# Electronic Supplementary Material (ESI) for Chemical Science # 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_apx1327s _database_code_depnum_ccdc_archive 'CCDC 906766' #TrackingRef 'web_deposit_cif_file_0_AndrewGaunt_1350598115.cif for 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H53 La O2 P3 Se6' _chemical_formula_weight 1355.47 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/nmc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y, z' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 31.601(4) _cell_length_b 31.601(4) _cell_length_c 10.671(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10657(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5256 _exptl_absorpt_coefficient_mu 5.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5003 _exptl_absorpt_correction_T_max 0.6335 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 100136 _diffrn_reflns_av_R_equivalents 0.0977 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.86 _reflns_number_total 5329 _reflns_number_gt 4811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _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. Two carbon atom positions in each bound thf ligand were refined as two one-half occupancy positions. The bond distances and temperature factors on these carbon atoms were restrained (36 restraints) to obtain chemically reasonable values. Hydrogen atom positions were not modeled on the disordered thf ligands. ; # 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 0.250 0.750 0.229 544 140 hexane 2 0.250 0.250 0.473 284 80 hexane 3 0.750 0.250 0.768 544 138 hexane 4 0.750 0.750 0.524 284 78 hexane _platon_squeeze_details ; ; _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^)+(0.0442P)^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 5329 _refine_ls_number_parameters 280 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1840 _refine_ls_goodness_of_fit_ref 2.384 _refine_ls_restrained_S_all 2.397 _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 La1 La 0.7500 0.50076(2) 0.04696(6) 0.0195(2) Uani 1 2 d S . . Se1 Se 0.69662(3) 0.46110(3) -0.16752(8) 0.0258(3) Uani 1 1 d . . . Se2 Se 0.65556(3) 0.50658(3) 0.11395(8) 0.0246(3) Uani 1 1 d . . . Se3 Se 0.7500 0.59256(5) 0.16079(12) 0.0359(4) Uani 1 2 d S . . Se4 Se 0.7500 0.49685(4) 0.34177(12) 0.0304(4) Uani 1 2 d S . . P1 P 0.64088(7) 0.47342(7) -0.05810(19) 0.0207(5) Uani 1 1 d . . . P2 P 0.7500 0.56458(11) 0.3454(3) 0.0269(8) Uani 1 2 d S . . O1 O 0.7500 0.5583(3) -0.1136(8) 0.039(2) Uani 1 2 d S . . O2 O 0.7500 0.4237(3) 0.1253(8) 0.031(2) Uani 1 2 d S . . C1 C 0.6028(3) 0.5036(3) -0.1492(8) 0.0217(19) Uani 1 1 d . . . C2 C 0.5873(3) 0.5417(3) -0.1105(8) 0.029(2) Uani 1 1 d . . . H2 H 0.5968 0.5536 -0.0358 0.035 Uiso 1 1 calc R . . C3 C 0.5570(4) 0.5631(3) -0.1836(9) 0.040(3) Uani 1 1 d . . . H3 H 0.5465 0.5892 -0.1577 0.048 Uiso 1 1 calc R . . C4 C 0.5431(3) 0.5453(3) -0.2926(9) 0.037(3) Uani 1 1 d . . . H4 H 0.5228 0.5594 -0.3400 0.045 Uiso 1 1 calc R . . C5 C 0.5584(3) 0.5069(3) -0.3339(9) 0.035(2) Uani 1 1 d . . . H5 H 0.5489 0.4956 -0.4093 0.043 Uiso 1 1 calc R . . C6 C 0.5878(3) 0.4856(3) -0.2628(8) 0.026(2) Uani 1 1 d . . . H6 H 0.5977 0.4593 -0.2891 0.031 Uiso 1 1 calc R . . C7 C 0.6140(3) 0.4243(3) -0.0227(8) 0.0242(19) Uani 1 1 d . . . C8 C 0.5810(3) 0.4236(3) 0.0632(9) 0.034(2) Uani 1 1 d . . . H8 H 0.5732 0.4484 0.1038 0.041 Uiso 1 1 calc R . . C9 C 0.5595(4) 0.3861(4) 0.0893(10) 0.051(3) Uani 1 1 d . . . H9 H 0.5376 0.3861 0.1477 0.061 Uiso 1 1 calc R . . C10 C 0.5701(4) 0.3494(4) 0.0302(11) 0.048(3) Uani 1 1 d . . . H10 H 0.5554 0.3246 0.0469 0.058 Uiso 1 1 calc R . . C11 C 0.6029(4) 0.3496(3) -0.0544(10) 0.047(3) Uani 1 1 d . . . H11 H 0.6104 0.3245 -0.0939 0.057 Uiso 1 1 calc R . . C12 C 0.6249(3) 0.3859(3) -0.0821(9) 0.032(2) Uani 1 1 d . . . H12 H 0.6469 0.3852 -0.1399 0.038 Uiso 1 1 calc R . . C13 C 0.7953(3) 0.5841(3) 0.4325(8) 0.033(2) Uani 1 1 d . . . C14 C 0.8074(4) 0.6261(4) 0.4259(12) 0.067(4) Uani 1 1 d . . . H14 H 0.7931 0.6441 0.3713 0.080 Uiso 1 1 calc R . . C15 C 0.8391(5) 0.6418(4) 0.4959(13) 0.082(5) Uani 1 1 d . . . H15 H 0.8457 0.6704 0.4910 0.098 Uiso 1 1 calc R . . C16 C 0.8619(4) 0.6160(4) 0.5745(12) 0.064(4) Uani 1 1 d . . . H16 H 0.8836 0.6270 0.6239 0.077 Uiso 1 1 calc R . . C17 C 0.8523(3) 0.5748(4) 0.5784(9) 0.045(3) Uani 1 1 d . . . H17 H 0.8684 0.5570 0.6290 0.054 Uiso 1 1 calc R . . C18 C 0.8190(3) 0.5576(3) 0.5098(9) 0.036(2) Uani 1 1 d . . . H18 H 0.8128 0.5289 0.5152 0.043 Uiso 1 1 calc R . . C19 C 0.7134(4) 0.3993(4) 0.1658(12) 0.063(4) Uani 1 1 d D . . C20 C 0.7273(2) 0.3755(11) 0.280(2) 0.093(14) Uani 0.50 1 d PDU . . C20' C 0.7274(3) 0.3636(8) 0.244(3) 0.079(12) Uani 0.50 1 d PDU . . C21 C 0.7133(5) 0.5795(4) -0.1617(16) 0.094(6) Uani 1 1 d D . . C22' C 0.7280(3) 0.6237(6) -0.181(3) 0.090(13) Uani 0.50 1 d PDU . . C22 C 0.7281(3) 0.6170(8) -0.233(3) 0.095(13) Uani 0.50 1 d PDU . . 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 La1 0.0188(4) 0.0256(4) 0.0142(4) -0.0031(3) 0.000 0.000 Se1 0.0170(5) 0.0399(6) 0.0206(5) -0.0089(4) 0.0007(3) -0.0003(4) Se2 0.0202(5) 0.0348(6) 0.0187(5) -0.0047(4) 0.0028(3) 0.0020(4) Se3 0.0611(10) 0.0298(8) 0.0169(6) -0.0010(6) 0.000 0.000 Se4 0.0428(9) 0.0299(8) 0.0185(7) 0.0000(5) 0.000 0.000 P1 0.0163(11) 0.0269(13) 0.0189(11) -0.0003(9) -0.0008(9) 0.0002(9) P2 0.034(2) 0.0287(19) 0.0178(16) -0.0003(14) 0.000 0.000 O1 0.057(7) 0.038(6) 0.023(5) 0.002(4) 0.000 0.000 O2 0.037(6) 0.024(5) 0.031(5) 0.012(4) 0.000 0.000 C1 0.015(4) 0.029(5) 0.020(4) 0.003(4) 0.001(3) -0.001(4) C2 0.032(5) 0.035(6) 0.021(5) -0.002(4) 0.002(4) 0.006(4) C3 0.053(7) 0.036(6) 0.031(6) 0.005(5) 0.010(5) 0.026(5) C4 0.031(6) 0.048(7) 0.033(6) 0.017(5) 0.001(4) 0.013(5) C5 0.035(6) 0.039(6) 0.032(5) 0.011(4) -0.019(4) 0.004(5) C6 0.026(5) 0.018(5) 0.034(5) 0.000(4) -0.005(4) -0.001(4) C7 0.023(5) 0.028(5) 0.022(4) 0.008(4) -0.006(4) -0.001(4) C8 0.032(6) 0.037(6) 0.034(5) -0.004(4) 0.008(4) -0.010(5) C9 0.048(7) 0.067(9) 0.039(6) 0.027(6) -0.005(5) -0.027(6) C10 0.060(8) 0.033(7) 0.052(7) 0.014(6) -0.028(6) -0.022(6) C11 0.068(8) 0.029(6) 0.045(7) -0.003(5) -0.013(6) -0.008(6) C12 0.039(6) 0.025(5) 0.031(5) 0.003(4) -0.010(4) 0.000(4) C13 0.038(6) 0.042(6) 0.020(5) 0.001(4) -0.006(4) 0.000(5) C14 0.089(10) 0.048(8) 0.063(8) 0.017(6) -0.035(7) -0.029(7) C15 0.102(12) 0.053(9) 0.091(10) 0.014(8) -0.052(10) -0.025(8) C16 0.066(9) 0.069(10) 0.058(8) -0.015(7) -0.014(7) -0.006(8) C17 0.036(6) 0.068(9) 0.031(5) -0.007(6) -0.015(5) 0.020(6) C18 0.044(6) 0.040(6) 0.024(5) 0.001(4) 0.003(4) 0.013(5) C19 0.052(8) 0.046(8) 0.089(10) 0.032(7) -0.006(7) -0.001(6) C20 0.094(17) 0.089(16) 0.096(16) 0.022(9) 0.019(9) 0.008(9) C20' 0.081(14) 0.071(14) 0.086(14) 0.018(9) 0.010(9) 0.008(9) C21 0.096(12) 0.045(9) 0.140(13) 0.063(9) -0.067(10) -0.026(8) C22' 0.096(16) 0.079(15) 0.095(15) 0.015(9) 0.006(9) 0.003(9) C22 0.104(16) 0.081(15) 0.098(15) 0.017(9) -0.010(9) -0.007(9) _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 La1 O1 2.499(9) . ? La1 O2 2.574(8) . ? La1 Se2 3.0744(10) . ? La1 Se2 3.0744(10) 14_755 ? La1 Se1 3.1073(11) . ? La1 Se1 3.1073(11) 14_755 ? La1 Se3 3.1451(16) . ? La1 Se4 3.1485(16) . ? Se1 P1 2.149(2) . ? Se2 P1 2.164(2) . ? Se3 P2 2.159(4) . ? Se4 P2 2.141(4) . ? P1 C7 1.809(9) . ? P1 C1 1.817(9) . ? P2 C13 1.816(10) . ? P2 C13 1.816(10) 14_755 ? O1 C21 1.433(14) 14_755 ? O1 C21 1.433(14) . ? O2 C19 1.457(13) 14_755 ? O2 C19 1.457(13) . ? C1 C2 1.364(12) . ? C1 C6 1.421(12) . ? C2 C3 1.409(13) . ? C3 C4 1.365(14) . ? C4 C5 1.379(14) . ? C5 C6 1.376(12) . ? C7 C8 1.389(12) . ? C7 C12 1.410(12) . ? C8 C9 1.395(14) . ? C9 C10 1.360(16) . ? C10 C11 1.374(16) . ? C11 C12 1.374(14) . ? C13 C14 1.381(15) . ? C13 C18 1.396(13) . ? C14 C15 1.346(16) . ? C15 C16 1.373(17) . ? C16 C17 1.339(17) . ? C17 C18 1.392(14) . ? C19 C20' 1.472(18) . ? C19 C20 1.500(18) . ? C20 C20' 0.54(5) . ? C20 C20 1.432(14) 14_755 ? C20 C20' 1.529(16) 14_755 ? C20' C20' 1.430(19) 14_755 ? C20' C20 1.529(16) 14_755 ? C21 C22 1.482(18) . ? C21 C22' 1.484(18) . ? C22' C22 0.59(4) . ? C22' C22' 1.389(19) 14_755 ? C22' C22 1.508(13) 14_755 ? C22 C22 1.385(19) 14_755 ? C22 C22' 1.508(13) 14_755 ? 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 O1 La1 O2 155.7(3) . . ? O1 La1 Se2 96.66(5) . . ? O2 La1 Se2 88.91(5) . . ? O1 La1 Se2 96.66(5) . 14_755 ? O2 La1 Se2 88.91(5) . 14_755 ? Se2 La1 Se2 152.22(4) . 14_755 ? O1 La1 Se1 77.79(18) . . ? O2 La1 Se1 81.82(17) . . ? Se2 La1 Se1 70.63(3) . . ? Se2 La1 Se1 136.25(3) 14_755 . ? O1 La1 Se1 77.79(18) . 14_755 ? O2 La1 Se1 81.81(17) . 14_755 ? Se2 La1 Se1 136.25(3) . 14_755 ? Se2 La1 Se1 70.63(3) 14_755 14_755 ? Se1 La1 Se1 65.76(4) . 14_755 ? O1 La1 Se3 66.0(2) . . ? O2 La1 Se3 138.3(2) . . ? Se2 La1 Se3 81.67(2) . . ? Se2 La1 Se3 81.67(2) 14_755 . ? Se1 La1 Se3 131.04(3) . . ? Se1 La1 Se3 131.04(3) 14_755 . ? O1 La1 Se4 135.5(2) . . ? O2 La1 Se4 68.8(2) . . ? Se2 La1 Se4 76.70(2) . . ? Se2 La1 Se4 76.70(2) 14_755 . ? Se1 La1 Se4 136.07(3) . . ? Se1 La1 Se4 136.07(3) 14_755 . ? Se3 La1 Se4 69.53(4) . . ? P1 Se1 La1 88.38(6) . . ? P1 Se2 La1 88.96(7) . . ? P2 Se3 La1 88.54(10) . . ? P2 Se4 La1 88.79(10) . . ? C7 P1 C1 104.5(4) . . ? C7 P1 Se1 110.0(3) . . ? C1 P1 Se1 110.3(3) . . ? C7 P1 Se2 109.8(3) . . ? C1 P1 Se2 110.0(3) . . ? Se1 P1 Se2 111.90(10) . . ? C13 P2 C13 104.2(6) . 14_755 ? C13 P2 Se4 110.5(4) . . ? C13 P2 Se4 110.5(4) 14_755 . ? C13 P2 Se3 109.1(3) . . ? C13 P2 Se3 109.1(3) 14_755 . ? Se4 P2 Se3 113.14(16) . . ? C21 O1 C21 107.9(12) 14_755 . ? C21 O1 La1 125.9(6) 14_755 . ? C21 O1 La1 125.9(6) . . ? C19 O2 C19 105.2(10) 14_755 . ? C19 O2 La1 126.7(5) 14_755 . ? C19 O2 La1 126.7(5) . . ? C2 C1 C6 119.5(8) . . ? C2 C1 P1 122.5(7) . . ? C6 C1 P1 117.9(7) . . ? C1 C2 C3 120.0(9) . . ? C4 C3 C2 119.6(9) . . ? C3 C4 C5 121.4(9) . . ? C6 C5 C4 119.5(9) . . ? C5 C6 C1 120.0(9) . . ? C8 C7 C12 117.8(9) . . ? C8 C7 P1 120.3(7) . . ? C12 C7 P1 122.0(7) . . ? C7 C8 C9 120.8(10) . . ? C10 C9 C8 120.6(11) . . ? C9 C10 C11 119.2(10) . . ? C10 C11 C12 121.7(11) . . ? C11 C12 C7 119.9(10) . . ? C14 C13 C18 117.4(10) . . ? C14 C13 P2 121.2(8) . . ? C18 C13 P2 121.4(8) . . ? C15 C14 C13 122.1(12) . . ? C14 C15 C16 120.8(13) . . ? C17 C16 C15 118.5(12) . . ? C16 C17 C18 122.5(11) . . ? C17 C18 C13 118.7(10) . . ? O2 C19 C20' 109.6(10) . . ? O2 C19 C20 105.8(11) . . ? C20' C19 C20 20.8(18) . . ? C20' C20 C20 89.9(13) . 14_755 ? C20' C20 C19 77(3) . . ? C20 C20 C19 107.1(6) 14_755 . ? C20' C20 C20' 69(2) . 14_755 ? C20 C20 C20' 20.6(17) 14_755 14_755 ? C19 C20 C20' 101.2(15) . 14_755 ? C20 C20' C20' 90.1(13) . 14_755 ? C20 C20' C19 83(3) . . ? C20' C20' C19 107.5(7) 14_755 . ? C20 C20' C20 69(2) . 14_755 ? C20' C20' C20 20.6(17) 14_755 14_755 ? C19 C20' C20 103.6(15) . 14_755 ? O1 C21 C22 107.6(12) . . ? O1 C21 C22' 103.7(11) . . ? C22 C21 C22' 23.0(14) . . ? C22 C22' C22' 89.8(14) . 14_755 ? C22 C22' C21 78(3) . . ? C22' C22' C21 108.2(7) 14_755 . ? C22 C22' C22 67(2) . 14_755 ? C22' C22' C22 23.1(14) 14_755 14_755 ? C21 C22' C22 102.0(15) . 14_755 ? C22' C22 C22 90.2(14) . 14_755 ? C22' C22 C21 79(3) . . ? C22 C22 C21 108.3(7) 14_755 . ? C22' C22 C22' 67(2) . 14_755 ? C22 C22 C22' 23.1(14) 14_755 14_755 ? C21 C22 C22' 102.3(15) . 14_755 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.359 _refine_diff_density_min -2.337 _refine_diff_density_rms 0.196 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 data_apx1324 _database_code_depnum_ccdc_archive 'CCDC 906767' #TrackingRef 'web_deposit_cif_file_1_AndrewGaunt_1350598115.cif for 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H46 Ce O2 P3 Se6' _chemical_formula_weight 1313.60 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8457(13) _cell_length_b 13.0684(17) _cell_length_c 19.024(2) _cell_angle_alpha 88.6000(10) _cell_angle_beta 85.6150(10) _cell_angle_gamma 70.4930(10) _cell_volume 2300.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1266 _exptl_absorpt_coefficient_mu 5.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4177 _exptl_absorpt_correction_T_max 0.5911 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26138 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.37 _reflns_number_total 10550 _reflns_number_gt 8443 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _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^)+(0.0313P)^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 10550 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 Ce1 Ce 0.03798(2) 0.785025(16) 0.237093(10) 0.01293(5) Uani 1 1 d . . . Se1 Se 0.29584(4) 0.68047(3) 0.331347(19) 0.01640(8) Uani 1 1 d . . . Se2 Se 0.03636(4) 0.55630(3) 0.29880(2) 0.01760(9) Uani 1 1 d . . . Se3 Se -0.06343(4) 0.87381(3) 0.386808(19) 0.01823(9) Uani 1 1 d . . . Se4 Se -0.21493(4) 1.00261(3) 0.231688(19) 0.01675(8) Uani 1 1 d . . . Se5 Se 0.01160(4) 0.89401(3) 0.09065(2) 0.02101(9) Uani 1 1 d . . . Se6 Se 0.20755(4) 0.61609(3) 0.122238(19) 0.02024(9) Uani 1 1 d . . . P1 P 0.25238(10) 0.52962(7) 0.32779(5) 0.01440(19) Uani 1 1 d . . . P2 P -0.22280(10) 1.01493(7) 0.34508(5) 0.01487(19) Uani 1 1 d . . . P3 P 0.16258(10) 0.74579(8) 0.04613(5) 0.0162(2) Uani 1 1 d . . . O1 O 0.1926(3) 0.9022(2) 0.23904(14) 0.0199(6) Uani 1 1 d . . . O2 O -0.1739(3) 0.7423(2) 0.20123(13) 0.0198(6) Uani 1 1 d . . . C1 C 0.3792(4) 0.4344(3) 0.26607(18) 0.0129(7) Uani 1 1 d . . . C2 C 0.4848(4) 0.4618(3) 0.2251(2) 0.0208(8) Uani 1 1 d . . . H2 H 0.4918 0.5307 0.2286 0.025 Uiso 1 1 calc R . . C3 C 0.5799(4) 0.3862(3) 0.1789(2) 0.0215(8) Uani 1 1 d . . . H3 H 0.6500 0.4050 0.1512 0.026 Uiso 1 1 calc R . . C4 C 0.5715(4) 0.2836(3) 0.1736(2) 0.0218(8) Uani 1 1 d . . . H4 H 0.6367 0.2327 0.1432 0.026 Uiso 1 1 calc R . . C5 C 0.4645(4) 0.2571(3) 0.2141(2) 0.0231(9) Uani 1 1 d . . . H5 H 0.4575 0.1882 0.2103 0.028 Uiso 1 1 calc R . . C6 C 0.3689(4) 0.3313(3) 0.2598(2) 0.0201(8) Uani 1 1 d . . . H6 H 0.2975 0.3128 0.2865 0.024 Uiso 1 1 calc R . . C7 C 0.2854(4) 0.4592(3) 0.41190(18) 0.0166(8) Uani 1 1 d . . . C8 C 0.4244(4) 0.4287(3) 0.4345(2) 0.0214(8) Uani 1 1 d . . . H8 H 0.4975 0.4428 0.4061 0.026 Uiso 1 1 calc R . . C9 C 0.4548(4) 0.3775(3) 0.4989(2) 0.0251(9) Uani 1 1 d . . . H9 H 0.5480 0.3569 0.5138 0.030 Uiso 1 1 calc R . . C10 C 0.3453(5) 0.3573(3) 0.5409(2) 0.0278(10) Uani 1 1 d . . . H10 H 0.3646 0.3241 0.5845 0.033 Uiso 1 1 calc R . . C11 C 0.2084(5) 0.3862(3) 0.5184(2) 0.0266(9) Uani 1 1 d . . . H11 H 0.1359 0.3712 0.5465 0.032 Uiso 1 1 calc R . . C12 C 0.1775(4) 0.4373(3) 0.4542(2) 0.0217(8) Uani 1 1 d . . . H12 H 0.0843 0.4570 0.4394 0.026 Uiso 1 1 calc R . . C13 C -0.1925(4) 1.1387(3) 0.36954(19) 0.0172(8) Uani 1 1 d . . . C14 C -0.2095(4) 1.2227(3) 0.3224(2) 0.0244(9) Uani 1 1 d . . . H14 H -0.2339 1.2150 0.2770 0.029 Uiso 1 1 calc R . . C15 C -0.1908(5) 1.3186(3) 0.3412(2) 0.0308(10) Uani 1 1 d . . . H15 H -0.2016 1.3746 0.3087 0.037 Uiso 1 1 calc R . . C16 C -0.1556(5) 1.3301(3) 0.4098(2) 0.0308(10) Uani 1 1 d . . . H16 H -0.1436 1.3943 0.4231 0.037 Uiso 1 1 calc R . . C17 C -0.1390(5) 1.2478(3) 0.4571(2) 0.0305(10) Uani 1 1 d . . . H17 H -0.1161 1.2562 0.5026 0.037 Uiso 1 1 calc R . . C18 C -0.1560(4) 1.1513(3) 0.4376(2) 0.0245(9) Uani 1 1 d . . . H18 H -0.1432 1.0949 0.4699 0.029 Uiso 1 1 calc R . . C19 C -0.4038(4) 1.0281(3) 0.38313(18) 0.0164(8) Uani 1 1 d . . . C20 C -0.5098(4) 1.1298(3) 0.38818(19) 0.0190(8) Uani 1 1 d . . . H20 H -0.4875 1.1914 0.3745 0.023 Uiso 1 1 calc R . . C21 C -0.6487(4) 1.1389(3) 0.4136(2) 0.0231(9) Uani 1 1 d . . . H21 H -0.7201 1.2069 0.4165 0.028 Uiso 1 1 calc R . . C22 C -0.6823(4) 1.0476(3) 0.43476(19) 0.0245(9) Uani 1 1 d . . . H22 H -0.7758 1.0543 0.4521 0.029 Uiso 1 1 calc R . . C23 C -0.5770(4) 0.9466(3) 0.4301(2) 0.0243(9) Uani 1 1 d . . . H23 H -0.5995 0.8851 0.4441 0.029 Uiso 1 1 calc R . . C24 C -0.4374(4) 0.9368(3) 0.40445(19) 0.0211(8) Uani 1 1 d . . . H24 H -0.3663 0.8688 0.4016 0.025 Uiso 1 1 calc R . . C25 C 0.0924(4) 0.7112(3) -0.03256(19) 0.0171(8) Uani 1 1 d . . . C26 C 0.0624(4) 0.7862(3) -0.0870(2) 0.0243(9) Uani 1 1 d . . . H26 H 0.0784 0.8519 -0.0826 0.029 Uiso 1 1 calc R . . C27 C 0.0091(5) 0.7639(4) -0.1474(2) 0.0325(10) Uani 1 1 d . . . H27 H -0.0110 0.8148 -0.1835 0.039 Uiso 1 1 calc R . . C28 C -0.0148(5) 0.6664(4) -0.1549(2) 0.0331(10) Uani 1 1 d . . . H28 H -0.0497 0.6514 -0.1961 0.040 Uiso 1 1 calc R . . C29 C 0.0134(4) 0.5916(4) -0.1010(2) 0.0307(10) Uani 1 1 d . . . H29 H -0.0044 0.5266 -0.1054 0.037 Uiso 1 1 calc R . . C30 C 0.0682(4) 0.6131(3) -0.0400(2) 0.0257(9) Uani 1 1 d . . . H30 H 0.0889 0.5619 -0.0041 0.031 Uiso 1 1 calc R . . C31 C 0.4574(4) 0.6798(4) 0.0071(2) 0.0281(10) Uani 1 1 d . . . H31 H 0.4573 0.6108 0.0202 0.034 Uiso 1 1 calc R . . C32 C 0.5851(5) 0.6949(5) -0.0189(2) 0.0420(13) Uani 1 1 d . . . H32 H 0.6701 0.6358 -0.0236 0.050 Uiso 1 1 calc R . . C33 C 0.5860(6) 0.7968(5) -0.0377(2) 0.0455(14) Uani 1 1 d . . . H33 H 0.6721 0.8071 -0.0539 0.055 Uiso 1 1 calc R . . C34 C 0.4598(6) 0.8836(4) -0.0326(2) 0.0431(14) Uani 1 1 d . . . H34 H 0.4602 0.9521 -0.0467 0.052 Uiso 1 1 calc R . . C35 C 0.3313(5) 0.8697(3) -0.0063(2) 0.0278(10) Uani 1 1 d . . . H35 H 0.2464 0.9290 -0.0022 0.033 Uiso 1 1 calc R . . C36 C 0.3300(4) 0.7677(3) 0.01355(19) 0.0205(8) Uani 1 1 d . . . C37 C 0.3271(4) 0.8768(3) 0.1955(2) 0.0275(10) Uani 1 1 d . . . H37A H 0.3226 0.8394 0.1528 0.033 Uiso 1 1 calc R . . H37B H 0.4076 0.8319 0.2209 0.033 Uiso 1 1 calc R . . C38 C 0.3416(5) 0.9863(3) 0.1786(2) 0.0275(9) Uani 1 1 d . . . H38A H 0.2824 1.0219 0.1408 0.033 Uiso 1 1 calc R . . H38B H 0.4413 0.9801 0.1658 0.033 Uiso 1 1 calc R . . C39 C 0.2872(5) 1.0462(4) 0.2481(2) 0.0305(10) Uani 1 1 d . . . H39A H 0.2468 1.1239 0.2406 0.037 Uiso 1 1 calc R . . H39B H 0.3644 1.0320 0.2796 0.037 Uiso 1 1 calc R . . C40 C 0.1709(5) 1.0006(4) 0.2782(2) 0.0318(10) Uani 1 1 d . . . H40A H 0.1806 0.9848 0.3280 0.038 Uiso 1 1 calc R . . H40B H 0.0754 1.0522 0.2723 0.038 Uiso 1 1 calc R . . C41 C -0.2273(5) 0.7188(4) 0.1374(2) 0.0308(10) Uani 1 1 d . . . H41A H -0.1481 0.6783 0.1047 0.037 Uiso 1 1 calc R . . H41B H -0.2827 0.7854 0.1147 0.037 Uiso 1 1 calc R . . C42 C -0.3229(5) 0.6514(4) 0.1602(2) 0.0344(11) Uani 1 1 d . . . H42A H -0.2823 0.5786 0.1410 0.041 Uiso 1 1 calc R . . H42B H -0.4192 0.6847 0.1444 0.041 Uiso 1 1 calc R . . C43 C -0.3269(5) 0.6490(3) 0.2411(2) 0.0298(10) Uani 1 1 d . . . H43A H -0.4233 0.6582 0.2618 0.036 Uiso 1 1 calc R . . H43B H -0.2600 0.5817 0.2579 0.036 Uiso 1 1 calc R . . C44 C -0.2811(4) 0.7442(3) 0.2572(2) 0.0262(9) Uani 1 1 d . . . H44A H -0.3621 0.8115 0.2569 0.031 Uiso 1 1 calc R . . H44B H -0.2406 0.7358 0.3027 0.031 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 Ce1 0.01374(10) 0.01256(10) 0.01264(11) 0.00005(8) 0.00009(8) -0.00481(8) Se1 0.01661(19) 0.01414(18) 0.01833(19) -0.00004(14) -0.00204(15) -0.00480(15) Se2 0.01565(19) 0.01729(19) 0.0204(2) 0.00230(15) -0.00176(15) -0.00627(15) Se3 0.0204(2) 0.01621(19) 0.01396(19) 0.00132(14) -0.00079(15) -0.00087(15) Se4 0.01894(19) 0.01543(19) 0.01320(18) -0.00027(14) -0.00078(14) -0.00225(15) Se5 0.0281(2) 0.01474(19) 0.01565(19) 0.00141(15) 0.00291(16) -0.00216(16) Se6 0.0278(2) 0.01446(19) 0.01531(19) 0.00079(15) 0.00115(16) -0.00352(16) P1 0.0140(5) 0.0150(5) 0.0134(5) 0.0001(4) 0.0003(4) -0.0040(4) P2 0.0174(5) 0.0124(5) 0.0134(5) 0.0003(4) -0.0002(4) -0.0033(4) P3 0.0196(5) 0.0155(5) 0.0127(5) 0.0001(4) 0.0016(4) -0.0057(4) O1 0.0174(14) 0.0150(13) 0.0277(15) -0.0023(11) 0.0027(11) -0.0065(11) O2 