data_4060246 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C36 H55 N O5 P3 Si V' _chemical_formula_weight 753.75 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' 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 9.4373(8) _cell_length_b 17.0040(11) _cell_length_c 27.820(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.682(3) _cell_angle_gamma 90.00 _cell_volume 4462.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7092 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 25.07 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.392 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4210 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 11.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7314 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2372 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.07 _reflns_number_total 7314 _reflns_number_gt 3346 _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^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7314 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1653 _refine_ls_R_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.2045 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.557 _refine_ls_shift/su_mean 0.012 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 V1 V 0.21492(12) 0.01886(7) 0.22448(5) 0.0190(3) Uani 1 1 d . . . P1 P 0.36309(19) -0.10485(10) 0.20468(8) 0.0222(5) Uani 1 1 d . . . P2 P 0.13951(19) -0.06167(11) 0.29492(8) 0.0240(5) Uani 1 1 d . . . P3 P 0.4234(2) 0.05492(11) 0.27858(8) 0.0255(5) Uani 1 1 d . . . Si1 Si 0.4519(2) -0.11873(11) 0.31332(8) 0.0234(5) Uani 1 1 d . . . O1 O 0.0648(6) 0.1503(3) 0.2675(2) 0.0472(17) Uani 1 1 d . . . O2 O 0.0600(5) -0.0318(3) 0.1892(2) 0.0277(13) Uani 1 1 d . . . O3 O -0.1589(5) -0.0074(3) 0.2148(2) 0.0400(15) Uani 1 1 d . . . O4 O 0.3152(4) 0.0642(3) 0.16992(18) 0.0225(11) Uani 1 1 d . . . O5 O 0.3233(5) 0.1953(3) 0.1749(2) 0.0298(13) Uani 1 1 d . . . N1 N 0.1259(6) 0.0981(3) 0.2459(3) 0.0269(15) Uani 1 1 d . . . C1 C 0.4225(7) -0.1689(4) 0.2537(3) 0.0271(18) Uani 1 1 d . . . H1A H 0.5122 -0.1943 0.2447 0.032 Uiso 1 1 calc R . . H1B H 0.3511 -0.2110 0.2576 0.032 Uiso 1 1 calc R . . C2 C 0.2730(8) -0.1001(4) 0.3382(3) 0.031(2) Uani 1 1 d . . . H2A H 0.2372 -0.1499 0.3517 0.037 Uiso 1 1 calc R . . H2B H 0.2838 -0.0622 0.3651 0.037 Uiso 1 1 calc R . . C3 C 0.5394(7) -0.0201(4) 0.3033(3) 0.0276(18) Uani 1 1 d . . . H3A H 0.5801 -0.0012 0.3344 0.033 Uiso 1 1 calc R . . H3B H 0.6189 -0.0277 0.2813 0.033 Uiso 1 1 calc R . . C4 C 0.5268(8) -0.0825(5) 0.1756(3) 0.0319(19) Uani 1 1 d . . . H4A H 0.5754 -0.1316 0.1678 0.048 Uiso 1 1 calc R . . H4B H 0.5876 -0.0510 0.1973 0.048 Uiso 1 1 