# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'R. E. Mulvey' 'A. R. Kennedy' 'Jan Klett' 'Sean Newton' 'D. S. Wright' _publ_contact_author_name 'R. E. Mulvey' _publ_contact_author_address ; Department of Pure & Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; anganese (II)-lithium and -sodium inverse crown ether (ICE) complexes ; data_grem250 _database_code_depnum_ccdc_archive 'CCDC 662468' #----------------------------------------------------------- #-------------------------COMPOUND 1------------------------ #----------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H72 Li2 Mn2 N4 O' _chemical_formula_weight 700.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' _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 16.9678(6) _cell_length_b 17.0135(6) _cell_length_c 15.7137(5) _cell_angle_alpha 90.00 _cell_angle_beta 118.803(2) _cell_angle_gamma 90.00 _cell_volume 3975.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4690 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'cut slat' _exptl_crystal_colour browned _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; checked lower sym sp groups - still disordered ; _diffrn_ambient_temperature 173(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 and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28348 _diffrn_reflns_av_R_equivalents 0.080 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3894 _reflns_number_gt 2648 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SHELXS _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0371P)^2^+2.4896P] 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 SHELXL _refine_ls_extinction_coef 0.00092(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3894 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.81328(4) 0.33635(4) 0.47987(4) 0.0236(2) Uani 0.4553(9) 1 d P . . Mn2 Mn 0.82862(4) 0.17648(3) 0.48328(4) 0.0230(2) Uani 0.5447(9) 1 d P . . Li1 Li 0.81328(4) 0.33635(4) 0.47987(4) 0.0236(2) Uani 0.5447(9) 1 d P . . Li2 Li 0.82862(4) 0.17648(3) 0.48328(4) 0.0230(2) Uani 0.4553(9) 1 d P . . O1 O 0.7500 0.2500 0.5000 0.0305(5) Uani 1 2 d S . . N1 N 0.73446(11) 0.42530(10) 0.49849(11) 0.0241(4) Uani 1 1 d . . . N2 N 0.90371(11) 0.26255(10) 0.45816(11) 0.0216(4) Uani 1 1 d . . . C1 C 0.67388(14) 0.47098(12) 0.41032(15) 0.0262(5) Uani 1 1 d . . . C2 C 0.72065(16) 0.54371(13) 0.39659(16) 0.0342(6) Uani 1 1 d . . . H2A H 0.7661 0.5262 0.3783 0.041 Uiso 1 1 calc R . . H2B H 0.6755 0.5758 0.3425 0.041 Uiso 1 1 calc R . . C3 C 0.76608(16) 0.59412(13) 0.48686(17) 0.0365(6) Uani 1 1 d . . . H3A H 0.7984 0.6381 0.4760 0.044 Uiso 1 1 calc R . . H3B H 0.7205 0.6164 0.5022 0.044 Uiso 1 1 calc R . . C4 C 0.83159(15) 0.54375(13) 0.57022(16) 0.0323(6) Uani 1 1 d . . . H4A H 0.8605 0.5762 0.6298 0.039 Uiso 1 1 calc R . . H4B H 0.8793 0.5252 0.5560 0.039 Uiso 1 1 calc R . . C5 C 0.78644(14) 0.47212(13) 0.58890(15) 0.0270(5) Uani 1 1 d . . . C6 C 0.64775(16) 0.41679(14) 0.32310(15) 0.0338(6) Uani 1 1 d . . . H6A H 0.7017 0.4024 0.3190 0.051 Uiso 1 1 calc R . . H6B H 0.6054 0.4441 0.2635 0.051 Uiso 1 1 calc R . . H6C H 0.6194 0.3692 0.3310 0.051 Uiso 1 1 calc R . . C7 C 0.58545(15) 0.49668(13) 0.40728(17) 0.0345(6) Uani 1 1 d . . . H7A H 0.5565 0.4510 0.4185 0.052 Uiso 1 1 calc R . . H7B H 0.5451 0.5194 0.3435 0.052 Uiso 1 1 calc R . . H7C H 0.5985 0.5361 0.4579 0.052 Uiso 1 1 calc R . . C8 C 0.86129(15) 0.41935(14) 0.66268(15) 0.0340(6) Uani 1 1 d . . . H8A H 0.8347 0.3722 0.6744 0.051 Uiso 1 1 calc R . . H8B H 0.8955 0.4481 0.7238 0.051 Uiso 1 1 calc R . . H8C H 0.9015 0.4040 0.6371 0.051 Uiso 1 1 calc R . . C9 C 0.73007(16) 0.49974(14) 0.63689(17) 0.0360(6) Uani 1 1 d . . . H9A H 0.6917 0.5439 0.5999 0.054 Uiso 1 1 calc R . . H9B H 0.7704 0.5165 0.7037 0.054 Uiso 1 1 calc R . . H9C H 0.6924 0.4563 0.6374 0.054 Uiso 1 1 calc R . . C10 C 0.88757(14) 0.26511(13) 0.35608(15) 0.0273(5) Uani 1 1 d . . . C11 C 0.95131(15) 0.21031(15) 0.34105(16) 0.0342(6) Uani 1 1 d . . . H11A H 0.9366 0.1552 0.3478 0.041 Uiso 1 1 calc R . . H11B H 0.9419 0.2172 0.2742 0.041 Uiso 1 1 calc R . . C12 C 1.04990(15) 0.22574(15) 0.41326(17) 0.0357(6) Uani 1 1 d . . . H12A H 1.0670 0.2795 0.4042 0.043 Uiso 1 1 calc R . . H12B H 1.0888 0.1877 0.4032 0.043 Uiso 1 1 calc R . . C13 C 1.06153(15) 0.21684(14) 0.51542(16) 0.0316(6) Uani 1 1 d . . . H13A H 1.1247 0.2288 0.5634 0.038 Uiso 1 1 calc R . . H13B H 1.0496 0.1615 0.5251 0.038 Uiso 1 1 calc R . . C14 C 0.99935(14) 0.27046(12) 0.53463(15) 0.0238(5) Uani 1 1 d . . . C15 C 0.89266(17) 0.34810(15) 0.32002(18) 0.0453(7) Uani 1 1 d . . . H15A H 0.8605 0.3852 0.3400 0.068 Uiso 1 1 calc R . . H15B H 0.8650 0.3478 0.2490 0.068 Uiso 1 1 calc R . . H15C H 0.9558 0.3642 0.3481 0.068 Uiso 1 1 calc R . . C16 C 0.79143(15) 0.23543(15) 0.29100(16) 0.0378(6) Uani 1 1 d . . . H16A H 0.7867 0.1807 0.3074 0.057 Uiso 1 1 calc R . . H16B H 0.7772 0.2387 0.2228 0.057 Uiso 1 1 calc R . . H16C H 0.7491 0.2679 0.3012 0.057 Uiso 1 1 calc R . . C17 C 1.03502(16) 0.35544(13) 0.55070(17) 0.0364(6) Uani 1 1 d . . . H17A H 1.0426 0.3720 0.4953 0.055 Uiso 1 1 calc R . . H17B H 1.0931 0.3580 0.6102 0.055 Uiso 1 1 calc R . . H17C H 0.9921 0.3904 0.5568 0.055 Uiso 1 1 calc R . . C18 C 1.00447(15) 0.24371(14) 0.63057(15) 0.0309(5) Uani 1 1 d . . . H18A H 0.9622 0.2746 0.6429 0.046 Uiso 1 1 calc R . . H18B H 1.0657 0.2516 0.6839 0.046 Uiso 1 1 calc R . . H18C H 0.9887 0.1879 0.6262 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0231(4) 0.0222(4) 0.0289(4) -0.0003(3) 0.0153(3) -0.0002(3) Mn2 0.0235(3) 0.0214(3) 0.0278(3) 0.0000(3) 0.0153(3) 0.0005(3) Li1 0.0231(4) 0.0222(4) 0.0289(4) -0.0003(3) 0.0153(3) -0.0002(3) Li2 0.0235(3) 0.0214(3) 0.0278(3) 0.0000(3) 0.0153(3) 0.0005(3) O1 0.0323(13) 0.0206(12) 0.0522(14) 0.0008(10) 0.0313(11) 0.0009(10) N1 0.0267(11) 0.0199(9) 0.0229(9) -0.0009(8) 0.0097(8) 0.0005(8) N2 0.0185(9) 0.0272(10) 0.0203(9) 0.0024(8) 0.0103(8) 0.0011(8) C1 0.0277(13) 0.0231(12) 0.0277(12) 0.0019(10) 0.0132(10) 0.0009(10) C2 0.0337(14) 0.0286(13) 0.0400(14) 0.0060(11) 0.0176(12) 0.0012(11) C3 0.0353(15) 0.0238(13) 0.0551(17) -0.0014(12) 0.0255(13) -0.0051(11) C4 0.0282(13) 0.0324(13) 0.0385(14) -0.0115(11) 0.0178(11) -0.0071(11) C5 0.0292(13) 0.0252(12) 0.0280(12) -0.0047(10) 0.0148(11) -0.0023(10) C6 0.0356(14) 0.0325(14) 0.0279(13) 0.0029(11) 0.0109(11) 0.0029(11) C7 0.0277(13) 0.0309(13) 0.0438(14) -0.0014(12) 0.0164(12) -0.0001(11) C8 0.0327(14) 0.0391(14) 0.0263(12) -0.0041(11) 0.0110(11) -0.0014(12) C9 0.0367(14) 0.0391(15) 0.0380(14) -0.0104(12) 0.0225(12) -0.0092(12) C10 0.0237(12) 0.0368(14) 0.0234(11) 0.0055(10) 0.0129(10) 0.0038(11) C11 0.0342(14) 0.0460(16) 0.0256(12) -0.0026(11) 0.0169(11) 0.0023(12) C12 0.0263(13) 0.0464(15) 0.0393(14) -0.0025(12) 0.0198(11) 0.0069(12) C13 0.0233(12) 0.0364(14) 0.0322(13) -0.0017(11) 0.0111(10) 0.0041(11) C14 0.0201(11) 0.0271(12) 0.0239(11) 0.0007(10) 0.0104(9) 0.0005(10) C15 0.0461(16) 0.0512(17) 0.0424(15) 0.0219(13) 0.0242(13) 0.0099(13) C16 0.0288(13) 0.0572(17) 0.0251(12) 0.0005(12) 0.0111(11) 0.0041(13) C17 0.0355(14) 0.0352(14) 0.0433(15) -0.0047(12) 0.0228(12) -0.0069(12) C18 0.0276(13) 0.0393(14) 0.0238(11) -0.0002(11) 0.0109(10) -0.0025(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 Mn1 O1 1.9334(6) . ? Mn1 N1 2.1311(18) . ? Mn1 N2 2.1334(17) . ? Mn1 Mn2 2.7304(8) . ? Mn1 Li2 2.7429(8) 7_656 ? Mn1 Mn2 2.7429(8) 7_656 ? Mn2 O1 1.9368(5) . ? Mn2 N2 2.0995(17) . ? Mn2 N1 2.1266(18) 7_656 ? Mn2 Mn1 2.7429(8) 7_656 ? Mn2 Li1 2.7429(8) 7_656 ? O1 Li1 1.9334(6) 7_656 ? O1 Mn1 1.9334(6) 7_656 ? O1 Li2 1.9368(5) 7_656 ? O1 Mn2 1.9368(5) 7_656 ? N1 C1 1.486(3) . ? N1 C5 1.491(3) . ? N1 Li2 2.1266(18) 7_656 ? N1 Mn2 2.1266(18) 7_656 ? N2 C14 1.489(3) . ? N2 C10 1.492(3) . ? C1 C6 1.529(3) . ? C1 C2 1.540(3) . ? C1 C7 1.541(3) . ? C2 C3 1.513(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.511(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.541(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C8 1.531(3) . ? C5 C9 1.549(3) . ? 