# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_12msh13-new _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 N2 Si' _chemical_formula_weight 458.75 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' 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 P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.1354(4) _cell_length_b 9.2400(3) _cell_length_c 20.1280(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.781(2) _cell_angle_gamma 90.00 _cell_volume 2755.63(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 156077 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.105 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.560 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35403 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6254 _reflns_number_gt 4983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. H1 and H2 - attached to N1 and N2, respectively, were located and refined at a distance of 0.98 Angstroms from the relevant parent atoms. H1A, attached to Si1, was also located and refined without restraints. ; _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^)+(0.0502P)^2^+1.8058P] 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 SHELXL _refine_ls_extinction_coef 0.011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6254 _refine_ls_number_parameters 319 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 0.23565(3) 0.68320(6) 0.30349(3) 0.02949(16) Uani 1 1 d . . . N1 N 0.14782(10) 0.65467(18) 0.23632(8) 0.0303(4) Uani 1 1 d D . . N2 N 0.32181(10) 0.74605(19) 0.26656(8) 0.0324(4) Uani 1 1 d D . . C1 C 0.25847(11) 0.5078(2) 0.35035(9) 0.0308(4) Uani 1 1 d . . . C2 C 0.29032(13) 0.3863(2) 0.32103(10) 0.0352(4) Uani 1 1 d . . . H2A H 0.2979 0.3916 0.2754 0.042 Uiso 1 1 calc R . . C3 C 0.31126(14) 0.2579(3) 0.35696(12) 0.0418(5) Uani 1 1 d . . . H3 H 0.3332 0.1769 0.3362 0.050 Uiso 1 1 calc R . . C4 C 0.29976(15) 0.2494(3) 0.42329(12) 0.0466(6) Uani 1 1 d . . . H4 H 0.3131 0.1618 0.4480 0.056 Uiso 1 1 calc R . . C5 C 0.26905(15) 0.3676(3) 0.45365(11) 0.0467(6) Uani 1 1 d . . . H5 H 0.2616 0.3614 0.4993 0.056 Uiso 1 1 calc R . . C6 C 0.24889(13) 0.4963(3) 0.41754(10) 0.0383(5) Uani 1 1 d . . . H6 H 0.2283 0.5774 0.4391 0.046 Uiso 1 1 calc R . . C7 C 0.12842(12) 0.7304(2) 0.17280(9) 0.0299(4) Uani 1 1 d . . . C8 C 0.14768(13) 0.6625(2) 0.11449(10) 0.0349(4) Uani 1 1 d . . . C9 C 0.18611(14) 0.5097(3) 0.11740(11) 0.0399(5) Uani 1 1 d . . . H9 H 0.2186 0.4919 0.1652 0.048 Uiso 1 1 calc R . . C10 C 0.25398(15) 0.4879(3) 0.07162(12) 0.0443(5) Uani 1 1 d . . . H10A H 0.2229 0.4952 0.0240 0.066 Uiso 1 1 calc R . . H10B H 0.2818 0.3921 0.0800 0.066 Uiso 1 1 calc R . . H10C H 0.3008 0.5625 0.0815 0.066 Uiso 1 1 calc R . . C11 C 0.11075(19) 0.3982(3) 0.10078(17) 0.0633(8) Uani 1 1 d . . . H11A H 0.0696 0.4093 0.1322 0.095 Uiso 1 1 calc R . . H11B H 0.1368 0.3007 0.1053 0.095 Uiso 1 1 calc R . . H11C H 0.0774 0.4128 0.0541 0.095 Uiso 1 1 calc R . . C12 C 0.12962(15) 0.7375(3) 0.05322(11) 0.0425(5) Uani 1 1 d . . . H12 H 0.1415 0.6924 0.0136 0.051 Uiso 1 1 calc R . . C13 C 0.09456(15) 0.8768(3) 0.04887(11) 0.0434(5) Uani 1 1 d . . . H13 H 0.0835 0.9269 0.0068 0.052 Uiso 1 1 calc R . . C14 C 0.07585(13) 0.9422(2) 0.10601(11) 0.0382(5) Uani 1 1 d . . . H14 H 0.0521 1.0377 0.1028 0.046 Uiso 1 1 calc R . . C15 C 0.09118(12) 0.8708(2) 0.16854(10) 0.0317(4) Uani 1 1 d . . . C16 C 0.07002(13) 0.9474(2) 0.23017(11) 0.0364(5) Uani 1 1 d . . . H16 H 0.0678 0.8725 0.2657 0.044 Uiso 1 1 calc R . . C17 C -0.02145(14) 1.0251(3) 0.21516(13) 0.0454(5) Uani 1 1 d . . . H17A H -0.0209 1.1001 0.1808 0.068 Uiso 1 1 calc R . . H17B H -0.0325 1.0698 0.2569 0.068 Uiso 1 1 calc R . . H17C H -0.0694 0.9550 0.1982 0.068 Uiso 1 1 calc R . . C18 C 0.14417(15) 1.0556(3) 0.25959(13) 0.0487(6) Uani 1 1 d . . . H18A H 0.2029 1.0066 0.2680 0.073 Uiso 1 1 calc R . . H18B H 0.1328 1.0946 0.3023 0.073 Uiso 1 1 calc R . . H18C H 0.1444 1.1348 0.2273 0.073 Uiso 1 1 calc R . . C19 C 0.38786(12) 0.8559(2) 0.28584(10) 0.0312(4) Uani 1 1 d . . . C20 C 0.44225(13) 0.8582(2) 0.35161(10) 0.0363(5) Uani 1 1 d . . . C21 C 0.43628(14) 0.7433(3) 0.40416(10) 0.0420(5) Uani 1 1 d . . . H21 H 0.3756 0.6968 0.3906 0.050 Uiso 1 1 calc R . . C22 C 0.5062(3) 0.6257(4) 0.40426(16) 0.0854(11) Uani 1 1 d . . . H22A H 0.5667 0.6684 0.4148 0.128 Uiso 1 1 calc R . . H22B H 0.4963 0.5798 0.3595 0.128 Uiso 1 1 calc R . . H22C H 0.5007 0.5530 0.4386 0.128 Uiso 1 1 calc R . . C23 C 0.4433(2) 0.8016(3) 0.47529(13) 0.0601(7) Uani 1 1 d . . . H23A H 0.4295 0.7242 0.5049 0.090 Uiso 1 1 calc R . . H23B H 0.4002 0.8811 0.4745 0.090 Uiso 1 1 calc R . . H23C H 0.5047 0.8371 0.4926 0.090 Uiso 1 1 calc R . . C24 C 0.50707(13) 0.9679(3) 0.36740(11) 0.0402(5) Uani 1 1 d . . . H24 H 0.5440 0.9707 0.4116 0.048 Uiso 1 1 calc R . . C25 C 0.51900(13) 1.0717(2) 0.32094(11) 0.0392(5) Uani 1 1 d . . . H25 H 0.5639 1.1443 0.3329 0.047 Uiso 1 1 calc R . . C26 C 0.46507(13) 1.0693(2) 0.25675(11) 0.0366(5) Uani 1 1 d . . . H26 H 0.4732 1.1408 0.2247 0.044 Uiso 1 1 calc R . . C27 C 0.39874(12) 0.9635(2) 0.23812(10) 0.0322(4) Uani 1 1 d . . . C28 C 0.34050(13) 0.9616(2) 0.16668(10) 0.0344(4) Uani 1 1 d . . . H28 H 0.2807 0.9193 0.1700 0.041 Uiso 1 1 calc R . . C29 C 0.32276(16) 1.1128(3) 0.13584(12) 0.0445(5) Uani 1 1 d . . . H29A H 0.3011 1.1763 0.1681 0.067 Uiso 1 1 calc R . . H29B H 0.2770 1.1068 0.0937 0.067 Uiso 1 1 calc R . . H29C H 0.3788 1.1521 0.1260 0.067 Uiso 1 1 calc R . . C30 C 0.38175(14) 0.8632(3) 0.11973(11) 0.0411(5) Uani 1 1 d . . . H30A H 0.3390 0.8520 0.0764 0.062 Uiso 1 1 calc R . . H30B H 0.3949 0.7681 0.1411 0.062 Uiso 1 1 calc R . . H30C H 0.4377 0.9066 0.1117 0.062 Uiso 1 1 calc R . . H1 H 0.1036(14) 0.582(2) 0.2431(13) 0.059(8) Uiso 1 1 d D . . H2 H 0.3082(15) 0.740(3) 0.2171(3) 0.042(6) Uiso 1 1 d D . . H1A H 0.2233(14) 0.778(2) 0.3532(10) 0.031(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0257(3) 0.0336(3) 0.0283(3) 0.0006(2) 0.00323(19) -0.0001(2) N1 0.0262(7) 0.0327(9) 0.0311(8) 0.0027(7) 0.0033(6) -0.0014(6) N2 0.0291(8) 0.0366(10) 0.0298(8) 0.0020(7) 0.0017(6) -0.0034(7) C1 0.0220(8) 0.0380(11) 0.0309(9) 0.0017(8) 0.0018(7) -0.0023(7) C2 0.0312(9) 0.0392(12) 0.0349(10) 0.0003(9) 0.0058(8) -0.0020(8) C3 0.0355(10) 0.0376(12) 0.0503(13) 0.0024(10) 0.0040(9) 0.0030(9) C4 0.0385(11) 0.0472(14) 0.0517(13) 0.0179(11) 0.0035(10) 0.0030(10) C5 0.0410(11) 0.0628(16) 0.0363(11) 0.0144(11) 0.0077(9) 0.0034(11) C6 0.0319(10) 0.0494(13) 0.0334(10) 0.0049(9) 0.0066(8) 0.0027(9) C7 0.0229(8) 0.0359(11) 0.0296(9) 0.0017(8) 0.0022(7) -0.0014(7) C8 0.0295(9) 0.0392(12) 0.0343(10) 0.0004(8) 0.0029(8) 0.0051(8) C9 0.0438(11) 0.0408(12) 0.0346(10) 0.0012(9) 0.0066(9) 0.0104(9) C10 0.0413(11) 0.0412(13) 0.0501(13) -0.0028(10) 0.0091(10) 0.0051(10) C11 0.0559(15) 0.0397(15) 0.102(2) 0.0016(14) 0.0337(15) 0.0016(12) C12 0.0457(12) 0.0496(14) 0.0315(10) 0.0028(9) 0.0061(9) 0.0114(10) C13 0.0424(11) 0.0501(14) 0.0362(11) 0.0111(10) 0.0043(9) 0.0108(10) C14 0.0317(10) 0.0374(12) 0.0438(11) 0.0069(9) 0.0041(8) 0.0066(8) C15 0.0237(8) 0.0336(11) 0.0367(10) 0.0006(8) 0.0037(7) 0.0008(7) C16 0.0334(10) 0.0351(11) 0.0411(11) -0.0008(9) 0.0086(8) 0.0025(8) C17 0.0327(10) 0.0435(14) 0.0609(14) -0.0081(11) 0.0119(10) 0.0035(9) C18 0.0395(12) 0.0504(15) 0.0541(14) -0.0139(11) 0.0044(10) -0.0005(10) C19 0.0236(8) 0.0322(10) 0.0375(10) 0.0000(8) 0.0058(7) -0.0014(7) C20 0.0270(9) 0.0429(12) 0.0373(10) 0.0006(9) 0.0029(8) -0.0020(8) C21 0.0363(11) 0.0501(14) 0.0351(11) 0.0053(10) -0.0034(8) -0.0076(9) C22 0.142(3) 0.061(2) 0.0637(18) 0.0247(15) 0.048(2) 0.041(2) C23 0.0682(17) 0.0672(19) 0.0493(14) 0.0016(13) 0.0222(13) 0.0000(14) C24 0.0292(10) 0.0480(13) 0.0412(11) -0.0045(10) 0.0021(8) -0.0037(9) C25 0.0298(10) 0.0362(12) 0.0514(12) -0.0059(9) 0.0081(9) -0.0055(8) C26 0.0311(9) 0.0328(11) 0.0475(12) 0.0019(9) 0.0115(8) 0.0010(8) C27 0.0254(9) 0.0330(11) 0.0389(10) 0.0013(8) 0.0081(7) 0.0013(7) C28 0.0276(9) 0.0362(11) 0.0392(11) 0.0073(8) 0.0059(8) 0.0021(8) C29 0.0463(12) 0.0409(13) 0.0453(12) 0.0083(10) 0.0069(10) 0.0069(10) C30 0.0371(10) 0.0448(13) 0.0404(11) 0.0017(9) 0.0057(9) 0.0031(9) _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 1.7119(16) . ? Si1 N2 1.7281(17) . ? Si1 C1 1.871(2) . ? Si1 H1A 1.37(2) . ? N1 C7 1.434(2) . ? N1 H1 0.976(5) . ? N2 C19 1.422(2) . ? N2 H2 0.976(5) . ? C1 C6 1.393(3) . ? C1 C2 1.399(3) . ? C2 C3 1.392(3) . ? C2 H2A 0.9500 . ? C3 C4 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.377(4) . ? C4 H4 0.9500 . ? C5 C6 1.394(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C15 1.410(3) . ? C7 C8 1.413(3) . ? C8 C12 1.392(3) . ? C8 C9 1.523(3) . ? C9 C11 1.523(4) . ? C9 C10 1.527(3) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 C14 1.379(3) . ? C13 H13 0.9500 . ? C14 C15 1.398(3) . ? C14 H14 0.9500 . ? C15 C16 1.518(3) . ? C16 C18 1.529(3) . ? C16 C17 1.534(3) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.409(3) . ? C19 C27 1.415(3) . ? C20 C24 1.401(3) . ? C20 C21 1.514(3) . ? C21 C23 1.513(3) . ? C21 C22 1.517(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.377(3) . ? C24 H24 0.9500 . ? C25 C26 1.380(3) . ? C25 H25 0.9500 . ? C26 C27 1.397(3) . ? C26 H26 0.9500 . ? C27 C28 1.526(3) . ? C28 C29 1.530(3) . ? C28 C30 1.533(3) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 N1 Si1 N2 104.15(8) . . ? N1 Si1 C1 107.36(8) . . ? N2 Si1 C1 115.47(8) . . ? N1 Si1 H1A 118.4(8) . . ? N2 Si1 H1A 109.0(9) . . ? C1 Si1 H1A 103.0(9) . . ? C7 N1 Si1 127.84(13) . . ? C7 N1 H1 116.0(15) . . ? Si1 N1 H1 116.1(15) . . ? C19 N2 Si1 132.27(14) . . ? C19 N2 H2 108.0(14) . . ? Si1 N2 H2 113.5(14) . . ? C6 C1 C2 117.46(19) . . ? C6 C1 Si1 120.69(16) . . ? C2 C1 Si1 121.76(15) . . ? C3 C2 C1 121.76(19) . . ? C3 C2 H2A 119.1 . . ? C1 C2 H2A 119.1 . . ? C4 C3 C2 119.3(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 120.2(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.2(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 121.1(2) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C15 C7 C8 120.39(18) . . ? C15 C7 N1 120.63(17) . . ? C8 C7 N1 118.98(18) . . ? C12 C8 C7 118.6(2) . . ? C12 C8 C9 119.98(19) . . ? C7 C8 C9 121.43(18) . . ? C11 C9 C8 110.84(18) . . ? C11 C9 C10 110.1(2) . . ? C8 C9 C10 113.43(19) . . ? C11 C9 H9 107.4 . . ? C8 C9 H9 107.4 . . ? C10 C9 H9 107.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C8 121.4(2) . . ? C13 C12 H12 119.3 . . ? C8 C12 H12 119.3 . . ? C14 C13 C12 119.7(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 121.3(2) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C7 118.68(18) . . ? C14 C15 C16 119.43(19) . . ? C7 C15 C16 121.86(18) . . ? C15 C16 C18 111.14(17) . . ? C15 C16 C17 112.95(17) . . ? C18 C16 C17 109.39(19) . . ? C15 C16 H16 107.7 . . ? C18 C16 H16 107.7 . . ? C17 C16 H16 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C27 120.05(18) . . ? C20 C19 N2 120.69(18) . . ? C27 C19 N2 119.26(17) . . ? C24 C20 C19 118.14(19) . . ? C24 C20 C21 119.17(18) . . ? C19 C20 C21 122.62(18) . . ? C23 C21 C20 114.1(2) . . ? C23 C21 C22 109.8(2) . . ? C20 C21 C22 111.2(2) . . ? C23 C21 H21 107.1 . . ? C20 C21 H21 107.1 . . ? C22 C21 H21 107.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C20 122.18(19) . . ? C25 C24 H24 118.9 . . ? C20 C24 H24 118.9 . . ? C24 C25 C26 119.32(19) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C27 121.2(2) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C19 119.09(18) . . ? C26 C27 C28 120.41(18) . . ? C19 C27 C28 120.48(17) . . ? C27 C28 C29 113.07(18) . . ? C27 C28 C30 110.98(16) . . ? C29 C28 C30 110.57(17) . . ? C27 C28 H28 107.3 . . ? C29 C28 H28 107.3 . . ? C30 C28 H28 107.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 Si1 N1 C7 -30.12(19) . . . . ? C1 Si1 N1 C7 -153.04(16) . . . . ? N1 Si1 N2 C19 140.07(18) . . . . ? C1 Si1 N2 C19 -102.48(19) . . . . ? N1 Si1 C1 C6 -117.94(15) . . . . ? N2 Si1 C1 C6 126.42(15) . . . . ? N1 Si1 C1 C2 65.62(17) . . . . ? N2 Si1 C1 C2 -50.01(18) . . . . ? C6 C1 C2 C3 0.4(3) . . . . ? Si1 C1 C2 C3 176.98(15) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? C2 C3 C4 C5 -0.9(3) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? C2 C1 C6 C5 -1.0(3) . . . . ? Si1 C1 C6 C5 -177.54(16) . . . . ? C4 C5 C6 C1 0.6(3) . . . . ? Si1 N1 C7 C15 -75.5(2) . . . . ? Si1 N1 C7 C8 104.1(2) . . . . ? C15 C7 C8 C12 0.4(3) . . . . ? N1 C7 C8 C12 -179.26(18) . . . . ? C15 C7 C8 C9 -178.73(18) . . . . ? N1 C7 C8 C9 1.6(3) . . . . ? C12 C8 C9 C11 -87.3(3) . . . . ? C7 C8 C9 C11 91.8(2) . . . . ? C12 C8 C9 C10 37.2(3) . . . . ? C7 C8 C9 C10 -143.70(19) . . . . ? C7 C8 C12 C13 0.9(3) . . . . ? C9 C8 C12 C13 180.0(2) . . . . ? C8 C12 C13 C14 -1.0(3) . . . . ? C12 C13 C14 C15 -0.2(3) . . . . ? C13 C14 C15 C7 1.4(3) . . . . ? C13 C14 C15 C16 179.67(19) . . . . ? C8 C7 C15 C14 -1.5(3) . . . . ? N1 C7 C15 C14 178.12(17) . . . . ? C8 C7 C15 C16 -179.70(17) . . . . ? N1 C7 C15 C16 -0.1(3) . . . . ? C14 C15 C16 C18 -78.4(2) . . . . ? C7 C15 C16 C18 99.8(2) . . . . ? C14 C15 C16 C17 45.0(3) . . . . ? C7 C15 C16 C17 -136.8(2) . . . . ? Si1 N2 C19 C20 51.6(3) . . . . ? Si1 N2 C19 C27 -128.51(18) . . . . ? C27 C19 C20 C24 -0.8(3) . . . . ? N2 C19 C20 C24 179.09(18) . . . . ? C27 C19 C20 C21 -177.74(19) . . . . ? N2 C19 C20 C21 2.1(3) . . . . ? C24 C20 C21 C23 43.1(3) . . . . ? C19 C20 C21 C23 -140.0(2) . . . . ? C24 C20 C21 C22 -81.9(3) . . . . ? C19 C20 C21 C22 95.0(3) . . . . ? C19 C20 C24 C25 -0.2(3) . . . . ? C21 C20 C24 C25 176.9(2) . . . . ? C20 C24 C25 C26 0.6(3) . . . . ? C24 C25 C26 C27 0.0(3) . . . . ? C25 C26 C27 C19 -0.9(3) . . . . ? C25 C26 C27 C28 -179.33(19) . . . . ? C20 C19 C27 C26 1.3(3) . . . . ? N2 C19 C27 C26 -178.54(18) . . . . ? C20 C19 C27 C28 179.72(18) . . . . ? N2 C19 C27 C28 -0.1(3) . . . . ? C26 C27 C28 C29 -32.2(3) . . . . ? C19 C27 C28 C29 149.44(19) . . . . ? C26 C27 C28 C30 92.7(2) . . . . ? C19 C27 C28 C30 -85.