Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Baskett, Martha' 'Lahti, Paul' 'Liao, Yi' 'Palacio, Fernando' _publ_contact_author_name 'Prof Paul Lahti' _publ_contact_author_address ; Chemistry University of Massachusetts Lederle GRT 713J Amherst MA 01003 UNITED STATES OF AMERICA ; _publ_contact_author_email 'LAHTI@CHEM.UMASS.EDU' _publ_section_title ; Structure and Exchange in Silicon-Linked Tetraradicals. ; data_mb28 _database_code_CSD 172624 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H68 N4 O8 Si' _chemical_formula_weight 713.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 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 19.0646(3) _cell_length_b 11.8693(2) _cell_length_c 19.1899(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.5005(11) _cell_angle_gamma 90.00 _cell_volume 4269.64(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7456 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.55 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9453 _exptl_absorpt_correction_T_max 0.9453 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13651 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7471 _reflns_number_gt 5113 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0615P)^2^+1.9599P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7471 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1569 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.000 _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 Si Si 0.25665(3) 0.04381(6) 0.96593(3) 0.04963(19) Uani 1 1 d . . . O1 O 0.22812(8) 0.14513(13) 1.01021(8) 0.0531(4) Uani 1 1 d . . . O2 O 0.22982(10) 0.06803(14) 0.88286(8) 0.0653(5) Uani 1 1 d . . . O3 O 0.34185(9) 0.04272(15) 0.98899(9) 0.0646(5) Uani 1 1 d . . . O4 O 0.22500(9) -0.07866(14) 0.98140(8) 0.0573(4) Uani 1 1 d . . . O5 O -0.03345(12) 0.3405(2) 1.00451(12) 0.1096(9) Uani 1 1 d . . . O6 O 0.11309(14) -0.1104(3) 0.62601(11) 0.1164(9) Uani 1 1 d . . . O7 O 0.56685(19) 0.2607(3) 1.15000(17) 0.1729(16) Uani 1 1 d . . . O8 O 0.22536(16) -0.3430(2) 1.21569(12) 0.1122(9) Uani 1 1 d . . . N1 N 0.03042(12) 0.3029(2) 1.00744(12) 0.0689(6) Uani 1 1 d . . . N2 N 0.14071(12) -0.0694(2) 0.68632(11) 0.0693(6) Uani 1 1 d . . . N3 N 0.51548(14) 0.2081(3) 1.11085(14) 0.0950(9) Uani 1 1 d . . . N4 N 0.22404(13) -0.28097(19) 1.16097(12) 0.0696(6) Uani 1 1 d . . . C1 C 0.05477(14) 0.2953(2) 0.93809(13) 0.0621(7) Uani 1 1 d . . . C2 C 0.13361(13) 0.2645(2) 0.94972(12) 0.0556(6) Uani 1 1 d . . . H2A H 0.1455 0.2411 0.9049 0.067 Uiso 1 1 calc R . . H2B H 0.1617 0.3309 0.9655 0.067 Uiso 1 1 calc R . . C3 C 0.15377(11) 0.17206(19) 1.00301(11) 0.0473(5) Uani 1 1 d . . . H3 H 0.1251 0.1048 0.9880 0.057 Uiso 1 1 calc R . . C4 C 0.13875(13) 0.2123(2) 1.07359(12) 0.0537(6) Uani 1 1 d . . . H4A H 0.1661 