# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'RajanBabu, T. V.' 'Gong, Wei' 'Singidi, Ramakrishna' 'Gallucci, Judith' _publ_contact_author_name 'Gallucci, Judith C.' _publ_contact_author_address ;Department of Chemistry The Ohio State University 100 West 18th Avenue Columbus, OH 43210 USA ; _publ_contact_author_email gallucci.1@osu.edu _publ_section_title ; On the Stereochemistry of Acetylide Additions to Highly Functionalized Biphenylcarboxaldehydes and Multi-component Cycliztions of 1,n-Diynes. Syntheses of Dibenzocyclooctadiene Lignans ; _publ_requested_category FO data_RajanBabu1635 _database_code_depnum_ccdc_archive 'CCDC 689830' _audit_creation_date 2008-04-09T14:16:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'RajanBabu 1635' _chemical_formula_moiety 'C35 H41 B1 O7' _chemical_formula_sum 'C35 H41 B O7' _chemical_formula_weight 584.49 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0671(1) _cell_length_b 12.5459(1) _cell_length_c 15.4229(2) _cell_angle_alpha 83.045(1) _cell_angle_beta 83.617(1) _cell_angle_gamma 81.899(1) _cell_volume 1526.94(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5345 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_special_details ;All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 4.0, which means that 90% of the reflections were measured at least 4.0 times. Phi and omega scans with a frame width of one degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.106575 _diffrn_orient_matrix_ub_12 0.668118E-1 _diffrn_orient_matrix_ub_13 -0.7053E-3 _diffrn_orient_matrix_ub_21 -0.54026E-2 _diffrn_orient_matrix_ub_22 -0.275151E-1 _diffrn_orient_matrix_ub_23 0.759671E-1 _diffrn_orient_matrix_ub_31 0.391859E-1 _diffrn_orient_matrix_ub_32 0.508219E-1 _diffrn_orient_matrix_ub_33 0.0137 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 39388 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5373 _reflns_number_gt 4532 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;The methyl group hydrogen atoms are included in the model at calculated positions using a riding model with U(H) = 1.5*Ueq(bonded carbon atom). The torsion angle, which defines the orientation of the methyl group about the C-C or the O-C bond, was refined. The hydrogen atoms bonded to atoms C(28) and C(29) were refined isotropically. The remaining hydrogen atoms are included in the model at calculated positions using a riding model with U(H) = 1.2*Ueq(bonded carbon atom). 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 'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.4503P] 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_number_reflns 5373 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.165 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.037 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.18777(15) 0.78696(10) 0.16791(8) 0.0194(3) Uani 1 1 d . . . C2 C 0.25985(15) 0.88401(10) 0.15907(8) 0.0204(3) Uani 1 1 d . . . C3 C 0.40028(16) 0.89468(11) 0.09936(8) 0.0233(3) Uani 1 1 d . . . H3 H 0.4474 0.9608 0.0918 0.028 Uiso 1 1 calc R . . C4 C 0.47356(16) 0.81156(11) 0.05060(9) 0.0245(3) Uani 1 1 d . . . H4 H 0.5712 0.8204 0.0113 0.029 Uiso 1 1 calc R . . C5 C 0.40360(16) 0.71530(10) 0.05939(8) 0.0213(3) Uani 1 1 d . . . C6 C 0.25941(16) 0.70465(10) 0.11752(8) 0.0200(3) Uani 1 1 d . . . C7 C 0.03154(15) 0.77244(10) 0.22762(8) 0.0194(3) Uani 1 1 d . . . C8 C 0.03789(15) 0.69670(10) 0.30153(8) 0.0207(3) Uani 1 1 d . . . C9 C -0.10588(16) 0.68424(10) 0.35981(8) 0.0231(3) Uani 1 1 d . . . C10 C -0.25739(17) 0.74496(11) 0.34089(9) 0.0271(3) Uani 1 1 d . . . H10 H -0.3565 0.7359 0.379 0.032 Uiso 1 1 calc R . . C11 C -0.26444(16) 0.81889(11) 0.26653(9) 0.0260(3) Uani 1 1 d . . . H11 H -0.3694 0.8592 0.254 0.031 Uiso 1 1 calc R . . C12 C -0.12189(16) 0.83556(10) 0.20991(8) 0.0215(3) Uani 1 1 d . . . C13 C 0.61215(17) 0.63458(12) -0.04345(9) 0.0293(3) Uani 1 1 d . . . H13A H 0.5918 0.6945 -0.0896 0.044 Uiso 1 1 calc R . . H13B H 0.6431 0.5666 -0.07 0.044 Uiso 1 1 calc R . . H13C H 0.7039 0.6473 -0.0109 0.044 Uiso 1 1 calc R . . C14 C 0.08194(19) 0.61114(12) 0.05524(10) 0.0334(3) Uani 1 1 d . . . H14A H -0.0133 0.6685 0.0612 0.05 Uiso 1 1 calc R . . H14B H 0.0399 0.541 0.0588 0.05 Uiso 1 1 calc R . . H14C H 0.1471 0.6248 -0.0016 0.05 Uiso 1 1 calc R . . C15 C 0.2887(2) 0.68055(14) 0.36763(11) 0.0416(4) Uani 1 1 d . . . H15A H 0.3244 0.7456 0.333 0.062 Uiso 1 1 calc R . . H15B H 0.388 0.6292 0.3814 0.062 Uiso 1 1 calc R . . H15C H 0.2243 0.7005 0.4223 0.062 Uiso 1 1 calc R . . C16 C -0.22065(19) 0.60587(13) 0.49867(9) 0.0347(3) Uani 1 1 d . . . H16A H -0.2544 0.6772 0.5195 0.052 Uiso 1 1 calc R . . H16B H -0.1871 0.5531 0.5478 0.052 Uiso 1 1 calc R . . H16C H -0.3154 0.5834 0.4739 0.052 Uiso 1 1 calc R . . C17 C 0.18520(15) 0.97798(10) 0.21055(8) 0.0214(3) Uani 1 1 d . . . H17 H 0.124 0.9498 0.2667 0.026 Uiso 1 1 calc R . . C18 C 0.06296(16) 1.05769(10) 0.15719(8) 0.0223(3) Uani 1 1 d . . . C19 C -0.11185(16) 1.03301(11) 0.15621(8) 0.0227(3) Uani 1 1 d . . . C20 C -0.13426(16) 0.92211(10) 0.13217(8) 0.0234(3) Uani 1 1 d . . . H20A H -0.2455 0.9262 0.1097 0.028 Uiso 1 1 calc R . . H20B H -0.0469 0.9014 0.0847 0.028 Uiso 1 1 calc R . . C21 C 0.27947(19) 1.10375(11) 0.29390(9) 0.0291(3) Uani 1 1 d . . . H21A H 0.1706 1.1473 0.282 0.035 Uiso 1 1 calc R . . H21B H 0.3655 1.1539 0.2876 0.035 Uiso 1 1 calc R . . C22 C 0.26528(17) 1.05121(11) 0.38708(9) 0.0292(3) Uani 1 1 d . . . C23 C 0.1595(2) 1.10318(13) 0.45078(10) 0.0388(4) Uani 1 1 d . . . H23 H 0.0915 1.1691 0.4343 0.047 Uiso 1 1 calc R . . C24 C 0.1518(2) 1.06031(15) 0.53769(11) 0.0491(5) Uani 1 1 d . . . H24 H 0.0802 1.0974 0.5806 0.059 Uiso 1 1 calc R . . C25 C 0.2473(3) 0.96409(16) 0.56223(11) 0.0533(5) Uani 1 1 d . . . H25 H 0.2421 0.9346 0.622 0.064 Uiso 1 1 calc R . . C26 C 0.3506(3) 0.91079(15) 0.49975(12) 0.0524(5) Uani 1 1 d . . . H26 H 0.4151 0.8435 0.5163 0.063 Uiso 1 1 calc R . . C27 C 0.3608(2) 0.95463(13) 0.41309(11) 0.0408(4) Uani 1 1 d . . . H27 H 0.4346 0.9179 0.3707 0.049 Uiso 1 1 calc R . . C28 C 0.1129(2) 1.14533(12) 0.11023(9) 0.0297(3) Uani 1 1 d . . . H1A H 0.226(2) 1.1641(13) 0.1140(10) 0.037(4) Uiso 1 1 d . . . H1B H 0.033(2) 1.1944(13) 0.0725(11) 0.040(4) Uiso 1 1 d . . . C29 C -0.24442(18) 1.10690(11) 0.17515(9) 0.0274(3) Uani 1 1 d . . . HC29 H -0.354(2) 1.0883(12) 0.1674(10) 0.031(4) Uiso 1 1 d . . . C30 C -0.1679(2) 1.35036(11) 0.28144(10) 0.0332(3) Uani 1 1 d . . . C31 C -0.3388(2) 1.38889(12) 0.24390(10) 0.0354(4) Uani 1 1 d . . . C32 C -0.0192(2) 1.39412(14) 0.22630(15) 0.0566(5) Uani 1 1 d . . . H32A H 0.0858 1.3555 0.247 0.085 Uiso 1 1 calc R . . H32B H -0.0242 1.4716 0.2317 0.085 Uiso 1 1 calc R . . H32C H -0.0234 1.3835 0.1647 0.085 Uiso 1 1 calc R . . C33 C -0.1640(3) 1.36713(15) 0.37612(12) 0.0605(6) Uani 1 1 d . . . H33A H -0.2458 1.3262 0.4127 0.091 Uiso 1 1 calc R . . H33B H -0.1924 1.4443 0.3832 0.091 Uiso 1 1 calc R . . H33C H -0.0511 1.3418 0.3941 0.091 Uiso 1 1 calc R . . C34 C -0.3526(3) 1.50121(14) 0.19371(13) 0.0566(5) Uani 1 1 d . . . H34A H -0.27 1.5015 0.1421 0.085 Uiso 1 1 calc R . . H34B H -0.3308 1.5538 0.2318 0.085 Uiso 1 1 calc R . . H34C H -0.4661 1.5207 0.1749 0.085 Uiso 1 1 calc R . . C35 C -0.4895(2) 1.37923(16) 0.31119(15) 0.0618(6) Uani 1 1 d . . . H35A H -0.5928 1.393 0.2815 0.093 Uiso 1 1 calc R . . H35B H -0.4929 1.4323 0.3532 0.093 Uiso 1 1 calc R . . H35C H -0.4801 1.3061 0.3424 0.093 Uiso 1 1 calc R . . B B -0.2412(2) 1.21740(13) 0.20994(10) 0.0267(3) Uani 1 1 d . . . O1 O 0.46276(11) 0.62784(7) 0.01525(6) 0.0262(2) Uani 1 1 d . . . O2 O 0.18694(11) 0.60981(7) 0.12419(6) 0.0228(2) Uani 1 1 d . . . O3 O 0.18646(11) 0.63174(7) 0.31873(6) 0.0253(2) Uani 1 1 d . . . O4 O -0.08234(12) 0.61153(8) 0.43274(6) 0.0295(2) Uani 1 1 d . . . O5 O 0.32367(11) 1.02827(7) 0.22953(6) 0.0261(2) Uani 1 1 d . . . O6 O -0.14620(13) 1.23368(7) 0.27391(6) 0.0314(2) Uani 1 1 d . . . O7 O -0.34452(14) 1.30854(8) 0.18320(7) 