# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_rac-(MesPH)2C14H8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 P2' _chemical_formula_weight 478.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.4465(6) _cell_length_b 26.2356(19) _cell_length_c 11.8552(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.1400(10) _cell_angle_gamma 90.00 _cell_volume 2623.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.22 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.664 _exptl_crystal_size_mid 0.253 _exptl_crystal_size_min 0.129 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.184 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.91730 _exptl_absorpt_correction_T_max 0.98384 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 36816 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.10 _reflns_number_total 5785 _reflns_number_gt 4929 _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^)+(0.0573P)^2^+1.4390P] 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 5785 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.76916(5) 1.01946(2) 0.31954(5) 0.04822(16) Uani 1 1 d . . . P2 P 0.76703(5) 0.840779(18) 0.45226(6) 0.05101(17) Uani 1 1 d . . . C11 C 1.06582(18) 0.96886(6) 0.34012(14) 0.0315(3) Uani 1 1 d . . . C9 C 0.98208(18) 0.83570(6) 0.44312(14) 0.0308(3) Uani 1 1 d . . . C24 C 0.70397(18) 0.77710(6) 0.49272(15) 0.0322(3) Uani 1 1 d . . . C1 C 0.98421(19) 1.01474(6) 0.30592(16) 0.0370(4) Uani 1 1 d . . . C14 C 1.06493(18) 0.87993(6) 0.40631(13) 0.0304(3) Uani 1 1 d . . . C13 C 1.23217(19) 0.87678(7) 0.39262(14) 0.0350(4) Uani 1 1 d . . . C7 C 1.2311(2) 0.78895(7) 0.45382(15) 0.0385(4) Uani 1 1 d . . . H7 H 1.2865 0.7582 0.4714 0.046 Uiso 1 1 calc R . . C19 C 0.5723(2) 1.13147(7) 0.11406(16) 0.0383(4) Uani 1 1 d . . . H19 H 0.5275 1.1643 0.1241 0.046 Uiso 1 1 calc R . . C8 C 1.0651(2) 0.79168(7) 0.46671(14) 0.0351(4) Uani 1 1 d . . . H8 H 1.0106 0.7625 0.4921 0.042 Uiso 1 1 calc R . . C20 C 0.63629(19) 1.10565(6) 0.20838(15) 0.0362(4) Uani 1 1 d . . . C25 C 0.6904(2) 0.76424(7) 0.60704(15) 0.0360(4) Uani 1 1 d . . . C28 C 0.5885(2) 0.69589(7) 0.43979(16) 0.0385(4) Uani 1 1 d . . . H28 H 0.5560 0.6721 0.3827 0.046 Uiso 1 1 calc R . . C10 C 0.98641(18) 0.92607(6) 0.38129(15) 0.0339(4) Uani 1 1 d . . . H10 H 0.8762 0.9285 0.3925 0.041 Uiso 1 1 calc R . . C26 C 0.6211(2) 0.71799(7) 0.63397(16) 0.0408(4) Uani 1 1 d . . . H26 H 0.6099 0.7097 0.7112 0.049 Uiso 1 1 calc R . . C15 C 0.70263(19) 1.05707(6) 0.19491(17) 0.0389(4) Uani 1 1 d . . . C29 C 0.65529(19) 0.74190(7) 0.40847(15) 0.0352(4) Uani 1 1 d . . . C5 C 1.3124(2) 0.91982(8) 0.35669(17) 0.0437(4) Uani 1 1 d . . . H5 H 1.4239 0.9180 0.3504 0.052 Uiso 1 1 calc R . . C6 C 1.3106(2) 0.82971(7) 0.41675(15) 0.0397(4) Uani 1 1 d . . . H6 H 1.4210 0.8269 0.4066 0.048 Uiso 1 1 calc R . . C12 C 1.23382(19) 0.96582(7) 0.32954(15) 0.0368(4) Uani 1 1 d . . . C2 C 1.0690(2) 1.05488(7) 0.26644(19) 0.0495(5) Uani 1 1 d . . . H2 H 1.0151 1.0853 0.2442 0.059 Uiso 1 1 calc R . . C4 C 1.3146(2) 1.00901(8) 0.28884(17) 0.0449(4) Uani 1 1 d . . . H4 H 1.4263 1.0077 0.2831 0.054 Uiso 1 1 calc R . . C3 C 1.2351(2) 1.05194(8) 0.2581(2) 0.0516(5) Uani 1 1 d . . . H3 H 1.2912 1.0804 0.2308 0.062 Uiso 1 1 calc R . . C18 C 0.5715(2) 1.11137(8) 0.00666(17) 0.0439(4) Uani 1 1 d . . . C27 C 0.5680(2) 0.68368(7) 0.55177(17) 0.0399(4) Uani 1 1 d . . . C16 C 0.7041(2) 1.03614(7) 0.0860(2) 0.0488(5) Uani 1 1 d . . . C17 C 0.6384(2) 1.06360(9) -0.00538(19) 0.0527(5) Uani 1 1 d . . . H17 H 0.6395 1.0491 -0.0787 0.063 Uiso 1 1 calc R . . C30 C 0.7532(3) 0.79857(9) 0.70169(18) 0.0535(5) Uani 1 1 d . . . H30A H 0.6865 0.8290 0.7047 0.080 Uiso 1 1 calc R . . H30B H 0.8623 0.8087 0.6881 0.080 Uiso 1 1 calc R . . H30C H 0.7517 0.7803 0.7737 0.080 Uiso 1 1 calc R . . C32 C 0.6752(3) 0.75215(9) 0.28494(17) 0.0544(5) Uani 1 1 d . . . H32A H 0.6519 0.7210 0.2414 0.082 Uiso 1 1 calc R . . H32B H 0.7845 0.7628 0.2742 0.082 Uiso 1 1 calc R . . H32C H 0.6021 0.7792 0.2589 0.082 Uiso 1 1 calc R . . C22 C 0.5031(3) 1.14107(10) -0.09321(19) 0.0603(6) Uani 1 1 d . . . H22A H 0.4219 1.1646 -0.0683 0.091 Uiso 1 1 calc R . . H22B H 0.4553 1.1175 -0.1494 0.091 Uiso 1 1 calc R . . H22C H 0.5876 1.1605 -0.1270 0.091 Uiso 1 1 calc R . . C23 C 0.6339(3) 1.13089(8) 0.32261(18) 0.0520(5) Uani 1 1 d . . . H23A H 0.5937 1.1658 0.3136 0.078 Uiso 1 1 calc R . . H23B H 0.7417 1.1317 0.3577 0.078 Uiso 1 1 calc R . . H23C H 0.5649 1.1116 0.3708 0.078 Uiso 1 1 calc R . . C31 C 0.4939(3) 0.63363(8) 0.5834(2) 0.0628(6) Uani 1 1 d . . . H31A H 0.4457 0.6174 0.5154 0.094 Uiso 1 1 calc R . . H31B H 0.4121 0.6399 0.6373 0.094 Uiso 1 1 calc R . . H31C H 0.5757 0.6112 0.6179 0.094 Uiso 1 1 calc R . . C21 C 0.7759(3) 0.98452(9) 0.0651(3) 0.0770(8) Uani 1 1 d . . . H21A H 0.7619 0.9761 -0.0153 0.116 Uiso 1 1 calc R . . H21B H 0.7232 0.9587 0.1096 0.116 Uiso 1 1 calc R . . H21C H 0.8893 0.9853 0.0876 0.116 Uiso 1 1 calc R . . H1P H 0.724(5) 0.9743(17) 0.265(4) 0.169(17) Uiso 1 1 d . . . H2P H 0.752(5) 0.8706(15) 0.537(3) 0.138(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0280(2) 0.0431(3) 0.0744(4) 0.0234(2) 0.0098(2) 0.00549(19) P2 0.0250(2) 0.0303(2) 0.0982(5) 0.0176(3) 0.0077(2) 0.00444(17) C11 0.0245(7) 0.0358(8) 0.0341(8) 0.0005(7) 0.0010(6) 0.0002(6) C9 0.0258(7) 0.0329(8) 0.0336(8) 0.0005(6) 0.0003(6) 0.0054(6) C24 0.0236(7) 0.0297(8) 0.0434(9) 0.0064(7) 0.0017(6) 0.0053(6) C1 0.0264(8) 0.0338(9) 0.0511(10) 0.0052(7) 0.0042(7) -0.0017(6) C14 0.0242(7) 0.0338(8) 0.0331(8) 0.0005(6) 0.0012(6) 0.0041(6) C13 0.0240(7) 0.0437(9) 0.0369(9) 0.0011(7) -0.0004(6) 0.0051(7) C7 0.0343(9) 0.0393(9) 0.0412(9) -0.0029(7) -0.0034(7) 0.0142(7) C19 0.0353(9) 0.0299(8) 0.0496(10) 0.0039(7) 0.0020(7) -0.0009(7) C8 0.0330(8) 0.0329(8) 0.0391(9) 0.0006(7) -0.0007(7) 0.0068(7) C20 0.0290(8) 0.0317(8) 0.0479(10) 0.0041(7) 0.0030(7) -0.0012(6) C25 0.0318(8) 0.0353(9) 0.0407(9) 0.0014(7) -0.0003(7) 0.0072(7) C28 0.0322(8) 0.0339(9) 0.0488(10) -0.0021(7) -0.0029(7) 0.0031(7) C10 0.0218(7) 0.0368(9) 0.0431(9) 0.0056(7) 0.0013(6) 0.0011(6) C26 0.0390(9) 0.0430(10) 0.0405(9) 0.0111(8) 0.0033(7) 0.0052(8) C15 0.0268(8) 0.0299(8) 0.0600(11) 0.0077(8) 0.0034(7) -0.0018(6) C29 0.0295(8) 0.0367(9) 0.0393(9) 0.0045(7) 0.0014(6) 0.0060(7) C5 0.0231(8) 0.0538(11) 0.0547(11) 0.0046(9) 0.0060(7) 0.0037(7) C6 0.0251(8) 0.0509(10) 0.0429(10) -0.0021(8) -0.0007(7) 0.0112(7) C12 0.0243(7) 0.0464(10) 0.0396(9) 0.0000(7) 0.0014(6) -0.0030(7) C2 0.0368(10) 0.0349(9) 0.0770(14) 0.0101(9) 0.0055(9) -0.0036(7) C4 0.0274(8) 0.0512(11) 0.0565(11) -0.0011(9) 0.0056(8) -0.0098(8) C3 0.0373(10) 0.0423(10) 0.0759(14) 0.0040(10) 0.0098(9) -0.0138(8) C18 0.0361(9) 0.0469(10) 0.0484(11) 0.0038(8) 0.0003(8) -0.0064(8) C27 0.0307(8) 0.0332(9) 0.0558(11) 0.0104(8) 0.0016(7) 0.0017(7) C16 0.0345(9) 0.0362(10) 0.0753(14) -0.0091(9) 0.0003(9) 0.0007(7) C17 0.0447(11) 0.0577(12) 0.0555(12) -0.0167(10) 0.0017(9) -0.0018(9) C30 0.0596(13) 0.0526(12) 0.0474(11) -0.0061(9) -0.0060(9) 0.0022(10) C32 0.0618(13) 0.0601(13) 0.0417(11) 0.0049(9) 0.0054(9) 0.0004(10) C22 0.0571(13) 0.0735(15) 0.0497(12) 0.0128(11) -0.0036(10) -0.0036(11) C23 0.0516(12) 0.0535(12) 0.0502(11) -0.0021(9) -0.0041(9) 0.0100(9) C31 0.0583(13) 0.0441(12) 0.0862(17) 0.0204(11) 0.0047(12) -0.0109(10) C21 0.0596(15) 0.0492(13) 0.121(2) -0.0284(14) -0.0095(14) 0.0147(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.8365(17) . ? P1 C15 1.8389(19) . ? P1 H1P 1.39(4) . ? P2 C24 1.8256(17) . ? P2 C9 1.8305(16) . ? P2 H2P 1.28(4) . ? C11 C10 1.409(2) . ? C11 C12 1.434(2) . ? C11 C1 1.435(2) . ? C9 C8 1.372(2) . ? C9 C14 1.435(2) . ? C24 C29 1.405(2) . ? C24 C25 1.407(2) . ? C1 C2 1.370(2) . ? C14 C10 1.404(2) . ? C14 C13 1.433(2) . ? C13 C5 1.396(3) . ? C13 C6 1.423(2) . ? C7 C6 1.349(3) . ? C7 C8 1.420(2) . ? C7 H7 0.9500 . ? C19 C18 1.378(3) . ? C19 C20 1.391(2) . ? C19 H19 0.9500 . ? C8 H8 0.9500 . ? C20 C15 1.405(2) . ? C20 C23 1.509(3) . ? C25 C26 1.392(3) . ? C25 C30 1.512(3) . ? C28 C27 1.386(3) . ? C28 C29 1.392(2) . ? C28 H28 0.9500 . ? C10 H10 0.9500 . ? C26 C27 1.383(3) . ? C26 H26 0.9500 . ? C15 C16 1.404(3) . ? C29 C32 1.507(3) . ? C5 C12 1.406(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C12 C4 1.421(3) . ? C2 C3 1.413(3) . ? C2 H2 0.9500 . ? C4 C3 1.351(3) . ? C4 H4 0.9500 . ? C3 H3 0.9500 . ? C18 C17 1.386(3) . ? C18 C22 1.506(3) . ? C27 C31 1.511(3) . ? C16 C17 1.391(3) . ? C16 C21 1.510(3) . ? C17 H17 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 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 C1 P1 C15 103.05(8) . . ? C1 P1 H1P 98.4(19) . . ? C15 P1 H1P 91.2(19) . . ? C24 P2 C9 104.70(7) . . ? C24 P2 H2P 108.0(17) . . ? C9 P2 H2P 103.6(17) . . ? C10 C11 C12 118.58(15) . . ? C10 C11 C1 122.42(14) . . ? C12 C11 C1 118.99(15) . . ? C8 C9 C14 119.36(15) . . ? C8 C9 P2 123.16(13) . . ? C14 C9 P2 117.46(11) . . ? C29 C24 C25 119.40(15) . . ? C29 C24 P2 119.53(13) . . ? C25 C24 P2 120.84(13) . . ? C2 C1 C11 119.28(15) . . ? C2 C1 P1 121.09(14) . . ? C11 C1 P1 119.60(12) . . ? C10 C14 C13 118.87(15) . . ? C10 C14 C9 121.91(14) . . ? C13 C14 C9 119.20(14) . . ? C5 C13 C6 122.34(15) . . ? C5 C13 C14 119.09(15) . . ? C6 C13 C14 118.57(16) . . ? C6 C7 C8 120.47(16) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C18 C19 C20 122.59(17) . . ? C18 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C9 C8 C7 121.12(16) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C19 C20 C15 119.35(17) . . ? C19 C20 C23 118.97(16) . . ? C15 C20 C23 121.68(17) . . ? C26 C25 C24 119.16(16) . . ? C26 C25 C30 118.94(17) . . ? C24 C25 C30 121.88(17) . . ? C27 C28 C29 122.01(17) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C14 C10 C11 122.14(14) . . ? C14 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C27 C26 C25 122.01(17) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C16 C15 C20 118.88(17) . . ? C16 C15 P1 120.77(14) . . ? C20 C15 P1 120.11(15) . . ? C28 C29 C24 119.18(16) . . ? C28 C29 C32 118.85(17) . . ? C24 C29 C32 121.96(16) . . ? C13 C5 C12 122.22(15) . . ? C13 C5 H5 118.9 . . ? C12 C5 H5 118.9 . . ? C7 C6 C13 121.25(15) . . ? C7 C6 H6 119.4 . . ? C13 C6 H6 119.4 . . ? C5 C12 C4 122.18(16) . . ? C5 C12 C11 119.01(16) . . ? C4 C12 C11 118.79(16) . . ? C1 C2 C3 121.42(18) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C3 C4 C12 121.01(17) . . ? C3 C4 H4 119.5 . . ? C12 C4 H4 119.5 . . ? C4 C3 C2 120.48(17) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C19 C18 C17 117.38(18) . . ? C19 C18 C22 120.73(19) . . ? C17 C18 C22 121.9(2) . . ? C26 C27 C28 118.14(16) . . ? C26 C27 C31 120.91(19) . . ? C28 C27 C31 120.93(19) . . ? C17 C16 C15 119.38(18) . . ? C17 C16 C21 118.9(2) . . ? C15 C16 C21 121.7(2) . . ? C18 C17 C16 122.41(19) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C27 C31 H31A 109.5 . . ? C27 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C27 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? 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 C24 P2 C9 C8 -1.55(17) . . . . ? C24 P2 C9 C14 176.67(13) . . . . ? C9 P2 C24 C29 -92.57(14) . . . . ? C9 P2 C24 C25 92.95(14) . . . . ? C10 C11 C1 C2 -179.87(18) . . . . ? C12 C11 C1 C2 -1.4(3) . . . . ? C10 C11 C1 P1 1.9(2) . . . . ? C12 C11 C1 P1 -179.68(13) . . . . ? C15 P1 C1 C2 37.62(19) . . . . ? C15 P1 C1 C11 -144.18(15) . . . . ? C8 C9 C14 C10 -179.80(16) . . . . ? P2 C9 C14 C10 1.9(2) . . . . ? C8 C9 C14 C13 1.4(2) . . . . ? P2 C9 C14 C13 -176.92(12) . . . . ? C10 C14 C13 C5 1.1(2) . . . . ? C9 C14 C13 C5 179.93(16) . . . . ? C10 C14 C13 C6 -179.21(16) . . . . ? C9 C14 C13 C6 -0.3(2) . . . . ? C14 C9 C8 C7 -0.9(3) . . . . ? P2 C9 C8 C7 177.31(13) . . . . ? C6 C7 C8 C9 -0.7(3) . . . . ? C18 C19 C20 C15 -0.2(3) . . . . ? C18 C19 C20 C23 179.21(17) . . . . ? C29 C24 C25 C26 -3.5(2) . . . . ? P2 C24 C25 C26 171.03(13) . . . . ? C29 C24 C25 C30 174.80(16) . . . . ? P2 C24 C25 C30 -10.7(2) . . . . ? C13 C14 C10 C11 1.9(3) . . . . ? C9 C14 C10 C11 -176.98(16) . . . . ? C12 C11 C10 C14 -3.5(3) . . . . ? C1 C11 C10 C14 174.93(16) . . . . ? C24 C25 C26 C27 1.4(3) . . . . ? C30 C25 C26 C27 -176.88(17) . . . . ? C19 C20 C15 C16 0.7(2) . . . . ? C23 C20 C15 C16 -178.66(17) . . . . ? C19 C20 C15 P1 -173.69(13) . . . . ? C23 C20 C15 P1 6.9(2) . . . . ? C1 P1 C15 C16 70.36(16) . . . . ? C1 P1 C15 C20 -115.32(14) . . . . ? C27 C28 C29 C24 0.2(2) . . . . ? C27 C28 C29 C32 179.37(17) . . . . ? C25 C24 C29 C28 2.7(2) . . . . ? P2 C24 C29 C28 -171.88(12) . . . . ? C25 C24 C29 C32 -176.49(16) . . . . ? P2 C24 C29 C32 9.0(2) . . . . ? C6 C13 C5 C12 177.98(17) . . . . ? C14 C13 C5 C12 -2.3(3) . . . . ? C8 C7 C6 C13 1.8(3) . . . . ? C5 C13 C6 C7 178.48(18) . . . . ? C14 C13 C6 C7 -1.3(3) . . . . ? C13 C5 C12 C4 -177.53(18) . . . . ? C13 C5 C12 C11 0.6(3) . . . . ? C10 C11 C12 C5 2.2(3) . . . . ? C1 C11 C12 C5 -176.25(17) . . . . ? C10 C11 C12 C4 -179.54(17) . . . . ? C1 C11 C12 C4 2.0(3) . . . . ? C11 C1 C2 C3 0.3(3) . . . . ? P1 C1 C2 C3 178.55(17) . . . . ? C5 C12 C4 C3 176.7(2) . . . . ? C11 C12 C4 C3 -1.4(3) . . . . ? C12 C4 C3 C2 0.3(3) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C20 C19 C18 C17 -0.3(3) . . . . ? C20 C19 C18 C22 -179.08(17) . . . . ? C25 C26 C27 C28 1.4(3) . . . . ? C25 C26 C27 C31 179.69(17) . . . . ? C29 C28 C27 C26 -2.2(3) . . . . ? C29 C28 C27 C31 179.49(17) . . . . ? C20 C15 C16 C17 -0.8(3) . . . . ? P1 C15 C16 C17 173.61(15) . . . . ? C20 C15 C16 C21 178.96(19) . . . . ? P1 C15 C16 C21 -6.7(3) . . . . ? C19 C18 C17 C16 0.2(3) . . . . ? C22 C18 C17 C16 179.01(19) . . . . ? C15 C16 C17 C18 0.3(3) . . . . ? C21 C16 C17 C18 -179.4(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.448 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.042 _database_code_depnum_ccdc_archive 'CCDC 948785' ####################################################################### # # 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_rac-4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 P2 Se2, 2(C5H12)' _chemical_formula_sum 'C26 H52 P2 Se2' _chemical_formula_weight 584.5643 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 9.2514(7) _cell_length_b 21.7558(18) _cell_length_c 12.7311(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.930(6) _cell_angle_gamma 90.00 _cell_volume 2562.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7061 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 23.53 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 3.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4144 _exptl_absorpt_correction_T_max 0.8333 _exptl_absorpt_process_details 'Blessing, R. H. (1995) Acta Cryst. A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29577 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4432 _reflns_number_gt 3159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4432 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.4966(4) 0.72902(16) 0.0163(3) 0.0366(9) Uani 1 1 d . . . C2 C 0.4886(5) 0.7320(2) 0.1365(3) 0.0603(12) Uani 1 1 d . . . H2A H 0.5512 0.7652 0.1627 0.090 Uiso 1 1 calc R . . H2B H 0.5209 0.6928 0.1665 0.090 Uiso 1 1 calc R . . H2C H 0.3887 0.7400 0.1569 0.090 Uiso 1 1 calc R . . C3 C 0.6489(4) 0.7117(2) -0.0188(4) 0.0619(13) Uani 1 1 d . . . H3A H 0.7170 0.7442 0.0018 0.093 Uiso 1 1 calc R . . H3B H 0.6492 0.7068 -0.0954 0.093 Uiso 1 1 calc R . . H3C H 0.6781 0.6729 0.0146 0.093 Uiso 1 1 calc R . . C4 C 0.4518(5) 0.79095(18) -0.0314(4) 0.0573(12) Uani 1 1 d . . . H4A H 0.5168 0.8232 -0.0051 0.086 Uiso 1 1 calc R . . H4B H 0.3523 0.8005 -0.0116 0.086 Uiso 1 1 calc R . . H4C H 0.4575 0.7888 -0.1081 0.086 Uiso 1 1 calc R . . P1 P 0.36740(10) 0.67067(4) -0.03405(7) 0.0292(2) Uani 1 1 d . . . Se1 Se 0.14840(4) 0.688042(17) 0.00201(3) 0.03560(14) Uani 1 1 d . . . C5 C 0.4392(4) 0.59570(15) 0.0062(3) 0.0365(9) Uani 1 1 d . . . H5A H 0.5305 0.5884 -0.0313 0.044 Uiso 1 1 calc R . . H5B H 0.4628 0.5972 0.0823 0.044 Uiso 1 1 calc R . . C6 C 0.3390(3) 0.54175(15) -0.0141(3) 0.0264(8) Uani 1 1 d . . . C7 C 0.3352(3) 0.51181(16) -0.1107(3) 0.0303(9) Uani 1 1 d . . . H7A H 0.3946 0.5258 -0.1660 0.036 Uiso 1 1 calc R . . C8 C 0.2457(3) 0.46199(16) -0.1265(3) 0.0302(9) Uani 1 1 d . . . H8A H 0.2429 0.4420 -0.1928 0.036 Uiso 1 1 calc R . . C9 C 0.1590(3) 0.44080(16) -0.0453(3) 0.0313(9) Uani 1 1 d . . . H9A H 0.0989 0.4059 -0.0562 0.038 Uiso 1 1 calc R . . C10 C 0.1600(3) 0.47009(16) 0.0504(3) 0.0288(8) Uani 1 1 d . . . C11 C 0.2502(3) 0.52113(15) 0.0654(3) 0.0287(8) Uani 1 1 d . . . H11A H 0.2507 0.5420 0.1310 0.034 Uiso 1 1 calc R . . C12 C 0.0628(4) 0.44963(16) 0.1384(3) 0.0312(9) Uani 1 1 d . . . H12A H -0.0278 0.4331 0.1071 0.037 Uiso 1 1 calc R . . H12B H 0.0371 0.4861 0.1807 0.037 Uiso 1 1 calc R . . P2 P 0.13982(10) 0.39163(4) 0.22622(7) 0.0292(2) Uani 1 1 d . . . Se2 Se 0.35848(4) 0.404657(19) 0.27028(3) 0.04181(14) Uani 1 1 d . . . C13 C 0.0152(4) 0.38408(16) 0.3378(3) 0.0311(9) Uani 1 1 d . . . C14 C -0.1372(4) 0.3683(2) 0.2952(3) 0.0453(11) Uani 1 1 d . . . H14A H -0.2012 0.3597 0.3541 0.068 Uiso 1 1 calc R . . H14B H -0.1320 0.3320 0.2499 0.068 Uiso 1 1 calc R . . H14C H -0.1755 0.4031 0.2546 0.068 Uiso 1 1 calc R . . C15 C 0.0123(4) 0.44407(18) 0.3998(3) 0.0505(11) Uani 1 1 d . . . H15A H -0.0468 0.4387 0.4623 0.076 Uiso 1 1 calc R . . H15B H -0.0292 0.4767 0.3556 0.076 Uiso 1 1 calc R . . H15C H 0.1110 0.4553 0.4212 0.076 Uiso 1 1 calc R . . C16 C 0.0725(4) 0.33213(17) 0.4074(3) 0.0465(11) Uani 1 1 d . . . H16A H 0.0065 0.3256 0.4658 0.070 Uiso 1 1 calc R . . H16B H 0.1685 0.3431 0.4351 0.070 Uiso 1 1 calc R . . H16C H 0.0793 0.2943 0.3659 0.070 Uiso 1 1 calc R . . H2 H 0.116(3) 0.3391(16) 0.170(3) 0.046(10) Uiso 1 1 d . . . H1 H 0.386(3) 0.6709(14) -0.144(2) 0.034(9) 