Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'J. Woollins' 'Ian P. Gray' 'A. Slawin' _publ_contact_author_name 'Prof J Woollins' _publ_contact_author_address ; School of Chemistry St Andrews University The Purdie Building St Andrews Fife KY16 9ST U.K. ; _publ_contact_author_email JDW3@ST-ANDREWS.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Structure of Novel [Ph(RO)PSe2]- Complexes ; data_igdw45 _database_code_depnum_ccdc_archive 'CCDC 266255' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 O4 P4 Pb2 Se8' _chemical_formula_weight 1602.48 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' Pb Pb -3.3944 10.1111 '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 17.309(4) _cell_length_b 6.4914(10) _cell_length_c 18.073(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.072(5) _cell_angle_gamma 90.00 _cell_volume 2029.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 7349 _cell_measurement_theta_min 2.2553 _cell_measurement_theta_max 25.3491 _exptl_crystal_description needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 2.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 15.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7217 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optic' _diffrn_measurement_device_type ccd _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time ? _diffrn_standards_decay_% - _diffrn_reflns_number 12314 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3650 _reflns_number_gt 3457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+2.1440P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3650 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0194 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_ref 0.0395 _refine_ls_wR_factor_gt 0.0387 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 Pb1 Pb 0.630722(7) -0.450532(17) -0.030503(7) 0.01402(5) Uani 1 1 d . . . Se1 Se 0.545671(18) -0.34431(4) -0.161632(18) 0.01594(8) Uani 1 1 d . . . Se2 Se 0.493660(17) -0.79233(4) -0.056102(17) 0.01352(8) Uani 1 1 d . . . P1 P 0.47084(5) -0.61024(12) -0.15443(5) 0.01243(17) Uani 1 1 d . . . C1 C 0.37022(19) -0.5368(5) -0.15950(18) 0.0143(7) Uani 1 1 d . . . C2 C 0.31448(19) -0.6906(5) -0.1716(2) 0.0223(8) Uani 1 1 d . . . H2A H 0.3301 -0.8280 -0.1812 0.027 Uiso 1 1 calc R . . C3 C 0.2366(2) -0.6428(6) -0.1696(2) 0.0269(8) Uani 1 1 d . . . H3A H 0.1988 -0.7467 -0.1786 0.032 Uiso 1 1 calc R . . C4 C 0.2141(2) -0.4419(5) -0.1545(2) 0.0256(9) Uani 1 1 d . . . H4A H 0.1607 -0.4090 -0.1526 0.031 Uiso 1 1 calc R . . C5 C 0.2692(2) -0.2894(6) -0.1421(2) 0.0255(8) Uani 1 1 d . . . H5A H 0.2534 -0.1526 -0.1318 0.031 Uiso 1 1 calc R . . C6 C 0.3470(2) -0.3354(5) -0.14467(19) 0.0207(8) Uani 1 1 d . . . H6A H 0.3846 -0.2304 -0.1364 0.025 Uiso 1 1 calc R . . O1 O 0.47503(12) -0.7498(3) -0.22729(12) 0.0169(5) Uani 1 1 d . . . C7 C 0.5488(2) -0.8394(5) -0.2456(2) 0.0219(8) Uani 1 1 d . . . H7A H 0.5784 -0.7395 -0.2738 0.033 Uiso 1 1 calc R . . H7B H 0.5399 -0.9637 -0.2755 0.033 Uiso 1 1 calc R . . H7C H 0.5779 -0.8754 -0.1999 0.033 Uiso 1 1 calc R . . Se11 Se 0.691441(18) -0.03848(4) -0.034506(19) 0.01522(8) Uani 1 1 d . . . Se12 Se 0.785421(18) -0.48842(5) -0.106725(19) 0.01567(8) Uani 1 1 d . . . P11 P 0.79878(4) -0.17595(11) -0.06931(5) 0.01152(17) Uani 1 1 d . . . C11 C 0.87319(17) -0.1539(5) 0.00316(18) 0.0131(7) Uani 1 1 d . . . C12 C 0.8870(2) 0.0389(5) 0.0359(2) 0.0202(8) Uani 1 1 d . . . H12A H 0.8590 0.1566 0.0189 0.024 Uiso 1 1 calc R . . C13 C 0.9416(2) 0.0566(5) 0.0933(2) 0.0218(8) Uani 1 1 d . . . H13A H 0.9507 0.1871 0.1157 0.026 Uiso 1 1 calc R . . C14 C 0.98330(19) -0.1138(6) 0.1186(2) 0.0232(8) Uani 1 1 d . . . H14A H 1.0201 -0.1005 0.1586 0.028 Uiso 1 1 calc R . . C15 C 0.9707(2) -0.3028(5) 0.0851(2) 0.0240(8) Uani 1 1 d . . . H15A H 1.0000 -0.4192 0.1013 0.029 Uiso 1 1 calc R . . C16 C 0.91513(19) -0.3235(5) 0.02760(19) 0.0197(7) Uani 1 1 d . . . H16A H 0.9062 -0.4542 0.0053 0.024 Uiso 1 1 calc R . . O11 O 0.83466(13) -0.0315(3) -0.13128(12) 0.0148(5) Uani 1 1 d . . . C17 C 0.7894(2) 0.0115(5) -0.19846(19) 0.0203(7) Uani 1 1 d . . . H17A H 0.7766 -0.1181 -0.2239 0.030 Uiso 1 1 calc R . . H17B H 0.8193 0.0992 -0.2310 0.030 Uiso 1 1 calc R . . H17C H 0.7416 0.0826 -0.1860 0.030 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 Pb1 0.01370(8) 0.01706(8) 0.01132(8) 0.00131(4) 0.00060(5) -0.00343(4) Se1 0.01965(18) 0.01484(17) 0.01323(18) 0.00371(12) -0.00070(14) -0.00475(12) Se2 0.01431(16) 0.01280(16) 0.01354(18) 0.00375(12) 0.00150(13) -0.00055(11) P1 0.0139(4) 0.0127(4) 0.0107(4) -0.0001(3) 0.0010(3) -0.0011(3) C1 0.0161(17) 0.0200(17) 0.0066(17) 0.0023(12) -0.0014(13) 0.0002(12) C2 0.0222(19) 0.0221(18) 0.023(2) -0.0014(14) 0.0003(16) -0.0017(14) C3 0.0197(19) 0.036(2) 0.025(2) 0.0039(16) -0.0004(16) -0.0048(15) C4 0.0183(19) 0.038(2) 0.021(2) 0.0071(15) 0.0034(16) 0.0067(15) C5 0.025(2) 0.0275(19) 0.024(2) 0.0039(15) 0.0016(16) 0.0089(15) C6 0.0229(19) 0.0222(18) 0.017(2) 0.0040(14) -0.0019(15) -0.0014(14) O1 0.0188(12) 0.0211(12) 0.0109(12) -0.0042(9) 0.0017(9) -0.0019(9) C7 0.0250(19) 0.0220(18) 0.019(2) -0.0025(14) 0.0070(16) 0.0022(14) Se11 0.01099(16) 0.01472(17) 0.0201(2) -0.00466(12) 0.00308(14) -0.00070(11) Se12 0.01555(17) 0.01464(16) 0.01685(19) -0.00483(12) 0.00098(14) -0.00012(12) P11 0.0104(4) 0.0131(4) 0.0111(4) -0.0008(3) 0.0006(3) -0.0010(3) C11 0.0099(16) 0.0196(17) 0.0099(17) 0.0024(13) 0.0013(13) -0.0018(12) C12 0.0203(18) 0.0167(18) 0.023(2) -0.0037(13) -0.0026(15) -0.0001(13) C13 0.0182(18) 0.0228(19) 0.024(2) -0.0065(14) -0.0025(16) -0.0051(13) C14 0.0145(18) 0.038(2) 0.017(2) 0.0006(16) -0.0013(15) -0.0045(15) C15 0.0229(19) 0.0244(19) 0.024(2) 0.0068(15) -0.0034(16) 0.0027(14) C16 0.0200(18) 0.0184(17) 0.020(2) 0.0026(13) -0.0023(15) -0.0028(13) O11 0.0154(12) 0.0174(12) 0.0115(13) 0.0029(9) 0.0014(10) -0.0035(8) C17 0.0184(18) 0.0279(18) 0.0142(19) 0.0050(14) -0.0051(15) -0.0016(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 Se1 2.8296(6) . ? Pb1 Se11 2.8757(5) . ? Pb1 Se12 3.0651(6) . ? Pb1 Se2 3.1327(5) 3_645 ? Pb1 Se2 3.2689(5) . ? Se1 P1 2.1649(9) . ? Se2 P1 2.1589(9) . ? Se2 Pb1 3.1327(5) 3_645 ? P1 O1 1.602(2) . ? P1 C1 1.805(3) . ? C1 C6 1.396(5) . ? C1 C2 1.400(4) . ? C2 C3 1.385(5) . ? C3 C4 1.391(5) . ? C4 C5 1.387(5) . ? C5 C6 1.382(5) . ? O1 C7 1.452(4) . ? Se11 P11 2.1745(9) . ? Se12 P11 2.1480(9) . ? P11 O11 1.603(2) . ? P11 C11 1.809(3) . ? C11 C16 1.383(4) . ? C11 C12 1.401(5) . ? C12 C13 1.382(5) . ? C13 C14 1.390(5) . ? C14 C15 1.382(5) . ? C15 C16 1.397(5) . ? O11 C17 1.448(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se1 Pb1 Se11 86.090(11) . . ? Se1 Pb1 Se12 94.568(17) . . ? Se11 Pb1 Se12 74.772(11) . . ? Se1 Pb1 Se2 87.116(17) . 3_645 ? Se11 Pb1 Se2 78.631(13) . 3_645 ? Se12 Pb1 Se2 153.158(10) . 3_645 ? Se1 Pb1 Se2 72.178(12) . . ? Se11 Pb1 Se2 153.098(9) . . ? Se12 Pb1 Se2 121.550(13) . . ? Se2 Pb1 Se2 84.488(16) 3_645 . ? P1 Se1 Pb1 92.84(3) . . ? P1 Se2 Pb1 91.56(3) . 3_645 ? P1 Se2 Pb1 81.67(2) . . ? Pb1 Se2 Pb1 95.512(16) 3_645 . ? O1 P1 C1 100.37(14) . . ? O1 P1 Se2 110.76(9) . . ? C1 P1 Se2 109.51(11) . . ? O1 P1 Se1 110.90(9) . . ? C1 P1 Se1 111.38(10) . . ? Se2 P1 Se1 113.20(4) . . ? C6 C1 C2 119.7(3) . . ? C6 C1 P1 121.4(2) . . ? C2 C1 P1 118.5(2) . . ? C3 C2 C1 120.2(3) . . ? C2 C3 C4 119.6(3) . . ? C5 C4 C3 120.3(3) . . ? C6 C5 C4 120.4(3) . . ? C5 C6 C1 119.7(3) . . ? C7 O1 P1 118.7(2) . . ? P11 Se11 Pb1 86.70(2) . . ? P11 Se12 Pb1 82.45(2) . . ? O11 P11 C11 100.13(13) . . ? O11 P11 Se12 111.86(9) . . ? C11 P11 Se12 111.62(10) . . ? O11 P11 Se11 108.59(9) . . ? C11 P11 Se11 110.58(11) . . ? Se12 P11 Se11 113.28(4) . . ? C16 C11 C12 119.8(3) . . ? C16 C11 P11 121.3(2) . . ? C12 C11 P11 118.9(2) . . ? C13 C12 C11 119.5(3) . . ? C12 C13 C14 120.9(3) . . ? C15 C14 C13 119.4(3) . . ? C14 C15 C16 120.3(3) . . ? C11 C16 C15 120.0(3) . . ? C17 O11 P11 119.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se11 Pb1 Se1 P1 -165.93(2) . . . . ? Se12 Pb1 Se1 P1 119.70(3) . . . . ? Se2 Pb1 Se1 P1 -87.14(3) 3_645 . . . ? Se2 Pb1 Se1 P1 -2.01(2) . . . . ? Se1 Pb1 Se2 P1 2.03(2) . . . . ? Se11 Pb1 Se2 P1 39.67(3) . . . . ? Se12 Pb1 Se2 P1 -82.27(3) . . . . ? Se2 Pb1 Se2 P1 90.77(3) 3_645 . . . ? Se1 Pb1 Se2 Pb1 -88.736(16) . . . 3_645 ? Se11 Pb1 Se2 Pb1 -51.11(3) . . . 3_645 ? Se12 Pb1 Se2 Pb1 -173.040(10) . . . 3_645 ? Se2 Pb1 Se2 Pb1 0.0 3_645 . . 3_645 ? Pb1 Se2 P1 O1 -142.14(9) 3_645 . . . ? Pb1 Se2 P1 O1 122.52(9) . . . . ? Pb1 Se2 P1 C1 -32.35(11) 3_645 . . . ? Pb1 Se2 P1 C1 -127.69(11) . . . . ? Pb1 Se2 P1 Se1 92.59(4) 3_645 . . . ? Pb1 Se2 P1 Se1 -2.76(3) . . . . ? Pb1 Se1 P1 O1 -122.05(9) . . . . ? Pb1 Se1 P1 C1 127.07(12) . . . . ? Pb1 Se1 P1 Se2 3.15(4) . . . . ? O1 P1 C1 C6 -137.1(3) . . . . ? Se2 P1 C1 C6 106.3(3) . . . . ? Se1 P1 C1 C6 -19.7(3) . . . . ? O1 P1 C1 C2 49.1(3) . . . . ? Se2 P1 C1 C2 -67.5(3) . . . . ? Se1 P1 C1 C2 166.5(2) . . . . ? C6 C1 C2 C3 0.6(5) . . . . ? P1 C1 C2 C3 174.6(3) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C2 C3 C4 C5 0.7(6) . . . . ? C3 C4 C5 C6 0.0(6) . . . . ? C4 C5 C6 C1 -0.3(5) . . . . ? C2 C1 C6 C5 0.0(5) . . . . ? P1 C1 C6 C5 -173.8(3) . . . . ? C1 P1 O1 C7 178.7(2) . . . . ? Se2 P1 O1 C7 -65.7(2) . . . . ? Se1 P1 O1 C7 60.9(2) . . . . ? Se1 Pb1 Se11 P11 -106.20(3) . . . . ? Se12 Pb1 Se11 P11 -10.39(2) . . . . ? Se2 Pb1 Se11 P11 165.96(2) 3_645 . . . ? Se2 Pb1 Se11 P11 -141.84(3) . . . . ? Se1 Pb1 Se12 P11 95.28(3) . . . . ? Se11 Pb1 Se12 P11 10.59(2) . . . . ? Se2 Pb1 Se12 P11 2.63(3) 3_645 . . . ? Se2 Pb1 Se12 P11 167.14(2) . . . . ? Pb1 Se12 P11 O11 -137.92(9) . . . . ? Pb1 Se12 P11 C11 110.81(12) . . . . ? Pb1 Se12 P11 Se11 -14.79(3) . . . . ? Pb1 Se11 P11 O11 140.59(9) . . . . ? Pb1 Se11 P11 C11 -110.48(11) . . . . ? Pb1 Se11 P11 Se12 15.68(4) . . . . ? O11 P11 C11 C16 -117.3(3) . . . . ? Se12 P11 C11 C16 1.3(3) . . . . ? Se11 P11 C11 C16 128.3(3) . . . . ? O11 P11 C11 C12 64.1(3) . . . . ? Se12 P11 C11 C12 -177.3(2) . . . . ? Se11 P11 C11 C12 -50.3(3) . . . . ? C16 C11 C12 C13 -1.1(5) . . . . ? P11 C11 C12 C13 177.5(3) . . . . ? C11 C12 C13 C14 0.4(5) . . . . ? C12 C13 C14 C15 1.0(6) . . . . ? C13 C14 C15 C16 -1.6(5) . . . . ? C12 C11 C16 C15 0.4(5) . . . . ? P11 C11 C16 C15 -178.1(3) . . . . ? C14 C15 C16 C11 0.9(5) . . . . ? C11 P11 O11 C17 -174.3(2) . . . . ? Se12 P11 O11 C17 67.4(2) . . . . ? Se11 P11 O11 C17 -58.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.027 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.112 data_5m _database_code_depnum_ccdc_archive 'CCDC 266256' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H16 Ni O2 P2 Se4' _chemical_formula_weight 652.76 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' 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2868(17) _cell_length_b 8.1246(19) _cell_length_c 9.089(2) _cell_angle_alpha 70.312(4) _cell_angle_beta 71.498(4) _cell_angle_gamma 85.256(4) _cell_volume 480.24(19) _cell_formula_units_Z 1 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 75 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour red/green _exptl_crystal_size_max .15 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .02 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 2.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 310 _exptl_absorpt_coefficient_mu 8.