Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _audit_creation_date 02-09-24 _audit_creation_method CRYSTALS _journal_coden_Cambridge 186 loop_ _publ_author_name 'Philip Mountford' 'Stuart R. Dubberley' 'Lutz Gade' 'Aline Maisse-Francois' 'Benjamin D. Ward' _publ_contact_author_name 'Dr Philip Mountford' _publ_contact_author_address ; Inorganic Chemistry Laboratory Oxford University 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_requested_journal 'Dalton Transactions' _publ_section_title ; Scandium chloride, alkyl and phenyl complexes of diamido-donor ligands ; _publ_contact_letter ; These are the CIF format data (5 compounds) for the paper Scandium chloride, alkyl and phenyl complexes of diamide-donor ligands B D Ward, S R Dubberley, A Maisse-Francois, L H Gade and P. Mountford ; data_COMPOUND_1 _database_code_CSD 194287 # Local code BDW3 _chemical_name_systematic ; [Sc(N2_TMS_Npy)Cl(THF)] ; _publ_section_exptl_refinement ; No special details ; _cell_length_a 19.1126(4) _cell_length_b 13.1361(2) _cell_length_c 19.5217(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4901.2(2) _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P b c a ' 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' 'x,-y+1/2,z+1/2' '-x,y+1/2,-z+1/2' '-x+1/2,-y,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 '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' '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' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' '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' _chemical_formula_sum ' C19 H37 Cl1 N3 O1 Sc1 Si2 ' _chemical_formula_moiety ' C19 H37 Cl1 N3 O1 Sc1 Si2 ' _chemical_formula_weight 460.11 _cell_measurement_reflns_used 5869 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 8 _exptl_crystal_description 'block' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.25 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1972.17 _exptl_absorpt_coefficient_mu 0.52 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_T_max 0.925 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 150 _diffrn_reflns_number 11144 _reflns_number_total 5603 _diffrn_reflns_av_R_equivalents 2.30 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_gt 3439 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min 0 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _refine_diff_density_min -0.29 _refine_diff_density_max 0.29 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3439 _refine_ls_number_parameters 244 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0246 _refine_ls_goodness_of_fit_ref 1.0645 _refine_ls_shift/su_max 0.0011 _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_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_extinction_coef 'none required' _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 0.194 -.150 -.434E-01-.872E-01 ; _refine_ls_extinction_method 'None' _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD 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 'CAMERON (Watkin, Prout and Pearce, 1996)' _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 Sc1 0.882348(19) 0.24921(3) 0.42649(2) 0.0190 1.0000 Uani Cl1 0.81621(4) 0.39625(5) 0.38559(4) 0.0392 1.0000 Uani N1 0.87361(9) 0.14945(14) 0.50512(9) 0.0213 1.0000 Uani N2 0.98117(9) 0.21969(14) 0.39497(9) 0.0204 1.0000 Uani N3 0.9318(1) 0.34926(14) 0.50934(9) 0.0220 1.0000 Uani O1 0.82095(8) 0.15961(12) 0.35225(8) 0.0250 1.0000 Uani Si1 0.79821(3) 0.11512(5) 0.54688(3) 0.0220 1.0000 Uani Si2 1.01395(3) 0.21017(5) 0.31343(3) 0.0226 1.0000 Uani C1 0.9396(1) 0.12641(17) 0.54033(12) 0.0212 1.0000 Uani C2 1.00372(11) 0.19721(16) 0.52509(11) 0.0194 1.0000 Uani C3 1.02938(11) 0.18925(17) 0.44976(11) 0.0215 1.0000 Uani C4 1.06359(11) 0.15507(17) 0.56926(12) 0.0243 1.0000 Uani C5 0.98635(12) 0.30680(16) 0.54333(11) 0.0208 1.0000 Uani C6 1.02275(13) 0.36349(18) 0.59207(12) 0.0280 1.0000 Uani C7 1.00279(15) 0.46252(19) 0.60679(13) 0.0362 1.0000 Uani C8 0.94572(15) 0.50332(19) 0.57348(13) 0.0354 1.0000 Uani C9 0.91203(13) 0.44470(18) 0.52490(12) 0.0288 1.0000 Uani C10 0.78919(13) -0.02612(19) 0.55775(14) 0.0353 1.0000 Uani C11 0.79322(15) 0.1731(2) 0.63435(13) 0.0451 1.0000 Uani C12 0.72248(12) 0.16301(18) 0.49537(13) 0.0305 1.0000 Uani C13 1.09596(14) 0.2854(2) 0.30033(14) 0.0425 1.0000 Uani C14 0.94739(13) 0.2599(2) 0.25219(12) 0.0342 1.0000 Uani C15 1.03674(15) 0.07464(19) 0.29162(13) 0.0357 1.0000 Uani C16 0.83567(12) 0.05079(18) 0.34386(13) 0.0291 1.0000 Uani C17 0.80881(15) 0.0258(2) 0.27296(13) 0.0411 1.0000 Uani C18 0.74377(16) 0.0928(2) 0.26796(14) 0.0446 1.0000 Uani C19 0.76335(12) 0.18881(19) 0.30648(12) 0.0318 1.0000 Uani H11 0.9303 0.12963 0.59069 0.0261 1.0000 Uiso H12 0.9534 0.05551 0.52747 0.0261 1.0000 Uiso H31 1.07206 0.23284 0.44559 0.0275 1.0000 Uiso H32 1.04224 0.11651 0.44141 0.0275 1.0000 Uiso H41 1.10649 0.19726 0.56192 0.0296 1.0000 Uiso H42 1.05006 0.15740 0.61872 0.0296 1.0000 Uiso H43 1.07334 0.08306 0.55566 0.0296 1.0000 Uiso H61 1.06375 0.33245 0.61608 0.0354 1.0000 Uiso H71 1.02958 0.50409 0.64076 0.0444 1.0000 Uiso H81 0.92855 0.57327 0.58468 0.0426 1.0000 Uiso H91 0.87156 0.47467 0.49945 0.0352 1.0000 Uiso H101 0.74447 -0.04148 0.58226 0.0465 1.0000 Uiso H102 0.82950 -0.05299 0.58495 0.0465 1.0000 Uiso H103 0.78860 -0.05921 0.51162 0.0465 1.0000 Uiso H111 0.74875 0.1517 0.65719 0.0562 1.0000 Uiso H112 0.83403 0.1496 0.66225 0.0562 1.0000 Uiso H113 0.79434 0.2489 0.63031 0.0562 1.0000 Uiso H121 0.67773 0.14398 0.51862 0.0383 1.0000 Uiso H122 0.72538 0.23876 0.49116 0.0383 1.0000 Uiso H123 0.72389 0.13166 0.44871 0.0383 1.0000 Uiso H131 1.11242 0.2767 0.25206 0.0531 1.0000 Uiso H132 1.13288 0.2606 0.33255 0.0531 1.0000 Uiso H133 1.08644 0.3591 0.30932 0.0531 1.0000 Uiso H141 0.96595 0.2548 0.20442 0.0415 1.0000 Uiso H142 0.93683 0.3328 0.26302 0.0415 1.0000 Uiso H143 0.90363 0.2186 0.25622 0.0415 1.0000 Uiso H151 1.05571 0.07180 0.24392 0.0459 1.0000 Uiso H152 1.07299 0.04951 0.32446 0.0459 1.0000 Uiso H153 0.99411 0.03076 0.29489 0.0459 1.0000 Uiso H161 0.88714 0.03774 0.34673 0.0370 1.0000 Uiso H162 0.81095 0.00969 0.37955 0.0370 1.0000 Uiso H171 0.84365 0.0442 0.23680 0.0501 1.0000 Uiso H172 0.79675 -0.0481 0.26902 0.0501 1.0000 Uiso H181 0.73217 0.1080 0.21907 0.0525 1.0000 Uiso H182 0.70286 0.0590 0.29038 0.0525 1.0000 Uiso H191 0.77945 0.24218 0.27353 0.0412 1.0000 Uiso H192 0.72280 0.21534 0.33349 0.0412 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 0.01757(17) 0.01917(18) 0.02014(18) 0.00064(18) -0.00093(16) 0.00252(18) Cl1 0.0451(4) 0.0295(3) 0.0430(4) -0.0013(3) -0.0147(3) 0.0159(3) N1 0.0194(9) 0.0216(9) 0.0229(9) 0.0015(8) -0.0023(7) -0.0015(8) N2 0.0184(9) 0.024(1) 0.0185(9) 0.0003(7) -0.0008(7) 0.0016(7) N3 0.026(1) 0.0176(9) 0.023(1) 0.0001(8) 0.0013(8) 0.0008(8) O1 0.0246(8) 0.0255(8) 0.0250(8) 0.0010(7) -0.0065(7) 0.0007(7) Si1 0.0187(3) 0.0253(3) 0.0219(3) -0.0006(3) 0.0015(2) -0.0010(3) Si2 0.0219(3) 0.0262(3) 0.0198(3) 0.0002(3) 0.0022(3) 0.0002(3) C1 0.019(1) 0.0196(11) 0.0253(11) 0.0028(9) -0.0008(9) -0.0005(9) C2 0.020(1) 0.0184(11) 0.020(1) 0.0003(9) -0.0033(9) 0.0010(9) C3 0.019(1) 0.0231(11) 0.022(1) -0.0015(9) 0.0011(9) 0.0021(9) C4 0.0242(11) 0.0248(12) 0.0237(11) 0.002(1) -0.0032(9) 0.0011(9) C5 0.0251(11) 0.0187(11) 0.019(1) 0.0036(9) 0.0015(9) -0.0027(9) C6 0.0374(14) 0.0230(12) 0.0236(11) 0.0019(9) -0.005(1) -0.005(1) C7 0.0546(17) 0.0262(13) 0.0278(13) -0.0035(11) -0.0038(12) -0.0089(12) C8 0.0576(17) 0.0210(12) 0.0275(12) -0.0039(11) 0.0022(13) 0.0035(11) C9 0.0359(13) 0.0219(12) 0.0286(12) -0.000(1) 0.0030(11) 0.004(1) C10 0.0260(12) 0.0342(14) 0.0459(16) 0.0122(12) -0.0011(11) -0.0031(11) C11 0.0353(15) 0.068(2) 0.0321(15) -0.0147(14) 0.0062(12) -0.0001(14) C12 0.0203(11) 0.0315(13) 0.0398(14) 0.0047(11) 0.001(1) -0.000(1) C13 0.0350(14) 0.0556(18) 0.0370(15) -0.0054(13) 0.0124(12) -0.0109(13) C14 0.0304(12) 0.0476(15) 0.0245(12) 0.0086(12) 0.001(1) 0.0040(12) C15 0.0459(15) 0.0334(14) 0.0278(13) -0.0075(11) 0.0024(12) 0.0053(12) C16 0.0255(12) 0.0230(12) 0.0387(14) 0.000(1) -0.004(1) -0.000(1) C17 0.0524(17) 0.0358(15) 0.0351(15) -0.0077(12) -0.0001(13) -0.0089(14) C18 0.0523(17) 0.0433(16) 0.0383(15) 0.0092(13) -0.0216(14) -0.0139(14) C19 0.0270(12) 0.0421(15) 0.0262(12) 0.0028(11) -0.011(1) 0.0029(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 . Cl1 . 