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.343 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.046 _database_code_depnum_ccdc_archive 'CCDC 945785' ####################################################################### # # 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_h12msh30 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H58 Mg N2 O2 Si' _chemical_formula_weight 627.26 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2940(4) _cell_length_b 12.1680(4) _cell_length_c 13.6040(4) _cell_angle_alpha 96.759(2) _cell_angle_beta 90.610(2) _cell_angle_gamma 90.961(2) _cell_volume 1856.13(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15834 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 0.113 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.896 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _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 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25602 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8357 _reflns_number_gt 5627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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. Hydrogen atoms attached to Si1 were located and refined subject to being similar distances from the parent. H1 attached to N1 was similarly located and refined at distance of 0.98 Angstroms from the nitrogen. C36 and C37 were found to be disordered in 1 50:50 ratio over two proximate sites. C-C distances were refined with distance restraints in the associated THF molecule to assist convergence. ; _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^)+(0.0960P)^2^+0.6467P] 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 8357 _refine_ls_number_parameters 435 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.30470(6) 0.93090(5) 0.38047(5) 0.03400(18) Uani 1 1 d D . . Mg1 Mg 0.41197(6) 0.70611(6) 0.26366(5) 0.02766(19) Uani 1 1 d . . . O1 O 0.51442(15) 0.78244(13) 0.16898(12) 0.0390(4) Uani 1 1 d . . . O2 O 0.53100(13) 0.70595(12) 0.37546(12) 0.0342(4) Uani 1 1 d . C . N1 N 0.35770(16) 0.55663(15) 0.20582(14) 0.0322(4) Uani 1 1 d D . . N2 N 0.28071(15) 0.80576(14) 0.31439(13) 0.0275(4) Uani 1 1 d . . . C1 C 0.15101(19) 1.01835(18) 0.53533(18) 0.0341(5) Uani 1 1 d . . . H1C H 0.1125 1.0527 0.4849 0.041 Uiso 1 1 calc R . . C2 C 0.1083(2) 1.0347(2) 0.63130(19) 0.0412(6) Uani 1 1 d . . . H2 H 0.0423 1.0808 0.6461 0.049 Uiso 1 1 calc R . . C3 C 0.1618(2) 0.9840(2) 0.70485(19) 0.0459(6) Uani 1 1 d . . . H3 H 0.1316 0.9937 0.7702 0.055 Uiso 1 1 calc R . . C4 C 0.2598(2) 0.9185(2) 0.68353(19) 0.0462(6) Uani 1 1 d . . . H4 H 0.2971 0.8838 0.7344 0.055 Uiso 1 1 calc R . . C5 C 0.3031(2) 0.9037(2) 0.58847(19) 0.0398(6) Uani 1 1 d . . . H5 H 0.3709 0.8595 0.5751 0.048 Uiso 1 1 calc R . . C6 C 0.24959(19) 0.95239(17) 0.51111(17) 0.0319(5) Uani 1 1 d . . . C7 C 0.16248(18) 0.77099(16) 0.28595(15) 0.0257(4) Uani 1 1 d . . . C8 C 0.11279(19) 0.79754(18) 0.19548(16) 0.0299(5) Uani 1 1 d . . . C9 C 0.1812(2) 0.8674(2) 0.12904(17) 0.0369(5) Uani 1 1 d . . . H9 H 0.2530 0.8981 0.1670 0.044 Uiso 1 1 calc R . . C10 C 0.2241(3) 0.7951(3) 0.0374(2) 0.0624(8) Uani 1 1 d . . . H1C0A H 0.1557 0.7649 -0.0024 0.094 Uiso 1 1 calc R . . H1C0B H 0.2706 0.7342 0.0578 0.094 Uiso 1 1 calc R . . H1C0C H 0.2735 0.8398 -0.0021 0.094 Uiso 1 1 calc R . . C11 C 0.1109(3) 0.9651(3) 0.1012(3) 0.0644(9) Uani 1 1 d . . . H1C1A H 0.0412 0.9378 0.0616 0.097 Uiso 1 1 calc R . . H1C1B H 0.1608 1.0104 0.0627 0.097 Uiso 1 1 calc R . . H1C1C H 0.0854 1.0101 0.1616 0.097 Uiso 1 1 calc R . . C12 C 0.0016(2) 0.7556(2) 0.16541(17) 0.0363(5) Uani 1 1 d . . . H1C2 H -0.0307 0.7726 0.1043 0.044 Uiso 1 1 calc R . . C13 C -0.0636(2) 0.6899(2) 0.22169(18) 0.0371(5) Uani 1 1 d . . . H1C3 H -0.1391 0.6612 0.1992 0.044 Uiso 1 1 calc R . . C14 C -0.01756(19) 0.66639(18) 0.31082(17) 0.0330(5) Uani 1 1 d . . . H1C4 H -0.0629 0.6223 0.3503 0.040 Uiso 1 1 calc R . . C15 C 0.09428(18) 0.70585(17) 0.34464(15) 0.0274(4) Uani 1 1 d . . . C16 C 0.13981(19) 0.67634(18) 0.44378(16) 0.0305(5) Uani 1 1 d . . . H1C6 H 0.2179 0.7154 0.4577 0.037 Uiso 1 1 calc R . . C17 C 0.0575(2) 0.7157(2) 0.52831(17) 0.0393(6) Uani 1 1 d . . . H1C7A H 0.0468 0.7957 0.5306 0.059 Uiso 1 1 calc R . . H1C7B H 0.0922 0.6991 0.5911 0.059 Uiso 1 1 calc R . . H1C7C H -0.0195 0.6775 0.5176 0.059 Uiso 1 1 calc R . . C18 C 0.1608(2) 0.5525(2) 0.44028(18) 0.0405(6) Uani 1 1 d . . . H1C8A H 0.0872 0.5115 0.4209 0.061 Uiso 1 1 calc R . . H1C8B H 0.1866 0.5357 0.5058 0.061 Uiso 1 1 calc R . . H1C8C H 0.2223 0.5307 0.3919 0.061 Uiso 1 1 calc R . . C19 C 0.36950(19) 0.44370(17) 0.20601(15) 0.0295(5) Uani 1 1 d . . . C20 C 0.2683(2) 0.36988(19) 0.19815(16) 0.0340(5) Uani 1 1 d . . . C21 C 0.1459(2) 0.4140(2) 0.18199(17) 0.0368(5) Uani 1 1 d . . . H21 H 0.1400 0.4855 0.2259 0.044 Uiso 1 1 calc R . . C22 C 0.1300(3) 0.4402(3) 0.0758(2) 0.0576(8) Uani 1 1 d . . . H22A H 0.1950 0.4890 0.0594 0.086 Uiso 1 1 calc R . . H22B H 0.0544 0.4772 0.0692 0.086 Uiso 1 1 calc R . . H22C H 0.1305 0.3713 0.0305 0.086 Uiso 1 1 calc R . . C23 C 0.0439(3) 0.3394(3) 0.2086(2) 0.0621(8) Uani 1 1 d . . . H23A H 0.0415 0.2714 0.1623 0.093 Uiso 1 1 calc R . . H23B H -0.0310 0.3782 0.2045 0.093 Uiso 1 1 calc R . . H23C H 0.0558 0.3209 0.2762 0.093 Uiso 1 1 calc R . . C24 C 0.2835(3) 0.2579(2) 0.2027(2) 0.0544(7) Uani 1 1 d . . . H24 H 0.2157 0.2103 0.2003 0.065 Uiso 1 1 calc R . . C25 C 0.3944(3) 0.2134(2) 0.2106(3) 0.0722(10) Uani 1 1 d . . . H25 H 0.4032 0.1362 0.2131 0.087 Uiso 1 1 calc R . . C26 C 0.4920(3) 0.2832(2) 0.2148(3) 0.0625(9) Uani 1 1 d . . . H26 H 0.5684 0.2525 0.2187 0.075 Uiso 1 1 calc R . . C27 C 0.4830(2) 0.39679(19) 0.21361(18) 0.0368(5) Uani 1 1 d . . . C28 C 0.5960(2) 0.46598(19) 0.21502(17) 0.0356(5) Uani 1 1 d . . . H28 H 0.5741 0.5456 0.2284 0.043 Uiso 1 1 calc R . . C29 C 0.6556(3) 0.4495(2) 0.1146(2) 0.0559(7) Uani 1 1 d . . . H29A H 0.6762 0.3715 0.0990 0.084 Uiso 1 1 calc R . . H29B H 0.7277 0.4957 0.1166 0.084 Uiso 1 1 calc R . . H29C H 0.6013 0.4705 0.0637 0.084 Uiso 1 1 calc R . . C30 C 0.6841(3) 0.4417(3) 0.2956(2) 0.0568(7) Uani 1 1 d . . . H30A H 0.6455 0.4515 0.3602 0.085 Uiso 1 1 calc R . . H30B H 0.7523 0.4927 0.2965 0.085 Uiso 1 1 calc R . . H30C H 0.7110 0.3653 0.2819 0.085 Uiso 1 1 calc R . . C31 C 0.5851(3) 0.7277(3) 0.0903(2) 0.0667(10) Uani 1 1 d . . . H31A H 0.5363 0.7050 0.0302 0.080 Uiso 1 1 calc R . . H31B H 0.6240 0.6617 0.1112 0.080 Uiso 1 1 calc R . . C32 C 0.6776(4) 0.8186(4) 0.0720(3) 0.0881(13) Uani 1 1 d . . . H32A H 0.7425 0.8236 0.1219 0.106 Uiso 1 1 calc R . . H32B H 0.7115 0.8045 0.0050 0.106 Uiso 1 1 calc R . . C33 C 0.6085(3) 0.9161(3) 0.0818(2) 0.0597(8) Uani 1 1 d . . . H33A H 0.5633 0.9226 0.0200 0.072 Uiso 1 1 calc R . . H33B H 0.6596 0.9829 0.0974 0.072 Uiso 1 1 calc R . . C34 C 0.5262(3) 0.9021(2) 0.1657(2) 0.0543(7) Uani 1 1 d . . . H34A H 0.5596 0.9390 0.2289 0.065 Uiso 1 1 calc R . . H34B H 0.4482 0.9342 0.1537 0.065 Uiso 1 1 calc R . . C35 C 0.6449(2) 0.7640(2) 0.3936(2) 0.0476(6) Uani 1 1 d D . . H35A H 0.6332 0.8450 0.4046 0.057 Uiso 1 1 calc R A 1 H35B H 0.6971 0.7475 0.3359 0.057 Uiso 1 1 calc R A 1 C38 C 0.5010(2) 0.6481(2) 0.46030(19) 0.0436(6) Uani 1 1 d D . . H38A H 0.5076 0.5670 0.4438 0.052 Uiso 1 1 calc R B 1 H38B H 0.4197 0.6652 0.4829 0.052 Uiso 1 1 calc R B 1 H1CA H 0.254(2) 1.0201(18) 0.3337(17) 0.041(7) Uiso 1 1 d D . . H1B H 0.4300(17) 0.947(2) 0.3862(18) 0.041(7) Uiso 1 1 d D . . H1 H 0.2748(8) 0.572(2) 0.193(2) 0.051(8) Uiso 1 1 d D . . C37 C 0.5928(7) 0.6927(9) 0.5392(7) 0.070(3) Uani 0.50 1 d PD C 1 H37A H 0.5620 0.7579 0.5810 0.084 Uiso 0.50 1 calc PR C 1 H37B H 0.6125 0.6352 0.5822 0.084 Uiso 0.50 1 calc PR C 1 C36A C 0.6609(7) 0.7627(6) 0.5057(5) 0.0443(17) Uani 0.50 1 d PD C 2 H36A H 0.7451 0.7727 0.5262 0.053 Uiso 0.50 1 calc PR C 2 H36B H 0.6134 0.8205 0.5436 0.053 Uiso 0.50 1 calc PR C 2 C36 C 0.6995(6) 0.7243(7) 0.4842(6) 0.054(2) Uani 0.50 1 d PD C 1 H36C H 0.7507 0.6599 0.4663 0.065 Uiso 0.50 1 calc PR C 1 H36D H 0.7465 0.7839 0.5232 0.065 Uiso 0.50 1 calc PR C 1 C37A C 0.6143(6) 0.6461(5) 0.5182(7) 0.0440(19) Uani 0.50 1 d PD C 2 H37C H 0.6678 0.5879 0.4888 0.053 Uiso 0.50 1 calc PR C 2 H37D H 0.6002 0.6368 0.5884 0.053 Uiso 0.50 1 calc PR C 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 0.0301(3) 0.0270(3) 0.0430(4) -0.0038(3) 0.0049(3) -0.0049(2) Mg1 0.0219(4) 0.0246(4) 0.0358(4) 0.0008(3) 0.0019(3) -0.0006(3) O1 0.0382(9) 0.0345(9) 0.0434(9) 0.0005(7) 0.0125(7) -0.0046(7) O2 0.0264(8) 0.0316(8) 0.0443(9) 0.0046(7) -0.0046(7) -0.0056(6) N1 0.0275(10) 0.0246(9) 0.0435(11) 0.0007(8) -0.0050(8) 0.0016(8) N2 0.0217(9) 0.0244(9) 0.0355(9) -0.0002(7) 0.0010(7) -0.0011(7) C1 0.0256(11) 0.0277(11) 0.0468(13) -0.0041(10) -0.0034(10) 0.0007(9) C2 0.0286(12) 0.0367(13) 0.0547(15) -0.0096(11) 0.0034(11) 0.0040(10) C3 0.0460(15) 0.0465(15) 0.0414(14) -0.0106(12) 0.0033(11) -0.0012(12) C4 0.0509(16) 0.0428(14) 0.0432(14) -0.0017(11) -0.0093(12) 0.0069(12) C5 0.0313(12) 0.0357(13) 0.0494(14) -0.0082(11) -0.0053(10) 0.0075(10) C6 0.0243(11) 0.0248(11) 0.0442(12) -0.0055(9) -0.0020(9) -0.0015(8) C7 0.0216(10) 0.0224(10) 0.0318(10) -0.0021(8) 0.0018(8) 0.0020(8) C8 0.0296(11) 0.0277(11) 0.0318(11) -0.0003(9) 0.0026(9) 0.0020(9) C9 0.0366(13) 0.0392(13) 0.0355(12) 0.0069(10) 0.0032(10) 0.0007(10) C10 0.075(2) 0.066(2) 0.0458(16) 0.0035(14) 0.0218(15) -0.0053(16) C11 0.0589(19) 0.0550(18) 0.086(2) 0.0364(17) 0.0095(17) 0.0036(15) C12 0.0347(12) 0.0386(13) 0.0346(12) 0.0004(10) -0.0059(10) 0.0030(10) C13 0.0262(11) 0.0380(13) 0.0462(13) 0.0024(11) -0.0060(10) -0.0042(10) C14 0.0253(11) 0.0317(12) 0.0418(12) 0.0044(10) 0.0007(9) -0.0047(9) C15 0.0234(10) 0.0242(10) 0.0338(11) 0.0005(9) 0.0009(8) 0.0017(8) C16 0.0258(11) 0.0308(11) 0.0347(11) 0.0032(9) -0.0002(9) -0.0022(9) C17 0.0379(13) 0.0410(13) 0.0381(13) 0.0014(10) 0.0033(10) -0.0032(11) C18 0.0496(15) 0.0342(13) 0.0383(13) 0.0068(10) -0.0028(11) 0.0029(11) C19 0.0311(11) 0.0269(11) 0.0294(11) -0.0012(9) 0.0018(9) -0.0001(9) C20 0.0332(12) 0.0330(12) 0.0346(11) -0.0001(9) 0.0033(9) -0.0061(10) C21 0.0312(12) 0.0422(13) 0.0345(12) -0.0048(10) 0.0010(9) -0.0068(10) C22 0.0503(17) 0.076(2) 0.0458(15) 0.0049(14) -0.0128(13) -0.0078(15) C23 0.0387(16) 0.074(2) 0.072(2) 0.0043(16) 0.0073(14) -0.0152(14) C24 0.0497(17) 0.0329(13) 0.080(2) 0.0051(13) 0.0026(15) -0.0106(12) C25 0.063(2) 0.0264(14) 0.128(3) 0.0153(16) -0.004(2) 0.0007(13) C26 0.0457(17) 0.0314(14) 0.111(3) 0.0095(15) -0.0033(17) 0.0088(12) C27 0.0322(12) 0.0310(12) 0.0465(13) 0.0013(10) 0.0005(10) 0.0026(10) C28 0.0292(12) 0.0320(12) 0.0442(13) -0.0027(10) 0.0031(10) 0.0047(9) C29 0.0637(19) 0.0492(16) 0.0518(16) -0.0071(13) 0.0159(14) -0.0075(14) C30 0.0460(16) 0.0608(18) 0.0634(18) 0.0082(15) -0.0117(14) -0.0013(14) C31 0.097(3) 0.0491(17) 0.0557(17) 0.0075(14) 0.0383(18) 0.0144(17) C32 0.084(3) 0.104(3) 0.084(3) 0.039(2) 0.039(2) 0.015(2) C33 0.066(2) 0.0556(18) 0.0586(18) 0.0093(14) 0.0165(15) -0.0110(15) C34 0.0581(18) 0.0371(14) 0.0672(18) 0.0032(13) 0.0234(15) -0.0113(13) C35 0.0316(13) 0.0503(16) 0.0610(16) 0.0100(13) -0.0101(12) -0.0149(11) C38 0.0335(13) 0.0460(15) 0.0542(15) 0.0179(12) -0.0009(11) -0.0006(11) C37 0.037(4) 0.121(9) 0.057(5) 0.027(6) -0.004(3) 0.016(6) C36A 0.032(4) 0.043(4) 0.056(4) 0.004(3) -0.019(3) -0.008(3) C36 0.036(4) 0.054(5) 0.072(5) 0.013(4) -0.019(3) -0.008(3) C37A 0.039(4) 0.030(3) 0.065(5) 0.015(3) -0.018(3) 0.004(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 N2 1.6908(18) . ? Si1 C6 1.880(2) . ? Si1 Mg1 3.2563(9) . ? Si1 H1CA 1.444(19) . ? Si1 H1B 1.43(2) . ? Mg1 N1 1.9795(19) . ? Mg1 N2 2.0073(18) . ? Mg1 O2 2.0194(16) . ? Mg1 O1 2.0341(17) . ? Mg1 H1 2.35(2) . ? O1 C31 1.448(3) . ? O1 C34 1.465(3) . ? O2 C38 1.461(3) . ? O2 C35 1.461(3) . ? N1 C19 1.383(3) . ? N1 H1 0.976(5) . ? N2 C7 1.429(3) . ? C1 C2 1.390(3) . ? C1 C6 1.403(3) . ? C1 H1C 0.9500 . ? C2 C3 1.375(4) . ? C2 H2 0.9500 . ? C3 C4 1.388(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 C6 1.403(3) . ? C5 H5 0.9500 . ? C7 C15 1.414(3) . ? C7 C8 1.421(3) . ? C8 C12 1.387(3) . ? C8 C9 1.520(3) . ? C9 C11 1.523(4) . ? C9 C10 1.527(4) . ? C9 H9 1.0000 . ? C10 H1C0A 0.9800 . ? C10 H1C0B 0.9800 . ? C10 H1C0C 0.9800 . ? C11 H1C1A 0.9800 . ? C11 H1C1B 0.9800 . ? C11 H1C1C 0.9800 . ? C12 C13 1.380(3) . ? C12 H1C2 0.9500 . ? C13 C14 1.377(3) . ? C13 H1C3 0.9500 . ? C14 C15 1.397(3) . ? C14 H1C4 0.9500 . ? C15 C16 1.522(3) . ? C16 C17 1.524(3) . ? C16 C18 1.525(3) . ? C16 H1C6 1.0000 . ? C17 H1C7A 0.9800 . ? C17 H1C7B 0.9800 . ? C17 H1C7C 0.9800 . ? C18 H1C8A 0.9800 . ? C18 H1C8B 0.9800 . ? C18 H1C8C 0.9800 . ? C19 C27 1.420(3) . ? C19 C20 1.437(3) . ? C20 C24 1.385(3) . ? C20 C21 1.514(3) . ? C21 C22 1.525(4) . ? C21 C23 1.527(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.382(4) . ? C24 H24 0.9500 . ? C25 C26 1.376(4) . ? C25 H25 0.9500 . ? C26 C27 1.390(3) . ? C26 H26 0.9500 . ? C27 C28 1.515(3) . ? C28 C29 1.523(3) . ? C28 C30 1.531(4) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.552(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.425(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.503(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.506(7) . ? C35 C36A 1.536(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C38 C37A 1.496(7) . ? C38 C37 1.530(9) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C37 C36 1.495(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C36A C37A 1.534(8) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C36 H36C 0.9900 . ? C36 H36D 0.9900 . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? 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 Si1 C6 118.09(9) . . ? N2 Si1 Mg1 31.06(6) . . ? C6 Si1 Mg1 127.66(7) . . ? N2 Si1 H1CA 112.7(10) . . ? C6 Si1 H1CA 104.5(10) . . ? Mg1 Si1 H1CA 125.0(10) . . ? N2 Si1 H1B 106.0(10) . . ? C6 Si1 H1B 106.6(10) . . ? Mg1 Si1 H1B 75.0(10) . . ? H1CA Si1 H1B 108.6(14) . . ? N1 Mg1 N2 114.07(8) . . ? N1 Mg1 O2 114.05(7) . . ? N2 Mg1 O2 106.86(7) . . ? N1 Mg1 O1 112.31(8) . . ? N2 Mg1 O1 110.04(8) . . ? O2 Mg1 O1 98.30(7) . . ? N1 Mg1 Si1 139.45(6) . . ? N2 Mg1 Si1 25.76(5) . . ? O2 Mg1 Si1 88.01(5) . . ? O1 Mg1 Si1 96.39(5) . . ? N1 Mg1 H1 24.2(4) . . ? N2 Mg1 H1 91.2(4) . . ? O2 Mg1 H1 132.2(6) . . ? O1 Mg1 H1 116.9(7) . . ? Si1 Mg1 H1 116.9(4) . . ? C31 O1 C34 107.92(19) . . ? C31 O1 Mg1 125.84(15) . . ? C34 O1 Mg1 126.21(14) . . ? C38 O2 C35 109.70(17) . . ? C38 O2 Mg1 119.07(13) . . ? C35 O2 Mg1 130.98(14) . . ? C19 N1 Mg1 146.39(16) . . ? C19 N1 H1 108.6(16) . . ? Mg1 N1 H1 99.6(16) . . ? C7 N2 Si1 119.49(13) . . ? C7 N2 Mg1 117.15(13) . . ? Si1 N2 Mg1 123.18(10) . . ? C2 C1 C6 121.6(2) . . ? C2 C1 H1C 119.2 . . ? C6 C1 H1C 119.2 . . ? C3 C2 C1 119.9(2) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.9(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 121.7(2) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 116.8(2) . . ? C1 C6 Si1 120.71(18) . . ? C5 C6 Si1 122.51(17) . . ? C15 C7 C8 118.54(19) . . ? C15 C7 N2 121.08(18) . . ? C8 C7 N2 120.33(18) . . ? C12 C8 C7 119.4(2) . . ? C12 C8 C9 119.3(2) . . ? C7 C8 C9 121.22(19) . . ? C8 C9 C11 112.7(2) . . ? C8 C9 C10 110.3(2) . . ? C11 C9 C10 111.5(2) . . ? C8 C9 H9 107.3 . . ? C11 C9 H9 107.3 . . ? C10 C9 H9 107.3 . . ? C9 C10 H1C0A 109.5 . . ? C9 C10 H1C0B 109.5 . . ? H1C0A C10 H1C0B 109.5 . . ? C9 C10 H1C0C 109.5 . . ? H1C0A C10 H1C0C 109.5 . . ? H1C0B C10 H1C0C 109.5 . . ? C9 C11 H1C1A 109.5 . . ? C9 C11 H1C1B 109.5 . . ? H1C1A C11 H1C1B 109.5 . . ? C9 C11 H1C1C 109.5 . . ? H1C1A C11 H1C1C 109.5 . . ? H1C1B C11 H1C1C 109.5 . . ? C13 C12 C8 121.9(2) . . ? C13 C12 H1C2 119.1 . . ? C8 C12 H1C2 119.1 . . ? C14 C13 C12 119.1(2) . . ? C14 C13 H1C3 120.5 . . ? C12 C13 H1C3 120.5 . . ? C13 C14 C15 121.6(2) . . ? C13 C14 H1C4 119.2 . . ? C15 C14 H1C4 119.2 . . ? C14 C15 C7 119.5(2) . . ? C14 C15 C16 118.76(19) . . ? C7 C15 C16 121.77(18) . . ? C15 C16 C17 112.04(18) . . ? C15 C16 C18 111.41(18) . . ? C17 C16 C18 110.63(19) . . ? C15 C16 H1C6 107.5 . . ? C17 C16 H1C6 107.5 . . ? C18 C16 H1C6 107.5 . . ? C16 C17 H1C7A 109.5 . . ? C16 C17 H1C7B 109.5 . . ? H1C7A C17 H1C7B 109.5 . . ? C16 C17 H1C7C 109.5 . . ? H1C7A C17 H1C7C 109.5 . . ? H1C7B C17 H1C7C 109.5 . . ? C16 C18 H1C8A 109.5 . . ? C16 C18 H1C8B 109.5 . . ? H1C8A C18 H1C8B 109.5 . . ? C16 C18 H1C8C 109.5 . . ? H1C8A C18 H1C8C 109.5 . . ? H1C8B C18 H1C8C 109.5 . . ? N1 C19 C27 120.7(2) . . ? N1 C19 C20 121.6(2) . . ? C27 C19 C20 117.7(2) . . ? C24 C20 C19 119.8(2) . . ? C24 C20 C21 120.1(2) . . ? C19 C20 C21 120.1(2) . . ? C20 C21 C22 110.9(2) . . ? C20 C21 C23 114.8(2) . . ? C22 C21 C23 109.8(2) . . ? C20 C21 H21 107.0 . . ? C22 C21 H21 107.0 . . ? C23 C21 H21 107.