# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'R.E. Mulvey' 'Prokopis C. Andrikopoulos' 'David R. Armstrong' 'Eva. Hevia' 'Alan R. Kennedy' "Charles T. O'Hara" _publ_contact_author_name 'Prof R. E. Mulvey' _publ_contact_author_address ; Department of Pure & Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL ; _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Stoichiometrically-controlled reactivity and supramolecular storage of butylmagnesiate anions ; data_grem142 _database_code_depnum_ccdc_archive 'CCDC 255283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H80 Mg N6 Na2' _chemical_formula_weight 727.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mg Mg 0.0486 0.0363 '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' 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.6369(11) _cell_length_b 20.2159(7) _cell_length_c 22.1129(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8778.3(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5897 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 22.02 _exptl_crystal_description blade _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Diffraction intensity dropped sharply at higher angles. Several crystals examined - all showed this feature. ; _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10172 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 21.99 _reflns_number_total 5355 _reflns_number_gt 3094 _reflns_threshold_expression I>2sigma(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 ; Both toluene and 3 of the 4 butyl groups were modeled as disordered. (Two sites, 50:50 occupancy). Some H atoms omitted from final model. 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^)+(0.0733P)^2^+13.7786P] 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 5355 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1385 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.1959 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Mg1 Mg 0.14477(10) 0.25188(10) 0.29250(9) 0.0668(6) Uani 1 1 d . . . Na1 Na 0.41873(9) 0.05156(8) 0.41323(8) 0.0458(5) Uani 1 1 d . . . Na2 Na 0.05376(9) -0.06866(8) 0.39225(8) 0.0463(5) Uani 1 1 d . . . N1 N 0.2950(2) 0.01581(19) 0.4117(2) 0.0504(11) Uani 1 1 d . D . N2 N 0.16921(19) -0.02473(18) 0.40697(19) 0.0465(11) Uani 1 1 d . . . N3 N 0.4255(2) 0.17704(18) 0.3965(2) 0.0520(12) Uani 1 1 d . D . N4 N 0.4286(2) 0.30559(19) 0.3888(2) 0.0539(12) Uani 1 1 d . . . N5 N 0.4680(2) 0.00983(18) 0.31496(18) 0.0457(11) Uani 1 1 d . D . N6 N 0.5263(2) -0.0264(2) 0.21417(19) 0.0537(12) Uani 1 1 d . . . C1 C 0.2052(3) 0.1764(3) 0.2677(3) 0.0771(19) Uani 1 1 d . A 1 H1A H 0.2530 0.1890 0.2760 0.093 Uiso 1 1 calc R A 1 H1B H 0.1943 0.1378 0.2935 0.093 Uiso 1 1 calc R A 1 C2 C 0.1999(3) 0.1555(2) 0.2028(3) 0.0662(17) Uani 1 1 d . A 1 H2A H 0.2079 0.1946 0.1768 0.079 Uiso 1 1 calc R A 1 H2B H 0.1529 0.1399 0.1950 0.079 Uiso 1 1 calc R A 1 C3 C 0.2498(4) 0.1007(3) 0.1842(3) 0.096(2) Uani 1 1 d . A 1 H3A H 0.2965 0.1148 0.1952 0.115 Uiso 1 1 calc R A 1 H3B H 0.2392 0.0604 0.2077 0.115 Uiso 1 1 calc R A 1 C4 C 0.2487(5) 0.0845(4) 0.1210(4) 0.131(3) Uani 1 1 d . A 1 H4A H 0.2822 0.0496 0.1129 0.196 Uiso 1 1 calc R A 1 H4B H 0.2599 0.1239 0.0972 0.196 Uiso 1 1 calc R A 1 H4C H 0.2032 0.0688 0.1099 0.196 Uiso 1 1 calc R A 1 C5 C 0.0427(19) 0.2341(14) 0.2863(13) 0.089(10) Uani 0.50 1 d P A 1 H5A H 0.0255 0.2612 0.2523 0.107 Uiso 0.50 1 calc PR A 1 H5B H 0.0375 0.1873 0.2741 0.107 Uiso 0.50 1 calc PR A 1 C6 C 0.0007(10) 0.2438(7) 0.3324(10) 0.058(5) Uani 0.50 1 d P A 1 H6A H -0.0037 0.2924 0.3365 0.070 Uiso 0.50 1 calc PR A 1 H6B H 0.0253 0.2284 0.3688 0.070 Uiso 0.50 1 calc PR A 1 C7 C -0.0703(18) 0.2167(16) 0.3377(10) 0.097(11) Uani 0.50 1 d P A 1 H7A H -0.0900 0.2118 0.2967 0.117 Uiso 0.50 1 calc PR A 1 H7B H -0.0683 0.1722 0.3563 0.117 Uiso 0.50 1 calc PR A 1 C8 C -0.109(3) 0.2534(19) 0.369(3) 0.169(19) Uani 0.50 1 d P A 1 H8A H -0.1549 0.2351 0.3695 0.254 Uiso 0.50 1 calc PR A 1 H8B H -0.1097 0.2980 0.3517 0.254 Uiso 0.50 1 calc PR A 1 H8C H -0.0914 0.2557 0.4107 0.254 Uiso 0.50 1 calc PR A 1 C9 C 0.1671(4) 0.2893(4) 0.3760(3) 0.104(2) Uani 1 1 d . A 1 H9A H 0.2098 0.3151 0.3728 0.125 Uiso 1 1 calc R A 1 H9B H 0.1304 0.3205 0.3875 0.125 Uiso 1 1 calc R A 1 C10 C 0.1746(4) 0.2435(4) 0.4223(4) 0.114(3) Uani 1 1 d . A 1 H10A H 0.2135 0.2145 0.4120 0.137 Uiso 1 1 calc R A 1 H10B H 0.1333 0.2154 0.4231 0.137 Uiso 1 1 calc R A 1 C11 C 0.1870(7) 0.2720(6) 0.4904(4) 0.143(4) Uani 1 1 d . A 1 H11A H 0.2288 0.2994 0.4896 0.171 