Supplementary Material for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Peter C. Junk' 'Marcus L. Cole' _publ_contact_author_name 'Peter C. Junk' _publ_contact_author_address ; Monash University School of Chemistry Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email Peter.Junk@sci.monash.edu.au _publ_contact_author_fax 61399054597 _publ_contact_author_phone 61399054570 _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Unprecedented pyridyl induced 1,3-silyl migration in metal complexes of the guanidine CyHNC{N(SiMe3)Py}NCy, Py = 2-(6-MeC5H3N) ; data_compound2 _database_code_CSD 203278 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Na(DCCAMPTMS)(DME)2] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H57 N4 Na O4 Si' _chemical_formula_weight 588.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.943(2) _cell_length_b 12.892(3) _cell_length_c 12.249(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.84(3) _cell_angle_gamma 90.00 _cell_volume 1727.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular prisms' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9769 _exptl_absorpt_correction_T_max 0.9883 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10293 _diffrn_reflns_av_R_equivalents 0.1125 _diffrn_reflns_av_sigmaI/netI 0.1641 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 27.92 _reflns_number_total 6179 _reflns_number_gt 3585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack H D (1983), Acta Cryst. A39, 876-881 ; _refine_ls_abs_structure_Flack -0.29(19) _refine_ls_number_reflns 6179 _refine_ls_number_parameters 369 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1371 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.93389(9) 0.09433(10) 0.91740(8) 0.0262(3) Uani 1 1 d . . . Na1 Na 0.68868(11) 0.07849(12) 0.50178(10) 0.0204(3) Uani 1 1 d . . . N1 N 0.4875(2) 0.0928(3) 0.5976(2) 0.0163(6) Uani 1 1 d . . . N2 N 0.6688(2) 0.1055(3) 0.6937(2) 0.0171(7) Uani 1 1 d . . . C1 C 0.5465(3) 0.0969(3) 0.6979(2) 0.0156(7) Uani 1 1 d . . . C7 C 0.7403(3) 0.1214(3) 0.7875(3) 0.0177(9) Uani 1 1 d . . . C4 C 0.2944(3) 0.0766(3) 0.6835(3) 0.0240(9) Uani 1 1 d . . . H4 H 0.2079 0.0714 0.6768 0.029 Uiso 1 1 calc R . . C5 C 0.3647(3) 0.0829(3) 0.5930(3) 0.0202(8) Uani 1 1 d . . . C3 C 0.3542(3) 0.0781(4) 0.7856(3) 0.0267(9) Uani 1 1 d . . . H3 H 0.3081 0.0726 0.8498 0.032 Uiso 1 1 calc R . . N4 N 0.8374(3) 0.0516(2) 0.8086(2) 0.0196(7) Uani 1 1 d . . . N3 N 0.7402(2) 0.1983(3) 0.8566(2) 0.0216(7) Uani 1 1 d . . . C6 C 0.3076(3) 0.0777(4) 0.4785(3) 0.0276(9) Uani 1 1 d . . . H6A H 0.2184 0.0764 0.4827 0.041 Uiso 1 1 calc R . . H6B H 0.3353 0.0146 0.4420 0.041 Uiso 1 1 calc R . . H6C H 0.3324 0.1386 0.4368 0.041 Uiso 1 1 calc R . . C2 C 0.4778(3) 0.0873(3) 0.7942(3) 0.0207(8) Uani 1 1 d . . . H2 H 