data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_address ; Department of Chemistry University of Sussex Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Synthesis and structures of a 3-sila-beta-diketiminatomagnesium bromide, ketenimide and triflate ; _publ_requested_category FM loop_ _publ_author_name 'M. Lappert' 'James D. Farwell' 'P. B. Hitchcock' 'Andrey Protchenko' data_(1)-apr2501 _database_code_depnum_ccdc_archive 'CCDC 260822' _audit_creation_date 2004-12-07T11:38:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety ; 'C31 H53 Br Mg N2 O Si4, 0.5(C4 H8 O)' ; _chemical_formula_sum 'C33 H58 Br Mg N2 O1.5 Si4' _chemical_formula_weight 723.39 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnnm _symmetry_Int_Tables_number 58 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.7171(3) _cell_length_b 18.235 _cell_length_c 16.7049(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4178.51(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.15 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.637 _exptl_absorpt_correction_T_max 0.663 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 22453 _diffrn_reflns_av_R_equivalents 0.05 _diffrn_reflns_av_unetI/netI 0.0446 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 5127 _reflns_number_gt 3695 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; For the disordered thf group and the Et2O solvate disordered across an inversion centre the hydrogen atoms were omitted. 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^)+(0.0666P)^2^+9.8824P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5127 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1727 _refine_ls_wR_factor_gt 0.155 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.904 _refine_diff_density_min -1.334 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 Br Br 0.17275(5) 0.05481(3) 0 0.0520(2) Uani 1 2 d S . . Si1 Si 0.18496(10) 0.37217(6) 0 0.0298(3) Uani 1 2 d S . . Si2 Si 0.23588(13) 0.19190(6) 0.18464(7) 0.0629(4) Uani 1 1 d . . . Si4 Si 0.22533(12) 0.49691(7) 0 0.0409(4) Uani 1 2 d S . . Mg Mg 0.15693(12) 0.18970(8) 0 0.0287(3) Uani 1 2 d S . . O1 O 0.0099(3) 0.1970(2) 0 0.0552(10) Uani 1 2 d S . . N1 N 0.2076(2) 0.24620(15) 0.09936(16) 0.0351(6) Uani 1 1 d . . . C1 C 0.2120(2) 0.31836(17) 0.09178(18) 0.0289(7) Uani 1 1 d . . . C2 C 0.2372(3) 0.36538(17) 0.1630(2) 0.0367(8) Uani 1 1 d . . . C3 C 0.3346(3) 0.3845(2) 0.1771(2) 0.0473(10) Uani 1 1 d . . . C4 C 0.3550(4) 0.4278(2) 0.2445(3) 0.0649(14) Uani 1 1 d . . . H4 H 0.4206 0.4414 0.2551 0.078 Uiso 1 1 calc R . . C5 C 0.2843(6) 0.4509(2) 0.2949(3) 0.0768(18) Uani 1 1 d . . . H5 H 0.3005 0.4801 0.3401 0.092 Uiso 1 1 calc R . . C6 C 0.1898(5) 0.4323(2) 0.2806(3) 0.0718(16) Uani 1 1 d . . . H6 H 0.1406 0.4485 0.3166 0.086 Uiso 1 1 calc R . . C7 C 0.1631(3) 0.3897(2) 0.2142(2) 0.0517(11) Uani 1 1 d . . . C8 C 0.4154(3) 0.3567(3) 0.1252(3) 0.0626(12) Uani 1 1 d . . . H8A H 0.4309 0.306 0.1401 0.094 Uiso 1 1 calc R . . H8B H 0.4732 0.3875 0.1325 0.094 Uiso 1 1 calc R . . H8C H 0.395 0.3583 0.069 0.094 Uiso 1 1 calc R . . C9 C 0.0594(4) 0.3688(3) 0.2003(3) 0.0808(16) Uani 1 1 d . . . H9A H 0.0415 0.3799 0.1448 0.121 Uiso 1 1 calc R . . H9B H 0.0173 0.3965 0.2368 0.121 Uiso 1 1 calc R . . H9C H 0.0512 0.3162 0.2102 0.121 Uiso 1 1 calc R . . C10 C 0.3392(4) 0.1309(3) 0.1549(4) 0.0816(18) Uani 1 1 d . . . H10A H 0.3217 0.104 0.1062 0.122 Uiso 1 1 calc R . . H10B H 0.3526 0.096 0.1981 0.122 Uiso 1 1 calc R . . H10C H 0.3974 0.1607 0.1449 0.122 Uiso 1 1 calc R . . C11 C 0.1230(5) 0.1381(2) 0.2054(3) 0.0800(18) Uani 1 1 d . . . H11A H 0.0699 0.1717 0.2195 0.12 Uiso 1 1 calc R . . H11B H 0.1348 0.1044 0.2501 0.12 Uiso 1 1 calc R . . H11C H 0.1049 0.11 0.1577 0.12 Uiso 1 1 calc R . . C12 C 0.2731(9) 0.2380(3) 0.2796(3) 0.165(5) Uani 1 1 d . . . H12A H 0.3264 0.2723 0.2687 0.247 Uiso 1 1 calc R . . H12B H 0.2951 0.201 0.3182 0.247 Uiso 1 1 calc R . . H12C H 0.2175 0.2648 0.3018 0.247 Uiso 1 1 calc R . . C13 C 0.3578(7) 0.5214(4) 0 0.124(5) Uani 1 2 d S . . C14 C 0.1681(6) 0.5408(2) 0.0900(3) 0.094(2) Uani 1 1 d . . . C16 C -0.1548(5) 0.1596(4) 0 0.098(3) Uani 1 2 d S . . C17 C -0.1499(5) 0.2415(4) 0 0.073(2) Uani 1 2 d S . . C15 C -0.0573(14) 0.1458(11) 0.0491(15) 0.072(7) Uiso 0.295(18) 1 d P . . C18 C -0.0481(6) 0.2547(5) -0.0331(7) 0.071(3) Uani 0.5 1 d P . . C15A C -0.0571(12) 0.1263(9) 0 0.054(7) Uiso 0.41(4) 2 d SP . 1 C19 C 0.5355(16) 0.0259(14) 0 0.220(14) Uani 1 2 d S . 3 O2 O 0.5184(14) 0.0861(16) 0 0.159(8) Uani 0.5 2 d SP A 3 C20 C 0.5801(15) 0.144(3) 0 0.21(2) Uani 0.5 2 d SP A 3 C21 C 0.568(3) 0.220(2) 0 0.24(2) Uani 0.5 2 d SP A 3 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 Br 0.0984(5) 0.0239(2) 0.0337(3) 0 0 0.0029(3) Si1 0.0434(7) 0.0206(5) 0.0253(6) 0 0 0.0004(5) Si2 0.1312(13) 0.0290(5) 0.0284(5) 0.0052(4) -0.0207(7) -0.0105(6) Si4 0.0614(9) 0.0205(6) 0.0409(7) 0 0 -0.0004(6) Mg 0.0395(9) 0.0209(7) 0.0256(7) 0 0 -0.0024(6) O1 0.044(2) 0.053(2) 0.069(3) 0 0 -0.0023(18) N1 0.0570(18) 0.0246(13) 0.0238(13) 0.0026(11) -0.0034(13) -0.0044(12) C1 0.0354(17) 0.0270(15) 0.0243(15) -0.0012(12) 0.0018(14) -0.0006(12) C2 0.062(2) 0.0241(15) 0.0242(15) -0.0011(12) -0.0043(16) -0.0007(15) C3 0.071(3) 0.0336(18) 0.037(2) -0.0009(15) -0.021(2) -0.0016(17) C4 0.100(4) 0.042(2) 0.053(3) -0.003(2) -0.032(3) -0.012(2) C5 0.153(6) 0.039(2) 0.038(2) -0.0086(19) -0.024(3) -0.004(3) C6 0.136(5) 0.043(2) 0.036(2) -0.0091(19) 0.021(3) 0.008(3) C7 0.081(3) 0.040(2) 0.035(2) -0.0051(16) 0.013(2) 0.0004(19) C8 0.047(2) 0.074(3) 0.067(3) -0.006(3) -0.020(2) -0.001(2) C9 0.079(4) 0.097(4) 0.066(3) -0.009(3) 0.038(3) 0.004(3) C10 0.081(3) 0.052(3) 0.112(5) 0.029(3) -0.051(3) -0.003(2) C11 0.135(5) 0.041(2) 0.064(3) 0.015(2) 0.053(3) 0.009(3) C12 0.405(15) 0.042(3) 0.047(3) 0.009(2) -0.091(6) -0.025(5) C13 0.072(5) 0.051(4) 0.248(14) 0 0 -0.035(4) C14 0.189(7) 0.029(2) 0.062(3) -0.012(2) 0.032(4) 0.015(3) C16 0.043(4) 0.058(4) 0.192(11) 0 0 0.000(3) C17 0.058(4) 0.067(5) 0.095(6) 0 0 0.002(3) C18 0.040(4) 0.059(5) 0.115(10) 0.030(5) -0.002(5) 0.002(4) C19 0.16(2) 0.22(3) 0.29(2) 0 0 0.11(2) O2 0.085(12) 0.22(2) 0.175(18) 0 0 0.065(15) C20 0.027(10) 0.34(6) 0.26(4) 0 0 0.00(2) C21 0.16(3) 0.19(3) 0.36(6) 0 0 0.14(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Br Mg 2.4692(15) . ? Si1 C1 1.858(3) 6 ? Si1 C1 1.858(3) . ? Si1 Si4 2.3412(18) . ? Si2 N1 1.778(3) . ? Si2 C11 1.866(6) . ? Si2 C12 1.867(5) . ? Si2 C10 1.868(6) . ? Si4 C13 1.870(8) . ? Si4 C14 1.876(5) 6 ? Si4 C14 1.876(5) . ? Mg O1 2.021(4) . ? Mg N1 2.074(3) . ? Mg N1 2.074(3) 6 ? O1 C18 1.431(9) . ? O1 C18 1.431(9) 6 ? O1 C15 1.55(2) 6 ? O1 C15 1.55(2) . ? O1 C15A 1.584(17) . ? N1 C1 1.323(4) . ? C1 C2 1.507(4) . ? C2 C7 1.400(5) . ? C2 C3 1.401(6) . ? C3 C4 1.404(6) . ? C3 C8 1.496(6) . ? C4 C5 1.351(8) . ? C5 C6 1.361(8) . ? C6 C7 1.402(6) . ? C7 C9 1.492(7) . ? C16 C15A 1.472(18) . ? C16 C17 1.495(11) . ? C16 C15 1.59(2) . ? C17 C18 1.521(11) . ? C19 O2 1.12(3) . ? C19 C19 1.36(4) 5_655 ? O2 C20 1.35(5) . ? C20 C21 1.39(6) . ? 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 C1 Si1 C1 111.2(2) 6 . ? C1 Si1 Si4 117.78(10) 6 . ? C1 Si1 Si4 117.78(10) . . ? N1 Si2 C11 105.1(2) . . ? N1 Si2 C12 119.35(19) . . ? C11 Si2 C12 107.8(4) . . ? N1 Si2 C10 106.5(2) . . ? C11 Si2 C10 111.5(2) . . ? C12 Si2 C10 106.6(4) . . ? C13 Si4 C14 107.7(3) . 6 ? C13 Si4 C14 107.7(3) . . ? C14 Si4 C14 106.6(4) 6 . ? C13 Si4 Si1 117.5(3) . . ? C14 Si4 Si1 108.42(17) 6 . ? C14 Si4 Si1 108.42(17) . . ? O1 Mg N1 107.57(12) . . ? O1 Mg N1 107.57(12) . 6 ? N1 Mg N1 106.33(16) . 6 ? O1 Mg Br 98.82(13) . . ? N1 Mg Br 117.74(9) . . ? N1 Mg Br 117.74(9) 6 . ? C18 O1 C15 108.5(8) 6 6 ? C18 O1 C15 108.5(8) . . ? C18 O1 C15A 106.0(7) . . ? C18 O1 Mg 127.2(4) . . ? C18 O1 Mg 127.2(4) 6 . ? C15 O1 Mg 123.7(7) 6 . ? C15 O1 Mg 123.7(7) . . ? C15A O1 Mg 121.7(7) . . ? C1 N1 Si2 128.4(2) . . ? C1 N1 Mg 115.6(2) . . ? Si2 N1 Mg 115.96(14) . . ? N1 C1 C2 120.0(3) . . ? N1 C1 Si1 126.5(2) . . ? C2 C1 Si1 113.4(2) . . ? C7 C2 C3 120.7(3) . . ? C7 C2 C1 119.8(3) . . ? C3 C2 C1 119.5(3) . . ? C2 C3 C4 117.7(4) . . ? C2 C3 C8 121.7(3) . . ? C4 C3 C8 120.5(4) . . ? C5 C4 C3 122.1(5) . . ? C4 C5 C6 119.8(4) . . ? C5 C6 C7 121.6(5) . . ? C2 C7 C6 118.0(5) . . ? C2 C7 C9 121.0(4) . . ? C6 C7 C9 120.9(4) . . ? C15A C16 C17 111.8(9) . . ? C17 C16 C15 96.9(8) . . ? C16 C17 C18 101.5(6) . . ? O1 C15 C16 97.6(12) . . ? O1 C18 C17 104.7(6) . . ? C16 C15A O1 101.1(11) . . ? O2 C19 C19 122(3) . 5_655 ? C19 O2 C20 129(3) . . ? O2 C20 C21 134(3) . . ? #===END data_(2)-oct2399 _database_code_depnum_ccdc_archive 'CCDC 260823' _audit_creation_date 1999-10-22T13:52:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ;'(Mg(Me3SiNC(R)Si(SiMe3)C(R)NSiMe3)(NCR)2(NC(C6H4Me2))) R=C6H3Me2 ' ; _chemical_formula_moiety 'C54 H73 Mg N5 Si4' _chemical_formula_structural 'C54 H73 Mg N5 Si4' _chemical_formula_sum 'C54 H73 Mg N5 Si4' _chemical_formula_weight 928.84 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5706(3) _cell_length_b 34.3614(8) _cell_length_c 12.8282(4) _cell_angle_alpha 90 _cell_angle_beta 94.7770(10) _cell_angle_gamma 90 _cell_volume 5521.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29431 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.157 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 21222 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.28 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 9596 _reflns_number_gt 6636 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The two hydrogen atoms bonded to C32 were freely refined. The Si2 atom is disordered equally between two sites perpendicular to the N1,N2,Si4 plane. 