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2508 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time ? _diffrn_standards_decay_% - _diffrn_reflns_number 2122 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 23.23 _reflns_number_total 1254 _reflns_number_gt 1194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1063P)^2^+0.2650P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.008(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1254 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 Ni1 Ni 0.0000 0.0000 0.5000 0.0162(4) Uani 1 2 d S . . Se1 Se -0.16273(7) 0.20256(7) 0.33492(7) 0.0211(3) Uani 1 1 d . . . Se2 Se 0.25664(7) 0.20504(7) 0.40600(6) 0.0196(3) Uani 1 1 d . . . P1 P 0.12416(19) 0.32081(18) 0.21320(17) 0.0174(4) Uani 1 1 d . . . C1 C 0.2504(8) 0.2669(8) 0.0294(6) 0.0183(12) Uani 1 1 d . . . C2 C 0.3641(8) 0.3902(8) -0.1107(7) 0.0244(13) Uani 1 1 d . . . H2A H 0.3772 0.5062 -0.1120 0.029 Uiso 1 1 calc R . . C3 C 0.4579(8) 0.3442(9) -0.2476(7) 0.0267(14) Uani 1 1 d . . . H3A H 0.5337 0.4292 -0.3446 0.032 Uiso 1 1 calc R . . C4 C 0.4423(9) 0.1745(9) -0.2447(8) 0.0312(15) Uani 1 1 d . . . H4A H 0.5099 0.1425 -0.3388 0.037 Uiso 1 1 calc R . . C5 C 0.3281(9) 0.0511(8) -0.1045(8) 0.0297(15) Uani 1 1 d . . . H5A H 0.3175 -0.0655 -0.1025 0.036 Uiso 1 1 calc R . . C6 C 0.2308(9) 0.0974(8) 0.0307(7) 0.0247(13) Uani 1 1 d . . . H6A H 0.1498 0.0138 0.1257 0.030 Uiso 1 1 calc R . . O1 O 0.1322(5) 0.5281(5) 0.1445(5) 0.0207(9) Uani 1 1 d . . . C7 C 0.0439(9) 0.6263(8) 0.2551(8) 0.0262(14) Uani 1 1 d . . . H7A H -0.0408 0.5480 0.3583 0.039 Uiso 1 1 calc R . . H7B H -0.0325 0.7201 0.2041 0.039 Uiso 1 1 calc R . . H7C H 0.1452 0.6771 0.2776 0.039 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 Ni1 0.0187(6) 0.0090(6) 0.0188(6) -0.0010(4) -0.0066(4) 0.0001(4) Se1 0.0178(4) 0.0150(5) 0.0264(5) -0.0009(3) -0.0076(3) -0.0003(3) Se2 0.0206(4) 0.0137(5) 0.0246(5) -0.0035(3) -0.0096(3) -0.0016(3) P1 0.0208(8) 0.0100(8) 0.0204(8) -0.0035(6) -0.0066(6) 0.0006(6) C1 0.021(3) 0.024(3) 0.013(3) -0.006(2) -0.010(2) 0.008(2) C2 0.025(3) 0.025(3) 0.024(3) -0.005(3) -0.012(2) 0.003(3) C3 0.020(3) 0.038(4) 0.020(3) -0.004(3) -0.010(2) 0.005(3) C4 0.025(3) 0.043(4) 0.036(4) -0.023(3) -0.014(3) 0.011(3) C5 0.034(3) 0.026(3) 0.039(4) -0.019(3) -0.017(3) 0.010(3) C6 0.031(3) 0.019(3) 0.025(3) -0.005(3) -0.013(3) 0.004(2) O1 0.025(2) 0.008(2) 0.026(2) -0.0026(16) -0.0069(16) -0.0030(16) C7 0.031(3) 0.013(3) 0.034(4) -0.012(3) -0.007(3) 0.004(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 Ni1 Se1 2.3469(6) . ? Ni1 Se1 2.3469(6) 2_556 ? Ni1 Se2 2.3547(7) 2_556 ? Ni1 Se2 2.3547(7) . ? Se1 P1 2.1599(14) . ? Se2 P1 2.1679(15) . ? P1 O1 1.586(4) . ? P1 C1 1.812(5) . ? C1 C2 1.386(8) . ? C1 C6 1.391(8) . ? C2 C3 1.374(8) . ? C2 H2A 0.9500 . ? C3 C4 1.383(9) . ? C3 H3A 0.9500 . ? C4 C5 1.388(9) . ? C4 H4A 0.9500 . ? C5 C6 1.367(9) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? O1 C7 1.451(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se1 Ni1 Se1 180.00(2) . 2_556 ? Se1 Ni1 Se2 90.13(2) . 2_556 ? Se1 Ni1 Se2 89.87(2) 2_556 2_556 ? Se1 Ni1 Se2 89.87(2) . . ? Se1 Ni1 Se2 90.13(2) 2_556 . ? Se2 Ni1 Se2 180.00(2) 2_556 . ? P1 Se1 Ni1 81.77(4) . . ? P1 Se2 Ni1 81.42(4) . . ? O1 P1 C1 101.7(2) . . ? O1 P1 Se1 115.29(16) . . ? C1 P1 Se1 113.17(19) . . ? O1 P1 Se2 115.10(16) . . ? C1 P1 Se2 111.88(18) . . ? Se1 P1 Se2 100.23(6) . . ? C2 C1 C6 120.0(5) . . ? C2 C1 P1 121.4(5) . . ? C6 C1 P1 118.5(4) . . ? C3 C2 C1 119.7(6) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 120.2(6) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C3 C4 C5 120.0(6) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 119.9(6) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C1 120.0(5) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? C7 O1 P1 119.7(3) . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se1 Ni1 Se1 P1 -25(100) 2_556 . . . ? Se2 Ni1 Se1 P1 -161.47(4) 2_556 . . . ? Se2 Ni1 Se1 P1 18.53(4) . . . . ? Se1 Ni1 Se2 P1 -18.48(4) . . . . ? Se1 Ni1 Se2 P1 161.52(4) 2_556 . . . ? Se2 Ni1 Se2 P1 113(100) 2_556 . . . ? Ni1 Se1 P1 O1 -144.73(18) . . . . ? Ni1 Se1 P1 C1 98.7(2) . . . . ? Ni1 Se1 P1 Se2 -20.53(5) . . . . ? Ni1 Se2 P1 O1 144.81(17) . . . . ? Ni1 Se2 P1 C1 -99.7(2) . . . . ? Ni1 Se2 P1 Se1 20.48(5) . . . . ? O1 P1 C1 C2 16.0(5) . . . . ? Se1 P1 C1 C2 140.3(4) . . . . ? Se2 P1 C1 C2 -107.3(4) . . . . ? O1 P1 C1 C6 -163.8(4) . . . . ? Se1 P1 C1 C6 -39.5(5) . . . . ? Se2 P1 C1 C6 72.9(5) . . . . ? C6 C1 C2 C3 -0.3(8) . . . . ? P1 C1 C2 C3 179.9(4) . . . . ? C1 C2 C3 C4 -1.4(8) . . . . ? C2 C3 C4 C5 1.5(8) . . . . ? C3 C4 C5 C6 0.1(9) . . . . ? C4 C5 C6 C1 -1.7(9) . . . . ? C2 C1 C6 C5 1.9(8) . . . . ? P1 C1 C6 C5 -178.3(4) . . . . ? C1 P1 O1 C7 179.6(4) . . . . ? Se1 P1 O1 C7 56.8(4) . . . . ? Se2 P1 O1 C7 -59.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 1.042 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.205 data_6m _database_code_depnum_ccdc_archive 'CCDC 266257' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 Cd2 O4 P4 Se8' _chemical_formula_weight 1412.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 24.5905(4) _cell_length_b 6.95110(10) _cell_length_c 48.2341(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8244.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 19529 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 27.71 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 2.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5280 _exptl_absorpt_coefficient_mu 8.282 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6969 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optic' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time ? _diffrn_standards_decay_% - _diffrn_reflns_number 13389 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.35 _reflns_number_total 13389 _reflns_number_gt 11740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+332.1748P] 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 riding _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 0.416(17) _refine_ls_number_reflns 13389 _refine_ls_number_parameters 518 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1810 _refine_ls_wR_factor_gt 0.1669 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.003 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 Cd1 Cd 0.57793(5) -0.0536(2) 1.02860(3) 0.0195(3) Uani 1 1 d . . . Cd2 Cd 0.68260(6) -0.0889(2) 0.95909(3) 0.0215(3) Uani 1 1 d . . . Se1 Se 0.52348(7) -0.3690(3) 1.04265(4) 0.0193(4) Uani 1 1 d . . . Se2 Se 0.53723(8) 0.0809(3) 1.07758(4) 0.0241(4) Uani 1 1 d . . . P1 P 0.49793(18) -0.2000(8) 1.07885(10) 0.0152(9) Uani 1 1 d . . . C1 C 0.4234(7) -0.184(3) 1.0803(4) 0.020(4) Uiso 1 1 d . . . C2 C 0.3931(9) -0.248(3) 1.1024(5) 0.021(5) Uiso 1 1 d . . . H2A H 0.4108 -0.3015 1.1182 0.025 Uiso 1 1 calc R . . C3 C 0.3387(11) -0.236(3) 1.1019(7) 0.036(6) Uiso 1 1 d . . . H3A H 0.3180 -0.2845 1.1169 0.043 Uiso 1 1 calc R . . C4 C 0.3128(8) -0.154(3) 1.0795(4) 0.024(4) Uiso 1 1 d . . . H4A H 0.2743 -0.1458 1.0792 0.028 Uiso 1 1 calc R . . C5 C 0.3424(10) -0.086(4) 1.0581(6) 0.041(6) Uiso 1 1 d . . . H5A H 0.3242 -0.0287 1.0428 0.049 Uiso 1 1 calc R . . C6 C 0.3983(7) -0.097(3) 1.0579(4) 0.017(4) Uiso 1 1 d . . . H6A H 0.4190 -0.0472 1.0429 0.020 Uiso 1 1 calc R . . O1 O 0.5108(5) -0.3093(19) 1.1071(3) 0.017(3) Uiso 1 1 d . . . C7 C 0.5648(9) -0.368(4) 1.1124(5) 0.034(5) Uiso 1 1 d . . . H7A H 0.5763 -0.4599 1.0981 0.051 Uiso 1 1 calc R . . H7B H 0.5667 -0.4294 1.1306 0.051 Uiso 1 1 calc R . . H7C H 0.5888 -0.2557 1.1120 0.051 Uiso 1 1 calc R . . Se11 Se 0.68267(8) 0.2706(3) 0.97659(5) 0.0191(5) Uani 1 1 d . . . Se12 Se 0.68445(7) -0.0921(3) 1.03100(4) 0.0177(4) Uani 1 1 d . . . P11 P 0.71503(18) 0.1826(7) 1.01657(10) 0.0161(10) Uani 1 1 d . . . C11 C 0.7873(7) 0.162(3) 1.0179(4) 0.018(4) Uiso 1 1 d . . . C12 C 0.8120(8) 0.088(3) 1.0403(4) 0.019(4) Uiso 1 1 d . . . H12A H 0.7908 0.0403 1.0552 0.023 Uiso 1 1 calc R . . C13 C 0.8690(7) 0.080(3) 1.0418(4) 0.018(4) Uiso 1 1 d . . . H13A H 0.8866 0.0243 1.0574 0.022 Uiso 1 1 calc R . . C14 C 0.8993(8) 0.157(3) 1.0198(4) 0.023(4) Uiso 1 1 d . . . H14A H 0.9379 0.1563 1.0207 0.027 Uiso 1 1 calc R . . C15 C 0.8727(9) 0.236(3) 0.9962(5) 0.025(5) Uiso 1 1 d . . . H15A H 0.8923 0.2803 0.9805 0.030 Uiso 1 1 calc R . . C16 C 0.8187(10) 0.243(3) 0.9973(6) 0.026(5) Uiso 1 1 d . . . H16A H 0.8003 0.3093 0.9829 0.032 Uiso 1 1 calc R . . O11 O 0.7066(6) 0.350(2) 1.0388(3) 0.023(3) Uiso 1 1 d . . . C17 C 0.6517(8) 0.423(3) 1.0443(4) 0.020(4) Uiso 1 1 d . . . H17A H 0.6370 0.4816 1.0274 0.031 Uiso 1 1 calc R . . H17B H 0.6532 0.5199 1.0590 0.031 Uiso 1 1 calc R . . H17C H 0.6282 0.3166 1.0501 0.031 Uiso 1 1 calc R . . Se21 Se 0.59176(9) -0.2810(3) 0.96781(5) 0.0190(4) Uani 1 1 d . . . Se22 Se 0.52682(8) 0.1596(3) 0.99173(4) 0.0209(4) Uani 1 1 d . . . P21 P 0.5364(2) -0.0432(7) 0.95864(11) 0.0206(10) Uani 1 1 d . . . C21 C 0.5570(8) 0.073(3) 0.9281(4) 0.019(4) Uiso 1 1 d . . . C22 C 0.5573(11) -0.029(4) 0.9021(6) 0.043(6) Uiso 1 1 d . . . H22A H 0.5464 -0.1605 0.9012 0.052 Uiso 1 1 calc R . . C23 C 0.5737(9) 0.066(3) 0.8783(5) 0.028(5) Uiso 1 1 d . . . H23A H 0.5725 -0.0009 0.8612 0.034 Uiso 1 1 calc R . . C24 C 0.5916(9) 0.252(3) 0.8781(5) 0.025(5) Uiso 1 1 d . . . H24A H 0.6031 0.3119 0.8614 0.031 Uiso 1 1 calc R . . C25 C 0.5926(9) 0.350(3) 0.9034(5) 0.030(5) Uiso 1 1 d . . . H25A H 0.6061 0.4783 0.9036 0.036 Uiso 1 1 calc R . . C26 C 0.5752(12) 0.273(4) 0.9277(6) 0.040(6) Uiso 1 1 d . . . H26A H 0.5748 0.3483 0.9442 0.048 Uiso 1 1 calc R . . O21 O 0.4804(6) -0.130(2) 0.9498(3) 0.027(3) Uiso 1 1 d . . . C27 C 0.4481(9) -0.266(3) 0.9686(5) 0.025(5) Uiso 1 1 d . . . H27A H 0.4714 -0.3732 0.9742 0.038 Uiso 1 1 calc R . . H27B H 0.4165 -0.3154 0.9584 0.038 Uiso 1 1 calc R . . H27C H 0.4358 -0.1957 0.9850 0.038 Uiso 1 1 calc R . . Se31 Se 0.77640(8) -0.2665(3) 0.96473(5) 0.0194(5) Uani 1 1 d . . . Se32 Se 0.71239(8) -0.0821(3) 0.90411(4) 0.0226(4) Uani 1 1 d . . . P31 P 0.7830(2) -0.2260(7) 0.92097(11) 0.0177(11) Uani 1 1 d . . . C31 C 0.8457(8) -0.100(3) 0.9131(4) 0.026(4) Uiso 1 1 d . . . C32 C 0.8894(9) -0.186(3) 0.8967(5) 0.030(5) Uiso 1 1 d . . . H32A H 0.8866 -0.3153 0.8905 0.036 Uiso 1 1 calc R . . C33 C 0.9351(10) -0.077(3) 0.8904(5) 0.035(5) Uiso 1 1 d . . . H33A H 0.9631 -0.1288 0.8790 0.043 Uiso 1 1 calc R . . C34 C 0.9392(10) 0.109(3) 0.9011(5) 0.034(5) Uiso 1 1 d . . . H34A H 0.9716 0.1802 0.8978 0.041 Uiso 1 1 calc R . . C35 C 0.8970(9) 0.197(4) 0.9167(5) 0.033(5) Uiso 1 1 d . . . H35A H 0.8989 0.3270 0.9226 0.039 Uiso 1 1 calc R . . C36 C 0.8540(9) 0.084(3) 0.9225(5) 0.029(5) Uiso 1 1 d . . . H36A H 0.8269 0.1367 0.9343 0.035 Uiso 1 1 calc R . . O31 O 0.7944(6) -0.420(2) 0.9048(3) 0.029(3) Uiso 1 1 d . . . C37 C 0.7532(9) -0.563(3) 0.9053(5) 0.034(5) Uiso 1 1 d . . . H37A H 0.7419 -0.5861 0.9245 0.051 Uiso 1 1 calc R . . H37B H 0.7675 -0.6825 0.8973 0.051 Uiso 1 1 calc R . . H37C H 0.7219 -0.5193 0.8944 0.051 Uiso 1 1 calc R . . Cd41 Cd 1.32988(5) 0.5462(2) 0.69191(3) 0.0197(3) Uani 1 1 d . . . Cd42 Cd 1.43656(6) 0.5664(2) 0.76004(3) 0.0212(3) Uani 1 1 d . . . Se41 Se 1.27595(8) 0.8642(3) 0.67750(4) 0.0201(4) Uani 1 1 d . . . Se42 Se 1.28853(8) 0.4140(3) 0.64244(4) 0.0244(4) Uani 1 1 d . . . P41 P 1.2517(2) 0.6959(8) 0.64234(11) 0.0197(10) Uani 1 1 d . . . C41 C 1.1789(7) 0.683(3) 0.6405(4) 0.014(3) Uiso 1 1 d . . . C42 C 1.1522(8) 0.748(2) 0.6181(4) 0.014(4) Uiso 1 1 d . . . H42A H 1.1719 0.7989 0.6028 0.017 Uiso 1 1 calc R . . C43 C 1.0929(8) 0.740(2) 0.6173(5) 0.012(4) Uiso 1 1 d . . . H43A H 1.0735 0.7873 0.6017 0.015 Uiso 1 1 calc R . . C44 C 1.0656(9) 0.664(3) 0.6397(5) 0.031(5) Uiso 1 1 d . . . H44A H 1.0270 0.6606 0.6394 0.038 Uiso 1 1 calc R . . C45 C 1.0942(8) 0.589(3) 0.6634(4) 0.026(4) Uiso 1 1 d . . . H45A H 1.0757 0.5338 0.6788 0.031 Uiso 1 1 calc R . . C46 C 1.1493(9) 0.603(3) 