# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email cea@servidor.unam.mx _publ_contact_author_name 'Dr Raymundo Cea-Olivares' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; Institute of Chemistry National Autonomous Mexico Circuito Exterior, Ciudad Universit MEXICO CITY Federal District 04510 MEXICO ; _publ_contact_author_phone '5255 5622 4505' _publ_contact_author_fax '5255 5616 2217' _publ_section_title ; A powerful novel strategy for the preparation of discrete inorganic carbon free rings containing alkaline cations ; loop_ _publ_author_name 'Raymundo Cea-Olivares' 'Veronica Garcia-Montalvo' 'Michelle Hernandez-Arganis' ; S.Hernandez-Ortega ; 'Ruben A. Toscano' #==END data_compound8 _database_code_depnum_ccdc_archive 'CCDC 220669' _chemical_name_common '(Cs(18-crown-6)) tetraphenyldithiodimidodiphosphinate' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Cs(18-crown-6)] tetraphenyldithiodimidodiphosphinate ; _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 Cs N O6 P2 S2' _chemical_formula_weight 845.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 '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 9.136(3) _cell_length_b 20.316(3) _cell_length_c 21.355(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.37(2) _cell_angle_gamma 90.00 _cell_volume 3952.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 41 _cell_measurement_theta_min 5.00 _cell_measurement_theta_max 12.50 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.166 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_T_max 0.677 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4/PC diffractometer' _diffrn_measurement_method \w:2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3 _diffrn_reflns_number 7426 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0952 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6961 _reflns_number_gt 3329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS ver 2.1 1993' _computing_cell_refinement 'XSCANS ver 2.1 1993' _computing_data_reduction 'XSCANS ver 2.1 1993' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V 6.10' _computing_publication_material 'SHELXTL V 6.10' _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 w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+2.8180P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6961 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1596 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.2268 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.264 _refine_ls_shift/su_mean 0.018 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cs Cs 0.37534(11) -0.27304(4) 0.85038(3) 0.0955(4) Uani 1 d . . . S1 S 0.2936(6) -0.3554(2) 0.69933(16) 0.141(2) Uani 1 d . . . S2 S 0.1195(4) -0.39747(17) 0.87830(17) 0.1007(11) Uani 1 d . . . P1 P 0.1824(3) -0.43768(13) 0.70037(10) 0.0629(6) Uani 1 d . . . P2 P 0.1985(3) -0.47473(14) 0.83616(10) 0.0608(6) Uani 1 d . . . N1 N 0.1782(10) -0.4817(4) 0.7618(3) 0.079(3) Uani 1 d . . . O1 O 0.190(2) -0.1438(14) 0.8733(13) 0.254(12) Uani 1 d . . . C2 C 0.148(3) -0.1220(16) 0.8130(19) 0.37(4) Uani 1 d . . . H2A H 0.1133 -0.0780 0.8177 0.080 Uiso 1 d R . . H2B H 0.0680 -0.1485 0.7966 0.080 Uiso 1 d R . . C3 C 0.255(3) -0.1172(18) 0.7839(16) 0.36(4) Uani 1 d . . . H3A H 0.3087 -0.0780 0.7958 0.080 Uiso 1 d R . . H3B H 0.2005 -0.1060 0.7453 0.080 Uiso 1 d R . . O4 O 0.335(2) -0.1547(9) 0.7554(8) 0.195(8) Uani 1 d . . . C5 C 0.431(3) -0.1527(14) 0.7099(9) 0.200(15) Uani 1 d . . . H5A H 0.4851 -0.1130 0.7193 0.080 Uiso 1 d R . . H5B H 0.3791 -0.1470 0.6695 0.080 Uiso 1 d R . . C6 C 0.546(4) -0.1975(13) 0.7188(13) 0.226(18) Uani 1 d . . . H6A H 0.6141 -0.1859 0.6892 0.080 Uiso 1 d R . . H6B H 0.4938 -0.2357 0.7029 0.080 Uiso 1 d R . . O7 O 0.620(2) -0.2154(9) 0.7644(6) 0.179(7) Uani 1 d . . . C8 C 0.726(4) -0.2623(14) 0.7664(14) 0.30(3) Uani 1 d . . . H8A H 0.8010 -0.2488 0.7406 0.080 Uiso 1 d R . . H8B H 0.6846 -0.3025 0.7496 0.080 Uiso 1 d R . . C9 C 0.779(3) -0.2744(11) 0.8258(11) 0.192(13) Uani 1 d . . . H9A H 0.8348 -0.2359 0.8375 0.080 Uiso 1 d R . . H9B H 0.8477 -0.3097 0.8238 0.080 Uiso 1 d R . . O10 O 0.708(2) -0.2849(9) 0.8714(9) 0.229(9) Uani 1 d . . . C11 C 0.762(3) -0.2984(13) 0.9296(10) 0.189(11) Uani 1 d . . . H11A H 0.8239 -0.2615 0.9409 0.080 Uiso 1 d R . . H11B H 0.8231 -0.3366 0.9289 0.080 Uiso 1 d R . . C12 C 0.682(4) -0.299(2) 0.9755(15) 0.76(9) Uani 1 d . . . H12A H 0.7393 -0.2939 1.0149 0.080 Uiso 1 d R . . H12B H 0.6524 -0.3437 0.9729 0.080 Uiso 1 d R . . O13 O 0.5621(17) -0.2732(8) 0.9817(6) 0.163(5) Uani 1 d . . . C14 C 0.472(6) -0.251(2) 1.0093(19) 0.81(11) Uani 1 d . . . H14A H 0.5354 -0.2483 1.0472 0.080 Uiso 1 d R . . H14B H 0.4272 -0.2939 1.0095 0.080 Uiso 1 d R . . C15 C 0.386(4) -0.2424(18) 1.0322(6) 0.36(4) Uani 1 d . . . H15A H 0.4304 -0.2016 1.0458 0.080 Uiso 1 d R . . H15B H 0.3269 -0.2566 1.0644 0.080 Uiso 1 d R . . O16 O 0.285(2) -0.2143(9) 0.9813(11) 0.218(10) Uani 1 d . . . C17 C 0.184(4) -0.1780(18) 0.9793(14) 0.30(3) Uani 1 d . . . H17A H 0.2315 -0.1398 0.9977 0.080 Uiso 1 d R . . H17B H 0.1094 -0.1911 1.0055 0.080 Uiso 1 d R . . C18 C 0.147(4) -0.1427(16) 0.9223(18) 0.30(3) Uani 1 d . . . H18A H 0.0760 -0.1762 0.9120 0.080 Uiso 1 d R . . H18B H 0.0943 -0.1026 0.9265 0.080 Uiso 1 d R . . C19 C 0.2499(17) -0.4926(6) 0.6438(5) 0.101(4) Uani 1 d . . . C20 C 0.2917(15) -0.5537(7) 0.6544(5) 0.097(4) Uani 1 d . . . H20 H 0.2856 -0.5707 0.6960 0.080 Uiso 1 d R . . C21 C 0.351(2) -0.5978(8) 0.6131(7) 0.125(6) Uani 1 d . . . H21 H 0.3255 -0.6433 0.6080 0.080 Uiso 1 d R . . C22 C 0.435(3) -0.5679(16) 0.5769(15) 0.100(9) Uani 0.497(13) d P A 1 H22 H 0.5092 -0.5918 0.5577 0.080 Uiso 0.497(13) d PR A 1 C23 C 0.436(3) -0.502(2) 0.5660(13) 0.138(15) Uani 0.497(13) d P A 1 H23 H 0.4796 -0.4807 0.5319 0.080 Uiso 0.497(13) d PR A 1 C24 C 0.357(3) -0.4628(15) 0.6032(10) 0.103(10) Uani 0.497(13) d P A 1 H24 H 0.3761 -0.4166 0.6082 0.080 Uiso 0.497(13) d PR A 1 C22B C 0.291(3) -0.5866(12) 0.5455(10) 0.088(8) Uani 0.503(13) d P A 2 H22B H 0.3189 -0.6146 0.5124 0.080 Uiso 0.503(13) d PR A 2 C23B C 0.203(3) -0.5340(14) 0.5318(9) 0.102(9) Uani 0.503(13) d P A 2 H23B H 0.1682 -0.5258 0.4890 0.080 Uiso 0.503(13) d PR A 2 C24B C 0.173(3) -0.4900(11) 0.5778(9) 0.095(9) Uani 0.503(13) d P A 2 H24B H 0.1029 -0.4560 0.5686 0.080 Uiso 0.503(13) d PR A 2 C25 C -0.0006(13) -0.4204(8) 0.6717(5) 0.102(4) Uani 1 d . . . C26 C -0.1223(14) -0.4331(8) 0.6963(6) 0.107(5) Uani 1 d . . . H26 H -0.1089 -0.4552 0.7360 0.080 Uiso 1 d R . . C27 C -0.2595(16) -0.4233(9) 0.6698(8) 0.117(5) Uani 1 d . . . H27 H -0.3336 -0.4132 0.6972 0.080 Uiso 1 d R . . C28 C -0.290(4) -0.430(2) 0.600(2) 0.131(14) Uani 0.479(14) d P B 1 H28 H -0.3850 -0.4215 0.5798 0.080 Uiso 0.479(14) d PR B 1 C29 C -0.170(4) -0.4370(18) 0.5677(11) 0.127(13) Uani 0.479(14) d P B 1 H29 H -0.1871 -0.4465 0.5237 0.080 Uiso 0.479(14) d PR B 1 C30 C -0.030(3) -0.4433(14) 0.5952(11) 0.095(8) Uani 0.479(14) d P B 1 H30 H 0.0514 -0.4526 0.5717 0.080 Uiso 0.479(14) d PR B 1 C28B C -0.284(3) -0.3781(17) 0.6366(13) 0.097(9) Uani 0.521(14) d P B 2 H28B H -0.3788 -0.3778 0.6142 0.080 Uiso 0.521(14) d PR B 2 C29B C -0.168(3) -0.3417(12) 0.6173(11) 0.096(8) Uani 0.521(14) d P B 2 H29B H -0.1935 -0.3005 0.5975 0.080 Uiso 0.521(14) d PR B 2 C30B C -0.031(2) -0.3588(10) 0.6391(10) 0.077(6) Uani 0.521(14) d P B 2 H30B H 0.0480 -0.3310 0.6291 0.080 Uiso 0.521(14) d PR B 2 C31 C 0.3936(11) -0.4836(6) 0.8600(4) 0.079(3) Uani 1 d . . . C32 C 0.4978(12) -0.4616(6) 0.8253(5) 0.080(3) Uani 1 d . . . H32 H 0.4677 -0.4405 0.7862 0.080 Uiso 1 d R . . C33 C 0.6440(13) -0.4635(8) 0.8431(7) 0.104(4) Uani 1 d . . . H33 H 0.7134 -0.4424 0.8187 0.080 Uiso 1 d R . . C34 C 0.6906(17) -0.4909(11) 0.8948(9) 0.158(8) Uani 1 d . . . H34 H 0.7921 -0.4912 0.9088 0.080 Uiso 1 d R . . C35 C 0.596(2) -0.5259(12) 0.9300(8) 0.177(9) Uani 1 d . . . H35 H 0.6300 -0.5499 0.9669 0.080 Uiso 1 d R . . C36 C 0.4470(18) -0.5205(10) 0.9130(7) 0.153(8) Uani 1 d . . . H36 H 0.3772 -0.5434 0.9357 0.080 Uiso 1 d R . . C37 C 0.1163(10) -0.5483(5) 0.8664(4) 0.064(2) Uani 1 d . . . C38 C 0.0661(13) -0.5517(6) 0.9260(5) 0.082(3) Uani 1 d . . . H38 H 0.0758 -0.5135 0.9523 0.080 Uiso 1 d R . . C39 C 0.0007(15) -0.6071(7) 0.9470(6) 0.100(4) Uani 1 d . . . H39 H -0.0391 -0.6077 0.9871 0.080 Uiso 1 d R . . C40 C -0.0113(17) -0.6613(8) 0.9118(7) 0.114(5) Uani 1 d . . . H40 H -0.0572 -0.7004 0.9256 0.080 Uiso 1 d R . . C41 C 0.039(2) -0.6609(7) 0.8531(8) 0.135(6) Uani 1 d . . . H41 H 0.0326 -0.6989 0.8265 0.080 Uiso 1 d R . . C42 C 0.1032(17) -0.6049(7) 0.8313(6) 0.119(5) Uani 1 d . . . H42 H 0.1450 -0.6045 0.7917 0.080 Uiso 1 d 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 Cs 0.1305(8) 0.0807(5) 0.0753(4) -0.0103(4) 0.0087(4) -0.0245(5) S1 0.219(5) 0.119(3) 0.0786(19) 0.0256(19) -0.039(2) -0.101(3) S2 0.107(3) 0.095(2) 0.107(2) -0.0177(18) 0.049(2) -0.0063(19) P1 0.0703(17) 0.0732(15) 0.0443(10) 0.0041(10) -0.0022(10) -0.0147(13) P2 0.0530(14) 0.0850(16) 0.0447(10) 0.0018(11) 0.0063(9) -0.0048(13) N1 0.097(7) 0.091(6) 0.047(4) 0.005(4) 0.001(4) -0.033(5) O1 0.177(18) 0.33(3) 0.26(2) -0.06(2) 0.026(16) 0.123(19) C2 0.15(3) 0.27(4) 0.66(9) 0.26(5) -0.16(5) -0.03(3) C3 0.17(3) 0.51(8) 0.36(6) -0.26(6) -0.12(3) -0.01(4) O4 0.25(2) 0.186(16) 0.148(13) 0.032(12) -0.019(13) -0.034(15) C5 0.23(3) 0.26(3) 0.102(12) 0.088(17) -0.051(16) -0.13(2) C6 0.33(5) 0.18(3) 0.16(2) 0.06(2) -0.03(3) -0.11(3) O7 0.28(2) 0.167(13) 0.093(8) -0.009(8) 0.037(10) -0.077(13) C8 0.43(6) 0.16(2) 0.35(5) -0.03(3) 0.31(5) 0.07(3) C9 0.29(3) 0.116(13) 0.19(2) 0.004(15) 0.16(2) -0.006(17) O10 0.26(2) 0.235(18) 0.203(15) 0.085(14) 0.115(16) 0.123(16) C11 0.22(3) 0.20(2) 0.141(17) 0.044(16) -0.020(18) 0.055(19) C12 0.39(6) 1.7(2) 0.23(4) 0.31(8) 0.09(4) 0.66(11) O13 0.153(11) 0.220(14) 0.114(8) -0.008(9) 0.002(8) 0.017(11) C14 1.3(2) 0.74(14) 0.49(11) -0.31(9) 0.59(15) 0.02(14) C15 0.46(6) 0.60(8) 0.033(6) 0.013(17) 0.011(15) -0.36(6) O16 0.22(2) 0.201(17) 0.24(2) -0.117(15) 0.099(17) 0.018(14) C17 0.36(5) 0.30(5) 0.29(4) -0.15(4) 0.28(4) -0.19(4) C18 0.32(5) 0.15(2) 0.48(7) 0.03(3) 0.29(5) 0.02(2) C19 0.158(13) 0.076(7) 0.073(6) 0.013(6) 0.049(7) 0.032(8) C20 0.108(10) 0.117(10) 0.065(6) 0.016(6) 0.003(6) 0.020(8) C21 0.165(16) 0.108(11) 0.107(10) 0.013(9) 0.044(11) 0.032(11) C22 0.069(19) 0.11(2) 0.12(2) 0.003(18) 0.009(16) 0.034(17) C23 0.062(17) 0.27(5) 0.082(16) 0.03(2) 0.024(13) -0.03(2) C24 0.11(2) 0.13(2) 0.073(14) -0.013(14) 0.034(14) -0.053(18) C22B 0.11(2) 0.097(16) 0.067(12) -0.009(12) 0.042(13) 0.010(15) C23B 0.12(2) 0.13(2) 0.049(10) 0.005(12) 0.001(12) 0.037(19) C24B 0.16(3) 0.074(13) 0.054(11) -0.003(10) -0.006(13) 0.037(15) C25 0.066(8) 0.158(13) 0.082(7) 0.049(8) 0.000(6) 0.005(8) C26 0.068(9) 0.173(14) 0.080(7) 0.015(8) 0.007(6) -0.005(9) C27 0.070(10) 0.159(15) 0.122(11) -0.022(11) 0.009(8) -0.003(10) C28 0.06(2) 0.13(3) 0.19(4) 0.06(3) -0.03(2) -0.02(2) C29 0.09(2) 0.22(4) 0.062(13) 0.008(18) -0.051(15) -0.04(2) C30 0.085(19) 0.11(2) 0.088(15) -0.018(14) 0.026(14) -0.017(15) C28B 0.066(17) 0.13(2) 0.094(17) 0.039(18) -0.025(13) -0.004(17) C29B 0.12(2) 0.076(14) 0.086(14) -0.009(12) -0.017(15) 0.028(15) C30B 0.074(15) 0.068(12) 0.092(14) 0.020(11) 0.016(11) 0.012(11) C31 0.057(6) 0.131(9) 0.048(5) 0.007(5) 0.004(4) -0.008(6) C32 0.063(7) 0.100(8) 0.078(6) -0.003(6) 0.016(5) 0.008(6) C33 0.046(7) 0.134(12) 0.135(11) 0.011(9) 0.024(7) 0.007(7) C34 0.050(8) 0.23(2) 0.190(18) 0.067(17) -0.008(10) -0.008(11) C35 0.124(15) 0.29(3) 0.104(11) 0.049(15) -0.043(11) -0.011(18) C36 0.094(11) 0.26(2) 0.104(10) 0.079(13) -0.006(8) -0.007(13) C37 0.048(5) 0.083(6) 0.061(5) 0.017(5) 0.004(4) 0.003(5) C38 0.091(8) 0.090(8) 0.069(6) 0.019(6) 0.021(6) 0.017(6) C39 0.097(10) 0.115(10) 0.095(8) 0.039(8) 0.046(7) 0.016(8) C40 0.122(12) 0.111(11) 0.113(10) 0.052(9) 0.031(9) 0.000(10) C41 0.191(18) 0.087(9) 0.134(12) -0.006(9) 0.045(12) -0.054(11) C42 0.155(14) 0.130(11) 0.075(7) -0.006(8) 0.038(8) -0.056(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cs O10 3.05(2) . ? Cs O4 3.149(16) . ? Cs O1 3.18(2) . ? Cs O13 3.170(12) . ? Cs O16 3.205(18) . ? Cs O7 3.221(15) . ? Cs C14 3.47(4) . ? Cs S2 3.525(4) . ? Cs C3 3.61(4) . ? Cs C6 3.65(3) . ? Cs S1 3.660(4) . ? Cs C12 3.76(3) . ? S1 P1 1.957(4) . ? S2 P2 1.973(4) . ? P1 N1 1.591(8) . ? P1 C25 1.772(12) . ? P1 C19 1.788(11) . ? P2 N1 1.591(7) . ? P2 C37 1.813(10) . ? P2 C31 1.825(10) . ? O1 C18 1.14(3) . ? O1 C2 1.39(4) . ? C2 C3 1.20(5) . ? C3 O4 1.24(3) . ? O4 C5 1.36(3) . ? C5 C6 1.39(4) . ? C6 O7 1.20(3) . ? O7 C8 1.36(3) . ? C8 C9 1.34(4) . ? C9 O10 1.230(19) . ? O10 C11 1.33(2) . ? C11 C12 1.27(3) . ? C12 O13 1.23(3) . ? O13 C14 1.14(4) . ? C14 C15 0.97(5) . ? C15 O16 1.49(4) . ? O16 C17 1.18(4) . ? C17 C18 1.43(4) . ? C19 C20 1.314(16) . ? C19 C24 1.49(2) . ? C19 C24B 1.53(2) . ? C20 C21 1.398(18) . ? C21 C22 1.28(3) . ? C21 C22B 1.52(3) . ? C22 C23 1.37(5) . ? C23 C24 1.37(4) . ? C22B C23B 1.35(3) . ? C23B C24B 1.37(3) . ? C25 C26 1.292(16) . ? C25 C30B 1.45(2) . ? C25 C30 1.70(3) . ? C26 C27 1.350(18) . ? C27 C28B 1.17(3) . ? C27 C28 1.50(5) . ? C28 C29 1.35(5) . ? C29 C30 1.37(4) . ? C28B C29B 1.39(4) . ? C29B C30B 1.35(3) . ? C31 C32 1.328(14) . ? C31 C36 1.413(17) . ? C32 C33 1.361(16) . ? C33 C34 1.28(2) . ? C34 C35 1.39(2) . ? C35 C36 1.38(2) . ? C37 C42 1.373(16) . ? C37 C38 1.386(13) . ? C38 C39 1.366(17) . ? C39 C40 1.332(19) . ? C40 C41 1.368(19) . ? C41 C42 1.378(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Cs O4 102.9(5) . . ? O10 Cs O1 125.4(6) . . ? O4 Cs O1 55.3(7) . . ? O10 Cs O13 53.6(4) . . ? O4 Cs O13 126.8(4) . . ? O1 Cs O13 97.0(5) . . ? O10 Cs O16 102.7(6) . . ? O4 Cs O16 104.6(6) . . ? O1 Cs O16 51.9(7) . . ? O13 Cs O16 52.1(5) . . ? O10 Cs O7 52.0(5) . . ? O4 Cs O7 53.7(6) . . ? O1 Cs O7 100.9(7) . . ? O13 Cs O7 98.9(4) . . ? O16 Cs O7 126.7(5) . . ? O10 Cs C14 71.9(9) . . ? O4 Cs C14 122.8(9) . . ? O1 Cs C14 81.0(10) . . ? O13 Cs C14 19.1(8) . . ? O16 Cs C14 33.1(10) . . ? O7 Cs C14 112.0(9) . . ? O10 Cs S2 125.8(3) . . ? O4 Cs S2 127.6(4) . . ? O1 Cs S2 101.4(5) . . ? O13 Cs S2 99.7(3) . . ? O16 Cs S2 84.4(4) . . ? O7 Cs S2 148.8(2) . . ? C14 Cs S2 92.8(9) . . ? O10 Cs C3 113.4(6) . . ? O4 Cs C3 19.7(6) . . ? O1 Cs C3 35.6(8) . . ? O13 Cs C3 118.4(5) . . ? O16 Cs C3 85.8(7) . . ? O7 Cs C3 70.1(7) . . ? C14 Cs C3 108.7(10) . . ? S2 Cs C3 120.7(5) . . ? O10 Cs C6 70.6(6) . . ? O4 Cs C6 38.7(6) . . ? O1 Cs C6 92.0(8) . . ? O13 Cs C6 116.7(6) . . ? O16 Cs C6 131.9(6) . . ? O7 Cs C6 18.8(5) . . ? C14 Cs C6 127.4(10) . . ? S2 Cs C6 139.3(5) . . ? C3 Cs C6 57.5(7) . . ? O10 Cs S1 103.2(4) . . ? O4 Cs S1 77.0(3) . . ? O1 Cs S1 115.9(5) . . ? O13 Cs S1 147.1(3) . . ? O16 Cs S1 152.9(4) . . ? O7 Cs S1 76.6(2) . . ? C14 Cs S1 160.0(9) . . ? S2 Cs S1 74.21(8) . . ? C3 Cs S1 91.1(5) . . ? C6 Cs S1 65.4(4) . . ? O10 Cs C12 37.2(5) . . ? O4 Cs C12 127.4(8) . . ? O1 Cs C12 112.4(8) . . ? O13 Cs C12 18.0(5) . . ? O16 Cs C12 70.0(7) . . ? O7 Cs C12 86.7(7) . . ? C14 Cs C12 37.0(9) . . ? S2 Cs C12 104.4(7) . . ? C3 Cs C12 126.1(9) . . ? C6 Cs C12 105.5(8) . . ? S1 Cs C12 130.9(6) . . ? P1 S1 Cs 116.85(15) . . ? P2 S2 Cs 102.87(14) . . ? N1 P1 C25 108.4(5) . . ? N1 P1 C19 103.8(5) . . ? C25 P1 C19 104.8(7) . . ? N1 P1 S1 122.4(3) . . ? C25 P1 S1 107.7(5) . . ? C19 P1 S1 108.6(5) . . ? N1 P2 C37 105.2(4) . . ? N1 P2 C31 107.9(5) . . ? C37 P2 C31 104.0(5) . . ? N1 P2 S2 120.5(4) . . ? C37 P2 S2 108.5(3) . . ? C31 P2 S2 109.5(4) . . ? P1 N1 P2 139.9(6) . . ? C18 O1 C2 139(3) . . ? C18 O1 Cs 112(3) . . ? C2 O1 Cs 