0.0410(3) 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 0.0186(6) 0.0216(7) 0.0178(6) -0.0015(5) -0.0018(5) -0.0026(5) C2 0.0193(6) 0.0219(7) 0.0204(6) -0.0039(5) -0.0019(5) -0.0027(5) C3 0.0226(7) 0.0222(7) 0.0259(7) -0.0039(5) 0.0006(5) -0.0069(5) C4 0.0214(7) 0.0274(7) 0.0247(7) -0.0052(6) 0.0046(5) -0.0062(5) C5 0.0222(7) 0.0212(7) 0.0205(6) -0.0056(5) -0.0008(5) -0.0008(5) C6 0.0210(6) 0.0187(6) 0.0206(6) -0.0010(5) -0.0026(5) -0.0037(5) C7 0.0195(6) 0.0192(6) 0.0213(6) -0.0077(5) 0.0004(5) -0.0056(5) C8 0.0197(6) 0.0192(6) 0.0238(7) -0.0074(5) -0.0005(5) -0.0023(5) C9 0.0266(7) 0.0212(7) 0.0225(7) -0.0044(5) 0.0014(5) -0.0074(5) C10 0.0206(7) 0.0320(8) 0.0287(7) -0.0064(6) 0.0062(5) -0.0075(6) C11 0.0187(6) 0.0289(7) 0.0306(7) -0.0070(6) -0.0011(5) -0.0018(5) C12 0.0219(7) 0.0212(7) 0.0232(7) -0.0075(5) -0.0017(5) -0.0042(5) C13 0.0251(7) 0.0304(8) 0.0321(8) -0.0116(6) 0.0077(6) -0.0036(6) C14 0.0369(8) 0.0342(8) 0.0332(8) -0.0050(6) -0.0083(6) -0.0134(7) C15 0.0355(9) 0.0445(10) 0.0474(10) -0.0044(8) -0.0186(7) -0.0035(7) C16 0.0373(8) 0.0379(8) 0.0273(8) -0.0025(6) 0.0103(6) -0.0106(7) C17 0.0199(6) 0.0236(7) 0.0222(7) -0.0061(5) 0.0011(5) -0.0073(5) C18 0.0263(7) 0.0219(7) 0.0186(6) -0.0073(5) 0.0034(5) -0.0032(5) C19 0.0270(7) 0.0235(7) 0.0177(6) -0.0020(5) -0.0036(5) -0.0024(5) C20 0.0216(7) 0.0250(7) 0.0244(7) -0.0052(6) -0.0041(5) -0.0019(5) C21 0.0348(8) 0.0258(7) 0.0294(7) -0.0111(6) -0.0018(6) -0.0072(6) C22 0.0300(8) 0.0304(8) 0.0307(8) -0.0107(6) -0.0036(6) -0.0088(6) C23 0.0403(9) 0.0370(9) 0.0412(9) -0.0117(7) 0.0015(7) -0.0094(7) C24 0.0602(11) 0.0568(12) 0.0356(9) -0.0180(8) 0.0114(8) -0.0273(9) C25 0.0754(13) 0.0588(12) 0.0320(9) 0.0005(8) -0.0078(9) -0.0330(10) C26 0.0665(12) 0.0448(10) 0.0466(11) 0.0026(8) -0.0164(9) -0.0076(9) C27 0.0439(9) 0.0390(9) 0.0394(9) -0.0083(7) -0.0043(7) -0.0007(7) C28 0.0345(8) 0.0275(8) 0.0260(7) -0.0033(6) 0.0039(6) -0.0049(6) C29 0.0260(7) 0.0284(8) 0.0282(7) -0.0039(6) -0.0062(6) -0.0015(6) C30 0.0444(9) 0.0210(7) 0.0354(8) -0.0058(6) -0.0067(7) -0.0030(6) C31 0.0434(9) 0.0244(7) 0.0385(8) -0.0117(6) -0.0050(7) 0.0036(6) C32 0.0498(11) 0.0346(9) 0.0870(15) -0.0102(9) 0.0026(10) -0.0146(8) C33 0.1041(17) 0.0352(10) 0.0477(11) -0.0135(8) -0.0282(11) -0.0037(10) C34 0.0823(14) 0.0292(9) 0.0566(11) -0.0052(8) -0.0217(10) 0.0108(9) C35 0.0496(11) 0.0505(11) 0.0854(15) -0.0325(11) 0.0183(10) -0.0049(9) B 0.0262(8) 0.0267(8) 0.0258(8) -0.0023(6) -0.0001(6) -0.0012(6) O1 0.0260(5) 0.0232(5) 0.0288(5) -0.0094(4) 0.0085(4) -0.0044(4) O2 0.0254(5) 0.0197(5) 0.0243(5) -0.0038(4) -0.0011(4) -0.0062(4) O3 0.0220(5) 0.0243(5) 0.0290(5) -0.0026(4) -0.0026(4) -0.0009(4) O4 0.0302(5) 0.0307(5) 0.0250(5) 0.0022(4) 0.0058(4) -0.0059(4) O5 0.0234(5) 0.0292(5) 0.0286(5) -0.0119(4) 0.0011(4) -0.0091(4) O6 0.0406(6) 0.0210(5) 0.0337(5) -0.0052(4) -0.0103(4) -0.0010(4) O7 0.0496(7) 0.0293(6) 0.0456(6) -0.0139(5) -0.0202(5) 0.0104(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C6 1.3894(18) . ? C1 C2 1.4075(18) . ? C1 C7 1.4952(17) . ? C2 C3 1.3893(18) . ? C2 C17 1.5177(18) . ? C3 C4 1.3855(18) . ? C3 H3 0.95 . ? C4 C5 1.3896(19) . ? C4 H4 0.95 . ? C5 O1 1.3623(15) . ? C5 C6 1.3992(18) . ? C6 O2 1.3860(15) . ? C7 C8 1.3936(18) . ? C7 C12 1.4072(18) . ? C8 O3 1.3835(15) . ? C8 C9 1.4009(18) . ? C9 O4 1.3725(16) . ? C9 C10 1.3865(19) . ? C10 C11 1.3859(19) . ? C10 H10 0.95 . ? C11 C12 1.3890(18) . ? C11 H11 0.95 . ? C12 C20 1.5189(18) . ? C13 O1 1.4306(15) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 O2 1.4285(16) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 O3 1.4200(18) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 O4 1.4270(16) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 O5 1.4310(15) . ? C17 C18 1.5340(19) . ? C17 H17 1 . ? C18 C28 1.3278(19) . ? C18 C19 1.4878(19) . ? C19 C29 1.3436(19) . ? C19 C20 1.5221(18) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 O5 1.4364(16) . ? C21 C22 1.506(2) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 C27 1.382(2) . ? C22 C23 1.390(2) . ? C23 C24 1.381(2) . ? C23 H23 0.95 . ? C24 C25 1.373(3) . ? C24 H24 0.95 . ? C25 C26 1.375(3) . ? C25 H25 0.95 . ? C26 C27 1.381(2) . ? C26 H26 0.95 . ? C27 H27 0.95 . ? C28 H1A 0.981(17) . ? C28 H1B 1.011(17) . ? C29 B 1.550(2) . ? C29 HC29 0.966(16) . ? C30 O6 1.4668(17) . ? C30 C33 1.505(2) . ? C30 C32 1.519(2) . ? C30 C31 1.547(2) . ? C31 O7 1.4648(18) . ? C31 C35 1.517(2) . ? C31 C34 1.519(2) . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? B O6 1.3652(19) . ? B O7 1.3659(19) . ? 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 C6 C1 C2 119.31(11) . . ? C6 C1 C7 119.32(11) . . ? C2 C1 C7 121.32(11) . . ? C3 C2 C1 118.66(12) . . ? C3 C2 C17 119.42(11) . . ? C1 C2 C17 121.89(11) . . ? C4 C3 C2 121.86(12) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 119.74(12) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? O1 C5 C4 125.56(11) . . ? O1 C5 C6 115.50(11) . . ? C4 C5 C6 118.94(12) . . ? O2 C6 C1 119.73(11) . . ? O2 C6 C5 118.82(11) . . ? C1 C6 C5 121.44(11) . . ? C8 C7 C12 119.76(11) . . ? C8 C7 C1 119.95(11) . . ? C12 C7 C1 120.29(11) . . ? O3 C8 C7 120.63(11) . . ? O3 C8 C9 118.52(11) . . ? C7 C8 C9 120.85(11) . . ? O4 C9 C10 125.34(11) . . ? O4 C9 C8 115.63(11) . . ? C10 C9 C8 119.03(12) . . ? C11 C10 C9 120.11(12) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 121.67(12) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C7 118.50(12) . . ? C11 C12 C20 119.65(11) . . ? C7 C12 C20 121.84(11) . . ? O1 C13 H13A 109.5 . . ? O1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O4 C16 H16A 109.5 . . ? O4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 C2 106.51(10) . . ? O5 C17 C18 111.47(10) . . ? C2 C17 C18 110.55(10) . . ? O5 C17 H17 109.4 . . ? C2 C17 H17 109.4 . . ? C18 C17 H17 109.4 . . ? C28 C18 C19 120.27(13) . . ? C28 C18 C17 120.95(13) . . ? C19 C18 C17 118.74(11) . . ? C29 C19 C18 120.76(12) . . ? C29 C19 C20 121.59(12) . . ? C18 C19 C20 117.64(11) . . ? C12 C20 C19 112.24(10) . . ? C12 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? C12 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? O5 C21 C22 113.92(11) . . ? O5 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? O5 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C27 C22 C23 118.06(14) . . ? C27 C22 C21 122.23(13) . . ? C23 C22 C21 119.63(13) . . ? C24 C23 C22 120.93(16) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C25 C24 C23 120.15(16) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.61(16) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 120.28(17) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C22 120.95(16) . . ? C26 C27 H27 119.5 . . ? C22 C27 H27 119.5 . . ? C18 C28 H1A 120.1(9) . . ? C18 C28 H1B 119.7(9) . . ? H1A C28 H1B 120.1(13) . . ? C19 C29 B 127.05(13) . . ? C19 C29 HC29 116.3(9) . . ? B C29 HC29 116.7(9) . . ? O6 C30 C33 108.69(12) . . ? O6 C30 C32 106.10(12) . . ? C33 C30 C32 110.04(15) . . ? O6 C30 C31 102.28(11) . . ? C33 C30 C31 114.94(14) . . ? C32 C30 C31 114.00(14) . . ? O7 C31 C35 105.99(13) . . ? O7 C31 C34 109.25(13) . . ? C35 C31 C34 110.26(15) . . ? O7 C31 C30 102.06(11) . . ? C35 C31 C30 113.78(14) . . ? C34 C31 C30 114.74(14) . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O6 B O7 112.47(13) . . ? O6 B C29 124.88(13) . . ? O7 B C29 122.50(13) . . ? C5 O1 C13 117.24(10) . . ? C6 O2 C14 111.31(10) . . ? C8 O3 C15 113.02(10) . . ? C9 O4 C16 117.30(11) . . ? C17 O5 C21 113.76(10) . . ? B O6 C30 107.47(11) . . ? B O7 C31 107.69(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.52(18) . . . . ? C7 C1 C2 C3 -176.88(11) . . . . ? C6 C1 C2 C17 178.50(11) . . . . ? C7 C1 C2 C17 1.10(18) . . . . ? C1 C2 C3 C4 -1.95(19) . . . . ? C17 C2 C3 C4 -179.98(12) . . . . ? C2 C3 C4 C5 1.6(2) . . . . ? C3 C4 C5 O1 179.77(12) . . . . ? C3 C4 C5 C6 0.20(19) . . . . ? C2 C1 C6 O2 -178.43(11) . . . . ? C7 C1 C6 O2 -0.98(17) . . . . ? C2 C1 C6 C5 1.24(18) . . . . ? C7 C1 C6 C5 178.70(11) . . . . ? O1 C5 C6 O2 -1.55(17) . . . . ? C4 C5 C6 O2 178.06(11) . . . . ? O1 C5 C6 C1 178.78(11) . . . . ? C4 C5 C6 C1 -1.61(19) . . . . ? C6 C1 C7 C8 68.79(16) . . . . ? C2 C1 C7 C8 -113.81(14) . . . . ? C6 C1 C7 C12 -111.70(14) . . . . ? C2 C1 C7 C12 65.70(16) . . . . ? C12 C7 C8 O3 178.16(11) . . . . ? C1 C7 C8 O3 -2.33(18) . . . . ? C12 C7 C8 C9 -1.54(18) . . . . ? C1 C7 C8 C9 177.97(11) . . . . ? O3 C8 C9 O4 3.78(17) . . . . ? C7 C8 C9 O4 -176.51(11) . . . . ? O3 C8 C9 C10 -176.74(11) . . . . ? C7 C8 C9 C10 2.96(19) . . . . ? O4 C9 C10 C11 177.66(12) . . . . ? C8 C9 C10 C11 -1.8(2) . . . . ? C9 C10 C11 C12 -0.9(2) . . . . ? C10 C11 C12 C7 2.31(19) . . . . ? C10 C11 C12 C20 -176.47(12) . . . . ? C8 C7 C12 C11 -1.08(18) . . . . ? C1 C7 C12 C11 179.41(11) . . . . ? C8 C7 C12 C20 177.67(11) . . . . ? C1 C7 C12 C20 -1.84(18) . . . . ? C3 C2 C17 O5 -36.39(15) . . . . ? C1 C2 C17 O5 145.65(11) . . . . ? C3 C2 C17 C18 84.87(14) . . . . ? C1 C2 C17 C18 -93.09(14) . . . . ? O5 C17 C18 C28 22.07(17) . . . . ? C2 C17 C18 C28 -96.19(14) . . . . ? O5 C17 C18 C19 -160.18(10) . . . . ? C2 C17 C18 C19 81.55(14) . . . . ? C28 C18 C19 C29 -53.88(18) . . . . ? C17 C18 C19 C29 128.37(13) . . . . ? C28 C18 C19 C20 125.50(14) . . . . ? C17 C18 C19 C20 -52.26(16) . . . . ? C11 C12 C20 C19 86.71(14) . . . . ? C7 C12 C20 C19 -92.03(14) . . . . ? C29 C19 C20 C12 -98.05(14) . . . . ? C18 C19 C20 C12 82.59(14) . . . . ? O5 C21 C22 C27 30.72(19) . . . . ? O5 C21 C22 C23 -152.62(13) . . . . ? C27 C22 C23 C24 0.9(2) . . . . ? C21 C22 C23 C24 -175.93(14) . . . . ? C22 C23 C24 C25 -1.1(2) . . . . ? C23 C24 C25 C26 0.0(3) . . . . ? C24 C25 C26 C27 1.3(3) . . . . ? C25 C26 C27 C22 -1.5(3) . . . . ? C23 C22 C27 C26 0.4(2) . . . . ? C21 C22 C27 C26 177.10(15) . . . . ? C18 C19 C29 B -7.6(2) . . . . ? C20 C19 C29 B 173.04(12) . . . . ? O6 C30 C31 O7 -27.63(14) . . . . ? C33 C30 C31 O7 -145.21(13) . . . . ? C32 C30 C31 O7 86.43(15) . . . . ? O6 C30 C31 C35 86.06(15) . . . . ? C33 C30 C31 C35 -31.51(19) . . . . ? C32 C30 C31 C35 -159.88(14) . . . . ? O6 C30 C31 C34 -145.65(13) . . . . ? C33 C30 C31 C34 96.78(17) . . . . ? C32 C30 C31 C34 -31.59(19) . . . . ? C19 C29 B O6 -42.9(2) . . . . ? C19 C29 B O7 141.87(15) . . . . ? C4 C5 O1 C13 1.73(19) . . . . ? C6 C5 O1 C13 -178.69(11) . . . . ? C1 C6 O2 C14 97.98(14) . . . . ? C5 C6 O2 C14 -81.70(14) . . . . ? C7 C8 O3 C15 87.31(15) . . . . ? C9 C8 O3 C15 -92.99(14) . . . . ? C10 C9 O4 C16 -6.66(19) . . . . ? C8 C9 O4 C16 172.78(11) . . . . ? C2 C17 O5 C21 -167.15(10) . . . . ? C18 C17 O5 C21 72.18(13) . . . . ? C22 C21 O5 C17 79.52(14) . . . . ? O7 B O6 C30 -9.52(16) . . . . ? C29 B O6 C30 174.87(13) . . . . ? C33 C30 O6 B 145.15(15) . . . . ? C32 C30 O6 B -96.55(15) . . . . ? C31 C30 O6 B 23.20(14) . . . . ? O6 B O7 C31 -9.69(17) . . . . ? C29 B O7 C31 166.04(13) . . . . ? C35 C31 O7 B -96.08(15) . . . . ? C34 C31 O7 B 145.14(14) . . . . ? C30 C31 O7 B 23.27(15) . . . . ? #END OF CIF # Attachment '- ._15.archive.cif' #Mac OS X 2 R TEXTttxt # Attachment '- ._16 archive.cif' #Mac OS X 2 R TEXTttxt # Attachment '- ._21A archive.cif' #Mac OS X 2 R TEXTttxt # Attachment '- ._38 archive.cif' #Mac OS X 2 R TEXTttxt # Attachment '- ._49 archive.cif' #Mac OS X 2 R TEXTttxt # Attachment '- 15.archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-05-05 at 16:13:21 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : shelxl dreduc import struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# #TrackingRef '- 15.archive.cif' data_RajanBabu1762 _database_code_depnum_ccdc_archive 'CCDC 854082' #TrackingRef '- 15.archive.cif' _audit_creation_date 2011-05-05T16:13:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'RajanBabu 1762' _chemical_formula_moiety 'C28 H35 N1 O7 Si1' _chemical_formula_sum 'C28 H35 N O7 Si' _chemical_formula_weight 525.66 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.4194(1) _cell_length_b 10.9563(1) _cell_length_c 12.2162(1) _cell_angle_alpha 90 _cell_angle_beta 104.877(1) _cell_angle_gamma 90 _cell_volume 1477.19(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3563 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_special_details ;All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.3, which means that 90% of these reflections were measured at least 3.3 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.684225E-1 _diffrn_orient_matrix_ub_12 0.561054E-1 _diffrn_orient_matrix_ub_13 0.22236E-2 _diffrn_orient_matrix_ub_21 0.10018E-2 _diffrn_orient_matrix_ub_22 0.327975E-1 _diffrn_orient_matrix_ub_23 -0.761451E-1 _diffrn_orient_matrix_ub_31 -0.593891E-1 _diffrn_orient_matrix_ub_32 -0.640861E-1 _diffrn_orient_matrix_ub_33 -0.370223E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 43607 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 6764 _reflns_number_gt 5446 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded carbon atom). The torsion angle, which defines the orientation of the methyl group about the O-C, N-C, or Si-C bond, was refined. The hydroxyl hydrogen atom bonded to atom O(3) was refined isotropically. The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+0.1577P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6764 _refine_ls_number_parameters 346 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(13) _refine_diff_density_max 0.298 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.13601(15) 0.88515(16) 0.76583(14) 0.0283(4) Uani 1 1 d . . . C2 C 0.21121(16) 0.84615(17) 0.69845(14) 0.0301(4) Uani 1 1 d . . . C3 C 0.19127(17) 0.88768(19) 0.58603(15) 0.0351(4) Uani 1 1 d . . . H3 H 0.2419 0.8622 0.5396 0.042 Uiso 1 1 calc R . . C4 C 0.09743(17) 0.96526(19) 0.54633(15) 0.0358(4) Uani 1 1 d . . . C5 C 0.02344(17) 1.00447(19) 0.61270(15) 0.0357(4) Uani 1 1 d . . . C6 C 0.04068(16) 0.96665(18) 0.72312(14) 0.0331(4) Uani 1 1 d . . . H6 H -0.01 0.9947 0.7686 0.04 Uiso 1 1 calc R . . C7 C -0.0416(2) 1.0905(3) 0.44259(19) 0.0657(8) Uani 1 1 d . . . H7A H -0.114 1.0629 0.3843 0.079 Uiso 1 1 calc R . . H7B H -0.0246 1.1762 0.4261 0.079 Uiso 1 1 calc R . . C8 C 0.32199(17) 0.76932(19) 0.74872(16) 0.0375(4) Uani 1 1 d . . . H8 H 0.307 0.7213 0.8134 0.045 Uiso 1 1 calc R . . C9 C 0.35105(18) 0.68388(19) 0.66655(16) 0.0388(4) Uani 1 1 d . . . C10 C 0.3718(2) 0.6143(2) 0.59814(19) 0.0483(5) Uani 1 1 d . . . C11 C 0.3014(4) 0.3695(5) 0.4853(5) 0.154(2) Uani 1 1 d . . . H11A H 0.2271 0.3913 0.4282 0.232 Uiso 1 1 calc R . . H11B H 0.2823 0.353 0.5576 0.232 Uiso 1 1 calc R . . H11C H 0.3371 0.2964 0.4606 0.232 Uiso 1 1 calc R . . C12 C 0.4060(6) 0.5654(5) 0.3662(3) 0.168(3) Uani 1 1 d . . . H12A H 0.4728 0.6233 0.3723 0.252 Uiso 1 1 calc R . . H12B H 0.3286 0.608 0.3383 0.252 Uiso 1 1 calc R . . H12C H 0.4125 0.5001 0.3132 0.252 Uiso 1 1 calc R . . C13 C 0.5595(3) 0.4373(4) 0.5788(3) 0.0984(12) Uani 1 1 d . . . H13A H 0.5784 0.3667 0.5372 0.148 Uiso 1 1 calc R . . H13B H 0.5561 0.4118 0.6548 0.148 Uiso 1 1 calc R . . H13C H 0.6226 0.4995 0.5849 0.148 Uiso 1 1 calc R . . C14 C 0.14996(16) 0.83808(16) 0.88413(14) 0.0283(4) Uani 1 1 d . . . C15 C 0.20677(16) 0.90321(17) 0.98200(15) 0.0311(4) Uani 1 1 d . . . C16 C 0.19920(18) 0.86398(19) 1.08852(15) 0.0358(4) Uani 1 1 d . . . H16 H 0.2346 0.9118 1.1535 0.043 Uiso 1 1 calc R . . C17 C 0.14050(18) 0.75581(18) 1.10061(15) 0.0361(4) Uani 1 1 d . . . C18 C 0.09079(17) 0.68522(17) 1.00511(15) 0.0315(4) Uani 1 1 d . . . C19 C 0.09277(16) 0.72787(16) 0.89799(14) 0.0294(4) Uani 1 1 d . . . C20 C 0.1391(3) 0.7973(3) 1.29005(19) 0.0810(10) Uani 1 1 d . . . H20A H 0.2241 0.8221 1.3168 0.121 Uiso 1 1 calc R . . H20B H 0.1127 0.7597 1.3525 0.121 Uiso 1 1 calc R . . H20C H 0.0889 0.8692 1.2627 0.121 Uiso 1 1 calc R . . C21 C 0.1120(2) 0.47448(19) 1.0192(2) 0.0582(6) Uani 1 1 d . . . H21A H 0.1389 0.4722 0.9492 0.087 Uiso 1 1 calc R . . H21B H 0.0676 0.3994 1.0257 0.087 Uiso 1 1 calc R . . H21C H 0.1827 0.4813 1.0843 0.087 Uiso 1 1 calc R . . C22 C -0.09306(19) 0.6711(2) 0.77603(17) 0.0434(5) Uani 1 1 d . . . H22A H -0.1225 0.6459 0.8412 0.065 Uiso 1 1 calc R . . H22B H -0.1287 0.6184 0.7112 0.065 Uiso 1 1 calc R . . H22C H -0.1165 0.756 0.7567 0.065 Uiso 1 1 calc R . . C23 C 0.27773(16) 1.01448(18) 0.97660(14) 0.0340(4) Uani 1 1 d . . . C24 C 0.3985(2) 1.1582(2) 0.93715(18) 0.0453(5) Uani 1 1 d . . . H24 H 0.4885 1.1493 0.9549 0.054 Uiso 1 1 calc R . . C25 C 0.3632(3) 1.1920(3) 1.0470(2) 0.0676(8) Uani 1 1 d . . . H25A H 0.4351 1.1915 1.1127 0.081 Uiso 1 1 calc R . . H25B H 0.3251 1.2737 1.0406 0.081 Uiso 1 1 calc R . . C26 C 0.3582(2) 1.2467(2) 0.8387(2) 0.0582(6) Uani 1 1 d . . . H26 H 0.3855 1.2119 0.7737 0.07 Uiso 1 1 calc R . . C27 C 0.2243(3) 1.2631(3) 0.7991(3) 0.0942(11) Uani 1 1 d . . . H27A H 0.1858 1.1839 0.7761 0.141 Uiso 1 1 calc R . . H27B H 0.2052 1.3192 0.7345 0.141 Uiso 1 1 calc R . . H27C H 0.1938 1.2969 0.8608 0.141 Uiso 1 1 calc R . . C28 C 0.4227(3) 1.3701(3) 0.8678(3) 0.0746(8) Uani 1 1 d . . . H28A H 0.3932 1.4106 0.9271 0.112 Uiso 1 1 calc R . . H28B H 0.4059 1.4217 0.8 0.112 Uiso 1 1 calc R . . H28C H 0.5103 1.3567 0.8949 0.112 Uiso 1 1 calc R . . N N 0.34291(15) 1.03617(15) 0.90867(14) 0.0397(4) Uani 1 1 d . . . O1 O -0.06356(14) 1.08239(15) 0.55189(11) 0.0510(4) Uani 1 1 d . . . O2 O 0.05904(14) 1.01598(16) 0.44006(11) 0.0528(4) Uani 1 1 d . . . O3 O 0.42529(13) 0.84608(16) 0.79055(14) 0.0504(4) Uani 1 1 d . . . H1O3 H 0.401(2) 0.900(2) 0.826(2) 0.049(7) Uiso 1 1 d . . . O4 O 0.12669(15) 0.71164(14) 1.20017(11) 0.0496(4) Uani 1 1 d . . . O5 O 0.03548(12) 0.57614(12) 1.01684(11) 0.0373(3) Uani 1 1 d . . . O6 O 0.03699(11) 0.66069(12) 0.80387(10) 0.0343(3) Uani 1 1 d . . . O7 O 0.27786(14) 1.09809(13) 1.05830(12) 0.0484(4) Uani 1 1 d . . . Si Si 0.41341(8) 0.50069(8) 0.50342(6) 0.0693(2) 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 0.0312(9) 0.0290(9) 0.0249(8) -0.0005(7) 0.0077(7) -0.0034(7) C2 0.0325(9) 0.0321(9) 0.0268(8) 0.0007(7) 0.0100(7) -0.0014(8) C3 0.0392(10) 0.0399(11) 0.0295(9) 0.0010(8) 0.0149(8) 0.0046(8) C4 0.0438(10) 0.0413(11) 0.0242(8) 0.0067(8) 0.0123(7) 0.0072(8) C5 0.0380(10) 0.0389(10) 0.0305(8) 0.0034(8) 0.0096(7) 0.0103(8) C6 0.0348(9) 0.0398(11) 0.0280(9) 0.0000(7) 0.0139(7) 0.0040(8) C7 0.0720(16) 0.095(2) 0.0376(11) 0.0209(12) 0.0277(11) 0.0492(16) C8 0.0357(10) 0.0439(11) 0.0334(9) -0.0001(8) 0.0098(8) 0.0063(9) C9 0.0357(10) 0.0417(11) 0.0382(10) 0.0035(9) 0.0080(8) 0.0072(8) C10 0.0461(12) 0.0495(13) 0.0466(11) -0.0052(10) 0.0071(9) 0.0114(10) C11 0.098(3) 0.119(4) 0.225(6) -0.104(4) 0.003(3) 0.013(3) C12 0.315(7) 0.139(4) 0.065(2) 0.011(2) 0.075(3) 0.116(5) C13 0.078(2) 0.125(3) 0.094(2) -0.023(2) 0.0237(17) 0.046(2) C14 0.0291(8) 0.0286(9) 0.0273(8) 0.0003(7) 0.0075(7) 0.0009(7) C15 0.0350(9) 0.0319(9) 0.0267(8) -0.0011(7) 0.0086(7) -0.0033(8) C16 0.0437(11) 0.0393(11) 0.0240(8) -0.0021(7) 0.0078(7) -0.0074(8) C17 0.0462(11) 0.0364(10) 0.0268(9) 0.0026(8) 0.0113(8) -0.0032(9) C18 0.0398(10) 0.0277(9) 0.0286(9) 0.0028(7) 0.0118(7) -0.0010(7) C19 0.0353(9) 0.0279(9) 0.0261(8) -0.0023(7) 0.0097(7) 0.0008(7) C20 0.139(3) 0.083(2) 0.0291(11) -0.0124(12) 0.0365(14) -0.057(2) C21 0.0684(16) 0.0305(12) 0.0850(18) 0.0055(11) 0.0367(14) 0.0039(11) C22 0.0425(11) 0.0511(13) 0.0366(10) -0.0075(9) 0.0100(8) -0.0066(10) C23 0.0352(9) 0.0373(10) 0.0276(8) -0.0037(8) 0.0046(7) -0.0061(8) C24 0.0485(12) 0.0415(12) 0.0482(12) -0.0069(9) 0.0168(9) -0.0152(10) C25 0.0841(18) 0.0643(16) 0.0650(15) -0.0257(13) 0.0382(14) -0.0453(15) C26 0.0712(17) 0.0430(13) 0.0607(14) -0.0014(11) 0.0174(12) -0.0140(12) C27 0.090(2) 0.0540(17) 0.128(3) -0.0004(19) 0.010(2) 0.0012(17) C28 0.096(2) 0.0491(15) 0.0778(18) 0.0016(14) 0.0214(16) -0.0271(15) N 0.0448(9) 0.0358(9) 0.0427(9) -0.0021(7) 0.0188(7) -0.0110(7) O1 0.0597(9) 0.0660(10) 0.0302(7) 0.0139(7) 0.0167(6) 0.0324(8) O2 0.0680(10) 0.0655(10) 0.0299(7) 0.0169(7) 0.0217(7) 0.0336(9) O3 0.0335(8) 0.0562(10) 0.0572(9) -0.0167(8) 0.0039(7) 0.0065(7) O4 0.0779(11) 0.0478(9) 0.0245(6) 0.0016(6) 0.0157(7) -0.0163(8) O5 0.0473(8) 0.0290(7) 0.0385(7) 0.0025(5) 0.0167(6) -0.0040(6) O6 0.0409(7) 0.0352(7) 0.0284(6) -0.0067(5) 0.0118(5) -0.0070(6) O7 0.0630(9) 0.0447(9) 0.0425(8) -0.0157(7) 0.0229(7) -0.0239(7) Si 0.0806(5) 0.0693(5) 0.0519(4) -0.0177(3) 0.0060(3) 0.0360(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.400(2) . ? C1 C6 1.401(3) . ? C1 C14 1.504(2) . ? C2 C3 1.409(2) . ? C2 C8 1.512(3) . ? C3 C4 1.356(3) . ? C3 H3 0.95 . ? C4 O2 1.376(2) . ? C4 C5 1.381(3) . ? C5 O1 1.374(2) . ? C5 C6 1.376(2) . ? C6 H6 0.95 . ? C7 O2 1.416(3) . ? C7 O1 1.423(2) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 O3 1.432(3) . ? C8 C9 1.472(3) . ? C8 H8 1 . ? C9 C10 1.199(3) . ? C10 Si 1.843(2) . ? C11 Si 1.899(5) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 Si 1.803(4) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 Si 1.823(3) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C15 1.400(2) . ? C14 C19 1.404(2) . ? C15 C16 1.394(2) . ? C15 C23 1.475(3) . ? C16 C17 1.388(3) . ? C16 H16 0.95 . ? C17 O4 1.355(2) . ? C17 C18 1.393(3) . ? C18 O5 1.376(2) . ? C18 C19 1.395(2) . ? C19 O6 1.376(2) . ? C20 O4 1.424(3) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 O5 1.411(3) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 O6 1.440(2) . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 N 1.271(2) . ? C23 O7 1.355(2) . ? C24 N 1.482(3) . ? C24 C26 1.522(3) . ? C24 C25 1.541(3) . ? C24 H24 1 . ? C25 O7 1.448(3) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C27 1.492(5) . ? C26 C28 1.537(4) . ? C26 H26 1 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? O3 H1O3 0.82(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 C2 C1 C6 120.71(16) . . ? C2 C1 C14 122.05(16) . . ? C6 C1 C14 117.19(15) . . ? C1 C2 C3 120.30(17) . . ? C1 C2 C8 120.42(15) . . ? C3 C2 C8 118.99(15) . . ? C4 C3 C2 117.79(16) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 O2 128.43(17) . . ? C3 C4 C5 122.10(17) . . ? O2 C4 C5 109.48(16) . . ? O1 C5 C6 128.21(16) . . ? O1 C5 C4 110.01(15) . . ? C6 C5 C4 121.78(17) . . ? C5 C6 C1 117.32(16) . . ? C5 C6 H6 121.3 . . ? C1 C6 H6 121.3 . . ? O2 C7 O1 108.92(17) . . ? O2 C7 H7A 109.9 . . ? O1 C7 H7A 109.9 . . ? O2 C7 H7B 109.9 . . ? O1 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O3 C8 C9 107.92(16) . . ? O3 C8 C2 110.16(16) . . ? C9 C8 C2 112.87(16) . . ? O3 C8 H8 108.6 . . ? C9 C8 H8 108.6 . . ? C2 C8 H8 108.6 . . ? C10 C9 C8 178.4(2) . . ? C9 C10 Si 174.9(2) . . ? Si C11 H11A 109.5 . . ? Si C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si C12 H12A 109.5 . . ? Si C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si C13 H13A 109.5 . . ? Si C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 117.60(15) . . ? C15 C14 C1 123.86(15) . . ? C19 C14 C1 118.24(15) . . ? C16 C15 C14 120.91(16) . . ? C16 C15 C23 117.59(16) . . ? C14 C15 C23 121.50(15) . . ? C17 C16 C15 120.66(16) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? O4 C17 C16 124.82(17) . . ? O4 C17 C18 115.92(17) . . ? C16 C17 C18 119.27(16) . . ? O5 C18 C17 119.60(15) . . ? O5 C18 C19 120.46(16) . . ? C17 C18 C19 119.89(17) . . ? O6 C19 C18 119.28(15) . . ? O6 C19 C14 119.30(15) . . ? C18 C19 C14 121.42(16) . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O6 C22 H22A 109.5 . . ? O6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N C23 O7 117.68(17) . . ? N C23 C15 127.18(17) . . ? O7 C23 C15 115.01(15) . . ? N C24 C26 111.43(18) . . ? N C24 C25 103.25(17) . . ? C26 C24 C25 116.2(2) . . ? N C24 H24 108.6 . . ? C26 C24 H24 108.6 . . ? C25 C24 H24 108.6 . . ? O7 C25 C24 104.21(17) . . ? O7 C25 H25A 110.9 . . ? C24 C25 H25A 110.9 . . ? O7 C25 H25B 110.9 . . ? C24 C25 H25B 110.9 . . ? H25A C25 H25B 108.9 . . ? C27 C26 C24 114.1(2) . . ? C27 C26 C28 111.1(3) . . ? C24 C26 C28 110.4(2) . . ? C27 C26 H26 106.9 . . ? C24 C26 H26 106.9 . . ? C28 C26 H26 106.