0.6625(5) 0.032(5) Uiso 1 1 d . . . H46A H 1.1692 0.5550 0.6779 0.038 Uiso 1 1 calc R . . O41 O 1.2636(6) 0.811(2) 0.6138(3) 0.023(3) Uiso 1 1 d . . . C47 C 1.3183(8) 0.875(3) 0.6070(4) 0.024(4) Uiso 1 1 d . . . H47A H 1.3296 0.9749 0.6200 0.035 Uiso 1 1 calc R . . H47B H 1.3187 0.9266 0.5881 0.035 Uiso 1 1 calc R . . H47C H 1.3434 0.7655 0.6082 0.035 Uiso 1 1 calc R . . Se51 Se 1.43637(7) 0.5818(3) 0.68880(4) 0.0174(4) Uani 1 1 d . . . Se52 Se 1.43520(8) 0.2082(3) 0.74155(5) 0.0202(4) Uani 1 1 d . . . P51 P 1.46713(19) 0.3027(8) 0.70284(10) 0.0156(9) Uani 1 1 d . . . C51 C 1.5413(7) 0.314(2) 0.7024(4) 0.013(3) Uiso 1 1 d . . . C52 C 1.5661(7) 0.407(2) 0.6793(4) 0.015(4) Uiso 1 1 d . . . H52A H 1.5450 0.4616 0.6648 0.018 Uiso 1 1 calc R . . C53 C 1.6223(10) 0.415(3) 0.6790(5) 0.034(5) Uiso 1 1 d . . . H53A H 1.6397 0.4718 0.6635 0.041 Uiso 1 1 calc R . . C54 C 1.6531(9) 0.347(3) 0.6996(4) 0.028(5) Uiso 1 1 d . . . H54A H 1.6914 0.3640 0.6992 0.034 Uiso 1 1 calc R . . C55 C 1.6291(9) 0.254(3) 0.7210(5) 0.021(5) Uiso 1 1 d . . . H55A H 1.6516 0.1945 0.7345 0.025 Uiso 1 1 calc R . . C56 C 1.5716(8) 0.243(2) 0.7242(5) 0.012(4) Uiso 1 1 d . . . H56A H 1.5552 0.1892 0.7402 0.014 Uiso 1 1 calc R . . O51 O 1.4581(6) 0.140(2) 0.6793(3) 0.025(3) Uiso 1 1 d . . . C57 C 1.4049(8) 0.064(3) 0.6742(4) 0.025(4) Uiso 1 1 d . . . H57A H 1.3874 0.0320 0.6918 0.037 Uiso 1 1 calc R . . H57B H 1.4079 -0.0527 0.6628 0.037 Uiso 1 1 calc R . . H57C H 1.3831 0.1598 0.6643 0.037 Uiso 1 1 calc R . . Se61 Se 1.34738(9) 0.7677(3) 0.75279(5) 0.0191(4) Uani 1 1 d . . . Se62 Se 1.27867(8) 0.3342(3) 0.72880(4) 0.0208(4) Uani 1 1 d . . . P61 P 1.2902(2) 0.5372(7) 0.76246(11) 0.0200(10) Uani 1 1 d . . . C61 C 1.3086(7) 0.411(2) 0.7945(4) 0.014(4) Uiso 1 1 d . . . C62 C 1.3062(9) 0.507(3) 0.8197(5) 0.030(5) Uiso 1 1 d . . . H62A H 1.2924 0.6348 0.8206 0.036 Uiso 1 1 calc R . . C63 C 1.3238(11) 0.416(4) 0.8429(6) 0.046(6) Uiso 1 1 d . . . H63A H 1.3219 0.4811 0.8602 0.055 Uiso 1 1 calc R . . C64 C 1.3464(10) 0.215(4) 0.8419(6) 0.035(6) Uiso 1 1 d . . . H64A H 1.3595 0.1527 0.8581 0.043 Uiso 1 1 calc R . . C65 C 1.3470(10) 0.128(4) 0.8170(5) 0.037(5) Uiso 1 1 d . . . H65A H 1.3604 -0.0001 0.8152 0.044 Uiso 1 1 calc R . . C66 C 1.3272(8) 0.230(2) 0.7927(4) 0.010(4) Uiso 1 1 d . . . H66A H 1.3274 0.1677 0.7752 0.012 Uiso 1 1 calc R . . O61 O 1.2343(6) 0.626(2) 0.7719(3) 0.026(3) Uiso 1 1 d . . . C67 C 1.2088(9) 0.757(3) 0.7546(5) 0.026(5) Uiso 1 1 d . . . H67A H 1.2251 0.8850 0.7572 0.039 Uiso 1 1 calc R . . H67B H 1.1700 0.7630 0.7591 0.039 Uiso 1 1 calc R . . H67C H 1.2134 0.7172 0.7352 0.039 Uiso 1 1 calc R . . Se71 Se 1.53452(9) 0.7342(3) 0.75398(5) 0.0206(5) Uani 1 1 d . . . Se72 Se 1.46592(8) 0.5531(3) 0.81438(4) 0.0248(4) Uani 1 1 d . . . P71 P 1.5375(2) 0.6954(8) 0.79878(12) 0.0205(11) Uani 1 1 d . . . C71 C 1.5989(6) 0.578(2) 0.8079(3) 0.010(3) Uiso 1 1 d . . . C72 C 1.6376(7) 0.654(3) 0.8255(4) 0.018(4) Uiso 1 1 d . . . H72A H 1.6313 0.7768 0.8334 0.021 Uiso 1 1 calc R . . C73 C 1.6859(10) 0.556(4) 0.8323(5) 0.040(6) Uiso 1 1 d . . . H73A H 1.7116 0.6165 0.8441 0.047 Uiso 1 1 calc R . . C74 C 1.6964(10) 0.376(3) 0.8221(5) 0.035(5) Uiso 1 1 d . . . H74A H 1.7294 0.3120 0.8264 0.042 Uiso 1 1 calc R . . C75 C 1.6576(9) 0.290(3) 0.8052(5) 0.030(5) Uiso 1 1 d . . . H75A H 1.6632 0.1629 0.7985 0.036 Uiso 1 1 calc R . . C76 C 1.6075(9) 0.397(3) 0.7978(4) 0.026(4) Uiso 1 1 d . . . H76A H 1.5813 0.3397 0.7860 0.032 Uiso 1 1 calc R . . O71 O 1.5470(6) 0.897(2) 0.8146(3) 0.029(3) Uiso 1 1 d . . . C77 C 1.5048(9) 1.046(3) 0.8146(5) 0.036(5) Uiso 1 1 d . . . H77A H 1.5046 1.1122 0.7967 0.053 Uiso 1 1 calc R . . H77B H 1.5124 1.1390 0.8294 0.053 Uiso 1 1 calc R . . H77C H 1.4692 0.9867 0.8178 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0185(6) 0.0232(7) 0.0167(7) 0.0028(6) 0.0018(5) -0.0026(5) Cd2 0.0198(7) 0.0207(7) 0.0239(7) -0.0044(6) 0.0028(6) 0.0001(5) Se1 0.0200(9) 0.0171(9) 0.0207(10) -0.0019(8) 0.0035(7) -0.0009(7) Se2 0.0250(10) 0.0235(11) 0.0239(10) -0.0070(8) 0.0085(8) -0.0049(8) P1 0.012(2) 0.017(2) 0.016(2) -0.002(2) -0.0025(18) 0.0019(18) Se11 0.0224(10) 0.0175(10) 0.0174(11) 0.0018(8) -0.0005(8) 0.0025(7) Se12 0.0182(9) 0.0152(10) 0.0197(9) 0.0014(7) 0.0000(7) -0.0030(7) P11 0.013(2) 0.017(3) 0.019(2) 0.007(2) 0.0017(18) -0.0010(18) Se21 0.0214(10) 0.0167(9) 0.0188(11) -0.0001(8) 0.0020(8) -0.0026(7) Se22 0.0230(9) 0.0219(11) 0.0177(10) -0.0034(8) 0.0029(7) 0.0049(7) P21 0.027(3) 0.019(2) 0.016(2) -0.005(2) -0.003(2) -0.0032(19) Se31 0.0172(10) 0.0236(11) 0.0174(12) 0.0039(7) 0.0035(8) 0.0006(7) Se32 0.0240(10) 0.0253(11) 0.0186(9) 0.0006(8) -0.0005(8) 0.0016(8) P31 0.023(3) 0.019(3) 0.012(2) 0.0029(19) 0.0048(19) 0.0029(19) Cd41 0.0180(6) 0.0226(7) 0.0184(7) 0.0027(6) -0.0014(5) 0.0018(5) Cd42 0.0207(7) 0.0213(7) 0.0215(7) -0.0028(6) -0.0013(5) -0.0015(5) Se41 0.0210(9) 0.0175(9) 0.0219(10) -0.0008(8) -0.0039(7) 0.0016(7) Se42 0.0260(10) 0.0219(11) 0.0254(10) -0.0077(8) -0.0070(8) 0.0095(8) P41 0.025(3) 0.018(2) 0.016(2) 0.005(2) -0.005(2) 0.004(2) Se51 0.0184(9) 0.0178(10) 0.0159(9) 0.0018(7) 0.0009(7) 0.0012(7) Se52 0.0209(10) 0.0193(9) 0.0203(11) 0.0042(9) 0.0040(8) 0.0030(8) P51 0.017(2) 0.015(2) 0.015(2) -0.001(2) 0.0005(18) 0.0003(18) Se61 0.0192(9) 0.0180(10) 0.0201(11) -0.0008(7) 0.0021(8) -0.0023(7) Se62 0.0226(9) 0.0214(11) 0.0185(10) 0.0000(8) -0.0012(7) -0.0056(7) P61 0.019(2) 0.020(3) 0.021(3) -0.001(2) 0.0067(19) 0.0000(19) Se71 0.0216(10) 0.0232(11) 0.0171(11) 0.0048(7) 0.0026(8) -0.0014(7) Se72 0.0266(10) 0.0301(11) 0.0176(10) 0.0023(8) 0.0010(7) -0.0026(8) P71 0.026(3) 0.014(2) 0.022(3) -0.001(2) 0.000(2) 0.003(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 Cd1 Se22 2.634(2) . ? Cd1 Se12 2.636(2) . ? Cd1 Se1 2.657(2) . ? Cd1 Se2 2.731(2) . ? Cd2 Se31 2.630(2) . ? Cd2 Se21 2.636(3) . ? Cd2 Se11 2.638(3) . ? Cd2 Se32 2.751(2) . ? Se1 P1 2.196(5) . ? Se2 P1 2.180(6) . ? P1 O1 1.590(14) . ? P1 C1 1.838(19) . ? C1 C6 1.38(3) . ? C1 C2 1.38(3) . ? C2 C3 1.34(3) . ? C2 H2A 0.9500 . ? C3 C4 1.37(4) . ? C3 H3A 0.9500 . ? C4 C5 1.35(3) . ? C4 H4A 0.9500 . ? C5 C6 1.38(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? O1 C7 1.41(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? Se11 P11 2.174(5) . ? Se12 P11 2.167(5) . ? P11 O11 1.597(15) . ? P11 C11 1.784(19) . ? C11 C12 1.34(3) . ? C11 C16 1.38(3) . ? C12 C13 1.40(3) . ? C12 H12A 0.9500 . ? C13 C14 1.40(3) . ? C13 H13A 0.9500 . ? C14 C15 1.43(3) . ? C14 H14A 0.9500 . ? C15 C16 1.33(3) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? O11 C17 1.47(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? Se21 P21 2.187(6) . ? Se22 P21 2.143(5) . ? P21 O21 1.561(15) . ? P21 C21 1.76(2) . ? C21 C22 1.44(3) . ? C21 C26 1.46(3) . ? C22 C23 1.39(3) . ? C22 H22A 0.9500 . ? C23 C24 1.36(3) . ? C23 H23A 0.9500 . ? C24 C25 1.40(3) . ? C24 H24A 0.9500 . ? C25 C26 1.36(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? O21 C27 1.53(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? Se31 P31 2.136(6) . ? Se32 P31 2.162(6) . ? P31 O31 1.582(16) . ? P31 C31 1.81(2) . ? C31 C36 1.37(3) . ? C31 C32 1.46(3) . ? C32 C33 1.39(3) . ? C32 H32A 0.9500 . ? C33 C34 1.40(3) . ? C33 H33A 0.9500 . ? C34 C35 1.42(3) . ? C34 H34A 0.9500 . ? C35 C36 1.34(3) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? O31 C37 1.42(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? Cd41 Se62 2.631(2) . ? Cd41 Se51 2.635(2) . ? Cd41 Se41 2.669(2) . ? Cd41 Se42 2.752(2) . ? Cd42 Se61 2.625(3) . ? Cd42 Se52 2.646(3) . ? Cd42 Se71 2.692(3) . ? Cd42 Se72 2.720(2) . ? Se41 P41 2.144(6) . ? Se42 P41 2.159(6) . ? P41 O41 1.616(15) . ? P41 C41 1.796(18) . ? C41 C42 1.34(3) . ? C41 C46 1.40(3) . ? C42 C43 1.46(3) . ? C42 H42A 0.9500 . ? C43 C44 1.38(3) . ? C43 H43A 0.9500 . ? C44 C45 1.44(3) . ? C44 H44A 0.9500 . ? C45 C46 1.36(3) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? O41 C47 1.45(2) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? Se51 P51 2.190(6) . ? Se52 P51 2.129(6) . ? P51 O51 1.620(15) . ? P51 C51 1.825(17) . ? C51 C56 1.38(3) . ? C51 C52 1.43(2) . ? C52 C53 1.38(3) . ? C52 H52A 0.9500 . ? C53 C54 1.33(3) . ? C53 H53A 0.9500 . ? C54 C55 1.35(3) . ? C54 H54A 0.9500 . ? C55 C56 1.42(3) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? O51 C57 1.43(2) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? Se61 P61 2.182(5) . ? Se62 P61 2.170(6) . ? P61 O61 1.575(15) . ? P61 C61 1.836(19) . ? C61 C66 1.34(2) . ? C61 C62 1.39(3) . ? C62 C63 1.36(4) . ? C62 H62A 0.9500 . ? C63 C64 1.50(4) . ? C63 H63A 0.9500 . ? C64 C65 1.35(4) . ? C64 H64A 0.9500 . ? C65 C66 1.46(3) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? O61 C67 1.39(3) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? Se71 P71 2.179(6) . ? Se72 P71 2.155(6) . ? P71 O71 1.609(16) . ? P71 C71 1.772(17) . ? C71 C76 1.36(3) . ? C71 C72 1.38(3) . ? C72 C73 1.40(3) . ? C72 H72A 0.9500 . ? C73 C74 1.37(3) . ? C73 H73A 0.9500 . ? C74 C75 1.39(3) . ? C74 H74A 0.9500 . ? C75 C76 1.48(3) . ? C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? O71 C77 1.47(3) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se22 Cd1 Se12 124.13(8) . . ? Se22 Cd1 Se1 113.33(8) . . ? Se12 Cd1 Se1 113.94(8) . . ? Se22 Cd1 Se2 102.51(8) . . ? Se12 Cd1 Se2 111.16(8) . . ? Se1 Cd1 Se2 82.94(7) . . ? Se31 Cd2 Se21 119.26(8) . . ? Se31 Cd2 Se11 114.26(8) . . ? Se21 Cd2 Se11 115.44(8) . . ? Se31 Cd2 Se32 82.78(8) . . ? Se21 Cd2 Se32 112.83(8) . . ? Se11 Cd2 Se32 106.99(9) . . ? P1 Se1 Cd1 84.59(15) . . ? P1 Se2 Cd1 83.13(15) . . ? O1 P1 C1 101.3(8) . . ? O1 P1 Se2 111.3(5) . . ? C1 P1 Se2 112.9(7) . . ? O1 P1 Se1 111.6(5) . . ? C1 P1 Se1 110.3(7) . . ? Se2 P1 Se1 109.3(2) . . ? C6 C1 C2 120.4(18) . . ? C6 C1 P1 116.3(14) . . ? C2 C1 P1 123.3(16) . . ? C3 C2 C1 120(2) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 120(3) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 120(2) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 121(2) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C5 C6 C1 117.8(19) . . ? C5 C6 H6A 121.1 . . ? C1 C6 H6A 121.1 . . ? C7 O1 P1 118.7(13) . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P11 Se11 Cd2 91.01(16) . . ? P11 Se12 Cd1 103.96(14) . . ? O11 P11 C11 99.5(8) . . ? O11 P11 Se12 112.4(6) . . ? C11 P11 Se12 105.2(7) . . ? O11 P11 Se11 110.0(6) . . ? C11 P11 Se11 114.8(6) . . ? Se12 P11 Se11 114.0(2) . . ? C12 C11 C16 118.9(19) . . ? C12 C11 P11 120.8(15) . . ? C16 C11 P11 119.9(16) . . ? C11 C12 C13 120.6(18) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 118.5(18) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C13 C14 C15 120.5(19) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C16 C15 C14 116(2) . . ? C16 C15 H15A 121.9 . . ? C14 C15 H15A 121.9 . . ? C15 C16 C11 125(2) . . ? C15 C16 H16A 117.5 . . ? C11 C16 H16A 117.5 . . ? C17 O11 P11 119.6(12) . . ? O11 C17 H17A 109.5 . . ? O11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P21 Se21 Cd2 96.45(16) . . ? P21 Se22 Cd1 94.62(16) . . ? O21 P21 C21 101.7(9) . . ? O21 P21 Se22 111.1(6) . . ? C21 P21 Se22 110.7(7) . . ? O21 P21 Se21 108.2(6) . . ? C21 P21 Se21 109.8(7) . . ? Se22 P21 Se21 114.5(2) . . ? C22 C21 C26 117(2) . . ? C22 C21 P21 120.2(16) . . ? C26 C21 P21 122.6(17) . . ? C23 C22 C21 119(2) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C24 C23 C22 124(2) . . ? C24 C23 H23A 118.2 . . ? C22 C23 H23A 118.2 . . ? C23 C24 C25 118(2) . . ? C23 C24 H24A 121.2 . . ? C25 C24 H24A 121.2 . . ? C26 C25 C24 124(2) . . ? C26 C25 H25A 118.2 . . ? C24 C25 H25A 118.2 . . ? C25 C26 C21 119(2) . . ? C25 C26 H26A 120.6 . . ? C21 C26 H26A 120.6 . . ? C27 O21 P21 122.2(13) . . ? O21 C27 H27A 109.5 . . ? O21 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O21 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? P31 Se31 Cd2 84.39(16) . . ? P31 Se32 Cd2 80.99(16) . . ? O31 P31 C31 99.0(9) . . ? O31 P31 Se31 112.9(6) . . ? C31 P31 Se31 109.6(7) . . ? O31 P31 Se32 110.5(6) . . ? C31 P31 Se32 112.4(7) . . ? Se31 P31 Se32 111.8(2) . . ? C36 C31 C32 116.7(19) . . ? C36 C31 P31 120.5(16) . . ? C32 C31 P31 122.8(16) . . ? C33 C32 C31 120(2) . . ? C33 C32 H32A 120.2 . . ? C31 C32 H32A 120.2 . . ? C32 C33 C34 119(2) . . ? C32 C33 H33A 120.6 . . ? C34 C33 H33A 120.6 . . ? C33 C34 C35 123(2) . . ? C33 C34 H34A 118.7 . . ? C35 C34 H34A 118.7 . . ? C36 C35 C34 116(2) . . ? C36 C35 H35A 122.1 . . ? C34 C35 H35A 122.1 . . ? C35 C36 C31 126(2) . . ? C35 C36 H36A 116.9 . . ? C31 C36 H36A 116.9 . . ? C37 O31 P31 117.6(14) . . ? O31 C37 H37A 109.5 . . ? O31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Se62 Cd41 Se51 124.52(8) . . ? Se62 Cd41 Se41 113.71(8) . . ? Se51 Cd41 Se41 113.66(8) . . ? Se62 Cd41 Se42 102.85(8) . . ? Se51 Cd41 Se42 110.44(8) . . ? Se41 Cd41 Se42 82.36(7) . . ? Se61 Cd42 Se52 116.50(8) . . ? Se61 Cd42 Se71 120.14(8) . . ? Se52 Cd42 Se71 112.49(8) . . ? Se61 Cd42 Se72 111.62(9) . . ? Se52 Cd42 Se72 107.22(9) . . ? Se71 Cd42 Se72 83.23(8) . . ? P41 Se41 Cd41 83.84(15) . . ? P41 Se42 Cd41 81.59(15) . . ? O41 P41 C41 99.4(8) . . ? O41 P41 Se41 110.7(6) . . ? C41 P41 Se41 110.1(6) . . ? O41 P41 Se42 112.0(6) . . ? C41 P41 Se42 111.9(6) . . ? Se41 P41 Se42 112.1(2) . . ? C42 C41 C46 119.4(18) . . ? C42 C41 P41 120.6(14) . . ? C46 C41 P41 120.0(15) . . ? C41 C42 C43 119.7(18) . . ? C41 C42 H42A 120.2 . . ? C43 C42 H42A 120.2 . . ? C44 C43 C42 118.8(19) . . ? C44 C43 H43A 120.6 . . ? C42 C43 H43A 120.6 . . ? C43 C44 C45 122(2) . . ? C43 C44 H44A 119.2 . . ? C45 C44 H44A 119.2 . . ? C46 C45 C44 116(2) . . ? C46 C45 H45A 122.1 . . ? C44 C45 H45A 122.1 . . ? C45 C46 C41 125(2) . . ? C45 C46 H46A 117.6 . . ? C41 C46 H46A 117.6 . . ? C47 O41 P41 120.8(13) . . ? O41 C47 H47A 109.5 . . ? O41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? P51 Se51 Cd41 104.04(15) . . ? P51 Se52 Cd42 90.03(16) . . ? O51 P51 C51 99.2(8) . . ? O51 P51 Se52 110.4(6) . . ? C51 P51 Se52 113.0(6) . . ? O51 P51 Se51 110.8(6) . . ? C51 P51 Se51 107.7(6) . . ? Se52 P51 Se51 114.7(2) . . ? C56 C51 C52 121.7(16) . . ? C56 C51 P51 121.1(14) . . ? C52 C51 P51 117.1(13) . . ? C53 C52 C51 116.9(17) . . ? C53 C52 H52A 121.5 . . ? C51 C52 H52A 121.5 . . ? C54 C53 C52 123(2) . . ? C54 C53 H53A 118.4 . . ? C52 C53 H53A 118.4 . . ? C53 C54 C55 119(2) . . ? C53 C54 H54A 120.4 . . ? C55 C54 H54A 120.4 . . ? C54 C55 C56 123(2) . . ? C54 C55 H55A 118.6 . . ? C56 C55 H55A 118.6 . . ? C51 C56 C55 115.8(19) . . ? C51 C56 H56A 122.1 . . ? C55 C56 H56A 122.1 . . ? C57 O51 P51 120.3(13) . . ? O51 C57 H57A 109.5 . . ? O51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? P61 Se61 Cd42 96.77(15) . . ? P61 Se62 Cd41 94.53(15) . . ? O61 P61 C61 99.2(8) . . ? O61 P61 Se62 110.9(6) . . ? C61 P61 Se62 110.5(6) . . ? O61 P61 Se61 109.6(6) . . ? C61 P61 Se61 111.9(6) . . ? Se62 P61 Se61 113.7(2) . . ? C66 C61 C62 121.8(18) . . ? C66 C61 P61 118.5(14) . . ? C62 C61 P61 119.6(15) . . ? C63 C62 C61 119(2) . . ? C63 C62 H62A 120.6 . . ? C61 C62 H62A 120.6 . . ? C62 C63 C64 122(3) . . ? C62 C63 H63A 119.2 . . ? C64 C63 H63A 119.2 . . ? C65 C64 C63 117(3) . . ? C65 C64 H64A 121.5 . . ? C63 C64 H64A 121.5 . . ? C64 C65 C66 120(2) . . ? C64 C65 H65A 120.2 . . ? C66 C65 H65A 120.2 . . ? C61 C66 C65 121.3(19) . . ? C61 C66 H66A 119.3 . . ? C65 C66 H66A 119.3 . . ? C67 O61 P61 118.6(14) . . ? O61 C67 H67A 109.5 . . ? O61 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? O61 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? P71 Se71 Cd42 82.46(16) . . ? P71 Se72 Cd42 82.22(16) . . ? O71 P71 C71 99.2(8) . . ? O71 P71 Se72 110.6(6) . . ? C71 P71 Se72 113.4(6) . . ? O71 P71 Se71 111.5(6) . . ? C71 P71 Se71 109.4(6) . . ? Se72 P71 Se71 112.1(3) . . ? C76 C71 C72 117.6(17) . . ? C76 C71 P71 117.9(14) . . ? C72 C71 P71 124.4(14) . . ? C71 C72 C73 122.9(19) . . ? C71 C72 H72A 118.6 . . ? C73 C72 H72A 118.6 . . ? C74 C73 C72 121(2) . . ? C74 C73 H73A 119.5 . . ? C72 C73 H73A 119.5 . . ? C73 C74 C75 118(2) . . ? C73 C74 H74A 120.8 . . ? C75 C74 H74A 120.8 . . ? C74 C75 C76 119(2) . . ? C74 C75 H75A 120.3 . . ? C76 C75 H75A 120.2 . . ? C71 C76 C75 120.4(19) . . ? C71 C76 H76A 119.8 . . ? C75 C76 H76A 119.8 . . ? C77 O71 P71 120.9(14) . . ? O71 C77 H77A 109.5 . . ? O71 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? O71 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se22 Cd1 Se1 P1 -98.60(15) . . . . ? Se12 Cd1 Se1 P1 112.08(14) . . . . ? Se2 Cd1 Se1 P1 2.02(14) . . . . ? Se22 Cd1 Se2 P1 110.37(15) . . . . ? Se12 Cd1 Se2 P1 -115.02(15) . . . . ? Se1 Cd1 Se2 P1 -2.04(14) . . . . ? Cd1 Se2 P1 O1 126.3(6) . . . . ? Cd1 Se2 P1 C1 -120.6(7) . . . . ? Cd1 Se2 P1 Se1 2.59(18) . . . . ? Cd1 Se1 P1 O1 -126.2(6) . . . . ? Cd1 Se1 P1 C1 122.0(7) . . . . ? Cd1 Se1 P1 Se2 -2.66(18) . . . . ? O1 P1 C1 C6 -178.9(15) . . . . ? Se2 P1 C1 C6 62.0(17) . . . . ? Se1 P1 C1 C6 -60.6(17) . . . . ? O1 P1 C1 C2 3.1(19) . . . . ? Se2 P1 C1 C2 -116.1(17) . . . . ? Se1 P1 C1 C2 121.3(16) . . . . ? C6 C1 C2 C3 3(3) . . . . ? P1 C1 C2 C3 -178.5(18) . . . . ? C1 C2 C3 C4 -2(3) . . . . ? C2 C3 C4 C5 0(4) . . . . ? C3 C4 C5 C6 0(4) . . . . ? C4 C5 C6 C1 1(3) . . . . ? C2 C1 C6 C5 -3(3) . . . . ? P1 C1 C6 C5 178.9(16) . . . . ? C1 P1 O1 C7 173.3(16) . . . . ? Se2 P1 O1 C7 -66.4(16) . . . . ? Se1 P1 O1 C7 56.0(16) . . . . ? Se31 Cd2 Se11 P11 -52.72(16) . . . . ? Se21 Cd2 Se11 P11 91.17(15) . . . . ? Se32 Cd2 Se11 P11 -142.35(14) . . . . ? Se22 Cd1 Se12 P11 31.85(19) . . . . ? Se1 Cd1 Se12 P11 177.37(16) . . . . ? Se2 Cd1 Se12 P11 -91.05(17) . . . . ? Cd1 Se12 P11 O11 72.7(6) . . . . ? Cd1 Se12 P11 C11 -179.9(6) . . . . ? Cd1 Se12 P11 Se11 -53.4(2) . . . . ? Cd2 Se11 P11 O11 -163.3(6) . . . . ? Cd2 Se11 P11 C11 85.4(7) . . . . ? Cd2 Se11 P11 Se12 -36.0(2) . . . . ? O11 P11 C11 C12 70.2(17) . . . . ? Se12 P11 C11 C12 -46.3(17) . . . . ? Se11 P11 C11 C12 -172.4(14) . . . . ? O11 P11 C11 C16 -101.8(17) . . . . ? Se12 P11 C11 C16 141.7(16) . . . . ? Se11 P11 C11 C16 15.6(19) . . . . ? C16 C11 C12 C13 -5(3) . . . . ? P11 C11 C12 C13 -176.9(15) . . . . ? C11 C12 C13 C14 2(3) . . . . ? C12 C13 C14 C15 -2(3) . . . . ? C13 C14 C15 C16 4(3) . . . . ? C14 C15 C16 C11 -8(3) . . . . ? C12 C11 C16 C15 8(3) . . . . ? P11 C11 C16 C15 -179.8(18) . . . . ? C11 P11 O11 C17 178.0(14) . . . . ? Se12 P11 O11 C17 -71.0(14) . . . . ? Se11 P11 O11 C17 57.1(14) . . . . ? Se31 Cd2 Se21 P21 -179.20(16) . . . . ? Se11 Cd2 Se21 P21 38.81(18) . . . . ? Se32 Cd2 Se21 P21 -84.64(16) . . . . ? Se12 Cd1 Se22 P21 76.81(17) . . . . ? Se1 Cd1 Se22 P21 -68.90(16) . . . . ? Se2 Cd1 Se22 P21 -156.53(15) . . . . ? Cd1 Se22 P21 O21 112.7(6) . . . . ? Cd1 Se22 P21 C21 -135.0(7) . . . . ? Cd1 Se22 P21 Se21 -10.3(2) . . . . ? Cd2 Se21 P21 O21 156.2(6) . . . . ? Cd2 Se21 P21 C21 46.0(7) . . . . ? Cd2 Se21 P21 Se22 -79.3(2) . . . . ? O21 P21 C21 C22 -51.6(19) . . . . ? Se22 P21 C21 C22 -169.8(16) . . . . ? Se21 P21 C21 C22 62.8(18) . . . . ? O21 P21 C21 C26 129.4(19) . . . . ? Se22 P21 C21 C26 11(2) . . . . ? Se21 P21 C21 C26 -116.2(18) . . . . ? C26 C21 C22 C23 -1(3) . . . . ? P21 C21 C22 C23 180.0(17) . . . . ? C21 C22 C23 C24 2(4) . . . . ? C22 C23 C24 C25 -1(3) . . . . ? C23 C24 C25 C26 -2(4) . . . . ? C24 C25 C26 C21 3(4) . . . . ? C22 C21 C26 C25 -2(3) . . . . ? P21 C21 C26 C25 177.3(19) . . . . ? C21 P21 O21 C27 173.2(14) . . . . ? Se22 P21 O21 C27 -69.0(15) . . . . ? Se21 P21 O21 C27 57.6(15) . . . . ? Se21 Cd2 Se31 P31 112.78(18) . . . . ? Se11 Cd2 Se31 P31 -104.80(18) . . . . ? Se32 Cd2 Se31 P31 0.62(16) . . . . ? Se31 Cd2 Se32 P31 -0.62(16) . . . . ? Se21 Cd2 Se32 P31 -119.38(17) . . . . ? Se11 Cd2 Se32 P31 112.60(17) . . . . ? Cd2 Se31 P31 O31 -126.2(6) . . . . ? Cd2 Se31 P31 C31 124.4(7) . . . . ? Cd2 Se31 P31 Se32 -0.8(2) . . . . ? Cd2 Se32 P31 O31 127.5(6) . . . . ? Cd2 Se32 P31 C31 -122.9(8) . . . . ? Cd2 Se32 P31 Se31 0.8(2) . . . . ? O31 P31 C31 C36 178.3(18) . . . . ? Se31 P31 C31 C36 -63.4(19) . . . . ? Se32 P31 C31 C36 61.6(19) . . . . ? O31 P31 C31 C32 -1.8(19) . . . . ? Se31 P31 C31 C32 116.5(17) . . . . ? Se32 P31 C31 C32 -118.5(17) . . . . ? C36 C31 C32 C33 -3(3) . . . . ? P31 C31 C32 C33 176.8(17) . . . . ? C31 C32 C33 C34 3(3) . . . . ? C32 C33 C34 C35 -4(4) . . . . ? C33 C34 C35 C36 5(3) . . . . ? C34 C35 C36 C31 -5(4) . . . . ? C32 C31 C36 C35 5(3) . . . . ? P31 C31 C36 C35 -175.5(19) . . . . ? C31 P31 O31 C37 -179.0(16) . . . . ? Se31 P31 O31 C37 65.2(16) . . . . ? Se32 P31 O31 C37 -60.9(16) . . . . ? Se62 Cd41 Se41 P41 -98.82(17) . . . . ? Se51 Cd41 Se41 P41 110.93(16) . . . . ? Se42 Cd41 Se41 P41 1.91(16) . . . . ? Se62 Cd41 Se42 P41 110.77(16) . . . . ? Se51 Cd41 Se42 P41 -114.37(16) . . . . ? Se41 Cd41 Se42 P41 -1.90(16) . . . . ? Cd41 Se41 P41 O41 -128.5(6) . . . . ? Cd41 Se41 P41 C41 122.6(7) . . . . ? Cd41 Se41 P41 Se42 -2.6(2) . . . . ? Cd41 Se42 P41 O41 127.7(6) . . . . ? Cd41 Se42 P41 C41 -121.7(7) . . . . ? Cd41 Se42 P41 Se41 2.5(2) . . . . ? O41 P41 C41 C42 4.6(17) . . . . ? Se41 P41 C41 C42 120.8(15) . . . . ? Se42 P41 C41 C42 -113.8(15) . . . . ? O41 P41 C41 C46 -175.9(17) . . . . ? Se41 P41 C41 C46 -59.7(17) . . . . ? Se42 P41 C41 C46 65.7(17) . . . . ? C46 C41 C42 C43 2(3) . . . . ? P41 C41 C42 C43 -178.5(13) . . . . ? C41 C42 C43 C44 -1(3) . . . . ? C42 C43 C44 C45 -1(3) . . . . ? C43 C44 C45 C46 1(3) . . . . ? C44 C45 C46 C41 0(3) . . . . ? C42 C41 C46 C45 -2(3) . . . . ? P41 C41 C46 C45 178.9(17) . . . . ? C41 P41 O41 C47 174.0(15) . . . . ? Se41 P41 O41 C47 58.2(15) . . . . ? Se42 P41 O41 C47 -67.7(15) . . . . ? Se62 Cd41 Se51 P51 32.02(18) . . . . ? Se41 Cd41 Se51 P51 178.55(16) . . . . ? Se42 Cd41 Se51 P51 -90.96(16) . . . . ? Se61 Cd42 Se52 P51 91.70(16) . . . . ? Se71 Cd42 Se52 P51 -52.76(16) . . . . ? Se72 Cd42 Se52 P51 -142.46(15) . . . . ? Cd42 Se52 P51 O51 -163.0(6) . . . . ? Cd42 Se52 P51 C51 86.9(6) . . . . ? Cd42 Se52 P51 Se51 -37.0(2) . . . . ? Cd41 Se51 P51 O51 74.1(6) . . . . ? Cd41 Se51 P51 C51 -178.4(6) . . . . ? Cd41 Se51 P51 Se52 -51.7(2) . . . . ? O51 P51 C51 C56 -108.8(15) . . . . ? Se52 P51 C51 C56 8.1(17) . . . . ? Se51 P51 C51 C56 135.7(14) . . . . ? O51 P51 C51 C52 73.9(15) . . . . ? Se52 P51 C51 C52 -169.2(12) . . . . ? Se51 P51 C51 C52 -41.6(14) . . . . ? C56 C51 C52 C53 3(3) . . . . ? P51 C51 C52 C53 -179.8(15) . . . . ? C51 C52 C53 C54 -3(3) . . . . ? C52 C53 C54 C55 5(3) . . . . ? C53 C54 C55 C56 -7(3) . . . . ? C52 C51 C56 C55 -5(3) . . . . ? P51 C51 C56 C55 178.0(13) . . . . ? C54 C55 C56 C51 7(3) . . . . ? C51 P51 O51 C57 173.0(14) . . . . ? Se52 P51 O51 C57 54.1(15) . . . . ? Se51 P51 O51 C57 -74.0(15) . . . . ? Se52 Cd42 Se61 P61 40.05(19) . . . . ? Se71 Cd42 Se61 P61 -178.34(16) . . . . ? Se72 Cd42 Se61 P61 -83.55(17) . . . . ? Se51 Cd41 Se62 P61 76.38(17) . . . . ? Se41 Cd41 Se62 P61 -70.15(16) . . . . ? Se42 Cd41 Se62 P61 -157.35(15) . . . . ? Cd41 Se62 P61 O61 113.1(6) . . . . ? Cd41 Se62 P61 C61 -137.9(6) . . . . ? Cd41 Se62 P61 Se61 -11.0(2) . . . . ? Cd42 Se61 P61 O61 156.9(6) . . . . ? Cd42 Se61 P61 C61 47.9(6) . . . . ? Cd42 Se61 P61 Se62 -78.3(2) . . . . ? O61 P61 C61 C66 134.6(15) . . . . ? Se62 P61 C61 C66 18.0(16) . . . . ? Se61 P61 C61 C66 -109.8(14) . . . . ? O61 P61 C61 C62 -49.4(17) . . . . ? Se62 P61 C61 C62 -165.9(14) . . . . ? Se61 P61 C61 C62 66.2(17) . . . . ? C66 C61 C62 C63 1(3) . . . . ? P61 