# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- ccdc_comp_2.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2012-02-22 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ; ? 2012-02-22 # Formatted by publCIF ; #============================================================================== # # SUBMISSION DETAILS _publ_contact_author_name 'Strohmann, Carsten' _publ_contact_author_address ;Anorganische Chemie, Technische Universit\"at Dortmund, Otto-Hahn-Strasse 6, 44227 Dortmund, Germany ; _publ_contact_author_email mail@carsten-strohmann.de _publ_contact_author_fax '0049 231 755 7062' _publ_contact_author_phone '0049 231 755 3807' _publ_contact_letter ; Please consider this CIF for submission to the Cambridge Crystallographic Data Centre. I certify that all authors have seen and approved of this submission, that all have made significant scientific contributions to the work reported, and that all share responsibility and accountability for the results. This CIF is submitted as part of a journal submission to Chemical Communications Strohmann, Carsten ; #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ; Isolation of Reactive Intermediate in Deprotonation Reaction with Zinc Alkyls ; _publ_section_title_footnote . loop_ _publ_author_name _publ_author_address C.Strohmann ;Anorganische Chemie, Technische Universit\"at Dortmund, Otto-Hahn-Strasse 6, 44227 Dortmund, Germany ; V.P.Colquhoun ;Anorganische Chemie, Technische Universit\"at Dortmund, Otto-Hahn-Strasse 6, 44227 Dortmund, Germany ; C.Unkelbach ;Anorganische Chemie, Technische Universit\"at Dortmund, Otto-Hahn-Strasse 6, 44227 Dortmund, Germany ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 869490' #TrackingRef '- ccdc_comp_2.cif' _audit_creation_date 2012-02-22T11:21:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; adduct of diethylzinc and (tert butylamino)(piperidinomethyl)dimethylsilane ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_hall '-P 2ybc' _chemical_formula_sum 'C16 H38 N2 Si Zn' _chemical_formula_weight 351.94 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# 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 12.126(5) _cell_length_b 10.691(5) _cell_length_c 16.231(7) _cell_angle_alpha 90 _cell_angle_beta 106.918(7) _cell_angle_gamma 90 _cell_volume 2013.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4390 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.99 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1999)' _exptl_absorpt_correction_T_min 0.5151 _exptl_absorpt_correction_T_max 0.7846 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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 'Bruker APEXCCD' _diffrn_measurement_method \w _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_unetI/netI 0.0215 _diffrn_reflns_number 43766 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.99 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 4390 _reflns_number_gt 3869 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus (Bruker, 1999)' _computing_data_reduction 'SAINT-Plus (Bruker, 1999)' _computing_structure_solution 'SHELXS90 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Ortep-3 (Farrugia, 1997) and Schakal 92 (Keller 1992) ; _computing_publication_material 'wingx (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.5125P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4390 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.487 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.051 #----------------------------------------------------------------------------# # 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' 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' Zn Zn 0.2839 1.4301 '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 C1 C 0.32826(14) 1.12558(15) 0.05962(11) 0.0374(3) Uani 1 1 d . . . C2 C 0.29855(18) 1.07622(18) -0.03257(12) 0.0503(4) Uani 1 1 d . . . H2A H 0.323 0.9888 -0.0318 0.075 Uiso 1 1 calc R . . H2B H 0.3385 1.1264 -0.0656 0.075 Uiso 1 1 calc R . . H2C H 0.2151 1.0819 -0.0594 0.075 Uiso 1 1 calc R . . C3 C 0.29125(19) 1.26307(17) 0.05717(15) 0.0581(5) Uani 