# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1286 data_h15 _audit_creation_method SHELXL-97 _publ_requested_journal 'J. Chem. Soc. Chem. Commun.' _publ_contact_author ; Alan Kennedy Dept. of P & A Chemistry University of Strathclyde 295 Cathedral St Glasgow G1 1XL Scotland ; _publ_contact_letter ; Dear Sir, The following CIF contains the x-ray data associated with the recently submitted paper by Allan, Henderson & Kennedy " Bisamidomagnesium mediated aladol additions ......". Please contact me if there are any problems with the files construction or transmission. Yours, Alan Kennedy ; _publ_requested_coeditor_name 'Ed Constable' _publ_contact_author_phone '0141 548 2016 ' _publ_contact_author_fax '0141 552 0876 ' _publ_contact_author_email 'a.r.kennedy@ccsun.strath.ac.uk' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H82 Mg2 N2 O4 Si4' _chemical_formula_weight 768.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Si' 'Si' 0.0817 0.0704 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.610(3) _cell_length_b 11.381(2) _cell_length_c 12.024(4) _cell_angle_alpha 98.90(2) _cell_angle_beta 104.00(2) _cell_angle_gamma 105.996(19) _cell_volume 1191.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 21.35 _cell_measurement_theta_max 22.41 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 0.185 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Diffractometer' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6084 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 28.03 _reflns_number_total 5746 _reflns_number_gt 4652 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'AFC7S DIFFRACTOMETER CONTROL' _computing_cell_refinement 'AFC7S DIFFRACTOMETER CONTROL' _computing_data_reduction 'TEXSAN' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material 'SHELXL97' _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 w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.7217P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5746 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1337 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.40326(7) 0.24863(5) 1.22773(6) 0.03735(16) Uani 1 d . . . Si2 Si 0.71918(8) 0.27885(6) 1.36702(6) 0.04466(18) Uani 1 d . . . Mg1 Mg 0.57052(7) 0.07918(5) 1.11780(5) 0.02450(15) Uani 1 d . . . O1 O 0.58229(14) 0.08992(11) 0.95953(11) 0.0262(3) Uani 