103.5(19) . . ? C3 C2 O1 109(3) . . ? C3 C2 Cs 74(2) . . ? O1 C2 Cs 55.5(14) . . ? O4 C3 C2 137(4) . . ? O4 C3 Cs 58.8(18) . . ? C2 C3 Cs 88(2) . . ? C3 O4 C5 140(3) . . ? C3 O4 Cs 101(2) . . ? C5 O4 Cs 115.6(16) . . ? O4 C5 C6 113.8(19) . . ? O7 C6 C5 133(3) . . ? O7 C6 Cs 59.8(15) . . ? C5 C6 Cs 91.2(18) . . ? C6 O7 C8 127(2) . . ? C6 O7 Cs 101.3(19) . . ? C8 O7 Cs 104.6(13) . . ? C9 C8 O7 111.3(19) . . ? C9 C8 Cs 78.5(14) . . ? O7 C8 Cs 55.2(11) . . ? O10 C9 C8 127(3) . . ? O10 C9 Cs 46.3(15) . . ? C8 C9 Cs 81.0(17) . . ? C9 O10 C11 126(3) . . ? C9 O10 Cs 116.8(18) . . ? C11 O10 Cs 116.7(15) . . ? C12 C11 O10 122(3) . . ? C12 C11 Cs 77.0(18) . . ? O10 C11 Cs 45.2(12) . . ? O13 C12 C11 131(3) . . ? O13 C12 Cs 52.7(14) . . ? C11 C12 Cs 83.8(18) . . ? C14 O13 C12 155(3) . . ? C14 O13 Cs 96(3) . . ? C12 O13 Cs 109.3(18) . . ? C15 C14 O13 167(6) . . ? C15 C14 Cs 111(4) . . ? O13 C14 Cs 65(2) . . ? C14 C15 O16 101(4) . . ? C17 O16 C15 135(3) . . ? C17 O16 Cs 117(2) . . ? C15 O16 Cs 108.0(16) . . ? O16 C17 C18 118(2) . . ? O16 C17 Cs 47.3(16) . . ? C18 C17 Cs 74.6(17) . . ? O1 C18 C17 134(4) . . ? O1 C18 Cs 51(2) . . ? C17 C18 Cs 84(2) . . ? C20 C19 C24 106.8(16) . . ? C20 C19 C24B 107.3(13) . . ? C24 C19 C24B 74.0(15) . . ? C20 C19 P1 125.7(9) . . ? C24 C19 P1 114.7(14) . . ? C24B C19 P1 116.5(12) . . ? C19 C20 C21 128.3(12) . . ? C22 C21 C20 110.8(19) . . ? C22 C21 C22B 63.1(16) . . ? C20 C21 C22B 111.8(14) . . ? C21 C22 C23 126(3) . . ? C22 C23 C24 117(3) . . ? C23 C24 C19 120(3) . . ? C23B C22B C21 119.3(18) . . ? C22B C23B C24B 120(2) . . ? C23B C24B C19 123(2) . . ? C26 C25 C30B 103.3(14) . . ? C26 C25 C30 104.9(14) . . ? C30B C25 C30 76.3(14) . . ? C26 C25 P1 129.7(10) . . ? C30B C25 P1 118.5(13) . . ? C30 C25 P1 110.9(12) . . ? C25 C26 C27 126.9(14) . . ? C28B C27 C26 120(2) . . ? C28B C27 C28 57.1(19) . . ? C26 C27 C28 120.0(19) . . ? C29 C28 C27 115(2) . . ? C28 C29 C30 124(3) . . ? C29 C30 C25 118(2) . . ? C27 C28B C29B 119(2) . . ? C30B C29B C28B 118(2) . . ? C29B C30B C25 122(2) . . ? C32 C31 C36 114.0(11) . . ? C32 C31 P2 122.5(8) . . ? C36 C31 P2 123.1(10) . . ? C31 C32 C33 124.4(12) . . ? C34 C33 C32 120.5(14) . . ? C33 C34 C35 120.6(15) . . ? C36 C35 C34 117.4(16) . . ? C35 C36 C31 121.7(15) . . ? C42 C37 C38 115.9(10) . . ? C42 C37 P2 121.1(8) . . ? C38 C37 P2 123.0(9) . . ? C39 C38 C37 121.8(12) . . ? C40 C39 C38 121.0(11) . . ? C39 C40 C41 119.6(13) . . ? C40 C41 C42 119.7(14) . . ? C37 C42 C41 122.0(12) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.777 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.084 #==END data_compound9 _database_code_depnum_ccdc_archive 'CCDC 220670' _chemical_name_common '(Cs(18-crown-6)) tetraphenyldiselenodimidodiphosphinate' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Cs(18-crown-6)] tetraphenyldiselenodimidodiphosphinate ; _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 Cs N O6 P2 Se2' _chemical_formula_weight 939.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 '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 9.232(2) _cell_length_b 20.359(3) _cell_length_c 21.385(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.80(1) _cell_angle_gamma 90.00 _cell_volume 4005.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 5.00 _cell_measurement_theta_max 12.50 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 2.864 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.233 _exptl_absorpt_correction_T_max 0.371 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4/PC diffracometer' _diffrn_measurement_method \w:2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3 _diffrn_reflns_number 7512 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.1161 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7044 _reflns_number_gt 3011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS ver 2.1 1993' _computing_cell_refinement 'XSCANS ver 2.1 1993' _computing_data_reduction 'XSCANS ver 2.1 1993' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V 6.10' _computing_publication_material 'SHELXTL V 6.10' _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 w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+21.8789P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7044 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1952 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2045 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 1.260 _refine_ls_shift/su_mean 0.062 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cs Cs 0.37972(13) -0.27191(5) 0.85362(4) 0.0945(4) Uani 1 d . . . Se1 Se 0.2963(3) -0.35267(10) 0.69876(8) 0.1436(10) Uani 1 d . . . Se2 Se 0.11717(19) -0.39909(9) 0.88119(8) 0.0992(6) Uani 1 d . . . P1 P 0.1819(4) -0.44254(16) 0.69983(13) 0.0596(8) Uani 1 d . . . P2 P 0.2011(4) -0.48129(17) 0.83534(13) 0.0597(8) Uani 1 d . . . N1 N 0.1797(12) -0.4867(5) 0.7613(4) 0.074(3) Uani 1 d . . . O1 O 0.199(3) -0.1445(19) 0.880(2) 0.286(19) Uani 1 d . . . C2 C 0.146(4) -0.1206(19) 0.818(2) 0.30(3) Uani 1 d . . . H2A H 0.1109 -0.0766 0.8228 0.080 Uiso 1 d R . . H2B H 0.0656 -0.1472 0.8017 0.080 Uiso 1 d R . . C3 C 0.249(4) -0.125(2) 0.782(3) 0.46(7) Uani 1 d . . . H3A H 0.3022 -0.0854 0.7937 0.080 Uiso 1 d R . . H3B H 0.1940 -0.1134 0.7431 0.080 Uiso 1 d R . . O4 O 0.337(3) -0.1529(10) 0.7618(11) 0.189(8) Uani 1 d . . . C5 C 0.439(4) -0.1480(16) 0.7146(11) 0.22(2) Uani 1 d . . . H5A H 0.4930 -0.1084 0.7241 0.080 Uiso 1 d R . . H5B H 0.3870 -0.1424 0.6742 0.080 Uiso 1 d R . . C6 C 0.541(5) -0.1947(14) 0.7221(17) 0.24(2) Uani 1 d . . . H6A H 0.6098 -0.1831 0.6925 0.080 Uiso 1 d R . . H6B H 0.4895 -0.2329 0.7062 0.080 Uiso 1 d R . . O7 O 0.617(3) -0.2149(10) 0.7669(7) 0.184(9) Uani 1 d . . . C8 C 0.729(4) -0.2610(16) 0.7684(18) 0.34(4) Uani 1 d . . . H8A H 0.8041 -0.2475 0.7426 0.080 Uiso 1 d R . . H8B H 0.6877 -0.3011 0.7515 0.080 Uiso 1 d R . . C9 C 0.770(4) -0.2725(16) 0.8248(15) 0.24(2) Uani 1 d . . . H9A H 0.8252 -0.2339 0.8365 0.080 Uiso 1 d R . . H9B H 0.8381 -0.3077 0.8228 0.080 Uiso 1 d R . . O10 O 0.705(2) -0.2861(8) 0.8709(9) 0.176(7) Uani 1 d . . . C11 C 0.763(3) -0.2977(16) 0.9321(13) 0.197(13) Uani 1 d . . . H11A H 0.8245 -0.2609 0.9433 0.080 Uiso 1 d R . . H11B H 0.8237 -0.3359 0.9314 0.080 Uiso 1 d R . . C12 C 0.688(4) -0.290(3) 0.977(2) 0.58(8) Uani 1 d . . . H12A H 0.7449 -0.2855 1.0163 0.080 Uiso 1 d R . . H12B H 0.6580 -0.3354 0.9743 0.080 Uiso 1 d R . . O13 O 0.570(2) -0.2724(9) 0.9829(7) 0.157(5) Uani 1 d . . . C14 C 0.486(5) -0.260(2) 1.0186(16) 0.50(5) Uani 1 d . . . H14A H 0.5489 -0.2571 1.0564 0.080 Uiso 1 d R . . H14B H 0.4408 -0.3027 1.0188 0.080 Uiso 1 d R . . C15 C 0.394(4) -0.236(2) 1.0354(9) 0.32(3) Uani 1 d . . . H15A H 0.4382 -0.1953 1.0490 0.080 Uiso 1 d R . . H15B H 0.3346 -0.2504 1.0676 0.080 Uiso 1 d R . . O16 O 0.295(3) -0.2155(11) 0.9840(11) 0.203(10) Uani 1 d . . . C17 C 0.198(4) -0.174(2) 0.9797(18) 0.26(3) Uani 1 d . . . H17A H 0.2455 -0.1354 0.9981 0.080 Uiso 1 d R . . H17B H 0.1234 -0.1867 1.0059 0.080 Uiso 1 d R . . C18 C 0.127(5) -0.146(2) 0.922(2) 0.29(4) Uani 1 d . . . H18A H 0.0559 -0.1794 0.9115 0.080 Uiso 1 d R . . H18B H 0.0742 -0.1058 0.9259 0.080 Uiso 1 d R . . C19 C 0.248(2) -0.4968(7) 0.6435(6) 0.101(6) Uani 1 d . . . C20 C 0.2912(17) -0.5580(8) 0.6518(7) 0.093(5) Uani 1 d . . . H20 H 0.2851 -0.5750 0.6934 0.080 Uiso 1 d R . . C21 C 0.348(2) -0.5991(9) 0.6094(8) 0.116(6) Uani 1 d . . . H21 H 0.3223 -0.6446 0.6044 0.080 Uiso 1 d R . . C22 C 0.442(4) -0.568(3) 0.5716(18) 0.115(14) Uani 0.484(15) d P A 1 H22 H 0.5162 -0.5915 0.5523 0.080 Uiso 0.484(15) d PR A 1 C23 C 0.435(3) -0.499(2) 0.5651(14) 0.102(12) Uani 0.484(15) d P A 1 H23 H 0.4779 -0.4778 0.5311 0.080 Uiso 0.484(15) d PR A 1 C24 C 0.360(4) -0.4635(16) 0.6031(13) 0.095(12) Uani 0.484(15) d P A 1 H24 H 0.3792 -0.4174 0.6081 0.080 Uiso 0.484(15) d PR A 1 C22B C 0.294(4) -0.5854(15) 0.5431(12) 0.093(11) Uani 0.516(15) d P A 2 H22B H 0.3216 -0.6133 0.5100 0.080 Uiso 0.516(15) d PR A 2 C23B C 0.209(4) -0.5345(16) 0.5286(12) 0.107(12) Uani 0.516(15) d P A 2 H23B H 0.1735 -0.5263 0.4858 0.080 Uiso 0.516(15) d PR A 2 C24B C 0.176(4) -0.4903(14) 0.5761(12) 0.095(11) Uani 0.516(15) d P A 2 H24B H 0.1051 -0.4562 0.5670 0.080 Uiso 0.516(15) d PR A 2 C25 C -0.0021(16) -0.4262(9) 0.6712(7) 0.101(5) Uani 1 d . . . C26 C -0.118(2) -0.4377(9) 0.6971(7) 0.108(6) Uani 1 d . . . H26 H -0.1050 -0.4598 0.7368 0.080 Uiso 1 d R . . C27 C -0.255(2) -0.4248(12) 0.6750(11) 0.129(7) Uani 1 d . . . H27 H -0.3292 -0.4147 0.7024 0.080 Uiso 1 d R . . C28 C -0.283(4) -0.429(2) 0.603(2) 0.122(14) Uani 0.490(17) d P B 1 H28 H -0.3783 -0.4210 0.5831 0.080 Uiso 0.490(17) d PR B 1 C29 C -0.165(4) -0.4418(19) 0.5675(15) 0.107(12) Uani 0.490(17) d P B 1 H29 H -0.1826 -0.4512 0.5235 0.080 Uiso 0.490(17) d PR B 1 C30 C -0.027(4) -0.4428(17) 0.5950(13) 0.099(12) Uani 0.490(17) d P B 1 H30 H 0.0553 -0.4521 0.5716 0.080 Uiso 0.490(17) d PR B 1 C28B C -0.284(4) -0.384(3) 0.6398(15) 0.110(15) Uani 0.510(17) d P B 2 H28B H -0.3787 -0.3837 0.6174 0.080 Uiso 0.510(17) d PR B 2 C29B C -0.175(4) -0.3439(17) 0.6245(14) 0.096(11) Uani 0.510(17) d P B 2 H29B H -0.2006 -0.3028 0.6047 0.080 Uiso 0.510(17) d PR B 2 C30B C -0.033(3) -0.3624(13) 0.6402(11) 0.071(8) Uani 0.510(17) d P B 2 H30B H 0.0461 -0.3346 0.6303 0.080 Uiso 0.510(17) d PR B 2 C31 C 0.3948(14) -0.4897(7) 0.8604(6) 0.076(4) Uani 1 d . . . C32 C 0.4981(17) -0.4633(7) 0.8273(6) 0.078(4) Uani 1 d . . . H32 H 0.4680 -0.4422 0.7882 0.080 Uiso 1 d R . . C33 C 0.6419(17) -0.4661(10) 0.8465(9) 0.108(6) Uani 1 d . . . H33 H 0.7113 -0.4450 0.8222 0.080 Uiso 1 d R . . C34 C 0.6869(19) -0.4965(12) 0.8979(11) 0.136(8) Uani 1 d . . . H34 H 0.7885 -0.4967 0.9119 0.080 Uiso 1 d R . . C35 C 0.588(3) -0.5295(12) 0.9324(10) 0.165(9) Uani 1 d . . . H35 H 0.6221 -0.5535 0.9693 0.080 Uiso 1 d R . . C36 C 0.4430(19) -0.5266(11) 0.9140(7) 0.137(8) Uani 1 d . . . H36 H 0.3731 -0.5495 0.9367 0.080 Uiso 1 d R . . C37 C 0.1138(13) -0.5567(6) 0.8632(5) 0.062(3) Uani 1 d . . . C38 C 0.0613(16) -0.5573(8) 0.9214(6) 0.087(4) Uani 1 d . . . H38 H 0.0710 -0.5191 0.9477 0.080 Uiso 1 d R . . C39 C -0.0051(19) -0.6140(11) 0.9417(9) 0.115(7) Uani 1 d . . . H39 H -0.0450 -0.6146 0.9818 0.080 Uiso 1 d R . . C40 C -0.018(2) -0.6690(11) 0.9038(11) 0.127(7) Uani 1 d . . . H40 H -0.0635 -0.7081 0.9176 0.080 Uiso 1 d R . . C41 C 0.041(2) -0.6665(8) 0.8477(9) 0.129(7) Uani 1 d . . . H41 H 0.0345 -0.7045 0.8211 0.080 Uiso 1 d R . . C42 C 0.1067(19) -0.6114(8) 0.8270(8) 0.111(6) Uani 1 d . . . H42 H 0.1485 -0.6110 0.7874 0.080 Uiso 1 d 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 Cs 0.1251(9) 0.0846(6) 0.0739(6) -0.0144(5) 0.0084(5) -0.0222(7) Se1 0.224(3) 0.1191(15) 0.0785(11) 0.0271(10) -0.0432(13) -0.1021(16) Se2 0.0986(13) 0.0970(12) 0.1083(12) -0.0219(10) 0.0448(10) 0.0022(10) P1 0.063(2) 0.072(2) 0.0430(15) -0.0009(15) 0.0008(14) -0.0121(17) P2 0.056(2) 0.080(2) 0.0434(15) -0.0016(15) 0.0070(14) 0.0014(17) N1 0.101(9) 0.080(7) 0.040(5) 0.015(5) -0.005(5) -0.022(6) O1 0.16(2) 0.35(4) 0.34(4) -0.15(3) 0.00(3) 0.11(2) C2 0.19(4) 0.22(4) 0.47(8) 0.04(4) -0.17(6) 0.08(3) C3 0.12(4) 0.58(12) 0.65(15) -0.22(10) -0.17(6) 0.14(5) O4 0.19(2) 0.183(16) 0.181(18) 0.056(14) -0.044(15) -0.026(16) C5 0.33(5) 0.24(4) 0.081(15) 0.08(2) -0.04(2) -0.14(4) C6 0.39(7) 0.14(3) 0.19(4) 0.07(3) 0.00(4) -0.12(4) O7 0.30(3) 0.167(17) 0.088(10) 0.014(10) 0.051(13) -0.060(16) C8 0.44(7) 0.14(3) 0.50(9) -0.11(4) 0.43(7) -0.05(3) C9 0.27(4) 0.19(3) 0.28(4) 0.03(3) 0.21(4) -0.03(3) O10 0.205(18) 0.158(14) 0.176(15) 0.042(12) 0.080(15) 0.054(12) C11 0.19(4) 0.24(3) 0.15(3) 0.01(2) -0.03(2) 0.04(2) C12 0.18(4) 1.2(2) 0.31(7) 0.17(9) 0.01(4) 0.32(8) O13 0.139(13) 0.210(16) 0.124(11) 0.026(11) 0.013(10) -0.023(12) C14 0.69(11) 0.63(10) 0.22(4) -0.05(5) 0.31(6) 0.04(8) C15 0.40(6) 0.53(7) 0.036(12) -0.05(2) 0.05(2) -0.33(6) O16 0.21(2) 0.21(2) 0.20(2) -0.079(15) 0.077(18) 0.030(16) C17 0.20(5) 0.36(9) 0.24(5) -0.16(5) 0.12(4) -0.05(5) C18 0.14(4) 0.19(3) 0.55(13) -0.02(6) 0.08(6) 0.07(3) C19 0.174(17) 0.071(10) 0.065(9) 0.016(7) 0.053(10) 0.027(10) C20 0.116(13) 0.098(12) 0.065(9) 0.009(8) 0.013(8) 0.026(10) C21 0.154(18) 0.094(12) 0.105(14) 0.003(11) 0.037(13) 0.032(12) C22 0.05(2) 0.18(4) 0.11(3) 0.00(3) -0.01(2) 0.03(3) C23 0.07(2) 0.17(4) 0.07(2) 0.01(2) 0.006(16) -0.03(2) C24 0.11(3) 0.10(2) 0.08(2) -0.040(18) 0.06(2) -0.03(2) C22B 0.11(3) 0.11(2) 0.061(17) 0.010(17) 0.047(18) 0.04(2) C23B 0.17(3) 0.10(2) 0.043(15) -0.005(15) -0.013(18) 0.02(2) C24B 0.13(3) 0.09(2) 0.064(17) -0.002(15) 0.002(17) 0.04(2) C25 0.068(11) 0.146(15) 0.088(10) 0.059(10) 0.011(8) -0.013(10) C26 0.085(13) 0.163(17) 0.077(10) 0.008(11) 0.008(10) 0.010(12) C27 0.065(14) 0.20(2) 0.122(17) -0.038(17) 0.005(12) 0.004(14) C28 0.09(3) 0.15(4) 0.12(3) 0.00(3) -0.04(3) 0.02(3) C29 0.07(2) 0.17(4) 0.08(2) 0.01(2) -0.007(19) 0.00(2) C30 0.07(2) 0.15(3) 0.068(18) 0.035(19) -0.010(16) 0.00(2) C28B 0.09(3) 0.18(5) 0.047(19) 0.00(2) -0.039(19) -0.02(3) C29B 0.10(3) 0.09(2) 0.09(2) -0.004(18) -0.03(2) 0.03(2) C30B 0.09(2) 0.073(18) 0.056(14) 0.003(13) 0.026(14) 0.006(15) C31 0.054(8) 0.128(12) 0.048(7) -0.002(8) 0.008(6) 0.014(8) C32 0.089(12) 0.081(10) 0.066(8) 0.001(7) 0.017(8) 0.001(8) C33 0.043(10) 0.162(18) 0.118(14) -0.007(12) 0.006(9) 0.008(10) C34 0.041(11) 0.21(2) 0.150(19) -0.006(17) -0.022(12) -0.001(13) C35 0.12(2) 0.23(3) 0.135(18) 0.064(17) -0.049(16) 0.023(19) C36 0.074(13) 0.25(3) 0.085(11) 0.030(13) -0.027(9) -0.005(14) C37 0.051(8) 0.073(8) 0.061(7) 0.018(7) 0.004(6) 0.012(7) C38 0.094(11) 0.102(11) 0.069(9) 0.022(8) 0.027(8) 0.024(9) C39 0.094(13) 0.147(17) 0.110(14) 0.076(14) 0.044(11) 0.036(13) C40 0.110(15) 0.120(16) 0.154(19) 0.071(14) 0.027(14) -0.018(13) C41 0.18(2) 0.079(12) 0.137(16) 0.004(11) 0.056(15) -0.036(12) C42 0.141(16) 0.102(13) 0.097(11) 0.006(10) 0.044(11) -0.035(12) _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 Cs O10 3.013(19) . ? Cs O4 3.123(18) . ? Cs O16 3.175(19) . ? Cs O13 3.148(15) . ? Cs O1 3.16(3) . ? Cs O7 3.205(17) . ? Cs C3 3.54(5) . ? Cs Se2 3.629(2) . ? Cs C6 3.65(3) . ? Cs C9 3.70(3) . ? Cs C12 3.73(4) . ? Cs Se1 3.720(2) . ? Se1 P1 2.114(4) . ? Se2 P2 2.119(4) . ? P1 N1 1.593(9) . ? P1 C19 1.778(14) . ? P1 C25 1.787(15) . ? P2 N1 1.584(9) . ? P2 C31 1.831(13) . ? P2 C37 1.855(13) . ? O1 C18 1.16(5) . ? O1 C2 1.45(5) . ? C2 C3 1.28(6) . ? C3 O4 1.11(4) . ? O4 C5 1.44(4) . ? C5 C6 1.34(5) . ? C6 O7 1.21(3) . ? O7 C8 1.40(4) . ? C8 C9 1.25(5) . ? C9 O10 1.22(2) . ? O10 C11 1.39(3) . ? C11 C12 1.24(4) . ? C12 O13 1.16(3) . ? O13 C14 1.16(3) . ? C14 C15 1.07(6) . ? C15 O16 1.44(4) . ? O16 C17 1.23(4) . ? C17 C18 1.46(5) . ? C19 C20 1.318(18) . ? C19 C24B 1.54(3) . ? C19 C24 1.56(3) . ? C20 C21 1.370(19) . ? C21 C22 1.39(4) . ? C21 C22B 1.49(3) . ? C22 C23 1.41(5) . ? C23 C24 1.32(4) . ? C22B C23B 1.32(4) . ? C23B C24B 1.41(4) . ? C25 C26 1.271(19) . ? C25 C30B 1.48(3) . ? C25 C30 1.66(3) . ? C26 C27 1.34(2) . ? C27 C28B 1.14(4) . ? C27 C28 1.54(5) . ? C28 C29 1.41(5) . ? C29 C30 1.36(4) . ? C28B C29B 1.36(5) . ? C29B C30B 1.38(4) . ? C31 C32 1.346(17) . ? C31 C36 1.41(2) . ? C32 C33 1.358(19) . ? C33 C34 1.30(2) . ? C34 C35 1.40(3) . ? C35 C36 1.36(2) . ? C37 C42 1.354(19) . ? C37 C38 1.373(16) . ? C38 C39 1.39(2) . ? C39 C40 1.38(2) . ? C40 C41 1.36(2) . ? C41 C42 1.37(2) . ? 