) C161 0.0304(17) 0.0308(16) 0.0418(18) 0.0052(14) -0.0105(14) -0.0130(13) C21 0.0275(16) 0.0245(14) 0.0204(13) 0.0004(11) -0.0090(12) -0.0037(12) C22 0.0327(17) 0.0269(14) 0.0199(14) 0.0008(12) -0.0052(12) -0.0083(12) C221 0.0400(18) 0.0326(16) 0.0261(15) 0.0059(13) -0.0079(14) -0.0125(14) C23 0.0409(19) 0.0309(16) 0.0215(14) 0.0071(12) -0.0073(13) -0.0070(14) C24 0.0386(19) 0.0412(18) 0.0288(16) 0.0031(14) -0.0133(14) -0.0024(15) C241 0.050(2) 0.073(3) 0.045(2) 0.0120(19) -0.0246(18) 0.002(2) C25 0.0273(17) 0.0435(18) 0.0321(16) 0.0001(14) -0.0120(14) -0.0083(14) C26 0.0288(16) 0.0297(15) 0.0255(15) -0.0003(12) -0.0062(13) -0.0075(13) C261 0.0373(19) 0.0435(19) 0.0370(17) 0.0036(15) -0.0083(15) -0.0204(15) _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 N2 1.727(2) . ? P1 N1 1.728(2) . ? P1 P1 2.3240(16) 2 ? N1 C1 1.412(3) . ? N1 C11 1.435(3) . ? N2 C2 1.411(4) . ? N2 C21 1.428(3) . ? C1 C2 1.324(4) . ? C11 C12 1.398(4) . ? C11 C16 1.406(4) . ? C12 C13 1.399(4) . ? C12 C121 1.505(4) . ? C13 C14 1.378(4) . ? C14 C15 1.392(4) . ? C14 C141 1.515(4) . ? C15 C16 1.387(4) . ? C16 C161 1.497(4) . ? C21 C22 1.404(4) . ? C21 C26 1.406(4) . ? C22 C23 1.395(4) . ? C22 C221 1.502(4) . ? C23 C24 1.382(5) . ? C24 C25 1.390(4) . ? C24 C241 1.517(4) . ? C25 C26 1.388(4) . ? C26 C261 1.506(4) . ? 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 N2 P1 N1 89.76(11) . . ? N2 P1 P1 97.44(9) . 2 ? N1 P1 P1 97.95(9) . 2 ? C1 N1 C11 121.9(2) . . ? C1 N1 P1 109.59(18) . . ? C11 N1 P1 128.36(18) . . ? C2 N2 C21 122.4(2) . . ? C2 N2 P1 110.02(19) . . ? C21 N2 P1 127.51(18) . . ? C2 C1 N1 113.6(3) . . ? C1 C2 N2 112.9(3) . . ? C12 C11 C16 120.3(2) . . ? C12 C11 N1 119.3(2) . . ? C16 C11 N1 120.5(2) . . ? C11 C12 C13 118.6(3) . . ? C11 C12 C121 122.5(2) . . ? C13 C12 C121 118.9(3) . . ? C14 C13 C12 122.4(3) . . ? C13 C14 C15 117.7(3) . . ? C13 C14 C141 121.4(3) . . ? C15 C14 C141 120.9(3) . . ? C16 C15 C14 122.4(3) . . ? C15 C16 C11 118.7(3) . . ? C15 C16 C161 119.5(3) . . ? C11 C16 C161 121.8(2) . . ? C22 C21 C26 120.4(3) . . ? C22 C21 N2 119.8(3) . . ? C26 C21 N2 119.8(2) . . ? C23 C22 C21 118.0(3) . . ? C23 C22 C221 119.4(3) . . ? C21 C22 C221 122.6(3) . . ? C24 C23 C22 122.8(3) . . ? C23 C24 C25 117.8(3) . . ? C23 C24 C241 122.3(3) . . ? C25 C24 C241 120.0(3) . . ? C26 C25 C24 122.1(3) . . ? C25 C26 C21 118.9(3) . . ? C25 C26 C261 119.6(3) . . ? C21 C26 C261 121.6(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.364 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.125 # Attachment '1c.cif' data_dw0844 _database_code_depnum_ccdc_archive 'CCDC 707576' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H72 N4 P2, 0.25(C4 H8 O)' _chemical_formula_sum 'C53 H74 N4 O0.25 P2' _chemical_formula_weight 833.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1056(1) _cell_length_b 20.2299(2) _cell_length_c 21.6313(2) _cell_angle_alpha 72.598(1) _cell_angle_beta 77.804(1) _cell_angle_gamma 81.880(1) _cell_volume 4923.51(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35857 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.940 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; The THF solvent molecule is disordered about an inversion centre: bond length constraints were applied to this moiety. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 57801 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.04 _reflns_number_total 17212 _reflns_number_gt 14137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The THF solvent molecule is poorly resolved, disordered about an inversion centre. Two bond length restraints (one for the O-C distances and one for the C-C distances in this moiety) were added to the least squares refinement. ; _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^)+(0.0368P)^2^+2.2495P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17212 _refine_ls_number_parameters 1122 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 P1 P 0.59659(3) 0.22515(2) 0.264741(19) 0.02339(9) Uani 1 1 d . . . P2 P 0.69857(3) 0.22319(2) 0.345974(19) 0.02316(9) Uani 1 1 d . . . P3 P -0.19396(3) 0.77776(2) 0.158750(19) 0.02208(9) Uani 1 1 d . . . P4 P -0.04795(3) 0.68955(2) 0.174516(19) 0.02233(9) Uani 1 1 d . . . N1 N 0.71066(10) 0.24850(6) 0.19998(6) 0.0238(3) Uani 1 1 d . . . N2 N 0.59735(10) 0.14665(7) 0.24851(6) 0.0243(3) Uani 1 1 d . . . N3 N 0.73385(11) 0.14007(7) 0.39181(6) 0.0251(3) Uani 1 1 d . . . N4 N 0.58433(11) 0.23360(7) 0.40747(6) 0.0257(3) Uani 1 1 d . . . N5 N -0.25850(11) 0.80393(7) 0.22753(6) 0.0253(3) Uani 1 1 d . . . N6 N -0.10869(10) 0.84717(6) 0.13194(6) 0.0236(3) Uani 1 1 d . . . N7 N -0.04147(11) 0.64647(7) 0.25542(6) 0.0248(3) Uani 1 1 d . . . N8 N -0.12271(10) 0.62493(6) 0.16893(6) 0.0228(3) Uani 1 1 d . . . C1 C 0.75766(13) 0.19080(8) 0.17731(8) 0.0256(3) Uani 1 1 d . . . H1 H 0.8266 0.1909 0.1466 0.031 Uiso 1 1 calc R . . C2 C 0.69724(13) 0.13585(8) 0.20258(8) 0.0257(3) Uani 1 1 d . . . H2 H 0.7184 0.0934 0.1912 0.031 Uiso 1 1 calc R . . C3 C 0.76537(13) 0.31153(8) 0.18481(7) 0.0257(3) Uani 1 1 d . . . C4 C 0.87722(13) 0.30938(8) 0.19487(8) 0.0270(3) Uani 1 1 d . . . C5 C 0.92631(15) 0.37207(9) 0.17868(8) 0.0325(4) Uani 1 1 d . . . H5 H 1.0028 0.3713 0.1834 0.039 Uiso 1 1 calc R . . C6 C 0.86702(15) 0.43497(9) 0.15604(9) 0.0372(4) Uani 1 1 d . . . H6 H 0.9019 0.4770 0.1462 0.045 Uiso 1 1 calc R . . C7 C 0.75672(15) 0.43666(9) 0.14776(9) 0.0368(4) Uani 1 1 d . . . H7 H 0.7157 0.4803 0.1328 0.044 Uiso 1 1 calc R . . C8 C 0.70398(14) 0.37547(8) 0.16090(8) 0.0312(4) Uani 1 1 d . . . C9 C 0.58315(15) 0.38076(9) 0.14940(10) 0.0403(4) Uani 1 1 d . . . H9 H 0.5655 0.3331 0.1519 0.048 Uiso 1 1 calc R . . C10 C 0.5690(2) 0.42795(12) 0.08088(13) 0.0682(7) Uani 1 1 d . . . H10A H 0.6208 0.4098 0.0472 0.102 Uiso 1 1 calc R . . H10B H 0.5866 0.4751 0.0767 0.102 Uiso 1 1 calc R . . H10C H 0.4907 0.4291 0.0749 0.102 Uiso 1 1 calc R . . C11 C 0.49837(17) 0.40534(11) 0.20314(13) 0.0573(6) Uani 1 1 d . . . H11A H 0.5089 0.3746 0.2465 0.086 Uiso 1 1 calc R . . H11B H 0.4209 0.4041 0.1969 0.086 Uiso 1 1 calc R . . H11C H 0.5111 0.4530 0.2004 0.086 Uiso 1 1 calc R . . C12 C 0.94724(13) 0.24276(9) 0.22403(8) 0.0296(4) Uani 1 1 d . . . H12 H 0.8951 0.2047 0.2432 0.036 Uiso 1 1 calc R . . C13 C 1.03890(15) 0.22203(10) 0.17063(9) 0.0395(4) Uani 1 1 d . . . H13A H 1.0030 0.2153 0.1366 0.059 Uiso 1 1 calc R . . H13B H 1.0816 0.1787 0.1904 0.059 Uiso 1 1 calc R . . H13C H 1.0907 0.2589 0.1507 0.059 Uiso 1 1 calc R . . C14 C 1.00246(16) 0.24923(10) 0.27936(9) 0.0411(4) Uani 1 1 d . . . H14A H 0.9451 0.2674 0.3109 0.062 Uiso 1 1 calc R . . H14B H 1.0626 0.2811 0.2606 0.062 Uiso 1 1 calc R . . H14C H 