# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1547 data_mar799 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Al{Me3SiNC(tBu)CHSiMe3}2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H59 Al N2 Si4' _chemical_formula_weight 527.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 11.360(4) _cell_length_b 20.099(5) _cell_length_c 15.366(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.96(4) _cell_angle_gamma 90.00 _cell_volume 3432(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.020 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6343 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 24.98 _reflns_number_total 6033 _reflns_number_gt 4592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Hydrogen atoms on C2 and C14 were freely refined; other H atoms were riding. 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^)+(0.0425P)^2^+2.1652P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6033 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al Al 0.67976(6) 0.16618(3) 0.21891(5) 0.02329(17) Uani 1 1 d . . . Si1 Si 0.89062(6) 0.13024(4) 0.40670(5) 0.03310(18) Uani 1 1 d . . . Si2 Si 0.84304(6) 0.14325(3) 0.07333(5) 0.02803(17) Uani 1 1 d . . . Si3 Si 0.45331(7) 0.19493(3) 0.30259(5) 0.03381(18) Uani 1 1 d . . . Si4 Si 0.46467(6) -0.05904(3) 0.29251(5) 0.02825(17) Uani 1 1 d . . . N1 N 0.81568(17) 0.11663(9) 0.29488(13) 0.0247(4) Uani 1 1 d . . . N2 N 0.53316(17) 0.14434(9) 0.24405(13) 0.0238(4) Uani 1 1 d . . . C1 C 0.81169(19) 0.07318(11) 0.22996(15) 0.0229(5) Uani 1 1 d . . . C2 C 0.7492(2) 0.10008(11) 0.14396(15) 0.0218(5) Uani 1 1 d . . . H2 H 0.700(2) 0.0674(12) 0.1058(15) 0.023(6) Uiso 1 1 d . . . C3 C 0.8627(2) 0.00214(12) 0.24113(16) 0.0293(5) Uani 1 1 d . . . C4 C 0.8002(3) -0.04229(12) 0.16354(18) 0.0391(6) Uani 1 1 d . . . H4C H 0.8109 -0.0230 0.1071 0.059 Uiso 1 1 calc R . . H4B H 0.7142 -0.0453 0.1637 0.059 Uiso 1 1 calc R . . H4A H 0.8358 -0.0869 0.1704 0.059 Uiso 1 1 calc R . . C5 C 0.9975(2) 0.00549(15) 0.23900(19) 0.0428(7) Uani 1 1 d . . . H5C H 1.0073 0.0240 0.1819 0.064 Uiso 1 1 calc R . . H5B H 1.0320 -0.0394 0.2462 0.064 Uiso 1 1 calc R . . H5A H 1.0390 0.0340 0.2875 0.064 Uiso 1 1 calc R . . C6 C 0.8455(3) -0.02948(13) 0.32813(18) 0.0374(6) Uani 1 1 d . . . H6C H 0.8790 -0.0746 0.3330 0.056 Uiso 1 1 calc R . . H6B H 0.7594 -0.0315 0.3286 0.056 Uiso 1 1 calc R . . H6A H 0.8869 -0.0026 0.3785 0.056 Uiso 1 1 calc R . . C7 C 0.9005(3) 0.22197(15) 0.4176(2) 0.0515(8) Uani 1 1 d . . . H7C H 0.9373 0.2338 0.4791 0.077 Uiso 1 1 calc R . . H7B H 0.8195 0.2412 0.4019 0.077 Uiso 1 1 calc R . . H7A H 0.9498 0.2395 0.3775 0.077 Uiso 1 1 calc R . . C8 C 1.0486(3) 0.09993(16) 0.43862(19) 0.0491(8) Uani 1 1 d . . . H8C H 1.0961 0.1188 0.3982 0.074 Uiso 1 1 calc R . . H8B H 1.0496 0.0513 0.4348 0.074 Uiso 1 1 calc R . . H8A H 1.0833 0.1138 0.4997 0.074 Uiso 