# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_shelxs _database_code_depnum_ccdc_archive 'CCDC 863421' #TrackingRef 'compd4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H74 Mg N6 O6 Si2' _chemical_formula_weight 1127.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 15.3573(3) _cell_length_b 7.48620(10) _cell_length_c 27.0680(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.4350(10) _cell_angle_gamma 90.00 _cell_volume 3026.79(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 1.083 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6134 _exptl_absorpt_correction_T_max 0.8125 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10114 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 68.25 _reflns_number_total 5503 _reflns_number_gt 3199 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1391P)^2^+0.0000P] 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 5503 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2465 _refine_ls_wR_factor_gt 0.2148 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Si1 Si -0.00014(6) 0.34768(15) 0.22384(4) 0.0502(3) Uani 1 1 d . . . Mg1 Mg 0.0000 0.0000 0.5000 0.0410(4) Uani 1 2 d S . . O1 O -0.03783(13) -0.2668(3) 0.46775(9) 0.0453(6) Uani 1 1 d . . . N1 N 0.09866(16) 0.0236(4) 0.45934(11) 0.0396(7) Uani 1 1 d . . . N2 N -0.09219(16) 0.1195(4) 0.44118(11) 0.0423(7) Uani 1 1 d . . . C1 C -0.1810(2) 0.1502(4) 0.43903(13) 0.0393(8) Uani 1 1 d . . . C2 C 0.0062(2) 0.1561(4) 0.38150(13) 0.0389(8) Uani 1 1 d . . . C11 C 0.0074(2) 0.2176(5) 0.33114(13) 0.0412(8) Uani 1 1 d . . . C3 C 0.0870(2) 0.0897(5) 0.41109(13) 0.0393(8) Uani 1 1 d . . . C4 C -0.2235(2) 0.1143(4) 0.47881(13) 0.0402(8) Uani 1 1 d . . . C5 C -0.0776(2) 0.1698(5) 0.39495(13) 0.0404(8) Uani 1 1 d . . . C12 C -0.3923(2) 0.2112(5) 0.46423(14) 0.0470(9) Uani 1 1 d . . . C6 C 0.2301(2) -0.0039(5) 0.43303(13) 0.0453(9) Uani 1 1 d . . . H1 H 0.2904 -0.0324 0.4332 0.054 Uiso 1 1 calc R . . C7 C -0.1596(2) 0.2344(5) 0.36263(14) 0.0442(9) Uani 1 1 d . . . H2 H -0.1675 0.2773 0.3289 0.053 Uiso 1 1 calc R . . C8 C -0.2229(2) 0.2221(5) 0.38963(13) 0.0439(8) Uani 1 1 d . . . H3 H -0.2841 0.2547 0.3782 0.053 Uiso 1 1 calc R . . C9 C 0.18533(19) -0.0343(5) 0.47376(13) 0.0408(8) Uani 1 1 d . . . O2 O -0.78360(18) 0.4387(4) 0.47620(13) 0.0766(9) Uani 1 1 d . . . N3 N -0.7470(2) 0.4628(5) 0.44111(16) 0.0630(10) Uani 1 1 d . . . C30 C -0.1243(2) -0.3073(6) 0.43523(14) 0.0524(10) Uani 1 1 d . . . H4 H -0.1692 -0.2169 0.4392 0.063 Uiso 1 1 calc R . . H5 H -0.1452 -0.4267 0.4432 0.063 Uiso 1 1 calc R . . C13 C -0.4834(2) 0.2703(5) 0.45768(14) 0.0442(9) Uani 1 1 d . . . C14 C -0.3160(2) 0.1655(5) 0.47046(13) 0.0451(9) Uani 1 1 d . . . C15 C -0.6551(2) 0.3948(5) 0.44673(16) 0.0498(10) Uani 1 1 d . . . C16 C 0.0069(2) 0.2696(5) 0.28872(15) 0.0451(9) Uani 1 1 d . . . C17 C -0.6148(2) 0.3105(5) 0.49087(16) 0.0547(10) Uani 1 1 d . . . H6 H -0.6455 0.2950 0.5172 0.066 Uiso 1 1 calc R . . O3 O -0.78276(19) 0.5366(5) 0.40131(15) 0.0860(11) Uani 1 1 d . . . C10 C 0.1697(2) 0.0725(5) 0.39499(13) 0.0445(9) Uani 1 1 d . . . H7 H 0.1797 0.1088 0.3631 0.053 Uiso 1 1 calc R . . C31 C -0.0088(3) -0.3468(5) 0.38946(16) 0.0592(11) Uani 1 1 d . . . H8 H 0.0000 -0.4564 0.3707 0.071 Uiso 1 1 calc R . . H9 H 0.0238 -0.2468 0.3779 0.071 Uiso 1 1 calc R . . C18 C -0.5275(2) 0.3535(5) 0.41263(16) 0.0563(10) Uani 1 1 d . . . H10 H -0.4981 0.3667 0.3856 0.068 Uiso 1 1 calc R . . C32 C 0.0221(2) -0.3740(5) 0.44606(15) 0.0507(10) Uani 1 1 d . . . H11 H 0.0179 -0.5015 0.4550 0.061 Uiso 1 1 calc R . . H12 H 0.0847 -0.3337 0.4585 0.061 Uiso 1 1 calc R . . C19 C -0.5282(2) 0.2480(5) 0.49644(15) 0.0489(9) Uani 1 1 d . . . H13 H -0.4991 0.1894 0.5270 0.059 Uiso 1 1 calc R . . C20 C 0.1146(3) 0.3285(7) 0.21139(17) 0.0696(13) Uani 1 1 d . . . H14 H 0.1512 0.4174 0.2350 0.084 Uiso 1 1 calc R . . C21 C -0.6141(2) 0.4169(6) 0.40730(16) 0.0590(11) Uani 1 1 d . . . H15 H -0.6443 0.4745 0.3769 0.071 Uiso 1 1 calc R . . C22 C -0.1566(3) 0.1262(6) 0.20455(19) 0.0727(13) Uani 1 1 d . . . H16 H -0.1946 0.2270 0.2092 0.109 Uiso 1 1 calc R . . H17 H -0.1310 0.0707 0.2375 0.109 Uiso 1 1 calc R . . H18 H -0.1926 0.0380 0.1819 0.109 Uiso 1 1 calc R . . C23 C 0.1211(3) 0.3903(7) 0.15831(19) 0.0799(14) Uani 1 1 d . . . H19 H 0.1834 0.3820 0.1554 0.120 Uiso 1 1 calc R . . H20 H 0.1007 0.5143 0.1531 0.120 Uiso 1 1 calc R . . H21 H 0.0834 0.3139 0.1326 0.120 Uiso 1 1 calc R . . C33 C -0.1087(3) -0.3031(6) 0.38197(16) 0.0607(11) Uani 1 1 d . . . H22 H -0.1225 -0.1836 0.3664 0.073 Uiso 1 1 calc R . . H23 H -0.1461 -0.3933 0.3601 0.073 Uiso 1 1 calc R . . C24 C -0.0386(3) 0.5850(6) 0.21981(17) 0.0626(11) Uani 1 1 d . . . H24 H -0.0505 0.6217 0.1833 0.075 Uiso 1 1 calc R . . C25 C 0.1605(3) 0.1543(7) 0.2265(2) 0.0829(15) Uani 1 1 d . . . H25 H 0.1247 0.0572 0.2076 0.124 Uiso 1 1 calc R . . H26 H 0.1672 0.1355 0.2630 0.124 Uiso 1 1 calc R . . H27 H 0.2197 0.1559 0.2187 0.124 Uiso 1 1 calc R . . C26 C 0.0322(3) 0.7103(7) 0.2498(2) 0.0814(14) Uani 1 1 d . . . H28 H 0.0069 0.8305 0.2498 0.122 Uiso 1 1 calc R . . H29 H 0.0835 0.7138 0.2340 0.122 Uiso 1 1 calc R . . H30 H 0.0516 0.6673 0.2848 0.122 Uiso 1 1 calc R . . C27 C -0.1270(3) 0.6079(6) 0.23744(17) 0.0684(12) Uani 1 1 d . . . H31 H -0.1189 0.5632 0.2722 0.103 Uiso 1 1 calc R . . H32 H -0.1748 0.5404 0.2148 0.103 Uiso 1 1 calc R . . H33 H -0.1433 0.7347 0.2364 0.103 Uiso 1 1 calc R . . C28 C -0.0820(3) 0.1924(7) 0.18145(16) 0.0665(12) Uani 1 1 d . . . H34 H -0.0470 