0.0169(14) 0.0246(15) 0.0195(14) -0.0003(11) -0.0028(11) -0.0085(12) C1 0.0153(18) 0.0123(17) 0.0096(17) 0.0019(13) -0.0022(14) -0.0025(14) C2 0.020(2) 0.017(2) 0.026(2) 0.0020(16) 0.0007(16) -0.0077(16) C3 0.018(2) 0.026(2) 0.019(2) 0.0007(16) 0.0053(16) -0.0068(17) C4 0.023(2) 0.023(2) 0.015(2) -0.0057(16) 0.0027(16) -0.0037(17) C5 0.028(2) 0.019(2) 0.024(2) -0.0033(16) -0.0002(17) -0.0096(18) C6 0.020(2) 0.020(2) 0.020(2) -0.0018(16) 0.0044(16) -0.0081(16) C7 0.025(2) 0.0108(18) 0.0139(18) -0.0037(14) -0.0016(15) -0.0052(16) C8 0.025(2) 0.021(2) 0.018(2) 0.0034(16) -0.0024(16) -0.0070(17) C9 0.028(2) 0.021(2) 0.026(2) 0.0010(17) -0.0110(18) -0.0059(18) C10 0.048(3) 0.016(2) 0.015(2) 0.0027(16) -0.0007(19) -0.0069(19) C11 0.034(2) 0.014(2) 0.027(2) 0.0010(17) 0.0105(19) -0.0049(18) C12 0.020(2) 0.016(2) 0.025(2) 0.0005(16) 0.0042(17) -0.0028(16) C13 0.0166(19) 0.0151(19) 0.019(2) -0.0020(15) 0.0004(15) -0.0047(15) C14 0.034(2) 0.021(2) 0.021(2) 0.0018(16) -0.0105(18) -0.0119(18) C15 0.039(3) 0.021(2) 0.035(3) 0.0060(18) -0.008(2) -0.012(2) C16 0.035(3) 0.021(2) 0.040(3) -0.0020(19) -0.013(2) -0.0114(19) C17 0.038(3) 0.027(2) 0.028(2) -0.0047(19) -0.012(2) -0.010(2) C18 0.029(2) 0.021(2) 0.021(2) 0.0009(17) -0.0040(17) -0.0041(18) C19 0.0170(19) 0.020(2) 0.0097(17) -0.0018(14) 0.0007(14) -0.0037(16) C20 0.024(2) 0.0162(19) 0.0157(19) 0.0009(15) -0.0036(16) -0.0050(16) C21 0.020(2) 0.022(2) 0.023(2) -0.0005(17) -0.0018(16) -0.0018(17) C22 0.021(2) 0.035(2) 0.015(2) -0.0014(17) 0.0014(16) -0.0060(18) C23 0.032(2) 0.020(2) 0.022(2) 0.0021(16) 0.0017(18) -0.0116(18) C24 0.024(2) 0.016(2) 0.020(2) 0.0020(16) 0.0008(16) -0.0043(16) C25 0.0149(18) 0.022(2) 0.0139(18) -0.0036(15) 0.0007(14) -0.0061(16) C26 0.030(2) 0.023(2) 0.019(2) 0.0024(17) -0.0064(17) -0.0078(18) C27 0.034(3) 0.041(3) 0.023(2) 0.006(2) -0.0111(19) -0.011(2) C28 0.031(2) 0.046(3) 0.024(2) -0.005(2) -0.0081(19) -0.013(2) C29 0.030(2) 0.032(2) 0.034(3) -0.012(2) 0.004(2) -0.016(2) C30 0.032(2) 0.026(2) 0.022(2) -0.0005(17) 0.0008(18) -0.0138(19) C31 0.024(2) 0.042(3) 0.018(2) -0.0011(18) -0.0008(17) -0.011(2) C32 0.021(2) 0.076(4) 0.027(3) -0.001(2) 0.0002(19) -0.014(2) C33 0.043(3) 0.085(4) 0.024(3) -0.007(3) 0.006(2) -0.044(3) C34 0.069(4) 0.058(3) 0.023(2) -0.012(2) 0.015(2) -0.052(3) C35 0.039(3) 0.032(2) 0.017(2) -0.0067(18) 0.0083(18) -0.019(2) C36 0.024(2) 0.030(2) 0.0102(18) -0.0032(16) 0.0022(15) -0.0141(18) C37 0.020(2) 0.027(2) 0.036(3) -0.0025(19) 0.0037(18) -0.0097(18) C38 0.033(2) 0.032(2) 0.023(2) 0.0039(18) -0.0004(18) -0.019(2) C39 0.036(3) 0.030(2) 0.033(2) 0.0002(19) 0.000(2) -0.021(2) C40 0.037(3) 0.034(3) 0.032(2) -0.010(2) 0.004(2) -0.023(2) C41 0.033(2) 0.037(3) 0.028(2) -0.0017(19) -0.0113(19) -0.017(2) C42 0.024(2) 0.042(3) 0.041(3) -0.015(2) -0.002(2) -0.014(2) C43 0.024(2) 0.032(2) 0.037(3) -0.003(2) -0.0020(19) -0.0141(19) C44 0.018(2) 0.035(2) 0.028(2) -0.0010(19) -0.0009(17) -0.0115(18) _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 Ce1 O2 2.479(2) . ? Ce1 O1 2.496(2) . ? Ce1 Se3 3.0674(5) . ? Ce1 Se5 3.0867(5) . ? Ce1 Se4 3.0973(5) . ? Ce1 Se6 3.1068(5) . ? Ce1 Se1 3.1285(5) . ? Ce1 Se2 3.1892(5) . ? Se1 P1 2.1560(10) . ? Se2 P1 2.1503(10) . ? Se3 P2 2.1633(10) . ? Se4 P2 2.1606(10) . ? Se5 P3 2.1549(10) . ? Se6 P3 2.1547(10) . ? P1 C1 1.815(4) . ? P1 C7 1.822(4) . ? P2 C13 1.817(4) . ? P2 C19 1.826(4) . ? P3 C25 1.823(4) . ? P3 C36 1.825(4) . ? O1 C40 1.446(4) . ? O1 C37 1.450(4) . ? O2 C44 1.435(4) . ? O2 C41 1.438(4) . ? C1 C2 1.388(5) . ? C1 C6 1.393(5) . ? C2 C3 1.387(5) . ? C3 C4 1.377(5) . ? C4 C5 1.390(5) . ? C5 C6 1.374(5) . ? C7 C12 1.385(5) . ? C7 C8 1.391(5) . ? C8 C9 1.387(5) . ? C9 C10 1.385(6) . ? C10 C11 1.372(6) . ? C11 C12 1.383(5) . ? C13 C14 1.375(5) . ? C13 C18 1.398(5) . ? C14 C15 1.385(5) . ? C15 C16 1.400(6) . ? C16 C17 1.360(6) . ? C17 C18 1.390(5) . ? C19 C24 1.384(5) . ? C19 C20 1.389(5) . ? C20 C21 1.382(5) . ? C21 C22 1.384(5) . ? C22 C23 1.380(5) . ? C23 C24 1.388(5) . ? C25 C26 1.386(5) . ? C25 C30 1.392(5) . ? C26 C27 1.376(5) . ? C27 C28 1.383(6) . ? C28 C29 1.377(6) . ? C29 C30 1.389(5) . ? C31 C36 1.389(6) . ? C31 C32 1.389(6) . ? C32 C33 1.374(7) . ? C33 C34 1.373(7) . ? C34 C35 1.391(6) . ? C35 C36 1.381(5) . ? C37 C38 1.509(5) . ? C38 C39 1.520(5) . ? C39 C40 1.527(5) . ? C41 C42 1.523(6) . ? C42 C43 1.536(6) . ? C43 C44 1.503(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 O2 Ce1 O1 153.11(8) . . ? O2 Ce1 Se3 102.08(6) . . ? O1 Ce1 Se3 83.42(6) . . ? O2 Ce1 Se5 81.16(6) . . ? O1 Ce1 Se5 76.15(6) . . ? Se3 Ce1 Se5 132.714(14) . . ? O2 Ce1 Se4 72.88(6) . . ? O1 Ce1 Se4 84.73(6) . . ? Se3 Ce1 Se4 70.056(11) . . ? Se5 Ce1 Se4 66.006(11) . . ? O2 Ce1 Se6 84.07(6) . . ? O1 Ce1 Se6 101.31(6) . . ? Se3 Ce1 Se6 156.731(12) . . ? Se5 Ce1 Se6 70.145(14) . . ? Se4 Ce1 Se6 132.758(13) . . ? O2 Ce1 Se1 137.29(6) . . ? O1 Ce1 Se1 69.58(6) . . ? Se3 Ce1 Se1 73.048(13) . . ? Se5 Ce1 Se1 133.902(13) . . ? Se4 Ce1 Se1 136.927(12) . . ? Se6 Ce1 Se1 87.142(13) . . ? O2 Ce1 Se2 68.98(6) . . ? O1 Ce1 Se2 137.90(6) . . ? Se3 Ce1 Se2 86.401(13) . . ? Se5 Ce1 Se2 135.722(12) . . ? Se4 Ce1 Se2 129.212(13) . . ? Se6 Ce1 Se2 74.779(13) . . ? Se1 Ce1 Se2 68.370(11) . . ? P1 Se1 Ce1 88.76(3) . . ? P1 Se2 Ce1 87.28(3) . . ? P2 Se3 Ce1 90.41(3) . . ? P2 Se4 Ce1 89.66(3) . . ? P3 Se5 Ce1 89.07(3) . . ? P3 Se6 Ce1 88.55(3) . . ? C1 P1 C7 103.03(16) . . ? C1 P1 Se2 108.97(11) . . ? C7 P1 Se2 111.72(12) . . ? C1 P1 Se1 111.63(12) . . ? C7 P1 Se1 110.18(11) . . ? Se2 P1 Se1 111.05(4) . . ? C13 P2 C19 105.36(16) . . ? C13 P2 Se4 110.09(12) . . ? C19 P2 Se4 109.87(12) . . ? C13 P2 Se3 110.81(12) . . ? C19 P2 Se3 110.79(12) . . ? Se4 P2 Se3 109.84(4) . . ? C25 P3 C36 104.17(16) . . ? C25 P3 Se6 111.90(13) . . ? C36 P3 Se6 110.01(13) . . ? C25 P3 Se5 109.22(12) . . ? C36 P3 Se5 109.96(13) . . ? Se6 P3 Se5 111.34(4) . . ? C40 O1 C37 108.8(3) . . ? C40 O1 Ce1 130.2(2) . . ? C37 O1 Ce1 121.0(2) . . ? C44 O2 C41 106.8(3) . . ? C44 O2 Ce1 115.1(2) . . ? C41 O2 Ce1 138.0(2) . . ? C2 C1 C6 119.5(3) . . ? C2 C1 P1 121.9(3) . . ? C6 C1 P1 118.6(3) . . ? C3 C2 C1 119.9(3) . . ? C4 C3 C2 120.6(3) . . ? C3 C4 C5 119.2(3) . . ? C6 C5 C4 120.8(4) . . ? C5 C6 C1 119.9(3) . . ? C12 C7 C8 119.4(3) . . ? C12 C7 P1 122.6(3) . . ? C8 C7 P1 117.9(3) . . ? C9 C8 C7 120.4(4) . . ? C10 C9 C8 119.4(4) . . ? C11 C10 C9 120.3(4) . . ? C10 C11 C12 120.5(4) . . ? C11 C12 C7 119.9(4) . . ? C14 C13 C18 118.9(3) . . ? C14 C13 P2 120.8(3) . . ? C18 C13 P2 120.3(3) . . ? C13 C14 C15 121.2(4) . . ? C14 C15 C16 119.1(4) . . ? C17 C16 C15 120.4(4) . . ? C16 C17 C18 120.3(4) . . ? C17 C18 C13 120.2(4) . . ? C24 C19 C20 119.8(3) . . ? C24 C19 P2 120.3(3) . . ? C20 C19 P2 119.8(3) . . ? C21 C20 C19 119.7(4) . . ? C20 C21 C22 120.4(4) . . ? C23 C22 C21 120.0(4) . . ? C22 C23 C24 119.9(4) . . ? C19 C24 C23 120.2(4) . . ? C26 C25 C30 119.1(3) . . ? C26 C25 P3 118.2(3) . . ? C30 C25 P3 122.7(3) . . ? C27 C26 C25 120.4(4) . . ? C26 C27 C28 120.6(4) . . ? C29 C28 C27 119.7(4) . . ? C28 C29 C30 120.1(4) . . ? C29 C30 C25 120.2(4) . . ? C36 C31 C32 120.0(4) . . ? C33 C32 C31 120.2(5) . . ? C34 C33 C32 119.9(4) . . ? C33 C34 C35 120.5(5) . . ? C36 C35 C34 119.8(4) . . ? C35 C36 C31 119.5(4) . . ? C35 C36 P3 121.1(3) . . ? C31 C36 P3 119.4(3) . . ? O1 C37 C38 104.0(3) . . ? C37 C38 C39 101.8(3) . . ? C38 C39 C40 104.0(3) . . ? O1 C40 C39 106.1(3) . . ? O2 C41 C42 105.4(3) . . ? C41 C42 C43 105.1(3) . . ? C44 C43 C42 102.3(3) . . ? O2 C44 C43 103.6(3) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.805 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.132 data_apx1320s _database_code_depnum_ccdc_archive 'CCDC 906768' #TrackingRef 'web_deposit_cif_file_2_AndrewGaunt_1350598115.cif for 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H53 Nd O2 P3 Se6' _chemical_formula_weight 1360.80 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/nmc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y, z' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 31.4695(18) _cell_length_b 31.4695(18) _cell_length_c 10.6442(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10541.3(15) _cell_formula_units_Z 8 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light purple' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5280 _exptl_absorpt_coefficient_mu 5.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5267 _exptl_absorpt_correction_T_max 0.5713 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 75919 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.84 _reflns_number_total 5291 _reflns_number_gt 4561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The symmetry related C-C distances (-0.5-x, y, z) in each thf ligand were restrained to chemically reasonably values. ; # 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 0.250 0.750 0.229 544 140 hexane 2 0.250 0.250 0.473 284 80 hexane 3 0.750 0.250 0.768 544 138 hexane 4 0.750 0.750 0.524 284 78 hexane _platon_squeeze_details ; ; _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^)+(0.0300P)^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 5291 _refine_ls_number_parameters 262 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.346 _refine_ls_restrained_S_all 1.352 _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 Nd1 Nd 0.7500 0.500204(10) 0.04385(3) 0.01651(9) Uani 1 2 d S . . Se1 Se 0.697457(13) 0.460317(14) -0.16732(4) 0.02235(11) Uani 1 1 d . . . Se2 Se 0.657027(12) 0.506888(13) 0.11207(4) 0.02072(11) Uani 1 1 d . . . Se3 Se 0.7500 0.59183(2) 0.15382(5) 0.02790(16) Uani 1 2 d S . . Se4 Se 0.7500 0.496748(19) 0.33543(5) 0.02460(15) Uani 1 2 d S . . P1 P 0.64126(3) 0.47316(3) -0.05893(9) 0.0175(2) Uani 1 1 d . . . P2 P 0.7500 0.56496(5) 0.33983(14) 0.0226(4) Uani 1 2 d S . . O1 O 0.7500 0.55626(13) -0.1160(4) 0.0286(10) Uani 1 2 d S . . O2 O 0.7500 0.42439(12) 0.1229(4) 0.0244(9) Uani 1 2 d S . . C1 C 0.60296(12) 0.50295(13) -0.1510(4) 0.0190(9) Uani 1 1 d . . . C2 C 0.58799(13) 0.54210(13) -0.1132(4) 0.0261(10) Uani 1 1 d . . . H2 H 0.5980 0.5542 -0.0393 0.031 Uiso 1 1 calc R . . C3 C 0.55798(14) 0.56362(14) -0.1850(4) 0.0322(11) Uani 1 1 d . . . H3 H 0.5478 0.5899 -0.1587 0.039 Uiso 1 1 calc R . . C4 C 0.54357(13) 0.54601(14) -0.2938(4) 0.0295(11) Uani 1 1 d . . . H4 H 0.5233 0.5603 -0.3411 0.035 Uiso 1 1 calc R . . C5 C 0.55855(14) 0.50733(14) -0.3349(4) 0.0313(11) Uani 1 1 d . . . H5 H 0.5489 0.4960 -0.4104 0.038 Uiso 1 1 calc R . . C6 C 0.58787(13) 0.48551(13) -0.2640(4) 0.0264(10) Uani 1 1 d . . . H6 H 0.5977 0.4592 -0.2910 0.032 Uiso 1 1 calc R . . C7 C 0.61393(12) 0.42385(13) -0.0219(4) 0.0205(9) Uani 1 1 d . . . C8 C 0.58072(14) 0.42375(14) 0.0647(4) 0.0313(11) Uani 1 1 d . . . H8 H 0.5731 0.4489 0.1044 0.038 Uiso 1 1 calc R . . C9 C 0.55899(16) 0.38681(16) 0.0925(4) 0.0393(12) Uani 1 1 d . . . H9 H 0.5370 0.3872 0.1509 0.047 Uiso 1 1 calc R . . C10 C 0.56984(16) 0.34935(15) 0.0340(5) 0.0403(13) Uani 1 1 d . . . H10 H 0.5551 0.3245 0.0521 0.048 Uiso 1 1 calc R . . C11 C 0.60274(16) 0.34887(15) -0.0519(5) 0.0387(12) Uani 1 1 d . . . H11 H 0.6102 0.3235 -0.0909 0.046 Uiso 1 1 calc R . . C12 C 0.62457(14) 0.38562(13) -0.0803(4) 0.0274(10) Uani 1 1 d . . . H12 H 0.6465 0.3849 -0.1388 0.033 Uiso 1 1 calc R . . C13 C 0.79553(13) 0.58495(14) 0.4268(4) 0.0268(10) Uani 1 1 d . . . C14 C 0.80654(18) 0.62724(17) 0.4223(5) 0.0539(16) Uani 1 1 d . . . H14 H 0.7916 0.6453 0.3691 0.065 Uiso 1 1 calc R . . C15 C 0.83887(18) 0.64360(18) 0.4936(6) 0.0623(17) Uani 1 1 d . . . H15 H 0.8452 0.6724 0.4895 0.075 Uiso 1 1 calc R . . C16 C 0.86196(17) 0.61749(19) 0.5712(5) 0.0503(15) Uani 1 1 d . . . H16 H 0.8837 0.6285 0.6205 0.060 Uiso 1 1 calc R . . C17 C 0.85256(15) 0.57520(18) 0.5751(4) 0.0397(13) Uani 1 1 d . . . H17 H 0.8687 0.5573 0.6255 0.048 Uiso 1 1 calc R . . C18 C 0.81931(15) 0.55842(16) 0.5050(4) 0.0341(11) Uani 1 1 d . . . H18 H 0.8129 0.5296 0.5102 0.041 Uiso 1 1 calc R . . C19 C 0.71306(15) 0.40055(15) 0.1611(5) 0.0439(13) Uani 1 1 d . . . H19A H 0.7000 0.3870 0.0889 0.053 Uiso 1 1 calc R . . H19B H 0.6923 0.4192 0.1997 0.053 Uiso 1 1 calc R . . C20 C 0.72752(12) 0.3681(2) 0.2524(7) 0.108(3) Uani 1 1 d D . . H20A H 0.7169 0.3749 0.3357 0.130 Uiso 1 1 calc R . . H20B H 0.7169 0.3403 0.2287 0.130 Uiso 1 1 calc R . . C21 C 0.71262(18) 0.57814(17) -0.1603(6) 0.0659(19) Uani 1 1 d . . . H21A H 0.6929 0.5830 -0.0918 0.079 Uiso 1 1 calc R . . H21B H 0.6984 0.5616 -0.2248 0.079 Uiso 1 1 calc R . . C22 C 0.72794(13) 0.6192(2) -0.2124(9) 0.135(4) Uani 1 1 d D . . H22A H 0.7174 0.6228 -0.2974 0.161 Uiso 1 1 calc R . . H22B H 0.7174 0.6425 -0.1616 0.161 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 Nd1 0.01476(17) 0.02105(18) 0.01371(15) -0.00160(13) 0.000 0.000 Se1 0.0149(2) 0.0323(3) 0.0199(2) -0.00779(18) 0.00074(17) -0.00022(18) Se2 0.0164(2) 0.0278(2) 0.0179(2) -0.00450(18) 0.00189(17) 0.00008(18) Se3 0.0417(4) 0.0246(3) 0.0174(3) -0.0009(3) 0.000 0.000 Se4 0.0311(4) 0.0253(3) 0.0174(3) -0.0003(3) 0.000 0.000 P1 0.0143(5) 0.0203(6) 0.0179(5) 0.0001(4) -0.0004(4) -0.0001(4) P2 0.0254(9) 0.0252(9) 0.0173(8) -0.0028(7) 0.000 0.000 O1 0.036(3) 0.027(2) 0.023(2) 0.0051(19) 0.000 0.000 O2 0.027(2) 0.019(2) 0.027(2) 0.0083(18) 0.000 0.000 C1 0.014(2) 0.025(2) 0.018(2) 0.0049(18) 0.0023(16) -0.0015(18) C2 0.032(3) 0.029(3) 0.017(2) -0.0002(19) 0.0034(19) 0.007(2) C3 0.037(3) 0.029(3) 0.030(3) 0.004(2) 0.009(2) 0.017(2) C4 0.018(2) 0.037(3) 0.034(3) 0.017(2) -0.001(2) 0.008(2) C5 0.036(3) 0.028(3) 0.029(2) 0.005(2) -0.013(2) -0.004(2) C6 0.025(2) 0.021(2) 0.033(3) -0.0013(19) -0.008(2) 0.0014(19) C7 0.017(2) 0.024(2) 0.020(2) 0.0043(18) -0.0035(17) -0.0032(18) C8 0.033(3) 0.030(3) 0.031(3) 0.004(2) 0.003(2) -0.006(2) C9 0.040(3) 0.046(3) 0.032(3) 0.013(2) 0.003(2) -0.013(3) C10 0.047(3) 0.032(3) 0.043(3) 0.017(2) -0.018(3) -0.018(2) C11 0.053(3) 0.021(3) 0.042(3) -0.003(2) -0.009(3) -0.006(2) C12 0.029(3) 0.024(2) 0.029(2) 0.0015(19) -0.006(2) 0.001(2) C13 0.024(2) 0.032(3) 0.024(2) -0.0028(19) -0.0001(19) -0.003(2) C14 0.066(4) 0.043(3) 0.053(4) 0.007(3) -0.026(3) -0.015(3) C15 0.064(4) 0.050(4) 0.074(4) 0.008(3) -0.026(3) -0.024(3) C16 0.038(3) 0.066(4) 0.046(3) -0.010(3) -0.009(3) -0.010(3) C17 0.028(3) 0.064(4) 0.027(3) -0.001(3) -0.008(2) 0.011(3) C18 0.031(3) 0.041(3) 0.031(3) -0.002(2) 0.001(2) 0.004(2) C19 0.035(3) 0.035(3) 0.062(3) 0.015(3) -0.001(3) -0.002(2) C20 0.061(4) 0.101(6) 0.163(7) 0.104(5) 0.049(4) 0.033(4) C21 0.065(4) 0.040(4) 0.093(5) 0.036(3) -0.035(4) -0.009(3) C22 0.088(6) 0.066(5) 0.250(11) 0.102(6) -0.020(6) -0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.451(4) . ? Nd1 O2 2.530(4) . ? Nd1 Se2 3.0219(4) . ? Nd1 Se2 3.0220(4) 14_755 ? Nd1 Se1 3.0597(5) 14_755 ? Nd1 Se1 3.0598(5) . ? Nd1 Se4 3.1055(7) . ? Nd1 Se3 3.1119(7) . ? Se1 P1 2.1499(11) . ? Se2 P1 2.1646(11) . ? Se3 P2 2.1530(16) . ? Se4 P2 2.1472(17) . ? P1 C1 1.814(4) . ? P1 C7 1.817(4) . ? P2 C13 1.818(4) 14_755 ? P2 C13 1.818(4) . ? O1 C21 1.442(5) 14_755 ? O1 C21 1.442(5) . ? O2 C19 1.442(5) . ? O2 C19 1.442(5) 14_755 ? C1 C2 1.379(5) . ? C1 C6 1.405(5) . ? C2 C3 1.390(6) . ? C3 C4 1.362(6) . ? C4 C5 1.376(6) . ? C5 C6 1.375(6) . ? C7 C8 1.394(6) . ? C7 C12 1.395(6) . ? C8 C9 1.381(6) . ? C9 C10 1.377(7) . ? C10 C11 1.381(7) . ? C11 C12 1.379(6) . ? C13 C14 1.376(6) . ? C13 C18 1.397(6) . ? C14 C15 1.370(7) . ? C15 C16 1.373(7) . ? C16 C17 1.364(7) . ? C17 C18 1.389(6) . ? C19 C20 1.481(7) . ? C20 C20 1.415(8) 14_755 ? C21 C22 1.486(7) . ? C22 C22 1.389(8) 14_755 ? 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 O1 Nd1 O2 155.46(13) . . ? O1 Nd1 Se2 96.70(2) . . ? O2 Nd1 Se2 89.18(2) . . ? O1 Nd1 Se2 96.70(2) . 14_755 ? O2 Nd1 Se2 89.18(2) . 14_755 ? Se2 Nd1 Se2 151.029(18) . 14_755 ? O1 Nd1 Se1 77.60(8) . 14_755 ? O2 Nd1 Se1 81.80(8) . 14_755 ? Se2 Nd1 Se1 136.741(13) . 14_755 ? Se2 Nd1 Se1 71.448(12) 14_755 14_755 ? O1 Nd1 Se1 77.60(8) . . ? O2 Nd1 Se1 81.80(8) . . ? Se2 Nd1 Se1 71.448(11) . . ? Se2 Nd1 Se1 136.741(13) 14_755 . ? Se1 Nd1 Se1 65.420(17) 14_755 . ? O1 Nd1 Se4 135.97(10) . . ? O2 Nd1 Se4 68.57(9) . . ? Se2 Nd1 Se4 76.251(9) . . ? Se2 Nd1 Se4 76.252(9) 14_755 . ? Se1 Nd1 Se4 136.041(13) 14_755 . ? Se1 Nd1 Se4 136.039(13) . . ? O1 Nd1 Se3 66.06(9) . . ? O2 Nd1 Se3 138.49(9) . . ? Se2 Nd1 Se3 81.091(10) . . ? Se2 Nd1 Se3 81.091(10) 14_755 . ? Se1 Nd1 Se3 131.026(14) 14_755 . ? Se1 Nd1 Se3 131.027(13) . . ? Se4 Nd1 Se3 69.914(17) . . ? P1 Se1 Nd1 88.46(3) . . ? P1 Se2 Nd1 89.18(3) . . ? P2 Se3 Nd1 88.97(5) . . ? P2 Se4 Nd1 89.24(4) . . ? C1 P1 C7 104.12(18) . . ? C1 P1 Se1 110.73(13) . . ? C7 P1 Se1 110.19(14) . . ? C1 P1 Se2 110.67(14) . . ? C7 P1 Se2 110.16(13) . . ? Se1 P1 Se2 110.79(5) . . ? C13 P2 C13 104.0(3) 14_755 . ? C13 P2 Se4 110.92(15) 14_755 . ? C13 P2 Se4 110.92(15) . . ? C13 P2 Se3 109.40(15) 14_755 . ? C13 P2 Se3 109.40(15) . . ? Se4 P2 Se3 111.87(7) . . ? C21 O1 C21 109.3(5) 14_755 . ? C21 O1 Nd1 124.8(3) 14_755 . ? C21 O1 Nd1 124.8(3) . . ? C19 O2 C19 107.4(4) . 14_755 ? C19 O2 Nd1 125.8(2) . . ? C19 O2 Nd1 125.8(2) 14_755 . ? C2 C1 C6 118.9(4) . . ? C2 C1 P1 122.1(3) . . ? C6 C1 P1 119.0(3) . . ? C1 C2 C3 120.5(4) . . ? C4 C3 C2 119.7(4) . . ? C3 C4 C5 121.1(4) . . ? C6 C5 C4 119.8(4) . . ? C5 C6 C1 120.1(4) . . ? C8 C7 C12 118.2(4) . . ? C8 C7 P1 120.0(3) . . ? C12 C7 P1 121.7(3) . . ? C9 C8 C7 121.0(4) . . ? C10 C9 C8 120.1(5) . . ? C9 C10 C11 119.7(4) . . ? C12 C11 C10 120.6(5) . . ? C11 C12 C7 120.4(4) . . ? C14 C13 C18 117.6(4) . . ? C14 C13 P2 121.0(4) . . ? C18 C13 P2 121.3(3) . . ? C15 C14 C13 122.1(5) . . ? C14 C15 C16 120.1(5) . . ? C17 C16 C15 119.2(5) . . ? C16 C17 C18 121.2(5) . . ? C17 C18 C13 119.8(5) . . ? O2 C19 C20 107.2(4) . . ? C20 C20 C19 107.9(2) 14_755 . ? O1 C21 C22 105.8(4) . . ? C22 C22 C21 108.9(3) 14_755 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.795 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.102 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 data_apx1349 _database_code_depnum_ccdc_archive 'CCDC 906769' #TrackingRef 'web_deposit_cif_file_3_AndrewGaunt_1350598115.cif for 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 La N2 P3 Se6' _chemical_formula_weight 1250.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.5653(10) _cell_length_b 9.0111(7) _cell_length_c 35.576(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.9450(10) _cell_angle_gamma 90.00 _cell_volume 4346.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 6.