Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'D. 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_section_title ; Stepwise nucleophilic substitution of manganocene; syntheses and structures of the dimer [CpMn(hpp)]2 and the unusual manganate cage [(hpp)3MnLi]2 (hppH= 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2,a]pyrimidine) ; loop_ _publ_author_name 'D. S. Wright' 'Christine Brinkmann' 'Felipe Garcia' 'M. McPartlin' 'James V. Morey' 'Sanjay Singh' ; A.E.H.Wheatley ; data_mw0601 _database_code_depnum_ccdc_archive 'CCDC 633166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Mn2 N6' _chemical_formula_weight 516.45 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' Mn Mn 0.3368 0.7283 '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 8.2486(16) _cell_length_b 9.0047(18) _cell_length_c 9.1825(18) _cell_angle_alpha 77.67(3) _cell_angle_beta 67.55(3) _cell_angle_gamma 83.75(3) _cell_volume 615.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3986 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description blocks _exptl_crystal_colour green/brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 270 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _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 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 5349 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2379 _reflns_number_gt 2274 _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 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0474P)^2^+0.1164P] 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 2379 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Mn1 Mn -0.13271(2) 0.12426(2) 0.03928(2) 0.02303(10) Uani 1 1 d . . . N1 N -0.00902(15) 0.18347(14) -0.21771(14) 0.0266(3) Uani 1 1 d . . . N2 N 0.28206(15) 0.27144(14) -0.33245(14) 0.0284(3) Uani 1 1 d . . . N3 N 0.16195(14) 0.11822(13) -0.07157(13) 0.0233(2) Uani 1 1 d . . . C1 C -0.0436(2) 0.2506(2) -0.36248(19) 0.0411(4) Uani 1 1 d . . . H1A H -0.1111 0.3450 -0.3469 0.049 Uiso 1 1 calc R . . H1B H -0.1137 0.1820 -0.3809 0.049 Uiso 1 1 calc R . . C2 C 0.1246(2) 0.2825(2) -0.50994(18) 0.0408(4) Uani 1 1 d . . . H2A H 0.1787 0.1876 -0.5422 0.049 Uiso 1 1 calc R . . H2B H 0.0976 0.3453 -0.5982 0.049 Uiso 1 1 calc R . . C3 C 0.2497(2) 0.36339(18) -0.47072(18) 0.0343(3) Uani 1 1 d . . . H3A H 0.3594 0.3793 -0.5622 0.041 Uiso 1 1 calc R . . H3B H 0.1995 0.4619 -0.4468 0.041 Uiso 1 1 calc R . . C4 C 0.44032(18) 0.30355(18) -0.31017(18) 0.0319(3) Uani 1 1 d . . . H4A H 0.4285 0.4043 -0.2848 0.038 Uiso 1 1 calc R . . H4B H 0.5407 0.3023 -0.4093 0.038 Uiso 1 1 calc R . . C5 C 0.47138(19) 0.18797(19) -0.1769(2) 0.0352(3) Uani 1 1 d . . . H5A H 0.5117 0.0918 -0.2123 0.042 Uiso 1 1 calc R . . H5B H 0.5611 0.2228 -0.1491 0.042 Uiso 1 1 calc R . . C6 C 0.30098(19) 0.16664(18) -0.03103(18) 0.0316(3) Uani 1 1 d . . . H6A H 0.3198 0.0908 0.0539 0.038 Uiso 1 1 calc R . . H6B H 0.2651 0.2616 0.0079 0.038 Uiso 1 1 calc R . . C7 C 0.14676(17) 0.19512(15) -0.21224(16) 0.0232(3) Uani 1 1 d . . . C11 C -0.2940(3) 0.3681(2) 0.0987(3) 0.0580(5) Uani 1 1 d . . . H11 H -0.3016 0.4438 0.0149 0.070 Uiso 1 1 calc R . . C12 C -0.1652(3) 0.3539(2) 0.1657(3) 0.0586(6) Uani 1 1 d . . . H12 H -0.0722 0.4184 0.1343 0.070 Uiso 1 1 calc R . . C13 C -0.2007(3) 0.2274(3) 0.2866(2) 0.0525(5) Uani 1 1 d . . . H13 H -0.1352 0.1917 0.3506 0.063 Uiso 1 1 calc R . . C14 C -0.3520(2) 0.1616(2) 0.2969(2) 0.0489(5) Uani 1 1 d . . . H14 H -0.4050 0.0754 0.3690 0.059 Uiso 1 1 calc R . . C15 C -0.4086(2) 0.2493(3) 0.1791(2) 0.0510(5) Uani 1 1 d . . . H15 H -0.5058 0.2313 0.1581 0.061 