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 O10 Cs O4 102.9(5) . . ? O10 Cs O16 104.2(6) . . ? O4 Cs O16 104.1(7) . . ? O10 Cs O13 54.1(5) . . ? O4 Cs O13 125.8(5) . . ? O16 Cs O13 52.5(6) . . ? O10 Cs O1 126.4(7) . . ? O4 Cs O1 55.6(10) . . ? O16 Cs O1 51.2(10) . . ? O13 Cs O1 96.3(8) . . ? O10 Cs O7 51.8(6) . . ? O4 Cs O7 53.9(7) . . ? O16 Cs O7 127.5(5) . . ? O13 Cs O7 98.7(5) . . ? O1 Cs O7 101.7(10) . . ? O10 Cs C3 115.8(7) . . ? O4 Cs C3 17.9(8) . . ? O16 Cs C3 88.5(10) . . ? O13 Cs C3 122.0(9) . . ? O1 Cs C3 38.3(12) . . ? O7 Cs C3 70.5(8) . . ? O10 Cs Se2 125.8(3) . . ? O4 Cs Se2 127.3(4) . . ? O16 Cs Se2 84.1(5) . . ? O13 Cs Se2 100.7(3) . . ? O1 Cs Se2 100.8(7) . . ? O7 Cs Se2 148.3(3) . . ? C3 Cs Se2 117.9(7) . . ? O10 Cs C6 70.6(7) . . ? O4 Cs C6 38.6(7) . . ? O16 Cs C6 132.0(7) . . ? O13 Cs C6 116.4(7) . . ? O1 Cs C6 92.3(10) . . ? O7 Cs C6 19.0(7) . . ? C3 Cs C6 56.4(9) . . ? Se2 Cs C6 139.0(6) . . ? O10 Cs C9 17.4(6) . . ? O4 Cs C9 88.3(7) . . ? O16 Cs C9 117.6(8) . . ? O13 Cs C9 70.6(6) . . ? O1 Cs C9 124.5(9) . . ? O7 Cs C9 35.2(7) . . ? C3 Cs C9 103.4(8) . . ? Se2 Cs C9 134.2(5) . . ? C6 Cs C9 53.6(8) . . ? O10 Cs C12 37.8(6) . . ? O4 Cs C12 124.7(9) . . ? O16 Cs C12 69.2(8) . . ? O13 Cs C12 16.9(6) . . ? O1 Cs C12 109.8(10) . . ? O7 Cs C12 85.8(8) . . ? C3 Cs C12 127.2(12) . . ? Se2 Cs C12 107.1(8) . . ? C6 Cs C12 104.5(9) . . ? C9 Cs C12 54.8(8) . . ? O10 Cs Se1 101.4(4) . . ? O4 Cs Se1 77.2(4) . . ? O16 Cs Se1 153.4(5) . . ? O13 Cs Se1 147.0(4) . . ? O1 Cs Se1 116.7(7) . . ? O7 Cs Se1 75.3(3) . . ? C3 Cs Se1 87.1(9) . . ? Se2 Cs Se1 74.81(4) . . ? C6 Cs Se1 64.6(5) . . ? C9 Cs Se1 89.0(6) . . ? C12 Cs Se1 132.3(7) . . ? P1 Se1 Cs 116.07(10) . . ? P2 Se2 Cs 102.31(11) . . ? N1 P1 C19 103.7(6) . . ? N1 P1 C25 108.0(6) . . ? C19 P1 C25 104.6(9) . . ? N1 P1 Se1 122.6(4) . . ? C19 P1 Se1 109.3(5) . . ? C25 P1 Se1 107.3(6) . . ? N1 P2 C31 108.9(6) . . ? N1 P2 C37 104.0(6) . . ? C31 P2 C37 105.6(6) . . ? N1 P2 Se2 119.9(4) . . ? C31 P2 Se2 108.9(5) . . ? C37 P2 Se2 108.6(4) . . ? P2 N1 P1 140.9(7) . . ? C18 O1 C2 123(4) . . ? C18 O1 Cs 118(4) . . ? C2 O1 Cs 105(2) . . ? C3 C2 O1 109(3) . . ? C3 C2 Cs 68(3) . . ? O1 C2 Cs 53.5(16) . . ? O4 C3 C2 151(5) . . ? O4 C3 Cs 60(3) . . ? C2 C3 Cs 92(3) . . ? C3 O4 C5 141(4) . . ? C3 O4 Cs 103(3) . . ? C5 O4 Cs 116.0(18) . . ? C6 C5 O4 111(2) . . ? O7 C6 C5 134(4) . . ? O7 C6 Cs 59.3(19) . . ? C5 C6 Cs 94(2) . . ? C6 O7 C8 129(3) . . ? C6 O7 Cs 102(2) . . ? C8 O7 Cs 106.6(15) . . ? C9 C8 O7 108(2) . . ? C9 C8 Cs 74.1(19) . . ? O7 C8 Cs 53.1(11) . . ? O10 C9 C8 134(4) . . ? O10 C9 Cs 47.5(17) . . ? C8 C9 Cs 87(3) . . ? C9 O10 C11 129(3) . . ? C9 O10 Cs 115(2) . . ? C11 O10 Cs 115.4(16) . . ? C12 C11 O10 121(3) . . ? C12 C11 Cs 76(3) . . ? O10 C11 Cs 45.4(13) . . ? O13 C12 C11 135(4) . . ? O13 C12 Cs 52(2) . . ? C11 C12 Cs 85(3) . . ? C12 O13 C14 145(4) . . ? C12 O13 Cs 111(2) . . ? C14 O13 Cs 103(2) . . ? O13 C14 C15 156(5) . . ? O13 C14 Cs 59(2) . . ? C15 C14 Cs 102(3) . . ? C14 C15 O16 110(3) . . ? C17 O16 C15 132(3) . . ? C17 O16 Cs 115(3) . . ? C15 O16 Cs 112(2) . . ? O16 C17 C18 127(4) . . ? O1 C18 C17 115(5) . . ? O1 C18 Cs 47(3) . . ? C17 C18 Cs 80(3) . . ? C20 C19 C24B 108.0(16) . . ? C20 C19 C24 105.9(17) . . ? C24B C19 C24 72.7(17) . . ? C20 C19 P1 127.9(11) . . ? C24B C19 P1 115.8(14) . . ? C24 C19 P1 112.8(14) . . ? C19 C20 C21 128.2(15) . . ? C20 C21 C22 113(2) . . ? C20 C21 C22B 113.4(17) . . ? C22 C21 C22B 62.5(18) . . ? C21 C22 C23 119(3) . . ? C24 C23 C22 120(3) . . ? C23 C24 C19 121(3) . . ? C23B C22B C21 121(2) . . ? C22B C23B C24B 119(3) . . ? C23B C24B C19 121(2) . . ? C26 C25 C30B 102.8(18) . . ? C26 C25 C30 109.9(17) . . ? C30B C25 C30 74.5(15) . . ? C26 C25 P1 129.0(13) . . ? C30B C25 P1 117.3(15) . . ? C30 C25 P1 110.2(15) . . ? C25 C26 C27 128.1(18) . . ? C28B C27 C26 123(3) . . ? C28B C27 C28 51(3) . . ? C26 C27 C28 115(2) . . ? C29 C28 C27 119(3) . . ? C30 C29 C28 121(3) . . ? C29 C30 C25 118(3) . . ? C27 C28B C29B 117(4) . . ? C28B C29B C30B 119(3) . . ? C29B C30B C25 119(3) . . ? C32 C31 C36 116.8(13) . . ? C32 C31 P2 121.7(11) . . ? C36 C31 P2 121.5(12) . . ? C33 C32 C31 122.8(14) . . ? C34 C33 C32 120.8(18) . . ? C33 C34 C35 119.9(18) . . ? C36 C35 C34 119.8(19) . . ? C35 C36 C31 119.5(18) . . ? C42 C37 C38 120.4(13) . . ? C42 C37 P2 120.0(10) . . ? C38 C37 P2 119.6(11) . . ? C37 C38 C39 119.2(16) . . ? C40 C39 C38 120.3(16) . . ? C41 C40 C39 117.9(17) . . ? C40 C41 C42 122.6(18) . . ? C37 C42 C41 119.5(15) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.939 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.094 #==END #==END data_compound6 _database_code_depnum_ccdc_archive 'CCDC 220671' _chemical_name_common ;Rubidium(18-crown-6) imidobis(diphenylselenophosphinate- Se,Se') ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Rubidium(18-crown-6) imidobis(diphenylselenophosphinate-Se,Se') ; _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 N O6 P2 Rb Se2' _chemical_formula_weight 892.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'F d d 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 23.618(3) _cell_length_b 72.846(8) _cell_length_c 9.100(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15656(6) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 4.50 _cell_measurement_theta_max 12.50 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7200 _exptl_absorpt_coefficient_mu 3.249 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.292 _exptl_absorpt_correction_T_max 0.333 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4/PC diffractometer' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.57 _diffrn_reflns_number 7367 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.1495 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -86 _diffrn_reflns_limit_k_max 86 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6891 _reflns_number_gt 3806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS ver 2.1 1993' _computing_cell_refinement 'XSCANS ver 2.1 1993' _computing_data_reduction 'XSCANS ver 2.1 1993' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V 6.10' _computing_publication_material 'SHELXTL V 6.10' _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 w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+65.3033P] 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 noref _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 0.28(2) _refine_ls_number_reflns 6891 _refine_ls_number_parameters 434 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1556 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rb Rb 0.32166(6) 0.035640(18) 0.82717(18) 0.0490(4) Uani 1 d . . . Se1 Se 0.46327(6) 0.04888(2) 0.81491(19) 0.0519(4) Uani 1 d . . . Se2 Se 0.32153(7) 0.07244(2) 1.0779(2) 0.0618(5) Uani 1 d . . . P1 P 0.48542(14) 0.06923(5) 0.9738(4) 0.0371(8) Uani 1 d . . . P2 P 0.38122(15) 0.09123(5) 0.9846(4) 0.0370(8) Uani 1 d . . . N1 N 0.4475(4) 0.08696(14) 0.9960(14) 0.046(3) Uani 1 d . . . O1 O 0.2954(5) 0.03915(16) 0.4964(12) 0.072(3) Uani 1 d . . . C2 C 0.2746(10) 0.0574(2) 0.498(2) 0.092(7) Uani 1 d . . . H2A H 0.2726 0.0620 0.3991 0.111 Uiso 1 d R . . H2B H 0.2992 0.0652 0.5537 0.111 Uiso 1 d R . . C3 C 0.2169(9) 0.0574(2) 0.566(2) 0.085(6) Uani 1 d . . . H3A H 0.1935 0.0487 0.5144 0.102 Uiso 1 d R . . H3B H 0.1996 0.0693 0.5584 0.102 Uiso 1 d R . . O4 O 0.2201(5) 0.05229(15) 0.7159(12) 0.067(3) Uani 1 d . . . C5 C 0.1673(7) 0.0521(3) 0.793(2) 0.081(6) Uani 1 d . . . H5A H 0.1441 0.0422 0.7584 0.097 Uiso 1 d R . . H5B H 0.1477 0.0635 0.7750 0.097 Uiso 1 d R . . C6 C 0.1778(7) 0.0501(2) 0.950(2) 0.069(5) Uani 1 d . . . H6A H 0.1425 0.0509 1.0012 0.083 Uiso 1 d R . . H6B H 0.2019 0.0598 0.9835 0.083 Uiso 1 d R . . O7 O 0.2038(4) 0.03310(15) 0.9792(12) 0.055(3) Uani 1 d . . . C8 C 0.2184(7) 0.0310(3) 1.1280(19) 0.070(5) Uani 1 d . . . H8A H 0.1855 0.0326 1.1886 0.084 Uiso 1 d R . . H8B H 0.2456 0.0402 1.1544 0.084 Uiso 1 d R . . C9 C 0.2439(7) 0.0126(2) 1.1532(18) 0.064(5) Uani 1 d . . . H9A H 0.2188 0.0035 1.1143 0.077 Uiso 1 d R . . H9B H 0.2489 0.0103 1.2563 0.077 Uiso 1 d R . . O10 O 0.2970(4) 0.01161(12) 1.0776(15) 0.063(3) Uani 1 d . . . C11 C 0.3232(8) -0.00623(19) 1.081(3) 0.084(6) Uani 1 d . . . H11A H 0.3001 -0.0147 1.0268 0.101 Uiso 1 d R . . H11B H 0.3253 -0.0105 1.1811 0.101 Uiso 1 d R . . C12 C 0.3798(8) -0.0059(3) 1.014(2) 0.087(7) Uani 1 d . . . H12A H 0.3999 -0.0171 1.0334 0.105 Uiso 1 d R . . H12B H 0.4011 0.0042 1.0529 0.105 Uiso 1 d R . . O13 O 0.3700(4) -0.00341(14) 0.8583(15) 0.069(4) Uani 1 d . . . C14 C 0.4233(7) -0.0034(3) 0.780(2) 0.087(7) Uani 1 d . . . H14A H 0.4428 -0.0148 0.7962 0.104 Uiso 1 d R . . H14B H 0.4466 0.0064 0.8154 0.104 Uiso 1 d R . . C15 C 0.4131(7) -0.0008(2) 0.618(2) 0.079(7) Uani 1 d . . . H15A H 0.3890 -0.0104 0.5835 0.095 Uiso 1 d R . . H15B H 0.4481 -0.0013 0.5646 0.095 Uiso 1 d R . . O16 O 0.3862(5) 0.01648(17) 0.5946(14) 0.074(3) Uani 1 d . . . C17 C 0.3755(8) 0.0195(3) 0.452(2) 0.087(6) Uani 1 d . . . H17A H 0.3461 0.0113 0.4208 0.104 Uiso 1 d R . . H17B H 0.4082 0.0176 0.3909 0.104 Uiso 1 d R . . C18 C 0.3531(9) 0.0388(4) 0.435(2) 0.109(9) Uani 1 d . . . H18A H 0.3768 0.0466 0.4930 0.131 Uiso 1 d R . . H18B H 0.3530 0.0432 0.3351 0.131 Uiso 1 d R . . C19 C 0.4957(6) 0.05830(19) 1.1533(15) 0.039(3) Uani 1 d . . . C20 C 0.5123(7) 0.0405(2) 1.1629(17) 0.058(4) Uani 1 d . . . H20 H 0.5180 0.0335 1.0749 0.070 Uiso 1 d R . . C21 C 0.5203(7) 0.0325(2) 1.300(2) 0.069(5) Uani 1 d . . . H21 H 0.5305 0.0198 1.3076 0.083 Uiso 1 d R . . C22 C 0.5149(7) 0.0424(2) 1.4257(16) 0.058(4) Uani 1 d . . . H22 H 0.5217 0.0371 1.5206 0.069 Uiso 1 d R . . C23 C 0.4975(8) 0.0608(2) 1.411(2) 0.067(5) Uani 1 d . . . H23 H 0.4927 0.0682 1.4973 0.080 Uiso 1 d R . . C24 C 0.4882(7) 0.0684(2) 1.2791(14) 0.059(5) Uani 1 d . . . H24 H 0.4755 0.0809 1.2714 0.071 Uiso 1 d R . . C25 C 0.5555(5) 0.07889(16) 0.9285(14) 0.032(3) Uani 1 d . . . C26 C 0.5741(7) 0.09458(19) 1.0014(19) 0.061(4) Uani 1 d . . . H26 H 0.5508 0.0998 1.0769 0.073 Uiso 1 d R . . C27 C 0.6244(6) 0.1026(2) 0.968(2) 0.064(5) Uani 1 d . . . H27 H 0.6362 0.1135 1.0188 0.077 Uiso 1 d R . . C28 C 0.6583(6) 0.0952(2) 0.8629(18) 0.060(4) Uani 1 d . . . H28 H 0.6934 0.1012 0.8395 0.072 Uiso 1 d R . . C29 C 0.6425(6) 0.0797(3) 0.7891(19) 0.069(5) Uani 1 d . . . H29 H 0.6662 0.0744 0.7146 0.083 Uiso 1 d R . . C30 C 0.5902(5) 0.07174(19) 0.827(2) 0.056(4) Uani 1 d . . . H30 H 0.5790 0.0605 0.7797 0.067 Uiso 1 d R . . C31 C 0.3719(5) 0.11353(16) 1.073(2) 0.046(3) Uani 1 d . . . C32 C 0.3175(6) 0.1200(2) 1.1046(19) 0.061(4) Uani 1 d . . . H32 H 0.2854 0.1124 1.0838 0.073 Uiso 1 d R . . C33 C 0.3100(7) 0.1369(2) 1.1647(17) 0.061(4) Uani 1 d . . . H33 H 0.2724 0.1414 1.1837 0.073 Uiso 1 d R . . C34 C 0.3540(7) 0.1475(2) 1.202(2) 0.069(5) Uani 1 d . . . H34 H 0.3485 0.1595 1.2433 0.083 Uiso 1 d R . . C35 C 0.4073(7) 0.1414(2) 1.176(3) 0.087(7) Uani 1 d . . . H35 H 0.4393 0.1488 1.2042 0.105 Uiso 1 d R . . C36 C 0.4165(6) 0.1242(2) 1.109(2) 0.063(5) Uani 1 d . . . H36 H 0.4543 0.1200 1.0905 0.076 Uiso 1 d R . . C37 C 0.3638(6) 0.09602(17) 0.7922(14) 0.041(3) Uani 1 d . . . C38 C 0.4045(8) 0.0970(2) 0.687(2) 0.072(5) Uani 1 d . . . H38 H 0.4432 0.0945 0.7128 0.086 Uiso 1 d R . . C39 C 0.3902(10) 0.1011(3) 0.543(2) 0.101(7) Uani 1 d . . . H39 H 0.4182 0.1013 0.4662 0.121 Uiso 1 d R . . C40 C 0.3353(10) 0.1053(3) 0.510(2) 0.091(7) Uani 1 d . . . H40 H 0.3247 0.1084 0.4110 0.109 Uiso 1 d R . . C41 C 0.2945(9) 0.1043(3) 0.611(2) 0.088(6) Uani 1 d . . . H41 H 0.2561 0.1075 0.5870 0.106 Uiso 1 d R . . C42 C 0.3094(7) 0.0997(2) 0.753(2) 0.070(5) Uani 1 d . . . H42 H 0.2806 0.0987 0.8267 0.085 Uiso 1 d 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 Rb 0.0498(7) 0.0457(7) 0.0515(8) -0.0040(8) 0.0005(8) 0.0011(6) Se1 0.0563(8) 0.0463(8) 0.0531(9) -0.0157(9) -0.0066(9) -0.0018(7) Se2 0.0767(10) 0.0466(8) 0.0620(10) 0.0012(10) 0.0182(11) -0.0192(8) P1 0.0404(19) 0.035(2) 0.036(2) -0.0017(16) -0.0025(16) 0.0029(16) P2 0.0419(19) 0.0281(17) 0.041(2) -0.0010(16) -0.0019(17) 0.0015(15) N1 0.043(6) 0.026(6) 0.069(8) -0.013(6) -0.011(6) 0.004(5) O1 0.101(9) 0.058(7) 0.058(7) 0.012(6) 0.000(7) -0.020(7) C2 0.134(19) 0.060(13) 0.083(15) 0.011(11) -0.002(14) -0.021(13) C3 0.136(17) 0.039(8) 0.081(13) 0.019(11) -0.028(15) 0.017(10) O4 0.070(8) 0.075(8) 0.055(7) -0.004(6) -0.019(6) 0.018(6) C5 0.049(10) 0.078(12) 0.115(19) -0.018(12) -0.009(12) 0.013(8) C6 0.050(9) 0.056(11) 0.101(14) -0.024(11) 0.014(11) 0.010(8) O7 0.058(6) 0.059(7) 0.049(6) -0.005(6) -0.001(5) -0.007(5) C8 0.058(11) 0.086(14) 0.066(12) -0.004(10) 0.011(9) -0.001(9) C9 0.069(11) 0.062(11) 0.060(11) 0.023(9) 0.002(9) -0.030(9) O10 0.063(6) 0.047(6) 0.078(7) 0.009(7) 0.004(7) -0.010(5) C11 0.105(14) 0.048(9) 0.099(14) 0.028(12) -0.042(15) 0.001(10) C12 0.064(12) 0.086(14) 0.111(19) 0.008(12) -0.042(12) 0.028(11) O13 0.040(6) 0.047(6) 0.121(11) -0.015(7) -0.014(7) 0.004(5) C14 0.053(10) 0.063(11) 0.14(2) -0.029(13) 0.006(13) 0.012(8) C15 0.049(10) 0.068(12) 0.121(19) -0.042(12) 0.035(11) -0.002(8) O16 0.069(7) 0.087(9) 0.065(9) -0.040(7) 0.023(7) -0.014(6) C17 0.077(13) 0.106(17) 0.077(15) -0.025(13) 0.038(11) -0.013(12) C18 0.117(18) 0.17(3) 0.042(11) 0.035(14) -0.019(11) -0.067(18) C19 0.036(8) 0.037(8) 0.045(8) -0.003(7) -0.008(6) 0.004(6) C20 0.060(10) 0.076(12) 0.039(9) 0.008(8) 0.016(8) 0.020(9) C21 0.076(11) 0.057(10) 0.074(14) 0.019(10) 0.003(11) 0.011(8) C22 0.069(11) 0.072(12) 0.032(8) 0.023(8) -0.016(8) -0.004(9) C23 0.080(13) 0.066(12) 0.054(11) -0.009(9) 0.004(9) -0.006(10) C24 0.102(13) 0.043(9) 0.032(9) 0.000(7) -0.014(8) 0.000(9) C25 0.029(6) 0.029(7) 0.037(7) -0.015(6) -0.007(5) 0.006(5) C26 0.059(10) 0.040(8) 0.085(12) -0.011(8) -0.011(9) 0.013(8) C27 0.044(9) 0.048(9) 0.101(14) -0.010(10) -0.019(10) -0.003(8) C28 0.045(9) 0.074(11) 0.060(11) 0.015(9) -0.003(8) -0.013(8) C29 0.051(9) 0.094(13) 0.063(12) -0.004(10) 0.014(9) 0.003(9) C30 0.056(9) 0.051(8) 0.060(9) -0.016(10) -0.006(10) 0.006(7) C31 0.043(7) 0.031(7) 0.062(9) 0.007(8) 0.010(9) -0.006(6) C32 0.048(8) 0.056(9) 0.077(13) -0.011(9) -0.020(9) -0.004(7) C33 0.059(10) 0.059(10) 0.065(11) -0.019(9) -0.016(9) 0.021(8) C34 0.089(13) 0.037(9) 0.081(13) -0.024(9) -0.029(11) 0.022(9) C35 0.061(11) 0.046(10) 0.15(2) -0.038(12) -0.014(12) -0.008(9) C36 0.038(8) 0.053(9) 0.098(15) -0.015(9) 0.018(9) 0.002(7) C37 0.061(8) 0.029(7) 0.034(9) -0.005(6) -0.013(7) 0.005(6) C38 0.069(12) 0.085(14) 0.061(12) 0.032(11) 0.003(9) 0.025(10) C39 0.126(19) 0.098(16) 0.079(17) 0.022(13) 0.035(15) 0.027(14) C40 0.14(2) 0.090(15) 0.045(11) 0.007(10) -0.002(13) 0.027(15) C41 0.092(14) 0.110(16) 0.062(14) 0.007(11) -0.030(11) 0.001(13) C42 0.057(10) 0.086(13) 0.068(12) 0.002(10) 0.001(9) -0.002(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rb O4 2.872(10) . ? Rb O10 2.932(12) . ? Rb O16 2.958(10) . ? Rb O13 3.079(10) . ? Rb O1 3.084(11) . ? Rb O7 3.113(10) . ? Rb Se1 3.483(2) . ? Rb Se2 3.520(2) . ? Rb C2 3.57(2) . ? Rb C18 3.656(19) . ? Rb C8 3.682(17) . ? Rb C6 3.727(15) . ? Se1 P1 2.136(4) . ? Se2 P2 2.141(4) . ? P1 N1 1.585(10) . ? P1 C19 1.834(14) . ? P1 C25 1.845(13) . ? P2 N1 1.599(11) . ? P2 C31 1.825(14) . ? P2 C37 1.832(13) . ? O1 C2 1.41(2) . ? O1 C18 1.47(2) . ? C2 C3 1.50(3) . ? C3 O4 1.42(2) . ? O4 C5 1.43(2) . ? C5 C6 1.45(3) . ? C6 O7 1.409(18) . ? O7 C8 1.406(19) . ? C8 C9 1.48(2) . ? C9 O10 1.432(18) . ? O10 C11 1.440(16) . ? C11 C12 1.47(3) . ? C12 O13 1.45(2) . ? O13 C14 1.450(19) . ? C14 C15 1.50(3) . ? C15 O16 1.42(2) . ? O16 C17 1.34(2) . ? C17 C18 1.51(3) . ? C19 C20 1.36(2) . ? C19 C24 1.373(19) . ? C20 C21 1.39(2) . ? C21 C22 1.36(2) . ? C22 C23 1.41(2) . ? C23 C24 1.34(2) . ? C25 C30 1.341(18) . ? C25 C26 1.393(18) . ? C26 C27 1.36(2) . ? C27 C28 1.35(2) . ? C28 C29 1.37(2) . ? C29 C30 1.41(2) . ? C31 C36 1.351(18) . ? C31 C32 1.401(19) . ? C32 C33 1.357(19) . ? C33 C34 1.34(2) . ? C34 C35 1.35(2) . ? C35 C36 1.41(2) . ? C37 C38 1.36(2) . ? C37 C42 1.36(2) . ? C38 C39 1.39(3) . ? C39 C40 1.37(3) . ? C40 C41 1.33(3) . ? C41 C42 1.38(2) . ? 