data_global _journal_coden_Cambridge 207 _publ_requested_journal 'Perkin Transactions 1' loop_ _publ_author_name 'Blakemore, Paul R.' 'Kim, Sung-Kee' 'Schulze, Volker K.' 'White, James D.' 'Yokochi, A.' _publ_contact_author_name 'Prof James D White' _publ_contact_author_address ; Prof James D White Department of Chemistry Oregon State University Corvallis Oregon 97331-4003 UNITED STATES OF AMERICA ; _publ_contact_author_email 'JAMES.WHITE@ORST.EDU' #Compound 28 data_VS042398 _database_code_CSD 163574 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H23 N O3 Si' _chemical_formula_weight 269.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.645(2) _cell_length_b 6.180(1) _cell_length_c 18.791(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.73(1) _cell_angle_gamma 90.00 _cell_volume 1579.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 63 _cell_measurement_theta_min 5.23 _cell_measurement_theta_max 23.34 _exptl_crystal_description 'Trigonal prism' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.7772 _exptl_absorpt_correction_T_max 0.8787 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 3328 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 57.09 _reflns_number_total 2862 _reflns_number_gt 1685 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS V2.20' _computing_cell_refinement 'XSCANS V2.20' _computing_data_reduction 'XSCANS V2.20' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for windows' _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^)+(0.0760P)^2^+1.1046P] 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 SHELXL _refine_ls_extinction_coef 0.0018(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(10) _refine_ls_number_reflns 2862 _refine_ls_number_parameters 328 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1247 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1880 _refine_ls_wR_factor_gt 0.1551 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.085 _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 N1 N 0.9533(10) 0.6801(16) 0.1489(5) 0.104(3) Uani 1 1 d . A . O11 O 0.8763(5) 0.3821(12) 0.2551(3) 0.123(3) Uani 1 1 d . . . O12 O 0.8314(7) 0.758(2) 0.0635(5) 0.213(5) Uani 1 1 d U . . O13 O 1.0187(7) 0.8358(13) 0.1264(5) 0.142(3) Uani 1 1 d . . . C11 C 0.8663(13) 0.635(4) 0.1090(7) 0.150(7) Uani 1 1 d . A . C12 C 0.8350(9) 0.426(3) 0.1302(6) 0.125(5) Uani 1 1 d . . . H12A H 0.8317 0.3269 0.0900 0.150 Uiso 1 1 calc R A . H12B H 0.7704 0.4344 0.1480 0.150 Uiso 1 1 calc R . . C13 C 0.9099(9) 0.3472(18) 0.1885(5) 0.097(3) Uani 1 1 d . A . H13 H 0.9256 0.1941 0.1818 0.116 Uiso 1 1 calc R . . C14 C 0.9986(9) 0.4882(19) 0.1796(5) 0.091(3) Uani 1 1 d . . . H14 H 1.0313 0.5224 0.2266 0.110 Uiso 1 1 calc R A . C15 C 1.0732(8) 0.4115(18) 0.1313(7) 0.101(3) Uani 1 1 d . A . H15 H 1.1018 0.2761 0.1391 0.122 Uiso 1 1 calc R . . C16 C 1.0990(8) 0.529(3) 0.0790(6) 0.113(4) Uani 1 1 d . . . H16 H 1.1407 0.4684 0.0476 0.136 Uiso 1 1 calc R A . C17 C 1.0659(9) 0.752(2) 0.0665(5) 0.123(4) Uani 1 1 d . A . H17A H 1.1219 0.8428 0.0582 0.147 Uiso 1 1 calc R . . H17B H 1.0203 0.7578 0.0242 0.147 Uiso 1 1 calc R . . Si11 Si 0.8053(6) 0.2497(10) 0.3096(4) 0.074(2) Uani 0.50 1 d P A 1 C111 C 0.7636(17) -0.011(4) 0.2443(10) 0.088(8) Uiso 0.50 1 d P A 1 H11A H 0.7310 0.0408 0.2004 0.133 Uiso 0.50 1 calc PR A 1 H11B H 0.7197 -0.1025 0.2680 0.133 Uiso 0.50 1 calc PR A 1 H11C H 0.8209 -0.0923 0.2343 0.133 Uiso 0.50 1 calc PR A 1 C112 C 0.7133(19) 0.406(4) 0.3475(14) 0.094(8) Uiso 0.50 1 d P A 1 H11D H 0.7403 0.5427 0.3629 0.141 Uiso 0.50 1 calc PR A 1 H11E H 0.6907 0.3297 0.3876 0.141 Uiso 0.50 1 calc PR A 1 H11F H 0.6591 0.4283 0.3124 0.141 Uiso 0.50 1 calc PR A 1 C113 C 0.9045(18) 0.129(4) 0.3753(10) 0.092(6) Uiso 0.50 1 d P A 1 C114 C 0.980(3) 0.021(6) 0.3449(19) 0.199(17) Uiso 0.50 1 d P A 1 H11G H 0.9991 0.1023 0.3048 0.299 Uiso 0.50 1 calc PR A 1 H11H H 0.9573 -0.1195 0.3292 0.299 Uiso 0.50 1 calc PR A 1 H11I H 1.0350 0.0059 0.3797 0.299 Uiso 0.50 1 calc PR A 1 C115 C 0.9668(19) 0.306(4) 0.4130(12) 0.138(10) Uiso 0.50 1 d P A 1 H11J H 0.9839 0.2652 0.4617 0.206 Uiso 0.50 1 calc PR A 1 H11K H 0.9300 0.4390 0.4119 0.206 Uiso 0.50 1 calc PR A 1 H11L H 1.0257 0.3268 0.3891 0.206 Uiso 0.50 1 calc PR A 1 C116 C 0.8535(18) -0.008(4) 0.4309(12) 0.134(9) Uiso 0.50 1 d P A 1 H11M H 0.8862 -0.1448 0.4372 0.201 Uiso 0.50 1 calc PR A 1 H11N H 0.7859 -0.0306 0.4143 0.201 Uiso 0.50 1 calc PR A 1 H11O H 0.8569 0.0678 0.4757 0.201 Uiso 0.50 1 calc PR A 1 Si12 Si 0.8524(8) 0.1410(16) 0.2985(4) 0.109(3) Uani 0.50 1 d P A 2 C121 C 0.7338(17) 0.029(4) 0.2621(12) 0.108(9) Uiso 0.50 1 d P A 2 H12C H 0.7115 -0.0762 0.2946 0.163 Uiso 0.50 1 calc PR A 2 H12D H 0.7415 -0.0377 0.2168 0.163 Uiso 0.50 1 calc PR A 2 H12E H 0.6863 0.1440 0.2559 0.163 Uiso 0.50 1 calc PR A 2 C122 C 0.964(2) -0.060(4) 0.3211(14) 0.119(9) Uiso 0.50 1 d P A 2 H12F H 1.0174 0.0174 0.3462 0.178 Uiso 0.50 1 calc PR A 2 H12G H 0.9855 -0.1177 0.2776 0.178 Uiso 0.50 1 calc PR A 2 H12H H 0.9436 -0.1755 0.3504 0.178 Uiso 0.50 1 calc PR A 2 C123 C 0.824(3) 0.246(6) 0.3779(17) 0.175(11) Uiso 0.50 1 d P A 2 C124 C 0.904(2) 0.343(4) 0.4298(12) 0.140(10) Uiso 0.50 1 d P A 2 H12I H 0.9446 0.2300 0.4510 0.210 Uiso 0.50 1 calc PR A 2 H12J H 0.8740 0.4213 0.4665 0.210 Uiso 0.50 1 calc PR A 2 H12K H 0.9437 0.4406 0.4045 0.210 Uiso 0.50 1 calc PR A 2 C125 C 0.740(2) 0.415(5) 0.3681(15) 0.126(12) Uiso 0.50 1 d