#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4060000.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4060000 _journal_name_full 'Organometallics' _journal_year 2005 _chemical_formula_sum 'C42 H52 O6' _chemical_formula_weight 652.84 _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(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 8.574(2) _cell_length_b 15.235(4) _cell_length_c 28.536(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3727.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3320 _cell_measurement_theta_min 4.961 _cell_measurement_theta_max 39.124 _exptl_crystal_colour colorless _exptl_crystal_size_max 0.516 _exptl_crystal_size_mid 0.192 _exptl_crystal_size_min 0.086 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.77100 _exptl_absorpt_correction_T_max 1.00000 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 22118 _diffrn_reflns_av_R_equivalents 0.1084 _diffrn_reflns_av_sigmaI/netI 0.1032 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8094 _reflns_number_gt 4651 _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^)+(0.0482P)^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 SHELXL _refine_ls_extinction_coef 0.0022(6) _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 0.8(14) _chemical_absolute_configuration unk _refine_ls_number_reflns 8094 _refine_ls_number_parameters 442 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1267 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.081 _refine_ls_shift/su_mean 0.028 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 O1 O 0.4659(4) 0.2290(2) -0.02842(12) 0.1236(13) Uani 1 1 d . . . O2 O 0.5423(3) 0.14530(15) 0.03059(8) 0.0692(6) Uani 1 1 d . . . O3 O 0.8468(2) 0.12866(12) 0.15366(9) 0.0584(6) Uani 1 1 d . . . H3 H 0.8633 0.0763 0.1581 0.088 Uiso 1 1 calc R . . O4 O 0.3909(3) -0.31124(17) -0.00115(9) 0.0841(8) Uani 1 1 d . . . O5 O 0.3281(3) -0.18699(13) 0.03477(7) 0.0608(6) Uani 1 1 d . . . O6 O 0.0008(3) -0.04142(15) 0.15350(9) 0.0712(7) Uani 1 1 d . . . H6 H -0.0091 -0.0556 0.1259 0.107 Uiso 1 1 calc R . . C1 C 0.5591(3) 0.11234(17) 0.16266(10) 0.0453(7) Uani 1 1 d . . . H1 H 0.4739 0.1533 0.1694 0.054 Uiso 1 1 calc R . . C2 C 0.5074(3) 0.02120(18) 0.17950(10) 0.0457(7) Uani 1 1 d . . . H2 H 0.5105 0.0120 0.2135 0.055 Uiso 1 1 calc R . . C3 C 0.6135(3) -0.03669(17) 0.15123(11) 0.0448(7) Uani 1 1 d . . . H3A H 0.6571 -0.0893 0.1613 0.054 Uiso 1 1 calc R . . C4 C 0.6341(3) -0.00058(17) 0.11006(10) 0.0419(7) Uani 1 1 d . . . C5 C 0.5469(3) 0.08702(16) 0.10998(10) 0.0404(7) Uani 1 1 d . . . C6 C 0.6086(4) 0.15587(18) 0.07694(10) 0.0491(7) Uani 1 1 d . . . H6A H 0.7221 0.1496 0.0748 0.059 Uiso 1 1 calc R . . C7 C 