data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Stalke, Dietmar' _publ_contact_author_email dstalke@chemie.uni-goettingen.de _publ_section_title ; Synthesis and single crystal X-ray structures of new hemilabile tripodal ligands and their magnesium complex; ; loop_ _publ_author_name D.Stalke M.Meinholz S.Pandey # Attachment '- all_full.cif' data_p-1a _database_code_depnum_ccdc_archive 'CCDC 779986' #TrackingRef '- all_comm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H52 Li2 N4 P2 S2' _chemical_formula_weight 512.62 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' Li Li -0.0003 0.0001 '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 9.4916(4) _cell_length_b 9.6726(4) _cell_length_c 18.7808(8) _cell_angle_alpha 98.7720(10) _cell_angle_beta 92.0040(10) _cell_angle_gamma 114.7780(10) _cell_volume 1537.76(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9975 _cell_measurement_theta_min 2.208 _cell_measurement_theta_max 28.74 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.293 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7806 _exptl_absorpt_correction_T_max 0.9893 _exptl_absorpt_process_details SADABS-2008/2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS-Mo rotating anode' _diffrn_radiation_monochromator 'INCOATEC Helios mirror optics' _diffrn_measurement_device_type 'Bruker TXS-Mo rotating anode' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27095 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 28.75 _reflns_number_total 7923 _reflns_number_gt 6893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.2-0' _computing_cell_refinement 'SAINT V7.46A' _computing_data_reduction 'SAINT V7.46A' _computing_structure_solution 'SHELXS in SHELXTL v2008/4 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL in SHELXTL v2008/4 (Sheldrick 2008)' _computing_molecular_graphics 'XSHELL v4.01' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.4680P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7923 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.67079(12) 0.49683(12) 0.37342(6) 0.0176(2) Uani 1 1 d . . . C2 C 0.72744(14) 0.44452(13) 0.43730(6) 0.0235(2) Uani 1 1 d . . . H2A H 0.7938 0.3939 0.4207 0.035 Uiso 1 1 calc R . . H2B H 0.6372 0.3714 0.4568 0.035 Uiso 1 1 calc R . . H2C H 0.7874 0.5349 0.4753 0.035 Uiso 1 1 calc R . . C3 C 0.56609(14) 0.57478(14) 0.40007(7) 0.0252(2) Uani 1 1 d . . . H3A H 0.6260 0.6652 0.4380 0.038 Uiso 1 1 calc R . . H3B H 0.4767 0.5010 0.4198 0.038 Uiso 1 1 calc R . . H3C H 0.5287 0.6079 0.3595 0.038 Uiso 1 1 calc R . . C4 C 0.57532(14) 0.35459(13) 0.31540(6) 0.0247(2) Uani 1 1 d . . . H4A H 0.5362 0.3864 0.2748 0.037 Uiso 1 1 calc R . . H4B H 0.4870 0.2819 0.3361 0.037 Uiso 1 1 calc R . . H4C H 0.6414 0.3042 0.2980 0.037 Uiso 1 1 calc R . . C5 C 1.21558(12) 0.78467(12) 0.38120(6) 0.0175(2) Uani 1 1 d . . . C6 C 1.26103(14) 0.87546(14) 0.45950(6) 0.0251(2) Uani 1 1 d . . . H6A H 1.2850 0.9844 0.4595 0.038 Uiso 1 1 calc R . . H6B H 1.3530 0.8683 0.4806 0.038 Uiso 1 1 calc R . . H6C H 1.1740 0.8316 0.4882 0.038 Uiso 1 1 calc R . . C7 C 1.17751(13) 0.61477(13) 0.38255(6) 0.0213(2) Uani 1 1 d . . . H7A H 1.0887 0.5716 0.4104 0.032 Uiso 1 1 calc R . . H7B H 1.2685 0.6082 0.4053 0.032 Uiso 1 1 calc R . . H7C H 1.1510 0.5559 0.3328 0.032 Uiso 1 1 calc R . . C8 C 1.35474(13) 0.85277(14) 0.33834(7) 0.0244(2) Uani 1 1 d . . . H8A H 1.3273 0.7976 0.2880 0.037 Uiso 1 1 calc R . . H8B H 1.4440 0.8416 0.3599 0.037 Uiso 1 1 calc R . . H8C H 1.3822 0.9628 0.3396 0.037 Uiso 1 1 calc R . . C9 C 0.87220(13) 0.90831(12) 0.37648(6) 0.0204(2) Uani 1 1 d . . . H9A H 0.7629 0.8600 0.3536 0.024 Uiso 1 1 calc R . . H9B H 0.8741 0.9646 0.4254 0.024 Uiso 1 1 calc R . . C10 C 1.14556(15) 1.19217(14) 0.39218(7) 0.0282(3) Uani 1 1 d . . . H10A H 1.0992 1.2118 0.4362 0.042 Uiso 1 1 calc R . . H10B H 1.1989 1.2891 0.3742 0.042 Uiso 1 1 calc R . . H10C H 1.2210 1.1516 0.4033 0.042 Uiso 1 1 calc R . . C11 C 0.86591(15) 1.15150(14) 0.31822(7) 0.0264(2) Uani 1 1 d . . . H11A H 0.8355 1.1734 0.3665 0.040 Uiso 1 1 calc R . . H11B H 0.7722 1.0859 0.2845 0.040 Uiso 1 1 calc R . . H11C H 0.9230 1.2490 0.3012 0.040 Uiso 1 1 calc R . . C12 C 0.75324(12) 0.66453(13) 0.12814(6) 0.0187(2) Uani 1 1 d . . . C13 C 0.64808(15) 0.49324(16) 0.09824(8) 0.0375(3) Uani 1 1 d . . . H13A H 0.6960 0.4547 0.0594 0.056 Uiso 1 1 calc R . . H13B H 0.5458 0.4820 0.0790 0.056 Uiso 1 1 calc R . . H13C H 0.6352 0.4335 0.1372 0.056 Uiso 1 1 calc R . . C14 C 0.76796(16) 0.75701(19) 0.06732(7) 0.0366(3) Uani 1 1 d . . . H14A H 0.8399 0.8658 0.0851 0.055 Uiso 1 1 calc R . . H14B H 0.6652 0.7497 0.0515 0.055 Uiso 1 1 calc R . . H14C H 0.8082 0.7148 0.0264 0.055 Uiso 1 1 calc R . . C15 C 0.67615(13) 0.72256(15) 0.18794(6) 0.0250(2) Uani 1 1 d . . . H15A H 0.6699 0.6678 0.2284 0.037 Uiso 1 1 calc R . . H15B H 0.5708 0.7032 0.1690 0.037 Uiso 1 1 calc R . . H15C H 0.7382 0.8340 0.2049 0.037 Uiso 1 1 calc R . . C16 C 1.31860(13) 0.91967(13) 0.12001(6) 0.0194(2) Uani 1 1 d . . . C17 C 1.45983(14) 1.01230(15) 0.17634(7) 0.0286(3) Uani 1 1 d . . . H17A H 1.4301 1.0671 0.2170 0.043 Uiso 1 1 calc R . . H17B H 1.5432 1.0876 0.1543 0.043 Uiso 1 1 calc R . . H17C H 1.4969 0.9418 0.1939 0.043 Uiso 1 1 calc R . . C18 C 1.36684(14) 0.83256(14) 0.05765(6) 0.0252(2) Uani 1 1 d . . . H18A H 1.3951 0.7565 0.0756 0.038 Uiso 1 1 calc R . . H18B H 1.4568 0.9064 0.0383 0.038 Uiso 1 1 calc R . . H18C H 1.2795 0.7791 0.0192 0.038 Uiso 1 1 calc R . . C19 C 1.26554(16) 1.03214(15) 0.09081(8) 0.0310(3) Uani 1 1 d . . . H19A H 1.1743 0.9735 0.0548 0.047 Uiso 1 1 calc R . . H19B H 1.3505 1.1042 0.0681 0.047 Uiso 1 1 calc R . . H19C H 1.2380 1.0905 0.1309 0.047 Uiso 1 1 calc R . . C20 C 1.03819(13) 0.50793(12) 0.09219(6) 0.0189(2) Uani 1 1 d . . . H20A H 1.1318 0.5153 0.0683 0.023 Uiso 1 1 calc R . . H20B H 0.9454 0.4355 0.0583 0.023 Uiso 1 1 calc R . . C21 C 0.94610(16) 0.21879(14) 0.13297(7) 0.0282(3) Uani 1 1 d . . . H21A H 0.9971 0.2020 0.0901 0.042 Uiso 1 1 calc R . . H21B H 0.8350 0.1861 0.1186 0.042 Uiso 1 1 calc R . . H21C H 0.9576 0.1580 0.1681 0.042 Uiso 1 1 calc R . . C22 C 1.24065(14) 0.45648(16) 0.18984(7) 0.0298(3) Uani 1 1 d . . . H22A H 1.2516 0.4043 0.2291 0.045 Uiso 1 1 calc R . . H22B H 1.3080 0.5678 0.2034 0.045 Uiso 1 1 calc R . . H22C H 1.2712 0.4141 0.1454 0.045 Uiso 1 1 calc R . . Li1 Li 0.9110(2) 0.5859(2) 0.25274(10) 0.0209(4) Uani 1 1 d . . . Li2 Li 1.0872(2) 0.8641(2) 0.24244(10) 0.0202(4) Uani 1 1 d . . . N1 N 0.80074(10) 0.59661(10) 0.33685(5) 0.01601(17) Uani 1 1 d . . . N2 N 1.08429(10) 0.80123(10) 0.34249(5) 0.01613(17) Uani 1 1 d . . . N3 N 0.90586(10) 0.68391(10) 0.16300(5) 0.01602(17) Uani 1 1 d . . . N4 N 1.19769(10) 0.81253(10) 0.15885(5) 0.01724(17) Uani 1 1 d . . . P1 P 0.99195(3) 1.05051(3) 0.322930(15) 0.01791(6) Uani 1 1 d . . . P2 P 1.03736(3) 0.42535(3) 0.174266(15) 0.01757(6) Uani 1 1 d . . . S1 S 0.93051(3) 0.75275(3) 0.386810(13) 0.01480(6) Uani 1 1 d . . . S2 S 1.03775(3) 0.69947(3) 0.107592(13) 0.01546(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0171(5) 0.0156(5) 0.0202(5) 0.0038(4) 0.0053(4) 0.0067(4) C2 0.0291(6) 0.0202(5) 0.0230(5) 0.0084(4) 0.0062(4) 0.0107(5) C3 0.0212(5) 0.0231(6) 0.0346(6) 0.0081(5) 0.0133(5) 0.0110(5) C4 0.0209(5) 0.0204(5) 0.0268(6) 0.0019(4) 0.0044(4) 0.0037(4) C5 0.0149(5) 0.0210(5) 0.0174(5) 0.0032(4) 0.0010(4) 0.0087(4) C6 0.0254(6) 0.0290(6) 0.0206(5) -0.0005(4) -0.0037(4) 0.0136(5) C7 0.0216(5) 0.0240(5) 0.0219(5) 0.0056(4) 0.0023(4) 0.0126(4) C8 0.0160(5) 0.0301(6) 0.0286(6) 0.0095(5) 0.0042(4) 0.0098(4) C9 0.0210(5) 0.0167(5) 0.0265(5) 0.0051(4) 0.0092(4) 0.0103(4) C10 0.0270(6) 0.0196(5) 0.0315(6) 0.0003(5) 0.0010(5) 0.0054(5) C11 0.0334(6) 0.0236(6) 0.0298(6) 0.0068(5) 0.0078(5) 0.0185(5) C12 0.0152(5) 0.0228(5) 0.0185(5) 0.0028(4) 0.0006(4) 0.0089(4) C13 0.0201(6) 0.0313(7) 0.0502(8) -0.0115(6) -0.0031(5) 0.0074(5) C14 0.0300(7) 0.0620(10) 0.0323(7) 0.0251(6) 0.0077(5) 0.0280(7) C15 0.0201(5) 0.0345(6) 0.0238(5) 0.0018(5) 0.0016(4) 0.0163(5) C16 0.0169(5) 0.0191(5) 0.0214(5) 0.0051(4) 0.0067(4) 0.0064(4) C17 0.0206(6) 0.0277(6) 0.0270(6) 0.0026(5) 0.0052(4) 0.0008(5) C18 0.0233(6) 0.0282(6) 0.0235(5) 0.0046(4) 0.0099(4) 0.0100(5) C19 0.0321(7) 0.0256(6) 0.0411(7) 0.0158(5) 0.0115(5) 0.0141(5) C20 0.0231(5) 0.0178(5) 0.0164(5) 0.0013(4) 0.0043(4) 0.0099(4) C21 0.0352(7) 0.0195(5) 0.0284(6) 0.0048(4) 0.0066(5) 0.0099(5) C22 0.0240(6) 0.0388(7) 0.0303(6) 0.0022(5) 0.0018(5) 0.0187(5) Li1 0.0246(10) 0.0225(9) 0.0195(9) 0.0050(7) 0.0061(7) 0.0133(8) Li2 0.0202(9) 0.0211(9) 0.0193(9) 0.0030(7) 0.0048(7) 0.0091(7) N1 0.0151(4) 0.0153(4) 0.0163(4) 0.0021(3) 0.0039(3) 0.0054(3) N2 0.0135(4) 0.0205(4) 0.0164(4) 0.0052(3) 0.0037(3) 0.0085(3) N3 0.0144(4) 0.0214(4) 0.0144(4) 0.0034(3) 0.0028(3) 0.0096(3) N4 0.0153(4) 0.0185(4) 0.0152(4) 0.0022(3) 0.0033(3) 0.0049(3) P1 0.02022(13) 0.01593(13) 0.01862(13) 0.00303(10) 0.00499(10) 0.00860(10) P2 0.01922(13) 0.01898(13) 0.01674(13) 0.00319(10) 0.00431(10) 0.01020(11) S1 0.01524(11) 0.01554(12) 0.01434(11) 0.00258(8) 0.00361(8) 0.00722(9) S2 0.01633(12) 0.01717(12) 0.01339(11) 0.00281(9) 0.00316(8) 0.00759(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 C1 N1 1.4792(13) . ? C1 C4 1.5264(15) . ? C1 C2 1.5339(15) . ? C1 C3 1.5344(15) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N2 1.4989(13) . ? C5 C8 1.5275(15) . ? C5 C7 1.5321(15) . ? C5 C6 1.5374(15) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 P1 1.8403(11) . ? C9 S1 1.8406(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 P1 1.8287(12) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 P1 1.8417(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N3 1.4936(13) . ? C12 C15 1.5235(15) . ? C12 C14 1.5306(16) . ? C12 C13 1.5322(16) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N4 1.4884(13) . ? C16 C17 1.5244(16) . ? C16 C18 1.5334(15) . ? C16 C19 1.5362(16) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 S2 1.8329(11) . ? C20 P2 1.8399(11) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 P2 1.8367(12) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 P2 1.8292(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? Li1 N1 1.939(2) . ? Li1 N3 2.065(2) . ? Li1 N2 2.398(2) . ? Li1 P2 2.6470(19) . ? Li2 N4 2.032(2) . ? Li2 N2 2.059(2) . ? Li2 N3 2.177(2) . ? Li2 P1 2.6425(19) . ? N1 S1 1.6144(9) . ? N2 S1 1.6351(9) . ? N3 S2 1.6290(9) . ? N4 S2 1.6163(9) . ? 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 C1 C4 104.83(8) . . ? N1 C1 C2 112.64(9) . . ? C4 C1 C2 108.80(9) . . ? N1 C1 C3 112.53(9) . . ? C4 C1 C3 108.95(9) . . ? C2 C1 C3 108.91(9) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C8 105.41(8) . . ? N2 C5 C7 111.89(9) . . ? C8 C5 C7 109.63(9) . . ? N2 C5 C6 112.98(9) . . ? C8 C5 C6 108.27(9) . . ? C7 C5 C6 108.53(9) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P1 C9 S1 116.24(6) . . ? P1 C9 H9A 108.2 . . ? S1 C9 H9A 108.2 . . ? P1 C9 H9B 108.2 . . ? S1 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? P1 C10 H10A 109.5 . . ? P1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C15 106.10(8) . . ? N3 C12 C14 114.11(9) . . ? C15 C12 C14 108.29(10) . . ? N3 C12 C13 110.65(9) . . ? C15 C12 C13 108.66(10) . . ? C14 C12 C13 108.85(11) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 105.50(9) . . ? N4 C16 C18 112.22(9) . . ? C17 C16 C18 108.58(9) . . ? N4 C16 C19 112.14(9) . . ? C17 C16 C19 108.91(10) . . ? C18 C16 C19 109.32(10) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? S2 C20 P2 115.07(5) . . ? S2 C20 H20A 108.5 . . ? P2 C20 H20A 108.5 . . ? S2 C20 H20B 108.5 . . ? P2 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 Li1 N3 126.03(10) . . ? N1 Li1 N2 71.93(7) . . ? N3 Li1 N2 103.61(9) . . ? N1 Li1 Li2 106.62(9) . . ? N3 Li1 Li2 55.14(7) . . ? N2 Li1 Li2 49.11(6) . . ? N1 Li1 P2 144.95(10) . . ? N3 Li1 P2 86.58(7) . . ? N2 Li1 P2 116.60(8) . . ? Li2 Li1 P2 102.86(8) . . ? N4 Li2 N2 126.46(10) . . ? N4 Li2 N3 73.69(7) . . ? N2 Li2 N3 112.03(9) . . ? N4 Li2 Li1 96.76(9) . . ? N2 Li2 Li1 61.67(7) . . ? N3 Li2 Li1 51.10(6) . . ? N4 Li2 P1 152.46(10) . . ? N2 Li2 P1 76.79(6) . . ? N3 Li2 P1 114.07(8) . . ? Li1 Li2 P1 108.57(8) . . ? C1 N1 S1 116.43(7) . . ? C1 N1 Li1 140.75(9) . . ? S1 N1 Li1 100.05(7) . . ? C5 N2 S1 112.01(7) . . ? C5 N2 Li2 125.16(8) . . ? S1 N2 Li2 122.73(7) . . ? C5 N2 Li1 117.48(8) . . ? S1 N2 Li1 82.93(6) . . ? Li2 N2 Li1 69.23(7) . . ? C12 N3 S2 114.51(7) . . ? C12 N3 Li1 119.72(8) . . ? S2 N3 Li1 118.44(7) . . ? C12 N3 Li2 134.31(8) . . ? S2 N3 Li2 88.69(6) . . ? Li1 N3 Li2 73.75(8) . . ? C16 N4 S2 113.46(7) . . ? C16 N4 Li2 128.89(9) . . ? S2 N4 Li2 94.28(7) . . ? C10 P1 C9 101.61(6) . . ? C10 P1 C11 99.35(6) . . ? C9 P1 C11 97.24(5) . . ? C10 P1 Li2 112.21(6) . . ? C9 P1 Li2 96.36(5) . . ? C11 P1 Li2 142.14(6) . . ? C22 P2 C21 100.10(6) . . ? C22 P2 C20 102.06(6) . . ? C21 P2 C20 99.06(5) . . ? C22 P2 Li1 124.51(6) . . ? C21 P2 Li1 128.13(6) . . ? C20 P2 Li1 96.18(5) . . ? N1 S1 N2 104.74(5) . . ? N1 S1 C9 106.38(5) . . ? N2 S1 C9 100.60(5) . . ? N4 S2 N3 102.24(5) . . ? N4 S2 C20 105.39(5) . . ? N3 S2 C20 104.04(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Li1 Li2 N4 174.63(9) . . . . ? N3 Li1 Li2 N4 -62.67(7) . . . . ? N2 Li1 Li2 N4 128.02(10) . . . . ? P2 Li1 Li2 N4 13.82(10) . . . . ? S1 Li1 Li2 N4 156.44(8) . . . . ? N1 Li1 Li2 N2 46.61(9) . . . . ? N3 Li1 Li2 N2 169.30(9) . . . . ? P2 Li1 Li2 N2 -114.20(8) . . . . ? S1 Li1 Li2 N2 28.42(4) . . . . ? N1 Li1 Li2 N3 -122.69(11) . . . . ? N2 Li1 Li2 N3 -169.30(9) . . . . ? P2 Li1 Li2 N3 76.49(7) . . . . ? S1 Li1 Li2 N3 -140.88(8) . . . . ? N1 Li1 Li2 P1 -16.32(12) . . . . ? N3 Li1 Li2 P1 106.37(8) . . . . ? N2 Li1 Li2 P1 -62.94(7) . . . . ? P2 Li1 Li2 P1 -177.14(6) . . . . ? S1 Li1 Li2 P1 -34.51(7) . . . . ? N1 Li1 Li2 S2 -155.55(9) . . . . ? N3 Li1 Li2 S2 -32.86(4) . . . . ? N2 Li1 Li2 S2 157.84(8) . . . . ? P2 Li1 Li2 S2 43.63(6) . . . . ? S1 Li1 Li2 S2 -173.74(6) . . . . ? C4 C1 N1 S1 -175.76(7) . . . . ? C2 C1 N1 S1 -57.62(11) . . . . ? C3 C1 N1 S1 65.97(11) . . . . ? C4 C1 N1 Li1 -19.37(17) . . . . ? C2 C1 N1 Li1 98.77(15) . . . . ? C3 C1 N1 Li1 -137.64(13) . . . . ? N3 Li1 N1 C1 111.38(15) . . . . ? N2 Li1 N1 C1 -154.68(13) . . . . ? Li2 Li1 N1 C1 170.02(11) . . . . ? P2 Li1 N1 C1 -43.9(3) . . . . ? S1 Li1 N1 C1 -158.64(16) . . . . ? N3 Li1 N1 S1 -89.98(12) . . . . ? N2 Li1 N1 S1 3.96(5) . . . . ? Li2 Li1 N1 S1 -31.34(10) . . . . ? P2 Li1 N1 S1 114.75(16) . . . . ? C8 C5 N2 S1 -173.12(7) . . . . ? C7 C5 N2 S1 67.78(10) . . . . ? C6 C5 N2 S1 -55.07(11) . . . . ? C8 C5 N2 Li2 10.44(13) . . . . ? C7 C5 N2 Li2 -108.66(11) . . . . ? C6 C5 N2 Li2 128.49(11) . . . . ? C8 C5 N2 Li1 93.40(10) . . . . ? C7 C5 N2 Li1 -25.70(12) . . . . ? C6 C5 N2 Li1 -148.55(9) . . . . ? N4 Li2 N2 C5 33.08(17) . . . . ? N3 Li2 N2 C5 118.63(10) . . . . ? Li1 Li2 N2 C5 109.66(10) . . . . ? P1 Li2 N2 C5 -130.46(9) . . . . ? S2 Li2 N2 C5 80.61(14) . . . . ? N4 Li2 N2 S1 -142.99(10) . . . . ? N3 Li2 N2 S1 -57.44(12) . . . . ? Li1 Li2 N2 S1 -66.41(8) . . . . ? P1 Li2 N2 S1 53.47(8) . . . . ? S2 Li2 N2 S1 -95.46(12) . . . . ? N4 Li2 N2 Li1 -76.58(12) . . . . ? N3 Li2 N2 Li1 8.97(8) . . . . ? P1 Li2 N2 Li1 119.88(7) . . . . ? S2 Li2 N2 Li1 -29.05(10) . . . . ? N1 Li1 N2 C5 107.29(8) . . . . ? N3 Li1 N2 C5 -128.82(9) . . . . ? Li2 Li1 N2 C5 -119.80(10) . . . . ? P2 Li1 N2 C5 -35.81(11) . . . . ? S1 Li1 N2 C5 111.17(8) . . . . ? N1 Li1 N2 S1 -3.88(5) . . . . ? N3 Li1 N2 S1 120.01(8) . . . . ? Li2 Li1 N2 S1 129.03(7) . . . . ? P2 Li1 N2 S1 -146.98(8) . . . . ? N1 Li1 N2 Li2 -132.90(9) . . . . ? N3 Li1 N2 Li2 -9.02(8) . . . . ? P2 Li1 N2 Li2 84.00(9) . . . . ? S1 Li1 N2 Li2 -129.03(7) . . . . ? C15 C12 N3 S2 -155.58(8) . . . . ? C14 C12 N3 S2 -36.43(12) . . . . ? C13 C12 N3 S2 86.73(10) . . . . ? C15 C12 N3 Li1 54.78(12) . . . . ? C14 C12 N3 Li1 173.92(10) . . . . ? C13 C12 N3 Li1 -62.91(12) . . . . ? C15 C12 N3 Li2 -41.37(15) . . . . ? C14 C12 N3 Li2 77.77(14) . . . . ? C13 C12 N3 Li2 -159.06(11) . . . . ? N1 Li1 N3 C12 -46.51(16) . . . . ? N2 Li1 N3 C12 -123.88(9) . . . . ? Li2 Li1 N3 C12 -132.18(10) . . . . ? P2 Li1 N3 C12 119.56(8) . . . . ? S1 Li1 N3 C12 -88.02(11) . . . . ? N1 Li1 N3 S2 165.02(10) . . . . ? N2 Li1 N3 S2 87.64(8) . . . . ? Li2 Li1 N3 S2 79.34(8) . . . . ? P2 Li1 N3 S2 -28.91(8) . . . . ? S1 Li1 N3 S2 123.51(8) . . . . ? N1 Li1 N3 Li2 85.67(13) . . . . ? N2 Li1 N3 Li2 8.30(7) . . . . ? P2 Li1 N3 Li2 -108.26(7) . . . . ? S1 Li1 N3 Li2 44.16(9) . . . . ? N4 Li2 N3 C12 -130.89(10) . . . . ? N2 Li2 N3 C12 105.77(12) . . . . ? Li1 Li2 N3 C12 115.92(12) . . . . ? P1 Li2 N3 C12 20.89(15) . . . . ? S2 Li2 N3 C12 -123.89(12) . . . . ? N4 Li2 N3 S2 -7.00(6) . . . . ? N2 Li2 N3 S2 -130.34(9) . . . . ? Li1 Li2 N3 S2 -120.19(7) . . . . ? P1 Li2 N3 S2 144.78(7) . . . . ? N4 Li2 N3 Li1 113.19(8) . . . . ? N2 Li2 N3 Li1 -10.15(9) . . . . ? P1 Li2 N3 Li1 -95.03(9) . . . . ? S2 Li2 N3 Li1 120.19(7) . . . . ? C17 C16 N4 S2 -178.61(8) . . . . ? C18 C16 N4 S2 -60.54(11) . . . . ? C19 C16 N4 S2 62.97(11) . . . . ? C17 C16 N4 Li2 64.36(14) . . . . ? C18 C16 N4 Li2 -177.57(10) . . . . ? C19 C16 N4 Li2 -54.06(14) . . . . ? N2 Li2 N4 C16 -122.31(12) . . . . ? N3 Li2 N4 C16 132.04(10) . . . . ? Li1 Li2 N4 C16 178.13(9) . . . . ? P1 Li2 N4 C16 21.1(3) . . . . ? S2 Li2 N4 C16 124.97(12) . . . . ? N2 Li2 N4 S2 112.73(11) . . . . ? N3 Li2 N4 S2 7.08(6) . . . . ? Li1 Li2 N4 S2 53.17(8) . . . . ? P1 Li2 N4 S2 -103.9(2) . . . . ? S1 C9 P1 C10 -87.65(7) . . . . ? S1 C9 P1 C11 171.21(7) . . . . ? S1 C9 P1 Li2 26.63(8) . . . . ? N4 Li2 P1 C10 -82.4(2) . . . . ? N2 Li2 P1 C10 68.10(7) . . . . ? N3 Li2 P1 C10 176.59(8) . . . . ? Li1 Li2 P1 C10 121.72(8) . . . . ? S2 Li2 P1 C10 -149.76(11) . . . . ? N4 Li2 P1 C9 172.3(2) . . . . ? N2 Li2 P1 C9 -37.22(7) . . . . ? N3 Li2 P1 C9 71.27(9) . . . . ? Li1 Li2 P1 C9 16.40(9) . . . . ? S2 Li2 P1 C9 104.92(12) . . . . ? N4 Li2 P1 C11 61.8(2) . . . . ? N2 Li2 P1 C11 -147.71(8) . . . . ? N3 Li2 P1 C11 -39.21(14) . . . . ? Li1 Li2 P1 C11 -94.08(11) . . . . ? S2 Li2 P1 C11 -5.56(18) . . . . ? S2 C20 P2 C22 -103.27(7) . . . . ? S2 C20 P2 C21 154.28(7) . . . . ? S2 C20 P2 Li1 24.02(7) . . . . ? N1 Li1 P2 C22 -90.23(18) . . . . ? N3 Li1 P2 C22 109.58(8) . . . . ? N2 Li1 P2 C22 6.07(12) . . . . ? Li2 Li1 P2 C22 56.52(10) . . . . ? S1 Li1 P2 C22 -27.07(16) . . . . ? N1 Li1 P2 C21 53.9(2) . . . . ? N3 Li1 P2 C21 -106.30(8) . . . . ? N2 Li1 P2 C21 150.19(7) . . . . ? Li2 Li1 P2 C21 -159.36(7) . . . . ? S1 Li1 P2 C21 117.05(13) . . . . ? N1 Li1 P2 C20 160.53(17) . . . . ? N3 Li1 P2 C20 0.35(7) . . . . ? N2 Li1 P2 C20 -103.17(8) . . . . ? Li2 Li1 P2 C20 -52.72(8) . . . . ? S1 Li1 P2 C20 -136.30(13) . . . . ? C1 N1 S1 N2 159.38(7) . . . . ? Li1 N1 S1 N2 -5.71(8) . . . . ? C1 N1 S1 C9 -94.62(8) . . . . ? Li1 N1 S1 C9 100.29(8) . . . . ? C1 N1 S1 Li1 165.09(11) . . . . ? C5 N2 S1 N1 -112.26(7) . . . . ? Li2 N2 S1 N1 64.28(9) . . . . ? Li1 N2 S1 N1 4.58(6) . . . . ? C5 N2 S1 C9 137.50(7) . . . . ? Li2 N2 S1 C9 -45.96(9) . . . . ? Li1 N2 S1 C9 -105.66(6) . . . . ? C5 N2 S1 Li1 -116.84(9) . . . . ? Li2 N2 S1 Li1 59.70(9) . . . . ? P1 C9 S1 N1 -107.63(7) . . . . ? P1 C9 S1 N2 1.33(7) . . . . ? P1 C9 S1 Li1 -61.05(8) . . . . ? N3 Li1 S1 N1 112.96(12) . . . . ? N2 Li1 S1 N1 -173.66(9) . . . . ? Li2 Li1 S1 N1 149.08(10) . . . . ? P2 Li1 S1 N1 -118.32(16) . . . . ? N1 Li1 S1 N2 173.66(9) . . . . ? N3 Li1 S1 N2 -73.38(9) . . . . ? Li2 Li1 S1 N2 -37.26(6) . . . . ? P2 Li1 S1 N2 55.34(12) . . . . ? N1 Li1 S1 C9 -94.52(7) . . . . ? N3 Li1 S1 C9 18.44(11) . . . . ? N2 Li1 S1 C9 91.82(6) . . . . ? Li2 Li1 S1 C9 54.56(7) . . . . ? P2 Li1 S1 C9 147.17(12) . . . . ? C16 N4 S2 N3 -145.25(7) . . . . ? Li2 N4 S2 N3 -9.30(7) . . . . ? C16 N4 S2 C20 106.25(8) . . . . ? Li2 N4 S2 C20 -117.80(7) . . . . ? C16 N4 S2 Li2 -135.95(11) . . . . ? C12 N3 S2 N4 147.90(7) . . . . ? Li1 N3 S2 N4 -62.04(9) . . . . ? Li2 N3 S2 N4 8.66(7) . . . . ? C12 N3 S2 C20 -102.58(8) . . . . ? Li1 N3 S2 C20 47.48(9) . . . . ? Li2 N3 S2 C20 118.18(7) . . . . ? C12 N3 S2 Li2 139.25(10) . . . . ? Li1 N3 S2 Li2 -70.69(9) . . . . ? P2 C20 S2 N4 61.90(7) . . . . ? P2 C20 S2 N3 -45.29(7) . . . . ? P2 C20 S2 Li2 10.94(9) . . . . ? N2 Li2 S2 N4 -98.25(13) . . . . ? N3 Li2 S2 N4 -168.74(9) . . . . ? Li1 Li2 S2 N4 -124.54(9) . . . . ? P1 Li2 S2 N4 134.60(15) . . . . ? N4 Li2 S2 N3 168.74(9) . . . . ? N2 Li2 S2 N3 70.49(11) . . . . ? Li1 Li2 S2 N3 44.20(6) . . . . ? P1 Li2 S2 N3 -56.65(11) . . . . ? N4 Li2 S2 C20 83.60(8) . . . . ? N2 Li2 S2 C20 -14.65(14) . . . . ? N3 Li2 S2 C20 -85.15(7) . . . . ? Li1 Li2 S2 C20 -40.94(8) . . . . ? P1 Li2 S2 C20 -141.80(11) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.433 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.042 #===END data_p-1 _database_code_depnum_ccdc_archive 'CCDC 779987' #TrackingRef '- all_comm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point '123\%C (decomp.)' _chemical_formula_moiety ? _chemical_formula_sum 'C42 H60 Li2 N4 P2 S2' _chemical_formula_weight 760.88 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' 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 9.6236(11) _cell_length_b 10.1512(12) _cell_length_c 11.3253(13) _cell_angle_alpha 73.936(2) _cell_angle_beta 84.728(2) _cell_angle_gamma 88.960(2) _cell_volume 1058.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6011 _cell_measurement_theta_min 2.707 _cell_measurement_theta_max 31.5625 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 0.235 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8676 _exptl_absorpt_correction_T_max 0.9916 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS-Mo rotating anode' _diffrn_radiation_monochromator 'INCOATEC Helios mirror optics' _diffrn_measurement_device_type 'Bruker TXS-Mo rotating anode' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25994 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5259 _reflns_number_gt 4031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.2-0' _computing_cell_refinement 'SAINT v7.46A' _computing_data_reduction 'SAINT v7.46A' _computing_structure_solution 'SHELXS in SHELXTL v2008/2 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL in SHELXTL v2008/2 (Sheldrick, 2008)' _computing_molecular_graphics 'XSHELL v4.01' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.3215P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5259 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.68258(18) 0.66971(17) 0.26483(15) 0.0203(3) Uani 1 1 d . . . C2 C 0.61020(19) 0.74617(18) 0.33525(15) 0.0246(4) Uani 1 1 d . . . H2 H 0.5223 0.7145 0.3781 0.029 Uiso 1 1 calc R . . C3 C 0.6658(2) 0.86806(19) 0.34315(17) 0.0301(4) Uani 1 1 d . . . H3 H 0.6149 0.9197 0.3906 0.036 Uiso 1 1 calc R . . C4 C 0.7941(2) 0.9156(2) 0.28305(17) 0.0317(4) Uani 1 1 d . . . H4 H 0.8320 0.9985 0.2903 0.038 Uiso 1 1 calc R . . C5 C 0.8671(2) 0.8413(2) 0.21199(18) 0.0317(4) Uani 1 1 d . . . H5 H 0.9554 0.8733 0.1701 0.038 Uiso 1 1 calc R . . C6 C 0.81118(19) 0.72032(18) 0.20210(16) 0.0251(4) Uani 1 1 d . . . H6 H 0.8610 0.6709 0.1519 0.030 Uiso 1 1 calc R . . C7 C 0.70730(17) 0.38572(17) 0.37890(15) 0.0196(3) Uani 1 1 d . . . C8 C 0.79558(17) 0.42678(18) 0.45356(15) 0.0207(3) Uani 1 1 d . . . H8 H 0.8130 0.5216 0.4414 0.025 Uiso 1 1 calc R . . C9 C 0.85849(19) 0.33022(19) 0.54574(15) 0.0245(4) Uani 1 1 d . . . H9 H 0.9191 0.3596 0.5952 0.029 Uiso 1 1 calc R . . C10 C 0.8330(2) 0.1921(2) 0.56531(16) 0.0281(4) Uani 1 1 d . . . H10 H 0.8752 0.1263 0.6285 0.034 Uiso 1 1 calc R . . C11 C 0.7450(2) 0.15021(19) 0.49174(17) 0.0300(4) Uani 1 1 d . . . H11 H 0.7270 0.0553 0.5050 0.036 Uiso 1 1 calc R . . C12 C 0.6836(2) 0.24528(19) 0.39957(16) 0.0266(4) Uani 1 1 d . . . H12 H 0.6244 0.2149 0.3495 0.032 Uiso 1 1 calc R . . C13 C 0.44325(17) 0.48376(19) 0.31327(15) 0.0223(3) Uani 1 1 d . . . H13A H 0.4242 0.5455 0.3668 0.027 Uiso 1 1 calc R . . H13B H 0.4277 0.3884 0.3654 0.027 Uiso 1 1 calc R . . C14 C 0.17241(18) 0.29936(17) 0.22240(15) 0.0203(3) Uani 1 1 d . . . C15 C 0.1819(2) 0.2451(2) 0.36176(16) 0.0282(4) Uani 1 1 d . . . H15A H 0.2698 0.1960 0.3773 0.042 Uiso 1 1 calc R . . H15B H 0.1034 0.1826 0.3987 0.042 Uiso 1 1 calc R . . H15C H 0.1784 0.3221 0.3984 0.042 Uiso 1 1 calc R . . C16 C 0.1683(2) 0.1769(2) 0.16982(18) 0.0309(4) Uani 1 1 d . . . H16A H 0.1642 0.2093 0.0803 0.046 Uiso 1 1 calc R . . H16B H 0.0855 0.1206 0.2073 0.046 Uiso 1 1 calc R . . H16C H 0.2524 0.1219 0.1880 0.046 Uiso 1 1 calc R . . C17 C 0.03773(18) 0.3813(2) 0.19867(18) 0.0288(4) Uani 1 1 d . . . H17A H 0.0404 0.4609 0.2316 0.043 Uiso 1 1 calc R . . H17B H -0.0425 0.3230 0.2395 0.043 Uiso 1 1 calc R . . H17C H 0.0291 0.4126 0.1097 0.043 Uiso 1 1 calc R . . C18 C 0.34919(17) 0.75286(16) 0.02427(14) 0.0182(3) Uani 1 1 d . . . C19 C 0.45500(19) 0.83451(18) -0.07594(16) 0.0257(4) Uani 1 1 d . . . H19A H 0.5395 0.8493 -0.0390 0.039 Uiso 1 1 calc R . . H19B H 0.4151 0.9233 -0.1164 0.039 Uiso 1 1 calc R . . H19C H 0.4786 0.7836 -0.1370 0.039 Uiso 1 1 calc R . . C20 C 0.3192(2) 0.83168(19) 0.12108(17) 0.0272(4) Uani 1 1 d . . . H20A H 0.2506 0.7807 0.1863 0.041 Uiso 1 1 calc R . . H20B H 0.2820 0.9222 0.0820 0.041 Uiso 1 1 calc R . . H20C H 0.4057 0.8426 0.1569 0.041 Uiso 1 1 calc R . . C21 C 0.21298(18) 0.73737(19) -0.03110(17) 0.0259(4) Uani 1 1 d . . . H21A H 0.2317 0.6905 -0.0957 0.039 Uiso 1 1 calc R . . H21B H 0.1744 0.8282 -0.0667 0.039 Uiso 1 1 calc R . . H21C H 0.1457 0.6835 0.0337 0.039 Uiso 1 1 calc R . . Li1 Li 0.3935(3) 0.4349(3) -0.0085(3) 0.0217(6) Uani 1 1 d . . . N1 N 0.29773(14) 0.38053(14) 0.15817(12) 0.0180(3) Uani 1 1 d . . . N2 N 0.41501(14) 0.61626(14) 0.07609(12) 0.0178(3) Uani 1 1 d . . . P1 P 0.62715(4) 0.50419(4) 0.24997(4) 0.01814(11) Uani 1 1 d . . . S1 S 0.31921(4) 0.52137(4) 0.19400(3) 0.01635(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0229(8) 0.0223(8) 0.0157(7) -0.0040(6) -0.0059(6) 0.0012(6) C2 0.0290(9) 0.0277(9) 0.0181(8) -0.0076(7) -0.0038(7) 0.0003(7) C3 0.0443(11) 0.0258(9) 0.0238(9) -0.0102(7) -0.0106(8) 0.0032(8) C4 0.0449(12) 0.0244(9) 0.0260(9) -0.0037(7) -0.0139(8) -0.0066(8) C5 0.0326(10) 0.0285(10) 0.0305(10) -0.0005(8) -0.0073(8) -0.0071(8) C6 0.0268(9) 0.0252(9) 0.0215(8) -0.0034(7) -0.0018(7) -0.0009(7) C7 0.0211(8) 0.0226(8) 0.0148(7) -0.0057(6) 0.0007(6) 0.0009(6) C8 0.0219(8) 0.0254(9) 0.0158(7) -0.0076(6) -0.0007(6) 0.0005(7) C9 0.0262(9) 0.0342(10) 0.0143(8) -0.0084(7) -0.0036(6) 0.0034(7) C10 0.0368(10) 0.0310(10) 0.0154(8) -0.0048(7) -0.0030(7) 0.0090(8) C11 0.0453(12) 0.0223(9) 0.0215(9) -0.0049(7) -0.0027(8) 0.0029(8) C12 0.0363(10) 0.0263(9) 0.0188(8) -0.0083(7) -0.0047(7) -0.0023(8) C13 0.0215(8) 0.0309(9) 0.0150(7) -0.0075(7) -0.0003(6) -0.0049(7) C14 0.0219(8) 0.0222(8) 0.0161(7) -0.0049(6) 0.0013(6) -0.0044(6) C15 0.0315(10) 0.0315(10) 0.0186(8) -0.0025(7) 0.0014(7) -0.0085(8) C16 0.0355(11) 0.0292(10) 0.0299(10) -0.0141(8) 0.0085(8) -0.0138(8) C17 0.0208(9) 0.0336(10) 0.0312(10) -0.0077(8) -0.0014(7) -0.0046(7) C18 0.0213(8) 0.0172(8) 0.0167(7) -0.0058(6) -0.0019(6) 0.0010(6) C19 0.0280(9) 0.0210(9) 0.0242(9) -0.0008(7) 0.0011(7) 0.0000(7) C20 0.0390(11) 0.0222(9) 0.0227(9) -0.0100(7) -0.0028(7) 0.0031(7) C21 0.0253(9) 0.0268(9) 0.0250(9) -0.0051(7) -0.0061(7) 0.0016(7) Li1 0.0220(14) 0.0287(16) 0.0160(13) -0.0089(11) 0.0001(11) -0.0022(12) N1 0.0207(7) 0.0190(7) 0.0151(6) -0.0067(5) 0.0012(5) -0.0042(5) N2 0.0210(7) 0.0176(7) 0.0143(6) -0.0039(5) -0.0004(5) -0.0004(5) P1 0.0205(2) 0.0223(2) 0.01240(19) -0.00593(16) -0.00198(15) -0.00144(16) S1 0.01798(19) 0.0188(2) 0.01281(18) -0.00554(14) -0.00049(14) -0.00100(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.394(2) . ? C1 C6 1.400(2) . ? C1 P1 1.8280(18) . ? C2 C3 1.385(3) . ? C2 H2 0.9500 . ? C3 C4 1.381(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.396(2) . ? C7 C12 1.399(2) . ? C7 P1 1.8371(17) . ? C8 C9 1.395(2) . ? C8 H8 0.9500 . ? C9 C10 1.380(3) . ? C9 H9 0.9500 . ? C10 C11 1.389(3) . ? C10 H10 0.9500 . ? C11 C12 1.381(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 P1 1.8404(17) . ? C13 S1 1.8412(17) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N1 1.485(2) . ? C14 C16 1.523(2) . ? C14 C17 1.532(3) . ? C14 C15 1.532(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N2 1.502(2) . ? C18 C19 1.520(2) . ? C18 C20 1.531(2) . ? C18 C21 1.533(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? Li1 N1 1.959(3) . ? Li1 N2 2.318(3) . ? N1 S1 1.6120(14) . ? N2 S1 1.6295(14) . ? P1 Li1 2.657(3) 2_665 ? 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 C2 C1 C6 118.18(16) . . ? C2 C1 P1 125.73(14) . . ? C6 C1 P1 116.06(13) . . ? C3 C2 C1 120.37(17) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 121.00(18) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.40(18) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 119.94(18) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 121.08(18) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C12 118.09(16) . . ? C8 C7 P1 124.06(13) . . ? C12 C7 P1 117.77(13) . . ? C9 C8 C7 120.81(16) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 120.24(16) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.41(16) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 120.59(18) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C7 120.86(17) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? P1 C13 S1 113.51(9) . . ? P1 C13 H13A 108.9 . . ? S1 C13 H13A 108.9 . . ? P1 C13 H13B 108.9 . . ? S1 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N1 C14 C16 105.81(13) . . ? N1 C14 C17 112.08(14) . . ? C16 C14 C17 109.21(15) . . ? N1 C14 C15 112.30(14) . . ? C16 C14 C15 108.08(15) . . ? C17 C14 C15 109.21(15) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 C19 105.96(13) . . ? N2 C18 C20 112.37(13) . . ? C19 C18 C20 108.33(14) . . ? N2 C18 C21 111.44(13) . . ? C19 C18 C21 109.89(14) . . ? C20 C18 C21 108.77(14) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 Li1 N2 131.18(16) . 2_665 ? N1 Li1 N2 72.88(10) . . ? N2 Li1 N2 110.12(13) 2_665 . ? N1 Li1 Li1 105.33(17) . 2_665 ? N2 Li1 Li1 60.20(12) 2_665 2_665 ? N2 Li1 Li1 49.92(11) . 2_665 ? N1 Li1 P1 147.48(14) . 2_665 ? N2 Li1 P1 76.78(9) 2_665 2_665 ? N2 Li1 P1 117.31(12) . 2_665 ? Li1 Li1 P1 103.75(15) 2_665 2_665 ? N1 Li1 S1 36.12(6) . . ? N2 Li1 S1 130.19(13) 2_665 . ? N2 Li1 S1 36.82(5) . . ? Li1 Li1 S1 77.64(13) 2_665 . ? P1 Li1 S1 142.83(12) 2_665 . ? C14 N1 S1 114.75(11) . . ? C14 N1 Li1 137.74(13) . . ? S1 N1 Li1 98.12(11) . . ? C18 N2 S1 111.75(10) . . ? C18 N2 Li1 122.53(13) . 2_665 ? S1 N2 Li1 125.65(11) . 2_665 ? C18 N2 Li1 122.01(12) . . ? S1 N2 Li1 84.68(9) . . ? Li1 N2 Li1 69.88(13) 2_665 . ? C1 P1 C7 101.08(8) . . ? C1 P1 C13 105.45(8) . . ? C7 P1 C13 99.23(8) . . ? C1 P1 Li1 100.78(8) . 2_665 ? C7 P1 Li1 143.77(8) . 2_665 ? C13 P1 Li1 102.33(8) . 2_665 ? N1 S1 N2 104.15(7) . . ? N1 S1 C13 106.45(8) . . ? N2 S1 C13 101.29(7) . . ? N1 S1 Li1 45.76(8) . . ? N2 S1 Li1 58.49(8) . . ? C13 S1 Li1 115.95(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.6(2) . . . . ? P1 C1 C2 C3 177.40(13) . . . . ? C1 C2 C3 C4 -0.8(3) . . . . ? C2 C3 C4 C5 1.2(3) . . . . ? C3 C4 C5 C6 -0.2(3) . . . . ? C4 C5 C6 C1 -1.2(3) . . . . ? C2 C1 C6 C5 1.6(2) . . . . ? P1 C1 C6 C5 -176.59(14) . . . . ? C12 C7 C8 C9 0.2(2) . . . . ? P1 C7 C8 C9 -176.58(13) . . . . ? C7 C8 C9 C10 -0.7(3) . . . . ? C8 C9 C10 C11 0.5(3) . . . . ? C9 C10 C11 C12 0.1(3) . . . . ? C10 C11 C12 C7 -0.6(3) . . . . ? C8 C7 C12 C11 0.4(3) . . . . ? P1 C7 C12 C11 177.43(14) . . . . ? C16 C14 N1 S1 176.82(12) . . . . ? C17 C14 N1 S1 57.88(16) . . . . ? C15 C14 N1 S1 -65.49(17) . . . . ? C16 C14 N1 Li1 39.2(2) . . . . ? C17 C14 N1 Li1 -79.7(2) . . . . ? C15 C14 N1 Li1 156.91(19) . . . . ? N2 Li1 N1 C14 -113.4(2) 2_665 . . . ? N2 Li1 N1 C14 144.56(18) . . . . ? Li1 Li1 N1 C14 -176.98(17) 2_665 . . . ? P1 Li1 N1 C14 30.4(4) 2_665 . . . ? S1 Li1 N1 C14 141.8(2) . . . . ? N2 Li1 N1 S1 104.8(2) 2_665 . . . ? N2 Li1 N1 S1 2.78(8) . . . . ? Li1 Li1 N1 S1 41.23(19) 2_665 . . . ? P1 Li1 N1 S1 -111.4(3) 2_665 . . . ? C19 C18 N2 S1 174.77(11) . . . . ? C20 C18 N2 S1 56.65(16) . . . . ? C21 C18 N2 S1 -65.72(15) . . . . ? C19 C18 N2 Li1 -2.37(19) . . . 2_665 ? C20 C18 N2 Li1 -120.50(16) . . . 2_665 ? C21 C18 N2 Li1 117.13(16) . . . 