P A 2 H12L H 0.7178 0.4501 0.4138 0.188 Uiso 0.50 1 calc PR A 2 H12M H 0.6867 0.3561 0.3378 0.188 Uiso 0.50 1 calc PR A 2 H12N H 0.7642 0.5435 0.3467 0.188 Uiso 0.50 1 calc PR A 2 C126 C 0.7833(19) 0.028(5) 0.4277(13) 0.148(10) Uiso 0.50 1 d P A 2 H12O H 0.8325 -0.0836 0.4310 0.222 Uiso 0.50 1 calc PR A 2 H12P H 0.7234 -0.0286 0.4045 0.222 Uiso 0.50 1 calc PR A 2 H12Q H 0.7717 0.0768 0.4748 0.222 Uiso 0.50 1 calc PR A 2 N2 N 0.4114(9) -0.5596(12) 0.1368(4) 0.082(3) Uani 1 1 d . B . O21 O 0.4023(5) -0.2543(11) 0.2605(3) 0.120(3) Uani 1 1 d . . . O23 O 0.3696(5) -0.7097(10) 0.0867(4) 0.110(2) Uani 1 1 d . . . C21 C 0.5095(15) -0.546(3) 0.1538(6) 0.117(5) Uani 1 1 d . B . O22 O 0.5646(8) -0.695(2) 0.1399(4) 0.166(4) Uani 1 1 d . . . C22 C 0.5307(10) -0.332(2) 0.1848(6) 0.128(5) Uani 1 1 d . . . H22A H 0.5696 -0.2465 0.1544 0.153 Uiso 1 1 calc R B . H22B H 0.5658 -0.3445 0.2317 0.153 Uiso 1 1 calc R . . C23 C 0.4282(10) -0.2308(18) 0.1899(5) 0.105(4) Uani 1 1 d . B . H23 H 0.4293 -0.0774 0.1769 0.126 Uiso 1 1 calc R . . C24 C 0.3608(7) -0.3524(18) 0.1378(4) 0.082(3) Uani 1 1 d . . . H24 H 0.2964 -0.3704 0.1566 0.099 Uiso 1 1 calc R B . C25 C 0.3486(6) -0.2703(16) 0.0626(5) 0.090(3) Uani 1 1 d . B . H25 H 0.3303 -0.1272 0.0540 0.108 Uiso 1 1 calc R . . C26 C 0.3635(7) -0.3974(19) 0.0089(5) 0.090(3) Uani 1 1 d . . . H26 H 0.3607 -0.3374 -0.0366 0.108 Uiso 1 1 calc R B . C27 C 0.3840(8) -0.625(2) 0.0163(5) 0.106(3) Uani 1 1 d . B . H27A H 0.4515 -0.6504 0.0061 0.127 Uiso 1 1 calc R . . H27B H 0.3417 -0.7028 -0.0188 0.127 Uiso 1 1 calc R . . Si21 Si 0.3684(7) -0.0267(15) 0.3019(4) 0.102(3) Uani 0.50 1 d P B 1 C211 C 0.2529(8) 0.077(2) 0.2468(5) 0.139(4) Uiso 0.50 1 d P B 1 H21A H 0.2682 0.1050 0.1987 0.208 Uiso 0.50 1 calc PR B 1 H21B H 0.2309 0.2089 0.2677 0.208 Uiso 0.50 1 calc PR B 1 H21C H 0.2018 -0.0295 0.2467 0.208 Uiso 0.50 1 calc PR B 1 C212 C 0.4603(18) 0.177(4) 0.3177(11) 0.106(8) Uiso 0.50 1 d P B 1 H21D H 0.4834 0.1771 0.3674 0.159 Uiso 0.50 1 calc PR B 1 H21E H 0.4328 0.3157 0.3048 0.159 Uiso 0.50 1 calc PR B 1 H21F H 0.5142 0.1470 0.2895 0.159 Uiso 0.50 1 calc PR B 1 C213 C 0.317(2) -0.130(5) 0.3825(11) 0.120(8) Uiso 0.50 1 d P B 1 C214 C 0.4082(19) -0.250(4) 0.4285(11) 0.129(9) Uiso 0.50 1 d P B 1 H21G H 0.4280 -0.1658 0.4700 0.193 Uiso 0.50 1 calc PR B 1 H21H H 0.4626 -0.2647 0.3995 0.193 Uiso 0.50 1 calc PR B 1 H21I H 0.3877 -0.3913 0.4429 0.193 Uiso 0.50 1 calc PR B 1 C215 C 0.2692(16) 0.046(4) 0.4240(10) 0.109(7) Uiso 0.50 1 d P B 1 H21J H 0.1991 0.0397 0.4141 0.163 Uiso 0.50 1 calc PR B 1 H21K H 0.2927 0.1847 0.4099 0.163 Uiso 0.50 1 calc PR B 1 H21L H 0.2857 0.0252 0.4742 0.163 Uiso 0.50 1 calc PR B 1 C216 C 0.2366(19) -0.305(4) 0.3688(13) 0.123(10) Uiso 0.50 1 d P B 1 H21M H 0.1976 -0.3130 0.4089 0.185 Uiso 0.50 1 calc PR B 1 H21N H 0.2672 -0.4431 0.3622 0.185 Uiso 0.50 1 calc PR B 1 H21O H 0.1953 -0.2690 0.3267 0.185 Uiso 0.50 1 calc PR B 1 Si22 Si 0.3147(7) -0.1347(13) 0.3063(3) 0.095(3) Uani 0.50 1 d P B 2 C221 C 0.2529(8) 0.077(2) 0.2468(5) 0.139(4) Uiso 0.50 1 d P B 2 H22C H 0.2399 0.2029 0.2747 0.208 Uiso 0.50 1 calc PR B 2 H22D H 0.1921 0.0214 0.2249 0.208 Uiso 0.50 1 calc PR B 2 H22E H 0.2951 0.1167 0.2105 0.208 Uiso 0.50 1 calc PR B 2 C222 C 0.2261(19) -0.334(4) 0.3353(13) 0.134(10) Uiso 0.50 1 d P B 2 H22F H 0.2610 -0.4513 0.3594 0.200 Uiso 0.50 1 calc PR B 2 H22G H 0.1871 -0.3889 0.2943 0.200 Uiso 0.50 1 calc PR B 2 H22H H 0.1841 -0.2662 0.3672 0.200 Uiso 0.50 1 calc PR B 2 C223 C 0.3891(18) -0.028(4) 0.3806(10) 0.100(6) Uiso 0.50 1 d P B 2 C224 C 0.461(2) 0.168(5) 0.3534(12) 0.129(9) Uiso 0.50 1 d P B 2 H22I H 0.5153 0.1901 0.3886 0.193 Uiso 0.50 1 calc PR B 2 H22J H 0.4240 0.2989 0.3468 0.193 Uiso 0.50 1 calc PR B 2 H22K H 0.4858 0.1262 0.3089 0.193 Uiso 0.50 1 calc PR B 2 C225 C 0.3332(17) 0.103(4) 0.4361(9) 0.105(7) Uiso 0.50 1 d P B 2 H22L H 0.3168 0.0090 0.4739 0.158 Uiso 0.50 1 calc PR B 2 H22M H 0.2741 0.1634 0.4128 0.158 Uiso 0.50 1 calc PR B 2 H22N H 0.3745 0.2184 0.4556 0.158 Uiso 0.50 1 calc PR B 2 C226 C 0.4595(18) -0.169(5) 0.4234(12) 0.138(10) Uiso 0.50 1 d P B 2 H22O H 0.4955 -0.2547 0.3919 0.207 Uiso 0.50 1 calc PR B 2 H22P H 0.4241 -0.2617 0.4531 0.207 Uiso 0.50 1 calc PR B 2 H22Q H 0.5045 -0.0805 0.4528 0.207 Uiso 0.50 1 calc PR B 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 N1 0.111(11) 0.095(8) 0.112(7) 0.019(6) 0.043(7) -0.001(8) O11 0.169(7) 0.123(6) 0.079(4) 0.004(4) 0.022(4) -0.045(5) O12 0.152(8) 0.298(11) 0.194(8) 0.133(9) 0.038(6) 0.052(8) O13 0.177(9) 0.103(6) 0.155(7) 0.008(6) 0.060(6) 0.001(6) C11 0.087(15) 0.26(2) 0.104(10) 0.071(12) 0.023(9) 0.029(14) C12 0.071(11) 0.208(16) 0.097(8) 0.000(9) 0.007(7) -0.008(10) C13 0.098(11) 0.099(8) 0.092(7) -0.004(6) -0.002(7) -0.023(8) C14 0.089(12) 0.099(9) 0.082(6) 0.003(6) -0.020(7) -0.003(9) C15 0.059(11) 0.106(8) 0.137(9) -0.002(8) -0.005(8) 0.024(7) C16 0.082(10) 0.153(12) 0.108(9) -0.004(8) 0.022(7) -0.012(9) C17 0.127(12) 0.144(11) 0.100(8) 0.017(8) 0.020(7) -0.006(9) Si11 0.075(7) 0.062(4) 0.085(4) -0.005(4) 0.002(4) 0.014(4) Si12 0.110(9) 0.116(7) 0.100(5) 0.013(5) 0.001(5) -0.010(6) N2 0.096(10) 0.061(6) 0.089(5) -0.004(4) -0.003(6) 0.012(6) O21 0.163(7) 0.115(6) 0.084(4) -0.024(4) 0.023(4) 0.044(5) O23 0.155(7) 0.077(4) 0.094(4) -0.007(4) -0.009(4) -0.006(4) C21 0.101(18) 0.168(16) 0.079(7) -0.006(8) -0.018(8) 0.042(13) O22 0.134(10) 0.226(11) 0.135(6) -0.048(7) -0.006(5) 