Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Alexander Rothenberger' _publ_contact_author_address ; Department of Inorganic Chemistry University of Karlsruhe Engesserstr. 15 Karlsruhe 76131 GERMANY ; _publ_contact_author_email ROTHENBERGER@CHEMIE.UNI-KARLSRUHE.DE _publ_section_title ; Polymeric arrangements of P-Se anions and a first insight into their reactivity ; loop_ _publ_author_name 'Alexander Rothenberger' 'Christopher E. Anson' 'Maryam Shafaei-Fallah' 'Weifang Shi.' # Attachment 'cc.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 292989' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Na4 O3 P2 Se6' _chemical_formula_weight 998.17 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7746(8) _cell_length_b 11.4669(10) _cell_length_c 16.7949(14) _cell_angle_alpha 71.905(6) _cell_angle_beta 78.473(6) _cell_angle_gamma 85.510(7) _cell_volume 1753.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14580 _cell_measurement_theta_min 3.65 _cell_measurement_theta_max 56.43 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 6.428 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2119 _exptl_absorpt_correction_T_max 0.5658 _exptl_absorpt_process_details 'stoe x-red32' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe ipds 2' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15513 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.18 _reflns_number_total 7931 _reflns_number_gt 5653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe x-area' _computing_cell_refinement 'stoe x-area' _computing_data_reduction 'stoe x-area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^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 7931 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0972 _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 C1 C 0.2814(6) 0.7915(4) 0.3208(3) 0.0210(10) Uani 1 1 d . . . C2 C 0.4145(6) 0.8287(5) 0.2759(3) 0.0291(12) Uani 1 1 d . . . H2A H 0.4917 0.8113 0.3046 0.035 Uiso 1 1 calc R . . C3 C 0.4347(6) 0.8908(6) 0.1895(4) 0.0336(13) Uani 1 1 d . . . H3A H 0.5258 0.9157 0.1591 0.040 Uiso 1 1 calc R . . C4 C 0.3227(7) 0.9169(5) 0.1471(3) 0.0335(13) Uani 1 1 d . . . H4A H 0.3365 0.9612 0.0882 0.040 Uiso 1 1 calc R . . C5 C 0.1914(6) 0.8782(5) 0.1910(3) 0.0307(13) Uani 1 1 d . . . H5A H 0.1149 0.8938 0.1618 0.037 Uiso 1 1 calc R . . C6 C 0.1705(6) 0.8166(5) 0.2777(3) 0.0269(12) Uani 1 1 d . . . H6A H 0.0793 0.7914 0.3077 0.032 Uiso 1 1 calc R . . C7 C 0.1325(5) 0.3187(5) 0.8968(3) 0.0228(10) Uani 1 1 d . . . C8 C 0.1150(6) 0.3820(5) 0.9567(3) 0.0287(12) Uani 1 1 d . . . H8A H 0.1210 0.4689 0.9381 0.034 Uiso 1 1 calc R . . C9 C 0.0888(7) 0.3197(6) 1.0435(4) 0.0353(13) Uani 1 1 d . . . H9A H 0.0777 0.3640 1.0838 0.042 Uiso 1 1 calc R . . C10 C 0.0789(7) 0.1932(6) 1.0711(3) 0.0397(16) Uani 1 1 d . . . H10A H 0.0604 0.1502 1.1303 0.048 Uiso 1 1 calc R . . C11 C 0.0963(8) 0.1303(6) 1.0119(4) 0.0444(17) Uani 1 1 d . . . H11A H 0.0900 0.0434 1.0309 0.053 Uiso 1 1 calc R . . C12 C 0.1229(6) 0.1915(5) 0.9248(3) 0.0314(13) Uani 1 1 d . . . H12A H 0.1344 0.1467 0.8848 0.038 Uiso 1 1 calc R . . C13 C 0.2301(12) 0.9028(7) 0.7342(5) 0.070(3) Uani 1 1 d . . . H13A H 0.2633 0.8256 0.7720 0.084 Uiso 1 1 calc R . . H13B H 0.1868 0.9566 0.7688 0.084 Uiso 1 1 calc R . . C14 C 0.3492(9) 0.9676(9) 0.6628(8) 0.084(4) Uani 1 1 d . . . H14A H 0.3980 1.0247 0.6810 0.101 Uiso 1 1 calc R . . H14B H 0.4177 0.9073 0.6460 0.101 Uiso 1 1 calc R . . C15 C 0.2765(9) 1.0356(7) 0.5915(5) 0.062(2) Uani 1 1 d . . . H15A H 0.2759 1.1251 0.5829 0.074 Uiso 1 1 calc R . . H15B H 0.3224 1.0193 0.5378 0.074 Uiso 1 1 calc R . . C16 C 0.1341(9) 0.9881(6) 0.6189(5) 0.058(2) Uani 1 1 d . . . H16A H 0.0690 1.0491 0.6376 0.070 Uiso 1 1 calc R . . H16B H 0.1027 0.9711 0.5712 0.070 Uiso 1 1 calc R . . C17 C -0.3037(7) 0.7585(5) 0.6337(4) 0.0362(14) Uani 1 1 d . . . H17A H -0.3878 0.7753 0.6071 0.043 Uiso 1 1 calc R . . H17B H -0.2291 0.7251 0.5971 0.043 Uiso 1 1 calc R . . C18 C -0.2561(7) 0.8752(6) 0.6431(4) 0.0394(14) Uani 1 1 d . . . H18A H -0.1673 0.9033 0.6035 0.047 Uiso 1 1 calc R . . H18B H -0.3276 0.9414 0.6320 0.047 Uiso 1 1 calc R . . C19 C -0.2368(8) 0.8388(6) 0.7346(4) 0.0464(17) Uani 1 1 d . . . H19A H -0.1399 0.8098 0.7398 0.056 Uiso 1 1 calc R . . H19B H -0.2592 0.9082 0.7585 0.056 Uiso 1 1 calc R . . C20 C -0.3385(8) 0.7370(7) 0.7783(4) 0.0447(16) Uani 1 1 d . . . H20A H -0.3097 0.6823 0.8309 0.054 Uiso 1 1 calc R . . H20B H -0.4334 0.7701 0.7933 0.054 Uiso 1 1 calc R . . C21 C -0.2787(17) 0.3578(12) 0.9617(9) 0.0317(18) Uiso 0.50 1 d P A 1 H21A H -0.2540 0.4351 0.9695 0.038 Uiso 0.50 1 calc PR A 1 H21B H -0.1924 0.3205 0.9370 0.038 Uiso 0.50 1 calc PR A 1 C22 C -0.3428(15) 0.2725(13) 1.0447(8) 0.039(3) Uiso 0.50 1 d P A 1 H22A H -0.2743 0.2086 1.0672 0.047 Uiso 0.50 1 calc PR A 1 H22B H -0.3765 0.3174 1.0868 0.047 Uiso 0.50 1 calc PR A 1 C23 C -0.4637(16) 0.2153(14) 1.0270(10) 0.0363(19) Uiso 0.50 1 d P A 1 H23A H -0.5409 0.1952 1.0769 0.044 Uiso 0.50 1 calc PR A 1 H23B H -0.4337 0.1402 1.0104 0.044 Uiso 0.50 1 calc PR A 1 C24 C -0.5057(15) 0.3190(12) 0.9523(8) 0.0330(19) Uiso 0.50 1 d P A 1 H24A H -0.5470 0.2853 0.9151 0.040 Uiso 0.50 1 calc PR A 1 H24B H -0.5745 0.3757 0.9735 0.040 Uiso 0.50 1 calc PR A 1 C21A C -0.2717(17) 0.3241(12) 0.9586(9) 0.0317(18) Uiso 0.50 1 d P A 2 H21C H -0.1929 0.2909 0.9244 0.038 Uiso 0.50 1 calc PR A 2 H21D H -0.2350 0.3849 0.9795 0.038 Uiso 0.50 1 calc PR A 2 C22A C -0.3422(17) 0.2233(15) 1.0315(9) 0.047(3) Uiso 0.50 1 d P A 2 H22C H -0.3406 0.2379 1.0864 0.056 Uiso 0.50 1 calc PR A 2 H22D H -0.2962 0.1432 1.0318 0.056 Uiso 0.50 1 calc PR A 2 C23A C -0.4953(16) 0.2266(14) 1.0163(10) 0.0363(19) Uiso 0.50 1 d P A 2 H23C H -0.5067 0.1682 0.9855 0.044 Uiso 0.50 1 calc PR A 2 H23D H -0.5630 0.2072 1.0708 0.044 Uiso 0.50 1 calc PR A 2 C24A C -0.5128(15) 0.3559(12) 0.9634(8) 0.0330(19) Uiso 0.50 1 d P A 2 H24C H -0.5888 0.3637 0.9309 0.040 Uiso 0.50 1 calc PR A 2 H24D H -0.5331 0.4117 0.9991 0.040 Uiso 0.50 1 calc PR A 2 Se1 Se 0.04323(5) 0.72886(5) 0.49470(3) 0.02288(12) Uani 1 1 d . . . Se2 Se 0.41570(6) 0.73637(5) 0.49355(3) 0.02333(12) Uani 1 1 d . . . Se3 Se 0.27643(5) 0.50822(4) 0.42998(3) 0.02089(11) Uani 1 1 d . . . Se4 Se -0.02502(5) 0.51767(5) 0.75955(3) 0.02246(12) Uani 1 1 d . . . Se5 Se 0.20423(6) 0.27679(5) 0.70896(3) 0.02494(12) Uani 1 1 d . . . Se6 Se 0.34061(5) 0.52598(5) 0.75907(3) 0.02356(12) Uani 1 1 d . . . P1 P 0.25491(14) 0.69922(11) 0.43331(8) 0.0186(3) Uani 1 1 d . . . P2 P 0.16340(14) 0.40569(12) 0.78331(8) 0.0204(3) Uani 1 1 d . . . Na1 Na 0.1735(2) 0.70619(18) 0.64630(13) 0.0273(5) Uani 1 1 d . . . Na2 Na 0.0292(2) 0.44928(18) 0.59750(12) 0.0242(4) Uani 1 1 d . . . Na3 Na 0.4145(2) 0.45304(19) 0.59748(13) 0.0256(4) Uani 1 1 d . . . Na4 Na -0.3392(2) 0.4595(2) 0.76037(13) 0.0326(5) Uani 1 1 d . . . O1 O 0.1360(5) 0.8796(4) 0.6867(3) 0.0385(10) Uani 1 1 d . . . O2 O -0.3349(5) 0.6723(4) 0.7173(2) 0.0357(10) Uani 1 1 d . . . O3 O -0.3773(4) 0.3820(4) 0.9064(3) 