2_665 ? C19 C18 N2 Li1 -87.65(16) . . . . ? C20 C18 N2 Li1 154.22(14) . . . . ? C21 C18 N2 Li1 31.85(19) . . . . ? N1 Li1 N2 C18 -115.11(13) . . . . ? N2 Li1 N2 C18 116.51(16) 2_665 . . . ? Li1 Li1 N2 C18 116.51(16) 2_665 . . . ? P1 Li1 N2 C18 31.39(19) 2_665 . . . ? S1 Li1 N2 C18 -112.38(14) . . . . ? N1 Li1 N2 S1 -2.73(8) . . . . ? N2 Li1 N2 S1 -131.11(13) 2_665 . . . ? Li1 Li1 N2 S1 -131.11(13) 2_665 . . . ? P1 Li1 N2 S1 143.77(12) 2_665 . . . ? N1 Li1 N2 Li1 128.38(17) . . . 2_665 ? N2 Li1 N2 Li1 0.0 2_665 . . 2_665 ? P1 Li1 N2 Li1 -85.13(15) 2_665 . . 2_665 ? S1 Li1 N2 Li1 131.11(13) . . . 2_665 ? C2 C1 P1 C7 -89.47(15) . . . . ? C6 C1 P1 C7 88.58(13) . . . . ? C2 C1 P1 C13 13.45(16) . . . . ? C6 C1 P1 C13 -168.50(13) . . . . ? C2 C1 P1 Li1 119.60(15) . . . 2_665 ? C6 C1 P1 Li1 -62.35(14) . . . 2_665 ? C8 C7 P1 C1 -5.01(16) . . . . ? C12 C7 P1 C1 178.20(14) . . . . ? C8 C7 P1 C13 -112.88(15) . . . . ? C12 C7 P1 C13 70.33(15) . . . . ? C8 C7 P1 Li1 121.12(17) . . . 2_665 ? C12 C7 P1 Li1 -55.7(2) . . . 2_665 ? S1 C13 P1 C1 101.49(10) . . . . ? S1 C13 P1 C7 -154.22(10) . . . . ? S1 C13 P1 Li1 -3.52(12) . . . 2_665 ? C14 N1 S1 N2 -156.63(11) . . . . ? Li1 N1 S1 N2 -3.90(12) . . . . ? C14 N1 S1 C13 96.82(12) . . . . ? Li1 N1 S1 C13 -110.45(11) . . . . ? C14 N1 S1 Li1 -152.73(16) . . . . ? C18 N2 S1 N1 125.69(11) . . . . ? Li1 N2 S1 N1 -57.27(14) 2_665 . . . ? Li1 N2 S1 N1 3.27(10) . . . . ? C18 N2 S1 C13 -123.94(11) . . . . ? Li1 N2 S1 C13 53.10(14) 2_665 . . . ? Li1 N2 S1 C13 113.64(10) . . . . ? C18 N2 S1 Li1 122.42(13) . . . . ? Li1 N2 S1 Li1 -60.54(16) 2_665 . . . ? P1 C13 S1 N1 87.25(11) . . . . ? P1 C13 S1 N2 -21.34(11) . . . . ? P1 C13 S1 Li1 38.95(13) . . . . ? N2 Li1 S1 N1 -107.7(2) 2_665 . . . ? N2 Li1 S1 N1 -175.57(13) . . . . ? Li1 Li1 S1 N1 -139.40(19) 2_665 . . . ? P1 Li1 S1 N1 124.1(2) 2_665 . . . ? N1 Li1 S1 N2 175.57(13) . . . . ? N2 Li1 S1 N2 67.84(17) 2_665 . . . ? Li1 Li1 S1 N2 36.17(11) 2_665 . . . ? P1 Li1 S1 N2 -60.36(18) 2_665 . . . ? N1 Li1 S1 C13 88.03(12) . . . . ? N2 Li1 S1 C13 -19.7(2) 2_665 . . . ? N2 Li1 S1 C13 -87.54(10) . . . . ? Li1 Li1 S1 C13 -51.37(16) 2_665 . . . ? P1 Li1 S1 C13 -147.90(17) 2_665 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.391 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.055 #===END data_fdd2 _database_code_depnum_ccdc_archive 'CCDC 779988' #TrackingRef '- all_comm.cif' __audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H52 Mg N4 P2 S2' _chemical_formula_sum 'C22 H52 Mg N4 P2 S2' _chemical_formula_weight 523.05 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' Mg Mg 0.0486 0.0363 '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 orthorhombic _symmetry_space_group_name_H-M Fdd2 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 37.169(8) _cell_length_b 10.175(2) _cell_length_c 16.851(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6373(2) _cell_formula_units_Z 8 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 8090 _cell_measurement_theta_min 2.1915 _cell_measurement_theta_max 25.9835 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.83307 _exptl_absorpt_correction_T_max 0.98931 _exptl_absorpt_process_details SADABS-2008/2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS-Mo rotating anode' _diffrn_radiation_monochromator 'INCOATEC Helios mirror optics' _diffrn_measurement_device_type 'Bruker TXS-Mo rotating anode' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21122 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.40 _reflns_number_total 3270 _reflns_number_gt 3060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX v2009.11-0' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.68A' _computing_structure_solution 'SHELXS in SHELXTL v2008/4' _computing_structure_refinement 'SHELXL in SHELXTL v2008/4' _computing_molecular_graphics 'XSHELL v4.01' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+7.7268P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(12) _refine_ls_number_reflns 3270 _refine_ls_number_parameters 162 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.04436(6) 0.5778(3) 0.15105(17) 0.0548(6) Uani 0.397(8) 1 d PD A 1 C1 C 0.05529(9) 0.6541(4) 0.0802(2) 0.0713(10) Uani 0.397(8) 1 d PD A 1 C2 C 0.0221(5) 0.682(2) 0.0335(15) 0.103(5) Uani 0.397(8) 1 d PD A 1 H2A H 0.0171 0.6088 -0.0015 0.154 Uiso 0.397(8) 1 calc PR A 1 H2B H 0.0257 0.7612 0.0022 0.154 Uiso 0.397(8) 1 calc PR A 1 H2C H 0.0020 0.6949 0.0694 0.154 Uiso 0.397(8) 1 calc PR A 1 C3 C 0.0689(4) 0.7896(13) 0.1151(11) 0.136(5) Uani 0.397(8) 1 d PD A 1 H3A H 0.0494 0.8323 0.1433 0.203 Uiso 0.397(8) 1 calc PR A 1 H3B H 0.0769 0.8457 0.0721 0.203 Uiso 0.397(8) 1 calc PR A 1 H3C H 0.0887 0.7740 0.1513 0.203 Uiso 0.397(8) 1 calc PR A 1 C4 C 0.0870(4) 0.6052(17) 0.0330(8) 0.110(3) Uani 0.397(8) 1 d PD A 1 H4A H 0.1084 0.6064 0.0661 0.166 Uiso 0.397(8) 1 calc PR A 1 H4B H 0.0907 0.6617 -0.0127 0.166 Uiso 0.397(8) 1 calc PR A 1 H4C H 0.0824 0.5161 0.0152 0.166 Uiso 0.397(8) 1 calc PR A 1 N1' N 0.04436(6) 0.5778(3) 0.15105(17) 0.0548(6) Uani 0.603(8) 1 d PD A 2 C1' C 0.05529(9) 0.6541(4) 0.0802(2) 0.0713(10) Uani 0.603(8) 1 d PD A 2 C2' C 0.0226(3) 0.7331(13) 0.0564(10) 0.103(5) Uani 0.603(8) 1 d PD A 2 H2'1 H 0.0019 0.6752 0.0521 0.154 Uiso 0.603(8) 1 calc PR A 2 H2'2 H 0.0269 0.7750 0.0056 0.154 Uiso 0.603(8) 1 calc PR A 2 H2'3 H 0.0179 0.7998 0.0962 0.154 Uiso 0.603(8) 1 calc PR A 2 C3' C 0.0871(3) 0.7453(11) 0.0943(8) 0.136(5) Uani 0.603(8) 1 d PD A 2 H3'1 H 0.0801 0.8152 0.1301 0.203 Uiso 0.603(8) 1 calc PR A 2 H3'2 H 0.0948 0.7828 0.0441 0.203 Uiso 0.603(8) 1 calc PR A 2 H3'3 H 0.1068 0.6959 0.1175 0.203 Uiso 0.603(8) 1 calc PR A 2 C4' C 0.0632(3) 0.5511(10) 0.0142(5) 0.110(3) Uani 0.603(8) 1 d PD A 2 H4'1 H 0.0818 0.4915 0.0321 0.166 Uiso 0.603(8) 1 calc PR A 2 H4'2 H 0.0711 0.5959 -0.0335 0.166 Uiso 0.603(8) 1 calc PR A 2 H4'3 H 0.0414 0.5017 0.0029 0.166 Uiso 0.603(8) 1 calc PR A 2 C5 C 0.05905(9) 0.2408(3) 0.2373(3) 0.0701(10) Uani 1 1 d D . . C6 C 0.09105(13) 0.2313(5) 0.2946(4) 0.112(2) Uani 1 1 d D . . H6A H 0.1115 0.2780 0.2724 0.168 Uiso 1 1 calc R . . H6B H 0.0974 0.1397 0.3024 0.168 Uiso 1 1 calc R . . H6C H 0.0845 0.2702 0.3451 0.168 Uiso 1 1 calc R . . C7 C 0.06966(15) 0.1831(5) 0.1576(4) 0.114(2) Uani 1 1 d D . . H7A H 0.0497 0.1915 0.1208 0.171 Uiso 1 1 calc R . . H7B H 0.0757 0.0910 0.1642 0.171 Uiso 1 1 calc R . . H7C H 0.0904 0.2301 0.1370 0.171 Uiso 1 1 calc R . . C8 C 0.02786(12) 0.1642(4) 0.2716(4) 0.0976(16) Uani 1 1 d D . . H8A H 0.0217 0.1993 0.3233 0.146 Uiso 1 1 calc R . . H8B H 0.0346 0.0725 0.2768 0.146 Uiso 1 1 calc R . . H8C H 0.0072 0.1715 0.2366 0.146 Uiso 1 1 calc R . . C9 C 0.08799(9) 0.5740(4) 0.2795(2) 0.0713(10) Uani 1 1 d . A . H9A H 0.1010 0.6536 0.2637 0.086 Uiso 1 1 calc R . . H9B H 0.1041 0.5201 0.3121 0.086 Uiso 1 1 calc R . . C10 C 0.05448(16) 0.5347(6) 0.4306(3) 0.1123(17) Uani 1 1 d . . . H10A H 0.0539 0.4404 0.4225 0.168 Uiso 1 1 calc R . . H10B H 0.0356 0.5597 0.4674 0.168 Uiso 1 1 calc R . . H10C H 0.0777 0.5598 0.4523 0.168 Uiso 1 1 calc R . . C11 C 0.05825(15) 0.7869(5) 0.3658(4) 0.1109(18) Uani 1 1 d . . . H11A H 0.0791 0.7866 0.4005 0.166 Uiso 1 1 calc R . . H11B H 0.0379 0.8247 0.3936 0.166 Uiso 1 1 calc R . . H11C H 0.0635 0.8388 0.3189 0.166 Uiso 1 1 calc R . . Mg1 Mg 0.0000 0.5000 0.21247(7) 0.0405(3) Uani 1 2 d S . . N2 N 0.04595(6) 0.3766(2) 0.22910(17) 0.0537(6) Uani 1 1 d D A . P1 P 0.04754(2) 0.61786(10) 0.33627(6) 0.0633(3) Uani 1 1 d . A . S1 S 0.073878(17) 0.48167(8) 0.19106(5) 0.0562(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0367(11) 0.0559(14) 0.0717(17) 0.0230(12) 0.0000(11) 0.0001(10) C1 0.0559(18) 0.072(2) 0.086(2) 0.035(2) 0.0067(18) -0.0021(16) C2 0.077(3) 0.109(11) 0.122(10) 0.067(8) -0.016(5) -0.008(6) C3 0.080(7) 0.145(9) 0.182(10) 0.103(8) -0.020(7) -0.058(7) C4 0.107(7) 0.135(8) 0.089(5) 0.033(5) 0.028(5) 0.017(6) N1' 0.0367(11) 0.0559(14) 0.0717(17) 0.0230(12) 0.0000(11) 0.0001(10) C1' 0.0559(18) 0.072(2) 0.086(2) 0.035(2) 0.0067(18) -0.0021(16) C2' 0.077(3) 0.109(11) 0.122(10) 0.067(8) -0.016(5) -0.008(6) C3' 0.080(7) 0.145(9) 0.182(10) 0.103(8) -0.020(7) -0.058(7) C4' 0.107(7) 0.135(8) 0.089(5) 0.033(5) 0.028(5) 0.017(6) C5 0.0517(18) 0.0514(18) 0.107(3) 0.0216(18) 0.0168(18) 0.0136(15) C6 0.074(3) 0.089(3) 0.173(5) 0.059(3) -0.009(3) 0.026(2) C7 0.120(4) 0.066(3) 0.155(5) -0.006(3) 0.056(4) 0.025(3) C8 0.081(3) 0.052(2) 0.160(5) 0.043(3) 0.031(3) 0.0083(19) C9 0.0401(16) 0.081(2) 0.093(3) 0.024(2) -0.0178(16) -0.0128(16) C10 0.099(3) 0.145(5) 0.092(3) 0.034(4) -0.006(3) 0.010(3) C11 0.095(3) 0.085(3) 0.153(5) -0.024(3) -0.028(3) -0.019(3) Mg1 0.0296(5) 0.0367(6) 0.0553(8) 0.000 0.000 0.0008(5) N2 0.0347(11) 0.0463(13) 0.0802(18) 0.0183(12) 0.0076(11) 0.0075(9) P1 0.0497(4) 0.0640(5) 0.0762(6) 0.0071(4) -0.0170(4) -0.0067(4) S1 0.0320(3) 0.0591(4) 0.0776(5) 0.0223(4) 0.0055(3) 0.0015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.481(4) . ? N1 S1 1.617(2) . ? N1 Mg1 2.102(2) . ? C1 C2 1.490(12) . ? C1 C4 1.508(11) . ? C1 C3 1.582(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C3' H3'1 0.9700 . ? C3' H3'2 0.9700 . ? C3' H3'3 0.9700 . ? C2' H2'1 0.9700 . ? C2' H2'2 0.9700 . ? C2' H2'3 0.9700 . ? C4' H4'1 0.9700 . ? C4' H4'2 0.9700 . ? C4' H4'3 0.9700 . ? C5 N2 1.472(4) . ? C5 C8 1.512(5) . ? C5 C7 1.517(7) . ? C5 C6 1.535(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 S1 1.838(4) . ? C9 P1 1.838(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 P1 1.819(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 P1 1.834(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? Mg1 N1' 2.102(2) 2_565 ? Mg1 N1 2.102(2) 2_565 ? Mg1 N2 2.138(2) . ? Mg1 S1 2.7757(9) 2_565 ? Mg1 P1 2.9855(13) . ? N2 S1 1.622(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 C1 N1 S1 117.8(2) . . ? C1 N1 Mg1 144.1(2) . . ? S1 N1 Mg1 95.69(12) . . ? N1 C1 C2 107.4(11) . . ? N1 C1 C4 117.8(6) . . ? C2 C1 C4 115.6(12) . . ? N1 C1 C3 104.2(7) . . ? C2 C1 C3 107.1(10) . . ? C4 C1 C3 103.5(8) . . ? H3'1 C3' H3'2 109.5 . . ? H3'1 C3' H3'3 109.5 . . ? H3'2 C3' H3'3 109.5 . . ? H2'1 C2' H2'2 109.5 . . ? H2'1 C2' H2'3 109.5 . . ? H2'2 C2' H2'3 109.5 . . ? H4'1 C4' H4'2 109.5 . . ? H4'1 C4' H4'3 109.5 . . ? H4'2 C4' H4'3 109.5 . . ? N2 C5 C8 105.4(3) . . ? N2 C5 C7 111.5(3) . . ? C8 C5 C7 109.8(4) . . ? N2 C5 C6 112.0(3) . . ? C8 C5 C6 108.8(4) . . ? C7 C5 C6 109.3(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? S1 C9 P1 108.24(16) . . ? S1 C9 H9A 110.1 . . ? P1 C9 H9A 110.1 . . ? S1 C9 H9B 110.1 . . ? P1 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? P1 C10 H10A 109.5 . . ? P1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1' Mg1 N1 0.00(18) 2_565 2_565 ? N1' Mg1 N1 120.99(17) 2_565 . ? N1 Mg1 N1 120.99(17) 2_565 . ? N1' Mg1 N2 118.03(10) 2_565 . ? N1 Mg1 N2 118.03(10) 2_565 . ? N1 Mg1 N2 70.07(9) . . ? N1' Mg1 N2 70.07(9) 2_565 2_565 ? N1 Mg1 N2 70.07(9) 2_565 2_565 ? N1 Mg1 N2 118.03(10) . 2_565 ? N2 Mg1 N2 164.93(17) . 2_565 ? N1' Mg1 S1 35.43(7) 2_565 2_565 ? N1 Mg1 S1 35.43(7) 2_565 2_565 ? N1 Mg1 S1 133.38(8) . 2_565 ? N2 Mg1 S1 147.84(7) . 2_565 ? N2 Mg1 S1 35.66(6) 2_565 2_565 ? N1' Mg1 P1 163.71(8) 2_565 . ? N1 Mg1 P1 163.71(8) 2_565 . ? N1 Mg1 P1 74.24(8) . . ? N2 Mg1 P1 70.82(8) . . ? N2 Mg1 P1 98.35(8) 2_565 . ? S1 Mg1 P1 130.49(4) 2_565 . ? N1' Mg1 P1 74.24(8) 2_565 2_565 ? N1 Mg1 P1 74.24(8) 2_565 2_565 ? N1 Mg1 P1 163.71(8) . 2_565 ? N2 Mg1 P1 98.35(8) . 2_565 ? N2 Mg1 P1 70.82(8) 2_565 2_565 ? S1 Mg1 P1 62.11(3) 2_565 2_565 ? P1 Mg1 P1 91.34(5) . 2_565 ? C5 N2 S1 116.4(2) . . ? C5 N2 Mg1 145.9(2) . . ? S1 N2 Mg1 94.14(11) . . ? C10 P1 C11 99.7(3) . . ? C10 P1 C9 103.1(2) . . ? C11 P1 C9 101.1(2) . . ? C10 P1 Mg1 120.5(2) . . ? C11 P1 Mg1 134.00(19) . . ? C9 P1 Mg1 91.30(12) . . ? N1 S1 N2 97.43(12) . . ? N1 S1 C9 102.86(16) . . ? N2 S1 C9 101.49(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 N1 C1 C2 153.9(11) . . . . ? Mg1 N1 C1 C2 -3.0(12) . . . . ? S1 N1 C1 C4 21.2(10) . . . . ? Mg1 N1 C1 C4 -135.7(9) . . . . ? S1 N1 C1 C3 -92.7(7) . . . . ? Mg1 N1 C1 C3 110.3(8) . . . . ? C1 N1 Mg1 N1' 37.1(4) . . . 2_565 ? S1 N1 Mg1 N1' -122.53(15) . . . 2_565 ? C1 N1 Mg1 N1 37.1(4) . . . 2_565 ? S1 N1 Mg1 N1 -122.53(15) . . . 2_565 ? C1 N1 Mg1 N2 148.5(5) . . . . ? S1 N1 Mg1 N2 -11.10(13) . . . . ? C1 N1 Mg1 N2 -45.4(5) . . . 2_565 ? S1 N1 Mg1 N2 154.98(12) . . . 2_565 ? C1 N1 Mg1 S1 -5.2(5) . . . 2_565 ? S1 N1 Mg1 S1 -164.78(7) . . . 2_565 ? C1 N1 Mg1 P1 -136.6(5) . . . . ? S1 N1 Mg1 P1 63.79(11) . . . . ? C1 N1 Mg1 P1 -165.1(3) . . . 2_565 ? S1 N1 Mg1 P1 35.3(4) . . . 2_565 ? C8 C5 N2 S1 -178.5(3) . . . . ? C7 C5 N2 S1 -59.4(4) . . . . ? C6 C5 N2 S1 63.4(4) . . . . ? C8 C5 N2 Mg1 -27.3(6) . . . . ? C7 C5 N2 Mg1 91.7(5) . . . . ? C6 C5 N2 Mg1 -145.5(4) . . . . ? N1' Mg1 N2 C5 -28.0(5) 2_565 . . . ? N1 Mg1 N2 C5 -28.0(5) 2_565 . . . ? N1 Mg1 N2 C5 -143.3(5) . . . . ? N2 Mg1 N2 C5 91.5(4) 2_565 . . . ? S1 Mg1 N2 C5 -0.5(6) 2_565 . . . ? P1 Mg1 N2 C5 137.1(5) . . . . ? P1 Mg1 N2 C5 48.6(5) 2_565 . . . ? N1' Mg1 N2 S1 126.34(14) 2_565 . . . ? N1 Mg1 N2 S1 126.34(14) 2_565 . . . ? N1 Mg1 N2 S1 11.04(13) . . . . ? N2 Mg1 N2 S1 -114.16(12) 2_565 . . . ? S1 Mg1 N2 S1 153.78(12) 2_565 . . . ? P1 Mg1 N2 S1 -68.61(11) . . . . ? P1 Mg1 N2 S1 -157.12(11) 2_565 . . . ? S1 C9 P1 C10 118.4(3) . . . . ? S1 C9 P1 C11 -138.8(3) . . . . ? S1 C9 P1 Mg1 -3.35(17) . . . . ? N1' Mg1 P1 C10 59.9(4) 2_565 . . . ? N1 Mg1 P1 C10 59.9(4) 2_565 . . . ? N1 Mg1 P1 C10 -139.7(2) . . . . ? N2 Mg1 P1 C10 -65.8(2) . . . . ? N2 Mg1 P1 C10 103.4(2) 2_565 . . . ? S1 Mg1 P1 C10 86.1(2) 2_565 . . . ? P1 Mg1 P1 C10 32.6(2) 2_565 . . . ? N1' Mg1 P1 C11 -87.3(4) 2_565 . . . ? N1 Mg1 P1 C11 -87.3(4) 2_565 . . . ? N1 Mg1 P1 C11 73.1(3) . . . . ? N2 Mg1 P1 C11 147.0(3) . . . . ? N2 Mg1 P1 C11 -43.8(3) 2_565 . . . ? S1 Mg1 P1 C11 -61.1(3) 2_565 . . . ? P1 Mg1 P1 C11 -114.6(3) 2_565 . . . ? N1' Mg1 P1 C9 166.0(3) 2_565 . . . ? N1 Mg1 P1 C9 166.0(3) 2_565 . . . ? N1 Mg1 P1 C9 -33.66(14) . . . . ? N2 Mg1 P1 C9 40.27(14) . . . . ? N2 Mg1 P1 C9 -150.54(15) 2_565 . . . ? S1 Mg1 P1 C9 -167.89(12) 2_565 . . . ? P1 Mg1 P1 C9 138.64(13) 2_565 . . . ? C1 N1 S1 N2 -152.7(3) . . . . ? Mg1 N1 S1 N2 13.92(16) . . . . ? C1 N1 S1 C9 103.6(3) . . . . ? Mg1 N1 S1 C9 -89.72(15) . . . . ? C5 N2 S1 N1 150.6(3) . . . . ? Mg1 N2 S1 N1 -13.64(16) . . . . ? C5 N2 S1 C9 -104.6(3) . . . . ? Mg1 N2 S1 C9 91.16(15) . . . . ? P1 C9 S1 N1 53.2(2) . . . . ? P1 C9 S1 N2 -47.