Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _audit_creation_date 17-12-01 _audit_creation_method CRYSTALS _publ_contact_letter ; These are the CIF format data (4 compounds) for the paper Scandium and yttrium complexes of the diamide-diamine donor ligand (2-C5H4N)CH2N(CH2CH2NSiMe3)2: chloride, primary and secondary amide, benzamidinate and alkyl functionalised derivatives M. E. G. Skinner and P. Mountford ; _journal_coden_Cambridge 186 loop_ _publ_author_name 'Mountford, Philip' 'Skinner, Michael E. G.' _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Dr Philip Mountford' _publ_contact_author_address ; Inorganic Chemistry Laboratory University of Oxford South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_phone '+44 1865 272679' _contact_author_fax '+44 1865 272690' _publ_contact_author_email Philip.Mountford@chem.ox.ac.uk _publ_section_title ; Scandium and yttrium complexes of the diamide-diamine donor ligand (2-C5H4N)CH2N(CH2CH2NSiMe3)2: chloride, primary and secondary amide, benzamidinate and alkyl functionalised derivatives ; data_COMPOUND_5 _database_code_CSD 176539 # Local code MEGS30 _chemical_name_systematic ; [Y{N(SiMe3)2}(N2NN')] ; _publ_section_exptl_refinement ; NO SPECIAL DETAILS ; _cell_length_a 9.281(1) _cell_angle_alpha 90 _cell_length_b 17.696(2) _cell_angle_beta 90 _cell_length_c 19.399(2) _cell_angle_gamma 90 _cell_volume 3186.0(6) _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,-y+1/2,-z' '-x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Y ' -2.9510 3.5420 17.7760 1.4029 10.2946 12.8006 5.7263 0.1256 3.2659 104.3540 1.9121 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C22 H50 N5 Si4 Y1 ' _chemical_formula_moiety ' C22 H50 N5 Si4 Y1 ' _chemical_compound_source ; [[Y(N2NN')Cl]" + LiN(SiMe3)2 ; _chemical_formula_weight 585.93 _cell_measurement_reflns_used 17528 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 175 _cell_formula_units_Z 4 _exptl_crystal_description 'block ' _exptl_crystal_colour 'Colourless ' _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_size_min 0.4 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_max 0.5 _exptl_crystal_density_diffrn 1.22 _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 2.01 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.366 _exptl_absorpt_correction_T_max 0.448 _diffrn_reflns_av_sigmaI/netI 0.063 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device-type 'Enraf-nonius DIP2000' _diffrn_ambient_temperature 175 _diffrn_reflns_number 17528 _reflns_number_total 6521 _diffrn_reflns_av_R_equivalents 0.031 _reflns_number_observed 5692 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.43 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _reflns_observed_criterion >3.00\s(I) _refine_ls_number_reflns 5692 _refine_diff_density_min -0.92 _refine_diff_density_max 0.66 _refine_ls_number_parameters 289 _refine_ls_R_factor_obs 0.0289 _refine_ls_wR_factor_obs 0.0332 _refine_ls_goodness_of_fit_obs 1.1016 _refine_ls_shift/su_max 0.0016 _refine_ls_structure_factor_coef F _refine_ls_extinction_method 'none' _refine_ls_hydrogen_treatment riding _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.40 0.674E-010.800 ; _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack 0.003(99) _refine_ls_extinction_coef 'None required' _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_data_collection 'DIP2000 software Xpress (MAC Science, 1989)' _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Y1 0.64813(2) 0.984286(13) 0.355567(12) 0.0219 1.0000 Uani N1 0.5502(3) 0.97266(14) 0.25083(12) 0.0313 1.0000 Uani N2 0.5640(2) 0.89876(13) 0.43096(12) 0.0275 1.0000 Uani N3 0.9006(2) 0.95271(13) 0.38443(12) 0.0276 1.0000 Uani N4 0.7290(2) 0.85846(13) 0.30630(11) 0.0273 1.0000 Uani N5 0.6966(2) 1.10905(12) 0.37623(12) 0.0279 1.0000 Uani Si1 0.41030(8) 1.02171(5) 0.21484(4) 0.0313 1.0000 Uani Si2 0.58646(9) 0.88678(4) 0.51807(4) 0.0295 1.0000 Uani Si3 0.61546(8) 1.16109(4) 0.44010(4) 0.0309 1.0000 Uani Si4 0.81265(9) 1.14930(5) 0.31901(4) 0.0326 1.0000 Uani C1 0.6241(4) 0.91940(17) 0.20421(14) 0.0359 1.0000 Uani C2 0.6511(3) 0.84554(16) 0.24082(14) 0.0331 1.0000 Uani C3 0.5439(3) 0.82633(17) 0.39370(15) 0.0326 1.0000 Uani C4 0.6845(3) 0.80205(14) 0.35831(16) 0.0323 1.0000 Uani C5 0.8860(3) 0.85620(17) 0.29564(15) 0.0341 1.0000 Uani C6 0.9676(3) 0.89529(15) 0.35230(16) 0.0303 1.0000 Uani C7 1.1096(3) 0.87666(19) 0.36739(17) 0.0406 1.0000 Uani C8 1.1839(3) 0.9180(2) 0.41663(18) 0.0445 1.0000 Uani C9 1.1153(3) 0.9771(2) 0.44920(15) 0.0386 1.0000 Uani C10 0.9739(3) 0.99247(17) 0.43176(14) 0.0321 1.0000 Uani C11 0.2610(4) 0.9580(2) 0.1848(2) 0.0510 1.0000 Uani C12 0.4680(4) 1.0791(2) 0.13850(19) 0.0460 1.0000 Uani C13 0.3345(4) 1.0875(2) 0.28076(18) 0.0464 1.0000 Uani C14 0.7251(5) 0.8128(2) 0.53961(19) 0.0547 1.0000 Uani C15 0.4168(5) 0.8579(3) 0.56366(19) 0.0651 1.0000 Uani C16 0.6484(4) 0.97633(18) 0.55867(15) 0.0420 1.0000 Uani C17 0.5782(4) 1.26151(19) 0.4147(2) 0.0536 1.0000 Uani C18 0.4376(3) 1.1168(2) 0.46423(17) 0.0424 1.0000 Uani C19 0.7286(4) 1.1714(2) 0.51981(18) 0.0459 1.0000 Uani C20 0.8924(4) 1.0756(2) 0.25978(18) 0.0460 1.0000 Uani C21 0.9686(4) 1.1991(2) 0.3608(2) 0.0515 1.0000 Uani C22 0.7254(5) 1.2189(2) 0.2583(2) 0.0538 1.0000 Uani H11 0.7182 0.94166 0.18952 0.0432 1.0000 Uiso H12 0.5625 0.91030 0.16272 0.0432 1.0000 Uiso H21 0.7103 0.81208 0.21044 0.0395 1.0000 Uiso H22 0.5567 0.82056 0.25075 0.0395 1.0000 Uiso H31 0.5141 0.78639 0.42726 0.0396 1.0000 Uiso H32 0.4671 0.83272 0.35801 0.0396 1.0000 Uiso H41 0.7621 0.79716 0.39383 0.0390 1.0000 Uiso H42 0.6695 0.75218 0.33518 0.0390 1.0000 Uiso H51 0.9087 0.88177 0.25099 0.0411 1.0000 Uiso H52 0.9176 0.80223 0.29345 0.0411 1.0000 Uiso H71 1.1579 0.83400 0.34274 0.0485 1.0000 Uiso H81 1.2859 0.9050 0.42829 0.0533 1.0000 Uiso H91 1.1666 1.0081 0.48456 0.0463 1.0000 Uiso H101 0.9237 1.03506 0.45568 0.0387 1.0000 Uiso H111 0.1820 0.9891 0.1642 0.0617 1.0000 Uiso H112 0.2225 0.9288 0.2249 0.0617 1.0000 Uiso H113 0.2990 0.9222 0.1493 0.0617 1.0000 Uiso H121 0.3828 1.1066 0.11932 0.0552 1.0000 Uiso H122 0.5430 1.1164 0.15298 0.0552 1.0000 Uiso H123 0.5087 1.0448 0.10242 0.0552 1.0000 Uiso H131 0.2524 1.1166 0.26036 0.0566 