0.0845 0.1760 0.080 Uiso 1 1 calc R . . C29 C -0.1214(3) 0.2710(8) 0.12868(17) 0.0882(16) Uani 1 1 d . . . H35 H -0.1597 0.1818 0.1076 0.132 Uiso 1 1 calc R . . H36 H -0.0727 0.3045 0.1127 0.132 Uiso 1 1 calc R . . H37 H -0.1570 0.3771 0.1320 0.132 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 Si1 0.0386(6) 0.0744(8) 0.0389(6) 0.0060(5) 0.0116(5) 0.0031(5) Mg1 0.0230(7) 0.0636(11) 0.0369(10) 0.0028(8) 0.0077(7) 0.0015(6) O1 0.0272(11) 0.0631(15) 0.0450(15) -0.0037(12) 0.0072(10) 0.0015(10) N1 0.0222(13) 0.0580(18) 0.0384(18) -0.0013(14) 0.0066(12) -0.0004(11) N2 0.0239(13) 0.0626(19) 0.0396(18) 0.0012(14) 0.0057(12) 0.0010(12) C1 0.0268(15) 0.053(2) 0.040(2) 0.0001(16) 0.0118(15) 0.0043(14) C2 0.0292(16) 0.053(2) 0.0323(19) -0.0016(15) 0.0028(14) -0.0013(14) C11 0.0251(16) 0.061(2) 0.035(2) -0.0031(17) 0.0027(15) 0.0005(14) C3 0.0262(15) 0.058(2) 0.0332(19) -0.0039(16) 0.0057(14) -0.0012(14) C4 0.0238(15) 0.056(2) 0.041(2) 0.0009(16) 0.0085(14) 0.0033(14) C5 0.0293(16) 0.056(2) 0.0342(19) 0.0008(16) 0.0043(14) 0.0007(14) C12 0.0317(18) 0.064(2) 0.045(2) 0.0047(18) 0.0076(16) 0.0017(15) C6 0.0261(17) 0.068(2) 0.044(2) 0.0012(18) 0.0121(16) 0.0016(15) C7 0.0288(16) 0.066(2) 0.035(2) 0.0027(17) 0.0032(15) 0.0031(15) C8 0.0278(16) 0.063(2) 0.040(2) 0.0027(17) 0.0046(15) 0.0020(15) C9 0.0248(16) 0.059(2) 0.040(2) -0.0005(17) 0.0103(15) -0.0007(14) O2 0.0407(15) 0.101(2) 0.096(3) -0.0061(19) 0.0306(16) 0.0073(14) N3 0.0333(17) 0.071(2) 0.087(3) 0.000(2) 0.0177(19) 0.0055(15) C30 0.0276(17) 0.073(3) 0.053(2) -0.008(2) 0.0019(17) -0.0047(16) C13 0.0260(16) 0.059(2) 0.048(2) -0.0017(17) 0.0088(15) 0.0027(14) C14 0.0308(18) 0.062(2) 0.042(2) 0.0004(17) 0.0083(16) 0.0001(15) C15 0.0230(16) 0.068(2) 0.059(3) 0.002(2) 0.0109(17) 0.0026(15) C16 0.0283(17) 0.058(2) 0.048(2) 0.0027(18) 0.0059(16) -0.0009(15) C17 0.0371(19) 0.074(3) 0.056(3) -0.002(2) 0.0166(18) -0.0008(18) O3 0.0426(17) 0.107(3) 0.105(3) 0.024(2) 0.0104(18) 0.0227(16) C10 0.0344(18) 0.069(2) 0.033(2) 0.0025(17) 0.0124(15) -0.0014(16) C31 0.065(3) 0.063(3) 0.054(3) -0.005(2) 0.024(2) -0.0040(19) C18 0.0314(18) 0.084(3) 0.055(3) 0.009(2) 0.0123(17) 0.0029(17) C32 0.0359(18) 0.061(2) 0.057(3) -0.0018(18) 0.0135(17) 0.0063(16) C19 0.0312(17) 0.071(2) 0.045(2) 0.0026(18) 0.0095(16) 0.0023(16) C20 0.054(2) 0.102(4) 0.059(3) 0.016(3) 0.025(2) 0.010(2) C21 0.0344(19) 0.079(3) 0.062(3) 0.014(2) 0.0073(19) 0.0069(18) C22 0.060(3) 0.083(3) 0.069(3) -0.003(2) 0.002(2) -0.010(2) C23 0.070(3) 0.110(4) 0.071(3) 0.021(3) 0.041(3) 0.013(3) C33 0.056(2) 0.065(3) 0.053(3) -0.002(2) -0.004(2) -0.0043(19) C24 0.054(2) 0.083(3) 0.053(3) 0.013(2) 0.015(2) 0.003(2) C25 0.059(3) 0.122(4) 0.076(4) 0.020(3) 0.032(2) 0.028(3) C26 0.077(3) 0.082(3) 0.089(4) 0.000(3) 0.029(3) -0.005(3) C27 0.060(3) 0.082(3) 0.063(3) 0.009(2) 0.014(2) 0.016(2) C28 0.057(2) 0.097(3) 0.043(2) -0.002(2) 0.007(2) 0.014(2) C29 0.074(3) 0.138(5) 0.046(3) -0.002(3) 0.001(2) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C16 1.830(4) . ? Si1 C24 1.867(5) . ? Si1 C20 1.875(4) . ? Si1 C28 1.892(5) . ? Mg1 N2 2.072(3) 3_556 ? Mg1 N2 2.072(3) . ? Mg1 N1 2.077(2) 3_556 ? Mg1 N1 2.077(2) . ? Mg1 O1 2.203(2) 3_556 ? Mg1 O1 2.203(2) . ? O1 C32 1.444(4) . ? O1 C30 1.445(4) . ? N1 C9 1.368(4) . ? N1 C3 1.369(4) . ? N2 C1 1.372(4) . ? N2 C5 1.374(4) . ? C1 C4 1.409(5) . ? C1 C8 1.446(5) . ? C2 C3 1.402(4) . ? C2 C5 1.420(4) . ? C2 C11 1.443(5) . ? C11 C16 1.211(5) . ? C3 C10 1.441(4) . ? C4 C9 1.415(5) 3_556 ? C4 C14 1.437(4) . ? C5 C7 1.439(4) . ? C12 C14 1.195(4) . ? C12 C13 1.438(4) . ? C6 C10 1.343(5) . ? C6 C9 1.446(4) . ? C6 H1 0.9500 . ? C7 C8 1.349(5) . ? C7 H2 0.9500 . ? C8 H3 0.9500 . ? C9 C4 1.415(5) 3_556 ? O2 N3 1.224(4) . ? N3 O3 1.221(5) . ? N3 C15 1.475(4) . ? C30 C33 1.515(6) . ? C30 H4 0.9900 . ? C30 H5 0.9900 . ? C13 C19 1.392(5) . ? C13 C18 1.396(5) . ? C15 C21 1.370(5) . ? C15 C17 1.366(5) . ? C17 C19 1.384(5) . ? C17 H6 0.9500 . ? C10 H7 0.9500 . ? C31 C32 1.509(6) . ? C31 C33 1.536(5) . ? C31 H8 0.9900 . ? C31 H9 0.9900 . ? C18 C21 1.388(5) . ? C18 H10 0.9500 . ? C32 H11 0.9900 . ? C32 H12 0.9900 . ? C19 H13 0.9500 . ? C20 C25 1.493(6) . ? C20 C23 1.535(6) . ? C20 H14 1.0000 . ? C21 H15 0.9500 . ? C22 C28 1.511(6) . ? C22 H16 0.9800 . ? C22 H17 0.9800 . ? C22 H18 0.9800 . ? C23 H19 0.9800 . ? C23 H20 0.9800 . ? C23 H21 0.9800 . ? C33 H22 0.9900 . ? C33 H23 0.9900 . ? C24 C26 1.519(6) . ? C24 C27 1.550(5) . ? C24 H24 1.0000 . ? C25 H25 0.9800 . ? C25 H26 0.9800 . ? C25 H27 0.9800 . ? C26 H28 0.9800 . ? C26 H29 0.9800 . ? C26 H30 0.9800 . ? C27 H31 0.9800 . ? C27 H32 0.9800 . ? C27 H33 0.9800 . ? C28 C29 1.533(6) . ? C28 H34 1.0000 . ? C29 H35 0.9800 . ? C29 H36 0.9800 . ? C29 H37 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 C16 Si1 C24 107.91(18) . . ? C16 Si1 C20 107.41(17) . . ? C24 Si1 C20 111.1(2) . . ? C16 Si1 C28 105.59(18) . . ? C24 Si1 C28 113.1(2) . . ? C20 Si1 C28 111.3(2) . . ? N2 Mg1 N2 180.00(13) 3_556 . ? N2 Mg1 N1 90.48(11) 3_556 3_556 ? N2 Mg1 N1 89.52(11) . 3_556 ? N2 Mg1 N1 89.52(11) 3_556 . ? N2 Mg1 N1 90.48(11) . . ? N1 Mg1 N1 180.00(11) 3_556 . ? N2 Mg1 O1 90.96(10) 3_556 3_556 ? N2 Mg1 O1 89.04(10) . 3_556 ? N1 Mg1 O1 91.43(9) 3_556 3_556 ? N1 Mg1 O1 88.57(9) . 