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.227 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.052 data_p-1a _database_code_depnum_ccdc_archive 'CCDC 779990' #TrackingRef '- all_full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H52 Li2 N4 P2 S2 Si4' _chemical_formula_weight 576.94 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' Si Si 0.0817 0.0704 '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 10.2715(11) _cell_length_b 10.3560(11) _cell_length_c 10.4832(11) _cell_angle_alpha 68.6360(10) _cell_angle_beta 65.7280(10) _cell_angle_gamma 60.9900(10) _cell_volume 869.77(16) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7152 _cell_measurement_theta_min 2.2985 _cell_measurement_theta_max 26.755 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 312 _exptl_absorpt_coefficient_mu 0.396 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9447 _exptl_absorpt_correction_T_max 0.9897 _exptl_absorpt_process_details SADABS-2008/2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC Mo micro source' _diffrn_radiation_monochromator 'INCOATEC quazar mirror optics' _diffrn_measurement_device_type 'Bruker Smart Apex II with D8-Goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21105 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3546 _reflns_number_gt 3300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex v2.2-0' _computing_cell_refinement 'SAINT v7.46A' _computing_data_reduction 'SAINT v7.46A' _computing_structure_solution 'SHELXS in SHELXTL v2008/2 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL in SHELXTL v2008/2 (Sheldrick, 2008)' _computing_molecular_graphics 'XSHELL v4.01' _computing_publication_material 'XSHELL v4.01' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.5002P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3546 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0619 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.67155(14) 0.66104(13) 0.56528(13) 0.0208(2) Uani 1 1 d . . . H1A H 0.7317 0.5530 0.5607 0.025 Uiso 1 1 calc R . . H1B H 0.5601 0.6818 0.5906 0.025 Uiso 1 1 calc R . . C2 C 0.91628(15) 0.62329(16) 0.65576(14) 0.0275(3) Uani 1 1 d . . . H2A H 0.9530 0.6879 0.5668 0.041 Uiso 1 1 calc R . . H2B H 0.9605 0.5202 0.6412 0.041 Uiso 1 1 calc R . . H2C H 0.9491 0.6228 0.7316 0.041 Uiso 1 1 calc R . . C3 C 0.67127(17) 0.53900(15) 0.85184(14) 0.0287(3) Uani 1 1 d . . . H3A H 0.6985 0.5335 0.9335 0.043 Uiso 1 1 calc R . . H3B H 0.7363 0.4443 0.8177 0.043 Uiso 1 1 calc R . . H3C H 0.5616 0.5553 0.8814 0.043 Uiso 1 1 calc R . . C4 C 0.81094(17) 0.73284(19) 0.04414(15) 0.0354(3) Uani 1 1 d . . . H4A H 0.7970 0.8381 -0.0008 0.053 Uiso 1 1 calc R . . H4B H 0.8290 0.6811 -0.0271 0.053 Uiso 1 1 calc R . . H4C H 0.9005 0.6824 0.0821 0.053 Uiso 1 1 calc R . . C5 C 0.6623(2) 0.52425(15) 0.26971(17) 0.0365(3) Uani 1 1 d . . . H5A H 0.7520 0.4721 0.3077 0.055 Uiso 1 1 calc R . . H5B H 0.6815 0.4769 0.1946 0.055 Uiso 1 1 calc R . . H5C H 0.5693 0.5175 0.3469 0.055 Uiso 1 1 calc R . . C6 C 0.45834(16) 0.82382(17) 0.12650(16) 0.0322(3) Uani 1 1 d . . . H6A H 0.3719 0.7996 0.2005 0.048 Uiso 1 1 calc R . . H6B H 0.4827 0.7896 0.0406 0.048 Uiso 1 1 calc R . . H6C H 0.4289 0.9332 0.1032 0.048 Uiso 1 1 calc R . . C7 C 0.76306(16) 1.15187(15) 0.16399(14) 0.0267(3) Uani 1 1 d . . . H7A H 0.7639 1.0976 0.1040 0.040 Uiso 1 1 calc R . . H7B H 0.8372 1.2002 0.1098 0.040 Uiso 1 1 calc R . . H7C H 0.6585 1.2291 0.1929 0.040 Uiso 1 1 calc R . . C8 C 0.81309(15) 1.11897(15) 0.44392(15) 0.0249(3) Uani 1 1 d . . . H8A H 0.7065 1.1914 0.4766 0.037 Uiso 1 1 calc R . . H8B H 0.8821 1.1730 0.3899 0.037 Uiso 1 1 calc R . . H8C H 0.8473 1.0468 0.5268 0.037 Uiso 1 1 calc R . . C9 C 1.02319(14) 0.88049(15) 0.26074(15) 0.0287(3) Uani 1 1 d . . . H9A H 1.0599 0.8083 0.3424 0.043 Uiso 1 1 calc R . . H9B H 1.0905 0.9362 0.2055 0.043 Uiso 1 1 calc R . . H9C H 1.0259 0.8261 0.1997 0.043 Uiso 1 1 calc R . . S1 S 0.72692(3) 0.77499(3) 0.38842(3) 0.01553(8) Uani 1 1 d . . . P1 P 0.70386(3) 0.69614(3) 0.70762(3) 0.01899(8) Uani 1 1 d . . . Si1 Si 0.63216(4) 0.72697(4) 0.19344(3) 0.01819(8) Uani 1 1 d . . . Si2 Si 0.81935(4) 1.01589(4) 0.32679(3) 0.01732(8) Uani 1 1 d . . . N1 N 0.59257(11) 0.81657(11) 0.32199(11) 0.0185(2) Uani 1 1 d . . . N2 N 0.69080(11) 0.92835(11) 0.42898(10) 0.0164(2) Uani 1 1 d . . . Li1 Li 0.4577(2) 1.0138(2) 0.3817(2) 0.0222(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0250(6) 0.0181(6) 0.0210(6) -0.0020(5) -0.0066(5) -0.0112(5) C2 0.0206(6) 0.0324(7) 0.0255(6) -0.0064(5) -0.0068(5) -0.0071(5) C3 0.0330(7) 0.0252(7) 0.0214(6) 0.0006(5) -0.0070(5) -0.0112(6) C4 0.0290(7) 0.0510(9) 0.0266(7) -0.0174(6) -0.0007(6) -0.0153(7) C5 0.0533(9) 0.0204(7) 0.0447(9) -0.0068(6) -0.0229(7) -0.0139(6) C6 0.0293(7) 0.0366(8) 0.0342(7) -0.0098(6) -0.0155(6) -0.0086(6) C7 0.0286(7) 0.0269(7) 0.0231(6) -0.0013(5) -0.0057(5) -0.0139(5) C8 0.0247(6) 0.0236(6) 0.0320(7) -0.0061(5) -0.0103(5) -0.0118(5) C9 0.0179(6) 0.0284(7) 0.0336(7) -0.0078(6) 0.0001(5) -0.0096(5) S1 0.01456(14) 0.01380(14) 0.01749(14) -0.00544(10) -0.00316(10) -0.00470(10) P1 0.01912(15) 0.01736(15) 0.01761(15) -0.00435(11) -0.00416(12) -0.00547(12) Si1 0.01976(16) 0.01692(16) 0.01943(16) -0.00636(12) -0.00614(13) -0.00613(13) Si2 0.01502(16) 0.01688(16) 0.01992(16) -0.00420(12) -0.00289(12) -0.00766(12) N1 0.0169(5) 0.0175(5) 0.0220(5) -0.0078(4) -0.0061(4) -0.0045(4) N2 0.0155(5) 0.0147(5) 0.0191(5) -0.0065(4) -0.0017(4) -0.0065(4) Li1 0.0224(10) 0.0182(9) 0.0233(10) -0.0074(8) -0.0045(8) -0.0056(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 C9 Si2 1.8701(13) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? S1 N1 1.6031(10) . ? S1 N2 1.6221(10) . ? S1 C1 1.8286(12) . ? P1 C2 1.8310(13) . ? P1 C3 1.8346(13) . ? P1 C1 1.8406(13) . ? Si2 N2 1.7331(10) . ? Si2 C8 1.8642(13) . ? Si2 C7 1.8710(13) . ? Si1 N1 1.7138(10) . ? Si1 C6 1.8618(14) . ? Si1 C5 1.8688(14) . ? Si1 C4 1.8712(14) . ? N1 Li1 1.989(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N2 Li1 2.315(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Li1 P1 2.655(2) 2_676 ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 S1 N2 105.89(5) . . ? N1 S1 C1 102.66(6) . . ? N2 S1 C1 101.53(5) . . ? C2 P1 C3 100.05(6) . . ? C2 P1 C1 101.71(6) . . ? C3 P1 C1 99.36(6) . . ? C2 P1 Li1 119.58(7) . 2_676 ? C3 P1 Li1 138.00(7) . 2_676 ? C1 P1 Li1 86.45(6) . 2_676 ? N2 Si2 C8 106.30(5) . . ? N2 Si2 C9 113.23(5) . . ? C8 Si2 C9 109.71(6) . . ? N2 Si2 C7 111.80(6) . . ? C8 Si2 C7 109.76(6) . . ? C9 Si2 C7 106.06(6) . . ? N1 Si1 C6 106.51(6) . . ? N1 Si1 C5 111.34(6) . . ? C6 Si1 C5 108.41(7) . . ? N1 Si1 C4 112.08(6) . . ? C6 Si1 C4 110.97(7) . . ? C5 Si1 C4 107.50(8) . . ? S1 N1 Si1 119.57(6) . . ? S1 N1 Li1 95.76(8) . . ? Si1 N1 Li1 140.18(9) . . ? S1 C1 P1 113.96(6) . . ? S1 C1 H1A 108.8 . . ? P1 C1 H1A 108.8 . . ? S1 C1 H1B 108.8 . . ? P1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? S1 N2 Si2 116.70(6) . . ? S1 N2 Li1 122.12(8) . 2_676 ? Si2 N2 Li1 119.18(8) . 2_676 ? S1 N2 Li1 83.70(6) . . ? Si2 N2 Li1 120.51(7) . . ? Li1 N2 Li1 80.96(9) 2_676 . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 Li1 N2 133.07(12) . 2_676 ? N1 Li1 N2 73.00(8) . . ? N2 Li1 N2 99.04(9) 2_676 . ? N1 Li1 P1 144.16(11) . 2_676 ? N2 Li1 P1 79.63(7) 2_676 2_676 ? N2 Li1 P1 122.61(9) . 2_676 ? N1 Li1 Li1 104.51(12) . 2_676 ? N2 Li1 Li1 53.94(7) 2_676 2_676 ? N2 Li1 Li1 45.10(7) . 2_676 ? P1 Li1 Li1 108.18(10) 2_676 2_676 ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 S1 N1 Si1 148.77(6) . . . . ? C1 S1 N1 Si1 -105.16(7) . . . . ? N2 S1 N1 Li1 -12.10(8) . . . . ? C1 S1 N1 Li1 93.97(8) . . . . ? C6 Si1 N1 S1 -172.27(7) . . . . ? C5 Si1 N1 S1 69.73(9) . . . . ? C4 Si1 N1 S1 -50.73(9) . . . . ? C6 Si1 N1 Li1 -22.88(15) . . . . ? C5 Si1 N1 Li1 -140.88(13) . . . . ? C4 Si1 N1 Li1 98.66(14) . . . . ? N1 S1 C1 P1 -141.24(7) . . . . ? N2 S1 C1 P1 -31.84(8) . . . . ? C2 P1 C1 S1 -67.20(8) . . . . ? C3 P1 C1 S1 -169.61(7) . . . . ? Li1 P1 C1 S1 52.29(8) 2_676 . . . ? N1 S1 N2 Si2 -110.69(7) . . . . ? C1 S1 N2 Si2 142.42(6) . . . . ? N1 S1 N2 Li1 85.55(10) . . . 2_676 ? C1 S1 N2 Li1 -21.34(10) . . . 2_676 ? N1 S1 N2 Li1 10.39(7) . . . . ? C1 S1 N2 Li1 -96.50(7) . . . . ? C8 Si2 N2 S1 -152.29(6) . . . . ? C9 Si2 N2 S1 -31.78(9) . . . . ? C7 Si2 N2 S1 87.96(8) . . . . ? C8 Si2 N2 Li1 11.96(10) . . . 2_676 ? C9 Si2 N2 Li1 132.48(10) . . . 2_676 ? C7 Si2 N2 Li1 -107.79(10) . . . 2_676 ? C8 Si2 N2 Li1 108.86(8) . . . . ? C9 Si2 N2 Li1 -130.62(8) . . . . ? C7 Si2 N2 Li1 -10.89(9) . . . . ? S1 N1 Li1 N2 -78.02(16) . . . 2_676 ? Si1 N1 Li1 N2 128.41(14) . . . 2_676 ? S1 N1 Li1 N2 8.50(6) . . . . ? Si1 N1 Li1 N2 -145.08(11) . . . . ? S1 N1 Li1 P1 131.12(16) . . . 2_676 ? Si1 N1 Li1 P1 -22.5(3) . . . 2_676 ? S1 N1 Li1 Li1 -24.21(12) . . . 2_676 ? Si1 N1 Li1 Li1 -177.78(9) . . . 2_676 ? S1 N2 Li1 N1 -8.40(6) . . . . ? Si2 N2 Li1 N1 108.96(8) . . . . ? Li1 N2 Li1 N1 -132.41(11) 2_676 . . . ? S1 N2 Li1 N2 124.00(9) . . . 2_676 ? Si2 N2 Li1 N2 -118.63(9) . . . 2_676 ? Li1 N2 Li1 N2 0.0 2_676 . . 2_676 ? S1 N2 Li1 P1 -152.57(9) . . . 2_676 ? Si2 N2 Li1 P1 -35.21(13) . . . 2_676 ? Li1 N2 Li1 P1 83.43(10) 2_676 . . 2_676 ? S1 N2 Li1 Li1 124.01(9) . . . 2_676 ? Si2 N2 Li1 Li1 -118.63(9) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.314 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.039 #===END data_p-1 _database_code_depnum_ccdc_archive 'CCDC 779991' #TrackingRef '- all_full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H64 Li2 N4 P2 S2 Si4' _chemical_formula_weight 661.09 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' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6002(6) _cell_length_b 10.6350(10) _cell_length_c 10.7744(6) _cell_angle_alpha 100.7850(10) _cell_angle_beta 117.3660(10) _cell_angle_gamma 103.4460(10) _cell_volume 986.48(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 2.5065 _cell_measurement_theta_max 29.125 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8587 _exptl_absorpt_correction_T_max 0.9893 _exptl_absorpt_process_details SADABS-2008/2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS-Mo rotating anode' _diffrn_radiation_monochromator 'INCOATEC Helios mirror optics' _diffrn_measurement_device_type 'Bruker TXS-Mo rotating anode' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39887 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0074 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4676 _reflns_number_gt 4365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.2-0' _computing_cell_refinement 'SAINT V7.46A' _computing_data_reduction 'SAINT V7.46A' _computing_structure_solution 'SHELXS in SHELXTL v2008/4' _computing_structure_refinement 'SHELXL in SHELXTL v2008/4' _computing_molecular_graphics 'XSHELL v4.01' _computing_publication_material 'XSHELL v4.01' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.4560P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4676 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.03063(16) 0.53036(15) 0.25222(17) 0.0340(3) Uani 1 1 d . . . H1A H 0.0014 0.5787 0.1805 0.051 Uiso 1 1 calc R . . H1B H -0.0577 0.4858 0.2578 0.051 Uiso 1 1 calc R . . H1C H 0.0660 0.4606 0.2203 0.051 Uiso 1 1 calc R . . C2 C 0.10781(17) 0.77313(16) 0.50719(18) 0.0344(3) Uani 1 1 d . . . H2A H 0.1870 0.8373 0.6074 0.052 Uiso 1 1 calc R . . H2B H 0.0213 0.7183 0.5096 0.052 Uiso 1 1 calc R . . H2C H 0.0734 0.8249 0.4400 0.052 Uiso 1 1 calc R . . C3 C 0.25392(18) 0.55830(15) 0.56846(18) 0.0343(3) Uani 1 1 d . . . H3A H 0.2921 0.4945 0.5312 0.051 Uiso 1 1 calc R . . H3B H 0.1686 0.5064 0.5743 0.051 Uiso 1 1 calc R . . H3C H 0.3359 0.6227 0.6676 0.051 Uiso 1 1 calc R . . C4 C 0.89791(17) 0.84578(17) 0.72055(17) 0.0362(3) Uani 1 1 d . . . H4A H 0.8420 0.7462 0.6787 0.054 Uiso 1 1 calc R . . H4B H 0.9907 0.8686 0.8169 0.054 Uiso 1 1 calc R . . H4C H 0.9256 0.8756 0.6527 0.054 Uiso 1 1 calc R . . C5 C 0.71900(17) 0.87026(15) 0.87042(15) 0.0316(3) Uani 1 1 d . . . H5A H 0.6386 0.9012 0.8697 0.047 Uiso 1 1 calc R . . H5B H 0.8080 0.9059 0.9719 0.047 Uiso 1 1 calc R . . H5C H 0.6812 0.7695 0.8347 0.047 Uiso 1 1 calc R . . C6 C 0.88623(15) 1.12360(14) 0.83362(15) 0.0282(3) Uani 1 1 d . . . H6A H 0.9523 1.1491 0.7949 0.042 Uiso 1 1 calc R . . H6B H 0.9490 1.1472 0.9416 0.042 Uiso 1 1 calc R . . H6C H 0.8161 1.1736 0.8106 0.042 Uiso 1 1 calc R . . C7 C 0.51522(15) 0.68832(12) 0.33825(14) 0.0227(2) Uani 1 1 d . . . H7 H 0.6175 0.6796 0.3799 0.027 Uiso 1 1 calc R . . C8 C 0.39809(18) 0.54279(14) 0.24487(17) 0.0331(3) Uani 1 1 d . . . H8A H 0.4050 0.4875 0.3093 0.050 Uiso 1 1 calc R . . H8B H 0.4185 0.5014 0.1702 0.050 Uiso 1 1 calc R . . H8C H 0.2954 0.5460 0.1951 0.050 Uiso 1 1 calc R . . C9 C 0.35850(15) 0.72585(14) 0.05206(14) 0.0277(3) Uani 1 1 d . . . H9A H 0.3677 0.6388 0.0127 0.033 Uiso 1 1 calc R . . H9B H 0.2623 0.7025 0.0517 0.033 Uiso 1 1 calc R . . C10 C 0.3517(2) 0.81040(17) -0.04908(16) 0.0391(3) Uani 1 1 d . . . H10A H 0.3497 0.8994 -0.0068 0.059 Uiso 1 1 calc R . . H10B H 0.2592 0.7610 -0.1477 0.059 Uiso 1 1 calc R . . H10C H 0.4417 0.8252 -0.0577 0.059 Uiso 1 1 calc R . . C11 C 0.68650(15) 0.82307(14) 0.22816(16) 0.0283(3) Uani 1 1 d . . . H11A H 0.6980 0.8878 0.1756 0.034 Uiso 1 1 calc R . . H11B H 0.7782 0.8619 0.3298 0.034 Uiso 1 1 calc R . . C12 C 0.68595(18) 0.68781(16) 0.14904(18) 0.0356(3) Uani 1 1 d . . . H12A H 0.6778 0.6227 0.2009 0.053 Uiso 1 1 calc R . . H12B H 0.7809 0.7045 0.1491 0.053 Uiso 1 1 calc R . . H12C H 0.5988 0.6494 0.0463 0.053 Uiso 1 1 calc R . . Li1 Li 0.4151(2) 0.9641(2) 0.5438(2) 0.0213(4) Uani 1 1 d . . . N1 N 0.33293(11) 0.75951(10) 0.43262(11) 0.01938(19) Uani 1 1 d . . . N2 N 0.61443(11) 0.90764(10) 0.57732(11) 0.01837(19) Uani 1 1 d . . . P1 P 0.52025(4) 0.81858(3) 0.24417(3) 0.02007(8) Uani 1 1 d . . . S1 S 0.49701(3) 0.74885(3) 0.49762(3) 0.01809(8) Uani 1 1 d . . . Si1 Si 0.18756(4) 0.65625(3) 0.43937(4) 0.02178(8) Uani 1 1 d . . . Si2 Si 0.77471(4) 0.93548(3) 0.74601(4) 0.01909(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0225(6) 0.0262(7) 0.0385(8) 0.0020(6) 0.0116(6) 0.0013(5) C2 0.0313(7) 0.0316(7) 0.0451(8) 0.0090(6) 0.0249(7) 0.0123(6) C3 0.0386(8) 0.0291(7) 0.0423(8) 0.0192(6) 0.0248(7) 0.0107(6) C4 0.0296(7) 0.0472(9) 0.0311(7) 0.0093(6) 0.0115(6) 0.0254(7) C5 0.0351(7) 0.0337(7) 0.0253(6) 0.0135(5) 0.0157(6) 0.0089(6) C6 0.0228(6) 0.0269(6) 0.0241(6) 0.0097(5) 0.0052(5) 0.0059(5) C7 0.0270(6) 0.0198(6) 0.0240(6) 0.0065(5) 0.0151(5) 0.0101(5) C8 0.0452(8) 0.0187(6) 0.0342(7) 0.0031(5) 0.0247(7) 0.0066(6) C9 0.0255(6) 0.0282(6) 0.0224(6) 0.0044(5) 0.0098(5) 0.0078(5) C10 0.0496(9) 0.0366(8) 0.0216(6) 0.0099(6) 0.0129(6) 0.0131(7) C11 0.0257(6) 0.0277(6) 0.0312(7) 0.0065(5) 0.0173(5) 0.0069(5) C12 0.0363(8) 0.0356(8) 0.0416(8) 0.0074(6) 0.0271(7) 0.0142(6) Li1 0.0234(10) 0.0189(9) 0.0214(9) 0.0064(8) 0.0114(8) 0.0084(8) N1 0.0162(4) 0.0169(4) 0.0220(5) 0.0072(4) 0.0077(4) 0.0059(4) N2 0.0162(4) 0.0158(4) 0.0204(5) 0.0064(4) 0.0076(4) 0.0058(4) P1 0.02167(15) 0.01801(15) 0.01846(15) 0.00453(11) 0.00976(12) 0.00696(12) S1 0.01958(14) 0.01509(13) 0.02124(14) 0.00674(10) 0.01131(11) 0.00733(10) Si1 0.01907(16) 0.01721(16) 0.02695(17) 0.00562(13) 0.01215(14) 0.00466(12) Si2 0.01809(15) 0.02150(16) 0.01913(16) 0.00892(12) 0.00895(13) 0.00985(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 C1 Si1 1.8698(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 Si1 1.8736(14) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si1 1.8703(15) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 Si2 1.8712(14) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Si2 1.8741(14) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si2 1.8597(14) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.5246(18) . ? C7 S1 1.8300(12) . ? C7 P1 1.8682(13) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.525(2) . ? C9 P1 1.8395(13) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.5259(19) . ? C11 P1 1.8389(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? Li1 N1 2.028(2) . ? Li1 N2 2.219(2) . ? Li1 P1 2.622(2) 2_676 ? N1 S1 1.5906(10) . ? N1 Si1 1.7122(11) . ? N2 S1 1.6235(10) . ? N2 Si2 1.7330(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 Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 S1 107.92(9) . . ? C8 C7 P1 118.47(9) . . ? S1 C7 P1 111.63(6) . . ? C8 C7 H7 106.0 . . ? S1 C7 H7 106.0 . . ? P1 C7 H7 106.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 112.08(10) . . ? C10 C9 H9A 109.2 . . ? P1 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? P1 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 P1 117.80(10) . . ? C12 C11 H11A 107.9 . . ? P1 C11 H11A 107.9 . . ? C12 C11 H11B 107.9 . . ? P1 C11 H11B 107.9 . . ? H11A C11 H11B 107.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 Li1 N2 117.92(11) . 2_676 ? N1 Li1 N2 73.19(8) . . ? N2 Li1 N2 110.54(10) 2_676 . ? N1 Li1 Li1 97.38(12) . 2_676 ? N2 Li1 Li1 58.80(9) 2_676 2_676 ? N2 Li1 Li1 51.74(8) . 2_676 ? N1 Li1 P1 154.66(11) . 2_676 ? N2 Li1 P1 83.25(7) 2_676 2_676 ? N2 Li1 P1 114.22(9) . 2_676 ? Li1 Li1 P1 106.03(12) 2_676 2_676 ? N1 Li1 S1 36.41(4) . . ? N2 Li1 S1 125.63(10) 2_676 . ? N2 Li1 S1 37.35(4) . . ? Li1 Li1 S1 76.24(10) 2_676 . ? P1 Li1 S1 141.66(9) 2_676 . ? S1 N1 Si1 123.87(6) . . ? S1 N1 Li1 94.40(8) . . ? Si1 N1 Li1 117.57(8) . . ? S1 N2 Si2 112.80(6) . . ? S1 N2 Li1 118.62(8) . 2_676 ? Si2 N2 Li1 127.08(8) . 2_676 ? S1 N2 Li1 86.64(7) . . ? Si2 N2 Li1 126.67(8) . . ? Li1 N2 Li1 69.46(10) 2_676 . ? C11 P1 C9 103.00(6) . . ? C11 P1 C7 100.84(6) . . ? C9 P1 C7 103.57(6) . . ? C11 P1 Li1 111.58(6) . 2_676 ? C9 P1 Li1 133.73(7) . 2_676 ? C7 P1 Li1 99.18(6) . 