# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_monoclinc2c _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-bis(2,6-diisopropylphenyl)-2-phosphinylidene-2,3-dihydro-1H-imidazole ; _chemical_name_common 1,3-bis(2,6-diisopropylphenyl)-2-phosphinylidene-2,3-dihydro-1H-imidazole _chemical_melting_point ? _chemical_formula_moiety 'C27 H37 N2 P' _chemical_formula_sum 'C27 H37 N2 P' _chemical_formula_weight 420.56 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 Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.0613(13) _cell_length_b 6.9855(6) _cell_length_c 38.187(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.741(2) _cell_angle_gamma 90.00 _cell_volume 5219.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9897 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 31.88 _exptl_crystal_description Hexagon _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7053 _exptl_absorpt_correction_T_max 0.7467 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41431 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 31.00 _reflns_number_total 8261 _reflns_number_gt 6513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+0.1200P] 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 8261 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1410 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 C1 C 0.72790(5) 0.63220(15) 0.11893(3) 0.0155(2) Uani 1 1 d . . . C2 C 0.72640(6) 0.94275(16) 0.13666(3) 0.0190(2) Uani 1 1 d . . . C3 C 0.73220(6) 0.83463(16) 0.16620(3) 0.0192(2) Uani 1 1 d . . . C4 C 0.71875(5) 0.88239(15) 0.07135(3) 0.0158(2) Uani 1 1 d . . . C5 C 0.77811(6) 0.94176(16) 0.06077(3) 0.0185(2) Uani 1 1 d . . . C6 C 0.77103(7) 1.00343(18) 0.02541(3) 0.0242(2) Uani 1 1 d . . . C7 C 0.70794(7) 1.00919(18) 0.00208(3) 0.0255(3) Uani 1 1 d . . . H7 H 0.7042 1.0528 -0.0218 0.031 Uiso 1 1 calc R . . C8 C 0.65004(6) 0.95172(19) 0.01333(3) 0.0245(3) Uani 1 1 d . . . C9 C 0.65415(6) 0.88534(17) 0.04810(3) 0.0203(2) Uani 1 1 d . . . C10 C 0.84791(6) 0.93517(19) 0.08638(3) 0.0255(3) Uani 1 1 d . . . C11 C 0.88583(9) 0.7544(3) 0.08049(6) 0.0592(6) Uani 1 1 d . . . H11A H 0.8944 0.7554 0.0562 0.089 Uiso 1 1 calc R . . H11B H 0.8581 0.6424 0.0834 0.089 Uiso 1 1 calc R . . H11C H 0.9295 0.7488 0.0981 0.089 Uiso 1 1 calc R . . C12 C 0.89034(7) 1.1134(2) 0.08362(5) 0.0375(3) Uani 1 1 d . . . H12A H 0.9333 1.1074 0.1018 0.056 Uiso 1 1 calc R . . H12B H 0.8647 1.2276 0.0877 0.056 Uiso 1 1 calc R . . H12C H 0.9003 1.1197 0.0597 0.056 Uiso 1 1 calc R . . C13 C 0.58982(6) 0.8212(2) 0.05984(4) 0.0303(3) Uani 1 1 d . . . C14 C 0.55289(8) 0.6622(3) 0.03545(5) 0.0444(4) Uani 1 1 d . . . H14A H 0.5371 0.7119 0.0110 0.067 Uiso 1 1 calc R . . H14B H 0.5135 0.6179 0.0445 0.067 Uiso 1 1 calc R . . H14C H 0.5843 0.5552 0.0352 0.067 Uiso 1 1 calc R . . C15 C 0.54296(7) 0.9912(3) 0.06132(4) 0.0438(4) Uani 1 1 d . . . H15A H 0.5688 1.0928 0.0760 0.066 Uiso 1 1 calc R . . H15B H 0.5049 0.9508 0.0719 0.066 Uiso 1 1 calc R . . H15C H 0.5250 1.0394 0.0370 0.066 Uiso 1 1 calc R . . C16 C 0.74444(5) 0.48565(14) 0.17969(3) 0.01334(19) Uani 1 1 d . . . C17 C 0.81220(5) 0.44391(16) 0.19683(3) 0.0160(2) Uani 1 1 d . . . C18 C 0.82268(6) 0.30288(17) 0.22333(3) 0.0203(2) Uani 1 1 d . . . C19 C 0.76801(6) 0.20583(16) 0.23175(3) 0.0203(2) Uani 1 1 d . . . H19 H 0.7760 0.1125 0.2503 0.024 Uiso 1 1 calc R . . C20 C 0.70176(6) 0.24408(16) 0.21323(3) 0.0181(2) Uani 1 1 d . . . C21 C 0.68838(5) 0.38512(15) 0.18672(3) 0.0149(2) Uani 1 1 d . . . C22 C 0.61595(6) 0.43104(19) 0.16689(3) 0.0229(2) Uani 1 1 d . . . C23 C 0.58390(7) 0.5814(3) 0.18721(4) 0.0409(4) Uani 1 1 d . . . H23A H 0.5814 0.5311 0.2108 0.061 Uiso 1 1 calc R . . H23B H 0.5378 0.6119 0.1736 0.061 Uiso 1 1 calc R . . H23C H 0.6120 0.6976 0.1902 0.061 Uiso 1 1 calc R . . C24 C 0.57080(7) 0.2521(2) 0.16023(4) 0.0390(3) Uani 1 1 d . . . H24A H 0.5926 0.1551 0.1480 0.058 Uiso 1 1 calc R . . H24B H 0.5261 0.2857 0.1452 0.058 Uiso 1 1 calc R . . H24C H 0.5648 0.2011 0.1832 0.058 Uiso 1 1 calc R . . C25 C 0.87236(6) 0.54484(19) 0.18668(3) 0.0235(2) Uani 1 1 d . . . C26 C 0.92348(8) 0.4010(2) 0.17813(5) 0.0427(4) Uani 1 1 d . . . H26A H 0.9578 0.4683 0.1681 0.064 Uiso 1 1 calc R . . H26B H 0.8995 0.3076 0.1607 0.064 Uiso 1 1 calc R . . H26C H 0.9460 0.3346 0.2002 0.064 Uiso 1 1 calc R . . C27 C 0.90650(7) 0.6857(3) 0.21589(4) 0.0400(4) Uani 1 1 d . . . H27A H 0.9252 0.6155 0.2381 0.060 Uiso 1 1 calc R . . H27B H 0.8726 0.7788 0.2202 0.060 Uiso 1 1 calc R . . H27C H 0.9435 0.7530 0.2081 0.060 Uiso 1 1 calc R . . H2 H 0.7228(8) 1.077(3) 0.1325(5) 0.040(5) Uiso 1 1 d . . . H3 H 0.7357(7) 0.866(2) 0.1901(4) 0.022(3) Uiso 1 1 d . . . H8 H 0.6089(8) 0.952(2) -0.0023(5) 0.036(4) Uiso 1 1 d . . . H9 H 0.8093(8) 1.042(3) 0.0174(5) 0.044(5) Uiso 1 1 d . . . H10 H 0.8429(8) 0.932(3) 0.1115(5) 0.045(5) Uiso 1 1 d . . . H13 H 0.6035(8) 0.768(2) 0.0837(4) 0.033(4) Uiso 1 1 d . . . H18 H 0.8699(7) 0.275(2) 0.2356(4) 0.029(4) Uiso 1 1 d . . . H20 H 0.6641(8) 0.163(2) 0.2189(4) 0.029(4) Uiso 1 1 d . . . H22 H 0.6190(7) 0.484(2) 0.1437(4) 0.031(4) Uiso 1 1 d . . . H25 H 0.8552(8) 0.621(2) 0.1635(4) 0.030(4) Uiso 1 1 d . . . N1 N 0.72407(5) 0.81939(13) 0.10765(2) 0.01581(19) Uani 1 1 d . . . N2 N 0.73244(5) 0.64396(13) 0.15527(2) 0.01594(18) Uani 1 1 d . . . P1 P 0.726687(18) 0.41623(4) 0.095495(8) 0.02321(10) Uani 1 1 d . . . H1P H 0.7195(7) 0.498(2) 0.0641(4) 0.033(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0229(5) 0.0117(5) 0.0121(5) 0.0022(4) 0.0042(4) 0.0026(4) C2 0.0306(6) 0.0110(5) 0.0164(5) 0.0006(4) 0.0072(4) 0.0035(4) C3 0.0324(6) 0.0119(5) 0.0140(5) -0.0012(4) 0.0068(4) 0.0028(4) C4 0.0233(5) 0.0118(4) 0.0130(5) 0.0034(4) 0.0055(4) 0.0022(4) C5 0.0234(5) 0.0155(5) 0.0169(5) -0.0005(4) 0.0052(4) -0.0028(4) C6 0.0314(6) 0.0235(6) 0.0199(6) 0.0030(5) 0.0105(5) -0.0061(5) C7 0.0392(7) 0.0239(6) 0.0145(5) 0.0073(4) 0.0081(5) 0.0010(5) C8 0.0266(6) 0.0282(6) 0.0176(6) 0.0073(5) 0.0022(5) 0.0062(5) C9 0.0219(5) 0.0220(5) 0.0176(5) 0.0056(4) 0.0057(4) 0.0051(4) C10 0.0237(5) 0.0304(7) 0.0211(6) -0.0027(5) 0.0020(4) -0.0064(5) C11 0.0447(9) 0.0378(9) 0.0740(13) -0.0155(9) -0.0322(9) 0.0132(7) C12 0.0245(6) 0.0370(8) 0.0515(10) -0.0061(7) 0.0092(6) -0.0112(6) C13 0.0205(5) 0.0466(8) 0.0246(6) 0.0092(6) 0.0068(5) 0.0047(5) C14 0.0310(7) 0.0515(10) 0.0530(10) 0.0036(8) 0.0142(7) -0.0093(7) C15 0.0269(7) 0.0641(11) 0.0412(9) -0.0005(8) 0.0093(6) 0.0151(7) C16 0.0213(5) 0.0099(4) 0.0089(4) 0.0006(3) 0.0037(4) 0.0015(4) C17 0.0179(5) 0.0165(5) 0.0138(5) 0.0007(4) 0.0042(4) 0.0009(4) C18 0.0229(5) 0.0209(5) 0.0161(5) 0.0034(4) 0.0023(4) 0.0059(4) C19 0.0344(6) 0.0132(5) 0.0135(5) 0.0036(4) 0.0061(4) 0.0022(4) C20 0.0279(5) 0.0139(5) 0.0142(5) -0.0014(4) 0.0081(4) -0.0045(4) C21 0.0186(4) 0.0157(5) 0.0103(5) -0.0027(4) 0.0026(4) -0.0009(4) C22 0.0180(5) 0.0326(7) 0.0168(5) -0.0019(5) 0.0010(4) 0.0009(5) C23 0.0250(6) 0.0502(9) 0.0433(9) -0.0140(7) -0.0015(6) 0.0141(6) C24 0.0242(6) 0.0499(9) 0.0395(8) -0.0108(7) -0.0001(6) -0.0117(6) C25 0.0201(5) 0.0296(6) 0.0224(6) 0.0010(5) 0.0081(4) -0.0026(5) C26 0.0331(7) 0.0462(9) 0.0572(10) -0.0054(8) 0.0281(7) 0.0005(6) C27 0.0334(7) 0.0477(9) 0.0426(9) -0.0134(7) 0.0161(6) -0.0186(6) N1 0.0253(4) 0.0112(4) 0.0113(4) 0.0022(3) 0.0049(3) 0.0024(3) N2 0.0268(4) 0.0100(4) 0.0111(4) 0.0014(3) 0.0044(3) 0.0031(3) P1 0.0447(2) 0.01196(15) 0.01414(16) -0.00067(10) 0.00896(13) 0.00231(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.3730(13) . ? C1 N1 1.3735(13) . ? C1 P1 1.7515(11) . ? C2 C3 1.3411(15) . ? C2 N1 1.3960(14) . ? C2 H2 0.954(18) . ? C3 N2 1.3961(14) . ? C3 H3 0.925(15) . ? C4 C9 1.4001(15) . ? C4 C5 1.4020(15) . ? C4 N1 1.4360(13) . ? C5 C6 1.3942(16) . ? C5 C10 1.5216(16) . ? C6 C7 1.3787(18) . ? C6 H9 0.927(17) . ? C7 C8 1.3838(17) . ? C7 H7 0.9500 . ? C8 C9 1.3916(16) . ? C8 H8 0.906(16) . ? C9 C13 1.5239(16) . ? C10 C11 1.516(2) . ? C10 C12 1.5249(18) . ? C10 H10 0.987(18) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.523(2) . ? C13 C14 1.532(2) . ? C13 H13 0.966(16) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.4013(14) . ? C16 C17 1.4031(14) . ? C16 N2 1.4322(13) . ? C17 C18 1.3947(15) . ? C17 C25 1.5200(15) . ? C18 C19 1.3861(16) . ? C18 H18 0.980(15) . ? C19 C20 1.3867(16) . ? C19 H19 0.9500 . ? C20 C21 1.3957(15) . ? C20 H20 1.005(15) . ? C21 C22 1.5173(15) . ? C22 C23 1.5292(19) . ? C22 C24 1.5315(19) . ? C22 H22 0.975(16) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.5216(19) . ? C25 C27 1.5311(19) . ? C25 H25 1.027(16) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? P1 H1P 1.306(16) . ? 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 C1 N1 104.27(9) . . ? N2 C1 P1 123.94(8) . . ? N1 C1 P1 131.79(8) . . ? C3 C2 N1 107.53(10) . . ? C3 C2 H2 133.2(10) . . ? N1 C2 H2 119.2(10) . . ? C2 C3 N2 106.94(10) . . ? C2 C3 H3 132.1(9) . . ? N2 C3 H3 120.9(9) . . ? C9 C4 C5 122.63(10) . . ? C9 C4 N1 118.56(9) . . ? C5 C4 N1 118.81(9) . . ? C6 C5 C4 117.32(11) . . ? C6 C5 C10 120.96(10) . . ? C4 C5 C10 121.70(10) . . ? C7 C6 C5 121.19(11) . . ? C7 C6 H9 119.1(11) . . ? C5 C6 H9 119.7(11) . . ? C6 C7 C8 120.30(11) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 121.06(11) . . ? C7 C8 H8 119.9(11) . . ? C9 C8 H8 118.9(11) . . ? C8 C9 C4 117.49(10) . . ? C8 C9 C13 120.19(11) . . ? C4 C9 C13 122.32(10) . . ? C11 C10 C5 110.52(11) . . ? C11 C10 C12 111.31(13) . . ? C5 C10 C12 112.30(11) . . ? C11 C10 H10 106.6(11) . . ? C5 C10 H10 110.4(10) . . ? C12 C10 H10 105.4(10) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C15 110.56(12) . . ? C9 C13 C14 111.20(11) . . ? C15 C13 C14 111.59(12) . . ? C9 C13 H13 107.9(9) . . ? C15 C13 H13 108.4(10) . . ? C14 C13 H13 107.0(10) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 122.85(9) . . ? C21 C16 N2 119.00(9) . . ? C17 C16 N2 118.08(9) . . ? C18 C17 C16 117.45(10) . . ? C18 C17 C25 120.76(10) . . ? C16 C17 C25 121.78(10) . . ? C19 C18 C17 120.88(10) . . ? C19 C18 H18 121.6(9) . . ? C17 C18 H18 117.6(9) . . ? C18 C19 C20 120.40(10) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 121.02(10) . . ? C19 C20 H20 117.6(9) . . ? C21 C20 H20 121.3(9) . . ? C20 C21 C16 117.30(9) . . ? C20 C21 C22 121.41(10) . . ? C16 C21 C22 121.28(10) . . ? C21 C22 C23 110.83(10) . . ? C21 C22 C24 112.12(11) . . ? C23 C22 C24 110.21(12) . . ? C21 C22 H22 106.8(9) . . ? C23 C22 H22 108.4(10) . . ? C24 C22 H22 108.3(9) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C17 C25 C26 111.05(11) . . ? C17 C25 C27 111.42(10) . . ? C26 C25 C27 111.49(12) . . ? C17 C25 H25 109.1(8) . . ? C26 C25 H25 105.8(9) . . ? C27 C25 H25 107.8(9) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C1 N1 C2 110.44(9) . . ? C1 N1 C4 125.56(9) . . ? C2 N1 C4 124.00(9) . . ? C1 N2 C3 110.81(9) . . ? C1 N2 C16 125.17(9) . . ? C3 N2 C16 123.59(9) . . ? C1 P1 H1P 94.5(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -0.85(13) . . . . ? C9 C4 C5 C6 -0.73(17) . . . . ? N1 C4 C5 C6 -179.51(10) . . . . ? C9 C4 C5 C10 -179.30(11) . . . . ? N1 C4 C5 C10 1.91(16) . . . . ? C4 C5 C6 C7 1.25(18) . . . . ? C10 C5 C6 C7 179.83(12) . . . . ? C5 C6 C7 C8 -0.6(2) . . . . ? C6 C7 C8 C9 -0.7(2) . . . . ? C7 C8 C9 C4 1.16(19) . . . . ? C7 C8 C9 C13 -179.49(12) . . . . ? C5 C4 C9 C8 -0.45(17) . . . . ? N1 C4 C9 C8 178.34(11) . . . . ? C5 C4 C9 C13 -179.79(11) . . . . ? N1 C4 C9 C13 -1.00(16) . . . . ? C6 C5 C10 C11 -81.44(17) . . . . ? C4 C5 C10 C11 97.08(16) . . . . ? C6 C5 C10 C12 43.51(16) . . . . ? C4 C5 C10 C12 -137.97(12) . . . . ? C8 C9 C13 C15 -67.61(16) . . . . ? C4 C9 C13 C15 111.71(13) . . . . ? C8 C9 C13 C14 56.94(17) . . . . ? C4 C9 C13 C14 -123.74(13) . . . . ? C21 C16 C17 C18 -3.63(16) . . . . ? N2 C16 C17 C18 173.32(9) . . . . ? C21 C16 C17 C25 175.26(10) . . . . ? N2 C16 C17 C25 -7.80(15) . . . . ? C16 C17 C18 C19 1.21(16) . . . . ? C25 C17 C18 C19 -177.68(11) . . . . ? C17 C18 C19 C20 1.66(17) . . . . ? C18 C19 C20 C21 -2.29(17) . . . . ? C19 C20 C21 C16 -0.01(15) . . . . ? C19 C20 C21 C22 -178.63(10) . . . . ? C17 C16 C21 C20 3.03(15) . . . . ? N2 C16 C21 C20 -173.89(9) . . . . ? C17 C16 C21 C22 -178.34(10) . . . . ? N2 C16 C21 C22 4.74(15) . . . . ? C20 C21 C22 C23 87.61(14) . . . . ? C16 C21 C22 C23 -90.96(14) . . . . ? C20 C21 C22 C24 -36.00(15) . . . . ? C16 C21 C22 C24 145.42(11) . . . . ? C18 C17 C25 C26 51.87(16) . . . . ? C16 C17 C25 C26 -126.99(13) . . . . ? C18 C17 C25 C27 -73.06(15) . . . . ? C16 C17 C25 C27 108.09(14) . . . . ? N2 C1 N1 C2 0.12(12) . . . . ? P1 C1 N1 C2 179.33(9) . . . . ? N2 C1 N1 C4 179.85(9) . . . . ? P1 C1 N1 C4 -0.95(17) . . . . ? C3 C2 N1 C1 0.47(13) . . . . ? C3 C2 N1 C4 -179.26(10) . . . . ? C9 C4 N1 C1 83.14(14) . . . . ? C5 C4 N1 C1 -98.02(13) . . . . ? C9 C4 N1 C2 -97.17(13) . . . . ? C5 C4 N1 C2 81.66(13) . . . . ? N1 C1 N2 C3 -0.66(12) . . . . ? P1 C1 N2 C3 -179.95(8) . . . . ? N1 C1 N2 C16 -173.34(9) . . . . ? P1 C1 N2 C16 7.37(15) . . . . ? C2 C3 N2 C1 0.97(13) . . . . ? C2 C3 N2 C16 173.79(10) . . . . ? C21 C16 N2 C1 -90.59(13) . . . . ? C17 C16 N2 C1 92.35(13) . . . . ? C21 C16 N2 C3 97.63(13) . . . . ? C17 C16 N2 C3 -79.43(13) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.431 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.050 _database_code_depnum_ccdc_archive 'CCDC 937637' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_nhcpppnhccl2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[1,3-bis(1,3-bis(2,6-diisopropylphenyl)-1H-imidazol-2-ylidene)triphosphin-2-ium]Chloride' _chemical_melting_point ? _chemical_formula_moiety 'C58 H80 Cl N4 O P3' _chemical_formula_sum 'C58 H80 Cl N4 O P3' _chemical_formula_weight 977.66 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.0305(12) _cell_length_b 21.4738(9) _cell_length_c 16.7809(11) _cell_angle_alpha 90.00 _cell_angle_beta 115.996(3) _cell_angle_gamma 90.00 _cell_volume 5516.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9886 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 32.02 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.195 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9548 _exptl_absorpt_correction_T_max 0.9695 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 130221 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 30.51 _reflns_number_total 16821 _reflns_number_gt 12024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0679P)^2^+1.8270P] 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 16821 _refine_ls_number_parameters 620 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.002 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 C1 C 0.23161(9) 0.47205(6) 0.93512(9) 0.0114(3) Uani 1 1 d . . . C2 C 0.25776(9) 0.41612(7) 1.05791(10) 0.0151(3) Uani 1 1 d . . . H2 H 0.2781 0.3840 1.1011 0.018 Uiso 1 1 calc R . . C3 C 0.21292(9) 0.46710(7) 1.06004(10) 0.0152(3) Uani 1 1 d . . . H3 H 0.1960 0.4778 1.1052 0.018 Uiso 1 1 calc R . . C4 C 0.29509(9) 0.36449(6) 0.94820(10) 0.0126(3) Uani 1 1 d . . . C5 C 0.22992(9) 0.31971(7) 0.90519(10) 0.0146(3) Uani 1 1 d . . . C6 C 0.25601(10) 0.26435(7) 0.88099(10) 0.0175(3) Uani 1 1 d . . . H6 H 0.2138 0.2330 0.8515 0.021 Uiso 1 1 calc R . . C7 C 0.34271(10) 0.25418(7) 0.89924(11) 0.0194(3) Uani 1 1 d . . . H7 H 0.3594 0.2159 0.8827 0.023 Uiso 1 1 calc R . . C8 C 0.40508(10) 0.29957(7) 0.94156(11) 0.0170(3) Uani 1 1 d . . . H8 H 0.4641 0.2920 0.9533 0.020 Uiso 1 1 calc R . . C9 C 0.38290(9) 0.35616(7) 0.96728(10) 0.0137(3) Uani 1 1 d . . . C10 C 0.13555(9) 0.32942(8) 0.88886(11) 0.0181(3) Uani 1 1 d . . . H10 H 0.1316 0.3717 0.9118 0.022 Uiso 1 1 calc R . . C11 C 0.10948(13) 0.28238(13) 0.94039(16) 0.0494(7) Uani 1 1 d . . . H11A H 0.0502 0.2915 0.9327 0.074 Uiso 1 1 calc R . . H11B H 0.1503 0.2848 1.0034 0.074 Uiso 1 1 calc R . . H11C H 0.1111 0.2404 0.9183 0.074 Uiso 1 1 calc R . . C12 C 0.07216(11) 0.32798(10) 0.79083(12) 0.0281(4) Uani 1 1 d . . . H12A H 0.0903 0.3586 0.7589 0.042 Uiso 1 1 calc R . . H12B H 0.0133 0.3381 0.7835 0.042 Uiso 1 1 calc R . . H12C H 0.0721 0.2863 0.7670 0.042 Uiso 1 1 calc R . . C13 C 0.45230(9) 0.40464(7) 1.01665(11) 0.0165(3) Uani 1 1 d . . . H13 H 0.4221 0.4432 1.0222 0.020 Uiso 1 1 calc R . . C14 C 0.51261(12) 0.38176(8) 1.11048(13) 0.0285(4) Uani 1 1 d . . . H14A H 0.5413 0.3431 1.1067 0.043 Uiso 1 1 calc R . . H14B H 0.4781 0.3741 1.1433 0.043 Uiso 1 1 calc R . . H14C H 0.5570 0.4135 1.1413 0.043 Uiso 1 1 calc R . . C15 C 0.50569(11) 0.42143(8) 0.96625(13) 0.0267(4) Uani 1 1 d . . . H15A H 0.5502 0.4523 1.0002 0.040 Uiso 1 1 calc R . . H15B H 0.4669 0.4388 0.9082 0.040 Uiso 1 1 calc R . . H15C H 0.5342 0.3839 0.9581 0.040 Uiso 1 1 calc R . . C16 C 0.14195(9) 0.55684(7) 0.96004(10) 0.0132(3) Uani 1 1 d . . . C17 C 0.05523(9) 0.55198(7) 0.89384(10) 0.0159(3) Uani 1 1 d . . . C18 C 0.00181(10) 0.60410(8) 0.88036(11) 0.0210(3) Uani 1 1 d . . . H18 H -0.0570 0.6029 0.8362 0.025 Uiso 1 1 calc R . . C19 C 0.03344(10) 0.65750(8) 0.93043(12) 0.0234(3) Uani 1 1 d . . . H19 H -0.0045 0.6920 0.9212 0.028 Uiso 1 1 calc R . . C20 C 0.11943(10) 0.66144(7) 0.99371(11) 0.0202(3) Uani 1 1 d . . . H20 H 0.1401 0.6988 1.0267 0.024 Uiso 1 1 calc R . . C21 C 0.17608(9) 0.61082(7) 1.00937(10) 0.0149(3) Uani 1 1 d . . . C22 C 0.26973(9) 0.61657(7) 1.07971(10) 0.0163(3) Uani 1 1 d . . . H22 H 0.3025 0.5787 1.0769 0.020 Uiso 1 1 calc R . . C23 C 0.27266(11) 0.61993(8) 1.17217(11) 0.0242(3) Uani 1 1 d . . . H23A H 0.3330 0.6265 1.2165 0.036 Uiso 1 1 calc R . . H23B H 0.2506 0.5808 1.1848 0.036 Uiso 1 1 calc R . . H23C H 0.2362 0.6546 1.1743 0.036 Uiso 1 1 calc R . . C24 C 0.31416(10) 0.67390(8) 1.06340(12) 0.0231(3) Uani 1 1 d . . . H24A H 0.2858 0.7117 1.0709 0.035 Uiso 1 1 calc R . . H24B H 0.3090 0.6725 1.0029 0.035 Uiso 1 1 calc R . . H24C H 0.3760 0.6742 1.1059 0.035 Uiso 1 1 calc R . . C25 C 0.01791(9) 0.49286(7) 0.84128(10) 0.0166(3) Uani 1 1 d . . . H25 H 0.0680 0.4668 0.8449 0.020 Uiso 1 1 calc R . . C26 C -0.03171(13) 0.45569(9) 0.88217(14) 0.0327(4) Uani 1 1 d . . . H26A H 0.0067 0.4478 0.9449 0.049 Uiso 1 1 calc R . . H26B H -0.0508 0.4159 0.8509 0.049 Uiso 1 1 calc R . . H26C H -0.0829 0.4795 0.8770 0.049 Uiso 1 1 calc R . . C27 C -0.03988(13) 0.50662(9) 0.74344(12) 0.0301(4) Uani 1 1 d . . . H27A H -0.0931 0.5280 0.7373 0.045 Uiso 1 1 calc R . . H27B H -0.0556 0.4675 0.7101 0.045 Uiso 1 1 calc R . . H27C H -0.0080 0.5332 0.7201 0.045 Uiso 1 1 calc R . . C28 C 0.28245(8) 0.46634(6) 0.59591(9) 0.0106(2) Uani 1 1 d . . . C29 C 0.29384(9) 0.45812(7) 0.46729(10) 0.0147(3) Uani 1 1 d . . . H29 H 0.3069 0.4678 0.4192 0.018 Uiso 1 1 calc R . . C30 C 0.25537(10) 0.40590(7) 0.47722(10) 0.0154(3) Uani 1 1 d . . . H30 H 0.2360 0.3718 0.4371 0.018 Uiso 1 1 calc R . . C31 C 0.36188(9) 0.55188(7) 0.56107(9) 0.0118(3) Uani 1 1 d . . . C32 C 0.45061(9) 0.54778(7) 0.62058(10) 0.0144(3) Uani 1 1 d . . . C33 C 0.50035(10) 0.60223(8) 0.63769(11) 0.0211(3) Uani 1 1 d . . . H33 H 0.5609 0.6012 0.6771 0.025 Uiso 1 1 calc R . . C34 C 0.46185(11) 0.65772(8) 0.59738(12) 0.0249(4) Uani 1 1 d . . . H34 H 0.4961 0.6946 0.6104 0.030 Uiso 1 1 calc R . . C35 C 0.37421(10) 0.66024(7) 0.53847(12) 0.0215(3) Uani 1 1 d . . . H35 H 0.3493 0.6987 0.5111 0.026 Uiso 1 1 calc R . . C36 C 0.32171(9) 0.60710(7) 0.51853(10) 0.0139(3) Uani 1 1 d . . . C37 C 0.49377(9) 0.48703(7) 0.66365(10) 0.0167(3) Uani 1 1 d . . . H37 H 0.4466 0.4559 0.6536 0.020 Uiso 1 1 calc R . . C38 C 0.54816(12) 0.49413(9) 0.76330(12) 0.0286(4) Uani 1 1 d . . . H38A H 0.5690 0.4531 0.7898 0.043 Uiso 1 1 calc R . . H38B H 0.5122 0.5126 0.7894 0.043 Uiso 1 1 calc R . . H38C H 0.5983 0.5212 0.7748 0.043 Uiso 1 1 calc R . . C39 C 0.54982(16) 0.46206(11) 0.62062(15) 0.0453(6) Uani 1 1 d . . . H39A H 0.5143 0.4587 0.5564 0.068 Uiso 1 1 calc R . . H39B H 0.5725 0.4209 0.6450 0.068 Uiso 1 1 calc R . . H39C H 0.5987 0.4906 0.6327 0.068 Uiso 1 1 calc R . . C40 C 0.22717(9) 0.61002(7) 0.44934(10) 0.0163(3) Uani 1 1 d . . . H40 H 0.1962 0.5723 0.4561 0.020 Uiso 1 1 calc R . . C41 C 0.17971(10) 0.66778(8) 0.45952(13) 0.0240(3) Uani 1 1 d . . . H41A H 0.2077 0.7053 0.4506 0.036 Uiso 1 1 calc R . . H41B H 0.1826 0.6684 0.5191 0.036 Uiso 1 1 calc R . . H41C H 0.1185 0.6666 0.4153 0.036 Uiso 1 1 calc R . . C42 C 0.22409(11) 0.60872(9) 0.35680(11) 0.0254(4) Uani 1 1 d . . . H42A H 0.1633 0.6123 0.3119 0.038 Uiso 1 1 calc R . . H42B H 0.2489 0.5694 0.3486 0.038 Uiso 1 1 calc R . . H42C H 0.2581 0.6436 0.3507 0.038 Uiso 1 1 calc R . . C43 C 0.21977(9) 0.35990(6) 0.59299(10) 0.0124(3) Uani 1 1 d . . . C44 C 0.13221(9) 0.35786(7) 0.57704(10) 0.0142(3) Uani 1 1 d . . . C45 C 0.10557(10) 0.30627(7) 0.60952(11) 0.0174(3) Uani 1 1 d . . . H45 H 0.0462 0.3028 0.5991 0.021 Uiso 1 1 calc R . . C46 C 0.16428(10) 0.26000(7) 0.65682(11) 0.0185(3) Uani 1 1 d . . . H46 H 0.1452 0.2258 0.6798 0.022 Uiso 1 1 calc R . . C47 C 0.25069(10) 0.26329(7) 0.67074(11) 0.0179(3) Uani 1 1 d . . . H47 H 0.2901 0.2310 0.7027 0.021 Uiso 1 1 calc R . . C48 C 0.28058(9) 0.31314(7) 0.63854(10) 0.0145(3) Uani 1 1 d . . . C49 C 0.37519(9) 0.31600(7) 0.65326(10) 0.0171(3) Uani 1 1 d . . . H49 H 0.3782 0.3438 0.6068 0.021 Uiso 1 1 calc R . . C50 C 0.43342(10) 0.34381(8) 0.74385(12) 0.0233(3) Uani 1 1 d . . . H50A H 0.4118 0.3853 0.7486 0.035 Uiso 1 1 calc R . . H50B H 0.4934 0.3472 0.7506 0.035 Uiso 1 1 calc R . . H50C H 0.4325 0.3168 0.7905 0.035 Uiso 1 1 calc R . . C51 C 0.41039(12) 0.25216(9) 0.64510(14) 0.0302(4) Uani 1 1 d . . . H51A H 0.4148 0.2257 0.6945 0.045 Uiso 1 1 calc R . . H51B H 0.4683 0.2569 0.6467 0.045 Uiso 1 1 calc R . . H51C H 0.3706 0.2329 0.5889 0.045 Uiso 1 1 calc R . . C52 C 0.06689(9) 0.40833(7) 0.52608(10) 0.0162(3) Uani 1 1 d . . . H52 H 0.0996 0.4430 0.5143 0.019 Uiso 1 1 calc R . . C53 C 0.02220(10) 0.43463(8) 0.58036(12) 0.0211(3) Uani 1 1 d . . . H53A H -0.0074 0.4009 0.5958 0.032 Uiso 1 1 calc R . . H53B H -0.0207 0.4661 0.5454 0.032 Uiso 1 1 calc R . . H53C H 0.0661 0.4537 0.6347 0.032 Uiso 1 1 calc R . . C54 C -0.00113(11) 0.38372(8) 0.43646(12) 0.0255(4) Uani 1 1 d . . . H54A H -0.0340 0.3496 0.4464 0.038 Uiso 1 1 calc R . . H54B H 0.0285 0.3685 0.4017 0.038 Uiso 1 1 calc R . . H54C H -0.0414 0.4174 0.4041 0.038 Uiso 1 1 calc R . . C1S C 0.73648(13) 0.18927(9) 0.68957(13) 0.0323(4) Uani 1 1 d . . . H1SA H 0.7060 0.2245 0.6499 0.039 Uiso 1 1 calc R . . H1SB H 0.7098 0.1496 0.6599 0.039 Uiso 1 1 calc R . . C2S C 0.73377(16) 0.19526(11) 0.77808(16) 0.0440(5) Uani 1 1 d . . . H2SA H 0.6817 0.2193 0.7716 0.053 Uiso 1 1 calc R . . H2SB H 0.7312 0.1536 0.8020 0.053 Uiso 1 1 calc R . . C3S C 0.83335(13) 0.19064(10) 0.71536(14) 0.0365(4) Uani 1 1 d . . . H3SA H 0.8604 0.1492 0.7352 0.044 Uiso 1 1 calc R . . H3SB H 0.8453 0.2052 0.6658 0.044 Uiso 1 1 calc R . . C4S C 0.86503(13) 0.23698(9) 0.79091(14) 0.0341(4) Uani 1 1 d . . . H4SA H 0.9274 0.2298 0.8313 0.041 Uiso 1 1 calc R . . H4SB H 0.8582 0.2801 0.7680 0.041 Uiso 1 1 calc R . . Cl1 Cl 0.74800(2) 0.604437(19) 0.73769(3) 0.01995(8) Uani 1 1 d . . . N1 N 0.26892(8) 0.41919(6) 0.98086(8) 0.0120(2) Uani 1 1 d . . . N2 N 0.19603(8) 0.50120(6) 0.98391(8) 0.0123(2) Uani 1 1 d . . . N3 N 0.31073(7) 0.49513(5) 0.54068(8) 0.0111(2) Uani 1 1 d . . . N4 N 0.24914(8) 0.41092(5) 0.55660(8) 0.0125(2) Uani 1 1 d . . . O1S O 0.81202(10) 0.22707(7) 0.83615(10) 0.0392(3) Uani 1 1 d . . . P1 P 0.22938(3) 0.511304(18) 0.83865(3) 0.01598(9) Uani 1 1 d . . . P2 P 0.25957(2) 0.442884(18) 0.76793(3) 0.01395(8) Uani 1 1 d . . . P3 P 0.28569(3) 0.508894(18) 0.69056(3) 0.01474(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0115(6) 0.0110(6) 0.0133(6) 0.0012(5) 0.0069(5) 0.0022(5) C2 0.0158(6) 0.0170(7) 0.0131(7) 0.0034(5) 0.0068(5) 0.0012(5) C3 0.0159(6) 0.0199(7) 0.0113(7) 0.0035(5) 0.0074(5) 0.0025(5) C4 0.0150(6) 0.0091(6) 0.0152(7) 0.0027(5) 0.0081(5) 0.0024(5) C5 0.0143(6) 0.0147(7) 0.0142(7) 0.0030(5) 0.0058(5) -0.0004(5) C6 0.0206(7) 0.0130(7) 0.0164(7) 0.0012(5) 0.0059(6) -0.0029(5) C7 0.0228(7) 0.0120(7) 0.0231(8) -0.0016(6) 0.0099(6) 0.0024(5) C8 0.0165(7) 0.0141(7) 0.0213(8) -0.0006(6) 0.0092(6) 0.0025(5) C9 0.0146(6) 0.0099(6) 0.0179(7) 0.0011(5) 0.0082(5) 0.0001(5) C10 0.0143(6) 0.0216(8) 0.0178(7) 0.0020(6) 0.0065(6) -0.0021(5) C11 0.0207(9) 0.0797(18) 0.0459(13) 0.0408(13) 0.0128(9) 0.0001(10) C12 0.0184(8) 0.0438(11) 0.0197(8) 0.0025(8) 0.0063(6) 0.0058(7) C13 0.0141(6) 0.0116(7) 0.0255(8) -0.0021(6) 0.0102(6) -0.0008(5) C14 0.0260(8) 0.0221(9) 0.0290(10) -0.0027(7) 0.0043(7) -0.0056(7) C15 0.0261(8) 0.0221(8) 0.0411(11) -0.0070(7) 0.0233(8) -0.0079(6) C16 0.0134(6) 0.0146(7) 0.0141(7) 0.0021(5) 0.0083(5) 0.0048(5) C17 0.0128(6) 0.0208(7) 0.0154(7) 0.0013(6) 0.0073(5) 0.0034(5) C18 0.0136(7) 0.0242(8) 0.0216(8) 0.0007(6) 0.0044(6) 0.0075(6) C19 0.0195(7) 0.0213(8) 0.0261(9) 0.0006(6) 0.0068(6) 0.0107(6) C20 0.0195(7) 0.0173(8) 0.0214(8) -0.0007(6) 0.0067(6) 0.0059(6) C21 0.0151(6) 0.0161(7) 0.0131(7) 0.0017(5) 0.0057(5) 0.0055(5) C22 0.0151(6) 0.0163(7) 0.0146(7) 0.0005(5) 0.0037(5) 0.0051(5) C23 0.0260(8) 0.0279(9) 0.0154(8) 0.0012(6) 0.0060(6) 0.0056(7) C24 0.0179(7) 0.0244(8) 0.0231(8) 0.0009(7) 0.0053(6) 0.0013(6) C25 0.0127(6) 0.0216(8) 0.0166(7) -0.0019(6) 0.0075(5) 0.0013(5) C26 0.0404(11) 0.0340(10) 0.0355(11) -0.0097(8) 0.0275(9) -0.0132(8) C27 0.0335(9) 0.0327(10) 0.0168(8) -0.0030(7) 0.0043(7) 0.0017(7) C28 0.0108(6) 0.0105(6) 0.0115(6) 0.0006(5) 0.0058(5) -0.0005(5) C29 0.0184(7) 0.0165(7) 0.0108(6) -0.0017(5) 0.0078(5) 0.0009(5) C30 0.0194(7) 0.0146(7) 0.0129(7) -0.0038(5) 0.0077(6) -0.0008(5) C31 0.0115(6) 0.0141(7) 0.0115(6) 0.0002(5) 0.0065(5) -0.0032(5) C32 0.0130(6) 0.0184(7) 0.0129(7) 0.0021(5) 0.0066(5) -0.0010(5) C33 0.0126(6) 0.0240(8) 0.0223(8) 0.0023(6) 0.0035(6) -0.0054(6) C34 0.0194(7) 0.0201(8) 0.0309(9) 0.0029(7) 0.0072(7) -0.0080(6) C35 0.0173(7) 0.0168(8) 0.0280(9) 0.0064(6) 0.0077(6) -0.0027(5) C36 0.0122(6) 0.0147(7) 0.0148(7) 0.0019(5) 0.0059(5) -0.0017(5) C37 0.0136(6) 0.0209(8) 0.0141(7) 0.0043(6) 0.0046(5) 0.0009(5) C38 0.0303(9) 0.0284(9) 0.0170(8) 0.0030(7) 0.0012(7) 0.0045(7) C39 0.0632(14) 0.0520(14) 0.0352(11) 0.0224(10) 0.0347(11) 0.0377(11) C40 0.0124(6) 0.0151(7) 0.0187(7) 