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 O4 Rb O10 111.1(3) . . ? O4 Rb O16 112.2(4) . . ? O10 Rb O16 112.1(3) . . ? O4 Rb O13 137.1(3) . . ? O10 Rb O13 56.7(3) . . ? O16 Rb O13 55.9(4) . . ? O4 Rb O1 56.8(3) . . ? O10 Rb O1 140.2(3) . . ? O16 Rb O1 56.3(4) . . ? O13 Rb O1 104.0(3) . . ? O4 Rb O7 55.6(3) . . ? O10 Rb O7 56.0(3) . . ? O16 Rb O7 138.6(3) . . ? O13 Rb O7 103.6(3) . . ? O1 Rb O7 105.0(3) . . ? O4 Rb Se1 132.4(2) . . ? O10 Rb Se1 112.4(2) . . ? O16 Rb Se1 67.2(2) . . ? O13 Rb Se1 84.41(19) . . ? O1 Rb Se1 98.0(2) . . ? O7 Rb Se1 152.8(2) . . ? O4 Rb Se2 84.6(2) . . ? O10 Rb Se2 87.2(2) . . ? O16 Rb Se2 145.4(2) . . ? O13 Rb Se2 130.1(2) . . ? O1 Rb Se2 124.7(2) . . ? O7 Rb Se2 75.9(2) . . ? Se1 Rb Se2 79.09(5) . . ? O4 Rb C2 41.9(4) . . ? O10 Rb C2 148.9(4) . . ? O16 Rb C2 76.6(4) . . ? O13 Rb C2 127.1(4) . . ? O1 Rb C2 23.1(4) . . ? O7 Rb C2 97.0(4) . . ? Se1 Rb C2 98.6(4) . . ? Se2 Rb C2 101.9(3) . . ? O4 Rb C18 78.4(5) . . ? O10 Rb C18 146.8(5) . . ? O16 Rb C18 39.3(5) . . ? O13 Rb C18 94.1(5) . . ? O1 Rb C18 23.3(4) . . ? O7 Rb C18 128.3(4) . . ? Se1 Rb C18 75.9(3) . . ? Se2 Rb C18 125.9(4) . . ? C2 Rb C18 38.2(5) . . ? O4 Rb C8 75.4(4) . . ? O10 Rb C8 40.1(3) . . ? O16 Rb C8 146.1(4) . . ? O13 Rb C8 95.3(4) . . ? O1 Rb C8 126.9(4) . . ? O7 Rb C8 21.9(3) . . ? Se1 Rb C8 133.3(3) . . ? Se2 Rb C8 65.6(3) . . ? C2 Rb C8 117.3(5) . . ? C18 Rb C8 150.1(4) . . ? O4 Rb C6 39.2(4) . . ? O10 Rb C6 75.8(4) . . ? O16 Rb C6 144.8(4) . . ? O13 Rb C6 124.9(3) . . ? O1 Rb C6 94.9(4) . . ? O7 Rb C6 21.5(3) . . ? Se1 Rb C6 143.8(3) . . ? Se2 Rb C6 65.8(3) . . ? C2 Rb C6 80.9(5) . . ? C18 Rb C6 117.3(5) . . ? C8 Rb C6 36.9(4) . . ? P1 Se1 Rb 113.93(11) . . ? P2 Se2 Rb 103.25(12) . . ? N1 P1 C19 108.4(6) . . ? N1 P1 C25 103.0(6) . . ? C19 P1 C25 104.2(6) . . ? N1 P1 Se1 120.9(4) . . ? C19 P1 Se1 109.5(4) . . ? C25 P1 Se1 109.5(4) . . ? N1 P2 C31 105.2(6) . . ? N1 P2 C37 108.6(6) . . ? C31 P2 C37 102.9(7) . . ? N1 P2 Se2 119.6(4) . . ? C31 P2 Se2 108.4(4) . . ? C37 P2 Se2 110.7(5) . . ? P1 N1 P2 134.7(7) . . ? C2 O1 C18 110.0(15) . . ? C2 O1 Rb 98.0(10) . . ? C18 O1 Rb 100.7(9) . . ? O1 C2 C3 108.6(15) . . ? O1 C2 Rb 58.9(9) . . ? C3 C2 Rb 86.4(11) . . ? O4 C3 C2 110.5(16) . . ? C3 O4 C5 115.5(14) . . ? C3 O4 Rb 119.6(11) . . ? C5 O4 Rb 123.4(10) . . ? O4 C5 C6 109.4(14) . . ? O7 C6 C5 110.7(14) . . ? O7 C6 Rb 53.9(7) . . ? C5 C6 Rb 83.9(10) . . ? C8 O7 C6 112.8(14) . . ? C8 O7 Rb 102.5(9) . . ? C6 O7 Rb 104.6(9) . . ? O7 C8 C9 110.3(15) . . ? O7 C8 Rb 55.6(7) . . ? C9 C8 Rb 85.9(9) . . ? O10 C9 C8 109.2(12) . . ? C9 O10 C11 114.4(12) . . ? C9 O10 Rb 121.1(8) . . ? C11 O10 Rb 118.2(12) . . ? O10 C11 C12 111.4(14) . . ? O13 C12 C11 105.3(14) . . ? O13 C12 Rb 52.7(7) . . ? C11 C12 Rb 82.5(9) . . ? C12 O13 C14 110.2(14) . . ? C12 O13 Rb 105.3(9) . . ? C14 O13 Rb 106.0(9) . . ? O13 C14 C15 110.2(15) . . ? O13 C14 Rb 52.2(7) . . ? C15 C14 Rb 85.1(10) . . ? O16 C15 C14 109.3(15) . . ? C17 O16 C15 112.0(14) . . ? C17 O16 Rb 121.2(11) . . ? C15 O16 Rb 122.6(11) . . ? O16 C17 C18 108.6(16) . . ? O1 C18 C17 107.7(16) . . ? O1 C18 Rb 56.0(8) . . ? C17 C18 Rb 85.0(11) . . ? C20 C19 C24 119.7(14) . . ? C20 C19 P1 120.7(11) . . ? C24 C19 P1 119.6(10) . . ? C19 C20 C21 119.8(15) . . ? C22 C21 C20 121.3(15) . . ? C21 C22 C23 116.8(15) . . ? C24 C23 C22 121.9(16) . . ? C23 C24 C19 120.3(15) . . ? C30 C25 C26 117.0(13) . . ? C30 C25 P1 123.6(10) . . ? C26 C25 P1 119.3(10) . . ? C27 C26 C25 121.4(15) . . ? C28 C27 C26 120.4(16) . . ? C27 C28 C29 120.7(15) . . ? C28 C29 C30 117.4(15) . . ? C25 C30 C29 123.1(14) . . ? C36 C31 C32 117.9(13) . . ? C36 C31 P2 121.9(10) . . ? C32 C31 P2 120.2(10) . . ? C33 C32 C31 120.7(14) . . ? C34 C33 C32 121.4(15) . . ? C33 C34 C35 119.6(15) . . ? C34 C35 C36 120.4(15) . . ? C31 C36 C35 120.0(13) . . ? C38 C37 C42 118.2(14) . . ? C38 C37 P2 121.6(11) . . ? C42 C37 P2 120.2(12) . . ? C37 C38 C39 120.3(17) . . ? C40 C39 C38 119.2(19) . . ? C41 C40 C39 121.4(19) . . ? C40 C41 C42 118.3(19) . . ? C37 C42 C41 122.4(17) . . ? _diffrn_measured_fraction_theta_max 0.254 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.254 _refine_diff_density_max 0.454 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.102 #==END data_compound5 _database_code_depnum_ccdc_archive 'CCDC 220672' _chemical_name_common "Rubidium(18-crown-6) imidobis(diphenylthiophosphinate-S,S')" _audit_creation_method SHELXL-97 _chemical_name_systematic ; Rubidium(18-crown-6) imidobis(diphenylthiophosphinate-S,S') ; _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 N O6 P2 Rb S2' _chemical_formula_weight 798.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 23.534(2) _cell_length_b 72.099(5) _cell_length_c 9.043(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15344(4) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 5.00 _cell_measurement_theta_max 12.50 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6624 _exptl_absorpt_coefficient_mu 1.527 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.511 _exptl_absorpt_correction_T_max 0.818 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4/PC diffractometer' _diffrn_measurement_method \q:2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4 _diffrn_reflns_number 6424 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.1624 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -85 _diffrn_reflns_limit_k_max 85 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5994 _reflns_number_gt 3321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS ver 2.1 1993' _computing_cell_refinement 'XSCANS ver 2.1 1993' _computing_data_reduction 'XSCANS ver 2.1 1993' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V 6.10' _computing_publication_material 'SHELXTL V 6.10' _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 w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+13.9480P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00015(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.019(15) _refine_ls_number_reflns 5994 _refine_ls_number_parameters 434 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1617 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rb Rb -0.07142(5) 0.213409(16) 0.17545(13) 0.0459(3) Uani 1 d . . . S1 S -0.21074(12) 0.20109(4) 0.1693(4) 0.0512(8) Uani 1 d . . . S2 S -0.06844(14) 0.17789(4) -0.0714(4) 0.0588(8) Uani 1 d . . . P1 P -0.22990(11) 0.18170(4) 0.0225(3) 0.0358(7) Uani 1 d . . . P2 P -0.12390(12) 0.16025(4) 0.0106(3) 0.0339(7) Uani 1 d . . . N1 N -0.1907(3) 0.16384(13) -0.0016(11) 0.045(2) Uani 1 d . . . O1 O -0.0429(4) 0.21019(14) 0.5097(10) 0.070(3) Uani 1 d . . . C2 C -0.0195(8) 0.1918(2) 0.5053(18) 0.096(6) Uani 1 d . . . H2A H -0.0174 0.1872 0.6039 0.115 Uiso 1 d R . . H2B H -0.0440 0.1840 0.4494 0.115 Uiso 1 d R . . C3 C 0.0390(7) 0.1929(2) 0.4396(17) 0.078(4) Uani 1 d . . . H3A H 0.0624 0.2016 0.4909 0.093 Uiso 1 d R . . H3B H 0.0563 0.1810 0.4468 0.093 Uiso 1 d R . . O4 O 0.0319(4) 0.19748(13) 0.2900(10) 0.060(3) Uani 1 d . . . C5 C 0.0840(5) 0.19761(19) 0.2123(15) 0.068(5) Uani 1 d . . . H5A H 0.1072 0.2075 0.2474 0.081 Uiso 1 d R . . H5B H 0.1035 0.1863 0.2308 0.081 Uiso 1 d R . . C6 C 0.0738(5) 0.19936(19) 0.0505(16) 0.060(4) Uani 1 d . . . H6A H 0.1092 0.1985 -0.0011 0.072 Uiso 1 d R . . H6B H 0.0498 0.1896 0.0166 0.072 Uiso 1 d R . . O7 O 0.0478(3) 0.21693(12) 0.0238(10) 0.053(2) Uani 1 d . . . C8 C 0.0321(5) 0.2189(2) -0.1305(14) 0.059(4) Uani 1 d . . . H8A H 0.0651 0.2174 -0.1911 0.071 Uiso 1 d R . . H8B H 0.0049 0.2097 -0.1568 0.071 Uiso 1 d R . . C9 C 0.0064(5) 0.23727(19) -0.1487(16) 0.062(4) Uani 1 d . . . H9A H 0.0315 0.2464 -0.1098 0.075 Uiso 1 d R . . H9B H 0.0013 0.2396 -0.2518 0.075 Uiso 1 d R . . O10 O -0.0471(3) 0.23801(10) -0.0767(11) 0.055(2) Uani 1 d . . . C11 C -0.0716(6) 0.25575(17) -0.0835(17) 0.067(4) Uani 1 d . . . H11A H -0.0485 0.2642 -0.0289 0.081 Uiso 1 d R . . H11B H -0.0737 0.2600 -0.1832 0.081 Uiso 1 d R . . C12 C -0.1277(6) 0.2555(2) -0.0064(18) 0.075(5) Uani 1 d . . . H12A H -0.1478 0.2667 -0.0257 0.090 Uiso 1 d R . . H12B H -0.1490 0.2454 -0.0452 0.090 Uiso 1 d R . . O13 O -0.1201(3) 0.25284(11) 0.1436(10) 0.053(2) Uani 1 d . . . C14 C -0.1723(5) 0.2522(2) 0.2262(18) 0.074(5) Uani 1 d . . . H14A H -0.1918 0.2636 0.2095 0.089 Uiso 1 d R . . H14B H -0.1956 0.2424 0.1904 0.089 Uiso 1 d R . . C15 C -0.1619(6) 0.2501(2) 0.385(2) 0.081(5) Uani 1 d . . . H15A H -0.1378 0.2598 0.4198 0.097 Uiso 1 d R . . H15B H -0.1969 0.2507 0.4387 0.097 Uiso 1 d R . . O16 O -0.1339(3) 0.23312(13) 0.4106(11) 0.064(2) Uani 1 d . . . C17 C -0.1231(6) 0.2298(3) 0.5568(19) 0.086(5) Uani 1 d . . . H17A H -0.0937 0.2381 0.5876 0.103 Uiso 1 d R . . H17B H -0.1558 0.2317 0.6175 0.103 Uiso 1 d R . . C18 C -0.0982(7) 0.2109(3) 0.5792(17) 0.093(6) Uani 1 d . . . H18A H -0.1220 0.2031 0.5207 0.112 Uiso 1 d R . . H18B H -0.0982 0.2065 0.6786 0.112 Uiso 1 d R . . C19 C -0.2417(4) 0.19232(18) -0.1565(13) 0.039(3) Uani 1 d . . . C20 C -0.2606(5) 0.21065(18) -0.1739(14) 0.051(4) Uani 1 d . . . H20 H -0.2663 0.2177 -0.0860 0.061 Uiso 1 d R . . C21 C -0.2710(5) 0.21806(18) -0.3120(19) 0.069(4) Uani 1 d . . . H21 H -0.2812 0.2308 -0.3194 0.083 Uiso 1 d R . . C22 C -0.2620(5) 0.2077(2) -0.4349(17) 0.063(4) Uani 1 d . . . H22 H -0.2688 0.2130 -0.5297 0.076 Uiso 1 d R . . C23 C -0.2428(5) 0.19006(18) -0.4223(14) 0.052(3) Uani 1 d . . . H23 H -0.2381 0.1827 -0.5090 0.062 Uiso 1 d R . . C24 C -0.2328(5) 0.18220(18) -0.2861(11) 0.051(3) Uani 1 d . . . H24 H -0.2201 0.1697 -0.2783 0.061 Uiso 1 d R . . C25 C -0.2990(4) 0.17148(13) 0.0656(11) 0.030(2) Uani 1 d . . . C26 C -0.3158(5) 0.15577(16) -0.0050(13) 0.050(3) Uani 1 d . . . H26 H -0.2925 0.1505 -0.0805 0.060 Uiso 1 d R . . C27 C -0.3674(5) 0.14722(18) 0.0307(17) 0.065(4) Uani 1 d . . . H27 H -0.3792 0.1364 -0.0204 0.078 Uiso 1 d R . . C28 C -0.4012(5) 0.1540(2) 0.1380(14) 0.055(4) Uani 1 d . . . H28 H -0.4363 0.1481 0.1613 0.066 Uiso 1 d R . . C29 C -0.3840(5) 0.1698(2) 0.2075(14) 0.068(4) Uani 1 d . . . H29 H -0.4077 0.1750 0.2820 0.081 Uiso 1 d R . . C30 C -0.3337(5) 0.17898(17) 0.1727(16) 0.055(3) Uani 1 d . . . H30 H -0.3225 0.1902 0.2198 0.066 Uiso 1 d R . . C31 C -0.1142(4) 0.13765(13) -0.0785(13) 0.035(2) Uani 1 d . . . C32 C -0.0610(4) 0.13138(16) -0.1099(13) 0.051(3) Uani 1 d . . . H32 H -0.0289 0.1390 -0.0891 0.061 Uiso 1 d R . . C33 C -0.0507(6) 0.1140(2) -0.1686(17) 0.073(5) Uani 1 d . . . H33 H -0.0132 0.1095 -0.1876 0.088 Uiso 1 d R . . C34 C -0.0962(5) 0.10259(19) -0.1992(17) 0.067(4) Uani 1 d . . . H34 H -0.0907 0.0906 -0.2406 0.080 Uiso 1 d R . . C35 C -0.1493(6) 0.10913(19) -0.176(2) 0.084(5) Uani 1 d . . . H35 H -0.1812 0.1018 -0.2039 0.101 Uiso 1 d R . . C36 C -0.1588(5) 0.12638(16) -0.1126(15) 0.057(4) Uani 1 d . . . H36 H -0.1967 0.1306 -0.0939 0.068 Uiso 1 d R . . C37 C -0.1075(4) 0.15519(15) 0.2037(12) 0.038(3) Uani 1 d . . . C38 C -0.1479(6) 0.1543(2) 0.3116(15) 0.071(4) Uani 1 d . . . H38 H -0.1865 0.1567 0.2857 0.085 Uiso 1 d R . . C39 C -0.1330(7) 0.1491(2) 0.4561(15) 0.077(5) Uani 1 d . . . H39 H -0.1609 0.1489 0.5327 0.093 Uiso 1 d R . . C40 C -0.0795(8) 0.1447(2) 0.4920(17) 0.083(5) Uani 1 d . . . H40 H -0.0690 0.1416 0.5907 0.099 Uiso 1 d R . . C41 C -0.0371(7) 0.1455(2) 0.3884(15) 0.076(5) Uani 1 d . . . H41 H 0.0012 0.1423 0.4123 0.091 Uiso 1 d R . . C42 C -0.0515(5) 0.15129(19) 0.2462(15) 0.060(4) Uani 1 d . . . H42 H -0.0228 0.1522 0.1721 0.071 Uiso 1 d 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 Rb 0.0458(5) 0.0427(6) 0.0491(6) -0.0064(7) 0.0000(7) 0.0002(6) S1 0.0546(16) 0.0426(17) 0.0563(18) -0.023(2) -0.0132(19) 0.0011(14) S2 0.0738(19) 0.0479(18) 0.0548(18) 0.002(2) 0.011(2) -0.0212(17) P1 0.0379(15) 0.0276(16) 0.0419(17) -0.0086(15) -0.0075(15) 0.0061(13) P2 0.0377(14) 0.0291(15) 0.0348(15) -0.0004(14) -0.0023(14) 0.0032(13) N1 0.032(4) 0.042(6) 0.060(6) -0.005(5) -0.015(5) 0.007(4) O1 0.077(6) 0.074(7) 0.058(5) -0.002(6) 0.019(5) -0.034(5) C2 0.182(18) 0.045(10) 0.061(9) 0.032(9) -0.015(12) -0.039(11) C3 0.113(12) 0.054(9) 0.066(10) 0.017(9) -0.036(11) 0.010(9) O4 0.063(6) 0.062(7) 0.056(6) 0.002(5) -0.022(5) 0.007(5) C5 0.066(9) 0.046(8) 0.091(13) -0.022(8) -0.031(8) 0.028(7) C6 0.046(7) 0.051(9) 0.082(10) -0.011(8) -0.003(8) -0.005(7) O7 0.050(4) 0.044(5) 0.065(6) -0.006(5) 0.000(5) 0.002(4) C8 0.053(7) 0.073(11) 0.051(8) 0.000(8) 0.003(7) -0.018(7) C9 0.068(8) 0.068(11) 0.052(8) 0.016(8) 0.008(8) -0.018(8) O10 0.050(4) 0.049(5) 0.065(5) 0.006(6) -0.004(5) -0.006(4) C11 0.085(9) 0.058(8) 0.059(8) 0.005(9) -0.025(10) 0.007(8) C12 0.075(9) 0.049(9) 0.101(13) -0.008(9) -0.042(10) 0.023(8) O13 0.042(4) 0.047(5) 0.069(6) -0.014(5) -0.013(5) 0.012(4) C14 0.034(6) 0.063(9) 0.125(15) -0.033(10) -0.009(8) 0.009(6) C15 0.047(8) 0.074(11) 0.122(16) -0.042(12) 0.029(9) -0.003(7) O16 0.062(5) 0.068(6) 0.061(6) -0.031(6) 0.011(6) -0.007(5) C17 0.061(9) 0.115(16) 0.081(12) -0.032(12) 0.023(9) -0.019(10) C18 0.099(12) 0.125(17) 0.056(9) 0.018(11) -0.007(9) -0.050(12) C19 0.030(5) 0.047(8) 0.041(6) -0.005(7) -0.010(5) -0.004(6) C20 0.057(8) 0.037(7) 0.058(8) 0.001(7) 0.025(7) 0.016(6) C21 0.069(8) 0.051(9) 0.088(11) 0.036(10) 0.008(10) 0.025(7) C22 0.042(7) 0.083(12) 0.064(9) 0.012(9) 0.008(7) 0.005(8) C23 0.074(8) 0.040(8) 0.042(7) -0.012(7) -0.004(7) -0.002(7) C24 0.075(8) 0.044(7) 0.033(7) 0.003(6) 0.003(6) 0.022(7) C25 0.037(5) 0.017(5) 0.037(6) 0.004(5) -0.014(5) -0.003(5) C26 0.044(6) 0.050(8) 0.057(7) -0.016(7) 0.001(6) 0.015(6) C27 0.057(8) 0.038(7) 0.101(11) -0.013(9) -0.014(9) -0.005(6) C28 0.044(6) 0.065(9) 0.056(9) 0.001(8) -0.001(7) -0.002(7) C29 0.066(8) 0.095(11) 0.043(8) -0.009(8) 0.011(7) 0.013(8) C30 0.057(7) 0.053(7) 0.055(7) -0.005(9) 0.000(8) -0.004(6) C31 0.055(6) 0.024(5) 0.027(5) -0.006(6) -0.013(6) 0.006(5) C32 0.040(6) 0.045(7) 0.068(9) -0.017(7) 0.002(6) 0.007(5) C33 0.059(8) 0.071(10) 0.091(11) -0.030(10) -0.005(8) 0.031(8) C34 0.066(8) 0.042(8) 0.092(11) -0.019(8) -0.006(8) 0.026(7) C35 0.065(8) 0.046(9) 0.143(15) -0.046(10) -0.018(10) -0.006(7) C36 0.050(6) 0.038(7) 0.083(10) -0.033(7) -0.011(7) 0.000(6) C37 0.044(6) 0.034(6) 0.035(6) -0.002(5) -0.008(6) 0.003(5) C38 0.066(9) 0.090(12) 0.056(9) 0.007(9) 0.009(8) 0.018(9) C39 0.116(13) 0.071(11) 0.046(9) 0.009(8) 0.027(9) 0.003(10) C40 0.142(15) 0.054(9) 0.052(9) 0.012(8) -0.032(12) 0.005(11) C41 0.079(9) 0.100(13) 0.047(10) 0.006(9) -0.025(8) -0.011(10) C42 0.050(7) 0.070(10) 0.058(8) -0.005(8) -0.011(7) 0.000(7) _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 Rb O4 2.882(8) . ? Rb O10 2.945(9) . ? Rb O16 2.950(9) . ? Rb O13 3.078(8) . ? Rb O1 3.105(9) . ? Rb O7 3.133(8) . ? Rb S1 3.398(3) . ? Rb S2 3.398(4) . ? Rb C2 3.579(15) . ? Rb C12 3.696(14) . ? Rb C14 3.699(13) . ? Rb C8 3.708(13) . ? S1 P1 1.980(4) . ? S2 P2 1.967(4) . ? P1 N1 1.598(9) . ? P1 C19 1.812(12) . ? P1 C25 1.828(10) . ? P2 N1 1.598(8) . ? P2 C37 1.825(11) . ? P2 C31 1.832(10) . ? O1 C2 1.435(18) . ? O1 C18 1.447(17) . ? C2 C3 1.50(2) . ? C3 O4 1.402(15) . ? O4 C5 1.412(15) . ? C5 C6 1.488(19) . ? C6 O7 1.428(15) . ? O7 C8 1.450(14) . ? C8 C9 1.465(18) . ? C9 O10 1.418(14) . ? O10 C11 1.405(13) . ? C11 C12 1.492(19) . ? C12 O13 1.381(16) . ? O13 C14 1.439(14) . ? C14 C15 1.47(2) . ? C15 O16 1.410(17) . ? O16 C17 1.367(19) . ? C17 C18 1.50(2) . ? C19 C24 1.396(15) . ? C19 C20 1.404(17) . ? C20 C21 1.380(18) . ? C21 C22 1.36(2) . ? C22 C23 1.354(19) . ? C23 C24 1.376(16) . ? C25 C26 1.359(15) . ? C25 C30 1.376(15) . ? C26 C27 1.399(16) . ? C27 C28 1.346(17) . ? C28 C29 1.359(18) . ? C29 C30 1.394(16) . ? C31 C32 1.362(14) . ? C31 C36 1.362(14) . ? C32 C33 1.384(17) . ? C33 C34 1.377(18) . ? C34 C35 1.350(17) . ? C35 C36 1.389(17) . ? C37 C38 1.362(16) . ? C37 C42 1.402(14) . ? C38 C39 1.404(19) . ? C39 C40 1.34(2) . ? C40 C41 1.370(19) . ? C41 C42 1.394(18) . ? 