data_Global _audit_creation_method SHELXL-97 #------------------------------------------------------------------------------ _publ_contact_author ; Masood Parvez Department of Chemistry University of Calgary 2500 University Drive N.W. Calgary, Alberta, Canada T2N 1N4 ; #----------------------------------------------------------------------------- _publ_requested_journal ' ? ' _publ_requested_coeditor_name ' ? ' _publ_contact_author_phone ' (403)220-5348 ' _publ_contact_author_fax ' (403)289-9488 ' _publ_contact_author_email ' parvez@ucalgary.ca ' #------------------------------------------------------------------------------ _publ_section_title ; ? ; loop_ _publ_author_name _publ_author_address 'Parvez, Masood' ; Department of Chemistry The University of Calgary 2500 University Drive NW Calgary Alberta Canada T2N 1N4 ; #------------------------------------------------------------------------------ data_Compound_I #----------------------------------------------------------------------------- _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SAPI91 (Fan, 1991)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' #----------------------------------------------------------------------------- _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: Will appear in the paper ; # end Validation Reply Form _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H71 N2 Sc Si2' _chemical_formula_weight 693.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sc' 'Sc' 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.554(2) _cell_length_b 11.027(3) _cell_length_c 20.204(6) _cell_angle_alpha 83.646(13) _cell_angle_beta 88.720(14) _cell_angle_gamma 75.618(15) _cell_volume 2263.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18806 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 27.43 _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9443 _exptl_absorpt_correction_T_max 0.9624 _exptl_absorpt_process_details 'SORTAV: (Blessing, 1997)' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ' \w and \f ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18806 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.43 _reflns_number_total 10256 _reflns_number_gt 7040 _reflns_threshold_expression >2sigma(I) _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^)+(0.0550P)^2^+0.9700P] 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 10256 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.28032(4) 0.34538(4) 0.26138(2) 0.02777(11) Uani 1 1 d . . . Si1 Si 0.46396(6) 0.19086(6) 0.40660(3) 0.03321(15) Uani 1 1 d . . . Si2 Si 0.12680(6) 