0.0023(6) 0.0044(5) -0.0010(5) C41 0.0175(7) 0.0203(8) 0.0320(9) 0.0006(7) 0.0087(7) 0.0025(6) C42 0.0247(8) 0.0280(9) 0.0177(8) 0.0019(7) 0.0039(6) 0.0020(7) C43 0.0155(6) 0.0088(6) 0.0131(7) -0.0013(5) 0.0063(5) -0.0017(5) C44 0.0156(6) 0.0106(6) 0.0158(7) -0.0018(5) 0.0064(5) -0.0012(5) C45 0.0163(7) 0.0146(7) 0.0211(8) -0.0013(6) 0.0080(6) -0.0036(5) C46 0.0208(7) 0.0133(7) 0.0196(8) 0.0012(6) 0.0072(6) -0.0034(5) C47 0.0198(7) 0.0130(7) 0.0174(7) 0.0007(5) 0.0051(6) 0.0009(5) C48 0.0155(6) 0.0121(7) 0.0143(7) -0.0034(5) 0.0048(5) -0.0009(5) C49 0.0146(6) 0.0186(7) 0.0170(7) -0.0007(6) 0.0060(6) 0.0026(5) C50 0.0188(7) 0.0272(9) 0.0224(8) -0.0034(7) 0.0075(6) -0.0006(6) C51 0.0289(9) 0.0284(9) 0.0360(11) -0.0067(8) 0.0166(8) 0.0061(7) C52 0.0154(6) 0.0119(7) 0.0199(7) 0.0022(5) 0.0065(6) 0.0013(5) C53 0.0187(7) 0.0196(8) 0.0262(9) 0.0013(6) 0.0108(6) 0.0035(6) C54 0.0252(8) 0.0220(8) 0.0216(8) 0.0003(6) 0.0031(7) 0.0033(6) C1S 0.0354(10) 0.0284(10) 0.0286(10) -0.0049(8) 0.0099(8) -0.0010(7) C2S 0.0623(15) 0.0358(12) 0.0433(13) -0.0131(10) 0.0319(12) -0.0188(10) C3S 0.0392(11) 0.0358(11) 0.0349(11) 0.0009(9) 0.0166(9) 0.0033(8) C4S 0.0332(10) 0.0232(9) 0.0359(11) 0.0068(8) 0.0058(8) -0.0006(7) Cl1 0.02106(17) 0.02300(19) 0.01561(17) -0.00170(14) 0.00786(14) -0.00041(14) N1 0.0127(5) 0.0116(6) 0.0130(6) 0.0026(4) 0.0070(4) 0.0026(4) N2 0.0133(5) 0.0133(6) 0.0117(6) 0.0024(4) 0.0069(4) 0.0042(4) N3 0.0118(5) 0.0120(6) 0.0101(5) -0.0004(4) 0.0054(4) -0.0010(4) N4 0.0148(5) 0.0103(6) 0.0131(6) -0.0015(4) 0.0068(5) -0.0011(4) O1S 0.0551(9) 0.0308(8) 0.0291(8) -0.0067(6) 0.0159(7) -0.0063(6) P1 0.02413(19) 0.01253(18) 0.01801(19) 0.00496(14) 0.01543(16) 0.00640(14) P2 0.01955(18) 0.01154(17) 0.01389(18) 0.00013(14) 0.01022(14) -0.00015(13) P3 0.02239(19) 0.01148(17) 0.01572(19) -0.00340(14) 0.01331(15) -0.00502(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.3615(18) . ? C1 N2 1.3654(18) . ? C1 P1 1.8107(15) . ? C2 C3 1.344(2) . ? C2 N1 1.3884(19) . ? C2 H2 0.9500 . ? C3 N2 1.3889(19) . ? C3 H3 0.9500 . ? C4 C9 1.3969(19) . ? C4 C5 1.406(2) . ? C4 N1 1.4466(18) . ? C5 C6 1.391(2) . ? C5 C10 1.522(2) . ? C6 C7 1.388(2) . ? C6 H6 0.9500 . ? C7 C8 1.386(2) . ? C7 H7 0.9500 . ? C8 C9 1.396(2) . ? C8 H8 0.9500 . ? C9 C13 1.519(2) . ? C10 C11 1.517(2) . ? C10 C12 1.522(2) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.532(2) . ? C13 C14 1.536(2) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.395(2) . ? C16 C17 1.410(2) . ? C16 N2 1.4537(17) . ? C17 C18 1.397(2) . ? C17 C25 1.517(2) . ? C18 C19 1.384(2) . ? C18 H18 0.9500 . ? C19 C20 1.384(2) . ? C19 H19 0.9500 . ? C20 C21 1.400(2) . ? C20 H20 0.9500 . ? C21 C22 1.517(2) . ? C22 C24 1.531(2) . ? C22 C23 1.532(2) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.527(2) . ? C25 C27 1.528(2) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N4 1.3583(18) . ? C28 N3 1.3654(17) . ? C28 P3 1.8123(14) . ? C29 C30 1.345(2) . ? C29 N3 1.3858(18) . ? C29 H29 0.9500 . ? C30 N4 1.3860(19) . ? C30 H30 0.9500 . ? C31 C36 1.399(2) . ? C31 C32 1.4020(19) . ? C31 N3 1.4490(17) . ? C32 C33 1.398(2) . ? C32 C37 1.516(2) . ? C33 C34 1.385(2) . ? C33 H33 0.9500 . ? C34 C35 1.384(2) . ? C34 H34 0.9500 . ? C35 C36 1.397(2) . ? C35 H35 0.9500 . ? C36 C40 1.518(2) . ? C37 C39 1.525(2) . ? C37 C38 1.523(2) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.530(2) . ? C40 C42 1.531(2) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.3955(19) . ? C43 C48 1.404(2) . ? C43 N4 1.4461(18) . ? C44 C45 1.395(2) . ? C44 C52 1.520(2) . ? C45 C46 1.386(2) . ? C45 H45 0.9500 . ? C46 C47 1.387(2) . ? C46 H46 0.9500 . ? C47 C48 1.392(2) . ? C47 H47 0.9500 . ? C48 C49 1.520(2) . ? C49 C51 1.526(2) . ? C49 C50 1.526(2) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.528(2) . ? C52 C54 1.535(2) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C1S C2S 1.512(3) . ? C1S C3S 1.511(3) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S O1S 1.433(3) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S C4S 1.513(3) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S O1S 1.427(3) . ? C4S H4SA 0.9900 . ? C4S H4SB 0.9900 . ? P1 P2 2.0895(5) . ? P2 P3 2.0974(5) . ? 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 C1 N2 105.32(12) . . ? N1 C1 P1 135.55(11) . . ? N2 C1 P1 118.80(10) . . ? C3 C2 N1 107.29(13) . . ? C3 C2 H2 126.4 . . ? N1 C2 H2 126.4 . . ? C2 C3 N2 107.22(13) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? C9 C4 C5 123.72(13) . . ? C9 C4 N1 119.59(13) . . ? C5 C4 N1 116.42(12) . . ? C6 C5 C4 116.96(13) . . ? C6 C5 C10 120.80(13) . . ? C4 C5 C10 122.19(13) . . ? C7 C6 C5 121.03(14) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C8 C7 C6 120.31(14) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 121.35(14) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 116.63(13) . . ? C8 C9 C13 120.92(13) . . ? C4 C9 C13 122.41(13) . . ? C11 C10 C12 110.89(15) . . ? C11 C10 C5 110.85(14) . . ? C12 C10 C5 112.62(13) . . ? C11 C10 H10 107.4 . . ? C12 C10 H10 107.4 . . ? C5 C10 H10 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C15 111.62(13) . . ? C9 C13 C14 110.53(13) . . ? C15 C13 C14 110.45(14) . . ? C9 C13 H13 108.0 . . ? C15 C13 H13 108.0 . . ? C14 C13 H13 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 123.32(13) . . ? C21 C16 N2 118.08(12) . . ? C17 C16 N2 118.34(13) . . ? C18 C17 C16 116.82(14) . . ? C18 C17 C25 119.94(13) . . ? C16 C17 C25 123.17(13) . . ? C19 C18 C17 120.88(14) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 121.06(14) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 120.46(15) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C16 C21 C20 117.41(13) . . ? C16 C21 C22 123.50(12) . . ? C20 C21 C22 119.07(14) . . ? C21 C22 C24 111.09(13) . . ? C21 C22 C23 110.37(13) . . ? C24 C22 C23 110.12(14) . . ? C21 C22 H22 108.4 . . ? C24 C22 H22 108.4 . . ? C23 C22 H22 108.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C17 C25 C26 110.47(13) . . ? C17 C25 C27 111.79(14) . . ? C26 C25 C27 111.19(15) . . ? C17 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 N3 105.28(12) . . ? N4 C28 P3 135.50(11) . . ? N3 C28 P3 118.83(10) . . ? C30 C29 N3 106.89(13) . . ? C30 C29 H29 126.6 . . ? N3 C29 H29 126.6 . . ? C29 C30 N4 107.50(13) . . ? C29 C30 H30 126.2 . . ? N4 C30 H30 126.2 . . ? C36 C31 C32 123.38(13) . . ? C36 C31 N3 118.93(12) . . ? C32 C31 N3 117.65(12) . . ? C33 C32 C31 117.44(13) . . ? C33 C32 C37 119.88(13) . . ? C31 C32 C37 122.65(13) . . ? C34 C33 C32 120.31(14) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 120.94(15) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 121.07(15) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 116.86(13) . . ? C35 C36 C40 120.16(13) . . ? C31 C36 C40 122.88(13) . . ? C32 C37 C39 110.50(13) . . ? C32 C37 C38 111.82(14) . . ? C39 C37 C38 110.46(15) . . ? C32 C37 H37 108.0 . . ? C39 C37 H37 108.0 . . ? C38 C37 H37 108.0 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 C41 112.52(13) . . ? C36 C40 C42 109.16(12) . . ? C41 C40 C42 110.07(13) . . ? C36 C40 H40 108.3 . . ? C41 C40 H40 108.3 . . ? C42 C40 H40 108.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 123.59(13) . . ? C44 C43 N4 118.76(12) . . ? C48 C43 N4 117.56(12) . . ? C45 C44 C43 116.94(13) . . ? C45 C44 C52 120.19(13) . . ? C43 C44 C52 122.86(13) . . ? C46 C45 C44 121.09(14) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C46 C47 120.38(14) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C48 121.01(14) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? C47 C48 C43 116.96(13) . . ? C47 C48 C49 120.64(13) . . ? C43 C48 C49 122.40(13) . . ? C48 C49 C51 112.28(13) . . ? C48 C49 C50 110.93(13) . . ? C51 C49 C50 109.35(14) . . ? C48 C49 H49 108.0 . . ? C51 C49 H49 108.0 . . ? C50 C49 H49 108.0 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C44 C52 C53 111.17(13) . . ? C44 C52 C54 110.97(13) . . ? C53 C52 C54 110.61(13) . . ? C44 C52 H52 108.0 . . ? C53 C52 H52 108.0 . . ? C54 C52 H52 108.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C2S C1S C3S 102.51(17) . . ? C2S C1S H1SA 111.3 . . ? C3S C1S H1SA 111.3 . . ? C2S C1S H1SB 111.3 . . ? C3S C1S H1SB 111.3 . . ? H1SA C1S H1SB 109.2 . . ? O1S C2S C1S 106.80(17) . . ? O1S C2S H2SA 110.4 . . ? C1S C2S H2SA 110.4 . . ? O1S C2S H2SB 110.4 . . ? C1S C2S H2SB 110.4 . . ? H2SA C2S H2SB 108.6 . . ? C4S C3S C1S 101.32(16) . . ? C4S C3S H3SA 111.5 . . ? C1S C3S H3SA 111.5 . . ? C4S C3S H3SB 111.5 . . ? C1S C3S H3SB 111.5 . . ? H3SA C3S H3SB 109.3 . . ? O1S C4S C3S 105.74(16) . . ? O1S C4S H4SA 110.6 . . ? C3S C4S H4SA 110.6 . . ? O1S C4S H4SB 110.6 . . ? C3S C4S H4SB 110.6 . . ? H4SA C4S H4SB 108.7 . . ? C1 N1 C2 110.13(12) . . ? C1 N1 C4 127.48(12) . . ? C2 N1 C4 120.32(12) . . ? C1 N2 C3 110.02(12) . . ? C1 N2 C16 127.28(12) . . ? C3 N2 C16 122.52(12) . . ? C28 N3 C29 110.24(12) . . ? C28 N3 C31 125.09(12) . . ? C29 N3 C31 124.15(12) . . ? C28 N4 C30 110.08(12) . . ? C28 N4 C43 127.35(12) . . ? C30 N4 C43 122.23(12) . . ? C4S O1S C2S 109.01(16) . . ? C1 P1 P2 105.45(5) . . ? P1 P2 P3 92.76(2) . . ? C28 P3 P2 105.58(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.43(16) . . . . ? C9 C4 C5 C6 0.0(2) . . . . ? N1 C4 C5 C6 -174.08(13) . . . . ? C9 C4 C5 C10 177.48(14) . . . . ? N1 C4 C5 C10 3.4(2) . . . . ? C4 C5 C6 C7 0.3(2) . . . . ? C10 C5 C6 C7 -177.14(14) . . . . ? C5 C6 C7 C8 -0.5(2) . . . . ? C6 C7 C8 C9 0.4(2) . . . . ? C7 C8 C9 C4 0.0(2) . . . . ? C7 C8 C9 C13 177.72(15) . . . . ? C5 C4 C9 C8 -0.2(2) . . . . ? N1 C4 C9 C8 173.72(13) . . . . ? C5 C4 C9 C13 -177.89(14) . . . . ? N1 C4 C9 C13 -4.0(2) . . . . ? C6 C5 C10 C11 62.2(2) . . . . ? C4 C5 C10 C11 -115.12(19) . . . . ? C6 C5 C10 C12 -62.7(2) . . . . ? C4 C5 C10 C12 119.98(17) . . . . ? C8 C9 C13 C15 54.6(2) . . . . ? C4 C9 C13 C15 -127.78(16) . . . . ? C8 C9 C13 C14 -68.71(19) . . . . ? C4 C9 C13 C14 108.87(17) . . . . ? C21 C16 C17 C18 -1.9(2) . . . . ? N2 C16 C17 C18 172.15(13) . . . . ? C21 C16 C17 C25 -179.02(14) . . . . ? N2 C16 C17 C25 -5.0(2) . . . . ? C16 C17 C18 C19 -0.3(2) . . . . ? C25 C17 C18 C19 177.01(15) . . . . ? C17 C18 C19 C20 1.7(3) . . . . ? C18 C19 C20 C21 -1.0(3) . . . . ? C17 C16 C21 C20 2.5(2) . . . . ? N2 C16 C21 C20 -171.55(13) . . . . ? C17 C16 C21 C22 -179.04(14) . . . . ? N2 C16 C21 C22 6.9(2) . . . . ? C19 C20 C21 C16 -1.0(2) . . . . ? C19 C20 C21 C22 -179.54(15) . . . . ? C16 C21 C22 C24 127.50(16) . . . . ? C20 C21 C22 C24 -54.04(19) . . . . ? C16 C21 C22 C23 -110.07(17) . . . . ? C20 C21 C22 C23 68.40(18) . . . . ? C18 C17 C25 C26 -80.63(19) . . . . ? C16 C17 C25 C26 96.45(18) . . . . ? C18 C17 C25 C27 43.8(2) . . . . ? C16 C17 C25 C27 -139.16(16) . . . . ? N3 C29 C30 N4 -0.24(16) . . . . ? C36 C31 C32 C33 0.2(2) . . . . ? N3 C31 C32 C33 177.84(13) . . . . ? C36 C31 C32 C37 -177.81(14) . . . . ? N3 C31 C32 C37 -0.2(2) . . . . ? C31 C32 C33 C34 0.7(2) . . . . ? C37 C32 C33 C34 178.80(16) . . . . ? C32 C33 C34 C35 -1.1(3) . . . . ? C33 C34 C35 C36 0.7(3) . . . . ? C34 C35 C36 C31 0.3(2) . . . . ? C34 C35 C36 C40 -176.11(16) . . . . ? C32 C31 C36 C35 -0.7(2) . . . . ? N3 C31 C36 C35 -178.28(13) . . . . ? C32 C31 C36 C40 175.54(14) . . . . ? N3 C31 C36 C40 -2.0(2) . . . . ? C33 C32 C37 C39 -73.4(2) . . . . ? C31 C32 C37 C39 104.61(19) . . . . ? C33 C32 C37 C38 50.1(2) . . . . ? C31 C32 C37 C38 -131.91(16) . . . . ? C35 C36 C40 C41 -44.8(2) . . . . ? C31 C36 C40 C41 139.11(15) . . . . ? C35 C36 C40 C42 77.75(18) . . . . ? C31 C36 C40 C42 -98.39(17) . . . . ? C48 C43 C44 C45 0.6(2) . . . . ? N4 C43 C44 C45 176.88(13) . . . . ? C48 C43 C44 C52 -178.80(14) . . . . ? N4 C43 C44 C52 -2.5(2) . . . . ? C43 C44 C45 C46 1.2(2) . . . . ? C52 C44 C45 C46 -179.44(14) . . . . ? C44 C45 C46 C47 -1.8(2) . . . . ? C45 C46 C47 C48 0.7(2) . . . . ? C46 C47 C48 C43 1.0(2) . . . . ? C46 C47 C48 C49 -179.33(14) . . . . ? C44 C43 C48 C47 -1.6(2) . . . . ? N4 C43 C48 C47 -177.97(13) . . . . ? C44 C43 C48 C49 178.70(14) . . . . ? N4 C43 C48 C49 2.4(2) . . . . ? C47 C48 C49 C51 38.4(2) . . . . ? C43 C48 C49 C51 -141.98(15) . . . . ? C47 C48 C49 C50 -84.33(18) . . . . ? C43 C48 C49 C50 95.33(17) . . . . ? C45 C44 C52 C53 55.80(19) . . . . ? C43 C44 C52 C53 -124.84(15) . . . . ? C45 C44 C52 C54 -67.76(19) . . . . ? C43 C44 C52 C54 111.60(16) . . . . ? C3S C1S C2S O1S 26.1(2) . . . . ? C2S C1S C3S C4S -36.6(2) . . . . ? C1S C3S C4S O1S 35.4(2) . . . . ? N2 C1 N1 C2 -0.93(15) . . . . ? P1 C1 N1 C2 172.09(12) . . . . ? N2 C1 N1 C4 162.52(13) . . . . ? P1 C1 N1 C4 -24.5(2) . . . . ? C3 C2 N1 C1 0.31(17) . . . . ? C3 C2 N1 C4 -164.50(13) . . . . ? C9 C4 N1 C1 100.32(17) . . . . ? C5 C4 N1 C1 -85.31(18) . . . . ? C9 C4 N1 C2 -97.73(16) . . . . ? C5 C4 N1 C2 76.64(17) . . . . ? N1 C1 N2 C3 1.20(16) . . . . ? P1 C1 N2 C3 -173.22(10) . . . . ? N1 C1 N2 C16 -174.09(13) . . . . ? P1 C1 N2 C16 11.48(19) . . . . ? C2 C3 N2 C1 -1.04(17) . . . . ? C2 C3 N2 C16 174.52(13) . . . . ? C21 C16 N2 C1 -112.87(16) . . . . ? C17 C16 N2 C1 72.80(19) . . . . ? C21 C16 N2 C3 72.37(18) . . . . ? C17 C16 N2 C3 -101.95(17) . . . . ? N4 C28 N3 C29 0.85(15) . . . . ? P3 C28 N3 C29 -173.08(10) . . . . ? N4 C28 N3 C31 -171.13(12) . . . . ? P3 C28 N3 C31 14.94(18) . . . . ? C30 C29 N3 C28 -0.39(16) . . . . ? C30 C29 N3 C31 171.69(13) . . . . ? C36 C31 N3 C28 -107.32(16) . . . . ? C32 C31 N3 C28 74.98(18) . . . . ? C36 C31 N3 C29 81.78(18) . . . . ? C32 C31 N3 C29 -95.92(17) . . . . ? N3 C28 N4 C30 -1.00(15) . . . . ? P3 C28 N4 C30 171.41(12) . . . . ? N3 C28 N4 C43 172.35(12) . . . . ? P3 C28 N4 C43 -15.2(2) . . . . ? C29 C30 N4 C28 0.79(16) . . . . ? C29 C30 N4 C43 -172.96(12) . . . . ? C44 C43 N4 C28 91.03(18) . . . . ? C48 C43 N4 C28 -92.45(17) . . . . ? C44 C43 N4 C30 -96.36(17) . . . . ? C48 C43 N4 C30 80.16(17) . . . . ? C3S C4S O1S C2S -19.9(2) . . . . ? C1S C2S O1S C4S -4.0(2) . . . . ? N1 C1 P1 P2 21.87(16) . . . . ? N2 C1 P1 P2 -165.82(10) . . . . ? C1 P1 P2 P3 -164.61(5) . . . . ? N4 C28 P3 P2 18.66(16) . . . . ? N3 C28 P3 P2 -169.70(9) . . . . ? P1 P2 P3 C28 -162.75(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.486 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.072 _database_code_depnum_ccdc_archive 'CCDC 937642' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sadp21n _audit_creation_method SHELXL-97 _chemical_name_systematic 'di(N,N bis(2,6 diisopropylphenyl) imidazolium) chloride bis(trimethylsilyl)heptaphosphide tritetrahydrofuran' _chemical_name_common 'di(N,N bis(2,6 diisopropylphenyl) imidazolium) chloride bis(trimethylsilyl)heptaphosphide tritetrahydrofuran' _chemical_formula_moiety 'C33 H55 N2 P7 Si2' _chemical_formula_sum 'C72 H116 Cl N4 O3 P7 Si2' _chemical_properties_physical 'air-sensitive, moisture-sensitive' _exptl_crystal_recrystallization_method 'Saturated THF solution at -30C' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour orange _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1394.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 22.3995(3) _cell_length_b 12.1255(2) _cell_length_c 29.5997(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.8200(10) _cell_angle_gamma 90.00 _cell_volume 8038.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9854 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 29.86 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3000 _exptl_absorpt_coefficient_mu 0.261 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6728 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104129 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 30.55 _reflns_number_total 23887 _reflns_number_gt 17711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep 3v2' _computing_publication_material 'Ortep 3v2' _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^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23887 _refine_ls_number_parameters 844 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.311 _refine_ls_restrained_S_all 1.311 _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 Cl1 Cl 0.183820(18) 0.34887(4) 0.505540(14) 0.02789(9) Uani 1 1 d . . . P3 P 0.468365(17) 1.05554(3) 0.639811(14) 0.02000(9) Uani 1 1 d . . . P2 P 0.528036(17) 0.91346(3) 0.650855(14) 0.01971(9) Uani 1 1 d . . . P4 P 0.430520(18) 1.07372(3) 0.707328(15) 0.02136(9) Uani 1 1 d . . . Si2 Si 0.53221(2) 1.20131(4) 0.639360(16) 0.02299(10) Uani 1 1 d . . . P6 P 0.496344(18) 0.98776(4) 0.752559(14) 0.02074(9) Uani 1 1 d . . . Si1 Si 0.48606(2) 0.65721(4) 0.697546(16) 0.02277(10) Uani 1 1 d . . . P7 P 0.572277(17) 0.94085(4) 0.714269(15) 0.02182(9) Uani 1 1 d . . . P1 P 0.448188(17) 0.81331(3) 0.665023(14) 0.02022(9) Uani 1 1 d . . . P5 P 0.415804(17) 0.89812(4) 0.725124(14) 0.02056(9) Uani 1 1 d . . . N4 N 0.08274(5) 0.33115(10) 0.61176(4) 0.0158(2) Uani 1 1 d . . . N3 N 0.15308(5) 0.21695(10) 0.62943(4) 0.0155(2) Uani 1 1 d . . . C32 C 0.25449(6) 0.14244(13) 0.62200(5) 0.0180(3) Uani 1 1 d . . . C37 C 0.28042(7) 0.25710(13) 0.61748(6) 0.0217(3) Uani 1 1 d . . . H37 H 0.2471 0.3086 0.6093 0.026 Uiso 1 1 calc R . . C33 C 0.29136(7) 0.04945(14) 0.62242(5) 0.0226(3) Uani 1 1 d . . . H33 H 0.3332 0.0586 0.6195 0.027 Uiso 1 1 calc R . . C30 C 0.08901(7) 0.33345(13) 0.65820(5) 0.0185(3) Uani 1 1 d . . . H30 H 0.0664 0.3768 0.6785 0.022 Uiso 1 1 calc R . . C31 C 0.19352(6) 0.12329(12) 0.62701(5) 0.0168(3) Uani 1 1 d . . . C44 C 0.04406(7) 0.50398(13) 0.58083(5) 0.0198(3) Uani 1 1 d . . . C36 C 0.16816(7) 0.01915(13) 0.63202(6) 0.0208(3) Uani 1 1 d . . . C34 C 0.26825(7) -0.05540(14) 0.62704(6) 0.0244(3) Uani 1 1 d . . . H34 H 0.2942 -0.1174 0.6272 0.029 Uiso 1 1 calc R . . C43 C 0.03685(6) 0.39082(12) 0.58665(5) 0.0169(3) Uani 1 1 d . . . C49 C 0.09862(7) 0.56630(13) 0.59795(6) 0.0232(3) Uani 1 1 d . . . H49 H 0.1284 0.5110 0.6093 0.028 Uiso 1 1 calc R . . C47 C -0.05966(7) 0.39463(15) 0.55216(6) 0.0250(3) Uani 1 1 d . . . H47 H -0.0951 0.3583 0.5424 0.030 Uiso 1 1 calc R . . C45 C -0.00301(7) 0.56039(14) 0.55961(6) 0.0239(3) Uani 1 1 d . . . H45 H 0.0005 0.6375 0.5546 0.029 Uiso 1 1 calc R . . C29 C 0.13344(6) 0.26221(12) 0.66946(5) 0.0177(3) Uani 1 1 d . . . H29 H 0.1482 0.2465 0.6990 0.021 Uiso 1 1 calc R . . C28 C 0.12213(6) 0.25979(12) 0.59481(5) 0.0164(3) Uani 1 1 d . . . H28 H 0.1271 0.2427 0.5638 0.020 Uiso 1 1 calc R . . C52 C -0.02208(7) 0.20965(14) 0.57982(6) 0.0262(4) Uani 1 1 d . . . H52 H 0.0165 0.1800 0.5922 0.031 Uiso 1 1 calc R . . C40 C 0.10175(7) 0.00115(14) 0.63787(6) 0.0262(4) Uani 1 1 d . . . H40 H 0.0827 0.0754 0.6405 0.031 Uiso 1 1 calc R . . C48 C -0.01417(7) 0.33297(13) 0.57267(6) 0.0216(3) Uani 1 1 d . . . C35 C 0.20722(7) -0.07056(13) 0.63145(6) 0.0245(3) Uani 1 1 d . . . H35 H 0.1917 -0.1432 0.6341 0.029 Uiso 1 1 calc R . . C46 C -0.05453(7) 0.50642(14) 0.54571(6) 0.0251(3) Uani 1 1 d . . . H46 H -0.0862 0.5465 0.5318 0.030 Uiso 1 1 calc R . . C59 C 0.60058(9) 1.15835(17) 0.60848(8) 0.0419(5) Uani 1 1 d . . . H59A H 0.6231 1.2240 0.5996 0.063 Uiso 1 1 calc R . . H59B H 0.5889 1.1165 0.5814 0.063 Uiso 1 1 calc R . . H59C H 0.6256 1.1121 0.6282 0.063 Uiso 1 1 calc R . . C50 C 0.08095(8) 0.63995(14) 0.63791(6) 0.0287(4) Uani 1 1 d . . . H50A H 0.0521 0.6954 0.6275 0.043 Uiso 1 1 calc R . . H50B H 0.1166 0.6769 0.6502 0.043 Uiso 1 1 calc R . . H50C H 0.0630 0.5945 0.6615 0.043 Uiso 1 1 calc R . . C51 C 0.12798(8) 0.63321(15) 0.56056(6) 0.0291(4) Uani 1 1 d . . . H51A H 0.1424 0.5831 0.5371 0.044 Uiso 1 1 calc R . . H51B H 0.1616 0.6751 0.5733 0.044 Uiso 1 1 calc R . . H51C H 0.0987 0.6843 0.5473 0.044 Uiso 1 1 calc R . . C55 C 0.55020(8) 0.61086(16) 0.66245(7) 0.0339(4) Uani 1 1 d . . . H55A H 0.5644 0.5390 0.6733 0.051 Uiso 1 1 calc R . . H55B H 0.5827 0.6648 0.6649 0.051 Uiso 1 1 calc R . . H55C H 0.5372 0.6045 0.6308 0.051 Uiso 1 1 calc R . . C60 C 0.49360(9) 1.31304(15) 0.60669(7) 0.0360(4) Uani 1 1 d . . . H60A H 0.4576 1.3359 0.6226 0.054 Uiso 1 1 calc R . . H60B H 0.4824 1.2855 0.5766 0.054 Uiso 1 1 calc R . . H60C H 0.5205 1.3763 0.6037 0.054 Uiso 1 1 calc R . . C56 C 0.51094(8) 0.66939(15) 0.75776(6) 0.0287(4) Uani 1 1 d . . . H56A H 0.4765 0.6861 0.7766 0.043 Uiso 1 1 calc R . . H56B H 0.5404 0.7288 0.7607 0.043 Uiso 1 1 calc R . . H56C H 0.5290 0.5997 0.7676 0.043 Uiso 1 1 calc R . . C42 C 0.07448(8) -0.05529(16) 0.59592(7) 0.0341(4) Uani 1 1 d . . . H42A H 0.0804 -0.0085 0.5694 0.051 Uiso 1 1 calc R . . H42B H 0.0316 -0.0667 0.6003 0.051 Uiso 1 1 calc R . . H42C H 0.0940 -0.1267 0.5913 0.051 Uiso 1 1 calc R . . C58 C 0.55066(8) 1.25607(15) 0.69669(6) 0.0317(4) Uani 1 1 d . . . H58A H 0.5699 1.1982 0.7148 0.048 Uiso 1 1 calc R . . H58B H 0.5139 1.2799 0.7114 0.048 Uiso 1 1 calc R . . H58C H 0.5778 1.3190 0.6940 0.048 Uiso 1 1 calc R . . C57 C 0.42486(9) 0.55284(15) 0.69522(7) 0.0337(4) Uani 1 1 d . . . H57A H 0.4397 0.4823 0.7070 0.051 Uiso 1 1 calc R . . H57B H 0.4112 0.5434 0.6639 0.051 Uiso 1 1 calc R . . H57C H 0.3915 0.5781 0.7136 0.051 Uiso 1 1 calc R . . C39 C 0.30759(9) 0.29498(15) 0.66258(7) 0.0339(4) Uani 1 1 d . . . H39A H 0.2767 0.2948 0.6857 0.051 Uiso 1 1 calc R . . H39B H 0.3236 0.3697 0.6593 0.051 Uiso 1 1 calc R . . H39C H 0.3399 0.2447 0.6716 0.051 Uiso 1 1 calc R . . C41 C 0.08871(8) -0.06203(16) 0.68121(7) 0.0345(4) Uani 1 1 d . . . H41A H 0.1069 -0.1354 0.6797 0.052 Uiso 1 1 calc R . . H41B H 0.0454 -0.0694 0.6846 0.052 Uiso 1 1 calc R . . H41C H 0.1054 -0.0218 0.7072 0.052 Uiso 1 1 calc R . . C53 C -0.03546(10) 0.14976(16) 0.53539(7) 0.0405(5) Uani 1 1 d . . . H53A H -0.0729 0.1777 0.5223 0.061 Uiso 1 1 calc R . . H53B H -0.0392 0.0705 0.5411 0.061 Uiso 1 1 calc R . . H53C H -0.0029 0.1627 0.5143 0.061 Uiso 1 1 calc R . . C38 C 0.32631(8) 0.26174(17) 0.57994(7) 0.0360(4) Uani 1 1 d . . . H38A H 0.3604 0.2146 0.5879 0.054 Uiso 1 1 calc R . . H38B H 0.3400 0.3379 0.5762 0.054 Uiso 1 1 calc R . . H38C H 0.3080 0.2357 0.5516 0.054 Uiso 1 1 calc R . . C54 C -0.07028(9) 0.18784(17) 0.61498(7) 0.0405(5) Uani 1 1 d . . . H54A H -0.0592 0.2243 0.6434 0.061 Uiso 1 1 calc R . . H54B H -0.0739 0.1083 0.6200 0.061 Uiso 1 1 calc R . . H54C H -0.1086 0.2170 0.6039 0.061 Uiso 1 1 calc R . . N2 N 0.80543(5) 0.32702(11) 0.92104(4) 0.0175(3) Uani 1 1 d . . . N1 N 0.74681(5) 0.22407(10) 0.88105(4) 0.0175(3) Uani 1 1 d . . . C1 C 0.76161(6) 0.25245(13) 0.92319(5) 0.0180(3) Uani 1 1 d . . . H1 H 0.7442 0.2247 0.9500 0.022 Uiso 1 1 calc R . . C4 C 0.70165(6) 0.14387(13) 0.86798(5) 0.0192(3) Uani 1 1 d . . . C17 C 0.88951(7) 0.35523(14) 0.97355(5) 0.0219(3) Uani 1 1 d . . . C16 C 0.83181(7) 0.38644(13) 0.95890(5) 0.0196(3) Uani 1 1 d . . . C10 C 0.62885(7) 0.30372(14) 0.85911(6) 0.0256(4) Uani 1 1 d . . . H10 H 0.6669 0.3470 0.8596 0.031 Uiso 1 1 calc R . . C2 C 0.78174(6) 0.28135(13) 0.85107(5) 0.0199(3) Uani 1 1 d . . . H2 H 0.7805 0.2760 0.8191 0.024 Uiso 1 1 calc R . . C22 C 0.73694(7) 0.50405(14) 0.96148(6) 0.0255(3) Uani 1 1 d . . . H22 H 0.7264 0.4571 0.9348 0.031 Uiso 1 1 calc R . . C21 C 0.79959(7) 0.47317(13) 0.97709(5) 0.0214(3) Uani 1 1 d . . . C5 C 0.71764(7) 0.03273(14) 0.86731(6) 0.0256(3) Uani 1 1 d . . . C25 C 0.92073(7) 0.25587(15) 0.95388(6) 0.0256(4) Uani 1 1 d . . . H25 H 0.9112 0.2537 0.9208 0.031 Uiso 1 1 calc R . . C3 C 0.81822(7) 0.34686(13) 0.87627(5) 0.0204(3) Uani 1 1 d . . . H3 H 0.8471 0.3970 0.8652 0.025 Uiso 1 1 calc R . . C9 C 0.64492(7) 0.18274(13) 0.85542(5) 0.0203(3) Uani 1 1 d . . . C18 C 0.91473(7) 0.41891(15) 1.00831(6) 0.0266(4) Uani 1 1 d . . . H18 H 0.9538 0.4021 1.0191 0.032 Uiso 1 1 calc R . . C7 C 0.61741(8) -0.00625(15) 0.84050(6) 0.0293(4) Uani 1 1 d . . . H7 H 0.5882 -0.0583 0.8309 0.035 Uiso 1 1 calc R . . C19 C 0.88419(8) 0.50510(15) 1.02709(6) 0.0291(4) Uani 1 1 d . . . H19 H 0.9025 0.5466 1.0507 0.035 Uiso 1 1 calc R . . C20 C 0.82716(8) 0.53286(14) 1.01231(6) 0.0260(4) Uani 1 1 d . . . H20 H 0.8067 0.5924 1.0260 0.031 Uiso 1 1 calc R . . C23 C 0.69217(8) 0.47946(18) 0.99842(7) 0.0390(5) Uani 1 1 d . . . H23A H 0.6942 0.4011 1.0064 0.059 Uiso 1 1 calc R . . H23B H 0.6518 0.4973 0.9875 0.059 Uiso 1 1 calc R . . H23C H 0.7017 0.5242 1.0252 0.059 Uiso 1 1 calc R . . C27 C 0.98870(7) 0.26075(19) 0.95936(7) 0.0380(5) Uani 1 1 d . . . H27A H 1.0033 0.3315 0.9479 0.057 Uiso 1 1 calc R . . H27B H 1.0067 0.2003 0.9423 0.057 Uiso 1 1 calc R . . H27C H 0.9996 0.2536 0.9914 0.057 Uiso 1 1 calc R . . C8 C 0.60338(7) 0.10446(15) 0.84147(6) 0.0257(4) Uani 1 1 d . . . H8 H 0.5645 0.1276 0.8324 0.031 Uiso 1 1 calc R . . C6 C 0.67394(8) -0.04221(15) 0.85342(7) 0.0316(4) Uani 1 1 d . . . H6 H 0.6829 -0.1188 0.8528 0.038 Uiso 1 1 calc R . . C26 C 0.89734(8) 0.14936(15) 0.97475(7) 0.0327(4) Uani 1 1 d . . . H26A H 0.9084 0.1471 1.0069 0.049 Uiso 1 1 calc R . . H26B H 0.9148 0.0859 0.9593 0.049 Uiso 1 1 calc R . . H26C H 0.8538 0.1468 0.9715 0.049 Uiso 1 1 calc R . . C13 C 0.77941(8) -0.00720(15) 0.88187(7) 0.0345(4) Uani 1 1 d . . . H13 H 0.8055 0.0591 0.8857 0.041 Uiso 1 1 calc R . . C24 C 0.73406(9) 0.62439(17) 0.94652(8) 0.0428(5) Uani 1 1 d . . . H24A H 0.7423 0.6724 0.9725 0.064 Uiso 1 1 calc R . . H24B H 0.6942 0.6405 0.9342 0.064 Uiso 1 1 calc R . . H24C H 0.7639 0.6375 0.9232 0.064 Uiso 1 1 calc R . . C11 C 0.59721(9) 0.32444(16) 0.90388(7) 0.0388(5) Uani 1 1 d . . . H11A H 0.5588 0.2859 0.9037 0.058 Uiso 1 1 calc R . . H11B H 0.5905 0.4038 0.9077 0.058 Uiso 1 1 calc R . . H11C H 0.6221 0.2970 0.9289 0.058 Uiso 1 1 calc R . . C12 C 0.59104(10) 0.34416(18) 0.81935(8) 0.0466(6) Uani 1 1 d . . . H12A H 0.6125 0.3316 0.7912 0.070 Uiso 1 1 calc R . . H12B H 0.5831 0.4232 0.8228 0.070 Uiso 1 1 calc R . . H12C H 0.5532 0.3038 0.8184 0.070 Uiso 1 1 calc R . . C14 C 0.80766(10) -0.0812(2) 0.84633(10) 0.0562(7) Uani 1 1 d . . . H14A H 0.7845 -0.1494 0.8434 0.084 Uiso 1 1 calc R . . H14B H 0.8487 -0.0989 0.8556 0.084 Uiso 1 1 calc R . . H14C H 0.8079 -0.0427 0.8172 0.084 Uiso 1 1 calc R . . C15 C 0.77602(11) -0.06470(19) 0.92742(9) 0.0509(6) Uani 1 1 d . . . H15A H 0.7599 -0.0136 0.9498 0.076 Uiso 1 1 calc R . . H15B H 0.8161 -0.0882 0.9370 0.076 Uiso 1 1 calc R . . H15C H 0.7499 -0.1293 0.9248 0.076 Uiso 1 1 calc R . . O1 O 0.21031(7) 0.15085(12) 0.74692(5) 