# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- CC-Scallyl_revised_08-09-2011.cif' # 1. SUBMISSION DETAILS _publ_contact_author ; Jun Okuda Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52056 Aachen Germany ; _publ_contact_author_phone '+49 241 80 94645' _publ_contact_author_fax '+49 241 80 92644' _publ_contact_author_email jun.okuda@ac.rwth-aachen.de _publ_requested_coeditor_name ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ; loop_ _publ_author_name _publ_author_address S.Standfuss ; Institut fur Anorganische Chemie RWTH Aachen Landoltweg 1 D-52056 Aachen Germany ; E.Abinet ; Institut fur Anorganische Chemie RWTH Aachen Landoltweg 1 D-52056 Aachen Germany ; T.P.Spaniol ; Institut fur Anorganische Chemie RWTH Aachen Landoltweg 1 D-52056 Aachen Germany ; J.Okuda ; Institut fur Anorganische Chemie RWTH Aachen Landoltweg 1 D-52056 Aachen Germany ; _publ_contact_author_name 'Jun Okuda' _publ_contact_author_address ; Institut fur Anorganische Chemie RWTH Aachen Landoltweg 1 Aachen D-52056 Germany ; _publ_contact_letter ; These three crystal structures are a part of a manuscript that is sent for publication in the Journal 'Chem. Commun.'. ; #================================================== data_1a _database_code_depnum_ccdc_archive 'CCDC 832188' #TrackingRef '- CC-Scallyl_revised_08-09-2011.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H31 O2 Sc' _chemical_formula_sum 'C17 H31 O2 Sc' _chemical_formula_weight 312.38 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' 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 1 21/c 1' _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 14.341(6) _cell_length_b 21.027(9) _cell_length_c 11.963(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.738(7) _cell_angle_gamma 90.00 _cell_volume 3489(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4816 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 25.81 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8296 _exptl_absorpt_correction_T_max 0.9129 _exptl_absorpt_process_details 'Bruker Mulabs' _exptl_special_details ; The space group P21/c was determined based on systematic absences in the data set. The value of Rint of 0.114 does not improve significantly by lowering the lattice symmetry (with a value of 0.108 for Laue symmetry -1). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41084 _diffrn_reflns_av_R_equivalents 0.1140 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.71 _reflns_number_total 7333 _reflns_number_gt 4296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The atoms C25 and C29 were refined with split positions as C25A/C25B and C29A/C29B; we have carried out the refinement with isotropic displacement parameters for these disordered atom positions since unrestrained refinement with anisotropic parameters led to an ADPmax/min ratio of 4.9 for C29A. ; _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^)+(0.1229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7333 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.2238 _refine_ls_wR_factor_gt 0.1986 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.49338(5) 0.87914(3) 0.72831(6) 0.0165(2) Uani 1 1 d . . . Sc2 Sc 0.98386(5) 0.86980(3) 0.73966(6) 0.0170(2) Uani 1 1 d . . . O1 O 0.5936(2) 0.87809(12) 0.9041(2) 0.0339(7) Uani 1 1 d . . . O2 O 0.38952(19) 0.87883(11) 0.5567(2) 0.0252(6) Uani 1 1 d . . . O3 O 0.86296(19) 0.86944(12) 0.5796(2) 0.0269(6) Uani 1 1 d . B . O4 O 1.10565(18) 0.87318(11) 0.8966(2) 0.0252(6) Uani 1 1 d . B . C1 C 0.5560(3) 0.77943(17) 0.6895(3) 0.0237(9) Uani 1 1 d . . . H1A H 0.5455 0.7764 0.6046 0.028 Uiso 1 1 calc R . . H1B H 0.6266 0.7810 0.7227 0.028 Uiso 1 1 calc R . . C2 C 0.5217(3) 0.71914(18) 0.7283(4) 0.0326(10) Uani 1 1 d . . . H2 H 0.5407 0.7115 0.8092 0.039 Uiso 1 1 calc R . . C3 C 0.4685(3) 0.6748(2) 0.6661(4) 0.0463(12) Uani 1 1 d . . . H3A H 0.4470 0.6794 0.5846 0.056 Uiso 1 1 calc R . . H3B H 0.4515 0.6380 0.7026 0.056 Uiso 1 1 calc R . . C4 C 0.5341(3) 0.98966(18) 0.7029(4) 0.0330(10) Uani 1 1 d . . . H4A H 0.4738 0.9807 0.6501 0.040 Uiso 1 1 calc R . . H4B H 0.5384 1.0218 0.7597 0.040 Uiso 1 1 calc R . . C5 C 0.6156(3) 0.95577(19) 0.6968(4) 0.0389(11) Uani 1 1 d . . . H5 H 0.6741 0.9665 0.7514 0.047 Uiso 1 1 calc R . . C6 C 0.6199(3) 0.9087(2) 0.6204(4) 0.0411(12) Uani 1 1 d . . . H6A H 0.5633 0.8963 0.5641 0.049 Uiso 1 1 calc R . . H6B H 0.6796 0.8883 0.6233 0.049 Uiso 1 1 calc R . . C7 C 0.3819(3) 0.8121(2) 0.8075(4) 0.0337(10) Uani 1 1 d . . . H7A H 0.4446 0.8120 0.8588 0.040 Uiso 1 1 calc R . . H7B H 0.3519 0.7730 0.7786 0.040 Uiso 1 1 calc R . . C8 C 0.3351(3) 0.8681(2) 0.7755(4) 0.0481(13) Uani 1 1 d . . . H8 H 0.2726 0.8665 0.7241 0.058 Uiso 1 1 calc R . . C9 C 0.3736(3) 0.9289(2) 0.8138(4) 0.0393(11) Uani 1 1 d . . . H9A H 0.4359 0.9323 0.8652 0.047 Uiso 1 1 calc R . . H9B H 0.3370 0.9662 0.7880 0.047 Uiso 1 1 calc R . . C10 C 0.6136(4) 0.9320(2) 0.9842(4) 0.0638(18) Uani 1 1 d . . . H10A H 0.6172 0.9719 0.9417 0.077 Uiso 1 1 calc R . . H10B H 0.5620 0.9363 1.0250 0.077 Uiso 1 1 calc R . . C11 C 0.7022(4) 0.9194(2) 1.0631(5) 0.0609(16) Uani 1 1 d . . . H11A H 0.7045 0.9395 1.1387 0.073 Uiso 1 1 calc R . . H11B H 0.7560 0.9364 1.0341 0.073 Uiso 1 1 calc R . . C12 C 0.7099(3) 0.84777(19) 1.0755(3) 0.0333(10) Uani 1 1 d . . . H12A H 0.6868 0.8330 1.1424 0.040 Uiso 1 1 calc R . . H12B H 0.7772 0.8334 1.0853 0.040 Uiso 1 1 calc R . . C13 C 0.6452(3) 0.82351(18) 0.9627(3) 0.0247(9) Uani 1 1 d . . . H13A H 0.6843 0.8037 0.9148 0.030 Uiso 1 1 calc R . . H13B H 0.5994 0.7914 0.9780 0.030 Uiso 1 1 calc R . . C14 C 0.3253(3) 0.93007(18) 0.4979(3) 0.0289(9) Uani 1 1 d . . . H14A H 0.3631 0.9677 0.4860 0.035 Uiso 1 1 calc R . . H14B H 0.2797 0.9429 0.5436 0.035 Uiso 1 1 calc R . . C15 C 0.2724(3) 0.90165(18) 0.3841(3) 0.0283(9) Uani 1 1 d . . . H15A H 0.3106 0.9050 0.3261 0.034 Uiso 1 1 calc R . . H15B H 0.2090 0.9224 0.3535 0.034 Uiso 1 1 calc R . . C16 C 0.2606(3) 0.83247(18) 0.4167(3) 0.0273(9) Uani 1 1 d . . . H16A H 0.2092 0.8278 0.4578 0.033 Uiso 1 1 calc R . . H16B H 0.2464 0.8045 0.3479 0.033 Uiso 1 1 calc R . . C17 C 0.3594(3) 0.81882(18) 0.4957(3) 0.0299(10) Uani 1 1 d . . . H17A H 0.3558 0.7844 0.5509 0.036 Uiso 1 1 calc R . . H17B H 0.4052 0.8060 0.4503 0.036 Uiso 1 1 calc R . . C18 C 0.9320(3) 0.97167(16) 0.7812(3) 0.0240(9) Uani 1 1 d . B . H18A H 0.8614 0.9733 0.7473 0.029 Uiso 1 1 calc R . . H18B H 0.9422 0.9741 0.8661 0.029 Uiso 1 1 calc R . . C19 C 0.9727(3) 1.03045(17) 0.7453(4) 0.0305(10) Uani 1 1 d . . . H19 H 0.9564 1.0384 0.6644 0.037 Uiso 1 1 calc R B . C20 C 1.0295(3) 1.07425(19) 0.8110(4) 0.0453(12) Uani 1 1 d . B . H20A H 1.0486 1.0693 0.8926 0.054 Uiso 1 1 calc R . . H20B H 1.0505 1.1102 0.7758 0.054 Uiso 1 1 calc R . . C21 C 1.0906(3) 0.92759(19) 0.6388(4) 0.0343(10) Uani 1 1 d . B . H21A H 1.1178 0.9312 0.7197 0.041 Uiso 1 1 calc R . . H21B H 1.0765 0.9648 0.5925 0.041 Uiso 1 1 calc R . . C22 C 1.0710(3) 0.8662(2) 0.5866(4) 0.0414(12) Uani 1 1 d . B . H22 H 1.0439 0.8646 0.5055 0.050 Uiso 1 1 calc R . . C23 C 1.0886(3) 0.80882(19) 0.6456(4) 0.0324(10) Uani 1 1 d . B . H23A H 1.1157 0.8085 0.7268 0.039 Uiso 1 1 calc R . . H23B H 1.0736 0.7699 0.6047 0.039 Uiso 1 1 calc R . . C24 C 0.8698(4) 0.8472(2) 0.8694(4) 0.0487(13) Uani 1 1 d . B . H24A H 0.9296 0.8615 0.9170 0.058 Uiso 0.66 1 calc PR A 1 H24B H 0.8117 0.8681 0.8718 0.058 Uiso 0.66 1 calc PR A 1 H24C H 0.8301 0.8599 0.7965 0.058 Uiso 0.34 1 calc PR A 2 H24D H 0.8663 0.8692 0.9375 0.058 Uiso 0.34 1 calc PR A 2 C25A C 0.8675(4) 0.7983(3) 0.7999(5) 0.0272(13) Uiso 0.66 1 d P B 1 H25A H 0.8054 0.7866 0.7548 0.033 Uiso 0.66 1 calc PR B 1 C25B C 0.9228(9) 0.8046(6) 0.8751(11) 0.034(3) Uiso 0.34 1 d P B 2 H25B H 0.9595 0.7953 0.9513 0.041 Uiso 0.34 1 calc PR B 2 C26 C 0.9438(3) 0.76149(18) 0.7835(4) 0.0375(11) Uani 1 1 d . B . H26A H 1.0080 0.7706 0.8259 0.045 Uiso 0.66 1 calc PR C 1 H26B H 0.9317 0.7272 0.7300 0.045 Uiso 0.66 1 calc PR C 1 H26C H 0.9105 0.7673 0.7047 0.045 Uiso 0.34 1 calc PR C 2 H26D H 0.9904 0.7286 0.8047 0.045 Uiso 0.34 1 calc PR C 2 C27 C 0.8327(3) 0.92635(19) 0.5099(3) 0.0333(10) Uani 1 1 d . . . H27A H 0.8896 0.9503 0.5005 0.040 Uiso 1 1 calc R B . H27B H 0.7944 0.9544 0.5477 0.040 Uiso 1 1 calc R . . C28 C 0.7733(4) 0.9049(2) 0.3957(4) 0.0665(18) Uani 1 1 d . B . H28A H 0.8087 0.9110 0.3354 0.080 Uiso 0.50 1 calc PR D 1 H28B H 0.7122 0.9290 0.3736 0.080 Uiso 0.50 1 calc PR D 1 H28C H 0.7044 0.9140 0.3893 0.080 Uiso 0.50 1 calc PR D 2 H28D H 0.7928 0.9280 0.3332 0.080 Uiso 0.50 1 calc PR D 2 C29A C 0.7534(6) 0.8338(4) 0.4101(7) 0.0273(19) Uiso 0.50 1 d P B 1 H29A H 0.6877 0.8276 0.4204 0.033 Uiso 0.50 1 calc PR B 1 H29B H 0.7595 0.8094 0.3416 0.033 Uiso 0.50 1 calc PR B 1 C29B C 0.7863(7) 0.8406(4) 0.3849(8) 0.037(2) Uiso 0.50 1 d P B 2 H29C H 0.8340 0.8325 0.3395 0.045 Uiso 0.50 1 calc PR B 2 H29D H 0.7247 0.8200 0.3452 0.045 Uiso 0.50 1 calc PR B 2 C30 C 0.8233(3) 0.8142(2) 0.5094(4) 0.0374(11) Uani 1 1 d . . . H30A H 0.8757 0.7912 0.4863 0.045 Uiso 0.50 1 calc PR B 1 H30B H 0.7937 0.7848 0.5552 0.045 Uiso 0.50 1 calc PR B 1 H30C H 0.7699 0.7951 0.5364 0.045 Uiso 0.50 1 calc PR B 2 H30D H 0.8737 0.7815 0.5127 0.045 Uiso 0.50 1 calc PR B 2 C31 C 1.1354(3) 0.93266(18) 0.9594(4) 0.0348(11) Uani 1 1 d . . . H31A H 1.0831 0.9491 0.9917 0.042 Uiso 1 1 calc R B . H31B H 1.1509 0.9652 0.9070 0.042 Uiso 1 1 calc R . . C32 C 1.2225(3) 0.91753(18) 1.0541(3) 0.0313(10) Uani 1 1 d . B . H32A H 1.2255 0.9441 1.1232 0.038 Uiso 1 1 calc R . . H32B H 1.2824 0.9234 1.0286 0.038 Uiso 1 1 calc R . . C33 C 1.2061(3) 0.84750(18) 1.0778(3) 0.0306(10) Uani 1 1 d . . . H33A H 1.2671 0.8261 1.1172 0.037 Uiso 1 1 calc R B . H33B H 1.1589 0.8426 1.1249 0.037 Uiso 1 1 calc R . . C34 C 1.1674(3) 0.82260(18) 0.9587(3) 0.0257(9) Uani 1 1 d . B . H34A H 1.2204 0.8132 0.9220 0.031 Uiso 1 1 calc R . . H34B H 1.1297 0.7832 0.9598 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0178(4) 0.0159(4) 0.0180(4) 0.0007(3) 0.0085(3) 0.0017(3) Sc2 0.0165(4) 0.0151(4) 0.0217(4) 0.0013(3) 0.0089(3) 0.0014(3) O1 0.0466(19) 0.0192(15) 0.0279(15) -0.0026(12) -0.0052(14) 0.0037(13) O2 0.0290(15) 0.0165(14) 0.0257(14) -0.0004(11) -0.0013(12) 0.0015(11) O3 0.0316(16) 0.0210(15) 0.0250(15) -0.0025(11) 0.0012(12) -0.0009(12) O4 0.0229(14) 0.0205(14) 0.0296(15) -0.0023(11) 0.0018(12) 0.0068(11) C1 0.020(2) 0.027(2) 0.024(2) -0.0008(16) 0.0072(17) 0.0024(16) C2 0.036(2) 0.025(2) 0.038(2) -0.0017(18) 0.011(2) 0.0015(19) C3 0.048(3) 0.037(3) 0.057(3) 0.005(2) 0.019(3) 0.000(2) C4 0.033(2) 0.023(2) 0.043(3) -0.0060(18) 0.010(2) -0.0075(18) C5 0.029(2) 0.027(2) 0.062(3) 