Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'Sept 17 15:42:34 2005' _audit_update_record ; Sep 17, 2005 updated by author Karl W. Tornroos ; #=============================================================================== _journal_coden_Cambridge 222 _publ_contact_author_name # Name of author for correspondence ; Reiner Anwander ; _publ_contact_author_address # address of author for correspondence ; Department of Chemistry University of Bergen Allegaten 41 5007 Bergen (Norway) ; _publ_contact_author_email reiner.anwander@kj.uib.no _publ_contact_author_fax '47 55589490' _publ_contact_author_phone '47 55589491' _publ_requested_journal 'Dalton Trans.' _publ_section_title ; Synthesis and structural characterization of scandium SALEN complexes ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Meermann, C.' ; Department of Chemistry University of Bergen Allegaten 41 5007 Bergen (Norway) ; 'Sirsch, P.' ; Department of Chemistry University of New Brunswick Fredericton, NB E3B 6E2 (Canada) ; 'Tornroos, K. W.' ; Department of Chemistry University of Bergen Allegaten 41 5007 Bergen (Norway) ; 'Anwander, R.' ; Department of Chemistry University of Bergen Allegaten 41 5007 Bergen (Norway) ; #=========================================================================== data_cm60 # Compound 6 _database_code_depnum_ccdc_archive 'CCDC 284496' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [N,N'-bis(3,5-di-tert.-butylsalicylidene)-2,2-dimethyl propylendiamino][diisopropylamido]scandium(III) (Salpren)Sc(NiPr2) n-hexane solvate ; _chemical_name_common '(Salpren)Sc(NiPr2) n-hexane solvate' _chemical_melting_point ? _chemical_formula_moiety 'C41 H64 N3 O2 Sc, 0.5(C6 H14)' _chemical_formula_sum 'C44 H73 N3 O2 Sc' _chemical_formula_weight 721.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_HALL '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9991(9) _cell_length_b 11.0506(6) _cell_length_c 25.1676(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.2030(10) _cell_angle_gamma 90.00 _cell_volume 4414.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 15687 _cell_measurement_theta_min 2.443 _cell_measurement_theta_max 24.962 _exptl_crystal_description 'flat prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.93051 _exptl_absorpt_correction_T_max 0.97290 _exptl_absorpt_process_details ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_special_details ; Crystals diffracts very poorly also at 123K. R~int~ is 0.10 despite numerical absorption and incident beam corrections. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART 2K CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean '48 \mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49571 _diffrn_reflns_av_R_equivalents 0.1005 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.05 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_theta_full 25.05 _reflns_number_total 7798 _reflns_number_gt 5253 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; Bruker (1999). SMART, version 5.059, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_cell_refinement ; Bruker (2001). SAINT, version 6.02a, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_data_reduction ; Bruker (2001). SAINT, version 6.02a, Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_structure_solution ; Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Gottingen, Germany. ; _computing_structure_refinement ; Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Gottingen, Germany. ; _computing_molecular_graphics ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _computing_publication_material ; Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, Wisconsin, USA. ; _refine_special_details ; Refinement of F^2^ against ALL reflections except 1 0 0 which was evidently in error. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The diisopropylamine ligand is two fold disordered (ratio 52:48). There is two fold disorder in the hexane molecule (ratio 76:24). Total Potential Solvent Area Vol 75.4 Ang^3^ was found. All hydrogen atoms were calculated in idealized geometry and refined using a riding group model. Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.2890 0.8638 0.2599 [ 0.98 A from N2 ] Deepest hole -0.35 at 0.2776 0.7568 0.2799 [ 0.69 A from SC ] ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+6.6036P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7798 _refine_ls_number_parameters 495 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.324 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.058 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc Sc 0.30766(4) 0.74343(6) 0.26320(2) 0.02151(15) Uani 1 1 d . . . O1 O 0.22070(13) 0.6140(2) 0.24982(8) 0.0253(5) Uani 1 1 d . A . N1 N 0.23477(16) 0.7803(2) 0.33362(10) 0.0259(6) Uani 1 1 d . A . C1 C 0.2485(2) 1.0045(3) 0.34576(13) 0.0366(9) Uani 1 1 d . A . O2 O 0.33077(13) 0.7636(2) 0.18679(8) 0.0272(5) Uani 1 1 d . A . N2 N 0.30342(18) 0.9496(2) 0.25791(10) 0.0289(6) Uani 1 1 d . A . C2 C 0.2620(2) 0.8797(3) 0.37052(12) 0.0320(8) Uani 1 1 d . . . H2A H 0.3226 0.8694 0.3834 0.038 Uiso 1 1 calc R A . H2B H 0.2307 0.8744 0.4020 0.038 Uiso 1 1 calc R . . N3 N 0.41265(16) 0.6892(2) 0.30846(9) 0.0271(6) Uani 1 1 d D A . C3 C 0.1760(2) 0.7115(3) 0.34738(12) 0.0295(8) Uani 1 1 d . . . H3A H 0.1542 0.7346 0.3793 0.035 Uiso 1 1 calc R A . C4 C 0.1386(2) 0.6051(3) 0.32160(12) 0.0275(7) Uani 1 1 d . A . C5 C 0.16297(19) 0.5573(3) 0.27365(11) 0.0241(7) Uani 1 1 d . . . C6 C 0.12408(19) 0.4488(3) 0.25301(12) 0.0249(7) Uani 1 1 d . A . C7 C 0.1464(2) 0.3930(3) 0.20067(12) 0.0272(7) Uani 1 1 d . . . C8 C 0.0994(2) 0.2741(3) 0.18638(14) 0.0371(9) Uani 1 1 d . A . H8A H 0.0385 0.2889 0.1823 0.056 Uiso 1 1 calc R . . H8B H 0.1141 0.2150 0.2150 0.056 Uiso 1 1 calc R . . H8C H 0.1155 0.2426 0.1527 0.056 Uiso 1 1 calc R . . C9 C 0.2414(2) 0.3658(3) 0.20625(13) 0.0319(8) Uani 1 1 d . A . H9A H 0.2731 0.4416 0.2121 0.048 Uiso 1 1 calc R . . H9B H 0.2552 0.3269 0.1735 0.048 Uiso 1 1 calc R . . H9C H 0.2565 0.3117 0.2368 0.048 Uiso 1 1 calc R . . C10 C 0.1228(2) 0.4816(3) 0.15455(12) 0.0337(8) Uani 1 1 d . A . H10A H 0.0616 0.4936 0.1495 0.051 Uiso 1 1 calc R . . H10B H 0.1407 0.4486 0.1216 0.051 Uiso 1 1 calc R . . H10C H 0.1509 0.5593 0.1630 0.051 Uiso 1 1 calc R . . C11 C 0.0646(2) 0.3948(3) 0.28100(12) 0.0282(7) Uani 1 1 d . . . H11A H 0.0393 0.3217 0.2671 0.034 Uiso 1 1 calc R A . C12 C 0.0392(2) 0.4416(3) 0.32908(12) 0.0285(8) Uani 1 1 d . A . C13 C -0.0242(2) 0.3720(3) 0.35807(13) 0.0305(8) Uani 1 1 d . . . C14 C 0.0170(2) 0.2568(3) 0.38179(14) 0.0410(9) Uani 1 1 d . A . H14A H 0.0650 0.2778 0.4083 0.062 Uiso 1 1 calc R . . H14B H 0.0366 0.2082 0.3532 0.062 Uiso 1 1 calc R . . H14C H -0.0241 0.2102 0.3991 0.062 Uiso 1 1 calc R . . C15 C -0.0542(2) 0.4479(3) 0.40306(14) 0.0409(9) Uani 1 1 d . A . H15A H -0.0065 0.4642 0.4305 0.061 Uiso 1 1 calc R . . H15B H -0.0978 0.4033 0.4191 0.061 Uiso 1 1 calc R . . H15C H -0.0775 0.5246 0.3883 0.061 Uiso 1 1 calc R . . C16 C -0.1020(2) 0.3381(4) 0.31854(15) 0.0450(10) Uani 1 1 d . A . H16A H -0.0847 0.2861 0.2903 0.068 Uiso 1 1 calc R . . H16B H -0.1281 0.4119 0.3025 0.068 Uiso 1 1 calc R . . H16C H -0.1426 0.2949 0.3376 0.068 Uiso 1 1 calc R . . C17 C 0.0774(2) 0.5467(3) 0.34787(12) 0.0294(8) Uani 1 1 d . . . H17A H 0.0621 0.5814 0.3798 0.035 Uiso 1 1 calc R A . C18 C 0.1581(3) 1.0213(4) 0.31976(16) 0.0549(12) Uani 1 1 d . . . H18A H 0.1461 0.9637 0.2902 0.082 Uiso 1 1 calc R A . H18B H 0.1507 1.1041 0.3060 0.082 Uiso 1 1 calc R . . H18C H 0.1195 1.0071 0.3464 0.082 Uiso 1 1 calc R . . C19 C 0.2695(3) 1.0971(4) 0.39135(14) 0.0521(11) Uani 1 1 d . . . H19A H 0.2309 1.0859 0.4183 0.078 Uiso 1 1 calc R A . H19B H 0.2633 1.1793 0.3767 0.078 Uiso 1 1 calc R . . H19C H 0.3276 1.0850 0.4080 0.078 Uiso 1 1 calc R . . C20 C 0.3117(3) 1.0288(3) 0.30597(13) 0.0389(9) Uani 1 1 d . . . H20A H 0.3054 1.1140 0.2939 0.047 Uiso 1 1 calc R A . H20B H 0.3694 1.0195 0.3250 0.047 Uiso 1 1 calc R . . C21 C 0.2948(2) 1.0077(3) 0.21305(12) 0.0331(8) Uani 1 1 d . . . H21A H 0.2848 1.0921 0.2158 0.040 Uiso 1 1 calc R A . C22 C 0.2980(2) 0.9637(3) 0.15921(12) 0.0267(7) Uani 1 1 d . A . C23 C 0.32051(19) 0.8443(3) 0.14831(11) 0.0245(7) Uani 1 1 d . . . C24 C 0.3334(2) 0.8147(3) 0.09427(12) 0.0266(7) Uani 1 1 d . A . C25 C 0.3659(2) 0.6898(3) 0.08022(12) 0.0325(8) Uani 1 1 d . . . C26 C 0.3737(3) 0.6772(4) 0.01993(13) 0.0529(12) Uani 1 1 d . A . H26A H 0.3187 0.6917 -0.0009 0.079 Uiso 1 1 calc R . . H26B H 0.3931 0.5954 0.0126 0.079 Uiso 1 1 calc R . . H26C H 0.4144 0.7365 0.0098 0.079 Uiso 1 1 calc R . . C27 C 0.3063(3) 0.5899(3) 0.09433(14) 0.0418(9) Uani 1 1 d . A . H27A H 0.3025 0.5917 0.1329 0.063 Uiso 1 1 calc R . . H27B H 0.3280 0.5111 0.0846 0.063 Uiso 1 1 calc R . . H27C H 0.2503 0.6030 0.0746 0.063 Uiso 1 1 calc R . . C28 C 0.4537(2) 0.6698(4) 0.11055(15) 0.0442(10) Uani 1 1 d . A . H28A H 0.4512 0.6766 0.1491 0.066 Uiso 1 1 calc R . . H28B H 0.4925 0.7309 0.0996 0.066 Uiso 1 1 calc R . . H28C H 0.4739 0.5889 0.1024 0.066 Uiso 1 1 calc R . . C29 C 0.3176(2) 0.9052(3) 0.05608(12) 0.0295(8) Uani 1 1 d . . . H29A H 0.3257 0.8856 0.0203 0.035 Uiso 1 1 calc R A . C30 C 0.2908(2) 1.0230(3) 0.06577(12) 0.0283(8) Uani 1 1 d . A . C31 C 0.2753(2) 1.1155(3) 0.02000(13) 0.0340(8) Uani 1 1 d . . . C32 C 0.2320(3) 1.2292(4) 0.03737(15) 0.0563(12) Uani 1 1 d . A . H32A H 0.2698 1.2714 0.0650 0.084 Uiso 1 1 calc R . . H32B H 0.1801 1.2066 0.0518 0.084 Uiso 1 1 calc R . . H32C H 0.2184 1.2827 0.0064 0.084 Uiso 1 1 calc R . . C33 C 0.3601(3) 1.1521(4) 0.00253(15) 0.0506(11) Uani 1 1 d . A . H33A H 0.3945 1.1922 0.0323 0.076 Uiso 1 1 calc R . . H33B H 0.3505 1.2077 -0.0280 0.076 Uiso 1 1 calc R . . H33C H 0.3894 1.0798 -0.0080 0.076 Uiso 1 1 calc R . . C34 C 0.2197(3) 1.0597(4) -0.02746(15) 0.0539(11) Uani 1 1 d . A . H34A H 0.2090 1.1197 -0.0562 0.081 Uiso 1 1 calc R . . H34B H 0.1661 1.0340 -0.0161 0.081 Uiso 1 1 calc R . . H34C H 0.2484 0.9895 -0.0406 0.081 Uiso 1 1 calc R . . C35 C 0.2832(2) 1.0510(3) 0.11832(12) 0.0300(8) Uani 1 1 d . . . H35A H 0.2677 1.1308 0.1271 0.036 Uiso 1 1 calc R A . C36 C 0.4333(5) 0.5982(5) 0.35109(18) 0.0394(19) Uani 0.525(4) 1 d PD A 1 H36 H 0.4945 0.5778 0.3529 0.047 Uiso 0.525(4) 1 calc PR A 1 C37 C 0.3825(5) 0.4845(7) 0.3358(3) 0.0543(17) Uani 0.525(4) 1 d PD A 1 H37A H 0.3811 0.4697 0.2973 0.081 Uiso 0.525(4) 1 calc PR A 1 H37B H 0.3248 0.4951 0.3444 0.081 Uiso 0.525(4) 1 calc PR A 1 H37C H 0.4087 0.4154 0.3558 0.081 Uiso 0.525(4) 1 calc PR A 1 C38 C 0.4167(8) 0.6441(9) 0.4058(3) 0.050(2) Uani 0.525(4) 1 d PD A 1 H38A H 0.4192 0.5762 0.4310 0.074 Uiso 0.525(4) 1 calc PR A 1 H38B H 0.3608 0.6814 0.4028 0.074 Uiso 0.525(4) 1 calc PR A 1 H38C H 0.4595 0.7042 0.4187 0.074 Uiso 0.525(4) 1 calc PR A 1 C39 C 0.5011(3) 0.7280(10) 0.3095(4) 0.040(2) Uani 0.525(4) 1 d PD A 1 H39 H 0.5318 0.6604 0.3299 0.048 Uiso 0.525(4) 1 calc PR A 1 C40 C 0.526(2) 0.835(2) 0.3457(14) 0.071(4) Uani 0.525(4) 1 d PD A 1 H40A H 0.4803 0.8551 0.3665 0.106 Uiso 0.525(4) 1 calc PR A 1 H40B H 0.5381 0.9053 0.3239 0.106 Uiso 0.525(4) 1 calc PR A 1 H40C H 0.5770 0.8148 0.3702 0.106 Uiso 0.525(4) 1 calc PR A 1 C41 C 0.534(3) 0.718(3) 0.2556(8) 0.090(5) Uani 0.525(4) 1 d PD A 1 H41A H 0.4943 0.6712 0.2309 0.136 Uiso 0.525(4) 1 calc PR A 1 H41B H 0.5889 0.6766 0.2603 0.136 Uiso 0.525(4) 1 calc PR A 1 H41C H 0.5408 0.7989 0.2410 0.136 Uiso 0.525(4) 1 calc PR A 1 C36A C 0.4022(6) 0.5759(4) 0.3381(3) 0.0394(19) Uani 0.475(4) 1 d PD A 2 H36A H 0.3398 0.5631 0.3340 0.047 Uiso 0.475(4) 1 calc PR A 2 C37A C 0.4362(6) 0.4615(7) 0.3151(4) 0.0543(17) Uani 0.475(4) 1 d PD A 2 H37D H 0.4185 0.4586 0.2764 0.081 Uiso 0.475(4) 1 calc PR A 2 H37E H 0.4141 0.3905 0.3321 0.081 Uiso 0.475(4) 1 calc PR A 2 H37F H 0.4978 0.4615 0.3219 0.081 Uiso 0.475(4) 1 calc PR A 2 C38A C 0.4269(9) 0.5859(10) 0.3982(3) 0.050(2) Uani 0.475(4) 1 d PD A 2 H38D H 0.4038 0.6608 0.4113 0.074 Uiso 0.475(4) 1 calc PR A 2 H38E H 0.4885 0.5870 0.4061 0.074 Uiso 0.475(4) 1 calc PR A 2 H38F H 0.4045 0.5163 0.4160 0.074 Uiso 0.475(4) 1 calc PR A 2 C39A C 0.4807(4) 0.7629(10) 0.2903(4) 0.040(2) Uani 0.475(4) 1 d PD A 2 H39A H 0.4569 0.8241 0.2633 0.048 Uiso 0.475(4) 1 calc PR A 2 C40A C 0.533(3) 0.825(3) 0.3374(15) 0.071(4) Uani 0.475(4) 1 d PD A 2 H40D H 0.4971 0.8827 0.3538 0.106 Uiso 0.475(4) 1 calc PR A 2 H40E H 0.5801 0.8671 0.3249 0.106 Uiso 0.475(4) 1 calc PR A 2 H40F H 0.5537 0.7636 0.3641 0.106 Uiso 0.475(4) 1 calc PR A 2 C41A C 0.539(3) 0.676(3) 0.2658(10) 0.090(5) Uani 0.475(4) 1 d PD A 2 H41D H 0.5076 0.6361 0.2346 0.136 Uiso 0.475(4) 1 calc PR A 2 H41E H 0.5599 0.6150 0.2924 0.136 Uiso 0.475(4) 1 calc PR A 2 H41F H 0.5863 0.7211 0.2545 0.136 Uiso 0.475(4) 1 calc PR A 2 C1S C 0.0418(5) 0.7647(7) 0.4704(2) 0.073(2) Uani 0.761(5) 1 d PD B 3 H1S1 H -0.0045 0.7457 0.4911 0.110 Uiso 0.761(5) 1 calc PR B 3 H1S2 H 0.0818 0.6971 0.4730 0.110 Uiso 0.761(5) 1 calc PR B 3 H1S3 H 0.0193 0.7777 0.4328 0.110 Uiso 0.761(5) 1 calc PR B 3 C2S C 0.0864(4) 0.8785(6) 0.4926(3) 0.0633(19) Uani 0.761(5) 1 d PD B 3 H2S1 H 0.1072 0.8632 0.5308 0.076 Uiso 0.761(5) 1 calc PR B 3 H2S2 H 0.1366 0.8898 0.4738 0.076 Uiso 0.761(5) 1 calc PR B 3 C3S C 0.0409(4) 0.9920(6) 0.4898(2) 0.0601(17) Uani 0.761(5) 1 d PD . 3 H3S1 H 0.0323 1.0157 0.4516 0.072 Uiso 0.761(5) 1 calc PR B 3 H3S2 H 0.0796 1.0528 0.5084 0.072 Uiso 0.761(5) 1 calc PR B 3 C1SA C 0.1160(14) 0.7518(12) 0.4877(7) 0.073(2) Uani 0.239(5) 1 d PD B 4 H1S4 H 0.0945 0.6693 0.4815 0.110 Uiso 0.239(5) 1 calc PR B 4 H1S5 H 0.1452 0.7582 0.5242 0.110 Uiso 0.239(5) 1 calc PR B 4 H1S6 H 0.1554 0.7706 0.4620 0.110 Uiso 0.239(5) 1 calc PR B 4 C2SA C 0.0438(16) 0.840(2) 0.4806(10) 0.0633(19) Uani 0.239(5) 1 d PD B 4 H2S3 H 0.0527 0.8707 0.4449 0.076 Uiso 0.239(5) 1 calc PR B 4 H2S4 H -0.0023 0.7799 0.4727 0.076 Uiso 0.239(5) 1 calc PR B 4 C3SA C -0.0067(14) 0.9390(19) 0.4964(8) 0.0601(17) Uani 0.239(5) 1 d PD . 4 H3S3 H -0.0586 0.9350 0.4704 0.072 Uiso 0.239(5) 1 calc PR B 4 H3S4 H -0.0239 0.9119 0.5309 0.072 Uiso 0.239(5) 1 calc PR B 4 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 Sc 0.0249(3) 0.0263(3) 0.0137(3) -0.0011(3) 0.0043(2) -0.0011(3) O1 0.0254(12) 0.0333(13) 0.0180(11) -0.0035(9) 0.0060(9) -0.0028(10) N1 0.0290(15) 0.0310(16) 0.0180(13) -0.0051(11) 0.0038(11) -0.0018(12) C1 0.052(2) 0.037(2) 0.0207(17) -0.0091(15) 0.0073(16) 0.0020(17) O2 0.0377(13) 0.0277(13) 0.0168(10) -0.0003(10) 0.0053(9) 0.0025(10) N2 0.0431(17) 0.0282(15) 0.0155(13) -0.0042(12) 0.0045(12) 0.0013(13) C2 0.040(2) 0.038(2) 0.0193(16) -0.0083(15) 0.0100(15) -0.0059(16) N3 0.0274(15) 0.0364(16) 0.0177(13) -0.0005(12) 0.0037(11) -0.0049(12) C3 0.0307(18) 0.039(2) 0.0212(16) -0.0074(14) 0.0109(14) 0.0000(15) C4 0.0287(18) 0.0333(19) 0.0216(16) -0.0025(14) 0.0073(14) -0.0027(15) C5 0.0210(16) 0.0326(19) 0.0189(15) 0.0004(14) 0.0029(13) 0.0015(14) C6 0.0240(17) 0.0298(18) 0.0207(15) -0.0009(14) 0.0025(13) 0.0004(14) C7 0.0289(18) 0.0306(18) 0.0230(16) -0.0059(14) 0.0067(14) -0.0025(15) C8 0.041(2) 0.037(2) 0.0345(19) -0.0090(16) 0.0086(16) -0.0107(17) C9 0.0323(19) 0.034(2) 0.0310(18) -0.0071(15) 0.0104(15) 0.0029(15) C10 0.039(2) 0.040(2) 0.0213(17) -0.0040(15) 0.0024(15) 0.0005(16) C11 0.0262(18) 0.0314(19) 0.0269(17) -0.0005(15) 0.0026(14) 0.0006(14) C12 0.0242(17) 0.036(2) 0.0262(17) 0.0047(15) 0.0081(14) 0.0000(15) C13 0.0238(18) 0.038(2) 0.0306(18) 0.0024(15) 0.0071(14) -0.0052(15) C14 0.042(2) 0.042(2) 0.042(2) 0.0109(19) 0.0144(17) -0.0040(19) C15 0.044(2) 0.042(2) 0.041(2) 0.0008(18) 0.0242(18) -0.0052(18) C16 0.029(2) 0.067(3) 0.040(2) 0.005(2) 0.0066(17) -0.0108(19) C17 0.0277(18) 0.038(2) 0.0236(17) -0.0024(15) 0.0097(14) -0.0022(15) C18 0.063(3) 0.063(3) 0.039(2) -0.012(2) 0.010(2) 0.025(2) C19 0.091(3) 0.040(2) 0.028(2) -0.0132(18) 0.020(2) -0.002(2) C20 0.070(3) 0.029(2) 0.0198(17) -0.0046(15) 0.0122(17) -0.0032(18) C21 0.047(2) 0.0277(19) 0.0248(18) 0.0001(15) 0.0075(16) 0.0080(16) C22 0.0319(18) 0.0317(19) 0.0175(16) 0.0015(14) 0.0077(14) 0.0036(15) C23 0.0290(18) 0.0286(18) 0.0161(15) 0.0033(14) 0.0039(13) -0.0009(14) C24 0.0286(18) 0.0314(19) 0.0201(16) -0.0014(14) 0.0049(14) -0.0009(14) C25 0.050(2) 0.035(2) 0.0139(15) -0.0010(14) 0.0090(15) 0.0063(17) C26 0.099(3) 0.042(2) 0.0206(18) -0.0025(17) 0.019(2) 0.013(2) C27 0.063(3) 0.035(2) 0.0269(18) -0.0052(16) 0.0045(18) -0.0020(19) C28 0.048(2) 0.047(2) 0.040(2) -0.0027(18) 0.0134(18) 0.0127(19) C29 0.0360(19) 0.039(2) 0.0146(15) -0.0016(14) 0.0055(14) -0.0001(16) C30 0.0327(19) 0.033(2) 0.0197(16) 0.0048(14) 0.0048(14) 0.0048(15) C31 0.042(2) 