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 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.530(3) . ? C10 C16 1.534(3) . ? C10 C15 1.539(3) . ? C11 C12 1.525(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.528(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.531(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C18 1.537(3) . ? C14 C17 1.540(3) . ? 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 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 O1 Mn1 N1 94.73(5) . . ? O1 Mn1 N2 94.47(5) . . ? N1 Mn1 N2 170.80(7) . . ? O1 Mn1 Mn2 45.181(17) . . ? N1 Mn1 Mn2 139.91(5) . . ? N2 Mn1 Mn2 49.29(5) . . ? O1 Mn1 Li2 44.917(17) . 7_656 ? N1 Mn1 Li2 49.82(5) . 7_656 ? N2 Mn1 Li2 139.38(5) . 7_656 ? Mn2 Mn1 Li2 90.10(2) . 7_656 ? O1 Mn1 Mn2 44.917(17) . 7_656 ? N1 Mn1 Mn2 49.82(5) . 7_656 ? N2 Mn1 Mn2 139.38(5) . 7_656 ? Mn2 Mn1 Mn2 90.10(2) . 7_656 ? Li2 Mn1 Mn2 0.00(2) 7_656 7_656 ? O1 Mn2 N2 95.46(5) . . ? O1 Mn2 N1 94.78(5) . 7_656 ? N2 Mn2 N1 169.66(7) . 7_656 ? O1 Mn2 Mn1 45.082(17) . . ? N2 Mn2 Mn1 50.38(5) . . ? N1 Mn2 Mn1 139.85(5) 7_656 . ? O1 Mn2 Mn1 44.820(17) . 7_656 ? N2 Mn2 Mn1 140.27(5) . 7_656 ? N1 Mn2 Mn1 49.96(5) 7_656 7_656 ? Mn1 Mn2 Mn1 89.90(2) . 7_656 ? O1 Mn2 Li1 44.820(17) . 7_656 ? N2 Mn2 Li1 140.27(5) . 7_656 ? N1 Mn2 Li1 49.96(5) 7_656 7_656 ? Mn1 Mn2 Li1 89.90(2) . 7_656 ? Mn1 Mn2 Li1 0.00(3) 7_656 7_656 ? Mn1 O1 Li1 180.00(2) . 7_656 ? Mn1 O1 Mn1 180.00(2) . 7_656 ? Li1 O1 Mn1 0.00(4) 7_656 7_656 ? Mn1 O1 Li2 90.26(2) . 7_656 ? Li1 O1 Li2 89.74(2) 7_656 7_656 ? Mn1 O1 Li2 89.74(2) 7_656 7_656 ? Mn1 O1 Mn2 90.26(2) . 7_656 ? Li1 O1 Mn2 89.74(2) 7_656 7_656 ? Mn1 O1 Mn2 89.74(2) 7_656 7_656 ? Li2 O1 Mn2 0.00(3) 7_656 7_656 ? Mn1 O1 Mn2 89.74(2) . . ? Li1 O1 Mn2 90.26(2) 7_656 . ? Mn1 O1 Mn2 90.26(2) 7_656 . ? Li2 O1 Mn2 180.00(3) 7_656 . ? Mn2 O1 Mn2 180.00(3) 7_656 . ? C1 N1 C5 115.79(16) . . ? C1 N1 Li2 112.61(12) . 7_656 ? C5 N1 Li2 114.31(12) . 7_656 ? C1 N1 Mn2 112.61(12) . 7_656 ? C5 N1 Mn2 114.31(12) . 7_656 ? Li2 N1 Mn2 0.00(3) 7_656 7_656 ? C1 N1 Mn1 116.19(12) . . ? C5 N1 Mn1 112.83(12) . . ? Li2 N1 Mn1 80.22(6) 7_656 . ? Mn2 N1 Mn1 80.22(6) 7_656 . ? C14 N2 C10 115.42(16) . . ? C14 N2 Mn2 115.82(12) . . ? C10 N2 Mn2 114.12(13) . . ? C14 N2 Mn1 113.96(12) . . ? C10 N2 Mn1 112.40(12) . . ? Mn2 N2 Mn1 80.33(6) . . ? N1 C1 C6 106.98(17) . . ? N1 C1 C2 112.28(17) . . ? C6 C1 C2 107.76(17) . . ? N1 C1 C7 113.78(17) . . ? C6 C1 C7 106.60(18) . . ? C2 C1 C7 109.10(18) . . ? C3 C2 C1 112.84(18) . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 108.73(19) . . ? C4 C3 H3A 109.9 . . ? C2 C3 H3A 109.9 . . ? C4 C3 H3B 109.9 . . ? C2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C3 C4 C5 112.84(18) . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N1 C5 C8 107.59(17) . . ? N1 C5 C4 111.16(17) . . ? C8 C5 C4 107.51(18) . . ? N1 C5 C9 113.92(17) . . ? C8 C5 C9 106.91(17) . . ? C4 C5 C9 109.45(18) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 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 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 111.77(17) . . ? N2 C10 C16 107.01(17) . . ? C11 C10 C16 107.47(18) . . ? N2 C10 C15 114.13(18) . . ? C11 C10 C15 109.43(18) . . ? C16 C10 C15 106.66(18) . . ? C12 C11 C10 112.57(19) . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C13 107.75(19) . . ? C11 C12 H12A 110.2 . . ? C13 C12 H12A 110.2 . . ? C11 C12 H12B 110.2 . . ? C13 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? C12 C13 C14 113.31(18) . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N2 C14 C13 111.95(17) . . ? N2 C14 C18 106.83(16) . . ? C13 C14 C18 107.36(17) . . ? N2 C14 C17 113.98(18) . . ? C13 C14 C17 109.75(18) . . ? C18 C14 C17 106.57(18) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 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 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 N1 Mn1 Mn2 O1 1.30(8) . . . . ? N2 Mn1 Mn2 O1 -179.15(6) . . . . ? Li2 Mn1 Mn2 O1 0.0 7_656 . . . ? Mn2 Mn1 Mn2 O1 0.0 7_656 . . . ? O1 Mn1 Mn2 N2 179.15(6) . . . . ? N1 Mn1 Mn2 N2 -179.56(10) . . . . ? Li2 Mn1 Mn2 N2 179.15(6) 7_656 . . . ? Mn2 Mn1 Mn2 N2 179.15(6) 7_656 . . . ? O1 Mn1 Mn2 N1 1.30(8) . . . 7_656 ? N1 Mn1 Mn2 N1 2.59(15) . . . 7_656 ? N2 Mn1 Mn2 N1 -177.85(10) . . . 7_656 ? Li2 Mn1 Mn2 N1 1.30(8) 7_656 . . 7_656 ? Mn2 Mn1 Mn2 N1 1.30(8) 7_656 . . 7_656 ? O1 Mn1 Mn2 Mn1 0.0 . . . 7_656 ? N1 Mn1 Mn2 Mn1 1.30(8) . . . 7_656 ? N2 Mn1 Mn2 Mn1 -179.15(6) . . . 7_656 ? Li2 Mn1 Mn2 Mn1 0.0 7_656 . . 7_656 ? Mn2 Mn1 Mn2 Mn1 0.0 7_656 . . 7_656 ? O1 Mn1 Mn2 Li1 0.0 . . . 7_656 ? N1 Mn1 Mn2 Li1 1.30(8) . . . 7_656 ? N2 Mn1 Mn2 Li1 -179.15(6) . . . 7_656 ? Li2 Mn1 Mn2 Li1 0.0 7_656 . . 7_656 ? Mn2 Mn1 Mn2 Li1 0.0 7_656 . . 7_656 ? N1 Mn1 O1 Li1 -172(100) . . . 7_656 ? N2 Mn1 O1 Li1 8(100) . . . 7_656 ? Mn2 Mn1 O1 Li1 7(100) . . . 7_656 ? Li2 Mn1 O1 Li1 -173(100) 7_656 . . 7_656 ? Mn2 Mn1 O1 Li1 -173(100) 7_656 . . 7_656 ? N1 Mn1 O1 Mn1 -172(100) . . . 7_656 ? N2 Mn1 O1 Mn1 8(100) . . . 7_656 ? Mn2 Mn1 O1 Mn1 7(100) . . . 7_656 ? Li2 Mn1 O1 Mn1 -173(100) 7_656 . . 7_656 ? Mn2 Mn1 O1 Mn1 -173(100) 7_656 . . 7_656 ? N1 Mn1 O1 Li2 0.84(5) . . . 7_656 ? N2 Mn1 O1 Li2 -179.35(5) . . . 7_656 ? Mn2 Mn1 O1 Li2 180.0 . . . 7_656 ? Mn2 Mn1 O1 Li2 0.0 7_656 . . 7_656 ? N1 Mn1 O1 Mn2 0.84(5) . . . 7_656 ? N2 Mn1 O1 Mn2 -179.35(5) . . . 7_656 ? Mn2 Mn1 O1 Mn2 180.0 . . . 7_656 ? Li2 Mn1 O1 Mn2 0.0 7_656 . . 7_656 ? N1 Mn1 O1 Mn2 -179.16(5) . . . . ? N2 Mn1 O1 Mn2 0.65(5) . . . . ? Li2 Mn1 O1 Mn2 180.0 7_656 . . . ? Mn2 Mn1 O1 Mn2 180.0 7_656 . . . ? N2 Mn2 O1 Mn1 -0.66(5) . . . . ? N1 Mn2 O1 Mn1 -179.16(5) 7_656 . . . ? Mn1 Mn2 O1 Mn1 180.0 7_656 . . . ? Li1 Mn2 O1 Mn1 180.0 7_656 . . . ? N2 Mn2 O1 Li1 179.34(5) . . . 7_656 ? N1 Mn2 O1 Li1 0.84(5) 7_656 . . 7_656 ? Mn1 Mn2 O1 Li1 180.0 . . . 7_656 ? Mn1 Mn2 O1 Li1 0.0 7_656 . . 7_656 ? N2 Mn2 O1 Mn1 179.34(5) . . . 7_656 ? N1 Mn2 O1 Mn1 0.84(5) 7_656 . . 7_656 ? Mn1 Mn2 O1 Mn1 180.0 . . . 7_656 ? Li1 Mn2 O1 Mn1 0.0 7_656 . . 7_656 ? N2 Mn2 O1 Li2 -150(100) . . . 7_656 ? N1 Mn2 O1 Li2 31(100) 7_656 . . 7_656 ? Mn1 Mn2 O1 Li2 -149(100) . . . 7_656 ? Mn1 Mn2 O1 Li2 31(100) 7_656 . . 7_656 ? Li1 Mn2 O1 Li2 31(100) 7_656 . . 7_656 ? N2 Mn2 O1 Mn2 -150(100) . . . 7_656 ? N1 Mn2 O1 Mn2 31(100) 7_656 . . 7_656 ? Mn1 Mn2 O1 Mn2 -149(100) . . . 7_656 ? Mn1 Mn2 O1 Mn2 31(100) 7_656 . . 7_656 ? Li1 Mn2 O1 Mn2 31(100) 7_656 . . 7_656 ? O1 Mn1 N1 C1 -111.26(13) . . . . ? N2 Mn1 N1 C1 69.9(5) . . . . ? Mn2 Mn1 N1 C1 -112.18(13) . . . . ? Li2 Mn1 N1 C1 -110.48(15) 7_656 . . . ? Mn2 Mn1 N1 C1 -110.48(15) 7_656 . . . ? O1 Mn1 N1 C5 111.60(13) . . . . ? N2 Mn1 N1 C5 -67.2(5) . . . . ? Mn2 Mn1 N1 C5 110.68(13) . . . . ? Li2 Mn1 N1 C5 112.38(14) 7_656 . . . ? Mn2 Mn1 N1 C5 112.38(14) 7_656 . . . ? O1 Mn1 N1 Li2 -0.77(5) . . . 7_656 ? N2 Mn1 N1 Li2 -179.6(4) . . . 7_656 ? Mn2 Mn1 N1 Li2 -1.70(10) . . . 7_656 ? Mn2 Mn1 N1 Li2 0.0 7_656 . . 7_656 ? O1 Mn1 N1 Mn2 -0.77(5) . . . 7_656 ? N2 Mn1 N1 Mn2 -179.6(4) . . . 7_656 ? Mn2 Mn1 N1 Mn2 -1.70(10) . . . 7_656 ? Li2 Mn1 N1 Mn2 0.0 7_656 . . 