0.012(2) 0.015(2) -0.0095(19) C6 0.031(3) 0.036(3) 0.067(3) 0.014(2) 0.032(2) -0.002(2) C7 0.021(2) 0.040(3) 0.045(3) 0.011(2) 0.017(2) 0.0011(19) C8 0.029(3) 0.065(4) 0.058(3) 0.006(3) 0.025(2) 0.004(2) C9 0.030(2) 0.044(3) 0.050(3) -0.011(2) 0.021(2) 0.011(2) C10 0.092(5) 0.035(3) 0.041(3) -0.007(2) -0.026(3) 0.007(3) C11 0.057(4) 0.047(3) 0.062(4) -0.024(3) -0.017(3) 0.020(3) C12 0.030(2) 0.040(3) 0.024(2) 0.0080(18) -0.0031(19) -0.0070(19) C13 0.023(2) 0.025(2) 0.026(2) 0.0054(16) 0.0052(17) -0.0010(16) C14 0.027(2) 0.022(2) 0.033(2) 0.0049(17) 0.0001(19) 0.0082(17) C15 0.025(2) 0.026(2) 0.030(2) 0.0034(17) -0.0009(18) 0.0011(17) C16 0.024(2) 0.027(2) 0.032(2) -0.0037(17) 0.0094(18) -0.0037(17) C17 0.040(3) 0.024(2) 0.021(2) -0.0024(16) -0.0017(18) 0.0019(18) C18 0.018(2) 0.022(2) 0.031(2) -0.0007(16) 0.0049(17) 0.0048(16) C19 0.026(2) 0.020(2) 0.044(3) 0.0055(18) 0.0059(19) 0.0061(17) C20 0.039(3) 0.021(2) 0.070(3) 0.004(2) 0.002(2) 0.000(2) C21 0.032(2) 0.035(3) 0.043(3) 0.014(2) 0.023(2) 0.0040(19) C22 0.036(3) 0.063(3) 0.033(2) 0.004(2) 0.022(2) 0.004(2) C23 0.038(3) 0.035(2) 0.029(2) -0.0077(18) 0.018(2) 0.0070(19) C24 0.052(3) 0.044(3) 0.066(3) -0.005(2) 0.045(3) -0.018(2) C26 0.042(3) 0.022(2) 0.053(3) 0.0055(19) 0.019(2) -0.0025(19) C27 0.033(2) 0.026(2) 0.040(3) 0.0084(18) 0.009(2) 0.0001(18) C28 0.109(5) 0.046(3) 0.028(3) 0.009(2) -0.014(3) -0.022(3) C30 0.043(3) 0.028(2) 0.036(3) -0.0118(19) 0.000(2) -0.004(2) C31 0.036(3) 0.024(2) 0.035(2) -0.0071(18) -0.009(2) 0.0029(18) C32 0.031(2) 0.029(2) 0.030(2) -0.0027(18) 0.0012(19) 0.0020(18) C33 0.029(2) 0.034(2) 0.023(2) 0.0052(17) -0.0021(18) 0.0029(18) C34 0.020(2) 0.025(2) 0.031(2) 0.0048(17) 0.0049(17) 0.0067(16) _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 Sc1 O2 2.208(3) . ? Sc1 O1 2.225(3) . ? Sc1 C1 2.373(4) . ? Sc1 C4 2.434(4) . ? Sc1 C9 2.447(4) . ? Sc1 C5 2.479(4) . ? Sc1 C8 2.485(4) . ? Sc1 C7 2.493(4) . ? Sc1 C6 2.557(4) . ? Sc2 O4 2.216(3) . ? Sc2 O3 2.233(3) . ? Sc2 C18 2.362(4) . ? Sc2 C26 2.438(4) . ? Sc2 C25B 2.448(13) . ? Sc2 C23 2.455(4) . ? Sc2 C22 2.467(4) . ? Sc2 C25A 2.484(6) . ? Sc2 C21 2.494(4) . ? Sc2 C24 2.569(4) . ? O1 C13 1.446(4) . ? O1 C10 1.464(5) . ? O2 C17 1.467(4) . ? O2 C14 1.474(4) . ? O3 C27 1.460(4) . ? O3 C30 1.462(4) . ? O4 C34 1.460(4) . ? O4 C31 1.465(4) . ? C1 C2 1.477(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.310(6) . ? C2 H2 0.9500 . ? C3 H3A 0.9500 . ? C3 H3B 0.9500 . ? C4 C5 1.387(6) . ? C4 H4A 0.9500 . ? C4 H4B 0.9500 . ? C5 C6 1.359(6) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C7 C8 1.363(6) . ? C7 H7A 0.9500 . ? C7 H7B 0.9500 . ? C8 C9 1.421(6) . ? C8 H8 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C10 C11 1.403(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.515(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.518(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.504(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.527(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.517(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.476(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.343(6) . ? C19 H19 0.9500 . ? C20 H20A 0.9500 . ? C20 H20B 0.9500 . ? C21 C22 1.429(6) . ? C21 H21A 0.9500 . ? C21 H21B 0.9500 . ? C22 C23 1.389(6) . ? C22 H22 0.9500 . ? C23 H23A 0.9500 . ? C23 H23B 0.9500 . ? C24 C25B 1.166(13) . ? C24 C25A 1.317(7) . ? C24 H24A 0.9500 . ? C24 H24B 0.9500 . ? C24 H24C 0.9500 . ? C24 H24D 0.9500 . ? C25A C26 1.395(7) . ? C25A H25A 0.9500 . ? C25B C26 1.510(13) . ? C25B H25B 0.9500 . ? C26 H26A 0.9500 . ? C26 H26B 0.9500 . ? C26 H26C 0.9500 . ? C26 H26D 0.9500 . ? C27 C28 1.484(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29B 1.375(10) . ? C28 C29A 1.539(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 H28C 0.9900 . ? C28 H28D 0.9900 . ? C29A C30 1.407(9) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C29B C30 1.551(10) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C30 H30C 0.9900 . ? C30 H30D 0.9900 . ? C31 C32 1.491(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.529(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.486(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 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 O2 Sc1 O1 177.82(11) . . ? O2 Sc1 C1 90.85(11) . . ? O1 Sc1 C1 89.46(11) . . ? O2 Sc1 C4 90.75(12) . . ? O1 Sc1 C4 90.57(12) . . ? C1 Sc1 C4 134.78(14) . . ? O2 Sc1 C9 90.60(13) . . ? O1 Sc1 C9 87.86(14) . . ? C1 Sc1 C9 143.22(14) . . ? C4 Sc1 C9 81.94(15) . . ? O2 Sc1 C5 101.34(13) . . ? O1 Sc1 C5 80.69(14) . . ? C1 Sc1 C5 103.11(14) . . ? C4 Sc1 C5 32.78(13) . . ? C9 Sc1 C5 112.59(15) . . ? O2 Sc1 C8 76.81(14) . . ? O1 Sc1 C8 101.08(15) . . ? C1 Sc1 C8 112.05(15) . . ? C4 Sc1 C8 112.28(15) . . ? C9 Sc1 C8 33.48(14) . . ? C5 Sc1 C8 144.78(16) . . ? O2 Sc1 C7 90.32(13) . . ? O1 Sc1 C7 87.57(13) . . ? C1 Sc1 C7 83.44(13) . . ? C4 Sc1 C7 141.74(14) . . ? C9 Sc1 C7 59.80(15) . . ? C5 Sc1 C7 166.42(16) . . ? C8 Sc1 C7 31.79(13) . . ? O2 Sc1 C6 85.93(14) . . ? O1 Sc1 C6 96.24(14) . . ? C1 Sc1 C6 76.31(13) . . ? C4 Sc1 C6 58.74(14) . . ? C9 Sc1 C6 140.42(15) . . ? C5 Sc1 C6 31.26(14) . . ? C8 Sc1 C6 160.71(16) . . ? C7 Sc1 C6 159.34(15) . . ? O4 Sc2 O3 178.06(10) . . ? O4 Sc2 C18 90.88(11) . . ? O3 Sc2 C18 88.05(11) . . ? O4 Sc2 C26 91.47(13) . . ? O3 Sc2 C26 90.43(13) . . ? C18 Sc2 C26 134.27(14) . . ? O4 Sc2 C25B 78.2(3) . . ? O3 Sc2 C25B 103.6(3) . . ? C18 Sc2 C25B 100.6(3) . . ? C26 Sc2 C25B 36.0(3) . . ? O4 Sc2 C23 87.86(13) . . ? O3 Sc2 C23 92.13(13) . . ? C18 Sc2 C23 146.34(14) . . ? C26 Sc2 C23 79.39(14) . . ? C25B Sc2 C23 112.0(3) . . ? O4 Sc2 C22 100.99(14) . . ? O3 Sc2 C22 78.03(13) . . ? C18 Sc2 C22 115.46(14) . . ? C26 Sc2 C22 108.83(15) . . ? C25B Sc2 C22 143.9(3) . . ? C23 Sc2 C22 32.77(13) . . ? O4 Sc2 C25A 102.50(16) . . ? O3 Sc2 C25A 79.32(16) . . ? C18 Sc2 C25A 102.52(16) . . ? C26 Sc2 C25A 32.90(16) . . ? C25B Sc2 C25A 24.5(3) . . ? C23 Sc2 C25A 110.58(17) . . ? C22 Sc2 C25A 134.54(18) . . ? O4 Sc2 C21 86.89(13) . . ? O3 Sc2 C21 91.42(13) . . ? C18 Sc2 C21 85.69(13) . . ? C26 Sc2 C21 140.04(14) . . ? C25B Sc2 C21 163.8(3) . . ? C23 Sc2 C21 60.65(14) . . ? C22 Sc2 C21 33.49(14) . . ? C25A Sc2 C21 167.28(18) . . ? O4 Sc2 C24 88.85(15) . . ? O3 Sc2 C24 92.45(15) . . ? C18 Sc2 C24 75.97(14) . . ? C26 Sc2 C24 58.43(14) . . ? C25B Sc2 C24 26.7(3) . . ? C23 Sc2 C24 137.58(15) . . ? C22 Sc2 C24 164.45(16) . . ? C25A Sc2 C24 30.15(16) . . ? C21 Sc2 C24 161.11(14) . . ? C13 O1 C10 107.8(3) . . ? C13 O1 Sc1 126.4(2) . . ? C10 O1 Sc1 125.6(2) . . ? C17 O2 C14 108.8(3) . . ? C17 O2 Sc1 120.6(2) . . ? C14 O2 Sc1 129.3(2) . . ? C27 O3 C30 107.9(3) . . ? C27 O3 Sc2 122.7(2) . . ? C30 O3 Sc2 126.8(2) . . ? C34 O4 C31 107.5(3) . . ? C34 O4 Sc2 130.8(2) . . ? C31 O4 Sc2 121.7(2) . . ? C2 C1 Sc1 121.6(3) . . ? C2 C1 H1A 106.9 . . ? Sc1 C1 H1A 106.9 . . ? C2 C1 H1B 106.9 . . ? Sc1 C1 H1B 106.9 . . ? H1A C1 H1B 106.7 . . ? C3 C2 C1 128.7(4) . . ? C3 C2 H2 115.6 . . ? C1 C2 H2 115.6 . . ? C2 C3 H3A 120.0 . . ? C2 C3 H3B 120.0 . . ? H3A C3 H3B 120.0 . . ? C5 C4 Sc1 75.4(2) . . ? C5 C4 H4A 120.0 . . ? Sc1 C4 H4A 71.8 . . ? C5 C4 H4B 120.0 . . ? Sc1 C4 H4B 124.4 . . ? H4A C4 H4B 120.0 . . ? C6 C5 C4 126.3(4) . . ? C6 C5 Sc1 77.5(2) . . ? C4 C5 Sc1 71.8(2) . . ? C6 C5 H5 116.8 . . ? C4 C5 H5 116.8 . . ? Sc1 C5 H5 125.8 . . ? C5 C6 Sc1 71.2(2) . . ? C5 C6 H6A 120.0 . . ? Sc1 C6 H6A 72.7 . . ? C5 C6 H6B 120.0 . . ? Sc1 C6 H6B 128.3 . . ? H6A C6 H6B 120.0 . . ? C8 C7 Sc1 73.8(2) . . ? C8 C7 H7A 120.0 . . ? Sc1 C7 H7A 69.7 . . ? C8 C7 H7B 120.0 . . ? Sc1 C7 H7B 128.7 . . ? H7A C7 H7B 120.0 . . ? C7 C8 C9 124.4(5) . . ? C7 C8 Sc1 74.4(2) . . ? C9 C8 Sc1 71.8(2) . . ? C7 C8 H8 117.8 . . ? C9 C8 H8 117.8 . . ? Sc1 C8 H8 128.5 . . ? C8 C9 Sc1 74.7(2) . . ? C8 C9 H9A 120.0 . . ? Sc1 C9 H9A 70.0 . . ? C8 C9 H9B 120.0 . . ? Sc1 C9 H9B 127.3 . . ? H9A C9 H9B 120.0 . . ? C11 C10 O1 106.8(4) . . ? C11 C10 H10A 110.4 . . ? O1 C10 H10A 110.4 . . ? C11 C10 H10B 110.4 . . ? O1 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? C10 C11 C12 106.5(4) . . ? C10 C11 H11A 110.4 . . ? C12 C11 H11A 110.4 . . ? C10 C11 H11B 110.4 . . ? C12 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? C11 C12 C13 103.6(3) . . ? C11 C12 H12A 111.0 . . ? C13 C12 H12A 111.0 . . ? C11 C12 H12B 111.0 . . ? C13 C12 H12B 111.0 . . ? H12A C12 H12B 109.0 . . ? O1 C13 C12 106.6(3) . . ? O1 C13 H13A 110.4 . . ? C12 C13 H13A 110.4 . . ? O1 C13 H13B 110.4 . . ? C12 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? O2 C14 C15 104.6(3) . . ? O2 C14 H14A 110.8 . . ? C15 C14 H14A 110.8 . . ? O2 C14 H14B 110.8 . . ? C15 C14 H14B 110.8 . . ? H14A C14 H14B 108.9 . . ? C14 C15 C16 102.1(3) . . ? C14 C15 H15A 111.3 . . ? C16 C15 H15A 111.3 . . ? C14 C15 H15B 111.3 . . ? C16 C15 H15B 111.3 . . ? H15A C15 H15B 109.2 . . ? C17 C16 C15 101.1(3) . . ? C17 C16 H16A 111.5 . . ? C15 C16 H16A 111.5 . . ? C17 C16 H16B 111.5 . . ? C15 C16 H16B 111.5 . . ? H16A C16 H16B 109.4 . . ? O2 C17 C16 104.9(3) . . ? O2 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? O2 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.8 . . ? C19 C18 Sc2 121.9(3) . . ? C19 C18 H18A 106.8 . . ? Sc2 C18 H18A 106.8 . . ? C19 C18 H18B 106.8 . . ? Sc2 C18 H18B 106.8 . . ? H18A C18 H18B 106.7 . . ? C20 C19 C18 129.0(4) . . ? C20 C19 H19 115.5 . . ? C18 C19 H19 115.5 . . ? C19 C20 H20A 120.0 . . ? C19 C20 H20B 120.0 . . ? H20A C20 H20B 120.0 . . ? C22 C21 Sc2 72.2(2) . . ? C22 C21 H21A 120.0 . . ? Sc2 C21 H21A 71.8 . . ? C22 C21 H21B 120.0 . . ? Sc2 C21 H21B 128.1 . . ? H21A C21 H21B 120.0 . . ? C23 C22 C21 125.0(4) . . ? C23 C22 Sc2 73.2(2) . . ? C21 C22 Sc2 74.3(2) . . ? C23 C22 H22 117.5 . . ? C21 C22 H22 117.5 . . ? Sc2 C22 H22 127.3 . . ? C22 C23 Sc2 74.1(2) . . ? C22 C23 H23A 120.0 . . ? Sc2 C23 H23A 71.0 . . ? C22 C23 H23B 120.0 . . ? Sc2 C23 H23B 126.9 . . ? H23A C23 H23B 120.0 . . ? C25B C24 C25A 49.3(7) . . ? C25B C24 Sc2 70.8(7) . . ? C25A C24 Sc2 71.4(3) . . ? C25B C24 H24A 74.5 . . ? C25A C24 H24A 120.0 . . ? Sc2 C24 H24A 71.8 . . ? C25B C24 H24B 156.7 . . ? C25A C24 H24B 120.0 . . ? Sc2 C24 H24B 129.2 . . ? H24A C24 H24B 120.0 . . ? C25B C24 H24C 120.0 . . ? C25A C24 H24C 74.2 . . ? Sc2 C24 H24C 73.7 . . ? H24A C24 H24C 134.4 . . ? H24B C24 H24C 64.7 . . ? C25B C24 H24D 120.0 . . ? C25A C24 H24D 157.4 . . ? Sc2 C24 H24D 127.6 . . ? H24A C24 H24D 64.4 . . ? H24B C24 H24D 60.6 . . ? H24C C24 H24D 120.0 . . ? C24 C25A C26 128.9(6) . . ? C24 C25A Sc2 78.5(3) . . ? C26 C25A Sc2 71.7(3) . . ? C24 C25A H25A 115.6 . . ? C26 C25A H25A 115.6 . . ? Sc2 C25A H25A 126.5 . . ? C24 C25B C26 131.8(11) . . ? C24 C25B