1 1 calc R . . C9 C 0.7987(3) 0.09626(16) 0.48362(19) 0.0508(8) Uani 1 1 d . . . H9C H 0.7988 0.0475 0.4809 0.076 Uiso 1 1 calc R . . H9B H 0.7159 0.1126 0.4660 0.076 Uiso 1 1 calc R . . H9A H 0.8329 0.1107 0.5445 0.076 Uiso 1 1 calc R . . C10 C 0.9690(2) 0.19052(14) 0.14463(19) 0.0408(7) Uani 1 1 d . . . H10C H 1.0171 0.2124 0.1068 0.061 Uiso 1 1 calc R . . H10B H 1.0201 0.1598 0.1854 0.061 Uiso 1 1 calc R . . H10A H 0.9359 0.2242 0.1790 0.061 Uiso 1 1 calc R . . C11 C 0.9111(2) 0.08417(14) 0.00324(18) 0.0384(6) Uani 1 1 d . . . H11C H 0.8471 0.0585 -0.0348 0.058 Uiso 1 1 calc R . . H11B H 0.9660 0.0538 0.0419 0.058 Uiso 1 1 calc R . . H11A H 0.9558 0.1093 -0.0339 0.058 Uiso 1 1 calc R . . C12 C 0.7419(3) 0.19846(15) -0.00689(19) 0.0477(8) Uani 1 1 d . . . H12C H 0.7892 0.2221 -0.0437 0.072 Uiso 1 1 calc R . . H12B H 0.7034 0.2308 0.0260 0.072 Uiso 1 1 calc R . . H12A H 0.6801 0.1715 -0.0451 0.072 Uiso 1 1 calc R . . C13 C 0.48596(19) 0.07881(11) 0.21872(15) 0.0215(5) Uani 1 1 d . . . C14 C 0.5147(2) 0.02791(11) 0.27623(16) 0.0233(5) Uani 1 1 d . . . H14 H 0.566(2) 0.0414(12) 0.3296(16) 0.029(7) Uiso 1 1 d . . . C15 C 0.4016(2) 0.07342(11) 0.12576(15) 0.0249(5) Uani 1 1 d . . . C16 C 0.4075(2) 0.00406(12) 0.08611(16) 0.0302(6) Uani 1 1 d . . . H16C H 0.3817 -0.0291 0.1251 0.045 Uiso 1 1 calc R . . H16B H 0.4903 -0.0054 0.0807 0.045 Uiso 1 1 calc R . . H16A H 0.3542 0.0022 0.0272 0.045 Uiso 1 1 calc R . . C17 C 0.2707(2) 0.08724(14) 0.13327(18) 0.0361(6) Uani 1 1 d . . . H17C H 0.2182 0.0851 0.0740 0.054 Uiso 1 1 calc R . . H17B H 0.2654 0.1316 0.1586 0.054 Uiso 1 1 calc R . . H17A H 0.2451 0.0538 0.1719 0.054 Uiso 1 1 calc R . . C18 C 0.4343(2) 0.12398(13) 0.05947(17) 0.0347(6) Uani 1 1 d . . . H18C H 0.3797 0.1186 0.0016 0.052 Uiso 1 1 calc R . . H18B H 0.5173 0.1164 0.0531 0.052 Uiso 1 1 calc R . . H18A H 0.4268 0.1692 0.0815 0.052 Uiso 1 1 calc R . . C19 C 0.3453(3) 0.14574(15) 0.3535(2) 0.0446(7) Uani 1 1 d . . . H19C H 0.3066 0.1751 0.3901 0.067 Uiso 1 1 calc R . . H19B H 0.3888 0.1104 0.3908 0.067 Uiso 1 1 calc R . . H19A H 0.2839 0.1259 0.3064 0.067 Uiso 1 1 calc R . . C20 C 0.3672(3) 0.26237(15) 0.2321(2) 0.0601(9) Uani 1 1 d . . . H20C H 0.3057 0.2423 0.1852 0.090 Uiso 1 1 calc R . . H20B H 0.4225 0.2888 0.2049 0.090 Uiso 1 1 calc R . . H20A H 0.3284 0.2912 0.2692 0.090 Uiso 1 1 calc R . . C21 C 0.5546(3) 0.23886(16) 0.3967(2) 0.0559(9) Uani 1 1 d . . . H21C H 0.5065 0.2677 0.4271 0.084 Uiso 1 1 calc R . . H21B H 0.6130 0.2659 0.3734 0.084 Uiso 1 1 calc R . . H21A H 0.5974 0.2060 0.4387 0.084 Uiso 1 1 calc R . . C22 C 0.5321(3) -0.07881(15) 0.41127(19) 0.0523(8) Uani 1 1 d . . . H22C H 0.6199 -0.0754 0.4211 0.078 Uiso 1 1 calc R . . H22B H 0.5097 -0.1241 0.4248 0.078 Uiso 1 1 calc R . . H22A H 0.5020 -0.0473 0.4501 0.078 Uiso 1 1 calc R . . C23 C 0.5165(3) -0.12636(12) 0.22521(19) 0.0418(7) Uani 1 