Supplementary Information (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_rem157 _database_code_CSD 151831 _journal_coden_Cambridge 186 _publ_requested_journal 'J.Chem.Soc.,Dalton Trans.' loop_ _publ_author_name 'Armstrong, David R.' 'Clegg, W.' 'Mulvey, R. E.' 'Rowlings, Rene B.' _publ_contact_author_name 'Dr Rene B Rowlings' _publ_contact_author_address ; Dr Rene B Rowlings Department of Pure & Applied Chemistry University of Strathclyde Glasgow G1 1XL UNITED KINGDOM ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H64 Mg2 N4 O2 Si4' _chemical_formula_weight 697.85 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9338(4) _cell_length_b 21.3111(10) _cell_length_c 10.8059(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.616(2) _cell_angle_gamma 90.00 _cell_volume 2047.45(16) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 11358 _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method ? _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14245 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.45 _reflns_number_total 4728 _reflns_number_observed 4204 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.6762P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4728 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_obs 0.0299 _refine_ls_wR_factor_all 0.0803 _refine_ls_wR_factor_obs 0.0770 _refine_ls_goodness_of_fit_all 1.091 _refine_ls_goodness_of_fit_obs 1.112 _refine_ls_restrained_S_all 1.091 _refine_ls_restrained_S_obs 1.112 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mg Mg 0.39704(4) 0.531041(18) 0.40005(3) 0.01953(10) Uani 1 d . . N1 N 0.62404(11) 0.49761(5) 0.41633(9) 0.0209(2) Uani 1 d . . H1 H 0.6910 0.5310 0.4153 0.025 Uiso 1 calc R . C1 C 0.65659(13) 0.45137(6) 0.32897(10) 0.0210(2) Uani 1 d . . C2 C 0.74990(14) 0.46255(6) 0.23438(11) 0.0262(3) Uani 1 d . . H2 H 0.7983 0.5021 0.2300 0.031 Uiso 1 calc R . C3 C 0.77270(17) 0.41668(7) 0.14693(12) 0.0351(3) Uani 1 d . . H3 H 0.8350 0.4255 0.0827 0.042 Uiso 1 calc R . C4 C 0.70618(19) 0.35844(7) 0.15191(13) 0.0395(4) Uani 1 d . . H4 H 0.7215 0.3274 0.0914 0.047 Uiso 1 calc R . C5 C 0.61662(18) 0.34607(7) 0.24660(13) 0.0360(3) Uani 1 d . . H5 H 0.5714 0.3059 0.2518 0.043 Uiso 1 calc R . C6 C 0.59227(15) 0.39169(6) 0.33407(12) 0.0274(3) Uani 1 d . . H6 H 0.5308 0.3822 0.3986 0.033 Uiso 1 calc R . O1 O 0.29358(10) 0.47104(4) 0.27385(7) 0.02504(19) Uani 1 d . . C7 C 0.31329(15) 0.48472(6) 0.14375(11) 0.0282(3) Uani 1 d . . H7A H 0.4118 0.4693 0.1218 0.034 Uiso 1 calc R . H7B H 0.3064 0.5304 0.1273 0.034 Uiso 1 calc R . C8 C 0.18594(16) 0.45012(6) 0.07159(12) 0.0299(3) Uani 1 d . . H8A H 0.2093 0.4408 -0.0142 0.036 Uiso 1 calc R . H8B H 0.0909 0.4743 0.0684 0.036 Uiso 1 calc R . C9 C 0.17747(16) 