1.0350 0.2034 0.3019 0.062 Uiso 1 1 calc R . . C15 C 0.49361(13) 0.12131(8) 0.24348(8) 0.0251(3) Uani 1 1 d . . . C16 C 0.44114(13) 0.15214(8) 0.18818(8) 0.0285(4) Uani 1 1 d . . . C17 C 0.34360(14) 0.12530(10) 0.18465(9) 0.0359(4) Uani 1 1 d . . . H17 H 0.3075 0.1456 0.1476 0.043 Uiso 1 1 calc R . . C18 C 0.29835(15) 0.06998(10) 0.23374(9) 0.0395(4) Uani 1 1 d . . . H18 H 0.2312 0.0528 0.2307 0.047 Uiso 1 1 calc R . . C19 C 0.35094(15) 0.03967(10) 0.28724(9) 0.0372(4) Uani 1 1 d . . . H19 H 0.3195 0.0015 0.3209 0.045 Uiso 1 1 calc R . . C20 C 0.44958(14) 0.06401(9) 0.29288(8) 0.0304(4) Uani 1 1 d . . . C21 C 0.50484(16) 0.02631(10) 0.35207(9) 0.0393(4) Uani 1 1 d . . . H21 H 0.5763 0.0481 0.3477 0.047 Uiso 1 1 calc R . . C22 C 0.5352(2) -0.05078(11) 0.35542(12) 0.0584(6) Uani 1 1 d . . . H22A H 0.5872 -0.0549 0.3151 0.088 Uiso 1 1 calc R . . H22B H 0.4660 -0.0730 0.3597 0.088 Uiso 1 1 calc R . . H22C H 0.5718 -0.0737 0.3936 0.088 Uiso 1 1 calc R . . C23 C 0.42670(19) 0.03331(12) 0.41529(9) 0.0545(6) Uani 1 1 d . . . H23A H 0.4070 0.0827 0.4126 0.082 Uiso 1 1 calc R . . H23B H 0.4653 0.0112 0.4528 0.082 Uiso 1 1 calc R . . H23C H 0.3574 0.0105 0.4212 0.082 Uiso 1 1 calc R . . C24 C 0.48584(14) 0.21303(9) 0.13211(8) 0.0338(4) Uani 1 1 d . . . H24 H 0.5511 0.2285 0.1443 0.041 Uiso 1 1 calc R . . C25 C 0.52953(18) 0.19167(12) 0.06837(9) 0.0497(5) Uani 1 1 d . . . H25A H 0.5884 0.1530 0.0759 0.074 Uiso 1 1 calc R . . H25B H 0.5615 0.2313 0.0336 0.074 Uiso 1 1 calc R . . H25C H 0.4667 0.1771 0.0549 0.074 Uiso 1 1 calc R . . C26 C 0.39552(17) 0.27415(10) 0.12151(11) 0.0515(5) Uani 1 1 d . . . H26A H 0.3687 0.2871 0.1627 0.077 Uiso 1 1 calc R . . H26B H 0.3318 0.2608 0.1078 0.077 Uiso 1 1 calc R . . H26C H 0.4282 0.3138 0.0872 0.077 Uiso 1 1 calc R . . C27 C 0.64359(13) 0.11855(9) 0.44540(8) 0.0300(4) Uani 1 1 d . . . H27 H 0.6411 0.0723 0.4732 0.036 Uiso 1 1 calc R . . C28 C 0.56310(14) 0.16879(9) 0.45312(8) 0.0294(4) Uani 1 1 d . . . H28 H 0.4973 0.1616 0.4864 0.035 Uiso 1 1 calc R . . C29 C 0.84910(13) 0.11532(8) 0.40151(8) 0.0264(3) Uani 1 1 d . . . C30 C 0.90999(14) 0.06822(8) 0.36775(8) 0.0312(4) Uani 1 1 d . . . C31 C 1.02068(15) 0.04479(10) 0.37740(10) 0.0401(4) Uani 1 1 d . . . H31 H 1.0639 0.0141 0.3539 0.048 Uiso 1 1 calc R . . C32 C 1.06878(15) 0.06518(10) 0.42035(10) 0.0442(5) Uani 1 1 d . . . H32 H 1.1442 0.0484 0.4265 0.053 Uiso 1 1 calc R . . C33 C 1.00704(15) 0.11000(10) 0.45442(9) 0.0389(4) Uani 1 1 d . . . H33 H 1.0401 0.1231 0.4846 0.047 Uiso 1 1 calc R . . C34 C 0.89735(14) 0.13645(9) 0.44551(8) 0.0295(4) Uani 1 1 d . . . C35 C 0.83352(14) 0.18516(9) 0.48492(8) 0.0336(4) Uani 1 1 d . . . H35 H 0.7623 0.2050 0.4672 0.040 Uiso 1 1 calc R . . C36 C 0.80008(18) 0.14506(11) 0.55736(9) 0.0478(5) Uani 1 1 d . . . H36A H 0.7556 0.1068 0.5607 0.072 Uiso 1 1 calc R . . H36B H 0.7546 0.1765 0.5816 0.072 Uiso 1 1 calc R . . H36C H 0.8687 0.1262 0.5762 0.072 Uiso 1 1 calc R . . C37 C 0.90256(17) 0.24577(10) 0.47793(10) 0.0453(5) Uani 1 1 d . . . H37A H 0.9209 0.2716 0.4314 0.068 Uiso 1 1 calc R . . H37B H 0.9729 0.2276 0.4950 0.068 Uiso 1 1 calc R . . H37C H 0.8581 0.2768 0.5029 0.068 Uiso 1 1 calc R . . C38 C 0.85538(16) 0.03722(9) 0.32726(9) 0.0395(4) Uani 1 1 d . . . H38 H 0.7883 0.0693 0.3141 0.047 Uiso 1 1 calc R . . C39 C 0.93322(19) 0.02745(12) 0.26478(11) 0.0548(6) Uani 1 1 d . . . H39A H 0.9651 0.0714 0.2391 0.082 Uiso 1 1 calc R . . H39B H 0.8897 0.0128 0.2385 0.082 Uiso 1 1 calc R . . H39C H 0.9949 -0.0082 0.2766 0.082 Uiso 1 1 calc R . . C40 C 0.8123(2) -0.03207(11) 0.37135(12) 0.0588(6) Uani 1 1 d . . . H40A H 0.7583 -0.0242 0.4097 0.088 Uiso 1 1 calc R . . H40B H 0.8764 -0.0639 0.3862 0.088 Uiso 1 1 calc R . . H40C H 0.7746 -0.0525 0.3464 0.088 Uiso 1 1 calc R . . C41 C 0.50714(14) 0.29494(9) 0.40358(8) 0.0290(4) Uani 1 1 d . . . C42 C 0.54698(15) 0.35707(9) 0.40373(8) 0.0336(4) Uani 1 1 d . . . C43 C 0.47050(18) 0.41574(10) 0.40024(10) 0.0469(5) Uani 1 1 d . . . H43 H 0.4968 0.4584 0.3987 0.056 Uiso 1 1 calc R . . C44 C 0.35815(18) 0.41371(11) 0.39892(11) 0.0538(5) Uani 1 1 d . . . H44 H 0.3071 0.4541 0.3979 0.065 Uiso 1 1 calc R . . C45 C 0.32004(16) 0.35253(11) 0.39903(10) 0.0478(5) Uani 1 1 d . . . H45 H 0.2420 0.3511 0.3988 0.057 Uiso 1 1 calc R . . C46 C 0.39296(14) 0.29289(10) 0.39948(8) 0.0349(4) Uani 1 1 d . . . C47 C 0.34590(15) 0.22926(11) 0.39481(9) 0.0401(4) Uani 1 1 d . . . H47 H 0.4114 0.1945 0.3881 0.048 Uiso 1 1 calc R . . C48 C 0.28422(17) 0.24560(14) 0.33615(11) 0.0581(6) Uani 1 1 d . . . H48A H 0.3336 0.2696 0.2959 0.087 Uiso 1 1 calc R . . H48B H 0.2145 0.2754 0.3439 0.087 Uiso 1 1 calc R . . H48C H 0.2651 0.2022 0.3312 0.087 Uiso 1 1 calc R . . C49 C 0.26659(17) 0.19576(12) 0.45884(11) 0.0535(5) Uani 1 1 d . . . H49A H 0.3069 0.1848 0.4959 0.080 Uiso 1 1 calc R . . H49B H 0.2422 0.1529 0.4556 0.080 Uiso 1 1 calc R . . H49C H 0.2000 0.2282 0.4658 0.080 Uiso 1 1 calc R . . C50 C 0.66873(15) 0.36339(9) 0.40790(9) 0.0359(4) Uani 1 1 d . . . H50 H 0.7098 0.3160 0.4142 0.043 Uiso 1 1 calc R . . C51 C 0.6742(2) 0.38871(12) 0.46702(12) 0.0577(6) Uani 1 1 d . . . H51A H 0.6384 0.3564 0.5075 0.087 Uiso 1 1 calc R . . H51B H 0.6341 0.4351 0.4622 0.087 Uiso 1 1 calc R . . H51C H 0.7536 0.3909 0.4692 0.087 Uiso 1 1 calc R . . C52 C 0.7291(2) 0.41068(12) 0.34432(11) 0.0594(6) Uani 1 1 d . . . H52A H 0.7273 0.3926 0.3073 0.089 Uiso 1 1 calc R . . H52B H 0.8080 0.4122 0.3479 0.089 Uiso 1 1 calc R . . H52C H 0.6906 0.4577 0.3369 0.089 Uiso 1 1 calc R . . C53 C -0.19808(13) 0.85644(8) 0.23391(8) 0.0282(4) Uani 1 1 d . . . H53 H -0.2143 0.8738 0.2714 0.034 Uiso 1 1 calc R . . C54 C -0.11698(13) 0.87880(8) 0.18259(8) 0.0270(3) Uani 1 1 d . . . H54 H -0.0690 0.9131 0.1803 0.032 Uiso 1 1 calc R . . C55 C -0.38129(13) 0.80897(8) 0.24699(8) 0.0258(3) Uani 1 1 d . . . C56 C -0.44854(13) 0.86202(8) 0.20936(8) 0.0280(4) Uani 1 1 d . . . C57 C -0.56533(14) 0.86552(9) 0.23086(9) 0.0344(4) Uani 1 1 d . . . H57 H -0.6119 0.9017 0.2068 0.041 Uiso 1 1 calc R . . C58 C -0.61518(14) 0.81768(10) 0.28623(9) 0.0390(4) Uani 1 1 d . . . H58 H -0.6953 0.8202 0.2993 0.047 Uiso 1 1 calc R . . C59 C -0.54849(14) 0.76635(10) 0.32245(9) 0.0375(4) Uani 1 1 d . . . H59 H -0.5835 0.7337 0.3606 0.045 Uiso 1 1 calc R . . C60 C -0.43061(14) 0.76106(9) 0.30460(8) 0.0303(4) Uani 1 1 d . . . C61 C -0.36202(15) 0.70722(9) 0.35039(8) 0.0351(4) Uani 1 1 d . . . H61 H -0.2803 0.7079 0.3290 0.042 Uiso 1 1 calc R . . C62 C -0.39679(17) 0.63368(10) 0.36534(10) 0.0465(5) Uani 1 1 d . . . H62A H -0.3905 0.6217 0.3240 0.070 Uiso 1 1 calc R . . H62B H -0.4754 0.6313 0.3889 0.070 Uiso 1 1 calc R . . H62C H -0.3468 0.6008 0.3927 0.070 Uiso 1 