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C20 121.9(3) . . ? C25 C24 H24 119.1 . . ? C20 C24 H24 119.1 . . ? C26 C25 C24 118.6(3) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 122.6(3) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C26 C27 C19 119.4(2) . . ? C26 C27 C28 118.5(2) . . ? C19 C27 C28 122.0(2) . . ? C27 C28 C29 110.6(2) . . ? C27 C28 C30 113.1(2) . . ? C29 C28 C30 109.5(2) . . ? C27 C28 H28 107.8 . . ? C29 C28 H28 107.8 . . ? C30 C28 H28 107.8 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 C31 C32 102.7(3) . . ? O1 C31 H31A 111.2 . . ? C32 C31 H31A 111.2 . . ? O1 C31 H31B 111.2 . . ? C32 C31 H31B 111.2 . . ? H31A C31 H31B 109.1 . . ? C33 C32 C31 102.3(3) . . ? C33 C32 H32A 111.3 . . ? C31 C32 H32A 111.3 . . ? C33 C32 H32B 111.3 . . ? C31 C32 H32B 111.3 . . ? H32A C32 H32B 109.2 . . ? C32 C33 C34 104.8(3) . . ? C32 C33 H33A 110.8 . . ? C34 C33 H33A 110.8 . . ? C32 C33 H33B 110.8 . . ? C34 C33 H33B 110.8 . . ? H33A C33 H33B 108.9 . . ? O1 C34 C33 105.7(2) . . ? O1 C34 H34A 110.6 . . ? C33 C34 H34A 110.6 . . ? O1 C34 H34B 110.6 . . ? C33 C34 H34B 110.6 . . ? H34A C34 H34B 108.7 . . ? O2 C35 C36 107.2(3) . . ? O2 C35 C36A 101.5(3) . . ? C36 C35 C36A 26.1(3) . . ? O2 C35 H35A 110.3 . . ? C36 C35 H35A 110.3 . . ? C36A C35 H35A 89.5 . . ? O2 C35 H35B 110.3 . . ? C36 C35 H35B 110.3 . . ? C36A C35 H35B 134.1 . . ? H35A C35 H35B 108.5 . . ? O2 C38 C37A 104.9(4) . . ? O2 C38 C37 103.7(4) . . ? C37A C38 C37 25.0(4) . . ? O2 C38 H38A 111.0 . . ? C37A C38 H38A 87.9 . . ? C37 C38 H38A 111.0 . . ? O2 C38 H38B 111.0 . . ? C37A C38 H38B 130.3 . . ? C37 C38 H38B 111.0 . . ? H38A C38 H38B 109.0 . . ? C36 C37 C38 106.0(6) . . ? C36 C37 H37A 110.5 . . ? C38 C37 H37A 110.5 . . ? C36 C37 H37B 110.5 . . ? C38 C37 H37B 110.5 . . ? H37A C37 H37B 108.7 . . ? C37A C36A C35 101.1(5) . . ? C37A C36A H36A 111.6 . . ? C35 C36A H36A 111.6 . . ? C37A C36A H36B 111.6 . . ? C35 C36A H36B 111.6 . . ? H36A C36A H36B 109.4 . . ? C37 C36 C35 102.0(5) . . ? C37 C36 H36C 111.4 . . ? C35 C36 H36C 111.4 . . ? C37 C36 H36D 111.4 . . ? C35 C36 H36D 111.4 . . ? H36C C36 H36D 109.2 . . ? C38 C37A C36A 98.6(5) . . ? C38 C37A H37C 112.1 . . ? C36A C37A H37C 112.1 . . ? C38 C37A H37D 112.1 . . ? C36A C37A H37D 112.1 . . ? H37C C37A H37D 109.7 . . ? 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 Si1 Mg1 N1 -11.81(15) . . . . ? C6 Si1 Mg1 N1 70.80(13) . . . . ? C6 Si1 Mg1 N2 82.61(15) . . . . ? N2 Si1 Mg1 O2 -137.73(13) . . . . ? C6 Si1 Mg1 O2 -55.12(10) . . . . ? N2 Si1 Mg1 O1 124.14(13) . . . . ? C6 Si1 Mg1 O1 -153.25(10) . . . . ? N1 Mg1 O1 C31 -26.2(2) . . . . ? N2 Mg1 O1 C31 -154.4(2) . . . . ? O2 Mg1 O1 C31 94.2(2) . . . . ? Si1 Mg1 O1 C31 -176.9(2) . . . . ? N1 Mg1 O1 C34 151.3(2) . . . . ? N2 Mg1 O1 C34 23.0(2) . . . . ? O2 Mg1 O1 C34 -88.4(2) . . . . ? Si1 Mg1 O1 C34 0.5(2) . . . . ? N1 Mg1 O2 C38 -55.07(18) . . . . ? N2 Mg1 O2 C38 71.94(17) . . . . ? O1 Mg1 O2 C38 -174.10(16) . . . . ? Si1 Mg1 O2 C38 89.73(16) . . . . ? N1 Mg1 O2 C35 131.3(2) . . . . ? N2 Mg1 O2 C35 -101.7(2) . . . . ? O1 Mg1 O2 C35 12.3(2) . . . . ? Si1 Mg1 O2 C35 -83.9(2) . . . . ? N2 Mg1 N1 C19 -127.0(3) . . . . ? O2 Mg1 N1 C19 -3.9(3) . . . . ? O1 Mg1 N1 C19 106.9(3) . . . . ? Si1 Mg1 N1 C19 -121.5(3) . . . . ? C6 Si1 N2 C7 67.78(18) . . . . ? Mg1 Si1 N2 C7 -175.1(2) . . . . ? C6 Si1 N2 Mg1 -117.14(12) . . . . ? N1 Mg1 N2 C7 -13.19(18) . . . . ? O2 Mg1 N2 C7 -140.19(14) . . . . ? O1 Mg1 N2 C7 114.08(15) . . . . ? Si1 Mg1 N2 C7 175.2(2) . . . . ? N1 Mg1 N2 Si1 171.62(11) . . . . ? O2 Mg1 N2 Si1 44.62(13) . . . . ? O1 Mg1 N2 Si1 -61.11(13) . . . . ? C6 C1 C2 C3 -1.1(4) . . . . ? C1 C2 C3 C4 1.4(4) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C2 C1 C6 C5 0.0(3) . . . . ? C2 C1 C6 Si1 179.53(18) . . . . ? C4 C5 C6 C1 1.0(3) . . . . ? C4 C5 C6 Si1 -178.54(19) . . . . ? N2 Si1 C6 C1 -107.36(18) . . . . ? Mg1 Si1 C6 C1 -142.81(15) . . . . ? N2 Si1 C6 C5 72.2(2) . . . . ? Mg1 Si1 C6 C5 36.7(2) . . . . ? Si1 N2 C7 C15 -93.9(2) . . . . ? Mg1 N2 C7 C15 90.7(2) . . . . ? Si1 N2 C7 C8 88.8(2) . . . . ? Mg1 N2 C7 C8 -86.6(2) . . . . ? C15 C7 C8 C12 -2.5(3) . . . . ? N2 C7 C8 C12 174.88(19) . . . . ? C15 C7 C8 C9 179.88(19) . . . . ? N2 C7 C8 C9 -2.7(3) . . . . ? C12 C8 C9 C11 54.4(3) . . . . ? C7 C8 C9 C11 -128.0(3) . . . . ? C12 C8 C9 C10 -71.0(3) . . . . ? C7 C8 C9 C10 106.6(3) . . . . ? C7 C8 C12 C13 1.0(3) . . . . ? C9 C8 C12 C13 178.7(2) . . . . ? C8 C12 C13 C14 0.8(4) . . . . ? C12 C13 C14 C15 -1.2(3) . . . . ? C13 C14 C15 C7 -0.4(3) . . . . ? C13 C14 C15 C16 -179.8(2) . . . . ? C8 C7 C15 C14 2.2(3) . . . . ? N2 C7 C15 C14 -175.19(19) . . . . ? C8 C7 C15 C16 -178.38(18) . . . . ? N2 C7 C15 C16 4.2(3) . . . . ? C14 C15 C16 C17 -58.5(3) . . . . ? C7 C15 C16 C17 122.1(2) . . . . ? C14 C15 C16 C18 66.0(3) . . . . ? C7 C15 C16 C18 -113.4(2) . . . . ? Mg1 N1 C19 C27 -40.9(4) . . . . ? Mg1 N1 C19 C20 139.3(2) . . . . ? N1 C19 C20 C24 -177.4(2) . . . . ? C27 C19 C20 C24 2.9(3) . . . . ? N1 C19 C20 C21 4.4(3) . . . . ? C27 C19 C20 C21 -175.3(2) . . . . ? C24 C20 C21 C22 -104.0(3) . . . . ? C19 C20 C21 C22 74.2(3) . . . . ? C24 C20 C21 C23 21.2(3) . . . . ? C19 C20 C21 C23 -160.6(2) . . . . ? C19 C20 C24 C25 -2.7(4) . . . . ? C21 C20 C24 C25 175.5(3) . . . . ? C20 C24 C25 C26 0.5(6) . . . . ? C24 C25 C26 C27 1.5(6) . . . . ? C25 C26 C27 C19 -1.1(5) . . . . ? C25 C26 C27 C28 -177.9(3) . . . . ? N1 C19 C27 C26 179.2(2) . . . . ? C20 C19 C27 C26 -1.0(4) . . . . ? N1 C19 C27 C28 -4.1(3) . . . . ? C20 C19 C27 C28 175.6(2) . . . . ? C26 C27 C28 C29 74.2(3) . . . . ? C19 C27 C28 C29 -102.5(3) . . . . ? C26 C27 C28 C30 -49.0(3) . . . . ? C19 C27 C28 C30 134.2(2) . . . . ? C34 O1 C31 C32 23.6(3) . . . . ? Mg1 O1 C31 C32 -158.6(2) . . . . ? O1 C31 C32 C33 -39.0(4) . . . . ? C31 C32 C33 C34 38.7(4) . . . . ? C31 O1 C34 C33 -0.6(3) . . . . ? Mg1 O1 C34 C33 -178.40(19) . . . . ? C32 C33 C34 O1 -25.0(4) . . . . ? C38 O2 C35 C36 10.8(4) . . . . ? Mg1 O2 C35 C36 -175.1(4) . . . . ? C38 O2 C35 C36A -15.5(4) . . . . ? Mg1 O2 C35 C36A 158.6(3) . . . . ? C35 O2 C38 C37A -15.4(4) . . . . ? Mg1 O2 C38 C37A 169.7(3) . . . . ? C35 O2 C38 C37 10.4(4) . . . . ? Mg1 O2 C38 C37 -164.5(4) . . . . ? O2 C38 C37 C36 -28.0(7) . . . . ? C37A C38 C37 C36 68.1(13) . . . . ? O2 C35 C36A C37A 39.6(5) . . . . ? C36 C35 C36A C37A -66.2(11) . . . . ? C38 C37 C36 C35 34.0(8) . . . . ? O2 C35 C36 C37 -27.6(7) . . . . ? C36A C35 C36 C37 53.3(10) . . . . ? O2 C38 C37A C36A 39.2(6) . . . . ? C37 C38 C37A C36A -51.2(12) . . . . ? C35 C36A C37A C38 -48.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.156 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.084 _database_code_depnum_ccdc_archive 'CCDC 945786' ####################################################################### # # 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_k12msh24-new _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H68 Mg N2 O3.50 Si' _chemical_formula_weight 733.40 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.0310(1) _cell_length_b 30.0170(5) _cell_length_c 16.5560(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.903(1) _cell_angle_gamma 90.00 _cell_volume 4817.34(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 68142 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.098 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _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 ? _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 10746 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1093 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.44 _reflns_number_total 10746 _reflns_number_gt 5593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. H1a, attached to Si1 was located and refined freely. Some disorder was present. In particular, c36/37 were disordered over 2 sites in a 50:50 ratio, while C41 was similarly fragmented bit in a 70:30 ratio. The unit cell was seen to contain 2 areas of diffuse solvent which could not be modelled in any plausible manner. Hence PLATON SQUEEZE was employed to treat these regions. Based on pre-PLATON electron density and the results for the SQUEEZE analysis, guest solvent has been included in the asymmetric unit as 1/2 of a THF molecule. ; _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^)+(0.1408P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10746 _refine_ls_number_parameters 481 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.1607 _refine_ls_R_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.2434 _refine_ls_wR_factor_gt 0.2128 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.978 _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 0.19007(8) 0.15231(3) 0.71264(5) 0.0304(2) Uani 1 1 d . . . Mg1 Mg 0.45156(9) 0.14555(3) 0.81157(6) 0.0315(3) Uani 1 1 d . . . O1 O 0.5400(2) 0.10870(7) 0.92452(14) 0.0432(6) Uani 1 1 d . B . O2 O 0.5951(2) 0.11516(7) 0.76091(14) 0.0400(6) Uani 1 1 d . D . O3 O 0.5621(2) 0.19772(7) 0.87955(14) 0.0441(6) Uani 1 1 d . . . N1 N 0.2675(2) 0.11238(8) 0.78153(15) 0.0309(6) Uani 1 1 d . . . N2 N 0.3263(2) 0.18690(8) 0.71984(15) 0.0325(6) Uani 1 1 d . . . C1 C 0.1929(3) 0.08441(11) 0.82222(18) 0.0331(7) Uani 1 1 d . . . C2 C 0.1572(3) 0.04034(11) 0.79302(19) 0.0355(7) Uani 1 1 d . . . C3 C 0.1908(3) 0.02256(10) 0.7149(2) 0.0376(7) Uani 1 1 d . . . H3 H 0.2426 0.0465 0.6939 0.045 Uiso 1 1 calc R . . C4 C 0.0592(3) 0.01329(12) 0.6456(2) 0.0454(8) Uani 1 1 d . . . H4A H 0.0042 -0.0095 0.6646 0.068 Uiso 1 1 calc R . . H4B H 0.0842 0.0027 0.5955 0.068 Uiso 1 1 calc R . . H4C H 0.0051 0.0408 0.6325 0.068 Uiso 1 1 calc R . . C5 C 0.2841(4) -0.01840(13) 0.7322(3) 0.0588(10) Uani 1 1 d . . . H5A H 0.3688 -0.0112 0.7750 0.088 Uiso 1 1 calc R . . H5B H 0.3076 -0.0275 0.6806 0.088 Uiso 1 1 calc R . . H5C H 0.2359 -0.0428 0.7520 0.088 Uiso 1 1 calc R . . C6 C 0.0855(3) 0.01253(12) 0.8353(2) 0.0445(8) Uani 1 1 d . . . H6 H 0.0619 -0.0168 0.8149 0.053 Uiso 1 1 calc R . . C7 C 0.0485(4) 0.02656(15) 0.9052(2) 0.0598(11) Uani 1 1 d . . . H7 H 0.0005 0.0073 0.9334 0.072 Uiso 1 1 calc R . . C8 C 0.0830(4) 0.07009(15) 0.9342(2) 0.0576(11) Uani 1 1 d . . . H8 H 0.0566 0.0801 0.9823 0.069 Uiso 1 1 calc R . . C9 C 0.1535(3) 0.09863(12) 0.8954(2) 0.0431(8) Uani 1 1 d . . . C10 C 0.1858(4) 0.14529(14) 0.9290(2) 0.0551(10) Uani 1 1 d . . . H10 H 0.2434 0.1599 0.8954 0.066 Uiso 1 1 calc R . . C11 C 0.0538(4) 0.17372(14) 0.9190(3) 0.0666(12) Uani 1 1 d . . . H11A H -0.0045 0.1605 0.9519 0.100 Uiso 1 1 calc R . . H11B H 0.0030 0.1746 0.8599 0.100 Uiso 1 1 calc R . . H11C H 0.0795 0.2041 0.9388 0.100 Uiso 1 1 calc R . . C12 C 0.2677(4) 0.14623(18) 1.0199(2) 0.0800(15) Uani 1 1 d . . . H12A H 0.2148 0.1315 1.0544 0.120 Uiso 1 1 calc R . . H12B H 0.2856 0.1772 1.0381 0.120 Uiso 1 1 calc R . . H12C H 0.3555 0.1306 1.0258 0.120 Uiso 1 1 calc R . . C13 C 0.1037(3) 0.13282(10) 0.60299(19) 0.0339(7) Uani 1 1 d . . . C14 C 0.1681(4) 0.11057(12) 0.5506(2) 0.0457(9) Uani 1 1 d . . . H14 H 0.2638 0.1041 0.5698 0.055 Uiso 1 1 calc R . . C15 C 0.0972(4) 0.09734(14) 0.4703(2) 0.0587(10) Uani 1 1 d . . . H15 H 0.1446 0.0819 0.4361 0.070 Uiso 1 1 calc R . . C16 C -0.0407(5) 0.10656(13) 0.4405(2) 0.0627(11) Uani 1 1 d . . . H16 H -0.0887 0.0978 0.3855 0.075 Uiso 1 1 calc R . . C17 C -0.1080(4) 0.12835(13) 0.4902(3) 0.0604(11) Uani 1 1 d . . . H17 H -0.2037 0.1346 0.4702 0.073 Uiso 1 1 calc R . . C18 C -0.0366(3) 0.14167(11) 0.5708(2) 0.0440(8) Uani 1 1 d . . . H18 H -0.0850 0.1571 0.6046 0.053 Uiso 1 1 calc R . . C19 C 0.3415(3) 0.22926(10) 0.6889(2) 0.0368(8) Uani 1 1 d . . . C20 C 0.4365(3) 0.23706(12) 0.6398(2) 0.0453(9) Uani 1 1 d . . . C21 C 0.5100(3) 0.19812(13) 0.6102(2) 0.0501(10) Uani 1 1 d . . . H21 H 0.5076 0.1721 0.6476 0.060 Uiso 1 1 calc R . . C22 C 0.4350(4) 0.18506(15) 0.5224(3) 0.0632(11) Uani 1 1 d . . . H22A H 0.3409 0.1758 0.5212 0.095 Uiso 1 1 calc R . . H22B H 0.4837 0.1603 0.5038 0.095 Uiso 1 1 calc R . . H22C H 0.4316 0.2106 0.4850 0.095 Uiso 1 1 calc R . . C23 C 0.6613(4) 0.20741(18) 0.6126(3) 0.0857(16) Uani 1 1 d . . . H23A H 0.6657 0.2276 0.5668 0.129 Uiso 1 1 calc R . . H23B H 0.7076 0.1794 0.6063 0.129 Uiso 1 1 calc R . . H23C H 0.7074 0.2212 0.6661 0.129 Uiso 1 1 calc R . . C24 C 0.4598(4) 0.28047(14) 0.6153(3) 0.0608(11) Uani 1 1 d . . . H24 H 0.5254 0.2850 0.5837 0.073 Uiso 1 1 calc R . . C25 C 0.3925(5) 0.31599(14) 0.6351(3) 0.0687(12) Uani 1 1 d . . . H25 H 0.4103 0.3451 0.6177 0.082 Uiso 1 1 calc R . . C26 C 0.2982(4) 0.30938(13) 0.6805(3) 0.0626(11) Uani 1 1 d . . . H26 H 0.2493 0.3344 0.6932 0.075 Uiso 1 1 calc R . . C27 C 0.2702(3) 0.26732(11) 0.7093(2) 0.0432(8) Uani 1 1 d . . . C28 C 0.1641(3) 0.26283(12) 0.7599(2) 0.0482(9) Uani 1 1 d . . . H28 H 0.1763 0.2330 0.7877 0.058 Uiso 1 1 calc R . . C29 C 0.0175(4) 0.26513(14) 0.7012(3) 0.0645(12) Uani 1 1 d . . . H29A H 0.0020 0.2947 0.6755 0.097 Uiso 1 1 calc R . . H29B H -0.0503 0.2596 0.7334 0.097 Uiso 1 1 calc R . . H29C H 0.0077 0.2425 0.6574 0.097 Uiso 1 1 calc R . . C30 C 0.1788(4) 0.29870(14) 0.8277(3) 0.0695(12) Uani 1 1 d . . . H30A H 0.2735 0.2987 0.8632 0.104 Uiso 1 1 calc R . . H30B H 0.1146 0.2924 0.8620 0.104 Uiso 1 1 calc R . . H30C H 0.1577 0.3280 0.8013 0.104 Uiso 1 1 calc R . . C31 C 0.6520(4) 0.22711(12) 0.8487(2) 0.0528(10) Uani 1 1 d . . . H31A H 0.6344 0.2244 0.7872 0.063 Uiso 1 1 calc R . . H31B H 0.7499 0.2198 0.8745 0.063 Uiso 1 1 calc R . . C32 C 0.6189(4) 0.27370(12) 0.8726(3) 0.0641(12) Uani 1 1 d . . . H32A H 0.6999 0.2936 0.8804 0.077 Uiso 1 1 calc R . . H32B H 0.5406 0.2867 0.8301 0.077 Uiso 1 1 calc R . . C33 C 0.5820(4) 0.26559(13) 0.9534(3) 0.0635(11) Uani 1 1 d . . . H33A H 0.5262 0.2903 0.9670 0.076 Uiso 1 1 calc R . . H33B H 0.6654 0.2615 1.0001 0.076 Uiso 1 1 calc R . . C34 C 0.4984(4) 0.22289(13) 0.9348(3) 0.0594(11) Uani 1 1 d . . . H34A H 0.5028 0.2061 0.9869 0.071 Uiso 1 1 calc R . . H34B H 0.4006 0.2295 0.9070 0.071 Uiso 1 1 calc R . . C35 C 0.6523(4) 0.12004(13) 0.9953(2) 0.0551(10) Uani 1 1 d . . . H35A H 0.7245 0.1361 0.9758 0.066 Uiso 1 1 calc R A 1 H35B H 0.6185 0.1400 1.0333 0.066 Uiso 1 1 calc R A 1 C36 C 0.7085(16) 0.0814(5) 1.0385(10) 0.072(5) Uani 0.50 1 d PDU B 1 H36A H 0.7231 0.0858 1.0994 0.086 Uiso 0.50 1 calc PR B 1 H36B H 0.7986 0.0745 1.0272 0.086 Uiso 0.50 1 calc PR B 1 C37 C 0.6139(10) 0.0457(3) 1.0104(6) 0.061(3) Uani 0.50 1 d PDU B 1 H37A H 0.5594 0.0398 1.0513 0.073 Uiso 0.50 1 calc PR B 1 H37B H 0.6641 0.0182 1.0032 0.073 Uiso 0.50 1 calc PR B 1 C38 C 0.5173(4) 0.06081(12) 0.9249(3) 0.0590(10) Uani 1 1 d . . . H38A H 0.5435 0.0462 0.8775 0.071 Uiso 1 1 calc R B 1 H38B H 0.4197 0.0539 0.9218 0.071 Uiso 1 1 calc R B 1 C39 C 0.7449(3) 0.11882(13) 0.7868(3) 0.0554(10) Uani 1 1 d . D . H39A H 0.7798 0.1119 0.8470 0.066 Uiso 1 1 calc R . . H39B H 0.7745 0.1493 0.7767 0.066 Uiso 1 1 calc R . . C40 C 0.7972(4) 0.08636(16) 0.7360(3) 0.0760(14) Uani 1 1 d D . . H40A H 0.8718 0.1001 0.7152 0.091 Uiso 0.60 1 calc PR C 1 H40B H 0.8361 0.0603 0.7708 0.091 Uiso 0.60 1 calc PR C 1 H40C H 0.8144 0.1008 0.6859 0.091 Uiso 0.40 1 calc PR C 2 H40D H 0.8842 0.0727 0.7689 0.091 Uiso 0.40 1 calc PR C 2 C41 C 0.6883(5) 0.05290(18) 0.7124(4) 0.0586(15) Uani 0.70 1 d PDU D 2 H41A H 0.6934 0.0311 0.7579 0.070 Uiso 0.70 1 calc PR D 2 H41B H 0.6938 0.0368 0.6611 0.070 Uiso 0.70 1 calc PR D 2 C42 C 0.5574(4) 0.08059(13) 0.6972(2) 0.0548(10) Uani 1 1 d . . . H42A H 0.4804 0.0907 0.6505 0.066 Uiso 1 1 calc R D 1 H42B H 0.5289 0.0531 0.7212 0.066 Uiso 1 1 calc R D 1 C36A C 0.7345(14) 0.0750(5) 1.0164(10) 0.066(4) Uani 0.55 1 d PDU B 2 H36C H 0.8226 0.0767 1.0000 0.079 Uiso 0.50 1 calc PR B 2 H36D H 0.7554 0.0688 1.0771 0.079 Uiso 0.50 1 calc PR B 2 C37A C 0.6483(11) 0.0402(4) 0.9700(8) 0.075(3) Uani 0.50 1 d PDU B 2 H37C H 0.6313 0.0170 1.0086 0.091 Uiso 0.50 1 calc PR B 2 H37D H 0.6939 0.0262 0.9301 0.091 Uiso 0.50 1 calc PR B 2 C41A C 0.6876(10) 0.0722(5) 0.6668(7) 0.062(4) Uani 0.30 1 d PDU D 1 H41C H 0.6968 0.0403 0.6544 0.074 Uiso 0.30 1 calc PR D 1 H41D H 0.6860 0.0899 0.6162 0.074 Uiso 0.30 1 calc PR D 1 H1A H 0.070(3) 0.1695(9) 0.7350(17) 0.031(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0217(4) 0.0407(5) 0.0291(4) -0.0039(4) 0.0070(3) -0.0002(3) Mg1 0.0229(5) 0.0371(6) 0.0325(6) -0.0010(5) 0.0035(4) -0.0001(4) O1 0.0394(13) 0.0459(14) 0.0368(13) 0.0059(11) -0.0038(10) -0.0059(10) O2 0.0235(11) 0.0491(13) 0.0469(14) -0.0016(11) 0.0083(10) 0.0039(9) O3 0.0362(13) 0.0418(13) 