0.39055(6) 0.14780(13) 0.0312(3) Uani 1 d . . H9A H 0.0781 0.3701 0.1313 0.037 Uiso 1 calc R . H9B H 0.2570 0.3604 0.1301 0.037 Uiso 1 calc R . C10 C 0.20166(16) 0.41444(6) 0.28001(12) 0.0306(3) Uani 1 d . . H10A H 0.1043 0.4245 0.3120 0.037 Uiso 1 calc R . H10B H 0.2546 0.3827 0.3351 0.037 Uiso 1 calc R . N2 N 0.34636(11) 0.61707(5) 0.33393(9) 0.0209(2) Uani 1 d . . Si1 Si 0.48069(4) 0.663512(15) 0.27931(3) 0.02278(9) Uani 1 d . . C11 C 0.57566(17) 0.62358(7) 0.15309(14) 0.0345(3) Uani 1 d . . H11A H 0.6585 0.6498 0.1298 0.052 Uiso 1 calc R . H11B H 0.5027 0.6172 0.0804 0.052 Uiso 1 calc R . H11C H 0.6153 0.5829 0.1833 0.052 Uiso 1 calc R . C12 C 0.63434(19) 0.68327(8) 0.40484(14) 0.0437(4) Uani 1 d . . H12A H 0.7136 0.7069 0.3688 0.066 Uiso 1 calc R . H12B H 0.6766 0.6445 0.4423 0.066 Uiso 1 calc R . H12C H 0.5929 0.7088 0.4688 0.066 Uiso 1 calc R . C13 C 0.41116(19) 0.74021(7) 0.21022(15) 0.0405(4) Uani 1 d . . H13A H 0.3557 0.7628 0.2703 0.061 Uiso 1 calc R . H13B H 0.3445 0.7323 0.1343 0.061 Uiso 1 calc R . H13C H 0.4970 0.7656 0.1900 0.061 Uiso 1 calc R . Si2 Si 0.16429(4) 0.639313(16) 0.34038(3) 0.02354(9) Uani 1 d . . C14 C 0.05978(18) 0.65245(9) 0.18239(14) 0.0460(4) Uani 1 d . . H14A H -0.0450 0.6635 0.1920 0.069 Uiso 1 calc R . H14B H 0.0625 0.6140 0.1329 0.069 Uiso 1 calc R . H14C H 0.1074 0.6867 0.1401 0.069 Uiso 1 calc R . C15 C 0.05557(16) 0.57618(7) 0.41420(15) 0.0383(3) Uani 1 d . . H15A H 0.1020 0.5680 0.4986 0.057 Uiso 1 calc R . H15B H 0.0567 0.5377 0.3646 0.057 Uiso 1 calc R . H15C H -0.0485 0.5900 0.4178 0.057 Uiso 1 calc R . C16 C 0.13945(18) 0.71109(7) 0.43641(15) 0.0410(3) Uani 1 d . . H16A H 0.1877 0.7045 0.5208 0.061 Uiso 1 calc R . H16B H 0.0319 0.7191 0.4398 0.061 Uiso 1 calc R . H16C H 0.1858 0.7472 0.3988 0.061 Uiso 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 Mg 0.0237(2) 0.01709(19) 0.01772(19) -0.00002(14) 0.00161(15) 0.00115(15) N1 0.0243(5) 0.0185(5) 0.0201(5) -0.0009(4) 0.0042(4) -0.0007(4) C1 0.0214(6) 0.0234(6) 0.0178(5) 0.0009(4) -0.0007(4) 0.0048(4) C2 0.0243(6) 0.0301(7) 0.0244(6) 0.0020(5) 0.0040(5) 0.0052(5) C3 0.0367(8) 0.0447(8) 0.0248(6) -0.0005(6) 0.0080(5) 0.0149(6) C4 0.0528(9) 0.0367(8) 0.0281(7) -0.0107(6) -0.0004(6) 0.0163(7) C5 0.0489(9) 0.0242(7) 0.0333(7) -0.0057(5) -0.0050(6) 0.0034(6) C6 0.0335(7) 0.0241(6) 0.0243(6) -0.0001(5) 0.0012(5) 0.0006(5) O1 0.0322(5) 0.0232(4) 0.0193(4) -0.0006(3) 0.0010(3) -0.0060(4) C7 0.0350(7) 0.0301(7) 0.0198(6) 0.0004(5) 0.0038(5) -0.0046(5) C8 0.0354(7) 0.0291(7) 0.0242(6) -0.0014(5) -0.0028(5) -0.0005(5) C9 0.0357(7) 0.0222(6) 0.0341(7) -0.0036(5) -0.0041(5) -0.0009(5) C10 0.0362(7) 0.0261(6) 0.0292(6) 0.0032(5) 0.0007(5) -0.0086(5) N2 0.0233(5) 0.0177(5) 0.0222(5) 0.0010(4) 0.0040(4) 0.0014(4) Si1 