Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Dominic S. Wright' 'Dana Eisler' 'Robert J. Less' 'Vesal Naseri' 'J. Rawson' _publ_contact_author_name 'Dominic S. Wright' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email DSW1000@CAM.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The 6pi, phosphide-stabilised stannylene dianion [C6H4P2Sn]2- ; the first member of a new class of Arduengo-type carbene analogues ; data_1 _database_code_depnum_ccdc_archive 'CCDC 674806' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H36 Li2 N4 P2 Sn' _chemical_formula_sum 'C18 H36 Li2 N4 P2 Sn' _chemical_formula_weight 503.02 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 8.6104(2) _cell_length_b 14.8211(3) _cell_length_c 19.5316(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.1437(8) _cell_angle_gamma 90.00 _cell_volume 2488.79(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 24702 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _publ_section_exptl_refinement ; The crystals of the complex form as non-merohedral twins. Application of the twin determination program ROTAX (Parsons 2002) determined that twinning occurred around the [100] direct lattice axis. The program WinGX (Farrugia 1999) was used to prepare an HKLF5 file for further refinement. The R values, K value, esds and background noise were all substantially improved, indicating the correct twin assignment. One of the coordinated molecules of TMEDA was disordered, and was modeled as an isotropic 50:50 mixture with geometric restraints. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_reflns_number 28089 _diffrn_reflns_av_R_equivalents 0.107 _diffrn_reflns_av_sigmaI/netI 0.069 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11383 _reflns_number_gt 9301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+5.6717P] 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 11383 _refine_ls_number_parameters 234 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.042 _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 Sn1 Sn 1.25997(6) 1.11465(2) 0.828449(17) 0.03755(12) Uani 1 1 d . A . P1 P 1.26398(14) 1.15060(6) 0.70497(6) 0.0333(3) Uani 1 1 d . A . P2 P 1.27284(14) 0.95410(6) 0.79696(5) 0.0351(3) Uani 1 1 d . . . C1 C 1.2928(5) 1.0402(3) 0.66627(19) 0.0309(9) Uani 1 1 d . A . C2 C 1.3182(5) 1.0325(2) 0.59635(19) 0.0352(10) Uani 1 1 d . . . H2A H 1.3152 1.0858 0.5693 0.042 Uiso 1 1 calc R . . C3 C 1.3469(7) 0.9529(3) 0.5651(3) 0.0397(12) Uani 1 1 