0.0489(14) -0.0052(11) 0.0011(11) -0.0032(10) N1 0.0222(13) 0.0416(15) 0.0293(14) 0.0010(11) 0.0071(11) -0.0023(11) N2 0.0250(13) 0.0354(14) 0.0355(15) 0.0000(11) 0.0049(11) 0.0001(10) C1 0.0211(16) 0.0494(19) 0.0281(16) 0.0018(14) 0.0051(13) -0.0012(13) C2 0.0287(17) 0.0445(19) 0.0323(17) 0.0075(15) 0.0063(14) -0.0020(14) C3 0.0340(18) 0.0375(18) 0.0428(19) 0.0013(15) 0.0123(15) -0.0022(14) C4 0.045(2) 0.049(2) 0.040(2) -0.0023(16) 0.0065(17) -0.0069(16) C5 0.056(2) 0.058(2) 0.061(3) -0.004(2) 0.010(2) 0.0161(18) C6 0.0354(19) 0.050(2) 0.046(2) 0.0099(17) 0.0055(16) -0.0036(15) C7 0.054(2) 0.081(3) 0.049(2) 0.015(2) 0.023(2) -0.019(2) C8 0.049(2) 0.096(3) 0.033(2) -0.005(2) 0.0201(18) -0.016(2) C9 0.0351(19) 0.066(2) 0.0292(17) -0.0102(17) 0.0097(15) -0.0147(16) C10 0.043(2) 0.087(3) 0.041(2) -0.024(2) 0.0208(17) -0.0210(19) C11 0.064(3) 0.079(3) 0.067(3) -0.033(2) 0.036(2) -0.013(2) C12 0.069(3) 0.133(4) 0.041(2) -0.030(3) 0.019(2) -0.032(3) C13 0.0295(17) 0.0366(17) 0.0340(17) 0.0036(14) 0.0052(14) -0.0022(13) C14 0.043(2) 0.058(2) 0.0335(19) -0.0049(16) 0.0050(16) 0.0053(16) C15 0.072(3) 0.068(3) 0.031(2) -0.0126(18) 0.0036(19) 0.009(2) C16 0.076(3) 0.056(2) 0.040(2) -0.0037(19) -0.015(2) -0.001(2) C17 0.050(2) 0.057(2) 0.058(3) 0.000(2) -0.015(2) -0.0005(19) C18 0.0353(19) 0.0428(19) 0.046(2) -0.0021(16) -0.0032(16) -0.0008(14) C19 0.0259(16) 0.0391(18) 0.0384(18) 0.0034(14) -0.0043(14) 0.0027(13) C20 0.0321(18) 0.055(2) 0.042(2) 0.0147(17) -0.0017(16) -0.0001(15) C21 0.0333(19) 0.068(2) 0.053(2) 0.0297(19) 0.0182(17) 0.0123(17) C22 0.047(2) 0.076(3) 0.070(3) 0.008(2) 0.023(2) 0.014(2) C23 0.038(2) 0.142(5) 0.081(3) 0.027(3) 0.021(2) 0.015(3) C24 0.057(2) 0.062(3) 0.059(3) 0.029(2) 0.005(2) -0.003(2) C25 0.074(3) 0.048(2) 0.075(3) 0.024(2) 0.002(3) -0.002(2) C26 0.063(3) 0.043(2) 0.065(3) 0.005(2) -0.014(2) 0.0148(19) C27 0.0354(19) 0.0411(19) 0.045(2) 0.0002(16) -0.0052(16) 0.0066(14) C28 0.0354(19) 0.050(2) 0.053(2) -0.0136(18) 0.0005(17) 0.0072(15) C29 0.036(2) 0.067(3) 0.079(3) -0.019(2) -0.006(2) 0.0124(18) C30 0.064(3) 0.061(3) 0.078(3) -0.028(2) 0.008(2) 0.010(2) C31 0.046(2) 0.055(2) 0.051(2) 0.0053(18) 0.0015(18) -0.0173(17) C32 0.064(3) 0.042(2) 0.069(3) 0.007(2) -0.017(2) -0.0091(18) C33 0.056(2) 0.045(2) 0.079(3) -0.018(2) -0.002(2) -0.0015(18) C34 0.041(2) 0.060(2) 0.072(3) -0.024(2) 0.005(2) -0.0007(18) C35 0.045(2) 0.068(3) 0.041(2) 0.0039(19) -0.0095(17) -0.0042(18) C36 0.076(8) 0.065(7) 0.058(7) -0.001(5) -0.013(6) -0.003(6) C37 0.052(5) 0.056(5) 0.064(6) 0.018(5) -0.008(4) -0.002(4) C38 0.058(2) 0.051(2) 0.059(3) 0.0121(19) -0.001(2) -0.0105(18) C39 0.0219(18) 0.073(3) 0.069(3) -0.003(2) 0.0070(17) 0.0027(17) C40 0.045(2) 0.093(3) 0.099(4) -0.001(3) 0.034(3) 0.013(2) C41 0.070(4) 0.058(3) 0.046(3) -0.006(3) 0.010(3) 0.024(3) C42 0.038(2) 0.063(2) 0.062(3) -0.018(2) 0.0117(19) -0.0005(17) C36A 0.053(5) 0.065(6) 0.073(8) 0.006(5) 0.002(5) 0.002(4) C37A 0.069(6) 0.069(6) 0.080(7) 0.002(5) 0.003(5) 0.016(5) C41A 0.068(7) 0.068(7) 0.049(7) -0.005(6) 0.016(6) 0.017(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 Si1 N2 1.696(2) . ? Si1 N1 1.699(3) . ? Si1 C13 1.892(3) . ? Si1 Mg1 2.7193(12) . ? Si1 H1A 1.44(3) . ? Mg1 N1 2.044(2) . ? Mg1 O2 2.057(2) . ? Mg1 O3 2.075(2) . ? Mg1 N2 2.108(3) . ? Mg1 O1 2.157(2) . ? O1 C35 1.442(4) . ? O1 C38 1.456(4) . ? O2 C39 1.457(4) . ? O2 C42 1.458(4) . ? O3 C31 1.445(4) . ? O3 C34 1.455(4) . ? N1 C1 1.406(4) . ? N2 C19 1.394(4) . ? C1 C2 1.422(4) . ? C1 C9 1.433(4) . ? C2 C6 1.401(4) . ? C2 C3 1.515(4) . ? C3 C5 1.527(5) . ? C3 C4 1.535(4) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.369(5) . ? C6 H6 0.9500 . ? C7 C8 1.405(5) . ? C7 H7 0.9500 . ? C8 C9 1.371(5) . ? C8 H8 0.9500 . ? C9 C10 1.511(5) . ? C10 C12 1.517(5) . ? C10 C11 1.547(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.380(4) . ? C13 C18 1.397(4) . ? C14 C15 1.395(5) . ? C14 H14 0.9500 . ? C15 C16 1.372(5) . ? C15 H15 0.9500 . ? C16 C17 1.359(6) . ? C16 H16 0.9500 . ? C17 C18 1.402(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.422(5) . ? C19 C27 1.433(4) . ? C20 C24 1.402(5) . ? C20 C21 1.528(5) . ? C21 C22 1.507(5) . ? C21 C23 1.534(5) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.346(6) . ? C24 H24 0.9500 . ? C25 C26 1.366(6) . ? C25 H25 0.9500 . ? C26 C27 1.403(5) . ? C26 H26 0.9500 . ? C27 C28 1.520(5) . ? C28 C30 1.536(5) . ? C28 C29 1.542(5) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.513(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.498(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.519(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.402(18) . ? C35 C36A 1.577(17) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.427(12) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.563(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C37A 1.470(11) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.469(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41A 1.433(5) . ? C40 C41 1.462(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 H40C 0.9900 . ? C40 H40D 0.9900 . ? C41 C42 1.519(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C41A 1.536(13) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C36A C37A 1.443(11) . ? C36A H36C 0.9900 . ? C36A H36D 0.9900 . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? C41A H41C 0.9900 . ? C41A H41D 0.9900 . ? 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 Si1 N1 99.43(12) . . ? N2 Si1 C13 114.75(13) . . ? N1 Si1 C13 116.33(13) . . ? N2 Si1 Mg1 50.82(9) . . ? N1 Si1 Mg1 48.65(8) . . ? C13 Si1 Mg1 133.43(10) . . ? N2 Si1 H1A 118.3(11) . . ? N1 Si1 H1A 110.3(11) . . ? C13 Si1 H1A 98.6(11) . . ? Mg1 Si1 H1A 127.7(11) . . ? N1 Mg1 O2 111.61(10) . . ? N1 Mg1 O3 145.39(10) . . ? O2 Mg1 O3 102.90(9) . . ? N1 Mg1 N2 77.15(10) . . ? O2 Mg1 N2 108.51(10) . . ? O3 Mg1 N2 94.75(10) . . ? N1 Mg1 O1 96.05(10) . . ? O2 Mg1 O1 87.20(9) . . ? O3 Mg1 O1 82.74(9) . . ? N2 Mg1 O1 164.22(10) . . ? N1 Mg1 Si1 38.60(7) . . ? O2 Mg1 Si1 117.10(8) . . ? O3 Mg1 Si1 124.64(7) . . ? N2 Mg1 Si1 38.58(7) . . ? O1 Mg1 Si1 132.70(7) . . ? C35 O1 C38 108.7(3) . . ? C35 O1 Mg1 130.1(2) . . ? C38 O1 Mg1 118.7(2) . . ? C39 O2 C42 108.8(2) . . ? C39 O2 Mg1 128.6(2) . . ? C42 O2 Mg1 122.12(17) . . ? C31 O3 C34 108.7(3) . . ? C31 O3 Mg1 124.3(2) . . ? C34 O3 Mg1 118.22(19) . . ? C1 N1 Si1 122.38(19) . . ? C1 N1 Mg1 137.1(2) . . ? Si1 N1 Mg1 92.75(11) . . ? C19 N2 Si1 134.0(2) . . ? C19 N2 Mg1 134.47(19) . . ? Si1 N2 Mg1 90.60(11) . . ? N1 C1 C2 120.7(3) . . ? N1 C1 C9 121.6(3) . . ? C2 C1 C9 117.7(3) . . ? C6 C2 C1 120.1(3) . . ? C6 C2 C3 118.1(3) . . ? C1 C2 C3 121.7(3) . . ? C2 C3 C5 112.6(3) . . ? C2 C3 C4 111.4(3) . . ? C5 C3 C4 111.2(3) . . ? C2 C3 H3 107.1 . . ? C5 C3 H3 107.1 . . ? C4 C3 H3 107.1 . . ? 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 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 121.6(3) . . ? C7 C6 H6 119.2 . . ? C2 C6 H6 119.2 . . ? C6 C7 C8 118.6(3) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C9 C8 C7 122.1(3) . . ? C9 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C8 C9 C1 119.9(3) . . ? C8 C9 C10 119.6(3) . . ? C1 C9 C10 120.5(3) . . ? C9 C10 C12 113.1(4) . . ? C9 C10 C11 112.0(3) . . ? C12 C10 C11 109.1(3) . . ? C9 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 116.2(3) . . ? C14 C13 Si1 125.5(2) . . ? C18 C13 Si1 118.3(2) . . ? C13 C14 C15 122.0(3) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C16 C15 C14 120.4(4) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.4(4) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.2(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 121.8(3) . . ? C13 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? N2 C19 C20 120.9(3) . . ? N2 C19 C27 122.2(3) . . ? C20 C19 C27 116.9(3) . . ? C24 C20 C19 120.3(3) . . ? C24 C20 C21 119.2(3) . . ? C19 C20 C21 120.5(3) . . ? C22 C21 C20 110.2(3) . . ? C22 C21 C23 108.5(3) . . ? C20 C21 C23 114.1(3) . . ? C22 C21 H21 107.9 . . ? C20 C21 H21 107.9 . . ? C23 C21 H21 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C20 122.3(4) . . ? C25 C24 H24 118.8 . . ? C20 C24 H24 118.8 . . ? C24 C25 C26 118.7(4) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? C25 C26 C27 123.0(4) . . ? C25 C26 H26 118.5 . . ? C27 C26 H26 118.5 . . ? C26 C27 C19 118.8(3) . . ? C26 C27 C28 119.8(3) . . ? C19 C27 C28 121.4(3) . . ? C27 C28 C30 113.1(3) . . ? C27 C28 C29 109.8(3) . . ? C30 C28 C29 109.0(3) . . ? C27 C28 H28 108.3 . . ? C30 C28 H28 108.3 . . ? C29 C28 H28 108.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 C31 C32 105.8(3) . . ? O3 C31 H31A 110.6 . . ? C32 C31 H31A 110.6 . . ? O3 C31 H31B 110.6 . . ? C32 C31 H31B 110.6 . . ? H31A C31 H31B 108.7 . . ? C33 C32 C31 101.8(3) . . ? C33 C32 H32A 111.4 . . ? C31 C32 H32A 111.4 . . ? C33 C32 H32B 111.4 . . ? C31 C32 H32B 111.4 . . ? H32A C32 H32B 109.3 . . ? C32 C33 C34 101.9(3) . . ? C32 C33 H33A 111.4 . . ? C34 C33 H33A 111.4 . . ? C32 C33 H33B 111.4 . . ? C34 C33 H33B 111.4 . . ? H33A C33 H33B 109.3 . . ? O3 C34 C33 104.9(3) . . ? O3 C34 H34A 110.8 . . ? C33 C34 H34A 110.8 . . ? O3 C34 H34B 110.8 . . ? C33 C34 H34B 110.8 . . ? H34A C34 H34B 108.8 . . ? C36 C35 O1 110.3(6) . . ? C36 C35 C36A 19.7(10) . . ? O1 C35 C36A 103.5(5) . . ? C36 C35 H35A 109.6 . . ? O1 C35 H35A 109.6 . . ? C36A C35 H35A 96.0 . . ? C36 C35 H35B 109.6 . . ? O1 C35 H35B 109.6 . . ? C36A C35 H35B 128.6 . . ? H35A C35 H35B 108.1 . . ? C35 C36 C37 107.9(11) . . ? C35 C36 H36A 110.1 . . ? C37 C36 H36A 110.1 . . ? C35 C36 H36B 110.1 . . ? C37 C36 H36B 110.1 . . ? H36A C36 H36B 108.4 . . ? C36 C37 C38 106.4(9) . . ? C36 C37 H37A 110.4 . . ? C38 C37 H37A 110.4 . . ? C36 C37 H37B 110.4 . . ? C38 C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? O1 C38 C37A 107.3(5) . . ? O1 C38 C37 103.2(4) . . ? C37A C38 C37 32.1(5) . . ? O1 C38 H38A 111.1 . . ? C37A C38 H38A 80.4 . . ? C37 C38 H38A 111.1 . . ? O1 C38 H38B 111.1 . . ? C37A C38 H38B 132.9 . . ? C37 C38 H38B 111.1 . . ? H38A C38 H38B 109.1 . . ? O2 C39 C40 106.0(3) . . ? O2 C39 H39A 110.5 . . ? C40 C39 H39A 110.5 . . ? O2 C39 H39B 110.5 . . ? C40 C39 H39B 110.5 . . ? H39A C39 H39B 108.7 . . ? C41A C40 C41 38.3(6) . . ? C41A C40 C39 109.9(6) . . ? C41 C40 C39 104.9(3) . . ? C41A C40 H40A 109.7 . . ? C41 C40 H40A 140.5 . . ? C39 C40 H40A 109.7 . . ? C41A C40 H40B 109.7 . . ? C41 C40 H40B 76.6 . . ? C39 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C41A C40 H40C 73.9 . . ? C41 C40 H40C 110.8 . . ? C39 C40 H40C 110.8 . . ? H40A C40 H40C 38.3 . . ? H40B C40 H40C 134.9 . . ? C41A C40 H40D 134.6 . . ? C41 C40 H40D 110.8 . . ? C39 C40 H40D 110.8 . . ? H40A C40 H40D 74.1 . . ? H40B C40 H40D 36.3 . . ? H40C C40 H40D 108.9 . . ? C40 C41 C42 102.9(4) . . ? C40 C41 H41A 111.2 . . ? C42 C41 H41A 111.2 . . ? C40 C41 H41B 111.2 . . ? C42 C41 H41B 111.2 . . ? H41A C41 H41B 109.1 . . ? O2 C42 C41A 105.6(4) . . ? O2 C42 C41 102.6(3) . . ? C41A C42 C41 36.2(5) . . ? O2 C42 H42A 110.6 . . ? C41A C42 H42A 110.6 . . ? C41 C42 H42A 139.8 . . ? O2 C42 H42B 110.6 . . ? C41A C42 H42B 110.6 . . ? C41 C42 H42B 78.7 . . ? H42A C42 H42B 108.7 . . ? C37A C36A C35 107.1(10) . . ? C37A C36A H36C 110.3 . . ? C35 C36A H36C 110.3 . . ? C37A C36A H36D 110.3 . . ? C35 C36A H36D 110.3 . . ? H36C C36A H36D 108.6 . . ? C36A C37A C38 107.6(9) . . ? C36A C37A H37C 110.2 . . ? C38 C37A H37C 110.2 . . ? C36A C37A H37D 110.2 . . ? C38 C37A H37D 110.2 . . ? H37C C37A H37D 108.5 . . ? C40 C41A C42 103.4(7) . . ? C40 C41A H41C 111.1 . . ? C42 C41A H41C 111.1 . . ? C40 C41A H41D 111.1 . . ? C42 C41A H41D 111.1 . . ? H41C C41A H41D 109.0 . . ? 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 Si1 Mg1 N1 -177.27(15) . . . . ? C13 Si1 Mg1 N1 -88.87(17) . . . . ? N2 Si1 Mg1 O2 -86.00(13) . . . . ? N1 Si1 Mg1 O2 91.26(13) . . . . ? C13 Si1 Mg1 O2 2.39(16) . . . . ? N2 Si1 Mg1 O3 45.18(14) . . . . ? N1 Si1 Mg1 O3 -137.55(14) . . . . ? C13 Si1 Mg1 O3 133.58(16) . . . . ? N1 Si1 Mg1 N2 177.27(15) . . . . ? C13 Si1 Mg1 N2 88.40(17) . . . . ? N2 Si1 Mg1 O1 160.56(15) . . . . ? N1 Si1 Mg1 O1 -22.17(14) . . . . ? C13 Si1 Mg1 O1 -111.04(16) . . . . ? N1 Mg1 O1 C35 -159.7(3) . . . . ? O2 Mg1 O1 C35 88.9(3) . . . . ? O3 Mg1 O1 C35 -14.5(3) . . . . ? N2 Mg1 O1 C35 -96.3(4) . . . . ? Si1 Mg1 O1 C35 -146.0(3) . . . . ? N1 Mg1 O1 C38 40.5(2) . . . . ? O2 Mg1 O1 C38 -70.9(2) . . . . ? O3 Mg1 O1 C38 -174.3(2) . . . . ? N2 Mg1 O1 C38 104.0(4) . . . . ? Si1 Mg1 O1 C38 54.2(3) . . . . ? N1 Mg1 O2 C39 -158.9(3) . . . . ? O3 Mg1 O2 C39 18.4(3) . . . . ? N2 Mg1 O2 C39 118.0(3) . . . . ? O1 Mg1 O2 C39 -63.5(3) . . . . ? Si1 Mg1 O2 C39 159.0(2) . . . . ? N1 Mg1 O2 C42 12.5(3) . . . . ? O3 Mg1 O2 C42 -170.2(2) . . . . ? N2 Mg1 O2 C42 -70.6(3) . . . . ? O1 Mg1 O2 C42 107.9(3) . . . . ? Si1 Mg1 O2 C42 -29.6(3) . . . . ? N1 Mg1 O3 C31 -139.0(2) . . . . ? O2 Mg1 O3 C31 45.4(3) . . . . ? N2 Mg1 O3 C31 -64.8(2) . . . . ? O1 Mg1 O3 C31 130.9(2) . . . . ? Si1 Mg1 O3 C31 -91.1(2) . . . . ? N1 Mg1 O3 C34 4.7(3) . . . . ? O2 Mg1 O3 C34 -170.8(2) . . . . ? N2 Mg1 O3 C34 78.9(2) . . . . ? O1 Mg1 O3 C34 -85.4(2) . . . . ? Si1 Mg1 O3 C34 52.6(3) . . . . ? N2 Si1 N1 C1 156.2(2) . . . . ? C13 Si1 N1 C1 -80.0(3) . . . . ? Mg1 Si1 N1 C1 154.1(3) . . . . ? N2 Si1 N1 Mg1 2.15(12) . . . . ? C13 Si1 N1 Mg1 125.90(12) . . . . ? O2 Mg1 N1 C1 106.1(3) . . . . ? O3 Mg1 N1 C1 -69.3(4) . . . . ? N2 Mg1 N1 C1 -148.9(3) . . . . ? O1 Mg1 N1 C1 16.7(3) . . . . ? Si1 Mg1 N1 C1 -147.1(3) . . . . ? O2 Mg1 N1 Si1 -106.81(11) . . . . ? O3 Mg1 N1 Si1 77.8(2) . . . . ? N2 Mg1 N1 Si1 -1.75(10) . . . . ? O1 Mg1 N1 Si1 163.81(10) . . . . ? N1 Si1 N2 C19 -172.0(3) . . . . ? C13 Si1 N2 C19 63.1(3) . . . . ? Mg1 Si1 N2 C19 -169.9(3) . . . . ? N1 Si1 N2 Mg1 -2.08(12) . . . . ? C13 Si1 N2 Mg1 -126.94(12) . . . . ? N1 Mg1 N2 C19 171.6(3) . . . . ? O2 Mg1 N2 C19 -79.6(3) . . . . ? O3 Mg1 N2 C19 25.7(3) . . . . ? O1 Mg1 N2 C19 105.8(4) . . . . ? Si1 Mg1 N2 C19 169.8(3) . . . . ? N1 Mg1 N2 Si1 1.75(10) . . . . ? O2 Mg1 N2 Si1 110.53(11) . . . . ? O3 Mg1 N2 Si1 -144.16(11) . . . . ? O1 Mg1 N2 Si1 -64.1(4) . . . . ? Si1 N1 C1 C2 99.7(3) . . . . ? Mg1 N1 C1 C2 -120.2(3) . . . . ? Si1 N1 C1 C9 -82.0(3) . . . . ? Mg1 N1 C1 C9 58.1(4) . . . . ? N1 C1 C2 C6 178.6(3) . . . . ? C9 C1 C2 C6 0.3(4) . . . . ? N1 C1 C2 C3 -3.3(4) . . . . ? C9 C1 C2 C3 178.4(3) . . . . ? C6 C2 C3 C5 -61.7(4) . . . . ? C1 C2 C3 C5 120.1(3) . . . . ? C6 C2 C3 C4 64.0(4) . . . . ? C1 C2 C3 C4 -114.1(3) . . . . ? C1 C2 C6 C7 -0.3(5) . . . . ? C3 C2 C6 C7 -178.4(3) . . . . ? C2 C6 C7 C8 0.5(6) . . . . ? C6 C7 C8 C9 -0.7(6) . . . . ? C7 C8 C9 C1 0.7(6) . . . . ? C7 C8 C9 C10 179.1(4) . . . . ? N1 C1 C9 C8 -178.8(3) . . . . ? C2 C1 C9 C8 -0.5(5) . . . . ? N1 C1 C9 C10 2.8(5) . . . . ? C2 C1 C9 C10 -178.9(3) . . . . ? C8 C9 C10 C12 57.2(4) . . . . ? C1 C9 C10 C12 -124.4(3) . . . . ? C8 C9 C10 C11 -66.6(5) . . . . ? C1 C9 C10 C11 111.8(3) . . . . ? N2 Si1 C13 C14 57.1(3) . . . . ? N1 Si1 C13 C14 -58.3(3) . . . . ? Mg1 Si1 C13 C14 -1.4(4) . . . . ? N2 Si1 C13 C18 -122.3(2) . . . . ? N1 Si1 C13 C18 122.3(2) . . . . ? Mg1 Si1 C13 C18 179.17(19) . . . . ? C18 C13 C14 C15 -0.5(5) . . . . ? Si1 C13 C14 C15 -179.9(3) . . . . ? C13 C14 C15 C16 0.5(6) . . . . ? C14 C15 C16 C17 -0.6(6) . . . . ? C15 C16 C17 C18 0.7(6) . . . . ? C14 C13 C18 C17 0.5(5) . . . . ? Si1 C13 C18 C17 180.0(3) . . . . ? C16 C17 C18 C13 -0.6(6) . . . . ? Si1 N2 C19 C20 -124.6(3) . . . . ? Mg1 N2 C19 C20 69.6(4) . . . . ? Si1 N2 C19 C27 59.7(4) . . . . ? Mg1 N2 C19 C27 -106.1(3) . . . . ? N2 C19 C20 C24 -174.3(3) . . . . ? C27 C19 C20 C24 1.6(5) . . . . ? N2 C19 C20 C21 8.1(5) . . . . ? C27 C19 C20 C21 -175.9(3) . . . . ? C24 C20 C21 C22 -81.1(4) . . . . ? C19 C20 C21 C22 96.5(4) . . . . ? C24 C20 C21 C23 41.3(5) . . . . ? C19 C20 C21 C23 -141.1(3) . . . . ? C19 C20 C24 C25 -1.5(6) . . . . ? C21 C20 C24 C25 176.1(4) . . . . ? C20 C24 C25 C26 -0.1(6) . . . . ? C24 C25 C26 C27 1.5(6) . . . . ? C25 C26 C27 C19 -1.3(6) . . . . ? C25 C26 C27 C28 179.7(4) . . . . ? N2 C19 C27 C26 175.6(3) . . . . ? C20 C19 C27 C26 -0.3(5) . . . . ? N2 C19 C27 C28 -5.4(5) . . . . ? C20 C19 C27 C28 178.7(3) . . . . ? C26 C27 C28 C30 -44.8(4) . . . . ? C19 C27 C28 C30 136.2(3) . . . . ? C26 C27 C28 C29 77.2(4) . . . . ? C19 C27 C28 C29 -101.8(4) . . . . ? C34 O3 C31 C32 -11.5(4) . . . . ? Mg1 O3 C31 C32 135.1(2) . . . . ? O3 C31 C32 C33 32.8(4) . . . . ? C31 C32 C33 C34 -40.5(4) . . . . ? C31 O3 C34 C33 -14.3(4) . . . . ? Mg1 O3 C34 C33 -163.2(2) . . . . ? C32 C33 C34 O3 34.4(4) . . . . ? C38 O1 C35 C36 3.4(8) . . . . ? Mg1 O1 C35 C36 -157.9(7) . . . . ? C38 O1 C35 C36A 22.7(7) . . . . ? Mg1 O1 C35 C36A -138.6(6) . . . . ? O1 C35 C36 C37 -14.5(13) . . . . ? C36A C35 C36 C37 -87(3) . . . . ? C35 C36 C37 C38 18.9(14) . . . . ? C35 O1 C38 C37A -25.2(6) . . . . ? Mg1 O1 C38 C37A 138.6(5) . . . . ? C35 O1 C38 C37 7.8(5) . . . . ? Mg1 O1 C38 C37 171.6(4) . . . . ? C36 C37 C38 O1 -16.3(11) . . . . ? C36 C37 C38 C37A 85.2(14) . . . . ? C42 O2 C39 C40 1.2(4) . . . . ? Mg1 O2 C39 C40 173.5(3) . . . . ? O2 C39 C40 C41A 15.3(9) . . . . ? O2 C39 C40 C41 -24.6(5) . . . . ? C41A C40 C41 C42 -65.8(9) . . . . ? C39 C40 C41 C42 37.6(5) . . . . ? C39 O2 C42 C41A -15.7(7) . . . . ? Mg1 O2 C42 C41A 171.4(6) . . . . ? C39 O2 C42 C41 21.5(4) . . . . ? Mg1 O2 C42 C41 -151.4(3) . . . . ? C40 C41 C42 O2 -36.1(5) . . . . ? C40 C41 C42 C41A 63.2(5) . . . . ? C36 C35 C36A C37A 100(3) . . . . ? O1 C35 C36A C37A -12.5(11) . . . . ? C35 C36A C37A C38 -2.2(13) . . . . ? O1 C38 C37A C36A 16.3(11) . . . . ? C37 C38 C37A C36A -71.1(13) . . . . ? C41 C40 C41A C42 64.7(9) . . . . ? C39 C40 C41A C42 -24.3(11) . . . . ? O2 C42 C41A C40 24.3(11) . . . . ? C41 C42 C41A C40 -65.