2.4426(7) yes Sc1 . N1 . 2.0252(18) yes Sc1 . N2 . 2.0239(18) yes Sc1 . N3 . 2.2881(19) yes Sc1 . O1 . 2.2051(16) yes N1 . Si1 . 1.7161(19) yes N1 . C1 . 1.468(3) yes N2 . Si2 . 1.7153(19) yes N2 . C3 . 1.467(3) yes N3 . C5 . 1.356(3) yes N3 . C9 . 1.344(3) yes O1 . C16 . 1.466(3) yes O1 . C19 . 1.469(3) yes Si1 . C10 . 1.875(3) yes Si1 . C11 . 1.872(3) yes Si1 . C12 . 1.871(2) yes Si2 . C13 . 1.871(3) yes Si2 . C14 . 1.864(2) yes Si2 . C15 . 1.882(2) yes C1 . C2 . 1.566(3) yes C2 . C3 . 1.554(3) yes C2 . C4 . 1.536(3) yes C2 . C5 . 1.520(3) yes C5 . C6 . 1.394(3) yes C6 . C7 . 1.386(3) yes C7 . C8 . 1.378(4) yes C8 . C9 . 1.381(3) yes C16 . C17 . 1.512(3) yes C17 . C18 . 1.526(4) yes C18 . C19 . 1.515(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 Cl1 . Sc1 . N1 . 135.79(6) yes Cl1 . Sc1 . N2 . 122.35(6) yes N1 . Sc1 . N2 . 100.57(7) yes Cl1 . Sc1 . N3 . 89.45(5) yes N1 . Sc1 . N3 . 82.53(7) yes N2 . Sc1 . N3 . 86.54(7) yes Cl1 . Sc1 . O1 . 86.09(4) yes N1 . Sc1 . O1 . 96.25(7) yes N2 . Sc1 . O1 . 101.22(7) yes N3 . Sc1 . O1 . 172.22(6) yes Sc1 . N1 . Si1 . 126.8(1) yes Sc1 . N1 . C1 . 114.67(13) yes Si1 . N1 . C1 . 116.43(14) yes Sc1 . N2 . Si2 . 129.6(1) yes Sc1 . N2 . C3 . 114.62(13) yes Si2 . N2 . C3 . 115.30(13) yes Sc1 . N3 . C5 . 115.28(14) yes Sc1 . N3 . C9 . 125.44(16) yes C5 . N3 . C9 . 119.3(2) yes Sc1 . O1 . C16 . 119.45(13) yes Sc1 . O1 . C19 . 131.24(14) yes C16 . O1 . C19 . 109.30(17) yes N1 . Si1 . C10 . 113.0(1) yes N1 . Si1 . C11 . 111.67(11) yes C10 . Si1 . C11 . 107.11(14) yes N1 . Si1 . C12 . 107.8(1) yes C10 . Si1 . C12 . 108.81(11) yes C11 . Si1 . C12 . 108.31(13) yes N2 . Si2 . C13 . 113.23(11) yes N2 . Si2 . C14 . 108.7(1) yes C13 . Si2 . C14 . 107.39(13) yes N2 . Si2 . C15 . 111.3(1) yes C13 . Si2 . C15 . 105.96(13) yes C14 . Si2 . C15 . 110.17(12) yes N1 . C1 . C2 . 117.43(17) yes C1 . C2 . C3 . 112.75(17) yes C1 . C2 . C4 . 105.19(17) yes C3 . C2 . C4 . 105.78(17) yes C1 . C2 . C5 . 110.31(17) yes C3 . C2 . C5 . 110.75(17) yes C4 . C2 . C5 . 111.88(18) yes N2 . C3 . C2 . 118.26(17) yes N3 . C5 . C2 . 116.30(19) yes N3 . C5 . C6 . 119.9(2) yes C2 . C5 . C6 . 123.8(2) yes C5 . C6 . C7 . 120.4(2) yes C6 . C7 . C8 . 119.0(2) yes C7 . C8 . C9 . 118.4(2) yes N3 . C9 . C8 . 123.0(2) yes O1 . C16 . C17 . 104.41(19) yes C16 . C17 . C18 . 102.1(2) yes C17 . C18 . C19 . 104.3(2) yes O1 . C19 . C18 . 105.64(19) yes #===end data_COMPOUND_2 _database_code_CSD 194288 # Local code BDW4 _chemical_name_systematic ; [Sc(N2N_C2,TMS)Cl(THF)] ; _publ_section_exptl_refinement ; No special details ; _cell_length_a 10.5815(2) _cell_length_b 21.2366(4) _cell_length_c 12.6644(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.642(1) _cell_angle_gamma 90.00 _cell_volume 2663.2(1) _diffrn_reflns_number 9233 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-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' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 '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' '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' _chemical_formula_sum ' C17 H43 Cl1 N3 O1 Sc1 Si3 ' _chemical_formula_moiety ' C17 H43 Cl1 N3 O1 Sc1 Si3 ' _chemical_formula_weight 470.22 _cell_measurement_reflns_used 4002 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description 'block ' _exptl_crystal_colour 'white ' _exptl_crystal_size_min 0.70 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_max 0.75 _exptl_crystal_density_diffrn 1.17 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1018.35 _exptl_absorpt_coefficient_mu 0.52 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_T_max 0.695 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_ambient_temperature 150 _diffrn_reflns_number 9233 _reflns_number_total 5571 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_gt 4148 _diffrn_reflns_theta_min 0.998 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -13 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_diff_density_min -0.67 _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_diff_density_max 0.78 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4148 _refine_ls_number_parameters 236 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0312 _refine_ls_goodness_of_fit_ref 1.0493 _refine_ls_shift/su_max 0.0015 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'Chebychev polynomial ' _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 0.589 -.818 0.145 -.415 ; _refine_ls_extinction_coef 213(17) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD 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 'CAMERON (Watkin, Prout and Pearce, 1996)' _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 Sc1 0.64849(4) 0.147448(17) 0.23467(3) 0.0170 1.0000 Uani Cl1 0.60538(6) 0.14057(3) 0.03599(4) 0.0281 1.0000 Uani O1 0.50874(15) 0.22718(7) 0.20525(12) 0.0252 1.0000 Uani N1 0.54700(17) 0.09437(8) 0.31357(14) 0.0222 1.0000 Uani N2 0.81874(17) 0.19346(8) 0.33367(14) 0.0215 1.0000 Uani N3 0.80532(16) 0.05961(8) 0.31036(14) 0.0196 1.0000 Uani Si1 0.38290(6) 0.06978(3) 0.27738(5) 0.0247 1.0000 Uani Si2 0.88936(6) 0.26273(3) 0.31119(5) 0.0243 1.0000 Uani Si3 0.82843(6) 0.00539(3) 0.21029(5) 0.0246 1.0000 Uani C1 0.6441(2) 0.06631(11) 0.41627(17) 0.0249 1.0000 Uani C2 0.7456(2) 0.0261(1) 0.38577(18) 0.0243 1.0000 Uani C3 0.9340(2) 0.0918(1) 0.37711(19) 0.0263 1.0000 Uani C4 0.9104(2) 0.15444(11) 0.42535(18) 0.0286 1.0000 Uani C5 0.2781(2) 0.10918(13) 0.1420(2) 0.0355 1.0000 Uani C6 0.3126(3) 0.09074(13) 0.3901(2) 0.0380 1.0000 Uani C7 0.3647(3) -0.01768(12) 0.2583(3) 0.0436 1.0000 Uani C8 0.9292(3) 0.31675(13) 0.4354(2) 0.0448 1.0000 Uani C9 0.7721(3) 0.30427(12) 0.1846(2) 0.0419 1.0000 Uani C10 1.0515(3) 0.24764(14) 0.2860(3) 0.0461 1.0000 Uani C11 0.9148(3) 0.04494(15) 0.1240(2) 0.0425 1.0000 Uani C12 0.6600(3) -0.02439(12) 0.1202(2) 0.0376 1.0000 Uani C13 0.9370(3) -0.06146(13) 0.2880(2) 0.0439 1.0000 Uani C14 0.4913(3) 0.25660(12) 0.3036(2) 0.0376 1.0000 Uani C15 0.4033(3) 0.31337(15) 0.2574(2) 0.0505 1.0000 Uani C16 0.3228(3) 0.29690(14) 0.1384(2) 0.0450 1.0000 Uani C17 0.4198(2) 0.25710(11) 0.10231(19) 0.0302 1.0000 Uani H11 0.6935 0.10063 0.46866 0.0295 1.0000 Uiso H12 0.5949 0.03963 0.45419 0.0295 1.0000 Uiso H21 0.8203 0.0137 0.45659 0.0295 1.0000 Uiso H22 0.6980 -0.0125 0.34603 0.0295 1.0000 Uiso H31 0.9871 0.0636 0.44046 0.0278 1.0000 Uiso H32 0.9867 0.0999 0.32669 0.0278 1.0000 Uiso H41 0.9981 0.17703 0.46093 0.0290 1.0000 Uiso H42 0.8683 0.14651 0.48345 0.0290 1.0000 Uiso H51 0.1820 0.09513 0.1199 0.0384 1.0000 Uiso H52 0.2830 0.15589 0.1526 0.0384 1.0000 Uiso H53 0.3139 0.09749 0.0814 0.0384 1.0000 Uiso H61 0.2170 0.07599 0.3673 0.0502 1.0000 Uiso H62 0.3679 0.07021 0.4628 0.0502 1.0000 Uiso H63 0.3158 0.13749 0.4001 0.0502 1.0000 Uiso H71 0.2675 -0.02965 0.2372 0.0517 1.0000 Uiso H72 0.4189 -0.03907 0.3304 0.0517 1.0000 Uiso H73 0.3983 -0.03098 0.1971 0.0517 1.0000 Uiso H81 0.9701 0.35635 0.4191 0.0533 1.0000 Uiso H82 0.9947 0.29580 0.5035 0.0533 1.0000 Uiso H83 0.8445 0.32711 0.4498 0.0533 1.0000 Uiso H91 0.8151 0.34433 0.1728 0.0455 1.0000 Uiso H92 0.7529 0.27679 0.1166 0.0455 1.0000 Uiso