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 Mn1 0.02152(14) 0.02179(15) 0.02220(15) -0.00468(10) -0.00391(10) -0.00042(9) N1 0.0227(6) 0.0318(6) 0.0226(6) 0.0004(5) -0.0078(4) -0.0024(5) N2 0.0249(6) 0.0275(6) 0.0270(6) 0.0016(5) -0.0056(5) -0.0051(5) N3 0.0219(5) 0.0234(6) 0.0246(6) -0.0024(4) -0.0089(4) -0.0034(4) C1 0.0316(8) 0.0573(11) 0.0299(8) 0.0066(7) -0.0137(6) -0.0040(7) C2 0.0415(9) 0.0528(10) 0.0232(7) 0.0048(7) -0.0111(6) -0.0074(7) C3 0.0363(8) 0.0306(8) 0.0253(7) 0.0046(6) -0.0039(6) -0.0046(6) C4 0.0250(7) 0.0311(8) 0.0343(8) -0.0082(6) -0.0018(6) -0.0093(6) C5 0.0241(7) 0.0387(8) 0.0456(9) -0.0094(7) -0.0139(6) -0.0050(6) C6 0.0316(7) 0.0342(8) 0.0332(8) -0.0040(6) -0.0161(6) -0.0071(6) C7 0.0236(6) 0.0199(6) 0.0228(6) -0.0042(5) -0.0050(5) -0.0003(5) C11 0.0798(15) 0.0368(10) 0.0526(11) -0.0198(9) -0.0187(10) 0.0196(9) C12 0.0521(11) 0.0539(12) 0.0689(14) -0.0386(11) -0.0045(9) -0.0109(9) C13 0.0495(10) 0.0743(14) 0.0448(10) -0.0364(10) -0.0197(8) 0.0117(9) C14 0.0491(10) 0.0529(11) 0.0345(9) -0.0207(8) 0.0036(7) -0.0061(8) C15 0.0331(8) 0.0715(13) 0.0568(11) -0.0424(10) -0.0136(8) 0.0127(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 Mn1 N1 2.1533(14) . ? Mn1 N3 2.1673(12) 2 ? Mn1 N3 2.2477(13) . ? Mn1 C15 2.4335(19) . ? Mn1 C14 2.4334(19) . ? Mn1 C13 2.4798(18) . ? Mn1 C11 2.492(2) . ? Mn1 C12 2.5227(19) . ? Mn1 C7 2.5847(17) . ? Mn1 Mn1 2.9561(11) 2 ? N1 C7 1.3212(17) . ? N1 C1 1.4571(19) . ? N2 C7 1.3560(18) . ? N2 C4 1.4632(18) . ? N2 C3 1.460(2) . ? N3 C7 1.3735(18) . ? N3 C6 1.4656(17) . ? N3 Mn1 2.1673(12) 2 ? C1 C2 1.526(2) . ? C2 C3 1.512(2) . ? C4 C5 1.511(2) . ? C5 C6 1.523(2) . ? C11 C15 1.390(3) . ? C11 C12 1.400(3) . ? C12 C13 1.378(3) . ? C13 C14 1.402(3) . ? C14 C15 1.397(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mn1 N3 101.12(6) . 2 ? N1 Mn1 N3 61.45(5) . . ? N3 Mn1 N3 95.96(5) 2 . ? N1 Mn1 C15 120.11(7) . . ? N3 Mn1 C15 111.35(7) 2 . ? N3 Mn1 C15 150.73(6) . . ? N1 Mn1 C14 152.92(6) . . ? N3 Mn1 C14 97.40(7) 2 . ? N3 Mn1 C14 135.87(6) . . ? C15 Mn1 C14 33.37(7) . . ? N1 Mn1 C13 141.60(7) . . ? N3 Mn1 C13 116.32(7) 2 . ? N3 Mn1 C13 104.33(6) . . ? C15 Mn1 C13 54.66(7) . . ? C14 Mn1 C13 33.14(7) . . ? N1 Mn1 C11 100.10(7) . . ? N3 Mn1 C11 143.99(7) 2 . ? N3 Mn1 C11 119.76(7) . . ? C15 Mn1 C11 32.76(8) . . ? C14 Mn1 C11 54.47(8) . . ? C13 Mn1 C11 53.70(8) . . ? N1 Mn1 C12 110.61(7) . . ? N3 Mn1 C12 148.17(6) 2 . ? N3 Mn1 C12 96.86(6) . . ? C15 Mn1 C12 54.23(7) . . ? C14 Mn1 C12 54.17(7) . . ? C13 Mn1 C12 31.97(8) . . ? C11 Mn1 C12 32.42(7) . . ? N1 Mn1 C7 30.69(4) . . ? N3 Mn1 C7 106.68(5) 2 . ? N3 Mn1 C7 32.07(4) . . ? C15 Mn1 C7 137.15(7) . . ? C14 Mn1 C7 153.46(6) . . ? C13 Mn1 C7 122.11(6) . . ? C11 Mn1 C7 106.44(7) . . ? C12 Mn1 C7 99.56(6) . . ? N1 Mn1 Mn1 77.17(5) . 2 ? N3 Mn1 Mn1 49.14(4) 2 2 ? N3 Mn1 Mn1 46.82(4) . 2 ? C15 Mn1 Mn1 158.46(6) . 2 ? C14 Mn1 Mn1 129.80(6) . 2 ? C13 Mn1 Mn1 120.88(6) . 2 ? C11 Mn1 Mn1 166.04(6) . 2 ? C12 Mn1 Mn1 135.54(6) . 2 ? C7 Mn1 Mn1 64.28(4) . 2 ? C7 N1 C1 120.25(12) . . ? C7 N1 Mn1 93.01(9) . . ? C1 N1 Mn1 142.89(10) . . ? C7 N2 C4 122.34(12) . . ? C7 N2 C3 118.46(12) . . ? C4 N2 C3 116.57(12) . . ? C7 N3 C6 116.27(11) . . ? C7 N3 Mn1 111.73(8) . 2 ? C6 N3 Mn1 117.22(9) . 