0.2802 1.0874 0.064 Uiso 1 1 calc R . . H4B H 0.1544 0.1553 1.1092 0.064 Uiso 1 1 calc R . . C5 C 0.06012(13) 0.2369(2) 1.07172(13) 0.0568(6) Uani 1 1 d . . . C6 C 0.0433(2) 0.4112(3) 0.90302(18) 0.0978(11) Uani 1 1 d . . . H6A H 0.0724 0.4658 0.9318 0.147 Uiso 1 1 calc R . . H6B H -0.0060 0.4321 0.8983 0.147 Uiso 1 1 calc R . . H6C H 0.0563 0.4083 0.8570 0.147 Uiso 1 1 calc R . . C7 C 0.00928(16) 0.2080(3) 0.89215(16) 0.0880(10) Uani 1 1 d . . . H7A H -0.0401 0.2291 0.8862 0.132 Uiso 1 1 calc R . . H7B H 0.0159 0.1356 0.9147 0.132 Uiso 1 1 calc R . . H7C H 0.0233 0.2043 0.8466 0.132 Uiso 1 1 calc R . . C8 C 0.05070(15) 0.3088(3) 1.13531(15) 0.0724(8) Uani 1 1 d . . . H8A H 0.0009 0.3236 1.1335 0.109 Uiso 1 1 calc R . . H8B H 0.0757 0.3788 1.1341 0.109 Uiso 1 1 calc R . . H8C H 0.0696 0.2693 1.1783 0.109 Uiso 1 1 calc R . . C9 C 0.01697(18) 0.1278(3) 1.0717(2) 0.0934(10) Uani 1 1 d . . . H9A H -0.0323 0.1459 1.0704 0.140 Uiso 1 1 calc R . . H9B H 0.0348 0.0854 1.1138 0.140 Uiso 1 1 calc R . . H9C H 0.0214 0.0838 1.0307 0.140 Uiso 1 1 calc R . . C11 C 0.21573(14) -0.0321(2) 0.69434(13) 0.0646(7) Uani 1 1 d . . . C12 C 0.23488(14) 0.0394(2) 0.76087(12) 0.0607(6) Uani 1 1 d . . . H12A H 0.2862 0.0496 0.7712 0.073 Uiso 1 1 calc R . . H12B H 0.2133 0.1131 0.7516 0.073 Uiso 1 1 calc R . . C13 C 0.21140(13) -0.0099(2) 0.82510(11) 0.0534(6) Uani 1 1 d . . . H13 H 0.2348 -0.0826 0.8372 0.064 Uiso 1 1 calc R . . C14 C 0.13172(14) -0.0244(2) 0.80939(13) 0.0641(7) Uani 1 1 d . . . H14A H 0.1097 0.0491 0.8004 0.077 Uiso 1 1 calc R . . H14B H 0.1165 -0.0554 0.8510 0.077 Uiso 1 1 calc R . . C15 C 0.10509(15) -0.1004(3) 0.74645(14) 0.0689(7) Uani 1 1 d . . . C16 C 0.2211(2) 0.0401(4) 0.62950(15) 0.1048(12) Uani 1 1 d . . . H16A H 0.1905 0.1045 0.6284 0.157 Uiso 1 1 calc R . . H16B H 0.2067 -0.0036 0.5872 0.157 Uiso 1 1 calc R . . H16C H 0.2695 0.0646 0.6321 0.157 Uiso 1 1 calc R . . C17 C 0.26435(19) -0.1351(3) 0.6972(2) 0.1035(12) Uani 1 1 d . . . H17A H 0.2604 -0.1797 0.7381 0.155 Uiso 1 1 calc R . . H17B H 0.3129 -0.1109 0.7002 0.155 Uiso 1 1 calc R . . H17C H 0.2503 -0.1794 0.6552 0.155 Uiso 1 1 calc R . . C18 C 0.02515(17) -0.0813(4) 0.72166(19) 0.1142(14) Uani 1 1 d . . . H18A H 0.0081 -0.1290 0.6818 0.171 Uiso 1 1 calc R . . H18B H 0.0168 -0.0039 0.7081 0.171 Uiso 1 1 calc R . . H18C H 0.0003 -0.0989 0.7595 0.171 Uiso 1 1 calc R . . C19 C 0.1192(2) -0.2246(3) 0.7652(2) 0.1083(12) Uani 1 1 d . . . H19A H 0.1024 -0.2703 0.7243 0.163 Uiso 1 1 calc R . . H19B H 0.0946 -0.2453 0.8027 0.163 Uiso 1 1 calc R . . H19C H 0.1695 -0.2363 0.7804 0.163 Uiso 1 1 calc R . . C21 C 0.48187(16) 0.1187(3) 1.14675(15) 0.0823(9) Uani 1 1 d . . . C22 C 0.43172(16) 0.0503(3) 1.09286(15) 0.0770(8) Uani 1 1 d . . . H22A H 0.4596 -0.0022 1.0704 0.092 Uiso 1 1 calc R . . H22B H 0.4009 0.0065 1.1175 0.092 Uiso 1 1 calc R . . C23 C 0.38642(12) 0.1181(2) 1.03676(13) 0.0569(6) Uani 1 1 d . . . H23 H 0.3566 0.1701 1.0583 0.068 Uiso 1 1 calc R . . C24 C 0.43340(17) 0.1829(3) 0.99700(14) 0.0786(8) Uani 1 1 d . . . H24A H 0.4036 0.2252 0.9595 0.094 Uiso 1 1 calc R . . H24B H 0.4614 0.1302 0.9748 0.094 Uiso 1 1 calc R . . C25 C 0.4839(2) 0.2644(3) 1.04268(17) 0.1015(12) Uani 1 1 d . . . C26 C 0.5410(3) 0.0431(4) 1.1854(3) 0.163(2) Uani 1 1 d . . . H26A H 0.5727 0.0868 1.2198 0.245 Uiso 1 1 calc R . . H26B H 0.5672 0.0115 1.1519 0.245 Uiso 1 1 calc R . . H26C H 0.5205 -0.0164 1.2090 0.245 Uiso 1 1 calc R . . C27 C 0.4424(3) 0.1745(6) 1.2001(2) 0.172(3) Uani 1 1 d . . . H27A H 0.4755 0.2176 1.2334 0.257 Uiso 1 1 calc R . . H27B H 0.4209 0.1175 1.2249 0.257 Uiso 1 1 calc R . . H27C H 0.4060 0.2233 1.1756 0.257 Uiso 1 1 calc R . . C28 C 0.5449(3) 0.2943(6) 1.0037(3) 0.185(3) Uani 1 1 d . . . H28A H 0.5687 0.2266 0.9936 0.278 Uiso 1 1 calc R . . H28B H 0.5782 0.3429 1.0329 0.278 Uiso 1 1 calc R . . H28C H 0.5258 0.3320 0.9601 0.278 Uiso 1 1 calc R . . C29 C 0.4456(3) 0.3706(4) 1.0585(3) 0.171(3) Uani 1 1 d . . . H29A H 0.4785 0.4194 1.0881 0.257 Uiso 1 1 calc R . . H29B H 0.4073 0.3512 1.0826 0.257 Uiso 1 1 calc R . . H29C H 0.4267 0.4085 1.0150 0.257 Uiso 1 1 calc R . . C31 C 0.23093(15) -0.1579(2) 1.17455(13) 0.0659(7) Uani 1 1 d . . . C32 C 0.21281(15) -0.0944(2) 1.10442(12) 0.0634(7) Uani 1 1 d . . . H32A H 0.1614 -0.0945 1.0892 0.076 Uiso 1 1 calc R . . H32B H 0.2279 -0.0166 1.1123 0.076 Uiso 1 1 calc R . . C33 C 0.24644(13) -0.1417(2) 1.04558(12) 0.0533(6) Uani 1 1 d . . . H33 H 0.2985 -0.1395 1.0594 0.064 Uiso 1 1 calc R . . C34 C 0.22233(15) -0.2619(2) 1.03233(13) 0.0618(6) Uani 1 1 d . . . H34A H 0.2436 -0.2922 0.9941 0.074 Uiso 1 1 calc R . . H34B H 0.1710 -0.2628 1.0169 0.074 Uiso 1 1 calc R . . C35 C 0.24167(15) -0.3382(2) 1.09690(15) 0.0670(7) Uani 1 1 d . . . C36 C 0.30635(18) -0.1306(3) 1.21295(16) 0.0992(12) Uani 1 1 d . . . H36A H 0.3164 -0.1721 1.2566 0.149 Uiso 1 1 calc R . . H36B H 0.3101 -0.0514 1.2229 0.149 Uiso 1 1 calc R . . H36C H 0.3400 -0.1513 1.1835 0.149 Uiso 1 1 calc R . . C37 C 0.17908(19) -0.1238(3) 1.22261(16) 0.0932(10) Uani 1 1 d . . . H37A H 0.1312 -0.1405 1.1996 0.140 Uiso 1 1 calc R . . H37B H 0.1834 -0.0445 1.2322 0.140 Uiso 1 1 calc R . . H37C H 0.1900 -0.1649 1.2663 0.140 Uiso 1 1 calc R . . C38 C 0.32121(18) -0.3685(3) 1.1112(2) 0.1024(11) Uani 1 1 d . . . H38A H 0.3316 -0.4160 1.1523 0.154 Uiso 1 1 calc R . . H38B H 0.3491 -0.3009 1.1193 0.154 Uiso 1 1 calc R . . H38C H 0.3327 -0.4076 1.0710 0.154 Uiso 1 1 calc R . . C39 C 0.1974(2) -0.4458(3) 1.08518(19) 0.0934(10) Uani 1 1 d . . . H39A H 0.2090 -0.4934 1.1261 0.140 Uiso 1 1 calc R . . H39B H 0.2077 -0.4848 1.0444 0.140 