calc R . . H4C H 0.5062 -0.0529 0.1460 0.048 Uiso 1 1 calc R . . C5 C 0.2827(8) -0.1728(5) 0.1612(3) 0.036(2) Uani 1 1 d . . . H5A H 0.2712 -0.1466 0.1300 0.054 Uiso 1 1 calc R . . H5B H 0.1898 -0.1895 0.1723 0.054 Uiso 1 1 calc R . . H5C H 0.3440 -0.2190 0.1580 0.054 Uiso 1 1 calc R . . C6 C 0.0091(8) -0.0118(5) 0.3311(4) 0.047(2) Uani 1 1 d . . . H6A H -0.0783 -0.0039 0.3119 0.070 Uiso 1 1 calc R . . H6B H 0.0467 0.0393 0.3416 0.070 Uiso 1 1 calc R . . H6C H -0.0111 -0.0439 0.3593 0.070 Uiso 1 1 calc R . . C7 C 0.0451(8) -0.1488(4) 0.2753(3) 0.034(2) Uani 1 1 d . . . H7A H 0.0128 -0.1778 0.3034 0.051 Uiso 1 1 calc R . . H7B H 0.1083 -0.1824 0.2569 0.051 Uiso 1 1 calc R . . H7C H -0.0369 -0.1337 0.2549 0.051 Uiso 1 1 calc R . . C8 C 0.5451(8) 0.1213(5) 0.2506(3) 0.040(2) Uani 1 1 d . . . H8A H 0.6216 0.1350 0.2736 0.060 Uiso 1 1 calc R . . H8B H 0.4946 0.1691 0.2404 0.060 Uiso 1 1 calc R . . H8C H 0.5851 0.0958 0.2224 0.060 Uiso 1 1 calc R . . C9 C 0.3717(10) 0.1077(5) 0.3320(3) 0.046(2) Uani 1 1 d . . . H9A H 0.4549 0.1337 0.3467 0.069 Uiso 1 1 calc R . . H9B H 0.3323 0.0706 0.3550 0.069 Uiso 1 1 calc R . . H9C H 0.3001 0.1472 0.3231 0.069 Uiso 1 1 calc R . . C10 C 0.5667(8) -0.1800(4) 0.3563(3) 0.0309(19) Uani 1 1 d . . . C11 C 0.7117(9) -0.1907(7) 0.3365(5) 0.076(4) Uani 1 1 d . . . H11A H 0.7696 -0.2229 0.3587 0.113 Uiso 1 1 calc R . . H11B H 0.7565 -0.1392 0.3327 0.113 Uiso 1 1 calc R . . H11C H 0.7035 -0.2170 0.3052 0.113 Uiso 1 1 calc R . . C12 C 0.5012(9) -0.2617(5) 0.3622(4) 0.051(3) Uani 1 1 d . . . H12A H 0.5581 -0.2919 0.3857 0.077 Uiso 1 1 calc R . . H12B H 0.4994 -0.2890 0.3312 0.077 Uiso 1 1 calc R . . H12C H 0.4043 -0.2563 0.3735 0.077 Uiso 1 1 calc R . . C13 C 0.5818(14) -0.1413(7) 0.4049(4) 0.083(4) Uani 1 1 d . . . H13A H 0.4878 -0.1343 0.4183 0.124 Uiso 1 1 calc R . . H13B H 0.6275 -0.0899 0.4015 0.124 Uiso 1 1 calc R . . H13C H 0.6399 -0.1746 0.4265 0.124 Uiso 1 1 calc R . . C14 C -0.0715(7) -0.0056(4) 0.1829(3) 0.0274(18) Uani 1 1 d . . . C15 C -0.1040(7) 0.0279(4) 0.1349(3) 0.0256(18) Uani 1 1 d . . . C16 C -0.0029(8) 0.0269(5) 0.0995(3) 0.0330(19) Uani 1 1 d . . . H16 H 0.0864 0.0026 0.1058 0.040 Uiso 1 1 calc . . . C17 C -0.0326(8) 0.0613(5) 0.0551(3) 0.039(2) Uani 1 1 d . . . H17 H 0.0385 0.0616 0.0317 0.047 Uiso 1 1 calc . . . C18 C -0.1646(8) 0.0958(5) 0.0439(3) 0.033(2) Uani 1 1 d . . . C19 C -0.2631(7) 0.0954(5) 0.0793(3) 0.033(2) Uani 1 1 d . . . H19 H -0.3532 0.1186 0.0727 0.039 Uiso 1 1 calc . . . C20 C -0.2359(7) 0.0621(5) 0.1244(3) 0.0312(19) Uani 1 1 d . . . H20 H -0.3069 0.0627 0.1480 0.037 Uiso 1 1 calc . . . C21 C -0.1922(9) 0.1345(5) -0.0034(3) 0.048(3) Uani 1 1 d . . . H21A H -0.2910 0.1256 -0.0138 