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 0.036(2) 0.023(2) 0.051(3) 0.0022(18) -0.0038(18) -0.0048(17) C2 0.067(3) 0.059(3) 0.054(3) -0.016(2) -0.010(2) -0.013(2) C3 0.042(3) 0.035(3) 0.108(4) -0.018(3) 0.004(2) -0.015(2) C4 0.063(3) 0.029(3) 0.080(3) -0.005(2) -0.003(2) -0.007(2) P1 0.0295(5) 0.0230(5) 0.0354(6) 0.0009(4) 0.0017(4) 0.0006(4) Se1 0.0311(2) 0.0328(2) 0.0430(2) 0.00061(18) 0.00540(17) 0.00563(17) C5 0.029(2) 0.027(2) 0.054(3) 0.0024(18) 0.0026(17) -0.0030(17) C6 0.0254(19) 0.0156(19) 0.038(2) 0.0078(17) 0.0002(16) 0.0070(15) C7 0.0257(19) 0.028(2) 0.038(2) 0.0069(17) 0.0100(16) 0.0028(16) C8 0.029(2) 0.028(2) 0.033(2) 0.0003(17) 0.0002(16) 0.0058(17) C9 0.027(2) 0.024(2) 0.042(2) 0.0064(18) -0.0024(17) -0.0029(16) C10 0.0246(19) 0.025(2) 0.037(2) 0.0092(17) 0.0018(16) 0.0018(16) C11 0.0270(19) 0.025(2) 0.033(2) 0.0006(16) -0.0031(16) 0.0059(16) C12 0.032(2) 0.028(2) 0.033(2) 0.0106(17) 0.0042(16) 0.0028(16) P2 0.0305(5) 0.0266(6) 0.0306(5) 0.0044(4) 0.0029(4) 0.0005(4) Se2 0.0304(2) 0.0503(3) 0.0445(3) 0.0106(2) -0.00318(17) -0.00381(18) C13 0.039(2) 0.027(2) 0.027(2) 0.0046(17) 0.0047(16) -0.0032(17) C14 0.040(2) 0.054(3) 0.042(2) 0.011(2) 0.0042(19) -0.010(2) C15 0.065(3) 0.043(3) 0.044(3) -0.007(2) 0.018(2) -0.004(2) C16 0.055(3) 0.038(2) 0.047(3) 0.013(2) 0.004(2) -0.005(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 C4 1.532(5) . ? C1 C3 1.533(5) . ? C1 C2 1.535(5) . ? C1 P1 1.851(4) . ? P1 C5 1.831(3) . ? P1 Se1 2.1186(10) . ? C5 C6 1.515(4) . ? C6 C11 1.388(4) . ? C6 C7 1.391(5) . ? C7 C8 1.377(5) . ? C8 C9 1.397(4) . ? C9 C10 1.374(5) . ? C10 C11 1.400(4) . ? C10 C12 1.515(4) . ? C12 P2 1.823(3) . ? P2 C13 1.851(3) . ? P2 Se2 2.1096(10) . ? C13 C15 1.525(5) . ? C13 C16 1.526(5) . ? C13 C14 1.541(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 C4 C1 C3 110.2(3) . . ? C4 C1 C2 109.9(3) . . ? C3 C1 C2 111.1(3) . . ? C4 C1 P1 107.3(3) . . ? C3 C1 P1 108.8(3) . . ? C2 C1 P1 109.5(3) . . ? C5 P1 C1 106.55(16) . . ? C5 P1 Se1 116.24(12) . . ? C1 P1 Se1 114.65(12) . . ? C6 C5 P1 115.1(2) . . ? C11 C6 C7 119.1(3) . . ? C11 C6 C5 119.6(3) . . ? C7 C6 C5 121.4(3) . . ? C8 C7 C6 120.3(3) . . ? C7 C8 C9 120.2(3) . . ? C10 C9 C8 120.5(3) . . ? C9 C10 C11 119.0(3) . . ? C9 C10 C12 121.6(3) . . ? C11 C10 C12 119.5(3) . . ? C6 C11 C10 121.0(3) . . ? C10 C12 P2 115.2(2) . . ? C12 P2 C13 106.84(16) . . ? C12 P2 Se2 115.70(12) . . ? C13 P2 Se2 114.48(12) . . ? C15 C13 C16 110.0(3) . . ? C15 C13 C14 110.4(3) . . ? C16 C13 C14 110.3(3) . . ? C15 C13 P2 109.7(2) . . ? C16 C13 P2 107.2(2) . . ? C14 C13 P2 109.1(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.647 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.076 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.026 0.000 0.000 411 155 ' ' 2 -0.008 0.500 0.500 411 155 ' ' _platon_squeeze_details ; The unit cell of the diselenide contained heavily disordered solvent molecules (either of isoelectronic pentane or diethyl ether) for which no suitable model could be found. The electron density associated with these molecules was removed from the reflection data using the program SQUEEZE (PLATON). After this treatment, two voids of ca. 411 A3 remained in the unit cell, each originally containing 155 electrons and corresponding to ca. two solvent molecules. Accordingly, two solvent molecule (arbitrarily selected to be pentane) are included in _chemical_formula_moiety (and _sum), and calculations of Mr, density, and F(OOO) to more accurately reflect the unit cell properties. ; _database_code_depnum_ccdc_archive 'CCDC 948786' ####################################################################### # # 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_(TrippPH)2C14H10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H58 P2, 0.5(C6 H6)' _chemical_formula_sum 'C47 H61 P2' _chemical_formula_weight 687.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 33.518(3) _cell_length_b 15.0365(13) _cell_length_c 16.5961(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.1550(10) _cell_angle_gamma 90.00 _cell_volume 8299.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4973 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 19.49 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 0.135 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9460 _exptl_absorpt_correction_T_max 0.9918 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 49571 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7324 _reflns_number_gt 4636 _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^)+(0.0501P)^2^+10.0450P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00039(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7324 _refine_ls_number_parameters 522 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.17877(2) 0.74287(5) 0.28931(5) 0.0460(2) Uani 1 1 d . . . P2 P 0.30617(2) 0.75323(5) 0.19218(6) 0.0593(3) Uani 1 1 d . . . C14 C 0.22172(7) 0.58301(16) 0.30588(15) 0.0351(6) Uani 1 1 d . . . C12 C 0.28770(7) 0.58556(16) 0.24838(14) 0.0345(6) Uani 1 1 d . . . C7 C 0.29659(8) 0.50104(16) 0.27984(16) 0.0383(6) Uani 1 1 d . A . C13 C 0.24430(7) 0.61578(17) 0.23813(16) 0.0408(6) Uani 1 1 d . A . H13A H 0.2307 0.5936 0.1856 0.049 Uiso 1 1 calc R . . H13B H 0.2434 0.6816 0.2367 0.049 Uiso 1 1 calc R . . C2 C 0.17224(8) 0.59899(17) 0.39776(16) 0.0414(6) Uani 1 1 d . . . H2 H 0.1518 0.6328 0.4183 0.050 Uiso 1 1 calc R . . C5 C 0.23133(7) 0.49878(16) 0.33781(16) 0.0385(6) Uani 1 1 d . A . C8 C 0.33600(8) 0.47101(17) 0.28929(16) 0.0434(7) Uani 1 1 d . . . H8 H 0.3420 0.4133 0.3107 0.052 Uiso 1 1 calc R A . C3 C 0.18186(8) 0.51563(18) 0.42980(16) 0.0444(7) Uani 1 1 d . A . H3 H 0.1680 0.4925 0.4718 0.053 Uiso 1 1 calc R . . C16 C 0.09941(8) 0.78409(18) 0.31122(17) 0.0455(7) Uani 1 1 d . . . C20 C 0.14889(8) 0.82033(18) 0.42580(16) 0.0427(6) Uani 1 1 d . . . C6 C 0.26255(8) 0.44445(17) 0.30164(19) 0.0501(7) Uani 1 1 d . . . H6A H 0.2733 0.3984 0.3411 0.060 Uiso 1 1 calc R A . H6B H 0.2497 0.4138 0.2523 0.060 Uiso 1 1 calc R . . C9 C 0.36646(8) 0.52415(18) 0.26797(17) 0.0475(7) Uani 1 1 d . A . H9 H 0.3934 0.5030 0.2744 0.057 Uiso 1 1 calc R . . C4 C 0.21156(8) 0.46634(17) 0.40051(16) 0.0431(7) Uani 1 1 d . . . H4 H 0.2186 0.4097 0.4234 0.052 Uiso 1 1 calc R A . C18 C 0.07803(8) 0.85157(18) 0.43189(17) 0.0458(7) Uani 1 1 d . . . C10 C 0.35775(8) 0.60841(17) 0.23716(16) 0.0437(7) Uani 1 1 d . . . H10 H 0.3789 0.6450 0.2228 0.052 Uiso 1 1 calc R A . C19 C 0.11793(8) 0.85333(19) 0.46607(17) 0.0481(7) Uani 1 1 d . B . H19 H 0.1244 0.8779 0.5188 0.058 Uiso 1 1 calc R . . C17 C 0.06987(8) 0.81677(19) 0.35479(18) 0.0504(7) Uani 1 1 d . B . H17 H 0.0427 0.8151 0.3303 0.060 Uiso 1 1 calc R . . C24 C 0.04337(9) 0.8831(2) 0.47543(19) 0.0585(8) Uani 1 1 d . B . H24 H 0.0238 0.9126 0.4334 0.070 Uiso 1 1 calc R . . C27 C 0.19181(8) 0.8259(2) 0.46816(18) 0.0608(9) Uani 1 1 d . B . H27 H 0.2085 0.7850 0.4386 0.073 Uiso 1 1 calc R . . C25 C 0.02142(10) 0.8038(3) 0.5068(2) 0.0861(12) Uani 1 1 d . . . H25A H 0.0390 0.7745 0.5506 0.129 Uiso 1 1 calc R B . H25B H 0.0143 0.7615 0.4624 0.129 Uiso 1 1 calc R . . H25C H -0.0031 0.8245 0.5277 0.129 Uiso 1 1 calc R . . C28 C 0.19616(10) 0.7957(3) 0.55622(19) 0.0849(12) Uani 1 1 d . . . H28A H 0.2246 0.7968 0.5787 0.127 Uiso 1 1 calc R B . H28B H 0.1858 0.7350 0.5591 0.127 Uiso 1 1 calc R . . H28C H 0.1809 0.8357 0.5876 0.127 Uiso 1 1 calc R . . C26 C 0.05449(11) 0.9509(3) 0.5402(2) 0.1013(15) Uani 1 1 d . . . H26A H 0.0733 0.9246 0.5837 0.152 Uiso 1 1 calc R B . H26B H 0.0302 0.9706 0.5625 0.152 Uiso 1 1 calc R . . H26C H 0.0672 1.0019 0.5170 0.152 Uiso 1 1 calc R . . C29 C 0.20820(12) 0.9189(3) 0.4604(3) 0.0999(14) Uani 1 1 d . . . H29A H 0.1926 0.9609 0.4891 0.150 Uiso 1 1 calc R B . H29B H 0.2061 0.9353 0.4029 0.150 Uiso 1 1 calc R . . H29C H 0.2365 0.9207 0.4841 0.150 Uiso 1 1 calc R . . C1 C 0.19197(7) 0.63443(16) 0.33591(14) 0.0340(6) Uani 1 1 d . . . C11 C 0.31848(7) 0.64035(16) 0.22693(14) 0.0354(6) Uani 1 1 d . A . C15 C 0.13980(7) 0.78528(17) 0.34736(15) 0.0375(6) Uani 1 1 d . B . C30 C 0.35495(15) 0.7961(4) 0.1648(3) 0.048(3) Uani 0.734(9) 1 d PG A 1 C31 C 0.36492(14) 0.7790(4) 0.0875(3) 0.0412(14) Uani 0.734(9) 1 d PG A 1 C32 C 0.39690(13) 0.8236(4) 0.0598(2) 0.0548(14) Uani 0.734(9) 1 d PG A 1 H32 H 0.4037 0.8119 0.0069 0.066 Uiso 0.734(9) 1 calc PR A 1 C33 C 0.41892(10) 0.8853(3) 0.1094(3) 0.0471(12) Uani 0.734(9) 1 d PG A 1 C34 C 0.40895(11) 0.9024(3) 0.1868(3) 0.0440(11) Uani 0.734(9) 1 d PG A 1 H34 H 0.4240 0.9445 0.2207 0.053 Uiso 0.734(9) 1 calc PR A 1 C35 C 0.37697(15) 0.8578(4) 0.2145(2) 0.0419(14) Uani 0.734(9) 1 d PG A 1 C36 C 0.36741(17) 0.8783(5) 0.3016(3) 0.0622(17) Uani 0.734(9) 1 d P A 1 H36 H 0.3390 0.8587 0.3029 0.075 Uiso 0.734(9) 1 calc PR A 1 C37 C 0.3927(2) 0.8214(4) 0.3647(4) 0.0724(18) Uani 0.734(9) 1 d P A 1 H37A H 0.3896 0.7585 0.3496 0.109 Uiso 0.734(9) 1 calc PR A 1 H37B H 0.3837 0.8306 0.4181 0.109 Uiso 0.734(9) 1 calc PR A 1 H37C H 0.4211 0.8383 0.3670 0.109 Uiso 0.734(9) 1 calc PR A 1 C38 C 0.3683(3) 0.9768(5) 0.3248(4) 0.108(3) Uani 0.734(9) 1 d P A 1 H38A H 0.3562 0.9847 0.3751 0.162 Uiso 0.734(9) 1 calc PR A 1 H38B H 0.3531 1.0112 0.2811 0.162 Uiso 0.734(9) 1 calc PR A 1 H38C H 0.3962 0.9977 0.3329 0.162 Uiso 0.734(9) 1 calc PR A 1 C39 C 0.3433(3) 0.7111(7) 0.0306(6) 0.064(2) Uani 0.734(9) 1 d P A 1 H39 H 0.3214 0.6830 0.0576 0.077 Uiso 0.734(9) 1 calc PR A 1 C40 C 0.3236(7) 0.7674(15) -0.0466(9) 0.116(7) Uani 0.734(9) 1 d P A 1 H40A H 0.3448 0.7987 -0.0709 0.174 Uiso 0.734(9) 1 calc PR A 1 H40B H 0.3046 0.8109 -0.0292 0.174 Uiso 0.734(9) 1 calc PR A 1 H40C H 0.3093 0.7271 -0.0868 0.174 Uiso 0.734(9) 1 calc PR A 1 C41 C 0.3712(3) 0.6397(5) 0.0074(5) 0.084(2) Uani 0.734(9) 1 d P A 1 H41A H 0.3917 0.6664 -0.0223 0.126 Uiso 0.734(9) 1 calc PR A 1 H41B H 0.3559 0.5955 -0.0271 0.126 Uiso 0.734(9) 1 calc PR A 1 H41C H 0.3843 0.6107 0.0566 0.126 Uiso 0.734(9) 1 calc PR A 1 C42 C 0.45221(14) 0.9401(3) 0.0781(4) 0.0612(16) Uani 0.734(9) 1 d P A 1 H42 H 0.4575 0.9133 0.0253 0.073 Uiso 0.734(9) 1 calc PR A 1 C43 C 0.49082(14) 0.9433(5) 0.1312(5) 0.099(3) Uani 0.734(9) 1 d P A 1 H43A H 0.4870 0.9729 0.1823 0.148 Uiso 0.734(9) 1 calc PR A 1 H43B H 0.5105 0.9766 0.1041 0.148 Uiso 0.734(9) 1 calc PR A 1 H43C H 0.5007 0.8827 0.1425 0.148 Uiso 0.734(9) 1 calc PR A 1 C44 C 0.43758(19) 1.0390(4) 0.0601(5) 0.074(2) Uani 0.734(9) 1 d P A 1 H44A H 0.4159 1.0394 0.0147 0.111 Uiso 0.734(9) 1 calc PR A 1 H44B H 0.4601 1.0749 0.0461 0.111 Uiso 0.734(9) 1 calc PR A 1 H44C H 0.4277 1.0639 0.1085 0.111 Uiso 0.734(9) 1 calc PR A 1 C21 C 0.08783(17) 0.7540(5) 0.2226(4) 0.0460(15) Uani 0.708(16) 1 d P B 1 H21 H 0.1128 0.7554 0.1952 0.055 Uiso 0.708(16) 1 calc PR B 1 C22 C 0.0745(4) 0.6567(4) 0.2265(5) 0.119(5) Uani 0.708(16) 1 d P B 1 H22A H 0.0520 0.6524 0.2586 0.179 Uiso 0.708(16) 1 calc PR B 1 H22B H 0.0970 0.6206 0.2519 0.179 Uiso 0.708(16) 1 calc PR B 1 H22C H 0.0661 0.6348 0.1714 0.179 Uiso 0.708(16) 1 calc PR B 1 C23 C 0.0569(2) 0.8117(5) 0.1741(3) 0.0639(18) Uani 0.708(16) 1 d P B 1 H23A H 0.0517 0.7889 0.1184 0.096 Uiso 0.708(16) 1 calc PR B 1 H23B H 0.0670 0.8728 0.1730 0.096 Uiso 0.708(16) 1 calc PR B 1 H23C H 0.0320 0.8109 0.1991 0.096 Uiso 0.708(16) 1 calc PR B 1 C30B C 0.3509(4) 0.8028(11) 0.1642(7) 0.011(3) Uiso 0.266(9) 1 d PG A 2 C31B C 0.3655(4) 0.7988(10) 0.0894(6) 0.049(5) Uiso 0.266(9) 1 d PG A 2 C32B C 0.3995(4) 0.8472(8) 0.0766(6) 0.031(3) Uiso 0.266(9) 1 d PG A 2 H32B H 0.4094 0.8445 0.0255 0.038 Uiso 0.266(9) 1 calc PR A 2 C33B C 0.4188(3) 0.8997(7) 0.1384(8) 0.039(4) Uiso 0.266(9) 1 d PG A 2 C34B C 0.4043(4) 0.9037(8) 0.2132(7) 0.048(4) Uiso 0.266(9) 1 d PG A 2 H34B H 0.4175 0.9395 0.2555 0.058 Uiso 0.266(9) 1 calc PR A 2 C35B C 0.3703(4) 0.8553(10) 0.2260(6) 0.037(4) Uiso 0.266(9) 1 d PG A 2 C36B C 0.3623(5) 0.8468(11) 0.3123(11) 0.048(5) Uiso 0.266(9) 1 d P A 2 H36B H 0.3441 0.7962 0.3219 0.058 Uiso 0.266(9) 1 calc PR A 2 C37B C 0.4072(5) 0.8398(14) 0.3642(13) 0.064(6) Uiso 0.266(9) 1 d P A 2 H37D H 0.4215 0.7886 0.3451 0.096 Uiso 0.266(9) 1 calc PR A 2 H37E H 0.4046 0.8324 0.4220 0.096 Uiso 0.266(9) 1 calc PR A 2 H37F H 0.4223 0.8943 0.3565 0.096 Uiso 0.266(9) 1 calc PR A 2 C38B C 0.3459(5) 0.9370(10) 0.3315(10) 0.059(4) Uiso 0.266(9) 1 d P A 2 H38D H 0.3658 0.9830 0.3240 0.089 Uiso 0.266(9) 1 calc PR A 2 H38E H 0.3401 0.9377 0.3880 0.089 Uiso 0.266(9) 1 calc PR A 2 H38F H 0.3211 0.9486 0.2952 0.089 Uiso 0.266(9) 1 calc PR A 2 C39B C 0.3486(9) 0.7322(19) 0.022(2) 0.064(8) Uiso 0.266(9) 1 d P A 2 H39B H 0.3330 0.6919 0.0549 0.077 Uiso 0.266(9) 1 calc PR A 2 C40B C 0.3190(19) 0.751(4) -0.042(3) 0.095(10) Uiso 0.266(9) 1 d P A 2 H40D H 0.2980 0.7880 -0.0226 0.142 Uiso 0.266(9) 1 calc PR A 2 H40E H 0.3072 0.6958 -0.0648 0.142 Uiso 0.266(9) 1 calc PR A 2 H40F H 0.3311 0.7838 -0.0842 0.142 Uiso 0.266(9) 1 calc PR A 2 C41B C 0.3795(8) 0.6646(16) -0.0052(17) 0.084(8) Uiso 0.266(9) 1 d P A 2 H41D H 0.3653 0.6209 -0.0422 0.125 Uiso 0.266(9) 1 calc PR A 2 H41E H 0.3933 0.6340 0.0425 0.125 Uiso 0.266(9) 1 calc PR A 2 H41F H 0.3992 0.6964 -0.0332 0.125 Uiso 0.266(9) 1 calc PR A 2 C42B C 0.4534(4) 0.9642(9) 0.1248(10) 0.057(4) Uiso 0.266(9) 1 d P A 2 H42B H 0.4651 1.0029 0.1709 0.069 Uiso 0.266(9) 1 calc PR A 2 C43B C 0.4830(6) 0.9080(13) 0.0779(13) 0.097(6) Uiso 0.266(9) 1 d P A 2 H43D H 0.4919 0.8552 0.1099 0.145 Uiso 0.266(9) 1 calc PR A 2 H43E H 0.5064 0.9444 0.0696 0.145 Uiso 0.266(9) 1 calc PR A 2 H43F H 0.4691 0.8896 0.0251 0.145 Uiso 0.266(9) 1 calc PR A 2 C44B C 0.4386(6) 1.0117(14) 0.0343(12) 0.060(6) Uiso 0.266(9) 1 d P A 2 H44D H 0.4611 1.0447 0.0163 0.090 Uiso 0.266(9) 1 calc PR A 2 H44E H 0.4163 1.0526 0.0395 0.090 Uiso 0.266(9) 1 calc PR A 2 H44F H 0.4297 0.9655 -0.0056 0.090 Uiso 0.266(9) 1 calc PR A 2 C21B C 0.0837(5) 0.7242(12) 0.2386(10) 0.044(4) Uiso 0.292(16) 1 d P B 2 H21B H 0.1064 0.6864 0.2246 0.053 Uiso 0.292(16) 1 calc PR B 2 C22B C 0.0477(5) 0.6683(10) 0.2367(8) 0.064(4) Uiso 0.292(16) 1 d P B 2 H22D H 0.0520 0.6233 0.2796 0.096 Uiso 0.292(16) 1 calc PR B 2 H22E H 0.0425 0.6389 0.1838 0.096 Uiso 0.292(16) 1 calc PR B 2 H22F H 0.0246 0.7054 0.2455 0.096 Uiso 0.292(16) 1 calc PR B 2 C23B C 0.0741(7) 0.7948(12) 0.1712(12) 0.078(6) Uiso 0.292(16) 1 d P B 2 H23D H 0.0543 0.8371 0.1875 0.117 Uiso 0.292(16) 1 calc PR B 2 H23E H 0.0631 0.7654 0.1206 0.117 Uiso 0.292(16) 1 calc PR B 2 H23F H 0.0987 0.8266 0.1629 0.117 Uiso 0.292(16) 1 calc PR B 2 C1A C 0.0000 0.0254(3) 0.2500 0.0757(15) Uani 1 2 d S . . H1S H 0.0000 -0.0377 0.2500 0.091 Uiso 1 2 calc SR . . C3S C 0.03055(10) 0.1616(3) 0.2940(2) 0.0722(10) Uani 1 1 d . . . H3S H 0.0517 0.1935 0.3247 0.087 Uiso 1 1 calc R . . C2S C 0.03076(10) 0.0713(3) 0.2942(2) 0.0726(10) Uani 1 1 d . . . H2S H 0.0521 0.0399 0.3249 0.087 Uiso 1 1 calc R . . C4S C 0.0000 0.2065(3) 0.2500 0.0761(14) Uani 1 2 d S . . H4S H 0.0000 0.2697 0.2500 0.091 Uiso 1 2 calc SR . . H1P H 0.2099(9) 0.7867(19) 0.3172(17) 0.071(9) Uiso 1 1 d . . . H2P H 0.2863(11) 0.737(2) 0.130(2) 0.102(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0403(4) 0.0476(4) 0.0536(4) 0.0069(4) 0.0191(3) 0.0108(3) P2 0.0369(4) 0.0440(4) 0.1006(7) 0.0270(5) 0.0234(4) 0.0077(4) C14 0.0277(13) 0.0366(14) 0.0416(15) -0.0041(11) 0.0068(11) -0.0051(11) C12 0.0323(14) 0.0354(14) 0.0366(14) -0.0043(11) 0.0074(11) 0.0038(11) C7 0.0378(15) 0.0331(13) 0.0461(16) -0.0022(12) 0.0130(12) 0.0000(11) C13 0.0333(14) 0.0415(15) 0.0496(16) 0.0055(12) 0.0125(12) 0.0022(12) C2 0.0360(15) 0.0441(16) 0.0457(16) -0.0066(13) 0.0116(12) -0.0032(12) C5 0.0313(14) 0.0347(14) 0.0499(16) -0.0014(12) 0.0070(12) -0.0053(11) C8 0.0421(16) 0.0336(14) 0.0554(17) 0.0049(12) 0.0102(13) 0.0061(12) C3 0.0431(16) 0.0463(17) 0.0462(16) 0.0006(13) 0.0148(13) -0.0102(13) C16 0.0347(15) 0.0495(16) 0.0511(17) -0.0076(13) 0.0010(13) 0.0074(12) C20 0.0319(14) 0.0506(16) 0.0464(16) -0.0077(13) 0.0080(12) -0.0030(12) C6 0.0446(17) 0.0359(15) 0.073(2) 0.0016(14) 0.0211(15) 0.0006(12) C9 0.0357(15) 0.0443(16) 0.0634(19) 0.0068(14) 0.0097(13) 0.0092(13) C4 0.0439(16) 0.0347(14) 0.0508(17) 0.0030(13) 0.0063(13) -0.0079(12) C18 0.0373(16) 0.0473(16) 0.0548(18) -0.0040(14) 0.0135(13) 0.0050(13) C10 0.0342(15) 0.0413(16) 0.0576(18) 0.0066(13) 0.0137(13) 0.0034(12) C19 0.0464(17) 0.0539(18) 0.0453(16) -0.0099(13) 0.0101(13) -0.0018(14) C17 0.0302(15) 0.0571(18) 0.0630(19) -0.0074(15) 0.0030(13) 0.0093(13) C24 0.0495(18) 0.069(2) 0.061(2) 0.0006(16) 0.0206(15) 0.0170(16) C27 0.0378(17) 0.092(2) 0.0532(19) -0.0247(17) 0.0094(14) -0.0080(16) C25 0.061(2) 0.115(3) 0.089(3) 0.021(2) 0.035(2) 0.015(2) C28 0.050(2) 0.146(4) 0.056(2) -0.019(2) -0.0071(17) 0.007(2) C26 0.065(2) 0.139(4) 0.104(3) -0.065(3) 0.026(2) 0.013(2) C29 0.072(3) 0.122(4) 0.104(3) -0.023(3) 0.005(2) -0.046(2) C1 0.0279(13) 0.0373(14) 0.0368(14) -0.0059(11) 0.0044(11) -0.0046(11) C11 0.0349(14) 0.0367(14) 0.0356(14) -0.0021(11) 0.0082(11) 0.0035(11) C15 0.0316(14) 0.0389(14) 0.0429(15) -0.0022(12) 0.0077(11) 0.0016(11) C30 0.043(4) 0.043(4) 0.059(4) 0.016(2) 0.012(2) 0.007(2) C31 0.042(3) 0.038(3) 0.046(3) 0.0021(18) 0.0151(19) 0.0032(19) C32 0.060(3) 0.057(4) 0.051(3) -0.010(3) 0.024(2) -0.007(2) C33 0.043(3) 0.056(3) 0.045(3) 0.009(3) 0.014(2) -0.002(2) C34 0.034(2) 0.046(3) 0.051(3) -0.006(2) 0.002(2) -0.0036(17) C35 0.031(3) 0.051(3) 0.045(3) 0.003(2) 0.0072(19) 0.005(2) C36 0.049(3) 0.091(5) 0.045(3) -0.007(3) -0.001(2) -0.021(3) C37 0.092(5) 0.065(4) 0.057(3) 0.012(3) -0.005(3) -0.029(4) C38 0.148(7) 0.102(6) 0.066(4) -0.021(4) -0.013(4) 0.066(5) C39 0.066(4) 0.074(5) 0.056(4) -0.025(4) 0.020(3) -0.016(4) C40 0.134(11) 0.138(13) 0.063(5) -0.055(7) -0.035(6) 0.040(9) C41 0.105(5) 0.062(4) 0.094(5) -0.022(4) 0.042(4) -0.009(4) C42 0.050(3) 0.067(3) 0.070(4) 0.006(3) 0.023(3) -0.014(2) C43 0.032(3) 0.132(6) 0.133(6) 0.068(5) 0.012(3) -0.012(3) C44 0.064(4) 0.057(4) 0.103(6) 0.027(4) 0.026(4) -0.007(3) C21 0.037(3) 0.052(4) 0.048(3) 0.002(3) -0.002(2) 0.003(3) C22 0.186(13) 0.055(4) 0.101(5) -0.023(3) -0.044(6) -0.005(5) C23 0.049(4) 0.086(4) 0.053(3) 0.000(3) -0.007(3) 0.005(3) C1A 0.087(4) 0.055(3) 0.095(4) 0.000 0.052(3) 0.000 C3S 0.056(2) 0.089(3) 0.073(2) -0.013(2) 0.0158(18) -0.014(2) C2S 0.058(2) 0.092(3) 0.072(2) 0.015(2) 0.0253(18) 0.016(2) C4S 0.082(4) 0.060(3) 0.092(4) 0.000 0.030(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C15 1.832(2) . ? P1 C1 1.835(3) . ? P1 H1P 1.27(3) . ? P2 C30B 1.788(9) . ? P2 C11 1.823(3) . ? P2 C30 1.866(3) . ? P2 H2P 1.18(4) . ? C14 C5 1.395(3) . ? C14 C1 1.402(3) . ? C14 C13 1.514(3) . ? C12 C7 1.392(3) . ? C12 C11 1.400(3) . ? C12 C13 1.513(3) . ? C7 C8 1.386(3) . ? C7 C6 1.503(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C2 C3 1.384(4) . ? C2 C1 1.394(3) . ? C2 H2 0.9500 . ? C5 C4 1.390(3) . ? C5 C6 1.510(3) . ? C8 C9 1.377(4) . ? C8 H8 0.9500 . ? C3 C4 1.377(4) . ? C3 H3 0.9500 . ? C16 C17 1.387(4) . ? C16 C15 1.411(3) . ? C16 C21 1.541(6) . ? C16 C21B 1.543(17) . ? C20 C19 1.394(3) . ? C20 C15 1.402(3) . ? C20 C27 1.523(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C9 C10 1.384(4) . ? C9 H9 0.9500 . ? C4 H4 0.9500 . ? C18 C17 1.378(4) . ? C18 C19 1.386(4) . ? C18 C24 1.518(4) . ? C10 C11 1.391(3) . ? C10 H10 0.9500 . ? C19 H19 0.9500 . ? C17 H17 0.9500 . ? C24 C26 1.495(4) . ? C24 C25 1.526(5) . ? C24 H24 1.0000 . ? C27 C29 1.514(5) . ? C27 C28 1.520(4) . ? C27 H27 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C31 C32 1.3900 . ? C31 C39 1.513(10) . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 C34 1.3900 . ? C33 C42 1.529(5) . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 C36 1.551(6) . ? C36 C37 1.526(8) . ? C36 C38 1.530(9) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.507(12) . ? C39 C40 1.61(2) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.473(9) . ? C42 C44 1.583(8) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C21 C23 1.505(8) . ? C21 C22 1.534(9) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C30B C31B 1.3900 . ? C30B C35B 1.3900 . ? C31B C32B 1.3900 . ? C31B C39B 1.55(3) . ? C32B C33B 1.3900 . ? C32B H32B 0.9500 . ? C33B C34B 1.3900 . ? C33B C42B 1.550(15) . ? C34B C35B 1.3900 . ? C34B H34B 0.9500 . ? C35B C36B 1.49(2) . ? C36B C38B 1.51(2) . ? C36B C37B 1.64(2) . ? C36B H36B 1.0000 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? C39B C40B 1.39(6) . ? C39B C41B 1.56(4) . ? C39B H39B 1.0000 . ? C40B H40D 0.9800 . ? C40B H40E 0.9800 . ? C40B H40F 0.9800 . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? C42B C43B 1.58(3) . ? C42B C44B 1.68(3) . ? C42B H42B 1.0000 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C44B H44D 0.9800 . ? C44B H44E 0.9800 . ? C44B H44F 0.9800 . ? C21B C22B 1.47(2) . ? C21B C23B 1.55(2) . ? C21B H21B 1.0000 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C1A C2S 1.375(4) . ? C1A C2S 1.375(4) 2 ? C1A H1S 0.9500 . ? C3S C2S 1.358(5) . ? C3S C4S 1.361(4) . ? C3S H3S 0.9500 . ? C2S H2S 0.9500 . ? C4S C3S 1.361(4) 2 ? C4S H4S 0.9500 . ? 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 C15 P1 C1 103.77(11) . . ? C15 P1 H1P 103.6(13) . . ? C1 P1 H1P 99.4(13) . . ? C30B P2 C11 107.8(7) . . ? C30B P2 C30 4.6(9) . . ? C11 P2 C30 103.2(2) . . ? C30B P2 H2P 105.1(17) . . ? C11 P2 H2P 99.4(17) . . ? C30 P2 H2P 106.0(17) . . ? C5 C14 C1 120.4(2) . . ? C5 C14 C13 117.7(2) . . ? C1 C14 C13 121.9(2) . . ? C7 C12 C11 120.2(2) . . ? C7 C12 C13 118.3(2) . . ? C11 C12 C13 121.5(2) . . ? C8 C7 C12 119.8(2) . . ? C8 C7 C6 122.0(2) . . ? C12 C7 C6 118.3(2) . . ? C12 C13 C14 112.4(2) . . ? C12 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.9 . . ? C3 C2 C1 121.3(2) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C4 C5 C14 119.6(2) . . ? C4 C5 C6 121.8(2) . . ? C14 C5 C6 118.6(2) . . ? C9 C8 C7 120.6(2) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C4 C3 C2 119.7(2) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C17 C16 C15 118.9(2) . . ? C17 C16 C21 119.4(3) . . ? C15 C16 C21 121.6(3) . . ? C17 C16 C21B 114.6(6) . . ? C15 C16 C21B 123.8(6) . . ? C21 C16 C21B 20.5(5) . . ? C19 C20 C15 119.3(2) . . ? C19 C20 C27 118.4(2) . . ? C15 C20 C27 122.2(2) . . ? C7 C6 C5 111.9(2) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C9 C10 119.8(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C3 C4 C5 120.6(2) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C17 C18 C19 117.2(2) . . ? C17 C18 C24 119.0(2) . . ? C19 C18 C24 123.8(3) . . ? C9 C10 C11 120.9(2) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C18 C19 C20 122.3(3) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C18 C17 C16 123.1(3) . . ? C18 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C26 C24 C18 114.7(3) . . ? C26 C24 C25 112.0(3) . . ? C18 C24 C25 110.4(3) . . ? C26 C24 H24 106.4 . . ? C18 C24 H24 106.4 . . ? C25 C24 H24 106.4 . . ? C29 C27 C28 111.5(3) . . ? C29 C27 C20 110.1(3) . . ? C28 C27 C20 113.5(2) . . ? C29 C27 H27 107.1 . . ? C28 C27 H27 107.1 . . ? C20 C27 H27 107.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C2 C1 C14 118.3(2) . . ? C2 C1 P1 122.57(19) . . ? C14 C1 P1 119.02(18) . . ? C10 C11 C12 118.8(2) . . ? C10 C11 P2 122.23(19) . . ? C12 C11 P2 118.89(18) . . ? C20 C15 C16 119.1(2) . . ? C20 C15 P1 122.16(19) . . ? C16 C15 P1 118.77(19) . . ? C31 C30 C35 120.0 . . ? C31 C30 P2 118.7(3) . . ? C35 C30 P2 120.2(3) . . ? C32 C31 C30 120.0 . . ? C32 C31 C39 116.7(4) . . ? C30 C31 C39 123.3(5) . . ? C31 C32 C33 120.0 . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 C42 118.9(3) . . ? C32 C33 C42 120.9(3) . . ? C33 C34 C35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C30 120.0 . . ? C34 C35 C36 118.0(3) . . ? C30 C35 C36 122.0(3) . . ? C37 C36 C38 112.3(5) . . ? C37 C36 C35 111.5(5) . . ? C38 C36 C35 115.3(5) . . ? C37 C36 H36 105.6 . . ? C38 C36 H36 105.6 . . ? C35 C36 H36 105.6 . . ? C41 C39 C31 112.0(7) . . ? C41 C39 C40 112.3(9) . . ? C31 C39 C40 105.0(9) . . ? C41 C39 H39 109.1 . . ? C31 C39 H39 109.1 . . ? C40 C39 H39 109.1 . . ? C43 C42 C33 116.0(4) . . ? C43 C42 C44 108.1(6) . . ? C33 C42 C44 110.4(4) . . ? C43 C42 H42 107.4 . . ? C33 C42 H42 107.4 . . ? C44 C42 H42 107.4 . . ? C23 C21 C22 112.8(5) . . ? C23 C21 C16 114.6(4) . . ? C22 C21 C16 106.3(6) . . ? C23 C21 H21 107.6 . . ? C22 C21 H21 107.6 . . ? C16 C21 H21 107.6 . . ? C31B C30B C35B 120.0 . . ? C31B C30B P2 127.9(6) . . ? C35B C30B P2 112.0(6) . . ? C32B C31B C30B 120.0 . . ? C32B C31B C39B 117.5(12) . . ? C30B C31B C39B 122.0(12) . . ? C31B C32B C33B 120.0 . . ? C31B C32B H32B 120.0 . . ? C33B C32B H32B 120.0 . . ? C32B C33B C34B 120.0 . . ? C32B C33B C42B 122.5(9) . . ? C34B C33B C42B 117.1(9) . . ? C35B C34B C33B 120.0 . . ? C35B C34B H34B 120.0 . . ? C33B C34B H34B 120.0 . . ? C34B C35B C30B 120.0 . . ? C34B C35B C36B 116.1(10) . . ? C30B C35B C36B 122.4(10) . . ? C35B C36B C38B 103.9(13) . . ? C35B C36B C37B 104.2(14) . . ? C38B C36B C37B 106.3(14) . . ? C35B C36B H36B 113.8 . . ? C38B C36B H36B 113.8 . . ? C37B C36B H36B 113.8 . . ? C36B C37B H37D 109.5 . . ? C36B C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? C36B C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? C36B C38B H38D 109.5 . . ? C36B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C36B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C40B C39B C31B 125(3) . . ? C40B C39B C41B 110(3) . . ? C31B C39B C41B 116(2) . . ? C40B C39B H39B 99.9 . . ? C31B C39B H39B 99.9 . . ? C41B C39B H39B 99.9 . . ? C39B C40B H40D 109.5 . . ? C39B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C39B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C39B C41B H41D 109.5 . . ? C39B C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? C39B C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? C33B C42B C43B 105.3(13) . . ? C33B C42B C44B 104.6(12) . . ? C43B C42B C44B 85.5(15) . . ? C33B C42B H42B 118.7 . . ? C43B C42B H42B 118.7 . . ? C44B C42B H42B 118.7 . . ? C42B C43B H43D 109.5 . . ? C42B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C42B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C42B C44B H44D 109.5 . . ? C42B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C42B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? C22B C21B C16 123.5(12) . . ? C22B C21B C23B 106.3(12) . . ? C16 C21B C23B 100.6(13) . . ? C22B C21B H21B 108.5 . . ? C16 C21B H21B 108.5 . . ? C23B C21B H21B 108.5 . . ? C21B C22B H22D 109.5 . . ? C21B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C21B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C21B C23B H23D 109.5 . . ? C21B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C21B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C2S C1A C2S 119.7(5) . 2 ? C2S C1A H1S 120.1 . . ? C2S C1A H1S 120.1 2 . ? C2S C3S C4S 120.0(4) . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C3S C2S C1A 119.8(4) . . ? C3S C2S H2S 120.1 . . ? C1A C2S H2S 120.1 . . ? C3S C4S C3S 120.6(5) . 2 ? C3S C4S H4S 119.7 . . ? C3S C4S H4S 119.7 2 . ? 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 C11 C12 C7 C8 -0.5(4) . . . . ? C13 C12 C7 C8 179.4(2) . . . . ? C11 C12 C7 C6 -179.7(2) . . . . ? C13 C12 C7 C6 0.2(4) . . . . ? C7 C12 C13 C14 36.6(3) . . . . ? C11 C12 C13 C14 -143.5(2) . . . . ? C5 C14 C13 C12 -35.6(3) . . . . ? C1 C14 C13 C12 144.7(2) . . . . ? C1 C14 C5 C4 -0.8(4) . . . . ? C13 C14 C5 C4 179.5(2) . . . . ? C1 C14 C5 C6 177.9(2) . . . . ? C13 C14 C5 C6 -1.8(3) . . . . ? C12 C7 C8 C9 0.1(4) . . . . ? C6 C7 C8 C9 179.3(3) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C8 C7 C6 C5 143.3(3) . . . . ? C12 C7 C6 C5 -37.4(4) . . . . ? C4 C5 C6 C7 -142.9(3) . . . . ? C14 C5 C6 C7 38.4(3) . . . . ? C7 C8 C9 C10 0.3(4) . . . . ? C2 C3 C4 C5 -1.4(4) . . . . ? C14 C5 C4 C3 1.8(4) . . . . ? C6 C5 C4 C3 -176.9(3) . . . . ? C8 C9 C10 C11 -0.3(4) . . . . ? C17 C18 C19 C20 -1.0(4) . . . . ? C24 C18 C19 C20 177.1(3) . . . . ? C15 C20 C19 C18 1.1(4) . . . . ? C27 C20 C19 C18 179.5(3) . . . . ? C19 C18 C17 C16 0.1(4) . . . . ? C24 C18 C17 C16 -178.2(3) . . . . ? C15 C16 C17 C18 0.8(4) . . . . ? C21 C16 C17 C18 -174.7(5) . . . . ? C21B C16 C17 C18 162.9(8) . . . . ? C17 C18 C24 C26 -156.2(3) . . . . ? C19 C18 C24 C26 25.6(5) . . . . ? C17 C18 C24 C25 76.1(4) . . . . ? C19 C18 C24 C25 -102.1(3) . . . . ? C19 C20 C27 C29 -79.4(3) . . . . ? C15 C20 C27 C29 99.0(3) . . . . ? C19 C20 C27 C28 46.3(4) . . . . ? C15 C20 C27 C28 -135.3(3) . . . . ? C3 C2 C1 C14 0.7(4) . . . . ? C3 C2 C1 P1 177.7(2) . . . . ? C5 C14 C1 C2 -0.4(3) . . . . ? C13 C14 C1 C2 179.3(2) . . . . ? C5 C14 C1 P1 -177.45(19) . . . . ? C13 C14 C1 P1 2.2(3) . . . . ? C15 P1 C1 C2 3.5(2) . . . . ? C15 P1 C1 C14 -179.62(19) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? C9 C10 C11 P2 176.3(2) . . . . ? C7 C12 C11 C10 0.4(4) . . . . ? C13 C12 C11 C10 -179.4(2) . . . . ? C7 C12 C11 P2 -176.04(19) . . . . ? C13 C12 C11 P2 4.1(3) . . . . ? C30B P2 C11 C10 7.0(4) . . . . ? C30 P2 C11 C10 7.3(3) . . . . ? C30B P2 C11 C12 -176.6(4) . . . . ? C30 P2 C11 C12 -176.4(2) . . . . ? C19 C20 C15 C16 -0.2(4) . . . . ? C27 C20 C15 C16 -178.6(3) . . . . ? C19 C20 C15 P1 178.6(2) . . . . ? C27 C20 C15 P1 0.2(4) . . . . ? C17 C16 C15 C20 -0.7(4) . . . . ? C21 C16 C15 C20 174.6(5) . . . . ? C21B C16 C15 C20 -161.1(8) . . . . ? C17 C16 C15 P1 -179.5(2) . . . . ? C21 C16 C15 P1 -4.2(5) . . . . ? C21B C16 C15 P1 20.1(9) . . . . ? C1 P1 C15 C20 76.1(2) . . . . ? C1 P1 C15 C16 -105.1(2) . . . . ? C30B P2 C30 C31 -97(6) . . . . ? C11 P2 C30 C31 85.9(3) . . . . ? C30B P2 C30 C35 71(6) . . . . ? C11 P2 C30 C35 -106.3(3) . . . . ? C35 C30 C31 C32 0.0 . . . . ? P2 C30 C31 C32 167.8(5) . . . . ? C35 C30 C31 C39 178.2(7) . . . . ? P2 C30 C31 C39 -14.0(6) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C39 C31 C32 C33 -178.3(7) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C31 C32 C33 C42 -175.5(4) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C42 C33 C34 C35 175.6(4) . . . . ? C33 C34 C35 C30 0.0 . . . . ? C33 C34 C35 C36 179.2(5) . . . . ? C31 C30 C35 C34 0.0 . . . . ? P2 C30 C35 C34 -167.6(5) . . . . ? C31 C30 C35 C36 -179.2(5) . . . . ? P2 C30 C35 C36 13.2(5) . . . . ? C34 C35 C36 C37 -85.8(7) . . . . ? C30 C35 C36 C37 93.4(6) . . . . ? C34 C35 C36 C38 43.8(7) . . . . ? C30 C35 C36 C38 -137.0(5) . . . . ? C32 C31 C39 C41 58.0(9) . . . . ? C30 C31 C39 C41 -120.3(7) . . . . ? C32 C31 C39 C40 -64.1(11) . . . . ? C30 C31 C39 C40 117.6(10) . . . . ? C34 C33 C42 C43 52.7(7) . . . . ? C32 C33 C42 C43 -131.8(6) . . . . ? C34 C33 C42 C44 -70.6(7) . . . . ? C32 C33 C42 C44 104.9(6) . . . . ? C17 C16 C21 C23 38.8(9) . . . . ? C15 C16 C21 C23 -136.5(5) . . . . ? C21B C16 C21 C23 121(2) . . . . ? C17 C16 C21 C22 -86.5(8) . . . . ? C15 C16 C21 C22 98.2(6) . . . . ? C21B C16 C21 C22 -4(2) . . . . ? C11 P2 C30B C31B 87.2(10) . . . . ? C30 P2 C30B C31B 84(6) . . . . ? C11 P2 C30B C35B -97.4(7) . . . . ? C30 P2 C30B C35B -101(6) . . . . ? C35B C30B C31B C32B 0.0 . . . . ? P2 C30B C31B C32B 175.1(15) . . . . ? C35B C30B C31B C39B 172(2) . . . . ? P2 C30B C31B C39B -13.1(19) . . . . ? C30B C31B C32B C33B 0.0 . . . . ? C39B C31B C32B C33B -172.2(18) . . . . ? C31B C32B C33B C34B 0.0 . . . . ? C31B C32B C33B C42B -172.1(12) . . . . ? C32B C33B C34B C35B 0.0 . . . . ? C42B C33B C34B C35B 172.5(12) . . . . ? C33B C34B C35B C30B 0.0 . . . . ? C33B C34B C35B C36B 166.5(15) . . . . ? C31B C30B C35B C34B 0.0 . . . . ? P2 C30B C35B C34B -175.8(13) . . . . ? C31B C30B C35B C36B -165.6(16) . . . . ? P2 C30B C35B C36B 18.5(13) . . . . ? C34B C35B C36B C38B 75.7(15) . . . . ? C30B C35B C36B C38B -118.2(12) . . . . ? C34B C35B C36B C37B -35.5(17) . . . . ? C30B C35B C36B C37B 130.7(13) . . . . ? C32B C31B C39B C40B -92(4) . . . . ? C30B C31B C39B C40B 96(4) . . . . ? C32B C31B C39B C41B 52(2) . . . . ? C30B C31B C39B C41B -119.8(18) . . . . ? C32B C33B C42B C43B -48.0(15) . . . . ? C34B C33B C42B C43B 139.7(13) . . . . ? C32B C33B C42B C44B 41.3(15) . . . . ? C34B C33B C42B C44B -131.0(12) . . . . ? C17 C16 C21B C22B -30.4(19) . . . . ? C15 C16 C21B C22B 130.7(14) . . . . ? C21 C16 C21B C22B -139(3) . . . . ? C17 C16 C21B C23B 87.4(15) . . . . ? C15 C16 C21B C23B -111.5(11) . . . . ? C21 C16 C21B C23B -20.9(17) . . . . ? C4S C3S C2S C1A -0.2(5) . . . . ? C2S C1A C2S C3S 0.1(2) 2 . . . ? C2S C3S C4S C3S 0.1(2) . . . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.325 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.042 _iucr_refine_instructions_details ; TITL PH09023 in C2/c CELL 0.71073 33.5179 15.0365 16.5961 90.000 97.155 90.000 ZERR 8.00 0.0029 0.0013 0.0015 0.000 0.001 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H P UNIT 376 488 16 L.S. 12 ACTA BOND $H FMAP 2 PLAN 5 mpla conf SIZE 0.061 0.104 0.416 TEMP -100 WGHT 0.050100 10.045000 EXTI 0.000395 FVAR 0.05254 0.73374 0.70826 MOLE 1 P1 3 0.178774 0.742867 0.289308 11.00000 0.04033 0.04756 = 0.05356 0.00693 0.01909 0.01083 P2 3 0.306169 0.753232 0.192183 11.00000 0.03691 0.04404 = 0.10062 0.02698 0.02342 0.00767 C14 1 0.221723 0.583015 0.305877 11.00000 0.02767 0.03662 = 0.04163 -0.00409 0.00685 -0.00513 C12 1 0.287704 0.585562 0.248382 11.00000 0.03229 0.03535 = 0.03656 -0.00425 0.00741 0.00375 C7 1 0.296590 0.501044 0.279836 11.00000 0.03777 0.03312 = 0.04606 -0.00217 0.01296 0.00000 C13 1 0.244304 0.615783 0.238131 11.00000 0.03327 0.04151 = 0.04962 0.00552 0.01254 0.00224 AFIX 23 H13A 2 0.230738 0.593605 0.185570 11.00000 -1.20000 H13B 2 0.243445 0.681582 0.236689 11.00000 -1.20000 AFIX 0 C2 1 0.172239 0.598995 0.397762 11.00000 0.03599 0.04409 = 0.04568 -0.00659 0.01165 -0.00316 AFIX 43 H2 2 0.151782 0.632752 0.418322 11.00000 -1.20000 AFIX 0 C5 1 0.231333 0.498777 0.337813 11.00000 0.03130 0.03472 = 0.04987 -0.00143 0.00699 -0.00533 C8 1 0.336004 0.471006 0.289293 11.00000 0.04215 0.03356 = 0.05539 0.00486 0.01016 0.00610 AFIX 43 H8 2 0.342047 0.413274 0.310664 11.00000 -1.20000 AFIX 0 C3 1 0.181859 0.515629 0.429803 11.00000 0.04315 0.04625 = 0.04618 0.00063 0.01476 -0.01021 AFIX 43 H3 2 0.168036 0.492496 0.471824 11.00000 -1.20000 AFIX 0 C16 1 0.099411 0.784092 0.311217 11.00000 0.03465 0.04947 = 0.05113 -0.00764 0.00097 0.00738 C20 1 0.148894 0.820328 0.425803 11.00000 0.03195 0.05062 = 0.04644 -0.00770 0.00799 -0.00298 C6 1 0.262549 0.444445 0.301636 11.00000 0.04465 0.03591 = 0.07324 0.00164 0.02109 0.00059 AFIX 23 H6A 2 0.273343 0.398424 0.341120 11.00000 -1.20000 H6B 2 0.249706 0.413807 0.252301 11.00000 -1.20000 AFIX 0 C9 1 0.366465 0.524153 0.267969 11.00000 0.03570 0.04430 = 0.06342 0.00679 0.00971 0.00917 AFIX 43 H9 2 0.393386 0.503032 0.274395 11.00000 -1.20000 AFIX 0 C4 1 0.211563 0.466338 0.400509 11.00000 0.04391 0.03469 = 0.05080 0.00302 0.00630 -0.00790 AFIX 43 H4 2 0.218593 0.409693 0.423356 11.00000 -1.20000 AFIX 0 C18 1 0.078030 0.851572 0.431894 11.00000 0.03725 0.04733 = 0.05482 -0.00401 0.01350 0.00501 C10 1 0.357747 0.608412 0.237156 11.00000 0.03419 0.04130 = 0.05756 0.00662 0.01372 0.00342 AFIX 43 H10 2 0.378872 0.644969 0.222778 11.00000 -1.20000 AFIX 0 C19 1 0.117934 0.853334 0.466071 11.00000 0.04637 0.05385 = 0.04526 -0.00991 0.01006 -0.00181 AFIX 43 H19 2 0.124403 0.877914 0.518813 11.00000 -1.20000 AFIX 0 C17 1 0.069871 0.816772 0.354794 11.00000 0.03022 0.05714 = 0.06298 -0.00737 0.00298 0.00930 AFIX 43 H17 2 0.042707 0.815086 0.330316 11.00000 -1.20000 AFIX 0 C24 1 0.043370 0.883058 0.475433 11.00000 0.04947 0.06863 = 0.06101 0.00060 0.02061 0.01702 AFIX 13 H24 2 0.023774 0.912569 0.433441 11.00000 -1.20000 AFIX 0 C27 1 0.191812 