# Electronic Supplementary Material for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _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_section_title ; Dizincation and dimagnesiation of benzene using alkali-metal-mediated metallation ; loop_ _publ_author_name 'R. E. Mulvey' 'David R. Armstrong' 'W. Clegg' 'Sophie Dale' 'David V. Graham' 'Eva Hevia' ; L.M.Hogg ; 'Gordon W Honeyman' 'A. R. Kennedy' # Attachment 'cif.txt' data_rem331_compound_1 _database_code_depnum_ccdc_archive 'CCDC 621932' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H90 N6 Na2 Zn2' _chemical_formula_sum 'C44 H90 N6 Na2 Zn2' _chemical_formula_weight 879.94 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' N N 0.0061 0.0033 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.3869(17) _cell_length_b 21.158(4) _cell_length_c 14.333(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.72(3) _cell_angle_gamma 90.00 _cell_volume 2543.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 556 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 0.993 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details 'Bruker SHELXTL' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24259 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.98 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5770 _reflns_number_gt 4019 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DIRAX _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0223P)^2^+0.7922P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary . _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5770 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.14358(3) 0.505124(10) 0.733015(14) 0.01816(7) Uani 1 1 d . . . Na1 Na 0.20768(9) 0.38459(3) 0.61523(5) 0.02235(18) Uani 1 1 d . . . C1 C 0.0622(2) 0.49957(9) 0.59663(12) 0.0190(4) Uani 1 1 d . . . C2 C 0.1602(2) 0.49780(9) 0.51745(12) 0.0201(4) Uani 1 1 d . . . H2 H 0.2725 0.4964 0.5268 0.024 Uiso 1 1 calc R . . C3 C -0.1007(2) 0.50206(9) 0.57409(12) 0.0203(4) Uani 1 1 d . . . H3 H -0.1746 0.5037 0.6237 0.024 Uiso 1 1 calc R . . C4 C 0.0877(2) 0.58379(9) 0.80924(13) 0.0249(5) Uani 1 1 d . . . C5 C -0.0943(3) 0.58923(12) 0.81197(16) 0.0438(6) Uani 1 1 d . . . H5A H -0.1380 0.5532 0.8463 0.066 Uiso 1 1 calc R . . H5B H -0.1376 0.5893 0.7481 0.066 Uiso 1 1 calc R . . H5C H -0.1239 0.6286 0.8433 0.066 Uiso 1 1 calc R . . C6 C 0.1499(3) 0.64125(11) 0.75574(16) 0.0504(7) Uani 1 1 d . . . H6A H 0.1092 0.6800 0.7842 0.076 Uiso 1 1 calc R . . H6B H 0.1137 0.6389 0.6906 0.076 Uiso 1 1 calc R . . H6C H 0.2668 0.6415 0.7582 0.076 Uiso 1 1 calc R . . C7 C 0.1516(3) 0.58695(11) 0.90882(14) 0.0354(6) Uani 1 1 d . . . H7A H 0.2685 0.5870 0.9083 0.053 Uiso 1 1 calc R . . H7B H 0.1141 0.5502 0.9438 0.053 Uiso 1 1 calc R . . H7C H 0.1136 0.6257 0.9386 0.053 Uiso 1 1 calc R . . N1 N 0.27163(18) 0.42637(7) 0.76572(10) 0.0185(4) Uani 1 1 d . . . C8 C 0.4426(2) 0.43995(10) 0.78552(14) 0.0250(5) Uani 1 1 d . . . C9 C 0.4761(2) 0.45399(10) 0.88952(14) 0.0290(5) Uani 1 1 d . . . H9A H 0.5928 0.4565 0.9002 0.035 Uiso 1 1 calc R . . H9B H 