Sc2 82.4(7) . . ? C26 C25B Sc2 71.6(5) . . ? C24 C25B H25B 114.1 . . ? C26 C25B H25B 114.1 . . ? Sc2 C25B H25B 123.1 . . ? C25A C26 Sc2 75.4(3) . . ? C25B C26 Sc2 72.3(5) . . ? C25A C26 H26A 120.0 . . ? Sc2 C26 H26A 71.1 . . ? C25A C26 H26B 120.0 . . ? Sc2 C26 H26B 125.2 . . ? H26A C26 H26B 120.0 . . ? C25B C26 H26C 120.0 . . ? Sc2 C26 H26C 75.7 . . ? H26A C26 H26C 132.7 . . ? H26B C26 H26C 57.9 . . ? C25A C26 H26D 152.9 . . ? C25B C26 H26D 120.0 . . ? Sc2 C26 H26D 123.3 . . ? H26A C26 H26D 59.1 . . ? H26B C26 H26D 67.9 . . ? H26C C26 H26D 120.0 . . ? O3 C27 C28 107.1(3) . . ? O3 C27 H27A 110.3 . . ? C28 C27 H27A 110.3 . . ? O3 C27 H27B 110.3 . . ? C28 C27 H27B 110.3 . . ? H27A C27 H27B 108.6 . . ? C29B C28 C27 109.1(5) . . ? C27 C28 C29A 105.8(4) . . ? C27 C28 H28A 110.6 . . ? C29A C28 H28A 110.6 . . ? C29B C28 H28B 127.7 . . ? C27 C28 H28B 110.6 . . ? C29A C28 H28B 110.6 . . ? H28A C28 H28B 108.7 . . ? C29B C28 H28C 109.9 . . ? C27 C28 H28C 109.9 . . ? C29B C28 H28D 109.9 . . ? C27 C28 H28D 109.9 . . ? H28C C28 H28D 108.3 . . ? C30 C29A C28 105.5(6) . . ? C30 C29A H29A 110.6 . . ? C28 C29A H29A 110.6 . . ? C30 C29A H29B 110.6 . . ? C28 C29A H29B 110.6 . . ? H29A C29A H29B 108.8 . . ? C28 C29B C30 106.4(6) . . ? C28 C29B H29C 110.4 . . ? C30 C29B H29C 110.4 . . ? C28 C29B H29D 110.4 . . ? C30 C29B H29D 110.4 . . ? H29C C29B H29D 108.6 . . ? C29A C30 O3 109.9(4) . . ? O3 C30 C29B 104.8(4) . . ? C29A C30 H30A 109.7 . . ? O3 C30 H30A 109.7 . . ? C29A C30 H30B 109.7 . . ? O3 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? O3 C30 H30C 110.8 . . ? C29B C30 H30C 110.8 . . ? O3 C30 H30D 110.8 . . ? C29B C30 H30D 110.8 . . ? H30C C30 H30D 108.9 . . ? O4 C31 C32 106.6(3) . . ? O4 C31 H31A 110.4 . . ? C32 C31 H31A 110.4 . . ? O4 C31 H31B 110.4 . . ? C32 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C31 C32 C33 102.0(3) . . ? C31 C32 H32A 111.4 . . ? C33 C32 H32A 111.4 . . ? C31 C32 H32B 111.4 . . ? C33 C32 H32B 111.4 . . ? H32A C32 H32B 109.2 . . ? C34 C33 C32 101.5(3) . . ? C34 C33 H33A 111.5 . . ? C32 C33 H33A 111.5 . . ? C34 C33 H33B 111.5 . . ? C32 C33 H33B 111.5 . . ? H33A C33 H33B 109.3 . . ? O4 C34 C33 105.2(3) . . ? O4 C34 H34A 110.7 . . ? C33 C34 H34A 110.7 . . ? O4 C34 H34B 110.7 . . ? C33 C34 H34B 110.7 . . ? H34A C34 H34B 108.8 . . ? 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 C1 Sc1 O1 C13 -16.1(3) . . . . ? C4 Sc1 O1 C13 -150.9(3) . . . . ? C9 Sc1 O1 C13 127.2(3) . . . . ? C5 Sc1 O1 C13 -119.5(3) . . . . ? C8 Sc1 O1 C13 96.3(3) . . . . ? C7 Sc1 O1 C13 67.3(3) . . . . ? C6 Sc1 O1 C13 -92.3(3) . . . . ? C1 Sc1 O1 C10 168.5(4) . . . . ? C4 Sc1 O1 C10 33.7(4) . . . . ? C9 Sc1 O1 C10 -48.2(4) . . . . ? C5 Sc1 O1 C10 65.1(4) . . . . ? C8 Sc1 O1 C10 -79.1(4) . . . . ? C7 Sc1 O1 C10 -108.0(4) . . . . ? C6 Sc1 O1 C10 92.3(4) . . . . ? C1 Sc1 O2 C17 23.9(3) . . . . ? C4 Sc1 O2 C17 158.7(3) . . . . ? C9 Sc1 O2 C17 -119.4(3) . . . . ? C5 Sc1 O2 C17 127.4(3) . . . . ? C8 Sc1 O2 C17 -88.6(3) . . . . ? C7 Sc1 O2 C17 -59.6(3) . . . . ? C6 Sc1 O2 C17 100.1(3) . . . . ? C1 Sc1 O2 C14 -170.9(3) . . . . ? C4 Sc1 O2 C14 -36.1(3) . . . . ? C9 Sc1 O2 C14 45.8(3) . . . . ? C5 Sc1 O2 C14 -67.4(3) . . . . ? C8 Sc1 O2 C14 76.6(3) . . . . ? C7 Sc1 O2 C14 105.6(3) . . . . ? C6 Sc1 O2 C14 -94.7(3) . . . . ? C18 Sc2 O3 C27 37.3(3) . . . . ? C26 Sc2 O3 C27 171.6(3) . . . . ? C25B Sc2 O3 C27 137.7(4) . . . . ? C23 Sc2 O3 C27 -109.0(3) . . . . ? C22 Sc2 O3 C27 -79.3(3) . . . . ? C25A Sc2 O3 C27 140.4(3) . . . . ? C21 Sc2 O3 C27 -48.4(3) . . . . ? C24 Sc2 O3 C27 113.1(3) . . . . ? C18 Sc2 O3 C30 -163.0(3) . . . . ? C26 Sc2 O3 C30 -28.7(3) . . . . ? C25B Sc2 O3 C30 -62.6(4) . . . . ? C23 Sc2 O3 C30 50.7(3) . . . . ? C22 Sc2 O3 C30 80.5(3) . . . . ? C25A Sc2 O3 C30 -59.9(3) . . . . ? C21 Sc2 O3 C30 111.4(3) . . . . ? C24 Sc2 O3 C30 -87.1(3) . . . . ? C18 Sc2 O4 C34 163.5(3) . . . . ? C26 Sc2 O4 C34 29.2(3) . . . . ? C25B Sc2 O4 C34 62.8(4) . . . . ? C23 Sc2 O4 C34 -50.2(3) . . . . ? C22 Sc2 O4 C34 -80.4(3) . . . . ? C25A Sc2 O4 C34 60.4(3) . . . . ? C21 Sc2 O4 C34 -110.9(3) . . . . ? C24 Sc2 O4 C34 87.5(3) . . . . ? C18 Sc2 O4 C31 -14.4(3) . . . . ? C26 Sc2 O4 C31 -148.8(3) . . . . ? C25B Sc2 O4 C31 -115.1(4) . . . . ? C23 Sc2 O4 C31 131.9(3) . . . . ? C22 Sc2 O4 C31 101.7(3) . . . . ? C25A Sc2 O4 C31 -117.5(3) . . . . ? C21 Sc2 O4 C31 71.2(3) . . . . ? C24 Sc2 O4 C31 -90.4(3) . . . . ? O2 Sc1 C1 C2 -95.5(3) . . . . ? O1 Sc1 C1 C2 82.3(3) . . . . ? C4 Sc1 C1 C2 172.6(3) . . . . ? C9 Sc1 C1 C2 -3.4(4) . . . . ? C5 Sc1 C1 C2 162.6(3) . . . . ? C8 Sc1 C1 C2 -19.4(4) . . . . ? C7 Sc1 C1 C2 -5.3(3) . . . . ? C6 Sc1 C1 C2 178.9(3) . . . . ? Sc1 C1 C2 C3 109.2(5) . . . . ? O2 Sc1 C4 C5 -110.1(3) . . . . ? O1 Sc1 C4 C5 71.7(3) . . . . ? C1 Sc1 C4 C5 -18.1(4) . . . . ? C9 Sc1 C4 C5 159.4(3) . . . . ? C8 Sc1 C4 C5 173.9(3) . . . . ? C7 Sc1 C4 C5 158.5(3) . . . . ? C6 Sc1 C4 C5 -25.3(3) . . . . ? Sc1 C4 C5 C6 58.4(4) . . . . ? O2 Sc1 C5 C6 -62.0(3) . . . . ? O1 Sc1 C5 C6 118.8(3) . . . . ? C1 Sc1 C5 C6 31.6(3) . . . . ? C4 Sc1 C5 C6 -135.3(4) . . . . ? C9 Sc1 C5 C6 -157.4(3) . . . . ? C8 Sc1 C5 C6 -145.1(3) . . . . ? C7 Sc1 C5 C6 149.3(5) . . . . ? O2 Sc1 C5 C4 73.3(3) . . . . ? O1 Sc1 C5 C4 -105.9(3) . . . . ? C1 Sc1 C5 C4 166.9(3) . . . . ? C9 Sc1 C5 C4 -22.1(3) . . . . ? C8 Sc1 C5 C4 -9.8(4) . . . . ? C7 Sc1 C5 C4 -75.4(7) . . . . ? C6 Sc1 C5 C4 135.3(4) . . . . ? C4 C5 C6 Sc1 -56.0(4) . . . . ? O2 Sc1 C6 C5 119.8(3) . . . . ? O1 Sc1 C6 C5 -60.4(3) . . . . ? C1 Sc1 C6 C5 -148.3(3) . . . . ? C4 Sc1 C6 C5 26.4(3) . . . . ? C9 Sc1 C6 C5 33.8(4) . . . . ? C8 Sc1 C6 C5 93.4(6) . . . . ? C7 Sc1 C6 C5 -160.1(4) . . . . ? O2 Sc1 C7 C8 -63.8(3) . . . . ? O1 Sc1 C7 C8 115.7(3) . . . . ? C1 Sc1 C7 C8 -154.6(3) . . . . ? C4 Sc1 C7 C8 27.9(4) . . . . ? C9 Sc1 C7 C8 26.8(3) . . . . ? C5 Sc1 C7 C8 85.7(7) . . . . ? C6 Sc1 C7 C8 -143.0(4) . . . . ? Sc1 C7 C8 C9 -54.3(4) . . . . ? O2 Sc1 C8 C7 112.9(3) . . . . ? O1 Sc1 C8 C7 -66.5(3) . . . . ? C1 Sc1 C8 C7 27.4(3) . . . . ? C4 Sc1 C8 C7 -161.8(3) . . . . ? C9 Sc1 C8 C7 -135.1(5) . . . . ? C5 Sc1 C8 C7 -156.1(3) . . . . ? C6 Sc1 C8 C7 140.0(4) . . . . ? O2 Sc1 C8 C9 -112.0(3) . . . . ? O1 Sc1 C8 C9 68.6(3) . . . . ? C1 Sc1 C8 C9 162.5(3) . . . . ? C4 Sc1 C8 C9 -26.6(3) . . . . ? C5 Sc1 C8 C9 -20.9(4) . . . . ? C7 Sc1 C8 C9 135.1(5) . . . . ? C6 Sc1 C8 C9 -84.8(6) . . . . ? C7 C8 C9 Sc1 55.4(4) . . . . ? O2 Sc1 C9 C8 64.6(3) . . . . ? O1 Sc1 C9 C8 -113.9(3) . . . . ? C1 Sc1 C9 C8 -27.7(4) . . . . ? C4 Sc1 C9 C8 155.2(3) . . . . ? C5 Sc1 C9 C8 167.1(3) . . . . ? C7 Sc1 C9 C8 -25.5(3) . . . . ? C6 Sc1 C9 C8 148.9(3) . . . . ? C13 O1 C10 C11 24.7(6) . . . . ? Sc1 O1 C10 C11 -159.2(4) . . . . ? O1 C10 C11 C12 -30.6(6) . . . . ? C10 C11 C12 C13 24.8(6) . . . . ? C10 O1 C13 C12 -8.4(5) . . . . ? Sc1 O1 C13 C12 175.6(2) . . . . ? C11 C12 C13 O1 -9.5(4) . . . . ? C17 O2 C14 C15 -13.6(4) . . . . ? Sc1 O2 C14 C15 179.9(2) . . . . ? O2 C14 C15 C16 35.0(4) . . . . ? C14 C15 C16 C17 -42.6(4) . . . . ? C14 O2 C17 C16 -13.6(4) . . . . ? Sc1 O2 C17 C16 154.3(2) . . . . ? C15 C16 C17 O2 34.7(4) . . . . ? O4 Sc2 C18 C19 85.0(3) . . . . ? O3 Sc2 C18 C19 -93.3(3) . . . . ? C26 Sc2 C18 C19 178.0(3) . . . . ? C25B Sc2 C18 C19 163.2(4) . . . . ? C23 Sc2 C18 C19 -2.4(5) . . . . ? C22 Sc2 C18 C19 -17.6(4) . . . . ? C25A Sc2 C18 C19 -171.9(3) . . . . ? C21 Sc2 C18 C19 -1.8(3) . . . . ? C24 Sc2 C18 C19 173.6(3) . . . . ? Sc2 C18 C19 C20 -110.9(5) . . . . ? O4 Sc2 C21 C22 115.4(3) . . . . ? O3 Sc2 C21 C22 -65.6(3) . . . . ? C18 Sc2 C21 C22 -153.5(3) . . . . ? C26 Sc2 C21 C22 26.8(4) . . . . ? C25B Sc2 C21 C22 92.8(11) . . . . ? C23 Sc2 C21 C22 26.1(2) . . . . ? C25A Sc2 C21 C22 -22.7(9) . . . . ? C24 Sc2 C21 C22 -167.4(5) . . . . ? Sc2 C21 C22 C23 -55.7(4) . . . . ? O4 Sc2 C22 C23 68.2(3) . . . . ? O3 Sc2 C22 C23 -113.5(3) . . . . ? C18 Sc2 C22 C23 164.5(2) . . . . ? C26 Sc2 C22 C23 -27.2(3) . . . . ? C25B Sc2 C22 C23 -16.8(7) . . . . ? C25A Sc2 C22 C23 -51.9(4) . . . . ? C21 Sc2 C22 C23 135.0(4) . . . . ? C24 Sc2 C22 C23 -60.3(7) . . . . ? O4 Sc2 C22 C21 -66.8(3) . . . . ? O3 Sc2 C22 C21 111.5(3) . . . . ? C18 Sc2 C22 C21 29.5(3) . . . . ? C26 Sc2 C22 C21 -162.2(3) . . . . ? C25B Sc2 C22 C21 -151.7(6) . . . . ? C23 Sc2 C22 C21 -135.0(4) . . . . ? C25A Sc2 C22 C21 173.2(3) . . . . ? C24 Sc2 C22 C21 164.7(5) . . . . ? C21 C22 C23 Sc2 56.2(4) . . . . ? O4 Sc2 C23 C22 -114.2(3) . . . . ? O3 Sc2 C23 C22 63.8(3) . . . . ? C18 Sc2 C23 C22 -25.9(4) . . . . ? C26 Sc2 C23 C22 153.9(3) . . . . ? C25B Sc2 C23 C22 169.4(4) . . . . ? C25A Sc2 C23 C22 143.2(3) . . . . ? C21 Sc2 C23 C22 -26.6(3) . . . . ? C24 Sc2 C23 C22 159.8(3) . . . . ? O4 Sc2 C24 C25B -65.4(7) . . . . ? O3 Sc2 C24 C25B 116.0(7) . . . . ? C18 Sc2 C24 C25B -156.6(8) . . . . ? C26 Sc2 C24 C25B 27.1(7) . . . . ? C23 Sc2 C24 C25B 20.2(8) . . . . ? C22 Sc2 C24 C25B 64.4(10) . . . . ? C25A Sc2 C24 C25B 52.4(7) . . . . ? C21 Sc2 C24 C25B -142.3(8) . . . . ? O4 Sc2 C24 C25A -117.7(4) . . . . ? O3 Sc2 C24 C25A 63.7(4) . . . . ? C18 Sc2 C24 C25A 151.1(4) . . . . ? C26 Sc2 C24 C25A -25.3(3) . . . . ? C25B Sc2 C24 C25A -52.4(7) . . . . ? C23 Sc2 C24 C25A -32.2(5) . . . . ? C22 Sc2 C24 C25A 12.0(8) . . . . ? C21 Sc2 C24 C25A 165.3(4) . . . . ? C25B C24 C25A C26 -25.5(9) . . . . ? Sc2 C24 C25A C26 54.9(6) . . . . ? C25B C24 C25A Sc2 -80.4(9) . . . . ? O4 Sc2 C25A C24 65.0(4) . . . . ? O3 Sc2 C25A C24 -114.3(4) . . . . ? C18 Sc2 C25A C24 -28.7(4) . . . . ? C26 Sc2 C25A C24 137.9(6) . . . . ? C25B Sc2 C25A C24 59.3(8) . . . . ? C23 Sc2 C25A C24 157.4(3) . . . . ? C22 Sc2 C25A C24 -175.5(3) . . . . ? C21 Sc2 C25A C24 -158.1(6) . . . . ? O4 Sc2 C25A C26 -72.9(3) . . . . ? O3 Sc2 C25A C26 107.8(3) . . . . ? C18 Sc2 C25A C26 -166.6(3) . . . . ? C25B Sc2 C25A C26 -78.6(8) . . . . ? C23 Sc2 C25A C26 19.5(4) . . . . ? C22 Sc2 C25A C26 46.6(4) . . . . ? C21 Sc2 C25A C26 64.0(9) . . . . ? C24 Sc2 C25A C26 -137.9(6) . . . . ? C25A C24 C25B C26 24.5(9) . . . . ? Sc2 C24 C25B C26 -57.0(11) . . . . ? C25A C24 C25B Sc2 81.5(7) . . . . ? O4 Sc2 C25B C24 111.8(7) . . . . ? O3 Sc2 C25B C24 -67.5(7) . . . . ? C18 Sc2 C25B C24 23.1(7) . . . . ? C26 Sc2 C25B C24 -138.8(10) . . . . ? C23 Sc2 C25B C24 -165.5(6) . . . . ? C22 Sc2 C25B C24 -155.8(4) . . . . ? C25A Sc2 C25B C24 -73.9(9) . . . . ? C21 Sc2 C25B C24 134.8(9) . . . . ? O4 Sc2 C25B C26 -109.5(5) . . . . ? O3 Sc2 C25B C26 71.3(5) . . . . ? C18 Sc2 C25B C26 161.9(4) . . . . ? C23 Sc2 C25B C26 -26.7(6) . . . . ? C22 Sc2 C25B C26 -17.0(9) . . . . ? C25A Sc2 C25B C26 64.9(7) . . . . ? C21 Sc2 C25B C26 -86.4(12) . . . . ? C24 Sc2 C25B C26 138.8(10) . . . . ? C24 C25A C26 C25B 22.2(8) . . . . ? Sc2 C25A C26 C25B 79.7(8) . . . . ? C24 C25A C26 Sc2 -57.6(6) . . . . ? C24 C25B C26 C25A -26.4(10) . . . . ? Sc2 C25B C26 C25A -87.6(7) . . . . ? C24 C25B C26 Sc2 61.2(12) . . . . ? O4 Sc2 C26 C25A 111.0(3) . . . . ? O3 Sc2 C26 C25A -69.3(3) . . . . ? C18 Sc2 C26 C25A 18.4(4) . . . . ? C25B Sc2 C26 C25A 43.6(6) . . . . ? C23 Sc2 C26 C25A -161.4(3) . . . . ? C22 Sc2 C26 C25A -146.8(3) . . . . ? C21 Sc2 C26 C25A -162.1(3) . . . . ? C24 Sc2 C26 C25A 23.3(3) . . . . ? O4 Sc2 C26 C25B 67.4(6) . . . . ? O3 Sc2 C26 C25B -113.0(6) . . . . ? C18 Sc2 C26 C25B -25.3(6) . . . . ? C23 Sc2 C26 C25B 154.9(6) . . . . ? C22 Sc2 C26 C25B 169.5(6) . . . . ? C25A Sc2 C26 C25B -43.6(6) . . . . ? C21 Sc2 C26 C25B 154.3(6) . . . . ? C24 Sc2 C26 C25B -20.4(6) . . . . ? C30 O3 C27 C28 0.2(5) . . . . ? Sc2 O3 C27 C28 163.3(3) . . . . ? O3 C27 C28 C29B -14.3(7) . . . . ? O3 C27 C28 C29A 11.1(6) . . . . ? C29B C28 C29A C30 82.8(14) . . . . ? C27 C28 C29A C30 -18.7(8) . . . . ? C27 C28 C29B C30 21.6(8) . . . . ? C29A C28 C29B C30 -64.6(12) . . . . ? C28 C29A C30 O3 19.4(7) . . . . ? C28 C29A C30 C29B -62.4(12) . . . . ? C27 O3 C30 C29A -12.8(6) . . . . ? Sc2 O3 C30 C29A -175.0(4) . . . . ? C27 O3 C30 C29B 12.1(6) . . . . ? Sc2 O3 C30 C29B -150.1(4) . . . . ? C28 C29B C30 C29A 84.8(14) . . . . ? C28 C29B C30 O3 -21.0(8) . . . . ? C34 O4 C31 C32 5.3(4) . . . . ? Sc2 O4 C31 C32 -176.3(3) . . . . ? O4 C31 C32 C33 -28.4(4) . . . . ? C31 C32 C33 C34 40.4(4) . . . . ? C31 O4 C34 C33 20.9(4) . . . . ? Sc2 O4 C34 C33 -157.2(3) . . . . ? C32 C33 C34 O4 -37.