0.59540(6) 0.14260(3) 0.03803(16) Uani 1 1 d . . . N1 N 0.29199(15) 0.17872(16) 0.21516(8) 0.0295(4) Uani 1 1 d . . . N2 N 0.10734(15) 0.30408(15) 0.30369(8) 0.0271(4) Uani 1 1 d . . . C1 C 0.4371(2) 0.3168(2) 0.33677(11) 0.0325(5) Uani 1 1 d . . . H1A H 0.5205 0.3059 0.3120 0.039 Uiso 1 1 calc R . . H1B H 0.4239 0.3971 0.3567 0.039 Uiso 1 1 calc R . . C2 C 0.2770(2) 0.5117(2) 0.18888(12) 0.0402(5) Uani 1 1 d . . . H2A H 0.3047 0.5742 0.2131 0.048 Uiso 1 1 calc R . . H2B H 0.3454 0.4850 0.1555 0.048 Uiso 1 1 calc R . . C3 C 0.2766(2) -0.0347(2) 0.19846(13) 0.0463(6) Uani 1 1 d . . . H3A H 0.2448 -0.1017 0.2242 0.056 Uiso 1 1 calc R . . H3B H 0.3723 -0.0602 0.1960 0.056 Uiso 1 1 calc R . . H3C H 0.2395 -0.0197 0.1534 0.056 Uiso 1 1 calc R . . C4 C 0.23576(19) 0.08423(19) 0.23198(11) 0.0306(5) Uani 1 1 d . . . C5 C 0.13824(19) 0.09020(19) 0.28060(11) 0.0308(5) Uani 1 1 d . . . H5 H 0.1125 0.0142 0.2931 0.037 Uiso 1 1 calc R . . C6 C 0.07410(19) 0.19377(19) 0.31293(10) 0.0275(4) Uani 1 1 d . . . C7 C -0.0337(2) 0.1764(2) 0.36075(12) 0.0382(5) Uani 1 1 d . . . H7A H -0.0188 0.0872 0.3777 0.046 Uiso 1 1 calc R . . H7B H -0.1182 0.2042 0.3375 0.046 Uiso 1 1 calc R . . H7C H -0.0341 0.2263 0.3980 0.046 Uiso 1 1 calc R . . C8 C 0.38765(19) 0.17305(19) 0.16300(10) 0.0293(4) Uani 1 1 d . . . C9 C 0.3493(2) 0.2030(2) 0.09648(10) 0.0335(5) Uani 1 1 d . . . H9 H 0.2598 0.2162 0.0848 0.040 Uiso 1 1 calc R . . C10 C 0.4405(2) 0.2139(2) 0.04713(10) 0.0325(5) Uani 1 1 d . . . C11 C 0.5709(2) 0.1942(2) 0.06597(10) 0.0314(5) Uani 1 1 d . . . H11 H 0.6337 0.2028 0.0325 0.038 Uiso 1 1 calc R . . C12 C 0.61298(19) 0.16213(19) 0.13214(10) 0.0290(4) Uani 1 1 d . . . C13 C 0.51852(19) 0.15254(19) 0.18036(10) 0.0291(4) Uani 1 1 d . . . H13 H 0.5440 0.1317 0.2258 0.035 Uiso 1 1 calc R . . C14 C 0.4005(2) 0.2517(2) -0.02649(11) 0.0418(6) Uani 1 1 d . . . C15 C 0.2607(3) 0.2469(5) -0.03866(16) 0.1032(15) Uani 1 1 d . . . H15A H 0.2387 0.2718 -0.0859 0.124 Uiso 1 1 calc R . . H15B H 0.2013 0.3047 -0.0116 0.124 Uiso 1 1 calc R . . H15C H 0.2516 0.1609 -0.0263 0.124 Uiso 1 1 calc R . . C16 C 0.4875(3) 0.1634(3) -0.07045(13) 0.0778(11) Uani 1 1 d . . . H16A H 0.4619 0.1901 -0.1172 0.093 Uiso 1 1 calc R . . H16B H 0.4781 0.0775 -0.0583 0.093 Uiso 1 1 calc R . . H16C H 0.5788 0.1653 -0.0644 0.093 Uiso 1 1 calc R . . C17 C 0.4125(5) 0.3843(3) -0.04603(16) 0.1064(16) Uani 1 1 d . . . H17A H 0.3938 0.4072 -0.0937 0.128 Uiso 1 1 calc R . . H17B H 0.5015 0.3896 -0.0366 0.128 Uiso 1 1 calc R . . H17C H 0.3499 0.4424 -0.0205 0.128 Uiso 1 1 calc R . . C18 C 0.7573(2) 0.1436(2) 