0.4298 0.4956 0.9054 0.035 Uiso 1 1 calc R . . C10 C 0.4071(3) 0.40393(10) 0.95360(15) 0.0339(5) Uani 1 1 d . . . H10A H 0.4609 0.3629 0.9429 0.041 Uiso 1 1 calc R . . H10B H 0.4251 0.4162 1.0196 0.041 Uiso 1 1 calc R . . C11 C 0.2295(3) 0.39749(10) 0.93371(13) 0.0299(5) Uani 1 1 d . . . H11A H 0.1757 0.4374 0.9509 0.036 Uiso 1 1 calc R . . H11B H 0.1860 0.3634 0.9734 0.036 Uiso 1 1 calc R . . C12 C 0.1911(2) 0.38244(9) 0.83095(13) 0.0227(4) Uani 1 1 d . . . C13 C 0.4871(2) 0.49882(11) 0.72945(15) 0.0367(5) Uani 1 1 d . . . H13A H 0.4678 0.4909 0.6629 0.055 Uiso 1 1 calc R . . H13B H 0.6002 0.5086 0.7399 0.055 Uiso 1 1 calc R . . H13C H 0.4219 0.5346 0.7496 0.055 Uiso 1 1 calc R . . C14 C 0.5561(3) 0.38686(12) 0.75269(17) 0.0411(6) Uani 1 1 d . . . H14A H 0.5435 0.3497 0.7927 0.062 Uiso 1 1 calc R . . H14B H 0.6666 0.4018 0.7567 0.062 Uiso 1 1 calc R . . H14C H 0.5299 0.3756 0.6880 0.062 Uiso 1 1 calc R . . C15 C 0.0114(2) 0.39029(10) 0.81546(15) 0.0303(5) Uani 1 1 d . . . H15A H -0.0200 0.4335 0.8319 0.045 Uiso 1 1 calc R . . H15B H -0.0457 0.3602 0.8548 0.045 Uiso 1 1 calc R . . H15C H -0.0153 0.3823 0.7498 0.045 Uiso 1 1 calc R . . C16 C 0.2303(3) 0.31184(9) 0.81192(14) 0.0311(5) Uani 1 1 d . . . H16A H 0.2116 0.3024 0.7457 0.047 Uiso 1 1 calc R . . H16B H 0.1618 0.2849 0.8500 0.047 Uiso 1 1 calc R . . H16C H 0.3423 0.3036 0.8280 0.047 Uiso 1 1 calc R . . N2 N 0.3605(2) 0.33013(8) 0.49325(11) 0.0267(4) Uani 1 1 d . . . C17 C 0.2332(3) 0.30428(11) 0.43375(15) 0.0378(6) Uani 1 1 d . . . H17A H 0.2820 0.2790 0.3835 0.045 Uiso 1 1 calc R . . H17B H 0.1750 0.3398 0.4039 0.045 Uiso 1 1 calc R . . C18 C 0.1148(3) 0.26329(11) 0.48465(16) 0.0381(6) Uani 1 1 d . . . H18A H 0.0356 0.2469 0.4389 0.046 Uiso 1 1 calc R . . H18B H 0.1720 0.2266 0.5117 0.046 Uiso 1 1 calc R . . N3 N 0.02927(19) 0.29618(8) 0.55993(12) 0.0269(4) Uani 1 1 d . . . C19 C 0.4583(3) 0.27971(10) 0.53449(16) 0.0359(5) Uani 1 1 d . . . H19A H 0.4962 0.2517 0.4850 0.054 Uiso 1 1 calc R . . H19B H 0.3942 0.2554 0.5785 0.054 Uiso 1 1 calc R . . H19C H 0.5498 0.2983 0.5676 0.054 Uiso 1 1 calc R . . C20 C 0.4621(3) 0.37171(11) 0.43715(18) 0.0453(7) Uani 1 1 d . . . H20A H 0.5448 0.3906 0.4773 0.068 Uiso 1 1 calc R . . H20B H 0.3968 0.4053 0.4091 0.068 Uiso 1 1 calc R . . H20C H 0.5124 0.3470 0.3877 0.068 Uiso 1 1 calc R . . C21 C -0.0490(3) 0.24950(11) 0.62021(17) 0.0446(6) Uani 1 1 d . . . H21A H -0.1031 0.2714 0.6711 0.067 Uiso 1 1 calc R . . H21B H 0.0312 0.2206 0.6463 0.067 Uiso 1 1 calc R . . H21C H -0.1273 0.2254 0.5834 0.067 Uiso 1 1 calc R . . C22 C -0.0928(3) 0.33794(10) 0.52019(16) 0.0353(5) Uani 1 1 d . . . H22A H -0.1679 0.3131 0.4823 0.053 Uiso 1 1 calc R . . H22B H -0.0420 0.3699 0.4809 0.053 Uiso 1 1 calc R . . H22C H -0.1502 0.3589 0.5707 0.053 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 Zn1 0.02043(12) 0.01972(13) 0.01428(10) -0.00143(10) -0.00200(8) 0.00037(10) Na1 0.0245(4) 0.0217(4) 0.0209(4) -0.0022(3) -0.0014(3) -0.0001(3) C1 0.0241(10) 0.0158(10) 0.0170(8) -0.0016(8) -0.0025(7) 0.0023(9) C2 0.0175(10) 0.0192(10) 0.0234(9) 