1.0000 Uiso H132 0.4114 1.1234 0.29595 0.0566 1.0000 Uiso H133 0.2994 1.0579 0.32132 0.0566 1.0000 Uiso H141 0.7341 0.8081 0.59080 0.0670 1.0000 Uiso H142 0.8201 0.8283 0.51971 0.0670 1.0000 Uiso H143 0.6955 0.7631 0.51964 0.0670 1.0000 Uiso H151 0.4365 0.8519 0.61404 0.0783 1.0000 Uiso H152 0.3413 0.8976 0.55680 0.0783 1.0000 Uiso H153 0.3820 0.8089 0.54429 0.0783 1.0000 Uiso H161 0.6610 0.96840 0.60936 0.0514 1.0000 Uiso H162 0.5750 1.01674 0.55061 0.0514 1.0000 Uiso H163 0.7424 0.99199 0.53791 0.0514 1.0000 Uiso H171 0.5310 1.28833 0.4540 0.0644 1.0000 Uiso H172 0.6710 1.28720 0.4031 0.0644 1.0000 Uiso H173 0.5130 1.26263 0.3736 0.0644 1.0000 Uiso H181 0.3910 1.1474 0.50137 0.0515 1.0000 Uiso H182 0.3733 1.1153 0.42290 0.0515 1.0000 Uiso H183 0.4543 1.0642 0.48128 0.0515 1.0000 Uiso H191 0.6752 1.2021 0.55471 0.0550 1.0000 Uiso H192 0.8213 1.1971 0.50801 0.0550 1.0000 Uiso H193 0.7493 1.1202 0.53923 0.0550 1.0000 Uiso H201 0.9600 1.1004 0.22661 0.0549 1.0000 Uiso H202 0.9462 1.0374 0.28774 0.0549 1.0000 Uiso H203 0.8134 1.0500 0.23367 0.0549 1.0000 Uiso H211 1.0321 1.2214 0.3244 0.0620 1.0000 Uiso H212 0.9316 1.2403 0.3913 0.0620 1.0000 Uiso H213 1.0250 1.1621 0.3889 0.0620 1.0000 Uiso H221 0.8003 1.2398 0.2265 0.0662 1.0000 Uiso H222 0.6812 1.2610 0.2854 0.0662 1.0000 Uiso H223 0.6491 1.1928 0.2307 0.0662 1.0000 Uiso 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 Y1 0.0195(1) 0.0220(1) 0.0241(1) -0.0003(1) -0.00163(9) 0.0014(1) N1 0.0331(12) 0.0339(13) 0.0270(11) -0.003(1) -0.0050(9) 0.005(1) N2 0.0229(11) 0.0296(11) 0.0299(11) 0.0004(9) 0.0000(9) -0.0018(9) N3 0.021(1) 0.0310(11) 0.0304(11) 0.0008(9) -0.0000(9) 0.0024(9) N4 0.0261(11) 0.0273(11) 0.0285(11) -0.0026(9) -0.0024(9) 0.0024(9) N5 0.0270(11) 0.0225(11) 0.0343(12) -0.0011(9) -0.0019(9) -0.0006(9) Si1 0.0272(3) 0.0356(4) 0.0310(4) 0.0006(3) -0.0066(3) 0.0013(3) Si2 0.0304(4) 0.0300(4) 0.0280(4) 0.0031(3) 0.0002(3) -0.0044(3) Si3 0.0279(4) 0.0265(4) 0.0384(4) -0.0025(3) 0.0023(3) 0.0025(3) Si4 0.0338(4) 0.0289(4) 0.0351(4) 0.0015(3) 0.0017(3) -0.0060(3) C1 0.0406(17) 0.0389(15) 0.0281(13) -0.0027(11) -0.0047(12) 0.0023(13) C2 0.0346(14) 0.0338(13) 0.0310(13) -0.0082(11) -0.0013(13) 0.0006(13) C3 0.0307(14) 0.0312(14) 0.0359(15) -0.0013(12) -0.0003(12) -0.0061(12) C4 0.0395(15) 0.0227(12) 0.0348(13) 0.0004(12) -0.0009(13) 0.002(1) C5 0.0296(15) 0.0360(14) 0.0368(14) -0.0055(12) 0.0034(11) 0.0069(12) C6 0.0246(12) 0.0311(13) 0.0352(14) 0.0031(13) 0.0029(12) 0.004(1) C7 0.0262(14) 0.0482(17) 0.0474(18) -0.0021(14) 0.0000(12) 0.0115(12) C8 0.0241(15) 0.063(2) 0.0469(18) -0.0005(16) -0.0011(13) 0.0079(14) C9 0.0245(13) 0.0518(17) 0.0394(14) 0.0018(15) -0.0064(11) -0.0062(13) C10 0.0252(13) 0.0380(15) 0.0331(13) 0.0013(12) 0.001(1) -0.0014(11) C11 0.0417(19) 0.050(2) 0.061(2) -0.0008(17) -0.0138(17) -0.0062(15) C12 0.0417(17) 0.0532(19) 0.0432(18) 0.0123(16) -0.0070(15) 0.0025(14) C13 0.0392(18) 0.0533(19) 0.0467(18) -0.0064(15) -0.0036(15) 0.0077(16) C14 0.075(3) 0.0435(19) 0.046(2) 0.0050(16) -0.0157(18) 0.0183(18) C15 0.061(2) 0.095(3) 0.0390(18) 0.001(2) 0.0127(17) -0.035(2) C16 0.0499(17) 0.0392(15) 0.0368(14) -0.0006(13) -0.0090(14) -0.0044(16) C17 0.055(2) 0.0350(16) 0.070(2) 0.0036(16) 0.0148(19) 0.0147(16) C18 0.0313(16) 0.0519(19) 0.0440(17) 0.0027(14) 0.0031(13) -0.0006(14) C19 0.0438(19) 0.0477(19) 0.0462(18) -0.0151(16) -0.0053(15) -0.0043(15) C20 0.050(2) 0.0450(17) 0.0430(17) -0.0037(14) 0.0164(15) -0.0083(15) C21 0.0437(18) 0.054(2) 0.057(2) -0.0041(18) 0.0069(17) -0.0202(15) C22 0.067(2) 0.0426(19) 0.052(2) 0.0146(16) 0.0006(18) -0.0003(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Y1 . N1 . 2.235(2) yes Y1 . N2 . 2.245(2) yes Y1 . N3 . 2.473(2) yes Y1 . N4 . 2.537(2) yes Y1 . N5 . 2.289(2) yes N1 . Si1 . 1.711(2) yes N1 . C1 . 1.475(4) yes N2 . Si2 . 1.716(2) yes N2 . C3 . 1.483(4) yes N3 . C6 . 1.344(4) yes N3 . C10 . 1.342(4) yes N4 . C2 . 1.480(3) yes N4 . C4 . 1.478(4) yes N4 . C5 . 1.472(4) yes N5 . Si3 . 1.717(2) yes N5 . Si4 . 1.703(2) yes Si1 . C11 . 1.879(3) yes Si1 . C12 . 1.874(3) yes Si1 . C13 . 1.867(3) yes Si2 . C14 . 1.882(4) yes Si2 . C15 . 1.877(4) yes Si2 . C16 . 1.861(3) yes Si3 . C17 . 1.876(3) yes Si3 . C18 . 1.886(3) yes Si3 . C19 . 1.878(3) yes Si4 . C20 . 1.889(3) yes Si4 . C21 . 1.878(3) yes Si4 . C22 . 1.887(4) yes C1 . C2 . 1.508(4) yes C3 . C4 . 1.536(4) yes C5 . C6 . 1.503(4) yes C6 . C7 . 1.390(4) yes C7 . C8 . 1.387(5) yes C8 . C9 . 1.378(5) yes C9 . C10 . 1.382(4) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Y1 . N2 . 112.87(9) yes N1 . Y1 . N3 . 124.76(8) yes N2 . Y1 . N3 . 91.71(8) yes N1 . Y1 . N4 . 72.37(8) yes N2 . Y1 . N4 . 75.91(8) yes N3 . Y1 . N4 . 66.83(7) yes N1 . Y1 . N5 . 109.14(9) yes N2 . Y1 . N5 . 127.20(8) yes N3 . Y1 . N5 . 89.55(8) yes N4 . Y1 . N5 . 148.72(8) yes Y1 . N1 . Si1 . 129.26(13) yes Y1 . N1 . C1 . 115.28(17) yes Si1 . N1 . C1 . 115.26(18) yes Y1 . N2 . Si2 . 133.04(12) yes Y1 . N2 . C3 . 107.99(17) yes Si2 . N2 . C3 . 112.86(18) yes Y1 . N3 . C6 . 120.23(18) yes Y1 . N3 . C10 . 121.10(18) yes C6 . N3 . C10 . 118.7(2) yes Y1 . N4 . C2 . 108.33(16) yes Y1 . N4 . C4 . 104.64(15) yes C2 . N4 . C4 . 110.2(2) yes Y1 . N4 . C5 . 111.70(16) yes C2 . N4 . C5 . 111.0(2) yes C4 . N4 . C5 . 110.7(2) yes Y1 . N5 . Si3 . 123.89(12) yes Y1 . N5 . Si4 . 114.42(12) yes Si3 . N5 . Si4 . 121.55(13) yes N1 . Si1 . C11 . 112.46(15) yes N1 . Si1 . C12 . 112.37(14) yes C11 . Si1 . C12 . 106.87(17) yes N1 . Si1 . C13 . 108.85(13) yes C11 . Si1 . C13 . 107.99(18) yes C12 . Si1 . C13 . 108.13(17) yes N2 . Si2 . C14 . 112.81(15) yes N2 . Si2 . C15 . 113.30(15) yes C14 . Si2 . C15 . 106.3(2) yes N2 . Si2 . C16 . 110.44(13) yes C14 . Si2 . C16 . 106.66(17) yes C15 . Si2 . C16 . 106.94(18) yes N5 . Si3 . C17 . 113.51(15) yes N5 . Si3 . C18 . 109.86(14) yes C17 . Si3 . C18 . 107.31(17) yes N5 . Si3 . C19 . 113.65(14) yes C17 . Si3 . C19 . 103.17(18) yes C18 . Si3 . C19 . 108.96(16) yes N5 . Si4 . C20 . 110.84(13) yes N5 . Si4 . C21 . 113.73(15) yes C20 . Si4 . C21 . 106.52(17) yes N5 . Si4 . C22 . 114.10(16) yes C20 . Si4 . C22 . 103.81(17) yes C21 . Si4 . C22 . 107.09(18) yes N1 . C1 . C2 . 110.0(2) yes N4 . C2 . C1 . 110.6(2) yes N2 . C3 . C4 . 