H93 0.6858 0.31407 0.1966 0.0455 1.0000 Uiso H101 1.0898 0.28876 0.2732 0.0587 1.0000 Uiso H102 1.1176 0.22625 0.3533 0.0587 1.0000 Uiso H103 1.0334 0.22026 0.2180 0.0587 1.0000 Uiso H111 0.9270 0.01436 0.0683 0.0533 1.0000 Uiso H112 1.0051 0.06043 0.1745 0.0533 1.0000 Uiso H113 0.8592 0.08136 0.0828 0.0533 1.0000 Uiso H121 0.6711 -0.05467 0.0637 0.0393 1.0000 Uiso H122 0.6165 -0.04633 0.1685 0.0393 1.0000 Uiso H123 0.6019 0.01158 0.0801 0.0393 1.0000 Uiso H131 0.9504 -0.09191 0.2327 0.0508 1.0000 Uiso H132 1.0266 -0.04478 0.3378 0.0508 1.0000 Uiso H133 0.8920 -0.08333 0.3352 0.0508 1.0000 Uiso H141 0.5803 0.26951 0.3603 0.0447 1.0000 Uiso H142 0.4454 0.22668 0.3394 0.0447 1.0000 Uiso H151 0.4600 0.35153 0.2609 0.0571 1.0000 Uiso H152 0.3421 0.32130 0.3008 0.0571 1.0000 Uiso H161 0.2948 0.33565 0.0910 0.0536 1.0000 Uiso H162 0.2409 0.27191 0.1336 0.0536 1.0000 Uiso H171 0.4730 0.28447 0.06898 0.0342 1.0000 Uiso H172 0.3698 0.22465 0.04582 0.0342 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 0.01638(18) 0.01668(18) 0.01689(18) 0.00173(14) 0.00454(14) -0.00042(14) Cl1 0.0346(3) 0.0301(3) 0.0187(2) 0.0012(2) 0.0083(2) 0.0018(2) O1 0.0306(8) 0.0240(7) 0.0200(7) 0.0014(6) 0.0077(6) 0.0082(6) N1 0.0190(8) 0.0238(9) 0.0235(9) 0.0044(7) 0.0072(7) 0.0019(7) N2 0.0218(8) 0.0175(8) 0.0221(8) 0.0004(7) 0.0039(7) -0.0036(7) N3 0.0170(8) 0.0207(8) 0.0206(8) 0.0022(7) 0.0061(7) -0.0002(7) Si1 0.0202(3) 0.0249(3) 0.0318(3) 0.0024(2) 0.0129(2) -0.0008(2) Si2 0.0243(3) 0.0202(3) 0.0292(3) -0.0031(2) 0.0105(2) -0.0057(2) Si3 0.0250(3) 0.0234(3) 0.0262(3) 0.0005(2) 0.0103(2) 0.0058(2) C1 0.024(1) 0.0295(11) 0.022(1) 0.0064(8) 0.0090(9) 0.0052(9) C2 0.025(1) 0.024(1) 0.0249(11) 0.0073(8) 0.0104(9) 0.0047(9) C3 0.016(1) 0.0279(11) 0.0286(11) 0.0016(9) 0.0001(8) 0.0015(8) C4 0.0257(11) 0.0289(11) 0.0235(11) 0.0003(9) -0.0009(9) -0.0037(9) C5 0.0218(11) 0.0454(14) 0.0348(13) 0.0033(11) 0.004(1) -0.005(1) C6 0.0307(12) 0.0481(15) 0.0423(14) 0.0090(12) 0.0217(11) 0.0081(11) C7 0.0387(14) 0.0302(13) 0.0666(19) -0.0022(13) 0.0244(14) -0.0085(11) C8 0.0545(17) 0.0338(14) 0.0469(15) -0.0176(12) 0.0190(13) -0.0162(13) C9 0.0412(14) 0.0321(13) 0.0463(15) 0.0120(11) 0.0080(12) -0.0095(11) C10 0.0400(14) 0.0425(16) 0.0672(19) 0.0018(14) 0.0331(14) -0.0035(12) C11 0.0374(14) 0.0574(18) 0.0420(14) 0.0026(13) 0.0257(12) 0.0057(13) C12 0.0420(14) 0.0284(12) 0.0363(13) -0.007(1) 0.0061(11) -0.0062(11) C13 0.0517(16) 0.0372(14) 0.0408(14) 0.0008(11) 0.0139(13) 0.0213(13) C14 0.0532(16) 0.0339(13) 0.0274(12) -0.003(1) 0.0163(11) 0.0121(12) C15 0.0440(16) 0.0527(17) 0.0495(17) -0.0113(14) 0.0101(13) 0.0201(14) C16 0.0463(15) 0.0463(16) 0.0448(15) 0.0130(12) 0.0188(13) 0.0227(13) C17 0.0324(12) 0.0308(12) 0.0265(11) 0.0093(9) 0.0090(9) 0.011(1) 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 . Cl1 . 2.3982(6) yes Sc1 . O1 . 2.1919(15) yes Sc1 . N1 . 2.0442(18) yes Sc1 . N2 . 2.0444(17) yes Sc1 . N3 . 2.4558(17) yes O1 . C14 . 1.462(3) yes O1 . C17 . 1.457(2) yes N1 . Si1 . 1.7138(18) yes N1 . C1 . 1.470(2) yes N2 . Si2 . 1.7186(18) yes N2 . C4 . 1.477(3) yes N3 . Si3 . 1.7917(18) yes N3 . C2 . 1.498(3) yes N3 . C3 . 1.491(3) yes Si1 . C5 . 1.878(2) yes Si1 . C6 . 1.881(3) yes Si1 . C7 . 1.874(3) yes Si2 . C8 . 1.871(3) yes Si2 . C9 . 1.867(3) yes Si2 . C10 . 1.880(3) yes Si3 . C11 . 1.855(3) yes Si3 . C12 . 1.856(2) yes Si3 . C13 . 1.873(3) yes C1 . C2 . 1.524(3) yes C3 . C4 . 1.521(3) yes C14 . C15 . 1.510(4) yes C15 . C16 . 1.487(4) yes C16 . C17 . 1.519(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 Cl1 . Sc1 . O1 . 90.07(4) yes Cl1 . Sc1 . N1 . 122.74(5) yes O1 . Sc1 . N1 . 94.00(6) yes Cl1 . Sc1 . N2 . 118.24(5) yes O1 . Sc1 . N2 . 97.52(7) yes N1 . Sc1 . N2 . 117.71(7) yes Cl1 . Sc1 . N3 . 102.45(4) yes O1 . Sc1 . N3 . 167.35(6) yes N1 . Sc1 . N3 . 77.85(6) yes N2 . Sc1 . N3 . 78.20(6) yes Sc1 . O1 . C14 . 117.75(12) yes Sc1 . O1 . C17 . 132.30(13) yes C14 . O1 . C17 . 109.89(17) yes Sc1 . N1 . Si1 . 134.0(1) yes Sc1 . N1 . C1 . 109.40(13) yes Si1 . N1 . C1 . 116.07(14) yes Sc1 . N2 . Si2 . 130.4(1) yes Sc1 . N2 . C4 . 113.98(13) yes Si2 . N2 . C4 . 114.02(14) yes Sc1 . N3 . Si3 . 117.00(8) yes Sc1 . N3 . C2 . 103.31(12) yes Si3 . N3 . C2 . 109.86(13) yes Sc1 . N3 . C3 . 103.25(12) yes Si3 . N3 . C3 . 111.76(14) yes C2 . N3 . C3 . 111.24(16) yes N1 . Si1 . C5 . 109.0(1) yes N1 . Si1 . C6 . 111.06(11) yes C5 . Si1 . C6 . 108.84(12) yes N1 . Si1 . C7 . 112.62(11) yes C5 . Si1 . C7 . 108.85(13) yes C6 . Si1 . C7 . 106.41(13) yes N2 . Si2 . C8 . 111.58(11) yes N2 . Si2 . C9 . 110.5(1) yes C8 . Si2 . C9 . 108.48(14) yes N2 . Si2 . C10 . 110.99(11) yes C8 . Si2 . C10 . 107.37(14) yes C9 . Si2 . C10 . 107.75(14) yes N3 . Si3 . C11 . 110.14(11) yes N3 . Si3 . C12 . 108.2(1) yes C11 . Si3 . C12 . 110.99(13) yes N3 . Si3 . C13 . 109.1(1) yes C11 . Si3 . C13 . 108.35(13) yes C12 . Si3 . C13 . 110.06(13) yes N1 . C1 . C2 . 109.75(17) yes N3 . C2 . C1 . 112.93(17) yes N3 . C3 . C4 . 112.49(17) yes N2 . C4 . C3 . 109.28(17) yes O1 . C14 . C15 . 104.9(2) yes C14 . C15 . C16 . 105.0(2) yes C15 . C16 . C17 . 103.3(2) yes O1 . C17 . C16 . 105.37(19) yes #===end data_COMPOUND_3 _database_code_CSD 194289 # Local code BDW7 _chemical_name_systematic ; [Sc2(N2N_C3,Me)2(mu-Cl)2] ; _publ_section_exptl_refinement ; The asymmetric unit contains two crystallographically independent halfs of the title compound, each related to their counterpart by a crystallographic inversion centre ; _cell_length_a 10.6049(2) _cell_length_b 12.1528(2) _cell_length_c 16.7295(4) _cell_angle_alpha 79.9117(8) _cell_angle_beta 77.1004(9) _cell_angle_gamma 77.102(1) _cell_volume 2030.75(7) _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 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' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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 ' C26 H66 Cl2 N6 Sc2 Si4 ' _chemical_formula_moiety ' C26 H66 Cl2 N6 Sc2 Si4 ' _chemical_compound_source ; ? ; _chemical_formula_weight 736.02 _cell_measurement_reflns_used 8719 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.20 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 794.03 _exptl_absorpt_coefficient_mu 0.61 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.885 _exptl_absorpt_correction_T_max 0.885 _diffrn_ambient_temperature 150 _diffrn_reflns_number 17186 _reflns_number_total 9128 _diffrn_reflns_av_R_equivalents 0.02 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method CCD _reflns_number_gt 6361 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_reflns_theta_min 2.910 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -0.30 _refine_diff_density_max 0.40 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 6361 _refine_ls_number_parameters 361 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0231 _refine_ls_goodness_of_fit_ref 1.0733 _refine_ls_shift/su_max 0.00074 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 0.182 -.530 -.137 -.221 ; _refine_ls_extinction_method None _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD 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 'CAMERON (Watkin, Prout and Pearce, 1996)' _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 Sc1 0.42984(3) -0.36507(3) 0.05692(2) 0.0165 1.0000 Uani Cl1 0.41327(5) -0.57231(4) 0.07864(3) 0.0234 1.0000 Uani N1 0.56068(16) -0.33514(14) 0.1178(1) 0.0214 1.0000 Uani N2 0.27539(16) -0.34238(14) 0.1779(1) 0.0218 1.0000 Uani N3 0.31309(16) -0.23139(13) 0.0016(1) 0.0213 1.0000 Uani Si1 0.66100(6) -0.23630(5) 0.08801(4) 0.0265 1.0000 Uani Si2 0.24049(5) -0.22932(5) -0.08124(3) 0.0216 1.0000 Uani C1 0.5701(2) -0.41069(18) 0.19679(13) 0.0278 1.0000 Uani C2 0.4519(2) -0.38633(19) 0.26667(12) 0.0289 1.0000 Uani C3 