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 O4 Rb O10 110.8(2) . . ? O4 Rb O16 110.7(3) . . ? O10 Rb O16 111.4(3) . . ? O4 Rb O13 135.7(2) . . ? O10 Rb O13 56.2(2) . . ? O16 Rb O13 55.7(3) . . ? O4 Rb O1 55.8(3) . . ? O10 Rb O1 139.2(2) . . ? O16 Rb O1 56.1(3) . . ? O13 Rb O1 103.9(3) . . ? O4 Rb O7 55.5(2) . . ? O10 Rb O7 55.8(2) . . ? O16 Rb O7 136.3(2) . . ? O13 Rb O7 102.6(2) . . ? O1 Rb O7 103.8(2) . . ? O4 Rb S1 135.7(2) . . ? O10 Rb S1 109.41(16) . . ? O16 Rb S1 69.94(17) . . ? O13 Rb S1 83.16(15) . . ? O1 Rb S1 101.84(17) . . ? O7 Rb S1 151.43(16) . . ? O4 Rb S2 85.32(19) . . ? O10 Rb S2 86.63(18) . . ? O16 Rb S2 147.88(17) . . ? O13 Rb S2 129.96(17) . . ? O1 Rb S2 125.4(2) . . ? O7 Rb S2 75.82(16) . . ? S1 Rb S2 79.17(8) . . ? O4 Rb C2 40.5(4) . . ? O10 Rb C2 147.2(3) . . ? O16 Rb C2 77.2(4) . . ? O13 Rb C2 127.3(3) . . ? O1 Rb C2 23.4(3) . . ? O7 Rb C2 95.4(4) . . ? S1 Rb C2 103.3(3) . . ? S2 Rb C2 102.3(3) . . ? O4 Rb C12 142.1(3) . . ? O10 Rb C12 39.7(3) . . ? O16 Rb C12 75.3(3) . . ? O13 Rb C12 21.1(3) . . ? O1 Rb C12 124.9(3) . . ? O7 Rb C12 93.4(3) . . ? S1 Rb C12 82.0(2) . . ? S2 Rb C12 109.5(2) . . ? C2 Rb C12 148.2(4) . . ? O4 Rb C14 143.0(3) . . ? O10 Rb C14 76.4(3) . . ? O16 Rb C14 39.3(3) . . ? O13 Rb C14 22.2(3) . . ? O1 Rb C14 94.3(3) . . ? O7 Rb C14 124.6(3) . . ? S1 Rb C14 65.2(2) . . ? S2 Rb C14 131.7(2) . . ? C2 Rb C14 116.4(4) . . ? C12 Rb C14 37.3(3) . . ? O4 Rb C8 75.9(3) . . ? O10 Rb C8 39.7(3) . . ? O16 Rb C8 144.5(3) . . ? O13 Rb C8 94.4(3) . . ? O1 Rb C8 126.3(3) . . ? O7 Rb C8 22.5(2) . . ? S1 Rb C8 130.6(2) . . ? S2 Rb C8 65.0(2) . . ? C2 Rb C8 116.3(4) . . ? C12 Rb C8 79.4(3) . . ? C14 Rb C8 115.7(3) . . ? P1 S1 Rb 114.54(15) . . ? P2 S2 Rb 103.05(16) . . ? N1 P1 C19 107.9(5) . . ? N1 P1 C25 102.6(5) . . ? C19 P1 C25 103.0(5) . . ? N1 P1 S1 121.9(4) . . ? C19 P1 S1 109.6(4) . . ? C25 P1 S1 110.1(4) . . ? N1 P2 C37 107.8(5) . . ? N1 P2 C31 103.6(5) . . ? C37 P2 C31 102.5(5) . . ? N1 P2 S2 121.5(4) . . ? C37 P2 S2 110.5(4) . . ? C31 P2 S2 109.1(4) . . ? P2 N1 P1 133.5(6) . . ? C2 O1 C18 113.0(13) . . ? C2 O1 Rb 97.1(8) . . ? C18 O1 Rb 103.0(7) . . ? O1 C2 C3 108.3(11) . . ? O1 C2 Rb 59.4(7) . . ? C3 C2 Rb 87.8(8) . . ? O4 C3 C2 106.6(12) . . ? C3 O4 C5 112.2(10) . . ? C3 O4 Rb 122.7(9) . . ? C5 O4 Rb 123.4(7) . . ? O4 C5 C6 110.5(10) . . ? O7 C6 C5 108.1(12) . . ? O7 C6 Rb 54.5(5) . . ? C5 C6 Rb 82.7(8) . . ? C6 O7 C8 111.1(10) . . ? C6 O7 Rb 103.8(7) . . ? C8 O7 Rb 101.6(6) . . ? O7 C8 C9 107.7(12) . . ? O7 C8 Rb 55.9(5) . . ? C9 C8 Rb 84.8(8) . . ? O10 C9 C8 110.5(11) . . ? C11 O10 C9 112.3(10) . . ? C11 O10 Rb 120.2(8) . . ? C9 O10 Rb 120.4(7) . . ? O10 C11 C12 109.3(11) . . ? O13 C12 C11 110.3(11) . . ? O13 C12 Rb 53.4(6) . . ? C11 C12 Rb 84.4(7) . . ? C12 O13 C14 113.8(10) . . ? C12 O13 Rb 105.5(7) . . ? C14 O13 Rb 103.9(7) . . ? O13 C14 C15 111.7(10) . . ? O13 C14 Rb 53.9(6) . . ? C15 C14 Rb 86.3(8) . . ? O16 C15 C14 109.2(13) . . ? C17 O16 C15 113.3(13) . . ? C17 O16 Rb 121.4(9) . . ? C15 O16 Rb 122.2(9) . . ? O16 C17 C18 111.1(14) . . ? O1 C18 C17 109.0(13) . . ? O1 C18 Rb 54.7(6) . . ? C17 C18 Rb 83.7(9) . . ? C24 C19 C20 116.5(11) . . ? C24 C19 P1 120.4(9) . . ? C20 C19 P1 123.1(9) . . ? C21 C20 C19 121.5(12) . . ? C22 C21 C20 120.0(12) . . ? C23 C22 C21 120.0(14) . . ? C22 C23 C24 121.3(13) . . ? C23 C24 C19 120.7(11) . . ? C26 C25 C30 119.0(10) . . ? C26 C25 P1 119.6(9) . . ? C30 C25 P1 121.3(8) . . ? C25 C26 C27 120.7(11) . . ? C28 C27 C26 121.2(12) . . ? C27 C28 C29 117.5(12) . . ? C28 C29 C30 123.1(12) . . ? C25 C30 C29 118.4(12) . . ? C32 C31 C36 117.6(10) . . ? C32 C31 P2 120.0(8) . . ? C36 C31 P2 122.3(8) . . ? C31 C32 C33 122.7(11) . . ? C34 C33 C32 118.8(11) . . ? C35 C34 C33 118.7(12) . . ? C34 C35 C36 121.7(12) . . ? C31 C36 C35 120.2(11) . . ? C38 C37 C42 116.7(11) . . ? C38 C37 P2 123.2(8) . . ? C42 C37 P2 120.0(9) . . ? C37 C38 C39 120.4(13) . . ? C40 C39 C38 121.5(14) . . ? C39 C40 C41 120.7(13) . . ? C40 C41 C42 117.7(13) . . ? C41 C42 C37 122.8(13) . . ? _diffrn_measured_fraction_theta_max 0.227 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.227 _refine_diff_density_max 0.354 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.080 #==END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 220673' _chemical_name_common "(Aquarubidium(18-crown-6)) imidobis(diphenylphosphinate-O,O')" _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Aquarubidium(18-crown-6)] imidobis(diphenylphosphinate-O,O') ; _chemical_formula_moiety ? _chemical_formula_sum 'C36 H46 N O9 P2 Rb' _chemical_formula_weight 784.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.114(4) _cell_length_b 15.598(2) _cell_length_c 24.412(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3851.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 5.00 _cell_measurement_theta_max 12.50 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.420 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.514 _exptl_absorpt_correction_T_max 0.572 _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4/PC diffractometer' _diffrn_measurement_method \q:2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_reflns_number 7620 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.2043 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6777 _reflns_number_gt 3116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS ver 2.1 1993' _computing_cell_refinement 'XSCANS ver 2.1 1993' _computing_data_reduction 'XSCANS ver 2.1 1993' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V 6.10' _computing_publication_material 'SHELXTL V 6.10' _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 w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0033(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 6777 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2032 _refine_ls_R_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.2338 _refine_ls_wR_factor_gt 0.1658 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.301 _refine_ls_shift/su_mean 0.023 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rb Rb 0.77793(13) 0.90206(9) 0.20710(6) 0.0515(4) Uani 1 d . . . P1 P 0.7448(3) 1.1034(2) 0.12032(11) 0.0366(8) Uani 1 d . . . O2 O 0.8131(7) 1.0806(5) 0.1726(3) 0.045(2) Uani 1 d . . . P2 P 0.8106(3) 0.9576(2) 0.05243(15) 0.0406(9) Uani 1 d . . . O3 O 0.8859(8) 0.8999(6) 0.0905(4) 0.053(2) Uani 1 d . . . N1 N 0.7149(11) 1.0286(6) 0.0763(4) 0.042(2) Uani 1 d . . . O1 O 0.4866(9) 0.9008(9) 0.1987(5) 0.080(3) Uani 1 d . . . C2 C 0.419(2) 0.8346(15) 0.1689(10) 0.123(9) Uani 1 d . . . H2A H 0.3473 0.8591 0.1484 0.080 Uiso 1 d R . . H2B H 0.3821 0.7936 0.1940 0.080 Uiso 1 d R . . C3 C 0.512(2) 0.7872(19) 0.1327(9) 0.128(10) Uani 1 d . . . H3A H 0.5519 0.8272 0.1078 0.080 Uiso 1 d R . . H3B H 0.4664 0.7442 0.1119 0.080 Uiso 1 d R . . O4 O 0.6109(14) 0.7489(8) 0.1661(5) 0.084(4) Uani 1 d . . . C5 C 0.692(3) 0.7035(15) 0.1300(9) 0.115(8) Uani 1 d . . . H5A H 0.7367 0.7430 0.1061 0.080 Uiso 1 d R . . H5B H 0.6433 0.6631 0.1083 0.080 Uiso 1 d R . . C6 C 0.792(2) 0.6647(12) 0.1660(8) 0.101(7) Uani 1 d . . . H6A H 0.8421 0.6237 0.1456 0.080 Uiso 1 d R . . H6B H 0.7433 0.6344 0.1938 0.080 Uiso 1 d R . . O7 O 0.8792(13) 0.7260(8) 0.1924(5) 0.089(4) Uani 1 d . . . C8 C 0.973(2) 0.6912(14) 0.2265(12) 0.142(13) Uani 1 d . . . H8A H 1.0246 0.6491 0.2072 0.080 Uiso 1 d R . . H8B H 0.9312 0.6641 0.2572 0.080 Uiso 1 d R . . C9 C 1.054(2) 0.7609(19) 0.2501(11) 0.142(12) Uani 1 d . . . H9A H 1.0836 0.7935 0.2190 0.080 Uiso 1 d R . . H9B H 1.1304 0.7391 0.2688 0.080 Uiso 1 d R . . O10 O 0.9780(12) 0.8175(9) 0.2831(6) 0.097(4) Uani 1 d . . . C11 C 1.047(3) 0.8845(18) 0.3101(13) 0.19(2) Uani 1 d . . . H11A H 1.0798 0.9218 0.2820 0.080 Uiso 1 d R . . H11B H 1.1205 0.8631 0.3307 0.080 Uiso 1 d R . . C12 C 0.959(4) 0.9383(19) 0.3445(13) 0.18(2) Uani 1 d . . . H12A H 1.0091 0.9774 0.3665 0.080 Uiso 1 d R . . H12B H 0.9137 0.8993 0.3685 0.080 Uiso 1 d R . . O13 O 0.8671(16) 0.9809(9) 0.3142(5) 0.099(5) Uani 1 d . . . C14 C 0.767(3) 1.025(2) 0.3458(9) 0.157(16) Uani 1 d . . . H14A H 0.8049 1.0705 0.3670 0.080 Uiso 1 d R . . H14B H 0.7242 0.9862 0.3708 0.080 Uiso 1 d R . . C15 C 0.669(3) 1.0589(15) 0.3119(12) 0.158(15) Uani 1 d . . . H15A H 0.7095 1.0897 0.2823 0.080 Uiso 1 d R . . H15B H 0.6099 1.0966 0.3311 0.080 Uiso 1 d R . . O16 O 0.5953(13) 0.9907(7) 0.2895(6) 0.090(4) Uani 1 d . . . C17 C 0.483(3) 1.0156(16) 0.2598(11) 0.130(10) Uani 1 d . . . H17A H 0.5139 1.0503 0.2299 0.080 Uiso 1 d R . . H17B H 0.4266 1.0503 0.2823 0.080 Uiso 1 d R . . C18 C 0.4091(17) 0.9442(15) 0.2346(10) 0.111(8) Uani 1 d . . . H18A H 0.3832 0.9068 0.2640 0.080 Uiso 1 d R . . H18B H 0.3306 0.9644 0.2166 0.080 Uiso 1 d R . . C19 C 0.8369(12) 1.1890(8) 0.0878(5) 0.039(3) Uani 1 d . . . C20 C 0.9737(13) 1.1917(9) 0.0913(6) 0.052(4) Uani 1 d . . . H20 H 1.0179 1.1528 0.1157 0.080 Uiso 1 d R . . C21 C 1.0475(14) 1.2491(10) 0.0619(6) 0.057(4) Uani 1 d . . . H21 H 1.1422 1.2467 0.0640 0.080 Uiso 1 d R . . C22 C 0.9893(15) 1.3093(10) 0.0293(6) 0.060(4) Uani 1 d . . . H22 H 1.0423 1.3505 0.0100 0.080 Uiso 1 d R . . C23 C 0.8522(16) 1.3082(9) 0.0248(6) 0.061(4) Uani 1 d . . . H23 H 0.8096 1.3496 0.0017 0.080 Uiso 1 d R . . C24 C 0.7796(15) 1.2491(8) 0.0540(5) 0.048(3) Uani 1 d . . . H24 H 0.6850 1.2494 0.0507 0.080 Uiso 1 d R . . C25 C 0.5819(12) 1.1473(9) 0.1347(5) 0.042(3) Uani 1 d . . . C26 C 0.5689(12) 1.2179(8) 0.1697(6) 0.042(3) Uani 1 d . . . H26 H 0.6474 1.2467 0.1820 0.080 Uiso 1 d R . . C27 C 0.4478(15) 1.2465(11) 0.1858(7) 0.074(5) Uani 1 d . . . H27 H 0.4422 1.2941 0.2106 0.080 Uiso 1 d R . . C28 C 0.3375(15) 1.2072(11) 0.1687(6) 0.064(4) Uani 1 d . . . H28 H 0.2526 1.2283 0.1799 0.080 Uiso 1 d R . . C29 C 0.3463(14) 1.1364(10) 0.1333(7) 0.065(4) Uani 1 d . . . H29 H 0.2670 1.1085 0.1211 0.080 Uiso 1 d R . . C30 C 0.4687(13) 1.1078(10) 0.1167(6) 0.055(4) Uani 1 d . . . H30 H 0.4747 1.0588 0.0931 0.080 Uiso 1 d R . . C31 C 0.7054(12) 0.8921(7) 0.0090(4) 0.037(3) Uani 1 d . . . C32 C 0.7579(16) 0.8201(8) -0.0149(6) 0.061(4) Uani 1 d . . . H32 H 0.8499 0.8076 -0.0097 0.080 Uiso 1 d R . . C33 C 0.6820(16) 0.7659(10) -0.0444(7) 0.071(5) Uani 1 d . . . H33 H 0.7185 0.7128 -0.0573 0.080 Uiso 1 d R . . C34 C 0.5509(16) 0.7854(11) -0.0567(6) 0.064(5) Uani 1 d . . . H34 H 0.4995 0.7510 -0.0813 0.080 Uiso 1 d R . . C35 C 0.4991(18) 0.8569(11) -0.0316(8) 0.082(6) Uani 1 d . . . H35 H 0.4063 0.8679 -0.0357 0.080 Uiso 1 d R . . C36 C 0.5739(14) 0.9130(9) -0.0013(6) 0.054(4) Uani 1 d . . . H36 H 0.5365 0.9654 0.0123 0.080 Uiso 1 d R . . C37 C 0.9268(14) 1.0023(9) 0.0034(6) 0.051(4) Uani 1 d . . . C38 C 0.8891(16) 1.0704(10) -0.0301(6) 0.064(4) Uani 1 d . . . H38 H 0.8042 1.0970 -0.0256 0.080 Uiso 1 d R . . C39 C 0.981(2) 1.0970(14) -0.0696(6) 0.090(6) Uani 1 d . . . H39 H 0.9590 1.1445 -0.0929 0.080 Uiso 1 d R . . C40 C 1.097(2) 1.0563(17) -0.0742(9) 0.119(10) Uani 1 d . . . H40 H 1.1525 1.0738 -0.1041 0.080 Uiso 1 d R . . C41 C 1.141(2) 0.9961(14) -0.0390(11) 0.121(10) Uani 1 d . . . H41 H 1.2285 0.9727 -0.0418 0.080 Uiso 1 d R . . C42 C 1.0480(15) 0.9685(11) -0.0040(9) 0.086(6) Uani 1 d . . . H42 H 1.0719 0.9214 0.0193 0.080 Uiso 1 d R . . O43 O 1.0572(11) 0.9806(9) 0.1707(6) 0.116(5) Uani 1 d . . . H43A H 1.0769 0.9622 0.1390 0.080 Uiso 1 d R . . H43B H 1.0515 1.0350 0.1699 0.080 Uiso 1 d 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 Rb 0.0488(7) 0.0501(7) 0.0556(8) 0.0084(8) 0.0019(7) 0.0005(8) P1 0.0356(18) 0.0364(16) 0.0378(17) -0.0024(17) -0.0006(13) 0.0032(17) O2 0.039(5) 0.047(5) 0.049(5) 0.003(4) -0.013(4) 0.008(4) P2 0.043(2) 0.0339(17) 0.045(2) -0.0053(16) 0.0047(16) -0.0023(15) O3 0.063(5) 0.042(4) 0.056(5) 0.003(6) -0.008(5) 0.012(5) N1 0.046(6) 0.037(5) 0.044(6) -0.009(5) 0.006(6) 0.005(5) O1 0.047(5) 0.106(9) 0.088(8) 0.033(9) 0.012(6) 0.019(7) C2 0.067(14) 0.15(2) 0.16(2) 0.010(19) -0.058(15) -0.044(15) C3 0.097(18) 0.20(3) 0.085(17) 0.001(19) 0.012(15) -0.039(19) O4 0.098(10) 0.094(9) 0.060(8) -0.013(7) 0.003(8) -0.039(8) C5 0.15(2) 0.111(18) 0.086(15) -0.009(14) 0.050(17) -0.026(17) C6 0.131(19) 0.080(13) 0.091(14) -0.041(12) 0.063(14) -0.035(14) O7 0.094(9) 0.070(8) 0.101(11) 0.006(7) 0.024(8) 0.021(7) C8 0.090(17) 0.099(17) 0.24(4) 0.04(2) 0.09(2) 0.054(15) C9 0.051(13) 0.20(3) 0.17(3) 0.09(2) -0.001(15) 0.063(17) O10 0.066(8) 0.109(10) 0.115(11) 0.059(10) -0.010(8) -0.006(8) C11 0.16(3) 0.16(3) 0.25(4) 0.12(3) -0.18(3) -0.12(2) C12 0.30(6) 0.11(3) 0.13(3) 0.02(2) -0.10(3) -0.11(3) O13 0.138(12) 0.091(10) 0.069(8) 0.022(8) -0.021(9) -0.050(9) C14 0.21(3) 0.18(3) 0.078(17) -0.065(19) 0.07(2) -0.12(3) C15 0.26(4) 0.073(15) 0.14(3) -0.050(18) 0.08(3) -0.04(2) O16 0.116(10) 0.059(7) 0.094(9) 0.000(8) 0.044(9) 0.006(7) C17 0.114(19) 0.12(2) 0.15(2) 0.043(19) 0.051(18) 0.053(18) C18 0.050(11) 0.15(2) 0.14(2) 0.068(17) 0.010(12) 0.016(13) C19 0.043(7) 0.045(7) 0.031(6) -0.011(6) 0.002(6) 0.003(6) C20 0.040(8) 0.060(9) 0.055(9) -0.002(8) -0.008(7) 0.012(7) C21 0.039(8) 0.069(10) 0.063(10) 0.005(8) 0.015(7) -0.003(8) C22 0.052(9) 0.062(10) 0.066(10) 0.015(9) 0.006(8) -0.003(8) C23 0.079(11) 0.046(8) 0.056(9) 0.009(7) 0.004(8) 0.009(8) C24 0.052(8) 0.056(8) 0.035(7) 0.000(6) -0.009(7) -0.022(8) C25 0.043(8) 0.044(8) 0.040(8) 0.001(6) 0.006(6) 0.004(6) C26 0.029(7) 0.039(7) 0.059(9) -0.006(7) 0.007(6) 0.008(6) C27 0.054(10) 0.066(11) 0.101(15) -0.017(10) 0.018(10) 0.010(9) C28 0.045(9) 0.081(12) 0.065(10) 0.024(9) 0.007(8) 0.022(8) C29 0.038(8) 0.070(11) 0.086(12) 0.001(9) -0.015(8) -0.001(7) C30 0.045(8) 0.058(9) 0.061(9) 0.001(9) -0.003(7) 0.000(8) C31 0.052(7) 0.025(6) 0.034(6) -0.009(5) 0.018(6) -0.009(6) C32 0.062(10) 0.050(8) 0.071(9) -0.011(7) 0.020(8) -0.013(8) C33 0.074(12) 0.053(9) 0.087(12) -0.032(9) 0.013(10) -0.016(8) C34 0.069(11) 0.079(11) 0.046(9) -0.006(9) -0.008(8) -0.036(9) C35 0.065(11) 0.069(11) 0.110(16) -0.018(11) -0.013(11) -0.001(10) C36 0.061(9) 0.043(8) 0.059(9) -0.015(7) -0.016(7) 0.004(8) C37 0.048(9) 0.042(8) 0.063(10) -0.011(7) 0.013(7) -0.003(7) C38 0.065(10) 0.080(12) 0.047(9) -0.012(8) -0.005(8) -0.004(9) C39 0.141(18) 0.095(13) 0.036(8) 0.003(10) 0.019(10) -0.054(16) C40 0.083(15) 0.19(3) 0.090(16) -0.079(16) 0.075(13) -0.065(16) C41 0.093(17) 0.095(17) 0.18(3) 0.011(17) 0.058(18) -0.014(13) C42 0.053(10) 0.073(12) 0.131(18) -0.010(12) 0.034(11) 0.005(9) O43 0.062(8) 0.131(12) 0.153(14) 0.033(11) -0.007(8) 0.001(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rb O2 2.931(8) . ? Rb O1 2.954(10) . ? Rb O7 2.953(12) . ? Rb O13 3.026(13) . ? Rb O3 3.049(9) . ? Rb O10 3.045(12) . ? Rb O16 3.062(12) . ? Rb O4 3.092(11) . ? Rb O43 3.205(12) . ? Rb C3 3.71(3) . ? Rb C17 3.70(2) . ? Rb C15 3.71(2) . ? P1 O2 1.494(8) . ? P1 N1 1.614(10) . ? P1 C19 1.811(13) . ? P1 C25 1.818(13) . ? P2 O3 1.502(9) . ? P2 N1 1.582(10) . ? P2 C37 1.816(14) . ? P2 C31 1.817(12) . ? O1 C18 1.36(2) . ? O1 C2 1.44(2) . ? C2 C3 1.49(3) . ? C3 O4 1.42(3) . ? O4 C5 1.40(2) . ? C5 C6 1.47(3) . ? C6 O7 1.45(2) . ? O7 C8 1.38(3) . ? C8 C9 1.48(3) . ? C9 O10 1.42(3) . ? O10 C11 1.42(3) . ? C11 C12 1.48(4) . ? C12 