110.7(2) yes N4 . C4 . C3 . 110.7(2) yes N4 . C5 . C6 . 112.5(2) yes N3 . C6 . C5 . 117.0(2) yes N3 . C6 . C7 . 121.3(3) yes C5 . C6 . C7 . 121.5(3) yes C6 . C7 . C8 . 119.4(3) yes C7 . C8 . C9 . 119.1(3) yes C8 . C9 . C10 . 118.4(3) yes N3 . C10 . C9 . 123.0(3) yes #===end data_COMPOUND_11 _database_code_CSD 176540 # Local code MEGS31 _chemical_name_systematic ; [Sc{PhC(NSiMe3)2}(N2NN')] ; _publ_section_exptl_refinement ; H atoms were placed geometrically. U[iso] values were refined for groups of chemically related H atoms ; _cell_length_a 11.064(1) _cell_angle_alpha 90 _cell_length_b 20.177(2) _cell_angle_beta 92.17(1) _cell_length_c 16.808(2) _cell_angle_gamma 90 _cell_volume 3749.5(6) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Sc ' 0.2260 0.3720 9.1890 9.0213 7.3679 0.5729 1.6409 136.1080 1.4680 51.3531 1.3329 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C29 H55 N6 Sc1 Si4 ' _chemical_formula_moiety ' C29 H55 N6 Sc1 Si4 ' _chemical_compound_source ; [Sc(N2NN')Cl] + Li[PhC(NSiMe3)2] ; _chemical_formula_weight 645.10 _cell_measurement_reflns_used 19051 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 175 _cell_formula_units_Z 4 _exptl_crystal_description 'block ' _exptl_crystal_colour 'Colourless ' _exptl_crystal_size_min 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_max 0.5 _exptl_crystal_density_diffrn 1.14 _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.35 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.952 _exptl_absorpt_correction_T_max 0.952 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _diffrn_reflns_av_sigmaI/netI 0.037 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_measurement_device-type 'Enraf-nonius DIP2000' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 175 _diffrn_reflns_number 19051 _reflns_number_total 7779 _diffrn_reflns_av_R_equivalents 0.025 _reflns_number_observed 6145 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.46 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _reflns_observed_criterion >3\s(I) _refine_diff_density_min -0.57 _refine_diff_density_max 0.66 _refine_ls_number_reflns 6145 _refine_ls_number_parameters 368 _refine_ls_R_factor_obs 0.0347 _refine_ls_wR_factor_obs 0.0403 _refine_ls_goodness_of_fit_obs 1.0117 _refine_ls_shift/esd_max 0.0009 _refine_ls_structure_factor_coef F _refine_ls_hydrogen_treatment 'Riding model' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_extinction_coef 43.4(121) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_data_collection 'DIP2000 software Xpress (MAC Science, 1989)' _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Sc1 0.55901(2) 0.11839(1) 0.28876(2) 0.0206 1.0000 Uani N1 0.4682(1) 0.02629(6) 0.29579(8) 0.0290 1.0000 Uani N2 0.5985(1) 0.19130(6) 0.37658(7) 0.0287 1.0000 Uani N3 0.4448(1) 0.20051(6) 0.21588(8) 0.0298 1.0000 Uani N4 0.3681(1) 0.14130(7) 0.35025(8) 0.0319 1.0000 Uani N5 0.7495(1) 0.07926(6) 0.29911(7) 0.0255 1.0000 Uani N6 0.6725(1) 0.11399(6) 0.17920(7) 0.0228 1.0000 Uani Si1 0.50495(4) -0.05194(2) 0.26357(2) 0.0291 1.0000 Uani Si2 0.67975(4) 0.26298(2) 0.37135(3) 0.0345 1.0000 Uani Si3 0.84502(4) 0.05866(3) 0.37928(3) 0.0342 1.0000 Uani Si4 0.65440(4) 0.10995(2) 0.07554(2) 0.0273 1.0000 Uani C1 0.3504(2) 0.02183(8) 0.3337(1) 0.0390 1.0000 Uani C2 0.3357(2) 0.07905(9) 0.3902(1) 0.0395 1.0000 Uani C3 0.5150(2) 0.19137(9) 0.4425(1) 0.0383 1.0000 Uani C4 0.3866(2) 0.19507(9) 0.4098(1) 0.0399 1.0000 Uani C5 0.2768(2) 0.16000(9) 0.2885(1) 0.0403 1.0000 Uani C6 0.3291(2) 0.21047(8) 0.2344(1) 0.0359 1.0000 Uani C7 0.2632(2) 0.2645(1) 0.2051(1) 0.0491 1.0000 Uani C8 0.3168(2) 0.3095(1) 0.1565(1) 0.0543 1.0000 Uani C9 0.4362(2) 0.29996(9) 0.1380(1) 0.0470 1.0000 Uani C10 0.4968(2) 0.24506(8) 0.1688(1) 0.0359 1.0000 Uani C11 0.6399(2) -0.05491(8) 0.2010(1) 0.0439 1.0000 Uani C12 0.5328(2) -0.11032(9) 0.3499(1) 0.0476 1.0000 Uani C13 0.3772(2) -0.0880(1) 0.2004(1) 0.0516 1.0000 Uani C14 0.7812(2) 0.2780(1) 0.4616(1) 0.0598 1.0000 Uani C15 0.7800(2) 0.2603(1) 0.2839(1) 0.0478 1.0000 Uani C16 0.5789(2) 0.33811(9) 0.3631(1) 0.0579 1.0000 Uani C17 0.7677(1) 0.09364(7) 0.22372(8) 0.0231 1.0000 Uani C18 0.8904(1) 0.08895(8) 0.18870(9) 0.0284 1.0000 Uani C19 0.9426(2) 0.14483(9) 0.1550(1) 0.0360 1.0000 Uani C20 1.0531(2) 0.1397(1) 0.1189(1) 0.0497 1.0000 Uani C21 1.1118(2) 0.0796(1) 0.1152(1) 0.0554 1.0000 Uani C22 1.0611(2) 0.0242(1) 0.1484(1) 0.0501 1.0000 Uani C23 0.9514(2) 0.02864(9) 0.1857(1) 0.0373 1.0000 Uani C24 0.9792(2) 0.1140(2) 0.3887(1) 0.0700 1.0000 Uani C25 0.8998(3) -0.0290(1) 0.3766(1) 0.0766 1.0000 Uani C26 0.7553(2) 0.0657(1) 0.4701(1) 0.0458 1.0000 Uani C27 0.4926(2) 0.08779(9) 0.0553(1) 0.0393 1.0000 Uani C28 0.6875(2) 0.1897(1) 0.0229(1) 0.0512 1.0000 Uani C29 0.7508(2) 0.04605(9) 0.0276(1) 0.0380 1.0000 Uani H11 0.3456 -0.01928 0.3621 0.045 1.0000 Uiso H12 0.2866 0.02374 0.2934 0.045 1.0000 Uiso H21 0.3891 0.07258 0.4359 0.045 1.0000 Uiso H22 0.2537 0.08135 0.4069 0.045 1.0000 Uiso H31 0.5320 0.22875 0.4764 0.045 1.0000 Uiso H32 0.5253 0.15120 0.4726 0.045 1.0000 Uiso H41 0.3312 0.18986 0.4519 0.045 1.0000 Uiso H42 0.3734 0.23723 0.3844 0.045 1.0000 Uiso H51 0.2072 0.17822 0.3129 0.045 1.0000 Uiso H52 0.2535 0.12142 0.2582 0.045 1.0000 Uiso H71 0.1803 0.2701 0.2187 0.049 1.0000 Uiso H81 0.2727 0.3472 0.1363 0.049 1.0000 Uiso H91 0.4758 0.33055 0.1038 0.049 1.0000 Uiso H101 0.5799 0.23857 0.1561 0.049 1.0000 Uiso H111 0.6547 -0.09986 0.1854 0.078 1.0000 Uiso H112 0.7091 -0.03823 0.2308 0.078 1.0000 Uiso H113 0.6254 -0.02813 0.1544 0.078 1.0000 Uiso H121 0.5529 -0.15339 0.3301 0.078 1.0000 Uiso H122 0.5985 -0.09400 0.3833 0.078 1.0000 Uiso H123 0.4612 -0.11335 0.3802 0.078 1.0000 Uiso H131 0.3989 -0.1315 0.1829 0.078 1.0000 Uiso H132 0.3061 -0.0907 0.2312 0.078 1.0000 Uiso H133 0.3612 -0.0601 0.1549 0.078 1.0000 Uiso H141 0.8245 0.3188 0.4555 0.104 1.0000 Uiso H142 0.8377 0.2421 0.4679 0.104 1.0000 Uiso H143 0.7328 0.2807 0.5077 0.104 1.0000 Uiso H151 0.8253 0.3008 0.2814 0.104 1.0000 Uiso H152 0.8347 0.2236 0.2898 0.104 1.0000 Uiso H153 0.7315 0.2551 0.2357 0.104 1.0000 Uiso H161 0.6276 0.37740 0.3604 0.104 1.0000 Uiso H162 0.5297 0.34047 0.4089 0.104 1.0000 Uiso H163 0.5280 0.33464 0.3158 0.104 1.0000 Uiso H191 0.9014 