0.093(8) C22 0.102(13) 0.167(12) 0.111(8) -0.038(9) -0.010(7) -0.017(10) C23 0.124(13) 0.098(8) 0.090(7) -0.008(7) 0.003(8) 0.010(9) C24 0.071(9) 0.103(9) 0.072(6) -0.010(6) 0.007(5) 0.004(7) C25 0.069(9) 0.094(7) 0.107(7) 0.018(6) 0.009(6) 0.002(6) C26 0.076(9) 0.113(9) 0.081(6) 0.007(6) 0.010(5) -0.018(7) C27 0.088(9) 0.130(10) 0.099(7) -0.018(7) 0.005(6) -0.007(7) Si21 0.077(8) 0.104(6) 0.125(5) -0.030(5) 0.016(4) -0.016(5) Si22 0.099(9) 0.095(6) 0.087(4) -0.006(4) -0.018(4) -0.011(5) _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 N1 C11 1.379(15) . ? N1 O13 1.401(11) . ? N1 C14 1.437(13) . ? O11 C13 1.386(10) . ? O11 Si11 1.678(10) . ? O11 Si12 1.741(11) . ? O12 C11 1.215(15) . ? O13 C17 1.437(12) . ? C11 C12 1.427(19) . ? C12 C13 1.515(14) . ? C13 C14 1.512(12) . ? C14 C15 1.495(13) . ? C15 C16 1.294(13) . ? C16 C17 1.467(15) . ? Si11 C112 1.78(3) . ? Si11 C113 1.91(2) . ? Si11 C111 2.08(2) . ? C113 C114 1.39(4) . ? C113 C115 1.53(3) . ? C113 C116 1.55(3) . ? Si12 C123 1.70(3) . ? Si12 C121 1.84(2) . ? Si12 C122 1.98(3) . ? C123 C124 1.52(3) . ? C123 C125 1.55(4) . ? C123 C126 1.76(4) . ? N2 C21 1.352(15) . ? N2 O23 1.409(10) . ? N2 C24 1.456(12) . ? O21 C23 1.408(10) . ? O21 Si21 1.690(11) . ? O21 Si22 1.699(11) . ? O23 C27 1.451(10) . ? C21 O22 1.230(14) . ? C21 C22 1.464(18) . ? C22 C23 1.543(14) . ? C23 C24 1.489(13) . ? C24 C25 1.498(11) . ? C25 C26 1.308(11) . ? C26 C27 1.435(12) . ? Si21 C212 1.78(3) . ? Si21 C213 1.84(3) . ? Si21 C211 1.923(15) . ? C213 C215 1.52(3) . ? C213 C216 1.54(3) . ? C213 C214 1.64(3) . ? Si22 C223 1.79(2) . ? Si22 C222 1.84(3) . ? C223 C226 1.48(3) . ? C223 C225 1.57(3) . ? C223 C224 1.66(3) . ? 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 C11 N1 O13 121.1(13) . . ? C11 N1 C14 111.9(13) . . ? O13 N1 C14 115.1(12) . . ? C13 O11 Si11 136.5(7) . . ? C13 O11 Si12 112.2(8) . . ? Si11 O11 Si12 32.7(3) . . ? N1 O13 C17 109.2(8) . . ? O12 C11 N1 122(2) . . ? O12 C11 C12 131(2) . . ? N1 C11 C12 107.3(14) . . ? C11 C12 C13 106.9(12) . . ? O11 C13 C14 109.8(9) . . ? O11 C13 C12 110.4(9) . . ? C14 C13 C12 103.6(10) . . ? N1 C14 C15 108.1(9) . . ? N1 C14 C13 101.4(10) . . ? C15 C14 C13 118.4(10) . . ? C16 C15 C14 121.7(10) . . ? C15 C16 C17 123.3(11) . . ? O13 C17 C16 111.4(9) . . ? O11 Si11 C112 116.3(9) . . ? O11 Si11 C113 99.8(8) . . ? C112 Si11 C113 116.0(11) . . ? O11 Si11 C111 99.3(7) . . ? C112 Si11 C111 119.3(12) . . ? C113 Si11 C111 103.0(9) . . ? C114 C113 C115 98(2) . . ? C114 C113 C116 114(2) . . ? C115 C113 C116 110.0(18) . . ? C114 C113 Si11 116(2) . . ? C115 C113 Si11 111.0(16) . . ? C116 C113 Si11 108.4(17) . . ? C123 Si12 O11 98.6(14) . . ? C123 Si12 C121 102.3(15) . . ? O11 Si12 C121 109.8(9) . . ? C123 Si12 C122 106.0(16) . . ? O11 Si12 C122 117.7(9) . . ? C121 Si12 C122 118.9(13) . . ? C124 C123 C125 107(3) . . ? C124 C123 Si12 121(3) . . ? C125 C123 Si12 112(2) . . ? C124 C123 C126 102(2) . . ? C125 C123 C126 108(2) . . ? Si12 C123 C126 106(2) . . ? C21 N2 O23 122.4(10) . . ? C21 N2 C24 113.8(10) . . ? O23 N2 C24 114.9(9) . . ? C23 O21 Si21 116.5(7) . . ? C23 O21 Si22 132.3(7) . . ? Si21 O21 Si22 34.3(3) . . ? N2 O23 C27 107.0(6) . . ? O22 C21 N2 120.9(16) . . ? O22 C21 C22 131.1(19) . . ? N2 C21 C22 108.0(14) . . ? C21 C22 C23 104.0(12) . . ? O21 C23 C24 112.2(10) . . ? O21 C23 C22 108.4(9) . . ? C24 C23 C22 105.6(9) . . ? N2 C24 C23 100.6(8) . . ? N2 C24 C25 107.5(8) . . ? C23 C24 C25 117.6(9) . . ? C26 C25 C24 120.8(9) . . ? C25 C26 C27 123.7(9) . . ? C26 C27 O23 113.8(8) . . ? O21 Si21 C212 116.6(9) . . ? O21 Si21 C213 103.1(9) . . ? C212 Si21 C213 114.8(11) . . ? O21 Si21 C211 106.0(6) . . ? C212 Si21 C211 112.8(11) . . ? C213 Si21 C211 102.0(10) . . ? C215 C213 C216 105(2) . . ? C215 C213 C214 113.2(18) . . ? C216 C213 C214 106(2) . . ? C215 C213 Si21 112.5(17) . . ? C216 C213 Si21 114.9(17) . . ? C214 C213 Si21 105.4(18) . . ? O21 Si22 C223 100.3(9) . . ? O21 Si22 C222 111.4(10) . . ? C223 Si22 C222 111.2(11) . . ? C226 C223 C225 105.8(18) . . ? C226 C223 C224 103(2) . . ? C225 C223 C224 99.3(18) . . ? C226 C223 Si22 120.5(19) . . ? C225 C223 Si22 115.8(18) . . ? C224 C223 Si22 109.9(15) . . ? _diffrn_measured_fraction_theta_max 0.693 _diffrn_reflns_theta_full 57.09 _diffrn_measured_fraction_theta_full 0.693 _refine_diff_density_max 0.262 _refine_diff_density_min -0.164 _refine_diff_density_rms 0.032 #===END #Compound 42 data_VS060299 _database_code_CSD 163575 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H25 N O4 Si' _chemical_formula_weight 287.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 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' _cell_length_a 14.546(1) _cell_length_b 6.262(1) _cell_length_c 35.155(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.72(1) _cell_angle_gamma 90.00 _cell_volume 3165.