1 1 d . . . H3A H 0.2084 1.2697 0.0281 0.087 Uiso 1 1 calc R . . H3B H 0.334 1.3123 0.0257 0.087 Uiso 1 1 calc R . . H3C H 0.3077 1.295 0.1161 0.087 Uiso 1 1 calc R . . C4 C 0.45819(15) 1.1157(2) 0.10187(14) 0.0535(5) Uani 1 1 d . . . H4A H 0.4776 1.1509 0.1601 0.08 Uiso 1 1 calc R . . H4B H 0.4988 1.1622 0.0676 0.08 Uiso 1 1 calc R . . H4C H 0.4814 1.0276 0.1051 0.08 Uiso 1 1 calc R . . C5 C 0.28686(18) 1.18070(16) 0.28162(13) 0.0507(5) Uani 1 1 d . . . H5A H 0.3469 1.2392 0.2768 0.076 Uiso 1 1 calc R . . H5B H 0.298 1.1606 0.3424 0.076 Uiso 1 1 calc R . . H5C H 0.2109 1.2191 0.2574 0.076 Uiso 1 1 calc R . . C6 C 0.44075(14) 0.96256(15) 0.27275(11) 0.0401(4) Uani 1 1 d . . . H6A H 0.4548 0.8951 0.2362 0.06 Uiso 1 1 calc R . . H6B H 0.4425 0.9286 0.3292 0.06 Uiso 1 1 calc R . . H6C H 0.5006 1.0266 0.28 0.06 Uiso 1 1 calc R . . C7 C 0.17082(13) 0.93298(14) 0.22773(10) 0.0346(3) Uani 1 1 d . . . H7A H 0.1723 0.928 0.2889 0.041 Uiso 1 1 calc R . . H7B H 0.0986 0.9762 0.1964 0.041 Uiso 1 1 calc R . . C8 C 0.24503(13) 0.72183(15) 0.25919(10) 0.0341(3) Uani 1 1 d . . . H8A H 0.2264 0.7297 0.3144 0.041 Uiso 1 1 calc R . . H8B H 0.3251 0.7514 0.2686 0.041 Uiso 1 1 calc R . . C9 C 0.23758(15) 0.58486(15) 0.23280(12) 0.0417(4) Uani 1 1 d . . . H9A H 0.2902 0.5348 0.2791 0.05 Uiso 1 1 calc R . . H9B H 0.2621 0.5753 0.1801 0.05 Uiso 1 1 calc R . . C10 C 0.11440(16) 0.53663(17) 0.21593(13) 0.0507(5) Uani 1 1 d . . . H10A H 0.1092 0.4493 0.1948 0.061 Uiso 1 1 calc R . . H10B H 0.0922 0.5379 0.27 0.061 Uiso 1 1 calc R . . C11 C 0.03338(16) 0.61995(18) 0.14880(13) 0.0513(5) Uani 1 1 d . . . H11A H 0.0514 0.6119 0.0933 0.062 Uiso 1 1 calc R . . H11B H -0.0471 0.5922 0.1399 0.062 Uiso 1 1 calc R . . C12 C 0.04512(14) 0.75576(17) 0.17713(12) 0.0423(4) Uani 1 1 d . . . H12A H -0.0074 0.8076 0.1319 0.051 Uiso 1 1 calc R . . H12B H 0.0214 0.7644 0.2303 0.051 Uiso 1 1 calc R . . C13 C 0.37078(14) 0.73928(15) 0.08149(11) 0.0388(4) Uani 1 1 d . . . H13A H 0.4251 0.8035 0.0727 0.047 Uiso 1 1 calc R . . H13B H 0.4007 0.7087 0.1414 0.047 Uiso 1 1 calc R . . C14 C 0.3687(2) 0.6303(2) 0.02018(14) 0.0639(6) Uani 1 1 d . . . H14A H 0.3202 0.5631 0.0316 0.096 Uiso 1 1 calc R . . H14B H 0.4473 0.5991 0.029 0.096 Uiso 1 1 calc R . . H14C H 0.3373 0.6589 -0.0394 0.096 Uiso 1 1 calc R . . C15 C 0.06743(15) 0.84706(16) -0.02546(11) 0.0419(4) Uani 1 1 d . . . H15A H 0.0092 0.8761 0.0022 0.05 Uiso 1 1 calc R . . H15B H 0.0786 0.9149 -0.0637 0.05 Uiso 1 1 calc R . . C16 C 0.01954(16) 0.73346(19) -0.08042(12) 0.0488(4) Uani 1 1 d . . . H16A H 0.0795 0.6973 -0.1026 0.073 Uiso 1 1 calc R . . H16B H -0.0463 0.7587 -0.1287 0.073 Uiso 1 1 calc R . . H16C H -0.0055 0.6711 -0.0454 0.073 Uiso 1 1 calc R . . H1N H 0.1973(16) 1.0604(16) 0.0874(11) 0.034(5) Uiso 1 1 d . . . N1 N 0.26566(11) 1.04865(11) 0.10912(8) 0.0298(3) Uani 1 1 d . . . N2 N 0.16547(10) 0.80290(11) 0.19365(8) 0.0306(3) Uani 1 1 d . . . Si Si 0.29611(4) 1.03388(4) 0.22094(3) 0.03045(10) Uani 1 1 d . . . Zn Zn 0.216945(15) 0.819627(16) 0.066778(11) 0.03283(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0378(8) 0.0313(8) 0.0444(9) 0.0043(7) 0.0143(7) -0.0019(6) C2 0.0633(12) 0.0487(10) 0.0420(10) 0.0085(8) 0.0202(9) -0.0030(9) C3 0.0728(14) 0.0310(9) 0.0775(14) 0.0088(9) 0.0330(12) -0.0005(9) C4 0.0383(10) 0.0617(12) 0.0619(12) 0.0089(10) 0.0171(9) -0.0085(8) C5 0.0590(12) 0.0408(10) 0.0468(11) -0.0163(8) 0.0069(9) 0.0025(8) C6 0.0322(8) 0.0384(8) 0.0426(9) -0.0015(7) -0.0005(7) -0.0034(6) C7 0.0332(8) 0.0344(8) 0.0378(8) -0.0010(6) 0.0130(7) 0.0023(6) C8 0.0322(8) 0.0355(8) 0.0315(8) 0.0034(6) 0.0043(6) -0.0039(6) C9 0.0461(10) 0.0327(8) 0.0434(9) 0.0057(7) 0.0084(8) -0.0025(7) C10 0.0547(11) 0.0411(9) 0.0518(11) 0.0055(8) 0.0086(9) -0.0181(8) C11 0.0429(10) 0.0552(11) 0.0488(11) 0.0034(9) 0.0023(8) -0.0221(8) C12 0.0278(8) 0.0507(10) 0.0462(10) 0.0072(8) 0.0074(7) -0.0065(7) C13 0.0423(9) 0.0342(8) 0.0432(9) 0.0048(7) 0.0174(7) 0.0074(7) C14 0.0844(16) 0.0539(12) 0.0564(13) -0.0036(10) 0.0254(11) 0.0275(11) C15 0.0445(9) 0.0376(8) 0.0347(9) -0.0046(7) -0.0024(7) 0.0036(7) C16 0.0481(10) 0.0568(11) 0.0357(9) -0.0111(8) 