0.18664 0.1570 0.091(3 1.0000 Uiso H201 1.0886 0.1785 0.0963 0.091 1.0000 Uiso H211 1.1881 0.0764 0.0900 0.091 1.0000 Uiso H221 1.1016 -0.0178 0.1455 0.091 1.0000 Uiso H231 0.9170 -0.00999 0.2093 0.091 1.0000 Uiso H241 1.0292 0.1006 0.4338 0.101 1.0000 Uiso H242 1.0248 0.1113 0.3414 0.101 1.0000 Uiso H243 0.9525 0.1588 0.3961 0.101 1.0000 Uiso H251 0.9522 -0.0376 0.4222 0.101 1.0000 Uiso H252 0.9433 -0.0361 0.3290 0.101 1.0000 Uiso H253 0.8316 -0.0584 0.3770 0.101 1.0000 Uiso H261 0.8052 0.0546 0.5162 0.101 1.0000 Uiso H262 0.7265 0.1103 0.4749 0.101 1.0000 Uiso H263 0.6878 0.0359 0.4660 0.101 1.0000 Uiso H271 0.4765 0.08474 -0.0011 0.079 1.0000 Uiso H272 0.4419 0.12126 0.0772 0.079 1.0000 Uiso H273 0.4762 0.04588 0.0797 0.079 1.0000 Uiso H281 0.6758 0.1838 -0.0336 0.079 1.0000 Uiso H282 0.7699 0.2023 0.0350 0.079 1.0000 Uiso H283 0.6344 0.2239 0.0405 0.079 1.0000 Uiso H291 0.7359 0.04694 -0.0290 0.079 1.0000 Uiso H292 0.8345 0.05563 0.0396 0.079 1.0000 Uiso H293 0.7316 0.00293 0.0477 0.079 1.0000 Uiso 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 Sc1 0.0212(1) 0.0203(1) 0.0207(1) 0.00040(9) 0.00542(9) -0.00057(9) N1 0.0304(7) 0.0243(6) 0.0330(7) 0.0001(5) 0.0114(5) -0.0029(5) N2 0.0346(7) 0.0270(6) 0.0251(6) -0.0031(5) 0.0070(5) -0.0030(5) N3 0.0316(7) 0.0279(6) 0.0301(7) -0.0008(5) 0.0022(5) 0.0041(5) N4 0.0303(7) 0.0286(6) 0.0375(7) -0.0010(5) 0.0126(5) 0.0002(5) N5 0.0241(6) 0.0309(6) 0.0217(6) 0.0024(5) 0.0034(4) 0.0021(5) N6 0.0237(6) 0.0244(6) 0.0204(6) 0.0002(4) 0.0046(4) -0.0010(4) Si1 0.0395(2) 0.0216(2) 0.0265(2) 0.0024(1) 0.0066(2) -0.0031(2) Si2 0.0414(3) 0.0287(2) 0.0336(2) -0.0072(2) 0.0037(2) -0.0074(2) Si3 0.0283(2) 0.0498(3) 0.0244(2) 0.0049(2) -0.0000(2) 0.0085(2) Si4 0.0342(2) 0.0289(2) 0.0190(2) 0.0021(1) 0.0029(2) -0.0006(2) C1 0.0337(9) 0.0308(8) 0.054(1) 0.0020(7) 0.0171(8) -0.0067(6) C2 0.0358(9) 0.0363(9) 0.048(1) 0.0032(7) 0.0242(8) -0.0019(7) C3 0.050(1) 0.0392(9) 0.0262(8) -0.0068(6) 0.0127(7) -0.0040(7) C4 0.044(1) 0.0352(9) 0.0417(9) -0.0075(7) 0.0217(8) 0.0023(7) C5 0.0256(8) 0.0416(9) 0.054(1) 0.0001(8) 0.0083(7) 0.0037(7) C6 0.0310(8) 0.0350(8) 0.0418(9) -0.0045(7) 0.0009(7) 0.0078(6) C7 0.043(1) 0.048(1) 0.055(1) 0.0005(9) 0.0013(9) 0.0205(8) C8 0.070(1) 0.041(1) 0.052(1) 0.0063(9) -0.001(1) 0.025(1) C9 0.066(1) 0.0351(9) 0.040(1) 0.0079(7) 0.0035(9) 0.0082(8) C10 0.046(1) 0.0311(8) 0.0311(8) 0.0026(6) 0.0033(7) 0.0026(7) C11 0.060(1) 0.0247(8) 0.049(1) -0.0014(7) 0.0249(9) 0.0030(7) C12 0.063(1) 0.040(1) 0.040(1) 0.0144(8) 0.0089(9) 0.0077(8) C13 0.065(1) 0.044(1) 0.046(1) -0.0037(8) -0.0032(9) -0.0177(9) C14 0.058(1) 0.074(1) 0.047(1) -0.021(1) -0.006(1) -0.017(1) C15 0.056(1) 0.040(1) 0.048(1) -0.0064(8) 0.0158(9) -0.0184(8) C16 0.076(2) 0.0281(9) 0.070(1) -0.0054(9) 0.012(1) -0.0011(9) C17 0.0254(7) 0.0218(6) 0.0224(6) -0.0023(5) 0.0043(5) -0.0016(5) C18 0.0231(7) 0.0395(8) 0.0228(7) -0.0036(6) 0.0038(5) -0.0019(6) C19 0.0314(8) 0.0455(9) 0.0316(8) -0.0029(7) 0.0082(6) -0.0078(7) C20 0.038(1) 0.070(1) 0.042(1) -0.0065(9) 0.0162(8) -0.0169(9) C21 0.0285(9) 0.087(2) 0.052(1) -0.018(1) 0.0158(8) -0.0051(9) C22 0.0310(9) 0.069(1) 0.051(1) -0.015(1) 0.0089(8) 0.0108(9) C23 0.0295(8) 0.047(1) 0.0358(9) -0.0070(7) 0.0040(7) 0.0064(7) C24 0.035(1) 0.127(2) 0.047(1) 0.012(1) -0.0083(9) -0.022(1) C25 0.105(2) 0.078(2) 0.046(1) 0.006(1) -0.013(1) 0.054(2) C26 0.046(1) 0.065(1) 0.0266(8) 0.0115(8) 0.0043(7) 0.0055(9) C27 0.0385(9) 0.044(1) 0.0349(9) -0.0031(7) -0.0102(7) 0.0041(7) C28 0.080(1) 0.043(1) 0.0316(9) 0.0127(8) 0.0132(9) -0.006(1) C29 0.0410(9) 0.049(1) 0.0239(7) -0.0073(7) 0.0045(6) 0.0042(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sc1 . N1 . 2.118(1) yes Sc1 . N2 . 2.118(1) yes Sc1 . N3 . 2.393(1) yes Sc1 . N4 . 2.431(1) yes Sc1 . N5 . 2.251(1) yes Sc1 . N6 . 2.269(1) yes N1 . Si1 . 1.722(1) yes N1 . C1 . 1.475(2) yes N2 . Si2 . 1.707(1) yes N2 . C3 . 1.470(2) yes N3 . C6 . 1.344(2) yes N3 . C10 . 1.342(2) yes N4 . C2 . 1.475(2) yes N4 . C4 . 1.485(2) yes N4 . C5 . 1.470(2) yes N5 . Si3 . 1.731(1) yes N5 . C17 . 1.323(2) yes N6 . Si4 . 1.748(1) yes N6 . C17 . 1.334(2) yes Si1 . C11 . 1.860(2) yes Si1 . C12 . 1.885(2) yes Si1 . C13 . 1.882(2) yes Si2 . C14 . 1.877(2) yes Si2 . C15 . 1.876(2) yes Si2 . C16 . 1.884(2) yes Si3 . C24 . 1.859(2) yes Si3 . C25 . 1.871(2) yes Si3 . C26 . 1.858(2) yes Si4 . C27 . 1.863(2) yes Si4 . C28 . 1.880(2) yes Si4 . C29 . 1.875(2) yes C1 . C2 . 1.508(2) yes C3 . C4 . 1.505(3) yes C5 . C6 . 1.497(3) yes C6 . C7 . 1.390(2) yes C7 . C8 . 1.372(3) yes C8 . C9 . 1.382(3) yes C9 . C10 . 1.385(2) yes C17 . C18 . 1.503(2) yes C18 . C19 . 1.396(2) yes C18 . C23 . 1.393(2) yes C19 . C20 . 1.390(2) yes C20 . C21 . 1.378(3) yes C21 . C22 . 1.379(3) yes C22 . C23 . 1.390(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Sc1 . N2 . 131.02(5) yes N1 . Sc1 . N3 . 113.18(5) yes N2 . Sc1 . N3 . 88.10(5) yes N1 . Sc1 . N4 . 73.82(5) yes N2 . Sc1 . N4 . 74.41(5) yes N3 . Sc1 . N4 . 68.63(5) yes N1 . Sc1 . N5 . 97.64(5) yes N2 . Sc1 . N5 . 91.26(5) yes N3 . Sc1 . N5 . 139.20(5) yes N4 . Sc1 . N5 . 149.31(5) yes N1 . Sc1 . N6 . 106.81(5) yes N2 . Sc1 . N6 . 119.14(5) yes N3 . Sc1 . N6 . 84.79(4) yes N4 . Sc1 . N6 . 150.31(5) yes N5 . Sc1 . N6 . 60.26(4) yes Sc1 . N1 . Si1 . 131.92(7) yes Sc1 . N1 . C1 . 120.4(1) yes Si1 . N1 . C1 . 107.6(1) yes Sc1 . N2 . Si2 . 130.38(7) yes Sc1 . N2 . C3 . 114.0(1) yes Si2 . N2 . C3 . 112.7(1) yes Sc1 . N3 . C6 . 118.3(1) yes Sc1 . N3 . C10 . 122.4(1) yes C6 . N3 . C10 . 118.0(1) yes Sc1 . N4 . C2 . 105.20(9) yes Sc1 . N4 . C4 . 109.0(1) yes C2 . N4 . C4 . 110.2(1) yes Sc1 . N4 . C5 . 109.5(1) yes C2 . N4 . C5 . 111.6(1) yes C4 . N4 . C5 . 111.2(1) yes Sc1 . N5 . Si3 . 133.33(7) yes Sc1 . N5 . C17 . 91.45(9) yes Si3 . N5 . C17 . 133.5(1) yes Sc1 . N6 . Si4 . 139.89(7) yes Sc1 . N6 . C17 . 90.37(8) yes Si4 . N6 . C17 . 127.1(1) yes N1 . Si1 . C11 . 114.32(7) yes N1 . Si1 . C12 . 111.36(8) yes C11 . Si1 . C12 . 107.68(9) yes N1 . Si1 . C13 . 110.48(9) yes C11 . Si1 . C13 . 105.7(1) yes C12 . Si1 . C13 . 106.9(1) yes N2 . Si2 . C14 . 113.30(9) yes N2 . Si2 . C15 . 110.14(7) yes C14 . Si2 . C15 . 106.6(1) yes N2 . Si2 . C16 . 111.97(9) yes C14 . Si2 . C16 . 105.3(1) yes C15 . Si2 . C16 . 