0.15059(11) 0.0344(5) Uani 1 1 d . . . C19 C 0.8465(2) 0.0642(3) 0.10309(15) 0.0649(8) Uani 1 1 d . . . H19A H 0.9378 0.0519 0.1166 0.078 Uiso 1 1 calc R . . H19B H 0.8336 0.1073 0.0578 0.078 Uiso 1 1 calc R . . H19C H 0.8257 -0.0178 0.1043 0.078 Uiso 1 1 calc R . . C20 C 0.7872(3) 0.2721(3) 0.1463(2) 0.0853(12) Uani 1 1 d . . . H20A H 0.8806 0.2615 0.1550 0.102 Uiso 1 1 calc R . . H20B H 0.7355 0.3214 0.1794 0.102 Uiso 1 1 calc R . . H20C H 0.7650 0.3161 0.1016 0.102 Uiso 1 1 calc R . . C21 C 0.7883(3) 0.0767(4) 0.22032(14) 0.0746(10) Uani 1 1 d . . . H21A H 0.8821 0.0618 0.2292 0.090 Uiso 1 1 calc R . . H21B H 0.7641 -0.0040 0.2239 0.090 Uiso 1 1 calc R . . H21C H 0.7387 0.1292 0.2529 0.090 Uiso 1 1 calc R . . C22 C 0.02831(18) 0.41580(18) 0.32744(10) 0.0257(4) Uani 1 1 d . . . C23 C -0.10322(19) 0.46336(19) 0.30928(10) 0.0279(4) Uani 1 1 d . . . H23 H -0.1443 0.4171 0.2833 0.033 Uiso 1 1 calc R . . C24 C -0.17433(19) 0.57690(19) 0.32865(10) 0.0283(4) Uani 1 1 d . . . C25 C -0.11017(19) 0.64423(19) 0.36579(10) 0.0279(4) Uani 1 1 d . . . H25 H -0.1588 0.7214 0.3801 0.034 Uiso 1 1 calc R . . C26 C 0.02149(19) 0.60254(19) 0.38246(10) 0.0270(4) Uani 1 1 d . . . C27 C 0.08966(19) 0.48560(19) 0.36326(10) 0.0264(4) Uani 1 1 d . . . H27 H 0.1794 0.4536 0.3750 0.032 Uiso 1 1 calc R . . C28 C -0.3191(2) 0.6312(2) 0.31006(12) 0.0353(5) Uani 1 1 d . . . C29 C -0.3681(2) 0.5535(2) 0.26301(14) 0.0504(7) Uani 1 1 d . . . H29A H -0.4608 0.5914 0.2527 0.060 Uiso 1 1 calc R . . H29B H -0.3577 0.4673 0.2844 0.060 Uiso 1 1 calc R . . H29C H -0.3174 0.5518 0.2217 0.060 Uiso 1 1 calc R . . C30 C -0.3370(2) 0.7651(2) 0.27382(15) 0.0542(7) Uani 1 1 d . . . H30A H -0.4295 0.8005 0.2622 0.065 Uiso 1 1 calc R . . H30B H -0.2845 0.7613 0.2331 0.065 Uiso 1 1 calc R . . H30C H -0.3085 0.8185 0.3031 0.065 Uiso 1 1 calc R . . C31 C -0.4008(2) 0.6370(3) 0.37347(15) 0.0630(8) Uani 1 1 d . . . H31A H -0.4930 0.6747 0.3620 0.076 Uiso 1 1 calc R . . H31B H -0.3705 0.6883 0.4033 0.076 Uiso 1 1 calc R . . H31C H -0.3914 0.5516 0.3958 0.076 Uiso 1 1 calc R . . C32 C 0.0945(2) 0.6781(2) 0.42037(11) 0.0326(5) Uani 1 1 d . . . C33 C 0.1460(3) 0.6027(2) 0.48646(13) 0.0539(7) Uani 1 1 d . . . H33A H 0.1924 0.6511 0.5106 0.065 Uiso 1 1 calc R . . H33B H 0.2061 0.5228 0.4779 0.065 Uiso 1 1 calc R . . H33C H 0.0726 0.5858 0.5133 0.065 Uiso 1 1 calc R . . C34 C 0.0072(2) 0.8050(2) 0.43514(14) 0.0503(7) Uani 1 1 d . . . H34A H 0.0590 0.8513 0.4574 0.060 Uiso 1 1 calc R . . H34B H -0.0646 0.7912 0.4642 0.060 Uiso 1 1 calc R . . H34C H -0.0287 0.8540 0.3933 0.060 Uiso 1 1 calc