# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_exp_1084 _database_code_depnum_ccdc_archive 'CCDC 903850' #TrackingRef 'exp_1084.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H58 Ba N2 O2 P2 Se2' _chemical_formula_sum 'C58 H58 Ba N2 O2 P2 Se2' _chemical_formula_weight 1172.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -1.0456 8.4617 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M ' P 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.7828(7) _cell_length_b 11.0357(3) _cell_length_c 16.9825(7) _cell_angle_alpha 90 _cell_angle_beta 117.366(5) _cell_angle_gamma 90 _cell_volume 2626.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5949 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 70.78 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 8.372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.21313 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _exptl_special_details ; Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10905 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 70.78 _reflns_number_total 7106 _reflns_number_gt 6586 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP III & Olex 2.1' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0871P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.114(5) _refine_ls_number_reflns 7106 _refine_ls_number_parameters 604 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba1 Ba 0.24709(4) 0.62686(5) 0.25380(3) 0.02545(13) Uani 1 1 d . . . Se1 Se 0.21367(6) 0.40527(7) 0.10708(5) 0.0273(2) Uani 1 1 d . . . Se2 Se 0.28996(6) 0.83203(7) 0.41159(6) 0.0269(2) Uani 1 1 d . . . P1 P 0.29902(14) 0.52791(18) 0.07469(12) 0.0211(4) Uani 1 1 d . . . P2 P 0.18350(15) 0.72567(18) 0.42588(13) 0.0209(4) Uani 1 1 d . . . O1 O 0.1045(5) 0.7769(6) 0.1456(4) 0.0386(16) Uani 1 1 d . . . C27 C 0.1198(6) 0.4002(8) 0.3439(5) 0.0263(17) Uani 1 1 d . . . C2 C 0.3784(5) 0.8507(7) 0.1632(5) 0.0218(16) Uani 1 1 d . . . C32 C 0.1081(6) 0.3628(8) 0.2607(6) 0.0298(19) Uani 1 1 d . . . H7 H 0.0760 0.4123 0.2115 0.036 Uiso 1 1 calc R . . C20 C 0.2254(6) 0.5769(8) -0.0406(5) 0.0292(18) Uani 1 1 d . . . C3 C 0.3979(7) 0.8813(8) 0.2487(6) 0.0315(19) Uani 1 1 d . . . H11 H 0.4277 0.8251 0.2940 0.038 Uiso 1 1 calc R . . C51 C 0.0510(7) 0.7674(9) 0.0514(6) 0.036(2) Uani 1 1 d . . . H15A H -0.0143 0.7432 0.0340 0.043 Uiso 1 1 calc R . . H15B H 0.0798 0.7090 0.0281 0.043 Uiso 1 1 calc R . . C1 C 0.4018(6) 0.7265(8) 0.1415(5) 0.0235(16) Uani 1 1 d . . . H16 H 0.3946 0.7288 0.0811 0.028 Uiso 1 1 calc R . . C8 C 0.5068(6) 0.6950(8) 0.2053(6) 0.0286(18) Uani 1 1 d . . . C29 C 0.2062(7) 0.2151(8) 0.4052(7) 0.039(2) Uani 1 1 d . . . H21 H 0.2405 0.1663 0.4545 0.047 Uiso 1 1 calc R . . C9 C 0.5805(7) 0.7486(9) 0.1953(6) 0.039(2) Uani 1 1 d . . . H22 H 0.5660 0.8011 0.1480 0.046 Uiso 1 1 calc R . . C52 C 0.0549(7) 0.8955(10) 0.0183(6) 0.039(2) Uani 1 1 d . . . H24A H 0.1135 0.9087 0.0143 0.047 Uiso 1 1 calc R . . H24B H 0.0009 0.9108 -0.0390 0.047 Uiso 1 1 calc R . . C31 C 0.1444(7) 0.2512(8) 0.2516(7) 0.037(2) Uani 1 1 d . . . H25 H 0.1360 0.2266 0.1961 0.045 Uiso 1 1 calc R . . C13 C 0.5312(6) 0.6161(10) 0.2768(6) 0.039(2) Uani 1 1 d . . . H28 H 0.4830 0.5784 0.2848 0.047 Uiso 1 1 calc R . . C25 C 0.1917(6) 0.6936(9) -0.0566(6) 0.0324(19) Uani 1 1 d . . . H29 H 0.2121 0.7496 -0.0106 0.039 Uiso 1 1 calc R . . C39 C 0.0902(6) 0.8251(8) 0.4239(5) 0.0250(17) Uani 1 1 d . . . C10 C 0.6739(7) 0.7267(10) 0.2530(7) 0.045(2) Uani 1 1 d . . . H34 H 0.7218 0.7646 0.2445 0.055 Uiso 1 1 calc R . . C30 C 0.1921(7) 0.1775(9) 0.3235(7) 0.040(2) Uani 1 1 d . . . H36 H 0.2147 0.1025 0.3168 0.048 Uiso 1 1 calc R . . C53 C 0.0508(8) 0.9734(10) 0.0899(6) 0.047(3) Uani 1 1 d . . . H37A H 0.0908 1.0445 0.1009 0.057 Uiso 1 1 calc R . . H37B H -0.0141 0.9996 0.0723 0.057 Uiso 1 1 calc R . . C42 C -0.0506(7) 0.9750(9) 0.4291(5) 0.037(2) Uani 1 1 d . . . H38 H -0.0977 1.0247 0.4302 0.044 Uiso 1 1 calc R . . C44 C 0.0050(6) 0.7774(8) 0.4175(6) 0.0302(18) Uani 1 1 d . . . H40 H -0.0048 0.6941 0.4116 0.036 Uiso 1 1 calc R . . C28 C 0.1701(7) 0.3249(9) 0.4156(6) 0.033(2) Uani 1 1 d . . . H43 H 0.1798 0.3484 0.4717 0.040 Uiso 1 1 calc R . . C54 C 0.0866(10) 0.8955(12) 0.1712(7) 0.066(4) Uani 1 1 d . . . H45A H 0.1448 0.9290 0.2180 0.080 Uiso 1 1 calc R . . H45B H 0.0392 0.8903 0.1925 0.080 Uiso 1 1 calc R . . C21 C 0.1964(6) 0.4918(8) -0.1093(5) 0.0335(19) Uani 1 1 d . . . H46 H 0.2198 0.4130 -0.0982 0.040 Uiso 1 1 calc R . . C43 C -0.0648(6) 0.8504(9) 0.4197(5) 0.034(2) Uani 1 1 d . . . H49 H -0.1209 0.8165 0.4148 0.041 Uiso 1 1 calc R . . C40 C 0.1015(7) 0.9491(8) 0.4335(6) 0.0344(19) Uani 1 1 d . . . H51 H 0.1573 0.9836 0.4380 0.041 Uiso 1 1 calc R . . C24 C 0.1261(6) 0.7276(10) -0.1428(6) 0.039(2) Uani 1 1 d . . . H52 H 0.1021 0.8062 -0.1542 0.047 Uiso 1 1 calc R . . C22 C 0.1318(7) 0.5276(10) -0.1946(6) 0.043(2) Uani 1 1 d . . . H54 H 0.1116 0.4724 -0.2411 0.052 Uiso 1 1 calc R . . C41 C 0.0322(7) 1.0246(9) 0.4369(6) 0.041(2) Uani 1 1 d . . . H56 H 0.0423 1.1078 0.4443 0.049 Uiso 1 1 calc R . . C11 C 0.6980(7) 0.6495(11) 0.3233(7) 0.051(3) Uani 1 1 d . . . H58 H 0.7617 0.6349 0.3623 0.061 Uiso 1 1 calc R . . C12 C 0.6254(8) 0.5927(11) 0.3359(7) 0.050(3) Uani 1 1 d . . . H71 H 0.6405 0.5401 0.3833 0.060 Uiso 1 1 calc R . . C23 C 0.0974(7) 0.6451(11) -0.2103(6) 0.047(3) Uani 1 1 d . . . H76 H 0.0543 0.6683 -0.2676 0.056 Uiso 1 1 calc R . . N1 N 0.3327(5) 0.6398(7) 0.1431(4) 0.0240(14) Uani 1 1 d . . . O2 O 0.3948(5) 0.4851(6) 0.3677(4) 0.0386(16) Uani 1 1 d . . . C58 C 0.4538(6) 0.4936(9) 0.4606(6) 0.037(2) Uani 1 1 d . . . H2A H 0.4294 0.5537 0.4867 0.044 Uiso 1 1 calc R . . H2B H 0.5186 0.5149 0.4739 0.044 Uiso 1 1 calc R . . N2 N 0.1490(5) 0.6194(7) 0.3540(4) 0.0247(14) Uani 1 1 d . . . C45 C 0.2349(5) 0.6675(7) 0.5392(5) 0.0232(16) Uani 1 1 d . . . C50 C 0.2885(6) 0.5620(8) 0.5592(6) 0.0300(19) Uani 1 1 d . . . H5 H 0.2982 0.5245 0.5150 0.036 Uiso 1 1 calc R . . C46 C 0.2256(6) 0.7241(8) 0.6078(5) 0.0293(18) Uani 1 1 d . . . H4 H 0.1922 0.7967 0.5972 0.035 Uiso 1 1 calc R . . C57 C 0.4500(7) 0.3671(10) 0.4951(6) 0.038(2) Uani 1 1 d . . . H9A H 0.3936 0.3571 0.5035 0.046 Uiso 1 1 calc R . . H9B H 0.5062 0.3510 0.5507 0.046 Uiso 1 1 calc R . . C14 C 0.3992(6) 0.4476(8) 0.0697(5) 0.0267(17) Uani 1 1 d . . . C4 C 0.3740(7) 0.9947(8) 0.2687(6) 0.037(2) Uani 1 1 d . . . H12 H 0.3882 1.0135 0.3268 0.045 Uiso 1 1 calc R . . C7 C 0.3333(6) 0.9381(8) 0.0976(5) 0.0265(17) Uani 1 1 d . . . H13 H 0.3187 0.9198 0.0392 0.032 Uiso 1 1 calc R . . C5 C 0.3288(7) 1.0799(9) 0.2019(6) 0.036(2) Uani 1 1 d . . . H14 H 0.3117 1.1553 0.2146 0.043 Uiso 1 1 calc R . . C15 C 0.4361(7) 0.3438(9) 0.1168(6) 0.038(2) Uani 1 1 d . . . H17 H 0.4077 0.3080 0.1483 0.046 Uiso 1 1 calc R . . C19 C 0.4414(7) 0.5015(9) 0.0225(6) 0.0356(19) Uani 1 1 d . . . H18 H 0.4154 0.5714 -0.0106 0.043 Uiso 1 1 calc R . . C56 C 0.4463(7) 0.2844(9) 0.4211(6) 0.036(2) Uani 1 1 d . . . H1AA H 0.5085 0.2494 0.4369 0.044 Uiso 1 1 calc R . . H1AB H 0.4005 0.2195 0.4088 0.044 Uiso 1 1 calc R . . C26 C 0.0833(6) 0.5243(8) 0.3539(5) 0.0247(17) Uani 1 1 d . . . H1B H 0.0844 0.5261 0.4120 0.030 Uiso 1 1 calc R . . C34 C -0.0443(6) 0.6131(10) 0.2100(5) 0.036(2) Uani 1 1 d . . . H1C H 0.0033 0.6549 0.2036 0.043 Uiso 1 1 calc R . . C33 C -0.0195(6) 0.5404(8) 0.2843(6) 0.0322(19) Uani 1 1 d . . . C38 C -0.0919(7) 0.4787(10) 0.2921(7) 0.042(2) Uani 1 1 d . . . H1E H -0.0778 0.4274 0.3400 0.051 Uiso 1 1 calc R . . C35 C -0.1371(8) 0.6247(14) 0.1459(7) 0.057(3) Uani 1 1 d . . . H1F H -0.1511 0.6742 0.0971 0.068 Uiso 1 1 calc R . . C47 C 0.2654(7) 0.6737(10) 0.6919(6) 0.042(2) Uani 1 1 d . . . H1G H 0.2574 0.7118 0.7369 0.051 Uiso 1 1 calc R . . C18 C 0.5233(7) 0.4493(10) 0.0253(7) 0.046(2) Uani 1 1 d . . . H1H H 0.5528 0.4848 -0.0053 0.056 Uiso 1 1 calc R . . C48 C 0.3161(7) 0.5689(9) 0.7090(6) 0.041(2) Uani 1 1 d . . . H1I H 0.3430 0.5360 0.7658 0.049 Uiso 1 1 calc R . . C6 C 0.3100(6) 1.0507(8) 0.1169(6) 0.034(2) Uani 1 1 d . . . H1J H 0.2812 1.1075 0.0718 0.041 Uiso 1 1 calc R . . C17 C 0.5599(7) 0.3461(12) 0.0731(7) 0.053(3) Uani 1 1 d . . . H1K H 0.6150 0.3122 0.0757 0.063 Uiso 1 1 calc R . . C49 C 0.3278(7) 0.5111(9) 0.6427(6) 0.038(2) Uani 1 1 d . . . H1L H 0.3616 0.4388 0.6541 0.046 Uiso 1 1 calc R . . C16 C 0.5165(8) 0.2923(10) 0.1171(7) 0.052(3) Uani 1 1 d . . . H1M H 0.5409 0.2204 0.1477 0.063 Uiso 1 1 calc R . . C36 C -0.2095(8) 0.5649(11) 0.1525(8) 0.056(3) Uani 1 1 d . . . H1N H -0.2721 0.5714 0.1083 0.068 Uiso 1 1 calc R . . C37 C -0.1868(7) 0.4944(11) 0.2269(8) 0.055(3) Uani 1 1 d . . . H1O H -0.2355 0.4564 0.2339 0.066 Uiso 1 1 calc R . . C55 C 0.4161(11) 0.3677(10) 0.3431(7) 0.065(4) Uani 1 1 d . . . H1PA H 0.4668 0.3751 0.3262 0.078 Uiso 1 1 calc R . . H1PB H 0.3600 0.3355 0.2930 0.078 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 Ba1 0.0344(2) 0.0234(2) 0.0248(2) 0.00136(17) 0.01900(18) 0.00518(16) Se1 0.0368(5) 0.0220(4) 0.0302(4) -0.0016(4) 0.0214(4) -0.0046(3) Se2 0.0322(4) 0.0226(5) 0.0344(4) -0.0040(4) 0.0227(4) -0.0056(3) P1 0.0298(10) 0.0159(9) 0.0230(8) -0.0024(7) 0.0168(8) -0.0012(8) P2 0.0269(9) 0.0161(9) 0.0245(8) -0.0022(8) 0.0160(8) -0.0014(7) O1 0.050(4) 0.037(4) 0.033(3) 0.004(3) 0.022(3) 0.013(3) C27 0.027(4) 0.023(4) 0.035(4) -0.007(4) 0.020(3) -0.011(3) C2 0.027(4) 0.017(4) 0.029(4) 0.002(3) 0.019(3) 0.000(3) C32 0.043(5) 0.021(4) 0.032(4) -0.004(3) 0.022(4) -0.005(3) C20 0.041(5) 0.028(4) 0.029(4) -0.002(3) 0.025(4) -0.007(4) C3 0.048(5) 0.019(4) 0.031(4) 0.000(3) 0.022(4) 0.004(4) C51 0.047(5) 0.025(5) 0.040(5) -0.004(4) 0.024(4) -0.003(4) C1 0.033(4) 0.023(4) 0.021(3) -0.004(3) 0.018(3) 0.001(3) C8 0.031(4) 0.020(4) 0.038(4) -0.008(3) 0.017(4) -0.002(3) C29 0.044(5) 0.019(4) 0.054(5) 0.001(4) 0.023(5) -0.006(4) C9 0.048(5) 0.028(5) 0.046(5) -0.012(4) 0.027(4) 0.001(4) C52 0.038(5) 0.038(5) 0.039(4) 0.009(4) 0.015(4) 0.000(4) C31 0.051(5) 0.022(5) 0.052(5) -0.008(4) 0.035(5) -0.007(4) C13 0.033(4) 0.040(6) 0.041(4) 0.003(5) 0.015(4) 0.003(4) C25 0.048(5) 0.029(4) 0.034(4) -0.001(4) 0.031(4) 0.002(4) C39 0.032(4) 0.026(4) 0.023(3) -0.002(3) 0.018(3) 0.000(3) C10 0.035(5) 0.047(6) 0.063(6) -0.011(5) 0.030(5) -0.004(5) C30 0.052(6) 0.016(4) 0.063(6) -0.003(4) 0.035(5) -0.003(4) C53 0.058(7) 0.034(5) 0.044(5) 0.002(5) 0.018(5) 0.009(5) C42 0.042(5) 0.046(6) 0.028(4) 0.008(4) 0.021(4) 0.020(4) C44 0.034(4) 0.022(4) 0.044(5) -0.010(4) 0.026(4) -0.006(3) C28 0.048(5) 0.027(5) 0.036(4) -0.002(4) 0.029(4) -0.007(4) C54 0.099(10) 0.052(7) 0.041(5) 0.005(5) 0.027(6) 0.036(7) C21 0.050(5) 0.029(4) 0.030(4) -0.003(4) 0.025(4) 0.001(4) C43 0.031(4) 0.043(5) 0.032(4) -0.008(4) 0.017(4) 0.002(4) C40 0.042(5) 0.024(4) 0.044(5) 0.003(4) 0.025(4) 0.002(4) C24 0.036(5) 0.046(6) 0.040(5) 0.012(4) 0.022(4) 0.009(4) C22 0.056(6) 0.048(6) 0.029(4) -0.006(4) 0.022(4) -0.005(5) C41 0.058(6) 0.030(5) 0.045(5) 0.002(4) 0.033(5) 0.011(4) C11 0.030(5) 0.051(7) 0.058(6) -0.019(5) 0.009(5) -0.002(4) C12 0.040(5) 0.056(7) 0.048(5) 0.004(5) 0.015(5) 0.009(5) C23 0.051(6) 0.059(7) 0.029(4) 0.008(5) 0.018(4) -0.003(5) N1 0.037(4) 0.017(3) 0.027(3) -0.004(3) 0.023(3) -0.001(3) O2 0.059(4) 0.024(3) 0.031(3) 0.007(3) 0.019(3) 0.013(3) C58 0.034(5) 0.042(6) 0.036(4) -0.016(4) 0.018(4) -0.007(4) N2 0.033(3) 0.022(3) 0.028(3) -0.008(3) 0.022(3) -0.002(3) C45 0.028(4) 0.019(4) 0.029(4) 0.003(3) 0.019(3) -0.004(3) C50 0.041(5) 0.024(4) 0.032(4) 0.006(4) 0.023(4) 0.007(4) C46 0.034(4) 0.027(4) 0.026(4) -0.002(3) 0.013(3) 0.000(3) C57 0.038(5) 0.050(6) 0.029(4) 0.009(4) 0.017(4) 0.008(4) C14 0.034(4) 0.024(4) 0.030(4) -0.010(3) 0.020(3) -0.003(3) C4 0.063(6) 0.022(4) 0.040(4) -0.008(4) 0.034(5) -0.003(4) C7 0.037(4) 0.018(4) 0.030(4) 0.001(3) 0.020(4) -0.005(3) C5 0.047(5) 0.023(4) 0.052(5) -0.005(4) 0.035(5) -0.004(4) C15 0.046(5) 0.032(5) 0.043(5) 0.004(4) 0.027(4) 0.006(4) C19 0.048(5) 0.032(5) 0.041(4) -0.004(4) 0.032(4) -0.003(4) C56 0.040(5) 0.028(5) 0.041(5) 0.002(4) 0.020(4) 0.001(4) C26 0.031(4) 0.022(4) 0.031(4) -0.003(3) 0.024(3) -0.004(3) C34 0.035(4) 0.040(6) 0.034(4) -0.007(4) 0.018(4) -0.004(4) C33 0.033(4) 0.025(4) 0.040(4) -0.010(4) 0.018(4) -0.002(4) C38 0.047(5) 0.033(5) 0.062(6) -0.016(5) 0.039(5) -0.012(4) C35 0.044(6) 0.074(8) 0.045(5) 0.000(6) 0.013(5) 0.014(6) C47 0.054(6) 0.045(6) 0.032(4) -0.009(4) 0.024(4) -0.010(5) C18 0.045(5) 0.047(6) 0.061(6) -0.020(5) 0.036(5) -0.008(5) C48 0.053(6) 0.036(5) 0.027(4) 0.005(4) 0.013(4) -0.005(4) C6 0.037(5) 0.020(4) 0.043(5) 0.006(4) 0.017(4) 0.001(4) C17 0.034(5) 0.066(8) 0.058(6) -0.012(6) 0.022(5) 0.009(5) C49 0.050(5) 0.026(4) 0.040(5) 0.007(4) 0.023(4) 0.009(4) C16 0.058(6) 0.040(6) 0.056(6) 0.005(5) 0.024(5) 0.019(5) C36 0.039(6) 0.052(7) 0.057(6) -0.013(6) 0.005(5) 0.013(5) C37 0.036(5) 0.047(7) 0.090(8) -0.032(6) 0.035(6) -0.014(5) C55 0.119(11) 0.030(6) 0.036(5) -0.001(4) 0.027(6) 0.032(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ba1 O1 2.716(6) . ? Ba1 O2 2.734(6) . ? Ba1 N1 2.777(6) . ? Ba1 N2 2.778(6) . ? Ba1 Se2 3.3314(10) . ? Ba1 Se1 3.3553(10) . ? Ba1 P1 3.662(2) . ? Ba1 P2 3.665(2) . ? Se1 P1 2.152(2) . ? Se2 P2 2.153(2) . ? P1 N1 1.609(7) . ? P1 C20 1.840(9) . ? P1 C14 1.847(9) . ? P2 N2 1.597(7) . ? P2 C39 1.824(9) . ? P2 C45 1.827(8) . ? O1 C51 1.430(10) . ? O1 C54 1.447(13) . ? C27 C28 1.385(12) . ? C27 C32 1.399(11) . ? C27 C26 1.526(12) . ? C2 C3 1.381(11) . ? C2 C7 1.397(11) . ? C2 C1 1.508(11) . ? C32 C31 1.397(12) . ? C32 H7 0.9300 . ? C20 C25 1.372(13) . ? C20 C21 1.400(12) . ? C3 C4 1.394(12) . ? C3 H11 0.9300 . ? C51 C52 1.533(13) . ? C51 H15A 0.9700 . ? C51 H15B 0.9700 . ? C1 N1 1.460(10) . ? C1 C8 1.546(11) . ? C1 H16 0.9800 . ? C8 C9 1.383(13) . ? C8 C13 1.397(13) . ? C29 C30 1.364(14) . ? C29 C28 1.385(13) . ? C29 H21 0.9300 . ? C9 C10 1.366(13) . ? C9 H22 0.9300 . ? C52 C53 1.514(14) . ? C52 H24A 0.9700 . ? C52 H24B 0.9700 . ? C31 C30 1.369(14) . ? C31 H25 0.9300 . ? C13 C12 1.383(13) . ? C13 H28 0.9300 . ? C25 C24 1.401(12) . ? C25 H29 0.9300 . ? C39 C40 1.380(12) . ? C39 C44 1.401(11) . ? C10 C11 1.371(16) . ? C10 H34 0.9300 . ? C30 H36 0.9300 . ? C53 C54 1.500(14) . ? C53 H37A 0.9700 . ? C53 H37B 0.9700 . ? C42 C41 1.366(14) . ? C42 C43 1.391(14) . ? C42 H38 0.9300 . ? C44 C43 1.377(12) . ? C44 H40 0.9300 . ? C28 H43 0.9300 . ? C54 H45A 0.9700 . ? C54 H45B 0.9700 . ? C21 C22 1.391(12) . ? C21 H46 0.9300 . ? C43 H49 0.9300 . ? C40 C41 1.398(12) . ? C40 H51 0.9300 . ? C24 C23 1.368(14) . ? C24 H52 0.9300 . ? C22 C23 1.383(15) . ? C22 H54 0.9300 . ? C41 H56 0.9300 . ? C11 C12 1.406(16) . ? C11 H58 0.9300 . ? C12 H71 0.9300 . ? C23 H76 0.9300 . ? O2 C58 1.419(9) . ? O2 C55 1.448(11) . ? C58 C57 1.525(14) . ? C58 H2A 0.9700 . ? C58 H2B 0.9700 . ? N2 C26 1.475(10) . ? C45 C50 1.387(12) . ? C45 C46 1.388(11) . ? C50 C49 1.379(12) . ? C50 H5 0.9300 . ? C46 C47 1.385(12) . ? C46 H4 0.9300 . ? C57 C56 1.533(13) . ? C57 H9A 0.9700 . ? C57 H9B 0.9700 . ? C14 C15 1.365(12) . ? C14 C19 1.390(12) . ? C4 C5 1.391(13) . ? C4 H12 0.9300 . ? C7 C6 1.378(12) . ? C7 H13 0.9300 . ? C5 C6 1.372(13) . ? C5 H14 0.9300 . ? C15 C16 1.388(13) . ? C15 H17 0.9300 . ? C19 C18 1.396(13) . ? C19 H18 0.9300 . ? C56 C55 1.498(13) . ? C56 H1AA 0.9700 . ? C56 H1AB 0.9700 . ? C26 C33 1.516(11) . ? C26 H1B 0.9800 . ? C34 C35 1.372(13) . ? C34 C33 1.391(13) . ? C34 H1C 0.9300 . ? C33 C38 1.388(13) . ? C38 C37 1.404(14) . ? C38 H1E 0.9300 . ? C35 C36 1.368(18) . ? C35 H1F 0.9300 . ? C47 C48 1.359(15) . ? C47 H1G 0.9300 . ? C18 C17 1.363(16) . ? C18 H1H 0.9300 . ? C48 C49 1.379(14) . ? C48 H1I 0.9300 . ? C6 H1J 0.9300 . ? C17 C16 1.360(16) . ? C17 H1K 0.9300 . ? C49 H1L 0.9300 . ? C16 H1M 0.9300 . ? C36 C37 1.383(17) . ? C36 H1N 0.9300 . ? C37 H1O 0.9300 . ? C55 H1PA 0.9700 . ? C55 H1PB 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ba1 O2 177.3(2) . . ? O1 Ba1 N1 91.2(2) . . ? O2 Ba1 N1 89.2(2) . . ? O1 Ba1 N2 84.9(2) . . ? O2 Ba1 N2 94.8(2) . . ? N1 Ba1 N2 175.8(2) . . ? O1 Ba1 Se2 85.90(14) . . ? O2 Ba1 Se2 91.58(13) . . ? N1 Ba1 Se2 121.82(15) . . ? N2 Ba1 Se2 59.46(15) . . ? O1 Ba1 Se1 98.25(13) . . ? O2 Ba1 Se1 84.29(13) . . ? N1 Ba1 Se1 59.62(15) . . ? N2 Ba1 Se1 119.44(15) . . ? Se2 Ba1 Se1 175.66(3) . . ? O1 Ba1 P1 93.00(14) . . ? O2 Ba1 P1 88.50(14) . . ? N1 Ba1 P1 24.34(15) . . ? N2 Ba1 P1 154.20(15) . . ? Se2 Ba1 P1 146.16(4) . . ? Se1 Ba1 P1 35.37(4) . . ? O1 Ba1 P2 84.97(14) . . ? O2 Ba1 P2 93.59(14) . . ? N1 Ba1 P2 157.07(15) . . ? N2 Ba1 P2 24.03(15) . . ? Se2 Ba1 P2 35.44(3) . . ? Se1 Ba1 P2 143.30(4) . . ? P1 Ba1 P2 177.39(5) . . ? P1 Se1 Ba1 80.11(6) . . ? P2 Se2 Ba1 80.77(6) . . ? N1 P1 C20 112.4(4) . . ? N1 P1 C14 113.3(4) . . ? C20 P1 C14 103.1(4) . . ? N1 P1 Se1 109.6(3) . . ? C20 P1 Se1 107.1(3) . . ? C14 P1 Se1 111.1(3) . . ? N1 P1 Ba1 45.3(3) . . ? C20 P1 Ba1 121.6(3) . . ? C14 P1 Ba1 134.7(3) . . ? Se1 P1 Ba1 64.52(5) . . ? N2 P2 C39 116.0(4) . . ? N2 P2 C45 112.2(4) . . ? C39 P2 C45 101.2(4) . . ? N2 P2 Se2 108.9(3) . . ? C39 P2 Se2 109.6(3) . . ? C45 P2 Se2 108.6(3) . . ? N2 P2 Ba1 45.1(2) . . ? C39 P2 Ba1 132.7(2) . . ? C45 P2 Ba1 125.7(3) . . ? Se2 P2 Ba1 63.79(6) . . ? C51 O1 C54 107.8(7) . . ? C51 O1 Ba1 126.3(5) . . ? C54 O1 Ba1 124.3(6) . . ? C28 C27 C32 117.9(8) . . ? C28 C27 C26 122.2(7) . . ? C32 C27 C26 119.7(8) . . ? C3 C2 C7 117.1(8) . . ? C3 C2 C1 121.2(7) . . ? C7 C2 C1 121.7(7) . . ? C31 C32 C27 120.1(9) . . ? C31 C32 H7 120.0 . . ? C27 C32 H7 120.0 . . ? C25 C20 C21 121.1(8) . . ? C25 C20 P1 118.9(7) . . ? C21 C20 P1 119.6(7) . . ? C2 C3 C4 