1 calc R . . C63 C -0.37522(18) 0.72770(12) 0.41468(10) 0.0510(5) Uani 1 1 d . . . H63A H -0.3451 0.7729 0.4051 0.076 Uiso 1 1 calc R . . H63B H -0.3333 0.6925 0.4453 0.076 Uiso 1 1 calc R . . H63C H -0.4557 0.7308 0.4346 0.076 Uiso 1 1 calc R . . C64 C -0.39997(14) 0.91571(8) 0.14731(8) 0.0311(4) Uani 1 1 d . . . H64 H -0.3187 0.8998 0.1340 0.037 Uiso 1 1 calc R . . C65 C -0.40280(18) 0.98656(10) 0.15980(11) 0.0495(5) Uani 1 1 d . . . H65A H -0.3605 0.9819 0.1950 0.074 Uiso 1 1 calc R . . H65B H -0.4816 1.0036 0.1729 0.074 Uiso 1 1 calc R . . H65C H -0.3681 1.0196 0.1195 0.074 Uiso 1 1 calc R . . C66 C -0.46052(16) 0.92278(11) 0.09012(9) 0.0448(5) Uani 1 1 d . . . H66A H -0.4581 0.8772 0.0825 0.067 Uiso 1 1 calc R . . H66B H -0.4227 0.9551 0.0503 0.067 Uiso 1 1 calc R . . H66C H -0.5397 0.9406 0.1009 0.067 Uiso 1 1 calc R . . C67 C -0.02264(13) 0.85944(8) 0.07414(8) 0.0272(3) Uani 1 1 d . . . C68 C -0.05487(15) 0.87766(8) 0.01165(8) 0.0315(4) Uani 1 1 d . . . C69 C 0.03034(17) 0.89124(10) -0.04379(9) 0.0434(5) Uani 1 1 d . . . H69 H 0.0107 0.9025 -0.0862 0.052 Uiso 1 1 calc R . . C70 C 0.14245(17) 0.88876(12) -0.03869(10) 0.0522(6) Uani 1 1 d . . . H70 H 0.1987 0.9000 -0.0773 0.063 Uiso 1 1 calc R . . C71 C 0.17278(16) 0.87004(11) 0.02222(10) 0.0452(5) Uani 1 1 d . . . H71 H 0.2503 0.8685 0.0252 0.054 Uiso 1 1 calc R . . C72 C 0.09242(14) 0.85318(9) 0.07989(9) 0.0330(4) Uani 1 1 d . . . C73 C 0.13402(14) 0.82700(9) 0.14536(9) 0.0382(4) Uani 1 1 d . . . H73 H 0.0684 0.8087 0.1803 0.046 Uiso 1 1 calc R . . C74 C 0.22768(16) 0.76750(12) 0.14561(13) 0.0611(6) Uani 1 1 d . . . H74A H 0.2027 0.7317 0.1308 0.092 Uiso 1 1 calc R . . H74B H 0.2437 0.7473 0.1903 0.092 Uiso 1 1 calc R . . H74C H 0.2966 0.7854 0.1158 0.092 Uiso 1 1 calc R . . C75 C 0.17573(17) 0.88588(11) 0.16325(10) 0.0479(5) Uani 1 1 d . . . H75A H 0.1150 0.9234 0.1639 0.072 Uiso 1 1 calc R . . H75B H 0.2416 0.9039 0.1305 0.072 Uiso 1 1 calc R . . H75C H 0.1972 0.8681 0.2068 0.072 Uiso 1 1 calc R . . C76 C -0.17686(15) 0.88145(9) 0.00298(8) 0.0341(4) Uani 1 1 d . . . H76 H -0.2265 0.8819 0.0462 0.041 Uiso 1 1 calc R . . C77 C -0.2103(2) 0.94787(12) -0.04831(11) 0.0610(6) Uani 1 1 d . . . H77A H -0.1954 0.9885 -0.0365 0.092 Uiso 1 1 calc R . . H77B H -0.2912 0.9499 -0.0496 0.092 Uiso 1 1 calc R . . H77C H -0.1657 0.9478 -0.0917 0.092 Uiso 1 1 calc R . . C78 C -0.20039(16) 0.81776(11) -0.01500(9) 0.0420(4) Uani 1 1 d . . . H78A H -0.1792 0.7754 0.0181 0.063 Uiso 1 1 calc R . . H78B H -0.1557 0.8173 -0.0583 0.063 Uiso 1 1 calc R . . H78C H -0.2813 0.8198 -0.0163 0.063 Uiso 1 1 calc R . . C79 C -0.11558(13) 0.59192(8) 0.27903(8) 0.0271(3) Uani 1 1 d . . . H79 H -0.1315 0.5657 0.3239 0.032 Uiso 1 1 calc R . . C80 C -0.16016(13) 0.58138(8) 0.23200(8) 0.0256(3) Uani 1 1 d . . . H80 H -0.2125 0.5476 0.2402 0.031 Uiso 1 1 calc R . . C81 C 0.06341(13) 0.63744(8) 0.28016(8) 0.0266(3) Uani 1 1 d . . . C82 C 0.07428(14) 0.67822(9) 0.32074(8) 0.0298(4) Uani 1 1 d . . . C83 C 0.17544(15) 0.66935(10) 0.34454(9) 0.0375(4) Uani 1 1 d . . . H83 H 0.1846 0.6967 0.3717 0.045 Uiso 1 1 calc R . . C84 C 0.26238(15) 0.62174(10) 0.32949(9) 0.0400(4) Uani 1 1 d . . . H84 H 0.3308 0.6166 0.3460 0.048 Uiso 1 1 calc R . . C85 C 0.24978(14) 0.58153(9) 0.29025(9) 0.0368(4) Uani 1 1 d . . . H85 H 0.3097 0.5484 0.2805 0.044 Uiso 1 1 calc R . . C86 C 0.15115(14) 0.58851(9) 0.26464(8) 0.0302(4) Uani 1 1 d . . . C87 C 0.14329(15) 0.54265(9) 0.22166(9) 0.0363(4) Uani 1 1 d . . . H87 H 0.0721 0.5585 0.2030 0.044 Uiso 1 1 calc R . . C88 C 0.1360(2) 0.46666(10) 0.26248(12) 0.0565(6) Uani 1 1 d . . . H88A H 0.0696 0.4630 0.2979 0.085 Uiso 1 1 calc R . . H88B H 0.2048 0.4500 0.2815 0.085 Uiso 1 1 calc R . . H88C H 0.1288 0.4383 0.2341 0.085 Uiso 1 1 calc R . . C89 C 0.24340(16) 0.54978(12) 0.16401(10) 0.0526(5) Uani 1 1 d . . . H89A H 0.2449 0.5985 0.1377 0.079 Uiso 1 1 calc R . . H89B H 0.2350 0.5209 0.1364 0.079 Uiso 1 1 calc R . . H89C H 0.3144 0.5346 0.1811 0.079 Uiso 1 1 calc R . . C90 C -0.02265(15) 0.72720(9) 0.34239(9) 0.0373(4) Uani 1 1 d . . . H90 H -0.0793 0.7355 0.3127 0.045 Uiso 1 1 calc R . . C91 C 0.01449(18) 0.79748(10) 0.33889(11) 0.0484(5) Uani 1 1 d . . . H91A H 0.0531 0.8189 0.2941 0.073 Uiso 1 1 calc R . . H91B H 0.0664 0.7908 0.3698 0.073 Uiso 1 1 calc R . . H91C H -0.0522 0.8279 0.3505 0.073 Uiso 1 1 calc R . . C92 C -0.08020(18) 0.69236(12) 0.41247(11) 0.0534(5) Uani 1 1 d . . . H92A H -0.1105 0.6496 0.4133 0.080 Uiso 1 1 calc R . . H92B H -0.1423 0.7241 0.4271 0.080 Uiso 1 1 calc R . . H92C H -0.0247 0.6811 0.4420 0.080 Uiso 1 1 calc R . . C93 C -0.16296(13) 0.62561(7) 0.11092(7) 0.0241(3) Uani 1 1 d . . . C94 C -0.08348(14) 0.61939(8) 0.05460(8) 0.0273(3) Uani 1 1 d . . . C95 C -0.12412(16) 0.61689(9) -0.00026(8) 0.0341(4) Uani 1 1 d . . . H95 H -0.0717 0.6136 -0.0389 0.041 Uiso 1 1 calc R . . C96 C -0.23841(16) 0.61907(9) 0.00025(9) 0.0381(4) Uani 1 1 d . . . H96 H -0.2641 0.6149 -0.0369 0.046 Uiso 1 1 calc R . . C97 C -0.31559(15) 0.62738(9) 0.05496(9) 0.0347(4) Uani 1 1 d . . . H97 H -0.3944 0.6295 0.0547 0.042 Uiso 1 1 calc R . . C98 C -0.28042(13) 0.63268(8) 0.11054(8) 0.0272(3) Uani 1 1 d . . . C99 C -0.37042(13) 0.64839(9) 0.16646(9) 0.0320(4) Uani 1 1 d . . . H99 H -0.3307 0.6591 0.1980 0.038 Uiso 1 1 calc R . . C100 C -0.43970(16) 0.58647(10) 0.20436(10) 0.0450(5) Uani 1 1 d . . . H10D H -0.3887 0.5462 0.2218 0.067 Uiso 1 1 calc R . . H10E H -0.4807 0.5754 0.1747 0.067 Uiso 1 1 calc R . . H10F H -0.4941 0.5982 0.2409 0.067 Uiso 1 1 calc R . . C101 C -0.45022(15) 0.71228(10) 0.14098(11) 0.0445(5) Uani 1 1 d . . . H10G H -0.4053 0.7508 0.1136 0.067 Uiso 1 1 calc R . . H10H H -0.4986 0.7259 0.1784 0.067 Uiso 1 1 calc R . . H10I H -0.4977 0.7010 0.1146 0.067 Uiso 1 1 calc R . . C102 C 0.04426(14) 0.61444(8) 0.05070(8) 0.0299(4) Uani 1 1 d . . . H102 H 0.0587 0.6109 0.0955 0.036 Uiso 1 1 calc R . . C103 C 0.10297(16) 0.54940(10) 0.03143(9) 0.0395(4) Uani 1 1 d . . . H10K H 0.0722 0.5079 0.0638 0.059 Uiso 1 1 calc R . . H10L H 0.1847 0.5474 0.0304 0.059 Uiso 1 1 calc R . . H10M H 0.0895 0.5513 -0.0122 0.059 Uiso 1 1 calc R . . C104 C 0.09568(17) 0.67984(10) 0.00284(10) 0.0462(5) Uani 1 1 d . . . H10N H 0.0583 0.7209 0.0162 0.069 Uiso 1 1 calc R . . H10O H 0.0846 0.6839 -0.0418 0.069 Uiso 1 1 calc R . . H10P H 0.1770 0.6765 0.0035 0.069 Uiso 1 1 calc R . . O1 O -0.0762(3) 0.50409(18) 0.43923(14) 0.0640(8) Uani 0.50 1 d PD A -1 C105 C 0.0390(10) 0.4850(8) 0.4423(8) 0.072(3) Uani 0.50 1 d PD A -1 H10Q H 0.0871 0.5069 0.3999 0.087 Uiso 0.50 1 calc PR A -1 H10R H 0.0549 0.4339 0.4521 0.087 Uiso 0.50 1 calc PR A -1 C106 C 0.0621(5) 0.5102(4) 0.4967(3) 0.0714(18) Uani 0.50 