0.0031(8) -0.0059(9) N1 0.0266(6) 0.0271(6) 0.0337(7) -0.0003(5) 0.0057(5) -0.0006(5) N2 0.0258(6) 0.0324(6) 0.0325(7) 0.0010(5) 0.0066(5) -0.0030(5) Si 0.0304(2) 0.0272(2) 0.0310(2) -0.00570(15) 0.00480(17) -0.00128(15) Zn 0.03251(11) 0.03201(11) 0.03092(11) -0.00144(7) 0.00445(8) 0.00269(7) #----------------------------------------------------------------------------# # 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 C1 N1 1.501(2) . ? C1 C2 1.528(3) . ? C1 C4 1.528(2) . ? C1 C3 1.534(2) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 Si 1.8737(18) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 Si 1.8726(18) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 N2 1.491(2) . ? C7 Si 1.8925(17) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 N2 1.489(2) . ? C8 C9 1.521(2) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.528(2) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.524(3) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.517(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 N2 1.493(2) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.528(3) . ? C13 Zn 2.0040(18) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.519(2) . ? C15 Zn 2.0087(18) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? N1 Si 1.7508(16) . ? N1 Zn 2.5652(16) . ? N1 H1N 0.810(18) . ? N2 Zn 2.3261(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 108.85(13) . . ? N1 C1 C4 109.75(14) . . ? C2 C1 C4 109.52(15) . . ? N1 C1 C3 110.44(14) . . ? C2 C1 C3 108.77(15) . . ? C4 C1 C3 109.50(16) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si C5 H5A 109.5 . . ? Si C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si C6 H6A 109.5 . . ? Si C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 Si 117.33(10) . . ? N2 C7 H7A 108 . . ? Si C7 H7A 108 . . ? N2 C7 H7B 108 . . ? Si C7 H7B 108 . . ? H7A C7 H7B 107.2 . . ? N2 C8 C9 112.73(13) . . ? N2 C8 H8A 109 . . ? C9 C8 H8A 109 . . ? N2 C8 H8B 109 . . ? C9 C8 H8B 109 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 110.51(15) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 108.91(14) . . ? C11 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? C11 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C12 C11 C10 111.01(15) . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108 . . ? N2 C12 C11 112.23(14) . . ? N2 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? N2 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 Zn 114.26(13) . . ? C14 C13 H13A 108.7 . . ? Zn C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? Zn C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 Zn 115.40(12) . . ? C16 C15 H15A 108.4 . . ? Zn C15 H15A 108.4 . . ? C16 C15 H15B 108.4 . . ? Zn C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 N1 Si 128.12(11) . . ? C1 N1 Zn 119.51(9) . . ? Si N1 Zn 98.88(5) . . ? C1 N1 H1N 107.2(13) . . ? Si N1 H1N 110.2(13) . . ? Zn N1 H1N 84.6(12) . . ? C8 N2 C7 109.20(12) . . ? C8 N2 C12 109.16(12) . . ? C7 N2 C12 108.44(12) . . ? C8 N2 Zn 113.09(9) . . ? C7 N2 Zn 105.24(9) . . ? C12 N2 Zn 111.54(10) . . ? N1 Si C6 112.93(7) . . ? N1 Si C5 116.27(8) . . ? C6 Si C5 107.25(9) . . ? N1 Si C7 100.43(7) . . ? C6 Si C7 113.87(8) . . ? C5 Si C7 105.97(9) . . ? C13 Zn C15 139.33(7) . . ? C13 Zn N2 109.99(6) . . ? C15 Zn N2 104.74(7) . . ? C13 Zn N1 104.09(6) . . ? C15 Zn N1 98.50(6) . . ? N2 Zn N1 86.35(4) . . ? _chemical_name_common ;adduct of diethylzinc and (tert butylamino)(piperidinomethyl)dimethylsilane ; # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment '- ccdc_comp_3.