0.0443(4) Uani 1 1 d . D . C70 C 0.24350(10) 0.04960(17) 0.74732(7) 0.0396(5) Uani 1 1 d . D . H70A H 0.2698 0.0458 0.7208 0.047 Uiso 1 1 calc R . . H70B H 0.2160 -0.0143 0.7464 0.047 Uiso 1 1 calc R . . C66 C 0.28030(9) 0.04823(17) 0.79044(7) 0.0388(5) Uani 1 1 d . . . H66A H 0.2799 -0.0258 0.8045 0.047 Uiso 1 1 calc R A 1 H66B H 0.3222 0.0695 0.7846 0.047 Uiso 1 1 calc R A 1 C68 C 0.22734(11) 0.21343(19) 0.78576(8) 0.0510(6) Uani 1 1 d . . . H68A H 0.1926 0.2542 0.7976 0.061 Uiso 1 1 calc R B 1 H68B H 0.2589 0.2672 0.7781 0.061 Uiso 1 1 calc R B 1 O2 O 0.16194(8) 0.03594(15) 0.90448(6) 0.0655(5) Uani 1 1 d . . . C72 C 0.21131(11) 0.1618(2) 0.95164(9) 0.0539(6) Uani 1 1 d . . . H72A H 0.2279 0.2194 0.9317 0.065 Uiso 1 1 calc R . . H72B H 0.2324 0.1642 0.9812 0.065 Uiso 1 1 calc R . . C71 C 0.21584(12) 0.0489(2) 0.93033(10) 0.0639(8) Uani 1 1 d . . . H71A H 0.2511 0.0445 0.9106 0.077 Uiso 1 1 calc R . . H71B H 0.2192 -0.0090 0.9538 0.077 Uiso 1 1 calc R . . C74 C 0.11616(11) 0.0909(2) 0.92874(9) 0.0548(6) Uani 1 1 d . . . H74A H 0.0945 0.0375 0.9478 0.066 Uiso 1 1 calc R . . H74B H 0.0872 0.1250 0.9074 0.066 Uiso 1 1 calc R . . C73 C 0.14429(12) 0.1762(3) 0.95712(14) 0.1008(14) Uani 1 1 d . . . H73A H 0.1331 0.1664 0.9891 0.121 Uiso 1 1 calc R . . H73B H 0.1316 0.2506 0.9471 0.121 Uiso 1 1 calc R . . C65 C 0.71553(10) 0.1359(2) 0.73772(8) 0.0561(7) Uani 1 1 d . C . H65A H 0.6809 0.1670 0.7209 0.067 Uiso 1 1 calc R . . H65B H 0.7008 0.1004 0.7656 0.067 Uiso 1 1 calc R . . O3 O 0.75705(7) 0.22116(16) 0.74899(6) 0.0600(5) Uani 1 1 d . C . C63B C 0.79896(17) 0.1197(4) 0.69118(16) 0.0551(15) Uani 0.692(11) 1 d P C 1 H63A H 0.8332 0.0710 0.6844 0.066 Uiso 0.692(11) 1 calc PR C 1 H63B H 0.7875 0.1616 0.6637 0.066 Uiso 0.692(11) 1 calc PR C 1 C63A C 0.8141(5) 0.0816(9) 0.7222(7) 0.096(6) Uani 0.308(11) 1 d P C 2 H63C H 0.8273 0.0419 0.7498 0.115 Uiso 0.308(11) 1 calc PR C 2 H63D H 0.8409 0.0626 0.6971 0.115 Uiso 0.308(11) 1 calc PR C 2 C64 C 0.74634(14) 0.0547(3) 0.70975(13) 0.0883(11) Uani 1 1 d . . . H64A H 0.7200 0.0276 0.6850 0.106 Uiso 1 1 calc R C 1 H64B H 0.7603 -0.0088 0.7281 0.106 Uiso 1 1 calc R C 1 C62 C 0.81226(11) 0.1930(3) 0.72925(9) 0.0663(8) Uani 1 1 d . . . H62A H 0.8384 0.1552 0.7516 0.080 Uiso 1 1 calc R C 1 H62B H 0.8329 0.2602 0.7187 0.080 Uiso 1 1 calc R C 1 C67B C 0.25029(13) 0.1319(3) 0.82024(10) 0.0347(9) Uani 0.682(7) 1 d P D 1 H67A H 0.2173 0.0985 0.8374 0.042 Uiso 0.682(7) 1 calc PR D 1 H67B H 0.2791 0.1666 0.8416 0.042 Uiso 0.682(7) 1 calc PR D 1 C67A C 0.2804(4) 0.1706(6) 0.7991(3) 0.045(3) Uani 0.318(7) 1 d P D 2 H67C H 0.2872 0.1849 0.8317 0.054 Uiso 0.318(7) 1 calc PR D 2 H67D H 0.3131 0.2059 0.7822 0.054 Uiso 0.318(7) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.02583(19) 0.0339(2) 0.0241(2) 0.00129(17) 0.00605(15) 0.00762(16) P3 0.01799(18) 0.0239(2) 0.0180(2) 0.00155(16) -0.00173(15) -0.00181(15) P2 0.01712(18) 0.0231(2) 0.0190(2) -0.00180(16) 0.00394(15) -0.00041(15) P4 0.01756(18) 0.0227(2) 0.0239(2) -0.00025(16) 0.00385(15) 0.00204(15) Si2 0.0235(2) 0.0230(2) 0.0225(2) 0.00081(18) 0.00201(18) -0.00391(17) P6 0.02077(19) 0.0253(2) 0.0161(2) -0.00103(16) 0.00062(15) -0.00332(15) Si1 0.0240(2) 0.0212(2) 0.0232(2) -0.00072(18) 0.00277(18) -0.00112(17) P7 0.01458(17) 0.0271(2) 0.0237(2) 0.00186(17) -0.00130(15) -0.00109(15) P1 0.01905(18) 0.0218(2) 0.0198(2) -0.00188(16) -0.00053(15) -0.00311(15) P5 0.01632(18) 0.0242(2) 0.0213(2) -0.00026(16) 0.00390(15) -0.00296(15) N4 0.0149(5) 0.0151(6) 0.0174(6) -0.0007(5) 0.0004(5) 0.0014(4) N3 0.0127(5) 0.0147(6) 0.0192(6) -0.0003(5) 0.0008(5) 0.0009(4) C32 0.0153(6) 0.0219(8) 0.0169(7) 0.0000(6) 0.0006(5) 0.0022(5) C37 0.0143(7) 0.0232(8) 0.0277(9) 0.0052(6) 0.0017(6) 0.0004(6) C33 0.0175(7) 0.0287(9) 0.0218(8) 0.0006(7) 0.0013(6) 0.0066(6) C30 0.0190(7) 0.0194(8) 0.0171(7) -0.0008(6) 0.0021(6) 0.0022(5) C31 0.0163(6) 0.0172(7) 0.0171(7) -0.0006(6) 0.0003(5) 0.0043(5) C44 0.0200(7) 0.0208(8) 0.0187(8) -0.0012(6) 0.0015(6) 0.0037(6) C36 0.0194(7) 0.0185(8) 0.0245(8) -0.0021(6) 0.0005(6) 0.0009(6) C34 0.0261(8) 0.0231(8) 0.0241(8) -0.0021(7) 0.0003(6) 0.0097(6) C43 0.0155(6) 0.0185(7) 0.0167(7) 0.0003(6) 0.0005(5) 0.0050(5) C49 0.0249(8) 0.0173(8) 0.0275(9) 0.0013(6) -0.0019(6) 0.0011(6) C47 0.0175(7) 0.0331(9) 0.0243(8) 0.0003(7) -0.0031(6) 0.0025(6) C45 0.0273(8) 0.0203(8) 0.0241(8) 0.0019(6) 0.0015(6) 0.0087(6) C29 0.0187(7) 0.0178(7) 0.0167(7) -0.0015(6) 0.0004(6) 0.0010(5) C28 0.0149(6) 0.0149(7) 0.0195(7) -0.0018(6) 0.0012(5) 0.0004(5) C52 0.0204(7) 0.0237(8) 0.0343(10) 0.0024(7) -0.0074(7) -0.0037(6) C40 0.0203(7) 0.0169(8) 0.0415(10) -0.0026(7) 0.0034(7) -0.0015(6) C48 0.0191(7) 0.0235(8) 0.0223(8) 0.0002(6) -0.0004(6) 0.0008(6) C35 0.0257(8) 0.0187(8) 0.0292(9) -0.0021(7) 0.0012(7) 0.0028(6) C46 0.0221(8) 0.0311(9) 0.0222(8) 0.0019(7) -0.0002(6) 0.0106(7) C59 0.0369(10) 0.0341(11) 0.0554(14) -0.0022(9) 0.0213(9) -0.0079(8) C50 0.0354(9) 0.0231(9) 0.0275(9) -0.0007(7) -0.0011(7) -0.0023(7) C51 0.0314(9) 0.0250(9) 0.0308(10) 0.0002(7) 0.0035(7) -0.0045(7) C55 0.0379(10) 0.0272(10) 0.0370(11) 0.0025(8) 0.0111(8) 0.0063(8) C60 0.0484(11) 0.0270(10) 0.0324(10) 0.0055(8) -0.0048(9) -0.0045(8) C56 0.0313(9) 0.0278(9) 0.0270(9) 0.0040(7) -0.0014(7) 0.0019(7) C42 0.0273(9) 0.0288(10) 0.0461(12) 0.0008(8) -0.0044(8) -0.0057(7) C58 0.0359(9) 0.0287(9) 0.0303(10) -0.0011(7) -0.0043(8) -0.0098(7) C57 0.0376(10) 0.0274(9) 0.0360(11) 0.0042(8) -0.0012(8) -0.0099(8) C39 0.0377(10) 0.0260(9) 0.0378(11) -0.0024(8) -0.0029(8) -0.0051(8) C41 0.0313(9) 0.0330(10) 0.0394(11) -0.0052(8) 0.0111(8) -0.0052(8) C53 0.0489(12) 0.0288(10) 0.0436(12) -0.0061(9) -0.0054(10) -0.0051(9) C38 0.0302(9) 0.0400(11) 0.0381(11) 0.0035(9) 0.0103(8) -0.0060(8) C54 0.0446(11) 0.0365(11) 0.0404(12) 0.0058(9) 0.0006(9) -0.0131(9) N2 0.0135(5) 0.0219(7) 0.0170(6) 0.0021(5) -0.0006(5) -0.0026(5) N1 0.0139(5) 0.0193(6) 0.0191(7) 0.0002(5) 0.0003(5) -0.0011(5) C1 0.0142(6) 0.0218(8) 0.0179(7) 0.0021(6) 0.0001(5) -0.0010(5) C4 0.0165(7) 0.0213(8) 0.0199(8) -0.0020(6) 0.0009(6) -0.0029(6) C17 0.0156(7) 0.0304(9) 0.0198(8) 0.0065(6) -0.0008(6) -0.0045(6) C16 0.0181(7) 0.0250(8) 0.0156(7) 0.0036(6) -0.0013(6) -0.0062(6) C10 0.0179(7) 0.0243(8) 0.0345(10) -0.0017(7) -0.0044(7) 0.0001(6) C2 0.0175(7) 0.0249(8) 0.0175(8) 0.0018(6) 0.0017(6) -0.0002(6) C22 0.0221(8) 0.0265(9) 0.0277(9) -0.0033(7) -0.0041(6) 0.0016(6) C21 0.0208(7) 0.0237(8) 0.0197(8) 0.0041(6) -0.0032(6) -0.0047(6) C5 0.0221(8) 0.0230(8) 0.0318(9) -0.0029(7) 0.0020(7) 0.0000(6) C25 0.0174(7) 0.0390(10) 0.0204(8) 0.0035(7) -0.0001(6) 0.0027(7) C3 0.0168(7) 0.0258(8) 0.0188(8) 0.0032(6) 0.0022(6) -0.0027(6) C9 0.0165(7) 0.0243(8) 0.0202(8) -0.0015(6) 0.0004(6) -0.0008(6) C18 0.0219(8) 0.0349(10) 0.0230(9) 0.0074(7) -0.0055(6) -0.0072(7) C7 0.0267(8) 0.0292(9) 0.0321(10) -0.0073(7) 0.0009(7) -0.0089(7) C19 0.0311(9) 0.0322(10) 0.0237(9) 0.0018(7) -0.0087(7) -0.0127(7) C20 0.0317(9) 0.0245(9) 0.0218(8) -0.0001(7) -0.0035(7) -0.0047(7) C23 0.0265(9) 0.0488(12) 0.0417(12) 0.0030(9) 0.0015(8) 0.0005(8) C27 0.0199(8) 0.0646(14) 0.0294(10) 0.0054(9) -0.0005(7) 0.0069(8) C8 0.0182(7) 0.0327(9) 0.0262(9) -0.0037(7) -0.0011(6) -0.0027(6) C6 0.0314(9) 0.0226(9) 0.0408(11) -0.0046(8) 0.0011(8) -0.0026(7) C26 0.0303(9) 0.0325(10) 0.0353(11) 0.0026(8) 0.0022(8) 0.0064(7) C13 0.0249(8) 0.0222(9) 0.0563(13) -0.0018(8) -0.0035(8) 0.0040(7) C24 0.0375(11) 0.0372(11) 0.0534(14) 0.0136(10) -0.0118(10) 0.0028(9) C11 0.0398(11) 0.0301(10) 0.0465(13) -0.0071(9) 0.0073(9) 0.0094(8) C12 0.0511(13) 0.0379(12) 0.0500(14) 0.0033(10) -0.0210(11) 0.0089(10) C14 0.0351(11) 0.0496(14) 0.0840(19) -0.0129(13) 0.0074(12) 0.0147(10) C15 0.0474(12) 0.0416(13) 0.0634(16) 0.0105(11) -0.0109(11) 0.0114(10) O1 0.0597(9) 0.0428(8) 0.0300(7) -0.0042(6) -0.0149(7) 0.0214(7) C70 0.0497(12) 0.0382(11) 0.0306(10) -0.0059(8) -0.0051(9) 0.0124(9) C66 0.0430(11) 0.0332(10) 0.0399(12) -0.0005(9) -0.0076(9) 0.0070(8) C68 0.0666(15) 0.0380(12) 0.0479(14) -0.0149(10) -0.0182(12) 0.0210(11) O2 0.0644(11) 0.0594(11) 0.0716(12) -0.0280(9) -0.0332(10) 0.0306(9) C72 0.0472(13) 0.0502(14) 0.0642(17) -0.0218(12) -0.0039(12) 0.0040(11) C71 0.0611(15) 0.0499(14) 0.0797(19) -0.0201(13) -0.0380(14) 0.0195(12) C74 0.0585(15) 0.0456(13) 0.0601(16) -0.0075(12) -0.0102(12) 0.0107(11) C73 0.0450(15) 0.114(3) 0.143(3) -0.090(3) -0.0034(18) 0.0003(16) C65 0.0368(11) 0.0846(19) 0.0469(14) -0.0224(13) 0.0056(10) -0.0233(12) O3 0.0501(9) 0.0803(12) 0.0497(10) -0.0291(9) 0.0053(8) -0.0189(9) C63B 0.049(2) 0.066(3) 0.050(3) -0.008(2) 0.0199(18) 0.0068(18) C63A 0.076(8) 0.057(7) 0.156(17) 0.027(7) 0.057(9) 0.025(5) C64 0.073(2) 0.076(2) 0.117(3) -0.048(2) 0.0226(19) -0.0285(17) C62 0.0437(13) 0.102(2) 0.0535(16) 0.0008(15) 0.0087(12) -0.0271(14) C67B 0.0247(14) 0.055(2) 0.0239(15) -0.0039(13) -0.0017(11) -0.0049(13) C67A 0.042(4) 0.043(4) 0.050(5) -0.014(3) -0.022(4) 0.005(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 P3 P4 2.1931(6) . ? P3 P2 2.2020(6) . ? P3 Si2 2.2738(6) . ? P2 P7 2.1360(6) . ? P2 P1 2.2070(6) . ? P4 P5 2.2192(6) . ? P4 P6 2.2352(6) . ? Si2 C58 1.8632(18) . ? Si2 C59 1.869(2) . ? Si2 C60 1.8693(19) . ? P6 P7 2.1345(6) . ? P6 P5 2.2480(6) . ? Si1 C56 1.8656(18) . ? Si1 C57 1.8662(18) . ? Si1 C55 1.8713(19) . ? Si1 P1 2.2816(6) . ? P1 P5 2.1876(6) . ? N4 C28 1.3385(18) . ? N4 C30 1.3801(19) . ? N4 C43 1.4529(18) . ? N3 C28 1.3339(18) . ? N3 C29 1.3833(19) . ? N3 C31 1.4551(18) . ? C32 C31 1.395(2) . ? C32 C33 1.398(2) . ? C32 C37 1.513(2) . ? C37 C38 1.526(2) . ? C37 C39 1.530(2) . ? C37 H37 1.0000 . ? C33 C34 1.380(2) . ? C33 H33 0.9500 . ? C30 C29 1.356(2) . ? C30 H30 0.9500 . ? C31 C36 1.393(2) . ? C44 C43 1.392(2) . ? C44 C45 1.398(2) . ? C44 C49 1.518(2) . ? C36 C35 1.396(2) . ? C36 C40 1.516(2) . ? C34 C35 1.387(2) . ? C34 H34 0.9500 . ? C43 C48 1.398(2) . ? C49 C51 1.529(2) . ? C49 C50 1.538(2) . ? C49 H49 1.0000 . ? C47 C46 1.374(2) . ? C47 C48 1.396(2) . ? C47 H47 0.9500 . ? C45 C46 1.384(2) . ? C45 H45 0.9500 . ? C29 H29 0.9500 . ? C28 H28 0.9500 . ? C52 C48 1.521(2) . ? C52 C53 1.528(3) . ? C52 C54 1.533(3) . ? C52 H52 1.0000 . ? C40 C41 1.526(3) . ? C40 C42 1.537(3) . ? C40 H40 1.0000 . ? C35 H35 0.9500 . ? C46 H46 0.9500 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? N2 C1 1.3367(19) . ? N2 C3 1.381(2) . ? N2 C16 1.4511(19) . ? N1 C1 1.3315(19) . ? N1 C2 1.379(2) . ? N1 C4 1.4516(19) . ? C1 H1 0.9500 . ? C4 C5 1.395(2) . ? C4 C9 1.401(2) . ? C17 C18 1.399(2) . ? C17 C16 1.409(2) . ? C17 C25 1.514(2) . ? C16 C21 1.388(2) . ? C10 C9 1.515(2) . ? C10 C12 1.521(2) . ? C10 C11 1.532(3) . ? C10 H10 1.0000 . ? C2 C3 1.356(2) . ? C2 H2 0.9500 . ? C22 C21 1.518(2) . ? C22 C23 1.524(3) . ? C22 C24 1.526(3) . ? C22 H22 1.0000 . ? C21 C20 1.405(2) . ? C5 C6 1.393(2) . ? C5 C13 1.522(2) . ? C25 C26 1.527(3) . ? C25 C27 1.530(2) . ? C25 H25 1.0000 . ? C3 H3 0.9500 . ? C9 C8 1.388(2) . ? C18 C19 1.371(3) . ? C18 H18 0.9500 . ? C7 C8 1.379(2) . ? C7 C6 1.388(2) . ? C7 H7 0.9500 . ? C19 C20 1.386(2) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C8 H8 0.9500 . ? C6 H6 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C13 C15 1.521(3) . ? C13 C14 1.527(3) . ? C13 H13 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? O1 C68 1.425(2) . ? O1 C70 1.435(2) . ? C70 C66 1.509(3) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C66 C67A 1.505(7) . ? C66 C67B 1.509(4) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C68 C67A 1.351(7) . ? C68 C67B 1.506(4) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? O2 C74 1.426(3) . ? O2 C71 1.429(3) . ? C72 C71 1.511(3) . ? C72 C73 1.522(3) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C74 C73 1.468(3) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C65 O3 1.427(3) . ? C65 C64 1.465(4) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? O3 C62 1.417(3) . ? C63B C62 1.462(5) . ? C63B C64 1.527(5) . ? C63B H63A 0.9900 . ? C63B H63B 0.9900 . ? C63A C62 1.367(11) . ? C63A C64 1.591(15) . ? C63A H63C 0.9900 . ? C63A H63D 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C67B H67A 0.9900 . ? C67B H67B 0.9900 . ? C67A H67C 0.9900 . ? C67A H67D 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 P4 P3 P2 100.67(2) . . ? P4 P3 Si2 100.28(2) . . ? P2 P3 Si2 103.21(2) . . ? P7 P2 P3 106.37(2) . . ? P7 P2 P1 106.60(2) . . ? P3 P2 P1 88.10(2) . . ? P3 P4 P5 100.40(2) . . ? P3 P4 P6 103.81(2) . . ? P5 P4 P6 60.618(18) . . ? C58 Si2 C59 111.85(10) . . ? C58 Si2 C60 107.93(9) . . ? C59 Si2 C60 108.99(10) . . ? C58 Si2 P3 113.77(6) . . ? C59 Si2 P3 107.82(7) . . ? C60 Si2 P3 106.26(6) . . ? P7 P6 P4 109.27(2) . . ? P7 P6 P5 108.71(2) . . ? P4 P6 P5 59.338(18) . . ? C56 Si1 C57 107.35(9) . . ? C56 Si1 C55 109.45(9) . . ? C57 Si1 C55 110.20(9) . . ? C56 Si1 P1 116.20(6) . . ? C57 Si1 P1 106.17(6) . . ? C55 Si1 P1 107.38(6) . . ? P6 P7 P2 98.33(2) . . ? P5 P1 P2 100.07(2) . . ? P5 P1 Si1 99.93(2) . . ? P2 P1 Si1 103.84(2) . . ? P1 P5 P4 101.88(2) . . ? P1 P5 P6 104.32(2) . . ? P4 P5 P6 60.044(18) . . ? C28 N4 C30 109.15(12) . . ? C28 N4 C43 126.55(13) . . ? C30 N4 C43 124.11(12) . . ? C28 N3 C29 109.59(12) . . ? C28 N3 C31 125.67(13) . . ? C29 N3 C31 123.89(12) . . ? C31 C32 C33 116.36(14) . . ? C31 C32 C37 122.66(13) . . ? C33 C32 C37 120.96(13) . . ? C32 C37 C38 111.20(14) . . ? C32 C37 C39 110.30(13) . . ? C38 C37 C39 111.15(14) . . ? C32 C37 H37 108.0 . . ? C38 C37 H37 108.0 . . ? C39 C37 H37 108.0 . . ? C34 C33 C32 121.44(14) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C29 C30 N4 107.20(13) . . ? C29 C30 H30 126.4 . . ? N4 C30 H30 126.4 . . ? C36 C31 C32 124.28(14) . . ? C36 C31 N3 116.55(13) . . ? C32 C31 N3 119.11(13) . . ? C43 C44 C45 116.72(14) . . ? C43 C44 C49 122.93(13) . . ? C45 C44 C49 120.31(14) . . ? C31 C36 C35 116.64(14) . . ? C31 C36 C40 123.01(14) . . ? C35 C36 C40 120.35(14) . . ? C33 C34 C35 120.19(15) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C44 C43 C48 123.60(13) . . ? C44 C43 N4 118.13(13) . . ? C48 C43 N4 118.08(13) . . ? C44 C49 C51 112.04(14) . . ? C44 C49 C50 109.33(14) . . ? C51 C49 C50 111.51(14) . . ? C44 C49 H49 107.9 . . ? C51 C49 H49 107.9 . . ? C50 C49 H49 107.9 . . ? C46 C47 C48 121.79(15) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C46 C45 C44 121.49(15) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C30 C29 N3 106.47(13) . . ? C30 C29 H29 126.8 . . ? N3 C29 H29 126.8 . . ? N3 C28 N4 107.58(13) . . ? N3 C28 H28 126.2 . . ? N4 C28 H28 126.2 . . ? C48 C52 C53 111.67(15) . . ? C48 C52 C54 110.40(15) . . ? C53 C52 C54 111.76(15) . . ? C48 C52 H52 107.6 . . ? C53 C52 H52 107.6 . . ? C54 C52 H52 107.6 . . ? C36 C40 C41 111.61(14) . . ? C36 C40 C42 110.56(15) . . ? C41 C40 C42 112.15(14) . . ? C36 C40 H40 107.4 . . ? C41 C40 H40 107.4 . . ? C42 C40 H40 107.4 . . ? C47 C48 C43 116.64(15) . . ? C47 C48 C52 120.09(14) . . ? C43 C48 C52 123.26(14) . . ? C34 C35 C36 121.08(15) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C47 C46 C45 119.75(14) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? Si2 C59 H59A 109.5 . . ? Si2 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? Si2 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si1 C55 H55A 109.5 . . ? Si1 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? Si1 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? Si2 C60 H60A 109.5 . . ? Si2 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? Si2 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? Si1 C56 H56A 109.5 . . ? Si1 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? Si1 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si2 C58 H58A 109.5 . . ? Si2 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? Si2 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? Si1 C57 H57A 109.5 . . ? Si1 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? Si1 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C1 N2 C3 109.04(13) . . ? C1 N2 C16 126.18(13) . . ? C3 N2 C16 124.53(13) . . ? C1 N1 C2 109.67(12) . . ? C1 N1 C4 125.88(13) . . ? C2 N1 C4 124.44(13) . . ? N1 C1 N2 107.66(13) . . ? N1 C1 H1 126.2 . . ? N2 C1 H1 126.2 . . ? C5 C4 C9 123.62(14) . . ? C5 C4 N1 118.24(13) . . ? C9 C4 N1 118.12(14) . . ? C18 C17 C16 115.92(15) . . ? C18 C17 C25 122.57(14) . . ? C16 C17 C25 121.47(14) . . ? C21 C16 C17 124.31(14) . . ? C21 C16 N2 117.86(13) . . ? C17 C16 N2 117.77(14) . . ? C9 C10 C12 112.74(15) . . ? C9 C10 C11 109.55(15) . . ? C12 C10 C11 110.92(16) . . ? C9 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C3 C2 N1 106.52(14) . . ? C3 C2 H2 126.7 . . ? N1 C2 H2 126.7 . . ? C21 C22 C23 110.39(14) . . ? C21 C22 C24 111.05(14) . . ? C23 C22 C24 111.71(16) . . ? C21 C22 H22 107.8 . . ? C23 C22 H22 107.8 . . ? C24 C22 H22 107.8 . . ? C16 C21 C20 116.91(14) . . ? C16 C21 C22 123.52(14) . . ? C20 C21 C22 119.56(15) . . ? C6 C5 C4 117.06(15) . . ? C6 C5 C13 120.53(16) . . ? C4 C5 C13 122.40(15) . . ? C17 C25 C26 110.75(14) . . ? C17 C25 C27 113.13(15) . . ? C26 C25 C27 109.65(15) . . ? C17 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C2 C3 N2 107.11(13) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? C8 C9 C4 116.78(15) . . ? C8 C9 C10 121.65(14) . . ? C4 C9 C10 121.50(14) . . ? C19 C18 C17 121.35(15) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C8 C7 C6 120.49(16) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C18 C19 C20 121.34(16) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C21 120.17(17) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C7 C8 C9 121.33(15) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C7 C6 C5 120.72(17) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C15 C13 C5 109.89(17) . . ? C15 C13 C14 111.59(18) . . ? C5 C13 C14 112.07(17) . . ? C15 C13 H13 107.7 . . ? C5 C13 H13 107.7 . . ? C14 C13 H13 107.7 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C68 O1 C70 108.44(14) . . ? O1 C70 C66 107.03(16) . . ? O1 C70 H70A 110.3 . . ? C66 C70 H70A 110.3 . . ? O1 C70 H70B 110.3 . . ? C66 C70 H70B 110.3 . . ? H70A C70 H70B 108.6 . . ? C67A C66 C67B 40.3(4) . . ? C67A C66 C70 97.6(3) . . ? C67B C66 C70 104.15(17) . . ? C67A C66 H66A 145.3 . . ? C67B C66 H66A 110.9 . . ? C70 C66 H66A 110.9 . . ? C67A C66 H66B 76.9 . . ? C67B C66 H66B 110.9 . . ? C70 C66 H66B 110.9 . . ? H66A C66 H66B 108.9 . . ? C67A C68 O1 104.8(3) . . ? C67A C68 C67B 42.2(4) . . ? O1 C68 C67B 106.38(19) . . ? C67A C68 H68A 141.3 . . ? O1 C68 H68A 110.5 . . ? C67B C68 H68A 110.5 . . ? C67A C68 H68B 72.1 . . ? O1 C68 H68B 110.5 . . ? C67B C68 H68B 110.5 . . ? H68A C68 H68B 108.6 . . ? C74 O2 C71 106.69(19) . . ? C71 C72 C73 102.7(2) . . ? C71 C72 H72A 111.2 . . ? C73 C72 H72A 111.2 . . ? C71 C72 H72B 111.2 . . ? C73 C72 H72B 111.2 . . ? H72A C72 H72B 109.1 . . ? O2 C71 C72 105.18(18) . . ? O2 C71 H71A 110.7 . . ? C72 C71 H71A 110.7 . . ? O2 C71 H71B 110.7 . . ? C72 C71 H71B 110.7 . . ? H71A C71 H71B 108.8 . . ? O2 C74 C73 108.1(2) . . ? O2 C74 H74A 110.1 . . ? C73 C74 H74A 110.1 . . ? O2 C74 H74B 110.1 . . ? C73 C74 H74B 110.1 . . ? H74A C74 H74B 108.4 . . ? C74 C73 C72 105.9(2) . . ? C74 C73 H73A 110.6 . . ? C72 C73 H73A 110.6 . . ? C74 C73 H73B 110.6 . . ? C72 C73 H73B 110.6 . . ? H73A C73 H73B 108.7 . . ? O3 C65 C64 107.94(19) . . ? O3 C65 H65A 110.1 . . ? C64 C65 H65A 110.1 . . ? O3 C65 H65B 110.1 . . ? C64 C65 H65B 110.1 . . ? H65A C65 H65B 108.4 . . ? C62 O3 C65 107.38(19) . . ? C62 C63B C64 100.7(3) . . ? C62 C63B H63A 111.6 . . ? C64 C63B H63A 111.6 . . ? C62 C63B H63B 111.6 . . ? C64 C63B H63B 111.6 . . ? H63A C63B H63B 109.4 . . ? C62 C63A C64 102.0(8) . . ? C62 C63A H63C 111.4 . . ? C64 C63A H63C 111.4 . . ? C62 C63A H63D 111.4 . . ? C64 C63A H63D 111.4 . . ? H63C C63A H63D 109.2 . . ? C65 C64 C63B 103.2(2) . . ? C65 C64 C63A 100.8(5) . . ? C63B C64 C63A 40.4(6) . . ? C65 C64 H64A 111.1 . . ? C63B C64 H64A 111.1 . . ? C63A C64 H64A 142.8 . . ? C65 C64 H64B 111.1 . . ? C63B C64 H64B 111.1 . . ? C63A C64 H64B 74.9 . . ? H64A C64 H64B 109.1 . . ? C63A C62 O3 109.2(5) . . ? C63A C62 C63B 44.7(8) . . ? O3 C62 C63B 107.1(2) . . ? C63A C62 H62A 68.0 . . ? O3 C62 H62A 110.3 . . ? C63B C62 H62A 110.3 . . ? C63A C62 H62B 138.5 . . ? O3 C62 H62B 110.3 . . ? C63B C62 H62B 110.3 . . ? H62A C62 H62B 108.5 . . ? C68 C67B C66 101.3(2) . . ? C68 C67B H67A 111.5 . . ? C66 C67B H67A 111.5 . . ? C68 C67B H67B 111.5 . . ? C66 C67B H67B 111.5 . . ? H67A C67B H67B 109.3 . . ? C68 C67A C66 109.3(5) . . ? C68 C67A H67C 109.8 . . ? C66 C67A H67C 109.8 . . ? C68 C67A H67D 109.8 . . ? C66 C67A H67D 109.8 . . ? H67C C67A H67D 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 P4 P3 P2 P7 -43.14(3) . . . . ? Si2 P3 P2 P7 60.21(3) . . . . ? P4 P3 P2 P1 63.61(2) . . . . ? Si2 P3 P2 P1 166.96(2) . . . . ? P2 P3 P4 P5 -41.19(2) . . . . ? Si2 P3 P4 P5 -146.89(2) . . . . ? P2 P3 P4 P6 20.87(3) . . . . ? Si2 P3 P4 P6 -84.83(2) . . . . ? P4 P3 Si2 C58 18.46(7) . . . . ? P2 P3 Si2 C58 -85.18(7) . . . . ? P4 P3 Si2 C59 143.12(8) . . . . ? P2 P3 Si2 C59 39.48(8) . . . . ? P4 P3 Si2 C60 -100.15(7) . . . . ? P2 P3 Si2 C60 156.21(7) . . . . ? P3 P4 P6 P7 6.53(3) . . . . ? P5 P4 P6 P7 100.82(3) . . . . ? P3 P4 P6 P5 -94.30(2) . . . . ? P4 P6 P7 P2 -31.62(3) . . . . ? P5 P6 P7 P2 31.51(3) . . . . ? P3 P2 P7 P6 46.20(3) . . . . ? P1 P2 P7 P6 -46.75(3) . . . . ? P7 P2 P1 P5 43.66(3) . . . . ? P3 P2 P1 P5 -62.86(2) . . . . ? P7 P2 P1 Si1 -59.30(3) . . . . ? P3 P2 P1 Si1 -165.81(2) . . . . ? C56 Si1 P1 P5 -26.30(7) . . . . ? C57 Si1 P1 P5 92.96(7) . . . . ? C55 Si1 P1 P5 -149.18(7) . . . . ? C56 Si1 P1 P2 76.76(7) . . . . ? C57 Si1 P1 P2 -163.98(7) . . . . ? C55 Si1 P1 P2 -46.11(7) . . . . ? P2 P1 P5 P4 40.51(3) . . . . ? Si1 P1 P5 P4 146.63(2) . . . . ? P2 P1 P5 P6 -21.27(3) . . . . ? Si1 P1 P5 P6 84.86(2) . . . . ? P3 P4 P5 P1 0.27(3) . . . . ? P6 P4 P5 P1 -99.81(2) . . . . ? P3 P4 P5 P6 100.09(2) . . . . ? P7 P6 P5 P1 -6.15(3) . . . . ? P4 P6 P5 P1 95.63(2) . . . . ? P7 P6 P5 P4 -101.79(3) . . . . ? C31 C32 C37 C38 -135.43(16) . . . . ? C33 C32 C37 C38 46.1(2) . . . . ? C31 C32 C37 C39 100.78(17) . . . . ? C33 C32 C37 C39 -77.67(19) . . . . ? C31 C32 C33 C34 0.7(2) . . . . ? C37 C32 C33 C34 179.25(15) . . . . ? C28 N4 C30 C29 0.32(17) . . . . ? C43 N4 C30 C29 175.65(13) . . . . ? C33 C32 C31 C36 -0.4(2) . . . . ? C37 C32 C31 C36 -178.87(15) . . . . ? C33 C32 C31 N3 176.55(13) . . . . ? C37 C32 C31 N3 -2.0(2) . . . . ? C28 N3 C31 C36 -87.31(18) . . . . ? C29 N3 C31 C36 81.02(18) . . . . ? C28 N3 C31 C32 95.54(18) . . . . ? C29 N3 C31 C32 -96.13(18) . . . . ? C32 C31 C36 C35 -0.6(2) . . . . ? N3 C31 C36 C35 -177.61(14) . . . . ? C32 C31 C36 C40 179.36(15) . . . . ? N3 C31 C36 C40 2.4(2) . . . . ? C32 C33 C34 C35 -0.1(3) . . . . ? C45 C44 C43 C48 -0.2(2) . . . . ? C49 C44 C43 C48 177.36(15) . . . . ? C45 C44 C43 N4 -175.16(14) . . . . ? C49 C44 C43 N4 2.4(2) . . . . ? C28 N4 C43 C44 -109.08(17) . . . . ? C30 N4 C43 C44 76.41(19) . . . . ? C28 N4 C43 C48 75.7(2) . . . . ? C30 N4 C43 C48 -98.81(18) . . . . ? C43 C44 C49 C51 126.28(16) . . . . ? C45 C44 C49 C51 -56.2(2) . . . . ? C43 C44 C49 C50 -109.58(17) . . . . ? C45 C44 C49 C50 67.91(19) . . . . ? C43 C44 C45 C46 0.9(2) . . . . ? C49 C44 C45 C46 -176.73(16) . . . . ? N4 C30 C29 N3 -0.53(16) . . . . ? C28 N3 C29 C30 0.58(16) . . . . ? C31 N3 C29 C30 -169.37(13) . . . . ? C29 N3 C28 N4 -0.39(16) . . . . ? C31 N3 C28 N4 169.34(13) . . . . ? C30 N4 C28 N3 0.04(16) . . . . ? C43 N4 C28 N3 -175.14(13) . . . . ? C31 C36 C40 C41 -123.21(17) . . . . ? C35 C36 C40 C41 56.8(2) . . . . ? C31 C36 C40 C42 111.21(18) . . . . ? C35 C36 C40 C42 -68.8(2) . . . . ? C46 C47 C48 C43 0.4(2) . . . . ? C46 C47 C48 C52 179.04(16) . . . . ? C44 C43 C48 C47 -0.4(2) . . . . ? N4 C43 C48 C47 174.52(14) . . . . ? C44 C43 C48 C52 -179.01(16) . . . . ? N4 C43 C48 C52 -4.1(2) . . . . ? C53 C52 C48 C47 57.0(2) . . . . ? C54 C52 C48 C47 -68.0(2) . . . . ? C53 C52 C48 C43 -124.46(18) . . . . ? C54 C52 C48 C43 110.55(18) . . . . ? C33 C34 C35 C36 -1.0(3) . . . . ? C31 C36 C35 C34 1.3(2) . . . . ? C40 C36 C35 C34 -178.69(16) . . . . ? C48 C47 C46 C45 0.3(3) . . . . ? C44 C45 C46 C47 -1.0(3) . . . . ? C2 N1 C1 N2 0.04(17) . . . . ? C4 N1 C1 N2 179.03(13) . . . . ? C3 N2 C1 N1 0.52(17) . . . . ? C16 N2 C1 N1 174.93(13) . . . . ? C1 N1 C4 C5 -84.0(2) . . . . ? C2 N1 C4 C5 94.87(19) . . . . ? C1 N1 C4 C9 97.92(19) . . . . ? C2 N1 C4 C9 -83.23(19) . . . . ? C18 C17 C16 C21 -1.0(2) . . . . ? C25 C17 C16 C21 176.66(15) . . . . ? C18 C17 C16 N2 176.26(14) . . . . ? C25 C17 C16 N2 -6.1(2) . . . . ? C1 N2 C16 C21 -76.4(2) . . . . ? C3 N2 C16 C21 97.20(18) . . . . ? C1 N2 C16 C17 106.21(18) . . . . ? C3 N2 C16 C17 -80.20(19) . . . . ? C1 N1 C2 C3 -0.58(17) . . . . ? C4 N1 C2 C3 -179.60(13) . . . . ? C17 C16 C21 C20 0.2(2) . . . . ? N2 C16 C21 C20 -177.07(14) . . . . ? C17 C16 C21 C22 -178.70(15) . . . . ? N2 C16 C21 C22 4.1(2) . . . . ? C23 C22 C21 C16 111.69(19) . . . . ? C24 C22 C21 C16 -123.85(18) . . . . ? C23 C22 C21 C20 -67.1(2) . . . . ? C24 C22 C21 C20 57.3(2) . . . . ? C9 C4 C5 C6 -0.3(3) . . . . ? N1 C4 C5 C6 -178.25(16) . . . . ? C9 C4 C5 C13 -179.01(17) . . . . ? N1 C4 C5 C13 3.0(3) . . . . ? C18 C17 C25 C26 98.44(18) . . . . ? C16 C17 C25 C26 -79.03(19) . . . . ? C18 C17 C25 C27 -25.1(2) . . . . ? C16 C17 C25 C27 157.40(15) . . . . ? N1 C2 C3 N2 0.88(17) . . . . ? C1 N2 C3 C2 -0.89(17) . . . . ? C16 N2 C3 C2 -175.41(14) . . . . ? C5 C4 C9 C8 -0.4(3) . . . . ? N1 C4 C9 C8 177.64(14) . . . . ? C5 C4 C9 C10 176.72(16) . . . . ? N1 C4 C9 C10 -5.3(2) . . . . ? C12 C10 C9 C8 -42.8(2) . . . . ? C11 C10 C9 C8 81.2(2) . . . . ? C12 C10 C9 C4 140.27(18) . . . . ? C11 C10 C9 C4 -95.71(18) . . . . ? C16 C17 C18 C19 1.0(2) . . . . ? C25 C17 C18 C19 -176.62(16) . . . . ? C17 C18 C19 C20 -0.2(3) . . . . ? C18 C19 C20 C21 -0.7(3) . . . . ? C16 C21 C20 C19 0.7(2) . . . . ? C22 C21 C20 C19 179.58(16) . . . . ? C6 C7 C8 C9 -0.2(3) . . . . ? C4 C9 C8 C7 0.6(3) . . . . ? C10 C9 C8 C7 -176.47(17) . . . . ? C8 C7 C6 C5 -0.4(3) . . . . ? C4 C5 C6 C7 0.6(3) . . . . ? C13 C5 C6 C7 179.42(18) . . . . ? C6 C5 C13 C15 -71.7(2) . . . . ? C4 C5 C13 C15 107.0(2) . . . . ? C6 C5 C13 C14 53.0(3) . . . . ? C4 C5 C13 C14 -128.3(2) . . . . ? C68 O1 C70 C66 3.3(2) . . . . ? O1 C70 C66 C67A -21.6(4) . . . . ? O1 C70 C66 C67B 18.9(3) . . . . ? C70 O1 C68 C67A 19.3(5) . . . . ? C70 O1 C68 C67B -24.5(3) . . . . ? C74 O2 C71 C72 -34.5(3) . . . . ? C73 C72 C71 O2 30.0(3) . . . . ? C71 O2 C74 C73 24.9(3) . . . . ? O2 C74 C73 C72 -5.2(4) . . . . ? C71 C72 C73 C74 -15.0(4) . . . . ? C64 C65 O3 C62 -0.9(3) . . . . ? O3 C65 C64 C63B -21.0(4) . . . . ? O3 C65 C64 C63A 20.3(7) . . . . ? C62 C63B C64 C65 33.9(4) . . . . ? C62 C63B C64 C63A -57.2(7) . . . . ? C62 C63A C64 C65 -33.3(12) . . . . ? C62 C63A C64 C63B 64.6(7) . . . . ? C64 C63A C62 O3 34.8(13) . . . . ? C64 C63A C62 C63B -60.4(10) . . . . ? C65 O3 C62 C63A -23.1(10) . . . . ? C65 O3 C62 C63B 24.0(4) . . . . ? C64 C63B C62 C63A 64.5(7) . . . . ? C64 C63B C62 O3 -35.8(4) . . . . ? C67A C68 C67B C66 -58.9(4) . . . . ? O1 C68 C67B C66 35.2(3) . . . . ? C67A C66 C67B C68 52.9(4) . . . . ? C70 C66 C67B C68 -32.1(3) . . . . ? O1 C68 C67A C66 -35.2(7) . . . . ? C67B C68 C67A C66 63.1(5) . . . . ? C67B C66 C67A C68 -67.5(6) . . . . ? C70 C66 C67A C68 35.