C61 C62 C63 -175.1(18) . . . . ? C61 C62 C63 C64 1(4) . . . . ? C62 C63 C64 C65 -2(4) . . . . ? C63 C64 C65 C66 1(4) . . . . ? C62 C61 C66 C65 -2(3) . . . . ? P61 C61 C66 C65 174.4(16) . . . . ? C64 C65 C66 C61 1(3) . . . . ? C61 P61 O61 C67 171.7(15) . . . . ? Se62 P61 O61 C67 -72.0(15) . . . . ? Se61 P61 O61 C67 54.4(16) . . . . ? Se61 Cd42 Se71 P71 109.93(18) . . . . ? Se52 Cd42 Se71 P71 -107.04(17) . . . . ? Se72 Cd42 Se71 P71 -1.17(16) . . . . ? Se61 Cd42 Se72 P71 -118.61(16) . . . . ? Se52 Cd42 Se72 P71 112.68(17) . . . . ? Se71 Cd42 Se72 P71 1.18(16) . . . . ? Cd42 Se72 P71 O71 123.5(6) . . . . ? Cd42 Se72 P71 C71 -126.1(6) . . . . ? Cd42 Se72 P71 Se71 -1.6(2) . . . . ? Cd42 Se71 P71 O71 -123.0(6) . . . . ? Cd42 Se71 P71 C71 128.3(6) . . . . ? Cd42 Se71 P71 Se72 1.6(2) . . . . ? O71 P71 C71 C76 -178.9(15) . . . . ? Se72 P71 C71 C76 63.9(16) . . . . ? Se71 P71 C71 C76 -62.1(16) . . . . ? O71 P71 C71 C72 4.0(17) . . . . ? Se72 P71 C71 C72 -113.3(15) . . . . ? Se71 P71 C71 C72 120.8(15) . . . . ? C76 C71 C72 C73 3(3) . . . . ? P71 C71 C72 C73 -179.9(17) . . . . ? C71 C72 C73 C74 -2(3) . . . . ? C72 C73 C74 C75 -1(4) . . . . ? C73 C74 C75 C76 3(3) . . . . ? C72 C71 C76 C75 -1(3) . . . . ? P71 C71 C76 C75 -178.7(16) . . . . ? C74 C75 C76 C71 -1(3) . . . . ? C71 P71 O71 C77 -176.7(15) . . . . ? Se72 P71 O71 C77 -57.3(16) . . . . ? Se71 P71 O71 C77 68.1(16) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.593 _refine_diff_density_min -1.309 _refine_diff_density_rms 0.230 data_igdw44 _database_code_depnum_ccdc_archive 'CCDC 266258' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 O2 P2 Pb Se4' _chemical_formula_weight 829.29 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' 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' Pb Pb -3.3944 10.1111 '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 6.4975(7) _cell_length_b 13.1066(13) _cell_length_c 14.502(2) _cell_angle_alpha 110.741(14) _cell_angle_beta 97.96(2) _cell_angle_gamma 100.16(2) _cell_volume 1109.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 4081 _cell_measurement_theta_min 2.7121 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Platelet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0100 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 2.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 14.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3132 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optic' _diffrn_measurement_device_type ccd _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time ? _diffrn_standards_decay_% - _diffrn_reflns_number 6681 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.1026 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3780 _reflns_number_gt 3124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3780 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 0.602 _refine_ls_restrained_S_all 0.602 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.21605(4) 0.05464(2) 0.12720(2) 0.01558(13) Uani 1 1 d . . . Se1 Se 0.62606(11) 0.20687(6) 0.25059(5) 0.01482(19) Uani 1 1 d . . . Se2 Se 0.15056(11) 0.13336(7) 0.33463(6) 0.0181(2) Uani 1 1 d . . . P1 P 0.4952(3) 0.19297(16) 0.37633(14) 0.0125(4) Uani 1 1 d . . . C1 C 0.5817(12) 0.3242(6) 0.4853(5) 0.0162(17) Uani 1 1 d . . . C2 C 0.4379(14) 0.3728(8) 0.5374(6) 0.030(2) Uani 1 1 d . . . H2A H 0.2900 0.3358 0.5173 0.036 Uiso 1 1 calc R . . C3 C 0.5100(17) 0.4763(8) 0.6196(7) 0.042(3) Uani 1 1 d . . . H3A H 0.4106 0.5109 0.6539 0.050 Uiso 1 1 calc R . . C4 C 0.7240(18) 0.5274(8) 0.6504(7) 0.045(3) Uani 1 1 d . . . H4A H 0.7725 0.5967 0.7074 0.053 Uiso 1 1 calc R . . C5 C 0.8703(17) 0.4804(9) 0.6005(7) 0.042(3) Uani 1 1 d . . . H5A H 1.0181 0.5178 0.6220 0.050 Uiso 1 1 calc R . . C6 C 0.8004(13) 0.3772(7) 0.5179(6) 0.027(2) Uani 1 1 d . . . H6A H 0.9010 0.3431 0.4842 0.032 Uiso 1 1 calc R . . O1 O 0.6089(7) 0.1173(4) 0.4213(4) 0.0145(11) Uani 1 1 d . . . C7 C 0.5825(12) -0.0020(7) 0.3603(6) 0.0226(19) Uani 1 1 d . . . H7A H 0.6265 -0.0109 0.2957 0.027 Uiso 1 1 calc R . . H7B H 0.4303 -0.0426 0.3448 0.027 Uiso 1 1 calc R . . C8 C 0.7175(12) -0.0491(7) 0.4180(6) 0.0222(18) Uani 1 1 d . . . H8A H 0.7021 -0.1290 0.3777 0.033 Uiso 1 1 calc R . . H8B H 0.6717 -0.0410 0.4813 0.033 Uiso 1 1 calc R . . H8C H 0.8678 -0.0085 0.4332 0.033 Uiso 1 1 calc R . . Se11 Se 0.01866(11) 0.22114(7) 0.09608(6) 0.0175(2) Uani 1 1 d . . . Se12 Se 0.30871(11) 0.07672(6) -0.07849(6) 0.0171(2) Uani 1 1 d . . . P11 P 0.1881(3) 0.22458(17) -0.02257(15) 0.0154(4) Uani 1 1 d . . . C11 C 0.0163(13) 0.2423(8) -0.1208(6) 0.025(2) Uani 1 1 d . . . C12 C 0.0501(19) 0.2116(10) -0.2159(7) 0.050(3) Uani 1 1 d . B . H12A H 0.1593 0.1732 -0.2326 0.061 Uiso 1 1 calc R . . C13 C -0.0711(18) 0.2348(9) -0.2897(8) 0.046(3) Uani 1 1 d . . . H13A H -0.0388 0.2145 -0.3548 0.055 Uiso 1 1 calc R A 1 C14 C -0.2277(15) 0.2837(10) -0.2718(8) 0.049(3) Uani 1 1 d . B 1 H14A H -0.2791 0.3222 -0.3111 0.059 Uiso 1 1 calc R B 1 C15A C -0.309(3) 0.2763(16) -0.1966(14) 0.030(4) Uiso 0.50 1 d P B 1 H15A H -0.4496 0.2864 -0.1934 0.036 Uiso 0.50 1 calc PR B 1 C16A C -0.189(2) 0.2530(13) -0.1180(11) 0.016(3) Uiso 0.50 1 d P B 1 H16A H -0.2516 0.2451 -0.0648 0.019 Uiso 0.50 1 calc PR B 1 C15B C -0.226(3) 0.3560(18) -0.1585(15) 0.038(5) Uiso 0.50 1 d P B 2 C16B C -0.100(3) 0.3320(15) -0.0891(13) 0.028(4) Uiso 0.50 1 d P B 2 O11 O 0.3664(8) 0.3391(5) 0.0142(4) 0.0249(13) Uani 1 1 d . . . C17 C 0.5451(12) 0.3689(7) 0.0982(7) 0.0250(19) Uani 1 1 d . B . H17A H 0.6314 0.3123 0.0822 0.030 Uiso 1 1 calc R . . H17B H 0.4914 0.3702 0.1591 0.030 Uiso 1 1 calc R . . C18 C 0.680(2) 0.4814(10) 0.1179(9) 0.069(4) Uani 1 1 d . . . H18A H 0.8007 0.5019 0.1749 0.103 Uiso 1 1 calc R B . H18B H 0.5939 0.5372 0.1342 0.103 Uiso 1 1 calc R . . H18C H 0.7341 0.4795 0.0577 0.103 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 Pb1 0.0166(2) 0.0170(2) 0.01154(19) 0.00617(14) -0.00088(12) 0.00183(13) Se1 0.0135(4) 0.0192(4) 0.0123(4) 0.0074(3) 0.0030(3) 0.0022(3) Se2 0.0118(4) 0.0279(5) 0.0149(4) 0.0096(4) 0.0035(3) 0.0026(3) P1 0.0127(9) 0.0150(10) 0.0099(10) 0.0057(8) 0.0007(7) 0.0035(7) C1 0.026(4) 0.013(4) 0.011(4) 0.008(3) -0.002(3) 0.007(3) C2 0.038(5) 0.031(5) 0.018(5) 0.006(4) -0.004(4) 0.017(4) C3 0.071(7) 0.038(6) 0.012(5) -0.001(4) -0.003(4) 0.036(5) C4 0.091(8) 0.021(5) 0.012(5) 0.006(4) -0.007(5) 0.002(5) C5 0.057(6) 0.038(6) 0.020(5) 0.013(5) 0.000(4) -0.012(5) C6 0.033(5) 0.029(5) 0.015(4) 0.013(4) 0.002(3) -0.004(4) O1 0.018(3) 0.014(3) 0.014(3) 0.009(2) 0.005(2) 0.004(2) C7 0.023(4) 0.021(5) 0.019(4) 0.003(4) 0.002(3) 0.004(3) C8 0.026(4) 0.027(5) 0.018(4) 0.011(4) 0.008(3) 0.011(4) Se11 0.0182(4) 0.0236(4) 0.0143(4) 0.0088(3) 0.0065(3) 0.0087(3) Se12 0.0190(4) 0.0180(4) 0.0170(4) 0.0079(3) 0.0074(3) 0.0067(3) P11 0.0182(10) 0.0166(11) 0.0128(10) 0.0069(9) 0.0035(8) 0.0048(8) C11 0.030(5) 0.037(5) 0.026(5) 0.025(4) 0.015(4) 0.015(4) C12 0.084(8) 0.068(8) 0.019(5) 0.025(5) 0.011(5) 0.052(7) C13 0.076(8) 0.041(6) 0.029(6) 0.015(5) 0.011(5) 0.031(6) C14 0.031(5) 0.079(9) 0.055(7) 0.052(7) 0.008(5) 0.006(5) O11 0.030(3) 0.019(3) 0.024(3) 0.008(3) 0.009(2) 0.003(2) C17 0.022(4) 0.022(5) 0.033(5) 0.016(4) 0.003(4) 0.002(3) C18 0.096(9) 0.039(7) 0.043(7) 0.019(6) -0.022(6) -0.031(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 Pb1 Se11 2.8522(9) . ? Pb1 Se1 2.9249(12) . ? Pb1 Se2 2.9335(9) . ? Pb1 Se12 3.2235(10) . ? Se1 P1 2.166(2) . ? Se2 P1 2.160(2) . ? P1 O1 1.593(5) . ? P1 C1 1.805(7) . ? C1 C2 1.383(11) . ? C1 C6 1.399(11) . ? C2 C3 1.399(12) . ? C2 H2A 0.9500 . ? C3 C4 1.367(14) . ? C3 H3A 0.9500 . ? C4 C5 1.374(14) . ? C4 H4A 0.9500 . ? C5 C6 1.399(12) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? O1 C7 1.463(9) . ? C7 C8 1.486(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? Se11 P11 2.176(2) . ? Se12 P11 2.151(2) . ? P11 O11 1.591(6) . ? P11 C11 1.793(9) . ? C11 C12 1.354(13) . ? C11 C16A 1.369(16) . ? C11 C16B 1.479(18) . ? C12 C13 1.394(14) . ? C12 H12A 0.9500 . ? C13 C14 1.303(14) . ? C13 H13A 0.9500 . ? C14 C15A 1.30(2) . ? C14 H14A 0.9500 . ? C15A C16A 1.45(2) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C15B C16B 1.37(3) . ? O11 C17 1.448(10) . ? C17 C18 1.483(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se11 Pb1 Se1 97.05(3) . . ? Se11 Pb1 Se2 88.73(3) . . ? Se1 Pb1 Se2 75.22(3) . . ? Se11 Pb1 Se12 71.63(3) . . ? Se1 Pb1 Se12 93.82(3) . . ? Se2 Pb1 Se12 156.37(2) . . ? P1 Se1 Pb1 84.42(5) . . ? P1 Se2 Pb1 84.32(6) . . ? O1 P1 C1 98.8(3) . . ? O1 P1 Se2 112.8(2) . . ? C1 P1 Se2 112.0(2) . . ? O1 P1 Se1 110.2(2) . . ? C1 P1 Se1 111.0(3) . . ? Se2 P1 Se1 111.50(9) . . ? C2 C1 C6 119.5(7) . . ? C2 C1 P1 121.7(6) . . ? C6 C1 P1 118.8(6) . . ? C1 C2 C3 120.1(8) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C4 C3 C2 119.7(9) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 121.2(9) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C4 C5 C6 119.6(9) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C5 C6 C1 119.7(8) . . ? C5 C6 H6A 120.2 . . ? C1 C6 H6A 120.2 . . ? C7 O1 P1 120.3(5) . . ? O1 C7 C8 108.6(6) . . ? O1 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O1 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P11 Se11 Pb1 91.38(6) . . ? P11 Se12 Pb1 82.35(6) . . ? O11 P11 C11 98.7(4) . . ? O11 P11 Se12 113.7(2) . . ? C11 P11 Se12 112.3(3) . . ? O11 P11 Se11 110.8(2) . . ? C11 P11 Se11 109.7(3) . . ? Se12 P11 Se11 111.08(10) . . ? C12 C11 C16A 111.8(10) . . ? C12 C11 C16B 116.4(10) . . ? C16A C11 C16B 40.8(9) . . ? C12 C11 P11 121.8(7) . . ? C16A C11 P11 123.5(9) . . ? C16B C11 P11 116.9(9) . . ? C11 C12 C13 121.7(9) . . ? C11 C12 H12A 119.2 . . ? C13 C12 H12A 119.2 . . ? C14 C13 C12 121.7(10) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C15A C14 C13 115.7(13) . . ? C15A C14 H14A 122.1 . . ? C13 C14 H14A 122.1 . . ? C14 C15A C16A 120.9(15) . . ? C14 C15A H15A 119.6 . . ? C16A C15A H15A 119.6 . . ? C11 C16A C15A 119.6(14) . . ? C11 C16A H16A 120.2 . . ? C15A C16A H16A 120.2 . . ? C15B C16B C11 121.4(15) . . ? C17 O11 P11 121.1(6) . . ? O11 C17 C18 109.3(8) . . ? O11 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? O11 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se11 Pb1 Se1 P1 100.24(6) . . . . ? Se2 Pb1 Se1 P1 13.43(6) . . . . ? Se12 Pb1 Se1 P1 172.18(6) . . . . ? Se11 Pb1 Se2 P1 -111.11(6) . . . . ? Se1 Pb1 Se2 P1 -13.48(6) . . . . ? Se12 Pb1 Se2 P1 -77.95(8) . . . . ? Pb1 Se2 P1 O1 -105.5(2) . . . . ? Pb1 Se2 P1 C1 144.1(3) . . . . ? Pb1 Se2 P1 Se1 19.09(8) . . . . ? Pb1 Se1 P1 O1 106.9(2) . . . . ? Pb1 Se1 P1 C1 -144.7(3) . . . . ? Pb1 Se1 P1 Se2 -19.14(8) . . . . ? O1 P1 C1 C2 -114.6(7) . . . . ? Se2 P1 C1 C2 4.4(8) . . . . ? Se1 P1 C1 C2 129.7(7) . . . . ? O1 P1 C1 C6 64.8(7) . . . . ? Se2 P1 C1 C6 -176.2(6) . . . . ? Se1 P1 C1 C6 -50.9(7) . . . . ? C6 C1 C2 C3 2.6(14) . . . . ? P1 C1 C2 C3 -178.1(8) . . . . ? C1 C2 C3 C4 -2.2(15) . . . . ? C2 C3 C4 C5 1.6(16) . . . . ? C3 C4 C5 C6 -1.4(16) . . . . ? C4 C5 C6 C1 1.7(15) . . . . ? C2 C1 C6 C5 -2.3(13) . . . . ? P1 C1 C6 C5 178.3(7) . . . . ? C1 P1 O1 C7 178.7(5) . . . . ? Se2 P1 O1 C7 60.2(5) . . . . ? Se1 P1 O1 C7 -65.0(5) . . . . ? P1 O1 C7 C8 176.0(5) . . . . ? Se1 Pb1 Se11 P11 79.94(6) . . . . ? Se2 Pb1 Se11 P11 154.88(6) . . . . ? Se12 Pb1 Se11 P11 -11.76(5) . . . . ? Se11 Pb1 Se12 P11 12.00(5) . . . . ? Se1 Pb1 Se12 P11 -84.17(6) . . . . ? Se2 Pb1 Se12 P11 -23.18(8) . . . . ? Pb1 Se12 P11 O11 109.7(3) . . . . ? Pb1 Se12 P11 C11 -139.3(3) . . . . ? Pb1 Se12 P11 Se11 -16.09(7) . . . . ? Pb1 Se11 P11 O11 -109.3(3) . . . . ? Pb1 Se11 P11 C11 142.9(3) . . . . ? Pb1 Se11 P11 Se12 18.09(8) . . . . ? O11 P11 C11 C12 86.0(9) . . . . ? Se12 P11 C11 C12 -34.1(10) . . . . ? Se11 P11 C11 C12 -158.1(9) . . . . ? O11 P11 C11 C16A -115.2(10) . . . . ? Se12 P11 C11 C16A 124.7(10) . . . . ? Se11 P11 C11 C16A 0.6(11) . . . . ? O11 P11 C11 C16B -68.1(10) . . . . ? Se12 P11 C11 C16B 171.7(9) . . . . ? Se11 P11 C11 C16B 47.7(10) . . . . ? C16A C11 C12 C13 25.0(17) . . . . ? C16B C11 C12 C13 -19.7(18) . . . . ? P11 C11 C12 C13 -174.0(9) . . . . ? C11 C12 C13 C14 -2.5(19) . . . . ? C12 C13 C14 C15A -21.6(19) . . . . ? C13 C14 C15A C16A 21(2) . . . . ? C12 C11 C16A C15A -24.5(18) . . . . ? C16B C11 C16A C15A 81.2(19) . . . . ? P11 C11 C16A C15A 174.9(11) . . . . ? C14 C15A C16A C11 2(2) . . . . ? C12 C11 C16B C15B 21(2) . . . . ? C16A C11 C16B C15B -72.3(19) . . . . ? P11 C11 C16B C15B 176.7(14) . . . . ? C11 P11 O11 C17 177.7(6) . . . . ? Se12 P11 O11 C17 -63.2(6) . . . . ? Se11 P11 O11 C17 62.7(6) . . . . ? P11 O11 C17 C18 -177.