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-02-23 at 09:47:25 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.reqdat # CIF files read : compound_3 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 869491' #TrackingRef '- ccdc_comp_3.cif' _audit_creation_date 2012-02-23T09:47:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; (tert-butyl(dimethyl(piperidin-1-ylmethyl)silyl)amino)(ethyl)zinc ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_hall '-P 1' _chemical_formula_sum 'C14 H32 N2 Si Zn' _chemical_formula_weight 321.88 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3337(2) _cell_length_b 9.9823(2) _cell_length_c 11.3766(2) _cell_angle_alpha 100.8621(18) _cell_angle_beta 91.5344(17) _cell_angle_gamma 109.845(2) _cell_volume 870.03(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3799 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.00 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 348 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.469 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5911 _exptl_absorpt_correction_T_max 0.7577 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur S Oxford Diffraction' _diffrn_measurement_method Omega-scan _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_unetI/netI 0.0166 _diffrn_reflns_number 46205 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27 _diffrn_reflns_theta_full 27 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 3799 _reflns_number_gt 3403 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38)' ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Ortep-3 (Farrugia, 1997) and Schakal 92 (Keller 1992) ; _computing_publication_material 'wingx (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0365P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3799 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.022 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0556 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.295 _refine_diff_density_min -0.246 _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' 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' Zn Zn 0.2839 1.4301 '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 C1 C 0.4435(2) 0.89429(16) 0.77826(15) 0.0362(4) Uani 1 1 d . . . H1A H 0.3933 0.8873 0.6974 0.054 Uiso 1 1 calc R . . H1B H 0.5682 0.9217 0.7786 0.054 Uiso 1 1 calc R . . H1C H 0.4166 0.9683 0.8356 0.054 Uiso 1 1 calc R . . C2 C 0.4682(2) 0.73375(17) 0.97262(13) 0.0320(3) Uani 1 1 d . . . H2A H 0.4361 0.801 1.0337 0.048 Uiso 1 1 calc R . . H2B H 0.5921 0.7724 0.9676 0.048 Uiso 1 1 calc R . . H2C H 0.4367 0.6385 0.9948 0.048 Uiso 1 1 calc R . . C3 C 0.01318(17) 0.69844(15) 0.86448(12) 0.0232(3) Uani 1 1 d . . . C4 C -0.14361(19) 0.57831(17) 0.89098(14) 0.0313(3) Uani 1 1 d . . . H4A H -0.1957 0.5066 0.8164 0.047 Uiso 1 1 calc R . . H4B H -0.2271 0.6208 0.9241 0.047 Uiso 1 1 calc R . . H4C H -0.1087 0.5304 0.9494 0.047 Uiso 1 1 calc R . . C5 C -0.0455(2) 0.77764(17) 0.77794(15) 0.0342(4) Uani 1 1 d . . . H5A H 0.0541 0.8555 0.7606 0.051 Uiso 1 1 calc R . . H5B H -0.1271 0.8197 0.8151 0.051 Uiso 1 1 calc R . . H5C H -0.1008 0.7082 0.7029 0.051 Uiso 1 1 calc R . . C6 C 0.0921(2) 0.80768(19) 0.98319(14) 0.0396(4) Uani 1 1 d . . . H6A H 0.1249 0.7576 1.0408 0.059 Uiso 1 1 calc R . . H6B H 0.008 0.8496 1.0161 0.059 Uiso 1 1 calc R . . H6C H 0.1939 0.8856 0.9685 0.059 Uiso 1 1 calc R . . C7 C 0.41674(16) 0.58517(13) 0.70348(11) 0.0182(3) Uani 1 1 d . . . H7A H 0.4281 0.6228 0.6284 0.022 Uiso 1 1 calc R . . H7B H 0.5305 0.5851 0.7308 0.022 Uiso 1 1 calc R . . C8 C 0.31286(17) 0.35926(14) 0.77490(11) 0.0199(3) Uani 1 1 d . . . H8A H 0.2898 0.4126 0.8513 0.024 Uiso 1 1 calc R . . H8B H 0.4325 0.3622 0.7841 0.024 Uiso 1 1 calc R . . C9 C 0.19178(19) 0.20178(14) 0.75060(12) 0.0253(3) Uani 1 1 d . . . H9A H 0.0717 0.1988 0.7475 0.03 Uiso 1 1 calc R . . H9B H 0.2107 0.1558 0.817 0.03 Uiso 1 1 calc R . . C10 C 0.22080(19) 0.11686(14) 0.63214(13) 0.0268(3) Uani 1 1 d . . . H10A H 0.3356 0.1085 0.6387 0.032 Uiso 1 1 calc R . . H10B H 0.1339 0.0174 0.614 0.032 Uiso 1 1 calc R . . C11 C 0.20788(18) 0.19448(14) 0.53115(12) 0.0235(3) Uani 1 1 d . . . H11A H 0.2377 0.144 0.456 0.028 Uiso 1 1 calc R . . H11B H 0.0885 0.1906 0.5173 0.028 Uiso 1 1 calc R . . C12 C 0.32736(17) 0.35201(13) 0.56194(11) 0.0189(3) Uani 1 1 d . . . H12A H 0.4474 0.3554 0.5686 0.023 Uiso 1 1 calc R . . H12B H 0.3135 0.4006 0.4961 0.023 Uiso 1 1 calc R . . C13 C -0.15261(18) 0.34152(16) 0.56989(14) 0.0288(3) Uani 1 1 d . . . H13A H -0.226 0.3993 0.5597 0.035 Uiso 1 1 calc R . . H13B H -0.1138 0.3142 0.4904 0.035 Uiso 1 1 calc R . . C14 C -0.2625(2) 0.20248(17) 0.60668(17) 