0.038(2) 0.0222(17) 0.0081(15) 0.0023(15) 0.0067(16) C32 0.083(3) 0.052(3) 0.036(2) 0.018(2) 0.017(2) 0.029(2) C33 0.057(3) 0.060(3) 0.037(2) 0.018(2) 0.0129(19) -0.001(2) C34 0.068(3) 0.056(3) 0.032(2) 0.0109(19) -0.012(2) 0.000(2) C35 0.0349(19) 0.0310(19) 0.0246(17) 0.0026(15) 0.0056(15) 0.0050(15) C36 0.057(6) 0.048(4) 0.009(3) -0.001(3) -0.014(3) 0.013(3) C37 0.066(5) 0.037(4) 0.056(4) 0.003(3) -0.007(3) 0.007(4) C38 0.069(4) 0.057(7) 0.024(3) 0.004(4) 0.009(3) 0.004(5) C39 0.020(3) 0.059(6) 0.041(6) -0.015(3) -0.003(3) 0.002(3) C40 0.062(5) 0.067(4) 0.077(9) -0.015(4) -0.012(6) -0.024(4) C41 0.046(5) 0.20(2) 0.026(8) 0.013(6) 0.016(8) -0.024(13) C36A 0.057(6) 0.048(4) 0.009(3) -0.001(3) -0.014(3) 0.013(3) C37A 0.066(5) 0.037(4) 0.056(4) 0.003(3) -0.007(3) 0.007(4) C38A 0.069(4) 0.057(7) 0.024(3) 0.004(4) 0.009(3) 0.004(5) C39A 0.020(3) 0.059(6) 0.041(6) -0.015(3) -0.003(3) 0.002(3) C40A 0.062(5) 0.067(4) 0.077(9) -0.015(4) -0.012(6) -0.024(4) C41A 0.046(5) 0.20(2) 0.026(8) 0.013(6) 0.016(8) -0.024(13) C1S 0.088(5) 0.100(5) 0.035(3) -0.003(4) 0.019(3) 0.012(5) C2S 0.060(5) 0.089(5) 0.042(3) -0.001(3) 0.009(3) 0.001(4) C3S 0.051(4) 0.079(5) 0.052(3) -0.013(3) 0.011(3) 0.006(3) C1SA 0.088(5) 0.100(5) 0.035(3) -0.003(4) 0.019(3) 0.012(5) C2SA 0.060(5) 0.089(5) 0.042(3) -0.001(3) 0.009(3) 0.001(4) C3SA 0.051(4) 0.079(5) 0.052(3) -0.013(3) 0.011(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc O1 1.994(2) . ? Sc N3 2.000(3) . ? Sc O2 2.016(2) . ? Sc N1 2.277(2) . ? Sc N2 2.283(3) . ? Sc C39A 2.775(7) . ? O1 C5 1.321(4) . ? N1 C3 1.290(4) . ? N1 C2 1.469(4) . ? C1 C2 1.518(5) . ? C1 C18 1.522(5) . ? C1 C20 1.533(5) . ? C1 C19 1.543(5) . ? O2 C23 1.311(4) . ? N2 C21 1.291(4) . ? N2 C20 1.485(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N3 C36 1.477(3) . ? N3 C39 1.477(3) . ? N3 C36A 1.477(3) . ? N3 C39A 1.477(3) . ? C3 C4 1.437(4) . ? C3 H3A 0.9500 . ? C4 C17 1.404(4) . ? C4 C5 1.416(4) . ? C5 C6 1.418(4) . ? C6 C11 1.388(4) . ? C6 C7 1.536(4) . ? C7 C10 1.529(4) . ? C7 C8 1.534(4) . ? C7 C9 1.540(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.422(4) . ? C11 H11A 0.9500 . ? C12 C17 1.369(5) . ? C12 C13 1.530(4) . ? C13 C14 1.520(5) . ? C13 C15 1.534(5) . ? C13 C16 1.538(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.447(4) . ? C21 H21A 0.9500 . ? C22 C23 1.404(4) . ? C22 C35 1.409(4) . ? C23 C24 1.439(4) . ? C24 C29 1.388(4) . ? C24 C25 1.532(5) . ? C25 C28 1.529(5) . ? C25 C27 1.529(5) . ? C25 C26 1.544(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.401(5) . ? C29 H29A 0.9500 . ? C30 C35 1.379(4) . ? C30 C31 1.537(4) . ? C31 C32 1.525(5) . ? C31 C34 1.527(5) . ? C31 C33 1.531(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9500 . ? C36 C37 1.5201(10) . ? C36 C38 1.5203(10) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.5199(10) . ? C39 C40 1.5200(10) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C36A C37A 1.5200(10) . ? C36A C38A 1.5202(10) . ? C36A H36A 1.0000 . ? C37A H37D 0.9800 . ? C37A H37E 0.9800 . ? C37A H37F 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A C41A 1.5199(10) . ? C39A C40A 1.5200(10) . ? C39A H39A 1.0000 . ? C40A H40D 0.9800 . ? C40A H40E 0.9800 . ? C40A H40F 0.9800 . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? C1S C2S 1.518(7) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S C3S 1.448(7) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C3S 1.476(12) 3_576 ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C1SA C2SA 1.50(3) . ? C1SA H1S4 0.9800 . ? C1SA H1S5 0.9800 . ? C1SA H1S6 0.9800 . ? C2SA C3SA 1.448(7) . ? C2SA H2S3 0.9900 . ? C2SA H2S4 0.9900 . ? C3SA C3SA 1.37(4) 3_576 ? C3SA H3S3 0.9900 . ? C3SA H3S4 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sc N3 113.55(9) . . ? O1 Sc O2 97.23(9) . . ? N3 Sc O2 109.58(9) . . ? O1 Sc N1 81.10(9) . . ? N3 Sc N1 94.93(10) . . ? O2 Sc N1 153.61(9) . . ? O1 Sc N2 133.70(10) . . ? N3 Sc N2 110.44(10) . . ? O2 Sc N2 80.88(9) . . ? N1 Sc N2 81.51(9) . . ? O1 Sc C39A 138.6(2) . . ? N3 Sc C39A 30.94(16) . . ? O2 Sc C39A 86.0(2) . . ? N1 Sc C39A 112.8(2) . . ? N2 Sc C39A 87.6(2) . . ? C5 O1 Sc 140.93(19) . . ? C3 N1 C2 116.1(3) . . ? C3 N1 Sc 124.4(2) . . ? C2 N1 Sc 119.06(19) . . ? C2 C1 C18 111.5(3) . . ? C2 C1 C20 110.9(3) . . ? C18 C1 C20 111.5(3) . . ? C2 C1 C19 106.9(3) . . ? C18 C1 C19 110.1(3) . . ? C20 C1 C19 105.7(3) . . ? C23 O2 Sc 139.4(2) . . ? C21 N2 C20 114.1(3) . . ? C21 N2 Sc 123.1(2) . . ? C20 N2 Sc 122.8(2) . . ? N1 C2 C1 113.8(3) . . ? N1 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C36 N3 C39 93.4(5) . . ? C39 N3 C36A 114.0(6) . . ? C36 N3 C39A 119.6(5) . . ? C36A N3 C39A 139.3(6) . . ? C36 N3 Sc 135.5(3) . . ? C39 N3 Sc 131.1(4) . . ? C36A N3 Sc 113.7(4) . . ? C39A N3 Sc 104.9(4) . . ? N1 C3 C4 129.6(3) . . ? N1 C3 H3A 115.2 . . ? C4 C3 H3A 115.2 . . ? C17 C4 C5 120.9(3) . . ? C17 C4 C3 116.0(3) . . ? C5 C4 C3 123.1(3) . . ? O1 C5 C4 119.6(3) . . ? O1 C5 C6 122.3(3) . . ? C4 C5 C6 118.1(3) . . ? C11 C6 C5 118.4(3) . . ? C11 C6 C7 120.6(3) . . ? C5 C6 C7 121.0(3) . . ? C10 C7 C8 107.7(3) . . ? C10 C7 C6 109.4(3) . . ? C8 C7 C6 112.7(3) . . ? C10 C7 C9 110.0(3) . . ? C8 C7 C9 107.7(3) . . ? C6 C7 C9 109.4(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 C12 124.3(3) . . ? C6 C11 H11A 117.9 . . ? C12 C11 H11A 117.9 . . ? C17 C12 C11 116.1(3) . . ? C17 C12 C13 123.8(3) . . ? C11 C12 C13 120.0(3) . . ? C14 C13 C12 109.1(3) . . ? C14 C13 C15 109.2(3) . . ? C12 C13 C15 111.4(3) . . ? C14 C13 C16 109.0(3) . . ? C12 C13 C16 110.2(3) . . ? C15 C13 C16 107.9(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 C4 122.3(3) . . ? C12 C17 H17A 118.9 . . ? C4 C17 H17A 118.9 . . ? C1 C18 H18A 109.5 . . ? C1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 C19 H19A 109.5 . . ? C1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 C1 115.5(3) . . ? N2 C20 H20A 108.4 . . ? C1 C20 H20A 108.4 . . ? N2 C20 H20B 108.4 . . ? C1 C20 H20B 108.4 . . ? H20A C20 H20B 107.5 . . ? N2 C21 C22 129.7(3) . . ? N2 C21 H21A 115.1 . . ? C22 C21 H21A 115.1 . . ? C23 C22 C35 121.6(3) . . ? C23 C22 C21 122.6(3) . . ? C35 C22 C21 115.6(3) . . ? O2 C23 C22 120.4(3) . . ? O2 C23 C24 121.6(3) . . ? C22 C23 C24 118.0(3) . . ? C29 C24 C23 117.1(3) . . ? C29 C24 C25 121.8(3) . . ? C23 C24 C25 121.1(3) . . ? C28 C25 C27 109.9(3) . . ? C28 C25 C24 109.4(3) . . ? C27 C25 C24 110.9(3) . . ? C28 C25 C26 107.2(3) . . ? C27 C25 C26 107.0(3) . . ? C24 C25 C26 112.3(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 C30 125.6(3) . . ? C24 C29 H29A 117.2 . . ? C30 C29 H29A 117.2 . . ? C35 C30 C29 116.2(3) . . ? C35 C30 C31 123.0(3) . . ? C29 C30 C31 120.8(3) . . ? C32 C31 C34 108.4(3) . . ? C32 C31 C33 108.4(3) . . ? C34 C31 C33 109.4(3) . . ? C32 C31 C30 111.7(3) . . ? C34 C31 C30 109.9(3) . . ? C33 C31 C30 109.0(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 C22 121.3(3) . . ? C30 C35 H35A 119.3 . . ? C22 C35 H35A 119.3 . . ? N3 C36 C37 108.3(5) . . ? N3 C36 C38 112.5(6) . . ? C37 C36 C38 110.9(7) . . ? N3 C36 H36 108.3 . . ? C37 C36 H36 108.3 . . ? C38 C36 H36 108.3 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N3 C39 C41 114(2) . . ? N3 C39 C40 114.8(19) . . ? C41 C39 C40 120(3) . . ? N3 C39 H39 101.5 . . ? C41 C39 H39 101.5 . . ? C40 C39 H39 101.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C36A C37A 116.4(6) . . ? N3 C36A C38A 114.1(6) . . ? C37A C36A C38A 112.3(7) . . ? N3 C36A H36A 104.1 . . ? C37A C36A H36A 104.1 . . ? C38A C36A H36A 104.1 . . ? C36A C37A H37D 109.5 . . ? C36A C37A H37E 109.5 . . ? H37D C37A H37E 109.5 . . ? C36A C37A H37F 109.5 . . ? H37D C37A H37F 109.5 . . ? H37E C37A H37F 109.5 . . ? C36A C38A H38D 109.5 . . ? C36A C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C36A C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? N3 C39A C41A 107(2) . . ? N3 C39A C40A 111(2) . . ? C41A C39A C40A 107(3) . . ? C41A C39A Sc 120(2) . . ? C40A C39A Sc 131(2) . . ? N3 C39A H39A 110.5 . . ? C41A C39A H39A 110.5 . . ? C40A C39A H39A 110.5 . . ? Sc C39A H39A 66.6 . . ? C39A C40A H40D 109.5 . . ? C39A C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? C39A C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? C39A C41A H41D 109.5 . . ? C39A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C39A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C3S C2S C1S 119.3(7) . . ? C3S C2S H2S1 107.5 . . ? C1S C2S H2S1 107.5 . . ? C3S C2S H2S2 107.5 . . ? C1S C2S H2S2 107.5 . . ? H2S1 C2S H2S2 107.0 . . ? C2S C3S C3S 123.3(8) . 3_576 ? C2S C3S H3S1 106.5 . . ? C3S C3S H3S1 106.5 3_576 . ? C2S C3S H3S2 106.5 . . ? C3S C3S H3S2 106.5 3_576 . ? H3S1 C3S H3S2 106.5 . . ? C2SA C1SA H1S4 109.5 . . ? C2SA C1SA H1S5 109.5 . . ? H1S4 C1SA H1S5 109.5 . . ? C2SA C1SA H1S6 109.5 . . ? H1S4 C1SA H1S6 109.5 . . ? H1S5 C1SA H1S6 109.5 . . ? C3SA C2SA C1SA 155(2) . . ? C3SA C2SA H2S3 97.7 . . ? C1SA C2SA H2S3 97.7 . . ? C3SA C2SA H2S4 97.7 . . ? C1SA C2SA H2S4 97.7 . . ? H2S3 C2SA H2S4 103.7 . . ? C3SA C3SA C2SA 134(3) 3_576 . ? C3SA C3SA H3S3 103.6 3_576 . ? C2SA C3SA H3S3 103.6 . . ? C3SA C3SA H3S4 103.6 3_576 . ? C2SA C3SA H3S4 103.6 . . ? H3S3 C3SA H3S4 105.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Sc O1 C5 77.4(3) . . . . ? O2 Sc O1 C5 -167.5(3) . . . . ? N1 Sc O1 C5 -14.1(3) . . . . ? N2 Sc O1 C5 -83.2(3) . . . . ? C39A Sc O1 C5 100.4(4) . . . . ? O1 Sc N1 C3 8.3(3) . . . . ? N3 Sc N1 C3 -104.8(3) . . . . ? O2 Sc N1 C3 96.6(3) . . . . ? N2 Sc N1 C3 145.2(3) . . . . ? C39A Sc N1 C3 -131.0(3) . . . . ? O1 Sc N1 C2 -179.8(2) . . . . ? N3 Sc N1 C2 67.1(2) . . . . ? O2 Sc N1 C2 -91.5(3) . . . . ? N2 Sc N1 C2 -42.9(2) . . . . ? C39A Sc N1 C2 40.9(3) . . . . ? O1 Sc O2 C23 112.5(3) . . . . ? N3 Sc O2 C23 -129.3(3) . . . . ? N1 Sc O2 C23 27.9(4) . . . . ? N2 Sc O2 C23 -20.7(3) . . . . ? C39A Sc O2 C23 -109.0(4) . . . . ? O1 Sc N2 C21 -74.2(3) . . . . ? N3 Sc N2 C21 124.7(3) . . . . ? O2 Sc N2 C21 17.1(3) . . . . ? N1 Sc N2 C21 -143.2(3) . . . . ? C39A Sc N2 C21 103.4(3) . . . . ? O1 Sc N2 C20 106.7(3) . . . . ? N3 Sc N2 C20 -54.3(3) . . . . ? O2 Sc N2 C20 -161.9(3) . . . . ? N1 Sc N2 C20 37.8(3) . . . . ? C39A Sc N2 C20 -75.7(3) . . . . ? C3 N1 C2 C1 -118.9(3) . . . . ? Sc N1 C2 C1 68.5(3) . . . . ? C18 C1 C2 N1 52.5(4) . . . . ? C20 C1 C2 N1 -72.4(4) . . . . ? C19 C1 C2 N1 172.9(3) . . . . ? O1 Sc N3 C36 -28.9(4) . . . . ? O2 Sc N3 C36 -136.4(4) . . . . ? N1 Sc N3 C36 53.5(4) . . . . ? N2 Sc N3 C36 136.3(4) . . . . ? C39A Sc N3 C36 -178.8(7) . . . . ? O1 Sc N3 C39 149.6(6) . . . . ? O2 Sc N3 C39 42.1(6) . . . . ? N1 Sc N3 C39 -127.9(6) . . . . ? N2 Sc N3 C39 -45.2(6) . . . . ? C39A Sc N3 C39 -0.2(10) . . . . ? O1 Sc N3 C36A -16.8(4) . . . . ? O2 Sc N3 C36A -124.3(3) . . . . ? N1 Sc N3 C36A 65.6(4) . . . . ? N2 Sc N3 C36A 148.4(3) . . . . ? C39A Sc N3 C36A -166.7(7) . . . . ? O1 Sc N3 C39A 149.9(5) . . . . ? O2 Sc N3 C39A 42.4(5) . . . . ? N1 Sc N3 C39A -127.7(5) . . . . ? N2 Sc N3 C39A -44.9(5) . . . . ? C2 N1 C3 C4 -177.0(3) . . . . ? Sc N1 C3 C4 -4.9(5) . . . . ? N1 C3 C4 C17 177.6(3) . . . . ? N1 C3 C4 C5 -0.1(6) . . . . ? Sc O1 C5 C4 13.5(5) . . . . ? Sc O1 C5 C6 -166.3(2) . . . . ? C17 C4 C5 O1 -179.9(3) . . . . ? C3 C4 C5 O1 -2.4(5) . . . . ? C17 C4 C5 C6 -0.1(5) . . . . ? C3 C4 C5 C6 177.4(3) . . . . ? O1 C5 C6 C11 179.4(3) . . . . ? C4 C5 C6 C11 -0.4(4) . . . . ? O1 C5 C6 C7 -1.3(5) . . . . ? C4 C5 C6 C7 178.9(3) . . . . ? C11 C6 C7 C10 117.3(3) . . . . ? C5 C6 C7 C10 -62.1(4) . . . . ? C11 C6 C7 C8 -2.4(4) . . . . ? C5 C6 C7 C8 178.2(3) . . . . ? C11 C6 C7 C9 -122.2(3) . . . . ? C5 C6 C7 C9 58.5(4) . . . . ? C5 C6 C11 C12 0.7(5) . . . . ? C7 C6 C11 C12 -178.7(3) . . . . ? C6 C11 C12 C17 -0.3(5) . . . . ? C6 C11 C12 C13 -177.4(3) . . . . ? C17 C12 C13 C14 -107.7(4) . . . . ? C11 C12 C13 C14 69.2(4) . . . . ? C17 C12 C13 C15 12.8(5) . . . . ? C11 C12 C13 C15 -170.2(3) . . . . ? C17 C12 C13 C16 132.6(4) . . . . ? C11 C12 C13 C16 -50.5(4) . . . . ? C11 C12 C17 C4 -0.3(5) . . . . ? C13 C12 C17 C4 176.7(3) . . . . ? C5 C4 C17 C12 0.5(5) . . . . ? C3 C4 C17 C12 -177.2(3) . . . . ? C21 N2 C20 C1 125.3(3) . . . . ? Sc N2 C20 C1 -55.6(4) . . . . ? C2 C1 C20 N2 64.7(4) . . . . ? C18 C1 C20 N2 -60.1(4) . . . . ? C19 C1 C20 N2 -179.8(3) . . . . ? C20 N2 C21 C22 169.4(4) . . . . ? Sc N2 C21 C22 -9.7(5) . . . . ? N2 C21 C22 C23 -6.6(6) . . . . ? N2 C21 C22 C35 178.0(4) . . . . ? Sc O2 C23 C22 12.4(5) . . . . ? Sc O2 C23 C24 -168.9(2) . . . . ? C35 C22 C23 O2 -177.4(3) . . . . ? C21 C22 C23 O2 7.5(5) . . . . ? C35 C22 C23 C24 3.8(5) . . . . ? C21 C22 C23 C24 -171.2(3) . . . . ? O2 C23 C24 C29 177.5(3) . . . . ? C22 C23 C24 C29 -3.8(4) . . . . ? O2 C23 C24 C25 -4.4(5) . . . . ? C22 C23 C24 C25 174.3(3) . . . . ? C29 C24 C25 C28 116.0(3) . . . . ? C23 C24 C25 C28 -62.0(4) . . . . ? C29 C24 C25 C27 -122.6(3) . . . . ? C23 C24 C25 C27 59.4(4) . . . . ? C29 C24 C25 C26 -2.9(5) . . . . ? C23 C24 C25 C26 179.1(3) . . . . ? C23 C24 C29 C30 0.5(5) . . . . ? C25 C24 C29 C30 -177.6(3) . . . . ? C24 C29 C30 C35 2.8(5) . . . . ? C24 C29 C30 C31 -180.0(3) . . . . ? C35 C30 C31 C32 -13.1(5) . . . . ? C29 C30 C31 C32 169.9(3) . . . . ? C35 C30 C31 C34 -133.5(4) . . . . ? C29 C30 C31 C34 49.5(4) . . . . ? C35 C30 C31 C33 106.6(4) . . . . ? C29 C30 C31 C33 -70.4(4) . . . . ? C29 C30 C35 C22 -2.8(5) . . . . ? C31 C30 C35 C22 -180.0(3) . . . . ? C23 C22 C35 C30 -0.4(5) . . . . ? C21 C22 C35 C30 175.0(3) . . . . ? C39 N3 C36 C37 -138.3(7) . . . . ? C36A N3 C36 C37 12.4(10) . . . . ? C39A N3 C36 C37 -138.0(8) . . . . ? Sc N3 C36 C37 40.6(8) . . . . ? C39 N3 C36 C38 98.8(8) . . . . ? C36A N3 C36 C38 -110.5(16) . . . . ? C39A N3 C36 C38 99.0(9) . . . . ? Sc N3 C36 C38 -82.3(8) . . . . ? C36 N3 C39 C41 123.3(11) . . . . ? C36A N3 C39 C41 110.8(11) . . . . ? C39A N3 C39 C41 -56(2) . . . . ? Sc N3 C39 C41 -55.6(12) . . . . ? C36 N3 C39 C40 -93.2(16) . . . . ? C36A N3 C39 C40 -105.8(16) . . . . ? C39A N3 C39 C40 87(2) . . . . ? Sc N3 C39 C40 87.8(16) . . . . ? C36 N3 C36A C37A -99.3(15) . . . . ? C39 N3 C36A C37A -66.9(9) . . . . ? C39A N3 C36A C37A -58.2(12) . . . . ? Sc N3 C36A C37A 101.9(7) . . . . ? C36 N3 C36A C38A 34.0(12) . . . . ? C39 N3 C36A C38A 66.3(9) . . . . ? C39A N3 C36A C38A 75.1(12) . . . . ? Sc N3 C36A C38A -124.8(7) . . . . ? C36 N3 C39A C41A 63.7(17) . . . . ? C39 N3 C39A C41A 64(2) . . . . ? C36A N3 C39A C41A 45.8(19) . . . . ? Sc N3 C39A C41A -115.3(16) . . . . ? C36 N3 C39A C40A -53.1(14) . . . . ? C39 N3 C39A C40A -53(2) . . . . ? C36A N3 C39A C40A -70.9(16) . . . . ? Sc N3 C39A C40A 127.9(12) . . . . ? C36 N3 C39A Sc 179.0(6) . . . . ? C39 N3 C39A Sc 179.6(17) . . . . ? C36A N3 C39A Sc 161.2(9) . . . . ? O1 Sc C39A N3 -44.1(7) . . . . ? O2 Sc C39A N3 -140.5(5) . . . . ? N1 Sc C39A N3 58.7(5) . . . . ? N2 Sc C39A N3 138.5(5) . . . . ? O1 Sc C39A C41A 39.8(11) . . . . ? N3 Sc C39A C41A 83.9(10) . . . . ? O2 Sc C39A C41A -56.6(10) . . . . ? N1 Sc C39A C41A 142.6(9) . . . . ? N2 Sc C39A C41A -137.6(10) . . . . ? O1 Sc C39A C40A -122(2) . . . . ? N3 Sc C39A C40A -78(2) . . . . ? O2 Sc C39A C40A 142(2) . . . . ? N1 Sc C39A C40A -19(2) . . . . ? N2 Sc C39A C40A 61(2) . . . . ? C1S C2S C3S C3S 53.0(10) . . . 3_576 ? C1SA C2SA C3SA C3SA 67(7) . . . 3_576 ? # # End of Crystallographic Information File for Compound 6 # # # CIF-file generated for meed_g002_173 / compound 9 #============================================================================== data_meed_g002_173 # compound 9 _database_code_depnum_ccdc_archive 'CCDC 284497' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; [N,N'-bis(3,5-di-tert.