121.4(8) . . ? C2 C3 H11 119.3 . . ? C4 C3 H11 119.3 . . ? O1 C51 C52 103.9(7) . . ? O1 C51 H15A 111.0 . . ? C52 C51 H15A 111.0 . . ? O1 C51 H15B 111.0 . . ? C52 C51 H15B 111.0 . . ? H15A C51 H15B 109.0 . . ? N1 C1 C2 108.8(6) . . ? N1 C1 C8 114.1(7) . . ? C2 C1 C8 109.7(6) . . ? N1 C1 H16 108.0 . . ? C2 C1 H16 108.0 . . ? C8 C1 H16 108.0 . . ? C9 C8 C13 117.5(8) . . ? C9 C8 C1 120.6(8) . . ? C13 C8 C1 121.8(8) . . ? C30 C29 C28 120.7(9) . . ? C30 C29 H21 119.6 . . ? C28 C29 H21 119.6 . . ? C10 C9 C8 121.9(10) . . ? C10 C9 H22 119.1 . . ? C8 C9 H22 119.1 . . ? C53 C52 C51 101.9(8) . . ? C53 C52 H24A 111.4 . . ? C51 C52 H24A 111.4 . . ? C53 C52 H24B 111.4 . . ? C51 C52 H24B 111.4 . . ? H24A C52 H24B 109.2 . . ? C30 C31 C32 120.6(9) . . ? C30 C31 H25 119.7 . . ? C32 C31 H25 119.7 . . ? C12 C13 C8 121.5(10) . . ? C12 C13 H28 119.3 . . ? C8 C13 H28 119.3 . . ? C20 C25 C24 119.4(9) . . ? C20 C25 H29 120.3 . . ? C24 C25 H29 120.3 . . ? C40 C39 C44 116.6(8) . . ? C40 C39 P2 122.3(7) . . ? C44 C39 P2 120.9(7) . . ? C9 C10 C11 120.7(10) . . ? C9 C10 H34 119.7 . . ? C11 C10 H34 119.7 . . ? C29 C30 C31 119.5(9) . . ? C29 C30 H36 120.2 . . ? C31 C30 H36 120.2 . . ? C54 C53 C52 106.1(9) . . ? C54 C53 H37A 110.5 . . ? C52 C53 H37A 110.5 . . ? C54 C53 H37B 110.5 . . ? C52 C53 H37B 110.5 . . ? H37A C53 H37B 108.7 . . ? C41 C42 C43 120.2(9) . . ? C41 C42 H38 119.9 . . ? C43 C42 H38 119.9 . . ? C43 C44 C39 121.9(8) . . ? C43 C44 H40 119.0 . . ? C39 C44 H40 119.0 . . ? C29 C28 C27 121.1(8) . . ? C29 C28 H43 119.5 . . ? C27 C28 H43 119.5 . . ? O1 C54 C53 106.5(8) . . ? O1 C54 H45A 110.4 . . ? C53 C54 H45A 110.4 . . ? O1 C54 H45B 110.4 . . ? C53 C54 H45B 110.4 . . ? H45A C54 H45B 108.6 . . ? C22 C21 C20 118.6(9) . . ? C22 C21 H46 120.7 . . ? C20 C21 H46 120.7 . . ? C44 C43 C42 119.6(9) . . ? C44 C43 H49 120.2 . . ? C42 C43 H49 120.2 . . ? C39 C40 C41 122.3(9) . . ? C39 C40 H51 118.8 . . ? C41 C40 H51 118.8 . . ? C23 C24 C25 119.9(9) . . ? C23 C24 H52 120.1 . . ? C25 C24 H52 120.1 . . ? C23 C22 C21 120.2(9) . . ? C23 C22 H54 119.9 . . ? C21 C22 H54 119.9 . . ? C42 C41 C40 119.3(9) . . ? C42 C41 H56 120.4 . . ? C40 C41 H56 120.4 . . ? C10 C11 C12 119.4(10) . . ? C10 C11 H58 120.3 . . ? C12 C11 H58 120.3 . . ? C13 C12 C11 119.0(11) . . ? C13 C12 H71 120.5 . . ? C11 C12 H71 120.5 . . ? C24 C23 C22 120.8(9) . . ? C24 C23 H76 119.6 . . ? C22 C23 H76 119.6 . . ? C1 N1 P1 119.4(5) . . ? C1 N1 Ba1 130.2(5) . . ? P1 N1 Ba1 110.3(3) . . ? C58 O2 C55 105.0(7) . . ? C58 O2 Ba1 131.3(6) . . ? C55 O2 Ba1 122.9(6) . . ? O2 C58 C57 104.2(7) . . ? O2 C58 H2A 110.9 . . ? C57 C58 H2A 110.9 . . ? O2 C58 H2B 110.9 . . ? C57 C58 H2B 110.9 . . ? H2A C58 H2B 108.9 . . ? C26 N2 P2 121.0(5) . . ? C26 N2 Ba1 127.6(5) . . ? P2 N2 Ba1 110.9(3) . . ? C50 C45 C46 117.4(7) . . ? C50 C45 P2 118.6(6) . . ? C46 C45 P2 124.0(6) . . ? C49 C50 C45 122.0(8) . . ? C49 C50 H5 119.0 . . ? C45 C50 H5 119.0 . . ? C47 C46 C45 120.8(8) . . ? C47 C46 H4 119.6 . . ? C45 C46 H4 119.6 . . ? C58 C57 C56 102.9(7) . . ? C58 C57 H9A 111.2 . . ? C56 C57 H9A 111.2 . . ? C58 C57 H9B 111.2 . . ? C56 C57 H9B 111.2 . . ? H9A C57 H9B 109.1 . . ? C15 C14 C19 120.6(9) . . ? C15 C14 P1 121.3(7) . . ? C19 C14 P1 117.9(7) . . ? C5 C4 C3 120.2(8) . . ? C5 C4 H12 119.9 . . ? C3 C4 H12 119.9 . . ? C6 C7 C2 121.8(8) . . ? C6 C7 H13 119.1 . . ? C2 C7 H13 119.1 . . ? C6 C5 C4 118.7(9) . . ? C6 C5 H14 120.6 . . ? C4 C5 H14 120.6 . . ? C14 C15 C16 119.3(10) . . ? C14 C15 H17 120.4 . . ? C16 C15 H17 120.4 . . ? C14 C19 C18 119.0(9) . . ? C14 C19 H18 120.5 . . ? C18 C19 H18 120.5 . . ? C55 C56 C57 103.6(8) . . ? C55 C56 H1AA 111.0 . . ? C57 C56 H1AA 111.0 . . ? C55 C56 H1AB 111.0 . . ? C57 C56 H1AB 111.0 . . ? H1AA C56 H1AB 109.0 . . ? N2 C26 C33 114.7(7) . . ? N2 C26 C27 109.7(6) . . ? C33 C26 C27 110.0(7) . . ? N2 C26 H1B 107.4 . . ? C33 C26 H1B 107.4 . . ? C27 C26 H1B 107.4 . . ? C35 C34 C33 121.8(10) . . ? C35 C34 H1C 119.1 . . ? C33 C34 H1C 119.1 . . ? C38 C33 C34 117.9(9) . . ? C38 C33 C26 120.1(9) . . ? C34 C33 C26 121.9(8) . . ? C33 C38 C37 119.4(11) . . ? C33 C38 H1E 120.3 . . ? C37 C38 H1E 120.3 . . ? C36 C35 C34 121.1(12) . . ? C36 C35 H1F 119.4 . . ? C34 C35 H1F 119.4 . . ? C48 C47 C46 120.4(9) . . ? C48 C47 H1G 119.8 . . ? C46 C47 H1G 119.8 . . ? C17 C18 C19 119.9(10) . . ? C17 C18 H1H 120.1 . . ? C19 C18 H1H 120.1 . . ? C47 C48 C49 120.3(9) . . ? C47 C48 H1I 119.8 . . ? C49 C48 H1I 119.8 . . ? C5 C6 C7 120.7(8) . . ? C5 C6 H1J 119.7 . . ? C7 C6 H1J 119.7 . . ? C16 C17 C18 120.6(10) . . ? C16 C17 H1K 119.7 . . ? C18 C17 H1K 119.7 . . ? C48 C49 C50 119.1(9) . . ? C48 C49 H1L 120.5 . . ? C50 C49 H1L 120.5 . . ? C17 C16 C15 120.6(10) . . ? C17 C16 H1M 119.7 . . ? C15 C16 H1M 119.7 . . ? C35 C36 C37 118.1(10) . . ? C35 C36 H1N 121.0 . . ? C37 C36 H1N 121.0 . . ? C36 C37 C38 121.6(11) . . ? C36 C37 H1O 119.2 . . ? C38 C37 H1O 119.2 . . ? O2 C55 C56 108.4(8) . . ? O2 C55 H1PA 110.0 . . ? C56 C55 H1PA 110.0 . . ? O2 C55 H1PB 110.0 . . ? C56 C55 H1PB 110.0 . . ? H1PA C55 H1PB 108.4 . . ? 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 O1 Ba1 Se1 P1 83.52(17) . . . . ? O2 Ba1 Se1 P1 -95.47(16) . . . . ? N1 Ba1 Se1 P1 -3.01(17) . . . . ? N2 Ba1 Se1 P1 172.26(18) . . . . ? Se2 Ba1 Se1 P1 -113.6(4) . . . . ? P2 Ba1 Se1 P1 176.17(8) . . . . ? O1 Ba1 Se2 P2 87.09(17) . . . . ? O2 Ba1 Se2 P2 -93.97(17) . . . . ? N1 Ba1 Se2 P2 175.95(17) . . . . ? N2 Ba1 Se2 P2 0.63(18) . . . . ? Se1 Ba1 Se2 P2 -75.9(4) . . . . ? P1 Ba1 Se2 P2 176.36(9) . . . . ? Ba1 Se1 P1 N1 4.8(3) . . . . ? Ba1 Se1 P1 C20 -117.4(3) . . . . ? Ba1 Se1 P1 C14 130.7(3) . . . . ? O1 Ba1 P1 N1 86.3(4) . . . . ? O2 Ba1 P1 N1 -91.4(4) . . . . ? N2 Ba1 P1 N1 170.7(5) . . . . ? Se2 Ba1 P1 N1 -0.8(4) . . . . ? Se1 Ba1 P1 N1 -173.7(4) . . . . ? P2 Ba1 P1 N1 125.3(12) . . . . ? O1 Ba1 P1 C20 -4.9(4) . . . . ? O2 Ba1 P1 C20 177.3(4) . . . . ? N1 Ba1 P1 C20 -91.2(5) . . . . ? N2 Ba1 P1 C20 79.5(5) . . . . ? Se2 Ba1 P1 C20 -92.0(3) . . . . ? Se1 Ba1 P1 C20 95.1(3) . . . . ? P2 Ba1 P1 C20 34.1(13) . . . . ? O1 Ba1 P1 C14 164.9(4) . . . . ? O2 Ba1 P1 C14 -12.8(4) . . . . ? N1 Ba1 P1 C14 78.6(5) . . . . ? N2 Ba1 P1 C14 -110.7(5) . . . . ? Se2 Ba1 P1 C14 77.8(4) . . . . ? Se1 Ba1 P1 C14 -95.1(4) . . . . ? P2 Ba1 P1 C14 -156.1(11) . . . . ? O1 Ba1 P1 Se1 -100.04(16) . . . . ? O2 Ba1 P1 Se1 82.24(16) . . . . ? N1 Ba1 P1 Se1 173.7(4) . . . . ? N2 Ba1 P1 Se1 -15.6(4) . . . . ? Se2 Ba1 P1 Se1 172.85(5) . . . . ? P2 Ba1 P1 Se1 -61.0(12) . . . . ? Ba1 Se2 P2 N2 -1.0(3) . . . . ? Ba1 Se2 P2 C39 -128.9(3) . . . . ? Ba1 Se2 P2 C45 121.4(3) . . . . ? O1 Ba1 P2 N2 88.7(4) . . . . ? O2 Ba1 P2 N2 -93.7(4) . . . . ? N1 Ba1 P2 N2 169.8(5) . . . . ? Se2 Ba1 P2 N2 178.7(4) . . . . ? Se1 Ba1 P2 N2 -8.4(4) . . . . ? P1 Ba1 P2 N2 49.5(12) . . . . ? O1 Ba1 P2 C39 3.1(4) . . . . ? O2 Ba1 P2 C39 -179.2(4) . . . . ? N1 Ba1 P2 C39 84.2(5) . . . . ? N2 Ba1 P2 C39 -85.6(5) . . . . ? Se2 Ba1 P2 C39 93.1(4) . . . . ? Se1 Ba1 P2 C39 -94.0(4) . . . . ? P1 Ba1 P2 C39 -36.0(13) . . . . ? O1 Ba1 P2 C45 175.2(3) . . . . ? O2 Ba1 P2 C45 -7.1(3) . . . . ? N1 Ba1 P2 C45 -103.7(5) . . . . ? N2 Ba1 P2 C45 86.5(5) . . . . ? Se2 Ba1 P2 C45 -94.8(3) . . . . ? Se1 Ba1 P2 C45 78.1(3) . . . . ? P1 Ba1 P2 C45 136.1(11) . . . . ? O1 Ba1 P2 Se2 -89.99(16) . . . . ? O2 Ba1 P2 Se2 87.68(16) . . . . ? N1 Ba1 P2 Se2 -8.9(4) . . . . ? N2 Ba1 P2 Se2 -178.7(4) . . . . ? Se1 Ba1 P2 Se2 172.95(5) . . . . ? P1 Ba1 P2 Se2 -129.1(11) . . . . ? O2 Ba1 O1 C51 146(4) . . . . ? N1 Ba1 O1 C51 47.4(7) . . . . ? N2 Ba1 O1 C51 -131.1(7) . . . . ? Se2 Ba1 O1 C51 169.2(7) . . . . ? Se1 Ba1 O1 C51 -12.1(7) . . . . ? P1 Ba1 O1 C51 23.1(7) . . . . ? P2 Ba1 O1 C51 -155.3(7) . . . . ? O2 Ba1 O1 C54 -17(5) . . . . ? N1 Ba1 O1 C54 -116.5(9) . . . . ? N2 Ba1 O1 C54 65.0(9) . . . . ? Se2 Ba1 O1 C54 5.4(9) . . . . ? Se1 Ba1 O1 C54 -175.9(9) . . . . ? P1 Ba1 O1 C54 -140.8(9) . . . . ? P2 Ba1 O1 C54 40.9(9) . . . . ? C28 C27 C32 C31 1.6(13) . . . . ? C26 C27 C32 C31 177.6(8) . . . . ? N1 P1 C20 C25 -11.9(9) . . . . ? C14 P1 C20 C25 -134.2(8) . . . . ? Se1 P1 C20 C25 108.6(7) . . . . ? Ba1 P1 C20 C25 38.4(8) . . . . ? N1 P1 C20 C21 175.1(7) . . . . ? C14 P1 C20 C21 52.8(8) . . . . ? Se1 P1 C20 C21 -64.5(8) . . . . ? Ba1 P1 C20 C21 -134.6(7) . . . . ? C7 C2 C3 C4 -0.2(14) . . . . ? C1 C2 C3 C4 -178.1(8) . . . . ? C54 O1 C51 C52 35.6(11) . . . . ? Ba1 O1 C51 C52 -130.4(7) . . . . ? C3 C2 C1 N1 74.3(10) . . . . ? C7 C2 C1 N1 -103.5(8) . . . . ? C3 C2 C1 C8 -51.2(10) . . . . ? C7 C2 C1 C8 131.0(8) . . . . ? N1 C1 C8 C9 163.1(8) . . . . ? C2 C1 C8 C9 -74.5(10) . . . . ? N1 C1 C8 C13 -19.6(11) . . . . ? C2 C1 C8 C13 102.8(9) . . . . ? C13 C8 C9 C10 -0.5(14) . . . . ? C1 C8 C9 C10 177.0(8) . . . . ? O1 C51 C52 C53 -36.0(10) . . . . ? C27 C32 C31 C30 -0.3(14) . . . . ? C9 C8 C13 C12 0.4(15) . . . . ? C1 C8 C13 C12 -177.0(9) . . . . ? C21 C20 C25 C24 0.8(14) . . . . ? P1 C20 C25 C24 -172.1(7) . . . . ? N2 P2 C39 C40 -138.0(7) . . . . ? C45 P2 C39 C40 100.3(8) . . . . ? Se2 P2 C39 C40 -14.2(8) . . . . ? Ba1 P2 C39 C40 -86.2(8) . . . . ? N2 P2 C39 C44 45.8(8) . . . . ? C45 P2 C39 C44 -75.9(7) . . . . ? Se2 P2 C39 C44 169.5(6) . . . . ? Ba1 P2 C39 C44 97.6(7) . . . . ? C8 C9 C10 C11 0.3(15) . . . . ? C28 C29 C30 C31 2.1(15) . . . . ? C32 C31 C30 C29 -1.6(15) . . . . ? C51 C52 C53 C54 23.6(12) . . . . ? C40 C39 C44 C43 0.7(13) . . . . ? P2 C39 C44 C43 177.2(7) . . . . ? C30 C29 C28 C27 -0.8(14) . . . . ? C32 C27 C28 C29 -1.1(13) . . . . ? C26 C27 C28 C29 -177.0(8) . . . . ? C51 O1 C54 C53 -20.5(13) . . . . ? Ba1 O1 C54 C53 145.9(7) . . . . ? C52 C53 C54 O1 -3.3(14) . . . . ? C25 C20 C21 C22 -0.4(14) . . . . ? P1 C20 C21 C22 172.5(7) . . . . ? C39 C44 C43 C42 -0.5(14) . . . . ? C41 C42 C43 C44 -0.5(14) . . . . ? C44 C39 C40 C41 0.0(13) . . . . ? P2 C39 C40 C41 -176.4(7) . . . . ? C20 C25 C24 C23 -0.9(14) . . . . ? C20 C21 C22 C23 0.0(15) . . . . ? C43 C42 C41 C40 1.2(14) . . . . ? C39 C40 C41 C42 -0.9(14) . . . . ? C9 C10 C11 C12 -0.1(16) . . . . ? C8 C13 C12 C11 -0.2(17) . . . . ? C10 C11 C12 C13 0.0(17) . . . . ? C25 C24 C23 C22 0.5(16) . . . . ? C21 C22 C23 C24 -0.1(16) . . . . ? C2 C1 N1 P1 145.3(5) . . . . ? C8 C1 N1 P1 -91.8(7) . . . . ? C2 C1 N1 Ba1 -37.0(9) . . . . ? C8 C1 N1 Ba1 85.8(8) . . . . ? C20 P1 N1 C1 -69.0(7) . . . . ? C14 P1 N1 C1 47.4(7) . . . . ? Se1 P1 N1 C1 172.0(5) . . . . ? Ba1 P1 N1 C1 178.1(8) . . . . ? C20 P1 N1 Ba1 112.9(4) . . . . ? C14 P1 N1 Ba1 -130.7(4) . . . . ? Se1 P1 N1 Ba1 -6.0(3) . . . . ? O1 Ba1 N1 C1 87.6(6) . . . . ? O2 Ba1 N1 C1 -89.7(6) . . . . ? N2 Ba1 N1 C1 108(3) . . . . ? Se2 Ba1 N1 C1 1.7(7) . . . . ? Se1 Ba1 N1 C1 -173.6(7) . . . . ? P1 Ba1 N1 C1 -177.8(9) . . . . ? P2 Ba1 N1 C1 7.7(9) . . . . ? O1 Ba1 N1 P1 -94.6(3) . . . . ? O2 Ba1 N1 P1 88.1(3) . . . . ? N2 Ba1 N1 P1 -74(4) . . . . ? Se2 Ba1 N1 P1 179.4(2) . . . . ? Se1 Ba1 N1 P1 4.2(2) . . . . ? P2 Ba1 N1 P1 -174.52(13) . . . . ? O1 Ba1 O2 C58 31(5) . . . . ? N1 Ba1 O2 C58 130.0(8) . . . . ? N2 Ba1 O2 C58 -51.3(8) . . . . ? Se2 Ba1 O2 C58 8.1(8) . . . . ? Se1 Ba1 O2 C58 -170.5(8) . . . . ? P1 Ba1 O2 C58 154.3(8) . . . . ? P2 Ba1 O2 C58 -27.3(8) . . . . ? O1 Ba1 O2 C55 -161(4) . . . . ? N1 Ba1 O2 C55 -62.2(9) . . . . ? N2 Ba1 O2 C55 116.5(9) . . . . ? Se2 Ba1 O2 C55 176.0(9) . . . . ? Se1 Ba1 O2 C55 -2.7(9) . . . . ? P1 Ba1 O2 C55 -37.9(9) . . . . ? P2 Ba1 O2 C55 140.6(9) . . . . ? C55 O2 C58 C57 -40.1(11) . . . . ? Ba1 O2 C58 C57 129.3(7) . . . . ? C39 P2 N2 C26 -62.1(7) . . . . ? C45 P2 N2 C26 53.5(7) . . . . ? Se2 P2 N2 C26 173.7(5) . . . . ? Ba1 P2 N2 C26 172.4(8) . . . . ? C39 P2 N2 Ba1 125.4(4) . . . . ? C45 P2 N2 Ba1 -118.9(4) . . . . ? Se2 P2 N2 Ba1 1.3(4) . . . . ? O1 Ba1 N2 C26 99.0(6) . . . . ? O2 Ba1 N2 C26 -83.7(6) . . . . ? N1 Ba1 N2 C26 78(4) . . . . ? Se2 Ba1 N2 C26 -172.7(7) . . . . ? Se1 Ba1 N2 C26 2.4(7) . . . . ? P1 Ba1 N2 C26 12.7(9) . . . . ? P2 Ba1 N2 C26 -171.8(9) . . . . ? O1 Ba1 N2 P2 -89.2(4) . . . . ? O2 Ba1 N2 P2 88.1(4) . . . . ? N1 Ba1 N2 P2 -110(3) . . . . ? Se2 Ba1 N2 P2 -0.9(3) . . . . ? Se1 Ba1 N2 P2 174.3(3) . . . . ? P1 Ba1 N2 P2 -175.43(12) . . . . ? N2 P2 C45 C50 36.4(8) . . . . ? C39 P2 C45 C50 160.7(7) . . . . ? Se2 P2 C45 C50 -84.0(6) . . . . ? Ba1 P2 C45 C50 -13.4(8) . . . . ? N2 P2 C45 C46 -145.2(7) . . . . ? C39 P2 C45 C46 -20.9(8) . . . . ? Se2 P2 C45 C46 94.4(7) . . . . ? Ba1 P2 C45 C46 165.0(6) . . . . ? C46 C45 C50 C49 3.0(13) . . . . ? P2 C45 C50 C49 -178.5(7) . . . . ? C50 C45 C46 C47 -2.5(12) . . . . ? P2 C45 C46 C47 179.1(7) . . . . ? O2 C58 C57 C56 36.2(9) . . . . ? N1 P1 C14 C15 97.7(8) . . . . ? C20 P1 C14 C15 -140.6(7) . . . . ? Se1 P1 C14 C15 -26.2(8) . . . . ? Ba1 P1 C14 C15 48.3(9) . . . . ? N1 P1 C14 C19 -76.9(7) . . . . ? C20 P1 C14 C19 44.8(7) . . . . ? Se1 P1 C14 C19 159.2(6) . . . . ? Ba1 P1 C14 C19 -126.3(6) . . . . ? C2 C3 C4 C5 0.4(15) . . . . ? C3 C2 C7 C6 0.6(13) . . . . ? C1 C2 C7 C6 178.5(8) . . . . ? C3 C4 C5 C6 -1.1(15) . . . . ? C19 C14 C15 C16 0.0(13) . . . . ? P1 C14 C15 C16 -174.5(7) . . . . ? C15 C14 C19 C18 -1.3(13) . . . . ? P1 C14 C19 C18 173.4(7) . . . . ? C58 C57 C56 C55 -18.1(11) . . . . ? P2 N2 C26 C33 101.9(8) . . . . ? Ba1 N2 C26 C33 -87.0(8) . . . . ? P2 N2 C26 C27 -133.7(6) . . . . ? Ba1 N2 C26 C27 37.4(9) . . . . ? C28 C27 C26 N2 99.2(9) . . . . ? C32 C27 C26 N2 -76.6(9) . . . . ? C28 C27 C26 C33 -133.7(9) . . . . ? C32 C27 C26 C33 50.5(10) . . . . ? C35 C34 C33 C38 0.2(15) . . . . ? C35 C34 C33 C26 178.1(10) . . . . ? N2 C26 C33 C38 -162.3(8) . . . . ? C27 C26 C33 C38 73.4(10) . . . . ? N2 C26 C33 C34 19.8(12) . . . . ? C27 C26 C33 C34 -104.4(10) . . . . ? C34 C33 C38 C37 -1.8(14) . . . . ? C26 C33 C38 C37 -179.8(9) . . . . ? C33 C34 C35 C36 0.0(18) . . . . ? C45 C46 C47 C48 1.3(14) . . . . ? C14 C19 C18 C17 0.8(14) . . . . ? C46 C47 C48 C49 -0.5(16) . . . . ? C4 C5 C6 C7 1.5(14) . . . . ? C2 C7 C6 C5 -1.3(14) . . . . ? C19 C18 C17 C16 1.0(16) . . . . ? C47 C48 C49 C50 0.9(16) . . . . ? C45 C50 C49 C48 -2.2(15) . . . . ? C18 C17 C16 C15 -2.3(17) . . . . ? C14 C15 C16 C17 1.8(16) . . . . ? C34 C35 C36 C37 1.5(19) . . . . ? C35 C36 C37 C38 -3.3(17) . . . . ? C33 C38 C37 C36 3.5(16) . . . . ? C58 O2 C55 C56 28.7(13) . . . . ? Ba1 O2 C55 C56 -141.8(7) . . . . ? C57 C56 C55 O2 -5.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 70.78 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.801 _refine_diff_density_min -1.495 _refine_diff_density_rms 0.156 data_exp_1344 _database_code_depnum_ccdc_archive 'CCDC 903851' #TrackingRef 'exp_1344.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H22 N P Se, C4 H8 O' _chemical_formula_sum 'C29 H30 N O P Se' _chemical_formula_weight 518.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.7943 1.1372 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4326(8) _cell_length_b 14.8835(14) _cell_length_c 20.239(2) _cell_angle_alpha 90 _cell_angle_beta 116.921(7) _cell_angle_gamma 90 _cell_volume 2533.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2976 _cell_measurement_theta_min 3.85 _cell_measurement_theta_max 70.86 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 2.