0.0405(4) Uani 1 1 d . . . H14A H -0.1955 0.139 0.6091 0.061 Uiso 1 1 calc R . . H14B H -0.3634 0.1519 0.5481 0.061 Uiso 1 1 calc R . . H14C H -0.2994 0.227 0.6864 0.061 Uiso 1 1 calc R . . N1 N 0.13577(13) 0.63397(11) 0.80918(10) 0.0195(2) Uani 1 1 d . . . N2 N 0.29307(13) 0.43243(11) 0.67657(9) 0.0148(2) Uani 1 1 d . . . Si Si 0.35228(4) 0.71334(4) 0.82261(3) 0.01884(9) Uani 1 1 d . . . Zn Zn 0.050513(18) 0.467815(15) 0.680516(13) 0.01833(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0375(9) 0.0200(7) 0.0464(10) 0.0050(7) 0.0045(7) 0.0053(6) C2 0.0309(8) 0.0362(8) 0.0238(8) -0.0067(6) -0.0066(6) 0.0131(7) C3 0.0251(7) 0.0281(7) 0.0220(7) 0.0052(6) 0.0058(6) 0.0162(6) C4 0.0284(8) 0.0400(8) 0.0363(9) 0.0164(7) 0.0136(7) 0.0203(7) C5 0.0394(9) 0.0390(8) 0.0388(9) 0.0176(7) 0.0120(7) 0.0265(7) C6 0.0439(10) 0.0475(10) 0.0305(9) -0.0057(7) 0.0065(7) 0.0274(8) C7 0.0150(6) 0.0187(6) 0.0196(7) 0.0039(5) 0.0024(5) 0.0041(5) C8 0.0223(7) 0.0236(6) 0.0153(6) 0.0053(5) 0.0005(5) 0.0095(5) C9 0.0306(8) 0.0241(7) 0.0224(7) 0.0106(6) 0.0039(6) 0.0080(6) C10 0.0326(8) 0.0181(6) 0.0285(8) 0.0049(6) 0.0013(6) 0.0074(6) C11 0.0286(7) 0.0210(6) 0.0196(7) -0.0002(5) 0.0016(6) 0.0092(6) C12 0.0227(6) 0.0214(6) 0.0144(6) 0.0035(5) 0.0050(5) 0.0099(5) C13 0.0189(7) 0.0312(8) 0.0337(8) 0.0017(6) -0.0047(6) 0.0086(6) C14 0.0242(8) 0.0326(8) 0.0521(11) -0.0024(7) 0.0005(7) 0.0000(7) N1 0.0181(5) 0.0209(5) 0.0198(6) 0.0006(4) 0.0025(4) 0.0093(4) N2 0.0149(5) 0.0161(5) 0.0131(5) 0.0026(4) 0.0020(4) 0.0053(4) Si 0.01811(18) 0.01703(17) 0.01896(19) -0.00044(14) -0.00066(14) 0.00553(14) Zn 0.01461(9) 0.01952(9) 0.01941(9) 0.00188(6) -0.00034(6) 0.00547(6) #----------------------------------------------------------------------------# # 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 C1 Si 1.8780(15) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 Si 1.8798(15) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 N1 1.4771(16) . ? C3 C4 1.526(2) . ? C3 C6 1.535(2) . ? C3 C5 1.5372(19) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 N2 1.4903(15) . ? C7 Si 1.9011(13) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 N2 1.4805(16) . ? C8 C9 1.5200(18) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.5229(19) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.5223(19) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.5158(18) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 N2 1.4859(15) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.522(2) . ? C13 Zn 1.9692(14) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? N1 Si 1.6958(11) . ? N1 Zn 1.9046(10) . ? N2 Zn 2.1672(10) . ? 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 Si C1 H1A 109.5 . . ? Si C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si C2 H2A 109.5 . . ? Si C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 109.65(11) . . ? N1 C3 C6 111.92(11) . . ? C4 C3 C6 107.99(12) . . ? N1 C3 C5 110.00(11) . . ? C4 C3 C5 108.71(12) . . ? C6 C3 C5 108.50(12) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 Si 113.86(8) . . ? N2 C7 H7A 108.8 . . ? Si C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? Si C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N2 C8 C9 111.78(10) . . ? N2 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C10 110.80(11) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 109.87(11) . . ? C11 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? C11 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C12 C11 C10 110.96(11) . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108 . . ? N2 C12 C11 112.01(10) . . ? N2 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? N2 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 Zn 116.60(11) . . ? C14 C13 H13A 108.1 . . ? Zn C13 H13A 108.1 . . ? C14 C13 H13B 108.1 . . ? Zn C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C3 N1 Si 126.66(9) . . ? C3 N1 Zn 118.36(8) . . ? Si N1 Zn 113.21(6) . . ? C8 N2 C12 109.18(9) . . ? C8 N2 C7 109.67(10) . . ? C12 N2 C7 109.55(9) . . ? C8 N2 Zn 109.48(7) . . ? C12 N2 Zn 117.41(8) . . ? C7 N2 Zn 101.18(7) . . ? N1 Si C1 117.28(7) . . ? N1 Si C2 116.71(7) . . ? C1 Si C2 106.23(7) . . ? N1 Si C7 102.36(5) . . ? C1 Si C7 103.66(7) . . ? C2 Si C7 109.60(6) . . ? N1 Zn C13 144.34(5) . . ? N1 Zn N2 93.27(4) . . ? C13 Zn N2 122.39(5) . . ? _chemical_name_common ;(tert-butyl(dimethyl(piperidin-1- ylmethyl)silyl)amino)(ethyl)zinc ; # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment '- ccdc_comp_4.