Uiso 1 1 calc R . . H39C H 0.1476 -0.4271 1.0777 0.140 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 Si 0.0550(4) 0.0501(4) 0.0409(3) -0.0029(3) 0.0011(3) -0.0011(3) O1 0.0495(9) 0.0587(10) 0.0481(8) -0.0071(7) 0.0008(7) 0.0033(7) O2 0.0980(13) 0.0519(10) 0.0412(8) -0.0021(7) 0.0004(8) -0.0055(9) O3 0.0544(10) 0.0648(11) 0.0726(11) -0.0223(9) 0.0065(8) 0.0001(8) O4 0.0691(10) 0.0528(10) 0.0442(8) 0.0038(7) -0.0048(7) -0.0059(8) O5 0.0689(13) 0.158(2) 0.0966(16) -0.0177(16) 0.0006(11) 0.0443(14) O6 0.1239(19) 0.164(3) 0.0576(12) -0.0452(15) 0.0064(12) -0.0429(18) O7 0.155(3) 0.194(3) 0.133(2) 0.017(2) -0.073(2) -0.088(3) O8 0.169(2) 0.0868(16) 0.0839(15) 0.0349(13) 0.0302(15) -0.0108(16) N1 0.0579(13) 0.0796(16) 0.0652(13) -0.0062(12) 0.0005(10) 0.0157(11) N2 0.0773(15) 0.0817(16) 0.0468(11) -0.0163(11) 0.0056(10) -0.0094(12) N3 0.0809(17) 0.107(2) 0.0821(17) 0.0056(16) -0.0243(14) -0.0283(16) N4 0.0829(16) 0.0609(14) 0.0624(13) 0.0145(11) 0.0066(11) -0.0076(12) C1 0.0677(16) 0.0639(16) 0.0498(13) 0.0019(12) -0.0025(12) 0.0148(13) C2 0.0634(15) 0.0533(14) 0.0494(13) 0.0055(11) 0.0083(11) 0.0003(12) C3 0.0460(12) 0.0463(13) 0.0471(12) -0.0008(10) 0.0022(10) -0.0011(10) C4 0.0609(14) 0.0517(14) 0.0465(12) 0.0027(11) 0.0046(11) 0.0044(11) C5 0.0587(14) 0.0553(15) 0.0565(14) -0.0071(11) 0.0106(12) -0.0062(12) C6 0.124(3) 0.079(2) 0.083(2) 0.0179(18) 0.001(2) 0.033(2) C7 0.0745(19) 0.106(3) 0.0723(18) -0.0214(18) -0.0172(15) 0.0055(18) C8 0.0746(18) 0.0764(19) 0.0680(17) -0.0114(14) 0.0178(14) 0.0039(15) C9 0.098(2) 0.081(2) 0.111(3) -0.0209(19) 0.046(2) -0.0346(19) C11 0.0712(17) 0.0746(18) 0.0505(13) -0.0098(13) 0.0173(12) -0.0051(14) C12 0.0711(16) 0.0600(16) 0.0507(13) -0.0027(12) 0.0104(12) -0.0098(13) C13 0.0708(15) 0.0457(13) 0.0412(12) -0.0041(10) 0.0035(11) -0.0027(11) C14 0.0702(16) 0.0758(18) 0.0476(13) -0.0012(12) 0.0138(12) -0.0029(14) C15 0.0672(16) 0.080(2) 0.0580(15) -0.0055(14) 0.0082(13) -0.0147(15) C16 0.126(3) 0.140(3) 0.0524(16) 0.0007(19) 0.0269(18) -0.031(3) C17 0.099(2) 0.109(3) 0.109(3) -0.035(2) 0.036(2) 0.013(2) C18 0.074(2) 0.178(4) 0.086(2) -0.007(3) 0.0029(18) -0.026(2) C19 0.135(3) 0.075(2) 0.116(3) -0.006(2) 0.026(2) -0.035(2) C21 0.0788(19) 0.104(2) 0.0560(16) 0.0084(16) -0.0086(14) -0.0038(18) C22 0.0832(19) 0.0759(19) 0.0664(16) 0.0145(15) -0.0007(14) -0.0117(16) C23 0.0472(13) 0.0641(16) 0.0564(13) -0.0163(12) 0.0013(11) 0.0018(12) C24 0.090(2) 0.080(2) 0.0581(15) 0.0087(15) -0.0061(14) -0.0195(17) C25 0.120(3) 0.097(3) 0.073(2) 0.0126(19) -0.0210(19) -0.045(2) C26 0.150(4) 0.150(4) 0.150(4) 0.038(3) -0.079(3) 0.014(3) C27 0.139(4) 0.305(8) 0.072(2) -0.067(4) 0.022(2) -0.033(4) C28 0.169(5) 0.251(7) 0.128(4) 0.035(4) 0.009(3) -0.135(5) C29 0.260(6) 0.070(3) 0.141(4) -0.015(3) -0.075(4) -0.015(3) C31 