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5257 _exptl_absorpt_correction_T_max 0.7485 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47827 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.40 _reflns_number_total 10171 _reflns_number_gt 7646 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _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^)+(0.0327P)^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 10171 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 La1 La 0.660245(18) 0.74315(3) 0.122632(7) 0.01410(7) Uani 1 1 d . . . Se1 Se 0.80882(3) 0.98018(5) 0.149678(13) 0.02113(11) Uani 1 1 d . . . Se2 Se 0.82334(3) 0.77573(5) 0.063743(13) 0.02011(11) Uani 1 1 d . . . Se3 Se 0.81624(3) 0.52637(5) 0.157118(12) 0.01875(11) Uani 1 1 d . . . Se4 Se 0.62324(3) 0.70901(5) 0.206952(13) 0.02228(11) Uani 1 1 d . . . Se5 Se 0.44072(3) 0.64453(5) 0.122898(12) 0.01703(10) Uani 1 1 d . . . Se6 Se 0.55381(3) 0.84423(5) 0.048698(12) 0.01872(11) Uani 1 1 d . . . P1 P 0.90227(8) 0.90649(12) 0.10580(3) 0.0156(2) Uani 1 1 d . . . P2 P 0.75193(8) 0.56832(12) 0.21047(3) 0.0156(2) Uani 1 1 d . . . P3 P 0.41788(8) 0.79514(12) 0.07617(3) 0.0157(2) Uani 1 1 d . . . N1 N 0.5674(3) 0.9880(4) 0.14631(11) 0.0216(9) Uani 1 1 d . . . N2 N 0.6508(3) 0.4862(4) 0.08760(11) 0.0236(9) Uani 1 1 d . . . C1 C 1.0063(3) 0.8015(5) 0.12531(13) 0.0178(10) Uani 1 1 d . . . C2 C 1.0590(3) 0.7092(5) 0.10159(14) 0.0217(10) Uani 1 1 d . . . H2 H 1.0394 0.6991 0.0764 0.026 Uiso 1 1 calc R . . C3 C 1.1414(3) 0.6324(5) 0.11600(15) 0.0261(11) Uani 1 1 d . . . H3 H 1.1778 0.5732 0.1002 0.031 Uiso 1 1 calc R . . C4 C 1.1690(3) 0.6439(5) 0.15345(15) 0.0286(12) Uani 1 1 d . . . H4 H 1.2229 0.5904 0.1630 0.034 Uiso 1 1 calc R . . C5 C 1.1167(4) 0.7348(5) 0.17673(15) 0.0291(12) Uani 1 1 d . . . H5 H 1.1362 0.7438 0.2019 0.035 Uiso 1 1 calc R . . C6 C 1.0345(3) 0.8138(5) 0.16270(13) 0.0238(11) Uani 1 1 d . . . H6 H 0.9991 0.8742 0.1786 0.029 Uiso 1 1 calc R . . C7 C 0.9584(3) 1.0670(5) 0.08372(12) 0.0177(9) Uani 1 1 d . . . C8 C 1.0220(3) 1.0467(5) 0.05443(13) 0.0230(10) Uani 1 1 d . . . H8 H 1.0344 0.9514 0.0457 0.028 Uiso 1 1 calc R . . C9 C 1.0670(3) 1.1670(6) 0.03817(14) 0.0283(12) Uani 1 1 d . . . H9 H 1.1093 1.1529 0.0184 0.034 Uiso 1 1 calc R . . C10 C 1.0491(4) 1.3081(6) 0.05127(15) 0.0340(13) Uani 1 1 d . . . H10 H 1.0803 1.3892 0.0407 0.041 Uiso 1 1 calc R . . C11 C 0.9853(4) 1.3289(6) 0.07999(15) 0.0322(12) Uani 1 1 d . . . H11 H 0.9725 1.4243 0.0885 0.039 Uiso 1 1 calc R . . C12 C 0.9401(4) 1.2089(5) 0.09639(13) 0.0233(11) Uani 1 1 d . . . H12 H 0.8973 1.2237 0.1159 0.028 Uiso 1 1 calc R . . C13 C 0.8443(3) 0.6426(5) 0.24370(12) 0.0178(9) Uani 1 1 d . . . C14 C 0.8222(4) 0.7533(5) 0.26919(14) 0.0240(11) Uani 1 1 d . . . H14 H 0.7602 0.7974 0.2685 0.029 Uiso 1 1 calc R . . C15 C 0.8938(4) 0.7978(6) 0.29586(14) 0.0292(12) Uani 1 1 d . . . H15 H 0.8797 0.8724 0.3129 0.035 Uiso 1 1 calc R . . C16 C 0.9854(4) 0.7315(5) 0.29696(14) 0.0280(12) Uani 1 1 d . . . H16 H 1.0328 0.7609 0.3149 0.034 Uiso 1 1 calc R . . C17 C 1.0067(4) 0.6227(6) 0.27170(15) 0.0311(12) Uani 1 1 d . . . H17 H 1.0684 0.5776 0.2726 0.037 Uiso 1 1 calc R . . C18 C 0.9368(3) 0.5796(5) 0.24488(14) 0.0256(11) Uani 1 1 d . . . H18 H 0.9523 0.5073 0.2274 0.031 Uiso 1 1 calc R . . C19 C 0.7147(3) 0.3960(5) 0.23240(12) 0.0183(10) Uani 1 1 d . . . C20 C 0.6638(3) 0.4053(5) 0.26573(13) 0.0259(11) Uani 1 1 d . . . H20 H 0.6525 0.4973 0.2766 0.031 Uiso 1 1 calc R . . C21 C 0.6300(4) 0.2767(6) 0.28264(14) 0.0288(12) Uani 1 1 d . . . H21 H 0.5951 0.2822 0.3046 0.035 Uiso 1 1 calc R . . C22 C 0.6489(4) 0.1396(5) 0.26633(14) 0.0270(11) Uani 1 1 d . . . H22 H 0.6259 0.0534 0.2774 0.032 Uiso 1 1 calc R . . C23 C 0.7010(4) 0.1304(5) 0.23421(14) 0.0272(11) Uani 1 1 d . . . H23 H 0.7139 0.0380 0.2238 0.033 Uiso 1 1 calc R . . C24 C 0.7349(4) 0.2587(5) 0.21698(14) 0.0231(10) Uani 1 1 d . . . H24 H 0.7708 0.2521 0.1952 0.028 Uiso 1 1 calc R . . C25 C 0.3307(3) 0.7119(5) 0.04271(12) 0.0181(10) Uani 1 1 d . . . C26 C 0.2427(3) 0.7796(5) 0.03199(14) 0.0254(11) Uani 1 1 d . . . H26 H 0.2275 0.8726 0.0415 0.030 Uiso 1 1 calc R . . C27 C 0.1771(4) 0.7093(6) 0.00708(14) 0.0298(12) Uani 1 1 d . . . H27 H 0.1179 0.7552 0.0001 0.036 Uiso 1 1 calc R . . C28 C 0.1995(3) 0.5714(5) -0.00733(13) 0.0257(11) Uani 1 1 d . . . H28 H 0.1553 0.5246 -0.0240 0.031 Uiso 1 1 calc R . . C29 C 0.2876(4) 0.5031(5) 0.00304(13) 0.0269(11) Uani 1 1 d . . . H29 H 0.3026 0.4101 -0.0066 0.032 Uiso 1 1 calc R . . C30 C 0.3533(4) 0.5731(5) 0.02767(13) 0.0232(10) Uani 1 1 d . . . H30 H 0.4129 0.5276 0.0343 0.028 Uiso 1 1 calc R . . C31 C 0.3565(3) 0.9644(5) 0.09146(12) 0.0167(9) Uani 1 1 d . . . C32 C 0.3667(3) 1.0957(5) 0.07181(14) 0.0271(11) Uani 1 1 d . . . H32 H 0.4059 1.0995 0.0509 0.033 Uiso 1 1 calc R . . C33 C 0.3179(4) 1.2217(5) 0.08366(17) 0.0367(14) Uani 1 1 d . . . H33 H 0.3264 1.3113 0.0712 0.044 Uiso 1 1 calc R . . C34 C 0.2572(4) 1.2145(5) 0.11367(16) 0.0322(13) Uani 1 1 d . . . H34 H 0.2228 1.2987 0.1208 0.039 Uiso 1 1 calc R . . C35 C 0.2466(4) 1.0849(5) 0.13337(14) 0.0275(11) Uani 1 1 d . . . H35 H 0.2059 1.0815 0.1539 0.033 Uiso 1 1 calc R . . C36 C 0.2971(3) 0.9583(5) 0.12240(13) 0.0212(10) Uani 1 1 d . . . H36 H 0.2911 0.8703 0.1358 0.025 Uiso 1 1 calc R . . C37 C 0.5352(3) 1.0937(6) 0.15849(14) 0.0277(11) Uani 1 1 d . . . C38 C 0.4951(4) 1.2311(6) 0.17335(18) 0.0442(16) Uani 1 1 d . . . H38A H 0.5334 1.3136 0.1650 0.066 Uiso 1 1 calc R . . H38B H 0.4977 1.2276 0.2003 0.066 Uiso 1 1 calc R . . H38C H 0.4279 1.2424 0.1645 0.066 Uiso 1 1 calc R . . C39 C 0.6493(4) 0.3656(5) 0.07675(13) 0.0247(11) Uani 1 1 d . . . C40 C 0.6481(5) 0.2139(5) 0.06379(16) 0.0423(15) Uani 1 1 d . . . H40A H 0.7101 0.1677 0.0703 0.063 Uiso 1 1 calc R . . H40B H 0.6374 0.2121 0.0370 0.063 Uiso 1 1 calc R . . H40C H 0.5958 0.1610 0.0755 0.063 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 La1 0.01442(13) 0.01356(13) 0.01430(13) -0.00037(10) 0.00007(10) -0.00065(10) Se1 0.0190(2) 0.0227(3) 0.0219(3) -0.00655(19) 0.0035(2) -0.00398(19) Se2 0.0183(2) 0.0254(3) 0.0166(2) -0.00392(19) 0.00175(19) -0.00727(19) Se3 0.0216(2) 0.0195(2) 0.0154(2) 0.00186(18) 0.00265(19) 0.00450(18) Se4 0.0192(2) 0.0288(3) 0.0190(2) 0.00395(19) 0.0022(2) 0.00737(19) Se5 0.0163(2) 0.0172(2) 0.0176(2) 0.00153(18) 0.00101(18) -0.00028(17) Se6 0.0175(2) 0.0226(2) 0.0161(2) 0.00233(18) 0.00083(18) -0.00229(18) P1 0.0156(6) 0.0158(6) 0.0156(6) -0.0008(4) 0.0027(5) -0.0011(4) P2 0.0159(6) 0.0162(6) 0.0148(6) 0.0008(4) 0.0004(5) 0.0007(4) P3 0.0160(6) 0.0161(6) 0.0150(6) -0.0003(4) -0.0008(5) -0.0003(4) N1 0.017(2) 0.022(2) 0.025(2) -0.0015(17) -0.0049(17) -0.0003(16) N2 0.026(2) 0.024(2) 0.021(2) -0.0045(17) -0.0004(18) 0.0010(17) C1 0.012(2) 0.015(2) 0.026(3) 0.0021(19) -0.0022(19) -0.0034(17) C2 0.022(2) 0.015(2) 0.028(3) 0.0015(19) 0.003(2) -0.0010(18) C3 0.021(2) 0.020(3) 0.039(3) 0.005(2) 0.007(2) 0.0023(19) C4 0.014(2) 0.026(3) 0.046(3) 0.012(2) 0.000(2) 0.000(2) C5 0.025(3) 0.040(3) 0.021(3) 0.009(2) -0.006(2) -0.009(2) C6 0.019(2) 0.026(3) 0.026(3) 0.000(2) -0.001(2) -0.006(2) C7 0.017(2) 0.017(2) 0.019(2) 0.0027(18) -0.0050(19) -0.0019(18) C8 0.021(2) 0.024(3) 0.024(3) 0.006(2) 0.001(2) 0.001(2) C9 0.017(2) 0.044(3) 0.024(3) 0.012(2) 0.001(2) -0.002(2) C10 0.035(3) 0.031(3) 0.036(3) 0.012(2) -0.007(3) -0.013(2) C11 0.041(3) 0.020(3) 0.035(3) 0.003(2) -0.004(3) -0.009(2) C12 0.026(3) 0.025(3) 0.018(2) 0.000(2) 0.000(2) -0.009(2) C13 0.022(2) 0.018(2) 0.014(2) 0.0039(18) -0.0001(19) -0.0030(18) C14 0.026(3) 0.020(2) 0.026(3) -0.004(2) 0.007(2) -0.003(2) C15 0.037(3) 0.027(3) 0.023(3) -0.006(2) 0.000(2) -0.008(2) C16 0.032(3) 0.028(3) 0.023(3) 0.008(2) -0.009(2) -0.014(2) C17 0.024(3) 0.034(3) 0.036(3) 0.003(2) -0.008(2) -0.003(2) C18 0.020(2) 0.027(3) 0.029(3) -0.005(2) -0.002(2) 0.000(2) C19 0.017(2) 0.019(2) 0.018(2) 0.0017(18) -0.0042(19) -0.0027(18) C20 0.029(3) 0.027(3) 0.022(3) -0.002(2) 0.004(2) -0.009(2) C21 0.024(3) 0.043(3) 0.019(3) 0.008(2) 0.002(2) -0.011(2) C22 0.028(3) 0.026(3) 0.027(3) 0.006(2) -0.003(2) -0.010(2) C23 0.032(3) 0.019(3) 0.031(3) 0.001(2) -0.001(2) 0.001(2) C24 0.024(3) 0.024(3) 0.021(3) 0.002(2) -0.002(2) -0.001(2) C25 0.023(2) 0.018(2) 0.014(2) -0.0011(18) 0.0047(19) -0.0049(18) C26 0.018(2) 0.029(3) 0.029(3) -0.012(2) 0.000(2) 0.001(2) C27 0.019(3) 0.042(3) 0.027(3) -0.009(2) -0.008(2) 0.000(2) C28 0.024(3) 0.031(3) 0.022(3) -0.009(2) 0.002(2) -0.011(2) C29 0.043(3) 0.017(2) 0.021(3) -0.001(2) 0.002(2) -0.001(2) C30 0.026(3) 0.023(3) 0.021(3) 0.002(2) -0.002(2) 0.001(2) C31 0.017(2) 0.015(2) 0.018(2) -0.0044(18) -0.0074(19) 0.0015(17) C32 0.025(3) 0.029(3) 0.027(3) 0.006(2) 0.003(2) 0.007(2) C33 0.045(3) 0.017(3) 0.047(4) 0.012(2) -0.001(3) 0.010(2) C34 0.034(3) 0.023(3) 0.038(3) -0.006(2) -0.011(3) 0.014(2) C35 0.029(3) 0.027(3) 0.027(3) -0.007(2) 0.003(2) 0.001(2) C36 0.024(3) 0.019(2) 0.021(2) 0.0007(19) 0.001(2) -0.0015(19) C37 0.019(2) 0.036(3) 0.027(3) -0.004(2) -0.015(2) -0.002(2) C38 0.036(3) 0.039(3) 0.056(4) -0.009(3) -0.013(3) 0.008(3) C39 0.026(3) 0.029(3) 0.020(3) 0.001(2) 0.005(2) -0.005(2) C40 0.067(4) 0.021(3) 0.039(3) -0.001(2) 0.008(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 N2 2.630(4) . ? La1 N1 2.689(4) . ? La1 Se1 3.0689(5) . ? La1 Se4 3.0736(6) . ? La1 Se6 3.0943(5) . ? La1 Se3 3.1021(5) . ? La1 Se5 3.1081(5) . ? La1 Se2 3.1121(5) . ? Se1 P1 2.1492(12) . ? Se2 P1 2.1597(12) . ? Se3 P2 2.1491(12) . ? Se4 P2 2.1576(12) . ? Se5 P3 2.1601(12) . ? Se6 P3 2.1619(12) . ? P1 C1 1.817(5) . ? P1 C7 1.825(4) . ? P2 C19 1.817(4) . ? P2 C13 1.821(4) . ? P3 C25 1.812(5) . ? P3 C31 1.829(4) . ? N1 C37 1.140(6) . ? N2 C39 1.153(6) . ? C1 C6 1.376(6) . ? C1 C2 1.399(6) . ? C2 C3 1.397(6) . ? C3 C4 1.376(7) . ? C4 C5 1.379(7) . ? C5 C6 1.401(7) . ? C7 C12 1.381(6) . ? C7 C8 1.387(6) . ? C8 C9 1.381(6) . ? C9 C10 1.379(7) . ? C10 C11 1.374(7) . ? C11 C12 1.382(6) . ? C13 C18 1.376(6) . ? C13 C14 1.388(6) . ? C14 C15 1.393(7) . ? C15 C16 1.378(7) . ? C16 C17 1.368(7) . ? C17 C18 1.378(6) . ? C19 C24 1.385(6) . ? C19 C20 1.395(6) . ? C20 C21 1.390(6) . ? C21 C22 1.393(7) . ? C22 C23 1.366(7) . ? C23 C24 1.394(6) . ? C25 C26 1.383(6) . ? C25 C30 1.398(6) . ? C26 C27 1.388(6) . ? C27 C28 1.382(7) . ? C28 C29 1.384(7) . ? C29 C30 1.381(6) . ? C31 C32 1.384(6) . ? C31 C36 1.386(6) . ? C32 C33 1.387(7) . ? C33 C34 1.372(8) . ? C34 C35 1.373(7) . ? C35 C36 1.393(6) . ? C37 C38 1.459(7) . ? C39 C40 1.443(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 La1 N1 148.71(11) . . ? N2 La1 Se1 141.45(8) . . ? N1 La1 Se1 68.92(8) . . ? N2 La1 Se4 111.55(9) . . ? N1 La1 Se4 71.50(8) . . ? Se1 La1 Se4 83.740(15) . . ? N2 La1 Se6 80.94(8) . . ? N1 La1 Se6 79.34(8) . . ? Se1 La1 Se6 110.130(15) . . ? Se4 La1 Se6 140.543(15) . . ? N2 La1 Se3 69.81(8) . . ? N1 La1 Se3 135.47(8) . . ? Se1 La1 Se3 83.243(15) . . ? Se4 La1 Se3 71.507(13) . . ? Se6 La1 Se3 144.480(15) . . ? N2 La1 Se5 73.65(8) . . ? N1 La1 Se5 76.99(8) . . ? Se1 La1 Se5 144.801(15) . . ? Se4 La1 Se5 77.301(14) . . ? Se6 La1 Se5 70.565(13) . . ? Se3 La1 Se5 117.360(14) . . ? N2 La1 Se2 77.79(8) . . ? N1 La1 Se2 118.98(8) . . ? Se1 La1 Se2 70.796(14) . . ? Se4 La1 Se2 144.080(15) . . ? Se6 La1 Se2 73.852(14) . . ? Se3 La1 Se2 80.481(14) . . ? Se5 La1 Se2 137.068(15) . . ? P1 Se1 La1 87.39(3) . . ? P1 Se2 La1 86.11(3) . . ? P2 Se3 La1 86.94(3) . . ? P2 Se4 La1 87.52(3) . . ? P3 Se5 La1 86.01(3) . . ? P3 Se6 La1 86.33(3) . . ? C1 P1 C7 104.3(2) . . ? C1 P1 Se1 110.67(16) . . ? C7 P1 Se1 109.45(15) . . ? C1 P1 Se2 109.94(15) . . ? C7 P1 Se2 109.79(15) . . ? Se1 P1 Se2 112.39(5) . . ? C19 P2 C13 103.32(19) . . ? C19 P2 Se3 110.85(15) . . ? C13 P2 Se3 110.30(15) . . ? C19 P2 Se4 106.92(15) . . ? C13 P2 Se4 111.06(15) . . ? Se3 P2 Se4 113.83(5) . . ? C25 P3 C31 104.3(2) . . ? C25 P3 Se5 108.59(15) . . ? C31 P3 Se5 110.48(15) . . ? C25 P3 Se6 109.59(15) . . ? C31 P3 Se6 111.59(15) . . ? Se5 P3 Se6 111.98(5) . . ? C37 N1 La1 173.9(4) . . ? C39 N2 La1 171.1(4) . . ? C6 C1 C2 120.0(4) . . ? C6 C1 P1 121.0(4) . . ? C2 C1 P1 119.0(4) . . ? C3 C2 C1 119.5(5) . . ? C4 C3 C2 120.4(5) . . ? C3 C4 C5 119.8(5) . . ? C4 C5 C6 120.5(5) . . ? C1 C6 C5 119.7(5) . . ? C12 C7 C8 119.4(4) . . ? C12 C7 P1 120.7(4) . . ? C8 C7 P1 119.9(3) . . ? C9 C8 C7 120.4(5) . . ? C10 C9 C8 119.8(5) . . ? C11 C10 C9 119.9(5) . . ? C10 C11 C12 120.5(5) . . ? C7 C12 C11 119.9(5) . . ? C18 C13 C14 119.6(4) . . ? C18 C13 P2 118.4(3) . . ? C14 C13 P2 122.0(4) . . ? C13 C14 C15 119.4(5) . . ? C16 C15 C14 120.1(5) . . ? C17 C16 C15 120.2(5) . . ? C16 C17 C18 120.1(5) . . ? C13 C18 C17 120.7(5) . . ? C24 C19 C20 120.0(4) . . ? C24 C19 P2 122.2(4) . . ? C20 C19 P2 117.8(3) . . ? C21 C20 C19 119.9(5) . . ? C20 C21 C22 119.4(5) . . ? C23 C22 C21 120.7(4) . . ? C22 C23 C24 120.3(5) . . ? C19 C24 C23 119.6(5) . . ? C26 C25 C30 119.2(4) . . ? C26 C25 P3 122.4(3) . . ? C30 C25 P3 118.4(4) . . ? C25 C26 C27 120.2(4) . . ? C28 C27 C26 120.2(5) . . ? C27 C28 C29 120.0(4) . . ? C30 C29 C28 119.9(4) . . ? C29 C30 C25 120.4(4) . . ? C32 C31 C36 120.4(4) . . ? C32 C31 P3 120.5(4) . . ? C36 C31 P3 119.1(3) . . ? C31 C32 C33 119.3(5) . . ? C34 C33 C32 120.2(5) . . ? C33 C34 C35 120.9(5) . . ? C34 C35 C36 119.5(5) . . ? C31 C36 C35 119.6(4) . . ? N1 C37 C38 178.6(6) . . ? N2 C39 C40 179.0(6) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.832 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.157 data_xpl204a _database_code_depnum_ccdc_archive 'CCDC 906770' #TrackingRef 'web_deposit_cif_file_4_AndrewGaunt_1350598115.cif for 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H46 N0 O2 P3 Pu Se6' _chemical_formula_weight 1412.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pu Pu -9.4100 4.3056 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.344(4) _cell_length_b 18.862(5) _cell_length_c 20.428(5) _cell_angle_alpha 79.465(4) _cell_angle_beta 89.356(4) _cell_angle_gamma 70.120(3) _cell_volume 4747(2) _cell_formula_units_Z 4 _cell_measurement_temperature 141(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2676 _exptl_absorpt_coefficient_mu 6.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4407 _exptl_absorpt_correction_T_max 0.4809 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 141(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 SMART 1k CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 55569 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.1488 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.98 _reflns_number_total 22561 _reflns_number_gt 13211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 4.210 (Bruker, 1996)' _computing_cell_refinement 'SAINT 4.05 (Bruker, 1996)' _computing_data_reduction 'SAINT 4.05 (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.10 (Bruker, 2001)' _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. Four thf carbon atom positions and two phenyl ring carbon atom positions were restrained to approximate isotropic behaviour in order to force convergence. A small twin in the crystal is probably responsible for the bad ellipsoids on these carbon atoms. ; _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^)+(0.0958P)^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 22561 _refine_ls_number_parameters 1009 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.1816 _refine_ls_wR_factor_gt 0.1556 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pu1 Pu 0.72289(3) 0.72148(2) 0.30442(2) 0.01808(11) Uani 1 1 d . . . Pu2 Pu 0.62158(3) 0.25262(2) 0.231708(19) 0.01836(11) Uani 1 1 d . . . Se1 Se 0.49123(10) 0.83858(7) 0.27720(6) 0.0291(3) Uani 1 1 d . . . Se2 Se 0.62638(9) 0.70057(7) 0.17857(6) 0.0240(3) Uani 1 1 d . . . Se3 Se 0.81539(10) 0.54589(7) 0.32259(6) 0.0283(3) Uani 1 1 d . . . Se4 Se 0.91869(10) 0.67593(7) 0.21804(6) 0.0268(3) Uani 1 1 d . . . Se5 Se 0.89932(9) 0.67233(6) 0.41531(6) 0.0246(3) Uani 1 1 d . . . Se6 Se 0.66287(9) 0.83304(7) 0.40049(6) 0.0272(3) Uani 1 1 d . . . Se7 Se 0.37569(9) 0.32401(7) 0.21863(5) 0.0235(3) Uani 1 1 d . . . Se8 Se 0.54597(9) 0.28898(7) 0.08396(6) 0.0267(3) Uani 1 1 d . . . Se9 Se 0.75780(10) 0.09942(7) 0.19441(6) 0.0278(3) Uani 1 1 d . . . Se10 Se 0.81493(10) 0.27399(6) 0.15441(6) 0.0247(3) Uani 1 1 d . . . Se11 Se 0.80494(9) 0.20438(7) 0.33760(6) 0.0246(3) Uani 1 1 d . . . Se12 Se 0.53415(9) 0.29388(7) 0.36792(6) 0.0289(3) Uani 1 1 d . . . P1 P 0.4789(2) 0.79107(17) 0.19041(15) 0.0219(6) Uani 1 1 d . . . P2 P 0.9434(2) 0.55718(17) 0.26085(14) 0.0219(6) Uani 1 1 d . . . P3 P 0.8244(2) 0.78215(17) 0.44482(14) 0.0210(6) Uani 1 1 d . . . P4 P 0.3826(2) 0.33531(17) 0.11145(14) 0.0210(6) Uani 1 1 d . . . P5 P 0.8641(2) 0.15468(16) 0.14695(14) 0.0213(6) Uani 1 1 d . . . P6 P 0.6934(2) 0.23432(18) 0.41416(15) 0.0241(7) Uani 1 1 d . . . O1 O 0.7519(6) 0.8367(4) 0.2347(4) 0.0276(19) Uani 1 1 d . . . O2 O 0.6141(6) 0.6562(5) 0.3765(4) 0.0292(19) Uani 1 1 d . . . O3 O 0.6074(6) 0.3883(4) 0.2186(4) 0.0286(19) Uani 1 1 d . . . O4 O 0.5540(7) 0.1442(5) 0.2698(5) 0.038(2) Uani 1 1 d . . . C1 C 0.3691(10) 0.7544(7) 0.1957(6) 0.030(3) Uani 1 1 d . . . C2 C 0.3640(11) 0.7059(8) 0.1528(7) 0.039(3) Uani 1 1 d . . . H2 H 0.4145 0.6942 0.1211 0.047 Uiso 1 1 calc R . . C3 C 0.2814(12) 0.6751(8) 0.1581(9) 0.062(5) Uani 1 1 d . . . H3 H 0.2792 0.6410 0.1309 0.074 Uiso 1 1 calc R . . C4 C 0.2003(12) 0.6954(9) 0.2049(9) 0.055(5) Uani 1 1 d . . . H4 H 0.1446 0.6761 0.2080 0.066 Uiso 1 1 calc R . . C5 C 0.2080(11) 0.7430(10) 0.2436(7) 0.053(4) Uani 1 1 d . . . H5 H 0.1567 0.7556 0.2747 0.063 Uiso 1 1 calc R . . C6 C 0.2910(10) 0.7763(8) 0.2404(6) 0.036(3) Uani 1 1 d . . . H6 H 0.2919 0.8110 0.2672 0.044 Uiso 1 1 calc R . . C7 C 0.4473(9) 0.8654(7) 0.1142(5) 0.026(3) Uani 1 1 d . . . C8 C 0.4040(10) 0.9429(7) 0.1189(7) 0.036(3) Uani 1 1 d . . . H8 H 0.3925 0.9579 0.1601 0.044 Uiso 1 1 calc R . . C9 C 0.3782(11) 0.9979(7) 0.0588(8) 0.051(4) Uani 1 1 d . . . H9 H 0.3522 1.0499 0.0605 0.061 Uiso 1 1 calc R . . C10 C 0.3908(11) 0.9760(9) -0.0013(7) 0.043(3) Uani 1 1 d U . . H10 H 0.3709 1.0131 -0.0401 0.051 Uiso 1 1 calc R . . C11 C 0.4309(11) 0.9024(9) -0.0054(6) 0.047(4) Uani 1 1 d . . . H11 H 0.4406 0.8882 -0.0469 0.056 Uiso 1 1 calc R . . C12 C 0.4589(11) 0.8458(8) 0.0533(6) 0.040(3) Uani 1 1 d . . . H12 H 0.4858 0.7943 0.0501 0.048 Uiso 1 1 calc R . . C13 C 0.9568(9) 0.5025(6) 0.1960(6) 0.025(3) Uani 1 1 d . . . C14 C 0.9998(10) 0.4225(7) 0.2103(6) 0.031(3) Uani 1 1 d . . . H14 H 1.0232 0.3981 0.2540 0.038 Uiso 1 1 calc R . . C15 C 1.0092(10) 0.3776(8) 0.1621(7) 0.035(3) Uani 1 1 d . . . H15 H 1.0393 0.3244 0.1733 0.042 Uiso 1 1 calc R . . C16 C 0.9728(11) 0.4136(8) 0.0972(7) 0.040(3) Uani 1 1 d . . . H16 H 0.9794 0.3847 0.0641 0.048 Uiso 1 1 calc R . . C17 C 0.9263(11) 0.4931(8) 0.0817(6) 0.040(3) Uani 1 1 d . . . H17 H 0.9006 0.5166 0.0381 0.048 Uiso 1 1 calc R . . C18 C 0.9170(9) 0.5391(7) 0.1299(6) 0.030(3) Uani 1 1 d . . . H18 H 0.8855 0.5922 0.1187 0.036 Uiso 1 1 calc R . . C19 C 1.0697(8) 0.5119(6) 0.3101(6) 0.022(2) Uani 1 1 d . . . C20 C 1.1615(10) 0.5160(7) 0.2789(6) 0.034(3) Uani 1 1 d . . . H20 H 1.1564 0.5418 0.2350 0.041 Uiso 1 1 calc R . . C21 C 1.2620(11) 0.4813(8) 0.3135(7) 0.046(4) Uani 1 1 d . . . H21 H 1.3238 0.4851 0.2942 0.055 Uiso 1 1 calc R . . C22 C 1.2641(11) 0.4403(8) 0.3795(8) 0.045(4) Uani 1 1 d . . . H22 H 1.3298 0.4142 0.4026 0.054 Uiso 1 1 calc R . . C23 C 1.1765(12) 0.4377(8) 0.4094(7) 0.046(4) Uani 1 1 d . . . H23 H 1.1811 0.4123 0.4534 0.055 Uiso 1 1 calc R . . C24 C 1.0770(11) 0.4730(8) 0.3747(6) 0.037(3) Uani 1 1 d . . . H24 H 1.0157 0.4701 0.3953 0.044 Uiso 1 1 calc R . . C25 C 0.8246(10) 0.7723(6) 0.5349(5) 0.026(3) Uani 1 1 d . . . C26 C 0.7350(10) 0.7728(7) 0.5688(5) 0.028(3) Uani 1 1 d . . . H26 H 0.6723 0.7803 0.5448 0.033 Uiso 1 1 calc R . . C27 C 0.7351(11) 0.7627(8) 0.6368(7) 0.040(3) Uani 1 1 d . . . H27 H 0.6733 0.7636 0.6586 0.048 Uiso 1 1 calc R . . C28 C 0.8286(10) 0.7511(7) 0.6725(6) 0.033(3) Uani 1 1 d . . . H28 H 0.8298 0.7433 0.7188 0.039 Uiso 1 1 calc R . . C29 C 0.9195(11) 0.7508(8) 0.6405(7) 0.044(4) Uani 1 1 d . . . H29 H 0.9816 0.7441 0.6649 0.053 Uiso 1 1 calc R . . C30 C 0.9185(10) 0.7608(7) 0.5718(6) 0.028(3) Uani 1 1 d . . . H30 H 0.9804 0.7598 0.5499 0.034 Uiso 1 1 calc R . . C31 C 0.8983(9) 0.8472(6) 0.4168(5) 0.021(2) Uani 1 1 d . . . C32 C 1.0037(10) 0.8186(7) 0.4018(6) 0.029(3) Uani 1 1 d . . . H32 H 1.0401 0.7659 0.4101 0.035 Uiso 1 1 calc R . . C33 C 1.0556(11) 0.8688(8) 0.3743(6) 0.037(3) Uani 1 1 d . . . H33 H 1.1269 0.8495 0.3644 0.044 Uiso 1 1 calc R . . C34 C 1.0016(11) 0.9478(7) 