0.02662(18) 0.01925(17) 0.02298(16) 0.00166(12) 0.00507(13) -0.00118(13) C11 0.0358(7) 0.0327(7) 0.0373(7) 0.0032(6) 0.0161(6) 0.0041(6) C12 0.0453(9) 0.0477(9) 0.0369(8) 0.0031(7) -0.0015(6) -0.0222(7) C13 0.0514(9) 0.0252(7) 0.0480(8) 0.0104(6) 0.0211(7) 0.0055(6) Si2 0.02246(17) 0.02374(17) 0.02455(17) 0.00120(13) 0.00298(12) 0.00391(13) C14 0.0346(8) 0.0669(11) 0.0347(8) 0.0065(7) -0.0055(6) 0.0071(7) C15 0.0244(7) 0.0389(8) 0.0526(9) 0.0081(7) 0.0088(6) -0.0003(6) C16 0.0418(8) 0.0344(8) 0.0487(9) -0.0066(7) 0.0149(7) 0.0091(6) _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 Mg N2 2.0034(11) . ? Mg O1 2.0255(9) . ? Mg N1 2.1020(10) 3_666 ? Mg N1 2.1404(11) . ? N1 C1 1.4144(15) . ? N1 Mg 2.1020(10) 3_666 ? C1 C6 1.3990(18) . ? C1 C2 1.4012(17) . ? C2 C3 1.3885(19) . ? C3 C4 1.379(2) . ? C4 C5 1.385(2) . ? C5 C6 1.3877(18) . ? O1 C7 1.4632(14) . ? O1 C10 1.4642(15) . ? C7 C8 1.5074(18) . ? C8 C9 1.5193(18) . ? C9 C10 1.5122(18) . ? N2 Si2 1.7022(10) . ? N2 Si1 1.7049(10) . ? Si1 C13 1.8772(15) . ? Si1 C11 1.8791(14) . ? Si1 C12 1.8808(15) . ? Si2 C16 1.8738(15) . ? Si2 C15 1.8819(15) . ? Si2 C14 1.8849(15) . ? 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 N2 Mg O1 105.39(4) . . ? N2 Mg N1 124.37(4) . 3_666 ? O1 Mg N1 112.03(4) . 3_666 ? N2 Mg N1 120.88(4) . . ? O1 Mg N1 102.21(4) . . ? N1 Mg N1 89.85(4) 3_666 . ? C1 N1 Mg 118.10(7) . 3_666 ? C1 N1 Mg 115.60(7) . . ? Mg N1 Mg 90.15(4) 3_666 . ? C6 C1 C2 117.34(11) . . ? C6 C1 N1 119.68(11) . . ? C2 C1 N1 122.97(11) . . ? C3 C2 C1 120.94(13) . . ? C4 C3 C2 120.96(13) . . ? C3 C4 C5 118.85(13) . . ? C4 C5 C6 120.69(14) . . ? C5 C6 C1 121.18(13) . . ? C7 O1 C10 109.18(9) . . ? C7 O1 Mg 115.54(7) . . ? C10 O1 Mg 135.27(7) . . ? O1 C7 C8 104.11(10) . . ? C7 C8 C9 101.74(10) . . ? C10 C9 C8 102.74(10) . . ? O1 C10 C9 105.27(10) . . ? Si2 N2 Si1 124.08(6) . . ? Si2 N2 Mg 115.07(5) . . ? Si1 N2 Mg 120.83(6) . . ? N2 Si1 C13 115.24(6) . . ? N2 Si1 C11 111.81(6) . . ? C13 Si1 C11 105.13(7) . . ? N2 Si1 C12 111.66(6) . . ? C13 Si1 C12 106.36(8) . . ? C11 Si1 C12 105.98(8) . . ? N2 Si2 C16 114.55(6) . . ? N2 Si2 C15 110.68(6) . . ? C16 Si2 C15 104.77(7) . . ? N2 Si2 C14 113.26(6) . . ? C16 Si2 C14 107.78(8) . . ? C15 Si2 C14 105.05(8) . . ? _refine_diff_density_max 0.319 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.040 #===END # ----------------------------------------------------------------- # Prof. W. Clegg, Department of Chemistry, University of Newcastle, # Newcastle upon Tyne NE1 7RU, U.K. # Tel. (44)191 222 6649 or 6641, fax. (44)191 222 6929, w.clegg@ncl.ac.uk # Also part-time at Daresbury Laboratory, Daresbury, Warrington, # Cheshire WA4 4AD, fax. (44)1925 603124, e-mail as above. # http://www.staff.ncl.ac.uk/w.clegg