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 92 _cell_measurement_theta_min 5.093 _cell_measurement_theta_max 24.734 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 1.401 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.7821 _exptl_absorpt_correction_T_max 0.9452 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3443 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 67.55 _reflns_number_total 3006 _reflns_number_gt 2866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS V2.20' _computing_cell_refinement 'XSCANS V2.20' _computing_data_reduction 'XSCANS V2.20' _computing_structure_solution 'SHELXS-90' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for windows' _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^)+(0.0971P)^2^+1.7325P] 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 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 3006 _refine_ls_number_parameters 346 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Si1 Si 0.10644(12) -0.60112(16) 0.16216(3) 0.0473(6) Uani 1 1 d . . . N11 N 0.0647(4) -0.2027(4) 0.04879(9) 0.0329(19) Uani 1 1 d . . . O12 O -0.0580(3) 0.0057(5) 0.05981(8) 0.0462(12) Uani 1 1 d . . . O14 O 0.0800(2) -0.4416(4) 0.12471(6) 0.0391(11) Uani 1 1 d . . . O16 O 0.2586(3) -0.5575(4) 0.06528(7) 0.0415(12) Uani 1 1 d . . . H16A H 0.3122 -0.5223 0.0637 0.047(3) Uiso 1 1 calc R . . O17 O 0.2272(3) -0.2853(4) 0.00464(7) 0.0496(11) Uani 1 1 d . . . H17A H 0.2296 -0.1911 -0.0114 0.047(3) Uiso 1 1 calc R . . C12 C -0.0145(5) -0.1673(6) 0.06101(11) 0.035(2) Uani 1 1 d . . . C13 C -0.0481(4) -0.3798(6) 0.07483(12) 0.0406(19) Uani 1 1 d . . . H13A H -0.0817 -0.3600 0.0964 0.047(3) Uiso 1 1 calc R . . H13B H -0.0878 -0.4534 0.0543 0.047(3) Uiso 1 1 calc R . . C14 C 0.0417(4) -0.5004(5) 0.08682(9) 0.0297(16) Uani 1 1 d . . . H14A H 0.0322 -0.6551 0.0845 0.047(3) Uiso 1 1 calc R . . C15 C 0.1018(5) -0.4178(5) 0.05773(9) 0.0259(19) Uani 1 1 d . . . H15A H 0.0915 -0.5062 0.0345 0.047(3) Uiso 1 1 calc R . . C16 C 0.2041(5) -0.3723(5) 0.06834(10) 0.028(2) Uani 1 1 d . . . H16B H 0.2161 -0.3195 0.0949 0.047(3) Uiso 1 1 calc R . . C17 C 0.2207(4) -0.1910(6) 0.04094(10) 0.0325(19) Uani 1 1 d . . . H17B H 0.2772 -0.1112 0.0508 0.047(3) Uiso 1 1 calc R . . C18 C 0.1341(4) -0.0506(6) 0.03964(10) 0.0321(17) Uani 1 1 d . . . H18A H 0.1441 0.0629 0.0586 0.047(3) Uiso 1 1 calc R . . H18B H 0.1161 0.0112 0.0143 0.047(3) Uiso 1 1 calc R . . C19 C 0.1852(6) -0.4383(11) 0.19718(15) 0.099(3) Uani 1 1 d . . . H19A H 0.1519 -0.3171 0.2048 0.146(6) Uiso 1 1 calc R . . H19B H 0.2369 -0.3902 0.1855 0.146(6) Uiso 1 1 calc R . . H19C H 0.2074 -0.5234 0.2194 0.146(6) Uiso 1 1 calc R . . C110 C 0.1701(6) -0.8414(9) 0.14765(15) 0.093(3) Uani 1 1 d . . . H11A H 0.1289 -0.9251 0.1296 0.146(6) Uiso 1 1 calc R . . H11B H 0.1916 -0.9260 0.1700 0.146(6) Uiso 1 1 calc R . . H11C H 0.2223 -0.7959 0.1360 0.146(6) Uiso 1 1 calc R . . C111 C -0.0011(5) -0.6824(9) 0.18168(12) 0.064(2) Uani 1 1 d . . . C112 C -0.0650(6) -0.8107(14) 0.15268(16) 0.127(4) Uani 1 1 d . . . H11D H -0.1193 -0.8505 0.1634 0.146(6) Uiso 1 1 calc R . . H11E H -0.0334 -0.9369 0.1461 0.146(6) Uiso 1 1 calc R . . H11F H -0.0830 -0.7264 0.1300 0.146(6) Uiso 1 1 calc R . . C113 C 0.0268(6) -0.8169(12) 0.21824(16) 0.125(3) Uani 1 1 d . . . H11G H -0.0280 -0.8580 0.2286 0.146(6) Uiso 1 1 calc R . . H11H H 0.0666 -0.7342 0.2370 0.146(6) Uiso 1 1 calc R . . H11I H 0.0593 -0.9425 0.2120 0.146(6) Uiso 1 1 calc R . . C114 C -0.0538(7) -0.4807(13) 0.1921(2) 0.114(3) Uani 1 1 d . . . H11J H -0.1085 -0.5229 0.2025 0.146(6) Uiso 1 1 calc R . . H11K H -0.0715 -0.3960 0.1694 0.146(6) Uiso 1 1 calc R . . H11L H -0.0141 -0.3983 0.2109 0.146(6) Uiso 1 1 calc R . . Si2 Si 0.40070(13) -0.83672(16) 0.33290(3) 0.0525(7) Uani 1 1 d . . . O22 O 0.5550(3) -0.2477(5) 0.43565(9) 0.0509(13) Uani 1 1 d . . . O24 O 0.4060(3) -0.6994(4) 0.37297(7) 0.0440(11) Uani 1 1 d . . . O27 O 0.2403(3) -0.8066(4) 0.43548(6) 0.0437(12) Uani 1 1 d . . . H27A H 0.1860 -0.7712 0.4354 0.047(3) Uiso 1 1 calc R . . O28 O 0.2781(3) -0.5390(4) 0.49703(7) 0.0487(12) Uani 1 1 d . . . H28A H 0.2739 -0.4458 0.5131 0.047(3) Uiso 1 1 calc R . . N21 N 0.4369(4) -0.4576(5) 0.44974(8) 0.0313(16) Uani 1 1 d . . . C22 C 0.5127(5) -0.4220(6) 0.43527(11) 0.0355(19) Uani 1 1 d . . . C23 C 0.5436(4) -0.6334(6) 0.41919(12) 0.0489(19) Uani 1 1 d . . . H23A H 0.5716 -0.6106 0.3962 0.047(3) Uiso 1 1 calc R . . H23B H 0.5873 -0.7085 0.4381 0.047(3) Uiso 1 1 calc R . . C24 C 0.4521(4) -0.7541(6) 0.41018(9) 0.0351(16) Uani 1 1 d . . . H24A H 0.4621 -0.9086 0.4125 0.047(3) Uiso 1 1 calc R . . C25 C 0.3980(5) -0.6718(5) 0.44122(10) 0.030(2) Uani 1 1 d . . . H25A H 0.4105 -0.7622 0.4642 0.047(3) Uiso 1 1 calc R . . C26 C 0.2952(5) -0.6223(6) 0.43239(9) 0.031(2) Uani 1 1 d . . . H26A H 0.2812 -0.5662 0.4061 0.047(3) Uiso 1 1 calc R . . C27 C 0.2815(4) -0.4436(6) 0.46091(9) 0.0372(18) Uani 1 1 d . . . H27B H 0.2251 -0.3606 0.4521 0.047(3) Uiso 1 1 calc R . . C28 C 0.3698(4) -0.3071(6) 0.46145(9) 0.0355(16) Uani 1 1 d . . . H28B H 0.3588 -0.1890 0.4435 0.047(3) Uiso 1 1 calc R . . H28C H 0.3911 -0.2513 0.4870 0.047(3) Uiso 1 1 calc R . . C29 C 0.4149(7) -0.6336(10) 0.29433(15) 0.123(4) Uani 1 1 d . . . H29A H 0.4748 -0.5667 0.3002 0.146(6) Uiso 1 1 calc R . . H29B H 0.3671 -0.5272 0.2934 0.146(6) Uiso 1 1 calc R . . H29C H 0.4100 -0.7038 0.2698 0.146(6) Uiso 1 1 calc R . . C210 C 0.4991(6) -1.0298(11) 0.33643(18) 0.095(3) Uani 1 1 d . . . H21A H 0.4923 -1.1352 0.3556 0.146(6) Uiso 1 1 calc R . . H21B H 0.5568 -0.9551 0.3435 0.146(6) Uiso 1 1 calc R . . H21C H 0.4989 -1.0987 0.3120 0.146(6) Uiso 1 1 calc R . . C211 C 0.2859(5) -0.9673(8) 0.32136(12) 0.070(2) Uani 1 1 d . . . C212 C 0.2787(6) -1.1425(10) 0.35160(16) 0.102(3) Uani 1 1 d . . . H21D H 0.2192 -1.2111 0.3461 0.146(6) Uiso 1 1 calc R . . H21E H 0.2855 -1.0793 0.3767 0.146(6) Uiso 1 1 calc R . . H21F H 0.3270 -1.2461 0.3507 0.146(6) Uiso 1 1 calc R . . C213 C 0.2752(6) -1.0685(10) 0.28084(14) 0.097(3) Uani 