#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/32/2003292.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003292 loop_ _publ_author_name 'Chiaroni, A.' 'Gu\'enard, D.' 'Gu\'eritte-Voegelein, F.' 'Khuong-Huu, F.' 'Py, S.' 'Riche, C.' 'Wahl, A.' _publ_contact_author ; Dr Claude Riche Institut de Chimie des Substances Naturelles CNRS 91198 Gif-sur-Yvette CEDEX France ; _publ_section_title ; A Baccatin III Derivative ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 465 _journal_page_last 468 _journal_paper_doi 10.1107/S0108270194007341 _journal_volume 51 _journal_year 1995 _chemical_compound_source ; chemical synthesis ; _chemical_formula_moiety 'C26 H44 O8 Si' _chemical_formula_sum 'C26 H44 O8 Si' _chemical_formula_weight 512.72 _chemical_name_systematic ; Baccatin III derivative ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_type_scat_source ;International Tables for X-ray Crystallography (1974, Vol IV, Table 2.2B) ; _cell_angle_alpha 90.00 _cell_angle_beta 100.15(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.323(4) _cell_length_b 10.569(5) _cell_length_c 17.022(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 22.2 _cell_measurement_theta_min 13.4 _cell_volume 1473.9(13) _computing_data_collection 'CAD4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'NONIUS (Riche, 1989)' _computing_molecular_graphics 'R3M (Riche, 1983), ORTEP (Johnson, 1965)' _computing_publication_material 'ACTACIF (Riche, 1992)' _computing_structure_refinement 'SHELX76 (Sheldrick, 1976)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 293 _diffrn_measurement_device 'Nonius CAD4 diffractometer' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.079 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2766 _diffrn_reflns_theta_max 65.68 _diffrn_reflns_theta_min 2.64 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 166 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.03 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.16 _exptl_crystal_description prism _exptl_crystal_F_000 556.00 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.53 _refine_diff_density_min -0.56 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.25 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 285 _refine_ls_number_reflns 1615 _refine_ls_R_factor_obs 0.105 _refine_ls_shift/esd_max 0.04 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w=1/[\s^2^(F) + 0.163230 F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.145 _reflns_number_observed 1630 _reflns_number_total 2674 _reflns_observed_criterion refl_observed_if_I_>_2.5_sigma(I) _cod_data_source_file pa1126.cif _cod_data_source_block taxane _cod_depositor_comments ; Adding _atom_site_type_symbol tag to prevent confusion between Ho and H atoms. Andrius Merkys 2013-10-29 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(F) + 0.163230 F^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(F) + 0.163230 F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2003292 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,-z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.0307(47) 0.0064(45) 0.0208(47) 0.0382(61) 0.0230(58) 0.0609(70) C2 