Uiso 1 1 calc R A 1 H11B H 0.1486 0.3018 0.5002 0.171 Uiso 1 1 calc R A 1 C12 C 0.1935(8) 0.2270(6) 0.5373(6) 0.074(4) Uani 0.50 1 d P A 1 H12A H 0.2000 0.2508 0.5754 0.111 Uiso 0.50 1 calc PR A 1 H12B H 0.2328 0.1983 0.5298 0.111 Uiso 0.50 1 calc PR A 1 H12C H 0.1521 0.1999 0.5398 0.111 Uiso 0.50 1 calc PR A 1 C13 C 0.1604(3) 0.3244(3) 0.2319(3) 0.084(2) Uani 1 1 d . A 1 H13A H 0.1384 0.3115 0.1934 0.101 Uiso 1 1 calc R A 1 H13B H 0.1373 0.3649 0.2466 0.101 Uiso 1 1 calc R A 1 C14 C 0.2326(3) 0.3409(3) 0.2192(3) 0.084(2) Uani 1 1 d . A 1 H14A H 0.2551 0.3010 0.2026 0.101 Uiso 1 1 calc R A 1 H14B H 0.2552 0.3516 0.2580 0.101 Uiso 1 1 calc R A 1 C15 C 0.2446(6) 0.3983(4) 0.1754(5) 0.133(3) Uani 1 1 d . A 1 H15A H 0.2133 0.4348 0.1863 0.159 Uiso 1 1 calc R A 1 H15B H 0.2917 0.4146 0.1810 0.159 Uiso 1 1 calc R A 1 C16 C 0.2353(9) 0.3833(8) 0.1147(7) 0.108(5) Uani 0.50 1 d P A 1 H16A H 0.2426 0.4231 0.0903 0.162 Uiso 0.50 1 calc PR A 1 H16B H 0.1888 0.3670 0.1084 0.162 Uiso 0.50 1 calc PR A 1 H16C H 0.2680 0.3491 0.1026 0.162 Uiso 0.50 1 calc PR A 1 C5A C 0.0537(15) 0.2106(14) 0.3028(12) 0.095(9) Uani 0.50 1 d P A 2 H5A1 H 0.0263 0.2320 0.2708 0.114 Uiso 0.50 1 calc PR A 2 H5A2 H 0.0611 0.1648 0.2885 0.114 Uiso 0.50 1 calc PR A 2 C6A C 0.0105(14) 0.2031(13) 0.3459(10) 0.112(8) Uani 0.50 1 d P A 2 H6A1 H 0.0204 0.2407 0.3733 0.134 Uiso 0.50 1 calc PR A 2 H6A2 H 0.0272 0.1634 0.3674 0.134 Uiso 0.50 1 calc PR A 2 C7A C -0.0662(19) 0.196(2) 0.350(2) 0.19(2) Uani 0.50 1 d P A 2 H7A1 H -0.0812 0.2027 0.3072 0.233 Uiso 0.50 1 calc PR A 2 H7A2 H -0.0732 0.1488 0.3581 0.233 Uiso 0.50 1 calc PR A 2 C8A C -0.116(2) 0.2270(18) 0.3828(13) 0.133(14) Uani 0.50 1 d P A 2 H8A1 H -0.1611 0.2127 0.3681 0.200 Uiso 0.50 1 calc PR A 2 H8A2 H -0.1122 0.2751 0.3785 0.200 Uiso 0.50 1 calc PR A 2 H8A3 H -0.1115 0.2149 0.4255 0.200 Uiso 0.50 1 calc PR A 2 C12A C 0.1442(16) 0.2692(16) 0.5198(18) 0.225(17) Uani 0.50 1 d P B 2 C16A C 0.3021(12) 0.4063(11) 0.1451(14) 0.180(10) Uani 0.50 1 d P C 2 C17 C 0.2800(3) -0.0195(3) 0.3544(3) 0.0650(16) Uani 1 1 d . . . H17A H 0.3136 -0.0554 0.3486 0.078 Uiso 1 1 calc R D . H17B H 0.2842 0.0116 0.3201 0.078 Uiso 1 1 calc R . . C18 C 0.2079(3) -0.0488(3) 0.3552(3) 0.0670(17) Uani 1 1 d . . . H18A H 0.1840 -0.0367 0.3174 0.080 Uiso 1 1 calc R . . H18B H 0.2109 -0.0977 0.3570 0.080 Uiso 1 1 calc R . . C19 C 0.2792(3) -0.0302(3) 0.4616(3) 0.0603(16) Uani 1 1 d . . . H19A H 0.2916 -0.0094 0.5006 0.072 Uiso 1 1 calc R D . H19B H 0.3067 -0.0710 0.4569 0.072 Uiso 1 1 calc R . . C20 C 0.2033(3) -0.0483(3) 0.4622(3) 0.0653(17) Uani 1 1 d . . . H20A H 0.1983 -0.0969 0.4654 0.078 Uiso 1 1 calc R . . H20B H 0.1813 -0.0281 0.4981 0.078 Uiso 1 1 calc R . . C21 C 0.2471(3) 0.0719(2) 0.4157(3) 0.0571(15) Uani 1 1 d . . . H21A H 0.2582 0.1048 0.3842 0.069 Uiso 1 1 calc R D . H21B H 0.2519 0.0935 0.4557 0.069 Uiso 1 1 calc R . . C22 C 0.1725(2) 0.0477(2) 0.4074(2) 0.0527(14) Uani 1 1 d . . . H22A H 0.1439 0.0650 0.4407 0.063 Uiso 1 1 calc R . . H22B H 0.1541 0.0651 0.3688 0.063 Uiso 1 1 calc R . . C23 C 0.4961(3) 0.2018(2) 0.3937(3) 0.0637(16) Uani 1 1 d . . . H23A H 0.5197 0.1816 0.3588 0.076 Uiso 1 1 calc R D . H23B H 0.5207 0.1889 0.4309 0.076 Uiso 1 1 calc R . . C24 C 0.4972(3) 0.2775(2) 0.3873(3) 0.0709(18) Uani 1 1 d . D . H24A H 0.5245 0.2967 0.4206 0.085 Uiso 1 1 calc R . . H24B H 0.5193 0.2895 0.3486 0.085 Uiso 1 1 calc R . . C25 C 0.3906(3) 0.2001(3) 0.3421(3) 0.0707(18) Uani 1 1 d . . . H25A H 0.3432 0.1835 0.3422 0.085 Uiso 1 1 calc R D . H25B H 0.4138 0.1820 0.3060 0.085 Uiso 1 1 calc R . . C26 C 0.3900(3) 0.2765(3) 0.3385(3) 0.0751(19) Uani 1 1 d . D . H26A H 0.4103 0.2907 0.2996 0.090 Uiso 1 1 calc R . . H26B H 0.3424 0.2925 0.3398 0.090 Uiso 1 1 calc R . . C27 C 0.3931(3) 0.2077(3) 0.4491(3) 0.0709(17) Uani 1 1 d . . . H27A H 0.4165 0.1931 0.4864 0.085 Uiso 1 1 calc R D . H27B H 0.3450 0.1933 0.4515 0.085 Uiso 1 1 calc R . . C28 C 0.3960(3) 0.2840(2) 0.4448(3) 0.0768(19) Uani 1 1 d . D . H28A H 0.3492 0.3021 0.4466 0.092 Uiso 1 1 calc R . . H28B H 0.4217 0.3017 0.4798 0.092 Uiso 1 1 calc R . . C29 C 0.4783(3) -0.0623(2) 0.3134(2) 0.0531(14) Uani 1 1 d . . . H29A H 0.4338 -0.0849 0.3179 0.064 Uiso 1 1 calc R D . H29B H 0.5076 -0.0758 0.3476 0.064 Uiso 1 1 calc R . . C30 C 0.5118(3) -0.0837(2) 0.2532(2) 0.0603(15) Uani 1 1 d . D . H30A H 0.5548 -0.1075 0.2619 0.072 Uiso 1 1 calc R . . H30B H 0.4810 -0.1145 0.2316 0.072 Uiso 1 1 calc R . . C31 C 0.4269(3) 0.0277(3) 0.2617(3) 0.0733(18) Uani 1 1 d . . . H31A H 0.4187 0.0760 