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C23 N C24 107.60(16) . . ? C5 O1 C7 105.58(15) . . ? C4 O2 C7 106.01(14) . . ? C8 O3 H1O3 104.8(17) . . ? C17 O4 C20 116.43(17) . . ? C18 O5 C21 112.90(14) . . ? C19 O6 C22 112.52(14) . . ? C23 O7 C25 106.45(16) . . ? C12 Si C13 116.0(2) . . ? C12 Si C10 111.12(16) . . ? C13 Si C10 106.87(13) . . ? C12 Si C11 108.7(3) . . ? C13 Si C11 105.8(2) . . ? C10 Si C11 108.06(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.6(3) . . . . ? C14 C1 C2 C3 176.74(17) . . . . ? C6 C1 C2 C8 173.29(17) . . . . ? C14 C1 C2 C8 -9.4(3) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C8 C2 C3 C4 -174.23(18) . . . . ? C2 C3 C4 O2 -178.8(2) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C3 C4 C5 O1 179.77(19) . . . . ? O2 C4 C5 O1 -0.7(2) . . . . ? C3 C4 C5 C6 -0.2(3) . . . . ? O2 C4 C5 C6 179.37(19) . . . . ? O1 C5 C6 C1 179.39(19) . . . . ? C4 C5 C6 C1 -0.7(3) . . . . ? C2 C1 C6 C5 1.0(3) . . . . ? C14 C1 C6 C5 -176.40(17) . . . . ? C1 C2 C8 O3 -90.7(2) . . . . ? C3 C2 C8 O3 83.2(2) . . . . ? C1 C2 C8 C9 148.60(18) . . . . ? C3 C2 C8 C9 -37.5(3) . . . . ? C2 C1 C14 C15 101.6(2) . . . . ? C6 C1 C14 C15 -81.0(2) . . . . ? C2 C1 C14 C19 -84.8(2) . . . . ? C6 C1 C14 C19 92.6(2) . . . . ? C19 C14 C15 C16 -4.4(3) . . . . ? C1 C14 C15 C16 169.23(17) . . . . ? C19 C14 C15 C23 174.86(16) . . . . ? C1 C14 C15 C23 -11.5(3) . . . . ? C14 C15 C16 C17 3.4(3) . . . . ? C23 C15 C16 C17 -175.86(18) . . . . ? C15 C16 C17 O4 -178.7(2) . . . . ? C15 C16 C17 C18 1.1(3) . . . . ? O4 C17 C18 O5 -2.0(3) . . . . ? C16 C17 C18 O5 178.15(17) . . . . ? O4 C17 C18 C19 175.29(18) . . . . ? C16 C17 C18 C19 -4.6(3) . . . . ? O5 C18 C19 O6 1.1(3) . . . . ? C17 C18 C19 O6 -176.14(17) . . . . ? O5 C18 C19 C14 -179.19(16) . . . . ? C17 C18 C19 C14 3.6(3) . . . . ? C15 C14 C19 O6 -179.36(16) . . . . ? C1 C14 C19 O6 6.6(2) . . . . ? C15 C14 C19 C18 0.9(3) . . . . ? C1 C14 C19 C18 -173.08(17) . . . . ? C16 C15 C23 N 144.4(2) . . . . ? C14 C15 C23 N -34.9(3) . . . . ? C16 C15 C23 O7 -31.3(2) . . . . ? C14 C15 C23 O7 149.45(17) . . . . ? N C24 C25 O7 -8.8(3) . . . . ? C26 C24 C25 O7 113.5(2) . . . . ? N C24 C26 C27 57.3(3) . . . . ? C25 C24 C26 C27 -60.5(3) . . . . ? N C24 C26 C28 -176.7(2) . . . . ? C25 C24 C26 C28 65.4(3) . . . . ? O7 C23 N C24 -3.2(2) . . . . ? C15 C23 N C24 -178.75(18) . . . . ? C26 C24 N C23 -118.0(2) . . . . ? C25 C24 N C23 7.5(2) . . . . ? C6 C5 O1 C7 -179.8(2) . . . . ? C4 C5 O1 C7 0.3(3) . . . . ? O2 C7 O1 C5 0.2(3) . . . . ? C3 C4 O2 C7 -179.7(2) . . . . ? C5 C4 O2 C7 0.8(3) . . . . ? O1 C7 O2 C4 -0.6(3) . . . . ? C16 C17 O4 C20 20.1(3) . . . . ? C18 C17 O4 C20 -159.7(2) . . . . ? C17 C18 O5 C21 -98.0(2) . . . . ? C19 C18 O5 C21 84.7(2) . . . . ? C18 C19 O6 C22 75.4(2) . . . . ? C14 C19 O6 C22 -104.35(19) . . . . ? N C23 O7 C25 -2.9(3) . . . . ? C15 C23 O7 C25 173.1(2) . . . . ? C24 C25 O7 C23 7.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H1O3 N 0.82(3) 2.01(3) 2.829(2) 178(3) . # END of CIF # Attachment '- 16 archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-05-05 at 17:44:31 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : shelxl dreduc import struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_RajanBabu1763 _database_code_depnum_ccdc_archive 'CCDC 854083' #TrackingRef '- 16 archive.cif' _audit_creation_date 2011-05-05T17:44:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'RajanBabu 1763' _chemical_formula_moiety 'C28 H35 N1 O7 Si1' _chemical_formula_sum 'C28 H35 N O7 Si' _chemical_formula_weight 525.66 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.6948(1) _cell_length_b 14.0253(2) _cell_length_c 18.4358(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2765.33(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2734 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular pyramid' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_special_details ; All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space with a redundancy factor of 3.7, which means that 90% of these reflections were measured at least 3.7 times. Omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.13 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.64619E-2 _diffrn_orient_matrix_ub_12 -0.412003E-1 _diffrn_orient_matrix_ub_13 0.441106E-1 _diffrn_orient_matrix_ub_21 -0.879112E-1 _diffrn_orient_matrix_ub_22 0.221231E-1 _diffrn_orient_matrix_ub_23 0.76253E-2 _diffrn_orient_matrix_ub_31 -0.311889E-1 _diffrn_orient_matrix_ub_32 -0.538215E-1 _diffrn_orient_matrix_ub_33 -0.306323E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 47105 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.2 _diffrn_reflns_theta_max 24.89 _diffrn_reflns_theta_full 24.89 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 4782 _reflns_number_gt 4415 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded carbon atom). The torsion angle, which defines the orientation of the methyl group about the O-C, N-C, or Si-C bond, was refined. The hydroxyl hydrogen atom bonded to atom O(3) was refined isotropically. The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+1.7106P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4782 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(15) _refine_diff_density_max 0.33 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.044 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 -0.0402(2) 0.97209(17) 0.24443(12) 0.0226(5) Uani 1 1 d . . . C2 C 0.0670(2) 0.93443(18) 0.21214(13) 0.0244(5) Uani 1 1 d . . . C3 C 0.1839(2) 0.94094(18) 0.24637(13) 0.0265(6) Uani 1 1 d . . . H3 H 0.2573 0.916 0.2243 0.032 Uiso 1 1 calc R . . C4 C 0.1883(2) 0.98474(19) 0.31293(14) 0.0268(6) Uani 1 1 d . . . C5 C 0.0821(2) 1.02034(18) 0.34541(13) 0.0256(6) Uani 1 1 d . . . C6 C -0.0322(2) 1.01585(18) 0.31309(13) 0.0254(5) Uani 1 1 d . . . H6 H -0.1043 1.0414 0.3361 0.031 Uiso 1 1 calc R . . C7 C 0.2458(3) 1.0522(2) 0.41765(15) 0.0385(7) Uani 1 1 d . . . H7A H 0.2728 1.0246 0.4646 0.046 Uiso 1 1 calc R . . H7B H 0.2804 1.1174 0.4137 0.046 Uiso 1 1 calc R . . C8 C 0.0606(2) 0.89337(19) 0.13585(13) 0.0269(6) Uani 1 1 d . . . H8 H -0.0257 0.8682 0.1274 0.032 Uiso 1 1 calc R . . C9 C 0.1506(2) 0.8161(2) 0.12326(13) 0.0295(6) Uani 1 1 d . . . C10 C 0.2263(3) 0.7548(2) 0.10937(14) 0.0306(6) Uani 1 1 d . . . C11 C 0.4025(3) 0.5949(2) 0.15278(17) 0.0412(7) Uani 1 1 d . . . H11A H 0.4427 0.6354 0.1893 0.062 Uiso 1 1 calc R . . H11B H 0.4631 0.5484 0.1344 0.062 Uiso 1 1 calc R . . H11C H 0.3318 0.5613 0.1748 0.062 Uiso 1 1 calc R . . C12 C 0.4758(3) 0.7407(2) 0.03821(15) 0.0372(7) Uani 1 1 d . . . H12A H 0.444 0.7824 -0.0002 0.056 Uiso 1 1 calc R . . H12B H 0.5389 0.6975 0.018 0.056 Uiso 1 1 calc R . . H12C H 0.5137 0.7796 0.0765 0.056 Uiso 1 1 calc R . . C13 C 0.2721(3) 0.5954(2) 0.00516(17) 0.0440(8) Uani 1 1 d . . . H13A H 0.1994 0.5623 0.0255 0.066 Uiso 1 1 calc R . . H13B H 0.3328 0.5484 -0.0124 0.066 Uiso 1 1 calc R . . H13C H 0.2452 0.636 -0.0352 0.066 Uiso 1 1 calc R . . C14 C -0.1686(2) 0.96684(18) 0.21078(12) 0.0230(5) Uani 1 1 d . . . C15 C -0.2221(2) 1.04121(18) 0.17088(12) 0.0228(5) Uani 1 1 d . . . C16 C -0.3486(2) 1.03836(19) 0.14969(13) 0.0263(5) Uani 1 1 d . . . H16 H -0.3837 1.0897 0.123 0.032 Uiso 1 1 calc R . . C17 C -0.4218(2) 0.9603(2) 0.16802(12) 0.0282(6) Uani 1 1 d . . . C18 C -0.3697(2) 0.88530(19) 0.20615(13) 0.0276(6) Uani 1 1 d . . . C19 C -0.2440(2) 0.88842(18) 0.22647(13) 0.0240(5) Uani 1 1 d . . . C20 C -0.6002(3) 1.0236(3) 0.10759(18) 0.0535(9) Uani 1 1 d . . . H20A H -0.5928 1.0853 0.1321 0.08 Uiso 1 1 calc R . . H20B H -0.6887 1.0089 0.0995 0.08 Uiso 1 1 calc R . . H20C H -0.5567 1.0263 0.0608 0.08 Uiso 1 1 calc R . . C21 C -0.4930(3) 0.8095(3) 0.29426(17) 0.0502(8) Uani 1 1 d . . . H21A H -0.4255 0.8016 0.3297 0.075 Uiso 1 1 calc R . . H21B H -0.5538 0.7578 0.3 0.075 Uiso 1 1 calc R . . H21C H -0.5345 0.8709 0.3022 0.075 Uiso 1 1 calc R . . C22 C -0.1838(3) 0.7250(2) 0.22864(18) 0.0466(8) Uani 1 1 d . . . H22A H -0.266 0.7057 