0.0000(9) -0.0046(7) 0.0028(9) C3 0.0232(10) 0.0201(10) 0.0176(9) -0.0005(8) 0.0024(7) 0.0026(9) C4 0.0318(13) 0.0235(11) 0.0194(10) -0.0043(8) -0.0015(9) 0.0025(9) C5 0.0428(16) 0.0505(16) 0.0379(14) -0.0170(12) -0.0049(11) 0.0165(12) C6 0.089(2) 0.0245(13) 0.0378(15) -0.0054(10) 0.0117(14) -0.0053(13) C7 0.0453(15) 0.0340(13) 0.0268(12) -0.0122(10) -0.0062(10) 0.0081(11) N1 0.0147(9) 0.0221(9) 0.0187(8) 0.0025(7) -0.0038(6) -0.0005(7) C8 0.0184(11) 0.0302(12) 0.0263(11) -0.0001(9) -0.0040(9) 0.0015(9) C9 0.0261(12) 0.0314(12) 0.0292(12) -0.0018(10) -0.0127(9) -0.0014(10) C10 0.0481(15) 0.0312(13) 0.0219(11) 0.0014(9) -0.0161(10) 0.0011(11) C11 0.0430(14) 0.0264(12) 0.0203(11) 0.0038(9) 0.0013(10) -0.0024(10) C12 0.0255(12) 0.0226(11) 0.0199(10) 0.0029(8) -0.0021(8) -0.0027(9) C13 0.0226(11) 0.0517(15) 0.0356(12) 0.0093(12) -0.0030(9) -0.0144(11) C14 0.0220(13) 0.0558(17) 0.0454(15) -0.0110(12) -0.0029(10) 0.0093(11) C15 0.0263(12) 0.0318(13) 0.0327(12) 0.0066(10) 0.0030(9) -0.0064(10) C16 0.0402(14) 0.0232(12) 0.0296(12) 0.0022(9) -0.0071(10) -0.0032(10) N2 0.0278(10) 0.0223(9) 0.0301(10) 0.0025(8) 0.0064(8) 0.0020(8) C17 0.0403(14) 0.0450(15) 0.0282(12) -0.0104(11) 0.0008(10) 0.0059(11) C18 0.0359(14) 0.0277(13) 0.0505(15) -0.0139(11) -0.0078(11) -0.0010(10) N3 0.0263(10) 0.0230(9) 0.0312(10) 0.0011(8) -0.0048(8) -0.0041(8) C19 0.0335(13) 0.0323(13) 0.0421(13) 0.0004(11) 0.0043(10) 0.0074(10) C20 0.0422(15) 0.0403(15) 0.0541(16) 0.0104(12) 0.0231(12) 0.0047(12) C21 0.0466(15) 0.0364(14) 0.0506(16) 0.0109(12) -0.0065(12) -0.0188(12) C22 0.0317(14) 0.0319(13) 0.0421(14) 0.0009(10) -0.0057(10) 0.0000(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 Zn1 C1 2.0657(18) . ? Zn1 C4 2.0485(19) . ? Zn1 N1 2.0339(16) . ? Na1 C1 2.733(2) . ? Na1 C2 2.801(2) . ? Na1 N1 2.3859(17) . ? Na1 N2 2.4668(18) . ? Na1 N3 2.5173(18) . ? C1 C2 1.410(3) . ? C1 C3 1.401(3) . ? C2 C3 1.398(2) 3_566 ? C4 C5 1.532(3) . ? C4 C6 1.532(3) . ? C4 C7 1.520(3) . ? N1 C8 1.486(2) . ? N1 C12 1.486(2) . ? C8 C9 1.542(3) . ? C8 C13 1.531(3) . ? C8 C14 1.549(3) . ? C9 C10 1.521(3) . ? C10 C11 1.520(3) . ? C11 C12 1.537(3) . ? C12 C15 1.530(3) . ? C12 C16 1.554(3) . ? N2 C17 1.464(3) . ? N2 C19 1.465(3) . ? N2 C20 1.471(3) . ? C17 C18 1.513(3) . ? C18 N3 1.477(3) . ? N3 C21 1.472(3) . ? N3 C22 1.462(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 C1 Zn1 C4 118.42(8) . . ? C1 Zn1 N1 109.79(7) . . ? C4 Zn1 N1 131.79(7) . . ? C1 Na1 C2 29.49(5) . . ? C1 Na1 N1 81.57(6) . . ? C1 Na1 N2 125.59(6) . . ? C1 Na1 N3 111.59(6) . . ? C2 Na1 N1 99.46(6) . . ? C2 Na1 N2 96.70(6) . . ? C2 Na1 N3 113.44(6) . . ? N1 Na1 N2 134.50(6) . . ? N1 Na1 N3 133.31(6) . . ? N2 Na1 N3 75.04(6) . . ? Zn1 C1 Na1 79.43(6) . . ? Zn1 C1 C2 125.05(13) . . ? Zn1 C1 C3 121.70(13) . . ? Na1 C1 C2 77.94(11) . . ? Na1 C1 C3 119.26(13) . . ? C2 C1 C3 113.08(16) . . ? Na1 C2 C1 72.58(11) . . ? Na1 C2 C3 121.21(13) . 3_566 ? C1 C2 C3 123.39(17) . 3_566 ? C1 C3 C2 123.53(16) . 