R . . C35 C 0.2085(2) 0.7043(3) 0.37775(14) 0.0507(7) Uani 1 1 d . . . H35A H 0.2541 0.7546 0.4010 0.061 Uiso 1 1 calc R . . H35B H 0.1749 0.7507 0.3350 0.061 Uiso 1 1 calc R . . H35C H 0.2695 0.6244 0.3700 0.061 Uiso 1 1 calc R . . C36 C 0.5035(3) 0.0345(2) 0.37377(13) 0.0585(7) Uani 1 1 d . . . H36A H 0.5169 -0.0323 0.4110 0.070 Uiso 1 1 calc R . . H36B H 0.5834 0.0251 0.3471 0.070 Uiso 1 1 calc R . . H36C H 0.4310 0.0285 0.3459 0.070 Uiso 1 1 calc R . . C37 C 0.3139(2) 0.2016(3) 0.45908(12) 0.0477(6) Uani 1 1 d . . . H37A H 0.3303 0.1324 0.4952 0.057 Uiso 1 1 calc R . . H37B H 0.2409 0.1958 0.4315 0.057 Uiso 1 1 calc R . . H37C H 0.2920 0.2823 0.4780 0.057 Uiso 1 1 calc R . . C38 C 0.6012(3) 0.1955(3) 0.46290(14) 0.0622(8) Uani 1 1 d . . . H38A H 0.6108 0.1274 0.4994 0.075 Uiso 1 1 calc R . . H38B H 0.5818 0.2768 0.4812 0.075 Uiso 1 1 calc R . . H38C H 0.6827 0.1849 0.4375 0.075 Uiso 1 1 calc R . . C39 C 0.0214(2) 0.7119(2) 0.19364(13) 0.0487(6) Uani 1 1 d . . . H39A H -0.0605 0.7525 0.1696 0.058 Uiso 1 1 calc R . . H39B H 0.0674 0.7760 0.2019 0.058 Uiso 1 1 calc R . . H39C H 0.0020 0.6686 0.2362 0.058 Uiso 1 1 calc R . . C40 C 0.1550(3) 0.6861(3) 0.06191(15) 0.0725(9) Uani 1 1 d . . . H40A H 0.0707 0.7266 0.0401 0.087 Uiso 1 1 calc R . . H40B H 0.2089 0.6285 0.0328 0.087 Uiso 1 1 calc R . . H40C H 0.2000 0.7505 0.0706 0.087 Uiso 1 1 calc R . . C41 C 0.0325(3) 0.4797(3) 0.12316(15) 0.0600(8) Uani 1 1 d . . . H41A H -0.0506 0.5253 0.1017 0.072 Uiso 1 1 calc R . . H41B H 0.0153 0.4312 0.1645 0.072 Uiso 1 1 calc R . . H41C H 0.0838 0.4224 0.0931 0.072 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 0.0268(2) 0.0294(2) 0.0284(2) -0.00161(16) -0.00003(16) -0.01011(16) Si1 0.0314(3) 0.0383(4) 0.0293(3) -0.0019(3) -0.0035(2) -0.0081(3) Si2 0.0352(3) 0.0408(4) 0.0345(3) 0.0074(3) 0.0014(3) -0.0077(3) N1 0.0260(8) 0.0346(10) 0.0277(9) -0.0061(7) 0.0022(7) -0.0063(7) N2 0.0273(8) 0.0278(9) 0.0268(9) -0.0068(7) 0.0020(7) -0.0066(7) C1 0.0311(11) 0.0338(12) 0.0343(12) -0.0039(9) -0.0008(9) -0.0107(9) C2 0.0349(12) 0.0414(13) 0.0429(13) 0.0086(11) 0.0002(10) -0.0123(10) C3 0.0480(14) 0.0371(13) 0.0561(16) -0.0191(12) 0.0133(12) -0.0099(11) C4 0.0275(10) 0.0303(11) 0.0340(12) -0.0083(9) -0.0015(9) -0.0047(8) C5 0.0306(10) 0.0259(11) 0.0372(12) -0.0047(9) 0.0025(9) -0.0091(8) C6 0.0273(10) 0.0294(11) 0.0267(10) -0.0037(8) 0.0001(8) -0.0084(8) C7 0.0413(12) 0.0358(13) 0.0395(13) -0.0060(10) 0.0126(10) -0.0138(10) C8 0.0281(10) 0.0313(11) 0.0283(11) -0.0082(9) 0.0021(9) -0.0051(8) C9 0.0294(11) 0.0399(13) 0.0302(11) -0.0104(10) -0.0021(9) -0.0035(9) C10 