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63153 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _exptl_special_details ; Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10946 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 70.86 _reflns_number_total 4807 _reflns_number_gt 3737 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP III & Olex 2.1' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0792P)^2^+2.8004P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4807 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1675 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.30399(6) -0.30894(4) 0.13122(3) 0.04060(18) Uani 1 1 d . . . P1 P 0.33291(12) -0.23180(8) 0.05077(6) 0.0315(3) Uani 1 1 d . . . O1 O 0.2134(4) -0.1464(2) -0.15415(19) 0.0511(9) Uani 1 1 d . . . N1 N 0.2172(4) -0.2632(3) -0.0348(2) 0.0363(8) Uani 1 1 d . . . H1 H 0.1993 -0.2252 -0.0697 0.044 Uiso 1 1 calc R . . C1 C 0.1427(5) -0.3515(3) -0.0553(2) 0.0332(9) Uani 1 1 d . . . H1A H 0.1722 -0.3864 -0.0099 0.040 Uiso 1 1 calc R . . C2 C -0.0403(5) -0.3446(3) -0.0964(2) 0.0329(9) Uani 1 1 d . . . C3 C -0.1302(5) -0.4198(3) -0.0964(2) 0.0385(10) Uani 1 1 d . . . H3 H -0.0790 -0.4712 -0.0705 0.046 Uiso 1 1 calc R . . C4 C -0.2949(5) -0.4178(4) -0.1346(3) 0.0474(12) Uani 1 1 d . . . H4 H -0.3538 -0.4675 -0.1339 0.057 Uiso 1 1 calc R . . C5 C -0.3709(6) -0.3418(4) -0.1734(3) 0.0512(13) Uani 1 1 d . . . H5 H -0.4812 -0.3407 -0.1995 0.061 Uiso 1 1 calc R . . C6 C -0.2840(5) -0.2674(4) -0.1738(3) 0.0476(12) Uani 1 1 d . . . H6 H -0.3358 -0.2163 -0.2001 0.057 Uiso 1 1 calc R . . C7 C -0.1189(5) -0.2687(3) -0.1348(3) 0.0418(11) Uani 1 1 d . . . H7 H -0.0610 -0.2180 -0.1346 0.050 Uiso 1 1 calc R . . C8 C 0.2000(5) -0.4027(3) -0.1049(2) 0.0348(9) Uani 1 1 d . . . C9 C 0.2763(6) -0.4840(3) -0.0831(3) 0.0461(11) Uani 1 1 d . . . H9 H 0.2942 -0.5086 -0.0378 0.055 Uiso 1 1 calc R . . C10 C 0.3269(6) -0.5300(4) -0.1288(3) 0.0554(14) Uani 1 1 d . . . H10 H 0.3789 -0.5848 -0.1135 0.066 Uiso 1 1 calc R . . C11 C 0.3007(6) -0.4952(4) -0.1955(3) 0.0486(12) Uani 1 1 d . . . H11 H 0.3341 -0.5264 -0.2258 0.058 Uiso 1 1 calc R . . C12 C 0.2243(5) -0.4134(4) -0.2182(3) 0.0462(12) Uani 1 1 d . . . H12 H 0.2061 -0.3895 -0.2638 0.055 Uiso 1 1 calc R . . C13 C 0.1750(5) -0.3671(3) -0.1729(3) 0.0416(11) Uani 1 1 d . . . H13 H 0.1247 -0.3118 -0.1880 0.050 Uiso 1 1 calc R . . C14 C 0.2915(5) -0.1137(3) 0.0521(2) 0.0313(9) Uani 1 1 d . . . C15 C 0.2128(6) -0.0823(3) 0.0914(3) 0.0477(12) Uani 1 1 d . . . H15 H 0.1864 -0.1221 0.1195 0.057 Uiso 1 1 calc R . . C16 C 0.1734(6) 0.0078(4) 0.0890(3) 0.0540(14) Uani 1 1 d . . . H16 H 0.1215 0.0279 0.1159 0.065 Uiso 1 1 calc R . . C17 C 0.2105(6) 0.0686(3) 0.0470(3) 0.0474(12) Uani 1 1 d . . . H17 H 0.1842 0.1290 0.0457 0.057 Uiso 1 1 calc R . . C18 C 0.2875(5) 0.0376(3) 0.0072(3) 0.0413(10) Uani 1 1 d . . . H18 H 0.3118 0.0774 -0.0216 0.050 Uiso 1 1 calc R . . C19 C 0.3285(5) -0.0517(3) 0.0098(3) 0.0393(10) Uani 1 1 d . . . H19 H 0.3812 -0.0712 -0.0168 0.047 Uiso 1 1 calc R . . C20 C 0.5369(5) -0.2350(3) 0.0651(2) 0.0322(9) Uani 1 1 d . . . C21 C 0.6573(5) -0.2037(3) 0.1329(3) 0.0406(11) Uani 1 1 d . . . H21 H 0.6315 -0.1781 0.1679 0.049 Uiso 1 1 calc R . . C22 C 0.8147(5) -0.2115(4) 0.1469(3) 0.0515(13) Uani 1 1 d . . . H22 H 0.8947 -0.1904 0.1915 0.062 Uiso 1 1 calc R . . C23 C 0.8540(6) -0.2500(4) 0.0955(3) 0.0488(13) Uani 1 1 d . . . H23 H 0.9603 -0.2554 0.1058 0.059 Uiso 1 1 calc R . . C24 C 0.7364(5) -0.2808(3) 0.0287(3) 0.0432(11) Uani 1 1 d . . . H24 H 0.7632 -0.3067 -0.0060 0.052 Uiso 1 1 calc R . . C25 C 0.5775(5) -0.2727(3) 0.0135(3) 0.0372(10) Uani 1 1 d . . . H25 H 0.4981 -0.2927 -0.0316 0.045 Uiso 1 1 calc R . . C26 C 0.1025(7) -0.0779(4) -0.1962(3) 0.0593(15) Uani 1 1 d . . . H26A H 0.0945 -0.0328 -0.1635 0.071 Uiso 1 1 calc R . . H26B H -0.0020 -0.1037 -0.2255 0.071 Uiso 1 1 calc R . . C27 C 0.1653(6) -0.0364(4) -0.2462(3) 0.0579(14) Uani 1 1 d . . . H27A H 0.1432 0.0275 -0.2526 0.070 Uiso 1 1 calc R . . H27B H 0.1197 -0.0652 -0.2945 0.070 Uiso 1 1 calc R . . C28 C 0.3433(6) -0.0544(4) -0.2039(3) 0.0514(13) Uani 1 1 d . . . H28A H 0.3927 -0.0558 -0.2368 0.062 Uiso 1 1 calc R . . H28B H 0.3962 -0.0097 -0.1656 0.062 Uiso 1 1 calc R . . C29 C 0.3456(6) -0.1457(4) -0.1711(3) 0.0482(12) Uani 1 1 d . . . H29A H 0.3342 -0.1927 -0.2064 0.058 Uiso 1 1 calc R . . H29B H 0.4446 -0.1549 -0.1266 0.058 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 Se1 0.0395(3) 0.0437(3) 0.0431(3) 0.0056(2) 0.0227(2) -0.0005(2) P1 0.0275(5) 0.0326(6) 0.0358(6) -0.0006(5) 0.0156(4) -0.0007(4) O1 0.062(2) 0.048(2) 0.055(2) 0.0125(17) 0.0374(18) 0.0107(18) N1 0.0327(18) 0.037(2) 0.0344(19) 0.0046(16) 0.0111(15) -0.0010(16) C1 0.0244(19) 0.033(2) 0.044(2) 0.0081(19) 0.0172(18) 0.0027(17) C2 0.026(2) 0.036(2) 0.038(2) -0.0064(19) 0.0151(17) -0.0001(18) C3 0.036(2) 0.040(2) 0.043(2) -0.006(2) 0.021(2) -0.006(2) C4 0.041(3) 0.047(3) 0.062(3) -0.013(2) 0.030(2) -0.010(2) C5 0.029(2) 0.065(3) 0.062(3) -0.021(3) 0.022(2) -0.008(2) C6 0.035(2) 0.053(3) 0.051(3) 0.001(2) 0.016(2) 0.015(2) C7 0.031(2) 0.041(3) 0.056(3) -0.005(2) 0.022(2) 0.000(2) C8 0.0264(19) 0.036(2) 0.043(2) -0.0065(19) 0.0158(18) -0.0029(18) C9 0.046(3) 0.039(3) 0.060(3) 0.005(2) 0.029(2) 0.007(2) C10 0.054(3) 0.035(3) 0.086(4) 0.001(3) 0.040(3) 0.012(2) C11 0.041(3) 0.046(3) 0.070(3) -0.013(3) 0.035(3) -0.003(2) C12 0.038(2) 0.059(3) 0.043(3) -0.008(2) 0.019(2) -0.003(2) C13 0.032(2) 0.046(3) 0.044(3) -0.003(2) 0.0150(19) 0.004(2) C14 0.0278(19) 0.032(2) 0.034(2) 0.0001(18) 0.0140(17) 0.0006(17) C15 0.059(3) 0.041(3) 0.061(3) 0.003(2) 0.043(3) 0.005(2) C16 0.067(3) 0.042(3) 0.075(4) 0.000(3) 0.051(3) 0.012(3) C17 0.049(3) 0.035(3) 0.063(3) 0.004(2) 0.029(2) 0.010(2) C18 0.043(2) 0.037(2) 0.049(3) 0.003(2) 0.025(2) 0.002(2) C19 0.039(2) 0.038(2) 0.048(3) 0.000(2) 0.026(2) 0.001(2) C20 0.029(2) 0.033(2) 0.038(2) 0.0013(18) 0.0171(18) 0.0012(17) C21 0.030(2) 0.048(3) 0.040(2) -0.004(2) 0.0140(19) -0.002(2) C22 0.028(2) 0.062(3) 0.052(3) 0.002(3) 0.007(2) -0.002(2) C23 0.031(2) 0.046(3) 0.075(4) 0.006(3) 0.030(2) 0.003(2) C24 0.041(2) 0.038(2) 0.063(3) 0.005(2) 0.034(2) 0.005(2) C25 0.035(2) 0.034(2) 0.046(3) 0.001(2) 0.021(2) -0.0023(19) C26 0.059(3) 0.062(4) 0.067(4) 0.022(3) 0.037(3) 0.023(3) C27 0.061(3) 0.060(3) 0.062(3) 0.021(3) 0.035(3) 0.023(3) C28 0.054(3) 0.044(3) 0.058(3) 0.009(3) 0.028(3) 0.004(2) C29 0.048(3) 0.048(3) 0.052(3) 0.007(2) 0.026(2) 0.007(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Se1 P1 2.1086(12) . ? P1 N1 1.642(4) . ? P1 C14 1.804(4) . ? P1 C20 1.812(4) . ? O1 C26 1.431(6) . ? O1 C29 1.436(5) . ? N1 C1 1.459(6) . ? N1 H1 0.8600 . ? C1 C2 1.543(5) . ? C1 C8 1.541(6) . ? C1 H1A 0.9800 . ? C2 C7 1.381(6) . ? C2 C3 1.404(6) . ? C3 C4 1.387(6) . ? C3 H3 0.9300 . ? C4 C5 1.378(8) . ? C4 H4 0.9300 . ? C5 C6 1.380(7) . ? C5 H5 0.9300 . ? C6 C7 1.391(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.375(6) . ? C8 C13 1.390(7) . ? C9 C10 1.397(7) . ? C9 H9 0.9300 . ? C10 C11 1.360(8) . ? C10 H10 0.9300 . ? C11 C12 1.383(7) . ? C11 H11 0.9300 . ? C12 C13 1.386(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.391(6) . ? C14 C19 1.406(6) . ? C15 C16 1.387(7) . ? C15 H15 0.9300 . ? C16 C17 1.391(7) . ? C16 H16 0.9300 . ? C17 C18 1.385(6) . ? C17 H17 0.9300 . ? C18 C19 1.379(6) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C25 1.383(6) . ? C20 C21 1.406(6) . ? C21 C22 1.385(6) . ? C21 H21 0.9300 . ? C22 C23 1.378(7) . ? C22 H22 0.9300 . ? C23 C24 1.382(7) . ? C23 H23 0.9300 . ? C24 C25 1.392(6) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.517(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.524(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.508(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 C14 104.35(19) . . ? N1 P1 C20 108.20(19) . . ? C14 P1 C20 104.16(19) . . ? N1 P1 Se1 113.75(14) . . ? C14 P1 Se1 114.48(14) . . ? C20 P1 Se1 111.19(14) . . ? C26 O1 C29 109.4(4) . . ? C1 N1 P1 124.1(3) . . ? C1 N1 H1 117.9 . . ? P1 N1 H1 117.9 . . ? N1 C1 C2 111.7(3) . . ? N1 C1 C8 111.4(3) . . ? C2 C1 C8 108.6(3) . . ? N1 C1 H1A 108.3 . . ? C2 C1 H1A 108.3 . . ? C8 C1 H1A 108.3 . . ? C7 C2 C3 118.8(4) . . ? C7 C2 C1 122.8(4) . . ? C3 C2 C1 118.4(4) . . ? C4 C3 C2 120.5(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.8(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 120.1(5) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C2 C7 C6 120.6(5) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C13 118.9(4) . . ? C9 C8 C1 120.9(4) . . ? C13 C8 C1 120.2(4) . . ? C8 C9 C10 120.3(5) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 120.6(5) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 119.8(5) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 119.9(5) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C8 120.5(5) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? C15 C14 C19 118.1(4) . . ? C15 C14 P1 120.8(3) . . ? C19 C14 P1 121.0(3) . . ? C16 C15 C14 120.7(5) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 120.8(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 118.8(5) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C19 C18 C17 120.7(4) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C14 120.8(4) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? C25 C20 C21 119.5(4) . . ? C25 C20 P1 121.8(3) . . ? C21 C20 P1 118.5(3) . . ? C22 C21 C20 119.3(4) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C21 120.7(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.4(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 119.6(5) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C20 C25 C24 120.5(4) . . ? C20 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? O1 C26 C27 106.6(4) . . ? O1 C26 H26A 110.4 . . ? C27 C26 H26A 110.4 . . ? O1 C26 H26B 110.4 . . ? C27 C26 H26B 110.4 . . ? H26A C26 H26B 108.6 . . ? C26 C27 C28 102.5(4) . . ? C26 C27 H27A 111.3 . . ? C28 C27 H27A 111.3 . . ? C26 C27 H27B 111.3 . . ? C28 C27 H27B 111.3 . . ? H27A C27 H27B 109.2 . . ? C29 C28 C27 101.4(4) . . ? C29 C28 H28A 111.5 . . ? C27 C28 H28A 111.5 . . ? C29 C28 H28B 111.5 . . ? C27 C28 H28B 111.5 . . ? H28A C28 H28B 109.3 . . ? O1 C29 C28 105.7(4) . . ? O1 C29 H29A 110.6 . . ? C28 C29 H29A 110.6 . . ? O1 C29 H29B 110.6 . . ? C28 C29 H29B 110.6 . . ? H29A C29 H29B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 P1 N1 C1 -145.8(3) . . . . ? C20 P1 N1 C1 103.7(3) . . . . ? Se1 P1 N1 C1 -20.4(4) . . . . ? P1 N1 C1 C2 120.4(4) . . . . ? P1 N1 C1 C8 -117.9(4) . . . . ? N1 C1 C2 C7 24.4(6) . . . . ? C8 C1 C2 C7 -98.9(5) . . . . ? N1 C1 C2 C3 -157.4(4) . . . . ? C8 C1 C2 C3 79.3(5) . . . . ? C7 C2 C3 C4 0.4(6) . . . . ? C1 C2 C3 C4 -177.9(4) . . . . ? C2 C3 C4 C5 0.6(7) . . . . ? C3 C4 C5 C6 -0.8(7) . . . . ? C4 C5 C6 C7 0.0(8) . . . . ? C3 C2 C7 C6 -1.2(7) . . . . ? C1 C2 C7 C6 177.0(4) . . . . ? C5 C6 C7 C2 1.0(7) . . . . ? N1 C1 C8 C9 120.0(4) . . . . ? C2 C1 C8 C9 -116.5(4) . . . . ? N1 C1 C8 C13 -60.1(5) . . . . ? C2 C1 C8 C13 63.4(5) . . . . ? C13 C8 C9 C10 -0.2(7) . . . . ? C1 C8 C9 C10 179.6(4) . . . . ? C8 C9 C10 C11 -0.4(8) . . . . ? C9 C10 C11 C12 0.4(8) . . . . ? C10 C11 C12 C13 0.1(7) . . . . ? C11 C12 C13 C8 -0.7(7) . . . . ? C9 C8 C13 C12 0.8(7) . . . . ? C1 C8 C13 C12 -179.1(4) . . . . ? N1 P1 C14 C15 111.1(4) . . . . ? C20 P1 C14 C15 -135.5(4) . . . . ? Se1 P1 C14 C15 -13.9(4) . . . . ? N1 P1 C14 C19 -64.8(4) . . . . ? C20 P1 C14 C19 48.6(4) . . . . ? Se1 P1 C14 C19 170.2(3) . . . . ? C19 C14 C15 C16 -0.5(8) . . . . ? P1 C14 C15 C16 -176.5(4) . . . . ? C14 C15 C16 C17 0.5(9) . . . . ? C15 C16 C17 C18 0.2(8) . . . . ? C16 C17 C18 C19 -0.8(8) . . . . ? C17 C18 C19 C14 0.8(7) . . . . ? C15 C14 C19 C18 -0.1(7) . . . . ? P1 C14 C19 C18 175.8(4) . . . . ? N1 P1 C20 C25 -9.5(4) . . . . ? C14 P1 C20 C25 -120.1(4) . . . . ? Se1 P1 C20 C25 116.1(4) . . . . ? N1 P1 C20 C21 174.9(4) . . . . ? C14 P1 C20 C21 64.3(4) . . . . ? Se1 P1 C20 C21 -59.5(4) . . . . ? C25 C20 C21 C22 -0.2(7) . . . . ? P1 C20 C21 C22 175.5(4) . . . . ? C20 C21 C22 C23 -0.6(8) . . . . ? C21 C22 C23 C24 0.7(8) . . . . ? C22 C23 C24 C25 -0.1(8) . . . . ? C21 C20 C25 C24 0.8(7) . . . . ? P1 C20 C25 C24 -174.7(3) . . . . ? C23 C24 C25 C20 -0.7(7) . . . . ? C29 O1 C26 C27 4.0(6) . . . . ? O1 C26 C27 C28 -25.7(6) . . . . ? C26 C27 C28 C29 36.3(6) . . . . ? C26 O1 C29 C28 19.9(6) . . . . ? C27 C28 C29 O1 -35.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 70.86 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.569 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.090 data_exp_837 _database_code_depnum_ccdc_archive 'CCDC 903852' #TrackingRef 'exp_837.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H58 Ca N2 O2 P2 Se2, 2(C4 H6 O)' _chemical_formula_sum 'C66 H70 Ca N2 O4 P2 Se2' _chemical_formula_weight 1215.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.3641 1.2855 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 10.2981(9) _cell_length_b 10.9898(9) _cell_length_c 14.4141(13) _cell_angle_alpha 99.955(7) _cell_angle_beta 101.789(8) _cell_angle_gamma 103.034(7) _cell_volume 1514.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3757 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 70.99 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 630 _exptl_absorpt_coefficient_mu 3.144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67571 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _exptl_special_details ; Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11585 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 70.99 _reflns_number_total 5710 _reflns_number_gt 4729 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP III & Olex 2.1' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0337P)^2^+10.1904P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5710 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2068 _refine_ls_wR_factor_gt 0.1998 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.186 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.35051(7) 0.39848(7) 0.63964(5) 0.0379(2) Uani 1 1 d . . . Ca1 Ca 0.5000 0.5000 0.5000 0.0355(4) Uani 1 2 d S . . P1 P 0.49668(17) 0.57085(16) 0.72949(11) 0.0317(4) Uani 1 1 d . . . O1 O 0.3192(5) 0.6006(5) 0.4481(4) 0.0449(12) Uani 1 1 d . . . O2 O 0.1660(14) 0.1009(14) 0.9423(10) 0.170(5) Uani 1 1 d . . . N1 N 0.5696(5) 0.6529(5) 0.6609(4) 0.0337(12) Uani 1 1 d . . . C1 C 0.6636(7) 0.7791(6) 0.7093(5) 0.0366(14) Uani 1 1 d . . . H5 H 0.7082 0.7747 0.7751 0.044 Uiso 1 1 calc R . . C2 C 0.7761(7) 0.8074(7) 0.6551(5) 0.0397(15) Uani 1 1 d . . . C3 C 0.9072(9) 0.7948(9) 0.6918(7) 0.065(3) Uani 1 1 d . . . H19 H 0.9273 0.7704 0.7506 0.079 Uiso 1 1 calc R . . C4 C 1.0078(9) 0.8185(10) 0.6417(9) 0.080(3) Uani 1 1 d . . . H29 H 1.0952 0.8102 0.6671 0.096 Uiso 1 1 calc R . . C5 C 0.9796(9) 0.8537(9) 0.5551(8) 0.067(3) Uani 1 1 d . . . H14 H 1.0475 0.8691 0.5215 0.080 Uiso 1 1 calc R . . C6 C 0.8493(9) 0.8667(8) 0.5171(6) 0.054(2) Uani 1 1 d . . . H21 H 0.8294 0.8893 0.4576 0.065 Uiso 1 1 calc R . . C7 C 0.7495(8) 0.8459(7) 0.5682(5) 0.0458(17) Uani 1 1 d . . . H6 H 0.6636 0.8580 0.5439 0.055 Uiso 1 1 calc R . . C8 C 0.5961(7) 0.8887(7) 0.7192(5) 0.0391(15) Uani 1 1 d . . . C9 C 0.4645(8) 0.8772(8) 0.6654(6) 0.0487(18) Uani 1 1 d . . . H17 H 0.4127 0.7988 0.6243 0.058 Uiso 1 1 calc R . . C10 C 0.4086(10) 0.9812(9) 0.6720(7) 0.064(2) Uani 1 1 d . . . H30 H 0.3207 0.9724 0.6343 0.076 Uiso 1 1 calc R . . C11 C 0.4821(10) 1.0964(9) 0.7335(7) 0.063(2) Uani 1 1 d . . . H27 H 0.4441 1.1657 0.7379 0.076 Uiso 1 1 calc R . . C12 C 0.6120(11) 1.1095(8) 0.7887(7) 0.067(3) Uani 1 1 d . . . H26 H 0.6622 1.1875 0.8310 0.081 Uiso 1 1 calc R . . C13 C 0.6684(9) 1.0052(7) 0.7811(6) 0.0524(19) Uani 1 1 d . . . H11 H 0.7565 1.0146 0.8186 0.063 Uiso 1 1 calc R . . C14 C 0.4154(7) 0.6607(7) 0.8087(5) 0.0389(15) Uani 1 1 d . . . C15 C 0.2738(8) 0.6449(8) 0.7859(6) 0.0491(19) Uani 1 1 d . . . H18 H 0.2167 0.5823 0.7323 0.059 Uiso 1 1 calc R . . C16 C 0.2180(11) 0.7231(10) 0.8439(7) 0.068(3) Uani 1 1 d . . . H31 H 0.1233 0.7125 0.8277 0.082 Uiso 1 1 calc R . . C17 C 0.2996(12) 0.8160(9) 0.9249(7) 0.067(3) Uani 1 1 d . . . H28 H 0.2610 0.8680 0.9628 0.081 Uiso 1 1 calc R . . C18 C 0.4399(11) 0.8298(8) 0.9482(7) 0.065(3) Uani 1 1 d . . . H23 H 0.4960 0.8909 1.0030 0.077 Uiso 1 1 calc R . . C19 C 0.4988(9) 0.7543(7) 0.8913(6) 0.0485(18) Uani 1 1 d . . . H12 H 0.5935 0.7657 0.9078 0.058 Uiso 1 1 calc R . . C20 C 0.6223(7) 0.5279(6) 0.8179(4) 0.0341(14) Uani 1 1 d . . . C21 C 0.5881(7) 0.4838(7) 0.8967(5) 0.0385(15) Uani 1 1 d . . . H8 H 0.5018 0.4817 0.9078 0.046 Uiso 1 1 calc R . . C22 C 0.6817(7) 0.4427(7) 0.9591(5) 0.0406(16) Uani 1 1 d . . . H7 H 0.6581 0.4131 1.0117 0.049 Uiso 1 1 calc R . . C23 C 0.8119(7) 0.4459(7) 0.9429(5) 0.0435(17) Uani 1 1 d . . . H3 H 0.8750 0.4188 0.9847 0.052 Uiso 1 1 calc R . . C24 C 0.8459(7) 0.4895(7) 0.8643(5) 0.0422(16) Uani 1 1 d . . . H16 H 0.9323 0.4918 0.8533 0.051 Uiso 1 1 calc R . . C25 C 0.7520(7) 0.5296(6) 0.8020(5) 0.0362(14) Uani 1 1 d . . . H2 H 0.7754 0.5580 0.7489 0.043 Uiso 1 1 calc R . . C26 C 0.219(2) 0.128(2) 0.8629(15) 0.177(9) Uani 1 1 d . . . H1C H 0.3041 0.1209 0.8544 0.213 Uiso 1 1 calc R . . C27 C 0.112(2) 0.170(2) 0.7916(17) 0.169(8) Uani 1 1 d . . . H1DA H 0.1546 0.2302 0.7574 0.203 Uiso 1 1 calc R . . H1DB H 0.0432 0.0984 0.7454 0.203 Uiso 1 1 calc R . . C28 C 0.053(2) 0.2352(17) 0.8699(18) 0.176(10) Uani 1 1 d . . . H1A H 0.0113 0.3011 0.8638 0.212 Uiso 1 1 calc R . . C29 C 0.072(2) 0.177(2) 0.9603(18) 0.221(15) Uani 1 1 d . . . H1BA H 0.1122 0.2440 1.0197 0.265 Uiso 1 1 calc R . . H1BB H -0.0146 0.1246 0.9646 0.265 Uiso 1 1 calc R . . C30 C 0.1818(8) 0.5672(9) 0.4629(6) 0.057(2) Uani 1 1 d . . . H22A H 0.1821 0.6060 0.5287 0.068 Uiso 1 1 calc R . . H22B H 0.1463 0.4748 0.4515 0.068 Uiso 1 1 calc R . . C31 C 0.0959(8) 0.6194(9) 0.3896(6) 0.057(2) Uani 1 1 d . . . H24A H 0.0176 0.6377 0.4112 0.068 Uiso 1 1 calc R . . H24B H 0.0632 0.5600 0.3263 0.068 Uiso 1 1 calc R . . C32 C 0.1975(10) 0.7410(11) 0.3868(9) 0.079(3) Uani 1 1 d . . . H33A H 0.1977 0.8125 0.4370 0.094 Uiso 1 1 calc R . . H33B H 0.1750 0.7621 0.3239 0.094 Uiso 1 1 calc R . . C33 C 0.3359(8) 0.7108(8) 0.4051(6) 0.0477(18) Uani 1 1 d . . . H13A H 0.3622 0.6915 0.3445 0.057 Uiso 1 1 calc R . . H13B H 0.4065 0.7833 0.4491 0.057 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 Se1 0.0353(4) 0.0364(4) 0.0381(4) 0.0099(3) 0.0077(3) 0.0028(3) Ca1 0.0345(10) 0.0430(11) 0.0291(9) 0.0106(8) 0.0076(7) 0.0095(8) P1 0.0324(8) 0.0321(8) 0.0313(8) 0.0101(7) 0.0090(6) 0.0073(7) O1 0.038(3) 0.058(3) 0.045(3) 0.020(2) 0.012(2) 0.018(2) O2 0.162(12) 0.200(14) 0.173(12) 0.041(10) 0.056(10) 0.090(11) N1 0.036(3) 0.036(3) 0.030(3) 0.008(2) 0.005(2) 0.014(2) C1 0.033(3) 0.037(4) 0.040(4) 0.012(3) 0.011(3) 0.006(3) C2 0.039(4) 0.037(4) 0.043(4) 0.010(3) 0.013(3) 0.008(3) C3 0.049(5) 0.078(6) 0.088(7) 0.050(5) 0.026(5) 0.022(4) C4 0.044(5) 0.084(7) 0.140(10) 0.067(7) 0.041(6) 0.024(5) C5 0.051(5) 0.060(5) 0.094(7) 0.017(5) 0.044(5) 0.003(4) C6 0.062(5) 0.053(5) 0.043(4) 0.008(4) 0.024(4) -0.001(4) C7 0.041(4) 0.051(4) 0.041(4) 0.008(3) 0.011(3) 0.003(3) C8 0.042(4) 0.038(4) 0.036(3) 0.011(3) 0.013(3) 0.004(3) C9 0.049(4) 0.044(4) 0.054(5) 0.012(4) 0.014(4) 0.015(3) C10 0.060(5) 0.057(5) 0.087(7) 0.029(5) 0.026(5) 0.026(4) C11 0.076(6) 0.049(5) 0.084(7) 0.028(5) 0.041(5) 0.027(5) C12 0.094(7) 0.038(5) 0.068(6) 0.003(4) 0.034(5) 0.011(5) C13 0.059(5) 0.041(4) 0.052(5) 0.009(3) 0.013(4) 0.005(4) C14 0.048(4) 0.041(4) 0.043(4) 0.023(3) 0.024(3) 0.020(3) C15 0.054(5) 0.063(5) 0.048(4) 0.030(4) 0.022(4) 0.029(4) C16 0.074(6) 0.097(8) 0.077(6) 0.052(6) 0.047(5) 0.060(6) C17 0.100(8) 0.064(6) 0.071(6) 0.033(5) 0.050(6) 0.050(6) C18 0.105(8) 0.040(4) 0.063(5) 0.013(4) 0.048(5) 0.023(5) C19 0.066(5) 0.035(4) 0.052(4) 0.012(3) 0.031(4) 