0.2617 0.088 Uiso 1 1 calc R D . H31B H 0.3822 0.0052 0.2641 0.088 Uiso 1 1 calc R . . C32 C 0.4621(3) 0.0083(3) 0.2033(2) 0.0688(17) Uani 1 1 d . D . H32A H 0.4315 -0.0206 0.1795 0.083 Uiso 1 1 calc R . . H32B H 0.4712 0.0485 0.1791 0.083 Uiso 1 1 calc R . . C33 C 0.5353(3) 0.0410(3) 0.3074(3) 0.0647(17) Uani 1 1 d . . . H33A H 0.5645 0.0294 0.3423 0.078 Uiso 1 1 calc R D . H33B H 0.5299 0.0897 0.3069 0.078 Uiso 1 1 calc R . . C34 C 0.5704(3) 0.0188(3) 0.2488(3) 0.0665(17) Uani 1 1 d . D . H34A H 0.5812 0.0581 0.2238 0.080 Uiso 1 1 calc R . . H34B H 0.6137 -0.0037 0.2588 0.080 Uiso 1 1 calc R . . C35 C -0.0221(7) 0.0373(6) 0.4740(5) 0.100(10) Uani 0.50 1 d PG . -1 H35 H -0.0229 0.0826 0.4627 0.120 Uiso 0.50 1 calc PR . -1 C36 C 0.0229(6) 0.0156(5) 0.5183(5) 0.059(3) Uani 0.50 1 d PG . -1 C37 C 0.0241(4) -0.0507(6) 0.5349(4) 0.045(4) Uani 0.50 1 d PG . -1 H37 H 0.0549 -0.0654 0.5652 0.054 Uiso 0.50 1 calc PR . -1 C38 C -0.0197(5) -0.0954(5) 0.5072(5) 0.071(4) Uani 0.50 1 d PG . -1 H38 H -0.0189 -0.1407 0.5185 0.086 Uiso 0.50 1 calc PR . -1 C39 C -0.0647(5) -0.0737(8) 0.4629(5) 0.093(12) Uani 0.50 1 d PG . -1 H39 H -0.0946 -0.1043 0.4439 0.112 Uiso 0.50 1 calc PR . -1 C40 C -0.0659(6) -0.0074(9) 0.4463(4) 0.133(10) Uani 0.50 1 d PG . -1 H40 H -0.0967 0.0073 0.4160 0.159 Uiso 0.50 1 calc PR . -1 C41 C 0.0645(13) 0.0626(11) 0.5497(11) 0.108(11) Uani 0.50 1 d P . -1 H41A H 0.0938 0.0394 0.5786 0.162 Uiso 0.50 1 calc PR . -1 H41B H 0.0354 0.0940 0.5714 0.162 Uiso 0.50 1 calc PR . -1 H41C H 0.0928 0.0866 0.5205 0.162 Uiso 0.50 1 calc PR . -1 C42 C 0.4455(4) 0.0320(5) 0.5351(3) 0.094(2) Uani 1 1 d . D -1 C43 C 0.5066(5) 0.0704(5) 0.5175(3) 0.110(3) Uani 1 1 d . D -1 C44 C 0.4463(4) -0.0389(4) 0.5172(3) 0.080(2) Uani 1 1 d . . -1 C45 C 0.4012(9) 0.0630(8) 0.5586(7) 0.109(6) Uani 0.50 1 d P D -1 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 Mg1 0.0643(13) 0.0833(13) 0.0528(12) -0.0181(10) 0.0069(10) -0.0216(10) Na1 0.0488(12) 0.0451(11) 0.0436(12) 0.0012(9) -0.0018(9) -0.0075(9) Na2 0.0423(11) 0.0422(11) 0.0544(13) 0.0029(9) -0.0012(10) -0.0008(8) N1 0.042(3) 0.050(3) 0.059(3) 0.007(2) -0.004(2) -0.003(2) N2 0.039(2) 0.040(3) 0.060(3) 0.000(2) -0.005(2) -0.0016(19) N3 0.058(3) 0.036(2) 0.062(3) -0.002(2) 0.004(3) -0.006(2) N4 0.049(3) 0.039(2) 0.074(3) 0.004(2) 0.006(3) -0.003(2) N5 0.054(3) 0.042(3) 0.041(3) 0.001(2) 0.007(2) 0.001(2) N6 0.055(3) 0.055(3) 0.051(3) -0.002(2) 0.010(2) -0.001(2) C1 0.092(5) 0.076(4) 0.063(5) 0.017(3) -0.011(4) -0.016(3) C2 0.078(4) 0.042(3) 0.079(5) 0.002(3) 0.007(4) 0.002(3) C3 0.134(6) 0.065(4) 0.088(6) 0.012(4) 0.004(5) -0.002(4) C4 0.196(9) 0.096(6) 0.100(7) -0.007(5) 0.021(6) 0.025(6) C5 0.069(13) 0.109(14) 0.09(2) 0.055(12) -0.018(14) -0.011(9) C6 0.047(9) 0.053(9) 0.074(12) -0.005(9) -0.004(8) -0.001(8) C7 0.09(2) 0.14(2) 0.063(11) -0.073(13) 0.027(12) -0.056(16) C8 0.10(2) 0.10(2) 0.31(5) 0.01(2) 0.00(2) 0.009(17) C9 0.101(6) 0.110(6) 0.101(6) 0.014(5) -0.014(5) -0.029(5) C10 0.116(6) 0.108(6) 0.119(7) 0.021(5) -0.049(5) -0.023(5) C11 0.177(11) 0.165(9) 0.086(7) 0.011(7) -0.007(7) -0.089(8) C12 0.103(11) 0.064(8) 0.055(9) 0.005(7) 0.002(8) 0.003(7) C13 0.075(5) 0.073(4) 0.105(6) -0.020(4) 0.017(4) 0.012(3) C14 0.103(6) 0.063(4) 0.086(5) -0.010(4) 0.017(4) -0.009(4) C15 0.173(10) 0.063(5) 0.163(10) -0.002(6) 0.053(8) -0.011(5) C16 0.125(14) 0.139(14) 0.060(11) 0.032(10) -0.028(10) -0.013(11) C5A 0.089(19) 0.15(2) 0.042(13) -0.058(16) 0.025(13) -0.039(17) C6A 0.111(19) 0.15(2) 0.070(15) -0.014(15) -0.010(14) -0.071(18) C7A 0.07(2) 0.20(3) 0.31(4) 0.06(3) 0.08(2) 0.026(18) C8A 0.11(2) 0.18(4) 0.108(18) -0.09(2) -0.007(18) -0.01(2) C12A 0.20(3) 0.17(3) 0.30(4) -0.03(2) 0.15(3) -0.04(2) C16A 0.15(2) 0.155(18) 0.23(3) -0.006(18) 0.08(2) -0.019(15) C17 0.053(4) 0.069(4) 0.073(5) 0.000(3) 0.009(3) 0.010(3) C18 0.046(4) 0.076(4) 0.079(5) -0.022(3) -0.001(3) 0.004(3) C19 0.053(4) 0.058(3) 0.070(4) 0.020(3) -0.016(3) -0.015(3) C20 0.054(4) 0.060(4) 0.081(5) 0.024(3) -0.013(3) -0.014(3) C21 0.054(4) 0.049(3) 0.069(4) 0.007(3) 0.001(3) -0.005(3) C22 0.045(3) 0.050(3) 0.063(4) 0.005(3) 0.002(3) 0.002(2) C23 0.064(4) 0.042(3) 0.086(5) -0.005(3) 0.003(3) -0.001(3) C24 0.053(4) 0.043(3) 0.117(6) -0.004(3) 0.005(4) -0.003(3) C25 0.081(4) 0.053(4) 0.079(5) 0.003(3) -0.012(4) -0.012(3) C26 0.073(4) 0.052(4) 0.100(5) 0.004(3) -0.017(4) -0.003(3) C27 0.082(4) 0.056(4) 0.074(5) 0.005(3) 0.021(4) 0.004(3) C28 0.097(5) 0.046(4) 0.087(5) -0.008(3) 0.021(4) -0.004(3) C29 0.058(4) 0.050(4) 0.051(4) 0.003(3) 