-butylsalicylidene)-trans-1,2-cyclohexylendiamino] [bis(dimethylsilyl)amido] scandium(III) (Salcyc)Sc[N(SiHMe2)2] ; _chemical_name_common (R,R)-(Salcyc)Sc[N(SiHMe2)2] _chemical_melting_point ? _chemical_formula_moiety 'C40 H66 N3 O2 Sc Si2' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C40 H66 N3 O2 Sc Si2' _chemical_formula_iupac ? _chemical_formula_weight 722.10 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,-z _cell_length_a 14.5528(1) _cell_length_b 12.6006(1) _cell_length_c 26.9905(2) _cell_angle_alpha 90 _cell_angle_beta 103.7265(3) _cell_angle_gamma 90 _cell_volume 4808.00(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 10242 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 26.37 _cell_special_details ; ? ; _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.640 _exptl_crystal_size_mid 0.440 _exptl_crystal_size_min 0.280 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.998 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.233 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Sortav (R.H. Blessing, 1995)' _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 0.936 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD (Nonius)' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 70269 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.45 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 18030 # number of observed reflections (> n sig(I)) _reflns_number_gt 14745 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_data_reduction 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_structure_solution 'SIR-92 (C. Giacovazzo, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. Electron density synthesis with coefficients Fo-Fc Highest peak 1.17 at 0.2077 0.7853 0.2310 [ 0.96 A from SI4 ] Deepest hole -0.70 at 0.3182 0.7728 0.2156 [ 0.75 A from SI3 ] All hydrogen atoms were calculated in idealized geometry and refined using a riding group model. An initial structure solution using the centrosymmetric space group P21/c was not successfull (high R values, incorrect geometry of the bridging cyclohexane unit). A disordering in the t-butyl group C69-C72 could not be resolved. A Total Potential Solvent Accessible Area Vol of 804.1 Ang^3^ was found. Due to severe disorder no solvent molecule could be located. Thus the BYPASS method (as implemented as the 'SQUEEZE option' in PLATON) was applied to account for the disordered solvent contribution to the structure factor in the final refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+1.7868P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(3) _chemical_absolute_configuration rm _refine_ls_number_reflns 18030 _refine_ls_number_parameters 865 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.170 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.056 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Sc1 Sc Uani 0.13352(4) 0.35260(5) 0.60816(2) 1.000 0.0266(2) . . Si1 Si Uani 0.13028(7) 0.26361(11) 0.71654(4) 1.000 0.0424(3) . . Si2 Si Uani 0.32376(8) 0.27464(12) 0.69788(4) 1.000 0.0520(4) . . O1 O Uani 0.03313(17) 0.4558(2) 0.61330(9) 1.000 0.0328(8) . . O2 O Uani 0.21892(17) 0.4444(2) 0.58009(9) 1.000 0.0331(8) . . N1 N Uani 0.00671(19) 0.2492(2) 0.57670(10) 1.000 0.0294(8) . . N2 N Uani 0.17168(19) 0.2412(2) 0.55218(10) 1.000 0.0294(8) . . N3 N Uani 0.2042(2) 0.2911(3) 0.67687(11) 1.000 0.0357(10) . . C1 C Uani 0.0228(2) 0.1528(3) 0.54781(13) 1.000 0.0304(10) . . C2 C Uani 0.1292(2) 0.1357(2) 0.55699(13) 1.000 0.0299(10) . . C3 C Uani 0.1526(3) 0.0452(3) 0.52505(15) 1.000 0.0372(11) . . C4 C Uani 0.1042(3) -0.0561(3) 0.53738(16) 1.000 0.0444(13) . . C5 C Uani -0.0014(3) -0.0406(3) 0.52843(15) 1.000 0.0427(11) . . C6 C Uani -0.0259(3) 0.0510(3) 0.55991(15) 1.000 0.0385(11) . . C7 C Uani 0.2186(2) 0.2591(3) 0.51840(13) 1.000 0.0334(10) . . C8 C Uani 0.2595(2) 0.3585(3) 0.50923(14) 1.000 0.0340(11) . . C9 C Uani 0.2584(2) 0.4490(3) 0.54052(13) 1.000 0.0295(10) . . C10 C Uani 0.3005(2) 0.5456(3) 0.52867(13) 1.000 0.0305(11) . . C11 C Uani 0.3383(3) 0.5452(3) 0.48677(14) 1.000 0.0379(12) . . C12 C Uani 0.3391(3) 0.4570(4) 0.45442(14) 1.000 0.0384(12) . . C13 C Uani 0.3014(3) 0.3657(3) 0.46743(14) 1.000 0.0384(12) . . C14 C Uani 0.3816(3) 0.4678(4) 0.40837(16) 1.000 0.0481(16) . . C15 C Uani 0.4852(4) 0.5102(4) 0.4247(2) 1.000 0.074(2) . . C16 C Uani 0.3902(4) 0.3624(4) 0.3837(2) 1.000 0.0675(17) . . C17 C Uani 0.3225(4) 0.5447(5) 0.3706(2) 1.000 0.082(2) . . C18 C Uani 0.3028(3) 0.6439(3) 0.56270(15) 1.000 0.0352(11) . . C19 C Uani 0.3488(3) 0.7398(3) 0.54367(17) 1.000 0.0492(16) . . C20 C Uani 0.3610(3) 0.6192(4) 0.61672(16) 1.000 0.0509(14) . . C21 C Uani 0.2029(3) 0.6760(3) 0.56561(17) 1.000 0.0441(14) . . C22 C Uani -0.0794(2) 0.2711(3) 0.57776(12) 1.000 0.0315(10) . . C23 C Uani -0.1127(2) 0.3657(3) 0.59761(13) 1.000 0.0299(10) . . C24 C Uani -0.0569(2) 0.4543(3) 0.61470(13) 1.000 0.0318(11) . . C25 C Uani -0.0994(3) 0.5452(3) 0.63392(13) 1.000 0.0321(11) . . C26 C Uani -0.1948(3) 0.5399(3) 0.63061(14) 1.000 0.0376(12) . . C27 C Uani -0.2545(3) 0.4542(3) 0.61076(14) 1.000 0.0380(12) . . C28 C Uani -0.2118(2) 0.3683(3) 0.59608(14) 1.000 0.0353(11) . . C29 C Uani -0.3612(3) 0.4620(4) 0.60671(16) 1.000 0.0447(14) . . C30 C Uani -0.3996(3) 0.5539(5) 0.56881(19) 1.000 0.0609(18) . . C31 C Uani -0.4134(3) 0.3592(5) 0.5863(3) 1.000 0.082(2) . . C32 C Uani -0.3795(3) 0.4859(5) 0.65874(18) 1.000 0.0695(19) . . C33 C Uani -0.0408(3) 0.6431(3) 0.65405(16) 1.000 0.0416(12) . . C34 C Uani -0.0090(3) 0.6977(4) 0.61078(17) 1.000 0.0504(14) . . C35 C Uani 0.0460(3) 0.6115(4) 0.69692(16) 1.000 0.0542(16) . . C36 C Uani -0.0986(3) 0.7237(4) 0.6768(2) 1.000 0.0606(17) . . C37 C Uani 0.3819(4) 0.2393(8) 0.6461(2) 1.000 0.125(4) . . C38 C Uani 0.3848(4) 0.3974(7) 0.7294(2) 1.000 0.095(3) . . C39 C Uani 0.1597(4) 0.3390(5) 0.77850(16) 1.000 0.0701(18) . . C40 C Uani 0.1219(4) 0.1188(5) 0.7298(2) 1.000 0.074(2) . . Sc2 Sc Uani 0.12888(4) 0.68244(5) 0.10858(2) 1.000 0.0272(2) . . Si3 Si Uani 0.32462(9) 0.76692(14) 0.18883(6) 1.000 0.0720(5) . . Si4 Si Uani 0.14019(10) 0.77626(12) 0.21963(4) 1.000 0.0558(4) . . O3 O Uani 0.20201(18) 0.5851(2) 0.07485(9) 1.000 0.0366(8) . . O4 O Uani 0.03088(17) 0.5847(2) 0.12147(9) 1.000 0.0331(8) . . N4 N Uani 0.14094(19) 0.7859(2) 0.04165(10) 1.000 0.0304(8) . . N5 N Uani 0.00656(19) 0.7923(2) 0.09178(11) 1.000 0.0294(8) . . N6 N Uani 0.2057(2) 0.7474(3) 0.17523(11) 1.000 0.0401(10) . . C41 C Uani 0.0793(2) 0.8819(2) 0.03219(13) 1.000 0.0315(10) . . C42 C Uani 0.0385(2) 0.8983(2) 0.07835(13) 1.000 0.0313(10) . . C43 C Uani -0.0321(3) 0.9891(3) 0.07096(15) 1.000 0.0384(11) . . C44 C Uani 0.0166(3) 1.0910(3) 0.05932(15) 1.000 0.0433(11) . . C45 C Uani 0.0596(3) 1.0762(3) 0.01347(16) 1.000 0.0473(14) . . C46 C Uani 0.1292(3) 0.9834(3) 0.02093(16) 1.000 0.0413(12) . . C47 C Uani -0.0796(2) 0.7742(3) 0.09202(13) 1.000 0.0340(11) . . C48 C Uani -0.1180(2) 0.6735(3) 0.10518(13) 1.000 0.0318(11) . . C49 C Uani -0.0593(2) 0.5838(3) 0.12196(12) 1.000 0.0287(10) . . C50 C Uani -0.1011(3) 0.4931(3) 0.13846(13) 1.000 0.0354(11) . . C51 C Uani -0.1988(3) 0.4933(3) 0.13308(14) 1.000 0.0395(12) . . C52 C Uani -0.2578(3) 0.5791(4) 0.11421(14) 1.000 0.0394(14) . . C53 C Uani -0.2151(3) 0.6697(4) 0.10110(14) 1.000 0.0376(11) . . C54 C Uani -0.3662(3) 0.5672(4) 0.10695(17) 1.000 0.0506(16) . . C55 C Uani -0.3871(3) 0.5375(7) 0.1578(2) 1.000 0.100(3) . . C56 C Uani -0.4168(4) 0.6679(6) 0.0878(3) 1.000 0.103(3) . . C57 C Uani -0.4010(4) 0.4805(6) 0.0698(2) 1.000 0.087(3) . . C58 C Uani -0.0398(3) 0.3974(3) 0.16161(14) 1.000 0.0377(12) . . C59 C Uani 0.0045(4) 0.3484(4) 0.12143(18) 1.000 0.0608(18) . . C60 C Uani 0.0373(3) 0.4322(4) 0.20818(16) 1.000 0.0541(16) . . C61 C Uani -0.0977(4) 0.3088(5) 0.1803(3) 1.000 0.089(2) . . C62 C Uani 0.1877(2) 0.7639(3) 0.00789(13) 1.000 0.0334(11) . . C63 C Uani 0.2420(2) 0.6664(3) 0.00443(13) 1.000 0.0311(10) . . C64 C Uani 0.2440(2) 0.5794(3) 0.03664(13) 1.000 0.0323(11) . . C65 C Uani 0.2912(2) 0.4859(3) 0.02689(14) 1.000 0.0339(11) . . C66 C Uani 0.3320(3) 0.4861(3) -0.01491(15) 1.000 0.0363(11) . . C67 C Uani 0.3320(3) 0.5732(3) -0.04706(15) 1.000 0.0401(12) . . C68 C Uani 0.2853(3) 0.6629(3) -0.03663(14) 1.000 0.0379(11) . . C69 C Uani 0.3773(3) 0.5652(4) -0.09348(17) 1.000 0.0460(16) . . C70 C Uani 0.3350(9) 0.4828(8) -0.1255(3) 1.000 0.228(7) . . C71 C Uani 0.3729(7) 0.6702(8) -0.1212(3) 1.000 0.162(5) . . C72 C Uani 0.4809(4) 0.5300(9) -0.0743(3) 1.000 0.126(4) . . C73 C Uani 0.2940(3) 0.3867(3) 0.06046(15) 1.000 0.0364(11) . . C74 C Uani 0.1929(3) 0.3468(4) 0.05519(17) 1.000 0.0496(14) . . C75 C Uani 0.3399(3) 0.4112(4) 0.11593(15) 1.000 0.0469(12) . . C76 C Uani 0.3496(3) 0.2959(4) 0.04337(19) 1.000 0.0559(17) . . C77 C Uani 0.1286(4) 0.9197(5) 0.2298(2) 1.000 0.0739(19) . . C78 C Uani 0.1834(4) 0.7104(6) 0.2824(2) 1.000 0.084(2) . . C79 C Uani 0.3934(4) 0.6521(6) 0.2220(2) 1.000 0.094(2) . . C80 C Uani 0.3687(4) 0.7997(6) 0.1362(3) 1.000 0.101(3) . . H1 H Uiso -0.00200 0.16820 0.51070 1.000 0.0370 calc R H2 H Uiso 0.15200 0.11380 0.59350 1.000 0.0360 calc R H3A H Uiso 0.22190 0.03450 0.53260 1.000 0.0440 calc R H3B H Uiso 0.13020 0.06230 0.48840 1.000 0.0440 calc R H4A H Uiso 0.11730 -0.11490 0.51570 1.000 0.0530 calc R H4B H Uiso 0.13060 -0.07590 0.57340 1.000 0.0530 calc R H5A H Uiso -0.03040 -0.10670 0.53750 1.000 0.0510 calc R H5B H Uiso -0.02830 -0.02630 0.49180 1.000 0.0510 calc R H6A H Uiso -0.00450 0.03440 0.59670 1.000 0.0460 calc R H6B H Uiso -0.09530 0.06150 0.55180 1.000 0.0460 calc R H7 H Uiso 0.22690 0.20100 0.49750 1.000 0.0400 calc R H11 H Uiso 0.36610 0.60920 0.47880 1.000 0.0450 calc R H13 H Uiso 0.30350 0.30400 0.44750 1.000 0.0460 calc R H15A H Uiso 0.51070 0.51860 0.39440 1.000 0.1100 calc R H15B H Uiso 0.52430 0.45960 0.44820 1.000 0.1100 calc R H15C H Uiso 0.48570 0.57900 0.44170 1.000 0.1100 calc R H16A H Uiso 0.32690 0.33370 0.36920 1.000 0.1010 calc R H16B H Uiso 0.42550 0.31290 0.40930 1.000 0.1010 calc R H16C H Uiso 0.42380 0.37170 0.35650 1.000 0.1010 calc R H17A H Uiso 0.34980 0.55180 0.34080 1.000 0.1230 calc R H17B H Uiso 0.32190 0.61420 0.38680 1.000 0.1230 calc R H17C H Uiso 0.25770 0.51780 0.35960 1.000 0.1230 calc R H19A H Uiso 0.34800 0.80020 0.56640 1.000 0.0740 calc R H19B H Uiso 0.31350 0.75800 0.50910 1.000 0.0740 calc R H19C H Uiso 0.41430 0.72260 0.54330 1.000 0.0740 calc R H20A H Uiso 0.42610 0.60170 0.61550 1.000 0.0760 calc R H20B H Uiso 0.33280 0.55880 0.63060 1.000 0.0760 calc R H20C H Uiso 0.36130 0.68140 0.63860 1.000 0.0760 calc R H21A H Uiso 0.20640 0.73640 0.58880 1.000 0.0660 calc R H21B H Uiso 0.17220 0.61610 0.57830 1.000 0.0660 calc R H21C H Uiso 0.16620 0.69600 0.53160 1.000 0.0660 calc R H22 H Uiso -0.12570 0.21910 0.56400 1.000 0.0380 calc R H26 H Uiso -0.22310 0.59920 0.64280 1.000 0.0450 calc R H28 H Uiso -0.24900 0.30730 0.58430 1.000 0.0420 calc R H30A H Uiso -0.37750 0.54410 0.53750 1.000 0.0920 calc R H30B H Uiso -0.37640 0.62190 0.58450 1.000 0.0920 calc R H30C H Uiso -0.46890 0.55340 0.56060 1.000 0.0920 calc R H31A H Uiso -0.39460 0.30250 0.61160 1.000 0.1230 calc R H31B H Uiso -0.39710 0.33880 0.55440 1.000 0.1230 calc R H31C H Uiso -0.48180 0.37070 0.58000 1.000 0.1230 calc R H32A H Uiso -0.44750 0.49540 0.65540 1.000 0.1040 calc R H32B H Uiso -0.34600 0.55100 0.67240 1.000 0.1040 calc R H32C H Uiso -0.35660 0.42670 0.68200 1.000 0.1040 calc R H34A H Uiso 0.02020 0.64550 0.59240 1.000 0.0760 calc R H34B H Uiso 0.03700 0.75320 0.62470 1.000 0.0760 calc R H34C H Uiso -0.06390 0.72960 0.58730 1.000 0.0760 calc R H35A H Uiso 0.08900 0.56780 0.68260 1.000 0.0810 calc R H35B H Uiso 0.02480 0.57110 0.72320 1.000 0.0810 calc R H35C H Uiso 0.07910 0.67570 0.71210 1.000 0.0810 calc R H36A H Uiso -0.05750 0.78210 0.69260 1.000 0.0910 calc R H36B H Uiso -0.12520 0.68870 0.70270 1.000 0.0910 calc R H36C H Uiso -0.15010 0.75170 0.64970 1.000 0.0910 calc R H37A H Uiso 0.36250 0.16770 0.63370 1.000 0.1880 calc R H37B H Uiso 0.45070 0.24120 0.65910 1.000 0.1880 calc R H37C H Uiso 0.36320 0.29010 0.61800 1.000 0.1880 calc R H38A H Uiso 0.37740 0.45490 0.70430 1.000 0.1420 calc R H38B H Uiso 0.45220 0.38260 0.74280 1.000 0.1420 calc R H38C H Uiso 0.35650 0.41870 0.75740 1.000 0.1420 calc R H39A H Uiso 0.22410 0.32120 0.79730 1.000 0.1050 calc R H39B H Uiso 0.11490 0.31970 0.79900 1.000 0.1050 calc R H39C H Uiso 0.15550 0.41540 0.77150 1.000 0.1050 calc R H40A H Uiso 0.09520 0.08130 0.69780 1.000 0.1120 calc R H40B H Uiso 0.08100 0.10840 0.75350 1.000 0.1120 calc R H40C H Uiso 0.18520 0.09090 0.74500 1.000 0.1120 calc R H81 H Uiso 0.03640 0.29730 0.68970 1.000 0.0510 calc R H82 H Uiso 0.34070 0.18950 0.73510 1.000 0.0620 calc R H41 H Uiso 0.02570 0.86710 0.00220 1.000 0.0380 calc R H42 H Uiso 0.09250 0.91940 0.10710 1.000 0.0380 calc R H43A H Uiso -0.05550 0.99880 0.10220 1.000 0.0460 calc R H43B H Uiso -0.08690 0.97270 0.04240 1.000 0.0460 calc R H44A H Uiso -0.03010 1.14950 0.05230 1.000 0.0520 calc R H44B H Uiso 0.06700 1.11090 0.08950 1.000 0.0520 calc R H45A H Uiso 0.09290 1.14210 0.00790 1.000 0.0570 calc R H45B H Uiso 0.00840 1.06340 -0.01740 1.000 0.0570 calc R H46A H Uiso 0.18390 0.99870 0.04970 1.000 0.0490 calc R H46B H Uiso 0.15290 0.97340 -0.01020 1.000 0.0490 calc R H47 H Uiso -0.12280 0.83140 0.08280 1.000 0.0410 calc R H51 H Uiso -0.22710 0.43120 0.14280 1.000 0.0470 calc R H53 H Uiso -0.25270 0.73030 0.08910 1.000 0.0450 calc R H55A H Uiso -0.45540 0.52800 0.15340 1.000 0.1490 calc R H55B H Uiso -0.36500 0.59420 0.18270 1.000 0.1490 calc R H55C H Uiso -0.35450 0.47120 0.17020 1.000 0.1490 calc R H56A H Uiso -0.39630 0.69260 0.05770 1.000 0.1540 calc R H56B H Uiso -0.40210 0.72210 0.11460 1.000 0.1540 calc R H56C H Uiso -0.48520 0.65500 0.07860 1.000 0.1540 calc R H57A H Uiso -0.38560 0.49720 0.03720 1.000 0.1310 calc R H57B H Uiso -0.46970 0.47360 0.06460 1.000 0.1310 calc R H57C H Uiso -0.37050 0.41360 0.08310 1.000 0.1310 calc R H59A H Uiso 0.04620 0.28990 0.13660 1.000 0.0910 calc R H59B H Uiso 0.04130 0.40230 0.10850 1.000 0.0910 calc R H59C H Uiso -0.04550 0.32120 0.09330 1.000 0.0910 calc R H60A H Uiso 0.08030 0.37270 0.22000 1.000 0.0810 calc R H60B H Uiso 0.00790 0.45440 0.23560 1.000 0.0810 calc R H60C H Uiso 0.07300 0.49170 0.19870 1.000 0.0810 calc R H61A H Uiso -0.14610 0.28180 0.15140 1.000 0.1340 calc R H61B H Uiso -0.12820 0.33800 0.20610 1.000 0.1340 calc R H61C H Uiso -0.05530 0.25080 0.19530 1.000 0.1340 calc R H62 H Uiso 0.18710 0.81610 -0.01750 1.000 0.0400 calc R H66 H Uiso 0.36180 0.42270 -0.02210 1.000 0.0440 calc R H68 H Uiso 0.28250 0.72360 -0.05780 1.000 0.0450 calc R H70A H Uiso 0.26720 0.49710 -0.13770 1.000 0.3420 calc R H70B H Uiso 0.34390 0.41580 -0.10650 1.000 0.3420 calc R H70C H Uiso 0.36410 0.47780 -0.15460 1.000 0.3420 calc R H71A H Uiso 0.40550 0.66360 -0.14900 1.000 0.2420 calc R H71B H Uiso 0.40370 0.72520 -0.09730 1.000 0.2420 calc R H71C H Uiso 0.30670 0.68970 -0.13540 1.000 0.2420 calc R H72A H Uiso 0.48290 0.45620 -0.06260 1.000 0.1890 calc R H72B H Uiso 0.51240 0.57570 -0.04600 1.000 0.1890 calc R H72C H Uiso 0.51340 0.53560 -0.10210 1.000 0.1890 calc R H74A H Uiso 0.19380 0.28360 0.07650 1.000 0.0740 calc R H74B H Uiso 0.16490 0.32890 0.01950 1.000 0.0740 calc R H74C H Uiso 0.15510 0.40250 0.06630 1.000 0.0740 calc R H75A H Uiso 0.33660 0.34840 0.13690 1.000 0.0710 calc R H75B H Uiso 0.30650 0.47030 0.12750 1.000 0.0710 calc R H75C H Uiso 0.40630 0.43080 0.11920 1.000 0.0710 calc R H76A H Uiso 0.41470 0.31890 0.04540 1.000 0.0840 calc R H76B H Uiso 0.31950 0.27630 0.00810 1.000 0.0840 calc R H76C H Uiso 0.35010 0.23430 0.06560 1.000 0.0840 calc R H77A H Uiso 0.19150 0.95090 0.24230 1.000 0.1100 calc R H77B H Uiso 0.09100 0.93110 0.25500 1.000 0.1100 calc R H77C H Uiso 0.09700 0.95340 0.19750 1.000 0.1100 calc R H78A H Uiso 0.19440 0.63500 0.27710 1.000 0.1260 calc R H78B H Uiso 0.13590 0.71780 0.30250 1.000 0.1260 calc R H78C H Uiso 0.24260 0.74380 0.30060 1.000 0.1260 calc R H79A H Uiso 0.37930 0.64250 0.25550 1.000 0.1420 calc R H79B H Uiso 0.46120 0.66570 0.22650 1.000 0.1420 calc R H79C H Uiso 0.37590 0.58780 0.20160 1.000 0.1420 calc R H80A H Uiso 0.35500 0.74200 0.11110 1.000 0.1510 calc R H80B H Uiso 0.43720 0.81020 0.14710 1.000 0.1510 calc R H80C H Uiso 0.33860 0.86520 0.12070 1.000 0.1510 calc R H83 H Uiso 0.34460 0.85620 0.22360 1.000 0.0860 calc R H84 H Uiso 0.04550 0.73640 0.19870 1.000 0.0670 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0296(3) 0.0246(4) 0.0268(3) 0.0000(3) 0.0093(3) 0.0024(3) Si1 0.0376(5) 0.0562(7) 0.0332(5) 0.0087(5) 0.0080(4) -0.0075(5) Si2 0.0393(6) 0.0729(9) 0.0434(6) 0.0188(6) 0.0090(5) 0.0081(6) O1 0.0328(13) 0.0276(13) 0.0395(13) -0.0042(11) 0.0118(10) 0.0017(11) O2 0.0387(13) 0.0245(13) 0.0398(13) -0.0046(11) 0.0167(11) -0.0020(10) N1 0.0327(15) 0.0259(15) 0.0306(14) 0.0016(12) 0.0096(11) 0.0039(12) N2 0.0327(15) 0.0231(15) 0.0329(14) 0.0026(12) 0.0089(12) 0.0020(12) N3 0.0358(16) 0.038(2) 0.0314(15) 0.0060(14) 0.0042(12) -0.0021(15) C1 0.0375(18) 0.0251(17) 0.0292(16) -0.0022(14) 0.0092(14) 0.0003(14) C2 0.0358(18) 0.0206(16) 0.0351(17) 0.0015(13) 0.0119(14) -0.0014(13) C3 0.046(2) 0.0219(18) 0.046(2) -0.0006(16) 0.0157(17) 0.0066(16) C4 0.066(3) 0.0191(17) 0.050(2) -0.0033(17) 0.0177(19) 0.0044(17) C5 0.057(2) 0.0211(18) 0.049(2) 0.0017(16) 0.0105(18) -0.0037(16) C6 0.045(2) 0.0253(19) 0.047(2) -0.0036(16) 0.0144(17) -0.0043(16) C7 0.0383(18) 0.0285(19) 0.0343(17) -0.0041(15) 0.0104(14) 0.0013(15) C8 0.0362(18) 0.0284(19) 0.0413(19) 0.0023(16) 0.0167(15) 0.0057(16) C9 0.0297(17) 0.0259(19) 0.0339(18) 