0.012(4) C20 0.041(4) 0.033(3) 0.025(3) 0.005(3) 0.008(3) 0.004(3) C21 0.044(4) 0.040(4) 0.040(4) 0.016(3) 0.017(3) 0.016(3) C22 0.046(4) 0.045(4) 0.035(4) 0.015(3) 0.013(3) 0.014(3) C23 0.042(4) 0.052(4) 0.036(4) 0.014(3) 0.002(3) 0.015(3) C24 0.037(4) 0.049(4) 0.038(4) 0.010(3) 0.009(3) 0.009(3) C25 0.037(3) 0.041(4) 0.034(3) 0.013(3) 0.012(3) 0.009(3) C26 0.137(16) 0.30(3) 0.158(17) 0.092(19) 0.093(14) 0.097(18) C27 0.123(15) 0.152(18) 0.26(3) 0.069(18) 0.053(16) 0.066(13) C28 0.158(17) 0.106(13) 0.22(2) -0.039(14) -0.047(16) 0.083(12) C29 0.153(19) 0.23(3) 0.21(2) -0.10(2) -0.048(17) 0.117(19) C30 0.037(4) 0.081(6) 0.055(5) 0.026(4) 0.011(4) 0.014(4) C31 0.043(4) 0.080(6) 0.050(5) 0.014(4) 0.010(4) 0.026(4) C32 0.065(6) 0.091(8) 0.117(9) 0.057(7) 0.049(6) 0.047(6) C33 0.046(4) 0.049(4) 0.048(4) 0.013(3) 0.010(3) 0.013(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Se1 P1 2.1449(18) . ? Se1 Ca1 2.9889(8) . ? Ca1 O1 2.427(5) . ? Ca1 O1 2.427(5) 2_666 ? Ca1 N1 2.479(5) 2_666 ? Ca1 N1 2.479(5) . ? Ca1 Se1 2.9889(8) 2_666 ? Ca1 P1 3.2737(16) 2_666 ? Ca1 P1 3.2737(16) . ? P1 N1 1.631(6) . ? P1 C20 1.825(7) . ? P1 C14 1.831(7) . ? O1 C33 1.446(9) . ? O1 C30 1.448(9) . ? O2 C26 1.410(19) . ? O2 C29 1.45(2) . ? N1 C1 1.460(8) . ? C1 C8 1.520(10) . ? C1 C2 1.531(9) . ? C1 H5 0.9800 . ? C2 C7 1.385(10) . ? C2 C3 1.392(11) . ? C3 C4 1.383(12) . ? C3 H19 0.9300 . ? C4 C5 1.364(14) . ? C4 H29 0.9300 . ? C5 C6 1.391(13) . ? C5 H14 0.9300 . ? C6 C7 1.382(10) . ? C6 H21 0.9300 . ? C7 H6 0.9300 . ? C8 C13 1.375(10) . ? C8 C9 1.384(10) . ? C9 C10 1.388(11) . ? C9 H17 0.9300 . ? C10 C11 1.366(13) . ? C10 H30 0.9300 . ? C11 C12 1.372(14) . ? C11 H27 0.9300 . ? C12 C13 1.395(12) . ? C12 H26 0.9300 . ? C13 H11 0.9300 . ? C14 C15 1.391(10) . ? C14 C19 1.404(11) . ? C15 C16 1.392(11) . ? C15 H18 0.9300 . ? C16 C17 1.383(14) . ? C16 H31 0.9300 . ? C17 C18 1.382(14) . ? C17 H28 0.9300 . ? C18 C19 1.387(11) . ? C18 H23 0.9300 . ? C19 H12 0.9300 . ? C20 C21 1.388(9) . ? C20 C25 1.398(9) . ? C21 C22 1.386(9) . ? C21 H8 0.9300 . ? C22 C23 1.401(10) . ? C22 H7 0.9300 . ? C23 C24 1.381(10) . ? C23 H3 0.9300 . ? C24 C25 1.382(9) . ? C24 H16 0.9300 . ? C25 H2 0.9300 . ? C26 C27 1.56(2) . ? C26 H1C 0.9300 . ? C27 C28 1.53(3) . ? C27 H1DA 0.9700 . ? C27 H1DB 0.9700 . ? C28 C29 1.54(3) . ? C28 H1A 0.9300 . ? C29 H1BA 0.9700 . ? C29 H1BB 0.9700 . ? C30 C31 1.512(11) . ? C30 H22A 0.9700 . ? C30 H22B 0.9700 . ? C31 C32 1.513(13) . ? C31 H24A 0.9700 . ? C31 H24B 0.9700 . ? C32 C33 1.517(11) . ? C32 H33A 0.9700 . ? C32 H33B 0.9700 . ? C33 H13A 0.9700 . ? C33 H13B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Se1 Ca1 77.31(5) . . ? O1 Ca1 O1 180.000(1) . 2_666 ? O1 Ca1 N1 90.77(17) . 2_666 ? O1 Ca1 N1 89.23(17) 2_666 2_666 ? O1 Ca1 N1 89.23(17) . . ? O1 Ca1 N1 90.77(17) 2_666 . ? N1 Ca1 N1 180.000(1) 2_666 . ? O1 Ca1 Se1 90.35(11) . 2_666 ? O1 Ca1 Se1 89.65(11) 2_666 2_666 ? N1 Ca1 Se1 68.20(13) 2_666 2_666 ? N1 Ca1 Se1 111.80(13) . 2_666 ? O1 Ca1 Se1 89.65(11) . . ? O1 Ca1 Se1 90.35(11) 2_666 . ? N1 Ca1 Se1 111.80(13) 2_666 . ? N1 Ca1 Se1 68.20(13) . . ? Se1 Ca1 Se1 180.0 2_666 . ? O1 Ca1 P1 86.45(12) . 2_666 ? O1 Ca1 P1 93.55(12) 2_666 2_666 ? N1 Ca1 P1 28.95(13) 2_666 2_666 ? N1 Ca1 P1 151.05(13) . 2_666 ? Se1 Ca1 P1 39.73(3) 2_666 2_666 ? Se1 Ca1 P1 140.27(3) . 2_666 ? O1 Ca1 P1 93.55(12) . . ? O1 Ca1 P1 86.45(12) 2_666 . ? N1 Ca1 P1 151.05(13) 2_666 . ? N1 Ca1 P1 28.95(13) . . ? Se1 Ca1 P1 140.27(3) 2_666 . ? Se1 Ca1 P1 39.73(3) . . ? P1 Ca1 P1 180.0 2_666 . ? N1 P1 C20 111.9(3) . . ? N1 P1 C14 114.0(3) . . ? C20 P1 C14 101.7(3) . . ? N1 P1 Se1 109.3(2) . . ? C20 P1 Se1 108.9(2) . . ? C14 P1 Se1 110.7(2) . . ? N1 P1 Ca1 47.37(19) . . ? C20 P1 Ca1 118.0(2) . . ? C14 P1 Ca1 139.9(2) . . ? Se1 P1 Ca1 62.96(4) . . ? C33 O1 C30 109.2(6) . . ? C33 O1 Ca1 125.0(4) . . ? C30 O1 Ca1 125.6(4) . . ? C26 O2 C29 110.4(18) . . ? C1 N1 P1 116.7(4) . . ? C1 N1 Ca1 139.0(4) . . ? P1 N1 Ca1 103.7(3) . . ? N1 C1 C8 115.2(5) . . ? N1 C1 C2 108.7(5) . . ? C8 C1 C2 110.1(5) . . ? N1 C1 H5 107.6 . . ? C8 C1 H5 107.6 . . ? C2 C1 H5 107.6 . . ? C7 C2 C3 118.5(7) . . ? C7 C2 C1 120.6(6) . . ? C3 C2 C1 120.8(7) . . ? C4 C3 C2 120.6(9) . . ? C4 C3 H19 119.7 . . ? C2 C3 H19 119.7 . . ? C5 C4 C3 120.3(9) . . ? C5 C4 H29 119.8 . . ? C3 C4 H29 119.8 . . ? C4 C5 C6 120.0(8) . . ? C4 C5 H14 120.0 . . ? C6 C5 H14 120.0 . . ? C7 C6 C5 119.7(8) . . ? C7 C6 H21 120.1 . . ? C5 C6 H21 120.1 . . ? C6 C7 C2 120.7(8) . . ? C6 C7 H6 119.6 . . ? C2 C7 H6 119.6 . . ? C13 C8 C9 118.0(7) . . ? C13 C8 C1 119.8(7) . . ? C9 C8 C1 122.2(6) . . ? C8 C9 C10 120.9(8) . . ? C8 C9 H17 119.6 . . ? C10 C9 H17 119.6 . . ? C11 C10 C9 120.4(9) . . ? C11 C10 H30 119.8 . . ? C9 C10 H30 119.8 . . ? C10 C11 C12 119.8(8) . . ? C10 C11 H27 120.1 . . ? C12 C11 H27 120.1 . . ? C11 C12 C13 119.7(8) . . ? C11 C12 H26 120.2 . . ? C13 C12 H26 120.2 . . ? C8 C13 C12 121.3(8) . . ? C8 C13 H11 119.4 . . ? C12 C13 H11 119.4 . . ? C15 C14 C19 118.8(7) . . ? C15 C14 P1 121.8(6) . . ? C19 C14 P1 119.3(6) . . ? C14 C15 C16 119.7(9) . . ? C14 C15 H18 120.1 . . ? C16 C15 H18 120.1 . . ? C17 C16 C15 121.7(9) . . ? C17 C16 H31 119.1 . . ? C15 C16 H31 119.1 . . ? C18 C17 C16 118.3(8) . . ? C18 C17 H28 120.8 . . ? C16 C17 H28 120.8 . . ? C17 C18 C19 121.3(9) . . ? C17 C18 H23 119.4 . . ? C19 C18 H23 119.4 . . ? C18 C19 C14 120.1(8) . . ? C18 C19 H12 119.9 . . ? C14 C19 H12 119.9 . . ? C21 C20 C25 119.1(6) . . ? C21 C20 P1 121.3(5) . . ? C25 C20 P1 119.4(5) . . ? C22 C21 C20 120.4(7) . . ? C22 C21 H8 119.8 . . ? C20 C21 H8 119.8 . . ? C21 C22 C23 120.0(6) . . ? C21 C22 H7 120.0 . . ? C23 C22 H7 120.0 . . ? C24 C23 C22 119.6(6) . . ? C24 C23 H3 120.2 . . ? C22 C23 H3 120.2 . . ? C23 C24 C25 120.2(7) . . ? C23 C24 H16 119.9 . . ? C25 C24 H16 119.9 . . ? C24 C25 C20 120.6(6) . . ? C24 C25 H2 119.7 . . ? C20 C25 H2 119.7 . . ? O2 C26 C27 109.5(15) . . ? O2 C26 H1C 125.3 . . ? C27 C26 H1C 125.3 . . ? C28 C27 C26 95.8(17) . . ? C28 C27 H1DA 112.6 . . ? C26 C27 H1DA 112.6 . . ? C28 C27 H1DB 112.6 . . ? C26 C27 H1DB 112.6 . . ? H1DA C27 H1DB 110.1 . . ? C27 C28 C29 111.5(15) . . ? C27 C28 H1A 124.3 . . ? C29 C28 H1A 124.3 . . ? O2 C29 C28 102.2(19) . . ? O2 C29 H1BA 111.3 . . ? C28 C29 H1BA 111.3 . . ? O2 C29 H1BB 111.3 . . ? C28 C29 H1BB 111.3 . . ? H1BA C29 H1BB 109.2 . . ? O1 C30 C31 105.2(6) . . ? O1 C30 H22A 110.7 . . ? C31 C30 H22A 110.7 . . ? O1 C30 H22B 110.7 . . ? C31 C30 H22B 110.7 . . ? H22A C30 H22B 108.8 . . ? C30 C31 C32 102.2(7) . . ? C30 C31 H24A 111.3 . . ? C32 C31 H24A 111.3 . . ? C30 C31 H24B 111.3 . . ? C32 C31 H24B 111.3 . . ? H24A C31 H24B 109.2 . . ? C31 C32 C33 104.6(7) . . ? C31 C32 H33A 110.8 . . ? C33 C32 H33A 110.8 . . ? C31 C32 H33B 110.8 . . ? C33 C32 H33B 110.8 . . ? H33A C32 H33B 108.9 . . ? O1 C33 C32 106.3(6) . . ? O1 C33 H13A 110.5 . . ? C32 C33 H13A 110.5 . . ? O1 C33 H13B 110.5 . . ? C32 C33 H13B 110.5 . . ? H13A C33 H13B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Se1 Ca1 O1 -95.98(13) . . . . ? P1 Se1 Ca1 O1 84.02(13) . . . 2_666 ? P1 Se1 Ca1 N1 173.32(14) . . . 2_666 ? P1 Se1 Ca1 N1 -6.68(14) . . . . ? P1 Se1 Ca1 Se1 -168(100) . . . 2_666 ? P1 Se1 Ca1 P1 180.0 . . . 2_666 ? Ca1 Se1 P1 N1 10.0(2) . . . . ? Ca1 Se1 P1 C20 -112.5(2) . . . . ? Ca1 Se1 P1 C14 136.5(2) . . . . ? O1 Ca1 P1 N1 -82.0(3) . . . . ? O1 Ca1 P1 N1 98.0(3) 2_666 . . . ? N1 Ca1 P1 N1 180.000(1) 2_666 . . . ? Se1 Ca1 P1 N1 12.9(3) 2_666 . . . ? Se1 Ca1 P1 N1 -167.1(3) . . . . ? P1 Ca1 P1 N1 175(100) 2_666 . . . ? O1 Ca1 P1 C20 -176.8(3) . . . . ? O1 Ca1 P1 C20 3.2(3) 2_666 . . . ? N1 Ca1 P1 C20 85.1(4) 2_666 . . . ? N1 Ca1 P1 C20 -94.9(4) . . . . ? Se1 Ca1 P1 C20 -82.0(2) 2_666 . . . ? Se1 Ca1 P1 C20 98.0(2) . . . . ? P1 Ca1 P1 C20 80(100) 2_666 . . . ? O1 Ca1 P1 C14 -5.4(4) . . . . ? O1 Ca1 P1 C14 174.6(4) 2_666 . . . ? N1 Ca1 P1 C14 -103.5(4) 2_666 . . . ? N1 Ca1 P1 C14 76.5(4) . . . . ? Se1 Ca1 P1 C14 89.4(4) 2_666 . . . ? Se1 Ca1 P1 C14 -90.6(4) . . . . ? P1 Ca1 P1 C14 -109(100) 2_666 . . . ? O1 Ca1 P1 Se1 85.16(13) . . . . ? O1 Ca1 P1 Se1 -94.84(13) 2_666 . . . ? N1 Ca1 P1 Se1 -12.9(3) 2_666 . . . ? N1 Ca1 P1 Se1 167.1(3) . . . . ? Se1 Ca1 P1 Se1 180.0 2_666 . . . ? P1 Ca1 P1 Se1 -18(100) 2_666 . . . ? O1 Ca1 O1 C33 71(100) 2_666 . . . ? N1 Ca1 O1 C33 -92.7(5) 2_666 . . . ? N1 Ca1 O1 C33 87.3(5) . . . . ? Se1 Ca1 O1 C33 -24.5(5) 2_666 . . . ? Se1 Ca1 O1 C33 155.5(5) . . . . ? P1 Ca1 O1 C33 -64.0(5) 2_666 . . . ? P1 Ca1 O1 C33 116.0(5) . . . . ? O1 Ca1 O1 C30 -104(100) 2_666 . . . ? N1 Ca1 O1 C30 93.0(6) 2_666 . . . ? N1 Ca1 O1 C30 -87.0(6) . . . . ? Se1 Ca1 O1 C30 161.2(6) 2_666 . . . ? Se1 Ca1 O1 C30 -18.8(6) . . . . ? P1 Ca1 O1 C30 121.7(6) 2_666 . . . ? P1 Ca1 O1 C30 -58.3(6) . . . . ? C20 P1 N1 C1 -64.6(5) . . . . ? C14 P1 N1 C1 50.2(6) . . . . ? Se1 P1 N1 C1 174.7(4) . . . . ? Ca1 P1 N1 C1 -173.1(6) . . . . ? C20 P1 N1 Ca1 108.5(3) . . . . ? C14 P1 N1 Ca1 -136.7(3) . . . . ? Se1 P1 N1 Ca1 -12.2(2) . . . . ? O1 Ca1 N1 C1 -90.6(6) . . . . ? O1 Ca1 N1 C1 89.4(6) 2_666 . . . ? N1 Ca1 N1 C1 126(100) 2_666 . . . ? Se1 Ca1 N1 C1 -0.6(6) 2_666 . . . ? Se1 Ca1 N1 C1 179.4(6) . . . . ? P1 Ca1 N1 C1 -9.4(8) 2_666 . . . ? P1 Ca1 N1 C1 170.6(8) . . . . ? O1 Ca1 N1 P1 98.8(3) . . . . ? O1 Ca1 N1 P1 -81.2(3) 2_666 . . . ? N1 Ca1 N1 P1 -44(100) 2_666 . . . ? Se1 Ca1 N1 P1 -171.17(18) 2_666 . . . ? Se1 Ca1 N1 P1 8.83(18) . . . . ? P1 Ca1 N1 P1 180.000(1) 2_666 . . . ? P1 N1 C1 C8 -87.3(6) . . . . ? Ca1 N1 C1 C8 102.9(7) . . . . ? P1 N1 C1 C2 148.7(5) . . . . ? Ca1 N1 C1 C2 -21.0(9) . . . . ? N1 C1 C2 C7 77.7(8) . . . . ? C8 C1 C2 C7 -49.3(9) . . . . ? N1 C1 C2 C3 -102.3(8) . . . . ? C8 C1 C2 C3 130.8(8) . . . . ? C7 C2 C3 C4 -1.0(14) . . . . ? C1 C2 C3 C4 178.9(9) . . . . ? C2 C3 C4 C5 -0.4(17) . . . . ? C3 C4 C5 C6 0.3(16) . . . . ? C4 C5 C6 C7 1.1(14) . . . . ? C5 C6 C7 C2 -2.5(12) . . . . ? C3 C2 C7 C6 2.5(12) . . . . ? C1 C2 C7 C6 -177.5(7) . . . . ? N1 C1 C8 C13 166.0(6) . . . . ? C2 C1 C8 C13 -70.7(8) . . . . ? N1 C1 C8 C9 -16.1(9) . . . . ? C2 C1 C8 C9 107.2(7) . . . . ? C13 C8 C9 C10 1.6(11) . . . . ? C1 C8 C9 C10 -176.3(7) . . . . ? C8 C9 C10 C11 -1.4(13) . . . . ? C9 C10 C11 C12 0.3(14) . . . . ? C10 C11 C12 C13 0.4(14) . . . . ? C9 C8 C13 C12 -0.9(11) . . . . ? C1 C8 C13 C12 177.1(7) . . . . ? C11 C12 C13 C8 -0.1(13) . . . . ? N1 P1 C14 C15 101.1(6) . . . . ? C20 P1 C14 C15 -138.2(6) . . . . ? Se1 P1 C14 C15 -22.7(6) . . . . ? Ca1 P1 C14 C15 49.5(7) . . . . ? N1 P1 C14 C19 -74.7(6) . . . . ? C20 P1 C14 C19 46.0(6) . . . . ? Se1 P1 C14 C19 161.6(5) . . . . ? Ca1 P1 C14 C19 -126.2(5) . . . . ? C19 C14 C15 C16 1.2(10) . . . . ? P1 C14 C15 C16 -174.5(6) . . . . ? C14 C15 C16 C17 -0.8(12) . . . . ? C15 C16 C17 C18 -0.4(13) . . . . ? C16 C17 C18 C19 1.1(13) . . . . ? C17 C18 C19 C14 -0.6(12) . . . . ? C15 C14 C19 C18 -0.6(10) . . . . ? P1 C14 C19 C18 175.3(6) . . . . ? N1 P1 C20 C21 165.5(5) . . . . ? C14 P1 C20 C21 43.4(6) . . . . ? Se1 P1 C20 C21 -73.5(6) . . . . ? Ca1 P1 C20 C21 -142.3(5) . . . . ? N1 P1 C20 C25 -19.7(6) . . . . ? C14 P1 C20 C25 -141.8(6) . . . . ? Se1 P1 C20 C25 101.3(5) . . . . ? Ca1 P1 C20 C25 32.5(6) . . . . ? C25 C20 C21 C22 0.4(10) . . . . ? P1 C20 C21 C22 175.3(5) . . . . ? C20 C21 C22 C23 0.1(11) . . . . ? C21 C22 C23 C24 -0.3(11) . . . . ? C22 C23 C24 C25 -0.1(11) . . . . ? C23 C24 C25 C20 0.6(11) . . . . ? C21 C20 C25 C24 -0.8(10) . . . . ? P1 C20 C25 C24 -175.7(5) . . . . ? C29 O2 C26 C27 -29(2) . . . . ? O2 C26 C27 C28 32(2) . . . . ? C26 C27 C28 C29 -26(2) . . . . ? C26 O2 C29 C28 10(2) . . . . ? C27 C28 C29 O2 12(2) . . . . ? C33 O1 C30 C31 24.5(9) . . . . ? Ca1 O1 C30 C31 -160.4(5) . . . . ? O1 C30 C31 C32 -34.9(9) . . . . ? C30 C31 C32 C33 32.3(10) . . . . ? C30 O1 C33 C32 -3.7(9) . . . . ? Ca1 O1 C33 C32 -178.8(6) . . . . ? C31 C32 C33 O1 -18.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 70.99 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.321 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.107 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 903853' #TrackingRef 'exp_843(1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H74 N2 Na2 O4 P2 Se2' _chemical_formula_sum 'C66 H74 N2 Na2 O4 P2 Se2' _chemical_formula_weight 1225.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Y Y -0.2670 2.0244 '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' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 10.3920(17) _cell_length_b 12.981(2) _cell_length_c 13.4630(17) _cell_angle_alpha 109.103(13) _cell_angle_beta 107.189(13) _cell_angle_gamma 104.478(14) _cell_volume 1513.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5008 _cell_measurement_theta_min 3.8136 _cell_measurement_theta_max 70.6634 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 2.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74401 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _exptl_special_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 16.1293 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11164 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 70.74 _reflns_number_total 5681 _reflns_number_gt 4886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Intel duo core 2 computer' _computing_cell_refinement 'Intel duo core 2 computer' _computing_data_reduction 'Intel duo core 2 computer' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III & Olex 2.1' _computing_publication_material WinGX _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. Disordered C30 of a coordinated tetrahydrofuran was refined with split model with site occupation factor 0.49(2). ; _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^)+(0.0580P)^2^+0.3810P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5681 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.25480(3) 0.46324(2) 0.91709(2) 0.03984(10) Uani 1 1 d . . . Na1 Na 0.48028(10) 0.51213(8) 1.14385(8) 0.0398(2) Uani 1 1 d . . . O1 O 0.5620(2) 0.3853(2) 1.2231(2) 0.0638(6) Uani 1 1 d . . . O2 O 0.2906(2) 0.4814(2) 1.21094(18) 0.0621(6) Uani 1 1 d . B . P1 P 0.20461(6) 0.29402(5) 0.78303(5) 0.03080(14) Uani 1 1 d . . . N1 N 0.3387(2) 0.29264(16) 0.74878(16) 0.0320(4) Uani 1 1 d . . . C1 C 0.3467(2) 0.17971(19) 0.68502(19) 0.0320(5) Uani 1 1 d . . . H7AA H 0.2538 0.1161 0.6610 0.038 Uiso 1 1 calc R . . C2 C 0.4672(3) 0.16051(19) 0.76488(19) 0.0330(5) Uani 1 1 d . . . C3 C 0.4360(3) 0.0709(2) 0.7991(2) 0.0393(5) Uani 1 1 d . . . H2 H 0.3396 0.0203 0.7718 0.047 Uiso 1 1 calc R . . C4 C 0.5468(3) 0.0554(2) 0.8739(2) 0.0451(6) Uani 1 1 d . . . H2DA H 0.5241 -0.0050 0.8963 0.054 Uiso 1 1 calc R . . C5 C 0.6901(3) 0.1296(2) 0.9146(2) 0.0470(6) Uani 1 1 d . . . H5BA H 0.7642 0.1186 0.9635 0.056 Uiso 1 1 calc R . . C6 C 0.7236(3) 0.2205(2) 0.8826(2) 0.0442(6) Uani 1 1 d . . . H1BA H 0.8200 0.2716 0.9112 0.053 Uiso 1 1 calc R . . C7 C 0.6126(3) 0.2353(2) 0.8074(2) 0.0371(5) Uani 1 1 d . . . H7 H 0.6357 0.2959 0.7853 0.044 Uiso 1 1 calc R . . C8 C 0.3698(2) 0.1743(2) 0.57660(19) 0.0325(5) Uani 1 1 d . . . C9 C 0.3563(3) 0.0669(2) 0.4969(2) 0.0414(6) Uani 1 1 d . . . H7DA H 0.3355 0.0008 0.5115 0.050 Uiso 1 1 calc R . . C10 C 0.3733(3) 0.0573(3) 0.3963(2) 0.0471(6) Uani 1 1 d . . . H6 H 0.3633 -0.0150 0.3438 0.057 Uiso 1 1 calc R . . C11 C 0.4052(3) 0.1551(3) 0.3741(2) 0.0463(6) Uani 1 1 d . . . H17 H 0.4159 0.1489 0.3064 0.056 Uiso 1 1 calc R . . C12 C 0.4210(3) 0.2617(2) 0.4527(2) 0.0445(6) Uani 1 1 d . . . H12 H 0.4438 0.3280 0.4385 0.053 Uiso 1 1 calc R . . C13 C 0.0387(2) 0.26443(19) 0.6626(2) 0.0329(5) Uani 1 1 d . . . C14 C -0.0865(3) 0.2699(2) 0.6793(2) 0.0389(5) Uani 1 1 d . . . H5AA H -0.0863 0.2874 0.7521 0.047 Uiso 1 1 calc R . . C15 C -0.2108(3) 0.2496(2) 0.5884(2) 0.0427(6) Uani 1 1 d . . . H9AA H -0.2930 0.2546 0.6005 0.051 Uiso 1 1 calc R . . C16 C -0.2123(3) 0.2219(2) 0.4796(2) 0.0443(6) Uani 1 1 d . . . H15 H -0.2958 0.2076 0.4183 0.053 Uiso 1 1 calc R . . C17 C -0.0891(3) 0.2156(2) 0.4622(2) 0.0446(6) Uani 1 1 d . . . H1 H -0.0898 0.1975 0.3892 0.054 Uiso 1 1 calc R . . C18 C 0.0350(3) 0.2361(2) 0.5530(2) 0.0383(5) Uani 1 1 d . . . H19 H 0.1169 0.2307 0.5404 0.046 Uiso 1 1 calc R . . C19 C 0.1420(2) 0.1741(2) 0.8219(2) 0.0345(5) Uani 1 1 d . . . C20 C 0.2095(3) 0.1867(2) 0.9338(2) 0.0484(6) Uani 1 1 d . . . H1B H 0.2819 0.2589 0.9903 0.058 Uiso 1 1 calc R . . C21 C 0.1706(3) 0.0938(3) 0.9620(3) 0.0579(8) Uani 1 1 d . . . H13 H 0.2175 0.1036 1.0368 0.070 Uiso 1 1 calc R . . C22 C 0.0628(3) -0.0131(3) 0.8797(3) 0.0553(7) Uani 1 1 d . . . H3 H 0.0363 -0.0754 0.8990 0.066 Uiso 1 1 calc R . . C23 C -0.0063(3) -0.0278(2) 0.7682(3) 0.0506(7) Uani 1 1 d . . . H8 H -0.0790 -0.1000 0.7124 0.061 Uiso 1 1 calc R . . C24 C 0.0330(3) 0.0655(2) 0.7395(2) 0.0421(6) Uani 1 1 d . . . H9 H -0.0141 0.0551 0.6644 0.050 Uiso 1 1 calc R . . C25 C 0.6852(4) 0.4435(3) 1.3328(3) 0.0672(9) Uani 1 1 d . . . H18A H 0.6600 0.4222 1.3892 0.081 Uiso 1 1 calc R . . H18B H 0.7177 0.5285 1.3606 0.081 Uiso 1 1 calc R . . C26 C 0.8022(3) 0.4031(3) 1.3135(3) 0.0580(8) Uani 1 1 d . . . H0CA H 0.8658 0.4028 1.3825 0.070 Uiso 1 1 calc R . . H0CB H 0.8602 0.4524 1.2892 0.070 Uiso 1 1 calc R . . C27 C 0.7138(4) 0.2779(3) 1.2172(3) 0.0603(8) Uani 1 1 d . . . H5A H 0.7667 0.2544 1.1711 0.072 Uiso 1 1 calc R . . H5B H 0.6912 0.2217 1.2486 0.072 Uiso 1 1 calc R . . C28 C 0.5796(4) 0.2853(3) 1.1479(3) 0.0737(10) Uani 1 1 d . . . H1CA H 0.5883 0.2968 1.0822 0.088 Uiso 1 1 calc R . . H1CB H 0.4961 0.2132 1.1198 0.088 Uiso 1 1 calc R . . C29 C 0.2975(4) 0.4412(4) 1.2986(3) 0.0790(12) Uani 