1 d . . . O2 O 0.28821(15) 0.01199(12) 0.80470(12) 0.0322(3) Uani 1 d . . . N1 N 0.56748(19) 0.21512(15) 1.24241(15) 0.0316(3) Uani 1 d . . . C1 C 0.4191(3) 0.4120(2) 1.2068(3) 0.0700(9) Uani 1 d . . . H1A H 0.4893 0.4741 1.2781 0.105 Uiso 1 calc R . . H1B H 0.3190 0.4226 1.1918 0.105 Uiso 1 calc R . . H1C H 0.4574 0.4243 1.1394 0.105 Uiso 1 calc R . . C2 C 0.2484(2) 0.1415(2) 1.0936(2) 0.0434(5) Uani 1 d . . . H2A H 0.2780 0.1536 1.0227 0.065 Uiso 1 calc R . . H2B H 0.1545 0.1612 1.0896 0.065 Uiso 1 calc R . . H2C H 0.2319 0.0538 1.0987 0.065 Uiso 1 calc R . . C3 C 0.3265(4) 0.2309(3) 1.3561(3) 0.0653(8) Uani 1 d . . . H3A H 0.3102 0.1449 1.3663 0.098 Uiso 1 calc R . . H3B H 0.2300 0.2481 1.3410 0.098 Uiso 1 calc R . . H3C H 0.3994 0.2906 1.4279 0.098 Uiso 1 calc R . . C4 C 0.7093(4) 0.1811(3) 1.4792(2) 0.0712(9) Uani 1 d . . . H4A H 0.6163 0.1745 1.5015 0.107 Uiso 1 calc R . . H4B H 0.7977 0.2211 1.5493 0.107 Uiso 1 calc R . . H4C H 0.7087 0.0969 1.4454 0.107 Uiso 1 calc R . . C5 C 0.7410(4) 0.4419(3) 1.4444(3) 0.0839(11) Uani 1 d . . . H5A H 0.7599 0.4991 1.3926 0.126 Uiso 1 calc R . . H5B H 0.8267 0.4700 1.5169 0.126 Uiso 1 calc R . . H5C H 0.6480 0.4418 1.4643 0.126 Uiso 1 calc R . . C6 C 0.9024(3) 0.2892(3) 1.3346(3) 0.0582(7) Uani 1 d . . . H6A H 0.8962 0.2065 1.2916 0.087 Uiso 1 calc R . . H6B H 0.9852 0.3163 1.4088 0.087 Uiso 1 calc R . . H6C H 0.9219 0.3504 1.2864 0.087 Uiso 1 calc R . . C7 C 0.6086(3) 0.1738(2) 0.8846(2) 0.0235(5) Uani 0.805(3) d P . . C8 C 0.7600(2) 0.2862(2) 0.9457(3) 0.0280(5) Uani 0.805(3) d P . . C9 C 0.7409(3) 0.3793(2) 1.0444(2) 0.0333(6) Uani 0.805(3) d P . . H9A H 0.6899 0.3323 1.0932 0.050 Uiso 0.805(3) calc PR . . H9B H 0.6797 0.4277 1.0091 0.050 Uiso 0.805(3) calc PR . . H9C H 0.8409 0.4368 1.0936 0.050 Uiso 0.805(3) calc PR . . C10 C 0.8869(3) 0.2383(3) 0.9994(4) 0.0319(7) Uani 0.805(3) d P . . H10A H 0.8996 0.1785 0.9378 0.048 Uiso 0.805(3) calc PR . . H10B H 0.8616 0.1962 1.0605 0.048 Uiso 0.805(3) calc PR . . H10C H 0.9815 0.3092 1.0346 0.048 Uiso 0.805(3) calc PR . . C11 C 0.8069(2) 0.3618(2) 0.8573(2) 0.0404(5) Uani 1 d . . . H11A H 0.8923 0.4384 0.8998 0.061 Uiso 1 calc R . . H11B H 0.7210 0.3846 0.8153 0.061 Uiso 1 calc R . . H11C H 0.8372 0.3105 0.8004 0.061 Uiso 1 calc R . . C12 C 0.6164(3) 0.1045(2) 0.7664(2) 0.0312(5) Uani 0.805(3) d P . . H12A H 0.7113 