0.0379(12) 0.0320(12) 0.0246(11) -0.0065(9) -0.0028(9) -0.0009(9) C11 0.0342(11) 0.0350(12) 0.0247(11) -0.0038(9) 0.0036(9) -0.0080(9) C12 0.0308(10) 0.0277(11) 0.0290(11) -0.0044(9) 0.0008(9) -0.0076(8) C13 0.0326(11) 0.0304(11) 0.0233(10) -0.0034(8) -0.0014(9) -0.0054(9) C14 0.0457(13) 0.0478(14) 0.0256(11) -0.0068(10) -0.0045(10) 0.0017(11) C15 0.067(2) 0.200(5) 0.0382(18) -0.008(2) -0.0221(16) -0.025(3) C16 0.083(2) 0.099(3) 0.0311(15) -0.0206(16) -0.0099(14) 0.0230(19) C17 0.208(5) 0.056(2) 0.0446(19) 0.0078(16) -0.038(2) -0.016(2) C18 0.0289(11) 0.0414(13) 0.0346(12) -0.0030(10) 0.0009(9) -0.0125(9) C19 0.0369(14) 0.089(2) 0.0578(18) -0.0134(16) -0.0029(13) 0.0076(14) C20 0.0539(18) 0.061(2) 0.150(4) -0.018(2) -0.016(2) -0.0282(15) C21 0.0342(14) 0.137(3) 0.0491(17) 0.0197(18) -0.0121(13) -0.0260(17) C22 0.0276(10) 0.0247(10) 0.0255(10) -0.0032(8) 0.0041(8) -0.0080(8) C23 0.0288(10) 0.0295(11) 0.0286(11) -0.0049(9) 0.0018(8) -0.0127(8) C24 0.0270(10) 0.0289(11) 0.0299(11) -0.0018(9) 0.0037(8) -0.0094(8) C25 0.0283(10) 0.0258(11) 0.0304(11) -0.0035(8) 0.0052(9) -0.0083(8) C26 0.0299(10) 0.0283(11) 0.0261(10) -0.0041(8) 0.0056(8) -0.0131(8) C27 0.0233(9) 0.0299(11) 0.0263(10) -0.0015(8) 0.0030(8) -0.0079(8) C28 0.0249(10) 0.0386(13) 0.0427(13) -0.0069(10) -0.0002(9) -0.0072(9) C29 0.0321(12) 0.0511(16) 0.0684(18) -0.0152(13) -0.0138(12) -0.0062(11) C30 0.0398(13) 0.0438(15) 0.074(2) -0.0051(13) -0.0142(13) -0.0007(11) C31 0.0287(12) 0.097(2) 0.0615(18) -0.0132(17) 0.0083(12) -0.0115(14) C32 0.0342(11) 0.0335(12) 0.0346(12) -0.0089(9) 0.0020(9) -0.0145(9) C33 0.0755(19) 0.0509(16) 0.0436(15) -0.0072(12) -0.0170(14) -0.0287(14) C34 0.0478(14) 0.0413(14) 0.0694(18) -0.0283(13) 0.0042(13) -0.0159(11) C35 0.0486(14) 0.0576(16) 0.0593(17) -0.0228(14) 0.0139(13) -0.0324(13) C36 0.087(2) 0.0410(15) 0.0397(15) 0.0008(12) 0.0020(14) -0.0032(14) C37 0.0452(14) 0.0562(16) 0.0365(13) 0.0062(12) 0.0021(11) -0.0082(12) C38 0.0522(16) 0.083(2) 0.0529(17) 0.0091(15) -0.0172(14) -0.0248(15) C39 0.0468(14) 0.0448(15) 0.0501(15) 0.0020(12) 0.0044(12) -0.0068(11) C40 0.0640(19) 0.085(2) 0.0519(18) 0.0258(16) 0.0114(15) -0.0016(16) C41 0.0553(16) 0.0580(18) 0.0643(19) -0.0060(14) -0.0175(14) -0.0082(14) _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 N1 2.1277(18) . ? Sc1 N2 2.1279(17) . ? Sc1 C2 2.210(2) . ? Sc1 C1 2.215(2) . ? Si1 C1 1.841(2) . ? Si1 C36 1.863(3) . ? Si1 C37 1.872(2) . ? Si1 C38 1.876(3) . ? Si2 C2 1.840(2) . ? Si2 C39 1.867(3) . ? Si2 C40 1.874(3) . ? Si2 C41 1.879(3) . ? N1 C4 1.332(3) . ? N1 C8 1.439(3) . ? N2 