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-02-23 at 09:49:22 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.reqdat # CIF files read : compounds_4 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_compounds_4 _database_code_depnum_ccdc_archive 'CCDC 869492' #TrackingRef '- ccdc_comp_4.cif' _audit_creation_date 2012-02-23T09:49:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; adduct of diethylzinc and (tert butylamino)-(N,N?,N?-trimethylcyclohexyl-1R,2R-diamino-N-methyl)-dimethylsilane ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_hall 'C 2y' _chemical_formula_sum 'C20 H47 N3 Si Zn' _chemical_formula_weight 423.07 _chemical_absolute_configuration syn #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 14.7303(5) _cell_length_b 10.1126(3) _cell_length_c 17.4314(6) _cell_angle_alpha 90 _cell_angle_beta 107.870(4) _cell_angle_gamma 90 _cell_volume 2471.35(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4845 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 26.00 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.05 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7435 _exptl_absorpt_correction_T_max 0.7435 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur S Oxford Diffraction' _diffrn_measurement_method Omega-scan _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_unetI/netI 0.0283 _diffrn_reflns_number 22745 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 4845 _reflns_number_gt 4495 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38)' ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET) (compiled Oct 24 2008,09:44:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Ortep-3 (Farrugia, 1997) and Schakal 92 (Keller 1992) ; _computing_publication_material 'wingx (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4845 _refine_ls_number_parameters 240 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.01 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(7) _refine_diff_density_max 0.364 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.039 #----------------------------------------------------------------------------# # 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' 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' Zn Zn 0.2839 1.4301 '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 C1 C 0.2804(2) 0.4546(2) 0.80506(19) 0.0610(8) Uani 1 1 d . . . H1A H 0.227 0.4671 0.7557 0.092 Uiso 1 1 calc R . . H1B H 0.3407 0.4662 0.7931 0.092 Uiso 1 1 calc R . . H1C H 0.2762 0.5199 0.8454 0.092 Uiso 1 1 calc R . . C2 C 0.36598(19) 0.2784(3) 0.94567(16) 0.0591(8) Uani 1 1 d . . . H2A H 0.3472 0.3379 0.9825 0.089 Uiso 1 1 calc R . . H2B H 0.4279 0.3062 0.9411 0.089 Uiso 1 1 calc R . . H2C H 0.3709 0.1879 0.9666 0.089 Uiso 1 1 calc R . . C3 C 0.09945(17) 0.2894(3) 0.88698(16) 0.0468(6) Uani 1 1 d . . . C4 C 0.1286(3) 0.2250(6) 0.9701(2) 0.122(2) Uani 1 1 d . . . H4A H 0.1231 0.1287 0.9641 0.183 Uiso 1 1 calc R . . H4B H 0.0868 0.2564 1.0004 0.183 Uiso 1 1 calc R . . H4C H 0.1948 0.2485 0.9991 0.183 Uiso 1 1 calc R . . C5 C 0.1050(3) 0.4350(4) 0.8938(4) 0.155(3) Uani 1 1 d . . . H5A H 0.1708 0.4613 0.9221 0.232 Uiso 1 1 calc R . . H5B H 0.063 0.4659 0.9241 0.232 Uiso 1 1 calc R . . H5C H 0.0849 0.4742 0.8398 0.232 Uiso 1 1 calc R . . C6 C -0.0008(2) 0.2489(4) 0.84218(19) 0.0731(10) Uani 1 1 d . . . H6A H -0.0194 0.2872 0.7879 0.11 Uiso 1 1 calc R . . H6B H -0.044 0.2807 0.8711 0.11 Uiso 1 1 calc R . . H6C H -0.0044 0.1522 0.8382 0.11 Uiso 1 1 calc R . . C7 C 0.31956(14) 0.15462(19) 0.78696(12) 0.0242(4) Uani 1 1 d . . . H7A H 0.3808 0.1875 0.782 0.029 Uiso 1 1 calc R . . H7B H 0.3347 0.075 0.8216 0.029 Uiso 1 1 calc R . . C8 C 0.22252(16) 0.2234(2) 0.65410(14) 0.0248(5) Uani 1 1 d . . . H8A