2 ? C7 N3 Mn1 87.61(8) . . ? C6 N3 Mn1 134.13(9) . . ? Mn1 N3 Mn1 84.04(5) 2 . ? N1 C1 C2 112.40(13) . . ? C3 C2 C1 109.36(14) . . ? N2 C3 C2 109.27(12) . . ? N2 C4 C5 111.32(12) . . ? C6 C5 C4 109.27(13) . . ? N3 C6 C5 110.77(12) . . ? N1 C7 N3 113.22(12) . . ? N1 C7 N2 124.79(13) . . ? N3 C7 N2 121.98(12) . . ? N1 C7 Mn1 56.30(7) . . ? N3 C7 Mn1 60.33(7) . . ? N2 C7 Mn1 163.80(10) . . ? C15 C11 C12 108.2(2) . . ? C15 C11 Mn1 71.32(10) . . ? C12 C11 Mn1 75.01(11) . . ? C13 C12 C11 107.81(19) . . ? C13 C12 Mn1 72.30(11) . . ? C11 C12 Mn1 72.57(10) . . ? C12 C13 C14 108.63(19) . . ? C12 C13 Mn1 75.73(11) . . ? C14 C13 Mn1 71.61(10) . . ? C15 C14 C13 107.41(18) . . ? C15 C14 Mn1 73.32(10) . . ? C13 C14 Mn1 75.25(10) . . ? C14 C15 C11 107.95(17) . . ? C14 C15 Mn1 73.31(10) . . ? C11 C15 Mn1 75.92(11) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.251 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.041 # Attachment 'mw0603.cif' data_mw0603 _database_code_depnum_ccdc_archive 'CCDC 633167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H72 Li2 Mn2 N18' _chemical_formula_weight 952.94 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' Mn Mn 0.3368 0.7283 '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 14.668(3) _cell_length_b 18.026(4) _cell_length_c 18.697(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.01(3) _cell_angle_gamma 90.00 _cell_volume 4727.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 16469 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.869 _exptl_absorpt_correction_T_max 0.933 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _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 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 25912 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9235 _reflns_number_gt 7110 _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 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0296P)^2^+4.8780P] 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 9235 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Mn1 Mn 0.22642(4) 0.88653(3) 0.09520(3) 0.02324(17) Uani 0.5207(8) 1 d P A 1 Mn2 Mn 0.31094(4) 0.89872(4) 0.30884(3) 0.02355(17) Uani 0.5207(8) 1 d P A 1 Li1 Li 0.13649(5) 0.88537(4) 0.20406(4) 0.02350(18) Uani 0.5207(8) 1 d P A 1 Li2 Li 0.39445(5) 0.93223(4) 0.19695(4) 0.02351(18) Uani 0.5207(8) 1 d P A 1 Li1' Li 0.22642(4) 0.88653(3) 0.09520(3) 0.02324(17) Uani 0.4793(8) 1 d P A 2 Li2' Li 0.31094(4) 0.89872(4) 0.30884(3) 0.02355(17) Uani 0.4793(8) 1 d P A 2 Mn1' Mn 0.13649(5) 0.88537(4) 0.20406(4) 0.02350(18) Uani 0.4793(8) 1 d P A 2 Mn2' Mn 0.39445(5) 0.93223(4) 0.19695(4) 0.02351(18) Uani 0.4793(8) 1 d P A 2 N1 N 0.17886(13) 0.97510(10) 0.14549(10) 0.0235(4) Uani 1 1 d . . . N2 N 0.21081(15) 1.09777(11) 0.19019(11) 0.0287(5) Uani 1 1 d . . . N3 N 0.30647(13) 0.99710(10) 0.24956(10) 0.0231(4) Uani 1 1 d . . . N4 N 0.10810(15) 0.93934(12) 0.29410(11) 0.0293(5) Uani 1 1 d . . . N5 N 0.11856(15) 0.98261(12) 0.41566(12) 0.0337(5) Uani 1 1 d . . . N6 N 0.24439(14) 0.91581(11) 0.38914(11) 0.0283(5) Uani 1 1 d . . . N7 N 0.38782(15) 0.99581(11) 0.10285(11) 0.0284(5) Uani 1 1 d . . . N8 N 0.34309(15) 1.03556(11) -0.02323(11) 0.0312(5) Uani 1 1 d . . . N9 N 0.28253(15) 0.92480(11) 0.01372(11) 0.0277(5) Uani 1 1 d . . . N10 N 0.02176(15) 0.83584(12) 0.12729(12) 0.0311(5) Uani 1 1 d . . . N11 N -0.02121(15) 0.73850(12) 0.03845(13) 0.0366(5) Uani 1 1 d . . . N12 N 0.12301(14) 0.80462(11) 0.05918(12) 0.0289(5) Uani 1 1 d . . . N13 N 0.24301(14) 0.80612(10) 0.24317(11) 0.0250(4) Uani 1 1 d . . . N14 N 0.31925(15) 0.70269(11) 0.20804(12) 0.0285(5) Uani 1 1 d . . . N15 N 0.34231(14) 0.82483(11) 0.16944(11) 0.0244(4) Uani 1 1 d . . . N16 N 0.45093(14) 0.86296(11) 0.35344(11) 0.0291(5) Uani 1 1 d . . . N17 N 0.61640(15) 0.84708(12) 0.37371(12) 0.0329(5) Uani 1 1 d . . . N18 N 0.52382(14) 0.92524(11) 0.27753(11) 0.0287(5) Uani 1 1 d . . . C1 C 0.0985(2) 1.00573(15) 0.08645(16) 0.0417(7) Uani 1 1 d . A . H1A H 0.0801 0.9709 0.0452 0.050 Uiso 1 1 calc R . . H1B H 0.0444 