0.0319(50) -0.0101(50) 0.0050(42) 0.0546(73) 0.0052(52) 0.0350(60) C3 0.0314(46) -0.0030(40) 0.0256(45) 0.0310(54) -0.0026(46) 0.0491(62) C4 0.0395(53) -0.0064(53) 0.0228(50) 0.0503(69) -0.0166(60) 0.0502(71) C5 0.0322(52) -0.0125(49) 0.0251(53) 0.0450(70) -0.0170(66) 0.0823(89) C6 0.0315(54) 0.0062(60) 0.0051(51) 0.0724(95) 0.0082(74) 0.0621(78) C7 0.0454(57) -0.0029(59) 0.0374(55) 0.0565(76) -0.0071(66) 0.0573(71) C8 0.0448(56) 0.0086(48) 0.0224(54) 0.0318(61) 0.0137(55) 0.0572(70) C9 0.0321(43) 0.0071(43) 0.0273(43) 0.0226(47) 0.0146(50) 0.0519(61) C10 0.0280(42) 0.0124(42) 0.0188(40) 0.0327(55) 0.0064(50) 0.0453(59) C11 0.0284(44) 0.0003(42) 0.0172(42) 0.0295(52) 0.0002(49) 0.0458(59) C12 0.0384(52) 0.0025(46) 0.0179(48) 0.0354(61) -0.0092(51) 0.0459(64) C13 0.0471(62) -0.0114(67) 0.0203(53) 0.0879(99) -0.0369(73) 0.0446(68) C14 0.0469(59) -0.0003(64) 0.0317(57) 0.0601(82) -0.0022(73) 0.0655(80) C15 0.0272(43) 0.0026(44) -0.0009(40) 0.0380(59) 0.0054(53) 0.0392(57) C16 0.0433(56) -0.0100(48) 0.0336(56) 0.0284(54) -0.0044(63) 0.0785(85) C17 0.0551(65) 0.0026(60) 0.0173(56) 0.0626(85) 0.0086(61) 0.0416(66) C18 0.0712(85) 0.0131(65) 0.0218(77) 0.0426(74) 0.0171(74) 0.0855(97) C19 0.0452(59) -0.0013(55) 0.0244(59) 0.0461(71) -0.0091(70) 0.0713(81) C20 0.0497(60) -0.0230(57) 0.0105(50) 0.0531(73) -0.0080(55) 0.0341(57) O1 0.0421(38) -0.0032(39) 0.0139(37) 0.0569(56) 0.0184(47) 0.0659(50) O2 0.0565(47) -0.0288(47) 0.0160(43) 0.0684(64) 0.0137(52) 0.0677(57) O4 0.0384(38) 0.0074(41) 0.0318(40) 0.0706(61) -0.0289(54) 0.0812(63) O5 0.0553(47) -0.0104(48) 0.0242(40) 0.0724(65) -0.0040(49) 0.0612(55) O7 0.0547(44) 0.0051(45) 0.0430(40) 0.0656(59) 0.0225(52) 0.0654(54) O9 0.0282(33) -0.0007(35) 0.0177(33) 0.0591(54) -0.0162(43) 0.0658(51) O10 0.0477(42) -0.0129(35) 0.0324(39) 0.0350(44) -0.0022(41) 0.0750(58) O13 0.0460(45) 0.0164(43) 0.0310(43) 0.0742(70) -0.0288(57) 0.0857(66) Si 0.0807(27) 0.0193(28) 0.0628(26) 0.1040(40) 0.0484(35) 0.1088(36) loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom C C1 0.7446(12) -0.0157(13) 0.9630(7) 0.044(11) Uani ? ? C C2 0.6801(12) -0.0723(14) 0.8826(6) 0.041(11) Uani ? ? C C3 0.6388(11) 0.0138(12) 0.8073(6) 0.037(10) Uani ? ? C C4 0.4554(13) -0.0163(14) 0.7747(7) 0.047(11) Uani ? ? C C5 0.3929(13) 0.0032(14) 0.6865(9) 0.054(13) Uani ? ? C C6 0.5218(13) -0.0052(17) 0.6354(8) 0.056(14) Uani ? ? C C7 0.6778(13) 0.0625(15) 0.6691(7) 0.053(12) Uani ? ? C C8 0.7618(13) -0.0040(13) 0.7481(7) 0.045(11) Uani ? ? C C9 0.9228(11) 0.0660(11) 0.7784(6) 0.036(9) Uani ? ? C C10 0.9349(11) 0.1860(12) 0.8330(6) 0.036(9) Uani ? ? C C11 0.8630(11) 0.1721(12) 0.9086(6) 0.035(9) Uani ? ? C C12 0.7356(12) 0.2423(12) 0.9166(7) 0.040(10) Uani ? ? C C13 0.6175(14) 0.2139(17) 0.9723(8) 0.060(14) Uani ? ? C C14 0.6232(14) 0.0724(16) 0.9955(8) 0.058(13) Uani ? ? C C15 0.9073(11) 0.0581(12) 0.9659(6) 0.036(9) Uani ? ? C C16 1.0429(13) -0.0259(12) 0.9452(8) 0.051(12) Uani ? ? C C17 0.9750(15) 0.1107(14) 1.0475(7) 0.054(13) Uani ? ? C C18 0.6803(17) 0.3622(15) 0.8631(10) 0.068(15) Uani ? ? C C19 0.8045(14) -0.1407(14) 0.7299(8) 0.055(13) Uani ? ? C C20 0.4331(14) -0.1443(14) 0.8085(6) 0.046(11) Uani ? ? O O1 0.7820(9) -0.1210(10) 1.0167(5) 0.056(9) Uani ? ? O O2 0.5346(11) -0.1429(11) 0.8863(5) 0.065(10) Uani ? ? O O4 0.3753(9) 0.0781(12) 0.8168(6) 0.064(10) Uani ? ? O O5 0.2616(10) -0.0798(12) 0.6550(5) 0.064(10) Uani ? ? O O7 0.7870(9) 0.0609(9) 0.6145(5) 0.062(9) Uani ? ? O O9 1.0440(8) 0.0325(10) 0.7546(5) 0.052(8) Uani ? ? O O10 1.0986(9) 0.2254(9) 0.8459(5) 0.053(9) Uani ? ? O O13 0.4630(10) 0.2522(12) 0.9393(6) 0.069(11) Uani ? ? Si Si 0.8044(6) 0.1623 0.5424(3) 0.099(6) Uani ? ? C C21 1.0141(12) 0.1475(15) 0.5218(8) 0.083(5) Uiso ? ? C C22 1.0581(17) 0.2205(20) 0.4567(10) 0.097(6) Uiso ? ? C C23 0.7612(23) 0.3239(9) 0.5752(12) 0.216(18) Uiso ? ? C C24 0.8852(36) 0.3834(23) 0.6339(21) 0.200(16) Uiso ? ? C C25 0.6503(19) 0.1201(18) 0.4530(8) 0.229(20) Uiso ? ? C C26 0.6611(38) -0.0049(26) 0.4196(18) 0.201(16) Uiso ? ? H H2 0.77739 -0.12217 0.87362 0.045 Uiso calc C2 H H3 0.65217 0.10649 0.81837 0.041 Uiso calc C3 H H5 0.35159 0.09221 0.68416 0.059 Uiso calc C5 H H6a 0.47727 0.03228 0.58205 0.062 Uiso calc C6 H H6b 0.54755 -0.09652 0.62850 0.062 Uiso calc C6 H H7 0.65012 0.15207 0.68002 0.059 Uiso calc C7 H H10 0.86285 0.25370 0.80483 0.039 Uiso calc C10 H H13 0.65141 0.26309 1.02266 0.066 Uiso calc C13 H H14a 0.64965 0.06816 1.05502 0.064 Uiso calc C14 H H14b 0.51143 0.03728 0.97693 0.064 Uiso calc C14 H H16a 1.14494 0.02513 0.94769 0.056 Uiso calc C16 H H16b 1.06363 -0.09729 0.98417 0.056 Uiso calc C16 H H16c 1.00934 -0.06055 0.89007 0.056 Uiso calc C16 H H17a 1.07902 0.15690 1.04549 0.059 Uiso calc C17 H H17b 0.89404 0.17031 1.06424 0.059 Uiso calc C17 H H17c 0.99671 0.03975 1.08677 0.059 Uiso calc C17 H H18a 0.58158 0.40058 0.87952 0.074 Uiso calc C18 H H18b 0.77075 0.42570 0.86998 0.074 Uiso calc C18 H H18c 0.65366 0.33613 0.80576 0.074 Uiso calc C18 H H19a 0.88337 -0.14077 0.69185 0.060 Uiso calc C19 H H19b 0.85514 -0.18393 0.78051 0.060 Uiso calc C19 H H19c 0.70301 -0.18673 0.70546 0.060 Uiso calc C19 H H20a 0.46903 -0.21201 0.77440 0.051 Uiso calc C20 H H20b 0.31626 -0.15860 0.81287 0.051 Uiso calc C20 H H21a 1.03204 0.05630 0.51036 0.091 Uiso calc C21 H H21b 1.09034 0.17281 0.57153 0.091 Uiso calc C21 H H22a 1.17442 0.20316 0.45257 0.107 Uiso calc C22 H H22b 0.98587 0.19602 0.40558 0.107 Uiso calc C22 H H22c 1.04426 0.31270 0.46684 0.107 Uiso calc C22 H H23a 0.65824 0.31498 0.59734 0.237 Uiso calc C23 H H23b 0.73997 0.37721 0.52590 0.237 Uiso calc C23 H H24a 0.84666 0.46895 0.64749 0.220 Uiso calc C24 H H24b 0.90642 0.33005 0.68321 0.220 Uiso calc C24 H H24c 0.98815 0.39228 0.61177 0.220 Uiso calc C24 H H25a 0.53571 0.13620 0.46069 0.252 Uiso calc C25 H H25b 0.68227 0.18478 0.41575 0.252 Uiso calc C25 H H26a 0.77568 -0.02103 0.41193 0.221 Uiso calc C26 H H26b 0.62912 -0.06961 0.45687 0.221 Uiso calc C26 H H26c 0.58594 -0.01053 0.36700 0.221 Uiso calc C26 H HO1 0.68014 -0.17073 1.01747 0.061 Uiso calc O1 H HO4 0.25430 0.06639 0.80427 0.070 Uiso calc O4 H HO5 0.16747 -0.06608 0.68327 0.070 Uiso calc O5 H HO10 1.13923 0.23740 0.90433 0.059 Uiso calc O10 H HO13 0.42572 0.20692 0.88772 0.076 Uiso calc O13 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 2 3 -2 -1 4 