H 0.1744 0.267 0.6736 0.037 Uiso 1 1 calc R . . H8B H 0.1929 0.193 0.5986 0.037 Uiso 1 1 calc R . . H8C H 0.2737 0.2861 0.6555 0.037 Uiso 1 1 calc R . . C9 C 0.32031(13) 0.02082(16) 0.67045(12) 0.0215(5) Uani 1 1 d . . . H9 H 0.3582 -0.0383 0.7147 0.026 Uiso 1 1 calc R . . C10 C 0.39173(15) 0.0957(2) 0.63824(14) 0.0329(5) Uani 1 1 d . . . H10A H 0.3565 0.1586 0.596 0.04 Uiso 1 1 calc R . . H10B H 0.4352 0.1476 0.6826 0.04 Uiso 1 1 calc R . . C11 C 0.45032(15) 0.0037(3) 0.60321(15) 0.0434(6) Uani 1 1 d . . . H11A H 0.4885 -0.0563 0.6458 0.052 Uiso 1 1 calc R . . H11B H 0.4947 0.0561 0.5827 0.052 Uiso 1 1 calc R . . C12 C 0.38472(18) -0.0769(2) 0.53497(16) 0.0423(6) Uani 1 1 d . . . H12A H 0.3483 -0.0172 0.4913 0.051 Uiso 1 1 calc R . . H12B H 0.4229 -0.1375 0.5125 0.051 Uiso 1 1 calc R . . C13 C 0.31671(15) -0.1557(2) 0.56691(14) 0.0308(5) Uani 1 1 d . . . H13A H 0.3536 -0.2193 0.6078 0.037 Uiso 1 1 calc R . . H13B H 0.2732 -0.2069 0.5222 0.037 Uiso 1 1 calc R . . C14 C 0.25793(13) -0.06807(19) 0.60448(12) 0.0220(4) Uani 1 1 d . . . H14 H 0.2188 -0.0089 0.5609 0.026 Uiso 1 1 calc R . . C15 C 0.23321(19) -0.2623(2) 0.68205(17) 0.0394(7) Uani 1 1 d . . . H15A H 0.2471 -0.3281 0.6459 0.059 Uiso 1 1 calc R . . H15B H 0.1886 -0.2999 0.7078 0.059 Uiso 1 1 calc R . . H15C H 0.2925 -0.2374 0.7235 0.059 Uiso 1 1 calc R . . C16 C 0.10721(15) -0.1862(2) 0.56876(15) 0.0377(6) Uani 1 1 d . . . H16A H 0.0796 -0.1093 0.5356 0.057 Uiso 1 1 calc R . . H16B H 0.0595 -0.2255 0.5906 0.057 Uiso 1 1 calc R . . H16C H 0.127 -0.2517 0.5356 0.057 Uiso 1 1 calc R . . C17 C 0.01866(14) 0.07424(19) 0.63985(13) 0.0274(5) Uani 1 1 d . . . H17A H 0.0129 0.165 0.6592 0.033 Uiso 1 1 calc R . . H17B H 0.0253 0.0814 0.5852 0.033 Uiso 1 1 calc R . . C18 C -0.07285(13) -0.0020(3) 0.63438(13) 0.0370(5) Uani 1 1 d . . . H18A H -0.0675 -0.0925 0.6162 0.056 Uiso 1 1 calc R . . H18B H -0.1272 0.0421 0.5959 0.056 Uiso 1 1 calc R . . H18C H -0.0824 -0.0043 0.6876 0.056 Uiso 1 1 calc R . . C19 C 0.16893(18) -0.1030(2) 0.82176(13) 0.0364(5) Uani 1 1 d . . . H19A H 0.2289 -0.1536 0.8312 0.044 Uiso 1 1 calc R . . H19B H 0.1789 -0.0364 0.8652 0.044 Uiso 1 1 calc R . . C20 C 0.0892(2) -0.1965(3) 0.82463(17) 0.0602(8) Uani 1 1 d . . . H20A H 0.0317 -0.1452 0.8216 0.09 Uiso 1 1 calc R . . H20B H 0.1088 -0.2466 0.8752 0.09 Uiso 1 1 calc R . . H20C H 0.0756 -0.2578 0.779 0.09 Uiso 1 1 calc R . . H1N H 0.1500(16) 0.174(2) 0.8291(13) 0.017(6) Uiso 1 1 d . . . N1 N 0.16262(14) 0.2432(2) 0.84179(12) 0.0334(4) Uani 1 1 d . . . N2 N 0.26228(11) 0.10950(15) 0.70592(9) 0.0198(3) Uani 1 1 d . . . N3 N 0.19042(11) -0.14463(16) 0.63542(10) 0.0237(4) Uani 1 1 d . . . Si1 Si 0.27524(4) 0.28449(6) 0.84511(4) 0.02857(13) Uani 1 1 d . . . Zn1 Zn 0.137511(13) -0.009927(18) 0.713701(11) 0.02165(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.097(2) 0.0303(15) 0.075(2) -0.0108(12) 0.0555(19) -0.0131(13) C2 0.0409(15) 0.092(2) 0.0398(15) -0.0254(15) 0.0059(12) -0.0060(15) C3 0.0347(13) 0.0679(17) 0.0445(15) -0.0205(13) 0.0222(12) -0.0006(13) C4 0.067(2) 0.265(6) 0.048(2) 0.000(3) 0.0373(19) 0.017(3) C5 0.146(4) 0.088(3) 0.299(8) -0.098(4) 0.169(5) -0.031(3) C6 0.0413(16) 0.120(3) 0.064(2) -0.015(2) 0.0259(14) 0.0054(18) C7 0.0201(10) 0.0270(10) 0.0263(11) -0.0009(8) 0.0081(8) -0.0032(8) C8 0.0251(11) 0.0228(11) 0.0270(12) 0.0060(9) 0.0089(9) 0.0027(9) C9 0.0198(9) 0.0181(12) 0.0304(11) 0.0007(7) 0.0133(8) -0.0005(7) C10 0.0306(12) 0.0321(11) 0.0425(14) -0.0098(10) 0.0207(10) -0.0119(9) C11 0.0371(11) 0.0432(14) 0.0640(15) -0.0146(15) 0.0363(11) -0.0152(14) C12 0.0485(15) 0.0401(12) 0.0526(15) -0.0151(12) 0.0365(13) -0.0119(11) C13 0.0320(12) 0.0269(10) 0.0400(13) -0.0088(10) 0.0205(10) -0.0053(9) C14 0.0225(10) 0.0214(9) 0.0230(10) 0.0019(8) 0.0082(9) -0.0011(8) C15 0.0466(15) 0.0228(11) 0.0592(18) 0.0085(11) 0.0315(14) 0.0064(10) C16 0.0257(12) 0.0392(13) 0.0498(15) -0.0224(11) 0.0141(11) -0.0082(10) C17 0.0210(10) 0.0269(11) 0.0334(12) -0.0015(9) 0.0071(9) 0.0052(8) C18 0.0224(9) 0.0455(12) 0.0443(12) -0.0062(15) 0.0119(8) 0.0049(14) C19 0.0520(15) 0.0314(12) 0.0257(12) 0.0023(9) 0.0118(11) -0.0080(10) C20 