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^)+(0.0492P)^2^+4.3750P] 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_number_reflns 9596 _refine_ls_number_parameters 616 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.426 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' 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 Mg Mg 0.76391(7) 0.08715(2) 0.26604(7) 0.0282(2) Uani 1 1 d . . . Si1 Si 0.75544(7) 0.07104(2) 0.51696(6) 0.0324(2) Uani 1 1 d . . . Si2 Si 0.7982(3) 0.18255(17) 0.3291(5) 0.0360(9) Uani 0.5 1 d P A . Si2A Si 0.7525(3) 0.18214(17) 0.3266(5) 0.0549(13) Uani 0.5 1 d P A . Si3 Si 0.77124(8) 0.11746(3) 0.02045(7) 0.0445(2) Uani 1 1 d . . . Si4 Si 0.76930(8) 0.24898(2) 0.36386(7) 0.0428(2) Uani 1 1 d . . . N1 N 0.76682(17) 0.10756(6) 0.42061(16) 0.0267(5) Uani 1 1 d . A . N2 N 0.77374(18) 0.13078(6) 0.15397(17) 0.0319(6) Uani 1 1 d . A . N3 N 0.7462(2) 0.02864(7) 0.2524(2) 0.0402(6) Uani 1 1 d . . . N4 N 0.5862(2) 0.09344(7) 0.2354(2) 0.0412(6) Uani 1 1 d . . . N5 N 0.9401(2) 0.07937(7) 0.2697(2) 0.0431(6) Uani 1 1 d . . . C1 C 0.7663(2) 0.14588(8) 0.4317(2) 0.0300(6) Uani 1 1 d . . . C2 C 0.7762(2) 0.16679(8) 0.1919(2) 0.0333(7) Uani 1 1 d . . . C3 C 0.7579(3) 0.16393(8) 0.5383(2) 0.0347(7) Uani 1 1 d . A . C4 C 0.6570(3) 0.17120(9) 0.5721(3) 0.0499(9) Uani 1 1 d . . . C5 C 0.6513(4) 0.18818(11) 0.6712(3) 0.0727(12) Uani 1 1 d . A . H5 H 0.5836 0.1935 0.6959 0.087 Uiso 1 1 calc R . . C6 C 0.7418(5) 0.19711(12) 0.7321(3) 0.0809(15) Uani 1 1 d . . . H6 H 0.7364 0.2088 0.7986 0.097 Uiso 1 1 calc R A . C7 C 0.8400(4) 0.18961(11) 0.6994(3) 0.0678(12) Uani 1 1 d . A . H7 H 0.9019 0.1958 0.7439 0.081 Uiso 1 1 calc R . . C8 C 0.8515(3) 0.17293(9) 0.6011(2) 0.0466(8) Uani 1 1 d . . . C9 C 0.5568(3) 0.16130(12) 0.5053(4) 0.0746(12) Uani 1 1 d . A . H9A H 0.4945 0.1686 0.5421 0.112 Uiso 0.5 1 calc PR . . H9B H 0.555 0.1333 0.4911 0.112 Uiso 0.5 1 calc PR . . H9C H 0.5555 0.1756 0.4391 0.112 Uiso 0.5 1 calc PR . . H9D H 0.5755 0.1497 0.4395 0.112 Uiso 0.5 1 calc PR . . H9E H 0.515 0.185 0.4904 0.112 Uiso 0.5 1 calc PR . . H9F H 0.5145 0.1427 0.5425 0.112 Uiso 0.5 1 calc PR . . C10 C 0.9600(3) 0.16432(11) 0.5663(3) 0.0672(11) Uani 1 1 d . A . H10A H 0.9526 0.1528 0.4962 0.101 Uiso 0.5 1 calc PR . . H10B H 0.9973 0.146 0.6153 0.101 Uiso 0.5 1 calc PR . . H10C H 1.0011 0.1885 0.5646 0.101 Uiso 0.5 1 calc PR . . H10D H 1.0147 0.1721 0.6212 0.101 Uiso 0.5 1 calc PR . . H10E H 0.9701 0.1789 0.5021 0.101 Uiso 0.5 1 calc PR . . H10F H 0.9662 0.1364 0.5528 0.101 Uiso 0.5 1 calc PR . . C11 C 0.7785(3) 0.20121(8) 0.1187(2) 0.0381(7) Uani 1 1 d . A . C12 C 0.8762(3) 0.21617(10) 0.0932(3) 0.0549(9) Uani 1 1 d . . . C13 C 0.8752(4) 0.24765(12) 0.0237(4) 0.0817(14) Uani 1 1 d . A . H13 H 0.9409 0.2577 0.0035 0.098 Uiso 1 1 calc R . . C14 C 0.7820(5) 0.26409(13) -0.0153(3) 0.0881(16) Uani 1 1 d . . . H14 H 0.7834 0.2856 -0.0615 0.106 Uiso 1 1 calc R A . C15 C 0.6859(4) 0.24997(11) 0.0113(3) 0.0746(13) Uani 1 1 d . A . H15 H 0.6215 0.262 -0.016 0.089 Uiso 1 1 calc R . . C16 C 0.6819(3) 0.21812(9) 0.0780(3) 0.0502(9) Uani 1 1 d . . . C17 C 0.9810(3) 0.19987(13) 0.1383(4) 0.0857(14) Uani 1 1 d . A . H17A H 1.0397 0.2144 0.1108 0.129 Uiso 0.5 1 calc PR . . H17B H 0.9859 0.1724 0.119 0.129 Uiso 0.5 1 calc PR . . H17C H 0.9858 0.2022 0.2147 0.129 Uiso 0.5 1 calc PR . . H17D H 0.9679 0.1783 0.1855 0.129 Uiso 0.5 1 calc PR . . H17E H 1.0217 0.2203 0.1773 0.129 Uiso 0.5 1 calc PR . . H17F H 1.0218 0.1904 0.0816 0.129 Uiso 0.5 1 calc PR . . C18 C 0.5752(3) 0.20341(12) 0.1067(3) 0.0689(11) Uani 1 1 d . A . H18A H 0.586 0.181 0.1539 0.103 Uiso 0.5 1 calc PR . . H18B H 0.532 0.1955 0.0432 0.103 Uiso 0.5 1 calc PR . . H18C H 0.5383 0.2241 0.1419 0.103 Uiso 0.5 1 calc PR . . H18D H 0.5182 0.2194 0.0721 0.103 Uiso 0.5 1 calc PR . . H18E H 0.5723 0.205 0.1827 0.103 Uiso 0.5 1 calc PR . . H18F H 0.5659 0.1763 0.0841 0.103 Uiso 0.5 1 calc PR . . C19 C 0.8671(3) 0.03611(9) 0.5048(3) 0.0454(8) Uani 1 1 d . . . H19C H 0.8641 0.0262 0.433 0.068 Uiso 1 1 calc R . . H19B H 0.8606 0.0144 0.5534 0.068 Uiso 1 1 calc R . . H19A H 0.9354 0.0494 0.5215 0.068 Uiso 1 1 calc R . . C20 C 0.6241(2) 0.04700(9) 0.4820(2) 0.0438(8) Uani 1 1 d . . . H20C H 0.5663 0.0654 0.4917 0.066 Uiso 1 1 calc R . . H20B H 0.6169 0.0243 0.5272 0.066 Uiso 1 1 calc R . . H20A H 0.6202 0.0386 0.4088 0.066 Uiso 1 1 calc R . . C21 C 0.7607(3) 0.08516(9) 0.6579(2) 0.0486(9) Uani 1 1 d . . . H21C H 0.828 0.0987 0.6777 0.073 Uiso 1 1 calc R . . H21B H 0.7561 0.0618 0.701 0.073 Uiso 1 1 calc R . . H21A H 0.7007 0.1025 0.6691 0.073 Uiso 1 1 calc R . . C22 C 0.7700(4) 0.06328(10) 0.0173(3) 0.0691(12) Uani 1 1 d . . . H22C H 0.8362 0.0533 0.0537 0.104 Uiso 1 1 calc R . . H22B H 0.7646 0.0543 -0.0555 0.104 Uiso 1 1 calc R . . H22A H 0.7087 0.0536 0.0522 0.104 Uiso 1 1 calc R . . C23 C 0.6487(3) 0.13373(11) -0.0608(3) 0.0592(10) Uani 1 1 d . . . H23C H 0.5851 0.1262 -0.0262 0.089 Uiso 1 1 calc R . . H23B H 0.6465 0.1214 -0.1298 0.089 Uiso 1 1 calc R . . H23A H 0.6502 0.1621 -0.0689 0.089 Uiso 1 1 calc R . . C24 C 0.8910(3) 0.13270(13) -0.0447(3) 0.0697(11) Uani 1 1 d . . . H24C H 0.8908 0.1611 -0.0527 0.105 Uiso 1 1 calc R . . H24B H 0.8897 0.1204 -0.1138 0.105 Uiso 1 1 calc R . . H24A H 0.9555 0.1246 -0.0021 0.105 Uiso 1 1 calc R . . C28 C 0.7453(2) -0.00540(9) 0.2572(2) 0.0351(7) Uani 1 1 d . . . C29 C 0.7478(3) -0.04536(8) 0.2638(2) 0.0414(8) Uani 1 1 d . . . C30 C 0.8478(3) -0.06602(9) 0.2529(2) 0.0490(9) Uani 1 1 d . . . C31 C 0.8528(4) -0.10480(11) 0.2558(3) 0.0651(11) Uani 1 1 d . . . H31 H 0.9194 -0.1169 0.2472 0.078 Uiso 1 1 calc R . . C32 C 0.7604(5) -0.12980(13) 0.2717(4) 0.0841(15) Uani 1 1 d . . . H32B H 0.747(3) -0.1464(14) 0.209(4) 0.103(16) Uiso 1 1 d . . . H32A H 0.778(4) -0.1480(15) 0.332(4) 0.119(18) Uiso 1 1 d . . . C33 C 0.6591(4) -0.10757(12) 0.2822(3) 0.0772(13) Uani 1 1 d . . . H33 H 0.596 -0.1218 0.2925 0.093 Uiso 1 1 calc R . . C34 C 0.6534(3) -0.06752(10) 0.2777(3) 0.0569(10) Uani 1 1 d . . . C35 C 0.9437(3) -0.04269(12) 0.2316(3) 0.0650(11) Uani 1 1 d . . . H35A H 0.9259 -0.0149 0.2322 0.098 Uiso 0.5 1 calc PR . . H35B H 0.9666 -0.0498 0.163 0.098 Uiso 0.5 1 calc PR . . H35C H 1.0015 -0.048 0.2857 0.098 Uiso 0.5 1 calc PR . . H35D H 1.0035 -0.0602 0.2217 0.098 Uiso 0.5 1 calc PR . . H35E H 0.9627 -0.0254 0.291 0.098 Uiso 0.5 1 calc PR . . H35F H 0.9278 -0.0271 0.1682 0.098 Uiso 0.5 1 calc PR . . C36 C 0.5509(3) -0.04594(13) 0.2865(3) 0.0796(14) Uani 1 1 d . . . H36A H 0.5637 -0.0179 0.2809 0.119 Uiso 0.5 1 calc PR . . H36B H 0.5237 -0.0517 0.3543 0.119 Uiso 0.5 1 calc PR . . H36C H 0.4983 -0.0541 0.2301 0.119 Uiso 0.5 1 calc PR . . H36D H 0.4935 -0.0646 0.296 0.119 Uiso 0.5 1 calc PR . . H36E H 0.5335 -0.0308 0.2226 0.119 Uiso 0.5 1 calc PR . . H36F H 0.5589 -0.0283 0.3468 0.119 Uiso 0.5 1 calc PR . . C37 C 0.5040(3) 0.09917(8) 0.1934(2) 0.0365(7) Uani 1 1 d . . . C38 C 0.4025(2) 0.10668(9) 0.1369(2) 0.0362(7) Uani 1 1 d . . . C39 C 0.3757(3) 0.08493(10) 0.0458(2) 0.0473(8) Uani 1 1 d . . . C40 C 0.2811(3) 0.09319(13) -0.0099(3) 0.0665(11) Uani 1 1 d . . . H40 H 0.2612 0.0792 -0.0724 0.08 Uiso 1 1 calc R . . C41 C 0.2147(3) 0.12127(15) 0.0227(4) 0.0747(13) Uani 1 1 d . . . H41 H 0.1494 0.1265 -0.0176 0.09 Uiso 1 1 calc R . . C42 C 0.2404(3) 0.14213(12) 0.1129(3) 0.0640(11) Uani 1 1 d . . . H42 H 0.1924 0.1613 0.1346 0.077 Uiso 1 1 calc R . . C43 C 0.3359(3) 0.13536(10) 0.1723(3) 0.0476(8) Uani 1 1 d . . . C44 C 0.4461(3) 0.05302(12) 0.0112(3) 0.0691(11) Uani 1 1 d . . . H44A H 0.5102 0.0511 0.06 0.104 Uiso 0.5 1 calc PR . . H44B H 0.4669 0.0588 -0.0591 0.104 Uiso 0.5 1 calc PR . . H44C H 0.4073 0.0283 0.0101 0.104 Uiso 0.5 1 calc PR . . H44D H 0.4127 0.041 -0.0527 0.104 Uiso 0.5 1 calc PR . . H44E H 0.456 0.0333 0.0664 0.104 Uiso 0.5 1 calc PR . . H44F H 0.5156 0.0639 -0.0028 0.104 Uiso 0.5 1 calc PR . . C45 C 0.3664(3) 0.15793(12) 0.2704(3) 0.0727(12) Uani 1 1 d . . . H45A H 0.4362 0.149 0.3011 0.109 Uiso 0.5 1 calc PR . . H45B H 0.3127 0.1539 0.3204 0.109 Uiso 0.5 1 calc PR . . H45C H 0.3704 0.1857 0.2536 0.109 Uiso 0.5 1 calc PR . . H45D H 0.31 0.1767 0.2823 0.109 Uiso 0.5 1 calc PR . . H45E H 0.4335 0.1718 0.263 0.109 Uiso 0.5 1 calc PR . . H45F H 0.3758 0.14 0.3298 0.109 Uiso 0.5 1 calc PR . . C46 C 1.0287(3) 0.07143(9) 0.2772(2) 0.0399(7) Uani 1 1 d . . . C47 C 1.1392(2) 0.05977(9) 0.2884(3) 0.0440(8) Uani 1 1 d . . . C48 C 1.1784(3) 0.03699(10) 0.2084(3) 0.0558(10) Uani 1 1 d . . . C49 C 1.2827(3) 0.02454(11) 0.2250(4) 0.0750(13) Uani 1 1 d . . . H49 H 1.3117 0.0088 0.1734 0.09 Uiso 1 1 calc R . . C50 C 1.3450(4) 0.03401(14) 0.3126(5) 0.0825(15) Uani 1 1 d . . . H50 H 1.4164 0.0247 0.3212 0.099 Uiso 1 1 calc R . . C51 C 1.3074(3) 0.05674(14) 0.3890(4) 0.0765(14) Uani 1 1 d . . . H51 H 1.3529 0.0635 0.4491 0.092 Uiso 1 1 calc R . . C52 C 1.2011(3) 0.07014(11) 0.3784(3) 0.0575(10) Uani 1 1 d . . . C53 C 1.1112(3) 0.02768(13) 0.1098(4) 0.0830(14) Uani 1 1 d . . . H53A H 1.0399 0.039 0.1131 0.125 Uiso 0.5 1 calc PR . . H53B H 1.105 -0.0006 0.1019 0.125 Uiso 0.5 1 calc PR . . H53C H 1.1445 0.0386 0.0499 0.125 Uiso 0.5 1 calc PR . . H53D H 1.153 0.0123 0.0635 0.125 Uiso 0.5 1 calc PR . . H53E H 1.0879 