1.0123 0.1058 0.050 Uiso 1 1 calc R . . C2 C 0.1230(2) 1.07856(15) 0.05850(15) 0.0399(7) Uani 1 1 d . . . H2A H 0.1770 1.0728 0.0389 0.048 Uiso 1 1 calc R A . H2B H 0.0693 1.0971 0.0188 0.048 Uiso 1 1 calc R . . C3 C 0.1473(2) 1.13175(15) 0.12328(16) 0.0437(7) Uani 1 1 d . A . H3A H 0.0891 1.1475 0.1336 0.052 Uiso 1 1 calc R . . H3B H 0.1777 1.1754 0.1102 0.052 Uiso 1 1 calc R . . C4 C 0.2511(2) 1.14962(15) 0.25069(15) 0.0415(7) Uani 1 1 d . A . H4A H 0.2010 1.1814 0.2576 0.050 Uiso 1 1 calc R . . H4B H 0.2978 1.1808 0.2377 0.050 Uiso 1 1 calc R . . C5 C 0.2979(2) 1.10904(15) 0.32259(14) 0.0356(6) Uani 1 1 d . . . H5A H 0.2501 1.0861 0.3419 0.043 Uiso 1 1 calc R A . H5B H 0.3352 1.1431 0.3599 0.043 Uiso 1 1 calc R . . C6 C 0.36159(19) 1.05055(15) 0.30437(15) 0.0355(6) Uani 1 1 d . A . H6A H 0.4084 1.0743 0.2846 0.043 Uiso 1 1 calc R . . H6B H 0.3954 1.0246 0.3498 0.043 Uiso 1 1 calc R . . C7 C 0.23187(16) 1.02374(13) 0.19490(13) 0.0225(5) Uani 1 1 d . A . C8 C 0.02254(19) 0.98534(16) 0.27031(14) 0.0359(6) Uani 1 1 d . A . H8A H -0.0133 0.9726 0.2195 0.043 Uiso 1 1 calc R . . H8B H 0.0406 1.0372 0.2711 0.043 Uiso 1 1 calc R . . C9 C -0.03905(19) 0.97359(17) 0.32174(15) 0.0399(7) Uani 1 1 d . . . H9A H -0.0556 0.9216 0.3226 0.048 Uiso 1 1 calc R A . H9B H -0.0974 1.0021 0.3043 0.048 Uiso 1 1 calc R . . C10 C 0.01713(19) 0.99868(16) 0.39875(15) 0.0359(6) Uani 1 1 d . A . H10A H 0.0086 1.0517 0.4030 0.043 Uiso 1 1 calc R . . H10B H -0.0076 0.9743 0.4354 0.043 Uiso 1 1 calc R . . C11 C 0.1716(2) 0.99414(16) 0.49338(14) 0.0379(7) Uani 1 1 d . A . H11A H 0.1528 0.9572 0.5240 0.045 Uiso 1 1 calc R . . H11B H 0.1564 1.0427 0.5092 0.045 Uiso 1 1 calc R . . C12 C 0.2778(2) 0.98887(15) 0.50479(15) 0.0383(7) Uani 1 1 d . . . H12A H 0.3118 0.9885 0.5578 0.046 Uiso 1 1 calc R A . H12B H 0.2995 1.0311 0.4820 0.046 Uiso 1 1 calc R . . C13 C 0.29610(19) 0.91808(15) 0.46879(14) 0.0353(6) Uani 1 1 d . A . H13A H 0.3639 0.9135 0.4751 0.042 Uiso 1 1 calc R . . H13B H 0.2768 0.8763 0.4937 0.042 Uiso 1 1 calc R . . C14 C 0.15737(17) 0.94460(13) 0.36629(13) 0.0256(5) Uani 1 1 d . A . C15 C 0.4314(2) 1.06866(14) 0.11980(15) 0.0347(6) Uani 1 1 d . A . H15A H 0.4746 1.0688 0.1703 0.042 Uiso 1 1 calc R . . H15B H 0.3824 1.1055 0.1171 0.042 Uiso 1 1 calc R . . C16 C 0.4860(2) 1.08844(15) 0.06489(17) 0.0399(7) Uani 1 1 d . . . H16A H 0.5180 1.1357 0.0783 0.048 Uiso 1 1 calc R A . H16B H 0.5336 1.0509 0.0658 0.048 Uiso 1 1 calc R . . C17 C 0.4158(2) 1.09295(15) -0.01158(16) 0.0407(7) Uani 1 1 d . A . H17A H 0.3853 1.1413 -0.0180 0.049 Uiso 1 1 calc R . . H17B H 0.4494 1.0879 -0.0489 0.049 Uiso 1 1 calc R . . C18 C 0.2814(2) 1.03209(16) -0.09975(14) 0.0384(7) Uani 1 1 d . A . H18A H 0.3185 1.0167 -0.1324 0.046 Uiso 1 1 calc R . . H18B H 0.2561 1.0811 -0.1153 0.046 Uiso 1 1 calc R . . C19 C 0.2001(2) 0.97893(16) -0.10783(15) 0.0405(7) Uani 1 1 d . . . H19A H 0.1523 1.0008 -0.0879 0.049 Uiso 1 1 calc R A . H19B H 0.1706 0.9675 -0.1602 0.049 Uiso 1 1 calc R . . C20 C 0.2390(2) 0.90933(15) -0.06553(14) 0.0360(6) Uani 1 1 d . A . H20A H 0.1878 0.8737 -0.0712 0.043 Uiso 1 1 calc R . . H20B H 0.2863 0.8876 -0.0863 0.043 Uiso 1 1 calc R . . C21 C 0.33826(17) 0.98467(13) 0.03098(13) 0.0239(5) Uani 1 1 d . A . C22 C -0.0719(2) 0.82849(18) 0.13828(18) 0.0469(8) Uani 1 1 d . A . H22A H -0.1165 0.8599 0.1025 0.056 Uiso 1 1 calc R . . H22B H -0.0687 0.8459 0.1880 0.056 Uiso 1 1 calc R . . C23 C -0.1080(3) 0.7516(2) 0.1296(2) 0.0677(10) Uani 1 1 d . . . H23A H -0.1725 0.7509 0.1334 0.081 Uiso 1 1 calc R A . H23B H -0.0686 0.7212 0.1696 0.081 Uiso 1 1 calc R . . C24 C -0.1073(2) 0.72040(17) 0.05723(19) 0.0498(8) Uani 