7_656 ? O1 Mn2 N2 C14 112.64(13) . . . . ? N1 Mn2 N2 C14 -75.7(4) 7_656 . . . ? Mn1 Mn2 N2 C14 112.03(15) . . . . ? Mn1 Mn2 N2 C14 113.37(13) 7_656 . . . ? Li1 Mn2 N2 C14 113.37(13) 7_656 . . . ? O1 Mn2 N2 C10 -109.71(13) . . . . ? N1 Mn2 N2 C10 61.9(4) 7_656 . . . ? Mn1 Mn2 N2 C10 -110.32(14) . . . . ? Mn1 Mn2 N2 C10 -108.98(13) 7_656 . . . ? Li1 Mn2 N2 C10 -108.98(13) 7_656 . . . ? O1 Mn2 N2 Mn1 0.61(5) . . . . ? N1 Mn2 N2 Mn1 172.3(4) 7_656 . . . ? Mn1 Mn2 N2 Mn1 1.33(10) 7_656 . . . ? Li1 Mn2 N2 Mn1 1.33(10) 7_656 . . . ? O1 Mn1 N2 C14 -114.67(13) . . . . ? N1 Mn1 N2 C14 64.1(5) . . . . ? Mn2 Mn1 N2 C14 -114.06(14) . . . . ? Li2 Mn1 N2 C14 -115.37(13) 7_656 . . . ? Mn2 Mn1 N2 C14 -115.37(13) 7_656 . . . ? O1 Mn1 N2 C10 111.61(13) . . . . ? N1 Mn1 N2 C10 -69.6(5) . . . . ? Mn2 Mn1 N2 C10 112.22(14) . . . . ? Li2 Mn1 N2 C10 110.91(13) 7_656 . . . ? Mn2 Mn1 N2 C10 110.91(13) 7_656 . . . ? O1 Mn1 N2 Mn2 -0.61(5) . . . . ? N1 Mn1 N2 Mn2 178.2(4) . . . . ? Li2 Mn1 N2 Mn2 -1.31(10) 7_656 . . . ? Mn2 Mn1 N2 Mn2 -1.31(10) 7_656 . . . ? C5 N1 C1 C6 164.98(17) . . . . ? Li2 N1 C1 C6 -60.87(18) 7_656 . . . ? Mn2 N1 C1 C6 -60.87(18) 7_656 . . . ? Mn1 N1 C1 C6 29.1(2) . . . . ? C5 N1 C1 C2 47.0(2) . . . . ? Li2 N1 C1 C2 -178.89(13) 7_656 . . . ? Mn2 N1 C1 C2 -178.89(13) 7_656 . . . ? Mn1 N1 C1 C2 -88.91(18) . . . . ? C5 N1 C1 C7 -77.6(2) . . . . ? Li2 N1 C1 C7 56.6(2) 7_656 . . . ? Mn2 N1 C1 C7 56.6(2) 7_656 . . . ? Mn1 N1 C1 C7 146.55(15) . . . . ? N1 C1 C2 C3 -51.1(2) . . . . ? C6 C1 C2 C3 -168.60(19) . . . . ? C7 C1 C2 C3 76.0(2) . . . . ? C1 C2 C3 C4 56.0(2) . . . . ? C2 C3 C4 C5 -57.4(2) . . . . ? C1 N1 C5 C8 -165.26(17) . . . . ? Li2 N1 C5 C8 61.37(18) 7_656 . . . ? Mn2 N1 C5 C8 61.37(18) 7_656 . . . ? Mn1 N1 C5 C8 -27.93(19) . . . . ? C1 N1 C5 C4 -47.8(2) . . . . ? Li2 N1 C5 C4 178.84(13) 7_656 . . . ? Mn2 N1 C5 C4 178.84(13) 7_656 . . . ? Mn1 N1 C5 C4 89.54(17) . . . . ? C1 N1 C5 C9 76.4(2) . . . . ? Li2 N1 C5 C9 -56.9(2) 7_656 . . . ? Mn2 N1 C5 C9 -56.9(2) 7_656 . . . ? Mn1 N1 C5 C9 -146.25(15) . . . . ? C3 C4 C5 N1 53.3(2) . . . . ? C3 C4 C5 C8 170.82(18) . . . . ? C3 C4 C5 C9 -73.4(2) . . . . ? C14 N2 C10 C11 48.5(2) . . . . ? Mn2 N2 C10 C11 -89.36(18) . . . . ? Mn1 N2 C10 C11 -178.53(14) . . . . ? C14 N2 C10 C16 165.86(17) . . . . ? Mn2 N2 C10 C16 28.0(2) . . . . ? Mn1 N2 C10 C16 -61.14(19) . . . . ? C14 N2 C10 C15 -76.4(2) . . . . ? Mn2 N2 C10 C15 145.78(15) . . . . ? Mn1 N2 C10 C15 56.6(2) . . . . ? N2 C10 C11 C12 -54.0(3) . . . . ? C16 C10 C11 C12 -171.07(19) . . . . ? C15 C10 C11 C12 73.5(2) . . . . ? C10 C11 C12 C13 57.2(3) . . . . ? C11 C12 C13 C14 -56.4(3) . . . . ? C10 N2 C14 C13 -47.3(2) . . . . ? Mn2 N2 C14 C13 89.79(17) . . . . ? Mn1 N2 C14 C13 -179.59(13) . . . . ? C10 N2 C14 C18 -164.57(17) . . . . ? Mn2 N2 C14 C18 -27.5(2) . . . . ? Mn1 N2 C14 C18 63.15(18) . . . . ? C10 N2 C14 C17 78.0(2) . . . . ? Mn2 N2 C14 C17 -144.89(14) . . . . ? Mn1 N2 C14 C17 -54.3(2) . . . . ? C12 C13 C14 N2 51.9(3) . . . . ? C12 C13 C14 C18 168.82(19) . . . . ? C12 C13 C14 C17 -75.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.261 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.048 #===END # Attachment 'Compound4.cif' #----------------------------------------------------------- #-------------------------COMPOUND 4------------------------ #----------------------------------------------------------- data_grem262 _database_code_depnum_ccdc_archive 'CCDC 662469' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H47 Mn N2 Na Si5' _chemical_formula_weight 485.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2226(3) _cell_length_b 11.9296(3) _cell_length_c 12.0857(3) _cell_angle_alpha 97.180(1) _cell_angle_beta 100.700(1) _cell_angle_gamma 93.377(1) _cell_volume 1431.78(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6477 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'large needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Xles quickly brown in removal from Schlenk. From same sample as GREM261 (inverse crown). ; _diffrn_ambient_temperature 150(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 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32095 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.57 _reflns_number_total 6576 _reflns_number_gt 5179 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0299P)^2^+0.6397P] 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 6576 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Mn1 Mn 0.78870(3) 0.26076(2) 0.74278(2) 0.01911(8) Uani 1 1 d . . . Na1 Na 0.94982(7) 0.04764(6) 0.74658(6) 0.02324(16) Uani 1 1 d . . . Si1 Si 0.64175(5) 0.52425(5) 0.75877(5) 0.02942(13) Uani 1 1 d . . . Si2 Si 0.83253(5) 0.20390(4) 0.98910(4) 0.02108(11) Uani 1 1 d . . . Si3 Si 0.66694(5) 0.02479(4) 0.81375(4) 0.02124(11) Uani 1 1 d . . . Si4 Si 0.85872(5) 0.20777(4) 0.50248(4) 0.02054(11) Uani 1 1 d . . . Si5 Si 1.09539(5) 0.26915(4) 0.69366(4) 0.02000(11) Uani 1 1 d . . . N1 N 0.79057(14) 0.13387(12) 0.85278(12) 0.0185(3) Uani 1 1 d . . . N2 N 0.93279(14) 0.21323(12) 0.64298(12) 0.0189(3) Uani 1 1 d . . . C1 C 0.6341(2) 0.3710(2) 0.7183(3) 0.0419(6) Uani 1 1 d . . . C2 C 0.7848(3) 0.5984(2) 0.7132(3) 0.0647(8) Uani 1 1 d . . . H2A H 0.8683 0.5681 0.7457 0.097 Uiso 1 1 calc R . . H2B H 0.7893 0.6798 0.7399 0.097 Uiso 1 1 calc R . . H2C H 0.7719 0.5861 0.6300 0.097 Uiso 1 1 calc R . . C3 C 0.4871(2) 0.5870(2) 0.6923(2) 0.0546(7) Uani 1 1 d . . . H3A H 0.4754 0.5719 0.6093 0.082 Uiso 1 1 calc R . . H3B H 0.4959 0.6690 0.7166 0.082 Uiso 1 1 calc R . . H3C H 0.4094 0.5527 0.7164 0.082 Uiso 1 1 calc R . . C4 C 0.6604(3) 0.5633(2) 0.9158(2) 0.0613(8) Uani 1 1 d . . . H4A H 0.5876 0.5238 0.9421 0.092 Uiso 1 1 calc R . . H4B H 0.6571 0.6454 0.9338 0.092 Uiso 1 1 calc R . . H4C H 0.7463 0.5413 0.9541 0.092 Uiso 1 1 calc R . . C5 C 0.9334(2) 0.34066(16) 0.99061(17) 0.0300(4) Uani 1 1 d . . . H5A H 1.0183 0.3246 0.9679 0.045 Uiso 1 1 calc R . . H5B H 0.9510 0.3831 1.0674 0.045 Uiso 1 1 calc R . . H5C H 0.8836 0.3857 0.9373 0.045 Uiso 1 1 calc R . . C6 C 0.6874(2) 0.2421(2) 1.0558(2) 0.0433(6) Uani 1 1 d . . . H6A H 0.6318 0.2893 1.0087 0.065 Uiso 1 1 calc R . . H6B H 0.7201 0.2843 1.1318 0.065 Uiso 1 1 calc R . . H6C H 0.6342 0.1729 1.0617 0.065 Uiso 1 1 calc R . . C7 C 0.9388(2) 0.1217(2) 1.08939(19) 0.0337(5) Uani 1 1 d . . . C8 C 0.49735(19) 0.07488(18) 0.77125(19) 0.0350(5) Uani 1 1 d . . . H8A H 0.4799 0.1307 0.8323 0.052 Uiso 1 1 calc R . . H8B H 0.4298 0.0103 0.7575 0.052 Uiso 1 1 calc R . . H8C H 0.4934 0.1099 0.7017 0.052 Uiso 1 1 calc R . . C9 C 0.6576(2) -0.06951(19) 0.92555(19) 0.0369(5) Uani 1 1 d . . . H9A H 0.7438 -0.1011 0.9461 0.055 Uiso 1 1 calc R . . H9B H 0.5877 -0.1314 0.8960 0.055 Uiso 1 1 calc R . . H9C H 0.6364 -0.0254 0.9930 0.055 Uiso 1 1 calc R . . C10 C 0.7006(2) -0.07157(18) 0.68816(19) 0.0305(5) Uani 1 1 d . . . C11 C 0.6764(2) 0.1581(2) 0.47638(18) 0.0372(5) Uani 1 1 d . . . H11A H 0.6666 0.0782 0.4871 0.056 Uiso 1 1 calc R . . H11B H 0.6345 0.1666 0.3984 0.056 Uiso 1 1 calc R . . H11C H 0.6329 0.2036 0.5301 0.056 Uiso 1 1 calc R . . C12 C 0.8726(2) 0.34674(18) 0.44780(18) 0.0357(5) Uani 1 1 d . . . H12A H 0.8322 0.4036 0.4936 0.054 Uiso 1 1 calc R . . H12B H 0.8259 0.3386 0.3684 0.054 Uiso 1 1 calc R . . H12C H 0.9670 0.3711 0.4528 0.054 Uiso 1 1 calc R . . C13 C 0.9283(2) 0.1026(2) 0.40313(18) 0.0321(5) Uani 1 1 d . . . C14 C 1.1075(2) 0.42362(16) 0.74907(18) 0.0317(5) Uani 1 1 d . . . H14A H 1.0747 0.4661 0.6866 0.048 Uiso 1 1 calc R . . H14B H 1.2008 0.4499 0.7820 0.048 Uiso 1 1 calc R . . H14C H 1.0531 0.4358 0.8076 0.048 Uiso 1 1 calc R . . C15 C 1.20965(19) 0.2510(2) 0.58936(17) 0.0346(5) Uani 1 1 d . . . H15A H 1.2132 0.1700 0.5645 0.052 Uiso 1 1 calc R . . H15B H 1.2995 0.2847 0.6256 0.052 Uiso 1 1 calc R . . H15C H 1.1761 0.2886 0.5234 0.052 Uiso 1 1 calc R . . C16 C 1.1736(2) 0.19521(18) 0.81543(17) 0.0258(4) Uani 1 1 d . . . H1A H 0.603(3) 0.359(2) 0.640(3) 0.076(10) Uiso 1 1 d . . . H1B H 0.565(3) 0.338(3) 0.747(3) 0.085(11) Uiso 1 1 d . . . H7A H 0.887(2) 0.056(2) 1.100(2) 0.050(7) Uiso 1 1 d . . . H7B H 0.964(2) 0.171(2) 1.164(2) 0.050(7) Uiso 1 1 d . . . H7C H 1.013(3) 0.101(2) 1.061(2) 0.049(7) Uiso 1 1 d . . . H10A H 0.719(2) -0.032(2) 0.625(2) 0.044(7) Uiso 1 1 d . . . H10B H 0.776(2) -0.1151(17) 0.7104(16) 0.028(5) Uiso 1 1 d . . . H10C H 0.631(3) -0.123(2) 0.656(2) 0.050(7) Uiso 1 1 d . . . H13A H 0.921(2) 0.029(2) 0.425(2) 0.058(8) Uiso 1 1 d . . . H13B H 1.014(3) 0.123(2) 0.402(2) 0.059(8) Uiso 1 1 d . . . H13C H 0.879(2) 0.1022(19) 0.324(2) 0.042(6) Uiso 1 1 d . . . H16A H 1.124(2) 0.1931(17) 0.8716(18) 0.030(6) Uiso 1 1 d . . . H16B H 1.255(2) 0.2357(19) 0.8501(19) 0.039(6) Uiso 1 1 d . . . H16C H 1.193(2) 0.1198(19) 0.7901(18) 0.034(6) Uiso 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 Mn1 0.01976(14) 0.01854(15) 0.02015(15) 0.00353(11) 0.00519(11) 0.00480(10) Na1 0.0233(4) 0.0217(4) 0.0269(4) 0.0043(3) 0.0085(3) 0.0054(3) Si1 0.0282(3) 0.0240(3) 0.0372(3) 0.0055(2) 0.0058(2) 0.0107(2) Si2 0.0209(2) 0.0246(3) 0.0184(3) 0.0014(2) 0.0065(2) 0.0025(2) Si3 0.0169(2) 0.0214(3) 0.0257(3) 0.0035(2) 0.0048(2) 0.00063(19) Si4 0.0228(2) 0.0220(3) 0.0169(2) 0.00378(19) 0.00280(19) 0.0042(2) Si5 0.0181(2) 0.0223(3) 0.0200(3) 0.0040(2) 0.00436(19) 0.00127(19) N1 0.0180(7) 0.0198(8) 0.0184(7) 0.0034(6) 0.0049(6) 0.0018(6) N2 0.0191(7) 0.0218(8) 0.0166(7) 0.0029(6) 0.0052(6) 0.0034(6) C1 0.0321(12) 0.0306(12) 0.0556(16) -0.0038(11) -0.0066(11) 0.0124(10) C2 0.0535(16) 0.0478(16) 0.106(2) 0.0365(16) 0.0296(16) 0.0140(13) C3 0.0463(14) 0.0459(15) 0.0710(18) 0.0129(13) -0.0006(13) 0.0255(12) C4 0.0740(19) 0.0609(18) 0.0474(16) -0.0041(13) 0.0085(14) 0.0278(15) C5 0.0333(11) 0.0260(10) 0.0285(11) -0.0032(8) 0.0057(9) 0.0008(8) C6 0.0375(12) 0.0527(15) 0.0400(13) -0.0100(11) 0.0200(10) 0.0023(11) C7 0.0370(12) 0.0393(13) 0.0237(11) 0.0068(10) 0.0016(9) 0.0022(10) C8 0.0209(10) 0.0343(12) 0.0465(13) -0.0013(10) 0.0028(9) 0.0023(8) C9 0.0313(11) 0.0384(13) 0.0436(13) 0.0152(10) 0.0102(10) -0.0062(9) C10 0.0264(11) 0.0241(11) 0.0380(12) -0.0040(9) 0.0053(9) -0.0022(9) C11 0.0291(11) 0.0479(14) 0.0292(11) -0.0009(10) -0.0022(9) -0.0019(9) C12 0.0436(12) 0.0319(12) 0.0310(11) 0.0128(9) -0.0002(9) 0.0049(9) C13 0.0387(13) 0.0366(13) 0.0203(11) 0.0005(9) 0.0041(9) 0.0088(10) C14 0.0341(11) 0.0239(10) 0.0363(12) 0.0062(9) 0.0050(9) -0.0023(8) C15 0.0250(10) 0.0499(14) 0.0299(11) 0.0046(10) 0.0096(9) 0.0001(9) C16 0.0220(10) 0.0287(11) 0.0254(10) 0.0029(8) 0.0013(8) 0.0038(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 C1 2.117(2) . ? Mn1 N2 2.1291(14) . ? Mn1 N1 2.1345(14) . ? Mn1 Na1 3.1102(7) . ? Na1 N1 2.4493(15) . ? Na1 N2 2.4655(16) . ? Na1 C16 2.734(2) . ? Na1 C10 2.768(2) . ? Na1 C13 2.886(2) 2_756 ? Na1 C7 3.121(2) 2_757 ? Na1 Si5 3.1495(9) . ? Na1 Si3 3.1511(8) . ? Na1 H10A 2.59(2) . ? Na1 H10B 2.49(2) . ? Na1 H16A 2.54(2) . ? Na1 H16C 2.52(2) . ? Si1 C1 1.826(2) . ? Si1 C4 1.868(3) . ? Si1 C2 1.869(3) . ? Si1 C3 1.876(2) . ? Si2 N1 1.7169(15) . ? Si2 C6 1.868(2) . ? Si2 C5 1.874(2) . ? Si2 C7 1.883(2) . ? Si3 N1 1.7159(15) . ? Si3 C8 1.8694(19) . ? Si3 C9 1.875(2) . ? Si3 C10 1.884(2) . ? Si4 N2 1.7175(15) . ? Si4 C12 1.867(2) . ? Si4 C11 1.879(2) . ? Si4 C13 1.889(2) . ? Si5 N2 1.7240(15) . ? Si5 C14 1.869(2) . ? Si5 C15 1.8731(19) . ? Si5 C16 1.885(2) . ? C1 H1A 0.93(3) . ? C1 H1B 0.93(3) . ? 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 . ? C7 Na1 3.121(2) 2_757 ? C7 H7A 0.96(3) . ? C7 H7B 1.00(3) . ? C7 H7C 0.93(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.99(2) . ? C10 H10B 0.97(2) . ? C10 H10C 0.91(3) . ? 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 Na1 2.886(2) 2_756 ? C13 H13A 0.95(3) . ? C13 H13B 0.90(3) . ? C13 H13C 0.99(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 0.92(2) . ? C16 H16B 0.93(2) . ? C16 H16C 0.96(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 Mn1 N2 131.38(10) . . ? C1 Mn1 N1 122.66(10) . . ? N2 Mn1 N1 103.73(5) . . ? C1 Mn1 Na1 163.73(7) . . ? N2 Mn1 Na1 52.14(4) . . ? N1 Mn1 Na1 51.69(4) . . ? N1 Na1 N2 86.05(5) . . ? N1 Na1 C16 102.92(6) . . ? N2 Na1 C16 68.98(6) . . ? N1 Na1 C10 68.29(6) . . ? N2 Na1 C10 105.84(6) . . ? C16 Na1 C10 170.48(7) . . ? N1 Na1 C13 163.16(7) . 2_756 ? N2 Na1 C13 100.19(6) . 2_756 ? C16 Na1 C13 93.92(7) . 2_756 ? C10 Na1 C13 94.90(7) . 2_756 ? N1 Na1 Mn1 43.15(3) . . ? N2 Na1 Mn1 42.99(3) . . ? C16 Na1 Mn1 86.51(5) . . ? C10 Na1 Mn1 84.44(5) . . ? C13 Na1 Mn1 139.89(5) 2_756 . ? N1 Na1 C7 99.44(6) . 2_757 ? N2 Na1 C7 161.59(6) . 2_757 ? C16 Na1 C7 92.63(6) . 2_757 ? C10 Na1 C7 92.49(7) . 2_757 ? C13 Na1 C7 79.55(7) 2_756 2_757 ? Mn1 Na1 C7 140.54(5) . 2_757 ? N1 Na1 Si5 99.34(4) . . ? N2 Na1 Si5 32.99(3) . . ? C16 Na1 Si5 36.52(4) . . ? C10 Na1 Si5 138.83(6) . . ? C13 Na1 Si5 94.17(6) 2_756 . ? Mn1 Na1 Si5 63.531(17) . . ? C7 Na1 Si5 128.66(5) 2_757 . ? N1 Na1 Si3 32.74(4) . . ? N2 Na1 Si3 101.94(4) . . ? C16 Na1 Si3 135.36(5) . . ? C10 Na1 Si3 36.39(5) . . ? C13 Na1 Si3 130.50(6) 2_756 . ? Mn1 Na1 Si3 63.303(16) . . ? C7 Na1 Si3 91.71(5) 2_757 . ? Si5 Na1 Si3 126.67(2) . . ? N1 Na1 H10A 76.4(5) . . ? N2 Na1 H10A 87.7(5) . . ? C16 Na1 H10A 156.6(6) . . ? C10 Na1 H10A 20.8(5) . . ? C13 Na1 H10A 88.2(5) 2_756 . ? Mn1 Na1 H10A 77.1(5) . . ? C7 Na1 H10A 110.6(6) 2_757 . ? Si5 Na1 H10A 120.1(6) . . ? Si3 Na1 H10A 49.5(5) . . ? N1 Na1 H10B 81.5(5) . . ? N2 Na1 H10B 123.8(5) . . ? C16 Na1 H10B 167.0(5) . . ? C10 Na1 H10B 20.5(5) . . ? C13 Na1 H10B 82.1(5) 2_756 . ? Mn1 Na1 H10B 104.5(5) . . ? C7 Na1 H10B 74.5(5) 2_757 . ? Si5 Na1 H10B 155.7(5) . . ? Si3 Na1 H10B 48.9(5) . . ? H10A Na1 H10B 36.1(7) . . ? N1 Na1 H16A 85.9(5) . . ? N2 Na1 H16A 77.1(5) . . ? C16 Na1 H16A 19.7(5) . . ? C10 Na1 H16A 153.5(5) . . ? C13 Na1 H16A 110.7(5) 2_756 . ? Mn1 Na1 H16A 80.4(5) . . ? C7 Na1 H16A 85.7(5) 2_757 . ? Si5 Na1 H16A 48.8(5) . . ? Si3 Na1 H16A 117.2(5) . . ? H10A Na1 H16A 157.4(7) . . ? H10B Na1 H16A 154.3(7) . . ? N1 Na1 H16C 121.2(5) . . ? N2 Na1 H16C 81.4(5) . . ? C16 Na1 H16C 20.5(5) . . ? C10 Na1 H16C 169.0(5) . . ? C13 Na1 H16C 75.4(5) 2_756 . ? Mn1 Na1 H16C 106.3(5) . . ? C7 Na1 H16C 80.7(5) 2_757 . ? Si5 Na1 H16C 48.9(5) . . ? Si3 Na1 H16C 151.4(5) . . ? H10A Na1 H16C 158.3(7) . . ? H10B Na1 H16C 149.1(7) . . ? H16A Na1 H16C 35.3(7) . . ? C1 Si1 C4 111.77(14) . . ? C1 Si1 C2 111.46(13) . . ? C4 Si1 C2 107.99(15) . . ? C1 Si1 C3 112.50(12) . . ? C4 Si1 C3 106.35(12) . . ? C2 Si1 C3 106.45(12) . . ? N1 Si2 C6 114.79(9) . . ? N1 Si2 C5 109.78(8) . . ? C6 Si2 C5 106.09(10) . . ? N1 Si2 C7 112.97(9) . . ? C6 Si2 C7 106.45(11) . . ? C5 Si2 C7 106.19(10) . . ? N1 Si3 C8 112.87(8) . . ? N1 Si3 C9 114.19(9) . . ? C8 Si3 C9 107.59(10) . . ? N1 Si3 C10 109.46(9) . . ? C8 Si3 C10 107.35(10) . . ? C9 Si3 C10 104.88(10) . . ? N1 Si3 Na1 50.52(5) . . ? C8 Si3 Na1 138.54(8) . . ? C9 Si3 Na1 113.83(7) . . ? C10 Si3 Na1 60.68(7) . . ? N2 Si4 C12 113.51(9) . . ? N2 Si4 C11 111.67(8) . . ? C12 Si4 C11 107.50(10) . . ? N2 Si4 C13 113.78(9) . . ? C12 Si4 C13 106.12(11) . . ? C11 Si4 C13 103.53(11) . . ? N2 Si5 C14 112.66(8) . . ? N2 Si5 C15 115.26(8) . . ? C14 Si5 C15 107.16(10) . . ? N2 Si5 C16 109.72(8) . . ? C14 Si5 C16 106.83(9) . . ? C15 Si5 C16 104.60(10) . . ? N2 Si5 Na1 51.15(5) . . ? C14 Si5 Na1 135.51(7) . . ? C15 Si5 Na1 117.17(7) . . ? C16 Si5 Na1 59.67(7) . . ? Si3 N1 Si2 122.20(8) . . ? Si3 N1 Mn1 116.74(7) . . ? Si2 N1 Mn1 106.36(7) . . ? Si3 N1 Na1 96.74(7) . . ? Si2 N1 Na1 124.47(7) . . ? Mn1 N1 Na1 85.16(5) . . ? Si4 N2 Si5 121.55(8) . . ? Si4 N2 Mn1 107.75(7) . . ? Si5 N2 Mn1 117.20(8) . . ? Si4 N2 Na1 124.44(8) . . ? Si5 N2 Na1 95.86(6) . . ? Mn1 N2 Na1 84.87(5) . . ? Si1 C1 Mn1 129.04(13) . . ? Si1 C1 H1A 105.4(18) . . ? Mn1 C1 H1A 103.3(18) . . ? Si1 C1 H1B 108(2) . . ? Mn1 C1 H1B 105(2) . . ? H1A C1 H1B 104(3) . . ? 