C6 1.340(3) . ? N2 C22 1.430(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.506(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.401(3) . ? C5 C6 1.397(3) . ? C5 H5 0.9500 . ? C6 C7 1.511(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.389(3) . ? C8 C9 1.393(3) . ? C9 C10 1.387(3) . ? C9 H9 0.9500 . ? C10 C11 1.394(3) . ? C10 C14 1.539(3) . ? C11 C12 1.398(3) . ? C11 H11 0.9500 . ? C12 C13 1.393(3) . ? C12 C18 1.534(3) . ? C13 H13 0.9500 . ? C14 C17 1.508(4) . ? C14 C16 1.513(3) . ? C14 C15 1.517(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.519(4) . ? C18 C21 1.519(3) . ? C18 C19 1.520(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.388(3) . ? C22 C23 1.398(3) . ? C23 C24 1.383(3) . ? C23 H23 0.9500 . ? C24 C25 1.403(3) . ? C24 C28 1.534(3) . ? C25 C26 1.387(3) . ? C25 H25 0.9500 . ? C26 C27 1.403(3) . ? C26 C32 1.537(3) . ? C27 H27 0.9500 . ? C28 C29 1.526(3) . ? C28 C31 1.527(3) . ? C28 C30 1.542(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.527(3) . ? C32 C34 1.528(3) . ? C32 C35 1.531(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sc1 N2 83.06(6) . . ? N1 Sc1 C2 112.89(9) . . ? N2 Sc1 C2 122.74(8) . . ? N1 Sc1 C1 111.31(7) . . ? N2 Sc1 C1 111.89(7) . . ? C2 Sc1 C1 111.65(8) . . ? C1 Si1 C36 109.67(11) . . ? C1 Si1 C37 111.25(11) . . ? C36 Si1 C37 107.63(13) . . ? C1 Si1 C38 112.71(12) . . ? C36 Si1 C38 108.10(14) . . ? C37 Si1 C38 107.30(13) . . ? C2 Si2 C39 110.14(12) . . ? C2 Si2 C40 114.54(12) . . ? C39 Si2 C40 106.24(14) . . ? C2 Si2 C41 109.73(12) . . ? C39 Si2 C41 108.58(13) . . ? C40 Si2 C41 107.39(15) . . ? C4 N1 C8 121.58(17) . . ? C4 N1 Sc1 129.85(14) . . ? C8 N1 Sc1 108.23(12) . . ? C6 N2 C22 122.07(16) . . ? C6 N2 Sc1 129.30(13) . . ? C22 N2 Sc1 108.47(12) . . ? Si1 C1 Sc1 123.33(10) . . ? Si1 C1 H1A 106.5 . . ? Sc1 C1 H1A 106.5 . . ? Si1 C1 H1B 106.5 . . ? Sc1 C1 H1B 106.5 . . ? H1A C1 H1B 106.5 . . ? Si2 C2 Sc1 121.11(11) . . ? Si2 C2 H2A 107.0 . . ? Sc1 C2 H2A 107.0 . . ? Si2 C2 H2B 107.0 . . ? Sc1 C2 H2B 107.0 . . ? H2A C2 H2B 106.8 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 122.44(18) . . ? N1 C4 C3 120.03(19) . . ? C5 C4 C3 117.53(19) . . ? C6 C5 C4 128.17(19) . . ? C6 C5 H5 115.9 . . ? C4 C5 H5 115.9 . . ? N2 C6 C5 122.18(18) . . ? N2 C6 C7 120.48(18) . . ? C5 C6 C7 117.32(18) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 120.01(19) . . ? C13 C8 N1 118.71(18) . . ? C9 C8 N1 120.80(17) . . ? C10 C9 C8 120.57(19) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 118.25(19) . . ? C9 C10 C14 121.83(19) . . ? C11 C10 C14 119.9(2) . . ? C10 C11 C12 