0.3615(6) 0.038(3) Uani 1 1 d . . . H34 H 1.0356 0.9813 0.3418 0.046 Uiso 1 1 calc R . . C35 C 0.8977(11) 0.9754(7) 0.3784(6) 0.038(3) Uani 1 1 d . . . H35 H 0.8617 1.0281 0.3715 0.045 Uiso 1 1 calc R . . C36 C 0.8450(11) 0.9247(7) 0.4061(6) 0.035(3) Uani 1 1 d . . . H36 H 0.7742 0.9437 0.4171 0.042 Uiso 1 1 calc R . . C37 C 0.8358(10) 0.8626(8) 0.2547(7) 0.037(3) Uani 1 1 d . . . H37A H 0.8858 0.8227 0.2873 0.044 Uiso 1 1 calc R . . H37B H 0.8057 0.9080 0.2742 0.044 Uiso 1 1 calc R . . C38 C 0.8913(10) 0.8806(7) 0.1919(6) 0.032(3) Uani 1 1 d . . . H38A H 0.9516 0.8364 0.1855 0.038 Uiso 1 1 calc R . . H38B H 0.9153 0.9236 0.1928 0.038 Uiso 1 1 calc R . . C39 C 0.8022(12) 0.9009(11) 0.1383(7) 0.063(5) Uani 1 1 d . . . H39A H 0.7751 0.9559 0.1220 0.075 Uiso 1 1 calc R . . H39B H 0.8296 0.8759 0.1011 0.075 Uiso 1 1 calc R . . C40 C 0.7157(13) 0.8753(9) 0.1669(7) 0.057(5) Uani 1 1 d . . . H40A H 0.6507 0.9189 0.1662 0.068 Uiso 1 1 calc R . . H40B H 0.7019 0.8404 0.1417 0.068 Uiso 1 1 calc R . . C41 C 0.5388(12) 0.6267(8) 0.3511(7) 0.043(4) Uani 1 1 d . . . H41A H 0.5567 0.6151 0.3073 0.051 Uiso 1 1 calc R . . H41B H 0.4669 0.6637 0.3483 0.051 Uiso 1 1 calc R . . C42 C 0.5479(12) 0.5550(7) 0.4007(6) 0.038(3) Uani 1 1 d . . . H42A H 0.6054 0.5110 0.3909 0.045 Uiso 1 1 calc R . . H42B H 0.4817 0.5442 0.4016 0.045 Uiso 1 1 calc R . . C43 C 0.5726(10) 0.5760(7) 0.4673(6) 0.038(3) Uani 1 1 d . . . H43A H 0.5074 0.6003 0.4882 0.045 Uiso 1 1 calc R . . H43B H 0.6168 0.5309 0.4981 0.045 Uiso 1 1 calc R . . C44 C 0.6297(15) 0.6295(10) 0.4466(7) 0.063(5) Uani 1 1 d U . . H44A H 0.6035 0.6727 0.4693 0.076 Uiso 1 1 calc R . . H44B H 0.7052 0.6040 0.4586 0.076 Uiso 1 1 calc R . . C45 C 0.3177(9) 0.4372(6) 0.0733(5) 0.021(2) Uani 1 1 d . . . C46 C 0.2202(10) 0.4771(7) 0.0957(5) 0.027(3) Uani 1 1 d . . . H46 H 0.1870 0.4531 0.1284 0.032 Uiso 1 1 calc R . . C47 C 0.1725(11) 0.5566(7) 0.0667(6) 0.034(3) Uani 1 1 d . . . H47 H 0.1067 0.5849 0.0804 0.041 Uiso 1 1 calc R . . C48 C 0.2222(11) 0.5923(7) 0.0185(6) 0.034(3) Uani 1 1 d . . . H48 H 0.1910 0.6444 0.0010 0.041 Uiso 1 1 calc R . . C49 C 0.3175(12) 0.5506(8) -0.0032(6) 0.040(3) Uani 1 1 d . . . H49 H 0.3496 0.5744 -0.0367 0.049 Uiso 1 1 calc R . . C50 C 0.3669(10) 0.4740(7) 0.0237(6) 0.032(3) Uani 1 1 d . . . H50 H 0.4325 0.4467 0.0092 0.038 Uiso 1 1 calc R . . C51 C 0.3025(9) 0.2869(6) 0.0772(5) 0.022(2) Uani 1 1 d . . . C52 C 0.2898(10) 0.2942(7) 0.0096(6) 0.032(3) Uani 1 1 d . . . H52 H 0.3199 0.3249 -0.0188 0.038 Uiso 1 1 calc R . . C53 C 0.2327(11) 0.2563(8) -0.0164(6) 0.041(3) Uani 1 1 d . . . H53 H 0.2239 0.2622 -0.0624 0.049 Uiso 1 1 calc R . . C54 C 0.1886(11) 0.2101(8) 0.0244(7) 0.042(3) Uani 1 1 d . . . H54 H 0.1532 0.1828 0.0062 0.050 Uiso 1 1 calc R . . C55 C 0.1968(11) 0.2043(8) 0.0903(7) 0.038(3) Uani 1 1 d . . . H55 H 0.1645 0.1745 0.1179 0.045 Uiso 1 1 calc R . . C56 C 0.2537(10) 0.2426(7) 0.1181(6) 0.031(3) Uani 1 1 d . . . H56 H 0.2587 0.2385 0.1641 0.037 Uiso 1 1 calc R . . C57 C 0.9297(10) 0.1861(7) 0.0177(6) 0.032(3) Uani 1 1 d . . . H57 H 0.9603 0.2168 0.0349 0.038 Uiso 1 1 calc R . . C58 C 0.9381(10) 0.1811(8) -0.0491(6) 0.038(3) Uani 1 1 d . . . H58 H 0.9743 0.2080 -0.0767 0.045 Uiso 1 1 calc R . . C59 C 0.8925(11) 0.1362(8) -0.0737(7) 0.040(3) Uani 1 1 d . . . H59 H 0.8980 0.1327 -0.1185 0.048 Uiso 1 1 calc R . . C60 C 0.8387(11) 0.0960(8) -0.0342(6) 0.038(3) Uani 1 1 d . . . H60 H 0.8073 0.0663 -0.0524 0.046 Uiso 1 1 calc R . . C61 C 0.8312(10) 0.0995(7) 0.0315(6) 0.033(3) Uani 1 1 d . . . H61 H 0.7962 0.0711 0.0585 0.040 Uiso 1 1 calc R . . C62 C 0.8761(10) 0.1459(7) 0.0594(6) 0.027(3) Uani 1 1 d . . . C63 C 0.9982(9) 0.1031(6) 0.1845(5) 0.024(3) Uani 1 1 d . . . C64 C 1.0585(10) 0.0324(7) 0.1663(6) 0.034(3) Uani 1 1 d . . . H64 H 1.0310 0.0152 0.1331 0.040 Uiso 1 1 calc R . . C65 C 1.1573(9) -0.0113(7) 0.1970(7) 0.035(3) Uani 1 1 d . . . H65 H 1.1961 -0.0574 0.1843 0.042 Uiso 1 1 calc R . . C66 C 1.1993(10) 0.0136(7) 0.2470(7) 0.037(3) Uani 1 1 d . . . H66 H 1.2657 -0.0158 0.2681 0.044 Uiso 1 1 calc R . . C67 C 1.1405(9) 0.0828(6) 0.2648(6) 0.025(3) Uani 1 1 d . . . H67 H 1.1684 0.0996 0.2980 0.030 Uiso 1 1 calc R . . C68 C 1.0409(9) 0.1277(7) 0.2343(6) 0.027(3) Uani 1 1 d . . . H68 H 1.0029 0.1739 0.2471 0.033 Uiso 1 1 calc R . . C69 C 0.7313(8) 0.2903(7) 0.4649(6) 0.025(3) Uani 1 1 d . . . C70 C 0.7866(10) 0.3405(7) 0.4374(6) 0.033(3) Uani 1 1 d . . . H70 H 0.8035 0.3441 0.3929 0.039 Uiso 1 1 calc R . . C71 C 0.8152(11) 0.3840(7) 0.4767(7) 0.040(3) Uani 1 1 d . . . H71 H 0.8520 0.4163 0.4585 0.048 Uiso 1 1 calc R . . C72 C 0.7898(10) 0.3799(7) 0.5419(7) 0.037(3) Uani 1 1 d . . . H72 H 0.8097 0.4091 0.5679 0.045 Uiso 1 1 calc R . . C73 C 0.7343(10) 0.3323(8) 0.5697(6) 0.039(3) Uani 1 1 d . . . H73 H 0.7166 0.3302 0.6140 0.047 Uiso 1 1 calc R . . C74 C 0.7056(9) 0.2883(7) 0.5320(6) 0.030(3) Uani 1 1 d . . . H74 H 0.6685 0.2567 0.5511 0.037 Uiso 1 1 calc R . . C75 C 0.6984(9) 0.1474(7) 0.4730(6) 0.026(3) Uani 1 1 d . . . C76 C 0.7985(10) 0.0929(7) 0.4945(6) 0.034(3) Uani 1 1 d . . . H76 H 0.8604 0.1015 0.4801 0.040 Uiso 1 1 calc R . . C77 C 0.8043(11) 0.0237(8) 0.5388(6) 0.040(3) Uani 1 1 d . . . H77 H 0.8703 -0.0128 0.5543 0.048 Uiso 1 1 calc R . . C78 C 0.7122(11) 0.0113(8) 0.5585(6) 0.038(3) Uani 1 1 d U . . H78 H 0.7166 -0.0349 0.5860 0.046 Uiso 1 1 calc R . . C79 C 0.6144(13) 0.0652(10) 0.5388(8) 0.070(6) Uani 1 1 d . . . H79 H 0.5528 0.0566 0.5540 0.084 Uiso 1 1 calc R . . C80 C 0.6075(12) 0.1361(9) 0.4938(7) 0.052(4) Uani 1 1 d . . . H80 H 0.5414 0.1732 0.4795 0.062 Uiso 1 1 calc R . . C81 C 0.6879(10) 0.4165(8) 0.2432(6) 0.036(3) Uani 1 1 d . . . H81A H 0.7574 0.3763 0.2510 0.043 Uiso 1 1 calc R . . H81B H 0.6672 0.4354 0.2842 0.043 Uiso 1 1 calc R . . C82 C 0.6884(11) 0.4808(8) 0.1868(7) 0.045(4) Uani 1 1 d . . . H82A H 0.7179 0.5157 0.2022 0.054 Uiso 1 1 calc R . . H82B H 0.7290 0.4608 0.1505 0.054 Uiso 1 1 calc R . . C83 C 0.5728(11) 0.5197(8) 0.1660(7) 0.042(4) Uani 1 1 d . . . H83A H 0.5634 0.5455 0.1196 0.051 Uiso 1 1 calc R . . H83B H 0.5380 0.5569 0.1935 0.051 Uiso 1 1 calc R . . C84 C 0.5285(11) 0.4542(8) 0.1760(7) 0.042(3) Uani 1 1 d U . . H84A H 0.4610 0.4687 0.1972 0.050 Uiso 1 1 calc R . . H84B H 0.5171 0.4415 0.1335 0.050 Uiso 1 1 calc R . . C85 C 0.5895(14) 0.0866(10) 0.3315(8) 0.064(5) Uani 1 1 d . . . H85A H 0.5977 0.1108 0.3681 0.077 Uiso 1 1 calc R . . H85B H 0.6576 0.0482 0.3261 0.077 Uiso 1 1 calc R . . C86 C 0.5085(16) 0.0512(9) 0.3449(10) 0.085(7) Uani 1 1 d U . . H86A H 0.5404 -0.0030 0.3640 0.102 Uiso 1 1 calc R . . H86B H 0.4577 0.0762 0.3750 0.102 Uiso 1 1 calc R . . C87 C 0.455(2) 0.0630(15) 0.2760(16) 0.139(11) Uani 1 1 d U . . H87A H 0.4716 0.0143 0.2615 0.167 Uiso 1 1 calc R . . H87B H 0.3779 0.0856 0.2773 0.167 Uiso 1 1 calc R . . C88 C 0.4963(12) 0.1145(9) 0.2307(8) 0.056(4) Uani 1 1 d . . . H88A H 0.5429 0.0867 0.2001 0.068 Uiso 1 1 calc R . . H88B H 0.4380 0.1561 0.2049 0.068 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 Pu1 0.0186(2) 0.0158(2) 0.0176(2) 0.00084(16) -0.00205(16) -0.00507(17) Pu2 0.0225(2) 0.0133(2) 0.0174(2) 0.00358(15) -0.00135(16) -0.00702(17) Se1 0.0254(7) 0.0268(7) 0.0299(7) -0.0089(5) -0.0058(5) -0.0004(5) Se2 0.0226(6) 0.0218(6) 0.0238(6) -0.0032(5) -0.0036(5) -0.0032(5) Se3 0.0297(7) 0.0210(6) 0.0314(7) -0.0012(5) 0.0036(5) -0.0073(5) Se4 0.0265(7) 0.0173(6) 0.0318(7) 0.0016(5) 0.0010(5) -0.0047(5) Se5 0.0274(7) 0.0182(6) 0.0250(6) -0.0030(5) -0.0057(5) -0.0041(5) Se6 0.0219(6) 0.0265(7) 0.0283(6) -0.0063(5) -0.0048(5) -0.0013(5) Se7 0.0266(6) 0.0251(6) 0.0176(6) 0.0026(5) 0.0002(5) -0.0110(5) Se8 0.0233(6) 0.0324(7) 0.0205(6) 0.0011(5) 0.0013(5) -0.0077(5) Se9 0.0318(7) 0.0180(6) 0.0335(7) -0.0008(5) 0.0056(5) -0.0107(5) Se10 0.0283(7) 0.0156(6) 0.0275(6) 0.0014(5) 0.0034(5) -0.0070(5) Se11 0.0229(6) 0.0259(6) 0.0206(6) -0.0004(5) 0.0013(5) -0.0048(5) Se12 0.0206(6) 0.0344(7) 0.0245(6) -0.0007(5) -0.0014(5) -0.0028(5) P1 0.0194(16) 0.0208(15) 0.0220(15) 0.0000(12) -0.0029(12) -0.0042(12) P2 0.0232(16) 0.0188(15) 0.0217(15) -0.0005(12) -0.0008(12) -0.0062(13) P3 0.0217(16) 0.0190(15) 0.0206(15) -0.0012(12) -0.0005(12) -0.0062(12) P4 0.0226(16) 0.0198(15) 0.0187(15) 0.0041(12) -0.0029(12) -0.0086(13) P5 0.0239(16) 0.0153(15) 0.0229(15) 0.0013(12) 0.0004(12) -0.0068(12) P6 0.0197(16) 0.0265(17) 0.0207(15) -0.0010(12) 0.0003(12) -0.0026(13) O1 0.034(5) 0.024(4) 0.026(4) 0.001(3) 0.000(4) -0.014(4) O2 0.030(5) 0.027(5) 0.027(4) 0.005(4) 0.005(4) -0.011(4) O3 0.030(5) 0.015(4) 0.039(5) 0.002(4) -0.008(4) -0.008(4) O4 0.030(5) 0.027(5) 0.057(6) 0.008(4) 0.002(4) -0.015(4) C1 0.028(7) 0.026(7) 0.031(7) 0.001(5) -0.006(5) -0.006(5) C2 0.039(8) 0.034(8) 0.048(9) 0.000(6) -0.004(6) -0.019(6) C3 0.043(10) 0.032(8) 0.113(15) -0.014(9) -0.038(10) -0.014(7) C4 0.031(9) 0.050(10) 0.081(12) 0.011(9) -0.014(8) -0.021(8) C5 0.031(8) 0.075(12) 0.043(9) 0.023(8) -0.003(7) -0.024(8) C6 0.029(7) 0.048(9) 0.033(7) 0.002(6) -0.005(6) -0.019(6) C7 0.020(6) 0.035(7) 0.018(6) 0.005(5) -0.004(5) -0.009(5) C8 0.033(8) 0.031(7) 0.039(8) 0.001(6) 0.009(6) -0.008(6) C9 0.033(8) 0.014(7) 0.090(12) 0.022(7) 0.004(8) -0.003(6) C10 0.041(4) 0.042(4) 0.042(4) -0.001(3) 0.001(3) -0.015(3) C11 0.050(9) 0.076(12) 0.017(6) 0.010(7) -0.002(6) -0.034(9) C12 0.041(8) 0.042(8) 0.033(8) 0.012(6) -0.012(6) -0.019(7) C13 0.031(7) 0.021(6) 0.026(6) -0.009(5) -0.001(5) -0.012(5) C14 0.042(8) 0.019(6) 0.033(7) -0.002(5) -0.008(6) -0.011(6) C15 0.025(7) 0.039(8) 0.047(8) -0.024(7) -0.003(6) -0.010(6) C16 0.047(9) 0.038(8) 0.041(8) -0.008(6) -0.012(7) -0.023(7) C17 0.048(9) 0.059(10) 0.015(6) -0.012(6) -0.004(6) -0.020(7) C18 0.026(7) 0.029(7) 0.031(7) -0.005(5) 0.000(5) -0.003(5) C19 0.014(6) 0.023(6) 0.026(6) -0.009(5) 0.000(5) -0.002(5) C20 0.032(7) 0.037(8) 0.032(7) -0.012(6) 0.002(6) -0.006(6) C21 0.024(7) 0.055(10) 0.049(9) -0.025(8) 0.004(6) 0.007(7) C22 0.033(8) 0.029(8) 0.062(10) -0.016(7) -0.026(7) 0.008(6) C23 0.057(10) 0.039(9) 0.034(8) 0.000(6) -0.013(7) -0.009(8) C24 0.039(8) 0.046(8) 0.031(7) -0.002(6) -0.002(6) -0.024(7) C25 0.039(7) 0.016(6) 0.021(6) -0.002(5) -0.005(5) -0.008(5) C26 0.028(7) 0.039(7) 0.019(6) 0.000(5) 0.000(5) -0.018(6) C27 0.036(8) 0.036(8) 0.044(8) 0.001(6) 0.013(6) -0.012(6) C28 0.041(8) 0.029(7) 0.022(6) 0.001(5) -0.002(6) -0.009(6) C29 0.040(9) 0.053(9) 0.036(8) -0.004(7) -0.012(7) -0.016(7) C30 0.026(7) 0.031(7) 0.025(6) -0.003(5) 0.002(5) -0.007(5) C31 0.028(7) 0.015(6) 0.019(6) -0.002(4) -0.004(5) -0.008(5) C32 0.029(7) 0.018(6) 0.041(7) 0.006(5) -0.002(6) -0.012(5) C33 0.029(7) 0.043(8) 0.038(8) 0.003(6) 0.003(6) -0.015(6) C34 0.057(10) 0.032(8) 0.030(7) 0.015(6) 0.003(6) -0.032(7) C35 0.055(10) 0.015(6) 0.037(8) 0.005(5) -0.003(7) -0.009(6) C36 0.047(9) 0.019(7) 0.039(8) -0.001(5) 0.006(6) -0.013(6) C37 0.037(8) 0.035(8) 0.040(8) -0.006(6) -0.001(6) -0.015(6) C38 0.035(8) 0.023(7) 0.034(7) -0.001(5) -0.004(6) -0.008(6) C39 0.050(10) 0.113(15) 0.031(8) 0.019(9) -0.009(7) -0.052(10) C40 0.060(11) 0.049(10) 0.046(9) 0.031(7) -0.005(8) -0.019(8) C41 0.045(9) 0.055(10) 0.032(7) -0.003(7) 0.007(6) -0.026(8) C42 0.051(9) 0.029(7) 0.034(7) 0.005(6) -0.003(6) -0.022(7) C43 0.026(7) 0.030(7) 0.043(8) 0.009(6) 0.000(6) 0.001(6) C44 0.108(14) 0.076(12) 0.028(8) 0.012(8) 0.002(8) -0.072(11) C45 0.035(7) 0.018(6) 0.010(5) 0.007(4) -0.009(5) -0.013(5) C46 0.038(8) 0.024(6) 0.018(6) 0.005(5) -0.006(5) -0.015(6) C47 0.037(8) 0.025(7) 0.040(8) -0.003(6) -0.007(6) -0.011(6) C48 0.039(8) 0.020(7) 0.040(8) 0.006(6) -0.003(6) -0.011(6) C49 0.052(9) 0.043(9) 0.027(7) 0.008(6) -0.002(6) -0.025(7) C50 0.033(7) 0.032(7) 0.029(7) -0.001(5) 0.006(5) -0.013(6) C51 0.024(6) 0.017(6) 0.027(6) 0.003(5) -0.001(5) -0.011(5) C52 0.039(8) 0.038(8) 0.027(7) -0.006(6) -0.001(6) -0.023(6) C53 0.051(9) 0.052(9) 0.025(7) -0.013(6) -0.007(6) -0.020(7) C54 0.039(8) 0.044(9) 0.047(9) -0.016(7) -0.002(7) -0.016(7) C55 0.043(8) 0.041(8) 0.041(8) -0.004(6) 0.011(6) -0.032(7) C56 0.032(7) 0.033(7) 0.029(7) -0.004(5) 0.003(5) -0.015(6) C57 0.038(8) 0.030(7) 0.029(7) -0.004(5) 0.004(6) -0.013(6) C58 0.026(7) 0.059(9) 0.027(7) -0.007(6) -0.002(5) -0.015(7) C59 0.045(9) 0.046(9) 0.031(7) -0.009(6) -0.015(6) -0.015(7) C60 0.046(9) 0.046(9) 0.037(8) -0.017(7) 0.001(6) -0.028(7) C61 0.039(8) 0.034(7) 0.033(7) 0.002(6) -0.002(6) -0.023(6) C62 0.030(7) 0.023(6) 0.024(6) -0.002(5) -0.006(5) -0.005(5) C63 0.027(7) 0.021(6) 0.018(6) 0.003(5) 0.007(5) -0.005(5) C64 0.043(8) 0.028(7) 0.033(7) -0.013(6) 0.013(6) -0.013(6) C65 0.015(6) 0.029(7) 0.054(9) -0.011(6) -0.007(6) 0.004(5) C66 0.023(7) 0.018(6) 0.059(9) -0.008(6) -0.009(6) 0.007(5) C67 0.026(7) 0.020(6) 0.025(6) -0.001(5) -0.003(5) -0.005(5) C68 0.028(7) 0.023(6) 0.028(7) 0.001(5) -0.009(5) -0.008(5) C69 0.009(5) 0.029(7) 0.033(7) -0.002(5) -0.004(5) -0.005(5) C70 0.043(8) 0.027(7) 0.033(7) -0.002(5) -0.005(6) -0.018(6) C71 0.050(9) 0.025(7) 0.039(8) 0.002(6) -0.007(7) -0.010(6) C72 0.038(8) 0.029(7) 0.038(8) -0.011(6) -0.017(6) -0.001(6) C73 0.035(8) 0.047(9) 0.027(7) -0.005(6) 0.004(6) -0.005(7) C74 0.026(7) 0.039(8) 0.019(6) -0.003(5) 0.001(5) -0.002(6) C75 0.020(6) 0.029(7) 0.027(6) -0.004(5) 0.005(5) -0.005(5) C76 0.025(7) 0.034(7) 0.037(7) 0.000(6) -0.006(6) -0.006(6) C77 0.047(9) 0.036(8) 0.024(7) 0.001(6) -0.005(6) -0.002(7) C78 0.039(4) 0.037(4) 0.037(4) 0.000(3) 0.003(3) -0.015(3) C79 0.045(10) 0.076(13) 0.077(12) 0.040(10) -0.001(9) -0.034(9) C80 0.034(8) 0.053(10) 0.053(9) 0.017(7) 0.004(7) -0.009(7) C81 0.035(8) 0.042(8) 0.042(8) -0.019(6) 0.002(6) -0.022(7) C82 0.047(9) 0.037(8) 0.055(9) 0.002(7) -0.011(7) -0.025(7) C83 0.049(9) 0.042(9) 0.031(7) 0.008(6) -0.002(6) -0.016(7) C84 0.042(4) 0.038(4) 0.044(4) -0.003(3) 0.001(3) -0.015(3) C85 0.066(12) 0.065(12) 0.057(11) 0.018(9) 0.006(9) -0.032(10) C86 0.097(14) 0.027(8) 0.114(15) 0.022(9) 0.059(12) -0.021(9) C87 0.137(19) 0.107(17) 0.22(2) -0.049(17) 0.022(18) -0.097(16) C88 0.044(10) 0.048(10) 0.071(11) 0.005(8) -0.011(8) -0.016(8) _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 Pu1 O2 2.510(8) . ? Pu1 O1 2.516(8) . ? Pu1 Se2 3.0354(13) . ? Pu1 Se6 3.0414(14) . ? Pu1 Se5 3.0663(13) . ? Pu1 Se3 3.0677(15) . ? Pu1 Se4 3.0989(14) . ? Pu1 Se1 3.1128(14) . ? Pu2 O3 2.466(7) . ? Pu2 O4 2.502(8) . ? Pu2 Se11 3.0627(13) . ? Pu2 Se8 3.0723(14) . ? Pu2 Se9 3.0719(14) . ? Pu2 Se7 3.0879(15) . ? Pu2 Se10 3.1138(14) . ? Pu2 Se12 3.1323(15) . ? Se1 P1 2.159(3) . ? Se2 P1 2.168(3) . ? Se3 P2 2.157(3) . ? Se4 P2 2.163(3) . ? Se5 P3 2.165(3) . ? Se6 P3 2.169(3) . ? Se7 P4 2.165(3) . ? Se8 P4 2.165(3) . ? Se9 P5 2.155(3) . ? Se10 P5 2.153(3) . ? Se11 P6 2.163(3) . ? Se12 P6 2.168(3) . ? P1 C1 1.815(13) . ? P1 C7 1.839(11) . ? P2 C13 1.794(11) . ? P2 C19 1.824(11) . ? P3 C25 1.815(11) . ? P3 C31 1.833(11) . ? P4 C51 1.838(11) . ? P4 C45 1.840(11) . ? P5 C63 1.820(12) . ? P5 C62 1.827(12) . ? P6 C69 1.795(12) . ? P6 C75 1.828(12) . ? O1 C37 1.454(14) . ? O1 C40 1.445(14) . ? O2 C44 1.420(15) . ? O2 C41 1.444(15) . ? O3 C84 1.464(14) . ? O3 C81 1.478(13) . ? O4 C88 1.419(17) . ? O4 C85 1.468(16) . ? C1 C6 1.384(18) . ? C1 C2 1.394(17) . ? C2 C3 1.406(19) . ? C3 C4 1.44(2) . ? C4 C5 1.33(2) . ? C5 C6 1.442(18) . ? C7 C12 1.355(17) . ? C7 C8 1.398(17) . ? C8 C9 1.416(18) . ? C9 C10 1.35(2) . ? C10 C11 1.33(2) . ? C11 C12 1.409(17) . ? C13 C14 1.394(16) . ? C13 C18 1.418(15) . ? C14 C15 1.390(16) . ? C15 C16 1.383(18) . ? C16 C17 1.391(18) . ? C17 C18 1.404(16) . ? C19 C24 1.375(16) . ? C19 C20 1.393(16) . ? C20 C21 1.408(17) . ? C21 C22 1.42(2) . ? C22 C23 1.33(2) . ? C23 C24 1.398(18) . ? C25 C26 1.373(16) . ? C25 C30 1.400(16) . ? C26 C27 1.367(17) . ? C27 C28 1.383(17) . ? C28 C29 1.371(18) . ? C29 C30 1.382(17) . ? C31 C36 1.367(16) . ? C31 C32 1.377(16) . ? C32 C33 1.392(16) . ? C33 C34 1.392(18) . ? C34 C35 1.370(19) . ? C35 C36 1.408(17) . ? C37 C38 1.516(17) . ? C38 C39 1.525(17) . ? C39 C40 1.471(19) . ? C41 C42 1.503(17) . ? C42 C43 1.554(18) . ? C43 C44 1.462(18) . ? C45 C46 1.385(16) . ? C45 C50 1.405(15) . ? C46 C47 1.428(16) . ? C47 C48 1.381(17) . ? C48 C49 1.366(19) . ? C49 C50 1.377(17) . ? C51 C52 1.369(16) . ? C51 C56 1.386(15) . ? C52 C53 1.376(16) . ? C53 C54 1.368(19) . ? C54 C55 1.333(18) . ? C55 C56 1.399(16) . ? C57 C62 1.388(17) . ? C57 C58 1.387(17) . ? C58 C59 1.361(17) . ? C59 C60 1.369(19) . ? C60 C61 1.357(17) . ? C61 C62 1.412(16) . ? C63 C68 1.393(15) . ? C63 C64 1.419(16) . ? C64 C65 1.379(16) . ? C65 C66 1.395(17) . ? C66 C67 1.387(16) . ? C67 C68 1.390(15) . ? C69 C74 1.405(16) . ? C69 C70 1.423(16) . ? C70 C71 1.388(17) . ? C71 C72 1.366(18) . ? C72 C73 1.390(19) . ? C73 C74 1.373(18) . ? C75 C80 1.352(18) . ? C75 C76 1.397(16) . ? C76 C77 1.423(17) . ? C77 C78 1.370(18) . ? C78 C79 1.36(2) . ? C79 C80 1.453(19) . ? C81 C82 1.515(18) . ? C82 C83 1.493(18) . ? C83 C84 1.523(18) . ? C85 C86 1.45(2) . ? C86 C87 1.53(3) . ? C87 C88 1.46(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 O2 Pu1 O1 153.2(3) . . ? O2 Pu1 Se2 91.52(19) . . ? O1 Pu1 Se2 87.05(17) . . ? O2 Pu1 Se6 83.71(19) . . ? O1 Pu1 Se6 79.40(18) . . ? Se2 Pu1 Se6 137.39(3) . . ? O2 Pu1 Se5 91.69(18) . . ? O1 Pu1 Se5 101.96(18) . . ? Se2 Pu1 Se5 152.14(3) . . ? Se6 Pu1 Se5 70.47(3) . . ? O2 Pu1 Se3 67.14(19) . . ? O1 Pu1 Se3 138.51(19) . . ? Se2 Pu1 Se3 80.51(3) . . ? Se6 Pu1 Se3 133.87(4) . . ? Se5 Pu1 Se3 75.32(3) . . ? O2 Pu1 Se4 137.85(19) . . ? O1 Pu1 Se4 67.79(19) . . ? Se2 Pu1 Se4 77.62(4) . . ? Se6 Pu1 Se4 130.92(4) . . ? Se5 Pu1 Se4 81.51(4) . . ? Se3 Pu1 Se4 70.91(3) . . ? O2 Pu1 Se1 76.45(18) . . ? O1 Pu1 Se1 77.81(19) . . ? Se2 Pu1 Se1 70.94(3) . . ? Se6 Pu1 Se1 66.77(3) . . ? Se5 Pu1 Se1 136.53(4) . . ? Se3 Pu1 Se1 132.60(4) . . ? Se4 Pu1 Se1 134.06(4) . . ? O3 Pu2 O4 152.3(3) . . ? O3 Pu2 Se11 91.05(18) . . ? O4 Pu2 Se11 97.7(2) . . ? O3 Pu2 Se8 87.01(18) . . ? O4 Pu2 Se8 98.2(2) . . ? Se11 Pu2 Se8 149.10(4) . . ? O3 Pu2 Se9 142.2(2) . . ? O4 Pu2 Se9 65.4(2) . . ? Se11 Pu2 Se9 81.02(4) . . ? Se8 Pu2 Se9 81.81(4) . . ? O3 Pu2 Se7 82.33(19) . . ? O4 Pu2 Se7 74.0(2) . . ? Se11 Pu2 Se7 139.64(3) . . ? Se8 Pu2 Se7 70.60(3) . . ? Se9 Pu2 Se7 126.33(3) . . ? O3 Pu2 Se10 71.6(2) . . ? O4 Pu2 Se10 136.1(2) . . ? Se11 Pu2 Se10 74.75(4) . . ? Se8 Pu2 Se10 75.39(4) . . ? Se9 Pu2 Se10 70.67(3) . . ? Se7 Pu2 Se10 137.85(3) . . ? O3 Pu2 Se12 77.6(2) . . ? O4 Pu2 Se12 81.0(2) . . ? Se11 Pu2 Se12 69.51(4) . . ? Se8 Pu2 Se12 139.33(4) . . ? Se9 Pu2 Se12 131.48(3) . . ? Se7 Pu2 Se12 70.19(3) . . ? Se10 Pu2 Se12 131.68(4) . . ? P1 Se1 Pu1 88.06(9) . . ? P1 Se2 Pu1 89.91(9) . . ? P2 Se3 Pu1 88.86(9) . . ? P2 Se4 Pu1 87.95(9) . . ? P3 Se5 Pu1 88.37(8) . . ? P3 Se6 Pu1 88.94(9) . . ? P4 Se7 Pu2 89.18(9) . . ? P4 Se8 Pu2 89.58(8) . . ? P5 Se9 Pu2 89.05(9) . . ? P5 Se10 Pu2 87.98(9) . . ? P6 Se11 Pu2 91.10(9) . . ? P6 Se12 Pu2 89.15(9) . . ? C1 P1 C7 105.1(5) . . ? C1 P1 Se1 110.8(4) . . ? C7 P1 Se1 111.2(4) . . ? C1 P1 Se2 109.9(4) . . ? C7 P1 Se2 108.6(4) . . ? Se1 P1 Se2 111.09(13) . . ? C13 P2 C19 104.1(5) . . ? C13 P2 Se3 110.1(4) . . ? C19 P2 Se3 109.1(4) . . ? C13 P2 Se4 110.1(4) . . ? C19 P2 Se4 111.4(4) . . ? Se3 P2 Se4 111.78(14) . . ? C25 P3 C31 105.5(5) . . ? C25 P3 Se5 111.5(4) . . ? C31 P3 Se5 111.0(4) . . ? C25 P3 Se6 110.9(4) . . ? C31 P3 Se6 109.2(4) . . ? Se5 P3 Se6 108.77(13) . . ? C51 P4 C45 103.9(5) . . ? C51 P4 Se7 112.1(4) . . ? C45 P4 Se7 108.4(4) . . ? C51 P4 Se8 109.1(4) . . ? C45 P4 Se8 112.6(4) . . ? Se7 P4 Se8 110.60(13) . . ? C63 P5 C62 104.3(5) . . ? C63 P5 Se9 108.7(4) . . ? C62 P5 Se9 111.2(4) . . ? C63 P5 Se10 