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 . . ? 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 . . ? 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 . . ? Si2 C7 Na1 166.31(12) . 2_757 ? Si2 C7 H7A 109.6(14) . . ? Na1 C7 H7A 56.9(14) 2_757 . ? Si2 C7 H7B 107.5(14) . . ? Na1 C7 H7B 77.0(14) 2_757 . ? H7A C7 H7B 107.5(19) . . ? Si2 C7 H7C 110.2(15) . . ? Na1 C7 H7C 78.9(15) 2_757 . ? H7A C7 H7C 110(2) . . ? H7B C7 H7C 112(2) . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si3 C10 Na1 82.93(8) . . ? Si3 C10 H10A 114.1(13) . . ? Na1 C10 H10A 69.2(13) . . ? Si3 C10 H10B 111.1(12) . . ? Na1 C10 H10B 63.4(12) . . ? H10A C10 H10B 107.1(17) . . ? Si3 C10 H10C 112.7(15) . . ? Na1 C10 H10C 164.0(15) . . ? H10A C10 H10C 105(2) . . ? H10B C10 H10C 106.0(19) . . ? Si4 C11 H11A 109.5 . . ? Si4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si4 C12 H12A 109.5 . . ? Si4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si4 C13 Na1 176.21(13) . 2_756 ? Si4 C13 H13A 109.8(15) . . ? Na1 C13 H13A 72.7(15) 2_756 . ? Si4 C13 H13B 111.5(17) . . ? Na1 C13 H13B 64.7(17) 2_756 . ? H13A C13 H13B 110(2) . . ? Si4 C13 H13C 109.2(13) . . ? Na1 C13 H13C 72.0(13) 2_756 . ? H13A C13 H13C 110(2) . . ? H13B C13 H13C 106(2) . . ? Si5 C14 H14A 109.5 . . ? Si5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si5 C15 H15A 109.5 . . ? Si5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si5 C16 Na1 83.81(7) . . ? Si5 C16 H16A 114.1(13) . . ? Na1 C16 H16A 68.1(13) . . ? Si5 C16 H16B 107.9(14) . . ? Na1 C16 H16B 168.2(14) . . ? H16A C16 H16B 106.1(18) . . ? Si5 C16 H16C 112.1(13) . . ? Na1 C16 H16C 67.2(13) . . ? H16A C16 H16C 109.4(18) . . ? H16B C16 H16C 106.9(18) . . ? 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 C1 Mn1 Na1 N1 -75.4(3) . . . . ? N2 Mn1 Na1 N1 175.64(7) . . . . ? C1 Mn1 Na1 N2 109.0(3) . . . . ? N1 Mn1 Na1 N2 -175.64(7) . . . . ? C1 Mn1 Na1 C16 171.5(3) . . . . ? N2 Mn1 Na1 C16 62.51(7) . . . . ? N1 Mn1 Na1 C16 -113.13(7) . . . . ? C1 Mn1 Na1 C10 -11.5(3) . . . . ? N2 Mn1 Na1 C10 -120.44(7) . . . . ? N1 Mn1 Na1 C10 63.92(7) . . . . ? C1 Mn1 Na1 C13 79.5(3) . . . 2_756 ? N2 Mn1 Na1 C13 -29.43(10) . . . 2_756 ? N1 Mn1 Na1 C13 154.93(10) . . . 2_756 ? C1 Mn1 Na1 C7 -98.6(3) . . . 2_757 ? N2 Mn1 Na1 C7 152.40(10) . . . 2_757 ? N1 Mn1 Na1 C7 -23.23(9) . . . 2_757 ? C1 Mn1 Na1 Si5 141.8(3) . . . . ? N2 Mn1 Na1 Si5 32.86(5) . . . . ? N1 Mn1 Na1 Si5 -142.77(5) . . . . ? C1 Mn1 Na1 Si3 -42.6(3) . . . . ? N2 Mn1 Na1 Si3 -151.53(5) . . . . ? N1 Mn1 Na1 Si3 32.83(5) . . . . ? N2 Na1 Si3 N1 -62.68(7) . . . . ? C16 Na1 Si3 N1 9.40(9) . . . . ? C10 Na1 Si3 N1 -163.25(11) . . . . ? C13 Na1 Si3 N1 -177.42(9) 2_756 . . . ? Mn1 Na1 Si3 N1 -43.28(6) . . . . ? C7 Na1 Si3 N1 104.88(8) 2_757 . . . ? Si5 Na1 Si3 N1 -38.38(7) . . . . ? N1 Na1 Si3 C8 80.10(12) . . . . ? N2 Na1 Si3 C8 17.42(12) . . . . ? C16 Na1 Si3 C8 89.50(13) . . . . ? C10 Na1 Si3 C8 -83.15(13) . . . . ? C13 Na1 Si3 C8 -97.32(12) 2_756 . . . ? Mn1 Na1 Si3 C8 36.82(11) . . . . ? C7 Na1 Si3 C8 -175.02(11) 2_757 . . . ? Si5 Na1 Si3 C8 41.72(11) . . . . ? N1 Na1 Si3 C9 -102.51(10) . . . . ? N2 Na1 Si3 C9 -165.19(9) . . . . ? C16 Na1 Si3 C9 -93.11(11) . . . . ? C10 Na1 Si3 C9 94.24(12) . . . . ? C13 Na1 Si3 C9 80.07(11) 2_756 . . . ? Mn1 Na1 Si3 C9 -145.79(8) . . . . ? C7 Na1 Si3 C9 2.37(10) 2_757 . . . ? Si5 Na1 Si3 C9 -140.89(8) . . . . ? N1 Na1 Si3 C10 163.25(11) . . . . ? N2 Na1 Si3 C10 100.57(9) . . . . ? C16 Na1 Si3 C10 172.65(11) . . . . ? C13 Na1 Si3 C10 -14.17(11) 2_756 . . . ? Mn1 Na1 Si3 C10 119.97(8) . . . . ? C7 Na1 Si3 C10 -91.87(10) 2_757 . . . ? Si5 Na1 Si3 C10 124.87(9) . . . . ? N1 Na1 Si5 N2 -67.58(7) . . . . ? C16 Na1 Si5 N2 -166.72(10) . . . . ? C10 Na1 Si5 N2 -0.01(10) . . . . ? C13 Na1 Si5 N2 102.32(8) 2_756 . . . ? Mn1 Na1 Si5 N2 -42.80(6) . . . . ? C7 Na1 Si5 N2 -177.72(9) 2_757 . . . ? Si3 Na1 Si5 N2 -47.69(7) . . . . ? N1 Na1 Si5 C14 15.86(11) . . . . ? N2 Na1 Si5 C14 83.44(11) . . . . ? C16 Na1 Si5 C14 -83.28(12) . . . . ? C10 Na1 Si5 C14 83.44(12) . . . . ? C13 Na1 Si5 C14 -174.23(10) 2_756 . . . ? Mn1 Na1 Si5 C14 40.65(10) . . . . ? C7 Na1 Si5 C14 -94.28(11) 2_757 . . . ? Si3 Na1 Si5 C14 35.75(10) . . . . ? N1 Na1 Si5 C15 -169.26(8) . . . . ? N2 Na1 Si5 C15 -101.68(10) . . . . ? C16 Na1 Si5 C15 91.60(11) . . . . ? C10 Na1 Si5 C15 -101.69(11) . . . . ? C13 Na1 Si5 C15 0.65(9) 2_756 . . . ? Mn1 Na1 Si5 C15 -144.47(8) . . . . ? C7 Na1 Si5 C15 80.60(10) 2_757 . . . ? Si3 Na1 Si5 C15 -149.37(8) . . . . ? N1 Na1 Si5 C16 99.14(9) . . . . ? N2 Na1 Si5 C16 166.72(10) . . . . ? C10 Na1 Si5 C16 166.71(11) . . . . ? C13 Na1 Si5 C16 -90.95(9) 2_756 . . . ? Mn1 Na1 Si5 C16 123.92(8) . . . . ? C7 Na1 Si5 C16 -11.00(10) 2_757 . . . ? Si3 Na1 Si5 C16 119.03(8) . . . . ? C8 Si3 N1 Si2 86.65(12) . . . . ? C9 Si3 N1 Si2 -36.65(13) . . . . ? C10 Si3 N1 Si2 -153.86(10) . . . . ? Na1 Si3 N1 Si2 -138.40(12) . . . . ? C8 Si3 N1 Mn1 -46.98(11) . . . . ? C9 Si3 N1 Mn1 -170.28(9) . . . . ? C10 Si3 N1 Mn1 72.51(11) . . . . ? Na1 Si3 N1 Mn1 87.96(8) . . . . ? C8 Si3 N1 Na1 -134.94(9) . . . . ? C9 Si3 N1 Na1 101.75(9) . . . . ? C10 Si3 N1 Na1 -15.45(10) . . . . ? C6 Si2 N1 Si3 -44.54(14) . . . . ? C5 Si2 N1 Si3 -163.92(10) . . . . ? C7 Si2 N1 Si3 77.77(13) . . . . ? C6 Si2 N1 Mn1 93.11(11) . . . . ? C5 Si2 N1 Mn1 -26.27(10) . . . . ? C7 Si2 N1 Mn1 -144.57(9) . . . . ? C6 Si2 N1 Na1 -171.44(10) . . . . ? C5 Si2 N1 Na1 69.18(11) . . . . ? C7 Si2 N1 Na1 -49.13(12) . . . . ? C1 Mn1 N1 Si3 66.10(12) . . . . ? N2 Mn1 N1 Si3 -98.67(8) . . . . ? Na1 Mn1 N1 Si3 -95.12(8) . . . . ? C1 Mn1 N1 Si2 -74.24(11) . . . . ? N2 Mn1 N1 Si2 121.00(7) . . . . ? Na1 Mn1 N1 Si2 124.55(8) . . . . ? C1 Mn1 N1 Na1 161.22(8) . . . . ? N2 Mn1 N1 Na1 -3.55(6) . . . . ? N2 Na1 N1 Si3 119.39(7) . . . . ? C16 Na1 N1 Si3 -173.24(7) . . . . ? C10 Na1 N1 Si3 10.60(7) . . . . ? C13 Na1 N1 Si3 6.8(2) 2_756 . . . ? Mn1 Na1 N1 Si3 116.40(8) . . . . ? C7 Na1 N1 Si3 -78.32(7) 2_757 . . . ? Si5 Na1 N1 Si3 149.69(5) . . . . ? N2 Na1 N1 Si2 -103.56(9) . . . . ? C16 Na1 N1 Si2 -36.19(10) . . . . ? C10 Na1 N1 Si2 147.65(11) . . . . ? C13 Na1 N1 Si2 143.84(19) 2_756 . . . ? Mn1 Na1 N1 Si2 -106.54(10) . . . . ? C7 Na1 N1 Si2 58.73(10) 2_757 . . . ? Si5 Na1 N1 Si2 -73.26(9) . . . . ? Si3 Na1 N1 Si2 137.05(12) . . . . ? N2 Na1 N1 Mn1 2.98(5) . . . . ? C16 Na1 N1 Mn1 70.36(6) . . . . ? C10 Na1 N1 Mn1 -105.80(7) . . . . ? C13 Na1 N1 Mn1 -109.6(2) 2_756 . . . ? C7 Na1 N1 Mn1 165.28(6) 2_757 . . . ? Si5 Na1 N1 Mn1 33.29(4) . . . . ? Si3 Na1 N1 Mn1 -116.40(8) . . . . ? C12 Si4 N2 Si5 -51.76(13) . . . . ? C11 Si4 N2 Si5 -173.48(10) . . . . ? C13 Si4 N2 Si5 69.76(13) . . . . ? C12 Si4 N2 Mn1 87.68(10) . . . . ? C11 Si4 N2 Mn1 -34.05(11) . . . . ? C13 Si4 N2 Mn1 -150.81(10) . . . . ? C12 Si4 N2 Na1 -176.25(9) . . . . ? C11 Si4 N2 Na1 62.02(12) . . . . ? C13 Si4 N2 Na1 -54.74(12) . . . . ? C14 Si5 N2 Si4 92.07(11) . . . . ? C15 Si5 N2 Si4 -31.34(14) . . . . ? C16 Si5 N2 Si4 -149.06(10) . . . . ? Na1 Si5 N2 Si4 -136.90(12) . . . . ? C14 Si5 N2 Mn1 -43.80(11) . . . . ? C15 Si5 N2 Mn1 -167.20(9) . . . . ? C16 Si5 N2 Mn1 75.08(10) . . . . ? Na1 Si5 N2 Mn1 87.23(8) . . . . ? C14 Si5 N2 Na1 -131.03(8) . . . . ? C15 Si5 N2 Na1 105.57(9) . . . . ? C16 Si5 N2 Na1 -12.16(9) . . . . ? C1 Mn1 N2 Si4 -34.75(13) . . . . ? N1 Mn1 N2 Si4 128.10(7) . . . . ? Na1 Mn1 N2 Si4 124.57(9) . . . . ? C1 Mn1 N2 Si5 106.71(11) . . . . ? N1 Mn1 N2 Si5 -90.44(9) . . . . ? Na1 Mn1 N2 Si5 -93.97(8) . . . . ? C1 Mn1 N2 Na1 -159.33(9) . . . . ? N1 Mn1 N2 Na1 3.52(6) . . . . ? N1 Na1 N2 Si4 -111.03(9) . . . . ? C16 Na1 N2 Si4 143.51(10) . . . . ? C10 Na1 N2 Si4 -44.92(10) . . . . ? C13 Na1 N2 Si4 53.20(10) 2_756 . . . ? Mn1 Na1 N2 Si4 -108.04(10) . . . . ? C7 Na1 N2 Si4 140.73(17) 2_757 . . . ? Si5 Na1 N2 Si4 135.09(12) . . . . ? Si3 Na1 N2 Si4 -82.23(8) . . . . ? N1 Na1 N2 Si5 113.89(6) . . . . ? C16 Na1 N2 Si5 8.42(6) . . . . ? C10 Na1 N2 Si5 179.99(7) . . . . ? C13 Na1 N2 Si5 -81.89(7) 2_756 . . . ? Mn1 Na1 N2 Si5 116.88(8) . . . . ? C7 Na1 N2 Si5 5.6(2) 2_757 . . . ? Si3 Na1 N2 Si5 142.68(5) . . . . ? N1 Na1 N2 Mn1 -2.99(5) . . . . ? C16 Na1 N2 Mn1 -108.46(7) . . . . ? C10 Na1 N2 Mn1 63.12(6) . . . . ? C13 Na1 N2 Mn1 161.24(6) 2_756 . . . ? C7 Na1 N2 Mn1 -111.24(19) 2_757 . . . ? Si5 Na1 N2 Mn1 -116.88(8) . . . . ? Si3 Na1 N2 Mn1 25.80(5) . . . . ? C4 Si1 C1 Mn1 -72.2(2) . . . . ? C2 Si1 C1 Mn1 48.7(2) . . . . ? C3 Si1 C1 Mn1 168.22(18) . . . . ? N2 Mn1 C1 Si1 -86.3(2) . . . . ? N1 Mn1 C1 Si1 113.6(2) . . . . ? Na1 Mn1 C1 Si1 177.99(12) . . . . ? N1 Si2 C7 Na1 -76.8(5) . . . 