O13 1.36(3) . ? O13 C14 1.45(3) . ? C14 C15 1.39(4) . ? C15 O16 1.41(3) . ? O16 C17 1.40(3) . ? C17 C18 1.48(3) . ? C19 C24 1.377(17) . ? C19 C20 1.387(17) . ? C20 C21 1.369(19) . ? C21 C22 1.364(19) . ? C22 C23 1.39(2) . ? C23 C24 1.377(18) . ? C25 C30 1.373(18) . ? C25 C26 1.398(17) . ? C26 C27 1.362(18) . ? C27 C28 1.34(2) . ? C28 C29 1.40(2) . ? C29 C30 1.377(19) . ? C31 C32 1.373(17) . ? C31 C36 1.392(18) . ? C32 C33 1.349(19) . ? C33 C34 1.39(2) . ? C34 C35 1.38(2) . ? C35 C36 1.37(2) . ? C37 C42 1.35(2) . ? C37 C38 1.39(2) . ? C38 C39 1.40(2) . ? C39 C40 1.34(3) . ? C40 C41 1.35(3) . ? C41 C42 1.34(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Rb O1 96.2(3) . . ? O2 Rb O7 143.8(3) . . ? O1 Rb O7 109.4(4) . . ? O2 Rb O13 80.0(3) . . ? O1 Rb O13 111.1(4) . . ? O7 Rb O13 112.3(4) . . ? O2 Rb O3 72.5(2) . . ? O1 Rb O3 107.0(3) . . ? O7 Rb O3 75.7(3) . . ? O13 Rb O3 134.8(3) . . ? O2 Rb O10 120.4(3) . . ? O1 Rb O10 134.6(3) . . ? O7 Rb O10 56.0(4) . . ? O13 Rb O10 56.8(4) . . ? O3 Rb O10 109.0(3) . . ? O2 Rb O16 80.4(3) . . ? O1 Rb O16 56.4(4) . . ? O7 Rb O16 135.2(3) . . ? O13 Rb O16 55.2(4) . . ? O3 Rb O16 146.6(3) . . ? O10 Rb O16 101.3(4) . . ? O2 Rb O4 135.0(3) . . ? O1 Rb O4 55.1(4) . . ? O7 Rb O4 55.4(4) . . ? O13 Rb O4 139.1(3) . . ? O3 Rb O4 83.4(3) . . ? O10 Rb O4 103.0(4) . . ? O16 Rb O4 103.4(4) . . ? O2 Rb O43 56.6(3) . . ? O1 Rb O43 149.6(3) . . ? O7 Rb O43 90.9(4) . . ? O13 Rb O43 79.7(4) . . ? O3 Rb O43 55.2(3) . . ? O10 Rb O43 75.5(3) . . ? O16 Rb O43 122.8(4) . . ? O4 Rb O43 133.4(4) . . ? O2 Rb C3 114.0(5) . . ? O1 Rb C3 40.5(5) . . ? O7 Rb C3 75.1(5) . . ? O13 Rb C3 146.7(5) . . ? O3 Rb C3 78.3(4) . . ? O10 Rb C3 124.8(5) . . ? O16 Rb C3 95.9(5) . . ? O4 Rb C3 21.8(5) . . ? O43 Rb C3 133.5(4) . . ? O2 Rb C17 75.1(4) . . ? O1 Rb C17 39.0(5) . . ? O7 Rb C17 140.1(5) . . ? O13 Rb C17 75.3(6) . . ? O3 Rb C17 128.2(4) . . ? O10 Rb C17 122.1(5) . . ? O16 Rb C17 21.4(5) . . ? O4 Rb C17 92.4(5) . . ? O43 Rb C17 128.6(5) . . ? C3 Rb C17 79.5(6) . . ? O2 Rb C15 66.9(5) . . ? O1 Rb C15 75.8(6) . . ? O7 Rb C15 143.2(5) . . ? O13 Rb C15 39.2(6) . . ? O3 Rb C15 139.3(5) . . ? O10 Rb C15 93.6(6) . . ? O16 Rb C15 21.4(5) . . ? O4 Rb C15 124.8(5) . . ? O43 Rb C15 101.6(6) . . ? C3 Rb C15 116.2(6) . . ? C17 Rb C15 37.3(7) . . ? O2 P1 N1 118.9(5) . . ? O2 P1 C19 108.2(5) . . ? N1 P1 C19 109.7(5) . . ? O2 P1 C25 110.1(5) . . ? N1 P1 C25 103.4(6) . . ? C19 P1 C25 105.9(6) . . ? O2 P1 Rb 44.5(3) . . ? N1 P1 Rb 77.9(4) . . ? C19 P1 Rb 143.8(4) . . ? C25 P1 Rb 106.4(4) . . ? P1 O2 Rb 114.6(4) . . ? O3 P2 N1 120.1(6) . . ? O3 P2 C37 108.0(6) . . ? N1 P2 C37 111.8(6) . . ? O3 P2 C31 108.7(5) . . ? N1 P2 C31 104.6(6) . . ? C37 P2 C31 102.1(6) . . ? O3 P2 Rb 46.2(3) . . ? N1 P2 Rb 75.3(4) . . ? C37 P2 Rb 141.3(5) . . ? C31 P2 Rb 113.1(4) . . ? P2 O3 Rb 112.9(4) . . ? P2 N1 P1 129.6(7) . . ? C18 O1 C2 114.2(15) . . ? C18 O1 Rb 121.9(12) . . ? C2 O1 Rb 121.1(11) . . ? O1 C2 C3 110.8(18) . . ? O4 C3 C2 108.2(19) . . ? O4 C3 Rb 54.0(10) . . ? C2 C3 Rb 85.9(13) . . ? C5 O4 C3 105.3(16) . . ? C5 O4 Rb 105.9(12) . . ? C3 O4 Rb 104.2(13) . . ? O4 C5 C6 103.5(17) . . ? O4 C5 Rb 52.9(10) . . ? C6 C5 Rb 83.1(13) . . ? C5 C6 O7 114.4(18) . . ? C8 O7 C6 115.5(17) . . ? C8 O7 Rb 122.3(14) . . ? C6 O7 Rb 117.0(11) . . ? O7 C8 C9 109.1(18) . . ? O10 C9 C8 112.2(17) . . ? O10 C9 Rb 52.0(8) . . ? C8 C9 Rb 84.9(11) . . ? C9 O10 C11 117(2) . . ? C9 O10 Rb 106.4(12) . . ? C11 O10 Rb 106.8(11) . . ? O10 C11 C12 113(2) . . ? O10 C11 Rb 51.7(9) . . ? C12 C11 Rb 84.4(17) . . ? O13 C12 C11 112(3) . . ? C12 O13 C14 115(2) . . ? C12 O13 Rb 118.3(16) . . ? C14 O13 Rb 116.4(14) . . ? C15 C14 O13 111(2) . . ? O16 C15 C14 109(2) . . ? O16 C15 Rb 52.5(10) . . ? C14 C15 Rb 87.0(17) . . ? C15 O16 C17 114.8(19) . . ? C15 O16 Rb 106.1(14) . . ? C17 O16 Rb 105.8(13) . . ? O16 C17 C18 114.7(19) . . ? O16 C17 Rb 52.8(10) . . ? C18 C17 Rb 84.4(13) . . ? O1 C18 C17 110.6(17) . . ? C24 C19 C20 115.9(13) . . ? C24 C19 P1 123.2(10) . . ? C20 C19 P1 120.5(11) . . ? C21 C20 C19 122.0(14) . . ? C22 C21 C20 121.4(13) . . ? C21 C22 C23 117.9(14) . . ? C24 C23 C22 119.9(14) . . ? C23 C24 C19 122.8(14) . . ? C30 C25 C26 118.1(12) . . ? C30 C25 P1 121.6(10) . . ? C26 C25 P1 120.0(10) . . ? C27 C26 C25 121.2(13) . . ? C28 C27 C26 120.6(15) . . ? C27 C28 C29 119.9(14) . . ? C30 C29 C28 119.5(14) . . ? C25 C30 C29 120.7(14) . . ? C32 C31 C36 119.0(13) . . ? C32 C31 P2 118.8(11) . . ? C36 C31 P2 122.2(10) . . ? C33 C32 C31 121.3(15) . . ? C32 C33 C34 121.3(15) . . ? C35 C34 C33 116.3(15) . . ? C34 C35 C36 123.1(16) . . ? C35 C36 C31 118.3(14) . . ? C42 C37 C38 118.0(15) . . ? C42 C37 P2 121.8(14) . . ? C38 C37 P2 120.1(11) . . ? C39 C38 C37 116.7(17) . . ? C40 C39 C38 120(2) . . ? C39 C40 C41 124(2) . . ? C42 C41 C40 113(2) . . ? C37 C42 C41 127(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O43 H43B O2 0.85 2.51 2.921(15) 110.3 . O43 H43A O3 0.85 2.47 2.903(16) 112.8 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.510 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.117 #==END data_compound7 _database_code_depnum_ccdc_archive 'CCDC 220674' _chemical_name_common "(Aquacesium(18-crown-6)) imidobis(diphenylphosphinate-O,O')" _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Aquacesium(18-crown-6)] imidobis(diphenylphosphinate-O,O') ; _chemical_formula_moiety ? _chemical_formula_sum 'C36 H46 Cs N O9 P2' _chemical_formula_weight 831.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.059(1) _cell_length_b 15.769(3) _cell_length_c 24.871(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3945.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 12.50 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.518 _exptl_absorpt_correction_T_max 0.579 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4/PC diffractometer' _diffrn_measurement_method \w:2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3 _diffrn_reflns_number 7784 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6930 _reflns_number_gt 5295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS ver 2.1 1993' _computing_cell_refinement 'XSCANS ver 2.1 1993' _computing_data_reduction 'XSCANS ver 2.1 1993' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V 6.10' _computing_publication_material 'SHELXTL V 6.10' _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 w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+5.3075P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0043(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_number_reflns 6930 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1797 _refine_ls_wR_factor_gt 0.1424 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cs Cs 0.77858(6) 0.89920(4) 0.20031(3) 0.0591(2) Uani 1 d . . . P1 P 0.75770(17) 1.10560(14) 0.11786(8) 0.0358(4) Uani 1 d . . . O2 O 0.8281(6) 1.0836(4) 0.1688(3) 0.0472(15) Uani 1 d . . . P2 P 0.8213(2) 0.96141(15) 0.04884(10) 0.0450(5) Uani 1 d . . . O3 O 0.9017(7) 0.9044(5) 0.0838(3) 0.0640(18) Uani 1 d . . . N1 N 0.7293(8) 1.0313(4) 0.0750(3) 0.0465(16) Uani 1 d . . . O1 O 0.4760(8) 0.8898(9) 0.1957(5) 0.107(4) Uani 1 d . . . C2 C 0.4137(19) 0.8210(16) 0.1686(9) 0.142(10) Uani 1 d . . . H2A H 0.3422 0.8455 0.1480 0.080 Uiso 1 d R . . H2B H 0.3770 0.7800 0.1937 0.080 Uiso 1 d R . . C3 C 0.509(3) 0.7737(17) 0.1361(8) 0.143(10) Uani 1 d . . . H3A H 0.5492 0.8138 0.1112 0.080 Uiso 1 d R . . H3B H 0.4636 0.7307 0.1153 0.080 Uiso 1 d R . . O4 O 0.6057(13) 0.7388(8) 0.1664(4) 0.104(4) Uani 1 d . . . C5 C 0.701(3) 0.6950(14) 0.1334(9) 0.167(13) Uani 1 d . . . H5A H 0.7451 0.7345 0.1096 0.080 Uiso 1 d R . . H5B H 0.6517 0.6546 0.1118 0.080 Uiso 1 d R . . C6 C 0.799(3) 0.6547(12) 0.1694(10) 0.154(12) Uani 1 d . . . H6A H 0.8500 0.6137 0.1489 0.080 Uiso 1 d R . . H6B H 0.7512 0.6244 0.1972 0.080 Uiso 1 d R . . O7 O 0.8792(12) 0.7170(7) 0.1933(6) 0.116(5) Uani 1 d . . . C8 C 0.972(2) 0.6889(16) 0.2320(11) 0.174(14) Uani 1 d . . . H8A H 1.0234 0.6469 0.2128 0.080 Uiso 1 d R . . H8B H 0.9300 0.6618 0.2627 0.080 Uiso 1 d R . . C9 C 1.0481(18) 0.763(2) 0.2567(13) 0.21(2) Uani 1 d . . . H9A H 1.0777 0.7958 0.2257 0.080 Uiso 1 d R . . H9B H 1.1245 0.7414 0.2755 0.080 Uiso 1 d R . . O10 O 0.9637(10) 0.8098(10) 0.2848(6) 0.135(6) Uani 1 d . . . C11 C 1.028(3) 0.8768(16) 0.3146(12) 0.185(17) Uani 1 d . . . H11A H 1.0612 0.9141 0.2865 0.080 Uiso 1 d R . . H11B H 1.1019 0.8555 0.3352 0.080 Uiso 1 d R . . C12 C 0.928(4) 0.9329(19) 0.3462(12) 0.22(2) Uani 1 d . . . H12A H 0.9781 0.9720 0.3683 0.080 Uiso 1 d R . . H12B H 0.8827 0.8938 0.3702 0.080 Uiso 1 d R . . O13 O 0.8588(17) 0.9708(9) 0.3116(5) 0.134(6) Uani 1 d . . . C14 C 0.757(3) 1.0204(19) 0.3393(8) 0.167(14) Uani 1 d . . . H14A H 0.7954 1.0660 0.3604 0.080 Uiso 1 d R . . H14B H 0.7146 0.9817 0.3643 0.080 Uiso 1 d R . . C15 C 0.653(3) 1.0510(12) 0.3038(11) 0.155(11) Uani 1 d . . . H15A H 0.6938 1.0818 0.2742 0.080 Uiso 1 d R . . H15B H 0.5942 1.0887 0.3231 0.080 Uiso 1 d R . . O16 O 0.5803(13) 0.9827(6) 0.2841(5) 0.103(4) Uani 1 d . . . C17 C 0.476(2) 1.0089(14) 0.2513(11) 0.150(11) Uani 1 d . . . H17A H 0.5065 1.0437 0.2214 0.080 Uiso 1 d R . . H17B H 0.4192 1.0436 0.2738 0.080 Uiso 1 d R . . C18 C 0.3985(16) 0.9359(16) 0.2292(10) 0.151(11) Uani 1 d . . . H18A H 0.3727 0.8985 0.2586 0.080 Uiso 1 d R . . H18B H 0.3201 0.9561 0.2112 0.080 Uiso 1 d R . . C19 C 0.8484(8) 1.1911(5) 0.0849(3) 0.0390(18) Uani 1 d . . . C20 C 0.9868(9) 1.1926(7) 0.0884(4) 0.050(2) Uani 1 d . . . H20 H 1.0310 1.1537 0.1128 0.080 Uiso 1 d R . . C21 C 1.0606(11) 1.2505(7) 0.0604(5) 0.062(3) Uani 1 d . . . H21 H 1.1553 1.2481 0.0624 0.080 Uiso 1 d R . . C22 C 0.9968(12) 1.3103(7) 0.0286(4) 0.062(3) Uani 1 d . . . H22 H 1.0498 1.3515 0.0093 0.080 Uiso 1 d R . . C23 C 0.8604(11) 1.3114(7) 0.0250(4) 0.059(3) Uani 1 d . . . H23 H 0.8178 1.3528 0.0018 0.080 Uiso 1 d R . . C24 C 0.7862(10) 1.2508(6) 0.0531(3) 0.0448(18) Uani 1 d . . . H24 H 0.6916 1.2511 0.0498 0.080 Uiso 1 d R . . C25 C 0.5951(8) 1.1483(6) 0.1341(4) 0.044(2) Uani 1 d . . . C26 C 0.5805(10) 1.2140(7) 0.1699(4) 0.055(2) Uani 1 d . . . H26 H 0.6590 1.2428 0.1822 0.080 Uiso 1 d R . . C27 C 0.4583(12) 1.2417(8) 0.1871(5) 0.072(3) Uani 1 d . . . H27 H 0.4527 1.2893 0.2118 0.080 Uiso 1 d R . . C28 C 0.3462(11) 1.2040(9) 0.1681(5) 0.072(3) Uani 1 d . . . H28 H 0.2613 1.2252 0.1794 0.080 Uiso 1 d R . . C29 C 0.3555(10) 1.1376(9) 0.1321(6) 0.075(3) Uani 1 d . . . H29 H 0.2762 1.1098 0.1199 0.080 Uiso 1 d R . . C30 C 0.4808(9) 1.1111(8) 0.1149(4) 0.058(2) Uani 1 d . . . H30 H 0.4868 1.0620 0.0912 0.080 Uiso 1 d R . . C31 C 0.7102(10) 0.8959(6) 0.0089(4) 0.053(2) Uani 1 d . . . C32 C 0.7587(13) 0.8224(7) -0.0138(5) 0.077(4) Uani 1 d . . . H32 H 0.8507 0.8099 -0.0085 0.080 Uiso 1 d R . . C33 C 0.6776(16) 0.7691(9) -0.0425(6) 0.089(5) Uani 1 d . . . H33 H 0.7141 0.7160 -0.0554 0.080 Uiso 1 d R . . C34 C 0.5485(18) 0.7906(10) -0.0526(7) 0.101(5) Uani 1 d . . . H34 H 0.4970 0.7561 -0.0772 0.080 Uiso 1 d R . . C35 C 0.4992(16) 0.8625(10) -0.0295(8) 0.102(5) Uani 1 d . . . H35 H 0.4064 0.8735 -0.0336 0.080 Uiso 1 d R . . C36 C 0.5791(13) 0.9171(8) -0.0001(6) 0.079(4) Uani 1 d . . . H36 H 0.5417 0.9695 0.0135 0.080 Uiso 1 d R . . C37 C 0.9296(10) 1.0081(7) -0.0017(4) 0.054(2) Uani 1 d . . . C38 C 0.8878(12) 1.0767(8) -0.0324(4) 0.065(3) Uani 1 d . . . H38 H 0.8029 1.1033 -0.0280 0.080 Uiso 1 d R . . C39 C 0.9649(16) 1.1089(11) -0.0709(5) 0.087(4) Uani 1 d . . . H39 H 0.9432 1.1564 -0.0942 0.080 Uiso 1 d R . . C40 C 1.0899(18) 1.0758(11) -0.0822(7) 0.108(6) Uani 1 d . . . H40 H 1.1456 1.0933 -0.1121 0.080 Uiso 1 d R . . C41 C 1.1325(16) 1.0087(11) -0.0504(8) 0.112(6) Uani 1 d . . . H41 H 1.2200 0.9853 -0.0532 0.080 Uiso 1 d R . . C42 C 1.0541(13) 0.9754(9) -0.0109(8) 0.095(5) Uani 1 d . . . H42 H 1.0781 0.9283 0.0124 0.080 Uiso 1 d R . . O43 O 1.0697(11) 0.9873(11) 0.1687(7) 0.187(9) Uani 1 d . . . H43A H 1.0894 0.9688 0.1370 0.080 Uiso 1 d R . . H43B H 1.0639 1.0416 0.1679 0.080 Uiso 1 d 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 Cs 0.0499(3) 0.0586(3) 0.0686(4) 0.0213(3) 0.0035(3) -0.0016(3) P1 0.0312(10) 0.0351(9) 0.0411(9) 0.0007(9) 0.0026(7) 0.0000(9) O2 0.043(3) 0.044(4) 0.055(3) 0.007(3) -0.007(3) 0.001(3) P2 0.0475(13) 0.0391(11) 0.0485(12) -0.0056(10) 0.0028(10) 0.0015(9) O3 0.075(5) 0.052(4) 0.065(4) -0.004(4) -0.006(3) 0.019(4) N1 0.044(4) 0.039(4) 0.057(4) -0.006(3) 0.006(4) 0.000(4) O1 0.051(4) 0.151(10) 0.118(8) 0.049(9) 0.010(5) 0.023(6) C2 0.090(13) 0.19(2) 0.145(18) 0.026(17) -0.067(13) -0.062(15) C3 0.16(2) 0.19(2) 0.081(11) -0.012(14) -0.019(14) -0.077(19) O4 0.123(9) 0.121(9) 0.067(6) -0.001(6) 0.006(6) -0.054(7) C5 0.27(4) 0.109(15) 0.121(15) -0.039(13) 0.11(2) -0.04(2) C6 0.23(3) 0.063(10) 0.16(2) -0.004(11) 0.11(2) 0.001(14) O7 0.115(8) 0.082(7) 0.153(11) 0.045(8) 0.064(9) 0.037(6) C8 0.121(17) 0.18(2) 0.22(3) 0.11(2) 0.085(18) 0.110(18) C9 0.040(8) 0.29(4) 0.30(4) 0.19(3) 0.012(15) 0.033(16) O10 0.055(6) 0.188(13) 0.162(12) 0.114(11) -0.019(7) -0.011(7) C11 0.17(2) 0.16(2) 0.22(3) 0.11(2) -0.16(2) -0.098(19) C12 0.36(6) 0.16(3) 0.14(2) 0.07(2) -0.12(3) -0.14(3) O13 0.186(13) 0.133(10) 0.081(8) 0.040(8) -0.031(9) -0.079(10) C14 0.23(3) 0.20(3) 0.070(10) -0.018(14) 0.040(16) -0.10(3) C15 0.22(3) 0.078(11) 0.17(2) -0.045(14) 0.10(2) -0.037(14) O16 0.137(10) 0.071(6) 0.101(8) 0.011(5) 0.049(7) 0.000(6) C17 0.132(18) 0.111(15) 0.21(3) 0.037(16) 0.094(18) 0.071(15) C18 0.069(10) 0.21(3) 0.18(2) 0.10(2) 0.027(12) 0.062(14) C19 0.035(4) 0.036(4) 0.046(4) -0.005(4) 0.007(3) -0.002(3) C20 0.033(4) 0.065(6) 0.052(5) -0.001(5) -0.002(4) -0.003(4) C21 0.044(5) 0.069(7) 0.073(7) 0.000(6) 0.009(5) -0.009(5) C22 0.064(6) 0.061(6) 0.062(6) 0.010(5) 0.016(5) -0.011(5) C23 0.072(7) 0.046(5) 0.060(6) 0.009(5) 0.007(5) -0.007(5) C24 0.041(4) 0.052(5) 0.042(4) 0.003(4) -0.007(4) -0.001(4) C25 0.035(4) 0.044(5) 0.053(5) 0.008(4) 0.004(4) 0.004(4) C26 0.045(5) 0.055(6) 0.065(6) -0.007(5) 0.006(4) 0.014(4) C27 0.066(7) 0.066(7) 0.084(8) -0.013(6) 0.018(6) 0.026(6) C28 0.042(6) 0.086(8) 0.087(8) 0.011(7) 0.029(6) 0.013(6) C29 0.033(5) 0.100(9) 0.093(9) 0.001(7) -0.005(5) -0.003(5) C30 0.042(5) 0.068(6) 0.063(6) -0.008(5) 0.000(4) -0.001(5) C31 0.059(5) 0.034(4) 0.064(5) -0.003(4) 0.016(5) -0.009(5) C32 0.072(8) 0.061(7) 0.099(9) -0.033(6) 0.013(7) -0.014(6) C33 0.106(11) 0.079(8) 0.083(8) -0.043(7) 0.029(8) -0.024(8) C34 0.106(12) 0.077(9) 0.120(13) -0.036(9) 0.009(10) -0.044(9) C35 0.071(8) 0.094(10) 0.140(14) -0.031(10) -0.038(9) -0.013(8) C36 0.074(8) 0.064(8) 0.098(9) -0.024(7) -0.018(7) 0.000(6) C37 0.046(5) 0.050(6) 0.065(6) -0.017(5) 0.007(4) -0.011(4) C38 0.060(6) 0.084(8) 0.053(6) 0.005(5) -0.004(5) -0.006(5) C39 0.110(11) 0.088(10) 0.063(7) 0.006(7) 0.005(7) -0.035(10) C40 0.107(12) 0.098(12) 0.118(13) -0.031(10) 0.052(10) -0.052(10) C41 0.075(10) 0.093(11) 0.166(18) -0.035(12) 0.048(11) -0.008(8) C42 0.060(7) 0.060(8) 0.164(16) -0.005(8) 0.046(9) 0.004(6) O43 0.055(6) 0.231(18) 0.28(2) 0.142(17) -0.032(9) -0.018(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cs O1 3.049(8) . ? Cs O7 3.051(10) . ? Cs O2 3.053(6) . ? Cs O13 3.096(13) . ? Cs O10 3.143(10) . ? Cs O3 3.153(7) . ? Cs O16 3.171(11) . ? Cs O4 3.183(11) . ? Cs O43 3.334(12) . ? Cs C5 3.71(2) . ? Cs C3 3.71(2) . ? Cs C17 3.726(16) . ? P1 O2 1.493(6) . ? P1 N1 1.609(7) . ? P1 C25 1.814(9) . ? P1 C19 1.823(8) . ? P2 O3 1.489(8) . ? P2 N1 1.580(7) . ? P2 C31 1.818(10) . ? P2 C37 1.818(10) . ? O1 C18 1.35(2) . ? O1 C2 1.42(2) . ? C2 C3 1.46(3) . ? C3 O4 1.34(3) . ? O4 C5 1.43(2) . ? C5 C6 1.48(4) . ? C6 O7 1.40(3) . ? O7 C8 1.41(3) . ? C8 C9 1.53(4) . ? C9 O10 1.32(3) . ? O10 C11 1.44(3) . ? C11 C12 1.55(4) . ? C12 O13 1.26(3) . ? O13 C14 1.46(3) . ? C14 C15 1.45(4) . ? C15 O16 1.39(2) . ? O16 C17 1.40(3) . ? C17 C18 1.49(3) . ? C19 C24 1.379(12) . ? C19 C20 1.396(12) . ? C20 C21 1.368(15) . ? C21 C22 1.388(16) . ? C22 C23 1.375(16) . ? C23 C24 1.400(14) . ? C25 C26 1.375(14) . ? C25 C30 1.377(14) . ? C26 C27 1.372(14) . ? C27 C28 1.358(19) . ? C28 C29 1.381(19) . ? C29 C30 1.396(15) . ? C31 C32 1.378(14) . ? C31 C36 1.379(17) . ? C32 C33 1.372(18) . ? C33 C34 1.37(2) . ? C34 C35 1.36(2) . ? C35 C36 1.385(18) . ? C37 C42 1.374(16) . ? C37 C38 1.390(16) . ? C38 C39 1.334(17) . ? C39 C40 1.39(2) . ? C40 C41 1.39(3) . ? C41 C42 1.36(2) . ? 