1 1 d . . . H1AA H 0.3322 0.3773 1.2851 0.095 Uiso 1 1 calc R A 1 H1AB H 0.3645 0.5051 1.3737 0.095 Uiso 1 1 calc R A 1 C30A C 0.1574(11) 0.4019(17) 1.2955(11) 0.074(3) Uani 0.49(2) 1 d P B 1 H30A H 0.1385 0.4656 1.3430 0.089 Uiso 0.49(2) 1 calc PR B 1 H30B H 0.1417 0.3386 1.3194 0.089 Uiso 0.49(2) 1 calc PR B 1 C30B C 0.1679(11) 0.3404(12) 1.2544(11) 0.070(4) Uani 0.51(2) 1 d P B 2 H30C H 0.1335 0.3395 1.3138 0.084 Uiso 0.51(2) 1 calc PR B 2 H30D H 0.1833 0.2681 1.2230 0.084 Uiso 0.51(2) 1 calc PR B 2 C31 C 0.0590(4) 0.3551(4) 1.1586(4) 0.1020(17) Uani 1 1 d . . . H7CA H 0.0630 0.2824 1.1112 0.122 Uiso 1 1 calc R B 1 H7CB H -0.0417 0.3458 1.1423 0.122 Uiso 1 1 calc R B 1 C32 C 0.1395(3) 0.4557(3) 1.1485(3) 0.0563(7) Uani 1 1 d . B . H4DA H 0.1180 0.4378 1.0682 0.068 Uiso 1 1 calc R . . H4DB H 0.1148 0.5225 1.1815 0.068 Uiso 1 1 calc R . . C33 C 0.4031(3) 0.2713(2) 0.5537(2) 0.0381(5) Uani 1 1 d . . . H4BA H 0.4137 0.3439 0.6061 0.046 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 Se1 0.04263(16) 0.03673(16) 0.03196(15) 0.00789(11) 0.01122(11) 0.01702(12) Na1 0.0357(5) 0.0315(5) 0.0406(5) 0.0136(4) 0.0086(4) 0.0064(4) O1 0.0525(12) 0.0632(13) 0.0883(16) 0.0467(13) 0.0256(12) 0.0269(11) O2 0.0374(10) 0.0814(15) 0.0643(13) 0.0497(12) 0.0119(9) 0.0044(10) P1 0.0306(3) 0.0293(3) 0.0297(3) 0.0111(2) 0.0116(2) 0.0103(2) N1 0.0303(9) 0.0266(9) 0.0334(10) 0.0098(8) 0.0123(8) 0.0075(7) C1 0.0301(11) 0.0257(10) 0.0348(12) 0.0114(9) 0.0124(9) 0.0058(9) C2 0.0375(12) 0.0284(11) 0.0313(11) 0.0107(9) 0.0146(10) 0.0126(9) C3 0.0464(14) 0.0315(12) 0.0358(12) 0.0128(10) 0.0158(11) 0.0123(10) C4 0.0613(17) 0.0368(13) 0.0401(14) 0.0203(11) 0.0190(12) 0.0206(12) C5 0.0551(16) 0.0480(15) 0.0348(13) 0.0171(11) 0.0099(12) 0.0267(13) C6 0.0369(13) 0.0472(14) 0.0399(13) 0.0138(11) 0.0113(11) 0.0150(11) C7 0.0368(12) 0.0358(12) 0.0362(12) 0.0162(10) 0.0130(10) 0.0120(10) C8 0.0264(10) 0.0335(11) 0.0317(11) 0.0117(9) 0.0091(9) 0.0093(9) C9 0.0462(14) 0.0354(12) 0.0365(13) 0.0117(10) 0.0148(11) 0.0141(11) C10 0.0487(15) 0.0519(16) 0.0340(13) 0.0099(12) 0.0160(12) 0.0220(13) C11 0.0362(13) 0.0705(18) 0.0363(13) 0.0243(13) 0.0166(11) 0.0231(13) C12 0.0410(14) 0.0547(16) 0.0465(14) 0.0295(13) 0.0201(12) 0.0190(12) C13 0.0337(12) 0.0269(11) 0.0353(12) 0.0134(9) 0.0120(10) 0.0102(9) C14 0.0394(13) 0.0414(13) 0.0378(13) 0.0171(11) 0.0173(11) 0.0169(11) C15 0.0345(13) 0.0448(14) 0.0516(15) 0.0218(12) 0.0188(11) 0.0172(11) C16 0.0343(13) 0.0465(14) 0.0437(14) 0.0197(12) 0.0070(11) 0.0134(11) C17 0.0425(14) 0.0526(15) 0.0354(13) 0.0181(12) 0.0134(11) 0.0176(12) C18 0.0345(12) 0.0412(13) 0.0364(12) 0.0153(10) 0.0135(10) 0.0134(10) C19 0.0305(11) 0.0378(12) 0.0386(12) 0.0185(10) 0.0159(10) 0.0138(10) C20 0.0481(15) 0.0464(15) 0.0441(15) 0.0231(12) 0.0141(12) 0.0093(12) C21 0.0584(18) 0.0656(19) 0.0550(17) 0.0392(16) 0.0199(15) 0.0184(15) C22 0.0481(16) 0.0562(17) 0.079(2) 0.0464(16) 0.0307(15) 0.0189(13) C23 0.0379(14) 0.0448(15) 0.0662(18) 0.0276(14) 0.0181(13) 0.0108(12) C24 0.0362(13) 0.0396(13) 0.0476(14) 0.0214(11) 0.0142(11) 0.0105(10) C25 0.072(2) 0.0553(18) 0.078(2) 0.0296(17) 0.0297(19) 0.0294(17) C26 0.0547(17) 0.0578(18) 0.0658(19) 0.0367(16) 0.0191(15) 0.0217(14) C27 0.0559(18) 0.070(2) 0.0536(17) 0.0241(16) 0.0201(15) 0.0282(16) C28 0.064(2) 0.0420(16) 0.093(3) 0.0306(17) 0.0070(19) 0.0150(15) C29 0.0525(19) 0.107(3) 0.083(2) 0.071(2) 0.0178(18) 0.0101(19) C30A 0.080(5) 0.085(9) 0.089(7) 0.052(6) 0.055(5) 0.037(6) C30B 0.060(5) 0.057(6) 0.071(6) 0.041(5) 0.005(4) -0.006(4) C31 0.051(2) 0.119(4) 0.114(3) 0.078(3) 0.005(2) -0.005(2) C32 0.0437(15) 0.0651(19) 0.0575(18) 0.0287(16) 0.0168(14) 0.0190(14) C33 0.0382(13) 0.0392(13) 0.0395(13) 0.0186(11) 0.0173(11) 0.0151(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 Se1 P1 2.1519(8) . ? Se1 Na1 2.9956(12) . ? Se1 Na1 3.0694(11) 2_667 ? Na1 N1 2.380(2) 2_667 ? Na1 O2 2.399(2) . ? Na1 O1 2.426(2) . ? Na1 Se1 3.0694(11) 2_667 ? Na1 P1 3.2214(13) 2_667 ? Na1 Na1 3.934(2) 2_667 ? O1 C25 1.435(4) . ? O1 C28 1.453(4) . ? O2 C29 1.429(3) . ? O2 C32 1.434(3) . ? P1 N1 1.594(2) . ? P1 C19 1.831(2) . ? P1 C13 1.832(2) . ? P1 Na1 3.2214(13) 2_667 ? N1 C1 1.474(3) . ? N1 Na1 2.380(2) 2_667 ? C1 C2 1.524(3) . ? C1 C8 1.530(3) . ? C1 H7AA 0.9800 . ? C2 C3 1.387(3) . ? C2 C7 1.395(3) . ? C3 C4 1.394(4) . ? C3 H2 0.9300 . ? C4 C5 1.379(4) . ? C4 H2DA 0.9300 . ? C5 C6 1.385(4) . ? C5 H5BA 0.9300 . ? C6 C7 1.392(3) . ? C6 H1BA 0.9300 . ? C7 H7 0.9300 . ? C8 C33 1.378(3) . ? C8 C9 1.396(3) . ? C9 C10 1.387(4) . ? C9 H7DA 0.9300 . ? C10 C11 1.382(4) . ? C10 H6 0.9300 . ? C11 C12 1.373(4) . ? C11 H17 0.9300 . ? C12 C33 1.397(3) . ? C12 H12 0.9300 . ? C13 C18 1.384(3) . ? C13 C14 1.399(3) . ? C14 C15 1.386(3) . ? C14 H5AA 0.9300 . ? C15 C16 1.383(4) . ? C15 H9AA 0.9300 . ? C16 C17 1.385(4) . ? C16 H15 0.9300 . ? C17 C18 1.384(4) . ? C17 H1 0.9300 . ? C18 H19 0.9300 . ? C19 C24 1.392(3) . ? C19 C20 1.394(3) . ? C20 C21 1.381(4) . ? C20 H1B 0.9300 . ? C21 C22 1.376(4) . ? C21 H13 0.9300 . ? C22 C23 1.382(4) . ? C22 H3 0.9300 . ? C23 C24 1.390(4) . ? C23 H8 0.9300 . ? C24 H9 0.9300 . ? C25 C26 1.496(5) . ? C25 H18A 0.9700 . ? C25 H18B 0.9700 . ? C26 C27 1.529(4) . ? C26 H0CA 0.9700 . ? C26 H0CB 0.9700 . ? C27 C28 1.477(4) . ? C27 H5A 0.9700 . ? C27 H5B 0.9700 . ? C28 H1CA 0.9700 . ? C28 H1CB 0.9700 . ? C29 C30A 1.400(10) . ? C29 C30B 1.420(8) . ? C29 H1AA 0.9700 . ? C29 H1AB 0.9700 . ? C30A C31 1.629(12) . ? C30A H30A 0.9700 . ? C30A H30B 0.9700 . ? C30B C31 1.544(9) . ? C30B H30C 0.9700 . ? C30B H30D 0.9700 . ? C31 C32 1.436(5) . ? C31 H7CA 0.9700 . ? C31 H7CB 0.9700 . ? C32 H4DA 0.9700 . ? C32 H4DB 0.9700 . ? C33 H4BA 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Se1 Na1 112.50(3) . . ? P1 Se1 Na1 73.85(3) . 2_667 ? Na1 Se1 Na1 80.86(3) . 2_667 ? N1 Na1 O2 112.65(8) 2_667 . ? N1 Na1 O1 108.79(8) 2_667 . ? O2 Na1 O1 87.63(8) . . ? N1 Na1 Se1 115.92(6) 2_667 . ? O2 Na1 Se1 88.37(6) . . ? O1 Na1 Se1 132.94(7) . . ? N1 Na1 Se1 68.15(5) 2_667 2_667 ? O2 Na1 Se1 171.24(6) . 2_667 ? O1 Na1 Se1 83.95(6) . 2_667 ? Se1 Na1 Se1 99.14(3) . 2_667 ? N1 Na1 P1 28.30(5) 2_667 2_667 ? O2 Na1 P1 139.98(7) . 2_667 ? O1 Na1 P1 98.30(6) . 2_667 ? Se1 Na1 P1 114.01(4) . 2_667 ? Se1 Na1 P1 39.915(19) 2_667 2_667 ? N1 Na1 Na1 92.43(6) 2_667 2_667 ? O2 Na1 Na1 138.54(7) . 2_667 ? O1 Na1 Na1 115.89(7) . 2_667 ? Se1 Na1 Na1 50.39(2) . 2_667 ? Se1 Na1 Na1 48.75(3) 2_667 2_667 ? P1 Na1 Na1 73.23(3) 2_667 2_667 ? C25 O1 C28 109.0(2) . . ? C25 O1 Na1 116.30(18) . . ? C28 O1 Na1 118.21(19) . . ? C29 O2 C32 106.4(2) . . ? C29 O2 Na1 122.8(2) . . ? C32 O2 Na1 126.92(17) . . ? N1 P1 C19 112.51(10) . . ? N1 P1 C13 113.31(11) . . ? C19 P1 C13 101.49(11) . . ? N1 P1 Se1 111.15(7) . . ? C19 P1 Se1 111.51(8) . . ? C13 P1 Se1 106.36(8) . . ? N1 P1 Na1 45.05(7) . 2_667 ? C19 P1 Na1 134.00(8) . 2_667 ? C13 P1 Na1 123.75(8) . 2_667 ? Se1 P1 Na1 66.23(3) . 2_667 ? C1 N1 P1 120.36(15) . . ? C1 N1 Na1 131.32(14) . 2_667 ? P1 N1 Na1 106.65(10) . 2_667 ? N1 C1 C2 109.44(18) . . ? N1 C1 C8 111.94(18) . . ? C2 C1 C8 111.21(18) . . ? N1 C1 H7AA 108.0 . . ? C2 C1 H7AA 108.0 . . ? C8 C1 H7AA 108.0 . . ? C3 C2 C7 118.3(2) . . ? C3 C2 C1 121.5(2) . . ? C7 C2 C1 120.2(2) . . ? C2 C3 C4 121.0(2) . . ? C2 C3 H2 119.5 . . ? C4 C3 H2 119.5 . . ? C5 C4 C3 119.9(2) . . ? C5 C4 H2DA 120.0 . . ? C3 C4 H2DA 120.0 . . ? C4 C5 C6 120.0(2) . . ? C4 C5 H5BA 120.0 . . ? C6 C5 H5BA 120.0 . . ? C5 C6 C7 119.9(2) . . ? C5 C6 H1BA 120.1 . . ? C7 C6 H1BA 120.1 . . ? C6 C7 C2 120.8(2) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? C33 C8 C9 118.3(2) . . ? C33 C8 C1 122.7(2) . . ? C9 C8 C1 119.0(2) . . ? C10 C9 C8 121.0(2) . . ? C10 C9 H7DA 119.5 . . ? C8 C9 H7DA 119.5 . . ? C11 C10 C9 120.0(2) . . ? C11 C10 H6 120.0 . . ? C9 C10 H6 120.0 . . ? C12 C11 C10 119.5(2) . . ? C12 C11 H17 120.2 . . ? C10 C11 H17 120.2 . . ? C11 C12 C33 120.5(2) . . ? C11 C12 H12 119.7 . . ? C33 C12 H12 119.7 . . ? C18 C13 C14 118.7(2) . . ? C18 C13 P1 120.47(18) . . ? C14 C13 P1 120.85(18) . . ? C15 C14 C13 120.6(2) . . ? C15 C14 H5AA 119.7 . . ? C13 C14 H5AA 119.7 . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H9AA 120.1 . . ? C14 C15 H9AA 120.1 . . ? C15 C16 C17 119.9(2) . . ? C15 C16 H15 120.1 . . ? C17 C16 H15 120.1 . . ? C18 C17 C16 120.2(2) . . ? C18 C17 H1 119.9 . . ? C16 C17 H1 119.9 . . ? C17 C18 C13 120.7(2) . . ? C17 C18 H19 119.6 . . ? C13 C18 H19 119.6 . . ? C24 C19 C20 118.2(2) . . ? C24 C19 P1 121.18(18) . . ? C20 C19 P1 120.53(19) . . ? C21 C20 C19 121.0(3) . . ? C21 C20 H1B 119.5 . . ? C19 C20 H1B 119.5 . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H13 119.9 . . ? C20 C21 H13 119.9 . . ? C21 C22 C23 119.8(3) . . ? C21 C22 H3 120.1 . . ? C23 C22 H3 120.1 . . ? C22 C23 C24 120.1(3) . . ? C22 C23 H8 120.0 . . ? C24 C23 H8 120.0 . . ? C23 C24 C19 120.7(2) . . ? C23 C24 H9 119.7 . . ? C19 C24 H9 119.7 . . ? O1 C25 C26 106.2(3) . . ? O1 C25 H18A 110.5 . . ? C26 C25 H18A 110.5 . . ? O1 C25 H18B 110.5 . . ? C26 C25 H18B 110.5 . . ? H18A C25 H18B 108.7 . . ? C25 C26 C27 102.2(3) . . ? C25 C26 H0CA 111.3 . . ? C27 C26 H0CA 111.3 . . ? C25 C26 H0CB 111.3 . . ? C27 C26 H0CB 111.3 . . ? H0CA C26 H0CB 109.2 . . ? C28 C27 C26 104.0(3) . . ? C28 C27 H5A 111.0 . . ? C26 C27 H5A 111.0 . . ? C28 C27 H5B 111.0 . . ? C26 C27 H5B 111.0 . . ? H5A C27 H5B 109.0 . . ? O1 C28 C27 106.9(3) . . ? O1 C28 H1CA 110.3 . . ? C27 C28 H1CA 110.3 . . ? O1 C28 H1CB 110.3 . . ? C27 C28 H1CB 110.3 . . ? H1CA C28 H1CB 108.6 . . ? C30A C29 C30B 35.6(4) . . ? C30A C29 O2 108.4(5) . . ? C30B C29 O2 107.7(4) . . ? C30A C29 H1AA 110.0 . . ? C30B C29 H1AA 77.5 . . ? O2 C29 H1AA 110.0 . . ? C30A C29 H1AB 110.0 . . ? C30B C29 H1AB 136.4 . . ? O2 C29 H1AB 110.0 . . ? H1AA C29 H1AB 108.4 . . ? C29 C30A C31 100.2(6) . . ? C29 C30A H30A 111.7 . . ? C31 C30A H30A 111.7 . . ? C29 C30A H30B 111.7 . . ? C31 C30A H30B 111.7 . . ? H30A C30A H30B 109.5 . . ? C29 C30B C31 103.4(5) . . ? C29 C30B H30C 111.1 . . ? C31 C30B H30C 111.1 . . ? C29 C30B H30D 111.1 . . ? C31 C30B H30D 111.1 . . ? H30C C30B H30D 109.0 . . ? C32 C31 C30B 106.8(4) . . ? C32 C31 C30A 95.8(6) . . ? C30B C31 C30A 31.4(4) . . ? C32 C31 H7CA 112.6 . . ? C30B C31 H7CA 81.2 . . ? C30A C31 H7CA 112.6 . . ? C32 C31 H7CB 112.6 . . ? C30B C31 H7CB 129.4 . . ? C30A C31 H7CB 112.6 . . ? H7CA C31 H7CB 110.1 . . ? O2 C32 C31 105.9(3) . . ? O2 C32 H4DA 110.6 . . ? C31 C32 H4DA 110.6 . . ? O2 C32 H4DB 110.6 . . ? C31 C32 H4DB 110.6 . . ? H4DA C32 H4DB 108.7 . . ? C8 C33 C12 120.7(2) . . ? C8 C33 H4BA 119.7 . . ? C12 C33 H4BA 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Se1 Na1 N1 138.25(6) . . . 2_667 ? Na1 Se1 Na1 N1 70.06(6) 2_667 . . 2_667 ? P1 Se1 Na1 O2 -107.27(7) . . . . ? Na1 Se1 Na1 O2 -175.46(7) 2_667 . . . ? P1 Se1 Na1 O1 -22.04(10) . . . . ? Na1 Se1 Na1 O1 -90.23(10) 2_667 . . . ? P1 Se1 Na1 Se1 68.19(3) . . . 2_667 ? Na1 Se1 Na1 Se1 0.000(2) 2_667 . . 2_667 ? P1 Se1 Na1 P1 107.04(3) . . . 2_667 ? Na1 Se1 Na1 P1 38.85(2) 2_667 . . 2_667 ? P1 Se1 Na1 Na1 68.19(3) . . . 2_667 ? N1 Na1 O1 C25 12.5(2) 2_667 . . . ? O2 Na1 O1 C25 -100.6(2) . . . . ? Se1 Na1 O1 C25 173.84(19) . . . . ? Se1 Na1 O1 C25 77.0(2) 2_667 . . . ? P1 Na1 O1 C25 39.6(2) 2_667 . . . ? Na1 Na1 O1 C25 114.9(2) 2_667 . . . ? N1 Na1 O1 C28 -120.1(2) 2_667 . . . ? O2 Na1 O1 C28 126.7(2) . . . . ? Se1 Na1 O1 C28 41.2(2) . . . . ? Se1 Na1 O1 C28 -55.7(2) 2_667 . . . ? P1 Na1 O1 C28 -93.0(2) 2_667 . . . ? Na1 Na1 O1 C28 -17.7(2) 2_667 . . . ? N1 Na1 O2 C29 -89.8(3) 2_667 . . . ? O1 Na1 O2 C29 19.6(3) . . . . ? Se1 Na1 O2 C29 152.7(3) . . . . ? Se1 Na1 O2 C29 3.6(6) 2_667 . . . ? P1 Na1 O2 C29 -80.5(3) 2_667 . . . ? Na1 Na1 O2 C29 147.4(2) 2_667 . . . ? N1 Na1 O2 C32 115.4(2) 2_667 . . . ? O1 Na1 O2 C32 -135.2(2) . . . . ? Se1 Na1 O2 C32 -2.1(2) . . . . ? Se1 Na1 O2 C32 -151.2(4) 2_667 . . . ? P1 Na1 O2 C32 124.7(2) 2_667 . . . ? Na1 Na1 O2 C32 -7.4(3) 2_667 . . . ? Na1 Se1 P1 N1 -69.06(8) . . . . ? Na1 Se1 P1 N1 3.55(8) 2_667 . . . ? Na1 Se1 P1 C19 57.36(9) . . . . ? Na1 Se1 P1 C19 129.97(9) 2_667 . . . ? Na1 Se1 P1 C13 167.17(8) . . . . ? Na1 Se1 P1 C13 -120.22(8) 2_667 . . . ? Na1 Se1 P1 Na1 -72.61(4) . . . 2_667 ? C19 P1 N1 C1 36.4(2) . . . . ? C13 P1 N1 C1 -78.00(19) . . . . ? Se1 P1 N1 C1 162.29(14) . . . . ? Na1 P1 N1 C1 166.9(2) 2_667 . . . ? C19 P1 N1 Na1 -130.46(10) . . . 2_667 ? C13 P1 N1 Na1 115.12(10) . . . 2_667 ? Se1 P1 N1 Na1 -4.59(10) . . . 2_667 ? P1 N1 C1 C2 -108.71(19) . . . . ? Na1 N1 C1 C2 54.5(2) 2_667 . . . ? P1 N1 C1 C8 127.52(17) . . . . ? Na1 N1 C1 C8 -69.3(2) 2_667 . . . ? N1 C1 C2 C3 112.7(2) . . . . ? C8 C1 C2 C3 -123.1(2) . . . . ? N1 C1 C2 C7 -65.9(3) . . . . ? C8 C1 C2 C7 58.3(3) . . . . ? C7 C2 C3 C4 -0.2(4) . . . . ? C1 C2 C3 C4 -178.8(2) . . . . ? C2 C3 C4 C5 -0.2(4) . . . . ? C3 C4 C5 C6 1.0(4) . . . . ? C4 C5 C6 C7 -1.3(4) . . . . ? C5 C6 C7 C2 0.9(4) . . . . ? C3 C2 C7 C6 -0.1(4) . . . . ? C1 C2 C7 C6 178.5(2) . . . . ? N1 C1 C8 C33 10.0(3) . . . . ? C2 C1 C8 C33 -112.8(2) . . . . ? N1 C1 C8 C9 -169.7(2) . . . . ? C2 C1 C8 C9 67.5(3) . . . . ? C33 C8 C9 C10 -1.1(4) . . . . ? C1 C8 C9 C10 178.6(2) . . . . ? C8 C9 C10 C11 0.5(4) . . . . ? C9 C10 C11 C12 0.5(4) . . . . ? C10 C11 C12 C33 -0.9(4) . . . . ? N1 P1 C13 C18 4.2(2) . . . . ? C19 P1 C13 C18 -116.6(2) . . . . ? Se1 P1 C13 C18 126.65(18) . . . . ? Na1 P1 C13 C18 54.6(2) 2_667 . . . ? N1 P1 C13 C14 -175.79(18) . . . . ? C19 P1 C13 C14 63.3(2) . . . . ? Se1 P1 C13 C14 -53.4(2) . . . . ? Na1 P1 C13 C14 -125.38(17) 2_667 . . . ? C18 C13 C14 C15 -1.2(4) . . . . ? P1 C13 C14 C15 178.79(19) . . . . ? C13 C14 C15 C16 1.0(4) . . . . ? C14 C15 C16 C17 -0.6(4) . . . . ? C15 C16 C17 C18 0.4(4) . . . . ? C16 C17 C18 C13 -0.7(4) . . . . ? C14 C13 C18 C17 1.1(4) . . . . ? P1 C13 C18 C17 -178.90(19) . . . . ? N1 P1 C19 C24 -91.1(2) . . . . ? C13 P1 C19 C24 30.4(2) . . . . ? Se1 P1 C19 C24 143.27(18) . . . . ? Na1 P1 C19 C24 -139.53(17) 2_667 . . . ? N1 P1 C19 C20 84.6(2) . . . . ? C13 P1 C19 C20 -154.0(2) . . . . ? Se1 P1 C19 C20 -41.1(2) . . . . ? Na1 P1 C19 C20 36.1(3) 2_667 . . . ? C24 C19 C20 C21 0.7(4) . . . . ? P1 C19 C20 C21 -175.1(2) . . . . ? C19 C20 C21 C22 -0.7(5) . . . . ? C20 C21 C22 C23 0.4(5) . . . . ? C21 C22 C23 C24 -0.2(5) . . . . ? C22 C23 C24 C19 0.2(4) . . . . ? C20 C19 C24 C23 -0.5(4) . . . . ? P1 C19 C24 C23 175.3(2) . . . . ? C28 O1 C25 C26 17.9(3) . . . . ? Na1 O1 C25 C26 -118.8(2) . . . . ? O1 C25 C26 C27 -31.5(3) . . . . ? C25 C26 C27 C28 33.3(3) . . . . ? C25 O1 C28 C27 3.9(4) . . . . ? Na1 O1 C28 C27 139.7(2) . . . . ? C26 C27 C28 O1 -23.4(4) . . . . ? C32 O2 C29 C30A -4.8(10) . . . . ? Na1 O2 C29 C30A -164.0(9) . . . . ? C32 O2 C29 C30B 32.7(10) . . . . ? Na1 O2 C29 C30B -126.5(9) . . . . ? C30B C29 C30A C31 -64.2(10) . . . . ? O2 C29 C30A C31 30.8(11) . . . . ? C30A C29 C30B C31 73.9(12) . . . . ? O2 C29 C30B C31 -23.1(14) . . . . ? C29 C30B C31 C32 5.8(14) . . . . ? C29 C30B C31 C30A -67.4(8) . . . . ? C29 C30A C31 C32 -45.2(10) . . . . ? C29 C30A C31 C30B 67.7(8) . . . . ? C29 O2 C32 C31 -28.0(4) . . . . ? Na1 O2 C32 C31 130.1(3) . . . . ? C30B C31 C32 O2 13.4(9) . . . . ? C30A C31 C32 O2 43.5(6) . . . . ? C9 C8 C33 C12 0.7(4) . . . . ? C1 C8 C33 C12 -179.0(2) . . . . ? C11 C12 C33 C8 0.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 70.74 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.337 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.060 data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 903854' #TrackingRef 'exp_877.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H58 N2 O2 P2 Se2 Sr, 2(C4 H8 O)' _chemical_formula_sum 'C66 H74 N2 O4 P2 Se2 Sr' _chemical_formula_weight 1266.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 10.191(5) _cell_length_b 10.912(5) _cell_length_c 14.641(5) _cell_angle_alpha 99.369(5) _cell_angle_beta 101.195(5) _cell_angle_gamma 103.621(5) _cell_volume 1514.7(11) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4909 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 25.79 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 2.