0.0848 0.7796 0.047 Uiso 0.805(3) calc PR . . H12B H 0.6128 0.1584 0.7103 0.047 Uiso 0.805(3) calc PR . . H12C H 0.5301 0.0263 0.7344 0.047 Uiso 0.805(3) calc PR . . C13 C 0.4715(2) 0.2209(2) 0.8588(2) 0.0264(5) Uani 0.805(3) d P . . H13A H 0.4668 0.2654 0.9347 0.040 Uiso 0.805(3) calc PR . . H13B H 0.4895 0.2833 0.8106 0.040 Uiso 0.805(3) calc PR . . C14 C 0.3165(2) 0.12086(18) 0.79530(17) 0.0281(4) Uani 1 d . . . C15 C 0.1863(4) 0.1649(4) 0.7345(4) 0.0296(7) Uani 0.805(3) d P . . C16 C 0.0330(3) 0.0666(3) 0.7179(4) 0.0509(9) Uani 0.805(3) d P . . H16A H 0.0220 0.0570 0.7952 0.076 Uiso 0.805(3) calc PR . . H16B H 0.0278 -0.0142 0.6716 0.076 Uiso 0.805(3) calc PR . . H16C H -0.0489 0.0940 0.6762 0.076 Uiso 0.805(3) calc PR . . C17 C 0.2084(6) 0.1777(4) 0.6134(3) 0.0530(10) Uani 0.805(3) d P . . H17A H 0.1253 0.2011 0.5676 0.079 Uiso 0.805(3) calc PR . . H17B H 0.2088 0.0973 0.5705 0.079 Uiso 0.805(3) calc PR . . H17C H 0.3053 0.2430 0.6251 0.079 Uiso 0.805(3) calc PR . . C18 C 0.1949(6) 0.2936(5) 0.8027(6) 0.0391(11) Uani 0.805(3) d P . . H18A H 0.1143 0.3206 0.7584 0.059 Uiso 0.805(3) calc PR . . H18B H 0.2939 0.3553 0.8130 0.059 Uiso 0.805(3) calc PR . . H18C H 0.1822 0.2871 0.8802 0.059 Uiso 0.805(3) calc PR . . C19 C 0.5923(12) 0.2091(11) 0.9152(10) 0.024(3) Uiso 0.195(3) d P . . C20 C 0.7542(12) 0.2387(11) 0.8958(11) 0.030(2) Uiso 0.195(3) d P . . C21 C 0.7675(13) 0.1362(11) 0.8055(10) 0.038(2) Uiso 0.195(3) d P . . C22 C 0.876(2) 0.2603(17) 1.0270(16) 0.039(5) Uiso 0.195(3) d P . . C23 C 0.5715(11) 0.3169(9) 0.9927(8) 0.027(2) Uiso 0.195(3) d P . . C24 C 0.4715(10) 0.1726(9) 0.7888(8) 0.0234(19) Uiso 0.195(3) d P . . C25 C 0.2060(19) 0.1619(16) 0.7094(14) 0.024(4) Uiso 0.195(3) d P . . C26 C 0.0566(16) 0.0524(13) 0.6718(11) 0.034(3) Uiso 0.195(3) d P . . C27 C 0.2601(18) 0.1927(17) 0.6055(17) 0.041(4) Uiso 0.195(3) d P . . C28 C 0.192(3) 0.272(2) 0.780(2) 0.035(5) Uiso 0.195(3) d P . . 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 0.0360(3) 0.0272(3) 0.0525(4) 0.0102(2) 0.0146(3) 0.0143(2) Si2 0.0470(4) 0.0385(3) 0.0342(3) -0.0010(2) -0.0047(3) 0.0115(3) Mg1 0.0202(3) 0.0207(3) 0.0272(3) 0.0072(2) 0.0005(2) 0.0031(2) O1 0.0222(6) 0.0221(6) 0.0287(6) 0.0102(5) 0.0025(5) 0.0006(5) O2 0.0262(6) 0.0249(6) 0.0358(7) 0.0080(5) -0.0043(5) 0.0049(5) N1 0.0301(8) 0.0282(8) 0.0332(8) 0.0061(6) 0.0041(7) 