0.5700(4) 0.25156(17) 0.09082(12) 0.0572(9) Uani 1 1 d . . . H7 H 0.4675 0.2541 0.1059 0.069 Uiso 1 1 calc R . . C8 C 0.6932(4) 0.28978(19) 0.12314(14) 0.0698(10) Uani 1 1 d . . . H8A H 0.7942 0.2806 0.1086 0.084 Uiso 1 1 calc R . . H8B H 0.6766 0.3527 0.1248 0.084 Uiso 1 1 calc R . . C9 C 0.7017(4) 0.25504(19) 0.17284(14) 0.0680(10) Uani 1 1 d . . . H9A H 0.6105 0.2760 0.1895 0.082 Uiso 1 1 calc R . . H9B H 0.7922 0.2810 0.1878 0.082 Uiso 1 1 calc R . . C10 C 0.7111(4) 0.15524(18) 0.17970(11) 0.0532(8) Uani 1 1 d . . . C11 C 0.5639(4) 0.2965(2) 0.04350(15) 0.0804(12) Uani 1 1 d . . . H11 H 0.6695 0.3158 0.0354 0.096 Uiso 1 1 calc R . . C12 C 0.5182(5) 0.2248(3) 0.01054(17) 0.0838(12) Uani 1 1 d . . . C13 C 0.4540(5) 0.3754(3) 0.0390(2) 0.1194(18) Uani 1 1 d . . . H13A H 0.4638 0.4003 0.0082 0.149 Uiso 1 1 calc R . . H13B H 0.4811 0.4188 0.0620 0.149 Uiso 1 1 calc R . . H13C H 0.3484 0.3566 0.0439 0.149 Uiso 1 1 calc R . . C14 C 0.7375(5) 0.1349(3) 0.23119(12) 0.0829(12) Uani 1 1 d . . . H14A H 0.7664 0.0744 0.2346 0.124 Uiso 1 1 calc R . . H14B H 0.6433 0.1460 0.2484 0.124 Uiso 1 1 calc R . . H14C H 0.8195 0.1716 0.2431 0.124 Uiso 1 1 calc R . . C15 C 0.7153(4) -0.0371(2) 0.06834(12) 0.0657(9) Uani 1 1 d . . . H15A H 0.7539 -0.0947 0.0755 0.098 Uiso 1 1 calc R . . H15B H 0.8009 0.0004 0.0600 0.098 Uiso 1 1 calc R . . H15C H 0.6436 -0.0405 0.0426 0.098 Uiso 1 1 calc R . . C31 C 0.7577(6) 0.5586(3) 0.10769(19) 0.1061(16) Uani 1 1 d . . . H31 H 0.8078 0.5162 0.0897 0.127 Uiso 1 1 calc R . . C32 C 0.7028(6) 0.6332(4) 0.08705(17) 0.1018(15) Uani 1 1 d . . . H32 H 0.7155 0.6417 0.0550 0.122 Uiso 1 1 calc R . . C33 C 0.6290(5) 0.6957(3) 0.1136(2) 0.0975(14) Uani 1 1 d . . . H33 H 0.5934 0.7470 0.0996 0.117 Uiso 1 1 calc R . . C34 C 0.6079(6) 0.6832(4) 0.1595(2) 0.1065(15) Uani 1 1 d . . . H34 H 0.5550 0.7246 0.1774 0.128 Uiso 1 1 calc R . . C35 C 0.6648(8) 0.6096(4) 0.17956(18) 0.1230(19) Uani 1 1 d . . . H35 H 0.6527 0.6018 0.2117 0.148 Uiso 1 1 calc R . . C36 C 0.7392(8) 0.5462(3) 0.1543(2) 0.130(2) Uani 1 1 d . . . H36 H 0.7764 0.4957 0.1688 0.155 Uiso 1 1 calc R . . C37 C 0.2647(11) 0.4117(4) 0.1680(4) 0.157(3) Uani 1 1 d D . . H37 H 0.2926 0.4664 0.1563 0.159 Uiso 1 1 calc R . . C38 C 0.3176(8) 0.3862(7) 0.2091(4) 0.149(3) Uani 1 1 d D . . H38 H 0.3839 0.4222 0.2263 0.159 Uiso 1 1 calc R . . C39 C 0.2735(15) 0.3054(10) 0.2264(2) 0.150(6) Uani 1 1 d D . . H39 H 0.3053 0.2852 0.2556 0.158 Uiso 1 1 calc R . . C40 C 0.1831(13) 0.2589(5) 0.1985(5) 0.159(6) Uani 1 1 d D . . H40 H 0.1536 0.2032 0.2085 0.163 Uiso 1 1 calc R . . C41 C 0.1335(8) 0.2852(7) 0.1589(5) 0.155(5) Uani 1 1 d D . . H41 H 0.0683 0.2497 0.1409 0.160 Uiso 1 1 calc R . . C42 