1 d PD A -1 H10S H 0.0879 0.5577 0.4793 0.086 Uiso 0.50 1 calc PR A -1 H10T H 0.1203 0.4787 0.5195 0.086 Uiso 0.50 1 calc PR A -1 C107 C -0.0527(10) 0.5097(8) 0.5427(6) 0.059(3) Uani 0.50 1 d PD A -1 H10U H -0.0513 0.4726 0.5846 0.071 Uiso 0.50 1 calc PR A -1 H10W H -0.0749 0.5550 0.5524 0.071 Uiso 0.50 1 calc PR A -1 C108 C -0.1312(6) 0.4956(4) 0.5041(3) 0.0754(18) Uani 0.50 1 d PD A -1 H10V H -0.1541 0.4476 0.5236 0.090 Uiso 0.50 1 calc PR A -1 H10Y H -0.2003 0.5282 0.5056 0.090 Uiso 0.50 1 calc PR A -1 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 0.0235(2) 0.0253(2) 0.0208(2) -0.00567(16) -0.00406(16) -0.00153(16) P2 0.0234(2) 0.0253(2) 0.0210(2) -0.00663(16) -0.00314(16) -0.00382(16) P3 0.0220(2) 0.0219(2) 0.0227(2) -0.00698(16) -0.00345(15) -0.00224(15) P4 0.0223(2) 0.0217(2) 0.0235(2) -0.00719(16) -0.00397(15) -0.00187(15) N1 0.0251(7) 0.0225(7) 0.0231(7) -0.0061(5) -0.0030(5) -0.0022(5) N2 0.0229(7) 0.0257(7) 0.0246(7) -0.0063(6) -0.0049(5) -0.0036(5) N3 0.0244(7) 0.0254(7) 0.0254(7) -0.0050(6) -0.0064(5) -0.0036(5) N4 0.0250(7) 0.0290(7) 0.0223(7) -0.0067(6) -0.0020(5) -0.0039(6) N5 0.0227(7) 0.0291(7) 0.0253(7) -0.0104(6) -0.0019(5) -0.0042(5) N6 0.0238(7) 0.0226(7) 0.0245(7) -0.0074(5) -0.0019(5) -0.0038(5) N7 0.0249(7) 0.0260(7) 0.0245(7) -0.0068(6) -0.0064(5) -0.0034(5) N8 0.0258(7) 0.0223(6) 0.0218(7) -0.0075(5) -0.0047(5) -0.0029(5) C1 0.0240(8) 0.0277(8) 0.0247(8) -0.0086(7) -0.0039(6) 0.0009(6) C2 0.0236(8) 0.0258(8) 0.0280(8) -0.0081(7) -0.0066(6) 0.0012(6) C3 0.0295(8) 0.0247(8) 0.0207(8) -0.0057(6) 0.0007(6) -0.0046(7) C4 0.0298(8) 0.0289(8) 0.0213(8) -0.0079(7) 0.0012(6) -0.0058(7) C5 0.0323(9) 0.0345(9) 0.0301(9) -0.0110(7) 0.0029(7) -0.0091(7) C6 0.0427(10) 0.0291(9) 0.0368(10) -0.0099(8) 0.0065(8) -0.0118(8) C7 0.0435(11) 0.0240(9) 0.0360(10) -0.0049(7) 0.0023(8) -0.0015(8) C8 0.0339(9) 0.0278(9) 0.0281(9) -0.0056(7) -0.0007(7) -0.0022(7) C9 0.0380(10) 0.0274(9) 0.0494(11) -0.0004(8) -0.0111(8) 0.0003(8) C10 0.0667(15) 0.0522(13) 0.0742(17) 0.0190(12) -0.0377(13) -0.0096(11) C11 0.0360(11) 0.0387(11) 0.0932(18) -0.0224(12) -0.0016(11) 0.0039(9) C12 0.0259(8) 0.0314(9) 0.0295(9) -0.0040(7) -0.0045(7) -0.0060(7) C13 0.0302(9) 0.0394(10) 0.0453(11) -0.0108(9) -0.0027(8) 0.0010(8) C14 0.0369(10) 0.0492(11) 0.0381(10) -0.0047(9) -0.0127(8) -0.0140(9) C15 0.0224(8) 0.0288(8) 0.0250(8) -0.0085(7) -0.0046(6) -0.0020(6) C16 0.0258(8) 0.0319(9) 0.0282(9) -0.0087(7) -0.0069(7) 0.0001(7) C17 0.0289(9) 0.0463(11) 0.0333(10) -0.0084(8) -0.0121(7) -0.0014(8) C18 0.0281(9) 0.0520(11) 0.0403(10) -0.0090(9) -0.0101(8) -0.0113(8) C19 0.0337(9) 0.0430(10) 0.0339(10) -0.0052(8) -0.0052(8) -0.0133(8) C20 0.0292(9) 0.0350(9) 0.0277(9) -0.0069(7) -0.0063(7) -0.0069(7) C21 0.0416(10) 0.0422(10) 0.0325(10) 0.0051(8) -0.0146(8) -0.0201(8) C22 0.0631(14) 0.0464(12) 0.0621(14) 0.0025(11) -0.0299(12) -0.0035(10) C23 0.0713(15) 0.0626(14) 0.0309(10) 0.0008(10) -0.0135(10) -0.0335(12) C24 0.0312(9) 0.0385(10) 0.0296(9) -0.0014(8) -0.0122(7) -0.0031(7) C25 0.0499(12) 0.0673(14) 0.0294(10) -0.0061(10) -0.0070(9) -0.0138(10) C26 0.0442(11) 0.0430(11) 0.0601(13) 0.0039(10) -0.0237(10) 0.0015(9) C27 0.0290(9) 0.0314(9) 0.0273(9) -0.0005(7) -0.0055(7) -0.0108(7) C28 0.0263(8) 0.0362(9) 0.0246(8) -0.0048(7) -0.0023(7) -0.0106(7) C29 0.0256(8) 0.0266(8) 0.0258(8) -0.0032(7) -0.0070(6) -0.0039(6) C30 0.0353(9) 0.0278(9) 0.0310(9) -0.0071(7) -0.0104(7) 0.0004(7) C31 0.0340(10) 0.0406(10) 0.0481(11) -0.0179(9) -0.0105(8) 0.0065(8) C32 0.0290(9) 0.0529(12) 0.0549(12) -0.0183(10) -0.0170(9) 0.0043(8) C33 0.0324(9) 0.0502(11) 0.0395(10) -0.0149(9) -0.0144(8) -0.0038(8) C34 0.0280(9) 0.0331(9) 0.0276(9) -0.0066(7) -0.0057(7) -0.0064(7) C35 0.0312(9) 0.0436(10) 0.0317(9) -0.0163(8) -0.0092(7) -0.0038(8) C36 0.0492(12) 0.0645(13) 0.0330(10) -0.0184(10) -0.0053(9) -0.0085(10) C37 0.0451(11) 0.0507(12) 0.0511(12) -0.0247(10) -0.0153(9) -0.0063(9) C38 0.0422(10) 0.0376(10) 0.0480(11) -0.0228(9) -0.0211(9) 0.0094(8) C39 0.0638(14) 0.0586(13) 0.0519(13) -0.0322(11) -0.0216(11) 0.0163(11) C40 0.0611(14) 0.0479(12) 0.0808(17) -0.0329(12) -0.0170(12) -0.0094(10) C41 0.0292(9) 0.0352(9) 0.0210(8) -0.0085(7) -0.0022(6) 0.0004(7) C42 0.0385(10) 0.0345(9) 0.0258(9) -0.0091(7) -0.0016(7) -0.0007(8) C43 0.0549(13) 0.0351(10) 0.0486(12) -0.0130(9) -0.0079(10) 0.0036(9) C44 0.0511(13) 0.0468(12) 0.0569(13) -0.0142(10) -0.0097(10) 0.0170(10) C45 0.0332(10) 0.0612(13) 0.0460(12) -0.0152(10) -0.0098(9) 0.0103(9) C46 0.0288(9) 0.0469(11) 0.0278(9) -0.0117(8) -0.0035(7) 0.0012(8) C47 0.0259(9) 0.0595(12) 0.0400(10) -0.0213(9) -0.0054(8) -0.0047(8) C48 0.0360(11) 0.0919(18) 0.0583(14) -0.0350(13) -0.0194(10) 0.0035(11) C49 0.0353(11) 0.0751(15) 0.0548(13) -0.0270(12) 0.0048(9) -0.0194(10) C50 0.0399(10) 0.0307(9) 0.0380(10) -0.0124(8) -0.0025(8) -0.0071(8) C51 0.0602(14) 0.0654(14) 0.0624(14) -0.0369(12) -0.0150(11) -0.0061(11) C52 0.0599(14) 0.0524(13) 0.0572(14) -0.0063(11) 0.0037(11) -0.0179(11) C53 0.0276(8) 0.0323(9) 0.0301(9) -0.0155(7) -0.0067(7) -0.0028(7) C54 0.0256(8) 0.0263(8) 0.0322(9) -0.0112(7) -0.0066(7) -0.0038(7) C55 0.0224(8) 0.0307(9) 0.0284(8) -0.0156(7) -0.0018(6) -0.0036(7) C56 0.0265(8) 0.0304(9) 0.0308(9) -0.0148(7) -0.0035(7) -0.0030(7) C57 0.0260(9) 0.0412(10) 0.0375(10) -0.0148(8) -0.0060(7) 0.0004(7) C58 0.0220(9) 0.0560(12) 0.0387(10) -0.0153(9) -0.0002(7) -0.0053(8) C59 0.0302(9) 0.0496(11) 0.0310(9) -0.0101(8) 0.0007(7) -0.0099(8) C60 0.0290(9) 0.0368(9) 0.0271(9) -0.0123(7) -0.0019(7) -0.0065(7) C61 0.0317(9) 0.0411(10) 0.0285(9) -0.0057(8) -0.0019(7) -0.0038(8) C62 0.0460(11) 0.0424(11) 0.0426(11) -0.0056(9) 0.0022(9) -0.0049(9) C63 0.0566(13) 0.0630(14) 0.0352(11) -0.0125(10) -0.0138(9) -0.0053(10) C64 0.0247(8) 0.0302(9) 0.0366(9) -0.0101(7) -0.0027(7) 0.0010(7) C65 0.0503(12) 0.0326(10) 0.0612(13) -0.0138(10) 0.0022(10) -0.0059(9) C66 0.0400(11) 0.0499(12) 0.0385(11) -0.0031(9) -0.0108(8) 0.0011(9) C67 0.0284(8) 0.0220(8) 0.0285(9) -0.0065(7) 0.0015(7) -0.0048(6) C68 0.0383(9) 0.0259(8) 0.0294(9) -0.0093(7) 0.0001(7) -0.0058(7) C69 0.0523(12) 0.0509(12) 0.0278(9) -0.0131(9) 0.0027(8) -0.0175(9) C70 0.0470(12) 0.0725(15) 0.0385(11) -0.0231(11) 0.0161(9) -0.0289(11) C71 0.0331(10) 0.0594(13) 0.0468(12) -0.0239(10) 0.0074(8) -0.0178(9) C72 0.0298(9) 0.0314(9) 0.0378(10) -0.0111(8) 0.0002(7) -0.0084(7) C73 0.0266(9) 0.0381(10) 0.0449(11) -0.0024(8) -0.0054(8) -0.0078(8) C74 0.0287(10) 0.0535(13) 0.0824(17) 0.0026(12) -0.0028(10) -0.0003(9) C75 0.0417(11) 0.0574(13) 0.0448(11) -0.0011(10) -0.0169(9) -0.0198(9) C76 0.0387(10) 0.0366(10) 0.0232(8) -0.0061(7) -0.0060(7) 0.0051(8) C77 0.0760(16) 0.0522(13) 0.0420(12) 