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.71 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.565 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.125 #==END data_2a _database_code_depnum_ccdc_archive 'CCDC 832189' #TrackingRef '- CC-Scallyl_revised_08-09-2011.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H34 O3 Sc, C24 H20 B' _chemical_formula_sum 'C42 H54 B O3 Sc' _chemical_formula_weight 662.62 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' B B 0.0013 0.0007 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.6886(18) _cell_length_b 9.9269(6) _cell_length_c 23.1586(13) _cell_angle_alpha 90.00 _cell_angle_beta 93.9940(10) _cell_angle_gamma 90.00 _cell_volume 7267.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6428 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.55 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 0.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9143 _exptl_absorpt_correction_T_max 0.9380 _exptl_absorpt_process_details 'Platon Mulabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'APEX Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53345 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.49 _reflns_number_total 10704 _reflns_number_gt 7566 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10704 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.585219(9) 0.45592(3) 0.859926(12) 0.01543(8) Uani 1 1 d . . . O1 O 0.61919(3) 0.62309(10) 0.82332(4) 0.0202(2) Uani 1 1 d . A . O2 O 0.63824(3) 0.45050(10) 0.92897(4) 0.0185(2) Uani 1 1 d . A . O3 O 0.55479(3) 0.28651(10) 0.90268(4) 0.0198(2) Uani 1 1 d . A . B1 B 0.64590(5) 0.09890(17) 0.60386(7) 0.0162(3) Uani 1 1 d . . . C1 C 0.62805(6) 0.27864(16) 0.81374(7) 0.0292(4) Uani 1 1 d . A . H1A H 0.6131 0.2391 0.8436 0.035 Uiso 1 1 calc R . . H1B H 0.6579 0.2690 0.8140 0.035 Uiso 1 1 calc R . . C2 C 0.60642(6) 0.35005(17) 0.77006(7) 0.0294(4) Uani 1 1 d . A . H2 H 0.6225 0.3880 0.7410 0.035 Uiso 1 1 calc R . . C3 C 0.56319(6) 0.37100(17) 0.76501(7) 0.0279(4) Uani 1 1 d . A . H3A H 0.5459 0.3348 0.7931 0.033 Uiso 1 1 calc R . . H3B H 0.5508 0.4216 0.7334 0.033 Uiso 1 1 calc R . . C4 C 0.51846(5) 0.56364(16) 0.84041(7) 0.0267(4) Uani 1 1 d . A . H4A H 0.5137 0.4703 0.8462 0.032 Uiso 0.763(5) 1 calc PR A 1 H4B H 0.5100 0.6042 0.8043 0.032 Uiso 0.763(5) 1 calc PR A 1 H4C H 0.5400 0.6041 0.8197 0.032 Uiso 0.237(5) 1 calc PR A 2 H4D H 0.4941 0.5270 0.8200 0.032 Uiso 0.237(5) 1 calc PR A 2 C5A C 0.53821(7) 0.6424(2) 0.88564(10) 0.0240(6) Uani 0.763(5) 1 d P A 1 H5A H 0.5423 0.7352 0.8778 0.029 Uiso 0.763(5) 1 calc PR A 1 C5B C 0.5228(2) 0.5579(7) 0.9024(3) 0.026(2) Uani 0.237(5) 1 d P A 2 H5B H 0.4998 0.5158 0.9195 0.032 Uiso 0.237(5) 1 calc PR A 2 C6 C 0.55164(6) 0.59886(18) 0.93811(8) 0.0340(4) Uani 1 1 d . A . H6A H 0.5483 0.5068 0.9481 0.041 Uiso 0.763(5) 1 calc PR A 1 H6B H 0.5646 0.6598 0.9656 0.041 Uiso 0.763(5) 1 calc PR A 1 H6C H 0.5759 0.6422 0.9248 0.041 Uiso 0.237(5) 1 calc PR A 2 H6D H 0.5492 0.5864 0.9784 0.041 Uiso 0.237(5) 1 calc PR A 2 C7 C 0.60168(5) 0.71087(17) 0.77600(8) 0.0294(4) Uani 1 1 d . . . H7A H 0.5802 0.7728 0.7902 0.035 Uiso 1 1 calc R A . H7B H 0.5883 0.6562 0.7440 0.035 Uiso 1 1 calc R . . C8 C 0.63878(5) 0.78896(16) 0.75581(7) 0.0248(4) Uani 1 1 d . A . H8A H 0.6429 0.8745 0.7775 0.030 Uiso 1 1 calc R . . H8B H 0.6350 0.8089 0.7139 0.030 Uiso 1 1 calc R . . C9 C 0.67558(5) 0.69297(17) 0.76906(7) 0.0286(4) Uani 1 1 d . . . H9A H 0.6768 0.6234 0.7386 0.034 Uiso 1 1 calc R A . H9B H 0.7028 0.7421 0.7728 0.034 Uiso 1 1 calc R . . C10 C 0.66552(5) 0.63108(16) 0.82603(7) 0.0211(3) Uani 1 1 d . A . H10A H 0.6783 0.5403 0.8306 0.025 Uiso 1 1 calc R . . H10B H 0.6763 0.6883 0.8588 0.025 Uiso 1 1 calc R . . C11 C 0.65108(5) 0.56634(15) 0.96588(7) 0.0204(3) Uani 1 1 d . . . H11A H 0.6366 0.5647 1.0024 0.024 Uiso 1 1 calc R A . H11B H 0.6445 0.6523 0.9456 0.024 Uiso 1 1 calc R . . C12 C 0.69810(5) 0.54907(17) 0.97758(7) 0.0263(4) Uani 1 1 d . A . H12A H 0.7086 0.5971 1.0132 0.032 Uiso 1 1 calc R . . H12B H 0.7137 0.5814 0.9447 0.032 Uiso 1 1 calc R . . C13 C 0.70208(5) 0.39690(17) 0.98484(7) 0.0285(4) Uani 1 1 d . . . H13A H 0.7309 0.3657 0.9773 0.034 Uiso 1 1 calc R A . H13B H 0.6956 0.3688 1.0243 0.034 Uiso 1 1 calc R . . C14 C 0.66966(6) 0.34317(18) 0.94002(9) 0.0358(4) Uani 1 1 d . A . H14A H 0.6831 0.3200 0.9040 0.043 Uiso 1 1 calc R . . H14B H 0.6560 0.2613 0.9546 0.043 Uiso 1 1 calc R . . C15 C 0.52217(5) 0.19411(16) 0.87763(7) 0.0242(4) Uani 1 1 d . . . H15A H 0.5340 0.1352 0.8483 0.029 Uiso 1 1 calc R A . H15B H 0.4981 0.2454 0.8589 0.029 Uiso 1 1 calc R . . C16 C 0.50779(5) 0.11105(16) 0.92746(7) 0.0235(3) Uani 1 1 d . A . H16A H 0.5223 0.0227 0.9298 0.028 Uiso 1 1 calc R . . H16B H 0.4768 0.0962 0.9236 0.028 Uiso 1 1 calc R . . C17 C 0.52038(5) 0.19706(17) 0.98012(7) 0.0269(4) Uani 1 1 d . . . H17A H 0.4993 0.2686 0.9856 0.032 Uiso 1 1 calc R A . H17B H 0.5239 0.1417 1.0157 0.032 Uiso 1 1 calc R . . C18 C 0.56203(5) 0.25576(16) 0.96429(6) 0.0227(3) Uani 1 1 d . A . H18A H 0.5691 0.3383 0.9869 0.027 Uiso 1 1 calc R . . H18B H 0.5853 0.1898 0.9711 0.027 Uiso 1 1 calc R . . C19 C 0.60459(4) 0.02443(14) 0.62871(6) 0.0157(3) Uani 1 1 d . . . C20 C 0.58540(5) 0.07444(15) 0.67711(7) 0.0190(3) Uani 1 1 d . . . H20 H 0.5952 0.1574 0.6935 0.023 Uiso 1 1 calc R . . C21 C 0.55268(5) 0.00801(16) 0.70218(7) 0.0211(3) Uani 1 1 d . . . H21 H 0.5405 0.0461 0.7348 0.025 Uiso 1 1 calc R . . C22 C 0.53780(5) -0.11386(16) 0.67969(7) 0.0216(3) Uani 1 1 d . . . H22 H 0.5152 -0.1594 0.6963 0.026 Uiso 1 1 calc R . . C23 C 0.55645(5) -0.16821(15) 0.63254(7) 0.0193(3) Uani 1 1 d . . . H23 H 0.5468 -0.2522 0.6170 0.023 Uiso 1 1 calc R . . C24 C 0.58913(5) -0.10033(14) 0.60796(6) 0.0171(3) Uani 1 1 d . . . H24 H 0.6015 -0.1399 0.5758 0.021 Uiso 1 1 calc R . . C25 C 0.68587(5) 0.02972(14) 0.64197(6) 0.0174(3) Uani 1 1 d . . . C26 C 0.70618(5) -0.08754(15) 0.62483(7) 0.0214(3) Uani 1 1 d . . . H26 H 0.6979 -0.1254 0.5881 0.026 Uiso 1 1 calc R . . C27 C 0.73800(5) -0.15104(17) 0.65947(8) 0.0264(4) Uani 1 1 d . . . H27 H 0.7510 -0.2303 0.6460 0.032 Uiso 1 1 calc R . . C28 C 0.75074(5) -0.09909(17) 0.71333(8) 0.0287(4) Uani 1 1 d . . . H28 H 0.7729 -0.1405 0.7367 0.034 Uiso 1 1 calc R . . C29 C 0.73055(5) 0.01433(17) 0.73260(7) 0.0276(4) Uani 1 1 d . . . H29 H 0.7384 0.0499 0.7699 0.033 Uiso 1 1 calc R . . C30 C 0.69890(5) 0.07630(16) 0.69771(7) 0.0222(3) Uani 1 1 d . . . H30 H 0.6854 0.1536 0.7121 0.027 Uiso 1 1 calc R . . C31 C 0.64361(5) 0.26338(15) 0.61284(6) 0.0177(3) Uani 1 1 d . . . C32 C 0.67961(5) 0.34344(15) 0.62472(6) 0.0219(3) Uani 1 1 d . . . H32 H 0.7065 0.3009 0.6297 0.026 Uiso 1 1 calc R . . C33 C 0.67740(6) 0.48306(16) 0.62948(7) 0.0264(4) Uani 1 1 d . . . H33 H 0.7026 0.5336 0.6376 0.032 Uiso 1 1 calc R . . C34 C 0.63896(6) 0.54858(16) 0.62248(7) 0.0281(4) Uani 1 1 d . . . H34 H 0.6374 0.6437 0.6262 0.034 Uiso 1 1 calc R . . C35 C 0.60278(6) 0.47324(16) 0.61003(7) 0.0258(4) Uani 1 1 d . . . H35 H 0.5761 0.5169 0.6047 0.031 Uiso 1 1 calc R . . C36 C 0.60524(5) 0.33419(15) 0.60524(6) 0.0209(3) Uani 1 1 d . . . H36 H 0.5799 0.2848 0.5965 0.025 Uiso 1 1 calc R . . C37 C 0.64914(5) 0.07831(14) 0.53376(6) 0.0169(3) Uani 1 1 d . . . C38 C 0.61390(5) 0.07015(15) 0.49387(7) 0.0209(3) Uani 1 1 d . . . H38 H 0.5864 0.0730 0.5079 0.025 Uiso 1 1 calc R . . C39 C 0.61748(6) 0.05807(15) 0.43443(7) 0.0252(4) Uani 1 1 d . . . H39 H 0.5927 0.0530 0.4090 0.030 Uiso 1 1 calc R . . C40 C 0.65682(6) 0.05340(16) 0.41229(7) 0.0267(4) Uani 1 1 d . . . H40 H 0.6594 0.0422 0.3719 0.032 Uiso 1 1 calc R . . C41 C 0.69234(6) 0.06530(17) 0.44990(7) 0.0282(4) Uani 1 1 d . . . H41 H 0.7196 0.0643 0.4353 0.034 Uiso 1 1 calc R . . C42 C 0.68835(5) 0.07872(16) 0.50910(7) 0.0232(3) Uani 1 1 d . . . H42 H 0.7133 0.0886 0.5339 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.01527(14) 0.01484(14) 0.01648(15) 0.00014(11) 0.00325(11) 0.00053(11) O1 0.0189(5) 0.0203(5) 0.0217(6) 0.0057(4) 0.0029(4) 0.0005(4) O2 0.0166(5) 0.0179(5) 0.0210(6) -0.0012(4) 0.0016(4) 0.0034(4) O3 0.0211(6) 0.0214(6) 0.0169(5) 0.0005(4) 0.0019(4) -0.0064(4) B1 0.0156(8) 0.0151(8) 0.0180(8) -0.0010(6) 0.0025(7) -0.0007(6) C1 0.0314(10) 0.0302(9) 0.0271(9) -0.0079(7) 0.0107(8) 0.0028(8) C2 0.0431(11) 0.0257(9) 0.0212(9) -0.0091(7) 0.0143(8) -0.0039(8) C3 0.0384(10) 0.0278(9) 0.0179(8) -0.0031(7) 0.0051(7) -0.0010(8) C4 0.0242(9) 0.0255(9) 0.0297(9) -0.0018(7) -0.0034(7) 0.0086(7) C5A 0.0188(11) 0.0168(12) 0.0370(14) -0.0040(9) 0.0063(9) 0.0067(9) C5B 0.018(4) 0.023(4) 0.039(5) -0.008(3) 0.007(3) 0.011(3) C6 0.0307(10) 0.0324(10) 0.0384(11) -0.0131(8) -0.0019(8) 0.0138(8) C7 0.0290(9) 0.0281(9) 0.0306(9) 0.0155(7) -0.0021(7) -0.0003(7) C8 0.0336(9) 0.0211(8) 0.0198(8) 0.0043(6) 0.0038(7) -0.0042(7) C9 0.0296(9) 0.0316(9) 0.0259(9) 0.0069(7) 0.0099(7) -0.0013(8) C10 0.0176(8) 0.0231(8) 0.0231(8) 0.0028(6) 0.0049(6) -0.0009(6) C11 0.0218(8) 0.0221(8) 0.0174(8) -0.0029(6) 0.0024(6) -0.0001(6) C12 0.0206(8) 0.0335(9) 0.0244(9) -0.0021(7) -0.0011(7) -0.0013(7) C13 0.0240(9) 0.0365(10) 