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 1.938 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.253 data_4 _database_code_depnum_ccdc_archive 'CCDC 266259' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H14 Na O3 P Se' _chemical_formula_weight 303.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 '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 25.7072(6) _cell_length_b 8.4911(2) _cell_length_c 25.3606(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.228(2) _cell_angle_gamma 90.00 _cell_volume 5124.4(2) _cell_formula_units_Z 16 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 3526 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 69.72 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 5.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4395 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optic' _diffrn_measurement_device_type 'image plate' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.82 _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time ? _diffrn_standards_decay_% - _diffrn_reflns_number 7507 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 70.01 _reflns_number_total 4475 _reflns_number_gt 4370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+19.4639P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00056(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4475 _refine_ls_number_parameters 289 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.060 _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 1.05313(5) 0.35757(14) 0.22913(5) 0.0234(3) Uani 1 1 d . . . Na11 Na 0.95530(5) 0.69123(14) 0.18272(5) 0.0233(3) Uani 1 1 d . . . Se1 Se 1.168202(15) 0.77421(4) 0.310661(16) 0.02858(15) Uani 1 1 d . . . P1 P 1.11099(3) 0.68598(9) 0.23161(3) 0.0215(2) Uani 1 1 d . . . O1 O 1.05156(9) 0.6643(3) 0.22767(9) 0.0249(5) Uani 1 1 d . . . C1 C 1.11247(14) 0.7998(4) 0.17189(14) 0.0255(7) Uani 1 1 d . . . C2 C 1.07305(18) 0.7645(5) 0.11790(17) 0.0368(9) Uani 1 1 d . . . H2A H 1.0453 0.6861 0.1133 0.044 Uiso 1 1 calc R . . C3 C 1.07478(19) 0.8448(6) 0.07114(17) 0.0503(11) Uani 1 1 d . . . H3A H 1.0476 0.8216 0.0344 0.060 Uiso 1 1 calc R . . C4 C 1.1146(2) 0.9565(5) 0.07658(18) 0.0465(10) Uani 1 1 d . . . H4A H 1.1154 1.0091 0.0438 0.056 Uiso 1 1 calc R . . C5 C 1.1536(2) 0.9928(5) 0.12988(19) 0.0451(10) Uani 1 1 d . . . H5A H 1.1812 1.0713 0.1338 0.054 Uiso 1 1 calc R . . C6 C 1.15286(16) 0.9152(4) 0.17778(15) 0.0316(7) Uani 1 1 d . . . H6A H 1.1798 0.9406 0.2144 0.038 Uiso 1 1 calc R . . O7 O 1.12741(9) 0.5098(3) 0.21925(10) 0.0260(5) Uani 1 1 d . . . C7 C 1.18201(15) 0.4667(4) 0.21817(18) 0.0367(8) Uani 1 1 d . . . H7A H 1.2114 0.5416 0.2423 0.044 Uiso 1 1 calc R . . C8 C 1.19459(18) 0.3047(5) 0.24276(19) 0.0431(9) Uani 1 1 d . . . H8A H 1.1966 0.3061 0.2821 0.065 Uiso 1 1 calc R . . H8B H 1.2306 0.2692 0.2422 0.065 Uiso 1 1 calc R . . H8C H 1.1648 0.2325 0.2201 0.065 Uiso 1 1 calc R . . C9 C 1.1797(3) 0.4713(7) 0.1581(3) 0.086(2) Uani 1 1 d . . . H9A H 1.1719 0.5791 0.1434 0.130 Uiso 1 1 calc R . . H9B H 1.1499 0.4010 0.1342 0.130 Uiso 1 1 calc R . . H9C H 1.2159 0.4368 0.1576 0.130 Uiso 1 1 calc R . . O10 O 1.07612(11) 0.0913(3) 0.25831(11) 0.0330(5) Uani 1 1 d D . . H10A H 1.0585(18) 0.052(6) 0.2839(17) 0.064(15) Uiso 1 1 d D . . H10B H 1.1118(11) 0.034(5) 0.272(2) 0.070(16) Uiso 1 1 d D . . Se11 Se 0.991187(16) 0.24707(4) 0.092694(16) 0.02915(15) Uani 1 1 d . . . P11 P 0.93415(3) 0.36798(9) 0.12090(3) 0.0226(2) Uani 1 1 d . . . O11 O 0.95527(9) 0.4012(3) 0.18381(9) 0.0239(5) Uani 1 1 d . . . C11 C 0.86582(15) 0.2768(4) 0.09803(14) 0.0270(7) Uani 1 1 d . . . C12 C 0.85172(15) 0.1413(4) 0.06523(16) 0.0354(8) Uani 1 1 d . . . H12A H 0.8786 0.0927 0.0531 0.042 Uiso 1 1 calc R . . C13 C 0.79834(17) 0.0759(5) 0.05003(19) 0.0462(10) Uani 1 1 d . . . H13A H 0.7891 -0.0181 0.0281 0.055 Uiso 1 1 calc R . . C14 C 0.75928(17) 0.1464(5) 0.06649(17) 0.0423(9) Uani 1 1 d . . . H14A H 0.7230 0.1009 0.0559 0.051 Uiso 1 1 calc R . . C15 C 0.77174(17) 0.2821(5) 0.09812(18) 0.0412(9) Uani 1 1 d . . . H15A H 0.7441 0.3310 0.1090 0.049 Uiso 1 1 calc R . . C16 C 0.82503(15) 0.3478(5) 0.11417(16) 0.0358(8) Uani 1 1 d . . . H16A H 0.8338 0.4416 0.1362 0.043 Uiso 1 1 calc R . . O17 O 0.92091(10) 0.5429(3) 0.09359(9) 0.0273(5) Uani 1 1 d . . . C17 C 0.89436(15) 0.5653(4) 0.03177(14) 0.0327(8) Uani 1 1 d . . . H17A H 0.8823 0.4611 0.0127 0.039 Uiso 1 1 calc R . . C18 C 0.93662(18) 0.6393(6) 0.01162(17) 0.0460(10) Uani 1 1 d . . . H18A H 0.9686 0.5678 0.0193 0.069 Uiso 1 1 calc R . . H18B H 0.9498 0.7388 0.0319 0.069 Uiso 1 1 calc R . . H18C H 0.9191 0.6596 -0.0294 0.069 Uiso 1 1 calc R . . C19 C 0.84323(17) 0.6687(5) 0.02115(19) 0.0468(10) Uani 1 1 d . . . H19A H 0.8170 0.6150 0.0349 0.070 Uiso 1 1 calc R . . H19B H 0.8246 0.6891 -0.0198 0.070 Uiso 1 1 calc R . . H19C H 0.8550 0.7687 0.0415 0.070 Uiso 1 1 calc R . . O20 O 0.97645(11) 0.9554(3) 0.17280(11) 0.0328(5) Uani 1 1 d D . . H20A H 1.0147(9) 0.972(7) 0.2006(18) 0.078(18) Uiso 1 1 d D . . H20B H 0.969(2) 1.016(5) 0.1378(12) 0.064(15) Uiso 1 1 d 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 Na1 0.0253(6) 0.0181(6) 0.0300(6) 0.0003(5) 0.0139(5) -0.0004(5) Na11 0.0262(6) 0.0171(6) 0.0275(6) 0.0000(5) 0.0114(5) 0.0003(5) Se1 0.0277(2) 0.0278(2) 0.0297(2) -0.00151(14) 0.01033(16) -0.00361(14) P1 0.0226(4) 0.0168(4) 0.0282(4) 0.0004(3) 0.0129(3) -0.0001(3) O1 0.0206(11) 0.0253(11) 0.0299(11) 0.0007(9) 0.0110(9) -0.0016(9) C1 0.0321(17) 0.0202(15) 0.0292(16) 0.0053(13) 0.0171(13) 0.0060(13) C2 0.039(2) 0.043(2) 0.0327(19) 0.0025(15) 0.0183(17) -0.0001(16) C3 0.052(2) 0.069(3) 0.0298(19) 0.004(2) 0.0157(18) 0.006(2) C4 0.069(3) 0.042(2) 0.041(2) 0.0145(18) 0.035(2) 0.011(2) C5 0.070(3) 0.0248(19) 0.056(2) 0.0057(17) 0.042(2) 0.0023(19) C6 0.046(2) 0.0187(15) 0.0394(18) -0.0013(14) 0.0266(16) -0.0033(14) O7 0.0235(11) 0.0189(11) 0.0417(13) -0.0002(9) 0.0192(10) 0.0012(9) C7 0.0280(17) 0.0233(17) 0.069(3) -0.0027(17) 0.0297(17) 0.0000(14) C8 0.045(2) 0.039(2) 0.052(2) 0.0054(19) 0.0258(19) 0.0153(19) C9 0.114(5) 0.078(4) 0.115(5) 0.058(4) 0.098(4) 0.067(4) O10 0.0387(13) 0.0207(12) 0.0449(14) 0.0005(10) 0.0218(11) 0.0014(10) Se11 0.0356(3) 0.0264(2) 0.0310(2) 0.00089(13) 0.01903(18) 0.00358(14) P11 0.0275(4) 0.0180(4) 0.0237(4) -0.0009(3) 0.0110(3) -0.0006(3) O11 0.0281(11) 0.0215(11) 0.0234(11) -0.0033(8) 0.0113(9) -0.0051(9) C11 0.0306(17) 0.0233(16) 0.0268(16) -0.0002(13) 0.0106(14) -0.0031(13) C12 0.0360(19) 0.0250(18) 0.041(2) -0.0065(15) 0.0100(15) 0.0010(15) C13 0.042(2) 0.0277(19) 0.059(2) -0.0088(18) 0.0079(18) -0.0048(17) C14 0.0347(19) 0.042(2) 0.045(2) 0.0024(17) 0.0090(16) -0.0092(17) C15 0.0328(19) 0.051(2) 0.045(2) -0.0040(18) 0.0203(17) -0.0030(18) C16 0.0363(19) 0.035(2) 0.0387(19) -0.0126(15) 0.0167(15) -0.0076(16) O17 0.0351(12) 0.0189(11) 0.0268(11) 0.0014(9) 0.0104(9) 0.0003(9) C17 0.0381(19) 0.0272(17) 0.0267(16) 0.0032(14) 0.0051(14) -0.0007(15) C18 0.048(2) 0.052(3) 0.038(2) 0.0143(19) 0.0164(17) -0.003(2) C19 0.041(2) 0.035(2) 0.052(2) 0.0096(18) 0.0044(18) 0.0076(18) O20 0.0379(13) 0.0217(12) 0.0413(13) 0.0039(10) 0.0179(11) 0.0023(10) _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 O11 2.328(2) 2_755 ? Na1 O11 2.366(2) . ? Na1 O10 2.383(3) . ? Na1 O7 2.396(2) . ? Na1 O1 2.605(3) . ? Na1 P1 3.1498(14) . ? Na1 P11 3.2474(14) . ? Na1 Na1 3.282(2) 2_755 ? Na1 Se11 3.3496(13) . ? Na1 Na11 3.6658(17) 2_755 ? Na1 Na11 3.6739(17) . ? Na11 O1 2.311(2) . ? Na11 O20 2.344(3) . ? Na11 O1 2.356(2) 2_755 ? Na11 O17 2.442(2) . ? Na11 O11 2.463(3) . ? Na11 P11 3.1052(14) . ? Na11 P1 3.2291(14) 2_755 ? Na11 Na11 3.316(2) 2_755 ? Na11 Se1 3.3178(13) 2_755 ? Na11 Na1 3.6658(17) 2_755 ? Se1 P1 2.1243(9) . ? Se1 Na11 3.3178(13) 2_755 ? P1 O1 1.504(2) . ? P1 O7 1.617(2) . ? P1 C1 1.809(3) . ? P1 Na11 3.2291(14) 2_755 ? O1 Na11 2.356(2) 2_755 ? C1 C2 1.393(5) . ? C1 C6 1.394(5) . ? C2 C3 1.383(6) . ? C2 H2A 0.9500 . ? C3 C4 1.363(7) . ? C3 H3A 0.9500 . ? C4 C5 1.380(7) . ? C4 H4A 0.9500 . ? C5 C6 1.389(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? O7 C7 1.461(4) . ? C7 C8 1.494(5) . ? C7 C9 1.502(7) . ? C7 H7A 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O10 H10A 0.9800(10) . ? O10 H10B 0.9799(11) . ? Se11 P11 2.1234(9) . ? P11 O11 1.505(2) . ? P11 O17 1.619(2) . ? P11 C11 1.803(4) . ? O11 Na1 2.328(2) 2_755 ? C11 C12 1.386(5) . ? C11 C16 1.399(5) . ? C12 C13 1.392(5) . ? C12 H12A 0.9500 . ? C13 C14 1.363(6) . ? C13 H13A 0.9500 . ? C14 C15 1.371(6) . ? C14 H14A 0.9500 . ? C15 C16 1.390(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? O17 C17 1.467(4) . ? C17 C18 1.502(5) . ? C17 C19 1.518(5) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O20 H20A 0.9800(11) . ? O20 H20B 0.9800(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 O11 Na1 O11 88.43(8) 2_755 . ? O11 Na1 O10 87.57(9) 2_755 . ? O11 Na1 O10 113.12(9) . . ? O11 Na1 O7 112.13(9) 2_755 . ? O11 Na1 O7 127.41(9) . . ? O10 Na1 O7 115.50(9) . . ? O11 Na1 O1 81.24(8) 2_755 . ? O11 Na1 O1 80.13(8) . . ? O10 Na1 O1 162.52(10) . . ? O7 Na1 O1 57.85(7) . . ? O11 Na1 P1 93.01(7) 2_755 . ? O11 Na1 P1 106.15(7) . . ? O10 Na1 P1 140.72(8) . . ? O7 Na1 P1 30.18(5) . . ? O1 Na1 P1 28.33(5) . . ? O11 Na1 P11 113.68(7) 2_755 . ? O11 Na1 P11 25.43(5) . . ? O10 Na1 P11 109.39(8) . . ? O7 Na1 P11 115.47(7) . . ? O1 Na1 P11 87.49(6) . . ? P1 Na1 P11 106.23(4) . . ? O11 Na1 Na1 46.13(6) 2_755 2_755 ? O11 Na1 Na1 45.17(6) . 2_755 ? O10 Na1 Na1 92.21(7) . 2_755 ? O7 Na1 Na1 145.81(6) . 2_755 ? O1 Na1 Na1 89.67(5) . 2_755 ? P1 Na1 Na1 115.97(3) . 2_755 ? P11 Na1 Na1 68.89(4) . 2_755 ? O11 Na1 Se11 147.77(7) 2_755 . ? O11 Na1 Se11 62.58(6) . . ? O10 Na1 Se11 91.16(7) . . ? O7 Na1 Se11 97.43(7) . . ? O1 Na1 Se11 105.47(6) . . ? P1 Na1 Se11 107.76(4) . . ? P11 Na1 Se11 37.51(2) . . ? Na1 Na1 Se11 101.81(5) 2_755 . ? O11 Na1 Na11 41.45(6) 2_755 2_755 ? O11 Na1 Na11 82.98(6) . 2_755 ? O10 Na1 Na11 127.50(8) . 2_755 ? O7 Na1 Na11 83.12(6) . 2_755 ? O1 Na1 Na11 39.80(5) . 2_755 ? P1 Na1 Na11 55.94(3) . 2_755 ? P11 Na1 Na11 103.91(4) . 2_755 ? Na1 Na1 Na11 63.57(3) 2_755 2_755 ? Se11 Na1 Na11 137.04(4) . 2_755 ? O11 Na1 Na11 83.29(6) 2_755 . ? O11 Na1 Na11 41.45(6) . . ? O10 Na1 Na11 152.93(8) . . ? O7 Na1 Na11 91.52(6) . . ? O1 Na1 Na11 38.68(5) . . ? P1 Na1 Na11 65.45(3) . . ? P11 Na1 Na11 52.88(3) . . ? Na1 Na1 Na11 63.31(3) 2_755 . ? Se11 Na1 Na11 83.38(3) . . ? Na11 Na1 Na11 53.71(4) 2_755 . ? O1 Na11 O20 84.21(9) . . ? O1 Na11 O1 88.36(8) . 2_755 ? O20 Na11 O1 107.55(10) . 