0.825900 0.468159 11.00000 0.03779 0.09220 = 0.05323 -0.02468 0.00943 -0.00798 AFIX 13 H27 2 0.208524 0.785022 0.438638 11.00000 -1.20000 AFIX 0 C25 1 0.021420 0.803785 0.506835 11.00000 0.06147 0.11457 = 0.08855 0.02092 0.03450 0.01505 AFIX 137 H25A 2 0.038973 0.774497 0.550563 11.00000 -1.50000 H25B 2 0.014259 0.761504 0.462449 11.00000 -1.50000 H25C 2 -0.003069 0.824451 0.527659 11.00000 -1.50000 AFIX 0 C28 1 0.196161 0.795655 0.556219 11.00000 0.05002 0.14553 = 0.05567 -0.01903 -0.00708 0.00678 AFIX 137 H28A 2 0.224611 0.796832 0.578729 11.00000 -1.50000 H28B 2 0.185762 0.734976 0.559100 11.00000 -1.50000 H28C 2 0.180916 0.835658 0.587598 11.00000 -1.50000 AFIX 0 C26 1 0.054492 0.950890 0.540237 11.00000 0.06488 0.13903 = 0.10379 -0.06470 0.02580 0.01338 AFIX 137 H26A 2 0.073296 0.924560 0.583670 11.00000 -1.50000 H26B 2 0.030231 0.970646 0.562469 11.00000 -1.50000 H26C 2 0.067238 1.001918 0.517041 11.00000 -1.50000 AFIX 0 C29 1 0.208201 0.918918 0.460368 11.00000 0.07243 0.12232 = 0.10359 -0.02291 0.00544 -0.04580 AFIX 137 H29A 2 0.192641 0.960940 0.489089 11.00000 -1.50000 H29B 2 0.206108 0.935348 0.402853 11.00000 -1.50000 H29C 2 0.236464 0.920672 0.484119 11.00000 -1.50000 AFIX 0 C1 1 0.191972 0.634432 0.335906 11.00000 0.02794 0.03728 = 0.03676 -0.00594 0.00441 -0.00459 C11 1 0.318482 0.640349 0.226933 11.00000 0.03493 0.03671 = 0.03560 -0.00215 0.00820 0.00354 C15 1 0.139795 0.785285 0.347364 11.00000 0.03161 0.03885 = 0.04293 -0.00217 0.00768 0.00158 PART 1 AFIX 66 C30 1 0.354955 0.796145 0.164822 21.00000 0.04263 0.04320 = 0.05853 0.01557 0.01199 0.00738 C31 1 0.364921 0.779045 0.087479 21.00000 0.04222 0.03813 = 0.04566 0.00215 0.01506 0.00320 C32 1 0.396901 0.823619 0.059791 21.00000 0.06017 0.05713 = 0.05147 -0.01039 0.02401 -0.00699 AFIX 43 H32 2 0.403712 0.811932 0.006931 21.00000 -1.20000 AFIX 65 C33 1 0.418916 0.885293 0.109445 21.00000 0.04268 0.05598 = 0.04472 0.00939 0.01416 -0.00209 C34 1 0.408950 0.902394 0.186788 21.00000 0.03364 0.04608 = 0.05141 -0.00589 0.00201 -0.00356 AFIX 43 H34 2 0.423996 0.944545 0.220724 21.00000 -1.20000 AFIX 65 C35 1 0.376970 0.857820 0.214477 21.00000 0.03091 0.05060 = 0.04467 0.00270 0.00721 0.00470 AFIX 0 C36 1 0.367406 0.878312 0.301609 21.00000 0.04877 0.09132 = 0.04491 -0.00693 -0.00068 -0.02061 AFIX 13 H36 2 0.338986 0.858686 0.302889 21.00000 -1.20000 AFIX 0 C37 1 0.392708 0.821351 0.364696 21.00000 0.09160 0.06523 = 0.05697 0.01176 -0.00478 -0.02899 AFIX 137 H37A 2 0.389585 0.758499 0.349595 21.00000 -1.50000 H37B 2 0.383737 0.830627 0.418056 21.00000 -1.50000 H37C 2 0.421053 0.838340 0.366961 21.00000 -1.50000 AFIX 0 C38 1 0.368298 0.976831 0.324767 21.00000 0.14841 0.10249 = 0.06597 -0.02103 -0.01259 0.06635 AFIX 137 H38A 2 0.356179 0.984673 0.375073 21.00000 -1.50000 H38B 2 0.353079 1.011231 0.281122 21.00000 -1.50000 H38C 2 0.396208 0.997702 0.332943 21.00000 -1.50000 AFIX 0 C39 1 0.343269 0.711109 0.030600 21.00000 0.06634 0.07448 = 0.05563 -0.02503 0.01999 -0.01566 AFIX 13 H39 2 0.321360 0.683000 0.057561 21.00000 -1.20000 AFIX 0 C40 1 0.323583 0.767442 -0.046616 21.00000 0.13443 0.13782 = 0.06326 -0.05535 -0.03463 0.03966 AFIX 137 H40A 2 0.344808 0.798666 -0.070900 21.00000 -1.50000 H40B 2 0.304594 0.810860 -0.029222 21.00000 -1.50000 H40C 2 0.309345 0.727139 -0.086798 21.00000 -1.50000 AFIX 0 C41 1 0.371249 0.639687 0.007435 21.00000 0.10454 0.06177 = 0.09395 -0.02167 0.04227 -0.00949 AFIX 137 H41A 2 0.391720 0.666412 -0.022313 21.00000 -1.50000 H41B 2 0.355882 0.595542 -0.027074 21.00000 -1.50000 H41C 2 0.384343 0.610653 0.056625 21.00000 -1.50000 AFIX 0 C42 1 0.452212 0.940056 0.078094 21.00000 0.05049 0.06747 = 0.06977 0.00630 0.02329 -0.01362 AFIX 13 H42 2 0.457526 0.913269 0.025318 21.00000 -1.20000 AFIX 0 C43 1 0.490816 0.943307 0.131180 21.00000 0.03212 0.13154 = 0.13320 0.06788 0.01235 -0.01165 AFIX 137 H43A 2 0.487005 0.972868 0.182291 21.00000 -1.50000 H43B 2 0.510476 0.976566 0.104082 21.00000 -1.50000 H43C 2 0.500655 0.882652 0.142491 21.00000 -1.50000 AFIX 0 C44 1 0.437576 1.038995 0.060121 21.00000 0.06424 0.05743 = 0.10334 0.02730 0.02596 -0.00721 AFIX 137 H44A 2 0.415886 1.039385 0.014694 21.00000 -1.50000 H44B 2 0.460101 1.074944 0.046071 21.00000 -1.50000 H44C 2 0.427682 1.063900 0.108471 21.00000 -1.50000 AFIX 0 C21 1 0.087835 0.754040 0.222608 31.00000 0.03667 0.05172 = 0.04768 0.00162 -0.00214 0.00295 AFIX 13 H21 2 0.112759 0.755430 0.195196 31.00000 -1.20000 AFIX 0 C22 1 0.074528 0.656667 0.226476 31.00000 0.18571 0.05489 = 0.10127 -0.02324 -0.04397 -0.00539 AFIX 137 H22A 2 0.051989 0.652385 0.258646 31.00000 -1.50000 H22B 2 0.097023 0.620647 0.251878 31.00000 -1.50000 H22C 2 0.066073 0.634773 0.171375 31.00000 -1.50000 AFIX 0 C23 1 0.056937 0.811679 0.174072 31.00000 0.04920 0.08641 = 0.05278 -0.00028 -0.00696 0.00458 AFIX 137 H23A 2 0.051693 0.788863 0.118447 31.00000 -1.50000 H23B 2 0.067032 0.872783 0.173026 31.00000 -1.50000 H23C 2 0.031966 0.810928 0.199137 31.00000 -1.50000 PART 2 AFIX 66 C30B 1 0.350931 0.802799 0.164167 -21.00000 0.01127 C31B 1 0.365512 0.798776 0.089428 -21.00000 0.04937 C32B 1 0.399472 0.847206 0.076557 -21.00000 0.03148 AFIX 43 H32B 2 0.409437 0.844456 0.025476 -21.00000 -1.20000 AFIX 65 C33B 1 0.418850 0.899658 0.138426 -21.00000 0.03944 C34B 1 0.404269 0.903682 0.213166 -21.00000 0.04803 AFIX 43 H34B 2 0.417513 0.939531 0.255451 -21.00000 -1.20000 AFIX 65 C35B 1 0.370310 0.855253 0.226038 -21.00000 0.03732 AFIX 0 C36B 1 0.362294 0.846825 0.312270 -21.00000 0.04814 AFIX 13 H36B 2 0.344135 0.796190 0.321908 -21.00000 -1.20000 AFIX 0 C37B 1 0.407184 0.839824 0.364220 -21.00000 0.06388 AFIX 137 H37D 2 0.421468 0.788608 0.345134 -21.00000 -1.50000 H37E 2 0.404570 0.832385 0.421992 -21.00000 -1.50000 H37F 2 0.422312 0.894301 0.356544 -21.00000 -1.50000 AFIX 0 C38B 1 0.345851 0.936977 0.331544 -21.00000 0.05901 AFIX 137 H38D 2 0.365769 0.982963 0.323988 -21.00000 -1.50000 H38E 2 0.340058 0.937733 0.387980 -21.00000 -1.50000 H38F 2 0.321072 0.948648 0.295152 -21.00000 -1.50000 AFIX 0 C39B 1 0.348560 0.732176 0.022337 -21.00000 0.06413 AFIX 13 H39B 2 0.333033 0.691855 0.054874 -21.00000 -1.20000 AFIX 0 C40B 1 0.319044 0.751359 -0.042112 -21.00000 0.09482 AFIX 137 H40D 2 0.298040 0.787982 -0.022612 -21.00000 -1.50000 H40E 2 0.307215 0.695786 -0.064833 -21.00000 -1.50000 H40F 2 0.331124 0.783796 -0.084210 -21.00000 -1.50000 AFIX 0 C41B 1 0.379464 0.664597 -0.005191 -21.00000 0.08350 AFIX 137 H41D 2 0.365329 0.620908 -0.042178 -21.00000 -1.50000 H41E 2 0.393255 0.633978 0.042478 -21.00000 -1.50000 H41F 2 0.399229 0.696440 -0.033171 -21.00000 -1.50000 AFIX 0 C42B 1 0.453450 0.964196 0.124821 -21.00000 0.05726 AFIX 13 H42B 2 0.465057 1.002878 0.170885 -21.00000 -1.20000 AFIX 0 C43B 1 0.483028 0.907995 0.077903 -21.00000 0.09691 AFIX 137 H43D 2 0.491903 0.855210 0.109857 -21.00000 -1.50000 H43E 2 0.506440 0.944354 0.069622 -21.00000 -1.50000 H43F 2 0.469091 0.889559 0.025123 -21.00000 -1.50000 AFIX 0 C44B 1 0.438556 1.011707 0.034300 -21.00000 0.06003 AFIX 137 H44D 2 0.461059 1.044682 0.016280 -21.00000 -1.50000 H44E 2 0.416258 1.052626 0.039458 -21.00000 -1.50000 H44F 2 0.429673 0.965492 -0.005575 -21.00000 -1.50000 AFIX 0 C21B 1 0.083671 0.724187 0.238643 -31.00000 0.04448 AFIX 13 H21B 2 0.106379 0.686434 0.224607 -31.00000 -1.20000 AFIX 0 C22B 1 0.047714 0.668299 0.236726 -31.00000 0.06418 AFIX 137 H22D 2 0.052045 0.623251 0.279598 -31.00000 -1.50000 H22E 2 0.042458 0.638909 0.183762 -31.00000 -1.50000 H22F 2 0.024607 0.705386 0.245537 -31.00000 -1.50000 AFIX 0 C23B 1 0.074068 0.794775 0.171241 -31.00000 0.07808 AFIX 137 H23D 2 0.054310 0.837078 0.187490 -31.00000 -1.50000 H23E 2 0.063059 0.765407 0.120594 -31.00000 -1.50000 H23F 2 0.098750 0.826568 0.162928 -31.00000 -1.50000 PART 0 AFIX 0 MOLE 2 C1A 1 0.000000 0.025445 0.250000 10.50000 0.08697 0.05479 = 0.09540 0.00000 0.05150 0.00000 AFIX 43 H1S 2 0.000001 -0.037734 0.249996 10.50000 -1.20000 AFIX 0 C3S 1 0.030547 0.161647 0.294048 11.00000 0.05583 0.08935 = 0.07328 -0.01282 0.01583 -0.01377 AFIX 43 H3S 2 0.051735 0.193515 0.324681 11.00000 -1.20000 AFIX 0 C2S 1 0.030759 0.071324 0.294238 11.00000 0.05763 0.09248 = 0.07208 0.01471 0.02525 0.01624 AFIX 43 H2S 2 0.052108 0.039940 0.324864 11.00000 -1.20000 AFIX 0 C4S 1 0.000000 0.206511 0.250000 10.50000 0.08159 0.05989 = 0.09181 0.00000 0.03008 0.00000 AFIX 43 H4S 2 0.000000 0.269690 0.249997 10.50000 -1.20000 AFIX 0 H1P 2 0.209925 0.786673 0.317188 11.00000 0.07141 H2P 2 0.286315 0.736983 0.130151 11.00000 0.10242 HKLF 4 REM PH09023 in C2/c REM R1 = 0.0529 for 4636 Fo > 4sig(Fo) and 0.0967 for all 7324 data REM 522 parameters refined using 0 restraints END WGHT 0.0501 10.0483 REM Highest difference peak 0.325, deepest hole -0.516, 1-sigma level 0.042 Q1 1 0.3080 0.7332 0.1433 11.00000 0.05 0.33 Q2 1 0.0478 0.8228 0.5605 11.00000 0.05 0.28 Q3 1 0.3375 0.7875 0.1665 11.00000 0.05 0.27 Q4 1 0.1624 0.7470 0.2140 11.00000 0.05 0.24 Q5 1 0.4178 0.9030 0.0864 11.00000 0.05 0.23 ; _database_code_depnum_ccdc_archive 'CCDC 948787' ####################################################################### # # 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_complex7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H136 K2 O16 P2, 2(C4 H8 O)' _chemical_formula_sum 'C92 H152 K2 O18 P2' _chemical_formula_weight 1686.3456 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 13.3096(19) _cell_length_b 17.990(3) _cell_length_c 21.542(3) _cell_angle_alpha 87.891(2) _cell_angle_beta 87.743(2) _cell_angle_gamma 68.936(2) _cell_volume 4808.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7013 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 19.68 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 0.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8866 _exptl_absorpt_correction_T_max 0.9907 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 58552 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.03 _reflns_number_total 16947 _reflns_number_gt 10086 _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^)+(0.0957P)^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 16947 _refine_ls_number_parameters 1028 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1624 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.029 _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 K1 K 0.23231(6) 0.56903(5) 0.62591(3) 0.0470(2) Uani 1 1 d . . . K2 K 1.0000 0.5000 0.0000 0.0348(2) Uani 1 2 d S . . K3 K 1.0000 0.0000 0.0000 0.0542(3) Uani 1 2 d S . . O1 O 0.1542(2) 0.50332(17) 0.53268(12) 0.0633(7) Uani 1 1 d . B . O2 O 0.33784(19) 0.54550(15) 0.51000(10) 0.0572(7) Uani 1 1 d . B . O3 O 0.3836(2) 0.64248(15) 0.60160(12) 0.0586(7) Uani 1 1 d . B . O4 O 0.32174(19) 0.61967(15) 0.72537(12) 0.0556(7) Uani 1 1 d . B . O5 O 0.16039(18) 0.56092(14) 0.75193(10) 0.0495(6) Uani 1 1 d . B . O6 O 0.10815(18) 0.47506(15) 0.65909(12) 0.0558(7) Uani 1 1 d . B . O7 O 0.4152(2) 0.43986(17) 0.65692(13) 0.0740(8) Uani 1 1 d . B . O9 O 1.02667(19) 0.34731(13) -0.04331(10) 0.0489(6) Uani 1 1 d . . . O10 O 1.12924(19) 0.36292(13) 0.06397(10) 0.0503(6) Uani 1 1 d . . . O11 O 1.05834(17) 0.51410(13) 0.11858(9) 0.0410(5) Uani 1 1 d . . . O12 O 0.8065(2) 0.50059(18) 0.04726(14) 0.0723(8) Uani 1 1 d . . . O13 O 0.8591(2) -0.07331(15) 0.04669(12) 0.0637(7) Uani 1 1 d . . . O14 O 1.0081(2) -0.04924(14) 0.12396(11) 0.0578(7) Uani 1 1 d . . . O15 O 1.1798(2) -0.00929(14) 0.06950(12) 0.0618(7) Uani 1 1 d . . . P1 P 0.13270(7) 0.65448(5) 0.31129(4) 0.0359(2) Uani 1 1 d . . . P2 P 0.25720(7) 0.34753(5) 0.33164(4) 0.0341(2) Uani 1 1 d . . . C1 C 0.2106(2) 0.64143(17) 0.23980(13) 0.0299(7) Uani 1 1 d . A . C2 C 0.2013(3) 0.70494(18) 0.19650(13) 0.0347(7) Uani 1 1 d . . . H2 H 0.1508 0.7565 0.2051 0.042 Uiso 1 1 calc R A . C3 C 0.2627(3) 0.69437(19) 0.14279(14) 0.0413(8) Uani 1 1 d . A . H3 H 0.2528 0.7382 0.1147 0.050 Uiso 1 1 calc R . . C4 C 0.3387(3) 0.62092(19) 0.12887(14) 0.0385(8) Uani 1 1 d . . . H4 H 0.3827 0.6146 0.0922 0.046 Uiso 1 1 calc R A . C5 C 0.3503(2) 0.55593(17) 0.16927(13) 0.0321(7) Uani 1 1 d . A . C6 C 0.4370(3) 0.47815(18) 0.15565(15) 0.0411(8) Uani 1 1 d . . . H6A H 0.5052 0.4785 0.1722 0.049 Uiso 1 1 calc R A . H6B H 0.4469 0.4732 0.1100 0.049 Uiso 1 1 calc R . . C7 C 0.4168(2) 0.40586(18) 0.18204(14) 0.0330(7) Uani 1 1 d . A . C8 C 0.4674(3) 0.33362(19) 0.15232(15) 0.0421(8) Uani 1 1 d . . . H8 H 0.5085 0.3312 0.1149 0.050 Uiso 1 1 calc R A . C9 C 0.4563(3) 0.26574(19) 0.17857(16) 0.0471(9) Uani 1 1 d . A . H9 H 0.4909 0.2160 0.1592 0.057 Uiso 1 1 calc R . . C10 C 0.3959(3) 0.26894(18) 0.23230(15) 0.0402(8) Uani 1 1 d . . . H10 H 0.3918 0.2208 0.2498 0.048 Uiso 1 1 calc R A . C11 C 0.3396(2) 0.34139(17) 0.26262(13) 0.0299(7) Uani 1 1 d . A . C12 C 0.3530(2) 0.41202(17) 0.23529(13) 0.0287(7) Uani 1 1 d . . . C13 C 0.2945(2) 0.49182(16) 0.26376(13) 0.0287(7) Uani 1 1 d . A . H13A H 0.3313 0.4944 0.3022 0.034 Uiso 1 1 calc R . . H13B H 0.2207 0.4947 0.2761 0.034 Uiso 1 1 calc R . . C14 C 0.2857(2) 0.56457(17) 0.22344(13) 0.0281(7) Uani 1 1 d . . . C30 C 0.2792(2) 0.24002(18) 0.34961(14) 0.0343(7) Uani 1 1 d . . . C31 C 0.3452(3) 0.19862(18) 0.39867(15) 0.0402(8) Uani 1 1 d . . . C32 C 0.3525(3) 0.1217(2) 0.41640(16) 0.0497(9) Uani 1 1 d . . . H32 H 0.3972 0.0958 0.4499 0.060 Uiso 1 1 calc R . . C33 C 0.2972(3) 0.0815(2) 0.38716(16) 0.0486(9) Uani 1 1 d . . . C34 C 0.2322(3) 0.12166(19) 0.33846(16) 0.0464(9) Uani 1 1 d . . . H34 H 0.1926 0.0959 0.3177 0.056 Uiso 1 1 calc R . . C35 C 0.2234(3) 0.19832(19) 0.31925(15) 0.0397(8) Uani 1 1 d . . . C36 C 0.4126(3) 0.2342(2) 0.43428(16) 0.0479(9) Uani 1 1 d . . . H36 H 0.3987 0.2892 0.4170 0.057 Uiso 1 1 calc R . . C37 C 0.3805(4) 0.2413(3) 0.50268(18) 0.0735(13) Uani 1 1 d . . . H37A H 0.3038 0.2738 0.5074 0.110 Uiso 1 1 calc R . . H37B H 0.4232 0.2667 0.5238 0.110 Uiso 1 1 calc R . . H37C H 0.3937 0.1881 0.5211 0.110 Uiso 1 1 calc R . . C38 C 0.5322(3) 0.1862(2) 0.4238(2) 0.0721(13) Uani 1 1 d . . . H38A H 0.5749 0.2142 0.4414 0.108 Uiso 1 1 calc R . . H38B H 0.5485 0.1798 0.3791 0.108 Uiso 1 1 calc R . . H38C H 0.5498 0.1336 0.4442 0.108 Uiso 1 1 calc R . . C39 C 0.3061(4) -0.0022(2) 0.40756(19) 0.0626(11) Uani 1 1 d . . . H39 H 0.2602 -0.0197 0.3802 0.075 Uiso 1 1 calc R . . C40 C 0.2671(5) -0.0049(3) 0.4731(2) 0.1055(18) Uani 1 1 d . . . H40A H 0.3097 0.0138 0.5005 0.158 Uiso 1 1 calc R . . H40B H 0.2750 -0.0598 0.4849 0.158 Uiso 1 1 calc R . . H40C H 0.1911 0.0295 0.4769 0.158 Uiso 1 1 calc R . . C41 C 0.4219(4) -0.0610(2) 0.4012(3) 0.0940(16) Uani 1 1 d . . . H41A H 0.4685 -0.0443 0.4271 0.141 Uiso 1 1 calc R . . H41B H 0.4466 -0.0623 0.3577 0.141 Uiso 1 1 calc R . . H41C H 0.4248 -0.1143 0.4149 0.141 Uiso 1 1 calc R . . C42 C 0.1486(3) 0.2370(2) 0.26598(16) 0.0507(10) Uani 1 1 d . . . H42 H 0.1636 0.2855 0.2512 0.061 Uiso 1 1 calc R . . C43 C 0.0330(4) 0.2632(3) 0.2884(3) 0.1006(18) Uani 1 1 d . . . H43A H 0.0167 0.2167 0.3036 0.151 Uiso 1 1 calc R . . H43B H -0.0141 0.2893 0.2541 0.151 Uiso 1 1 calc R . . H43C H 0.0211 0.3007 0.3222 0.151 Uiso 1 1 calc R . . C44 C 0.1670(5) 0.1819(3) 0.21127(19) 0.0955(18) Uani 1 1 d . . . H44A H 0.2415 0.1674 0.1956 0.143 Uiso 1 1 calc R . . H44B H 0.1176 0.2093 0.1782 0.143 Uiso 1 1 calc R . . H44C H 0.1536 0.1336 0.2249 0.143 Uiso 1 1 calc R . . C45 C 0.2249(3) 0.4814(3) 0.4781(2) 0.0871(17) Uani 1 1 d . . . H45A H 0.1840 0.4750 0.4426 0.104 Uiso 1 1 calc R B . H45B H 0.2837 0.4298 0.4862 0.104 Uiso 1 1 calc R . . C46 C 0.2707(4) 0.5433(3) 0.46271(18) 0.0793(15) Uani 1 1 d . B . H46A H 0.3123 0.5313 0.4229 0.095 Uiso 1 1 calc R . . H46B H 0.2121 0.5958 0.4581 0.095 Uiso 1 1 calc R . . C47 C 0.3892(4) 0.6035(2) 0.4981(2) 0.0772(15) Uani 1 1 d . . . H47A H 0.3338 0.6569 0.4906 0.093 Uiso 1 1 calc R B . H47B H 0.4368 0.5890 0.4605 0.093 Uiso 1 1 calc R . . C48 C 0.4533(4) 0.6057(3) 0.5523(2) 0.0731(12) Uani 1 1 d . B . H48A H 0.4988 0.5507 0.5649 0.088 Uiso 1 1 calc R . . H48B H 0.5012 0.6356 0.5410 0.088 Uiso 1 1 calc R . . C49 C 0.4417(3) 0.6452(3) 0.6555(2) 0.0685(12) Uani 1 1 d . . . H49A H 0.4854 0.6789 0.6463 0.082 Uiso 1 1 calc R B . H49B H 0.4913 0.5908 0.6665 0.082 Uiso 1 1 calc R . . C50 C 0.3682(3) 0.6771(2) 0.7071(2) 0.0621(11) Uani 1 1 d . B . H50A H 0.4072 0.6874 0.7420 0.075 Uiso 1 1 calc R . . H50B H 0.3114 0.7278 0.6945 0.075 Uiso 1 1 calc R . . C51 C 0.2591(3) 0.6381(3) 0.78086(18) 0.0650(12) Uani 1 1 d . . . H51A H 0.1951 0.6870 0.7747 0.078 Uiso 1 1 calc R B . H51B H 0.3019 0.6474 0.8143 0.078 Uiso 1 1 calc R . . C52 C 0.2254(3) 0.5703(3) 0.79815(17) 0.0619(11) Uani 1 1 d . B . H52A H 0.2896 0.5211 0.8027 0.074 Uiso 1 1 calc R . . H52B H 0.1849 0.5802 0.8384 0.074 Uiso 1 1 calc R . . C53 C 0.1245(3) 0.4958(2) 0.76512(17) 0.0574(10) Uani 1 1 d . . . H53A H 0.0875 0.5022 0.8064 0.069 Uiso 1 1 calc R B . H53B H 0.1869 0.4450 0.7657 0.069 Uiso 1 1 calc R . . C54 C 0.0496(3) 0.4943(2) 0.71672(18) 0.0583(10) Uani 1 1 d . B . H54A H 0.0169 0.4540 0.7280 0.070 Uiso 1 1 calc R . . H54B H -0.0089 0.5470 0.7131 0.070 Uiso 1 1 calc R . . C55 C 0.0393(3) 0.4739(3) 0.6098(2) 0.0657(12) Uani 1 1 d . . . H55A H -0.0148 0.5278 0.6025 0.079 Uiso 1 1 calc R B . H55B H 0.0008 0.4371 0.6209 0.079 Uiso 1 1 calc R . . C56 C 0.1080(3) 0.4467(3) 0.5526(2) 0.0732(13) Uani 1 1 d . B . H56A H 0.1659 0.3948 0.5613 0.088 Uiso 1 1 calc R . . H56B H 0.0638 0.4391 0.5192 0.088 Uiso 1 1 calc R . . C57 C 0.4040(4) 0.3668(3) 0.6473(3) 0.0921(16) Uani 1 1 d . . . H57A H 0.4604 0.3348 0.6178 0.111 Uiso 1 1 calc R B . H57B H 0.3325 0.3753 0.6304 0.111 Uiso 1 1 calc R . . C58 C 0.4155(4) 0.3252(3) 0.7105(3) 0.0960(18) Uani 1 1 d . B . H58A H 0.4535 0.2670 0.7070 0.115 Uiso 1 1 calc R . . H58B H 0.3443 0.3354 