0.0246(9) -0.0001(7) -0.0002(7) 0.0083(8) C14 0.0254(9) 0.0291(10) 0.0516(12) -0.0020(9) -0.0061(9) 0.0101(8) C15 0.0234(8) 0.0250(8) 0.0241(8) -0.0002(7) 0.0006(7) -0.0101(7) C16 0.0183(8) 0.0253(8) 0.0270(9) 0.0043(7) 0.0031(7) -0.0047(7) C17 0.0260(9) 0.0329(9) 0.0225(8) 0.0043(7) 0.0073(7) -0.0025(7) C18 0.0239(8) 0.0251(8) 0.0189(8) 0.0040(6) -0.0002(7) -0.0027(7) C19 0.0140(7) 0.0153(7) 0.0176(7) 0.0012(6) 0.0010(6) 0.0020(6) C20 0.0199(8) 0.0165(7) 0.0206(8) -0.0017(6) 0.0023(6) -0.0010(6) C21 0.0207(8) 0.0238(8) 0.0195(8) -0.0006(6) 0.0065(6) 0.0019(6) C22 0.0172(8) 0.0237(8) 0.0242(8) 0.0049(6) 0.0045(6) -0.0031(6) C23 0.0189(8) 0.0151(7) 0.0237(8) 0.0002(6) -0.0003(6) -0.0018(6) C24 0.0170(7) 0.0166(7) 0.0176(7) -0.0008(6) 0.0010(6) 0.0014(6) C25 0.0138(7) 0.0173(7) 0.0213(8) 0.0021(6) 0.0036(6) -0.0036(6) C26 0.0183(8) 0.0210(8) 0.0255(8) 0.0017(6) 0.0056(7) -0.0004(6) C27 0.0194(8) 0.0246(8) 0.0364(10) 0.0101(7) 0.0101(7) 0.0033(7) C28 0.0157(8) 0.0322(9) 0.0380(10) 0.0181(8) 0.0001(7) -0.0020(7) C29 0.0244(9) 0.0322(9) 0.0255(9) 0.0063(7) -0.0041(7) -0.0071(7) C30 0.0205(8) 0.0218(8) 0.0242(8) 0.0016(6) 0.0004(7) -0.0028(6) C31 0.0218(8) 0.0168(7) 0.0151(7) 0.0002(6) 0.0041(6) -0.0007(6) C32 0.0235(8) 0.0211(8) 0.0212(8) 0.0007(6) 0.0019(7) -0.0026(7) C33 0.0354(10) 0.0212(8) 0.0228(9) -0.0016(7) 0.0029(7) -0.0091(7) C34 0.0478(11) 0.0143(8) 0.0229(9) -0.0022(6) 0.0087(8) 0.0010(7) C35 0.0325(9) 0.0220(8) 0.0241(9) 0.0024(7) 0.0096(7) 0.0076(7) C36 0.0226(8) 0.0199(8) 0.0205(8) 0.0013(6) 0.0046(6) 0.0006(6) C37 0.0193(8) 0.0117(7) 0.0198(8) 0.0001(6) 0.0026(6) -0.0001(6) C38 0.0202(8) 0.0190(8) 0.0236(8) 0.0024(6) 0.0022(6) -0.0017(6) C39 0.0315(9) 0.0220(8) 0.0213(8) 0.0036(6) -0.0047(7) -0.0046(7) C40 0.0412(10) 0.0216(8) 0.0176(8) 0.0015(6) 0.0051(7) -0.0005(7) C41 0.0265(9) 0.0334(10) 0.0260(9) 0.0041(7) 0.0104(7) 0.0040(7) C42 0.0199(8) 0.0283(9) 0.0216(8) 0.0013(7) 0.0021(7) 0.0011(7) _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 Sc1 O1 2.1814(10) . ? Sc1 O3 2.2071(10) . ? Sc1 O2 2.2379(10) . ? Sc1 C4 2.3854(16) . ? Sc1 C3 2.4117(16) . ? Sc1 C2 2.4662(16) . ? Sc1 C5A 2.474(2) . ? Sc1 C5B 2.486(6) . ? Sc1 C1 2.5071(16) . ? Sc1 C6 2.5870(17) . ? O1 C10 1.4671(18) . ? O1 C7 1.4778(18) . ? O2 C14 1.4684(19) . ? O2 C11 1.4732(17) . ? O3 C18 1.4615(17) . ? O3 C15 1.4706(18) . ? B1 C19 1.642(2) . ? B1 C25 1.643(2) . ? B1 C37 1.647(2) . ? B1 C31 1.648(2) . ? C1 C2 1.378(2) . ? C1 H1A 0.9500 . ? C1 H1B 0.9500 . ? C2 C3 1.382(2) . ? C2 H2 0.9500 . ? C3 H3A 0.9500 . ? C3 H3B 0.9500 . ? C4 C5A 1.417(3) . ? C4 C5B 1.434(8) . ? C4 H4A 0.9500 . ? C4 H4B 0.9500 . ? C4 H4C 0.9500 . ? C4 H4D 0.9500 . ? C5A C6 1.331(3) . ? C5A H5A 0.9500 . ? C5B C6 1.257(7) . ? C5B H5B 0.9500 . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C6 H6C 0.9500 . ? C6 H6D 0.9500 . ? C7 C8 1.509(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.521(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.509(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.506(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.524(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.506(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.514(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.519(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.511(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.403(2) . ? C19 C24 1.4043(19) . ? C20 C21 1.390(2) . ? C20 H20 0.9500 . ? C21 C22 1.387(2) . ? C21 H21 0.9500 . ? C22 C23 1.387(2) . ? C22 H22 0.9500 . ? C23 C24 1.390(2) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.401(2) . ? C25 C30 1.406(2) . ? C26 C27 1.395(2) . ? C26 H26 0.9500 . ? C27 C28 1.384(2) . ? C27 H27 0.9500 . ? C28 C29 1.384(2) . ? C28 H28 0.9500 . ? C29 C30 1.387(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.402(2) . ? C31 C36 1.405(2) . ? C32 C33 1.393(2) . ? C32 H32 0.9500 . ? C33 C34 1.380(2) . ? C33 H33 0.9500 . ? C34 C35 1.382(2) . ? C34 H34 0.9500 . ? C35 C36 1.387(2) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.401(2) . ? C37 C42 1.403(2) . ? C38 C39 1.394(2) . ? C38 H38 0.9500 . ? C39 C40 1.382(2) . ? C39 H39 0.9500 . ? C40 C41 1.379(2) . ? C40 H40 0.9500 . ? C41 C42 1.392(2) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? 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 Sc1 O3 175.44(4) . . ? O1 Sc1 O2 85.96(4) . . ? O3 Sc1 O2 89.48(4) . . ? O1 Sc1 C4 92.32(5) . . ? O3 Sc1 C4 90.98(5) . . ? O2 Sc1 C4 139.29(5) . . ? O1 Sc1 C3 91.78(5) . . ? O3 Sc1 C3 92.00(5) . . ? O2 Sc1 C3 142.94(5) . . ? C4 Sc1 C3 77.72(6) . . ? O1 Sc1 C2 79.95(5) . . ? O3 Sc1 C2 101.95(5) . . ? O2 Sc1 C2 110.95(5) . . ? C4 Sc1 C2 108.74(6) . . ? C3 Sc1 C2 32.90(6) . . ? O1 Sc1 C5A 81.15(6) . . ? O3 Sc1 C5A 99.95(6) . . ? O2 Sc1 C5A 106.30(6) . . ? C4 Sc1 C5A 33.85(6) . . ? C3 Sc1 C5A 109.87(7) . . ? C2 Sc1 C5A 136.54(7) . . ? O1 Sc1 C5B 105.77(19) . . ? O3 Sc1 C5B 75.42(19) . . ? O2 Sc1 C5B 107.81(18) . . ? C4 Sc1 C5B 34.15(18) . . ? C3 Sc1 C5B 108.37(18) . . ? C2 Sc1 C5B 141.14(18) . . ? C5A Sc1 C5B 24.62(18) . . ? O1 Sc1 C1 94.11(5) . . ? O3 Sc1 C1 85.58(5) . . ? O2 Sc1 C1 83.46(5) . . ? C4 Sc1 C1 137.15(6) . . ? C3 Sc1 C1 59.78(6) . . ? C2 Sc1 C1 32.16(6) . . ? C5A Sc1 C1 168.69(7) . . ? C5B Sc1 C1 157.56(19) . . ? O1 Sc1 C6 95.33(5) . . ? O3 Sc1 C6 83.69(5) . . ? O2 Sc1 C6 80.69(5) . . ? C4 Sc1 C6 58.94(6) . . ? C3 Sc1 C6 136.27(6) . . ? C2 Sc1 C6 166.88(6) . . ? C5A Sc1 C6 30.39(6) . . ? C5B Sc1 C6 28.60(17) . . ? C1 Sc1 C6 160.90(6) . . ? C10 O1 C7 108.83(11) . . ? C10 O1 Sc1 122.95(8) . . ? C7 O1 Sc1 124.53(9) . . ? C14 O2 C11 107.98(12) . . ? C14 O2 Sc1 127.46(9) . . ? C11 O2 Sc1 123.99(8) . . ? C18 O3 C15 108.25(11) . . ? C18 O3 Sc1 123.59(9) . . ? C15 O3 Sc1 127.97(9) . . ? C19 B1 C25 103.13(11) . . ? C19 B1 C37 113.31(12) . . ? C25 B1 C37 112.28(12) . . ? C19 B1 C31 111.01(12) . . ? C25 B1 C31 112.67(12) . . ? C37 B1 C31 104.69(11) . . ? C2 C1 Sc1 72.29(9) . . ? C2 C1 H1A 120.0 . . ? Sc1 C1 H1A 70.6 . . ? C2 C1 H1B 120.0 . . ? Sc1 C1 H1B 129.5 . . ? H1A C1 H1B 120.0 . . ? C1 C2 C3 125.37(16) . . ? C1 C2 Sc1 75.56(9) . . ? C3 C2 Sc1 71.38(9) . . ? C1 C2 H2 117.3 . . ? C3 C2 H2 117.3 . . ? Sc1 C2 H2 128.3 . . ? C2 C3 Sc1 75.72(10) . . ? C2 C3 H3A 120.0 . . ? Sc1 C3 H3A 69.6 . . ? C2 C3 H3B 120.0 . . ? Sc1 C3 H3B 126.5 . . ? H3A C3 H3B 120.0 . . ? C5A C4 Sc1 76.52(10) . . ? C5B C4 Sc1 76.8(3) . . ? C5A C4 H4A 120.0 . . ? C5B C4 H4A 79.9 . . ? Sc1 C4 H4A 71.5 . . ? C5A C4 H4B 120.0 . . ? C5B C4 H4B 154.1 . . ? Sc1 C4 H4B 123.4 . . ? H4A C4 H4B 120.0 . . ? C5A C4 H4C 81.0 . . ? C5B C4 H4C 120.0 . . ? Sc1 C4 H4C 68.0 . . ? H4A C4 H4C 127.6 . . ? H4B C4 H4C 63.0 . . ? C5A C4 H4D 151.7 . . ? C5B C4 H4D 120.0 . . ? Sc1 C4 H4D 127.1 . . ? H4A C4 H4D 64.2 . . ? H4B C4 H4D 63.5 . . ? H4C C4 H4D 120.0 . . ? C6 C5A C4 126.3(2) . . ? C6 C5A Sc1 79.49(11) . . ? C4 C5A Sc1 69.63(10) . . ? C6 C5A H5A 116.8 . . ? C4 C5A H5A 116.8 . . ? Sc1 C5A H5A 126.0 . . ? C6 C5B C4 131.3(7) . . ? C6 C5B Sc1 80.2(3) . . ? C4 C5B Sc1 69.1(3) . . ? C6 C5B H5B 114.3 . . ? C4 C5B H5B 114.3 . . ? Sc1 C5B H5B 129.8 . . ? C5B C6 C5A 48.1(4) . . ? C5B C6 Sc1 71.2(3) . . ? C5A C6 Sc1 70.12(11) . . ? C5B C6 H6A 76.2 . . ? C5A C6 H6A 120.0 . . ? Sc1 C6 H6A 72.6 . . ? C5B C6 H6B 155.0 . . ? C5A C6 H6B 120.0 . . ? Sc1 C6 H6B 129.7 . . ? H6A C6 H6B 120.0 . . ? C5B C6 H6C 120.0 . . ? C5A C6 H6C 76.7 . . ? Sc1 C6 H6C 68.9 . . ? H6A C6 H6C 128.4 . . ? H6B C6 H6C 67.0 . . ? C5B C6 H6D 120.0 . . ? C5A C6 H6D 153.7 . . ? Sc1 C6 H6D 133.0 . . ? H6A C6 H6D 67.5 . . ? H6B C6 H6D 59.0 . . ? H6C C6 H6D 120.0 . . ? O1 C7 C8 105.80(13) . . ? O1 C7 H7A 110.6 . . ? C8 C7 H7A 110.6 . . ? O1 C7 H7B 110.6 . . ? C8 C7 H7B 110.6 . . ? H7A C7 H7B 108.7 . . ? C7 C8 C9 102.62(13) . . ? C7 C8 H8A 111.2 . . ? C9 C8 H8A 111.2 . . ? C7 C8 H8B 111.2 . . ? C9 C8 H8B 111.2 . . ? H8A C8 H8B 109.2 . . ? C10 C9 C8 103.05(13) . . ? C10 C9 H9A 111.2 . . ? C8 C9 H9A 111.2 . . ? C10 C9 H9B 111.2 . . ? C8 C9 H9B 111.2 . . ? H9A C9 H9B 109.1 . . ? O1 C10 C9 104.84(12) . . ? O1 C10 H10A 110.8 . . ? C9 C10 H10A 110.8 . . ? O1 C10 H10B 110.8 . . ? C9 C10 H10B 110.8 . . ? H10A C10 H10B 108.9 . . ? O2 C11 C12 104.21(12) . . ? O2 C11 H11A 110.9 . . ? C12 C11 H11A 110.9 . . ? O2 C11 H11B 110.9 . . ? C12 C11 H11B 110.9 . . ? H11A C11 H11B 108.9 . . ? C11 C12 C13 101.88(13) . . ? C11 C12 H12A 111.4 . . ? C13 C12 H12A 111.4 . . ? C11 C12 H12B 111.4 . . ? C13 C12 H12B 111.4 . . ? H12A C12 H12B 109.3 . . ? C14 C13 C12 103.17(13) . . ? C14 C13 H13A 111.1 . . ? C12 C13 H13A 111.1 . . ? C14 C13 H13B 111.1 . . ? C12 C13 H13B 111.1 . . ? H13A C13 H13B 109.1 . . ? O2 C14 C13 106.55(13) . . ? O2 C14 H14A 110.4 . . ? C13 C14 H14A 110.4 . . ? O2 C14 H14B 110.4 . . ? C13 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? O3 C15 C16 106.24(12) . . ? O3 C15 H15A 110.5 . . ? C16 C15 H15A 110.5 . . ? O3 C15 H15B 110.5 . . ? C16 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? C15 C16 C17 103.27(12) . . ? C15 C16 H16A 111.1 . . ? C17 C16 H16A 111.1 . . ? C15 C16 H16B 111.1 . . ? C17 C16 H16B 111.1 . . ? H16A C16 H16B 109.1 . . ? C18 C17 C16 101.95(13) . . ? C18 C17 H17A 111.4 . . ? C16 C17 H17A 111.4 . . ? C18 C17 H17B 111.4 . . ? C16 C17 H17B 111.4 . . ? H17A C17 H17B 109.2 . . ? O3 C18 C17 103.70(12) . . ? O3 C18 H18A 111.0 . . ? C17 C18 H18A 111.0 . . ? O3 C18 H18B 111.0 . . ? C17 C18 H18B 111.0 . . ? H18A C18 H18B 109.0 . . ? C20 C19 C24 115.16(13) . . ? C20 C19 B1 121.43(13) . . ? C24 C19 B1 123.01(13) . . ? C21 C20 C19 122.94(14) . . ? C21 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? C22 C21 C20 120.07(14) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 118.88(14) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 120.29(14) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 122.64(14) . . ? C23 C24 H24 118.7 . . ? C19 C24 H24 118.7 . . ? C26 C25 C30 114.98(14) . . ? C26 C25 B1 123.19(13) . . ? C30 C25 B1 121.45(13) . . ? C27 C26 C25 122.72(15) . . ? C27 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? C28 C27 C26 120.26(16) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 118.78(15) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C28 C29 C30 120.30(16) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 122.90(15) . . ? C29 C30 H30 118.6 . . ? C25 C30 H30 118.6 . . ? C32 C31 C36 115.24(14) . . ? C32 C31 B1 122.95(13) . . ? C36 C31 B1 121.68(13) . . ? C33 C32 C31 122.34(15) . . ? C33 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C34 C33 C32 120.57(16) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 118.80(15) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C34 C35 C36 120.30(16) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 122.73(15) . . ? C35 C36 H36 118.6 . . ? C31 C36 H36 118.6 . . ? C38 C37 C42 114.80(14) . . ? C38 C37 B1 123.76(13) . . ? C42 C37 B1 121.24(13) . . ? C39 C38 C37 122.69(15) . . ? C39 C38 H38 118.7 . . ? C37 C38 H38 118.7 . . ? C40 C39 C38 120.46(16) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C41 C40 C39 118.72(15) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C40 C41 C42 120.26(16) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C37 122.98(15) . . ? C41 C42 H42 118.5 . . ? C37 C42 H42 118.5 . . ? 