2_757 ? C6 Si2 C7 Na1 50.1(5) . . . 2_757 ? C5 Si2 C7 Na1 162.8(5) . . . 2_757 ? N1 Si3 C10 Na1 13.65(9) . . . . ? C8 Si3 C10 Na1 136.48(8) . . . . ? C9 Si3 C10 Na1 -109.28(8) . . . . ? N1 Na1 C10 Si3 -9.66(6) . . . . ? N2 Na1 C10 Si3 -88.71(8) . . . . ? C16 Na1 C10 Si3 -32.9(5) . . . . ? C13 Na1 C10 Si3 169.23(8) 2_756 . . . ? Mn1 Na1 C10 Si3 -51.04(7) . . . . ? C7 Na1 C10 Si3 89.51(8) 2_757 . . . ? Si5 Na1 C10 Si3 -88.70(10) . . . . ? N2 Si4 C13 Na1 -74.4(18) . . . 2_756 ? C12 Si4 C13 Na1 51.2(18) . . . 2_756 ? C11 Si4 C13 Na1 164.2(17) . . . 2_756 ? N2 Si5 C16 Na1 10.95(8) . . . . ? C14 Si5 C16 Na1 133.36(8) . . . . ? C15 Si5 C16 Na1 -113.23(8) . . . . ? N1 Na1 C16 Si5 -88.27(7) . . . . ? N2 Na1 C16 Si5 -7.70(6) . . . . ? C10 Na1 C16 Si5 -66.2(4) . . . . ? C13 Na1 C16 Si5 91.72(8) 2_756 . . . ? Mn1 Na1 C16 Si5 -48.09(6) . . . . ? C7 Na1 C16 Si5 171.42(8) 2_757 . . . ? Si3 Na1 C16 Si5 -93.47(8) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.290 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.057 #===END # Attachment 'Compound5.cif' #----------------------------------------------------------- #-------------------------COMPOUND 5------------------------ #----------------------------------------------------------- data_grem261 _database_code_depnum_ccdc_archive 'CCDC 662470' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H72 Mn2 N4 Na2 O Si8' _chemical_formula_weight 813.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8889(2) _cell_length_b 10.8003(3) _cell_length_c 12.7193(4) _cell_angle_alpha 95.656(1) _cell_angle_beta 108.382(1) _cell_angle_gamma 98.832(1) _cell_volume 1130.89(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7103 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 31.00 _exptl_crystal_description 'tablet, parallelogram' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Samples quickly darken on removal from Schlenk. Grem262 obtained from same sample. ; _diffrn_ambient_temperature 150(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 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29980 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 30.93 _reflns_number_total 7145 _reflns_number_gt 5578 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0278P)^2^+0.3815P] 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 7145 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Mn1 Mn 0.11874(3) -0.02279(2) 0.649931(18) 0.01692(6) Uani 1 1 d . . . Na1 Na 0.07912(8) 0.21829(6) 0.55702(5) 0.02628(14) Uani 1 1 d . . . Si1 Si 0.44416(5) 0.18217(4) 0.75006(3) 0.01890(9) Uani 1 1 d . . . Si2 Si 0.18170(5) 0.21363(4) 0.84685(3) 0.01867(8) Uani 1 1 d . . . Si3 Si 0.08606(5) 0.25649(4) 0.29240(4) 0.02111(9) Uani 1 1 d . . . Si4 Si -0.21607(5) 0.30061(4) 0.34225(3) 0.01916(9) Uani 1 1 d . . . O1 O 0.0000 0.0000 0.5000 0.0221(3) Uani 1 2 d S . . N1 N 0.24292(14) 0.15656(11) 0.73872(10) 0.0177(2) Uani 1 1 d . . . N2 N -0.06513(14) 0.21746(11) 0.34776(10) 0.0185(2) Uani 1 1 d . . . C1 C 0.4671(2) 0.07854(17) 0.63072(14) 0.0317(4) Uani 1 1 d . . . H1A H 0.4470 -0.0104 0.6411 0.048 Uiso 1 1 calc R . . H1B H 0.5771 0.1022 0.6289 0.048 Uiso 1 1 calc R . . H1C H 0.3893 0.0898 0.5598 0.048 Uiso 1 1 calc R . . C2 C 0.5289(2) 0.34878(16) 0.73929(16) 0.0324(4) Uani 1 1 d . . . H2A H 0.4702 0.3689 0.6658 0.049 Uiso 1 1 calc R . . H2B H 0.6436 0.3566 0.7480 0.049 Uiso 1 1 calc R . . H2C H 0.5171 0.4079 0.7985 0.049 Uiso 1 1 calc R . . C3 C 0.57858(19) 0.14263(18) 0.88328(14) 0.0329(4) Uani 1 1 d . . . H3A H 0.5924 0.2091 0.9457 0.049 Uiso 1 1 calc R . . H3B H 0.6842 0.1370 0.8765 0.049 Uiso 1 1 calc R . . H3C H 0.5295 0.0611 0.8974 0.049 Uiso 1 1 calc R . . C4 C 0.3064(2) 0.36944(15) 0.93115(14) 0.0304(4) Uani 1 1 d . . . H4A H 0.4176 0.3593 0.9683 0.046 Uiso 1 1 calc R . . H4B H 0.2603 0.3972 0.9879 0.046 Uiso 1 1 calc R . . H4C H 0.3064 0.4331 0.8813 0.046 Uiso 1 1 calc R . . C5 C 0.1869(2) 0.09955(16) 0.94986(14) 0.0296(3) Uani 1 1 d . . . H5A H 0.1478 0.0126 0.9092 0.044 Uiso 1 1 calc R . . H5B H 0.1175 0.1185 0.9934 0.044 Uiso 1 1 calc R . . H5C H 0.2981 0.1081 1.0007 0.044 Uiso 1 1 calc R . . C6 C -0.03012(19) 0.24231(16) 0.78770(15) 0.0285(3) Uani 1 1 d . . . H6A H -0.0292 0.3156 0.7481 0.043 Uiso 1 1 calc R . . H6B H -0.0727 0.2591 0.8489 0.043 Uiso 1 1 calc R . . H6C H -0.0989 0.1672 0.7353 0.043 Uiso 1 1 calc R . . C7 C 0.2536(2) 0.38564(17) 0.38756(18) 0.0418(5) Uani 1 1 d . . . H7A H 0.2095 0.4607 0.4025 0.063 Uiso 1 1 calc R . . H7B H 0.3345 0.4075 0.3515 0.063 Uiso 1 1 calc R . . H7C H 0.3043 0.3562 0.4584 0.063 Uiso 1 1 calc R . . C8 C 0.0168(3) 0.3078(2) 0.15145(16) 0.0424(5) Uani 1 1 d . . . H8A H -0.0657 0.2397 0.0982 0.064 Uiso 1 1 calc R . . H8B H 0.1089 0.3266 0.1250 0.064 Uiso 1 1 calc R . . H8C H -0.0291 0.3841 0.1573 0.064 Uiso 1 1 calc R . . C9 C 0.1842(2) 0.11638(16) 0.27903(15) 0.0307(4) Uani 1 1 d . . . H9A H 0.2149 0.0841 0.3506 0.046 Uiso 1 1 calc R . . H9B H 0.2809 0.1424 0.2590 0.046 Uiso 1 1 calc R . . H9C H 0.1081 0.0495 0.2204 0.046 Uiso 1 1 calc R . . C10 C -0.3961(2) 0.24815(18) 0.21160(15) 0.0349(4) Uani 1 1 d . . . H10A H -0.3637 0.2611 0.1460 0.052 Uiso 1 1 calc R . . H10B H -0.4787 0.2979 0.2138 0.052 Uiso 1 1 calc R . . H10C H -0.4402 0.1580 0.2065 0.052 Uiso 1 1 calc R . . C11 C -0.1519(2) 0.47693(15) 0.34907(15) 0.0284(3) Uani 1 1 d . . . H11A H -0.0612 0.5109 0.4185 0.043 Uiso 1 1 calc R . . H11B H -0.2428 0.5186 0.3479 0.043 Uiso 1 1 calc R . . H11C H -0.1185 0.4929 0.2844 0.043 Uiso 1 1 calc R . . C12 C -0.2849(2) 0.27936(16) 0.46620(14) 0.0294(3) Uani 1 1 d . . . H12A H -0.3069 0.1889 0.4715 0.044 Uiso 1 1 calc R . . H12B H -0.3837 0.3134 0.4565 0.044 Uiso 1 1 calc R . . H12C H -0.2001 0.3247 0.5350 0.044 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 0.01821(10) 0.01566(10) 0.01477(10) 0.00295(8) 0.00310(8) 0.00195(8) Na1 0.0334(3) 0.0181(3) 0.0204(3) 0.0032(2) 0.0002(3) 0.0032(2) Si1 0.01584(18) 0.02087(19) 0.01851(19) 0.00267(15) 0.00466(15) 0.00182(14) Si2 0.01880(18) 0.01974(19) 0.01657(19) 0.00149(15) 0.00608(15) 0.00165(15) Si3 0.0235(2) 0.01864(19) 0.0240(2) 0.00487(16) 0.01175(17) 0.00356(15) Si4 0.01863(18) 0.01940(19) 0.0198(2) 0.00504(15) 0.00579(15) 0.00478(15) O1 0.0263(7) 0.0178(7) 0.0160(7) 0.0035(5) -0.0008(6) 0.0027(6) N1 0.0164(5) 0.0184(6) 0.0160(6) 0.0012(4) 0.0039(4) 0.0007(4) N2 0.0201(6) 0.0168(6) 0.0196(6) 0.0054(4) 0.0069(5) 0.0038(4) C1 0.0271(8) 0.0381(9) 0.0305(9) -0.0024(7) 0.0133(7) 0.0053(7) C2 0.0259(8) 0.0273(8) 0.0458(11) 0.0085(7) 0.0154(7) 0.0016(6) C3 0.0224(8) 0.0453(10) 0.0280(9) 0.0089(7) 0.0021(7) 0.0089(7) C4 0.0350(9) 0.0264(8) 0.0258(8) -0.0038(6) 0.0101(7) -0.0004(7) C5 