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 Cs O7 106.4(4) . . ? O1 Cs O2 101.5(3) . . ? O7 Cs O2 145.9(2) . . ? O1 Cs O13 108.2(4) . . ? O7 Cs O13 108.0(4) . . ? O2 Cs O13 80.7(3) . . ? O1 Cs O10 126.5(3) . . ? O7 Cs O10 54.5(4) . . ? O2 Cs O10 120.1(3) . . ? O13 Cs O10 53.9(5) . . ? O1 Cs O3 111.0(3) . . ? O7 Cs O3 80.9(3) . . ? O2 Cs O3 71.04(19) . . ? O13 Cs O3 135.2(3) . . ? O10 Cs O3 113.2(3) . . ? O1 Cs O16 54.4(4) . . ? O7 Cs O16 129.6(3) . . ? O2 Cs O16 82.9(2) . . ? O13 Cs O16 54.9(4) . . ? O10 Cs O16 96.8(4) . . ? O3 Cs O16 147.2(2) . . ? O1 Cs O4 53.6(4) . . ? O7 Cs O4 54.4(4) . . ? O2 Cs O4 141.1(3) . . ? O13 Cs O4 132.0(3) . . ? O10 Cs O4 98.3(4) . . ? O3 Cs O4 89.5(2) . . ? O16 Cs O4 99.2(3) . . ? O1 Cs O43 152.6(3) . . ? O7 Cs O43 95.0(4) . . ? O2 Cs O43 53.1(3) . . ? O13 Cs O43 80.2(4) . . ? O10 Cs O43 79.9(3) . . ? O3 Cs O43 55.1(3) . . ? O16 Cs O43 122.3(4) . . ? O4 Cs O43 138.4(4) . . ? O1 Cs C5 74.3(5) . . ? O7 Cs C5 39.4(6) . . ? O2 Cs C5 138.3(4) . . ? O13 Cs C5 140.6(5) . . ? O10 Cs C5 92.1(6) . . ? O3 Cs C5 72.2(3) . . ? O16 Cs C5 121.5(4) . . ? O4 Cs C5 22.4(4) . . ? O43 Cs C5 116.2(5) . . ? O1 Cs C3 39.7(5) . . ? O7 Cs C3 73.5(6) . . ? O2 Cs C3 121.1(4) . . ? O13 Cs C3 140.2(4) . . ? O10 Cs C3 118.7(5) . . ? O3 Cs C3 84.6(4) . . ? O16 Cs C3 92.6(5) . . ? O4 Cs C3 20.7(5) . . ? O43 Cs C3 139.5(5) . . ? C5 Cs C3 35.9(6) . . ? O1 Cs C17 38.7(5) . . ? O7 Cs C17 136.7(4) . . ? O2 Cs C17 77.2(4) . . ? O13 Cs C17 74.9(6) . . ? O10 Cs C17 117.7(5) . . ? O3 Cs C17 128.5(4) . . ? O16 Cs C17 21.5(5) . . ? O4 Cs C17 90.7(5) . . ? O43 Cs C17 127.2(5) . . ? C5 Cs C17 112.5(7) . . ? C3 Cs C17 78.3(7) . . ? O2 P1 N1 118.5(4) . . ? O2 P1 C25 109.0(4) . . ? N1 P1 C25 104.9(5) . . ? O2 P1 C19 108.4(4) . . ? N1 P1 C19 109.3(4) . . ? C25 P1 C19 106.0(4) . . ? O2 P1 Cs 47.6(2) . . ? N1 P1 Cs 75.4(3) . . ? C25 P1 Cs 104.1(3) . . ? C19 P1 Cs 146.8(3) . . ? P1 O2 Cs 111.2(3) . . ? O3 P2 N1 119.9(4) . . ? O3 P2 C31 108.1(5) . . ? N1 P2 C31 105.2(5) . . ? O3 P2 C37 108.8(5) . . ? N1 P2 C37 110.7(4) . . ? C31 P2 C37 102.8(4) . . ? O3 P2 Cs 49.2(3) . . ? N1 P2 Cs 73.4(3) . . ? C31 P2 Cs 108.4(3) . . ? C37 P2 Cs 146.3(4) . . ? P2 O3 Cs 109.8(4) . . ? P2 N1 P1 132.6(6) . . ? P2 N1 Cs 83.0(3) . . ? P1 N1 Cs 80.3(3) . . ? C18 O1 C2 116.6(16) . . ? C18 O1 Cs 121.7(13) . . ? C2 O1 Cs 119.7(11) . . ? O1 C2 C3 111.1(15) . . ? O4 C3 C2 111.9(16) . . ? O4 C3 Cs 56.8(9) . . ? C2 C3 Cs 88.3(11) . . ? C3 O4 C5 110.8(17) . . ? C3 O4 Cs 102.5(12) . . ? C5 O4 Cs 99.8(11) . . ? O4 C5 C6 107.9(17) . . ? O4 C5 Cs 57.8(9) . . ? C6 C5 Cs 87.7(13) . . ? O7 C6 C5 109.9(16) . . ? C6 O7 C8 116.6(17) . . ? C6 O7 Cs 119.6(12) . . ? C8 O7 Cs 118.3(14) . . ? O7 C8 C9 111.4(17) . . ? O10 C9 C8 108.4(15) . . ? O10 C9 Cs 54.1(9) . . ? C8 C9 Cs 85.7(10) . . ? C9 O10 C11 112.9(19) . . ? C9 O10 Cs 106.0(13) . . ? C11 O10 Cs 106.3(10) . . ? O10 C11 C12 113(2) . . ? O10 C11 Cs 52.4(7) . . ? C12 C11 Cs 84.1(13) . . ? O13 C12 C11 106(3) . . ? C12 O13 C14 109(2) . . ? C12 O13 Cs 125.6(19) . . ? C14 O13 Cs 115.7(14) . . ? C15 C14 O13 113.3(17) . . ? O16 C15 C14 109.6(19) . . ? O16 C15 Cs 55.9(8) . . ? C14 C15 Cs 87.9(14) . . ? C15 O16 C17 111.9(17) . . ? C15 O16 Cs 102.8(10) . . ? C17 O16 Cs 102.3(10) . . ? O16 C17 C18 112.2(15) . . ? O16 C17 Cs 56.3(7) . . ? C18 C17 Cs 86.7(10) . . ? O1 C18 C17 110.0(15) . . ? C24 C19 C20 118.5(8) . . ? C24 C19 P1 122.4(7) . . ? C20 C19 P1 118.9(7) . . ? C21 C20 C19 121.4(10) . . ? C20 C21 C22 119.6(10) . . ? C23 C22 C21 120.5(10) . . ? C22 C23 C24 119.4(10) . . ? C19 C24 C23 120.7(9) . . ? C26 C25 C30 117.2(9) . . ? C26 C25 P1 121.4(7) . . ? C30 C25 P1 121.1(8) . . ? C27 C26 C25 122.4(11) . . ? C28 C27 C26 119.8(11) . . ? C27 C28 C29 120.0(10) . . ? C28 C29 C30 119.2(11) . . ? C25 C30 C29 121.3(11) . . ? C32 C31 C36 118.4(11) . . ? C32 C31 P2 119.0(9) . . ? C36 C31 P2 122.6(8) . . ? C33 C32 C31 121.2(13) . . ? C34 C33 C32 120.6(13) . . ? C35 C34 C33 118.3(13) . . ? C34 C35 C36 121.8(15) . . ? C31 C36 C35 119.3(13) . . ? C42 C37 C38 118.4(12) . . ? C42 C37 P2 120.6(10) . . ? C38 C37 P2 120.9(8) . . ? C39 C38 C37 121.0(13) . . ? C38 C39 C40 121.9(16) . . ? C41 C40 C39 116.7(14) . . ? C42 C41 C40 121.7(15) . . ? C41 C42 C37 120.2(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O43 H43B O2 0.86 2.46 2.866(15) 109.4 . O43 H43A O3 0.86 2.52 3.004(18) 116.4 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.699 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.149 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 220675' _chemical_name_common (Li(15C5))(Ph2SPNPSPh2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety ? _chemical_formula_sum 'C34 H42 Li N O6 P2 S2' _chemical_formula_weight 693.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 11.473(2) _cell_length_b 12.017(3) _cell_length_c 13.736(2) _cell_angle_alpha 96.49(2) _cell_angle_beta 90.96(1) _cell_angle_gamma 103.93(3) _cell_volume 1824.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 5.31 _cell_measurement_theta_max 24.48 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.9169 _exptl_absorpt_correction_T_max 0.9624 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4/PC' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3 _diffrn_reflns_number 6777 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 6426 _reflns_number_gt 3968 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'xscans ver 2.1 (Siemens 1994)' _computing_cell_refinement 'xscans ver 2.1 (Siemens 1994)' _computing_data_reduction 'xscans ver 2.1 (Siemens 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP SHELXTL/PC (Sheldrick 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] 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 'noref, except H6A and H6B' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6426 _refine_ls_number_parameters 422 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1788 _refine_ls_wR_factor_gt 0.1594 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 1.853 _refine_ls_shift/su_mean 0.006 _refine_diff_density_max 0.799 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.061 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.30369(9) 0.29045(9) 0.21783(7) 0.0396(3) Uani 1 d . . . P2 P 0.11905(9) 0.41350(9) 0.28292(7) 0.0387(3) Uani 1 d . . . S1 S 0.25601(12) 0.12700(10) 0.24484(10) 0.0637(4) Uani 1 d . . . S2 S 0.07741(11) 0.35222(11) 0.40888(8) 0.0568(3) Uani 1 d . . . N1 N 0.2058(3) 0.3636(3) 0.2098(2) 0.0454(8) Uani 1 d . . . C1 C 0.3727(3) 0.2945(4) 0.0982(3) 0.0436(9) Uani 1 d . . . C2 C 0.4445(4) 0.2213(4) 0.0692(3) 0.0586(12) Uani 1 d . . . H2 H 0.4604 0.1710 0.1114 0.060 Uiso 1 calc R . . C3 C 0.4936(5) 0.2218(5) -0.0228(4) 0.0701(14) Uani 1 d . . . H3 H 0.5422 0.1720 -0.0413 0.060 Uiso 1 calc R . . C4 C 0.4710(4) 0.2952(5) -0.0868(3) 0.0643(13) Uani 1 d . . . H4 H 0.5031 0.2944 -0.1486 0.060 Uiso 1 calc R . . C5 C 0.4007(5) 0.3696(5) -0.0586(3) 0.0639(13) Uani 1 d . . . H5 H 0.3856 0.4199 -0.1011 0.060 Uiso 1 calc R . . C6 C 0.3517(4) 0.3702(4) 0.0339(3) 0.0538(11) Uani 1 d . . . H6 H 0.3048 0.4215 0.0527 0.060 Uiso 1 calc R . . C7 C 0.4281(3) 0.3710(4) 0.3014(3) 0.0425(9) Uani 1 d . . . C8 C 0.4819(4) 0.3183(5) 0.3692(3) 0.0607(12) Uani 1 d . . . H8 H 0.4528 0.2399 0.3735 0.060 Uiso 1 calc R . . C9 C 0.5777(5) 0.3814(7) 0.4297(4) 0.0800(17) Uani 1 d . . . H9 H 0.6121 0.3452 0.4748 0.060 Uiso 1 calc R . . C10 C 0.6228(5) 0.4964(7) 0.4242(4) 0.0819(18) Uani 1 d . . . H10 H 0.6874 0.5382 0.4654 0.060 Uiso 1 calc R . . C11 C 0.5717(5) 0.5512(5) 0.3565(4) 0.0735(14) Uani 1 d . . . H11 H 0.6027 0.6293 0.3516 0.060 Uiso 1 calc R . . C12 C 0.4743(4) 0.4880(4) 0.2966(3) 0.0564(11) Uani 1 d . . . H12 H 0.4391 0.5247 0.2524 0.060 Uiso 1 calc R . . C13 C -0.0174(3) 0.4034(3) 0.2079(3) 0.0395(8) Uani 1 d . . . C14 C -0.0156(4) 0.3869(4) 0.1066(3) 0.0532(11) Uani 1 d . . . H14 H 0.0537 0.3763 0.0767 0.060 Uiso 1 calc R . . C15 C -0.1175(5) 0.3862(5) 0.0492(4) 0.0661(13) Uani 1 d . . . H15 H -0.1157 0.3759 -0.0189 0.060 Uiso 1 calc R . . C16 C -0.2203(4) 0.4007(4) 0.0931(4) 0.0639(13) Uani 1 d . . . H16 H -0.2882 0.3996 0.0547 0.060 Uiso 1 calc R . . C17 C -0.2235(4) 0.4166(5) 0.1927(4) 0.0674(14) Uani 1 d . . . H17 H -0.2934 0.4262 0.2220 0.060 Uiso 1 calc R . . C18 C -0.1218(4) 0.4185(4) 0.2508(3) 0.0543(11) Uani 1 d . . . H18 H -0.1242 0.4300 0.3188 0.060 Uiso 1 calc R . . C19 C 0.1776(3) 0.5706(4) 0.3052(3) 0.0450(9) Uani 1 d . . . C20 C 0.2307(4) 0.6309(4) 0.2303(4) 0.0556(11) Uani 1 d . . . H20 H 0.2413 0.5904 0.1707 0.060 Uiso 1 calc R . . C21 C 0.2679(5) 0.7501(5) 0.2430(5) 0.0750(15) Uani 1 d . . . H21 H 0.3033 0.7893 0.1922 0.060 Uiso 1 calc R . . C22 C 0.2521(5) 0.8110(5) 0.3318(5) 0.0812(17) Uani 1 d . . . H22 H 0.2759 0.8912 0.3403 0.060 Uiso 1 calc R . . C23 C 0.2009(5) 0.7523(5) 0.4075(4) 0.0733(15) Uani 1 d . . . H23 H 0.1924 0.7932 0.4675 0.060 Uiso 1 calc R . . C24 C 0.1625(4) 0.6336(4) 0.3948(3) 0.0559(11) Uani 1 d . . . H24 H 0.1263 0.5950 0.4456 0.060 Uiso 1 calc R . . O1 O 0.1975(4) 0.1779(3) 0.6302(3) 0.0791(10) Uani 1 d . . . O2 O 0.2902(4) -0.0039(3) 0.5973(3) 0.0842(11) Uani 1 d . . . O3 O 0.2938(5) -0.0474(5) 0.7819(4) 0.1123(16) Uani 1 d . . . O4 O 0.1379(7) 0.0325(6) 0.8896(4) 0.144(2) Uani 1 d . . . O5 O 0.0524(6) 0.1618(4) 0.7783(4) 0.124(2) Uani 1 d . . . O6 O 0.0234(4) -0.0816(4) 0.6777(4) 0.0914(13) Uani 1 d D . . H6A H -0.047(2) -0.077(4) 0.702(3) 0.060 Uiso 1 d D . . H6B H 0.009(4) -0.1548(16) 0.650(3) 0.060 Uiso 1 d D . . Li Li 0.1597(8) 0.0373(7) 0.7261(6) 0.064(2) Uani 1 d . . . C25 C 0.2206(6) 0.1405(6) 0.5342(4) 0.0884(18) Uani 1 d . . . H25A H 0.2419 0.2055 0.4967 0.060 Uiso 1 calc R . . H25B H 0.1498 0.0862 0.5027 0.060 Uiso 1 calc R . . C26 C 0.3208(6) 0.0845(5) 0.5393(4) 0.0868(18) Uani 1 d . . . H26A H 0.3373 0.0538 0.4740 0.060 Uiso 1 calc R . . H26B H 0.3927 0.1404 0.5670 0.060 Uiso 1 calc R . . C27 C 0.3822(7) -0.0452(7) 0.6317(6) 0.107(2) Uani 1 d . . . H27A H 0.4498 0.0189 0.6542 0.060 Uiso 1 calc R . . H27B H 0.4082 -0.0932 0.5791 0.060 Uiso 1 calc R . . C28 C 0.3430(9) -0.1132(8) 0.7130(6) 0.132(3) Uani 1 d . . . H28A H 0.2838 -0.1837 0.6888 0.060 Uiso 1 calc R . . H28B H 0.4111 -0.1340 0.7424 0.060 Uiso 1 calc R . . C29 C 0.2663(9) -0.0908(8) 0.8646(6) 0.129(3) Uani 1 d . . . H29A H 0.3391 -0.0995 0.8966 0.060 Uiso 1 calc R . . H29B H 0.2128 -0.1671 0.8500 0.060 Uiso 1 calc R . . C30 C 0.2090(8) -0.0202(9) 0.9321(5) 0.118(3) Uani 1 d . . . H30A H 0.1626 -0.0691 0.9765 0.060 Uiso 1 calc R . . H30B H 0.2711 0.0374 0.9712 0.060 Uiso 1 calc R . . C31 C 0.0902(9) 0.1087(8) 0.9322(6) 0.134(3) Uani 1 d . . . H31A H 0.1537 0.1659 0.9701 0.060 Uiso 1 calc R . . H31B H 0.0358 0.0717 0.9788 0.060 Uiso 1 calc R . . C32 C 0.0282(13) 0.1668(9) 0.8793(6) 0.199(7) Uani 1 d . . . H32A H 0.0472 0.2472 0.9075 0.060 Uiso 1 calc R . . H32B H -0.0572 0.1354 0.8855 0.060 Uiso 1 calc R . . C33 C 0.0785(6) 0.2594(5) 0.7409(5) 0.0884(18) Uani 1 d . . . H33A H 0.1467 0.3119 0.7774 0.060 Uiso 1 calc R . . H33B H 0.0107 0.2945 0.7461 0.060 Uiso 1 calc R . . C34 C 0.1066(6) 0.2407(6) 0.6387(5) 0.0879(19) Uani 1 d . . . H34A H 0.0350 0.1976 0.6003 0.060 Uiso 1 calc R . . H34B H 0.1346 0.3144 0.6138 0.060 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0342(5) 0.0453(6) 0.0412(5) 0.0061(4) 0.0047(4) 0.0127(4) P2 0.0354(5) 0.0479(6) 0.0353(5) 0.0067(4) 0.0023(4) 0.0142(4) S1 0.0638(8) 0.0489(7) 0.0809(9) 0.0174(6) 0.0187(7) 0.0134(6) S2 0.0682(8) 0.0655(7) 0.0409(6) 0.0166(5) 0.0082(5) 0.0198(6) N1 0.0393(18) 0.059(2) 0.0430(18) 0.0084(15) 0.0043(15) 0.0211(16) C1 0.034(2) 0.051(2) 0.043(2) 0.0029(18) 0.0035(17) 0.0065(18) C2 0.053(3) 0.077(3) 0.054(3) 0.009(2) 0.010(2) 0.031(2) C3 0.060(3) 0.090(4) 0.068(3) 0.000(3) 0.019(3) 0.035(3) C4 0.061(3) 0.084(3) 0.047(3) 0.005(2) 0.017(2) 0.014(3) C5 0.069(3) 0.075(3) 0.052(3) 0.020(2) 0.016(2) 0.017(3) C6 0.056(3) 0.053(3) 0.054(3) 0.005(2) 0.015(2) 0.015(2) C7 0.033(2) 0.058(2) 0.039(2) 0.0044(17) 0.0047(16) 0.0164(18) C8 0.059(3) 0.083(3) 0.050(3) 0.012(2) 0.002(2) 0.034(3) C9 0.067(3) 0.127(6) 0.053(3) 0.006(3) -0.014(3) 0.042(4) C10 0.052(3) 0.131(6) 0.055(3) -0.022(3) -0.012(2) 0.023(3) C11 0.055(3) 0.075(3) 0.078(4) -0.016(3) 0.002(3) 0.003(3) C12 0.047(2) 0.061(3) 0.059(3) 0.001(2) 0.001(2) 0.012(2) C13 0.0310(19) 0.044(2) 0.046(2) 0.0085(17) 0.0027(16) 0.0120(16) C14 0.046(2) 0.073(3) 0.044(2) 0.006(2) 0.0007(19) 0.022(2) C15 0.070(3) 0.080(3) 0.049(3) 0.006(2) -0.013(2) 0.021(3) C16 0.051(3) 0.061(3) 0.080(4) 0.003(2) -0.021(2) 0.018(2) C17 0.037(2) 0.075(3) 0.094(4) 0.005(3) 0.004(2) 0.022(2) C18 0.044(2) 0.066(3) 0.057(3) 0.004(2) 0.006(2) 0.022(2) C19 0.036(2) 0.049(2) 0.050(2) 0.0021(18) -0.0002(18) 0.0144(18) C20 0.055(3) 0.052(3) 0.061(3) 0.007(2) 0.012(2) 0.015(2) C21 0.064(3) 0.062(3) 0.099(4) 0.018(3) 0.022(3) 0.012(3) C22 0.067(3) 0.049(3) 0.120(5) -0.004(3) 0.000(3) 0.006(3) C23 0.074(4) 0.062(3) 0.077(4) -0.017(3) -0.006(3) 0.017(3) C24 0.055(3) 0.065(3) 0.047(2) -0.001(2) -0.004(2) 0.018(2) O1 0.082(3) 0.086(3) 0.074(2) 0.022(2) 0.012(2) 0.021(2) O2 0.092(3) 0.078(3) 0.091(3) 0.020(2) 0.010(2) 0.030(2) O3 0.117(4) 0.139(4) 0.099(3) 0.045(3) 0.023(3) 0.050(3) O4 0.224(7) 0.148(5) 0.084(3) 0.003(3) 0.008(4) 0.095(5) O5 0.205(6) 0.080(3) 0.110(4) 0.027(3) 0.066(4) 0.065(4) O6 0.061(2) 0.075(3) 0.122(4) -0.020(2) 0.018(2) -0.001(2) Li 0.069(5) 0.053(4) 0.070(5) 0.010(4) 0.001(4) 0.013(4) C25 0.104(5) 0.094(4) 0.072(4) 0.029(3) 0.021(3) 0.024(4) C26 0.108(5) 0.083(4) 0.077(4) 0.014(3) 0.032(4) 0.033(4) C27 0.103(5) 0.123(6) 0.108(5) 0.005(5) 0.008(4) 0.056(5) C28 0.158(8) 0.156(8) 0.128(6) 0.051(6) 0.053(6) 0.112(7) C29 0.160(8) 0.143(7) 0.114(6) 0.072(6) 0.015(6) 0.067(7) C30 0.102(5) 0.182(9) 0.074(4) 0.042(5) -0.003(4) 0.029(6) C31 0.176(9) 0.115(6) 0.117(6) 0.023(5) 0.086(7) 0.039(6) C32 0.389(19) 0.181(9) 0.107(6) 0.054(6) 0.144(9) 0.199(12) C33 0.076(4) 0.080(4) 0.115(5) 0.015(4) 0.006(4) 0.028(3) C34 0.098(4) 0.103(5) 0.091(4) 0.045(4) 0.024(4) 0.063(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 P1 N1 1.593(3) . ? P1 C7 1.822(4) . ? P1 C1 1.837(4) . ? P1 S1 1.9873(16) . ? P2 N1 1.595(3) . ? P2 C13 1.831(4) . ? P2 C19 1.833(4) . ? P2 S2 1.9775(14) . ? C1 C2 1.376(6) . ? C1 C6 1.394(6) . ? C2 C3 1.392(6) . ? C3 C4 1.377(7) . ? C4 C5 1.370(7) . ? C5 C6 1.398(6) . ? C7 C12 1.388(6) . ? C7 C8 1.396(6) . ? C8 C9 1.378(8) . ? C9 C10 1.366(9) . ? C10 C11 1.395(8) . ? C11 C12 1.387(7) . ? C13 C14 1.385(6) . ? C13 C18 1.385(5) . ? C14 C15 1.397(6) . ? C15 C16 1.373(7) . ? C16 C17 1.361(7) . ? C17 C18 1.397(7) . ? C19 C20 1.390(6) . ? C19 C24 1.406(6) . ? C20 C21 1.382(7) . ? C21 C22 1.387(8) . ? C22 C23 1.383(8) . ? C23 C24 1.377(7) . ? O1 C25 1.395(7) . ? O1 C34 1.426(6) . ? O1 Li 2.224(9) . ? O2 C27 1.368(7) . ? O2 C26 1.380(7) . ? O2 Li 2.421(9) . ? O3 C29 1.315(8) . ? O3 