109.3(1) yes N5 . Si3 . C24 . 112.59(9) yes N5 . Si3 . C25 . 113.39(9) yes C24 . Si3 . C25 . 108.1(1) yes N5 . Si3 . C26 . 106.99(7) yes C24 . Si3 . C26 . 109.5(1) yes C25 . Si3 . C26 . 106.0(1) yes N6 . Si4 . C27 . 105.41(7) yes N6 . Si4 . C28 . 114.36(8) yes C27 . Si4 . C28 . 108.8(1) yes N6 . Si4 . C29 . 114.53(7) yes C27 . Si4 . C29 . 108.35(8) yes C28 . Si4 . C29 . 105.20(9) yes N1 . C1 . C2 . 110.1(1) yes N4 . C2 . C1 . 109.3(1) yes N2 . C3 . C4 . 109.6(1) yes N4 . C4 . C3 . 108.3(1) yes N4 . C5 . C6 . 109.4(1) yes N3 . C6 . C5 . 115.6(1) yes N3 . C6 . C7 . 121.8(2) yes C5 . C6 . C7 . 122.6(2) yes C6 . C7 . C8 . 119.7(2) yes C7 . C8 . C9 . 118.8(2) yes C8 . C9 . C10 . 118.7(2) yes N3 . C10 . C9 . 123.0(2) yes N5 . C17 . N6 . 117.3(1) yes N5 . C17 . C18 . 122.3(1) yes N6 . C17 . C18 . 120.4(1) yes C17 . C18 . C19 . 120.1(1) yes C17 . C18 . C23 . 121.0(1) yes C19 . C18 . C23 . 118.9(2) yes C18 . C19 . C20 . 120.1(2) yes C19 . C20 . C21 . 120.6(2) yes C20 . C21 . C22 . 119.7(2) yes C21 . C22 . C23 . 120.4(2) yes C18 . C23 . C22 . 120.4(2) yes #===end data_compound_12 _database_code_CSD 176541 # Local code MEGS23 _publ_section_exptl_refinement ; no special details ; _chemical_name_systematic ; [Y{PhC(NSiMe3)2}(N2NN')] ; _cell_length_a 11.4020(3) _cell_angle_alpha 90 _cell_length_b 20.0640(7) _cell_angle_beta 93.423(2) _cell_length_c 16.8640(5) _cell_angle_gamma 90 _cell_volume 3851.1(5) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Y ' -2.9510 3.5420 17.7760 1.4029 10.2946 12.8006 5.7263 0.1256 3.2659 104.3540 1.9121 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C29 H55 Y1 N6 Si4 ' _chemical_formula_moiety ' C29 H55 Y1 N6 Si4 ' _chemical_compound_source ; [Y(N2NN')Cl(py)].(1.5 LiCl) + Li(PhC{NSiMe3}2) ; _chemical_formula_weight 689.05 _cell_measurement_reflns_used 17138 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 175 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.40 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_max 0.60 _exptl_crystal_density_diffrn 1.19 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 1.67 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.436 _exptl_absorpt_correction_T_max 0.670 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_measurement_device-type 'Enraf-nonius DIP2000' _diffrn_ambient_temperature 175 _diffrn_reflns_number 17138 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.40 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens 'geometric' _reflns_number_total 7865 _reflns_number_observed 4702 _reflns_observed_criterion >3.00\s(I) _refine_ls_number_reflns 4702 _refine_diff_density_min -0.28 _refine_diff_density_max 0.28 _refine_ls_number_parameters 361 _refine_ls_R_factor_obs 0.0276 _refine_ls_wR_factor_obs 0.0360 _refine_ls_goodness_of_fit_obs 0.9922 _refine_ls_shift/esd_max 0.0007 _refine_ls_structure_factor_coef F _refine_ls_hydrogen_treatment riding _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Unit weights' _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_extinction_method 'None' _refine_ls_extinction_coef none _computing_data_collection 'DIP2000 software Xpress (MAC Science, 1989)' _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Y1 0.56751(3) 0.115014(17) 0.289202(19) 0.0236 1.0000 Uani N1 0.4685(3) 0.01813(15) 0.30054(18) 0.0330 1.0000 Uani N2 0.5997(3) 0.19445(15) 0.38291(17) 0.0347 1.0000 Uani N3 0.4399(3) 0.19915(14) 0.21349(19) 0.0343 1.0000 Uani N4 0.3745(3) 0.13873(15) 0.35362(19) 0.0378 1.0000 Uani N5 0.7665(2) 0.07855(15) 0.29802(16) 0.0302 1.0000 Uani N6 0.6873(2) 0.11150(15) 0.17625(15) 0.0266 1.0000 Uani Si1 0.5010(1) -0.05868(5) 0.26351(6) 0.0336 1.0000 Uani Si2 0.6752(1) 0.26678(5) 0.37491(7) 0.0389 1.0000 Uani Si3 0.8610(1) 0.05863(7) 0.37827(6) 0.0421 1.0000 Uani Si4 0.67020(9) 0.10889(6) 0.07317(5) 0.0322 1.0000 Uani C1 0.3560(4) 0.0167(2) 0.3397(3) 0.0463 1.0000 Uani C2 0.3450(4) 0.0762(2) 0.3939(3) 0.0458 1.0000 Uani C3 0.5182(4) 0.1921(2) 0.4470(2) 0.0463 1.0000 Uani C4 0.3919(4) 0.1935(2) 0.4122(3) 0.0486 1.0000 Uani C5 0.2840(3) 0.1567(2) 0.2910(3) 0.0475 1.0000 Uani C6 0.3298(3) 0.2087(2) 0.2362(2) 0.0416 1.0000 Uani C7 0.2640(4) 0.2636(2) 0.2100(3) 0.0565 1.0000 Uani C8 0.3107(5) 0.3088(2) 0.1604(3) 0.0626 1.0000 Uani C9 0.4230(4) 0.2999(2) 0.1371(3) 0.0513 1.0000 Uani C10 0.4837(4) 0.2447(2) 0.1645(2) 0.0405 1.0000 Uani C11 0.6338(4) -0.05636(19) 0.2043(3) 0.0480 1.0000 Uani C12 0.5279(4) -0.1224(2) 0.3438(2) 0.0519 1.0000 Uani C13 0.3770(4) -0.0909(2) 0.1956(3) 0.0594 1.0000 Uani C14 0.7788(4) 0.2847(3) 0.4625(3) 0.0643 1.0000 Uani C15 0.7648(4) 0.2618(2) 0.2858(2) 0.0506 1.0000 Uani C16 0.5761(5) 0.3415(2) 0.3654(3) 0.0633 1.0000 Uani C17 0.7815(3) 0.09305(17) 0.2223(2) 0.0266 1.0000 Uani C18 0.8998(3) 0.08948(18) 0.1887(2) 0.0308 1.0000 Uani C19 0.9499(3) 0.1464(2) 0.1576(2) 0.0399 1.0000 Uani C20 1.0567(4) 0.1427(3) 0.1233(3) 0.0531 1.0000 Uani C21 1.1134(4) 0.0820(3) 0.1183(3) 0.0602 1.0000 Uani C22 1.0657(4) 0.0256(3) 0.1492(3) 0.0527 1.0000 Uani C23 0.9595(3) 0.0291(2) 0.1847(2) 0.0405 1.0000 Uani C24 0.9891(4) 0.1153(4) 0.3889(3) 0.0842 1.0000 Uani C25 0.9160(6) -0.0288(3) 0.3763(3) 0.0970 1.0000 Uani C26 0.7740(4) 0.0658(2) 0.4672(2) 0.0517 1.0000 Uani C27 0.5120(3) 0.0901(2) 0.0500(2) 0.0438 1.0000 Uani C28 0.7066(4) 0.1893(2) 0.0240(3) 0.0557 1.0000 Uani C29 0.7591(4) 0.0427(2) 0.0264(2) 0.0467 1.0000 Uani H11 0.3509 -0.0254 0.3709 0.0596 1.0000 Uiso H12 0.2899 0.0183 0.2979 0.0596 1.0000 Uiso H21 0.4013 0.0700 0.4411 0.0580 1.0000 Uiso H22 0.2631 0.0790 0.4117 0.0580 1.0000 Uiso H31 0.5332 0.2309 0.4834 0.0581 1.0000 Uiso H32 0.5309 0.1497 0.4774 0.0581 1.0000 Uiso H41 0.3357 0.1886 0.4551 0.0602 1.0000 Uiso H42 0.3777 0.2371 0.3844 0.0602 1.0000 Uiso H51 0.2129 0.1743 0.3158 0.0593 1.0000 Uiso H52 0.2624 0.1158 0.2594 0.0593 1.0000 Uiso H71 0.1824 0.2696 0.2275 0.0671 1.0000 Uiso H81 0.2642 0.3488 0.1420 0.0738 1.0000 Uiso H91 0.4586 0.3324 0.1006 0.0639 1.0000 Uiso H101 0.5655 0.2378 0.1476 0.0482 1.0000 Uiso H111 0.6501 -0.10193 0.1837 0.0613 1.0000 Uiso H112 0.7026 -0.04083 0.2391 0.0613 1.0000 Uiso H113 0.6202 -0.02485 0.1588 0.0613 1.0000 Uiso H121 0.5466 -0.1662 0.3193 0.0634 1.0000 Uiso H122 0.5956 -0.1079 0.3802 