0.7313 0.115 Uiso 1 1 calc R . . C59 C 0.4819(3) 0.3625(2) 0.74560(19) 0.0622(11) Uani 1 1 d . . . H59A H 0.4427 0.3882 0.7837 0.075 Uiso 1 1 calc R B . H59B H 0.5519 0.3219 0.7573 0.075 Uiso 1 1 calc R . . C60 C 0.4980(3) 0.4230(2) 0.70088(17) 0.0551(10) Uani 1 1 d . B . H60A H 0.4922 0.4719 0.7227 0.066 Uiso 1 1 calc R . . H60B H 0.5698 0.4015 0.6800 0.066 Uiso 1 1 calc R . . C65 C 1.1140(3) 0.2830(2) -0.01740(18) 0.0594(11) Uani 1 1 d . . . H65A H 1.1833 0.2834 -0.0355 0.071 Uiso 1 1 calc R . . H65B H 1.1073 0.2315 -0.0269 0.071 Uiso 1 1 calc R . . C66 C 1.1108(4) 0.2926(2) 0.05112(18) 0.0631(11) Uani 1 1 d . . . H66A H 1.0396 0.2956 0.0687 0.076 Uiso 1 1 calc R . . H66B H 1.1666 0.2461 0.0705 0.076 Uiso 1 1 calc R . . C67 C 1.1327(3) 0.3732(2) 0.12921(15) 0.0552(10) Uani 1 1 d . . . H67A H 1.1929 0.3283 0.1472 0.066 Uiso 1 1 calc R . . H67B H 1.0647 0.3735 0.1498 0.066 Uiso 1 1 calc R . . C68 C 1.1478(3) 0.4496(2) 0.14040(16) 0.0504(9) Uani 1 1 d . . . H68A H 1.1552 0.4548 0.1854 0.060 Uiso 1 1 calc R . . H68B H 1.2144 0.4501 0.1186 0.060 Uiso 1 1 calc R . . C69 C 1.0658(3) 0.5887(2) 0.13417(15) 0.0483(9) Uani 1 1 d . . . H69A H 1.1331 0.5929 0.1160 0.058 Uiso 1 1 calc R . . H69B H 1.0669 0.5924 0.1799 0.058 Uiso 1 1 calc R . . C70 C 0.9712(3) 0.6541(2) 0.10915(16) 0.0528(10) Uani 1 1 d . . . H70A H 0.9041 0.6481 0.1259 0.063 Uiso 1 1 calc R . . H70B H 0.9719 0.7060 0.1225 0.063 Uiso 1 1 calc R . . C71 C 0.7252(4) 0.5751(3) 0.0588(3) 0.0925(16) Uani 1 1 d . . . H71A H 0.7376 0.6174 0.0324 0.111 Uiso 1 1 calc R . . H71B H 0.7242 0.5889 0.1029 0.111 Uiso 1 1 calc R . . C72 C 0.6218(4) 0.5668(4) 0.0433(4) 0.135(3) Uani 1 1 d . . . H72A H 0.5685 0.5843 0.0782 0.162 Uiso 1 1 calc R . . H72B H 0.5914 0.5989 0.0057 0.162 Uiso 1 1 calc R . . C73 C 0.6496(4) 0.4807(4) 0.0324(3) 0.119(2) Uani 1 1 d . . . H73A H 0.6326 0.4533 0.0698 0.143 Uiso 1 1 calc R . . H73B H 0.6096 0.4727 -0.0030 0.143 Uiso 1 1 calc R . . C74 C 0.7611(4) 0.4519(3) 0.0189(3) 0.0924(16) Uani 1 1 d . . . H74A H 0.7941 0.3963 0.0348 0.111 Uiso 1 1 calc R . . H74B H 0.7745 0.4525 -0.0266 0.111 Uiso 1 1 calc R . . C75 C 0.8483(4) -0.0761(3) 0.1129(2) 0.0759(13) Uani 1 1 d . . . H75A H 0.8090 -0.1118 0.1258 0.091 Uiso 1 1 calc R . . H75B H 0.8068 -0.0222 0.1283 0.091 Uiso 1 1 calc R . . C76 C 0.9572(4) -0.1060(2) 0.13977(18) 0.0650(11) Uani 1 1 d . . . H76A H 0.9513 -0.1121 0.1855 0.078 Uiso 1 1 calc R . . H76B H 1.0005 -0.1587 0.1227 0.078 Uiso 1 1 calc R . . C77 C 1.1109(3) -0.0706(2) 0.15149(17) 0.0619(11) Uani 1 1 d . . . H77A H 1.1597 -0.1227 0.1360 0.074 Uiso 1 1 calc R . . H77B H 1.1031 -0.0753 0.1972 0.074 Uiso 1 1 calc R . . C78 C 1.1562(4) -0.0085(2) 0.13502(19) 0.0692(12) Uani 1 1 d . . . H78A H 1.1039 0.0444 0.1466 0.083 Uiso 1 1 calc R . . H78B H 1.2228 -0.0185 0.1581 0.083 Uiso 1 1 calc R . . C79 C 1.2221(4) 0.0500(3) 0.0510(2) 0.0798(14) Uani 1 1 d . . . H79A H 1.2902 0.0407 0.0724 0.096 Uiso 1 1 calc R . . H79B H 1.1703 0.1032 0.0624 0.096 Uiso 1 1 calc R . . C80 C 0.7580(4) -0.0471(3) 0.0175(2) 0.0805(14) Uani 1 1 d . . . H80A H 0.7148 0.0080 0.0297 0.097 Uiso 1 1 calc R . . H80B H 0.7176 -0.0820 0.0305 0.097 Uiso 1 1 calc R . . C15 C 0.0666(8) 0.7656(6) 0.3140(5) 0.031(3) Uani 0.652(10) 1 d PU A 1 C16 C 0.1240(9) 0.8205(7) 0.3216(5) 0.033(3) Uani 0.652(10) 1 d P A 1 C17 C 0.0726(9) 0.8977(7) 0.3266(6) 0.038(3) Uani 0.652(10) 1 d P A 1 H17 H 0.1140 0.9309 0.3279 0.046 Uiso 0.652(10) 1 calc PR A 1 C18 C -0.0401(12) 0.9338(8) 0.3301(6) 0.049(3) Uani 0.652(10) 1 d P A 1 C19 C -0.1019(10) 0.8849(7) 0.3241(5) 0.049(2) Uani 0.652(10) 1 d P A 1 H19 H -0.1783 0.9076 0.3257 0.058 Uiso 0.652(10) 1 calc PR A 1 C20 C -0.0495(10) 0.8020(6) 0.3156(7) 0.038(2) Uani 0.652(10) 1 d P A 1 C21 C 0.2431(16) 0.7885(10) 0.3209(9) 0.038(3) Uani 0.652(10) 1 d P A 1 H21 H 0.2672 0.7326 0.3062 0.046 Uiso 0.652(10) 1 calc PR A 1 C22 C 0.2790(9) 0.7845(7) 0.3892(5) 0.052(2) Uani 0.652(10) 1 d P A 1 H22A H 0.2460 0.7528 0.4148 0.078 Uiso 0.652(10) 1 calc PR A 1 H22B H 0.2561 0.8385 0.4053 0.078 Uiso 0.652(10) 1 calc PR A 1 H22C H 0.3576 0.7596 0.3905 0.078 Uiso 0.652(10) 1 calc PR A 1 C23 C 0.2992(12) 0.8296(8) 0.2833(8) 0.048(3) Uani 0.652(10) 1 d P A 1 H23A H 0.3770 0.8009 0.2858 0.072 Uiso 0.652(10) 1 calc PR A 1 H23B H 0.2810 0.8837 0.2984 0.072 Uiso 0.652(10) 1 calc PR A 1 H23C H 0.2778 0.8322 0.2400 0.072 Uiso 0.652(10) 1 calc PR A 1 C24 C -0.0969(7) 1.0231(4) 0.3376(4) 0.057(2) Uani 0.652(10) 1 d P A 1 H24 H -0.0504 1.0422 0.3633 0.069 Uiso 0.652(10) 1 calc PR A 1 C25 C -0.1054(8) 1.0655(5) 0.2720(4) 0.087(3) Uani 0.652(10) 1 d PU A 1 H25A H -0.0334 1.0513 0.2525 0.130 Uiso 0.652(10) 1 calc PR A 1 H25B H -0.1370 1.1233 0.2767 0.130 Uiso 0.652(10) 1 calc PR A 1 H25C H -0.1512 1.0482 0.2458 0.130 Uiso 0.652(10) 1 calc PR A 1 C26 C -0.1988(8) 1.0490(4) 0.3649(5) 0.120(5) Uani 0.652(10) 1 d P A 1 H26A H -0.2257 1.1072 0.3677 0.181 Uiso 0.652(10) 1 calc PR A 1 H26B H -0.1958 1.0251 0.4068 0.181 Uiso 0.652(10) 1 calc PR A 1 H26C H -0.2472 1.0332 0.3398 0.181 Uiso 0.652(10) 1 calc PR A 1 C27 C -0.1193(6) 0.7520(5) 0.3120(4) 0.043(2) Uani 0.652(10) 1 d P A 1 H27 H -0.0727 0.6958 0.3225 0.052 Uiso 0.652(10) 1 calc PR A 1 C28 C -0.1550(12) 0.7524(8) 0.2466(5) 0.109(5) Uani 0.652(10) 1 d P A 1 H28A H -0.2006 0.7203 0.2451 0.164 Uiso 0.652(10) 1 calc PR A 1 H28B H -0.0917 0.7300 0.2190 0.164 Uiso 0.652(10) 1 calc PR A 1 H28C H -0.1959 0.8073 0.2331 0.164 Uiso 0.652(10) 1 calc PR A 1 C29 C -0.2150(7) 0.7738(7) 0.3569(3) 0.078(3) Uani 0.652(10) 1 d P A 1 H29A H -0.1909 0.7756 0.3990 0.117 Uiso 0.652(10) 1 calc PR A 1 H29B H -0.2490 0.7338 0.3557 0.117 Uiso 0.652(10) 1 calc PR A 1 H29C H -0.2671 0.8261 0.3450 0.117 Uiso 0.652(10) 1 calc PR A 1 O8 O 0.1030(8) 0.7030(6) 0.5577(6) 0.091(3) Uani 0.748(17) 1 d P B 1 C61 C 0.0063(9) 0.7160(6) 0.5246(7) 0.124(5) Uani 0.748(17) 1 d P B 1 H61A H 0.0202 0.6753 0.4925 0.149 Uiso 0.748(17) 1 calc PR B 1 H61B H -0.0507 0.7113 0.5536 0.149 Uiso 0.748(17) 1 calc PR B 1 C62 C -0.0265(12) 0.7900(9) 0.4974(6) 0.145(6) Uani 0.748(17) 1 d P B 1 H62A H -0.1058 0.8156 0.5013 0.174 Uiso 0.748(17) 1 calc PR B 1 H62B H -0.0056 0.7864 0.4527 0.174 Uiso 0.748(17) 1 calc PR B 1 C63 C 0.0256(7) 0.8376(6) 0.5290(5) 0.123(4) Uani 0.748(17) 1 d P B 1 H63A H 0.0510 0.8699 0.4985 0.148 Uiso 0.748(17) 1 calc PR B 1 H63B H -0.0253 0.8737 0.5591 0.148 Uiso 0.748(17) 1 calc PR B 1 C64 C 0.1146(9) 0.7805(6) 0.5605(5) 0.086(3) Uani 0.748(17) 1 d P B 1 H64A H 0.1144 0.7955 0.6043 0.104 Uiso 0.748(17) 1 calc PR B 1 H64B H 0.1834 0.7785 0.5400 0.104 Uiso 0.748(17) 1 calc PR B 1 C15B C 0.0547(16) 0.7629(12) 0.3077(9) 0.035(7) Uiso 0.348(10) 1 d P A 2 C16B C 0.1086(18) 0.8114(14) 0.3168(11) 0.028(5) Uiso 0.348(10) 1 d P A 2 C17B C 0.044(2) 0.9022(16) 0.3280(12) 0.031(5) Uiso 0.348(10) 1 d P A 2 H17B H 0.0804 0.9361 0.3401 0.037 Uiso 0.348(10) 1 calc PR A 2 C18B C -0.061(2) 0.9306(16) 0.3202(11) 0.030(5) Uiso 0.348(10) 1 d P A 2 C19B C -0.102(2) 0.8746(15) 0.3081(9) 0.041(6) Uiso 0.348(10) 1 d P A 2 H19B H -0.1780 0.8945 0.3027 0.050 Uiso 0.348(10) 1 calc PR A 2 C20B C -0.053(3) 0.7925(16) 0.3023(12) 0.046(8) Uiso 0.348(10) 1 d P A 2 C21B C 0.236(3) 0.789(2) 0.3334(15) 0.041(9) Uiso 0.348(10) 1 d P A 2 H21B H 0.2752 0.7316 0.3232 0.049 Uiso 0.348(10) 1 calc PR A 2 C22B C 0.2517(17) 0.7985(15) 0.4000(11) 0.049(6) Uiso 0.348(10) 1 d P A 2 H22D H 0.2193 0.7665 0.4257 0.074 Uiso 0.348(10) 1 calc PR A 2 H22E H 0.2173 0.8548 0.4105 0.074 Uiso 0.348(10) 1 calc PR A 2 H22F H 0.3289 0.7808 0.4078 0.074 Uiso 0.348(10) 1 calc PR A 2 C23B C 0.284(2) 0.8461(16) 0.2839(14) 0.043(7) Uiso 0.348(10) 1 d P A 2 H23D H 0.2691 0.8383 0.2409 0.064 Uiso 0.348(10) 1 calc PR A 2 H23E H 0.3622 0.8302 0.2884 0.064 Uiso 0.348(10) 1 calc PR A 2 H23F H 0.2490 0.9023 0.2941 0.064 Uiso 0.348(10) 1 calc PR A 2 C24B C -0.1215(16) 1.0193(11) 0.3223(8) 0.051(5) Uiso 0.348(10) 1 d P A 2 H24B H -0.1992 1.0349 0.3123 0.061 Uiso 0.348(10) 1 calc PR A 2 C25B C -0.0679(10) 1.0703(6) 0.2895(5) 0.045(3) Uiso 0.348(10) 1 d P A 2 H25D H -0.1110 1.1265 0.2961 0.067 Uiso 0.348(10) 1 calc PR A 2 H25E H -0.0614 1.0598 0.2450 0.067 Uiso 0.348(10) 1 calc PR A 2 H25F H 0.0040 1.0580 0.3061 0.067 Uiso 0.348(10) 1 calc PR A 2 C26B C -0.1020(16) 1.0412(10) 0.3967(8) 0.103(6) Uiso 0.348(10) 1 d P A 2 H26D H -0.1390 1.0984 0.4032 0.155 Uiso 0.348(10) 1 calc PR A 2 H26E H -0.0247 1.0269 0.4031 0.155 Uiso 0.348(10) 1 calc PR A 2 H26F H -0.1311 1.0110 0.4264 0.155 Uiso 0.348(10) 1 calc PR A 2 C27B C -0.1200(14) 0.7441(10) 0.2905(8) 0.031(4) Uiso 0.348(10) 1 d P A 2 H27B H -0.0721 0.6918 0.2736 0.037 Uiso 0.348(10) 1 calc PR A 2 C28B C -0.2064(11) 0.7822(9) 0.2461(8) 0.045(4) Uiso 0.348(10) 1 d P A 2 H28D H -0.2448 0.7461 0.2388 0.068 Uiso 0.348(10) 1 calc PR A 2 H28E H -0.1748 0.7938 0.2067 0.068 Uiso 0.348(10) 1 calc PR A 2 H28F H -0.2568 0.8319 0.2632 0.068 Uiso 0.348(10) 1 calc PR A 2 C29B C -0.1667(12) 0.7288(8) 0.3524(6) 0.055(4) Uiso 0.348(10) 1 d P A 2 H29D H -0.2078 0.6940 0.3469 0.082 Uiso 0.348(10) 1 calc PR A 2 H29E H -0.2145 0.7794 0.3694 0.082 Uiso 0.348(10) 1 calc PR A 2 H29F H -0.1083 0.7029 0.3811 0.082 Uiso 0.348(10) 1 calc PR A 2 O8B O 0.087(3) 0.692(2) 0.5761(13) 0.076(8) Uiso 0.252(17) 1 d P B 2 C61B C -0.008(2) 0.6879(15) 0.5412(12) 0.063(7) Uiso 0.252(17) 1 d P B 2 H61C H -0.0569 0.6704 0.5688 0.075 Uiso 0.252(17) 1 calc PR B 2 H61D H 0.0159 0.6520 0.5055 0.075 Uiso 0.252(17) 1 calc PR B 2 C62B C -0.063(3) 0.777(2) 0.5194(17) 0.098(11) Uiso 0.252(17) 1 d P B 2 H62C H -0.1165 0.7827 0.4874 0.117 Uiso 0.252(17) 1 calc PR B 2 H62D H -0.0982 0.8112 0.5548 0.117 Uiso 0.252(17) 1 calc PR B 2 C63B C 0.027(2) 0.7971(19) 0.4938(17) 0.077(9) Uiso 0.252(17) 1 d P B 2 H63C H 0.0107 0.8552 0.4889 0.093 Uiso 0.252(17) 1 calc PR B 2 H63D H 0.0584 0.7695 0.4549 0.093 Uiso 0.252(17) 1 calc PR B 2 C64B C 0.095(3) 0.758(2) 0.5545(16) 0.068(9) Uiso 0.252(17) 1 d P B 2 H64C H 0.1722 0.7474 0.5445 0.082 Uiso 0.252(17) 1 calc PR B 2 H64D H 0.0727 0.7970 0.5880 0.082 Uiso 0.252(17) 1 calc PR B 2 O16 O 0.9222(3) 0.1489(2) 0.05361(19) 0.1378(11) Uani 1 1 d U . . C81 C 0.8660(5) 0.1591(4) 0.1139(3) 0.1385(11) Uani 1 1 d U . . H81A H 0.8858 0.1077 0.1373 0.166 Uiso 1 1 calc R . . H81B H 0.8839 0.1976 0.1389 0.166 Uiso 1 1 calc R . . C82 C 0.7575(5) 0.1878(4) 0.1006(3) 0.1386(11) Uani 1 1 d U . . H82A H 0.7135 0.2193 0.1353 0.166 Uiso 1 1 calc R . . H82B H 0.7324 0.1437 0.0923 0.166 Uiso 1 1 calc R . . C83 C 0.7518(5) 0.2387(4) 0.0441(3) 0.1401(11) Uani 1 1 d U . . H83A H 0.6960 0.2362 0.0161 0.168 Uiso 1 1 calc R . . H83B H 0.7355 0.2949 0.0552 0.168 Uiso 1 1 calc R . . C84 C 0.8584(5) 0.2049(4) 0.0154(3) 0.1386(11) Uani 1 1 d U . . H84A H 0.8540 0.1811 -0.0246 0.166 Uiso 1 1 calc R . . H84B H 0.8888 0.2472 0.0071 0.166 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0403(5) 0.0712(6) 0.0340(4) 0.0020(4) -0.0053(3) -0.0253(4) K2 0.0349(6) 0.0387(6) 0.0316(5) -0.0009(4) -0.0083(4) -0.0132(5) K3 0.0705(8) 0.0449(7) 0.0418(6) 0.0031(5) -0.0015(6) -0.0146(6) O1 0.0460(16) 0.088(2) 0.0504(16) -0.0246(14) -0.0072(13) -0.0146(15) O2 0.0533(16) 0.0693(17) 0.0364(14) 0.0084(12) 0.0007(12) -0.0081(14) O3 0.0463(15) 0.0580(16) 0.0662(18) 0.0064(13) 0.0129(14) -0.0146(13) O4 0.0499(16) 0.0645(17) 0.0604(17) -0.0023(13) -0.0085(13) -0.0295(13) O5 0.0423(14) 0.0614(16) 0.0430(14) 0.0027(12) -0.0055(11) -0.0162(12) O6 0.0361(14) 0.0741(18) 0.0605(17) -0.0070(13) -0.0021(13) -0.0232(13) O7 0.0646(18) 0.077(2) 0.080(2) 0.0006(16) -0.0346(16) -0.0208(16) O9 0.0604(16) 0.0430(14) 0.0418(14) -0.0062(11) -0.0035(12) -0.0162(12) O10 0.0629(16) 0.0436(14) 0.0422(14) 0.0053(11) -0.0131(12) -0.0158(12) O11 0.0425(13) 0.0517(14) 0.0337(12) -0.0009(10) -0.0130(10) -0.0216(11) O12 0.0476(17) 0.081(2) 0.094(2) -0.0122(17) 0.0042(15) -0.0298(16) O13 0.0653(19) 0.0579(17) 0.0644(18) 0.0160(13) -0.0036(14) -0.0193(14) O14 0.0825(19) 0.0399(14) 0.0440(14) 0.0068(11) -0.0051(14) -0.0140(14) O15 0.0791(19) 0.0469(15) 0.0609(17) 0.0095(13) -0.0173(14) -0.0237(14) P1 0.0402(5) 0.0303(4) 0.0359(5) 0.0014(4) 0.0026(4) -0.0118(4) P2 0.0386(5) 0.0296(4) 0.0334(5) 0.0016(3) -0.0012(4) -0.0115(4) C1 0.0315(17) 0.0356(17) 0.0280(16) 0.0005(13) -0.0087(13) -0.0180(14) C2 0.0425(19) 0.0319(17) 0.0304(18) 0.0023(13) -0.0066(15) -0.0139(15) C3 0.061(2) 0.0362(19) 0.0314(18) 0.0105(14) -0.0107(17) -0.0235(18) C4 0.045(2) 0.044(2) 0.0297(17) 0.0024(15) 0.0021(15) -0.0202(17) C5 0.0380(18) 0.0332(17) 0.0283(17) -0.0015(13) -0.0025(14) -0.0163(15) C6 0.046(2) 0.0419(19) 0.0350(18) -0.0001(15) 0.0088(15) -0.0170(17) C7 0.0306(17) 0.0354(18) 0.0316(17) -0.0001(14) -0.0030(14) -0.0099(14) C8 0.040(2) 0.045(2) 0.0366(19) -0.0061(16) 0.0069(15) -0.0102(16) C9 0.054(2) 0.0332(19) 0.048(2) -0.0108(16) 0.0068(18) -0.0073(17) C10 0.048(2) 0.0303(18) 0.041(2) 0.0008(14) -0.0013(16) -0.0122(16) C11 0.0281(17) 0.0301(17) 0.0307(16) 0.0008(13) -0.0071(13) -0.0087(14) C12 0.0291(17) 0.0307(17) 0.0254(16) -0.0006(13) -0.0066(13) -0.0091(13) C13 0.0283(17) 0.0340(17) 0.0251(16) 0.0020(13) -0.0056(13) -0.0127(14) C14 0.0308(17) 0.0313(16) 0.0258(16) -0.0018(12) -0.0070(13) -0.0147(14) C30 0.0345(18) 0.0338(17) 0.0344(17) 0.0032(14) -0.0020(14) -0.0125(15) C31 0.043(2) 0.0345(18) 0.043(2) 0.0037(15) -0.0082(16) -0.0144(16) C32 0.062(2) 0.040(2) 0.050(2) 0.0125(16) -0.0210(18) -0.0205(18) C33 0.061(2) 0.038(2) 0.049(2) 0.0084(16) -0.0151(18) -0.0200(18) C34 0.055(2) 0.038(2) 0.051(2) 0.0043(16) -0.0138(18) -0.0225(17) C35 0.042(2) 0.0384(19) 0.0395(19) 0.0061(15) -0.0086(16) -0.0149(16) C36 0.051(2) 0.041(2) 0.056(2) 0.0102(17) -0.0201(18) -0.0207(18) C37 0.116(4) 0.068(3) 0.051(2) 0.003(2) -0.023(2) -0.048(3) C38 0.059(3) 0.055(3) 0.104(4) 0.008(2) -0.027(2) -0.021(2) C39 0.091(3) 0.039(2) 0.065(3) 0.0167(19) -0.023(2) -0.031(2) C40 0.160(5) 0.060(3) 0.103(4) 0.024(3) -0.003(4) -0.050(3) C41 0.109(4) 0.043(3) 0.130(4) 0.022(3) -0.038(3) -0.025(3) C42 0.063(3) 0.041(2) 0.056(2) 0.0129(17) -0.0283(19) -0.0267(19) C43 0.055(3) 0.094(4) 0.148(5) 0.050(3) -0.037(3) -0.021(3) C44 0.176(5) 0.062(3) 0.060(3) 0.011(2) -0.059(3) -0.051(3) C45 0.040(2) 0.144(5) 0.055(3) -0.059(3) -0.012(2) -0.001(3) C46 0.050(3) 0.123(4) 0.039(2) -0.002(2) 0.001(2) -0.001(3) C47 0.093(4) 0.052(3) 0.070(3) 0.014(2) 0.047(3) -0.012(2) C48 0.072(3) 0.070(3) 0.088(3) -0.003(3) 0.020(3) -0.040(3) C49 0.050(3) 0.075(3) 0.089(3) 0.030(2) -0.027(3) -0.033(2) C50 0.051(3) 0.060(3) 0.081(3) 0.007(2) -0.021(2) -0.025(2) C51 0.054(3) 0.083(3) 0.051(3) -0.022(2) -0.011(2) -0.013(2) C52 0.058(3) 0.087(3) 0.036(2) -0.002(2) -0.0047(19) -0.021(2) C53 0.050(2) 0.065(3) 0.050(2) 0.0075(19) 0.0114(19) -0.013(2) C54 0.044(2) 0.060(3) 0.073(3) 0.003(2) 0.012(2) -0.0226(19) C55 0.044(2) 0.075(3) 0.085(3) -0.005(2) -0.018(2) -0.027(2) C56 0.053(3) 0.078(3) 0.086(3) -0.028(3) -0.031(2) -0.015(2) C57 0.071(3) 0.088(4) 0.119(4) -0.029(3) -0.035(3) -0.024(3) C58 0.052(3) 0.064(3) 0.179(6) -0.011(3) -0.009(3) -0.028(2) C59 0.055(3) 0.055(2) 0.073(3) -0.006(2) 0.000(2) -0.014(2) C60 0.050(2) 0.059(2) 0.057(2) 0.0007(19) -0.0159(19) -0.0190(19) C65 0.072(3) 0.033(2) 0.066(3) -0.0031(18) -0.012(2) -0.0094(19) C66 0.086(3) 0.038(2) 0.063(3) 0.0100(18) -0.019(2) -0.019(2) C67 0.062(3) 0.060(2) 0.035(2) 0.0089(17) -0.0154(18) -0.011(2) C68 0.044(2) 0.066(3) 0.041(2) 0.0019(18) -0.0155(17) -0.0177(19) C69 0.059(2) 0.062(2) 0.0339(19) -0.0089(16) -0.0076(17) -0.034(2) C70 0.068(3) 0.054(2) 0.046(2) -0.0159(17) 0.0016(19) -0.031(2) C71 0.099(4) 0.080(4) 0.107(4) -0.012(3) 0.026(3) -0.044(3) C72 0.052(3) 0.117(5) 0.221(8) -0.015(5) -0.014(4) -0.010(3) C73 0.074(4) 0.168(6) 0.129(5) -0.073(5) 0.017(3) -0.055(4) C74 0.077(4) 0.101(4) 0.114(4) -0.029(3) 0.006(3) -0.047(3) C75 0.082(3) 0.067(3) 0.073(3) 0.017(2) 0.014(3) -0.023(3) C76 0.086(3) 0.055(3) 0.051(2) 0.0116(19) 0.006(2) -0.024(2) C77 0.088(3) 0.047(2) 0.042(2) 0.0057(18) -0.017(2) -0.013(2) C78 0.093(3) 0.054(3) 0.059(3) 0.001(2) -0.028(2) -0.022(2) C79 0.084(3) 0.067(3) 0.101(4) 0.027(3) -0.040(3) -0.039(3) C80 0.061(3) 0.081(3) 0.100(4) 0.031(3) -0.010(3) -0.028(3) C15 0.031(3) 0.031(3) 0.031(3) -0.0001(10) -0.0006(10) -0.0115(14) C16 0.049(6) 0.032(5) 0.028(4) -0.003(3) -0.005(3) -0.025(4) C17 0.026(6) 0.034(5) 0.050(5) -0.009(2) 0.008(5) -0.006(5) C18 0.056(8) 0.043(5) 0.049(6) -0.005(4) -0.004(5) -0.018(5) C19 0.041(4) 0.039(5) 0.050(7) -0.007(5) 0.013(4) 0.003(3) C20 0.043(5) 0.025(5) 0.044(6) -0.004(4) 0.007(4) -0.010(3) C21 0.047(6) 0.032(5) 0.035(7) -0.003(5) -0.006(6) -0.012(3) C22 0.063(6) 0.045(5) 0.046(5) -0.005(4) -0.007(5) -0.016(5) C23 0.052(6) 0.025(6) 0.064(6) -0.005(5) -0.003(4) -0.011(5) C24 0.062(6) 0.040(4) 0.052(5) -0.018(3) -0.016(4) 0.007(3) C25 0.087(3) 0.085(3) 0.087(3) -0.0010(10) -0.0016(10) -0.0299(13) C26 0.126(9) 0.056(5) 0.159(9) -0.013(5) 0.095(8) -0.016(5) C27 0.045(4) 0.045(4) 0.041(5) 0.000(4) -0.003(4) -0.018(3) C28 0.185(14) 0.129(11) 0.062(6) -0.031(7) 0.033(9) -0.116(11) C29 0.074(6) 0.115(8) 0.064(5) -0.019(5) 0.021(4) -0.058(6) O8 0.070(5) 0.079(6) 0.104(7) -0.003(5) -0.041(5) 0.002(4) C61 0.084(7) 0.080(8) 0.187(12) -0.017(8) -0.055(7) 0.004(6) C62 0.109(12) 0.200(15) 0.088(8) 0.027(9) -0.034(9) -0.007(11) C63 0.114(7) 0.116(8) 0.121(8) 0.004(6) -0.038(6) -0.015(6) C64 0.095(7) 0.065(6) 0.089(6) -0.018(4) -0.006(5) -0.013(5) O16 0.136(2) 0.121(2) 0.103(2) 0.0161(16) 0.0176(18) 0.0134(18) C81 0.136(2) 0.123(2) 0.104(2) 0.0166(17) 0.0166(18) 0.0129(19) C82 0.135(2) 0.123(2) 0.106(2) 0.0185(17) 0.0170(19) 0.0112(19) C83 0.137(2) 0.125(2) 0.108(2) 0.0187(17) 0.0154(19) 0.0117(19) C84 0.136(2) 0.123(2) 0.104(2) 0.0174(16) 0.0164(18) 0.0134(19) _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 K1 O8B 2.59(3) . ? K1 O7 