1 1 d . A . H24A H -0.1135 0.6669 0.0588 0.060 Uiso 1 1 calc R . . H24B H -0.1618 0.7392 0.0185 0.060 Uiso 1 1 calc R . . C25 C -0.0126(2) 0.69983(15) -0.02763(16) 0.0420(7) Uani 1 1 d . A . H25A H -0.0712 0.7062 -0.0679 0.050 Uiso 1 1 calc R . . H25B H -0.0045 0.6472 -0.0167 0.050 Uiso 1 1 calc R . . C26 C 0.0700(2) 0.72722(16) -0.05319(16) 0.0395(7) Uani 1 1 d . . . H26A H 0.0900 0.6891 -0.0820 0.047 Uiso 1 1 calc R A . H26B H 0.0514 0.7709 -0.0844 0.047 Uiso 1 1 calc R . . C27 C 0.15033(19) 0.74589(15) 0.01579(15) 0.0344(6) Uani 1 1 d . A . H27A H 0.1680 0.7019 0.0466 0.041 Uiso 1 1 calc R . . H27B H 0.2055 0.7617 0.0011 0.041 Uiso 1 1 calc R . . C28 C 0.04093(17) 0.79389(13) 0.07507(13) 0.0258(5) Uani 1 1 d . A . C29 C 0.2021(2) 0.75318(14) 0.28492(16) 0.0395(7) Uani 1 1 d . A . H29A H 0.2492 0.7409 0.3318 0.047 Uiso 1 1 calc R . . H29B H 0.1479 0.7756 0.2963 0.047 Uiso 1 1 calc R . . C30 C 0.1705(2) 0.68302(14) 0.23956(17) 0.0379(7) Uani 1 1 d . . . H30A H 0.1251 0.6949 0.1917 0.046 Uiso 1 1 calc R A . H30B H 0.1403 0.6494 0.2661 0.046 Uiso 1 1 calc R . . C31 C 0.2576(2) 0.64770(14) 0.22795(16) 0.0378(7) Uani 1 1 d . A . H31A H 0.2928 0.6224 0.2734 0.045 Uiso 1 1 calc R . . H31B H 0.2385 0.6110 0.1884 0.045 Uiso 1 1 calc R . . C32 C 0.3969(2) 0.67098(15) 0.18465(16) 0.0383(7) Uani 1 1 d . A . H32A H 0.3714 0.6459 0.1371 0.046 Uiso 1 1 calc R . . H32B H 0.4303 0.6346 0.2212 0.046 Uiso 1 1 calc R . . C33 C 0.4658(2) 0.73067(16) 0.17697(17) 0.0404(7) Uani 1 1 d . . . H33A H 0.5020 0.7488 0.2259 0.048 Uiso 1 1 calc R A . H33B H 0.5101 0.7110 0.1520 0.048 Uiso 1 1 calc R . . C34 C 0.4078(2) 0.79256(16) 0.13151(16) 0.0387(7) Uani 1 1 d . A . H34A H 0.4502 0.8309 0.1235 0.046 Uiso 1 1 calc R . . H34B H 0.3714 0.7736 0.0830 0.046 Uiso 1 1 calc R . . C35 C 0.30175(16) 0.77765(13) 0.20683(12) 0.0223(5) Uani 1 1 d . A . C36 C 0.4590(2) 0.80132(15) 0.40506(15) 0.0366(6) Uani 1 1 d . A . H36A H 0.4650 0.7553 0.3800 0.044 Uiso 1 1 calc R . . H36B H 0.4019 0.7985 0.4210 0.044 Uiso 1 1 calc R . . C37 C 0.5453(2) 0.81144(16) 0.47264(15) 0.0392(7) Uani 1 1 d . . . H37A H 0.5484 0.7719 0.5085 0.047 Uiso 1 1 calc R A . H37B H 0.5415 0.8585 0.4968 0.047 Uiso 1 1 calc R . . C38 C 0.63219(19) 0.80963(15) 0.44514(15) 0.0373(7) Uani 1 1 d . A . H38A H 0.6850 0.8332 0.4819 0.045 Uiso 1 1 calc R . . H38B H 0.6497 0.7584 0.4401 0.045 Uiso 1 1 calc R . . C39 C 0.70090(18) 0.85049(16) 0.34876(15) 0.0367(6) Uani 1 1 d . A . H39A H 0.7271 0.8010 0.3494 0.044 Uiso 1 1 calc R . . H39B H 0.7485 0.8810 0.3831 0.044 Uiso 1 1 calc R . . C40 C 0.6796(2) 0.88235(17) 0.27035(16) 0.0414(7) Uani 1 1 d . . . H40A H 0.7381 0.8981 0.2607 0.050 Uiso 1 1 calc R A . H40B H 0.6491 0.8453 0.2335 0.050 Uiso 1 1 calc R . . C41 C 0.61369(19) 0.94805(16) 0.26600(16) 0.0374(6) Uani 1 1 d . A . H41A H 0.6445 0.9842 0.3037 0.045 Uiso 1 1 calc R . . H41B H 0.6013 0.9714 0.2174 0.045 Uiso 1 1 calc R . . C42 C 0.53006(17) 0.87930(13) 0.33515(13) 0.0259(5) Uani 1 1 d . A . 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 Mn1 0.0231(3) 0.0242(3) 0.0218(3) 0.0014(3) 0.0056(3) -0.0015(3) Mn2 0.0233(3) 0.0254(3) 0.0217(3) 0.0009(3) 0.0062(3) 0.0019(3) Li1 0.0240(4) 0.0242(4) 0.0226(4) -0.0008(3) 0.0073(3) -0.0007(3) Li2 0.0216(4) 0.0253(4) 0.0227(4) 0.0012(3) 0.0049(3) 0.0017(3) Li1' 0.0231(3) 0.0242(3) 0.0218(3) 0.0014(3) 0.0056(3) -0.0015(3) Li2' 0.0233(3) 0.0254(3) 0.0217(3) 0.0009(3) 0.0062(3) 0.0019(3) Mn1' 0.0240(4) 0.0242(4) 0.0226(4) -0.0008(3) 0.0073(3) -0.0007(3) Mn2' 0.0216(4) 0.0253(4) 0.0227(4) 0.0012(3) 0.0049(3) 0.0017(3) N1 0.0231(10) 0.0224(10) 0.0213(10) 0.0013(8) 0.0010(8) -0.0010(8) N2 