110.5(4) . . ? C62 P5 Se10 109.6(4) . . ? Se9 P5 Se10 112.30(14) . . ? C69 P6 C75 103.8(5) . . ? C69 P6 Se11 111.6(4) . . ? C75 P6 Se11 109.7(4) . . ? C69 P6 Se12 111.7(4) . . ? C75 P6 Se12 110.8(4) . . ? Se11 P6 Se12 109.24(13) . . ? C37 O1 C40 107.8(10) . . ? C37 O1 Pu1 119.9(7) . . ? C40 O1 Pu1 130.6(8) . . ? C44 O2 C41 108.6(9) . . ? C44 O2 Pu1 126.2(8) . . ? C41 O2 Pu1 124.2(7) . . ? C84 O3 C81 107.0(9) . . ? C84 O3 Pu2 126.6(7) . . ? C81 O3 Pu2 125.7(7) . . ? C88 O4 C85 105.4(11) . . ? C88 O4 Pu2 127.2(8) . . ? C85 O4 Pu2 125.7(8) . . ? C6 C1 C2 121.2(12) . . ? C6 C1 P1 120.0(10) . . ? C2 C1 P1 118.8(10) . . ? C1 C2 C3 119.2(15) . . ? C2 C3 C4 120.9(14) . . ? C5 C4 C3 117.3(14) . . ? C4 C5 C6 124.1(15) . . ? C1 C6 C5 117.1(13) . . ? C12 C7 C8 119.4(11) . . ? C12 C7 P1 120.6(10) . . ? C8 C7 P1 119.8(9) . . ? C7 C8 C9 117.7(13) . . ? C10 C9 C8 121.1(14) . . ? C11 C10 C9 120.9(14) . . ? C10 C11 C12 119.8(14) . . ? C7 C12 C11 121.0(14) . . ? C14 C13 C18 118.2(11) . . ? C14 C13 P2 120.9(9) . . ? C18 C13 P2 120.8(9) . . ? C15 C14 C13 123.0(12) . . ? C14 C15 C16 118.7(13) . . ? C15 C16 C17 119.8(12) . . ? C16 C17 C18 121.9(12) . . ? C17 C18 C13 118.3(11) . . ? C24 C19 C20 120.1(11) . . ? C24 C19 P2 122.7(9) . . ? C20 C19 P2 117.2(9) . . ? C19 C20 C21 120.3(12) . . ? C20 C21 C22 116.7(13) . . ? C23 C22 C21 122.8(13) . . ? C22 C23 C24 119.9(13) . . ? C19 C24 C23 120.1(13) . . ? C26 C25 C30 118.3(11) . . ? C26 C25 P3 121.4(9) . . ? C30 C25 P3 120.2(10) . . ? C25 C26 C27 122.1(11) . . ? C26 C27 C28 118.9(12) . . ? C29 C28 C27 120.8(12) . . ? C28 C29 C30 119.7(12) . . ? C29 C30 C25 120.2(12) . . ? C36 C31 C32 120.4(11) . . ? C36 C31 P3 118.9(9) . . ? C32 C31 P3 120.5(8) . . ? C31 C32 C33 119.8(11) . . ? C34 C33 C32 120.4(12) . . ? C35 C34 C33 119.1(11) . . ? C34 C35 C36 120.5(12) . . ? C31 C36 C35 119.7(13) . . ? O1 C37 C38 106.4(10) . . ? C37 C38 C39 101.5(10) . . ? C40 C39 C38 109.2(11) . . ? O1 C40 C39 106.3(12) . . ? O2 C41 C42 104.9(10) . . ? C41 C42 C43 102.0(10) . . ? C44 C43 C42 103.3(11) . . ? O2 C44 C43 109.6(11) . . ? C46 C45 C50 120.8(10) . . ? C46 C45 P4 118.2(8) . . ? C50 C45 P4 120.9(9) . . ? C45 C46 C47 117.3(11) . . ? C48 C47 C46 121.3(13) . . ? C49 C48 C47 119.7(12) . . ? C48 C49 C50 121.1(12) . . ? C49 C50 C45 119.8(12) . . ? C52 C51 C56 118.3(11) . . ? C52 C51 P4 119.9(9) . . ? C56 C51 P4 121.8(9) . . ? C51 C52 C53 120.3(12) . . ? C54 C53 C52 121.0(12) . . ? C55 C54 C53 119.7(13) . . ? C54 C55 C56 120.5(12) . . ? C51 C56 C55 120.1(11) . . ? C62 C57 C58 120.9(12) . . ? C59 C58 C57 119.0(13) . . ? C60 C59 C58 121.7(13) . . ? C59 C60 C61 119.9(12) . . ? C60 C61 C62 120.6(12) . . ? C57 C62 C61 117.9(11) . . ? C57 C62 P5 120.1(9) . . ? C61 C62 P5 122.0(10) . . ? C68 C63 C64 118.5(11) . . ? C68 C63 P5 122.3(9) . . ? C64 C63 P5 119.0(9) . . ? C65 C64 C63 120.9(12) . . ? C64 C65 C66 120.2(12) . . ? C67 C66 C65 118.9(11) . . ? C68 C67 C66 121.8(11) . . ? C63 C68 C67 119.7(11) . . ? C74 C69 C70 117.5(11) . . ? C74 C69 P6 122.0(9) . . ? C70 C69 P6 120.4(9) . . ? C71 C70 C69 120.3(12) . . ? C72 C71 C70 120.5(13) . . ? C71 C72 C73 120.4(12) . . ? C74 C73 C72 120.2(12) . . ? C73 C74 C69 121.2(12) . . ? C80 C75 C76 121.3(12) . . ? C80 C75 P6 120.7(10) . . ? C76 C75 P6 118.0(9) . . ? C75 C76 C77 119.0(12) . . ? C78 C77 C76 119.8(12) . . ? C77 C78 C79 121.4(13) . . ? C78 C79 C80 119.3(14) . . ? C75 C80 C79 119.2(13) . . ? O3 C81 C82 102.9(10) . . ? C83 C82 C81 102.9(11) . . ? C82 C83 C84 103.8(11) . . ? O3 C84 C83 107.0(10) . . ? O4 C85 C86 107.1(14) . . ? C87 C86 C85 103.6(15) . . ? C88 C87 C86 106.6(16) . . ? O4 C88 C87 107.8(16) . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 5.287 _refine_diff_density_min -3.847 _refine_diff_density_rms 0.295 data_apx1367 _database_code_depnum_ccdc_archive 'CCDC 906771' #TrackingRef 'web_deposit_cif_file_5_AndrewGaunt_1350598115.cif for 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H68 Ce N O P4 Se8' _chemical_formula_weight 1714.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.6878(5) _cell_length_b 21.9927(9) _cell_length_c 22.9089(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6392.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3332 _exptl_absorpt_coefficient_mu 5.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3129 _exptl_absorpt_correction_T_max 0.6716 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 64022 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.67 _reflns_number_total 12112 _reflns_number_gt 10958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _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^)+(0.0159P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.018(5) _refine_ls_number_reflns 12112 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0461 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 Ce1 Ce 0.057854(17) 0.022789(10) 0.056129(10) 0.01238(5) Uani 1 1 d . . . Se1 Se 0.16114(4) -0.05438(2) 0.15226(2) 0.01998(11) Uani 1 1 d . . . Se2 Se -0.02688(3) -0.110430(18) 0.047646(19) 0.01679(10) Uani 1 1 d . . . Se3 Se 0.28108(3) 0.080693(19) 0.068822(19) 0.01603(10) Uani 1 1 d . . . Se4 Se 0.20357(3) -0.03855(2) -0.03007(2) 0.02087(11) Uani 1 1 d . . . Se5 Se 0.05322(4) 0.140583(19) -0.014691(19) 0.02097(10) Uani 1 1 d . . . Se6 Se -0.09352(3) 0.006660(18) -0.049876(19) 0.01581(10) Uani 1 1 d . . . Se7 Se 0.05617(4) 0.125541(19) 0.150353(19) 0.01860(10) Uani 1 1 d . . . Se8 Se -0.15080(3) 0.02048(2) 0.12140(2) 0.02210(11) Uani 1 1 d . . . P1 P 0.07326(9) -0.13202(5) 0.12117(5) 0.0160(2) Uani 1 1 d . . . P2 P 0.32480(8) 0.02440(5) -0.00446(5) 0.0159(2) Uani 1 1 d . . . P3 P -0.06373(9) 0.10091(5) -0.07051(5) 0.0146(2) Uani 1 1 d . . . P4 P -0.10004(9) 0.09587(5) 0.17377(5) 0.0168(3) Uani 1 1 d . . . N1 N 0.4343(3) 0.09776(15) 0.24365(14) 0.0193(8) Uani 1 1 d . . . O1 O 0.3884(3) 0.24061(18) 0.37073(16) 0.0511(11) Uani 1 1 d . . . C1 C -0.0066(3) -0.16080(18) 0.18089(18) 0.0157(10) Uani 1 1 d . . . C2 C -0.0782(3) -0.1206(2) 0.2061(2) 0.0265(11) Uani 1 1 d . . . H2 H -0.0847 -0.0814 0.1911 0.032 Uiso 1 1 calc R . . C3 C -0.1392(4) -0.1378(2) 0.2528(2) 0.0277(12) Uani 1 1 d . . . H3 H -0.1867 -0.1104 0.2690 0.033 Uiso 1 1 calc R . . C4 C -0.1303(4) -0.1960(2) 0.2760(2) 0.0267(12) Uani 1 1 d . . . H4 H -0.1707 -0.2077 0.3080 0.032 Uiso 1 1 calc R . . C5 C -0.0611(4) -0.2357(2) 0.2508(2) 0.0347(13) Uani 1 1 d . . . H5 H -0.0557 -0.2750 0.2655 0.042 Uiso 1 1 calc R . . C6 C 0.0016(4) -0.2186(2) 0.20365(19) 0.0263(12) Uani 1 1 d . . . H6 H 0.0490 -0.2461 0.1876 0.032 Uiso 1 1 calc R . . C7 C 0.1612(3) -0.19426(19) 0.10267(18) 0.0174(10) Uani 1 1 d . . . C8 C 0.1230(4) -0.2457(2) 0.0753(2) 0.0243(11) Uani 1 1 d . . . H8 H 0.0517 -0.2483 0.0662 0.029 Uiso 1 1 calc R . . C9 C 0.1893(4) -0.2935(2) 0.0614(2) 0.0346(13) Uani 1 1 d . . . H9 H 0.1627 -0.3279 0.0430 0.042 Uiso 1 1 calc R . . C10 C 0.2944(4) -0.2898(2) 0.0748(2) 0.0380(14) Uani 1 1 d . . . H10 H 0.3390 -0.3220 0.0656 0.046 Uiso 1 1 calc R . . C11 C 0.3341(4) -0.2392(2) 0.1014(2) 0.0420(15) Uani 1 1 d . . . H11 H 0.4056 -0.2368 0.1099 0.050 Uiso 1 1 calc R . . C12 C 0.2683(4) -0.1920(2) 0.1155(2) 0.0349(13) Uani 1 1 d . . . H12 H 0.2957 -0.1578 0.1339 0.042 Uiso 1 1 calc R . . C13 C 0.4446(3) -0.0159(2) 0.01421(17) 0.0194(10) Uani 1 1 d . . . C14 C 0.4431(4) -0.0760(2) 0.0324(2) 0.0319(12) Uani 1 1 d . . . H14 H 0.3797 -0.0972 0.0331 0.038 Uiso 1 1 calc R . . C15 C 0.5346(4) -0.1045(2) 0.0493(2) 0.0430(14) Uani 1 1 d . . . H15 H 0.5325 -0.1446 0.0622 0.052 Uiso 1 1 calc R . . C16 C 0.6292(4) -0.0741(2) 0.0472(2) 0.0346(13) Uani 1 1 d . . . H16 H 0.6911 -0.0937 0.0580 0.042 Uiso 1 1 calc R . . C17 C 0.6320(3) -0.0145(3) 0.02894(19) 0.0318(13) Uani 1 1 d . . . H17 H 0.6958 0.0062 0.0273 0.038 Uiso 1 1 calc R . . C18 C 0.5404(3) 0.0144(2) 0.01323(18) 0.0239(11) Uani 1 1 d . . . H18 H 0.5426 0.0549 0.0017 0.029 Uiso 1 1 calc R . . C19 C 0.3577(3) 0.07025(19) -0.06736(19) 0.0176(10) Uani 1 1 d . . . C20 C 0.3421(3) 0.1320(2) -0.0691(2) 0.0261(11) Uani 1 1 d . . . H20 H 0.3190 0.1525 -0.0360 0.031 Uiso 1 1 calc R . . C21 C 0.3608(4) 0.1642(2) -0.1206(2) 0.0354(13) Uani 1 1 d . . . H21 H 0.3508 0.2060 -0.1217 0.043 Uiso 1 1 calc R . . C22 C 0.3939(4) 0.1339(3) -0.1693(2) 0.0391(15) Uani 1 1 d . . . H22 H 0.4050 0.1555 -0.2036 0.047 Uiso 1 1 calc R . . C23 C 0.4112(4) 0.0722(3) -0.1686(2) 0.0406(15) Uani 1 1 d . . . H23 H 0.4353 0.0522 -0.2018 0.049 Uiso 1 1 calc R . . C24 C 0.3920(3) 0.0401(2) -0.11713(19) 0.0280(12) Uani 1 1 d . . . H24 H 0.4022 -0.0018 -0.1162 0.034 Uiso 1 1 calc R . . C25 C -0.0197(3) 0.10744(18) -0.14593(18) 0.0159(10) Uani 1 1 d . . . C26 C 0.0849(3) 0.09190(18) -0.15954(19) 0.0206(10) Uani 1 1 d . . . H26 H 0.1298 0.0780 -0.1304 0.025 Uiso 1 1 calc R . . C27 C 0.1207(4) 0.0974(2) -0.2161(2) 0.0300(12) Uani 1 1 d . . . H27 H 0.1898 0.0869 -0.2251 0.036 Uiso 1 1 calc R . . C28 C 0.0548(4) 0.1182(2) -0.2592(2) 0.0362(13) Uani 1 1 d . . . H28 H 0.0794 0.1220 -0.2973 0.043 Uiso 1 1 calc R . . C29 C -0.0478(4) 0.1336(2) -0.2460(2) 0.0418(14) Uani 1 1 d . . . H29 H -0.0925 0.1474 -0.2753 0.050 Uiso 1 1 calc R . . C30 C -0.0846(4) 0.1285(2) -0.1897(2) 0.0281(12) Uani 1 1 d . . . H30 H -0.1537 0.1393 -0.1811 0.034 Uiso 1 1 calc R . . C31 C -0.1846(3) 0.14508(18) -0.06774(18) 0.0151(9) Uani 1 1 d . . . C32 C -0.2827(3) 0.11791(19) -0.07190(18) 0.0190(10) Uani 1 1 d . . . H32 H -0.2872 0.0758 -0.0749 0.023 Uiso 1 1 calc R . . C33 C -0.3733(3) 0.15184(19) -0.07173(19) 0.0222(11) Uani 1 1 d . . . H33 H -0.4385 0.1328 -0.0749 0.027 Uiso 1 1 calc R . . C34 C -0.3676(3) 0.2146(2) -0.06679(19) 0.0222(11) Uani 1 1 d . . . H34 H -0.4289 0.2378 -0.0672 0.027 Uiso 1 1 calc R . . C35 C -0.2718(3) 0.24233(19) -0.0614(2) 0.0243(11) Uani 1 1 d . . . H35 H -0.2682 0.2843 -0.0572 0.029 Uiso 1 1 calc R . . C36 C -0.1795(3) 0.20817(18) -0.06209(19) 0.0198(10) Uani 1 1 d . . . H36 H -0.1145 0.2274 -0.0588 0.024 Uiso 1 1 calc R . . C37 C -0.1980(3) 0.15594(19) 0.16685(19) 0.0178(10) Uani 1 1 d . . . C38 C -0.2479(4) 0.1664(2) 0.1134(2) 0.0309(12) Uani 1 1 d . . . H38 H -0.2286 0.1436 0.0809 0.037 Uiso 1 1 calc R . . C39 C -0.3253(4) 0.2097(2) 0.1082(2) 0.0349(13) Uani 1 1 d . . . H39 H -0.3579 0.2160 0.0723 0.042 Uiso 1 1 calc R . . C40 C -0.3548(4) 0.2441(2) 0.1558(2) 0.0320(13) Uani 1 1 d . . . H40 H -0.4078 0.2731 0.1522 0.038 Uiso 1 1 calc R . . C41 C -0.3057(4) 0.2353(2) 0.2086(2) 0.0263(12) Uani 1 1 d . . . H41 H -0.3245 0.2589 0.2406 0.032 Uiso 1 1 calc R . . C42 C -0.2280(3) 0.19126(19) 0.2144(2) 0.0224(11) Uani 1 1 d . . . H42 H -0.1957 0.1853 0.2504 0.027 Uiso 1 1 calc R . . C43 C -0.1063(3) 0.07580(19) 0.25101(19) 0.0201(10) Uani 1 1 d . . . C44 C -0.1811(4) 0.0343(2) 0.2699(2) 0.0306(12) Uani 1 1 d . . . H44 H -0.2233 0.0143 0.2428 0.037 Uiso 1 1 calc R . . C45 C -0.1930(4) 0.0227(2) 0.3282(2) 0.0429(14) Uani 1 1 d . . . H45 H -0.2429 -0.0055 0.3405 0.052 Uiso 1 1 calc R . . C46 C -0.1326(5) 0.0518(2) 0.3683(2) 0.0421(15) Uani 1 1 d . . . H46 H -0.1433 0.0447 0.4078 0.050 Uiso 1 1 calc R . . C47 C -0.0554(5) 0.0921(2) 0.3506(2) 0.0391(13) Uani 1 1 d . . . H47 H -0.0127 0.1113 0.3779 0.047 Uiso 1 1 calc R . . C48 C -0.0424(4) 0.1036(2) 0.29122(19) 0.0301(12) Uani 1 1 d . . . H48 H 0.0098 0.1303 0.2788 0.036 Uiso 1 1 calc R . . C49 C 0.4110(3) 0.1654(2) 0.2466(2) 0.0275(12) Uani 1 1 d . . . H49A H 0.3739 0.1737 0.2828 0.033 Uiso 1 1 calc R . . H49B H 0.4774 0.1872 0.2480 0.033 Uiso 1 1 calc R . . C50 C 0.3464(4) 0.1906(2) 0.1966(2) 0.0369(14) Uani 1 1 d . . . H50A H 0.3801 0.1809 0.1603 0.055 Uiso 1 1 calc R . . H50B H 0.3409 0.2340 0.2005 0.055 Uiso 1 1 calc R . . H50C H 0.2772 0.1730 0.1974 0.055 Uiso 1 1 calc R . . C51 C 0.3344(3) 0.0611(2) 0.2335(2) 0.0269(12) Uani 1 1 d . . . H51A H 0.3073 0.0709 0.1950 0.032 Uiso 1 1 calc R . . H51B H 0.3526 0.0183 0.2334 0.032 Uiso 1 1 calc R . . C52 C 0.2472(4) 0.0711(2) 0.2777(2) 0.0379(14) Uani 1 1 d . . . H52A H 0.2710 0.0586 0.3156 0.057 Uiso 1 1 calc R . . H52B H 0.1865 0.0477 0.2668 0.057 Uiso 1 1 calc R . . H52C H 0.2289 0.1135 0.2787 0.057 Uiso 1 1 calc R . . C53 C 0.4835(4) 0.0781(2) 0.30064(19) 0.0274(12) Uani 1 1 d . . . H53A H 0.4305 0.0811 0.3310 0.033 Uiso 1 1 calc R . . H53B H 0.5032 0.0356 0.2974 0.033 Uiso 1 1 calc R . . C54 C 0.5790(4) 0.1137(2) 0.3196(2) 0.0384(14) Uani 1 1 d . . . H54A H 0.6300 0.1140 0.2886 0.058 Uiso 1 1 calc R . . H54B H 0.6093 0.0951 0.3536 0.058 Uiso 1 1 calc R . . H54C H 0.5587 0.1547 0.3286 0.058 Uiso 1 1 calc R . . C55 C 0.5089(4) 0.0871(2) 0.1926(2) 0.0272(12) Uani 1 1 d . . . H55A H 0.4758 0.1026 0.1575 0.033 Uiso 1 1 calc R . . H55B H 0.5723 0.1108 0.1992 0.033 Uiso 1 1 calc R . . C56 C 0.5405(4) 0.0220(2) 0.1820(2) 0.0383(13) Uani 1 1 d . . . H56A H 0.5653 0.0044 0.2178 0.058 Uiso 1 1 calc R . . H56B H 0.5957 0.0207 0.1533 0.058 Uiso 1 1 calc R . . H56C H 0.4807 -0.0005 0.1681 0.058 Uiso 1 1 calc R . . C57 C 0.3752(4) 0.2037(3) 0.4212(2) 0.0479(16) Uani 1 1 d . . . H57A H 0.4094 0.2224 0.4545 0.057 Uiso 1 1 calc R . . H57B H 0.4061 0.1639 0.4149 0.057 Uiso 1 1 calc R . . C58 C 0.2579(4) 0.1980(2) 0.4319(3) 0.0474(15) Uani 1 1 d . . . H58A H 0.2289 0.1626 0.4124 0.057 Uiso 1 1 calc R . . H58B H 0.2422 0.1957 0.4733 0.057 Uiso 1 1 calc R . . C59 C 0.2183(5) 0.2540(3) 0.4065(3) 0.086(3) Uani 1 1 d . . . H59A H 0.2123 0.2852 0.4363 0.103 Uiso 1 1 calc R . . H59B H 0.1493 0.2473 0.3895 0.103 Uiso 1 1 calc R . . C60 C 0.2936(5) 0.2727(3) 0.3614(2) 0.0457(15) Uani 1 1 d . . . H60A H 0.2658 0.2635 0.3229 0.055 Uiso 1 1 calc R . . H60B H 0.3062 0.3162 0.3638 0.055 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 Ce1 0.01181(11) 0.01348(12) 0.01187(12) 0.00012(10) -0.00013(11) -0.00059(10) Se1 0.0232(2) 0.0179(2) 0.0188(3) 0.0023(2) -0.0070(2) -0.0046(2) Se2 0.0190(2) 0.0155(2) 0.0158(2) 0.00104(19) -0.00378(19) -0.00264(17) Se3 0.0140(2) 0.0179(2) 0.0162(2) -0.00277(19) 0.00022(19) -0.00109(18) Se4 0.0158(2) 0.0240(3) 0.0228(3) -0.0088(2) 0.00284(19) -0.00324(19) Se5 0.0235(2) 0.0176(2) 0.0218(2) 0.00310(19) -0.0094(2) -0.0066(2) Se6 0.0167(2) 0.0133(2) 0.0175(2) 0.00118(19) -0.00444(19) -0.00174(17) Se7 0.0179(2) 0.0204(2) 0.0175(2) -0.00565(19) 0.0036(2) -0.0034(2) Se8 0.0174(2) 0.0223(2) 0.0266(3) -0.0050(2) 0.0039(2) -0.0029(2) P1 0.0180(6) 0.0148(6) 0.0152(6) 0.0015(5) -0.0019(5) -0.0010(5) P2 0.0125(6) 0.0191(6) 0.0163(6) -0.0011(5) 0.0014(5) -0.0015(5) P3 0.0144(6) 0.0142(6) 0.0151(6) 0.0010(4) -0.0028(5) -0.0009(5) P4 0.0154(6) 0.0176(6) 0.0174(6) 0.0005(5) 0.0029(5) 0.0010(5) N1 0.021(2) 0.022(2) 0.0145(19) 0.0013(16) -0.0044(17) -0.0015(17) O1 0.045(2) 0.073(3) 0.035(2) 0.010(2) 0.001(2) 0.002(2) C1 0.018(2) 0.013(2) 0.016(2) -0.0030(19) -0.0056(19) -0.0004(19) C2 0.027(3) 0.023(3) 0.029(3) 0.009(2) 0.005(2) 0.004(2) C3 0.023(3) 0.026(3) 0.034(3) 0.002(2) 0.008(2) 0.002(2) C4 0.033(3) 0.028(3) 0.019(3) 0.001(2) 0.002(2) -0.015(2) C5 0.060(4) 0.015(2) 0.029(3) 0.010(2) 0.004(3) -0.005(3) C6 0.040(3) 0.018(3) 0.021(3) 0.000(2) 0.006(2) 0.000(2) C7 0.018(2) 0.019(2) 0.015(2) 0.0014(19) -0.0044(19) 0.000(2) C8 0.028(3) 0.024(3) 0.021(3) 0.000(2) 0.002(2) 0.002(2) C9 0.051(4) 0.027(3) 0.025(3) -0.004(2) 0.004(3) 0.004(2) C10 0.045(3) 0.039(3) 0.031(3) 0.000(3) 0.002(3) 0.025(3) C11 0.030(3) 0.044(4) 0.052(4) -0.005(3) -0.008(3) 0.012(3) C12 0.028(3) 0.035(3) 0.042(3) -0.009(3) -0.011(3) 0.005(2) C13 0.016(2) 0.030(3) 0.012(2) -0.002(2) 0.0051(19) 0.003(2) C14 0.023(3) 0.028(3) 0.045(3) -0.004(2) -0.008(3) 0.001(2) C15 0.037(3) 0.026(3) 0.066(4) -0.004(3) -0.012(3) 0.011(2) C16 0.023(3) 0.052(4) 0.029(3) -0.011(3) -0.005(2) 0.018(2) C17 0.016(2) 0.062(4) 0.018(3) 0.005(3) -0.002(2) 0.003(2) C18 0.016(2) 0.034(3) 0.022(2) 0.010(2) 0.000(2) 0.002(2) C19 0.010(2) 0.025(3) 0.018(3) 0.002(2) -0.0012(19) -0.0030(18) C20 0.011(2) 0.040(3) 0.027(3) 0.008(2) 0.003(2) 0.004(2) C21 0.018(3) 0.042(3) 0.046(4) 0.022(3) 0.003(3) 0.000(2) C22 0.022(3) 0.068(4) 0.028(3) 0.027(3) -0.005(2) -0.010(3) C23 0.026(3) 0.080(5) 0.016(3) 0.002(3) 0.002(2) -0.016(3) C24 0.023(3) 0.042(3) 0.019(3) -0.001(2) 0.003(2) -0.012(2) C25 0.018(2) 0.013(2) 0.017(2) -0.0024(19) 0.0020(19) 0.0002(18) C26 0.022(3) 0.019(2) 0.021(3) -0.005(2) 0.000(2) 0.0019(19) C27 0.026(3) 0.028(3) 0.036(3) -0.009(2) 0.005(2) -0.006(2) C28 0.047(3) 0.034(3) 0.028(3) 0.002(2) 0.013(3) -0.003(3) C29 0.045(3) 0.062(4) 0.018(3) 0.011(3) 0.001(3) 0.006(3) C30 0.022(3) 0.041(3) 0.020(3) 0.002(2) 0.000(2) 0.010(2) C31 0.020(2) 0.016(2) 0.009(2) 0.0044(19) -0.0015(18) 0.0010(18) C32 0.023(2) 0.015(2) 0.019(2) -0.0022(19) -0.005(2) 0.0039(19) C33 0.021(2) 0.023(3) 0.023(3) 0.003(2) 0.002(2) 0.002(2) C34 0.021(3) 0.028(3) 0.018(3) 0.000(2) 0.000(2) 0.006(2) C35 0.031(3) 0.014(2) 0.028(3) -0.001(2) 0.002(2) 0.003(2) C36 0.019(2) 0.019(2) 0.022(3) 0.000(2) -0.002(2) -0.0022(19) C37 0.015(2) 0.014(2) 0.024(3) 0.001(2) 0.003(2) -0.0025(19) C38 0.036(3) 0.032(3) 0.025(3) 0.005(2) 0.005(2) 0.008(2) C39 0.038(3) 0.035(3) 0.032(3) 0.015(3) -0.008(3) 0.004(3) C40 0.023(3) 0.023(3) 0.050(4) 0.007(3) 0.009(3) 0.003(2) C41 0.025(3) 0.020(3) 0.035(3) 0.000(2) 0.006(2) 0.004(2) C42 0.019(3) 0.020(3) 0.028(3) 0.001(2) -0.001(2) 0.000(2) C43 0.025(3) 0.018(2) 0.017(3) 0.004(2) 0.006(2) 0.010(2) C44 0.033(3) 0.032(3) 0.027(3) 0.006(2) 0.010(2) 0.005(2) C45 0.053(4) 0.031(3) 0.044(4) 0.017(3) 0.018(3) 0.011(3) C46 0.075(4) 0.033(3) 0.018(3) 0.008(3) 0.018(3) 0.015(3) C47 0.055(4) 0.040(3) 0.022(3) 0.002(2) 0.001(3) 0.019(3) C48 0.043(3) 0.023(3) 0.025(3) 0.001(2) 0.006(2) 0.009(2) C49 0.026(3) 0.025(3) 0.032(3) -0.002(2) -0.003(2) 0.000(2) C50 0.041(3) 0.022(3) 0.047(4) 0.008(3) -0.011(3) 0.005(2) C51 0.028(3) 0.025(3) 0.027(3) -0.001(2) -0.001(2) -0.008(2) C52 0.026(3) 0.058(4) 0.029(3) 0.002(3) 0.006(2) -0.003(3) C53 0.034(3) 0.031(3) 0.018(3) 0.002(2) -0.004(2) -0.003(2) C54 0.031(3) 0.050(4) 0.034(3) 0.010(3) -0.007(2) -0.005(3) C55 0.025(3) 0.037(3) 0.020(3) 0.001(2) 0.003(2) -0.002(2) C56 0.032(3) 0.045(3) 0.038(3) -0.008(3) 0.006(2) 0.007(3) C57 0.056(4) 0.058(4) 0.030(3) -0.003(3) -0.004(3) 0.022(3) C58 0.060(4) 0.040(3) 0.041(4) 0.006(3) 0.007(3) -0.001(3) C59 0.066(5) 0.113(7) 0.078(6) 0.057(5) 0.031(4) 0.061(5) C60 0.057(4) 0.044(4) 0.036(4) 0.010(3) -0.006(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 Se4 3.0229(5) . ? Ce1 Se8 3.0409(5) . ? Ce1 Se5 3.0573(5) . ? Ce1 Se1 3.0736(5) . ? Ce1 Se6 3.1164(5) . ? Ce1 Se3 3.1190(5) . ? Ce1 Se7 3.1251(5) . ? Ce1 Se2 3.1269(5) . ? Se1 P1 2.1602(12) . ? Se2 P1 2.1626(12) . ? Se3 P2 2.1585(12) . ? Se4 P2 2.1509(12) . ? Se5 P3 2.1443(12) . ? Se6 P3 2.1593(11) . ? Se7 P4 2.1545(12) . ? Se8 P4 2.1457(12) . ? P1 C7 1.816(4) . ? P1 C1 1.816(4) . ? P2 C19 1.808(4) . ? P2 C13 1.811(4) . ? P3 C31 1.816(4) . ? P3 C25 1.821(4) . ? P4 C37 1.821(4) . ? P4 C43 1.826(4) . ? N1 C53 1.510(5) . ? N1 C49 1.519(5) . ? N1 C51 1.521(5) . ? N1 C55 1.522(5) . ? O1 C60 1.411(6) . ? O1 C57 1.421(6) . ? C1 C6 1.377(6) . ? C1 C2 1.393(6) . ? C2 C3 1.375(6) . ? C3 C4 1.390(6) . ? C4 C5 1.366(6) . ? C5 C6 1.394(6) . ? C7 C8 1.382(6) . ? C7 C12 1.391(6) . ? C8 C9 1.382(6) . ? C9 C10 1.371(7) . ? C10 C11 1.364(7) . ? C11 C12 1.371(6) . ? C13 C14 1.385(6) . ? C13 C18 1.386(6) . ? C14 C15 1.376(6) . ? C15 C16 1.375(7) . ? C16 C17 1.376(7) . ? C17 C18 1.372(6) . ? C19 C20 1.374(6) . ? C19 C24 1.389(6) . ? C20 C21 1.395(6) . ? C21 C22 1.365(7) . ? C22 C23 1.375(7) . ? C23 C24 1.395(6) . ? C25 C30 1.377(6) . ? C25 C26 1.406(6) . ? C26 C27 1.378(6) . ? C27 C28 1.373(6) . ? C28 C29 1.379(7) . ? C29 C30 1.377(6) . ? C31 C32 