0.001(3) -0.011(3) C30 0.066(4) 0.053(3) 0.062(4) -0.006(3) 0.010(3) -0.004(3) C31 0.079(4) 0.088(4) 0.052(4) 0.010(3) 0.010(4) 0.025(3) C32 0.079(4) 0.079(4) 0.049(4) 0.002(3) 0.007(3) 0.014(3) C33 0.082(4) 0.050(3) 0.063(4) -0.013(3) 0.023(3) -0.021(3) C34 0.068(4) 0.060(4) 0.071(4) -0.011(3) 0.019(3) -0.014(3) C35 0.12(2) 0.095(18) 0.090(16) 0.068(15) 0.041(15) 0.055(16) C36 0.073(11) 0.066(10) 0.039(9) -0.002(7) 0.022(7) 0.000(8) C37 0.067(11) 0.051(9) 0.017(7) -0.006(7) 0.023(7) 0.003(8) C38 0.081(10) 0.067(9) 0.066(10) -0.010(8) 0.039(8) -0.011(8) C39 0.044(13) 0.18(3) 0.053(13) -0.062(15) 0.027(10) -0.030(14) C40 0.091(15) 0.22(3) 0.088(15) -0.031(19) 0.024(11) 0.085(18) C41 0.14(3) 0.078(14) 0.104(16) -0.018(14) 0.090(17) 0.005(15) C42 0.089(6) 0.126(8) 0.067(5) 0.026(5) -0.043(5) -0.014(5) C43 0.090(6) 0.190(9) 0.050(5) 0.037(5) -0.023(4) -0.019(7) C44 0.090(5) 0.087(5) 0.062(5) 0.027(4) -0.033(4) -0.024(4) C45 0.114(13) 0.116(12) 0.097(12) -0.026(10) -0.071(11) 0.072(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 Mg1 C5A 1.99(3) . ? Mg1 C1 2.009(6) . ? Mg1 C13 2.010(7) . ? Mg1 C5 2.04(4) . ? Mg1 C9 2.042(7) . ? Na1 N5 2.524(4) . ? Na1 N1 2.535(4) . ? Na1 N3 2.567(4) . ? Na1 C42 2.773(7) . ? Na1 C43 2.905(7) . ? Na1 C44 2.987(6) . ? Na1 C44 3.075(6) 5_656 ? Na2 N2 2.456(4) . ? Na2 N6 2.561(4) 6_556 ? Na2 N4 2.567(4) 7_655 ? Na2 C41 2.66(2) 5_556 ? Na2 C36 2.706(8) 5_556 ? Na2 C39 2.803(11) . ? Na2 C40 2.912(11) . ? Na2 C38 2.971(10) . ? Na2 C35 3.088(12) 5_556 ? N1 C21 1.475(6) . ? N1 C19 1.476(6) . ? N1 C17 1.482(6) . ? N2 C18 1.458(6) . ? N2 C22 1.466(6) . ? N2 C20 1.473(6) . ? N3 C25 1.460(7) . ? N3 C27 1.464(6) . ? N3 C23 1.475(6) . ? N4 C28 1.461(7) . ? N4 C24 1.461(6) . ? N4 C26 1.470(7) . ? N4 Na2 2.567(4) 7_665 ? N5 C31 1.473(7) . ? N5 C29 1.473(6) . ? N5 C33 1.474(6) . ? N6 C32 1.463(6) . ? N6 C30 1.471(6) . ? N6 C34 1.475(6) . ? N6 Na2 2.561(4) 6_656 ? C1 C2 1.500(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.535(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.435(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.33(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.50(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.27(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.388(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.629(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.386(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.483(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.529(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.388(15) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C5A C6A 1.28(3) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A C7A 1.51(4) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A C8A 1.38(5) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C17 C18 1.534(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.535(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.556(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.536(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.546(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.546(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.547(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.517(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.534(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C35 Na2 3.088(12) 5_556 ? C35 H35 0.9500 . ? C36 C37 1.3900 . ? C36 C41 1.43(2) . ? C36 Na2 2.706(11) 5_556 ? C37 C38 1.3900 . ? C37 H37 0.9500 . ? C38 C39 1.3900 . ? C38 H38 0.9500 . ? C39 C40 1.3900 . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 Na2 2.66(2) 5_556 ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C45 1.192(15) . ? C42 C43 1.480(10) . ? C42 C44 1.488(11) . ? C44 Na1 3.075(6) 5_656 ? 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 C5A Mg1 C1 104.1(7) . . ? C5A Mg1 C13 121.4(9) . . ? C1 Mg1 C13 106.4(2) . . ? C5A Mg1 C5 18.1(11) . . ? C1 Mg1 C5 115.3(9) . . ? C13 Mg1 C5 103.5(6) . . ? C5A Mg1 C9 104.1(7) . . ? C1 Mg1 C9 113.7(3) . . ? C13 Mg1 C9 107.5(3) . . ? C5 Mg1 C9 109.6(10) . . ? N5 Na1 N1 105.10(15) . . ? N5 Na1 N3 100.74(14) . . ? N1 Na1 N3 109.23(14) . . ? N5 Na1 C42 135.7(2) . . ? N1 Na1 C42 98.9(2) . . ? N3 Na1 C42 105.7(2) . . ? N5 Na1 C43 120.0(2) . . ? N1 Na1 C43 128.1(2) . . ? N3 Na1 C43 87.4(2) . . ? C42 Na1 C43 30.1(2) . . ? N5 Na1 C44 112.8(2) . . ? N1 Na1 C44 90.57(17) . . ? N3 Na1 C44 134.97(19) . . ? C42 Na1 C44 29.7(2) . . ? C43 Na1 C44 50.3(2) . . ? N5 Na1 C44 94.2(2) . 5_656 ? N1 Na1 C44 144.00(17) . 