3_566 ? Zn1 C4 C5 108.02(14) . . ? Zn1 C4 C6 107.22(13) . . ? Zn1 C4 C7 117.15(14) . . ? C5 C4 C6 107.40(19) . . ? C5 C4 C7 108.22(17) . . ? C6 C4 C7 108.45(18) . . ? Zn1 N1 Na1 89.03(6) . . ? Zn1 N1 C8 113.02(12) . . ? Zn1 N1 C12 114.49(12) . . ? Na1 N1 C8 116.72(11) . . ? Na1 N1 C12 103.78(11) . . ? C8 N1 C12 116.45(15) . . ? N1 C8 C9 112.65(16) . . ? N1 C8 C13 107.34(15) . . ? N1 C8 C14 113.37(17) . . ? C9 C8 C13 107.95(17) . . ? C9 C8 C14 109.17(17) . . ? C13 C8 C14 106.00(18) . . ? C8 C9 C10 112.56(17) . . ? C9 C10 C11 109.17(17) . . ? C10 C11 C12 113.03(17) . . ? Na1 C12 N1 48.43(8) . . ? Na1 C12 C11 160.43(13) . . ? Na1 C12 C15 84.83(11) . . ? Na1 C12 C16 80.02(11) . . ? N1 C12 C11 112.46(16) . . ? N1 C12 C15 107.17(15) . . ? N1 C12 C16 113.06(16) . . ? C11 C12 C15 108.09(16) . . ? C11 C12 C16 108.97(16) . . ? C15 C12 C16 106.80(16) . . ? Na1 N2 C17 101.85(12) . . ? Na1 N2 C19 110.32(13) . . ? Na1 N2 C20 114.69(13) . . ? C17 N2 C19 111.31(17) . . ? C17 N2 C20 109.16(18) . . ? C19 N2 C20 109.33(17) . . ? N2 C17 C18 114.31(18) . . ? C17 C18 N3 114.19(17) . . ? Na1 N3 C18 106.74(12) . . ? Na1 N3 C21 125.55(13) . . ? Na1 N3 C22 94.82(12) . . ? C18 N3 C21 109.69(17) . . ? C18 N3 C22 110.12(17) . . ? C21 N3 C22 108.59(17) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.324 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.060 #===END data_dvgrem144reproc_compound_4 _database_code_depnum_ccdc_archive 'CCDC 621933' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H108 Mg2 N8 Na2' _chemical_formula_sum 'C54 H108 Mg2 N8 Na2' _chemical_formula_weight 964.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.3042(3) _cell_length_b 21.9621(8) _cell_length_c 16.3052(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.458(2) _cell_angle_gamma 90.00 _cell_volume 2972.74(19) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5697 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.51 _exptl_crystal_description 'cut needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.077 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61353 _diffrn_reflns_av_R_equivalents 0.1333 _diffrn_reflns_av_sigmaI/netI 0.1712 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5225 _reflns_number_gt 2367 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DENZO and COLLECT' _computing_cell_refinement DENZO _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution SHEXLS97 _computing_structure_refinement SHELXL97 _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL97 and local programs' _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^)+(0.0444P)^2^+1.6733P] 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 5225 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1944 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1471 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Na1 Na 0.13417(16) 0.37862(6) 0.40729(8) 0.0357(4) Uani 1 1 d . . . Mg1 Mg 0.02628(14) 0.48242(5) 0.27759(7) 0.0324(3) Uani 1 1 d . . . C1 C -0.1812(5) 0.56428(18) 0.1703(2) 0.0446(11) Uani 1 1 d . . . C2 C -0.2326(5) 0.63075(18) 0.1821(3) 0.0572(13) Uani 1 1 d . . . H2A H -0.3368 0.6375 0.1527 0.069 Uiso 1 1 calc R . . H2B H -0.2492 