0.0634 1.0000 Uiso H123 0.4561 -0.1270 0.3746 0.0634 1.0000 Uiso H131 0.3983 -0.1357 0.1748 0.0786 1.0000 Uiso H132 0.3042 -0.0948 0.2256 0.0786 1.0000 Uiso H133 0.3626 -0.0593 0.1502 0.0786 1.0000 Uiso H141 0.8206 0.3277 0.4541 0.0771 1.0000 Uiso H142 0.8375 0.2478 0.4690 0.0771 1.0000 Uiso H143 0.7335 0.2880 0.5113 0.0771 1.0000 Uiso H151 0.8100 0.3041 0.2806 0.0631 1.0000 Uiso H152 0.8208 0.2235 0.2922 0.0631 1.0000 Uiso H153 0.7118 0.2549 0.2371 0.0631 1.0000 Uiso H161 0.6248 0.3826 0.3609 0.0753 1.0000 Uiso H162 0.5289 0.3448 0.4133 0.0753 1.0000 Uiso H163 0.5221 0.3368 0.3168 0.0753 1.0000 Uiso H191 0.9081 0.1900 0.1606 0.0498 1.0000 Uiso H201 1.0933 0.1837 0.1019 0.0656 1.0000 Uiso H211 1.1895 0.0793 0.0920 0.0710 1.0000 Uiso H221 1.1080 -0.0179 0.1461 0.0632 1.0000 Uiso H231 0.9247 -0.0119 0.2075 0.0490 1.0000 Uiso H241 1.0413 0.1019 0.4360 0.1003 1.0000 Uiso H242 1.0345 0.1136 0.3400 0.1003 1.0000 Uiso H243 0.9598 0.1617 0.3967 0.1003 1.0000 Uiso H251 0.9700 -0.0373 0.4241 0.1128 1.0000 Uiso H252 0.9592 -0.0362 0.3271 0.1128 1.0000 Uiso H253 0.8475 -0.0599 0.3765 0.1128 1.0000 Uiso H261 0.8245 0.0547 0.5159 0.0642 1.0000 Uiso H262 0.7440 0.1124 0.4713 0.0642 1.0000 Uiso H263 0.7061 0.0342 0.4621 0.0642 1.0000 Uiso H271 0.4957 0.0879 -0.0089 0.0517 1.0000 Uiso H272 0.4629 0.1260 0.0724 0.0517 1.0000 Uiso H273 0.4924 0.0464 0.0742 0.0517 1.0000 Uiso H281 0.6953 0.1847 -0.0350 0.0680 1.0000 Uiso H282 0.7902 0.2013 0.0387 0.0680 1.0000 Uiso H283 0.6538 0.2252 0.0425 0.0680 1.0000 Uiso H291 0.7449 0.0443 -0.0326 0.0562 1.0000 Uiso H292 0.8445 0.0504 0.0408 0.0562 1.0000 Uiso H293 0.7356 -0.0020 0.0464 0.0562 1.0000 Uiso 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 Y1 0.02281(15) 0.02493(16) 0.02357(15) -0.00033(16) 0.00627(11) -0.00066(16) N1 0.0319(17) 0.0305(17) 0.0379(17) -0.0009(14) 0.0123(14) -0.0039(13) N2 0.0425(18) 0.0339(17) 0.0284(16) -0.0050(13) 0.0065(13) -0.0036(14) N3 0.0320(16) 0.0330(16) 0.0379(17) -0.0036(15) 0.0020(13) 0.0049(14) N4 0.0354(18) 0.0340(17) 0.0455(19) -0.0040(15) 0.0144(15) -0.0017(14) N5 0.0280(16) 0.0372(17) 0.0256(15) 0.0055(13) 0.0034(12) 0.0040(13) N6 0.0282(14) 0.0285(15) 0.0233(13) 0.0008(13) 0.0030(11) 0.0002(13) Si1 0.0459(6) 0.0261(5) 0.0295(5) 0.0027(4) 0.0074(5) -0.0025(5) Si2 0.0470(7) 0.0333(6) 0.0365(6) -0.0066(5) 0.0032(5) -0.0083(5) Si3 0.0332(6) 0.0643(8) 0.0287(5) 0.0076(5) -0.0001(4) 0.0110(5) Si4 0.0387(5) 0.0359(6) 0.0221(5) 0.0025(4) 0.0032(4) 0.0019(5) C1 0.043(2) 0.035(2) 0.063(3) -0.001(2) 0.022(2) -0.0066(18) C2 0.041(2) 0.043(2) 0.056(3) -0.001(2) 0.028(2) -0.0034(19) C3 0.061(3) 0.046(3) 0.033(2) -0.0097(19) 0.016(2) -0.009(2) C4 0.054(3) 0.043(2) 0.052(3) -0.012(2) 0.028(2) 0.001(2) C5 0.024(2) 0.048(3) 0.071(3) -0.004(2) 0.011(2) 0.0041(18) C6 0.033(2) 0.041(2) 0.050(2) -0.0061(19) 0.0026(18) 0.0047(18) C7 0.042(3) 0.057(3) 0.071(3) -0.003(3) 0.003(2) 0.019(2) C8 0.072(3) 0.047(3) 0.068(3) 0.008(2) -0.001(3) 0.024(2) C9 0.066(3) 0.041(3) 0.047(3) 0.004(2) -0.001(2) 0.007(2) C10 0.043(2) 0.041(2) 0.038(2) 0.0000(18) 0.0031(18) 0.0030(18) C11 0.066(3) 0.027(2) 0.054(3) -0.0014(18) 0.026(2) 0.0036(19) C12 0.066(3) 0.047(3) 0.044(2) 0.015(2) 0.013(2) 0.006(2) C13 0.080(4) 0.053(3) 0.044(3) -0.003(2) -0.005(2) -0.014(2) C14 0.063(3) 0.073(4) 0.056(3) -0.018(3) -0.007(2) -0.018(3) C15 0.061(3) 0.045(3) 0.047(3) -0.006(2) 0.015(2) -0.020(2) C16 0.079(4) 0.038(3) 0.073(3) -0.007(2) 0.008(3) -0.000(2) C17 0.0257(18) 0.0278(18) 0.0270(18) -0.0009(14) 0.0065(14) -0.0010(13) C18 0.0279(18) 0.041(2) 0.0237(17) -0.0040(15) 0.0027(14) -0.0010(15) C19 0.033(2) 0.051(2) 0.036(2) -0.0008(19) 0.0097(17) -0.0060(18) C20 0.043(3) 0.069(3) 0.049(3) -0.003(2) 0.015(2) -0.016(2) C21 0.032(2) 0.097(4) 0.053(3) -0.011(3) 0.016(2) 0.000(3) C22 0.035(2) 0.070(3) 0.054(3) -0.011(2) 0.009(2) 0.012(2) C23 0.032(2) 0.050(2) 0.039(2) -0.0055(18) 0.0051(17) 0.0071(18) C24 0.038(3) 0.162(6) 0.052(3) 0.016(4) -0.008(2) -0.025(3) C25 0.133(6) 0.106(5) 0.050(3) 0.007(3) -0.014(3) 0.074(4) C26 0.049(3) 0.076(3) 0.031(2) 0.014(2) 0.0024(19) 0.005(2) C27 0.048(2) 0.048(2) 0.034(2) -0.0039(18) -0.0104(18) 0.0079(19) C28 0.076(3) 0.054(3) 0.039(2) 0.015(2) 0.012(2) -0.006(2) C29 0.052(3) 0.060(3) 0.029(2) -0.009(2) 0.0042(18) 0.009(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Y1 . N1 . 2.262(3) yes Y1 . N2 . 2.259(3) yes Y1 . N3 . 2.525(3) yes Y1 . N4 . 2.557(3) yes Y1 . N5 . 2.380(3) yes Y1 . N6 . 2.410(3) yes Y1 . C17 . 2.783(3) yes N1 . Si1 . 1.712(3) yes N1 . C1 . 1.477(5) yes N2 . Si2 . 1.696(3) yes N2 . C3 . 1.468(4) yes N3 . C6 . 1.348(5) yes N3 . C10 . 1.347(5) yes N4 . C2 . 1.475(5) yes N4 . C4 . 1.483(5) yes N4 . C5 . 1.476(5) yes N5 . Si3 . 1.726(3) yes N5 . C17 . 1.330(4) yes N6 . Si4 . 1.738(3) yes N6 . C17 . 1.340(4) yes Si1 . C11 . 1.863(4) yes Si1 . C12 . 1.874(4) yes Si1 . C13 . 1.880(4) yes Si2 . C14 . 1.870(4) yes Si2 . C15 . 1.870(4) yes Si2 . C16 . 1.878(5) yes Si3 . C24 . 1.851(5) yes Si3 . C25 . 1.863(5) yes Si3 . C26 . 1.852(4) yes Si4 . C27 . 1.861(4) yes Si4 . C28 . 1.873(4) yes Si4 . C29 . 1.873(4) yes C1 . C2 . 1.513(5) yes C3 . C4 . 1.522(6) yes C5 . C6 . 1.507(6) yes C6 . C7 . 1.391(6) yes C7 . C8 . 1.363(7) yes C8 . C9 . 1.374(6) yes C9 . C10 . 1.372(6) yes C17 . C18 . 1.496(5) yes C18 . C19 . 1.392(5) yes C18 . C23 . 1.394(5) yes C19 . C20 . 1.382(5) yes C20 . C21 . 1.383(7) yes C21 . C22 . 1.372(7) yes C22 . C23 . 1.384(5) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Y1 . N2 . 127.5(1) yes N1 . Y1 . N3 . 110.00(11) yes N2 . Y1 . N3 . 86.95(11) yes N1 . Y1 . N4 . 71.2(1) yes N2 . Y1 . N4 . 71.3(1) yes N3 . Y1 . N4 . 66.8(1) yes N1 . Y1 . N5 . 102.1(1) yes N2 . Y1 . N5 . 93.35(11) yes N3 . Y1 . N5 . 139.1(1) yes N4 . Y1 . N5 . 150.7(1) yes N1 . Y1 . N6 . 110.5(1) yes N2 . Y1 . N6 . 119.8(1) yes N3 . Y1 . N6 . 87.5(1) yes N4 . Y1 . N6 . 152.1(1) yes N5 . Y1 . N6 . 57.14(9) yes N1 . Y1 . C17 . 110.6(1) yes N2 . Y1 . C17 . 106.6(1) yes N3 . Y1 . C17 . 113.2(1) yes N4 . Y1 . C17 . 177.9(1) yes N5 . Y1 . C17 . 28.51(9) yes N6 . Y1 . C17 . 28.76(9) yes Y1 . N1 . Si1 . 128.51(15) yes Y1 . N1 . C1 . 120.4(2) yes Si1 . N1 . C1 . 111.0(2) yes Y1 . N2 . Si2 . 127.59(16) yes Y1 . N2 . C3 . 114.1(2) yes Si2 . N2 . C3 . 