3_556 ? N2 Mg1 O1 89.04(10) 3_556 . ? N2 Mg1 O1 90.96(10) . . ? N1 Mg1 O1 88.57(9) 3_556 . ? N1 Mg1 O1 91.43(9) . . ? O1 Mg1 O1 180.00(5) 3_556 . ? C32 O1 C30 102.6(3) . . ? C32 O1 Mg1 122.0(2) . . ? C30 O1 Mg1 123.5(2) . . ? C9 N1 C3 106.9(3) . . ? C9 N1 Mg1 127.1(2) . . ? C3 N1 Mg1 125.90(19) . . ? C1 N2 C5 106.6(3) . . ? C1 N2 Mg1 126.9(2) . . ? C5 N2 Mg1 126.3(2) . . ? N2 C1 C4 124.6(3) . . ? N2 C1 C8 109.0(3) . . ? C4 C1 C8 126.3(3) . . ? C3 C2 C5 127.8(3) . . ? C3 C2 C11 116.7(3) . . ? C5 C2 C11 115.5(3) . . ? C16 C11 C2 179.0(3) . . ? N1 C3 C2 125.1(3) . . ? N1 C3 C10 109.1(3) . . ? C2 C3 C10 125.7(3) . . ? C1 C4 C9 127.3(3) . 3_556 ? C1 C4 C14 116.4(3) . . ? C9 C4 C14 116.2(3) 3_556 . ? N2 C5 C2 124.2(3) . . ? N2 C5 C7 110.0(3) . . ? C2 C5 C7 125.8(3) . . ? C14 C12 C13 178.4(4) . . ? C10 C6 C9 106.6(3) . . ? C10 C6 H1 126.7 . . ? C9 C6 H1 126.7 . . ? C8 C7 C5 106.7(3) . . ? C8 C7 H2 126.7 . . ? C5 C7 H2 126.7 . . ? C7 C8 C1 107.7(3) . . ? C7 C8 H3 126.1 . . ? C1 C8 H3 126.1 . . ? N1 C9 C4 124.4(3) . 3_556 ? N1 C9 C6 109.6(3) . . ? C4 C9 C6 126.0(3) 3_556 . ? O3 N3 O2 123.9(3) . . ? O3 N3 C15 118.0(4) . . ? O2 N3 C15 118.0(4) . . ? O1 C30 C33 104.4(3) . . ? O1 C30 H4 110.9 . . ? C33 C30 H4 110.9 . . ? O1 C30 H5 110.9 . . ? C33 C30 H5 110.9 . . ? H4 C30 H5 108.9 . . ? C19 C13 C18 119.2(3) . . ? C19 C13 C12 120.4(3) . . ? C18 C13 C12 120.3(3) . . ? C12 C14 C4 178.6(4) . . ? C21 C15 C17 122.6(3) . . ? C21 C15 N3 118.7(4) . . ? C17 C15 N3 118.6(3) . . ? C11 C16 Si1 177.0(3) . . ? C15 C17 C19 118.7(4) . . ? C15 C17 H6 120.6 . . ? C19 C17 H6 120.6 . . ? C6 C10 C3 107.8(3) . . ? C6 C10 H7 126.1 . . ? C3 C10 H7 126.1 . . ? C32 C31 C33 103.3(3) . . ? C32 C31 H8 111.1 . . ? C33 C31 H8 111.1 . . ? C32 C31 H9 111.1 . . ? C33 C31 H9 111.1 . . ? H8 C31 H9 109.1 . . ? C21 C18 C13 120.1(4) . . ? C21 C18 H10 120.0 . . ? C13 C18 H10 120.0 . . ? O1 C32 C31 105.0(3) . . ? O1 C32 H11 110.7 . . ? C31 C32 H11 110.7 . . ? O1 C32 H12 110.7 . . ? C31 C32 H12 110.7 . . ? H11 C32 H12 108.8 . . ? C17 C19 C13 120.5(4) . . ? C17 C19 H13 119.7 . . ? C13 C19 H13 119.7 . . ? C25 C20 C23 112.9(4) . . ? C25 C20 Si1 114.9(3) . . ? C23 C20 Si1 114.4(3) . . ? C25 C20 H14 104.3 . . ? C23 C20 H14 104.3 . . ? Si1 C20 H14 104.3 . . ? C15 C21 C18 118.8(4) . . ? C15 C21 H15 120.6 . . ? C18 C21 H15 120.6 . . ? C28 C22 H16 109.5 . . ? C28 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? C28 C22 H18 109.5 . . ? H16 C22 H18 109.5 . . ? H17 C22 H18 109.5 . . ? C20 C23 H19 109.5 . . ? C20 C23 H20 109.5 . . ? H19 C23 H20 109.5 . . ? C20 C23 H21 109.5 . . ? H19 C23 H21 109.5 . . ? H20 C23 H21 109.5 . . ? C30 C33 C31 104.1(3) . . ? C30 C33 H22 110.9 . . ? C31 C33 H22 110.9 . . ? C30 C33 H23 110.9 . . ? C31 C33 H23 110.9 . . ? H22 C33 H23 108.9 . . ? C26 C24 C27 109.7(4) . . ? C26 C24 Si1 112.3(3) . . ? C27 C24 Si1 112.0(3) . . ? C26 C24 H24 107.6 . . ? C27 C24 H24 107.6 . . ? Si1 C24 H24 107.6 . . ? C20 C25 H25 109.5 . . ? C20 C25 H26 109.5 . . ? H25 C25 H26 109.5 . . ? C20 C25 H27 109.5 . . ? H25 C25 H27 109.5 . . ? H26 C25 H27 109.5 . . ? C24 C26 H28 109.5 . . ? C24 C26 H29 109.5 . . ? H28 C26 H29 109.5 . . ? C24 C26 H30 109.5 . . ? H28 C26 H30 109.5 . . ? H29 C26 H30 109.5 . . ? C24 C27 H31 109.5 . . ? C24 C27 H32 109.5 . . ? H31 C27 H32 109.5 . . ? C24 C27 H33 109.5 . . ? H31 C27 H33 109.5 . . ? H32 C27 H33 109.5 . . ? C22 C28 C29 109.8(4) . . ? C22 C28 Si1 114.3(3) . . ? C29 C28 Si1 113.1(3) . . ? C22 C28 H34 106.4 . . ? C29 C28 H34 106.4 . . ? Si1 C28 H34 106.4 . . ? C28 C29 H35 109.5 . . ? C28 C29 H36 109.5 . . ? H35 C29 H36 109.5 . . ? C28 C29 H37 109.5 . . ? H35 C29 H37 109.5 . . ? H36 C29 H37 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 Mg1 O1 C32 -68.9(2) 3_556 . . . ? N2 Mg1 O1 C32 111.1(2) . . . . ? N1 Mg1 O1 C32 -159.5(2) 3_556 . . . ? N1 Mg1 O1 C32 20.5(2) . . . . ? O1 Mg1 O1 C32 62(20) 3_556 . . . ? N2 Mg1 O1 C30 154.8(2) 3_556 . . . ? N2 Mg1 O1 C30 -25.2(2) . . . . ? N1 Mg1 O1 C30 64.3(2) 3_556 . . . ? N1 Mg1 O1 C30 -115.7(2) . . . . ? O1 Mg1 O1 C30 -74(20) 3_556 . . . ? N2 Mg1 N1 C9 1.9(3) 3_556 . . . ? N2 Mg1 N1 C9 -178.1(3) . . . . ? N1 Mg1 N1 C9 -140(100) 3_556 . . . ? O1 Mg1 N1 C9 92.9(3) 3_556 . . . ? O1 Mg1 N1 C9 -87.1(3) . . . . ? N2 Mg1 N1 C3 177.0(3) 3_556 . . . ? N2 Mg1 N1 C3 -3.0(3) . . . . ? N1 Mg1 N1 C3 36(100) 3_556 . . . ? O1 Mg1 N1 C3 -92.0(3) 3_556 . . . ? O1 Mg1 N1 C3 88.0(3) . . . . ? N2 Mg1 N2 C1 149(49) 3_556 . . . ? N1 Mg1 N2 C1 -1.6(3) 3_556 . . . ? N1 Mg1 N2 C1 178.4(3) . . . . ? O1 Mg1 N2 C1 -93.1(3) 3_556 . . . ? O1 Mg1 N2 C1 86.9(3) . . . . ? N2 Mg1 N2 C5 -25(49) 3_556 . . . ? N1 Mg1 N2 C5 -175.9(3) 3_556 . . . ? N1 Mg1 N2 C5 4.1(3) . . . . ? O1 Mg1 N2 C5 92.7(3) 3_556 . . . ? O1 Mg1 N2 C5 -87.3(3) . . . . ? C5 N2 C1 C4 179.3(3) . . . . ? Mg1 N2 C1 C4 4.1(5) . . . . ? C5 N2 C1 C8 0.1(4) . . . . ? Mg1 N2 C1 C8 -175.1(2) . . . . ? C3 C2 C11 C16 172(100) . . . . ? C5 C2 C11 C16 -8(21) . . . . ? C9 N1 C3 C2 177.3(3) . . . . ? Mg1 N1 C3 C2 1.4(5) . . . . ? C9 N1 C3 C10 -0.1(4) . . . . ? Mg1 N1 C3 C10 -176.1(2) . . . . ? C5 C2 C3 N1 0.6(6) . . . . ? C11 C2 C3 N1 -179.2(3) . . . . ? C5 C2 C3 C10 177.6(3) . . . . ? C11 C2 C3 C10 -2.2(5) . . . . ? N2 C1 C4 C9 -3.2(6) . . . 3_556 ? C8 C1 C4 C9 175.9(3) . . . 3_556 ? N2 C1 C4 C14 176.4(3) . . . . ? C8 C1 C4 C14 -4.5(5) . . . . ? C1 N2 C5 C2 -178.9(3) . . . . ? Mg1 N2 C5 C2 -3.7(5) . . . . ? C1 N2 C5 C7 0.0(4) . . . . ? Mg1 N2 C5 C7 175.2(2) . . . . ? C3 C2 C5 N2 0.7(6) . . . . ? C11 C2 C5 N2 -179.6(3) . . . . ? C3 C2 C5 C7 -178.1(3) . . . . ? C11 C2 C5 C7 1.7(5) . . . . ? N2 C5 C7 C8 -0.1(4) . . . . ? C2 C5 C7 C8 178.8(3) . . . . ? C5 C7 C8 C1 0.2(4) . . . . ? N2 C1 C8 C7 -0.1(4) . . . . ? C4 C1 C8 C7 -179.3(3) . . . . ? C3 N1 C9 C4 -179.1(3) . . . 3_556 ? Mg1 N1 C9 C4 -3.2(5) . . . 