2_676 ? N1 S1 N2 104.22(5) . . ? N1 S1 C7 106.57(6) . . ? N2 S1 C7 102.80(6) . . ? N1 S1 Li1 49.19(6) . . ? N2 S1 Li1 56.02(6) . . ? C7 S1 Li1 122.99(6) . . ? N1 Si1 C1 112.28(6) . . ? N1 Si1 C3 112.57(6) . . ? C1 Si1 C3 108.21(7) . . ? N1 Si1 C2 106.28(6) . . ? C1 Si1 C2 108.07(7) . . ? C3 Si1 C2 109.30(7) . . ? N2 Si2 C6 107.83(5) . . ? N2 Si2 C4 111.48(6) . . ? C6 Si2 C4 108.69(7) . . ? N2 Si2 C5 110.75(6) . . ? C6 Si2 C5 110.25(7) . . ? C4 Si2 C5 107.82(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Li1 N1 S1 113.09(11) 2_676 . . . ? N2 Li1 N1 S1 8.33(6) . . . . ? Li1 Li1 N1 S1 54.59(12) 2_676 . . . ? P1 Li1 N1 S1 -103.0(2) 2_676 . . . ? N2 Li1 N1 Si1 -114.79(11) 2_676 . . . ? N2 Li1 N1 Si1 140.46(7) . . . . ? Li1 Li1 N1 Si1 -173.29(9) 2_676 . . . ? P1 Li1 N1 Si1 29.2(3) 2_676 . . . ? S1 Li1 N1 Si1 132.12(9) . . . . ? N1 Li1 N2 S1 -8.15(6) . . . . ? N2 Li1 N2 S1 -122.30(10) 2_676 . . . ? Li1 Li1 N2 S1 -122.30(10) 2_676 . . . ? P1 Li1 N2 S1 145.92(8) 2_676 . . . ? N1 Li1 N2 Si2 -124.27(8) . . . . ? N2 Li1 N2 Si2 121.58(10) 2_676 . . . ? Li1 Li1 N2 Si2 121.58(10) 2_676 . . . ? P1 Li1 N2 Si2 29.81(13) 2_676 . . . ? S1 Li1 N2 Si2 -116.11(9) . . . . ? N1 Li1 N2 Li1 114.15(11) . . . 2_676 ? N2 Li1 N2 Li1 0.0 2_676 . . 2_676 ? P1 Li1 N2 Li1 -91.77(11) 2_676 . . 2_676 ? S1 Li1 N2 Li1 122.30(10) . . . 2_676 ? C12 C11 P1 C9 -51.05(13) . . . . ? C12 C11 P1 C7 55.78(12) . . . . ? C12 C11 P1 Li1 160.28(11) . . . 2_676 ? C10 C9 P1 C11 -69.46(12) . . . . ? C10 C9 P1 C7 -174.19(10) . . . . ? C10 C9 P1 Li1 68.54(14) . . . 2_676 ? C8 C7 P1 C11 -102.25(11) . . . . ? S1 C7 P1 C11 131.48(7) . . . . ? C8 C7 P1 C9 4.13(11) . . . . ? S1 C7 P1 C9 -122.15(7) . . . . ? C8 C7 P1 Li1 143.53(10) . . . 2_676 ? S1 C7 P1 Li1 17.26(8) . . . 2_676 ? Si1 N1 S1 N2 -138.92(7) . . . . ? Li1 N1 S1 N2 -11.28(8) . . . . ? Si1 N1 S1 C7 112.78(8) . . . . ? Li1 N1 S1 C7 -119.57(8) . . . . ? Si1 N1 S1 Li1 -127.64(11) . . . . ? Si2 N2 S1 N1 138.91(6) . . . . ? Li1 N2 S1 N1 -54.09(10) 2_676 . . . ? Li1 N2 S1 N1 10.28(8) . . . . ? Si2 N2 S1 C7 -110.03(7) . . . . ? Li1 N2 S1 C7 56.96(10) 2_676 . . . ? Li1 N2 S1 C7 121.34(7) . . . . ? Si2 N2 S1 Li1 128.63(9) . . . . ? Li1 N2 S1 Li1 -64.38(11) 2_676 . . . ? C8 C7 S1 N1 -65.34(10) . . . . ? P1 C7 S1 N1 66.51(8) . . . . ? C8 C7 S1 N2 -174.64(9) . . . . ? P1 C7 S1 N2 -42.78(8) . . . . ? C8 C7 S1 Li1 -117.04(10) . . . . ? P1 C7 S1 Li1 14.81(10) . . . . ? N2 Li1 S1 N1 -89.94(13) 2_676 . . . ? N2 Li1 S1 N1 -166.78(10) . . . . ? Li1 Li1 S1 N1 -123.68(13) 2_676 . . . ? P1 Li1 S1 N1 137.75(17) 2_676 . . . ? N1 Li1 S1 N2 166.78(10) . . . . ? N2 Li1 S1 N2 76.84(12) 2_676 . . . ? Li1 Li1 S1 N2 43.10(8) 2_676 . . . ? P1 Li1 S1 N2 -55.47(13) 2_676 . . . ? N1 Li1 S1 C7 83.61(9) . . . . ? N2 Li1 S1 C7 -6.33(15) 2_676 . . . ? N2 Li1 S1 C7 -83.17(8) . . . . ? Li1 Li1 S1 C7 -40.07(12) 2_676 . . . ? P1 Li1 S1 C7 -138.63(12) 2_676 . . . ? S1 N1 Si1 C1 -109.09(8) . . . . ? Li1 N1 Si1 C1 133.86(9) . . . . ? S1 N1 Si1 C3 13.33(10) . . . . ? Li1 N1 Si1 C3 -103.72(10) . . . . ? S1 N1 Si1 C2 132.95(8) . . . . ? Li1 N1 Si1 C2 15.91(10) . . . . ? S1 N2 Si2 C6 -173.50(6) . . . . ? Li1 N2 Si2 C6 20.84(11) 2_676 . . . ? Li1 N2 Si2 C6 -69.99(10) . . . . ? S1 N2 Si2 C4 67.26(9) . . . . ? Li1 N2 Si2 C4 -98.40(11) 2_676 . . . ? Li1 N2 Si2 C4 170.77(10) . . . . ? S1 N2 Si2 C5 -52.79(8) . . . . ? Li1 N2 Si2 C5 141.55(10) 2_676 . . . ? Li1 N2 Si2 C5 50.73(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.686 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.049 #===END data_p21c _database_code_depnum_ccdc_archive 'CCDC 779992' #TrackingRef '- all_full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H56 Li2 N4 P2 S2' _chemical_formula_weight 636.75 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' 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5006(14) _cell_length_b 20.753(3) _cell_length_c 8.5699(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.279(2) _cell_angle_gamma 90.00 _cell_volume 1852.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9881 _cell_measurement_theta_min 2.1875 _cell_measurement_theta_max 26.7055 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.256 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9358 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details SADABS-2008/2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC Mo micro source' _diffrn_radiation_monochromator 'INCOATEC quazar mirror optics' _diffrn_measurement_device_type 'Bruker Smart Apex II with D8-Goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39157 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3784 _reflns_number_gt 3561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex v2.2-0' _computing_cell_refinement 'SAINT V7.46A' _computing_data_reduction 'SAINT V7.46A' _computing_structure_solution 'SHELXS in SHELXTL 2008/2 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL in SHELXTL 2008/2 (Sheldrick, 2008)' _computing_molecular_graphics 'XSHELL v4.01' _computing_publication_material 'XSHELL v4.01' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+1.0430P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3784 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.27778(13) 1.13975(6) 0.73400(16) 0.0207(3) Uani 1 1 d . . . C2 C 1.19028(14) 1.18199(6) 0.65285(16) 0.0232(3) Uani 1 1 d . . . H2 H 1.1095 1.1890 0.6888 0.028 Uiso 1 1 calc R . . C3 C 1.22007(15) 1.21402(7) 0.51954(17) 0.0277(3) Uani 1 1 d . . . H3 H 1.1599 1.2431 0.4657 0.033 Uiso 1 1 calc R . . C4 C 1.33691(16) 1.20375(7) 0.46486(18) 0.0300(3) Uani 1 1 d . . . H4 H 1.3568 1.2255 0.3735 0.036 Uiso 1 1 calc R . . C5 C 1.42436(16) 1.16167(8) 0.5439(2) 0.0335(4) Uani 1 1 d . . . H5 H 1.5046 1.1544 0.5067 0.040 Uiso 1 1 calc R . . C6 C 1.39523(14) 1.12990(7) 0.67786(18) 0.0285(3) Uani 1 1 d . . . H6 H 1.4561 1.1011 0.7317 0.034 Uiso 1 1 calc R . . C7 C 1.37954(14) 1.11254(7) 1.05062(17) 0.0278(3) Uani 1 1 d . . . H7A H 1.4535 1.0935 1.0087 0.042 Uiso 1 1 calc R . . H7B H 1.3690 1.0923 1.1515 0.042 Uiso 1 1 calc R . . H7C H 1.3936 1.1589 1.0662 0.042 Uiso 1 1 calc R . . C8 C 1.25590(14) 1.01463(6) 0.85495(16) 0.0216(3) Uani 1 1 d . . . H8A H 1.1920 1.0044 0.7631 0.026 Uiso 1 1 calc R . . H8B H 1.3423 1.0097 0.8217 0.026 Uiso 1 1 calc R . . C9 C 1.20401(14) 0.84081(7) 0.88319(18) 0.0259(3) Uani 1 1 d . . . C10 C 1.28919(19) 0.80919(8) 1.0215(2) 0.0409(4) Uani 1 1 d . . . H10A H 1.3613 0.8378 1.0572 0.061 Uiso 1 1 calc R . . H10B H 1.3221 0.7680 0.9872 0.061 Uiso 1 1 calc R . . H10C H 1.2384 0.8016 1.1082 0.061 Uiso 1 1 calc R . . C11 C 1.09134(18) 0.79676(9) 0.8283(3) 0.0548(6) Uani 1 1 d . . . H11A H 1.0378 0.7915 0.9132 0.082 Uiso 1 1 calc R . . H11B H 1.1236 0.7546 0.8001 0.082 Uiso 1 1 calc R . . H11C H 1.0400 0.8158 0.7363 0.082 Uiso 1 1 calc R . . C12 C 1.28476(14) 0.85154(7) 0.74880(17) 0.0269(3) Uani 1 1 d . . . H12A H 1.2310 0.8705 0.6586 0.040 Uiso 1 1 calc R . . H12B H 1.3190 0.8102 0.7179 0.040 Uiso 1 1 calc R . . H12C H 1.3559 0.8808 0.7838 0.040 Uiso 1 1 calc R . . C13 C 1.17331(13) 0.98442(7) 1.28929(15) 0.0216(3) Uani 1 1 d . . . C14 C 1.12212(15) 1.04333(7) 1.36803(17) 0.0291(3) Uani 1 1 d . . . H14A H 1.1732 1.0812 1.3478 0.044 Uiso 1 1 calc R . . H14B H 1.1280 1.0360 1.4817 0.044 Uiso 1 1 calc R . . H14C H 1.0323 1.0506 1.3251 0.044 Uiso 1 1 calc R . . C15 C 1.09786(15) 0.92450(7) 1.32738(17) 0.0287(3) Uani 1 1 d . . . H15A H 1.0069 0.9303 1.2878 0.043 Uiso 1 1 calc R . . H15B H 1.1073 0.9181 1.4416 0.043 Uiso 1 1 calc R . . H15C H 1.1312 0.8867 1.2772 0.043 Uiso 1 1 calc R . . C16 C 1.31428(14) 0.97469(9) 1.35611(17) 0.0323(3) Uani 1 1 d . . . H16A H 1.3462 0.9348 1.3140 0.049 Uiso 1 1 calc R . . H16B H 1.3217 0.9719 1.4711 0.049 Uiso 1 1 calc R . . H16C H 1.3652 1.0112 1.3261 0.049 Uiso 1 1 calc R . . Li1 Li 0.9759(2) 0.93383(12) 0.9684(3) 0.0255(5) Uani 1 1 d . . . N1 N 1.14402(11) 0.90132(5) 0.92972(14) 0.0214(2) Uani 1 1 d . . . N2 N 1.15211(11) 0.99907(5) 1.11692(12) 0.0189(2) Uani 1 1 d . . . P1 P 1.23442(3) 1.099420(16) 0.91135(4) 0.01870(10) Uani 1 1 d . . . S1 S 1.23887(3) 0.955929(15) 1.01187(4) 0.01720(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0243(7) 0.0171(6) 0.0210(6) -0.0014(5) 0.0038(5) -0.0027(5) C2 0.0248(7) 0.0200(6) 0.0248(7) -0.0026(5) 0.0034(5) -0.0002(5) C3 0.0337(8) 0.0218(7) 0.0269(7) 0.0035(6) 0.0012(6) 0.0016(6) C4 0.0415(9) 0.0236(7) 0.0264(7) 0.0054(6) 0.0096(6) -0.0019(6) C5 0.0320(8) 0.0325(8) 0.0389(9) 0.0073(7) 0.0159(7) 0.0026(6) C6 0.0262(7) 0.0271(7) 0.0331(8) 0.0076(6) 0.0072(6) 0.0043(6) C7 0.0278(7) 0.0286(7) 0.0258(7) 0.0011(6) -0.0012(6) -0.0055(6) C8 0.0284(7) 0.0183(6) 0.0193(6) -0.0003(5) 0.0076(5) -0.0006(5) C9 0.0263(7) 0.0168(6) 0.0371(8) -0.0046(6) 0.0140(6) -0.0009(5) C10 0.0573(11) 0.0255(8) 0.0447(10) 0.0134(7) 0.0256(8) 0.0159(7) C11 0.0378(10) 0.0320(9) 0.1006(17) -0.0338(10) 0.0323(10) -0.0138(8) C12 0.0288(7) 0.0279(7) 0.0250(7) -0.0068(6) 0.0077(6) 0.0014(6) C13 0.0214(7) 0.0276(7) 0.0156(6) 0.0013(5) 0.0023(5) 0.0021(5) C14 0.0342(8) 0.0342(8) 0.0191(7) -0.0050(6) 0.0035(6) 0.0036(6) C15 0.0328(8) 0.0328(8) 0.0210(7) 0.0053(6) 0.0054(6) -0.0004(6) C16 0.0244(7) 0.0500(10) 0.0220(7) 0.0070(7) 0.0004(6) 0.0044(7) Li1 0.0224(12) 0.0262(12) 0.0290(12) 0.0018(10) 0.0077(10) 0.0038(9) N1 0.0189(5) 0.0174(5) 0.0288(6) -0.0039(5) 0.0064(5) -0.0005(4) N2 0.0207(5) 0.0213(5) 0.0151(5) 0.0002(4) 0.0045(4) 0.0045(4) P1 0.01849(17) 0.01830(17) 0.01964(17) -0.00002(12) 0.00378(13) 0.00069(12) S1 0.01686(16) 0.01713(16) 0.01807(16) 0.00024(11) 0.00401(12) 0.00148(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 C1 C2 1.3908(19) . ? C1 C6 1.394(2) . ? C1 P1 1.8421(14) . ? C2 C3 1.391(2) . ? C2 H2 0.9500 . ? C3 C4 1.384(2) . ? C3 H3 0.9500 . ? C4 C5 1.381(2) . ? C4 H4 0.9500 . ? C5 C6 1.391(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 P1 1.8330(15) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 S1 1.8398(13) . ? C8 P1 1.8463(14) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N1 1.4820(17) . ? C9 C11 1.522(2) . ? C9 C12 1.530(2) . ? C9 C10 1.539(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N2 1.4969(16) . ? C13 C14 1.5266(19) . ? C13 C16 1.5314(19) . ? C13 C15 1.532(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? Li1 N1 1.957(3) . ? Li1 N2 2.506(3) . ? N1 S1 1.6107(11) . ? N2 S1 1.6278(11) . ? P1 Li1 2.644(2) 3_777 ? 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 C2 C1 C6 118.49(13) . . ? C2 C1 P1 118.83(10) . . ? C6 C1 P1 122.67(11) . . ? C1 C2 C3 120.58(13) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 120.37(14) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.62(14) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.16(14) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.78(14) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? P1 C7 H7A 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S1 C8 P1 114.41(7) . . ? S1 C8 H8A 108.7 . . ? P1 C8 H8A 108.7 . . ? S1 C8 H8B 108.7 . . ? P1 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N1 C9 C11 104.59(12) . . ? N1 C9 C12 111.97(12) . . ? C11 C9 C12 109.75(14) . . ? N1 C9 C10 112.31(12) . . ? C11 C9 C10 109.58(15) . . ? C12 C9 C10 108.56(12) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 104.89(11) . . ? N2 C13 C16 114.31(11) . . ? C14 C13 C16 108.55(12) . . ? N2 C13 C15 111.03(11) . . ? C14 C13 C15 109.60(12) . . ? C16 C13 C15 108.35(12) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 Li1 N2 138.96(14) . 3_777 ? N1 Li1 N2 69.41(8) . . ? N2 Li1 N2 103.14(11) 3_777 . ? N1 Li1 P1 142.36(12) . 3_777 ? N2 Li1 P1 76.66(8) 3_777 3_777 ? N2 Li1 P1 122.84(10) . 3_777 ? N1 Li1 Li1 102.92(14) . 3_777 ? N2 Li1 Li1 59.49(9) 3_777 3_777 ? N2 Li1 Li1 43.65(8) . 3_777 ? P1 Li1 Li1 108.43(12) 3_777 3_777 ? C9 N1 S1 116.96(9) . . ? C9 N1 Li1 139.55(12) . . ? S1 N1 Li1 101.81(9) . . ? C13 N2 S1 114.23(9) . . ? C13 N2 Li1 120.60(11) . 3_777 ? S1 N2 Li1 125.16(9) . 3_777 ? C13 N2 Li1 113.55(10) . . ? S1 N2 Li1 81.42(7) . . ? Li1 N2 Li1 76.86(11) 3_777 . ? C7 P1 C1 101.41(7) . . ? C7 P1 C8 101.13(7) . . ? C1 P1 C8 99.55(6) . . ? C7 P1 Li1 116.83(7) . 3_777 ? C1 P1 Li1 138.25(7) . 3_777 ? C8 P1 Li1 89.37(7) . 3_777 ? N1 S1 N2 105.68(6) . . ? N1 S1 C8 104.97(6) . . ? N2 S1 C8 98.81(6) . . ? N2 S1 Li1 63.16(7) . . ? C8 S1 Li1 101.44(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.6(2) . . . . ? P1 C1 C2 C3 179.18(11) . . . . ? C1 C2 C3 C4 0.7(2) . . . . ? C2 C3 C4 C5 -0.3(2) . . . . ? C3 C4 C5 C6 -0.1(2) . . . . ? C4 C5 C6 C1 0.2(2) . . . . ? C2 C1 C6 C5 0.1(2) . . . . ? P1 C1 C6 C5 -179.61(12) . . . . ? C11 C9 N1 S1 173.54(12) . . . . ? C12 C9 N1 S1 -67.68(15) . . . . ? C10 C9 N1 S1 54.77(15) . . . . ? C11 C9 N1 Li1 11.6(2) . . . . ? C12 C9 N1 Li1 130.43(17) . . . . ? C10 C9 N1 Li1 -107.12(19) . . . . ? N2 Li1 N1 C9 -118.6(2) 3_777 . . . ? N2 Li1 N1 C9 154.98(17) . . . . ? P1 Li1 N1 C9 37.5(3) 3_777 . . . ? S1 Li1 N1 C9 163.6(2) . . . . ? Li1 Li1 N1 C9 -176.56(15) 3_777 . . . ? N2 Li1 N1 S1 77.9(2) 3_777 . . . ? N2 Li1 N1 S1 -8.58(7) . . . . ? P1 Li1 N1 S1 -126.06(18) 3_777 . . . ? Li1 Li1 N1 S1 19.88(14) 3_777 . . . ? C14 C13 N2 S1 160.84(9) . . . . ? C16 C13 N2 S1 42.07(15) . . . . ? C15 C13 N2 S1 -80.87(13) . . . . ? C14 C13 N2 Li1 -19.88(16) . . . 3_777 ? C16 C13 N2 Li1 -138.65(14) . . . 3_777 ? C15 C13 N2 Li1 98.42(15) . . . 3_777 ? C14 C13 N2 Li1 -108.14(12) . . . . ? C16 C13 N2 Li1 133.09(12) . . . . ? C15 C13 N2 Li1 10.16(14) . . . . ? N1 Li1 N2 C13 -104.37(11) . . . . ? N2 Li1 N2 C13 117.93(12) 3_777 . . . ? P1 Li1 N2 C13 35.48(15) 3_777 . . . ? S1 Li1 N2 C13 -112.77(10) . . . . ? Li1 Li1 N2 C13 117.93(12) 3_777 . . . ? N1 Li1 N2 S1 8.41(7) . . . . ? N2 Li1 N2 S1 -129.30(10) 3_777 . . . ? P1 Li1 N2 S1 148.25(11) 3_777 . . . ? Li1 Li1 N2 S1 -129.29(10) 3_777 . . . ? N1 Li1 N2 Li1 137.70(14) . . . 3_777 ? N2 Li1 N2 Li1 0.0 3_777 . . 3_777 ? P1 Li1 N2 Li1 -82.45(12) 3_777 . . 3_777 ? S1 Li1 N2 Li1 129.29(10) . . . 3_777 ? C2 C1 P1 C7 -132.36(11) . . . . ? C6 C1 P1 C7 47.36(14) . . . . ? C2 C1 P1 C8 124.13(11) . . . . ? C6 C1 P1 C8 -56.15(13) . . . . ? C2 C1 P1 Li1 24.23(16) . . . 3_777 ? C6 C1 P1 Li1 -156.05(13) . . . 3_777 ? S1 C8 P1 C7 69.86(9) . . . . ? S1 C8 P1 C1 173.60(8) . . . . ? S1 C8 P1 Li1 -47.39(9) . . . 