0.5182 0.0874 0.8640 0.025 Uiso 1 1 calc R . . C9 C 0.7157(3) 0.3820(3) 0.8038(3) 0.0227(9) Uani 1 1 d . . . H9A H 0.7456 0.3693 0.7296 0.027 Uiso 1 1 calc R . . H9B H 0.7871 0.3991 0.8522 0.027 Uiso 1 1 calc R . . C13 C 0.6019(3) 0.3048(3) 0.9580(3) 0.0273(10) Uani 1 1 d . . . H13A H 0.5582 0.2421 0.9823 0.033 Uiso 1 1 calc R . . H13B H 0.6698 0.3185 1.0114 0.033 Uiso 1 1 calc R . . C8 C 0.6549(3) 0.2841(3) 0.8453(3) 0.0219(9) Uani 1 1 d . . . H8 H 0.5869 0.2640 0.7931 0.026 Uiso 1 1 calc R . . C10 C 0.6272(3) 0.4739(3) 0.8004(3) 0.0264(9) Uani 1 1 d . . . H10A H 0.5595 0.4596 0.7471 0.032 Uiso 1 1 calc R . . H10B H 0.6706 0.5368 0.7760 0.032 Uiso 1 1 calc R . . C21 C 1.0634(3) -0.0017(4) 0.9355(3) 0.0382(12) Uani 1 1 d . . . H21A H 1.0305 -0.0696 0.9550 0.057 Uiso 1 1 calc R . . H21B H 1.1200 0.0223 0.9938 0.057 Uiso 1 1 calc R . . H21C H 1.1070 -0.0075 0.8671 0.057 Uiso 1 1 calc R . . C19 C 0.9170(4) -0.1019(3) 0.7049(3) 0.0300(10) Uani 1 1 d . . . H19A H 0.9288 -0.0571 0.6404 0.036 Uiso 1 1 calc R . . H19B H 0.9946 -0.1034 0.7486 0.036 Uiso 1 1 calc R . . C20 C 1.0181(3) 0.2169(4) 0.8861(3) 0.0337(11) Uani 1 1 d . . . H20A H 1.0532 0.2114 0.8137 0.051 Uiso 1 1 calc R . . H20B H 1.0838 0.2277 0.9412 0.051 Uiso 1 1 calc R . . H20C H 0.9613 0.2756 0.8870 0.051 Uiso 1 1 calc R . . C12 C 0.5144(4) 0.3965(3) 0.9564(3) 0.0308(10) Uani 1 1 d . . . H12A H 0.4869 0.4097 1.0314 0.037 Uiso 1 1 calc R . . H12B H 0.4416 0.3796 0.9098 0.037 Uiso 1 1 calc R . . C14 C 0.8168(3) -0.0571(3) 0.7731(3) 0.0244(9) Uani 1 1 d . . . H14 H 0.7428 -0.0545 0.7231 0.029 Uiso 1 1 calc R . . C22 C 0.8601(4) 0.0973(5) 1.0537(3) 0.0444(12) Uani 1 1 d . . . H22A H 0.7790 0.0653 1.0472 0.067 Uiso 1 1 calc R . . H22B H 0.8520 0.1693 1.0779 0.067 Uiso 1 1 calc R . . H22C H 0.9108 0.0587 1.1072 0.067 Uiso 1 1 calc R . . C11 C 0.5752(4) 0.4934(4) 0.9131(3) 0.0309(10) Uani 1 1 d . . . H11A H 0.6420 0.5151 0.9646 0.037 Uiso 1 1 calc R . . H11B H 0.5146 0.5504 0.9080 0.037 Uiso 1 1 calc R . . C15 C 0.7818(4) -0.1280(3) 0.8660(3) 0.0297(10) Uani 1 1 d . . . H15A H 0.8495 -0.1295 0.9216 0.036 Uiso 1 1 calc R . . H15B H 0.7088 -0.0993 0.9009 0.036 Uiso 1 1 calc R . . C18 C 0.8847(4) -0.2109(3) 0.6673(3) 0.0304(10) Uani 1 1 d . . . H18A H 0.9539 -0.2400 0.6270 0.036 Uiso 1 1 calc R . . H18B H 0.8127 -0.2080 0.6165 0.036 Uiso 1 1 calc R . . C17 C 0.8567(4) -0.2825(4) 0.7623(3) 0.0339(11) Uani 1 1 d . . . H17A H 0.8318 -0.3515 0.7339 0.041 Uiso 1 1 calc R . . H17B H 0.9311 -0.2916 0.8096 0.041 Uiso 1 1 calc R . . C16 C 0.7548(4) -0.2369(4) 0.8287(4) 0.0357(11) Uani 1 1 d . . . H16A H 0.6779 -0.2372 0.7838 0.043 Uiso 1 1 calc R . . H16B H 0.7424 -0.2813 0.8934 0.043 Uiso 1 1 calc R . . O1 O 0.6596(2) 0.2096(2) 0.36378(19) 0.0264(6) Uani 1 1 d . . . O2 O 0.8665(2) 0.2038(2) 0.49763(18) 