0.0004(10) -0.0153(11) 0.0140(11) C78 0.0375(10) 0.0566(12) 0.0363(10) -0.0188(9) -0.0085(8) -0.0027(9) C79 0.0279(8) 0.0283(8) 0.0230(8) -0.0040(7) -0.0026(6) -0.0054(7) C80 0.0263(8) 0.0246(8) 0.0247(8) -0.0051(7) -0.0021(6) -0.0052(6) C81 0.0258(8) 0.0282(8) 0.0257(8) -0.0044(7) -0.0081(6) -0.0036(7) C82 0.0308(9) 0.0310(9) 0.0296(9) -0.0083(7) -0.0089(7) -0.0043(7) C83 0.0379(10) 0.0417(10) 0.0409(10) -0.0156(8) -0.0155(8) -0.0072(8) C84 0.0296(9) 0.0485(11) 0.0456(11) -0.0126(9) -0.0158(8) -0.0030(8) C85 0.0281(9) 0.0402(10) 0.0410(10) -0.0106(8) -0.0080(8) 0.0015(8) C86 0.0300(9) 0.0317(9) 0.0284(9) -0.0064(7) -0.0069(7) -0.0029(7) C87 0.0347(9) 0.0380(10) 0.0406(10) -0.0172(8) -0.0142(8) 0.0075(8) C88 0.0765(15) 0.0352(11) 0.0678(15) -0.0182(10) -0.0339(12) 0.0027(10) C89 0.0393(11) 0.0731(15) 0.0511(13) -0.0328(11) -0.0121(9) 0.0167(10) C90 0.0391(10) 0.0402(10) 0.0419(10) -0.0213(9) -0.0172(8) 0.0027(8) C91 0.0614(13) 0.0394(11) 0.0555(13) -0.0214(10) -0.0270(10) 0.0027(9) C92 0.0473(12) 0.0597(13) 0.0554(13) -0.0285(11) 0.0030(10) -0.0033(10) C93 0.0319(9) 0.0177(7) 0.0246(8) -0.0068(6) -0.0088(7) -0.0008(6) C94 0.0385(9) 0.0190(8) 0.0246(8) -0.0064(6) -0.0081(7) 0.0017(7) C95 0.0482(11) 0.0294(9) 0.0256(9) -0.0103(7) -0.0111(8) 0.0064(8) C96 0.0543(12) 0.0323(9) 0.0343(10) -0.0127(8) -0.0240(9) 0.0066(8) C97 0.0382(10) 0.0277(9) 0.0442(11) -0.0127(8) -0.0204(8) 0.0030(7) C98 0.0312(9) 0.0206(8) 0.0322(9) -0.0087(7) -0.0103(7) -0.0008(6) C99 0.0259(8) 0.0333(9) 0.0411(10) -0.0157(8) -0.0075(7) -0.0029(7) C100 0.0352(10) 0.0486(12) 0.0559(12) -0.0215(10) -0.0021(9) -0.0129(9) C101 0.0325(10) 0.0457(11) 0.0657(13) -0.0298(10) -0.0179(9) 0.0079(8) C102 0.0341(9) 0.0303(9) 0.0253(8) -0.0108(7) -0.0023(7) -0.0004(7) C103 0.0391(10) 0.0416(10) 0.0385(10) -0.0191(9) -0.0019(8) 0.0036(8) C104 0.0473(12) 0.0423(11) 0.0438(11) -0.0074(9) 0.0003(9) -0.0094(9) O1 0.073(2) 0.081(2) 0.0372(17) -0.0138(16) -0.0093(15) -0.0097(18) C105 0.069(6) 0.079(6) 0.055(6) -0.007(4) -0.012(4) 0.017(5) C106 0.070(4) 0.073(4) 0.064(4) 0.006(3) -0.031(4) -0.009(4) C107 0.063(4) 0.075(4) 0.043(6) -0.015(4) -0.004(4) -0.029(4) C108 0.078(4) 0.115(5) 0.036(3) -0.018(3) -0.006(3) -0.029(4) _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 N2 1.7243(13) . ? P1 N1 1.7502(13) . ? P1 P2 2.3397(6) . ? P2 N3 1.7239(13) . ? P2 N4 1.7420(13) . ? P3 N5 1.7228(13) . ? P3 N6 1.7445(13) . ? P3 P4 2.3290(5) . ? P4 N7 1.7190(13) . ? P4 N8 1.7370(12) . ? N1 C1 1.4014(19) . ? N1 C3 1.4382(19) . ? N2 C2 1.430(2) . ? N2 C15 1.4577(19) . ? N3 C27 1.423(2) . ? N3 C29 1.451(2) . ? N4 C28 1.405(2) . ? N4 C41 1.436(2) . ? N5 C53 1.426(2) . ? N5 C55 1.4544(19) . ? N6 C54 1.405(2) . ? N6 C67 1.4308(19) . ? N7 C79 1.426(2) . ? N7 C81 1.447(2) . ? N8 C80 1.405(2) . ? N8 C93 1.4347(19) . ? C1 C2 1.329(2) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C8 1.408(2) . ? C3 C4 1.409(2) . ? C4 C5 1.394(2) . ? C4 C12 1.526(2) . ? C5 C6 1.375(3) . ? C5 H5 0.9500 . ? C6 C7 1.379(3) . ? C6 H6 0.9500 . ? C7 C8 1.399(2) . ? C7 H7 0.9500 . ? C8 C9 1.519(2) . ? C9 C11 1.533(3) . ? C9 C10 1.534(3) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.534(2) . ? C12 C13 1.536(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.401(2) . ? C15 C16 1.409(2) . ? C16 C17 1.393(2) . ? C16 C24 1.516(2) . ? C17 C18 1.377(3) . ? C17 H17 0.9500 . ? C18 C19 1.377(3) . ? C18 H18 0.9500 . ? C19 C20 1.395(2) . ? C19 H19 0.9500 . ? C20 C21 1.517(2) . ? C21 C23 1.522(3) . ? C21 C22 1.534(3) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.527(3) . ? C24 C25 1.533(3) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.328(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.405(2) . ? C29 C34 1.407(2) . ? C30 C31 1.394(2) . ? C30 C38 1.512(2) . ? C31 C32 1.378(3) . ? C31 H31 0.9500 . ? C32 C33 1.378(3) . ? C32 H32 0.9500 . ? C33 C34 1.390(2) . ? C33 H33 0.9500 . ? C34 C35 1.518(2) . ? C35 C36 1.530(3) . ? C35 C37 1.533(2) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.524(3) . ? C38 C40 1.531(3) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.409(2) . ? C41 C46 1.411(2) . ? C42 C43 1.392(3) . ? C42 C50 1.521(2) . ? C43 C44 1.373(3) . ? C43 H43 0.9500 . ? C44 C45 1.380(3) . ? C44 H44 0.9500 . ? C45 C46 1.389(3) . ? C45 H45 0.9500 . ? C46 C47 1.517(3) . ? C47 C48 1.535(3) . ? C47 C49 1.536(3) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C52 1.525(3) . ? C50 C51 1.529(3) . ? C50 H50 1.0000 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.329(2) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.405(2) . ? C55 C56 1.410(2) . ? C56 C57 1.391(2) . ? C56 C64 1.517(2) . ? C57 C58 1.379(3) . ? C57 H57 0.9500 . ? C58 C59 1.374(3) . ? C58 H58 0.9500 . ? C59 C60 1.395(2) . ? C59 H59 0.9500 . ? C60 C61 1.518(2) . ? C61 C62 1.525(3) . ? C61 C63 1.537(3) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C66 1.528(3) . ? C64 C65 1.530(2) . ? C64 H64 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C72 1.409(2) . ? C67 C68 1.414(2) . ? C68 C69 1.392(2) . ? C68 C76 1.516(2) . ? C69 C70 1.377(3) . ? C69 H69 0.9500 . ? C70 C71 1.372(3) . ? C70 H70 0.9500 . ? C71 C72 1.395(2) . ? C71 H71 0.9500 . ? C72 C73 1.522(3) . ? C73 C74 1.532(3) . ? C73 C75 1.534(3) . ? C73 H73 1.0000 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C78 1.531(3) . ? C76 C77 1.531(3) . ? C76 H76 1.0000 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C80 1.329(2) . ? C79 H79 0.9500 . ? C80 H80 0.9500 . ? C81 C86 1.404(2) . ? C81 C82 1.407(2) . ? C82 C83 1.395(2) . ? C82 C90 1.515(2) . ? C83 C84 1.378(3) . ? C83 H83 0.9500 . ? C84 C85 1.381(3) . ? C84 H84 0.9500 . ? C85 C86 1.392(2) . ? C85 H85 0.9500 . ? C86 C87 1.521(2) . ? C87 C88 1.531(3) . ? C87 C89 1.532(3) . ? C87 H87 1.0000 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 C91 1.527(3) . ? C90 C92 1.528(3) . ? C90 H90 1.0000 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 C94 1.410(2) . ? C93 C98 1.410(2) . ? C94 C95 1.394(2) . ? C94 C102 1.521(2) . ? C95 C96 1.376(3) . ? C95 H95 0.9500 . ? C96 C97 1.382(3) . ? C96 H96 0.9500 . ? C97 C98 1.394(2) . ? C97 H97 0.9500 . ? C98 C99 1.525(2) . ? C99 C100 1.529(2) . ? C99 C101 1.534(2) . ? C99 H99 1.0000 . ? C100 H10D 0.9800 . ? C100 H10E 0.9800 . ? C100 H10F 0.9800 . ? C101 H10G 0.9800 . ? C101 H10H 0.9800 . ? C101 H10I 0.9800 . ? C102 C103 1.533(2) . ? C102 C104 1.533(2) . ? C102 H102 1.0000 . ? C103 H10K 0.9800 . ? C103 H10L 0.9800 . ? C103 H10M 0.9800 . ? C104 H10N 0.9800 . ? C104 H10O 0.9800 . ? C104 H10P 0.9800 . ? O1 C108 1.392(6) . ? O1 C105 1.404(11) . ? C105 C106 1.503(11) . ? C105 H10Q 0.9900 . ? C105 H10R 0.9900 . ? C106 C107 1.529(13) . ? C106 H10S 0.9900 . ? C106 H10T 0.9900 . ? C107 C108 1.494(10) . ? C107 H10U 0.9900 . ? C107 H10W 0.9900 . ? C108 H10V 0.9900 . ? C108 H10Y 0.9900 . ? 