C28 1.380(8) . ? O3 Li 2.209(9) . ? O4 C31 1.269(8) . ? O4 C30 1.314(8) . ? O4 Li 2.269(10) . ? O5 C33 1.305(7) . ? O5 C32 1.416(8) . ? O5 Li 2.223(9) . ? O6 Li 1.899(10) . ? C25 C26 1.471(8) . ? C27 C28 1.471(10) . ? C29 C30 1.457(10) . ? C31 C32 1.363(12) . ? C33 C34 1.450(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 C7 110.11(18) . . ? N1 P1 C1 103.52(17) . . ? C7 P1 C1 102.30(18) . . ? N1 P1 S1 120.83(15) . . ? C7 P1 S1 109.98(14) . . ? C1 P1 S1 108.29(14) . . ? N1 P2 C13 104.68(17) . . ? N1 P2 C19 107.65(18) . . ? C13 P2 C19 100.67(17) . . ? N1 P2 S2 121.90(13) . . ? C13 P2 S2 110.39(13) . . ? C19 P2 S2 109.42(14) . . ? P1 N1 P2 136.1(2) . . ? C2 C1 C6 118.5(4) . . ? C2 C1 P1 120.7(3) . . ? C6 C1 P1 120.9(3) . . ? C1 C2 C3 120.6(4) . . ? C4 C3 C2 120.8(4) . . ? C5 C4 C3 119.2(4) . . ? C4 C5 C6 120.4(4) . . ? C1 C6 C5 120.5(4) . . ? C12 C7 C8 118.1(4) . . ? C12 C7 P1 119.7(3) . . ? C8 C7 P1 122.2(4) . . ? C9 C8 C7 120.7(5) . . ? C10 C9 C8 120.8(5) . . ? C9 C10 C11 119.8(5) . . ? C12 C11 C10 119.2(6) . . ? C11 C12 C7 121.3(5) . . ? C14 C13 C18 118.9(4) . . ? C14 C13 P2 120.1(3) . . ? C18 C13 P2 120.9(3) . . ? C13 C14 C15 120.2(4) . . ? C16 C15 C14 120.0(4) . . ? C17 C16 C15 120.4(4) . . ? C16 C17 C18 120.1(4) . . ? C13 C18 C17 120.4(4) . . ? C20 C19 C24 118.5(4) . . ? C20 C19 P2 119.9(3) . . ? C24 C19 P2 121.4(3) . . ? C21 C20 C19 121.1(5) . . ? C20 C21 C22 119.7(5) . . ? C23 C22 C21 120.0(5) . . ? C24 C23 C22 120.5(5) . . ? C23 C24 C19 120.3(5) . . ? C25 O1 C34 114.9(5) . . ? C25 O1 Li 113.4(4) . . ? C34 O1 Li 109.9(4) . . ? C27 O2 C26 116.7(5) . . ? C27 O2 Li 112.0(4) . . ? C26 O2 Li 112.3(4) . . ? C29 O3 C28 116.2(6) . . ? C29 O3 Li 114.1(5) . . ? C28 O3 Li 116.4(5) . . ? C31 O4 C30 125.5(8) . . ? C31 O4 Li 115.5(6) . . ? C30 O4 Li 114.9(5) . . ? C33 O5 C32 117.1(6) . . ? C33 O5 Li 115.2(5) . . ? C32 O5 Li 115.2(5) . . ? O6 Li O3 107.1(4) . . ? O6 Li O5 94.3(4) . . ? O3 Li O5 140.2(5) . . ? O6 Li O1 111.5(4) . . ? O3 Li O1 125.5(4) . . ? O5 Li O1 73.0(3) . . ? O6 Li O4 99.5(4) . . ? O3 Li O4 71.8(3) . . ? O5 Li O4 71.7(3) . . ? O1 Li O4 134.1(4) . . ? O6 Li O2 96.0(4) . . ? O3 Li O2 69.6(3) . . ? O5 Li O2 142.2(4) . . ? O1 Li O2 69.4(3) . . ? O4 Li O2 141.1(4) . . ? O1 C25 C26 107.3(5) . . ? O2 C26 C25 108.9(5) . . ? O2 C27 C28 110.5(6) . . ? O3 C28 C27 108.5(6) . . ? O3 C29 C30 113.5(6) . . ? O4 C30 C29 114.5(6) . . ? O4 C31 C32 120.7(8) . . ? C31 C32 O5 114.5(7) . . ? O5 C33 C34 110.5(5) . . ? O1 C34 C33 109.4(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6A S1 0.894(10) 2.467(18) 3.334(4) 163(4) 2_556 O6 H6B S2 0.893(10) 2.384(17) 3.255(4) 165(4) 2_556 #==END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 220676' _chemical_name_common (Li(15C5))(Ph2SePNPSePh2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety ? _chemical_formula_sum 'C34 H42 Li N O6 P2 Se2' _chemical_formula_weight 787.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.449(5) _cell_length_b 12.050(3) _cell_length_c 13.894(3) _cell_angle_alpha 97.60(2) _cell_angle_beta 91.13(3) _cell_angle_gamma 103.26(3) _cell_volume 1846.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 4.85 _cell_measurement_theta_max 24.96 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 2.131 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.5093 _exptl_absorpt_correction_T_max 0.5667 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4/PC' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 6793 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0979 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6445 _reflns_number_gt 3589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'xscans ver 2.1 (Siemens 1994)' _computing_cell_refinement 'xscans ver 2.1 (Siemens 1994)' _computing_data_reduction 'xscans ver 2.1 (Siemens 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP SHELXTL/PC (Sheldrick 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^] 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 'noref except H6A and H6B on O6' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0055(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6445 _refine_ls_number_parameters 422 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1111 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.25690(6) 0.11487(5) 0.73943(5) 0.0654(2) Uani 1 d . . . Se2 Se 0.07678(6) 0.35078(5) 0.91223(4) 0.0557(2) Uani 1 d . . . P1 P 0.30559(11) 0.29078(11) 0.71294(9) 0.0393(3) Uani 1 d . . . P2 P 0.11959(11) 0.41444(10) 0.77840(9) 0.0371(3) Uani 1 d . . . N1 N 0.2049(4) 0.3624(4) 0.7052(3) 0.0472(10) Uani 1 d . . . C1 C 0.3740(4) 0.2934(4) 0.5939(3) 0.0405(11) Uani 1 d . . . C2 C 0.3539(5) 0.3691(5) 0.5336(4) 0.0553(14) Uani 1 d . . . H2 H 0.3077 0.4213 0.5538 0.060 Uiso 1 calc R . . C3 C 0.4021(6) 0.3685(6) 0.4420(4) 0.0676(17) Uani 1 d . . . H3 H 0.3875 0.4196 0.4012 0.060 Uiso 1 calc R . . C4 C 0.4706(5) 0.2930(5) 0.4126(4) 0.0644(16) Uani 1 d . . . H4 H 0.5013 0.2915 0.3511 0.060 Uiso 1 calc R . . C5 C 0.4946(6) 0.2187(6) 0.4736(5) 0.0701(17) Uani 1 d . . . H5 H 0.5438 0.1691 0.4542 0.060 Uiso 1 calc R . . C6 C 0.4447(5) 0.2182(5) 0.5647(4) 0.0597(15) Uani 1 d . . . H6 H 0.4594 0.1671 0.6055 0.060 Uiso 1 calc R . . C7 C 0.4287(4) 0.3727(4) 0.7980(3) 0.0434(11) Uani 1 d . . . C8 C 0.4802(5) 0.3237(6) 0.8661(4) 0.0631(16) Uani 1 d . . . H8 H 0.4508 0.2464 0.8718 0.060 Uiso 1 calc R . . C9 C 0.5748(7) 0.3882(9) 0.9258(5) 0.086(2) Uani 1 d . . . H9 H 0.6085 0.3535 0.9717 0.060 Uiso 1 calc R . . C10 C 0.6211(6) 0.5012(9) 0.9202(5) 0.091(3) Uani 1 d . . . H10 H 0.6850 0.5436 0.9619 0.060 Uiso 1 calc R . . C11 C 0.5711(6) 0.5523(7) 0.8507(6) 0.084(2) Uani 1 d . . . H11 H 0.6025 0.6292 0.8448 0.060 Uiso 1 calc R . . C12 C 0.4742(5) 0.4885(5) 0.7904(4) 0.0582(14) Uani 1 d . . . H12 H 0.4397 0.5231 0.7448 0.060 Uiso 1 calc R . . C13 C -0.0183(4) 0.4040(4) 0.7050(3) 0.0376(10) Uani 1 d . . . C14 C -0.1220(5) 0.4205(5) 0.7472(4) 0.0561(14) Uani 1 d . . . H14 H -0.1228 0.4342 0.8146 0.060 Uiso 1 calc R . . C15 C -0.2250(5) 0.4170(5) 0.6921(5) 0.0684(17) Uani 1 d . . . H15 H -0.2950 0.4258 0.7219 0.060 Uiso 1 calc R . . C16 C -0.2222(5) 0.4004(5) 0.5921(5) 0.0663(17) Uani 1 d . . . H16 H -0.2903 0.3996 0.5541 0.060 Uiso 1 calc R . . C17 C -0.1186(6) 0.3849(6) 0.5480(5) 0.0682(17) Uani 1 d . . . H17 H -0.1174 0.3733 0.4805 0.060 Uiso 1 calc R . . C18 C -0.0173(5) 0.3866(5) 0.6038(4) 0.0559(14) Uani 1 d . . . H18 H 0.0521 0.3761 0.5739 0.060 Uiso 1 calc R . . C19 C 0.1786(4) 0.5718(4) 0.8025(4) 0.0447(12) Uani 1 d . . . C20 C 0.2277(5) 0.6300(5) 0.7277(4) 0.0579(14) Uani 1 d . . . H20 H 0.2350 0.5882 0.6678 0.060 Uiso 1 calc R . . C21 C 0.2661(6) 0.7492(5) 0.7400(5) 0.0700(17) Uani 1 d . . . H21 H 0.3001 0.7866 0.6893 0.060 Uiso 1 calc R . . C22 C 0.2534(6) 0.8117(5) 0.8285(6) 0.0778(19) Uani 1 d . . . H22 H 0.2771 0.8916 0.8372 0.060 Uiso 1 calc R . . C23 C 0.2051(6) 0.7546(5) 0.9042(5) 0.0705(17) Uani 1 d . . . H23 H 0.1986 0.7967 0.9642 0.060 Uiso 1 calc R . . C24 C 0.1663(5) 0.6354(5) 0.8915(4) 0.0549(14) Uani 1 d . . . H24 H 0.1322 0.5981 0.9423 0.060 Uiso 1 calc R . . O1 O -0.2018(4) -0.1785(4) 0.8662(3) 0.0705(11) Uani 1 d . . . O2 O -0.0634(6) -0.1674(4) 0.7165(4) 0.0985(17) Uani 1 d . . . O3 O -0.1510(8) -0.0400(6) 0.6092(4) 0.139(3) Uani 1 d . . . O4 O -0.2929(6) 0.0507(5) 0.7170(4) 0.1115(19) Uani 1 d . . . O5 O -0.2953(4) 0.0046(4) 0.8969(4) 0.0800(13) Uani 1 d . . . O6 O -0.0280(5) 0.0719(4) 0.8247(4) 0.0985(17) Uani 1 d D . . H6A H 0.036(3) 0.052(5) 0.797(4) 0.060 Uiso 1 d D . . H6B H -0.023(5) 0.143(2) 0.854(4) 0.060 Uiso 1 d D . . Li Li -0.1682(9) -0.0401(8) 0.7713(8) 0.063(2) Uani 1 d . . . C25 C -0.1055(7) -0.2357(7) 0.8604(5) 0.089(2) Uani 1 d . . . H25A H -0.1265 -0.3051 0.8909 0.060 Uiso 1 calc R . . H25B H -0.0339 -0.1859 0.8944 0.060 Uiso 1 calc R . . C26 C -0.0826(7) -0.2653(6) 0.7581(5) 0.080(2) Uani 1 d . . . H26A H -0.0126 -0.2979 0.7528 0.060 Uiso 1 calc R . . H26B H -0.1510 -0.3216 0.7254 0.060 Uiso 1 calc R . . C27 C -0.0493(12) -0.1821(9) 0.6163(6) 0.147(5) Uani 1 d . . . H27A H 0.0354 -0.1739 0.6051 0.060 Uiso 1 calc R . . H27B H -0.0908 -0.2600 0.5894 0.060 Uiso 1 calc R . . C28 C -0.0907(10) -0.1080(9) 0.5683(6) 0.118(3) Uani 1 d . . . H28A H -0.0215 -0.0604 0.5426 0.060 Uiso 1 calc R . . H28B H -0.1399 -0.1533 0.5129 0.060 Uiso 1 calc R . . C29 C -0.2062(9) 0.0300(9) 0.5732(6) 0.110(3) Uani 1 d . . . H29A H -0.2628 -0.0152 0.5219 0.060 Uiso 1 calc R . . H29B H -0.1469 0.0837 0.5428 0.060 Uiso 1 calc R . . C30 C -0.2677(10) 0.0934(9) 0.6341(7) 0.128(4) Uani 1 d . . . H30A H -0.2200 0.1718 0.6490 0.060 Uiso 1 calc R . . H30B H -0.3422 0.0957 0.6008 0.060 Uiso 1 calc R . . C31 C -0.3449(9) 0.1205(9) 0.7879(7) 0.124(4) Uani 1 d . . . H31A H -0.4106 0.1448 0.7584 0.060 Uiso 1 calc R . . H31B H -0.2851 0.1883 0.8166 0.060 Uiso 1 calc R . . C32 C -0.3890(7) 0.0455(8) 0.8625(6) 0.101(3) Uani 1 d . . . H32A H -0.4202 0.0890 0.9157 0.060 Uiso 1 calc R . . H32B H -0.4535 -0.0185 0.8342 0.060 Uiso 1 calc R . . C33 C -0.3271(7) -0.0832(6) 0.9543(5) 0.084(2) Uani 1 d . . . H33A H -0.3975 -0.1399 0.9252 0.060 Uiso 1 calc R . . H33B H -0.3456 -0.0519 1.0186 0.060 Uiso 1 calc R . . C34 C -0.2239(7) -0.1375(7) 0.9611(5) 0.087(2) Uani 1 d . . . H34A H -0.1538 -0.0815 0.9915 0.060 Uiso 1 calc R . . H34B H -0.2432 -0.2003 0.9995 0.060 Uiso 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 0.0692(4) 0.0491(3) 0.0852(5) 0.0233(3) 0.0263(4) 0.0190(3) Se2 0.0702(4) 0.0592(4) 0.0415(3) 0.0173(3) 0.0094(3) 0.0164(3) P1 0.0350(7) 0.0443(7) 0.0427(7) 0.0086(5) 0.0083(5) 0.0156(6) P2 0.0354(7) 0.0421(7) 0.0364(6) 0.0078(5) 0.0041(5) 0.0131(5) N1 0.044(2) 0.055(3) 0.047(2) 0.012(2) 0.0061(19) 0.018(2) C1 0.033(3) 0.045(3) 0.041(3) 0.000(2) 0.004(2) 0.007(2) C2 0.066(4) 0.054(3) 0.053(3) 0.013(3) 0.018(3) 0.023(3) C3 0.074(4) 0.076(4) 0.061(4) 0.023(3) 0.021(3) 0.025(3) C4 0.062(4) 0.080(4) 0.048(3) 0.009(3) 0.020(3) 0.010(3) C5 0.065(4) 0.083(4) 0.069(4) 0.007(3) 0.029(3) 0.031(3) C6 0.057(4) 0.075(4) 0.058(3) 0.015(3) 0.017(3) 0.034(3) C7 0.029(2) 0.061(3) 0.044(3) 0.006(2) 0.008(2) 0.019(2) C8 0.050(3) 0.091(4) 0.056(3) 0.013(3) 0.000(3) 0.030(3) C9 0.067(5) 0.136(7) 0.059(4) -0.011(4) -0.015(4) 0.049(5) C10 0.050(4) 0.148(8) 0.057(4) -0.044(5) -0.018(3) 0.021(5) C11 0.062(4) 0.084(5) 0.088(5) -0.016(4) 0.004(4) -0.002(4) C12 0.046(3) 0.063(4) 0.063(4) -0.002(3) 0.003(3) 0.012(3) C13 0.034(3) 0.037(2) 0.043(3) 0.003(2) 0.002(2) 0.014(2) C14 0.051(3) 0.063(3) 0.059(3) 0.007(3) 0.009(3) 0.024(3) C15 0.037(3) 0.083(4) 0.092(5) 0.010(4) 0.005(3) 0.028(3) C16 0.052(4) 0.064(4) 0.084(5) 0.006(3) -0.024(3) 0.021(3) C17 0.065(4) 0.090(5) 0.051(3) 0.004(3) -0.012(3) 0.025(3) C18 0.044(3) 0.075(4) 0.048(3) 0.004(3) 0.001(3) 0.016(3) C19 0.043(3) 0.048(3) 0.045(3) 0.007(2) 0.003(2) 0.015(2) C20 0.068(4) 0.049(3) 0.060(3) 0.012(3) 0.009(3) 0.018(3) C21 0.066(4) 0.056(4) 0.088(5) 0.024(3) 0.020(4) 0.007(3) C22 0.069(4) 0.046(3) 0.107(6) 0.001(4) -0.002(4) -0.002(3) C23 0.083(5) 0.054(4) 0.067(4) -0.016(3) -0.006(4) 0.018(3) C24 0.053(3) 0.061(3) 0.052(3) 0.009(3) 0.002(3) 0.015(3) O1 0.076(3) 0.074(3) 0.069(3) 0.023(2) 0.017(2) 0.025(2) O2 0.160(5) 0.075(3) 0.075(3) 0.018(2) 0.041(3) 0.050(3) O3 0.238(8) 0.142(5) 0.073(4) 0.008(4) 0.017(4) 0.123(6) O4 0.134(5) 0.131(5) 0.095(4) 0.041(4) 0.038(4) 0.067(4) O5 0.076(3) 0.078(3) 0.096(3) 0.022(3) 0.018(3) 0.030(2) O6 0.071(3) 0.070(3) 0.136(5) -0.024(3) 0.029(3) -0.001(3) Li 0.056(6) 0.053(5) 0.076(6) 0.016(5) 0.001(5) 0.002(4) C25 0.102(6) 0.102(5) 0.093(5) 0.043(4) 0.030(4) 0.067(5) C26 0.089(5) 0.065(4) 0.100(5) 0.019(4) 0.017(4) 0.040(4) C27 0.258(14) 0.145(9) 0.083(6) 0.021(6) 0.070(7) 0.128(10) C28 0.163(9) 0.144(8) 0.064(5) 0.019(5) 0.048(6) 0.061(7) C29 0.117(7) 0.134(8) 0.089(6) 0.040(6) 0.006(5) 0.036(6) C30 0.179(10) 0.134(8) 0.112(7) 0.061(6) 0.038(7) 0.095(8) C31 0.144(8) 0.157(9) 0.119(7) 0.057(7) 0.044(6) 0.109(8) C32 0.087(5) 0.123(7) 0.107(6) 0.009(5) 0.030(5) 0.051(5) C33 0.101(6) 0.083(5) 0.071(4) 0.012(4) 0.035(4) 0.026(4) C34 0.107(6) 0.090(5) 0.075(5) 0.033(4) 0.019(4) 0.031(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 P1 2.1476(14) . ? Se2 P2 2.1276(13) . ? P1 N1 1.600(4) . ? P1 C7 1.829(5) . ? P1 C1 1.844(5) . ? P2 N1 1.592(4) . ? P2 C13 1.833(5) . ? P2 C19 1.844(5) . ? C1 C2 1.371(7) . ? C1 C6 1.376(7) . ? C2 C3 1.397(8) . ? C3 C4 1.360(9) . ? C4 C5 1.378(9) . ? C5 C6 1.400(8) . ? C7 C8 1.371(7) . ? C7 C12 1.392(8) . ? C8 C9 1.369(10) . ? C9 C10 1.356(11) . ? C10 C11 1.391(11) . ? C11 C12 1.388(9) . ? C13 C14 1.378(7) . ? C13 C18 1.394(7) . ? C14 C15 1.383(8) . ? C15 C16 1.380(9) . ? C16 C17 1.384(9) . ? C17 C18 1.377(8) . ? C19 C20 1.387(7) . ? C19 C24 1.394(7) . ? C20 C21 1.388(8) . ? C21 C22 1.383(9) . ? C22 C23 1.388(9) . ? C23 C24 1.389(8) . ? O1 C34 1.395(8) . ? O1 C25 1.426(7) . ? O1 Li 2.230(10) . ? O2 C26 1.356(7) . ? O2 C27 1.398(9) . ? O2 Li 2.223(11) . ? O3 C28 1.273(10) . ? O3 C29 1.305(9) . ? O3 Li 2.266(12) . ? O4 C30 1.332(9) . ? O4 C31 1.438(10) . ? O4 Li 2.167(11) . ? O5 C32 1.381(9) . ? O5 C33 1.396(8) . ? O5 Li 2.379(12) . ? O6 Li 1.908(11) . ? C25 C26 1.464(10) . ? C27 C28 1.344(11) . ? C29 C30 1.377(12) . ? C31 C32 1.485(11) . ? C33 C34 1.482(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 C7 110.2(2) . . ? N1 P1 C1 103.5(2) . . ? C7 P1 C1 103.2(2) . . ? N1 P1 Se1 120.45(17) . . ? C7 P1 Se1 110.03(17) . . ? C1 P1 Se1 107.87(16) . . ? N1 P2 C13 104.6(2) . . ? N1 P2 C19 108.0(2) . . ? C13 P2 C19 101.2(2) . . ? N1 P2 Se2 121.76(15) . . ? C13 P2 Se2 110.15(15) . . ? C19 P2 Se2 109.14(16) . . ? P2 N1 P1 135.9(3) . . ? C2 C1 C6 119.5(5) . . ? C2 C1 P1 120.4(4) . . ? C6 C1 P1 120.0(4) . . ? C1 C2 C3 120.5(5) . . ? C4 C3 C2 119.9(6) . . ? C3 C4 C5 120.3(5) . . ? C4 C5 C6 119.7(6) . . ? C1 C6 C5 120.0(5) . . ? C8 C7 C12 119.0(5) . . ? C8 C7 P1 122.7(4) . . ? C12 C7 P1 118.2(4) . . ? C9 C8 C7 120.2(7) . . ? C10 C9 C8 122.1(7) . . ? C9 C10 C11 118.6(6) . . ? C12 C11 C10 120.1(7) . . ? C11 C12 C7 119.9(6) . . ? C14 C13 C18 118.5(5) . . ? C14 C13 P2 121.5(4) . . ? C18 C13 P2 119.8(4) . . ? C13 C14 C15 121.8(5) . . ? C16 C15 C14 118.9(5) . . ? C15 C16 C17 120.3(5) . . ? C18 C17 C16 120.2(6) . . ? C17 C18 C13 120.3(5) . . ? C20 C19 C24 118.8(5) . . ? C20 C19 P2 119.2(4) . . ? C24 C19 P2 121.8(4) . . ? C19 C20 C21 121.6(6) . . ? C22 C21 C20 119.3(6) . . ? C21 C22 C23 119.8(6) . . ? C22 C23 C24 120.8(6) . . ? C23 C24 C19 119.7(5) . . ? C34 O1 C25 113.5(5) . . ? C34 O1 Li 112.3(5) . . ? C25 O1 Li 109.4(4) . . ? C26 O2 C27 115.2(6) . . ? C26 O2 Li 116.3(5) . . ? C27 O2 Li 116.1(6) . . ? C28 O3 C29 130.8(8) . . ? C28 O3 Li 115.4(6) . . ? C29 O3 Li 113.7(6) . . ? C30 O4 C31 115.2(7) . . ? C30 O4 Li 116.9(6) . . ? C31 O4 Li 116.9(6) . . ? C32 O5 C33 115.7(6) . . ? C32 O5 Li 112.1(5) . . ? C33 O5 Li 112.4(4) . . ? O6 Li O4 107.8(5) . . ? O6 Li O2 93.0(5) . . ? O4 Li O2 139.5(6) . . ? O6 Li O1 107.3(5) . . ? O4 Li O1 129.1(5) . . ? O2 Li O1 72.7(3) . . ? O6 Li O3 102.6(5) . . ? O4 Li O3 70.5(4) . . ? O2 Li O3 71.3(4) . . ? O1 Li O3 133.7(5) . . ? O6 Li O5 95.8(5) . . ? O4 Li O5 70.5(4) . . ? O2 Li O5 142.8(5) . . ? O1 Li O5 70.3(3) . . ? O3 Li O5 140.4(5) . . ? O1 C25 C26 109.0(6) . . ? O2 C26 C25 107.9(6) . . ? C28 C27 O2 114.5(7) . . ? O3 C28 C27 122.2(8) . . ? O3 C29 C30 119.0(8) . . ? O4 C30 C29 112.9(7) . . ? O4 C31 C32 105.2(7) . . ? O5 C32 C31 109.1(7) . . ? O5 C33 C34 107.8(6) . . ? O1 C34 C33 106.6(6) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.383 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.072