3_556 ? C3 N1 C9 C6 -0.1(4) . . . . ? Mg1 N1 C9 C6 175.8(2) . . . . ? C10 C6 C9 N1 0.3(4) . . . . ? C10 C6 C9 C4 179.3(3) . . . 3_556 ? C32 O1 C30 C33 -43.5(4) . . . . ? Mg1 O1 C30 C33 99.6(3) . . . . ? C14 C12 C13 C19 -73(16) . . . . ? C14 C12 C13 C18 106(16) . . . . ? C13 C12 C14 C4 1(30) . . . . ? C1 C4 C14 C12 -106(18) . . . . ? C9 C4 C14 C12 74(18) 3_556 . . . ? O3 N3 C15 C21 -0.1(6) . . . . ? O2 N3 C15 C21 178.4(4) . . . . ? O3 N3 C15 C17 -179.4(4) . . . . ? O2 N3 C15 C17 -0.8(5) . . . . ? C2 C11 C16 Si1 -8(27) . . . . ? C24 Si1 C16 C11 74(7) . . . . ? C20 Si1 C16 C11 -166(7) . . . . ? C28 Si1 C16 C11 -47(7) . . . . ? C21 C15 C17 C19 1.4(6) . . . . ? N3 C15 C17 C19 -179.4(3) . . . . ? C9 C6 C10 C3 -0.4(4) . . . . ? N1 C3 C10 C6 0.3(4) . . . . ? C2 C3 C10 C6 -177.1(3) . . . . ? C19 C13 C18 C21 1.6(6) . . . . ? C12 C13 C18 C21 -177.4(4) . . . . ? C30 O1 C32 C31 44.4(4) . . . . ? Mg1 O1 C32 C31 -99.4(3) . . . . ? C33 C31 C32 O1 -27.2(4) . . . . ? C15 C17 C19 C13 -0.2(6) . . . . ? C18 C13 C19 C17 -1.2(6) . . . . ? C12 C13 C19 C17 177.7(3) . . . . ? C16 Si1 C20 C25 47.3(4) . . . . ? C24 Si1 C20 C25 165.1(4) . . . . ? C28 Si1 C20 C25 -67.8(4) . . . . ? C16 Si1 C20 C23 -179.6(3) . . . . ? C24 Si1 C20 C23 -61.7(4) . . . . ? C28 Si1 C20 C23 65.3(4) . . . . ? C17 C15 C21 C18 -1.0(6) . . . . ? N3 C15 C21 C18 179.8(4) . . . . ? C13 C18 C21 C15 -0.5(6) . . . . ? O1 C30 C33 C31 25.8(4) . . . . ? C32 C31 C33 C30 0.8(4) . . . . ? C16 Si1 C24 C26 69.6(3) . . . . ? C20 Si1 C24 C26 -47.9(4) . . . . ? C28 Si1 C24 C26 -174.0(3) . . . . ? C16 Si1 C24 C27 -54.3(3) . . . . ? C20 Si1 C24 C27 -171.8(3) . . . . ? C28 Si1 C24 C27 62.1(4) . . . . ? C16 Si1 C28 C22 33.7(4) . . . . ? C24 Si1 C28 C22 -84.1(4) . . . . ? C20 Si1 C28 C22 149.9(3) . . . . ? C16 Si1 C28 C29 160.2(3) . . . . ? C24 Si1 C28 C29 42.4(4) . . . . ? C20 Si1 C28 C29 -83.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.470 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.073 data_PhMgPor _database_code_depnum_ccdc_archive 'CCDC 873617' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; DiphenylethynylBistriisopropylsilylethynelPorphyrinMg ; _chemical_name_common MgTIPSTEP-Ph _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H68 Mg N4 O2 Si2' _chemical_formula_weight 957.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7018(2) _cell_length_b 16.4164(3) _cell_length_c 16.4397(3) _cell_angle_alpha 102.6540(10) _cell_angle_beta 98.9910(10) _cell_angle_gamma 95.3040(10) _cell_volume 2759.28(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_type ? _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 1.54187 _diffrn_radiation_type CuK(J\(Ba _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17882 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0876 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 66.99 _reflns_number_total 9738 _reflns_number_gt 3561 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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/[(J\(Bs^2^(Fo^2^)+(0.2000P)^2^+0.0000P] 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 0.0020(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^(J\(Bl^3^/sin(2(J\(Bq)]^-1/4^ _refine_ls_number_reflns 9738 _refine_ls_number_parameters 642 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2162 _refine_ls_R_factor_gt 0.1206 _refine_ls_wR_factor_ref 0.4209 _refine_ls_wR_factor_gt 0.3153 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_restrained_S_all 1.202 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.7680(2) 0.59134(12) 0.05882(12) 0.0802(7) Uani 1 1 d . . . Mg1 Mg 0.7106(2) 0.11628(13) -0.20079(13) 0.0714(7) Uani 1 1 d . . . Si2 Si 0.8360(2) -0.33178(13) -0.44582(13) 0.0923(8) Uani 1 1 d . . . N1 N 0.7650(5) 0.1834(3) -0.0756(3) 0.0676(14) Uani 1 1 d . . . N2 N 0.7216(5) 0.0598(3) -0.3235(3) 0.0689(14) Uani 1 1 d . . . N3 N 0.7775(5) 0.0138(3) -0.1628(3) 0.0719(15) Uani 1 1 d . . . N4 N 0.7148(5) 0.2303(3) -0.2363(3) 0.0700(14) Uani 1 1 d . . . C1 C 0.7397(6) 0.3256(4) -0.0952(4) 0.0713(18) Uani 1 1 d . . . C2 C 0.7216(6) 0.3078(4) -0.1844(4) 0.0685(17) Uani 1 1 d . . . C3 C 0.8058(6) 0.0021(4) -0.0824(4) 0.0710(17) Uani 1 1 d . . . C4 C 0.8385(6) 0.0454(4) 0.0719(5) 0.0736(18) Uani 1 1 d . . . C5 C 0.7990(7) 0.2153(5) 0.0701(4) 0.085(2) Uani 1 1 d . . . H1 H 0.8150 0.2083 0.1252 0.102 Uiso 1 1 calc R . . C6 C 0.7106(6) 0.3708(4) -0.2323(4) 0.0741(19) Uani 1 1 d . . . H2 H 0.7140 0.4284 -0.2108 0.089 Uiso 1 1 calc R . . C7 C 0.8631(7) 0.0290(5) 0.1405(5) 0.081(2) Uani 1 1 d . . . C8 C 0.6580(7) 0.1983(4) -0.4713(5) 0.083(2) Uani 1 1 d . . . C9 C 0.8111(6) 0.0669(5) -0.0088(4) 0.0718(18) Uani 1 1 d . . . C10 C 0.6856(7) 0.1771(4) -0.3909(4) 0.0735(18) Uani 1 1 d . . . C11 C 0.7851(6) -0.0632(4) -0.2148(4) 0.0693(17) Uani 1 1 d . . . C12 C 0.6944(6) 0.3303(4) -0.3146(4) 0.0744(19) Uani 1 1 d . . . H3 H 0.6827 0.3541 -0.3612 0.089 Uiso 1 1 calc R . . C13 C 0.8880(7) 0.0087(5) 0.2221(4) 0.0760(19) Uani 1 1 d . . . C14 C 0.8221(7) -0.1218(4) -0.1653(4) 0.079(2) Uani 1 1 d . . . H4 H 0.8351 -0.1772 -0.1858 0.095 Uiso 1 1 calc R . . C15 C 0.7566(6) 0.2664(4) -0.0440(4) 0.0693(17) Uani 1 1 d . . . C16 C 0.6989(6) 0.2427(4) -0.3158(4) 0.0732(18) Uani 1 1 d . . . C17 C 0.7643(7) -0.0808(4) -0.3032(4) 0.078(2) Uani 1 1 d . . . C18 C 0.7787(7) 0.2881(5) 0.0473(4) 0.080(2) Uani 1 1 d . . . H5 H 0.7789 0.3407 0.0829 0.096 Uiso 1 1 calc R . . C19 C 0.7332(6) -0.0232(4) -0.3544(4) 0.0722(18) Uani 1 1 d . . . C20 C 0.7915(6) 