0.0418(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(3) 0.017(2) 0.021(2) -0.0044(18) -0.005(2) -0.002(2) C2 0.025(3) 0.031(3) 0.028(3) -0.002(2) -0.007(2) -0.004(2) C3 0.021(3) 0.041(3) 0.031(3) -0.003(2) 0.003(2) -0.001(3) C4 0.045(4) 0.032(3) 0.022(2) -0.005(2) -0.004(2) -0.002(3) C5 0.040(4) 0.027(3) 0.027(3) -0.002(2) -0.019(2) -0.006(2) C6 0.024(3) 0.025(2) 0.030(3) -0.002(2) -0.008(2) -0.009(2) C7 0.021(3) 0.024(2) 0.023(2) -0.0036(19) -0.007(2) -0.002(2) C8 0.029(3) 0.032(3) 0.024(2) -0.005(2) -0.007(2) 0.000(2) C9 0.035(4) 0.046(3) 0.025(3) -0.009(2) -0.008(2) -0.001(3) C10 0.053(4) 0.042(3) 0.019(2) 0.005(2) -0.015(3) -0.011(3) C11 0.063(5) 0.033(3) 0.033(3) 0.007(2) -0.024(3) -0.012(3) C12 0.041(4) 0.026(3) 0.030(3) -0.005(2) -0.016(3) -0.006(2) C13 0.137(9) 0.038(4) 0.053(4) -0.019(3) -0.054(5) 0.009(5) C14 0.039(5) 0.083(7) 0.166(11) -0.080(7) -0.038(6) 0.004(5) C15 0.071(6) 0.047(4) 0.064(5) -0.025(4) 0.017(4) -0.026(4) C16 0.069(6) 0.026(3) 0.079(5) -0.004(3) -0.033(5) -0.002(3) C17 0.041(4) 0.035(3) 0.036(3) -0.016(3) -0.003(3) -0.005(3) C18 0.038(4) 0.033(3) 0.051(4) -0.017(3) -0.006(3) -0.006(3) C19 0.056(5) 0.038(3) 0.055(4) -0.023(3) -0.018(4) 0.003(3) C20 0.045(4) 0.061(4) 0.037(3) -0.030(3) -0.006(3) 0.006(3) Se1 0.0187(3) 0.0251(2) 0.0244(2) -0.0064(2) -0.0046(2) 0.0000(2) Se2 0.0210(3) 0.0256(2) 0.0250(2) -0.0066(2) -0.0079(2) -0.0043(2) Se3 0.0206(3) 0.0178(2) 0.0241(2) -0.00506(18) -0.0054(2) -0.00172(19) Se4 0.0192(3) 0.0268(2) 0.0208(2) -0.00549(19) -0.00495(19) -0.0008(2) Se5 0.0234(3) 0.0271(3) 0.0263(2) -0.0099(2) -0.0056(2) -0.0019(2) Se6 0.0208(3) 0.0265(3) 0.0236(2) -0.0051(2) -0.0066(2) -0.0054(2) P1 0.0175(7) 0.0180(6) 0.0204(5) -0.0036(5) -0.0063(5) -0.0020(5) P2 0.0177(7) 0.0240(6) 0.0205(6) -0.0069(5) -0.0048(5) -0.0025(5) Na1 0.0305(13) 0.0232(10) 0.0289(10) -0.0075(8) -0.0071(9) -0.0031(9) Na2 0.0236(11) 0.0261(10) 0.0241(9) -0.0060(8) -0.0090(8) -0.0020(9) Na3 0.0214(12) 0.0279(10) 0.0254(10) -0.0061(8) -0.0022(8) -0.0019(9) Na4 0.0308(13) 0.0392(12) 0.0257(10) -0.0051(9) -0.0053(9) -0.0077(10) O1 0.037(3) 0.024(2) 0.053(3) -0.0116(19) -0.003(2) -0.0037(18) O2 0.041(3) 0.040(2) 0.0288(19) -0.0128(17) -0.0035(18) -0.013(2) O3 0.026(2) 0.060(3) 0.029(2) 0.0034(19) -0.0061(18) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.385(7) . ? C1 C2 1.392(7) . ? C1 P1 1.833(5) . ? C2 C3 1.385(7) . ? C3 C4 1.386(8) . ? C4 C5 1.376(9) . ? C5 C6 1.388(7) . ? C7 C12 1.391(7) . ? C7 C8 1.391(7) . ? C7 P2 1.832(5) . ? C8 C9 1.390(7) . ? C9 C10 1.384(9) . ? C10 C11 1.378(9) . ? C11 C12 1.392(8) . ? C13 O1 1.421(8) . ? C13 C14 1.539(14) . ? C14 C15 1.490(13) . ? C15 C16 1.467(11) . ? C16 O1 1.403(8) . ? C16 Na1 3.124(7) . ? C17 O2 1.434(7) . ? C17 C18 1.514(8) . ? C18 C19 1.509(9) . ? C19 C20 1.499(10) . ? C20 O2 1.434(7) . ? C21 O3 1.423(14) . ? C21 C22 1.480(19) . ? C22 C23 1.516(19) . ? C23 C24 1.536(19) . ? C24 O3 1.449(14) . ? C21A C22A 1.49(2) . ? C21A O3 1.471(15) . ? C22A C23A 1.56(2) . ? C23A C24A 1.489(19) . ? C24A O3 1.462(15) . ? Se1 P1 2.1713(15) . ? Se1 Na1 3.001(2) . ? Se1 Na2 3.1147(19) 2_566 ? Se1 Na2 3.133(2) . ? Se2 P1 2.1641(12) . ? Se2 Na1 3.075(2) . ? Se2 Na3 3.174(2) . ? Se2 Na3 3.208(2) 2_666 ? Se3 P1 2.2008(13) . ? Se3 Na3 3.010(2) 2_666 ? Se3 Na4 3.042(2) 2_566 ? Se3 Na2 3.092(2) 2_566 ? Se3 Na3 3.227(2) . ? Se3 Na2 3.251(2) . ? Se4 P2 2.1921(15) . ? Se4 Na1 2.947(2) . ? Se4 Na2 2.998(2) . ? Se4 Na4 3.190(2) . ? Se5 P2 2.1813(14) . ? Se5 Na3 2.929(2) . ? Se5 Na2 2.965(2) . ? Se6 P2 2.1936(13) . ? Se6 Na1 2.967(2) . ? Se6 Na3 3.020(2) . ? Se6 Na4 3.165(2) 1_655 ? Na1 O1 2.275(4) . ? Na1 Na2 3.735(3) . ? Na1 Na3 3.780(3) . ? Na2 Se3 3.092(2) 2_566 ? Na2 Se1 3.1146(19) 2_566 ? Na2 Na2 3.268(4) 2_566 ? Na2 Na3 3.770(3) . ? Na2 Na4 4.082(3) . ? Na3 Se3 3.010(2) 2_666 ? Na3 Se2 3.208(2) 2_666 ? Na3 Na3 3.252(4) 2_666 ? Na3 Na4 4.009(3) 1_655 ? Na4 O3 2.297(4) . ? Na4 O2 2.320(5) . ? Na4 Se3 3.041(2) 2_566 ? Na4 Se6 3.165(2) 1_455 ? Na4 Na3 4.009(3) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 119.1(5) . . ? C6 C1 P1 120.1(4) . . ? C2 C1 P1 120.7(4) . . ? C3 C2 C1 120.2(5) . . ? C2 C3 C4 120.4(6) . . ? C5 C4 C3 119.6(5) . . ? C4 C5 C6 120.2(5) . . ? C1 C6 C5 120.5(5) . . ? C12 C7 C8 119.1(5) . . ? C12 C7 P2 122.0(4) . . ? C8 C7 P2 118.9(4) . . ? C9 C8 C7 120.8(5) . . ? C10 C9 C8 120.0(6) . . ? C11 C10 C9 119.3(5) . . ? C10 C11 C12 121.3(6) . . ? C7 C12 C11 119.5(5) . . ? O1 C13 C14 101.6(6) . . ? C15 C14 C13 103.7(7) . . ? C16 C15 C14 104.3(7) . . ? O1 C16 C15 107.7(7) . . ? O1 C16 Na1 41.6(3) . . ? C15 C16 Na1 104.4(5) . . ? O2 C17 C18 107.6(5) . . ? C19 C18 C17 103.8(5) . . ? C20 C19 C18 103.1(5) . . ? O2 C20 C19 104.7(5) . . ? O3 C21 C22 108.0(11) . . ? C23 C22 C21 105.6(11) . . ? C22 C23 C24 101.2(11) . . ? O3 C24 C23 105.3(10) . . ? C22A C21A O3 106.9(11) . . ? C21A C22A C23A 104.5(12) . . ? C24A C23A C22A 102.7(12) . . ? O3 C24A C23A 103.1(11) . . ? P1 Se1 Na1 84.48(6) . . ? P1 Se1 Na2 82.89(5) . 2_566 ? Na1 Se1 Na2 136.21(6) . 2_566 ? P1 Se1 Na2 89.19(5) . . ? Na1 Se1 Na2 75.00(5) . . ? Na2 Se1 Na2 63.08(6) 2_566 . ? P1 Se2 Na1 82.78(5) . . ? P1 Se2 Na3 87.67(5) . . ? Na1 Se2 Na3 74.41(6) . . ? P1 Se2 Na3 80.84(5) . 2_666 ? Na1 Se2 Na3 133.04(5) . 2_666 ? Na3 Se2 Na3 61.26(6) . 2_666 ? P1 Se3 Na3 85.07(5) . 2_666 ? P1 Se3 Na4 102.30(6) . 2_566 ? Na3 Se3 Na4 82.97(6) 2_666 2_566 ? P1 Se3 Na2 82.99(5) . 2_566 ? Na3 Se3 Na2 159.56(5) 2_666 2_566 ? Na4 Se3 Na2 83.44(6) 2_566 2_566 ? P1 Se3 Na3 85.73(5) . . ? Na3 Se3 Na3 62.74(7) 2_666 . ? Na4 Se3 Na3 144.15(6) 2_566 . ? Na2 Se3 Na3 132.40(6) 2_566 . ? P1 Se3 Na2 85.68(5) . . ? Na3 Se3 Na2 133.49(5) 2_666 . ? Na4 Se3 Na2 143.48(6) 2_566 . ? Na2 Se3 Na2 61.97(6) 2_566 . ? Na3 Se3 Na2 71.18(5) . . ? P2 Se4 Na1 84.34(6) . . ? P2 Se4 Na2 83.37(5) . . ? Na1 Se4 Na2 77.85(6) . . ? P2 Se4 Na4 134.61(6) . . ? Na1 Se4 Na4 133.51(6) . . ? Na2 Se4 Na4 82.49(6) . . ? P2 Se5 Na3 84.70(6) . . ? P2 Se5 Na2 84.33(5) . . ? Na3 Se5 Na2 79.53(6) . . ? P2 Se6 Na1 83.83(5) . . ? P2 Se6 Na3 82.30(5) . . ? Na1 Se6 Na3 78.30(6) . . ? P2 Se6 Na4 129.90(6) . 1_655 ? Na1 Se6 Na4 136.87(6) . 1_655 ? Na3 Se6 Na4 80.76(6) . 1_655 ? C1 P1 Se2 110.24(16) . . ? C1 P1 Se1 109.29(18) . . ? Se2 P1 Se1 114.42(6) . . ? C1 P1 Se3 104.35(16) . . ? Se2 P1 Se3 109.53(6) . . ? Se1 P1 Se3 108.52(5) . . ? C7 P2 Se5 108.72(17) . . ? C7 P2 Se4 106.88(18) . . ? Se5 P2 Se4 111.71(5) . . ? C7 P2 Se6 107.62(16) . . ? Se5 P2 Se6 112.22(6) . . ? Se4 P2 Se6 109.47(6) . . ? O1 Na1 Se4 109.35(14) . . ? O1 Na1 Se6 109.87(13) . . ? Se4 Na1 Se6 74.53(5) . . ? O1 Na1 Se1 111.06(14) . . ? Se4 Na1 Se1 92.54(6) . . ? Se6 Na1 Se1 139.07(8) . . ? O1 Na1 Se2 111.50(14) . . ? Se4 Na1 Se2 139.14(8) . . ? Se6 Na1 Se2 90.86(6) . . ? Se1 Na1 Se2 73.71(5) . . ? O1 Na1 C16 24.17(19) . . ? Se4 Na1 C16 125.08(19) . . ? Se6 Na1 C16 128.76(15) . . ? Se1 Na1 C16 90.67(15) . . ? Se2 Na1 C16 94.00(18) . . ? O1 Na1 Na2 149.10(15) . . ? Se4 Na1 Na2 51.68(4) . . ? Se6 Na1 Na2 89.62(6) . . ? Se1 Na1 Na2 54.10(4) . . ? Se2 Na1 Na2 91.23(6) . . ? C16 Na1 Na2 141.08(16) . . ? O1 Na1 Na3 150.48(14) . . ? Se4 Na1 Na3 88.79(6) . . ? Se6 Na1 Na3 51.47(5) . . ? Se1 Na1 Na3 90.46(6) . . ? Se2 Na1 Na3 54.00(5) . . ? C16 Na1 Na3 146.02(19) . . ? Na2 Na1 Na3 60.22(5) . . ? Se5 Na2 Se4 74.73(5) . . ? Se5 Na2 Se3 140.94(7) . 