0.0353(9) 0.0328(9) 0.0219(8) 0.0079(7) 0.0110(7) 0.0051(7) C6 0.0240(7) 0.0285(8) 0.0359(9) 0.0074(7) 0.0125(7) 0.0068(6) C7 0.0330(9) 0.0313(9) 0.0589(13) -0.0088(9) 0.0225(9) -0.0058(7) C8 0.0574(12) 0.0507(12) 0.0374(10) 0.0242(9) 0.0297(10) 0.0241(10) C9 0.0297(8) 0.0278(8) 0.0396(10) 0.0048(7) 0.0171(7) 0.0091(7) C10 0.0264(8) 0.0437(10) 0.0293(9) 0.0036(8) 0.0019(7) 0.0083(7) C11 0.0317(8) 0.0229(8) 0.0344(9) 0.0104(7) 0.0123(7) 0.0101(6) C12 0.0334(9) 0.0269(8) 0.0309(9) 0.0017(7) 0.0174(7) 0.0029(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.9272(2) . ? Mn1 N2 2.0884(12) 2_556 ? Mn1 N1 2.0909(12) . ? Mn1 Na1 2.9877(6) . ? Mn1 Na1 3.0536(6) 2_556 ? Na1 O1 2.3262(6) . ? Na1 N1 2.5269(13) . ? Na1 N2 2.5627(14) . ? Na1 Mn1 3.0536(6) 2_556 ? Na1 Si4 3.4368(7) . ? Na1 Si3 3.4495(8) . ? Na1 Si1 3.5018(7) . ? Na1 Si2 3.5149(7) . ? Si1 N1 1.7247(12) . ? Si1 C3 1.8718(17) . ? Si1 C2 1.8765(16) . ? Si1 C1 1.8787(17) . ? Si2 N1 1.7249(12) . ? Si2 C4 1.8794(16) . ? Si2 C5 1.8800(16) . ? Si2 C6 1.8812(16) . ? Si3 N2 1.7208(12) . ? Si3 C8 1.8722(19) . ? Si3 C7 1.8764(18) . ? Si3 C9 1.8784(17) . ? Si4 N2 1.7130(13) . ? Si4 C10 1.8715(17) . ? Si4 C12 1.8842(16) . ? Si4 C11 1.8873(16) . ? O1 Mn1 1.9272(2) 2_556 ? O1 Na1 2.3262(6) 2_556 ? N2 Mn1 2.0884(12) 2_556 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? 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 . ? 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 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? 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 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 N2 105.36(3) . 2_556 ? O1 Mn1 N1 107.23(3) . . ? N2 Mn1 N1 147.42(5) 2_556 . ? O1 Mn1 Na1 51.115(12) . . ? N2 Mn1 Na1 155.80(4) 2_556 . ? N1 Mn1 Na1 56.41(3) . . ? O1 Mn1 Na1 49.605(12) . 2_556 ? N2 Mn1 Na1 56.07(4) 2_556 2_556 ? N1 Mn1 Na1 156.23(4) . 2_556 ? Na1 Mn1 Na1 100.720(16) . 2_556 ? O1 Na1 N1 83.54(3) . . ? O1 Na1 N2 81.46(3) . . ? N1 Na1 N2 161.97(5) . . ? O1 Na1 Mn1 40.158(10) . . ? N1 Na1 Mn1 43.57(3) . . ? N2 Na1 Mn1 121.44(3) . . ? O1 Na1 Mn1 39.122(10) . 2_556 ? N1 Na1 Mn1 122.50(3) . 2_556 ? N2 Na1 Mn1 42.55(3) . 2_556 ? Mn1 Na1 Mn1 79.280(16) . 2_556 ? O1 Na1 Si4 96.47(2) . . ? N1 Na1 Si4 165.53(4) . . ? N2 Na1 Si4 28.74(3) . . ? Mn1 Na1 Si4 133.65(2) . . ? Mn1 Na1 Si4 59.752(13) 2_556 . ? O1 Na1 Si3 89.95(2) . . ? N1 Na1 Si3 141.96(4) . . ? N2 Na1 Si3 28.72(3) . . ? Mn1 Na1 Si3 122.84(2) . . ? Mn1 Na1 Si3 57.869(13) 2_556 . ? Si4 Na1 Si3 52.415(13) . . ? O1 Na1 Si1 91.27(2) . . ? N1 Na1 Si1 27.67(3) . . ? N2 Na1 Si1 142.81(4) . . ? Mn1 Na1 Si1 57.817(13) . . ? Mn1 Na1 Si1 123.71(2) 2_556 . ? Si4 Na1 Si1 165.69(2) . . ? Si3 Na1 Si1 115.82(2) . . ? O1 Na1 Si2 96.97(2) . . ? N1 Na1 Si2 27.45(3) . . ? N2 Na1 Si2 166.08(4) . . ? Mn1 Na1 Si2 59.190(13) . . ? Mn1 Na1 Si2 133.32(2) 2_556 . ? Si4 Na1 Si2 139.26(2) . . ? Si3 Na1 Si2 164.79(2) . . ? Si1 Na1 Si2 50.763(13) . . ? N1 Si1 C3 113.36(7) . . ? N1 Si1 C2 114.07(7) . . ? C3 Si1 C2 107.20(8) . . ? N1 Si1 C1 108.72(7) . . ? C3 Si1 C1 107.30(8) . . ? C2 Si1 C1 105.73(8) . . ? N1 Si1 Na1 42.88(4) . . ? C3 Si1 Na1 156.22(6) . . ? C2 Si1 Na1 87.12(6) . . ? C1 Si1 Na1 86.07(6) . . ? N1 Si2 C4 114.70(7) . . ? N1 Si2 C5 111.76(7) . . ? C4 Si2 C5 106.11(8) . . ? N1 Si2 C6 109.37(7) . . ? C4 Si2 C6 105.54(8) . . ? C5 Si2 C6 109.06(8) . . ? N1 Si2 Na1 42.47(4) . . ? C4 Si2 Na1 111.76(6) . . ? C5 Si2 Na1 140.94(6) . . ? C6 Si2 Na1 69.88(5) . . ? N2 Si3 C8 114.39(8) . . ? N2 Si3 C7 112.15(7) . . ? C8 Si3 C7 107.41(10) . . ? N2 Si3 C9 109.48(7) . . ? C8 Si3 C9 107.99(9) . . ? C7 Si3 C9 104.92(9) . . ? N2 Si3 Na1 45.69(4) . . ? C8 Si3 Na1 155.94(6) . . ? C7 Si3 Na1 76.21(7) . . ? C9 Si3 Na1 93.50(6) . . ? N2 Si4 C10 113.21(7) . . ? N2 Si4 C12 109.06(7) . . ? C10 Si4 C12 108.08(8) . . ? N2 Si4 C11 113.86(7) . . ? C10 Si4 C11 105.75(8) . . ? C12 Si4 C11 106.51(8) . . ? N2 Si4 Na1 46.00(4) . . ? C10 Si4 Na1 148.17(6) . . ? C12 Si4 Na1 68.86(6) . . ? C11 Si4 Na1 105.36(6) . . ? Mn1 O1 Mn1 180.0 2_556 . ? Mn1 O1 Na1 91.273(16) 2_556 . ? Mn1 O1 Na1 88.727(16) . . ? Mn1 O1 Na1 88.727(16) 2_556 2_556 ? Mn1 O1 Na1 91.273(16) . 2_556 ? Na1 O1 Na1 180.0 . 2_556 ? Si1 N1 Si2 121.35(7) . . ? Si1 N1 Mn1 111.96(6) . . ? Si2 N1 Mn1 116.12(6) . . ? Si1 N1 Na1 109.45(6) . . ? Si2 N1 Na1 110.09(6) . . ? Mn1 N1 Na1 80.02(4) . . ? Si4 N2 Si3 124.66(7) . . ? Si4 N2 Mn1 117.17(6) . 2_556 ? Si3 N2 Mn1 112.03(6) . 2_556 ? Si4 N2 Na1 105.25(6) . . ? Si3 N2 Na1 105.59(6) . . ? Mn1 N2 Na1 81.38(4) 2_556 . ? 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 . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si4 C10 H10A 109.5 . . ? Si4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si4 C11 H11A 109.5 . . ? Si4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si4 C12 H12A 109.5 . . ? Si4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 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 Mn1 Na1 O1 -15.32(9) 2_556 . . . ? N1 Mn1 Na1 O1 172.92(4) . . . . ? Na1 Mn1 Na1 O1 0.0 2_556 . . . ? O1 Mn1 Na1 N1 -172.92(4) . . . . ? N2 Mn1 Na1 N1 171.75(10) 2_556 . . . ? Na1 Mn1 Na1 N1 -172.92(4) 2_556 . . . ? O1 Mn1 Na1 N2 -5.94(4) . . . . ? N2 Mn1 Na1 N2 -21.26(12) 2_556 . . . ? N1 Mn1 Na1 N2 166.98(6) . . . . ? Na1 Mn1 Na1 N2 -5.94(4) 2_556 . . . ? O1 Mn1 Na1 Mn1 0.0 . . . 2_556 ? N2 Mn1 Na1 Mn1 -15.32(9) 2_556 . . 2_556 ? N1 Mn1 Na1 Mn1 172.92(4) . . . 2_556 ? Na1 Mn1 Na1 Mn1 0.0 2_556 . . 2_556 ? O1 Mn1 Na1 Si4 27.23(2) . . . . ? N2 Mn1 Na1 Si4 11.91(10) 2_556 . . . ? N1 Mn1 Na1 Si4 -159.84(5) . . . . ? Na1 Mn1 Na1 Si4 27.23(2) 2_556 . . . ? O1 Mn1 Na1 Si3 -39.964(17) . . . . ? N2 Mn1 Na1 Si3 -55.29(10) 2_556 . . . ? N1 Mn1 Na1 Si3 132.96(5) . . . . ? Na1 Mn1 Na1 Si3 -39.964(17) 2_556 . . . ? O1 Mn1 Na1 Si1 -141.863(18) . . . . ? N2 Mn1 Na1 Si1 -157.19(9) 2_556 . . . ? N1 Mn1 Na1 Si1 31.06(4) . . . . ? Na1 Mn1 Na1 Si1 -141.864(18) 2_556 . . . ? O1 Mn1 Na1 Si2 157.798(18) . . . . ? N2 Mn1 Na1 Si2 142.47(9) 2_556 . . . ? N1 Mn1 Na1 Si2 -29.28(4) . . . . ? Na1 Mn1 Na1 Si2 157.798(18) 2_556 . . . ? O1 Na1 Si1 N1 -73.45(6) . . . . ? N2 Na1 Si1 N1 -150.95(8) . . . . ? Mn1 Na1 Si1 N1 -49.97(6) . . . . ? Mn1 Na1 Si1 N1 -96.81(6) 2_556 . . . ? Si4 Na1 Si1 N1 163.66(11) . . . . ? Si3 Na1 Si1 N1 -164.01(6) . . . . ? Si2 Na1 Si1 N1 24.52(6) . . . . ? O1 Na1 Si1 C3 -75.99(16) . . . . ? N1 Na1 Si1 C3 -2.54(16) . . . . ? N2 Na1 Si1 C3 -153.49(16) . . . . ? Mn1 Na1 Si1 C3 -52.51(15) . . . . ? Mn1 Na1 Si1 C3 -99.35(16) 2_556 . . . ? Si4 Na1 Si1 C3 161.11(16) . . . . ? Si3 Na1 Si1 C3 -166.55(15) . . . . ? Si2 Na1 Si1 C3 21.97(15) . . . . ? O1 Na1 Si1 C2 155.69(6) . . . . ? N1 Na1 Si1 C2 -130.87(8) . . . . ? N2 Na1 Si1 C2 78.19(8) . . . . ? Mn1 Na1 Si1 C2 179.16(6) . . . . ? Mn1 Na1 Si1 C2 132.33(6) 2_556 . . . ? Si4 Na1 Si1 C2 32.79(11) . . . . ? Si3 Na1 Si1 C2 65.12(6) . . . . ? Si2 Na1 Si1 C2 -106.35(6) . . . . ? O1 Na1 Si1 C1 49.69(6) . . . . ? N1 Na1 Si1 C1 123.14(8) . . . . ? N2 Na1 Si1 C1 -27.80(8) . . . . ? Mn1 Na1 Si1 C1 73.17(6) . . . . ? Mn1 Na1 Si1 C1 26.33(6) 2_556 . . . ? Si4 Na1 Si1 C1 -73.20(11) . . . . ? Si3 Na1 Si1 C1 -40.87(6) . . . . ? Si2 Na1 Si1 C1 147.66(6) . . . . ? O1 Na1 Si2 N1 61.22(6) . . . . ? N2 Na1 Si2 N1 143.82(16) . . . . ? Mn1 Na1 Si2 N1 47.00(6) . . . . ? Mn1 Na1 Si2 N1 77.69(6) 2_556 . . . ? Si4 Na1 Si2 N1 169.63(7) . . . . ? Si3 Na1 Si2 N1 -55.31(10) . . . . ? Si1 Na1 Si2 N1 -24.72(6) . . . . ? O1 Na1 Si2 C4 164.52(6) . . . . ? N1 Na1 Si2 C4 103.31(8) . . . . ? N2 Na1 Si2 C4 -112.87(16) . . . . ? Mn1 Na1 Si2 C4 150.31(6) . . . . ? Mn1 Na1 Si2 C4 -179.00(6) 2_556 . . . ? Si4 Na1 Si2 C4 -87.06(7) . . . . ? Si3 Na1 Si2 C4 48.00(11) . . . . ? Si1 Na1 Si2 C4 78.59(6) . . . . ? O1 