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.51136 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _exptl_special_details ; Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10504 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.79 _reflns_number_total 5692 _reflns_number_gt 5024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III & Olex 2.1' _computing_publication_material WinGX _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^)+(0.0496P)^2^+2.5163P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5692 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.5000 0.0000 0.0000 0.02723(13) Uani 1 2 d S . . Se1 Se 0.34337(4) -0.10138(4) 0.14894(3) 0.03531(12) Uani 1 1 d . . . P1 P 0.49265(9) 0.07210(8) 0.23526(6) 0.02406(19) Uani 1 1 d . . . O1 O 0.6891(3) -0.1111(3) 0.0519(2) 0.0396(6) Uani 1 1 d . . . C51 C 0.0761(8) -0.3296(7) 0.4657(5) 0.090(2) Uani 1 1 d . . . H51A H 0.1152 -0.2630 0.5238 0.108 Uiso 1 1 calc R . . H51B H -0.0096 -0.3856 0.4717 0.108 Uiso 1 1 calc R . . N1 N 0.5656(3) 0.1544(3) 0.1678(2) 0.0269(6) Uani 1 1 d . . . C1 C 0.6621(3) 0.2829(3) 0.2143(2) 0.0281(7) Uani 1 1 d . . . H6 H 0.7061 0.2799 0.2793 0.034 Uiso 1 1 calc R . . C23 C 0.8133(4) -0.0525(4) 0.4418(3) 0.0351(8) Uani 1 1 d . . . H7 H 0.8777 -0.0790 0.4826 0.042 Uiso 1 1 calc R . . C25 C 0.7506(4) 0.0308(3) 0.3024(3) 0.0322(8) Uani 1 1 d . . . H8 H 0.7736 0.0600 0.2497 0.039 Uiso 1 1 calc R . . C2 C 0.7763(4) 0.3103(3) 0.1600(3) 0.0323(8) Uani 1 1 d . . . C7 C 0.7487(4) 0.3391(4) 0.0709(3) 0.0375(8) Uani 1 1 d . . . H10 H 0.6601 0.3440 0.0440 0.045 Uiso 1 1 calc R . . C20 C 0.6200(4) 0.0275(3) 0.3200(2) 0.0269(7) Uani 1 1 d . . . C8 C 0.5917(4) 0.3920(3) 0.2205(3) 0.0324(8) Uani 1 1 d . . . C22 C 0.6841(4) -0.0561(4) 0.4596(3) 0.0344(8) Uani 1 1 d . . . H13 H 0.6618 -0.0850 0.5126 0.041 Uiso 1 1 calc R . . C21 C 0.5879(4) -0.0170(3) 0.3991(3) 0.0306(7) Uani 1 1 d . . . H14 H 0.5011 -0.0205 0.4112 0.037 Uiso 1 1 calc R . . C15 C 0.4957(4) 0.2552(3) 0.3940(3) 0.0370(8) Uani 1 1 d . . . H15 H 0.5911 0.2657 0.4097 0.044 Uiso 1 1 calc R . . C24 C 0.8464(4) -0.0096(4) 0.3634(3) 0.0347(8) Uani 1 1 d . . . H16 H 0.9330 -0.0076 0.3513 0.042 Uiso 1 1 calc R . . C26 C 0.6733(4) -0.2187(4) 0.0994(3) 0.0432(9) Uani 1 1 d . . . H17A H 0.6086 -0.2958 0.0568 0.052 Uiso 1 1 calc R . . H17B H 0.6386 -0.1989 0.1557 0.052 Uiso 1 1 calc R . . C19 C 0.2703(4) 0.1481(4) 0.2919(3) 0.0410(9) Uani 1 1 d . . . H18 H 0.2126 0.0860 0.2393 0.049 Uiso 1 1 calc R . . C6 C 0.8523(5) 0.3610(4) 0.0212(3) 0.0446(10) Uani 1 1 d . . . H19 H 0.8329 0.3800 -0.0388 0.054 Uiso 1 1 calc R . . C29 C 0.8275(4) -0.0798(5) 0.0365(4) 0.0517(11) Uani 1 1 d . . . H20A H 0.8613 0.0120 0.0396 0.062 Uiso 1 1 calc R . . H20B H 0.8285 -0.1271 -0.0254 0.062 Uiso 1 1 calc R . . C14 C 0.4129(4) 0.1630(3) 0.3138(3) 0.0311(8) Uani 1 1 d . . . C9 C 0.4638(4) 0.3809(4) 0.1620(3) 0.0422(9) Uani 1 1 d . . . H22 H 0.4158 0.3035 0.1188 0.051 Uiso 1 1 calc R . . C10 C 0.6598(5) 0.5079(4) 0.2853(3) 0.0471(10) Uani 1 1 d . . . H23 H 0.7456 0.5167 0.3257 0.056 Uiso 1 1 calc R . . C28 C 0.9149(5) -0.1189(5) 0.1147(3) 0.0546(12) Uani 1 1 d . . . H24A H 0.9456 -0.0520 0.1728 0.066 Uiso 1 1 calc R . . H24B H 0.9956 -0.1381 0.0964 0.066 Uiso 1 1 calc R . . O3 O 0.1719(5) -0.4021(5) 0.4508(4) 0.0882(13) Uani 1 1 d . . . C11 C 0.6016(6) 0.6112(4) 0.2908(4) 0.0586(13) Uani 1 1 d . . . H26 H 0.6482 0.6881 0.3351 0.070 Uiso 1 1 calc R . . C3 C 0.9091(4) 0.3060(5) 0.1994(3) 0.0500(11) Uani 1 1 d . . . H27 H 0.9297 0.2891 0.2600 0.060 Uiso 1 1 calc R . . C18 C 0.2139(5) 0.2269(5) 0.3491(4) 0.0528(12) Uani 1 1 d . . . H28 H 0.1185 0.2172 0.3341 0.063 Uiso 1 1 calc R . . C27 C 0.8161(6) -0.2387(6) 0.1269(4) 0.0678(16) Uani 1 1 d . . . H29A H 0.8222 -0.3153 0.0857 0.081 Uiso 1 1 calc R . . H29B H 0.8371 -0.2480 0.1925 0.081 Uiso 1 1 calc R . . C17 C 0.2984(6) 0.3189(5) 0.4278(4) 0.0544(12) Uani 1 1 d . . . H30 H 0.2604 0.3717 0.4650 0.065 Uiso 1 1 calc R . . C16 C 0.4389(5) 0.3319(4) 0.4509(3) 0.0486(11) Uani 1 1 d . . . H31 H 0.4959 0.3921 0.5048 0.058 Uiso 1 1 calc R . . C4 C 1.0123(5) 0.3268(5) 0.1498(4) 0.0617(14) Uani 1 1 d . . . H32 H 1.1010 0.3219 0.1765 0.074 Uiso 1 1 calc R . . C5 C 0.9833(5) 0.3544(4) 0.0613(4) 0.0520(11) Uani 1 1 d . . . H33 H 1.0527 0.3688 0.0282 0.062 Uiso 1 1 calc R . . C12 C 0.4754(6) 0.5999(4) 0.2311(4) 0.0585(14) Uani 1 1 d . . . H34 H 0.4371 0.6694 0.2338 0.070 Uiso 1 1 calc R . . C13 C 0.4062(5) 0.4849(5) 0.1673(4) 0.0551(12) Uani 1 1 d . . . H35 H 0.3202 0.4765 0.1272 0.066 Uiso 1 1 calc R . . C30 C 0.0480(7) -0.2701(7) 0.3825(6) 0.093(2) Uani 1 1 d . . . H39A H 0.0893 -0.1773 0.4007 0.111 Uiso 1 1 calc R . . H39B H -0.0514 -0.2871 0.3574 0.111 Uiso 1 1 calc R . . C31 C 0.1118(9) -0.3303(8) 0.3094(6) 0.106(3) Uani 1 1 d . . . H43A H 0.1534 -0.2679 0.2757 0.127 Uiso 1 1 calc R . . H43B H 0.0443 -0.4029 0.2637 0.127 Uiso 1 1 calc R . . C32 C 0.2207(8) -0.3732(8) 0.3719(5) 0.092(2) Uani 1 1 d . . . H11A H 0.2374 -0.4490 0.3366 0.110 Uiso 1 1 calc R . . H11B H 0.3074 -0.3050 0.3926 0.110 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 Sr1 0.0294(2) 0.0300(2) 0.0233(2) 0.00610(17) 0.00632(17) 0.01001(18) Se1 0.0338(2) 0.0311(2) 0.0377(2) 0.00804(15) 0.00742(16) 0.00328(15) P1 0.0248(4) 0.0234(4) 0.0255(4) 0.0065(3) 0.0076(3) 0.0073(3) O1 0.0336(14) 0.0497(16) 0.0417(15) 0.0172(13) 0.0107(12) 0.0170(12) C51 0.089(5) 0.099(5) 0.089(5) 0.003(4) 0.027(4) 0.043(4) N1 0.0286(14) 0.0238(14) 0.0281(14) 0.0060(11) 0.0070(12) 0.0068(11) C1 0.0257(17) 0.0281(17) 0.0290(17) 0.0068(14) 0.0050(14) 0.0055(13) C23 0.0372(19) 0.0340(19) 0.0329(19) 0.0075(15) 0.0006(15) 0.0137(16) C25 0.0348(19) 0.0345(19) 0.0313(18) 0.0091(15) 0.0129(15) 0.0117(15) C2 0.0298(18) 0.0258(17) 0.040(2) 0.0069(15) 0.0117(15) 0.0038(14) C7 0.0322(19) 0.039(2) 0.035(2) 0.0046(16) 0.0071(16) 0.0019(16) C20 0.0290(17) 0.0251(16) 0.0250(16) 0.0038(13) 0.0050(13) 0.0069(13) C8 0.039(2) 0.0272(17) 0.0337(19) 0.0084(14) 0.0161(16) 0.0069(15) C22 0.043(2) 0.0348(19) 0.0306(18) 0.0122(15) 0.0122(16) 0.0136(16) C21 0.0321(18) 0.0306(18) 0.0332(18) 0.0088(14) 0.0127(15) 0.0117(14) C15 0.046(2) 0.0266(18) 0.043(2) 0.0088(16) 0.0206(18) 0.0104(16) C24 0.0286(18) 0.041(2) 0.038(2) 0.0105(16) 0.0094(15) 0.0134(16) C26 0.043(2) 0.043(2) 0.044(2) 0.0118(18) 0.0074(18) 0.0118(18) C19 0.040(2) 0.052(2) 0.041(2) 0.0203(18) 0.0135(17) 0.0234(19) C6 0.054(3) 0.037(2) 0.038(2) 0.0057(17) 0.0190(19) -0.0023(18) C29 0.035(2) 0.063(3) 0.064(3) 0.024(2) 0.017(2) 0.015(2) C14 0.039(2) 0.0301(18) 0.0340(18) 0.0166(15) 0.0177(16) 0.0146(15) C9 0.038(2) 0.034(2) 0.055(3) 0.0102(18) 0.0116(19) 0.0111(17) C10 0.054(3) 0.032(2) 0.050(2) 0.0030(18) 0.012(2) 0.0057(18) C28 0.037(2) 0.080(3) 0.052(3) 0.012(2) 0.011(2) 0.026(2) O3 0.089(3) 0.093(3) 0.109(4) 0.040(3) 0.044(3) 0.046(3) C11 0.083(4) 0.026(2) 0.070(3) 0.003(2) 0.035(3) 0.011(2) C3 0.038(2) 0.065(3) 0.056(3) 0.031(2) 0.015(2) 0.016(2) C18 0.053(3) 0.070(3) 0.062(3) 0.035(3) 0.030(2) 0.042(2) C27 0.066(3) 0.089(4) 0.083(4) 0.047(3) 0.039(3) 0.052(3) C17 0.083(4) 0.048(3) 0.060(3) 0.024(2) 0.042(3) 0.043(3) C16 0.072(3) 0.031(2) 0.052(3) 0.0096(18) 0.032(2) 0.016(2) C4 0.036(2) 0.075(3) 0.088(4) 0.042(3) 0.024(2) 0.018(2) C5 0.045(2) 0.049(3) 0.066(3) 0.013(2) 0.032(2) 0.006(2) C12 0.076(3) 0.036(2) 0.089(4) 0.027(2) 0.051(3) 0.029(2) C13 0.047(3) 0.048(3) 0.083(4) 0.027(2) 0.023(2) 0.023(2) C30 0.072(4) 0.071(4) 0.116(6) -0.009(4) -0.007(4) 0.029(3) C31 0.108(6) 0.112(6) 0.125(7) 0.050(5) 0.040(5) 0.055(5) C32 0.089(5) 0.113(6) 0.102(5) 0.041(5) 0.048(4) 0.049(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sr1 O1 2.567(3) . ? Sr1 O1 2.567(3) 2_655 ? Sr1 N1 2.609(3) . ? Sr1 N1 2.609(3) 2_655 ? Sr1 Se1 3.1355(9) 2_655 ? Sr1 Se1 3.1356(9) . ? Sr1 P1 3.4255(14) . ? Sr1 P1 3.4256(14) 2_655 ? Se1 P1 2.1478(11) . ? P1 N1 1.611(3) . ? P1 C20 1.824(3) . ? P1 C14 1.827(4) . ? O1 C29 1.442(5) . ? O1 C26 1.452(5) . ? C51 O3 1.420(7) . ? C51 C30 1.482(10) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? N1 C1 1.475(4) . ? C1 C8 1.528(5) . ? C1 C2 1.532(5) . ? C1 H6 0.9800 . ? C23 C24 1.378(5) . ? C23 C22 1.385(5) . ? C23 H7 0.9300 . ? C25 C24 1.392(5) . ? C25 C20 1.398(5) . ? C25 H8 0.9300 . ? C2 C3 1.379(6) . ? C2 C7 1.382(5) . ? C7 C6 1.391(6) . ? C7 H10 0.9300 . ? C20 C21 1.392(5) . ? C8 C9 1.380(6) . ? C8 C10 1.386(5) . ? C22 C21 1.382(5) . ? C22 H13 0.9300 . ? C21 H14 0.9300 . ? C15 C16 1.384(5) . ? C15 C14 1.391(6) . ? C15 H15 0.9300 . ? C24 H16 0.9300 . ? C26 C27 1.509(6) . ? C26 H17A 0.9700 . ? C26 H17B 0.9700 . ? C19 C14 1.390(5) . ? C19 C18 1.399(6) . ? C19 H18 0.9300 . ? C6 C5 1.374(6) . ? C6 H19 0.9300 . ? C29 C28 1.493(6) . ? C29 H20A 0.9700 . ? C29 H20B 0.9700 . ? C9 C13 1.394(6) . ? C9 H22 0.9300 . ? C10 C11 1.391(6) . ? C10 H23 0.9300 . ? C28 C27 1.510(7) . ? C28 H24A 0.9700 . ? C28 H24B 0.9700 . ? O3 C32 1.395(8) . ? C11 C12 1.374(8) . ? C11 H26 0.9300 . ? C3 C4 1.387(6) . ? C3 H27 0.9300 . ? C18 C17 1.382(7) . ? C18 H28 0.9300 . ? C27 H29A 0.9700 . ? C27 H29B 0.9700 . ? C17 C16 1.373(7) . ? C17 H30 0.9300 . ? C16 H31 0.9300 . ? C4 C5 1.370(7) . ? C4 H32 0.9300 . ? C5 H33 0.9300 . ? C12 C13 1.375(7) . ? C12 H34 0.9300 . ? C13 H35 0.9300 . ? C30 C31 1.498(10) . ? C30 H39A 0.9700 . ? C30 H39B 0.9700 . ? C31 C32 1.509(9) . ? C31 H43A 0.9700 . ? C31 H43B 0.9700 . ? C32 H11A 0.9700 . ? C32 H11B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sr1 O1 180.00(10) . 2_655 ? O1 Sr1 N1 91.72(9) . . ? O1 Sr1 N1 88.28(9) 2_655 . ? O1 Sr1 N1 88.28(9) . 2_655 ? O1 Sr1 N1 91.72(9) 2_655 2_655 ? N1 Sr1 N1 180.0 . 2_655 ? O1 Sr1 Se1 89.69(7) . 2_655 ? O1 Sr1 Se1 90.31(7) 2_655 2_655 ? N1 Sr1 Se1 115.76(7) . 2_655 ? N1 Sr1 Se1 64.24(7) 2_655 2_655 ? O1 Sr1 Se1 90.31(7) . . ? O1 Sr1 Se1 89.69(7) 2_655 . ? N1 Sr1 Se1 64.23(7) . . ? N1 Sr1 Se1 115.77(7) 2_655 . ? Se1 Sr1 Se1 180.0 2_655 . ? O1 Sr1 P1 87.08(7) . . ? O1 Sr1 P1 92.92(7) 2_655 . ? N1 Sr1 P1 26.86(6) . . ? N1 Sr1 P1 153.14(6) 2_655 . ? Se1 Sr1 P1 142.11(2) 2_655 . ? Se1 Sr1 P1 37.89(2) . . ? O1 Sr1 P1 92.91(7) . 2_655 ? O1 Sr1 P1 87.08(7) 2_655 2_655 ? N1 Sr1 P1 153.14(6) . 2_655 ? N1 Sr1 P1 26.86(6) 2_655 2_655 ? Se1 Sr1 P1 37.89(2) 2_655 2_655 ? Se1 Sr1 P1 142.11(2) . 2_655 ? P1 Sr1 P1 180.0 . 2_655 ? P1 Se1 Sr1 78.39(4) . . ? N1 P1 C20 111.50(16) . . ? N1 P1 C14 113.66(15) . . ? C20 P1 C14 102.31(16) . . ? N1 P1 Se1 109.56(11) . . ? C20 P1 Se1 108.60(11) . . ? C14 P1 Se1 110.95(13) . . ? N1 P1 Sr1 47.02(10) . . ? C20 P1 Sr1 116.70(11) . . ? C14 P1 Sr1 140.46(12) . . ? Se1 P1 Sr1 63.72(3) . . ? C29 O1 C26 108.4(3) . . ? C29 O1 Sr1 125.9(2) . . ? C26 O1 Sr1 125.7(2) . . ? O3 C51 C30 107.9(6) . . ? O3 C51 H51A 110.1 . . ? C30 C51 H51A 110.1 . . ? O3 C51 H51B 110.1 . . ? C30 C51 H51B 110.1 . . ? H51A C51 H51B 108.4 . . ? C1 N1 P1 117.1(2) . . ? C1 N1 Sr1 136.2(2) . . ? P1 N1 Sr1 106.13(14) . . ? N1 C1 C8 113.9(3) . . ? N1 C1 C2 108.4(3) . . ? C8 C1 C2 110.3(3) . . ? N1 C1 H6 108.0 . . ? C8 C1 H6 108.0 . . ? C2 C1 H6 108.0 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H7 120.0 . . ? C22 C23 H7 120.0 . . ? C24 C25 C20 120.1(3) . . ? C24 C25 H8 119.9 . . ? C20 C25 H8 119.9 . . ? C3 C2 C7 118.8(4) . . ? C3 C2 C1 120.2(4) . . ? C7 C2 C1 121.0(3) . . ? C2 C7 C6 120.6(4) . . ? C2 C7 H10 119.7 . . ? C6 C7 H10 119.7 . . ? C21 C20 C25 118.8(3) . . ? C21 C20 P1 121.8(3) . . ? C25 C20 P1 119.3(3) . . ? C9 C8 C10 118.5(4) . . ? C9 C8 C1 122.4(3) . . ? C10 C8 C1 119.1(4) . . ? C21 C22 C23 120.2(3) . . ? C21 C22 H13 119.9 . . ? C23 C22 H13 119.9 . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H14 119.7 . . ? C20 C21 H14 119.7 . . ? C16 C15 C14 121.4(4) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C23 C24 C25 120.3(3) . . ? C23 C24 H16 119.9 . . ? C25 C24 H16 119.9 . . ? O1 C26 C27 106.3(4) . . ? O1 C26 H17A 110.5 . . ? C27 C26 H17A 110.5 . . ? O1 C26 H17B 110.5 . . ? C27 C26 H17B 110.5 . . ? H17A C26 H17B 108.7 . . ? C14 C19 C18 119.8(4) . . ? C14 C19 H18 120.1 . . ? C18 C19 H18 120.1 . . ? C5 C6 C7 119.7(4) . . ? C5 C6 H19 120.2 . . ? C7 C6 H19 120.2 . . ? O1 C29 C28 105.4(4) . . ? O1 C29 H20A 110.7 . . ? C28 C29 H20A 110.7 . . ? O1 C29 H20B 110.7 . . ? C28 C29 H20B 110.7 . . ? H20A C29 H20B 108.8 . . ? C19 C14 C15 118.5(4) . . ? C19 C14 P1 121.2(3) . . ? C15 C14 P1 120.2(3) . . ? C8 C9 C13 120.4(4) . . ? C8 C9 H22 119.8 . . ? C13 C9 H22 119.8 . . ? C8 C10 C11 121.0(5) . . ? C8 C10 H23 119.5 . . ? C11 C10 H23 119.5 . . ? C29 C28 C27 102.5(4) . . ? C29 C28 H24A 111.3 . . ? C27 C28 H24A 111.3 . . ? C29 C28 H24B 111.3 . . ? C27 C28 H24B 111.3 . . ? H24A C28 H24B 109.2 . . ? C32 O3 C51 107.9(5) . . ? C12 C11 C10 120.1(4) . . ? C12 C11 H26 119.9 . . ? C10 C11 H26 119.9 . . ? C2 C3 C4 120.8(4) . . ? C2 C3 H27 119.6 . . ? C4 C3 H27 119.6 . . ? C17 C18 C19 120.6(4) . . ? C17 C18 H28 119.7 . . ? C19 C18 H28 119.7 . . ? C26 C27 C28 105.0(4) . . ? C26 C27 H29A 110.7 . . ? C28 C27 H29A 110.7 . . ? C26 C27 H29B 110.7 . . ? C28 C27 H29B 110.7 . . ? H29A C27 H29B 108.8 . . ? C16 C17 C18 119.7(4) . . ? C16 C17 H30 120.1 . . ? C18 C17 H30 120.1 . . ? C17 C16 C15 120.0(4) . . ? C17 C16 H31 120.0 . . ? C15 C16 H31 120.0 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H32 120.1 . . ? C3 C4 H32 120.1 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H33 119.8 . . ? C6 C5 H33 119.8 . . ? C11 C12 C13 119.5(4) . . ? C11 C12 H34 120.3 . . ? C13 C12 H34 120.3 . . ? C12 C13 C9 120.6(5) . . ? C12 C13 H35 119.7 . . ? C9 C13 H35 119.7 . . ? C51 C30 C31 106.3(6) . . ? C51 C30 H39A 110.5 . . ? C31 C30 H39A 110.5 . . ? C51 C30 H39B 110.5 . . ? C31 C30 H39B 110.5 . . ? H39A C30 H39B 108.7 . . ? C30 C31 C32 100.8(6) . . ? C30 C31 H43A 111.6 . . ? C32 C31 H43A 111.6 . . ? C30 C31 H43B 111.6 . . ? C32 C31 H43B 111.6 . . ? H43A C31 H43B 109.4 . . ? O3 C32 C31 108.2(6) . . ? O3 C32 H11A 110.1 . . ? C31 C32 H11A 110.1 . . ? O3 C32 H11B 110.1 . . ? C31 C32 H11B 110.1 . . ? H11A C32 H11B 108.4 . . ? 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 O1 Sr1 Se1 P1 84.85(8) . . . . ? O1 Sr1 Se1 P1 -95.15(8) 2_655 . . . ? N1 Sr1 Se1 P1 -6.92(7) . . . . ? N1 Sr1 Se1 P1 173.08(7) 2_655 . . . ? Se1 Sr1 Se1 P1 -15(12) 2_655 . . . ? P1 Sr1 Se1 P1 180.0 2_655 . . . ? Sr1 Se1 P1 N1 10.74(11) . . . . ? Sr1 Se1 P1 C20 -111.26(12) . . . . ? Sr1 Se1 P1 C14 137.04(12) . . . . ? O1 Sr1 P1 N1 99.63(16) . . . . ? O1 Sr1 P1 N1 -80.37(16) 2_655 . . . ? N1 Sr1 P1 N1 180.0 2_655 . . . ? Se1 Sr1 P1 N1 13.89(14) 2_655 . . . ? Se1 Sr1 P1 N1 -166.11(14) . . . . ? P1 Sr1 P1 N1 101(2) 2_655 . . . ? O1 Sr1 P1 C20 4.36(14) . . . . ? O1 Sr1 P1 C20 -175.64(14) 2_655 . . . ? N1 Sr1 P1 C20 -95.27(19) . . . . ? N1 Sr1 P1 C20 84.73(19) 2_655 . . . ? Se1 Sr1 P1 C20 -81.38(13) 2_655 . . . ? Se1 Sr1 P1 C20 98.62(13) . . . . ? P1 Sr1 P1 C20 6(2) 2_655 . . . ? O1 Sr1 P1 C14 174.1(2) . . . . ? O1 Sr1 P1 C14 -5.9(2) 2_655 . . . ? N1 Sr1 P1 C14 74.5(2) . . . . ? N1 Sr1 P1 C14 -105.5(2) 2_655 . . . ? Se1 Sr1 P1 C14 88.39(19) 2_655 . . . ? Se1 Sr1 P1 C14 -91.61(19) . . . . ? P1 Sr1 P1 C14 175(2) 2_655 . . . ? O1 Sr1 P1 Se1 -94.26(8) . . . . ? O1 Sr1 P1 Se1 85.74(8) 2_655 . . . ? N1 Sr1 P1 Se1 166.11(14) . . . . ? N1 Sr1 P1 Se1 -13.89(14) 2_655 . . . ? Se1 Sr1 P1 Se1 180.0 2_655 . . . ? P1 Sr1 P1 Se1 -93(2) 2_655 . . . ? O1 Sr1 O1 C29 51(21) 2_655 . . . ? N1 Sr1 O1 C29 -95.7(3) . . . . ? N1 Sr1 O1 C29 84.3(3) 2_655 . . . ? Se1 Sr1 O1 C29 20.1(3) 2_655 . . . ? Se1 Sr1 O1 C29 -159.9(3) . . . . ? P1 Sr1 O1 C29 -122.2(3) . . . . ? P1 Sr1 O1 C29 57.8(3) 2_655 . . . ? O1 Sr1 O1 C26 -127(21) 2_655 . . . ? N1 Sr1 O1 C26 86.2(3) . . . . ? N1 Sr1 O1 C26 -93.8(3) 2_655 . . . ? Se1 Sr1 O1 C26 -158.0(3) 2_655 . . . ? Se1 Sr1 O1 C26 22.0(3) . . . . ? P1 Sr1 O1 C26 59.8(3) . . . . ? P1 Sr1 O1 C26 -120.2(3) 2_655 . . . ? C20 P1 N1 C1 -65.2(3) . . . . ? C14 P1 N1 C1 49.8(3) . . . . ? Se1 P1 N1 C1 174.5(2) . . . . ? Sr1 P1 N1 C1 -172.3(3) . . . . ? C20 P1 N1 Sr1 107.05(15) . . . . ? C14 P1 N1 Sr1 -137.95(15) . . . . ? Se1 P1 N1 Sr1 -13.20(13) . . . . ? O1 Sr1 N1 C1 90.0(3) . . . . ? O1 Sr1 N1 C1 -90.0(3) 2_655 . . . ? N1 Sr1 N1 C1 -151.0(2) 2_655 . . . ? Se1 Sr1 N1 C1 -0.5(3) 2_655 . . . ? Se1 Sr1 N1 C1 179.5(3) . . . . ? P1 Sr1 N1 C1 170.1(4) . . . . ? P1 Sr1 N1 C1 -9.9(4) 2_655 . . . ? O1 Sr1 N1 P1 -80.09(14) . . . . ? O1 Sr1 N1 P1 99.91(14) 2_655 . . . ? N1 Sr1 N1 P1 38.9(2) 2_655 . . . ? Se1 Sr1 N1 P1 -170.58(10) 2_655 . . . ? Se1 Sr1 N1 P1 9.42(10) . . . . ? P1 Sr1 N1 P1 180.0 2_655 . . . ? P1 N1 C1 C8 -88.9(3) . . . . ? Sr1 N1 C1 C8 101.8(3) . . . . ? P1 N1 C1 C2 147.9(2) . . . . ? Sr1 N1 C1 C2 -21.3(4) . . . . ? N1 C1 C2 C3 -106.9(4) . . . . ? C8 C1 C2 C3 127.9(4) . . . . ? N1 C1 C2 C7 72.9(4) . . . . ? C8 C1 C2 C7 -52.3(4) . . . . ? C3 C2 C7 C6 1.2(6) . . . . ? C1 C2 C7 C6 -178.6(3) . . . . ? C24 C25 C20 C21 -0.2(5) . . . . ? C24 C25 C20 P1 -176.5(3) . . . . ? N1 P1 C20 C21 164.9(3) . . . . ? C14 P1 C20 C21 43.1(3) . . . . ? Se1 P1 C20 C21 -74.2(3) . . . . ? Sr1 P1 C20 C21 -143.5(3) . . . . ? N1 P1 C20 C25 -18.9(3) . . . . ? C14 P1 C20 C25 -140.7(3) . . . . ? Se1 P1 C20 C25 101.9(3) . . . . ? Sr1 P1 C20 C25 32.7(3) . . . . ? N1 C1 C8 C9 -20.6(5) . . . . ? C2 C1 C8 C9 101.6(4) . . . . ? N1 C1 C8 C10 161.3(3) . . . . ? C2 C1 C8 C10 -76.6(4) . . . . ? C24 C23 C22 C21 0.1(6) . . . . ? C23 C22 C21 C20 -0.6(6) . . . . ? C25 C20 C21 C22 0.6(5) . . . . ? P1 C20 C21 C22 176.8(3) . . . . ? C22 C23 C24 C25 0.3(6) . . . . ? C20 C25 C24 C23 -0.3(6) . . . . ? C29 O1 C26 C27 8.9(5) . . . . ? Sr1 O1 C26 C27 -172.7(3) . . . . ? C2 C7 C6 C5 -0.3(6) . . . . ? C26 O1 C29 C28 -28.3(5) . . . . ? Sr1 O1 C29 C28 153.4(3) . . . . ? C18 C19 C14 C15 1.2(6) . . . . ? C18 C19 C14 P1 -174.7(3) . . . . ? C16 C15 C14 C19 -0.5(6) . . . . ? C16 C15 C14 P1 175.4(3) . . . . ? N1 P1 C14 C19 100.5(3) . . . . ? C20 P1 C14 C19 -139.2(3) . . . . ? Se1 P1 C14 C19 -23.5(3) . . . . ? Sr1 P1 C14 C19 50.2(4) . . . . ? N1 P1 C14 C15 -75.3(3) . . . . ? C20 P1 C14 C15 45.1(3) . . . . ? Se1 P1 C14 C15 160.7(3) . . . . ? Sr1 P1 C14 C15 -125.6(3) . . . . ? C10 C8 C9 C13 1.1(6) . . . . ? C1 C8 C9 C13 -177.1(4) . . . . ? C9 C8 C10 C11 -0.6(6) . . . . ? C1 C8 C10 C11 177.6(4) . . . . ? O1 C29 C28 C27 35.6(5) . . . . ? C30 C51 O3 C32 9.5(8) . . . . ? C8 C10 C11 C12 -0.5(7) . . . . ? C7 C2 C3 C4 -1.8(7) . . . . ? C1 C2 C3 C4 178.0(4) . . . . ? C14 C19 C18 C17 -0.5(6) . . . . ? O1 C26 C27 C28 13.5(5) . . . . ? C29 C28 C27 C26 -29.7(5) . . . . ? C19 C18 C17 C16 -1.0(7) . . . . ? C18 C17 C16 C15 1.7(7) . . . . ? C14 C15 C16 C17 -0.9(6) . . . . ? C2 C3 C4 C5 1.3(8) . . . . ? C3 C4 C5 C6 -0.4(8) . . . . ? C7 C6 C5 C4 -0.2(7) . . . . ? C10 C11 C12 C13 1.2(7) . . . . ? C11 C12 C13 C9 -0.8(7) . . . . ? C8 C9 C13 C12 -0.4(7) . . . . ? O3 C51 C30 C31 10.0(8) . . . . ? C51 C30 C31 C32 -23.6(8) . . . . ? C51 O3 C32 C31 -25.6(9) . . . . ? C30 C31 C32 O3 30.