0.0007(15) 0.0096(14) 0.0026(14) C10 0.0307(18) 0.0268(19) 0.0349(19) 0.0011(15) 0.0098(15) -0.0010(15) C11 0.038(2) 0.038(2) 0.042(2) 0.0033(18) 0.0179(17) 0.0039(17) C12 0.039(2) 0.043(2) 0.036(2) 0.0032(18) 0.0142(16) -0.0032(18) C13 0.045(2) 0.032(2) 0.042(2) -0.0053(17) 0.0179(16) 0.0032(17) C14 0.058(3) 0.052(3) 0.041(2) 0.000(2) 0.025(2) -0.002(2) C15 0.083(4) 0.065(3) 0.092(4) -0.022(3) 0.059(3) -0.031(3) C16 0.088(3) 0.056(3) 0.075(3) 0.004(3) 0.052(3) 0.015(3) C17 0.102(4) 0.088(4) 0.063(3) 0.016(3) 0.033(3) 0.003(3) C18 0.0347(19) 0.027(2) 0.044(2) 0.0020(17) 0.0094(16) -0.0009(16) C19 0.059(3) 0.035(2) 0.059(3) -0.015(2) 0.025(2) -0.012(2) C20 0.048(2) 0.054(3) 0.047(2) -0.008(2) 0.0042(18) 0.004(2) C21 0.039(2) 0.030(2) 0.064(3) -0.0024(19) 0.0138(18) 0.0058(17) C22 0.0342(17) 0.0245(18) 0.0348(17) 0.0033(15) 0.0060(13) -0.0021(15) C23 0.0324(17) 0.0287(19) 0.0304(17) 0.0002(15) 0.0109(13) 0.0059(15) C24 0.0326(18) 0.034(2) 0.0312(17) 0.0032(16) 0.0123(14) 0.0044(16) C25 0.0361(19) 0.030(2) 0.0316(18) -0.0005(15) 0.0106(15) -0.0015(16) C26 0.042(2) 0.036(2) 0.038(2) 0.0014(17) 0.0160(17) 0.0123(18) C27 0.037(2) 0.042(2) 0.040(2) 0.0058(18) 0.0193(17) 0.0044(18) C28 0.0317(18) 0.031(2) 0.044(2) 0.0001(17) 0.0109(15) 0.0001(16) C29 0.030(2) 0.053(3) 0.052(2) -0.002(2) 0.0118(18) 0.0093(18) C30 0.039(2) 0.076(4) 0.066(3) 0.014(3) 0.009(2) 0.016(2) C31 0.034(2) 0.067(4) 0.153(6) -0.024(4) 0.038(3) -0.016(3) C32 0.050(3) 0.106(4) 0.059(3) 0.006(3) 0.026(2) 0.022(3) C33 0.041(2) 0.036(2) 0.050(2) -0.0114(18) 0.0155(18) -0.0005(18) C34 0.053(2) 0.041(2) 0.061(3) -0.003(2) 0.021(2) -0.0069(19) C35 0.058(3) 0.056(3) 0.043(2) -0.010(2) 0.0011(19) -0.002(2) C36 0.060(3) 0.048(3) 0.080(3) -0.032(2) 0.029(2) -0.004(2) C37 0.044(3) 0.260(11) 0.076(4) -0.014(5) 0.022(3) 0.054(5) C38 0.054(3) 0.147(7) 0.074(4) -0.007(4) -0.003(3) -0.026(4) C39 0.074(3) 0.097(4) 0.040(2) -0.005(3) 0.015(2) -0.022(3) C40 0.082(4) 0.065(4) 0.082(4) 0.021(3) 0.031(3) -0.014(3) Sc2 0.0289(3) 0.0251(4) 0.0286(3) -0.0003(3) 0.0086(3) -0.0002(3) Si3 0.0359(6) 0.0695(10) 0.1025(11) -0.0025(9) 0.0001(7) -0.0099(7) Si4 0.0720(8) 0.0588(8) 0.0386(6) -0.0088(6) 0.0170(5) 0.0080(7) O3 0.0472(15) 0.0321(14) 0.0365(13) 0.0025(11) 0.0216(11) 0.0069(12) O4 0.0335(13) 0.0271(13) 0.0431(14) 0.0030(11) 0.0177(11) 0.0003(11) N4 0.0377(15) 0.0211(14) 0.0332(14) -0.0023(12) 0.0099(12) -0.0023(12) N5 0.0333(15) 0.0192(14) 0.0363(15) -0.0015(12) 0.0096(12) -0.0017(11) N6 0.0388(17) 0.047(2) 0.0343(16) -0.0074(15) 0.0083(13) -0.0060(16) C41 0.0373(18) 0.0213(16) 0.0345(17) 0.0004(14) 0.0056(14) 0.0017(14) C42 0.0381(18) 0.0210(16) 0.0349(18) -0.0027(14) 0.0090(14) -0.0034(13) C43 0.042(2) 0.0259(19) 0.046(2) -0.0011(16) 0.0080(17) 0.0045(16) C44 0.051(2) 0.0231(18) 0.053(2) -0.0069(17) 0.0066(18) 0.0056(16) C45 0.065(3) 0.027(2) 0.053(2) 0.0083(18) 0.020(2) 0.0065(18) C46 0.054(2) 0.029(2) 0.044(2) 0.0047(17) 0.0179(18) 0.0021(17) C47 0.0373(19) 0.0318(19) 0.0342(17) -0.0034(16) 0.0113(14) 0.0013(16) C48 0.0363(18) 0.032(2) 0.0297(17) -0.0056(16) 0.0132(14) -0.0024(16) C49 0.0346(18) 0.0283(19) 0.0250(16) -0.0049(14) 0.0105(14) -0.0020(15) C50 0.040(2) 0.038(2) 0.0302(18) 0.0010(16) 0.0125(16) -0.0087(17) C51 0.042(2) 0.042(2) 0.036(2) 0.0046(18) 0.0125(17) -0.0112(19) C52 0.034(2) 0.049(3) 0.036(2) -0.0020(19) 0.0098(16) -0.0092(19) C53 0.0356(19) 0.039(2) 0.039(2) -0.0065(18) 0.0105(15) -0.0011(18) C54 0.036(2) 0.056(3) 0.059(3) 0.006(2) 0.010(2) -0.007(2) C55 0.044(3) 0.196(8) 0.065(3) -0.008(4) 0.026(2) -0.039(4) C56 0.040(3) 0.088(5) 0.188(8) 0.032(5) 0.041(4) -0.001(3) C57 0.051(3) 0.121(6) 0.084(4) -0.025(4) 0.004(3) -0.012(3) C58 0.049(2) 0.030(2) 0.037(2) 0.0073(16) 0.0162(17) -0.0045(17) C59 0.095(4) 0.027(2) 0.063(3) 0.000(2) 0.024(3) 0.012(2) C60 0.064(3) 0.054(3) 0.044(2) 0.010(2) 0.012(2) 0.015(2) C61 0.064(3) 0.080(4) 0.125(5) 0.064(4) 0.025(3) -0.007(3) C62 0.0417(19) 0.0240(18) 0.0375(18) 0.0018(15) 0.0152(15) -0.0017(15) C63 0.0324(17) 0.0273(19) 0.0365(18) -0.0028(15) 0.0139(14) -0.0026(15) C64 0.0307(18) 0.035(2) 0.0336(18) -0.0034(16) 0.0125(14) -0.0030(16) C65 0.0257(17) 0.034(2) 0.044(2) -0.0020(17) 0.0125(15) -0.0036(15) C66 0.0332(19) 0.028(2) 0.048(2) -0.0040(18) 0.0103(17) 0.0054(16) C67 0.044(2) 0.038(2) 0.044(2) -0.0010(18) 0.0219(18) -0.0010(18) C68 0.048(2) 0.033(2) 0.0366(19) -0.0009(16) 0.0179(16) -0.0013(17) C69 0.056(3) 0.040(3) 0.052(2) 0.000(2) 0.033(2) 0.007(2) C70 0.415(17) 0.208(10) 0.136(7) -0.134(7) 0.213(10) -0.220(11) C71 0.256(10) 0.165(8) 0.123(6) 0.087(6) 0.163(7) 0.123(8) C72 0.066(4) 0.237(10) 0.088(4) -0.020(6) 0.043(3) -0.003(5) C73 0.0357(19) 0.028(2) 0.049(2) 0.0086(17) 0.0171(16) 0.0049(16) C74 0.048(2) 0.036(2) 0.064(3) 0.013(2) 0.0118(19) -0.0014(19) C75 0.050(2) 0.044(2) 0.047(2) 0.0079(19) 0.0120(18) 0.0023(19) C76 0.064(3) 0.039(3) 0.068(3) 0.001(2) 0.022(2) 0.018(2) C77 0.092(4) 0.058(3) 0.069(3) -0.016(3) 0.014(3) 0.017(3) C78 0.110(5) 0.094(4) 0.056(3) 0.005(3) 0.037(3) 0.020(4) C79 0.063(3) 0.106(5) 0.099(4) -0.016(4) -0.011(3) 0.020(3) C80 0.070(4) 0.109(5) 0.115(5) -0.020(4) 0.006(3) -0.011(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 O1 1.985(3) . . yes Sc1 O2 1.976(3) . . yes Sc1 N1 2.254(3) . . yes Sc1 N2 2.227(3) . . yes Sc1 N3 2.048(3) . . yes Sc2 N4 2.268(3) . . yes Sc2 N5 2.215(3) . . yes Sc2 N6 2.050(3) . . yes Sc2 O4 1.977(3) . . yes Sc2 O3 1.981(3) . . yes Si1 N3 1.723(3) . . yes Si1 C40 1.869(6) . . yes Si1 C39 1.882(5) . . yes Si2 C37 1.852(6) . . yes Si2 N3 1.710(3) . . yes Si2 C38 1.883(8) . . yes Si1 H81 1.4500 . . no Si2 H82 1.4500 . . no Si3 C80 1.741(8) . . yes Si3 N6 1.700(3) . . yes Si3 C79 1.863(7) . . yes Si4 C77 1.842(6) . . yes Si4 C78 1.857(6) . . yes Si4 N6 1.738(3) . . yes Si3 H83 1.4500 . . no Si4 H84 1.4500 . . no O1 C24 1.320(4) . . yes O2 C9 1.329(4) . . yes O3 C64 1.320(4) . . yes O4 C49 1.316(4) . . yes N1 C22 1.290(4) . . yes N1 C1 1.492(4) . . yes N2 C2 1.485(4) . . yes N2 C7 1.282(4) . . yes N4 C41 1.492(4) . . yes N4 C62 1.290(4) . . yes N5 C42 1.487(4) . . yes N5 C47 1.276(4) . . yes C1 C2 1.524(4) . . no C1 C6 1.538(5) . . no C2 C3 1.516(5) . . no C3 C4 1.532(6) . . no C4 C5 1.511(6) . . no C5 C6 1.525(6) . . no C7 C8 1.433(5) . . no C8 C13 1.407(5) . . no C8 C9 1.421(5) . . no C9 C10 1.433(5) . . no C10 C11 1.370(5) . . no C10 C18 1.538(5) . . no C11 C12 1.415(6) . . no C12 C14 1.520(6) . . no C12 C13 1.356(6) . . no C14 C17 1.517(7) . . no C14 C15 1.561(7) . . no C14 C16 1.504(7) . . no C18 C20 1.534(6) . . no C18 C19 1.528(6) . . no C18 C21 1.529(6) . . no C22 C23 1.437(5) . . no C23 C28 1.433(4) . . no C23 C24 1.393(5) . . no C24 C25 1.455(5) . . no C25 C33 1.525(6) . . no C25 C26 1.372(6) . . no C26 C27 1.410(6) . . no C27 C28 1.353(5) . . no C27 C29 1.534(6) . . no C29 C30 1.558(7) . . no C29 C32 1.520(6) . . no C29 C31 1.536(8) . . no C33 C36 1.537(6) . . no C33 C34 1.519(6) . . no C33 C35 1.549(6) . . no C1 H1 1.0000 . . no C2 H2 1.0000 . . no C3 H3A 0.9900 . . no C3 H3B 0.9900 . . no C4 H4B 0.9900 . . no C4 H4A 0.9900 . . no C5 H5B 0.9900 . . no C5 H5A 0.9900 . . no C6 H6B 0.9900 . . no C6 H6A 0.9900 . . no C7 H7 0.9500 . . no C11 H11 0.9500 . . no C13 H13 0.9500 . . no C15 H15A 0.9800 . . no C15 H15C 0.9800 . . no C15 H15B 0.9800 . . no C16 H16B 0.9800 . . no C16 H16C 0.9800 . . no C16 H16A 0.9800 . . no C17 H17C 0.9800 . . no C17 H17B 0.9800 . . no C17 H17A 0.9800 . . no C19 H19A 0.9800 . . no C19 H19C 0.9800 . . no C19 H19B 0.9800 . . no C20 H20C 0.9800 . . no C20 H20B 0.9800 . . no C20 H20A 0.9800 . . no C21 H21B 0.9800 . . no C21 H21C 0.9800 . . no C21 H21A 0.9800 . . no C22 H22 0.9500 . . no C26 H26 0.9500 . . no C28 H28 0.9500 . . no C30 H30B 0.9800 . . no C30 H30C 0.9800 . . no C30 H30A 0.9800 . . no C31 H31A 0.9800 . . no C31 H31C 0.9800 . . no C31 H31B 0.9800 . . no C32 H32C 0.9800 . . no C32 H32A 0.9800 . . no C32 H32B 0.9800 . . no C34 H34A 0.9800 . . no C34 H34B 0.9800 . . no C34 H34C 0.9800 . . no C35 H35C 0.9800 . . no C35 H35A 0.9800 . . no C35 H35B 0.9800 . . no C36 H36C 0.9800 . . no C36 H36A 0.9800 . . no C36 H36B 0.9800 . . no C37 H37B 0.9800 . . no C37 H37C 0.9800 . . no C37 H37A 0.9800 . . no C38 H38A 0.9800 . . no C38 H38C 0.9800 . . no C38 H38B 0.9800 . . no C39 H39C 0.9800 . . no C39 H39A 0.9800 . . no C39 H39B 0.9800 . . no C40 H40A 0.9800 . . no C40 H40C 0.9800 . . no C40 H40B 0.9800 . . no C41 C46 1.536(5) . . no C41 C42 1.516(5) . . no C42 C43 1.519(5) . . no C43 C44 1.535(6) . . no C44 C45 1.525(6) . . no C45 C46 1.529(6) . . no C47 C48 1.464(5) . . no C48 C49 1.424(5) . . no C48 C53 1.392(5) . . no C49 C50 1.415(5) . . no C50 C51 1.395(6) . . no C50 C58 1.541(6) . . no C51 C52 1.399(6) . . no C52 C53 1.385(7) . . no C52 C54 1.550(6) . . no C54 C56 1.496(9) . . no C54 C57 1.488(8) . . no C54 C55 1.521(7) . . no C58 C61 1.553(8) . . no C58 C59 1.518(7) . . no C58 C60 1.537(6) . . no C62 C63 1.476(5) . . no C63 C64 1.395(5) . . no C63 C68 1.400(5) . . no C64 C65 1.420(5) . . no C65 C66 1.394(5) . . no C65 C73 1.539(5) . . no C66 C67 1.399(5) . . no C67 C68 1.382(6) . . no C67 C69 1.551(6) . . no C69 C71 1.514(11) . . no C69 C72 1.539(8) . . no C69 C70 1.397(11) . . no C73 C76 1.534(6) . . no C73 C74 1.529(6) . . no C73 C75 1.519(6) . . no C41 H41 1.0000 . . no C42 H42 1.0000 . . no C43 H43A 0.9900 . . no C43 H43B 0.9900 . . no C44 H44A 0.9900 . . no C44 H44B 0.9900 . . no C45 H45A 0.9900 . . no C45 H45B 0.9900 . . no C46 H46A 0.9900 . . no C46 H46B 0.9900 . . no C47 H47 0.9500 . . no C51 H51 0.9500 . . no C53 H53 0.9500 . . no C55 H55A 0.9800 . . no C55 H55B 0.9800 . . no C55 H55C 0.9800 . . no C56 H56A 0.9800 . . no C56 H56B 0.9800 . . no C56 H56C 0.9800 . . no C57 H57A 0.9800 . . no C57 H57B 0.9800 . . no C57 H57C 0.9800 . . no C59 H59A 0.9800 . . no C59 H59B 0.9800 . . no C59 H59C 0.9800 . . no C60 H60A 0.9800 . . no C60 H60B 0.9800 . . no C60 H60C 0.9800 . . no C61 H61A 0.9800 . . no C61 H61B 0.9800 . . no C61 H61C 0.9800 . . no C62 H62 0.9500 . . no C66 H66 0.9500 . . no C68 H68 0.9500 . . no C70 H70A 0.9800 . . no C70 H70B 0.9800 . . no C70 H70C 0.9800 . . no C71 H71A 0.9800 . . no C71 H71B 0.9800 . . no C71 H71C 0.9800 . . no C72 H72A 0.9800 . . no C72 H72B 0.9800 . . no C72 H72C 0.9800 . . no C74 H74A 0.9800 . . no C74 H74B 0.9800 . . no C74 H74C 0.9800 . . no C75 H75A 0.9800 . . no C75 H75B 0.9800 . . no C75 H75C 0.9800 . . no C76 H76A 0.9800 . . no C76 H76B 0.9800 . . no C76 H76C 0.9800 . . no C77 H77A 0.9800 . . no C77 H77B 0.9800 . . no C77 H77C 0.9800 . . no C78 H78A 0.9800 . . no C78 H78B 0.9800 . . no C78 H78C 0.9800 . . no C79 H79A 0.9800 . . no C79 H79B 0.9800 . . no C79 H79C 0.9800 . . no C80 H80A 0.9800 . . no C80 H80B 0.9800 . . no C80 H80C 0.9800 . . no 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 O1 Sc1 O2 100.58(11) . . . yes O1 Sc1 N1 81.64(10) . . . yes O1 Sc1 N2 140.03(10) . . . yes O1 Sc1 N3 113.86(12) . . . yes O2 Sc1 N1 136.66(10) . . . yes O2 Sc1 N2 80.10(10) . . . yes O2 Sc1 N3 110.02(12) . . . yes N1 Sc1 N2 72.17(10) . . . yes N1 Sc1 N3 108.23(12) . . . yes N2 Sc1 N3 102.91(12) . . . yes O3 Sc2 O4 100.59(11) . . . yes O3 Sc2 N4 80.70(10) . . . yes O3 Sc2 N5 141.81(11) . . . yes O3 Sc2 N6 114.20(12) . . . yes O4 Sc2 N4 133.93(10) . . . yes O4 Sc2 N5 81.20(10) . . . yes O4 Sc2 N6 111.12(12) . . . yes N4 Sc2 N5 71.83(10) . . . yes N4 Sc2 N6 109.90(12) . . . yes N5 Sc2 N6 100.05(12) . . . yes N3 Si1 C40 113.2(2) . . . yes C39 Si1 C40 109.5(2) . . . yes N3 Si1 C39 114.0(2) . . . yes N3 Si2 C37 113.0(2) . . . yes C37 Si2 C38 106.7(3) . . . yes N3 Si2 C38 112.6(2) . . . yes C40 Si1 H81 107.00 . . . no C39 Si1 H81 107.00 . . . no N3 Si1 H81 106.00 . . . no C37 Si2 H82 108.00 . . . no C38 Si2 H82 108.00 . . . no N3 Si2 H82 108.00 . . . no N6 Si3 C80 114.3(3) . . . yes N6 Si3 C79 113.3(2) . . . yes C79 Si3 C80 108.4(3) . . . yes N6 Si4 C77 113.1(2) . . . yes N6 Si4 C78 114.4(2) . . . yes C77 Si4 C78 109.0(3) . . . yes N6 Si3 H83 107.00 . . . no C79 Si3 H83 107.00 . . . no C80 Si3 H83 107.00 . . . no C77 Si4 H84 107.00 . . . no C78 Si4 H84 107.00 . . . no N6 Si4 H84 107.00 . . . no Sc1 O1 C24 138.1(2) . . . yes Sc1 O2 C9 139.9(2) . . . yes Sc2 O3 C64 142.3(2) . . . yes Sc2 O4 C49 140.4(2) . . . yes Sc1 N1 C22 125.5(2) . . . yes Sc1 N1 C1 116.9(2) . . . yes C1 N1 C22 117.4(3) . . . yes Sc1 N2 C2 109.21(19) . . . yes Sc1 N2 C7 129.2(2) . . . yes C2 N2 C7 121.5(3) . . . yes Sc1 N3 Si2 126.82(17) . . . yes Sc1 N3 Si1 112.66(16) . . . yes Si1 N3 Si2 120.37(18) . . . yes Sc2 N4 C41 116.5(2) . . . yes Sc2 N4 C62 126.3(2) . . . yes C41 N4 C62 116.7(3) . . . yes C42 N5 C47 121.8(3) . . . yes Sc2 N5 C47 129.1(2) . . . yes Sc2 N5 C42 109.19(19) . . . yes Sc2 N6 Si4 114.49(16) . . . yes Sc2 N6 Si3 124.24(17) . . . yes Si3 N6 Si4 121.19(19) . . . yes N1 C1 C6 115.5(3) . . . yes C2 C1 C6 110.4(3) . . . no N1 C1 C2 108.0(3) . . . yes C1 C2 C3 111.7(3) . . . no N2 C2 C3 118.0(3) . . . yes N2 C2 C1 106.7(2) . . . yes C2 C3 C4 109.0(3) . . . no C3 C4 C5 111.1(3) . . . no C4 C5 C6 111.9(3) . . . no C1 C6 C5 109.4(3) . . . no N2 C7 C8 126.1(3) . . . yes C9 C8 C13 119.5(3) . . . no C7 C8 C13 118.1(3) . . . no C7 C8 C9 122.3(3) . . . no O2 C9 C8 120.7(3) . . . yes C8 C9 C10 118.9(3) . . . no O2 C9 C10 120.4(3) . . . yes C9 C10 C18 120.1(3) . . . no C11 C10 C18 122.7(3) . . . no C9 C10 C11 117.3(3) . . . no C10 C11 C12 125.2(4) . . . no C11 C12 C14 119.9(4) . . . no C13 C12 C14 123.8(4) . . . no C11 C12 C13 116.3(4) . . . no C8 C13 C12 122.8(4) . . . no C12 C14 C17 109.3(4) . . . no C12 C14 C16 112.1(4) . . . no C16 C14 C17 111.1(4) . . . no C15 C14 C16 104.5(4) . . . no C15 C14 C17 109.1(4) . . . no C12 C14 C15 110.7(4) . . . no C20 C18 C21 108.8(3) . . . no C10 C18 C21 111.0(3) . . . no C10 C18 C19 112.7(3) . . . no C10 C18 C20 109.5(3) . . . no C19 C18 C20 107.0(4) . . . no C19 C18 C21 107.8(3) . . . no N1 C22 C23 126.9(3) . . . yes C22 C23 C28 115.7(3) . . . no C22 C23 C24 124.5(3) . . . no C24 C23 C28 119.7(3) . . . no O1 C24 C23 120.4(3) . . . yes O1 C24 C25 120.5(3) . . . yes C23 C24 C25 119.0(3) . . . no C24 C25 C26 116.6(3) . . . no C26 C25 C33 122.3(4) . . . no C24 C25 C33 121.0(4) . . . no C25 C26 C27 125.8(4) . . . no C26 C27 C28 116.1(4) . . . no C26 C27 C29 120.0(4) . . . no C28 C27 C29 123.9(4) . . . no C23 C28 C27 122.6(3) . . . no C27 C29 C30 107.1(4) . . . no C27 C29 C31 112.2(4) . . . no C31 C29 C32 108.6(4) . . . no C30 C29 C32 110.2(4) . . . no C30 C29 C31 108.8(4) . . . no C27 C29 C32 110.1(3) . . . no C35 C33 C36 107.3(4) . . . no C25 C33 C36 111.4(4) . . . no C34 C33 C35 110.3(4) . . . no C25 C33 C35 110.3(3) . . . no C34 C33 C36 107.7(4) . . . no C25 C33 C34 109.8(3) . . . no C6 C1 H1 107.00 . . . no N1 C1 H1 108.00 . . . no C2 C1 H1 108.00 . . . no N2 C2 H2 107.00 . . . no C1 C2 H2 107.00 . . . no C3 C2 H2 107.00 . . . no C4 C3 H3A 110.00 . . . no C2 C3 H3A 110.00 . . . no C4 C3 H3B 110.00 . . . no H3A C3 H3B 108.00 . . . no C2 C3 H3B 110.00 . . . no H4A C4 H4B 108.00 . . . no C3 C4 H4A 109.00 . . . no C3 C4 H4B 109.00 . . . no C5 C4 H4B 109.00 . . . no C5 C4 H4A 109.00 . . . no C4 C5 H5A 109.00 . . . no C4 C5 H5B 109.00 . . . no C6 C5 H5A 109.00 . . . no C6 C5 H5B 109.00 . . . no H5A C5 H5B 108.00 . . . no C1 C6 H6A 110.00 . . . no C1 C6 H6B 110.00 . . . no C5 C6 H6B 110.00 . . . no H6A C6 H6B 108.00 . . . no C5 C6 H6A 110.00 . . . no N2 C7 H7 117.00 . . . no C8 C7 H7 117.00 . . . no C12 C11 H11 117.00 . . . no C10 C11 H11 117.00 . . . no C12 C13 H13 119.00 . . . no C8 C13 H13 119.00 . . . no C14 C15 H15A 109.00 . . . no C14 C15 H15B 109.00 . . . no H15A C15 H15B 109.00 . . . no H15A C15 H15C 109.00 . . . no H15B C15 H15C 109.00 . . . no C14 C15 H15C 110.00 . . . no C14 C16 H16A 109.00 . . . no H16A C16 H16B 109.00 . . . no H16A C16 H16C 109.00 . . . no H16B C16 H16C 109.00 . . . no C14 C16 H16C 110.00 . . . no C14 C16 H16B 110.00 . . . no C14 C17 H17B 110.00 . . . no C14 C17 H17A 109.00 . . . no H17A C17 H17C 109.00 . . . no C14 C17 H17C 110.00 . . . no H17A C17 H17B 109.00 . . . no H17B C17 H17C 110.00 . . . no C18 C19 H19B 109.00 . . . no C18 C19 H19C 109.00 . . . no H19A C19 H19C 110.00 . . . no H19B C19 H19C 109.00 . . . no H19A C19 H19B 109.00 . . . no C18 C19 H19A 109.00 . . . no C18 C20 H20C 109.00 . . . no H20A C20 H20B 109.00 . . . no H20A C20 H20C 109.00 . . . no H20B C20 H20C 109.00 . . . no C18 C20 H20B 110.00 . . . no C18 C20 H20A 109.00 . . . no C18 C21 H21B 109.00 . . . no C18 C21 H21A 109.00 . . . no H21A C21 H21C 109.00 . . . no H21B C21 H21C 109.00 . . . no C18 C21 H21C 109.00 . . . no H21A C21 H21B 110.00 . . . no N1 C22 