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.302 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.070 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.500 486 68 ' ' 2 0.000 0.500 1.000 486 68 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 945787' ####################################################################### # # 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_h10msh02 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H72 Ca N2 O3 Si' _chemical_formula_weight 805.26 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.2642(2) _cell_length_b 22.7621(6) _cell_length_c 20.7835(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.249(2) _cell_angle_gamma 90.00 _cell_volume 4805.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 58116 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description tabloid _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.195 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _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 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64099 _diffrn_reflns_av_R_equivalents 0.1702 _diffrn_reflns_av_sigmaI/netI 0.0747 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.04 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8386 _reflns_number_gt 5005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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. Crystal structure unambiguous, but data quality not great. Borderline for publication. Asymmetric unit contains 1 molecule solvent (toluene) in addition to 1 molecule of the complex. H1 located and freely refined. Some THF carbons disordered in 55:45 ratio [C36,37, 39, 40, 41, and 42]. ADP restraints applied to fractional occupancy atoms and distance restraints applied in disordered regions to assist convergence. ; _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^)+(0.1038P)^2^+4.6263P] 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 8386 _refine_ls_number_parameters 572 _refine_ls_number_restraints 106 _refine_ls_R_factor_all 0.1379 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2270 _refine_ls_wR_factor_gt 0.1990 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.089 _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 Ca1 Ca 0.97780(8) 0.23679(4) 0.46772(4) 0.0355(2) Uani 1 1 d . B . Si1 Si 0.71624(10) 0.23135(5) 0.38584(5) 0.0317(3) Uani 1 1 d . B . O1 O 1.1411(3) 0.17404(15) 0.44020(17) 0.0546(9) Uani 1 1 d . . . O2 O 1.0568(3) 0.20800(15) 0.57623(15) 0.0566(9) Uani 1 1 d . B . O3 O 1.0818(4) 0.32841(16) 0.4986(2) 0.0726(12) Uani 1 1 d D . . N1 N 0.7800(3) 0.18951(15) 0.45044(16) 0.0345(8) Uani 1 1 d . . . N2 N 0.8423(3) 0.27775(14) 0.37877(17) 0.0379(8) Uani 1 1 d . . . C1 C 0.7042(4) 0.16224(17) 0.49246(18) 0.0325(9) Uani 1 1 d . C . C2 C 0.6870(4) 0.10002(18) 0.4915(2) 0.0365(9) Uani 1 1 d . . . C3 C 0.7420(4) 0.06322(19) 0.4411(2) 0.0439(11) Uani 1 1 d . C . H3 H 0.7966 0.0897 0.4174 0.053 Uiso 1 1 calc R . . C4 C 0.8305(8) 0.0156(4) 0.4719(4) 0.107(3) Uani 1 1 d . . . H4A H 0.8949 0.0325 0.5063 0.161 Uiso 1 1 calc R C . H4B H 0.8768 -0.0026 0.4389 0.161 Uiso 1 1 calc R . . H4C H 0.7779 -0.0141 0.4905 0.161 Uiso 1 1 calc R . . C5 C 0.6342(6) 0.0384(3) 0.3917(3) 0.0664(15) Uani 1 1 d . . . H5A H 0.6733 0.0153 0.3596 0.100 Uiso 1 1 calc R C . H5B H 0.5824 0.0707 0.3697 0.100 Uiso 1 1 calc R . . H5C H 0.5769 0.0133 0.4136 0.100 Uiso 1 1 calc R . . C6 C 0.6180(5) 0.0741(2) 0.5363(2) 0.0495(12) Uani 1 1 d . C . H6 H 0.6104 0.0325 0.5367 0.059 Uiso 1 1 calc R . . C7 C 0.5588(5) 0.1068(2) 0.5811(2) 0.0512(12) Uani 1 1 d . . . H7 H 0.5084 0.0882 0.6102 0.061 Uiso 1 1 calc R C . C8 C 0.5758(5) 0.1667(2) 0.5817(2) 0.0480(11) Uani 1 1 d . C . H8 H 0.5371 0.1894 0.6123 0.058 Uiso 1 1 calc R . . C9 C 0.6471(4) 0.19517(19) 0.5396(2) 0.0398(10) Uani 1 1 d . . . C10 C 0.6649(4) 0.2615(2) 0.5448(2) 0.0445(10) Uani 1 1 d . C . H10 H 0.7097 0.2741 0.5074 0.053 Uiso 1 1 calc R . . C11 C 0.5348(5) 0.2938(2) 0.5386(3) 0.0662(15) Uani 1 1 d . . . H11A H 0.4811 0.2832 0.4974 0.099 Uiso 1 1 calc R C . H11B H 0.5509 0.3362 0.5397 0.099 Uiso 1 1 calc R . . H11C H 0.4882 0.2828 0.5748 0.099 Uiso 1 1 calc R . . C12 C 0.7536(5) 0.2794(2) 0.6067(3) 0.0586(13) Uani 1 1 d . . . H12A H 0.7097 0.2706 0.6444 0.088 Uiso 1 1 calc R C . H12B H 0.7719 0.3216 0.6054 0.088 Uiso 1 1 calc R . . H12C H 0.8365 0.2575 0.6101 0.088 Uiso 1 1 calc R . . C13 C 0.8584(4) 0.32733(17) 0.3420(2) 0.0358(9) Uani 1 1 d . C . C14 C 0.9631(4) 0.3299(2) 0.3037(2) 0.0437(10) Uani 1 1 d . . . C15 C 1.0513(5) 0.2767(2) 0.2993(3) 0.0587(13) Uani 1 1 d . C . H15 H 1.0569 0.2538 0.3407 0.070 Uiso 1 1 calc R . . C16 C 1.1905(7) 0.2929(4) 0.2874(5) 0.127(3) Uani 1 1 d . . . H16A H 1.1867 0.3111 0.2445 0.190 Uiso 1 1 calc R C . H16B H 1.2447 0.2574 0.2893 0.190 Uiso 1 1 calc R . . H16C H 1.2292 0.3206 0.3209 0.190 Uiso 1 1 calc R . . C17 C 0.9937(8) 0.2377(3) 0.2431(3) 0.088(2) Uani 1 1 d . . . H17A H 0.9072 0.2233 0.2506 0.132 Uiso 1 1 calc R C . H17B H 1.0525 0.2043 0.2397 0.132 Uiso 1 1 calc R . . H17C H 0.9842 0.2603 0.2025 0.132 Uiso 1 1 calc R . . C18 C 0.9827(5) 0.3798(2) 0.2683(2) 0.0559(13) Uani 1 1 d . C . H18 H 1.0524 0.3803 0.2428 0.067 Uiso 1 1 calc R . . C19 C 0.9040(6) 0.4286(2) 0.2690(3) 0.0622(15) Uani 1 1 d . . . H19 H 0.9184 0.4622 0.2438 0.075 Uiso 1 1 calc R C . C20 C 0.8042(5) 0.4280(2) 0.3067(3) 0.0543(13) Uani 1 1 d . C . H20 H 0.7499 0.4618 0.3073 0.065 Uiso 1 1 calc R . . C21 C 0.7806(4) 0.37936(18) 0.3440(2) 0.0407(10) Uani 1 1 d . . . C22 C 0.6711(5) 0.3822(2) 0.3860(2) 0.0500(12) Uani 1 1 d . C . H22 H 0.6842 0.3490 0.4179 0.060 Uiso 1 1 calc R . . C23 C 0.5358(5) 0.3746(3) 0.3451(3) 0.0687(16) Uani 1 1 d . . . H23A H 0.5211 0.4064 0.3131 0.103 Uiso 1 1 calc R C . H23B H 0.4674 0.3759 0.3735 0.103 Uiso 1 1 calc R . . H23C H 0.5322 0.3367 0.3226 0.103 Uiso 1 1 calc R . . C24 C 0.6704(7) 0.4398(3) 0.4246(3) 0.0814(19) Uani 1 1 d . . . H24A H 0.7541 0.4439 0.4536 0.122 Uiso 1 1 calc R C . H24B H 0.5977 0.4392 0.4504 0.122 Uiso 1 1 calc R . . H24C H 0.6591 0.4731 0.3944 0.122 Uiso 1 1 calc R . . C25 C 0.6558(4) 0.18465(18) 0.3110(2) 0.0380(10) Uani 1 1 d . . . C26 C 0.7313(5) 0.1443(2) 0.2839(2) 0.0566(13) Uani 1 1 d . C . H26 H 0.8227 0.1421 0.2997 0.068 Uiso 1 1 calc R . . C27 C 0.6787(6) 0.1062(3) 0.2338(3) 0.0675(15) Uani 1 1 d . . . H27 H 0.7344 0.0791 0.2160 0.081 Uiso 1 1 calc R C . C28 C 0.5484(6) 0.1080(3) 0.2107(3) 0.0654(15) Uani 1 1 d . C . H28 H 0.5122 0.0819 0.1772 0.078 Uiso 1 1 calc R . . C29 C 0.4688(6) 0.1477(3) 0.2361(2) 0.0614(14) Uani 1 1 d . . . H29 H 0.3776 0.1497 0.2198 0.074 Uiso 1 1 calc R C . C30 C 0.5230(4) 0.1853(2) 0.2860(2) 0.0458(11) Uani 1 1 d . C . H30 H 0.4669 0.2123 0.3035 0.055 Uiso 1 1 calc R . . C31 C 1.1241(5) 0.1284(2) 0.3920(3) 0.0534(12) Uani 1 1 d . . . H31A H 1.0656 0.1418 0.3526 0.064 Uiso 1 1 calc R . . H31B H 1.0855 0.0929 0.4092 0.064 Uiso 1 1 calc R . . C32 C 1.2606(6) 0.1158(3) 0.3764(4) 0.092(2) Uani 1 1 d . . . H32A H 1.2765 0.0729 0.3757 0.111 Uiso 1 1 calc R . . H32B H 1.2719 0.1324 0.3336 0.111 Uiso 1 1 calc R . . C33 C 1.3500(6) 0.1434(4) 0.4276(4) 0.099(2) Uani 1 1 d . . . H33A H 1.4042 0.1131 0.4531 0.119 Uiso 1 1 calc R . . H33B H 1.4096 0.1704 0.4086 0.119 Uiso 1 1 calc R . . C34 C 1.2765(5) 0.1749(4) 0.4685(4) 0.103(3) Uani 1 1 d . . . H34A H 1.3084 0.2160 0.4733 0.124 Uiso 1 1 calc R . . H34B H 1.2869 0.1566 0.5122 0.124 Uiso 1 1 calc R . . C35 C 1.0270(8) 0.1484(3) 0.5944(3) 0.088(2) Uani 1 1 d . . . H35A H 0.9374 0.1466 0.6067 0.105 Uiso 1 1 calc R A 1 H35B H 1.0306 0.1215 0.5573 0.105 Uiso 1 1 calc R A 1 C36 C 1.1232(13) 0.1310(5) 0.6488(6) 0.076(3) Uani 0.55 1 d PDU B 1 H36A H 1.2066 0.1179 0.6346 0.092 Uiso 0.55 1 calc PR B 1 H36B H 1.0892 0.0996 0.6749 0.092 Uiso 0.55 1 calc PR B 1 C37 C 1.1405(16) 0.1910(6) 0.6872(6) 0.074(3) Uani 0.55 1 d PDU B 1 H37A H 1.0656 0.1989 0.7111 0.089 Uiso 0.55 1 calc PR B 1 H37B H 1.2238 0.1922 0.7178 0.089 Uiso 0.55 1 calc PR B 1 C38 C 1.1428(6) 0.2340(3) 0.6297(3) 0.0710(16) Uani 1 1 d . . . H38A H 1.1101 0.2733 0.6404 0.085 Uiso 1 1 calc R B 1 H38B H 1.2332 0.2382 0.6190 0.085 Uiso 1 1 calc R B 1 C39 C 1.0021(10) 0.3806(4) 0.4960(6) 0.057(3) Uani 0.55 1 d PDU C 1 H39A H 0.9897 0.3937 0.5402 0.068 Uiso 0.55 1 calc PR C 1 H39B H 0.9148 0.3741 0.4699 0.068 Uiso 0.55 1 calc PR C 1 C40 C 1.0835(11) 0.4256(5) 0.4632(7) 0.076(3) Uani 0.55 1 d PDU C 1 H40A H 1.0640 0.4664 0.4753 0.091 Uiso 0.55 1 calc PR C 1 H40B H 1.0689 0.4216 0.4153 0.091 Uiso 0.55 1 calc PR C 1 C41 C 1.2253(12) 0.4067(6) 0.4929(8) 0.095(4) Uani 0.55 1 d PDU C 1 H41A H 1.2821 0.4024 0.4585 0.114 Uiso 0.55 1 calc PR C 1 H41B H 1.2654 0.4360 0.5250 0.114 Uiso 0.55 1 calc PR C 1 C42 C 1.2078(14) 0.3468(7) 0.5264(9) 0.135(6) Uani 0.55 1 d PDU C 1 H42A H 1.2758 0.3184 0.5172 0.162 Uiso 0.55 1 calc PR C 1 H42B H 1.2130 0.3516 0.5740 0.162 Uiso 0.55 1 calc PR C 1 C51 C 0.1443(9) 0.0262(3) 0.1941(5) 0.106(3) Uani 1 1 d . . . C52 C 0.2296(7) -0.0109(3) 0.2279(5) 0.093(2) Uani 1 1 d . . . H52 H 0.3061 -0.0221 0.2101 0.112 Uiso 1 1 calc R . . C53 C 0.2107(9) -0.0334(3) 0.2877(5) 0.101(3) Uani 1 1 d . . . H53 H 0.2721 -0.0603 0.3100 0.121 Uiso 1 1 calc R . . C54 C 0.1029(10) -0.0165(4) 0.3138(4) 0.108(3) Uani 1 1 d . . . H54 H 0.0889 -0.0317 0.3549 0.129 Uiso 1 1 calc R . . C55 C 0.0123(9) 0.0229(4) 0.2811(5) 0.108(3) Uani 1 1 d . . . H55 H -0.0634 0.0347 0.2992 0.130 Uiso 1 1 calc R . . C56 C 0.0355(7) 0.0441(3) 0.2223(5) 0.092(2) Uani 1 1 d . . . H56 H -0.0239 0.0718 0.2000 0.111 Uiso 1 1 calc R . . C57 C 0.1633(12) 0.0472(5) 0.1311(5) 0.161(5) Uani 1 1 d . . . H57A H 0.2562 0.0573 0.1314 0.241 Uiso 1 1 calc R . . H57B H 0.1088 0.0821 0.1202 0.241 Uiso 1 1 calc R . . H57C H 0.1381 0.0165 0.0986 0.241 Uiso 1 1 calc R . . C36A C 1.0623(19) 0.1576(11) 0.6736(10) 0.115(6) Uani 0.45 1 d PDU B 2 H36C H 1.0002 0.1843 0.6914 0.138 Uiso 0.45 1 calc PR B 2 H36D H 1.0699 0.1201 0.6979 0.138 Uiso 0.45 1 calc PR B 2 C37A C 1.2000(19) 0.1870(9) 0.6694(10) 0.097(6) Uani 0.45 1 d PDU B 2 H37C H 1.2457 0.2003 0.7122 0.116 Uiso 0.45 1 calc PR B 2 H37D H 1.2589 0.1620 0.6473 0.116 Uiso 0.45 1 calc PR B 2 C39A C 1.014(2) 0.3681(8) 0.5305(11) 0.111(7) Uani 0.45 1 d PDU C 2 H39C H 1.0148 0.3574 0.5767 0.134 Uiso 0.45 1 calc PR C 2 H39D H 0.9215 0.3724 0.5092 0.134 Uiso 0.45 1 calc PR C 2 C40A C 1.094(2) 0.4237(8) 0.5230(12) 0.124(6) Uani 0.45 1 d PDU C 2 H40C H 1.1570 0.4299 0.5633 0.149 Uiso 0.45 1 calc PR C 2 H40D H 1.0345 0.4580 0.5172 0.149 Uiso 0.45 1 calc PR C 2 C41A C 1.172(4) 0.4198(8) 0.4640(14) 0.161(12) Uani 0.45 1 d PDU C 2 H41C H 1.1226 0.4365 0.4238 0.193 Uiso 0.45 1 calc PR C 2 H41D H 1.2601 0.4386 0.4731 0.193 Uiso 0.45 1 calc PR C 2 C42A C 1.1810(14) 0.3531(6) 0.4618(7) 0.076(4) Uani 0.45 1 d PDU C 2 H42C H 1.1645 0.3394 0.4162 0.091 Uiso 0.45 1 calc PR C 2 H42D H 1.2700 0.3401 0.4811 0.091 Uiso 0.45 1 calc PR C 2 H1 H 0.602(3) 0.2552(15) 0.3936(17) 0.021(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0282(4) 0.0339(5) 0.0428(5) 0.0033(4) -0.0008(3) -0.0019(3) Si1 0.0283(6) 0.0288(6) 0.0371(6) 0.0032(5) 0.0016(4) -0.0001(4) O1 0.0304(16) 0.058(2) 0.071(2) -0.0174(17) -0.0069(15) 0.0087(14) O2 0.060(2) 0.060(2) 0.0444(18) 0.0028(16) -0.0126(15) -0.0016(17) O3 0.061(2) 0.045(2) 0.102(3) -0.002(2) -0.021(2) -0.0151(17) N1 0.0311(17) 0.0344(18) 0.0367(18) 0.0038(15) 0.0004(15) -0.0032(14) N2 0.0333(18) 0.0326(19) 0.046(2) 0.0081(16) 0.0006(15) 0.0002(14) C1 0.029(2) 0.036(2) 0.031(2) 0.0039(17) -0.0012(16) -0.0004(16) C2 0.031(2) 0.032(2) 0.047(2) 0.0027(18) 0.0048(18) -0.0031(17) C3 0.044(2) 0.032(2) 0.059(3) 0.000(2) 0.018(2) -0.0041(19) C4 0.124(6) 0.108(6) 0.086(5) -0.010(4) 0.003(4) 0.081(5) C5 0.066(3) 0.077(4) 0.058(3) -0.021(3) 0.015(3) -0.012(3) C6 0.054(3) 0.033(2) 0.063(3) 0.005(2) 0.011(2) -0.012(2) C7 0.062(3) 0.050(3) 0.045(3) 0.000(2) 0.021(2) -0.014(2) C8 0.053(3) 0.051(3) 0.042(2) -0.004(2) 0.014(2) -0.005(2) C9 0.042(2) 0.037(2) 0.039(2) -0.0027(19) -0.0005(19) -0.0057(18) C10 0.050(3) 0.041(2) 0.045(2) -0.010(2) 0.011(2) -0.008(2) C11 0.061(3) 0.047(3) 0.088(4) -0.011(3) 0.002(3) 0.002(2) C12 0.059(3) 0.053(3) 0.064(3) -0.017(3) 0.008(3) -0.012(2) C13 0.036(2) 0.030(2) 0.039(2) 0.0062(18) -0.0027(18) -0.0080(17) C14 0.045(3) 0.045(3) 0.041(2) 0.012(2) 0.003(2) -0.003(2) C15 0.050(3) 0.059(3) 0.071(3) 0.014(3) 0.023(3) 0.005(2) C16 0.059(4) 0.130(7) 0.195(10) 0.025(7) 0.028(5) 0.017(4) C17 0.121(6) 0.068(4) 0.083(4) 0.007(4) 0.039(4) 0.010(4) C18 0.051(3) 0.062(3) 0.055(3) 0.011(3) 0.009(2) -0.010(2) C19 0.071(4) 0.048(3) 0.065(3) 0.024(3) 0.001(3) -0.012(3) C20 0.065(3) 0.032(2) 0.063(3) 0.015(2) -0.004(3) -0.002(2) C21 0.044(2) 0.032(2) 0.043(2) 0.0037(19) -0.004(2) -0.0034(18) C22 0.058(3) 0.036(2) 0.056(3) 0.002(2) 0.007(2) 0.007(2) C23 0.050(3) 0.062(3) 0.091(4) 0.018(3) 0.002(3) 0.014(3) C24 0.111(5) 0.051(3) 0.088(4) -0.018(3) 0.033(4) 0.002(3) C25 0.038(2) 0.038(2) 0.037(2) 0.0080(19) 0.0031(18) -0.0029(18) C26 0.044(3) 0.070(3) 0.053(3) -0.009(3) -0.002(2) 0.007(2) C27 0.074(4) 0.067(4) 0.061(3) -0.017(3) 0.007(3) 0.008(3) C28 0.079(4) 0.066(4) 0.045(3) -0.011(3) -0.010(3) -0.001(3) C29 0.060(3) 0.071(4) 0.048(3) 0.006(3) -0.011(2) -0.014(3) C30 0.044(3) 0.047(3) 0.044(3) 0.003(2) 0.000(2) -0.002(2) C31 0.046(3) 0.051(3) 0.062(3) -0.015(2) 0.002(2) -0.001(2) C32 0.053(3) 0.098(5) 0.130(6) -0.052(5) 0.029(4) -0.011(3) C33 0.041(3) 0.159(7) 0.096(5) -0.031(5) 0.007(3) 0.007(4) C34 0.042(3) 0.117(6) 0.140(6) -0.071(5) -0.024(4) 0.015(3) C35 0.116(5) 0.071(4) 0.065(4) 0.019(3) -0.023(4) -0.025(4) C36 0.083(6) 0.072(6) 0.069(6) 0.011(5) -0.006(5) 0.018(5) C37 0.070(6) 0.087(7) 0.062(6) -0.004(5) -0.004(5) 