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.79 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.818 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.080 data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 903855' #TrackingRef 'exp_879.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H74 K2 N2 O4 P2 Se2' _chemical_formula_sum 'C66 H74 K2 N2 O4 P2 Se2' _chemical_formula_weight 1257.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 '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 triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4891(10) _cell_length_b 13.1334(10) _cell_length_c 13.4628(8) _cell_angle_alpha 67.483(6) _cell_angle_beta 84.963(6) _cell_angle_gamma 66.685(8) _cell_volume 1568.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3651 _cell_measurement_theta_min 3.5608 _cell_measurement_theta_max 70.5729 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 3.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63555 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _exptl_special_details ; Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 16.1293 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11473 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 70.72 _reflns_number_total 5891 _reflns_number_gt 4690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III & Olex 2.1' _computing_publication_material WinGX _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. Disordered carbon atoms of two coordinated tetrahydrofuran were refined with split model.C11 in one THF is splitted with site occupation factor 0.62(4).C13 and C2D are splitted with site occupation factors 0.42(10) and 0.48(4) respectively. ; _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^)+(0.0535P)^2^+0.6272P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5891 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se2A Se 0.29681(4) 0.45534(3) 0.56647(3) 0.03915(13) Uani 1 1 d . . . P P 0.39170(8) 0.31973(7) 0.50031(7) 0.03229(19) Uani 1 1 d . A . K K 0.37315(8) 0.60961(7) 0.32729(7) 0.0436(2) Uani 1 1 d . . . C1 C 0.3812(3) 0.3570(3) 0.2162(3) 0.0371(8) Uani 1 1 d . . . C2 C 0.6951(4) 0.3513(3) 0.2806(3) 0.0409(8) Uani 1 1 d . . . H H 0.6467 0.4177 0.2985 0.049 Uiso 1 1 calc R . . O1 O 0.4499(4) 0.7022(3) 0.1306(3) 0.0745(10) Uani 1 1 d . . . C2AA C 0.3318(4) 0.1241(3) 0.5145(3) 0.0395(8) Uani 1 1 d . A . H2AA H 0.4271 0.0792 0.5291 0.047 Uiso 1 1 calc R . . C3 C 0.6308(3) 0.2751(3) 0.2845(3) 0.0356(7) Uani 1 1 d . . . C7 C 0.2453(4) 0.0716(3) 0.5012(3) 0.0463(9) Uani 1 1 d . . . H7 H 0.2827 -0.0073 0.5059 0.056 Uiso 1 1 calc R . . C4 C 0.5210(4) 0.1239(3) 0.6956(3) 0.0481(9) Uani 1 1 d . A . H4 H 0.4324 0.1261 0.7131 0.058 Uiso 1 1 calc R . . C5 C 0.3829(4) 0.4572(3) 0.1303(3) 0.0431(8) Uani 1 1 d . . . H5 H 0.4491 0.4870 0.1327 0.052 Uiso 1 1 calc R . . C9AA C 0.1036(4) 0.1381(4) 0.4810(3) 0.0476(9) Uani 1 1 d . A . H9AA H 0.0454 0.1043 0.4708 0.057 Uiso 1 1 calc R . . C28 C 0.9028(4) 0.2317(4) 0.2237(3) 0.0538(10) Uani 1 1 d . . . H28 H 0.9935 0.2169 0.2036 0.065 Uiso 1 1 calc R . . C18 C 0.2817(4) 0.3136(4) 0.2114(3) 0.0502(10) Uani 1 1 d . . . H18 H 0.2786 0.2463 0.2679 0.060 Uiso 1 1 calc R . . C2BA C 0.7655(4) 0.0390(4) 0.7444(3) 0.0521(10) Uani 1 1 d . A . H2BA H 0.8408 -0.0149 0.7945 0.063 Uiso 1 1 calc R . . C4BA C 0.8301(4) 0.3295(3) 0.2504(3) 0.0450(9) Uani 1 1 d . . . H4BA H 0.8716 0.3810 0.2482 0.054 Uiso 1 1 calc R . . C6BA C 0.2888(4) 0.5138(4) 0.0414(3) 0.0508(10) Uani 1 1 d . . . H6BA H 0.2916 0.5811 -0.0154 0.061 Uiso 1 1 calc R . . C6 C 0.1901(4) 0.4696(4) 0.0373(4) 0.0607(12) Uani 1 1 d . . . H6 H 0.1265 0.5066 -0.0224 0.073 Uiso 1 1 calc R . . O7 O 0.1109(4) 0.7113(3) 0.2369(4) 0.0929(13) Uani 1 1 d . . . C8 C 0.8405(4) 0.1551(4) 0.2266(4) 0.0546(10) Uani 1 1 d . . . H8 H 0.8893 0.0891 0.2083 0.066 Uiso 1 1 calc R . . C16 C 0.6333(4) 0.0431(4) 0.7688(3) 0.0576(11) Uani 1 1 d . . . H16 H 0.6200 -0.0089 0.8348 0.069 Uiso 1 1 calc R . . C9 C 0.5852(5) 0.7015(4) 0.1233(4) 0.0665(12) Uani 1 1 d . A . H9A H 0.6494 0.6323 0.1092 0.080 Uiso 1 1 calc R . . H9B H 0.6176 0.6983 0.1902 0.080 Uiso 1 1 calc R . . C10 C 0.1870(4) 0.3707(5) 0.1221(4) 0.0629(12) Uani 1 1 d . . . H10 H 0.1203 0.3415 0.1197 0.076 Uiso 1 1 calc R . . C11A C 0.396(2) 0.7566(15) 0.0204(11) 0.069(4) Uani 0.62(4) 1 d P A 1 H11A H 0.2953 0.7889 0.0156 0.083 Uiso 0.62(4) 1 calc PR A 1 H11B H 0.4296 0.6981 -0.0131 0.083 Uiso 0.62(4) 1 calc PR A 1 C11B C 0.351(2) 0.806(3) 0.0392(14) 0.066(6) Uani 0.38(4) 1 d P A 2 H11C H 0.3001 0.7799 0.0041 0.079 Uiso 0.38(4) 1 calc PR A 2 H11D H 0.2846 0.8661 0.0643 0.079 Uiso 0.38(4) 1 calc PR A 2 C12 C 0.4459(7) 0.8532(5) -0.0336(5) 0.094(2) Uani 1 1 d . . . H12A H 0.3776 0.9292 -0.0339 0.113 Uiso 1 1 calc R A 1 H12B H 0.4648 0.8610 -0.1074 0.113 Uiso 1 1 calc R A 1 C13A C -0.012(5) 0.828(4) 0.199(4) 0.135(14) Uani 0.42(10) 1 d P A 1 H13A H -0.0361 0.8610 0.2550 0.162 Uiso 0.42(10) 1 calc PR A 1 H13B H 0.0054 0.8857 0.1350 0.162 Uiso 0.42(10) 1 calc PR A 1 C13B C 0.014(3) 0.821(2) 0.167(5) 0.174(16) Uani 0.58(10) 1 d P A 2 H13C H -0.0484 0.8638 0.2087 0.209 Uiso 0.58(10) 1 calc PR A 2 H13D H 0.0616 0.8701 0.1219 0.209 Uiso 0.58(10) 1 calc PR A 2 C2DA C -0.1185(14) 0.800(2) 0.178(3) 0.105(9) Uani 0.48(4) 1 d P A 1 H2D1 H -0.1659 0.8563 0.1077 0.126 Uiso 0.48(4) 1 calc PR A 1 H2D2 H -0.1859 0.8055 0.2316 0.126 Uiso 0.48(4) 1 calc PR A 1 C2DB C -0.063(6) 0.801(3) 0.103(4) 0.19(2) Uani 0.52(4) 1 d P A 2 H2D3 H -0.0180 0.7970 0.0376 0.233 Uiso 0.52(4) 1 calc PR A 2 H2D4 H -0.1567 0.8625 0.0838 0.233 Uiso 0.52(4) 1 calc PR A 2 N N 0.4367(3) 0.3717(2) 0.3818(2) 0.0356(6) Uani 1 1 d . . . C14 C 0.2774(3) 0.2424(3) 0.5060(3) 0.0341(7) Uani 1 1 d . . . C15 C 0.7052(4) 0.1772(3) 0.2568(3) 0.0424(8) Uani 1 1 d . . . H15 H 0.6639 0.1256 0.2585 0.051 Uiso 1 1 calc R . . C17 C 0.5770(5) 0.8154(4) 0.0319(4) 0.0664(12) Uani 1 1 d . A . H17A H 0.5712 0.8759 0.0586 0.080 Uiso 1 1 calc R . . H17B H 0.6573 0.8009 -0.0103 0.080 Uiso 1 1 calc R . . C19 C 0.0563(5) 0.6233(5) 0.2576(5) 0.0766(14) Uani 1 1 d . A . H19A H 0.0269 0.6005 0.3304 0.092 Uiso 1 1 calc R . . H19B H 0.1256 0.5524 0.2490 0.092 Uiso 1 1 calc R . . C1A C 0.4818(3) 0.2973(3) 0.3166(3) 0.0349(7) Uani 1 1 d . A . H1A H 0.4773 0.2195 0.3596 0.042 Uiso 1 1 calc R . . C1B C 0.5379(3) 0.2023(3) 0.5959(3) 0.0354(7) Uani 1 1 d . . . C1C C 0.6721(3) 0.1959(3) 0.5716(3) 0.0387(8) Uani 1 1 d . . . H1C H 0.6863 0.2461 0.5048 0.046 Uiso 1 1 calc R . . C1D C 0.0486(4) 0.2539(4) 0.4759(3) 0.0487(9) Uani 1 1 d . . . H1D H -0.0472 0.2973 0.4644 0.058 Uiso 1 1 calc R A . C1E C 0.1341(4) 0.3067(3) 0.4878(3) 0.0421(8) Uani 1 1 d . A . H1E H 0.0956 0.3855 0.4835 0.050 Uiso 1 1 calc R . . C1F C 0.7857(4) 0.1145(3) 0.6466(3) 0.0456(9) Uani 1 1 d . . . H1F H 0.8747 0.1115 0.6301 0.055 Uiso 1 1 calc R A . C1G C -0.0631(6) 0.6787(6) 0.1783(6) 0.104(2) Uani 1 1 d . . . H1GA H -0.0344 0.6774 0.1082 0.124 Uiso 1 1 calc R A 1 H1GB H -0.1292 0.6409 0.2023 0.124 Uiso 1 1 calc R A 1 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 Se2A 0.0383(2) 0.0364(2) 0.0435(2) -0.01945(17) 0.00366(15) -0.01151(16) P 0.0302(4) 0.0306(4) 0.0360(5) -0.0135(4) 0.0026(3) -0.0110(3) K 0.0475(4) 0.0357(4) 0.0459(5) -0.0129(4) -0.0005(3) -0.0163(3) C1 0.0326(17) 0.043(2) 0.0366(19) -0.0182(16) 0.0049(14) -0.0129(15) C2 0.0407(19) 0.042(2) 0.041(2) -0.0166(17) 0.0039(15) -0.0170(16) O1 0.094(3) 0.087(2) 0.0491(19) -0.0078(17) -0.0010(17) -0.059(2) C2AA 0.0339(17) 0.038(2) 0.046(2) -0.0155(17) 0.0031(15) -0.0147(15) C3 0.0356(17) 0.0337(18) 0.0325(18) -0.0093(14) -0.0009(13) -0.0112(14) C7 0.049(2) 0.038(2) 0.053(2) -0.0164(18) 0.0028(17) -0.0185(17) C4 0.0341(18) 0.048(2) 0.049(2) -0.0075(18) -0.0006(16) -0.0126(16) C5 0.0374(19) 0.050(2) 0.044(2) -0.0159(18) 0.0006(15) -0.0202(16) C9AA 0.044(2) 0.055(2) 0.054(2) -0.020(2) 0.0021(17) -0.0284(18) C28 0.0290(18) 0.056(2) 0.064(3) -0.015(2) 0.0032(17) -0.0120(17) C18 0.044(2) 0.065(3) 0.048(2) -0.018(2) 0.0043(17) -0.0317(19) C2BA 0.0367(19) 0.049(2) 0.053(2) -0.0116(19) -0.0090(17) -0.0048(17) C4BA 0.0396(19) 0.049(2) 0.044(2) -0.0112(18) -0.0015(16) -0.0205(17) C6BA 0.042(2) 0.053(2) 0.045(2) -0.0064(19) -0.0039(17) -0.0162(18) C6 0.042(2) 0.087(3) 0.049(3) -0.016(2) -0.0053(18) -0.028(2) O7 0.068(2) 0.064(2) 0.129(4) -0.020(2) -0.038(2) -0.0159(19) C8 0.037(2) 0.047(2) 0.071(3) -0.025(2) 0.0063(18) -0.0067(17) C16 0.045(2) 0.054(3) 0.048(2) 0.004(2) -0.0050(18) -0.0147(19) C9 0.083(3) 0.061(3) 0.049(3) -0.011(2) -0.002(2) -0.030(3) C10 0.047(2) 0.094(4) 0.058(3) -0.022(3) -0.0012(19) -0.043(2) C11A 0.085(9) 0.063(7) 0.059(6) -0.014(5) -0.005(5) -0.036(7) C11B 0.070(11) 0.079(14) 0.047(8) -0.022(8) -0.003(7) -0.027(10) C12 0.111(5) 0.089(4) 0.076(4) 0.005(3) -0.030(3) -0.060(4) C13A 0.19(3) 0.074(16) 0.14(3) -0.048(15) -0.088(19) -0.022(18) C13B 0.073(12) 0.051(10) 0.34(4) -0.012(16) -0.117(16) -0.003(7) C2DA 0.046(7) 0.098(13) 0.15(2) -0.059(14) -0.024(9) 0.013(7) C2DB 0.24(4) 0.137(17) 0.18(3) 0.030(18) -0.15(3) -0.10(2) N 0.0376(15) 0.0346(15) 0.0379(16) -0.0155(13) 0.0037(12) -0.0158(12) C14 0.0324(16) 0.0336(17) 0.0351(18) -0.0121(15) 0.0020(13) -0.0127(14) C15 0.0355(18) 0.039(2) 0.051(2) -0.0159(17) 0.0017(15) -0.0136(15) C17 0.082(3) 0.063(3) 0.056(3) -0.018(2) 0.008(2) -0.034(3) C19 0.066(3) 0.067(3) 0.088(4) -0.025(3) 0.009(3) -0.023(3) C1A 0.0356(17) 0.0361(18) 0.0321(17) -0.0094(14) 0.0033(13) -0.0168(14) C1B 0.0337(17) 0.0342(18) 0.0395(19) -0.0166(15) 0.0003(14) -0.0116(14) C1C 0.0351(17) 0.041(2) 0.041(2) -0.0163(16) 0.0049(14) -0.0160(15) C1D 0.0294(17) 0.053(2) 0.065(3) -0.022(2) -0.0015(16) -0.0175(16) C1E 0.0371(18) 0.0357(19) 0.048(2) -0.0141(17) 0.0025(15) -0.0109(15) C1F 0.0308(18) 0.049(2) 0.055(2) -0.0216(19) 0.0015(16) -0.0118(16) C1G 0.073(4) 0.099(5) 0.128(6) -0.026(4) -0.016(4) -0.034(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se2A P 2.1476(9) . ? Se2A K 3.3090(10) . ? Se2A K 3.5150(9) 2_666 ? P N 1.589(3) . ? P C1B 1.827(3) . ? P C14 1.834(3) . ? P K 3.5579(12) . ? K O1 2.659(3) . ? K O7 2.695(3) . ? K N 2.725(3) . ? K C1C 3.194(3) 2_666 ? K C19 3.450(5) . ? K C1B 3.463(3) 2_666 ? K C1F 3.482(4) 2_666 ? K Se2A 3.5150(9) 2_666 ? K C9 3.530(5) . ? K K 4.7802(17) 2_666 ? C1 C5 1.385(5) . ? C1 C18 1.389(5) . ? C1 C1A 1.529(5) . ? C2 C4BA 1.385(5) . ? C2 C3 1.395(5) . ? C2 H 0.9300 . ? O1 C9 1.411(6) . ? O1 C11A 1.430(12) . ? O1 C11B 1.51(2) . ? C2AA C14 1.388(5) . ? C2AA C7 1.395(5) . ? C2AA H2AA 0.9300 . ? C3 C15 1.388(5) . ? C3 C1A 1.528(4) . ? C7 C9AA 1.381(5) . ? C7 H7 0.9300 . ? C4 C16 1.378(5) . ? C4 C1B 1.392(5) . ? C4 H4 0.9300 . ? C5 C6BA 1.381(5) . ? C5 H5 0.9300 . ? C9AA C1D 1.373(5) . ? C9AA H9AA 0.9300 . ? C28 C4BA 1.375(5) . ? C28 C8 1.388(6) . ? C28 H28 0.9300 . ? C18 C10 1.387(6) . ? C18 H18 0.9300 . ? C2BA C1F 1.371(6) . ? C2BA C16 1.381(6) . ? C2BA H2BA 0.9300 . ? C4BA H4BA 0.9300 . ? C6BA C6 1.387(5) . ? C6BA H6BA 0.9300 . ? C6 C10 1.371(6) . ? C6 H6 0.9300 . ? O7 C13B 1.40(2) . ? O7 C19 1.411(6) . ? O7 C13A 1.49(4) . ? C8 C15 1.388(5) . ? C8 H8 0.9300 . ? C16 H16 0.9300 . ? C9 C17 1.505(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10 0.9300 . ? C11A C12 1.469(12) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C11B C12 1.481(19) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12 C17 1.501(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13A C2DA 1.39(4) . ? C13A H13A 0.9700 . ? C13A H13B 0.9700 . ? C13B C2DB 1.39(5) . ? C13B H13C 0.9700 . ? C13B H13D 0.9700 . ? C2DA C1G 1.455(18) . ? C2DA H2D1 0.9700 . ? C2DA H2D2 0.9700 . ? C2DB C1G 1.54(2) . ? C2DB H2D3 0.9700 . ? C2DB H2D4 0.9700 . ? N C1A 1.472(4) . ? C14 C1E 1.391(4) . ? C15 H15 0.9300 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C19 C1G 1.468(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C1A H1A 0.9800 . ? C1B C1C 1.394(5) . ? C1B K 3.463(3) 2_666 ? C1C C1F 1.399(5) . ? C1C K 3.194(3) 2_666 ? C1C H1C 0.9300 . ? C1D C1E 1.383(5) . ? C1D H1D 0.9300 . ? C1E H1E 0.9300 . ? C1F K 3.482(4) 2_666 ? C1F H1F 0.9300 . ? C1G H1GA 0.9700 . ? C1G H1GB 0.9700 . ? 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 P Se2A K 78.21(3) . . ? P Se2A K 89.36(3) . 2_666 ? K Se2A K 88.88(2) . 2_666 ? N P C1B 113.08(15) . . ? N P C14 111.87(15) . . ? C1B P C14 102.56(15) . . ? N P Se2A 112.21(11) . . ? C1B P Se2A 105.96(11) . . ? C14 P Se2A 110.61(11) . . ? N P K 46.66(10) . . ? C1B P K 125.99(11) . . ? C14 P K 130.99(11) . . ? Se2A P K 65.57(3) . . ? O1 K O7 87.07(12) . . ? O1 K N 109.95(10) . . ? O7 K N 102.29(10) . . ? O1 K C1C 103.94(10) . 2_666 ? O7 K C1C 94.96(11) . 2_666 ? N K C1C 142.46(9) . 2_666 ? O1 K Se2A 171.26(8) . . ? O7 K Se2A 94.77(10) . . ? N K Se2A 61.31(6) . . ? C1C K Se2A 84.44(7) 2_666 . ? O1 K C19 98.94(12) . . ? O7 K C19 22.55(11) . . ? N K C19 80.24(11) . . ? C1C K C19 110.28(11) 2_666 . ? Se2A K C19 80.12(10) . . ? O1 K C1B 89.47(10) . 2_666 ? O7 K C1B 113.31(10) . 2_666 ? N K C1B 140.30(8) . 2_666 ? C1C K C1B 23.73(8) 2_666 2_666 ? Se2A K C1B 97.61(6) . 2_666 ? C19 K C1B 132.07(10) . 2_666 ? O1 K C1F 93.79(11) . 2_666 ? O7 K C1F 72.95(10) . 2_666 ? N K C1F 155.69(9) . 2_666 ? C1C K C1F 23.69(8) 2_666 2_666 ? Se2A K C1F 94.92(7) . 2_666 ? C19 K C1F 91.29(11) . 2_666 ? C1B K C1F 40.89(8) 2_666 2_666 ? O1 K Se2A 88.87(8) . 2_666 ? O7 K Se2A 166.95(9) . 2_666 ? N K Se2A 90.75(6) . 2_666 ? C1C K Se2A 74.00(6) 2_666 2_666 ? Se2A K Se2A 91.12(2) . 2_666 ? C19 K Se2A 169.65(9) . 2_666 ? C1B K Se2A 54.21(5) 2_666 2_666 ? C1F K Se2A 94.97(6) 2_666 2_666 ? O1 K C9 20.87(10) . . ? O7 K C9 107.38(13) . . ? N K C9 108.97(10) . . ? C1C K C9 96.96(11) 2_666 . ? Se2A K C9 157.55(8) . . ? C19 K C9 119.68(13) . . ? C1B K C9 77.27(10) 2_666 . ? C1F K C9 95.05(11) 2_666 . ? Se2A K C9 68.00(8) 2_666 . ? O1 K P 135.04(8) . . ? O7 K P 100.97(9) . . ? N K P 25.09(6) . . ? C1C K P 119.04(7) 2_666 . ? Se2A K P 36.220(17) . . ? C19 K P 79.02(9) . . ? C1B K P 125.33(6) 2_666 . ? C1F K P 130.99(7) 2_666 . ? Se2A K P 90.65(2) 2_666 . ? C9 K P 131.55(8) . . ? O1 K K 132.05(8) . 2_666 ? O7 K K 140.70(11) . 2_666 ? N K K 71.18(6) . 2_666 ? C1C K K 74.35(7) 2_666 2_666 ? Se2A K K 47.322(17) . 2_666 ? C19 K K 127.20(10) . 2_666 ? C1B K K 70.22(6) 2_666 2_666 ? C1F K K 97.07(7) 2_666 2_666 ? Se2A K K 43.797(16) 2_666 2_666 ? C9 K K 111.37(8) . 2_666 ? P K K 56.63(2) . 2_666 ? C5 C1 C18 118.4(3) . . ? C5 C1 C1A 121.6(3) . . ? C18 C1 C1A 120.0(3) . . ? C4BA C2 C3 120.9(3) . . ? C4BA C2 H 119.6 . . ? C3 C2 H 119.6 . . ? C9 O1 C11A 103.1(7) . . ? C9 O1 C11B 111.7(8) . . ? C11A O1 C11B 29.8(6) . . ? C9 O1 K 117.0(3) . . ? C11A O1 K 140.0(7) . . ? C11B O1 K 123.4(9) . . ? C14 C2AA C7 120.9(3) . . ? C14 C2AA H2AA 119.6 . . ? C7 C2AA H2AA 119.6 . . ? C15 C3 C2 118.3(3) . . ? C15 C3 C1A 119.5(3) . . ? C2 C3 C1A 122.2(3) . . ? C9AA C7 C2AA 119.3(3) . . ? C9AA C7 H7 120.3 . . ? C2AA C7 H7 120.3 . . ? C16 C4 C1B 121.1(4) . . ? C16 C4 H4 119.5 . . ? C1B C4 H4 119.5 . . ? C6BA C5 C1 121.6(4) . . ? C6BA C5 H5 119.2 . . ? C1 C5 H5 119.2 . . ? C1D C9AA C7 120.1(3) . . ? C1D C9AA H9AA 119.9 . . ? C7 C9AA H9AA 119.9 . . ? C4BA C28 C8 119.9(4) . . ? C4BA C28 H28 120.1 . . ? C8 C28 H28 120.1 . . ? C10 C18 C1 119.9(4) . . ? C10 C18 H18 120.0 . . ? C1 C18 H18 120.0 . . ? C1F C2BA C16 120.0(4) . . ? C1F C2BA H2BA 120.0 . . ? C16 C2BA H2BA 120.0 . . ? C28 C4BA C2 120.1(4) . . ? C28 C4BA H4BA 119.9 . . ? C2 C4BA H4BA 119.9 . . ? C5 C6BA C6 119.5(4) . . ? C5 C6BA H6BA 120.3 . . ? C6 C6BA H6BA 120.3 . . ? C10 C6 C6BA 119.4(4) . . ? C10 C6 H6 120.3 . . ? C6BA C6 H6 120.3 . . ? C13B O7 C19 108.0(10) . . ? C13B O7 C13A 20(3) . . ? C19 O7 C13A 105.0(18) . . ? C13B O7 K 141.3(10) . . ? C19 O7 K 110.4(3) . . ? C13A O7 K 141.6(13) . . ? C28 C8 C15 120.0(4) . . ? C28 C8 H8 120.0 . . ? C15 C8 H8 120.0 . . ? C4 C16 C2BA 120.3(4) . . ? C4 C16 H16 119.9 . . ? C2BA C16 H16 119.9 . . ? O1 C9 C17 107.0(4) . . ? O1 C9 K 42.17(19) . . ? C17 C9 K 137.3(3) . . ? O1 C9 H9A 110.3 . . ? C17 C9 H9A 110.3 . . ? K C9 H9A 108.9 . . ? O1 C9 H9B 110.3 . . ? C17 C9 H9B 110.3 . . ? K C9 H9B 71.4 . . ? H9A C9 H9B 108.6 . . ? C6 C10 C18 121.2(4) . . ? C6 C10 H10 119.4 . . ? C18 C10 H10 119.4 . . ? O1 C11A C12 106.7(8) . . ? O1 C11A H11A 110.4 . . ? C12 C11A H11A 110.4 . . ? O1 C11A H11B 110.4 . . ? C12 C11A H11B 110.4 . . ? H11A C11A H11B 108.6 . . ? C12 C11B O1 102.2(12) . . ? C12 C11B H11C 111.3 . . ? O1 C11B H11C 111.3 . . ? C12 C11B H11D 111.3 . . ? O1 C11B H11D 111.3 . . ? H11C C11B H11D 109.2 . . ? C11A C12 C11B 29.9(7) . . ? C11A C12 C17 104.5(6) . . ? C11B C12 C17 108.3(8) . . ? C11A C12 H12A 110.8 . . ? C11B C12 H12A 82.3 . . ? C17 C12 H12A 110.8 . . ? C11A C12 H12B 110.8 . . ? C11B C12 H12B 131.3 . . ? C17 C12 H12B 110.8 . . ? H12A C12 H12B 108.9 . . ? C2DA C13A O7 104(3) . . ? C2DA C13A H13A 110.9 . . ? O7 C13A H13A 110.9 . . ? C2DA C13A H13B 110.9 . . ? O7 C13A H13B 110.9 . . ? H13A C13A H13B 108.9 . . ? C2DB C13B O7 110(3) . . ? C2DB C13B H13C 109.7 . . ? O7 C13B H13C 109.7 . . ? C2DB C13B H13D 109.7 . . ? O7 C13B H13D 109.7 . . ? H13C C13B H13D 108.2 . . ? C13A C2DA C1G 110.8(19) . . ? C13A C2DA H2D1 109.5 . . ? C1G C2DA H2D1 109.5 . . ? C13A C2DA H2D2 109.5 . . ? C1G C2DA H2D2 109.5 . . ? H2D1 C2DA H2D2 108.1 . . ? C13B C2DB C1G 101(2) . . ? C13B C2DB H2D3 111.5 . . ? C1G C2DB H2D3 111.5 . . ? C13B C2DB H2D4 111.5 . . ? C1G C2DB H2D4 111.5 . . ? H2D3 C2DB H2D4 109.3 . . ? C1A N P 119.9(2) . . ? C1A N K 131.1(2) . . ? P N K 108.25(13) . . ? C2AA C14 C1E 118.7(3) . . ? C2AA C14 P 121.1(2) . . ? C1E C14 P 119.8(3) . . ? C3 C15 C8 120.8(4) . . ? C3 C15 H15 119.6 . . ? C8 C15 H15 119.6 . . ? C12 C17 C9 103.6(4) . . ? C12 C17 H17A 111.0 . . ? C9 C17 H17A 111.0 . . ? C12 C17 H17B 111.0 . . ? C9 C17 H17B 111.0 . . ? H17A C17 H17B 109.0 . . ? O7 C19 C1G 105.7(5) . . ? O7 C19 K 47.1(2) . . ? C1G C19 K 148.7(4) . . ? O7 C19 H19A 110.6 . . ? C1G C19 H19A 110.6 . . ? K C19 H19A 95.8 . . ? O7 C19 H19B 110.6 . . ? C1G C19 H19B 110.6 . . ? K C19 H19B 74.4 . . ? H19A C19 H19B 108.7 . . ? N C1A C3 112.6(3) . . ? N C1A C1 109.3(3) . . ? C3 C1A C1 110.3(3) . . ? N C1A H1A 108.2 . . ? C3 C1A H1A 108.2 . . ? C1 C1A H1A 108.2 . . ? C4 C1B C1C 118.1(3) . . ? C4 C1B P 123.0(3) . . ? C1C C1B P 118.7(3) . . ? C4 C1B K 101.0(2) . 