1 1 d . . . H21G H 0.2152 -1.1352 0.2751 0.146(6) Uiso 1 1 calc R . . H21H H 0.3229 -1.1737 0.2801 0.146(6) Uiso 1 1 calc R . . H21I H 0.2807 -0.9596 0.2621 0.146(6) Uiso 1 1 calc R . . C214 C 0.2084(6) -0.8074(12) 0.32184(17) 0.120(3) Uani 1 1 d . . . H21J H 0.1495 -0.8785 0.3159 0.146(6) Uiso 1 1 calc R . . H21K H 0.2130 -0.6983 0.3030 0.146(6) Uiso 1 1 calc R . . H21L H 0.2133 -0.7437 0.3469 0.146(6) 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 Si1 0.0583(19) 0.0411(6) 0.0417(4) 0.0061(4) 0.0054(6) 0.0025(7) N11 0.031(7) 0.0225(14) 0.0459(16) 0.0033(11) 0.008(2) 0.001(2) O12 0.034(4) 0.0434(17) 0.0615(14) 0.0006(12) 0.0083(16) 0.0104(18) O14 0.043(4) 0.0374(13) 0.0382(11) 0.0040(10) 0.0093(13) 0.0007(15) O16 0.033(4) 0.0338(14) 0.0608(14) 0.0067(11) 0.0155(16) 0.0116(16) O17 0.061(4) 0.0451(14) 0.0480(12) 0.0043(11) 0.0253(15) 0.0090(19) C12 0.027(7) 0.033(2) 0.0431(17) -0.0013(14) 0.004(2) 0.004(3) C13 0.018(6) 0.044(2) 0.061(2) 0.0066(17) 0.008(2) -0.009(3) C14 0.018(5) 0.0260(17) 0.0451(16) 0.0016(13) 0.0049(19) -0.003(2) C15 0.013(7) 0.0253(17) 0.0387(15) 0.0028(13) 0.002(2) 0.005(2) C16 0.013(7) 0.0307(18) 0.0401(15) 0.0055(13) 0.009(2) 0.012(2) C17 0.020(6) 0.0312(18) 0.0478(17) -0.0019(14) 0.008(2) -0.012(2) C18 0.025(6) 0.0287(18) 0.0450(16) 0.0004(13) 0.014(2) -0.001(2) C19 0.121(9) 0.095(4) 0.069(3) 0.001(3) -0.021(4) -0.033(5) C110 0.135(10) 0.065(3) 0.083(3) 0.017(3) 0.021(4) 0.031(4) C111 0.063(7) 0.076(3) 0.057(2) 0.010(2) 0.021(3) -0.016(4) C112 0.154(11) 0.147(6) 0.079(3) 0.005(4) 0.022(4) -0.074(7) C113 0.175(10) 0.118(5) 0.086(4) 0.045(4) 0.029(4) -0.022(6) C114 0.121(11) 0.113(5) 0.123(5) -0.007(4) 0.072(5) 0.004(6) Si2 0.072(2) 0.0404(6) 0.0467(5) -0.0088(5) 0.0144(7) 0.0047(7) O22 0.039(4) 0.0426(17) 0.0716(17) -0.0003(13) 0.0103(18) -0.0123(18) O24 0.046(4) 0.0410(14) 0.0445(12) -0.0066(10) 0.0044(14) 0.0067(16) O27 0.046(4) 0.0337(14) 0.0538(12) -0.0055(11) 0.0160(15) -0.0112(17) O28 0.064(4) 0.0413(14) 0.0453(12) -0.0062(10) 0.0241(15) -0.0088(18) N21 0.025(6) 0.0244(14) 0.0455(15) -0.0017(12) 0.009(2) 0.002(2) C22 0.029(7) 0.033(2) 0.0437(18) 0.0004(14) 0.003(2) 0.002(3) C23 0.044(7) 0.039(2) 0.063(2) -0.0077(18) 0.008(3) 0.005(3) C24 0.035(6) 0.0236(17) 0.0488(18) 0.0001(13) 0.012(2) 0.005(2) C25 0.020(7) 0.0254(18) 0.0422(16) -0.0013(13) 0.000(2) -0.005(2) C26 0.028(7) 0.0272(17) 0.0405(15) -0.0042(14) 0.009(2) -0.008(3) C27 0.040(6) 0.0304(18) 0.0422(16) -0.0010(14) 0.009(2) 0.000(2) C28 0.033(6) 0.0302(19) 0.0442(16) -0.0031(14) 0.007(2) 0.006(2) C29 0.234(12) 0.073(3) 0.073(3) 0.000(3) 0.055(4) -0.023(5) C210 0.088(8) 0.098(4) 0.102(4) -0.046(3) 0.024(4) 0.032(5) C211 0.089(7) 0.054(3) 0.063(2) -0.022(2) 0.002(3) 0.003(3) C212 0.136(10) 0.083(4) 0.093(4) -0.013(3) 0.042(4) -0.037(5) C213 0.109(8) 0.099(4) 0.075(3) -0.041(3) -0.007(3) 0.008(4) C214 0.132(10) 0.120(6) 0.101(4) -0.052(4) -0.012(5) 0.031(6) _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 Si1 O14 1.651(2) . ? Si1 C19 1.854(6) . ? Si1 C111 1.871(6) . ? Si1 C110 1.877(6) . ? N11 C12 1.307(7) . ? N11 C18 1.459(6) . ? N11 C15 1.468(5) . ? O12 C12 1.252(6) . ? O14 C14 1.413(4) . ? O16 C16 1.418(5) . ? O17 C17 1.422(4) . ? C12 C13 1.522(6) . ? C13 C14 1.511(7) . ? C14 C15 1.533(6) . ? C15 C16 1.505(7) . ? C16 C17 1.531(5) . ? C17 C18 1.531(7) . ? C111 C112 1.504(8) . ? C111 C113 1.539(7) . ? C111 C114 1.550(10) . ? Si2 O24 1.642(2) . ? Si2 C211 1.848(7) . ? Si2 C210 1.864(7) . ? Si2 C29 1.893(5) . ? O22 C22 1.252(6) . ? O24 C24 1.418(4) . ? O27 C26 1.417(5) . ? O28 C27 1.411(4) . ? N21 C22 1.303(7) . ? N21 C28 1.460(6) . ? N21 C25 1.469(5) . ? C22 C23 1.533(6) . ? C23 C24 1.522(7) . ? C24 C25 1.529(6) . ? C25 C26 1.512(7) . ? C26 C27 1.536(5) . ? C27 C28 1.541(7) . ? C211 C214 1.510(9) . ? C211 C212 1.542(7) . ? C211 C213 1.546(6) . ? 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 O14 Si1 C19 104.0(2) . . ? O14 Si1 C111 110.5(2) . . ? C19 Si1 C111 111.9(3) . . ? O14 Si1 C110 109.44(18) . . ? C19 Si1 C110 109.9(4) . . ? C111 Si1 C110 110.8(3) . . ? C12 N11 C18 129.4(3) . . ? C12 N11 C15 113.6(4) . . ? C18 N11 C15 113.7(5) . . ? C14 O14 Si1 127.2(2) . . ? O12 C12 N11 127.0(4) . . ? O12 C12 C13 125.6(6) . . ? N11 C12 C13 107.3(4) . . ? C14 C13 C12 102.7(5) . . ? O14 C14 C13 109.5(3) . . ? O14 C14 C15 110.9(4) . . ? C13 C14 C15 101.6(3) . . ? N11 C15 C16 101.4(4) . . ? N11 C15 C14 102.9(4) . . ? C16 C15 C14 122.8(3) . . ? O16 C16 C15 111.7(4) . . ? O16 C16 C17 114.6(4) . . ? C15 C16 C17 103.2(4) . . ? O17 C17 C18 112.2(4) . . ? O17 C17 C16 107.1(3) . . ? C18 C17 C16 103.7(4) . . ? N11 C18 C17 102.3(3) . . ? C112 C111 C113 109.4(5) . . ? C112 C111 C114 108.6(7) . . ? C113 C111 C114 109.0(5) . . ? C112 C111 Si1 111.2(4) . . ? C113 C111 Si1 109.0(5) . . ? C114 C111 Si1 109.7(4) . . ? O24 Si2 C211 110.1(2) . . ? O24 Si2 C210 110.3(2) . . ? C211 Si2 C210 112.8(3) . . ? O24 Si2 C29 105.4(2) . . ? C211 Si2 C29 109.5(3) . . ? C210 Si2 C29 108.5(4) . . ? C24 O24 Si2 128.2(2) . . ? C22 N21 C28 129.9(3) . . ? C22 N21 C25 113.6(4) . . ? C28 N21 C25 113.2(5) . . ? O22 C22 N21 126.1(4) . . ? O22 C22 C23 125.9(6) . . ? N21 C22 C23 108.0(4) . . ? C24 C23 C22 102.1(5) . . ? O24 C24 C23 110.4(3) . . ? O24 C24 C25 110.8(4) . . ? C23 C24 C25 102.3(3) . . ? N21 C25 C26 101.1(4) . . ? N21 C25 C24 103.3(4) . . ? C26 C25 C24 121.5(4) . . ? O27 C26 C25 111.6(4) . . ? O27 C26 C27 114.4(4) . . ? C25 C26 C27 103.8(4) . . ? O28 C27 C26 107.7(3) . . ? O28 C27 C28 111.5(3) . . ? C26 C27 C28 102.8(4) . . ? N21 C28 C27 103.3(3) . . ? C214 C211 C212 109.6(6) . . ? C214 C211 C213 108.1(5) . . ? C212 C211 C213 109.6(4) . . ? C214 C211 Si2 110.8(4) . . ? C212 C211 Si2 108.5(4) . . ? C213 C211 Si2 110.2(5) . . ? _diffrn_measured_fraction_theta_max 0.553 _diffrn_reflns_theta_full 67.55 _diffrn_measured_fraction_theta_full 0.553 _refine_diff_density_max 0.276 _refine_diff_density_min -0.180 _refine_diff_density_rms 0.055 #===END Compound 44 data_pb092599 _database_code_CSD 163576 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H24 B N O4' _chemical_formula_weight 293.