1.385(5) . ? C31 C36 1.395(5) . ? C32 C33 1.371(5) . ? C33 C34 1.387(6) . ? C34 C35 1.365(6) . ? C35 C36 1.392(5) . ? C37 C42 1.390(6) . ? C37 C38 1.398(6) . ? C38 C39 1.374(6) . ? C39 C40 1.379(7) . ? C40 C41 1.375(6) . ? C41 C42 1.387(6) . ? C43 C48 1.371(6) . ? C43 C44 1.385(6) . ? C44 C45 1.369(6) . ? C45 C46 1.357(7) . ? C46 C47 1.381(7) . ? C47 C48 1.393(6) . ? C49 C50 1.513(6) . ? C51 C52 1.515(6) . ? C53 C54 1.508(6) . ? C55 C56 1.507(6) . ? C57 C58 1.514(7) . ? C58 C59 1.450(7) . ? C59 C60 1.468(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 Se4 Ce1 Se8 147.804(14) . . ? Se4 Ce1 Se5 92.477(14) . . ? Se8 Ce1 Se5 104.974(14) . . ? Se4 Ce1 Se1 87.761(14) . . ? Se8 Ce1 Se1 90.552(14) . . ? Se5 Ce1 Se1 148.901(14) . . ? Se4 Ce1 Se6 79.459(13) . . ? Se8 Ce1 Se6 81.067(13) . . ? Se5 Ce1 Se6 70.796(12) . . ? Se1 Ce1 Se6 139.310(13) . . ? Se4 Ce1 Se3 71.803(12) . . ? Se8 Ce1 Se3 138.726(14) . . ? Se5 Ce1 Se3 73.797(13) . . ? Se1 Ce1 Se3 76.790(13) . . ? Se6 Ce1 Se3 132.747(13) . . ? Se4 Ce1 Se7 141.086(14) . . ? Se8 Ce1 Se7 70.521(13) . . ? Se5 Ce1 Se7 75.741(13) . . ? Se1 Ce1 Se7 84.679(13) . . ? Se6 Ce1 Se7 128.049(13) . . ? Se3 Ce1 Se7 69.302(12) . . ? Se4 Ce1 Se2 75.614(12) . . ? Se8 Ce1 Se2 73.474(13) . . ? Se5 Ce1 Se2 138.970(13) . . ? Se1 Ce1 Se2 70.961(12) . . ? Se6 Ce1 Se2 68.471(11) . . ? Se3 Ce1 Se2 134.473(13) . . ? Se7 Ce1 Se2 135.899(14) . . ? P1 Se1 Ce1 88.86(3) . . ? P1 Se2 Ce1 87.44(3) . . ? P2 Se3 Ce1 85.79(3) . . ? P2 Se4 Ce1 88.39(3) . . ? P3 Se5 Ce1 89.14(3) . . ? P3 Se6 Ce1 87.33(3) . . ? P4 Se7 Ce1 87.67(3) . . ? P4 Se8 Ce1 90.04(3) . . ? C7 P1 C1 104.82(19) . . ? C7 P1 Se1 110.85(14) . . ? C1 P1 Se1 108.37(13) . . ? C7 P1 Se2 110.16(14) . . ? C1 P1 Se2 109.59(13) . . ? Se1 P1 Se2 112.74(5) . . ? C19 P2 C13 105.52(18) . . ? C19 P2 Se4 107.87(14) . . ? C13 P2 Se4 110.45(15) . . ? C19 P2 Se3 111.06(15) . . ? C13 P2 Se3 108.23(13) . . ? Se4 P2 Se3 113.43(5) . . ? C31 P3 C25 104.45(19) . . ? C31 P3 Se5 110.22(14) . . ? C25 P3 Se5 108.76(14) . . ? C31 P3 Se6 110.98(14) . . ? C25 P3 Se6 109.70(14) . . ? Se5 P3 Se6 112.41(5) . . ? C37 P4 C43 103.31(19) . . ? C37 P4 Se8 107.89(15) . . ? C43 P4 Se8 110.00(15) . . ? C37 P4 Se7 112.74(14) . . ? C43 P4 Se7 110.78(15) . . ? Se8 P4 Se7 111.77(5) . . ? C53 N1 C49 108.8(3) . . ? C53 N1 C51 108.9(3) . . ? C49 N1 C51 111.3(3) . . ? C53 N1 C55 111.3(3) . . ? C49 N1 C55 107.8(3) . . ? C51 N1 C55 108.6(3) . . ? C60 O1 C57 108.0(4) . . ? C6 C1 C2 118.6(4) . . ? C6 C1 P1 124.4(3) . . ? C2 C1 P1 117.0(3) . . ? C3 C2 C1 120.9(4) . . ? C2 C3 C4 120.4(4) . . ? C5 C4 C3 118.6(4) . . ? C4 C5 C6 121.5(4) . . ? C1 C6 C5 120.0(4) . . ? C8 C7 C12 117.8(4) . . ? C8 C7 P1 120.6(3) . . ? C12 C7 P1 121.6(4) . . ? C7 C8 C9 120.9(5) . . ? C10 C9 C8 119.7(5) . . ? C11 C10 C9 120.5(5) . . ? C10 C11 C12 119.9(5) . . ? C11 C12 C7 121.2(5) . . ? C14 C13 C18 118.4(4) . . ? C14 C13 P2 121.8(3) . . ? C18 C13 P2 119.8(3) . . ? C15 C14 C13 120.6(5) . . ? C16 C15 C14 120.3(5) . . ? C15 C16 C17 119.8(4) . . ? C18 C17 C16 119.9(5) . . ? C17 C18 C13 121.1(4) . . ? C20 C19 C24 119.6(4) . . ? C20 C19 P2 122.8(4) . . ? C24 C19 P2 117.4(3) . . ? C19 C20 C21 120.1(5) . . ? C22 C21 C20 119.7(5) . . ? C21 C22 C23 121.4(5) . . ? C22 C23 C24 118.7(5) . . ? C19 C24 C23 120.5(5) . . ? C30 C25 C26 119.0(4) . . ? C30 C25 P3 122.3(3) . . ? C26 C25 P3 118.7(3) . . ? C27 C26 C25 119.9(4) . . ? C28 C27 C26 120.3(5) . . ? C27 C28 C29 119.9(5) . . ? C30 C29 C28 120.4(5) . . ? C25 C30 C29 120.5(4) . . ? C32 C31 C36 118.5(4) . . ? C32 C31 P3 121.7(3) . . ? C36 C31 P3 119.8(3) . . ? C33 C32 C31 121.3(4) . . ? C32 C33 C34 119.9(4) . . ? C35 C34 C33 119.9(4) . . ? C34 C35 C36 120.5(4) . . ? C35 C36 C31 119.9(4) . . ? C42 C37 C38 118.1(4) . . ? C42 C37 P4 121.6(3) . . ? C38 C37 P4 120.3(3) . . ? C39 C38 C37 120.9(5) . . ? C38 C39 C40 120.4(5) . . ? C41 C40 C39 119.7(5) . . ? C40 C41 C42 120.3(5) . . ? C41 C42 C37 120.7(4) . . ? C48 C43 C44 119.3(4) . . ? C48 C43 P4 121.2(3) . . ? C44 C43 P4 119.4(4) . . ? C45 C44 C43 120.2(5) . . ? C46 C45 C44 120.6(5) . . ? C45 C46 C47 120.3(5) . . ? C46 C47 C48 119.1(5) . . ? C43 C48 C47 120.4(5) . . ? C50 C49 N1 115.5(4) . . ? C52 C51 N1 115.4(4) . . ? C54 C53 N1 115.6(4) . . ? C56 C55 N1 115.8(4) . . ? O1 C57 C58 107.2(4) . . ? C59 C58 C57 101.8(5) . . ? C58 C59 C60 107.2(5) . . ? O1 C60 C59 107.8(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.518 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.087 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 data_xpl209 _database_code_depnum_ccdc_archive 'CCDC 906772' #TrackingRef 'web_deposit_cif_file_6_AndrewGaunt_1350598115.cif for 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H68 N O P4 Pu Se8' _chemical_formula_weight 1813.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pu Pu -9.4100 4.3056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.7053(12) _cell_length_b 21.997(2) _cell_length_c 22.902(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6400.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 141(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3476 _exptl_absorpt_coefficient_mu 5.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1974 _exptl_absorpt_correction_T_max 0.6576 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 141(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 SMART 1k CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 74646 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.79 _reflns_number_total 15771 _reflns_number_gt 14364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 4.210 (Bruker, 1996)' _computing_cell_refinement 'SAINT 4.05 (Bruker, 1996)' _computing_data_reduction 'SAINT 4.05 (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.10 (Bruker, 2001)' _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^)+(0.0189P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.030(5) _refine_ls_number_reflns 15771 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0464 _refine_ls_wR_factor_gt 0.0448 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Pu1 Pu 0.057035(9) 0.022442(6) 0.055900(5) 0.01125(3) Uani 1 1 d . . . Se1 Se 0.15836(3) -0.052995(18) 0.151196(16) 0.01944(9) Uani 1 1 d . . . Se2 Se -0.02801(3) -0.110119(16) 0.047206(15) 0.01674(8) Uani 1 1 d . . . Se3 Se 0.27883(3) 0.080229(17) 0.068917(15) 0.01623(8) Uani 1 1 d . . . Se4 Se 0.19981(3) -0.038578(18) -0.029192(16) 0.02055(9) Uani 1 1 d . . . Se5 Se 0.05278(3) 0.138891(17) -0.013397(15) 0.02077(8) Uani 1 1 d . . . Se6 Se -0.09340(3) 0.005958(16) -0.049180(16) 0.01585(8) Uani 1 1 d . . . Se7 Se 0.05677(3) 0.124140(17) 0.149925(15) 0.01852(8) Uani 1 1 d . . . Se8 Se -0.14924(3) 0.020273(19) 0.119526(16) 0.02000(8) Uani 1 1 d . . . P1 P 0.07179(8) -0.13166(4) 0.12069(4) 0.0154(2) Uani 1 1 d . . . P2 P 0.32285(7) 0.02388(5) -0.00429(4) 0.01651(19) Uani 1 1 d . . . P3 P -0.06446(8) 0.10021(4) -0.07004(4) 0.01421(18) Uani 1 1 d . . . P4 P -0.09992(8) 0.09540(4) 0.17302(4) 0.0161(2) Uani 1 1 d . . . N1 N 0.4340(3) 0.09804(14) 0.24356(13) 0.0201(7) Uani 1 1 d . . . O1 O 0.3866(3) 0.24104(18) 0.37065(15) 0.0557(10) Uani 1 1 d . . . C1 C -0.0074(3) -0.16120(17) 0.18057(16) 0.0180(8) Uani 1 1 d . . . C2 C -0.0790(3) -0.12108(19) 0.20568(18) 0.0278(10) Uani 1 1 d . . . H2 H -0.0861 -0.0821 0.1904 0.033 Uiso 1 1 calc R . . C3 C -0.1399(3) -0.1383(2) 0.25325(18) 0.0306(10) Uani 1 1 d . . . H3 H -0.1873 -0.1110 0.2697 0.037 Uiso 1 1 calc R . . C4 C -0.1298(3) -0.1966(2) 0.27615(18) 0.0294(10) Uani 1 1 d . . . H4 H -0.1698 -0.2086 0.3081 0.035 Uiso 1 1 calc R . . C5 C -0.0599(4) -0.23623(19) 0.25090(17) 0.0329(10) Uani 1 1 d . . . H5 H -0.0534 -0.2754 0.2658 0.039 Uiso 1 1 calc R . . C6 C 0.0016(3) -0.21895(18) 0.20331(17) 0.0259(9) Uani 1 1 d . . . H6 H 0.0488 -0.2464 0.1869 0.031 Uiso 1 1 calc R . . C7 C 0.1610(3) -0.19355(17) 0.10260(16) 0.0191(8) Uani 1 1 d . . . C8 C 0.1226(3) -0.24522(19) 0.07434(18) 0.0273(10) Uani 1 1 d . . . H8 H 0.0517 -0.2478 0.0645 0.033 Uiso 1 1 calc R . . C9 C 0.1906(4) -0.2929(2) 0.0609(2) 0.0355(11) Uani 1 1 d . . . H9 H 0.1650 -0.3275 0.0423 0.043 Uiso 1 1 calc R . . C10 C 0.2956(4) -0.2889(2) 0.0751(2) 0.0402(12) Uani 1 1 d . . . H10 H 0.3408 -0.3209 0.0663 0.048 Uiso 1 1 calc R . . C11 C 0.3336(4) -0.2382(2) 0.1022(2) 0.0428(13) Uani 1 1 d . . . H11 H 0.4048 -0.2354 0.1114 0.051 Uiso 1 1 calc R . . C12 C 0.2667(4) -0.1911(2) 0.1159(2) 0.0356(11) Uani 1 1 d . . . H12 H 0.2933 -0.1569 0.1346 0.043 Uiso 1 1 calc R . . C13 C 0.4426(3) -0.01697(18) 0.01434(14) 0.0214(8) Uani 1 1 d . . . C14 C 0.4404(4) -0.07695(19) 0.03259(19) 0.0356(10) Uani 1 1 d . . . H14 H 0.3769 -0.0979 0.0336 0.043 Uiso 1 1 calc R . . C15 C 0.5326(4) -0.1059(2) 0.0494(2) 0.0467(13) Uani 1 1 d . . . H15 H 0.5304 -0.1460 0.0622 0.056 Uiso 1 1 calc R . . C16 C 0.6274(3) -0.0754(2) 0.04721(19) 0.0389(12) Uani 1 1 d . . . H16 H 0.6892 -0.0952 0.0578 0.047 Uiso 1 1 calc R . . C17 C 0.6301(3) -0.0160(2) 0.02932(17) 0.0341(11) Uani 1 1 d . . . H17 H 0.6939 0.0047 0.0281 0.041 Uiso 1 1 calc R . . C18 C 0.5382(3) 0.0131(2) 0.01316(15) 0.0273(10) Uani 1 1 d . . . H18 H 0.5407 0.0535 0.0013 0.033 Uiso 1 1 calc R . . C19 C 0.3572(3) 0.06898(18) -0.06764(16) 0.0203(8) Uani 1 1 d . . . C20 C 0.3411(3) 0.13168(19) -0.06987(18) 0.0255(9) Uani 1 1 d . . . H20 H 0.3177 0.1526 -0.0370 0.031 Uiso 1 1 calc R . . C21 C 0.3605(3) 0.1627(2) -0.1219(2) 0.0361(12) Uani 1 1 d . . . H21 H 0.3498 0.2045 -0.1236 0.043 Uiso 1 1 calc R . . C22 C 0.3950(3) 0.1325(3) -0.17027(19) 0.0395(13) Uani 1 1 d . . . H22 H 0.4077 0.1538 -0.2046 0.047 Uiso 1 1 calc R . . C23 C 0.4113(3) 0.0708(3) -0.16847(18) 0.0416(13) Uani 1 1 d . . . H23 H 0.4351 0.0504 -0.2015 0.050 Uiso 1 1 calc R . . C24 C 0.3920(3) 0.0386(2) -0.11690(17) 0.0311(11) Uani 1 1 d . . . H24 H 0.4025 -0.0033 -0.1157 0.037 Uiso 1 1 calc R . . C25 C -0.0198(3) 0.10747(17) -0.14531(16) 0.0175(8) Uani 1 1 d . . . C26 C 0.0843(3) 0.09112(18) -0.15920(17) 0.0224(9) Uani 1 1 d . . . H26 H 0.1287 0.0762 -0.1303 0.027 Uiso 1 1 calc R . . C27 C 0.1203(3) 0.09719(19) -0.21558(18) 0.0285(10) Uani 1 1 d . . . H27 H 0.1896 0.0871 -0.2245 0.034 Uiso 1 1 calc R . . C28 C 0.0540(4) 0.1182(2) -0.25904(19) 0.0377(11) Uani 1 1 d . . . H28 H 0.0784 0.1211 -0.2972 0.045 Uiso 1 1 calc R . . C29 C -0.0484(4) 0.1350(2) -0.24594(17) 0.0379(11) Uani 1 1 d . . . H29 H -0.0923 0.1501 -0.2750 0.045 Uiso 1 1 calc R . . C30 C -0.0851(3) 0.1290(2) -0.18894(17) 0.0280(10) Uani 1 1 d . . . H30 H -0.1542 0.1397 -0.1801 0.034 Uiso 1 1 calc R . . C31 C -0.1855(3) 0.14442(17) -0.06739(14) 0.0148(8) Uani 1 1 d . . . C32 C -0.2834(3) 0.11697(17) -0.07139(15) 0.0192(8) Uani 1 1 d . . . H32 H -0.2881 0.0749 -0.0743 0.023 Uiso 1 1 calc R . . C33 C -0.3741(3) 0.15151(18) -0.07112(17) 0.0232(9) Uani 1 1 d . . . H33 H -0.4393 0.1326 -0.0742 0.028 Uiso 1 1 calc R . . C34 C -0.3686(3) 0.21437(18) -0.06630(17) 0.0239(9) Uani 1 1 d . . . H34 H -0.4298 0.2375 -0.0665 0.029 Uiso 1 1 calc R . . C35 C -0.2720(3) 0.24217(18) -0.06121(18) 0.0259(9) Uani 1 1 d . . . H35 H -0.2680 0.2842 -0.0572 0.031 Uiso 1 1 calc R . . C36 C -0.1799(3) 0.20743(17) -0.06210(17) 0.0218(8) Uani 1 1 d . . . H36 H -0.1148 0.2264 -0.0592 0.026 Uiso 1 1 calc R . . C37 C -0.1977(3) 0.15624(17) 0.16633(16) 0.0173(8) Uani 1 1 d . . . C38 C -0.2470(3) 0.16569(19) 0.11306(18) 0.0288(10) Uani 1 1 d . . . H38 H -0.2279 0.1422 0.0810 0.035 Uiso 1 1 calc R . . C39 C -0.3246(4) 0.2098(2) 0.1071(2) 0.0366(11) Uani 1 1 d . . . H39 H -0.3565 0.2162 0.0710 0.044 Uiso 1 1 calc R . . C40 C -0.3545(3) 0.24437(19) 0.1552(2) 0.0336(11) Uani 1 1 d . . . H40 H -0.4073 0.2734 0.1517 0.040 Uiso 1 1 calc R . . C41 C -0.3057(3) 0.23529(18) 0.20778(19) 0.0272(10) Uani 1 1 d . . . H41 H -0.3249 0.2588 0.2398 0.033 Uiso 1 1 calc R . . C42 C -0.2278(3) 0.19141(18) 0.21391(18) 0.0218(9) Uani 1 1 d . . . H42 H -0.1957 0.1855 0.2500 0.026 Uiso 1 1 calc R . . C43 C -0.1081(3) 0.07505(18) 0.24991(16) 0.0209(9) Uani 1 1 d . . . C44 C -0.1835(3) 0.0331(2) 0.26872(18) 0.0300(10) Uani 1 1 d . . . H44 H -0.2251 0.0130 0.2414 0.036 Uiso 1 1 calc R . . C45 C -0.1969(4) 0.0211(2) 0.32709(19) 0.0409(12) Uani 1 1 d . . . H45 H -0.2470 -0.0070 0.3392 0.049 Uiso 1 1 calc R . . C46 C -0.1357(4) 0.0509(2) 0.3678(2) 0.0427(13) Uani 1 1 d . . . H46 H -0.1466 0.0437 0.4074 0.051 Uiso 1 1 calc R . . C47 C -0.0583(4) 0.0913(2) 0.35060(18) 0.0407(12) Uani 1 1 d . . . H47 H -0.0161 0.1103 0.3783 0.049 Uiso 1 1 calc R . . C48 C -0.0442(4) 0.10334(19) 0.29128(17) 0.0296(10) Uani 1 1 d . . . H48 H 0.0079 0.1303 0.2793 0.035 Uiso 1 1 calc R . . C49 C 0.4112(3) 0.16563(18) 0.24602(18) 0.0276(10) Uani 1 1 d . . . H49A H 0.3739 0.1741 0.2821 0.033 Uiso 1 1 calc R . . H49B H 0.4777 0.1872 0.2476 0.033 Uiso 1 1 calc R . . C50 C 0.3474(4) 0.1909(2) 0.1958(2) 0.0390(12) Uani 1 1 d . . . H50A H 0.3806 0.1803 0.1596 0.058 Uiso 1 1 calc R . . H50B H 0.3435 0.2344 0.1992 0.058 Uiso 1 1 calc R . . H50C H 0.2777 0.1741 0.1969 0.058 Uiso 1 1 calc R . . C51 C 0.3346(3) 0.0619(2) 0.23363(18) 0.0311(10) Uani 1 1 d . . . H51A H 0.3525 0.0191 0.2337 0.037 Uiso 1 1 calc R . . H51B H 0.3077 0.0717 0.1951 0.037 Uiso 1 1 calc R . . C52 C 0.2472(3) 0.0719(2) 0.27750(19) 0.0403(12) Uani 1 1 d . . . H52A H 0.2696 0.0580 0.3152 0.060 Uiso 1 1 calc R . . H52B H 0.1858 0.0497 0.2656 0.060 Uiso 1 1 calc R . . H52C H 0.2308 0.1145 0.2795 0.060 Uiso 1 1 calc R . . C53 C 0.4827(3) 0.0786(2) 0.30123(16) 0.0270(10) Uani 1 1 d . . . H53A H 0.4301 0.0827 0.3316 0.032 Uiso 1 1 calc R . . H53B H 0.5010 0.0359 0.2986 0.032 Uiso 1 1 calc R . . C54 C 0.5797(3) 0.1138(2) 0.31931(19) 0.0389(12) Uani 1 1 d . . . H54A H 0.6308 0.1125 0.2885 0.058 Uiso 1 1 calc R . . H54B H 0.6091 0.0960 0.3540 0.058 Uiso 1 1 calc R . . H54C H 0.5609 0.1553 0.3270 0.058 Uiso 1 1 calc R . . C55 C 0.5090(3) 0.0873(2) 0.19261(17) 0.0275(10) Uani 1 1 d . . . H55A H 0.5728 0.1104 0.1996 0.033 Uiso 1 1 calc R . . H55B H 0.4768 0.1032 0.1574 0.033 Uiso 1 1 calc R . . C56 C 0.5395(4) 0.0213(2) 0.1815(2) 0.0424(12) Uani 1 1 d . . . H56A H 0.5692 0.0042 0.2165 0.064 Uiso 1 1 calc R . . H56B H 0.5905 0.0195 0.1507 0.064 Uiso 1 1 calc R . . H56C H 0.4781 -0.0015 0.1706 0.064 Uiso 1 1 calc R . . C57 C 0.3755(5) 0.2041(3) 0.4205(2) 0.0568(16) Uani 1 1 d . . . H57A H 0.4101 0.2227 0.4537 0.068 Uiso 1 1 calc R . . H57B H 0.4065 0.1645 0.4137 0.068 Uiso 1 1 calc R . . C58 C 0.2581(5) 0.1982(2) 0.4317(3) 0.0556(15) Uani 1 1 d . . . H58A H 0.2300 0.1619 0.4134 0.067 Uiso 1 1 calc R . . H58B H 0.2432 0.1969 0.4732 0.067 Uiso 1 1 calc R . . C59 C 0.2146(6) 0.2523(4) 0.4054(3) 0.101(3) Uani 1 1 d . . . H59A H 0.2045 0.2837 0.4345 0.121 Uiso 1 1 calc R . . H59B H 0.1473 0.2435 0.3873 0.121 Uiso 1 1 calc R . . C60 C 0.2921(5) 0.2721(3) 0.3609(2) 0.0551(15) Uani 1 1 d . . . H60A H 0.2659 0.2632 0.3221 0.066 Uiso 1 1 calc R . . H60B H 0.3036 0.3156 0.3638 0.066 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 Pu1 0.01075(5) 0.01173(6) 0.01125(5) -0.00005(5) -0.00001(5) -0.00066(5) Se1 0.0236(2) 0.0167(2) 0.01795(19) 0.00197(16) -0.00675(16) -0.00453(17) Se2 0.01900(18) 0.01496(19) 0.01627(18) 0.00118(15) -0.00344(14) -0.00242(14) Se3 0.01396(18) 0.0182(2) 0.01655(19) -0.00219(15) 0.00013(14) -0.00174(15) Se4 0.01551(18) 0.0237(2) 0.02247(19) -0.00843(16) 0.00281(15) -0.00289(16) Se5 0.0239(2) 0.01635(19) 0.02208(18) 0.00316(15) -0.01045(18) -0.00668(18) Se6 0.01689(17) 0.01268(18) 0.01798(18) 0.00165(15) -0.00425(14) -0.00175(13) Se7 0.01766(18) 0.0194(2) 0.01845(17) -0.00583(15) 0.00352(17) -0.00394(18) Se8 0.01552(17) 0.0207(2) 0.02378(18) -0.00459(18) 0.00367(15) -0.00326(17) P1 0.0177(5) 0.0140(5) 0.0145(4) 0.0015(4) -0.0010(4) -0.0020(4) P2 0.0120(4) 0.0213(5) 0.0162(4) -0.0008(4) 0.0015(3) -0.0010(4) P3 0.0143(4) 0.0134(5) 0.0148(4) 0.0006(3) -0.0027(4) -0.0007(4) P4 0.0159(5) 0.0164(5) 0.0159(5) -0.0005(4) 0.0019(4) 0.0011(4) N1 0.0225(17) 0.0199(17) 0.0178(15) 0.0002(13) -0.0016(14) 0.0007(15) O1 0.050(2) 0.076(3) 0.041(2) 0.005(2) -0.0016(18) 0.004(2) C1 0.020(2) 0.016(2) 0.0177(19) 0.0008(15) 0.0009(16) -0.0035(16) C2 0.025(2) 0.023(2) 0.035(2) 0.0110(18) 0.0057(18) 0.0042(18) C3 0.026(2) 0.031(3) 0.035(2) 0.008(2) 0.0121(19) 0.003(2) C4 0.035(3) 0.031(3) 0.022(2) 0.0014(19) 0.0040(19) -0.010(2) C5 0.051(3) 0.018(2) 0.029(2) 0.0075(17) 0.007(2) -0.003(2) C6 0.037(3) 0.017(2) 0.024(2) 0.0002(17) 0.0070(19) 0.0054(19) C7 0.021(2) 0.019(2) 0.0170(19) 0.0022(16) -0.0027(16) 0.0032(16) C8 0.030(2) 0.022(2) 0.029(2) -0.0048(18) -0.0014(19) 0.0028(18) C9 0.049(3) 0.028(2) 0.030(2) -0.005(2) 0.004(2) 0.009(2) C10 0.046(3) 0.035(3) 0.039(3) 0.002(2) 0.004(2) 0.025(2) C11 0.031(3) 0.048(3) 0.049(3) -0.001(3) -0.008(2) 0.013(2) C12 0.033(3) 0.031(3) 0.043(3) -0.004(2) -0.010(2) 0.005(2) C13 0.0205(18) 0.028(2) 0.0155(16) -0.0044(16) 0.0053(16) 0.005(2) C14 0.031(2) 0.025(2) 0.051(3) -0.008(2) -0.007(2) 0.004(2) C15 0.042(3) 0.029(3) 0.070(4) -0.002(3) -0.018(3) 0.012(2) C16 0.025(2) 0.061(3) 0.031(3) -0.012(3) -0.005(2) 0.023(2) C17 0.018(2) 0.062(4) 0.022(2) 0.000(2) -0.0041(16) -0.003(2) C18 0.018(2) 0.045(3) 0.0190(18) 0.0031(19) -0.0005(15) -0.0020(19) C19 0.0093(17) 0.034(2) 0.0175(19) 0.0036(17) -0.0009(14) -0.0040(16) C20 0.0131(18) 0.036(3) 0.027(2) 0.0083(19) 0.0030(16) 0.0027(18) C21 0.019(2) 0.045(3) 0.044(3) 0.026(2) -0.002(2) -0.003(2) C22 0.021(2) 0.074(4) 0.023(2) 0.024(2) -0.0045(18) -0.016(2) C23 0.029(3) 0.080(4) 0.016(2) -0.003(2) 0.0055(18) -0.020(3) C24 0.022(2) 0.050(3) 0.022(2) -0.003(2) 0.0049(17) -0.012(2) C25 0.0194(19) 0.015(2) 0.0180(18) 0.0027(15) 0.0002(15) -0.0018(15) C26 0.019(2) 0.023(2) 0.025(2) -0.0052(17) 0.0011(16) 0.0001(16) C27 0.023(2) 0.029(2) 0.034(2) -0.010(2) 0.0077(19) -0.0076(19) C28 0.050(3) 0.033(3) 0.029(2) -0.003(2) 0.011(2) -0.010(3) C29 0.039(3) 0.055(3) 0.019(2) 0.007(2) -0.003(2) 0.008(3) C30 0.023(2) 0.038(3) 0.023(2) 0.0051(19) -0.0012(17) 0.0052(19) C31 0.0186(18) 0.019(2) 0.0068(17) 0.0007(14) -0.0004(14) 0.0015(15) C32 0.023(2) 0.0139(19) 0.0211(19) -0.0002(15) -0.0035(16) 0.0003(16) C33 0.018(2) 0.022(2) 0.029(2) 0.0039(17) 0.0013(16) 0.0013(17) C34 0.024(2) 0.020(2) 0.028(2) -0.0002(18) 0.0008(18) 0.0078(17) C35 0.033(2) 0.019(2) 0.025(2) 0.0001(18) -0.0032(19) 0.0015(17) C36 0.021(2) 0.018(2) 0.026(2) -0.0005(17) -0.0008(17) -0.0028(16) C37 0.0180(19) 0.016(2) 0.0179(19) 0.0032(15) 0.0024(15) -0.0001(16) C38 0.039(3) 0.026(2) 0.021(2) 0.0010(18) 0.0009(19) 0.009(2) C39 0.037(3) 0.035(3) 0.038(3) 0.011(2) -0.008(2) 0.007(2) C40 0.024(2) 0.020(2) 0.056(3) 0.006(2) 0.008(2) 0.0050(19) C41 0.025(2) 0.016(2) 0.040(3) -0.0005(19) 0.009(2) -0.0002(18) C42 0.018(2) 0.021(2) 0.026(2) 0.0031(17) 0.0011(17) 0.0024(17) C43 0.024(2) 0.019(2) 0.020(2) 0.0011(17) 0.0057(16) 0.0104(17) C44 0.031(2) 0.030(3) 0.029(2) 0.0052(19) 0.0106(18) 0.005(2) C45 0.049(3) 0.035(3) 0.038(3) 0.015(2) 0.025(2) 0.008(3) C46 0.071(4) 0.034(3) 0.023(2) 0.012(2) 0.012(2) 0.020(3) C47 0.062(3) 0.037(3) 0.022(2) -0.0006(19) -0.002(3) 0.019(3) C48 0.040(3) 0.023(2) 0.026(2) 0.0021(17) 0.000(2) 0.006(2) C49 0.034(2) 0.022(2) 0.027(2) -0.0022(18) -0.0054(18) 0.0017(18) C50 0.044(3) 0.026(3) 0.047(3) 0.003(2) -0.012(2) 0.007(2) C51 0.033(2) 0.032(3) 0.029(2) -0.001(2) -0.0023(19) -0.005(2) C52 0.029(3) 0.055(4) 0.037(3) 0.000(2) 0.001(2) -0.015(2) C53 0.034(2) 0.029(2) 0.018(2) 0.0043(18) -0.0072(17) 0.0004(19) C54 0.037(3) 0.046(3) 0.034(2) 0.011(2) -0.012(2) -0.002(2) C55 0.031(2) 0.034(3) 0.018(2) -0.0024(18) 0.0042(17) -0.002(2) C56 0.045(3) 0.034(3) 