0.6382 0.2412 0.069 Uiso 1 1 calc R . . C3 C -0.1109(5) 0.67600(18) 0.1514(3) 0.0558(13) Uani 1 1 d . . . H3A H -0.1458 0.7179 0.1643 0.067 Uiso 1 1 calc R . . H3B H -0.1027 0.6724 0.0912 0.067 Uiso 1 1 calc R . . C4 C 0.0518(5) 0.66339(17) 0.1923(3) 0.0454(11) Uani 1 1 d . . . H4A H 0.0460 0.6726 0.2516 0.055 Uiso 1 1 calc R . . H4B H 0.1331 0.6908 0.1687 0.055 Uiso 1 1 calc R . . C5 C 0.1059(5) 0.59721(17) 0.1815(2) 0.0425(11) Uani 1 1 d . . . C6 C -0.2067(7) 0.5457(2) 0.0796(3) 0.0870(18) Uani 1 1 d . . . H6A H -0.1587 0.5765 0.0443 0.131 Uiso 1 1 calc R . . H6B H -0.3223 0.5425 0.0668 0.131 Uiso 1 1 calc R . . H6C H -0.1552 0.5062 0.0703 0.131 Uiso 1 1 calc R . . C7 C -0.2939(4) 0.52463(19) 0.2188(3) 0.0549(13) Uani 1 1 d . . . H7A H -0.2699 0.4816 0.2086 0.082 Uiso 1 1 calc R . . H7B H -0.4056 0.5333 0.2018 0.082 Uiso 1 1 calc R . . H7C H -0.2791 0.5333 0.2775 0.082 Uiso 1 1 calc R . . C8 C 0.1700(6) 0.5901(2) 0.0931(3) 0.0832(17) Uani 1 1 d . . . H8A H 0.1989 0.5475 0.0836 0.125 Uiso 1 1 calc R . . H8B H 0.2653 0.6159 0.0869 0.125 Uiso 1 1 calc R . . H8C H 0.0862 0.6025 0.0531 0.125 Uiso 1 1 calc R . . C9 C 0.2492(5) 0.5873(2) 0.2398(3) 0.0693(15) Uani 1 1 d . . . H9A H 0.2135 0.5892 0.2966 0.104 Uiso 1 1 calc R . . H9B H 0.3298 0.6191 0.2310 0.104 Uiso 1 1 calc R . . H9C H 0.2968 0.5473 0.2295 0.104 Uiso 1 1 calc R . . C10 C -0.0453(5) 0.34993(17) 0.2340(2) 0.0376(10) Uani 1 1 d . . . C11 C 0.0044(5) 0.28263(17) 0.2393(3) 0.0465(12) Uani 1 1 d . . . H11A H 0.0219 0.2713 0.2976 0.056 Uiso 1 1 calc R . . H11B H -0.0842 0.2571 0.2165 0.056 Uiso 1 1 calc R . . C12 C 0.1568(5) 0.26967(18) 0.1929(3) 0.0529(12) Uani 1 1 d . . . H12A H 0.1371 0.2768 0.1335 0.063 Uiso 1 1 calc R . . H12B H 0.1887 0.2266 0.2007 0.063 Uiso 1 1 calc R . . C13 C 0.2909(5) 0.31122(17) 0.2245(2) 0.0451(11) Uani 1 1 d . . . H13A H 0.3880 0.3045 0.1917 0.054 Uiso 1 1 calc R . . H13B H 0.3184 0.3004 0.2821 0.054 Uiso 1 1 calc R . . C14 C 0.2442(4) 0.37896(17) 0.2201(2) 0.0385(10) Uani 1 1 d . . . C15 C -0.1807(4) 0.35854(17) 0.2956(2) 0.0435(11) Uani 1 1 d . . . H15A H -0.1415 0.3468 0.3505 0.065 Uiso 1 1 calc R . . H15B H -0.2728 0.3329 0.2795 0.065 Uiso 1 1 calc R . . H15C H -0.2140 0.4013 0.2960 0.065 Uiso 1 1 calc R . . C16 C -0.1207(5) 0.36288(19) 0.1477(2) 0.0552(12) Uani 1 1 d . . . H16A H -0.1350 0.4069 0.1406 0.083 Uiso 1 1 calc R . . H16B H -0.2256 0.3426 0.1425 0.083 Uiso 1 1 calc R . . H16C H -0.0493 0.3473 0.1056 0.083 Uiso 1 1 calc R . . C17 C 0.3731(4) 0.41441(18) 0.2700(2) 0.0478(12) Uani 1 1 d . . . H17A H 0.3446 0.4577 0.2710 0.072 Uiso 1 1 calc R . . H17B H 0.4780 0.4094 0.2447 0.072 Uiso 1 1 calc R . . H17C H 0.3788 0.3987 0.3263 0.072 Uiso 1 1 calc R . . C18 C 0.2548(5) 0.4010(2) 0.1302(2) 0.0612(13) Uani 1 1 d . . . H18A H 0.1908 0.3741 0.0943 0.092 Uiso 1 1 calc R . . H18B H 0.3675 0.4003 0.1137 0.092 Uiso 1 1 calc R . . H18C H 0.2130 0.4427 0.1258 0.092 Uiso 1 1 calc R . . C19 C 0.1744(5) 0.28347(18) 0.5610(2) 0.0441(11) Uani 1 1 d . . . H19A H 0.2305 0.2470 0.5403 0.053 Uiso 1 1 calc R . . H19B H 0.1301 0.2729 0.6150 