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 2(1) 2(1) 2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.480(1) _cell_length_b 9.322(2) _cell_length_c 20.143(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1592.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 65 _cell_measurement_theta_min 7.252 _cell_measurement_theta_max 26.485 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.7665 _exptl_absorpt_correction_T_max 0.9331 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3209 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 67.80 _reflns_number_total 2654 _reflns_number_gt 2320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS V2.20' _computing_cell_refinement 'XSCANS V2.20' _computing_data_reduction 'XSCANS V2.20' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for windows' _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^)+(0.0357P)^2^+0.3230P] 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 SHELXL _refine_ls_extinction_coef 0.0010(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(3) _refine_ls_number_reflns 2654 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 O17 O 0.47451(17) 0.83736(17) 0.26495(8) 0.0472(4) Uani 1 1 d . . . H17O H 0.412(4) 0.761(3) 0.2559(14) 0.082(9) Uiso 1 1 d . . . O16 O 0.6582(2) 0.60881(17) 0.22319(8) 0.0509(4) Uani 1 1 d . . . H16O H 0.619(4) 0.529(4) 0.2394(16) 0.093(11) Uiso 1 1 d . . . O12 O 0.79266(19) 0.76576(16) 0.41749(7) 0.0490(4) Uani 1 1 d . . . N N 0.82015(18) 0.94215(17) 0.28329(8) 0.0367(4) Uani 1 1 d . . . C11 C 0.6846(2) 0.9202(2) 0.33314(9) 0.0364(4) Uani 1 1 d . . . H11 H 0.6116(18) 1.007(2) 0.33161(10) 0.0592(17) Uiso 1 1 calc R . . C12 C 0.7621(3) 0.9120(2) 0.40165(10) 0.0446(5) Uani 1 1 d . . . H12 H 0.6978(19) 0.9554(13) 0.4343(9) 0.0592(17) Uiso 1 1 calc R . . C13 C 0.9136(3) 0.9967(3) 0.39159(12) 0.0538(6) Uani 1 1 d . . . H13A H 0.8929(4) 1.1016(19) 0.39080(12) 0.0592(17) Uiso 1 1 calc R . . H13B H 0.9919(14) 0.9751(4) 0.4269(6) 0.0592(17) Uiso 1 1 calc R . . C14 C 0.9688(2) 0.9436(3) 0.32480(11) 0.0475(5) Uani 1 1 d . . . H14A H 1.0170(9) 0.8411(17) 0.32853(12) 0.0592(17) Uiso 1 1 calc R . . H14B H 1.0527(14) 1.0124(11) 0.3046(4) 0.0592(17) Uiso 1 1 calc R . . C15 C 0.8148(3) 0.8161(2) 0.23699(10) 0.0415(5) Uani 1 1 d . . . H15A H 0.9247(18) 0.7803(6) 0.2273(2) 0.0592(17) Uiso 1 1 calc R . . H15B H 0.7628(9) 0.8437(5) 0.1937(7) 0.0592(17) Uiso 1 1 calc R . . C16 C 0.7192(2) 0.7015(2) 0.27231(10) 0.0379(5) Uani 1 1 d . . . H16 H 0.7868(18) 0.6473(14) 0.3041(9) 0.0592(17) Uiso 1 1 calc R . . C17 C 0.5949(2) 0.7895(2) 0.30964(10) 0.0368(4) Uani 1 1 d . . . H17 H 0.5491(11) 0.7341(14) 0.3480(9) 0.0592(17) Uiso 1 1 calc R . . B B 0.8022(3) 1.0882(3) 0.24225(14) 0.0477(6) Uani 1 1 d . . . H18A H 0.9061(18) 1.0993(9) 0.2056(8) 0.078(3) Uiso 1 1 calc R . . H18B H 0.802(2) 1.1842(13) 0.2784(5) 0.078(3) Uiso 1 1 calc R . . H18C H 0.6851(19) 1.0865(8) 0.2131(8) 0.078(3) Uiso 1 1 calc R . . O22 O 1.0475(3) 0.1741(2) 0.52451(9) 0.0718(6) Uani 1 1 d . . . C21 C 0.8357(4) 0.7439(3) 0.48525(11) 0.0638(7) Uani 1 1 d . . . H21A H 0.7411(16) 0.7674(6) 0.5157(5) 0.0592(17) Uiso 1 1 calc R . . H21B H 0.9276(16) 0.8115(12) 0.4977(3) 0.0592(17) Uiso 1 1 calc R . . C22 C 0.8848(3) 0.5909(3) 0.49521(10) 0.0488(5) Uani 1 1 d . . . C23 C 0.9713(3) 0.5172(3) 0.44738(11) 0.0562(6) Uani 1 1 d . . . H23 H 0.9965(7) 0.5647(12) 0.4053(11) 0.0592(17) Uiso 1 1 calc R . . C24 C 1.0222(3) 0.3785(3) 0.45817(11) 0.0572(6) Uani 1 1 d . . . H24 H 1.0836(16) 0.3262(13) 0.4224(9) 0.0592(17) Uiso 1 1 calc R . . C25 C 0.9893(3) 0.3105(3) 0.51795(10) 0.0504(6) Uani 1 1 d . . . C26 C 0.9039(3) 0.3820(3) 0.56584(11) 0.0499(6) Uani 1 1 d . . . H26 H 0.8787(7) 0.3334(13) 0.6094(11) 0.0592(17) Uiso 1 1 calc R . . C27 C 0.8527(3) 0.5205(3) 0.55403(11) 0.0508(6) Uani 1 1 d . . . H27 H 0.7937(17) 0.5687(14) 0.5874(10) 0.0592(17) Uiso 1 1 calc R . . C28 C 1.0328(5) 0.1053(3) 0.58548(14) 0.0890(10) Uani 1 1 d . . . H28A H 1.0851(9) 0.1651(10) 0.6211(6) 0.078(3) Uiso 1 1 calc R . . H28B H 1.0853(9) 0.0080(15) 0.58318(14) 0.078(3) Uiso 1 1 calc R . . H28C H 0.9172(19) 0.0927(4) 0.5965(2) 0.078(3) 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 O17 0.0389(7) 0.0358(8) 0.0669(10) 0.0014(7) -0.0160(7) -0.0006(6) O16 0.0692(10) 0.0370(8) 0.0466(8) -0.0061(7) -0.0084(8) -0.0090(8) O12 0.0606(10) 0.0467(9) 0.0399(7) -0.0016(6) -0.0097(7) 0.0032(7) N 0.0308(7) 0.0318(9) 0.0475(9) -0.0037(7) 0.0020(7) -0.0029(7) C11 0.0320(9) 0.0340(11) 0.0433(10) -0.0037(8) 0.0009(8) 0.0005(8) C12 0.0466(11) 0.0442(13) 0.0431(10) -0.0087(10) -0.0033(9) 0.0049(10) C13 0.0487(12) 0.0499(13) 0.0629(14) -0.0113(11) -0.0129(11) -0.0043(11) C14 0.0318(9) 0.0488(13) 