2_566 ? Se4 Na2 Se3 94.77(6) . 2_566 ? Se5 Na2 Se1 97.87(6) . 2_566 ? Se4 Na2 Se1 145.82(7) . 2_566 ? Se3 Na2 Se1 69.75(4) 2_566 2_566 ? Se5 Na2 Se1 134.79(7) . . ? Se4 Na2 Se1 88.99(5) . . ? Se3 Na2 Se1 81.08(5) 2_566 . ? Se1 Na2 Se1 116.92(6) 2_566 . ? Se5 Na2 Se3 94.10(6) . . ? Se4 Na2 Se3 134.15(6) . . ? Se3 Na2 Se3 118.03(6) 2_566 . ? Se1 Na2 Se3 78.89(5) 2_566 . ? Se1 Na2 Se3 67.52(4) . . ? Se5 Na2 Na2 143.68(11) . 2_566 ? Se4 Na2 Na2 140.50(11) . 2_566 ? Se3 Na2 Na2 61.41(6) 2_566 2_566 ? Se1 Na2 Na2 58.73(6) 2_566 2_566 ? Se1 Na2 Na2 58.19(6) . 2_566 ? Se3 Na2 Na2 56.62(6) . 2_566 ? Se5 Na2 Na1 88.37(5) . . ? Se4 Na2 Na1 50.47(4) . . ? Se3 Na2 Na1 114.07(7) 2_566 . ? Se1 Na2 Na1 163.65(8) 2_566 . ? Se1 Na2 Na1 50.89(4) . . ? Se3 Na2 Na1 85.63(6) . . ? Na2 Na2 Na1 108.05(9) 2_566 . ? Se5 Na2 Na3 49.81(4) . . ? Se4 Na2 Na3 88.22(5) . . ? Se3 Na2 Na3 169.24(7) 2_566 . ? Se1 Na2 Na3 112.77(7) 2_566 . ? Se1 Na2 Na3 88.65(6) . . ? Se3 Na2 Na3 54.12(5) . . ? Na2 Na2 Na3 110.26(10) 2_566 . ? Na1 Na2 Na3 60.47(6) . . ? Se5 Na2 Na4 103.00(6) . . ? Se4 Na2 Na4 50.78(4) . . ? Se3 Na2 Na4 47.75(4) 2_566 . ? Se1 Na2 Na4 100.98(6) 2_566 . ? Se1 Na2 Na4 97.93(6) . . ? Se3 Na2 Na4 162.70(7) . . ? Na2 Na2 Na4 108.29(9) 2_566 . ? Na1 Na2 Na4 92.23(6) . . ? Na3 Na2 Na4 138.03(7) . . ? Se5 Na3 Se3 138.99(8) . 2_666 ? Se5 Na3 Se6 75.23(5) . . ? Se3 Na3 Se6 95.88(6) 2_666 . ? Se5 Na3 Se2 135.89(8) . . ? Se3 Na3 Se2 82.24(5) 2_666 . ? Se6 Na3 Se2 88.01(6) . . ? Se5 Na3 Se2 95.20(6) . 2_666 ? Se3 Na3 Se2 69.89(5) 2_666 2_666 ? Se6 Na3 Se2 146.10(7) . 2_666 ? Se2 Na3 Se2 118.74(6) . 2_666 ? Se5 Na3 Se3 95.31(6) . . ? Se3 Na3 Se3 117.26(7) 2_666 . ? Se6 Na3 Se3 134.06(8) . . ? Se2 Na3 Se3 67.68(4) . . ? Se2 Na3 Se3 78.44(5) 2_666 . ? Se5 Na3 Na3 142.21(10) . 2_666 ? Se3 Na3 Na3 61.90(7) 2_666 2_666 ? Se6 Na3 Na3 141.71(10) . 2_666 ? Se2 Na3 Na3 59.88(6) . 2_666 ? Se2 Na3 Na3 58.86(7) 2_666 2_666 ? Se3 Na3 Na3 55.36(6) . 2_666 ? Se5 Na3 Na2 50.67(5) . . ? Se3 Na3 Na2 170.25(8) 2_666 . ? Se6 Na3 Na2 88.17(6) . . ? Se2 Na3 Na2 89.06(6) . . ? Se2 Na3 Na2 111.08(6) 2_666 . ? Se3 Na3 Na2 54.71(4) . . ? Na3 Na3 Na2 109.80(9) 2_666 . ? Se5 Na3 Na1 88.07(6) . . ? Se3 Na3 Na1 117.15(7) 2_666 . ? Se6 Na3 Na1 50.23(5) . . ? Se2 Na3 Na1 51.59(5) . . ? Se2 Na3 Na1 163.56(7) 2_666 . ? Se3 Na3 Na1 85.22(6) . . ? Na3 Na3 Na1 109.86(9) 2_666 . ? Na2 Na3 Na1 59.31(5) . . ? Se5 Na3 Na4 101.13(6) . 1_655 ? Se3 Na3 Na4 48.85(4) 2_666 1_655 ? Se6 Na3 Na4 51.20(5) . 1_655 ? Se2 Na3 Na4 99.07(6) . 1_655 ? Se2 Na3 Na4 101.02(7) 2_666 1_655 ? Se3 Na3 Na4 163.52(7) . 1_655 ? Na3 Na3 Na4 110.04(9) 2_666 1_655 ? Na2 Na3 Na4 137.79(7) . 1_655 ? Na1 Na3 Na4 94.11(6) . 1_655 ? O3 Na4 O2 110.89(18) . . ? O3 Na4 Se3 164.99(17) . 2_566 ? O2 Na4 Se3 84.00(11) . 2_566 ? O3 Na4 Se6 92.49(13) . 1_455 ? O2 Na4 Se6 78.92(13) . 1_455 ? Se3 Na4 Se6 92.30(6) 2_566 1_455 ? O3 Na4 Se4 89.88(12) . . ? O2 Na4 Se4 76.32(12) . . ? Se3 Na4 Se4 91.95(6) 2_566 . ? Se6 Na4 Se4 154.28(9) 1_455 . ? O3 Na4 Na3 129.48(13) . 1_455 ? O2 Na4 Na3 93.06(12) . 1_455 ? Se3 Na4 Na3 48.18(4) 2_566 1_455 ? Se6 Na4 Na3 48.03(4) 1_455 1_455 ? Se4 Na4 Na3 139.93(7) . 1_455 ? O3 Na4 Na2 126.35(14) . . ? O2 Na4 Na2 90.35(13) . . ? Se3 Na4 Na2 48.80(4) 2_566 . ? Se6 Na4 Na2 140.77(7) 1_455 . ? Se4 Na4 Na2 46.73(4) . . ? Na3 Na4 Na2 95.84(6) 1_455 . ? C16 O1 C13 104.7(5) . . ? C16 O1 Na1 114.2(4) . . ? C13 O1 Na1 117.3(4) . . ? C17 O2 C20 108.1(4) . . ? C17 O2 Na4 130.5(3) . . ? C20 O2 Na4 120.5(4) . . ? C21A O3 C24A 106.2(8) . . ? C21A O3 C24 104.9(8) . . ? C24A O3 C24 20.1(6) . . ? C21A O3 C21 16.0(8) . . ? C24A O3 C21 104.7(8) . . ? C24 O3 C21 109.2(8) . . ? C21A O3 Na4 126.2(7) . . ? C24A O3 Na4 126.4(6) . . ? C24 O3 Na4 120.2(5) . . ? C21 O3 Na4 128.7(7) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.991 _refine_diff_density_min -1.440 _refine_diff_density_rms 0.548 data_2 _database_code_depnum_ccdc_archive 'CCDC 292991' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H58 Na2 Ni O6 P2 Se6' _chemical_formula_weight 1227.21 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' Na Na 0.0362 0.0249 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.440(6) _cell_length_b 10.313(3) _cell_length_c 16.676(6) _cell_angle_alpha 90.00 _cell_angle_beta 116.31(4) _cell_angle_gamma 90.00 _cell_volume 2380.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 4.8 _cell_measurement_theta_max 51.7 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 5.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3088 _exptl_absorpt_correction_T_max 0.4275 _exptl_absorpt_process_details 'shelxtl v5.1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe ipds 1 on schneider rotary anode' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11125 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.97 _reflns_number_total 4458 _reflns_number_gt 2900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe expose' _computing_cell_refinement 'stoe expose' _computing_data_reduction 'stoe expose' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+2.6409P] 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 4458 _refine_ls_number_parameters 230 _refine_ls_number_restraints 100 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.016 _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 Na1 Na 0.7248(2) -0.2301(3) 0.0285(2) 0.0620(8) Uani 1 1 d . . . P1 P 0.61968(13) 0.02247(18) -0.11173(13) 0.0454(4) Uani 1 1 d . A . Ni1 Ni 0.5000 0.0000 0.0000 0.0419(3) Uani 1 2 d S . . Se1 Se 0.52413(5) -0.13103(7) -0.10314(5) 0.0492(2) Uani 1 1 d . A . Se2 Se 0.62345(6) 0.13325(8) 0.00421(5) 0.0566(3) Uani 1 1 d . A . Se3 Se 0.75366(6) -0.03978(10) -0.10365(7) 0.0719(3) Uani 1 1 d . A . C1 C 0.5547(5) 0.1141(6) -0.2155(5) 0.0473(17) Uani 1 1 d . . . C2 C 0.5950(7) 0.1398(8) -0.2736(6) 0.066(2) Uani 1 1 d . A . H2A H 0.6581 0.1114 -0.2589 0.079 Uiso 1 1 calc R . . C3 C 0.5441(9) 0.2059(10) -0.3520(7) 0.083(3) Uani 1 1 d . . . H3A H 0.5730 0.2225 -0.3900 0.100 Uiso 1 1 calc R A . C4 C 0.4501(9) 0.2490(9) -0.3761(7) 0.081(3) Uani 1 1 d . A . H4A H 0.4149 0.2937 -0.4301 0.098 Uiso 1 1 calc R . . C5 C 0.4107(7) 0.2238(8) -0.3181(6) 0.068(2) Uani 1 1 d . . . H5A H 0.3479 0.2532 -0.3327 0.082 Uiso 1 1 calc R A . C6 C 0.4613(6) 0.1558(7) -0.2381(6) 0.058(2) Uani 1 1 d . A . H6A H 0.4323 0.1386 -0.2001 0.069 Uiso 1 1 calc R . . O1 O 0.8861(4) -0.2208(6) 0.1205(5) 0.0776(18) Uani 1 1 d D A . C7 C 0.9519(9) -0.3197(11) 0.1315(11) 0.120(5) Uani 1 1 d D . . H7A H 0.9204 -0.3877 0.0869 0.144 Uiso 1 1 calc R A . H7B H 0.9741 -0.3581 0.1911 0.144 Uiso 1 1 calc R . . C8 C 1.0331(8) -0.2697(15) 0.1213(10) 0.122(5) Uani 1 1 d D A . H8A H 1.0400 -0.3134 0.0723 0.147 Uiso 1 1 calc R . . H8B H 1.0929 -0.2804 0.1766 0.147 Uiso 