d . . . H3A H 1.3625 0.9514 0.5173 0.048 Uiso 1 1 calc R . . C4 C 1.3536(5) 0.8726(2) 0.6034(2) 0.0412(10) Uani 1 1 d . . . H4A H 1.3750 0.8165 0.5823 0.049 Uiso 1 1 calc R . . C5 C 1.3285(6) 0.8772(3) 0.6717(3) 0.0355(12) Uani 1 1 d . . . H5A H 1.3305 0.8225 0.6972 0.043 Uiso 1 1 calc R . . C6 C 1.2999(6) 0.9574(2) 0.7066(2) 0.0344(12) Uani 1 1 d . A . Li1 Li 1.0329(7) 1.0286(4) 0.7224(3) 0.0380(15) Uiso 1 1 d D . . N1 N 0.8182(9) 1.0756(5) 0.7578(4) 0.041(3) Uiso 0.50 1 d PD A 1 N2 N 0.8905(10) 0.9567(5) 0.6535(4) 0.037(3) Uiso 0.50 1 d PD A 1 C7 C 0.793(2) 1.1731(7) 0.7429(9) 0.081(3) Uiso 0.50 1 d PD A 1 H7A H 0.6812 1.1859 0.7396 0.121 Uiso 0.50 1 calc PR A 1 H7B H 0.8382 1.1883 0.6994 0.121 Uiso 0.50 1 calc PR A 1 H7C H 0.8430 1.2092 0.7799 0.121 Uiso 0.50 1 calc PR A 1 C8 C 0.7793(15) 1.0451(8) 0.8247(5) 0.068(3) Uiso 0.50 1 d PD A 1 H8A H 0.6864 1.0770 0.8386 0.102 Uiso 0.50 1 calc PR A 1 H8B H 0.8663 1.0575 0.8578 0.102 Uiso 0.50 1 calc PR A 1 H8C H 0.7589 0.9801 0.8233 0.102 Uiso 0.50 1 calc PR A 1 C9 C 0.6900(10) 1.0266(7) 0.7253(5) 0.059(2) Uiso 0.50 1 d PD A 1 H9A H 0.6007 1.0680 0.7167 0.070 Uiso 0.50 1 calc PR A 1 H9B H 0.6573 0.9783 0.7564 0.070 Uiso 0.50 1 calc PR A 1 C10 C 0.7322(12) 0.9873(10) 0.6614(5) 0.068(3) Uiso 0.50 1 d PD A 1 H10A H 0.7077 1.0323 0.6249 0.081 Uiso 0.50 1 calc PR A 1 H10B H 0.6626 0.9351 0.6520 0.081 Uiso 0.50 1 calc PR A 1 C11 C 0.8937(19) 0.8607(7) 0.6786(8) 0.050(4) Uiso 0.50 1 d PD A 1 H11A H 0.8243 0.8238 0.6486 0.076 Uiso 0.50 1 calc PR A 1 H11B H 0.8588 0.8587 0.7255 0.076 Uiso 0.50 1 calc PR A 1 H11C H 1.0000 0.8372 0.6780 0.076 Uiso 0.50 1 calc PR A 1 C12 C 0.930(2) 0.9575(11) 0.5804(6) 0.052(2) Uiso 0.50 1 d PD A 1 H12A H 0.8549 0.9209 0.5533 0.079 Uiso 0.50 1 calc PR A 1 H12B H 1.0349 0.9324 0.5765 0.079 Uiso 0.50 1 calc PR A 1 H12C H 0.9278 1.0196 0.5632 0.079 Uiso 0.50 1 calc PR A 1 N1A N 0.8235(9) 1.0955(6) 0.7504(4) 0.040(3) Uiso 0.50 1 d PD A 2 N2A N 0.8934(10) 0.9370(6) 0.6630(4) 0.036(3) Uiso 0.50 1 d PD A 2 C7A C 0.8344(19) 1.1943(6) 0.7428(8) 0.081(3) Uiso 0.50 1 d PD A 2 H7D H 0.7410 1.2225 0.7597 0.121 Uiso 0.50 1 calc PR A 2 H7E H 0.8429 1.2094 0.6944 0.121 Uiso 0.50 1 calc PR A 2 H7F H 0.9265 1.2164 0.7694 0.121 Uiso 0.50 1 calc PR A 2 C8A C 0.790(3) 1.0935(14) 0.8256(6) 0.068(3) Uiso 0.50 1 d PD A 2 H8D H 0.6833 1.1135 0.8312 0.102 Uiso 0.50 1 calc PR A 2 H8E H 0.8626 1.1339 0.8511 0.102 Uiso 0.50 1 calc PR A 2 H8F H 0.8034 1.0319 0.8431 0.102 Uiso 0.50 1 calc PR A 2 C9A