H22 117.00 . . . no C23 C22 H22 117.00 . . . no C25 C26 H26 117.00 . . . no C27 C26 H26 117.00 . . . no C27 C28 H28 119.00 . . . no C23 C28 H28 119.00 . . . no C29 C30 H30B 109.00 . . . no C29 C30 H30C 109.00 . . . no C29 C30 H30A 109.00 . . . no H30A C30 H30C 110.00 . . . no H30B C30 H30C 110.00 . . . no H30A C30 H30B 109.00 . . . no C29 C31 H31B 110.00 . . . no C29 C31 H31C 109.00 . . . no H31A C31 H31B 110.00 . . . no H31A C31 H31C 109.00 . . . no H31B C31 H31C 110.00 . . . no C29 C31 H31A 109.00 . . . no C29 C32 H32A 109.00 . . . no C29 C32 H32C 109.00 . . . no H32A C32 H32B 109.00 . . . no H32A C32 H32C 110.00 . . . no H32B C32 H32C 109.00 . . . no C29 C32 H32B 109.00 . . . no C33 C34 H34B 109.00 . . . no C33 C34 H34C 109.00 . . . no C33 C34 H34A 109.00 . . . no H34A C34 H34C 109.00 . . . no H34B C34 H34C 109.00 . . . no H34A C34 H34B 110.00 . . . no C33 C35 H35C 109.00 . . . no C33 C35 H35B 109.00 . . . no H35A C35 H35C 109.00 . . . no C33 C35 H35A 110.00 . . . no H35B C35 H35C 110.00 . . . no H35A C35 H35B 110.00 . . . no C33 C36 H36C 109.00 . . . no H36A C36 H36B 109.00 . . . no H36A C36 H36C 110.00 . . . no C33 C36 H36B 109.00 . . . no C33 C36 H36A 110.00 . . . no H36B C36 H36C 109.00 . . . no Si2 C37 H37A 109.00 . . . no H37A C37 H37C 109.00 . . . no Si2 C37 H37B 110.00 . . . no H37B C37 H37C 109.00 . . . no Si2 C37 H37C 110.00 . . . no H37A C37 H37B 109.00 . . . no Si2 C38 H38C 109.00 . . . no Si2 C38 H38A 109.00 . . . no Si2 C38 H38B 110.00 . . . no H38A C38 H38C 109.00 . . . no H38B C38 H38C 110.00 . . . no H38A C38 H38B 109.00 . . . no Si1 C39 H39B 110.00 . . . no H39A C39 H39B 109.00 . . . no H39A C39 H39C 109.00 . . . no Si1 C39 H39C 110.00 . . . no H39B C39 H39C 109.00 . . . no Si1 C39 H39A 109.00 . . . no H40B C40 H40C 110.00 . . . no Si1 C40 H40C 109.00 . . . no H40A C40 H40C 109.00 . . . no Si1 C40 H40B 109.00 . . . no H40A C40 H40B 110.00 . . . no Si1 C40 H40A 109.00 . . . no N4 C41 C42 107.9(2) . . . yes N4 C41 C46 114.6(3) . . . yes C42 C41 C46 110.2(3) . . . no C41 C42 C43 112.3(3) . . . no N5 C42 C41 106.5(2) . . . yes N5 C42 C43 117.9(3) . . . yes C42 C43 C44 109.0(3) . . . no C43 C44 C45 111.2(3) . . . no C44 C45 C46 111.9(3) . . . no C41 C46 C45 109.5(3) . . . no N5 C47 C48 126.0(3) . . . yes C49 C48 C53 121.3(4) . . . no C47 C48 C49 122.0(3) . . . no C47 C48 C53 116.7(3) . . . no C48 C49 C50 118.1(3) . . . no O4 C49 C48 121.0(3) . . . yes O4 C49 C50 121.0(3) . . . yes C49 C50 C51 118.0(3) . . . no C51 C50 C58 121.4(3) . . . no C49 C50 C58 120.6(4) . . . no C50 C51 C52 124.2(4) . . . no C53 C52 C54 123.5(4) . . . no C51 C52 C53 117.1(4) . . . no C51 C52 C54 119.3(4) . . . no C48 C53 C52 121.1(4) . . . no C52 C54 C55 109.0(4) . . . no C55 C54 C56 109.4(5) . . . no C52 C54 C56 111.4(4) . . . no C52 C54 C57 109.3(4) . . . no C55 C54 C57 108.6(5) . . . no C56 C54 C57 109.2(5) . . . no C50 C58 C60 110.4(3) . . . no C50 C58 C59 109.4(3) . . . no C50 C58 C61 112.8(4) . . . no C59 C58 C60 110.4(4) . . . no C59 C58 C61 107.1(4) . . . no C60 C58 C61 106.7(4) . . . no N4 C62 C63 127.1(3) . . . yes C64 C63 C68 121.5(3) . . . no C62 C63 C64 123.2(3) . . . no C62 C63 C68 115.1(3) . . . no O3 C64 C63 120.0(3) . . . yes O3 C64 C65 121.6(3) . . . yes C63 C64 C65 118.4(3) . . . no C64 C65 C66 117.8(3) . . . no C64 C65 C73 120.8(3) . . . no C66 C65 C73 121.4(3) . . . no C65 C66 C67 124.5(4) . . . no C66 C67 C68 116.3(4) . . . no C68 C67 C69 122.8(4) . . . no C66 C67 C69 120.8(4) . . . no C63 C68 C67 121.5(4) . . . no C70 C69 C71 112.5(6) . . . no C70 C69 C72 104.3(7) . . . no C67 C69 C70 109.8(6) . . . no C67 C69 C71 111.5(5) . . . no C67 C69 C72 108.5(4) . . . no C71 C69 C72 110.0(6) . . . no C75 C73 C76 107.9(4) . . . no C65 C73 C74 108.8(3) . . . no C65 C73 C75 111.1(3) . . . no C65 C73 C76 111.8(3) . . . no C74 C73 C75 110.3(4) . . . no C74 C73 C76 106.9(3) . . . no N4 C41 H41 108.00 . . . no C42 C41 H41 108.00 . . . no C46 C41 H41 108.00 . . . no N5 C42 H42 106.00 . . . no C41 C42 H42 107.00 . . . no C43 C42 H42 106.00 . . . no C42 C43 H43A 110.00 . . . no C42 C43 H43B 110.00 . . . no C44 C43 H43A 110.00 . . . no C44 C43 H43B 110.00 . . . no H43A C43 H43B 108.00 . . . no C43 C44 H44A 109.00 . . . no C43 C44 H44B 109.00 . . . no C45 C44 H44A 109.00 . . . no C45 C44 H44B 109.00 . . . no H44A C44 H44B 108.00 . . . no C44 C45 H45A 109.00 . . . no C44 C45 H45B 109.00 . . . no C46 C45 H45A 109.00 . . . no C46 C45 H45B 109.00 . . . no H45A C45 H45B 108.00 . . . no C41 C46 H46A 110.00 . . . no C41 C46 H46B 110.00 . . . no C45 C46 H46A 110.00 . . . no C45 C46 H46B 110.00 . . . no H46A C46 H46B 108.00 . . . no N5 C47 H47 117.00 . . . no C48 C47 H47 117.00 . . . no C50 C51 H51 118.00 . . . no C52 C51 H51 118.00 . . . no C48 C53 H53 119.00 . . . no C52 C53 H53 119.00 . . . no C54 C55 H55A 110.00 . . . no C54 C55 H55B 110.00 . . . no C54 C55 H55C 109.00 . . . no H55A C55 H55B 109.00 . . . no H55A C55 H55C 109.00 . . . no H55B C55 H55C 109.00 . . . no C54 C56 H56A 110.00 . . . no C54 C56 H56B 109.00 . . . no C54 C56 H56C 109.00 . . . no H56A C56 H56B 110.00 . . . no H56A C56 H56C 109.00 . . . no H56B C56 H56C 109.00 . . . no C54 C57 H57A 109.00 . . . no C54 C57 H57B 110.00 . . . no C54 C57 H57C 109.00 . . . no H57A C57 H57B 109.00 . . . no H57A C57 H57C 109.00 . . . no H57B C57 H57C 110.00 . . . no C58 C59 H59A 109.00 . . . no C58 C59 H59B 109.00 . . . no C58 C59 H59C 109.00 . . . no H59A C59 H59B 109.00 . . . no H59A C59 H59C 109.00 . . . no H59B C59 H59C 110.00 . . . no C58 C60 H60A 109.00 . . . no C58 C60 H60B 110.00 . . . no C58 C60 H60C 110.00 . . . no H60A C60 H60B 109.00 . . . no H60A C60 H60C 109.00 . . . no H60B C60 H60C 109.00 . . . no C58 C61 H61A 110.00 . . . no C58 C61 H61B 109.00 . . . no C58 C61 H61C 109.00 . . . no H61A C61 H61B 110.00 . . . no H61A C61 H61C 109.00 . . . no H61B C61 H61C 109.00 . . . no N4 C62 H62 116.00 . . . no C63 C62 H62 116.00 . . . no C65 C66 H66 118.00 . . . no C67 C66 H66 118.00 . . . no C63 C68 H68 119.00 . . . no C67 C68 H68 119.00 . . . no C69 C70 H70A 109.00 . . . no C69 C70 H70B 109.00 . . . no C69 C70 H70C 109.00 . . . no H70A C70 H70B 109.00 . . . no H70A C70 H70C 110.00 . . . no H70B C70 H70C 110.00 . . . no C69 C71 H71A 109.00 . . . no C69 C71 H71B 109.00 . . . no C69 C71 H71C 110.00 . . . no H71A C71 H71B 110.00 . . . no H71A C71 H71C 109.00 . . . no H71B C71 H71C 110.00 . . . no C69 C72 H72A 109.00 . . . no C69 C72 H72B 109.00 . . . no C69 C72 H72C 110.00 . . . no H72A C72 H72B 110.00 . . . no H72A C72 H72C 109.00 . . . no H72B C72 H72C 109.00 . . . no C73 C74 H74A 109.00 . . . no C73 C74 H74B 110.00 . . . no C73 C74 H74C 109.00 . . . no H74A C74 H74B 110.00 . . . no H74A C74 H74C 109.00 . . . no H74B C74 H74C 109.00 . . . no C73 C75 H75A 110.00 . . . no C73 C75 H75B 109.00 . . . no C73 C75 H75C 109.00 . . . no H75A C75 H75B 109.00 . . . no H75A C75 H75C 109.00 . . . no H75B C75 H75C 109.00 . . . no C73 C76 H76A 110.00 . . . no C73 C76 H76B 109.00 . . . no C73 C76 H76C 110.00 . . . no H76A C76 H76B 109.00 . . . no H76A C76 H76C 109.00 . . . no H76B C76 H76C 109.00 . . . no Si4 C77 H77A 110.00 . . . no Si4 C77 H77B 109.00 . . . no Si4 C77 H77C 109.00 . . . no H77A C77 H77B 109.00 . . . no H77A C77 H77C 110.00 . . . no H77B C77 H77C 109.00 . . . no Si4 C78 H78A 109.00 . . . no Si4 C78 H78B 109.00 . . . no Si4 C78 H78C 109.00 . . . no H78A C78 H78B 110.00 . . . no H78A C78 H78C 110.00 . . . no H78B C78 H78C 109.00 . . . no Si3 C79 H79A 109.00 . . . no Si3 C79 H79B 110.00 . . . no Si3 C79 H79C 110.00 . . . no H79A C79 H79B 109.00 . . . no H79A C79 H79C 109.00 . . . no H79B C79 H79C 110.00 . . . no Si3 C80 H80A 109.00 . . . no Si3 C80 H80B 109.00 . . . no Si3 C80 H80C 110.00 . . . no H80A C80 H80B 109.00 . . . no H80A C80 H80C 109.00 . . . no H80B C80 H80C 110.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Sc1 O1 C24 156.5(3) . . . . no N1 Sc1 O1 C24 20.4(3) . . . . no N2 Sc1 O1 C24 69.3(4) . . . . no N3 Sc1 O1 C24 -85.9(3) . . . . no O1 Sc1 O2 C9 -123.9(3) . . . . no N1 Sc1 O2 C9 -34.9(4) . . . . no N2 Sc1 O2 C9 15.5(3) . . . . no N3 Sc1 O2 C9 115.7(3) . . . . no O1 Sc1 N1 C1 163.2(2) . . . . no O1 Sc1 N1 C22 -10.4(3) . . . . no O2 Sc1 N1 C1 66.6(3) . . . . no O2 Sc1 N1 C22 -107.0(3) . . . . no N2 Sc1 N1 C1 13.8(2) . . . . no N2 Sc1 N1 C22 -159.9(3) . . . . no N3 Sc1 N1 C1 -84.4(2) . . . . no N3 Sc1 N1 C22 102.0(3) . . . . no O1 Sc1 N2 C2 -90.0(2) . . . . no O1 Sc1 N2 C7 87.1(3) . . . . no O2 Sc1 N2 C2 175.3(2) . . . . no O2 Sc1 N2 C7 -7.6(3) . . . . no N1 Sc1 N2 C2 -38.40(19) . . . . no N1 Sc1 N2 C7 138.7(3) . . . . no N3 Sc1 N2 C2 66.9(2) . . . . no N3 Sc1 N2 C7 -116.0(3) . . . . no O1 Sc1 N3 Si1 40.1(2) . . . . no O1 Sc1 N3 Si2 -135.5(2) . . . . no O2 Sc1 N3 Si1 152.09(17) . . . . no O2 Sc1 N3 Si2 -23.4(3) . . . . no N1 Sc1 N3 Si1 -48.7(2) . . . . no N1 Sc1 N3 Si2 135.8(2) . . . . no N2 Sc1 N3 Si1 -123.90(18) . . . . no N2 Sc1 N3 Si2 60.6(3) . . . . no O3 Sc2 O4 C49 -143.4(3) . . . . no N4 Sc2 O4 C49 -56.2(4) . . . . no N5 Sc2 O4 C49 -2.2(3) . . . . no N6 Sc2 O4 C49 95.3(3) . . . . no O3 Sc2 N4 C41 167.4(2) . . . . no O3 Sc2 N4 C62 -4.4(3) . . . . no O4 Sc2 N4 C41 71.6(2) . . . . no O4 Sc2 N4 C62 -100.2(3) . . . . no N5 Sc2 N4 C41 14.3(2) . . . . no N5 Sc2 N4 C62 -157.6(3) . . . . no N6 Sc2 N4 C41 -80.1(2) . . . . no N6 Sc2 N4 C62 108.1(3) . . . . no O3 Sc2 N5 C42 -85.4(3) . . . . no O3 Sc2 N5 C47 93.8(3) . . . . no O4 Sc2 N5 C42 178.7(2) . . . . no O4 Sc2 N5 C47 -2.2(3) . . . . no N4 Sc2 N5 C42 -39.2(2) . . . . no N4 Sc2 N5 C47 140.0(3) . . . . no N6 Sc2 N5 C42 68.6(2) . . . . no N6 Sc2 N5 C47 -112.2(3) . . . . no O3 Sc2 N6 Si3 26.9(3) . . . . no O3 Sc2 N6 Si4 -150.01(17) . . . . no O4 Sc2 N6 Si3 139.9(2) . . . . no O4 Sc2 N6 Si4 -37.1(2) . . . . no N4 Sc2 N6 Si3 -61.6(3) . . . . no N4 Sc2 N6 Si4 121.47(19) . . . . no N5 Sc2 N6 Si3 -135.8(2) . . . . no N5 Sc2 N6 Si4 47.3(2) . . . . no O4 Sc2 O3 C64 137.9(4) . . . . no N4 Sc2 O3 C64 4.7(4) . . . . no N5 Sc2 O3 C64 48.7(4) . . . . no N6 Sc2 O3 C64 -103.1(4) . . . . no C39 Si1 N3 Sc1 -119.6(2) . . . . no C39 Si1 N3 Si2 56.2(3) . . . . no C40 Si1 N3 Sc1 114.3(2) . . . . no C40 Si1 N3 Si2 -69.8(3) . . . . no C37 Si2 N3 Sc1 -34.8(4) . . . . no C37 Si2 N3 Si1 150.0(4) . . . . no C38 Si2 N3 Sc1 86.1(3) . . . . no C38 Si2 N3 Si1 -89.1(3) . . . . no C79 Si3 N6 Sc2 -90.6(3) . . . . no C80 Si3 N6 Sc2 34.2(4) . . . . no C80 Si3 N6 Si4 -149.0(3) . . . . no C79 Si3 N6 Si4 86.1(3) . . . . no C78 Si4 N6 Sc2 122.6(3) . . . . no C77 Si4 N6 Sc2 -111.7(3) . . . . no C78 Si4 N6 Si3 -54.4(4) . . . . no C77 Si4 N6 Si3 71.2(3) . . . . no Sc1 O1 C24 C23 -18.9(5) . . . . no Sc1 O1 C24 C25 161.4(3) . . . . no Sc1 O2 C9 C10 165.3(2) . . . . no Sc1 O2 C9 C8 -14.6(5) . . . . no Sc2 O3 C64 C65 179.7(3) . . . . no Sc2 O3 C64 C63 -0.8(6) . . . . no Sc2 O4 C49 C48 6.6(5) . . . . no Sc2 O4 C49 C50 -174.3(2) . . . . no Sc1 N1 C1 C6 136.6(2) . . . . no C22 N1 C1 C2 -173.5(3) . . . . no Sc1 N1 C1 C2 12.4(3) . . . . no Sc1 N1 C22 C23 1.8(5) . . . . no C1 N1 C22 C23 -171.8(3) . . . . no C22 N1 C1 C6 -49.2(4) . . . . no Sc1 N2 C2 C1 57.9(3) . . . . no Sc1 N2 C2 C3 -175.4(2) . . . . no C7 N2 C2 C1 -119.4(3) . . . . no C7 N2 C2 C3 7.3(5) . . . . no Sc1 N2 C7 C8 0.8(5) . . . . no C2 N2 C7 C8 177.6(3) . . . . no Sc2 N4 C41 C42 12.4(3) . . . . no C62 N4 C41 C42 -175.0(3) . . . . no C41 N4 C62 C63 -170.5(3) . . . . no Sc2 N4 C41 C46 135.5(3) . . . . no Sc2 N4 C62 C63 1.3(5) . . . . no C62 N4 C41 C46 -51.9(4) . . . . no C47 N5 C42 C41 -120.0(3) . . . . no C47 N5 C42 C43 7.2(5) . . . . no Sc2 N5 C47 C48 1.7(5) . . . . no C42 N5 C47 C48 -179.3(3) . . . . no Sc2 N5 C42 C41 59.3(3) . . . . no Sc2 N5 C42 C43 -173.5(2) . . . . no N1 C1 C2 N2 -44.3(3) . . . . no C6 C1 C2 C3 58.2(4) . . . . no N1 C1 C6 C5 -178.9(3) . . . . no N1 C1 C2 C3 -174.6(3) . . . . no C6 C1 C2 N2 -171.5(3) . . . . no C2 C1 C6 C5 -55.9(4) . . . . no N2 C2 C3 C4 178.1(3) . . . . no C1 C2 C3 C4 -57.7(4) . . . . no C2 C3 C4 C5 56.9(4) . . . . no C3 C4 C5 C6 -57.6(4) . . . . no C4 C5 C6 C1 56.4(4) . . . . no N2 C7 C8 C9 5.2(5) . . . . no N2 C7 C8 C13 -174.4(3) . . . . no C7 C8 C9 C10 -179.8(3) . . . . no C7 C8 C13 C12 177.7(4) . . . . no C13 C8 C9 C10 -0.2(5) . . . . no C7 C8 C9 O2 0.2(5) . . . . no C9 C8 C13 C12 -1.9(6) . . . . no C13 C8 C9 O2 179.7(3) . . . . no C8 C9 C10 C11 1.1(5) . . . . no O2 C9 C10 C18 1.8(5) . . . . no C8 C9 C10 C18 -178.3(3) . . . . no O2 C9 C10 C11 -178.8(3) . . . . no C11 C10 C18 C21 122.6(4) . . . . no C9 C10 C18 C20 62.1(4) . . . . no C11 C10 C18 C20 -117.4(4) . . . . no C9 C10 C18 C21 -58.0(4) . . . . no C11 C10 C18 C19 1.6(5) . . . . no C9 C10 C18 C19 -179.0(3) . . . . no C18 C10 C11 C12 179.3(4) . . . . no C9 C10 C11 C12 -0.1(6) . . . . no C10 C11 C12 C13 -1.9(6) . . . . no C10 C11 C12 C14 178.7(4) . . . . no C13 C12 C14 C15 -124.8(5) . . . . no C11 C12 C14 C17 -65.6(5) . . . . no C14 C12 C13 C8 -177.8(4) . . . . no C11 C12 C14 C16 170.8(4) . . . . no C11 C12 C13 C8 2.9(6) . . . . no C13 C12 C14 C16 -8.6(6) . . . . no C13 C12 C14 C17 115.1(5) . . . . no C11 C12 C14 C15 54.6(6) . . . . no N1 C22 C23 C28 -177.5(3) . . . . no N1 C22 C23 C24 6.5(6) . . . . no C22 C23 C24 C25 180.0(3) . . . . no C22 C23 C24 O1 0.2(5) . . . . no C28 C23 C24 O1 -175.7(3) . . . . no C28 C23 C24 C25 4.1(5) . . . . no C22 C23 C28 C27 -176.3(3) . . . . no C24 C23 C28 C27 -0.1(6) . . . . no C23 C24 C25 C26 -4.3(5) . . . . no O1 C24 C25 C26 175.5(3) . . . . no C23 C24 C25 C33 178.7(3) . . . . no O1 C24 C25 C33 -1.5(5) . . . . no C24 C25 C33 C34 66.2(5) . . . . no C24 C25 C26 C27 0.6(6) . . . . no C24 C25 C33 C35 -55.6(5) . . . . no C26 C25 C33 C34 -110.5(4) . . . . no C26 C25 C33 C35 127.7(4) . . . . no C26 C25 C33 C36 8.6(5) . . . . no C33 C25 C26 C27 177.5(4) . . . . no C24 C25 C33 C36 -174.6(3) . . . . no C25 C26 C27 C28 3.3(6) . . . . no C25 C26 C27 C29 -176.6(4) . . . . no C28 C27 C29 C31 2.6(6) . . . . no C28 C27 C29 C32 123.5(5) . . . . no C26 C27 C29 C30 63.1(5) . . . . no C26 C27 C29 C31 -177.6(4) . . . . no C26 C27 C28 C23 -3.5(5) . . . . no C26 C27 C29 C32 -56.6(5) . . . . no C28 C27 C29 C30 -116.7(4) . . . . no C29 C27 C28 C23 176.3(4) . . . . no N4 C41 C42 N5 -44.8(3) . . . . no C46 C41 C42 C43 59.0(4) . . . . no N4 C41 C46 C45 -178.4(3) . . . . no C42 C41 C46 C45 -56.6(4) . . . . no C46 C41 C42 N5 -170.5(3) . . . . no N4 C41 C42 C43 -175.3(3) . . . . no C41 C42 C43 C44 -57.7(4) . . . . no N5 C42 C43 C44 178.0(3) . . . . no C42 C43 C44 C45 55.5(4) . . . . no C43 C44 C45 C46 -56.4(5) . . . . no C44 C45 C46 C41 56.1(4) . . . . no N5 C47 C48 C49 3.1(6) . . . . no N5 C47 C48 C53 -177.6(3) . . . . no C47 C48 C49 O4 -6.8(5) . . . . no C47 C48 C49 C50 174.1(3) . . . . no C53 C48 C49 O4 174.0(3) . . . . no C53 C48 C49 C50 -5.1(5) . . . . no C47 C48 C53 C52 -178.0(3) . . . . no C49 C48 C53 C52 1.3(6) . . . . no O4 C49 C50 C51 -173.5(3) . . . . no O4 C49 C50 C58 6.5(5) . . . . no C48 C49 C50 C51 5.6(5) . . . . no C48 C49 C50 C58 -174.4(3) . . . . no C58 C50 C51 C52 177.5(3) . . . . no C49 C50 C58 C59 -64.3(5) . . . . no C49 C50 C58 C60 57.4(4) . . . . no C49 C50 C58 C61 176.6(4) . . . . no C51 C50 C58 C59 115.7(4) . . . . no C51 C50 C58 C60 -122.7(4) . . . . no C51 C50 C58 C61 -3.5(5) . . . . no C49 C50 C51 C52 -2.6(6) . . . . no C50 C51 C52 C53 -1.2(6) . . . . no C50 C51 C52 C54 176.3(4) . . . . no C54 C52 C53 C48 -175.6(4) . . . . no C51 C52 C54 C55 57.7(6) . . . . no C51 C52 C53 C48 1.9(6) . . . . no C51 C52 C54 C57 -60.8(5) . . . . no C53 C52 C54 C55 -124.9(5) . . . . no C51 C52 C54 C56 178.5(4) . . . . no C53 C52 C54 C56 -4.1(6) . . . . no C53 C52 C54 C57 116.6(5) . . . . no N4 C62 C63 C64 4.8(5) . . . . no N4 C62 C63 C68 179.3(3) . . . . no C62 C63 C64 O3 -5.4(5) . . . . no C62 C63 C64 C65 174.1(3) . . . . no C68 C63 C64 O3 -179.6(3) . . . . no C68 C63 C64 C65 -0.1(5) . . . . no C62 C63 C68 C67 -174.7(4) . . . . no C64 C63 C68 C67 -0.1(6) . . . . no O3 C64 C65 C66 178.7(3) . . . . no O3 C64 C65 C73 0.7(5) . . . . no C63 C64 C65 C66 -0.8(5) . . . . no C63 C64 C65 C73 -178.8(3) . . . . no C64 C65 C66 C67 1.9(6) . . . . no C64 C65 C73 C75 -58.7(5) . . . . no C64 C65 C73 C76 -179.3(3) . . . . no C66 C65 C73 C74 -115.1(4) . . . . no C66 C65 C73 C75 123.4(4) . . . . no C66 C65 C73 C76 2.8(5) . . . . no C73 C65 C66 C67 179.9(4) . . . . no C64 C65 C73 C74 62.8(4) . . . . no C65 C66 C67 C68 -2.1(6) . . . . no C65 C66 C67 C69 -178.6(4) . . . . no C66 C67 C68 C63 1.1(6) . . . . no C66 C67 C69 C71 -177.4(5) . . . . no C66 C67 C69 C72 -56.2(7) . . . . no C68 C67 C69 C70 -119.1(6) . . . . no C68 C67 C69 C71 6.3(7) . . . . no C68 C67 C69 C72 127.5(6) . . . . no C69 C67 C68 C63 177.5(4) . . . . no C66 C67 C69 C70 57.2(7) . . . . no 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 Sc1 C5 3.967(4) . 