1 1 calc R . . C9 C 1.0097(10) -0.1303(14) 0.1008(10) 0.119(5) Uani 1 1 d D . . H9A H 0.9825 -0.1144 0.0363 0.143 Uiso 1 1 calc R A . H9B H 1.0674 -0.0764 0.1314 0.143 Uiso 1 1 calc R . . C10 C 0.9370(7) -0.1029(10) 0.1349(8) 0.088(3) Uani 1 1 d D A . H10A H 0.9686 -0.0805 0.1986 0.105 Uiso 1 1 calc R . . H10B H 0.8939 -0.0319 0.1015 0.105 Uiso 1 1 calc R . . O2 O 0.7425(11) -0.4061(13) -0.0543(9) 0.074(4) Uiso 0.50 1 d PD A 1 C11 C 0.791(2) -0.526(2) -0.0278(14) 0.129(10) Uiso 0.50 1 d PD A 1 H11A H 0.7822 -0.5601 0.0232 0.155 Uiso 0.50 1 calc PR A 1 H11B H 0.8598 -0.5137 -0.0087 0.155 Uiso 0.50 1 calc PR A 1 C12 C 0.754(2) -0.6167(18) -0.0987(14) 0.095(5) Uiso 0.50 1 d PD A 1 H12A H 0.7140 -0.6822 -0.0883 0.114 Uiso 0.50 1 calc PR A 1 H12B H 0.8067 -0.6604 -0.1054 0.114 Uiso 0.50 1 calc PR A 1 C13 C 0.6967(16) -0.5406(16) -0.1768(12) 0.080(6) Uiso 0.50 1 d PD A 1 H13A H 0.6306 -0.5745 -0.2062 0.096 Uiso 0.50 1 calc PR A 1 H13B H 0.7245 -0.5445 -0.2194 0.096 Uiso 0.50 1 calc PR A 1 C14 C 0.6959(16) -0.4057(16) -0.1482(10) 0.071(6) Uiso 0.50 1 d PD A 1 H14A H 0.7303 -0.3491 -0.1718 0.085 Uiso 0.50 1 calc PR A 1 H14B H 0.6294 -0.3744 -0.1700 0.085 Uiso 0.50 1 calc PR A 1 O2' O 0.7051(9) -0.4169(10) -0.0501(7) 0.056(3) Uiso 0.50 1 d PD A 2 C11' C 0.7225(15) -0.5487(14) -0.0248(11) 0.073(5) Uiso 0.50 1 d PD A 2 H11C H 0.6683 -0.5853 -0.0169 0.087 Uiso 0.50 1 calc PR A 2 H11D H 0.7814 -0.5576 0.0315 0.087 Uiso 0.50 1 calc PR A 2 C12' C 0.733(2) -0.615(2) -0.0962(14) 0.095(5) Uiso 0.50 1 d PD A 2 H12C H 0.7284 -0.7089 -0.0930 0.114 Uiso 0.50 1 calc PR A 2 H12D H 0.7941 -0.5918 -0.0983 0.114 Uiso 0.50 1 calc PR A 2 C13' C 0.6482(19) -0.557(2) -0.1716(14) 0.113(9) Uiso 0.50 1 d PD A 2 H13C H 0.5877 -0.5921 -0.1747 0.135 Uiso 0.50 1 calc PR A 2 H13D H 0.6500 -0.5715 -0.2289 0.135 Uiso 0.50 1 calc PR A 2 C14' C 0.6607(17) -0.4180(17) -0.1459(10) 0.082(7) Uiso 0.50 1 d PD A 2 H14C H 0.7021 -0.3748 -0.1684 0.098 Uiso 0.50 1 calc PR A 2 H14D H 0.5981 -0.3736 -0.1701 0.098 Uiso 0.50 1 calc PR A 2 O3 O 0.6804(7) -0.3302(10) 0.1381(7) 0.043(3) Uiso 0.50 1 d PD A 1 C15 C 0.5921(10) -0.3990(17) 0.1027(11) 0.057(5) Uiso 0.50 1 d PD A 1 H15A H 0.5387 -0.3402 0.0935 0.068 Uiso 0.50 1 calc PR A 1 H15B H 0.5800 -0.4375 0.0449 0.068 Uiso 0.50 1 calc PR A 1 C16 C 0.5989(12) -0.4970(18) 0.1641(13) 0.073(5) Uiso 0.50 1 d PD A 1 H16A H 0.5608 -0.5731 0.1328 0.088 Uiso 0.50 1 calc PR A 1 H16B H 0.5756 -0.4656 0.2065 0.088 Uiso 0.50 1 calc PR A 1 C17 C 0.7027(13) -0.5294(19) 0.2107(19) 0.091(8) Uiso 0.50 1 d PD A 1 H17A H 0.7175 -0.6038 0.1824 0.110 Uiso 0.50 1 calc PR A 1 H17B H 0.7217 -0.5502 0.2737 0.110 Uiso 0.50 1 calc PR A 1 C18 C 0.7534(10) -0.4120(17) 0.2031(12) 0.055(5) Uiso 0.50 1 d PD A 1 H18A H 0.7852 -0.3676 0.2609 0.066 Uiso 0.50 1 calc PR A 1 H18B H 0.8024 -0.4348 0.1832 0.066 Uiso 0.50 1 calc PR A 1 O3' O 0.6940(9) -0.3585(12) 0.1224(8) 0.062(4) Uiso 0.50 1 d PD A 2 C15' C 0.6083(13) -0.433(2) 0.0926(13) 0.089(8) Uiso 0.50 1 d PD A 2 H15C H 0.5900 -0.4654 0.0319 0.107 Uiso 0.50 1 calc PR A 2 H15D H 0.5553 -0.3800 0.0916 0.107 Uiso 0.50 1 calc PR A 2 C16' C 0.6264(14) -0.5406(17) 0.1532(11) 0.071(5) Uiso 0.50 1 d PD A 2 H16C H 0.6423 -0.6187 0.1290 0.086 Uiso 0.50 1 calc PR A 2 H16D H 0.5693 -0.5585 0.1627 0.086 Uiso 0.50 1 calc PR A 2 C17' C 0.7088(13) -0.5020(18) 0.2383(12) 0.071(6) Uiso 0.50 1 d PD A 2 H17C H 0.7586 -0.5696 0.2591 0.085 Uiso 0.50 1 calc PR A 2 H17D H 0.6875 -0.4863 0.2847 0.085 Uiso 0.50 1 calc PR A 2 C18' C 0.7466(13) -0.3808(19) 0.2172(11) 0.068(7) Uiso 0.50 1 d PD A 2 H18C H 0.7377 -0.3077 0.2503 0.081 Uiso 0.50 1 calc PR A 2 H18D H 0.8158 -0.3897 0.2341 0.081 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0591(18) 0.0488(16) 0.057(2) 0.0084(14) 0.0071(16) 0.0005(14) P1 0.0388(9) 0.0477(10) 0.0467(12) 0.0108(8) 0.0162(9) -0.0043(8) Ni1 0.0343(6) 0.0468(7) 0.0378(7) 0.0067(5) 0.0097(6) -0.0097(5) Se1 0.0467(4) 0.0423(4) 0.0559(5) 0.0053(3) 0.0202(4) -0.0072(3) Se2 0.0508(4) 0.0709(5) 0.0446(5) -0.0063(4) 0.0179(4) -0.0286(4) Se3 0.0512(5) 0.0815(6) 0.0908(8) 0.0322(5) 0.0385(5) 0.0125(4) C1 0.052(4) 0.036(3) 0.047(4) 0.002(3) 0.016(4) -0.006(3) C2 0.073(6) 0.072(5) 0.050(5) 0.011(4) 0.024(5) -0.009(4) C3 0.110(9) 0.085(7) 0.051(6) 0.011(5) 0.032(6) -0.006(6) C4 0.109(8) 0.059(5) 0.050(6) 0.015(4) 0.012(6) 0.007(5) C5 0.059(5) 0.057(5) 0.062(6) 0.004(4) 0.002(5) 0.011(4) C6 0.055(5) 0.058(5) 0.049(5) -0.001(4) 0.013(4) -0.001(4) O1 0.058(4) 0.082(4) 0.084(5) 0.023(4) 0.023(4) 0.004(3) C7 0.092(9) 0.101(9) 0.152(14) 0.040(9) 0.042(9) 0.023(7) C8 0.071(7) 0.209(17) 0.089(9) -0.005(10) 0.037(7) 0.037(9) C9 0.104(10) 0.165(14) 0.111(11) -0.003(9) 0.067(9) -0.046(9) C10 0.070(6) 0.096(7) 0.080(8) -0.020(6) 0.017(6) -0.012(6) _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 Na1 O3' 2.257(12) . ? Na1 O1 2.275(7) . ? Na1 O2' 2.274(11) . ? Na1 O2 2.369(13) . ? Na1 O3 2.447(11) . ? Na1 Se1 3.071(4) . ? Na1 Se3 3.127(3) . ? Na1 P1 3.394(4) . ? P1 C1 1.832(8) . ? P1 Se3 2.113(2) . ? P1 Se1 2.2114(19) . ? P1 Se2 2.224(2) . ? Ni1 Se2 2.3254(9) 3_655 ? Ni1 Se2 2.3254(9) . ? Ni1 Se1 2.3433(10) 3_655 ? Ni1 Se1 2.3434(10) . ? C1 C2 1.388(12) . ? C1 C6 1.389(11) . ? C2 C3 1.372(13) . ? C3 C4 1.396(16) . ? C4 C5 1.376(15) . ? C5 C6 1.399(12) . ? O1 C7 1.393(11) . ? O1 C10 1.410(10) . ? C7 C8 1.432(13) . ? C8 C9 1.484(14) . ? C9 C10 1.493(13) . ? O2 C11 1.410(15) . ? O2 C14 1.404(13) . ? C11 C12 1.414(16) . ? C12 C13 1.440(16) . ? C13 C14 1.472(15) . ? O2' C11' 1.413(13) . ? O2' C14' 1.433(14) . ? C11' C12' 1.444(16) . ? C12' C13' 1.481(17) . ? C13' C14' 1.488(16) . ? O3 C15 1.413(12) . ? O3 C18 1.440(12) . ? C15 C16 1.409(15) . ? C16 C17 1.477(16) . ? C17 C18 1.478(15) . ? O3' C15' 1.418(14) . ? O3' C18' 1.439(13) . ? C15' C16' 1.440(15) . ? C16' C17' 1.481(16) . ? C17' C18' 1.486(15) . ? 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 O3' Na1 O1 93.5(4) . . ? O3' Na1 O2' 83.5(5) . . ? O1 Na1 O2' 104.5(4) . . ? O3' Na1 O2 93.9(5) . . ? O1 Na1 O2 92.9(4) . . ? O2' Na1 O2 15.2(4) . . ? O3' Na1 O3 11.2(4) . . ? O1 Na1 O3 95.7(3) . . ? O2' Na1 O3 93.6(4) . . ? O2 Na1 O3 104.8(5) . . ? O3' Na1 Se1 103.6(3) . . ? O1 Na1 Se1 157.5(2) . . ? O2' Na1 Se1 92.0(3) . . ? O2 Na1 Se1 100.3(4) . . ? O3 Na1 Se1 98.4(3) . . ? O3' Na1 Se3 175.7(4) . . ? O1 Na1 Se3 89.62(19) . . ? O2' Na1 Se3 98.6(3) . . ? O2 Na1 Se3 88.9(4) . . ? O3 Na1 Se3 165.0(3) . . ? Se1 Na1 Se3 72.61(7) . . ? O3' Na1 P1 138.2(4) . . ? O1 Na1 P1 118.59(19) . . ? O2' Na1 P1 110.6(3) . . ? O2 Na1 P1 109.3(4) . . ? O3 Na1 P1 129.2(3) . . ? Se1 Na1 P1 39.60(5) . . ? Se3 Na1 P1 37.52(5) . . ? C1 P1 Se3 109.1(3) . . ? C1 P1 Se1 109.2(2) . . ? Se3 P1 Se1 116.16(9) . . ? C1 P1 Se2 110.4(2) . . ? Se3 P1 Se2 116.94(10) . . ? Se1 P1 Se2 94.16(8) . . ? C1 P1 Na1 160.3(2) . . ? Se3 P1 Na1 64.36(8) . . ? Se1 P1 Na1 62.30(8) . . ? Se2 P1 Na1 88.56(9) . . ? Se2 Ni1 Se2 180.0 3_655 . ? Se2 Ni1 Se1 88.17(4) 3_655 3_655 ? Se2 Ni1 Se1 91.83(4) . 