0.0519 0.0747 0.125 Uiso 0.5 1 calc PR . . H53F H 1.0485 0.0127 0.1267 0.125 Uiso 0.5 1 calc PR . . C54 C 1.1571(4) 0.09473(16) 0.4611(3) 0.0960(16) Uani 1 1 d . . . H54A H 1.2125 0.099 0.5183 0.144 Uiso 0.5 1 calc PR . . H54B H 1.096 0.0815 0.4879 0.144 Uiso 0.5 1 calc PR . . H54C H 1.134 0.1199 0.431 0.144 Uiso 0.5 1 calc PR . . H54D H 1.0825 0.1012 0.4398 0.144 Uiso 0.5 1 calc PR . . H54E H 1.199 0.1187 0.4702 0.144 Uiso 0.5 1 calc PR . . H54F H 1.161 0.0803 0.5272 0.144 Uiso 0.5 1 calc PR . . C25 C 0.7895(5) 0.25974(11) 0.5074(3) 0.0765(18) Uani 0.902(7) 1 d P A 1 H25C H 0.7934 0.288 0.5181 0.115 Uiso 0.902(7) 1 calc PR A 1 H25B H 0.8562 0.2477 0.5366 0.115 Uiso 0.902(7) 1 calc PR A 1 H25A H 0.7296 0.2492 0.5427 0.115 Uiso 0.902(7) 1 calc PR A 1 C26 C 0.6405(3) 0.27137(12) 0.3184(5) 0.0666(15) Uani 0.902(7) 1 d P A 1 H26C H 0.6383 0.2982 0.3443 0.1 Uiso 0.902(7) 1 calc PR A 1 H26B H 0.5822 0.2564 0.3449 0.1 Uiso 0.902(7) 1 calc PR A 1 H26A H 0.6325 0.2715 0.2418 0.1 Uiso 0.902(7) 1 calc PR A 1 C27 C 0.8802(4) 0.27602(12) 0.3058(5) 0.0685(15) Uani 0.902(7) 1 d P A 1 H27C H 0.8651 0.2776 0.2297 0.103 Uiso 0.902(7) 1 calc PR A 1 H27B H 0.9477 0.2622 0.3223 0.103 Uiso 0.902(7) 1 calc PR A 1 H27A H 0.8855 0.3023 0.3352 0.103 Uiso 0.902(7) 1 calc PR A 1 C25A C 0.682(4) 0.2584(12) 0.478(3) 0.067(13) Uiso 0.098(7) 1 d P A 2 H25D H 0.6081 0.2504 0.4573 0.101 Uiso 0.098(7) 1 calc PR A 2 H25E H 0.6833 0.2861 0.4954 0.101 Uiso 0.098(7) 1 calc PR A 2 H25F H 0.7094 0.2433 0.5392 0.101 Uiso 0.098(7) 1 calc PR A 2 C26A C 0.671(3) 0.2776(10) 0.253(3) 0.041(9) Uiso 0.098(7) 1 d P A 2 H26D H 0.6037 0.2636 0.241 0.061 Uiso 0.098(7) 1 calc PR A 2 H26E H 0.7061 0.279 0.1872 0.061 Uiso 0.098(7) 1 calc PR A 2 H26F H 0.6578 0.3041 0.2772 0.061 Uiso 0.098(7) 1 calc PR A 2 C27A C 0.891(4) 0.2629(17) 0.381(5) 0.092(17) Uiso 0.098(7) 1 d P A 2 H27D H 0.9269 0.2572 0.3178 0.139 Uiso 0.098(7) 1 calc PR A 2 H27E H 0.9264 0.2492 0.4407 0.139 Uiso 0.098(7) 1 calc PR A 2 H27F H 0.8928 0.291 0.3939 0.139 Uiso 0.098(7) 1 calc PR A 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 Mg 0.0336(5) 0.0252(5) 0.0253(5) -0.0005(4) -0.0003(4) 0.0036(4) Si1 0.0410(5) 0.0291(4) 0.0269(4) 0.0044(3) 0.0008(3) -0.0003(4) Si2 0.059(2) 0.0214(11) 0.0281(12) 0.0006(8) 0.0032(18) -0.0007(17) Si2A 0.108(4) 0.0262(14) 0.0319(15) 0.0044(10) 0.016(3) 0.011(3) Si3 0.0606(6) 0.0450(5) 0.0286(4) -0.0015(4) 0.0078(4) 0.0045(4) Si4 0.0612(6) 0.0246(4) 0.0428(5) 0.0009(4) 0.0048(4) 0.0031(4) N1 0.0291(13) 0.0242(12) 0.0261(12) 0.0018(10) -0.0014(10) 0.0002(9) N2 0.0379(14) 0.0310(13) 0.0269(12) 0.0007(11) 0.0036(10) 0.0029(10) N3 0.0424(16) 0.0306(15) 0.0476(16) -0.0055(12) 0.0037(12) 0.0014(11) N4 0.0362(16) 0.0486(16) 0.0382(14) 0.0041(13) 0.0002(12) 0.0013(12) N5 0.0364(16) 0.0462(16) 0.0467(16) 0.0018(13) 0.0037(12) 0.0054(13) C1 0.0321(16) 0.0303(16) 0.0272(15) 0.0008(13) 0.0010(12) 0.0027(12) C2 0.0402(18) 0.0299(16) 0.0300(16) 0.0051(13) 0.0048(13) 0.0022(13) C3 0.053(2) 0.0247(15) 0.0264(15) 0.0027(12) 0.0032(14) 0.0053(13) C4 0.068(3) 0.0375(18) 0.046(2) -0.0023(16) 0.0140(18) 0.0131(17) C5 0.110(4) 0.053(2) 0.060(3) -0.007(2) 0.039(3) 0.013(2) C6 0.156(5) 0.051(2) 0.039(2) -0.0132(19) 0.025(3) -0.006(3) C7 0.115(4) 0.048(2) 0.037(2) -0.0047(18) -0.011(2) -0.017(2) C8 0.068(2) 0.0334(17) 0.0360(18) 0.0006(15) -0.0084(17) -0.0062(16) C9 0.053(3) 0.072(3) 0.099(3) -0.008(2) 0.011(2) 0.021(2) C10 0.055(3) 0.067(3) 0.076(3) 0.003(2) -0.015(2) -0.015(2) C11 0.051(2) 0.0333(16) 0.0311(16) 0.0020(14) 0.0112(14) 0.0024(15) C12 0.064(2) 0.041(2) 0.063(2) 0.0006(18) 0.0283(19) -0.0028(17) C13 0.117(4) 0.049(2) 0.087(3) 0.008(2) 0.058(3) -0.014(3) C14 0.163(5) 0.048(2) 0.058(3) 0.022(2) 0.034(3) 0.003(3) C15 0.119(4) 0.050(2) 0.052(2) 0.014(2) -0.007(2) 0.016(2) C16 0.066(2) 0.0430(19) 0.0409(19) 0.0078(16) -0.0012(17) 0.0102(17) C17 0.049(3) 0.069(3) 0.141(4) -0.009(3) 0.017(3) -0.008(2) C18 0.050(2) 0.070(3) 0.085(3) 0.003(2) -0.005(2) 0.013(2) C19 0.053(2) 0.0388(18) 0.0432(18) 0.0115(15) -0.0041(16) 0.0078(15) C20 0.048(2) 0.0413(18) 0.0426(18) 0.0047(15) 0.0078(15) -0.0082(15) C21 0.075(2) 0.0415(18) 0.0286(17) 0.0080(14) 0.0001(16) -0.0054(17) C22 0.114(4) 0.053(2) 0.040(2) -0.0120(18) 0.004(2) 0.011(2) C23 0.071(3) 0.069(2) 0.0363(19) 0.0001(18) -0.0010(17) -0.007(2) C24 0.071(3) 0.095(3) 0.046(2) -0.005(2) 0.0246(19) 0.008(2) C28 0.0384(18) 0.0349(19) 0.0318(16) -0.0064(14) 0.0012(13) -0.0013(13) C29 0.058(2) 0.0279(16) 0.0385(18) -0.0041(14) 0.0029(15) -0.0062(15) C30 0.072(3) 0.0373(19) 0.0357(18) -0.0018(15) -0.0054(17) 0.0154(17) C31 0.098(3) 0.043(2) 0.052(2) -0.0034(18) -0.009(2) 0.014(2) C32 0.141(5) 0.042(2) 0.069(3) -0.001(2) 0.009(3) 0.010(3) C33 0.116(4) 0.058(3) 0.060(3) -0.009(2) 0.024(2) -0.040(3) C34 0.083(3) 0.048(2) 0.043(2) -0.0125(17) 0.0200(19) -0.0156(19) C35 0.051(2) 0.076(3) 0.066(2) -0.007(2) -0.0090(19) 0.014(2) C36 0.072(3) 0.092(3) 0.079(3) -0.038(2) 0.036(2) -0.039(2) C37 0.0392(19) 0.0367(17) 0.0338(16) 0.0000(14) 0.0042(15) -0.0022(14) C38 0.0295(17) 0.0402(17) 0.0385(17) 0.0051(14) 0.0001(13) -0.0029(13) C39 0.042(2) 0.060(2) 0.0390(18) 0.0043(17) -0.0025(15) -0.0102(16) C40 0.051(2) 0.095(3) 0.051(2) 0.008(2) -0.0110(19) -0.014(2) C41 0.040(2) 0.110(4) 0.071(3) 0.040(3) -0.016(2) -0.010(2) C42 0.038(2) 0.069(3) 0.085(3) 0.026(2) 0.008(2) 0.0152(18) C43 0.044(2) 0.0437(19) 0.056(2) 0.0060(17) 0.0081(16) 0.0027(15) C44 0.074(3) 0.075(3) 0.059(2) -0.025(2) 0.008(2) -0.008(2) C45 0.070(3) 0.061(2) 0.089(3) -0.018(2) 0.018(2) 0.011(2) C46 0.039(2) 0.0404(18) 0.0405(18) 0.0042(14) 0.0061(15) -0.0005(15) C47 0.0321(18) 0.0461(19) 0.055(2) 0.0157(16) 0.0084(16) -0.0005(14) C48 0.043(2) 0.0386(19) 0.089(3) 0.0035(19) 0.028(2) 0.0007(16) C49 0.056(3) 0.050(2) 0.124(4) 0.016(3) 0.040(3) 0.010(2) C50 0.051(3) 0.079(3) 0.120(4) 0.052(3) 0.027(3) 0.014(2) C51 0.045(2) 0.106(4) 0.077(3) 0.056(3) -0.005(2) -0.005(2) C52 0.043(2) 0.078(3) 0.052(2) 0.024(2) 0.0061(17) -0.0023(19) C53 0.077(3) 0.076(3) 0.101(3) -0.042(3) 0.033(3) -0.021(2) C54 0.077(3) 0.154(5) 0.056(3) -0.015(3) -0.001(2) -0.017(3) C25 0.145(5) 0.028(2) 0.054(3) -0.0084(19) -0.005(3) 0.002(2) C26 0.060(3) 0.045(2) 0.094(4) -0.011(2) 0.000(3) 0.011(2) C27 0.069(3) 0.039(2) 0.100(4) -0.013(2) 0.023(3) -0.012(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg N3 2.029(3) . ? Mg N2 2.088(2) . ? Mg N1 2.101(2) . ? Mg N5 2.228(3) . ? Mg N4 2.246(3) . ? Si1 N1 1.775(2) . ? Si1 C19 1.864(3) . ? Si1 C20 1.867(3) . ? Si1 C21 1.868(3) . ? Si2 Si2A 0.573(6) . ? Si2 C2 1.841(7) . ? Si2 C1 1.889(6) . ? Si2 Si4 2.360(6) . ? Si2A C1 1.834(7) . ? Si2A C2 1.855(7) . ? Si2A Si4 2.352(6) . ? Si3 N2 1.771(2) . ? Si3 C24 1.857(4) . ? Si3 C22 1.862(4) . ? Si3 C23 1.872(4) . ? Si4 C27A 1.60(5) . ? Si4 C26 1.843(4) . ? Si4 C25 1.875(4) . ? Si4 C27 1.880(4) . ? Si4 C25A 1.93(4) . ? Si4 C26A 2.05(3) . ? N1 C1 1.325(3) . ? N2 C2 1.329(3) . ? N3 C28 1.172(4) . ? N4 C37 1.142(4) . ? N5 C46 1.142(4) . ? C1 C3 1.513(4) . ? C2 C11 1.512(4) . ? C3 C4 1.397(4) . ? C3 C8 1.404(4) . ? C4 C5 1.406(5) . ? C4 C9 1.502(5) . ? C5 C6 1.361(6) . ? C6 C7 1.361(6) . ? C7 C8 1.403(5) . ? C8 C10 1.500(5) . ? C11 C12 1.395(4) . ? C11 C16 1.407(4) . ? C12 C13 1.401(5) . ? C12 C17 1.503(5) . ? C13 C14 1.358(6) . ? C14 C15 1.371(6) . ? C15 C16 1.392(5) . ? C16 C18 1.508(5) . ? C28 C29 1.376(4) . ? C29 C34 1.434(5) . ? C29 C30 1.461(4) . ? C30 C31 1.334(5) . ? C30 C35 1.491(5) . ? C31 C32 1.472(6) . ? C32 C33 1.500(7) . ? C33 C34 1.379(5) . ? C34 C36 1.498(6) . ? C37 C38 1.437(4) . ? C38 C43 1.393(4) . ? C38 C39 1.405(4) . ? C39 C40 1.366(5) . ? C39 C44 1.500(5) . ? C40 C41 1.364(6) . ? C41 C42 1.377(6) . ? C42 C43 1.387(5) . ? C43 C45 1.500(5) . ? C46 C47 1.441(4) . ? C47 C52 1.385(5) . ? C47 C48 1.411(5) . ? C48 C49 1.378(5) . ? C48 C53 1.496(6) . ? C49 C50 1.355(6) . ? C50 C51 1.367(6) . ? C51 C52 1.409(5) . ? C52 C54 1.497(6) . ? 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 N3 Mg N2 131.67(10) . . ? N3 Mg N1 113.89(10) . . ? N2 Mg N1 114.39(9) . . ? N3 Mg N5 89.13(10) . . ? N2 Mg N5 89.14(10) . . ? N1 Mg N5 94.65(9) . . ? N3 Mg N4 88.83(10) . . ? N2 Mg N4 85.72(9) . . ? N1 Mg N4 94.14(9) . . ? N5 Mg N4 171.05(10) . . ? N1 Si1 C19 106.97(13) . . ? N1 Si1 C20 105.45(12) . . ? C19 Si1 C20 110.62(15) . . ? N1 Si1 C21 119.47(13) . . ? C19 Si1 C21 106.40(15) . . ? C20 Si1 C21 107.87(15) . . ? Si2A Si2 C2 82.5(12) . . ? Si2A Si2 C1 75.7(11) . . ? C2 Si2 C1 116.5(3) . . ? Si2A Si2 Si4 82.2(11) . . ? C2 Si2 Si4 116.9(3) . . ? C1 Si2 Si4 117.9(3) . . ? Si2 Si2A C1 86.7(12) . . ? Si2 Si2A C2 79.7(12) . . ? C1 Si2A C2 118.6(3) . . ? Si2 Si2A Si4 83.8(11) . . ? C1 Si2A Si4 120.8(3) . . ? C2 Si2A Si4 116.7(3) . . ? N2 Si3 C24 114.39(15) . . ? N2 Si3 C22 106.18(14) . . ? C24 Si3 C22 106.13(19) . . ? N2 Si3 C23 114.13(14) . . ? C24 Si3 C23 108.99(18) . . ? C22 Si3 C23 106.37(18) . . ? C26 Si4 C25 105.8(2) . . ? C26 Si4 C27 109.2(2) . . ? C25 Si4 C27 104.3(2) . . ? C27A Si4 C25A 116(2) . . ? C27A Si4 C26A 117(2) . . ? C25A Si4 C26A 95.7(17) . . ? C27A Si4 Si2A 113(2) . . ? C26 Si4 Si2A 106.36(17) . . ? C25 Si4 Si2A 113.26(19) . . ? C27 Si4 Si2A 117.34(18) . . ? C25A Si4 Si2A 105.7(13) . . ? C26A Si4 Si2A 106.8(10) . . ? C27A Si4 Si2 99(2) . . ? C26 Si4 Si2 119.27(17) . . ? C25 Si4 Si2 111.47(19) . . ? C27 Si4 Si2 105.81(17) . . ? C25A Si4 Si2 114.3(12) . . ? C26A Si4 Si2 115.2(10) . . ? Si2A Si4 Si2 13.96(14) . . ? C1 N1 Si1 128.79(19) . . ? C1 