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.924 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 937641' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_nhcpppnhcdot _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1,3-bis(1,3-bis(2,6-diisopropylphenyl)-1H-imidazol-2(3H)-ylidene)triphosphinyl _chemical_melting_point ? _chemical_formula_moiety 'C54 H72 N4 P3' _chemical_formula_sum 'C54 H72 N4 P3' _chemical_formula_weight 870.07 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 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9151(2) _cell_length_b 13.5428(2) _cell_length_c 15.8914(3) _cell_angle_alpha 85.6800(10) _cell_angle_beta 89.6010(10) _cell_angle_gamma 79.2550(10) _cell_volume 2512.11(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5770 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 26.95 _exptl_crystal_description Plate _exptl_crystal_colour Purple _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 938 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9485 _exptl_absorpt_correction_T_max 0.9799 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26055 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.54 _reflns_number_total 11545 _reflns_number_gt 7850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0514P)^2^+0.7287P] 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 11545 _refine_ls_number_parameters 662 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.003 _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 C1 C 0.20357(15) 0.04569(14) 0.27848(11) 0.0165(4) Uani 1 1 d . . . C2 C 0.16326(16) -0.11071(15) 0.30833(12) 0.0205(4) Uani 1 1 d . . . C3 C 0.10212(17) -0.07006(14) 0.24028(12) 0.0211(4) Uani 1 1 d . . . C4 C 0.08316(16) 0.08265(13) 0.14281(11) 0.0172(4) Uani 1 1 d . . . C5 C -0.03149(16) 0.12816(14) 0.13988(11) 0.0191(4) Uani 1 1 d . . . C6 C -0.07630(18) 0.17157(15) 0.06168(12) 0.0241(4) Uani 1 1 d . . . C7 C -0.00891(19) 0.16913(16) -0.00916(12) 0.0281(5) Uani 1 1 d . . . C8 C 0.10504(19) 0.12543(16) -0.00404(12) 0.0263(5) Uani 1 1 d . . . C9 C 0.15509(16) 0.08157(14) 0.07234(11) 0.0205(4) Uani 1 1 d . . . C10 C -0.10569(16) 0.13630(15) 0.21798(12) 0.0210(4) Uani 1 1 d . . . C11 C -0.21023(18) 0.08711(16) 0.20850(13) 0.0293(5) Uani 1 1 d . . . H11A H -0.2570 0.1215 0.1607 0.044 Uiso 1 1 calc R . . H11B H -0.2555 0.0925 0.2602 0.044 Uiso 1 1 calc R . . H11C H -0.1851 0.0159 0.1985 0.044 Uiso 1 1 calc R . . C12 C -0.14014(18) 0.24700(15) 0.23747(13) 0.0275(5) Uani 1 1 d . . . H12A H -0.0714 0.2760 0.2432 0.041 Uiso 1 1 calc R . . H12B H -0.1832 0.2512 0.2902 0.041 Uiso 1 1 calc R . . H12C H -0.1879 0.2845 0.1914 0.041 Uiso 1 1 calc R . . C13 C 0.28104(17) 0.03538(15) 0.07819(13) 0.0233(4) Uani 1 1 d . . . C14 C 0.3033(2) -0.07422(16) 0.05600(15) 0.0361(5) Uani 1 1 d . . . H14A H 0.2563 -0.1123 0.0917 0.054 Uiso 1 1 calc R . . H14B H 0.3842 -0.1036 0.0654 0.054 Uiso 1 1 calc R . . H14C H 0.2836 -0.0772 -0.0034 0.054 Uiso 1 1 calc R . . C15 C 0.35456(19) 0.09661(18) 0.02545(16) 0.0400(6) Uani 1 1 d . . . H15A H 0.3399 0.0920 -0.0346 0.060 Uiso 1 1 calc R . . H15B H 0.4354 0.0700 0.0382 0.060 Uiso 1 1 calc R . . H15C H 0.3358 0.1673 0.0388 0.060 Uiso 1 1 calc R . . C16 C 0.32234(16) -0.06676(13) 0.39037(11) 0.0179(4) Uani 1 1 d . . . C17 C 0.29908(17) -0.05572(14) 0.47588(12) 0.0213(4) Uani 1 1 d . . . C18 C 0.38938(18) -0.08794(16) 0.53298(13) 0.0258(4) Uani 1 1 d . . . C19 C 0.49761(19) -0.12797(16) 0.50600(13) 0.0277(5) Uani 1 1 d . . . C20 C 0.51763(18) -0.13674(15) 0.42078(13) 0.0252(4) Uani 1 1 d . . . C21 C 0.43110(16) -0.10660(14) 0.36076(12) 0.0208(4) Uani 1 1 d . . . C22 C 0.18030(18) -0.01481(17) 0.50588(12) 0.0274(5) Uani 1 1 d . . . C23 C 0.12768(19) -0.10052(19) 0.54855(14) 0.0374(6) Uani 1 1 d . . . H23A H 0.1202 -0.1492 0.5073 0.056 Uiso 1 1 calc R . . H23B H 0.0521 -0.0729 0.5704 0.056 Uiso 1 1 calc R . . H23C H 0.1771 -0.1342 0.5952 0.056 Uiso 1 1 calc R . . C24 C 0.1776(2) 0.07077(18) 0.56361(14) 0.0397(6) Uani 1 1 d . . . H24A H 0.2224 0.0454 0.6148 0.059 Uiso 1 1 calc R . . H24B H 0.0984 0.0969 0.5790 0.059 Uiso 1 1 calc R . . H24C H 0.2102 0.1249 0.5341 0.059 Uiso 1 1 calc R . . C25 C 0.45620(18) -0.11700(16) 0.26748(13) 0.0256(4) Uani 1 1 d . . . C26 C 0.5394(2) -0.04915(18) 0.23624(14) 0.0359(5) Uani 1 1 d . . . H26A H 0.5074 0.0209 0.2467 0.054 Uiso 1 1 calc R . . H26B H 0.5518 -0.0544 0.1756 0.054 Uiso 1 1 calc R . . H26C H 0.6124 -0.0704 0.2664 0.054 Uiso 1 1 calc R . . C27 C 0.5002(2) -0.22660(17) 0.24950(15) 0.0376(5) Uani 1 1 d . . . H27A H 0.5715 -0.2521 0.2808 0.056 Uiso 1 1 calc R . . H27B H 0.5141 -0.2307 0.1889 0.056 Uiso 1 1 calc R . . H27C H 0.4431 -0.2673 0.2673 0.056 Uiso 1 1 calc R . . C28 C 0.19768(15) 0.48892(13) 0.23778(11) 0.0161(4) Uani 1 1 d . . . C29 C 0.26869(17) 0.60755(15) 0.15658(12) 0.0232(4) Uani 1 1 d . . . C30 C 0.20520(17) 0.65515(15) 0.21462(12) 0.0206(4) Uani 1 1 d . . . C31 C 0.34047(16) 0.43321(14) 0.12248(12) 0.0204(4) Uani 1 1 d . . . C32 C 0.44533(16) 0.38582(15) 0.15794(13) 0.0230(4) Uani 1 1 d . . . C33 C 0.52177(19) 0.32799(17) 0.10578(15) 0.0319(5) Uani 1 1 d . . . C34 C 0.4938(2) 0.31949(17) 0.02227(15) 0.0338(5) Uani 1 1 d . . . C35 C 0.3887(2) 0.36520(16) -0.01008(14) 0.0303(5) Uani 1 1 d . . . C36 C 0.30778(17) 0.42241(14) 0.03953(12) 0.0233(4) Uani 1 1 d . . . C37 C 0.47671(17) 0.39620(16) 0.24898(13) 0.0266(5) Uani 1 1 d . . . C38 C 0.52506(19) 0.29461(17) 0.29565(15) 0.0363(5) Uani 1 1 d . . . H38A H 0.4709 0.2489 0.2914 0.054 Uiso 1 1 calc R . . H38B H 0.5375 0.3041 0.3552 0.054 Uiso 1 1 calc R . . H38C H 0.5978 0.2656 0.2703 0.054 Uiso 1 1 calc R . . C39 C 0.5587(2) 0.46942(18) 0.25440(15) 0.0397(6) Uani 1 1 d . . . H39A H 0.6314 0.4420 0.2280 0.060 Uiso 1 1 calc R . . H39B H 0.5722 0.4790 0.3137 0.060 Uiso 1 1 calc R . . H39C H 0.5255 0.5343 0.2249 0.060 Uiso 1 1 calc R . . C40 C 0.19007(19) 0.46879(16) 0.00585(13) 0.0281(5) Uani 1 1 d . . . C41 C 0.1942(2) 0.55500(17) -0.06138(14) 0.0410(6) Uani 1 1 d . . . H41A H 0.2284 0.6070 -0.0371 0.061 Uiso 1 1 calc R . . H41B H 0.1165 0.5842 -0.0811 0.061 Uiso 1 1 calc R . . H41C H 0.2403 0.5291 -0.1090 0.061 Uiso 1 1 calc R . . C42 C 0.1304(2) 0.38905(17) -0.02766(14) 0.0356(5) Uani 1 1 d . . . H42A H 0.1755 0.3572 -0.0735 0.053 Uiso 1 1 calc R . . H42B H 0.0543 0.4210 -0.0489 0.053 Uiso 1 1 calc R . . H42C H 0.1232 0.3378 0.0180 0.053 Uiso 1 1 calc R . . C43 C 0.10266(16) 0.60215(13) 0.34476(11) 0.0182(4) Uani 1 1 d . . . C44 C 0.17034(17) 0.59641(14) 0.41738(12) 0.0223(4) Uani 1 1 d . . . C45 C 0.1136(2) 0.61661(16) 0.49302(13) 0.0292(5) Uani 1 1 d . . . C46 C -0.0039(2) 0.64152(17) 0.49633(13) 0.0314(5) Uani 1 1 d . . . C47 C -0.06814(19) 0.64695(16) 0.42350(13) 0.0265(5) Uani 1 1 d . . . C48 C -0.01641(16) 0.62707(14) 0.34581(12) 0.0206(4) Uani 1 1 d . . . C49 C -0.08968(17) 0.63495(15) 0.26732(12) 0.0234(4) Uani 1 1 d . . . C50 C -0.1445(2) 0.74505(16) 0.24361(14) 0.0346(5) Uani 1 1 d . . . H50A H -0.1929 0.7715 0.2899 0.052 Uiso 1 1 calc R . . H50B H -0.1910 0.7490 0.1924 0.052 Uiso 1 1 calc R . . H50C H -0.0845 0.7850 0.2333 0.052 Uiso 1 1 calc R . . C51 C -0.1802(2) 0.56923(18) 0.27784(14) 0.0376(6) Uani 1 1 d . . . H51A H -0.1431 0.4987 0.2898 0.056 Uiso 1 1 calc R . . H51B H -0.2254 0.5758 0.2257 0.056 Uiso 1 1 calc R . . H51C H -0.2305 0.5909 0.3247 0.056 Uiso 1 1 calc R . . C52 C 0.29923(18) 0.56879(16) 0.41645(13) 0.0276(5) Uani 1 1 d . . . C53 C 0.3551(2) 0.65109(17) 0.45089(16) 0.0408(6) Uani 1 1 d . . . H53A H 0.3256 0.7159 0.4198 0.061 Uiso 1 1 calc R . . H53B H 0.4381 0.6340 0.4439 0.061 Uiso 1 1 calc R . . H53C H 0.3372 0.6558 0.5109 0.061 Uiso 1 1 calc R . . C54 C 0.3419(2) 0.46713(17) 0.46435(15) 0.0374(5) Uani 1 1 d . . . H54A H 0.3238 0.4718 0.5243 0.056 Uiso 1 1 calc R . . H54B H 0.4247 0.4482 0.4577 0.056 Uiso 1 1 calc R . . H54C H 0.3045 0.4160 0.4418 0.056 Uiso 1 1 calc R . . H2 H 0.1680(18) -0.1733(17) 0.3391(13) 0.030(6) Uiso 1 1 d . . . H3 H 0.0516(18) -0.0945(16) 0.2099(13) 0.027(6) Uiso 1 1 d . . . H6 H -0.1520(18) 0.2031(15) 0.0583(12) 0.019(5) Uiso 1 1 d . . . H7 H -0.0432(18) 0.2043(16) -0.0609(14) 0.030(6) Uiso 1 1 d . . . H8 H 0.1515(18) 0.1274(15) -0.0503(13) 0.026(6) Uiso 1 1 d . . . H10 H -0.0596(16) 0.1007(14) 0.2657(12) 0.013(5) Uiso 1 1 d . . . H13 H 0.3055(17) 0.0363(15) 0.1355(13) 0.025(6) Uiso 1 1 d . . . H18 H 0.3756(18) -0.0819(15) 0.5944(13) 0.028(6) Uiso 1 1 d . . . H19 H 0.562(2) -0.1524(17) 0.5466(14) 0.037(6) Uiso 1 1 d . . . H20 H 0.5889(18) -0.1628(15) 0.4007(12) 0.018(5) Uiso 1 1 d . . . H22 H 0.1352(18) 0.0139(15) 0.4562(13) 0.025(5) Uiso 1 1 d . . . H25 H 0.3837(18) -0.0940(15) 0.2365(12) 0.022(5) Uiso 1 1 d . . . H29 H 0.3123(17) 0.6322(15) 0.1126(13) 0.026(6) Uiso 1 1 d . . . H30 H 0.1882(18) 0.7210(17) 0.2250(13) 0.032(6) Uiso 1 1 d . . . H33 H 0.5945(19) 0.2930(16) 0.1268(13) 0.028(6) Uiso 1 1 d . . . H34 H 0.550(2) 0.2817(18) -0.0108(15) 0.048(7) Uiso 1 1 d . . . H35 H 0.368(2) 0.3590(17) -0.0652(15) 0.040(7) Uiso 1 1 d . . . H37 H 0.4085(17) 0.4250(14) 0.2780(12) 0.018(5) Uiso 1 1 d . . . H40 H 0.1422(18) 0.4949(16) 0.0506(13) 0.029(6) Uiso 1 1 d . . . H45 H 0.1570(19) 0.6131(16) 0.5423(14) 0.034(6) Uiso 1 1 d . . . H46 H -0.045(2) 0.6561(18) 0.5472(15) 0.046(7) Uiso 1 1 d . . . H47 H -0.1469(18) 0.6636(15) 0.4263(12) 0.021(5) Uiso 1 1 d . . . H49 H -0.0416(16) 0.6116(14) 0.2243(12) 0.014(5) Uiso 1 1 d . . . H52 H 0.3279(17) 0.5644(15) 0.3593(13) 0.023(5) Uiso 1 1 d . . . N1 N 0.12791(12) 0.02506(11) 0.21982(9) 0.0159(3) Uani 1 1 d . . . N2 N 0.22888(13) -0.04221(11) 0.33061(9) 0.0169(3) Uani 1 1 d . . . N3 N 0.26614(13) 0.50534(11) 0.16980(9) 0.0180(3) Uani 1 1 d . . . N4 N 0.16027(13) 0.58354(11) 0.26530(9) 0.0170(3) Uani 1 1 d . . . P1 P 0.25553(5) 0.15383(4) 0.30308(3) 0.02222(12) Uani 1 1 d . . . P2 P 0.19850(5) 0.26590(4) 0.20219(3) 0.02176(12) Uani 1 1 d . . . P3 P 0.16127(5) 0.37958(4) 0.29041(3) 0.02185(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0145(9) 0.0173(9) 0.0172(9) -0.0035(7) 0.0025(7) -0.0008(7) C2 0.0213(10) 0.0165(10) 0.0238(10) -0.0006(8) 0.0020(8) -0.0043(8) C3 0.0226(10) 0.0176(10) 0.0249(10) -0.0031(8) -0.0029(8) -0.0079(8) C4 0.0208(10) 0.0151(9) 0.0159(9) -0.0029(7) -0.0010(7) -0.0034(7) C5 0.0200(10) 0.0173(9) 0.0202(9) -0.0015(7) -0.0005(8) -0.0045(8) C6 0.0219(11) 0.0250(11) 0.0239(10) 0.0003(8) -0.0049(8) -0.0013(9) C7 0.0363(13) 0.0312(12) 0.0163(10) 0.0031(9) -0.0057(9) -0.0068(10) C8 0.0329(12) 0.0313(12) 0.0159(9) -0.0040(8) 0.0038(9) -0.0087(9) C9 0.0216(10) 0.0203(10) 0.0205(9) -0.0066(8) 0.0016(8) -0.0046(8) C10 0.0171(10) 0.0234(10) 0.0203(10) 0.0012(8) 0.0007(8) 0.0008(8) C11 0.0250(11) 0.0306(12) 0.0325(11) -0.0005(9) 0.0039(9) -0.0066(9) C12 0.0241(11) 0.0267(11) 0.0303(11) -0.0029(9) 0.0058(9) -0.0008(9) C13 0.0219(11) 0.0274(11) 0.0209(10) -0.0070(8) 0.0045(8) -0.0039(8) C14 0.0322(13) 0.0299(12) 0.0456(14) -0.0133(10) 0.0011(11) 0.0000(10) C15 0.0286(13) 0.0409(14) 0.0495(14) -0.0027(11) 0.0157(11) -0.0044(10) C16 0.0191(10) 0.0134(9) 0.0207(9) -0.0001(7) -0.0047(8) -0.0017(7) C17 0.0229(10) 0.0185(10) 0.0212(9) 0.0025(8) -0.0034(8) -0.0020(8) C18 0.0291(12) 0.0273(11) 0.0202(10) 0.0021(8) -0.0058(9) -0.0042(9) C19 0.0267(12) 0.0255(11) 0.0301(11) 0.0039(9) -0.0095(9) -0.0048(9) C20 0.0172(10) 0.0238(11) 0.0336(11) 0.0002(9) -0.0008(9) -0.0015(8) C21 0.0203(10) 0.0167(9) 0.0257(10) -0.0022(8) -0.0007(8) -0.0035(8) C22 0.0243(11) 0.0370(12) 0.0176(10) -0.0002(9) -0.0017(8) 0.0021(9) C23 0.0263(12) 0.0565(16) 0.0291(12) -0.0031(11) 0.0050(10) -0.0074(11) C24 0.0407(14) 0.0408(14) 0.0331(12) -0.0107(11) -0.0001(11) 0.0070(11) C25 0.0200(11) 0.0285(11) 0.0270(11) -0.0059(9) 0.0001(9) 0.0006(9) C26 0.0342(13) 0.0432(14) 0.0307(12) -0.0036(10) 0.0076(10) -0.0080(11) C27 0.0326(13) 0.0361(13) 0.0428(13) -0.0151(11) 0.0015(11) 0.0014(10) C28 0.0137(9) 0.0165(9) 0.0175(9) -0.0028(7) -0.0005(7) -0.0001(7) C29 0.0274(11) 0.0193(10) 0.0228(10) 0.0029(8) 0.0024(9) -0.0059(8) C30 0.0289(11) 0.0128(10) 0.0195(9) 0.0012(8) -0.0030(8) -0.0034(8) C31 0.0228(10) 0.0162(9) 0.0221(9) -0.0024(8) 0.0079(8) -0.0034(8) C32 0.0188(10) 0.0210(10) 0.0303(10) -0.0039(8) 0.0074(8) -0.0058(8) C33 0.0201(12) 0.0308(12) 0.0440(13) -0.0064(10) 0.0080(10) -0.0017(9) C34 0.0314(13) 0.0282(12) 0.0430(13) -0.0129(10) 0.0206(11) -0.0054(10) C35 0.0394(14) 0.0272(12) 0.0255(11) -0.0072(9) 0.0126(10) -0.0077(10) C36 0.0292(11) 0.0180(10) 0.0229(10) -0.0014(8) 0.0071(8) -0.0054(8) C37 0.0165(10) 0.0287(11) 0.0331(11) -0.0049(9) 0.0026(9) 0.0004(9) C38 0.0299(13) 0.0355(13) 0.0429(13) 0.0026(11) -0.0053(10) -0.0064(10) C39 0.0431(15) 0.0358(13) 0.0425(13) -0.0070(11) -0.0042(11) -0.0114(11) C40 0.0354(13) 0.0298(12) 0.0183(10) -0.0032(9) 0.0024(9) -0.0038(9) C41 0.0614(17) 0.0283(12) 0.0312(12) 0.0017(10) -0.0017(11) -0.0044(11) C42 0.0423(14) 0.0352(13) 0.0289(11) 0.0011(10) -0.0066(10) -0.0075(11) C43 0.0222(10) 0.0139(9) 0.0174(9) -0.0037(7) 0.0018(8) 0.0001(7) C44 0.0271(11) 0.0195(10) 0.0202(9) -0.0018(8) -0.0009(8) -0.0037(8) C45 0.0416(14) 0.0288(12) 0.0185(10) -0.0046(9) -0.0020(10) -0.0082(10) C46 0.0431(14) 0.0316(12) 0.0208(10) -0.0101(9) 0.0099(10) -0.0077(10) C47 0.0230(11) 0.0289(12) 0.0278(11) -0.0085(9) 0.0080(9) -0.0027(9) C48 0.0227(10) 0.0172(9) 0.0220(9) -0.0071(8) 0.0018(8) -0.0021(8) C49 0.0191(10) 0.0279(11) 0.0236(10) -0.0085(8) 0.0028(8) -0.0030(8) C50 0.0364(13) 0.0308(12) 0.0359(12) -0.0014(10) -0.0089(10) -0.0046(10) C51 0.0386(14) 0.0436(14) 0.0352(12) -0.0026(11) -0.0056(10) -0.0192(11) C52 0.0275(12) 0.0306(12) 0.0237(11) 0.0002(9) -0.0052(9) -0.0035(9) C53 0.0347(14) 0.0299(13) 0.0569(15) 0.0073(11) -0.0181(12) -0.0070(10) C54 0.0384(14) 0.0285(12) 0.0429(13) -0.0007(10) -0.0117(11) -0.0006(10) N1 0.0149(8) 0.0156(8) 0.0171(7) -0.0023(6) -0.0006(6) -0.0022(6) N2 0.0175(8) 0.0156(8) 0.0175(8) -0.0020(6) -0.0015(6) -0.0020(6) N3 0.0193(8) 0.0148(8) 0.0191(8) -0.0015(6) 0.0032(6) -0.0013(6) N4 0.0186(8) 0.0155(8) 0.0163(7) -0.0020(6) 0.0017(6) -0.0017(6) P1 0.0276(3) 0.0168(3) 0.0228(3) -0.0012(2) -0.0054(2) -0.0053(2) P2 0.0300(3) 0.0167(3) 0.0191(2) -0.00232(19) 0.0014(2) -0.0052(2) P3 0.0275(3) 0.0163(3) 0.0225(3) -0.0041(2) 0.0087(2) -0.0053(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.380(2) . ? C1 N2 1.384(2) . ? C1 P1 1.7632(19) . ? C2 C3 1.332(3) . ? C2 N2 1.386(2) . ? C2 H2 0.94(2) . ? C3 N1 1.394(2) . ? C3 H3 0.90(2) . ? C4 C5 1.390(3) . ? C4 C9 1.405(2) . ? C4 N1 1.449(2) . ? C5 C6 1.399(3) . ? C5 C10 1.518(2) . ? C6 C7 1.377(3) . ? C6 H6 0.92(2) . ? C7 C8 1.377(3) . ? C7 H7 0.97(2) . ? C8 C9 1.397(3) . ? C8 H8 0.92(2) . ? C9 C13 1.515(3) . ? C10 C11 1.531(3) . ? C10 C12 1.533(3) . ? C10 H10 0.981(19) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.521(3) . ? C13 C14 1.526(3) . ? C13 H13 0.96(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.398(3) . ? C16 C21 1.400(3) . ? C16 N2 1.443(2) . ? C17 C18 1.397(3) . ? C17 C22 1.508(3) . ? C18 C19 1.381(3) . ? C18 H18 1.00(2) . ? C19 C20 1.384(3) . ? C19 H19 0.99(2) . ? C20 C21 1.392(3) . ? C20 H20 0.92(2) . ? C21 C25 1.522(3) . ? C22 C24 1.527(3) . ? C22 C23 1.532(3) . ? C22 H22 0.97(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.527(3) . ? C25 C26 1.529(3) . ? C25 H25 0.98(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N4 1.379(2) . ? C28 N3 1.379(2) . ? C28 P3 1.7687(18) . ? C29 C30 1.318(3) . ? C29 N3 1.390(2) . ? C29 H29 0.95(2) . ? C30 N4 1.395(2) . ? C30 H30 0.90(2) . ? C31 C32 1.395(3) . ? C31 C36 1.403(3) . ? C31 N3 1.443(2) . ? C32 C33 1.397(3) . ? C32 C37 1.520(3) . ? C33 C34 1.389(3) . ? C33 H33 0.96(2) . ? C34 C35 1.374(3) . ? C34 H34 0.94(3) . ? C35 C36 1.398(3) . ? C35 H35 0.93(2) . ? C36 C40 1.510(3) . ? C37 C39 1.524(3) . ? C37 C38 1.527(3) . ? C37 H37 0.96(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C42 1.528(3) . ? C40 C41 1.530(3) . ? C40 H40 0.96(2) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C48 1.396(3) . ? C43 C44 1.402(3) . ? C43 N4 1.449(2) . ? C44 C45 1.395(3) . ? C44 C52 1.512(3) . ? C45 C46 1.379(3) . ? C45 H45 0.93(2) . ? C46 C47 1.382(3) . ? C46 H46 0.96(2) . ? C47 C48 1.398(3) . ? C47 H47 0.93(2) . ? C48 C49 1.513(3) . ? C49 C51 1.522(3) . ? C49 C50 1.532(3) . ? C49 H49 0.924(19) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.523(3) . ? C52 C53 1.536(3) . ? C52 H52 0.97(2) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? P1 P2 2.1448(7) . ? P2 P3 2.1435(7) . ? 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 C1 N2 104.19(15) . . ? N1 C1 P1 135.24(14) . . ? N2 C1 P1 120.19(13) . . ? C3 C2 N2 107.52(17) . . ? C3 C2 H2 131.6(13) . . ? N2 C2 H2 120.9(13) . . ? C2 C3 N1 108.02(17) . . ? C2 C3 H3 130.4(13) . . ? N1 C3 H3 121.6(13) . . ? C5 C4 C9 123.14(17) . . ? C5 C4 N1 118.42(15) . . ? C9 C4 N1 118.16(16) . . ? C4 C5 C6 117.27(17) . . ? C4 C5 C10 122.53(16) . . ? C6 C5 C10 120.13(17) . . ? C7 C6 C5 121.0(2) . . ? C7 C6 H6 120.1(12) . . ? C5 C6 H6 118.9(12) . . ? C8 C7 C6 120.46(19) . . ? C8 C7 H7 121.9(13) . . ? C6 C7 H7 117.4(13) . . ? C7 C8 C9 121.26(18) . . ? C7 C8 H8 120.8(13) . . ? C9 C8 H8 117.8(13) . . ? C8 C9 C4 116.80(18) . . ? C8 C9 C13 121.17(17) . . ? C4 C9 C13 122.03(17) . . ? C5 C10 C11 111.49(16) . . ? C5 C10 C12 109.96(16) . . ? C11 C10 C12 111.64(16) . . ? C5 C10 H10 107.8(11) . . ? C11 C10 H10 108.4(11) . . ? C12 C10 H10 107.4(11) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C15 112.59(17) . . ? C9 C13 C14 111.56(17) . . ? C15 C13 C14 111.13(18) . . ? C9 C13 H13 108.1(12) . . ? C15 C13 H13 105.5(12) . . ? C14 C13 H13 107.6(12) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 122.86(17) . . ? C17 C16 N2 118.59(16) . . ? C21 C16 N2 118.42(16) . . ? C18 C17 C16 117.32(18) . . ? C18 C17 C22 121.12(18) . . ? C16 C17 C22 121.51(17) . . ? C19 C18 C17 121.34(19) . . ? C19 C18 H18 119.2(12) . . ? C17 C18 H18 119.4(12) . . ? C18 C19 C20 119.7(2) . . ? C18 C19 H19 121.5(13) . . ? C20 C19 H19 118.8(13) . . ? C19 C20 C21 121.74(19) . . ? C19 C20 H20 121.8(12) . . ? C21 C20 H20 116.5(12) . . ? C20 C21 C16 117.05(18) . . ? C20 C21 C25 120.37(17) . . ? C16 C21 C25 122.58(17) . . ? C17 C22 C24 112.64(18) . . ? C17 C22 C23 109.90(17) . . ? C24 C22 C23 111.48(18) . . ? C17 C22 H22 107.0(12) . . ? C24 C22 H22 106.5(12) . . ? C23 C22 H22 109.1(12) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C27 111.60(18) . . ? C21 C25 C26 110.63(17) . . ? C27 C25 C26 111.49(18) . . ? C21 C25 H25 107.3(11) . . ? C27 C25 H25 107.7(12) . . ? C26 C25 H25 107.9(11) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 N3 104.18(15) . . ? N4 C28 P3 121.97(13) . . ? N3 C28 P3 133.78(14) . . ? C30 C29 N3 108.16(17) . . ? C30 C29 H29 130.6(13) . . ? N3 C29 H29 121.2(13) . . ? C29 C30 N4 107.71(17) . . ? C29 C30 H30 132.0(14) . . ? N4 C30 H30 120.3(14) . . ? C32 C31 C36 123.44(17) . . ? C32 C31 N3 118.73(17) . . ? C36 C31 N3 117.51(17) . . ? C31 C32 C33 117.02(19) . . ? C31 C32 C37 122.20(17) . . ? C33 C32 C37 120.78(19) . . ? C34 C33 C32 120.8(2) . . ? C34 C33 H33 118.4(13) . . ? C32 C33 H33 120.8(13) . . ? C35 C34 C33 120.6(2) . . ? C35 C34 H34 122.1(15) . . ? C33 C34 H34 117.3(15) . . ? C34 C35 C36 121.1(2) . . ? C34 C35 H35 121.9(15) . . ? C36 C35 H35 117.0(15) . . ? C35 C36 C31 116.85(19) . . ? C35 C36 C40 121.52(19) . . ? C31 C36 C40 121.62(17) . . ? C32 C37 C39 111.35(17) . . ? C32 C37 C38 112.28(18) . . ? C39 C37 C38 110.89(19) . . ? C32 C37 H37 108.5(11) . . ? C39 C37 H37 106.1(11) . . ? C38 C37 H37 107.4(11) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 C42 111.07(18) . . ? C36 C40 C41 111.59(18) . . ? C42 C40 C41 111.23(18) . . ? C36 C40 H40 110.1(13) . . ? C42 C40 H40 104.3(13) . . ? C41 C40 H40 108.2(13) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 122.87(17) . . ? C48 C43 N4 119.29(16) . . ? C44 C43 N4 117.82(16) . . ? C45 C44 C43 117.06(19) . . ? C45 C44 C52 119.99(18) . . ? C43 C44 C52 122.94(17) . . ? C46 C45 C44 121.6(2) . . ? C46 C45 H45 119.9(14) . . ? C44 C45 H45 118.5(14) . . ? C45 C46 C47 119.89(19) . . ? C45 C46 H46 123.5(15) . . ? C47 C46 H46 116.7(15) . . ? C46 C47 C48 121.3(2) . . ? C46 C47 H47 119.4(12) . . ? C48 C47 H47 119.3(12) . . ? C43 C48 C47 117.31(18) . . ? C43 C48 C49 123.02(16) . . ? C47 C48 C49 119.66(18) . . ? C48 C49 C51 111.80(17) . . ? C48 C49 C50 110.40(16) . . ? C51 C49 C50 110.88(18) . . ? C48 C49 H49 106.8(12) . . ? C51 C49 H49 108.0(11) . . ? C50 C49 H49 108.8(11) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C44 C52 C54 111.46(18) . . ? C44 C52 C53 111.72(18) . . ? C54 C52 C53 110.85(18) . . ? C44 C52 H52 111.4(12) . . ? C54 C52 H52 107.3(12) . . ? C53 C52 H52 103.7(12) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C1 N1 C3 109.75(15) . . ? C1 N1 C4 129.88(15) . . ? C3 N1 C4 120.20(15) . . ? C1 N2 C2 110.29(15) . . ? C1 N2 C16 125.34(15) . . ? C2 N2 C16 123.65(15) . . ? C28 N3 C29 109.94(15) . . ? C28 N3 C31 129.35(15) . . ? C29 N3 C31 120.17(15) . . ? C28 N4 C30 110.00(15) . . ? C28 N4 C43 124.10(15) . . ? C30 N4 C43 124.79(15) . . ? C1 P1 P2 105.71(6) . . ? P3 P2 P1 90.53(3) . . ? C28 P3 P2 105.03(6) . . ? 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 C2 C3 N1 -0.7(2) . . . . ? C9 C4 C5 C6 2.1(3) . . . . ? N1 C4 C5 C6 -171.54(16) . . . . ? C9 C4 C5 C10 -174.82(17) . . . . ? N1 C4 C5 C10 11.5(3) . . . . ? C4 C5 C6 C7 -0.1(3) . . . . ? C10 C5 C6 C7 176.93(18) . . . . ? C5 C6 C7 C8 -1.3(3) . . . . ? C6 C7 C8 C9 0.7(3) . . . . ? C7 C8 C9 C4 1.2(3) . . . . ? C7 C8 C9 C13 -178.76(19) . . . . ? C5 C4 C9 C8 -2.7(3) . . . . ? N1 C4 C9 C8 171.04(17) . . . . ? C5 C4 C9 C13 177.27(17) . . . . ? N1 C4 C9 C13 -9.0(3) . . . . ? C4 C5 C10 C11 -122.73(19) . . . . ? C6 C5 C10 C11 60.4(2) . . . . ? C4 C5 C10 C12 112.9(2) . . . . ? C6 C5 C10 C12 -64.0(2) . . . . ? C8 C9 C13 C15 39.4(3) . . . . ? C4 C9 C13 C15 -140.54(19) . . . . ? C8 C9 C13 C14 -86.4(2) . . . . ? C4 C9 C13 C14 93.7(2) . . . . ? C21 C16 C17 C18 -1.1(3) . . . . ? N2 C16 C17 C18 174.79(16) . . . . ? C21 C16 C17 C22 -178.53(18) . . . . ? N2 C16 C17 C22 -2.7(3) . . . . ? C16 C17 C18 C19 0.8(3) . . . . ? C22 C17 C18 C19 178.24(19) . . . . ? C17 C18 C19 C20 -0.1(3) . . . . ? C18 C19 C20 C21 -0.3(3) . . . . ? C19 C20 C21 C16 0.0(3) . . . . ? C19 C20 C21 C25 179.80(19) . . . . ? C17 C16 C21 C20 0.7(3) . . . . ? N2 C16 C21 C20 -175.18(16) . . . . ? C17 C16 C21 C25 -179.09(18) . . . . ? N2 C16 C21 C25 5.0(3) . . . . ? C18 C17 C22 C24 53.3(3) . . . . ? C16 C17 C22 C24 -129.3(2) . . . . ? C18 C17 C22 C23 -71.7(2) . . . . ? C16 C17 C22 C23 105.7(2) . . . . ? C20 C21 C25 C27 60.2(2) . . . . ? C16 C21 C25 C27 -120.1(2) . . . . ? C20 C21 C25 C26 -64.6(2) . . . . ? C16 C21 C25 C26 115.2(2) . . . . ? N3 C29 C30 N4 -0.6(2) . . . . ? C36 C31 C32 C33 2.4(3) . . . . ? N3 C31 C32 C33 -170.90(17) . . . . ? C36 C31 C32 C37 -177.91(18) . . . . ? N3 C31 C32 C37 8.8(3) . . . . ? C31 C32 C33 C34 0.6(3) . . . . ? C37 C32 C33 C34 -179.16(19) . . . . ? C32 C33 C34 C35 -2.1(3) . . . . ? C33 C34 C35 C36 0.9(3) . . . . ? C34 C35 C36 C31 1.9(3) . . . . ? C34 C35 C36 C40 -177.04(19) . . . . ? C32 C31 C36 C35 -3.6(3) . . . . ? N3 C31 C36 C35 169.77(17) . . . . ? C32 C31 C36 C40 175.35(18) . . . . ? N3 C31 C36 C40 -11.3(3) . . . . ? C31 C32 C37 C39 -103.0(2) . . . . ? C33 C32 C37 C39 76.7(2) . . . . ? C31 C32 C37 C38 132.0(2) . . . . ? C33 C32 C37 C38 -48.3(3) . . . . ? C35 C36 C40 C42 54.9(2) . . . . ? C31 C36 C40 C42 -124.0(2) . . . . ? C35 C36 C40 C41 -69.8(2) . . . . ? C31 C36 C40 C41 111.3(2) . . . . ? C48 C43 C44 C45 0.2(3) . . . . ? N4 C43 C44 C45 178.68(17) . . . . ? C48 C43 C44 C52 179.61(18) . . . . ? N4 C43 C44 C52 -1.9(3) . . . . ? C43 C44 C45 C46 -0.2(3) . . . . ? C52 C44 C45 C46 -179.7(2) . . . . ? C44 C45 C46 C47 0.0(3) . . . . ? C45 C46 C47 C48 0.4(3) . . . . ? C44 C43 C48 C47 0.1(3) . . . . ? N4 C43 C48 C47 -178.36(17) . . . . ? C44 C43 C48 C49 179.00(18) . . . . ? N4 C43 C48 C49 0.5(3) . . . . ? C46 C47 C48 C43 -0.4(3) . . . . ? C46 C47 C48 C49 -179.33(19) . . . . ? C43 C48 C49 C51 126.0(2) . . . . ? C47 C48 C49 C51 -55.1(2) . . . . ? C43 C48 C49 C50 -110.1(2) . . . . ? C47 C48 C49 C50 68.8(2) . . . . ? C45 C44 C52 C54 66.8(2) . . . . ? C43 C44 C52 C54 -112.6(2) . . . . ? C45 C44 C52 C53 -57.8(3) . . . . ? C43 C44 C52 C53 122.8(2) . . . . ? N2 C1 N1 C3 4.35(18) . . . . ? P1 C1 N1 C3 -168.19(16) . . . . ? N2 C1 N1 C4 -170.74(16) . . . . ? P1 C1 N1 C4 16.7(3) . . . . ? C2 C3 N1 C1 -2.4(2) . . . . ? C2 C3 N1 C4 173.28(16) . . . . ? C5 C4 N1 C1 -110.4(2) . . . . ? C9 C4 N1 C1 75.6(2) . . . . ? C5 C4 N1 C3 74.9(2) . . . . ? C9 C4 N1 C3 -99.1(2) . . . . ? N1 C1 N2 C2 -4.82(19) . . . . ? P1 C1 N2 C2 169.12(13) . . . . ? N1 C1 N2 C16 165.70(15) . . . . ? P1 C1 N2 C16 -20.4(2) . . . . ? C3 C2 N2 C1 3.5(2) . . . . ? C3 C2 N2 C16 -167.17(16) . . . . ? C17 C16 N2 C1 102.0(2) . . . . ? C21 C16 N2 C1 -82.0(2) . . . . ? C17 C16 N2 C2 -88.7(2) . . . . ? C21 C16 N2 C2 87.3(2) . . . . ? N4 C28 N3 C29 -0.5(2) . . . . ? P3 C28 N3 C29 -177.43(16) . . . . ? N4 C28 N3 C31 170.97(17) . . . . ? P3 C28 N3 C31 -5.9(3) . . . . ? C30 C29 N3 C28 0.7(2) . . . . ? C30 C29 N3 C31 -171.69(17) . . . . ? C32 C31 N3 C28 -76.3(2) . . . . ? C36 C31 N3 C28 110.0(2) . . . . ? C32 C31 N3 C29 94.5(2) . . . . ? C36 C31 N3 C29 -79.2(2) . . . . ? N3 C28 N4 C30 0.17(19) . . . . ? P3 C28 N4 C30 177.54(13) . . . . ? N3 C28 N4 C43 -168.25(16) . . . . ? P3 C28 N4 C43 9.1(2) . . . . ? C29 C30 N4 C28 0.3(2) . . . . ? C29 C30 N4 C43 168.58(17) . . . . ? C48 C43 N4 C28 -97.7(2) . . . . ? C44 C43 N4 C28 83.8(2) . . . . ? C48 C43 N4 C30 95.6(2) . . . . ? C44 C43 N4 C30 -82.9(2) . . . . ? N1 C1 P1 P2 -10.29(19) . . . . ? N2 C1 P1 P2 178.08(12) . . . . ? C1 P1 P2 P3 139.84(6) . . . . ? N4 C28 P3 P2 163.74(13) . . . . ? N3 C28 P3 P2 -19.8(2) . . . . ? P1 P2 P3 C28 143.48(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.351 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.055 _database_code_depnum_ccdc_archive 'CCDC 937654' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_nhc2paspcl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[bis((1,3-bis(2,6-diisopropylphenyl)-1H-imidazol-2-ylidene)phosphino)arsinium]Chloride' _chemical_melting_point ? _chemical_formula_moiety 'C33 H48 As0.5 Cl0.5 N2 O1.5 P1' _chemical_formula_sum 'C66 H96 As Cl N4 O3 P2' _chemical_formula_weight 1165.78 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.9280(12) _cell_length_b 14.1030(7) _cell_length_c 17.8654(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.468(2) _cell_angle_gamma 90.00 _cell_volume 6274.