0.048(3) -0.010(2) 0.012(2) 0.004(3) C57 0.067(4) 0.076(4) 0.027(3) 0.003(3) 0.002(3) 0.019(3) C58 0.074(4) 0.038(3) 0.055(4) 0.006(3) 0.001(3) 0.006(3) C59 0.084(5) 0.133(7) 0.085(5) 0.065(5) 0.043(4) 0.067(5) C60 0.077(4) 0.048(4) 0.040(3) 0.010(3) -0.003(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pu1 Se4 2.9815(4) . ? Pu1 Se8 2.9990(4) . ? Pu1 Se5 3.0138(4) . ? Pu1 Se1 3.0288(4) . ? Pu1 Se6 3.0945(4) . ? Pu1 Se7 3.1050(4) . ? Pu1 Se3 3.1058(4) . ? Pu1 Se2 3.1160(5) . ? Se1 P1 2.1661(10) . ? Se2 P1 2.1597(10) . ? Se3 P2 2.1587(10) . ? Se4 P2 2.1579(10) . ? Se5 P3 2.1507(10) . ? Se6 P3 2.1590(10) . ? Se7 P4 2.1547(10) . ? Se8 P4 2.1504(11) . ? P1 C7 1.819(4) . ? P1 C1 1.820(4) . ? P2 C19 1.811(4) . ? P2 C13 1.817(4) . ? P3 C25 1.822(4) . ? P3 C31 1.820(4) . ? P4 C43 1.820(4) . ? P4 C37 1.832(4) . ? N1 C55 1.525(5) . ? N1 C51 1.510(5) . ? N1 C49 1.516(5) . ? N1 C53 1.520(4) . ? O1 C60 1.399(6) . ? O1 C57 1.407(6) . ? C1 C6 1.378(5) . ? C1 C2 1.392(5) . ? C2 C3 1.389(5) . ? C3 C4 1.392(6) . ? C4 C5 1.371(6) . ? C5 C6 1.394(5) . ? C7 C12 1.377(6) . ? C7 C8 1.396(5) . ? C8 C9 1.393(6) . ? C9 C10 1.377(6) . ? C10 C11 1.365(7) . ? C11 C12 1.376(6) . ? C13 C14 1.384(6) . ? C13 C18 1.384(5) . ? C14 C15 1.387(6) . ? C15 C16 1.379(7) . ? C16 C17 1.370(7) . ? C17 C18 1.382(6) . ? C19 C24 1.384(5) . ? C19 C20 1.395(6) . ? C20 C21 1.395(5) . ? C21 C22 1.364(7) . ? C22 C23 1.375(7) . ? C23 C24 1.399(6) . ? C25 C30 1.383(5) . ? C25 C26 1.407(5) . ? C26 C27 1.376(5) . ? C27 C28 1.383(6) . ? C28 C29 1.385(7) . ? C29 C30 1.392(5) . ? C31 C32 1.386(5) . ? C31 C36 1.393(5) . ? C32 C33 1.380(5) . ? C33 C34 1.389(5) . ? C34 C35 1.376(5) . ? C35 C36 1.397(5) . ? C37 C38 1.387(5) . ? C37 C42 1.390(5) . ? C38 C39 1.390(6) . ? C39 C40 1.392(6) . ? C40 C41 1.369(6) . ? C41 C42 1.389(5) . ? C43 C44 1.399(6) . ? C43 C48 1.394(6) . ? C44 C45 1.373(5) . ? C45 C46 1.380(7) . ? C46 C47 1.383(7) . ? C47 C48 1.396(5) . ? C49 C50 1.512(6) . ? C51 C52 1.513(6) . ? C53 C54 1.514(6) . ? C55 C56 1.523(6) . ? C57 C58 1.519(8) . ? C58 C59 1.443(7) . ? C59 C60 1.482(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 Se4 Pu1 Se8 147.360(12) . . ? Se4 Pu1 Se5 92.829(13) . . ? Se8 Pu1 Se5 104.696(12) . . ? Se4 Pu1 Se1 88.036(13) . . ? Se8 Pu1 Se1 90.724(12) . . ? Se5 Pu1 Se1 148.507(11) . . ? Se4 Pu1 Se6 79.323(12) . . ? Se8 Pu1 Se6 80.574(13) . . ? Se5 Pu1 Se6 71.275(11) . . ? Se1 Pu1 Se6 139.349(11) . . ? Se4 Pu1 Se7 141.101(12) . . ? Se8 Pu1 Se7 70.948(11) . . ? Se5 Pu1 Se7 75.691(13) . . ? Se1 Pu1 Se7 83.999(13) . . ? Se6 Pu1 Se7 128.541(11) . . ? Se4 Pu1 Se3 72.239(11) . . ? Se8 Pu1 Se3 138.833(11) . . ? Se5 Pu1 Se3 73.679(11) . . ? Se1 Pu1 Se3 76.667(11) . . ? Se6 Pu1 Se3 133.080(10) . . ? Se7 Pu1 Se3 68.872(11) . . ? Se4 Pu1 Se2 75.400(11) . . ? Se8 Pu1 Se2 73.330(11) . . ? Se5 Pu1 Se2 139.066(11) . . ? Se1 Pu1 Se2 71.383(11) . . ? Se6 Pu1 Se2 68.067(10) . . ? Se7 Pu1 Se2 135.900(11) . . ? Se3 Pu1 Se2 134.729(11) . . ? P1 Se1 Pu1 89.39(3) . . ? P1 Se2 Pu1 87.25(3) . . ? P2 Se3 Pu1 85.73(3) . . ? P2 Se4 Pu1 88.93(3) . . ? P3 Se5 Pu1 89.64(3) . . ? P3 Se6 Pu1 87.39(3) . . ? P4 Se7 Pu1 87.70(3) . . ? P4 Se8 Pu1 90.57(3) . . ? C7 P1 C1 104.40(17) . . ? C7 P1 Se2 110.65(12) . . ? C1 P1 Se2 109.94(12) . . ? C7 P1 Se1 110.77(13) . . ? C1 P1 Se1 108.82(12) . . ? Se2 P1 Se1 111.97(4) . . ? C19 P2 C13 104.91(16) . . ? C19 P2 Se4 108.14(12) . . ? C13 P2 Se4 110.71(14) . . ? C19 P2 Se3 111.72(14) . . ? C13 P2 Se3 108.57(11) . . ? Se4 P2 Se3 112.53(4) . . ? C25 P3 C31 104.35(16) . . ? C25 P3 Se5 108.68(12) . . ? C31 P3 Se5 110.70(12) . . ? C25 P3 Se6 110.28(13) . . ? C31 P3 Se6 111.21(12) . . ? Se5 P3 Se6 111.37(4) . . ? C43 P4 C37 102.82(17) . . ? C43 P4 Se8 110.22(14) . . ? C37 P4 Se8 108.43(13) . . ? C43 P4 Se7 111.25(13) . . ? C37 P4 Se7 113.05(12) . . ? Se8 P4 Se7 110.79(4) . . ? C55 N1 C51 109.0(3) . . ? C55 N1 C49 107.5(3) . . ? C51 N1 C49 111.2(3) . . ? C55 N1 C53 111.5(3) . . ? C51 N1 C53 108.9(3) . . ? C49 N1 C53 108.8(3) . . ? C60 O1 C57 109.0(4) . . ? C6 C1 C2 118.9(4) . . ? C6 C1 P1 124.6(3) . . ? C2 C1 P1 116.5(3) . . ? C3 C2 C1 121.0(4) . . ? C4 C3 C2 119.7(4) . . ? C5 C4 C3 119.1(4) . . ? C4 C5 C6 121.3(4) . . ? C1 C6 C5 120.0(4) . . ? C12 C7 C8 118.3(4) . . ? C12 C7 P1 121.9(3) . . ? C8 C7 P1 119.8(3) . . ? C7 C8 C9 119.9(4) . . ? C10 C9 C8 120.0(4) . . ? C11 C10 C9 120.2(4) . . ? C10 C11 C12 120.0(5) . . ? C11 C12 C7 121.5(4) . . ? C14 C13 C18 118.6(4) . . ? C14 C13 P2 121.7(3) . . ? C18 C13 P2 119.6(3) . . ? C13 C14 C15 120.2(5) . . ? C16 C15 C14 120.3(4) . . ? C17 C16 C15 119.7(4) . . ? C16 C17 C18 120.0(4) . . ? C17 C18 C13 121.0(4) . . ? C24 C19 C20 119.7(4) . . ? C24 C19 P2 117.7(3) . . ? C20 C19 P2 122.4(3) . . ? C21 C20 C19 119.3(4) . . ? C22 C21 C20 120.8(5) . . ? C23 C22 C21 120.4(4) . . ? C22 C23 C24 120.0(4) . . ? C19 C24 C23 120.0(4) . . ? C30 C25 C26 119.2(3) . . ? C30 C25 P3 121.8(3) . . ? C26 C25 P3 119.0(3) . . ? C27 C26 C25 120.0(4) . . ? C28 C27 C26 120.3(4) . . ? C27 C28 C29 120.3(4) . . ? C28 C29 C30 119.5(4) . . ? C25 C30 C29 120.6(4) . . ? C32 C31 C36 119.0(3) . . ? C32 C31 P3 121.6(3) . . ? C36 C31 P3 119.4(3) . . ? C33 C32 C31 120.6(4) . . ? C32 C33 C34 120.4(4) . . ? C35 C34 C33 119.6(4) . . ? C34 C35 C36 120.1(4) . . ? C31 C36 C35 120.2(3) . . ? C38 C37 C42 118.8(4) . . ? C38 C37 P4 119.3(3) . . ? C42 C37 P4 121.9(3) . . ? C39 C38 C37 120.8(4) . . ? C38 C39 C40 119.8(4) . . ? C41 C40 C39 119.5(4) . . ? C40 C41 C42 120.9(4) . . ? C41 C42 C37 120.2(4) . . ? C44 C43 C48 119.0(4) . . ? C44 C43 P4 120.0(3) . . ? C48 C43 P4 121.0(3) . . ? C45 C44 C43 120.7(4) . . ? C46 C45 C44 119.8(4) . . ? C45 C46 C47 120.9(4) . . ? C46 C47 C48 119.4(5) . . ? C47 C48 C43 120.2(4) . . ? C50 C49 N1 115.8(3) . . ? N1 C51 C52 115.9(3) . . ? C54 C53 N1 115.1(3) . . ? N1 C55 C56 115.7(3) . . ? O1 C57 C58 106.5(4) . . ? C59 C58 C57 103.6(5) . . ? C58 C59 C60 106.0(5) . . ? O1 C60 C59 108.4(4) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.376 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.121 data_apx088 _database_code_depnum_ccdc_archive 'CCDC 906773' #TrackingRef 'web_deposit_cif_file_7_AndrewGaunt_1350598115.cif for 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 P4 Se8 U' _chemical_formula_weight 1610.39 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.8131(6) _cell_length_b 9.7933(5) _cell_length_c 18.8547(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.5970(10) _cell_angle_gamma 90.00 _cell_volume 2549.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 9.052 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1488 _exptl_absorpt_correction_T_max 0.5312 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28707 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.94 _reflns_number_total 12148 _reflns_number_gt 10725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _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^)+(0.0240P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(3) _refine_ls_number_reflns 12148 _refine_ls_number_parameters 550 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0474 _refine_ls_wR_factor_gt 0.0463 _refine_ls_goodness_of_fit_ref 0.659 _refine_ls_restrained_S_all 0.659 _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 U1 U 0.818389(9) 0.133003(14) 0.256448(7) 0.01282(3) Uani 1 1 d . . . Se1 Se 0.99450(3) -0.04611(4) 0.23813(2) 0.01752(9) Uani 1 1 d . . . Se2 Se 0.96824(3) 0.30134(4) 0.19665(2) 0.01758(9) Uani 1 1 d . . . Se3 Se 0.78843(3) 0.43176(4) 0.29131(2) 0.01778(9) Uani 1 1 d . . . Se4 Se 0.89456(3) 0.17435(4) 0.39867(2) 0.01761(9) Uani 1 1 d . . . Se5 Se 0.62256(3) 0.13207(5) 0.30900(2) 0.01902(8) Uani 1 1 d . . . Se6 Se 0.80028(3) -0.12950(4) 0.34214(2) 0.01658(9) Uani 1 1 d . . . Se7 Se 0.75205(3) -0.07444(4) 0.15338(2) 0.02099(9) Uani 1 1 d . . . Se8 Se 0.70068(3) 0.27869(4) 0.14168(2) 0.01870(9) Uani 1 1 d . . . P1 P 1.05963(7) 0.12365(12) 0.18388(5) 0.01508(19) Uani 1 1 d . . . P2 P 0.87808(8) 0.39408(11) 0.38535(5) 0.0159(2) Uani 1 1 d . . . P3 P 0.65117(7) -0.06916(11) 0.35354(5) 0.0148(2) Uani 1 1 d . . . P4 P 0.67824(8) 0.08208(11) 0.09165(5) 0.0165(2) Uani 1 1 d . . . C1 C 1.1801(3) 0.1662(4) 0.21817(19) 0.0136(8) Uani 1 1 d . . . C2 C 1.1941(3) 0.2752(5) 0.2646(2) 0.0182(9) Uani 1 1 d . . . H2 H 1.1411 0.3236 0.2807 0.022 Uiso 1 1 calc R . . C3 C 1.2867(3) 0.3116(4) 0.2867(2) 0.0202(9) Uani 1 1 d . . . H3 H 1.2957 0.3844 0.3179 0.024 Uiso 1 1 calc R . . C4 C 1.3657(3) 0.2408(4) 0.2631(2) 0.0190(9) Uani 1 1 d . . . H4 H 1.4279 0.2676 0.2772 0.023 Uiso 1 1 calc R . . C5 C 1.3526(3) 0.1299(5) 0.21848(19) 0.0214(8) Uani 1 1 d . . . H5 H 1.4060 0.0808 0.2036 0.026 Uiso 1 1 calc R . . C6 C 1.2601(3) 0.0915(4) 0.1958(2) 0.0192(9) Uani 1 1 d . . . H6 H 1.2513 0.0166 0.1660 0.023 Uiso 1 1 calc R . . C7 C 1.0753(3) 0.0888(4) 0.0904(2) 0.0161(9) Uani 1 1 d . . . C8 C 1.1306(3) 0.1796(4) 0.0517(2) 0.0191(9) Uani 1 1 d . . . H8 H 1.1623 0.2517 0.0746 0.023 Uiso 1 1 calc R . . C9 C 1.1385(3) 0.1626(4) -0.0212(2) 0.0199(9) Uani 1 1 d . . . H9 H 1.1744 0.2242 -0.0472 0.024 Uiso 1 1 calc R . . C10 C 1.0935(3) 0.0550(5) -0.0545(2) 0.0261(10) Uani 1 1 d . . . H10 H 1.1006 0.0419 -0.1029 0.031 Uiso 1 1 calc R . . C11 C 1.0375(3) -0.0343(5) -0.0165(2) 0.0277(10) Uani 1 1 d . . . H11 H 1.0059 -0.1061 -0.0398 0.033 Uiso 1 1 calc R . . C12 C 1.0279(3) -0.0181(4) 0.0557(2) 0.0221(10) Uani 1 1 d . . . H12 H 0.9898 -0.0783 0.0810 0.026 Uiso 1 1 calc R . . C13 C 0.9949(3) 0.4790(4) 0.3840(2) 0.0159(8) Uani 1 1 d . . . C14 C 1.0718(3) 0.4231(4) 0.4243(2) 0.0199(9) Uani 1 1 d . . . H14 H 1.0639 0.3407 0.4479 0.024 Uiso 1 1 calc R . . C15 C 1.1600(3) 0.4917(5) 0.4287(2) 0.0239(10) Uani 1 1 d . . . H15 H 1.2116 0.4551 0.4552 0.029 Uiso 1 1 calc R . . C16 C 1.1707(3) 0.6143(5) 0.3937(2) 0.0272(10) Uani 1 1 d . . . H16 H 1.2290 0.6614 0.3973 0.033 Uiso 1 1 calc R . . C17 C 1.0953(3) 0.6666(5) 0.3535(3) 0.0377(13) Uani 1 1 d . . . H17 H 1.1033 0.7483 0.3292 0.045 Uiso 1 1 calc R . . C18 C 1.0077(3) 0.5992(4) 0.3485(2) 0.0266(11) Uani 1 1 d . . . H18 H 0.9571 0.6356 0.3210 0.032 Uiso 1 1 calc R . . C19 C 0.8194(3) 0.4549(4) 0.4643(2) 0.0170(8) Uani 1 1 d . . . C20 C 0.8722(3) 0.5141(5) 0.5198(2) 0.0249(10) Uani 1 1 d . . . H20 H 0.9376 0.5333 0.5146 0.030 Uiso 1 1 calc R . . C21 C 0.8277(3) 0.5449(5) 0.5829(2) 0.0298(11) Uani 1 1 d . . . H21 H 0.8630 0.5850 0.6201 0.036 Uiso 1 1 calc R . . C22 C 0.7304(3) 0.5153(5) 0.5901(2) 0.0297(11) Uani 1 1 d . . . H22 H 0.7009 0.5340 0.6328 0.036 Uiso 1 1 calc R . . C23 C 0.6765(3) 0.4581(5) 0.5346(2) 0.0230(9) Uani 1 1 d . . . H23 H 0.6111 0.4397 0.5397 0.028 Uiso 1 1 calc R . . C24 C 0.7205(3) 0.4286(4) 0.4714(2) 0.0199(9) Uani 1 1 d . . . H24 H 0.6845 0.3914 0.4338 0.024 Uiso 1 1 calc R . . C25 C 0.6166(3) -0.0681(4) 0.4457(2) 0.0155(8) Uani 1 1 d . . . C26 C 0.6056(3) 0.0533(5) 0.4822(2) 0.0215(9) Uani 1 1 d . . . H26 H 0.6205 0.1358 0.4607 0.026 Uiso 1 1 calc R . . C27 C 0.5723(3) 0.0520(5) 0.5510(2) 0.0262(10) Uani 1 1 d . . . H27 H 0.5634 0.1338 0.5751 0.031 Uiso 1 1 calc R . . C28 C 0.5523(3) -0.0695(5) 0.5837(2) 0.0245(10) Uani 1 1 d . . . H28 H 0.5285 -0.0696 0.6293 0.029 Uiso 1 1 calc R . . C29 C 0.5674(3) -0.1915(5) 0.5493(2) 0.0251(10) Uani 1 1 d . . . H29 H 0.5558 -0.2738 0.5721 0.030 Uiso 1 1 calc R . . C30 C 0.6000(3) -0.1907(4) 0.4802(2) 0.0214(9) Uani 1 1 d . . . H30 H 0.6108 -0.2728 0.4569 0.026 Uiso 1 1 calc R . . C31 C 0.5680(3) -0.1890(4) 0.3102(2) 0.0162(8) Uani 1 1 d . . . C32 C 0.6003(3) -0.3069(4) 0.2785(2) 0.0270(10) Uani 1 1 d . . . H32 H 0.6660 -0.3276 0.2797 0.032 Uiso 1 1 calc R . . C33 C 0.5350(4) -0.3941(5) 0.2451(3) 0.0350(12) Uani 1 1 d . . . H33 H 0.5571 -0.4737 0.2241 0.042 Uiso 1 1 calc R . . C34 C 0.4384(3) -0.3645(6) 0.2428(2) 0.0340(11) Uani 1 1 d . . . H34 H 0.3949 -0.4233 0.2198 0.041 Uiso 1 1 calc R . . C35 C 0.4052(3) -0.2467(5) 0.2747(2) 0.0284(11) Uani 1 1 d . . . H35 H 0.3393 -0.2268 0.2737 0.034 Uiso 1 1 calc R . . C36 C 0.4700(3) -0.1590(5) 0.3081(2) 0.0225(9) Uani 1 1 d . . . H36 H 0.4478 -0.0796 0.3293 0.027 Uiso 1 1 calc R . . C37 C 0.5506(3) 0.0396(4) 0.0777(2) 0.0158(8) Uani 1 1 d . . . C38 C 0.4939(3) 0.1281(5) 0.0363(2) 0.0238(9) Uani 1 1 d . . . H38 H 0.5195 0.2104 0.0209 0.029 Uiso 1 1 calc R . . C39 C 0.3996(3) 0.0932(5) 0.0181(2) 0.0277(11) Uani 1 1 d . . . H39 H 0.3621 0.1519 -0.0100 0.033 Uiso 1 1 calc R . . C40 C 0.3606(3) -0.0273(5) 0.0411(2) 0.0274(10) Uani 1 1 d . . . H40 H 0.2974 -0.0510 0.0281 0.033 Uiso 1 1 calc R . . C41 C 0.4162(3) -0.1135(4) 0.0840(2) 0.0256(10) Uani 1 1 d . . . H41 H 0.3894 -0.1942 0.1005 0.031 Uiso 1 1 calc R . . C42 C 0.5113(3) -0.0810(4) 0.1028(2) 0.0203(9) Uani 1 1 d . . . H42 H 0.5482 -0.1391 0.1317 0.024 Uiso 1 1 calc R . . C43 C 0.7248(3) 0.0824(4) 0.0026(2) 0.0212(9) Uani 1 1 d . . . C44 C 0.7983(3) 0.1696(5) -0.0166(2) 0.0247(10) Uani 1 1 d . . . H44 H 0.8229 0.2333 0.0158 0.030 Uiso 1 1 calc R . . C45 C 0.8357(3) 0.1617(5) -0.0846(2) 0.0328(12) Uani 1 1 d . . . H45 H 0.8837 0.2225 -0.0979 0.039 Uiso 1 1 calc R . . C46 C 0.8021(3) 0.0649(5) -0.1319(2) 0.0298(11) Uani 1 1 d . . . H46 H 0.8283 0.0589 -0.1767 0.036 Uiso 1 1 calc R . . C47 C 0.7298(3) -0.0231(5) -0.1130(2) 0.0246(10) Uani 1 1 d . . . H47 H 0.7072 -0.0884 -0.1453 0.029 Uiso 1 1 calc R . . C48 C 0.6899(3) -0.0157(4) -0.0462(2) 0.0209(9) Uani 1 1 d . . . H48 H 0.6406 -0.0751 -0.0338 0.025 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 U1 0.01234(6) 0.01510(7) 0.01099(6) -0.00057(6) -0.00047(5) 0.00135(7) Se1 0.0160(2) 0.0180(2) 0.0188(2) 0.00451(17) 0.00385(16) 0.00292(16) Se2 0.0168(2) 0.0170(2) 0.0190(2) 0.00283(16) 0.00253(16) 0.00210(16) Se3 0.0195(2) 0.0170(2) 0.0166(2) -0.00221(17) -0.00454(16) 0.00394(16) Se4 0.0226(2) 0.0169(2) 0.01309(19) -0.00039(15) -0.00346(16) 0.00184(15) Se5 0.01432(17) 0.01735(19) 0.0255(2) 0.0056(2) 0.00277(15) 0.0030(2) Se6 0.0135(2) 0.0173(2) 0.0190(2) 0.00218(16) 0.00110(16) 0.00182(16) Se7 0.0266(2) 0.0185(2) 0.0175(2) -0.00376(17) -0.00735(17) 0.00659(18) Se8 0.0230(2) 0.0180(2) 0.0148(2) -0.00102(16) -0.00516(16) 0.00241(17) P1 0.0145(4) 0.0176(5) 0.0132(4) 0.0015(5) 0.0015(4) 0.0013(5) P2 0.0164(5) 0.0165(6) 0.0148(5) -0.0021(4) -0.0007(4) 0.0013(4) P3 0.0134(5) 0.0146(5) 0.0163(5) 0.0014(4) 0.0005(4) -0.0002(4) P4 0.0179(5) 0.0195(5) 0.0120(5) -0.0013(4) -0.0018(4) 0.0033(4) C1 0.0159(19) 0.016(2) 0.0092(16) 0.0027(14) -0.0007(14) -0.0003(14) C2 0.017(2) 0.025(2) 0.013(2) 0.0010(17) 0.0034(15) 0.0041(17) C3 0.020(2) 0.025(2) 0.015(2) -0.0036(17) -0.0026(17) 0.0004(18) C4 0.016(2) 0.027(2) 0.014(2) 0.0033(17) -0.0012(16) -0.0019(17) C5 0.0151(18) 0.031(2) 0.0184(18) 0.001(2) -0.0009(15) 0.005(2) C6 0.019(2) 0.021(2) 0.017(2) 0.0001(16) -0.0002(17) 0.0044(16) C7 0.015(2) 0.022(2) 0.0109(19) 0.0019(15) 0.0011(16) 0.0051(15) C8 0.018(2) 0.021(2) 0.019(2) 0.0001(16) 0.0003(17) -0.0032(16) C9 0.022(2) 0.021(2) 0.0172(19) 0.0062(16) 0.0033(16) -0.0022(17) C10 0.028(2) 0.039(3) 0.012(2) -0.005(2) 0.0020(18) 0.004(2) C11 0.031(3) 0.032(3) 0.020(2) -0.004(2) 0.0000(19) -0.008(2) C12 0.024(2) 0.023(2) 0.020(2) -0.0008(18) 0.0038(18) -0.0042(18) C13 0.017(2) 0.018(2) 0.0130(19) -0.0036(16) 0.0030(16) 0.0015(16) C14 0.023(2) 0.020(2) 0.017(2) 0.0004(17) -0.0004(17) -0.0007(18) C15 0.018(2) 0.034(3) 0.020(2) -0.0014(19) -0.0011(18) 0.0026(19) C16 0.020(2) 0.028(3) 0.033(2) -0.001(2) -0.0044(18) -0.007(2) C17 0.030(3) 0.028(3) 0.054(3) 0.021(2) -0.005(2) -0.003(2) C18 0.020(2) 0.028(3) 0.032(2) 0.0094(19) -0.0095(19) -0.0007(17) C19 0.017(2) 0.020(2) 0.0140(19) -0.0025(17) 0.0004(16) -0.0008(17) C20 0.016(2) 0.036(3) 0.024(2) -0.008(2) 0.0042(18) -0.0024(19) C21 0.025(2) 0.040(3) 0.024(2) -0.015(2) 0.0030(19) -0.009(2) C22 0.032(3) 0.037(3) 0.021(2) -0.007(2) 0.009(2) 0.001(2) C23 0.015(2) 0.026(2) 0.028(2) -0.002(2) 0.0041(17) -0.0002(18) C24 0.019(2) 0.021(2) 0.020(2) -0.0034(18) -0.0019(16) -0.0060(18) C25 0.0095(18) 0.022(2) 0.0146(19) -0.0002(17) -0.0042(14) -0.0005(16) C26 0.021(2) 0.021(2) 0.022(2) 0.0038(18) -0.0031(18) 0.0007(18) C27 0.025(2) 0.031(3) 0.021(2) -0.009(2) -0.0029(19) 0.010(2) C28 0.020(2) 0.038(3) 0.016(2) -0.003(2) -0.0005(17) 0.002(2) C29 0.026(2) 0.027(3) 0.022(2) 0.0050(19) -0.0010(19) -0.0047(19) C30 0.025(2) 0.015(2) 0.024(2) -0.0008(18) 0.0002(18) -0.0020(17) C31 0.017(2) 0.017(2) 0.015(2) 0.0023(16) -0.0034(16) -0.0014(16) C32 0.022(2) 0.022(2) 0.036(3) -0.004(2) -0.006(2) -0.0024(19) C33 0.044(3) 0.020(3) 0.040(3) -0.008(2) -0.011(2) -0.003(2) C34 0.040(3) 0.033(3) 0.028(2) 0.010(3) -0.015(2) -0.019(3) C35 0.018(2) 0.038(3) 0.029(3) 0.008(2) -0.0054(19) -0.007(2) C36 0.020(2) 0.030(2) 0.017(2) 0.0019(18) -0.0013(17) -0.0028(18) C37 0.017(2) 0.019(2) 0.0112(19) -0.0056(16) -0.0001(15) 0.0040(16) C38 0.0193(19) 0.026(2) 0.026(2) 0.009(2) -0.0024(16) -0.001(2) C39 0.021(2) 0.029(3) 0.033(3) 0.0027(19) -0.004(2) 0.0034(18) C40 0.019(2) 0.039(3) 0.024(2) -0.010(2) 0.0018(18) 0.000(2) C41 0.031(3) 0.020(2) 0.027(2) -0.0044(18) 0.004(2) -0.0051(19) C42 0.028(2) 0.020(2) 0.013(2) -0.0032(17) 0.0025(17) 0.0044(18) C43 0.021(2) 0.027(2) 0.015(2) -0.0014(17) -0.0029(17) 0.0080(18) C44 0.019(2) 0.032(3) 0.023(2) -0.0036(18) 0.0008(17) 0.0032(18) C45 0.026(2) 0.038(3) 0.035(3) 0.001(2) 0.013(2) 0.002(2) C46 0.032(3) 0.039(3) 0.019(2) 0.001(2) 0.004(2) 0.014(2) C47 0.032(3) 0.028(2) 0.014(2) -0.0034(18) -0.0034(18) 0.015(2) C48 0.025(2) 0.019(2) 0.019(2) -0.0019(17) -0.0020(18) -0.0001(18) _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 U1 Se4 2.8817(4) . ? U1 Se2 2.8989(4) . ? U1 Se5 2.9066(4) . ? U1 Se7 2.9401(4) . ? U1 Se1 3.0266(4) . ? U1 Se8 3.0275(4) . ? U1 Se3 3.0296(5) . ? U1 Se6 3.0503(4) . ? Se1 P1 2.1612(12) . ? Se2 P1 2.1672(12) . ? Se3 P2 2.1657(11) . ? Se4 P2 2.1777(11) . ? Se5 P3 2.1740(12) . ? Se6 P3 2.1592(11) . ? Se7 P4 2.1627(11) . ? Se8 P4 2.1627(11) . ? P1 C7 1.814(4) . ? P1 C1 1.816(4) . ? P2 C19 1.816(4) . ? P2 C13 1.816(4) . ? P3 C25 1.816(4) . ? P3 C31 1.820(4) . ? P4 C43 1.815(4) . ? P4 C37 1.823(4) . ? C1 C2 1.390(6) . ? C1 C6 1.400(5) . ? C2 C3 1.381(5) . ? C3 C4 1.378(6) . ? C4 C5 1.383(6) . ? C5 C6 1.389(5) . ? C7 C12 1.389(6) . ? C7 C8 1.392(5) . ? C8 C9 1.392(5) . ? C9 C10 1.367(6) . ? C10 C11 1.381(6) . ? C11 C12 1.381(6) . ? C13 C18 1.368(6) . ? C13 C14 1.399(6) . ? C14 C15 1.393(6) . ? C15 C16 1.380(7) . ? C16 C17 1.370(6) . ? C17 C18 1.380(6) . ? C19 C20 1.386(6) . ? C19 C24 1.400(5) . ? C20 C21 1.389(6) . ? C21 C22 1.386(6) . ? C22 C23 1.386(6) . ? C23 C24 1.381(5) . ? C25 C26 1.384(6) . ? C25 C30 1.387(6) . ? C26 C27 1.389(6) . ? C27 C28 1.371(7) . ? C28 C29 1.378(6) . ? C29 C30 1.390(6) . ? C31 C32 1.379(6) . ? C31 C36 1.385(6) . ? C32 C33 1.381(6) . ? C33 C34 1.366(7) . ? C34 C35 1.385(7) . ? C35 C36 1.380(6) . ? C37 C42 1.387(6) . ? C37 C38 1.393(6) . ? C38 C39 1.381(6) . ? C39 C40 1.372(6) . ? C40 C41 1.385(6) . ? C41 C42 1.389(6) . ? C43 C44 1.382(6) . ? C43 C48 1.406(6) . ? C44 C45 1.398(6) . ? C45 C46 1.374(7) . ? C46 C47 1.374(7) . ? C47 C48 1.392(6) . ? 