5_656 ? N3 Na1 C44 96.31(17) . 5_656 ? C42 Na1 C44 48.6(2) . 5_656 ? C43 Na1 C44 26.09(19) . 5_656 ? C44 Na1 C44 53.7(2) . 5_656 ? N2 Na2 N6 101.26(15) . 6_556 ? N2 Na2 N4 103.74(14) . 7_655 ? N6 Na2 N4 109.36(16) 6_556 7_655 ? N2 Na2 C41 136.6(5) . 5_556 ? N6 Na2 C41 104.2(6) 6_556 5_556 ? N4 Na2 C41 100.2(5) 7_655 5_556 ? N2 Na2 C36 105.9(3) . 5_556 ? N6 Na2 C36 115.0(2) 6_556 5_556 ? N4 Na2 C36 119.3(3) 7_655 5_556 ? C41 Na2 C36 30.9(4) 5_556 5_556 ? N2 Na2 C39 134.9(2) . . ? N6 Na2 C39 110.5(3) 6_556 . ? N4 Na2 C39 95.3(4) 7_655 . ? C41 Na2 C39 6.8(7) 5_556 . ? C36 Na2 C39 31.4(5) 5_556 . ? N2 Na2 C40 122.5(4) . . ? N6 Na2 C40 93.8(2) 6_556 . ? N4 Na2 C40 122.8(4) 7_655 . ? C41 Na2 C40 22.6(7) 5_556 . ? C36 Na2 C40 23.5(4) 5_556 . ? C39 Na2 C40 28.07(10) . . ? N2 Na2 C38 113.6(3) . . ? N6 Na2 C38 138.1(3) 6_556 . ? N4 Na2 C38 84.9(2) 7_655 . ? C41 Na2 C38 34.0(7) 5_556 . ? C36 Na2 C38 34.6(4) 5_556 . ? C39 Na2 C38 27.66(10) . . ? C40 Na2 C38 48.29(14) . . ? N2 Na2 C35 89.1(3) . 5_556 ? N6 Na2 C35 140.3(2) 6_556 5_556 ? N4 Na2 C35 105.0(2) 7_655 5_556 ? C41 Na2 C35 49.6(5) 5_556 5_556 ? C36 Na2 C35 26.73(15) 5_556 5_556 ? C39 Na2 C35 46.1(4) . 5_556 ? C40 Na2 C35 50.0(4) . 5_556 ? C38 Na2 C35 28.4(4) . 5_556 ? C21 N1 C19 107.7(4) . . ? C21 N1 C17 107.2(4) . . ? C19 N1 C17 107.0(4) . . ? C21 N1 Na1 113.0(3) . . ? C19 N1 Na1 111.8(3) . . ? C17 N1 Na1 109.9(3) . . ? C18 N2 C22 108.4(4) . . ? C18 N2 C20 107.9(4) . . ? C22 N2 C20 107.3(4) . . ? C18 N2 Na2 104.9(3) . . ? C22 N2 Na2 113.7(3) . . ? C20 N2 Na2 114.4(3) . . ? C25 N3 C27 108.4(4) . . ? C25 N3 C23 107.3(4) . . ? C27 N3 C23 107.3(4) . . ? C25 N3 Na1 114.2(3) . . ? C27 N3 Na1 106.4(3) . . ? C23 N3 Na1 113.0(3) . . ? C28 N4 C24 107.9(5) . . ? C28 N4 C26 107.2(4) . . ? C24 N4 C26 107.6(4) . . ? C28 N4 Na2 109.2(3) . 7_665 ? C24 N4 Na2 105.2(3) . 7_665 ? C26 N4 Na2 119.2(3) . 7_665 ? C31 N5 C29 107.4(4) . . ? C31 N5 C33 107.2(4) . . ? C29 N5 C33 107.4(4) . . ? C31 N5 Na1 113.4(3) . . ? C29 N5 Na1 113.8(3) . . ? C33 N5 Na1 107.4(3) . . ? C32 N6 C30 107.8(4) . . ? C32 N6 C34 107.1(4) . . ? C30 N6 C34 107.3(4) . . ? C32 N6 Na2 100.9(3) . 6_656 ? C30 N6 Na2 108.5(3) . 6_656 ? C34 N6 Na2 124.1(3) . 6_656 ? C2 C1 Mg1 115.8(4) . . ? C2 C1 H1A 108.3 . . ? Mg1 C1 H1A 108.3 . . ? C2 C1 H1B 108.3 . . ? Mg1 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? C1 C2 C3 114.5(5) . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? C3 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 114.5(6) . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? C2 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 Mg1 122(2) . . ? C6 C5 H5A 106.8 . . ? Mg1 C5 H5A 106.8 . . ? C6 C5 H5B 106.8 . . ? Mg1 C5 H5B 106.8 . . ? H5A C5 H5B 106.6 . . ? C5 C6 C7 126(2) . . ? C5 C6 H6A 105.9 . . ? C7 C6 H6A 105.9 . . ? C5 C6 H6B 105.9 . . ? C7 C6 H6B 105.9 . . ? H6A C6 H6B 106.2 . . ? C8 C7 C6 112(3) . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 Mg1 116.3(6) . . ? C10 C9 H9A 108.2 . . ? Mg1 C9 H9A 108.2 . . ? C10 C9 H9B 108.2 . . ? Mg1 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 117.5(7) . . ? C9 C10 H10A 107.9 . . ? C11 C10 H10A 107.9 . . ? C9 C10 H10B 107.9 . . ? C11 C10 H10B 107.9 . . ? H10A C10 H10B 107.2 . . ? C12 C11 C10 118.3(10) . . ? C12 C11 H11A 107.7 . . ? C10 C11 H11A 107.7 . . ? C12 C11 H11B 107.7 . . ? C10 C11 H11B 107.7 . . ? H11A C11 H11B 107.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 Mg1 115.9(5) . . ? C14 C13 H13A 108.3 . . ? Mg1 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? Mg1 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C13 C14 C15 115.9(7) . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? C13 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C16 C15 C14 115.3(9) . . ? C16 C15 H15A 108.5 . . ? C14 C15 H15A 108.5 . . ? C16 C15 H15B 108.5 . . ? C14 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C6A C5A Mg1 136.8(16) . . ? C6A C5A H5A1 102.9 . . ? Mg1 C5A H5A1 102.9 . . ? C6A C5A H5A2 102.9 . . ? Mg1 C5A H5A2 102.9 . . ? H5A1 C5A H5A2 105.1 . . ? C5A C6A C7A 135(3) . . ? C5A C6A H6A1 103.4 . . ? C7A C6A H6A1 103.4 . . ? C5A C6A H6A2 103.4 . . ? C7A C6A H6A2 103.4 . . ? H6A1 C6A H6A2 105.2 . . ? C8A C7A C6A 134(3) . . ? C8A C7A H7A1 103.6 . . ? C6A C7A H7A1 103.6 . . ? C8A C7A H7A2 103.6 . . ? C6A C7A H7A2 103.6 . . ? H7A1 C7A H7A2 105.3 . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? N1 C17 C18 111.1(4) . . ? N1 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? N1 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N2 C18 C17 111.1(4) . . ? N2 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? N2 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? N1 C19 C20 111.2(4) . . ? N1 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? N1 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? N2 C20 C19 110.9(4) . . ? N2 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.0 . . ? N1 C21 C22 110.6(4) . . ? N1 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? N2 C22 C21 110.8(4) . . ? N2 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? N3 C23 C24 110.8(4) . . ? N3 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? N3 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? N4 C24 C23 111.8(4) . . ? N4 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? N4 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N3 C25 C26 111.5(5) . . ? N3 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? N3 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? N4 C26 C25 110.8(5) . . ? N4 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? N4 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? N3 C27 C28 111.0(4) . . ? N3 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? N3 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? N4 C28 C27 111.5(4) . . ? N4 C28 H28A 109.3 . . ? C27 C28 H28A 109.3 . . ? N4 C28 H28B 109.3 . . ? C27 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? N5 C29 C30 110.8(4) . . ? N5 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? N5 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? N6 C30 C29 111.6(4) . . ? N6 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? N6 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? N5 C31 C32 111.6(4) . . ? N5 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? N5 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? N6 C32 C31 112.1(5) . . ? N6 C32 H32A 109.2 . . ? C31 C32 H32A 109.2 . . ? N6 C32 H32B 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? N5 C33 C34 112.0(4) . . ? N5 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? N5 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? N6 C34 C33 110.9(4) . . ? N6 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? N6 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C36 C35 C40 120.0 . . ? C36 C35 Na2 61.1(4) . 5_556 ? C40 C35 Na2 115.6(4) . 5_556 ? C36 C35 H35 120.0 . . ? C40 C35 H35 120.0 . . ? Na2 C35 H35 92.9 5_556 . ? C35 C36 C37 120.0 . . ? C35 C36 C41 119.7(14) . . ? C37 C36 C41 120.1(14) . . ? C35 C36 Na2 92.1(4) . 5_556 ? C37 C36 Na2 101.5(4) . 5_556 ? C41 C36 Na2 72.6(11) . 5_556 ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 Na2 87.6(4) . . ? C39 C38 Na2 69.4(3) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? Na2 C38 H38 113.1 . . ? C40 C39 C38 120.0 . . ? C40 C39 Na2 80.3(4) . . ? C38 C39 Na2 82.9(3) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? Na2 C39 H39 106.9 . . ? C39 C40 C35 120.0 . . ? C39 C40 Na2 71.6(4) . . ? C35 C40 Na2 87.6(4) . . ? C39 C40 H40 120.0 . . ? C35 C40 H40 120.0 . . ? Na2 C40 H40 110.9 . . ? C36 C41 Na2 76.4(12) . 5_556 ? C36 C41 H41A 109.5 . . ? Na2 C41 H41A 102.7 5_556 . ? C36 C41 H41B 109.5 . . ? Na2 C41 H41B 39.0 5_556 . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? Na2 C41 H41C 142.3 5_556 . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C45 C42 C43 115.6(13) . . ? C45 C42 C44 129.0(12) . . ? C43 C42 C44 115.3(8) . . ? C45 C42 Na1 102.2(8) . . ? C43 C42 Na1 79.9(4) . . ? C44 C42 Na1 83.1(4) . . ? C42 C43 Na1 70.0(4) . . ? C42 C44 Na1 67.2(3) . . ? C42 C44 Na1 87.5(4) . 5_656 ? Na1 C44 Na1 126.3(2) . 5_656 ? 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 N5 Na1 N1 C21 -120.6(3) . . . . ? N3 Na1 N1 C21 -13.2(4) . . . . ? C42 Na1 N1 C21 97.0(4) . . . . ? C43 Na1 N1 C21 89.0(4) . . . . ? C44 Na1 N1 C21 125.5(4) . . . . ? C44 Na1 N1 C21 119.5(4) 5_656 . . . ? N5 Na1 N1 C19 117.7(3) . . . . ? N3 Na1 N1 C19 -134.9(3) . . . . ? C42 Na1 N1 C19 -24.7(4) . . . . ? C43 Na1 N1 C19 -32.7(5) . . . . ? C44 Na1 N1 C19 3.9(4) . . . . ? C44 Na1 N1 C19 -2.2(5) 5_656 . . . ? N5 Na1 N1 C17 -0.9(3) . . . . ? N3 Na1 N1 C17 106.4(3) . . . . ? C42 Na1 N1 C17 -143.4(4) . . . . ? C43 Na1 N1 C17 -151.3(4) . . . . ? C44 Na1 N1 C17 -114.8(4) . . . . ? C44 Na1 N1 C17 -120.9(4) 5_656 . . . ? N6 Na2 N2 C18 -54.5(3) 6_556 . . . ? N4 Na2 N2 C18 58.9(3) 7_655 . . . ? C41 Na2 N2 C18 -179.5(9) 5_556 . . . ? C36 Na2 N2 C18 -174.8(4) 5_556 . . . ? C39 Na2 N2 C18 171.0(6) . . . . ? C40 Na2 N2 C18 -156.4(4) . . . . ? C38 Na2 N2 C18 149.2(4) . . . . ? C35 Na2 N2 C18 164.1(4) 5_556 . . . ? N6 Na2 N2 C22 63.8(3) 6_556 . . . ? N4 Na2 N2 C22 177.2(3) 7_655 . . . ? C41 Na2 N2 C22 -61.2(9) 5_556 . . . ? C36 Na2 N2 C22 -56.5(4) 5_556 . . . ? C39 Na2 N2 C22 -70.7(6) . . . . ? C40 Na2 N2 C22 -38.1(5) . . . . ? C38 Na2 N2 C22 -92.5(4) . . . . ? C35 Na2 N2 C22 -77.6(4) 5_556 . . . ? N6 Na2 N2 C20 -172.4(3) 6_556 . . . ? N4 Na2 N2 C20 -59.1(4) 7_655 . . . ? C41 Na2 N2 C20 62.5(9) 5_556 . . . ? C36 Na2 N2 C20 67.3(4) 5_556 . . . ? C39 Na2 N2 C20 53.1(7) . . . . ? C40 Na2 N2 C20 85.7(5) . . . . ? C38 Na2 N2 C20 31.3(4) . . . . ? C35 Na2 N2 C20 46.2(4) 5_556 . . . ? N5 Na1 N3 C25 56.2(4) . . . . ? N1 Na1 N3 C25 -54.1(4) . . . . ? C42 Na1 N3 C25 -159.7(4) . . . . ? C43 Na1 N3 C25 176.2(4) . . . . ? C44 Na1 N3 C25 -165.4(4) . . . . ? C44 Na1 N3 C25 151.6(4) 5_656 . . . ? N5 Na1 N3 C27 175.7(3) . . . . ? N1 Na1 N3 C27 65.4(4) . . . . ? C42 Na1 N3 C27 -40.2(4) . . . . ? C43 Na1 N3 C27 -64.3(4) . . . . ? C44 Na1 N3 C27 -45.9(5) . . . . ? C44 Na1 N3 C27 -88.9(4) 5_656 . . . ? N5 Na1 N3 C23 -66.8(4) . . . . ? N1 Na1 N3 C23 -177.1(3) . . . . ? C42 Na1 N3 C23 77.3(4) . . . . ? C43 Na1 N3 C23 53.2(4) . . . . ? C44 Na1 N3 C23 71.6(5) . . . . ? C44 Na1 N3 C23 28.6(4) 5_656 . . . ? N1 Na1 N5 C31 50.0(4) . . . . ? N3 Na1 N5 C31 -63.4(4) . . . . ? C42 Na1 N5 C31 170.4(4) . . . . ? C43 Na1 N5 C31 -156.6(4) . . . . ? C44 Na1 N5 C31 147.2(4) . . . . ? C44 Na1 N5 C31 -160.7(4) 5_656 . . . ? N1 Na1 N5 C29 -73.1(3) . . . . ? N3 Na1 N5 C29 173.4(3) . . . . ? C42 Na1 N5 C29 47.3(4) . . . . ? C43 Na1 N5 C29 80.3(4) . . . . ? C44 Na1 N5 C29 24.1(4) . . . . ? C44 Na1 N5 C29 76.2(3) 5_656 . . . ? N1 Na1 N5 C33 168.2(3) . . . . ? N3 Na1 N5 C33 54.8(3) . . . . ? C42 Na1 N5 C33 -71.4(4) . . . . ? C43 Na1 N5 C33 -38.4(4) . . . . ? C44 Na1 N5 C33 -94.6(3) . . . . ? C44 Na1 N5 C33 -42.5(3) 5_656 . . . ? C5A Mg1 C1 C2 78.3(9) . . . . ? C13 Mg1 C1 C2 -50.9(5) . . . . ? C5 Mg1 C1 C2 63.2(9) . . . . ? C9 Mg1 C1 C2 -169.0(4) . . . . ? Mg1 C1 C2 C3 176.3(4) . . . . ? C1 C2 C3 C4 -175.2(6) . . . . ? C5A Mg1 C5 C6 73(4) . . . . ? C1 Mg1 C5 C6 127(2) . . . . ? C13 Mg1 C5 C6 -117.0(18) . . . . ? C9 Mg1 C5 C6 -3(2) . . . . ? Mg1 C5 C6 C7 -164(2) . . . . ? C5 C6 C7 C8 -151(3) . . . . ? C5A Mg1 C9 C10 64.3(11) . . . . ? C1 Mg1 C9 C10 -48.3(7) . . . . ? C13 Mg1 C9 C10 -165.7(6) . . . . ? C5 Mg1 C9 C10 82.4(10) . . . . ? Mg1 C9 C10 C11 -175.7(7) . . . . ? C9 C10 C11 C12 178.9(12) . . . . ? C5A Mg1 C13 C14 -167.3(8) . . . . ? C1 Mg1 C13 C14 -48.8(5) . . . . ? C5 Mg1 C13 C14 -170.8(11) . . . . ? C9 Mg1 C13 C14 73.2(5) . . . . ? Mg1 C13 C14 C15 -177.2(5) . . . . ? C13 C14 C15 C16 -77.4(14) . . . . ? C1 Mg1 C5A C6A 119(4) . . . . ? C13 Mg1 C5A C6A -121(4) . . . . ? C5 Mg1 C5A C6A -110(6) . . . . ? C9 Mg1 C5A C6A 0(4) . . . . ? Mg1 C5A C6A C7A 151(3) . . . . ? C5A C6A C7A C8A -130(5) . . . . ? C21 N1 C17 C18 -63.5(5) . . . . ? C19 N1 C17 C18 51.8(5) . . . . ? Na1 N1 C17 C18 173.4(3) . . . . ? C22 N2 C18 C17 52.4(6) . . . . ? C20 N2 C18 C17 -63.6(5) . . . . ? Na2 N2 C18 C17 174.2(4) . . . . ? N1 C17 C18 N2 10.0(6) . . . . ? C21 N1 C19 C20 52.0(6) . . . . ? C17 N1 C19 C20 -63.0(6) . . . . ? Na1 N1 C19 C20 176.7(4) . . . . ? C18 N2 C20 C19 52.3(5) . . . . ? C22 N2 C20 C19 -64.4(5) . . . . ? Na2 N2 C20 C19 168.5(3) . . . . ? N1 C19 C20 N2 10.2(6) . . . . ? C19 N1 C21 C22 -62.4(5) . . . . ? C17 N1 C21 C22 52.5(5) . . . . ? Na1 N1 C21 C22 173.7(3) . . . . ? C18 N2 C22 C21 -62.8(5) . . . . ? C20 N2 C22 C21 53.5(5) . . . . ? Na2 N2 C22 C21 -179.0(3) . . . . ? N1 C21 C22 N2 8.6(6) . . . . ? C25 N3 C23 C24 56.5(6) . . . . ? C27 N3 C23 C24 -59.8(6) . . . . ? Na1 N3 C23 C24 -176.8(4) . . . . ? C28 N4 C24 C23 55.9(6) . . . . ? C26 N4 C24 C23 -59.6(6) . . . . ? Na2 N4 C24 C23 172.4(4) 7_665 . . . ? N3 C23 C24 N4 3.0(7) . . . . ? C27 N3 C25 C26 55.5(6) . . . . ? C23 N3 C25 C26 -60.1(6) . . . . ? Na1 N3 C25 C26 173.8(4) . . . . ? C28 N4 C26 C25 -60.1(6) . . . . ? C24 N4 C26 C25 55.7(6) . . . . ? Na2 N4 C26 C25 175.2(4) 7_665 . . . ? N3 C25 C26 N4 3.7(7) . . . . ? C25 N3 C27 C28 -58.4(6) . . . . ? C23 N3 C27 C28 57.2(6) . . . . ? Na1 N3 C27 C28 178.4(4) . . . . ? C24 N4 C28 C27 -58.3(6) . . . . ? C26 N4 C28 C27 57.3(6) . . . . ? Na2 N4 C28 C27 -172.2(4) 7_665 . . . ? N3 C27 C28 N4 1.5(7) . . . . ? C31 N5 C29 C30 56.5(5) . . . . ? C33 N5 C29 C30 -58.5(5) . . . . ? Na1 N5 C29 C30 -177.2(3) . . . . ? C32 N6 C30 C29 -57.8(6) . . . . ? C34 N6 C30 C29 57.3(5) . . . . ? Na2 N6 C30 C29 -166.3(3) 6_656 . . . ? N5 