0.053 Uiso 1 1 calc R . . C20 C 0.2964(4) 0.33437(18) 0.5729(2) 0.0410(11) Uani 1 1 d . . . H20A H 0.2413 0.3701 0.5964 0.049 Uiso 1 1 calc R . . H20B H 0.3799 0.3209 0.6133 0.049 Uiso 1 1 calc R . . C21 C -0.0390(5) 0.24213(19) 0.4786(3) 0.0557(12) Uani 1 1 d . . . H21A H 0.0371 0.2161 0.4500 0.084 Uiso 1 1 calc R . . H21B H -0.1299 0.2521 0.4415 0.084 Uiso 1 1 calc R . . H21C H -0.0786 0.2206 0.5267 0.084 Uiso 1 1 calc R . . C22 C -0.0736(4) 0.33762(18) 0.5455(2) 0.0478(12) Uani 1 1 d . . . H22A H -0.1236 0.3151 0.5901 0.072 Uiso 1 1 calc R . . H22B H -0.1569 0.3507 0.5057 0.072 Uiso 1 1 calc R . . H22C H -0.0175 0.3734 0.5680 0.072 Uiso 1 1 calc R . . C23 C 0.4845(4) 0.40334(18) 0.5190(2) 0.0500(12) Uani 1 1 d . . . H23A H 0.4236 0.4369 0.5428 0.075 Uiso 1 1 calc R . . H23B H 0.5365 0.4175 0.4692 0.075 Uiso 1 1 calc R . . H23C H 0.5668 0.3893 0.5587 0.075 Uiso 1 1 calc R . . C24 C 0.4663(4) 0.30312(18) 0.4639(2) 0.0461(11) Uani 1 1 d . . . H24A H 0.5395 0.2862 0.5061 0.069 Uiso 1 1 calc R . . H24B H 0.5289 0.3180 0.4179 0.069 Uiso 1 1 calc R . . H24C H 0.3917 0.2714 0.4444 0.069 Uiso 1 1 calc R . . C25 C 0.0132(4) 0.49155(15) 0.4101(2) 0.0284(9) Uani 1 1 d . . . C26 C 0.1328(4) 0.51028(15) 0.5484(2) 0.0309(9) Uani 1 1 d . . . H26 H 0.2291 0.5175 0.5797 0.037 Uiso 1 1 calc R . . C27 C 0.1445(4) 0.50210(15) 0.4641(2) 0.0314(9) Uani 1 1 d . . . H27 H 0.2488 0.5038 0.4415 0.038 Uiso 1 1 calc R . . N1 N -0.0175(4) 0.55342(13) 0.20386(18) 0.0371(8) Uani 1 1 d . . . N2 N 0.0875(3) 0.39156(13) 0.25876(17) 0.0310(8) Uani 1 1 d . . . N3 N 0.0420(4) 0.29823(14) 0.50481(19) 0.0382(9) Uani 1 1 d . . . N4 N 0.3754(3) 0.35338(14) 0.49853(19) 0.0366(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0385(8) 0.0353(9) 0.0331(9) 0.0026(7) -0.0023(7) -0.0010(7) Mg1 0.0353(7) 0.0323(8) 0.0296(8) -0.0007(6) 0.0000(6) -0.0007(6) C1 0.059(3) 0.034(3) 0.040(3) 0.013(2) -0.010(2) -0.010(2) C2 0.054(3) 0.045(3) 0.071(3) 0.021(3) -0.019(2) 0.006(2) C3 0.068(3) 0.030(3) 0.069(3) 0.014(2) -0.016(3) -0.003(2) C4 0.053(3) 0.032(3) 0.051(3) 0.009(2) -0.007(2) -0.001(2) C5 0.054(3) 0.028(3) 0.047(3) 0.001(2) 0.012(2) 0.000(2) C6 0.142(5) 0.067(4) 0.050(3) 0.015(3) -0.027(3) -0.037(3) C7 0.045(3) 0.051(3) 0.068(3) 0.020(3) -0.011(2) 0.003(2) C8 0.121(4) 0.053(3) 0.077(4) -0.002(3) 0.050(3) -0.011(3) C9 0.046(3) 0.045(3) 0.118(4) 0.025(3) 0.005(3) -0.002(2) C10 0.046(3) 0.036(3) 0.030(2) -0.005(2) -0.008(2) 0.007(2) C11 0.053(3) 0.034(3) 0.052(3) -0.014(2) -0.008(2) 0.001(2) C12 0.070(3) 0.039(3) 0.049(3) -0.010(2) -0.012(3) 0.013(2) C13 0.054(3) 0.041(3) 0.041(3) 0.000(2) 0.006(2) 0.013(2) C14 0.043(2) 0.038(3) 0.035(3) 0.004(2) 0.007(2) 0.008(2) C15 0.037(2) 0.036(3) 0.057(3) -0.005(2) -0.008(2) -0.005(2) C16 0.062(3) 0.057(3) 0.045(3) -0.014(2) -0.016(2) 0.011(2) C17 0.037(2) 0.041(3) 0.067(3) 0.006(2) 0.013(2) 0.005(2) C18 0.081(3) 0.062(3) 0.042(3) 0.013(2) 0.023(2) 0.022(3) C19 0.047(3) 0.044(3) 0.041(3) 0.008(2) 0.006(2) 0.006(2) C20 0.042(2) 0.046(3) 0.035(3) 0.006(2) -0.002(2) 0.006(2) C21 0.065(3) 0.044(3) 0.059(3) 0.001(2) 