122.62(19) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 117.51(18) . . ? C13 C12 C18 121.74(18) . . ? C11 C12 C18 120.71(19) . . ? C8 C13 C12 121.03(19) . . ? C8 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C17 C14 C16 109.6(3) . . ? C17 C14 C15 108.6(3) . . ? C16 C14 C15 107.3(3) . . ? C17 C14 C10 108.7(2) . . ? C16 C14 C10 110.69(19) . . ? C15 C14 C10 111.8(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C21 109.5(3) . . ? C20 C18 C19 108.9(2) . . ? C21 C18 C19 107.0(2) . . ? C20 C18 C12 108.52(19) . . ? C21 C18 C12 111.85(18) . . ? C19 C18 C12 111.04(19) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 119.60(18) . . ? C27 C22 N2 117.83(17) . . ? C23 C22 N2 122.15(17) . . ? C24 C23 C22 120.84(18) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 118.19(18) . . ? C23 C24 C28 122.15(18) . . ? C25 C24 C28 119.65(18) . . ? C26 C25 C24 122.61(19) . . ? C26 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C25 C26 C27 117.53(18) . . ? C25 C26 C32 123.17(18) . . ? C27 C26 C32 119.30(18) . . ? C22 C27 C26 121.15(18) . . ? C22 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C29 C28 C31 109.4(2) . . ? C29 C28 C24 112.40(18) . . ? C31 C28 C24 109.13(19) . . ? C29 C28 C30 107.2(2) . . ? C31 C28 C30 109.5(2) . . ? C24 C28 C30 109.18(18) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C34 108.3(2) . . ? C33 C32 C35 109.9(2) . . ? C34 C32 C35 107.59(19) . . ? C33 C32 C26 109.57(18) . . ? C34 C32 C26 112.49(18) . . ? C35 C32 C26 108.94(17) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si1 C37 H37A 109.5 . . ? Si1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si1 C38 H38A 109.5 . . ? Si1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si2 C40 H40A 109.5 . . ? Si2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si2 C41 H41A 109.5 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? 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 N2 Sc1 N1 C4 -20.11(18) . . . . ? C2 Sc1 N1 C4 -142.80(18) . . . . ? C1 Sc1 N1 C4 90.72(18) . . . . ? N2 Sc1 N1 C8 166.59(13) . . . . ? C2 Sc1 N1 C8 43.91(14) . . . . ? C1 Sc1 N1 C8 -82.57(14) . . . . ? N1 Sc1 N2 C6 22.88(17) . . . . ? C2 Sc1 N2 C6 135.68(17) . . . . ? C1 Sc1 N2 C6 -87.35(18) . . . . ? N1 Sc1 N2 C22 -161.60(13) . . . . ? C2 Sc1 N2 C22 -48.80(16) . . . . ? C1 Sc1 N2 C22 88.17(14) . . . . ? C36 Si1 C1 Sc1 61.29(17) . . . . ? C37 Si1 C1 Sc1 -57.65(16) . . . . ? C38 Si1 C1 Sc1 -178.22(14) . . . . ? N1 Sc1 C1 Si1 -55.30(14) . . . . ? N2 Sc1 C1 Si1 35.67(15) . . . . ? C2 Sc1 C1 Si1 177.54(12) . . . . ? C39 Si2 C2 Sc1 84.29(16) . . . . ? C40 Si2 C2 