C 0.7153(14) 1.0563(6) 0.6965(6) 0.059(2) Uiso 0.50 1 d PD A 2 H9C H 0.7319 1.0861 0.6521 0.070 Uiso 0.50 1 calc PR A 2 H9D H 0.6067 1.0680 0.7083 0.070 Uiso 0.50 1 calc PR A 2 C10A C 0.7401(13) 0.9540(7) 0.6893(8) 0.068(3) Uiso 0.50 1 d PD A 2 H10C H 0.7329 0.9245 0.7345 0.081 Uiso 0.50 1 calc PR A 2 H10D H 0.6582 0.9284 0.6575 0.081 Uiso 0.50 1 calc PR A 2 C11A C 0.9488(13) 0.8427(6) 0.6638(5) 0.048(3) Uiso 0.50 1 d PD A 2 H11D H 0.8688 0.8038 0.6417 0.072 Uiso 0.50 1 calc PR A 2 H11E H 0.9701 0.8232 0.7114 0.072 Uiso 0.50 1 calc PR A 2 H11F H 1.0443 0.8386 0.6389 0.072 Uiso 0.50 1 calc PR A 2 C12A C 0.902(3) 0.9678(11) 0.5897(5) 0.052(2) Uiso 0.50 1 d PD A 2 H12D H 0.8409 0.9267 0.5594 0.079 Uiso 0.50 1 calc PR A 2 H12E H 1.0104 0.9677 0.5771 0.079 Uiso 0.50 1 calc PR A 2 H12F H 0.8594 1.0290 0.5849 0.079 Uiso 0.50 1 calc PR A 2 Li2 Li 1.2406(8) 1.3031(4) 0.6376(3) 0.0321(13) Uiso 1 1 d . . . N3 N 1.4062(5) 1.3149(3) 0.56149(17) 0.0405(10) Uani 1 1 d . A . N4 N 1.0670(5) 1.3126(3) 0.55249(18) 0.0426(11) Uani 1 1 d . A . C13 C 1.4674(15) 1.4088(7) 0.5585(7) 0.090(4) Uani 1 1 d . . . H13A H 1.5409 1.4132 0.5221 0.135 Uiso 1 1 calc R A . H13B H 1.5207 1.4243 0.6026 0.135 Uiso 1 1 calc R . . H13C H 1.3810 1.4508 0.5489 0.135 Uiso 1 1 calc R . . C14 C 1.5404(7) 1.2545(4) 0.5711(3) 0.0569(15) Uani 1 1 d . . . H14A H 1.6011 1.2560 0.5301 0.085 Uiso 1 1 calc R A . H14B H 1.5040 1.1928 0.5786 0.085 Uiso 1 1 calc R . . H14C H 1.6056 1.2742 0.6110 0.085 Uiso 1 1 calc R . . C15 C 1.3140(6) 1.2881(3) 0.4985(2) 0.0603(13) Uani 1 1 d . . . H15A H 1.2982 1.2219 0.4985 0.072 Uiso 1 1 calc R A . H15B H 1.3722 1.3038 0.4578 0.072 Uiso 1 1 calc R . . C16 C 1.1594(6) 1.3345(3) 0.4940(2) 0.0596(13) Uani 1 1 d . A . H16A H 1.1757 1.4006 0.4923 0.072 Uiso 1 1 calc R . . H16B H 1.1014 1.3162 0.4511 0.072 Uiso 1 1 calc R . . C17 C 0.9467(9) 1.3803(5) 0.5592(4) 0.046(2) Uani 1 1 d . . . H17A H 0.8763 1.3799 0.5181 0.068 Uiso 1 1 calc R A . H17B H 0.9949 1.4400 0.5647 0.068 Uiso 1 1 calc R . . H17C H 0.8878 1.3667 0.5995 0.068 Uiso 1 1 calc R . . C18 C 0.9906(7) 1.2242(4) 0.5413(3) 0.0593(17) Uani 1 1 d . . . H18A H 0.9234 1.2263 0.4992 0.089 Uiso 1 1 calc R A . H18B H 0.9278 1.2102 0.5803 0.089 Uiso 1 1 calc R . . H18C H 1.0699 1.1774 0.5370 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0535(3) 0.02679(17) 0.03150(16) -0.00226(12) -0.00544(14) -0.00040(17) P1 0.0442(8) 0.0220(5) 0.0334(6) 0.0038(4) -0.0002(5) 0.0020(5) P2 0.0489(8) 0.0243(5) 0.0317(5) 