0.085(2) 0.0615(18) 0.0413(16) 0.0045(13) 0.0301(16) -0.0314(17) N1 0.0349(11) 0.0338(11) 0.0341(11) -0.0080(9) 0.0146(9) -0.0047(9) N2 0.0203(8) 0.0199(8) 0.0207(9) 0.0010(6) 0.0084(7) 0.0002(6) N3 0.0180(8) 0.0202(8) 0.0348(10) -0.0004(7) 0.0109(8) -0.0009(7) Si1 0.0314(3) 0.0291(3) 0.0276(3) -0.0072(2) 0.0127(3) -0.0054(2) Zn1 0.01988(10) 0.02437(10) 0.02168(10) 0.00206(12) 0.00783(7) -0.00144(13) #----------------------------------------------------------------------------# # 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 C1 Si1 1.867(2) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 Si1 1.851(3) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 N1 1.468(3) . ? C3 C5 1.477(5) . ? C3 C6 1.500(4) . ? C3 C4 1.525(5) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 N2 1.478(2) . ? C7 Si1 1.893(2) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 N2 1.470(3) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 N2 1.497(2) . ? C9 C14 1.525(3) . ? C9 C10 1.536(3) . ? C9 H9 1 . ? C10 C11 1.519(3) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.519(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.513(3) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.520(3) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 N3 1.486(2) . ? C14 H14 1 . ? C15 N3 1.470(3) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 N3 1.468(3) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.530(3) . ? C17 Zn1 2.016(2) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C20 1.520(3) . ? C19 Zn1 2.028(2) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? N1 Si1 1.694(2) . ? N1 H1N 0.74(2) . ? N2 Zn1 2.2377(15) . ? N3 Zn1 2.2311(16) . ? 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 Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C5 109.4(2) . . ? N1 C3 C6 108.6(2) . . ? C5 C3 C6 109.6(3) . . ? N1 C3 C4 109.5(2) . . ? C5 C3 C4 110.9(4) . . ? C6 C3 C4 108.9(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 Si1 122.44(13) . . ? N2 C7 H7A 106.7 . . ? Si1 C7 H7A 106.7 . . ? N2 C7 H7B 106.7 . . ? Si1 C7 H7B 106.7 . . ? H7A C7 H7B 106.6 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C14 112.10(15) . . ? N2 C9 C10 113.42(14) . . ? C14 C9 C10 109.69(16) . . ? N2 C9 H9 107.1 . . ? C14 C9 H9 107.1 . . ? C10 C9 H9 107.1 . . ? C11 C10 C9 112.47(18) . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C10 C11 C12 109.88(18) . . ? C10 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C13 C12 C11 109.17(19) . . ? C13 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? C12 C13 C14 112.36(17) . . ? C12 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.9 . . ? N3 C14 C13 112.69(16) . . ? N3 C14 C9 110.41(15) . . ? C13 C14 C9 112.16(15) . . ? N3 C14 H14 107.1 . . ? C13 C14 H14 107.1 . . ? C9 C14 H14 107.1 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 Zn1 113.77(15) . . ? C18 C17 H17A 108.8 . . ? Zn1 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? Zn1 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 Zn1 111.14(17) . . ? C20 C19 H19A 109.4 . . ? Zn1 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? Zn1 C19 H19B 109.4 . . ? H19A C19 H19B 108 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C3 N1 Si1 132.72(17) . . ? C3 N1 H1N 108.6(19) . . ? Si1 N1 H1N 113.4(19) . . ? C8 N2 C7 110.40(16) . . ? C8 N2 C9 112.69(15) . . ? C7 N2 C9 110.41(15) . . ? C8 N2 Zn1 106.28(12) . . ? C7 N2 Zn1 110.32(11) . . ? C9 N2 Zn1 106.58(10) . . ? C16 N3 C15 108.53(18) . . ? C16 N3 C14 110.55(16) . . ? C15 N3 C14 113.67(16) . . ? C16 N3 Zn1 107.19(12) . . ? C15 N3 Zn1 109.10(14) . . ? C14 N3 Zn1 107.59(11) . . ? N1 Si1 C2 116.05(11) . . ? N1 Si1 C1 111.49(13) . . ? C2 Si1 C1 106.52(15) . . ? N1 Si1 C7 107.79(9) . . ? C2 Si1 C7 102.51(11) . . ? C1 Si1 C7 112.26(10) . . ? C17 Zn1 C19 134.03(10) . . ? C17 Zn1 N3 105.38(8) . . ? C19 Zn1 N3 105.17(8) . . ? C17 Zn1 N2 107.57(7) . . ? C19 Zn1 N2 110.44(8) . . ? N3 Zn1 N2 81.08(6) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _chemical_name_common ; adduct of diethylzinc and (tert butylamino)-(N,N?,N?- trimethylcyclohexyl-1R,2R-diamino-N-methyl)-dimethylsilane ;