2_556 no Sc2 C45 3.985(4) . 2_545 no Sc1 H35A 3.5300 . . no Sc1 H37C 3.3800 . . no Sc1 H5B 3.1600 . 2_556 no Sc1 H21B 3.4900 . . no Sc2 H45B 3.1600 . 2_545 no Sc2 H80A 3.3600 . . no Si2 H39A 3.3900 . . no Si4 H42 3.4600 . . no O1 O2 3.047(4) . . no O1 N1 2.779(4) . . no O1 C22 2.876(4) . . no O1 C34 3.107(6) . . no O1 Si1 3.709(3) . . no O1 C35 2.963(5) . . no O2 O1 3.047(4) . . no O2 N2 2.711(4) . . no O2 C21 2.946(5) . . no O2 C7 2.867(4) . . no O2 C20 3.022(5) . . no O3 O4 3.045(4) . . no O3 C74 3.047(6) . . no O3 N4 2.760(4) . . no O3 C62 2.865(4) . . no O3 C75 3.000(5) . . no O4 C60 3.012(5) . . no O4 C47 2.883(4) . . no O4 C59 3.002(6) . . no O4 Si4 3.657(3) . . no O4 O3 3.045(4) . . no O4 N5 2.734(4) . . no O1 H34A 2.4500 . . no O1 H35A 2.3300 . . no O1 H81 2.8600 . . no O1 H5B 2.8300 . 2_556 no O2 H20B 2.3700 . . no O2 H21B 2.2600 . . no O2 H37C 2.8700 . . no O3 H75B 2.3200 . . no O3 H74C 2.4000 . . no O4 H59B 2.3400 . . no O4 H45B 2.7400 . 2_545 no O4 H60C 2.3400 . . no O4 H84 2.8000 . . no N1 O1 2.779(4) . . no N1 Si1 3.780(3) . . no N1 C24 3.006(4) . . no N1 N2 2.639(4) . . no N1 C2 2.441(4) . . no N2 C9 2.956(4) . . no N2 O2 2.711(4) . . no N2 N1 2.639(4) . . no N2 C1 2.414(4) . . no N4 O3 2.760(4) . . no N4 N5 2.630(4) . . no N4 C42 2.431(4) . . no N4 C64 3.022(4) . . no N5 Si4 3.542(3) . . no N5 O4 2.734(4) . . no N5 N4 2.630(4) . . no N5 N6 3.270(4) . . no N5 C41 2.406(4) . . no N5 C49 2.976(4) . . no N6 N5 3.270(4) . . no N5 H84 2.8900 . . no C5 Sc1 3.967(4) . 2_546 no C17 C78 3.441(9) . . no C20 O2 3.022(5) . . no C21 C34 3.585(6) . . no C21 O2 2.946(5) . . no C34 O1 3.107(6) . . no C34 C21 3.585(6) . . no C35 O1 2.963(5) . . no C45 Sc2 3.985(4) . 2_555 no C59 O4 3.002(6) . . no C60 O4 3.012(5) . . no C74 O3 3.047(6) . . no C75 O3 3.000(5) . . no C78 C17 3.441(9) . . no C3 H7 2.4400 . . no C6 H22 2.5900 . . no C7 H3B 2.8200 . . no C7 H3A 2.8500 . . no C7 H37C 3.0200 . . no C8 H37C 3.0900 . . no C9 H37C 3.0300 . . no C9 H21B 2.7700 . . no C9 H20B 2.7800 . . no C11 H19B 2.7900 . . no C11 H15C 2.7400 . . no C11 H19C 2.7800 . . no C11 H30C 3.0300 . 1_655 no C11 H17B 2.7900 . . no C13 H16B 2.7400 . . no C13 H16A 2.7900 . . no C15 H11 2.8100 . . no C16 H13 2.4800 . . no C17 H78A 2.9800 . . no C17 H11 2.9500 . . no C19 H11 2.4600 . . no C21 H34A 2.9400 . . no C21 H4A 3.0800 . 1_565 no C22 H21C 3.0700 . 2_546 no C22 H6B 2.7300 . . no C22 H4A 2.8400 . 2_556 no C23 H4A 3.0500 . 2_556 no C23 H81 3.0100 . . no C24 H3B 3.0500 . 2_556 no C24 H81 2.9200 . . no C24 H35A 2.8400 . . no C24 H34A 2.7800 . . no C26 H32B 2.7000 . . no C26 H30B 2.8400 . . no C26 H36B 2.7200 . . no C26 H36C 2.7700 . . no C28 H31B 2.6900 . . no C28 H31A 2.9100 . . no C30 H26 2.9100 . . no C31 H28 2.4900 . . no C32 H26 2.8100 . . no C36 H26 2.4100 . . no C40 H60B 3.0900 . 2_546 no C43 H47 2.4500 . . no C46 H62 2.5800 . . no C47 H74B 3.0500 . 2_555 no C47 H84 3.0600 . . no C47 H43A 2.8600 . . no C47 H43B 2.8300 . . no C49 H60C 2.7300 . . no C49 H45B 3.0900 . 2_545 no C49 H59B 2.7900 . . no C49 H84 2.9700 . . no C51 H55C 2.7000 . . no C51 H57C 2.7300 . . no C51 H61A 2.7800 . . no C51 H61B 2.7900 . . no C53 H56B 2.9100 . . no C53 H56A 2.6300 . . no C55 H51 2.8000 . . no C56 H53 2.5100 . . no C57 H51 2.8800 . . no C59 H44A 3.0900 . 1_545 no C59 H74C 3.0000 . . no C61 H51 2.4600 . . no C62 H46B 2.7100 . . no C62 H59C 3.1000 . 2_555 no C62 H44A 2.8700 . 2_545 no C64 H74C 2.7900 . . no C64 H80A 3.0500 . . no C64 H43B 3.0400 . 2_545 no C64 H75B 2.7700 . . no C66 H76A 2.7600 . . no C66 H76B 2.7300 . . no C66 H72A 2.8200 . . no C66 H70B 2.6700 . . no C68 H71B 2.7600 . . no C68 H71C 2.7800 . . no C70 H66 2.8300 . . no C70 H39A 3.0800 . 1_554 no C71 H68 2.4900 . . no C72 H66 2.8200 . . no C74 H45A 3.0900 . 1_545 no C74 H59B 2.9900 . . no C76 H66 2.4200 . . no H1 H5B 2.5100 . . no H1 H3B 2.5300 . . no H1 H21C 2.4200 . 2_546 no H2 H4B 2.4500 . . no H2 H6A 2.5100 . . no H3A C7 2.8500 . . no H3A H7 2.3100 . . no H3B H1 2.5300 . . no H3B C24 3.0500 . 2_546 no H3B H5B 2.5800 . . no H3B H7 2.2200 . . no H3B C7 2.8200 . . no H4A C22 2.8400 . 2_546 no H4A C23 3.0500 . 2_546 no H4A C21 3.0800 . 1_545 no H4A H21C 2.4900 . 1_545 no H4B H2 2.4500 . . no H5A H34C 2.5700 . 1_545 no H5B H3B 2.5800 . . no H5B H1 2.5100 . . no H5B O1 2.8300 . 2_546 no H5B Sc1 3.1600 . 2_546 no H6A H2 2.5100 . . no H6B C22 2.7300 . . no H6B H22 2.0800 . . no H7 H3A 2.3100 . . no H7 C3 2.4400 . . no H7 H13 2.3400 . . no H7 H3B 2.2200 . . no H11 C19 2.4600 . . no H11 H15C 2.2400 . . no H11 H19B 2.2500 . . no H11 H19C 2.2300 . . no H11 H17B 2.4100 . . no H11 C17 2.9500 . . no H11 C15 2.8100 . . no H13 H16B 2.2600 . . no H13 C16 2.4800 . . no H13 H7 2.3400 . . no H13 H16A 2.2500 . . no H15A H16C 2.3400 . . no H15A H17A 2.4800 . . no H15B H16B 2.4200 . . no H15C C11 2.7400 . . no H15C H11 2.2400 . . no H15C H17B 2.5300 . . no H16A C13 2.7900 . . no H16A H13 2.2500 . . no H16A H17C 2.5200 . . no H16B C13 2.7400 . . no H16B H13 2.2600 . . no H16B H15B 2.4200 . . no H16B H30B 2.5300 . 2_546 no H16C H15A 2.3400 . . no H16C H17A 2.5000 . . no H17A H15A 2.4800 . . no H17A H16C 2.5000 . . no H17B C11 2.7900 . . no H17B H31A 2.5900 . 2_556 no H17B H15C 2.5300 . . no H17B H11 2.4100 . . no H17C H16A 2.5200 . . no H19A H21A 2.4200 . . no H19A H20C 2.4300 . . no H19B C11 2.7900 . . no H19B H28 2.5500 . 2_556 no H19B H11 2.2500 . . no H19B H21C 2.4900 . . no H19B H31B 2.5400 . 2_556 no H19C H11 2.2300 . . no H19C H20A 2.4500 . . no H19C C11 2.7800 . . no H20A H32A 2.3200 . 1_655 no H20A H19C 2.4500 . . no H20A H30C 2.4400 . 1_655 no H20B C9 2.7800 . . no H20B H21B 2.5300 . . no H20B H38A 2.3400 . . no H20B O2 2.3700 . . no H20C H19A 2.4300 . . no H20C H21A 2.4400 . . no H21A H19A 2.4200 . . no H21A H20C 2.4400 . . no H21B O2 2.2600 . . no H21B C9 2.7700 . . no H21B H20B 2.5300 . . no H21B H34A 2.3600 . . no H21B Sc1 3.4900 . . no H21C H4A 2.4900 . 1_565 no H21C H19B 2.4900 . . no H21C H22 2.5200 . 2_556 no H21C H1 2.4200 . 2_556 no H21C C22 3.0700 . 2_556 no H22 H6B 2.0800 . . no H22 H28 2.2900 . . no H22 C6 2.5900 . . no H22 H21C 2.5200 . 2_546 no H26 C32 2.8100 . . no H26 C30 2.9100 . . no H26 H32B 2.2100 . . no H26 H36B 2.2000 . . no H26 H36C 2.1800 . . no H26 H30B 2.4200 . . no H26 C36 2.4100 . . no H28 H22 2.2900 . . no H28 C31 2.4900 . . no H28 H31A 2.4000 . . no H28 H31B 2.1500 . . no H28 H19B 2.5500 . 2_546 no H30B C26 2.8400 . . no H30B H26 2.4200 . . no H30B H32B 2.4700 . . no H30B H16B 2.5300 . 2_556 no H30C C11 3.0300 . 1_455 no H30C H20A 2.4400 . 1_455 no H30C H31C 2.3800 . . no H31A C28 2.9100 . . no H31A H28 2.4000 . . no H31A H32C 2.4200 . . no H31A H17B 2.5900 . 2_546 no H31B C28 2.6900 . . no H31B H19B 2.5400 . 2_546 no H31B H28 2.1500 . . no H31C H32A 2.5300 . . no H31C H30C 2.3800 . . no H32A H20A 2.3200 . 1_455 no H32A H31C 2.5300 . . no H32B H26 2.2100 . . no H32B C26 2.7000 . . no H32B H30B 2.4700 . . no H32C H31A 2.4200 . . no H34A O1 2.4500 . . no H34A H35A 2.5900 . . no H34A C21 2.9400 . . no H34A C24 2.7800 . . no H34A H21B 2.3600 . . no H34B H35C 2.4900 . . no H34B H36A 2.5600 . . no H34C H5A 2.5700 . 1_565 no H34C H36C 2.3400 . . no H35A C24 2.8400 . . no H35A H34A 2.5900 . . no H35A O1 2.3300 . . no H35A Sc1 3.5300 . . no H35B H36B 2.5900 . . no H35C H36A 2.3500 . . no H35C H34B 2.4900 . . no H36A H35C 2.3500 . . no H36A H34B 2.5600 . . no H36B H26 2.2000 . . no H36B C26 2.7200 . . no H36B H35B 2.5900 . . no H36C H26 2.1800 . . no H36C C26 2.7700 . . no H36C H34C 2.3400 . . no H37C C8 3.0900 . . no H37C C9 3.0300 . . no H37C C7 3.0200 . . no H37C Sc1 3.3800 . . no H37C O2 2.8700 . . no H38A H20B 2.3400 . . no H38C H70C 2.4700 . 1_556 no H39A Si2 3.3900 . . no H39A C70 3.0800 . 1_556 no H39B H84 2.5700 . 2_546 no H40B H60B 2.3900 . 2_546 no H41 H43B 2.5400 . . no H41 H45B 2.5300 . . no H42 Si4 3.4600 . . no H42 H44B 2.4700 . . no H42 H46A 2.4800 . . no H42 H77C 2.4600 . . no H43A H47 2.3300 . . no H43A C47 2.8600 . . no H43B H47 2.2100 . . no H43B C64 3.0400 . 2_555 no H43B H74B 2.5400 . 2_555 no H43B H41 2.5400 . . no H43B C47 2.8300 . . no H44A C62 2.8700 . 2_555 no H44A C59 3.0900 . 1_565 no H44A H59C 2.4600 . 1_565 no H44B H42 2.4700 . . no H45A C74 3.0900 . 1_565 no H45A H74B 2.5700 . 1_565 no H45B H41 2.5300 . . no H45B C49 3.0900 . 2_555 no H45B Sc2 3.1600 . 2_555 no H45B O4 2.7400 . 2_555 no H46A H42 2.4800 . . no H46B H62 2.0600 . . no H46B C62 2.7100 . . no H47 C43 2.4500 . . no H47 H43A 2.3300 . . no H47 H43B 2.2100 . . no H47 H53 2.3200 . . no H51 C57 2.8800 . . no H51 H57C 2.3200 . . no H51 C61 2.4600 . . no H51 H55C 2.2100 . . no H51 C55 2.8000 . . no H51 H61A 2.2000 . . no H51 H61B 2.2800 . . no H53 H56B 2.4300 . . no H53 C56 2.5100 . . no H53 H56A 2.1100 . . no H53 H47 2.3200 . . no H55A H56C 2.5300 . . no H55A H57B 2.4500 . . no H55A H75C 2.3500 . 1_455 no H55B H82 2.4700 . 2_556 no H55B H56B 2.4100 . . no H55C H57C 2.4200 . . no H55C C51 2.7000 . . no H55C H51 2.2100 . . no H56A C53 2.6300 . . no H56A H53 2.1100 . . no H56A H57A 2.5400 . . no H56A H76B 2.5400 . 2_555 no H56B H55B 2.4100 . . no H56B C53 2.9100 . . no H56B H53 2.4300 . . no H56C H57B 2.3400 . . no H56C H55A 2.5300 . . no H57A H72B 2.5800 . 1_455 no H57A H56A 2.5400 . . no H57B H55A 2.4500 . . no H57B H56C 2.3400 . . no H57B H76A 2.5500 . 1_455 no H57C H51 2.3200 . . no H57C C51 2.7300 . . no H57C H55C 2.4200 . . no H57C H71B 2.4700 . 2_545 no H59A H60A 2.4200 . . no H59A H61C 2.4600 . . no H59B H74C 2.2200 . . no H59B O4 2.3400 . . no H59B C49 2.7900 . . no H59B C74 2.9900 . . no H59C C62 3.1000 . 2_545 no H59C H62 2.5400 . 2_545 no H59C H61A 2.4400 . . no H59C H44A 2.4600 . 1_545 no H60A H59A 2.4200 . . no H60A H61C 2.4600 . . no H60B C40 3.0900 . 2_556 no H60B H61B 2.4400 . . no H60B H40B 2.3900 . 2_556 no H60C O4 2.3400 . . no H60C C49 2.7300 . . no H61A H71C 2.5500 . 2_545 no H61A C51 2.7800 . . no H61A H51 2.2000 . . no H61A H59C 2.4400 . . no H61B H51 2.2800 . . no H61B H60B 2.4400 . . no H61B C51 2.7900 . . no H61C H59A 2.4600 . . no H61C H60A 2.4600 . . no H62 H68 2.2800 . . no H62 C46 2.5800 . . no H62 H46B 2.0600 . . no H62 H59C 2.5400 . 2_555 no H66 C70 2.8300 . . no H66 C72 2.8200 . . no H66 H76B 2.1600 . . no H66 C76 2.4200 . . no H66 H70B 2.2300 . . no H66 H72A 2.3200 . . no H66 H76A 2.2300 . . no H68 H71C 2.2500 . . no H68 C71 2.4900 . . no H68 H71B 2.2700 . . no H68 H62 2.2800 . . no H70A H71C 2.4900 . . no H70B H72A 2.1500 . . no H70B C66 2.6700 . . no H70B H66 2.2300 . . no H70C H38C 2.4700 . 1_554 no H70C H71A 2.4100 . . no H70C H72C 2.4100 . . no H71A H70C 2.4100 . . no H71A H72C 2.3900 . . no H71B H57C 2.4700 . 2_555 no H71B C68 2.7600 . . no H71B H68 2.2700 . . no H71C H68 2.2500 . . no H71C H70A 2.4900 . . no H71C H61A 2.5500 . 2_555 no H71C C68 2.7800 . . no H72A H70B 2.1500 . . no H72A C66 2.8200 . . no H72A H66 2.3200 . . no H72B H57A 2.5800 . 1_655 no H72C H70C 2.4100 . . no H72C H71A 2.3900 . . no H74A H75A 2.4600 . . no H74A H76C 2.4400 . . no H74B H43B 2.5400 . 2_545 no H74B H45A 2.5700 . 1_545 no H74B H76B 2.4300 . . no H74B C47 3.0500 . 2_545 no H74C C64 2.7900 . . no H74C H59B 2.2200 . . no H74C C59 3.0000 . . no H74C O3 2.4000 . . no H74C H75B 2.5700 . . no H75A H76C 2.4500 . . no H75A H74A 2.4600 . . no H75B O3 2.3200 . . no H75B C64 2.7700 . . no H75B H74C 2.5700 . . no H75B H79C 2.5000 . . no H75C H55A 2.3500 . 1_655 no H75C H76A 2.4700 . . no H76A H66 2.2300 . . no H76A C66 2.7600 . . no H76A H75C 2.4700 . . no H76A H57B 2.5500 . 1_655 no H76B C66 2.7300 . . no H76B H66 2.1600 . . no H76B H74B 2.4300 . . no H76B H56A 2.5400 . 2_545 no H76C H75A 2.4500 . . no H76C H74A 2.4400 . . no H77C H42 2.4600 . . no H78A C17 2.9800 . . no H79C H75B 2.5000 . . no H80A Sc2 3.3600 . . no H80A C64 3.0500 . . no H81 O1 2.8600 . . no H81 C23 3.0100 . . no H81 C24 2.9200 . . no H82 H55B 2.4700 . 2_546 no H84 O4 2.8000 . . no H84 N5 2.8900 . . no H84 C47 3.0600 . . no H84 C49 2.9700 . . no H84 H39B 2.5700 . 2_556 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C20 H20B O2 0.9800 2.3700 3.022(5) 123.00 . yes C21 H21B O2 0.9800 2.2600 2.946(5) 126.00 . yes C34 H34A O1 0.9800 2.4500 3.107(6) 124.00 . yes C35 H35A O1 0.9800 2.3300 2.963(5) 122.00 . yes C59 H59B O4 0.9800 2.3400 3.002(6) 125.00 . yes C60 H60C O4 0.9800 2.3400 3.012(5) 125.00 . yes C74 H74C O3 0.9800 2.4000 3.047(6) 123.00 . yes C75 H75B O3 0.9800 2.3200 3.000(5) 125.00 . yes # End of Crystallographic Information File for Compound 9 # # # CIF-file generated for meec_g001_123 / compound 11 data_meec_g001_123 # compound 11 _database_code_depnum_ccdc_archive 'CCDC 284498' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; [N,N'-bis(3,5-di-tert.-butylsalicylidene)ethylene diamino](diphenyl-tert. -butylsiloxy)scandium(III) (Salen)Sc(OSitBuPh2) ; _chemical_name_common (Salen)Sc(OSitBuPh2) _chemical_melting_point ? _chemical_formula_moiety 'C48 H65 N2 O3 Sc Si' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C48 H65 N2 O3 Sc Si' _chemical_formula_weight 791.07 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.0560(2) _cell_length_b 14.0187(2) _cell_length_c 16.0392(3) _cell_angle_alpha 66.9842(6) _cell_angle_beta 75.4467(6) _cell_angle_gamma 67.8923(6) _cell_volume 2294.25(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123 _cell_measurement_reflns_used 7219 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 26.37 _cell_special_details ; ? ; _exptl_crystal_description rhomb _exptl_crystal_colour yellow _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.227 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Sortav (R.H. Blessing, 1995)' _exptl_absorpt_correction_T_min 0.932 _exptl_absorpt_correction_T_max 0.978 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD (Nonius)' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 30449 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.39 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 9285 # number of observed reflections (> n sig(I)) _reflns_number_gt 6036 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_data_reduction 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_structure_solution 'SIR-92 (C. Giacovazzo, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. Electron density synthesis with coefficients Fo-Fc Highest peak 0.28 at 0.4635 0.6109 0.1791 [ 0.83 A from C43 ] Deepest hole -0.30 at 0.1549 0.5580 0.3130 [ 0.68 A from SC ] All hydrogen atoms were calculated in idealized geometry and refined using a riding group model. The atoms C1, C2 and N2 of the ethylene bridge are disordered over two positions (C49, C50, N3), pop. ratio: 0.62/0.38. The corresponding atoms were refined isotropically. A Total Potential Solvent Accessible Area Vol of 31.2 Ang^3^ was found. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+1.2564P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9285 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.277 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.054 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Sc Sc Uani 0.18201(4) 0.50366(4) 0.33273(3) 1.000 0.0221(2) . . Si Si Uani 0.46564(6) 0.53217(5) 0.22686(5) 1.000 0.0243(2) . . O1 O Uani 0.14466(14) 0.40106(12) 0.29622(11) 1.000 0.0273(6) . . O2 O Uani 0.05098(14) 0.63917(13) 0.28661(11) 1.000 0.0288(6) . . O3 O Uani 0.33482(14) 0.52373(12) 0.27967(11) 1.000 0.0276(6) . . N1 N Uani 0.23053(19) 0.35565(17) 0.45409(13) 1.000 0.0310(8) . . N2 N Uiso 0.1228(3) 0.5504(3) 0.4589(3) 0.624(7) 0.0207(10) . . C1 C Uiso 0.2565(5) 0.3685(4) 0.5322(3) 0.624(7) 0.0274(12) . . C2 C Uiso 0.1514(4) 0.4647(3) 0.5472(3) 0.624(7) 0.0263(13) . . C3A C Uani 0.0715(2) 0.6592(2) 0.45227(19) 0.624(7) 0.0396(10) . . C4 C Uani 0.0128(2) 0.7489(2) 0.37823(17) 1.000 0.0278(8) . . C5 C Uani -0.0403(2) 0.8523(2) 0.38967(18) 1.000 0.0346(10) . . C6 C Uani -0.1038(3) 0.9406(2) 0.32498(19) 1.000 0.0386(10) . . C7 C Uani -0.1171(3) 0.9233(2) 0.24798(18) 1.000 0.0375(9) . . C8 C Uani -0.0680(2) 0.82490(19) 0.23174(17) 1.000 0.0281(8) . . C9 C Uani 0.0010(2) 0.73539(19) 0.29810(17) 1.000 0.0254(8) . . C10 C Uani -0.1653(3) 1.0544(2) 0.3342(2) 1.000 0.0492(13) . . C11 C Uani -0.1335(3) 1.0616(2) 0.4176(2) 1.000 0.0587(11) . . C12 C Uani -0.3024(3) 1.0800(2) 0.3430(2) 1.000 0.0561(13) . . C13 C Uani -0.1252(4) 1.1397(3) 0.2486(2) 1.000 0.0900(18) . . C14 C Uani -0.0877(2) 0.81075(19) 0.14663(17) 1.000 0.0302(8) . . C15 C Uani -0.1538(2) 0.7263(2) 0.17616(18) 1.000 0.0378(10) . . C16 C Uani 0.0334(2) 0.7753(2) 0.08969(18) 1.000 0.0403(10) . . C17 C Uani -0.1653(3) 0.9172(2) 0.0851(2) 1.000 0.0540(11) . . C18 C Uani 0.2616(2) 0.2567(2) 0.45494(17) 1.000 0.0320(9) . . C19 C Uani 0.2573(2) 0.22337(19) 0.38144(16) 1.000 0.0273(8) . . C20 C Uani 0.3157(2) 0.1130(2) 0.38848(18) 1.000 0.0321(8) . . C21 C Uani 0.3157(2) 0.0726(2) 0.32298(17) 1.000 0.0319(8) . . C22 C Uani 0.2518(2) 0.1472(2) 0.24863(17) 1.000 0.0298(9) . . C23 C Uani 0.1925(2) 0.25680(19) 0.23673(16) 1.000 0.0254(8) . . C24 C Uani 0.1966(2) 0.29665(19) 0.30422(16) 1.000 0.0245(8) . . C25 C Uani 0.3787(2) -0.0464(2) 0.32675(19) 1.000 0.0399(9) . . C26 C Uani 0.4480(3) -0.1136(2) 0.4099(2) 1.000 0.0529(11) . . C27 C Uani 0.2843(3) -0.0983(2) 0.3323(2) 1.000 0.0488(11) . . C28 C Uani 0.4698(3) -0.0502(2) 0.2408(2) 1.000 0.0546(11) . . C29 C Uani 0.1279(2) 0.3341(2) 0.15257(17) 1.000 0.0291(8) . . C30 C Uani -0.0054(2) 0.3890(2) 0.18134(18) 1.000 0.0356(9) . . C31 C Uani 0.1898(2) 0.4217(2) 0.09691(18) 1.000 0.0399(10) . . C32 C Uani 0.1309(3) 0.2746(2) 0.08934(18) 1.000 0.0409(10) . . C33 C Uani 0.5681(2) 0.4947(2) 0.31435(18) 1.000 0.0305(9) . . C34 C Uani 0.6971(3) 0.4919(3) 0.2692(2) 1.000 0.0666(13) . . C35 C Uani 0.5180(3) 0.5782(2) 0.36487(19) 1.000 0.0442(11) . . C36 C Uani 0.5710(3) 0.3819(2) 0.3830(2) 1.000 0.0470(11) . . C37 C Uani 0.5286(2) 0.43366(19) 0.16187(16) 1.000 0.0272(8) . . C38 C Uani 0.4866(2) 0.34512(19) 0.18818(18) 1.000 0.0319(9) . . C39 C Uani 0.5314(3) 0.2691(2) 0.1437(2) 1.000 0.0392(10) . . C40 C Uani 0.6202(3) 0.2784(2) 0.0720(2) 1.000 0.0484(11) . . C41 C Uani 0.6647(4) 0.3640(3) 0.0440(2) 1.000 0.0748(14) . . C42 C Uani 0.6183(3) 0.4407(2) 0.0889(2) 1.000 0.0647(14) . . C43 C Uani 0.4470(2) 0.6779(2) 0.15132(17) 1.000 0.0295(9) . . C44 C Uani 0.3340(2) 0.7557(2) 0.15568(17) 1.000 0.0311(9) . . C45 C Uani 0.3147(3) 0.8649(2) 0.10308(18) 1.000 0.0368(9) . . C46 C Uani 0.4087(3) 0.8985(2) 0.04509(19) 1.000 0.0400(10) . . C47 C Uani 0.5211(3) 0.8241(2) 0.0394(2) 1.000 0.0439(11) . . C48 C Uani 0.5400(3) 0.7153(2) 0.09192(19) 1.000 0.0399(10) . . C3B C Uani 0.0715(2) 0.6592(2) 0.45227(19) 0.376(7) 0.0396(10) . . C49 C Uiso 0.2057(8) 0.3877(6) 0.5412(5) 0.376(7) 0.0217(19) . . N3 N Uiso 0.1441(6) 0.5800(5) 0.4412(4) 0.376(7) 0.0198(16) . . C50 C Uiso 0.2111(6) 0.5033(5) 0.5173(4) 0.376(7) 0.025(2) . . H1A H Uiso 0.33390 0.38410 0.51870 0.624(7) 0.0330 calc R H1B H Uiso 0.26020 0.30210 0.58650 0.624(7) 0.0330 calc R H7 H Uiso -0.16320 0.98380 0.20380 1.000 0.0450 calc R H11A H Uiso -0.16190 1.01030 0.47320 1.000 0.0880 calc R H11B H Uiso -0.17240 1.13600 0.41990 1.000 0.0880 calc R H11C H Uiso -0.04580 1.04330 0.41320 1.000 0.0880 calc R H12A H Uiso -0.32350 1.07700 0.28910 1.000 0.0840 calc R H12B H Uiso -0.34290 1.15310 0.34770 1.000 0.0840 calc R H12C H Uiso -0.32820 1.02610 0.39790 1.000 0.0840 calc R H13A H Uiso -0.03760 1.12320 0.24260 1.000 0.1350 calc R H13B H Uiso -0.16540 1.21240 0.25420 1.000 0.1350 calc R H13C H Uiso -0.14710 1.13780 0.19450 1.000 0.1350 calc R H15A H Uiso -0.10420 0.65580 0.21310 1.000 0.0570 calc R H15B H Uiso -0.16850 0.71890 0.12200 1.000 0.0570 calc R H15C H Uiso -0.23090 0.75020 0.21240 1.000 0.0570 calc R H16A H Uiso 0.08830 0.71090 0.12870 1.000 0.0610 calc R H16B H Uiso 0.06890 0.83480 0.06370 1.000 0.0610 calc R H16C H Uiso 0.02060 0.75740 0.04030 1.000 0.0610 calc R H17A H Uiso -0.17410 0.90580 0.03090 1.000 0.0810 calc R H17B H Uiso -0.12650 0.97380 0.06640 1.000 0.0810 calc R H17C H Uiso -0.24500 0.94030 0.11870 1.000 0.0810 calc R H18 H Uiso 0.28990 0.20040 0.50900 1.000 0.0380 calc R H20 H Uiso 0.35640 0.06490 0.44020 1.000 0.0390 calc R H22 H Uiso 0.24930 0.12030 0.20340 1.000 0.0360 calc R H26A H Uiso 0.51280 -0.08480 0.40490 1.000 0.0790 calc R H26B H Uiso 0.48270 -0.18990 0.41220 1.000 0.0790 calc R H26C H Uiso 0.39280 -0.10900 0.46560 1.000 0.0790 calc R H27A H Uiso 0.22570 -0.09430 0.38660 1.000 0.0730 calc R H27B H Uiso 0.32440 -0.17480 0.33620 1.000 0.0730 calc R H27C H Uiso 0.24260 -0.05890 0.27760 1.000 0.0730 calc R H28A H Uiso 0.42770 -0.00770 0.18640 1.000 0.0820 calc R H28B H Uiso 0.50820 -0.12610 0.24230 1.000 0.0820 calc R H28C H Uiso 0.53150 -0.01930 0.23870 1.000 0.0820 calc R H30A H Uiso -0.04200 0.33310 0.22320 1.000 0.0530 calc R H30B H Uiso -0.04800 0.42960 0.12720 1.000 0.0530 calc R H30C H Uiso -0.01110 0.43930 0.21200 1.000 0.0530 calc R H31A H Uiso 0.18050 0.46740 0.13300 1.000 0.0600 calc R H31B H Uiso 0.15250 0.46720 0.04070 1.000 0.0600 calc R H31C H Uiso 0.27570 0.38650 0.08150 1.000 0.0600 calc R H32A H Uiso 0.21460 0.24450 0.06480 1.000 0.0610 calc R H32B H Uiso 0.08400 0.32600 0.03900 1.000 0.0610 calc R H32C H Uiso 0.09610 0.21520 0.12380 1.000 0.0610 calc R H34A H Uiso 0.75180 0.45630 0.31620 1.000 0.1000 calc R H34B H Uiso 0.69950 0.56660 0.23600 1.000 0.1000 calc R H34C H Uiso 0.72220 0.45110 0.22650 1.000 0.1000 calc R H35A H Uiso 0.43510 0.58080 0.39260 1.000 0.0660 calc R H35B H Uiso 0.51880 0.65040 0.32160 1.000 0.0660 calc R H35C H Uiso 0.56820 0.55670 0.41270 1.000 0.0660 calc R H36A H Uiso 0.60730 0.32750 0.35190 1.000 0.0710 calc R H36B H Uiso 0.48850 0.38170 0.40990 1.000 0.0710 calc R H36C H Uiso 0.61890 0.36420 0.43120 1.000 0.0710 calc R H38 H Uiso 0.42510 0.33670 0.23830 1.000 0.0380 calc R H39 H Uiso 0.50010 0.20990 0.16320 1.000 0.0470 calc R H40 H Uiso 0.65100 0.22580 0.04160 1.000 0.0580 calc R H41 H Uiso 0.72690 0.37110 -0.00580 1.000 0.0900 calc R H42 H Uiso 0.64950 0.50010 0.06850 1.000 0.0780 calc R H44 H Uiso 0.26860 0.73360 0.19560 1.000 0.0370 calc R H45 H Uiso 0.23680 0.91640 0.10710 1.000 0.0440 calc R H46 H Uiso 0.39560 0.97310 0.00910 1.000 0.0480 calc R H47 H Uiso 0.58600 0.84720 -0.00050 1.000 0.0530 calc R H48 H Uiso 0.61830 0.66470 0.08750 1.000 0.0480 calc R H2A H Uiso 0.08000 0.44050 0.57910 0.624(7) 0.0320 calc R H2B H Uiso 0.17220 0.49430 0.58600 0.624(7) 0.0320 calc R H3A H Uiso 0.07550 0.67690 0.50270 0.624(7) 0.0480 calc R H5 H Uiso -0.03180 0.86080 0.44340 1.000 0.0420 calc R H3B H Uiso 0.05070 0.66440 0.51190 0.376(7) 0.0480 calc R H49A H Uiso 0.12500 0.38400 0.57330 0.376(7) 0.0260 calc R H49B H Uiso 0.26630 0.33500 0.58290 0.376(7) 0.0260 calc R H50A H Uiso 0.17720 0.52760 0.57130 0.376(7) 0.0300 calc R H50B H Uiso 0.29630 0.50220 0.50140 0.376(7) 0.0300 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc 0.0206(3) 0.0235(3) 0.0221(3) -0.0100(2) -0.0018(2) -0.0048(2) Si 0.0267(4) 0.0253(4) 0.0232(4) -0.0101(3) 0.0023(3) -0.0119(3) O1 0.0322(10) 0.0245(9) 0.0266(10) -0.0077(8) -0.0091(8) -0.0076(8) O2 0.0286(10) 0.0298(9) 0.0267(10) -0.0152(8) -0.0074(8) 0.0010(8) O3 0.0253(10) 0.0280(9) 0.0273(10) -0.0061(8) -0.0018(8) -0.0101(7) N1 0.0413(14) 0.0387(13) 0.0206(12) -0.0055(10) -0.0045(10) -0.0245(11) C3A 0.0285(16) 0.0557(18) 0.0413(18) -0.0350(15) -0.0115(13) 0.0041(14) C4 0.0236(14) 0.0351(15) 0.0296(15) -0.0162(12) 0.0004(12) -0.0111(11) C5 0.0403(17) 0.0388(16) 0.0351(17) -0.0215(14) 0.0040(13) -0.0193(13) C6 0.0557(19) 0.0282(15) 0.0346(17) -0.0116(13) 0.0060(14) -0.0222(14) C7 0.0519(18) 0.0240(14) 0.0316(16) -0.0072(12) -0.0025(14) -0.0103(13) C8 0.0333(15) 0.0258(13) 0.0247(14) -0.0077(12) -0.0003(12) -0.0114(11) C9 0.0225(14) 0.0265(14) 0.0289(15) -0.0134(12) 0.0031(11) -0.0091(11) C10 0.082(3) 0.0248(15) 0.0422(19) -0.0144(14) 0.0044(17) -0.0222(16) C11 0.075(2) 0.0457(19) 0.073(2) -0.0400(18) 0.0021(19) -0.0234(17) C12 0.084(3) 0.0261(16) 0.051(2) -0.0186(15) -0.0190(18) 0.0034(16) C13 0.168(4) 0.0366(19) 0.065(3) -0.0202(19) 0.025(3) -0.053(2) C14 0.0351(16) 0.0258(14) 0.0252(14) -0.0067(12) -0.0075(12) -0.0041(11) C15 0.0378(17) 0.0433(16) 0.0366(17) -0.0133(14) -0.0095(13) -0.0141(13) C16 0.0426(18) 0.0520(18) 0.0261(16) -0.0146(14) -0.0003(13) -0.0152(14) C17 0.075(2) 0.0370(17) 0.0376(18) -0.0086(14) -0.0214(17) 0.0011(16) C18 0.0384(16) 0.0339(15) 0.0248(15) 0.0010(12) -0.0092(12) -0.0201(13) C19 0.0285(14) 0.0311(14) 0.0231(14) -0.0055(12) -0.0019(11) -0.0145(12) C20 0.0315(15) 0.0279(14) 0.0286(15) -0.0014(12) -0.0086(12) -0.0054(11) C21 0.0299(15) 0.0296(14) 0.0296(15) -0.0077(12) -0.0022(12) -0.0053(12) C22 0.0292(15) 0.0329(15) 0.0274(15) -0.0136(12) 0.0005(12) -0.0085(12) C23 0.0221(14) 0.0292(14) 0.0221(14) -0.0069(11) 0.0003(11) -0.0087(11) C24 0.0225(13) 0.0253(13) 0.0243(14) -0.0067(11) -0.0002(11) -0.0093(11) C25 0.0389(17) 0.0297(15) 0.0393(17) -0.0125(13) -0.0025(14) 0.0015(13) C26 0.054(2) 0.0312(16) 0.054(2) -0.0069(15) -0.0173(17) 0.0070(14) C27 0.056(2) 0.0303(16) 0.057(2) -0.0183(15) -0.0050(16) -0.0072(14) C28 0.051(2) 0.0404(18) 0.054(2) -0.0199(16) 0.0037(16) 0.0035(15) C29 0.0278(15) 0.0332(14) 0.0252(14) -0.0100(12) -0.0050(12) -0.0070(11) C30 0.0289(15) 0.0404(16) 0.0395(17) -0.0170(14) -0.0098(13) -0.0053(12) C31 0.0427(18) 0.0429(17) 0.0273(16) -0.0003(13) -0.0078(13) -0.0157(14) C32 0.0447(18) 0.0467(17) 0.0314(16) -0.0179(14) -0.0095(14) -0.0062(14) C33 0.0254(14) 0.0362(15) 0.0353(16) -0.0214(13) -0.0008(12) -0.0073(12) C34 0.0344(18) 0.122(3) 0.072(2) -0.060(2) 0.0035(17) -0.032(2) C35 0.059(2) 0.0405(17) 0.0430(18) -0.0224(15) -0.0130(15) -0.0127(15) C36 0.054(2) 0.0358(16) 0.0497(19) -0.0174(15) -0.0243(16) 0.0026(14) C37 0.0354(15) 0.0271(13) 0.0219(14) -0.0092(11) 0.0013(12) -0.0147(12) C38 0.0333(15) 0.0296(14) 0.0367(16) -0.0123(13) -0.0020(13) -0.0140(12) C39 0.0518(19) 0.0262(14) 0.0473(19) -0.0123(14) -0.0120(16) -0.0164(13) C40 0.082(2) 0.0349(17) 0.0342(18) -0.0194(14) -0.0015(17) -0.0199(16) C41 0.123(3) 0.059(2) 0.050(2) -0.0371(19) 0.048(2) -0.054(2) C42 0.108(3) 0.050(2) 0.050(2) -0.0330(17) 0.040(2) -0.054(2) C43 0.0398(16) 0.0303(14) 0.0258(15) -0.0148(12) 0.0023(12) -0.0172(13) C44 0.0391(16) 0.0321(15) 0.0272(15) -0.0088(12) -0.0052(12) -0.0170(13) C45 0.0426(17) 0.0309(15) 0.0400(17) -0.0103(13) -0.0157(14) -0.0095(13) C46 0.063(2) 0.0270(15) 0.0370(17) -0.0061(13) -0.0108(16) -0.0233(15) C47 0.057(2) 0.0315(16) 0.0460(19) -0.0129(14) 0.0085(15) -0.0263(15) C48 0.0429(17) 0.0298(15) 0.0474(18) -0.0191(14) 0.0122(14) -0.0166(13) C3B 0.0285(16) 0.0557(18) 0.0413(18) -0.0350(15) -0.0115(13) 0.0041(14) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 O1 1.9731(18) . . yes Sc O2 1.9700(19) . . yes Sc O3 1.9006(19) . . yes Sc N1 2.222(2) . . yes Sc N2 2.234(4) . . yes Sc N3 2.251(6) . . yes Si O3 1.615(2) . . yes Si C33 1.891(3) . . yes Si C37 1.873(3) . . yes Si C43 1.884(3) . . yes O1 C24 1.325(3) . . yes O2 C9 1.320(3) . . yes N1 C1 1.455(6) . . yes N1 C18 1.289(4) . . yes N1 C49 1.557(8) . . yes N2 C2 1.473(6) . . yes N2 C3A 1.384(5) . . yes N3 C3B 1.173(7) . . yes N3 C50 1.454(9) . . yes C1 C2 1.515(7) . . no C3A C4 1.441(4) . . no C3B C4 1.441(4) . . no C4 C5 1.412(4) . . no C4 C9 1.418(4) . . no C5 C6 1.370(4) . . no C6 C7 1.405(4) . . no C6 C10 1.535(4) . . no C7 C8 1.382(4) . . no C8 C9 1.419(4) . . no C8 C14 1.539(4) . . no C10 C12 1.535(5) . . no C10 C11 1.529(4) . . no C10 C13 1.538(5) . . no C14 C15 1.531(4) . . no C14 C16 1.533(4) . . no C14 C17 1.529(4) . . no C18 C19 1.446(4) . . no C19 C20 1.409(4) . . no C19 C24 1.421(3) . . no C20 C21 1.375(4) . . no C21 C22 1.410(4) . . no C21 C25 1.534(4) . . no C22 C23 1.386(4) . . no C23 C24 1.417(4) . . no C23 C29 1.534(4) . . no C25 C28 1.537(4) . . no C25 C26 1.533(4) . . no C25 C27 1.534(5) . . no C29 C30 1.537(4) . . no C29 C31 1.536(4) . . no C29 C32 1.532(4) . . no C33 C36 1.527(4) . . no C33 C34 1.535(5) . . no C33 C35 1.535(4) . . no C37 C42 1.379(4) . . no C37 C38 1.390(4) . . no C38 C39 1.380(4) . . no C39 C40 1.362(5) . . no C40 C41 1.368(6) . . no C41 C42 1.392(5) . . no C43 C48 1.398(4) . . no C43 C44 1.394(4) . . no C44 C45 1.389(4) . . no C45 C46 1.379(5) . . no C46 C47 1.371(5) . . no C47 C48 1.385(4) . . no C49 C50 1.536(11) . . no C1 H1A 0.9902 . . no C1 H1B 0.9906 . . no C2 H2A 0.9902 . . no C2 H2B 0.9905 . . no C3A H3A 0.9506 . . no C3B H3B 0.9503 . . no C5 H5 0.9493 . . no C7 H7 0.9505 . . no C11 H11A 0.9798 . . no C11 H11B 0.9810 . . no C11 H11C 0.9804 . . no C12 H12A 0.9802 . . no C12 H12B 0.9796 . . no C12 H12C 0.9808 . . no C13 H13B 0.9796 . . no C13 H13C 0.9807 . . no C13 H13A 0.9801 . . no C15 H15B 0.9790 . . no C15 H15C 0.9800 . . no C15 H15A 0.9802 . . no C16 H16B 0.9797 . . no C16 H16C 0.9800 . . no C16 H16A 0.9804 . . no C17 H17A 0.9799 . . no C17 H17B 0.9804 . . no C17 H17C 0.9801 . . no C18 H18 0.9497 . . no C20 H20 0.9496 . . no C22 H22 0.9502 . . no C26 H26B 0.9801 . . no C26 H26C 0.9794 . . no C26 H26A 0.9800 . . no C27 H27B 0.9799 . . no C27 H27C 0.9804 . . no C27 H27A 0.9798 . . no C28 H28B 0.9807 . . no C28 H28C 0.9801 . . no C28 H28A 0.9810 . . no C30 H30B 0.9795 . . no C30 H30C 0.9805 . . no C30 H30A 0.9796 . . no C31 H31B 0.9798 . . no C31 H31C 0.9794 . . no C31 H31A 0.9805 . . no C32 H32B 0.9791 . . no C32 H32C 0.9805 . . no C32 H32A 0.9803 . . no C34 H34A 0.9799 . . no C34 H34C 0.9796 . . no C34 H34B 0.9798 . . no C35 H35A 0.9797 . . no C35 H35C 0.9802 . . no C35 H35B 0.9803 . . no C36 H36B 0.9803 . . no C36 H36C 0.9794 . . no C36 H36A 0.9790 . . no C38 H38 0.9498 . . no C39 H39 0.9499 . . no C40 H40 0.9505 . . no C41 H41 0.9504 . . no C42 H42 0.9502 . . no C44 H44 0.9501 . . no C45 H45 0.9503 . . no C46 H46 0.9494 . . no C47 H47 0.9506 . . no C48 H48 0.9492 . . no C49 H49A 0.9898 . . no C49 H49B 0.9899 . . no C50 H50A 0.9906 . . no C50 H50B 0.9899 . . no 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 O1 Sc O2 101.24(8) . . . yes O1 Sc O3 114.27(8) . . . yes O1 Sc N1 80.94(8) . . . yes O1 Sc N2 131.87(12) . . . yes O1 Sc N3 145.01(19) . . . yes O2 Sc O3 110.55(8) . . . yes O2 Sc N1 142.86(8) . . . yes O2 Sc N2 81.92(12) . . . yes O2 Sc N3 78.53(18) . . . yes O3 Sc N1 101.73(8) . . . yes O3 Sc N2 108.96(12) . . . yes O3 Sc N3 97.9(2) . . . yes N1 Sc N2 70.36(12) . . . yes N1 Sc N3 79.33(17) . . . yes O3 Si C33 108.56(11) . . . yes O3 Si C37 108.60(11) . . . yes O3 Si C43 108.22(11) . . . yes C33 Si C37 109.65(12) . . . yes C33 Si C43 108.70(12) . . . yes C37 Si C43 113.01(11) . . . yes Sc O1 C24 133.94(17) . . . yes Sc O2 C9 137.93(17) . . . yes Sc O3 Si 172.90(11) . . . yes Sc N1 C1 117.7(2) . . . yes Sc N1 C18 125.04(17) . . . yes Sc N1 C49 110.5(3) . . . yes C1 N1 C18 115.7(3) . . . yes C18 N1 C49 124.0(3) . . . yes Sc N2 C2 118.6(3) . . . yes Sc N2 C3A 120.0(3) . . . yes C2 N2 C3A 121.1(4) . . . yes Sc N3 C50 109.8(5) . . . yes C3B N3 C50 116.8(5) . . . yes Sc N3 C3B 132.4(5) . . . yes N1 C1 C2 103.6(4) . . . yes N2 C2 C1 110.0(4) . . . yes N2 C3A C4 127.9(3) . . . yes N3 C3B C4 122.0(4) . . . yes C3B C4 C5 117.6(2) . . . no C3A C4 C5 117.6(2) . . . no C3A C4 C9 122.5(2) . . . no C3B C4 C9 122.5(2) . . . no C5 C4 C9 119.7(2) . . . no C4 C5 C6 121.5(2) . . . no C5 C6 C7 117.2(3) . . . no C5 C6 C10 123.9(3) . . . no C7 C6 C10 118.8(3) . . . no C6 C7 C8 124.8(3) . . . no C7 C8 C14 122.3(2) . . . no C9 C8 C14 120.6(2) . . . no C7 C8 C9 117.1(2) . . . no O2 C9 C4 120.1(2) . . . yes C4 C9 C8 119.7(2) . . . no O2 C9 C8 120.2(2) . . . yes C11 C10 C12 109.1(3) . . . no C11 C10 C13 108.3(3) . . . no C6 C10 C13 109.5(3) . . . no C6 C10 C11 112.1(3) . . . no C12 C10 C13 109.3(3) . . . no C6 C10 C12 108.5(3) . . . no C8 C14 C15 109.4(2) . . . no C8 C14 C16 110.4(2) . . . no C8 C14 C17 111.7(2) . . . no C15 C14 C16 110.5(2) . . . no C15 C14 C17 107.4(2) . . . no C16 C14 C17 107.4(2) . . . no N1 C18 C19 126.2(2) . . . yes C18 C19 C20 117.5(2) . . . no C18 C19 C24 122.8(2) . . . no C20 C19 C24 119.7(2) . . . no C19 C20 C21 122.2(2) . . . no C22 C21 C25 119.2(2) . . . no C20 C21 C22 116.4(2) . . . no C20 C21 C25 124.4(2) . . . no C21 C22 C23 124.8(2) . . . no C22 C23 C24 117.5(2) . . . no C22 C23 C29 122.0(2) . . . no C24 C23 C29 120.5(2) . . . no O1 C24 C19 119.7(2) . . . yes O1 C24 C23 120.9(2) . . . yes C19 C24 C23 119.4(2) . . . no C21 C25 C27 109.5(2) . . . no C21 C25 C28 109.5(2) . . . no C21 C25 C26 111.7(2) . . . no C27 C25 C28 109.9(2) . . . no C26 C25 C27 108.5(2) . . . no C26 C25 C28 107.8(2) . . . no C23 C29 C32 112.3(2) . . . no C31 C29 C32 107.4(2) . . . no C30 C29 C31 109.6(2) . . . no C30 C29 C32 107.2(2) . . . no C23 C29 C31 109.7(2) . . . no C23 C29 C30 110.5(2) . . . no C34 C33 C36 108.7(3) . . . no C35 C33 C36 109.0(2) . . . no Si C33 C36 108.9(2) . . . yes Si C33 C34 111.22(19) . . . yes Si C33 C35 109.2(2) . . . yes C34 C33 C35 109.7(3) . . . no Si C37 C38 119.70(19) . . . yes Si C37 C42 124.3(2) . . . yes C38 C37 C42 116.0(2) . . . no C37 C38 C39 122.0(3) . . . no C38 C39 C40 120.4(3) . . . no C39 C40 C41 119.5(3) . . . no C40 C41 C42 119.6(3) . . . no C37 C42 C41 