2.779(3) . ? K1 O1 2.781(3) . ? K1 O2 2.786(2) . ? K1 O3 2.803(3) . ? K1 O8 2.808(10) . ? K1 O6 2.815(3) . ? K1 O4 2.822(2) . ? K1 O5 2.859(2) . ? K2 O12 2.728(3) 2_765 ? K2 O12 2.728(3) . ? K2 O11 2.745(2) 2_765 ? K2 O11 2.745(2) . ? K2 O10 2.798(2) . ? K2 O10 2.798(2) 2_765 ? K2 O9 2.829(2) 2_765 ? K2 O9 2.829(2) . ? K3 O14 2.776(2) 2_755 ? K3 O14 2.776(2) . ? K3 O16 2.779(4) 2_755 ? K3 O16 2.779(4) . ? K3 O13 2.793(3) 2_755 ? K3 O13 2.793(3) . ? K3 O15 2.824(3) . ? K3 O15 2.824(3) 2_755 ? K3 C84 3.506(6) 2_755 ? O1 C56 1.413(5) . ? O1 C45 1.450(5) . ? O2 C46 1.392(5) . ? O2 C47 1.450(5) . ? O3 C48 1.400(5) . ? O3 C49 1.431(4) . ? O4 C51 1.409(4) . ? O4 C50 1.419(4) . ? O5 C52 1.398(4) . ? O5 C53 1.431(4) . ? O6 C54 1.425(4) . ? O6 C55 1.436(4) . ? O7 C57 1.398(5) . ? O7 C60 1.422(4) . ? O9 C70 1.419(4) 2_765 ? O9 C65 1.428(4) . ? O10 C66 1.412(4) . ? O10 C67 1.429(4) . ? O11 C68 1.413(4) . ? O11 C69 1.434(4) . ? O12 C74 1.398(5) . ? O12 C71 1.411(5) . ? O13 C80 1.420(5) . ? O13 C75 1.429(5) . ? O14 C77 1.429(4) . ? O14 C76 1.440(4) . ? O15 C79 1.413(5) . ? O15 C78 1.433(5) . ? P1 C1 1.797(3) . ? P1 C15B 1.85(2) . ? P1 C15 1.875(11) . ? P2 C11 1.795(3) . ? P2 C30 1.877(3) . ? C1 C2 1.421(4) . ? C1 C14 1.432(4) . ? C2 C3 1.368(4) . ? C3 C4 1.380(4) . ? C4 C5 1.398(4) . ? C5 C14 1.401(4) . ? C5 C6 1.489(4) . ? C6 C7 1.507(4) . ? C7 C12 1.384(4) . ? C7 C8 1.397(4) . ? C8 C9 1.380(4) . ? C9 C10 1.374(4) . ? C10 C11 1.417(4) . ? C11 C12 1.447(4) . ? C12 C13 1.506(4) . ? C13 C14 1.515(4) . ? C30 C31 1.410(4) . ? C30 C35 1.420(4) . ? C31 C32 1.392(4) . ? C31 C36 1.519(4) . ? C32 C33 1.383(5) . ? C33 C34 1.392(4) . ? C33 C39 1.517(5) . ? C34 C35 1.390(4) . ? C35 C42 1.525(4) . ? C36 C37 1.515(5) . ? C36 C38 1.525(5) . ? C39 C40 1.489(6) . ? C39 C41 1.528(6) . ? C42 C43 1.503(6) . ? C42 C44 1.523(5) . ? C45 C46 1.472(7) . ? C47 C48 1.482(6) . ? C49 C50 1.443(6) . ? C51 C52 1.474(5) . ? C53 C54 1.478(5) . ? C55 C56 1.492(6) . ? C57 C58 1.515(7) . ? C58 C59 1.523(6) . ? C59 C60 1.494(5) . ? C65 C66 1.490(5) . ? C67 C68 1.486(5) . ? C69 C70 1.484(5) . ? C70 O9 1.418(4) 2_765 ? C71 C72 1.489(7) . ? C72 C73 1.483(8) . ? C73 C74 1.406(6) . ? C75 C76 1.486(6) . ? C77 C78 1.476(5) . ? C79 C80 1.489(6) 2_755 ? C80 C79 1.489(6) 2_755 ? C15 C20 1.446(17) . ? C15 C16 1.466(16) . ? C16 C17 1.316(15) . ? C16 C21 1.48(2) . ? C17 C18 1.403(18) . ? C18 C19 1.415(18) . ? C18 C24 1.523(15) . ? C19 C20 1.415(16) . ? C20 C27 1.514(15) . ? C21 C23 1.44(2) . ? C21 C22 1.56(2) . ? C24 C26 1.380(12) . ? C24 C25 1.569(12) . ? C27 C28 1.502(13) . ? C27 C29 1.511(10) . ? O8 C61 1.436(12) . ? O8 C64 1.460(14) . ? C61 C62 1.362(15) . ? C62 C63 1.477(16) . ? C63 C64 1.433(12) . ? C15B C16B 1.34(3) . ? C15B C20B 1.34(4) . ? C16B C17B 1.57(3) . ? C16B C21B 1.64(5) . ? C17B C18B 1.32(3) . ? C18B C19B 1.35(4) . ? C18B C24B 1.51(3) . ? C19B C20B 1.39(4) . ? C20B C27B 1.49(3) . ? C21B C22B 1.48(4) . ? C21B C23B 1.72(5) . ? C24B C25B 1.49(2) . ? C24B C26B 1.72(2) . ? C27B C28B 1.48(2) . ? C27B C29B 1.51(2) . ? O8B C64B 1.29(5) . ? O8B C61B 1.52(4) . ? C61B C62B 1.57(4) . ? C62B C63B 1.45(4) . ? C63B C64B 1.61(4) . ? O16 C84 1.338(6) . ? O16 C81 1.457(6) . ? C81 C82 1.387(8) . ? C82 C83 1.482(7) . ? C83 C84 1.451(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8B K1 O7 167.6(6) . . ? O8B K1 O1 76.9(8) . . ? O7 K1 O1 100.21(8) . . ? O8B K1 O2 87.0(6) . . ? O7 K1 O2 81.14(8) . . ? O1 K1 O2 61.08(8) . . ? O8B K1 O3 89.0(7) . . ? O7 K1 O3 82.35(8) . . ? O1 K1 O3 122.32(9) . . ? O2 K1 O3 62.57(8) . . ? O8B K1 O8 9.8(8) . . ? O7 K1 O8 157.9(3) . . ? O1 K1 O8 76.7(2) . . ? O2 K1 O8 78.2(3) . . ? O3 K1 O8 81.1(3) . . ? O8B K1 O6 100.3(7) . . ? O7 K1 O6 88.49(8) . . ? O1 K1 O6 60.87(8) . . ? O2 K1 O6 117.70(8) . . ? O3 K1 O6 170.70(8) . . ? O8 K1 O6 108.2(3) . . ? O8B K1 O4 108.8(8) . . ? O7 K1 O4 74.53(8) . . ? O1 K1 O4 174.14(8) . . ? O2 K1 O4 119.75(8) . . ? O3 K1 O4 60.16(8) . . ? O8 K1 O4 109.2(2) . . ? O6 K1 O4 115.78(8) . . ? O8B K1 O5 105.5(6) . . ? O7 K1 O5 86.44(8) . . ? O1 K1 O5 119.91(8) . . ? O2 K1 O5 167.43(7) . . ? O3 K1 O5 117.76(8) . . ? O8 K1 O5 114.3(3) . . ? O6 K1 O5 59.70(7) . . ? O4 K1 O5 57.84(7) . . ? O12 K2 O12 180.00(12) 2_765 . ? O12 K2 O11 88.82(8) 2_765 2_765 ? O12 K2 O11 91.18(8) . 2_765 ? O12 K2 O11 91.18(8) 2_765 . ? O12 K2 O11 88.82(8) . . ? O11 K2 O11 179.998(1) 2_765 . ? O12 K2 O10 83.03(8) 2_765 . ? O12 K2 O10 96.97(8) . . ? O11 K2 O10 118.75(7) 2_765 . ? O11 K2 O10 61.25(7) . . ? O12 K2 O10 96.97(8) 2_765 2_765 ? O12 K2 O10 83.03(8) . 2_765 ? O11 K2 O10 61.24(7) 2_765 2_765 ? O11 K2 O10 118.75(7) . 2_765 ? O10 K2 O10 179.999(1) . 2_765 ? O12 K2 O9 85.13(8) 2_765 2_765 ? O12 K2 O9 94.88(8) . 2_765 ? O11 K2 O9 119.28(6) 2_765 2_765 ? O11 K2 O9 60.72(6) . 2_765 ? O10 K2 O9 120.25(7) . 2_765 ? O10 K2 O9 59.75(7) 2_765 2_765 ? O12 K2 O9 94.87(8) 2_765 . ? O12 K2 O9 85.13(8) . . ? O11 K2 O9 60.72(6) 2_765 . ? O11 K2 O9 119.28(6) . . ? O10 K2 O9 59.75(7) . . ? O10 K2 O9 120.25(7) 2_765 . ? O9 K2 O9 180.000(1) 2_765 . ? O14 K3 O14 180.0 2_755 . ? O14 K3 O16 81.39(9) 2_755 2_755 ? O14 K3 O16 98.61(9) . 2_755 ? O14 K3 O16 98.61(9) 2_755 . ? O14 K3 O16 81.39(9) . . ? O16 K3 O16 179.999(1) 2_755 . ? O14 K3 O13 60.28(8) 2_755 2_755 ? O14 K3 O13 119.72(8) . 2_755 ? O16 K3 O13 103.61(11) 2_755 2_755 ? O16 K3 O13 76.39(11) . 2_755 ? O14 K3 O13 119.72(8) 2_755 . ? O14 K3 O13 60.28(8) . . ? O16 K3 O13 76.39(11) 2_755 . ? O16 K3 O13 103.62(11) . . ? O13 K3 O13 180.0 2_755 . ? O14 K3 O15 119.23(8) 2_755 . ? O14 K3 O15 60.77(8) . . ? O16 K3 O15 99.96(11) 2_755 . ? O16 K3 O15 80.04(11) . . ? O13 K3 O15 60.55(8) 2_755 . ? O13 K3 O15 119.45(8) . . ? O14 K3 O15 60.77(8) 2_755 2_755 ? O14 K3 O15 119.23(8) . 2_755 ? O16 K3 O15 80.04(11) 2_755 2_755 ? O16 K3 O15 99.96(11) . 2_755 ? O13 K3 O15 119.45(8) 2_755 2_755 ? O13 K3 O15 60.55(8) . 2_755 ? O15 K3 O15 180.0 . 2_755 ? O14 K3 C84 99.95(11) 2_755 2_755 ? O14 K3 C84 80.05(11) . 2_755 ? O16 K3 C84 20.72(13) 2_755 2_755 ? O16 K3 C84 159.28(13) . 2_755 ? O13 K3 C84 105.18(13) 2_755 2_755 ? O13 K3 C84 74.82(13) . 2_755 ? O15 K3 C84 82.91(13) . 2_755 ? O15 K3 C84 97.09(13) 2_755 2_755 ? C56 O1 C45 114.7(4) . . ? C56 O1 K1 115.8(2) . . ? C45 O1 K1 114.1(2) . . ? C46 O2 C47 113.1(3) . . ? C46 O2 K1 112.3(2) . . ? C47 O2 K1 110.4(2) . . ? C48 O3 C49 111.5(3) . . ? C48 O3 K1 110.4(2) . . ? C49 O3 K1 112.7(2) . . ? C51 O4 C50 113.5(3) . . ? C51 O4 K1 116.8(2) . . ? C50 O4 K1 113.2(2) . . ? C52 O5 C53 112.7(3) . . ? C52 O5 K1 117.0(2) . . ? C53 O5 K1 113.74(19) . . ? C54 O6 C55 111.4(3) . . ? C54 O6 K1 114.9(2) . . ? C55 O6 K1 111.3(2) . . ? C57 O7 C60 105.3(3) . . ? C57 O7 K1 112.5(2) . . ? C60 O7 K1 136.5(2) . . ? C70 O9 C65 111.9(3) 2_765 . ? C70 O9 K2 111.88(19) 2_765 . ? C65 O9 K2 115.29(19) . . ? C66 O10 C67 111.9(3) . . ? C66 O10 K2 115.2(2) . . ? C67 O10 K2 113.78(19) . . ? C68 O11 C69 110.9(2) . . ? C68 O11 K2 115.08(18) . . ? C69 O11 K2 117.36(17) . . ? C74 O12 C71 108.9(4) . . ? C74 O12 K2 117.1(3) . . ? C71 O12 K2 117.7(3) . . ? C80 O13 C75 112.4(3) . . ? C80 O13 K3 114.3(2) . . ? C75 O13 K3 115.1(2) . . ? C77 O14 C76 111.8(3) . . ? C77 O14 K3 115.5(2) . . ? C76 O14 K3 115.8(2) . . ? C79 O15 C78 111.7(3) . . ? C79 O15 K3 112.3(2) . . ? C78 O15 K3 111.7(2) . . ? C1 P1 C15B 101.3(6) . . ? C1 P1 C15 102.2(3) . . ? C15B P1 C15 7.1(8) . . ? C11 P2 C30 102.18(14) . . ? C2 C1 C14 116.4(3) . . ? C2 C1 P1 123.0(2) . . ? C14 C1 P1 120.6(2) . . ? C3 C2 C1 122.3(3) . . ? C2 C3 C4 120.9(3) . . ? C3 C4 C5 119.4(3) . . ? C4 C5 C14 120.8(3) . . ? C4 C5 C6 118.8(3) . . ? C14 C5 C6 120.3(3) . . ? C5 C6 C7 115.1(3) . . ? C12 C7 C8 122.3(3) . . ? C12 C7 C6 119.9(3) . . ? C8 C7 C6 117.8(3) . . ? C9 C8 C7 118.5(3) . . ? C10 C9 C8 121.0(3) . . ? C9 C10 C11 122.4(3) . . ? C10 C11 C12 116.1(3) . . ? C10 C11 P2 123.3(2) . . ? C12 C11 P2 120.6(2) . . ? C7 C12 C11 119.6(3) . . ? C7 C12 C13 120.7(3) . . ? C11 C12 C13 119.7(3) . . ? C12 C13 C14 116.5(2) . . ? C5 C14 C1 120.1(3) . . ? C5 C14 C13 119.5(3) . . ? C1 C14 C13 120.4(3) . . ? C31 C30 C35 116.3(3) . . ? C31 C30 P2 120.9(2) . . ? C35 C30 P2 122.6(2) . . ? C32 C31 C30 121.0(3) . . ? C32 C31 C36 116.5(3) . . ? C30 C31 C36 122.5(3) . . ? C33 C32 C31 122.6(3) . . ? C32 C33 C34 116.9(3) . . ? C32 C33 C39 121.6(3) . . ? C34 C33 C39 121.5(3) . . ? C35 C34 C33 122.1(3) . . ? C34 C35 C30 121.1(3) . . ? C34 C35 C42 117.6(3) . . ? C30 C35 C42 121.2(3) . . ? C37 C36 C31 111.7(3) . . ? C37 C36 C38 112.1(3) . . ? C31 C36 C38 110.2(3) . . ? C40 C39 C33 111.6(3) . . ? C40 C39 C41 108.9(4) . . ? C33 C39 C41 111.6(3) . . ? C43 C42 C44 110.0(4) . . ? C43 C42 C35 110.3(3) . . ? C44 C42 C35 112.3(3) . . ? O1 C45 C46 110.1(4) . . ? O2 C46 C45 109.1(3) . . ? O2 C47 C48 109.6(3) . . ? O3 C48 C47 109.4(4) . . ? O3 C49 C50 110.4(3) . . ? O4 C50 C49 107.3(3) . . ? O4 C51 C52 108.1(3) . . ? O5 C52 C51 109.2(3) . . ? O5 C53 C54 109.0(3) . . ? O6 C54 C53 108.7(3) . . ? O6 C55 C56 108.0(3) . . ? O1 C56 C55 110.4(3) . . ? O7 C57 C58 105.8(4) . . ? C57 C58 C59 103.2(4) . . ? C60 C59 C58 104.5(4) . . ? O7 C60 C59 106.0(3) . . ? O9 C65 C66 108.4(3) . . ? O10 C66 C65 109.4(3) . . ? O10 C67 C68 109.9(3) . . ? O11 C68 C67 109.8(3) . . ? O11 C69 C70 108.5(3) . . ? O9 C70 C69 110.3(3) 2_765 . ? O12 C71 C72 106.1(4) . . ? C73 C72 C71 105.1(4) . . ? C74 C73 C72 104.7(5) . . ? O12 C74 C73 108.7(4) . . ? O13 C75 C76 109.1(3) . . ? O14 C76 C75 107.9(3) . . ? O14 C77 C78 108.7(3) . . ? O15 C78 C77 109.4(3) . . ? O15 C79 C80 108.8(4) . 2_755 ? O13 C80 C79 108.3(4) . 2_755 ? C20 C15 C16 115.1(10) . . ? C20 C15 P1 119.9(8) . . ? C16 C15 P1 124.6(7) . . ? C17 C16 C15 121.8(11) . . ? C17 C16 C21 119.2(11) . . ? C15 C16 C21 118.9(11) . . ? C16 C17 C18 123.7(11) . . ? C17 C18 C19 118.1(11) . . ? C17 C18 C24 122.3(10) . . ? C19 C18 C24 119.6(11) . . ? C20 C19 C18 119.9(11) . . ? C19 C20 C15 121.3(11) . . ? C19 C20 C27 117.7(11) . . ? C15 C20 C27 120.9(9) . . ? C23 C21 C16 118.1(13) . . ? C23 C21 C22 108.5(14) . . ? C16 C21 C22 107.7(13) . . ? C26 C24 C18 117.5(9) . . ? C26 C24 C25 107.4(8) . . ? C18 C24 C25 108.8(8) . . ? C28 C27 C29 110.4(7) . . ? C28 C27 C20 110.5(8) . . ? C29 C27 C20 115.1(7) . . ? C61 O8 C64 106.4(9) . . ? C61 O8 K1 130.4(8) . . ? C64 O8 K1 122.4(6) . . ? C62 C61 O8 109.1(10) . . ? C61 C62 C63 108.0(9) . . ? C64 C63 C62 105.3(9) . . ? C63 C64 O8 107.6(9) . . ? C16B C15B C20B 120(2) . . ? C16B C15B P1 116.9(16) . . ? C20B C15B P1 122.3(17) . . ? C15B C16B C17B 119.4(19) . . ? C15B C16B C21B 129(2) . . ? C17B C16B C21B 110(2) . . ? C18B C17B C16B 119(2) . . ? C17B C18B C19B 114(2) . . ? C17B C18B C24B 120(2) . . ? C19B C18B C24B 126(2) . . ? C18B C19B C20B 131(3) . . ? C15B C20B C19B 116(2) . . ? C15B C20B C27B 125(2) . . ? C19B C20B C27B 119(2) . . ? C22B C21B C16B 113(3) . . ? C22B C21B C23B 114(3) . . ? C16B C21B C23B 106(2) . . ? C25B C24B C18B 115.8(17) . . ? C25B C24B C26B 97.0(13) . . ? C18B C24B C26B 102.7(13) . . ? C28B C27B C20B 113.7(17) . . ? C28B C27B C29B 110.6(13) . . ? C20B C27B C29B 107.1(16) . . ? C64B O8B C61B 102(3) . . ? C64B O8B K1 129(3) . . ? C61B O8B K1 124(2) . . ? O8B C61B C62B 101(2) . . ? C63B C62B C61B 103(3) . . ? C62B C63B C64B 90(3) . . ? O8B C64B C63B 117(3) . . ? C84 O16 C81 106.5(5) . . ? C84 O16 K3 112.0(4) . . ? C81 O16 K3 120.1(4) . . ? C82 C81 O16 105.0(5) . . ? C81 C82 C83 103.5(6) . . ? C84 C83 C82 103.7(5) . . ? O16 C84 C83 109.2(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.892 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.052 # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 1.000 645 134 ' ' _platon_squeeze_details ; The structure contained two severely disordered THF solvent molecules in the asymmetric unit, for which no suitable model could be found. The electron density associated with the disordered regions was removed from the reflection file using the SQUEEZE subroutine of PLATON, leaving a void of ca. 645 A^3. Accordingly, two THF molecules are included in _chemical_formula_moiety (and _sum), and calculations of Mr, density, mu, and F(OOO) to more accurately reflect the unit cell properties. ; _iucr_refine_instructions_details ; TITL PH09028 in P-1 CELL 0.71073 13.3096 17.9904 21.5418 87.891 87.743 68.936 ZERR 2.00 0.0019 0.0026 0.0031 0.002 0.002 0.002 LATT 1 SFAC C H O P K UNIT 168 272 32 4 4 L.S. 12 BOND acta isor 0.00001 c25 C15 delu 0.00001 o16 c81 c82 c83 c84 simu 0.00001 o16 c81 c82 c83 c84 FMAP 2 PLAN 5 SIZE 0.05 0.389 0.66 FREE K3 C84 TEMP -100 WGHT 0.095700 FVAR 0.92792 0.65182 0.74784 MOLE 1 K1 5 0.232314 0.569027 0.625907 11.00000 0.04035 0.07120 = 0.03396 0.00202 -0.00525 -0.02535 K2 5 1.000000 0.500000 0.000000 10.50000 0.03487 0.03869 = 0.03163 -0.00086 -0.00826 -0.01321 K3 5 1.000000 0.000000 0.000000 10.50000 0.07051 0.04487 = 0.04178 0.00306 -0.00152 -0.01455 O1 3 0.154163 0.503317 0.532679 11.00000 0.04596 0.08811 = 0.05039 -0.02458 -0.00719 -0.01459 O2 3 0.337838 0.545499 0.510004 11.00000 0.05331 0.06933 = 0.03641 0.00844 0.00070 -0.00809 O3 3 0.383613 0.642483 0.601595 11.00000 0.04630 0.05796 = 0.06623 0.00636 0.01292 -0.01456 O4 3 0.321737 0.619671 0.725369 11.00000 0.04989 0.06447 = 0.06038 -0.00227 -0.00850 -0.02948 O5 3 0.160393 0.560916 0.751934 11.00000 0.04235 0.06135 = 0.04298 0.00270 -0.00547 -0.01625 O6 3 0.108147 0.475058 0.659086 11.00000 0.03612 0.07413 = 0.06046 -0.00701 -0.00211 -0.02324 O7 3 0.415227 0.439861 0.656922 11.00000 0.06456 0.07673 = 0.07969 0.00064 -0.03462 -0.02085 O9 3 1.026674 0.347312 -0.043312 11.00000 0.06038 0.04303 = 0.04180 -0.00624 -0.00346 -0.01616 O10 3 1.129238 0.362923 0.063970 11.00000 0.06286 0.04364 = 0.04220 0.00525 -0.01314 -0.01577 O11 3 1.058337 0.514103 0.118576 11.00000 0.04246 0.05172 = 0.03371 -0.00086 -0.01301 -0.02158 O12 3 0.806548 0.500592 0.047257 11.00000 0.04762 0.08100 = 0.09423 -0.01224 0.00416 -0.02976 O13 3 0.859120 -0.073313 0.046688 11.00000 0.06533 0.05790 = 0.06438 0.01598 -0.00357 -0.01932 O14 3 1.008077 -0.049235 0.123957 11.00000 0.08251 0.03994 = 0.04400 0.00685 -0.00506 -0.01399 O15 3 1.179802 -0.009294 0.069501 11.00000 0.07909 0.04690 = 0.06085 0.00952 -0.01726 -0.02374 P1 4 0.132695 0.654476 0.311290 11.00000 0.04021 0.03032 = 0.03593 0.00136 0.00257 -0.01176 P2 4 0.257205 0.347534 0.331635 11.00000 0.03860 0.02958 = 0.03340 0.00159 -0.00122 -0.01148 C1 1 0.210610 0.641430 0.239804 11.00000 0.03149 0.03562 = 0.02801 0.00053 -0.00866 -0.01798 C2 1 0.201334 0.704940 0.196501 11.00000 0.04252 0.03185 = 0.03040 0.00227 -0.00662 -0.01385 AFIX 43 H2 2 0.150774 0.756515 0.205149 11.00000 -1.20000 AFIX 0 C3 1 0.262700 0.694370 0.142791 11.00000 0.06133 0.03616 = 0.03138 0.01054 -0.01069 -0.02347 AFIX 43 H3 2 0.252838 0.738212 0.114690 11.00000 -1.20000 AFIX 0 C4 1 0.338710 0.620917 0.128875 11.00000 0.04460 0.04422 = 0.02971 0.00243 0.00209 -0.02022 AFIX 43 H4 2 0.382724 0.614577 0.092200 11.00000 -1.20000 AFIX 0 C5 1 0.350320 0.555928 0.169265 11.00000 0.03795 0.03320 = 0.02830 -0.00154 -0.00246 -0.01631 C6 1 0.436997 0.478148 0.155650 11.00000 0.04647 0.04187 = 0.03497 -0.00009 0.00877 -0.01701 AFIX 23 H6A 2 0.505177 0.478456 0.172215 11.00000 -1.20000 H6B 2 0.446934 0.473190 0.110003 11.00000 -1.20000 AFIX 0 C7 1 0.416807 0.405858 0.182045 11.00000 0.03055 0.03535 = 0.03162 -0.00006 -0.00300 -0.00990 C8 1 0.467373 0.333617 0.152322 11.00000 0.04027 0.04487 = 0.03663 -0.00608 0.00686 -0.01019 AFIX 43 H8 2 0.508489 0.331247 0.114890 11.00000 -1.20000 AFIX 0 C9 1 0.456254 0.265741 0.178568 11.00000 0.05370 0.03317 = 0.04765 -0.01083 0.00681 -0.00727 AFIX 43 H9 2 0.490873 0.216043 0.159170 11.00000 -1.20000 AFIX 0 C10 1 0.395903 0.268943 0.232303 11.00000 0.04782 0.03031 = 0.04098 0.00078 -0.00132 -0.01224 AFIX 43 H10 2 0.391775 0.220836 0.249790 11.00000 -1.20000 AFIX 0 C11 1 0.339564 0.341391 0.262615 11.00000 0.02810 0.03008 = 0.03067 0.00082 -0.00711 -0.00873 C12 1 0.352995 0.412022 0.235293 11.00000 0.02914 0.03068 = 0.02538 -0.00061 -0.00661 -0.00908 C13 1 0.294459 0.491817 0.263763 11.00000 0.02829 0.03401 = 0.02513 0.00204 -0.00562 -0.01271 AFIX 23 H13A 2 0.331307 0.494448 0.302206 11.00000 -1.20000 H13B 2 0.220698 0.494739 0.276053 11.00000 -1.20000 AFIX 0 C14 1 0.285736 0.564570 0.223442 11.00000 0.03076 0.03127 = 0.02579 -0.00181 -0.00695 -0.01474 C30 1 0.279208 0.240021 0.349609 11.00000 0.03453 0.03385 = 0.03438 0.00317 -0.00201 -0.01247 C31 1 0.345171 0.198621 0.398666 11.00000 0.04327 0.03449 = 0.04332 0.00367 -0.00822 -0.01438 C32 1 0.352475 0.121691 0.416402 11.00000 0.06233 0.03966 = 0.04957 0.01250 -0.02097 -0.02047 AFIX 43 H32 2 0.397197 0.095766 0.449915 11.00000 -1.20000 AFIX 0 C33 1 0.297199 0.081523 0.387161 11.00000 0.06070 0.03839 = 0.04890 0.00842 -0.01505 -0.01997 C34 1 0.232201 0.121659 0.338464 11.00000 0.05536 0.03809 = 0.05121 0.00434 -0.01382 -0.02248 AFIX 43 H34 2 0.192622 0.095862 0.317702 11.00000 -1.20000 AFIX 0 C35 1 0.223385 0.198319 0.319254 11.00000 0.04172 0.03843 = 0.03945 0.00609 -0.00864 -0.01489 C36 1 0.412614 0.234224 0.434284 11.00000 0.05072 0.04105 = 0.05605 0.01018 -0.02011 -0.02065 AFIX 13 H36 2 0.398713 0.289246 0.416958 11.00000 -1.20000 AFIX 0 C37 1 0.380512 0.241332 0.502675 11.00000 0.11603 0.06752 = 0.05081 0.00277 -0.02255 -0.04796 AFIX 137 H37A 2 0.303845 0.273787 0.507386 11.00000 -1.50000 H37B 2 0.423225 0.266668 0.523822 11.00000 -1.50000 H37C 2 0.393698 0.188138 0.521066 11.00000 -1.50000 AFIX 0 C38 1 0.532156 0.186170 0.423822 11.00000 0.05856 0.05537 = 0.10384 0.00844 -0.02654 -0.02075 AFIX 137 H38A 2 0.574937 0.214226 0.441421 11.00000 -1.50000 H38B 2 0.548511 0.179832 0.379144 11.00000 -1.50000 H38C 2 0.549817 0.133580 0.444179 11.00000 -1.50000 AFIX 0 C39 1 0.306112 -0.002154 0.407564 11.00000 0.09051 0.03914 = 0.06511 0.01666 -0.02317 -0.03139 