0.0097(6) C1 0.0560(16) 0.0309(12) 0.120(3) 0.0200(15) 0.0124(17) 0.0200(12) C2 0.0275(10) 0.0377(11) 0.0659(15) 0.0156(10) 0.0091(10) 0.0146(9) C3 0.0649(18) 0.0628(17) 0.074(2) 0.0032(15) 0.0405(16) 0.0204(14) C4 0.084(2) 0.083(2) 0.0363(13) 0.0170(14) 0.0003(14) 0.0256(18) C5 0.082(2) 0.0518(17) 0.079(2) -0.0253(16) -0.0143(18) 0.0176(16) C6 0.0342(12) 0.0504(14) 0.0632(17) 0.0022(12) -0.0137(11) 0.0030(10) C7 0.0186(10) 0.0195(11) 0.0316(12) 0.0092(10) 0.0065(9) 0.0039(9) C8 0.0186(10) 0.0221(11) 0.0405(14) 0.0096(11) 0.0077(9) 0.0023(8) C9 0.0248(11) 0.0229(11) 0.0458(14) 0.0031(10) 0.0072(10) 0.0034(9) C10 0.0177(12) 0.0275(15) 0.0437(19) 0.0049(14) 0.0053(12) 0.0025(10) C11 0.0335(10) 0.0301(10) 0.0618(14) 0.0194(10) 0.0215(10) 0.0061(8) C12 0.0324(12) 0.0281(11) 0.0345(12) 0.0097(9) 0.0128(10) 0.0086(9) C13 0.0196(10) 0.0229(10) 0.0370(13) 0.0110(9) 0.0065(9) 0.0070(8) C14 0.0240(8) 0.0295(9) 0.0303(9) 0.0110(7) 0.0039(7) 0.0096(7) C15 0.0226(14) 0.0364(16) 0.0314(18) 0.0143(14) 0.0035(13) 0.0129(11) C16 0.0193(13) 0.0486(18) 0.075(3) 0.0226(18) -0.0064(15) 0.0097(12) C17 0.069(3) 0.064(2) 0.0376(18) 0.0251(16) 0.0128(19) 0.037(2) C18 0.0372(18) 0.033(2) 0.051(3) 0.010(2) 0.0096(18) 0.0223(16) _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 N1 1.6985(18) . ? Si1 C3 1.879(3) . ? Si1 C2 1.879(3) . ? Si1 C1 1.885(3) . ? Si1 Mg1 3.1618(11) . ? Si2 N1 1.7089(19) . ? Si2 C6 1.870(3) . ? Si2 C5 1.873(3) . ? Si2 C4 1.880(3) . ? Si2 Mg1 3.1964(15) . ? Mg1 O1 1.9540(15) . ? Mg1 O1 1.9881(15) 2_657 ? Mg1 N1 1.9920(19) . ? Mg1 O2 2.0619(15) 2_657 ? Mg1 Mg1 2.8855(16) 2_657 ? O1 C7 1.426(2) . ? O1 C19 1.520(11) . ? O1 Mg1 1.9881(15) 2_657 ? O2 C14 1.223(2) . ? O2 Mg1 2.0619(15) 2_657 ? C7 C13 1.537(3) . ? C7 C12 1.544(4) . ? C7 C8 1.568(3) . ? C8 C10 1.516(4) . ? C8 C11 1.541(3) . ? C8 C9 1.545(4) . ? C13 C14 1.531(3) . ? C14 C15 1.539(4) . ? C15 C16 1.530(5) . ? C15 C18 1.533(6) . ? C15 C17 1.544(6) . ? C19 C23 1.511(15) . ? C19 C20 1.581(16) . ? C19 C24 1.586(14) . ? C20 C21 1.521(17) . ? C20 C22 1.66(2) . ? C25 C28 1.46(2) . ? C25 C27 1.52(2) . ? C25 C26 1.53(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C3 113.36(13) . . ? N1 Si1 C2 111.63(10) . . ? C3 Si1 C2 105.89(14) . . ? N1 Si1 C1 113.60(12) . . ? C3 Si1 C1 107.15(16) . . ? C2 Si1 C1 104.54(13) . . ? N1 Si1 Mg1 33.91(6) . . ? C3 Si1 Mg1 