0.0230(6) Uani 1 1 d . . . O4 O 0.8536(2) -0.0342(2) 0.4001(2) 0.0273(7) Uani 1 1 d . . . O3 O 0.6123(2) -0.0847(2) 0.4321(2) 0.0254(7) Uani 1 1 d . . . C26 C 0.9378(3) 0.2142(4) 0.5971(3) 0.0318(11) Uani 1 1 d . . . H26A H 1.0059 0.2619 0.5856 0.048 Uiso 1 1 calc R . . H26B H 0.9700 0.1463 0.6193 0.048 Uiso 1 1 calc R . . H26C H 0.8864 0.2417 0.6544 0.048 Uiso 1 1 calc R . . C25 C 0.8147(3) 0.3005(3) 0.4635(3) 0.0271(10) Uani 1 1 d . . . H25A H 0.8798 0.3536 0.4590 0.032 Uiso 1 1 calc R . . H25B H 0.7549 0.3242 0.5170 0.032 Uiso 1 1 calc R . . C29 C 0.7797(4) -0.0793(3) 0.3143(3) 0.0270(10) Uani 1 1 d . . . H29A H 0.8311 -0.1201 0.2651 0.032 Uiso 1 1 calc R . . H29B H 0.7378 -0.0242 0.2710 0.032 Uiso 1 1 calc R . . C23 C 0.5894(4) 0.1991(4) 0.2646(3) 0.0377(12) Uani 1 1 d . . . H23A H 0.5505 0.2655 0.2460 0.057 Uiso 1 1 calc R . . H23B H 0.5264 0.1460 0.2736 0.057 Uiso 1 1 calc R . . H23C H 0.6431 0.1784 0.2059 0.057 Uiso 1 1 calc R . . C24 C 0.7533(4) 0.2864(3) 0.3547(3) 0.0290(10) Uani 1 1 d . . . H24A H 0.7169 0.3529 0.3295 0.035 Uiso 1 1 calc R . . H24B H 0.8134 0.2639 0.3009 0.035 Uiso 1 1 calc R . . C28 C 0.6874(3) -0.1482(3) 0.3656(3) 0.0276(10) Uani 1 1 d . . . H28A H 0.6366 -0.1833 0.3084 0.033 Uiso 1 1 calc R . . H28B H 0.7292 -0.2019 0.4109 0.033 Uiso 1 1 calc R . . C30 C 0.9586(4) 0.0153(4) 0.3598(3) 0.0362(11) Uani 1 1 d . . . H30A H 1.0066 -0.0350 0.3191 0.054 Uiso 1 1 calc R . . H30B H 1.0085 0.0427 0.4210 0.054 Uiso 1 1 calc R . . H30C H 0.9334 0.0723 0.3112 0.054 Uiso 1 1 calc R . . C27 C 0.5259(4) -0.1461(3) 0.4877(4) 0.0331(11) Uani 1 1 d . . . H27A H 0.4709 -0.1802 0.4343 0.050 Uiso 1 1 calc R . . H27B H 0.4783 -0.1016 0.5354 0.050 Uiso 1 1 calc R . . H27C H 0.5691 -0.1988 0.5319 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0211(5) 0.0373(8) 0.0199(5) 0.0036(6) -0.0032(4) -0.0022(6) Na1 0.0219(7) 0.0215(9) 0.0177(6) -0.0011(7) 0.0023(5) -0.0040(7) N1 0.0189(14) 0.0145(18) 0.0153(13) 0.0022(15) -0.0001(10) -0.0023(15) N2 0.0151(15) 0.0203(19) 0.0156(14) -0.0041(14) -0.0013(11) 0.0010(14) C1 0.0171(17) 0.010(2) 0.0194(16) 0.0008(17) -0.0019(13) 0.0006(17) C7 0.0132(18) 0.026(3) 0.0146(16) 0.0033(16) 0.0046(13) 0.0006(16) C4 0.0151(18) 0.023(3) 0.033(2) 0.004(2) -0.0045(15) -0.0016(19) C5 0.0216(18) 0.012(2) 0.0267(19) 0.0005(18) -0.0024(14) -0.0015(18) C3 0.024(2) 0.035(3) 0.0213(18) 0.003(2) 0.0082(15) -0.006(2) N4 0.0178(16) 0.021(2) 0.0203(15) 0.0025(13) 0.0031(12) 0.0040(14) N3 0.0201(16) 0.027(2) 0.0180(15) -0.0026(15) -0.0008(12) 0.0038(15) C6 0.029(2) 0.027(3) 0.026(2) 0.002(2) -0.0038(15) 0.000(2) C2 0.0276(19) 0.018(2) 0.0159(16) 0.0001(18) -0.0011(13) -0.003(2) C9 0.022(2) 0.029(3) 0.018(2) -0.0037(18) 0.0023(15) -0.0004(18) C13 0.029(2) 0.027(3) 0.026(2) 0.0016(19) 0.0052(16) 0.002(2) C8 0.019(2) 0.023(2) 