0.004(2) -0.011(3) C22 0.041(2) 0.051(3) 0.051(3) 0.004(2) 0.005(2) 0.000(2) C23 0.043(3) 0.050(3) 0.056(3) -0.001(2) -0.011(2) -0.008(2) C24 0.039(3) 0.049(3) 0.050(3) -0.004(2) -0.002(2) 0.009(2) C25 0.035(2) 0.020(2) 0.030(2) 0.0003(18) 0.001(2) -0.0021(18) C26 0.035(2) 0.028(2) 0.029(2) -0.0030(19) -0.0036(19) -0.0017(19) C27 0.033(2) 0.028(2) 0.033(2) -0.0023(19) 0.0064(19) -0.0002(18) N1 0.042(2) 0.031(2) 0.039(2) 0.0048(16) 0.0039(17) 0.0003(17) N2 0.0322(18) 0.0312(19) 0.0294(18) -0.0019(15) 0.0009(15) 0.0014(15) N3 0.040(2) 0.032(2) 0.043(2) -0.0032(17) -0.0006(18) 0.0009(18) N4 0.0341(19) 0.035(2) 0.041(2) 0.0026(17) -0.0013(17) 0.0011(17) _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 Na1 C25 2.677(4) . ? Na1 C27 2.866(4) . ? Na1 N2 2.459(3) . ? Na1 N3 2.509(3) . ? Na1 N4 2.526(3) . ? Mg1 C25 2.176(4) . ? Mg1 N1 1.997(3) . ? Mg1 N2 2.084(3) . ? C1 C2 1.534(5) . ? C1 C6 1.544(5) . ? C1 C7 1.516(5) . ? C1 N1 1.471(5) . ? C2 H2A 0.990 . ? C2 H2B 0.990 . ? C2 C3 1.511(5) . ? C3 H3A 0.990 . ? C3 H3B 0.990 . ? C3 C4 1.516(5) . ? C4 H4A 0.990 . ? C4 H4B 0.990 . ? C4 C5 1.533(5) . ? C5 C8 1.558(5) . ? C5 C9 1.520(5) . ? C5 N1 1.458(4) . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 C11 1.536(5) . ? C10 C15 1.538(5) . ? C10 C16 1.552(5) . ? C10 N2 1.480(4) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C11 C12 1.518(5) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.520(5) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C13 C14 1.539(5) . ? C14 C17 1.540(5) . ? C14 C18 1.548(5) . ? C14 N2 1.486(4) . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 0.980 . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19 C20 1.518(5) . ? C19 N3 1.450(4) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 N4 1.454(4) . ? C21 H21A 0.980 . ? C21 H21B 0.980 . ? C21 H21C 0.980 . ? C21 N3 1.463(4) . ? C22 H22A 0.980 . ? C22 H22B 0.980 . ? C22 H22C 0.980 . ? C22 N3 1.464(4) . ? C23 H23A 0.980 . ? C23 H23B 0.980 . ? C23 H23C 0.980 . ? C23 N4 1.456(4) . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? C24 N4 1.459(4) . ? C25 C26 1.404(5) 3_566 ? C25 C27 1.403(5) . ? C26 C25 1.404(5) 3_566 ? C26 H26 0.950 . ? C26 C27 1.393(5) . ? C27 H27 0.950 . ? 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 C25 Na1 C27 29.06(10) . . ? C25 Na1 N2 81.96(10) . . ? C25 Na1 N3 121.37(11) . . ? C25 Na1 N4 119.04(12) . . ? C27 Na1 N2 102.21(11) . . ? C27 Na1 N3 117.93(11) . . ? C27 Na1 N4 90.03(11) . . ? N2 Na1 N3 131.49(11) . . ? N2 Na1 N4 135.08(11) . . ? N3 Na1 N4 73.88(10) . . ? C25 Mg1 N1 120.88(13) . . ? C25 Mg1 N2 104.66(13) . . ? N1 Mg1 N2 134.46(13) . . ? C2 C1 C6 109.9(3) . . ? C2 C1 C7 107.7(3) . . ? C2 C1 N1 111.4(3) . . ? C6 C1 C7 106.0(3) . . ? C6 C1 N1 114.6(4) . . ? C7 C1 N1 106.9(3) . . ? C1 C2 H2A 108.9 . . ? C1 C2 H2B 108.9 . . ? C1 C2 C3 113.2(4) . . ? H2A C2 H2B 107.8 . . ? H2A C2 C3 108.9 . . ? H2B C2 C3 108.9 . . ? C2 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? C2 C3 C4 109.3(3) . . ? H3A C3 H3B 108.3 . . ? H3A C3 C4 109.8 . . ? H3B C3 C4 109.8 . . ? C3 