0.0788(18) 0.0661(17) 0.0491(13) 0.0027(12) 0.0020(13) -0.0116(14) C32 0.0821(18) 0.0538(15) 0.0507(13) 0.0006(12) 0.0026(13) 0.0004(13) C33 0.0565(14) 0.0495(14) 0.0497(13) 0.0071(10) -0.0014(11) -0.0005(11) C34 0.0725(16) 0.0517(15) 0.0587(14) -0.0023(12) 0.0055(13) -0.0021(12) C35 0.0741(17) 0.0501(15) 0.0755(17) 0.0095(13) 0.0101(14) 0.0014(13) C36 0.107(2) 0.115(3) 0.0621(17) 0.0137(18) -0.0214(17) -0.037(2) C37 0.118(3) 0.102(3) 0.0627(17) -0.0085(17) 0.0244(18) -0.016(2) C38 0.091(2) 0.091(2) 0.126(3) 0.034(2) 0.021(2) 0.025(2) C39 0.120(3) 0.0529(18) 0.106(2) 0.0063(17) 0.017(2) -0.0116(18) _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 Si O1 1.6225(17) . ? Si O2 1.6088(16) . ? Si O3 1.6038(17) . ? Si O4 1.6219(17) . ? O1 C3 1.435(3) . ? O2 C13 1.437(3) . ? O3 C23 1.442(3) . ? O4 C33 1.436(3) . ? O5 N1 1.288(3) . ? O6 N2 1.278(3) . ? O7 N3 1.283(3) . ? O8 N4 1.279(3) . ? N1 C1 1.490(3) . ? N1 C5 1.484(3) . ? N2 C11 1.478(3) . ? N2 C15 1.488(3) . ? N3 C21 1.474(4) . ? N3 C25 1.495(4) . ? N4 C31 1.486(4) . ? N4 C35 1.496(4) . ? C1 C2 1.523(3) . ? C1 C6 1.529(4) . ? C1 C7 1.525(4) . ? C2 C3 1.501(3) . ? C3 C4 1.512(3) . ? C4 C5 1.521(3) . ? C5 C8 1.526(3) . ? C5 C9 1.534(4) . ? C11 C12 1.521(3) . ? C11 C16 1.530(4) . ? C11 C17 1.529(4) . ? C12 C13 1.504(3) . ? C13 C14 1.504(4) . ? C14 C15 1.519(4) . ? C15 C18 1.528(4) . ? C15 C19 1.529(4) . ? C21 C22 1.510(4) . ? C21 C26 1.524(5) . ? C21 C27 1.528(5) . ? C22 C23 1.488(4) . ? C23 C24 1.492(4) . ? C24 C25 1.524(4) . ? C25 C29 1.515(6) . ? C25 C28 1.534(6) . ? C31 C32 1.526(3) . ? C31 C36 1.526(4) . ? C31 C37 1.524(4) . ? C32 C33 1.505(3) . ? C33 C34 1.505(3) . ? C34 C35 1.525(4) . ? C35 C39 1.525(4) . ? C35 C38 1.534(4) . ? 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 O3 Si O2 113.45(10) . . ? O3 Si O4 109.52(10) . . ? O2 Si O4 106.25(9) . . ? O3 Si O1 106.31(9) . . ? O2 Si O1 108.06(9) . . ? O4 Si O1 113.39(9) . . ? C3 O1 Si 122.29(13) . . ? C13 O2 Si 129.65(15) . . ? C23 O3 Si 128.34(15) . . ? C33 O4 Si 124.56(14) . . ? O5 N1 C5 115.7(2) . . ? O5 N1 C1 115.3(2) . . ? C5 N1 C1 125.2(2) . . ? O6 N2 C11 116.1(2) . . ? O6 N2 C15 115.9(2) . . ? C11 N2 C15 124.3(2) . . ? O7 N3 C21 115.3(3) . . ? O7 N3 C25 116.0(3) . . ? C21 N3 C25 126.2(2) . . ? O8 N4 C31 115.7(2) . . ? O8 N4 C35 116.1(2) . . ? C31 N4 C35 124.4(2) . . ? N1 C1 C2 110.08(19) . . ? N1 C1 C7 108.7(2) . . ? C2 C1 C7 111.3(2) . . ? N1 C1 C6 107.2(2) . . ? C2 C1 C6 109.8(3) . . ? C7 C1 C6 109.6(2) . . ? C3 C2 C1 113.5(2) . . ? O1 C3 C2 110.74(18) . . ? O1 C3 C4 109.21(17) . . ? C2 C3 C4 108.22(19) . . ? C3 C4 C5 112.71(19) . . ? N1 C5 C4 110.2(2) . . ? N1 C5 C8 106.7(2) . . ? C4 C5 C8 110.3(2) . . ? N1 C5 C9 108.8(2) . . ? C4 C5 C9 111.4(2) . . ? C8 C5 C9 109.4(2) . . ? N2 C11 C12 109.5(2) . . ? N2 C11 