0.024(2) -0.0078(17) -0.0018(15) -0.0024(18) C10 0.031(2) 0.023(3) 0.026(2) -0.0045(18) 0.0031(16) -0.0035(19) C21 0.023(2) 0.046(3) 0.044(3) 0.016(2) -0.0109(18) -0.008(2) C19 0.036(2) 0.023(3) 0.032(2) -0.0005(19) 0.0065(18) 0.001(2) C20 0.022(2) 0.039(3) 0.040(2) -0.007(2) -0.0050(17) -0.004(2) C12 0.033(2) 0.031(3) 0.029(2) -0.0076(19) 0.0115(17) 0.002(2) C14 0.022(2) 0.019(2) 0.032(2) 0.0027(18) 0.0021(16) -0.0002(18) C22 0.039(2) 0.071(4) 0.023(2) 0.003(3) -0.0042(17) -0.006(3) C11 0.033(2) 0.031(3) 0.029(2) -0.009(2) 0.0005(17) 0.010(2) C15 0.029(2) 0.028(3) 0.033(2) -0.001(2) 0.0130(18) -0.0055(19) C18 0.032(2) 0.029(3) 0.030(2) -0.0046(19) 0.0056(18) 0.004(2) C17 0.037(2) 0.022(3) 0.042(3) -0.003(2) 0.0005(19) 0.000(2) C16 0.032(3) 0.031(3) 0.045(3) 0.001(2) 0.011(2) -0.006(2) O1 0.0272(14) 0.0269(18) 0.0251(14) 0.0032(13) 0.0003(11) -0.0044(14) O2 0.0228(14) 0.0227(17) 0.0234(14) -0.0029(12) -0.0017(10) -0.0035(13) O4 0.0256(15) 0.0305(19) 0.0262(14) -0.0024(13) 0.0045(11) -0.0083(13) O3 0.0230(14) 0.0166(17) 0.0370(16) -0.0044(12) 0.0073(11) 0.0008(12) C26 0.028(2) 0.042(3) 0.025(2) -0.001(2) -0.0007(17) -0.009(2) C25 0.026(2) 0.023(3) 0.033(2) -0.0007(19) 0.0042(18) -0.0017(19) C29 0.030(2) 0.026(3) 0.025(2) -0.0058(19) 0.0008(17) 0.0032(19) C23 0.029(2) 0.056(4) 0.028(2) 0.007(2) -0.0042(17) -0.005(2) C24 0.030(2) 0.021(3) 0.036(2) 0.007(2) 0.0042(19) 0.001(2) C28 0.023(2) 0.029(3) 0.030(2) -0.0111(19) -0.0013(17) -0.0024(19) C30 0.030(2) 0.032(3) 0.047(3) -0.004(2) 0.008(2) -0.004(2) C27 0.029(3) 0.024(3) 0.047(3) -0.003(2) 0.009(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N4 1.761(3) . ? Si1 C22 1.879(4) . ? Si1 C20 1.875(5) . ? Si1 C21 1.890(4) . ? Na1 N2 2.394(3) . ? Na1 O1 2.405(3) . ? Na1 O3 2.410(3) . ? Na1 O2 2.531(3) . ? Na1 N1 2.535(3) . ? Na1 O4 2.658(3) . ? Na1 C1 2.914(3) . ? N1 C5 1.349(4) . ? N1 C1 1.371(4) . ? N2 C1 1.345(4) . ? N2 C7 1.384(4) . ? C1 C2 1.424(4) . ? C7 N3 1.303(5) . ? C7 N4 1.411(4) . ? C4 C5 1.372(5) . ? C4 C3 1.392(5) . ? C5 C6 1.519(4) . ? C3 C2 1.359(4) . ? N4 C14 1.483(5) . ? N3 C8 1.452(5) . ? C9 C8 1.522(5) . ? C9 C10 1.530(5) . ? C13 C12 1.521(6) . ? C13 C8 1.537(5) . ? C10 C11 1.531(5) . ? C19 C18 1.517(6) . ? C19 C14 1.514(5) . ? C12 C11 1.520(6) . ? C14 C15 1.517(5) . ? C15 C16 1.504(6) . ? C18 C17 1.524(6) . ? C17 C16 1.520(5) . ? O1 C23 1.422(4) . ? O1 C24 1.432(5) . ? O2 C25 1.427(5) . ? O2 C26 1.432(4) . ? O4 C30 1.418(4) . ? O4 C29 1.429(4) . ? O3 C27 1.423(4) . ? O3 C28 1.432(4) . ? C25 C24 1.484(5) . ? C29 C28 1.498(5) . ? 