126.76(11) . . ? C2 Si1 Mg1 77.75(8) . . ? C1 Si1 Mg1 123.60(12) . . ? N1 Si2 C6 111.76(11) . . ? N1 Si2 C5 114.36(13) . . ? C6 Si2 C5 105.95(17) . . ? N1 Si2 C4 112.07(13) . . ? C6 Si2 C4 105.79(15) . . ? C5 Si2 C4 106.31(18) . . ? N1 Si2 Mg1 32.93(6) . . ? C6 Si2 Mg1 84.31(9) . . ? C5 Si2 Mg1 143.01(12) . . ? C4 Si2 Mg1 104.66(11) . . ? O1 Mg1 O1 85.90(6) . 2_657 ? O1 Mg1 N1 126.96(7) . . ? O1 Mg1 N1 129.57(7) 2_657 . ? O1 Mg1 O2 111.60(7) . 2_657 ? O1 Mg1 O2 87.18(6) 2_657 2_657 ? N1 Mg1 O2 108.51(7) . 2_657 ? O1 Mg1 Mg1 43.41(4) . 2_657 ? O1 Mg1 Mg1 42.48(4) 2_657 2_657 ? N1 Mg1 Mg1 147.78(6) . 2_657 ? O2 Mg1 Mg1 102.44(6) 2_657 2_657 ? O1 Mg1 Si1 115.92(5) . . ? O1 Mg1 Si1 107.34(5) 2_657 . ? N1 Mg1 Si1 28.40(5) . . ? O2 Mg1 Si1 130.92(5) 2_657 . ? Mg1 Mg1 Si1 120.09(4) 2_657 . ? O1 Mg1 Si2 132.19(5) . . ? O1 Mg1 Si2 141.53(5) 2_657 . ? N1 Mg1 Si2 27.80(5) . . ? O2 Mg1 Si2 83.21(5) 2_657 . ? Mg1 Mg1 Si2 173.80(4) 2_657 . ? Si1 Mg1 Si2 56.05(3) . . ? C7 O1 C19 22.5(4) . . ? C7 O1 Mg1 144.29(16) . . ? C19 O1 Mg1 122.9(5) . . ? C7 O1 Mg1 116.06(13) . 2_657 ? C19 O1 Mg1 126.3(4) . 2_657 ? Mg1 O1 Mg1 94.10(6) . 2_657 ? C14 O2 Mg1 130.27(12) . 2_657 ? Si1 N1 Si2 122.52(11) . . ? Si1 N1 Mg1 117.69(9) . . ? Si2 N1 Mg1 119.27(10) . . ? O1 C7 C13 106.40(19) . . ? O1 C7 C12 110.9(2) . . ? C13 C7 C12 108.3(2) . . ? O1 C7 C8 110.88(19) . . ? C13 C7 C8 111.1(2) . . ? C12 C7 C8 109.2(2) . . ? C10 C8 C11 109.0(2) . . ? C10 C8 C9 108.6(3) . . ? C11 C8 C9 106.7(2) . . ? C10 C8 C7 110.4(2) . . ? C11 C8 C7 111.3(2) . . ? C9 C8 C7 110.8(2) . . ? C14 C13 C7 116.49(19) . . ? O2 C14 C13 122.26(17) . . ? O2 C14 C15 119.2(2) . . ? C13 C14 C15 117.8(2) . . ? C16 C15 C18 110.5(4) . . ? C16 C15 C14 110.2(3) . . ? C18 C15 C14 112.1(3) . . ? C16 C15 C17 110.2(3) . . ? C18 C15 C17 108.6(3) . . ? C14 C15 C17 105.1(3) . . ? C23 C19 O1 117.2(8) . . ? C23 C19 C20 114.5(9) . . ? O1 C19 C20 100.2(8) . . ? C23 C19 C24 109.2(9) . . ? O1 C19 C24 108.1(8) . . ? C20 C19 C24 107.0(9) . . ? C21 C20 C19 114.0(10) . . ? C21 C20 C22 110.9(10) . . ? C19 C20 C22 105.8(10) . . ? C28 C25 C27 111.3(17) . . ? C28 C25 C26 110.3(15) . . ? C27 C25 C26 112.6(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Si1 Mg1 O1 -120.43(12) . . . . ? C3 Si1 Mg1 O1 162.53(14) . . . . ? C2 Si1 Mg1 O1 61.72(9) . . . . ? C1 Si1 Mg1 O1 -37.73(14) . . . . ? N1 Si1 Mg1 O1 145.65(12) . . . 