N1 Mg 115.68(17) . . ? Si1 N1 Mg 115.16(11) . . ? C2 N2 Si3 126.34(19) . . ? C2 N2 Mg 114.69(18) . . ? Si3 N2 Mg 118.89(12) . . ? C28 N3 Mg 170.6(2) . . ? C37 N4 Mg 161.3(2) . . ? C46 N5 Mg 172.2(3) . . ? N1 C1 C3 120.4(2) . . ? N1 C1 Si2A 126.7(3) . . ? C3 C1 Si2A 112.1(3) . . ? N1 C1 Si2 125.8(3) . . ? C3 C1 Si2 113.0(3) . . ? Si2A C1 Si2 17.62(18) . . ? N2 C2 C11 120.2(2) . . ? N2 C2 Si2 128.4(3) . . ? C11 C2 Si2 110.7(3) . . ? N2 C2 Si2A 127.2(3) . . ? C11 C2 Si2A 111.6(3) . . ? Si2 C2 Si2A 17.83(18) . . ? C4 C3 C8 121.5(3) . . ? C4 C3 C1 119.2(3) . . ? C8 C3 C1 119.4(3) . . ? C3 C4 C5 118.1(4) . . ? C3 C4 C9 121.5(3) . . ? C5 C4 C9 120.4(4) . . ? C6 C5 C4 120.6(4) . . ? C7 C6 C5 121.1(4) . . ? C6 C7 C8 121.2(4) . . ? C7 C8 C3 117.5(4) . . ? C7 C8 C10 120.8(3) . . ? C3 C8 C10 121.7(3) . . ? C12 C11 C16 120.7(3) . . ? C12 C11 C2 119.8(3) . . ? C16 C11 C2 119.5(3) . . ? C11 C12 C13 118.2(4) . . ? C11 C12 C17 122.2(3) . . ? C13 C12 C17 119.6(4) . . ? C14 C13 C12 121.1(4) . . ? C13 C14 C15 120.8(4) . . ? C14 C15 C16 120.6(4) . . ? C15 C16 C11 118.6(4) . . ? C15 C16 C18 119.5(4) . . ? C11 C16 C18 121.9(3) . . ? N3 C28 C29 178.2(3) . . ? C28 C29 C34 121.5(3) . . ? C28 C29 C30 119.6(3) . . ? C34 C29 C30 118.8(3) . . ? C31 C30 C29 121.4(4) . . ? C31 C30 C35 120.4(4) . . ? C29 C30 C35 118.1(3) . . ? C30 C31 C32 123.4(4) . . ? C31 C32 C33 113.6(4) . . ? C34 C33 C32 123.1(4) . . ? C33 C34 C29 119.6(4) . . ? C33 C34 C36 122.2(4) . . ? C29 C34 C36 118.2(3) . . ? N4 C37 C38 177.8(3) . . ? C43 C38 C39 122.6(3) . . ? C43 C38 C37 119.7(3) . . ? C39 C38 C37 117.7(3) . . ? C40 C39 C38 117.6(3) . . ? C40 C39 C44 120.4(3) . . ? C38 C39 C44 121.9(3) . . ? C41 C40 C39 121.0(4) . . ? C40 C41 C42 121.3(4) . . ? C41 C42 C43 120.4(4) . . ? C42 C43 C38 117.1(3) . . ? C42 C43 C45 121.5(3) . . ? C38 C43 C45 121.4(3) . . ? N5 C46 C47 177.5(3) . . ? C52 C47 C48 122.8(3) . . ? C52 C47 C46 118.8(3) . . ? C48 C47 C46 118.3(3) . . ? C49 C48 C47 116.5(4) . . ? C49 C48 C53 121.8(4) . . ? C47 C48 C53 121.7(3) . . ? C50 C49 C48 122.0(4) . . ? C49 C50 C51 121.4(4) . . ? C50 C51 C52 120.0(4) . . ? C47 C52 C51 117.3(4) . . ? C47 C52 C54 121.3(3) . . ? C51 C52 C54 121.3(4) . . ? #===END data_(3)-mar3401 _database_code_depnum_ccdc_archive 'CCDC 260824' _audit_creation_date 2001-04-03T15:39:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ;'(Mg(thf)2(C6H6CN)(Me3SiNC(C6H3Me3)Si(SiMe3)C(C6H3Me2)NSiMe3)) ' ; _chemical_formula_moiety 'C44 H71 Mg1 N3 O2 Si4' _chemical_formula_structural 'C44 H71 N3 O2 SI4 MG' _chemical_formula_sum 'C44 H71 Mg N3 O2 Si4' _chemical_formula_weight 810.71 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6444(11) _cell_length_b 13.2595(17) _cell_length_c 17.768(2) _cell_angle_alpha 90.285(5) _cell_angle_beta 98.141(8) _cell_angle_gamma 110.075(8) _cell_volume 2327.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 27015 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.934 _exptl_absorpt_correction_T_max 0.990 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 11435 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_unetI/netI 0.1033 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 22.02 _diffrn_reflns_theta_full 22.02 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 5623 _reflns_number_gt 3826 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; One SiMe3 group has the methyls disordered. The Si4 atom has an alternative low occupancy site which shares two of the methyl sites. The third low occupancy methyl site was not located. 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^)+(0.0000P)^2^+3.5660P] 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_number_reflns 5623 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.433 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.052 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 Mg Mg 0.76388(15) 0.76501(12) 0.16537(9) 0.0304(4) Uani 1 1 d . A . Si1 Si 0.85854(14) 0.57460(11) 0.24511(9) 0.0391(4) Uani 1 1 d . . . Si2 Si 0.68446(14) 0.98026(11) 0.12555(8) 0.0374(4) Uani 1 1 d . A . Si3 Si 0.72847(13) 0.82675(10) 0.35252(8) 0.0310(4) Uani 1 1 d . . . O1 O 0.9771(3) 0.8568(2) 0.1798(2) 0.0405(9) Uani 1 1 d . . . O2 O 0.5564(3) 0.6592(3) 0.13595(19) 0.0425(9) Uani 1 1 d . . . N1 N 0.7965(3) 0.6794(3) 0.2625(2) 0.0277(9) Uani 1 1 d . A . N2 N 0.7150(3) 0.8993(3) 0.2006(2) 0.0258(9) Uani 1 1 d . . . N3 N 0.7791(4) 0.7416(4) 0.0527(3) 0.0487(12) Uani 1 1 d . . . C1 C 0.7700(4) 0.7076(3) 0.3297(3) 0.0273(11) Uani 1 1 d . A . C2 C 0.6985(4) 0.9092(3) 0.2726(3) 0.0273(11) Uani 1 1 d . A . C3 C 0.7823(5) 0.6413(4) 0.3976(3) 0.0312(12) Uani 1 1 d . . . C4 C 0.6691(5) 0.5549(4) 0.4124(3) 0.0350(12) Uani 1 1 d . A . C5 C 0.6815(6) 0.4934(4) 0.4740(3) 0.0484(15) Uani 1 1 d . . . H5 H 0.6052 0.4348 0.4839 0.058 Uiso 1 1 calc R A . C6 C 0.8037(6) 0.5165(5) 0.5211(3) 0.0580(16) Uani 1 1 d . A . H6 H 0.8111 0.4732 0.5628 0.07 Uiso 1 1 calc R . . C7 C 0.9134(6) 0.6007(4) 0.5083(3) 0.0515(15) Uani 1 1 d . . . H7 H 0.9969 0.6153 0.5412 0.062 Uiso 1 1 calc R A . C8 C 0.9058(5) 0.6667(4) 0.4473(3) 0.0383(13) Uani 1 1 d . A . C9 C 0.5346(5) 0.5261(4) 0.3624(3) 0.0450(14) Uani 1 1 d . . . H9A H 0.4661 0.4711 0.3858 0.067 Uiso 1 1 calc R A . H9B H 0.5407 0.498 0.3124 0.067 Uiso 1 1 calc R . . H9C H 0.5092 0.5903 0.3562 0.067 Uiso 1 1 calc R . . C10 C 1.0279(5) 0.7622(4) 0.4366(3) 0.0550(16) Uani 1 1 d . . . H10A H 1.0167 0.8282 0.4544 0.082 Uiso 1 1 calc R A . H10B H 1.0374 0.7656 0.3826 0.082 Uiso 1 1 calc R . . H10C H 1.1091 0.7548 0.4661 0.082 Uiso 1 1 calc R . . C11 C 0.6569(5) 1.0004(4) 0.2999(3) 0.0298(12) Uani 1 1 d . . . C12 C 0.7550(5) 1.0986(4) 0.3290(3) 0.0361(12) Uani 1 1 d . A . C13 C 0.7130(6) 1.1820(4) 0.3504(3) 0.0467(14) Uani 1 1 d . . . H13 H 0.7788 1.2493 0.3695 0.056 Uiso 1 1 calc R A . C14 C 0.5780(6) 1.1681(5) 0.3444(3) 0.0523(15) Uani 1 1 d . A . H14 H 0.5511 1.2259 0.3588 0.063 Uiso 1 1 calc R . . C15 C 0.4818(6) 1.0711(5) 0.3175(3) 0.0473(15) Uani 1 1 d . . . H15 H 0.3885 1.0619 0.314 0.057 Uiso 1 1 calc R A . C16 C 0.5196(5) 0.9853(4) 0.2950(3) 0.0382(13) Uani 1 1 d . A . C17 C 0.9046(5) 1.1187(4) 0.3355(3) 0.0493(15) Uani 1 1 d . . . H17A H 0.9555 1.1875 0.364 0.074 Uiso 1 1 calc R A . H17B H 0.93 1.1212 0.2844 0.074 Uiso 1 1 calc R . . H17C H 0.9255 1.0607 0.3622 0.074 Uiso 1 1 calc R . . C18 C 0.4106(5) 0.8818(4) 0.2636(3) 0.0533(16) Uani 1 1 d . . . H18A H 0.3267 0.8758 0.2829 0.08 Uiso 1 1 calc R A . H18B H 0.4386 0.8211 0.2795 0.08 Uiso 1 1 calc R . . H18C H 0.3955 0.8811 0.2079 0.08 Uiso 1 1 calc R . . C19 C 0.4461(5) 0.7826(4) 0.4475(3) 0.0461(16) Uani 0.928(4) 1 d P . . H19A H 0.414 0.7751 0.497 0.069 Uiso 0.928(4) 1 calc PR A 1 H19B H 0.4153 0.7118 0.4203 0.069 Uiso 0.928(4) 1 calc PR A 1 H19C H 0.41 0.831 0.4174 0.069 Uiso 0.928(4) 1 calc PR A 1 C20 C 0.7015(5) 0.7684(4) 0.5421(3) 0.0476(14) Uani 1 1 d . . . H20A H 0.8006 0.7935 0.5486 0.071 Uiso 0.928(4) 1 calc PR A 1 H20B H 0.665 0.6907 0.5295 0.071 Uiso 0.928(4) 1 calc PR A 1 H20C H 0.6727 0.7839 0.5895 0.071 Uiso 0.928(4) 1 calc PR A 1 C21 C 0.6829(6) 0.9813(4) 0.4980(3) 0.0570(16) Uani 1 1 d . . . H21A H 0.6443 0.9836 0.5446 0.086 Uiso 0.928(4) 1 calc PR A 1 H21B H 0.6473 1.0207 0.4591 0.086 Uiso 0.928(4) 1 calc PR A 1 H21C H 0.7817 1.0146 0.509 0.086 Uiso 0.928(4) 1 calc PR A 1 C25 C 0.5262(6) 0.8945(5) 0.0641(4) 0.086(2) Uani 1 1 d . . . H25A H 0.5327 0.8242 0.0527 0.13 Uiso 1 1 calc R A . H25B H 0.5141 0.9293 0.0165 0.13 Uiso 1 1 calc R . . H25C H 0.4487 0.8848 0.0908 0.13 Uiso 1 1 calc R . . C26 C 0.8236(6) 1.0105(5) 0.0671(3) 0.0669(19) Uani 1 1 d . . . H26A H 0.8355 0.9434 0.0523 0.1 Uiso 1 1 calc R A . H26B H 0.9078 1.0586 0.0969 0.1 Uiso 1 1 calc R . . H26C H 0.8008 1.0454 0.0213 0.1 Uiso 1 1 calc R . . C27 C 0.6760(6) 1.1137(4) 0.1479(3) 0.0527(15) Uani 1 1 d . . . H27A H 0.604 1.1056 0.1787 0.079 Uiso 1 1 calc R A . H27B H 0.6565 1.1466 0.1004 0.079 Uiso 1 1 calc R . . H27C H 0.7628 1.1597 0.1763 0.079 Uiso 1 1 calc R . . C28 C 0.7872(5) 0.7256(4) -0.0111(3) 0.0383(13) Uani 1 1 d . A . C29 C 0.7950(5) 0.7064(4) -0.0854(3) 0.0352(12) Uani 1 1 d . . . C30 C 0.9075(5) 0.6809(4) -0.1077(3) 0.0382(13) Uani 1 1 d . A . C31 C 0.9130(5) 0.6609(4) -0.1808(3) 0.0463(14) Uani 1 1 d . . . H31 H 0.9907 0.6479 -0.1924 0.056 Uiso 1 1 calc R A . C32 C 0.8041(5) 0.6576(4) -0.2458(3) 0.0543(15) Uani 1 1 d . A . H32A H 0.8445 0.7071 -0.2844 0.065 Uiso 1 1 calc R . . H32B H 0.7643 0.5839 -0.2702 0.065 Uiso 1 1 calc R . . C33 C 0.6948(5) 0.6892(4) -0.2192(3) 0.0438(13) Uani 1 1 d . . . H33 H 0.6244 0.6944 -0.2565 0.053 Uiso 1 1 calc R A . C34 C 0.6899(5) 0.7108(4) -0.1460(3) 0.0392(13) Uani 1 1 d . A . C35 C 1.0184(5) 0.6768(4) -0.0456(3) 0.0503(15) Uani 1 1 d . . . H35A H 0.9804 0.6202 -0.0115 0.075 Uiso 1 1 calc R A . H35B H 1.0579 0.7463 -0.0166 0.075 Uiso 1 1 calc R . . H35C H 1.0888 0.6614 -0.0686 0.075 Uiso 1 1 calc R . . C36 C 0.5762(5) 0.7418(4) -0.1245(3) 0.0487(14) Uani 1 1 d . . . H36A H 0.5166 0.7466 -0.1707 0.073 Uiso 1 1 calc R A . H36B H 0.6132 0.8118 -0.0959 0.073 Uiso 1 1 calc R . . H36C H 0.5244 0.6874 -0.0928 0.073 Uiso 1 1 calc R . . C37 C 1.0740(5) 0.8885(4) 0.1272(3) 0.0477(14) Uani 1 1 d . . . H37A H 1.0269 0.8838 0.0744 0.057 Uiso 1 1 calc R . . H37B H 1.1286 0.8409 0.1296 0.057 Uiso 1 1 calc R . . C38 C 1.1648(5) 1.0045(4) 0.1512(3) 0.0458(14) Uani 1 1 d . . . H38A H 1.2608 1.0104 0.1631 0.055 Uiso 1 1 calc R . . H38B H 1.1558 1.0533 0.1104 0.055 Uiso 