0.0031(4) -0.0002(5) 0.0021(5) C1 0.039(3) 0.0260(19) 0.028(2) 0.0027(15) 0.0068(19) -0.003(2) C2 0.035(3) 0.034(2) 0.036(2) 0.0085(16) -0.0023(19) -0.0024(19) C3 0.034(4) 0.048(3) 0.039(3) -0.001(2) 0.010(2) 0.000(2) C4 0.042(3) 0.038(2) 0.044(3) -0.0076(17) 0.0068(19) 0.0042(19) C5 0.037(4) 0.023(2) 0.046(3) 0.0060(19) -0.002(2) 0.005(2) C6 0.040(3) 0.0228(19) 0.041(3) 0.0066(16) 0.006(2) 0.006(2) N3 0.045(4) 0.035(2) 0.041(2) 0.0030(17) 0.0057(17) 0.001(2) N4 0.048(4) 0.043(2) 0.036(2) -0.0008(17) -0.0027(18) 0.005(2) C13 0.106(7) 0.026(4) 0.144(8) -0.001(4) 0.057(6) -0.019(4) C14 0.044(4) 0.057(4) 0.070(5) 0.001(3) 0.010(3) 0.013(3) C15 0.069(4) 0.078(3) 0.034(3) 0.001(2) 0.007(2) 0.007(3) C16 0.058(4) 0.082(3) 0.040(3) 0.014(2) 0.004(2) 0.013(3) C17 0.037(4) 0.048(7) 0.051(4) -0.018(4) -0.013(3) 0.016(4) C18 0.055(4) 0.063(4) 0.059(4) -0.018(3) -0.005(3) -0.009(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 Sn1 P2 2.4617(10) . ? Sn1 P1 2.4721(12) . ? Sn1 Li1 3.049(6) . ? P1 C1 1.825(4) . ? P1 Li2 2.617(5) . ? P1 Li1 2.724(6) . ? P2 C6 1.793(4) . ? P2 Li2 2.583(6) 2_746 ? P2 Li1 2.698(6) . ? C1 C2 1.400(6) . ? C1 C6 1.458(5) . ? C1 Li1 2.551(8) . ? C2 C3 1.358(7) . ? C3 C4 1.405(6) . ? C4 C5 1.365(6) . ? C5 C6 1.399(6) . ? C6 Li1 2.563(8) . ? Li1 N2 2.066(9) . ? Li1 N2A 2.116(10) . ? Li1 N1 2.127(10) . ? Li1 N1A 2.154(10) . ? N1 C9 1.439(8) . ? N1 C8 1.440(8) . ? N1 C7 1.487(8) . ? N2 C10 1.453(8) . ? N2 C12 1.487(9) . ? N2 C11 1.504(8) . ? C9 C10 1.443(8) . ? N1A C7A 1.475(8) . ? N1A C9A 1.485(8) . ? N1A C8A 1.511(9) . ? N2A C10A 1.464(9) . ? N2A C11A 1.476(8) . ? N2A C12A 1.509(8) . ? C9A C10A 1.539(9) . ? Li2 N3 2.123(8) . ? Li2 N4 2.178(7) . ? Li2 P2 2.583(6) 2_756 ? N3 C14 1.465(7) . ? N3 C15 1.482(5) . ? N3 C13 1.491(9) . ? N4 C17 1.454(9) . ? N4 C16 1.464(6) . ? N4 C18 1.477(6) . ? C15 C16 1.497(6) . ? 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 P2 Sn1 P1 87.79(3) . . ? P2 Sn1 Li1 57.44(11) . . ? P1 Sn1 Li1 58.00(12) . . ? C1 P1 Sn1 102.72(11) . . ? C1 P1 Li2 125.08(17) . . ? Sn1 P1 Li2 132.19(13) . . ? C1 P1 Li1 64.73(19) . . ? Sn1 P1 Li1 71.68(13) . . ? Li2 P1 Li1 126.83(19) . . ? C6 P2 Sn1 103.26(12) . . ? C6 P2 Li2 121.48(18) . 2_746 ? Sn1 P2 Li2 135.25(14) . 