0.0335(12) 0.0203(10) 0.0269(11) 0.0002(9) 0.0006(9) 0.0020(9) N3 0.0226(10) 0.0240(10) 0.0199(10) -0.0003(8) 0.0021(8) -0.0019(8) N4 0.0299(11) 0.0351(12) 0.0248(11) -0.0030(9) 0.0110(9) 0.0029(9) N5 0.0343(12) 0.0418(13) 0.0276(11) -0.0055(10) 0.0133(9) 0.0057(10) N6 0.0290(11) 0.0319(11) 0.0256(11) 0.0002(9) 0.0105(9) 0.0015(9) N7 0.0344(12) 0.0258(11) 0.0248(11) 0.0008(9) 0.0083(9) -0.0030(9) N8 0.0378(12) 0.0300(11) 0.0290(11) 0.0062(10) 0.0148(10) -0.0010(10) N9 0.0326(12) 0.0298(11) 0.0222(10) -0.0001(9) 0.0101(9) -0.0036(9) N10 0.0252(11) 0.0330(12) 0.0333(12) -0.0047(10) 0.0060(9) -0.0013(9) N11 0.0297(12) 0.0338(12) 0.0443(13) -0.0113(11) 0.0078(10) -0.0089(10) N12 0.0246(11) 0.0264(11) 0.0340(12) -0.0053(9) 0.0060(9) -0.0048(9) N13 0.0299(11) 0.0215(10) 0.0258(10) 0.0010(8) 0.0114(9) 0.0009(8) N14 0.0322(12) 0.0213(10) 0.0334(11) 0.0016(9) 0.0116(9) 0.0035(9) N15 0.0252(11) 0.0233(10) 0.0264(10) 0.0016(9) 0.0102(9) 0.0025(8) N16 0.0258(11) 0.0296(11) 0.0295(11) 0.0056(9) 0.0041(9) 0.0029(9) N17 0.0229(11) 0.0405(12) 0.0312(12) 0.0072(10) 0.0016(9) 0.0085(9) N18 0.0249(11) 0.0324(11) 0.0260(11) 0.0044(9) 0.0031(9) 0.0019(9) C1 0.0380(16) 0.0354(15) 0.0385(16) 0.0098(13) -0.0095(12) 0.0002(12) C2 0.0438(17) 0.0357(15) 0.0310(14) 0.0081(12) -0.0032(12) 0.0009(12) C3 0.0524(19) 0.0278(14) 0.0386(16) 0.0051(13) -0.0058(14) 0.0091(13) C4 0.0539(19) 0.0268(14) 0.0364(15) -0.0058(12) 0.0015(13) 0.0040(13) C5 0.0413(16) 0.0343(14) 0.0289(13) -0.0103(12) 0.0067(12) -0.0002(12) C6 0.0314(15) 0.0360(15) 0.0324(14) -0.0078(12) -0.0010(11) 0.0002(11) C7 0.0221(12) 0.0239(12) 0.0232(12) 0.0012(10) 0.0095(9) 0.0007(10) C8 0.0361(15) 0.0441(16) 0.0270(13) -0.0008(12) 0.0082(11) 0.0077(12) C9 0.0327(15) 0.0473(17) 0.0414(16) -0.0023(14) 0.0136(12) 0.0075(13) C10 0.0387(16) 0.0384(15) 0.0355(15) 0.0002(12) 0.0183(12) 0.0085(12) C11 0.0501(18) 0.0388(15) 0.0266(13) -0.0073(12) 0.0140(12) 0.0054(13) C12 0.0428(17) 0.0397(16) 0.0290(14) -0.0053(12) 0.0052(12) -0.0022(13) C13 0.0335(15) 0.0414(16) 0.0307(14) 0.0021(12) 0.0090(12) 0.0021(12) C14 0.0303(13) 0.0226(12) 0.0274(13) -0.0006(10) 0.0137(11) -0.0004(10) C15 0.0381(15) 0.0287(13) 0.0360(15) -0.0044(12) 0.0089(12) -0.0002(11) C16 0.0406(16) 0.0262(14) 0.0576(18) -0.0068(13) 0.0218(14) -0.0081(12) C17 0.0567(19) 0.0261(14) 0.0484(17) 0.0040(13) 0.0295(15) -0.0027(13) C18 0.0470(17) 0.0455(16) 0.0259(13) 0.0121(13) 0.0157(12) 0.0148(14) C19 0.0407(16) 0.0545(18) 0.0244(13) -0.0013(13) 0.0063(12) 0.0087(14) C20 0.0424(16) 0.0405(15) 0.0238(13) -0.0035(12) 0.0076(12) -0.0034(12) C21 0.0270(13) 0.0240(12) 0.0240(12) 0.0039(10) 0.0124(10) 0.0038(10) C22 0.0327(16) 0.0541(19) 0.0566(19) -0.0124(16) 0.0172(14) -0.0058(14) C23 0.058(2) 0.074(2) 0.083(3) -0.005(2) 0.040(2) -0.0212(19) C24 0.0365(17) 0.0406(16) 0.073(2) -0.0117(16) 0.0177(15) -0.0142(13) C25 0.0409(17) 0.0325(15) 0.0474(17) -0.0148(13) 0.0047(13) -0.0065(12) C26 0.0433(17) 0.0333(15) 0.0392(16) -0.0100(13) 0.0081(13) 0.0012(12) C27 0.0308(14) 0.0337(14) 0.0382(15) -0.0045(12) 0.0091(12) 0.0028(11) C28 0.0245(13) 0.0194(11) 0.0298(13) 0.0012(10) 0.0019(10) 0.0004(10) C29 0.0538(18) 0.0286(14) 0.0448(16) 0.0040(13) 0.0281(14) -0.0047(13) C30 0.0406(16) 0.0264(13) 0.0487(17) 0.0075(13) 0.0161(13) -0.0029(12) C31 0.0497(18) 0.0228(13) 0.0427(16) 0.0051(12) 0.0162(13) -0.0017(12) C32 0.0442(17) 0.0319(14) 0.0410(16) 0.0034(13) 0.0159(13) 0.0129(12) C33 0.0324(15) 0.0429(16) 0.0483(17) 0.0052(14) 0.0155(13) 0.0139(13) C34 0.0377(16) 0.0410(15) 0.0451(16) 0.0124(13) 0.0242(13) 0.0119(12) C35 0.0234(12) 0.0220(12) 0.0181(11) 0.0010(10) 0.0007(9) 0.0030(9) C36 0.0362(15) 