0.003(6) C38 0.064(3) 0.075(4) 0.066(4) -0.011(3) -0.018(3) -0.002(3) C39 0.060(5) 0.047(5) 0.060(5) -0.010(4) -0.002(4) 0.002(4) C40 0.074(6) 0.060(5) 0.093(6) 0.001(5) 0.009(5) -0.017(5) C41 0.084(7) 0.074(6) 0.126(8) 0.001(6) 0.011(6) -0.023(5) C42 0.127(8) 0.123(8) 0.149(9) -0.002(7) -0.001(7) 0.000(7) C51 0.103(6) 0.067(4) 0.138(7) -0.004(5) -0.014(5) -0.030(4) C52 0.080(5) 0.062(4) 0.125(7) -0.011(4) -0.027(4) 0.009(3) C53 0.100(6) 0.074(5) 0.119(7) -0.013(5) -0.021(5) 0.021(4) C54 0.133(7) 0.078(5) 0.103(6) -0.021(4) -0.012(6) -0.007(5) C55 0.094(6) 0.086(6) 0.137(8) -0.046(6) -0.010(6) 0.000(4) C56 0.066(4) 0.068(4) 0.136(7) -0.026(5) -0.008(4) 0.007(3) C57 0.215(12) 0.131(8) 0.131(8) 0.044(7) 0.003(8) -0.090(8) C36A 0.125(9) 0.114(9) 0.104(8) 0.019(7) 0.006(7) -0.002(7) C37A 0.095(9) 0.102(9) 0.087(8) 0.003(7) -0.007(7) -0.005(7) C39A 0.125(10) 0.104(9) 0.108(9) -0.011(7) 0.028(7) -0.005(7) C40A 0.141(9) 0.102(9) 0.134(9) -0.008(7) 0.032(7) -0.004(7) C41A 0.165(13) 0.157(13) 0.159(13) 0.016(8) 0.020(8) -0.008(8) C42A 0.085(7) 0.061(6) 0.086(7) -0.016(5) 0.032(6) -0.025(5) _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 Ca1 N1 2.281(3) . ? Ca1 O1 2.335(3) . ? Ca1 N2 2.342(3) . ? Ca1 O2 2.377(3) . ? Ca1 O3 2.388(3) . ? Ca1 Si1 2.9678(13) . ? Si1 N2 1.693(3) . ? Si1 N1 1.699(3) . ? Si1 C25 1.912(4) . ? Si1 H1 1.32(3) . ? O1 C34 1.429(6) . ? O1 C31 1.436(6) . ? O2 C38 1.444(6) . ? O2 C35 1.452(7) . ? O3 C39A 1.370(14) . ? O3 C42 1.403(13) . ? O3 C39 1.440(9) . ? O3 C42A 1.470(11) . ? N1 C1 1.396(5) . ? N2 C13 1.386(5) . ? C1 C9 1.424(6) . ? C1 C2 1.427(6) . ? C2 C6 1.381(6) . ? C2 C3 1.513(6) . ? C3 C4 1.497(7) . ? C3 C5 1.507(7) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.396(7) . ? C6 H6 0.9500 . ? C7 C8 1.376(7) . ? C7 H7 0.9500 . ? C8 C9 1.380(6) . ? C8 H8 0.9500 . ? C9 C10 1.523(6) . ? C10 C11 1.513(7) . ? C10 C12 1.521(7) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.427(6) . ? C13 C21 1.432(6) . ? C14 C18 1.384(7) . ? C14 C15 1.521(7) . ? C15 C17 1.520(9) . ? C15 C16 1.530(9) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.374(8) . ? C18 H18 0.9500 . ? C19 C20 1.377(8) . ? C19 H19 0.9500 . ? C20 C21 1.393(6) . ? C20 H20 0.9500 . ? C21 C22 1.520(7) . ? C22 C23 1.530(7) . ? C22 C24 1.538(7) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.374(7) . ? C25 C30 1.388(6) . ? C26 C27 1.402(7) . ? C26 H26 0.9500 . ? C27 C28 1.356(8) . ? C27 H27 0.9500 . ? C28 C29 1.374(8) . ? C28 H28 0.9500 . ? C29 C30 1.396(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.510(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.446(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.411(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.446(12) . ? C35 C36A 1.65(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.580(12) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.547(15) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C37A 1.43(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.541(12) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.559(13) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.552(14) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C51 C52 1.340(10) . ? C51 C56 1.395(11) . ? C51 C57 1.432(12) . ? C52 C53 1.383(11) . ? C52 H52 0.9500 . ? C53 C54 1.356(12) . ? C53 H53 0.9500 . ? C54 C55 1.397(12) . ? C54 H54 0.9500 . ? C55 C56 1.367(12) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C36A C37A 1.578(14) . ? C36A H36C 0.9900 . ? C36A H36D 0.9900 . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? C39A C40A 1.532(15) . ? C39A H39C 0.9900 . ? C39A H39D 0.9900 . ? C40A C41A 1.560(15) . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? C41A C42A 1.522(15) . ? C41A H41C 0.9900 . ? C41A H41D 0.9900 . ? C42A H42C 0.9900 . ? C42A H42D 0.9900 . ? 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 Ca1 O1 109.10(12) . . ? N1 Ca1 N2 69.46(12) . . ? O1 Ca1 N2 114.58(13) . . ? N1 Ca1 O2 101.20(12) . . ? O1 Ca1 O2 84.53(13) . . ? N2 Ca1 O2 160.41(13) . . ? N1 Ca1 O3 143.90(14) . . ? O1 Ca1 O3 106.91(13) . . ? N2 Ca1 O3 93.23(13) . . ? O2 Ca1 O3 84.68(13) . . ? N1 Ca1 Si1 34.74(8) . . ? O1 Ca1 Si1 117.14(8) . . ? N2 Ca1 Si1 34.72(8) . . ? O2 Ca1 Si1 133.63(9) . . ? O3 Ca1 Si1 121.55(10) . . ? N2 Si1 N1 101.88(16) . . ? N2 Si1 C25 116.02(18) . . ? N1 Si1 C25 111.98(18) . . ? N2 Si1 Ca1 51.97(12) . . ? N1 Si1 Ca1 49.92(11) . . ? C25 Si1 Ca1 130.58(14) . . ? N2 Si1 H1 117.2(15) . . ? N1 Si1 H1 112.4(15) . . ? C25 Si1 H1 97.9(15) . . ? Ca1 Si1 H1 131.1(15) . . ? C34 O1 C31 108.1(4) . . ? C34 O1 Ca1 125.5(3) . . ? C31 O1 Ca1 126.4(3) . . ? C38 O2 C35 108.1(4) . . ? C38 O2 Ca1 134.8(3) . . ? C35 O2 Ca1 116.6(3) . . ? C39A O3 C42 96.2(13) . . ? C39A O3 C39 31.4(9) . . ? C42 O3 C39 104.7(9) . . ? C39A O3 C42A 116.0(10) . . ? C42 O3 C42A 55.5(9) . . ? C39 O3 C42A 95.6(8) . . ? C39A O3 Ca1 117.8(8) . . ? C42 O3 Ca1 136.2(7) . . ? C39 O3 Ca1 118.8(4) . . ? C42A O3 Ca1 120.7(6) . . ? C1 N1 Si1 123.9(3) . . ? C1 N1 Ca1 132.4(2) . . ? Si1 N1 Ca1 95.34(15) . . ? C13 N2 Si1 135.1(3) . . ? C13 N2 Ca1 130.9(3) . . ? Si1 N2 Ca1 93.31(15) . . ? N1 C1 C9 121.1(4) . . ? N1 C1 C2 120.8(4) . . ? C9 C1 C2 118.0(4) . . ? C6 C2 C1 119.3(4) . . ? C6 C2 C3 120.6(4) . . ? C1 C2 C3 120.1(4) . . ? C4 C3 C5 111.2(5) . . ? C4 C3 C2 111.6(4) . . ? C5 C3 C2 111.7(4) . . ? C4 C3 H3 107.4 . . ? C5 C3 H3 107.4 . . ? C2 C3 H3 107.4 . . ? 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 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 C7 122.5(4) . . ? C2 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C8 C7 C6 117.8(4) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C7 C8 C9 122.5(4) . . ? C7 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C8 C9 C1 119.8(4) . . ? C8 C9 C10 119.3(4) . . ? C1 C9 C10 120.9(4) . . ? C11 C10 C12 110.9(4) . . ? C11 C10 C9 112.4(4) . . ? C12 C10 C9 112.1(4) . . ? C11 C10 H10 107.0 . . ? C12 C10 H10 107.0 . . ? C9 C10 H10 107.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 119.9(4) . . ? N2 C13 C21 123.1(4) . . ? C14 C13 C21 116.8(4) . . ? C18 C14 C13 120.5(4) . . ? C18 C14 C15 119.2(4) . . ? C13 C14 C15 120.2(4) . . ? C17 C15 C14 110.0(5) . . ? C17 C15 C16 106.6(6) . . ? C14 C15 C16 113.3(5) . . ? C17 C15 H15 108.9 . . ? C14 C15 H15 108.9 . . ? C16 C15 H15 108.9 . . ? 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 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C14 121.8(5) . . ? C19 C18 H18 119.1 . . ? C14 C18 H18 119.1 . . ? C18 C19 C20 119.0(5) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C19 C20 C21 121.8(5) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C13 119.9(4) . . ? C20 C21 C22 119.2(4) . . ? C13 C21 C22 120.8(4) . . ? C21 C22 C23 111.3(4) . . ? C21 C22 C24 113.2(4) . . ? C23 C22 C24 108.3(5) . . ? C21 C22 H22 108.0 . . ? C23 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 115.8(4) . . ? C26 C25 Si1 124.7(3) . . ? C30 C25 Si1 119.0(3) . . ? C25 C26 C27 122.6(5) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C28 C27 C26 119.9(5) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 119.7(5) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C28 C29 C30 119.5(5) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C25 C30 C29 122.5(5) . . ? C25 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? O1 C31 C32 105.3(4) . . ? O1 C31 H31A 110.7 . . ? C32 C31 H31A 110.7 . . ? O1 C31 H31B 110.7 . . ? C32 C31 H31B 110.7 . . ? H31A C31 H31B 108.8 . . ? C33 C32 C31 105.6(5) . . ? C33 C32 H32A 110.6 . . ? C31 C32 H32A 110.6 . . ? C33 C32 H32B 110.6 . . ? C31 C32 H32B 110.6 . . ? H32A C32 H32B 108.7 . . ? C34 C33 C32 109.1(5) . . ? C34 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? C34 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? C33 C34 O1 108.5(5) . . ? C33 C34 H34A 110.0 . . ? O1 C34 H34A 110.0 . . ? C33 C34 H34B 110.0 . . ? O1 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? C36 C35 O2 108.3(6) . . ? C36 C35 C36A 39.3(8) . . ? O2 C35 C36A 96.7(9) . . ? C36 C35 H35A 110.0 . . ? O2 C35 H35A 110.0 . . ? C36A C35 H35A 80.0 . . ? C36 C35 H35B 110.0 . . ? O2 C35 H35B 110.0 . . ? C36A C35 H35B 146.1 . . ? H35A C35 H35B 108.4 . . ? C35 C36 C37 99.9(8) . . ? C35 C36 H36A 111.8 . . ? C37 C36 H36A 111.8 . . ? C35 C36 H36B 111.8 . . ? C37 C36 H36B 111.8 . . ? H36A C36 H36B 109.5 . . ? C38 C37 C36 99.8(8) . . ? C38 C37 H37A 111.8 . . ? C36 C37 H37A 111.8 . . ? C38 C37 H37B 111.8 . . ? C36 C37 H37B 111.8 . . ? H37A C37 H37B 109.5 . . ? C37A C38 O2 107.1(9) . . ? C37A C38 C37 29.4(8) . . ? O2 C38 C37 105.0(6) . . ? C37A C38 H38A 132.2 . . ? O2 C38 H38A 110.7 . . ? C37 C38 H38A 110.7 . . ? C37A C38 H38B 83.2 . . ? O2 C38 H38B 110.7 . . ? C37 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? O3 C39 C40 102.9(8) . . ? O3 C39 H39A 111.2 . . ? C40 C39 H39A 111.2 . . ? O3 C39 H39B 111.2 . . ? C40 C39 H39B 111.2 . . ? H39A C39 H39B 109.1 . . ? C39 C40 C41 100.1(9) . . ? C39 C40 H40A 111.7 . . ? C41 C40 H40A 111.7 . . ? C39 C40 H40B 111.7 . . ? C41 C40 H40B 111.7 . . ? H40A C40 H40B 109.5 . . ? C42 C41 C40 105.0(10) . . ? C42 C41 H41A 110.8 . . ? C40 C41 H41A 110.8 . . ? C42 C41 H41B 110.8 . . ? C40 C41 H41B 110.8 . . ? H41A C41 H41B 108.8 . . ? O3 C42 C41 103.7(10) . . ? O3 C42 H42A 111.0 . . ? C41 C42 H42A 111.0 . . ? O3 C42 H42B 111.0 . . ? C41 C42 H42B 111.0 . . ? H42A C42 H42B 109.0 . . ? C52 C51 C56 117.8(9) . . ? C52 C51 C57 121.7(11) . . ? C56 C51 C57 120.6(10) . . ? C51 C52 C53 122.6(9) . . ? C51 C52 H52 118.7 . . ? C53 C52 H52 118.7 . . ? C54 C53 C52 118.8(8) . . ? C54 C53 H53 120.6 . . ? C52 C53 H53 120.6 . . ? C53 C54 C55 120.7(9) . . ? C53 C54 H54 119.6 . . ? C55 C54 H54 119.6 . . ? C56 C55 C54 118.3(9) . . ? C56 C55 H55 120.9 . . ? C54 C55 H55 120.9 . . ? C55 C56 C51 121.7(8) . . ? C55 C56 H56 119.2 . . ? C51 C56 H56 119.2 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C37A C36A C35 94.0(13) . . ? C37A C36A H36C 112.9 . . ? C35 C36A H36C 112.9 . . ? C37A C36A H36D 112.9 . . ? C35 C36A H36D 112.9 . . ? H36C C36A H36D 110.3 . . ? C38 C37A C36A 93.0(14) . . ? C38 C37A H37C 113.1 . . ? C36A C37A H37C 113.1 . . ? C38 C37A H37D 113.1 . . ? C36A C37A H37D 113.1 . . ? H37C C37A H37D 110.5 . . ? O3 C39A C40A 100.1(13) . . ? O3 C39A H39C 111.8 . . ? C40A C39A H39C 111.8 . . ? O3 C39A H39D 111.8 . . ? C40A C39A H39D 111.8 . . ? H39C C39A H39D 109.5 . . ? C39A C40A C41A 112.3(17) . . ? C39A C40A H40C 109.2 . . ? C41A C40A H40C 109.2 . . ? C39A C40A H40D 109.2 . . ? C41A C40A H40D 109.2 . . ? H40C C40A H40D 107.9 . . ? C42A C41A C40A 96.8(15) . . ? C42A C41A H41C 112.4 . . ? C40A C41A H41C 112.4 . . ? C42A C41A H41D 112.4 . . ? C40A C41A H41D 112.4 . . ? H41C C41A H41D 110.0 . . ? O3 C42A C41A 108.6(13) . . ? O3 C42A H42C 110.0 . . ? C41A C42A H42C 110.0 . . ? O3 C42A H42D 110.0 . . ? C41A C42A H42D 110.0 . . ? H42C C42A H42D 108.4 . . ? 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 Ca1 Si1 N2 -179.2(2) . . . . ? O1 Ca1 Si1 N2 -94.64(19) . . . . ? O2 Ca1 Si1 N2 155.4(2) . . . . ? O3 Ca1 Si1 N2 39.7(2) . . . . ? O1 Ca1 Si1 N1 84.59(19) . . . . ? N2 Ca1 Si1 N1 179.2(2) . . . . ? O2 Ca1 Si1 N1 -25.3(2) . . . . ? O3 Ca1 Si1 N1 -141.1(2) . . . . ? N1 Ca1 Si1 C25 -85.6(2) . . . . ? O1 Ca1 Si1 C25 -1.0(2) . . . . ? N2 Ca1 Si1 C25 93.6(2) . . . . ? O2 Ca1 Si1 C25 -110.9(2) . . . . ? O3 Ca1 Si1 C25 133.3(2) . . . . ? N1 Ca1 O1 C34 -150.9(6) . . . . ? N2 Ca1 O1 C34 133.6(6) . . . . ? O2 Ca1 O1 C34 -50.9(6) . . . . ? O3 Ca1 O1 C34 31.8(6) . . . . ? Si1 Ca1 O1 C34 172.2(5) . . . . ? N1 Ca1 O1 C31 29.6(4) . . . . ? N2 Ca1 O1 C31 -45.9(4) . . . . ? O2 Ca1 O1 C31 129.6(4) . . . . ? O3 Ca1 O1 C31 -147.7(4) . . . . ? Si1 Ca1 O1 C31 -7.3(4) . . . . ? N1 Ca1 O2 C38 -151.3(5) . . . . ? O1 Ca1 O2 C38 100.3(5) . . . . ? N2 Ca1 O2 C38 -92.0(6) . . . . ? O3 Ca1 O2 C38 -7.3(5) . . . . ? Si1 Ca1 O2 C38 -136.9(4) . . . . ? N1 Ca1 O2 C35 36.8(5) . . . . ? O1 Ca1 O2 C35 -71.7(4) . . . . ? N2 Ca1 O2 C35 96.0(6) . . . . ? O3 Ca1 O2 C35 -179.3(4) . . . . ? Si1 Ca1 O2 C35 51.1(5) . . . . ? N1 Ca1 O3 C39A 18.6(13) . . . . ? O1 Ca1 O3 C39A -165.8(12) . . . . ? N2 Ca1 O3 C39A 77.3(12) . . . . ? O2 Ca1 O3 C39A -83.1(12) . . . . ? Si1 Ca1 O3 C39A 56.0(12) . . . . ? N1 Ca1 O3 C42 155.2(12) . . . . ? O1 Ca1 O3 C42 -29.2(13) . . . . ? N2 Ca1 O3 C42 -146.1(13) . . . . ? O2 Ca1 O3 C42 53.5(13) . . . . ? Si1 Ca1 O3 C42 -167.4(12) . . . . ? N1 Ca1 O3 C39 -17.2(7) . . . . ? O1 Ca1 O3 C39 158.5(6) . . . . ? N2 Ca1 O3 C39 41.6(6) . . . . ? O2 Ca1 O3 C39 -118.9(6) . . . . ? Si1 Ca1 O3 C39 20.2(6) . . . . ? N1 Ca1 O3 C42A -134.2(8) . . . . ? O1 Ca1 O3 C42A 41.4(8) . . . . ? N2 Ca1 O3 C42A -75.5(8) . . . . ? O2 Ca1 O3 C42A 124.0(8) . . . . ? Si1 Ca1 O3 C42A -96.9(8) . . . . ? N2 Si1 N1 C1 152.2(3) . . . . ? C25 Si1 N1 C1 -83.1(4) . . . . ? Ca1 Si1 N1 C1 151.6(4) . . . . ? N2 Si1 N1 Ca1 0.62(18) . . . . ? C25 Si1 N1 Ca1 125.25(16) . . . . ? O1 Ca1 N1 C1 102.0(4) . . . . ? N2 Ca1 N1 C1 -148.1(4) . . . . ? O2 Ca1 N1 C1 13.9(4) . . . . ? O3 Ca1 N1 C1 -82.5(4) . . . . ? Si1 Ca1 N1 C1 -147.7(4) . . . . ? O1 Ca1 N1 Si1 -110.37(16) . . . . ? N2 Ca1 N1 Si1 -0.47(14) . . . . ? O2 Ca1 N1 Si1 161.60(15) . . . . ? O3 Ca1 N1 Si1 65.2(3) . . . . ? N1 Si1 N2 C13 -171.9(4) . . . . ? C25 Si1 N2 C13 66.2(5) . . . . ? Ca1 Si1 N2 C13 -171.3(5) . . . . ? N1 Si1 N2 Ca1 -0.60(18) . . . . ? C25 Si1 N2 Ca1 -122.50(17) . . . . ? N1 Ca1 N2 C13 172.4(4) . . . . ? O1 Ca1 N2 C13 -85.3(4) . . . . ? O2 Ca1 N2 C13 108.1(5) . . . . ? O3 Ca1 N2 C13 24.9(4) . . . . ? Si1 Ca1 N2 C13 171.9(5) . . . . ? N1 Ca1 N2 Si1 0.47(14) . . . . ? O1 Ca1 N2 Si1 102.75(16) . . . . ? O2 Ca1 N2 Si1 -63.8(4) . . . . ? O3 Ca1 N2 Si1 -147.00(17) . . . . ? Si1 N1 C1 C9 -74.5(4) . . . . ? Ca1 N1 C1 C9 65.6(5) . . . . ? Si1 N1 C1 C2 108.6(4) . . . . ? Ca1 N1 C1 C2 -111.3(4) . . . . ? N1 C1 C2 C6 176.2(4) . . . . ? C9 C1 C2 C6 -0.8(6) . . . . ? N1 C1 C2 C3 -4.9(6) . . . . ? C9 C1 C2 C3 178.1(4) . . . . ? C6 C2 C3 C4 -56.1(7) . . . . ? C1 C2 C3 C4 125.0(6) . . . . ? C6 C2 C3 C5 69.0(6) . . . . ? C1 C2 C3 C5 -109.8(5) . . . . ? C1 C2 C6 C7 2.8(7) . . . . ? C3 C2 C6 C7 -176.0(4) . . . . ? C2 C6 C7 C8 -2.8(7) . . . . ? C6 C7 C8 C9 0.8(7) . . . . ? C7 C8 C9 C1 1.2(7) . . . . ? C7 C8 C9 C10 -178.2(5) . . . . ? N1 C1 C9 C8 -178.2(4) . . . . ? C2 C1 C9 C8 -1.1(6) . . . . ? N1 C1 C9 C10 1.1(6) . . . . ? C2 C1 C9 C10 178.2(4) . . . . ? C8 C9 C10 C11 -56.5(6) . . . . ? C1 C9 C10 C11 124.3(5) . . . . ? C8 C9 C10 C12 69.2(5) . . . . ? C1 C9 C10 C12 -110.1(5) . . . . ? Si1 N2 C13 C14 -126.8(4) . . . . ? Ca1 N2 C13 C14 64.7(5) . . . . ? Si1 N2 C13 C21 58.3(6) . . . . ? Ca1 N2 C13 C21 -110.2(4) . . . . ? N2 C13 C14 C18 -178.1(4) . . . . ? C21 C13 C14 C18 -2.8(6) . . . . ? N2 C13 C14 C15 4.3(6) . . . . ? C21 C13 C14 C15 179.5(4) . . . . ? C18 C14 C15 C17 -88.2(6) . . . . ? C13 C14 C15 C17 89.5(5) . . . . ? C18 C14 C15 C16 31.0(8) . . . . ? C13 C14 C15 C16 -151.3(6) . . . . ? C13 C14 C18 C19 0.6(7) . . . . ? C15 C14 C18 C19 178.3(5) . . . . ? C14 C18 C19 C20 0.9(8) . . . . ? C18 C19 C20 C21 -0.2(8) . . . . ? C19 C20 C21 C13 -2.2(7) . . . . ? C19 C20 C21 C22 178.4(5) . . . . ? N2 C13 C21 C20 178.6(4) . . . . ? C14 C13 C21 C20 3.6(6) . . . . ? N2 C13 C21 C22 -1.9(6) . . . . ? C14 C13 C21 C22 -177.0(4) . . . . ? C20 C21 C22 C23 77.1(5) . . . . ? C13 C21 C22 C23 -102.3(5) . . . . ? C20 C21 C22 C24 -45.1(6) . . . . ? C13 C21 C22 C24 135.5(5) . . . . ? N2 Si1 C25 C26 61.6(4) . . . . ? N1 Si1 C25 C26 -54.8(4) . . . . ? Ca1 Si1 C25 C26 0.6(5) . . . . ? N2 Si1 C25 C30 -126.8(3) . . . . ? N1 Si1 C25 C30 116.9(3) . . . . ? Ca1 Si1 C25 C30 172.2(3) . . . . ? C30 C25 C26 C27 0.4(7) . . . . ? Si1 C25 C26 C27 172.3(4) . . . . ? C25 C26 C27 C28 -0.6(9) . . . . ? C26 C27 