1 1 calc R . . C39 C 1.1139(5) 1.0317(4) 0.2222(3) 0.0454(14) Uani 1 1 d . . . H39A H 1.19 1.0746 0.2611 0.054 Uiso 1 1 calc R . . H39B H 1.0514 1.0719 0.2095 0.054 Uiso 1 1 calc R . . C40 C 1.0414(5) 0.9225(4) 0.2491(3) 0.0411(13) Uani 1 1 d . . . H40A H 1.1061 0.894 0.2792 0.049 Uiso 1 1 calc R . . H40B H 0.9733 0.9258 0.2808 0.049 Uiso 1 1 calc R . . C41 C 0.4898(6) 0.5871(5) 0.0698(4) 0.077(2) Uani 1 1 d . . . H41A H 0.4915 0.514 0.0792 0.093 Uiso 1 1 calc R . . H41B H 0.535 0.6133 0.0251 0.093 Uiso 1 1 calc R . . C42 C 0.3466(6) 0.5859(5) 0.0565(4) 0.0678(19) Uani 1 1 d . . . H42A H 0.2825 0.5135 0.0378 0.081 Uiso 1 1 calc R . . H42B H 0.3362 0.6386 0.019 0.081 Uiso 1 1 calc R . . C43 C 0.3229(5) 0.6168(5) 0.1348(4) 0.0669(19) Uani 1 1 d . . . H43A H 0.301 0.6837 0.1337 0.08 Uiso 1 1 calc R . . H43B H 0.2484 0.5586 0.1527 0.08 Uiso 1 1 calc R . . C44 C 0.4561(5) 0.6335(5) 0.1848(3) 0.0587(16) Uani 1 1 d . . . H44A H 0.4762 0.6929 0.2237 0.07 Uiso 1 1 calc R . . H44B H 0.4532 0.5673 0.2111 0.07 Uiso 1 1 calc R . . Si4 Si 0.63671(15) 0.83973(11) 0.46279(9) 0.0336(6) Uani 0.928(4) 1 d P A 1 C22 C 1.0482(12) 0.6200(13) 0.2851(12) 0.091(6) Uani 0.60(2) 1 d P B 1 H22A H 1.0964 0.6873 0.263 0.137 Uiso 0.60(2) 1 calc PR B 1 H22B H 1.0841 0.5644 0.2721 0.137 Uiso 0.60(2) 1 calc PR B 1 H22C H 1.0606 0.6313 0.3406 0.137 Uiso 0.60(2) 1 calc PR B 1 C23 C 0.780(3) 0.4489(15) 0.2893(17) 0.138(13) Uani 0.60(2) 1 d P B 1 H23A H 0.8089 0.4587 0.3445 0.207 Uiso 0.60(2) 1 calc PR B 1 H23B H 0.8071 0.3922 0.2687 0.207 Uiso 0.60(2) 1 calc PR B 1 H23C H 0.6811 0.4283 0.2783 0.207 Uiso 0.60(2) 1 calc PR B 1 C24 C 0.843(2) 0.5532(13) 0.1432(6) 0.090(8) Uani 0.60(2) 1 d P B 1 H24A H 0.8933 0.6204 0.1217 0.135 Uiso 0.60(2) 1 calc PR B 1 H24B H 0.7473 0.5302 0.1207 0.135 Uiso 0.60(2) 1 calc PR B 1 H24C H 0.8799 0.4975 0.132 0.135 Uiso 0.60(2) 1 calc PR B 1 C22A C 1.012(3) 0.6294(14) 0.207(3) 0.14(2) Uani 0.40(2) 1 d P B 2 H22D H 0.9917 0.6268 0.1511 0.213 Uiso 0.40(2) 1 calc PR B 2 H22E H 1.0703 0.5873 0.2217 0.213 Uiso 0.40(2) 1 calc PR B 2 H22F H 1.0584 0.7042 0.2263 0.213 Uiso 0.40(2) 1 calc PR B 2 C23A C 0.862(5) 0.471(3) 0.3056(19) 0.127(18) Uani 0.40(2) 1 d P B 2 H23D H 0.9311 0.5004 0.3503 0.19 Uiso 0.40(2) 1 calc PR B 2 H23E H 0.8831 0.4159 0.2783 0.19 Uiso 0.40(2) 1 calc PR B 2 H23F H 0.7731 0.4387 0.322 0.19 Uiso 0.40(2) 1 calc PR B 2 C24A C 0.722(3) 0.4872(19) 0.1613(14) 0.091(9) Uani 0.40(2) 1 d P B 2 H24D H 0.6321 0.4666 0.1764 0.137 Uiso 0.40(2) 1 calc PR B 2 H24E H 0.742 0.4223 0.1499 0.137 Uiso 0.40(2) 1 calc PR B 2 H24F H 0.7248 0.5291 0.1159 0.137 Uiso 0.40(2) 1 calc PR B 2 Si4A Si 0.752(2) 0.8773(14) 0.4760(11) 0.028(7) Uiso 0.072(4) 1 d P A 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 Mg 0.0339(9) 0.0289(9) 0.0308(10) 0.0050(7) 0.0056(7) 0.0134(7) Si1 0.0499(9) 0.0316(8) 0.0456(10) 0.0119(7) 0.0159(7) 0.0233(7) Si2 0.0496(9) 0.0333(8) 0.0314(9) 0.0080(7) 0.0006(7) 0.0193(7) Si3 0.0381(8) 0.0314(8) 0.0297(9) 0.0085(6) 0.0094(6) 0.0182(6) O1 0.0368(19) 0.040(2) 0.042(2) -0.0005(18) 0.0175(17) 0.0053(16) O2 0.041(2) 0.042(2) 0.035(2) -0.0037(17) 0.0033(17) 0.0032(16) N1 0.029(2) 0.022(2) 0.033(3) 0.0048(18) 0.0053(18) 0.0090(17) N2 0.029(2) 0.028(2) 0.022(2) 0.0086(18) 0.0035(17) 0.0114(17) N3 0.038(3) 0.070(3) 0.038(3) -0.005(3) 0.004(2) 0.020(2) C1 0.017(2) 0.024(3) 0.036(3) 0.010(2) 0.002(2) 0.0016(19) C2 0.020(2) 0.022(3) 0.037(3) 0.004(2) 0.002(2) 0.005(2) C3 0.041(3) 0.027(3) 0.029(3) 0.003(2) 0.006(2) 0.015(2) C4 0.048(3) 0.026(3) 0.032(3) 0.002(2) 0.008(3) 0.013(2) C5 0.054(4) 0.036(3) 0.052(4) 0.013(3) 0.013(3) 0.009(3) C6 0.080(5) 0.051(4) 0.053(4) 0.024(3) 0.018(4) 0.032(3) C7 0.061(4) 0.052(4) 0.047(4) 0.008(3) -0.006(3) 0.032(3) C8 0.048(3) 0.029(3) 0.037(3) 0.002(3) -0.001(3) 0.017(3) C9 0.042(3) 0.037(3) 0.046(4) 0.009(3) 0.010(3) 0.000(2) C10 0.037(3) 0.051(4) 0.070(4) 0.007(3) -0.009(3) 0.013(3) C11 0.037(3) 0.030(3) 0.025(3) 0.010(2) 0.007(2) 0.015(2) C12 0.044(3) 0.035(3) 0.033(3) 0.007(2) 0.009(2) 0.017(3) C13 0.070(4) 0.033(3) 0.042(4) 0.003(3) 0.013(3) 0.022(3) C14 0.081(5) 0.056(4) 0.039(4) 0.013(3) 0.015(3) 0.046(4) C15 0.052(4) 0.063(4) 0.042(4) 0.008(3) 0.012(3) 0.038(3) C16 0.042(3) 0.049(3) 0.033(3) 0.010(3) 0.009(2) 0.028(3) C17 0.047(3) 0.038(3) 0.059(4) 0.000(3) 0.009(3) 0.010(3) C18 0.037(3) 0.062(4) 0.061(4) 0.007(3) 0.002(3) 0.019(3) C19 0.046(4) 0.058(4) 0.044(4) 0.011(3) 0.017(3) 0.026(3) C20 0.057(3) 0.063(4) 0.030(3) 0.010(3) 0.012(3) 0.029(3) C21 0.082(4) 0.050(4) 0.041(4) 0.000(3) 0.026(3) 0.019(3) C25 0.097(5) 0.053(4) 0.073(5) 0.023(4) -0.045(4) 0.003(4) C26 0.116(5) 0.070(4) 0.045(4) 0.033(3) 0.034(4) 0.061(4) C27 0.085(4) 0.045(3) 0.043(4) 0.015(3) 0.016(3) 0.038(3) C28 0.032(3) 0.039(3) 0.045(4) 0.002(3) 0.005(3) 0.014(2) C29 0.033(3) 0.037(3) 0.034(3) -0.001(2) 0.005(2) 0.009(2) C30 0.040(3) 0.034(3) 0.038(4) -0.001(3) 0.008(3) 0.008(2) C31 0.050(3) 0.040(3) 0.051(4) 0.001(3) 0.024(3) 0.013(3) C32 0.061(4) 0.049(4) 0.046(4) -0.003(3) 0.014(3) 0.008(3) C33 0.051(3) 0.036(3) 0.040(4) 0.003(3) 0.008(3) 0.009(3) C34 0.042(3) 0.031(3) 0.040(4) 0.004(3) 0.008(3) 0.007(2) C35 0.054(4) 0.052(4) 0.049(4) -0.003(3) 0.016(3) 0.021(3) C36 0.055(3) 0.048(3) 0.043(4) 0.002(3) 0.001(3) 0.020(3) C37 0.043(3) 0.048(4) 0.050(4) 0.004(3) 0.022(3) 0.007(3) C38 0.041(3) 0.040(3) 0.053(4) 0.005(3) 0.015(3) 0.006(3) C39 0.043(3) 0.039(3) 0.052(4) -0.001(3) 0.011(3) 0.009(2) C40 0.036(3) 0.043(3) 0.042(4) 0.001(3) 0.012(3) 0.010(2) C41 0.070(5) 0.073(5) 0.059(5) -0.028(4) 0.013(4) -0.013(4) C42 0.065(4) 0.053(4) 0.060(5) -0.003(3) -0.015(3) -0.003(3) C43 0.040(3) 0.052(4) 0.094(6) -0.003(4) -0.003(3) 0.002(3) C44 0.044(4) 0.076(4) 0.051(4) 0.001(3) 0.012(3) 0.012(3) Si4 0.0401(12) 0.0297(9) 0.0325(10) 0.0056(7) 0.0108(7) 0.0121(8) C22 0.051(7) 0.115(12) 0.125(15) -0.045(11) -0.014(8) 0.062(7) C23 0.21(2) 0.030(8) 0.25(3) 0.050(11) 0.18(2) 0.071(12) C24 0.19(2) 0.106(13) 0.034(7) 0.010(7) 0.019(9) 0.127(16) C22A 0.10(2) 0.042(12) 0.32(6) 0.03(2) 0.14(3) 0.033(13) C23A 0.27(5) 0.13(3) 0.089(19) 0.099(19) 0.13(3) 0.16(3) C24A 0.119(19) 0.085(16) 0.077(16) -0.034(13) -0.012(14) 0.055(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg N3 2.061(5) . ? Mg N1 2.124(4) . ? Mg N2 2.133(4) . ? Mg O1 2.152(3) . ? Mg O2 2.158(3) . ? Si1 C23A 1.76(2) . ? Si1 N1 1.773(4) . ? Si1 C22A 1.779(17) . ? Si1 C24 1.807(10) . ? Si1 C23 1.827(18) . ? Si1 C22 1.923(11) . ? Si1 C24A 1.970(18) . ? Si2 N2 1.780(4) . ? Si2 C27 1.846(5) . ? Si2 C26 1.862(6) . ? Si2 C25 1.864(6) . ? Si3 C1 1.839(5) . ? Si3 C2 1.855(5) . ? Si3 Si4A 2.246(19) . ? Si3 Si4 2.340(2) . ? O1 C40 1.445(6) . ? O1 C37 1.448(5) . ? O2 C44 1.424(6) . ? O2 C41 1.443(6) . ? N1 C1 1.345(6) . ? N2 C2 1.328(6) . ? N3 C28 1.174(6) . ? C1 C3 1.512(6) . ? C2 C11 1.521(6) . ? C3 C4 1.407(6) . ? C3 C8 1.409(6) . ? C4 C5 1.386(7) . ? C4 C9 1.499(6) . ? C5 C6 1.378(7) . ? C6 C7 1.358(7) . ? C7 C8 1.408(7) . ? C8 C10 1.507(7) . ? C11 C16 1.395(6) . ? C11 C12 1.400(6) . ? C12 C13 1.398(7) . ? C12 C17 1.509(6) . ? C13 C14 1.373(7) . ? C14 C15 1.373(7) . ? C15 C16 1.405(7) . ? C16 C18 1.502(7) . ? C19 Si4 1.884(5) . ? C20 Si4 1.882(5) . ? C21 Si4 1.851(5) . ? C28 C29 1.361(7) . ? C29 C30 1.455(6) . ? C29 C34 1.456(7) . ? C30 C31 1.336(7) . ? C30 C35 1.513(7) . ? C31 C32 1.506(7) . ? C32 C33 1.497(7) . ? C33 C34 1.341(7) . ? C34 C36 1.501(7) . ? C37 C38 1.530(7) . ? C38 C39 1.529(7) . ? C39 C40 1.505(6) . ? C41 C42 1.503(8) . ? C42 C43 1.527(8) . ? C43 C44 1.508(7) . ? 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 N3 Mg N1 131.42(18) . . ? N3 Mg N2 119.82(17) . . ? N1 Mg N2 108.71(16) . . ? N3 Mg O1 86.11(15) . . ? N1 Mg O1 89.84(14) . . ? N2 Mg O1 92.64(14) . . ? N3 Mg O2 85.65(16) . . ? N1 Mg O2 92.43(14) . . ? N2 Mg O2 95.14(14) . . ? O1 Mg O2 170.73(15) . . ? C23A Si1 N1 126.1(10) . . ? C23A Si1 C22A 111.9(13) . . ? N1 Si1 C22A 109.0(6) . . ? N1 Si1 C24 107.8(3) . . ? N1 Si1 C23 115.4(6) . . ? C24 Si1 C23 111.2(10) . . ? N1 Si1 C22 109.4(4) . . ? C24 Si1 C22 107.1(7) . . ? C23 Si1 C22 105.6(10) . . ? C23A Si1 C24A 98.4(15) . . ? N1 Si1 C24A 102.3(6) . . ? C22A Si1 C24A 106.2(14) . . ? N2 Si2 C27 120.0(2) . . ? N2 Si2 C26 108.9(2) . . ? C27 Si2 C26 103.7(3) . . ? N2 Si2 C25 105.9(2) . . ? C27 Si2 C25 110.6(3) . . ? C26 Si2 C25 107.3(3) . . ? C1 Si3 C2 117.4(2) . . ? C1 Si3 Si4A 117.5(5) . . ? C2 Si3 Si4A 124.2(5) . . ? C1 Si3 Si4 120.99(16) . . ? C2 Si3 Si4 117.65(16) . . ? C40 O1 C37 105.9(3) . . ? C40 O1 Mg 119.6(3) . . ? C37 O1 Mg 133.0(3) . . ? C44 O2 C41 102.9(4) . . ? C44 O2 Mg 126.0(3) . . ? C41 O2 Mg 130.5(3) . . ? C1 N1 Si1 126.2(3) . . ? C1 N1 Mg 119.3(3) . . ? Si1 N1 Mg 114.5(2) . . ? C2 N2 Si2 126.6(3) . . ? C2 N2 Mg 118.6(3) . . ? Si2 N2 Mg 114.5(2) . . ? C28 N3 Mg 178.3(4) . . ? N1 C1 C3 119.5(4) . . ? N1 C1 Si3 127.0(3) . . ? C3 C1 Si3 113.4(3) . . ? N2 C2 C11 120.8(4) . . ? N2 C2 Si3 128.1(3) . . ? C11 C2 Si3 111.0(3) . . ? C4 C3 C8 119.4(4) . . ? C4 C3 C1 120.0(4) . . ? C8 C3 C1 120.6(4) . . ? C5 C4 C3 119.7(5) . . ? C5 C4 C9 118.7(4) . . ? C3 C4 C9 121.6(4) . . ? C6 C5 C4 120.6(5) . . ? C7 C6 C5 120.4(5) . . ? C6 C7 C8 121.3(5) . . ? C7 C8 C3 118.5(5) . . ? C7 C8 C10 119.9(5) . . ? C3 C8 C10 121.6(4) . . ? C16 C11 C12 120.3(4) . . ? C16 C11 C2 119.2(4) . . ? C12 C11 C2 120.5(4) . . ? C13 C12 C11 118.9(5) . . ? C13 C12 C17 118.8(5) . . ? C11 C12 C17 122.3(4) . . ? C14 C13 C12 120.9(5) . . ? C15 C14 C13 120.2(5) . . ? C14 C15 C16 