3_777 ? C9 N1 S1 N2 -155.20(10) . . . . ? Li1 N1 S1 N2 12.91(10) . . . . ? C9 N1 S1 C8 100.93(11) . . . . ? Li1 N1 S1 C8 -90.96(10) . . . . ? C9 N1 S1 Li1 -168.11(15) . . . . ? C13 N2 S1 N1 102.10(10) . . . . ? Li1 N2 S1 N1 -77.15(12) 3_777 . . . ? Li1 N2 S1 N1 -9.94(8) . . . . ? C13 N2 S1 C8 -149.54(10) . . . . ? Li1 N2 S1 C8 31.22(12) 3_777 . . . ? Li1 N2 S1 C8 98.42(8) . . . . ? C13 N2 S1 Li1 112.04(11) . . . . ? Li1 N2 S1 Li1 -67.20(14) 3_777 . . . ? P1 C8 S1 N1 132.03(8) . . . . ? P1 C8 S1 N2 23.10(9) . . . . ? P1 C8 S1 Li1 87.32(9) . . . . ? N2 Li1 S1 N1 -130.15(17) 3_777 . . . ? N2 Li1 S1 N1 166.05(11) . . . . ? P1 Li1 S1 N1 107.3(2) 3_777 . . . ? Li1 Li1 S1 N1 -159.39(15) 3_777 . . . ? N1 Li1 S1 N2 -166.05(11) . . . . ? N2 Li1 S1 N2 63.80(13) 3_777 . . . ? P1 Li1 S1 N2 -58.77(18) 3_777 . . . ? Li1 Li1 S1 N2 34.56(8) 3_777 . . . ? N1 Li1 S1 C8 99.78(9) . . . . ? N2 Li1 S1 C8 -30.37(14) 3_777 . . . ? N2 Li1 S1 C8 -94.17(7) . . . . ? P1 Li1 S1 C8 -152.94(18) 3_777 . . . ? Li1 Li1 S1 C8 -59.61(10) 3_777 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.409 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.042 #===END data_c2c2 _database_code_depnum_ccdc_archive 'CCDC 779993' #TrackingRef '- all_full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27.50 H52 Li N4 P S Si2' _chemical_formula_sum 'C27.50 H52 Li N4 P S Si2' _chemical_formula_weight 564.88 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' Si Si 0.0817 0.0704 '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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.944(5) _cell_length_b 9.5352(13) _cell_length_c 21.921(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.895(3) _cell_angle_gamma 90.00 _cell_volume 6942.4(17) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8986 _cell_measurement_theta_min 2.222 _cell_measurement_theta_max 26.577 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 0.229 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8424 _exptl_absorpt_correction_T_max 0.9422 _exptl_absorpt_process_details 'SADABS 2008-2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC Mo micro source' _diffrn_radiation_monochromator 'INCOATEC quazar mirror optics' _diffrn_measurement_device_type 'Bruker Smart Apex II with D8 goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48696 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.02 _reflns_number_total 6847 _reflns_number_gt 5585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX v2009.11-0' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.68A' _computing_structure_solution 'SHELXS in SHELXTL v2008/4' _computing_structure_refinement 'SHELXL in SHELXTL v2008/4' _computing_molecular_graphics 'XSHELL v4.01' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+8.9902P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6847 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.24073(5) 0.07867(17) 0.14903(8) 0.0236(4) Uani 1 1 d . . . C2 C 0.27884(6) 0.07876(18) 0.18742(9) 0.0258(4) Uani 1 1 d . . . H2 H 0.2814 0.0772 0.2314 0.031 Uiso 1 1 calc R . . C3 C 0.31315(6) 0.0811(2) 0.16218(9) 0.0311(4) Uani 1 1 d . . . H3 H 0.3390 0.0808 0.1890 0.037 Uiso 1 1 calc R . . C4 C 0.30998(6) 0.0840(2) 0.09819(10) 0.0339(5) Uani 1 1 d . . . H4 H 0.3335 0.0848 0.0811 0.041 Uiso 1 1 calc R . . C5 C 0.27224(6) 0.0858(2) 0.05926(9) 0.0328(4) Uani 1 1 d . . . H5 H 0.2699 0.0887 0.0153 0.039 Uiso 1 1 calc R . . C6 C 0.23789(6) 0.08328(19) 0.08431(9) 0.0285(4) Uani 1 1 d . . . H6 H 0.2121 0.0847 0.0573 0.034 Uiso 1 1 calc R . . C7 C 0.21076(5) 0.07708(18) 0.26137(8) 0.0225(4) Uani 1 1 d . . . C8 C 0.22180(6) -0.04482(19) 0.29545(9) 0.0266(4) Uani 1 1 d . . . H8 H 0.2204 -0.1324 0.2744 0.032 Uiso 1 1 calc R . . C9 C 0.23481(6) -0.0402(2) 0.35965(9) 0.0297(4) Uani 1 1 d . . . H9 H 0.2417 -0.1247 0.3824 0.036 Uiso 1 1 calc R . . C10 C 0.23781(6) 0.0868(2) 0.39075(9) 0.0300(4) Uani 1 1 d . . . H10 H 0.2471 0.0898 0.4347 0.036 Uiso 1 1 calc R . . C11 C 0.22720(6) 0.2090(2) 0.35782(9) 0.0307(4) Uani 1 1 d . . . H11 H 0.2292 0.2965 0.3790 0.037 Uiso 1 1 calc R . . C12 C 0.21361(6) 0.20377(19) 0.29367(9) 0.0280(4) Uani 1 1 d . . . H12 H 0.2061 0.2883 0.2713 0.034 Uiso 1 1 calc R . . C13 C 0.17306(5) -0.09170(18) 0.15545(9) 0.0250(4) Uani 1 1 d . A . H13A H 0.1904 -0.1409 0.1311 0.030 Uiso 1 1 calc R . . H13B H 0.1728 -0.1467 0.1937 0.030 Uiso 1 1 calc R . . C14 C 0.13961(8) 0.0719(2) -0.07339(10) 0.0450(6) Uani 1 1 d . A . H14A H 0.1180 0.1417 -0.0809 0.067 Uiso 1 1 calc R . . H14B H 0.1416 0.0271 -0.1129 0.067 Uiso 1 1 calc R . . H14C H 0.1652 0.1181 -0.0556 0.067 Uiso 1 1 calc R . . C15 C 0.07926(7) -0.1490(3) -0.05210(11) 0.0455(6) Uani 1 1 d . A . H15A H 0.0728 -0.2184 -0.0227 0.068 Uiso 1 1 calc R . . H15B H 0.0812 -0.1957 -0.0912 0.068 Uiso 1 1 calc R . . H15C H 0.0580 -0.0777 -0.0603 0.068 Uiso 1 1 calc R . . C16 C 0.16760(7) -0.2052(2) -0.01000(10) 0.0376(5) Uani 1 1 d . A . H16A H 0.1943 -0.1645 0.0053 0.056 Uiso 1 1 calc R . . H16B H 0.1667 -0.2491 -0.0507 0.056 Uiso 1 1 calc R . . H16C H 0.1622 -0.2761 0.0196 0.056 Uiso 1 1 calc R . . C17 C 0.02481(7) -0.1142(3) 0.16227(13) 0.0554(7) Uani 1 1 d . A . H17A H 0.0082 -0.0421 0.1374 0.083 Uiso 1 1 calc R . . H17B H 0.0107 -0.1507 0.1937 0.083 Uiso 1 1 calc R . . H17C H 0.0297 -0.1909 0.1350 0.083 Uiso 1 1 calc R . . C18 C 0.06433(10) 0.1126(3) 0.25191(13) 0.0649(8) Uani 1 1 d . A . H18A H 0.0900 0.1545 0.2725 0.097 Uiso 1 1 calc R . . H18B H 0.0500 0.0781 0.2835 0.097 Uiso 1 1 calc R . . H18C H 0.0478 0.1835 0.2260 0.097 Uiso 1 1 calc R . . C19 C 0.10152(7) -0.1766(2) 0.25349(10) 0.0426(5) Uani 1 1 d . A . H19A H 0.1054 -0.2581 0.2282 0.064 Uiso 1 1 calc R . . H19B H 0.0857 -0.2043 0.2843 0.064 Uiso 1 1 calc R . . H19C H 0.1278 -0.1409 0.2751 0.064 Uiso 1 1 calc R . . C20 C 0.15243(11) 0.4675(3) 0.15703(16) 0.0439(7) Uani 0.6738(17) 1 d P A 1 H20A H 0.1607 0.5613 0.1464 0.066 Uiso 0.6738(17) 1 calc PR A 1 H20B H 0.1764 0.4096 0.1716 0.066 Uiso 0.6738(17) 1 calc PR A 1 H20C H 0.1369 0.4747 0.1900 0.066 Uiso 0.6738(17) 1 calc PR A 1 C21 C 0.15672(10) 0.3886(3) 0.05547(16) 0.0385(7) Uani 0.6738(17) 1 d P A 1 H21A H 0.1663 0.4810 0.0454 0.058 Uiso 0.6738(17) 1 calc PR A 1 H21B H 0.1414 0.3450 0.0174 0.058 Uiso 0.6738(17) 1 calc PR A 1 H21C H 0.1798 0.3292 0.0733 0.058 Uiso 0.6738(17) 1 calc PR A 1 C22 C 0.0954(6) 0.4928(19) 0.0760(8) 0.0393(13) Uani 0.6738(17) 1 d P A 1 H22A H 0.1059 0.5772 0.0585 0.047 Uiso 0.6738(17) 1 calc PR A 1 H22B H 0.0810 0.5243 0.1086 0.047 Uiso 0.6738(17) 1 calc PR A 1 C23 C 0.06512(10) 0.4190(3) 0.02385(17) 0.0411(7) Uani 0.6738(17) 1 d P A 1 H23A H 0.0406 0.4775 0.0120 0.049 Uiso 0.6738(17) 1 calc PR A 1 H23B H 0.0772 0.4084 -0.0133 0.049 Uiso 0.6738(17) 1 calc PR A 1 C24 C 0.02877(10) 0.3026(4) 0.09308(17) 0.0452(7) Uani 0.6738(17) 1 d P A 1 H24A H 0.0445 0.3518 0.1293 0.068 Uiso 0.6738(17) 1 calc PR A 1 H24B H 0.0210 0.2099 0.1059 0.068 Uiso 0.6738(17) 1 calc PR A 1 H24C H 0.0045 0.3569 0.0758 0.068 Uiso 0.6738(17) 1 calc PR A 1 C25 C 0.03075(11) 0.2008(4) -0.00512(19) 0.0517(8) Uani 0.6738(17) 1 d P A 1 H25A H 0.0050 0.2473 -0.0213 0.078 Uiso 0.6738(17) 1 calc PR A 1 H25B H 0.0258 0.1090 0.0120 0.078 Uiso 0.6738(17) 1 calc PR A 1 H25C H 0.0453 0.1882 -0.0389 0.078 Uiso 0.6738(17) 1 calc PR A 1 C26 C 1.0343(3) 0.4781(9) 0.3229(6) 0.073(3) Uani 0.50 1 d P B -1 H26A H 1.0220 0.5450 0.3474 0.109 Uiso 0.50 1 calc PR B -1 H26B H 1.0637 0.4866 0.3342 0.109 Uiso 0.50 1 calc PR B -1 H26C H 1.0264 0.3826 0.3317 0.109 Uiso 0.50 1 calc PR B -1 C27 C 1.0195(8) 0.510(2) 0.2513(13) 0.077(5) Uani 0.50 1 d P B -1 H27A H 1.0295 0.6040 0.2421 0.092 Uiso 0.50 1 calc PR B -1 H27B H 1.0313 0.4404 0.2269 0.092 Uiso 0.50 1 calc PR B -1 C28 C 0.9752(7) 0.507(2) 0.2314(11) 0.082(6) Uani 0.50 1 d P B -1 H28A H 0.9665 0.4139 0.2431 0.098 Uiso 0.50 1 calc PR B -1 H28B H 0.9648 0.5762 0.2580 0.098 Uiso 0.50 1 calc PR B -1 C29 C 0.9543(4) 0.5325(11) 0.1697(7) 0.106(5) Uani 0.50 1 d P B -1 H29A H 0.9533 0.6350 0.1623 0.127 Uiso 0.50 1 calc PR B -1 H29B H 0.9699 0.4904 0.1407 0.127 Uiso 0.50 1 calc PR B -1 C30 C 0.92029(19) 0.4872(7) 0.1569(3) 0.0664(16) Uani 0.50 1 d P B -1 H30A H 0.9162 0.4208 0.1891 0.100 Uiso 0.50 1 calc PR B -1 H30B H 0.9160 0.4394 0.1165 0.100 Uiso 0.50 1 calc PR B -1 H30C H 0.9011 0.5649 0.1547 0.100 Uiso 0.50 1 calc PR B -1 C20' C 0.1219(2) 0.4120(7) 0.1806(3) 0.0439(7) Uani 0.3262(17) 1 d P A 2 H20D H 0.1424 0.3536 0.2070 0.066 Uiso 0.3262(17) 1 calc PR A 2 H20E H 0.0951 0.3767 0.1823 0.066 Uiso 0.3262(17) 1 calc PR A 2 H20F H 0.1246 0.5091 0.1956 0.066 Uiso 0.3262(17) 1 calc PR A 2 C21' C 0.16672(19) 0.4552(7) 0.1113(3) 0.0385(7) Uani 0.3262(17) 1 d P A 2 H21D H 0.1743 0.4590 0.0705 0.058 Uiso 0.3262(17) 1 calc PR A 2 H21E H 0.1852 0.3926 0.1390 0.058 Uiso 0.3262(17) 1 calc PR A 2 H21F H 0.1683 0.5494 0.1294 0.058 Uiso 0.3262(17) 1 calc PR A 2 C22' C 0.0961(13) 0.502(4) 0.0705(18) 0.0393(13) Uani 0.3262(17) 1 d P A 2 H22C H 0.1012 0.5249 0.0288 0.047 Uiso 0.3262(17) 1 calc PR A 2 H22D H 0.0961 0.5904 0.0941 0.047 Uiso 0.3262(17) 1 calc PR A 2 C23' C 0.0553(2) 0.4297(7) 0.0637(4) 0.0411(7) Uani 0.3262(17) 1 d P A 2 H23C H 0.0471 0.4329 0.1044 0.049 Uiso 0.3262(17) 1 calc PR A 2 H23D H 0.0352 0.4836 0.0336 0.049 Uiso 0.3262(17) 1 calc PR A 2 C24' C 0.0197(2) 0.2116(8) 0.0391(4) 0.0452(7) Uani 0.3262(17) 1 d P A 2 H24D H 0.0139 0.2000 0.0808 0.068 Uiso 0.3262(17) 1 calc PR A 2 H24E H 0.0226 0.1192 0.0210 0.068 Uiso 0.3262(17) 1 calc PR A 2 H24F H -0.0025 0.2623 0.0125 0.068 Uiso 0.3262(17) 1 calc PR A 2 C25' C 0.0611(2) 0.2966(8) -0.0283(4) 0.0517(8) Uani 0.3262(17) 1 d P A 2 H25D H 0.0618 0.2021 -0.0457 0.078 Uiso 0.3262(17) 1 calc PR A 2 H25E H 0.0866 0.3444 -0.0286 0.078 Uiso 0.3262(17) 1 calc PR A 2 H25F H 0.0389 0.3497 -0.0536 0.078 Uiso 0.3262(17) 1 calc PR A 2 Li1 Li 0.10830(10) 0.1921(3) 0.09366(15) 0.0298(7) Uani 1 1 d . . . N1 N 0.12818(5) 0.01923(16) 0.05141(7) 0.0255(3) Uani 1 1 d . A . N2 N 0.10107(5) 0.02854(16) 0.15029(7) 0.0265(3) Uani 1 1 d . A . N3 N 0.12863(5) 0.40593(17) 0.10435(9) 0.0409(5) Uani 0.6738(17) 1 d P A 1 N4 N 0.05440(5) 0.28564(18) 0.04317(9) 0.0375(4) Uani 0.6738(17) 1 d P A 1 N3' N 0.12863(5) 0.40593(17) 0.10435(9) 0.0409(5) Uani 0.3262(17) 1 d P A 2 N4' N 0.05440(5) 0.28564(18) 0.04317(9) 0.0375(4) Uani 0.3262(17) 1 d P A 2 P1 P 0.193114(14) 0.08678(5) 0.17655(2) 0.02304(11) Uani 1 1 d . . . S1 S 0.121732(13) -0.07618(5) 0.10898(2) 0.02309(11) Uani 1 1 d . . . Si1 Si 0.128483(17) -0.06352(6) -0.01796(2) 0.02873(13) Uani 1 1 d . . . Si2 Si 0.074021(17) -0.03611(6) 0.20186(3) 0.03209(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0307(9) 0.0138(8) 0.0252(9) 0.0011(7) 0.0034(7) -0.0033(7) C2 0.0315(10) 0.0194(9) 0.0254(9) 0.0001(7) 0.0030(8) -0.0046(8) C3 0.0313(10) 0.0252(10) 0.0360(11) -0.0032(8) 0.0051(8) -0.0082(8) C4 0.0391(11) 0.0274(10) 0.0387(11) -0.0036(9) 0.0158(9) -0.0098(9) C5 0.0473(12) 0.0267(10) 0.0262(10) -0.0020(8) 0.0116(9) -0.0081(9) C6 0.0369(10) 0.0207(9) 0.0262(9) -0.0007(7) 0.0025(8) -0.0055(8) C7 0.0216(8) 0.0215(9) 0.0244(9) 0.0010(7) 0.0051(7) 0.0000(7) C8 0.0305(10) 0.0200(9) 0.0288(10) -0.0001(7) 0.0051(8) 0.0013(7) C9 0.0358(10) 0.0235(9) 0.0285(10) 0.0065(8) 0.0042(8) 0.0027(8) C10 0.0348(10) 0.0322(10) 0.0231(9) 0.0015(8) 0.0061(8) 0.0002(9) C11 0.0414(11) 0.0231(10) 0.0289(10) -0.0037(8) 0.0106(9) -0.0001(8) C12 0.0367(10) 0.0192(9) 0.0279(10) 0.0037(7) 0.0065(8) 0.0013(8) C13 0.0263(9) 0.0192(9) 0.0274(9) 0.0012(7) 0.0005(7) -0.0006(7) C14 0.0660(16) 0.0399(12) 0.0298(11) 0.0062(9) 0.0118(11) -0.0016(11) C15 0.0480(13) 0.0483(14) 0.0362(12) -0.0090(10) -0.0010(10) -0.0090(11) C16 0.0495(13) 0.0308(11) 0.0370(12) -0.0029(9) 0.0190(10) 0.0001(9) C17 0.0341(12) 0.0681(17) 0.0617(16) 0.0198(13) 0.0047(11) -0.0099(12) C18 0.089(2) 0.0551(16) 0.0640(18) -0.0058(13) 0.0475(16) 0.0005(15) C19 0.0460(13) 0.0501(14) 0.0306(11) 0.0087(10) 0.0053(10) -0.0073(11) C20 0.0471(17) 0.0306(15) 0.0468(18) -0.0065(13) -0.0065(14) 0.0030(13) C21 0.0355(15) 0.0308(15) 0.0500(17) 0.0105(12) 0.0109(13) -0.0017(12) C22 0.0338(13) 0.020(2) 0.059(3) 0.009(2) -0.0038(19) 0.0035(15) C23 0.0306(15) 0.0409(16) 0.0462(19) 0.0151(16) -0.0047(14) 0.0048(13) C24 0.0308(15) 0.0515(19) 0.0526(19) 0.0052(15) 0.0067(14) 0.0015(14) C25 0.0368(16) 0.054(2) 0.057(2) -0.0137(16) -0.0071(15) 0.0004(15) C26 0.059(5) 0.057(5) 0.111(8) 0.016(6) 0.040(5) 0.013(4) C27 0.108(9) 0.038(5) 0.081(10) 0.012(5) 0.013(8) -0.002(4) C28 0.090(10) 0.061(7) 0.105(17) 0.003(8) 0.044(12) -0.018(6) C29 0.090(8) 0.083(8) 0.138(10) -0.046(7) 0.010(7) 0.028(6) C30 0.057(4) 0.055(3) 0.091(5) -0.014(3) 0.024(3) 0.005(3) C20' 0.0471(17) 0.0306(15) 0.0468(18) -0.0065(13) -0.0065(14) 0.0030(13) C21' 0.0355(15) 0.0308(15) 0.0500(17) 0.0105(12) 0.0109(13) -0.0017(12) C22' 0.0338(13) 0.020(2) 0.059(3) 0.009(2) -0.0038(19) 0.0035(15) C23' 0.0306(15) 0.0409(16) 0.0462(19) 0.0151(16) -0.0047(14) 0.0048(13) C24' 0.0308(15) 0.0515(19) 0.0526(19) 0.0052(15) 0.0067(14) 0.0015(14) C25' 0.0368(16) 0.054(2) 0.057(2) -0.0137(16) -0.0071(15) 0.0004(15) Li1 0.0293(16) 0.0256(16) 0.0329(17) -0.0016(13) 0.0023(14) 0.0007(13) N1 0.0295(8) 0.0222(8) 0.0236(8) 0.0008(6) 0.0029(6) -0.0011(6) N2 0.0277(8) 0.0251(8) 0.0267(8) 0.0000(6) 0.0053(7) 0.0012(6) N3 0.0292(9) 0.0218(8) 0.0629(12) 0.0050(8) -0.0110(8) 0.0001(7) N4 0.0283(9) 0.0311(9) 0.0477(11) -0.0023(8) -0.0050(8) 0.0000(7) N3' 0.0292(9) 0.0218(8) 0.0629(12) 0.0050(8) -0.0110(8) 0.0001(7) N4' 0.0283(9) 0.0311(9) 0.0477(11) -0.0023(8) -0.0050(8) 0.0000(7) P1 0.0269(2) 0.0170(2) 0.0236(2) 0.00150(18) 0.00126(18) 0.00052(18) S1 0.0242(2) 0.0210(2) 0.0227(2) 0.00016(17) 0.00156(17) -0.00116(17) Si1 0.0372(3) 0.0259(3) 0.0225(3) -0.0010(2) 0.0048(2) -0.0037(2) Si2 0.0317(3) 0.0348(3) 0.0313(3) 0.0010(2) 0.0100(2) -0.0023(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.390(3) . ? C1 C6 1.403(3) . ? C1 P1 1.8398(19) . ? C2 C3 1.389(3) . ? C2 H2 0.9500 . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.386(3) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.391(2) . ? C7 C12 1.393(2) . ? C7 P1 1.8344(18) . ? C8 C9 1.386(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 C11 1.379(3) . ? C10 H10 0.9500 . ? C11 C12 1.387(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 S1 1.8338(18) . ? C13 P1 1.8557(18) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 Si1 1.864(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.871(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si1 1.877(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.871(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 Si2 1.863(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 Si2 1.874(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N3 1.395(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N3 1.583(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.43(2) . ? C22 C23 1.541(18) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N4 1.411(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N4 1.540(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N4 1.439(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.58(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.478(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.41(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.211(13) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C20' H20D 0.9800 . ? C20' H20E 0.9800 . ? C20' H20F 0.9800 . ? C21' H21D 0.9800 . ? C21' H21E 0.9800 . ? C21' H21F 0.9800 . ? C22' C23' 1.52(4) . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? C23' H23C 0.9900 . ? C23' H23D 0.9900 . ? C24' H24D 0.9800 . ? C24' H24E 0.9800 . ? C24' H24F 0.9800 . ? C25' H25D 0.9800 . ? C25' H25E 0.9800 . ? C25' H25F 0.9800 . ? Li1 N2 2.039(4) . ? Li1 N1 2.071(4) . ? Li1 N4 2.129(4) . ? Li1 N3 2.150(4) . ? N1 S1 1.6070(15) . ? N1 Si1 1.7150(16) . ? N2 S1 1.6032(16) . ? N2 Si2 1.7114(16) . ? 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 C2 C1 C6 118.29(17) . . ? C2 C1 P1 124.90(14) . . ? C6 C1 P1 116.63(14) . . ? C3 C2 C1 120.72(17) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.50(18) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.54(19) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 120.12(18) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.82(18) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C8 C7 C12 117.96(16) . . ? C8 C7 P1 125.59(14) . . ? C12 C7 P1 116.45(13) . . ? C9 C8 C7 120.88(17) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 120.24(17) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 119.81(17) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 119.78(17) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C7 121.32(17) . . ? C11 C12 H12 119.3 . . ? C7 C12 H12 119.3 . . ? S1 C13 P1 108.79(9) . . ? S1 C13 H13A 109.9 . . ? P1 C13 H13A 109.9 . . ? S1 C13 H13B 109.9 . . ? P1 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C22 C23 113.7(11) . . ? N3 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? N3 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? N4 C23 C22 111.3(7) . . ? N4 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? N4 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C28 C27 C26 112.7(14) . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C29 C28 C27 124.0(11) . . ? C29 C28 H28A 106.3 . . ? C27 C28 H28A 106.3 . . ? C29 C28 H28B 106.3 . . ? C27 C28 H28B 106.3 . . ? H28A C28 H28B 106.4 . . ? C30 C29 C28 115.3(15) . . ? C30 C29 H29A 108.4 . . ? C28 C29 H29A 108.4 . . ? C30 C29 H29B 108.4 . . ? C28 C29 H29B 108.4 . . ? H29A C29 H29B 107.5 . . ? H20D C20' H20E 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? H21D C21' H21E 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? C23' C22' H22C 109.8 . . ? C23' C22' H22D 109.8 . . ? H22C C22' H22D 108.2 . . ? C22' C23' H23C 108.5 . . ? C22' C23' H23D 108.5 . . ? H23C C23' H23D 107.5 . . ? H24D C24' H24E 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? H25D C25' H25E 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? N2 Li1 N1 75.80(12) . . ? N2 Li1 N4 116.00(16) . . ? N1 Li1 N4 115.16(16) . . ? N2 Li1 N3 137.32(18) . . ? N1 Li1 N3 132.61(18) . . ? N4 Li1 N3 83.19(13) . . ? S1 N1 Si1 117.55(9) . . ? S1 N1 Li1 89.41(12) . . ? Si1 N1 Li1 145.58(13) . . ? S1 N2 Si2 120.36(10) . . ? S1 N2 Li1 90.63(12) . . ? Si2 N2 Li1 145.67(13) . . ? C20 N3 C22 112.7(7) . . ? C20 N3 C21 106.1(2) . . ? C22 N3 C21 107.3(7) . . ? C20 N3 Li1 127.4(2) . . ? C22 N3 Li1 107.1(7) . . ? C21 N3 Li1 92.97(17) . . ? C23 N4 C25 115.2(3) . . ? C23 N4 C24 109.7(2) . . ? C25 N4 C24 105.7(2) . . ? C23 N4 Li1 106.64(18) . . ? C25 N4 Li1 115.9(2) . . ? C24 N4 Li1 103.03(18) . . ? C7 P1 C1 101.82(8) . . ? C7 P1 C13 103.46(8) . . ? C1 P1 C13 100.47(8) . . ? N2 S1 N1 103.72(8) . . ? N2 S1 C13 102.28(8) . . ? N1 S1 C13 102.38(8) . . ? N1 Si1 C14 107.35(9) . . ? N1 Si1 C15 112.77(10) . . ? C14 Si1 C15 108.99(11) . . ? N1 Si1 C16 112.47(9) . . ? C14 Si1 C16 108.95(11) . . ? C15 Si1 C16 106.24(11) . . ? N2 Si2 C18 107.38(10) . . ? N2 Si2 C17 112.73(10) . . ? C18 Si2 C17 109.08(14) . . ? N2 Si2 C19 112.85(9) . . ? C18 Si2 C19 108.36(12) . . ? C17 Si2 C19 106.33(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.0(3) . . . . ? P1 C1 C2 C3 -175.97(14) . . . . ? C1 C2 C3 C4 0.3(3) . . . . ? C2 C3 C4 C5 0.6(3) . . . . ? C3 C4 C5 C6 -0.6(3) . . . . ? C4 C5 C6 C1 -0.1(3) . . . . ? C2 C1 C6 C5 0.9(3) . . . . ? P1 C1 C6 C5 176.32(14) . . . . ? C12 C7 C8 C9 0.7(3) . . . . ? P1 C7 C8 C9 179.91(15) . . . . ? C7 C8 C9 C10 -1.3(3) . . . . ? C8 C9 C10 C11 1.0(3) . . . . ? C9 C10 C11 C12 0.0(3) . . . . ? C10 C11 C12 C7 -0.6(3) . . . . ? C8 C7 C12 C11 0.3(3) . . . . ? P1 C7 C12 C11 -179.00(15) . . . . ? N3 C22 C23 N4 48.3(12) . . . . ? C26 C27 C28 C29 -179.8(12) . . . . ? C27 C28 C29 C30 159(2) . . . . ? N2 Li1 N1 S1 -4.43(9) . . . . ? N4 Li1 N1 S1 -116.81(16) . . . . ? N3 Li1 N1 S1 138.5(2) . . . . ? N2 Li1 N1 Si1 139.01(19) . . . . ? N4 Li1 N1 Si1 26.6(3) . . . . ? N3 Li1 N1 Si1 -78.1(3) . . . . ? N1 Li1 N2 S1 4.44(9) . . . . ? N4 Li1 N2 S1 115.82(16) . . . . ? N3 Li1 N2 S1 -134.6(2) . . . . ? N1 Li1 N2 Si2 -151.38(19) . . . . ? N4 Li1 N2 Si2 -40.0(3) . . . . ? N3 Li1 N2 Si2 69.5(3) . . . . ? C23 C22 N3 C20 -171.4(7) . . . . ? C23 C22 N3 C21 72.2(11) . . . . ? C23 C22 N3 Li1 -26.6(12) . . . . ? N2 Li1 N3 C20 19.8(4) . . . . ? N1 Li1 N3 C20 -100.6(3) . . . . ? N4 Li1 N3 C20 141.2(3) . . . . ? N2 Li1 N3 C22 -118.2(7) . . . . ? N1 Li1 N3 C22 121.4(7) . . . . ? N4 Li1 N3 C22 3.3(7) . . . . ? N2 Li1 N3 C21 132.7(3) . . . . ? N1 Li1 N3 C21 12.3(3) . . . . ? N4 Li1 N3 C21 -105.86(17) . . . . ? C22 C23 N4 C25 -171.6(8) . . . . ? C22 C23 N4 C24 69.3(8) . . . . ? C22 C23 N4 Li1 -41.6(8) . . . . ? N2 Li1 N4 C23 161.6(2) . . . . ? N1 Li1 N4 C23 -112.6(2) . . . . ? N3 Li1 N4 C23 21.6(2) . . . . ? N2 Li1 N4 C25 -68.8(3) . . . . ? N1 Li1 N4 C25 17.1(3) . . . . ? N3 Li1 N4 C25 151.3(2) . . . . ? N2 Li1 N4 C24 46.1(2) . . . . ? N1 Li1 N4 C24 131.9(2) . . . . ? N3 Li1 N4 C24 -93.87(19) . . . . ? C8 C7 P1 C1 -80.18(17) . . . . ? C12 C7 P1 C1 99.08(15) . . . . ? C8 C7 P1 C13 23.76(18) . . . . ? C12 C7 P1 C13 -156.97(14) . . . . ? C2 C1 P1 C7 -5.18(17) . . . . ? C6 C1 P1 C7 179.76(13) . . . . ? C2 C1 P1 C13 -111.48(16) . . . . ? C6 C1 P1 C13 73.47(14) . . . . ? S1 C13 P1 C7 127.97(9) . . . . ? S1 C13 P1 C1 -127.06(10) . . . . ? Si2 N2 S1 N1 158.75(10) . . . . ? Li1 N2 S1 N1 -5.72(12) . . . . ? Si2 N2 S1 C13 -95.05(11) . . . . ? Li1 N2 S1 C13 100.48(11) . . . . ? Si1 N1 S1 N2 -152.05(10) . . . . ? Li1 N1 S1 N2 5.63(12) . . . . ? Si1 N1 S1 C13 101.83(11) . . . . ? Li1 N1 S1 C13 -100.49(11) . . . . ? P1 C13 S1 N2 -49.59(11) . . . . ? P1 C13 S1 N1 57.65(11) . . . . ? S1 N1 Si1 C14 -176.59(11) . . . . ? Li1 N1 Si1 C14 45.6(2) . . . . ? S1 N1 Si1 C15 63.36(13) . . . . ? Li1 N1 Si1 C15 -74.4(2) . . . . ? S1 N1 Si1 C16 -56.76(13) . . . . ? Li1 N1 Si1 C16 165.4(2) . . . . ? S1 N2 Si2 C18 168.33(13) . . . . ? Li1 N2 Si2 C18 -40.0(3) . . . . ? S1 N2 Si2 C17 -71.50(15) . . . . ? Li1 N2 Si2 C17 80.2(2) . . . . ? S1 N2 Si2 C19 48.99(14) . . . . ? Li1 N2 Si2 C19 -159.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.344 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.044 #===END data_p21na _database_code_depnum_ccdc_archive 'CCDC 779994' #TrackingRef '- all_full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H52 Mg N4 P2 S2 Si4' _chemical_formula_weight 587.37 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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2563(5) _cell_length_b 17.8142(8) _cell_length_c 19.2917(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.2730(10) _cell_angle_gamma 90.00 _cell_volume 3478.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9638 _cell_measurement_theta_min 2.9235 _cell_measurement_theta_max 30.119 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8176 _exptl_absorpt_correction_T_max 0.8857 _exptl_absorpt_process_details SADABS-2008/2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS-Mo rotating anode' _diffrn_radiation_monochromator 'INCOATEC Helios mirror optics' _diffrn_measurement_device_type 'Bruker TXS-Mo rotating anode' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 156125 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0072 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 29.13 _reflns_number_total 9326 _reflns_number_gt 8689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.2-0' _computing_cell_refinement 'SAINT V7.46A' _computing_data_reduction 'SAINT V7.46A' _computing_structure_solution 'SHELXS in SHELXTL v2008/4 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL in SHELXTL v2008/4 (Sheldrick, 2008)' _computing_molecular_graphics 'XSHELL v4.01' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.6229P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9326 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.55174(12) 0.05301(7) 0.15089(7) 0.0469(3) Uani 1 1 d . . . H1A H 0.6384 0.0374 0.1758 0.070 Uiso 1 1 calc R . . H1B H 0.5039 0.0090 0.1295 0.070 Uiso 1 1 calc R . . H1C H 0.5012 0.0764 0.1841 0.070 Uiso 1 1 calc R . . C2 C 0.40448(10) 0.14667(6) 0.03437(6) 0.0405(2) Uani 1 1 d . . . H2A H 0.3529 0.1682 0.0681 0.061 Uiso 1 1 calc R . . H2B H 0.3605 0.1013 0.0135 0.061 Uiso 1 1 calc R . . H2C H 0.4114 0.1834 -0.0027 0.061 Uiso 1 1 calc R . . C3 C 0.67192(13) 0.08001(7) 0.01762(8) 0.0510(3) Uani 1 1 d . . . H3A H 0.6755 0.1151 -0.0211 0.076 Uiso 1 1 calc R . . H3B H 0.6301 0.0331 -0.0009 0.076 Uiso 1 1 calc R . . H3C H 0.7618 0.0696 0.0416 0.076 Uiso 1 1 calc R . . C4 C 0.97153(11) 0.30443(9) 0.32816(6) 0.0490(3) Uani 1 1 d . . . H4A H 1.0184 0.2623 0.3106 0.073 Uiso 1 1 calc R . . H4B H 0.9971 0.3082 0.3792 0.073 Uiso 1 1 calc R . . H4C H 0.9946 0.3511 0.3061 0.073 Uiso 1 1 calc R . . C5 C 0.74229(13) 0.20379(7) 0.35344(6) 0.0439(2) Uani 1 1 d . . . H5A H 0.6465 0.1964 0.3421 0.066 Uiso 1 1 calc R . . H5B H 0.7675 0.2109 0.4042 0.066 Uiso 1 1 calc R . . H5C H 0.7876 0.1596 0.3386 0.066 Uiso 1 1 calc R . . C6 C 0.70040(13) 0.37085(7) 0.33575(6) 0.0468(3) Uani 1 1 d . . . H6A H 0.7259 0.4164 0.3129 0.070 Uiso 1 1 calc R . . H6B H 0.7232 0.3763 0.3868 0.070 Uiso 1 1 calc R . . H6C H 0.6050 0.3630 0.3230 0.070 Uiso 1 1 calc R . . C7 C 0.53375(9) 0.32681(6) 0.13889(5) 0.03252(19) Uani 1 1 d . . . H7A H 0.5195 0.3642 0.1749 0.039 Uiso 1 1 calc R . . H7B H 0.4468 0.3130 0.1117 0.039 Uiso 1 1 calc R . . C8 C 0.54262(11) 0.35128(7) -0.00674(6) 0.0403(2) Uani 1 1 d . . . H8A H 0.4518 0.3681 -0.0063 0.060 Uiso 1 1 calc R . . H8B H 0.5425 0.2977 -0.0183 0.060 Uiso 1 1 calc R . . H8C H 0.5808 0.3798 -0.0420 0.060 Uiso 1 1 calc R . . C9 C 0.61499(12) 0.46717(6) 0.09177(7) 0.0425(2) Uani 1 1 d . . . H9A H 0.6570 0.4956 0.0579 0.064 Uiso 1 1 calc R . . H9B H 0.6540 0.4818 0.1396 0.064 Uiso 1 1 calc R . . H9C H 0.5200 0.4778 0.0842 0.064 Uiso 1 1 calc R . . C10 C 1.10769(16) 0.03233(7) 0.11427(7) 0.0529(3) Uani 1 1 d . . . H10A H 1.0254 0.0201 0.0829 0.079 Uiso 1 1 calc R . . H10B H 1.1409 -0.0126 0.1408 0.079 Uiso 1 1 calc R . . H10C H 1.1736 0.0498 0.0864 0.079 Uiso 1 1 calc R . . C11 C 0.95284(13) 0.07306(7) 0.22977(8) 0.0522(3) Uani 1 1 d . . . H11A H 0.9419 0.1105 0.2656 0.078 Uiso 1 1 calc R . . H11B H 0.9838 0.0257 0.2526 0.078 Uiso 1 1 calc R . . H11C H 0.8679 0.0648 0.1993 0.078 Uiso 1 1 calc R . . C12 C 1.23366(13) 0.12980(8) 0.23581(7) 0.0507(3) Uani 1 1 d . . . H12A H 1.2988 0.1482 0.2079 0.076 Uiso 1 1 calc R . . H12B H 1.2675 0.0844 0.2613 0.076 Uiso 1 1 calc R . . H12C H 1.2174 0.1685 0.2695 0.076 Uiso 1 1 calc R . . C13 C 0.97530(11) 0.47737(6) 0.15723(6) 0.0385(2) Uani 1 1 d . . . H13A H 0.9154 0.4868 0.1131 0.058 Uiso 1 1 calc R . . H13B H 1.0189 0.5243 0.1742 0.058 Uiso 1 1 calc R . . H13C H 0.9248 0.4579 0.1924 0.058 Uiso 1 1 calc R . . C14 C 1.19183(11) 0.44243(6) 0.07076(6) 0.0381(2) Uani 1 1 d . . . H14A H 1.2555 0.4045 0.0609 0.057 Uiso 1 1 calc R . . H14B H 1.2386 0.4890 0.0862 0.057 Uiso 1 1 calc R . . H14C H 1.1281 0.4521 0.0281 0.057 Uiso 1 1 calc R . . C15 C 1.23021(11) 0.39622(7) 0.22227(6) 0.0407(2) Uani 1 1 d . . . H15A H 1.1868 0.3923 0.2638 0.061 Uiso 1 1 calc R . . H15B H 1.2890 0.4399 0.2271 0.061 Uiso 1 1 calc R . . H15C H 1.2818 0.3507 0.2180 0.061 Uiso 1 1 calc R . . C16 C 1.07110(9) 0.24072(5) 0.01281(5) 0.02937(18) Uani 1 1 d . . . H16A H 1.0963 0.1899 -0.0010 0.035 Uiso 1 1 calc R . . H16B H 1.1237 0.2780 -0.0089 0.035 Uiso 1 1 calc R . . C17 C 0.86535(12) 0.19627(7) -0.09518(6) 0.0447(3) Uani 1 1 d . . . H17A H 0.7746 0.2029 -0.1196 0.067 Uiso 1 1 calc R . . H17B H 0.8792 0.1437 -0.0809 0.067 Uiso 1 1 calc R . . H17C H 0.9274 0.2100 -0.1267 0.067 Uiso 1 1 calc R . . C18 C 0.89229(12) 0.34899(6) -0.05865(6) 0.0393(2) Uani 1 1 d . . . H18A H 0.9617 0.3510 -0.0881 0.059 Uiso 1 1 calc R . . H18B H 0.9086 0.3878 -0.0223 0.059 Uiso 1 1 calc R . . H18C H 0.8062 0.3577 -0.0878 0.059 Uiso 1 1 calc R . . Mg1 Mg 0.84415(3) 0.259423(15) 0.125479(15) 0.02079(6) Uani 1 1 d . . . N1 N 0.65840(7) 0.20131(4) 0.11403(4) 0.02503(14) Uani 1 1 d . . . N2 N 0.75639(7) 0.27743(5) 0.21678(4) 0.02680(14) Uani 1 1 d . . . N3 N 1.00987(7) 0.18657(4) 0.13298(4) 0.02494(14) Uani 1 1 d . . . N4 N 1.01921(7) 0.32483(4) 0.11849(4) 0.02351(13) Uani 1 1 d . . . P1 P 0.64113(2) 0.366561(13) 0.079863(12) 0.02736(5) Uani 1 1 d . . . P2 P 0.89308(2) 0.256598(13) -0.017241(12) 0.02547(5) Uani 1 1 d . . . S1 S 0.61595(2) 0.243711(12) 0.180783(11) 0.02574(5) Uani 1 1 d . . . S2 S 1.10343(2) 0.250117(11) 0.108218(11) 0.02316(5) Uani 1 1 d . . . Si1 Si 0.57413(2) 0.122104(14) 0.080760(14) 0.02768(6) Uani 1 1 d . . . Si2 Si 0.79036(3) 0.288572(16) 0.306406(13) 0.02863(6) Uani 1 1 d . . . Si3 Si 1.07576(2) 0.107430(13) 0.176304(13) 0.02652(6) Uani 1 1 d . . . Si4 Si 1.10212(2) 0.407293(13) 0.141933(13) 0.02562(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0438(6) 0.0382(5) 0.0572(7) 0.0169(5) 0.0039(5) -0.0045(5) C2 0.0317(5) 0.0420(5) 0.0435(6) 0.0035(4) -0.0071(4) -0.0066(4) C3 0.0505(7) 0.0420(6) 0.0650(8) -0.0225(6) 0.0227(6) -0.0094(5) C4 0.0327(5) 0.0827(9) 0.0305(5) -0.0031(5) 0.0022(4) -0.0085(5) C5 0.0522(6) 0.0508(6) 0.0316(5) 0.0083(4) 0.0157(5) 0.0022(5) C6 0.0540(7) 0.0465(6) 0.0412(6) -0.0132(5) 0.0120(5) 0.0029(5) C7 0.0252(4) 0.0374(5) 0.0358(5) -0.0003(4) 0.0075(4) 0.0089(4) C8 0.0413(5) 0.0439(6) 0.0331(5) 0.0009(4) -0.0020(4) 0.0060(4) C9 0.0407(5) 0.0292(5) 0.0572(7) -0.0031(4) 0.0065(5) 0.0078(4) C10 0.0798(9) 0.0314(5) 0.0479(6) -0.0020(5) 0.0115(6) 0.0175(6) C11 0.0524(7) 0.0446(6) 0.0645(8) 0.0257(6) 0.0247(6) 0.0073(5) C12 0.0440(6) 0.0505(7) 0.0507(7) 0.0104(5) -0.0132(5) 0.0068(5) C13 0.0370(5) 0.0287(4) 0.0509(6) -0.0096(4) 0.0101(4) -0.0008(4) C14 0.0372(5) 0.0333(5) 0.0462(6) 0.0085(4) 0.0139(4) -0.0045(4) C15 0.0346(5) 0.0480(6) 0.0372(5) -0.0012(4) -0.0013(4) -0.0103(4) C16 0.0282(4) 0.0344(4) 0.0274(4) 0.0008(3) 0.0105(3) 0.0060(3) C17 0.0446(6) 0.0531(6) 0.0366(5) -0.0173(5) 0.0074(4) -0.0014(5) C18 0.0461(6) 0.0374(5) 0.0351(5) 0.0114(4) 0.0085(4) 0.0078(4) Mg1 0.01980(13) 0.02171(13) 0.02118(13) 0.00122(10) 0.00429(10) 0.00095(10) N1 0.0220(3) 0.0278(3) 0.0256(3) -0.0023(3) 0.0050(3) -0.0010(3) N2 0.0232(3) 0.0361(4) 0.0215(3) -0.0013(3) 0.0048(3) -0.0026(3) N3 0.0225(3) 0.0220(3) 0.0304(4) 0.0055(3) 0.0049(3) 0.0018(3) N4 0.0223(3) 0.0205(3) 0.0283(3) -0.0003(3) 0.0059(3) 0.0001(2) P1 0.02629(11) 0.02635(11) 0.02890(11) 0.00022(8) 0.00278(8) 0.00706(8) P2 0.02820(11) 0.02676(11) 0.02230(10) -0.00055(8) 0.00662(8) 0.00360(8) S1 0.02109(10) 0.03269(11) 0.02422(10) 0.00005(7) 0.00600(8) -0.00032(7) S2 0.01987(9) 0.02317(9) 0.02693(10) 0.00248(7) 0.00524(7) 0.00179(7) Si1 0.02496(11) 0.02537(11) 0.03224(13) -0.00030(9) 0.00314(9) -0.00251(9) Si2 0.02771(12) 0.03848(14) 0.02036(11) -0.00221(9) 0.00588(9) -0.00127(10) Si3 0.02919(12) 0.02246(11) 0.02781(12) 0.00470(9) 0.00428(9) 0.00544(9) Si4 0.02519(11) 0.02257(11) 0.02939(12) -0.00048(9) 0.00531(9) -0.00361(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 C1 Si1 1.8704(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 Si1 1.8757(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si1 1.8561(12) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 Si2 1.8594(12) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Si2 1.8685(12) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si2 1.8677(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 S1 1.8263(10) . ? C7 P1 1.8481(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 P1 1.8281(11) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 P1 1.8321(11) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si3 1.8590(12) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si3 1.8567(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si3 1.8709(12) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si4 1.8603(11) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si4 1.8790(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si4 1.8737(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 S2 1.8245(10) . ? C16 P2 1.8463(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 P2 1.8326(11) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 P2 1.8290(10) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Mg1 N3 2.1248(8) . ? Mg1 N2 2.1276(8) . ? Mg1 N1 2.1481(8) . ? Mg1 N4 2.1627(8) . ? Mg1 P1 2.8570(4) . ? Mg1 P2 2.8776(4) . ? N1 S1 1.6123(8) . ? N1 Si1 1.7237(8) . ? N2 S1 1.6111(8) . ? N2 Si2 1.7193(8) . ? N3 S2 1.6057(7) . ? N3 Si3 1.7207(7) . ? N4 S2 1.6162(7) . ? N4 Si4 1.7209(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? S1 C7 P1 107.75(5) . . ? S1 C7 H7A 110.2 . . ? P1 C7 H7A 110.2 . . ? S1 C7 H7B 110.2 . . ? P1 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? P1 C8 H8A 109.5 . . ? P1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P1 C9 H9A 109.5 . . ? P1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si3 C10 H10A 109.5 . . ? Si3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si3 C11 H11A 109.5 . . ? Si3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si3 C12 H12A 109.5 . . ? Si3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si4 C13 H13A 109.5 . . ? Si4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si4 C14 H14A 109.5 . . ? Si4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si4 C15 H15A 109.5 . . ? Si4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? S2 C16 P2 108.21(5) . . ? S2 C16 H16A 110.1 . . ? P2 C16 H16A 110.1 . . ? S2 C16 H16B 110.1 . . ? P2 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? P2 C17 H17A 109.5 . . ? P2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P2 C18 H18A 109.5 . . ? P2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 Mg1 N2 118.44(3) . . ? N3 Mg1 N1 113.52(3) . . ? N2 Mg1 N1 70.81(3) . . ? N3 Mg1 N4 70.75(3) . . ? N2 Mg1 N4 115.88(3) . . ? N1 Mg1 N4 169.95(3) . . ? N3 Mg1 P1 164.65(2) . . ? N2 Mg1 P1 76.69(2) . . ? N1 Mg1 P1 72.54(2) . . ? N4 Mg1 P1 101.07(2) . . ? N3 Mg1 P2 78.09(2) . . ? N2 Mg1 P2 163.15(2) . . ? N1 Mg1 P2 100.47(2) . . ? N4 Mg1 P2 71.05(2) . . ? P1 Mg1 P2 87.007(10) . . ? S1 N1 Si1 119.81(4) . . ? S1 N1 Mg1 92.37(3) . . ? Si1 N1 Mg1 144.68(4) . . ? S1 N2 Si2 119.91(4) . . ? S1 N2 Mg1 93.15(4) . . ? Si2 N2 Mg1 143.69(4) . . ? S2 N3 Si3 121.02(4) . . ? S2 N3 Mg1 93.38(3) . . ? Si3 N3 Mg1 141.33(4) . . ? S2 N4 Si4 118.95(4) . . ? S2 N4 Mg1 91.68(3) . . ? Si4 N4 Mg1 145.44(4) . . ? C8 P1 C9 100.94(5) . . ? C8 P1 C7 102.10(5) . . ? C9 P1 C7 100.59(5) . . ? C8 P1 Mg1 116.75(4) . . ? C9 P1 