C17 109.5(2) . . ? C12 C11 C17 111.4(2) . . ? N2 C11 C16 106.8(2) . . ? C12 C11 C16 109.2(2) . . ? C17 C11 C16 110.3(3) . . ? C13 C12 C11 114.2(2) . . ? O2 C13 C14 108.9(2) . . ? O2 C13 C12 108.33(19) . . ? C14 C13 C12 108.7(2) . . ? C13 C14 C15 114.0(2) . . ? N2 C15 C14 109.6(2) . . ? N2 C15 C18 107.0(2) . . ? C14 C15 C18 109.2(3) . . ? N2 C15 C19 109.6(3) . . ? C14 C15 C19 111.5(3) . . ? C18 C15 C19 109.8(3) . . ? N3 C21 C22 110.0(2) . . ? N3 C21 C26 107.8(3) . . ? C22 C21 C26 109.7(3) . . ? N3 C21 C27 108.1(4) . . ? C22 C21 C27 111.3(3) . . ? C26 C21 C27 109.9(4) . . ? C23 C22 C21 114.6(3) . . ? O3 C23 C22 108.8(2) . . ? O3 C23 C24 109.5(2) . . ? C22 C23 C24 109.0(2) . . ? C23 C24 C25 114.1(2) . . ? N3 C25 C29 109.2(3) . . ? N3 C25 C24 109.3(3) . . ? C29 C25 C24 111.5(3) . . ? N3 C25 C28 108.1(4) . . ? C29 C25 C28 110.0(4) . . ? C24 C25 C28 108.7(3) . . ? N4 C31 C37 108.7(2) . . ? N4 C31 C36 109.8(3) . . ? C37 C31 C36 108.0(3) . . ? N4 C31 C32 109.4(2) . . ? C37 C31 C32 109.6(2) . . ? C36 C31 C32 111.3(2) . . ? C33 C32 C31 114.7(2) . . ? O4 C33 C32 110.80(19) . . ? O4 C33 C34 108.58(19) . . ? C32 C33 C34 108.8(2) . . ? C33 C34 C35 113.9(2) . . ? N4 C35 C39 107.5(2) . . ? N4 C35 C34 109.9(2) . . ? C39 C35 C34 109.4(2) . . ? N4 C35 C38 108.8(3) . . ? C39 C35 C38 109.4(3) . . ? C34 C35 C38 111.7(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.240 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.035 data_2 _database_code_CSD 172625 _audit_creation_method 'maXus' _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'needle, 0.150*0.200*0.650 mm' _exptl_crystal_colour 'red' _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment 'refxyz' # Submission details _diffrn_measurement_device 'KappaCCD' _computing_data_collection 'KappaCCD' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 6 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type 'X=UH' _diffrn_orient_matrix_UB_11 -0.03272 _diffrn_orient_matrix_UB_12 0.00452 _diffrn_orient_matrix_UB_13 0.11829 _diffrn_orient_matrix_UB_21 -0.05026 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 -0.07745 _diffrn_orient_matrix_UB_31 -0.00247 _diffrn_orient_matrix_UB_32 -0.05985 _diffrn_orient_matrix_UB_33 0.00893 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 680.966 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz '+X,+Y,+Z' '-X,-Y,-Z' '-X+ 1/2,-Y+ 1/2,+Z' '+X+ 1/2,+Y+ 1/2,-Z' '-Y,+X+ 1/2,+Z+ 1/2' '+Y,-X+ 1/2,-Z+ 1/2' '+Y+ 1/2,-X,+Z+ 1/2' '-Y+ 1/2,+X,-Z+ 1/2' _symmetry_space_group_name_H-M 'P 42/n ' _symmetry_cell_setting 'Tetragonal' _chemical_formula_moiety 'C40 H52 N4 O4 Si ' _chemical_formula_sum 'C40 H52 N4 O4 Si ' _chemical_name_systematic ; ? ; _cell_length_a 16.661(2) _cell_length_b 16.661(2) _cell_length_c 