0.3254(2) -0.41111(18) 0.25177(12) 0.0263 1.0000 Uani C4 0.2411(2) -0.21967(17) 0.19199(12) 0.0266 1.0000 Uani C5 0.1862(2) -0.13549(18) 0.12361(13) 0.0290 1.0000 Uani C6 0.2843(2) -0.12753(17) 0.04214(13) 0.0268 1.0000 Uani C7 0.8339(2) -0.2998(3) 0.10150(19) 0.0538 1.0000 Uani C8 0.6033(3) -0.1130(2) 0.14900(15) 0.0434 1.0000 Uani C9 0.6636(3) -0.1808(2) -0.02395(14) 0.0365 1.0000 Uani C10 0.1542(2) -0.3805(2) 0.17305(14) 0.0309 1.0000 Uani C11 0.0894(2) -0.11385(19) -0.08229(15) 0.0356 1.0000 Uani C12 0.3530(2) -0.2029(2) -0.18301(13) 0.0348 1.0000 Uani C13 0.1914(2) -0.36962(18) -0.07530(14) 0.0304 1.0000 Uani Sc101 0.07324(4) 0.13540(3) 0.44839(2) 0.0188 1.0000 Uani Cl101 0.09303(5) -0.06626(4) 0.42178(3) 0.0259 1.0000 Uani N101 0.17903(17) 0.19595(14) 0.5119(1) 0.0233 1.0000 Uani N102 0.23898(16) 0.15849(15) 0.3331(1) 0.0245 1.0000 Uani N103 -0.05166(17) 0.24542(14) 0.3829(1) 0.0242 1.0000 Uani Si101 0.24684(6) 0.12661(5) 0.59599(3) 0.0231 1.0000 Uani Si102 -0.16325(6) 0.36432(5) 0.41169(4) 0.0274 1.0000 Uani C101 0.2130(2) 0.30777(18) 0.47409(14) 0.0301 1.0000 Uani C102 0.3205(2) 0.29972(19) 0.39736(14) 0.0320 1.0000 Uani C103 0.2756(2) 0.27308(18) 0.32388(13) 0.0289 1.0000 Uani C104 0.1988(2) 0.14861(19) 0.25511(13) 0.0301 1.0000 Uani C105 0.0749(2) 0.2318(2) 0.23651(13) 0.0322 1.0000 Uani C106 -0.0503(2) 0.2157(2) 0.30064(13) 0.0291 1.0000 Uani C107 0.2966(2) -0.02902(18) 0.58642(14) 0.0318 1.0000 Uani C108 0.3972(2) 0.1803(2) 0.60137(14) 0.0338 1.0000 Uani C109 0.1308(2) 0.1429(2) 0.69684(14) 0.0372 1.0000 Uani C110 0.3572(2) 0.06854(19) 0.34163(14) 0.0320 1.0000 Uani C111 -0.1209(3) 0.4960(2) 0.34409(16) 0.0462 1.0000 Uani C112 -0.1648(3) 0.3756(2) 0.52202(15) 0.0410 1.0000 Uani C113 -0.3354(2) 0.3582(2) 0.4041(2) 0.0516 1.0000 Uani H11 0.6508 -0.40280 0.21515 0.0336 1.0000 Uiso H12 0.5789 -0.49086 0.18637 0.0336 1.0000 Uiso H21 0.4732 -0.43337 0.31901 0.0356 1.0000 Uiso H22 0.4364 -0.30373 0.27277 0.0356 1.0000 Uiso H31 0.3423 -0.49322 0.24399 0.0317 1.0000 Uiso H32 0.2552 -0.39723 0.30187 0.0317 1.0000 Uiso H41 0.3230 -0.19745 0.19878 0.0315 1.0000 Uiso H42 0.1738 -0.21335 0.24426 0.0315 1.0000 Uiso H51 0.1583 -0.05843 0.14230 0.0352 1.0000 Uiso H52 0.1078 -0.16031 0.11371 0.0352 1.0000 Uiso H61 0.3683 -0.11478 0.05339 0.0335 1.0000 Uiso H62 0.2474 -0.06148 0.00378 0.0335 1.0000 Uiso H71 0.8895 -0.2402 0.08363 0.0675 1.0000 Uiso H72 0.8342 -0.3301 0.16106 0.0675 1.0000 Uiso H73 0.8703 -0.3634 0.06709 0.0675 1.0000 Uiso H81 0.6646 -0.0579 0.12953 0.0568 1.0000 Uiso H82 0.6018 -0.1410 0.20902 0.0568 1.0000 Uiso H83 0.5126 -0.0742 0.14093 0.0568 1.0000 Uiso H91 0.7218 -0.1231 -0.04193 0.0466 1.0000 Uiso H92 0.6983 -0.2453 -0.05761 0.0466 1.0000 Uiso H93 0.5721 -0.1446 -0.03213 0.0466 1.0000 Uiso H101 0.1178 -0.3358 0.12434 0.0387 1.0000 Uiso H102 0.1760 -0.4633 0.16664 0.0387 1.0000 Uiso H103 0.0872 -0.3683 0.22479 0.0387 1.0000 Uiso H111 0.0498 -0.11524 -0.13094 0.0438 1.0000 Uiso H112 0.1144 -0.03817 -0.08623 0.0438 1.0000 Uiso H113 0.0238 -0.12669 -0.03013 0.0438 1.0000 Uiso H121 0.3069 -0.2025 -0.22908 0.0421 1.0000 Uiso H122 0.4335 -0.2645 -0.18647 0.0421 1.0000 Uiso H123 0.3792 -0.1275 -0.18773 0.0421 1.0000 Uiso H131 0.1491 -0.36878 -0.12323 0.0396 1.0000 Uiso H132 0.2713 -0.43165 -0.07684 0.0396 1.0000 Uiso H133 0.1275 -0.38343 -0.02246 0.0396 1.0000 Uiso H1011 0.2432 0.34017 0.51592 0.0387 1.0000 Uiso H1012 0.1324 0.35966 0.45832 0.0387 1.0000 Uiso H1021 0.3515 0.37386 0.38186 0.0410 1.0000 Uiso H1022 0.3952 0.23762 0.41071 0.0410 1.0000 Uiso H1031 0.3486 0.27801 0.27462 0.0371 1.0000 Uiso H1032 0.1966 0.33231 0.31378 0.0371 1.0000 Uiso H1041 0.2732 0.16072 0.20801 0.0370 1.0000 Uiso H1042 0.1820 0.06982 0.25928 0.0370 1.0000 Uiso H1051 0.0893 0.3107 0.23539 0.0401 1.0000 Uiso H1052 0.0610 0.2226 0.18104 0.0401 1.0000 Uiso H1061 -0.1283 0.2646 0.27949 0.0378 1.0000 Uiso H1062 -0.0577 0.1339 0.30731 0.0378 1.0000 Uiso H1071 0.3362 -0.07009 0.63489 0.0384 1.0000 Uiso H1072 0.2172 -0.05967 0.58503 0.0384 1.0000 Uiso H1073 0.3628 -0.04043 0.53421 0.0384 1.0000 Uiso H1081 0.4340 0.1384 0.65065 0.0439 1.0000 Uiso H1082 0.3726 0.2636 0.60637 0.0439 1.0000 Uiso H1083 0.4650 0.1678 0.54997 0.0439 1.0000 Uiso H1091 0.1754 0.1011 0.74313 0.0457 1.0000 Uiso H1092 0.1034 0.2255 0.70363 0.0457 1.0000 Uiso H1093 0.0513 0.1110 0.69772 0.0457 1.0000 Uiso H1101 0.3329 -0.00792 0.34832 0.0374 1.0000 Uiso H1102 0.3910 0.07581 0.39132 0.0374 1.0000 Uiso H1103 0.4273 0.07688 0.29108 0.0374 1.0000 Uiso H1111 -0.1873 0.5639 0.36213 0.0539 1.0000 Uiso H1112 -0.0313 0.5045 0.34872 0.0539 1.0000 Uiso H1113 -0.1216 0.4900 0.28533 0.0539 1.0000 Uiso H1121 -0.2298 0.4447 0.53910 0.0480 1.0000 Uiso H1122 -0.0749 0.3821 0.52758 0.0480 1.0000 Uiso H1123 -0.1903 0.3063 0.55826 0.0480 1.0000 Uiso H1131 -0.3971 0.4288 0.4215 0.0628 1.0000 Uiso H1132 -0.3627 0.2902 0.4412 0.0628 1.0000 Uiso H1133 -0.3380 0.3521 0.3457 0.0628 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 0.01702(17) 0.01543(17) 0.01642(17) -0.00199(13) -0.00428(13) -0.00114(13) Cl1 0.0280(3) 0.0180(2) 0.0216(2) -0.00300(18) 0.00116(19) -0.00448(18) N1 0.0216(8) 0.0260(9) 0.0174(8) -0.0006(7) -0.0073(7) -0.0045(7) N2 0.0204(8) 0.0221(8) 0.0210(8) -0.0020(7) -0.0028(7) -0.0018(7) N3 0.0248(9) 0.0173(8) 0.0210(8) -0.0018(6) -0.0076(7) 0.0005(6) Si1 0.0268(3) 0.0331(3) 0.0232(3) -0.0024(2) -0.0065(2) -0.0123(2) Si2 0.0211(3) 0.0220(3) 0.0213(3) -0.0015(2) -0.0076(2) -0.0006(2) C1 0.0244(11) 0.0313(11) 0.0246(11) 0.0035(9) -0.0087(8) -0.0010(9) C2 0.0333(12) 0.0334(12) 0.019(1) 0.0016(9) -0.0098(9) -0.0026(9) C3 0.0297(11) 0.0290(11) 0.0168(9) 0.0024(8) -0.0017(8) -0.0051(9) C4 0.0281(11) 0.0260(11) 0.023(1) -0.0092(8) -0.0023(8) 0.0036(8) C5 0.0306(12) 0.0238(11) 0.0308(12) -0.0091(9) -0.0093(9) 0.0063(9) C6 0.0341(12) 0.019(1) 0.0281(11) -0.0033(8) -0.0126(9) -0.0001(8) C7 0.0294(13) 0.0678(19) 0.068(2) 0.0033(15) -0.0130(13) -0.0216(13) C8 0.0624(17) 0.0449(15) 0.0325(13) -0.0089(11) -0.0098(12) -0.0266(13) C9 0.0504(15) 0.0363(13) 0.0265(12) -0.003(1) -0.002(1) -0.0221(11) C10 0.019(1) 0.0379(12) 0.0341(12) -0.006(1) 0.0008(9) -0.0060(9) C11 0.0331(13) 0.0333(12) 0.0424(14) -0.007(1) -0.0198(11) 0.004(1) C12 0.0383(13) 0.0430(14) 0.0226(11) -0.001(1) -0.0072(9) -0.007(1) C13 0.0320(12) 0.0293(11) 0.0322(12) -0.0064(9) -0.0101(9) -0.0046(9) Sc101 0.02045(18) 0.01883(18) 0.01737(18) -0.00032(14) -0.00466(14) -0.00473(14) Cl101 0.0299(3) 0.0219(2) 0.0243(2) -0.00420(19) 0.0015(2) -0.00749(19) N101 0.0281(9) 0.0216(9) 0.0218(9) -0.0004(7) -0.0087(7) -0.0064(7) N102 0.0221(9) 0.0293(9) 0.0216(9) -0.0002(7) -0.0045(7) -0.0057(7) N103 0.0254(9) 0.0263(9) 0.0207(8) -0.0006(7) -0.0076(7) -0.0035(7) Si101 0.0231(3) 0.0266(3) 0.0192(3) -0.0026(2) -0.0061(2) -0.0026(2) Si102 0.0281(3) 0.0233(3) 0.0276(3) 0.0010(2) -0.0062(2) -0.0011(2) C101 0.0394(13) 0.0238(11) 0.0320(12) -0.0005(9) -0.016(1) -0.0097(9) C102 0.0325(12) 0.0298(12) 0.0378(13) 0.005(1) -0.012(1) -0.0164(9) C103 0.0288(11) 0.0309(12) 0.0273(11) 0.0048(9) -0.0059(9) -0.0123(9) C104 0.0327(12) 0.0375(12) 0.018(1) -0.0047(9) -0.0004(9) -0.007(1) C105 0.0377(13) 0.0422(13) 0.018(1) -0.0020(9) -0.0081(9) -0.009(1) C106 0.0287(11) 0.0357(12) 0.0256(11) -0.0040(9) -0.0102(9) -0.0067(9) C107 0.0369(13) 0.0276(11) 0.0281(11) 0.0024(9) -0.0086(9) -0.0028(9) C108 0.0287(12) 0.0426(14) 0.0316(12) -0.004(1) -0.0123(9) -0.004(1) C109 0.0329(13) 0.0534(15) 0.0250(12) -0.007(1) -0.007(1) -0.0051(11) C110 0.0222(11) 0.0330(12) 0.0347(12) 0.002(1) -0.0006(9) -0.0019(9) C111 0.0655(18) 0.0302(13) 0.0365(14) 0.0031(11) -0.0050(13) -0.0064(12) C112 0.0500(16) 0.0334(13) 0.0328(13) -0.006(1) -0.0014(11) 0.0007(11) C113 0.0303(13) 0.0475(16) 0.073(2) -0.0093(14) -0.0141(13) 0.0062(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 . Cl1 . 