0.1511(4) -0.0058(4) 0.0721(18) Uani 1 1 d . . . C21 C 0.6862(7) 0.0271(5) -0.4704(4) 0.087(2) Uani 1 1 d . . . H6 H 0.6685 0.0339 -0.5255 0.104 Uiso 1 1 calc R . . C22 C 0.6945(6) 0.0909(4) -0.3942(4) 0.0702(17) Uani 1 1 d . . . C23 C 0.6126(7) 0.2243(5) -0.6256(4) 0.086(2) Uani 1 1 d . . . C24 C 0.8342(7) -0.0817(4) -0.0846(4) 0.0766(19) Uani 1 1 d . . . H7 H 0.8570 -0.1040 -0.0379 0.092 Uiso 1 1 calc R . . C25 C 0.7513(6) 0.4842(4) -0.0091(4) 0.0752(19) Uani 1 1 d . . . C26 C 0.7807(7) -0.1645(5) -0.3496(4) 0.082(2) Uani 1 1 d . . . C27 C 0.7454(7) 0.4127(5) -0.0487(4) 0.0766(19) Uani 1 1 d . . . C28 C 0.7092(7) -0.0449(5) -0.4470(4) 0.087(2) Uani 1 1 d . . . H8 H 0.7096 -0.0974 -0.4825 0.105 Uiso 1 1 calc R . . C29 C 0.6382(7) 0.2121(4) -0.5407(5) 0.086(2) Uani 1 1 d . . . C30 C 0.9258(7) -0.0673(5) 0.2305(4) 0.087(2) Uani 1 1 d . . . H9 H 0.9365 -0.1066 0.1828 0.105 Uiso 1 1 calc R . . C31 C 0.7992(7) -0.2323(4) -0.3865(4) 0.082(2) Uani 1 1 d . . . C32 C 0.9316(8) -0.0302(6) 0.3788(5) 0.103(3) Uani 1 1 d . . . H10 H 0.9448 -0.0439 0.4311 0.123 Uiso 1 1 calc R . . C33 C 0.8724(7) 0.0676(5) 0.2948(5) 0.087(2) Uani 1 1 d . . . H11 H 0.8471 0.1195 0.2910 0.105 Uiso 1 1 calc R . . C34 C 0.8956(8) 0.0464(6) 0.3717(5) 0.098(3) Uani 1 1 d . . . H12 H 0.8865 0.0851 0.4203 0.117 Uiso 1 1 calc R . . C35 C 0.9477(7) -0.0856(5) 0.3079(5) 0.095(2) Uani 1 1 d . . . H13 H 0.9743 -0.1371 0.3123 0.114 Uiso 1 1 calc R . . C36 C 0.9807(8) -0.3049(5) -0.4924(5) 0.098(2) Uani 1 1 d . . . H61 H 1.0469 -0.2759 -0.4438 0.117 Uiso 1 1 calc R . . C37 C 1.0360(11) -0.3808(6) -0.5365(6) 0.147(4) Uani 1 1 d . . . H19 H 0.9740 -0.4130 -0.5840 0.221 Uiso 1 1 calc R A . H20 H 1.0578 -0.4152 -0.4975 0.221 Uiso 1 1 calc R . . H21 H 1.1111 -0.3621 -0.5561 0.221 Uiso 1 1 calc R . . C38 C 0.9219(8) 0.6050(5) 0.1357(5) 0.100(2) Uani 1 1 d . . . H62 H 0.9881 0.6033 0.1006 0.119 Uiso 1 1 calc R . . C39 C 0.5348(9) 0.1624(8) -0.7739(6) 0.125(3) Uani 1 1 d . . . H14 H 0.4985 0.1166 -0.8182 0.150 Uiso 1 1 calc R . . C40 C 0.7742(11) 0.6699(6) -0.0084(6) 0.128(3) Uani 1 1 d . . . H63 H 0.7836 0.7264 0.0288 0.153 Uiso 1 1 calc R . . C41 C 0.8843(12) 0.6647(7) -0.0532(8) 0.168(5) Uani 1 1 d . . . H22 H 0.8715 0.6125 -0.0953 0.252 Uiso 1 1 calc R . . H23 H 0.9610 0.6674 -0.0131 0.252 Uiso 1 1 calc R . . H24 H 0.8916 0.7109 -0.0800 0.252 Uiso 1 1 calc R . . C43 C 0.8822(12) -0.3946(6) -0.3649(6) 0.124(3) Uani 1 1 d . . . H64 H 0.9044 -0.4483 -0.3948 0.149 Uiso 1 1 calc R . . C44 C 0.9628(9) -0.2423(6) -0.5489(5) 0.123(3) Uani 1 1 d . . . H25 H 1.0437 -0.2238 -0.5616 0.184 Uiso 1 1 calc R A . H26 H 0.9284 -0.1946 -0.5197 0.184 Uiso 1 1 calc R . . H27 H 0.9050 -0.2692 -0.6006 0.184 Uiso 1 1 calc R . . C45 C 0.5667(10) 0.2397(9) -0.7882(7) 0.129(4) Uani 1 1 d . . . H15 H 0.5538 0.2449 -0.8440 0.154 Uiso 1 1 calc R . . C46 C 0.5586(8) 0.1549(6) -0.6912(5) 0.111(3) Uani 1 1 d . . . H16 H 0.5384 0.1031 -0.6792 0.133 Uiso 1 1 calc R . . C47 C 0.9430(10) 0.5377(6) 0.1818(6) 0.143(4) Uani 1 1 d . . . H28 H 1.0296 0.5469 0.2117 0.214 Uiso 1 1 calc R . . H29 H 0.9274 0.4839 0.1420 0.214 Uiso 1 1 calc R . . H30 H 0.8858 0.5389 0.2215 0.214 Uiso 1 1 calc R . . C48 C 0.6412(12) 0.2987(7) -0.6427(6) 0.158(5) Uani 1 1 d . . . H17 H 0.6786 0.3446 -0.5988 0.190 Uiso 1 1 calc R . . C49 C 0.9516(8) 0.6918(6) 0.1964(5) 0.132(3) Uani 1 1 d . . . H31 H 0.8916 0.6976 0.2344 0.198 Uiso 1 1 calc R . . H32 H 0.9456 0.7344 0.1647 0.198 Uiso 1 1 calc R . . H33 H 1.0365 0.6983 0.2285 0.198 Uiso 1 1 calc R . . C50 C 0.6478(12) 0.6580(7) -0.0755(7) 0.190(6) Uani 1 1 d . . . H34 H 0.6451 0.7063 -0.0995 0.285 Uiso 1 1 calc R . . H35 H 0.5754 0.6521 -0.0483 0.285 Uiso 1 1 calc R . . H36 H 0.6456 0.6084 -0.1197 0.285 Uiso 1 1 calc R . . C51 C 0.9994(11) -0.3498(8) -0.2963(6) 0.162(4) Uani 1 1 d . . . H37 H 0.9817 -0.2956 -0.2681 0.242 Uiso 1 1 calc R A . H38 H 1.0724 -0.3429 -0.3226 0.242 Uiso 1 1 calc R . . H39 H 1.0167 -0.3832 -0.2557 0.242 Uiso 1 1 calc R . . C52 C 0.6119(11) 0.5339(7) 0.1665(7) 0.169(5) Uani 1 1 d . . . H40 H 0.6910 0.5403 0.2054 0.253 Uiso 1 1 calc R . . H41 H 0.5947 0.4775 0.1318 0.253 Uiso 1 1 calc R . . H42 H 0.5441 0.5448 0.1977 0.253 Uiso 1 1 calc R . . C53 C 0.6157(12) 0.3091(8) -0.7266(8) 0.162(5) Uani 1 1 d . . . H18 H 0.6320 0.3614 -0.7387 0.194 Uiso 1 1 calc R . . C54 C 0.6384(16) -0.3253(12) -0.5825(10) 0.131(7) Uani 0.50 1 d P A 1 H43 H 0.6983 -0.3076 -0.6150 0.196 Uiso 1 1 calc R A 1 H44 H 0.6168 -0.2768 -0.5456 0.196 Uiso 1 1 calc R A 1 H45 H 0.5627 -0.3557 -0.6202 0.196 Uiso 1 1 calc R A 1 C55 C 0.6956(12) -0.3801(7) -0.5318(8) 0.152(4) Uani 1 1 d . A 1 H65 H 0.6302 -0.3850 -0.4969 0.182 Uiso 1 1 calc R A 1 C56 C 0.7659(14) -0.4142(7) -0.3230(7) 0.187(6) Uani 1 1 d . . . H46 H 0.7890 -0.4473 -0.2829 0.280 Uiso 1 1 calc R A . H47 H 0.6961 -0.4450 -0.3659 0.280 Uiso 1 1 calc R . . H48 H 0.7410 -0.3624 -0.2944 0.280 Uiso 1 1 calc R . . O1 O 0.5189(4) 0.0881(3) -0.2116(3) 0.0831(14) Uani 1 1 d . . . H1A H 0.4903 0.0676 -0.1684 0.100 Uiso 1 1 calc R . . C58 C 0.4236(8) 0.0970(5) -0.2799(5) 0.110(3) Uani 1 1 d . . . H58 H 0.4621 0.1290 -0.3141 0.165 Uiso 1 1 calc R . . H59 H 0.3579 0.1258 -0.2572 0.165 Uiso 1 1 calc R . . H60 H 0.3869 0.0423 -0.3142 0.165 Uiso 1 1 calc R . . C59 C 0.6214(7) 0.5974(6) 0.1090(6) 0.116(3) Uani 1 1 d . . . H66 H 0.5469 0.5819 0.0631 0.139 Uiso 1 1 calc R . . C60 C 0.6151(8) 0.6888(6) 0.1596(7) 0.150(4) Uani 1 1 d . . . H49 H 0.5356 0.6909 0.1796 0.225 Uiso 1 1 calc R . . H50 H 0.6214 0.7269 