Na1 Si2 C5 -0.45(10) . . . . ? N1 Na1 Si2 C5 -61.66(11) . . . . ? N2 Na1 Si2 C5 82.16(18) . . . . ? Mn1 Na1 Si2 C5 -14.66(9) . . . . ? Mn1 Na1 Si2 C5 16.02(10) 2_556 . . . ? Si4 Na1 Si2 C5 107.96(9) . . . . ? Si3 Na1 Si2 C5 -116.97(12) . . . . ? Si1 Na1 Si2 C5 -86.38(9) . . . . ? O1 Na1 Si2 C6 -96.21(6) . . . . ? N1 Na1 Si2 C6 -157.43(8) . . . . ? N2 Na1 Si2 C6 -13.61(16) . . . . ? Mn1 Na1 Si2 C6 -110.43(6) . . . . ? Mn1 Na1 Si2 C6 -79.74(6) 2_556 . . . ? Si4 Na1 Si2 C6 12.20(6) . . . . ? Si3 Na1 Si2 C6 147.26(10) . . . . ? Si1 Na1 Si2 C6 177.85(6) . . . . ? O1 Na1 Si3 N2 72.08(6) . . . . ? N1 Na1 Si3 N2 151.50(8) . . . . ? Mn1 Na1 Si3 N2 96.56(6) . . . . ? Mn1 Na1 Si3 N2 48.38(6) 2_556 . . . ? Si4 Na1 Si3 N2 -26.12(6) . . . . ? Si1 Na1 Si3 N2 163.48(6) . . . . ? Si2 Na1 Si3 N2 -170.56(11) . . . . ? O1 Na1 Si3 C8 111.67(18) . . . . ? N1 Na1 Si3 C8 -168.92(18) . . . . ? N2 Na1 Si3 C8 39.58(18) . . . . ? Mn1 Na1 Si3 C8 136.14(17) . . . . ? Mn1 Na1 Si3 C8 87.96(18) 2_556 . . . ? Si4 Na1 Si3 C8 13.46(17) . . . . ? Si1 Na1 Si3 C8 -156.94(17) . . . . ? Si2 Na1 Si3 C8 -130.97(18) . . . . ? O1 Na1 Si3 C7 -146.46(7) . . . . ? N1 Na1 Si3 C7 -67.05(9) . . . . ? N2 Na1 Si3 C7 141.46(9) . . . . ? Mn1 Na1 Si3 C7 -121.99(7) . . . . ? Mn1 Na1 Si3 C7 -170.17(7) 2_556 . . . ? Si4 Na1 Si3 C7 115.33(7) . . . . ? Si1 Na1 Si3 C7 -55.07(7) . . . . ? Si2 Na1 Si3 C7 -29.10(11) . . . . ? O1 Na1 Si3 C9 -41.95(6) . . . . ? N1 Na1 Si3 C9 37.46(8) . . . . ? N2 Na1 Si3 C9 -114.03(8) . . . . ? Mn1 Na1 Si3 C9 -17.48(6) . . . . ? Mn1 Na1 Si3 C9 -65.66(5) 2_556 . . . ? Si4 Na1 Si3 C9 -140.16(6) . . . . ? Si1 Na1 Si3 C9 49.45(6) . . . . ? Si2 Na1 Si3 C9 75.41(10) . . . . ? O1 Na1 Si4 N2 -58.83(6) . . . . ? N1 Na1 Si4 N2 -148.02(15) . . . . ? Mn1 Na1 Si4 N2 -76.11(6) . . . . ? Mn1 Na1 Si4 N2 -44.74(5) 2_556 . . . ? Si3 Na1 Si4 N2 26.10(5) . . . . ? Si1 Na1 Si4 N2 63.52(10) . . . . ? Si2 Na1 Si4 N2 -167.42(6) . . . . ? O1 Na1 Si4 C10 0.07(12) . . . . ? N1 Na1 Si4 C10 -89.12(18) . . . . ? N2 Na1 Si4 C10 58.90(12) . . . . ? Mn1 Na1 Si4 C10 -17.21(12) . . . . ? Mn1 Na1 Si4 C10 14.15(11) 2_556 . . . ? Si3 Na1 Si4 C10 85.00(11) . . . . ? Si1 Na1 Si4 C10 122.41(14) . . . . ? Si2 Na1 Si4 C10 -108.52(12) . . . . ? O1 Na1 Si4 C12 90.52(6) . . . . ? N1 Na1 Si4 C12 1.33(15) . . . . ? N2 Na1 Si4 C12 149.35(8) . . . . ? Mn1 Na1 Si4 C12 73.24(6) . . . . ? Mn1 Na1 Si4 C12 104.60(6) 2_556 . . . ? Si3 Na1 Si4 C12 175.45(6) . . . . ? Si1 Na1 Si4 C12 -147.14(11) . . . . ? Si2 Na1 Si4 C12 -18.07(6) . . . . ? O1 Na1 Si4 C11 -167.37(6) . . . . ? N1 Na1 Si4 C11 103.44(15) . . . . ? N2 Na1 Si4 C11 -108.54(8) . . . . ? Mn1 Na1 Si4 C11 175.35(6) . . . . ? Mn1 Na1 Si4 C11 -153.29(6) 2_556 . . . ? Si3 Na1 Si4 C11 -82.44(6) . . . . ? Si1 Na1 Si4 C11 -45.03(11) . . . . ? Si2 Na1 Si4 C11 84.04(6) . . . . ? N2 Mn1 O1 Mn1 -14(100) 2_556 . . 2_556 ? N1 Mn1 O1 Mn1 166(100) . . . 2_556 ? Na1 Mn1 O1 Mn1 172(100) . . . 2_556 ? Na1 Mn1 O1 Mn1 -8(100) 2_556 . . 2_556 ? N2 Mn1 O1 Na1 173.55(4) 2_556 . . . ? N1 Mn1 O1 Na1 -6.17(4) . . . . ? Na1 Mn1 O1 Na1 180.0 2_556 . . . ? N2 Mn1 O1 Na1 -6.45(4) 2_556 . . 2_556 ? N1 Mn1 O1 Na1 173.83(4) . . . 2_556 ? Na1 Mn1 O1 Na1 180.0 . . . 2_556 ? N1 Na1 O1 Mn1 -175.10(3) . . . 2_556 ? N2 Na1 O1 Mn1 -5.12(3) . . . 2_556 ? Mn1 Na1 O1 Mn1 180.0 . . . 2_556 ? Si4 Na1 O1 Mn1 19.465(16) . . . 2_556 ? Si3 Na1 O1 Mn1 -32.660(15) . . . 2_556 ? Si1 Na1 O1 Mn1 -148.481(14) . . . 2_556 ? Si2 Na1 O1 Mn1 160.916(16) . . . 2_556 ? N1 Na1 O1 Mn1 4.90(3) . . . . ? N2 Na1 O1 Mn1 174.88(3) . . . . ? Mn1 Na1 O1 Mn1 180.0 2_556 . . . ? Si4 Na1 O1 Mn1 -160.535(16) . . . . ? Si3 Na1 O1 Mn1 147.340(15) . . . . ? Si1 Na1 O1 Mn1 31.519(14) . . . . ? Si2 Na1 O1 Mn1 -19.084(16) . . . . ? N1 Na1 O1 Na1 64(100) . . . 2_556 ? N2 Na1 O1 Na1 -126(100) . . . 2_556 ? Mn1 Na1 O1 Na1 59(100) . . . 2_556 ? Mn1 Na1 O1 Na1 -121(100) 2_556 . . 2_556 ? Si4 Na1 O1 Na1 -101(100) . . . 2_556 ? Si3 Na1 O1 Na1 -153(100) . . . 2_556 ? Si1 Na1 O1 Na1 91(100) . . . 2_556 ? Si2 Na1 O1 Na1 40(100) . . . 2_556 ? C3 Si1 N1 Si2 48.97(11) . . . . ? C2 Si1 N1 Si2 -74.10(10) . . . . ? C1 Si1 N1 Si2 168.19(9) . . . . ? Na1 Si1 N1 Si2 -129.92(11) . . . . ? C3 Si1 N1 Mn1 -94.31(9) . . . . ? C2 Si1 N1 Mn1 142.62(8) . . . . ? C1 Si1 N1 Mn1 24.91(9) . . . . ? Na1 Si1 N1 Mn1 86.80(7) . . . . ? C3 Si1 N1 Na1 178.88(7) . . . . ? C2 Si1 N1 Na1 55.81(9) . . . . ? C1 Si1 N1 Na1 -61.89(8) . . . . ? C4 Si2 N1 Si1 33.80(11) . . . . ? C5 Si2 N1 Si1 -87.03(9) . . . . ? C6 Si2 N1 Si1 152.10(8) . . . . ? Na1 Si2 N1 Si1 129.64(10) . . . . ? C4 Si2 N1 Mn1 175.65(7) . . . . ? C5 Si2 N1 Mn1 54.83(9) . . . . ? C6 Si2 N1 Mn1 -66.04(8) . . . . ? Na1 Si2 N1 Mn1 -88.50(7) . . . . ? C4 Si2 N1 Na1 -95.85(8) . . . . ? C5 Si2 N1 Na1 143.33(7) . . . . ? C6 Si2 N1 Na1 22.46(8) . . . . ? O1 Mn1 N1 Si1 -101.31(6) . . . . ? N2 Mn1 N1 Si1 79.19(10) 2_556 . . . ? Na1 Mn1 N1 Si1 -107.07(7) . . . . ? Na1 Mn1 N1 Si1 -89.60(10) 2_556 . . . ? O1 Mn1 N1 Si2 113.35(6) . . . . ? N2 Mn1 N1 Si2 -66.15(11) 2_556 . . . ? Na1 Mn1 N1 Si2 107.58(7) . . . . ? Na1 Mn1 N1 Si2 125.06(7) 2_556 . . . ? O1 Mn1 N1 Na1 5.76(4) . . . . ? N2 Mn1 N1 Na1 -173.73(7) 2_556 . . . ? Na1 Mn1 N1 Na1 17.47(11) 2_556 . . . ? O1 Na1 N1 Si1 105.32(6) . . . . ? N2 Na1 N1 Si1 71.53(16) . . . . ? Mn1 Na1 N1 Si1 109.91(7) . . . . ? Mn1 Na1 N1 Si1 101.66(6) 2_556 . . . ? Si4 Na1 N1 Si1 -163.84(11) . . . . ? Si3 Na1 N1 Si1 23.73(9) . . . . ? Si2 Na1 N1 Si1 -135.78(9) . . . . ? O1 Na1 N1 Si2 -118.89(5) . . . . ? N2 Na1 N1 Si2 -152.68(13) . . . . ? Mn1 Na1 N1 Si2 -114.31(7) . . . . ? Mn1 Na1 N1 Si2 -122.56(5) 2_556 . . . ? Si4 Na1 N1 Si2 -28.06(18) . . . . ? Si3 Na1 N1 Si2 159.51(4) . . . . ? Si1 Na1 N1 Si2 135.78(9) . . . . ? O1 Na1 N1 Mn1 -4.59(3) . . . . ? N2 Na1 N1 Mn1 -38.38(16) . . . . ? Mn1 Na1 N1 Mn1 -8.25(5) 2_556 . . . ? Si4 Na1 N1 Mn1 86.25(14) . . . . ? Si3 Na1 N1 Mn1 -86.18(5) . . . . ? Si1 Na1 N1 Mn1 -109.91(7) . . . . ? Si2 Na1 N1 Mn1 114.31(7) . . . . ? C10 Si4 N2 Si3 87.61(10) . . . . ? C12 Si4 N2 Si3 -152.03(9) . . . . ? C11 Si4 N2 Si3 -33.23(12) . . . . ? Na1 Si4 N2 Si3 -121.82(10) . . . . ? C10 Si4 N2 Mn1 -62.56(10) . . . 2_556 ? C12 Si4 N2 Mn1 57.81(9) . . . 2_556 ? C11 Si4 N2 Mn1 176.60(7) . . . 2_556 ? Na1 Si4 N2 Mn1 88.01(7) . . . 2_556 ? C10 Si4 N2 Na1 -150.57(7) . . . . ? C12 Si4 N2 Na1 -30.21(8) . . . . ? C11 Si4 N2 Na1 88.59(8) . . . . ? C8 Si3 N2 Si4 -41.76(12) . . . . ? C7 Si3 N2 Si4 80.87(11) . . . . ? C9 Si3 N2 Si4 -163.10(9) . . . . ? Na1 Si3 N2 Si4 121.67(10) . . . . ? C8 Si3 N2 Mn1 109.73(9) . . . 2_556 ? C7 Si3 N2 Mn1 -127.64(9) . . . 2_556 ? C9 Si3 N2 Mn1 -11.62(9) . . . 2_556 ? Na1 Si3 N2 Mn1 -86.85(7) . . . 2_556 ? C8 Si3 N2 Na1 -163.42(8) . . . . ? C7 Si3 N2 Na1 -40.79(10) . . . . ? C9 Si3 N2 Na1 75.23(8) . . . . ? O1 Na1 N2 Si4 120.71(5) . . . . ? N1 Na1 N2 Si4 154.69(13) . . . . ? Mn1 Na1 N2 Si4 124.58(5) . . . . ? Mn1 Na1 N2 Si4 115.93(7) 2_556 . . . ? Si3 Na1 N2 Si4 -133.48(9) . . . . ? Si1 Na1 N2 Si4 -158.54(4) . . . . ? Si2 Na1 N2 Si4 36.21(18) . . . . ? O1 Na1 N2 Si3 -105.81(5) . . . . ? N1 Na1 N2 Si3 -71.83(16) . . . . ? Mn1 Na1 N2 Si3 -101.94(5) . . . . ? Mn1 Na1 N2 Si3 -110.59(7) 2_556 . . . ? Si4 Na1 N2 Si3 133.48(9) . . . . ? Si1 Na1 N2 Si3 -25.06(9) . . . . ? Si2 Na1 N2 Si3 169.69(11) . . . . ? O1 Na1 N2 Mn1 4.78(3) . . . 2_556 ? N1 Na1 N2 Mn1 38.75(16) . . . 2_556 ? Mn1 Na1 N2 Mn1 8.65(5) . . . 2_556 ? Si4 Na1 N2 Mn1 -115.93(7) . . . 2_556 ? Si3 Na1 N2 Mn1 110.59(7) . . . 2_556 ? Si1 Na1 N2 Mn1 85.53(6) . . . 2_556 ? Si2 Na1 N2 Mn1 -79.72(15) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.93 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.370 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.063 #===END