2.5208(6) yes Sc1 . Cl1 2_645 2.6162(6) yes Sc1 . N1 . 2.0204(16) yes Sc1 . N2 . 2.3177(16) yes Sc1 . N3 . 2.0289(16) yes N1 . Si1 . 1.7168(17) yes N1 . C1 . 1.480(2) yes N2 . C3 . 1.496(2) yes N2 . C4 . 1.501(2) yes N2 . C10 . 1.483(3) yes N3 . Si2 . 1.7228(17) yes N3 . C6 . 1.477(2) yes Si1 . C7 . 1.871(3) yes Si1 . C8 . 1.873(2) yes Si1 . C9 . 1.873(2) yes Si2 . C11 . 1.881(2) yes Si2 . C12 . 1.870(2) yes Si2 . C13 . 1.872(2) yes C1 . C2 . 1.525(3) yes C2 . C3 . 1.520(3) yes C4 . C5 . 1.522(3) yes C5 . C6 . 1.521(3) yes Sc101 . Cl101 . 2.5217(6) yes Sc101 . Cl101 2_556 2.6162(6) yes Sc101 . N101 . 2.0262(17) yes Sc101 . N102 . 2.3246(17) yes Sc101 . N103 . 2.0213(17) yes N101 . Si101 . 1.7235(17) yes N101 . C101 . 1.481(3) yes N102 . C103 . 1.501(3) yes N102 . C104 . 1.492(3) yes N102 . C110 . 1.484(3) yes N103 . Si102 . 1.7163(18) yes N103 . C106 . 1.479(3) yes Si101 . C107 . 1.872(2) yes Si101 . C108 . 1.878(2) yes Si101 . C109 . 1.866(2) yes Si102 . C111 . 1.871(2) yes Si102 . C112 . 1.871(2) yes Si102 . C113 . 1.877(3) yes C101 . C102 . 1.516(3) yes C102 . C103 . 1.520(3) yes C104 . C105 . 1.524(3) yes C105 . C106 . 1.536(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 Cl1 . Sc1 . Cl1 2_645 80.657(19) yes Cl1 . Sc1 . N1 . 112.36(5) yes Cl1 2_645 Sc1 . N1 . 100.73(5) yes Cl1 . Sc1 . N2 . 88.52(4) yes Cl1 2_645 Sc1 . N2 . 168.61(4) yes N1 . Sc1 . N2 . 86.62(6) yes Cl1 . Sc1 . N3 . 127.74(5) yes Cl1 2_645 Sc1 . N3 . 96.73(5) yes N1 . Sc1 . N3 . 119.29(7) yes N2 . Sc1 . N3 . 87.06(6) yes Sc1 . Cl1 . Sc1 2_645 99.343(19) yes Sc1 . N1 . Si1 . 127.96(9) yes Sc1 . N1 . C1 . 114.23(13) yes Si1 . N1 . C1 . 117.80(13) yes Sc1 . N2 . C3 . 111.87(12) yes Sc1 . N2 . C4 . 110.27(12) yes C3 . N2 . C4 . 107.86(15) yes Sc1 . N2 . C10 . 110.11(12) yes C3 . N2 . C10 . 107.39(16) yes C4 . N2 . C10 . 109.25(16) yes Sc1 . N3 . Si2 . 127.64(9) yes Sc1 . N3 . C6 . 113.71(12) yes Si2 . N3 . C6 . 118.56(13) yes N1 . Si1 . C7 . 111.61(11) yes N1 . Si1 . C8 . 112.4(1) yes C7 . Si1 . C8 . 106.94(13) yes N1 . Si1 . C9 . 108.86(9) yes C7 . Si1 . C9 . 108.43(13) yes C8 . Si1 . C9 . 108.44(11) yes N3 . Si2 . C11 . 111.76(9) yes N3 . Si2 . C12 . 112.6(1) yes C11 . Si2 . C12 . 106.31(11) yes N3 . Si2 . C13 . 109.36(9) yes C11 . Si2 . C13 . 108.5(1) yes C12 . Si2 . C13 . 108.16(11) yes N1 . C1 . C2 . 114.80(17) yes C1 . C2 . C3 . 113.98(18) yes N2 . C3 . C2 . 115.58(16) yes N2 . C4 . C5 . 115.89(17) yes C4 . C5 . C6 . 113.56(17) yes N3 . C6 . C5 . 112.87(17) yes Cl101 . Sc101 . Cl101 2_556 80.779(19) yes Cl101 . Sc101 . N101 . 128.72(5) yes Cl101 2_556 Sc101 . N101 . 95.83(5) yes Cl101 . Sc101 . N102 . 88.71(5) yes Cl101 2_556 Sc101 . N102 . 168.59(5) yes N101 . Sc101 . N102 . 87.25(6) yes Cl101 . Sc101 . N103 . 111.09(5) yes Cl101 2_556 Sc101 . N103 . 100.74(5) yes N101 . Sc101 . N103 . 119.71(7) yes N102 . Sc101 . N103 . 87.13(6) yes Sc101 . Cl101 . Sc101 2_556 99.221(19) yes Sc101 . N101 . Si101 . 127.70(9) yes Sc101 . N101 . C101 . 114.18(12) yes Si101 . N101 . C101 . 117.71(13) yes Sc101 . N102 . C103 . 110.76(12) yes Sc101 . N102 . C104 . 112.14(12) yes C103 . N102 . C104 . 107.88(16) yes Sc101 . N102 . C110 . 109.75(12) yes C103 . N102 . C110 . 109.10(16) yes C104 . N102 . C110 . 107.10(17) yes Sc101 . N103 . Si102 . 128.8(1) yes Sc101 . N103 . C106 . 115.06(13) yes Si102 . N103 . C106 . 116.05(13) yes N101 . Si101 . C107 . 108.86(9) yes N101 . Si101 . C108 . 111.58(9) yes C107 . Si101 . C108 . 108.23(11) yes N101 . Si101 . C109 . 113.2(1) yes C107 . Si101 . C109 . 107.90(11) yes C108 . Si101 . C109 . 106.87(11) yes N103 . Si102 . C111 . 111.07(11) yes N103 . Si102 . C112 . 109.2(1) yes C111 . Si102 . C112 . 109.85(12) yes N103 . Si102 . C113 . 112.32(11) yes C111 . Si102 . C113 . 107.01(13) yes C112 . Si102 . C113 . 107.35(13) yes N101 . C101 . C102 . 112.79(18) yes C101 . C102 . C103 . 113.33(18) yes N102 . C103 . C102 . 116.06(17) yes N102 . C104 . C105 . 115.29(18) yes C104 . C105 . C106 . 113.91(18) yes N103 . C106 . C105 . 114.12(17) yes #===end data_COMPOUND_6 _database_code_CSD 194290 # Local code STR121 _chemical_name_systematic ; [Sc(N2_Mes_Npy)(CH2SiMe3)(THF)] ; _chemical_name_common ? _chemical_formula_moiety 'C37 H57 N3 O1.5 Sc1 Si1' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C37 H57 N3 O1.5 Sc1 Si1' _chemical_formula_weight 640.93 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_deScription _atom_type_Scat_dispersion_real _atom_type_Scat_dispersion_imag _atom_type_Scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Sc ? 0.226 0.372 International_Tables_Vol_IV_Table_2.3.1 Si ? 0.072 0.071 International_Tables_Vol_IV_Table_2.3.1 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 9.2011(2) _cell_length_b 10.1961(3) _cell_length_c 20.9786(6) _cell_angle_alpha 93.499(5) _cell_angle_beta 102.357(5) _cell_angle_gamma 103.593(5) _cell_volume 1855.8(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 10528 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_deScription prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.15 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 694 _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9541 _exptl_absorpt_correction_T_max 1.0000 _diffrn_special_details ; Residual electron density was modelled as a THF of crystallisation (0.5 per molecule of [Sc(N2NpyMes)(CH2SiMe3)(THF)] ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p Scans' _diffrn_measurement_details ; 10528 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 30. mm. Scan angle = 1.6 deg 1 Scans of 60 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.30 Omega = 0.00 Kappa = 0.00 114 frames Friedel pairs were averaged. Internal R = 0.03 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10528 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7849 _reflns_number_gt 4972 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_Scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4972 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.093 _refine_ls_R_factor_gt 0.056 _refine_ls_wR_factor_all 0.117 _refine_ls_wR_factor_ref 0.087 _refine_ls_goodness_of_fit_all 2.043 _refine_ls_goodness_of_fit_ref 1.487 _refine_ls_shift/su_max 0.010 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.744 _refine_diff_density_min -0.170 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 _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol Sc1 0.73848(6) 0.12540(6) 0.26467(3) 0.0264(2) 1.000 Uani ? ? Sc N1 0.5143(3) 0.0285(3) 0.2687(1) 0.030(1) 1.000 Uani ? ? N C1 0.4502(3) -0.0712(3) 0.3051(1) 0.032(1) 1.000 Uani ? ? C C2 0.3320(3) -0.1886(3) 0.2759(2) 0.037(2) 1.000 Uani ? ? C C3 0.2659(4) -0.2772(4) 0.3152(2) 0.043(2) 1.000 Uani ? ? C C4 0.3161(4) -0.2614(3) 0.3830(2) 0.048(2) 1.000 Uani ? ? C C5 0.4408(4) -0.1524(3) 0.4112(2) 0.045(2) 1.000 Uani ? ? C C6 0.5092(3) -0.0590(3) 0.3738(2) 0.034(1) 1.000 Uani ? ? C C7 0.2840(5) -0.2238(4) 0.2023(2) 0.054(2) 1.000 Uani ? ? C C8 0.2395(5) -0.3578(4) 0.4246(2) 0.070(2) 1.000 Uani ? ? C C9 0.6435(4) 0.0574(4) 0.4065(2) 0.041(2) 1.000 Uani ? ? C C10 0.3997(3) 0.0795(4) 0.2241(2) 0.038(2) 1.000 Uani ? ? C C11 0.4505(3) 0.2254(3) 0.2051(2) 0.040(2) 1.000 Uani ? ? C C12 0.3025(4) 0.2565(4) 0.1687(2) 0.056(2) 1.000 Uani ? ? C C13 0.5333(3) 0.3292(3) 0.2648(2) 0.040(1) 1.000 Uani ? ? C N2 0.6685(3) 0.3137(3) 0.2981(1) 0.036(1) 1.000 Uani ? ? N C14 0.7476(4) 0.4030(3) 0.3516(2) 0.043(2) 1.000 Uani ? ? C C15 0.6957(5) 0.5107(4) 0.3726(2) 0.056(2) 1.000 Uani ? ? C C16 0.5590(4) 0.5260(4) 0.3387(2) 0.064(2) 1.000 Uani ? ? C C17 0.4762(4) 0.4367(4) 0.2845(2) 0.057(2) 1.000 Uani ? ? C C18 0.5523(4) 0.2311(4) 0.1540(2) 0.041(2) 1.000 Uani ? ? C N3 0.6902(3) 0.1830(3) 0.1738(1) 