120.7(5) . . ? C11 C16 C15 118.9(5) . . ? C11 C16 C18 122.3(4) . . ? C15 C16 C18 118.7(5) . . ? N3 C28 C29 179.3(6) . . ? C28 C29 C30 122.0(5) . . ? C28 C29 C34 120.9(4) . . ? C30 C29 C34 117.1(5) . . ? C31 C30 C29 121.4(5) . . ? C31 C30 C35 120.6(5) . . ? C29 C30 C35 118.0(5) . . ? C30 C31 C32 124.3(5) . . ? C33 C32 C31 111.4(5) . . ? C34 C33 C32 124.3(5) . . ? C33 C34 C29 121.4(5) . . ? C33 C34 C36 120.7(5) . . ? C29 C34 C36 118.0(5) . . ? O1 C37 C38 106.6(4) . . ? C39 C38 C37 104.5(4) . . ? C40 C39 C38 102.8(4) . . ? O1 C40 C39 104.2(4) . . ? O2 C41 C42 105.9(5) . . ? C41 C42 C43 104.0(5) . . ? C44 C43 C42 103.5(5) . . ? O2 C44 C43 106.5(5) . . ? C21 Si4 C20 106.8(3) . . ? C21 Si4 C19 105.8(3) . . ? C20 Si4 C19 108.2(2) . . ? C21 Si4 Si3 111.69(18) . . ? C20 Si4 Si3 111.00(17) . . ? C19 Si4 Si3 112.94(19) . . ? #===END data_(4)-feb700 _database_code_depnum_ccdc_archive 'CCDC 260825' _audit_creation_date 2000-02-04T14:45:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common "'((Mg(O3SCF3)(Me3SiNCRSi(SiMe3)CRNSiMe3))2) R=C6H3Me2'" _chemical_formula_moiety 'C56 H90 F6 Mg2 N4 O6 S2 Si8' _chemical_formula_structural 'C56 H90 F6 Mg2 N4 O6 S2 Si8' _chemical_formula_sum 'C56 H90 F6 Mg2 N4 O6 S2 Si8' _chemical_formula_weight 1366.78 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.8609(2) _cell_length_b 23.2225(4) _cell_length_c 19.0143(3) _cell_angle_alpha 90 _cell_angle_beta 92.4670(10) _cell_angle_gamma 90 _cell_volume 7438.19(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 52054 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION not applied #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.277 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 71348 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.55 _diffrn_reflns_theta_max 30.02 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 21516 _reflns_number_gt 14520 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 _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_number_reflns 21516 _refine_ls_number_parameters 780 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.053 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.054 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.096 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 Mg Mg -0.05841(4) 0.55278(3) 0.10235(3) 0.02679(14) Uani 1 1 d . . . S S -0.09547(3) 0.44353(3) -0.00288(3) 0.03052(19) Uani 0.896(2) 1 d P A 1 Si1 Si 0.01222(3) 0.64866(2) 0.20652(3) 0.02759(12) Uani 1 1 d . B 1 Si2 Si 0.05868(4) 0.71964(2) 0.28483(3) 0.03210(13) Uani 1 1 d . B 1 Si3 Si -0.17961(3) 0.64978(3) 0.02928(3) 0.03581(14) Uani 1 1 d . B 1 Si4 Si -0.06493(3) 0.46262(2) 0.23695(3) 0.02941(12) Uani 1 1 d . B 1 F1 F -0.18994(10) 0.38027(8) -0.08092(9) 0.0745(5) Uani 1 1 d . A 1 F2 F -0.24552(9) 0.42110(10) 0.00539(9) 0.0845(7) Uani 1 1 d . A 1 F3 F -0.21625(10) 0.47124(10) -0.08496(10) 0.0857(6) Uani 1 1 d . A 1 O1 O -0.11128(8) 0.49494(7) 0.03885(7) 0.0363(3) Uani 1 1 d . A 1 O2 O -0.04795(8) 0.45623(7) -0.06185(8) 0.0414(4) Uani 1 1 d . . 1 O3 O -0.07274(13) 0.39366(9) 0.03595(9) 0.0634(5) Uani 1 1 d . A 1 N1 N -0.10291(9) 0.63451(7) 0.09359(8) 0.0275(3) Uani 1 1 d . B 1 N2 N -0.04615(9) 0.53352(7) 0.20704(8) 0.0262(3) Uani 1 1 d . B 1 C1 C -0.06339(11) 0.66976(9) 0.13721(9) 0.0266(4) Uani 1 1 d . B 1 C2 C -0.07450(12) 0.73415(9) 0.13107(11) 0.0347(5) Uani 1 1 d . B 1 C3 C -0.02745(16) 0.76560(10) 0.08549(13) 0.0471(6) Uani 1 1 d . B 1 C4 C -0.0400(2) 0.82472(12) 0.08021(17) 0.0700(9) Uani 1 1 d . B 1 H4 H -0.0089 0.8468 0.0496 0.084 Uiso 1 1 calc R B 1 C5 C -0.0959(2) 0.85151(13) 0.1182(2) 0.0806(12) Uani 1 1 d . B 1 H5 H -0.1037 0.8918 0.1132 0.097 Uiso 1 1 calc R B 1 C6 C -0.14132(19) 0.82077(13) 0.16356(19) 0.0699(10) Uani 1 1 d . B 1 H6 H -0.1797 0.8402 0.1899 0.084 Uiso 1 1 calc R B 1 C7 C -0.13151(14) 0.76091(11) 0.17132(14) 0.0475(6) Uani 1 1 d . B 1 C8 C -0.18321(15) 0.72657(14) 0.21827(16) 0.0616(8) Uani 1 1 d . B 1 H8A H -0.2191 0.7526 0.2421 0.092 Uiso 0.5 1 calc PR B 1 H8B H -0.1498 0.706 0.2534 0.092 Uiso 0.5 1 calc PR B 1 H8C H -0.2144 0.6988 0.1899 0.092 Uiso 0.5 1 calc PR B 1 H8D H -0.1698 0.6856 0.2148 0.092 Uiso 0.5 1 calc PR B 1 H8E H -0.2391 0.7323 0.2035 0.092 Uiso 0.5 1 calc PR B 1 H8F H -0.1745 0.7394 0.2671 0.092 Uiso 0.5 1 calc PR B 1 C9 C 0.03530(18) 0.73748(13) 0.04368(14) 0.0569(7) Uani 1 1 d . B 1 H9A H 0.0365 0.6961 0.0537 0.085 Uiso 0.5 1 calc PR B 1 H9B H 0.0871 0.7544 0.0567 0.085 Uiso 0.5 1 calc PR B 1 H9C H 0.0233 0.7436 -0.0066 0.085 Uiso 0.5 1 calc PR B 1 H9D H 0.0615 0.7666 0.0155 0.085 Uiso 0.5 1 calc PR B 1 H9E H 0.0108 0.7083 0.0124 0.085 Uiso 0.5 1 calc PR B 1 H9F H 0.0746 0.7191 0.0758 0.085 Uiso 0.5 1 calc PR B 1 C10 C -0.00841(10) 0.57609(8) 0.24145(9) 0.0235(4) Uani 1 1 d . B 1 C11 C 0.02632(11) 0.56543(8) 0.31479(10) 0.0267(4) Uani 1 1 d . B 1 C12 C -0.01880(13) 0.57709(9) 0.37308(10) 0.0346(5) Uani 1 1 d . B 1 C13 C 0.01350(18) 0.56365(11) 0.44033(11) 0.0502(7) Uani 1 1 d . B 1 H13 H -0.017 0.5707 0.4803 0.06 Uiso 1 1 calc R B 1 C14 C 0.08767(19) 0.54074(12) 0.44959(13) 0.0578(8) Uani 1 1 d . B 1 H14 H 0.1082 0.5316 0.4955 0.069 Uiso 1 1 calc R B 1 C15 C 0.13314(16) 0.53088(11) 0.39171(14) 0.0507(7) Uani 1 1 d . B 1 H15 H 0.1851 0.5155 0.3985 0.061 Uiso 1 1 calc R B 1 C16 C 0.10366(12) 0.54322(9) 0.32366(11) 0.0357(5) Uani 1 1 d . B 1 C17 C 0.15586(14) 0.53336(12) 0.26253(14) 0.0496(6) Uani 1 1 d . B 1 H17A H 0.1269 0.5439 0.2186 0.074 Uiso 0.5 1 calc PR B 1 H17B H 0.1709 0.4926 0.2608 0.074 Uiso 0.5 1 calc PR B 1 H17C H 0.2037 0.5571 0.2683 0.074 Uiso 0.5 1 calc PR B 1 H17D H 0.2075 0.5185 0.2799 0.074 Uiso 0.5 1 calc PR B 1 H17E H 0.1634 0.5698 0.2377 0.074 Uiso 0.5 1 calc PR B 1 H17F H 0.1306 0.5053 0.2302 0.074 Uiso 0.5 1 calc PR B 1 C18 C -0.10236(14) 0.60029(11) 0.36511(14) 0.0488(6) Uani 1 1 d . B 1 H18A H -0.1238 0.6056 0.4118 0.073 Uiso 0.5 1 calc PR B 1 H18B H -0.1357 0.573 0.3379 0.073 Uiso 0.5 1 calc PR B 1 H18C H -0.1018 0.6373 0.3405 0.073 Uiso 0.5 1 calc PR B 1 H18D H -0.1171 0.605 0.315 0.073 Uiso 0.5 1 calc PR B 1 H18E H -0.1052 0.6376 0.3888 0.073 Uiso 0.5 1 calc PR B 1 H18F H -0.1391 0.5733 0.3863 0.073 Uiso 0.5 1 calc PR B 1 C19 C -0.14366(16) 0.62446(14) -0.05653(12) 0.0538(7) Uani 1 1 d . B 1 H19A H -0.0981 0.6478 -0.0694 0.081 Uiso 1 1 calc R B 1 H19B H -0.1863 0.6283 -0.0929 0.081 Uiso 1 1 calc R B 1 H19C H -0.1276 0.584 -0.0525 0.081 Uiso 1 1 calc R B 1 C20 C -0.26452(15) 0.60452(15) 0.05495(15) 0.0633(8) Uani 1 1 d . B 1 H20A H -0.2478 0.5641 0.0579 0.095 Uiso 1 1 calc R B 1 H20B H -0.3083 0.6084 0.0196 0.095 Uiso 1 1 calc R B 1 H20C H -0.2823 0.6171 0.1009 0.095 Uiso 1 1 calc R B 1 C21 C -0.21463(19) 0.72541(13) 0.01791(17) 0.0722(10) Uani 1 1 d . B 1 H21A H -0.2326 0.74 0.0629 0.108 Uiso 1 1 calc R B 1 H21B H -0.2588 0.7266 -0.0173 0.108 Uiso 1 1 calc R B 1 H21C H -0.171 0.7494 0.0022 0.108 Uiso 1 1 calc R B 1 C22 C -0.01381(18) 0.75077(12) 0.34614(13) 0.0539(7) Uani 1 1 d . B 1 H22A H -0.0332 0.7203 0.3766 0.081 Uiso 1 1 calc R B 1 H22B H -0.0586 0.7677 0.3188 0.081 Uiso 1 1 calc R B 1 H22C H 0.0124 0.7807 0.3751 0.081 Uiso 1 1 calc R B 1 C23 C 0.09776(15) 0.78064(10) 0.23183(13) 0.0437(5) Uani 1 1 d . B 1 H23A H 0.1307 0.8058 0.2625 0.066 Uiso 1 1 calc R B 1 H23B H 0.0532 0.8028 0.2109 0.066 Uiso 1 1 calc R B 1 H23C H 0.1298 0.7653 0.1944 0.066 Uiso 1 1 calc R B 1 C24 C 0.14384(16) 0.68983(11) 0.33991(15) 0.0574(7) Uani 1 1 d . B 1 H24A H 0.1821 0.672 0.3093 0.086 Uiso 1 1 calc R B 1 H24B H 0.1241 0.6609 0.3724 0.086 Uiso 1 1 calc R B 1 H24C H 0.1698 0.7211 0.3669 0.086 Uiso 1 1 calc R B 1 C25 C 0.01617(15) 0.41638(10) 0.20447(14) 0.0474(6) Uani 1 1 d . B 1 H25A H 0.0223 0.4236 0.1542 0.071 Uiso 1 1 calc R B 1 H25B H 0.0029 0.3758 0.2115 0.071 Uiso 1 1 calc R B 1 H25C H 0.066 0.4254 0.2306 0.071 Uiso 1 1 calc R B 1 C26 C -0.07389(15) 0.45002(10) 0.33313(11) 0.0405(5) Uani 1 1 d . B 1 H26A H -0.0233 0.459 0.358 0.061 Uiso 1 1 calc R B 1 H26B H -0.0874 0.4096 0.3412 0.061 Uiso 1 1 calc R B 1 H26C H -0.1157 0.4748 0.3508 0.061 Uiso 1 1 calc R B 1 C27 C -0.16303(14) 0.44230(11) 0.19464(12) 0.0429(5) Uani 1 1 d . B 1 H27A H -0.1981 0.476 0.193 0.064 Uiso 1 1 calc R B 1 H27B H -0.1871 0.4117 0.2221 0.064 Uiso 1 1 calc R B 1 H27C H -0.1554 0.4286 0.1467 0.064 Uiso 1 1 calc R B 1 C28 C -0.19288(15) 0.42713(14) -0.04222(15) 0.0562(7) Uani 1 1 d . A 1 Mg1B Mg 0.43635(4) 0.56399(3) 0.58781(3) 0.02535(14) Uani 1 1 d . . 1 S1B S 0.38471(3) 0.46747(2) 0.46600(2) 0.03010(11) Uani 1 1 d . C 1 Si1B Si 0.51225(3) 0.65339(2) 0.69869(3) 0.02589(12) Uani 1 1 d . D 1 Si2B Si 0.55883(4) 0.71991(3) 0.78293(3) 0.03274(13) Uani 1 1 d . D 1 Si3B Si 0.32044(3) 0.66769(3) 0.52226(3) 0.03342(13) Uani 1 1 d . D 1 Si4B Si 0.41317(3) 0.47180(2) 0.71714(3) 0.03082(13) Uani 1 1 d . D 1 F1B F 0.34634(10) 0.37818(7) 0.54024(8) 0.0629(4) Uani 1 1 d . C 1 F2B F 0.31290(9) 0.37254(7) 0.43080(8) 0.0647(5) Uani 1 1 d . C 1 F3B F 0.24796(8) 0.42776(8) 0.49869(9) 0.0628(4) Uani 1 1 d . C 1 O1B O 0.38140(8) 0.50349(6) 0.52875(7) 0.0330(3) Uani 1 1 d . C 1 O2B O 0.35272(10) 0.49238(8) 0.40276(8) 0.0493(4) Uani 1 1 d . C 1 O3B O 0.46200(8) 0.43990(7) 0.46164(8) 0.0364(3) Uani 1 1 d . . 