0.1232 0.225 Uiso 1 1 calc R . . H51 H 0.6845 0.7049 0.2070 0.225 Uiso 1 1 calc R . . O2 O 0.4242(8) 0.0517(6) -0.0860(4) 0.179(4) Uani 1 1 d . . . H67 H 0.3727 0.0143 -0.0800 0.269 Uiso 1 1 calc R . . C61 C 0.4466(9) 0.1167(7) -0.0153(6) 0.150(4) Uani 1 1 d . . . H52 H 0.4280 0.0959 0.0324 0.224 Uiso 1 1 calc R . . H53 H 0.3930 0.1588 -0.0243 0.224 Uiso 1 1 calc R . . H54 H 0.5345 0.1409 -0.0042 0.224 Uiso 1 1 calc R . . C62 C 0.6971(15) -0.4721(9) -0.5701(10) 0.259(8) Uani 1 1 d . . . H55 H 0.6183 -0.4945 -0.6086 0.389 Uiso 1 1 calc R A 1 H56 H 0.7070 -0.5020 -0.5259 0.389 Uiso 1 1 calc R A 1 H57 H 0.7670 -0.4784 -0.6001 0.389 Uiso 1 1 calc R A 1 C63 C 0.566(4) -0.381(2) -0.519(2) 0.241(14) Uiso 0.50 1 d P B 2 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 Si1 0.0943(16) 0.0688(13) 0.0749(13) 0.0079(10) 0.0139(11) 0.0218(11) Mg1 0.0820(16) 0.0727(15) 0.0608(14) 0.0125(11) 0.0164(11) 0.0189(11) Si2 0.130(2) 0.0702(13) 0.0771(14) 0.0077(11) 0.0256(13) 0.0270(12) N1 0.078(4) 0.066(3) 0.061(3) 0.017(3) 0.016(3) 0.013(3) N2 0.084(4) 0.069(3) 0.062(3) 0.019(3) 0.023(3) 0.024(3) N3 0.085(4) 0.071(4) 0.057(3) 0.006(3) 0.015(3) 0.014(3) N4 0.088(4) 0.069(3) 0.055(3) 0.010(3) 0.019(3) 0.019(3) C1 0.076(5) 0.071(4) 0.064(4) 0.002(3) 0.020(3) 0.017(3) C2 0.079(5) 0.064(4) 0.063(4) 0.009(3) 0.018(3) 0.017(3) C3 0.072(5) 0.075(5) 0.064(4) 0.012(4) 0.014(3) 0.011(3) C4 0.083(5) 0.070(4) 0.065(4) 0.009(4) 0.017(4) 0.008(4) C5 0.098(6) 0.092(5) 0.062(4) 0.015(4) 0.015(4) 0.010(4) C6 0.098(5) 0.065(4) 0.062(4) 0.013(4) 0.017(4) 0.026(4) C7 0.089(5) 0.091(5) 0.063(5) 0.012(4) 0.018(4) 0.013(4) C8 0.109(6) 0.079(5) 0.071(5) 0.019(4) 0.036(4) 0.035(4) C9 0.080(5) 0.087(5) 0.050(4) 0.018(4) 0.016(3) 0.006(4) C10 0.086(5) 0.081(5) 0.059(4) 0.025(4) 0.016(4) 0.011(4) C11 0.081(5) 0.068(4) 0.063(4) 0.018(4) 0.021(3) 0.016(3) C12 0.091(5) 0.075(5) 0.067(4) 0.030(4) 0.015(4) 0.025(4) C13 0.083(5) 0.078(5) 0.066(5) 0.019(4) 0.010(4) 0.006(4) C14 0.109(6) 0.063(4) 0.071(5) 0.017(4) 0.024(4) 0.023(4) C15 0.066(4) 0.083(5) 0.061(4) 0.016(4) 0.015(3) 0.019(3) C16 0.077(5) 0.086(5) 0.059(4) 0.016(4) 0.018(3) 0.018(4) C17 0.098(6) 0.073(5) 0.069(5) 0.016(4) 0.029(4) 0.015(4) C18 0.103(6) 0.077(5) 0.055(4) 0.000(4) 0.018(4) 0.016(4) C19 0.075(5) 0.076(5) 0.068(4) 0.012(4) 0.026(4) 0.012(4) C20 0.082(5) 0.069(4) 0.061(4) 0.007(4) 0.015(4) 0.008(4) C21 0.112(6) 0.093(5) 0.051(4) 0.008(4) 0.011(4) 0.018(4) C22 0.082(5) 0.073(4) 0.056(4) 0.018(4) 0.012(3) 0.007(3) C23 0.104(6) 0.108(6) 0.050(4) 0.019(4) 0.020(4) 0.030(5) C24 0.094(5) 0.073(5) 0.070(5) 0.026(4) 0.019(4) 0.021(4) C25 0.080(5) 0.076(5) 0.068(4) 0.011(4) 0.014(4) 0.013(4) C26 0.098(6) 0.081(5) 0.069(5) 0.013(4) 0.026(4) 0.017(4) C27 0.087(5) 0.075(5) 0.062(4) 0.005(4) 0.013(4) 0.007(4) C28 0.124(7) 0.089(5) 0.053(4) 0.010(4) 0.028(4) 0.032(5) C29 0.109(6) 0.081(5) 0.069(5) 0.013(4) 0.023(4) 0.021(4) C30 0.105(6) 0.093(5) 0.064(5) 0.015(4) 0.012(4) 0.025(4) C31 0.116(6) 0.067(5) 0.065(4) 0.016(4) 0.019(4) 0.013(4) C32 0.134(8) 0.108(7) 0.064(5) 0.034(5) 0.002(5) 0.004(6) C33 0.111(6) 0.081(5) 0.069(5) 0.010(4) 0.019(4) 0.021(4) C34 0.119(7) 0.114(7) 0.054(5) 0.016(4) 0.014(4) -0.008(5) C35 0.109(6) 0.101(6) 0.076(5) 0.034(5) 0.006(5) 0.012(5) C36 0.114(6) 0.101(6) 0.087(5) 0.022(5) 0.031(5) 0.035(5) C37 0.199(11) 0.109(7) 0.161(9) 0.020(6) 0.106(8) 0.061(7) C38 0.117(7) 0.087(5) 0.083(5) 0.005(5) -0.005(5) 0.028(5) C39 0.134(8) 0.160(10) 0.066(6) 0.004(6) 0.007(5) 0.024(7) C40 0.166(10) 0.110(7) 0.122(8) 0.042(6) 0.039(8) 0.040(6) C41 0.175(11) 0.186(11) 0.197(12) 0.115(10) 0.076(10) 0.061(9) C43 0.201(11) 0.101(6) 0.105(7) 0.049(6) 0.068(8) 0.069(7) C44 0.157(9) 0.132(7) 0.098(6) 0.044(6) 0.038(6) 0.045(6) C45 0.139(9) 0.167(11) 0.098(8) 0.057(8) 0.031(7) 0.035(8) C46 0.135(8) 0.139(8) 0.062(5) 0.023(5) 0.021(5) 0.029(6) C47 0.148(9) 0.158(9) 0.130(8) 0.065(7) -0.010(7) 0.044(7) C48 0.276(15) 0.116(8) 0.092(7) 0.058(6) 0.024(8) 0.009(8) C49 0.095(6) 0.135(8) 0.126(7) -0.042(6) 0.003(5) 0.013(5) C50 0.214(13) 0.191(12) 0.150(10) 0.064(9) -0.065(9) 0.063(10) C51 0.176(11) 0.204(12) 0.112(8) 0.061(8) -0.003(8) 0.061(9) C52 0.173(11) 0.160(10) 0.208(12) 0.070(9) 0.107(9) 0.012(8) C53 0.242(14) 0.127(9) 0.119(9) 0.065(8) 0.012(9) -0.013(9) C54 0.087(13) 0.19(2) 0.088(13) -0.004(13) -0.029(10) 0.021(13) C55 0.151(11) 0.124(9) 0.140(9) -0.030(7) -0.002(8) 0.007(7) C56 0.306(18) 0.129(9) 0.150(10) 0.057(8) 0.094(11) 0.014(10) O1 0.068(3) 0.098(3) 0.083(3) 0.023(3) 0.017(3) 0.000(2) C58 0.099(6) 0.111(7) 0.105(6) 0.005(5) 0.000(5) 0.014(5) C59 0.074(5) 0.113(7) 0.145(8) -0.020(6) 0.044(5) 0.016(5) C60 0.089(7) 0.136(8) 0.200(10) -0.033(8) 0.041(7) 0.031(6) O2 0.148(7) 0.263(10) 0.094(5) 0.005(6) 0.035(4) -0.072(6) C61 0.127(9) 0.186(11) 0.122(9) 0.008(8) 0.046(7) -0.018(8) C62 0.271(18) 0.168(13) 0.243(16) -0.092(12) -0.006(13) -0.028(12) _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 Si1 C25 1.841(7) . ? Si1 C38 1.875(8) . ? Si1 C40 1.877(9) . ? Si1 C59 1.884(7) . ? Mg1 O1 2.032(5) . ? Mg1 N2 2.054(5) . ? Mg1 N3 2.067(6) . ? Mg1 N1 2.074(6) . ? Mg1 N4 2.078(6) . ? Si2 C31 1.821(8) . ? Si2 C55 1.873(11) . ? Si2 C43 1.889(8) . ? Si2 C36 1.889(8) . ? N1 C15 1.364(8) . ? N1 C20 1.368(8) . ? N2 C22 1.369(7) . ? N2 C19 1.371(8) . ? N3 C3 1.369(8) . ? N3 C11 1.379(7) . ? N4 C16 1.354(7) . ? N4 C2 1.357(7) . ? C1 C2 1.408(8) . ? C1 C15 1.424(9) . ? C1 C27 1.457(9) . ? C2 C6 1.434(8) . ? C3 C9 1.414(8) . ? C3 C24 1.430(8) . ? C4 C7 1.210(9) . ? C4 