0.2103 0.07 Uiso 1 1 calc R . . H22B H -0.1519 0.6761 0.2618 0.07 Uiso 1 1 calc R . . H22C H -0.1257 0.7325 0.1879 0.07 Uiso 1 1 calc R . . C23 C -0.1501(2) 1.12514(18) 0.14753(13) 0.0236(5) Uani 1 1 d . . . C24 C -0.0050(3) 1.2286(2) 0.11316(15) 0.0346(7) Uani 1 1 d . . . H24 H 0.0317 1.2617 0.1562 0.042 Uiso 1 1 calc R . . C25 C -0.1342(3) 1.2718(2) 0.0986(2) 0.0479(8) Uani 1 1 d . . . H25A H -0.141 1.3365 0.1196 0.057 Uiso 1 1 calc R . . H25B H -0.1515 1.2752 0.0459 0.057 Uiso 1 1 calc R . . C26 C 0.0887(3) 1.2347(2) 0.05157(15) 0.0381(7) Uani 1 1 d . . . H26 H 0.1646 1.1984 0.0671 0.046 Uiso 1 1 calc R . . C27 C 0.1295(3) 1.3390(2) 0.04014(18) 0.0476(8) Uani 1 1 d . . . H27A H 0.0564 1.3778 0.0276 0.071 Uiso 1 1 calc R . . H27B H 0.1908 1.3422 0.0007 0.071 Uiso 1 1 calc R . . H27C H 0.1672 1.3635 0.0849 0.071 Uiso 1 1 calc R . . C28 C 0.0423(4) 1.1890(3) -0.01674(17) 0.0584(10) Uani 1 1 d . . . H28A H 0.0101 1.1252 -0.0057 0.088 Uiso 1 1 calc R . . H28B H 0.1112 1.1839 -0.0516 0.088 Uiso 1 1 calc R . . H28C H -0.0247 1.228 -0.0376 0.088 Uiso 1 1 calc R . . N N -0.0340(2) 1.12956(16) 0.13444(12) 0.0311(5) Uani 1 1 d . . . O1 O 0.11181(17) 1.05489(15) 0.41375(10) 0.0381(5) Uani 1 1 d . . . O2 O 0.28991(16) 0.99424(15) 0.35871(10) 0.0358(5) Uani 1 1 d . . . O3 O 0.08599(17) 0.96625(14) 0.08307(9) 0.0333(4) Uani 1 1 d . . . H1O3 H 0.057(4) 1.028(3) 0.100(2) 0.085(13) Uiso 1 1 d . . . O4 O -0.54556(16) 0.95133(15) 0.15156(10) 0.0374(5) Uani 1 1 d . . . O5 O -0.44251(17) 0.80696(14) 0.22306(10) 0.0367(5) Uani 1 1 d . . . O6 O -0.19492(17) 0.81400(12) 0.26663(10) 0.0321(4) Uani 1 1 d . . . O7 O -0.21909(19) 1.20553(13) 0.13457(12) 0.0419(5) Uani 1 1 d . . . Si Si 0.34558(7) 0.67027(5) 0.07649(4) 0.02786(17) 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 0.0205(13) 0.0252(13) 0.0219(12) -0.0012(10) -0.0014(10) -0.0010(11) C2 0.0219(13) 0.0292(13) 0.0222(12) 0.0008(10) -0.0023(10) 0.0009(11) C3 0.0207(13) 0.0328(14) 0.0259(13) -0.0003(11) 0.0024(10) 0.0014(11) C4 0.0217(13) 0.0306(14) 0.0282(13) 0.0030(11) -0.0053(10) -0.0046(11) C5 0.0299(14) 0.0281(13) 0.0188(12) -0.0013(10) -0.0021(11) -0.0042(12) C6 0.0219(13) 0.0303(14) 0.0242(12) -0.0025(11) 0.0009(10) 0.0014(11) C7 0.0351(16) 0.0483(17) 0.0321(14) -0.0057(14) -0.0095(13) -0.0058(13) C8 0.0196(12) 0.0372(15) 0.0240(12) -0.0032(11) 0.0000(10) 0.0060(11) C9 0.0256(13) 0.0406(16) 0.0221(12) -0.0051(11) -0.0015(11) 0.0000(13) C10 0.0267(14) 0.0386(16) 0.0265(13) -0.0058(12) 0.0006(11) 0.0043(13) C11 0.0325(15) 0.0478(18) 0.0432(17) 0.0122(14) 0.0057(14) 0.0041(14) C12 0.0373(17) 0.0405(17) 0.0340(15) 0.0019(13) 0.0074(12) 0.0026(14) C13 0.0469(18) 0.0448(18) 0.0404(17) -0.0117(14) 0.0010(14) 0.0046(15) C14 0.0188(12) 0.0296(13) 0.0206(12) -0.0075(10) 0.0012(10) 0.0025(11) C15 0.0211(12) 0.0292(14) 0.0182(12) -0.0044(10) 0.0004(10) -0.0004(11) C16 0.0199(12) 0.0361(15) 0.0229(12) -0.0022(11) -0.0002(10) 0.0022(12) C17 0.0202(13) 0.0459(17) 0.0184(12) -0.0033(11) -0.0005(10) -0.0008(12) C18 0.0267(14) 0.0318(14) 0.0242(13) -0.0062(11) 0.0030(11) -0.0078(12) C19 0.0237(13) 0.0273(13) 0.0210(12) -0.0030(10) -0.0014(10) 0.0026(11) C20 0.0250(15) 0.083(2) 0.0521(19) 0.0268(19) -0.0141(14) -0.0043(17) C21 0.0485(19) 0.057(2) 0.0451(18) 0.0042(16) 0.0159(15) -0.0111(17) C22 0.056(2) 0.0279(15) 0.0554(19) -0.0110(14) -0.0090(16) 0.0030(15) C23 0.0257(13) 0.0259(13) 0.0193(11) -0.0049(10) -0.0033(11) 0.0012(11) C24 0.0412(17) 0.0342(15) 0.0285(14) 0.0039(12) -0.0031(13) -0.0090(13) C25 0.0466(19) 0.0305(16) 0.066(2) 0.0054(15) 0.0147(16) 0.0015(14) C26 0.0406(17) 0.0331(15) 0.0407(16) 0.0036(13) 0.0049(14) 0.0001(14) C27 0.058(2) 0.0382(17) 0.0465(18) 0.0088(14) 0.0109(15) -0.0061(16) C28 0.069(2) 0.069(2) 0.0377(17) -0.0046(17) 0.0082(17) -0.016(2) N 0.0273(13) 0.0296(12) 0.0364(13) 0.0071(10) 0.0001(10) -0.0026(10) O1 0.0332(11) 0.0535(12) 0.0277(10) -0.0136(9) -0.0073(8) -0.0010(9) O2 0.0237(10) 0.0525(12) 0.0313(10) -0.0065(9) -0.0086(8) -0.0036(9) O3 0.0339(10) 0.0421(12) 0.0239(9) 0.0015(9) 0.0017(8) 0.0074(9) O4 0.0189(9) 0.0570(13) 0.0365(10) 0.0022(10) -0.0032(8) -0.0066(9) O5 0.0339(10) 0.0434(12) 0.0329(10) -0.0010(9) 0.0014(9) -0.0165(9) O6 0.0371(10) 0.0247(9) 0.0346(10) -0.0026(8) -0.0063(8) -0.0005(8) O7 0.0375(11) 0.0302(10) 0.0581(13) 0.0037(9) 0.0108(10) 0.0078(9) Si 0.0263(4) 0.0320(4) 0.0253(3) -0.0007(3) 0.0028(3) 0.0051(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.396(4) . ? C1 C6 1.409(3) . ? C1 C14 1.508(3) . ? C2 C3 1.404(4) . ? C2 C8 1.521(3) . ? C3 C4 1.373(4) . ? C3 H3 0.95 . ? C4 C5 1.378(4) . ? C4 O2 1.383(3) . ? C5 C6 1.361(4) . ? C5 O1 1.387(3) . ? C6 H6 0.95 . ? C7 O1 1.436(3) . ? C7 O2 1.436(3) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 O3 1.437(3) . ? C8 C9 1.468(4) . ? C8 H8 1 . ? C9 C10 1.209(4) . ? C10 Si 1.843(3) . ? C11 Si 1.862(3) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 Si 1.848(3) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 Si 1.858(3) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C19 1.394(4) . ? C14 C15 1.399(4) . ? C15 C16 1.409(3) . ? C15 C23 1.471(4) . ? C16 C17 1.387(4) . ? C16 H16 0.95 . ? C17 O4 1.364(3) . ? C17 C18 1.382(4) . ? C18 O5 1.382(3) . ? C18 C19 1.397(4) . ? C19 O6 1.383(3) . ? C20 O4 1.423(4) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 O5 1.420(3) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 O6 1.436(3) . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 N 1.267(3) . ? C23 O7 1.368(3) . ? C24 N 1.476(3) . ? C24 C26 1.517(4) . ? C24 C25 1.533(4) . ? C24 H24 1 . ? C25 O7 1.459(4) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C28 1.498(4) . ? C26 C27 1.542(4) . ? C26 H26 1 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? O3 H1O3 0.97(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 C2 C1 C6 119.9(2) . . ? C2 C1 C14 123.6(2) . . ? C6 C1 C14 116.5(2) . . ? C1 C2 C3 121.0(2) . . ? C1 C2 C8 120.0(2) . . ? C3 C2 C8 118.7(2) . . ? C4 C3 C2 117.5(2) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 121.5(2) . . ? C3 C4 O2 128.0(2) . . ? C5 C4 O2 110.4(2) . . ? C6 C5 C4 122.2(2) . . ? C6 C5 O1 128.3(2) . . ? C4 C5 O1 109.4(2) . . ? C5 C6 C1 117.9(2) . . ? C5 C6 H6 121.1 . . ? C1 C6 H6 121.1 . . ? O1 C7 O2 107.8(2) . . ? O1 C7 H7A 110.2 . . ? O2 C7 H7A 110.2 . . ? O1 C7 H7B 110.2 . . ? O2 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? O3 C8 C9 107.1(2) . . ? O3 C8 C2 110.4(2) . . ? C9 C8 C2 113.3(2) . . ? O3 C8 H8 108.7 . . ? C9 C8 H8 108.7 . . ? C2 C8 H8 108.7 . . ? C10 C9 C8 176.5(3) . . ? C9 C10 Si 172.1(2) . . ? Si C11 H11A 109.5 . . ? Si C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si C12 H12A 109.5 . . ? Si C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si C13 H13A 109.5 . . ? Si C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 117.4(2) . . ? C19 C14 C1 118.7(2) . . ? C15 C14 C1 123.5(2) . . ? C14 C15 C16 121.2(2) . . ? C14 C15 C23 122.5(2) . . ? C16 C15 C23 116.4(2) . . ? C17 C16 C15 119.8(2) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? O4 C17 C18 115.7(2) . . ? O4 C17 C16 124.4(2) . . ? C18 C17 C16 119.8(2) . . ? C17 C18 O5 119.5(2) . . ? C17 C18 C19 120.0(2) . . ? O5 C18 C19 120.4(2) . . ? O6 C19 C14 119.1(2) . . ? O6 C19 C18 119.0(2) . . ? C14 C19 C18 121.7(2) . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O6 C22 H22A 109.5 . . ? O6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N C23 O7 117.1(2) . . ? N C23 C15 127.4(2) . . ? O7 C23 C15 115.4(2) . . ? N C24 C26 113.0(2) . . ? N C24 C25 103.2(2) . . ? C26 C24 C25 116.2(2) . . ? N C24 H24 108 . . ? C26 C24 H24 108 . . ? C25 C24 H24 108 . . ? O7 C25 C24 103.3(2) . . ? O7 C25 H25A 111.1 . . ? C24 C25 H25A 111.1 . . ? O7 C25 H25B 111.1 . . ? C24 C25 H25B 111.1 . . ? H25A C25 H25B 109.1 . . ? C28 C26 C24 112.7(3) . . ? C28 C26 C27 112.7(3) . . ? C24 C26 C27 110.1(2) . . ? C28 C26 H26 107 . . ? C24 C26 H26 107 . . ? C27 C26 H26 107 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C23 N C24 107.6(2) . . ? C5 O1 C7 105.4(2) . . ? C4 O2 C7 104.97(19) . . ? C8 O3 H1O3 111(2) . . ? C17 O4 C20 117.4(2) . . ? C18 O5 C21 113.7(2) . . ? C19 O6 C22 115.2(2) . . ? C23 O7 C25 105.6(2) . . ? C10 Si C12 107.65(13) . . ? C10 Si C13 107.66(14) . . ? C12 Si C13 110.55(14) . . ? C10 Si C11 110.05(13) . . ? C12 Si C11 110.21(14) . . ? C13 Si C11 110.64(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.2(4) . . . . ? C14 C1 C2 C3 -179.6(2) . . . . ? C6 C1 C2 C8 -175.7(2) . . . . ? C14 C1 C2 C8 5.9(4) . . . . ? C1 C2 C3 C4 0.7(4) . . . . ? C8 C2 C3 C4 175.3(2) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C2 C3 C4 O2 175.5(3) . . . . ? C3 C4 C5 C6 -1.3(4) . . . . ? O2 C4 C5 C6 -177.1(2) . . . . ? C3 C4 C5 O1 176.1(2) . . . . ? O2 C4 C5 O1 0.3(3) . . . . ? C4 C5 C6 C1 0.7(4) . . . . ? O1 C5 C6 C1 -176.2(2) . . . . ? C2 C1 C6 C5 0.5(4) . . . . ? C14 C1 C6 C5 179.0(2) . . . . ? C1 C2 C8 O3 90.1(3) . . . . ? C3 C2 C8 O3 -84.6(3) . . . . ? C1 C2 C8 C9 -149.9(2) . . . . ? C3 C2 C8 C9 35.5(3) . . . . ? C2 C1 C14 C19 90.0(3) . . . . ? C6 C1 C14 C19 -88.4(3) . . . . ? C2 C1 C14 C15 -97.3(3) . . . . ? C6 C1 C14 C15 84.3(3) . . . . ? C19 C14 C15 C16 2.2(3) . . . . ? C1 C14 C15 C16 -170.6(2) . . . . ? C19 C14 C15 C23 -176.5(2) . . . . ? C1 C14 C15 C23 10.6(3) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C23 C15 C16 C17 178.3(2) . . . . ? C15 C16 C17 O4 178.6(2) . . . . ? C15 C16 C17 C18 -0.8(4) . . . . ? O4 C17 C18 O5 1.8(3) . . . . ? C16 C17 C18 O5 -178.8(2) . . . . ? O4 C17 C18 C19 -179.1(2) . . . . ? C16 C17 C18 C19 0.3(4) . . . . ? C15 C14 C19 O6 -179.2(2) . . . . ? C1 C14 C19 O6 -6.0(3) . . . . ? C15 C14 C19 C18 -2.7(3) . . . . ? C1 C14 C19 C18 170.5(2) . . . . ? C17 C18 C19 O6 177.9(2) . . . . ? O5 C18 C19 O6 -2.9(3) . . . . ? C17 C18 C19 C14 1.5(4) . . . . ? O5 C18 C19 C14 -179.4(2) . . . . ? C14 C15 C23 N 28.2(4) . . . . ? C16 C15 C23 N -150.7(3) . . . . ? C14 C15 C23 O7 -156.1(2) . . . . ? C16 C15 C23 O7 25.1(3) . . . . ? N C24 C25 O7 17.5(3) . . . . ? C26 C24 C25 O7 141.8(2) . . . . ? N C24 C26 C28 61.9(3) . . . . ? C25 C24 C26 C28 -57.3(4) . . . . ? N C24 C26 C27 -171.4(2) . . . . ? C25 C24 C26 C27 69.4(3) . . . . ? O7 C23 N C24 4.6(3) . . . . ? C15 C23 N C24 -179.7(2) . . . . ? C26 C24 N C23 -140.3(2) . . . . ? C25 C24 N C23 -13.9(3) . . . . ? C6 C5 O1 C7 -174.2(3) . . . . ? C4 C5 O1 C7 8.6(3) . . . . ? O2 C7 O1 C5 -14.1(3) . . . . ? C3 C4 O2 C7 175.4(3) . . . . ? C5 C4 O2 C7 -9.1(3) . . . . ? O1 C7 O2 C4 14.3(3) . . . . ? C18 C17 O4 C20 -175.3(3) . . . . ? C16 C17 O4 C20 5.3(4) . . . . ? C17 C18 O5 C21 -97.2(3) . . . . ? C19 C18 O5 C21 83.7(3) . . . . ? C14 C19 O6 C22 -114.6(3) . . . . ? C18 C19 O6 C22 68.9(3) . . . . ? N C23 O7 C25 7.5(3) . . . . ? C15 C23 O7 C25 -168.7(2) . . . . ? C24 C25 O7 C23 -15.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H1O3 N 0.97(4) 1.84(4) 2.791(3) 166(4) . # END of CIF # Attachment '- 21A archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-05-05 at 14:35:08 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : shelxl dreduc import struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_RajanBabu1761 _database_code_depnum_ccdc_archive 'CCDC 854084' #TrackingRef '- 21A archive.cif' _audit_creation_date 2011-05-05T14:35:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'RajanBabu 1761' _chemical_formula_moiety 'C28 H36 O6 Si2' _chemical_formula_sum 'C28 H36 O6 Si2' _chemical_formula_weight 524.75 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3358(1) _cell_length_b 10.7754(1) _cell_length_c 13.7612(1) _cell_angle_alpha 103.096(1) _cell_angle_beta 100.398(1) _cell_angle_gamma 91.195(1) _cell_volume 1465.19(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6669 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular rod' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_special_details ;All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.5, which means that 90% of these reflections were measured at least 3.5 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.708066E-1 _diffrn_orient_matrix_ub_12 -0.44796E-2 _diffrn_orient_matrix_ub_13 0.589014E-1 _diffrn_orient_matrix_ub_21 -0.34583E-1 _diffrn_orient_matrix_ub_22 0.747406E-1 _diffrn_orient_matrix_ub_23 0.430838E-1 _diffrn_orient_matrix_ub_31 -0.592179E-1 _diffrn_orient_matrix_ub_32 -0.592482E-1 _diffrn_orient_matrix_ub_33 0.212079E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 44089 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 6685 _reflns_number_gt 4892 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded carbon atom). The torsion angle, which defines the orientation of the methyl group about the O-C or Si-C bond, was refined. The hydroxyl hydrogen atom bonded to atom O(3) was refined isotropically. The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.3496P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6685 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.04 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.067 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.335 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.69613(5) -0.00604(4) 0.30900(4) 0.03354(13) Uani 1 1 d . . . Si2 Si 0.21428(5) -0.13304(4) 0.07958(4) 0.02999(13) Uani 1 1 d . . . O1 O 0.71373(10) 0.59419(11) 0.00669(8) 0.0290(3) Uani 1 1 d . . . O2 O 0.92333(11) 0.57059(12) 0.09249(8) 0.0334(3) Uani 1 1 d . . . O3 O 0.87699(10) 0.47437(11) 0.42909(9) 0.0266(3) Uani 1 1 d . . . H1O3 H 0.871(2) 0.482(2) 0.4887(16) 0.048(6) Uiso 1 1 d . . . O4 O 0.51080(11) 0.66371(10) 0.36094(8) 0.0268(3) Uani 1 1 d . . . O5 O 0.27600(11) 0.61784(10) 0.42671(8) 0.0268(3) Uani 1 1 d . . . O6 O 0.14597(10) 0.39164(10) 0.36217(8) 0.0288(3) Uani 1 1 d . . . C1 C 0.61007(14) 0.48272(13) 0.21758(10) 0.0188(3) Uani 1 1 d . . . C2 C 0.73629(14) 0.46933(13) 0.26966(10) 0.0196(3) Uani 1 1 d . . . C3 C 0.84941(15) 0.49767(14) 0.23300(11) 0.0234(3) Uani 1 1 d . . . H3 H 0.9355 0.4883 0.2677 0.028 Uiso 1 1 calc R . . C4 C 0.82936(14) 0.53947(14) 0.14477(11) 0.0228(3) Uani 1 1 d . . . C5 C 0.70551(15) 0.55317(14) 0.09380(11) 0.0215(3) Uani 1 1 d . . . C6 C 0.59394(14) 0.52633(14) 0.12774(11) 0.0211(3) Uani 1 1 d . . . H6 H 0.5089 0.5368 0.0919 0.025 Uiso 1 1 calc R . . C7 C 0.85133(16) 0.61916(17) 0.01126(13) 0.0326(4) Uani 1 1 d . . . H7A H 0.8722 0.7122 0.0236 0.039 Uiso 1 1 calc R . . H7B H 0.876 0.5769 -0.0539 0.039 Uiso 1 1 calc R . . C8 C 0.75327(14) 0.42297(14) 0.36723(11) 0.0221(3) Uani 1 1 d . . . H8 H 0.6817 0.456 0.4043 0.027 Uiso 1 1 calc R . . C9 C 0.74330(15) 0.28182(15) 0.34558(11) 0.0252(3) Uani 1 1 d . . . C10 C 0.73123(16) 0.16716(16) 0.32841(12) 0.0311(4) Uani 1 1 d . . . C11 C 0.6864(2) -0.08536(19) 0.17308(15) 0.0476(5) Uani 1 1 d . . . H11A H 0.6167 -0.0497 0.1312 0.071 Uiso 1 1 calc R . . H11B H 0.6665 -0.1772 0.1628 0.071 Uiso 1 1 calc R . . H11C H 0.771 -0.071 0.1534 0.071 Uiso 1 1 calc R . . C12 C 0.8305(2) -0.0712(2) 0.38883(19) 0.0659(7) Uani 1 1 d . . . H12A H 0.9153 -0.0515 0.3716 0.099 Uiso 1 1 calc R . . H12B H 0.8148 -0.164 0.3762 0.099 Uiso 1 1 calc R . . H12C H 0.8322 -0.0325 0.4608 0.099 Uiso 1 1 calc R . . C13 C 0.5360(2) -0.02378(18) 0.34904(15) 0.0432(5) Uani 1 1 d . . . H13A H 0.545 0.0163 0.4215 0.065 Uiso 1 1 calc R . . H13B H 0.5095 -0.1147 0.337 0.065 Uiso 1 1 calc R . . H13C H 0.4689 0.0176 0.3097 0.065 Uiso 1 1 calc R . . C14 C 0.48803(14) 0.45286(14) 0.25464(10) 0.0187(3) Uani 1 1 d . . . C15 C 0.41545(14) 0.33552(14) 0.21679(10) 0.0196(3) Uani 1 1 d . . . C16 C 0.30160(14) 0.31176(14) 0.25201(11) 0.0222(3) Uani 1 1 d . . . H16 H 0.2548 0.2306 0.2278 0.027 Uiso 1 1 calc R . . C17 C 0.25594(14) 0.40582(15) 0.32218(11) 0.0223(3) Uani 1 1 d . . . C18 C 0.32375(14) 0.52549(14) 0.35729(10) 0.0213(3) Uani 1 1 d . . . C19 C 0.44076(14) 0.54692(14) 0.32553(11) 0.0207(3) Uani 1 1 d . . . C20 C 0.08669(17) 0.26510(17) 0.34361(14) 0.0350(4) Uani 1 1 d . . . H20A H 0.0489 0.2349 0.2711 0.053 Uiso 1 1 calc R . . H20B