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 N2 P1 N1 90.85(6) . . ? N2 P1 P2 115.52(5) . . ? N1 P1 P2 94.04(5) . . ? N3 P2 N4 91.16(6) . . ? N3 P2 P1 112.78(5) . . ? N4 P2 P1 98.39(5) . . ? N5 P3 N6 90.96(6) . . ? N5 P3 P4 115.55(5) . . ? N6 P3 P4 96.76(5) . . ? N7 P4 N8 90.68(6) . . ? N7 P4 P3 114.96(5) . . ? N8 P4 P3 95.88(4) . . ? C1 N1 C3 124.37(12) . . ? C1 N1 P1 110.02(10) . . ? C3 N1 P1 123.72(10) . . ? C2 N2 C15 117.18(12) . . ? C2 N2 P1 109.88(10) . . ? C15 N2 P1 121.68(10) . . ? C27 N3 C29 118.32(13) . . ? C27 N3 P2 109.32(10) . . ? C29 N3 P2 122.43(10) . . ? C28 N4 C41 124.15(13) . . ? C28 N4 P2 109.61(10) . . ? C41 N4 P2 124.63(10) . . ? C53 N5 C55 118.01(12) . . ? C53 N5 P3 109.88(10) . . ? C55 N5 P3 121.11(10) . . ? C54 N6 C67 123.69(12) . . ? C54 N6 P3 109.87(10) . . ? C67 N6 P3 124.77(10) . . ? C79 N7 C81 119.23(13) . . ? C79 N7 P4 110.28(10) . . ? C81 N7 P4 120.97(10) . . ? C80 N8 C93 123.99(12) . . ? C80 N8 P4 110.20(10) . . ? C93 N8 P4 124.33(10) . . ? C2 C1 N1 114.02(14) . . ? C2 C1 H1 123.0 . . ? N1 C1 H1 123.0 . . ? C1 C2 N2 113.71(14) . . ? C1 C2 H2 123.1 . . ? N2 C2 H2 123.1 . . ? C8 C3 C4 120.74(14) . . ? C8 C3 N1 118.58(14) . . ? C4 C3 N1 120.67(14) . . ? C5 C4 C3 118.14(15) . . ? C5 C4 C12 117.77(15) . . ? C3 C4 C12 124.07(14) . . ? C6 C5 C4 121.77(16) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 119.65(16) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C8 121.33(16) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C3 118.30(16) . . ? C7 C8 C9 118.80(15) . . ? C3 C8 C9 122.89(15) . . ? C8 C9 C11 111.20(16) . . ? C8 C9 C10 111.92(16) . . ? C11 C9 C10 110.75(18) . . ? C8 C9 H9 107.6 . . ? C11 C9 H9 107.6 . . ? C10 C9 H9 107.6 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 C14 112.07(14) . . ? C4 C12 C13 111.10(14) . . ? C14 C12 C13 109.66(14) . . ? C4 C12 H12 108.0 . . ? C14 C12 H12 108.0 . . ? C13 C12 H12 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 120.45(14) . . ? C20 C15 N2 119.13(14) . . ? C16 C15 N2 120.37(14) . . ? C17 C16 C15 118.48(15) . . ? C17 C16 C24 118.26(15) . . ? C15 C16 C24 123.26(14) . . ? C18 C17 C16 121.40(16) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 119.71(16) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 121.24(17) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C19 C20 C15 118.69(15) . . ? C19 C20 C21 118.14(15) . . ? C15 C20 C21 123.16(14) . . ? C20 C21 C23 110.41(16) . . ? C20 C21 C22 111.07(16) . . ? C23 C21 C22 109.94(17) . . ? C20 C21 H21 108.5 . . ? C23 C21 H21 108.5 . . ? C22 C21 H21 108.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C16 C24 C26 111.14(15) . . ? C16 C24 C25 111.21(15) . . ? C26 C24 C25 110.62(16) . . ? C16 C24 H24 107.9 . . ? C26 C24 H24 107.9 . . ? C25 C24 H24 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 N3 114.13(14) . . ? C28 C27 H27 122.9 . . ? N3 C27 H27 122.9 . . ? C27 C28 N4 113.75(14) . . ? C27 C28 H28 123.1 . . ? N4 C28 H28 123.1 . . ? C30 C29 C34 120.80(15) . . ? C30 C29 N3 118.71(14) . . ? C34 C29 N3 120.46(14) . . ? C31 C30 C29 118.25(15) . . ? C31 C30 C38 119.49(15) . . ? C29 C30 C38 121.97(15) . . ? C32 C31 C30 121.40(17) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C31 C32 C33 119.72(17) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 121.42(16) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C29 118.38(15) . . ? C33 C34 C35 118.85(15) . . ? C29 C34 C35 122.75(14) . . ? C34 C35 C36 110.35(15) . . ? C34 C35 C37 111.67(14) . . ? C36 C35 C37 110.85(15) . . ? C34 C35 H35 107.9 . . ? C36 C35 H35 107.9 . . ? C37 C35 H35 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C30 C38 C39 114.05(16) . . ? C30 C38 C40 108.04(16) . . ? C39 C38 C40 110.74(16) . . ? C30 C38 H38 107.9 . . ? C39 C38 H38 107.9 . . ? C40 C38 H38 107.9 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 120.55(15) . . ? C42 C41 N4 119.20(14) . . ? C46 C41 N4 120.25(15) . . ? C43 C42 C41 118.17(17) . . ? C43 C42 C50 118.23(16) . . ? C41 C42 C50 123.61(15) . . ? C44 C43 C42 121.83(19) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C43 C44 C45 119.44(18) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C44 C45 C46 121.63(18) . . ? C44 C45 H45 119.2 . . ? C46 C45 H45 119.2 . . ? C45 C46 C41 118.25(17) . . ? C45 C46 C47 118.28(16) . . ? C41 C46 C47 123.46(15) . . ? C46 C47 C48 112.33(17) . . ? C46 C47 C49 111.38(15) . . ? C48 C47 C49 109.95(16) . . ? C46 C47 H47 107.7 . . ? C48 C47 H47 107.7 . . ? C49 C47 H47 107.7 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C42 C50 C52 111.40(16) . . ? C42 C50 C51 111.38(15) . . ? C52 C50 C51 110.72(17) . . ? C42 C50 H50 107.7 . . ? C52 C50 H50 107.7 . . ? C51 C50 H50 107.7 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 N5 113.74(14) . . ? C54 C53 H53 123.1 . . ? N5 C53 H53 123.1 . . ? C53 C54 N6 113.91(14) . . ? C53 C54 H54 123.0 . . ? N6 C54 H54 123.0 . . ? C60 C55 C56 121.09(14) . . ? C60 C55 N5 118.64(14) . . ? C56 C55 N5 120.26(14) . . ? C57 C56 C55 118.02(15) . . ? C57 C56 C64 118.55(15) . . ? C55 C56 C64 123.43(14) . . ? C58 C57 C56 121.53(17) . . ? C58 C57 H57 119.2 . . ? C56 C57 H57 119.2 . . ? C59 C58 C57 119.74(16) . . ? C59 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? C58 C59 C60 121.60(17) . . ? C58 C59 H59 119.2 . . ? C60 C59 H59 119.2 . . ? C59 C60 C55 117.97(16) . . ? C59 C60 C61 118.55(15) . . ? C55 C60 C61 123.36(14) . . ? C60 C61 C62 112.99(15) . . ? C60 C61 C63 108.68(15) . . ? C62 C61 C63 110.04(16) . . ? C60 C61 H61 108.3 . . ? C62 C61 H61 108.3 . . ? C63 C61 H61 108.3 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C56 C64 C66 112.28(14) . . ? C56 C64 C65 111.30(14) . . ? C66 C64 C65 110.13(16) . . ? C56 C64 H64 107.6 . . ? C66 C64 H64 107.6 . . ? C65 C64 H64 107.6 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C72 C67 C68 120.86(15) . . ? C72 C67 N6 120.07(15) . . ? C68 C67 N6 119.07(14) . . ? C69 C68 C67 117.84(16) . . ? C69 C68 C76 119.32(16) . . ? C67 C68 C76 122.83(14) . . ? C70 C69 C68 121.66(18) . . ? C70 C69 H69 119.2 . . ? C68 C69 H69 119.2 . . ? C71 C70 C69 119.89(17) . . ? C71 C70 H70 120.1 . . ? C69 C70 H70 120.1 . . ? C70 C71 C72 121.53(18) . . ? C70 C71 H71 119.2 . . ? C72 C71 H71 119.2 . . ? C71 C72 C67 118.07(17) . . ? C71 C72 C73 118.26(16) . . ? C67 C72 C73 123.64(15) . . ? C72 C73 C74 112.04(17) . . ? C72 C73 C75 111.46(15) . . ? C74 C73 C75 109.86(16) . . ? C72 C73 H73 107.8 . . ? C74 C73 H73 107.8 . . ? C75 C73 H73 107.8 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C68 C76 C78 111.66(14) . . ? C68 C76 C77 112.41(16) . . ? C78 C76 C77 109.79(16) . . ? C68 C76 H76 107.6 . . ? C78 C76 H76 107.6 . . ? C77 C76 H76 107.6 . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C80 C79 N7 113.28(14) . . ? C80 C79 H79 123.4 . . ? N7 C79 H79 123.4 . . ? C79 C80 N8 113.73(14) . . ? C79 C80 H80 123.1 . . ? N8 C80 H80 123.1 . . ? C86 C81 C82 121.12(14) . . ? C86 C81 N7 120.60(14) . . ? C82 C81 N7 118.27(14) . . ? C83 C82 C81 118.13(15) . . ? C83 C82 C90 119.83(15) . . ? C81 C82 C90 121.91(14) . . ? C84 C83 C82 121.36(16) . . ? C84 C83 H83 119.3 . . ? C82 C83 H83 119.3 . . ? C83 C84 C85 119.76(16) . . ? C83 C84 H84 120.1 . . ? C85 C84 H84 120.1 . . ? C84 C85 C86 121.43(16) . . ? C84 C85 H85 119.3 . . ? C86 C85 H85 119.3 . . ? C85 C86 C81 118.20(15) . . ? C85 C86 C87 118.57(15) . . ? C81 C86 C87 123.23(14) . . ? C86 C87 C88 110.84(15) . . ? C86 C87 C89 111.19(15) . . ? C88 C87 C89 110.84(16) . . ? C86 C87 H87 107.9 . . ? C88 C87 H87 107.9 . . ? C89 C87 H87 107.9 . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C87 C89 H89A 109.5 . . ? C87 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C87 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C82 C90 C91 113.25(16) . . ? C82 C90 C92 109.03(15) . . ? C91 C90 C92 110.03(15) . . ? C82 C90 H90 108.1 . . ? C91 C90 H90 108.1 . . ? C92 C90 H90 108.1 . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C90 C92 H92A 109.5 . . ? C90 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C90 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C94 C93 C98 120.82(14) . . ? C94 C93 N8 119.03(14) . . ? C98 C93 N8 120.15(13) . . ? C95 C94 C93 118.22(15) . . ? C95 C94 C102 118.19(14) . . ? C93 C94 C102 123.59(14) . . ? C96 C95 C94 121.51(16) . . ? C96 C95 H95 119.2 . . ? C94 C95 H95 119.2 . . ? C95 C96 C97 119.72(16) . . ? C95 C96 H96 120.1 . . ? C97 C96 H96 120.1 . . ? C96 C97 C98 121.50(16) . . ? C96 C97 H97 119.3 . . ? C98 C97 H97 119.3 . . ? C97 C98 C93 118.01(15) . . ? C97 C98 C99 118.42(15) . . ? C93 C98 C99 123.53(14) . . ? C98 C99 C100 112.29(14) . . ? C98 C99 C101 111.28(15) . . ? C100 C99 C101 109.67(15) . . ? C98 C99 H99 107.8 . . ? C100 C99 H99 107.8 . . ? C101 C99 H99 107.8 . . ? C99 C100 H10D 109.5 . . ? C99 C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? C99 C100 H10F 109.5 . . ? H10D C100 H10F 109.5 . . ? H10E C100 H10F 109.5 . . ? C99 C101 H10G 109.5 . . ? C99 C101 H10H 109.5 . . ? H10G C101 H10H 109.5 . . ? C99 C101 H10I 109.5 . . ? H10G C101 H10I 109.5 . . ? H10H C101 H10I 109.5 . . ? C94 C102 C103 111.79(14) . . ? C94 C102 C104 111.27(14) . . ? C103 C102 C104 110.36(14) . . ? C94 C102 H102 107.7 . . ? C103 C102 H102 107.7 . . ? C104 C102 H102 107.7 . . ? C102 C103 H10K 109.5 . . ? C102 C103 H10L 109.5 . . ? H10K C103 H10L 109.5 . . ? C102 C103 H10M 109.5 . . ? H10K C103 H10M 109.5 . . ? H10L C103 H10M 109.5 . . ? C102 C104 H10N 109.5 . . ? C102 C104 H10O 109.5 . . ? H10N C104 H10O 109.5 . . ? C102 C104 H10P 109.5 . . ? H10N C104 H10P 109.5 . . ? H10O C104 H10P 109.5 . . ? C108 O1 C105 105.6(7) . . ? O1 C105 C106 105.9(9) . . ? O1 C105 H10Q 110.5 . . ? C106 C105 H10Q 110.5 . . ? O1 C105 H10R 110.5 . . ? C106 C105 H10R 110.5 . . ? H10Q C105 H10R 108.7 . . ? C105 C106 C107 103.6(8) . . ? C105 C106 H10S 111.0 . . ? C107 C106 H10S 111.0 . . ? C105 C106 H10T 111.0 . . ? C107 C106 H10T 111.0 . . ? H10S C106 H10T 109.0 . . ? C108 C107 C106 102.9(8) . . ? C108 C107 H10U 111.2 . . ? C106 C107 H10U 111.2 . . ? C108 C107 H10W 111.2 . . ? C106 C107 H10W 111.2 . . ? H10U C107 H10W 109.1 . . ? O1 C108 C107 109.2(7) . . ? O1 C108 H10V 109.8 . . ? C107 C108 H10V 109.8 . . ? O1 C108 H10Y 109.8 . . ? C107 C108 H10Y 109.8 . . ? H10V C108 H10Y 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 P1 P2 N3 -13.95(7) . . . . ? N1 P1 P2 N3 -106.83(6) . . . . ? N2 P1 P2 N4 -108.78(7) . . . . ? N1 P1 P2 N4 158.34(6) . . . . ? N5 P3 P4 N7 14.30(7) . . . . ? N6 P3 P4 N7 108.62(6) . . . . ? N5 P3 P4 N8 107.81(7) . . . . ? N6 P3 P4 N8 -157.87(6) . . . . ? N2 P1 N1 C1 -11.24(11) . . . . ? P2 P1 N1 C1 104.42(10) . . . . ? N2 P1 N1 C3 -176.15(12) . . . . ? P2 P1 N1 C3 -60.50(12) . . . . ? N1 P1 N2 C2 10.70(11) . . . . ? P2 P1 N2 C2 -84.19(10) . . . . ? N1 P1 N2 C15 -131.86(12) . . . . ? P2 P1 N2 C15 133.26(10) . . . . ? N4 P2 N3 C27 12.31(11) . . . . ? P1 P2 N3 C27 -87.30(10) . . . . ? N4 P2 N3 C29 -132.62(12) . . . . ? P1 P2 N3 C29 127.77(11) . . . . ? N3 P2 N4 C28 -13.03(11) . . . . ? P1 P2 N4 C28 100.21(10) . . . . ? N3 P2 N4 C41 -178.99(13) . . . . ? P1 P2 N4 C41 -65.76(12) . . . . ? N6 P3 N5 C53 -11.03(11) . . . . ? P4 P3 N5 C53 86.92(10) . . . . ? N6 P3 N5 C55 132.25(12) . . . . ? P4 P3 N5 C55 -129.80(11) . . . . ? N5 P3 N6 C54 11.72(11) . . . . ? P4 P3 N6 C54 -104.15(10) . . . . ? N5 P3 N6 C67 177.40(13) . . . . ? P4 P3 N6 C67 61.54(13) . . . . ? N8 P4 N7 C79 -11.61(11) . . . . ? P3 P4 N7 C79 85.20(10) . . . . ? N8 P4 N7 C81 134.39(12) . . . . ? P3 P4 N7 C81 -128.81(10) . . . . ? N7 P4 N8 C80 12.44(11) . . . . ? P3 P4 N8 C80 -102.74(10) . . . . ? N7 P4 N8 C93 178.97(12) . . . . ? P3 P4 N8 C93 63.78(12) . . . . ? C3 N1 C1 C2 173.79(14) . . . . ? P1 N1 C1 C2 9.00(17) . . . . ? N1 C1 C2 N2 -0.9(2) . . . . ? C15 N2 C2 C1 136.64(15) . . . . ? P1 N2 C2 C1 -7.80(17) . . . . ? C1 N1 C3 C8 129.71(16) . . . . ? P1 N1 C3 C8 -67.52(18) . . . . ? C1 N1 C3 C4 -51.5(2) . . . . ? P1 N1 C3 C4 111.26(14) . . . . ? C8 C3 C4 C5 -1.9(2) . . . . ? N1 C3 C4 C5 179.38(14) . . . . ? C8 C3 C4 C12 176.56(15) . . . . ? N1 C3 C4 C12 -2.2(2) . . . . ? C3 C4 C5 C6 2.7(2) . . . . ? C12 C4 C5 C6 -175.84(15) . . . . ? C4 C5 C6 C7 -1.3(3) . . . . ? C5 C6 C7 C8 -1.1(3) . . . . ? C6 C7 C8 C3 1.8(3) . . . . ? C6 C7 C8 C9 -178.70(16) . . . . ? C4 C3 C8 C7 -0.3(2) . . . . ? N1 C3 C8 C7 178.47(14) . . . . ? C4 C3 C8 C9 -179.79(15) . . . . ? N1 C3 C8 C9 -1.0(2) . . . . ? C7 C8 C9 C11 -74.3(2) . . . . ? C3 C8 C9 C11 105.21(19) . . . . ? C7 C8 C9 C10 50.2(2) . . . . ? C3 C8 C9 C10 -130.34(19) . . . . ? C5 C4 C12 C14 47.26(19) . . . . ? C3 C4 C12 C14 -131.17(16) . . . . ? C5 C4 C12 C13 -75.80(18) . . . . ? C3 C4 C12 C13 105.77(17) . . . . ? C2 N2 C15 C20 109.89(16) . . . . ? P1 N2 C15 C20 -110.10(15) . . . . ? C2 N2 C15 C16 -67.33(19) . . . . ? P1 N2 C15 C16 72.68(17) . . . . ? C20 C15 C16 C17 1.4(2) . . . . ? N2 C15 C16 C17 178.56(14) . . . . ? C20 C15 C16 C24 -178.41(15) . . . . ? N2 C15 C16 C24 -1.2(2) . . . . ? C15 C16 C17 C18 0.1(3) . . . . ? C24 C16 C17 C18 179.90(16) . . . . ? C16 C17 C18 C19 -0.8(3) . . . . ? C17 C18 C19 C20 0.1(3) . . . . ? C18 C19 C20 C15 1.3(3) . . . . ? C18 C19 C20 C21 -177.89(17) . . . . ? C16 C15 C20 C19 -2.1(2) . . . . ? N2 C15 C20 C19 -179.30(14) . . . . ? C16 C15 C20 C21 177.11(16) . . . . ? N2 C15 C20 C21 -0.1(2) . . . . ? C19 C20 C21 C23 -64.4(2) . . . . ? C15 C20 C21 C23 116.36(18) . . . . ? C19 C20 C21 C22 57.8(2) . . . . ? C15 C20 C21 C22 -121.42(19) . . . . ? C17 C16 C24 C26 56.6(2) . . . . ? C15 C16 C24 C26 -123.61(18) . . . . ? C17 C16 C24 C25 -67.1(2) . . . . ? C15 C16 C24 C25 112.67(18) . . . . ? C29 N3 C27 C28 137.75(15) . . . . ? P2 N3 C27 C28 -8.82(17) . . . . ? N3 C27 C28 N4 -1.2(2) . . . . ? C41 N4 C28 C27 176.56(14) . . . . ? P2 N4 C28 C27 10.51(17) . . . . ? C27 N3 C29 C30 111.50(17) . . . . ? P2 N3 C29 C30 -106.52(15) . . . . ? C27 N3 C29 C34 -66.5(2) . . . . ? P2 N3 C29 C34 75.51(18) . . . . ? C34 C29 C30 C31 -2.1(2) . . . . ? N3 C29 C30 C31 179.97(15) . . . . ? C34 C29 C30 C38 171.72(16) . . . . ? N3 C29 C30 C38 -6.2(2) . . . . ? C29 C30 C31 C32 2.0(3) . . . . ? C38 C30 C31 C32 -171.91(18) . . . . ? C30 C31 C32 C33 -0.4(3) . . . . ? C31 C32 C33 C34 -1.3(3) . . . . ? C32 C33 C34 C29 1.2(3) . . . . ? C32 C33 C34 C35 179.54(17) . . . . ? C30 C29 C34 C33 0.5(2) . . . . ? N3 C29 C34 C33 178.40(15) . . . . ? C30 C29 C34 C35 -177.76(15) . . . . ? N3 C29 C34 C35 0.2(2) . . . . ? C33 C34 C35 C36 -71.3(2) . . . . ? C29 C34 C35 C36 106.90(18) . . . . ? C33 C34 C35 C37 52.4(2) . . . . ? C29 C34 C35 C37 -129.33(17) . . . . ? C31 C30 C38 C39 -42.8(2) . . . . ? C29 C30 C38 C39 143.44(17) . . . . ? C31 C30 C38 C40 80.7(2) . . . . ? C29 C30 C38 C40 -93.0(2) . . . . ? C28 N4 C41 C42 128.53(16) . . . . ? P2 N4 C41 C42 -67.50(18) . . . . ? C28 N4 C41 C46 -51.6(2) . . . . ? P2 N4 C41 C46 112.32(15) . . . . ? C46 C41 C42 C43 0.5(2) . . . . ? N4 C41 C42 C43 -179.69(15) . . . . ? C46 C41 C42 C50 -179.89(15) . . . . ? N4 C41 C42 C50 -0.1(2) . . . . ? C41 C42 C43 C44 2.2(3) . . . . ? C50 C42 C43 C44 -177.46(18) . . . . ? C42 C43 C44 C45 -2.0(3) . . . . ? C43 C44 C45 C46 -1.0(3) . . . . ? C44 C45 C46 C41 3.5(3) . . . . ? C44 C45 C46 C47 -175.84(18) . . . . ? C42 C41 C46 C45 -3.3(2) . . . . ? N4 C41 C46 C45 176.93(15) . . . . ? C42 C41 C46 C47 176.07(16) . . . . ? N4 C41 C46 C47 -3.7(2) . . . . ? C45 C46 C47 C48 52.2(2) . . . . ? C41 C46 C47 C48 -127.13(18) . . . . ? C45 C46 C47 C49 -71.6(2) . . . . ? C41 C46 C47 C49 109.03(19) . . . . ? C43 C42 C50 C52 -67.2(2) . . . . ? C41 C42 C50 C52 113.16(19) . . . . ? C43 C42 C50 C51 56.9(2) . . . . ? C41 C42 C50 C51 -122.69(19) . . . . ? C55 N5 C53 C54 -136.72(15) . . . . ? P3 N5 C53 C54 7.84(17) . . . . ? N5 C53 C54 N6 1.2(2) . . . . ? C67 N6 C54 C53 -175.42(14) . . . . ? P3 N6 C54 C53 -9.55(17) . . . . ? C53 N5 C55 C60 -108.87(16) . . . . ? P3 N5 C55 C60 110.69(14) . . . . ? C53 N5 C55 C56 69.65(19) . . . . ? P3 N5 C55 C56 -70.79(17) . . . . ? C60 C55 C56 C57 -0.1(2) . . . . ? N5 C55 C56 C57 -178.59(14) . . . . ? C60 C55 C56 C64 179.18(14) . . . . ? N5 C55 C56 C64 0.7(2) . . . . ? C55 C56 C57 C58 -1.8(2) . . . . ? C64 C56 C57 C58 178.90(16) . . . . ? C56 C57 C58 C59 1.9(3) . . . . ? C57 C58 C59 C60 -0.1(3) . . . . ? C58 C59 C60 C55 -1.7(3) . . . . ? C58 C59 C60 C61 174.42(16) . . . . ? C56 C55 C60 C59 1.8(2) . . . . ? N5 C55 C60 C59 -179.70(14) . . . . ? C56 C55 C60 C61 -174.11(15) . . . . ? N5 C55 C60 C61 4.4(2) . . . . ? C59 C60 C61 C62 55.9(2) . . . . ? C55 C60 C61 C62 -128.19(17) . . . . ? C59 C60 C61 C63 -66.5(2) . . . . ? C55 C60 C61 C63 109.38(18) . . . . ? C57 C56 C64 C66 -50.0(2) . . . . ? C55 C56 C64 C66 130.76(16) . . . . ? C57 C56 C64 C65 74.0(2) . . . . ? C55 C56 C64 C65 -105.26(18) . . . . ? C54 N6 C67 C72 51.1(2) . . . . ? P3 N6 C67 C72 -112.68(15) . . . . ? C54 N6 C67 C68 -129.06(16) . . . . ? P3 N6 C67 C68 67.17(18) . . . . ? C72 C67 C68 C69 -1.9(2) . . . . ? N6 C67 C68 C69 178.21(14) . . . . ? C72 C67 C68 C76 176.77(15) . . . . ? N6 C67 C68 C76 -3.1(2) . . . . ? C67 C68 C69 C70 -1.5(3) . . . . ? C76 C68 C69 C70 179.76(18) . . . . ? C68 C69 C70 C71 2.4(3) . . . . ? C69 C70 C71 C72 0.1(3) . . . . ? C70 C71 C72 C67 -3.4(3) . . . . ? C70 C71 C72 C73 174.86(18) . . . . ? C68 C67 C72 C71 4.3(2) . . . . ? N6 C67 C72 C71 -175.87(15) . . . . ? C68 C67 C72 C73 -173.82(15) . . . . ? N6 C67 C72 C73 6.0(2) . . . . ? C71 C72 C73 C74 -50.6(2) . . . . ? C67 C72 C73 C74 127.45(18) . . . . ? C71 C72 C73 C75 72.9(2) . . . . ? C67 C72 C73 C75 -108.98(19) . . . . ? C69 C68 C76 C78 75.8(2) . . . . ? C67 C68 C76 C78 -102.87(18) . . . . ? C69 C68 C76 C77 -48.1(2) . . . . ? C67 C68 C76 C77 133.21(17) . . . . ? C81 N7 C79 C80 -138.58(15) . . . . ? P4 N7 C79 C80 8.09(17) . . . . ? N7 C79 C80 N8 1.49(19) . . . . ? C93 N8 C80 C79 -176.87(14) . . . . ? P4 N8 C80 C79 -10.30(17) . . . . ? C79 N7 C81 C86 68.0(2) . . . . ? P4 N7 C81 C86 -75.06(17) . . . . ? C79 N7 C81 C82 -111.17(16) . . . . ? P4 N7 C81 C82 105.78(15) . . . . ? C86 C81 C82 C83 0.8(2) . . . . ? N7 C81 C82 C83 179.96(15) . . . . ? C86 C81 C82 C90 -175.14(16) . . . . ? N7 C81 C82 C90 4.0(2) . . . . ? C81 C82 C83 C84 -0.5(3) . . . . ? C90 C82 C83 C84 175.49(17) . . . . ? C82 C83 C84 C85 -0.2(3) . . . . ? C83 C84 C85 C86 0.8(3) . . . . ? C84 C85 C86 C81 -0.5(3) . . . . ? C84 C85 C86 C87 179.84(17) . . . . ? C82 C81 C86 C85 -0.3(2) . . . . ? N7 C81 C86 C85 -179.42(15) . . . . ? C82 C81 C86 C87 179.34(15) . . . . ? N7 C81 C86 C87 0.2(2) . . . . ? C85 C86 C87 C88 69.0(2) . . . . ? C81 C86 C87 C88 -110.59(19) . . . . ? C85 C86 C87 C89 -54.7(2) . . . . ? C81 C86 C87 C89 125.65(18) . . . . ? C83 C82 C90 C91 46.8(2) . . . . ? C81 C82 C90 C91 -137.31(17) . . . . ? C83 C82 C90 C92 -76.0(2) . . . . ? C81 C82 C90 C92 99.84(19) . . . . ? C80 N8 C93 C94 -128.67(15) . . . . ? P4 N8 C93 C94 66.63(17) . . . . ? C80 N8 C93 C98 51.6(2) . . . . ? P4 N8 C93 C98 -113.13(14) . . . . ? C98 C93 C94 C95 -3.2(2) . . . . ? N8 C93 C94 C95 177.07(13) . . . . ? C98 C93 C94 C102 177.53(14) . . . . ? N8 C93 C94 C102 -2.2(2) . . . . ? C93 C94 C95 C96 -1.2(2) . . . . ? C102 C94 C95 C96 178.12(15) . . . . ? C94 C95 C96 C97 3.3(3) . . . . ? C95 C96 C97 C98 -0.9(3) . . . . ? C96 C97 C98 C93 -3.3(2) . . . . ? C96 C97 C98 C99 174.50(15) . . . . ? C94 C93 C98 C97 5.4(2) . . . . ? N8 C93 C98 C97 -174.88(14) . . . . ? C94 C93 C98 C99 -172.33(14) . . . . ? N8 C93 C98 C99 7.4(2) . . . . ? C97 C98 C99 C100 71.8(2) . . . . ? C93 C98 C99 C100 -110.52(18) . . . . ? C97 C98 C99 C101 -51.6(2) . . . . ? C93 C98 C99 C101 126.11(16) . . . . ? C95 C94 C102 C103 -54.7(2) . . . . ? C93 C94 C102 C103 124.61(16) . . . . ? C95 C94 C102 C104 69.21(19) . . . . ? C93 C94 C102 C104 -111.49(17) . . . . ? C108 O1 C105 C106 -36.9(11) . . . . ? O1 C105 C106 C107 27.9(16) . . . . ? C105 C106 C107 C108 -9.0(16) . . . . ? C105 O1 C108 C107 31.4(7) . . . . ? C106 C107 C108 O1 -12.9(12) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.301 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.037