C29 C30 N6 1.6(6) . . . . ? C29 N5 C31 C32 -59.6(6) . . . . ? C33 N5 C31 C32 55.5(6) . . . . ? Na1 N5 C31 C32 173.8(4) . . . . ? C30 N6 C32 C31 55.5(6) . . . . ? C34 N6 C32 C31 -59.7(6) . . . . ? Na2 N6 C32 C31 169.2(4) 6_656 . . . ? N5 C31 C32 N6 3.0(7) . . . . ? C31 N5 C33 C34 -58.1(6) . . . . ? C29 N5 C33 C34 57.0(6) . . . . ? Na1 N5 C33 C34 179.8(4) . . . . ? C32 N6 C34 C33 56.5(6) . . . . ? C30 N6 C34 C33 -59.1(6) . . . . ? Na2 N6 C34 C33 173.1(3) 6_656 . . . ? N5 C33 C34 N6 1.9(7) . . . . ? C40 C35 C36 C37 0.0 . . . . ? Na2 C35 C36 C37 104.5(4) 5_556 . . . ? C40 C35 C36 C41 -175.7(16) . . . . ? Na2 C35 C36 C41 -71.1(13) 5_556 . . . ? C40 C35 C36 Na2 -104.5(4) . . . 5_556 ? C35 C36 C37 C38 0.0 . . . . ? C41 C36 C37 C38 175.6(16) . . . . ? Na2 C36 C37 C38 99.2(5) 5_556 . . . ? C36 C37 C38 C39 0.0 . . . . ? C36 C37 C38 Na2 64.5(3) . . . . ? N2 Na2 C38 C37 22.2(5) . . . . ? N6 Na2 C38 C37 -121.6(5) 6_556 . . . ? N4 Na2 C38 C37 124.9(5) 7_655 . . . ? C41 Na2 C38 C37 -118.2(12) 5_556 . . . ? C36 Na2 C38 C37 -61.7(7) 5_556 . . . ? C39 Na2 C38 C37 -123.36(15) . . . . ? C40 Na2 C38 C37 -91.12(18) . . . . ? C35 Na2 C38 C37 -10.4(8) 5_556 . . . ? N2 Na2 C38 C39 145.5(6) . . . . ? N6 Na2 C38 C39 1.8(5) 6_556 . . . ? N4 Na2 C38 C39 -111.7(5) 7_655 . . . ? C41 Na2 C38 C39 5.2(12) 5_556 . . . ? C36 Na2 C38 C39 61.7(7) 5_556 . . . ? C40 Na2 C38 C39 32.24(8) . . . . ? C35 Na2 C38 C39 112.9(7) 5_556 . . . ? C37 C38 C39 C40 0.0 . . . . ? Na2 C38 C39 C40 -74.5(4) . . . . ? C37 C38 C39 Na2 74.5(4) . . . . ? N2 Na2 C39 C40 75.1(8) . . . . ? N6 Na2 C39 C40 -56.6(4) 6_556 . . . ? N4 Na2 C39 C40 -169.5(5) 7_655 . . . ? C41 Na2 C39 C40 -33(6) 5_556 . . . ? C36 Na2 C39 C40 48.2(7) 5_556 . . . ? C38 Na2 C39 C40 122.16(9) . . . . ? C35 Na2 C39 C40 84.7(5) 5_556 . . . ? N2 Na2 C39 C38 -47.0(8) . . . . ? N6 Na2 C39 C38 -178.7(4) 6_556 . . . ? N4 Na2 C39 C38 68.3(4) 7_655 . . . ? C41 Na2 C39 C38 -155(5) 5_556 . . . ? C36 Na2 C39 C38 -74.0(7) 5_556 . . . ? C40 Na2 C39 C38 -122.16(9) . . . . ? C35 Na2 C39 C38 -37.5(5) 5_556 . . . ? C38 C39 C40 C35 0.0 . . . . ? Na2 C39 C40 C35 -75.9(3) . . . . ? C38 C39 C40 Na2 75.9(3) . . . . ? C36 C35 C40 C39 0.0 . . . . ? Na2 C35 C40 C39 -70.0(4) 5_556 . . . ? C36 C35 C40 Na2 -67.1(3) . . . . ? Na2 C35 C40 Na2 -137.2(4) 5_556 . . . ? N2 Na2 C40 C39 -125.7(6) . . . . ? N6 Na2 C40 C39 128.4(4) 6_556 . . . ? N4 Na2 C40 C39 12.5(5) 7_655 . . . ? C41 Na2 C40 C39 9.6(17) 5_556 . . . ? C36 Na2 C40 C39 -76.2(12) 5_556 . . . ? C38 Na2 C40 C39 -31.76(9) . . . . ? C35 Na2 C40 C39 -69.6(5) 5_556 . . . ? N2 Na2 C40 C35 -2.9(6) . . . . ? N6 Na2 C40 C35 -108.8(4) 6_556 . . . ? N4 Na2 C40 C35 135.2(5) 7_655 . . . ? C41 Na2 C40 C35 132.4(16) 5_556 . . . ? C36 Na2 C40 C35 46.6(12) 5_556 . . . ? C39 Na2 C40 C35 122.77(10) . . . . ? C38 Na2 C40 C35 91.01(16) . . . . ? C35 Na2 C40 C35 53.2(4) 5_556 . . . ? C35 C36 C41 Na2 82.3(10) . . . 5_556 ? C37 C36 C41 Na2 -93.4(9) . . . 5_556 ? N5 Na1 C42 C45 -175.8(10) . . . . ? N1 Na1 C42 C45 -53.3(11) . . . . ? N3 Na1 C42 C45 59.7(10) . . . . ? C43 Na1 C42 C45 114.2(13) . . . . ? C44 Na1 C42 C45 -128.5(12) . . . . ? C44 Na1 C42 C45 144.2(11) 5_656 . . . ? N5 Na1 C42 C43 70.0(7) . . . . ? N1 Na1 C42 C43 -167.5(6) . . . . ? N3 Na1 C42 C43 -54.5(6) . . . . ? C44 Na1 C42 C43 117.3(8) . . . . ? C44 Na1 C42 C43 30.0(5) 5_656 . . . ? N5 Na1 C42 C44 -47.3(6) . . . . ? N1 Na1 C42 C44 75.3(5) . . . . ? N3 Na1 C42 C44 -171.8(4) . . . . ? C43 Na1 C42 C44 -117.3(8) . . . . ? C44 Na1 C42 C44 -87.3(5) 5_656 . . . ? C45 C42 C43 Na1 -98.8(9) . . . . ? C44 C42 C43 Na1 77.4(5) . . . . ? N5 Na1 C43 C42 -130.8(6) . . . . ? N1 Na1 C43 C42 15.8(7) . . . . ? N3 Na1 C43 C42 128.3(6) . . . . ? C44 Na1 C43 C42 -34.8(5) . . . . ? C44 Na1 C43 C42 -121.5(8) 5_656 . . . ? C45 C42 C44 Na1 100.2(11) . . . . ? C43 C42 C44 Na1 -75.4(5) . . . . ? C45 C42 C44 Na1 -128.4(11) . . . 5_656 ? C43 C42 C44 Na1 56.1(5) . . . 5_656 ? Na1 C42 C44 Na1 131.4(2) . . . 5_656 ? N5 Na1 C44 C42 146.2(5) . . . . ? N1 Na1 C44 C42 -107.2(5) . . . . ? N3 Na1 C44 C42 11.2(6) . . . . ? C43 Na1 C44 C42 35.4(4) . . . . ? C44 Na1 C44 C42 68.4(5) 5_656 . . . ? N5 Na1 C44 Na1 77.8(4) . . . 5_656 ? N1 Na1 C44 Na1 -175.6(4) . . . 5_656 ? N3 Na1 C44 Na1 -57.2(5) . . . 5_656 ? C42 Na1 C44 Na1 -68.4(5) . . . 5_656 ? C43 Na1 C44 Na1 -33.0(3) . . . 5_656 ? C44 Na1 C44 Na1 0.0 5_656 . . 5_656 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 21.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.438 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.046