C9 1.440(9) . ? C5 C18 1.354(9) . ? C5 C20 1.432(8) . ? C6 C12 1.346(8) . ? C7 C13 1.444(9) . ? C8 C29 1.200(9) . ? C8 C10 1.435(9) . ? C9 C20 1.410(9) . ? C10 C22 1.417(9) . ? C10 C16 1.427(8) . ? C11 C17 1.395(8) . ? C11 C14 1.436(8) . ? C12 C16 1.439(8) . ? C13 C30 1.374(9) . ? C13 C33 1.407(9) . ? C14 C24 1.326(8) . ? C15 C18 1.441(8) . ? C17 C19 1.426(9) . ? C17 C26 1.459(9) . ? C19 C28 1.460(9) . ? C21 C28 1.353(9) . ? C21 C22 1.430(8) . ? C23 C48 1.332(11) . ? C23 C46 1.393(10) . ? C23 C29 1.441(10) . ? C25 C27 1.202(8) . ? C26 C31 1.194(9) . ? C30 C35 1.361(9) . ? C32 C35 1.358(10) . ? C32 C34 1.372(10) . ? C33 C34 1.376(9) . ? C36 C37 1.518(10) . ? C36 C44 1.534(10) . ? C38 C47 1.485(10) . ? C38 C49 1.524(10) . ? C39 C45 1.362(13) . ? C39 C46 1.378(10) . ? C40 C41 1.483(12) . ? C40 C50 1.573(13) . ? C43 C51 1.553(13) . ? C43 C56 1.555(13) . ? C45 C53 1.347(13) . ? C48 C53 1.414(12) . ? C52 C59 1.560(12) . ? C54 C55 1.466(18) . ? C55 C62 1.506(15) . ? O1 C58 1.437(8) . ? C59 C60 1.561(11) . ? O2 C61 1.368(10) . ? 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 Si1 C38 106.2(3) . . ? C25 Si1 C40 109.3(4) . . ? C38 Si1 C40 110.4(4) . . ? C25 Si1 C59 106.4(3) . . ? C38 Si1 C59 114.6(4) . . ? C40 Si1 C59 109.7(5) . . ? O1 Mg1 N2 97.0(2) . . ? O1 Mg1 N3 102.0(2) . . ? N2 Mg1 N3 89.2(2) . . ? O1 Mg1 N1 102.4(2) . . ? N2 Mg1 N1 160.5(2) . . ? N3 Mg1 N1 87.5(2) . . ? O1 Mg1 N4 99.1(2) . . ? N2 Mg1 N4 87.8(2) . . ? N3 Mg1 N4 158.9(2) . . ? N1 Mg1 N4 88.4(2) . . ? C31 Si2 C55 108.2(5) . . ? C31 Si2 C43 105.9(4) . . ? C55 Si2 C43 116.5(6) . . ? C31 Si2 C36 106.1(3) . . ? C55 Si2 C36 110.8(5) . . ? C43 Si2 C36 108.7(4) . . ? C15 N1 C20 104.9(5) . . ? C15 N1 Mg1 126.8(4) . . ? C20 N1 Mg1 127.0(4) . . ? C22 N2 C19 104.6(5) . . ? C22 N2 Mg1 127.8(4) . . ? C19 N2 Mg1 126.4(4) . . ? C3 N3 C11 104.5(5) . . ? C3 N3 Mg1 128.5(4) . . ? C11 N3 Mg1 126.4(4) . . ? C16 N4 C2 105.4(5) . . ? C16 N4 Mg1 127.7(4) . . ? C2 N4 Mg1 126.6(4) . . ? C2 C1 C15 126.4(6) . . ? C2 C1 C27 118.5(6) . . ? C15 C1 C27 115.1(6) . . ? N4 C2 C1 125.4(6) . . ? N4 C2 C6 110.8(5) . . ? C1 C2 C6 123.8(6) . . ? N3 C3 C9 123.1(6) . . ? N3 C3 C24 110.6(6) . . ? C9 C3 C24 126.2(7) . . ? C7 C4 C9 178.6(8) . . ? C18 C5 C20 107.8(6) . . ? C12 C6 C2 106.7(6) . . ? C4 C7 C13 178.1(8) . . ? C29 C8 C10 176.1(7) . . ? C20 C9 C3 126.8(6) . . ? C20 C9 C4 115.8(6) . . ? C3 C9 C4 117.4(6) . . ? C22 C10 C16 126.1(6) . . ? C22 C10 C8 115.7(6) . . ? C16 C10 C8 118.3(6) . . ? N3 C11 C17 124.8(6) . . ? N3 C11 C14 110.5(6) . . ? C17 C11 C14 124.7(6) . . ? C6 C12 C16 106.0(6) . . ? C30 C13 C33 119.0(7) . . ? C30 C13 C7 121.6(7) . . ? C33 C13 C7 119.3(7) . . ? C24 C14 C11 106.8(6) . . ? N1 C15 C1 123.6(6) . . ? N1 C15 C18 111.8(6) . . ? C1 C15 C18 124.3(6) . . ? N4 C16 C10 124.2(6) . . ? N4 C16 C12 111.1(6) . . ? C10 C16 C12 124.7(6) . . ? C11 C17 C19 126.3(6) . . ? C11 C17 C26 118.5(6) . . ? C19 C17 C26 115.1(6) . . ? C5 C18 C15 105.0(6) . . ? N2 C19 C17 124.6(6) . . ? N2 C19 C28 110.8(6) . . ? C17 C19 C28 124.5(6) . . ? N1 C20 C9 124.4(6) . . ? N1 C20 C5 110.4(6) . . ? C9 C20 C5 125.2(7) . . ? C28 C21 C22 107.0(6) . . ? N2 C22 C10 123.4(6) . . ? N2 C22 C21 111.7(6) . . ? C10 C22 C21 124.7(6) . . ? C48 C23 C46 119.7(8) . . ? C48 C23 C29 122.1(8) . . ? C46 C23 C29 118.1(8) . . ? C14 C24 C3 107.6(6) . . ? C27 C25 Si1 175.3(6) . . ? C31 C26 C17 177.5(9) . . ? C25 C27 C1 178.9(8) . . ? C21 C28 C19 105.8(6) . . ? C8 C29 C23 177.3(8) . . ? C35 C30 C13 120.7(7) . . ? C26 C31 Si2 175.9(7) . . ? C35 C32 C34 118.8(8) . . ? C34 C33 C13 118.3(7) . . ? C32 C34 C33 121.9(8) . . ? C32 C35 C30 121.2(8) . . ? C37 C36 C44 110.7(7) . . ? C37 C36 Si2 114.4(6) . . ? C44 C36 Si2 114.3(6) . . ? C47 C38 C49 111.0(7) . . ? C47 C38 Si1 117.2(6) . . ? C49 C38 Si1 113.0(5) . . ? C45 C39 C46 117.3(10) . . ? C41 C40 C50 109.0(9) . . ? C41 C40 Si1 112.0(7) . . ? C50 C40 Si1 111.5(8) . . ? C51 C43 C56 110.5(8) . . ? C51 C43 Si2 112.9(7) . . ? C56 C43 Si2 109.6(7) . . ? C53 C45 C39 124.3(10) . . ? C39 C46 C23 120.7(9) . . ? C23 C48 C53 121.1(10) . . ? C45 C53 C48 116.9(10) . . ? C54 C55 C62 121.1(12) . . ? C54 C55 Si2 117.5(9) . . ? C62 C55 Si2 113.7(10) . . ? C58 O1 Mg1 125.9(5) . . ? C52 C59 C60 110.8(8) . . ? C52 C59 Si1 111.9(6) . . ? C60 C59 Si1 111.6(6) . . ? 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 O1 Mg1 N1 C15 -80.8(5) . . . . ? N2 Mg1 N1 C15 96.9(8) . . . . ? N3 Mg1 N1 C15 177.4(5) . . . . ? N4 Mg1 N1 C15 18.2(5) . . . . ? O1 Mg1 N1 C20 84.6(5) . . . . ? N2 Mg1 N1 C20 -97.6(8) . . . . ? N3 Mg1 N1 C20 -17.1(5) . . . . ? N4 Mg1 N1 C20 -176.4(5) . . . . ? O1 Mg1 N2 C22 79.9(5) . . . . ? N3 Mg1 N2 C22 -178.1(5) . . . . ? N1 Mg1 N2 C22 -97.9(8) . . . . ? N4 Mg1 N2 C22 -19.0(5) . . . . ? O1 Mg1 N2 C19 -86.1(5) . . . . ? N3 Mg1 N2 C19 15.9(5) . . . . ? N1 Mg1 N2 C19 96.1(8) . . . . ? N4 Mg1 N2 C19 175.0(5) . . . . ? O1 Mg1 N3 C3 -86.5(6) . . . . ? N2 Mg1 N3 C3 176.5(6) . . . . ? N1 Mg1 N3 C3 15.7(6) . . . . ? N4 Mg1 N3 C3 94.9(8) . . . . ? O1 Mg1 N3 C11 82.9(5) . . . . ? N2 Mg1 N3 C11 -14.1(5) . . . . ? N1 Mg1 N3 C11 -174.9(5) . . . . ? N4 Mg1 N3 C11 -95.7(8) . . . . ? O1 Mg1 N4 C16 -83.6(5) . . . . ? N2 Mg1 N4 C16 13.1(6) . . . . ? N3 Mg1 N4 C16 95.0(8) . . . . ? N1 Mg1 N4 C16 174.0(5) . . . . ? O1 Mg1 N4 C2 89.2(5) . . . . ? N2 Mg1 N4 C2 -174.0(5) . . . . ? N3 Mg1 N4 C2 -92.1(8) . . . . ? N1 Mg1 N4 C2 -13.1(5) . . . . ? C16 N4 C2 C1 -179.1(6) . . . . ? Mg1 N4 C2 C1 6.7(9) . . . . ? C16 N4 C2 C6 -0.5(7) . . . . ? Mg1 N4 C2 C6 -174.6(4) . . . . ? C15 