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 N4 Si1 C22 114.48(16) . . ? N4 Si1 C20 113.30(17) . . ? C22 Si1 C20 113.1(2) . . ? N4 Si1 C21 108.24(18) . . ? C22 Si1 C21 104.5(2) . . ? C20 Si1 C21 101.8(2) . . ? N2 Na1 O1 125.02(12) . . ? N2 Na1 O3 115.68(11) . . ? O1 Na1 O3 109.18(10) . . ? N2 Na1 O2 91.21(10) . . ? O1 Na1 O2 67.77(9) . . ? O3 Na1 O2 143.92(10) . . ? N2 Na1 N1 55.02(9) . . ? O1 Na1 N1 100.19(10) . . ? O3 Na1 N1 86.05(10) . . ? O2 Na1 N1 130.00(11) . . ? N2 Na1 O4 128.65(10) . . ? O1 Na1 O4 97.56(10) . . ? O3 Na1 O4 65.78(9) . . ? O2 Na1 O4 78.77(9) . . ? N1 Na1 O4 150.43(12) . . ? N2 Na1 C1 27.16(8) . . ? O1 Na1 C1 117.40(11) . . ? O3 Na1 C1 100.06(10) . . ? O2 Na1 C1 113.32(10) . . ? N1 Na1 C1 28.05(8) . . ? O4 Na1 C1 145.03(11) . . ? C5 N1 C1 118.8(3) . . ? C5 N1 Na1 148.5(2) . . ? C1 N1 Na1 91.52(18) . . ? C1 N2 C7 121.1(3) . . ? C1 N2 Na1 98.49(18) . . ? C7 N2 Na1 140.3(2) . . ? N2 C1 N1 114.2(3) . . ? N2 C1 C2 126.2(3) . . ? N1 C1 C2 119.5(3) . . ? N2 C1 Na1 54.35(15) . . ? N1 C1 Na1 60.43(16) . . ? C2 C1 Na1 170.4(3) . . ? N3 C7 N2 129.8(3) . . ? N3 C7 N4 112.4(3) . . ? N2 C7 N4 117.4(3) . . ? C5 C4 C3 117.8(3) . . ? N1 C5 C4 123.7(3) . . ? N1 C5 C6 115.0(3) . . ? C4 C5 C6 121.3(3) . . ? C2 C3 C4 120.5(3) . . ? C7 N4 C14 116.3(3) . . ? C7 N4 Si1 111.7(2) . . ? C14 N4 Si1 126.9(2) . . ? C7 N3 C8 122.1(3) . . ? C3 C2 C1 119.6(3) . . ? C8 C9 C10 111.6(3) . . ? C12 C13 C8 112.3(3) . . ? N3 C8 C9 112.2(3) . . ? N3 C8 C13 107.9(3) . . ? C9 C8 C13 109.7(3) . . ? C9 C10 C11 110.8(3) . . ? C18 C19 C14 110.8(3) . . ? C13 C12 C11 111.2(3) . . ? N4 C14 C15 112.8(3) . . ? N4 C14 C19 114.6(3) . . ? C15 C14 C19 112.9(3) . . ? C12 C11 C10 111.1(3) . . ? C16 C15 C14 112.7(3) . . ? C19 C18 C17 112.3(3) . . ? C16 C17 C18 110.1(4) . . ? C15 C16 C17 112.5(3) . . ? C23 O1 C24 111.6(3) . . ? C23 O1 Na1 126.0(3) . . ? C24 O1 Na1 117.5(2) . . ? C25 O2 C26 111.6(3) . . ? C25 O2 Na1 105.4(2) . . ? C26 O2 Na1 116.2(2) . . ? C30 O4 C29 111.9(3) . . ? C30 O4 Na1 119.2(2) . . ? C29 O4 Na1 100.9(2) . . ? C27 O3 C28 110.9(3) . . ? C27 O3 Na1 123.0(2) . . ? C28 O3 Na1 120.1(2) . . ? O2 C25 C24 108.7(3) . . ? O4 C29 C28 107.8(3) . . ? O1 C24 C25 108.7(3) . . ? O3 C28 C29 107.8(3) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.330 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.084 #===END data_Compound_4 _database_code_CSD 203279 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [AlCl2(AMPTMSDCC)] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H37 Al Cl2 N4 Si' _chemical_formula_weight 483.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.997(6) _cell_length_b 9.1761(18) _cell_length_c 21.752(4) _cell_angle_alpha 90.00 _cell_angle_beta 125.82(3) _cell_angle_gamma 90.00 _cell_volume 5178.4(18) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.348 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9337 _exptl_absorpt_correction_T_max 0.9661 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16593 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6305 _reflns_number_gt 4860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6305 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 Cl2 Cl 0.166020(19) 0.16240(5) 0.09649(3) 0.02386(13) Uani 1 1 d . . . Si1 Si 0.13716(2) 0.60235(5) 0.33678(3) 0.01863(14) Uani 1 1 d . . . Cl1 Cl 0.06393(2) 0.06838(5) 0.10766(3) 0.02940(15) Uani 1 1 d . . . Al1 Al 0.11757(2) 0.23359(5) 0.12776(3) 0.01517(14) Uani 1 1 d . . . N4 N 0.13787(6) 0.42064(14) 0.30887(8) 0.0147(3) Uani 1 1 d . . . N2 N 0.09833(6) 0.50804(15) 0.18854(9) 0.0161(3) Uani 1 1 d . . . N1 N 0.08148(6) 0.40775(15) 0.07395(8) 0.0152(3) Uani 1 1 d . . . N3 N 0.15321(6) 0.30336(15) 0.22521(8) 0.0142(3) Uani 1 1 d . . . C9 C 0.20756(7) 0.08218(18) 0.29279(11) 0.0179(4) Uani 1 1 d . . . H9A H 0.2040 0.0460 0.2470 0.022 Uiso 1 1 calc R . . H9B H 0.1793 0.0401 0.2934 0.022 Uiso 1 1 calc R . . C1 C 0.08483(7) 0.52317(18) 0.11696(10) 0.0145(3) Uani 1 1 d . . . C4 C 0.04183(7) 0.5625(2) -0.03515(11) 0.0222(4) Uani 1 1 d . . . H4 H 0.0257 0.5742 -0.0879 0.027 Uiso 1 1 calc R . . C5 C 0.05824(7) 0.4274(2) -0.00226(11) 0.0189(4) Uani 1 1 d . . . C13 C 0.24777(7) 0.31678(18) 0.29068(11) 0.0176(4) Uani 1 1 d . . . H13A H 0.2449 0.2862 0.2447 0.021 Uiso 1 1 calc R . . H13B H 0.2450 0.4243 0.2900 0.021 Uiso 1 1 calc R . . C11 C 0.30469(7) 0.10308(19) 0.36805(11) 0.0207(4) Uani 1 1 d . . . H11A H 0.3057 0.0636 0.3266 0.025 Uiso 1 1 calc R . . H11B H 0.3374 0.0764 0.4168 0.025 Uiso 1 1 calc R . . C8 C 0.20394(7) 0.24843(17) 0.29041(10) 0.0142(4) Uani 1 1 d . . . H8 H 0.2083 0.2807 0.3378 0.017 Uiso 1 1 calc R . . C7 C 0.12942(7) 0.40836(17) 0.23860(10) 0.0140(4) Uani 1 1 d . . . C12 C 0.30003(8) 0.26904(19) 0.36137(11) 0.0211(4) Uani 1 1 d . . . H12A H 0.3279 0.3087 0.3591 0.025 Uiso 1 1 calc R . . H12B H 0.3044 0.3096 0.4070 0.025 Uiso 1 1 calc R . . C19 C 0.17123(8) 0.24335(19) 0.41963(11) 0.0208(4) Uani 1 1 d . . . H19A H 0.1729 0.3164 0.4545 0.025 Uiso 1 1 calc R . . H19B H 0.2051 0.2414 0.4278 0.025 Uiso 1 1 calc R . . C14 C 0.12901(7) 0.28535(18) 0.33746(10) 0.0168(4) Uani 1 1 d . . . H14 H 0.1272 0.2040 0.3054 0.020 Uiso 1 1 calc R . . C2 C 0.06923(7) 0.66293(18) 0.08400(11) 0.0188(4) Uani 1 1 d . . . H2 H 0.0729 0.7438 0.1141 0.023 Uiso 1 1 calc R . . C10 C 0.25968(7) 0.03505(19) 0.36395(11) 0.0207(4) Uani 1 1 d . . . H10A H 0.2616 0.0638 0.4094 0.025 Uiso 1 1 calc R . . H10B H 0.2625 -0.0724 0.3642 0.025 Uiso 1 1 calc R . . C3 C 0.04906(7) 0.6830(2) 0.00976(12) 0.0225(4) Uani 1 1 d . . . H3 H 0.0399 0.7779 -0.0117 0.027 Uiso 1 1 calc R . . C6 C 0.05038(8) 0.2954(2) -0.04908(11) 0.0247(4) Uani 1 1 d . . . H6A H 0.0826 0.2721 -0.0426 0.037 Uiso 1 1 calc R . . H6B H 0.0234 0.3158 -0.1026 0.037 Uiso 1 1 calc R . . H6C H 0.0400 0.2125 -0.0325 0.037 Uiso 1 1 calc R . . C16 C 0.06441(9) 0.1407(2) 0.34396(13) 