2_746 ? C6 P2 Li1 66.1(2) . . ? Sn1 P2 Li1 72.29(11) . . ? Li2 P2 Li1 124.6(2) 2_746 . ? C2 C1 C6 117.1(4) . . ? C2 C1 P1 120.6(3) . . ? C6 C1 P1 122.2(3) . . ? C2 C1 Li1 127.0(3) . . ? C6 C1 Li1 73.9(3) . . ? P1 C1 Li1 75.0(2) . . ? C3 C2 C1 123.5(4) . . ? C2 C3 C4 120.0(5) . . ? C5 C4 C3 118.3(4) . . ? C4 C5 C6 124.1(4) . . ? C5 C6 C1 117.1(4) . . ? C5 C6 P2 119.5(3) . . ? C1 C6 P2 123.5(3) . . ? C5 C6 Li1 126.2(4) . . ? C1 C6 Li1 73.0(3) . . ? P2 C6 Li1 74.2(2) . . ? N2 Li1 N1 83.4(4) . . ? N2A Li1 N1 84.9(4) . . ? N2 Li1 N1A 85.9(4) . . ? N2A Li1 N1A 88.7(4) . . ? N2 Li1 C1 105.0(3) . . ? N2A Li1 C1 107.0(4) . . ? N1 Li1 C1 156.4(4) . . ? N1A Li1 C1 147.6(4) . . ? N2 Li1 C6 102.3(3) . . ? N2A Li1 C6 99.0(3) . . ? N1 Li1 C6 167.3(4) . . ? N1A Li1 C6 171.3(3) . . ? C1 Li1 C6 33.12(15) . . ? N2 Li1 P2 123.4(3) . . ? N2A Li1 P2 115.4(3) . . ? N1 Li1 P2 127.7(3) . . ? N1A Li1 P2 132.7(4) . . ? C1 Li1 P2 66.16(16) . . ? C6 Li1 P2 39.75(12) . . ? N2 Li1 P1 132.3(4) . . ? N2A Li1 P1 139.0(4) . . ? N1 Li1 P1 118.5(3) . . ? N1A Li1 P1 110.7(3) . . ? C1 Li1 P1 40.32(13) . . ? C6 Li1 P1 65.93(18) . . ? P2 Li1 P1 78.23(16) . . ? N2 Li1 Sn1 173.6(4) . . ? N2A Li1 Sn1 164.6(4) . . ? N1 Li1 Sn1 100.3(3) . . ? N1A Li1 Sn1 98.6(3) . . ? C1 Li1 Sn1 73.67(17) . . ? C6 Li1 Sn1 73.00(17) . . ? P2 Li1 Sn1 50.27(10) . . ? P1 Li1 Sn1 50.32(10) . . ? C9 N1 C8 91.7(8) . . ? C9 N1 C7 107.7(9) . . ? C8 N1 C7 116.4(9) . . ? C9 N1 Li1 110.6(6) . . ? C8 N1 Li1 116.2(7) . . ? C7 N1 Li1 112.0(9) . . ? C10 N2 C12 111.5(10) . . ? C10 N2 C11 105.1(10) . . ? C12 N2 C11 108.6(10) . . ? C10 N2 Li1 107.2(7) . . ? C12 N2 Li1 117.5(10) . . ? C11 N2 Li1 106.0(7) . . ? N1 C9 C10 111.2(9) . . ? C9 C10 N2 120.0(8) . . ? C7A N1A C9A 110.9(9) . . ? C7A N1A C8A 97.6(12) . . ? C9A N1A C8A 122.4(12) . . ? C7A N1A Li1 111.9(8) . . ? C9A N1A Li1 98.2(7) . . ? C8A N1A Li1 116.4(9) . . ? C10A N2A C11A 117.2(10) . . ? C10A N2A C12A 111.8(13) . . ? C11A N2A C12A 105.3(9) . . ? C10A N2A Li1 101.1(7) . . ? C11A N2A Li1 115.3(6) . . ? C12A N2A Li1 105.7(9) . . ? N1A C9A C10A 111.4(9) . . ? N2A C10A C9A 109.5(10) . . ? N3 Li2 N4 85.3(3) . . ? N3 Li2 P2 109.0(3) . 2_756 ? N4 Li2 P2 105.9(2) . 2_756 ? N3 Li2 P1 112.8(3) . . ? N4 Li2 P1 118.0(3) . . ? P2 Li2 P1 120.3(2) 2_756 . ? C14 N3 C15 109.0(4) . . ? C14 N3 C13 107.3(7) . . ? C15 N3 C13 113.1(6) . . ? C14 N3 Li2 114.5(4) . . ? C15 N3 Li2 102.2(3) . . ? C13 N3 Li2 110.9(7) . . ? C17 N4 C16 109.8(5) . . ? C17 N4 C18 108.2(5) . . ? C16 N4 C18 109.8(4) . . ? C17 N4 Li2 116.0(4) . . ? C16 N4 Li2 103.3(3) . . ? C18 N4 Li2 109.7(3) . . ? N3 C15 C16 111.0(4) . . ? N4 C16 C15 111.9(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.230 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.054