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 Se4 U1 Se2 92.056(12) . . ? Se4 U1 Se5 90.133(12) . . ? Se2 U1 Se5 144.661(14) . . ? Se4 U1 Se7 144.208(13) . . ? Se2 U1 Se7 110.403(13) . . ? Se5 U1 Se7 86.980(13) . . ? Se4 U1 Se1 85.056(12) . . ? Se2 U1 Se1 72.564(12) . . ? Se5 U1 Se1 142.717(13) . . ? Se7 U1 Se1 76.161(12) . . ? Se4 U1 Se8 140.692(12) . . ? Se2 U1 Se8 80.157(12) . . ? Se5 U1 Se8 76.041(12) . . ? Se7 U1 Se8 72.658(12) . . ? Se1 U1 Se8 127.513(12) . . ? Se4 U1 Se3 73.198(11) . . ? Se2 U1 Se3 68.808(12) . . ? Se5 U1 Se3 78.173(13) . . ? Se7 U1 Se3 140.243(12) . . ? Se1 U1 Se3 134.387(12) . . ? Se8 U1 Se3 68.042(11) . . ? Se4 U1 Se6 70.045(12) . . ? Se2 U1 Se6 139.052(12) . . ? Se5 U1 Se6 74.093(12) . . ? Se7 U1 Se6 74.880(13) . . ? Se1 U1 Se6 69.515(11) . . ? Se8 U1 Se6 136.506(12) . . ? Se3 U1 Se6 133.254(12) . . ? P1 Se1 U1 87.40(3) . . ? P1 Se2 U1 90.63(3) . . ? P2 Se3 U1 86.26(3) . . ? P2 Se4 U1 89.84(3) . . ? P3 Se5 U1 88.49(3) . . ? P3 Se6 U1 85.10(3) . . ? P4 Se7 U1 89.97(3) . . ? P4 Se8 U1 87.69(3) . . ? C7 P1 C1 104.84(17) . . ? C7 P1 Se1 112.19(14) . . ? C1 P1 Se1 113.39(12) . . ? C7 P1 Se2 110.16(13) . . ? C1 P1 Se2 107.87(13) . . ? Se1 P1 Se2 108.28(4) . . ? C19 P2 C13 106.16(18) . . ? C19 P2 Se3 110.93(13) . . ? C13 P2 Se3 113.51(13) . . ? C19 P2 Se4 106.08(14) . . ? C13 P2 Se4 111.35(14) . . ? Se3 P2 Se4 108.56(5) . . ? C25 P3 C31 104.72(18) . . ? C25 P3 Se6 111.97(13) . . ? C31 P3 Se6 111.75(13) . . ? C25 P3 Se5 108.34(14) . . ? C31 P3 Se5 107.78(13) . . ? Se6 P3 Se5 111.92(5) . . ? C43 P4 C37 103.50(19) . . ? C43 P4 Se8 110.59(15) . . ? C37 P4 Se8 113.08(13) . . ? C43 P4 Se7 109.00(14) . . ? C37 P4 Se7 110.81(14) . . ? Se8 P4 Se7 109.67(5) . . ? C2 C1 C6 119.6(4) . . ? C2 C1 P1 120.7(3) . . ? C6 C1 P1 119.7(3) . . ? C3 C2 C1 120.0(4) . . ? C4 C3 C2 120.5(4) . . ? C3 C4 C5 120.0(4) . . ? C4 C5 C6 120.3(4) . . ? C5 C6 C1 119.6(4) . . ? C12 C7 C8 119.6(4) . . ? C12 C7 P1 122.2(3) . . ? C8 C7 P1 118.1(3) . . ? C9 C8 C7 120.0(4) . . ? C10 C9 C8 120.0(4) . . ? C9 C10 C11 120.3(4) . . ? C10 C11 C12 120.6(4) . . ? C11 C12 C7 119.6(4) . . ? C18 C13 C14 119.7(4) . . ? C18 C13 P2 121.8(3) . . ? C14 C13 P2 118.3(3) . . ? C15 C14 C13 119.6(4) . . ? C16 C15 C14 119.7(4) . . ? C17 C16 C15 120.1(4) . . ? C16 C17 C18 120.7(4) . . ? C13 C18 C17 120.2(4) . . ? C20 C19 C24 120.0(4) . . ? C20 C19 P2 121.2(3) . . ? C24 C19 P2 118.5(3) . . ? C19 C20 C21 120.1(4) . . ? C22 C21 C20 119.5(4) . . ? C23 C22 C21 120.8(4) . . ? C24 C23 C22 119.8(4) . . ? C23 C24 C19 119.8(4) . . ? C26 C25 C30 119.3(4) . . ? C26 C25 P3 121.1(3) . . ? C30 C25 P3 119.6(3) . . ? C25 C26 C27 120.0(4) . . ? C28 C27 C26 120.2(4) . . ? C27 C28 C29 120.4(4) . . ? C28 C29 C30 119.6(4) . . ? C25 C30 C29 120.3(4) . . ? C32 C31 C36 119.5(4) . . ? C32 C31 P3 121.8(3) . . ? C36 C31 P3 118.7(3) . . ? C33 C32 C31 120.1(4) . . ? C34 C33 C32 120.5(5) . . ? C33 C34 C35 119.8(4) . . ? C36 C35 C34 119.9(4) . . ? C35 C36 C31 120.2(4) . . ? C42 C37 C38 120.1(4) . . ? C42 C37 P4 122.0(3) . . ? C38 C37 P4 117.7(3) . . ? C39 C38 C37 119.8(4) . . ? C40 C39 C38 120.6(4) . . ? C39 C40 C41 119.5(4) . . ? C40 C41 C42 120.9(4) . . ? C37 C42 C41 119.0(4) . . ? C44 C43 C48 119.5(4) . . ? C44 C43 P4 121.7(3) . . ? C48 C43 P4 118.6(3) . . ? C43 C44 C45 119.9(4) . . ? C46 C45 C44 120.4(4) . . ? C45 C46 C47 120.0(4) . . ? C46 C47 C48 120.7(4) . . ? C47 C48 C43 119.4(4) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.942 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.102 data_xpl206 _database_code_depnum_ccdc_archive 'CCDC 906774' #TrackingRef 'web_deposit_cif_file_8_AndrewGaunt_1350598115.cif for 9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 Np P4 Se8' _chemical_formula_weight 1609.36 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' Np Np -11.4937 4.1493 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.8899(19) _cell_length_b 9.9688(14) _cell_length_c 18.862(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.609(2) _cell_angle_gamma 90.00 _cell_volume 2610.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 141(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1506 _exptl_absorpt_coefficient_mu 7.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3713 _exptl_absorpt_correction_T_max 0.6544 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 141(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 SMART 1k CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 31242 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 29.08 _reflns_number_total 12593 _reflns_number_gt 9300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 4.210 (Bruker, 1996)' _computing_cell_refinement 'SAINT 4.05 (Bruker, 1996)' _computing_data_reduction 'SAINT 4.05 (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.10 (Bruker, 2001)' _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^)+(0.0214P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.068(10) _refine_ls_number_reflns 12593 _refine_ls_number_parameters 550 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0622 _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 Np1 Np 0.180837(17) 0.94323(3) 0.744519(13) 0.02810(7) Uani 1 1 d . . . Se1 Se 0.00573(5) 1.11805(8) 0.76250(4) 0.04038(19) Uani 1 1 d . . . Se2 Se 0.03263(5) 0.77824(8) 0.80378(4) 0.03958(19) Uani 1 1 d . . . Se3 Se 0.10512(6) 0.90305(7) 0.60260(4) 0.0419(2) Uani 1 1 d . . . Se4 Se 0.21322(5) 0.65296(8) 0.70812(4) 0.03983(19) Uani 1 1 d . . . Se5 Se 0.19723(5) 1.20155(7) 0.66087(4) 0.03916(19) Uani 1 1 d . . . Se6 Se 0.37674(5) 0.95307(10) 0.69489(4) 0.04611(19) Uani 1 1 d . . . Se7 Se 0.24239(6) 1.14164(9) 0.85031(4) 0.0512(2) Uani 1 1 d . . . Se8 Se 0.29768(6) 0.79754(8) 0.85788(4) 0.0431(2) Uani 1 1 d . . . P1 P -0.05924(11) 0.9515(2) 0.81655(8) 0.0336(4) Uani 1 1 d . . . P2 P 0.12328(13) 0.68792(19) 0.61418(10) 0.0345(5) Uani 1 1 d . . . P3 P 0.34684(13) 1.1490(2) 0.64954(10) 0.0347(4) Uani 1 1 d . . . P4 P 0.31831(14) 0.98808(19) 0.91032(10) 0.0394(5) Uani 1 1 d . . . C1 C -0.0749(5) 0.9831(7) 0.9091(3) 0.0341(18) Uani 1 1 d . . . C2 C -0.0281(6) 1.0858(9) 0.9445(4) 0.056(2) Uani 1 1 d . . . H2 H 0.0101 1.1449 0.9195 0.068 Uiso 1 1 calc R . . C3 C -0.0369(7) 1.1023(11) 1.0168(5) 0.076(3) Uani 1 1 d . . . H3 H -0.0048 1.1726 1.0396 0.091 Uiso 1 1 calc R . . C4 C -0.0908(7) 1.0186(10) 1.0545(4) 0.066(3) Uani 1 1 d . . . H4 H -0.0963 1.0311 1.1031 0.079 Uiso 1 1 calc R . . C5 C -0.1384(6) 0.9135(9) 1.0209(4) 0.056(2) Uani 1 1 d . . . H5 H -0.1758 0.8543 1.0465 0.068 Uiso 1 1 calc R . . C6 C -0.1291(6) 0.8981(8) 0.9489(4) 0.048(2) Uani 1 1 d . . . H6 H -0.1608 0.8273 0.9263 0.058 Uiso 1 1 calc R . . C7 C -0.1795(5) 0.9103(7) 0.7811(3) 0.0341(19) Uani 1 1 d . . . C8 C -0.2580(6) 0.9851(8) 0.8041(4) 0.054(2) Uani 1 1 d . . . H8 H -0.2491 1.0579 0.8344 0.064 Uiso 1 1 calc R . . C9 C -0.3492(5) 0.9478(11) 0.7803(4) 0.052(2) Uani 1 1 d . . . H9 H -0.4019 0.9971 0.7949 0.063 Uiso 1 1 calc R . . C10 C -0.3643(6) 0.8415(9) 0.7365(4) 0.050(2) Uani 1 1 d . . . H10 H -0.4264 0.8159 0.7227 0.060 Uiso 1 1 calc R . . C11 C -0.2859(5) 0.7728(9) 0.7131(4) 0.051(2) Uani 1 1 d . . . H11 H -0.2951 0.7034 0.6807 0.062 Uiso 1 1 calc R . . C12 C -0.1938(5) 0.8039(9) 0.7363(3) 0.0407(19) Uani 1 1 d . . . H12 H -0.1418 0.7531 0.7217 0.049 Uiso 1 1 calc R . . C13 C 0.0089(5) 0.6015(8) 0.6161(4) 0.0356(17) Uani 1 1 d . . . C14 C -0.0027(6) 0.4844(8) 0.6502(5) 0.065(3) Uani 1 1 d . . . H14 H 0.0485 0.4494 0.6770 0.078 Uiso 1 1 calc R . . C15 C -0.0887(7) 0.4147(10) 0.6464(5) 0.082(3) Uani 1 1 d . . . H15 H -0.0953 0.3342 0.6706 0.098 Uiso 1 1 calc R . . C16 C -0.1640(6) 0.4654(12) 0.6066(5) 0.071(3) Uani 1 1 d . . . H16 H -0.2215 0.4178 0.6027 0.086 Uiso 1 1 calc R . . C17 C -0.1554(6) 0.5834(10) 0.5731(5) 0.060(2) Uani 1 1 d . . . H17 H -0.2074 0.6180 0.5469 0.072 Uiso 1 1 calc R . . C18 C -0.0696(5) 0.6539(8) 0.5773(4) 0.0448(19) Uani 1 1 d . . . H18 H -0.0642 0.7360 0.5543 0.054 Uiso 1 1 calc R . . C19 C 0.1818(5) 0.6304(8) 0.5351(4) 0.0378(17) Uani 1 1 d . . . C20 C 0.1313(6) 0.5692(10) 0.4805(4) 0.066(3) Uani 1 1 d . . . H20 H 0.0667 0.5480 0.4857 0.079 Uiso 1 1 calc R . . C21 C 0.1759(7) 0.5387(10) 0.4178(5) 0.071(3) Uani 1 1 d . . . H21 H 0.1414 0.4979 0.3808 0.085 Uiso 1 1 calc R . . C22 C 0.2713(7) 0.5691(10) 0.4108(5) 0.066(3) Uani 1 1 d . . . H22 H 0.3011 0.5503 0.3684 0.079 Uiso 1 1 calc R . . C23 C 0.3229(6) 0.6266(10) 0.4652(4) 0.059(2) Uani 1 1 d . . . H23 H 0.3879 0.6458 0.4604 0.071 Uiso 1 1 calc R . . C24 C 0.2780(6) 0.6562(9) 0.5277(4) 0.055(2) Uani 1 1 d . . . H24 H 0.3134 0.6940 0.5652 0.066 Uiso 1 1 calc R . . C25 C 0.3818(5) 1.1509(8) 0.5580(4) 0.0372(17) Uani 1 1 d . . . C26 C 0.3930(6) 1.0331(8) 0.5215(4) 0.051(2) Uani 1 1 d . . . H26 H 0.3782 0.9525 0.5434 0.061 Uiso 1 1 calc R . . C27 C 0.4258(6) 1.0313(11) 0.4525(5) 0.067(3) Uani 1 1 d . . . H27 H 0.4348 0.9507 0.4287 0.081 Uiso 1 1 calc R . . C28 C 0.4445(6) 1.1510(11) 0.4208(4) 0.058(2) Uani 1 1 d . . . H28 H 0.4683 1.1517 0.3752 0.069 Uiso 1 1 calc R . . C29 C 0.4292(7) 1.2682(10) 0.4541(5) 0.065(3) Uani 1 1 d . . . H29 H 0.4396 1.3484 0.4303 0.078 Uiso 1 1 calc R . . C30 C 0.3982(6) 1.2712(9) 0.5238(4) 0.052(2) Uani 1 1 d . . . H30 H 0.3886 1.3525 0.5468 0.062 Uiso 1 1 calc R . . C31 C 0.4264(5) 1.2712(8) 0.6932(4) 0.0379(18) Uani 1 1 d . . . C32 C 0.3934(8) 1.3826(9) 0.7248(5) 0.075(3) Uani 1 1 d . . . H32 H 0.3275 1.3995 0.7242 0.090 Uiso 1 1 calc R . . C33 C 0.4552(9) 1.4719(10) 0.7580(6) 0.097(4) Uani 1 1 d . . . H33 H 0.4322 1.5494 0.7791 0.116 Uiso 1 1 calc R . . C34 C 0.5514(8) 1.4434(14) 0.7590(5) 0.086(3) Uani 1 1 d . . . H34 H 0.5938 1.5019 0.7822 0.103 Uiso 1 1 calc R . . C35 C 0.5864(7) 1.3349(12) 0.7279(5) 0.078(3) Uani 1 1 d . . . H35 H 0.6523 1.3182 0.7289 0.093 Uiso 1 1 calc R . . C36 C 0.5233(6) 1.2476(9) 0.6942(5) 0.060(2) Uani 1 1 d . . . H36 H 0.5470 1.1718 0.6719 0.072 Uiso 1 1 calc R . . C37 C 0.2727(6) 0.9845(8) 0.9992(4) 0.050(2) Uani 1 1 d . . . C38 C 0.2028(6) 0.8954(10) 1.0184(5) 0.065(3) Uani 1 1 d . . . H38 H 0.1808 0.8304 0.9866 0.078 Uiso 1 1 calc R . . C39 C 0.1648(8) 0.9030(12) 1.0864(6) 0.089(4) Uani 1 1 d . . . H39 H 0.1179 0.8424 1.1001 0.106 Uiso 1 1 calc R . . C40 C 0.1973(8) 1.0005(13) 1.1328(5) 0.081(4) Uani 1 1 d . . . H40 H 0.1717 1.0057 1.1778 0.097 Uiso 1 1 calc R . . C41 C 0.2645(7) 1.0871(11) 1.1145(4) 0.065(3) Uani 1 1 d . . . H41 H 0.2858 1.1520 1.1467 0.078 Uiso 1 1 calc R . . C42 C 0.3031(6) 1.0817(10) 1.0483(4) 0.062(3) Uani 1 1 d . . . H42 H 0.3499 1.1435 1.0360 0.074 Uiso 1 1 calc R . . C43 C 0.4450(5) 1.0313(8) 0.9244(4) 0.0403(18) Uani 1 1 d . . . C44 C 0.5015(5) 0.9473(12) 0.9645(4) 0.067(2) Uani 1 1 d . . . H44 H 0.4762 0.8666 0.9802 0.081 Uiso 1 1 calc R . . C45 C 0.5954(6) 0.9798(11) 0.9822(5) 0.075(3) Uani 1 1 d . . . H45 H 0.6331 0.9213 1.0095 0.089 Uiso 1 1 calc R . . C46 C 0.6326(6) 1.0967(10) 0.9598(5) 0.061(3) Uani 1 1 d . . . H46 H 0.6954 1.1202 0.9730 0.074 Uiso 1 1 calc R . . C47 C 0.5777(6) 1.1817(9) 0.9173(5) 0.059(2) Uani 1 1 d . . . H47 H 0.6043 1.2608 0.9004 0.071 Uiso 1 1 calc R . . C48 C 0.4834(6) 1.1494(9) 0.8998(4) 0.049(2) Uani 1 1 d . . . H48 H 0.4460 1.2069 0.8716 0.059 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 Np1 0.02439(12) 0.03314(14) 0.02666(13) -0.00078(14) -0.00136(10) 0.00336(15) Se1 0.0345(4) 0.0410(5) 0.0461(5) 0.0092(4) 0.0084(4) 0.0069(4) Se2 0.0332(4) 0.0388(5) 0.0470(5) 0.0075(4) 0.0056(4) 0.0046(4) Se3 0.0547(5) 0.0390(5) 0.0315(4) -0.0009(3) -0.0092(4) 0.0060(3) Se4 0.0403(4) 0.0385(4) 0.0400(4) -0.0058(4) -0.0110(4) 0.0115(4) Se5 0.0285(4) 0.0381(4) 0.0509(5) 0.0063(4) 0.0017(4) 0.0058(3) Se6 0.0296(4) 0.0428(4) 0.0663(5) 0.0147(5) 0.0073(3) 0.0092(4) Se7 0.0634(6) 0.0428(5) 0.0463(5) -0.0119(4) -0.0191(4) 0.0161(4) Se8 0.0506(5) 0.0400(4) 0.0379(5) -0.0022(4) -0.0129(4) 0.0054(4) P1 0.0276(8) 0.0432(10) 0.0302(9) 0.0001(11) 0.0025(7) 0.0048(11) P2 0.0300(10) 0.0391(12) 0.0340(11) -0.0088(9) -0.0043(8) 0.0031(9) P3 0.0255(10) 0.0360(11) 0.0427(11) 0.0052(9) 0.0019(8) -0.0003(9) P4 0.0378(11) 0.0468(13) 0.0331(10) -0.0065(9) -0.0065(9) 0.0059(9) C1 0.034(4) 0.042(5) 0.027(4) 0.000(3) 0.002(3) 0.005(3) C2 0.055(6) 0.080(7) 0.035(5) -0.003(5) 0.008(4) -0.018(5) C3 0.087(8) 0.098(9) 0.043(6) -0.022(6) 0.004(5) -0.027(7) C4 0.074(7) 0.096(8) 0.026(4) -0.012(5) 0.002(5) 0.003(6) C5 0.058(5) 0.074(7) 0.038(4) 0.016(5) 0.008(4) -0.003(5) C6 0.048(5) 0.061(6) 0.037(4) 0.000(4) 0.004(4) -0.006(4) C7 0.027(4) 0.056(6) 0.019(3) 0.004(3) 0.000(3) 0.000(3) C8 0.047(5) 0.066(6) 0.047(5) -0.013(4) -0.004(4) 0.005(4) C9 0.041(4) 0.072(6) 0.044(4) -0.001(6) -0.002(3) 0.019(6) C10 0.032(5) 0.066(6) 0.050(5) 0.004(5) -0.009(4) -0.002(4) C11 0.045(5) 0.069(6) 0.038(5) -0.020(4) -0.023(4) 0.009(5) C12 0.037(4) 0.059(5) 0.025(4) -0.006(4) -0.008(3) 0.003(4) C13 0.035(4) 0.044(5) 0.028(4) -0.004(3) 0.000(3) 0.006(3) C14 0.047(5) 0.051(6) 0.096(7) 0.009(5) -0.016(5) -0.002(4) C15 0.075(7) 0.060(7) 0.109(8) 0.026(6) -0.015(6) -0.018(6) C16 0.046(5) 0.076(8) 0.091(7) 0.003(7) -0.008(5) -0.020(5) C17 0.049(6) 0.073(7) 0.058(6) 0.000(5) -0.013(5) 0.005(5) C18 0.043(5) 0.040(5) 0.051(5) 0.005(4) -0.008(4) 0.000(4) C19 0.030(4) 0.045(5) 0.038(4) -0.005(4) 0.001(3) 0.000(4) C20 0.039(5) 0.101(8) 0.057(6) -0.032(5) 0.001(4) -0.015(5) C21 0.076(7) 0.091(8) 0.047(6) -0.029(5) 0.010(5) -0.002(6) C22 0.064(7) 0.089(7) 0.046(5) -0.022(5) 0.017(5) 0.005(6) C23 0.040(5) 0.080(7) 0.057(5) -0.014(5) 0.007(4) -0.010(5) C24 0.053(5) 0.067(6) 0.044(5) -0.011(5) 0.007(4) -0.011(5) C25 0.021(4) 0.046(5) 0.044(4) 0.001(4) -0.005(3) 0.001(3) C26 0.049(5) 0.046(5) 0.057(6) -0.008(4) 0.002(4) 0.006(4) C27 0.061(6) 0.094(8) 0.047(6) -0.018(6) -0.008(5) 0.030(6) C28 0.047(5) 0.094(8) 0.032(5) 0.003(5) 0.000(4) 0.012(5) C29 0.078(7) 0.075(8) 0.041(5) 0.016(5) -0.017(5) -0.013(6) C30 0.075(6) 0.047(5) 0.033(5) 0.007(4) -0.001(4) 0.000(5) C31 0.041(4) 0.040(5) 0.033(4) 0.009(4) 0.002(3) -0.010(4) C32 0.067(6) 0.059(6) 0.096(8) -0.011(6) -0.023(6) 0.008(5) C33 0.106(9) 0.042(7) 0.140(10) -0.027(6) -0.046(8) -0.003(6) C34 0.094(8) 0.072(7) 0.089(7) 0.012(8) -0.050(6) -0.039(8) C35 0.040(6) 0.103(10) 0.088(8) 0.000(7) -0.022(5) -0.021(6) C36 0.039(5) 0.073(7) 0.069(6) -0.009(5) 0.002(4) -0.004(5) C37 0.046(5) 0.069(7) 0.035(4) -0.007(4) -0.016(4) 0.012(4) C38 0.060(6) 0.090(8) 0.047(5) -0.005(5) 0.002(5) 0.000(5) C39 0.077(8) 0.110(10) 0.080(8) 0.014(7) 0.031(6) -0.012(7) C40 0.076(8) 0.112(10) 0.055(6) -0.008(7) 0.016(6) 0.036(7) C41 0.077(7) 0.087(8) 0.030(5) -0.013(5) -0.006(5) 0.026(6) C42 0.057(6) 0.081(7) 0.047(5) -0.002(5) -0.013(5) 0.001(5) C43 0.042(5) 0.042(5) 0.037(4) -0.006(4) 0.002(4) 0.002(4) C44 0.042(5) 0.080(6) 0.079(6) 0.037(7) -0.006(4) 0.002(6) C45 0.038(5) 0.099(10) 0.086(7) 0.010(6) -0.015(5) 0.011(5) C46 0.045(5) 0.078(7) 0.061(6) -0.017(5) 0.007(5) -0.009(5) C47 0.056(6) 0.058(6) 0.064(6) -0.008(5) 0.017(5) -0.014(5) C48 0.051(5) 0.048(5) 0.047(5) -0.003(4) 0.001(4) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Np1 Se3 2.8766(8) . ? Np1 Se2 2.8848(8) . ? Np1 Se6 2.9040(8) . ? Np1 Se7 2.9205(9) . ? Np1 Se4 3.0107(9) . ? Np1 Se1 3.0190(8) . ? Np1 Se8 3.0200(8) . ? Np1 Se5 3.0320(8) . ? Se1 P1 2.159(2) . ? Se2 P1 2.165(2) . ? Se3 P2 2.170(2) . ? Se4 P2 2.167(2) . ? Se5 P3 2.160(2) . ? Se6 P3 2.168(2) . ? Se7 P4 2.161(2) . ? Se8 P4 2.157(2) . ? P1 C1 1.794(7) . ? P1 C7 1.828(7) . ? P2 C13 1.809(8) . ? P2 C19 1.812(7) . ? P3 C25 1.807(7) . ? P3 C31 1.825(7) . ? P4 C37 1.809(8) . ? P4 C43 1.824(8) . ? C1 C6 1.371(10) . ? C1 C2 1.375(10) . ? C2 C3 1.381(11) . ? C3 C4 1.339(12) . ? C4 C5 1.382(12) . ? C5 C6 1.377(10) . ? C7 C12 1.367(10) . ? C7 C8 1.400(10) . ? C8 C9 1.382(10) . ? C9 C10 1.356(12) . ? C10 C11 1.371(11) . ? C11 C12 1.375(9) . ? C13 C14 1.344(10) . ? C13 C18 1.397(9) . ? C14 C15 1.382(11) . ? C15 C16 1.366(12) . ? C16 C17 1.342(13) . ? C17 C18 1.384(11) . ? C19 C24 1.372(10) . ? C19 C20 1.372(10) . ? C20 C21 1.384(11) . ? C21 C22 1.369(12) . ? C22 C23 1.363(11) . ? C23 C24 1.380(10) . ? C25 C26 1.372(10) . ? C25 C30 1.384(10) . ? C26 C27 1.391(11) . ? C27 C28 1.363(13) . ? C28 C29 1.347(13) . ? C29 C30 1.394(11) . ? C31 C32 1.347(11) . ? C31 C36 1.366(10) . ? C32 C33 1.375(12) . ? C33 C34 1.365(14) . ? C34 C35 1.330(15) . ? C35 C36 1.377(12) . ? C37 C38 1.372(11) . ? C37 C42 1.397(11) . ? C38 C39 1.403(13) . ? C39 C40 1.376(14) . ? C40 C41 1.325(14) . ? C41 C42 1.374(12) . ? C43 C44 1.363(11) . ? C43 C48 1.378(11) . ? C44 C45 1.375(11) . ? C45 C46 1.348(13) . ? C46 C47 1.382(12) . ? C47 C48 1.380(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se3 Np1 Se2 92.01(2) . . ? Se3 Np1 Se6 91.50(2) . . ? Se2 Np1 Se6 146.05(3) . . ? Se3 Np1 Se7 145.34(2) . . ? Se2 Np1 Se7 108.65(3) . . ? Se6 Np1 Se7 86.47(3) . . ? Se3 Np1 Se4 72.96(2) . . ? Se2 Np1 Se4 69.71(2) . . ? Se6 Np1 Se4 79.14(3) . . ? Se7 Np1 Se4 139.82(2) . . ? Se3 Np1 Se1 84.85(2) . . ? Se2 Np1 Se1 72.52(2) . . ? Se6 Np1 Se1 141.43(3) . . ? Se7 Np1 Se1 75.73(2) . . ? Se4 Np1 Se1 134.95(2) . . ? Se3 Np1 Se8 140.10(2) . . ? Se2 Np1 Se8 80.01(2) . . ? Se6 Np1 Se8 75.80(2) . . ? Se7 Np1 Se8 72.59(3) . . ? Se4 Np1 Se8 67.57(2) . . ? Se1 Np1 Se8 128.08(2) . . ? Se3 Np1 Se5 70.42(2) . . ? Se2 Np1 Se5 138.65(2) . . ? Se6 Np1 Se5 73.67(2) . . ? Se7 Np1 Se5 75.85(3) . . ? Se4 Np1 Se5 133.14(2) . . ? Se1 Np1 Se5 68.94(2) . . ? Se8 Np1 Se5 136.90(2) . . ? P1 Se1 Np1 87.59(6) . . ? P1 Se2 Np1 91.00(6) . . ? P2 Se3 Np1 90.31(5) . . ? P2 Se4 Np1 86.88(6) . . ? P3 Se5 Np1 86.11(6) . . ? P3 Se6 Np1 89.24(5) . . ? P4 Se7 Np1 90.42(6) . . ? P4 Se8 Np1 87.88(6) . . ? C1 P1 C7 105.1(3) . . ? C1 P1 Se1 112.9(3) . . ? C7 P1 Se1 113.0(2) . . ? C1 P1 Se2 109.6(2) . . ? C7 P1 Se2 108.4(3) . . ? Se1 P1 Se2 107.79(7) . . ? C13 P2 C19 106.3(3) . . ? C13 P2 Se4 113.2(2) . . ? C19 P2 Se4 111.2(2) . . ? C13 P2 Se3 111.9(3) . . ? C19 P2 Se3 106.5(3) . . ? Se4 P2 Se3 107.69(8) . . ? C25 P3 C31 104.4(3) . . ? C25 P3 Se5 112.2(2) . . ? C31 P3 Se5 111.4(3) . . ? C25 P3 Se6 109.4(3) . . ? C31 P3 Se6 108.5(2) . . ? Se5 P3 Se6 110.71(8) . . ? C37 P4 C43 103.4(4) . . ? C37 P4 Se8 111.2(3) . . ? C43 P4 Se8 113.0(2) . . ? C37 P4 Se7 108.7(3) . . ? C43 P4 Se7 111.3(3) . . ? Se8 P4 Se7 109.09(8) . . ? C6 C1 C2 117.0(7) . . ? C6 C1 P1 120.5(6) . . ? C2 C1 P1 122.3(6) . . ? C1 C2 C3 120.9(8) . . ? C4 C3 C2 121.1(9) . . ? C3 C4 C5 119.7(8) . . ? C6 C5 C4 118.6(8) . . ? C1 C6 C5 122.6(8) . . ? C12 C7 C8 120.2(7) . . ? C12 C7 P1 121.1(5) . . ? C8 C7 P1 118.6(6) . . ? C9 C8 C7 118.1(8) . . ? C10 C9 C8 122.2(8) . . ? C9 C10 C11 118.4(7) . . ? C10 C11 C12 121.7(7) . . ? C7 C12 C11 119.3(7) . . ? C14 C13 C18 118.2(8) . . ? C14 C13 P2 122.7(6) . . ? C18 C13 P2 118.9(6) . . ? C13 C14 C15 121.8(8) . . ? C16 C15 C14 119.3(9) . . ? C17 C16 C15 120.3(9) . . ? C16 C17 C18 120.5(8) . . ? C17 C18 C13 119.8(8) . . ? C24 C19 C20 119.0(7) . . ? C24 C19 P2 119.0(6) . . ? C20 C19 P2 121.8(6) . . ? C19 C20 C21 120.5(8) . . ? C22 C21 C20 119.5(8) . . ? C23 C22 C21 120.6(8) . . ? C22 C23 C24 119.5(8) . . ? C19 C24 C23 120.8(8) . . ? C26 C25 C30 119.0(7) . . ? C26 C25 P3 120.6(6) . . ? C30 C25 P3 120.4(6) . . ? C25 C26 C27 121.7(9) . . ? C28 C27 C26 118.0(9) . . ? C29 C28 C27 121.4(8) . . ? C28 C29 C30 121.1(9) . . ? C25 C30 C29 118.6(8) . . ? C32 C31 C36 118.9(8) . . ? C32 C31 P3 122.7(7) . . ? C36 C31 P3 118.4(6) . . ? C31 C32 C33 121.3(10) . . ? C34 C33 C32 118.0(10) . . ? C35 C34 C33 122.2(10) . . ? C34 C35 C36 118.8(9) . . ? C31 C36 C35 120.8(9) . . ? C38 C37 C42 118.5(8) . . ? C38 C37 P4 121.8(6) . . ? C42 C37 P4 119.5(7) . . ? C37 C38 C39 119.6(9) . . ? C40 C39 C38 119.6(10) . . ? C41 C40 C39 121.0(10) . . ? C40 C41 C42 120.5(10) . . ? C41 C42 C37 120.7(9) . . ? C44 C43 C48 119.3(8) . . ? C44 C43 P4 118.3(7) . . ? C48 C43 P4 122.2(6) . . ? C43 C44 C45 121.2(10) . . ? C46 C45 C44 119.8(9) . . ? C45 C46 C47 120.1(9) . . ? C48 C47 C46 120.0(9) . . ? C43 C48 C47 119.5(8) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.358 _refine_diff_density_min -1.381 _refine_diff_density_rms 0.143