3_655 ? Se2 Ni1 Se1 91.83(4) 3_655 . ? Se2 Ni1 Se1 88.17(4) . . ? Se1 Ni1 Se1 180.0 3_655 . ? P1 Se1 Ni1 87.85(6) . . ? P1 Se1 Na1 78.10(8) . . ? Ni1 Se1 Na1 96.04(8) . . ? P1 Se2 Ni1 87.99(6) . . ? P1 Se3 Na1 78.12(8) . . ? C2 C1 C6 119.0(8) . . ? C2 C1 P1 122.0(6) . . ? C6 C1 P1 118.9(6) . . ? C3 C2 C1 121.0(10) . . ? C2 C3 C4 121.1(10) . . ? C5 C4 C3 117.6(9) . . ? C4 C5 C6 122.1(9) . . ? C1 C6 C5 119.2(9) . . ? C7 O1 C10 106.9(7) . . ? C7 O1 Na1 125.1(7) . . ? C10 O1 Na1 120.8(6) . . ? O1 C7 C8 110.3(9) . . ? C7 C8 C9 103.9(8) . . ? C8 C9 C10 104.0(8) . . ? O1 C10 C9 103.1(8) . . ? C11 O2 C14 106.9(12) . . ? C11 O2 Na1 132.1(12) . . ? C14 O2 Na1 120.9(10) . . ? O2 C11 C12 111.0(14) . . ? C11 C12 C13 104.7(13) . . ? C12 C13 C14 108.2(12) . . ? O2 C14 C13 106.5(11) . . ? C11' O2' C14' 105.0(10) . . ? C11' O2' Na1 133.2(9) . . ? C14' O2' Na1 121.7(9) . . ? O2' C11' C12' 106.4(13) . . ? C11' C12' C13' 97.3(14) . . ? C12' C13' C14' 100.8(14) . . ? O2' C14' C13' 105.4(12) . . ? C15 O3 C18 108.0(9) . . ? C15 O3 Na1 115.9(9) . . ? C18 O3 Na1 115.1(9) . . ? C16 C15 O3 108.0(11) . . ? C15 C16 C17 105.0(13) . . ? C16 C17 C18 105.2(12) . . ? O3 C18 C17 106.1(11) . . ? C15' O3' C18' 106.5(11) . . ? C15' O3' Na1 121.8(10) . . ? C18' O3' Na1 131.7(9) . . ? O3' C15' C16' 108.1(13) . . ? C15' C16' C17' 106.4(12) . . ? C16' C17' C18' 105.1(11) . . ? O3' C18' C17' 107.7(11) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.658 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.124 data_3 _database_code_depnum_ccdc_archive 'CCDC 292992' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H42 K2 O4 P2 Se6' _chemical_formula_weight 1056.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6326(7) _cell_length_b 19.9940(10) _cell_length_c 15.4290(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.654(5) _cell_angle_gamma 90.00 _cell_volume 3889.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6290 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 5.971 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'stoe stadi 4' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29272 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 31.84 _reflns_number_total 8957 _reflns_number_gt 5506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'kuma ccd' _computing_cell_refinement 'kuma ccd' _computing_data_reduction 'kuma ccd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0947P)^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 8957 _refine_ls_number_parameters 373 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1743 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.07451(12) 0.47568(8) 0.12370(11) 0.0303(3) Uani 1 1 d . . . K2 K 0.43091(11) 0.58981(8) -0.04810(10) 0.0298(3) Uani 1 1 d . . . P1 P 0.10056(13) 0.64519(8) 0.02372(12) 0.0236(4) Uani 1 1 d . A . P2 P 0.40975(13) 0.53917(9) 0.18405(12) 0.0246(4) Uani 1 1 d . A . Se1 Se 0.16736(5) 0.57291(4) -0.05757(5) 0.02839(18) Uani 1 1 d . . . Se2 Se -0.06273(5) 0.63462(4) 0.04745(5) 0.0335(2) Uani 1 1 d . . . Se3 Se 0.16836(5) 0.64119(3) 0.16452(5) 0.02790(18) Uani 1 1 d . A . Se4 Se 0.35227(5) 0.64610(3) 0.15659(5) 0.02724(18) Uani 1 1 d . A . Se5 Se 0.33550(5) 0.46680(3) 0.10025(5) 0.02859(18) Uani 1 1 d . . . Se6 Se 0.57505(5) 0.55634(4) 0.17435(6) 0.0367(2) Uani 1 1 d . . . C1 C 0.1289(6) 0.7294(4) -0.0127(5) 0.0302(16) Uani 1 1 d . . . C2 C 0.0692(7) 0.7826(4) 0.0142(6) 0.0408(19) Uani 1 1 d . A . H2A H 0.0154 0.7758 0.0536 0.049 Uiso 1 1 calc R . . C3 C 0.0890(8) 0.8445(4) -0.0168(7) 0.055(3) Uani 1 1 d . . . H3A H 0.0472 0.8808 0.0012 0.067 Uiso 1 1 calc R A . C4 C 0.1667(8) 0.8571(4) -0.0728(7) 0.053(3) Uani 1 1 d . A . H4A H 0.1771 0.9011 -0.0940 0.064 Uiso 1 1 calc R . . C5 C 0.2296(7) 0.8049(4) -0.0981(6) 0.046(2) Uani 1 1 d . . . H5A H 0.2853 0.8127 -0.1354 0.055 Uiso 1 1 calc R A . C6 C 0.2099(5) 0.7405(4) -0.0678(5) 0.0313(16) Uani 1 1 d . A . H6A H 0.2521 0.7041 -0.0849 0.038 Uiso 1 1 calc R . . C7 C 0.3769(5) 0.5253(4) 0.2970(5) 0.0291(15) Uani 1 1 d . . . C8 C 0.3035(5) 0.4777(4) 0.3158(5) 0.0282(15) Uani 1 1 d . A . H8A H 0.2654 0.4536 0.2708 0.034 Uiso 1 1 calc R . . C9 C 0.2868(6) 0.4658(4) 0.4031(5) 0.0397(19) Uani 1 1 d . . . H9A H 0.2373 0.4324 0.4172 0.048 Uiso 1 1 calc R A . C10 C 0.3388(6) 0.5004(4) 0.4688(5) 0.0386(18) Uani 1 1 d . A . H10A H 0.3258 0.4916 0.5277 0.046 Uiso 1 1 calc R . . C11 C 0.4119(6) 0.5492(4) 0.4474(5) 0.0405(19) Uani 1 1 d . . . H11A H 0.4494 0.5739 0.4921 0.049 Uiso 1 1 calc R A . C12 C 0.4297(6) 0.5615(4) 0.3623(5) 0.0339(16) Uani 1 1 d . A . H12A H 0.4786 0.5953 0.3482 0.041 Uiso 1 1 calc R . . O1 O -0.0364(5) 0.5101(3) 0.2628(4) 0.0615(18) Uani 1 1 d . A . C13 C -0.0257(11) 0.4866(9) 0.3457(8) 0.118(6) Uani 1 1 d . . . H13A H 0.0388 0.5061 0.3756 0.142 Uiso 1 1 calc R A . H13B H -0.0171 0.4374 0.3448 0.142 Uiso 1 1 calc R . . C14 C -0.1153(8) 0.5032(7) 0.3923(7) 0.074(3) Uani 1 1 d . A . H14A H -0.0931 0.5189 0.4516 0.089 Uiso 1 1 calc R . . H14B H -0.1625 0.4640 0.3967 0.089 Uiso 1 1 calc R . . C15 C -0.1683(10) 0.5561(6) 0.3424(7) 0.079(4) Uani 1 1 d . . . H15A H -0.1439 0.6007 0.3632 0.095 Uiso 1 1 calc R A . H15B H -0.2462 0.5532 0.3453 0.095 Uiso 1 1 calc R . . C16 C -0.1370(11) 0.5433(8) 0.2550(7) 0.119(7) Uani 1 1 d . A . H16A H -0.1903 0.5147 0.2231 0.143 Uiso 1 1 calc R . . H16B H -0.1311 0.5859 0.2229 0.143 Uiso 1 1 calc R . . O2 O 0.1122(11) 0.3590(6) 0.2254(13) 0.0424(18) Uiso 0.50 1 d PD A 1 C17 C 0.0213(10) 0.3147(7) 0.2286(12) 0.036(4) Uiso 0.50 1 d PD A 1 H17A H -0.0362 0.3293 0.1862 0.043 Uiso 0.50 1 calc PR A 1 H17B H -0.0060 0.3153 0.2873 0.043 Uiso 0.50 1 calc PR A 1 C18 C 0.0573(12) 0.2461(7) 0.2070(13) 0.044(4) Uiso 0.50 1 d PD A 1 H18A H 0.0567 0.2390 0.1434 0.053 Uiso 0.50 1 calc PR A 1 H18B H 0.0137 0.2112 0.2332 0.053 Uiso 0.50 1 calc PR A 1 C19 C 0.1693(10) 0.2478(6) 0.2485(11) 0.034(3) Uiso 0.50 1 d PD A 1 H19A H 0.1701 0.2332 0.3099 0.041 Uiso 0.50 1 calc PR A 1 H19B H 0.2162 0.2179 0.2171 0.041 Uiso 0.50 1 calc PR A 1 C20 C 0.2055(11) 0.3188(7) 0.2429(15) 0.046(5) Uiso 0.50 1 d PD A 1 H20A H 0.2431 0.3327 0.2982 0.056 Uiso 0.50 1 calc PR A 1 H20B H 0.2543 0.3239 0.1956 0.056 Uiso 0.50 1 calc PR A 1 O2A O 0.1182(12) 0.3678(6) 0.2356(13) 0.0424(18) Uiso 0.50 1 d PD A 2 C17A C 0.0254(14) 0.3323(9) 0.2569(17) 0.066(7) Uiso 0.50 1 d PD A 2 H17C H -0.0375 0.3522 0.2251 0.079 Uiso 0.50 1 calc PR A 2 H17D H 0.0161 0.3367 0.3198 0.079 Uiso 0.50 1 calc PR A 2 C18A C 0.0329(13) 0.2594(8) 0.2338(15) 0.054(5) Uiso 0.50 1 d PD A 2 H18C H 0.0287 0.2308 0.2859 0.065 Uiso 0.50 1 calc PR A 2 H18D H -0.0244 0.2465 0.1903 0.065 Uiso 0.50 1 calc PR A 2 C19A C 0.1378(16) 0.2540(10) 0.1978(18) 0.088(8) Uiso 0.50 1 d PD A 2 H19C H 0.1294 0.2426 0.1353 0.105 Uiso 0.50 1 calc PR A 2 H19D H 0.1797 0.2181 0.2281 0.105 Uiso 0.50 1 calc PR A 2 C20A C 0.1943(12) 0.3197(8) 0.2096(15) 0.047(5) Uiso 0.50 1 d PD A 2 H20C H 0.2533 0.3157 0.2547 0.056 Uiso 0.50 1 calc PR A 2 H20D H 0.2238 0.3337 0.1546 0.056 Uiso 0.50 1 calc PR A 2 O3 O 0.3882(4) 0.6636(3) -0.1981(3) 0.0381(13) Uani 1 1 d . A . C21 C 0.3004(7) 0.6561(5) -0.2601(6) 