C 0.1745(10) 0.3612(9) 0.1439(2) 0.159(3) Uani 1 1 d D . . H42 H 0.1383 0.3803 0.1150 0.161 Uiso 1 1 calc R . . C1' C 0.2772(3) -0.07573(16) 0.14876(10) 0.0400(7) Uani 1 1 d . . . H1' H 0.3541 -0.1188 0.1596 0.048 Uiso 1 1 calc R . . C2' C 0.3445(3) 0.01794(16) 0.15717(10) 0.0426(7) Uani 1 1 d . . . H2' H 0.2711 0.0526 0.1759 0.051 Uiso 1 1 calc R . . C3' C 0.3681(3) 0.06132(17) 0.10877(10) 0.0440(7) Uani 1 1 d . . . H3' H 0.3042 0.1145 0.1065 0.053 Uiso 1 1 calc R . . C4' C 0.3103(3) -0.00572(17) 0.07491(10) 0.0477(7) Uani 1 1 d . . . C5' C 0.2687(3) -0.08049(17) 0.09615(10) 0.0419(7) Uani 1 1 d . . . C6' C 0.2145(3) -0.15965(17) 0.07014(10) 0.0464(7) Uani 1 1 d . . . H6' H 0.1174 -0.1444 0.0540 0.056 Uiso 1 1 calc R . . C7' C 0.1858(4) -0.24283(16) 0.09810(10) 0.0458(7) Uani 1 1 d . . . H7' H 0.2764 -0.2530 0.1183 0.055 Uiso 1 1 calc R . . C8' C 0.0428(4) -0.2374(2) 0.12873(12) 0.0617(9) Uani 1 1 d . . . H8'1 H 0.0063 -0.2964 0.1354 0.074 Uiso 1 1 calc R . . H8'2 H -0.0390 -0.2070 0.1118 0.074 Uiso 1 1 calc R . . C9' C 0.0721(4) -0.1901(2) 0.17468(12) 0.0637(9) Uani 1 1 d . . . H9'1 H 0.1520 -0.2226 0.1913 0.076 Uiso 1 1 calc R . . H9'2 H -0.0226 -0.1945 0.1931 0.076 Uiso 1 1 calc R . . C10' C 0.1215(4) -0.09306(19) 0.17460(11) 0.0517(8) Uani 1 1 d . . . C11' C 0.1890(4) -0.31030(18) 0.05891(11) 0.0536(8) Uani 1 1 d . . . H11' H 0.0885 -0.3082 0.0426 0.064 Uiso 1 1 calc R . . C12' C 0.3107(4) -0.2749(2) 0.02684(12) 0.0600(9) Uani 1 1 d . . . C13' C 0.2196(5) -0.4049(2) 0.07361(14) 0.0827(12) Uani 1 1 d . . . H13D H 0.2340 -0.4406 0.0462 0.124 Uiso 1 1 calc R . . H13E H 0.1322 -0.4265 0.0912 0.124 Uiso 1 1 calc R . . H13F H 0.3118 -0.4073 0.0926 0.124 Uiso 1 1 calc R . . C14' C 0.1299(5) -0.0651(2) 0.22538(12) 0.0780(11) Uani 1 1 d . . . H14D H 0.1331 -0.0022 0.2272 0.117 Uiso 1 1 calc R . . H14E H 0.2222 -0.0891 0.2395 0.117 Uiso 1 1 calc R . . H14F H 0.0396 -0.0863 0.2418 0.117 Uiso 1 1 calc R . . C15' C 0.2918(5) 0.0109(2) 0.02330(11) 0.0769(11) Uani 1 1 d . . . H15D H 0.3917 0.0070 0.0083 0.115 Uiso 1 1 calc R . . H15E H 0.2491 0.0685 0.0185 0.115 Uiso 1 1 calc R . . H15F H 0.2227 -0.0321 0.0101 0.115 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 O1 0.138(3) 0.140(3) 0.093(2) 0.063(2) -0.037(2) -0.028(2) O2 0.0856(17) 0.0618(14) 0.0602(14) 0.0168(13) -0.0057(14) -0.0131(13) O3 0.0527(13) 0.0415(11) 0.0810(16) -0.0103(12) 0.0011(12) -0.0052(10) O4 0.103(2) 0.0726(16) 0.0767(17) -0.0275(15) 0.0241(16) -0.0159(15) O5 0.0817(15) 0.0451(12) 0.0555(13) -0.0067(10) 0.0061(13) -0.0184(11) O6 0.0472(12) 0.0624(15) 0.104(2) -0.0089(15) -0.0027(14) 0.0126(11) C1 0.0524(18) 0.0369(15) 0.0464(17) -0.0081(14) 0.0013(15) -0.0039(13) C2 