122.4(3) . . . no Si C43 C44 118.7(2) . . . yes Si C43 C48 124.6(2) . . . yes C44 C43 C48 116.7(2) . . . no C43 C44 C45 121.6(3) . . . no C44 C45 C46 119.9(3) . . . no C45 C46 C47 120.0(3) . . . no C46 C47 C48 119.9(3) . . . no C43 C48 C47 121.9(3) . . . no N1 C49 C50 111.4(5) . . . yes N3 C50 C49 111.4(6) . . . yes N1 C1 H1A 111.07 . . . no N1 C1 H1B 111.10 . . . no C2 C1 H1A 111.03 . . . no C2 C1 H1B 111.03 . . . no H1A C1 H1B 108.96 . . . no N2 C2 H2A 109.64 . . . no N2 C2 H2B 109.63 . . . no C1 C2 H2A 109.63 . . . no C1 C2 H2B 109.67 . . . no H2A C2 H2B 108.21 . . . no N2 C3A H3A 116.03 . . . no C4 C3A H3A 116.05 . . . no C4 C3B H3B 118.98 . . . no N3 C3B H3B 118.99 . . . no C4 C5 H5 119.26 . . . no C6 C5 H5 119.25 . . . no C8 C7 H7 117.67 . . . no C6 C7 H7 117.52 . . . no C10 C11 H11C 109.47 . . . no H11A C11 H11B 109.39 . . . no H11A C11 H11C 109.47 . . . no H11B C11 H11C 109.44 . . . no C10 C11 H11A 109.58 . . . no C10 C11 H11B 109.48 . . . no C10 C12 H12A 109.47 . . . no H12A C12 H12B 109.52 . . . no H12A C12 H12C 109.50 . . . no H12B C12 H12C 109.49 . . . no C10 C12 H12B 109.44 . . . no C10 C12 H12C 109.41 . . . no C10 C13 H13C 109.45 . . . no C10 C13 H13A 109.47 . . . no C10 C13 H13B 109.44 . . . no H13B C13 H13C 109.49 . . . no H13A C13 H13B 109.46 . . . no H13A C13 H13C 109.52 . . . no C14 C15 H15A 109.44 . . . no H15A C15 H15B 109.53 . . . no C14 C15 H15B 109.43 . . . no C14 C15 H15C 109.43 . . . no H15B C15 H15C 109.57 . . . no H15A C15 H15C 109.43 . . . no C14 C16 H16C 109.52 . . . no H16A C16 H16B 109.40 . . . no C14 C16 H16B 109.49 . . . no H16B C16 H16C 109.50 . . . no H16A C16 H16C 109.40 . . . no C14 C16 H16A 109.51 . . . no C14 C17 H17A 109.52 . . . no H17A C17 H17B 109.50 . . . no H17A C17 H17C 109.57 . . . no H17B C17 H17C 109.40 . . . no C14 C17 H17C 109.40 . . . no C14 C17 H17B 109.45 . . . no C19 C18 H18 116.97 . . . no N1 C18 H18 116.87 . . . no C21 C20 H20 118.88 . . . no C19 C20 H20 118.92 . . . no C23 C22 H22 117.66 . . . no C21 C22 H22 117.56 . . . no C25 C26 H26A 109.46 . . . no H26A C26 H26B 109.51 . . . no C25 C26 H26B 109.37 . . . no C25 C26 H26C 109.46 . . . no H26B C26 H26C 109.56 . . . no H26A C26 H26C 109.47 . . . no C25 C27 H27B 109.44 . . . no C25 C27 H27A 109.41 . . . no H27A C27 H27C 109.51 . . . no C25 C27 H27C 109.48 . . . no H27A C27 H27B 109.53 . . . no H27B C27 H27C 109.45 . . . no C25 C28 H28C 109.58 . . . no H28A C28 H28B 109.35 . . . no H28A C28 H28C 109.47 . . . no H28B C28 H28C 109.51 . . . no C25 C28 H28B 109.46 . . . no C25 C28 H28A 109.46 . . . no C29 C30 H30C 109.47 . . . no C29 C30 H30A 109.41 . . . no C29 C30 H30B 109.49 . . . no H30B C30 H30C 109.45 . . . no H30A C30 H30B 109.51 . . . no H30A C30 H30C 109.50 . . . no C29 C31 H31A 109.49 . . . no H31A C31 H31B 109.43 . . . no C29 C31 H31B 109.41 . . . no C29 C31 H31C 109.51 . . . no H31B C31 H31C 109.47 . . . no H31A C31 H31C 109.52 . . . no C29 C32 H32B 109.44 . . . no C29 C32 H32C 109.49 . . . no H32A C32 H32C 109.48 . . . no H32B C32 H32C 109.50 . . . no H32A C32 H32B 109.47 . . . no C29 C32 H32A 109.45 . . . no C33 C34 H34C 109.41 . . . no H34A C34 H34B 109.51 . . . no H34A C34 H34C 109.55 . . . no H34B C34 H34C 109.43 . . . no C33 C34 H34A 109.49 . . . no C33 C34 H34B 109.44 . . . no C33 C35 H35A 109.51 . . . no H35A C35 H35B 109.50 . . . no H35A C35 H35C 109.43 . . . no H35B C35 H35C 109.48 . . . no C33 C35 H35B 109.46 . . . no C33 C35 H35C 109.45 . . . no C33 C36 H36A 109.48 . . . no H36A C36 H36B 109.44 . . . no C33 C36 H36B 109.41 . . . no C33 C36 H36C 109.48 . . . no H36B C36 H36C 109.54 . . . no H36A C36 H36C 109.48 . . . no C39 C38 H38 118.97 . . . no C37 C38 H38 118.98 . . . no C38 C39 H39 119.80 . . . no C40 C39 H39 119.78 . . . no C39 C40 H40 120.22 . . . no C41 C40 H40 120.24 . . . no C40 C41 H41 120.23 . . . no C42 C41 H41 120.17 . . . no C41 C42 H42 118.80 . . . no C37 C42 H42 118.81 . . . no C43 C44 H44 119.28 . . . no C45 C44 H44 119.15 . . . no C44 C45 H45 120.04 . . . no C46 C45 H45 120.03 . . . no C47 C46 H46 120.03 . . . no C45 C46 H46 120.00 . . . no C46 C47 H47 120.03 . . . no C48 C47 H47 120.03 . . . no C47 C48 H48 119.08 . . . no C43 C48 H48 119.07 . . . no N1 C49 H49A 109.35 . . . no N1 C49 H49B 109.36 . . . no C50 C49 H49A 109.33 . . . no C50 C49 H49B 109.34 . . . no H49A C49 H49B 108.02 . . . no N3 C50 H50A 109.41 . . . no N3 C50 H50B 109.39 . . . no C49 C50 H50A 109.34 . . . no C49 C50 H50B 109.34 . . . no H50A C50 H50B 107.90 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Sc O1 C24 178.7(2) . . . . no O3 Sc O1 C24 59.9(2) . . . . no N1 Sc O1 C24 -39.0(2) . . . . no N2 Sc O1 C24 -92.1(3) . . . . no O1 Sc O2 C9 164.1(2) . . . . no O3 Sc O2 C9 -74.4(2) . . . . no N1 Sc O2 C9 74.3(3) . . . . no N2 Sc O2 C9 32.9(3) . . . . no O1 Sc N1 C1 -170.7(3) . . . . no O1 Sc N1 C18 24.3(2) . . . . no O2 Sc N1 C1 -74.0(3) . . . . no O2 Sc N1 C18 121.0(2) . . . . no O3 Sc N1 C1 76.2(3) . . . . no O3 Sc N1 C18 -88.8(2) . . . . no N2 Sc N1 C1 -29.9(3) . . . . no N2 Sc N1 C18 165.1(3) . . . . no O1 Sc N2 C2 59.8(4) . . . . no O1 Sc N2 C3A -126.6(3) . . . . no O2 Sc N2 C2 157.7(3) . . . . no O2 Sc N2 C3A -28.8(3) . . . . no O3 Sc N2 C2 -93.3(3) . . . . no O3 Sc N2 C3A 80.3(3) . . . . no N1 Sc N2 C2 2.8(3) . . . . no N1 Sc N2 C3A 176.3(3) . . . . no O3 Si C33 C34 175.3(2) . . . . no O3 Si C33 C35 -63.4(2) . . . . no O3 Si C33 C36 55.5(2) . . . . no C37 Si C33 C34 56.8(2) . . . . no C37 Si C33 C35 178.06(19) . . . . no C37 Si C33 C36 -63.0(2) . . . . no C43 Si C33 C34 -67.2(2) . . . . no C43 Si C33 C35 54.1(2) . . . . no C43 Si C33 C36 172.99(19) . . . . no O3 Si C37 C38 -22.2(2) . . . . no O3 Si C37 C42 159.5(2) . . . . no C33 Si C37 C38 96.3(2) . . . . no C33 Si C37 C42 -82.1(3) . . . . no C43 Si C37 C38 -142.3(2) . . . . no C43 Si C37 C42 39.4(3) . . . . no O3 Si C43 C44 4.9(2) . . . . no O3 Si C43 C48 -176.9(2) . . . . no C33 Si C43 C44 -112.8(2) . . . . no C33 Si C43 C48 65.4(3) . . . . no C37 Si C43 C44 125.2(2) . . . . no C37 Si C43 C48 -56.6(3) . . . . no Sc O1 C24 C19 32.8(3) . . . . no Sc O1 C24 C23 -147.2(2) . . . . no Sc O2 C9 C4 -21.8(4) . . . . no Sc O2 C9 C8 160.27(19) . . . . no Sc N1 C1 C2 48.9(4) . . . . no C18 N1 C1 C2 -144.7(3) . . . . no Sc N1 C18 C19 -7.7(4) . . . . no C1 N1 C18 C19 -173.0(3) . . . . no Sc N2 C2 C1 21.7(5) . . . . no C3A N2 C2 C1 -151.7(4) . . . . no Sc N2 C3A C4 22.5(5) . . . . no C2 N2 C3A C4 -164.2(4) . . . . no N1 C1 C2 N2 -42.1(5) . . . . no N2 C3A C4 C5 175.7(3) . . . . no N2 C3A C4 C9 -0.6(5) . . . . no C9 C4 C5 C6 0.2(4) . . . . no C3A C4 C9 O2 -4.1(4) . . . . no C3A C4 C5 C6 -176.2(3) . . . . no C3A C4 C9 C8 173.8(3) . . . . no C5 C4 C9 O2 179.6(2) . . . . no C5 C4 C9 C8 -2.4(4) . . . . no C4 C5 C6 C10 178.9(3) . . . . no C4 C5 C6 C7 1.9(5) . . . . no C10 C6 C7 C8 -179.2(3) . . . . no C5 C6 C10 C11 7.6(5) . . . . no C5 C6 C7 C8 -2.0(5) . . . . no C7 C6 C10 C11 -175.4(3) . . . . no C7 C6 C10 C12 64.1(4) . . . . no C7 C6 C10 C13 -55.2(5) . . . . no C5 C6 C10 C13 127.8(4) . . . . no C5 C6 C10 C12 -112.9(4) . . . . no C6 C7 C8 C14 178.9(3) . . . . no C6 C7 C8 C9 -0.2(5) . . . . no C7 C8 C14 C16 119.9(3) . . . . no C7 C8 C14 C17 0.5(4) . . . . no C9 C8 C14 C15 60.8(3) . . . . no C9 C8 C14 C16 -61.1(3) . . . . no C9 C8 C14 C17 179.5(3) . . . . no C7 C8 C9 O2 -179.7(3) . . . . no C7 C8 C9 C4 2.4(4) . . . . no C14 C8 C9 O2 1.2(4) . . . . no C14 C8 C9 C4 -176.8(2) . . . . no C7 C8 C14 C15 -118.3(3) . . . . no N1 C18 C19 C20 168.4(3) . . . . no N1 C18 C19 C24 -12.0(4) . . . . no C20 C19 C24 O1 -178.0(2) . . . . no C18 C19 C24 O1 2.4(4) . . . . no C18 C19 C24 C23 -177.6(2) . . . . no C18 C19 C20 C21 179.1(3) . . . . no C24 C19 C20 C21 -0.4(4) . . . . no C20 C19 C24 C23 2.0(4) . . . . no C19 C20 C21 C22 -1.2(4) . . . . no C19 C20 C21 C25 179.4(3) . . . . no C20 C21 C25 C26 -3.3(4) . . . . no C20 C21 C25 C27 116.9(3) . . . . no C20 C21 C25 C28 -122.5(3) . . . . no C20 C21 C22 C23 1.4(4) . . . . no C25 C21 C22 C23 -179.2(3) . . . . no C22 C21 C25 C28 58.1(3) . . . . no C22 C21 C25 C26 177.4(3) . . . . no C22 C21 C25 C27 -62.4(3) . . . . no C21 C22 C23 C24 0.1(4) . . . . no C21 C22 C23 C29 178.1(2) . . . . no C24 C23 C29 C32 -178.5(3) . . . . no C22 C23 C24 C19 -1.8(4) . . . . no C24 C23 C29 C30 -58.9(3) . . . . no C24 C23 C29 C31 62.1(3) . . . . no C22 C23 C24 O1 178.2(2) . . . . no C22 C23 C29 C30 123.2(3) . . . . no C29 C23 C24 O1 0.2(4) . . . . no C29 C23 C24 C19 -179.8(2) . . . . no C22 C23 C29 C31 -115.9(3) . . . . no C22 C23 C29 C32 3.5(4) . . . . no Si C37 C38 C39 -178.8(2) . . . . no C42 C37 C38 C39 -0.4(4) . . . . no Si C37 C42 C41 178.3(3) . . . . no C38 C37 C42 C41 -0.1(5) . . . . no C37 C38 C39 C40 0.5(5) . . . . no C38 C39 C40 C41 -0.2(5) . . . . no C39 C40 C41 C42 -0.3(6) . . . . no C40 C41 C42 C37 0.4(6) . . . . no Si C43 C44 C45 178.8(2) . . . . no C48 C43 C44 C45 0.4(4) . . . . no Si C43 C48 C47 -178.7(2) . . . . no C44 C43 C48 C47 -0.4(4) . . . . no C43 C44 C45 C46 -0.2(4) . . . . no C44 C45 C46 C47 0.0(5) . . . . no C45 C46 C47 C48 0.0(5) . . . . no C46 C47 C48 C43 0.2(5) . . . . no 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 Sc C2 3.937(5) . 2_566 no Sc H16A 3.5184 . . no Sc H38 3.4263 . . no Sc H44 3.4861 . . no Sc H31A 3.4396 . . no Sc H2A 3.0578 . 2_566 no Sc H49A 3.6217 . 2_566 no O1 C30 2.974(3) . . no O1 C31 3.020(3) . . no O2 C16 2.997(3) . . no O2 C15 2.994(3) . . no O2 C2 3.398(5) . 2_566 no O1 H31A 2.3948 . . no O1 H30C 2.3642 . . no O2 H15A 2.3473 . . no O2 H16A 2.3248 . . no O2 H2A 2.4733 . 2_566 no O2 H49A 2.6847 . 2_566 no O3 H35A 2.8886 . . no O3 H36B 2.7706 . . no O3 H38 2.7109 . . no O3 H44 2.6043 . . no N2 C2 3.419(7) . 2_566 no N2 H2A 2.6113 . 2_566 no C2 N2 3.419(7) . 2_566 no C2 Sc 3.937(5) . 2_566 no C2 O2 3.398(5) . 2_566 no C4 C49 3.525(10) . 2_566 no C5 C18 3.523(4) . 2_566 no C9 C49 3.516(9) . 2_566 no C15 O2 2.994(3) . . no C16 O2 2.997(3) . . no C17 C46 3.578(5) . 2_575 no C18 C5 3.523(4) . 2_566 no C30 C34 3.476(5) . 1_455 no C30 O1 2.974(3) . . no C31 O1 3.020(3) . . no C34 C30 3.476(5) . 1_655 no C34 C48 3.572(5) . . no C40 C48 3.591(5) . 2_665 no C46 C17 3.578(5) . 2_575 no C48 C34 3.572(5) . . no C48 C40 3.591(5) . 2_665 no C49 C3A 3.379(9) . . no C49 C4 3.525(10) . 2_566 no C49 C9 3.516(9) . 2_566 no C50 C3A 2.242(7) . . no C1 H36B 3.0089 . . no C3A H2A 2.9113 . 2_566 no C3B H49A 2.8124 . 2_566 no C4 H2A 3.0332 . 2_566 no C4 H49A 2.7173 . 2_566 no C5 H11C 2.8214 . . no C5 H11A 2.7820 . . no C7 H13C 2.6887 . . no C7 H17B 2.7367 . . no C7 H17C 2.7709 . . no C7 H12A 2.7423 . . no C9 H49A 2.6463 . 2_566 no C9 H16A 2.7619 . . no C9 H15A 2.7992 . . no C9 H2A 2.8215 . 2_566 no C11 H5 2.5189 . . no C12 H7 2.8962 . . no C13 H7 2.7658 . . no C13 H30A 3.0823 . 1_565 no C15 H34B 3.0836 . 1_455 no C17 H7 2.4349 . . no C17 H46 3.0715 . 2_575 no C19 H38 3.0200 . . no C20 H26C 2.7331 . . no C20 H11A 2.9486 . 2_566 no C20 H26A 2.8616 . . no C22 H28A 2.7155 . . no C22 H27C 2.7824 . . no C22 H32C 2.7369 . . no C22 H32A 2.7954 . . no C24 H38 2.8737 . . no C24 H31A 2.8438 . . no C24 H30C 2.8699 . . no C26 H20 2.5137 . . no C27 H22 2.8904 . . no C28 H22 2.8350 . . no C30 H34C 3.0353 . 1_455 no C31 H42 2.9555 . 2_665 no C32 H22 2.4407 . . no C34 H48 3.0664 . . no C35 H50B 3.0833 . 2_666 no C37 H36A 3.0411 . . no C37 H34C 2.9027 . . no C39 H12A 3.0569 . 1_645 no C42 H34C 2.8705 . . no C43 H35B 2.9105 . . no C44 H40 3.0362 . 2_665 no C45 H40 2.9329 . 2_665 no C46 H40 2.9714 . 2_665 no C48 H42 2.9367 . . no C48 H34B 2.9720 . . no C50 H35C 2.8506 . 2_666 no H1A H36B 2.2101 . . no H1A H35C 2.3230 . 2_666 no H1B H18 2.1175 . . no H2A C3A 2.9113 . 2_566 no H2A Sc 3.0578 . 2_566 no H2A O2 2.4733 . 2_566 no H2A N2 2.6113 . 2_566 no H2A C9 2.8215 . 2_566 no H2A C4 3.0332 . 2_566 no H2B H3A 2.3578 . . no H2B H34A 2.4144 . 2_666 no H3A H5 2.3270 . . no H3A H2B 2.3578 . . no H3B H50A 2.0028 . . no H3B H5 2.4289 . . no H5 C11 2.5189 . . no H5 H11A 2.2390 . . no H5 H11C 2.3570 . . no H5 H3B 2.4289 . . no H5 H3A 2.3270 . . no H7 C12 2.8962 . . no H7 C17 2.4349 . . no H7 H12A 2.3414 . . no H7 C13 2.7658 . . no H7 H17C 2.2333 . . no H7 H13C 2.1840 . . no H7 H17B 2.1856 . . no H11A C20 2.9486 . 2_566 no H11A C5 2.7820 . . no H11A H5 2.2390 . . no H11A H12C 2.4902 . . no H11B H13B 2.4387 . . no H11B H12B 2.4964 . . no H11C H5 2.3570 . . no H11C H13A 2.5105 . . no H11C C5 2.8214 . . no H12A C7 2.7423 . . no H12A H7 2.3414 . . no H12A H13C 2.5066 . . no H12A C39 3.0569 . 1_465 no H12B H11B 2.4964 . . no H12B H13B 2.5041 . . no H12B H36A 2.3121 . 1_465 no H12C H11A 2.4902 . . no H12C H20 2.4038 . 2_566 no H13A H11C 2.5105 . . no H13A H32C 2.4478 . 1_565 no H13B H12B 2.5041 . . no H13B H30A 2.4877 . 1_565 no H13B H11B 2.4387 . . no H13C C7 2.6887 . . no H13C H7 2.1840 . . no H13C H12A 2.5066 . . no H15A O2 2.3473 . . no H15A C9 2.7992 . . no H15B H16C 2.4653 . . no H15B H17A 2.4346 . . no H15C H17C 2.4587 . . no H16A C9 2.7619 . . no H16A O2 2.3248 . . no H16A Sc 3.5184 . . no H16B H17B 2.4306 . . no H16C H17A 2.4734 . . no H16C H15B 2.4653 . . no H17A H16C 2.4734 . . no H17A H15B 2.4346 . . no H17B H7 2.1856 . . no H17B H16B 2.4306 . . no H17B C7 2.7367 . . no H17C C7 2.7709 . . no H17C H15C 2.4587 . . no H17C H7 2.2333 . . no H18 H1B 2.1175 . . no H18 H20 2.3488 . . no H18 H49B 2.4943 . . no H20 C26 2.5137 . . no H20 H18 2.3488 . . no H20 H26A 2.3862 . . no H20 H26C 2.1931 . . no H20 H12C 2.4038 . 2_566 no H22 C28 2.8350 . . no H22 C32 2.4407 . . no H22 H27C 2.3453 . . no H22 H28A 2.2590 . . no H22 H32A 2.2452 . . no H22 H32C 2.1951 . . no H22 C27 2.8904 . . no H26A C20 2.8616 . . no H26A H20 2.3862 . . no H26A H28C 2.4372 . . no H26B H27B 2.4158 . . no H26B H28B 2.4901 . . no H26C H27A 2.5441 . . no H26C C20 2.7331 . . no H26C H20 2.1931 . . no H27A H26C 2.5441 . . no H27B H28B 2.5104 . . no H27B H26B 2.4158 . . no H27C H22 2.3453 . . no H27C H28A 2.5256 . . no H27C C22 2.7824 . . no H28A H22 2.2590 . . no H28A H27C 2.5256 . . no H28A C22 2.7155 . . no H28B H26B 2.4901 . . no H28B H27B 2.5104 . . no H28C H26A 2.4372 . . no H30A C13 3.0823 . 1_545 no H30A H13B 2.4877 . 1_545 no H30A H32C 2.5886 . . no H30B H31B 2.5976 . . no H30B H32B 2.3192 . . no H30C C24 2.8699 . . no H30C H31A 2.4331 . . no H30C O1 2.3642 . . no H31A Sc 3.4396 . . no H31A C24 2.8438 . . no H31A H30C 2.4331 . . no H31A O1 2.3948 . . no H31B H32B 2.4259 . . no H31B H30B 2.5976 . . no H31C H32A 2.4894 . . no H31C H42 2.4752 . 2_665 no H32A H47 2.4413 . 2_665 no H32A H31C 2.4894 . . no H32A C22 2.7954 . . no H32A H22 2.2452 . . no H32B H31B 2.4259 . . no H32B H30B 2.3192 . . no H32C H13A 2.4478 . 1_545 no H32C H22 2.1951 . . no H32C H30A 2.5886 . . no H32C C22 2.7369 . . no H34A H2B 2.4144 . 2_666 no H34A H50A 2.2977 . 2_666 no H34A H36C 2.4178 . . no H34B C15 3.0836 . 1_655 no H34B C48 2.9720 . . no H34B H35B 2.4172 . . no H34B H48 2.4738 . . no H34C C30 3.0353 . 1_655 no H34C C37 2.9027 . . no H34C C42 2.8705 . . no H34C H36A 2.5783 . . no H35A H36B 2.5325 . . no H35A H50B 2.3401 . . no H35A O3 2.8886 . . no H35B C43 2.9105 . . no H35B H34B 2.4172 . . no H35C H36C 2.4429 . . no H35C H1A 2.3230 . 2_666 no H35C C50 2.8506 . 2_666 no H35C H50B 2.1154 . 2_666 no H36A C37 3.0411 . . no H36A H12B 2.3121 . 1_645 no H36A H34C 2.5783 . . no H36B H35A 2.5325 . . no H36B O3 2.7706 . . no H36B C1 3.0089 . . no H36B H1A 2.2101 . . no H36C H35C 2.4429 . . no H36C H34A 2.4178 . . no H38 Sc 3.4263 . . no H38 O3 2.7109 . . no H38 C24 2.8737 . . no H38 C19 3.0200 . . no H40 C44 3.0362 . 2_665 no H40 C45 2.9329 . 2_665 no H40 C46 2.9714 . 2_665 no H42 C48 2.9367 . . no H42 H48 2.3233 . . no H42 C31 2.9555 . 2_665 no H42 H31C 2.4752 . 2_665 no H44 Sc 3.4861 . . no H44 O3 2.6043 . . no H46 H47 2.5589 . 2_675 no H46 C17 3.0715 . 2_575 no H47 H32A 2.4413 . 2_665 no H47 H46 2.5589 . 2_675 no H48 H34B 2.4738 . . no H48 H42 2.3233 . . no H48 C34 3.0664 . . no H49A Sc 3.6217 . 2_566 no H49A O2 2.6847 . 2_566 no H49A C4 2.7173 . 2_566 no H49A C9 2.6463 . 2_566 no H49A C3B 2.8124 . 2_566 no H49B H18 2.4943 . . no H50A C3A 2.3176 . . no H50A H3B 2.0028 . . no H50A H34A 2.2977 . 2_666 no H50B H35A 2.3401 . . no H50B C3A 2.8350 . . no H50B C35 3.0833 . 2_666 no H50B H35C 2.1154 . 2_666 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C2 H2A O2 0.9902 2.4733 3.398(5) 155.33 2_566 yes C2 H2A N2 0.9902 2.6113 3.419(7) 138.75 2_566 yes C15 H15A O2 0.9802 2.3473 2.994(3) 122.77 . yes C16 H16A O2 0.9804 2.3248 2.997(3) 125.01 . yes C30 H30C O1 0.9805 2.3642 2.974(3) 119.67 . yes C31 H31A O1 0.9805 2.3948 3.020(3) 121.07 . yes # End of Crystallographic Information File #