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? C3 C4 C5 112.5(3) . . ? H4A C4 H4B 107.8 . . ? H4A C4 C5 109.1 . . ? H4B C4 C5 109.1 . . ? C4 C5 C8 108.0(3) . . ? C4 C5 C9 106.9(3) . . ? C4 C5 N1 112.8(3) . . ? C8 C5 C9 106.5(4) . . ? C8 C5 N1 115.1(3) . . ? C9 C5 N1 107.1(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 106.4(3) . . ? C11 C10 C16 109.2(3) . . ? C11 C10 N2 112.4(3) . . ? C15 C10 C16 106.5(3) . . ? C15 C10 N2 107.3(3) . . ? C16 C10 N2 114.5(3) . . ? C10 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? C10 C11 C12 112.3(3) . . ? H11A C11 H11B 107.9 . . ? H11A C11 C12 109.2 . . ? H11B C11 C12 109.2 . . ? C11 C12 H12A 109.8 . . ? C11 C12 H12B 109.8 . . ? C11 C12 C13 109.4(3) . . ? H12A C12 H12B 108.3 . . ? H12A C12 C13 109.8 . . ? H12B C12 C13 109.8 . . ? C12 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? C12 C13 C14 112.5(3) . . ? H13A C13 H13B 107.8 . . ? H13A C13 C14 109.1 . . ? H13B C13 C14 109.1 . . ? C13 C14 C17 107.0(3) . . ? C13 C14 C18 109.1(3) . . ? C13 C14 N2 112.5(3) . . ? C17 C14 C18 106.6(3) . . ? C17 C14 N2 106.6(3) . . ? C18 C14 N2 114.5(3) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? H19A C19 H19B 107.6 . . ? H19A C19 C20 108.7 . . ? H19A C19 N3 108.7 . . ? H19B C19 C20 108.7 . . ? H19B C19 N3 108.7 . . ? C20 C19 N3 114.1(3) . . ? C19 C20 H20A 108.6 . . ? C19 C20 H20B 108.6 . . ? C19 C20 N4 114.8(3) . . ? H20A C20 H20B 107.6 . . ? H20A C20 N4 108.6 . . ? H20B C20 N4 108.6 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21A C21 N3 109.5 . . ? H21B C21 H21C 109.5 . . ? H21B C21 N3 109.5 . . ? H21C C21 N3 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22A C22 N3 109.5 . . ? H22B C22 H22C 109.5 . . ? H22B C22 N3 109.5 . . ? H22C C22 N3 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23A C23 N4 109.5 . . ? H23B C23 H23C 109.5 . . ? H23B C23 N4 109.5 . . ? H23C C23 N4 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24A C24 N4 109.5 . . ? H24B C24 H24C 109.5 . . ? H24B C24 N4 109.5 . . ? H24C C24 N4 109.5 . . ? Na1 C25 Mg1 82.49(11) . . ? Na1 C25 C26 108.1(2) . 3_566 ? Na1 C25 C27 83.0(2) . . ? Mg1 C25 C26 122.7(3) . 3_566 ? Mg1 C25 C27 125.5(3) . . ? C26 C25 C27 111.7(3) 3_566 . ? C25 C26 H26 118.2 3_566 . ? C25 C26 C27 123.7(3) 3_566 . ? H26 C26 C27 118.2 . . ? Na1 C27 C25 67.95(19) . . ? Na1 C27 C26 116.0(2) . . ? Na1 C27 H27 86.1 . . ? C25 C27 C26 124.6(3) . . ? C25 C27 H27 117.7 . . ? C26 C27 H27 117.7 . . ? Mg1 N1 C1 120.2(2) . . ? Mg1 N1 C5 123.2(2) . . ? C1 N1 C5 116.7(3) . . ? Na1 N2 Mg1 89.91(11) . . ? Na1 N2 C10 107.1(2) . . ? Na1 N2 C14 106.2(2) . . ? Mg1 N2 C10 116.7(2) . . ? Mg1 N2 C14 117.4(2) . . ? C10 N2 C14 115.0(3) . . ? Na1 N3 C19 108.6(2) . . ? Na1 N3 C21 123.6(2) . . ? Na1 N3 C22 94.9(2) . . ? C19 N3 C21 109.4(3) . . ? C19 N3 C22 109.9(3) . . ? C21 N3 C22 109.2(3) . . ? Na1 N4 C20 100.8(2) . . ? Na1 N4 C23 116.7(2) . . ? Na1 N4 C24 110.4(2) . . ? C20 N4 C23 108.4(3) . . ? C20 N4 C24 110.8(3) . . ? C23 N4 C24 109.5(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.349 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.050 #===END