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C2 C1 C14 114.4(10) yes C2 C1 C15 113.4(10) yes C2 C1 O1 105.9(9) yes C14 C1 C15 107.9(10) yes C14 C1 O1 108.7(10) yes C15 C1 O1 106.2(9) yes C1 C2 C3 120.5(10) yes C1 C2 O2 109.6(10) yes C3 C2 O2 105.9(9) yes C2 C3 C4 103.5(9) yes C2 C3 C8 112.5(9) yes C4 C3 C8 117.1(9) yes C3 C4 C5 117.9(10) yes C3 C4 C20 103.2(10) yes C3 C4 O4 100.9(9) yes C5 C4 C20 117.5(11) yes C5 C4 O4 106.7(10) yes C20 C4 O4 109.4(10) yes C4 C5 C6 114.3(11) yes C4 C5 O5 113.3(11) yes C6 C5 O5 108.9(11) yes C5 C6 C7 114.1(11) yes C6 C7 C8 109.8(11) yes C6 C7 O7 110.9(11) yes C8 C7 O7 108.6(10) yes C3 C8 C7 104.7(9) yes C3 C8 C9 110.9(9) yes C3 C8 C19 116.4(10) yes C7 C8 C9 107.6(10) yes C7 C8 C19 109.4(10) yes C9 C8 C19 107.6(10) yes C8 C9 C10 123.4(9) yes C8 C9 O9 118.5(10) yes C10 C9 O9 117.9(9) yes C9 C10 C11 115.5(9) yes C9 C10 O10 107.0(8) yes C11 C10 O10 114.4(9) yes C10 C11 C12 118.4(10) yes C10 C11 C15 121.5(9) yes C12 C11 C15 118.5(10) yes C11 C12 C13 125.1(11) yes C11 C12 C18 123.2(11) yes C13 C12 C18 111.4(11) yes C12 C13 C14 111.0(11) yes C12 C13 O13 110.6(11) yes C14 C13 O13 112.0(12) yes C1 C14 C13 119.0(11) yes C1 C15 C11 105.1(9) yes C1 C15 C16 112.1(9) yes C1 C15 C17 113.2(10) yes C11 C15 C16 114.2(9) yes C11 C15 C17 107.5(9) yes C16 C15 C17 104.8(9) yes C4 C20 O2 104.6(10) yes C2 O2 C20 109.1(9) yes C7 O7 Si 129.2(8) yes O7 Si C21 107.2(5) yes O7 Si C23 109.1(6) yes O7 Si C25 108.2(6) yes C21 Si C23 112.1(7) yes C21 Si C25 111.3(7) yes C23 Si C25 109.0(8) yes Si C21 C22 118.3(11) yes Si C23 C24 117.1(16) yes Si C25 C26 117.2(15) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 1.50(2) yes C1 C14 1.55(2) yes C1 C15 1.560(10) yes C1 O1 1.44(2) yes C2 C3 1.56(2) yes C2 O2 1.43(2) yes C3 C4 1.560(10) yes C3 C8 1.57(2) yes C4 C5 1.51(2) yes C4 C20 1.49(2) yes C4 O4 1.46(2) yes C5 C6 1.50(2) yes C5 O5 1.43(2) yes C6 C7 1.50(2) yes C7 C8 1.57(2) yes C7 O7 1.410(10) yes C8 C9 1.54(2) yes C8 C19 1.53(2) yes C9 C10 1.56(2) yes C9 O9 1.200(10) yes C10 C11 1.520(10) yes C10 O10 1.400(10) yes C11 C12 1.32(2) yes C11 C15 1.55(2) yes C12 C13 1.51(2) yes C12 C18 1.58(2) yes C13 C14 1.55(2) yes C13 O13 1.37(2) yes C15 C16 1.53(2) yes C15 C17 1.51(2) yes C20 O2 1.440(10) yes O7 Si 1.660(10) yes Si C21 1.850(10) yes Si C23 1.850(10) yes Si C25 1.860(10) yes C21 C22 1.45(2) yes C23 C24 1.45(4) yes C25 C26 1.45(3) yes 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_publ_flag C15 C1 C2 C3 -59.3(11) yes C1 C2 C3 C8 109.7(12) yes C2 C3 C8 C9 -77.7(11) yes C3 C8 C9 C10 -27.4(9) yes C8 C9 C10 C11 53.4(10) yes C9 C10 C11 C15 49.8(10) yes C10 C11 C15 C1 -115.7(11) yes C11 C15 C1 C2 65.1(10) yes C14 C1 C15 C11 -62.8(11) yes C1 C15 C11 C12 49.7(10) yes C15 C11 C12 C13 -6.3(11) yes C11 C12 C13 C14 -20.9(12) yes C12 C13 C14 C1 1.7(11) yes C13 C14 C1 C15 39.9(11) yes C3 C2 O2 C20 21.0(10) yes C2 O2 C20 C4 -36.5(11) yes O2 C20 C4 C3 35.8(11) yes C20 C4 C3 C2 -22.7(10) yes C4 C3 C2 O2 2.0(10) yes C8 C3 C4 C5 -29.7(10) yes C3 C4 C5 C6 25.1(11) yes C4 C5 C6 C7 -43.4(12) yes C5 C6 C7 C8 65.7(12) yes C6 C7 C8 C3 -63.8(11) yes C7 C8 C3 C4 46.9(10) yes C20 C4 C5 O5 26.2(11) yes O4 C4 C5 O5 -96.9(12) yes