7.0586(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1959.3(4) _diffrn_reflns_number 1092 _diffrn_reflns_theta_max 20.61 _cell_measurement_reflns_used 1075 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 19.980 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_coefficient_mu 0.10 _exptl_crystal_F_000 732 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 'Waasmaier & Kirfel, 1995' 'H ' 'H ' 0.0000 0.0000 'Waasmaier & Kirfel, 1995' 'N ' 'N ' 0.0061 0.0033 'Waasmaier & Kirfel, 1995' 'O ' 'O ' 0.0106 0.0060 'Waasmaier & Kirfel, 1995' 'Si' 'Si' 0.0817 0.0704 'Waasmaier & Kirfel, 1995' _reflns_number_total 987 _reflns_number_gt 518 _reflns_threshold_expression 'I> 3.00 sigma(I)' _reflns_d_resolution_low 1.28 _reflns_d_resolution_high 0.71 _reflns_limit_h_max 16 _reflns_limit_h_min 0 _reflns_limit_k_max 11 _reflns_limit_k_min -11 _reflns_limit_l_max 16 _reflns_limit_l_min 0 _refine_ls_matrix_type full _refine_ls_R_factor_all 0.315 _refine_ls_wR_factor_all 0.264 _refine_ls_R_factor_gt 0.246 _refine_ls_wR_factor_gt 0.218 _refine_ls_wR_factor_ref 0.218 _refine_ls_goodness_of_fit_gt 5.890 _refine_ls_goodness_of_fit_ref 5.890 _refine_ls_goodness_of_fit_all 4.832 _refine_ls_number_parameters 54 _refine_ls_number_reflns 518 _refine_ls_shift/su_max 3.951 _refine_ls_shift/su_mean 0.934 _refine_ls_structure_factor_coef F^2^ _refine_special_details ; Refinement on F^2^. ; _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = 1 / ( s^2^(Fo^2^) + 0.03000 * Fo^2^) ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _computing_structure_refinement 'maxus(Mackay et al., 1999)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material 'maxus(Mackay et al., 1999)' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Si1 0.250000 0.250000 0.250000 0.0786(9) 0.25 Uiso C2 0.3609(3) 0.2391(3) 0.5516(7) 0.088(2) 1.00 Uiso C3 0.3621(3) 0.3668(3) 0.3774(6) 0.098(2) 1.00 Uiso C4 0.3308(3) 0.2892(3) 0.4013(8) 0.089(1) 1.00 Uiso C5 0.4304(3) 0.2613(3) 0.6709(7) 0.116(2) 1.00 Uiso C6 0.4262(4) 0.3956(3) 0.4953(8) 0.131(2) 1.00 Uiso C7 0.4576(4) 0.3408(4) 0.620(1) 0.135(2) 1.00 Uiso C8 0.5763(9) 0.333(1) 0.863(2) 0.273(6) 0.50 Uiso C9 0.5136(5) 0.3186(5) 1.057(1) 0.236(4) 0.50 Uiso N10 0.5282(9) 0.377(1) 0.767(2) 0.322(5) 0.50 Uiso C11 0.6307(7) 0.4169(8) 0.960(2) 0.309(5) 0.50 Uiso O12 0.5105(8) 0.453(1) 0.765(2) 0.293(6) 0.50 Uiso C13 0.6153(6) 0.2602(9) 0.848(2) 0.285(5) 0.50 Uiso 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 C4 Si1 C4 C2 50.0(4) . . . . ? C4 Si1 C4 C3 -128.2(5) . . . . ? C4 Si1 C4 C2 -70.2(5) . . . . ? C4 Si1 C4 C3 111.7(5) . . . . ? C4 Si1 C4 C2 170.1(5) . . . . ? C4 Si1 C4 C3 -8.1(4) . . . . ? C5 C2 C4 Si1 174.4(7) . . . . ? C5 C2 C4 C3 -7.4(5) . . . . ? C4 C2 C5 C7 3.7(5) . . . . ? C6 C3 C4 Si1 -178.9(7) . . . . ? C6 C3 C4 C2 2.9(5) . . . . ? C4 C3 C6 C7 4.6(6) . . . . ? Si1 C4 C2 C5 174.4(7) . . . . ? Si1 C4 C3 C6 -178.9(7) . . . . ? Si1 C4 C2 C5 174.4(7) . . . . ? Si1 C4 C3 C6 -178.9(7) . . . . ? Si1 C4 C2 C5 174.4(7) . . . . ? Si1 C4 C3 C6 -178.9(7) . . . . ? C2 C5 C7 C6 4.9(7) . . . . ? C3 C6 C7 C5 -9.1(6) . . . . ? C13 C8 N10 O12 -157.