0.054(2) Uani 1 1 d . . . H21A H 0.2588 0.6980 -0.2642 0.064 Uiso 1 1 calc R A . H21B H 0.2534 0.6198 -0.2417 0.064 Uiso 1 1 calc R . . C22 C 0.3389(9) 0.6403(8) -0.3431(8) 0.098(5) Uani 1 1 d . A . H22A H 0.3164 0.6748 -0.3865 0.118 Uiso 1 1 calc R . . H22B H 0.3117 0.5963 -0.3637 0.118 Uiso 1 1 calc R . . C23 C 0.4586(9) 0.6388(8) -0.3290(7) 0.094(5) Uani 1 1 d . . . H23A H 0.4850 0.5922 -0.3279 0.113 Uiso 1 1 calc R A . H23B H 0.4919 0.6634 -0.3759 0.113 Uiso 1 1 calc R . . C24 C 0.4825(7) 0.6707(6) -0.2466(6) 0.055(3) Uani 1 1 d . A . H24A H 0.4993 0.7186 -0.2549 0.066 Uiso 1 1 calc R . . H24B H 0.5441 0.6489 -0.2153 0.066 Uiso 1 1 calc R . . O4 O 0.5504(4) 0.7018(3) -0.0224(4) 0.0537(16) Uani 1 1 d D A . C25 C 0.5234(6) 0.7689(4) -0.0481(7) 0.057(3) Uani 1 1 d D . . H25A H 0.4774 0.7894 -0.0059 0.069 Uiso 1 1 calc R A . H25B H 0.4846 0.7689 -0.1060 0.069 Uiso 1 1 calc R . . C26 C 0.6233(7) 0.8073(5) -0.0513(8) 0.071(3) Uani 1 1 d D A . H26A H 0.6131 0.8546 -0.0350 0.085 Uiso 1 1 calc R . . H26B H 0.6510 0.8054 -0.1099 0.085 Uiso 1 1 calc R . . C27 C 0.6971(7) 0.7716(5) 0.0151(8) 0.068(3) Uani 1 1 d D . . H27A H 0.7689 0.7672 -0.0066 0.082 Uiso 1 1 calc R A . H27B H 0.7028 0.7969 0.0704 0.082 Uiso 1 1 calc R . . C28 C 0.6496(7) 0.7043(5) 0.0283(8) 0.073(3) Uani 1 1 d D A . H28A H 0.6977 0.6689 0.0093 0.087 Uiso 1 1 calc R . . H28B H 0.6379 0.6973 0.0905 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0262(7) 0.0318(8) 0.0332(9) 0.0021(7) 0.0046(6) -0.0037(6) K2 0.0258(7) 0.0328(8) 0.0312(8) 0.0029(7) 0.0061(6) 0.0015(6) P1 0.0232(8) 0.0215(9) 0.0261(9) 0.0001(7) 0.0017(7) 0.0005(6) P2 0.0223(8) 0.0239(9) 0.0278(9) 0.0002(7) 0.0024(7) 0.0013(7) Se1 0.0240(3) 0.0286(4) 0.0328(4) -0.0039(3) 0.0033(3) 0.0002(3) Se2 0.0248(4) 0.0370(4) 0.0393(4) 0.0001(3) 0.0076(3) 0.0011(3) Se3 0.0304(4) 0.0288(4) 0.0247(4) 0.0002(3) 0.0033(3) 0.0042(3) Se4 0.0305(4) 0.0212(3) 0.0298(4) 0.0008(3) 0.0001(3) -0.0012(3) Se5 0.0255(3) 0.0281(4) 0.0323(4) -0.0053(3) 0.0028(3) 0.0010(3) Se6 0.0233(4) 0.0434(5) 0.0438(5) -0.0007(4) 0.0056(3) -0.0045(3) C1 0.037(4) 0.028(4) 0.026(4) 0.000(3) 0.001(3) -0.008(3) C2 0.049(5) 0.032(4) 0.041(5) -0.005(4) 0.001(4) 0.009(4) C3 0.061(6) 0.031(5) 0.075(7) -0.005(5) 0.009(5) 0.002(4) C4 0.075(6) 0.021(4) 0.061(6) 0.011(4) -0.015(5) -0.012(4) C5 0.047(5) 0.041(5) 0.048(5) 0.011(4) -0.003(4) -0.015(4) C6 0.025(3) 0.038(4) 0.031(4) 0.001(3) -0.004(3) -0.005(3) C7 0.028(3) 0.032(4) 0.028(4) 0.005(3) 0.004(3) 0.008(3) C8 0.025(3) 0.035(4) 0.025(4) 0.004(3) 0.003(3) -0.003(3) C9 0.042(4) 0.036(4) 0.042(5) 0.013(4) 0.012(4) 0.007(3) C10 0.044(4) 0.043(5) 0.030(4) -0.001(4) 0.015(4) 0.008(4) C11 0.046(4) 0.045(5) 0.030(4) -0.009(4) -0.001(4) 0.008(4) C12 0.037(4) 0.032(4) 0.033(4) -0.002(3) 0.003(3) 0.005(3) O1 0.067(4) 0.068(4) 0.052(4) 0.011(3) 0.026(3) 0.022(3) C13 0.121(11) 0.189(16) 0.048(7) 0.015(9) 0.023(7) 0.104(11) C14 0.061(6) 0.113(10) 0.050(6) 0.014(6) 0.012(5) 0.023(6) C15 0.096(8) 0.100(9) 0.044(6) 0.017(6) 0.027(6) 0.058(7) C16 0.132(11) 0.182(15) 0.048(7) 0.039(8) 0.036(8) 0.115(11) O3 0.033(3) 0.056(3) 0.026(3) -0.002(2) 0.005(2) 0.007(2) C21 0.044(5) 0.082(7) 0.035(5) 0.005(5) 0.000(4) 0.000(5) C22 0.078(8) 0.169(15) 0.045(7) -0.043(8) -0.007(6) -0.002(8) C23 0.083(8) 0.168(14) 0.031(5) -0.012(7) 0.007(6) 0.058(8) C24 0.039(5) 0.095(8) 0.031(4) 0.009(5) 0.000(4) 0.004(5) O4 0.044(3) 0.042(3) 0.073(5) 0.003(3) -0.014(3) -0.010(3) C25 0.041(5) 0.049(5) 0.082(7) -0.025(5) 0.000(5) 0.006(4) C26 0.045(5) 0.045(6) 0.120(10) 0.010(6) -0.002(6) 0.002(4) C27 0.056(6) 0.050(6) 0.095(9) 0.007(6) -0.017(6) -0.012(5) C28 0.055(6) 0.059(7) 0.101(9) 0.022(6) -0.022(6) -0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O1 2.726(6) . ? K1 O2A 2.796(17) . ? K1 O2 2.834(16) . ? K1 Se1 3.3051(16) 3_565 ? K1 Se5 3.3443(16) . ? K1 Se2 3.4365(18) 3_565 ? K1 Se3 3.5577(17) . ? K1 Se1 3.6599(17) . ? K1 P1 3.747(2) . ? K1 Se2 3.7720(17) . ? K1 K1 4.260(3) 3_565 ? K2 O4 2.716(6) . ? K2 O3 2.769(6) . ? K2 Se5 3.3074(16) 3_665 ? K2 Se1 3.3403(16) . ? K2 Se6 3.5099(18) 3_665 ? K2 Se4 3.5535(17) . ? K2 Se5 3.6183(17) . ? K2 P2 3.748(2) . ? K2 Se6 3.8402(18) . ? K2 K2 4.221(3) 3_665 ? P1 C1 1.818(7) . ? P1 Se1 2.1233(19) . ? P1 Se2 2.1283(18) . ? P1 Se3 2.285(2) . ? P2 C7 1.839(7) . ? P2 Se5 2.1192(19) . ? P2 Se6 2.1309(18) . ? P2 Se4 2.2889(18) . ? Se1 K1 3.3051(16) 3_565 ? Se2 K1 3.4365(18) 3_565 ? Se3 Se4 2.3364(10) . ? Se5 K2 3.3073(16) 3_665 ? Se6 K2 3.5099(18) 3_665 ? C1 C2 1.382(10) . ? C1 C6 1.388(10) . ? C2 C3 1.356(12) . ? C3 C4 1.372(13) . ? C4 C5 1.383(13) . ? C5 C6 1.398(10) . ? C7 C8 1.371(9) . ? C7 C12 1.378(10) . ? C8 C9 1.398(10) . ? C9 C10 1.360(12) . ? C10 C11 1.397(12) . ? C11 C12 1.368(11) . ? O1 C13 1.361(13) . ? O1 C16 1.432(12) . ? C13 C14 1.418(14) . ? C14 C15 1.447(14) . ? C15 C16 1.452(14) . ? O2 C20 1.438(14) . ? O2 C17 1.453(13) . ? C17 C18 1.490(16) . ? C18 C19 1.516(15) . ? C19 C20 1.496(15) . ? O2A C17A 1.426(14) . ? O2A C20A 1.434(14) . ? C17A C18A 1.504(17) . ? C18A C19A 1.474(16) . ? C19A C20A 1.501(16) . ? O3 C21 1.426(10) . ? O3 C24 1.454(9) . ? C21 C22 1.433(14) . ? C22 C23 1.515(16) . ? C23 C24 1.437(14) . ? O4 C25 1.433(9) . ? O4 C28 1.435(9) . ? C25 C26 1.481(11) . ? C26 C27 1.519(12) . ? C27 C28 1.492(11) . ? 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 K1 O2A 78.4(4) . . ? O1 K1 O2 81.2(4) . . ? O2A K1 O2 4.9(7) . . ? O1 K1 Se1 78.79(16) . 3_565 ? O2A K1 Se1 96.1(3) . 3_565 ? O2 K1 Se1 92.8(3) . 3_565 ? O1 K1 Se5 131.19(17) . . ? O2A K1 Se5 82.5(3) . . ? O2 K1 Se5 83.4(3) . . ? Se1 K1 Se5 148.14(6) 3_565 . ? O1 K1 Se2 140.16(17) . 3_565 ? O2A K1 Se2 88.6(4) . 3_565 ? O2 K1 Se2 84.0(4) . 3_565 ? Se1 K1 Se2 65.18(3) 3_565 3_565 ? Se5 K1 Se2 82.96(4) . 3_565 ? O1 K1 Se3 78.95(16) . . ? O2A K1 Se3 123.9(3) . . ? O2 K1 Se3 128.7(3) . . ? Se1 K1 Se3 128.25(5) 3_565 . ? Se5 K1 Se3 75.46(3) . . ? Se2 K1 Se3 136.94(5) 3_565 . ? O1 K1 Se1 132.37(15) . . ? O2A K1 Se1 145.2(3) . . ? O2 K1 Se1 144.1(3) . . ? Se1 K1 Se1 104.79(4) 3_565 . ? Se5 K1 Se1 65.13(3) . . ? Se2 K1 Se1 75.76(4) 3_565 . ? Se3 K1 Se1 61.43(3) . . ? O1 K1 P1 99.16(15) . . ? O2A K1 P1 158.9(3) . . ? O2 K1 P1 163.0(3) . . ? Se1 K1 P1 104.03(5) 3_565 . ? Se5 K1 P1 83.71(4) . . ? Se2 K1 P1 105.35(5) 3_565 . ? Se3 K1 P1 36.35(3) . . ? Se1 K1 P1 33.29(3) . . ? O1 K1 Se2 77.53(14) . . ? O2A K1 Se2 155.7(3) . . ? O2 K1 Se2 157.4(3) . . ? Se1 K1 Se2 75.75(4) 3_565 . ? Se5 K1 Se2 116.60(4) . . ? Se2 K1 Se2 107.73(4) 3_565 . ? Se3 K1 Se2 54.05(3) . . ? Se1 K1 Se2 58.50(3) . . ? P1 K1 Se2 32.88(3) . . ? O1 K1 K1 115.35(16) . 3_565 ? O2A K1 K1 142.0(4) . 3_565 ? O2 K1 K1 137.1(4) . 3_565 ? Se1 K1 K1 56.18(4) 3_565 3_565 ? Se5 K1 K1 107.31(6) . 3_565 ? Se2 K1 K1 57.51(4) 3_565 3_565 ? Se3 K1 K1 93.99(5) . 3_565 ? Se1 K1 K1 48.61(3) . 3_565 ? P1 K1 K1 57.99(4) . 3_565 ? Se2 K1 K1 50.22(3) . 3_565 ? O4 K2 O3 76.07(18) . . ? O4 K2 Se5 79.73(14) . 3_665 ? O3 K2 Se5 96.22(11) . 3_665 ? O4 K2 Se1 129.26(14) . . ? O3 K2 Se1 82.93(11) . . ? Se5 K2 Se1 148.98(6) 3_665 . ? O4 K2 Se6 139.44(15) . 