AFIX 13 H39 2 0.260177 -0.019660 0.380233 11.00000 -1.20000 AFIX 0 C40 1 0.267149 -0.004903 0.473064 11.00000 0.16036 0.05963 = 0.10270 0.02418 -0.00270 -0.04968 AFIX 137 H40A 2 0.309676 0.013794 0.500491 11.00000 -1.50000 H40B 2 0.275007 -0.059781 0.484938 11.00000 -1.50000 H40C 2 0.191124 0.029471 0.476866 11.00000 -1.50000 AFIX 0 C41 1 0.421901 -0.061023 0.401233 11.00000 0.10851 0.04341 = 0.12955 0.02197 -0.03764 -0.02541 AFIX 137 H41A 2 0.468541 -0.044253 0.427073 11.00000 -1.50000 H41B 2 0.446645 -0.062260 0.357699 11.00000 -1.50000 H41C 2 0.424759 -0.114301 0.414870 11.00000 -1.50000 AFIX 0 C42 1 0.148642 0.237027 0.265984 11.00000 0.06335 0.04065 = 0.05587 0.01292 -0.02832 -0.02672 AFIX 13 H42 2 0.163607 0.285457 0.251159 11.00000 -1.20000 AFIX 0 C43 1 0.033048 0.263211 0.288418 11.00000 0.05452 0.09419 = 0.14761 0.04989 -0.03716 -0.02144 AFIX 137 H43A 2 0.016717 0.216668 0.303599 11.00000 -1.50000 H43B 2 -0.014068 0.289317 0.254076 11.00000 -1.50000 H43C 2 0.021137 0.300720 0.322206 11.00000 -1.50000 AFIX 0 C44 1 0.166976 0.181935 0.211268 11.00000 0.17578 0.06183 = 0.05986 0.01120 -0.05882 -0.05147 AFIX 137 H44A 2 0.241498 0.167433 0.195560 11.00000 -1.50000 H44B 2 0.117618 0.209283 0.178181 11.00000 -1.50000 H44C 2 0.153607 0.133647 0.224865 11.00000 -1.50000 AFIX 0 C45 1 0.224899 0.481393 0.478145 11.00000 0.04027 0.14407 = 0.05540 -0.05936 -0.01220 -0.00056 AFIX 23 H45A 2 0.183956 0.475023 0.442615 11.00000 -1.20000 H45B 2 0.283735 0.429842 0.486180 11.00000 -1.20000 AFIX 0 C46 1 0.270741 0.543296 0.462714 11.00000 0.05046 0.12326 = 0.03861 -0.00160 0.00101 -0.00053 AFIX 23 H46A 2 0.312305 0.531258 0.422862 11.00000 -1.20000 H46B 2 0.212100 0.595785 0.458113 11.00000 -1.20000 AFIX 0 C47 1 0.389240 0.603534 0.498085 11.00000 0.09327 0.05162 = 0.06966 0.01434 0.04721 -0.01194 AFIX 23 H47A 2 0.333813 0.656861 0.490564 11.00000 -1.20000 H47B 2 0.436834 0.589033 0.460532 11.00000 -1.20000 AFIX 0 C48 1 0.453309 0.605655 0.552293 11.00000 0.07157 0.06975 = 0.08811 -0.00283 0.01997 -0.03960 AFIX 23 H48A 2 0.498784 0.550739 0.564950 11.00000 -1.20000 H48B 2 0.501158 0.635611 0.540994 11.00000 -1.20000 AFIX 0 C49 1 0.441730 0.645152 0.655451 11.00000 0.04999 0.07509 = 0.08862 0.02954 -0.02728 -0.03291 AFIX 23 H49A 2 0.485354 0.678899 0.646307 11.00000 -1.20000 H49B 2 0.491329 0.590780 0.666474 11.00000 -1.20000 AFIX 0 C50 1 0.368191 0.677082 0.707101 11.00000 0.05103 0.05960 = 0.08056 0.00680 -0.02128 -0.02460 AFIX 23 H50A 2 0.407198 0.687380 0.742028 11.00000 -1.20000 H50B 2 0.311410 0.727837 0.694531 11.00000 -1.20000 AFIX 0 C51 1 0.259106 0.638089 0.780858 11.00000 0.05405 0.08286 = 0.05124 -0.02184 -0.01063 -0.01321 AFIX 23 H51A 2 0.195073 0.687025 0.774677 11.00000 -1.20000 H51B 2 0.301863 0.647366 0.814300 11.00000 -1.20000 AFIX 0 C52 1 0.225399 0.570325 0.798146 11.00000 0.05841 0.08731 = 0.03645 -0.00208 -0.00471 -0.02143 AFIX 23 H52A 2 0.289600 0.521117 0.802737 11.00000 -1.20000 H52B 2 0.184865 0.580246 0.838398 11.00000 -1.20000 AFIX 0 C53 1 0.124462 0.495801 0.765119 11.00000 0.04956 0.06512 = 0.04990 0.00754 0.01136 -0.01341 AFIX 23 H53A 2 0.087503 0.502166 0.806444 11.00000 -1.20000 H53B 2 0.186938 0.445022 0.765702 11.00000 -1.20000 AFIX 0 C54 1 0.049617 0.494310 0.716719 11.00000 0.04391 0.06010 = 0.07267 0.00331 0.01154 -0.02255 AFIX 23 H54A 2 0.016864 0.454036 0.728037 11.00000 -1.20000 H54B 2 -0.008869 0.547019 0.713057 11.00000 -1.20000 AFIX 0 C55 1 0.039272 0.473873 0.609762 11.00000 0.04400 0.07480 = 0.08468 -0.00510 -0.01761 -0.02714 AFIX 23 H55A 2 -0.014832 0.527819 0.602523 11.00000 -1.20000 H55B 2 0.000821 0.437069 0.620900 11.00000 -1.20000 AFIX 0 C56 1 0.108014 0.446653 0.552586 11.00000 0.05309 0.07809 = 0.08612 -0.02806 -0.03149 -0.01514 AFIX 23 H56A 2 0.165857 0.394824 0.561333 11.00000 -1.20000 H56B 2 0.063817 0.439110 0.519184 11.00000 -1.20000 AFIX 0 C57 1 0.403958 0.366846 0.647319 11.00000 0.07065 0.08770 = 0.11883 -0.02859 -0.03490 -0.02352 AFIX 23 H57A 2 0.460412 0.334754 0.617790 11.00000 -1.20000 H57B 2 0.332502 0.375259 0.630395 11.00000 -1.20000 AFIX 0 C58 1 0.415515 0.325233 0.710515 11.00000 0.05164 0.06408 = 0.17933 -0.01085 -0.00850 -0.02803 AFIX 23 H58A 2 0.453471 0.267026 0.706988 11.00000 -1.20000 H58B 2 0.344309 0.335393 0.731297 11.00000 -1.20000 AFIX 0 C59 1 0.481885 0.362546 0.745596 11.00000 0.05455 0.05493 = 0.07253 -0.00588 0.00047 -0.01406 AFIX 23 H59A 2 0.442743 0.388164 0.783727 11.00000 -1.20000 H59B 2 0.551856 0.321922 0.757250 11.00000 -1.20000 AFIX 0 C60 1 0.497993 0.423000 0.700881 11.00000 0.04978 0.05904 = 0.05717 0.00071 -0.01591 -0.01899 AFIX 23 H60A 2 0.492240 0.471882 0.722735 11.00000 -1.20000 H60B 2 0.569837 0.401540 0.679954 11.00000 -1.20000 AFIX 0 C65 1 1.113969 0.282969 -0.017403 11.00000 0.07242 0.03256 = 0.06649 -0.00310 -0.01170 -0.00940 AFIX 23 H65A 2 1.183286 0.283394 -0.035526 11.00000 -1.20000 H65B 2 1.107332 0.231520 -0.026859 11.00000 -1.20000 AFIX 0 C66 1 1.110770 0.292588 0.051124 11.00000 0.08584 0.03802 = 0.06344 0.01001 -0.01947 -0.01919 AFIX 23 H66A 2 1.039612 0.295605 0.068736 11.00000 -1.20000 H66B 2 1.166645 0.246051 0.070541 11.00000 -1.20000 AFIX 0 C67 1 1.132707 0.373235 0.129210 11.00000 0.06246 0.05956 = 0.03536 0.00889 -0.01542 -0.01148 AFIX 23 H67A 2 1.192877 0.328320 0.147165 11.00000 -1.20000 H67B 2 1.064747 0.373530 0.149803 11.00000 -1.20000 AFIX 0 C68 1 1.147769 0.449556 0.140404 11.00000 0.04429 0.06556 = 0.04065 0.00190 -0.01555 -0.01769 AFIX 23 H68A 2 1.155249 0.454751 0.185423 11.00000 -1.20000 H68B 2 1.214381 0.450077 0.118573 11.00000 -1.20000 AFIX 0 C69 1 1.065801 0.588702 0.134170 11.00000 0.05950 0.06230 = 0.03388 -0.00893 -0.00760 -0.03354 AFIX 23 H69A 2 1.133117 0.592876 0.116002 11.00000 -1.20000 H69B 2 1.066909 0.592430 0.179858 11.00000 -1.20000 AFIX 0 C70 1 0.971197 0.654097 0.109151 11.00000 0.06756 0.05375 = 0.04561 -0.01595 0.00156 -0.03085 AFIX 23 H70A 2 0.904124 0.648051 0.125873 11.00000 -1.20000 H70B 2 0.971895 0.705980 0.122493 11.00000 -1.20000 AFIX 0 C71 1 0.725229 0.575116 0.058781 11.00000 0.09852 0.07985 = 0.10748 -0.01161 0.02598 -0.04404 AFIX 23 H71A 2 0.737642 0.617436 0.032443 11.00000 -1.20000 H71B 2 0.724183 0.588921 0.102927 11.00000 -1.20000 AFIX 0 C72 1 0.621789 0.566756 0.043335 11.00000 0.05206 0.11702 = 0.22077 -0.01462 -0.01407 -0.00987 AFIX 23 H72A 2 0.568542 0.584259 0.078186 11.00000 -1.20000 H72B 2 0.591403 0.598948 0.005673 11.00000 -1.20000 AFIX 0 C73 1 0.649635 0.480665 0.032352 11.00000 0.07439 0.16794 = 0.12905 -0.07256 0.01728 -0.05526 AFIX 23 H73A 2 0.632643 0.453252 0.069753 11.00000 -1.20000 H73B 2 0.609643 0.472657 -0.003028 11.00000 -1.20000 AFIX 0 C74 1 0.761083 0.451907 0.018921 11.00000 0.07716 0.10058 = 0.11371 -0.02907 0.00633 -0.04732 AFIX 23 H74A 2 0.794125 0.396345 0.034790 11.00000 -1.20000 H74B 2 0.774515 0.452518 -0.026591 11.00000 -1.20000 AFIX 0 C75 1 0.848333 -0.076103 0.112896 11.00000 0.08199 0.06687 = 0.07311 0.01663 0.01351 -0.02309 AFIX 23 H75A 2 0.809041 -0.111811 0.125775 11.00000 -1.20000 H75B 2 0.806781 -0.022184 0.128272 11.00000 -1.20000 AFIX 0 C76 1 0.957194 -0.106050 0.139771 11.00000 0.08567 0.05544 = 0.05095 0.01161 0.00617 -0.02369 AFIX 23 H76A 2 0.951274 -0.112118 0.185487 11.00000 -1.20000 H76B 2 1.000454 -0.158653 0.122670 11.00000 -1.20000 AFIX 0 C77 1 1.110898 -0.070612 0.151485 11.00000 0.08812 0.04691 = 0.04215 0.00571 -0.01704 -0.01282 AFIX 23 H77A 2 1.159714 -0.122719 0.136014 11.00000 -1.20000 H77B 2 1.103114 -0.075250 0.197211 11.00000 -1.20000 AFIX 0 C78 1 1.156208 -0.008474 0.135015 11.00000 0.09335 0.05402 = 0.05879 0.00135 -0.02830 -0.02242 AFIX 23 H78A 2 1.103856 0.044420 0.146569 11.00000 -1.20000 H78B 2 1.222847 -0.018545 0.158132 11.00000 -1.20000 AFIX 0 C79 1 1.222059 0.050046 0.051018 11.00000 0.08370 0.06653 = 0.10051 0.02709 -0.03995 -0.03948 AFIX 23 H79A 2 1.290213 0.040655 0.072379 11.00000 -1.20000 H79B 2 1.170334 0.103214 0.062444 11.00000 -1.20000 AFIX 0 C80 1 0.757986 -0.047076 0.017523 11.00000 0.06066 0.08076 = 0.10038 0.03140 -0.00957 -0.02809 AFIX 23 H80A 2 0.714787 0.008045 0.029694 11.00000 -1.20000 H80B 2 0.717559 -0.081964 0.030547 11.00000 -1.20000 AFIX 0 PART 1 C15 1 0.066636 0.765612 0.314030 21.00000 0.03142 0.03129 = 0.03137 -0.00007 -0.00058 -0.01147 C16 1 0.124015 0.820516 0.321568 21.00000 0.04851 0.03248 = 0.02793 -0.00334 -0.00518 -0.02547 C17 1 0.072563 0.897716 0.326595 21.00000 0.02610 0.03370 = 0.05038 -0.00868 0.00834 -0.00626 AFIX 43 H17 2 0.114025 0.930950 0.327929 21.00000 -1.20000 AFIX 0 C18 1 -0.040076 0.933767 0.330098 21.00000 0.05622 0.04266 = 0.04894 -0.00466 -0.00392 -0.01821 C19 1 -0.101859 0.884885 0.324071 21.00000 0.04068 0.03941 = 0.05021 -0.00656 0.01350 0.00348 AFIX 43 H19 2 -0.178289 0.907629 0.325681 21.00000 -1.20000 AFIX 0 C20 1 -0.049523 0.802045 0.315641 21.00000 0.04276 0.02454 = 0.04421 -0.00390 0.00678 -0.00977 C21 1 0.243081 0.788484 0.320934 21.00000 0.04731 0.03198 = 0.03507 -0.00297 -0.00596 -0.01215 AFIX 13 H21 2 0.267227 0.732555 0.306163 21.00000 -1.20000 AFIX 0 C22 1 0.279030 0.784477 0.389199 21.00000 0.06340 0.04488 = 0.04555 -0.00474 -0.00705 -0.01635 AFIX 33 H22A 2 0.246038 0.752766 0.414806 21.00000 -1.50000 H22B 2 0.256065 0.838493 0.405263 21.00000 -1.50000 H22C 2 0.357635 0.759649 0.390536 21.00000 -1.50000 AFIX 0 C23 1 0.299217 0.829623 0.283253 21.00000 0.05193 0.02543 = 0.06438 -0.00480 -0.00299 -0.01083 AFIX 33 H23A 2 0.377042 0.800906 0.285752 21.00000 -1.50000 H23B 2 0.281047 0.883748 0.298361 21.00000 -1.50000 H23C 2 0.277796 0.832235 0.239984 21.00000 -1.50000 AFIX 0 C24 1 -0.096930 1.023147 0.337622 21.00000 0.06160 0.04002 = 0.05229 -0.01810 -0.01588 0.00693 AFIX 13 H24 2 -0.050398 1.042222 0.363260 21.00000 -1.20000 AFIX 0 C25 1 -0.105433 1.065464 0.271996 21.00000 0.08712 0.08529 = 0.08677 -0.00100 -0.00164 -0.02992 AFIX 33 H25A 2 -0.033402 1.051262 0.252528 21.00000 -1.50000 H25B 2 -0.137027 1.123333 0.276650 21.00000 -1.50000 H25C 2 -0.151179 1.048226 0.245823 21.00000 -1.50000 AFIX 0 C26 1 -0.198788 1.049045 0.364945 21.00000 0.12579 0.05603 = 0.15863 -0.01292 0.09507 -0.01639 AFIX 33 H26A 2 -0.225717 1.107213 0.367713 21.00000 -1.50000 H26B 2 -0.195793 1.025079 0.406751 21.00000 -1.50000 H26C 2 -0.247183 1.033233 0.339774 21.00000 -1.50000 AFIX 0 C27 1 -0.119305 0.751963 0.311976 21.00000 0.04540 0.04539 = 0.04087 -0.00012 -0.00300 -0.01823 AFIX 13 H27 2 -0.072732 0.695823 0.322514 21.00000 -1.20000 AFIX 0 C28 1 -0.154983 0.752431 0.246620 21.00000 0.18508 0.12881 = 0.06190 -0.03090 0.03334 -0.11580 AFIX 33 H28A 2 -0.200629 0.720276 0.245105 21.00000 -1.50000 H28B 2 -0.091682 0.730028 0.218998 21.00000 -1.50000 H28C 2 -0.195912 0.807295 0.233121 21.00000 -1.50000 AFIX 0 C29 1 -0.214975 0.773784 0.356883 21.00000 0.07444 0.11450 = 0.06411 -0.01925 0.02118 -0.05767 AFIX 33 H29A 2 -0.190872 0.775619 0.399013 21.00000 -1.50000 H29B 2 -0.248976 0.733755 0.355747 21.00000 -1.50000 H29C 2 -0.267129 0.826129 0.345016 21.00000 -1.50000 AFIX 0 O8 3 0.102964 0.703025 0.557728 31.00000 0.06996 0.07934 = 0.10379 -0.00284 -0.04074 0.00210 C61 1 0.006335 0.715971 0.524591 31.00000 0.08411 0.07957 = 0.18734 -0.01742 -0.05498 0.00350 AFIX 23 H61A 2 0.020225 0.675252 0.492450 31.00000 -1.20000 H61B 2 -0.050743 0.711324 0.553642 31.00000 -1.20000 AFIX 0 C62 1 -0.026462 0.790045 0.497380 31.00000 0.10874 0.19976 = 0.08824 0.02652 -0.03376 -0.00745 AFIX 23 H62A 2 -0.105786 0.815601 0.501311 31.00000 -1.20000 H62B 2 -0.005589 0.786377 0.452657 31.00000 -1.20000 AFIX 0 C63 1 0.025609 0.837586 0.529030 31.00000 0.11351 0.11644 = 0.12142 0.00355 -0.03771 -0.01547 AFIX 23 H63A 2 0.051038 0.869873 0.498501 31.00000 -1.20000 H63B 2 -0.025318 0.873701 0.559067 31.00000 -1.20000 AFIX 0 C64 1 0.114598 0.780492 0.560474 31.00000 0.09459 0.06458 = 0.08857 -0.01805 -0.00557 -0.01322 AFIX 23 H64A 2 0.114392 0.795456 0.604260 31.00000 -1.20000 H64B 2 0.183422 0.778479 0.540020 31.00000 -1.20000 AFIX 0 PART 2 C15B 1 0.054742 0.762886 0.307730 -21.00000 0.03514 C16B 1 0.108644 0.811361 0.316762 -21.00000 0.02773 C17B 1 0.044285 0.902193 0.327976 -21.00000 0.03110 AFIX 43 H17B 2 0.080360 0.936067 0.340133 -21.00000 -1.20000 AFIX 0 C18B 1 -0.060524 0.930563 0.320232 -21.00000 0.03030 C19B 1 -0.102388 0.874621 0.308134 -21.00000 0.04137 AFIX 43 H19B 2 -0.178035 0.894550 0.302731 -21.00000 -1.20000 AFIX 0 C20B 1 -0.052798 0.792515 0.302285 -21.00000 0.04574 C21B 1 0.235868 0.788765 0.333362 -21.00000 0.04091 AFIX 13 H21B 2 0.275191 0.731604 0.323200 -21.00000 -1.20000 AFIX 0 C22B 1 0.251692 0.798514 0.399989 -21.00000 0.04907 AFIX 33 H22D 2 0.219318 0.766474 0.425677 -21.00000 -1.50000 H22E 2 0.217274 0.854751 0.410514 -21.00000 -1.50000 H22F 2 0.328930 0.780751 0.407758 -21.00000 -1.50000 AFIX 0 C23B 1 0.284221 0.846067 0.283871 -21.00000 0.04251 AFIX 33 H23D 2 0.269052 0.838340 0.240922 -21.00000 -1.50000 H23E 2 0.362176 0.830182 0.288384 -21.00000 -1.50000 H23F 2 0.248997 0.902343 0.294093 -21.00000 -1.50000 AFIX 0 C24B 1 -0.121476 1.019280 0.322272 -21.00000 0.05097 AFIX 13 H24B 2 -0.199213 1.034903 0.312267 -21.00000 -1.20000 AFIX 0 C25B 1 -0.067854 1.070268 0.289547 -21.00000 0.04497 AFIX 33 H25D 2 -0.111018 1.126529 0.296073 -21.00000 -1.50000 H25E 2 -0.061375 1.059751 0.244972 -21.00000 -1.50000 H25F 2 0.004012 1.057976 0.306126 -21.00000 -1.50000 AFIX 0 C26B 1 -0.101988 1.041246 0.396734 -21.00000 0.10305 AFIX 33 H26D 2 -0.138953 1.098408 0.403193 -21.00000 -1.50000 H26E 2 -0.024741 1.026861 0.403147 -21.00000 -1.50000 H26F 2 -0.131148 1.011005 0.426350 -21.00000 -1.50000 AFIX 0 C27B 1 -0.120019 0.744090 0.290501 -21.00000 0.03098 AFIX 13 H27B 2 -0.072086 0.691813 0.273581 -21.00000 -1.20000 AFIX 0 C28B 1 -0.206396 0.782151 0.246069 -21.00000 0.04547 AFIX 33 H28D 2 -0.244842 0.746078 0.238755 -21.00000 -1.50000 H28E 2 -0.174839 0.793780 0.206730 -21.00000 -1.50000 H28F 2 -0.256849 0.831861 0.263224 -21.00000 -1.50000 AFIX 0 C29B 1 -0.166740 0.728760 0.352379 -21.00000 0.05490 AFIX 33 H29D 2 -0.207763 0.693966 0.346852 -21.00000 -1.50000 H29E 2 -0.214547 0.779433 0.369446 -21.00000 -1.50000 H29F 2 -0.108295 0.702910 0.381084 -21.00000 -1.50000 AFIX 0 O8B 3 0.087103 0.691830 0.576142 -31.00000 0.07566 C61B 1 -0.008060 0.687931 0.541212 -31.00000 0.06253 AFIX 23 H61C 2 -0.056905 0.670375 0.568849 -31.00000 -1.20000 H61D 2 0.015936 0.652042 0.505487 -31.00000 -1.20000 AFIX 0 C62B 1 -0.062662 0.777030 0.519369 -31.00000 0.09763 AFIX 23 H62C 2 -0.116536 0.782662 0.487404 -31.00000 -1.20000 H62D 2 -0.098240 0.811195 0.554760 -31.00000 -1.20000 AFIX 0 C63B 1 0.026849 0.797112 0.493817 -31.00000 0.07716 AFIX 23 H63C 2 0.010689 0.855159 0.488940 -31.00000 -1.20000 H63D 2 0.058431 0.769492 0.454874 -31.00000 -1.20000 AFIX 0 C64B 1 0.095270 0.757551 0.554546 -31.00000 0.06817 AFIX 23 H64C 2 0.172198 0.747430 0.544455 -31.00000 -1.20000 H64D 2 0.072664 0.797004 0.587981 -31.00000 -1.20000 AFIX 0 part 0 O16 3 0.922175 0.148896 0.053612 11.00000 0.13639 0.12138 = 0.10323 0.01611 0.01763 0.01341 C81 1 0.866033 0.159134 0.113924 11.00000 0.13634 0.12264 = 0.10421 0.01662 0.01658 0.01291 AFIX 23 H81A 2 0.885825 0.107700 0.137298 11.00000 -1.20000 H81B 2 0.883888 0.197621 0.138859 11.00000 -1.20000 AFIX 0 C82 1 0.757471 0.187839 0.100582 11.00000 0.13533 0.12324 = 0.10641 0.01848 0.01697 0.01119 AFIX 23 H82A 2 0.713484 0.219344 0.135255 11.00000 -1.20000 H82B 2 0.732360 0.143690 0.092321 11.00000 -1.20000 AFIX 0 C83 1 0.751759 0.238719 0.044136 11.00000 0.13654 0.12452 = 0.10762 0.01867 0.01537 0.01173 AFIX 23 H83A 2 0.695954 0.236234 0.016082 11.00000 -1.20000 H83B 2 0.735550 0.294865 0.055152 11.00000 -1.20000 AFIX 0 C84 1 0.858440 0.204870 0.015440 11.00000 0.13631 0.12269 = 0.10418 0.01745 0.01638 0.01336 AFIX 23 H84A 2 0.854036 0.181090 -0.024613 11.00000 -1.20000 H84B 2 0.888760 0.247198 0.007102 11.00000 -1.20000 HKLF 4 REM PH09028 in P-1 REM R1 = 0.0642 for 10086 Fo > 4sig(Fo) and 0.1122 for all 16947 data REM 1028 parameters refined using 42 restraints END WGHT 0.0957 0.0000 REM Highest difference peak 0.892, deepest hole -0.627, 1-sigma level 0.052 Q1 1 0.8368 0.1433 0.0235 11.00000 0.05 0.89 Q2 1 0.8682 0.2350 0.0994 11.00000 0.05 0.64 Q3 1 0.7797 0.1996 0.0152 11.00000 0.05 0.47 Q4 1 0.6532 0.5211 -0.0026 11.00000 0.05 0.39 Q5 1 0.3577 0.6308 0.5629 11.00000 0.05 0.38 ; _database_code_depnum_ccdc_archive 'CCDC 948788' ####################################################################### # # 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_complex8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H84 Li4 N4 P4' _chemical_formula_sum 'C44 H84 Li4 N4 P4' _chemical_formula_weight 820.79 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' Li Li -0.0003 0.0001 '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 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 16.3704(3) _cell_length_b 19.8946(4) _cell_length_c 17.4380(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.0830(10) _cell_angle_gamma 90.00 _cell_volume 5224.56(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 40844 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.03 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6703 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Blessing, R. H. (1995) Acta Cryst. A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ApexII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40844 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9222 _reflns_number_gt 6650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0524P)^2^+1.6801P] 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 9222 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1153 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 -0.09842(13) 0.60270(11) 0.31688(13) 0.0314(5) Uani 1 1 d . . . C2 C -0.03310(14) 0.55740(11) 0.36426(13) 0.0312(5) Uani 1 1 d . . . H2A H -0.0531 0.5115 0.3724 0.037 Uiso 1 1 calc R . . C3 C 0.05048(14) 0.57830(11) 0.42059(12) 0.0316(5) Uani 1 1 d . . . C4 C 0.06843(15) 0.64648(12) 0.42697(14) 0.0389(6) Uani 1 1 d . . . H4A H 0.1251 0.6620 0.4640 0.047 Uiso 1 1 calc R . . C5 C 0.00530(16) 0.69225(12) 0.38043(15) 0.0439(6) Uani 1 1 d . . . H5A H 0.0187 0.7389 0.3858 0.053 Uiso 1 1 calc R . . C6 C -0.07755(15) 0.67062(12) 0.32579(14) 0.0403(6) Uani 1 1 d . . . H6A H -0.1206 0.7027 0.2941 0.048 Uiso 1 1 calc R . . C7 C -0.18637(13) 0.57647(11) 0.25561(13) 0.0335(5) Uani 1 1 d . . . H7A H -0.2316 0.6124 0.2434 0.040 Uiso 1 1 calc R . . H7B H -0.2055 0.5384 0.2811 0.040 Uiso 1 1 calc R . . C8 C 0.11763(14) 0.52803(12) 0.47219(13) 0.0361(5) Uani 1 1 d . . . H8A H 0.0877 0.4940 0.4935 0.043 Uiso 1 1 calc R . . H8B H 0.1626 0.5511 0.5207 0.043 Uiso 1 1 calc R . . P1 P -0.17997(4) 0.54747(3) 0.15420(4) 0.03158(15) Uani 1 1 d . . . Li1 Li -0.2448(2) 0.42912(19) 0.1543(2) 0.0355(9) Uani 1 1 d . . . C9 C -0.20740(16) 0.68673(11) 0.10751(15) 0.0427(6) Uani 1 1 d . . . H9A H -0.2367 0.7190 0.0626 0.064 Uiso 1 1 calc R . . H9B H -0.1430 0.6889 0.1235 0.064 Uiso 1 1 calc R . . H9C H -0.2214 0.6978 0.1558 0.064 Uiso 1 1 calc R . . C10 C -0.22235(18) 0.60116(13) -0.00103(15) 0.0497(7) Uani 1 1 d . . . H10A H -0.2548 0.6335 -0.0448 0.075 Uiso 1 1 calc R . . H10B H -0.2421 0.5555 -0.0205 0.075 Uiso 1 1 calc R . . H10C H -0.1586 0.6051 0.0122 0.075 Uiso 1 1 calc R . . C11 C -0.34087(15) 0.61429(12) 0.05431(15) 0.0440(6) Uani 1 1 d . . . H11A H -0.3694 0.6500 0.0139 0.066 Uiso 1 1 calc R . . H11B H -0.3529 0.6213 0.1045 0.066 Uiso 1 1 calc R . . H11C H -0.3646 0.5706 0.0297 0.066 Uiso 1 1 calc R . . C12 C -0.24034(14) 0.61593(11) 0.07736(13) 0.0354(5) Uani 1 1 d . . . P2 P 0.17503(3) 0.48455(3) 0.41107(3) 0.02677(14) Uani 1 1 d . . . Li2 Li 0.2538(2) 0.56766(18) 0.3441(2) 0.0342(8) Uani 1 1 d . . . C13 C 0.17125(19) 0.36637(14) 0.50100(19) 0.0707(9) Uani 1 1 d . . . H13A H 0.2047 0.3332 0.5432 0.106 Uiso 1 1 calc R . . H13B H 0.1380 0.3434 0.4482 0.106 Uiso 1 1 calc R . . H13C H 0.1298 0.3902 0.5194 0.106 Uiso 1 1 calc R . . C14 C 0.2957(2) 0.38112(16) 0.45436(17) 0.0753(10) Uani 1 1 d . . . H14A H 0.3262 0.3440 0.4914 0.113 Uiso 1 1 calc R . . H14B H 0.3397 0.4129 0.4506 0.113 Uiso 1 1 calc R . . H14C H 0.2600 0.3634 0.3988 0.113 Uiso 1 1 calc R . . C15 C 0.29256(16) 0.44506(12) 0.57422(14) 0.0462(6) Uani 1 1 d . . . H15A H 0.3268 0.4086 0.6105 0.069 Uiso 1 1 calc R . . H15B H 0.2542 0.4659 0.5988 0.069 Uiso 1 1 calc R . . H15C H 0.3333 0.4788 0.5684 0.069 Uiso 1 1 calc R . . C16 C 0.23565(14) 0.41672(10) 0.48881(13) 0.0328(5) Uani 1 1 d . . . C17 C 0.02052(13) 0.38042(10) 0.15065(12) 0.0293(5) Uani 1 1 d . . . C18 C 0.02755(13) 0.44695(10) 0.12910(12) 0.0289(5) Uani 1 1 d . . . H18A H -0.0251 0.4728 0.1045 0.035 Uiso 1 1 calc R . . C19 C 0.10900(14) 0.47713(10) 0.14217(12) 0.0293(5) Uani 1 1 d . . . C20 C 0.18521(14) 0.43835(11) 0.17903(14) 0.0356(5) Uani 1 1 d . . . H20A H 0.2416 0.4576 0.1893 0.043 Uiso 1 1 calc R . . C21 C 0.18005(15) 0.37266(12) 0.20081(15) 0.0411(6) Uani 1 1 d . . . H21A H 0.2328 0.3469 0.2254 0.049 Uiso 1 1 calc R . . C22 C 0.09901(15) 0.34359(11) 0.18734(14) 0.0368(5) Uani 1 1 d . . . H22A H 0.0966 0.2982 0.2031 0.044 Uiso 1 1 calc R . . C23 C 0.11411(15) 0.54882(11) 0.11889(13) 0.0348(5) Uani 1 1 d . . . H23A H 0.0610 0.5602 0.0685 0.042 Uiso 1 1 calc R . . H23B H 0.1673 0.5554 0.1059 0.042 Uiso 1 1 calc R . . C24 C -0.06839(14) 0.35206(11) 0.13999(13) 0.0333(5) Uani 1 1 d . . . H24A H -0.0686 0.3029 0.1308 0.040 Uiso 1 1 calc R . . H24B H -0.1151 0.3724 0.0903 0.040 Uiso 1 1 calc R . . P3 P 0.12041(3) 0.60568(3) 0.20734(3) 0.02788(14) Uani 1 1 d . . . Li3 Li -0.0222(3) 0.5828(2) 0.2175(3) 0.0465(10) Uani 1 1 d . . . C25 C 0.04602(18) 0.69551(13) 0.06956(15) 0.0539(7) Uani 1 1 d . . . H25A H 0.0432 0.7416 0.0489 0.081 Uiso 1 1 calc R . . H25B H -0.0118 0.6829 0.0696 0.081 Uiso 1 1 calc R . . H25C H 0.0614 0.6648 0.0333 0.081 Uiso 1 1 calc R . . C26 C 0.09392(17) 0.74271(12) 0.21177(16) 0.0511(7) Uani 1 1 d . . . H26A H 0.0984 0.7881 0.1919 0.077 Uiso 1 1 calc R . . H26B H 0.1355 0.7382 0.2700 0.077 Uiso 1 1 calc R . . H26C H 0.0332 0.7349 0.2077 0.077 Uiso 1 1 calc R . . C27 C 0.20705(16) 0.70893(12) 0.15617(17) 0.0494(7) Uani 1 1 d . . . H27A H 0.2035 0.7532 0.1305 0.074 Uiso 1 1 calc R . . H27B H 0.2229 0.6751 0.1235 0.074 Uiso 1 1 calc R . . H27C H 0.2524 0.7098 0.2131 0.074 Uiso 1 1 calc R . . C28 C 0.11680(14) 0.69113(11) 0.15836(14) 0.0362(5) Uani 1 1 d . . . P4 P -0.09424(4) 0.36926(3) 0.23526(3) 0.03112(15) Uani 1 1 d . . . Li4 Li 0.0544(3) 0.4242(2) 0.2979(2) 0.0432(10) Uani 1 1 d . . . C29 C -0.16530(16) 0.23832(12) 0.23248(15) 0.0493(7) Uani 1 1 d . . . H29A H -0.1591 0.1944 0.2596 0.074 Uiso 1 1 calc R . . H29B H -0.1658 0.2325 0.1765 0.074 Uiso 1 1 calc R . . H29C H -0.2210 0.2593 0.2283 0.074 Uiso 1 1 calc R . . C30 C -0.09089(18) 0.29672(14) 0.36890(15) 0.0534(7) Uani 1 1 d . . . H30A H -0.0909 0.2538 0.3966 0.080 Uiso 1 1 calc R . . H30B H -0.1452 0.3216 0.3611 0.080 Uiso 1 1 calc R . . H30C H -0.0391 0.3233 0.4034 0.080 Uiso 1 1 calc R . . C31 C -0.00159(16) 0.24474(12) 0.29766(16) 0.0513(7) Uani 1 1 d . . . H31A H -0.0004 0.2030 0.3278 0.077 Uiso 1 1 calc R . . H31B H 0.0499 0.2724 0.3303 0.077 Uiso 1 1 calc R . . H31C H 0.0004 0.2342 0.2435 0.077 Uiso 1 1 calc R . . C32 C -0.08702(15) 0.28340(11) 0.28414(14) 0.0373(6) Uani 1 1 d . . . C33 C -0.33454(19) 0.39065(15) 0.27599(16) 0.0606(8) Uani 1 1 d . . . H33A H -0.3886 0.3841 0.2865 0.091 Uiso 1 1 calc R . . H33B H -0.2939 0.4205 0.3186 0.091 Uiso 1 1 calc R . . H33C H -0.3057 0.3471 0.2780 0.091 Uiso 1 1 calc R . . C34 C -0.40034(16) 0.48551(13) 0.19115(17) 0.0510(7) Uani 1 1 d . . . H34A H -0.4551 0.4787 0.2004 0.077 Uiso 1 1 calc R . . H34B H -0.4146 0.5066 0.1366 0.077 Uiso 1 1 calc R . . H34C H -0.3601 0.5147 0.2349 0.077 Uiso 1 1 calc R . . N1 N -0.35768(12) 0.42092(10) 0.19337(11) 0.0373(5) Uani 1 1 d . . . C35 C -0.41699(16) 0.37530(13) 0.12942(15) 0.0484(7) Uani 1 1 d . . . H35A H -0.4776 0.3787 0.1288 0.058 Uiso 1 1 calc R . . H35B H -0.3963 0.3285 0.1441 0.058 Uiso 1 1 calc R . . C36 C -0.42035(16) 0.39101(15) 0.04423(15) 0.0518(7) Uani 1 1 d . . . H36A H -0.4632 0.3604 0.0033 0.062 Uiso 1 1 calc R . . H36B H -0.4419 0.4376 0.0293 0.062 Uiso 1 1 calc R . . N2 N -0.33362(12) 0.38396(9) 0.03914(11) 0.0349(4) Uani 1 1 d . . . C37 C -0.33581(19) 0.41922(14) -0.03552(15) 0.0564(7) Uani 1 1 d . . . H37A H -0.3817 0.3993 -0.0851 0.085 Uiso 1 1 calc R . . H37B H -0.2779 0.4151 -0.0394 0.085 Uiso 1 1 calc R . . H37C H -0.3492 0.4668 -0.0319 0.085 Uiso 1 1 calc R . . C38 C -0.31300(17) 0.31373(13) 0.03173(16) 0.0530(7) Uani 1 1 d . . . H38A H -0.3580 0.2947 -0.0191 0.079 Uiso 1 1 calc R . . H38B H -0.3126 0.2887 0.0803 0.079 Uiso 1 1 calc R . . H38C H -0.2545 0.3105 0.0290 0.079 Uiso 1 1 calc R . . C39 C 0.3534(2) 0.62475(14) 0.51415(15) 0.0638(8) Uani 1 1 d . . . H39A H 0.3956 0.6561 0.5531 0.096 Uiso 1 1 calc R . . H39B H 0.3781 0.5792 0.5245 0.096 Uiso 1 1 calc R . . H39C H 0.2974 0.6257 0.5222 0.096 Uiso 1 1 calc R . . C40 C 0.30019(18) 0.71201(12) 0.41544(16) 0.0517(7) Uani 1 1 d . . . H40A H 0.3424 0.7430 0.4550 0.078 Uiso 1 1 calc R . . H40B H 0.2444 0.7123 0.4238 0.078 Uiso 1 1 calc R . . H40C H 0.2889 0.7262 0.3584 0.078 Uiso 1 1 calc R . . N3 N 0.38688(12) 0.54088(10) 0.33132(12) 0.0429(5) Uani 1 1 d . . . C41 C 0.42024(17) 0.64458(15) 0.4138(2) 0.0631(8) Uani 1 1 d . . . H41A H 0.4106 0.6717 0.3634 0.076 Uiso 1 1 calc R . . H41B H 0.4677 0.6666 0.4615 0.076 Uiso 1 1 calc R . . C42 C 0.45036(17) 0.57718(16) 0.40229(18) 0.0667(9) Uani 1 1 d . . . H42A H 0.5070 0.5814 0.3948 0.080 Uiso 1 1 calc R . . H42B H 0.4621 0.5505 0.4535 0.080 Uiso 1 1 calc R . . N4 N 0.33721(12) 0.64434(9) 0.42919(12) 0.0400(5) Uani 1 1 d . . . C43 C 0.41796(19) 0.47093(14) 0.33613(18) 0.0654(8) Uani 1 1 d . . . H43A H 0.4772 0.4703 0.3346 0.098 Uiso 1 1 calc R . . H43B H 0.3766 0.4454 0.2887 0.098 Uiso 1 1 calc R . . H43C H 0.4207 0.4505 0.3883 0.098 Uiso 1 1 calc R . . C44 C 0.38247(16) 0.56923(14) 0.25215(16) 0.0502(7) Uani 1 1 d . . . H44A H 0.4424 0.5719 0.2526 0.075 Uiso 1 1 calc R . . H44B H 0.3566 0.6144 0.2449 0.075 Uiso 1 1 calc R . . H44C H 0.3455 0.5404 0.2061 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0295(12) 0.0397(14) 0.0291(12) -0.0018(10) 0.0159(9) 0.0055(10) C2 0.0336(12) 0.0342(13) 0.0297(12) 0.0020(10) 0.0167(10) 0.0027(10) C3 0.0341(12) 0.0408(14) 0.0229(11) -0.0028(10) 0.0144(9) 0.0059(10) C4 0.0316(12) 0.0465(15) 0.0352(13) -0.0086(11) 0.0096(10) 0.0025(11) C5 0.0461(15) 0.0336(14) 0.0466(15) -0.0065(12) 0.0122(12) 0.0027(11) C6 0.0406(14) 0.0367(14) 0.0389(14) -0.0009(11) 0.0104(11) 0.0095(11) C7 0.0277(12) 0.0399(13) 0.0348(13) 0.0025(10) 0.0143(10) 0.0041(10) C8 0.0377(13) 0.0460(14) 0.0243(11) -0.0009(10) 0.0117(10) 0.0066(11) P1 0.0285(3) 0.0332(3) 0.0348(3) -0.0021(3) 0.0143(3) -0.0001(2) Li1 0.0301(19) 0.041(2) 0.035(2) -0.0051(17) 0.0119(16) -0.0040(16) C9 0.0478(14) 0.0373(14) 0.0441(14) 0.0050(12) 0.0193(12) -0.0010(11) C10 0.0645(17) 0.0530(16) 0.0393(14) 0.0013(13) 0.0286(13) -0.0035(13) C11 0.0378(13) 0.0483(15) 0.0393(14) 0.0025(12) 0.0081(11) 0.0045(11) C12 0.0378(13) 0.0393(14) 0.0306(12) 0.0029(10) 0.0151(10) 0.0006(10) P2 0.0281(3) 0.0290(3) 0.0217(3) -0.0006(2) 0.0082(2) 0.0003(2) Li2 0.033(2) 0.039(2) 0.029(2) 0.0017(17) 0.0098(16) -0.0018(16) C13 0.0663(19) 0.0506(17) 0.069(2) 0.0268(15) -0.0019(15) -0.0142(15) C14 0.103(3) 0.076(2) 0.0447(17) 0.0063(15) 0.0264(17) 0.0550(19) C15 0.0475(15) 0.0437(15) 0.0334(14) 0.0040(11) 0.0008(11) 0.0052(12) C16 0.0366(12) 0.0284(12) 0.0285(12) -0.0002(10) 0.0075(10) 0.0011(10) C17 0.0330(12) 0.0331(13) 0.0218(11) -0.0067(9) 0.0105(9) -0.0027(10) C18 0.0288(11) 0.0349(13) 0.0225(11) -0.0036(9) 0.0093(9) 0.0018(9) C19 0.0360(12) 0.0342(13) 0.0205(11) -0.0048(9) 0.0139(9) -0.0009(10) C20 0.0294(12) 0.0411(14) 0.0389(13) -0.0040(11) 0.0161(10) -0.0031(10) C21 0.0349(13) 0.0415(15) 0.0487(15) 0.0020(12) 0.0184(11) 0.0097(11) C22 0.0397(14) 0.0306(13) 0.0436(14) 0.0008(11) 0.0202(11) 0.0032(10) C23 0.0371(13) 0.0407(14) 0.0291(12) -0.0001(10) 0.0158(10) -0.0031(10) C24 0.0347(12) 0.0358(13) 0.0250(11) -0.0025(10) 0.0068(9) -0.0057(10) P3 0.0268(3) 0.0308(3) 0.0250(3) 0.0027(2) 0.0091(2) -0.0002(2) Li3 0.035(2) 0.056(3) 0.052(3) 0.001(2) 0.0217(19) -0.0023(19) C25 0.0603(17) 0.0482(16) 0.0411(15) 0.0174(13) 0.0066(13) 0.0080(13) C26 0.0518(16) 0.0380(15) 0.0603(17) 0.0007(13) 0.0183(13) 0.0062(12) C27 0.0524(16) 0.0379(14) 0.0616(17) 0.0116(13) 0.0262(13) -0.0049(12) C28 0.0378(13) 0.0316(13) 0.0372(13) 0.0067(11) 0.0124(10) 0.0022(10) P4 0.0293(3) 0.0334(3) 0.0289(3) -0.0012(3) 0.0095(2) -0.0044(2) Li4 0.040(2) 0.046(2) 0.037(2) -0.0072(19) 0.0075(18) -0.0100(18) C29 0.0527(16) 0.0440(15) 0.0439(15) 0.0051(12) 0.0110(12) -0.0191(12) C30 0.0576(17) 0.0647(18) 0.0338(14) 0.0081(13) 0.0135(12) -0.0135(14) C31 0.0522(16) 0.0427(15) 0.0506(16) 0.0110(13) 0.0113(12) 0.0017(12) C32 0.0367(13) 0.0398(14) 0.0304(12) 0.0035(10) 0.0076(10) -0.0086(10) C33 0.0691(19) 0.071(2) 0.0450(16) 0.0059(15) 0.0257(14) -0.0012(15) C34 0.0430(15) 0.0562(17) 0.0599(17) -0.0022(14) 0.0268(13) -0.0004(13) N1 0.0362(11) 0.0442(12) 0.0329(11) -0.0040(9) 0.0150(9) -0.0046(9) C35 0.0408(14) 0.0593(17) 0.0498(16) -0.0113(13) 0.0227(12) -0.0179(12) C36 0.0372(14) 0.0711(19) 0.0420(15) -0.0125(13) 0.0099(11) -0.0090(13) N2 0.0340(10) 0.0420(12) 0.0278(10) -0.0036(9) 0.0110(8) -0.0030(8) C37 0.0741(19) 0.0580(18) 0.0380(15) -0.0040(13) 0.0231(14) -0.0076(14) C38 0.0531(16) 0.0487(16) 0.0422(15) -0.0108(13) 0.0026(12) -0.0008(13) C39 0.073(2) 0.0636(19) 0.0357(15) 0.0011(14) 0.0012(13) -0.0212(15) C40 0.0638(17) 0.0432(16) 0.0474(16) -0.0025(13) 0.0211(13) -0.0029(13) N3 0.0321(11) 0.0563(13) 0.0341(11) -0.0010(10) 0.0062(9) -0.0008(9) C41 0.0389(15) 0.065(2) 0.079(2) -0.0181(16) 0.0157(14) -0.0191(14) C42 0.0336(14) 0.095(2) 0.0607(19) -0.0214(17) 0.0071(13) -0.0043(15) N4 0.0371(11) 0.0382(12) 0.0391(11) -0.0005(9) 0.0090(9) -0.0054(9) C43 0.0557(18) 0.067(2) 0.0628(19) 0.0109(16) 0.0120(15) 0.0158(15) C44 0.0430(15) 0.0600(17) 0.0497(16) 0.0068(13) 0.0204(12) 0.0001(13) _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 C6 1.388(3) . ? C1 C2 1.395(3) . ? C1 C7 1.510(3) . ? C1 Li3 2.533(5) . ? C2 C3 1.399(3) . ? C2 Li3 2.683(5) . ? C3 C4 1.383(3) . ? C3 C8 1.498(3) . ? C4 C5 1.378(3) . ? C5 C6 1.385(3) . ? C7 P1 1.902(2) . ? C8 P2 1.885(2) . ? P1 C12 1.894(2) . ? P1 Li3 2.480(4) . ? P1 Li1 2.583(4) . ? Li1 N2 2.160(4) . ? Li1 N1 2.212(4) . ? Li1 P4 2.599(4) . ? C9 C12 1.526(3) . ? C10 C12 1.535(3) . ? C11 C12 1.534(3) . ? P2 C16 1.894(2) . ? P2 Li4 2.486(4) . ? P2 Li2 2.634(4) . ? Li2 N4 2.192(4) . ? Li2 N3 2.337(4) . ? Li2 P3 2.635(3) . ? C13 C16 1.528(3) . ? C14 C16 1.514(3) . ? C15 C16 1.522(3) . ? C17 C18 1.393(3) . ? C17 C22 1.397(3) . ? C17 C24 1.503(3) . ? C17 Li4 2.557(4) . ? C18 C19 1.397(3) . ? C19 C20 1.391(3) . ? C19 C23 1.494(3) . ? C20 C21 1.373(3) . ? C21 C22 1.380(3) . ? C23 P3 1.883(2) . ? C24 P4 1.899(2) . ? P3 C28 1.893(2) . ? P3 Li3 2.451(4) . ? Li3 Li4 3.482(6) . ? C25 C28 1.530(3) . ? C26 C28 1.528(3) . ? C27 C28 1.534(3) . ? P4 C32 1.892(2) . ? P4 Li4 2.495(4) . ? C29 C32 1.534(3) . ? C30 C32 1.527(3) . ? C31 C32 1.531(3) . ? C33 N1 1.468(3) . ? C34 N1 1.456(3) . ? N1 C35 1.470(3) . ? C35 C36 1.498(3) . ? C36 N2 1.464(3) . ? N2 C38 1.455(3) . ? N2 C37 1.467(3) . ? C39 N4 1.452(3) . ? C40 N4 1.457(3) . ? N3 C42 1.458(3) . ? N3 C44 1.467(3) . ? N3 C43 1.473(3) . ? C41 C42 1.469(4) . ? C41 N4 1.485(3) . ? 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 C6 C1 C2 117.7(2) . . ? C6 C1 C7 122.71(19) . . ? C2 C1 C7 119.5(2) . . ? C6 C1 Li3 93.59(17) . . ? C2 C1 Li3 80.54(15) . . ? C7 C1 Li3 92.92(15) . . ? C1 C2 C3 122.4(2) . . ? C1 C2 Li3 68.61(14) . . ? C3 C2 Li3 101.59(16) . . ? C4 C3 C2 117.8(2) . . ? C4 C3 C8 121.6(2) . . ? C2 C3 C8 120.6(2) . . ? C5 C4 C3 120.9(2) . . ? C4 C5 C6 120.4(2) . . ? C5 C6 C1 120.7(2) . . ? C1 C7 P1 112.21(14) . . ? C3 C8 P2 112.21(14) . . ? C12 P1 C7 103.64(10) . . ? C12 P1 Li3 105.92(12) . . ? C7 P1 Li3 85.85(12) . . ? C12 P1 Li1 123.74(11) . . ? C7 P1 Li1 95.94(11) . . ? Li3 P1 Li1 127.94(13) . . ? N2 Li1 N1 85.22(14) . . ? N2 Li1 P1 120.36(17) . . ? N1 Li1 P1 117.42(16) . . ? N2 Li1 P4 117.63(16) . . ? N1 Li1 P4 121.85(17) . . ? P1 Li1 P4 96.64(12) . . ? C9 C12 C11 107.94(19) . . ? C9 C12 C10 108.55(19) . . ? C11 C12 C10 108.86(19) . . ? C9 C12 P1 113.83(15) . . ? C11 C12 P1 112.25(15) . . ? C10 C12 P1 105.25(16) . . ? C8 P2 C16 99.19(10) . . ? C8 P2 Li4 104.71(12) . . ? C16 P2 Li4 104.73(12) . . ? C8 P2 Li2 113.68(11) . . ? C16 P2 Li2 123.65(11) . . ? Li4 P2 Li2 109.00(12) . . ? N4 Li2 N3 82.32(14) . . ? N4 Li2 P2 114.86(16) . . ? N3 Li2 P2 122.40(16) . . ? N4 Li2 P3 119.21(16) . . ? N3 Li2 P3 116.84(15) . . ? P2 Li2 P3 101.86(12) . . ? C14 C16 C15 108.6(2) . . ? C14 C16 C13 109.8(2) . . ? C15 C16 C13 107.3(2) . . ? C14 C16 P2 106.78(16) . . ? C15 C16 P2 112.61(15) . . ? C13 C16 P2 111.72(16) . . ? C18 C17 C22 117.61(19) . . ? C18 C17 C24 120.11(19) . . ? C22 C17 C24 122.1(2) . . ? C18 C17 Li4 86.50(15) . . ? C22 C17 Li4 85.42(15) . . ? C24 C17 Li4 94.04(15) . . ? C17 C18 C19 122.61(19) . . ? C20 C19 C18 117.6(2) . . ? C20 C19 C23 121.28(19) . . ? C18 C19 C23 121.16(19) . . ? C21 C20 C19 121.0(2) . . ? C20 C21 C22 120.7(2) . . ? C21 C22 C17 120.5(2) . . ? C19 C23 P3 109.99(14) . . ? C17 C24 P4 111.18(14) . . ? C23 P3 C28 100.83(10) . . ? C23 P3 Li3 101.52(12) . . ? C28 P3 Li3 109.68(12) . . ? C23 P3 Li2 109.20(11) . . ? C28 P3 Li2 122.31(11) . . ? Li3 P3 Li2 110.85(13) . . ? P3 Li3 P1 151.13(19) . . ? P3 Li3 C1 139.38(19) . . ? P1 Li3 C1 69.01(11) . . ? P3 Li3 C2 121.69(17) . . ? P1 Li3 C2 85.61(13) . . ? C1 Li3 C2 30.85(8) . . ? P3 Li3 Li4 89.67(13) . . ? P1 Li3 Li4 94.00(14) . . ? C1 Li3 Li4 93.56(15) . . ? C2 Li3 Li4 65.99(12) . . ? C26 C28 C25 108.0(2) . . ? C26 C28 C27 109.2(2) . . ? C25 C28 C27 108.4(2) . . ? C26 C28 P3 107.45(16) . . ? C25 C28 P3 112.65(16) . . ? C27 C28 P3 111.01(15) . . ? C32 P4 C24 103.61(10) . . ? C32 P4 Li4 108.68(12) . . ? C24 P4 Li4 87.02(12) . . ? C32 P4 Li1 122.46(11) . . ? C24 P4 Li1 95.53(11) . . ? Li4 P4 Li1 126.26(13) . . ? P2 Li4 P4 153.33(19) . . ? P2 Li4 C17 138.92(18) . . ? P4 Li4 C17 67.74(10) . . ? P2 Li4 Li3 86.00(13) . . ? P4 Li4 Li3 94.90(13) . . ? C17 Li4 Li3 90.13(14) . . ? C30 C32 C31 108.7(2) . . ? C30 C32 C29 109.1(2) . . ? C31 C32 C29 107.4(2) . . ? C30 C32 P4 105.09(16) . . ? C31 C32 P4 114.51(16) . . ? C29 C32 P4 111.90(15) . . ? C34 N1 C33 109.0(2) . . ? C34 N1 C35 110.95(19) . . ? C33 N1 C35 109.3(2) . . ? C34 N1 Li1 112.13(17) . . ? C33 N1 Li1 114.04(18) . . ? C35 N1 Li1 101.24(16) . . ? N1 C35 C36 112.3(2) . . ? N2 C36 C35 112.4(2) . . ? C38 N2 C36 111.2(2) . . ? C38 N2 C37 107.83(19) . . ? C36 N2 C37 108.75(19) . . ? C38 N2 Li1 112.76(17) . . ? C36 N2 Li1 102.66(16) . . ? C37 N2 Li1 113.56(17) . . ? C42 N3 C44 111.4(2) . . ? C42 N3 C43 107.7(2) . . ? C44 N3 C43 107.8(2) . . ? C42 N3 Li2 100.77(17) . . ? C44 N3 Li2 107.37(16) . . ? C43 N3 Li2 121.61(19) . . ? C42 C41 N4 113.7(2) . . ? N3 C42 C41 113.7(2) . . ? C39 N4 C40 108.3(2) . . ? C39 N4 C41 111.8(2) . . ? C40 N4 C41 108.6(2) . . ? C39 N4 Li2 108.64(17) . . ? C40 N4 Li2 115.03(17) . . ? C41 N4 Li2 104.56(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.363 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.045 _database_code_depnum_ccdc_archive 'CCDC 948789'