0.0620(13) -0.0034(11) -0.0055(9) -0.0021(9) C15 0.0433(10) 0.0356(11) 0.0457(11) -0.0070(9) 0.0045(9) 0.0008(9) C16 0.0421(10) 0.0297(11) 0.0417(10) -0.0028(8) -0.0054(9) -0.0004(8) C17 0.0336(9) 0.0325(11) 0.0442(10) 0.0025(9) -0.0046(8) -0.0007(8) B 0.0498(13) 0.0321(13) 0.0612(15) 0.0033(11) 0.0051(12) -0.0013(11) O22 0.1061(15) 0.0541(11) 0.0551(10) 0.0006(8) 0.0044(10) 0.0084(11) C21 0.0817(18) 0.0709(17) 0.0387(12) -0.0060(12) -0.0115(12) 0.0171(15) C22 0.0480(11) 0.0593(14) 0.0389(10) 0.0000(10) -0.0081(9) 0.0023(11) C23 0.0652(14) 0.0677(16) 0.0358(10) 0.0028(11) 0.0029(10) 0.0056(13) C24 0.0700(15) 0.0640(17) 0.0376(11) -0.0041(11) 0.0053(11) 0.0056(13) C25 0.0593(13) 0.0495(14) 0.0422(11) -0.0026(9) -0.0041(10) -0.0036(11) C26 0.0521(12) 0.0607(15) 0.0369(10) 0.0009(10) 0.0006(9) -0.0080(12) C27 0.0417(11) 0.0716(17) 0.0390(10) -0.0063(11) 0.0003(9) 0.0008(11) C28 0.136(3) 0.0662(18) 0.0647(17) 0.0160(14) 0.0111(19) 0.019(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 O17 C17 1.432(2) . ? O16 C16 1.412(2) . ? O12 C12 1.424(3) . ? O12 C21 1.428(3) . ? N C15 1.501(3) . ? N C14 1.513(2) . ? N C11 1.540(2) . ? N B 1.600(3) . ? C11 C17 1.513(3) . ? C11 C12 1.530(3) . ? C12 C13 1.521(3) . ? C13 C14 1.509(3) . ? C15 C16 1.518(3) . ? C16 C17 1.533(3) . ? O22 C25 1.370(3) . ? O22 C28 1.391(3) . ? C21 C22 1.499(4) . ? C22 C27 1.382(3) . ? C22 C23 1.392(3) . ? C23 C24 1.381(4) . ? C24 C25 1.389(3) . ? C25 C26 1.379(3) . ? C26 C27 1.382(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 C12 O12 C21 113.41(17) . . ? C15 N C14 112.06(16) . . ? C15 N C11 106.19(14) . . ? C14 N C11 105.25(14) . . ? C15 N B 110.00(16) . . ? C14 N B 110.95(17) . . ? C11 N B 112.25(15) . . ? C17 C11 C12 117.25(17) . . ? C17 C11 N 106.15(15) . . ? C12 C11 N 105.90(16) . . ? O12 C12 C13 111.90(18) . . ? O12 C12 C11 109.15(16) . . ? C13 C12 C11 102.51(17) . . ? C14 C13 C12 102.16(18) . . ? C13 C14 N 103.69(16) . . ? N C15 C16 106.01(16) . . ? O16 C16 C15 107.34(17) . . ? O16 C16 C17 114.77(16) . . ? C15 C16 C17 102.74(16) . . ? O17 C17 C11 107.69(16) . . ? O17 C17 C16 110.41(16) . . ? C11 C17 C16 103.82(15) . . ? C25 O22 C28 118.7(2) . . ? O12 C21 C22 109.5(2) . . ? C27 C22 C23 117.6(2) . . ? C27 C22 C21 120.8(2) . . ? C23 C22 C21 121.5(2) . . ? C24 C23 C22 121.2(2) . . ? C23 C24 C25 120.1(2) . . ? O22 C25 C26 124.8(2) . . ? O22 C25 C24 115.8(2) . . ? C26 C25 C24 119.4(2) . . ? C25 C26 C27 119.8(2) . . ? C22 C27 C26 122.0(2) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 67.80 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.127 _refine_diff_density_min -0.117 _refine_diff_density_rms 0.032 #===END Compound 55 data_pb030100 _database_code_CSD 163577 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 N2 O6 S2' _chemical_formula_weight 404.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 9.649(1) _cell_length_b 9.649(1) _cell_length_c 20.808(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1937.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 12.129 _cell_measurement_theta_max 36.348 _exptl_crystal_description 'Square prism' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 2.801 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.4004 _exptl_absorpt_correction_T_max 0.7671 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4372 _diffrn_reflns_av_R_equivalents 0.1081 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.58 _diffrn_reflns_theta_max 67.57 _reflns_number_total 1912 _reflns_number_gt 1762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III for windows' _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^)+(0.1283P)^2^+0.0893P] 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 SHELXL _refine_ls_extinction_coef 0.0062(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_number_reflns 1912 _refine_ls_number_parameters 236 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1912 _refine_ls_wR_factor_gt 0.1805 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 C1 C 1.0542(7) 1.0271(9) 0.1688(4) 0.1267(18) Uani 1 1 d . . . H1A H 1.1168 1.0828 0.1431 0.152 Uiso 1 1 calc R . . H1B H 1.1064 0.9536 0.1894 0.152 Uiso 1 1 calc R . . C2 C 0.9787(7) 1.1161(6) 0.2186(3) 0.1227(16) Uani 1 1 d . . . H2A H 1.0338 1.1267 0.2573 0.147 Uiso 1 1 calc R . . H2B H 0.9574 1.2071 0.2014 0.147 Uiso 1 1 calc R . . C3 C 0.8482(6) 1.0350(6) 0.2318(3) 0.1113(13) Uani 1 1 d . . . H3 H 0.7770 1.0927 0.2522 0.134 Uiso 1 1 calc R . . C4 C 0.8058(5) 0.9904(6) 0.1636(3) 0.1045(12) Uani 1 1 d . . . H4 H 0.7531 1.0650 0.1429 0.125 Uiso 1 1 calc R . . C5 C 0.7237(6) 0.8548(6) 0.1599(3) 0.1112(13) Uani 1 1 d . . . H5 H 0.6816 0.8368 0.2019 0.133 Uiso 1 1 calc R . . C6 C 0.8385(7) 0.7460(6) 0.1479(3) 0.1190(15) Uani 1 1 d . . . H6 H 0.8745 0.7123 0.1891 0.143 Uiso 1 1 calc R . . C7 C 0.9536(8) 0.8209(7) 0.1110(4) 0.1282(18) Uani 1 1 d . . . H7A H 1.0439 0.7853 0.1232 0.154 Uiso 1 1 calc R . . H7B H 0.9418 0.8088 0.0650 0.154 Uiso 1 1 calc R . . C8 C 0.7117(10) 0.3965(9) 0.0797(5) 0.153(3) Uani 1 1 d . . . H8A H 0.7166 0.4363 0.0374 0.230 Uiso 1 1 calc R . . H8B H 0.6185 0.4034 0.0955 0.230 Uiso 1 1 calc R . . H8C H 0.7385 0.3008 0.0777 0.230 Uiso 1 1 calc R . . C9 C 0.6499(8) 0.8910(10) 0.0446(3) 0.1336(19) Uani 1 1 d . . . H9A H 0.5690 0.8839 0.0180 0.200 Uiso 0.50 1 calc PR . . H9B H 0.7208 0.8306 0.0285 0.200 Uiso 0.50 1 calc PR . . H9C H 0.6829 0.9849 0.0443 0.200 Uiso 0.50 1 calc PR . . H9D H 0.7462 