3_665 ? O3 K2 Se6 89.07(12) . 3_665 ? Se5 K2 Se6 64.41(3) 3_665 3_665 ? Se1 K2 Se6 84.58(4) . 3_665 ? O4 K2 Se4 78.07(15) . . ? O3 K2 Se4 121.57(12) . . ? Se5 K2 Se4 128.97(5) 3_665 . ? Se1 K2 Se4 74.73(3) . . ? Se6 K2 Se4 139.43(5) 3_665 . ? O4 K2 Se5 132.27(15) . . ? O3 K2 Se5 146.73(12) . . ? Se5 K2 Se5 105.04(4) 3_665 . ? Se1 K2 Se5 65.65(3) . . ? Se6 K2 Se5 77.81(4) 3_665 . ? Se4 K2 Se5 61.96(3) . . ? O4 K2 P2 98.98(15) . . ? O3 K2 P2 157.05(12) . . ? Se5 K2 P2 105.02(5) 3_665 . ? Se1 K2 P2 83.27(4) . . ? Se6 K2 P2 107.76(5) 3_665 . ? Se4 K2 P2 36.41(3) . . ? Se5 K2 P2 33.38(3) . . ? O4 K2 Se6 77.63(14) . . ? O3 K2 Se6 153.64(12) . . ? Se5 K2 Se6 77.18(3) 3_665 . ? Se1 K2 Se6 115.85(4) . . ? Se6 K2 Se6 110.06(4) 3_665 . ? Se4 K2 Se6 53.44(3) . . ? Se5 K2 Se6 58.28(3) . . ? P2 K2 Se6 32.59(3) . . ? O4 K2 K2 115.90(14) . 3_665 ? O3 K2 K2 143.28(13) . 3_665 ? Se5 K2 K2 55.87(3) 3_665 3_665 ? Se1 K2 K2 108.54(6) . 3_665 ? Se6 K2 K2 58.71(4) 3_665 3_665 ? Se4 K2 K2 95.15(5) . 3_665 ? Se5 K2 K2 49.17(3) . 3_665 ? P2 K2 K2 59.15(4) . 3_665 ? Se6 K2 K2 51.36(4) . 3_665 ? C1 P1 Se1 110.7(2) . . ? C1 P1 Se2 110.9(2) . . ? Se1 P1 Se2 117.39(8) . . ? C1 P1 Se3 104.9(2) . . ? Se1 P1 Se3 113.50(8) . . ? Se2 P1 Se3 98.14(8) . . ? C1 P1 K1 171.6(2) . . ? Se1 P1 K1 71.11(5) . . ? Se2 P1 K1 74.21(6) . . ? Se3 P1 K1 67.32(5) . . ? C7 P2 Se5 110.9(2) . . ? C7 P2 Se6 111.9(2) . . ? Se5 P2 Se6 117.69(9) . . ? C7 P2 Se4 103.2(2) . . ? Se5 P2 Se4 113.70(8) . . ? Se6 P2 Se4 97.89(7) . . ? C7 P2 K2 168.8(2) . . ? Se5 P2 K2 69.95(6) . . ? Se6 P2 K2 76.08(6) . . ? Se4 P2 K2 67.16(5) . . ? P1 Se1 K1 89.31(6) . 3_565 ? P1 Se1 K2 109.75(6) . . ? K1 Se1 K2 160.47(5) 3_565 . ? P1 Se1 K1 75.60(6) . . ? K1 Se1 K1 75.21(4) 3_565 . ? K2 Se1 K1 112.79(4) . . ? P1 Se2 K1 85.78(6) . 3_565 ? P1 Se2 K1 72.90(5) . . ? K1 Se2 K1 72.27(4) 3_565 . ? P1 Se3 Se4 105.21(5) . . ? P1 Se3 K1 76.34(5) . . ? Se4 Se3 K1 110.55(4) . . ? P2 Se4 Se3 104.82(5) . . ? P2 Se4 K2 76.43(6) . . ? Se3 Se4 K2 111.62(4) . . ? P2 Se5 K2 90.86(6) . 3_665 ? P2 Se5 K1 107.38(6) . . ? K2 Se5 K1 161.00(4) 3_665 . ? P2 Se5 K2 76.68(6) . . ? K2 Se5 K2 74.96(4) 3_665 . ? K1 Se5 K2 113.75(4) . . ? P2 Se6 K2 85.32(6) . 3_665 ? P2 Se6 K2 71.33(6) . . ? K2 Se6 K2 69.94(4) 3_665 . ? C2 C1 C6 119.9(7) . . ? C2 C1 P1 119.8(6) . . ? C6 C1 P1 120.3(6) . . ? C3 C2 C1 118.6(8) . . ? C2 C3 C4 123.1(9) . . ? C3 C4 C5 119.0(8) . . ? C4 C5 C6 118.9(8) . . ? C1 C6 C5 120.4(7) . . ? C8 C7 C12 120.9(7) . . ? C8 C7 P2 120.1(6) . . ? C12 C7 P2 119.0(6) . . ? C7 C8 C9 117.8(7) . . ? C10 C9 C8 122.4(7) . . ? C9 C10 C11 118.3(7) . . ? C12 C11 C10 120.3(8) . . ? C11 C12 C7 120.3(7) . . ? C13 O1 C16 105.9(8) . . ? C13 O1 K1 128.9(6) . . ? C16 O1 K1 123.2(6) . . ? O1 C13 C14 111.1(9) . . ? C13 C14 C15 105.0(9) . . ? C14 C15 C16 102.8(9) . . ? O1 C16 C15 107.2(9) . . ? C20 O2 C17 107.0(10) . . ? C20 O2 K1 132.1(11) . . ? C17 O2 K1 114.6(10) . . ? O2 C17 C18 107.6(10) . . ? C17 C18 C19 100.0(10) . . ? C20 C19 C18 106.0(11) . . ? O2 C20 C19 107.0(10) . . ? C17A O2A C20A 107.9(11) . . ? C17A O2A K1 113.2(13) . . ? C20A O2A K1 117.0(13) . . ? O2A C17A C18A 111.2(12) . . ? C19A C18A C17A 103.4(12) . . ? C18A C19A C20A 108.7(12) . . ? O2A C20A C19A 107.4(11) . . ? C21 O3 C24 107.1(6) . . ? C21 O3 K2 127.3(5) . . ? C24 O3 K2 111.1(4) . . ? O3 C21 C22 109.1(8) . . ? C21 C22 C23 105.6(9) . . ? C24 C23 C22 105.6(8) . . ? C23 C24 O3 106.2(8) . . ? C25 O4 C28 107.6(6) . . ? C25 O4 K2 127.7(5) . . ? C28 O4 K2 124.5(5) . . ? O4 C25 C26 107.8(7) . . ? C25 C26 C27 102.8(8) . . ? C28 C27 C26 106.2(7) . . ? O4 C28 C27 107.6(7) . . ? _diffrn_measured_fraction_theta_max 0.672 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.528 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.279 data_4 _database_code_depnum_ccdc_archive 'CCDC 292993' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H42 O4 P2 Rb2 Se6' _chemical_formula_weight 1149.26 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' 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' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.0598(12) _cell_length_b 23.1403(15) _cell_length_c 13.4145(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.154(6) _cell_angle_gamma 90.00 _cell_volume 4042.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9262 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 54.13 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 7.932 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3634 _exptl_absorpt_correction_T_max 0.6475 _exptl_absorpt_process_details 'stoe X-red' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe ipds2' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13034 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.08 _reflns_number_total 4419 _reflns_number_gt 2760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe x-area' _computing_cell_refinement 'stoe x-area' _computing_data_reduction 'stoe x-area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^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 4419 _refine_ls_number_parameters 154 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.39552(14) 0.37794(7) 0.37381(14) 0.0472(4) Uani 1 1 d . . . Rb1 Rb 0.36975(6) 0.47512(3) 0.03690(6) 0.0575(2) Uani 1 1 d . . . Se1 Se 0.35556(7) 0.45841(3) 0.29191(6) 0.0590(2) Uani 1 1 d . . . Se2 Se 0.46138(7) 0.37891(3) 0.54580(6) 0.0600(2) Uani 1 1 d . . . Se3 Se 0.52524(6) 0.33066(3) 0.34399(6) 0.05107(19) Uani 1 1 d . . . C1 C 0.2896(6) 0.3263(3) 0.3256(6) 0.0571(18) Uani 1 1 d . . . C2 C 0.2913(8) 0.2767(4) 0.3842(8) 0.078(3) Uani 1 1 d . . . H2 H 0.3472 0.2694 0.4501 0.094 Uiso 1 1 calc R . . C3 C 0.2096(11) 0.2375(5) 0.3451(11) 0.100(4) Uani 1 1 d . . . H3 H 0.2103 0.2037 0.3857 0.120 Uiso 1 1 calc R . . C4 C 0.1339(10) 0.2460(7) 0.2555(14) 0.115(5) Uani 1 1 d . . . H4 H 0.0817 0.2175 0.2297 0.138 Uiso 1 1 calc R . . C5 C 0.1266(9) 0.2947(6) 0.1969(13) 0.126(5) Uani 1 1 d . . . H5 H 0.0682 0.3014 0.1330 0.151 Uiso 1 1 calc R . . C6 C 0.2080(7) 0.3357(4) 0.2327(9) 0.091(3) Uani 1 1 d . . . H6 H 0.2052 0.3696 0.1916 0.109 Uiso 1 1 calc R . . O1 O 0.2277(12) 0.3950(6) -0.0831(12) 0.090(3) Uiso 0.50 1 d PD A 1 C7 C 0.174(2) 0.3722(10) -0.034(2) 0.131(7) Uiso 0.50 1 d PD A 1 H7A H 0.1053 0.3909 -0.0600 0.158 Uiso 0.50 1 calc PR A 1 H7B H 0.2075 0.3797 0.0438 0.158 Uiso 0.50 1 calc PR A 1 C8 C 0.161(2) 0.3137(10) -0.051(2) 0.134(7) Uiso 0.50 1 d PD A 1 H8A H 0.1942 0.2926 0.0173 0.161 Uiso 0.50 1 calc PR A 1 H8B H 0.0875 0.3037 -0.0822 0.161 Uiso 0.50 1 calc PR A 1 C9 C 0.2069(19) 0.2996(8) -0.1213(19) 0.103(5) Uiso 0.50 1 d PD A 1 H9A H 0.1564 0.2817 -0.1869 0.124 Uiso 0.50 1 calc PR A 1 H9B H 0.2635 0.2719 -0.0875 0.124 Uiso 0.50 1 calc PR A 1 C10 C 0.246(2) 0.3516(9) -0.148(2) 0.124(6) Uiso 0.50 1 d PD A 1 H10A H 0.3200 0.3480 -0.1323 0.148 Uiso 0.50 1 calc PR A 1 H10B H 0.2096 0.3608 -0.2250 0.148 Uiso 0.50 1 calc PR A 1 O1A O 0.1988(12) 0.4038(6) -0.1234(11) 0.090(3) Uiso 0.50 1 d PD A 2 C7A C 