115.6(2) yes Y1 . N3 . C6 . 118.0(3) yes Y1 . N3 . C10 . 122.7(3) yes C6 . N3 . C10 . 117.6(3) yes Y1 . N4 . C2 . 105.2(2) yes Y1 . N4 . C4 . 109.6(2) yes C2 . N4 . C4 . 110.5(3) yes Y1 . N4 . C5 . 108.9(2) yes C2 . N4 . C5 . 111.6(3) yes C4 . N4 . C5 . 110.8(3) yes Y1 . N5 . Si3 . 131.95(15) yes Y1 . N5 . C17 . 92.8(2) yes Si3 . N5 . C17 . 133.9(2) yes Y1 . N6 . Si4 . 139.14(14) yes Y1 . N6 . C17 . 91.29(19) yes Si4 . N6 . C17 . 127.5(2) yes N1 . Si1 . C11 . 111.95(16) yes N1 . Si1 . C12 . 112.33(18) yes C11 . Si1 . C12 . 107.5(2) yes N1 . Si1 . C13 . 111.1(2) yes C11 . Si1 . C13 . 106.8(2) yes C12 . Si1 . C13 . 106.9(2) yes N2 . Si2 . C14 . 113.6(2) yes N2 . Si2 . C15 . 108.80(17) yes C14 . Si2 . C15 . 107.1(2) yes N2 . Si2 . C16 . 112.61(19) yes C14 . Si2 . C16 . 105.2(2) yes C15 . Si2 . C16 . 109.2(2) yes N5 . Si3 . C24 . 112.7(2) yes N5 . Si3 . C25 . 113.5(2) yes C24 . Si3 . C25 . 108.4(3) yes N5 . Si3 . C26 . 106.08(17) yes C24 . Si3 . C26 . 109.4(2) yes C25 . Si3 . C26 . 106.5(2) yes N6 . Si4 . C27 . 105.41(16) yes N6 . Si4 . C28 . 113.72(18) yes C27 . Si4 . C28 . 108.6(2) yes N6 . Si4 . C29 . 114.27(16) yes C27 . Si4 . C29 . 108.09(19) yes C28 . Si4 . C29 . 106.6(2) yes N1 . C1 . C2 . 111.1(3) yes N4 . C2 . C1 . 111.3(3) yes N2 . C3 . C4 . 110.0(3) yes N4 . C4 . C3 . 109.2(3) yes N4 . C5 . C6 . 110.8(3) yes N3 . C6 . C5 . 116.0(3) yes N3 . C6 . C7 . 121.1(4) yes C5 . C6 . C7 . 122.9(4) yes C6 . C7 . C8 . 119.9(4) yes C7 . C8 . C9 . 119.6(4) yes C8 . C9 . C10 . 118.0(4) yes N3 . C10 . C9 . 123.7(4) yes N5 . C17 . N6 . 118.2(3) yes Y1 . C17 . C18 . 173.4(2) yes N5 . C17 . C18 . 121.6(3) yes N6 . C17 . C18 . 120.2(3) yes C17 . C18 . C19 . 120.2(3) yes C17 . C18 . C23 . 120.9(3) yes C19 . C18 . C23 . 118.8(3) yes C18 . C19 . C20 . 120.4(4) yes C19 . C20 . C21 . 119.9(4) yes C20 . C21 . C22 . 120.4(4) yes C21 . C22 . C23 . 120.0(4) yes C18 . C23 . C22 . 120.4(4) yes #===end data_COMPOUND_7 _database_code_CSD 170227 # Local code MEGS27 _chemical_name_systematic ; [Sc(CH2SiMe3)(N2NN')] ; _publ_section_exptl_refinement ; NO SPECIAL DETAILS ; _cell_length_a 12.131(1) _cell_angle_alpha 90 _cell_length_b 13.069(1) _cell_angle_beta 90 _cell_length_c 17.548(1) _cell_angle_gamma 90 _cell_volume 2782.0(3) _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,-y+1/2,-z' '-x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Sc ' 0.2260 0.3720 9.1890 9.0213 7.3679 0.5729 1.6409 136.1080 1.4680 51.3531 1.3329 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C20 H43 Sc1 N4 Si3 ' _chemical_formula_moiety ' C20 H43 Sc1 N4 Si3 ' _chemical_compound_source ; [Sc(N2NN')Cl] + LiCH2SiMe3 ; _chemical_formula_weight 468.81 _cell_measurement_reflns_used 15716 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 175 _cell_formula_units_Z 4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.45 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.12 _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.40 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.887 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_method \w _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator graphite _diffrn_measurement_device-type 'Enraf-nonius DIP2000' _diffrn_ambient_temperature 175 _diffrn_reflns_number 15718 _reflns_number_total 5422 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_observed 5037 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.42 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_ls_hydrogen_treatment 'riding model and U[iso]' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens 'diff maps and geometric' _reflns_observed_criterion >3.00\s(I) _refine_ls_number_reflns 5037 _refine_diff_density_min -0.45 _refine_diff_density_max 0.45 _refine_ls_number_parameters 253 _refine_ls_R_factor_obs 0.0299 _refine_ls_wR_factor_obs 0.0372 _refine_ls_goodness_of_fit_obs 1.0841 _refine_ls_shift/esd_max 0.0018 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc' _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.65 0.716 1.20 ; _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack 0.03 (.05) _refine_ls_extinction_coef none _refine_ls_extinction_method none _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_data_collection 'DIP2000 software Xpress (MAC Science, 1989)' _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Sc1 0.24823(2) 0.02595(2) 0.645239(15) 0.0252 1.0000 Uani N1 0.31074(14) -0.11450(13) 0.67944(9) 0.0351 1.0000 Uani N2 0.07833(12) 0.02525(14) 0.64690(8) 0.0354 1.0000 Uani N3 0.28766(13) 0.18871(13) 0.69349(9) 0.0347 1.0000 Uani N4 0.22034(13) 0.02807(14) 0.77836(8) 0.0369 1.0000 Uani Si1 0.28421(6) -0.22852(5) 0.63535(3) 0.0430 1.0000 Uani Si2 -0.01792(5) 0.02870(8) 0.57642(3) 0.0582 1.0000 Uani Si3 0.48805(4) 0.06143(5) 0.53805(3) 0.0369 1.0000 Uani C1 0.3388(2) -0.12078(18) 0.76063(12) 0.0449 1.0000 Uani C2 0.2454(2) -0.07512(17) 0.80752(9) 0.0461 1.0000 Uani C3 0.03418(17) 0.00204(19) 0.72369(11) 0.0458 1.0000 Uani C4 0.10149(17) 0.0558(2) 0.78529(11) 0.0452 1.0000 Uani C5 0.28910(19) 0.10513(18) 0.81635(11) 0.0447 1.0000 Uani C6 0.29639(17) 0.20088(17) 0.76967(12) 0.0403 1.0000 Uani C7 0.3133(2) 0.2957(2) 0.80275(15) 0.0548 1.0000 Uani C8 0.3202(2) 0.3810(2) 0.75602(19) 0.0656 1.0000 Uani C9 0.3108(2) 0.36970(19) 0.67857(18) 0.0577 1.0000 Uani C10 0.29447(18) 0.27261(17) 0.64968(14) 0.0448 1.0000 Uani C11 0.2447(2) -0.20294(16) 0.53401(12) 0.0471 1.0000 Uani C12 0.4063(3) -0.3183(2) 0.63876(16) 0.0665 1.0000 Uani C13 0.1667(3) -0.2999(3) 0.68040(19) 0.0870 1.0000 Uani C14 0.04828(19) 0.0567(3) 0.48258(12) 0.0589 1.0000 Uani C15 -0.0907(3) -0.0966(4) 0.56906(19) 0.1224 1.0000 Uani C16 -0.1271(3) 0.1271(5) 0.59406(19) 0.1140 1.0000 Uani C17 0.33699(14) 0.06518(14) 0.5339(1) 0.0293 1.0000 Uani C18 0.5410(2) 0.1180(3) 0.62968(17) 0.0684 1.0000 Uani C19 0.5627(3) 0.1287(3) 0.4595(2) 0.0770 1.0000 Uani C20 0.5401(2) -0.0731(2) 0.53426(17) 0.0591 1.0000 Uani H11 0.3497 -0.19404 0.77528 0.0539 1.0000 Uiso H12 0.4083 -0.08173 0.77043 0.0539 1.0000 Uiso H21 0.2681 -0.07068 0.86220 0.0559 1.0000 Uiso H22 0.1785 -0.11939 0.80302 0.0559 1.0000 Uiso H31 0.03692 -0.07354 0.73237 0.0545 1.0000 Uiso H32 -0.04398 0.02603 0.72666 0.0545 1.0000 Uiso H41 0.07390 