2_755 ? O1 Na11 O17 110.52(9) . . ? O20 Na11 O17 114.31(9) . . ? O1 Na11 O17 135.20(9) 2_755 . ? O1 Na11 O11 84.27(9) . . ? O20 Na11 O11 163.58(10) . . ? O1 Na11 O11 83.77(8) 2_755 . ? O17 Na11 O11 59.55(7) . . ? O1 Na11 P11 96.42(7) . . ? O20 Na11 P11 142.67(8) . . ? O1 Na11 P11 109.78(7) 2_755 . ? O17 Na11 P11 31.12(5) . . ? O11 Na11 P11 28.49(5) . . ? O1 Na11 P1 113.94(7) . 2_755 ? O20 Na11 P1 106.76(8) . 2_755 ? O1 Na11 P1 25.66(5) 2_755 2_755 ? O17 Na11 P1 121.14(7) . 2_755 ? O11 Na11 P1 88.63(6) . 2_755 ? P11 Na11 P1 106.94(4) . 2_755 ? O1 Na11 Na11 45.28(6) . 2_755 ? O20 Na11 Na11 90.68(7) . 2_755 ? O1 Na11 Na11 44.18(6) 2_755 2_755 ? O17 Na11 Na11 145.06(7) . 2_755 ? O11 Na11 Na11 89.51(6) . 2_755 ? P11 Na11 Na11 116.13(3) . 2_755 ? P1 Na11 Na11 69.16(4) 2_755 2_755 ? O1 Na11 Se1 149.61(7) . 2_755 ? O20 Na11 Se1 93.87(7) . 2_755 ? O1 Na11 Se1 63.23(6) 2_755 2_755 ? O17 Na11 Se1 97.94(7) . 2_755 ? O11 Na11 Se1 101.97(6) . 2_755 ? P11 Na11 Se1 103.01(4) . 2_755 ? P1 Na11 Se1 37.84(2) 2_755 2_755 ? Na11 Na11 Se1 104.59(5) 2_755 2_755 ? O1 Na11 Na1 85.52(7) . 2_755 ? O20 Na11 Na1 151.01(8) . 2_755 ? O1 Na11 Na1 45.04(6) 2_755 2_755 ? O17 Na11 Na1 94.68(7) . 2_755 ? O11 Na11 Na1 38.74(5) . 2_755 ? P11 Na11 Na1 65.50(3) . 2_755 ? P1 Na11 Na1 53.91(3) 2_755 2_755 ? Na11 Na11 Na1 63.27(3) 2_755 2_755 ? Se1 Na11 Na1 81.65(3) 2_755 2_755 ? O1 Na11 Na1 44.77(6) . . ? O20 Na11 Na1 127.87(8) . . ? O1 Na11 Na1 84.72(6) 2_755 . ? O17 Na11 Na1 82.13(6) . . ? O11 Na11 Na1 39.50(6) . . ? P11 Na11 Na1 56.50(3) . . ? P1 Na11 Na1 104.20(4) 2_755 . ? Na11 Na11 Na1 63.02(3) 2_755 . ? Se1 Na11 Na1 134.41(4) 2_755 . ? Na1 Na11 Na1 53.12(4) 2_755 . ? P1 Se1 Na11 68.82(3) . 2_755 ? O1 P1 O7 101.94(12) . . ? O1 P1 C1 110.63(14) . . ? O7 P1 C1 104.02(13) . . ? O1 P1 Se1 115.42(9) . . ? O7 P1 Se1 111.77(9) . . ? C1 P1 Se1 112.04(12) . . ? O1 P1 Na1 55.26(9) . . ? O7 P1 Na1 48.16(8) . . ? C1 P1 Na1 128.00(12) . . ? Se1 P1 Na1 118.96(4) . . ? O1 P1 Na11 42.71(9) . 2_755 ? O7 P1 Na11 112.72(8) . 2_755 ? C1 P1 Na11 137.69(11) . 2_755 ? Se1 P1 Na11 73.35(3) . 2_755 ? Na1 P1 Na11 70.14(3) . 2_755 ? P1 O1 Na11 153.09(14) . . ? P1 O1 Na11 111.64(12) . 2_755 ? Na11 O1 Na11 90.54(8) . 2_755 ? P1 O1 Na1 96.41(11) . . ? Na11 O1 Na1 96.55(9) . . ? Na11 O1 Na1 95.16(9) 2_755 . ? C2 C1 C6 119.5(3) . . ? C2 C1 P1 118.0(3) . . ? C6 C1 P1 122.5(3) . . ? C3 C2 C1 119.3(4) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C4 C3 C2 121.5(4) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 119.8(4) . . ? C5 C6 H6A 120.1 . . ? C1 C6 H6A 120.1 . . ? C7 O7 P1 124.0(2) . . ? C7 O7 Na1 132.53(19) . . ? P1 O7 Na1 101.65(10) . . ? O7 C7 C8 106.3(3) . . ? O7 C7 C9 110.1(4) . . ? C8 C7 C9 111.5(4) . . ? O7 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? C9 C7 H7A 109.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Na1 O10 H10A 114(3) . . ? Na1 O10 H10B 132(3) . . ? H10A O10 H10B 102(4) . . ? P11 Se11 Na1 68.63(3) . . ? O11 P11 O17 102.39(12) . . ? O11 P11 C11 109.77(14) . . ? O17 P11 C11 103.57(14) . . ? O11 P11 Se11 115.45(9) . . ? O17 P11 Se11 111.08(9) . . ? C11 P11 Se11 113.39(12) . . ? O11 P11 Na11 51.31(9) . . ? O17 P11 Na11 51.22(8) . . ? C11 P11 Na11 120.34(12) . . ? Se11 P11 Na11 125.88(4) . . ? O11 P11 Na1 42.46(9) . . ? O17 P11 Na1 111.39(9) . . ? C11 P11 Na1 138.74(11) . . ? Se11 P11 Na1 73.85(3) . . ? Na11 P11 Na1 70.63(3) . . ? P11 O11 Na1 148.21(13) . 2_755 ? P11 O11 Na1 112.11(12) . . ? Na1 O11 Na1 88.71(8) 2_755 . ? P11 O11 Na11 100.20(11) . . ? Na1 O11 Na11 99.81(9) 2_755 . ? Na1 O11 Na11 99.05(9) . . ? C12 C11 C16 118.6(3) . . ? C12 C11 P11 123.5(3) . . ? C16 C11 P11 117.9(3) . . ? C11 C12 C13 120.3(4) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? C13 C14 C15 120.8(4) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C14 C15 C16 119.7(4) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C15 C16 C11 120.4(3) . . ? C15 C16 H16A 119.8 . . ? C11 C16 H16A 119.8 . . ? C17 O17 P11 120.9(2) . . ? C17 O17 Na11 141.41(19) . . ? P11 O17 Na11 97.66(10) . . ? O17 C17 C18 108.3(3) . . ? O17 C17 C19 106.6(3) . . ? C18 C17 C19 112.8(3) . . ? O17 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? C19 C17 H17A 109.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Na11 O20 H20A 106(4) . . ? Na11 O20 H20B 129(3) . . ? H20A O20 H20B 112(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Na1 Na11 O1 84.35(10) 2_755 . . . ? O11 Na1 Na11 O1 179.61(13) . . . . ? O10 Na1 Na11 O1 155.4(2) . . . . ? O7 Na1 Na11 O1 -27.76(10) . . . . ? P1 Na1 Na11 O1 -12.07(8) . . . . ? P11 Na1 Na11 O1 -149.05(9) . . . . ? Na1 Na1 Na11 O1 128.14(10) 2_755 . . . ? Se11 Na1 Na11 O1 -125.06(9) . . . . ? Na11 Na1 Na11 O1 52.56(8) 2_755 . . . ? O11 Na1 Na11 O20 99.52(11) 2_755 . . . ? O11 Na1 Na11 O20 -165.23(13) . . . . ? O10 Na1 Na11 O20 170.61(18) . . . . ? O7 Na1 Na11 O20 -12.59(12) . . . . ? O1 Na1 Na11 O20 15.17(12) . . . . ? P1 Na1 Na11 O20 3.09(9) . . . . ? P11 Na1 Na11 O20 -133.88(10) . . . . ? Na1 Na1 Na11 O20 143.30(10) 2_755 . . . ? Se11 Na1 Na11 O20 -109.90(10) . . . . ? Na11 Na1 Na11 O20 67.73(9) 2_755 . . . ? O11 Na1 Na11 O1 -8.65(9) 2_755 . . 2_755 ? O11 Na1 Na11 O1 86.60(10) . . . 2_755 ? O10 Na1 Na11 O1 62.44(19) . . . 2_755 ? O7 Na1 Na11 O1 -120.76(9) . . . 2_755 ? O1 Na1 Na11 O1 -93.00(10) . . . 2_755 ? P1 Na1 Na11 O1 -105.07(7) . . . 2_755 ? P11 Na1 Na11 O1 117.95(7) . . . 2_755 ? Na1 Na1 Na11 O1 35.14(7) 2_755 . . 2_755 ? Se11 Na1 Na11 O1 141.93(6) . . . 2_755 ? Na11 Na1 Na11 O1 -40.44(6) 2_755 . . 2_755 ? O11 Na1 Na11 O17 -145.71(9) 2_755 . . . ? O11 Na1 Na11 O17 -50.46(10) . . . . ? O10 Na1 Na11 O17 -74.62(18) . . . . ? O7 Na1 Na11 O17 102.18(9) . . . . ? O1 Na1 Na11 O17 129.93(11) . . . . ? P1 Na1 Na11 O17 117.86(7) . . . . ? P11 Na1 Na11 O17 -19.11(6) . . . . ? Na1 Na1 Na11 O17 -101.93(7) 2_755 . . . ? Se11 Na1 Na11 O17 4.87(6) . . . . ? Na11 Na1 Na11 O17 -177.51(8) 2_755 . . . ? O11 Na1 Na11 O11 -95.25(10) 2_755 . . . ? O10 Na1 Na11 O11 -24.16(18) . . . . ? O7 Na1 Na11 O11 152.64(11) . . . . ? O1 Na1 Na11 O11 -179.61(13) . . . . ? P1 Na1 Na11 O11 168.32(9) . . . . ? P11 Na1 Na11 O11 31.35(8) . . . . ? Na1 Na1 Na11 O11 -51.47(8) 2_755 . . . ? Se11 Na1 Na11 O11 55.33(8) . . . . ? Na11 Na1 Na11 O11 -127.05(10) 2_755 . . . ? O11 Na1 Na11 P11 -126.60(7) 2_755 . . . ? O11 Na1 Na11 P11 -31.35(8) . . . . ? O10 Na1 Na11 P11 -55.51(17) . . . . ? O7 Na1 Na11 P11 121.29(7) . . . . ? O1 Na1 Na11 P11 149.05(9) . . . . ? P1 Na1 Na11 P11 136.97(4) . . . . ? Na1 Na1 Na11 P11 -82.82(4) 2_755 . . . ? Se11 Na1 Na11 P11 23.98(2) . . . . ? Na11 Na1 Na11 P11 -158.39(5) 2_755 . . . ? O11 Na1 Na11 P1 -25.48(7) 2_755 . . 2_755 ? O11 Na1 Na11 P1 69.77(9) . . . 2_755 ? O10 Na1 Na11 P1 45.61(18) . . . 2_755 ? O7 Na1 Na11 P1 -137.59(7) . . . 2_755 ? O1 Na1 Na11 P1 -109.83(9) . . . 2_755 ? P1 Na1 Na11 P1 -121.90(4) . . . 2_755 ? P11 Na1 Na11 P1 101.12(4) . . . 2_755 ? Na1 Na1 Na11 P1 18.31(4) 2_755 . . 2_755 ? Se11 Na1 Na11 P1 125.10(4) . . . 2_755 ? Na11 Na1 Na11 P1 -57.27(4) 2_755 . . 2_755 ? O11 Na1 Na11 Na11 31.79(7) 2_755 . . 2_755 ? O11 Na1 Na11 Na11 127.05(10) . . . 2_755 ? O10 Na1 Na11 Na11 102.89(17) . . . 2_755 ? O7 Na1 Na11 Na11 -80.32(7) . . . 2_755 ? O1 Na1 Na11 Na11 -52.56(8) . . . 2_755 ? P1 Na1 Na11 Na11 -64.63(4) . . . 2_755 ? P11 Na1 Na11 Na11 158.39(5) . . . 2_755 ? Na1 Na1 Na11 Na11 75.58(5) 2_755 . . 2_755 ? Se11 Na1 Na11 Na11 -177.62(4) . . . 2_755 ? O11 Na1 Na11 Se1 -52.29(8) 2_755 . . 2_755 ? O11 Na1 Na11 Se1 42.96(9) . . . 2_755 ? O10 Na1 Na11 Se1 18.8(2) . . . 2_755 ? O7 Na1 Na11 Se1 -164.40(7) . . . 2_755 ? O1 Na1 Na11 Se1 -136.64(10) . . . 2_755 ? P1 Na1 Na11 Se1 -148.72(6) . . . 2_755 ? P11 Na1 Na11 Se1 74.31(6) . . . 2_755 ? Na1 Na1 Na11 Se1 -8.51(6) 2_755 . . 2_755 ? Se11 Na1 Na11 Se1 98.29(5) . . . 2_755 ? Na11 Na1 Na11 Se1 -84.08(7) 2_755 . . 2_755 ? O11 Na1 Na11 Na1 -43.78(7) 2_755 . . 2_755 ? O11 Na1 Na11 Na1 51.47(8) . . . 2_755 ? O10 Na1 Na11 Na1 27.31(16) . . . 2_755 ? O7 Na1 Na11 Na1 -155.89(8) . . . 2_755 ? O1 Na1 Na11 Na1 -128.14(10) . . . 2_755 ? P1 Na1 Na11 Na1 -140.21(5) . . . 2_755 ? P11 Na1 Na11 Na1 82.82(4) . . . 2_755 ? Se11 Na1 Na11 Na1 106.80(4) . . . 2_755 ? Na11 Na1 Na11 Na1 -75.58(5) 2_755 . . 2_755 ? Na11 Se1 P1 O1 7.54(10) 2_755 . . . ? Na11 Se1 P1 O7 -108.33(9) 2_755 . . . ? Na11 Se1 P1 C1 135.36(12) 2_755 . . . ? Na11 Se1 P1 Na1 -55.20(4) 2_755 . . . ? O11 Na1 P1 O1 -65.23(12) 2_755 . . . ? O11 Na1 P1 O1 24.01(12) . . . . ? O10 Na1 P1 O1 -155.07(17) . . . . ? O7 Na1 P1 O1 163.48(16) . . . . ? P11 Na1 P1 O1 50.50(11) . . . . ? Na1 Na1 P1 O1 -23.51(11) 2_755 . . . ? Se11 Na1 P1 O1 89.77(11) . . . . ? Na11 Na1 P1 O1 -45.55(11) 2_755 . . . ? Na11 Na1 P1 O1 15.99(11) . . . . ? O11 Na1 P1 O7 131.29(13) 2_755 . . . ? O11 Na1 P1 O7 -139.47(13) . . . . ? O10 Na1 P1 O7 41.45(16) . . . . ? O1 Na1 P1 O7 -163.48(16) . . . . ? P11 Na1 P1 O7 -112.97(12) . . . . ? Na1 Na1 P1 O7 173.02(13) 2_755 . . . ? Se11 Na1 P1 O7 -73.71(12) . . . . ? Na11 Na1 P1 O7 150.97(12) 2_755 . . . ? Na11 Na1 P1 O7 -147.49(12) . . . . ? O11 Na1 P1 C1 -155.37(15) 2_755 . . . ? O11 Na1 P1 C1 -66.13(15) . . . . ? O10 Na1 P1 C1 114.79(18) . . . . ? O7 Na1 P1 C1 73.34(17) . . . . ? O1 Na1 P1 C1 -90.14(17) . . . . ? P11 Na1 P1 C1 -39.63(14) . . . . ? Na1 Na1 P1 C1 -113.64(14) 2_755 . . . ? Se11 Na1 P1 C1 -0.37(14) . . . . ? Na11 Na1 P1 C1 -135.69(14) 2_755 . . . ? Na11 Na1 P1 C1 -74.15(14) . . . . ? O11 Na1 P1 Se1 37.08(7) 2_755 . . . ? O11 Na1 P1 Se1 126.32(7) . . . . ? O10 Na1 P1 Se1 -52.76(13) . . . . ? O7 Na1 P1 Se1 -94.21(12) . . . . ? O1 Na1 P1 Se1 102.31(11) . . . . ? P11 Na1 P1 Se1 152.81(4) . . . . ? Na1 Na1 P1 Se1 78.80(7) 2_755 . . . ? Se11 Na1 P1 Se1 -167.92(3) . . . . ? Na11 Na1 P1 Se1 56.76(4) 2_755 . . . ? Na11 Na1 P1 Se1 118.30(4) . . . . ? O11 Na1 P1 Na11 -19.68(6) 2_755 . . 2_755 ? O11 Na1 P1 Na11 69.56(7) . . . 2_755 ? O10 Na1 P1 Na11 -109.52(12) . . . 2_755 ? O7 Na1 P1 Na11 -150.97(12) . . . 2_755 ? O1 Na1 P1 Na11 45.55(11) . . . 2_755 ? P11 Na1 P1 Na11 96.05(4) . . . 2_755 ? Na1 Na1 P1 Na11 22.04(6) 2_755 . . 2_755 ? Se11 Na1 P1 Na11 135.31(4) . . . 2_755 ? Na11 Na1 P1 Na11 61.54(4) . . . 2_755 ? O7 P1 O1 Na11 -105.9(3) . . . . ? C1 P1 O1 Na11 4.3(4) . . . . ? Se1 P1 O1 Na11 132.8(3) . . . . ? Na1 P1 O1 Na11 -118.4(3) . . . . ? Na11 P1 O1 Na11 143.5(4) 2_755 . . . ? O7 P1 O1 Na11 110.67(13) . . . 2_755 ? C1 P1 O1 Na11 -139.20(14) . . . 2_755 ? Se1 P1 O1 Na11 -10.68(15) . . . 2_755 ? Na1 P1 O1 Na11 98.16(13) . . . 2_755 ? O7 P1 O1 Na1 12.51(12) . . . . ? C1 P1 O1 Na1 122.64(13) . . . . ? Se1 P1 O1 Na1 -108.84(8) . . . . ? Na11 P1 O1 Na1 -98.16(13) 2_755 . . . ? O20 Na11 O1 P1 -49.7(3) . . . . ? O1 Na11 O1 P1 -157.5(3) 2_755 . . . ? O17 Na11 O1 P1 64.1(3) . . . . ? O11 Na11 O1 P1 118.6(3) . . . . ? P11 Na11 O1 P1 92.8(3) . . . . ? P1 Na11 O1 P1 -155.5(3) 2_755 . . . ? Na11 Na11 O1 P1 -146.4(4) 2_755 . . . ? Se1 Na11 O1 P1 -137.5(3) 2_755 . . . ? Na1 Na11 O1 P1 157.5(3) 2_755 . . . ? Na1 Na11 O1 P1 118.3(3) . . . . ? O20 Na11 O1 Na11 96.73(9) . . . 2_755 ? O1 Na11 O1 Na11 -11.10(12) 2_755 . . 2_755 ? O17 Na11 O1 Na11 -149.45(7) . . . 2_755 ? O11 Na11 O1 Na11 -95.00(9) . . . 2_755 ? P11 Na11 O1 Na11 -120.82(6) . . . 2_755 ? P1 Na11 O1 Na11 -9.06(11) 2_755 . . 2_755 ? Se1 Na11 O1 Na11 8.94(19) 2_755 . . 2_755 ? Na1 Na11 O1 Na11 -56.12(7) 2_755 . . 2_755 ? Na1 Na11 O1 Na11 -95.25(9) . . . 