1 d . . . H23C H 0.4885 -0.1168 0.1618 0.063 Uiso 1 1 calc R . . H23B H 0.4837 -0.1692 0.2394 0.063 Uiso 1 1 calc R . . H23A H 0.6047 -0.1284 0.2392 0.063 Uiso 1 1 calc R . . C24 C 0.2982(2) -0.06570(14) 0.2808(2) 0.0446(7) Uani 1 1 d . . . H24C H 0.2726 -0.0378 0.3258 0.067 Uiso 1 1 calc R . . H24B H 0.2764 -0.1121 0.2890 0.067 Uiso 1 1 calc R . . H24A H 0.2581 -0.0507 0.2213 0.067 Uiso 1 1 calc R . . C25 C 0.6944(2) 0.26396(10) 0.20403(17) 0.0290(6) Uani 1 1 d . . . H25A H 0.7731 0.2742 0.1907 0.044 Uiso 0.71(3) 1 calc PR . . H25B H 0.6866 0.2865 0.2591 0.044 Uiso 0.71(3) 1 calc PR . . H25C H 0.6307 0.2793 0.1550 0.044 Uiso 0.71(3) 1 calc PR . . H25D H 0.6205 0.2858 0.2125 0.044 Uiso 0.29(3) 1 calc PR . . H25E H 0.7070 0.2735 0.1441 0.044 Uiso 0.29(3) 1 calc PR . . H25F H 0.7629 0.2807 0.2482 0.044 Uiso 0.29(3) 1 calc PR . . 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 Al 0.0237(4) 0.0167(3) 0.0310(4) -0.0015(3) 0.0092(3) -0.0016(3) Si1 0.0341(4) 0.0383(4) 0.0261(4) -0.0036(3) 0.0046(3) -0.0076(3) Si2 0.0268(4) 0.0278(4) 0.0317(4) 0.0025(3) 0.0113(3) -0.0020(3) Si3 0.0344(4) 0.0244(4) 0.0468(4) -0.0064(3) 0.0181(3) 0.0047(3) Si4 0.0319(4) 0.0199(3) 0.0338(4) 0.0042(3) 0.0088(3) -0.0011(3) N1 0.0231(10) 0.0235(10) 0.0280(11) -0.0016(8) 0.0064(8) -0.0042(8) N2 0.0251(10) 0.0154(9) 0.0330(11) -0.0028(8) 0.0112(9) 0.0006(8) C1 0.0167(11) 0.0234(12) 0.0301(12) -0.0009(10) 0.0081(9) -0.0027(9) C2 0.0194(11) 0.0217(12) 0.0245(12) -0.0015(10) 0.0055(9) -0.0021(10) C3 0.0298(13) 0.0245(12) 0.0334(13) 0.0018(11) 0.0059(11) 0.0075(11) C4 0.0449(16) 0.0233(13) 0.0467(16) -0.0023(12) 0.0037(13) 0.0098(12) C5 0.0304(15) 0.0490(17) 0.0492(17) 0.0022(14) 0.0083(13) 0.0144(13) C6 0.0431(16) 0.0265(13) 0.0424(16) 0.0092(12) 0.0087(13) 0.0059(12) C7 0.059(2) 0.0466(18) 0.0459(18) -0.0172(14) 0.0026(15) -0.0141(15) C8 0.0421(17) 0.063(2) 0.0369(16) -0.0007(14) -0.0052(13) -0.0068(15) C9 0.063(2) 0.059(2) 0.0362(16) -0.0075(14) 0.0226(15) -0.0110(16) C10 0.0367(15) 0.0392(16) 0.0502(17) -0.0082(13) 0.0176(13) -0.0119(12) C11 0.0386(15) 0.0436(16) 0.0375(15) -0.0044(12) 0.0185(12) -0.0047(13) C12 0.0482(17) 0.0506(18) 0.0475(17) 0.0218(14) 0.0176(14) 0.0075(14) C13 0.0169(11) 0.0210(12) 0.0289(12) -0.0019(9) 0.0101(9) 0.0004(9) C14 0.0219(12) 0.0223(12) 0.0259(12) -0.0029(10) 0.0054(10) 0.0001(9) C15 0.0202(11) 0.0251(12) 0.0289(12) 0.0029(10) 0.0043(10) 0.0009(10) C16 0.0332(14) 0.0304(13) 0.0263(13) -0.0035(11) 0.0043(10) -0.0034(11) C17 0.0235(13) 0.0418(16) 0.0424(15) 0.0000(12) 0.0055(11) 0.0033(11) C18 0.0338(14) 0.0344(14) 0.0333(14) 0.0098(11) 0.0014(11) -0.0030(11) C19 0.0447(17) 0.0459(17) 0.0507(17) -0.0102(14) 0.0275(14) 0.0009(14) C20 0.065(2) 0.0351(17) 0.085(2) 0.0041(16) 0.0260(19) 0.0256(16) C21 0.0560(19) 0.0507(19) 0.068(2) -0.0303(17) 0.0282(17) -0.0023(16) C22 0.071(2) 0.0430(17) 0.0420(17) 