0.0318(14) 0.0398(15) 0.0077(12) 0.0084(12) 0.0019(12) C37 0.0437(17) 0.0373(15) 0.0332(15) 0.0103(13) 0.0060(12) 0.0078(13) C38 0.0333(15) 0.0358(15) 0.0352(15) 0.0051(12) -0.0019(12) 0.0091(12) C39 0.0260(14) 0.0406(15) 0.0396(15) -0.0035(13) 0.0036(12) 0.0069(12) C40 0.0289(15) 0.0545(18) 0.0412(16) -0.0057(14) 0.0109(12) 0.0020(13) C41 0.0330(15) 0.0441(16) 0.0352(15) 0.0068(13) 0.0100(12) -0.0011(12) C42 0.0246(13) 0.0243(12) 0.0245(12) -0.0030(10) 0.0006(10) 0.0042(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N1 2.075(2) . ? Mn1 N9 2.051(2) . ? Mn1 N12 2.082(2) . ? Mn1 N15 2.162(2) . ? Mn1 Li2 2.7620(13) . ? Mn1 Li1 2.7303(11) . ? Mn2 N6 2.039(2) . ? Mn2 N16 2.080(2) . ? Mn2 N3 2.082(2) . ? Mn2 N13 2.138(2) . ? Mn2 Li1 2.7405(14) . ? Mn2 Li2 2.7825(11) . ? Li1 N10 2.068(2) . ? Li1 N13 2.085(2) . ? Li1 N4 2.089(2) . ? Li1 N1 2.145(2) . ? Li2 N15 2.090(2) . ? Li2 N7 2.078(2) . ? Li2 N18 2.053(2) . ? Li2 N3 2.178(2) . ? N1 C7 1.344(3) . ? N1 C1 1.467(3) . ? N2 C7 1.367(3) . ? N2 C4 1.453(3) . ? N2 C3 1.458(3) . ? N3 C7 1.348(3) . ? N3 C6 1.465(3) . ? N4 C14 1.335(3) . ? N4 C8 1.461(3) . ? N5 C14 1.398(3) . ? N5 C11 1.449(3) . ? N5 C10 1.457(3) . ? N6 C14 1.327(3) . ? N6 C13 1.461(3) . ? N7 C21 1.343(3) . ? N7 C15 1.454(3) . ? N8 C21 1.384(3) . ? N8 C17 1.455(3) . ? N8 C18 1.453(3) . ? N9 C21 1.335(3) . ? N9 C20 1.458(3) . ? N10 C28 1.329(3) . ? N10 C22 1.453(3) . ? N11 C24 1.444(4) . ? N11 C25 1.456(4) . ? N11 C28 1.390(3) . ? N12 C28 1.336(3) . ? N12 C27 1.459(3) . ? N13 C35 1.345(3) . ? N13 C29 1.468(3) . ? N14 C35 1.374(3) . ? N14 C31 1.462(3) . ? N14 C32 1.451(3) . ? N15 C35 1.345(3) . ? N15 C34 1.470(3) . ? N16 C42 1.335(3) . ? N16 C36 1.453(3) . ? N17 C42 1.388(3) . ? N17 C38 1.453(3) . ? N17 C39 1.448(3) . ? N18 C42 1.340(3) . ? N18 C41 1.456(3) . ? C1 C2 1.495(4) . ? C2 C3 1.504(4) . ? C4 C5 1.508(4) . ? C5 C6 1.512(4) . ? C8 C9 1.515(4) . ? C9 C10 1.504(4) . ? C11 C12 1.512(4) . ? C12 C13 1.503(4) . ? C15 C16 1.517(4) . ? C16 C17 1.500(4) . ? C18 C19 1.502(4) . ? C19 C20 1.504(4) . ? C22 C23 1.475(5) . ? C23 C24 1.467(5) . ? C25 C26 1.510(4) . ? C26 C27 1.508(4) . ? C29 C30 1.518(4) . ? C30 C31 1.499(4) . ? C32 C33 1.512(4) . ? C33 C34 1.506(4) . ? C36 C37 1.515(4) . ? C37 C38 1.508(4) . ? C39 C40 1.519(4) . ? C40 C41 1.515(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mn1 N9 109.82(8) . . ? N1 Mn1 N12 112.49(8) . . ? N9 Mn1 N12 114.26(9) . . ? N1 Mn1 N15 114.23(8) . . ? N9 Mn1 N15 103.82(8) . . ? N12 Mn1 N15 101.80(8) . . ? N1 Mn1 Li2 78.98(6) . . ? N9 Mn1 Li2 86.57(6) . . ? N12 Mn1 Li2 148.53(7) . . ? N15 Mn1 Li2 48.36(6) . . ? N1 Mn1 Li1 50.81(6) . . ? N9 Mn1 Li1 160.48(7) . . ? N12 Mn1 Li1 76.73(6) . . ? N15 Mn1 Li1 88.74(6) . . ? Li2 Mn1 Li1 90.99(3) . . ? N6 Mn2 N16 112.38(9) . . ? N6 Mn2 N3 108.42(8) . . ? N16 Mn2 N3 110.55(8) . . ? N6 Mn2 N13 107.32(8) . . ? N16 Mn2 N13 103.17(8) . . ? N3 Mn2 N13 114.99(8) . . ? N6 Mn2 Li1 89.52(7) . . ? N16 Mn2 Li1 149.91(7) . . ? N3 Mn2 Li1 79.44(6) . . ? N13 Mn2 Li1 48.71(6) . . ? N6 Mn2 Li2 158.68(7) . . ? N16 Mn2 Li2 76.62(7) . . ? N3 Mn2 Li2 50.73(6) . . ? N13 Mn2 Li2 88.36(6) . . ? Li1 Mn2 Li2 90.34(3) . . ? N10 Li1 N13 108.77(9) . . ? N10 Li1 N4 116.54(9) . . ? N13 Li1 N4 109.99(8) . . ? N10 Li1 N1 105.65(8) . . ? N13 Li1 N1 113.35(8) . . ? N4 Li1 N1 102.49(8) . . ? N10 Li1 Mn2 159.10(7) . . ? N13 Li1 Mn2 50.38(6) . . ? N4 Li1 Mn2 75.38(6) . . ? N1 Li1 Mn2 87.10(6) . . ? N10 Li1 Mn1 87.62(7) . . ? N13 Li1 Mn1 77.93(6) . . ? N4 Li1 Mn1 148.31(7) . . ? N1 Li1 Mn1 48.56(6) . . ? Mn2 Li1 Mn1 88.77(3) . . ? N15 Li2 N7 112.30(8) . . ? N15 Li2 N18 108.48(8) . . ? N7 Li2 N18 117.36(9) . . ? N15 