C28 C29 0.8(9) . . . . ? C27 C28 C29 C30 -0.9(8) . . . . ? C26 C25 C30 C29 -0.5(7) . . . . ? Si1 C25 C30 C29 -172.8(4) . . . . ? C28 C29 C30 C25 0.7(8) . . . . ? C34 O1 C31 C32 -18.7(7) . . . . ? Ca1 O1 C31 C32 160.8(4) . . . . ? O1 C31 C32 C33 14.3(8) . . . . ? C31 C32 C33 C34 -4.7(10) . . . . ? C32 C33 C34 O1 -6.9(10) . . . . ? C31 O1 C34 C33 16.4(9) . . . . ? Ca1 O1 C34 C33 -163.2(5) . . . . ? C38 O2 C35 C36 -17.4(9) . . . . ? Ca1 O2 C35 C36 156.6(7) . . . . ? C38 O2 C35 C36A 21.1(9) . . . . ? Ca1 O2 C35 C36A -164.9(8) . . . . ? O2 C35 C36 C37 37.3(12) . . . . ? C36A C35 C36 C37 -40.5(11) . . . . ? C35 C36 C37 C38 -41.9(12) . . . . ? C35 O2 C38 C37A 19.1(11) . . . . ? Ca1 O2 C38 C37A -153.3(10) . . . . ? C35 O2 C38 C37 -11.4(8) . . . . ? Ca1 O2 C38 C37 176.1(6) . . . . ? C36 C37 C38 C37A -65.4(18) . . . . ? C36 C37 C38 O2 32.8(11) . . . . ? C39A O3 C39 C40 128(2) . . . . ? C42 O3 C39 C40 50.5(12) . . . . ? C42A O3 C39 C40 -5.2(10) . . . . ? Ca1 O3 C39 C40 -135.0(6) . . . . ? O3 C39 C40 C41 -36.0(11) . . . . ? C39 C40 C41 C42 11.4(15) . . . . ? C39A O3 C42 C41 -72.6(16) . . . . ? C39 O3 C42 C41 -41.8(15) . . . . ? C42A O3 C42 C41 44.8(11) . . . . ? Ca1 O3 C42 C41 145.1(8) . . . . ? C40 C41 C42 O3 17.4(17) . . . . ? C56 C51 C52 C53 2.7(11) . . . . ? C57 C51 C52 C53 -177.6(8) . . . . ? C51 C52 C53 C54 -1.3(11) . . . . ? C52 C53 C54 C55 0.0(11) . . . . ? C53 C54 C55 C56 -0.3(11) . . . . ? C54 C55 C56 C51 1.8(11) . . . . ? C52 C51 C56 C55 -3.0(11) . . . . ? C57 C51 C56 C55 177.3(8) . . . . ? C36 C35 C36A C37A 61.3(13) . . . . ? O2 C35 C36A C37A -49.6(14) . . . . ? O2 C38 C37A C36A -51.0(16) . . . . ? C37 C38 C37A C36A 39.5(14) . . . . ? C35 C36A C37A C38 59.9(15) . . . . ? C42 O3 C39A C40A 44.0(18) . . . . ? C39 O3 C39A C40A -64.2(18) . . . . ? C42A O3 C39A C40A -10(2) . . . . ? Ca1 O3 C39A C40A -164.6(12) . . . . ? O3 C39A C40A C41A 23(3) . . . . ? C39A C40A C41A C42A -25(3) . . . . ? C39A O3 C42A C41A -5(2) . . . . ? C42 O3 C42A C41A -84.4(18) . . . . ? C39 O3 C42A C41A 19.6(18) . . . . ? Ca1 O3 C42A C41A 148.0(15) . . . . ? C40A C41A C42A O3 18(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.590 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 945788' ####################################################################### # # 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_k12msh20 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H71 N2 O4 Si Sr' _chemical_formula_weight 831.76 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' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.3700(3) _cell_length_b 18.8520(8) _cell_length_c 12.6320(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.607(2) _cell_angle_gamma 90.00 _cell_volume 2262.83(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 142823 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 1.260 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.599 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37584 _diffrn_reflns_av_R_equivalents 0.1217 _diffrn_reflns_av_sigmaI/netI 0.1135 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.52 _reflns_number_total 10228 _reflns_number_gt 7151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0375P)^2^+1.0216P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(6) _chemical_absolute_configuration ; absolute configuration established by anomalous dispersion effects in diffraction measurements on the crystal. ; _refine_ls_number_reflns 10228 _refine_ls_number_parameters 544 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.031 _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 Sr1 Sr 0.31982(4) 0.83650(2) 0.75098(3) 0.03438(11) Uani 1 1 d . C . Si1 Si 0.04631(14) 0.92083(6) 0.71849(11) 0.0313(3) Uani 1 1 d . C . O1 O 0.2443(4) 0.70603(16) 0.6957(3) 0.0527(10) Uani 1 1 d . . . O2 O 0.3787(4) 0.81076(19) 0.5733(3) 0.0583(11) Uani 1 1 d . . . O3 O 0.4827(4) 0.77246(17) 0.9449(3) 0.0510(9) Uani 1 1 d D . . O4 O 0.5341(4) 0.91827(16) 0.8363(3) 0.0479(9) Uani 1 1 d . . . N1 N 0.1661(4) 0.88485(17) 0.8428(3) 0.0341(9) Uani 1 1 d . . . N2 N 0.1232(4) 0.91335(17) 0.6234(3) 0.0326(8) Uani 1 1 d . . . C1 C -0.0090(5) 1.0151(2) 0.7321(4) 0.0355(11) Uani 1 1 d . . . C2 C -0.1487(6) 1.0306(2) 0.7136(4) 0.0418(12) Uani 1 1 d . C . H2 H -0.2164 0.9936 0.6905 0.050 Uiso 1 1 calc R . . C3 C -0.1908(6) 1.0984(2) 0.7281(5) 0.0505(14) Uani 1 1 d . . . H3 H -0.2861 1.1076 0.7147 0.061 Uiso 1 1 calc R C . C4 C -0.0933(8) 1.1524(3) 0.7619(5) 0.0587(17) Uani 1 1 d . C . H4 H -0.1211 1.1986 0.7740 0.070 Uiso 1 1 calc R . . C5 C 0.0439(7) 1.1399(3) 0.7783(5) 0.0519(15) Uani 1 1 d . . . H5 H 0.1099 1.1777 0.8001 0.062 Uiso 1 1 calc R C . C6 C 0.0858(6) 1.0729(2) 0.7633(4) 0.0437(12) Uani 1 1 d . C . H6 H 0.1808 1.0652 0.7742 0.052 Uiso 1 1 calc R . . C7 C 0.0782(5) 0.9417(2) 0.5119(4) 0.0306(10) Uani 1 1 d . C . C8 C -0.0456(5) 0.9188(2) 0.4200(4) 0.0321(10) Uani 1 1 d . . . C9 C -0.1385(5) 0.8609(2) 0.4377(4) 0.0382(11) Uani 1 1 d . C . H9 H -0.0886 0.8419 0.5177 0.046 Uiso 1 1 calc R . . C10 C -0.1602(7) 0.7990(2) 0.3532(5) 0.0508(14) Uani 1 1 d . . . H10A H -0.2155 0.7618 0.3696 0.076 Uiso 1 1 calc R C . H10B H -0.0685 0.7799 0.3623 0.076 Uiso 1 1 calc R . . H10C H -0.2105 0.8160 0.2738 0.076 Uiso 1 1 calc R . . C11 C -0.2778(6) 0.8920(3) 0.4290(5) 0.0545(14) Uani 1 1 d . . . H11A H -0.2601 0.9284 0.4886 0.082 Uiso 1 1 calc R C . H11B H -0.3361 0.8543 0.4403 0.082 Uiso 1 1 calc R . . H11C H -0.3270 0.9133 0.3525 0.082 Uiso 1 1 calc R . . C12 C -0.0867(6) 0.9479(2) 0.3096(4) 0.0402(12) Uani 1 1 d . C . H12 H -0.1717 0.9325 0.2493 0.048 Uiso 1 1 calc R . . C13 C -0.0039(6) 0.9995(2) 0.2868(5) 0.0427(12) Uani 1 1 d . . . H13 H -0.0315 1.0191 0.2116 0.051 Uiso 1 1 calc R C . C14 C 0.1156(6) 1.0208(2) 0.3739(4) 0.0381(12) Uani 1 1 d . C . H14 H 0.1717 1.0556 0.3580 0.046 Uiso 1 1 calc R . . C15 C 0.1614(5) 0.9945(2) 0.4860(4) 0.0369(11) Uani 1 1 d . . . C16 C 0.2973(6) 1.0220(2) 0.5790(5) 0.0438(12) Uani 1 1 d . C . H16 H 0.3062 1.0011 0.6544 0.053 Uiso 1 1 calc R . . C17 C 0.2973(7) 1.1029(3) 0.5904(5) 0.0544(15) Uani 1 1 d . . . H17A H 0.2913 1.1247 0.5182 0.082 Uiso 1 1 calc R C . H17B H 0.3844 1.1181 0.6539 0.082 Uiso 1 1 calc R . . H17C H 0.2163 1.1176 0.6065 0.082 Uiso 1 1 calc R . . C18 C 0.4238(7) 0.9988(3) 0.5569(6) 0.0671(17) Uani 1 1 d . . . H18A H 0.4268 0.9469 0.5547 0.101 Uiso 1 1 calc R C . H18B H 0.5098 1.0165 0.6188 0.101 Uiso 1 1 calc R . . H18C H 0.4168 1.0180 0.4827 0.101 Uiso 1 1 calc R . . C19 C 0.1274(6) 0.8694(2) 0.9360(4) 0.0315(11) Uani 1 1 d . C . C20 C 0.0534(6) 0.8057(2) 0.9378(4) 0.0371(12) Uani 1 1 d . . . C21 C 0.0194(6) 0.7501(2) 0.8440(4) 0.0405(12) Uani 1 1 d . C . H21 H 0.0501 0.7691 0.7839 0.049 Uiso 1 1 calc R . . C22 C 0.1021(7) 0.6816(2) 0.8913(5) 0.0561(16) Uani 1 1 d . . . H22A H 0.2029 0.6924 0.9273 0.084 Uiso 1 1 calc R C . H22B H 0.0839 0.6479 0.8279 0.084 Uiso 1 1 calc R . . H22C H 0.0722 0.6608 0.9489 0.084 Uiso 1 1 calc R . . C23 C -0.1371(7) 0.7337(3) 0.7848(5) 0.0604(16) Uani 1 1 d . . . H23A H -0.1528 0.6982 0.7243 0.091 Uiso 1 1 calc R C . H23B H -0.1886 0.7772 0.7503 0.091 Uiso 1 1 calc R . . H23C H -0.1706 0.7152 0.8418 0.091 Uiso 1 1 calc R . . C24 C 0.0201(6) 0.7919(2) 1.0314(4) 0.0431(13) Uani 1 1 d . C . H24 H -0.0306 0.7498 1.0311 0.052 Uiso 1 1 calc R . . C25 C 0.0574(5) 0.8366(3) 1.1247(4) 0.0460(11) Uani 1 1 d . . . H25 H 0.0319 0.8260 1.1873 0.055 Uiso 1 1 calc R C . C26 C 0.1329(6) 0.8973(2) 1.1257(4) 0.0432(12) Uani 1 1 d . C . H26 H 0.1618 0.9278 1.1910 0.052 Uiso 1 1 calc R . . C27 C 0.1674(5) 0.9145(2) 1.0332(4) 0.0357(11) Uani 1 1 d . . . C28 C 0.2474(5) 0.9832(2) 1.0397(4) 0.0377(11) Uani 1 1 d . C . H28 H 0.2613 0.9883 0.9662 0.045 Uiso 1 1 calc R . . C29 C 0.1634(7) 1.0479(2) 1.0517(5) 0.0494(14) Uani 1 1 d . . . H29A H 0.0672 1.0458 0.9922 0.074 Uiso 1 1 calc R C . H29B H 0.2090 1.0916 1.0423 0.074 Uiso 1 1 calc R . . H29C H 0.1605 1.0476 1.1283 0.074 Uiso 1 1 calc R . . C30 C 0.3907(7) 0.9831(3) 1.1391(5) 0.0580(15) Uani 1 1 d . . . H30A H 0.3792 0.9815 1.2124 0.087 Uiso 1 1 calc R C . H30B H 0.4417 1.0263 1.1361 0.087 Uiso 1 1 calc R . . H30C H 0.4439 0.9414 1.1331 0.087 Uiso 1 1 calc R . . C31 C 0.2847(6) 0.8119(3) 0.4515(5) 0.0585(15) Uani 1 1 d . . . H31A H 0.2377 0.8586 0.4302 0.070 Uiso 1 1 calc R . . H31B H 0.2116 0.7747 0.4346 0.070 Uiso 1 1 calc R . . C32 C 0.3724(6) 0.7984(3) 0.3867(5) 0.0517(14) Uani 1 1 d . . . H32A H 0.4153 0.8428 0.3739 0.062 Uiso 1 1 calc R . . H32B H 0.3175 0.7758 0.3113 0.062 Uiso 1 1 calc R . . C33 C 0.4817(7) 0.7491(3) 0.4660(6) 0.0601(17) Uani 1 1 d . . . H33A H 0.5680 0.7497 0.4506 0.072 Uiso 1 1 calc R . . H33B H 0.4457 0.6999 0.4586 0.072 Uiso 1 1 calc R . . C34 C 0.5086(7) 0.7795(3) 0.5835(5) 0.0615(16) Uani 1 1 d . . . H34A H 0.5372 0.7417 0.6428 0.074 Uiso 1 1 calc R . . H34B H 0.5839 0.8158 0.6054 0.074 Uiso 1 1 calc R . . C35 C 0.1140(7) 0.6892(3) 0.6037(5) 0.0597(16) Uani 1 1 d . . . H35A H 0.0826 0.7291 0.5481 0.072 Uiso 1 1 calc R . . H35B H 0.0410 0.6802 0.6339 0.072 Uiso 1 1 calc R . . C36 C 0.1371(8) 0.6236(3) 0.5449(6) 0.0673(18) Uani 1 1 d . . . H36A H 0.0754 0.5845 0.5486 0.081 Uiso 1 1 calc R . . H36B H 0.1176 0.6334 0.4629 0.081 Uiso 1 1 calc R . . C37 C 0.2862(8) 0.6053(3) 0.6097(6) 0.072(2) Uani 1 1 d . . . H37A H 0.3437 0.6213 0.5677 0.086 Uiso 1 1 calc R . . H37B H 0.2980 0.5534 0.6221 0.086 Uiso 1 1 calc R . . C38 C 0.3275(7) 0.6430(3) 0.7209(5) 0.0622(17) Uani 1 1 d . . . H38A H 0.3083 0.6134 0.7777 0.075 Uiso 1 1 calc R . . H38B H 0.4290 0.6549 0.7528 0.075 Uiso 1 1 calc R . . C39 C 0.5318(7) 0.9863(3) 0.8885(5) 0.0604(16) Uani 1 1 d D B . H39A H 0.4535 0.9882 0.9144 0.073 Uiso 1 1 calc R A 1 H39B H 0.5193 1.0251 0.8324 0.073 Uiso 1 1 calc R A 1 C40 C 0.6669(10) 0.9932(6) 0.9870(9) 0.066(4) Uani 0.70 1 d PDU B 1 H40A H 0.6611 0.9744 1.0581 0.079 Uiso 0.70 1 calc PR B 1 H40B H 0.6967 1.0435 0.9997 0.079 Uiso 0.70 1 calc PR B 1 C41 C 0.7668(7) 0.9505(4) 0.9549(6) 0.0747(19) Uani 1 1 d D . . H41A H 0.8203 0.9816 0.9238 0.090 Uiso 1 1 calc R B 1 H41B H 0.8341 0.9250 1.0231 0.090 Uiso 1 1 calc R B 1 C42 C 0.6796(6) 0.8995(3) 0.8657(5) 0.0549(14) Uani 1 1 d . B . H42A H 0.7019 0.9025 0.7966 0.066 Uiso 1 1 calc R . . H42B H 0.6980 0.8505 0.8961 0.066 Uiso 1 1 calc R . . C43 C 0.4889(19) 0.8170(6) 1.0392(12) 0.045(4) Uani 0.50 1 d PDU C 1 H43A H 0.4149 0.8539 1.0124 0.054 Uiso 0.50 1 calc PR C 1 H43B H 0.5819 0.8403 1.0755 0.054 Uiso 0.50 1 calc PR C 1 C44 C 0.4646(17) 0.7666(9) 1.1240(13) 0.058(4) Uani 0.50 1 d PDU C 1 H44A H 0.5137 0.7831 1.2047 0.069 Uiso 0.50 1 calc PR C 1 H44B H 0.3631 0.7609 1.1061 0.069 Uiso 0.50 1 calc PR C 1 C45 C 0.528(3) 0.6980(10) 1.103(2) 0.069(8) Uani 0.50 1 d PDU C 1 H45A H 0.6137 0.6853 1.1721 0.082 Uiso 0.50 1 calc PR C 1 H45B H 0.4599 0.6586 1.0862 0.082 Uiso 0.50 1 calc PR C 1 C46 C 0.565(2) 0.7126(10) 1.0010(17) 0.075(7) Uani 0.50 1 d PDU C 1 H46A H 0.6663 0.7231 1.0267 0.089 Uiso 0.50 1 calc PR C 1 H46B H 0.5411 0.6713 0.9483 0.089 Uiso 0.50 1 calc PR C 1 C40A C 0.6772(14) 1.0128(9) 0.944(3) 0.068(9) Uani 0.30 1 d PDU B 2 H40C H 0.6950 1.0498 0.8960 0.081 Uiso 0.30 1 calc PR B 2 H40D H 0.6952 1.0330 1.0211 0.081 Uiso 0.30 1 calc PR B 2 C43A C 0.456(2) 0.7882(9) 1.0467(13) 0.066(5) Uani 0.50 1 d PDU C 2 H43C H 0.3578 0.8039 1.0244 0.080 Uiso 0.50 1 calc PR C 2 H43D H 0.5200 0.8261 1.0927 0.080 Uiso 0.50 1 calc PR C 2 C44A C 0.484(2) 0.7188(14) 1.1171(17) 0.068(7) Uani 0.50 1 d PDU C 2 H44C H 0.5420 0.7273 1.2000 0.081 Uiso 0.50 1 calc PR C 2 H44D H 0.3945 0.6956 1.1090 0.081 Uiso 0.50 1 calc PR C 2 C45A C 0.5617(19) 0.6758(8) 1.0609(19) 0.066(5) Uani 0.50 1 d PDU C 2 H45C H 0.5019 0.6362 1.0162 0.080 Uiso 0.50 1 calc PR C 2 H45D H 0.6484 0.6556 1.1207 0.080 Uiso 0.50 1 calc PR C 2 C46A C 0.599(2) 0.7240(11) 0.981(2) 0.063(6) Uani 0.50 1 d PDU C 2 H1 H -0.083(5) 0.888(2) 0.694(3) 0.027(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sr1 0.0383(2) 0.02716(17) 0.0358(2) 0.0000(2) 0.01283(17) 0.0026(2) Si1 0.0380(8) 0.0217(5) 0.0346(7) 0.0013(5) 0.0150(6) 0.0009(5) O1 0.062(3) 0.0301(16) 0.056(2) -0.0077(16) 0.014(2) -0.0012(17) O2 0.056(3) 0.072(3) 0.052(2) -0.0083(17) 0.028(2) 0.0048(19) O3 0.061(3) 0.0387(18) 0.048(2) 0.0056(16) 0.017(2) 0.0114(17) O4 0.048(2) 0.0370(17) 0.055(2) -0.0051(16) 0.0158(19) -0.0025(16) N1 0.047(3) 0.0221(17) 0.033(2) -0.0001(15) 0.015(2) 0.0040(16) N2 0.038(2) 0.0220(17) 0.037(2) -0.0007(16) 0.0145(19) -0.0020(16) C1 0.046(3) 0.025(2) 0.034(3) 0.0007(19) 0.015(2) 0.000(2) C2 0.052(4) 0.027(2) 0.049(3) -0.002(2) 0.023(3) 0.001(2) C3 0.059(4) 0.037(3) 0.058(4) 0.000(2) 0.025(3) 0.016(3) C4 0.095(5) 0.027(2) 0.048(3) 0.001(2) 0.022(3) 0.017(3) C5 0.067(4) 0.029(2) 0.048(3) -0.002(2) 0.011(3) -0.003(3) C6 0.056(4) 0.028(2) 0.041(3) 0.006(2) 0.013(3) 0.002(2) C7 0.039(3) 0.023(2) 0.036(3) 0.0011(18) 0.021(2) 0.0030(19) C8 0.035(3) 0.026(2) 0.033(2) -0.0006(19) 0.011(2) 0.0008(19) C9 0.041(3) 0.029(2) 0.042(3) 0.0018(19) 0.013(2) -0.006(2) C10 0.068(4) 0.030(2) 0.053(3) -0.004(2) 0.023(3) -0.007(3) C11 0.051(4) 0.045(3) 0.073(4) 0.005(3) 0.030(3) -0.005(3) C12 0.045(3) 0.033(2) 0.036(3) -0.003(2) 0.011(2) 0.002(2) C13 0.061(4) 0.031(2) 0.039(3) 0.009(2) 0.023(3) 0.004(2) C14 0.048(3) 0.029(2) 0.044(3) 0.003(2) 0.025(3) -0.001(2) C15 0.044(3) 0.027(2) 0.043(3) 0.000(2) 0.021(3) 0.004(2) C16 0.043(3) 0.035(3) 0.053(3) -0.001(2) 0.019(3) -0.008(2) C17 0.068(4) 0.035(3) 0.055(3) -0.005(2) 0.019(3) -0.017(3) C18 0.049(4) 0.066(4) 0.080(4) -0.007(3) 0.019(4) -0.008(3) C19 0.039(3) 0.0238(19) 0.030(2) 0.0022(18) 0.012(2) 0.007(2) C20 0.042(3) 0.025(2) 0.043(3) 0.0012(19) 0.015(3) 0.000(2) C21 0.052(3) 0.021(2) 0.051(3) -0.003(2) 0.023(3) -0.005(2) C22 0.080(5) 0.025(2) 0.058(3) -0.004(2) 0.023(3) -0.002(3) C23 0.066(4) 0.042(3) 0.068(4) -0.004(3) 0.021(3) -0.002(3) C24 0.062(4) 0.022(2) 0.049(3) 0.006(2) 0.025(3) -0.002(2) C25 0.062(3) 0.037(2) 0.045(2) 0.009(3) 0.028(2) 0.003(3) C26 0.061(4) 0.033(2) 0.037(3) 0.002(2) 0.021(3) 0.007(2) C27 0.042(3) 0.027(2) 0.033(2) 0.001(2) 0.010(2) 0.006(2) C28 0.045(3) 0.027(2) 0.041(3) -0.008(2) 0.017(3) -0.004(2) C29 0.072(4) 0.029(2) 0.052(3) -0.004(2) 0.031(3) 0.000(2) C30 0.056(4) 0.044(3) 0.066(4) -0.009(3) 0.017(3) -0.004(3) C31 0.051(4) 0.062(4) 0.060(4) -0.015(3) 0.019(3) -0.003(3) C32 0.051(4) 0.052(3) 0.053(3) -0.011(3) 0.023(3) -0.005(3) C33 0.072(5) 0.037(3) 0.089(5) -0.009(3) 0.050(4) -0.005(3) C34 0.053(4) 0.074(4) 0.057(4) 0.013(3) 0.023(3) 0.014(3) C35 0.066(5) 0.048(3) 0.059(4) -0.003(3) 0.018(4) 0.005(3) C36 0.092(6) 0.054(3) 0.062(4) -0.020(3) 0.037(4) -0.021(3) C37 0.071(5) 0.043(3) 0.104(6) -0.023(4) 0.038(4) -0.002(3) C38 0.061(4) 0.035(3) 0.074(4) -0.002(3) 0.009(3) 0.007(3) C39 0.063(4) 0.045(3) 0.069(4) -0.007(3) 0.023(4) 0.003(3) C40 0.063(7) 0.051(6) 0.052(6) -0.003(5) -0.011(5) -0.001(5) C41 0.047(4) 0.096(5) 0.074(5) -0.017(4) 0.016(4) -0.008(4) C42 0.050(4) 0.049(3) 0.070(4) -0.001(3) 0.029(3) 0.000(3) C43 0.042(8) 0.041(9) 0.041(6) -0.003(5) 0.005(6) 0.001(5) C44 0.056(9) 0.066(9) 0.045(8) -0.002(8) 0.014(7) -0.019(8) C45 0.080(18) 0.044(11) 0.066(13) 0.018(9) 0.011(10) 0.001(10) C46 0.121(18) 0.064(12) 0.029(7) 0.015(8) 0.020(10) 0.059(13) C40A 0.056(15) 0.033(11) 0.074(17) 0.002(11) -0.017(12) -0.007(9) C43A 0.048(11) 0.068(12) 0.076(12) -0.011(11) 0.018(9) 0.015(9) C44A 0.060(13) 0.085(16) 0.034(8) 0.003(11) -0.005(8) -0.004(12) C45A 0.067(10) 0.043(8) 0.089(13) 0.022(8) 0.032(9) 0.018(7) C46A 0.061(10) 0.066(9) 0.072(14) 0.024(8) 0.036(9) 0.003(7) _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 Sr1 N1 2.489(4) . ? Sr1 N2 2.494(4) . ? Sr1 O4 2.561(4) . ? Sr1 O1 2.591(3) . ? Sr1 O2 2.597(3) . ? Sr1 O3 2.645(3) . ? Si1 N2 1.693(4) . ? Si1 N1 1.704(4) . ? Si1 C1 1.897(4) . ? Si1 H1 1.39(4) . ? O1 C35 1.421(7) . ? O1 C38 1.427(6) . ? O2 C34 1.428(7) . ? O2 C31 1.455(7) . ? O3 C46 1.419(11) . ? O3 C46A 1.434(13) . ? O3 C43 1.437(11) . ? O3 C43A 1.449(12) . ? O4 C42 1.446(7) . ? O4 C39 1.446(6) . ? N1 C19 1.417(6) . ? N2 C7 1.401(6) . ? C1 C2 1.402(7) . ? C1 C6 1.413(7) . ? C2 C3 1.386(6) . ? C2 H2 0.9500 . ? C3 C4 1.376(8) . ? C3 H3 0.9500 . ? C4 C5 1.373(9) . ? C4 H4 0.9500 . ? C5 C6 1.373(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.411(7) . ? C7 C15 1.438(6) . ? C8 C12 1.397(6) . ? C8 C9 1.530(6) . ? C9 C11 1.521(8) . ? C9 C10 1.536(6) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.402(7) . ? C12 H12 0.9500 . ? C13 C14 1.348(7) . ? C13 H13 0.9500 . ? C14 C15 1.391(7) . ? C14 H14 0.9500 . ? C15 C16 1.519(7) . ? C16 C18 1.511(8) . ? C16 C17 1.532(7) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C27 1.413(6) . ? C19 C20 1.431(6) . ? C20 C24 1.383(7) . ? C20 C21 1.514(6) . ? C21 C23 1.522(8) . ? C21 C22 1.532(7) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.373(7) . ? C24 H24 0.9500 . ? C25 C26 1.385(7) . ? C25 H25 0.9500 . ? C26 C27 1.391(6) . ? C26 H26 0.9500 . ? C27 C28 1.521(6) . ? C28 C30 1.513(8) . ? C28 C29 1.542(6) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.469(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.498(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.509(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.510(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.471(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.477(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.460(10) . ? C39 C40A 1.473(15) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.491(11) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C40A 1.469(14) . ? C41 C42 1.481(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.527(16) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.52(2) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.51(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? C43A C44A 1.54(2) . ? C43A H43C 0.9900 . ? C43A H43D 0.9900 . ? C44A C45A 1.51(2) . ? C44A H44C 0.9900 . ? C44A H44D 0.9900 . ? C45A C46A 1.516(18) . ? C45A H45C 0.9900 . ? C45A H45D 0.9900 . ? 