2_755 ? O20 Na11 O1 Na1 -168.02(9) . . . . ? O1 Na11 O1 Na1 84.15(8) 2_755 . . . ? O17 Na11 O1 Na1 -54.20(10) . . . . ? O11 Na11 O1 Na1 0.25(8) . . . . ? P11 Na11 O1 Na1 -25.57(7) . . . . ? P1 Na11 O1 Na1 86.19(8) 2_755 . . . ? Na11 Na11 O1 Na1 95.25(9) 2_755 . . . ? Se1 Na11 O1 Na1 104.20(14) 2_755 . . . ? Na1 Na11 O1 Na1 39.13(7) 2_755 . . . ? O11 Na1 O1 P1 113.44(11) 2_755 . . . ? O11 Na1 O1 P1 -156.63(11) . . . . ? O10 Na1 O1 P1 62.7(3) . . . . ? O7 Na1 O1 P1 -9.72(10) . . . . ? P11 Na1 O1 P1 -132.13(10) . . . . ? Na1 Na1 O1 P1 158.99(10) 2_755 . . . ? Se11 Na1 O1 P1 -98.84(10) . . . . ? Na11 Na1 O1 P1 112.50(13) 2_755 . . . ? Na11 Na1 O1 P1 -156.36(15) . . . . ? O11 Na1 O1 Na11 -90.19(9) 2_755 . . . ? O11 Na1 O1 Na11 -0.26(9) . . . . ? O10 Na1 O1 Na11 -141.0(3) . . . . ? O7 Na1 O1 Na11 146.64(11) . . . . ? P1 Na1 O1 Na11 156.36(15) . . . . ? P11 Na1 O1 Na11 24.24(7) . . . . ? Na1 Na1 O1 Na11 -44.65(8) 2_755 . . . ? Se11 Na1 O1 Na11 57.52(8) . . . . ? Na11 Na1 O1 Na11 -91.13(9) 2_755 . . . ? O11 Na1 O1 Na11 0.94(8) 2_755 . . 2_755 ? O11 Na1 O1 Na11 90.87(8) . . . 2_755 ? O10 Na1 O1 Na11 -49.8(3) . . . 2_755 ? O7 Na1 O1 Na11 -122.22(10) . . . 2_755 ? P1 Na1 O1 Na11 -112.50(13) . . . 2_755 ? P11 Na1 O1 Na11 115.37(7) . . . 2_755 ? Na1 Na1 O1 Na11 46.49(8) 2_755 . . 2_755 ? Se11 Na1 O1 Na11 148.66(6) . . . 2_755 ? Na11 Na1 O1 Na11 91.13(9) . . . 2_755 ? O1 P1 C1 C2 -43.4(3) . . . . ? O7 P1 C1 C2 65.3(3) . . . . ? Se1 P1 C1 C2 -173.8(2) . . . . ? Na1 P1 C1 C2 18.0(3) . . . . ? Na11 P1 C1 C2 -84.6(3) 2_755 . . . ? O1 P1 C1 C6 139.5(3) . . . . ? O7 P1 C1 C6 -111.7(3) . . . . ? Se1 P1 C1 C6 9.2(3) . . . . ? Na1 P1 C1 C6 -159.0(2) . . . . ? Na11 P1 C1 C6 98.4(3) 2_755 . . . ? C6 C1 C2 C3 0.0(6) . . . . ? P1 C1 C2 C3 -177.1(3) . . . . ? C1 C2 C3 C4 0.7(7) . . . . ? C2 C3 C4 C5 -1.0(7) . . . . ? C3 C4 C5 C6 0.6(6) . . . . ? C4 C5 C6 C1 0.2(6) . . . . ? C2 C1 C6 C5 -0.4(5) . . . . ? P1 C1 C6 C5 176.6(3) . . . . ? O1 P1 O7 C7 180.0(3) . . . . ? C1 P1 O7 C7 64.9(3) . . . . ? Se1 P1 O7 C7 -56.2(3) . . . . ? Na1 P1 O7 C7 -166.2(3) . . . . ? Na11 P1 O7 C7 -136.6(2) 2_755 . . . ? O1 P1 O7 Na1 -13.82(14) . . . . ? C1 P1 O7 Na1 -128.91(13) . . . . ? Se1 P1 O7 Na1 110.02(8) . . . . ? Na11 P1 O7 Na1 29.65(12) 2_755 . . . ? O11 Na1 O7 C7 110.4(3) 2_755 . . . ? O11 Na1 O7 C7 -143.7(3) . . . . ? O10 Na1 O7 C7 12.1(3) . . . . ? O1 Na1 O7 C7 173.6(3) . . . . ? P1 Na1 O7 C7 164.5(4) . . . . ? P11 Na1 O7 C7 -117.3(3) . . . . ? Na1 Na1 O7 C7 153.2(3) 2_755 . . . ? Se11 Na1 O7 C7 -82.7(3) . . . . ? Na11 Na1 O7 C7 140.6(3) 2_755 . . . ? Na11 Na1 O7 C7 -166.3(3) . . . . ? O11 Na1 O7 P1 -54.10(13) 2_755 . . . ? O11 Na1 O7 P1 51.80(16) . . . . ? O10 Na1 O7 P1 -152.34(11) . . . . ? O1 Na1 O7 P1 9.17(9) . . . . ? P11 Na1 O7 P1 78.28(12) . . . . ? Na1 Na1 O7 P1 -11.2(2) 2_755 . . . ? Se11 Na1 O7 P1 112.80(10) . . . . ? Na11 Na1 O7 P1 -23.89(10) 2_755 . . . ? Na11 Na1 O7 P1 29.28(11) . . . . ? P1 O7 C7 C8 144.1(3) . . . . ? Na1 O7 C7 C8 -17.4(4) . . . . ? P1 O7 C7 C9 -95.0(4) . . . . ? Na1 O7 C7 C9 103.5(4) . . . . ? O11 Na1 Se11 P11 33.99(13) 2_755 . . . ? O11 Na1 Se11 P11 5.67(7) . . . . ? O10 Na1 Se11 P11 121.26(7) . . . . ? O7 Na1 Se11 P11 -122.83(7) . . . . ? O1 Na1 Se11 P11 -64.21(6) . . . . ? P1 Na1 Se11 P11 -93.71(4) . . . . ? Na1 Na1 Se11 P11 28.76(3) 2_755 . . . ? Na11 Na1 Se11 P11 -34.96(6) 2_755 . . . ? Na11 Na1 Se11 P11 -32.15(3) . . . . ? Na1 Se11 P11 O11 -8.79(10) . . . . ? Na1 Se11 P11 O17 107.18(9) . . . . ? Na1 Se11 P11 C11 -136.67(13) . . . . ? Na1 Se11 P11 Na11 50.53(5) . . . . ? O1 Na11 P11 O11 65.31(12) . . . . ? O20 Na11 P11 O11 154.17(18) . . . . ? O1 Na11 P11 O11 -25.26(12) 2_755 . . . ? O17 Na11 P11 O11 -174.94(16) . . . . ? P1 Na11 P11 O11 -52.15(11) 2_755 . . . ? Na11 Na11 P11 O11 22.49(11) 2_755 . . . ? Se1 Na11 P11 O11 -91.17(11) 2_755 . . . ? Na1 Na11 P11 O11 -16.78(11) 2_755 . . . ? Na1 Na11 P11 O11 43.93(11) . . . . ? O1 Na11 P11 O17 -119.75(13) . . . . ? O20 Na11 P11 O17 -30.89(16) . . . . ? O1 Na11 P11 O17 149.68(13) 2_755 . . . ? O11 Na11 P11 O17 174.94(16) . . . . ? P1 Na11 P11 O17 122.79(12) 2_755 . . . ? Na11 Na11 P11 O17 -162.57(13) 2_755 . . . ? Se1 Na11 P11 O17 83.77(11) 2_755 . . . ? Na1 Na11 P11 O17 158.16(12) 2_755 . . . ? Na1 Na11 P11 O17 -141.13(12) . . . . ? O1 Na11 P11 C11 157.22(14) . . . . ? O20 Na11 P11 C11 -113.92(18) . . . . ? O1 Na11 P11 C11 66.66(15) 2_755 . . . ? O17 Na11 P11 C11 -83.02(17) . . . . ? O11 Na11 P11 C11 91.92(17) . . . . ? P1 Na11 P11 C11 39.76(13) 2_755 . . . ? Na11 Na11 P11 C11 114.40(14) 2_755 . . . ? Se1 Na11 P11 C11 0.74(13) 2_755 . . . ? Na1 Na11 P11 C11 75.13(13) 2_755 . . . ? Na1 Na11 P11 C11 135.84(13) . . . . ? O1 Na11 P11 Se11 -30.44(8) . . . . ? O20 Na11 P11 Se11 58.42(14) . . . . ? O1 Na11 P11 Se11 -121.00(7) 2_755 . . . ? O17 Na11 P11 Se11 89.32(12) . . . . ? O11 Na11 P11 Se11 -95.74(12) . . . . ? P1 Na11 P11 Se11 -147.90(4) 2_755 . . . ? Na11 Na11 P11 Se11 -73.25(7) 2_755 . . . ? Se1 Na11 P11 Se11 173.09(4) 2_755 . . . ? Na1 Na11 P11 Se11 -112.53(5) 2_755 . . . ? Na1 Na11 P11 Se11 -51.82(5) . . . . ? O1 Na11 P11 Na1 21.38(7) . . . . ? O20 Na11 P11 Na1 110.24(13) . . . . ? O1 Na11 P11 Na1 -69.19(7) 2_755 . . . ? O17 Na11 P11 Na1 141.13(12) . . . . ? O11 Na11 P11 Na1 -43.93(11) . . . . ? P1 Na11 P11 Na1 -96.08(4) 2_755 . . . ? Na11 Na11 P11 Na1 -21.44(6) 2_755 . . . ? Se1 Na11 P11 Na1 -135.10(4) 2_755 . . . ? Na1 Na11 P11 Na1 -60.71(4) 2_755 . . . ? O11 Na1 P11 O11 7.21(9) 2_755 . . . ? O10 Na1 P11 O11 103.25(15) . . . . ? O7 Na1 P11 O11 -124.44(15) . . . . ? O1 Na1 P11 O11 -72.09(14) . . . . ? P1 Na1 P11 O11 -93.60(13) . . . . ? Na1 Na1 P11 O11 18.52(13) 2_755 . . . ? Se11 Na1 P11 O11 168.21(14) . . . . ? Na11 Na1 P11 O11 -35.52(13) 2_755 . . . ? Na11 Na1 P11 O11 -53.32(13) . . . . ? O11 Na1 P11 O17 92.22(12) 2_755 . . . ? O11 Na1 P11 O17 85.02(16) . . . . ? O10 Na1 P11 O17 -171.74(11) . . . . ? O7 Na1 P11 O17 -39.42(12) . . . . ? O1 Na1 P11 O17 12.92(11) . . . . ? P1 Na1 P11 O17 -8.58(10) . . . . ? Na1 Na1 P11 O17 103.54(9) 2_755 . . . ? Se11 Na1 P11 O17 -106.78(10) . . . . ? Na11 Na1 P11 O17 49.50(10) 2_755 . . . ? Na11 Na1 P11 O17 31.69(9) . . . . ? O11 Na1 P11 C11 -53.7(2) 2_755 . . . ? O11 Na1 P11 C11 -61.0(2) . . . . ? O10 Na1 P11 C11 42.3(2) . . . . ? O7 Na1 P11 C11 174.61(18) . . . . ? O1 Na1 P11 C11 -133.05(18) . . . . ? P1 Na1 P11 C11 -154.55(18) . . . . ? Na1 Na1 P11 C11 -42.43(18) 2_755 . . . ? Se11 Na1 P11 C11 107.25(18) . . . . ? Na11 Na1 P11 C11 -96.47(18) 2_755 . . . ? Na11 Na1 P11 C11 -114.28(18) . . . . ? O11 Na1 P11 Se11 -161.00(8) 2_755 . . . ? O11 Na1 P11 Se11 -168.21(14) . . . . ? O10 Na1 P11 Se11 -64.96(7) . . . . ? O7 Na1 P11 Se11 67.35(7) . . . . ? O1 Na1 P11 Se11 119.70(6) . . . . ? P1 Na1 P11 Se11 98.20(4) . . . . ? Na1 Na1 P11 Se11 -149.68(3) 2_755 . . . ? Na11 Na1 P11 Se11 156.27(4) 2_755 . . . ? Na11 Na1 P11 Se11 138.47(4) . . . . ? O11 Na1 P11 Na11 60.53(8) 2_755 . . . ? O11 Na1 P11 Na11 53.32(13) . . . . ? O10 Na1 P11 Na11 156.57(8) . . . . ? O7 Na1 P11 Na11 -71.12(8) . . . . ? O1 Na1 P11 Na11 -18.77(6) . . . . ? P1 Na1 P11 Na11 -40.27(4) . . . . ? Na1 Na1 P11 Na11 71.85(3) 2_755 . . . ? Se11 Na1 P11 Na11 -138.47(4) . . . . ? Na11 Na1 P11 Na11 17.81(4) 2_755 . . . ? O17 P11 O11 Na1 124.2(3) . . . 2_755 ? C11 P11 O11 Na1 14.7(3) . . . 2_755 ? Se11 P11 O11 Na1 -115.0(2) . . . 2_755 ? Na11 P11 O11 Na1 128.2(3) . . . 2_755 ? Na1 P11 O11 Na1 -127.5(3) . . . 2_755 ? O17 P11 O11 Na1 -108.25(13) . . . . ? C11 P11 O11 Na1 142.22(14) . . . . ? Se11 P11 O11 Na1 12.56(14) . . . . ? Na11 P11 O11 Na1 -104.22(13) . . . . ? O17 P11 O11 Na11 -4.04(13) . . . . ? C11 P11 O11 Na11 -113.57(14) . . . . ? Se11 P11 O11 Na11 116.77(8) . . . . ? Na1 P11 O11 Na11 104.22(13) . . . . ? O11 Na1 O11 P11 -173.40(8) 2_755 . . . ? O10 Na1 O11 P11 -86.72(14) . . . . ? O7 Na1 O11 P11 69.63(16) . . . . ? O1 Na1 O11 P11 105.22(13) . . . . ? P1 Na1 O11 P11 93.92(12) . . . . ? Na1 Na1 O11 P11 -155.30(17) 2_755 . . . ? Se11 Na1 O11 P11 -8.06(9) . . . . ? Na11 Na1 O11 P11 145.38(12) 2_755 . . . ? Na11 Na1 O11 P11 104.97(15) . . . . ? O11 Na1 O11 Na1 -18.10(12) 2_755 . . 2_755 ? O10 Na1 O11 Na1 68.58(11) . . . 2_755 ? O7 Na1 O11 Na1 -135.08(9) . . . 2_755 ? O1 Na1 O11 Na1 -99.48(8) . . . 2_755 ? P1 Na1 O11 Na1 -110.79(7) . . . 2_755 ? P11 Na1 O11 Na1 155.30(17) . . . 2_755 ? Se11 Na1 O11 Na1 147.24(8) . . . 2_755 ? Na11 Na1 O11 Na1 -59.33(7) 2_755 . . 2_755 ? Na11 Na1 O11 Na1 -99.73(9) . . . 2_755 ? O11 Na1 O11 Na11 81.63(8) 2_755 . . . ? O10 Na1 O11 Na11 168.32(9) . . . . ? O7 Na1 O11 Na11 -35.34(13) . . . . ? O1 Na1 O11 Na11 0.25(8) . . . . ? P1 Na1 O11 Na11 -11.05(9) . . . . ? P11 Na1 O11 Na11 -104.97(15) . . . . ? Na1 Na1 O11 Na11 99.73(9) 2_755 . . . ? Se11 Na1 O11 Na11 -113.03(8) . . . . ? Na11 Na1 O11 Na11 40.41(7) 2_755 . . . ? O1 Na11 O11 P11 -114.85(11) . . . . ? O20 Na11 O11 P11 -69.2(4) . . . . ? O1 Na11 O11 P11 156.18(11) 2_755 . . . ? O17 Na11 O11 P11 3.03(10) . . . . ? P1 Na11 O11 P11 130.92(10) 2_755 . . . ? Na11 Na11 O11 P11 -159.92(10) 2_755 . . . ? Se1 Na11 O11 P11 95.27(10) 2_755 . . . ? Na1 Na11 O11 P11 155.17(16) 2_755 . . . ? Na1 Na11 O11 P11 -114.57(13) . . . . ? O1 Na11 O11 Na1 89.97(9) . . . 2_755 ? O20 Na11 O11 Na1 135.6(3) . . . 2_755 ? O1 Na11 O11 Na1 1.00(9) 2_755 . . 2_755 ? O17 Na11 O11 Na1 -152.14(11) . . . 2_755 ? P11 Na11 O11 Na1 -155.17(16) . . . 2_755 ? P1 Na11 O11 Na1 -24.25(8) 2_755 . . 2_755 ? Na11 Na11 O11 Na1 44.91(8) 2_755 . . 2_755 ? Se1 Na11 O11 Na1 -59.90(8) 2_755 . . 2_755 ? Na1 Na11 O11 Na1 90.25(9) . . . 2_755 ? O1 Na11 O11 Na1 -0.28(9) . . . . ? O20 Na11 O11 Na1 45.4(4) . . . . ? O1 Na11 O11 Na1 -89.25(9) 2_755 . . . ? O17 Na11 O11 Na1 117.61(10) . . . . ? P11 Na11 O11 Na1 114.57(13) . . . . ? P1 Na11 O11 Na1 -114.50(7) 2_755 . . . ? Na11 Na11 O11 Na1 -45.34(8) 2_755 . . . ? Se1 Na11 O11 Na1 -150.15(6) 2_755 . . . ? Na1 Na11 O11 Na1 -90.25(9) 2_755 . . . ? O11 P11 C11 C12 -130.8(3) . . . . ? O17 P11 C11 C12 120.4(3) . . . . ? Se11 P11 C11 C12 -0.1(3) . . . . ? Na11 P11 C11 C12 173.2(3) . . . . ? Na1 P11 C11 C12 -92.0(3) . . . . ? O11 P11 C11 C16 49.5(3) . . . . ? O17 P11 C11 C16 -59.2(3) . . . . ? Se11 P11 C11 C16 -179.7(2) . . . . ? Na11 P11 C11 C16 -6.5(3) . . . . ? Na1 P11 C11 C16 88.4(3) . . . . ? C16 C11 C12 C13 -1.5(6) . . . . ? P11 C11 C12 C13 178.8(3) . . . . ? C11 C12 C13 C14 1.1(6) . . . . ? C12 C13 C14 C15 0.0(6) . . . . ? C13 C14 C15 C16 -0.7(6) . . . . ? C14 C15 C16 C11 0.3(6) . . . . ? C12 C11 C16 C15 0.8(6) . . . . ? P11 C11 C16 C15 -179.5(3) . . . . ? O11 P11 O17 C17 -174.6(2) . . . . ? C11 P11 O17 C17 -60.4(3) . . . . ? Se11 P11 O17 C17 61.6(2) . . . . ? Na11 P11 O17 C17 -178.7(3) . . . . ? Na1 P11 O17 C17 141.9(2) . . . . ? O11 P11 O17 Na11 4.04(13) . . . . ? C11 P11 O17 Na11 118.21(13) . . . . ? Se11 P11 O17 Na11 -119.74(7) . . . . ? Na1 P11 O17 Na11 -39.48(11) . . . . ? O1 Na11 O17 C17 -114.8(3) . . . . ? O20 Na11 O17 C17 -21.8(3) . . . . ? O1 Na11 O17 C17 135.8(3) 2_755 . . . ? O11 Na11 O17 C17 175.3(3) . . . . ? P11 Na11 O17 C17 178.1(4) . . . . ? P1 Na11 O17 C17 108.2(3) 2_755 . . . ? Na11 Na11 O17 C17 -153.8(3) 2_755 . . . ? Se1 Na11 O17 C17 76.1(3) 2_755 . . . ? Na1 Na11 O17 C17 158.3(3) 2_755 . . . ? Na1 Na11 O17 C17 -150.0(3) . . . . ? O1 Na11 O17 P11 67.10(13) . . . . ? O20 Na11 O17 P11 160.02(11) . . . . ? O1 Na11 O17 P11 -42.39(18) 2_755 . . . ? O11 Na11 O17 P11 -2.80(9) . . . . ? P1 Na11 O17 P11 -69.99(12) 2_755 . . . ? Na11 Na11 O17 P11 28.0(2) 2_755 . . . ? Se1 Na11 O17 P11 -102.06(10) 2_755 . . . ? Na1 Na11 O17 P11 -19.86(10) 2_755 . . . ? Na1 Na11 O17 P11 31.89(9) . . . . ? P11 O17 C17 C18 -112.0(3) . . . . ? Na11 O17 C17 C18 70.1(4) . . . . ? P11 O17 C17 C19 126.3(3) . . . . ? Na11 O17 C17 C19 -51.5(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10A O20 0.9800(10) 1.853(7) 2.828(4) 173(5) 2_745 O20 H20A O10 0.9800(11) 1.98(3) 2.898(4) 155(5) 1_565 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 70.01 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.661 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.109