0.033(1) 1.000 Uani ? ? N C19 0.7714(3) 0.1853(3) 0.1229(1) 0.031(1) 1.000 Uani ? ? C C20 0.7328(4) 0.0748(4) 0.0737(2) 0.040(2) 1.000 Uani ? ? C C21 0.8104(4) 0.0821(4) 0.0235(2) 0.051(2) 1.000 Uani ? ? C C22 0.9244(4) 0.1932(4) 0.0199(2) 0.050(2) 1.000 Uani ? ? C C23 0.9633(4) 0.3000(4) 0.0691(2) 0.046(2) 1.000 Uani ? ? C C24 0.8892(3) 0.2993(3) 0.1205(2) 0.034(1) 1.000 Uani ? ? C C25 0.6081(5) -0.0505(4) 0.0749(2) 0.053(2) 1.000 Uani ? ? C C26 1.0048(5) 0.1993(6) -0.0363(2) 0.080(3) 1.000 Uani ? ? C C27 0.9358(4) 0.4191(4) 0.1720(2) 0.048(2) 1.000 Uani ? ? C C28 0.9924(3) 0.2103(3) 0.3177(2) 0.033(1) 1.000 Uani ? ? C Si1 1.1040(1) 0.1735(1) 0.39497(5) 0.0372(4) 1.000 Uani ? ? Si C29 1.0582(5) 0.2581(4) 0.4672(2) 0.050(2) 1.000 Uani ? ? C C30 1.0640(4) -0.0136(4) 0.4021(2) 0.058(2) 1.000 Uani ? ? C C31 1.3196(4) 0.2361(5) 0.4069(2) 0.059(2) 1.000 Uani ? ? C O1 0.7945(2) -0.0713(2) 0.2449(1) 0.039(1) 1.000 Uani ? ? O C32 0.7198(4) -0.2026(4) 0.2621(2) 0.050(2) 1.000 Uani ? ? C C33 0.7984(5) -0.3009(4) 0.2416(2) 0.082(2) 1.000 Uani ? ? C C34 0.8690(4) -0.2400(4) 0.1885(2) 0.064(2) 1.000 Uani ? ? C C35 0.9140(4) -0.0908(4) 0.2125(2) 0.048(2) 1.000 Uani ? ? C C36 0.6537(8) 0.4060(7) -0.0543(4) 0.124(2) 1.000 Uiso ? ? C O2 0.464(2) 0.465(2) -0.0171(7) 0.187(5) 0.500 Uiso ? ? O C37 0.624(1) 0.443(1) -0.0016(5) 0.191(4) 1.000 Uiso ? ? C H1 0.1824 -0.3523 0.2947 0.0579 1.000 Uiso calc C3 H H2 0.4807 -0.1413 0.4574 0.0531 1.000 Uiso calc C5 H H3 0.2038 -0.3052 0.1914 0.0766 1.000 Uiso calc C7 H H4 0.2484 -0.1520 0.1827 0.0766 1.000 Uiso calc C7 H H5 0.3695 -0.2362 0.1863 0.0766 1.000 Uiso calc C7 H H6 0.1570 -0.4254 0.3970 0.0884 1.000 Uiso calc C8 H H7 0.3122 -0.3998 0.4486 0.0884 1.000 Uiso calc C8 H H8 0.2008 -0.3090 0.4543 0.0884 1.000 Uiso calc C8 H H9 0.6762 0.1111 0.3743 0.0546 1.000 Uiso calc C9 H H10 0.6136 0.1116 0.4373 0.0546 1.000 Uiso calc C9 H H11 0.7256 0.0231 0.4286 0.0546 1.000 Uiso calc C9 H H12 0.3162 0.0771 0.2442 0.0514 1.000 Uiso calc C10 H H13 0.3655 0.0191 0.1845 0.0514 1.000 Uiso calc C10 H H14 0.2349 0.2546 0.1972 0.0724 1.000 Uiso calc C12 H H15 0.3260 0.3440 0.1543 0.0724 1.000 Uiso calc C12 H H16 0.2545 0.1902 0.1317 0.0724 1.000 Uiso calc C12 H H17 0.8426 0.3910 0.3756 0.0572 1.000 Uiso calc C14 H H18 0.7544 0.5726 0.4100 0.0748 1.000 Uiso calc C15 H H19 0.5204 0.5988 0.3525 0.0759 1.000 Uiso calc C16 H H20 0.3807 0.4477 0.2605 0.0663 1.000 Uiso calc C17 H H21 0.5831 0.3228 0.1458 0.0527 1.000 Uiso calc C18 H H22 0.4911 0.1770 0.1147 0.0527 1.000 Uiso calc C18 H H23 0.7833 0.0070 -0.0097 0.0685 1.000 Uiso calc C21 H H24 1.0436 0.3771 0.0679 0.0596 1.000 Uiso calc C23 H H25 0.5972 -0.1146 0.0383 0.0786 1.000 Uiso calc C25 H H26 0.6350 -0.0894 0.1144 0.0786 1.000 Uiso calc C25 H H27 0.5136 -0.0265 0.0728 0.0786 1.000 Uiso calc C25 H H28 1.0800 0.2835 -0.0306 0.1036 1.000 Uiso calc C26 H H29 1.0533 0.1268 -0.0369 0.1036 1.000 Uiso calc C26 H H30 0.9314 0.1915 -0.0767 0.1036 1.000 Uiso calc C26 H H31 1.0167 0.4862 0.1625 0.0654 1.000 Uiso calc C27 H H32 0.8502 0.4559 0.1724 0.0654 1.000 Uiso calc C27 H H33 0.9702 0.3913 0.2138 0.0654 1.000 Uiso calc C27 H H34 1.0041 0.3056 0.3242 0.0422 1.000 Uiso calc C28 H H35 1.0466 0.1905 0.2861 0.0422 1.000 Uiso calc C28 H H36 1.1170 0.2379 0.5067 0.0729 1.000 Uiso calc C29 H H37 1.0826 0.3536 0.4659 0.0729 1.000 Uiso calc C29 H H38 0.9517 0.2258 0.4656 0.0729 1.000 Uiso calc C29 H H39 1.1239 -0.0283 0.4426 0.0739 1.000 Uiso calc C30 H H40 0.9579 -0.0486 0.4005 0.0739 1.000 Uiso calc C30 H H41 1.0901 -0.0585 0.3668 0.0739 1.000 Uiso calc C30 H H42 1.3695 0.2135 0.4477 0.0869 1.000 Uiso calc C31 H H43 1.3508 0.1944 0.3722 0.0869 1.000 Uiso calc C31 H H44 1.3467 0.3319 0.4068 0.0869 1.000 Uiso calc C31 H H45 0.6142 -0.2282 0.2399 0.0644 1.000 Uiso calc C32 H H46 0.7287 -0.1979 0.3082 0.0644 1.000 Uiso calc C32 H H47 0.7272 -0.3860 0.2250 0.1034 1.000 Uiso calc C33 H H48 0.8755 -0.3125 0.2773 0.1034 1.000 Uiso calc C33 H H49 0.7967 -0.2594 0.1473 0.0799 1.000 Uiso calc C34 H H50 0.9564 -0.2720 0.1851 0.0799 1.000 Uiso calc C34 H H51 1.0118 -0.0664 0.2426 0.0592 1.000 Uiso calc C35 H H52 0.9167 -0.0383 0.1767 0.0592 1.000 Uiso calc C35 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Sc1 0.0229(2) 0.0290(3) 0.0278(3) 0.0070(2) 0.0068(2) 0.0068(2) Sc N1 0.024(1) 0.037(1) 0.032(1) 0.006(1) 0.0076(9) 0.009(1) N C1 0.025(1) 0.036(1) 0.036(1) 0.010(1) 0.013(1) 0.006(1) C C2 0.027(1) 0.041(2) 0.045(2) 0.004(1) 0.011(1) 0.002(1) C C3 0.033(1) 0.038(2) 0.064(2) 0.005(1) 0.019(1) 0.006(2) C C4 0.050(2) 0.035(2) 0.062(2) 0.016(1) 0.034(1) 0.018(1) C C5 0.045(1) 0.047(2) 0.044(2) 0.024(1) 0.022(1) 0.016(1) C C6 0.028(1) 0.035(1) 0.039(2) 0.013(1) 0.013(1) 0.007(1) C C7 0.051(2) 0.058(2) 0.053(2) -0.009(2) 0.009(2) -0.003(2) C C8 0.084(2) 0.047(2) 0.086(2) 0.011(2) 0.049(2) 0.022(2) C C9 0.038(2) 0.051(2) 0.035(2) 0.011(1) 0.005(1) 0.008(2) C C10 0.028(1) 0.051(2) 0.040(2) 0.009(1) 0.008(1) 0.010(2) C C11 0.032(1) 0.050(2) 0.041(2) 0.019(1) 0.014(1) 0.019(1) C C12 0.036(2) 0.084(2) 0.056(2) 0.029(2) 0.010(1) 0.031(2) C C13 0.035(1) 0.043(2) 0.044(2) 0.016(1) 0.020(1) 0.022(1) C N2 0.038(1) 0.034(1) 0.035(1) 0.012(1) 0.014(1) 0.009(1) N C14 0.053(2) 0.037(2) 0.042(2) 0.010(1) 0.012(1) 0.005(2) C C15 0.080(2) 0.036(2) 0.063(2) 0.013(2) 0.033(2) -0.002(2) C C16 0.076(2) 0.045(2) 0.077(2) 0.032(1) 0.047(1) 0.016(2) C C17 0.054(2) 0.050(2) 0.070(2) 0.029(1) 0.037(1) 0.027(2) C C18 0.037(1) 0.055(2) 0.035(2) 0.018(1) 0.010(1) 0.019(1) C N3 0.029(1) 0.040(1) 0.031(1) 0.011(1) 0.0104(9) 0.010(1) N C19 0.030(1) 0.040(2) 0.026(1) 0.012(1) 0.005(1) 0.008(1) C C20 0.044(2) 0.041(2) 0.035(2) 0.009(1) 0.004(1) 0.005(1) C C21 0.071(2) 0.059(2) 0.031(2) 0.028(2) 0.008(2) -0.005(2) C C22 0.049(2) 0.072(2) 0.036(2) 0.030(1) 0.016(1) 0.012(2) C C23 0.032(1) 0.062(2) 0.048(2) 0.012(1) 0.016(1) 0.022(2) C C24 0.032(1) 0.040(2) 0.032(1) 0.010(1) 0.009(1) 0.010(1) C C25 0.074(3) 0.043(2) 0.047(2) -0.002(2) -0.002(2) 0.002(2) C C26 0.072(2) 0.139(4) 0.050(2) 0.053(2) 0.030(2) 0.027(2) C C27 0.058(2) 0.037(2) 0.053(2) -0.000(2) 0.018(2) 0.008(2) C C28 0.029(1) 0.035(2) 0.035(1) 0.008(1) 0.008(1) 0.009(1) C Si1 0.0292(4) 0.0480(5) 0.0367(5) 0.0054(4) 0.0035(4) 0.0150(4) Si C29 0.063(2) 0.053(2) 0.038(2) -0.007(2) 0.005(2) 0.006(2) C C30 0.055(2) 0.061(2) 0.059(2) 0.024(2) 0.008(2) 0.022(2) C C31 0.034(2) 0.096(3) 0.063(2) 0.008(2) -0.000(2) 0.032(2) C O1 0.0360(9) 0.031(1) 0.053(1) 0.0080(8) 0.0218(8) 0.007(1) O C32 0.053(2) 0.034(2) 0.068(2) 0.005(1) 0.035(1) 0.005(2) C C33 0.098(2) 0.045(2) 0.124(3) 0.024(2) 0.077(2) 0.024(2) C C34 0.062(2) 0.050(2) 0.085(2) 0.017(2) 0.042(2) 0.008(2) C C35 0.041(1) 0.045(2) 0.061(2) 0.017(1) 0.028(1) 0.011(2) C loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 N1 2.090(3) . . ? Sc1 N2 2.281(3) . . ? Sc1 N3 2.018(3) . . ? Sc1 C28 2.295(3) . . ? Sc1 O1 2.222(2) . . ? N1 C1 1.403(4) . . ? N1 C10 1.468(4) . . ? C1 C2 1.415(5) . . ? C1 C6 1.415(5) . . ? C2 C3 1.382(5) . . ? C2 C7 1.509(6) . . ? C3 C4 1.386(6) . . ? C4 C5 1.390(6) . . ? C4 C8 1.505(5) . . ? C5 C6 1.392(5) . . ? C6 C9 1.501(5) . . ? C10 C11 1.553(5) . . ? C11 C12 1.525(5) . . ? C11 C13 1.523(5) . . ? C11 C18 1.563(5) . . ? C13 N2 1.340(5) . . ? C13 C17 1.399(5) . . ? N2 C14 1.353(5) . . ? C14 C15 1.381(5) . . ? C15 C16 1.355(7) . . ? C16 C17 1.371(7) . . ? C18 N3 1.453(4) . . ? N3 C19 1.426(4) . . ? C19 C20 1.405(5) . . ? C19 C24 1.402(5) . . ? C20 C21 1.391(5) . . ? C20 C25 1.509(6) . . ? C21 C22 1.369(6) . . ? C22 C23 1.378(6) . . ? C22 C26 1.518(5) . . ? C23 C24 1.394(5) . . ? C24 C27 1.496(5) . . ? C28 Si1 1.835(4) . . ? Si1 C29 1.872(4) . . ? Si1 C30 1.877(5) . . ? Si1 C31 1.891(4) . . ? O1 C32 1.458(4) . . ? O1 C35 1.456(4) . . ? C32 C33 1.460(6) . . ? C33 C34 1.500(6) . . ? C34 C35 1.503(6) . . ? C36 C37 1.25(1) . . ? O2 C37 1.51(2) . . ? O2 C37 1.46(2) . 