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 C10 34.45(10) . . . . ? C4 Sc1 O1 C10 173.71(11) . . . . ? C3 Sc1 O1 C10 -108.51(11) . . . . ? C2 Sc1 O1 C10 -77.67(11) . . . . ? C5A Sc1 O1 C10 141.65(12) . . . . ? C5B Sc1 O1 C10 141.8(2) . . . . ? C1 Sc1 O1 C10 -48.68(11) . . . . ? C6 Sc1 O1 C10 114.69(11) . . . . ? O2 Sc1 O1 C7 -169.64(12) . . . . ? C4 Sc1 O1 C7 -30.39(12) . . . . ? C3 Sc1 O1 C7 47.40(12) . . . . ? C2 Sc1 O1 C7 78.24(12) . . . . ? C5A Sc1 O1 C7 -62.44(12) . . . . ? C5B Sc1 O1 C7 -62.3(2) . . . . ? C1 Sc1 O1 C7 107.22(12) . . . . ? C6 Sc1 O1 C7 -89.40(12) . . . . ? O1 Sc1 O2 C14 -113.49(13) . . . . ? O3 Sc1 O2 C14 66.74(13) . . . . ? C4 Sc1 O2 C14 157.64(13) . . . . ? C3 Sc1 O2 C14 -25.88(16) . . . . ? C2 Sc1 O2 C14 -35.87(14) . . . . ? C5A Sc1 O2 C14 166.95(13) . . . . ? C5B Sc1 O2 C14 141.2(2) . . . . ? C1 Sc1 O2 C14 -18.88(13) . . . . ? C6 Sc1 O2 C14 150.43(13) . . . . ? O1 Sc1 O2 C11 56.80(10) . . . . ? O3 Sc1 O2 C11 -122.97(10) . . . . ? C4 Sc1 O2 C11 -32.07(14) . . . . ? C3 Sc1 O2 C11 144.41(11) . . . . ? C2 Sc1 O2 C11 134.42(10) . . . . ? C5A Sc1 O2 C11 -22.75(12) . . . . ? C5B Sc1 O2 C11 -48.5(2) . . . . ? C1 Sc1 O2 C11 151.42(11) . . . . ? C6 Sc1 O2 C11 -39.28(11) . . . . ? O2 Sc1 O3 C18 24.74(11) . . . . ? C4 Sc1 O3 C18 -114.55(11) . . . . ? C3 Sc1 O3 C18 167.70(11) . . . . ? C2 Sc1 O3 C18 136.06(11) . . . . ? C5A Sc1 O3 C18 -81.72(12) . . . . ? C5B Sc1 O3 C18 -83.8(2) . . . . ? C1 Sc1 O3 C18 108.22(11) . . . . ? C6 Sc1 O3 C18 -55.95(11) . . . . ? O2 Sc1 O3 C15 -160.83(11) . . . . ? C4 Sc1 O3 C15 59.89(12) . . . . ? C3 Sc1 O3 C15 -17.86(12) . . . . ? C2 Sc1 O3 C15 -49.51(12) . . . . ? C5A Sc1 O3 C15 92.71(12) . . . . ? C5B Sc1 O3 C15 90.6(2) . . . . ? C1 Sc1 O3 C15 -77.35(12) . . . . ? C6 Sc1 O3 C15 118.49(12) . . . . ? O1 Sc1 C1 C2 -63.70(11) . . . . ? O3 Sc1 C1 C2 120.87(11) . . . . ? O2 Sc1 C1 C2 -149.15(11) . . . . ? C4 Sc1 C1 C2 34.19(14) . . . . ? C3 Sc1 C1 C2 25.97(10) . . . . ? C5A Sc1 C1 C2 1.0(4) . . . . ? C5B Sc1 C1 C2 88.9(5) . . . . ? C6 Sc1 C1 C2 176.83(16) . . . . ? Sc1 C1 C2 C3 -54.04(15) . . . . ? O1 Sc1 C2 C1 114.76(11) . . . . ? O3 Sc1 C2 C1 -61.02(11) . . . . ? O2 Sc1 C2 C1 33.06(11) . . . . ? C4 Sc1 C2 C1 -156.20(10) . . . . ? C3 Sc1 C2 C1 -135.85(16) . . . . ? C5A Sc1 C2 C1 -179.71(11) . . . . ? C5B Sc1 C2 C1 -142.5(3) . . . . ? C6 Sc1 C2 C1 -175.4(2) . . . . ? O1 Sc1 C2 C3 -109.40(10) . . . . ? O3 Sc1 C2 C3 74.83(10) . . . . ? O2 Sc1 C2 C3 168.91(9) . . . . ? C4 Sc1 C2 C3 -20.35(12) . . . . ? C5A Sc1 C2 C3 -43.86(15) . . . . ? C5B Sc1 C2 C3 -6.7(3) . . . . ? C1 Sc1 C2 C3 135.85(16) . . . . ? C6 Sc1 C2 C3 -39.6(3) . . . . ? C1 C2 C3 Sc1 55.81(16) . . . . ? O1 Sc1 C3 C2 68.31(10) . . . . ? O3 Sc1 C3 C2 -109.12(10) . . . . ? O2 Sc1 C3 C2 -17.35(15) . . . . ? C4 Sc1 C3 C2 160.30(11) . . . . ? C5A Sc1 C3 C2 149.55(11) . . . . ? C5B Sc1 C3 C2 175.6(2) . . . . ? C1 Sc1 C3 C2 -25.41(10) . . . . ? C6 Sc1 C3 C2 167.92(10) . . . . ? O1 Sc1 C4 C5A -70.32(13) . . . . ? O3 Sc1 C4 C5A 106.54(13) . . . . ? O2 Sc1 C4 C5A 16.19(16) . . . . ? C3 Sc1 C4 C5A -161.63(13) . . . . ? C2 Sc1 C4 C5A -150.49(12) . . . . ? C5B Sc1 C4 C5A 44.8(3) . . . . ? C1 Sc1 C4 C5A -168.90(12) . . . . ? C6 Sc1 C4 C5A 24.51(12) . . . . ? O1 Sc1 C4 C5B -115.1(3) . . . . ? O3 Sc1 C4 C5B 61.7(3) . . . . ? O2 Sc1 C4 C5B -28.6(4) . . . . ? C3 Sc1 C4 C5B 153.5(3) . . . . ? C2 Sc1 C4 C5B 164.7(3) . . . . ? C5A Sc1 C4 C5B -44.8(3) . . . . ? C1 Sc1 C4 C5B 146.3(3) . . . . ? C6 Sc1 C4 C5B -20.3(3) . . . . ? C5B C4 C5A C6 25.8(4) . . . . ? Sc1 C4 C5A C6 -59.02(19) . . . . ? C5B C4 C5A Sc1 84.9(4) . . . . ? O1 Sc1 C5A C6 -116.82(14) . . . . ? O3 Sc1 C5A C6 58.69(14) . . . . ? O2 Sc1 C5A C6 -33.70(14) . . . . ? C4 Sc1 C5A C6 135.4(2) . . . . ? C3 Sc1 C5A C6 154.48(13) . . . . ? C2 Sc1 C5A C6 178.08(11) . . . . ? C5B Sc1 C5A C6 63.6(4) . . . . ? C1 Sc1 C5A C6 177.3(3) . . . . ? O1 Sc1 C5A C4 107.80(12) . . . . ? O3 Sc1 C5A C4 -76.69(12) . . . . ? O2 Sc1 C5A C4 -169.07(11) . . . . ? C3 Sc1 C5A C4 19.11(14) . . . . ? C2 Sc1 C5A C4 42.70(17) . . . . ? C5B Sc1 C5A C4 -71.8(4) . . . . ? C1 Sc1 C5A C4 41.9(4) . . . . ? C6 Sc1 C5A C4 -135.4(2) . . . . ? C5A C4 C5B C6 -29.7(5) . . . . ? Sc1 C4 C5B C6 54.6(6) . . . . ? C5A C4 C5B Sc1 -84.3(3) . . . . ? O1 Sc1 C5B C6 -71.6(4) . . . . ? O3 Sc1 C5B C6 103.9(4) . . . . ? O2 Sc1 C5B C6 19.2(4) . . . . ? C4 Sc1 C5B C6 -141.6(6) . . . . ? C3 Sc1 C5B C6 -168.9(3) . . . . ? C2 Sc1 C5B C6 -165.08(18) . . . . ? C5A Sc1 C5B C6 -71.1(5) . . . . ? C1 Sc1 C5B C6 136.9(3) . . . . ? O1 Sc1 C5B C4 70.0(3) . . . . ? O3 Sc1 C5B C4 -114.5(3) . . . . ? O2 Sc1 C5B C4 160.8(2) . . . . ? C3 Sc1 C5B C4 -27.3(3) . . . . ? C2 Sc1 C5B C4 -23.5(5) . . . . ? C5A Sc1 C5B C4 70.5(4) . . . . ? C1 Sc1 C5B C4 -81.5(6) . . . . ? C6 Sc1 C5B C4 141.6(6) . . . . ? C4 C5B C6 C5A 29.2(5) . . . . ? Sc1 C5B C6 C5A 79.8(3) . . . . ? C4 C5B C6 Sc1 -50.6(5) . . . . ? C4 C5A C6 C5B -27.4(4) . . . . ? Sc1 C5A C6 C5B -82.2(4) . . . . ? C4 C5A C6 Sc1 54.84(18) . . . . ? O1 Sc1 C6 C5B 113.5(4) . . . . ? O3 Sc1 C6 C5B -71.0(4) . . . . ? O2 Sc1 C6 C5B -161.5(4) . . . . ? C4 Sc1 C6 C5B 24.0(4) . . . . ? C3 Sc1 C6 C5B 15.3(4) . . . . ? C2 Sc1 C6 C5B 45.4(5) . . . . ? C5A Sc1 C6 C5B 51.2(4) . . . . ? C1 Sc1 C6 C5B -127.2(4) . . . . ? O1 Sc1 C6 C5A 62.33(14) . . . . ? O3 Sc1 C6 C5A -122.15(14) . . . . ? O2 Sc1 C6 C5A 147.34(14) . . . . ? C4 Sc1 C6 C5A -27.18(13) . . . . ? C3 Sc1 C6 C5A -35.87(17) . . . . ? C2 Sc1 C6 C5A -5.8(3) . . . . ? C5B Sc1 C6 C5A -51.2(4) . . . . ? C1 Sc1 C6 C5A -178.38(17) . . . . ? C10 O1 C7 C8 -8.38(17) . . . . ? Sc1 O1 C7 C8 -167.16(10) . . . . ? O1 C7 C8 C9 28.93(17) . . . . ? C7 C8 C9 C10 -38.35(17) . . . . ? C7 O1 C10 C9 -15.94(16) . . . . ? Sc1 O1 C10 C9 143.25(10) . . . . ? C8 C9 C10 O1 33.68(16) . . . . ? C14 O2 C11 C12 24.33(16) . . . . ? Sc1 O2 C11 C12 -147.59(10) . . . . ? O2 C11 C12 C13 -38.46(15) . . . . ? C11 C12 C13 C14 38.12(17) . . . . ? C11 O2 C14 C13 0.03(17) . . . . ? Sc1 O2 C14 C13 171.58(10) . . . . ? C12 C13 C14 O2 -23.95(18) . . . . ? C18 O3 C15 C16 3.43(16) . . . . ? Sc1 O3 C15 C16 -171.69(9) . . . . ? O3 C15 C16 C17 21.49(16) . . . . ? C15 C16 C17 C18 -37.37(16) . . . . ? C15 O3 C18 C17 -27.18(16) . . . . ? Sc1 O3 C18 C17 148.20(10) . . . . ? C16 C17 C18 O3 39.83(15) . . . . ? C25 B1 C19 C20 87.34(16) . . . . ? C37 B1 C19 C20 -151.04(13) . . . . ? C31 B1 C19 C20 -33.57(19) . . . . ? C25 B1 C19 C24 -85.01(16) . . . . ? C37 B1 C19 C24 36.62(19) . . . . ? C31 B1 C19 C24 154.09(13) . . . . ? C24 C19 C20 C21 -1.6(2) . . . . ? B1 C19 C20 C21 -174.51(14) . . . . ? C19 C20 C21 C22 0.5(2) . . . . ? C20 C21 C22 C23 0.7(2) . . . . ? C21 C22 C23 C24 -0.8(2) . . . . ? C22 C23 C24 C19 -0.4(2) . . . . ? C20 C19 C24 C23 1.5(2) . . . . ? B1 C19 C24 C23 174.32(14) . . . . ? C19 B1 C25 C26 89.58(16) . . . . ? C37 B1 C25 C26 -32.73(19) . . . . ? C31 B1 C25 C26 -150.66(13) . . . . ? C19 B1 C25 C30 -82.95(16) . . . . ? C37 B1 C25 C30 154.74(13) . . . . ? C31 B1 C25 C30 36.81(19) . . . . ? C30 C25 C26 C27 -2.2(2) . . . . ? B1 C25 C26 C27 -175.14(14) . . . . ? C25 C26 C27 C28 0.2(2) . . . . ? C26 C27 C28 C29 1.7(2) . . . . ? C27 C28 C29 C30 -1.6(2) . . . . ? C28 C29 C30 C25 -0.4(2) . . . . ? C26 C25 C30 C29 2.3(2) . . . . ? B1 C25 C30 C29 175.38(14) . . . . ? C19 B1 C31 C32 145.97(14) . . . . ? C25 B1 C31 C32 30.88(19) . . . . ? C37 B1 C31 C32 -91.42(16) . . . . ? C19 B1 C31 C36 -38.31(19) . . . . ? C25 B1 C31 C36 -153.41(13) . . . . ? C37 B1 C31 C36 84.30(16) . . . . ? C36 C31 C32 C33 0.9(2) . . . . ? B1 C31 C32 C33 176.88(14) . . . . ? C31 C32 C33 C34 -0.1(2) . . . . ? C32 C33 C34 C35 -0.7(2) . . . . ? C33 C34 C35 C36 0.6(2) . . . . ? C34 C35 C36 C31 0.3(2) . . . . ? C32 C31 C36 C35 -1.0(2) . . . . ? B1 C31 C36 C35 -177.05(14) . . . . ? C19 B1 C37 C38 34.00(19) . . . . ? C25 B1 C37 C38 150.34(13) . . . . ? C31 B1 C37 C38 -87.11(16) . . . . ? C19 B1 C37 C42 -151.32(13) . . . . ? C25 B1 C37 C42 -34.98(19) . . . . ? C31 B1 C37 C42 87.57(16) . . . . ? C42 C37 C38 C39 2.4(2) . . . . ? B1 C37 C38 C39 177.38(14) . . . . ? C37 C38 C39 C40 0.1(2) . . . . ? C38 C39 C40 C41 -2.1(2) . . . . ? C39 C40 C41 C42 1.4(2) . . . . ? C40 C41 C42 C37 1.3(3) . . . . ? C38 C37 C42 C41 -3.1(2) . . . . ? B1 C37 C42 C41 -178.21(14) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.509 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.059 #==END data_3c _database_code_depnum_ccdc_archive 'CCDC 832190' #TrackingRef '- CC-Scallyl_revised_08-09-2011.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H48 Mg O6, 2(C12 H20 Sc), 2(C4 H8 O)' _chemical_formula_sum 'C56 H104 Mg O8 Sc2' _chemical_formula_weight 1019.62 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 '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/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0491(12) _cell_length_b 11.3146(10) _cell_length_c 20.4870(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.444(4) _cell_angle_gamma 90.00 _cell_volume 2999.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2209 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 19.56 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 0.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9428 _exptl_absorpt_correction_T_max 0.9695 _exptl_absorpt_process_details 'Platon Mulabs' _exptl_special_details ; The space group P21/n was determined based on systematic absences in the data set. The value for Rint of 0.222 does not improve significantly by lowering the lattice symmetry (with a value of 0.211 for Laue symmetry -1). ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'APEX Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43819 _diffrn_reflns_av_R_equivalents 0.2219 _diffrn_reflns_av_sigmaI/netI 0.3394 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.49 _reflns_number_total 6000 _reflns_number_gt 1929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal structure contains the solvent molecule THF. Due to strong disorder within this molecule, all carbon atom as well as the position for the oxygen atom were included with isotropic displacement parameters in the refinement. Refinement without restraints did not lead to a sufficiently reasonable geometry for this solvent molecule. To deal with this problem, the C-C distances (between neighboring carbon atoms) and the C-O distances are restrained to be equal. In addition, a common isotropic displacement parameter was used for all carbon atoms of this THF molecule. ; _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^)+(0.0638P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6000 _refine_ls_number_parameters 294 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.2375 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.854 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.53537(8) 0.49308(9) 0.73557(5) 0.0229(3) Uani 1 1 d . . . Mg1 Mg 0.5000 0.0000 0.0000 0.0187(6) Uani 1 2 d S . . O1 O 0.6311(3) 0.1005(3) -0.00512(15) 0.0183(9) Uani 1 1 d . . . O2 O 0.4820(3) -0.0233(3) -0.10157(14) 0.0201(9) Uani 1 1 d . . . O3 O 0.4085(3) 0.1550(3) -0.01319(15) 0.0191(9) Uani 1 1 d . . . C1 C 0.6751(5) 0.6258(5) 0.7134(3) 0.0365(16) Uani 1 1 d . . . H1A H 0.6120 0.6550 0.6908 0.044 Uiso 1 1 calc R . . H1B H 0.7161 0.6747 0.7442 0.044 Uiso 1 1 calc R . . C2 C 0.7066(5) 0.5145(6) 0.7016(3) 0.0392(16) Uani 1 1 d . . . H2 H 0.7702 0.4893 0.7254 0.047 Uiso 1 1 calc R . . C3 C 0.6553(5) 0.4347(5) 0.6587(3) 0.0378(16) Uani 1 1 d . . . H3A H 0.5913 0.4558 0.6338 0.045 Uiso 1 1 calc R . . H3B H 0.6837 0.3584 0.6539 0.045 Uiso 1 1 calc R . . C4 C 0.6148(5) 0.3758(5) 0.8318(3) 0.0403(17) Uani 1 1 d . . . H4A H 0.5815 0.4431 0.8471 0.048 Uiso 1 1 calc R . . H4B H 0.6859 0.3617 0.8465 0.048 Uiso 1 1 calc R . . C5 C 0.5603(5) 0.2988(5) 0.7883(3) 0.0372(17) Uani 1 1 d . . . H5 H 0.5971 0.2329 0.7745 0.045 Uiso 1 1 calc R . . C6 C 0.4582(5) 0.3078(4) 0.7631(3) 0.0336(16) Uani 1 1 d . . . H6A H 0.4181 0.3721 0.7755 0.040 Uiso 1 1 calc R . . H6B H 0.4275 0.2497 0.7333 0.040 Uiso 1 1 calc R . . C7 C 0.3972(4) 0.5138(5) 0.6568(2) 0.0323(15) Uani 1 1 d . . . H7A H 0.3940 0.4456 0.6263 0.039 Uiso 1 1 calc R . . H7B H 0.3329 0.5146 0.6777 0.039 Uiso 1 1 calc R . . C8 C 0.4046(4) 0.6240(5) 0.6194(3) 0.0319(15) Uani 1 1 d . . . H8 H 0.3880 0.6945 0.6410 0.038 Uiso 1 1 calc R . . C9 C 0.4315(4) 0.6379(5) 0.5592(3) 0.0350(16) Uani 1 1 d . . . H9A H 0.4491 0.5710 0.5350 0.042 Uiso 1 1 calc R . . H9B H 0.4331 0.7147 0.5407 0.042 Uiso 1 1 calc R . . C10 C 0.4891(4) 0.6388(4) 0.8026(3) 0.0309(15) Uani 1 1 d . . . H10A H 0.5505 0.6640 0.8329 0.037 Uiso 1 1 calc R . . H10B H 0.4637 0.7079 0.7756 0.037 Uiso 1 1 calc R . . C11 C 0.4092(5) 0.5994(5) 0.8406(3) 0.0365(17) Uani 1 1 d . . . H11 H 0.4331 0.5579 0.8799 0.044 Uiso 1 1 calc R . . C12 C 0.3083(5) 0.6129(5) 0.8283(3) 0.0402(17) Uani 1 1 d . . . H12A H 0.2789 0.6536 0.7898 0.048 Uiso 1 1 calc R . . H12B H 0.2648 0.5820 0.8580 0.048 Uiso 1 1 calc R . . C13 C 0.7356(4) 0.0550(4) -0.0080(3) 0.0274(15) Uani 1 1 d . . . H13A H 0.7348 -0.0062 -0.0426 0.033 Uiso 1 1 calc R . . H13B H 0.7643 0.0200 0.0347 0.033 Uiso 1 1 calc R . . C14 C 0.7988(5) 0.1594(5) -0.0239(3) 0.0389(16) Uani 1 1 d . . . H14A H 0.7946 0.1713 -0.0720 0.047 Uiso 1 1 calc R . . H14B H 0.8721 0.1499 -0.0051 0.047 Uiso 1 1 calc R . . C15 C 0.7495(4) 0.2602(5) 0.0081(3) 0.0347(16) Uani 1 1 d . . . H15A H 0.7629 0.3363 -0.0130 0.042 Uiso 1 1 calc R . . H15B H 0.7753 0.2648 0.0557 0.042 Uiso 1 1 calc R . . C16 C 0.6365(4) 0.2297(4) -0.0027(3) 0.0267(15) Uani 1 1 d . . . H16A H 0.6013 0.2605 0.0338 0.032 Uiso 1 1 calc R . . H16B H 0.6032 0.2642 -0.0446 0.032 Uiso 1 1 calc R . . C17 C 0.5561(4) 0.0127(4) -0.1446(2) 0.0236(13) Uani 1 1 d . . . H17A H 0.6233 -0.0271 -0.1318 0.028 Uiso 1 1 calc R . . H17B H 0.5671 0.0993 -0.1419 0.028 Uiso 1 1 calc R . . C18 C 0.5116(4) -0.0226(4) -0.2137(2) 0.0221(14) Uani 1 1 d . . . H18A H 0.5276 0.0372 -0.2462 0.027 Uiso 1 1 calc R . . H18B H 0.5385 -0.1003 -0.2257 0.027 Uiso 1 1 calc R . . C19 C 0.3966(4) -0.0284(4) -0.2101(2) 0.0262(15) Uani 1 1 d . . . H19A H 0.3647 0.0510 -0.2154 0.031 Uiso 1 1 calc R . . H19B H 0.3616 -0.0819 -0.2441 0.031 Uiso 1 1 calc R . . C20 C 0.3917(4) -0.0763(4) -0.1419(2) 0.0218(13) Uani 1 1 d . . . H20A H 0.3267 -0.0524 -0.1255 0.026 Uiso 1 1 calc R . . H20B H 0.3964 -0.1636 -0.1415 0.026 Uiso 1 1 calc R . . C21 C 0.3656(4) 0.2051(4) -0.0770(2) 0.0232(14) Uani 1 1 d . . . H21A H 0.3135 0.1511 -0.1004 0.028 Uiso 1 1 calc R . . H21B H 0.4209 0.2185 -0.1049 0.028 Uiso 1 1 calc R . . C22 C 0.3160(4) 0.3213(4) -0.0613(2) 0.0303(15) Uani 1 1 d . . . H22A H 0.3267 0.3823 -0.0943 0.036 Uiso 1 1 calc R . . H22B H 0.2410 0.3113 -0.0599 0.036 Uiso 1 1 calc R . . C23 C 0.3711(4) 0.3544(4) 0.0060(2) 0.0277(15) Uani 1 1 d . . . H23A H 0.4385 0.3926 0.0027 0.033 Uiso 1 1 calc R . . H23B H 0.3283 0.4074 0.0298 0.033 Uiso 1 1 calc R . . C24 C 0.3846(5) 0.2354(4) 0.0383(2) 0.0290(15) Uani 1 1 d . . . H24A H 0.4418 0.2371 0.0752 0.035 Uiso 1 1 calc R . . H24B H 0.3204 0.2108 0.0556 0.035 Uiso 1 1 calc R . . O4 O 0.1426(3) 0.4922(3) 0.07118(17) 0.0449(11) Uani 1 1 d D . . C25A C 0.0732(6) 0.5653(9) 0.1027(6) 0.0269(10) Uiso 0.708(8) 1 d PD A 1 H25A H 0.0612 0.6417 0.0793 0.032 Uiso 0.708(8) 1 calc PR A 1 H25B H 0.1018 0.5812 0.1490 0.032 Uiso 0.708(8) 1 calc PR A 1 C26A C -0.0250(6) 0.4959(6) 0.0992(4) 0.0269(10) Uiso 0.708(8) 1 d PD A 1 H26A H -0.0731 0.5175 0.0597 0.032 Uiso 0.708(8) 1 calc PR A 1 H26B H -0.0595 0.5094 0.1389 0.032 Uiso 0.708(8) 1 calc PR A 1 C27A C 0.0114(6) 0.3627(6) 0.0955(4) 0.0269(10) Uiso 0.708(8) 1 d PD A 1 H27A H -0.0234 0.3234 0.0555 0.032 Uiso 0.708(8) 1 calc PR A 1 H27B H -0.0032 0.3178 0.1347 0.032 Uiso 0.708(8) 1 calc PR A 1 C28A C 0.1328(6) 0.3734(6) 0.0931(4) 0.0269(10) Uiso 0.708(8) 1 d PD A 1 H28A H 0.1723 0.3609 0.1372 0.032 Uiso 0.708(8) 1 calc PR A 1 H28B H 0.1564 0.3161 0.0617 0.032 Uiso 0.708(8) 1 calc PR A 1 C25B C 0.0924(14) 0.578(2) 0.1074(15) 0.0269(10) Uiso 0.292(8) 1 d PD A 2 H25C H 0.0983 0.6577 0.0883 0.032 Uiso 0.292(8) 1 calc PR A 2 H25D H 0.1245 0.5798 0.1539 0.032 Uiso 0.292(8) 1 calc PR A 2 C26B C -0.0241(14) 0.5405(14) 0.1029(11) 0.0269(10) Uiso 0.292(8) 1 d PD A 2 H26C H -0.0604 0.5894 0.1328 0.032 Uiso 0.292(8) 1 calc PR A 2 H26D H -0.0591 0.5506 0.0574 0.032 Uiso 0.292(8) 1 calc PR A 2 C27B C -0.0250(13) 0.4074(15) 0.1237(9) 0.0269(10) Uiso 0.292(8) 1 d PD A 2 H27C H -0.0809 0.3607 0.0985 0.032 Uiso 0.292(8) 1 calc PR A 2 H27D H -0.0242 0.3955 0.1717 0.032 Uiso 0.292(8) 1 calc PR A 2 C28B C 0.0880(14) 0.3889(14) 0.0986(10) 0.0269(10) Uiso 0.292(8) 1 d PD A 2 H28C H 0.1351 0.3569 0.1362 0.032 Uiso 0.292(8) 1 calc PR A 2 H28D H 0.0799 0.3268 0.0643 0.032 Uiso 0.292(8) 1 calc PR A 2 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 0.0292(7) 0.0205(6) 0.0184(5) 0.0011(5) 0.0002(5) -0.0038(6) Mg1 0.0244(15) 0.0180(13) 0.0129(12) 0.0010(12) -0.0004(11) 0.0001(13) O1 0.019(2) 0.017(2) 0.019(2) 0.0023(16) 0.0033(17) 0.0030(17) O2 0.020(2) 0.025(2) 0.0144(19) 0.0004(16) -0.0008(17) -0.0079(17) O3 0.029(2) 0.0151(19) 0.0123(19) -0.0032(16) -0.0016(17) 0.0002(17) C1 0.028(4) 0.041(4) 0.040(4) -0.008(3) 0.002(3) -0.017(3) C2 0.032(4) 0.047(4) 0.040(4) 0.004(4) 0.010(3) 0.004(4) C3 0.040(4) 0.034(4) 0.042(4) -0.002(3) 0.018(3) 0.001(3) C4 0.042(4) 0.037(4) 0.040(4) 0.026(3) -0.004(3) 0.007(3) C5 0.055(5) 0.019(3) 0.037(4) 0.015(3) 0.006(4) 0.002(3) C6 0.048(5) 0.015(3) 0.038(4) 0.004(3) 0.008(3) -0.007(3) C7 0.026(4) 0.036(4) 0.034(3) 0.005(3) 0.002(3) -0.001(3) C8 0.028(4) 0.036(4) 0.029(4) -0.006(3) -0.008(3) 0.003(3) C9 0.034(4) 0.030(4) 0.039(4) 0.007(3) -0.001(3) 0.001(3) C10 0.042(4) 0.020(3) 0.030(3) -0.004(3) 0.001(3) -0.005(3) C11 0.053(5) 0.026(4) 0.029(4) -0.007(3) -0.004(4) 0.009(3) C12 0.055(5) 0.032(4) 0.033(4) -0.008(3) 0.004(4) -0.004(4) C13 0.031(4) 0.027(3) 0.023(3) 0.002(3) -0.001(3) -0.002(3) C14 0.041(4) 0.037(4) 0.041(4) -0.001(3) 0.013(3) -0.012(3) C15 0.030(4) 0.023(3) 0.051(4) -0.008(3) 0.003(3) -0.010(3) C16 0.036(4) 0.010(3) 0.031(4) 0.000(3) -0.008(3) 0.000(3) C17 0.030(4) 0.021(3) 0.020(3) 0.005(3) 0.005(3) -0.003(3) C18 0.037(4) 0.019(3) 0.010(3) 0.003(2) 0.004(2) -0.003(3) C19 0.036(4) 0.029(3) 0.012(3) -0.002(3) -0.004(3) -0.007(3) C20 0.019(3) 0.025(3) 0.020(3) -0.001(3) -0.003(3) 0.001(3) C21 0.032(4) 0.017(3) 0.018(3) 0.006(2) -0.006(3) 0.004(3) C22 0.035(4) 0.020(3) 0.034(4) 0.003(3) -0.003(3) 0.004(3) C23 0.035(4) 0.015(3) 0.031(3) -0.007(3) -0.003(3) 0.008(3) C24 0.041(4) 0.019(3) 0.027(3) -0.007(3) 0.005(3) 0.011(3) O4 0.048(3) 0.050(3) 0.037(2) 0.005(2) 0.010(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 C7 2.271(5) . ? Sc1 C10 2.277(5) . ? Sc1 C6 2.424(5) . ? Sc1 C2 2.436(6) . ? Sc1 C1 2.450(5) . ? Sc1 C3 2.450(6) . ? Sc1 C5 2.453(5) . ? Sc1 C4 2.488(5) . ? Mg1 O1 2.067(3) . ? Mg1 O1 2.067(3) 3_655 ? Mg1 O2 2.080(3) . ? Mg1 O2 2.080(3) 3_655 ? Mg1 O3 2.120(3) 3_655 ? Mg1 O3 2.120(3) . ? O1 C16 1.465(5) . ? O1 C13 1.466(6) . ? O2 C17 1.449(6) . ? O2 C20 1.476(5) . ? O3 C24 1.457(5) . ? O3 C21 1.467(5) . ? C1 C2 1.356(7) . ? C1 H1A 0.9500 . ? C1 H1B 0.9500 . ? C2 C3 1.373(7) . ? C2 H2 0.9500 . ? C3 H3A 0.9500 . ? C3 H3B 0.9500 . ? C4 C5 1.376(7) . ? C4 H4A 0.9500 . ? C4 H4B 0.9500 . ? C5 C6 1.368(8) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C7 C8 1.472(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.335(7) . ? C8 H8 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C10 C11 1.450(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.318(8) . ? C11 H11 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.500(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.501(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.502(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.514(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.513(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.507(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.518(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.516(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.501(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O4 C28A 1.428(7) . ? O4 C25B 1.432(14) . ? O4 C25A 1.439(8) . ? O4 C28B 1.514(13) . ? C25A C26A 1.497(9) . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? C26A C27A 1.584(8) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C27A C28A 1.595(9) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C25B C26B 1.571(14) . ? C25B H25C 0.9900 . ? C25B H25D 0.9900 . ? C26B C27B 1.566(14) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? C27B C28B 1.636(14) . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C28B H28C 0.9900 . ? C28B H28D 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 C7 Sc1 C10 96.1(2) . . ? C7 Sc1 C6 86.5(2) . . ? C10 Sc1 C6 109.6(2) . . ? C7 Sc1 C2 117.4(2) . . ? C10 Sc1 C2 115.1(2) . . ? C6 Sc1 C2 125.2(2) . . ? C7 Sc1 C1 110.2(2) . . ? C10 Sc1 C1 86.0(2) . . ? C6 Sc1 C1 156.2(2) . . ? C2 Sc1 C1 32.24(17) . . ? C7 Sc1 C3 94.9(2) . . ? C10 Sc1 C3 145.5(2) . . ? C6 Sc1 C3 103.63(19) . . ? C2 Sc1 C3 32.63(18) . . ? C1 Sc1 C3 59.56(19) . . ? C7 Sc1 C5 117.0(2) . . ? C10 Sc1 C5 114.4(2) . . ? C6 Sc1 C5 32.59(18) . . ? C2 Sc1 C5 98.1(2) . . ? C1 Sc1 C5 124.9(2) . . ? C3 Sc1 C5 89.0(2) . . ? C7 Sc1 C4 146.0(2) . . ? C10 Sc1 C4 91.4(2) . . ? C6 Sc1 C4 59.82(19) . . ? C2 Sc1 C4 88.6(2) . . ? C1 Sc1 C4 103.3(2) . . ? C3 Sc1 C4 97.5(2) . . ? C5 Sc1 C4 32.34(17) . . ? O1 Mg1 O1 180.0(2) . 3_655 ? O1 Mg1 O2 90.32(12) . . ? O1 Mg1 O2 89.68(12) 3_655 . ? O1 Mg1 O2 89.68(12) . 3_655 ? O1 Mg1 O2 90.32(12) 3_655 3_655 ? O2 Mg1 O2 180.00(18) . 3_655 ? O1 Mg1 O3 90.30(13) . 3_655 ? O1 Mg1 O3 89.70(13) 3_655 3_655 ? O2 Mg1 O3 90.65(12) . 3_655 ? O2 Mg1 O3 89.35(12) 3_655 3_655 ? O1 Mg1 O3 89.70(13) . . ? O1 Mg1 O3 90.30(13) 3_655 . ? O2 Mg1 O3 89.35(12) . . ? O2 Mg1 O3 90.65(12) 3_655 . ? O3 Mg1 O3 180.00(15) 3_655 . ? C16 O1 C13 108.1(4) . . ? C16 O1 Mg1 125.7(3) . . ? C13 O1 Mg1 126.1(3) . . ? C17 O2 C20 108.7(3) . . ? C17 O2 Mg1 125.1(3) . . ? C20 O2 Mg1 126.1(3) . . ? C24 O3 C21 108.2(3) . . ? C24 O3 Mg1 126.4(3) . . ? C21 O3 Mg1 125.2(3) . . ? C2 C1 Sc1 73.3(3) . . ? C2 C1 H1A 120.0 . . ? Sc1 C1 H1A 71.6 . . ? C2 C1 H1B 120.0 . . ? Sc1 C1 H1B 127.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 C3 126.2(6) . . ? C1 C2 Sc1 74.4(3) . . ? C3 C2 Sc1 74.2(3) . . ? C1 C2 H2 116.9 . . ? C3 C2 H2 116.9 . . ? Sc1 C2 H2 126.6 . . ? C2 C3 Sc1 73.1(3) . . ? C2 C3 H3A 120.0 . . ? Sc1 C3 H3A 71.8 . . ? C2 C3 H3B 120.0 . . ? Sc1 C3 H3B 127.0 . . ? H3A C3 H3B 120.0 . . ? C5 C4 Sc1 72.4(3) . . ? C5 C4 H4A 120.0 . . ? Sc1 C4 H4A 70.9 . . ? C5 C4 H4B 120.0 . . ? Sc1 C4 H4B 129.0 . . ? H4A C4 H4B 120.0 . . ? C6 C5 C4 126.4(6) . . ? C6 C5 Sc1 72.5(3) . . ? C4 C5 Sc1 75.3(3) . . ? C6 C5 H5 116.8 . . ? C4 C5 H5 116.8 . . ? Sc1 C5 H5 127.9 . . ? C5 C6 Sc1 74.9(3) . . ? C5 C6 H6A 120.0 . . ? Sc1 C6 H6A 70.1 . . ? C5 C6 H6B 120.0 . . ? Sc1 C6 H6B 127.0 . . ? H6A C6 H6B 120.0 . . ? C8 C7 Sc1 111.0(4) . . ? C8 C7 H7A 109.4 . . ? Sc1 C7 H7A 109.4 . . ? C8 C7 H7B 109.4 . . ? Sc1 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C7 128.5(5) . . ? C9 C8 H8 115.7 . . ? C7 C8 H8 115.7 . . ? C8 C9 H9A 120.0 . . ? C8 C9 H9B 120.0 . . ? H9A C9 H9B 120.0 . . ? C11 C10 Sc1 111.5(3) . . ? C11 C10 H10A 109.3 . . ? Sc1 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? Sc1 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 129.3(6) . . ? C12 C11 H11 115.4 . . ? C10 C11 H11 115.4 . . ? C11 C12 H12A 120.0 . . ? C11 C12 H12B 120.0 . . ? H12A C12 H12B 120.0 . . ? O1 C13 C14 105.8(4) . . ? O1 C13 H13A 110.6 . . ? C14 C13 H13A 110.6 . . ? O1 C13 H13B 110.6 . . ? C14 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? C13 C14 C15 103.0(5) . . ? C13 C14 H14A 111.2 . . ? C15 C14 H14A 111.2 . . ? C13 C14 H14B 111.2 . . ? C15 C14 H14B 111.2 . . ? H14A C14 H14B 109.1 . . ? C14 C15 C16 103.3(4) . . ? C14 C15 H15A 111.1 . . ? C16 C15 H15A 111.1 . . ? C14 C15 H15B 111.1 . . ? C16 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? O1 C16 C15 106.0(4) . . ? O1 C16 H16A 110.5 . . ? C15 C16 H16A 110.5 . . ? O1 C16 H16B 110.5 . . ? C15 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? O2 C17 C18 106.8(4) . . ? O2 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? O2 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C19 C18 C17 103.2(4) . . ? C19 C18 H18A 111.1 . . ? C17 C18 H18A 111.1 . . ? C19 C18 H18B 111.1 . . ? C17 C18 H18B 111.1 . . ? H18A C18 H18B 109.1 . . ? C20 C19 C18 102.9(4) . . ? C20 C19 H19A 111.2 . . ? C18 C19 H19A 111.2 . . ? C20 C19 H19B 111.2 . . ? C18 C19 H19B 111.2 . . ? H19A C19 H19B 109.1 . . ? O2 C20 C19 104.2(4) . . ? O2 C20 H20A 110.9 . . ? C19 C20 H20A 110.9 . . ? O2 C20 H20B 110.9 . . ? C19 C20 H20B 110.9 . . ? H20A C20 H20B 108.9 . . ? O3 C21 C22 105.6(4) . . ? O3 C21 H21A 110.6 . . ? C22 C21 H21A 110.6 . . ? O3 C21 H21B 110.6 . . ? C22 C21 H21B 110.6 . . ? H21A C21 H21B 108.8 . . ? C23 C22 C21 104.0(4) . . ? C23 C22 H22A 111.0 . . ? C21 C22 H22A 111.0 . . ? C23 C22 H22B 111.0 . . ? C21 C22 H22B 111.0 . . ? H22A C22 H22B 109.0 . . ? C24 C23 C22 101.2(4) . . ? C24 C23 H23A 111.5 . . ? C22 C23 H23A 111.5 . . ? C24 C23 H23B 111.5 . . ? C22 C23 H23B 111.5 . . ? H23A C23 H23B 109.3 . . ? O3 C24 C23 105.3(4) . . ? O3 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? O3 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? C28A O4 C25B 114.2(13) . . ? C28A O4 C25A 108.2(7) . . ? C25B O4 C28B 93.6(13) . . ? C25A O4 C28B 85.6(9) . . ? O4 C25A C26A 105.1(6) . . ? O4 C25A H25A 110.7 . . ? C26A C25A H25A 110.7 . . ? O4 C25A H25B 110.7 . . ? C26A C25A H25B 110.7 . . ? H25A C25A H25B 108.8 . . ? C25A C26A C27A 104.0(7) . . ? C25A C26A H26A 111.0 . . ? C27A C26A H26A 111.0 . . ? C25A C26A H26B 111.0 . . ? C27A C26A H26B 111.0 . . ? H26A C26A H26B 109.0 . . ? C26A C27A C28A 103.5(6) . . ? C26A C27A H27A 111.1 . . ? C28A C27A H27A 111.1 . . ? C26A C27A H27B 111.1 . . ? C28A C27A H27B 111.1 . . ? H27A C27A H27B 109.0 . . ? O4 C28A C27A 102.2(5) . . ? O4 C28A H28A 111.3 . . ? C27A C28A H28A 111.3 . . ? O4 C28A H28B 111.3 . . ? C27A C28A H28B 111.3 . . ? H28A C28A H28B 109.2 . . ? O4 C25B C26B 106.8(13) . . ? O4 C25B H25C 110.4 . . ? C26B C25B H25C 110.4 . . ? O4 C25B H25D 110.4 . . ? C26B C25B H25D 110.4 . . ? H25C C25B H25D 108.6 . . ? C27B C26B C25B 106.6(17) . . ? C27B C26B H26C 110.4 . . ? C25B C26B H26C 110.4 . . ? C27B C26B H26D 110.4 . . ? C25B C26B H26D 110.4 . . ? H26C C26B H26D 108.6 . . ? C26B C27B C28B 89.9(12) . . ? C26B C27B H27C 113.7 . . ? C28B C27B H27C 113.7 . . ? C26B C27B H27D 113.7 . . ? C28B C27B H27D 113.7 . . ? H27C C27B H27D 110.9 . . ? O4 C28B C27B 120.3(11) . . ? O4 C28B H28C 107.2 . . ? C27B C28B H28C 107.2 . . ? O4 C28B H28D 107.2 . . ? C27B C28B H28D 107.2 . . ? H28C C28B H28D 106.9 . . ? 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 Mg1 O1 C16 101.0(3) . . . . ? O2 Mg1 O1 C16 -79.0(3) 3_655 . . . ? O3 Mg1 O1 C16 -168.3(3) 3_655 . . . ? O3 Mg1 O1 C16 11.7(3) . . . . ? O2 Mg1 O1 C13 -82.6(3) . . . . ? O2 Mg1 O1 C13 97.4(3) 3_655 . . . ? O3 Mg1 O1 C13 8.0(3) 3_655 . . . ? O3 Mg1 O1 C13 -172.0(3) . . . . ? O1 Mg1 O2 C17 7.7(4) . . . . ? O1 Mg1 O2 C17 -172.3(4) 3_655 . . . ? O3 Mg1 O2 C17 -82.6(4) 3_655 . . . ? O3 Mg1 O2 C17 97.4(4) . . . . ? O1 Mg1 O2 C20 -170.9(3) . . . . ? O1 Mg1 O2 C20 9.1(3) 3_655 . . . ? O3 Mg1 O2 C20 98.8(3) 3_655 . . . ? O3 Mg1 O2 C20 -81.2(3) . . . . ? O1 Mg1 O3 C24 -86.6(4) . . . . ? O1 Mg1 O3 C24 93.4(4) 3_655 . . . ? O2 Mg1 O3 C24 -176.9(4) . . . . ? O2 Mg1 O3 C24 3.1(4) 3_655 . . . ? O1 Mg1 O3 C21 87.8(4) . . . . ? O1 Mg1 O3 C21 -92.2(4) 3_655 . . . ? O2 Mg1 O3 C21 -2.6(4) . . . . ? O2 Mg1 O3 C21 177.4(4) 3_655 . . . ? C7 Sc1 C1 C2 -109.5(4) . . . . ? C10 Sc1 C1 C2 155.5(4) . . . . ? C6 Sc1 C1 C2 23.1(7) . . . . ? C3 Sc1 C1 C2 -25.9(3) . . . . ? C5 Sc1 C1 C2 38.3(4) . . . . ? C4 Sc1 C1 C2 65.0(4) . . . . ? Sc1 C1 C2 C3 56.4(6) . . . . ? C7 Sc1 C2 C1 84.8(4) . . . . ? C10 Sc1 C2 C1 -27.2(4) . . . . ? C6 Sc1 C2 C1 -168.8(3) . . . . ? C3 Sc1 C2 C1 135.7(5) . . . . ? C5 Sc1 C2 C1 -149.1(4) . . . . ? C4 Sc1 C2 C1 -118.1(4) . . . . ? C7 Sc1 C2 C3 -50.9(4) . . . . ? C10 Sc1 C2 C3 -162.9(3) . . . . ? C6 Sc1 C2 C3 55.5(4) . . . . ? C1 Sc1 C2 C3 -135.7(5) . . . . ? C5 Sc1 C2 C3 75.2(4) . . . . ? C4 Sc1 C2 C3 106.2(4) . . . . ? C1 C2 C3 Sc1 -56.5(6) . . . . ? C7 Sc1 C3 C2 136.3(4) . . . . ? C10 Sc1 C3 C2 28.1(6) . . . . ? C6 Sc1 C3 C2 -136.1(4) . . . . ? C1 Sc1 C3 C2 25.6(3) . . . . ? C5 Sc1 C3 C2 -106.8(4) . . . . ? C4 Sc1 C3 C2 -75.5(4) . . . . ? C7 Sc1 C4 C5 34.3(6) . . . . ? C10 Sc1 C4 C5 137.3(4) . . . . ? C6 Sc1 C4 C5 25.4(4) . . . . ? C2 Sc1 C4 C5 -107.6(4) . . . . ? C1 Sc1 C4 C5 -136.5(4) . . . . ? C3 Sc1 C4 C5 -76.1(4) . . . . ? Sc1 C4 C5 C6 -54.6(5) . . . . ? C7 Sc1 C5 C6 -22.7(4) . . . . ? C10 Sc1 C5 C6 88.5(4) . . . . ? C2 Sc1 C5 C6 -149.1(4) . . . . ? C1 Sc1 C5 C6 -168.7(3) . . . . ? C3 Sc1 C5 C6 -117.7(4) . . . . ? C4 Sc1 C5 C6 136.6(6) . . . . ? C7 Sc1 C5 C4 -159.3(4) . . . . ? C10 Sc1 C5 C4 -48.1(4) . . . . ? C6 Sc1 C5 C4 -136.6(6) . . . . ? C2 Sc1 C5 C4 74.3(4) . . . . ? C1 Sc1 C5 C4 54.8(4) . . . . ? C3 Sc1 C5 C4 105.7(4) . . . . ? C4 C5 C6 Sc1 55.7(5) . . . . ? C7 Sc1 C6 C5 159.8(4) . . . . ? C10 Sc1 C6 C5 -105.0(4) . . . . ? C2 Sc1 C6 C5 38.4(4) . . . . ? C1 Sc1 C6 C5 23.6(7) . . . . ? C3 Sc1 C6 C5 65.6(4) . . . . ? C4 Sc1 C6 C5 -25.2(3) . . . . ? C10 Sc1 C7 C8 71.3(4) . . . . ? C6 Sc1 C7 C8 -179.3(4) . . . . ? C2 Sc1 C7 C8 -51.1(5) . . . . ? C1 Sc1 C7 C8 -16.6(5) . . . . ? C3 Sc1 C7 C8 -75.9(4) . . . . ? C5 Sc1 C7 C8 -167.3(4) . . . . ? C4 Sc1 C7 C8 172.9(4) . . . . ? Sc1 C7 C8 C9 103.2(6) . . . . ? C7 Sc1 C10 C11 78.5(4) . . . . ? C6 Sc1 C10 C11 -10.0(5) . . . . ? C2 Sc1 C10 C11 -157.4(4) . . . . ? C1 Sc1 C10 C11 -171.6(4) . . . . ? C3 Sc1 C10 C11 -173.7(4) . . . . ? C5 Sc1 C10 C11 -44.9(5) . . . . ? C4 Sc1 C10 C11 -68.3(4) . . . . ? Sc1 C10 C11 C12 -95.9(6) . . . . ? C16 O1 C13 C14 -13.5(5) . . . . ? Mg1 O1 C13 C14 169.7(3) . . . . ? O1 C13 C14 C15 31.5(5) . . . . ? C13 C14 C15 C16 -37.1(6) . . . . ? C13 O1 C16 C15 -10.1(5) . . . . ? Mg1 O1 C16 C15 166.8(3) . . . . ? C14 C15 C16 O1 29.5(6) . . . . ? C20 O2 C17 C18 -1.7(5) . . . . ? Mg1 O2 C17 C18 179.5(3) . . . . ? O2 C17 C18 C19 23.8(5) . . . . ? C17 C18 C19 C20 -36.2(5) . . . . ? C17 O2 C20 C19 -21.2(5) . . . . ? Mg1 O2 C20 C19 157.6(3) . . . . ? C18 C19 C20 O2 35.5(5) . . . . ? C24 O3 C21 C22 1.0(5) . . . . ? Mg1 O3 C21 C22 -174.3(3) . . . . ? O3 C21 C22 C23 22.9(5) . . . . ? C21 C22 C23 C24 -37.1(5) . . . . ? C21 O3 C24 C23 -24.9(5) . . . . ? Mg1 O3 C24 C23 150.3(3) . . . . ? C22 C23 C24 O3 38.2(5) . . . . ? C28A O4 C25A C26A -42.9(10) . . . . ? C25B O4 C25A C26A -165(10) . . . . ? C28B O4 C25A C26A -32.9(11) . . . . ? O4 C25A C26A C27A 26.1(11) . . . . ? C25A C26A C27A C28A -3.2(9) . . . . ? C25B O4 C28A C27A 50.0(12) . . . . ? C25A O4 C28A C27A 39.2(8) . . . . ? C28B O4 C28A C27A 14(2) . . . . ? C26A C27A C28A O4 -20.7(7) . . . . ? C28A O4 C25B C26B -57(2) . . . . ? C25A O4 C25B C26B 5(8) . . . . ? C28B O4 C25B C26B -43(2) . . . . ? O4 C25B C26B C27B 51(3) . . . . ? C25B C26B C27B C28B -27.3(19) . . . . ? C28A O4 C28B C27B 174(4) . . . . ? C25B O4 C28B C27B 26(2) . . . . ? C25A O4 C28B C27B 17.7(16) . . . . ? C26B C27B C28B O4 2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.850 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.078 #==END