2_657 ? C3 Si1 Mg1 O1 68.61(14) . . . 2_657 ? C2 Si1 Mg1 O1 -32.20(9) . . . 2_657 ? C1 Si1 Mg1 O1 -131.65(13) . . . 2_657 ? C3 Si1 Mg1 N1 -77.04(17) . . . . ? C2 Si1 Mg1 N1 -177.85(14) . . . . ? C1 Si1 Mg1 N1 82.70(17) . . . . ? N1 Si1 Mg1 O2 43.97(12) . . . 2_657 ? C3 Si1 Mg1 O2 -33.07(15) . . . 2_657 ? C2 Si1 Mg1 O2 -133.88(10) . . . 2_657 ? C1 Si1 Mg1 O2 126.67(14) . . . 2_657 ? N1 Si1 Mg1 Mg1 -169.75(11) . . . 2_657 ? C3 Si1 Mg1 Mg1 113.21(14) . . . 2_657 ? C2 Si1 Mg1 Mg1 12.40(9) . . . 2_657 ? C1 Si1 Mg1 Mg1 -87.04(13) . . . 2_657 ? N1 Si1 Mg1 Si2 4.52(10) . . . . ? C3 Si1 Mg1 Si2 -72.52(13) . . . . ? C2 Si1 Mg1 Si2 -173.33(8) . . . . ? C1 Si1 Mg1 Si2 87.23(13) . . . . ? N1 Si2 Mg1 O1 91.19(13) . . . . ? C6 Si2 Mg1 O1 -55.85(12) . . . . ? C5 Si2 Mg1 O1 53.2(2) . . . . ? C4 Si2 Mg1 O1 -160.72(14) . . . . ? N1 Si2 Mg1 O1 -78.96(13) . . . 2_657 ? C6 Si2 Mg1 O1 134.00(12) . . . 2_657 ? C5 Si2 Mg1 O1 -116.9(2) . . . 2_657 ? C4 Si2 Mg1 O1 29.13(15) . . . 2_657 ? C6 Si2 Mg1 N1 -147.04(15) . . . . ? C5 Si2 Mg1 N1 -38.0(3) . . . . ? C4 Si2 Mg1 N1 108.09(17) . . . . ? N1 Si2 Mg1 O2 -155.70(12) . . . 2_657 ? C6 Si2 Mg1 O2 57.26(11) . . . 2_657 ? C5 Si2 Mg1 O2 166.3(2) . . . 2_657 ? C4 Si2 Mg1 O2 -47.61(13) . . . 2_657 ? N1 Si2 Mg1 Mg1 48.5(4) . . . 2_657 ? C6 Si2 Mg1 Mg1 -98.6(4) . . . 2_657 ? C5 Si2 Mg1 Mg1 10.5(4) . . . 2_657 ? C4 Si2 Mg1 Mg1 156.6(4) . . . 2_657 ? N1 Si2 Mg1 Si1 -4.61(11) . . . . ? C6 Si2 Mg1 Si1 -151.65(10) . . . . ? C5 Si2 Mg1 Si1 -42.6(2) . . . . ? C4 Si2 Mg1 Si1 103.48(13) . . . . ? O1 Mg1 O1 C7 148.7(2) 2_657 . . . ? N1 Mg1 O1 C7 10.5(2) . . . . ? O2 Mg1 O1 C7 -126.0(2) 2_657 . . . ? Mg1 Mg1 O1 C7 148.7(2) 2_657 . . . ? Si1 Mg1 O1 C7 41.4(2) . . . . ? Si2 Mg1 O1 C7 -25.2(2) . . . . ? O1 Mg1 O1 C19 138.9(5) 2_657 . . . ? N1 Mg1 O1 C19 0.7(5) . . . . ? O2 Mg1 O1 C19 -135.8(5) 2_657 . . . ? Mg1 Mg1 O1 C19 138.9(5) 2_657 . . . ? Si1 Mg1 O1 C19 31.6(5) . . . . ? Si2 Mg1 O1 C19 -35.0(5) . . . . ? O1 Mg1 O1 Mg1 0.0 2_657 . . 2_657 ? N1 Mg1 O1 Mg1 -138.18(8) . . . 2_657 ? O2 Mg1 O1 Mg1 85.33(7) 2_657 . . 2_657 ? Si1 Mg1 O1 Mg1 -107.30(5) . . . 2_657 ? Si2 Mg1 O1 Mg1 -173.88(5) . . . 