2_665 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sc1 N2 82.5(1) . . . ? N1 Sc1 N3 98.1(1) . . . ? N1 Sc1 C28 148.9(1) . . . ? N1 Sc1 O1 92.2(1) . . . ? N2 Sc1 N3 85.4(1) . . . ? N2 Sc1 C28 93.8(1) . . . ? N2 Sc1 O1 171.29(9) . . . ? N3 Sc1 C28 112.4(1) . . . ? N3 Sc1 O1 102.2(1) . . . ? C28 Sc1 O1 87.2(1) . . . ? C1 N1 C10 113.8(2) . . . ? N1 C1 C2 123.1(3) . . . ? N1 C1 C6 119.5(3) . . . ? C2 C1 C6 117.4(3) . . . ? C1 C2 C3 119.9(3) . . . ? C1 C2 C7 120.8(3) . . . ? C3 C2 C7 119.1(3) . . . ? C2 C3 C4 122.9(4) . . . ? C3 C4 C5 117.1(3) . . . ? C3 C4 C8 121.6(4) . . . ? C5 C4 C8 121.3(4) . . . ? C4 C5 C6 122.1(4) . . . ? C1 C6 C5 120.2(3) . . . ? C1 C6 C9 119.7(3) . . . ? C5 C6 C9 120.1(3) . . . ? N1 C10 C11 117.9(3) . . . ? C10 C11 C12 105.1(3) . . . ? C10 C11 C13 112.4(3) . . . ? C10 C11 C18 111.8(3) . . . ? C12 C11 C13 111.8(3) . . . ? C12 C11 C18 105.2(3) . . . ? C13 C11 C18 110.2(3) . . . ? C11 C13 N2 116.0(3) . . . ? C11 C13 C17 123.5(3) . . . ? N2 C13 C17 120.5(4) . . . ? C13 N2 C14 118.7(3) . . . ? N2 C14 C15 122.6(4) . . . ? C14 C15 C16 118.4(4) . . . ? C15 C16 C17 120.2(4) . . . ? C13 C17 C16 119.6(4) . . . ? C11 C18 N3 115.6(3) . . . ? C18 N3 C19 111.6(3) . . . ? N3 C19 C20 120.7(3) . . . ? N3 C19 C24 120.4(3) . . . ? C20 C19 C24 118.9(3) . . . ? C19 C20 C21 119.3(4) . . . ? C19 C20 C25 120.7(3) . . . ? C21 C20 C25 120.0(4) . . . ? C20 C21 C22 122.5(4) . . . ? C21 C22 C23 117.7(3) . . . ? C21 C22 C26 121.3(4) . . . ? C23 C22 C26 121.0(4) . . . ? C22 C23 C24 122.5(4) . . . ? C19 C24 C23 119.0(3) . . . ? C19 C24 C27 121.1(3) . . . ? C23 C24 C27 119.9(3) . . . ? C28 Si1 C29 110.7(2) . . . ? C28 Si1 C30 112.1(2) . . . ? C28 Si1 C31 114.2(2) . . . ? C29 Si1 C30 107.8(2) . . . ? C29 Si1 C31 105.3(2) . . . ? C30 Si1 C31 106.1(2) . . . ? C32 O1 C35 108.0(3) . . . ? O1 C32 C33 107.0(3) . . . ? C32 C33 C34 104.7(4) . . . ? C33 C34 C35 102.1(3) . . . ? O1 C35 C34 104.6(3) . . . ? C37 O2 C37 141(1) . . 2_665 ? C36 C37 O2 108(1) . . . ? C36 C37 O2 134(1) . . 2_665 ? O2 C37 O2 38(1) . . 2_665 ? #===end data_COMPOUND_11 _database_code_CSD 194291 # Local code AMF1 _chemical_name_systematic ; [Sc2(N2_Tol_Npy)2(CH2SiMe3)2] ; _publ_section_exptl_refinement ; Vibrational restraints were applied to the carbon atoms of one of the toluene molecules of crystallisation. ; _cell_length_a 10.7764(1) _cell_length_b 15.7709(2) _cell_length_c 22.4009(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.9372(5) _cell_angle_gamma 90.00 _cell_volume 3798.1(1) _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' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 '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 ' C82 H104 N6 Sc2 Si2 ' _chemical_formula_moiety ' C54 H62 N6 Sc2 Si2 . 4 C7H8' _chemical_compound_source ; ? ; _chemical_formula_weight 1319.86 _cell_measurement_reflns_used 8448 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.46 _exptl_crystal_density_diffrn 1.15 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1417.35 _exptl_absorpt_coefficient_mu 0.26 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.944 _exptl_absorpt_correction_T_max 0.949 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method 'CCD' _diffrn_ambient_temperature 150 _diffrn_reflns_number 16705 _reflns_number_total 8621 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_gt 4793 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _refine_diff_density_min -0.48 _refine_diff_density_max 0.71 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4793 _refine_ls_number_parameters 416 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0257 _refine_ls_goodness_of_fit_ref 1.1314 _refine_ls_shift/su_max 0.001 _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_number_restraints 36 _refine_ls_abs_structure_flack none _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 0.409E-02-.954 -.370 -.366 ; _refine_ls_extinction_coef 96(24) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD 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 'CAMERON (Watkin, Prout and Pearce, 1996)' _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 Sc1 0.85310(4) -0.03359(3) 0.50948(2) 0.0212 1.0000 Uani N1 0.94539(17) 0.07475(13) 0.46924(8) 0.0223 1.0000 Uani N2 0.80505(18) 0.02182(13) 0.58814(8) 0.0249 1.0000 Uani N3 0.68608(17) 0.04272(13) 0.47157(8) 0.0248 1.0000 Uani Si1 0.73127(7) -0.23182(5) 0.42085(3) 0.0314 1.0000 Uani C1 0.9167(2) 0.15167(16) 0.50272(11) 0.0245 1.0000 Uani C2 0.7836(2) 0.15942(16) 0.52768(11) 0.0262 1.0000 Uani C3 0.7800(2) 0.11236(17) 0.58840(11) 0.0284 1.0000 Uani C4 0.7670(3) 0.25367(17) 0.54149(13) 0.0352 1.0000 Uani C5 0.6818(2) 0.12647(16) 0.48342(11) 0.0257 1.0000 Uani C6 0.5892(2) 0.17794(18) 0.45626(12) 0.0321 1.0000 Uani C7 0.4998(2) 0.14180(19) 0.41664(12) 0.0352 1.0000 Uani C8 0.5033(2) 0.05619(19) 0.40510(12) 0.0352 1.0000 Uani C9 0.5978(2) 0.00896(18) 0.43333(11) 0.0311 1.0000 Uani C10 0.9077(2) 0.07532(16) 0.4068(1) 0.0225 1.0000 Uani C11 0.9117(2) -0.00158(16) 0.37583(11) 0.0251 1.0000 Uani C12 0.8873(2) -0.00593(17) 0.31450(11) 0.0298 1.0000 Uani C13 0.8576(2) 0.06630(19) 0.28094(11) 0.0331 1.0000 Uani C14 0.8453(3) 0.14143(18) 0.31193(12) 0.0351 1.0000 Uani C15 0.8680(2) 0.14672(17) 0.37360(11) 0.0293 1.0000 Uani C16 0.8437(3) 0.0632(2) 0.21352(12) 0.0495 1.0000 Uani C17 0.8033(2) -0.01745(17) 0.6441(1) 0.0277 1.0000 Uani C18 0.7909(2) 0.0257(2) 0.69833(11) 0.0364 1.0000 Uani C19 0.7943(3) -0.0184(2) 0.75262(12) 0.0464 1.0000 Uani C20 0.8077(3) -0.1049(2) 0.75571(13) 0.0467 1.0000 Uani C21 0.8173(3) -0.1483(2) 0.70193(13) 0.0415 1.0000 Uani C22 0.8146(2) -0.10595(18) 0.64787(12) 0.0329 1.0000 Uani C23 0.8113(4) -0.1524(3) 0.81480(15) 0.0719 1.0000 Uani C24 0.7675(2) -0.16006(16) 0.48532(11) 0.0279 1.0000 Uani C25 0.6419(3) -0.3277(2) 0.44302(15) 0.0562 1.0000 Uani C26 0.6348(3) -0.1825(2) 0.35696(14) 0.0515 1.0000 Uani C27 0.8774(3) -0.2694(2) 0.38857(15) 0.0530 1.0000 Uani C101 0.5464(4) 0.3302(2) 0.33147(17) 0.0637 1.0000 Uani C102 0.4541(4) 0.3637(3) 0.3652(2) 0.0807 1.0000 Uani C103 0.4869(6) 0.4132(3) 0.4139(2) 0.0948 1.0000 Uani C104 0.6091(7) 0.4300(3) 0.4313(2) 0.0961 1.0000 Uani C105 0.6992(5) 0.3975(3) 0.39866(19) 0.0730 1.0000 Uani C106 0.6680(4) 0.3475(2) 0.34907(18) 0.0596 1.0000 Uani C107 0.5127(5) 0.2756(3) 0.2781(2) 0.1016 1.0000 Uani C201 0.4861(3) -0.0361(4) 0.1795(2) 0.0821 1.0000 Uani C202 0.4592(4) 0.0164(3) 0.13306(18) 0.0675 1.0000 Uani C203 0.4213(4) -0.0139(4) 0.0767(2) 0.1030 1.0000 Uani C204 0.4135(5) -0.1068(5) 0.0688(3) 0.1095 1.0000 Uani C205 0.4420(5) -0.1504(4) 0.1197(3) 0.1025 1.0000 Uani C206 0.4755(4) -0.1194(4) 0.1730(3) 0.1020 1.0000 Uani C207 0.5248(4) -0.0009(5) 0.2404(2) 0.1327 1.0000 Uani H11 0.9793 0.15589 0.53767 0.0309 1.0000 Uiso H12 0.9266 0.20096 0.47536 0.0309 1.0000 Uiso H31 0.8430 0.13956 0.61713 0.0364 1.0000 Uiso H32 0.6951 0.12034 0.60293 0.0364 1.0000 Uiso H41 0.6838 0.26285 0.55759 0.0434 1.0000 Uiso H42 0.8338 0.27199 0.57195 0.0434 1.0000 Uiso H43 0.7728 0.28766 0.50409 0.0434 1.0000 Uiso H61 0.5874 0.24000 0.46533 0.0416 1.0000 Uiso H71 0.4332 0.17780 0.39632 0.0432 1.0000 Uiso H81 0.4390 0.02876 0.37712 0.0427 1.0000 Uiso H91 0.6012 -0.05330 0.42516 0.0389 1.0000 Uiso H111 0.9322 -0.05454 0.39901 0.0303 1.0000 Uiso H121 0.8922 -0.06192 0.29385 0.0371 1.0000 Uiso H141 0.8196 0.19380 0.28912 0.0427 1.0000 Uiso H151 0.8563 0.20177 0.39466 0.0362 1.0000 Uiso H161 0.8218 0.1209 0.19757 0.0628 1.0000 Uiso H162 0.9239 0.0444 0.19788 0.0628 1.0000 Uiso H163 0.7763 0.0223 0.20042 0.0628 1.0000 Uiso H181 0.7796 0.0886 0.69787 0.0461 1.0000 Uiso H191 0.7872 0.0141 0.79058 0.0547 1.0000 