Sc1 -156.04(16) . . . . ? C41 Si2 C2 Sc1 -35.19(19) . . . . ? N1 Sc1 C2 Si2 77.93(15) . . . . ? N2 Sc1 C2 Si2 -18.70(19) . . . . ? C1 Sc1 C2 Si2 -155.76(13) . . . . ? C8 N1 C4 C5 -177.12(18) . . . . ? Sc1 N1 C4 C5 10.4(3) . . . . ? C8 N1 C4 C3 3.0(3) . . . . ? Sc1 N1 C4 C3 -169.52(16) . . . . ? N1 C4 C5 C6 7.9(3) . . . . ? C3 C4 C5 C6 -172.2(2) . . . . ? C22 N2 C6 C5 169.02(18) . . . . ? Sc1 N2 C6 C5 -16.0(3) . . . . ? C22 N2 C6 C7 -12.5(3) . . . . ? Sc1 N2 C6 C7 162.52(15) . . . . ? C4 C5 C6 N2 -5.0(3) . . . . ? C4 C5 C6 C7 176.4(2) . . . . ? C4 N1 C8 C13 -105.4(2) . . . . ? Sc1 N1 C8 C13 68.6(2) . . . . ? C4 N1 C8 C9 82.6(3) . . . . ? Sc1 N1 C8 C9 -103.44(19) . . . . ? C13 C8 C9 C10 -0.6(3) . . . . ? N1 C8 C9 C10 171.32(19) . . . . ? C8 C9 C10 C11 -0.1(3) . . . . ? C8 C9 C10 C14 -177.7(2) . . . . ? C9 C10 C11 C12 1.0(3) . . . . ? C14 C10 C11 C12 178.7(2) . . . . ? C10 C11 C12 C13 -1.3(3) . . . . ? C10 C11 C12 C18 -178.92(19) . . . . ? C9 C8 C13 C12 0.4(3) . . . . ? N1 C8 C13 C12 -171.73(18) . . . . ? C11 C12 C13 C8 0.6(3) . . . . ? C18 C12 C13 C8 178.18(19) . . . . ? C9 C10 C14 C17 107.7(3) . . . . ? C11 C10 C14 C17 -69.9(3) . . . . ? C9 C10 C14 C16 -131.8(3) . . . . ? C11 C10 C14 C16 50.6(3) . . . . ? C9 C10 C14 C15 -12.2(3) . . . . ? C11 C10 C14 C15 170.2(3) . . . . ? C13 C12 C18 C20 -103.3(3) . . . . ? C11 C12 C18 C20 74.2(3) . . . . ? C13 C12 C18 C21 17.6(3) . . . . ? C11 C12 C18 C21 -164.9(2) . . . . ? C13 C12 C18 C19 137.1(2) . . . . ? C11 C12 C18 C19 -45.4(3) . . . . ? C6 N2 C22 C27 131.0(2) . . . . ? Sc1 N2 C22 C27 -44.9(2) . . . . ? C6 N2 C22 C23 -56.5(3) . . . . ? Sc1 N2 C22 C23 127.54(17) . . . . ? C27 C22 C23 C24 -2.4(3) . . . . ? N2 C22 C23 C24 -174.76(19) . . . . ? C22 C23 C24 C25 1.3(3) . . . . ? C22 C23 C24 C28 -179.50(19) . . . . ? C23 C24 C25 C26 1.3(3) . . . . ? C28 C24 C25 C26 -177.89(19) . . . . ? C24 C25 C26 C27 -2.7(3) . . . . ? C24 C25 C26 C32 177.15(19) . . . . ? C23 C22 C27 C26 0.9(3) . . . . ? N2 C22 C27 C26 173.58(18) . . . . ? C25 C26 C27 C22 1.6(3) . . . . ? C32 C26 C27 C22 -178.30(18) . . . . ? C23 C24 C28 C29 -5.9(3) . . . . ? C25 C24 C28 C29 173.3(2) . . . . ? C23 C24 C28 C31 115.7(2) . . . . ? C25 C24 C28 C31 -65.2(3) . . . . ? C23 C24 C28 C30 -124.7(2) . . . . ? C25 C24 C28 C30 54.5(3) . . . . ? C25 C26 C32 C33 118.5(2) . . . . ? C27 C26 C32 C33 -61.6(3) . . . . ? C25 C26 C32 C34 -2.0(3) . . . . ? C27 C26 C32 C34 177.9(2) . . . . ? C25 C26 C32 C35 -121.2(2) . . . . ? C27 C26 C32 C35 58.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.494 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.051