2_666 ? C1C C1B K 67.23(18) . 2_666 ? P C1B K 96.65(12) . 2_666 ? C1B C1C C1F 120.6(3) . . ? C1B C1C K 89.0(2) . 2_666 ? C1F C1C K 89.8(2) . 2_666 ? C1B C1C H1C 119.7 . . ? C1F C1C H1C 119.7 . . ? K C1C H1C 91.2 2_666 . ? C9AA C1D C1E 120.7(3) . . ? C9AA C1D H1D 119.7 . . ? C1E C1D H1D 119.7 . . ? C1D C1E C14 120.2(3) . . ? C1D C1E H1E 119.9 . . ? C14 C1E H1E 119.9 . . ? C2BA C1F C1C 119.9(3) . . ? C2BA C1F K 101.2(2) . 2_666 ? C1C C1F K 66.50(19) . 2_666 ? C2BA C1F H1F 120.1 . . ? C1C C1F H1F 120.1 . . ? K C1F H1F 101.8 2_666 . ? C2DA C1G C19 99.2(10) . . ? C2DA C1G C2DB 43.7(17) . . ? C19 C1G C2DB 106.1(9) . . ? C2DA C1G H1GA 111.9 . . ? C19 C1G H1GA 111.9 . . ? C2DB C1G H1GA 69.5 . . ? C2DA C1G H1GB 111.9 . . ? C19 C1G H1GB 111.9 . . ? C2DB C1G H1GB 138.3 . . ? H1GA C1G H1GB 109.6 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 70.72 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.586 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.073 data_exp_915 _database_code_depnum_ccdc_archive 'CCDC 903856' #TrackingRef 'exp_915.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H26 N P Se, C4 H8 O' _chemical_formula_sum 'C35 H34 N O P Se' _chemical_formula_weight 594.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.7943 1.1372 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2406(3) _cell_length_b 13.6069(4) _cell_length_c 20.4841(6) _cell_angle_alpha 90 _cell_angle_beta 121.334(2) _cell_angle_gamma 90 _cell_volume 2914.16(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4059 _cell_measurement_theta_min 4.12 _cell_measurement_theta_max 70.78 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 2.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77660 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _exptl_special_details ; Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12004 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 70.78 _reflns_number_total 5495 _reflns_number_gt 4428 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)(compiled Oct 27 2011,15:02:11)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP III & Olex 2.1' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.1082P)^2^+5.7555P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5495 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 0.757 _refine_ls_restrained_S_all 0.757 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.12948(3) 0.57851(2) 0.85898(2) 0.03328(13) Uani 1 1 d . . . P1 P 0.07675(7) 0.71894(6) 0.80724(4) 0.02555(18) Uani 1 1 d . . . O1 O 0.9151(2) 0.72578(18) 0.57095(13) 0.0372(5) Uani 1 1 d . . . N1 N 0.1131(2) 0.75107(18) 0.74236(14) 0.0263(5) Uani 1 1 d . . . H1 H 0.0498 0.7710 0.6994 0.032 Uiso 1 1 calc R . . C1 C 0.2399(3) 0.7503(2) 0.74796(17) 0.0272(6) Uani 1 1 d . . . C2 C 0.2723(3) 0.6470(2) 0.73188(17) 0.0291(6) Uani 1 1 d . . . C3 C 0.3994(3) 0.6193(3) 0.7593(2) 0.0365(7) Uani 1 1 d . . . H3 H 0.4657 0.6617 0.7909 0.044 Uiso 1 1 calc R . . C4 C 0.4269(4) 0.5290(3) 0.7397(2) 0.0438(9) Uani 1 1 d . . . H4 H 0.5116 0.5119 0.7579 0.053 Uiso 1 1 calc R . . C5 C 0.3310(4) 0.4646(3) 0.6936(2) 0.0453(9) Uani 1 1 d . . . H5 H 0.3501 0.4041 0.6807 0.054 Uiso 1 1 calc R . . C6 C 0.2057(4) 0.4909(3) 0.6668(2) 0.0410(8) Uani 1 1 d . . . H6 H 0.1401 0.4477 0.6355 0.049 Uiso 1 1 calc R . . C7 C 0.1764(3) 0.5804(2) 0.68582(18) 0.0324(7) Uani 1 1 d . . . H7 H 0.0914 0.5964 0.6676 0.039 Uiso 1 1 calc R . . C8 C 0.2268(3) 0.8212(2) 0.68522(17) 0.0261(6) Uani 1 1 d . . . C9 C 0.3114(3) 0.8159(3) 0.65882(19) 0.0330(7) Uani 1 1 d . . . H9 H 0.3756 0.7686 0.6787 0.040 Uiso 1 1 calc R . . C10 C 0.3006(3) 0.8803(3) 0.6032(2) 0.0372(7) Uani 1 1 d . . . H10 H 0.3578 0.8755 0.5864 0.045 Uiso 1 1 calc R . . C11 C 0.2068(3) 0.9511(3) 0.57271(19) 0.0359(7) Uani 1 1 d . . . H11 H 0.1992 0.9931 0.5348 0.043 Uiso 1 1 calc R . . C12 C 0.1233(3) 0.9588(2) 0.59946(19) 0.0343(7) Uani 1 1 d . . . H12 H 0.0600 1.0068 0.5798 0.041 Uiso 1 1 calc R . . C13 C 0.1347(3) 0.8949(2) 0.65545(18) 0.0310(7) Uani 1 1 d . . . H13 H 0.0793 0.9015 0.6735 0.037 Uiso 1 1 calc R . . C14 C 0.3431(3) 0.7875(2) 0.82759(18) 0.0291(6) Uani 1 1 d . . . C15 C 0.3934(3) 0.7256(3) 0.89035(18) 0.0353(7) Uani 1 1 d . . . H15 H 0.3688 0.6600 0.8835 0.042 Uiso 1 1 calc R . . C16 C 0.4801(3) 0.7598(3) 0.9635(2) 0.0424(8) Uani 1 1 d . . . H16 H 0.5119 0.7172 1.0049 0.051 Uiso 1 1 calc R . . C17 C 0.5192(3) 0.8564(3) 0.9749(2) 0.0459(9) Uani 1 1 d . . . H17 H 0.5761 0.8796 1.0239 0.055 Uiso 1 1 calc R . . C18 C 0.4727(3) 0.9186(3) 0.9124(2) 0.0455(9) Uani 1 1 d . . . H18 H 0.5003 0.9835 0.9196 0.055 Uiso 1 1 calc R . . C19 C 0.3848(3) 0.8851(3) 0.8389(2) 0.0364(7) Uani 1 1 d . . . H19 H 0.3540 0.9277 0.7974 0.044 Uiso 1 1 calc R . . C20 C -0.0969(3) 0.7332(2) 0.75186(17) 0.0283(6) Uani 1 1 d . . . C21 C -0.1527(3) 0.8217(3) 0.71615(19) 0.0356(7) Uani 1 1 d . . . H21 H -0.1013 0.8734 0.7183 0.043 Uiso 1 1 calc R . . C22 C -0.2845(3) 0.8334(3) 0.6773(2) 0.0411(8) Uani 1 1 d . . . H22 H -0.3212 0.8929 0.6538 0.049 Uiso 1 1 calc R . . C23 C -0.3612(3) 0.7562(3) 0.6736(2) 0.0420(8) Uani 1 1 d . . . H23 H -0.4495 0.7637 0.6475 0.050 Uiso 1 1 calc R . . C24 C -0.3066(4) 0.6687(3) 0.7086(2) 0.0483(9) Uani 1 1 d . . . H24 H -0.3585 0.6169 0.7056 0.058 Uiso 1 1 calc R . . C25 C -0.1744(3) 0.6563(3) 0.7484(2) 0.0396(8) Uani 1 1 d . . . H25 H -0.1383 0.5969 0.7725 0.048 Uiso 1 1 calc R . . C26 C 0.1338(3) 0.8190(2) 0.87663(18) 0.0287(6) Uani 1 1 d . . . C27 C 0.1756(3) 0.7998(3) 0.95301(19) 0.0358(7) Uani 1 1 d . . . H27 H 0.1783 0.7356 0.9693 0.043 Uiso 1 1 calc R . . C28 C 0.2133(3) 0.8770(3) 1.00474(19) 0.0395(8) Uani 1 1 d . . . H28 H 0.2423 0.8640 1.0558 0.047 Uiso 1 1 calc R . . C29 C 0.2080(3) 0.9723(3) 0.9813(2) 0.0374(8) Uani 1 1 d . . . H29 H 0.2327 1.0235 1.0162 0.045 Uiso 1 1 calc R . . C30 C 0.1659(3) 0.9923(3) 0.9052(2) 0.0360(7) Uani 1 1 d . . . H30 H 0.1621 1.0568 0.8891 0.043 Uiso 1 1 calc R . . C31 C 0.1296(3) 0.9156(2) 0.85312(18) 0.0322(7) Uani 1 1 d . . . H31 H 0.1024 0.9289 0.8023 0.039 Uiso 1 1 calc R . . C32 C 0.8086(3) 0.7918(3) 0.5333(2) 0.0426(8) Uani 1 1 d . . . H32A H 0.8359 0.8591 0.5487 0.051 Uiso 1 1 calc R . . H32B H 0.7439 0.7754 0.5453 0.051 Uiso 1 1 calc R . . C33 C 0.7570(4) 0.7785(3) 0.4488(2) 0.0442(9) Uani 1 1 d . . . H33A H 0.7116 0.8366 0.4200 0.053 Uiso 1 1 calc R . . H33B H 0.7005 0.7221 0.4286 0.053 Uiso 1 1 calc R . . C34 C 0.8779(4) 0.7623(3) 0.4471(2) 0.0421(8) Uani 1 1 d . . . H34A H 0.8609 0.7240 0.4028 0.051 Uiso 1 1 calc R . . H34B H 0.9168 0.8242 0.4468 0.051 Uiso 1 1 calc R . . C35 C 0.9624(3) 0.7060(3) 0.52072(19) 0.0375(8) Uani 1 1 d . . . H35A H 0.9585 0.6361 0.5104 0.045 Uiso 1 1 calc R . . H35B H 1.0505 0.7274 0.5441 0.045 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 Se1 0.0380(2) 0.0259(2) 0.0374(2) 0.00360(14) 0.02067(16) -0.00001(14) P1 0.0279(4) 0.0237(4) 0.0272(4) -0.0007(3) 0.0158(3) -0.0013(3) O1 0.0387(12) 0.0381(13) 0.0365(12) 0.0032(10) 0.0208(11) 0.0021(10) N1 0.0263(12) 0.0272(13) 0.0259(12) 0.0007(10) 0.0140(10) 0.0004(10) C1 0.0261(14) 0.0290(16) 0.0282(15) -0.0010(12) 0.0153(12) -0.0001(12) C2 0.0373(16) 0.0264(15) 0.0286(15) 0.0059(12) 0.0206(13) 0.0039(13) C3 0.0383(17) 0.0355(18) 0.0406(18) 0.0046(15) 0.0240(15) 0.0063(15) C4 0.051(2) 0.042(2) 0.052(2) 0.0144(18) 0.0367(19) 0.0210(18) C5 0.071(3) 0.0294(18) 0.051(2) 0.0081(16) 0.043(2) 0.0161(18) C6 0.060(2) 0.0288(17) 0.0413(19) -0.0017(15) 0.0316(18) 0.0008(16) C7 0.0396(17) 0.0286(16) 0.0327(16) 0.0026(13) 0.0214(14) 0.0020(13) C8 0.0294(14) 0.0213(14) 0.0285(15) -0.0034(12) 0.0156(12) -0.0042(12) C9 0.0332(16) 0.0328(17) 0.0366(17) 0.0011(14) 0.0206(14) 0.0047(14) C10 0.0405(18) 0.0389(18) 0.0422(18) 0.0018(15) 0.0285(16) -0.0030(15) C11 0.0478(19) 0.0295(16) 0.0331(17) 0.0034(14) 0.0229(15) -0.0049(15) C12 0.0385(17) 0.0266(16) 0.0381(17) 0.0031(14) 0.0200(14) 0.0019(14) C13 0.0332(15) 0.0294(16) 0.0340(16) -0.0016(13) 0.0202(13) -0.0007(13) C14 0.0240(14) 0.0361(17) 0.0313(15) -0.0029(13) 0.0173(13) -0.0015(13) C15 0.0273(15) 0.045(2) 0.0325(16) 0.0022(15) 0.0148(13) -0.0025(14) C16 0.0314(17) 0.062(2) 0.0319(17) 0.0041(17) 0.0152(14) 0.0009(17) C17 0.0319(17) 0.066(3) 0.0343(18) -0.0164(18) 0.0132(15) -0.0031(18) C18 0.0364(18) 0.044(2) 0.049(2) -0.0192(18) 0.0175(17) -0.0066(16) C19 0.0331(16) 0.0373(18) 0.0382(17) -0.0070(15) 0.0182(14) -0.0015(14) C20 0.0281(15) 0.0304(16) 0.0297(15) -0.0035(12) 0.0174(13) -0.0002(13) C21 0.0345(17) 0.0366(18) 0.0377(17) 0.0004(14) 0.0201(14) -0.0017(14) C22 0.0385(18) 0.044(2) 0.0407(18) 0.0020(16) 0.0204(15) 0.0075(16) C23 0.0279(16) 0.056(2) 0.0423(19) -0.0025(17) 0.0186(15) 0.0008(16) C24 0.0363(18) 0.050(2) 0.059(2) -0.0024(19) 0.0252(18) -0.0086(17) C25 0.0357(17) 0.0329(18) 0.051(2) 0.0018(16) 0.0231(16) -0.0021(14) C26 0.0286(15) 0.0290(16) 0.0313(15) -0.0054(13) 0.0176(13) -0.0016(13) C27 0.0421(18) 0.0356(18) 0.0344(17) -0.0016(14) 0.0231(15) -0.0051(15) C28 0.0447(19) 0.047(2) 0.0310(16) -0.0060(15) 0.0228(15) -0.0046(17) C29 0.0354(17) 0.0400(19) 0.0392(18) -0.0152(15) 0.0210(15) -0.0069(15) C30 0.0385(17) 0.0266(16) 0.0424(18) -0.0054(14) 0.0207(15) -0.0016(14) C31 0.0346(16) 0.0304(17) 0.0316(16) 0.0005(13) 0.0173(14) 0.0007(13) C32 0.0321(17) 0.048(2) 0.0412(19) -0.0048(17) 0.0141(15) 0.0051(16) C33 0.0398(19) 0.044(2) 0.0377(19) -0.0030(16) 0.0126(16) -0.0017(16) C34 0.053(2) 0.0358(19) 0.0386(19) 0.0002(15) 0.0245(17) -0.0032(16) C35 0.0418(18) 0.0374(19) 0.0374(18) -0.0018(15) 0.0235(16) 0.0000(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Se1 P1 2.1166(8) . ? P1 N1 1.664(2) . ? P1 C26 1.825(3) . ? P1 C20 1.826(3) . ? O1 C32 1.434(4) . ? O1 C35 1.444(4) . ? N1 C1 1.496(4) . ? N1 H1 0.8600 . ? C1 C14 1.540(4) . ? C1 C2 1.541(4) . ? C1 C8 1.547(4) . ? C2 C7 1.392(5) . ? C2 C3 1.403(5) . ? C3 C4 1.387(5) . ? C3 H3 0.9300 . ? C4 C5 1.373(6) . ? C4 H4 0.9300 . ? C5 C6 1.380(6) . ? C5 H5 0.9300 . ? C6 C7 1.382(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.391(4) . ? C8 C9 1.397(4) . ? C9 C10 1.388(5) . ? C9 H9 0.9300 . ? C10 C11 1.375(5) . ? C10 H10 0.9300 . ? C11 C12 1.392(5) . ? C11 H11 0.9300 . ? C12 C13 1.387(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.385(5) . ? C14 C19 1.398(5) . ? C15 C16 1.390(5) . ? C15 H15 0.9300 . ? C16 C17 1.376(6) . ? C16 H16 0.9300 . ? C17 C18 1.386(6) . ? C17 H17 0.9300 . ? C18 C19 1.396(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C25 1.390(5) . ? C20 C21 1.389(5) . ? C21 C22 1.388(5) . ? C21 H21 0.9300 . ? C22 C23 1.384(5) . ? C22 H22 0.9300 . ? C23 C24 1.371(6) . ? C23 H23 0.9300 . ? C24 C25 1.392(5) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C31 1.391(5) . ? C26 C27 1.395(5) . ? C27 C28 1.390(5) . ? C27 H27 0.9300 . ? C28 C29 1.373(5) . ? C28 H28 0.9300 . ? C29 C30 1.390(5) . ? C29 H29 0.9300 . ? C30 C31 1.389(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.513(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.514(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.519(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 C26 105.83(14) . . ? N1 P1 C20 100.60(13) . . ? C26 P1 C20 104.78(14) . . ? N1 P1 Se1 119.90(10) . . ? C26 P1 Se1 112.96(11) . . ? C20 P1 Se1 111.13(11) . . ? C32 O1 C35 108.8(3) . . ? C1 N1 P1 129.4(2) . . ? C1 N1 H1 115.3 . . ? P1 N1 H1 115.3 . . ? N1 C1 C14 109.0(2) . . ? N1 C1 C2 111.3(2) . . ? C14 C1 C2 111.5(3) . . ? N1 C1 C8 106.0(2) . . ? C14 C1 C8 110.4(3) . . ? C2 C1 C8 108.5(2) . . ? C7 C2 C3 117.7(3) . . ? C7 C2 C1 121.2(3) . . ? C3 C2 C1 121.0(3) . . ? C4 C3 C2 120.5(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 121.0(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C5 C6 C7 120.9(4) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 120.9(3) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C13 C8 C9 117.6(3) . . ? C13 C8 C1 121.6(3) . . ? C9 C8 C1 120.8(3) . . ? C10 C9 C8 120.8(3) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 121.1(3) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.0(3) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C8 C13 C12 121.6(3) . . ? C8 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C15 C14 C19 118.4(3) . . ? C15 C14 C1 120.5(3) . . ? C19 C14 C1 121.1(3) . . ? C14 C15 C16 121.2(3) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 120.4(4) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 119.1(3) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 120.9(4) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C14 C19 C18 119.9(4) . . ? C14 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C25 C20 C21 119.4(3) . . ? C25 C20 P1 119.6(3) . . ? C21 C20 P1 120.9(2) . . ? C22 C21 C20 120.5(3) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 119.8(4) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.9(4) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C20 C25 C24 119.5(3) . . ? C20 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C31 C26 C27 119.4(3) . . ? C31 C26 P1 120.3(2) . . ? C27 C26 P1 120.2(3) . . ? C28 C27 C26 119.8(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 120.7(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 120.0(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C31 119.9(3) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C26 C31 C30 120.3(3) . . ? C26 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? O1 C32 C33 105.2(3) . . ? O1 C32 H32A 110.7 . . ? C33 C32 H32A 110.7 . . ? O1 C32 H32B 110.7 . . ? C33 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C32 C33 C34 102.2(3) . . ? C32 C33 H33A 111.3 . . ? C34 C33 H33A 111.3 . . ? C32 C33 H33B 111.3 . . ? C34 C33 H33B 111.3 . . ? H33A C33 H33B 109.2 . . ? C35 C34 C33 102.7(3) . . ? C35 C34 H34A 111.2 . . ? C33 C34 H34A 111.2 . . ? C35 C34 H34B 111.2 . . ? C33 C34 H34B 111.2 . . ? H34A C34 H34B 109.1 . . ? O1 C35 C34 107.2(3) . . ? O1 C35 H35A 110.3 . . ? C34 C35 H35A 110.3 . . ? O1 C35 H35B 110.3 . . ? C34 C35 H35B 110.3 . . ? H35A C35 H35B 108.5 . . ? 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 C26 P1 N1 C1 75.3(3) . . . . ? C20 P1 N1 C1 -175.9(3) . . . . ? Se1 P1 N1 C1 -53.8(3) . . . . ? P1 N1 C1 C14 -40.8(4) . . . . ? P1 N1 C1 C2 82.6(3) . . . . ? P1 N1 C1 C8 -159.6(2) . . . . ? N1 C1 C2 C7 26.9(4) . . . . ? C14 C1 C2 C7 148.8(3) . . . . ? C8 C1 C2 C7 -89.4(3) . . . . ? N1 C1 C2 C3 -157.1(3) . . . . ? C14 C1 C2 C3 -35.2(4) . . . . ? C8 C1 C2 C3 86.6(3) . . . . ? C7 C2 C3 C4 1.1(5) . . . . ? C1 C2 C3 C4 -175.1(3) . . . . ? C2 C3 C4 C5 -0.5(5) . . . . ? C3 C4 C5 C6 0.1(5) . . . . ? C4 C5 C6 C7 -0.1(5) . . . . ? C3 C2 C7 C6 -1.1(5) . . . . ? C1 C2 C7 C6 175.0(3) . . . . ? C5 C6 C7 C2 0.7(5) . . . . ? N1 C1 C8 C13 22.5(4) . . . . ? C14 C1 C8 C13 -95.5(3) . . . . ? C2 C1 C8 C13 142.1(3) . . . . ? N1 C1 C8 C9 -160.3(3) . . . . ? C14 C1 C8 C9 81.7(3) . . . . ? C2 C1 C8 C9 -40.7(4) . . . . ? C13 C8 C9 C10 -1.9(5) . . . . ? C1 C8 C9 C10 -179.2(3) . . . . ? C8 C9 C10 C11 0.1(5) . . . . ? C9 C10 C11 C12 1.2(5) . . . . ? C10 C11 C12 C13 -0.7(5) . . . . ? C9 C8 C13 C12 2.4(5) . . . . ? C1 C8 C13 C12 179.7(3) . . . . ? C11 C12 C13 C8 -1.1(5) . . . . ? N1 C1 C14 C15 79.7(3) . . . . ? C2 C1 C14 C15 -43.6(4) . . . . ? C8 C1 C14 C15 -164.3(3) . . . . ? N1 C1 C14 C19 -98.0(3) . . . . ? C2 C1 C14 C19 138.8(3) . . . . ? C8 C1 C14 C19 18.1(4) . . . . ? C19 C14 C15 C16 2.2(5) . . . . ? C1 C14 C15 C16 -175.5(3) . . . . ? C14 C15 C16 C17 -0.8(5) . . . . ? C15 C16 C17 C18 -1.1(5) . . . . ? C16 C17 C18 C19 1.6(6) . . . . ? C15 C14 C19 C18 -1.6(5) . . . . ? C1 C14 C19 C18 176.1(3) . . . . ? C17 C18 C19 C14 -0.3(5) . . . . ? N1 P1 C20 C25 127.9(3) . . . . ? C26 P1 C20 C25 -122.4(3) . . . . ? Se1 P1 C20 C25 -0.1(3) . . . . ? N1 P1 C20 C21 -55.3(3) . . . . ? C26 P1 C20 C21 54.4(3) . . . . ? Se1 P1 C20 C21 176.7(2) . . . . ? C25 C20 C21 C22 0.0(5) . . . . ? P1 C20 C21 C22 -176.8(3) . . . . ? C20 C21 C22 C23 -0.4(5) . . . . ? C21 C22 C23 C24 0.2(6) . . . . ? C22 C23 C24 C25 0.5(6) . . . . ? C21 C20 C25 C24 0.7(5) . . . . ? P1 C20 C25 C24 177.6(3) . . . . ? C23 C24 C25 C20 -0.9(6) . . . . ? N1 P1 C26 C31 34.4(3) . . . . ? C20 P1 C26 C31 -71.4(3) . . . . ? Se1 P1 C26 C31 167.5(2) . . . . ? N1 P1 C26 C27 -149.1(3) . . . . ? C20 P1 C26 C27 105.1(3) . . . . ? Se1 P1 C26 C27 -16.0(3) . . . . ? C31 C26 C27 C28 -0.4(5) . . . . ? P1 C26 C27 C28 -177.0(3) . . . . ? C26 C27 C28 C29 0.9(5) . . . . ? C27 C28 C29 C30 -0.6(5) . . . . ? C28 C29 C30 C31 -0.2(5) . . . . ? C27 C26 C31 C30 -0.4(5) . . . . ? P1 C26 C31 C30 176.1(2) . . . . ? C29 C30 C31 C26 0.7(5) . . . . ? C35 O1 C32 C33 23.4(4) . . . . ? O1 C32 C33 C34 -36.2(4) . . . . ? C32 C33 C34 C35 34.5(4) . . . . ? C32 O1 C35 C34 -0.9(4) . . . . ? C33 C34 C35 O1 -21.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 70.78 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.741 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.073