0.0533(18) 0.0435(16) 0.0402(16) 0.0017(14) -0.0060(15) -0.0052(14) C3 0.0445(17) 0.0322(14) 0.058(2) 0.0012(14) -0.0122(16) -0.0006(12) C4 0.0456(16) 0.0328(14) 0.0474(17) -0.0030(14) -0.0064(15) -0.0002(13) C5 0.0487(17) 0.0300(13) 0.0423(16) -0.0026(13) -0.0061(14) -0.0037(12) C6 0.0528(18) 0.0435(16) 0.0510(18) 0.0031(15) -0.0015(16) -0.0018(14) C7 0.0521(19) 0.0316(15) 0.088(2) 0.0095(17) 0.0066(18) -0.0020(14) C8 0.070(2) 0.0351(16) 0.104(3) -0.0008(19) 0.006(2) -0.0016(17) C9 0.062(2) 0.0423(17) 0.100(3) -0.0302(19) 0.006(2) -0.0059(17) C10 0.0549(19) 0.0432(16) 0.062(2) -0.0146(15) 0.0003(18) -0.0067(16) C11 0.068(2) 0.056(2) 0.118(3) 0.036(2) -0.007(2) -0.0086(19) C12 0.078(3) 0.088(3) 0.086(3) 0.044(3) -0.006(2) -0.013(2) C13 0.096(3) 0.089(3) 0.174(5) 0.064(3) -0.008(3) 0.019(3) C14 0.095(3) 0.093(3) 0.061(2) -0.020(2) -0.008(2) -0.028(2) C15 0.071(2) 0.0546(19) 0.071(2) -0.0091(17) 0.005(2) 0.0118(18) C31 0.147(5) 0.081(3) 0.090(3) -0.023(3) 0.006(3) -0.024(3) C32 0.112(4) 0.120(4) 0.074(3) 0.005(3) -0.012(3) -0.043(3) C33 0.090(3) 0.094(3) 0.109(4) 0.011(3) -0.024(3) -0.021(3) C34 0.104(3) 0.119(4) 0.097(4) -0.008(4) 0.010(3) 0.001(3) C35 0.190(6) 0.102(4) 0.077(3) 0.002(3) 0.009(4) -0.015(4) C36 0.207(7) 0.082(3) 0.100(4) -0.002(3) -0.011(5) -0.028(4) C37 0.160(7) 0.096(4) 0.216(9) 0.040(6) 0.001(6) -0.025(4) C38 0.123(5) 0.161(6) 0.162(7) -0.105(6) -0.049(5) 0.016(5) C39 0.213(12) 0.277(14) 0.080(4) 0.008(6) 0.039(5) 0.163(11) C40 0.163(11) 0.093(5) 0.251(13) 0.071(7) 0.123(10) 0.043(5) C41 0.066(3) 0.161(8) 0.297(15) -0.135(9) 0.018(7) -0.015(5) C42 0.134(7) 0.244(11) 0.099(4) 0.003(7) -0.024(4) 0.014(7) C1' 0.0407(16) 0.0286(13) 0.0508(17) 0.0068(12) -0.0069(14) -0.0011(12) C2' 0.0512(18) 0.0326(14) 0.0440(17) -0.0027(13) -0.0002(14) 0.0024(12) C3' 0.0505(17) 0.0281(13) 0.0535(18) 0.0011(13) -0.0063(16) 0.0013(12) C4' 0.0549(18) 0.0355(14) 0.0525(18) 0.0073(14) -0.0148(16) -0.0028(15) C5' 0.0433(17) 0.0343(14) 0.0479(17) 0.0014(13) -0.0114(14) -0.0019(12) C6' 0.0452(16) 0.0429(16) 0.0511(18) 0.0052(14) -0.0104(16) -0.0048(14) C7' 0.0447(17) 0.0338(14) 0.0589(19) 0.0050(13) -0.0054(15) -0.0022(13) C8' 0.058(2) 0.0422(17) 0.085(2) 0.0026(18) 0.009(2) -0.0120(16) C9' 0.062(2) 0.0586(19) 0.071(2) 0.0045(19) 0.0200(19) -0.0112(17) C10' 0.0466(18) 0.0497(17) 0.059(2) 0.0029(16) 0.0079(17) 0.0044(15) C11' 0.0579(19) 0.0394(15) 0.064(2) -0.0006(15) -0.0076(18) -0.0054(15) C12' 0.072(2) 0.0517(19) 0.057(2) -0.0062(17) -0.007(2) -0.0099(18) C13' 0.102(3) 0.0390(17) 0.107(3) -0.001(2) 0.016(3) 0.0036(19) C14' 0.088(3) 0.082(3) 0.064(2) -0.006(2) 0.016(2) -0.022(2) C15' 0.113(3) 0.0535(19) 0.064(2) 0.0164(18) -0.033(2) -0.022(2)