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9911 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 30.12 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6590 _exptl_absorpt_correction_T_max 0.8667 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 63359 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7764 _reflns_number_gt 6192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0418P)^2^+13.2729P] 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 7764 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 As1 As 0.0000 0.896983(19) 0.2500 0.02081(8) Uani 1 2 d S . . C1 C 0.11201(7) 0.95445(12) 0.17868(10) 0.0153(3) Uani 1 1 d . . . C2 C 0.17514(7) 0.87062(13) 0.12060(11) 0.0175(4) Uani 1 1 d . . . C3 C 0.19769(7) 0.95325(13) 0.14338(10) 0.0172(4) Uani 1 1 d . . . C4 C 0.08782(7) 0.78916(12) 0.14147(10) 0.0163(3) Uani 1 1 d . . . C5 C 0.09683(7) 0.72184(13) 0.19840(11) 0.0177(4) Uani 1 1 d . . . C6 C 0.06311(8) 0.64300(14) 0.19790(11) 0.0202(4) Uani 1 1 d . . . C7 C 0.02282(8) 0.63168(14) 0.14306(12) 0.0212(4) Uani 1 1 d . . . C8 C 0.01551(8) 0.69861(14) 0.08712(12) 0.0210(4) Uani 1 1 d . . . C9 C 0.04784(7) 0.77942(13) 0.08458(11) 0.0180(4) Uani 1 1 d . . . C10 C 0.14243(8) 0.73000(14) 0.25772(11) 0.0205(4) Uani 1 1 d . . . C11 C 0.12218(9) 0.73051(17) 0.33716(12) 0.0297(5) Uani 1 1 d . . . H11A H 0.0975 0.7839 0.3428 0.045 Uiso 1 1 calc R . . H11B H 0.1527 0.7370 0.3732 0.045 Uiso 1 1 calc R . . H11C H 0.1033 0.6710 0.3464 0.045 Uiso 1 1 calc R . . C12 C 0.18295(8) 0.65001(16) 0.24746(13) 0.0301(5) Uani 1 1 d . . . H12A H 0.1658 0.5889 0.2570 0.045 Uiso 1 1 calc R . . H12B H 0.2138 0.6587 0.2827 0.045 Uiso 1 1 calc R . . H12C H 0.1952 0.6512 0.1961 0.045 Uiso 1 1 calc R . . C13 C 0.03951(8) 0.85001(14) 0.02094(11) 0.0222(4) Uani 1 1 d . . . C14 C -0.01870(9) 0.88611(16) 0.01611(15) 0.0365(5) Uani 1 1 d . . . H14A H -0.0433 0.8321 0.0102 0.055 Uiso 1 1 calc R . . H14B H -0.0237 0.9286 -0.0271 0.055 Uiso 1 1 calc R . . H14C H -0.0263 0.9206 0.0621 0.055 Uiso 1 1 calc R . . C15 C 0.05480(11) 0.80505(17) -0.05306(13) 0.0373(5) Uani 1 1 d . . . H15A H 0.0928 0.7869 -0.0498 0.056 Uiso 1 1 calc R . . H15B H 0.0487 0.8508 -0.0938 0.056 Uiso 1 1 calc R . . H15C H 0.0327 0.7486 -0.0629 0.056 Uiso 1 1 calc R . . C16 C 0.16723(7) 1.09295(13) 0.21935(10) 0.0167(4) Uani 1 1 d . . . C17 C 0.17699(7) 1.08778(14) 0.29694(11) 0.0198(4) Uani 1 1 d . . . C18 C 0.18655(8) 1.17261(15) 0.33508(12) 0.0222(4) Uani 1 1 d . . . C19 C 0.18597(8) 1.25834(14) 0.29752(12) 0.0228(4) Uani 1 1 d . . . C20 C 0.17544(8) 1.26146(14) 0.22090(12) 0.0212(4) Uani 1 1 d . . . C21 C 0.16583(7) 1.17851(13) 0.17967(10) 0.0176(4) Uani 1 1 d . . . C22 C 0.15723(8) 1.18219(14) 0.09506(11) 0.0220(4) Uani 1 1 d . . . C23 C 0.12601(10) 1.26980(16) 0.06769(13) 0.0333(5) Uani 1 1 d . . . H23A H 0.0917 1.2728 0.0924 0.050 Uiso 1 1 calc R . . H23B H 0.1193 1.2658 0.0133 0.050 Uiso 1 1 calc R . . H23C H 0.1470 1.3269 0.0798 0.050 Uiso 1 1 calc R . . C24 C 0.21178(9) 1.17955(17) 0.05875(12) 0.0330(5) Uani 1 1 d . . . H24A H 0.2331 1.2347 0.0752 0.049 Uiso 1 1 calc R . . H24B H 0.2063 1.1810 0.0041 0.049 Uiso 1 1 calc R . . H24C H 0.2308 1.1213 0.0737 0.049 Uiso 1 1 calc R . . C25 C 0.17954(9) 0.99385(15) 0.33884(12) 0.0244(4) Uani 1 1 d . . . C26 C 0.23752(10) 0.9603(2) 0.34798(16) 0.0467(7) Uani 1 1 d . . . H26A H 0.2528 0.9544 0.2986 0.070 Uiso 1 1 calc R . . H26B H 0.2386 0.8985 0.3731 0.070 Uiso 1 1 calc R . . H26C H 0.2585 1.0063 0.3781 0.070 Uiso 1 1 calc R . . C27 C 0.15337(11) 0.99865(18) 0.41435(13) 0.0383(6) Uani 1 1 d . . . H27A H 0.1746 1.0401 0.4483 0.057 Uiso 1 1 calc R . . H27B H 0.1518 0.9349 0.4359 0.057 Uiso 1 1 calc R . . H27C H 0.1169 1.0241 0.4074 0.057 Uiso 1 1 calc R . . C1S C 0.03281(9) 0.38179(15) 0.20516(13) 0.0314(5) Uani 1 1 d . . . H1S1 H 0.0706 0.4036 0.2086 0.038 Uiso 1 1 calc R . . H1S2 H 0.0199 0.3839 0.1520 0.038 Uiso 1 1 calc R . . C2S C 0.02845(9) 0.28156(15) 0.23589(13) 0.0304(5) Uani 1 1 d . . . H2S1 H 0.0554 0.2699 0.2771 0.036 Uiso 1 1 calc R . . H2S2 H 0.0327 0.2335 0.1962 0.036 Uiso 1 1 calc R . . C3S C 0.11298(9) 0.54669(17) 0.88817(13) 0.0339(5) Uani 1 1 d . . . H3S1 H 0.0956 0.5086 0.8474 0.041 Uiso 1 1 calc R . . H3S2 H 0.1088 0.6147 0.8756 0.041 Uiso 1 1 calc R . . C4S C 0.08812(9) 0.52505(17) 0.96204(14) 0.0347(5) Uani 1 1 d . . . H4S1 H 0.0788 0.4571 0.9662 0.042 Uiso 1 1 calc R . . H4S2 H 0.0557 0.5640 0.9691 0.042 Uiso 1 1 calc R . . C5S C 0.13364(9) 0.55233(18) 1.01738(13) 0.0352(5) Uani 1 1 d . . . H5S1 H 0.1308 0.5185 1.0656 0.042 Uiso 1 1 calc R . . H5S2 H 0.1343 0.6215 1.0267 0.042 Uiso 1 1 calc R . . C6S C 0.18280(10) 0.5202(2) 0.97632(14) 0.0401(6) Uani 1 1 d . . . H6S1 H 0.2134 0.5632 0.9879 0.048 Uiso 1 1 calc R . . H6S2 H 0.1932 0.4552 0.9919 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.2500 0.7500 0.0000 0.0433(2) Uani 1 2 d S . . H2 H 0.1895(9) 0.8202(17) 0.0940(13) 0.025(6) Uiso 1 1 d . . . H3 H 0.2319(10) 0.9747(16) 0.1405(13) 0.025(6) Uiso 1 1 d . . . H6 H 0.0673(9) 0.6009(16) 0.2350(13) 0.022(6) Uiso 1 1 d . . . H7 H 0.0006(10) 0.5807(18) 0.1436(13) 0.028(6) Uiso 1 1 d . . . H8 H -0.0109(10) 0.6920(17) 0.0486(14) 0.028(6) Uiso 1 1 d . . . H10 H 0.1609(8) 0.7891(15) 0.2499(12) 0.015(5) Uiso 1 1 d . . . H13 H 0.0618(9) 0.9040(15) 0.0310(12) 0.017(5) Uiso 1 1 d . . . H18 H 0.1944(10) 1.1710(18) 0.3848(15) 0.032(7) Uiso 1 1 d . . . H19 H 0.1931(8) 1.3142(16) 0.3232(12) 0.018(5) Uiso 1 1 d . . . H20 H 0.1751(9) 1.3197(17) 0.1974(13) 0.027(6) Uiso 1 1 d . . . H22 H 0.1371(9) 1.1281(16) 0.0813(12) 0.017(5) Uiso 1 1 d . . . H25 H 0.1616(10) 0.9532(18) 0.3104(14) 0.028(6) Uiso 1 1 d . . . N1 N 0.12224(6) 0.87191(10) 0.14308(8) 0.0151(3) Uani 1 1 d . . . N2 N 0.15875(6) 1.00472(11) 0.17880(8) 0.0156(3) Uani 1 1 d . . . O1S O 0.0000 0.44060(15) 0.2500 0.0335(5) Uani 1 2 d S . . O2S O 0.16860(7) 0.52260(12) 0.89783(9) 0.0372(4) Uani 1 1 d . . . P2 P 0.05310(2) 1.01093(4) 0.21280(4) 0.03658(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.01658(14) 0.01757(14) 0.02902(16) 0.000 0.00960(10) 0.000 C1 0.0136(8) 0.0148(8) 0.0178(9) 0.0004(7) 0.0026(6) -0.0015(6) C2 0.0134(8) 0.0196(9) 0.0199(9) -0.0013(7) 0.0066(7) 0.0006(7) C3 0.0127(8) 0.0211(9) 0.0182(9) -0.0012(7) 0.0050(7) -0.0005(7) C4 0.0133(8) 0.0133(8) 0.0226(9) -0.0027(7) 0.0058(7) -0.0019(6) C5 0.0145(8) 0.0171(8) 0.0218(9) -0.0013(7) 0.0041(7) 0.0011(7) C6 0.0204(9) 0.0170(9) 0.0235(10) 0.0029(8) 0.0041(7) 0.0008(7) C7 0.0176(9) 0.0168(9) 0.0295(11) -0.0007(8) 0.0043(7) -0.0035(7) C8 0.0167(9) 0.0199(9) 0.0265(10) -0.0019(8) 0.0010(8) -0.0018(7) C9 0.0157(8) 0.0169(8) 0.0216(9) -0.0013(7) 0.0031(7) 0.0006(7) C10 0.0182(9) 0.0208(9) 0.0226(10) 0.0028(7) 0.0008(7) -0.0023(7) C11 0.0284(11) 0.0379(12) 0.0228(11) 0.0007(9) 0.0009(8) -0.0013(9) C12 0.0185(10) 0.0344(12) 0.0372(12) 0.0028(9) 0.0005(8) 0.0055(9) C13 0.0225(9) 0.0181(9) 0.0255(10) 0.0025(8) -0.0037(8) -0.0050(8) C14 0.0263(11) 0.0292(12) 0.0528(15) 0.0113(10) -0.0120(10) -0.0031(9) C15 0.0582(16) 0.0288(11) 0.0249(12) 0.0009(9) 0.0029(10) -0.0095(11) C16 0.0126(8) 0.0182(9) 0.0195(9) -0.0035(7) 0.0035(6) -0.0026(7) C17 0.0158(8) 0.0227(9) 0.0210(9) -0.0003(7) 0.0036(7) 0.0001(7) C18 0.0192(9) 0.0287(10) 0.0188(10) -0.0057(8) 0.0015(7) -0.0012(8) C19 0.0206(9) 0.0208(9) 0.0269(11) -0.0091(8) 0.0024(8) -0.0033(7) C20 0.0187(9) 0.0172(9) 0.0280(11) -0.0015(8) 0.0037(7) -0.0033(7) C21 0.0149(8) 0.0190(9) 0.0191(9) -0.0020(7) 0.0035(7) -0.0044(7) C22 0.0258(10) 0.0195(9) 0.0209(10) 0.0001(7) 0.0030(8) -0.0079(8) C23 0.0433(13) 0.0304(11) 0.0258(11) 0.0049(9) -0.0035(9) -0.0025(10) C24 0.0371(12) 0.0397(13) 0.0229(11) -0.0009(9) 0.0125(9) -0.0097(10) C25 0.0287(11) 0.0253(10) 0.0193(10) 0.0020(8) 0.0030(8) 0.0018(8) C26 0.0400(14) 0.0514(16) 0.0498(16) 0.0255(13) 0.0137(12) 0.0194(12) C27 0.0482(14) 0.0370(13) 0.0309(13) 0.0102(10) 0.0173(10) 0.0074(11) C1S 0.0339(12) 0.0253(11) 0.0355(12) -0.0002(9) 0.0084(9) 0.0011(9) C2S 0.0305(11) 0.0222(10) 0.0385(13) 0.0000(9) 0.0033(9) 0.0024(9) C3S 0.0356(12) 0.0309(12) 0.0351(13) -0.0027(9) 0.0008(10) -0.0022(9) C4S 0.0272(11) 0.0346(12) 0.0425(14) -0.0042(10) 0.0056(9) 0.0003(9) C5S 0.0311(12) 0.0431(14) 0.0315(12) -0.0023(10) 0.0036(9) 0.0030(10) C6S 0.0297(12) 0.0550(16) 0.0358(13) 0.0042(11) 0.0058(10) 0.0060(11) Cl1 0.0495(5) 0.0627(6) 0.0179(4) -0.0006(3) 0.0044(3) 0.0373(4) N1 0.0127(7) 0.0150(7) 0.0180(8) -0.0021(6) 0.0042(6) -0.0013(5) N2 0.0129(7) 0.0162(7) 0.0181(8) -0.0017(6) 0.0048(6) -0.0020(6) O1S 0.0414(13) 0.0183(10) 0.0419(13) 0.000 0.0141(10) 0.000 O2S 0.0349(9) 0.0432(10) 0.0343(9) -0.0023(7) 0.0107(7) 0.0018(7) P2 0.0236(3) 0.0160(3) 0.0724(5) -0.0046(3) 0.0275(3) -0.0017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 P2 2.2027(6) 2 ? As1 P2 2.2027(6) . ? C1 N1 1.356(2) . ? C1 N2 1.364(2) . ? C1 P2 1.7999(18) . ? C2 C3 1.349(3) . ? C2 N1 1.395(2) . ? C3 N2 1.387(2) . ? C4 C9 1.399(3) . ? C4 C5 1.402(3) . ? C4 N1 1.448(2) . ? C5 C6 1.394(3) . ? C5 C10 1.525(3) . ? C6 C7 1.382(3) . ? C7 C8 1.381(3) . ? C8 C9 1.398(3) . ? C9 C13 1.519(3) . ? C10 C11 1.527(3) . ? C10 C12 1.531(3) . ? C13 C15 1.529(3) . ? C13 C14 1.537(3) . ? C16 C17 1.399(3) . ? C16 C21 1.399(3) . ? C16 N2 1.451(2) . ? C17 C18 1.392(3) . ? C17 C25 1.522(3) . ? C18 C19 1.383(3) . ? C19 C20 1.383(3) . ? C20 C21 1.398(3) . ? C21 C22 1.518(3) . ? C22 C23 1.529(3) . ? C22 C24 1.532(3) . ? C25 C26 1.523(3) . ? C25 C27 1.525(3) . ? C1S O1S 1.434(2) . ? C1S C2S 1.522(3) . ? C2S C2S 1.526(4) 2 ? C3S O2S 1.431(3) . ? C3S C4S 1.513(3) . ? C4S C5S 1.522(3) . ? C5S C6S 1.524(3) . ? C6S O2S 1.432(3) . ? O1S C1S 1.434(2) 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 P2 As1 P2 86.30(3) 2 . ? N1 C1 N2 105.62(15) . . ? N1 C1 P2 135.34(13) . . ? N2 C1 P2 118.61(13) . . ? C3 C2 N1 106.78(16) . . ? C2 C3 N2 107.40(16) . . ? C9 C4 C5 123.17(16) . . ? C9 C4 N1 119.76(16) . . ? C5 C4 N1 117.07(16) . . ? C6 C5 C4 117.24(17) . . ? C6 C5 C10 119.74(17) . . ? C4 C5 C10 122.98(16) . . ? C7 C6 C5 121.10(18) . . ? C8 C7 C6 120.22(18) . . ? C7 C8 C9 121.49(18) . . ? C8 C9 C4 116.76(17) . . ? C8 C9 C13 119.89(17) . . ? C4 C9 C13 123.33(16) . . ? C5 C10 C11 112.33(16) . . ? C5 C10 C12 109.71(16) . . ? C11 C10 C12 111.17(17) . . ? C9 C13 C15 110.14(17) . . ? C9 C13 C14 110.94(17) . . ? C15 C13 C14 111.02(19) . . ? C17 C16 C21 123.13(17) . . ? C17 C16 N2 117.74(16) . . ? C21 C16 N2 119.13(16) . . ? C18 C17 C16 117.32(18) . . ? C18 C17 C25 120.32(18) . . ? C16 C17 C25 122.32(17) . . ? C19 C18 C17 121.06(19) . . ? C18 C19 C20 120.37(18) . . ? C19 C20 C21 121.05(18) . . ? C20 C21 C16 117.05(17) . . ? C20 C21 C22 120.64(17) . . ? C16 C21 C22 122.23(16) . . ? C21 C22 C23 113.20(17) . . ? C21 C22 C24 109.33(17) . . ? C23 C22 C24 109.45(18) . . ? C17 C25 C26 110.05(18) . . ? C17 C25 C27 112.70(18) . . ? C26 C25 C27 111.0(2) . . ? O1S C1S C2S 106.52(18) . . ? C1S C2S C2S 101.60(13) . 2 ? O2S C3S C4S 106.15(19) . . ? C3S C4S C5S 101.17(19) . . ? C4S C5S C6S 101.81(19) . . ? O2S C6S C5S 107.13(19) . . ? C1 N1 C2 110.20(15) . . ? C1 N1 C4 125.31(14) . . ? C2 N1 C4 123.39(15) . . ? C1 N2 C3 110.00(15) . . ? C1 N2 C16 123.57(14) . . ? C3 N2 C16 125.94(15) . . ? C1S O1S C1S 109.3(2) . 2 ? C3S O2S C6S 108.73(17) . . ? C1 P2 As1 106.80(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -0.5(2) . . . . ? C9 C4 C5 C6 -1.3(3) . . . . ? N1 C4 C5 C6 178.77(16) . . . . ? C9 C4 C5 C10 176.46(17) . . . . ? N1 C4 C5 C10 -3.5(3) . . . . ? C4 C5 C6 C7 0.5(3) . . . . ? C10 C5 C6 C7 -177.33(17) . . . . ? C5 C6 C7 C8 0.4(3) . . . . ? C6 C7 C8 C9 -0.7(3) . . . . ? C7 C8 C9 C4 -0.1(3) . . . . ? C7 C8 C9 C13 178.32(18) . . . . ? C5 C4 C9 C8 1.1(3) . . . . ? N1 C4 C9 C8 -178.98(16) . . . . ? C5 C4 C9 C13 -177.25(17) . . . . ? N1 C4 C9 C13 2.7(3) . . . . ? C6 C5 C10 C11 -59.9(2) . . . . ? C4 C5 C10 C11 122.3(2) . . . . ? C6 C5 C10 C12 64.2(2) . . . . ? C4 C5 C10 C12 -113.5(2) . . . . ? C8 C9 C13 C15 -67.1(2) . . . . ? C4 C9 C13 C15 111.2(2) . . . . ? C8 C9 C13 C14 56.2(2) . . . . ? C4 C9 C13 C14 -125.5(2) . . . . ? C21 C16 C17 C18 -1.1(3) . . . . ? N2 C16 C17 C18 178.27(16) . . . . ? C21 C16 C17 C25 -178.66(17) . . . . ? N2 C16 C17 C25 0.8(3) . . . . ? C16 C17 C18 C19 0.5(3) . . . . ? C25 C17 C18 C19 178.05(18) . . . . ? C17 C18 C19 C20 0.4(3) . . . . ? C18 C19 C20 C21 -0.8(3) . . . . ? C19 C20 C21 C16 0.1(3) . . . . ? C19 C20 C21 C22 -176.74(18) . . . . ? C17 C16 C21 C20 0.8(3) . . . . ? N2 C16 C21 C20 -178.57(16) . . . . ? C17 C16 C21 C22 177.66(17) . . . . ? N2 C16 C21 C22 -1.7(3) . . . . ? C20 C21 C22 C23 -36.6(2) . . . . ? C16 C21 C22 C23 146.72(18) . . . . ? C20 C21 C22 C24 85.7(2) . . . . ? C16 C21 C22 C24 -91.0(2) . . . . ? C18 C17 C25 C26 -82.9(2) . . . . ? C16 C17 C25 C26 94.5(2) . . . . ? C18 C17 C25 C27 41.6(3) . . . . ? C16 C17 C25 C27 -140.9(2) . . . . ? O1S C1S C2S C2S 31.3(3) . . . 2 ? O2S C3S C4S C5S 35.9(2) . . . . ? C3S C4S C5S C6S -36.9(2) . . . . ? C4S C5S C6S O2S 26.6(3) . . . . ? N2 C1 N1 C2 -0.3(2) . . . . ? P2 C1 N1 C2 171.74(16) . . . . ? N2 C1 N1 C4 168.03(16) . . . . ? P2 C1 N1 C4 -19.9(3) . . . . ? C3 C2 N1 C1 0.5(2) . . . . ? C3 C2 N1 C4 -168.08(17) . . . . ? C9 C4 N1 C1 89.6(2) . . . . ? C5 C4 N1 C1 -90.4(2) . . . . ? C9 C4 N1 C2 -103.5(2) . . . . ? C5 C4 N1 C2 76.4(2) . . . . ? N1 C1 N2 C3 0.0(2) . . . . ? P2 C1 N2 C3 -173.66(13) . . . . ? N1 C1 N2 C16 -172.38(16) . . . . ? P2 C1 N2 C16 14.0(2) . . . . ? C2 C3 N2 C1 0.3(2) . . . . ? C2 C3 N2 C16 172.49(17) . . . . ? C17 C16 N2 C1 76.6(2) . . . . ? C21 C16 N2 C1 -104.0(2) . . . . ? C17 C16 N2 C3 -94.5(2) . . . . ? C21 C16 N2 C3 84.9(2) . . . . ? C2S C1S O1S C1S -12.24(11) . . . 2 ? C4S C3S O2S C6S -20.0(2) . . . . ? C5S C6S O2S C3S -4.5(3) . . . . ? N1 C1 P2 As1 33.2(2) . . . . ? N2 C1 P2 As1 -155.51(13) . . . . ? P2 As1 P2 C1 176.27(8) 2 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.932 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.067 _database_code_depnum_ccdc_archive 'CCDC 937655' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_paspcc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common arsenyl[bis((1,3-bis(2,6-diisopropylphenyl)-1H-imidazol-2-ylidene)phosphine)] _chemical_melting_point ? _chemical_formula_moiety 'C54 H72 As1 N4 P2' _chemical_formula_sum 'C108 H144 As2 N8 P4' _chemical_formula_weight 1828.09 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' 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' As As 0.0499 2.0058 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'Cc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 10.2682(6) _cell_length_b 42.469(3) _cell_length_c 24.2300(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.756(2) _cell_angle_gamma 90.00 _cell_volume 10553.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9964 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.04 _exptl_crystal_description Platelette _exptl_crystal_colour Purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3896 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8369 _exptl_absorpt_correction_T_max 0.9711 _exptl_absorpt_process_details ' SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 117515 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 27.10 _reflns_number_total 22831 _reflns_number_gt 16569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0528P)^2^+1.0080P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.203(5) _refine_ls_number_reflns 22831 _refine_ls_number_parameters 1132 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.003 _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 As1 As 0.55012(3) 0.815612(8) 0.978412(13) 0.02466(9) Uani 1 1 d . . . As2 As 0.95895(3) 0.540672(8) 0.026804(13) 0.02165(9) Uani 1 1 d . . . C1 C 0.6319(3) 0.76368(8) 0.88752(13) 0.0208(8) Uani 1 1 d . . . C2 C 0.6639(4) 0.73765(9) 0.80785(13) 0.0266(8) Uani 1 1 d . . . H2 H 0.6846 0.7212 0.7831 0.032 Uiso 1 1 calc R . . C3 C 0.6288(4) 0.76702(8) 0.79365(14) 0.0281(9) Uani 1 1 d . . . H3 H 0.6191 0.7752 0.7572 0.034 Uiso 1 1 calc R . . C4 C 0.7028(3) 0.70754(8) 0.89648(13) 0.0209(8) Uani 1 1 d . . . C5 C 0.6072(3) 0.68570(8) 0.90934(13) 0.0243(8) Uani 1 1 d . . . C6 C 0.6488(4) 0.65875(8) 0.93789(13) 0.0261(8) Uani 1 1 d . . . H6 H 0.5863 0.6434 0.9475 0.031 Uiso 1 1 calc R . . C7 C 0.7787(4) 0.65385(8) 0.95253(14) 0.0283(9) Uani 1 1 d . . . H7 H 0.8049 0.6351 0.9713 0.034 Uiso 1 1 calc R . . C8 C 0.8704(4) 0.67591(8) 0.94014(13) 0.0249(8) Uani 1 1 d . . . H8 H 0.9594 0.6723 0.9506 0.030 Uiso 1 1 calc R . . C9 C 0.8345(3) 0.70379(8) 0.91217(13) 0.0233(8) Uani 1 1 d . . . C10 C 0.9378(4) 0.72817(9) 0.90018(15) 0.0299(9) Uani 1 1 d . . . H10 H 0.8924 0.7470 0.8836 0.036 Uiso 1 1 calc R . . C11 C 1.0313(4) 0.71566(11) 0.85819(17) 0.0473(11) Uani 1 1 d . . . H11A H 1.0803 0.6978 0.8742 0.071 Uiso 1 1 calc R . . H11B H 1.0920 0.7324 0.8486 0.071 Uiso 1 1 calc R . . H11C H 0.9814 0.7088 0.8248 0.071 Uiso 1 1 calc R . . C12 C 1.0127(4) 0.73889(10) 0.95374(16) 0.0378(10) Uani 1 1 d . . . H12A H 0.9508 0.7471 0.9798 0.057 Uiso 1 1 calc R . . H12B H 1.0749 0.7554 0.9450 0.057 Uiso 1 1 calc R . . H12C H 1.0598 0.7209 0.9704 0.057 Uiso 1 1 calc R . . C13 C 0.4631(4) 0.69088(9) 0.89452(16) 0.0325(9) Uani 1 1 d . . . H13 H 0.4539 0.7107 0.8723 0.039 Uiso 1 1 calc R . . C14 C 0.3866(4) 0.69481(13) 0.94668(18) 0.0551(13) Uani 1 1 d . . . H14A H 0.3946 0.6756 0.9690 0.083 Uiso 1 1 calc R . . H14B H 0.2946 0.6986 0.9363 0.083 Uiso 1 1 calc R . . H14C H 0.4217 0.7127 0.9682 0.083 Uiso 1 1 calc R . . C15 C 0.4064(4) 0.66359(9) 0.85960(17) 0.0420(10) Uani 1 1 d . . . H15A H 0.4509 0.6624 0.8248 0.063 Uiso 1 1 calc R . . H15B H 0.3131 0.6671 0.8518 0.063 Uiso 1 1 calc R . . H15C H 0.4192 0.6438 0.8799 0.063 Uiso 1 1 calc R . . C16 C 0.5763(3) 0.81624(8) 0.84331(13) 0.0172(8) Uani 1 1 d . . . C17 C 0.6780(3) 0.83833(8) 0.84968(13) 0.0223(8) Uani 1 1 d . . . C18 C 0.6441(3) 0.87025(8) 0.84916(13) 0.0240(8) Uani 1 1 d . . . H18 H 0.7106 0.8858 0.8523 0.029 Uiso 1 1 calc R . . C19 C 0.5144(3) 0.87954(8) 0.84407(13) 0.0239(8) Uani 1 1 d . . . H19 H 0.4928 0.9013 0.8449 0.029 Uiso 1 1 calc R . . C20 C 0.4162(3) 0.85722(8) 0.83777(13) 0.0205(8) Uani 1 1 d . . . H20 H 0.3280 0.8639 0.8337 0.025 Uiso 1 1 calc R . . C21 C 0.4449(3) 0.82504(8) 0.83729(13) 0.0189(7) Uani 1 1 d . . . C22 C 0.3340(3) 0.80127(8) 0.83012(14) 0.0257(8) Uani 1 1 d . . . H22 H 0.3728 0.7797 0.8293 0.031 Uiso 1 1 calc R . . C23 C 0.2443(4) 0.80287(13) 0.87857(17) 0.0548(13) Uani 1 1 d . . . H23A H 0.2956 0.7997 0.9133 0.082 Uiso 1 1 calc R . . H23B H 0.1776 0.7864 0.8744 0.082 Uiso 1 1 calc R . . H23C H 0.2020 0.8236 0.8791 0.082 Uiso 1 1 calc R . . C24 C 0.2551(4) 0.80659(9) 0.77569(15) 0.0287(9) Uani 1 1 d . . . H24A H 0.2103 0.8269 0.7769 0.043 Uiso 1 1 calc R . . H24B H 0.1906 0.7897 0.7703 0.043 Uiso 1 1 calc R . . H24C H 0.3139 0.8065 0.7450 0.043 Uiso 1 1 calc R . . C25 C 0.8202(3) 0.82843(10) 0.85697(15) 0.0308(9) Uani 1 1 d . . . H25 H 0.8232 0.8053 0.8650 0.037 Uiso 1 1 calc R . . C26 C 0.8908(4) 0.84564(11) 0.90487(16) 0.0446(11) Uani 1 1 d . . . H26A H 0.8981 0.8680 0.8958 0.067 Uiso 1 1 calc R . . H26B H 0.9782 0.8367 0.9113 0.067 Uiso 1 1 calc R . . H26C H 0.8416 0.8432 0.9383 0.067 Uiso 1 1 calc R . . C27 C 0.8889(4) 0.83426(16) 0.80336(18) 0.0734(18) Uani 1 1 d . . . H27A H 0.8413 0.8235 0.7728 0.110 Uiso 1 1 calc R . . H27B H 0.9782 0.8261 0.8070 0.110 Uiso 1 1 calc R . . H27C H 0.8912 0.8569 0.7958 0.110 Uiso 1 1 calc R . . C28 C 0.6151(3) 0.83791(8) 1.10366(13) 0.0206(8) Uani 1 1 d . . . C29 C 0.4790(3) 0.85893(9) 1.16499(14) 0.0274(9) Uani 1 1 d . . . H29 H 0.4013 0.8658 1.1810 0.033 Uiso 1 1 calc R . . C30 C 0.5993(3) 0.86174(9) 1.18750(14) 0.0288(9) Uani 1 1 d . . . H30 H 0.6230 0.8707 1.2225 0.035 Uiso 1 1 calc R . . C31 C 0.3702(3) 0.83399(8) 1.08241(13) 0.0201(8) Uani 1 1 d . . . C32 C 0.3215(3) 0.80354(9) 1.09131(14) 0.0237(8) Uani 1 1 d . . . C33 C 0.2017(4) 0.79612(9) 1.06583(15) 0.0307(9) Uani 1 1 d . . . H33 H 0.1664 0.7757 1.0708 0.037 Uiso 1 1 calc R . . C34 C 0.1321(4) 0.81777(9) 1.03328(16) 0.0347(10) Uani 1 1 d . . . H34 H 0.0485 0.8124 1.0175 0.042 Uiso 1 1 calc R . . C35 C 0.1850(3) 0.84726(9) 1.02391(14) 0.0291(9) Uani 1 1 d . . . H35 H 0.1375 0.8618 1.0010 0.035 Uiso 1 1 calc R . . C36 C 0.3056(3) 0.85589(9) 1.04731(13) 0.0233(8) Uani 1 1 d . . . C37 C 0.3662(3) 0.88783(8) 1.03545(14) 0.0261(8) Uani 1 1 d . . . H37 H 0.4593 0.8872 1.0496 0.031 Uiso 1 1 calc R . . C38 C 0.3001(4) 0.91456(9) 1.06498(17) 0.0430(11) Uani 1 1 d . . . H38A H 0.2091 0.9162 1.0512 0.064 Uiso 1 1 calc R . . H38B H 0.3455 0.9344 1.0580 0.064 Uiso 1 1 calc R . . H38C H 0.3032 0.9103 1.1048 0.064 Uiso 1 1 calc R . . C39 C 0.3655(4) 0.89434(9) 0.97342(15) 0.0389(10) Uani 1 1 d . . . H39A H 0.2762 0.8926 0.9575 0.058 Uiso 1 1 calc R . . H39B H 0.4212 0.8790 0.9558 0.058 Uiso 1 1 calc R . . H39C H 0.3985 0.9156 0.9672 0.058 Uiso 1 1 calc R . . C40 C 0.3974(4) 0.77907(9) 1.12654(15) 0.0296(9) Uani 1 1 d . . . H40 H 0.4874 0.7875 1.1341 0.036 Uiso 1 1 calc R . . C41 C 0.3372(5) 0.77408(11) 1.18196(17) 0.0510(12) Uani 1 1 d . . . H41A H 0.2485 0.7658 1.1760 0.076 Uiso 1 1 calc R . . H41B H 0.3343 0.7942 1.2017 0.076 Uiso 1 1 calc R . . H41C H 0.3900 0.7590 1.2039 0.076 Uiso 1 1 calc R . . C42 C 0.4098(5) 0.74789(10) 1.09678(18) 0.0556(13) Uani 1 1 d . . . H42A H 0.4667 0.7338 1.1190 0.083 Uiso 1 1 calc R . . H42B H 0.4473 0.7514 1.0609 0.083 Uiso 1 1 calc R . . H42C H 0.3234 0.7383 1.0912 0.083 Uiso 1 1 calc R . . C43 C 0.8232(3) 0.84618(8) 1.16061(13) 0.0220(8) Uani 1 1 d . . . C44 C 0.9015(3) 0.87190(9) 1.14894(15) 0.0253(8) Uani 1 1 d . . . C45 C 1.0344(3) 0.86910(9) 1.16218(15) 0.0319(9) Uani 1 1 d . . . H45 H 1.0908 0.8862 1.1550 0.038 Uiso 1 1 calc R . . C46 C 1.0863(4) 0.84158(10) 1.18591(16) 0.0346(10) Uani 1 1 d . . . H46 H 1.1768 0.8402 1.1958 0.042 Uiso 1 1 calc R . . C47 C 1.0055(4) 0.81648(9) 1.19477(15) 0.0297(9) Uani 1 1 d . . . H47 H 1.0419 0.7976 1.2098 0.036 Uiso 1 1 calc R . . C48 C 0.8723(4) 0.81788(8) 1.18249(15) 0.0249(9) Uani 1 1 d . . . C49 C 0.7863(4) 0.78945(9) 1.19119(14) 0.0306(9) Uani 1 1 d . . . H49 H 0.7016 0.7933 1.1702 0.037 Uiso 1 1 calc R . . C50 C 0.7564(5) 0.78545(10) 1.25141(16) 0.0492(12) Uani 1 1 d . . . H50A H 0.6894 0.7692 1.2547 0.074 Uiso 1 1 calc R . . H50B H 0.7245 0.8054 1.2658 0.074 Uiso 1 1 calc R . . H50C H 0.8358 0.7791 1.2726 0.074 Uiso 1 1 calc R . . C51 C 0.8435(5) 0.75930(10) 1.16887(18) 0.0564(14) Uani 1 1 d . . . H51A H 0.9254 0.7544 1.1896 0.085 Uiso 1 1 calc R . . H51B H 0.8604 0.7621 1.1297 0.085 Uiso 1 1 calc R . . H51C H 0.7817 0.7420 1.1729 0.085 Uiso 1 1 calc R . . C52 C 0.8481(4) 0.90151(9) 1.12030(16) 0.0308(9) Uani 1 1 d . . . H52 H 0.7518 0.8987 1.1141 0.037 Uiso 1 1 calc R . . C53 C 0.8703(5) 0.93057(10) 1.1557(2) 0.0582(13) Uani 1 1 d . . . H53A H 0.8266 0.9280 1.1905 0.087 Uiso 1 1 calc R . . H53B H 0.8345 0.9490 1.1359 0.087 Uiso 1 1 calc R . . H53C H 0.9640 0.9335 1.1635 0.087 Uiso 1 1 calc R . . C54 C 0.9064(5) 0.90490(13) 1.06355(19) 0.0678(16) Uani 1 1 d . . . H54A H 1.0014 0.9067 1.0682 0.102 Uiso 1 1 calc R . . H54B H 0.8710 0.9238 1.0451 0.102 Uiso 1 1 calc R . . H54C H 0.8840 0.8863 1.0410 0.102 Uiso 1 1 calc R . . C55 C 0.8698(3) 0.58836(8) 0.12278(13) 0.0182(7) Uani 1 1 d . . . C56 C 0.8558(4) 0.61360(9) 0.20525(13) 0.0321(9) Uani 1 1 d . . . H56 H 0.8419 0.6296 0.2317 0.039 Uiso 1 1 calc R . . C57 C 0.8939(4) 0.58406(9) 0.21590(14) 0.0300(9) Uani 1 1 d . . . H57 H 0.9121 0.5753 0.2515 0.036 Uiso 1 1 calc R . . C58 C 0.8059(3) 0.64505(8) 0.11946(12) 0.0203(8) Uani 1 1 d . . . C59 C 0.6735(3) 0.65066(8) 0.10552(13) 0.0225(8) Uani 1 1 d . . . C60 C 0.6420(3) 0.67934(8) 0.07952(14) 0.0241(8) Uani 1 1 d . . . H60 H 0.5535 0.6840 0.0696 0.029 Uiso 1 1 calc R . . C61 C 0.7374(4) 0.70098(8) 0.06804(14) 0.0272(9) Uani 1 1 d . . . H61 H 0.7142 0.7205 0.0512 0.033 Uiso 1 1 calc R . . C62 C 0.8661(4) 0.69412(8) 0.08108(14) 0.0246(8) Uani 1 1 d . . . H62 H 0.9309 0.7090 0.0722 0.029 Uiso 1 1 calc R . . C63 C 0.9045(3) 0.66628(8) 0.10676(13) 0.0224(8) Uani 1 1 d . . . C64 C 1.0479(3) 0.65883(9) 0.12061(14) 0.0311(9) Uani 1 1 d . . . H64 H 1.0542 0.6363 0.1325 0.037 Uiso 1 1 calc R . . C65 C 1.1304(4) 0.66296(12) 0.07043(17) 0.0519(13) Uani 1 1 d . . . H65A H 1.0957 0.6496 0.0402 0.078 Uiso 1 1 calc R . . H65B H 1.2207 0.6569 0.0802 0.078 Uiso 1 1 calc R . . H65C H 1.1277 0.6850 0.0587 0.078 Uiso 1 1 calc R . . C66 C 1.1008(4) 0.67952(10) 0.16896(16) 0.0443(11) Uani 1 1 d . . . H66A H 1.0905 0.7018 0.1590 0.066 Uiso 1 1 calc R . . H66B H 1.1934 0.6749 0.1767 0.066 Uiso 1 1 calc R . . H66C H 1.0522 0.6750 0.2019 0.066 Uiso 1 1 calc R . . C67 C 0.5670(4) 0.62723(9) 0.11711(15) 0.0298(9) Uani 1 1 d . . . H67 H 0.6098 0.6078 0.1328 0.036 Uiso 1 1 calc R . . C68 C 0.4898(4) 0.61786(10) 0.06456(16) 0.0393(10) Uani 1 1 d . . . H68A H 0.4498 0.6366 0.0474 0.059 Uiso 1 1 calc R . . H68B H 0.4215 0.6029 0.0736 0.059 Uiso 1 1 calc R . . H68C H 0.5483 0.6080 0.0388 0.059 Uiso 1 1 calc R . . C69 C 0.4776(4) 0.64039(11) 0.16052(17) 0.0446(11) Uani 1 1 d . . . H69A H 0.5293 0.6452 0.1945 0.067 Uiso 1 1 calc R . . H69B H 0.4108 0.6247 0.1684 0.067 Uiso 1 1 calc R . . H69C H 0.4354 0.6597 0.1464 0.067 Uiso 1 1 calc R . . C70 C 0.9400(3) 0.53544(8) 0.16316(13) 0.0176(8) Uani 1 1 d . . . C71 C 1.0716(3) 0.52836(8) 0.17298(13) 0.0216(8) Uani 1 1 d . . . C72 C 1.1046(4) 0.49624(9) 0.17482(14) 0.0281(9) Uani 1 1 d . . . H72 H 1.1928 0.4903 0.1824 0.034 Uiso 1 1 calc R . . C73 C 1.0124(4) 0.47335(8) 0.16592(14) 0.0294(9) Uani 1 1 d . . . H73 H 1.0368 0.4518 0.1678 0.035 Uiso 1 1 calc R . . C74 C 0.8833(4) 0.48155(8) 0.15412(14) 0.0278(9) Uani 1 1 d . . . H74 H 0.8209 0.4654 0.1467 0.033 Uiso 1 1 calc R . . C75 C 0.8427(3) 0.51287(8) 0.15287(12) 0.0191(8) Uani 1 1 d . . . C76 C 0.7007(3) 0.52172(9) 0.14232(13) 0.0270(9) Uani 1 1 d . . . H76 H 0.6980 0.5440 0.1289 0.032 Uiso 1 1 calc R . . C77 C 0.6298(4) 0.52057(14) 0.19602(16) 0.0596(15) Uani 1 1 d . . . H77A H 0.6334 0.4991 0.2109 0.089 Uiso 1 1 calc R . . H77B H 0.5386 0.5268 0.1889 0.089 Uiso 1 1 calc R . . H77C H 0.6717 0.5351 0.2228 0.089 Uiso 1 1 calc R . . C78 C 0.6307(4) 0.50137(11) 0.09785(17) 0.0458(11) Uani 1 1 d . . . H78A H 0.6760 0.5031 0.0633 0.069 Uiso 1 1 calc R . . H78B H 0.5406 0.5087 0.0918 0.069 Uiso 1 1 calc R . . H78C H 0.6307 0.4794 0.1100 0.069 Uiso 1 1 calc R . . C79 C 1.1770(3) 0.55331(9) 0.17912(14) 0.0301(9) Uani 1 1 d . . . H79 H 1.1339 0.5743 0.1739 0.036 Uiso 1 1 calc R . . C80 C 1.2456(4) 0.55309(10) 0.23680(16) 0.0403(10) Uani 1 1 d . . . H80A H 1.2865 0.5325 0.2436 0.060 Uiso 1 1 calc R . . H80B H 1.1815 0.5571 0.2647 0.060 Uiso 1 1 calc R . . H80C H 1.3125 0.5696 0.2389 0.060 Uiso 1 1 calc R . . C81 C 1.2754(4) 0.54986(12) 0.13444(17) 0.0472(12) Uani 1 1 d . . . H81A H 1.3163 0.5290 0.1373 0.071 Uiso 1 1 calc R . . H81B H 1.3425 0.5662 0.1393 0.071 Uiso 1 1 calc R . . H81C H 1.2307 0.5521 0.0980 0.071 Uiso 1 1 calc R . . C82 C 0.8965(3) 0.52104(8) -0.10135(13) 0.0185(7) Uani 1 1 d . . . C83 C 0.9150(3) 0.50104(8) -0.18778(13) 0.0224(8) Uani 1 1 d . . . H83 H 0.8927 0.4936 -0.2240 0.027 Uiso 1 1 calc R . . C84 C 1.0352(3) 0.50268(8) -0.16379(13) 0.0219(8) Uani 1 1 d . . . H84 H 1.1136 0.4965 -0.1800 0.026 Uiso 1 1 calc R . . C85 C 0.6902(3) 0.51603(8) -0.16054(13) 0.0207(8) Uani 1 1 d . . . C86 C 0.6089(3) 0.49063(9) -0.15047(13) 0.0259(9) Uani 1 1 d . . . C87 C 0.4763(3) 0.49445(9) -0.16469(15) 0.0304(9) Uani 1 1 d . . . H87 H 0.4175 0.4776 -0.1590 0.036 Uiso 1 1 calc R . . C88 C 0.4298(4) 0.52236(10) -0.18689(15) 0.0343(10) Uani 1 1 d . . . H88 H 0.3395 0.5243 -0.1967 0.041 Uiso 1 1 calc R . . C89 C 0.5119(4) 0.54748(9) -0.19509(15) 0.0314(9) Uani 1 1 d . . . H89 H 0.4774 0.5666 -0.2101 0.038 Uiso 1 1 calc R . . C90 C 0.6452(4) 0.54508(9) -0.18145(14) 0.0253(9) Uani 1 1 d . . . C91 C 0.7356(4) 0.57307(9) -0.18833(15) 0.0329(9) Uani 1 1 d . . . H91 H 0.8157 0.5692 -0.1642 0.039 Uiso 1 1 calc R . . C92 C 0.7781(5) 0.57644(11) -0.24616(18) 0.0613(14) Uani 1 1 d . . . H92A H 0.8231 0.5572 -0.2570 0.092 Uiso 1 1 calc R . . H92B H 0.8374 0.5944 -0.2482 0.092 Uiso 1 1 calc R . . H92C H 0.7016 0.5799 -0.2712 0.092 Uiso 1 1 calc R . . C93 C 0.6763(6) 0.60398(12) -0.1696(3) 0.095(2) Uani 1 1 d . . . H93A H 0.6009 0.6093 -0.1942 0.143 Uiso 1 1 calc R . . H93B H 0.7415 0.6208 -0.1709 0.143 Uiso 1 1 calc R . . H93C H 0.6483 0.6017 -0.1317 0.143 Uiso 1 1 calc R . . C94 C 0.6569(4) 0.46032(9) -0.12281(15) 0.0314(9) Uani 1 1 d . . . H94 H 0.7543 0.4613 -0.1191 0.038 Uiso 1 1 calc R . . C95 C 0.6191(5) 0.43102(10) -0.15688(18) 0.0534(12) Uani 1 1 d . . . H95A H 0.5240 0.4290 -0.1596 0.080 Uiso 1 1 calc R . . H95B H 0.6572 0.4123 -0.1388 0.080 Uiso 1 1 calc R . . H95C H 0.6521 0.4330 -0.1940 0.080 Uiso 1 1 calc R . . C96 C 0.6056(4) 0.45839(11) -0.06464(16) 0.0494(12) Uani 1 1 d . . . H96A H 0.5101 0.4580 -0.0671 0.074 Uiso 1 1 calc R . . H96B H 0.6355 0.4768 -0.0432 0.074 Uiso 1 1 calc R . . H96C H 0.6384 0.4392 -0.0464 0.074 Uiso 1 1 calc R . . C97 C 1.1402(3) 0.52344(8) -0.07727(13) 0.0168(7) Uani 1 1 d . . . C98 C 1.1994(3) 0.49978(8) -0.04451(13) 0.0187(7) Uani 1 1 d . . . C99 C 1.3200(3) 0.50709(9) -0.01797(14) 0.0266(8) Uani 1 1 d . . . H99 H 1.3638 0.4916 0.0044 0.032 Uiso 1 1 calc R . . C100 C 1.3764(4) 0.53661(9) -0.02387(15) 0.0311(9) Uani 1 1 d . . . H100 H 1.4596 0.5409 -0.0067 0.037 Uiso 1 1 calc R . . C101 C 1.3116(3) 0.55966(9) -0.05454(15) 0.0291(9) Uani 1 1 d . . . H101 H 1.3500 0.5799 -0.0572 0.035 Uiso 1 1 calc R . . C102 C 1.1909(3) 0.55388(8) -0.08172(14) 0.0217(8) Uani 1 1 d . . . C103 C 1.1194(4) 0.57965(8) -0.11377(15) 0.0301(9) Uani 1 1 d . . . H103 H 1.0285 0.5720 -0.1221 0.036 Uiso 1 1 calc R . . C104 C 1.1782(5) 0.58654(10) -0.16848(17) 0.0491(12) Uani 1 1 d . . . H10J H 1.2720 0.5903 -0.1625 0.074 Uiso 1 1 calc R . . H10K H 1.1366 0.6052 -0.1851 0.074 Uiso 1 1 calc R . . H10L H 1.1643 0.5685 -0.1933 0.074 Uiso 1 1 calc R . . C105 C 1.1096(4) 0.60987(9) -0.07973(18) 0.0434(11) Uani 1 1 d . . . H10G H 1.0701 0.6051 -0.0447 0.065 Uiso 1 1 calc R . . H10H H 1.0554 0.6252 -0.1004 0.065 Uiso 1 1 calc R . . H10I H 1.1970 0.6186 -0.0723 0.065 Uiso 1 1 calc R . . C106 C 1.1364(3) 0.46772(8) -0.03703(14) 0.0244(8) Uani 1 1 d . . . H106 H 1.0460 0.4688 -0.0542 0.029 Uiso 1 1 calc R . . C107 C 1.2086(4) 0.44166(9) -0.06669(17) 0.0379(11) Uani 1 1 d . . . H10D H 1.2095 0.4465 -0.1062 0.057 Uiso 1 1 calc R . . H10E H 1.1641 0.4215 -0.0616 0.057 Uiso 1 1 calc R . . H10F H 1.2984 0.4402 -0.0512 0.057 Uiso 1 1 calc R . . C108 C 1.1246(4) 0.45995(9) 0.02444(15) 0.0348(9) Uani 1 1 d . . . H10A H 1.2104 0.4619 0.0437 0.052 Uiso 1 1 calc R . . H10B H 1.0927 0.4383 0.0282 0.052 Uiso 1 1 calc R . . H10C H 1.0634 0.4746 0.0406 0.052 Uiso 1 1 calc R . . N1 N 0.6649(3) 0.73534(6) 0.86505(11) 0.0220(7) Uani 1 1 d . . . N2 N 0.6090(3) 0.78335(6) 0.84248(11) 0.0200(7) Uani 1 1 d . . . N3 N 0.4867(3) 0.84408(7) 1.11393(11) 0.0201(6) Uani 1 1 d . . . N4 N 0.6832(3) 0.84915(7) 1.15048(11) 0.0221(7) Uani 1 1 d . . . N5 N 0.9022(3) 0.56840(6) 0.16576(10) 0.0196(6) Uani 1 1 d . . . N6 N 0.8405(3) 0.61640(7) 0.14818(11) 0.0228(7) Uani 1 1 d . . . N7 N 1.0252(3) 0.51506(6) -0.11095(10) 0.0163(6) Uani 1 1 d . . . N8 N 0.8291(3) 0.51227(7) -0.14979(11) 0.0230(7) Uani 1 1 d . . . P1 P 0.64244(10) 0.76880(2) 0.96010(4) 0.0302(2) Uani 1 1 d . . . P2 P 0.69798(9) 0.81923(2) 1.05065(4) 0.0273(2) Uani 1 1 d . . . P3 P 0.85433(10) 0.58518(2) 0.04997(3) 0.0264(2) Uani 1 1 d . . . P4 P 0.81234(9) 0.53804(3) -0.04634(4) 0.0293(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0313(2) 0.0267(2) 0.01583(17) -0.00368(15) -0.00105(15) 0.01212(17) As2 0.0273(2) 0.0238(2) 0.01379(17) -0.00372(14) -0.00079(14) 0.00861(16) C1 0.0226(19) 0.023(2) 0.0167(18) 0.0023(15) 0.0008(15) 0.0067(16) C2 0.039(2) 0.029(2) 0.0117(17) -0.0035(14) 0.0018(15) 0.0098(17) C3 0.044(2) 0.029(2) 0.0109(17) 0.0007(15) -0.0021(16) 0.0121(18) C4 0.032(2) 0.0165(18) 0.0138(16) 0.0003(14) -0.0004(14) 0.0111(16) C5 0.031(2) 0.021(2) 0.0208(18) -0.0047(15) -0.0007(15) 0.0054(16) C6 0.037(2) 0.020(2) 0.0208(18) 0.0005(15) 0.0028(16) -0.0006(17) C7 0.045(2) 0.0162(19) 0.0236(19) -0.0009(15) 0.0010(17) 0.0115(18) C8 0.029(2) 0.025(2) 0.0194(17) -0.0012(15) -0.0015(15) 0.0123(17) C9 0.030(2) 0.0193(19) 0.0205(18) -0.0045(14) 0.0055(15) 0.0084(16) C10 0.031(2) 0.028(2) 0.031(2) 0.0039(16) 0.0104(17) 0.0075(17) C11 0.038(2) 0.067(3) 0.038(2) -0.003(2) 0.013(2) 0.001(2) C12 0.037(2) 0.040(2) 0.037(2) -0.0019(18) 0.0108(18) -0.0108(19) C13 0.031(2) 0.030(2) 0.036(2) -0.0007(17) -0.0076(17) 0.0023(17) C14 0.036(3) 0.083(4) 0.047(3) -0.006(2) 0.006(2) 0.016(2) C15 0.034(2) 0.039(3) 0.052(3) 0.000(2) -0.009(2) -0.0036(19) C16 0.0216(19) 0.020(2) 0.0098(16) 0.0024(13) 0.0035(14) 0.0052(15) C17 0.024(2) 0.029(2) 0.0142(17) 0.0007(14) 0.0011(15) -0.0013(16) C18 0.022(2) 0.030(2) 0.0195(18) 0.0016(15) -0.0019(15) -0.0108(17) C19 0.038(2) 0.0172(19) 0.0163(17) -0.0007(14) -0.0022(15) 0.0021(17) C20 0.0178(18) 0.025(2) 0.0186(17) 0.0043(14) 0.0014(14) 0.0063(15) C21 0.024(2) 0.0175(19) 0.0150(17) 0.0043(14) -0.0008(14) 0.0005(16) C22 0.025(2) 0.020(2) 0.033(2) 0.0054(16) -0.0021(17) 0.0002(16) C23 0.041(3) 0.089(4) 0.034(2) 0.012(2) 0.004(2) -0.037(3) C24 0.022(2) 0.029(2) 0.036(2) -0.0042(17) 0.0008(16) -0.0061(17) C25 0.021(2) 0.044(2) 0.028(2) -0.0002(18) 0.0001(16) 0.0026(18) C26 0.025(2) 0.074(3) 0.034(2) -0.004(2) -0.0051(18) 0.000(2) C27 0.026(3) 0.160(6) 0.035(3) 0.002(3) 0.008(2) 0.010(3) C28 0.0195(19) 0.0214(19) 0.0208(18) 0.0042(14) 0.0009(15) -0.0030(15) C29 0.020(2) 0.037(2) 0.0254(19) -0.0139(16) 0.0066(16) 0.0025(17) C30 0.026(2) 0.040(2) 0.0209(18) -0.0138(16) 0.0024(16) 0.0005(17) C31 0.0152(18) 0.029(2) 0.0164(17) -0.0045(15) 0.0044(14) -0.0006(16) C32 0.022(2) 0.028(2) 0.0216(18) -0.0047(16) 0.0096(15) 0.0008(17) C33 0.030(2) 0.031(2) 0.032(2) -0.0069(17) 0.0040(18) -0.0091(18) C34 0.025(2) 0.046(3) 0.032(2) -0.0128(18) -0.0026(19) -0.0080(19) C35 0.025(2) 0.036(2) 0.027(2) -0.0031(17) -0.0028(16) 0.0056(18) C36 0.0200(19) 0.033(2) 0.0175(17) -0.0046(15) 0.0036(15) 0.0023(16) C37 0.024(2) 0.026(2) 0.028(2) 0.0026(16) 0.0009(16) -0.0006(16) C38 0.059(3) 0.032(2) 0.039(2) -0.0050(19) 0.016(2) -0.008(2) C39 0.055(3) 0.030(2) 0.033(2) 0.0062(17) 0.0118(19) 0.010(2) C40 0.025(2) 0.026(2) 0.038(2) 0.0027(17) 0.0067(17) -0.0010(17) C41 0.070(3) 0.051(3) 0.033(2) 0.011(2) 0.011(2) 0.023(2) C42 0.087(4) 0.033(3) 0.049(3) 0.002(2) 0.021(3) 0.018(2) C43 0.0158(18) 0.031(2) 0.0188(18) -0.0077(15) -0.0006(14) 0.0027(16) C44 0.0157(19) 0.030(2) 0.030(2) -0.0061(16) -0.0009(16) -0.0022(16) C45 0.021(2) 0.033(2) 0.041(2) 0.0055(18) -0.0011(17) -0.0029(17) C46 0.021(2) 0.044(3) 0.039(2) 0.0031(19) -0.0029(17) 0.0034(19) C47 0.028(2) 0.030(2) 0.031(2) 0.0026(16) -0.0082(17) 0.0084(17) C48 0.029(2) 0.030(2) 0.0160(18) -0.0045(15) -0.0020(16) 0.0020(17) C49 0.032(2) 0.033(2) 0.027(2) 0.0052(17) -0.0035(17) -0.0016(18) C50 0.068(3) 0.039(3) 0.042(3) 0.004(2) 0.020(2) -0.012(2) C51 0.091(4) 0.038(3) 0.042(3) -0.015(2) 0.021(3) -0.020(3) C52 0.024(2) 0.023(2) 0.045(2) 0.0012(18) -0.0068(17) 0.0057(17) C53 0.068(3) 0.030(3) 0.074(3) -0.004(2) -0.027(3) 0.012(2) C54 0.067(3) 0.079(4) 0.060(3) 0.036(3) 0.019(3) 0.039(3) C55 0.0192(18) 0.0190(19) 0.0166(17) -0.0027(14) 0.0020(14) 0.0056(15) C56 0.055(3) 0.028(2) 0.0124(17) -0.0046(15) -0.0012(17) 0.0121(19) C57 0.050(2) 0.028(2) 0.0116(17) -0.0016(15) -0.0027(16) 0.0097(18) C58 0.031(2) 0.0159(18) 0.0137(16) -0.0049(13) 0.0001(15) 0.0093(16) C59 0.032(2) 0.020(2) 0.0156(17) -0.0059(14) 0.0016(15) 0.0086(16) C60 0.0238(19) 0.025(2) 0.0231(18) -0.0038(15) -0.0023(15) 0.0118(16) C61 0.041(2) 0.0154(19) 0.0250(19) -0.0016(15) -0.0021(17) 0.0087(18) C62 0.032(2) 0.0195(19) 0.0217(18) -0.0060(15) 0.0007(16) -0.0034(17) C63 0.034(2) 0.0162(18) 0.0160(17) -0.0080(14) -0.0052(15) 0.0078(16) C64 0.029(2) 0.036(2) 0.027(2) -0.0080(17) -0.0053(16) 0.0058(18) C65 0.033(2) 0.087(4) 0.035(2) -0.015(2) -0.0029(19) 0.017(2) C66 0.035(2) 0.060(3) 0.037(2) -0.020(2) -0.0108(18) 0.004(2) C67 0.032(2) 0.028(2) 0.030(2) 0.0026(16) 0.0044(17) 0.0022(17) C68 0.042(2) 0.040(2) 0.037(2) 0.0007(18) 0.0091(19) -0.008(2) C69 0.044(3) 0.054(3) 0.037(2) -0.008(2) 0.020(2) -0.004(2) C70 0.028(2) 0.0152(18) 0.0102(16) 0.0026(13) 0.0018(14) 0.0083(15) C71 0.024(2) 0.025(2) 0.0164(18) 0.0038(15) 0.0055(14) 0.0048(17) C72 0.029(2) 0.028(2) 0.0268(19) 0.0091(16) 0.0039(16) 0.0134(17) C73 0.047(3) 0.0138(19) 0.028(2) 0.0031(15) 0.0085(18) 0.0088(18) C74 0.044(2) 0.021(2) 0.0190(18) 0.0009(15) 0.0020(16) -0.0043(18) C75 0.026(2) 0.023(2) 0.0082(15) -0.0001(13) 0.0016(14) 0.0007(16) C76 0.023(2) 0.038(2) 0.0202(18) 0.0070(16) -0.0010(15) 0.0028(17) C77 0.027(2) 0.124(5) 0.028(2) 0.000(3) -0.0001(18) 0.020(3) C78 0.029(2) 0.068(3) 0.039(2) -0.005(2) -0.0043(19) -0.011(2) C79 0.029(2) 0.029(2) 0.031(2) 0.0117(17) -0.0057(17) 0.0009(18) C80 0.043(3) 0.041(3) 0.036(2) 0.004(2) -0.0080(19) -0.008(2) C81 0.034(2) 0.067(3) 0.040(2) 0.009(2) -0.005(2) -0.015(2) C82 0.0184(19) 0.022(2) 0.0147(17) -0.0051(14) -0.0012(14) 0.0014(15) C83 0.025(2) 0.031(2) 0.0123(16) -0.0069(14) 0.0044(15) 0.0060(16) C84 0.0210(19) 0.026(2) 0.0188(17) -0.0055(14) 0.0057(15) 0.0053(15) C85 0.0142(18) 0.035(2) 0.0132(16) -0.0081(15) -0.0008(14) 0.0022(16) C86 0.024(2) 0.034(2) 0.0198(18) -0.0073(16) 0.0015(15) 0.0095(17) C87 0.018(2) 0.040(2) 0.033(2) -0.0040(18) 0.0008(16) -0.0030(17) C88 0.0155(19) 0.051(3) 0.036(2) -0.0004(19) -0.0032(16) 0.0081(19) C89 0.032(2) 0.034(2) 0.027(2) -0.0018(17) -0.0044(17) 0.0121(18) C90 0.022(2) 0.038(2) 0.0157(18) -0.0063(16) 0.0036(15) 0.0054(17) C91 0.031(2) 0.038(2) 0.030(2) 0.0023(17) -0.0031(17) -0.0005(18) C92 0.099(4) 0.040(3) 0.047(3) -0.001(2) 0.025(3) -0.005(3) C93 0.117(5) 0.058(4) 0.116(5) -0.052(3) 0.066(4) -0.036(4) C94 0.0194(19) 0.038(2) 0.037(2) -0.0027(18) -0.0010(16) 0.0051(17) C95 0.078(3) 0.035(3) 0.046(3) 0.000(2) 0.001(2) 0.005(2) C96 0.056(3) 0.058(3) 0.034(2) 0.005(2) 0.002(2) 0.025(2) C97 0.0109(17) 0.023(2) 0.0174(17) -0.0047(14) 0.0033(14) 0.0037(15) C98 0.0189(18) 0.0202(19) 0.0171(17) -0.0019(14) 0.0027(14) 0.0036(15) C99 0.025(2) 0.031(2) 0.0235(19) -0.0039(16) -0.0020(16) 0.0031(17) C100 0.019(2) 0.037(2) 0.037(2) -0.0085(18) -0.0074(18) -0.0037(18) C101 0.025(2) 0.025(2) 0.037(2) -0.0077(17) 0.0030(17) -0.0075(17) C102 0.0211(19) 0.021(2) 0.0228(19) -0.0050(15) 0.0027(15) 0.0009(16) C103 0.027(2) 0.018(2) 0.045(2) 0.0048(17) 0.0031(18) 0.0050(17) C104 0.077(3) 0.036(3) 0.034(2) 0.0082(19) 0.005(2) 0.023(2) C105 0.057(3) 0.025(2) 0.051(3) 0.0012(19) 0.019(2) 0.008(2) C106 0.0215(19) 0.023(2) 0.0280(19) 0.0036(15) -0.0010(15) 0.0009(15) C107 0.052(3) 0.025(2) 0.037(2) -0.0033(18) 0.011(2) -0.006(2) C108 0.042(2) 0.026(2) 0.038(2) 0.0085(17) 0.0096(19) 0.0071(19) N1 0.0326(17) 0.0163(16) 0.0173(15) -0.0011(12) 0.0027(13) 0.0096(14) N2 0.0289(18) 0.0159(16) 0.0155(15) 0.0004(12) 0.0020(13) 0.0081(13) N3 0.0150(15) 0.0267(17) 0.0187(15) -0.0034(12) 0.0003(12) 0.0006(13) N4 0.0157(15) 0.0313(17) 0.0191(15) -0.0093(12) -0.0011(12) 0.0010(13) N5 0.0289(17) 0.0187(16) 0.0109(14) -0.0014(12) -0.0020(12) 0.0093(13) N6 0.0381(18) 0.0175(15) 0.0124(14) 0.0005(11) -0.0014(12) 0.0134(13) N7 0.0141(15) 0.0214(16) 0.0133(14) -0.0037(11) 0.0002(11) 0.0025(12) N8 0.0179(16) 0.0352(18) 0.0157(14) -0.0075(13) -0.0006(12) 0.0016(13) P1 0.0533(7) 0.0244(5) 0.0131(4) 0.0015(4) 0.0045(4) 0.0169(5) P2 0.0198(5) 0.0439(7) 0.0182(5) -0.0088(4) 0.0018(4) 0.0065(4) P3 0.0470(6) 0.0201(5) 0.0119(4) 0.0006(4) -0.0007(4) 0.0144(5) P4 0.0185(5) 0.0524(7) 0.0171(5) -0.0130(4) 0.0019(4) 0.0045(5) _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 As1 P1 2.2558(10) . ? As1 P2 2.2665(10) . ? As2 P3 2.2584(9) . ? As2 P4 2.2723(10) . ? C1 N1 1.370(4) . ? C1 N2 1.385(4) . ? C1 P1 1.770(3) . ? C2 C3 1.339(5) . ? C2 N1 1.389(4) . ? C2 H2 0.9500 . ? C3 N2 1.395(4) . ? C3 H3 0.9500 . ? C4 C5 1.396(5) . ? C4 C9 1.396(5) . ? C4 N1 1.448(4) . ? C5 C6 1.394(5) . ? C5 C13 1.521(5) . ? C6 C7 1.380(5) . ? C6 H6 0.9500 . ? C7 C8 1.371(5) . ? C7 H7 0.9500 . ? C8 C9 1.404(5) . ? C8 H8 0.9500 . ? C9 C10 1.520(5) . ? C10 C11 1.527(5) . ? C10 C12 1.545(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.529(6) . ? C13 C15 1.533(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.401(5) . ? C16 C17 1.407(5) . ? C16 N2 1.437(4) . ? C17 C18 1.400(5) . ? C17 C25 1.522(5) . ? C18 C19 1.389(5) . ? C18 H18 0.9500 . ? C19 C20 1.386(5) . ? C19 H19 0.9500 . ? C20 C21 1.398(5) . ? C20 H20 0.9500 . ? C21 C22 1.526(5) . ? C22 C23 1.528(5) . ? C22 C24 1.531(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.525(5) . ? C25 C27 1.528(6) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N3 1.378(4) . ? C28 N4 1.389(4) . ? C28 P2 1.763(3) . ? C29 C30 1.332(5) . ? C29 N3 1.394(4) . ? C29 H29 0.9500 . ? C30 N4 1.381(4) . ? C30 H30 0.9500 . ? C31 C36 1.405(5) . ? C31 C32 1.407(5) . ? C31 N3 1.453(4) . ? C32 C33 1.386(5) . ? C32 C40 1.534(5) . ? C33 C34 1.387(5) . ? C33 H33 0.9500 . ? C34 C35 1.388(5) . ? C34 H34 0.9500 . ? C35 C36 1.387(5) . ? C35 H35 0.9500 . ? C36 C37 1.526(5) . ? C37 C38 1.519(5) . ? C37 C39 1.528(5) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C42 1.516(6) . ? C40 C41 1.520(5) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.394(5) . ? C43 C48 1.398(5) . ? C43 N4 1.451(4) . ? C44 C45 1.392(5) . ? C44 C52 1.525(5) . ? C45 C46 1.397(5) . ? C45 H45 0.9500 . ? C46 C47 1.374(5) . ? C46 H46 0.9500 . ? C47 C48 1.387(5) . ? C47 H47 0.9500 . ? C48 C49 1.517(5) . ? C49 C50 1.515(5) . ? C49 C51 1.519(6) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.513(6) . ? C52 C54 1.533(6) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N5 1.371(4) . ? C55 N6 1.381(4) . ? C55 P3 1.769(3) . ? C56 C57 1.336(5) . ? C56 N6 1.389(4) . ? C56 H56 0.9500 . ? C57 N5 1.391(4) . ? C57 H57 0.9500 . ? C58 C63 1.401(5) . ? C58 C59 1.406(5) . ? C58 N6 1.437(4) . ? C59 C60 1.402(5) . ? C59 C67 1.514(5) . ? C60 C61 1.381(5) . ? C60 H60 0.9500 . ? C61 C62 1.375(5) . ? C61 H61 0.9500 . ? C62 C63 1.384(5) . ? C62 H62 0.9500 . ? C63 C64 1.527(5) . ? C64 C65 1.525(6) . ? C64 C66 1.542(5) . ? 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 C68 1.520(5) . ? C67 C69 1.535(5) . ? C67 H67 1.0000 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.394(5) . ? C70 C75 1.399(5) . ? C70 N5 1.455(4) . ? C71 C72 1.406(5) . ? C71 C79 1.517(5) . ? C72 C73 1.367(5) . ? C72 H72 0.9500 . ? C73 C74 1.387(5) . ? C73 H73 0.9500 . ? C74 C75 1.394(5) . ? C74 H74 0.9500 . ? C75 C76 1.516(5) . ? C76 C77 1.522(5) . ? C76 C78 1.533(5) . ? 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 C81 1.523(5) . ? C79 C80 1.535(5) . ? C79 H79 1.0000 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 N7 1.377(4) . ? C82 N8 1.385(4) . ? C82 P4 1.776(3) . ? C83 C84 1.341(5) . ? C83 N8 1.389(4) . ? C83 H83 0.9500 . ? C84 N7 1.392(4) . ? C84 H84 0.9500 . ? C85 C86 1.392(5) . ? C85 C90 1.403(5) . ? C85 N8 1.447(4) . ? C86 C87 1.398(5) . ? C86 C94 1.522(5) . ? C87 C88 1.377(5) . ? C87 H87 0.9500 . ? C88 C89 1.380(5) . ? C88 H88 0.9500 . ? C89 C90 1.396(5) . ? C89 H89 0.9500 . ? C90 C91 1.522(5) . ? C91 C92 1.494(5) . ? C91 C93 1.525(6) . ? C91 H91 1.0000 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 C96 1.531(5) . ? C94 C95 1.533(6) . ? C94 H94 1.0000 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 C102 1.400(5) . ? C97 C98 1.401(4) . ? C97 N7 1.447(4) . ? C98 C99 1.403(5) . ? C98 C106 1.522(5) . ? C99 C100 1.391(5) . ? C99 H99 0.9500 . ? C100 C101 1.380(5) . ? C100 H100 0.9500 . ? C101 C102 1.396(5) . ? C101 H101 0.9500 . ? C102 C103 1.512(5) . ? C103 C104 1.511(5) . ? C103 C105 1.532(5) . ? C103 H103 1.0000 . ? C104 H10J 0.9800 . ? C104 H10K 0.9800 . ? C104 H10L 0.9800 . ? C105 H10G 0.9800 . ? C105 H10H 0.9800 . ? C105 H10I 0.9800 . ? C106 C107 1.531(5) . ? C106 C108 1.536(5) . ? C106 H106 1.0000 . ? C107 H10D 0.9800 . ? C107 H10E 0.9800 . ? C107 H10F 0.9800 . ? C108 H10A 0.9800 . ? C108 H10B 0.9800 . ? C108 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 As1 P2 86.53(4) . . ? P3 As2 P4 85.98(4) . . ? N1 C1 N2 104.6(3) . . ? N1 C1 P1 119.9(2) . . ? N2 C1 P1 135.1(3) . . ? C3 C2 N1 108.1(3) . . ? C3 C2 H2 125.9 . . ? N1 C2 H2 125.9 . . ? C2 C3 N2 107.1(3) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? C5 C4 C9 123.0(3) . . ? C5 C4 N1 119.0(3) . . ? C9 C4 N1 117.9(3) . . ? C6 C5 C4 117.0(3) . . ? C6 C5 C13 120.5(3) . . ? C4 C5 C13 122.5(3) . . ? C7 C6 C5 121.4(3) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C8 C7 C6 120.4(3) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 121.0(3) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C4 C9 C8 117.1(3) . . ? C4 C9 C10 123.1(3) . . ? C8 C9 C10 119.8(3) . . ? C9 C10 C11 110.9(3) . . ? C9 C10 C12 111.3(3) . . ? C11 C10 C12 111.0(3) . . ? C9 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 C14 110.7(3) . . ? C5 C13 C15 111.1(3) . . ? C14 C13 C15 110.0(3) . . ? C5 C13 H13 108.3 . . ? C14 C13 H13 108.3 . . ? C15 C13 H13 108.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 122.7(3) . . ? C21 C16 N2 118.8(3) . . ? C17 C16 N2 118.5(3) . . ? C18 C17 C16 117.5(3) . . ? C18 C17 C25 120.4(3) . . ? C16 C17 C25 122.1(3) . . ? C19 C18 C17 120.9(3) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 121.1(3) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C16 117.5(3) . . ? C20 C21 C22 119.4(3) . . ? C16 C21 C22 123.0(3) . . ? C21 C22 C23 110.9(3) . . ? C21 C22 C24 111.2(3) . . ? C23 C22 C24 110.0(3) . . ? C21 C22 H22 108.2 . . ? C23 C22 H22 108.2 . . ? C24 C22 H22 108.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C17 C25 C26 112.0(3) . . ? C17 C25 C27 109.6(3) . . ? C26 C25 C27 110.3(4) . . ? C17 C25 H25 108.3 . . ? C26 C25 H25 108.3 . . ? C27 C25 H25 108.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 N4 103.6(3) . . ? N3 C28 P2 135.8(3) . . ? N4 C28 P2 120.5(2) . . ? C30 C29 N3 108.2(3) . . ? C30 C29 H29 125.9 . . ? N3 C29 H29 125.9 . . ? C29 C30 N4 107.1(3) . . ? C29 C30 H30 126.4 . . ? N4 C30 H30 126.4 . . ? C36 C31 C32 122.7(3) . . ? C36 C31 N3 118.4(3) . . ? C32 C31 N3 118.7(3) . . ? C33 C32 C31 117.1(3) . . ? C33 C32 C40 120.7(3) . . ? C31 C32 C40 122.2(3) . . ? C32 C33 C34 121.6(4) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C33 C34 C35 119.7(4) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 121.4(4) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C31 117.3(3) . . ? C35 C36 C37 121.5(3) . . ? C31 C36 C37 121.2(3) . . ? C38 C37 C36 112.3(3) . . ? C38 C37 C39 110.3(3) . . ? C36 C37 C39 111.3(3) . . ? C38 C37 H37 107.6 . . ? C36 C37 H37 107.6 . . ? C39 C37 H37 107.6 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C40 C41 110.2(3) . . ? C42 C40 C32 112.3(3) . . ? C41 C40 C32 111.6(3) . . ? C42 C40 H40 107.5 . . ? C41 C40 H40 107.5 . . ? C32 C40 H40 107.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 123.3(3) . . ? C44 C43 N4 118.3(3) . . ? C48 C43 N4 118.4(3) . . ? C45 C44 C43 117.1(3) . . ? C45 C44 C52 120.2(3) . . ? C43 C44 C52 122.7(3) . . ? C44 C45 C46 121.1(4) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C47 C46 C45 119.5(4) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C46 C47 C48 122.0(3) . . ? C46 C47 H47 119.0 . . ? C48 C47 H47 119.0 . . ? C47 C48 C43 116.9(3) . . ? C47 C48 C49 120.7(3) . . ? C43 C48 C49 122.4(3) . . ? C50 C49 C48 111.7(3) . . ? C50 C49 C51 110.4(3) . . ? C48 C49 C51 112.6(3) . . ? C50 C49 H49 107.3 . . ? C48 C49 H49 107.3 . . ? C51 C49 H49 107.3 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C44 111.9(3) . . ? C53 C52 C54 112.1(4) . . ? C44 C52 C54 109.8(3) . . ? C53 C52 H52 107.6 . . ? C44 C52 H52 107.6 . . ? C54 C52 H52 107.6 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N5 C55 N6 104.2(3) . . ? N5 C55 P3 135.8(3) . . ? N6 C55 P3 120.0(2) . . ? C57 C56 N6 106.9(3) . . ? C57 C56 H56 126.5 . . ? N6 C56 H56 126.5 . . ? C56 C57 N5 108.1(3) . . ? C56 C57 H57 126.0 . . ? N5 C57 H57 126.0 . . ? C63 C58 C59 122.6(3) . . ? C63 C58 N6 119.1(3) . . ? C59 C58 N6 118.3(3) . . ? C60 C59 C58 117.0(3) . . ? C60 C59 C67 120.1(3) . . ? C58 C59 C67 122.8(3) . . ? C61 C60 C59 121.2(3) . . ? C61 C60 H60 119.4 . . ? C59 C60 H60 119.4 . . ? C62 C61 C60 119.7(3) . . ? C62 C61 H61 120.2 . . ? C60 C61 H61 120.2 . . ? C61 C62 C63 122.3(3) . . ? C61 C62 H62 118.9 . . ? C63 C62 H62 118.9 . . ? C62 C63 C58 117.1(3) . . ? C62 C63 C64 121.8(3) . . ? C58 C63 C64 121.2(3) . . ? C65 C64 C63 111.6(3) . . ? C65 C64 C66 110.5(3) . . ? C63 C64 C66 110.5(3) . . ? C65 C64 H64 108.0 . . ? C63 C64 H64 108.0 . . ? C66 C64 H64 108.0 . . ? 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 . . ? C59 C67 C68 111.6(3) . . ? C59 C67 C69 110.4(3) . . ? C68 C67 C69 111.3(3) . . ? C59 C67 H67 107.8 . . ? C68 C67 H67 107.8 . . ? C69 C67 H67 107.8 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C71 C70 C75 124.1(3) . . ? C71 C70 N5 117.3(3) . . ? C75 C70 N5 118.5(3) . . ? C70 C71 C72 116.4(3) . . ? C70 C71 C79 123.2(3) . . ? C72 C71 C79 120.4(3) . . ? C73 C72 C71 121.4(3) . . ? C73 C72 H72 119.3 . . ? C71 C72 H72 119.3 . . ? C72 C73 C74 120.1(3) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C73 C74 C75 121.7(3) . . ? C73 C74 H74 119.1 . . ? C75 C74 H74 119.1 . . ? C74 C75 C70 116.1(3) . . ? C74 C75 C76 121.6(3) . . ? C70 C75 C76 122.2(3) . . ? C75 C76 C77 110.1(3) . . ? C75 C76 C78 113.2(3) . . ? C77 C76 C78 110.8(3) . . ? C75 C76 H76 107.5 . . ? C77 C76 H76 107.5 . . ? C78 C76 H76 107.5 . . ? 