0.0140(14) 0.0091(15) -0.0049(16) C23 0.0511(17) 0.0201(13) 0.0554(18) 0.0011(12) 0.0136(14) 0.0054(12) C24 0.0411(16) 0.0381(16) 0.0590(19) 0.0070(14) 0.0204(14) -0.0064(13) C25 0.0331(13) 0.0104(11) 0.0476(15) 0.0003(10) 0.0177(12) -0.0021(10) _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 Al N2 1.839(2) . ? Al C25 1.990(2) . ? Al N1 1.998(2) . ? Al C2 2.022(2) . ? Al C1 2.380(2) . ? Si1 N1 1.774(2) . ? Si1 C7 1.853(3) . ? Si1 C9 1.862(3) . ? Si1 C8 1.862(3) . ? Si2 C12 1.866(3) . ? Si2 C10 1.871(3) . ? Si2 C11 1.874(3) . ? Si2 C2 1.883(2) . ? Si3 N2 1.7333(19) . ? Si3 C19 1.869(3) . ? Si3 C21 1.872(3) . ? Si3 C20 1.879(3) . ? Si4 C24 1.867(3) . ? Si4 C22 1.869(3) . ? Si4 C14 1.870(2) . ? Si4 C23 1.871(3) . ? N1 C1 1.320(3) . ? N2 C13 1.445(3) . ? C1 C2 1.468(3) . ? C1 C3 1.537(3) . ? C3 C6 1.529(3) . ? C3 C5 1.539(3) . ? C3 C4 1.540(4) . ? C13 C14 1.347(3) . ? C13 C15 1.550(3) . ? C15 C16 1.528(3) . ? C15 C18 1.538(3) . ? C15 C17 1.541(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 N2 Al C25 111.15(9) . . ? N2 Al N1 112.47(9) . . ? C25 Al N1 119.12(10) . . ? N2 Al C2 116.10(9) . . ? C25 Al C2 122.12(10) . . ? N1 Al C2 70.12(9) . . ? N2 Al C1 112.45(8) . . ? C25 Al C1 135.86(9) . . ? N1 Al C1 33.67(8) . . ? C2 Al C1 37.86(8) . . ? N1 Si1 C7 104.41(12) . . ? N1 Si1 C9 109.80(12) . . ? C7 Si1 C9 109.82(15) . . ? N1 Si1 C8 116.59(12) . . ? C7 Si1 C8 105.36(15) . . ? C9 Si1 C8 110.46(15) . . ? C12 Si2 C10 112.10(14) . . ? C12 Si2 C11 105.54(14) . . ? C10 Si2 C11 107.55(13) . . ? C12 Si2 C2 108.06(12) . . ? C10 Si2 C2 110.63(12) . . ? C11 Si2 C2 112.92(12) . . ? N2 Si3 C19 111.50(11) . . ? N2 Si3 C21 111.93(12) . . ? C19 Si3 C21 106.14(15) . . ? N2 Si3 C20 112.94(13) . . ? C19 Si3 C20 108.34(15) . . ? C21 Si3 C20 105.58(16) . . ? C24 Si4 C22 106.31(15) . . ? C24 Si4 C14 112.58(12) . . ? C22 Si4 C14 104.76(13) . . ? C24 Si4 C23 108.87(14) . . ? C22 Si4 C23 105.88(14) . . ? C14 Si4 C23 117.55(12) . . ? C1 N1 Si1 140.25(17) . . ? C1 N1 Al 89.24(14) . . ? Si1 N1 Al 130.31(11) . . ? C13 N2 Si3 118.02(14) . . ? C13 N2 Al 117.56(14) . . ? Si3 N2 Al 124.27(11) . . ? N1 C1 C2 111.8(2) . . ? N1 C1 C3 125.3(2) . . ? C2 C1 C3 122.9(2) . . ? N1 C1 Al 57.08(12) . . ? C2 C1 Al 57.75(12) . . ? C3 C1 Al 162.73(16) . . ? C1 C2 Si2 117.55(16) . . ? C1 C2 Al 84.39(14) . . ? Si2 C2 Al 111.08(12) . . ? C6 C3 C1 111.7(2) . . ? C6 C3 C5 110.2(2) . . ? C1 C3 C5 108.1(2) . . ? C6 C3 C4 108.3(2) . . ? C1 C3 C4 110.44(19) . . ? C5 C3 C4 108.0(2) . . ? C14 C13 N2 119.3(2) . . ? C14 C13 C15 124.8(2) . . ? N2 C13 C15 115.84(19) . . ? C13 C14 Si4 139.29(19) . . ? C16 C15 C18 107.6(2) . . ? C16 C15 C17 108.5(2) . . ? C18 C15 C17 107.5(2) . . ? C16 C15 C13 111.18(19) . . ? C18 C15 C13 112.10(19) . . ? C17 C15 C13 109.90(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.297 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.049