Mg1 136.80(4) . . ? C7 P1 Mg1 91.80(3) . . ? C18 P2 C17 100.38(6) . . ? C18 P2 C16 102.10(5) . . ? C17 P2 C16 100.53(5) . . ? C18 P2 Mg1 114.39(4) . . ? C17 P2 Mg1 140.11(4) . . ? C16 P2 Mg1 91.05(3) . . ? N2 S1 N1 100.44(4) . . ? N2 S1 C7 101.86(4) . . ? N1 S1 C7 101.02(4) . . ? N3 S2 N4 100.80(4) . . ? N3 S2 C16 102.43(4) . . ? N4 S2 C16 100.69(4) . . ? N1 Si1 C3 106.47(5) . . ? N1 Si1 C1 112.46(5) . . ? C3 Si1 C1 110.56(6) . . ? N1 Si1 C2 110.95(4) . . ? C3 Si1 C2 109.81(6) . . ? C1 Si1 C2 106.63(5) . . ? N2 Si2 C4 106.12(5) . . ? N2 Si2 C6 111.44(5) . . ? C4 Si2 C6 109.69(6) . . ? N2 Si2 C5 111.62(5) . . ? C4 Si2 C5 110.21(6) . . ? C6 Si2 C5 107.77(6) . . ? N3 Si3 C11 106.94(5) . . ? N3 Si3 C10 111.90(5) . . ? C11 Si3 C10 109.03(7) . . ? N3 Si3 C12 110.91(5) . . ? C11 Si3 C12 109.12(7) . . ? C10 Si3 C12 108.87(7) . . ? N4 Si4 C13 106.62(4) . . ? N4 Si4 C15 112.24(4) . . ? C13 Si4 C15 110.75(5) . . ? N4 Si4 C14 111.82(4) . . ? C13 Si4 C14 109.25(5) . . ? C15 Si4 C14 106.19(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Mg1 N1 S1 125.45(4) . . . . ? N2 Mg1 N1 S1 11.97(3) . . . . ? N4 Mg1 N1 S1 -121.25(17) . . . . ? P1 Mg1 N1 S1 -69.63(3) . . . . ? P2 Mg1 N1 S1 -153.10(3) . . . . ? N3 Mg1 N1 Si1 -31.34(9) . . . . ? N2 Mg1 N1 Si1 -144.82(8) . . . . ? N4 Mg1 N1 Si1 82.0(2) . . . . ? P1 Mg1 N1 Si1 133.58(8) . . . . ? P2 Mg1 N1 Si1 50.12(8) . . . . ? N3 Mg1 N2 S1 -118.96(4) . . . . ? N1 Mg1 N2 S1 -11.98(3) . . . . ? N4 Mg1 N2 S1 159.89(3) . . . . ? P1 Mg1 N2 S1 63.89(3) . . . . ? P2 Mg1 N2 S1 48.98(11) . . . . ? N3 Mg1 N2 Si2 37.72(9) . . . . ? N1 Mg1 N2 Si2 144.70(9) . . . . ? N4 Mg1 N2 Si2 -43.43(9) . . . . ? P1 Mg1 N2 Si2 -139.42(8) . . . . ? P2 Mg1 N2 Si2 -154.33(5) . . . . ? N2 Mg1 N3 S2 -121.97(4) . . . . ? N1 Mg1 N3 S2 157.93(3) . . . . ? N4 Mg1 N3 S2 -12.29(3) . . . . ? P1 Mg1 N3 S2 47.49(11) . . . . ? P2 Mg1 N3 S2 61.58(3) . . . . ? N2 Mg1 N3 Si3 32.19(8) . . . . ? N1 Mg1 N3 Si3 -47.91(8) . . . . ? N4 Mg1 N3 Si3 141.87(8) . . . . ? P1 Mg1 N3 Si3 -158.34(5) . . . . ? P2 Mg1 N3 Si3 -144.26(7) . . . . ? N3 Mg1 N4 S2 12.19(3) . . . . ? N2 Mg1 N4 S2 125.22(4) . . . . ? N1 Mg1 N4 S2 -104.69(17) . . . . ? P1 Mg1 N4 S2 -154.33(3) . . . . ? P2 Mg1 N4 S2 -71.42(3) . . . . ? N3 Mg1 N4 Si4 -141.48(8) . . . . ? N2 Mg1 N4 Si4 -28.45(9) . . . . ? N1 Mg1 N4 Si4 101.65(18) . . . . ? P1 Mg1 N4 Si4 52.01(8) . . . . ? P2 Mg1 N4 Si4 134.92(8) . . . . ? S1 C7 P1 C8 113.25(6) . . . . ? S1 C7 P1 C9 -143.01(6) . . . . ? S1 C7 P1 Mg1 -4.61(5) . . . . ? N3 Mg1 P1 C8 52.33(10) . . . . ? N2 Mg1 P1 C8 -137.18(5) . . . . ? N1 Mg1 P1 C8 -63.42(5) . . . . ? N4 Mg1 P1 C8 108.56(5) . . . . ? P2 Mg1 P1 C8 38.53(5) . . . . ? N3 Mg1 P1 C9 -95.58(11) . . . . ? N2 Mg1 P1 C9 74.91(7) . . . . ? N1 Mg1 P1 C9 148.67(7) . . . . ? N4 Mg1 P1 C9 -39.35(7) . . . . ? P2 Mg1 P1 C9 -109.37(6) . . . . ? N3 Mg1 P1 C7 156.84(10) . . . . ? N2 Mg1 P1 C7 -32.67(4) . . . . ? N1 Mg1 P1 C7 41.09(4) . . . . ? N4 Mg1 P1 C7 -146.93(4) . . . . ? P2 Mg1 P1 C7 143.05(3) . . . . ? S2 C16 P2 C18 107.54(6) . . . . ? S2 C16 P2 C17 -149.33(6) . . . . ? S2 C16 P2 Mg1 -7.70(4) . . . . ? N3 Mg1 P2 C18 -133.37(5) . . . . ? N2 Mg1 P2 C18 57.45(10) . . . . ? N1 Mg1 P2 C18 114.56(5) . . . . ? N4 Mg1 P2 C18 -59.85(5) . . . . ? P1 Mg1 P2 C18 42.93(4) . . . . ? N3 Mg1 P2 C17 78.31(7) . . . . ? N2 Mg1 P2 C17 -90.88(11) . . . . ? N1 Mg1 P2 C17 -33.77(7) . . . . ? N4 Mg1 P2 C17 151.82(7) . . . . ? P1 Mg1 P2 C17 -105.39(7) . . . . ? N3 Mg1 P2 C16 -29.57(4) . . . . ? N2 Mg1 P2 C16 161.25(9) . . . . ? N1 Mg1 P2 C16 -141.64(4) . . . . ? N4 Mg1 P2 C16 43.95(4) . . . . ? P1 Mg1 P2 C16 146.73(3) . . . . ? Si2 N2 S1 N1 -148.91(5) . . . . ? Mg1 N2 S1 N1 15.40(4) . . . . ? Si2 N2 S1 C7 107.37(6) . . . . ? Mg1 N2 S1 C7 -88.32(4) . . . . ? Si1 N1 S1 N2 149.53(5) . . . . ? Mg1 N1 S1 N2 -15.24(4) . . . . ? Si1 N1 S1 C7 -106.07(6) . . . . ? Mg1 N1 S1 C7 89.16(4) . . . . ? P1 C7 S1 N2 56.09(6) . . . . ? P1 C7 S1 N1 -47.18(6) . . . . ? Si3 N3 S2 N4 -145.59(5) . . . . ? Mg1 N3 S2 N4 15.88(4) . . . . ? Si3 N3 S2 C16 110.80(6) . . . . ? Mg1 N3 S2 C16 -87.73(4) . . . . ? Si4 N4 S2 N3 147.71(5) . . . . ? Mg1 N4 S2 N3 -15.58(4) . . . . ? Si4 N4 S2 C16 -107.28(5) . . . . ? Mg1 N4 S2 C16 89.43(4) . . . . ? P2 C16 S2 N3 59.27(5) . . . . ? P2 C16 S2 N4 -44.43(5) . . . . ? S1 N1 Si1 C3 -168.90(6) . . . . ? Mg1 N1 Si1 C3 -15.90(10) . . . . ? S1 N1 Si1 C1 -47.68(7) . . . . ? Mg1 N1 Si1 C1 105.33(8) . . . . ? S1 N1 Si1 C2 71.65(7) . . . . ? Mg1 N1 Si1 C2 -135.34(8) . . . . ? S1 N2 Si2 C4 165.73(7) . . . . ? Mg1 N2 Si2 C4 12.85(10) . . . . ? S1 N2 Si2 C6 -74.91(7) . . . . ? Mg1 N2 Si2 C6 132.21(8) . . . . ? S1 N2 Si2 C5 45.64(7) . . . . ? Mg1 N2 Si2 C5 -107.24(8) . . . . ? S2 N3 Si3 C11 154.42(7) . . . . ? Mg1 N3 Si3 C11 4.93(9) . . . . ? S2 N3 Si3 C10 -86.24(8) . . . . ? Mg1 N3 Si3 C10 124.27(8) . . . . ? S2 N3 Si3 C12 35.55(8) . . . . ? Mg1 N3 Si3 C12 -113.94(8) . . . . ? S2 N4 Si4 C13 -174.59(5) . . . . ? Mg1 N4 Si4 C13 -25.03(9) . . . . ? S2 N4 Si4 C15 -53.15(7) . . . . ? Mg1 N4 Si4 C15 96.40(8) . . . . ? S2 N4 Si4 C14 66.07(6) . . . . ? Mg1 N4 Si4 C14 -144.38(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.286 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.040 #===END data_p21n _database_code_depnum_ccdc_archive 'CCDC 779995' #TrackingRef '- all_full.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H31 N2 P S Si2' _chemical_formula_weight 406.67 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' Si Si 0.0817 0.0704 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9937(7) _cell_length_b 9.9367(6) _cell_length_c 18.1145(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.8430(10) _cell_angle_gamma 90.00 _cell_volume 2304.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9935 _cell_measurement_theta_min 2.595 _cell_measurement_theta_max 29.949 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8590 _exptl_absorpt_correction_T_max 0.9422 _exptl_absorpt_process_details SADABS-2008/2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS Mo rotating anode' _diffrn_radiation_monochromator 'INCOATEC Helios mirror optics' _diffrn_measurement_device_type 'Bruker TXS Mo rotating anode' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43786 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_av_sigmaI/netI 0.0083 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.88 _reflns_number_total 5491 _reflns_number_gt 5259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.2-0' _computing_cell_refinement 'SAINT v46A' _computing_data_reduction 'SAINT v46A' _computing_structure_solution 'SHELXS in SHELXTL v2008/4' _computing_structure_refinement 'SHELXL in SHELXTL v2008/4' _computing_molecular_graphics 'XSHELL v4.01' _computing_publication_material 'XSHELL v4.01' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+1.0873P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5491 _refine_ls_number_parameters 235 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.18064(9) 0.23395(12) -0.15557(7) 0.0245(2) Uani 1 1 d . . . C2 C 0.24069(10) 0.12721(13) -0.17411(7) 0.0282(3) Uani 1 1 d . . . H2 H 0.3031 0.1033 -0.1414 0.034 Uiso 1 1 calc R . . C3 C 0.21013(11) 0.05492(15) -0.24034(8) 0.0342(3) Uani 1 1 d . . . H3 H 0.2523 -0.0169 -0.2528 0.041 Uiso 1 1 calc R . . C4 C 0.11859(12) 0.08754(17) -0.28789(8) 0.0381(3) Uani 1 1 d . . . H4 H 0.0972 0.0374 -0.3325 0.046 Uiso 1 1 calc R . . C5 C 0.05814(12) 0.19382(17) -0.27012(8) 0.0374(3) Uani 1 1 d . . . H5 H -0.0050 0.2161 -0.3025 0.045 Uiso 1 1 calc R . . C6 C 0.08939(10) 0.26754(14) -0.20537(7) 0.0311(3) Uani 1 1 d . . . H6 H 0.0485 0.3419 -0.1945 0.037 Uiso 1 1 calc R . . C7 C 0.31581(9) 0.23499(13) -0.01330(7) 0.0256(2) Uani 1 1 d . . . C8 C 0.41939(10) 0.27605(16) -0.00750(8) 0.0344(3) Uani 1 1 d . . . H8 H 0.4357 0.3541 -0.0335 0.041 Uiso 1 1 calc R . . C9 C 0.49921(11) 0.20344(19) 0.03617(9) 0.0450(4) Uani 1 1 d . . . H9 H 0.5697 0.2317 0.0392 0.054 Uiso 1 1 calc R . . C10 C 0.47693(13) 0.09175(19) 0.07473(9) 0.0455(4) Uani 1 1 d . . . H10 H 0.5318 0.0432 0.1047 0.055 Uiso 1 1 calc R . . C11 C 0.37517(13) 0.04968(18) 0.07016(9) 0.0441(4) Uani 1 1 d . . . H11 H 0.3596 -0.0277 0.0970 0.053 Uiso 1 1 calc R . . C12 C 0.29491(11) 0.12096(15) 0.02603(8) 0.0354(3) Uani 1 1 d . . . H12 H 0.2248 0.0911 0.0228 0.043 Uiso 1 1 calc R . . C13 C 0.09890(8) 0.30418(12) -0.03031(7) 0.0219(2) Uani 1 1 d . . . H13A H 0.0380 0.3470 -0.0620 0.026 Uiso 1 1 calc R . . H13B H 0.0865 0.2059 -0.0310 0.026 Uiso 1 1 calc R . . C14 C -0.00610(10) 0.06696(13) 0.11966(8) 0.0316(3) Uani 1 1 d . . . H14A H -0.0296 0.0371 0.0680 0.047 Uiso 1 1 calc R . . H14B H -0.0299 0.0028 0.1542 0.047 Uiso 1 1 calc R . . H14C H 0.0704 0.0718 0.1298 0.047 Uiso 1 1 calc R . . C15 C -0.02014(11) 0.29300(15) 0.23134(7) 0.0321(3) Uani 1 1 d . . . H15A H 0.0563 0.2951 0.2433 0.048 Uiso 1 1 calc R . . H15B H -0.0472 0.2305 0.2653 0.048 Uiso 1 1 calc R . . H15C H -0.0478 0.3834 0.2373 0.048 Uiso 1 1 calc R . . C16 C -0.20572(9) 0.23779(13) 0.10572(7) 0.0254(2) Uani 1 1 d . . . H16A H -0.2300 0.3308 0.0974 0.038 Uiso 1 1 calc R . . H16B H -0.2375 0.1975 0.1458 0.038 Uiso 1 1 calc R . . H16C H -0.2259 0.1859 0.0595 0.038 Uiso 1 1 calc R . . C17 C 0.35759(11) 0.5869(2) 0.09588(11) 0.0491(4) Uani 1 1 d . . . H17A H 0.3856 0.4960 0.1064 0.074 Uiso 1 1 calc R . . H17B H 0.4045 0.6525 0.1247 0.074 Uiso 1 1 calc R . . H17C H 0.3520 0.6060 0.0423 0.074 Uiso 1 1 calc R . . C18 C 0.23047(18) 0.5345(2) 0.21939(9) 0.0695(7) Uani 1 1 d . . . H18A H 0.1610 0.5417 0.2333 0.104 Uiso 1 1 calc R . . H18B H 0.2804 0.5879 0.2542 0.104 Uiso 1 1 calc R . . H18C H 0.2525 0.4401 0.2217 0.104 Uiso 1 1 calc R . . C19 C 0.18521(13) 0.77830(15) 0.11963(9) 0.0417(3) Uani 1 1 d . . . H19A H 0.1787 0.8116 0.0681 0.063 Uiso 1 1 calc R . . H19B H 0.2378 0.8314 0.1524 0.063 Uiso 1 1 calc R . . H19C H 0.1178 0.7866 0.1366 0.063 Uiso 1 1 calc R . . N1 N -0.01665(7) 0.34967(10) 0.07235(5) 0.01986(18) Uani 1 1 d D . . H1 H -0.0571(11) 0.3869(15) 0.0362(8) 0.024 Uiso 1 1 d D . . N2 N 0.13491(7) 0.51754(10) 0.05796(5) 0.02069(19) Uani 1 1 d . . . P1 P 0.21729(2) 0.33885(3) -0.071450(18) 0.02381(8) Uani 1 1 d . . . S1 S 0.10774(2) 0.36460(3) 0.064784(15) 0.01901(7) Uani 1 1 d . . . Si1 Si -0.06140(2) 0.23621(3) 0.133005(17) 0.01848(8) Uani 1 1 d . . . Si2 Si 0.22564(2) 0.59867(4) 0.122995(18) 0.02355(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0236(5) 0.0245(6) 0.0270(6) 0.0058(4) 0.0093(4) -0.0027(4) C2 0.0251(6) 0.0316(6) 0.0296(6) 0.0017(5) 0.0094(5) 0.0002(5) C3 0.0378(7) 0.0379(7) 0.0304(6) -0.0011(5) 0.0155(5) -0.0018(6) C4 0.0437(8) 0.0494(9) 0.0227(6) 0.0018(6) 0.0103(5) -0.0106(7) C5 0.0355(7) 0.0496(8) 0.0263(6) 0.0131(6) 0.0027(5) -0.0031(6) C6 0.0303(6) 0.0319(7) 0.0319(6) 0.0114(5) 0.0078(5) 0.0017(5) C7 0.0186(5) 0.0288(6) 0.0300(6) -0.0066(5) 0.0053(4) 0.0028(4) C8 0.0212(6) 0.0398(7) 0.0426(7) -0.0114(6) 0.0062(5) -0.0023(5) C9 0.0204(6) 0.0597(10) 0.0518(9) -0.0223(8) -0.0028(6) 0.0039(6) C10 0.0381(8) 0.0570(10) 0.0367(7) -0.0140(7) -0.0069(6) 0.0215(7) C11 0.0448(8) 0.0458(9) 0.0420(8) 0.0060(7) 0.0084(7) 0.0193(7) C12 0.0267(6) 0.0368(7) 0.0437(8) 0.0053(6) 0.0087(5) 0.0087(5) C13 0.0170(5) 0.0193(5) 0.0300(6) -0.0023(4) 0.0058(4) -0.0004(4) C14 0.0293(6) 0.0202(6) 0.0477(8) 0.0065(5) 0.0134(5) 0.0025(5) C15 0.0317(6) 0.0418(7) 0.0218(6) 0.0031(5) 0.0018(5) -0.0036(6) C16 0.0182(5) 0.0274(6) 0.0307(6) 0.0022(5) 0.0047(4) -0.0006(4) C17 0.0218(6) 0.0604(10) 0.0628(10) -0.0254(9) 0.0009(6) -0.0056(6) C18 0.0806(14) 0.0902(15) 0.0278(7) 0.0188(9) -0.0189(8) -0.0461(12) C19 0.0456(8) 0.0316(7) 0.0452(8) -0.0155(6) -0.0003(6) -0.0045(6) N1 0.0142(4) 0.0219(5) 0.0228(4) 0.0057(4) 0.0012(3) 0.0003(3) N2 0.0189(4) 0.0186(4) 0.0223(4) 0.0033(3) -0.0028(3) -0.0029(3) P1 0.01853(14) 0.02000(15) 0.03418(17) 0.00116(11) 0.00816(12) -0.00154(10) S1 0.01400(12) 0.01791(13) 0.02406(13) 0.00461(9) 0.00021(9) 0.00045(9) Si1 0.01671(14) 0.01759(15) 0.02107(15) 0.00292(11) 0.00303(11) 0.00027(10) Si2 0.01951(15) 0.02748(17) 0.02184(15) -0.00006(12) -0.00160(11) -0.00580(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 C1 C2 1.3915(18) . ? C1 C6 1.4018(18) . ? C1 P1 1.8404(13) . ? C2 C3 1.3964(19) . ? C2 H2 0.9500 . ? C3 C4 1.383(2) . ? C3 H3 0.9500 . ? C4 C5 1.386(2) . ? C4 H4 0.9500 . ? C5 C6 1.384(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.3898(19) . ? C7 C8 1.3930(17) . ? C7 P1 1.8310(13) . ? C8 C9 1.393(2) . ? C8 H8 0.9500 . ? C9 C10 1.368(3) . ? C9 H9 0.9500 . ? C10 C11 1.376(2) . ? C10 H10 0.9500 . ? C11 C12 1.394(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 S1 1.8092(12) . ? C13 P1 1.8526(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 Si1 1.8607(13) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.8581(13) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si1 1.8559(12) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.8661(16) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 Si2 1.8498(16) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 Si2 1.8587(16) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N1 S1 1.6520(9) . ? N1 Si1 1.7421(10) . ? N1 H1 0.850(13) . ? N2 S1 1.5698(10) . ? N2 Si2 1.7184(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 C2 C1 C6 118.27(12) . . ? C2 C1 P1 123.72(10) . . ? C6 C1 P1 117.94(10) . . ? C1 C2 C3 120.71(12) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 120.17(14) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.68(14) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.28(13) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.85(13) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C12 C7 C8 118.10(12) . . ? C12 C7 P1 125.15(10) . . ? C8 C7 P1 116.73(11) . . ? C7 C8 C9 120.46(15) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 120.52(14) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.05(14) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 119.82(16) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 121.04(14) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? S1 C13 P1 113.54(6) . . ? S1 C13 H13A 108.9 . . ? P1 C13 H13A 108.9 . . ? S1 C13 H13B 108.9 . . ? P1 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? S1 N1 Si1 123.18(6) . . ? S1 N1 H1 112.4(10) . . ? Si1 N1 H1 122.6(10) . . ? S1 N2 Si2 122.50(6) . . ? C7 P1 C1 102.33(6) . . ? C7 P1 C13 102.17(6) . . ? C1 P1 C13 96.47(5) . . ? N2 S1 N1 109.26(5) . . ? N2 S1 C13 102.99(5) . . ? N1 S1 C13 98.36(5) . . ? N1 Si1 C16 104.92(5) . . ? N1 Si1 C15 109.59(6) . . ? C16 Si1 C15 111.45(6) . . ? N1 Si1 C14 108.97(5) . . ? C16 Si1 C14 111.60(6) . . ? C15 Si1 C14 110.15(7) . . ? N2 Si2 C18 113.21(7) . . ? N2 Si2 C19 105.73(6) . . ? C18 Si2 C19 109.00(10) . . ? N2 Si2 C17 110.10(6) . . ? C18 Si2 C17 110.02(10) . . ? C19 Si2 C17 108.60(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.54(18) . . . . ? P1 C1 C2 C3 -177.57(10) . . . . ? C1 C2 C3 C4 -1.0(2) . . . . ? C2 C3 C4 C5 1.1(2) . . . . ? C3 C4 C5 C6 0.4(2) . . . . ? C4 C5 C6 C1 -1.9(2) . . . . ? C2 C1 C6 C5 1.98(18) . . . . ? P1 C1 C6 C5 179.19(10) . . . . ? C12 C7 C8 C9 0.5(2) . . . . ? P1 C7 C8 C9 179.43(11) . . . . ? C7 C8 C9 C10 -0.8(2) . . . . ? C8 C9 C10 C11 0.5(2) . . . . ? C9 C10 C11 C12 0.1(2) . . . . ? C8 C7 C12 C11 0.1(2) . . . . ? P1 C7 C12 C11 -178.70(11) . . . . ? C10 C11 C12 C7 -0.4(2) . . . . ? C12 C7 P1 C1 -75.07(12) . . . . ? C8 C7 P1 C1 106.11(10) . . . . ? C12 C7 P1 C13 24.43(13) . . . . ? C8 C7 P1 C13 -154.39(10) . . . . ? C2 C1 P1 C7 -17.45(11) . . . . ? C6 C1 P1 C7 165.51(9) . . . . ? C2 C1 P1 C13 -121.45(11) . . . . ? C6 C1 P1 C13 61.51(10) . . . . ? S1 C13 P1 C7 65.67(7) . . . . ? S1 C13 P1 C1 169.81(7) . . . . ? Si2 N2 S1 N1 118.05(7) . . . . ? Si2 N2 S1 C13 -138.14(7) . . . . ? Si1 N1 S1 N2 -139.35(7) . . . . ? Si1 N1 S1 C13 113.67(7) . . . . ? P1 C13 S1 N2 54.81(7) . . . . ? P1 C13 S1 N1 166.90(6) . . . . ? S1 N1 Si1 C16 -169.28(7) . . . . ? S1 N1 Si1 C15 70.96(9) . . . . ? S1 N1 Si1 C14 -49.64(9) . . . . ? S1 N2 Si2 C18 -33.31(13) . . . . ? S1 N2 Si2 C19 -152.57(8) . . . . ? S1 N2 Si2 C17 90.31(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.596 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.043