0.073 Uiso 1 1 calc R . . H21B H -0.1290 0.1123 -0.0272 0.073 Uiso 1 1 calc R . . H21C H -0.1749 0.1911 -0.0003 0.073 Uiso 1 1 calc R . . C22 C 0.3277(7) 0.1344(4) 0.1520(3) 0.0263(19) Uani 1 1 d . . . C23 C 0.3513(7) 0.1338(4) 0.0991(3) 0.0214(17) Uani 1 1 d . . . C24 C 0.3501(7) 0.0657(4) 0.0720(3) 0.0264(18) Uani 1 1 d . . . H24 H 0.3359 0.0167 0.0875 0.032 Uiso 1 1 calc . . . C25 C 0.3688(7) 0.0669(5) 0.0238(3) 0.0320(19) Uani 1 1 d . . . H25 H 0.3704 0.0184 0.0068 0.038 Uiso 1 1 calc . . . C26 C 0.3856(8) 0.1360(5) -0.0015(3) 0.036(2) Uani 1 1 d . . . C27 C 0.3864(10) 0.2044(5) 0.0260(4) 0.051(3) Uani 1 1 d . . . H27 H 0.3984 0.2533 0.0101 0.061 Uiso 1 1 calc . . . C28 C 0.3707(9) 0.2045(4) 0.0753(3) 0.036(2) Uani 1 1 d . . . H28 H 0.3731 0.2526 0.0927 0.043 Uiso 1 1 calc . . . C29 C 0.4053(11) 0.1378(6) -0.0550(4) 0.062(3) Uani 1 1 d . . . H29A H 0.4149 0.1925 -0.0657 0.093 Uiso 1 1 calc R . . H29B H 0.3228 0.1138 -0.0715 0.093 Uiso 1 1 calc R . . H29C H 0.4909 0.1084 -0.0628 0.093 Uiso 1 1 calc R . . C30 C -0.154(2) -0.3142(13) 0.0762(4) 0.053(4) Uiso 0.65 1 d PG A 1 C31 C -0.2599(18) -0.3490(6) 0.1026(9) 0.057(5) Uiso 0.65 1 d PG A 1 H31 H -0.3061 -0.3951 0.0908 0.068 Uiso 0.65 1 calc P B 1 C32 C -0.2982(11) -0.3164(13) 0.1461(7) 0.052(4) Uiso 0.65 1 d PG A 1 H32 H -0.3707 -0.3401 0.1641 0.062 Uiso 0.65 1 calc P C 1 C33 C -0.231(2) -0.2490(13) 0.1633(3) 0.048(4) Uiso 0.65 1 d PG A 1 H33 H -0.2568 -0.2266 0.1930 0.058 Uiso 0.65 1 calc P D 1 C34 C -0.1246(19) -0.2142(5) 0.1369(8) 0.046(4) Uiso 0.65 1 d PG A 1 H34 H -0.0783 -0.1681 0.1486 0.055 Uiso 0.65 1 calc P E 1 C35 C -0.0862(10) -0.2468(12) 0.0934(7) 0.045(4) Uiso 0.65 1 d PG A 1 H35 H -0.0137 -0.2230 0.0753 0.053 Uiso 0.65 1 calc P F 1 C36 C -0.109(3) -0.3566(17) 0.0281(10) 0.132(9) Uiso 0.65 1 d P A 1 H36A H -0.0079 -0.3703 0.0305 0.197 Uiso 0.65 1 calc PR A 1 H36B H -0.1253 -0.3210 0.0008 0.197 Uiso 0.65 1 calc PR A 1 H36C H -0.1650 -0.4045 0.0233 0.197 Uiso 0.65 1 calc PR A 1 C37 C -0.107(4) -0.280(3) 0.0752(9) 0.064(9) Uiso 0.35 1 d PG G 2 C38 C -0.092(2) -0.2220(16) 0.1101(17) 0.052(8) Uiso 0.35 1 d PG G 2 H38 H -0.0263 -0.1806 0.1062 0.063 Uiso 0.35 1 calc P H 2 C39 C -0.175(4) -0.2245(15) 0.1506(11) 0.035(6) Uiso 0.35 1 d PG G 2 H39 H -0.1652 -0.1847 0.1745 0.042 Uiso 0.35 1 calc P I 2 C40 C -0.272(3) -0.285(3) 0.1563(9) 0.053(8) Uiso 0.35 1 d PG G 2 H40 H -0.3281 -0.2869 0.1840 0.064 Uiso 0.35 1 calc P J 2 C41 C -0.286(3) -0.3434(15) 0.1214(18) 0.048(8) Uiso 0.35 1 d PG G 2 H41 H -0.3521 -0.3849 0.1253 0.057 Uiso 0.35 1 calc P K 2 C42 C -0.203(5) -0.3409(18) 0.0809(12) 0.076(10) Uiso 0.35 1 d PG G 2 H42 H -0.2132 -0.3807 0.0570 0.091 Uiso 0.35 1 calc P L 2 C43 C -0.059(6) -0.283(4) 0.027(2) 0.17(2) Uiso 0.35 1 d P G 2 H43A H -0.0089 -0.2343 0.0192 0.255 Uiso 0.35 1 calc PR G 2 H43B H -0.1414 -0.2887 0.0044 0.255 Uiso 0.35 1 calc PR G 2 H43C H 0.0044 -0.3279 0.0228 0.255 Uiso 0.35 1 calc PR G 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 V1 0.0189(6) 0.0141(6) 0.0238(8) 0.0018(6) -0.0023(5) -0.0019(5) P1 0.0208(10) 0.0169(10) 0.0288(13) -0.0023(9) -0.0035(8) 0.0005(8) P2 0.0214(10) 0.0194(10) 0.0313(13) 0.0073(10) 0.0015(8) 0.0008(8) P3 0.0308(11) 0.0147(10) 0.0304(13) -0.0019(9) -0.0080(9) -0.0058(8) Si1 0.0233(10) 0.0172(11) 0.0294(14) 0.0080(10) -0.0039(9) -0.0013(8) O1 0.064(4) 0.022(3) 0.056(5) 0.005(3) 0.025(3) 0.021(3) O2 0.024(3) 0.020(3) 0.038(4) 0.001(2) -0.006(2) 0.002(2) O3 0.023(3) 0.053(4) 0.044(4) 0.015(3) 0.003(3) -0.001(2) O4 0.025(3) 0.018(3) 0.025(3) 0.005(2) 0.001(2) -0.001(2) O5 0.044(3) 0.011(3) 0.034(4) -0.003(3) 0.001(3) 0.003(2) N1 0.030(3) 0.014(3) 0.037(4) 0.004(3) 0.006(3) 0.003(3) C1 0.025(4) 0.016(4) 0.039(5) 0.005(4) 0.001(3) 0.007(3) C2 0.036(4) 0.023(4) 0.034(5) 0.009(4) -0.012(4) -0.002(3) C3 0.023(4) 0.027(4) 0.033(5) 0.000(4) -0.008(3) -0.002(3) C4 0.033(4) 0.038(5) 0.025(5) 0.000(4) -0.001(4) 0.000(3) C5 0.039(5) 0.031(5) 0.038(6) 0.000(4) -0.011(4) -0.004(4) C6 0.038(5) 0.047(6) 0.055(7) 0.013(5) 0.014(4) 0.012(4) C7 0.025(4) 0.022(4) 0.056(6) 0.008(4) -0.003(4) -0.004(3) C8 0.037(5) 0.032(5) 0.049(6) 0.010(4) -0.024(4) -0.021(4) C9 0.071(6) 0.031(5) 0.034(6) -0.015(4) -0.018(5) -0.001(4) C10 0.026(4) 0.029(5) 0.038(6) 0.006(4) -0.003(3) -0.001(3) C11 0.026(5) 0.096(9) 0.105(11) 0.071(8) 0.001(5) 0.011(5) C12 0.041(5) 0.034(5) 0.078(8) 0.026(5) -0.015(5) -0.007(4) C13 0.117(10) 0.078(9) 0.050(8) 0.012(6) -0.046(7) 0.010(7) C14 0.019(4) 0.027(5) 0.036(5) 0.000(4) -0.003(3) -0.005(3) C15 0.017(4) 0.025(4) 0.034(5) 0.002(4) -0.008(3) -0.005(3) C16 0.026(4) 0.045(5) 0.027(5) -0.006(4) -0.008(3) 0.004(4) C17 0.033(5) 0.050(6) 0.034(6) -0.013(5) -0.002(4) 0.000(4) C18 0.031(4) 0.034(5) 0.032(5) -0.001(4) -0.011(4) -0.007(3) C19 0.020(4) 0.041(5) 0.037(6) 0.003(4) -0.006(4) -0.005(3) C20 0.020(4) 0.037(5) 0.036(5) 0.006(4) -0.007(3) -0.008(3) C21 0.051(6) 0.052(6) 0.041(6) 0.018(5) -0.011(5) -0.005(4) C22 0.022(4) 0.020(4) 0.037(5) 0.011(4) -0.005(3) 0.002(3) C23 0.020(4) 0.024(4) 0.020(4) 0.008(3) -0.008(3) 0.001(3) C24 0.012(3) 0.029(4) 0.038(5) -0.002(4) -0.008(3) 0.002(3) C25 0.024(4) 0.047(5) 0.024(5) -0.006(4) -0.001(3) 0.009(4) C26 0.030(4) 0.048(5) 0.031(5) 0.003(5) -0.001(4) 0.020(4) C27 0.065(6) 0.047(6) 0.041(7) 0.016(5) 0.016(5) 0.026(5) C28 0.053(5) 0.022(4) 0.034(6) 0.010(4) 0.014(4) 0.009(4) C29 0.076(7) 0.083(8) 0.028(6) 0.005(5) 0.006(5) 0.039(6)