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 Sr1 N2 65.04(12) . . ? N1 Sr1 O4 101.15(12) . . ? N2 Sr1 O4 105.62(11) . . ? N1 Sr1 O1 107.00(12) . . ? N2 Sr1 O1 107.25(12) . . ? O4 Sr1 O1 143.37(12) . . ? N1 Sr1 O2 152.50(13) . . ? N2 Sr1 O2 87.95(12) . . ? O4 Sr1 O2 90.66(12) . . ? O1 Sr1 O2 74.92(12) . . ? N1 Sr1 O3 91.50(12) . . ? N2 Sr1 O3 156.49(11) . . ? O4 Sr1 O3 76.14(11) . . ? O1 Sr1 O3 80.12(11) . . ? O2 Sr1 O3 115.55(12) . . ? N2 Si1 N1 104.10(19) . . ? N2 Si1 C1 112.83(18) . . ? N1 Si1 C1 115.1(2) . . ? N2 Si1 H1 119.2(16) . . ? N1 Si1 H1 108.2(17) . . ? C1 Si1 H1 97.8(16) . . ? C35 O1 C38 106.8(4) . . ? C35 O1 Sr1 121.2(3) . . ? C38 O1 Sr1 129.8(3) . . ? C34 O2 C31 108.0(4) . . ? C34 O2 Sr1 122.6(3) . . ? C31 O2 Sr1 128.4(3) . . ? C46 O3 C46A 22.3(10) . . ? C46 O3 C43 103.4(11) . . ? C46A O3 C43 110.7(14) . . ? C46 O3 C43A 90.5(10) . . ? C46A O3 C43A 106.2(12) . . ? C43 O3 C43A 26.7(7) . . ? C46 O3 Sr1 149.0(9) . . ? C46A O3 Sr1 136.9(10) . . ? C43 O3 Sr1 107.5(7) . . ? C43A O3 Sr1 116.8(8) . . ? C42 O4 C39 107.8(4) . . ? C42 O4 Sr1 127.0(3) . . ? C39 O4 Sr1 123.7(3) . . ? C19 N1 Si1 120.2(3) . . ? C19 N1 Sr1 139.3(3) . . ? Si1 N1 Sr1 94.77(15) . . ? C7 N2 Si1 128.3(3) . . ? C7 N2 Sr1 136.8(3) . . ? Si1 N2 Sr1 94.90(16) . . ? C2 C1 C6 116.3(4) . . ? C2 C1 Si1 120.6(3) . . ? C6 C1 Si1 123.0(4) . . ? C3 C2 C1 121.9(5) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C4 C3 C2 119.5(5) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 120.5(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 120.2(5) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 121.5(5) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? N2 C7 C8 122.5(4) . . ? N2 C7 C15 120.3(4) . . ? C8 C7 C15 117.1(4) . . ? C12 C8 C7 121.0(4) . . ? C12 C8 C9 117.9(4) . . ? C7 C8 C9 121.1(4) . . ? C11 C9 C8 110.5(4) . . ? C11 C9 C10 111.8(5) . . ? C8 C9 C10 111.5(4) . . ? C11 C9 H9 107.6 . . ? C8 C9 H9 107.6 . . ? C10 C9 H9 107.6 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 C13 120.7(5) . . ? C8 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 118.5(5) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C15 123.5(4) . . ? C13 C14 H14 118.3 . . ? C15 C14 H14 118.3 . . ? C14 C15 C7 119.2(5) . . ? C14 C15 C16 119.9(4) . . ? C7 C15 C16 121.0(4) . . ? C18 C16 C15 111.3(4) . . ? C18 C16 C17 109.7(4) . . ? C15 C16 C17 112.1(4) . . ? C18 C16 H16 107.8 . . ? C15 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C27 C19 N1 121.0(4) . . ? C27 C19 C20 117.6(4) . . ? N1 C19 C20 121.2(4) . . ? C24 C20 C19 119.4(4) . . ? C24 C20 C21 118.7(4) . . ? C19 C20 C21 121.7(4) . . ? C20 C21 C23 113.1(4) . . ? C20 C21 C22 111.1(4) . . ? C23 C21 C22 109.9(4) . . ? C20 C21 H21 107.5 . . ? C23 C21 H21 107.5 . . ? C22 C21 H21 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C20 122.5(4) . . ? C25 C24 H24 118.7 . . ? C20 C24 H24 118.7 . . ? C24 C25 C26 118.7(4) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? C25 C26 C27 121.3(4) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C19 120.3(4) . . ? C26 C27 C28 118.1(4) . . ? C19 C27 C28 121.6(4) . . ? C30 C28 C27 112.2(4) . . ? C30 C28 C29 109.0(4) . . ? C27 C28 C29 111.2(4) . . ? C30 C28 H28 108.1 . . ? C27 C28 H28 108.1 . . ? C29 C28 H28 108.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O2 C31 C32 106.5(5) . . ? O2 C31 H31A 110.4 . . ? C32 C31 H31A 110.4 . . ? O2 C31 H31B 110.4 . . ? C32 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C31 C32 C33 101.9(5) . . ? C31 C32 H32A 111.4 . . ? C33 C32 H32A 111.4 . . ? C31 C32 H32B 111.4 . . ? C33 C32 H32B 111.4 . . ? H32A C32 H32B 109.3 . . ? C32 C33 C34 102.3(4) . . ? C32 C33 H33A 111.3 . . ? C34 C33 H33A 111.3 . . ? C32 C33 H33B 111.3 . . ? C34 C33 H33B 111.3 . . ? H33A C33 H33B 109.2 . . ? O2 C34 C33 105.8(5) . . ? O2 C34 H34A 110.6 . . ? C33 C34 H34A 110.6 . . ? O2 C34 H34B 110.6 . . ? C33 C34 H34B 110.6 . . ? H34A C34 H34B 108.7 . . ? O1 C35 C36 107.4(5) . . ? O1 C35 H35A 110.2 . . ? C36 C35 H35A 110.2 . . ? O1 C35 H35B 110.2 . . ? C36 C35 H35B 110.2 . . ? H35A C35 H35B 108.5 . . ? C37 C36 C35 104.9(5) . . ? C37 C36 H36A 110.8 . . ? C35 C36 H36A 110.8 . . ? C37 C36 H36B 110.8 . . ? C35 C36 H36B 110.8 . . ? H36A C36 H36B 108.8 . . ? C36 C37 C38 104.8(5) . . ? C36 C37 H37A 110.8 . . ? C38 C37 H37A 110.8 . . ? C36 C37 H37B 110.8 . . ? C38 C37 H37B 110.8 . . ? H37A C37 H37B 108.9 . . ? O1 C38 C37 105.7(5) . . ? O1 C38 H38A 110.6 . . ? C37 C38 H38A 110.6 . . ? O1 C38 H38B 110.6 . . ? C37 C38 H38B 110.6 . . ? H38A C38 H38B 108.7 . . ? O4 C39 C40 106.4(6) . . ? O4 C39 C40A 108.5(8) . . ? C40 C39 C40A 27.5(11) . . ? O4 C39 H39A 110.5 . . ? C40 C39 H39A 110.5 . . ? C40A C39 H39A 130.4 . . ? O4 C39 H39B 110.5 . . ? C40 C39 H39B 110.5 . . ? C40A C39 H39B 84.6 . . ? H39A C39 H39B 108.6 . . ? C39 C40 C41 104.7(7) . . ? C39 C40 H40A 110.8 . . ? C41 C40 H40A 110.8 . . ? C39 C40 H40B 110.8 . . ? C41 C40 H40B 110.8 . . ? H40A C40 H40B 108.9 . . ? C40A C41 C42 106.1(9) . . ? C40A C41 C40 27.3(11) . . ? C42 C41 C40 106.2(6) . . ? C40A C41 H41A 85.7 . . ? C42 C41 H41A 110.5 . . ? C40 C41 H41A 110.5 . . ? C40A C41 H41B 131.9 . . ? C42 C41 H41B 110.5 . . ? C40 C41 H41B 110.5 . . ? H41A C41 H41B 108.7 . . ? O4 C42 C41 107.0(4) . . ? O4 C42 H42A 110.3 . . ? C41 C42 H42A 110.3 . . ? O4 C42 H42B 110.3 . . ? C41 C42 H42B 110.3 . . ? H42A C42 H42B 108.6 . . ? O3 C43 C44 104.6(10) . . ? O3 C43 H43A 110.8 . . ? C44 C43 H43A 110.8 . . ? O3 C43 H43B 110.8 . . ? C44 C43 H43B 110.8 . . ? H43A C43 H43B 108.9 . . ? C45 C44 C43 101.8(14) . . ? C45 C44 H44A 111.4 . . ? C43 C44 H44A 111.4 . . ? C45 C44 H44B 111.4 . . ? C43 C44 H44B 111.4 . . ? H44A C44 H44B 109.3 . . ? C46 C45 C44 105.5(14) . . ? C46 C45 H45A 110.6 . . ? C44 C45 H45A 110.6 . . ? C46 C45 H45B 110.6 . . ? C44 C45 H45B 110.6 . . ? H45A C45 H45B 108.8 . . ? O3 C46 C45 105.5(12) . . ? O3 C46 H46A 110.6 . . ? C45 C46 H46A 110.6 . . ? O3 C46 H46B 110.6 . . ? C45 C46 H46B 110.6 . . ? H46A C46 H46B 108.8 . . ? C41 C40A C39 105.2(11) . . ? C41 C40A H40C 110.7 . . ? C39 C40A H40C 110.7 . . ? C41 C40A H40D 110.7 . . ? C39 C40A H40D 110.7 . . ? H40C C40A H40D 108.8 . . ? O3 C43A C44A 106.4(12) . . ? O3 C43A H43C 110.4 . . ? C44A C43A H43C 110.4 . . ? O3 C43A H43D 110.4 . . ? C44A C43A H43D 110.4 . . ? H43C C43A H43D 108.6 . . ? C45A C44A C43A 101.2(15) . . ? C45A C44A H44C 111.5 . . ? C43A C44A H44C 111.5 . . ? C45A C44A H44D 111.5 . . ? C43A C44A H44D 111.5 . . ? H44C C44A H44D 109.4 . . ? C44A C45A C46A 108.5(17) . . ? C44A C45A H45C 110.0 . . ? C46A C45A H45C 110.0 . . ? C44A C45A H45D 110.0 . . ? C46A C45A H45D 110.0 . . ? H45C C45A H45D 108.4 . . ? O3 C46A C45A 100.9(12) . . ? 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 Sr1 O1 C35 71.1(4) . . . . ? N2 Sr1 O1 C35 2.6(4) . . . . ? O4 Sr1 O1 C35 -150.3(4) . . . . ? O2 Sr1 O1 C35 -80.3(4) . . . . ? O3 Sr1 O1 C35 159.6(4) . . . . ? N1 Sr1 O1 C38 -128.4(4) . . . . ? N2 Sr1 O1 C38 163.1(4) . . . . ? O4 Sr1 O1 C38 10.2(5) . . . . ? O2 Sr1 O1 C38 80.2(5) . . . . ? O3 Sr1 O1 C38 -39.9(4) . . . . ? N1 Sr1 O2 C34 175.9(4) . . . . ? N2 Sr1 O2 C34 165.4(4) . . . . ? O4 Sr1 O2 C34 59.7(4) . . . . ? O1 Sr1 O2 C34 -86.2(4) . . . . ? O3 Sr1 O2 C34 -15.2(4) . . . . ? N1 Sr1 O2 C31 -16.4(5) . . . . ? N2 Sr1 O2 C31 -27.0(4) . . . . ? O4 Sr1 O2 C31 -132.6(4) . . . . ? O1 Sr1 O2 C31 81.5(4) . . . . ? O3 Sr1 O2 C31 152.5(4) . . . . ? N1 Sr1 O3 C46 142(2) . . . . ? N2 Sr1 O3 C46 146(2) . . . . ? O4 Sr1 O3 C46 -117(2) . . . . ? O1 Sr1 O3 C46 35(2) . . . . ? O2 Sr1 O3 C46 -33(2) . . . . ? N1 Sr1 O3 C46A 173.6(15) . . . . ? N2 Sr1 O3 C46A 177.3(15) . . . . ? O4 Sr1 O3 C46A -85.3(15) . . . . ? O1 Sr1 O3 C46A 66.6(15) . . . . ? O2 Sr1 O3 C46A -1.3(15) . . . . ? N1 Sr1 O3 C43 -34.8(7) . . . . ? N2 Sr1 O3 C43 -31.0(8) . . . . ? O4 Sr1 O3 C43 66.3(7) . . . . ? O1 Sr1 O3 C43 -141.8(7) . . . . ? O2 Sr1 O3 C43 150.3(7) . . . . ? N1 Sr1 O3 C43A -7.6(9) . . . . ? N2 Sr1 O3 C43A -3.9(10) . . . . ? O4 Sr1 O3 C43A 93.5(9) . . . . ? O1 Sr1 O3 C43A -114.6(9) . . . . ? O2 Sr1 O3 C43A 177.5(9) . . . . ? N1 Sr1 O4 C42 146.1(4) . . . . ? N2 Sr1 O4 C42 -146.9(4) . . . . ? O1 Sr1 O4 C42 6.2(5) . . . . ? O2 Sr1 O4 C42 -58.9(4) . . . . ? O3 Sr1 O4 C42 57.3(4) . . . . ? N1 Sr1 O4 C39 -18.2(4) . . . . ? N2 Sr1 O4 C39 48.7(4) . . . . ? O1 Sr1 O4 C39 -158.1(4) . . . . ? O2 Sr1 O4 C39 136.8(4) . . . . ? O3 Sr1 O4 C39 -107.0(4) . . . . ? N2 Si1 N1 C19 -167.9(3) . . . . ? C1 Si1 N1 C19 68.1(4) . . . . ? N2 Si1 N1 Sr1 -9.67(18) . . . . ? C1 Si1 N1 Sr1 -133.71(18) . . . . ? N2 Sr1 N1 C19 157.6(5) . . . . ? O4 Sr1 N1 C19 -100.3(5) . . . . ? O1 Sr1 N1 C19 56.0(5) . . . . ? O2 Sr1 N1 C19 145.9(4) . . . . ? O3 Sr1 N1 C19 -24.1(5) . . . . ? N2 Sr1 N1 Si1 7.01(13) . . . . ? O4 Sr1 N1 Si1 109.19(15) . . . . ? O1 Sr1 N1 Si1 -94.52(15) . . . . ? O2 Sr1 N1 Si1 -4.6(3) . . . . ? O3 Sr1 N1 Si1 -174.64(15) . . . . ? N1 Si1 N2 C7 -172.0(4) . . . . ? C1 Si1 N2 C7 -46.5(4) . . . . ? N1 Si1 N2 Sr1 9.65(17) . . . . ? C1 Si1 N2 Sr1 135.17(19) . . . . ? N1 Sr1 N2 C7 174.8(4) . . . . ? O4 Sr1 N2 C7 79.6(4) . . . . ? O1 Sr1 N2 C7 -84.1(4) . . . . ? O2 Sr1 N2 C7 -10.5(4) . . . . ? O3 Sr1 N2 C7 170.7(4) . . . . ? N1 Sr1 N2 Si1 -7.05(13) . . . . ? O4 Sr1 N2 Si1 -102.29(15) . . . . ? O1 Sr1 N2 Si1 94.08(15) . . . . ? O2 Sr1 N2 Si1 167.60(15) . . . . ? O3 Sr1 N2 Si1 -11.2(4) . . . . ? N2 Si1 C1 C2 124.6(4) . . . . ? N1 Si1 C1 C2 -116.1(4) . . . . ? N2 Si1 C1 C6 -56.8(4) . . . . ? N1 Si1 C1 C6 62.5(4) . . . . ? C6 C1 C2 C3 -1.7(7) . . . . ? Si1 C1 C2 C3 177.0(4) . . . . ? C1 C2 C3 C4 -0.2(8) . . . . ? C2 C3 C4 C5 1.8(8) . . . . ? C3 C4 C5 C6 -1.3(8) . . . . ? C4 C5 C6 C1 -0.7(8) . . . . ? C2 C1 C6 C5 2.1(7) . . . . ? Si1 C1 C6 C5 -176.5(4) . . . . ? Si1 N2 C7 C8 -67.2(5) . . . . ? Sr1 N2 C7 C8 110.4(5) . . . . ? Si1 N2 C7 C15 115.1(4) . . . . ? Sr1 N2 C7 C15 -67.3(5) . . . . ? N2 C7 C8 C12 -179.5(4) . . . . ? C15 C7 C8 C12 -1.7(6) . . . . ? N2 C7 C8 C9 0.0(6) . . . . ? C15 C7 C8 C9 177.8(4) . . . . ? C12 C8 C9 C11 -69.6(6) . . . . ? C7 C8 C9 C11 110.9(5) . . . . ? C12 C8 C9 C10 55.3(6) . . . . ? C7 C8 C9 C10 -124.2(5) . . . . ? C7 C8 C12 C13 1.5(7) . . . . ? C9 C8 C12 C13 -178.0(4) . . . . ? C8 C12 C13 C14 -0.4(7) . . . . ? C12 C13 C14 C15 -0.4(7) . . . . ? C13 C14 C15 C7 0.1(7) . . . . ? C13 C14 C15 C16 -179.6(4) . . . . ? N2 C7 C15 C14 178.7(4) . . . . ? C8 C7 C15 C14 0.9(6) . . . . ? N2 C7 C15 C16 -1.5(6) . . . . ? C8 C7 C15 C16 -179.4(4) . . . . ? C14 C15 C16 C18 -68.3(6) . . . . ? C7 C15 C16 C18 112.0(5) . . . . ? C14 C15 C16 C17 55.1(6) . . . . ? C7 C15 C16 C17 -124.6(5) . . . . ? Si1 N1 C19 C27 -101.9(5) . . . . ? Sr1 N1 C19 C27 112.6(5) . . . . ? Si1 N1 C19 C20 81.5(5) . . . . ? Sr1 N1 C19 C20 -64.0(7) . . . . ? C27 C19 C20 C24 2.0(7) . . . . ? N1 C19 C20 C24 178.7(5) . . . . ? C27 C19 C20 C21 -173.4(5) . . . . ? N1 C19 C20 C21 3.3(7) . . . . ? C24 C20 C21 C23 61.2(6) . . . . ? C19 C20 C21 C23 -123.3(5) . . . . ? C24 C20 C21 C22 -62.9(6) . . . . ? C19 C20 C21 C22 112.6(5) . . . . ? C19 C20 C24 C25 -1.1(8) . . . . ? C21 C20 C24 C25 174.5(5) . . . . ? C20 C24 C25 C26 -0.9(8) . . . . ? C24 C25 C26 C27 1.9(8) . . . . ? C25 C26 C27 C19 -0.9(8) . . . . ? C25 C26 C27 C28 178.5(5) . . . . ? N1 C19 C27 C26 -177.7(4) . . . . ? C20 C19 C27 C26 -1.0(7) . . . . ? N1 C19 C27 C28 2.9(7) . . . . ? C20 C19 C27 C28 179.6(4) . . . . ? C26 C27 C28 C30 62.5(6) . . . . ? C19 C27 C28 C30 -118.1(5) . . . . ? C26 C27 C28 C29 -59.8(6) . . . . ? C19 C27 C28 C29 119.6(5) . . . . ? C34 O2 C31 C32 -14.8(6) . . . . ? Sr1 O2 C31 C32 176.1(3) . . . . ? O2 C31 C32 C33 33.6(5) . . . . ? C31 C32 C33 C34 -38.8(6) . . . . ? C31 O2 C34 C33 -10.3(6) . . . . ? Sr1 O2 C34 C33 159.5(3) . . . . ? C32 C33 C34 O2 30.7(6) . . . . ? C38 O1 C35 C36 -19.9(6) . . . . ? Sr1 O1 C35 C36 144.6(4) . . . . ? O1 C35 C36 C37 0.2(7) . . . . ? C35 C36 C37 C38 18.7(7) . . . . ? C35 O1 C38 C37 32.0(6) . . . . ? Sr1 O1 C38 C37 -130.7(4) . . . . ? C36 C37 C38 O1 -31.4(7) . . . . ? C42 O4 C39 C40 -24.7(7) . . . . ? Sr1 O4 C39 C40 142.2(6) . . . . ? C42 O4 C39 C40A 4.1(14) . . . . ? Sr1 O4 C39 C40A 171.0(13) . . . . ? O4 C39 C40 C41 28.6(9) . . . . ? C40A C39 C40 C41 -70.1(17) . . . . ? C39 C40 C41 C40A 72.0(17) . . . . ? C39 C40 C41 C42 -21.9(10) . . . . ? C39 O4 C42 C41 10.6(6) . . . . ? Sr1 O4 C42 C41 -155.8(4) . . . . ? C40A C41 C42 O4 -21.2(14) . . . . ? C40 C41 C42 O4 7.2(8) . . . . ? C46 O3 C43 C44 -44.7(17) . . . . ? C46A O3 C43 C44 -66.8(15) . . . . ? C43A O3 C43 C44 18(2) . . . . ? Sr1 O3 C43 C44 133.5(11) . . . . ? O3 C43 C44 C45 31.0(18) . . . . ? C43 C44 C45 C46 -7(2) . . . . ? C46A O3 C46 C45 152(7) . . . . ? C43 O3 C46 C45 40(2) . . . . ? C43A O3 C46 C45 16.1(19) . . . . ? Sr1 O3 C46 C45 -136.9(14) . . . . ? C44 C45 C46 O3 -20(2) . . . . ? C42 C41 C40A C39 23(2) . . . . ? C40 C41 C40A C39 -70.9(15) . . . . ? O4 C39 C40A C41 -17(2) . . . . ? C40 C39 C40A C41 73.0(15) . . . . ? C46 O3 C43A C44A -20.5(18) . . . . ? C46A O3 C43A C44A -36.5(19) . . . . ? C43 O3 C43A C44A -140(4) . . . . ? Sr1 O3 C43A C44A 144.3(12) . . . . ? O3 C43A C44A C45A 15(2) . . . . ? C43A C44A C45A C46A 10(2) . . . . ? C46 O3 C46A C45A -5(4) . . . . ? C43 O3 C46A C45A 69.2(19) . . . . ? C43A O3 C46A C45A 41(2) . . . . ? Sr1 O3 C46A C45A -139.8(10) . . . . ? C44A C45A C46A O3 -32(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.779 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.068 #===end _database_code_depnum_ccdc_archive 'CCDC 945789'