0.0312(5) Uani 1 1 d . . . H16A H 0.0318 0.1482 0.3394 0.037 Uiso 1 1 calc R . . H16B H 0.0596 0.0665 0.3072 0.037 Uiso 1 1 calc R . . C15 C 0.07659(8) 0.2890(2) 0.32455(11) 0.0221(4) Uani 1 1 d . . . H15A H 0.0494 0.3133 0.2709 0.026 Uiso 1 1 calc R . . H15B H 0.0768 0.3658 0.3567 0.026 Uiso 1 1 calc R . . C22 C 0.16755(9) 0.6047(2) 0.44056(12) 0.0307(5) Uani 1 1 d . . . H22A H 0.1465 0.5475 0.4510 0.046 Uiso 1 1 calc R . . H22B H 0.1699 0.7054 0.4573 0.046 Uiso 1 1 calc R . . H22C H 0.2022 0.5624 0.4679 0.046 Uiso 1 1 calc R . . C20 C 0.17965(9) 0.7126(2) 0.32264(13) 0.0316(5) Uani 1 1 d . . . H20A H 0.2111 0.6576 0.3406 0.047 Uiso 1 1 calc R . . H20B H 0.1888 0.8038 0.3513 0.047 Uiso 1 1 calc R . . H20C H 0.1615 0.7347 0.2686 0.047 Uiso 1 1 calc R . . C17 C 0.10753(9) 0.0923(2) 0.42399(13) 0.0316(5) Uani 1 1 d . . . H17A H 0.1089 0.1586 0.4611 0.038 Uiso 1 1 calc R . . H17B H 0.1001 -0.0071 0.4329 0.038 Uiso 1 1 calc R . . C18 C 0.15933(9) 0.0926(2) 0.43630(12) 0.0274(5) Uani 1 1 d . . . H18A H 0.1591 0.0194 0.4027 0.033 Uiso 1 1 calc R . . H18B H 0.1867 0.0652 0.4894 0.033 Uiso 1 1 calc R . . C21 C 0.07209(9) 0.6858(2) 0.28873(13) 0.0320(5) Uani 1 1 d . . . H21A H 0.0568 0.6992 0.2348 0.048 Uiso 1 1 calc R . . H21B H 0.0752 0.7805 0.3119 0.048 Uiso 1 1 calc R . . H21C H 0.0500 0.6215 0.2943 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl2 0.0271(3) 0.0253(3) 0.0229(3) -0.00254(18) 0.0167(2) 0.00629(19) Si1 0.0254(3) 0.0120(2) 0.0221(3) -0.00145(19) 0.0159(2) 0.0017(2) Cl1 0.0288(3) 0.0155(2) 0.0379(3) 0.00138(19) 0.0161(2) -0.00581(18) Al1 0.0184(3) 0.0105(3) 0.0173(3) -0.0003(2) 0.0109(2) 0.0012(2) N4 0.0216(8) 0.0093(6) 0.0184(8) 0.0006(6) 0.0147(7) 0.0013(6) N2 0.0203(8) 0.0113(7) 0.0201(8) 0.0019(6) 0.0138(7) 0.0027(6) N1 0.0146(7) 0.0147(7) 0.0188(8) 0.0005(6) 0.0112(7) 0.0005(6) N3 0.0179(8) 0.0115(7) 0.0168(8) 0.0012(6) 0.0122(7) 0.0032(6) C9 0.0203(10) 0.0117(8) 0.0241(10) 0.0028(7) 0.0143(8) 0.0015(7) C1 0.0133(8) 0.0114(8) 0.0201(9) 0.0021(7) 0.0105(7) 0.0020(6) C4 0.0189(10) 0.0276(10) 0.0222(10) 0.0088(8) 0.0133(9) 0.0041(8) C5 0.0155(9) 0.0255(9) 0.0190(9) 0.0025(7) 0.0120(8) 0.0002(7) C13 0.0193(9) 0.0141(8) 0.0213(10) 0.0004(7) 0.0129(8) -0.0005(7) C11 0.0181(9) 0.0197(9) 0.0225(10) 0.0002(7) 0.0109(8) 0.0046(7) C8 0.0165(9) 0.0118(8) 0.0155(9) 0.0030(6) 0.0102(8) 0.0036(6) C7 0.0173(9) 0.0090(7) 0.0185(9) -0.0006(6) 0.0120(8) -0.0018(6) C12 0.0181(9) 0.0191(9) 0.0257(10) -0.0020(8) 0.0126(8) 0.0002(7) C19 0.0260(10) 0.0193(9) 0.0219(10) 0.0040(7) 0.0167(9) 0.0038(7) C14 0.0245(10) 0.0096(8) 0.0212(9) 0.0018(7) 0.0161(8) 0.0017(7) C2 0.0182(9) 0.0125(8) 0.0281(10) 0.0034(7) 0.0149(9) 0.0020(7) C10 0.0227(10) 0.0150(8) 0.0257(10) 0.0057(7) 0.0149(9) 0.0058(7) C3 0.0186(10) 0.0205(9) 0.0327(11) 0.0131(8) 0.0175(9) 