1 N1B N 0.39679(9) 0.64741(7) 0.58480(8) 0.0262(3) Uani 1 1 d . D 1 N2B N 0.44372(9) 0.54144(7) 0.69196(8) 0.0252(3) Uani 1 1 d . D 1 C1B C 0.43866(10) 0.67971(8) 0.63027(9) 0.0251(4) Uani 1 1 d . D 1 C2B C 0.43219(12) 0.74449(9) 0.62768(11) 0.0329(4) Uani 1 1 d . D 1 C3B C 0.48355(15) 0.77566(11) 0.58539(13) 0.0476(6) Uani 1 1 d . D 1 C4B C 0.4766(2) 0.83546(13) 0.58415(18) 0.0727(10) Uani 1 1 d . D 1 H4B H 0.5107 0.8574 0.556 0.087 Uiso 1 1 calc R D 1 C5B C 0.4214(2) 0.86327(13) 0.6228(2) 0.0880(14) Uani 1 1 d . D 1 H5B H 0.4174 0.904 0.6206 0.106 Uiso 1 1 calc R D 1 C6B C 0.3724(2) 0.83299(13) 0.66426(19) 0.0714(10) Uani 1 1 d . D 1 H6B H 0.3351 0.853 0.6912 0.086 Uiso 1 1 calc R D 1 C7B C 0.37613(14) 0.77265(10) 0.66777(13) 0.0464(6) Uani 1 1 d . D 1 C8B C 0.31913(15) 0.73975(14) 0.71076(16) 0.0599(8) Uani 1 1 d . D 1 H8B1 H 0.2849 0.7668 0.7349 0.09 Uiso 0.5 1 calc PR D 1 H8B2 H 0.3488 0.7163 0.7457 0.09 Uiso 0.5 1 calc PR D 1 H8B3 H 0.2864 0.7147 0.6799 0.09 Uiso 0.5 1 calc PR D 1 H8B4 H 0.3285 0.6984 0.7054 0.09 Uiso 0.5 1 calc PR D 1 H8B5 H 0.2646 0.7489 0.6946 0.09 Uiso 0.5 1 calc PR D 1 H8B6 H 0.327 0.7505 0.7604 0.09 Uiso 0.5 1 calc PR D 1 C9B C 0.54457(17) 0.74601(14) 0.54271(14) 0.0626(8) Uani 1 1 d . D 1 H9B1 H 0.5412 0.7043 0.5498 0.094 Uiso 0.5 1 calc PR D 1 H9B2 H 0.5977 0.7595 0.5578 0.094 Uiso 0.5 1 calc PR D 1 H9B3 H 0.5345 0.7549 0.4927 0.094 Uiso 0.5 1 calc PR D 1 H9B4 H 0.5744 0.7748 0.5171 0.094 Uiso 0.5 1 calc PR D 1 H9B5 H 0.518 0.7196 0.5091 0.094 Uiso 0.5 1 calc PR D 1 H9B6 H 0.5811 0.7243 0.5742 0.094 Uiso 0.5 1 calc PR D 1 C10B C 0.48093(10) 0.58167(8) 0.73063(9) 0.0237(4) Uani 1 1 d . D 1 C11B C 0.50390(11) 0.57082(8) 0.80721(9) 0.0261(4) Uani 1 1 d . D 1 C12B C 0.45047(12) 0.58556(9) 0.85878(10) 0.0299(4) Uani 1 1 d . D 1 C13B C 0.47182(14) 0.57555(10) 0.92932(11) 0.0393(5) Uani 1 1 d . D 1 H13B H 0.4357 0.585 0.9646 0.047 Uiso 1 1 calc R D 1 C14B C 0.54469(14) 0.55212(10) 0.94860(11) 0.0412(5) Uani 1 1 d . D 1 H14B H 0.559 0.546 0.9969 0.049 Uiso 1 1 calc R D 1 C15B C 0.59647(14) 0.53764(10) 0.89761(11) 0.0388(5) Uani 1 1 d . D 1 H15B H 0.6463 0.521 0.9113 0.047 Uiso 1 1 calc R D 1 C16B C 0.57789(12) 0.54667(9) 0.82630(10) 0.0321(4) Uani 1 1 d . D 1 C17B C 0.63689(13) 0.53017(12) 0.77265(12) 0.0449(6) Uani 1 1 d . D 1 H17G H 0.615 0.5392 0.7254 0.067 Uiso 0.5 1 calc PR D 1 H17H H 0.6479 0.4888 0.7761 0.067 Uiso 0.5 1 calc PR D 1 H17I H 0.6862 0.5518 0.7816 0.067 Uiso 0.5 1 calc PR D 1 H17J H 0.6844 0.514 0.7966 0.067 Uiso 0.5 1 calc PR D 1 H17K H 0.6515 0.5644 0.7459 0.067 Uiso 0.5 1 calc PR D 1 H17L H 0.6132 0.5014 0.7404 0.067 Uiso 0.5 1 calc PR D 1 C18B C 0.36879(12) 0.60926(11) 0.83939(12) 0.0409(5) Uani 1 1 d . D 1 H18G H 0.3629 0.6139 0.7882 0.061 Uiso 0.5 1 calc PR D 1 H18H H 0.3623 0.6467 0.8622 0.061 Uiso 0.5 1 calc PR D 1 H18I H 0.3283 0.5825 0.8553 0.061 Uiso 0.5 1 calc PR D 1 H18J H 0.3394 0.6149 0.8822 0.061 Uiso 0.5 1 calc PR D 1 H18K H 0.3401 0.582 0.8083 0.061 Uiso 0.5 1 calc PR D 1 H18L H 0.374 0.6462 0.8151 0.061 Uiso 0.5 1 calc PR D 1 C19B C 0.23092(15) 0.62905(15) 0.55135(16) 0.0655(8) Uani 1 1 d . D 1 H19D H 0.2419 0.5877 0.5539 0.098 Uiso 1 1 calc R D 1 H19E H 0.1864 0.636 0.5176 0.098 Uiso 1 1 calc R D 1 H19F H 0.2172 0.6431 0.5979 0.098 Uiso 1 1 calc R D 1 C20B C 0.35018(17) 0.63969(13) 0.43603(12) 0.0538(7) Uani 1 1 d . D 1 H20D H 0.4017 0.656 0.4248 0.081 Uiso 1 1 calc R D 1 H20E H 0.3103 0.6506 0.3995 0.081 Uiso 1 1 calc R D 1 H20F H 0.3543 0.5976 0.4382 0.081 Uiso 1 1 calc R D 1 C21B C 0.29665(19) 0.74540(12) 0.51007(17) 0.0691(9) Uani 1 1 d . D 1 H21D H 0.2787 0.7614 0.5544 0.104 Uiso 1 1 calc R D 1 H21E H 0.2545 0.7497 0.4733 0.104 Uiso 1 1 calc R D 1 H21F H 0.3442 0.766 0.4961 0.104 Uiso 1 1 calc R D 1 C22B C 0.48607(18) 0.74756(13) 0.84659(13) 0.0586(7) Uani 1 1 d . D 1 H22D H 0.4663 0.7154 0.8742 0.088 Uiso 1 1 calc R D 1 H22E H 0.4416 0.7661 0.8206 0.088 Uiso 1 1 calc R D 1 H22F H 0.5123 0.7757 0.8782 0.088 Uiso 1 1 calc R D 1 C23B C 0.59837(14) 0.78391(10) 0.73554(12) 0.0404(5) Uani 1 1 d . D 1 H23D H 0.6316 0.807 0.7683 0.061 Uiso 1 1 calc R D 1 H23E H 0.554 0.8074 0.7168 0.061 Uiso 1 1 calc R D 1 H23F H 0.6302 0.7708 0.6967 0.061 Uiso 1 1 calc R D 1 C24B C 0.64410(17) 0.68714(11) 0.83545(14) 0.0579(8) Uani 1 1 d . D 1 H24D H 0.6808 0.669 0.8035 0.087 Uiso 1 1 calc R D 1 H24E H 0.624 0.658 0.8675 0.087 Uiso 1 1 calc R D 1 H24F H 0.6721 0.7172 0.8628 0.087 Uiso 1 1 calc R D 1 C25B C 0.47986(15) 0.42148(10) 0.67183(13) 0.0447(5) Uani 1 1 d . D 1 H25D H 0.4837 0.4333 0.6226 0.067 Uiso 1 1 calc R D 1 H25E H 0.4583 0.3823 0.6737 0.067 Uiso 1 1 calc R D 1 H25F H 0.5327 0.4223 0.6953 0.067 Uiso 1 1 calc R D 1 C26B C 0.41187(16) 0.45381(10) 0.81258(12) 0.0451(6) Uani 1 1 d . D 1 H26D H 0.4649 0.4598 0.8345 0.068 Uiso 1 1 calc R D 1 H26E H 0.3963 0.4135 0.8181 0.068 Uiso 1 1 calc R D 1 H26F H 0.3737 0.4787 0.8354 0.068 Uiso 1 1 calc R D 1 C27B C 0.30809(13) 0.46520(12) 0.68318(13) 0.0454(6) Uani 1 1 d . D 1 H27D H 0.2751 0.4931 0.7072 0.068 Uiso 1 1 calc R D 1 H27E H 0.2888 0.4262 0.692 0.068 Uiso 1 1 calc R D 1 H27F H 0.3051 0.4729 0.6324 0.068 Uiso 1 1 calc R D 1 C28B C 0.31916(13) 0.40775(11) 0.48509(12) 0.0428(5) Uani 1 1 d . C 1 S1' S -0.1218(3) 0.4697(2) -0.0333(3) 0.0305(16) Uiso 0.104(2) 1 d P A 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 Mg 0.0304(3) 0.0277(3) 0.0221(3) -0.0048(3) 0.0004(3) -0.0015(3) S 0.0289(3) 0.0346(3) 0.0279(3) -0.0088(2) -0.0002(2) -0.0030(2) Si1 0.0343(3) 0.0230(3) 0.0246(2) 0.0002(2) -0.0087(2) -0.0018(2) Si2 0.0404(3) 0.0261(3) 0.0287(3) -0.0022(2) -0.0102(2) -0.0044(2) Si3 0.0311(3) 0.0459(4) 0.0295(3) -0.0052(3) -0.0099(2) 0.0022(3) Si4 0.0353(3) 0.0252(3) 0.0282(3) -0.0025(2) 0.0064(2) -0.0039(2) F1 0.0605(10) 0.0811(13) 0.0814(11) -0.0495(10) -0.0013(9) -0.0246(9) F2 0.0466(9) 0.1384(18) 0.0705(11) -0.0352(11) 0.0243(8) -0.0426(10) F3 0.0615(11) 0.1166(18) 0.0765(12) -0.0048(12) -0.0237(9) 0.0243(11) O1 0.0346(7) 0.0406(9) 0.0338(7) -0.0139(7) 0.0022(6) -0.0053(6) O2 0.0309(7) 0.0549(10) 0.0387(8) -0.0142(7) 0.0061(6) -0.0067(7) O3 0.0902(14) 0.0517(12) 0.0479(10) -0.0002(9) -0.0034(10) 0.0146(10) N1 0.0273(8) 0.0314(9) 0.0236(7) -0.0016(6) -0.0031(6) -0.0002(6) N2 0.0292(8) 0.0243(8) 0.0251(7) -0.0017(6) 0.0016(6) -0.0010(6) C1 0.0265(9) 0.0300(10) 0.0229(8) -0.0004(7) -0.0020(7) 0.0016(7) C2 0.0401(11) 0.0280(10) 0.0343(10) -0.0021(8) -0.0174(9) 0.0048(8) C3 0.0643(15) 0.0335(12) 0.0415(12) 0.0106(10) -0.0220(12) -0.0060(11) C4 0.099(2) 0.0349(15) 0.0725(19) 0.0166(14) -0.0402(18) -0.0026(15) C5 0.100(3) 0.0293(14) 0.108(3) 0.0035(17) -0.054(2) 0.0079(16) C6 0.0679(18) 0.0462(17) 0.092(2) -0.0267(16) -0.0386(18) 0.0286(15) C7 0.0432(13) 0.0426(14) 0.0548(14) -0.0133(11) -0.0205(11) 0.0148(11) C8 0.0406(13) 0.074(2) 0.0698(18) -0.0293(16) -0.0012(13) 0.0137(13) C9 0.0738(18) 0.0559(17) 0.0409(13) 0.0139(12) 0.0023(13) -0.0158(14) C10 0.0230(8) 0.0265(9) 0.0213(8) -0.0026(7) 0.0032(7) 0.0008(7) C11 0.0321(9) 0.0245(9) 0.0235(8) -0.0003(7) -0.0003(7) -0.0032(7) C12 0.0480(12) 0.0304(11) 0.0259(9) -0.0059(8) 0.0070(9) -0.0105(9) C13 0.086(2) 0.0429(14) 0.0219(10) -0.0040(9) 0.0050(11) -0.0270(13) C14 0.086(2) 0.0519(16) 0.0330(12) 0.0137(11) -0.0257(13) -0.0281(15) C15 0.0536(14) 0.0414(14) 0.0549(15) 0.0170(11) -0.0237(12) -0.0101(11) C16 0.0352(11) 0.0319(11) 0.0393(11) 0.0064(9) -0.0061(9) -0.0034(8) C17 0.0341(11) 0.0509(15) 0.0641(16) 0.0069(12) 0.0071(11) 0.0083(10) C18 0.0513(14) 0.0426(14) 0.0546(14) -0.0110(11) 0.0271(12) -0.0029(11) C19 0.0546(15) 0.077(2) 0.0291(11) -0.0026(12) -0.0046(11) 0.0031(14) C20 0.0359(13) 0.098(2) 0.0554(16) -0.0097(16) -0.0039(12) -0.0138(14) C21 0.0744(19) 0.0618(19) 0.0757(19) -0.0108(16) -0.0507(17) 0.0234(15) C22 0.0795(18) 0.0458(15) 0.0370(12) -0.0136(11) 0.0083(12) -0.0116(13) C23 0.0505(13) 0.0329(12) 0.0470(13) 0.0006(10) -0.0074(11) -0.0102(10) C24 0.0649(16) 0.0399(14) 0.0636(16) 0.0051(12) -0.0401(14) -0.0112(12) C25 0.0543(14) 0.0326(12) 0.0565(15) 0.0005(11) 0.0155(12) 0.0047(10) C26 0.0591(14) 0.0298(11) 0.0332(11) 0.0014(9) 0.0083(10) -0.0105(10) C27 0.0448(12) 0.0437(13) 0.0406(12) -0.0035(10) 0.0046(10) -0.0152(10) C28 0.0358(12) 0.074(2) 0.0593(16) -0.0280(15) 0.0065(12) -0.0160(13) Mg1B 0.0277(3) 0.0256(3) 0.0226(3) -0.0036(2) -0.0005(2) 0.0004(2) S1B 0.0290(2) 0.0352(3) 0.0262(2) -0.0081(2) 0.00126(19) -0.0039(2) Si1B 0.0311(3) 0.0233(3) 0.0226(2) 0.0001(2) -0.0060(2) -0.0021(2) Si2B 0.0429(3) 0.0276(3) 0.0268(3) -0.0022(2) -0.0093(2) -0.0054(2) Si3B 0.0317(3) 0.0346(3) 0.0329(3) -0.0030(2) -0.0113(2) 0.0032(2) Si4B 0.0360(3) 0.0255(3) 0.0312(3) -0.0009(2) 0.0048(2) -0.0047(2) F1B 0.0754(11) 0.0500(9) 0.0634(10) 0.0049(8) 0.0057(8) -0.0180(8) F2B 0.0626(9) 0.0689(11) 0.0634(9) -0.0364(8) 0.0111(8) -0.0312(8) F3B 0.0336(7) 0.0800(12) 0.0757(11) -0.0205(9) 0.0147(7) -0.0151(7) O1B 0.0329(7) 0.0364(8) 0.0297(7) -0.0111(6) 0.0029(6) -0.0056(6) O2B 0.0594(10) 0.0557(11) 0.0323(8) -0.0037(8) -0.0062(7) 0.0040(9) O3B 0.0291(7) 0.0411(9) 0.0395(8) -0.0103(7) 0.0068(6) -0.0024(6) N1B 0.0263(7) 0.0270(8) 0.0247(7) -0.0013(6) -0.0037(6) 0.0008(6) N2B 0.0285(8) 0.0231(8) 0.0241(7) -0.0007(6) 0.0008(6) -0.0001(6) C1B 0.0253(8) 0.0266(9) 0.0233(8) 0.0011(7) -0.0004(7) -0.0001(7) C2B 0.0363(10) 0.0265(10) 0.0345(10) 0.0019(8) -0.0146(9) -0.0007(8) C3B 0.0527(14) 0.0421(13) 0.0456(13) 0.0183(11) -0.0242(11) -0.0125(11) C4B 0.086(2) 0.0432(16) 0.084(2) 0.0341(16) -0.0477(19) -0.0244(16) C5B 0.102(3) 0.0272(14) 0.129(3) 0.0105(18) -0.067(3) 0.0006(17) C6B 0.078(2) 0.0366(15) 0.095(2) -0.0232(16) -0.0442(19) 0.0228(14) C7B 0.0464(13) 0.0353(12) 0.0553(14) -0.0122(11) -0.0227(11) 0.0126(10) C8B 0.0431(13) 0.071(2) 0.0661(17) -0.0185(15) 0.0028(13) 