0.9157 0.0425 0.200 Uiso 0.50 1 calc PR . . H9E H 0.5944 0.9689 0.0320 0.200 Uiso 0.50 1 calc PR . . H9F H 0.6323 0.8147 0.0162 0.200 Uiso 0.50 1 calc PR . . C10 C 0.4210(6) 1.0447(7) 0.1432(3) 0.1169(15) Uani 1 1 d . . . C11 C 0.4212(8) 1.1047(10) 0.2038(4) 0.1326(19) Uani 1 1 d . . . H11 H 0.4426 1.0522 0.2399 0.159 Uiso 1 1 calc R . . C12 C 0.3894(9) 1.2431(10) 0.2095(5) 0.151(3) Uani 1 1 d . . . H12 H 0.3896 1.2831 0.2502 0.181 Uiso 1 1 calc R . . C13 C 0.3572(8) 1.3244(8) 0.1576(5) 0.142(2) Uani 1 1 d . . . C14 C 0.3590(8) 1.2622(9) 0.0972(5) 0.139(2) Uani 1 1 d . . . H14 H 0.3394 1.3160 0.0613 0.166 Uiso 1 1 calc R . . C15 C 0.3888(8) 1.1243(8) 0.0889(4) 0.1264(17) Uani 1 1 d . . . H15 H 0.3876 1.0846 0.0482 0.152 Uiso 1 1 calc R . . C16 C 0.3251(16) 1.4766(12) 0.1647(8) 0.200(5) Uani 1 1 d . . . H16A H 0.3032 1.5151 0.1234 0.300 Uiso 0.50 1 calc PR . . H16B H 0.4042 1.5236 0.1823 0.300 Uiso 0.50 1 calc PR . . H16C H 0.2474 1.4881 0.1930 0.300 Uiso 0.50 1 calc PR . . H16D H 0.3334 1.5028 0.2091 0.300 Uiso 0.50 1 calc PR . . H16E H 0.2323 1.4943 0.1502 0.300 Uiso 0.50 1 calc PR . . H16F H 0.3892 1.5297 0.1394 0.300 Uiso 0.50 1 calc PR . . N1 N 0.9404(5) 0.9696(5) 0.1289(2) 0.1125(11) Uani 1 1 d . . . N2 N 0.6145(5) 0.8508(6) 0.1107(2) 0.1176(13) Uani 1 1 d . . . O1 O 0.8742(5) 0.9130(4) 0.26749(17) 0.1179(10) Uani 1 1 d . . . H1 H 0.9574 0.9071 0.2751 0.177 Uiso 1 1 calc R . . O2 O 0.7855(8) 0.6314(4) 0.1109(3) 0.153(2) Uani 1 1 d . . . O3 O 0.803(2) 0.4569(13) 0.1918(4) 0.296(8) Uani 1 1 d . . . O4 O 0.9571(7) 0.4613(12) 0.1036(9) 0.259(6) Uani 1 1 d . . . O5 O 0.4422(5) 0.8011(5) 0.1941(2) 0.1381(15) Uani 1 1 d . . . O6 O 0.3711(5) 0.8181(5) 0.0805(3) 0.1398(16) Uani 1 1 d . . . S1 S 0.8202(2) 0.48318(18) 0.12966(11) 0.1451(7) Uani 1 1 d . . . S2 S 0.45377(16) 0.86624(16) 0.13313(8) 0.1206(5) Uani 1 1 d . . . 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 C1 0.113(3) 0.151(5) 0.116(4) 0.014(3) -0.006(3) -0.016(3) C2 0.141(4) 0.110(3) 0.117(4) 0.005(3) -0.014(3) -0.013(3) C3 0.118(3) 0.113(3) 0.103(3) -0.011(2) -0.005(3) 0.004(3) C4 0.111(3) 0.107(3) 0.095(2) 0.001(2) 0.000(2) 0.004(2) C5 0.123(3) 0.115(3) 0.095(2) 0.004(2) -0.007(3) -0.006(2) C6 0.144(4) 0.107(3) 0.105(3) -0.003(2) -0.019(3) 0.010(3) C7 0.135(4) 0.127(4) 0.123(4) -0.006(3) -0.003(3) 0.022(3) C8 0.173(6) 0.130(5) 0.156(6) -0.006(4) 0.003(6) -0.028(4) C9 0.137(4) 0.167(5) 0.097(3) 0.007(3) -0.012(3) -0.018(4) C10 0.113(3) 0.137(4) 0.101(3) 0.000(3) -0.006(2) -0.014(3) C11 0.127(4) 0.159(5) 0.112(4) -0.002(4) 0.001(3) -0.021(4) C12 0.146(5) 0.169(7) 0.138(6) -0.024(5) 0.013(4) -0.003(5) C13 0.139(5) 0.136(5) 0.152(6) -0.007(4) 0.032(4) 0.004(4) C14 0.137(5) 0.136(5) 0.143(5) 0.004(4) 0.013(4) -0.001(4) C15 0.131(4) 0.130(4) 0.118(4) 0.009(3) 0.003(3) -0.011(3) C16 0.240(12) 0.152(7) 0.208(10) -0.010(7) 0.049(10) 0.034(7) N1 0.116(3) 0.119(3) 0.103(2) 0.005(2) 0.000(2) 0.004(2) N2 0.118(3) 0.132(3) 0.103(3) 0.006(2) -0.011(2) -0.004(2) O1 0.130(3) 0.126(2) 0.0979(19) 0.0067(18) -0.0069(19) -0.0111(19) O2 0.235(6) 0.099(2) 0.126(3) 0.001(2) -0.044(4) 0.007(3) O3 0.53(2) 0.224(9) 0.136(5) 0.058(6) -0.082(10) -0.140(12) O4 0.140(5) 0.236(8) 0.402(19) -0.006(12) -0.036(8) 0.041(5) O5 0.145(3) 0.147(3) 0.122(3) 0.020(3) 0.002(3) -0.032(3) O6 0.136(3) 0.145(3) 0.138(3) -0.005(3) -0.026(3) -0.026(3) S1 0.1722(16) 0.1114(9) 0.1516(14) 0.0116(9) -0.0322(13) -0.0012(9) S2 0.1188(8) 0.1245(9) 0.1186(8) 0.0041(7) -0.0093(7) -0.0198(6) _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 C1 N1 1.485(8) . ? C1 C2 1.530(11) . ? C2 C3 1.508(9) . ? C3 O1 1.414(7) . ? C3 C4 1.540(7) . ? C4 N1 1.499(7) . ? C4 C5 1.532(8) . ? C5 N2 1.468(7) . ? C5 C6 1.546(9) . ? C6 O2 1.442(8) . ? C6 C7 1.532(11) . ? C7 N1 1.488(8) . ? C8 S1 1.697(9) . ? C9 N2 1.470(8) . ? C10 C11 1.386(10) . ? C10 C15 1.401(9) . ? C10 S2 1.764(7) . ? C11 C12 1.375(13) . ? C12 C13 1.371(14) . ? C13 C14 1.392(13) . ? C13 C16 1.509(14) . ? C14 C15 1.372(11) . ? N2 S2 1.626(6) . ? O2 S1 1.520(5) . ? O3 S1 1.327(10) . ? O4 S1 1.443(10) . ? O5 S2 1.421(5) . ? O6 S2 1.433(5) . ? 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 C1 C2 103.7(5) . . ? C3 C2 C1 103.3(5) . . ? O1 C3 C2 112.3(5) . . ? O1 C3 C4 107.4(4) . . ? C2 C3 C4 101.4(5) . . ? N1 C4 C5 108.0(4) . . ? N1 C4 C3 104.6(4) . . ? C5 C4 C3 115.0(4) . . ? N2 C5 C4 115.4(5) . . ? N2 C5 C6 112.6(5) . . ? C4 C5 C6 102.5(5) . . ? O2 C6 C7 110.6(6) . . ? O2 C6 C5 110.6(6) . . ? C7 C6 C5 106.3(5) . . ? N1 C7 C6 105.5(5) . . ? C11 C10 C15 120.3(7) . . ? C11 C10 S2 121.0(6) . . ? C15 C10 S2 118.6(5) . . ? C12 C11 C10 119.0(8) . . ? C13 C12 C11 122.5(8) . . ? C12 C13 C14 117.5(7) . . ? C12 C13 C16 121.7(10) . . ? C14 C13 C16 120.7(10) . . ? C15 C14 C13 122.3(9) . . ? C14 C15 C10 118.4(8) . . ? C1 N1 C7 115.9(5) . . ? C1 N1 C4 108.7(5) . . ? C7 N1 C4 108.9(5) . . ? C5 N2 C9 118.6(5) . . ? C5 N2 S2 118.8(4) . . ? C9 N2 S2 117.7(4) . . ? C6 O2 S1 120.5(4) . . ? O3 S1 O4 116.7(12) . . ? O3 S1 O2 113.8(7) . . ? O4 S1 O2 104.1(6) . . ? O3 S1 C8 115.3(6) . . ? O4 S1 C8 105.2(7) . . ? O2 S1 C8 99.8(4) . . ? O5 S2 O6 119.7(3) . . ? O5 S2 N2 106.9(3) . . ? O6 S2 N2 106.4(3) . . ? O5 S2 C10 108.2(3) . . ? O6 S2 C10 107.9(3) . . ? N2 S2 C10 107.1(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 67.57 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.479 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.167 #===END