C1 C2 N4 1.3(11) . . . . ? C27 C1 C2 N4 179.7(6) . . . . ? C15 C1 C2 C6 -177.2(6) . . . . ? C27 C1 C2 C6 1.2(10) . . . . ? C11 N3 C3 C9 178.8(6) . . . . ? Mg1 N3 C3 C9 -10.0(9) . . . . ? C11 N3 C3 C24 1.5(7) . . . . ? Mg1 N3 C3 C24 172.8(4) . . . . ? N4 C2 C6 C12 1.2(8) . . . . ? C1 C2 C6 C12 179.9(6) . . . . ? C9 C4 C7 C13 131(29) . . . . ? N3 C3 C9 C20 -1.3(11) . . . . ? C24 C3 C9 C20 175.5(7) . . . . ? N3 C3 C9 C4 178.3(6) . . . . ? C24 C3 C9 C4 -4.9(10) . . . . ? C7 C4 C9 C20 -38(32) . . . . ? C7 C4 C9 C3 142(31) . . . . ? C29 C8 C10 C22 -27(13) . . . . ? C29 C8 C10 C16 155(12) . . . . ? C3 N3 C11 C17 -179.6(6) . . . . ? Mg1 N3 C11 C17 9.0(9) . . . . ? C3 N3 C11 C14 -1.7(7) . . . . ? Mg1 N3 C11 C14 -173.2(4) . . . . ? C2 C6 C12 C16 -1.4(7) . . . . ? C4 C7 C13 C30 97(24) . . . . ? C4 C7 C13 C33 -83(24) . . . . ? N3 C11 C14 C24 1.3(8) . . . . ? C17 C11 C14 C24 179.1(7) . . . . ? C20 N1 C15 C1 174.9(6) . . . . ? Mg1 N1 C15 C1 -17.0(9) . . . . ? C20 N1 C15 C18 0.3(7) . . . . ? Mg1 N1 C15 C18 168.4(4) . . . . ? C2 C1 C15 N1 4.2(11) . . . . ? C27 C1 C15 N1 -174.3(6) . . . . ? C2 C1 C15 C18 178.1(7) . . . . ? C27 C1 C15 C18 -0.4(9) . . . . ? C2 N4 C16 C10 -179.2(6) . . . . ? Mg1 N4 C16 C10 -5.2(9) . . . . ? C2 N4 C16 C12 -0.4(7) . . . . ? Mg1 N4 C16 C12 173.6(4) . . . . ? C22 C10 C16 N4 -4.0(11) . . . . ? C8 C10 C16 N4 174.6(6) . . . . ? C22 C10 C16 C12 177.3(6) . . . . ? C8 C10 C16 C12 -4.0(10) . . . . ? C6 C12 C16 N4 1.2(8) . . . . ? C6 C12 C16 C10 180.0(6) . . . . ? N3 C11 C17 C19 0.6(11) . . . . ? C14 C11 C17 C19 -177.0(7) . . . . ? N3 C11 C17 C26 177.6(6) . . . . ? C14 C11 C17 C26 0.0(10) . . . . ? C20 C5 C18 C15 0.9(8) . . . . ? N1 C15 C18 C5 -0.8(8) . . . . ? C1 C15 C18 C5 -175.4(7) . . . . ? C22 N2 C19 C17 178.5(6) . . . . ? Mg1 N2 C19 C17 -12.8(9) . . . . ? C22 N2 C19 C28 -1.5(7) . . . . ? Mg1 N2 C19 C28 167.1(5) . . . . ? C11 C17 C19 N2 1.4(11) . . . . ? C26 C17 C19 N2 -175.6(6) . . . . ? C11 C17 C19 C28 -178.5(7) . . . . ? C26 C17 C19 C28 4.4(10) . . . . ? C15 N1 C20 C9 -178.6(6) . . . . ? Mg1 N1 C20 C9 13.4(9) . . . . ? C15 N1 C20 C5 0.2(7) . . . . ? Mg1 N1 C20 C5 -167.8(4) . . . . ? C3 C9 C20 N1 -0.6(11) . . . . ? C4 C9 C20 N1 179.7(6) . . . . ? C3 C9 C20 C5 -179.3(6) . . . . ? C4 C9 C20 C5 1.1(10) . . . . ? C18 C5 C20 N1 -0.8(8) . . . . ? C18 C5 C20 C9 178.0(7) . . . . ? C19 N2 C22 C10 -174.4(6) . . . . ? Mg1 N2 C22 C10 17.2(9) . . . . ? C19 N2 C22 C21 1.1(7) . . . . ? Mg1 N2 C22 C21 -167.3(5) . . . . ? C16 C10 C22 N2 -2.1(11) . . . . ? C8 C10 C22 N2 179.2(6) . . . . ? C16 C10 C22 C21 -177.1(6) . . . . ? C8 C10 C22 C21 4.2(10) . . . . ? C28 C21 C22 N2 -0.3(8) . . . . ? C28 C21 C22 C10 175.2(7) . . . . ? C11 C14 C24 C3 -0.3(8) . . . . ? N3 C3 C24 C14 -0.8(8) . . . . ? C9 C3 C24 C14 -177.9(6) . . . . ? C38 Si1 C25 C27 28(8) . . . . ? C40 Si1 C25 C27 147(8) . . . . ? C59 Si1 C25 C27 -94(8) . . . . ? C11 C17 C26 C31 -70(17) . . . . ? C19 C17 C26 C31 108(17) . . . . ? Si1 C25 C27 C1 0(48) . . . . ? C2 C1 C27 C25 -155(42) . . . . ? C15 C1 C27 C25 23(42) . . . . ? C22 C21 C28 C19 -0.6(8) . . . . ? N2 C19 C28 C21 1.4(8) . . . . ? C17 C19 C28 C21 -178.7(7) . . . . ? C10 C8 C29 C23 42(26) . . . . ? C48 C23 C29 C8 -173(17) . . . . ? C46 C23 C29 C8 5(17) . . . . ? C33 C13 C30 C35 0.1(11) . . . . ? C7 C13 C30 C35 -179.4(7) . . . . ? C17 C26 C31 Si2 -51(24) . . . . ? C55 Si2 C31 C26 -111(10) . . . . ? C43 Si2 C31 C26 123(10) . . . . ? C36 Si2 C31 C26 8(10) . . . . ? C30 C13 C33 C34 -0.1(11) . . . . ? C7 C13 C33 C34 179.4(7) . . . . ? C35 C32 C34 C33 1.6(13) . . . . ? C13 C33 C34 C32 -0.7(12) . . . . ? C34 C32 C35 C30 -1.6(13) . . . . ? C13 C30 C35 C32 0.8(12) . . . . ? C31 Si2 C36 C37 173.5(7) . . . . ? C55 Si2 C36 C37 -69.2(8) . . . . ? C43 Si2 C36 C37 60.0(8) . . . . ? C31 Si2 C36 C44 -57.4(7) . . . . ? C55 Si2 C36 C44 59.9(7) . . . . ? C43 Si2 C36 C44 -170.9(6) . . . . ? C25 Si1 C38 C47 -49.8(7) . . . . ? C40 Si1 C38 C47 -168.2(7) . . . . ? C59 Si1 C38 C47 67.3(8) . . . . ? C25 Si1 C38 C49 179.1(6) . . . . ? C40 Si1 C38 C49 60.7(7) . . . . ? C59 Si1 C38 C49 -63.7(7) . . . . ? C25 Si1 C40 C41 -60.7(9) . . . . ? C38 Si1 C40 C41 55.8(9) . . . . ? C59 Si1 C40 C41 -177.0(8) . . . . ? C25 Si1 C40 C50 61.7(8) . . . . ? C38 Si1 C40 C50 178.2(7) . . . . ? C59 Si1 C40 C50 -54.6(8) . . . . ? C31 Si2 C43 C51 -59.7(8) . . . . ? C55 Si2 C43 C51 179.9(7) . . . . ? C36 Si2 C43 C51 54.0(8) . . . . ? C31 Si2 C43 C56 64.0(8) . . . . ? C55 Si2 C43 C56 -56.4(9) . . . . ? C36 Si2 C43 C56 177.7(7) . . . . ? C46 C39 C45 C53 -2.2(17) . . . . ? C45 C39 C46 C23 0.3(14) . . . . ? C48 C23 C46 C39 0.2(14) . . . . ? C29 C23 C46 C39 -178.5(8) . . . . ? C46 C23 C48 C53 1.1(17) . . . . ? C29 C23 C48 C53 179.7(10) . . . . ? C39 C45 C53 C48 3.4(19) . . . . ? C23 C48 C53 C45 -2.8(19) . . . . ? C31 Si2 C55 C54 46.3(13) . . . . ? C43 Si2 C55 C54 165.4(11) . . . . ? C36 Si2 C55 C54 -69.7(12) . . . . ? C31 Si2 C55 C62 -164.0(10) . . . . ? C43 Si2 C55 C62 -44.9(13) . . . . ? C36 Si2 C55 C62 80.0(12) . . . . ? N2 Mg1 O1 C58 -45.3(6) . . . . ? N3 Mg1 O1 C58 -136.0(5) . . . . ? N1 Mg1 O1 C58 133.9(5) . . . . ? N4 Mg1 O1 C58 43.5(6) . . . . ? C25 Si1 C59 C52 62.4(7) . . . . ? C38 Si1 C59 C52 -54.7(8) . . . . ? C40 Si1 C59 C52 -179.5(7) . . . . ? C25 Si1 C59 C60 -172.8(7) . . . . ? C38 Si1 C59 C60 70.1(8) . . . . ? C40 Si1 C59 C60 -54.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 66.99 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.700 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.095