0.0184(13) C9B 0.0593(16) 0.085(2) 0.0435(14) 0.0256(14) 0.0007(13) -0.0223(15) C10B 0.0235(8) 0.0253(9) 0.0225(8) -0.0008(7) 0.0009(7) 0.0015(7) C11B 0.0301(9) 0.0252(9) 0.0229(8) 0.0011(7) -0.0006(7) -0.0030(7) C12B 0.0332(10) 0.0298(10) 0.0267(9) -0.0039(8) 0.0013(8) -0.0046(8) C13B 0.0472(12) 0.0467(13) 0.0244(9) -0.0021(9) 0.0060(9) -0.0099(10) C14B 0.0560(14) 0.0429(13) 0.0238(10) 0.0067(9) -0.0070(9) -0.0117(11) C15B 0.0431(12) 0.0377(12) 0.0345(11) 0.0073(9) -0.0098(9) 0.0010(9) C16B 0.0358(10) 0.0296(10) 0.0303(10) 0.0032(8) -0.0041(8) 0.0012(8) C17B 0.0373(12) 0.0551(15) 0.0422(12) -0.0002(11) 0.0006(10) 0.0168(11) C18B 0.0333(11) 0.0508(14) 0.0392(12) -0.0055(10) 0.0067(9) -0.0008(10) C19B 0.0345(12) 0.098(3) 0.0635(17) -0.0010(17) -0.0085(12) -0.0145(14) C20B 0.0673(17) 0.0618(18) 0.0311(11) 0.0017(11) -0.0120(11) 0.0119(14) C21B 0.0796(19) 0.0448(16) 0.078(2) -0.0097(14) -0.0526(17) 0.0199(14) C22B 0.083(2) 0.0554(17) 0.0379(13) -0.0171(12) 0.0102(13) -0.0120(15) C23B 0.0467(12) 0.0320(11) 0.0414(12) 0.0014(9) -0.0107(10) -0.0092(9) C24B 0.0692(17) 0.0404(14) 0.0602(16) 0.0093(12) -0.0421(14) -0.0114(12) C25B 0.0555(14) 0.0282(11) 0.0512(14) -0.0023(10) 0.0107(11) 0.0033(10) C26B 0.0641(15) 0.0336(12) 0.0378(12) 0.0056(10) 0.0049(11) -0.0116(11) C27B 0.0392(12) 0.0555(15) 0.0422(12) -0.0081(11) 0.0082(10) -0.0140(11) C28B 0.0381(12) 0.0478(14) 0.0427(12) -0.0149(11) 0.0045(10) -0.0122(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg O1 1.9909(15) . ? Mg O2 1.9930(16) 3_565 ? Mg N2 2.0419(16) . ? Mg N1 2.0451(18) . ? Mg C10 2.7942(18) . ? Mg C1 2.798(2) . ? Mg Si1 3.1774(8) . ? S O3 1.417(2) . ? S O2 1.4365(16) . ? S O1 1.4643(15) . ? S C28 1.816(2) . ? Si1 C10 1.8499(19) . ? Si1 C1 1.8594(18) . ? Si1 Si2 2.3341(8) . ? Si2 C22 1.870(3) . ? Si2 C24 1.873(2) . ? Si2 C23 1.874(2) . ? Si3 N1 1.7769(16) . ? Si3 C20 1.858(3) . ? Si3 C19 1.860(2) . ? Si3 C21 1.863(3) . ? Si4 N2 1.7748(17) . ? Si4 C26 1.865(2) . ? Si4 C25 1.865(2) . ? Si4 C27 1.868(2) . ? F1 C28 1.316(3) . ? F2 C28 1.302(3) . ? F3 C28 1.356(4) . ? O2 Mg 1.9930(16) 3_565 ? N1 C1 1.324(2) . ? N2 C10 1.332(2) . ? C1 C2 1.511(3) . ? C2 C7 1.400(3) . ? C2 C3 1.405(3) . ? C3 C4 1.392(4) . ? C3 C9 1.500(4) . ? C4 C5 1.362(5) . ? C5 C6 1.377(5) . ? C6 C7 1.407(4) . ? C7 C8 1.503(4) . ? C10 C11 1.509(2) . ? C11 C12 1.398(3) . ? C11 C16 1.406(3) . ? C12 C13 1.403(3) . ? C12 C18 1.510(3) . ? C13 C14 1.363(4) . ? C14 C15 1.387(4) . ? C15 C16 1.396(3) . ? C16 C17 1.505(3) . ? Mg1B O3B 1.9921(15) 3_666 ? Mg1B O1B 2.0010(15) . ? Mg1B N2B 2.0470(16) . ? Mg1B N1B 2.0489(17) . ? Mg1B C1B 2.806(2) . ? Mg1B C10B 2.8165(18) . ? Mg1B Si1B 3.1875(8) . ? S1B O2B 1.4197(16) . ? S1B O3B 1.4575(15) . ? S1B O1B 1.4601(14) . ? S1B C28B 1.820(2) . ? Si1B C10B 1.8572(19) . ? Si1B C1B 1.8619(18) . ? Si1B Si2B 2.3367(7) . ? Si2B C22B 1.874(3) . ? Si2B C23B 1.875(2) . ? Si2B C24B 1.876(2) . ? Si3B N1B 1.7780(16) . ? Si3B C20B 1.853(3) . ? Si3B C19B 1.860(3) . ? Si3B C21B 1.861(3) . ? Si4B N2B 1.7697(17) . ? Si4B C25B 1.859(2) . ? Si4B C26B 1.863(2) . ? Si4B C27B 1.866(2) . ? F1B C28B 1.319(3) . ? F2B C28B 1.318(3) . ? F3B C28B 1.323(3) . ? O3B Mg1B 1.9921(15) 3_666 ? N1B C1B 1.325(2) . ? N2B C10B 1.329(2) . ? C1B C2B 1.509(3) . ? C2B C7B 1.401(3) . ? C2B C3B 1.407(3) . ? C3B C4B 1.394(4) . ? C3B C9B 1.504(4) . ? C4B C5B 1.371(5) . ? C5B C6B 1.362(5) . ? C6B C7B 1.404(4) . ? C7B C8B 1.498(4) . ? C10B C11B 1.512(2) . ? C11B C16B 1.401(3) . ? C11B C12B 1.402(3) . ? C12B C13B 1.393(3) . ? C12B C18B 1.514(3) . ? C13B C14B 1.379(3) . ? C14B C15B 1.374(3) . ? C15B C16B 1.394(3) . ? C16B C17B 1.505(3) . ? 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 O1 Mg O2 94.68(6) . 3_565 ? O1 Mg N2 117.86(7) . . ? O2 Mg N2 107.37(7) 3_565 . ? O1 Mg N1 115.06(7) . . ? O2 Mg N1 113.52(7) 3_565 . ? N2 Mg N1 107.70(7) . . ? O1 Mg C10 144.46(7) . . ? O2 Mg C10 98.41(6) 3_565 . ? N2 Mg C10 26.61(6) . . ? N1 Mg C10 89.54(6) . . ? O1 Mg C1 141.38(6) . . ? O2 Mg C1 103.31(7) 3_565 . ? N2 Mg C1 89.12(6) . . ? N1 Mg C1 26.32(6) . . ? C10 Mg C1 66.34(5) . . ? O1 Mg Si1 175.42(5) . . ? O2 Mg Si1 89.72(5) 3_565 . ? N2 Mg Si1 61.73(5) . . ? N1 Mg Si1 61.75(5) . . ? C10 Mg Si1 35.36(4) . . ? C1 Mg Si1 35.54(4) . . ? O3 S O2 115.27(11) . . ? O3 S O1 115.81(10) . . ? O2 S O1 112.10(10) . . ? O3 S C28 105.23(14) . . ? O2 S C28 104.28(11) . . ? O1 S C28 102.23(11) . . ? C10 Si1 C1 111.15(9) . . ? C10 Si1 Si2 118.51(6) . . ? C1 Si1 Si2 117.85(7) . . ? C10 Si1 Mg 60.94(6) . . ? C1 Si1 Mg 61.04(6) . . ? Si2 Si1 Mg 177.55(3) . . ? C22 Si2 C24 107.47(14) . . ? C22 Si2 C23 107.29(12) . . ? C24 Si2 C23 107.53(12) . . ? C22 Si2 Si1 117.40(9) . . ? C24 Si2 Si1 108.90(9) . . ? C23 Si2 Si1 107.87(8) . . ? N1 Si3 C20 104.63(11) . . ? N1 Si3 C19 106.60(10) . . ? C20 Si3 C19 109.61(13) . . ? N1 Si3 C21 119.06(10) . . ? C20 Si3 C21 108.65(16) . . ? C19 Si3 C21 108.05(15) . . ? N2 Si4 C26 118.88(9) . . ? N2 Si4 C25 106.53(10) . . ? C26 Si4 C25 109.03(12) . . ? N2 Si4 C27 105.26(10) . . ? C26 Si4 C27 105.96(11) . . ? C25 Si4 C27 111.12(12) . . ? S O1 Mg 142.32(10) . . ? S O2 Mg 145.23(11) . 3_565 ? C1 N1 Si3 129.74(14) . . ? C1 N1 Mg 110.47(12) . . ? Si3 N1 Mg 119.66(9) . . ? C10 N2 Si4 128.25(13) . . ? C10 N2 Mg 110.03(12) . . ? Si4 N2 Mg 120.24(8) . . ? N1 C1 C2 120.39(16) . . ? N1 C1 Si1 126.30(15) . . ? C2 C1 Si1 113.23(13) . . ? N1 C1 Mg 43.21(10) . . ? C2 C1 Mg 161.32(13) . . ? Si1 C1 Mg 83.42(7) . . ? C7 C2 C3 121.7(2) . . ? C7 C2 C1 118.9(2) . . ? C3 C2 C1 119.4(2) . . ? C4 C3 C2 118.0(3) . . ? C4 C3 C9 120.0(3) . . ? C2 C3 C9 122.0(2) . . ? C5 C4 C3 121.2(3) . . ? C4 C5 C6 120.7(3) . . ? C5 C6 C7 120.8(3) . . ? C2 C7 C6 117.5(3) . . ? C2 C7 C8 121.2(2) . . ? C6 C7 C8 121.2(3) . . ? N2 C10 C11 119.35(16) . . ? N2 C10 Si1 126.36(14) . . ? C11 C10 Si1 114.19(13) . . ? N2 C10 Mg 43.36(9) . . ? C11 C10 Mg 158.74(13) . . ? Si1 C10 Mg 83.70(6) . . ? C12 C11 C16 120.64(18) . . ? C12 C11 C10 119.88(17) . . ? C16 C11 C10 119.47(17) . . ? C11 C12 C13 118.5(2) . . ? C11 C12 C18 121.80(19) . . ? C13 C12 C18 119.7(2) . . ? C14 C13 C12 121.5(2) . . ? C13 C14 C15 119.8(2) . . ? C14 C15 C16 121.0(2) . . ? C15 C16 C11 118.6(2) . . ? C15 C16 C17 119.2(2) . . ? C11 C16 C17 122.23(19) . . ? F2 C28 F1 110.1(2) . . ? F2 C28 F3 108.0(2) . . ? F1 C28 F3 107.9(2) . . ? F2 C28 S 111.57(19) . . ? F1 C28 S 110.41(19) . . ? F3 C28 S 108.84(19) . . ? O3B Mg1B O1B 95.18(6) 3_666 . ? O3B Mg1B N2B 115.30(7) 3_666 . ? O1B Mg1B N2B 111.76(7) . . ? O3B Mg1B N1B 108.39(7) 3_666 . ? O1B Mg1B N1B 120.39(7) . . ? N2B Mg1B N1B 105.96(7) . . ? O3B Mg1B C1B 100.23(6) 3_666 . ? O1B Mg1B C1B 146.55(6) . . ? N2B Mg1B C1B 88.12(6) . . ? N1B Mg1B C1B 26.22(5) . . ? O3B Mg1B C10B 105.21(6) 3_666 . ? O1B Mg1B C10B 137.85(6) . . ? N2B Mg1B C10B 26.09(6) . . ? N1B Mg1B C10B 87.83(6) . . ? C1B Mg1B C10B 65.36(5) . . ? O3B Mg1B Si1B 90.72(5) 3_666 . ? O1B Mg1B Si1B 172.54(5) . . ? N2B Mg1B Si1B 61.37(5) . . ? N1B Mg1B Si1B 61.55(4) . . ? C1B Mg1B Si1B 35.48(4) . . ? C10B Mg1B Si1B 35.36(4) . . ? O2B S1B O3B 116.03(10) . . ? O2B S1B O1B 115.60(10) . . ? O3B S1B O1B 111.33(8) . . ? O2B S1B C28B 105.52(11) . . ? O3B S1B C28B 103.22(10) . . ? O1B S1B C28B 103.22(9) . . ? C10B Si1B C1B 109.43(8) . . ? C10B Si1B Si2B 117.42(6) . . ? C1B Si1B Si2B 117.14(6) . . ? C10B Si1B Mg1B 61.35(6) . . ? C1B Si1B Mg1B 61.00(6) . . ? Si2B Si1B Mg1B 175.91(3) . . ? C22B Si2B C23B 107.16(12) . . ? C22B Si2B C24B 107.65(14) . . ? C23B Si2B C24B 107.28(11) . . ? C22B Si2B Si1B 117.35(9) . . ? C23B Si2B Si1B 108.09(7) . . ? C24B Si2B Si1B 108.90(9) . . ? N1B Si3B C20B 106.45(10) . . ? N1B Si3B C19B 104.28(11) . . ? C20B Si3B C19B 110.35(14) . . ? N1B Si3B C21B 119.08(10) . . ? C20B Si3B C21B 107.17(14) . . ? C19B Si3B C21B 109.36(16) . . ? N2B Si4B C25B 105.08(9) . . ? N2B Si4B C26B 118.96(9) . . ? C25B Si4B C26B 110.07(12) . . ? N2B Si4B C27B 105.34(10) . . ? C25B Si4B C27B 111.86(11) . . ? C26B Si4B C27B 105.54(11) . . ? S1B O1B Mg1B 145.87(9) . . ? S1B O3B Mg1B 146.75(11) . 3_666 ? C1B N1B Si3B 129.54(14) . . ? C1B N1B Mg1B 110.68(12) . . ? Si3B N1B Mg1B 119.64(8) . . ? C10B N2B Si4B 128.94(13) . . ? C10B N2B Mg1B 111.28(12) . . ? Si4B N2B Mg1B 119.29(8) . . ? N1B C1B C2B 120.48(16) . . ? N1B C1B Si1B 126.18(14) . . ? C2B C1B Si1B 113.27(13) . . ? N1B C1B Mg1B 43.09(9) . . ? C2B C1B Mg1B 160.98(13) . . ? Si1B C1B Mg1B 83.52(7) . . ? C7B C2B C3B 121.1(2) . . ? C7B C2B C1B 119.8(2) . . ? C3B C2B C1B 119.1(2) . . ? C4B C3B C2B 117.9(3) . . ? C4B C3B C9B 120.4(3) . . ? C2B C3B C9B 121.6(2) . . ? C5B C4B C3B 121.2(3) . . ? C6B C5B C4B 120.6(3) . . ? C5B C6B C7B 121.1(3) . . ? C2B C7B C6B 118.0(3) . . ? C2B C7B C8B 121.5(2) . . ? C6B C7B C8B 120.4(3) . . ? N2B C10B C11B 120.73(16) . . ? N2B C10B Si1B 125.68(14) . . ? C11B C10B Si1B 113.57(13) . . ? N2B C10B Mg1B 42.63(9) . . ? C11B C10B Mg1B 162.02(13) . . ? Si1B C10B Mg1B 83.29(6) . . ? C16B C11B C12B 120.55(17) . . ? C16B C11B C10B 120.30(17) . . ? C12B C11B C10B 119.15(16) . . ? C13B C12B C11B 119.03(19) . . ? C13B C12B C18B 119.32(19) . . ? C11B C12B C18B 121.58(17) . . ? C14B C13B C12B 120.8(2) . . ? C15B C14B C13B 119.66(19) . . ? C14B C15B C16B 121.8(2) . . ? C15B C16B C11B 118.18(19) . . ? C15B C16B C17B 119.58(19) . . ? C11B C16B C17B 122.24(18) . . ? F2B C28B F1B 108.2(2) . . ? F2B C28B F3B 109.17(18) . . ? F1B C28B F3B 108.3(2) . . ? F2B C28B S1B 110.22(16) . . ? F1B C28B S1B 111.24(15) . . ? F3B C28B S1B 109.59(18) . . ? #===END