2_657 ? C3 Si1 N1 Si2 -49.92(17) . . . . ? C2 Si1 N1 Si2 -169.40(12) . . . . ? C1 Si1 N1 Si2 72.70(18) . . . . ? Mg1 Si1 N1 Si2 -171.66(19) . . . . ? C3 Si1 N1 Mg1 121.74(14) . . . . ? C2 Si1 N1 Mg1 2.26(14) . . . . ? C1 Si1 N1 Mg1 -115.64(16) . . . . ? C6 Si2 N1 Si1 -152.81(13) . . . . ? C5 Si2 N1 Si1 -32.4(2) . . . . ? C4 Si2 N1 Si1 88.63(17) . . . . ? Mg1 Si2 N1 Si1 171.5(2) . . . . ? C6 Si2 N1 Mg1 35.66(15) . . . . ? C5 Si2 N1 Mg1 156.02(18) . . . . ? C4 Si2 N1 Mg1 -82.90(16) . . . . ? O1 Mg1 N1 Si1 76.04(13) . . . . ? O1 Mg1 N1 Si1 -44.32(14) 2_657 . . . ? O2 Mg1 N1 Si1 -146.41(9) 2_657 . . . ? Mg1 Mg1 N1 Si1 16.79(19) 2_657 . . . ? Si2 Mg1 N1 Si1 -171.94(19) . . . . ? O1 Mg1 N1 Si2 -112.02(11) . . . . ? O1 Mg1 N1 Si2 127.62(10) 2_657 . . . ? O2 Mg1 N1 Si2 25.53(12) 2_657 . . . ? Mg1 Mg1 N1 Si2 -171.27(7) 2_657 . . . ? Si1 Mg1 N1 Si2 171.94(19) . . . . ? C19 O1 C7 C13 -47.4(11) . . . . ? Mg1 O1 C7 C13 -69.5(3) . . . . ? Mg1 O1 C7 C13 75.3(2) 2_657 . . . ? C19 O1 C7 C12 -165.0(12) . . . . ? Mg1 O1 C7 C12 172.95(15) . . . . ? Mg1 O1 C7 C12 -42.3(2) 2_657 . . . ? C19 O1 C7 C8 73.5(12) . . . . ? Mg1 O1 C7 C8 51.4(3) . . . . ? Mg1 O1 C7 C8 -163.82(17) 2_657 . . . ? O1 C7 C8 C10 46.9(4) . . . . ? C13 C7 C8 C10 165.0(2) . . . . ? C12 C7 C8 C10 -75.5(3) . . . . ? O1 C7 C8 C11 168.1(2) . . . . ? C13 C7 C8 C11 -73.8(3) . . . . ? C12 C7 C8 C11 45.6(3) . . . . ? O1 C7 C8 C9 -73.4(3) . . . . ? C13 C7 C8 C9 44.7(3) . . . . ? C12 C7 C8 C9 164.1(2) . . . . ? O1 C7 C13 C14 -61.2(3) . . . . ? C12 C7 C13 C14 58.1(2) . . . . ? C8 C7 C13 C14 178.1(2) . . . . ? Mg1 O2 C14 C13 -8.8(3) 2_657 . . . ? Mg1 O2 C14 C15 -178.7(2) 2_657 . . . ? C7 C13 C14 O2 28.4(3) . . . . ? C7 C13 C14 C15 -161.5(3) . . . . ? O2 C14 C15 C16 11.8(4) . . . . ? C13 C14 C15 C16 -158.5(3) . . . . ? O2 C14 C15 C18 135.3(3) . . . . ? C13 C14 C15 C18 -35.0(4) . . . . ? O2 C14 C15 C17 -106.9(3) . . . . ? C13 C14 C15 C17 82.7(3) . . . . ? C7 O1 C19 C23 -173.0(18) . . . . ? Mg1 O1 C19 C23 -8.1(10) . . . . ? Mg1 O1 C19 C23 117.4(7) 2_657 . . . ? C7 O1 C19 C20 -48.6(10) . . . . ? Mg1 O1 C19 C20 116.3(7) . . . . ? Mg1 O1 C19 C20 -118.2(6) 2_657 . . . ? C7 O1 C19 C24 63.2(11) . . . . ? Mg1 O1 C19 C24 -131.9(6) . . . . ? Mg1 O1 C19 C24 -6.4(10) 2_657 . . . ? C23 C19 C20 C21 -172.6(9) . . . . ? O1 C19 C20 C21 61.2(10) . . . . ? C24 C19 C20 C21 -51.5(12) . . . . ? C23 C19 C20 C22 65.3(12) . . . . ? O1 C19 C20 C22 -61.0(11) . . . . ? C24 C19 C20 C22 -173.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.524 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.052 #=END