Uiso H211 0.8261 -0.2115 0.70260 0.0512 1.0000 Uiso H221 0.8203 -0.13895 0.61004 0.0401 1.0000 Uiso H231 0.8209 -0.2146 0.80755 0.0885 1.0000 Uiso H232 0.8835 -0.1316 0.84114 0.0885 1.0000 Uiso H233 0.7325 -0.1421 0.83476 0.0885 1.0000 Uiso H271 0.8559 -0.3076 0.35379 0.0646 1.0000 Uiso H272 0.9294 -0.3010 0.41985 0.0646 1.0000 Uiso H273 0.9251 -0.2194 0.37490 0.0646 1.0000 Uiso H1021 0.3644 0.3515 0.3540 0.1021 1.0000 Uiso H1031 0.4199 0.4377 0.4374 0.1192 1.0000 Uiso H1041 0.6306 0.4662 0.4672 0.1184 1.0000 Uiso H1051 0.7887 0.4089 0.41081 0.0938 1.0000 Uiso H1061 0.7357 0.3239 0.32557 0.0736 1.0000 Uiso H2021 0.4666 0.0789 0.13985 0.0901 1.0000 Uiso H2031 0.4004 0.0255 0.0425 0.1198 1.0000 Uiso H2041 0.3889 -0.1346 0.0296 0.1236 1.0000 Uiso H2051 0.4363 -0.2135 0.1162 0.1190 1.0000 Uiso H2061 0.4936 -0.1577 0.2081 0.1215 1.0000 Uiso H2071 0.5415 -0.0484 0.2694 0.1451 1.0000 Uiso H2072 0.6020 0.0338 0.2379 0.1451 1.0000 Uiso H2073 0.4566 0.0357 0.2543 0.1451 1.0000 Uiso H1071 0.5905 0.2577 0.2597 0.1284 1.0000 Uiso H1072 0.4668 0.2243 0.2907 0.1284 1.0000 Uiso H1073 0.4589 0.3084 0.2481 0.1284 1.0000 Uiso H241 0.8187 -0.19837 0.51272 0.0372 1.0000 Uiso H242 0.6830 -0.15305 0.50062 0.0372 1.0000 Uiso H251 0.6238 -0.3650 0.40742 0.0763 1.0000 Uiso H252 0.6925 -0.3597 0.47460 0.0763 1.0000 Uiso H253 0.5620 -0.3092 0.45912 0.0763 1.0000 Uiso H261 0.6200 -0.2252 0.32419 0.0689 1.0000 Uiso H262 0.6801 -0.1326 0.34158 0.0689 1.0000 Uiso H263 0.5532 -0.1636 0.37105 0.0689 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 0.0220(2) 0.0230(2) 0.0184(2) -0.0013(2) 0.00079(16) 0.0002(2) N1 0.025(1) 0.0243(11) 0.018(1) -0.0016(8) 0.0014(8) 0.0007(8) N2 0.025(1) 0.0315(12) 0.018(1) -0.0019(9) 0.0006(8) 0.0008(9) N3 0.022(1) 0.0302(12) 0.022(1) -0.0027(9) 0.0017(8) 0.0013(9) Si1 0.0370(4) 0.0284(4) 0.0286(4) -0.0043(3) 0.0013(3) -0.0056(3) C1 0.0281(13) 0.0237(13) 0.0217(12) -0.002(1) 0.001(1) -0.001(1) C2 0.0274(13) 0.0268(13) 0.0244(13) -0.0040(11) 0.002(1) 0.005(1) C3 0.0306(13) 0.0347(15) 0.0202(12) -0.0054(11) 0.003(1) 0.0020(11) C4 0.0390(15) 0.0306(15) 0.0362(15) -0.0074(12) 0.0041(12) 0.0068(12) C5 0.0227(12) 0.0331(14) 0.0217(12) 0.0006(11) 0.0045(9) 0.002(1) C6 0.0297(14) 0.0368(16) 0.0303(14) 0.0022(12) 0.0055(11) 0.0077(12) C7 0.0248(13) 0.0488(18) 0.0319(15) 0.0087(13) 0.0004(11) 0.0071(12) C8 0.0232(13) 0.0495(19) 0.0322(14) 0.0008(13) -0.0034(11) 0.0005(12) C9 0.0260(13) 0.0377(16) 0.0294(14) -0.0043(12) 0.001(1) -0.0014(11) C10 0.0199(12) 0.0251(13) 0.0226(12) 0.002(1) 0.0020(9) -0.001(1) C11 0.0252(12) 0.0247(12) 0.0252(12) 0.000(1) 0.000(1) -0.000(1) C12 0.0307(13) 0.0332(14) 0.0252(13) -0.0071(11) 0.001(1) 0.0005(11) C13 0.0336(14) 0.0414(16) 0.0235(13) -0.0006(12) -0.003(1) 0.0045(12) C14 0.0437(16) 0.0346(16) 0.0266(14) 0.0043(12) -0.0010(12) 0.0106(12) C15 0.0361(15) 0.0282(14) 0.0236(13) 0.0002(11) 0.002(1) 0.0050(11) C16 0.065(2) 0.056(2) 0.0268(15) -0.0009(14) -0.0049(14) 0.0097(17) C17 0.0206(11) 0.0415(17) 0.0206(12) 0.0025(11) 0.0000(9) -0.0025(11) C18 0.0395(15) 0.0488(18) 0.0213(13) -0.0007(13) 0.0049(11) -0.0019(14) C19 0.0504(18) 0.068(2) 0.0214(14) -0.0018(14) 0.0070(12) -0.0017(16) C20 0.0434(17) 0.072(2) 0.0248(15) 0.0146(15) 0.0049(12) 0.0018(16) C21 0.0381(16) 0.0516(19) 0.0354(16) 0.0128(14) 0.0067(12) 0.0077(14) C22 0.0291(14) 0.0416(17) 0.0280(14) 0.0019(12) 0.0025(11) 0.0010(12) C23 0.091(3) 0.091(3) 0.0350(19) 0.023(2) 0.0125(18) 0.016(2) C24 0.0290(13) 0.0278(14) 0.0271(13) -0.0005(11) 0.003(1) -0.0029(11) C25 0.079(2) 0.044(2) 0.0460(19) -0.0060(16) 0.0027(17) -0.0252(18) C26 0.070(2) 0.0433(19) 0.0391(17) -0.0100(15) -0.0148(15) -0.0007(16) C27 0.0448(18) 0.060(2) 0.055(2) -0.0307(18) 0.0041(15) -0.0012(16) C101 0.087(3) 0.047(2) 0.058(2) 0.0171(18) 0.007(2) 0.001(2) C102 0.077(3) 0.067(3) 0.102(4) 0.044(3) 0.027(3) 0.019(2) C103 0.135(5) 0.066(3) 0.090(4) 0.027(3) 0.056(4) 0.037(3) C104 0.188(6) 0.045(2) 0.057(3) 0.010(2) 0.021(3) 0.008(3) C105 0.105(3) 0.051(2) 0.063(3) 0.018(2) 0.007(2) -0.003(2) C106 0.073(3) 0.041(2) 0.067(2) 0.0149(18) 0.019(2) 0.0127(18) C107 0.145(5) 0.086(4) 0.073(3) 0.018(3) -0.006(3) -0.020(3) C201 0.0422(19) 0.121(3) 0.084(3) 0.018(3) 0.0086(18) -0.010(2) C202 0.076(2) 0.060(2) 0.068(2) 0.005(2) 0.011(2) -0.002(2) C203 0.082(3) 0.147(4) 0.079(3) 0.020(3) 0.004(2) 0.022(3) C204 0.070(3) 0.154(5) 0.104(4) -0.050(4) 0.007(3) -0.013(3) C205 0.081(3) 0.085(4) 0.145(5) -0.035(4) 0.037(4) -0.006(3) C206 0.060(3) 0.099(4) 0.151(5) 0.036(4) 0.035(3) 0.011(3) C207 0.070(3) 0.240(7) 0.088(4) -0.002(4) 0.004(3) -0.016(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag SC N1 2.090(3) . . ? SC N2 2.281(3) . . ? SC N3 2.018(3) . . ? SC C28 2.295(3) . . ? SC O1 2.222(2) . . ? N1 C1 1.403(4) . . ? N1 C10 1.468(4) . . ? C1 C2 1.415(5) . . ? C1 C6 1.415(5) . . ? C2 C3 1.382(5) . . ? C2 C7 1.509(6) . . ? C3 C4 1.386(6) . . ? C4 C5 1.390(6) . . ? C4 C8 1.505(5) . . ? C5 C6 1.392(5) . . ? C6 C9 1.501(5) . . ? C10 C11 1.553(5) . . ? C11 C12 1.525(5) . . ? C11 C13 1.523(5) . . ? C11 C18 1.563(5) . . ? C13 N2 1.340(5) . . ? C13 C17 1.399(5) . . ? N2 C14 1.353(5) . . ? C14 C15 1.381(5) . . ? C15 C16 1.355(7) . . ? C16 C17 1.371(7) . . ? C18 N3 1.453(4) . . ? N3 C19 1.426(4) . . ? C19 C20 1.405(5) . . ? C19 C24 1.402(5) . . ? C20 C21 1.391(5) . . ? C20 C25 1.509(6) . . ? C21 C22 1.369(6) . . ? C22 C23 1.378(6) . . ? C22 C26 1.518(5) . . ? C23 C24 1.394(5) . . ? C24 C27 1.496(5) . . ? C28 SI 1.835(4) . . ? SI C29 1.872(4) . . ? SI C30 1.877(5) . . ? SI C31 1.891(4) . . ? O1 C32 1.458(4) . . ? O1 C35 1.456(4) . . ? C32 C33 1.460(6) . . ? C33 C34 1.500(6) . . ? C34 C35 1.503(6) . . ? C36 C37 1.25(1) . . ? O2 C37 1.51(2) . . ? O2 C37 1.46(2) . 2_665 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 SC N2 82.5(1) . . . ? N1 SC N3 98.1(1) . . . ? N1 SC C28 148.9(1) . . . ? N1 SC O1 92.2(1) . . . ? N2 SC N3 85.4(1) . . . ? N2 SC C28 93.8(1) . . . ? N2 SC O1 171.29(9) . . . ? N3 SC C28 112.4(1) . . . ? N3 SC O1 102.2(1) . . . ? C28 SC O1 87.2(1) . . . ? C1 N1 C10 113.8(2) . . . ? N1 C1 C2 123.1(3) . . . ? N1 C1 C6 119.5(3) . . . ? C2 C1 C6 117.4(3) . . . ? C1 C2 C3 119.9(3) . . . ? C1 C2 C7 120.8(3) . . . ? C3 C2 C7 119.1(3) . . . ? C2 C3 C4 122.9(4) . . . ? C3 C4 C5 117.1(3) . . . ? C3 C4 C8 121.6(4) . . . ? C5 C4 C8 121.3(4) . . . ? C4 C5 C6 122.1(4) . . . ? C1 C6 C5 120.2(3) . . . ? C1 C6 C9 119.7(3) . . . ? C5 C6 C9 120.1(3) . . . ? N1 C10 C11 117.9(3) . . . ? C10 C11 C12 105.1(3) . . . ? C10 C11 C13 112.4(3) . . . ? C10 C11 C18 111.8(3) . . . ? C12 C11 C13 111.8(3) . . . ? C12 C11 C18 105.2(3) . . . ? C13 C11 C18 110.2(3) . . . ? C11 C13 N2 116.0(3) . . . ? C11 C13 C17 123.5(3) . . . ? N2 C13 C17 120.5(4) . . . ? C13 N2 C14 118.7(3) . . . ? N2 C14 C15 122.6(4) . . . ? C14 C15 C16 118.4(4) . . . ? C15 C16 C17 120.2(4) . . . ? C13 C17 C16 119.6(4) . . . ? C11 C18 N3 115.6(3) . . . ? C18 N3 C19 111.6(3) . . . ? N3 C19 C20 120.7(3) . . . ? N3 C19 C24 120.4(3) . . . ? C20 C19 C24 118.9(3) . . . ? C19 C20 C21 119.3(4) . . . ? C19 C20 C25 120.7(3) . . . ? C21 C20 C25 120.0(4) . . . ? C20 C21 C22 122.5(4) . . . ? C21 C22 C23 117.7(3) . . . ? C21 C22 C26 121.3(4) . . . ? C23 C22 C26 121.0(4) . . . ? C22 C23 C24 122.5(4) . . . ? C19 C24 C23 119.0(3) . . . ? C19 C24 C27 121.1(3) . . . ? C23 C24 C27 119.9(3) . . . ? C28 SI C29 110.7(2) . . . ? C28 SI C30 112.1(2) . . . ? C28 SI C31 114.2(2) . . . ? C29 SI C30 107.8(2) . . . ? C29 SI C31 105.3(2) . . . ? C30 SI C31 106.1(2) . . . ? C32 O1 C35 108.0(3) . . . ? O1 C32 C33 107.0(3) . . . ? C32 C33 C34 104.7(4) . . . ? C33 C34 C35 102.1(3) . . . ? O1 C35 C34 104.6(3) . . . ? C37 O2 C37 141(1) . . 2_665 ? C36 C37 O2 108(1) . . . ? C36 C37 O2 134(1) . . 2_665 ? O2 C37 O2 38(1) . . 2_665 ? #===end