0.125(2) 0.3866(10) -0.091(2) 0.131(7) Uiso 0.50 1 d PD A 2 H7A1 H 0.0645 0.4119 -0.1231 0.158 Uiso 0.50 1 calc PR A 2 H7A2 H 0.1495 0.3898 -0.0119 0.158 Uiso 0.50 1 calc PR A 2 C8A C 0.097(2) 0.3288(10) -0.122(2) 0.134(7) Uiso 0.50 1 d PD A 2 H8A1 H 0.1085 0.3043 -0.0584 0.161 Uiso 0.50 1 calc PR A 2 H8A2 H 0.0241 0.3264 -0.1706 0.161 Uiso 0.50 1 calc PR A 2 C9A C 0.1583(19) 0.3118(8) -0.1738(19) 0.103(5) Uiso 0.50 1 d PD A 2 H9A1 H 0.1198 0.2875 -0.2369 0.124 Uiso 0.50 1 calc PR A 2 H9A2 H 0.2179 0.2896 -0.1251 0.124 Uiso 0.50 1 calc PR A 2 C10A C 0.1913(6) 0.3654(3) -0.2070(6) 0.124(6) Uiso 0.50 1 d PD A 2 H10C H 0.2585 0.3607 -0.2141 0.148 Uiso 0.50 1 calc PR A 2 H10D H 0.1402 0.3791 -0.2765 0.148 Uiso 0.50 1 calc PR A 2 O2 O 0.1719(6) 0.5205(3) 0.0060(6) 0.130(3) Uani 1 1 d D A . C11 C 0.1113(6) 0.5369(3) -0.0966(6) 0.175(7) Uiso 1 1 d D A . H11A H 0.0550 0.5087 -0.1279 0.210 Uiso 1 1 calc R . . H11B H 0.1527 0.5377 -0.1421 0.210 Uiso 1 1 calc R . . C12 C 0.0708(19) 0.5911(8) -0.0945(17) 0.228(10) Uiso 1 1 d D . . H12A H 0.0869 0.6176 -0.1440 0.273 Uiso 1 1 calc R A . H12B H -0.0048 0.5888 -0.1171 0.273 Uiso 1 1 calc R . . C13 C 0.1135(18) 0.6104(8) 0.0069(16) 0.210(9) Uiso 1 1 d D A . H13A H 0.0596 0.6233 0.0326 0.252 Uiso 1 1 calc R . . H13B H 0.1595 0.6435 0.0109 0.252 Uiso 1 1 calc R . . C14 C 0.1720(12) 0.5627(6) 0.0731(11) 0.141(5) Uiso 1 1 d D A . H14A H 0.2431 0.5750 0.1160 0.169 Uiso 1 1 calc R . . H14B H 0.1396 0.5494 0.1231 0.169 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0503(10) 0.0430(9) 0.0518(9) 0.0023(8) 0.0233(8) 0.0006(8) Rb1 0.0603(4) 0.0557(4) 0.0625(4) 0.0108(3) 0.0299(3) 0.0052(3) Se1 0.0800(6) 0.0499(4) 0.0544(4) 0.0088(3) 0.0339(4) 0.0163(4) Se2 0.0728(5) 0.0570(4) 0.0484(4) 0.0066(3) 0.0209(4) -0.0031(4) Se3 0.0483(4) 0.0456(4) 0.0631(4) 0.0070(3) 0.0254(3) 0.0048(3) C1 0.052(4) 0.058(4) 0.069(5) -0.016(4) 0.032(4) -0.001(3) C2 0.094(7) 0.076(6) 0.085(6) -0.021(5) 0.057(5) -0.035(5) C3 0.128(10) 0.089(7) 0.120(9) -0.042(7) 0.089(9) -0.057(7) C4 0.071(8) 0.124(11) 0.172(14) -0.078(11) 0.073(9) -0.045(8) C5 0.060(7) 0.109(10) 0.183(14) -0.056(10) 0.016(8) 0.002(7) C6 0.060(6) 0.073(6) 0.121(8) -0.016(6) 0.013(6) -0.003(5) O2 0.130(7) 0.147(7) 0.102(5) 0.034(5) 0.031(5) 0.069(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.826(8) . ? P1 Se1 2.1271(19) . ? P1 Se2 2.1376(19) . ? P1 Se3 2.2876(19) . ? P1 Rb1 3.795(2) 2_655 ? Rb1 O1 2.755(14) . ? Rb1 O2 2.854(7) . ? Rb1 O1A 3.037(13) . ? Rb1 C7 3.49(3) . ? Rb1 Se1 3.5223(10) . ? Rb1 Se1 3.5654(10) 6_565 ? Rb1 Se2 3.6010(11) 6_565 ? Rb1 C14 3.619(15) . ? Rb1 C11 3.681(7) . ? Rb1 Se1 3.6944(12) 2_655 ? Rb1 Se2 3.7162(11) 2_655 ? Rb1 Se3 3.7587(10) 2_655 ? Se1 Rb1 3.5653(10) 6_566 ? Se1 Rb1 3.6944(12) 2_655 ? Se2 Rb1 3.6010(11) 6_566 ? Se2 Rb1 3.7161(11) 2_655 ? Se3 Se3 2.3480(15) 2_655 ? Se3 Rb1 3.7586(10) 2_655 ? C1 C6 1.356(12) . ? C1 C2 1.387(12) . ? C2 C3 1.401(14) . ? C3 C4 1.286(18) . ? C4 C5 1.355(19) . ? C5 C6 1.423(16) . ? O1 C7 1.287(15) . ? O1 C10 1.411(16) . ? C7 C8 1.373(19) . ? C8 C9 1.359(19) . ? C9 C10 1.419(18) . ? O1A C7A 1.323(15) . ? O1A C10A 1.403(13) . ? C7A C8A 1.411(19) . ? C8A C9A 1.347(19) . ? C9A C10A 1.453(17) . ? O2 C14 1.328(13) . ? O2 C11 1.3706 . ? C11 C12 1.382(17) . ? C12 C13 1.340(18) . ? C13 C14 1.460(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 Se1 111.6(3) . . ? C1 P1 Se2 110.6(3) . . ? Se1 P1 Se2 118.08(9) . . ? C1 P1 Se3 102.9(2) . . ? Se1 P1 Se3 113.65(8) . . ? Se2 P1 Se3 98.30(8) . . ? C1 P1 Rb1 174.3(2) . 2_655 ? Se1 P1 Rb1 70.92(5) . 2_655 ? Se2 P1 Rb1 71.45(5) . 2_655 ? Se3 P1 Rb1 71.51(5) . 2_655 ? O1 Rb1 O2 73.2(4) . . ? O1 Rb1 O1A 10.0(4) . . ? O2 Rb1 O1A 68.2(3) . . ? O1 Rb1 C7 19.6(4) . . ? O2 Rb1 C7 65.5(5) . . ? O1A Rb1 C7 26.3(5) . . ? O1 Rb1 Se1 101.5(3) . . ? O2 Rb1 Se1 76.85(15) . . ? O1A Rb1 Se1 108.0(3) . . ? C7 Rb1 Se1 82.1(4) . . ? O1 Rb1 Se1 88.6(3) . 6_565 ? O2 Rb1 Se1 89.69(15) . 6_565 ? O1A Rb1 Se1 80.1(3) . 6_565 ? C7 Rb1 Se1 106.1(5) . 6_565 ? Se1 Rb1 Se1 159.82(3) . 6_565 ? O1 Rb1 Se2 145.3(3) . 6_565 ? O2 Rb1 Se2 88.66(16) . 6_565 ? O1A Rb1 Se2 135.3(3) . 6_565 ? C7 Rb1 Se2 152.2(5) . 6_565 ? Se1 Rb1 Se2 102.79(3) . 6_565 ? Se1 Rb1 Se2 61.369(19) 6_565 6_565 ? O1 Rb1 C14 91.8(4) . . ? O2 Rb1 C14 19.5(3) . . ? O1A Rb1 C14 87.5(3) . . ? C7 Rb1 C14 81.5(5) . . ? Se1 Rb1 C14 66.6(2) . . ? Se1 Rb1 C14 95.9(2) 6_565 . ? Se2 Rb1 C14 75.7(3) 6_565 . ? O1 Rb1 C11 67.2(3) . . ? O2 Rb1 C11 19.42(5) . . ? O1A Rb1 C11 59.6(3) . . ? C7 Rb1 C11 66.4(5) . . ? Se1 Rb1 C11 96.20(12) . . ? Se1 Rb1 C11 71.46(12) 6_565 . ? Se2 Rb1 C11 85.80(13) 6_565 . ? C14 Rb1 C11 34.9(2) . . ? O1 Rb1 Se1 130.6(3) . 2_655 ? O2 Rb1 Se1 149.56(16) . 2_655 ? O1A Rb1 Se1 138.2(3) . 2_655 ? C7 Rb1 Se1 129.1(5) . 2_655 ? Se1 Rb1 Se1 79.26(3) . 2_655 ? Se1 Rb1 Se1 107.46(2) 6_565 2_655 ? Se2 Rb1 Se1 78.49(2) 6_565 2_655 ? C14 Rb1 Se1 130.6(2) . 2_655 ? C11 Rb1 Se1 162.14(13) . 2_655 ? O1 Rb1 Se2 80.0(3) . 2_655 ? O2 Rb1 Se2 150.99(16) . 2_655 ? O1A Rb1 Se2 83.5(3) . 2_655 ? C7 Rb1 Se2 92.1(4) . 2_655 ? Se1 Rb1 Se2 120.05(3) . 2_655 ? Se1 Rb1 Se2 78.66(2) 6_565 2_655 ? Se2 Rb1 Se2 108.12(2) 6_565 2_655 ? C14 Rb1 Se2 170.2(2) . 2_655 ? C11 Rb1 Se2 135.42(12) . 2_655 ? Se1 Rb1 Se2 59.14(2) 2_655 2_655 ? O1 Rb1 Se3 74.5(3) . 2_655 ? O2 Rb1 Se3 126.45(16) . 2_655 ? O1A Rb1 Se3 84.1(3) . 2_655 ? C7 Rb1 Se3 69.7(5) . 2_655 ? Se1 Rb1 Se3 69.30(2) . 2_655 ? Se1 Rb1 Se3 130.69(3) 6_565 2_655 ? Se2 Rb1 Se3 137.89(3) 6_565 2_655 ? C14 Rb1 Se3 129.8(2) . 2_655 ? C11 Rb1 Se3 135.23(13) . 2_655 ? Se1 Rb1 Se3 59.454(19) 2_655 2_655 ? Se2 Rb1 Se3 53.227(19) 2_655 2_655 ? P1 Se1 Rb1 119.80(5) . . ? P1 Se1 Rb1 89.40(5) . 6_566 ? Rb1 Se1 Rb1 147.56(2) . 6_566 ? P1 Se1 Rb1 76.11(6) . 2_655 ? Rb1 Se1 Rb1 99.41(3) . 2_655 ? Rb1 Se1 Rb1 72.54(2) 6_566 2_655 ? P1 Se2 Rb1 88.29(5) . 6_566 ? P1 Se2 Rb1 75.50(5) . 2_655 ? Rb1 Se2 Rb1 71.88(2) 6_566 2_655 ? P1 Se3 Se3 104.47(6) . 2_655 ? P1 Se3 Rb1 73.24(5) . 2_655 ? Se3 Se3 Rb1 111.576(19) 2_655 2_655 ? C6 C1 C2 118.8(8) . . ? C6 C1 P1 121.0(7) . . ? C2 C1 P1 120.2(7) . . ? C1 C2 C3 119.2(11) . . ? C4 C3 C2 121.6(12) . . ? C3 C4 C5 121.7(12) . . ? C4 C5 C6 118.9(13) . . ? C1 C6 C5 119.8(11) . . ? C7 O1 C10 107.2(13) . . ? C7 O1 Rb1 114.6(15) . . ? C10 O1 Rb1 125.5(13) . . ? O1 C7 C8 112.5(16) . . ? O1 C7 Rb1 45.8(12) . . ? C8 C7 Rb1 139(2) . . ? C9 C8 C7 106.7(17) . . ? C8 C9 C10 107.1(15) . . ? O1 C10 C9 106.0(14) . . ? C7A O1A C10A 103.8(12) . . ? C7A O1A Rb1 116.1(13) . . ? C10A O1A Rb1 135.3(9) . . ? O1A C7A C8A 110.7(16) . . ? C9A C8A C7A 105.6(17) . . ? C8A C9A C10A 104.2(15) . . ? O1A C10A C9A 103.4(10) . . ? C14 O2 C11 108.6(7) . . ? C14 O2 Rb1 114.8(8) . . ? C11 O2 Rb1 116.78(15) . . ? O2 C11 C12 109.7(10) . . ? O2 C11 Rb1 43.81(12) . . ? C12 C11 Rb1 133.0(11) . . ? C13 C12 C11 107.0(15) . . ? C12 C13 C14 107.5(15) . . ? O2 C14 C13 106.7(11) . . ? O2 C14 Rb1 45.7(6) . . ? C13 C14 Rb1 128.8(12) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.668 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.112