0.0071(7) C6 0.0259(11) 0.0298(10) 0.0192(10) -0.0002(8) 0.0136(9) 0.0029(9) C16 0.0335(12) 0.0279(11) 0.0352(12) 0.0057(9) 0.0218(11) -0.0069(9) C15 0.0237(10) 0.0219(9) 0.0250(10) 0.0033(8) 0.0167(9) -0.0002(8) C22 0.0458(14) 0.0214(10) 0.0260(11) -0.0036(8) 0.0216(11) 0.0037(9) C20 0.0432(14) 0.0176(9) 0.0406(13) -0.0063(9) 0.0283(12) -0.0093(9) C17 0.0420(14) 0.0268(11) 0.0337(12) 0.0086(9) 0.0264(11) -0.0020(9) C18 0.0407(13) 0.0200(9) 0.0274(11) 0.0078(8) 0.0233(11) 0.0069(9) C21 0.0373(13) 0.0269(11) 0.0360(13) 0.0040(9) 0.0238(11) 0.0161(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl2 Al1 2.1275(8) . ? Si1 N4 1.7791(15) . ? Si1 C20 1.859(2) . ? Si1 C21 1.862(2) . ? Si1 C22 1.864(2) . ? Cl1 Al1 2.1348(8) . ? Al1 N3 1.8369(17) . ? Al1 N1 1.9172(16) . ? N4 C7 1.392(2) . ? N4 C14 1.488(2) . ? N2 C7 1.321(2) . ? N2 C1 1.357(2) . ? N1 C1 1.375(2) . ? N1 C5 1.375(2) . ? N3 C7 1.361(2) . ? N3 C8 1.485(2) . ? C9 C8 1.528(2) . ? C9 C10 1.531(3) . ? C1 C2 1.410(2) . ? C4 C5 1.373(3) . ? C4 C3 1.402(3) . ? C5 C6 1.505(3) . ? C13 C12 1.531(3) . ? C13 C8 1.533(2) . ? C11 C10 1.524(3) . ? C11 C12 1.529(2) . ? C19 C14 1.530(3) . ? C19 C18 1.533(3) . ? C14 C15 1.530(3) . ? C2 C3 1.356(3) . ? C16 C17 1.523(3) . ? C16 C15 1.541(3) . ? C17 C18 1.516(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 N4 Si1 C20 107.28(8) . . ? N4 Si1 C21 115.30(9) . . ? C20 Si1 C21 111.66(11) . . ? N4 Si1 C22 108.80(8) . . ? C20 Si1 C22 106.29(11) . . ? C21 Si1 C22 107.13(11) . . ? N3 Al1 N1 99.16(7) . . ? N3 Al1 Cl2 113.55(6) . . ? N1 Al1 Cl2 110.61(5) . . ? N3 Al1 Cl1 111.44(6) . . ? N1 Al1 Cl1 110.00(6) . . ? Cl2 Al1 Cl1 111.44(3) . . ? C7 N4 C14 115.41(13) . . ? C7 N4 Si1 114.67(11) . . ? C14 N4 Si1 126.56(11) . . ? C7 N2 C1 126.67(15) . . ? C1 N1 C5 119.42(15) . . ? C1 N1 Al1 116.58(12) . . ? C5 N1 Al1 123.54(12) . . ? C7 N3 C8 118.14(14) . . ? C7 N3 Al1 116.52(12) . . ? C8 N3 Al1 125.24(11) . . ? C8 C9 C10 109.41(15) . . ? N2 C1 N1 123.18(14) . . ? N2 C1 C2 117.16(15) . . ? N1 C1 C2 119.41(16) . . ? C5 C4 C3 119.49(18) . . ? C4 C5 N1 121.23(17) . . ? C4 C5 C6 120.81(17) . . ? N1 C5 C6 117.96(16) . . ? C12 C13 C8 110.23(15) . . ? C10 C11 C12 111.50(16) . . ? N3 C8 C9 112.94(14) . . ? N3 C8 C13 110.53(13) . . ? C9 C8 C13 110.93(14) . . ? N2 C7 N3 124.03(16) . . ? N2 C7 N4 114.70(14) . . ? N3 C7 N4 121.24(15) . . ? C11 C12 C13 111.65(15) . . ? C14 C19 C18 109.37(16) . . ? N4 C14 C19 116.37(15) . . ? N4 C14 C15 111.20(14) . . ? C19 C14 C15 110.08(16) . . ? C3 C2 C1 120.60(17) . . ? C11 C10 C9 112.12(15) . . ? C2 C3 C4 119.48(17) . . ? C17 C16 C15 111.43(18) . . ? C14 C15 C16 110.87(16) . . ? C18 C17 C16 111.50(17) . . ? C17 C18 C19 110.93(16) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.932 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.083