0.0343 0.83655 0.0543 1.0000 Uiso H42 0.09309 0.1315 0.77963 0.0543 1.0000 Uiso H51 0.25600 0.12203 0.86701 0.0536 1.0000 Uiso H52 0.36489 0.07681 0.82390 0.0536 1.0000 Uiso H71 0.3203 0.3026 0.85930 0.0655 1.0000 Uiso H81 0.3324 0.4503 0.77860 0.0787 1.0000 Uiso H91 0.3150 0.43041 0.64401 0.0696 1.0000 Uiso H101 0.28788 0.26441 0.59321 0.0538 1.0000 Uiso H111 0.2290 -0.26923 0.50770 0.0569 1.0000 Uiso H112 0.3067 -0.16719 0.50751 0.0569 1.0000 Uiso H113 0.1774 -0.15879 0.53266 0.0569 1.0000 Uiso H121 0.3871 -0.3837 0.61238 0.0800 1.0000 Uiso H122 0.4259 -0.3328 0.69305 0.0800 1.0000 Uiso H123 0.4706 -0.2857 0.61260 0.0800 1.0000 Uiso H131 0.1547 -0.3657 0.65252 0.1035 1.0000 Uiso H132 0.1844 -0.3147 0.73496 0.1035 1.0000 Uiso H133 0.0983 -0.2573 0.67755 0.1035 1.0000 Uiso H141 -0.00932 0.0585 0.44183 0.0725 1.0000 Uiso H142 0.08607 0.1246 0.48525 0.0725 1.0000 Uiso H143 0.10355 0.0023 0.47050 0.0725 1.0000 Uiso H151 -0.1469 -0.0934 0.52745 0.1469 1.0000 Uiso H152 -0.1280 -0.1121 0.61853 0.1469 1.0000 Uiso H153 -0.0359 -0.1515 0.55736 0.1469 1.0000 Uiso H161 -0.1815 0.1263 0.55126 0.1372 1.0000 Uiso H162 -0.1657 0.1114 0.64302 0.1372 1.0000 Uiso H163 -0.0922 0.1963 0.59739 0.1372 1.0000 Uiso H181 0.6234 0.1149 0.63016 0.0843 1.0000 Uiso H182 0.5112 0.0781 0.67373 0.0843 1.0000 Uiso H183 0.5167 0.1909 0.63386 0.0843 1.0000 Uiso H191 0.6440 0.1218 0.4674 0.0938 1.0000 Uiso H192 0.5421 0.2028 0.4596 0.0938 1.0000 Uiso H193 0.5420 0.0974 0.4095 0.0938 1.0000 Uiso H201 0.6225 -0.0730 0.53654 0.0711 1.0000 Uiso H202 0.5100 -0.1124 0.57851 0.0711 1.0000 Uiso H203 0.5154 -0.1058 0.48565 0.0711 1.0000 Uiso H171 0.31443 0.13582 0.5186 0.0385 1.0000 Uiso H172 0.31239 0.01523 0.4943 0.0385 1.0000 Uiso 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 Sc1 0.02424(13) 0.03211(17) 0.01938(13) -0.00086(11) -0.00057(12) -0.00103(13) N1 0.047(1) 0.0341(9) 0.0248(7) 0.0013(6) -0.0023(6) 0.0010(7) N2 0.0246(6) 0.055(1) 0.0266(7) -0.0074(7) 0.0015(5) -0.0047(6) N3 0.0297(7) 0.0380(9) 0.0366(8) -0.0075(6) -0.0028(6) 0.0028(6) N4 0.0395(8) 0.049(1) 0.0222(6) -0.0042(6) -0.0004(6) 0.0006(7) Si1 0.0656(4) 0.0311(3) 0.0324(3) 0.0046(2) -0.0028(2) -0.0078(2) Si2 0.0242(2) 0.1188(6) 0.0317(3) -0.0103(3) -0.0009(2) -0.0098(3) Si3 0.0279(2) 0.0474(3) 0.0355(3) -0.0041(2) 0.0046(2) -0.0038(2) C1 0.0594(13) 0.0434(13) 0.032(1) 0.0062(8) -0.0098(9) 0.008(1) C2 0.0633(12) 0.0551(13) 0.0200(8) 0.0058(7) -0.0004(9) -0.0009(11) C3 0.0357(9) 0.0699(16) 0.0318(9) -0.0045(9) 0.0077(8) -0.0072(9) C4 0.040(1) 0.0693(15) 0.0265(9) -0.0065(9) 0.0088(8) -0.0004(9) C5 0.0508(11) 0.0581(14) 0.0253(8) -0.0106(8) -0.0085(8) 0.0018(9) C6 0.0318(8) 0.0500(13) 0.039(1) -0.0148(8) -0.0053(8) 0.0020(8) C7 0.0531(13) 0.0542(16) 0.0571(14) -0.0242(11) -0.0060(11) -0.001(1) C8 0.0635(16) 0.0481(17) 0.085(2) -0.0308(14) -0.0023(14) -0.0013(11) C9 0.0570(15) 0.0353(14) 0.0808(18) -0.0058(11) 0.0007(12) 0.002(1) C10 0.044(1) 0.0385(12) 0.0514(12) -0.006(1) -0.000(1) 0.0036(9) C11 0.0672(13) 0.0367(11) 0.0376(9) -0.0035(7) -0.0064(11) -0.007(1) C12 0.106(2) 0.0394(14) 0.0544(14) -0.0013(11) -0.0180(15) 0.0166(13) C13 0.119(3) 0.075(2) 0.0677(19) 0.0110(15) 0.0090(18) -0.048(2) C14 0.0379(11) 0.108(2) 0.031(1) -0.0007(11) -0.0042(8) 0.0045(12) C15 0.091(3) 0.221(5) 0.0560(17) -0.035(2) 0.0099(17) -0.102(3) C16 0.0430(15) 0.241(6) 0.0582(17) 0.009(2) 0.0038(13) 0.058(2) C17 0.0297(8) 0.0337(9) 0.0244(7) 0.0011(6) -0.0004(6) -0.0029(7) C18 0.0371(12) 0.102(2) 0.0665(16) -0.0363(16) -0.0102(11) -0.0009(12) C19 0.0608(16) 0.087(2) 0.084(2) 0.0139(17) 0.0258(15) -0.0246(15) C20 0.0433(12) 0.0625(17) 0.0716(16) -0.0022(13) 0.0044(11) 0.0162(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sc1 . N1 . 2.0748(17) yes Sc1 . N2 . 2.0613(14) yes Sc1 . N3 . 2.3388(17) yes Sc1 . N4 . 2.3606(14) yes Sc1 . C17 . 2.2885(17) yes N1 . Si1 . 1.7096(17) yes N1 . C1 . 1.467(2) yes N2 . Si2 . 1.7014(16) yes N2 . C3 . 1.481(2) yes N3 . C6 . 1.350(3) yes N3 . C10 . 1.342(3) yes N4 . C2 . 1.474(3) yes N4 . C4 . 1.492(3) yes N4 . C5 . 1.468(3) yes Si1 . C11 . 1.872(2) yes Si1 . C12 . 1.891(3) yes Si1 . C13 . 1.878(3) yes Si2 . C14 . 1.868(2) yes Si2 . C15 . 1.865(4) yes Si2 . C16 . 1.872(4) yes Si3 . C17 . 1.8347(17) yes Si3 . C18 . 1.883(3) yes Si3 . C19 . 1.869(3) yes Si3 . C20 . 1.869(3) yes C1 . C2 . 1.523(3) yes C3 . C4 . 1.526(3) yes C5 . C6 . 1.498(3) yes C6 . C7 . 1.384(3) yes C7 . C8 . 1.386(4) yes C8 . C9 . 1.372(4) yes C9 . C10 . 1.381(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Sc1 . N2 . 110.94(7) yes N1 . Sc1 . N3 . 128.69(6) yes N2 . Sc1 . N3 . 101.74(6) yes N1 . Sc1 . N4 . 77.08(6) yes N2 . Sc1 . N4 . 80.96(6) yes N3 . Sc1 . N4 . 70.15(6) yes N1 . Sc1 . C17 . 105.85(6) yes N2 . Sc1 . C17 . 118.91(6) yes N3 . Sc1 . C17 . 90.52(6) yes N4 . Sc1 . C17 . 155.43(6) yes Sc1 . N1 . Si1 . 124.85(9) yes Sc1 . N1 . C1 . 114.53(13) yes Si1 . N1 . C1 . 115.75(14) yes Sc1 . N2 . Si2 . 132.52(8) yes Sc1 . N2 . C3 . 112.04(12) yes Si2 . N2 . C3 . 114.74(12) yes Sc1 . N3 . C6 . 118.78(14) yes Sc1 . N3 . C10 . 123.26(13) yes C6 . N3 . C10 . 117.78(18) yes Sc1 . N4 . C2 . 107.66(11) yes Sc1 . N4 . C4 . 102.8(1) yes C2 . N4 . C4 . 113.14(18) yes Sc1 . N4 . C5 . 112.09(12) yes C2 . N4 . C5 . 110.68(16) yes C4 . N4 . C5 . 110.22(17) yes N1 . Si1 . C11 . 108.81(9) yes N1 . Si1 . C12 . 112.26(11) yes C11 . Si1 . C12 . 109.98(12) yes N1 . Si1 . C13 . 112.66(13) yes C11 . Si1 . C13 . 107.11(14) yes C12 . Si1 . C13 . 105.87(18) yes N2 . Si2 . C14 . 110.54(9) yes N2 . Si2 . C15 . 110.61(17) yes C14 . Si2 . C15 . 108.34(15) yes N2 . Si2 . C16 . 112.55(14) yes C14 . Si2 . C16 . 108.37(16) yes C15 . Si2 . C16 . 106.2(2) yes C17 . Si3 . C18 . 111.4(1) yes C17 . Si3 . C19 . 116.27(13) yes C18 . Si3 . C19 . 106.24(16) yes C17 . Si3 . C20 . 111.2(1) yes C18 . Si3 . C20 . 106.52(15) yes C19 . Si3 . C20 . 104.61(15) yes N1 . C1 . C2 . 109.28(17) yes N4 . C2 . C1 . 108.93(16) yes N2 . C3 . C4 . 110.90(16) yes N4 . C4 . C3 . 110.35(16) yes N4 . C5 . C6 . 110.99(16) yes N3 . C6 . C5 . 116.00(17) yes N3 . C6 . C7 . 122.2(2) yes C5 . C6 . C7 . 121.8(2) yes C6 . C7 . C8 . 118.7(2) yes C7 . C8 . C9 . 119.6(2) yes C8 . C9 . C10 . 118.3(3) yes N3 . C10 . C9 . 123.3(2) yes #===end