(4) . . . . ? _geom_special_details ; All standard uncertainties (except dihedral angles between l.s. planes) are estimated using the full covariance matrix. The standard uncertainties in cell dimensions are are used in calculating the standard uncertainties of bond distances, angles and torsion angles. Angles between l.s. planes have standard uncertainties calculated from atomic positional standard uncertainties; the errors in cell dimensions are not used in this case. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C4 1.839(5) . . ? Si1 C4 1.839(5) . 3_555 ? Si1 C4 1.839(5) . 6_556 ? Si1 C4 1.839(5) . 8_656 ? C2 C4 1.440(7) . . ? C2 C5 1.480(7) . . ? C3 C4 1.406(7) . . ? C3 C6 1.436(8) . . ? C5 C7 1.446(9) . . ? C6 C7 1.372(9) . . ? C8 N10 1.28(2) . . ? C8 C13 1.37(2) . . ? N10 O12 1.31(2) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Si1 C4 109.0(3) . . 3_555 ? C4 Si1 C4 109.7(3) . . 6_556 ? C4 Si1 C4 109.7(3) . . 8_656 ? C4 Si1 C4 109.7(3) 3_555 . 6_556 ? C4 Si1 C4 109.7(3) 3_555 . 8_656 ? C4 Si1 C4 109.0(3) 6_556 . 8_656 ? C4 C2 C5 123.2(5) . . . ? C4 C3 C6 120.9(5) . . . ? Si1 C4 C2 118.5(4) . . . ? Si1 C4 C3 121.9(4) . . . ? Si1 C4 C2 118.5(4) 3_555 . . ? Si1 C4 C3 121.9(4) 3_555 . . ? Si1 C4 C2 118.5(4) 6_556 . . ? Si1 C4 C3 121.9(4) 6_556 . . ? Si1 C4 C2 118.5(4) 8_656 . . ? Si1 C4 C3 121.9(4) 8_656 . . ? C2 C4 C3 119.6(5) . . . ? C2 C5 C7 109.5(5) . . . ? C3 C6 C7 115.7(6) . . . ? C5 C7 C6 130.5(6) . . . ? N10 C8 C13 139.(2) . . . ? C8 N10 O12 135.(2) . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Si1 C2 2.824(5) 1_555 3_555 ? Si1 C2 2.824(5) 1_555 6_566 ? Si1 C2 2.824(5) 1_555 8_656 ? Si1 C3 2.844(5) 1_555 3_555 ? Si1 C3 2.844(5) 1_555 6_566 ? Si1 C3 2.844(5) 1_555 8_656 ? C2 C2 3.712(6) 1_555 3_555 ? C2 C2 3.839(7) 1_555 6_567 ? C2 C2 3.839(7) 1_555 8_657 ? C2 C3 3.467(7) 1_555 6_566 ? C2 C4 3.398(7) 1_555 3_555 ? C2 C4 3.606(7) 1_555 6_566 ? C2 C5 3.816(7) 1_555 6_567 ? C3 C4 3.253(7) 1_555 8_656 ? C3 C5 3.939(7) 1_555 8_657 ? C3 C9 3.48(1) 1_555 1_554 ? C3 C9 3.907(9) 1_555 8_657 ? C4 C4 2.993(7) 1_555 3_555 ? C4 C4 3.007(7) 1_555 6_566 ? C4 C4 3.007(7) 1_555 8_656 ? C4 C9 3.93(1) 1_555 1_554 ? C5 C6 3.956(8) 1_555 6_567 ? C5 C11 3.67(1) 1_555 5_644 ? C6 C9 3.65(1) 1_555 1_554 ? C6 O12 3.29(2) 1_555 2_666 ? C11 C13 3.53(2) 1_555 7_565 ? #=================================================== _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Waasmaier, D. & Kirfel, A. (1995). Acta Cryst. A51, 416-431. ; # Intensity data