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 . . ? C71 C79 C81 111.0(3) . . ? C71 C79 C80 112.3(3) . . ? C81 C79 C80 110.9(3) . . ? C71 C79 H79 107.5 . . ? C81 C79 H79 107.5 . . ? C80 C79 H79 107.5 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N7 C82 N8 104.6(3) . . ? N7 C82 P4 135.0(2) . . ? N8 C82 P4 120.3(2) . . ? C84 C83 N8 107.2(3) . . ? C84 C83 H83 126.4 . . ? N8 C83 H83 126.4 . . ? C83 C84 N7 108.1(3) . . ? C83 C84 H84 125.9 . . ? N7 C84 H84 125.9 . . ? C86 C85 C90 123.7(3) . . ? C86 C85 N8 118.5(3) . . ? C90 C85 N8 117.8(3) . . ? C85 C86 C87 116.9(3) . . ? C85 C86 C94 123.2(3) . . ? C87 C86 C94 119.8(3) . . ? C88 C87 C86 120.7(4) . . ? C88 C87 H87 119.6 . . ? C86 C87 H87 119.6 . . ? C87 C88 C89 121.3(3) . . ? C87 C88 H88 119.4 . . ? C89 C88 H88 119.4 . . ? C88 C89 C90 120.5(4) . . ? C88 C89 H89 119.7 . . ? C90 C89 H89 119.7 . . ? C89 C90 C85 116.8(3) . . ? C89 C90 C91 120.9(3) . . ? C85 C90 C91 122.3(3) . . ? C92 C91 C90 112.6(3) . . ? C92 C91 C93 109.6(4) . . ? C90 C91 C93 112.7(3) . . ? C92 C91 H91 107.2 . . ? C90 C91 H91 107.2 . . ? C93 C91 H91 107.2 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C91 C93 H93A 109.5 . . ? C91 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C91 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C86 C94 C96 109.4(3) . . ? C86 C94 C95 112.4(3) . . ? C96 C94 C95 111.3(3) . . ? C86 C94 H94 107.9 . . ? C96 C94 H94 107.9 . . ? C95 C94 H94 107.9 . . ? C94 C95 H95A 109.5 . . ? C94 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C94 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C94 C96 H96A 109.5 . . ? C94 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C94 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C102 C97 C98 123.6(3) . . ? C102 C97 N7 118.7(3) . . ? C98 C97 N7 117.6(3) . . ? C97 C98 C99 116.8(3) . . ? C97 C98 C106 122.3(3) . . ? C99 C98 C106 121.0(3) . . ? C100 C99 C98 121.0(3) . . ? C100 C99 H99 119.5 . . ? C98 C99 H99 119.5 . . ? C101 C100 C99 120.1(3) . . ? C101 C100 H100 119.9 . . ? C99 C100 H100 119.9 . . ? C100 C101 C102 121.5(3) . . ? C100 C101 H101 119.2 . . ? C102 C101 H101 119.2 . . ? C101 C102 C97 116.8(3) . . ? C101 C102 C103 120.9(3) . . ? C97 C102 C103 122.3(3) . . ? C104 C103 C102 112.7(3) . . ? C104 C103 C105 110.5(3) . . ? C102 C103 C105 111.9(3) . . ? C104 C103 H103 107.1 . . ? C102 C103 H103 107.1 . . ? C105 C103 H103 107.1 . . ? C103 C104 H10J 109.5 . . ? C103 C104 H10K 109.5 . . ? H10J C104 H10K 109.5 . . ? C103 C104 H10L 109.5 . . ? H10J C104 H10L 109.5 . . ? H10K C104 H10L 109.5 . . ? C103 C105 H10G 109.5 . . ? C103 C105 H10H 109.5 . . ? H10G C105 H10H 109.5 . . ? C103 C105 H10I 109.5 . . ? H10G C105 H10I 109.5 . . ? H10H C105 H10I 109.5 . . ? C98 C106 C107 111.9(3) . . ? C98 C106 C108 111.2(3) . . ? C107 C106 C108 111.2(3) . . ? C98 C106 H106 107.4 . . ? C107 C106 H106 107.4 . . ? C108 C106 H106 107.4 . . ? C106 C107 H10D 109.5 . . ? C106 C107 H10E 109.5 . . ? H10D C107 H10E 109.5 . . ? C106 C107 H10F 109.5 . . ? H10D C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? C106 C108 H10A 109.5 . . ? C106 C108 H10B 109.5 . . ? H10A C108 H10B 109.5 . . ? C106 C108 H10C 109.5 . . ? H10A C108 H10C 109.5 . . ? H10B C108 H10C 109.5 . . ? C1 N1 C2 110.1(3) . . ? C1 N1 C4 124.9(3) . . ? C2 N1 C4 124.9(3) . . ? C1 N2 C3 110.0(3) . . ? C1 N2 C16 127.3(3) . . ? C3 N2 C16 122.6(3) . . ? C28 N3 C29 110.0(3) . . ? C28 N3 C31 128.3(3) . . ? C29 N3 C31 121.3(3) . . ? C30 N4 C28 111.0(3) . . ? C30 N4 C43 124.6(3) . . ? C28 N4 C43 124.3(3) . . ? C55 N5 C57 110.2(3) . . ? C55 N5 C70 128.1(3) . . ? C57 N5 C70 121.7(3) . . ? C55 N6 C56 110.7(3) . . ? C55 N6 C58 124.6(3) . . ? C56 N6 C58 124.6(3) . . ? C82 N7 C84 109.8(3) . . ? C82 N7 C97 128.5(3) . . ? C84 N7 C97 121.2(3) . . ? C82 N8 C83 110.3(3) . . ? C82 N8 C85 124.8(3) . . ? C83 N8 C85 124.8(3) . . ? C1 P1 As1 107.31(12) . . ? C28 P2 As1 105.31(12) . . ? C55 P3 As2 106.90(11) . . ? C82 P4 As2 106.10(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.6(4) . . . . ? C9 C4 C5 C6 -1.7(5) . . . . ? N1 C4 C5 C6 177.7(3) . . . . ? C9 C4 C5 C13 176.8(3) . . . . ? N1 C4 C5 C13 -3.7(5) . . . . ? C4 C5 C6 C7 -0.3(5) . . . . ? C13 C5 C6 C7 -178.9(3) . . . . ? C5 C6 C7 C8 1.3(5) . . . . ? C6 C7 C8 C9 -0.3(5) . . . . ? C5 C4 C9 C8 2.7(5) . . . . ? N1 C4 C9 C8 -176.8(3) . . . . ? C5 C4 C9 C10 -177.5(3) . . . . ? N1 C4 C9 C10 3.0(5) . . . . ? C7 C8 C9 C4 -1.6(5) . . . . ? C7 C8 C9 C10 178.6(3) . . . . ? C4 C9 C10 C11 -112.2(4) . . . . ? C8 C9 C10 C11 67.7(4) . . . . ? C4 C9 C10 C12 123.7(4) . . . . ? C8 C9 C10 C12 -56.5(4) . . . . ? C6 C5 C13 C14 64.9(5) . . . . ? C4 C5 C13 C14 -113.7(4) . . . . ? C6 C5 C13 C15 -57.7(4) . . . . ? C4 C5 C13 C15 123.8(4) . . . . ? C21 C16 C17 C18 -0.8(5) . . . . ? N2 C16 C17 C18 178.6(3) . . . . ? C21 C16 C17 C25 179.1(3) . . . . ? N2 C16 C17 C25 -1.4(5) . . . . ? C16 C17 C18 C19 1.7(5) . . . . ? C25 C17 C18 C19 -178.2(3) . . . . ? C17 C18 C19 C20 -1.9(5) . . . . ? C18 C19 C20 C21 1.1(5) . . . . ? C19 C20 C21 C16 -0.1(5) . . . . ? C19 C20 C21 C22 -179.9(3) . . . . ? C17 C16 C21 C20 0.0(5) . . . . ? N2 C16 C21 C20 -179.4(3) . . . . ? C17 C16 C21 C22 179.7(3) . . . . ? N2 C16 C21 C22 0.3(5) . . . . ? C20 C21 C22 C23 -63.7(4) . . . . ? C16 C21 C22 C23 116.6(4) . . . . ? C20 C21 C22 C24 59.0(4) . . . . ? C16 C21 C22 C24 -120.7(3) . . . . ? C18 C17 C25 C26 47.8(5) . . . . ? C16 C17 C25 C26 -132.2(4) . . . . ? C18 C17 C25 C27 -75.0(5) . . . . ? C16 C17 C25 C27 105.0(4) . . . . ? N3 C29 C30 N4 0.9(4) . . . . ? C36 C31 C32 C33 -3.1(5) . . . . ? N3 C31 C32 C33 172.1(3) . . . . ? C36 C31 C32 C40 175.7(3) . . . . ? N3 C31 C32 C40 -9.1(5) . . . . ? C31 C32 C33 C34 -0.5(5) . . . . ? C40 C32 C33 C34 -179.3(3) . . . . ? C32 C33 C34 C35 2.6(6) . . . . ? C33 C34 C35 C36 -1.2(6) . . . . ? C34 C35 C36 C31 -2.1(5) . . . . ? C34 C35 C36 C37 177.8(3) . . . . ? C32 C31 C36 C35 4.4(5) . . . . ? N3 C31 C36 C35 -170.9(3) . . . . ? C32 C31 C36 C37 -175.5(3) . . . . ? N3 C31 C36 C37 9.2(5) . . . . ? C35 C36 C37 C38 73.9(4) . . . . ? C31 C36 C37 C38 -106.2(4) . . . . ? C35 C36 C37 C39 -50.4(4) . . . . ? C31 C36 C37 C39 129.5(3) . . . . ? C33 C32 C40 C42 50.1(5) . . . . ? C31 C32 C40 C42 -128.7(4) . . . . ? C33 C32 C40 C41 -74.3(4) . . . . ? C31 C32 C40 C41 107.0(4) . . . . ? C48 C43 C44 C45 -2.6(5) . . . . ? N4 C43 C44 C45 176.2(3) . . . . ? C48 C43 C44 C52 174.3(3) . . . . ? N4 C43 C44 C52 -6.8(5) . . . . ? C43 C44 C45 C46 0.3(5) . . . . ? C52 C44 C45 C46 -176.8(3) . . . . ? C44 C45 C46 C47 2.0(6) . . . . ? C45 C46 C47 C48 -2.1(6) . . . . ? C46 C47 C48 C43 -0.1(6) . . . . ? C46 C47 C48 C49 178.2(4) . . . . ? C44 C43 C48 C47 2.6(5) . . . . ? N4 C43 C48 C47 -176.2(3) . . . . ? C44 C43 C48 C49 -175.7(3) . . . . ? N4 C43 C48 C49 5.5(5) . . . . ? C47 C48 C49 C50 78.7(5) . . . . ? C43 C48 C49 C50 -103.1(4) . . . . ? C47 C48 C49 C51 -46.1(5) . . . . ? C43 C48 C49 C51 132.1(4) . . . . ? C45 C44 C52 C53 -62.7(5) . . . . ? C43 C44 C52 C53 120.4(4) . . . . ? C45 C44 C52 C54 62.5(5) . . . . ? C43 C44 C52 C54 -114.4(4) . . . . ? N6 C56 C57 N5 -0.1(4) . . . . ? C63 C58 C59 C60 -2.1(5) . . . . ? N6 C58 C59 C60 177.5(3) . . . . ? C63 C58 C59 C67 177.5(3) . . . . ? N6 C58 C59 C67 -2.9(5) . . . . ? C58 C59 C60 C61 0.2(5) . . . . ? C67 C59 C60 C61 -179.4(3) . . . . ? C59 C60 C61 C62 1.5(5) . . . . ? C60 C61 C62 C63 -1.5(5) . . . . ? C61 C62 C63 C58 -0.3(5) . . . . ? C61 C62 C63 C64 179.5(3) . . . . ? C59 C58 C63 C62 2.2(5) . . . . ? N6 C58 C63 C62 -177.5(3) . . . . ? C59 C58 C63 C64 -177.7(3) . . . . ? N6 C58 C63 C64 2.7(4) . . . . ? C62 C63 C64 C65 -51.4(5) . . . . ? C58 C63 C64 C65 128.4(4) . . . . ? C62 C63 C64 C66 71.9(4) . . . . ? C58 C63 C64 C66 -108.2(4) . . . . ? C60 C59 C67 C68 57.4(4) . . . . ? C58 C59 C67 C68 -122.2(4) . . . . ? C60 C59 C67 C69 -67.1(4) . . . . ? C58 C59 C67 C69 113.3(4) . . . . ? C75 C70 C71 C72 -2.9(5) . . . . ? N5 C70 C71 C72 174.9(3) . . . . ? C75 C70 C71 C79 174.5(3) . . . . ? N5 C70 C71 C79 -7.7(5) . . . . ? C70 C71 C72 C73 1.7(5) . . . . ? C79 C71 C72 C73 -175.8(3) . . . . ? C71 C72 C73 C74 0.8(5) . . . . ? C72 C73 C74 C75 -2.3(5) . . . . ? C73 C74 C75 C70 1.1(5) . . . . ? C73 C74 C75 C76 -177.4(3) . . . . ? C71 C70 C75 C74 1.5(5) . . . . ? N5 C70 C75 C74 -176.3(3) . . . . ? C71 C70 C75 C76 -179.9(3) . . . . ? N5 C70 C75 C76 2.3(4) . . . . ? C74 C75 C76 C77 84.6(4) . . . . ? C70 C75 C76 C77 -93.8(4) . . . . ? C74 C75 C76 C78 -40.0(4) . . . . ? C70 C75 C76 C78 141.5(3) . . . . ? C70 C71 C79 C81 -118.6(4) . . . . ? C72 C71 C79 C81 58.7(4) . . . . ? C70 C71 C79 C80 116.7(4) . . . . ? C72 C71 C79 C80 -65.9(4) . . . . ? N8 C83 C84 N7 -0.3(4) . . . . ? C90 C85 C86 C87 3.0(5) . . . . ? N8 C85 C86 C87 -176.0(3) . . . . ? C90 C85 C86 C94 -174.1(3) . . . . ? N8 C85 C86 C94 7.0(5) . . . . ? C85 C86 C87 C88 -0.8(5) . . . . ? C94 C86 C87 C88 176.3(3) . . . . ? C86 C87 C88 C89 -0.9(6) . . . . ? C87 C88 C89 C90 0.6(6) . . . . ? C88 C89 C90 C85 1.4(5) . . . . ? C88 C89 C90 C91 -177.7(3) . . . . ? C86 C85 C90 C89 -3.2(5) . . . . ? N8 C85 C90 C89 175.7(3) . . . . ? C86 C85 C90 C91 175.8(3) . . . . ? N8 C85 C90 C91 -5.3(5) . . . . ? C89 C90 C91 C92 -82.8(5) . . . . ? C85 C90 C91 C92 98.2(4) . . . . ? C89 C90 C91 C93 41.8(5) . . . . ? C85 C90 C91 C93 -137.2(4) . . . . ? C85 C86 C94 C96 109.0(4) . . . . ? C87 C86 C94 C96 -68.0(4) . . . . ? C85 C86 C94 C95 -126.9(4) . . . . ? C87 C86 C94 C95 56.2(5) . . . . ? C102 C97 C98 C99 -4.1(5) . . . . ? N7 C97 C98 C99 171.6(3) . . . . ? C102 C97 C98 C106 175.2(3) . . . . ? N7 C97 C98 C106 -9.1(4) . . . . ? C97 C98 C99 C100 0.6(5) . . . . ? C106 C98 C99 C100 -178.7(3) . . . . ? C98 C99 C100 C101 2.4(5) . . . . ? C99 C100 C101 C102 -2.0(6) . . . . ? C100 C101 C102 C97 -1.2(5) . . . . ? C100 C101 C102 C103 178.2(3) . . . . ? C98 C97 C102 C101 4.4(5) . . . . ? N7 C97 C102 C101 -171.3(3) . . . . ? C98 C97 C102 C103 -175.0(3) . . . . ? N7 C97 C102 C103 9.3(5) . . . . ? C101 C102 C103 C104 75.3(4) . . . . ? C97 C102 C103 C104 -105.3(4) . . . . ? C101 C102 C103 C105 -49.9(4) . . . . ? C97 C102 C103 C105 129.5(4) . . . . ? C97 C98 C106 C107 109.4(4) . . . . ? C99 C98 C106 C107 -71.4(4) . . . . ? C97 C98 C106 C108 -125.6(3) . . . . ? C99 C98 C106 C108 53.6(4) . . . . ? N2 C1 N1 C2 0.8(4) . . . . ? P1 C1 N1 C2 -173.2(3) . . . . ? N2 C1 N1 C4 177.4(3) . . . . ? P1 C1 N1 C4 3.5(5) . . . . ? C3 C2 N1 C1 -0.9(4) . . . . ? C3 C2 N1 C4 -177.6(3) . . . . ? C5 C4 N1 C1 92.2(4) . . . . ? C9 C4 N1 C1 -88.3(4) . . . . ? C5 C4 N1 C2 -91.6(4) . . . . ? C9 C4 N1 C2 87.8(4) . . . . ? N1 C1 N2 C3 -0.4(4) . . . . ? P1 C1 N2 C3 172.2(3) . . . . ? N1 C1 N2 C16 -177.2(3) . . . . ? P1 C1 N2 C16 -4.6(6) . . . . ? C2 C3 N2 C1 -0.2(4) . . . . ? C2 C3 N2 C16 176.8(3) . . . . ? C21 C16 N2 C1 -96.4(4) . . . . ? C17 C16 N2 C1 84.2(4) . . . . ? C21 C16 N2 C3 87.2(4) . . . . ? C17 C16 N2 C3 -92.3(4) . . . . ? N4 C28 N3 C29 0.8(4) . . . . ? P2 C28 N3 C29 177.6(3) . . . . ? N4 C28 N3 C31 -171.6(3) . . . . ? P2 C28 N3 C31 5.1(6) . . . . ? C30 C29 N3 C28 -1.1(4) . . . . ? C30 C29 N3 C31 172.0(3) . . . . ? C36 C31 N3 C28 -102.5(4) . . . . ? C32 C31 N3 C28 82.1(4) . . . . ? C36 C31 N3 C29 85.8(4) . . . . ? C32 C31 N3 C29 -89.6(4) . . . . ? C29 C30 N4 C28 -0.4(4) . . . . ? C29 C30 N4 C43 -176.7(3) . . . . ? N3 C28 N4 C30 -0.2(4) . . . . ? P2 C28 N4 C30 -177.6(3) . . . . ? N3 C28 N4 C43 176.1(3) . . . . ? P2 C28 N4 C43 -1.3(5) . . . . ? C44 C43 N4 C30 -85.5(4) . . . . ? C48 C43 N4 C30 93.3(4) . . . . ? C44 C43 N4 C28 98.7(4) . . . . ? C48 C43 N4 C28 -82.5(4) . . . . ? N6 C55 N5 C57 -0.6(4) . . . . ? P3 C55 N5 C57 -178.0(3) . . . . ? N6 C55 N5 C70 179.1(3) . . . . ? P3 C55 N5 C70 1.7(6) . . . . ? C56 C57 N5 C55 0.4(4) . . . . ? C56 C57 N5 C70 -179.3(3) . . . . ? C71 C70 N5 C55 104.7(4) . . . . ? C75 C70 N5 C55 -77.4(4) . . . . ? C71 C70 N5 C57 -75.6(4) . . . . ? C75 C70 N5 C57 102.3(4) . . . . ? N5 C55 N6 C56 0.5(4) . . . . ? P3 C55 N6 C56 178.4(3) . . . . ? N5 C55 N6 C58 177.3(3) . . . . ? P3 C55 N6 C58 -4.8(5) . . . . ? C57 C56 N6 C55 -0.3(4) . . . . ? C57 C56 N6 C58 -177.1(3) . . . . ? C63 C58 N6 C55 -90.4(4) . . . . ? C59 C58 N6 C55 89.9(4) . . . . ? C63 C58 N6 C56 85.9(4) . . . . ? C59 C58 N6 C56 -93.7(4) . . . . ? N8 C82 N7 C84 -0.6(4) . . . . ? P4 C82 N7 C84 -176.5(3) . . . . ? N8 C82 N7 C97 171.4(3) . . . . ? P4 C82 N7 C97 -4.6(6) . . . . ? C83 C84 N7 C82 0.6(4) . . . . ? C83 C84 N7 C97 -172.1(3) . . . . ? C102 C97 N7 C82 -82.2(4) . . . . ? C98 C97 N7 C82 101.8(4) . . . . ? C102 C97 N7 C84 88.9(4) . . . . ? C98 C97 N7 C84 -87.1(4) . . . . ? N7 C82 N8 C83 0.4(4) . . . . ? P4 C82 N8 C83 177.1(2) . . . . ? N7 C82 N8 C85 -176.2(3) . . . . ? P4 C82 N8 C85 0.5(5) . . . . ? C84 C83 N8 C82 0.0(4) . . . . ? C84 C83 N8 C85 176.5(3) . . . . ? C86 C85 N8 C82 -95.3(4) . . . . ? C90 C85 N8 C82 85.7(4) . . . . ? C86 C85 N8 C83 88.6(4) . . . . ? C90 C85 N8 C83 -90.4(4) . . . . ? N1 C1 P1 As1 -171.3(3) . . . . ? N2 C1 P1 As1 17.0(4) . . . . ? P2 As1 P1 C1 -147.11(13) . . . . ? N3 C28 P2 As1 15.6(4) . . . . ? N4 C28 P2 As1 -168.0(2) . . . . ? P1 As1 P2 C28 -143.91(12) . . . . ? N5 C55 P3 As2 -16.9(4) . . . . ? N6 C55 P3 As2 166.0(2) . . . . ? P4 As2 P3 C55 149.99(13) . . . . ? N7 C82 P4 As2 -13.3(4) . . . . ? N8 C82 P4 As2 171.2(2) . . . . ? P3 As2 P4 C82 146.65(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.546 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 937995' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_finalpppcc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H78 N4 O4 P6' _chemical_formula_weight 1105.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 23.6782(11) _cell_length_b 18.3268(9) _cell_length_c 29.7342(14) _cell_angle_alpha 90.00 _cell_angle_beta 103.9810(10) _cell_angle_gamma 90.00 _cell_volume 12520.8(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9168 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 68.04 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu 1.957 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6359 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_process_details 'SADABS-2012/1 - Bruker AXS area detector scaling and absorption correction' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 157386 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 63.02 _reflns_number_total 20182 _reflns_number_gt 15958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0334P)^2^+21.0990P] 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 20182 _refine_ls_number_parameters 1369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 C1 C 0.26993(10) 0.67369(14) 0.69563(9) 0.0272(6) Uani 1 1 d . . . C2 C 0.19442(11) 0.63722(14) 0.63824(9) 0.0306(6) Uani 1 1 d . . . H2 H 0.1565 0.6222 0.6223 0.037 Uiso 1 1 calc R . . C3 C 0.24000(11) 0.64743(15) 0.61963(10) 0.0321(6) Uani 1 1 d . . . H3 H 0.2404 0.6411 0.5880 0.039 Uiso 1 1 calc R . . C4 C 0.17849(10) 0.64327(14) 0.71863(9) 0.0274(6) Uani 1 1 d . . . C5 C 0.13854(11) 0.69702(14) 0.72244(9) 0.0293(6) Uani 1 1 d . . . C6 C 0.10594(11) 0.68581(15) 0.75515(10) 0.0342(6) Uani 1 1 d . . . H6 H 0.0786 0.7218 0.7590 0.041 Uiso 1 1 calc R . . C7 C 0.11257(12) 0.62380(17) 0.78184(11) 0.0417(7) Uani 1 1 d . . . H7 H 0.0897 0.6172 0.8038 0.050 Uiso 1 1 calc R . . C8 C 0.15194(13) 0.57154(17) 0.77700(11) 0.0465(8) Uani 1 1 d . . . H8 H 0.1560 0.5289 0.7957 0.056 Uiso 1 1 calc R . . C9 C 0.18623(12) 0.57946(15) 0.74518(11) 0.0389(7) Uani 1 1 d . . . C10 C 0.22927(14) 0.52015(17) 0.74016(14) 0.0561(9) Uani 1 1 d . . . H10 H 0.2505 0.5373 0.7169 0.067 Uiso 1 1 calc R . . C11 C 0.19786(16) 0.44914(18) 0.72188(13) 0.0604(10) Uani 1 1 d . . . H11A H 0.1781 0.4298 0.7447 0.091 Uiso 1 1 calc R . . H11B H 0.2263 0.4133 0.7165 0.091 Uiso 1 1 calc R . . H11C H 0.1692 0.4588 0.6927 0.091 Uiso 1 1 calc R . . C12 C 0.27406(16) 0.5080(2) 0.78572(17) 0.0910(16) Uani 1 1 d . . . H12A H 0.2909 0.5550 0.7978 0.137 Uiso 1 1 calc R . . H12B H 0.3049 0.4758 0.7805 0.137 Uiso 1 1 calc R . . H12C H 0.2552 0.4854 0.8082 0.137 Uiso 1 1 calc R . . C13 C 0.12887(11) 0.76483(15) 0.69254(10) 0.0342(7) Uani 1 1 d . . . H13 H 0.1583 0.7652 0.6735 0.041 Uiso 1 1 calc R . . C14 C 0.06827(12) 0.76357(16) 0.65959(10) 0.0397(7) Uani 1 1 d . . . H14A H 0.0642 0.7198 0.6401 0.060 Uiso 1 1 calc R . . H14B H 0.0631 0.8071 0.6399 0.060 Uiso 1 1 calc R . . H14C H 0.0387 0.7630 0.6776 0.060 Uiso 1 1 calc R . . C15 C 0.13712(14) 0.83340(16) 0.72206(12) 0.0529(9) Uani 1 1 d . . . H15A H 0.1078 0.8348 0.7403 0.079 Uiso 1 1 calc R . . H15B H 0.1328 0.8764 0.7019 0.079 Uiso 1 1 calc R . . H15C H 0.1761 0.8332 0.7430 0.079 Uiso 1 1 calc R . . C16 C 0.34458(11) 0.67827(16) 0.64840(9) 0.0313(6) Uani 1 1 d . . . C17 C 0.38029(11) 0.61580(17) 0.65374(9) 0.0362(7) Uani 1 1 d . . . C18 C 0.43418(13) 0.6248(2) 0.64397(10) 0.0456(8) Uani 1 1 d . . . H18 H 0.4595 0.5841 0.6461 0.055 Uiso 1 1 calc R . . C19 C 0.45152(12) 0.6911(2) 0.63128(10) 0.0485(9) Uani 1 1 d . . . H19 H 0.4889 0.6956 0.6251 0.058 Uiso 1 1 calc R . . C20 C 0.41630(13) 0.7518(2) 0.62720(10) 0.0472(8) Uani 1 1 d . . . H20 H 0.4298 0.7974 0.6188 0.057 Uiso 1 1 calc R . . C21 C 0.36040(12) 0.74625(17) 0.63544(10) 0.0385(7) Uani 1 1 d . . . C22 C 0.32091(14) 0.81281(17) 0.62944(12) 0.0486(8) Uani 1 1 d . . . H22 H 0.2833 0.7977 0.6363 0.058 Uiso 1 1 calc R . . C23 C 0.3477(2) 0.8726(2) 0.66404(13) 0.0790(13) Uani 1 1 d . . . H23A H 0.3851 0.8877 0.6585 0.118 Uiso 1 1 calc R . . H23B H 0.3537 0.8537 0.6957 0.118 Uiso 1 1 calc R . . H23C H 0.3214 0.9146 0.6601 0.118 Uiso 1 1 calc R . . C24 C 0.30742(15) 0.8424(2) 0.57992(12) 0.0573(9) Uani 1 1 d . . . H24A H 0.3435 0.8587 0.5725 0.086 Uiso 1 1 calc R . . H24B H 0.2804 0.8835 0.5772 0.086 Uiso 1 1 calc R . . H24C H 0.2897 0.8038 0.5583 0.086 Uiso 1 1 calc R . . C25 C 0.41197(16) 0.4991(2) 0.69791(13) 0.0637(10) Uani 1 1 d . . . H25A H 0.4375 0.4840 0.6781 0.095 Uiso 1 1 calc R . . H25B H 0.3970 0.4557 0.7105 0.095 Uiso 1 1 calc R . . H25C H 0.4340 0.5291 0.7235 0.095 Uiso 1 1 calc R . . C26 C 0.36134(13) 0.54316(17) 0.66953(11) 0.0457(8) Uani 1 1 d . . . H26 H 0.3347 0.5539 0.6901 0.055 Uiso 1 1 calc R . . C27 C 0.32755(17) 0.4967(2) 0.62981(15) 0.0768(13) Uani 1 1 d . . . H27A H 0.2925 0.5230 0.6135 0.115 Uiso 1 1 calc R . . H27B H 0.3163 0.4507 0.6420 0.115 Uiso 1 1 calc R . . H27C H 0.3520 0.4865 0.6082 0.115 Uiso 1 1 calc R . . C28 C 0.48312(10) 0.76379(13) 0.84481(8) 0.0220(5) Uani 1 1 d . . . C29 C 0.56309(10) 0.72542(14) 0.89639(8) 0.0248(6) Uani 1 1 d . . . H29 H 0.5915 0.6939 0.9146 0.030 Uiso 1 1 calc R . . C30 C 0.56422(10) 0.79847(14) 0.89694(8) 0.0253(6) Uani 1 1 d . . . H30 H 0.5933 0.8285 0.9157 0.030 Uiso 1 1 calc R . . C31 C 0.49933(10) 0.89707(14) 0.85322(9) 0.0294(6) Uani 1 1 d . . . C32 C 0.46431(11) 0.93237(15) 0.87743(10) 0.0367(7) Uani 1 1 d . . . C33 C 0.44925(12) 1.00548(17) 0.86370(12) 0.0500(9) Uani 1 1 d . . . H33 H 0.4263 1.0333 0.8797 0.060 Uiso 1 1 calc R . . C34 C 0.46754(14) 1.03634(17) 0.82757(13) 0.0523(9) Uani 1 1 d . . . H34 H 0.4554 1.0845 0.8181 0.063 Uiso 1 1 calc R . . C35 C 0.50219(14) 1.00019(17) 0.80520(13) 0.0501(8) Uani 1 1 d . . . H35 H 0.5147 1.0235 0.7808 0.060 Uiso 1 1 calc R . . C36 C 0.51974(12) 0.92918(15) 0.81756(11) 0.0399(7) Uani 1 1 d . . . C37 C 0.44561(13) 0.89786(19) 0.91721(11) 0.0481(8) Uani 1 1 d . . . H37 H 0.4607 0.8467 0.9207 0.058 Uiso 1 1 calc R . . C38 C 0.37932(14) 0.8949(3) 0.90993(14) 0.0744(13) Uani 1 1 d . . . H38A H 0.3638 0.9447 0.9082 0.112 Uiso 1 1 calc R . . H38B H 0.3696 0.8692 0.9359 0.112 Uiso 1 1 calc R . . H38C H 0.3622 0.8691 0.8810 0.112 Uiso 1 1 calc R . . C39 C 0.47264(15) 0.9393(2) 0.96177(12) 0.0613(10) Uani 1 1 d . . . H39A H 0.5151 0.9395 0.9668 0.092 Uiso 1 1 calc R . . H39B H 0.4620 0.9153 0.9880 0.092 Uiso 1 1 calc R . . H39C H 0.4582 0.9896 0.9592 0.092 Uiso 1 1 calc R . . C40 C 0.56068(15) 0.89152(18) 0.79348(12) 0.0533(9) Uani 1 1 d . . . H40 H 0.5696 0.8424 0.8081 0.064 Uiso 1 1 calc R . . C41 C 0.5331(2) 0.8795(3) 0.74160(13) 0.0809(13) Uani 1 1 d . . . H41A H 0.4981 0.8493 0.7380 0.121 Uiso 1 1 calc R . . H41B H 0.5611 0.8548 0.7273 0.121 Uiso 1 1 calc R . . H41C H 0.5225 0.9268 0.7265 0.121 Uiso 1 1 calc R . . C42 C 0.61827(16) 0.9336(2) 0.80130(15) 0.0759(12) Uani 1 1 d . . . H42A H 0.6110 0.9823 0.7875 0.114 Uiso 1 1 calc R . . H42B H 0.6452 0.9072 0.7868 0.114 Uiso 1 1 calc R . . H42C H 0.6355 0.9382 0.8346 0.114 Uiso 1 1 calc R . . C43 C 0.49973(10) 0.62894(13) 0.85085(8) 0.0225(5) Uani 1 1 d . . . C44 C 0.52616(10) 0.60009(13) 0.81767(8) 0.0224(5) Uani 1 1 d . . . C45 C 0.51509(11) 0.52703(14) 0.80597(9) 0.0276(6) Uani 1 1 d . . . H45 H 0.5326 0.5051 0.7837 0.033 Uiso 1 1 calc R . . C46 C 0.47918(12) 0.48630(15) 0.82620(10) 0.0348(7) Uani 1 1 d . . . H46 H 0.4718 0.4367 0.8176 0.042 Uiso 1 1 calc R . . C47 C 0.45365(12) 0.51674(15) 0.85900(10) 0.0370(7) Uani 1 1 d . . . H47 H 0.4287 0.4878 0.8724 0.044 Uiso 1 1 calc R . . C48 C 0.46390(11) 0.58892(14) 0.87262(9) 0.0307(6) Uani 1 1 d . . . C49 C 0.43822(13) 0.62074(17) 0.91042(11) 0.0426(7) Uani 1 1 d . . . H49 H 0.4496 0.6734 0.9141 0.051 Uiso 1 1 calc R . . C50 C 0.37168(15) 0.6167(2) 0.89743(13) 0.0649(11) Uani 1 1 d . . . H50A H 0.3566 0.6413 0.8677 0.097 Uiso 1 1 calc R . . H50B H 0.3564 0.6408 0.9215 0.097 Uiso 1 1 calc R . . H50C H 0.3594 0.5655 0.8948 0.097 Uiso 1 1 calc R . . C51 C 0.46355(16) 0.5826(2) 0.95651(11) 0.0547(9) Uani 1 1 d . . . H51A H 0.4546 0.5303 0.9534 0.082 Uiso 1 1 calc R . . H51B H 0.4464 0.6034 0.9805 0.082 Uiso 1 1 calc R . . H51C H 0.5058 0.5894 0.9652 0.082 Uiso 1 1 calc R . . C52 C 0.56632(10) 0.64457(14) 0.79553(8) 0.0251(6) Uani 1 1 d . . . H52 H 0.5682 0.6954 0.8081 0.030 Uiso 1 1 calc R . . C53 C 0.62739(11) 0.61303(18) 0.80748(11) 0.0424(8) Uani 1 1 d . . . H53A H 0.6412 0.6088 0.8412 0.064 Uiso 1 1 calc R . . H53B H 0.6535 0.6453 0.7956 0.064 Uiso 1 1 calc R . . H53C H 0.6269 0.5646 0.7934 0.064 Uiso 1 1 calc R . . C54 C 0.54332(12) 0.64831(18) 0.74306(10) 0.0434(8) Uani 1 1 d . . . H54A H 0.5432 0.5993 0.7299 0.065 Uiso 1 1 calc R . . H54B H 0.5684 0.6804 0.7299 0.065 Uiso 1 1 calc R . . H54C H 0.5036 0.6677 0.7356 0.065 Uiso 1 1 calc R . . C55 C 0.06785(10) 0.73556(14) -0.05371(8) 0.0253(6) Uani 1 1 d . . . C56 C 0.00583(11) 0.75101(15) -0.12336(8) 0.0293(6) Uani 1 1 d . . . H56 H -0.0272 0.7458 -0.1486 0.035 Uiso 1 1 calc R . . C57 C 0.05112(11) 0.79511(15) -0.12155(9) 0.0289(6) Uani 1 1 d . . . H57 H 0.0562 0.8272 -0.1453 0.035 Uiso 1 1 calc R . . C58 C -0.02319(11) 0.66265(15) -0.06873(9) 0.0299(6) Uani 1 1 d . . . C59 C -0.01690(12) 0.58951(17) -0.07857(10) 0.0389(7) Uani 1 1 d . . . C60 C -0.05624(15) 0.54150(19) -0.06621(11) 0.0519(9) Uani 1 1 d . . . H60 H -0.0534 0.4908 -0.0720 0.062 Uiso 1 1 calc R . . C61 C -0.09888(15) 0.5659(2) -0.04590(11) 0.0554(9) Uani 1 1 d . . . H61 H -0.1257 0.5322 -0.0384 0.067 Uiso 1 1 calc R . . C62 C -0.10327(13) 0.6390(2) -0.03619(10) 0.0486(9) Uani 1 1 d . . . H62 H -0.1328 0.6548 -0.0217 0.058 Uiso 1 1 calc R . . C63 C -0.06537(11) 0.68981(17) -0.04721(9) 0.0357(7) Uani 1 1 d . . . C64 C -0.07015(12) 0.77023(17) -0.03691(10) 0.0396(7) Uani 1 1 d . . . H64 H -0.0359 0.7954 -0.0442 0.048 Uiso 1 1 calc R . . C65 C -0.12476(14) 0.8044(2) -0.06713(12) 0.0557(9) Uani 1 1 d . . . H65A H -0.1245 0.7985 -0.0998 0.084 Uiso 1 1 calc R . . H65B H -0.1258 0.8565 -0.0599 0.084 Uiso 1 1 calc R . . H65C H -0.1592 0.7803 -0.0612 0.084 Uiso 1 1 calc R . . C66 C -0.06733(18) 0.7833(2) 0.01397(12) 0.0723(12) Uani 1 1 d . . . H66A H -0.1019 0.7625 0.0217 0.108 Uiso 1 1 calc R . . H66B H -0.0659 0.8359 0.0201 0.108 Uiso 1 1 calc R . . H66C H -0.0324 0.7600 0.0330 0.108 Uiso 1 1 calc R . . C67 C 0.03027(13) 0.56206(17) -0.10111(11) 0.0463(8) Uani 1 1 d . . . H67 H 0.0513 0.6059 -0.1088 0.056 Uiso 1 1 calc R . . C68 C 0.07478(17) 0.5154(2) -0.06789(14) 0.0776(13) Uani 1 1 d . . . H68A H 0.0560 0.4708 -0.0606 0.116 Uiso 1 1 calc R . . H68B H 0.0905 0.5428 -0.0393 0.116 Uiso 1 1 calc R . . H68C H 0.1065 0.5025 -0.0824 0.116 Uiso 1 1 calc R . . C69 C 0.00533(14) 0.52217(18) -0.14626(11) 0.0501(8) Uani 1 1 d . . . H69A H 0.0370 0.5084 -0.1606 0.075 Uiso 1 1 calc R . . H69B H -0.0220 0.5542 -0.1673 0.075 Uiso 1 1 calc R . . H69C H -0.0150 0.4782 -0.1400 0.075 Uiso 1 1 calc R . . C70 C 0.14256(11) 0.82633(14) -0.06255(9) 0.0270(6) Uani 1 1 d . . . C71 C 0.14212(12) 0.88462(15) -0.03233(9) 0.0341(6) Uani 1 1 d . . . C72 C 0.19424(13) 0.92158(16) -0.01623(10) 0.0413(7) Uani 1 1 d . . . H72 H 0.1960 0.9611 0.0047 0.050 Uiso 1 1 calc R . . C73 C 0.24340(13) 0.90172(17) -0.03025(11) 0.0442(8) Uani 1 1 d . . . H73 H 0.2787 0.9275 -0.0187 0.053 Uiso 1 1 calc R . . C74 C 0.24208(12) 0.84496(16) -0.06079(11) 0.0408(7) Uani 1 1 d . . . H74 H 0.2764 0.8326 -0.0702 0.049 Uiso 1 1 calc R . . C75 C 0.19130(11) 0.80541(15) -0.07805(9) 0.0302(6) Uani 1 1 d . . . C76 C 0.19056(12) 0.74256(16) -0.11137(10) 0.0346(7) Uani 1 1 d . . . H76 H 0.1492 0.7348 -0.1286 0.042 Uiso 1 1 calc R . . C77 C 0.22557(16) 0.7576(2) -0.14712(12) 0.0614(10) Uani 1 1 d . . . H77A H 0.2122 0.8033 -0.1634 0.092 Uiso 1 1 calc R . . H77B H 0.2201 0.7174 -0.1695 0.092 Uiso 1 1 calc R . . H77C H 0.2669 0.7618 -0.1315 0.092 Uiso 1 1 calc R . . C78 C 0.21159(19) 0.67222(19) -0.08567(12) 0.0680(11) Uani 1 1 d . . . H78A H 0.2517 0.6785 -0.0675 0.102 Uiso 1 1 calc R . . H78B H 0.2101 0.6326 -0.1081 0.102 Uiso 1 1 calc R . . H78C H 0.1865 0.6602 -0.0649 0.102 Uiso 1 1 calc R . . C79 C 0.08688(13) 0.90853(18) -0.01907(10) 0.0446(8) Uani 1 1 d . . . H79 H 0.0594 0.8662 -0.0249 0.054 Uiso 1 1 calc R . . C80 C 0.09659(16) 0.9287(2) 0.03155(12) 0.0679(11) Uani 1 1 d . . . H80A H 0.1179 0.8893 0.0508 0.102 Uiso 1 1 calc R . . H80B H 0.0589 0.9359 0.0391 0.102 Uiso 1 1 calc R . . H80C H 0.1193 0.9739 0.0376 0.102 Uiso 1 1 calc R . . C81 C 0.0581(2) 0.9704(3) -0.05028(16) 0.1038(18) Uani 1 1 d . . . H81A H 0.0825 1.0142 -0.0437 0.156 Uiso 1 1 calc R . . H81B H 0.0198 0.9807 -0.0445 0.156 Uiso 1 1 calc R . . H81C H 0.0534 0.9564 -0.0828 0.156 Uiso 1 1 calc R . . C82 C 0.25722(10) 0.65404(13) 0.11362(8) 0.0216(5) Uani 1 1 d . . . C83 C 0.33350(10) 0.61997(14) 0.17063(8) 0.0239(5) Uani 1 1 d . . . H83 H 0.3612 0.5901 0.1909 0.029 Uiso 1 1 calc R . . C84 C 0.33087(10) 0.69274(14) 0.17105(8) 0.0242(6) Uani 1 1 d . . . H84 H 0.3565 0.7243 0.1918 0.029 Uiso 1 1 calc R . . C85 C 0.26742(10) 0.78973(13) 0.12760(8) 0.0239(5) Uani 1 1 d . . . C86 C 0.30379(11) 0.83596(15) 0.10990(9) 0.0300(6) Uani 1 1 d . . . C87 C 0.28831(13) 0.90918(16) 0.10551(11) 0.0424(7) Uani 1 1 d . . . H87 H 0.3113 0.9422 0.0929 0.051 Uiso 1 1 calc R . . C88 C 0.24039(14) 0.93478(17) 0.11903(12) 0.0500(9) Uani 1 1 d . . . H88 H 0.2309 0.9852 0.1160 0.060 Uiso 1 1 calc R . . C89 C 0.20622(13) 0.88795(16) 0.13689(11) 0.0425(7) Uani 1 1 d . . . H89 H 0.1734 0.9067 0.1461 0.051 Uiso 1 1 calc R . . C90 C 0.21836(11) 0.81392(15) 0.14181(9) 0.0294(6) Uani 1 1 d . . . C91 C 0.35830(11) 0.80792(16) 0.09682(10) 0.0373(7) Uani 1 1 d . . . H91 H 0.3761 0.7708 0.1207 0.045 Uiso 1 1 calc R . . C92 C 0.40386(15) 0.8668(2) 0.09862(14) 0.0712(12) Uani 1 1 d . . . H92A H 0.4411 0.8441 0.0979 0.107 Uiso 1 1 calc R . . H92B H 0.4084 0.8950 0.1273 0.107 Uiso 1 1 calc R . . H92C H 0.3915 0.8993 0.0719 0.107 Uiso 1 1 calc R . . C93 C 0.34429(13) 0.76922(19) 0.05095(12) 0.0548(9) Uani 1 1 d . . . H93A H 0.3143 0.7323 0.0507 0.082 Uiso 1 1 calc R . . H93B H 0.3795 0.7456 0.0461 0.082 Uiso 1 1 calc R . . H93C H 0.3300 0.8046 0.0261 0.082 Uiso 1 1 calc R . . C94 C 0.11667(12) 0.7739(2) 0.14371(11) 0.0500(9) Uani 1 1 d . . . H94A H 0.1051 0.8231 0.1507 0.075 Uiso 1 1 calc R . . H94B H 0.0952 0.7378 0.1574 0.075 Uiso 1 1 calc R . . H94C H 0.1078 0.7671 0.1100 0.075 Uiso 1 1 calc R . . C95 C 0.19675(14) 0.7750(2) 0.21619(11) 0.0565(9) Uani 1 1 d . . . H95A H 0.2385 0.7669 0.2286 0.085 Uiso 1 1 calc R . . H95B H 0.1747 0.7403 0.2303 0.085 Uiso 1 1 calc R . . H95C H 0.1868 0.8249 0.2233 0.085 Uiso 1 1 calc R . . C96 C 0.18154(11) 0.76413(16) 0.16384(9) 0.0338(6) Uani 1 1 d . . . H96 H 0.1916 0.7127 0.1577 0.041 Uiso 1 1 calc R . . C97 C 0.27289(10) 0.52140(13) 0.12334(8) 0.0238(5) Uani 1 1 d . . . C98 C 0.28932(11) 0.49122(14) 0.08518(9) 0.0270(6) Uani 1 1 d . . . C99 C 0.27303(11) 0.41919(15) 0.07447(9) 0.0317(6) Uani 1 1 d . . . H99 H 0.2834 0.3962 0.0490 0.038 Uiso 1 1 calc R . . C100 C 0.24198(11) 0.38068(15) 0.10039(10) 0.0321(6) Uani 1 1 d . . . H100 H 0.2310 0.3317 0.0922 0.038 Uiso 1 1 calc R . . C101 C 0.22664(11) 0.41211(15) 0.13796(9) 0.0307(6) Uani 1 1 d . . . H101 H 0.2057 0.3844 0.1555 0.037 Uiso 1 1 calc R . . C102 C 0.24166(10) 0.48426(14) 0.15028(9) 0.0262(6) Uani 1 1 d . . . C103 C 0.22280(11) 0.51959(15) 0.19063(9) 0.0306(6) Uani 1 1 d . . . H103 H 0.2387 0.5704 0.1943 0.037 Uiso 1 1 calc R . . C104 C 0.15630(12) 0.52485(18) 0.17968(11) 0.0446(8) Uani 1 1 d . . . H10G H 0.1422 0.5518 0.1507 0.067 Uiso 1 1 calc R . . H10H H 0.1446 0.5505 0.2049 0.067 Uiso 1 1 calc R . . H10I H 0.1396 0.4757 0.1765 0.067 Uiso 1 1 calc R . . C105 C 0.24671(12) 0.47931(16) 0.23597(9) 0.0359(7) Uani 1 1 d . . . H10A H 0.2324 0.4290 0.2331 0.054 Uiso 1 1 calc R . . H10B H 0.2338 0.5039 0.2610 0.054 Uiso 1 1 calc R . . H10C H 0.2893 0.4792 0.2430 0.054 Uiso 1 1 calc R . . C106 C 0.32395(12) 0.53391(15) 0.05726(9) 0.0331(6) Uani 1 1 d . . . H106 H 0.3229 0.5865 0.0660 0.040 Uiso 1 1 calc R . . C107 C 0.38754(12) 0.50975(17) 0.06953(10) 0.0414(7) Uani 1 1 d . . . H10J H 0.4034 0.5141 0.1031 0.062 Uiso 1 1 calc R . . H10K H 0.4099 0.5408 0.0533 0.062 Uiso 1 1 calc R . . H10L H 0.3901 0.4589 0.0601 0.062 Uiso 1 1 calc R . . C108 C 0.29751(14) 0.52800(18) 0.00505(10) 0.0456(8) Uani 1 1 d . . . H10D H 0.3002 0.4774 -0.0049 0.068 Uiso 1 1 calc R . . H10E H 0.3188 0.5599 -0.0115 0.068 Uiso 1 1 calc R . . H10F H 0.2566 0.5429 -0.0018 0.068 Uiso 1 1 calc R . . C109 C 0.36604(11) 0.16278(14) 0.98512(9) 0.0265(6) Uani 1 1 d . . . C110 C 0.33614(10) 0.22309(14) 0.99597(8) 0.0252(6) Uani 1 1 d . . . C111 C 0.34869(11) 0.29779(15) 0.98281(9) 0.0287(6) Uani 1 1 d . . . C112 C 0.41805(11) 0.17214(15) 0.96634(9) 0.0299(6) Uani 1 1 d . . . C113 C 0.36234(17) 0.37363(17) 0.92246(11) 0.0537(9) Uani 1 1 d . . . H11G H 0.3351 0.4093 0.9300 0.081 Uiso 1 1 calc R . . H11H H 0.3586 0.3733 0.8889 0.081 Uiso 1 1 calc R . . H11I H 0.4022 0.3870 0.9384 0.081 Uiso 1 1 calc R . . C114 C 0.50498(13) 0.2389(2) 0.97358(12) 0.0545(9) Uani 1 1 d . . . H11J H 0.5233 0.1925 0.9689 0.082 Uiso 1 1 calc R . . H11K H 0.5322 0.2679 0.9968 0.082 Uiso 1 1 calc R . . H11L H 0.4947 0.2658 0.9443 0.082 Uiso 1 1 calc R . . C115 C 0.87074(10) 0.77903(14) 0.78933(8) 0.0255(6) Uani 1 1 d . . . C116 C 0.91349(10) 0.82531(14) 0.78000(8) 0.0244(6) Uani 1 1 d . . . C117 C 0.82095(11) 0.81201(15) 0.80444(9) 0.0297(6) Uani 1 1 d . . . C118 C 0.91556(10) 0.90374(14) 0.79277(9) 0.0261(6) Uani 1 1 d . . . C119 C 0.74058(12) 0.79200(18) 0.83623(11) 0.0419(7) Uani 1 1 d . . . H11D H 0.7535 0.8260 0.8621 0.063 Uiso 1 1 calc R . . H11E H 0.7187 0.7520 0.8459 0.063 Uiso 1 1 calc R . . H11F H 0.7156 0.8177 0.8099 0.063 Uiso 1 1 calc R . . C120 C 0.91647(16) 0.98476(17) 0.85369(11) 0.0526(9) Uani 1 1 d . . . H12D H 0.9450 1.0174 0.8452 0.079 Uiso 1 1 calc R . . H12E H 0.9217 0.9853 0.8874 0.079 Uiso 1 1 calc R . . H12F H 0.8770 1.0012 0.8387 0.079 Uiso 1 1 calc R . . N1 N 0.21305(8) 0.65274(11) 0.68504(7) 0.0269(5) Uani 1 1 d . . . N2 N 0.28660(8) 0.66907(12) 0.65517(7) 0.0278(5) Uani 1 1 d . . . N3 N 0.01607(8) 0.71452(12) -0.08173(7) 0.0256(5) Uani 1 1 d . . . N4 N 0.08937(8) 0.78558(12) -0.07877(7) 0.0257(5) Uani 1 1 d . . . N5 N 0.28400(8) 0.71400(11) 0.13563(7) 0.0206(4) Uani 1 1 d . . . N6 N 0.28816(8) 0.59652(11) 0.13510(7) 0.0218(4) Uani 1 1 d . . . N7 N 0.51282(8) 0.70413(11) 0.86432(7) 0.0206(4) Uani 1 1 d . . . N8 N 0.51504(8) 0.82170(11) 0.86504(7) 0.0232(5) Uani 1 1 d . . . O1 O 0.43013(8) 0.13706(11) 0.93547(6) 0.0365(5) Uani 1 1 d . . . O2 O 0.45313(8) 0.22478(11) 0.98941(7) 0.0408(5) Uani 1 1 d . . . O3 O 0.35601(8) 0.35067(10) 1.00761(7) 0.0360(5) Uani 1 1 d . . . O4 O 0.34920(9) 0.30222(10) 0.93731(6) 0.0383(5) Uani 1 1 d . . . O5 O 0.91159(8) 0.95465(10) 0.76654(6) 0.0358(4) Uani 1 1 d . . . O6 O 0.92484(9) 0.91212(10) 0.83881(6) 0.0381(5) Uani 1 1 d . . . O7 O 0.80724(9) 0.87522(12) 0.80017(8) 0.0521(6) Uani 1 1 d . . . O8 O 0.79065(7) 0.76294(10) 0.82267(6) 0.0334(4) Uani 1 1 d . . . P1 P 0.30198(3) 0.71317(4) 0.75188(2) 0.03310(17) Uani 1 1 d . . . P2 P 0.39093(3) 0.69035(4) 0.76401(2) 0.03013(16) Uani 1 1 d . . . P3 P 0.41171(3) 0.78131(4) 0.80661(3) 0.03386(17) Uani 1 1 d . . . P4 P 0.08998(3) 0.69894(4) 0.00427(2) 0.03206(17) Uani 1 1 d . . . P5 P 0.17827(3) 0.72696(4) 0.02775(2) 0.02758(15) Uani 1 1 d . . . P6 P 0.19077(3) 0.63527(4) 0.06986(2) 0.02979(16) Uani 1 1 d . . . P7 P 0.27908(3) 0.21311(4) 1.02366(3) 0.03137(16) Uani 1 1 d . . . P8 P 0.27962(3) 0.09916(4) 1.02914(3) 0.03983(18) Uani 1 1 d . . . P9 P 0.34802(3) 0.07396(4) 0.99825(3) 0.03566(17) Uani 1 1 d . . . P10 P 0.87153(3) 0.68537(4) 0.77726(2) 0.03027(16) Uani 1 1 d . . . P11 P 0.94556(3) 0.68191(4) 0.75049(2) 0.03220(16) Uani 1 1 d . . . P12 P 0.96851(3) 0.79334(4) 0.75536(2) 0.02785(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0228(13) 0.0260(14) 0.0326(15) -0.0021(11) 0.0063(11) 0.0014(11) C2 0.0239(13) 0.0289(15) 0.0347(16) -0.0043(12) -0.0012(12) 0.0002(11) C3 0.0275(14) 0.0338(16) 0.0298(15) -0.0060(12) -0.0030(12) -0.0009(12) C4 0.0193(12) 0.0268(14) 0.0343(15) -0.0012(11) 0.0032(11) -0.0046(11) C5 0.0225(13) 0.0269(15) 0.0376(16) 0.0012(12) 0.0055(11) -0.0028(11) C6 0.0268(14) 0.0323(16) 0.0447(18) 0.0029(13) 0.0110(12) -0.0023(12) C7 0.0340(16) 0.0487(19) 0.0446(19) 0.0103(15) 0.0139(14) -0.0062(14) C8 0.0365(16) 0.0425(19) 0.060(2) 0.0245(16) 0.0098(15) -0.0018(14) C9 0.0270(14) 0.0299(16) 0.057(2) 0.0097(14) 0.0048(13) 0.0004(12) C10 0.0406(18) 0.0341(18) 0.096(3) 0.0189(18) 0.0202(18) 0.0091(15) C11 0.061(2) 0.042(2) 0.074(3) 0.0040(18) 0.0091(19) 0.0124(17) C12 0.046(2) 0.049(2) 0.152(4) 0.003(3) -0.026(2) 0.0181(19) C13 0.0285(14) 0.0275(15) 0.0507(18) 0.0078(13) 0.0174(13) 0.0035(12) C14 0.0446(17) 0.0383(17) 0.0358(17) 0.0054(13) 0.0089(13) 0.0038(14) C15 0.0486(19) 0.0289(17) 0.071(2) 0.0048(16) -0.0050(17) -0.0054(14) C16 0.0227(13) 0.0465(18) 0.0244(14) -0.0106(12) 0.0050(11) -0.0039(12) C17 0.0262(14) 0.057(2) 0.0240(15) -0.0130(13) 0.0024(11) 0.0057(13) C18 0.0337(16) 0.073(2) 0.0300(17) -0.0048(16) 0.0071(13) 0.0104(16) C19 0.0214(14) 0.093(3) 0.0306(17) -0.0022(17) 0.0063(12) 0.0021(17) C20 0.0406(17) 0.067(2) 0.0360(18) -0.0015(16) 0.0130(14) -0.0134(17) C21 0.0323(15) 0.055(2) 0.0290(16) -0.0075(14) 0.0093(12) -0.0031(14) C22 0.0528(19) 0.0426(19) 0.057(2) 0.0007(16) 0.0261(16) -0.0071(15) C23 0.130(4) 0.057(2) 0.052(2) -0.0105(19) 0.026(2) -0.001(2) C24 0.055(2) 0.053(2) 0.059(2) -0.0023(18) 0.0048(17) -0.0031(17) C25 0.070(2) 0.054(2) 0.057(2) -0.0022(18) -0.0045(19) 0.0033(19) C26 0.0431(17) 0.0397(18) 0.054(2) -0.0138(15) 0.0104(15) 0.0053(14) C27 0.071(3) 0.049(2) 0.091(3) -0.020(2) -0.019(2) 0.002(2) C28 0.0273(13) 0.0198(13) 0.0201(13) -0.0017(10) 0.0080(10) -0.0004(10) C29 0.0246(13) 0.0278(15) 0.0204(13) -0.0003(11) 0.0021(10) 0.0036(11) C30 0.0234(13) 0.0281(15) 0.0213(13) -0.0052(11) -0.0004(10) 0.0019(11) C31 0.0221(13) 0.0201(14) 0.0396(16) -0.0061(12) -0.0051(11) 0.0007(11) C32 0.0229(13) 0.0329(16) 0.0495(19) -0.0126(13) -0.0006(13) 0.0001(12) C33 0.0290(16) 0.0408(19) 0.071(2) -0.0216(17) -0.0058(15) 0.0143(14) C34 0.0474(19) 0.0254(17) 0.074(3) 0.0028(16) -0.0056(18) -0.0040(15) C35 0.0439(18) 0.0324(18) 0.069(2) 0.0106(16) 0.0031(17) 0.0024(15) C36 0.0380(16) 0.0269(16) 0.0484(19) 0.0094(13) -0.0020(14) -0.0026(13) C37 0.0351(16) 0.054(2) 0.055(2) -0.0241(16) 0.0097(15) 0.0100(15) C38 0.042(2) 0.124(4) 0.062(3) -0.028(2) 0.0215(18) -0.008(2) C39 0.049(2) 0.071(3) 0.057(2) -0.0208(19) 0.0004(17) 0.0235(18) C40 0.068(2) 0.044(2) 0.055(2) 0.0222(16) 0.0265(18) 0.0063(17) C41 0.102(3) 0.092(3) 0.054(3) 0.003(2) 0.032(2) -0.005(3) C42 0.056(2) 0.084(3) 0.093(3) 0.022(2) 0.027(2) 0.010(2) C43 0.0233(12) 0.0195(13) 0.0239(14) -0.0001(10) 0.0042(10) 0.0006(10) C44 0.0217(12) 0.0224(13) 0.0210(13) 0.0000(10) 0.0015(10) 0.0013(10) C45 0.0299(14) 0.0259(14) 0.0262(14) -0.0055(11) 0.0052(11) 0.0005(11) C46 0.0385(15) 0.0232(15) 0.0417(17) -0.0025(12) 0.0075(13) -0.0059(12) C47 0.0372(16) 0.0322(16) 0.0451(18) 0.0029(13) 0.0170(14) -0.0097(13) C48 0.0312(14) 0.0276(15) 0.0361(16) 0.0009(12) 0.0137(12) -0.0012(12) C49 0.0542(19) 0.0348(17) 0.0494(19) 0.0021(14) 0.0332(16) -0.0010(14) C50 0.055(2) 0.086(3) 0.067(3) 0.013(2) 0.0402(19) 0.016(2) C51 0.071(2) 0.060(2) 0.041(2) -0.0029(16) 0.0283(17) -0.0002(18) C52 0.0294(13) 0.0231(14) 0.0247(14) -0.0034(11) 0.0102(11) -0.0013(11) C53 0.0238(14) 0.053(2) 0.0499(19) 0.0122(15) 0.0072(13) -0.0027(13) C54 0.0336(16) 0.061(2) 0.0359(17) 0.0135(15) 0.0090(13) 0.0008(15) C55 0.0180(12) 0.0333(15) 0.0225(14) -0.0032(11) 0.0005(10) 0.0042(11) C56 0.0275(14) 0.0400(16) 0.0168(13) 0.0013(11) -0.0015(11) 0.0066(12) C57 0.0253(13) 0.0374(16) 0.0207(14) 0.0032(11) -0.0008(11) 0.0039(12) C58 0.0243(13) 0.0410(17) 0.0200(14) 0.0032(12) -0.0034(11) -0.0037(12) C59 0.0342(15) 0.0418(18) 0.0333(17) 0.0037(13) -0.0064(12) -0.0027(13) C60 0.055(2) 0.046(2) 0.047(2) 0.0055(16) -0.0037(16) -0.0097(17) C61 0.056(2) 0.066(3) 0.041(2) 0.0112(17) 0.0044(16) -0.0272(19) C62 0.0378(17) 0.078(3) 0.0288(17) 0.0012(16) 0.0053(13) -0.0160(17) C63 0.0266(14) 0.0569(19) 0.0202(14) -0.0003(13) -0.0006(11) -0.0083(13) C64 0.0254(14) 0.060(2) 0.0340(17) -0.0094(14) 0.0087(12) -0.0041(14) C65 0.050(2) 0.063(2) 0.051(2) 0.0005(17) 0.0050(16) 0.0019(17) C66 0.085(3) 0.089(3) 0.038(2) -0.016(2) 0.0055(19) 0.023(2) C67 0.0423(17) 0.0358(18) 0.054(2) -0.0047(15) -0.0021(15) 0.0052(14) C68 0.072(3) 0.078(3) 0.069(3) -0.006(2) -0.011(2) 0.031(2) C69 0.0492(19) 0.050(2) 0.050(2) -0.0023(16) 0.0095(16) -0.0013(16) C70 0.0245(13) 0.0289(15) 0.0244(14) 0.0038(11) -0.0004(11) -0.0001(11) C71 0.0363(15) 0.0331(16) 0.0293(15) 0.0025(12) 0.0009(12) 0.0052(13) C72 0.0493(18) 0.0282(16) 0.0390(18) -0.0034(13) -0.0041(14) -0.0023(14) C73 0.0369(17) 0.0384(18) 0.052(2) 0.0011(15) 0.0002(14) -0.0102(14) C74 0.0323(15) 0.0416(18) 0.0479(19) 0.0034(15) 0.0086(14) -0.0060(13) C75 0.0275(14) 0.0306(15) 0.0299(15) 0.0063(12) 0.0018(11) -0.0010(12) C76 0.0266(14) 0.0409(17) 0.0371(16) -0.0018(13) 0.0092(12) 0.0017(12) C77 0.070(2) 0.079(3) 0.041(2) -0.0101(18) 0.0244(18) -0.019(2) C78 0.113(3) 0.050(2) 0.049(2) -0.0002(17) 0.034(2) 0.026(2) C79 0.0450(17) 0.0476(19) 0.0372(18) -0.0118(14) 0.0021(14) 0.0125(15) C80 0.061(2) 0.091(3) 0.049(2) -0.020(2) 0.0084(18) 0.023(2) C81 0.104(4) 0.132(4) 0.077(3) 0.026(3) 0.026(3) 0.086(3) C82 0.0212(12) 0.0219(13) 0.0222(13) 0.0003(10) 0.0061(10) 0.0027(10) C83 0.0202(12) 0.0295(15) 0.0193(13) -0.0020(11) -0.0005(10) 0.0030(11) C84 0.0191(12) 0.0306(15) 0.0201(13) -0.0033(11) -0.0006(10) 0.0014(11) C85 0.0233(12) 0.0212(13) 0.0237(14) -0.0021(10) -0.0015(10) 0.0017(10) C86 0.0264(13) 0.0308(16) 0.0287(15) 0.0003(12) -0.0016(11) -0.0039(11) C87 0.0431(17) 0.0312(17) 0.0478(19) 0.0049(14) 0.0011(14) -0.0085(14) C88 0.054(2) 0.0247(16) 0.063(2) -0.0009(15) -0.0032(17) 0.0091(15) C89 0.0375(16) 0.0372(18) 0.0498(19) -0.0077(14) 0.0047(14) 0.0148(14) C90 0.0251(13) 0.0333(16) 0.0270(15) -0.0067(12) 0.0008(11) 0.0065(12) C91 0.0276(14) 0.0442(18) 0.0405(17) 0.0051(14) 0.0092(12) -0.0055(13) C92 0.051(2) 0.091(3) 0.081(3) -0.035(2) 0.034(2) -0.035(2) C93 0.0349(17) 0.061(2) 0.070(2) -0.0179(19) 0.0141(16) 0.0003(16) C94 0.0303(16) 0.081(3) 0.0389(18) -0.0029(17) 0.0081(13) 0.0005(16) C95 0.0387(17) 0.092(3) 0.0364(19) 0.0049(18) 0.0050(14) -0.0038(18) C96 0.0268(14) 0.0432(17) 0.0332(16) -0.0038(13) 0.0105(12) 0.0071(12) C97 0.0221(12) 0.0204(13) 0.0258(14) 0.0009(10) 0.0001(10) 0.0034(10) C98 0.0258(13) 0.0279(15) 0.0261(14) 0.0001(11) 0.0039(11) 0.0044(11) C99 0.0359(15) 0.0295(15) 0.0286(15) -0.0064(12) 0.0058(12) 0.0052(12) C100 0.0290(14) 0.0247(15) 0.0403(17) -0.0045(12) 0.0039(12) -0.0012(11) C101 0.0251(13) 0.0292(15) 0.0373(16) 0.0005(12) 0.0063(12) -0.0018(11) C102 0.0203(12) 0.0285(15) 0.0281(14) -0.0006(11) 0.0028(10) 0.0029(11) C103 0.0303(14) 0.0280(15) 0.0370(16) -0.0024(12) 0.0147(12) -0.0010(12) C104 0.0379(16) 0.055(2) 0.0465(19) 0.0020(15) 0.0200(14) 0.0104(15) C105 0.0352(15) 0.0394(17) 0.0348(16) -0.0042(13) 0.0120(13) -0.0040(13) C106 0.0453(16) 0.0267(15) 0.0301(15) -0.0005(12) 0.0148(13) 0.0045(13) C107 0.0414(17) 0.0478(19) 0.0372(17) 0.0021(14) 0.0139(14) -0.0080(14) C108 0.0555(19) 0.050(2) 0.0341(17) 0.0116(14) 0.0158(15) 0.0150(16) C109 0.0252(13) 0.0287(15) 0.0222(14) -0.0040(11) -0.0007(10) 0.0040(11) C110 0.0242(13) 0.0272(14) 0.0226(14) -0.0023(11) 0.0025(10) -0.0017(11) C111 0.0270(13) 0.0297(15) 0.0310(15) -0.0016(12) 0.0099(11) 0.0032(11) C112 0.0268(14) 0.0330(16) 0.0270(15) -0.0064(12) 0.0007(11) 0.0059(12) C113 0.090(3) 0.0376(19) 0.045(2) 0.0044(15) 0.0370(19) -0.0054(17) C114 0.0340(17) 0.080(3) 0.054(2) -0.0243(19) 0.0179(15) -0.0142(17) C115 0.0233(13) 0.0311(15) 0.0200(13) 0.0043(11) 0.0014(10) 0.0017(11) C116 0.0234(13) 0.0288(14) 0.0181(13) 0.0025(10) -0.0006(10) 0.0024(11) C117 0.0279(14) 0.0334(17) 0.0272(15) 0.0060(12) 0.0056(11) 0.0011(12) C118 0.0205(12) 0.0313(15) 0.0257(15) 0.0018(12) 0.0039(10) 0.0014(11) C119 0.0317(15) 0.054(2) 0.0448(18) 0.0055(15) 0.0181(13) 0.0032(14) C120 0.074(2) 0.0381(19) 0.045(2) -0.0105(15) 0.0135(17) 0.0137(17) N1 0.0202(10) 0.0255(12) 0.0335(13) -0.0027(9) 0.0035(9) 0.0008(9) N2 0.0208(11) 0.0336(13) 0.0278(12) -0.0066(10) 0.0035(9) 0.0007(9) N3 0.0197(10) 0.0349(13) 0.0203(11) 0.0007(9) 0.0011(8) 0.0016(9) N4 0.0215(10) 0.0324(12) 0.0212(11) 0.0016(9) 0.0014(9) 0.0023(9) N5 0.0184(10) 0.0222(11) 0.0200(11) 0.0000(9) 0.0024(8) 0.0024(8) N6 0.0211(10) 0.0241(11) 0.0189(11) -0.0019(9) 0.0023(8) 0.0010(9) N7 0.0235(10) 0.0201(11) 0.0181(11) -0.0019(8) 0.0047(8) -0.0002(8) N8 0.0246(11) 0.0211(11) 0.0229(11) -0.0027(9) 0.0036(9) 0.0014(9) O1 0.0330(10) 0.0445(12) 0.0304(11) -0.0113(9) 0.0044(8) 0.0081(9) O2 0.0285(10) 0.0559(13) 0.0408(12) -0.0229(10) 0.0136(9) -0.0104(9) O3 0.0478(12) 0.0255(10) 0.0379(11) -0.0059(9) 0.0163(9) 0.0002(9) O4 0.0571(13) 0.0297(11) 0.0328(11) 0.0000(8) 0.0199(9) -0.0038(9) O5 0.0441(11) 0.0292(11) 0.0334(11) 0.0064(9) 0.0080(9) -0.0069(9) O6 0.0560(12) 0.0315(11) 0.0262(11) -0.0035(8) 0.0086(9) 0.0114(9) O7 0.0443(12) 0.0382(13) 0.0831(17) 0.0208(12) 0.0336(12) 0.0161(10) O8 0.0302(10) 0.0372(11) 0.0361(11) 0.0040(9) 0.0141(8) -0.0013(8) P1 0.0215(3) 0.0465(4) 0.0314(4) -0.0130(3) 0.0066(3) -0.0020(3) P2 0.0225(3) 0.0385(4) 0.0277(4) -0.0086(3) 0.0027(3) -0.0008(3) P3 0.0283(4) 0.0269(4) 0.0388(4) -0.0046(3) -0.0067(3) 0.0025(3) P4 0.0207(3) 0.0496(5) 0.0230(4) 0.0060(3) -0.0003(3) 0.0002(3) P5 0.0218(3) 0.0355(4) 0.0224(4) 0.0020(3) -0.0006(3) 0.0018(3) P6 0.0250(3) 0.0265(4) 0.0313(4) -0.0007(3) -0.0060(3) 0.0000(3) P7 0.0300(4) 0.0286(4) 0.0381(4) 0.0009(3) 0.0132(3) 0.0007(3) P8 0.0443(4) 0.0299(4) 0.0464(5) 0.0017(3) 0.0132(4) -0.0068(3) P9 0.0394(4) 0.0246(4) 0.0398(4) -0.0037(3) 0.0035(3) 0.0026(3) P10 0.0290(3) 0.0278(4) 0.0326(4) 0.0026(3) 0.0049(3) -0.0015(3) P11 0.0306(4) 0.0320(4) 0.0328(4) -0.0031(3) 0.0053(3) 0.0042(3) P12 0.0233(3) 0.0345(4) 0.0255(4) -0.0009(3) 0.0055(3) 0.0011(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 C1 N2 1.356(3) . ? C1 N1 1.362(3) . ? C1 P1 1.812(3) . ? C2 C3 1.340(4) . ? C2 N1 1.384(3) . ? C3 N2 1.389(3) . ? C4 C5 1.389(4) . ? C4 C9 1.398(4) . ? C4 N1 1.446(3) . ? C5 C6 1.395(4) . ? C5 C13 1.513(4) . ? C6 C7 1.373(4) . ? C7 C8 1.368(4) . ? C8 C9 1.395(4) . ? C9 C10 1.522(4) . ? C10 C12 1.522(5) . ? C10 C11 1.532(5) . ? C13 C15 1.518(4) . ? C13 C14 1.530(4) . ? C16 C21 1.382(4) . ? C16 C17 1.409(4) . ? C16 N2 1.445(3) . ? C17 C18 1.385(4) . ? C17 C26 1.515(4) . ? C18 C19 1.365(5) . ? C19 C20 1.377(5) . ? C20 C21 1.407(4) . ? C21 C22 1.521(4) . ? C22 C24 1.528(5) . ? C22 C23 1.532(5) . ? C25 C26 1.521(4) . ? C26 C27 1.518(4) . ? C28 N7 1.353(3) . ? C28 N8 1.356(3) . ? C28 P3 1.823(2) . ? C29 C30 1.339(4) . ? C29 N7 1.389(3) . ? C30 N8 1.380(3) . ? C31 C32 1.383(4) . ? C31 C36 1.397(4) . ? C31 N8 1.452(3) . ? C32 C33 1.421(4) . ? C32 C37 1.499(5) . ? C33 C34 1.374(5) . ? C34 C35 1.348(5) . ? C35 C36 1.388(4) . ? C36 C40 1.505(4) . ? C37 C39 1.527(4) . ? C37 C38 1.533(4) . ? C40 C42 1.535(5) . ? C40 C41 1.539(5) . ? C43 C48 1.394(3) . ? C43 C44 1.394(3) . ? C43 N7 1.448(3) . ? C44 C45 1.392(3) . ? C44 C52 1.518(3) . ? C45 C46 1.374(4) . ? C46 C47 1.383(4) . ? C47 C48 1.388(4) . ? C48 C49 1.518(4) . ? C49 C51 1.526(4) . ? C49 C50 1.530(4) . ? C52 C53 1.518(4) . ? C52 C54 1.525(4) . ? C55 N4 1.356(3) . ? C55 N3 1.361(3) . ? C55 P4 1.806(3) . ? C56 C57 1.333(4) . ? C56 N3 1.376(3) . ? C57 N4 1.383(3) . ? C58 C59 1.388(4) . ? C58 C63 1.401(4) . ? C58 N3 1.446(3) . ? C59 C60 1.394(4) . ? C59 C67 1.520(4) . ? C60 C61 1.370(5) . ? C61 C62 1.380(5) . ? C62 C63 1.386(4) . ? C63 C64 1.515(4) . ? C64 C66 1.517(4) . ? C64 C65 1.520(4) . ? C67 C69 1.517(4) . ? C67 C68 1.522(4) . ? C70 C75 1.396(4) . ? C70 C71 1.397(4) . ? C70 N4 1.443(3) . ? C71 C72 1.388(4) . ? C71 C79 1.519(4) . ? C72 C73 1.377(4) . ? C73 C74 1.376(4) . ? C74 C75 1.392(4) . ? C75 C76 1.516(4) . ? C76 C78 1.520(4) . ? C76 C77 1.523(4) . ? C79 C80 1.513(4) . ? C79 C81 1.519(5) . ? C82 N6 1.353(3) . ? C82 N5 1.355(3) . ? C82 P6 1.816(2) . ? C83 C84 1.335(4) . ? C83 N6 1.380(3) . ? C84 N5 1.389(3) . ? C85 C86 1.398(4) . ? C85 C90 1.401(3) . ? C85 N5 1.446(3) . ? C86 C87 1.389(4) . ? C86 C91 1.524(4) . ? C87 C88 1.375(4) . ? C88 C89 1.371(4) . ? C89 C90 1.387(4) . ? C90 C96 1.516(4) . ? C91 C93 1.502(4) . ? C91 C92 1.518(4) . ? C94 C96 1.518(4) . ? C95 C96 1.524(4) . ? C97 C102 1.392(3) . ? C97 C98 1.399(3) . ? C97 N6 1.445(3) . ? C98 C99 1.391(4) . ? C98 C106 1.517(4) . ? C99 C100 1.381(4) . ? C100 C101 1.381(4) . ? C101 C102 1.395(4) . ? C102 C103 1.522(4) . ? C103 C105 1.521(4) . ? C103 C104 1.532(4) . ? C106 C107 1.527(4) . ? C106 C108 1.531(4) . ? C109 C110 1.392(3) . ? C109 C112 1.480(4) . ? C109 P9 1.751(3) . ? C110 C111 1.474(4) . ? C110 P7 1.753(3) . ? C111 O3 1.205(3) . ? C111 O4 1.358(3) . ? C112 O1 1.210(3) . ? C112 O2 1.348(3) . ? C113 O4 1.439(3) . ? C114 O2 1.441(3) . ? C115 C116 1.399(3) . ? C115 C117 1.488(4) . ? C115 P10 1.755(3) . ? C116 C118 1.484(4) . ? C116 P12 1.743(3) . ? C117 O7 1.202(3) . ? C117 O8 1.344(3) . ? C118 O5 1.205(3) . ? C118 O6 1.342(3) . ? C119 O8 1.443(3) . ? C120 O6 1.432(3) . ? P1 P2 2.0913(9) . ? P2 P3 2.0796(10) . ? P4 P5 2.1016(9) . ? P5 P6 2.0737(10) . ? P7 P8 2.0945(10) . ? P8 P9 2.0975(11) . ? P10 P11 2.0940(10) . ? P11 P12 2.1093(10) . ? 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 C1 N1 105.1(2) . . ? N2 C1 P1 134.18(19) . . ? N1 C1 P1 119.74(19) . . ? C3 C2 N1 107.1(2) . . ? C2 C3 N2 107.3(2) . . ? C5 C4 C9 123.1(2) . . ? C5 C4 N1 118.8(2) . . ? C9 C4 N1 118.1(2) . . ? C4 C5 C6 117.0(2) . . ? C4 C5 C13 123.0(2) . . ? C6 C5 C13 120.0(2) . . ? C7 C6 C5 121.3(3) . . ? C8 C7 C6 120.3(3) . . ? C7 C8 C9 121.4(3) . . ? C8 C9 C4 116.9(3) . . ? C8 C9 C10 120.4(3) . . ? C4 C9 C10 122.8(3) . . ? C12 C10 C9 110.9(3) . . ? C12 C10 C11 111.5(3) . . ? C9 C10 C11 111.2(3) . . ? C5 C13 C15 111.1(2) . . ? C5 C13 C14 110.5(2) . . ? C15 C13 C14 110.6(2) . . ? C21 C16 C17 124.6(2) . . ? C21 C16 N2 118.3(2) . . ? C17 C16 N2 117.0(2) . . ? C18 C17 C16 115.9(3) . . ? C18 C17 C26 121.8(3) . . ? C16 C17 C26 122.3(2) . . ? C19 C18 C17 121.2(3) . . ? C18 C19 C20 121.8(3) . . ? C19 C20 C21 120.1(3) . . ? C16 C21 C20 116.3(3) . . ? C16 C21 C22 123.7(2) . . ? C20 C21 C22 120.0(3) . . ? C21 C22 C24 112.1(3) . . ? C21 C22 C23 110.6(3) . . ? C24 C22 C23 110.5(3) . . ? C17 C26 C27 113.1(3) . . ? C17 C26 C25 112.7(3) . . ? C27 C26 C25 109.3(3) . . ? N7 C28 N8 105.4(2) . . ? N7 C28 P3 135.84(18) . . ? N8 C28 P3 118.17(17) . . ? C30 C29 N7 107.5(2) . . ? C29 C30 N8 106.8(2) . . ? C32 C31 C36 124.0(3) . . ? C32 C31 N8 118.0(3) . . ? C36 C31 N8 118.0(2) . . ? C31 C32 C33 115.6(3) . . ? C31 C32 C37 122.8(3) . . ? C33 C32 C37 121.5(3) . . ? C34 C33 C32 120.6(3) . . ? C35 C34 C33 121.9(3) . . ? C34 C35 C36 120.6(3) . . ? C35 C36 C31 117.3(3) . . ? C35 C36 C40 119.3(3) . . ? C31 C36 C40 123.3(2) . . ? C32 C37 C39 109.5(3) . . ? C32 C37 C38 113.0(3) . . ? C39 C37 C38 109.9(3) . . ? C36 C40 C42 110.4(3) . . ? C36 C40 C41 112.1(3) . . ? C42 C40 C41 111.7(3) . . ? C48 C43 C44 123.8(2) . . ? C48 C43 N7 119.1(2) . . ? C44 C43 N7 117.0(2) . . ? C45 C44 C43 116.9(2) . . ? C45 C44 C52 120.5(2) . . ? C43 C44 C52 122.6(2) . . ? C46 C45 C44 120.8(2) . . ? C45 C46 C47 120.8(3) . . ? C46 C47 C48 121.0(3) . . ? C47 C48 C43 116.7(2) . . ? C47 C48 C49 120.6(2) . . ? C43 C48 C49 122.7(2) . . ? C48 C49 C51 110.4(2) . . ? C48 C49 C50 111.5(3) . . ? C51 C49 C50 111.2(3) . . ? C53 C52 C44 110.8(2) . . ? C53 C52 C54 110.0(2) . . ? C44 C52 C54 111.2(2) . . ? N4 C55 N3 104.9(2) . . ? N4 C55 P4 135.64(19) . . ? N3 C55 P4 119.32(19) . . ? C57 C56 N3 107.0(2) . . ? C56 C57 N4 107.6(2) . . ? C59 C58 C63 124.3(3) . . ? C59 C58 N3 118.0(2) . . ? C63 C58 N3 117.6(2) . . ? C58 C59 C60 116.2(3) . . ? C58 C59 C67 122.7(3) . . ? C60 C59 C67 121.1(3) . . ? C61 C60 C59 121.4(3) . . ? C60 C61 C62 120.7(3) . . ? C61 C62 C63 121.1(3) . . ? C62 C63 C58 116.3(3) . . ? C62 C63 C64 121.4(3) . . ? C58 C63 C64 122.3(2) . . ? C63 C64 C66 111.6(3) . . ? C63 C64 C65 112.1(2) . . ? C66 C64 C65 110.5(3) . . ? C69 C67 C59 112.3(3) . . ? C69 C67 C68 111.4(3) . . ? C59 C67 C68 111.5(3) . . ? C75 C70 C71 123.9(2) . . ? C75 C70 N4 118.2(2) . . ? C71 C70 N4 118.0(2) . . ? C72 C71 C70 116.8(3) . . ? C72 C71 C79 121.3(3) . . ? C70 C71 C79 121.9(2) . . ? C73 C72 C71 120.9(3) . . ? C74 C73 C72 120.9(3) . . ? C73 C74 C75 121.1(3) . . ? C74 C75 C70 116.4(3) . . ? C74 C75 C76 120.6(2) . . ? C70 C75 C76 123.0(2) . . ? C75 C76 C78 111.4(2) . . ? C75 C76 C77 113.3(2) . . ? C78 C76 C77 109.7(3) . . ? C80 C79 C81 111.3(3) . . ? C80 C79 C71 113.3(3) . . ? C81 C79 C71 110.1(3) . . ? N6 C82 N5 105.48(19) . . ? N6 C82 P6 117.87(17) . . ? N5 C82 P6 136.28(18) . . ? C84 C83 N6 106.8(2) . . ? C83 C84 N5 107.7(2) . . ? C86 C85 C90 123.6(2) . . ? C86 C85 N5 118.4(2) . . ? C90 C85 N5 117.8(2) . . ? C87 C86 C85 116.6(3) . . ? C87 C86 C91 121.5(3) . . ? C85 C86 C91 121.9(2) . . ? C88 C87 C86 121.3(3) . . ? C89 C88 C87 120.4(3) . . ? C88 C89 C90 121.8(3) . . ? C89 C90 C85 116.3(3) . . ? C89 C90 C96 120.5(2) . . ? C85 C90 C96 123.0(2) . . ? C93 C91 C92 111.5(3) . . ? C93 C91 C86 112.1(2) . . ? C92 C91 C86 112.9(3) . . ? C90 C96 C94 113.0(2) . . ? C90 C96 C95 110.1(2) . . ? C94 C96 C95 110.7(2) . . ? C102 C97 C98 124.3(2) . . ? C102 C97 N6 117.6(2) . . ? C98 C97 N6 118.1(2) . . ? C99 C98 C97 116.4(2) . . ? C99 C98 C106 121.4(2) . . ? C97 C98 C106 122.2(2) . . ? C100 C99 C98 120.9(2) . . ? C99 C100 C101 121.2(3) . . ? C100 C101 C102 120.5(2) . . ? C97 C102 C101 116.7(2) . . ? C97 C102 C103 122.9(2) . . ? C101 C102 C103 120.4(2) . . ? C105 C103 C102 112.0(2) . . ? C105 C103 C104 111.2(2) . . ? C102 C103 C104 110.0(2) . . ? C98 C106 C107 110.6(2) . . ? C98 C106 C108 112.1(2) . . ? C107 C106 C108 111.1(2) . . ? C110 C109 C112 120.8(2) . . ? C110 C109 P9 121.4(2) . . ? C112 C109 P9 117.50(19) . . ? C109 C110 C111 122.0(2) . . ? C109 C110 P7 121.3(2) . . ? C111 C110 P7 116.70(18) . . ? O3 C111 O4 121.8(2) . . ? O3 C111 C110 126.4(2) . . ? O4 C111 C110 111.8(2) . . ? O1 C112 O2 122.5(2) . . ? O1 C112 C109 126.5(2) . . ? O2 C112 C109 111.0(2) . . ? C116 C115 C117 118.5(2) . . ? C116 C115 P10 120.57(19) . . ? C117 C115 P10 120.51(19) . . ? C115 C116 C118 121.1(2) . . ? C115 C116 P12 122.0(2) . . ? C118 C116 P12 116.82(18) . . ? O7 C117 O8 122.1(2) . . ? O7 C117 C115 125.0(2) . . ? O8 C117 C115 112.9(2) . . ? O5 C118 O6 122.7(2) . . ? O5 C118 C116 126.3(2) . . ? O6 C118 C116 111.0(2) . . ? C1 N1 C2 110.3(2) . . ? C1 N1 C4 124.5(2) . . ? C2 N1 C4 125.0(2) . . ? C1 N2 C3 110.2(2) . . ? C1 N2 C16 127.3(2) . . ? C3 N2 C16 122.3(2) . . ? C55 N3 C56 110.5(2) . . ? C55 N3 C58 124.4(2) . . ? C56 N3 C58 125.1(2) . . ? C55 N4 C57 109.9(2) . . ? C55 N4 C70 125.4(2) . . ? C57 N4 C70 124.5(2) . . ? C82 N5 C84 109.5(2) . . ? C82 N5 C85 128.44(19) . . ? C84 N5 C85 122.0(2) . . ? C82 N6 C83 110.6(2) . . ? C82 N6 C97 123.58(19) . . ? C83 N6 C97 125.8(2) . . ? C28 N7 C29 109.7(2) . . ? C28 N7 C43 126.6(2) . . ? C29 N7 C43 123.2(2) . . ? C28 N8 C30 110.5(2) . . ? C28 N8 C31 123.7(2) . . ? C30 N8 C31 125.8(2) . . ? C112 O2 C114 115.5(2) . . ? C111 O4 C113 114.5(2) . . ? C118 O6 C120 114.9(2) . . ? C117 O8 C119 114.9(2) . . ? C1 P1 P2 105.01(8) . . ? P3 P2 P1 91.43(4) . . ? C28 P3 P2 106.60(8) . . ? C55 P4 P5 105.19(8) . . ? P6 P5 P4 89.31(4) . . ? C82 P6 P5 104.58(8) . . ? C110 P7 P8 98.61(9) . . ? P7 P8 P9 100.15(4) . . ? C109 P9 P8 98.54(9) . . ? C115 P10 P11 99.13(9) . . ? P10 P11 P12 99.79(4) . . ? C116 P12 P11 98.51(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 63.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.485 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.053 _database_code_depnum_ccdc_archive 'CCDC 937996'