Li2 N3 112.70(8) . . ? N7 Li2 N3 101.49(8) . . ? N18 Li2 N3 104.13(8) . . ? N15 Li2 Mn1 50.62(6) . . ? N7 Li2 Mn1 76.71(6) . . ? N18 Li2 Mn1 159.10(7) . . ? N3 Li2 Mn1 86.79(6) . . ? N15 Li2 Mn2 76.94(6) . . ? N7 Li2 Mn2 146.56(7) . . ? N18 Li2 Mn2 87.17(7) . . ? N3 Li2 Mn2 47.74(5) . . ? Mn1 Li2 Mn2 87.29(3) . . ? C7 N1 C1 116.6(2) . . ? C7 N1 Mn1 127.59(16) . . ? C1 N1 Mn1 104.56(16) . . ? C7 N1 Li1 109.69(14) . . ? C1 N1 Li1 112.27(16) . . ? Mn1 N1 Li1 80.63(7) . . ? C7 N2 C4 123.0(2) . . ? C7 N2 C3 122.8(2) . . ? C4 N2 C3 114.2(2) . . ? C7 N3 C6 117.08(19) . . ? C7 N3 Mn2 126.80(15) . . ? C6 N3 Mn2 105.23(15) . . ? C7 N3 Li2 107.79(14) . . ? C6 N3 Li2 112.97(15) . . ? Mn2 N3 Li2 81.53(7) . . ? C14 N4 C8 115.5(2) . . ? C14 N4 Li1 132.16(17) . . ? C8 N4 Li1 112.03(15) . . ? C14 N5 C11 122.0(2) . . ? C14 N5 C10 122.8(2) . . ? C11 N5 C10 113.8(2) . . ? C14 N6 C13 118.7(2) . . ? C14 N6 Mn2 116.39(16) . . ? C13 N6 Mn2 122.49(17) . . ? C21 N7 C15 115.3(2) . . ? C21 N7 Li2 129.96(16) . . ? C15 N7 Li2 113.88(16) . . ? C21 N8 C17 123.6(2) . . ? C21 N8 C18 122.8(2) . . ? C17 N8 C18 113.3(2) . . ? C21 N9 C20 117.1(2) . . ? C21 N9 Mn1 116.27(15) . . ? C20 N9 Mn1 122.61(17) . . ? C28 N10 C22 117.7(2) . . ? C28 N10 Li1 116.85(16) . . ? C22 N10 Li1 123.52(18) . . ? C24 N11 C25 113.4(2) . . ? C24 N11 C28 122.5(2) . . ? C25 N11 C28 123.7(2) . . ? C28 N12 C27 115.5(2) . . ? C28 N12 Mn1 130.50(16) . . ? C27 N12 Mn1 113.67(16) . . ? C35 N13 C29 116.3(2) . . ? C35 N13 Li1 127.52(15) . . ? C29 N13 Li1 104.53(16) . . ? C35 N13 Mn2 109.15(15) . . ? C29 N13 Mn2 113.37(16) . . ? Li1 N13 Mn2 80.91(7) . . ? C35 N14 C31 123.0(2) . . ? C35 N14 C32 122.8(2) . . ? C31 N14 C32 114.1(2) . . ? C35 N15 C34 116.8(2) . . ? C35 N15 Li2 130.05(16) . . ? C34 N15 Li2 103.98(16) . . ? C35 N15 Mn1 105.95(15) . . ? C34 N15 Mn1 113.31(15) . . ? Li2 N15 Mn1 81.02(7) . . ? C42 N16 C36 115.5(2) . . ? C42 N16 Mn2 131.23(17) . . ? C36 N16 Mn2 112.50(17) . . ? C42 N17 C38 123.2(2) . . ? C42 N17 C39 123.5(2) . . ? C38 N17 C39 113.2(2) . . ? C42 N18 C41 116.2(2) . . ? C42 N18 Li2 117.31(16) . . ? C41 N18 Li2 123.81(16) . . ? C2 C1 N1 111.8(2) . . ? C3 C2 C1 107.6(2) . . ? C2 C3 N2 111.4(2) . . ? N2 C4 C5 110.9(2) . . ? C4 C5 C6 106.7(2) . . ? N3 C6 C5 111.4(2) . . ? N1 C7 N3 117.8(2) . . ? N1 C7 N2 121.2(2) . . ? N3 C7 N2 121.0(2) . . ? N4 C8 C9 110.2(2) . . ? C8 C9 C10 107.7(2) . . ? N5 C10 C9 112.7(2) . . ? N5 C11 C12 111.2(2) . . ? C11 C12 C13 107.6(2) . . ? N6 C13 C12 111.9(2) . . ? N6 C14 N4 118.9(2) . . ? N6 C14 N5 121.2(2) . . ? N4 C14 N5 119.9(2) . . ? N7 C15 C16 110.5(2) . . ? C17 C16 C15 107.9(2) . . ? N8 C17 C16 111.9(2) . . ? N8 C18 C19 112.0(2) . . ? C20 C19 C18 108.2(2) . . ? N9 C20 C19 111.1(2) . . ? N9 C21 N8 121.2(2) . . ? N9 C21 N7 118.5(2) . . ? N8 C21 N7 120.3(2) . . ? N10 C22 C23 113.2(3) . . ? C22 C23 C24 111.3(3) . . ? N11 C24 C23 112.3(2) . . ? N11 C25 C26 112.9(2) . . ? C27 C26 C25 107.5(2) . . ? N12 C27 C26 111.4(2) . . ? N10 C28 N12 118.6(2) . . ? N10 C28 N11 121.4(2) . . ? N12 C28 N11 119.9(2) . . ? C30 C29 N13 110.5(2) . . ? C29 C30 C31 107.5(2) . . ? N14 C31 C30 111.5(2) . . ? N14 C32 C33 110.7(2) . . ? C34 C33 C32 107.3(2) . . ? N15 C34 C33 111.2(2) . . ? N13 C35 N15 117.9(2) . . ? N13 C35 N14 120.7(2) . . ? N15 C35 N14 121.4(2) . . ? N16 C36 C37 110.4(2) . . ? C36 C37 C38 107.2(2) . . ? N17 C38 C37 112.3(2) . . ? N17 C39 C40 111.9(2) . . ? C41 C40 C39 107.2(2) . . ? N18 C41 C40 111.2(2) . . ? N18 C42 N16 118.8(2) . . ? N18 C42 N17 120.9(2) . . ? N16 C42 N17 120.3(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.716 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.056