H 0.0169 0.2658 0.3833 0.053 Uiso 1 1 calc R . . H20C H 0.1537 0.208 0.3636 0.053 Uiso 1 1 calc R . . C21 C 0.20793(19) 0.71250(18) 0.38314(14) 0.0414(5) Uani 1 1 d . . . H21A H 0.27 0.7617 0.358 0.062 Uiso 1 1 calc R . . H21B H 0.1696 0.77 0.4349 0.062 Uiso 1 1 calc R . . H21C H 0.1376 0.6706 0.3266 0.062 Uiso 1 1 calc R . . C22 C 0.55998(19) 0.70016(17) 0.46846(12) 0.0375(4) Uani 1 1 d . . . H22A H 0.4858 0.7135 0.5043 0.056 Uiso 1 1 calc R . . H22B H 0.616 0.7794 0.4849 0.056 Uiso 1 1 calc R . . H22C H 0.6117 0.6324 0.4896 0.056 Uiso 1 1 calc R . . C23 C 0.46183(15) 0.23355(14) 0.13610(11) 0.0227(3) Uani 1 1 d . . . H23A H 0.4576 0.2654 0.0736 0.027 Uiso 1 1 calc R . . H23B H 0.555 0.219 0.1607 0.027 Uiso 1 1 calc R . . C24 C 0.38360(15) 0.11192(15) 0.11095(11) 0.0249(3) Uani 1 1 d . . . C25 C 0.31621(17) 0.01370(16) 0.09425(12) 0.0310(4) Uani 1 1 d . . . C26 C 0.32356(19) -0.26248(17) 0.10092(15) 0.0434(5) Uani 1 1 d . . . H26A H 0.3787 -0.2791 0.049 0.065 Uiso 1 1 calc R . . H26B H 0.2698 -0.3402 0.0966 0.065 Uiso 1 1 calc R . . H26C H 0.3799 -0.2365 0.1684 0.065 Uiso 1 1 calc R . . C27 C 0.1135(2) -0.17599(19) -0.05107(14) 0.0447(5) Uani 1 1 d . . . H27A H 0.0473 -0.1132 -0.0581 0.067 Uiso 1 1 calc R . . H27B H 0.0692 -0.2609 -0.0633 0.067 Uiso 1 1 calc R . . H27C H 0.1708 -0.1765 -0.1006 0.067 Uiso 1 1 calc R . . C28 C 0.10824(19) -0.10081(18) 0.17761(14) 0.0406(4) Uani 1 1 d . . . H28A H 0.1639 -0.0706 0.245 0.061 Uiso 1 1 calc R . . H28B H 0.0575 -0.1795 0.1755 0.061 Uiso 1 1 calc R . . H28C H 0.0477 -0.0354 0.1638 0.061 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 0.0406(3) 0.0247(2) 0.0353(3) 0.0089(2) 0.0046(2) 0.0007(2) Si2 0.0325(3) 0.0223(2) 0.0338(3) 0.00283(19) 0.0079(2) -0.00287(19) O1 0.0264(6) 0.0393(7) 0.0265(6) 0.0163(5) 0.0083(5) -0.0013(5) O2 0.0239(6) 0.0502(8) 0.0332(6) 0.0198(5) 0.0116(5) -0.0009(5) O3 0.0225(6) 0.0345(7) 0.0202(6) 0.0042(5) 0.0013(5) -0.0046(5) O4 0.0331(6) 0.0207(5) 0.0249(6) 0.0003(4) 0.0081(5) -0.0052(5) O5 0.0337(6) 0.0250(6) 0.0253(6) 0.0056(5) 0.0143(5) 0.0085(5) O6 0.0230(6) 0.0304(6) 0.0341(6) 0.0033(5) 0.0143(5) -0.0017(5) C1 0.0188(7) 0.0163(7) 0.0202(7) 0.0013(6) 0.0051(6) -0.0013(6) C2 0.0213(8) 0.0178(7) 0.0193(7) 0.0030(6) 0.0045(6) -0.0006(6) C3 0.0188(8) 0.0262(8) 0.0252(8) 0.0059(6) 0.0048(6) 0.0000(6) C4 0.0206(8) 0.0231(8) 0.0269(8) 0.0061(6) 0.0103(6) -0.0011(6) C5 0.0270(8) 0.0188(7) 0.0194(7) 0.0053(6) 0.0057(6) 0.0005(6) C6 0.0200(8) 0.0216(8) 0.0211(7) 0.0041(6) 0.0033(6) -0.0001(6) C7 0.0283(9) 0.0428(10) 0.0330(9) 0.0173(8) 0.0118(7) -0.0001(7) C8 0.0180(7) 0.0272(8) 0.0218(7) 0.0076(6) 0.0033(6) -0.0005(6) C9 0.0233(8) 0.0319(9) 0.0210(8) 0.0087(7) 0.0026(6) -0.0009(7) C10 0.0322(9) 0.0322(10) 0.0285(9) 0.0096(7) 0.0019(7) -0.0016(7) C11 0.0569(13) 0.0368(11) 0.0482(12) 0.0013(9) 0.0189(10) 0.0022(9) C12 0.0679(16) 0.0507(14) 0.0783(17) 0.0298(12) -0.0068(13) 0.0074(12) C13 0.0584(13) 0.0315(10) 0.0419(11) 0.0094(8) 0.0155(9) -0.0059(9) C14 0.0175(7) 0.0216(7) 0.0182(7) 0.0064(6) 0.0042(6) 0.0012(6) C15 0.0190(7) 0.0210(7) 0.0190(7) 0.0047(6) 0.0044(6) 0.0019(6) C16 0.0213(8) 0.0213(8) 0.0233(8) 0.0040(6) 0.0045(6) -0.0026(6) C17 0.0166(7) 0.0292(8) 0.0228(8) 0.0083(6) 0.0057(6) 0.0011(6) C18 0.0241(8) 0.0230(8) 0.0181(7) 0.0048(6) 0.0066(6) 0.0053(6) C19 0.0233(8) 0.0191(7) 0.0199(7) 0.0061(6) 0.0028(6) -0.0006(6) C20 0.0284(9) 0.0358(10) 0.0431(10) 0.0068(8) 0.0165(8) -0.0053(7) C21 0.0499(12) 0.0347(10) 0.0423(10) 0.0096(8) 0.0130(9) 0.0195(9) C22 0.0479(11) 0.0285(9) 0.0295(9) 0.0017(7) -0.0029(8) -0.0040(8) C23 0.0221(8) 0.0226(8) 0.0234(8) 0.0028(6) 0.0075(6) 0.0000(6) C24 0.0269(8) 0.0250(8) 0.0227(8) 0.0027(6) 0.0082(6) 0.0040(7) C25 0.0338(9) 0.0264(9) 0.0321(9) 0.0023(7) 0.0101(7) 0.0018(7) C26 0.0486(12) 0.0271(10) 0.0534(12) 0.0042(8) 0.0127(9) 0.0028(8) C27 0.0505(12) 0.0401(11) 0.0386(10) 0.0033(8) 0.0050(9) -0.0122(9) C28 0.0414(11) 0.0381(10) 0.0451(11) 0.0112(8) 0.0142(9) -0.0010(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C10 1.8430(18) . ? Si1 C13 1.855(2) . ? Si1 C11 1.856(2) . ? Si1 C12 1.863(2) . ? Si2 C25 1.8330(17) . ? Si2 C26 1.8545(19) . ? Si2 C27 1.8598(19) . ? Si2 C28 1.8652(18) . ? O1 C5 1.3836(17) . ? O1 C7 1.4294(19) . ? O2 C4 1.3861(17) . ? O2 C7 1.435(2) . ? O3 C8 1.4249(17) . ? O3 H1O3 0.82(2) . ? O4 C19 1.3792(17) . ? O4 C22 1.4349(19) . ? O5 C18 1.3806(17) . ? O5 C21 1.432(2) . ? O6 C17 1.3693(17) . ? O6 C20 1.4320(19) . ? C1 C2 1.398(2) . ? C1 C6 1.403(2) . ? C1 C14 1.4981(19) . ? C2 C3 1.408(2) . ? C2 C8 1.5184(19) . ? C3 C4 1.371(2) . ? C3 H3 0.95 . ? C4 C5 1.372(2) . ? C5 C6 1.369(2) . ? C6 H6 0.95 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 C9 1.480(2) . ? C8 H8 1 . ? C9 C10 1.204(2) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C15 1.398(2) . ? C14 C19 1.401(2) . ? C15 C16 1.391(2) . ? C15 C23 1.527(2) . ? C16 C17 1.387(2) . ? C16 H16 0.95 . ? C17 C18 1.395(2) . ? C18 C19 1.390(2) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C24 1.463(2) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 C25 1.208(2) . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? 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 C10 Si1 C13 105.64(8) . . ? C10 Si1 C11 109.66(8) . . ? C13 Si1 C11 111.37(9) . . ? C10 Si1 C12 109.10(9) . . ? C13 Si1 C12 111.26(11) . . ? C11 Si1 C12 109.72(11) . . ? C25 Si2 C26 108.90(8) . . ? C25 Si2 C27 108.88(8) . . ? C26 Si2 C27 110.26(9) . . ? C25 Si2 C28 107.37(8) . . ? C26 Si2 C28 109.94(9) . . ? C27 Si2 C28 111.41(9) . . ? C5 O1 C7 105.37(11) . . ? C4 O2 C7 105.19(11) . . ? C8 O3 H1O3 107.8(14) . . ? C19 O4 C22 115.78(12) . . ? C18 O5 C21 113.78(12) . . ? C17 O6 C20 117.31(12) . . ? C2 C1 C6 120.27(13) . . ? C2 C1 C14 122.23(12) . . ? C6 C1 C14 117.50(13) . . ? C1 C2 C3 121.09(13) . . ? C1 C2 C8 120.08(12) . . ? C3 C2 C8 118.83(13) . . ? C4 C3 C2 116.81(14) . . ? C4 C3 H3 121.6 . . ? C2 C3 H3 121.6 . . ? C3 C4 C5 122.15(13) . . ? C3 C4 O2 127.88(14) . . ? C5 C4 O2 109.95(13) . . ? C6 C5 C4 122.24(13) . . ? C6 C5 O1 127.64(14) . . ? C4 C5 O1 110.11(13) . . ? C5 C6 C1 117.43(13) . . ? C5 C6 H6 121.3 . . ? C1 C6 H6 121.3 . . ? O1 C7 O2 108.28(12) . . ? O1 C7 H7A 110 . . ? O2 C7 H7A 110 . . ? O1 C7 H7B 110 . . ? O2 C7 H7B 110 . . ? H7A C7 H7B 108.4 . . ? O3 C8 C9 111.44(12) . . ? O3 C8 C2 108.68(11) . . ? C9 C8 C2 111.11(12) . . ? O3 C8 H8 108.5 . . ? C9 C8 H8 108.5 . . ? C2 C8 H8 108.5 . . ? C10 C9 C8 177.98(17) . . ? C9 C10 Si1 173.47(15) . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 118.52(13) . . ? C15 C14 C1 121.94(13) . . ? C19 C14 C1 119.46(12) . . ? C16 C15 C14 120.36(13) . . ? C16 C15 C23 120.15(13) . . ? C14 C15 C23 119.49(12) . . ? C17 C16 C15 120.44(13) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? O6 C17 C16 124.94(13) . . ? O6 C17 C18 115.08(13) . . ? C16 C17 C18 119.99(13) . . ? O5 C18 C19 121.62(13) . . ? O5 C18 C17 118.95(13) . . ? C19 C18 C17 119.36(13) . . ? O4 C19 C18 120.32(13) . . ? O4 C19 C14 118.44(13) . . ? C18 C19 C14 121.20(13) . . ? O6 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C15 113.30(12) . . ? C24 C23 H23A 108.9 . . ? C15 C23 H23A 108.9 . . ? C24 C23 H23B 108.9 . . ? C15 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C25 C24 C23 176.80(16) . . ? C24 C25 Si2 175.54(15) . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.7(2) . . . . ? C14 C1 C2 C3 179.80(13) . . . . ? C6 C1 C2 C8 179.58(13) . . . . ? C14 C1 C2 C8 0.1(2) . . . . ? C1 C2 C3 C4 0.4(2) . . . . ? C8 C2 C3 C4 -179.86(13) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? C2 C3 C4 O2 -178.46(14) . . . . ? C7 O2 C4 C3 -174.98(16) . . . . ? C7 O2 C4 C5 6.53(17) . . . . ? C3 C4 C5 C6 0.2(2) . . . . ? O2 C4 C5 C6 178.75(14) . . . . ? C3 C4 C5 O1 -178.85(14) . . . . ? O2 C4 C5 O1 -0.26(17) . . . . ? C7 O1 C5 C6 174.90(15) . . . . ? C7 O1 C5 C4 -6.16(17) . . . . ? C4 C5 C6 C1 -0.4(2) . . . . ? O1 C5 C6 C1 178.40(14) . . . . ? C2 C1 C6 C5 0.7(2) . . . . ? C14 C1 C6 C5 -179.79(13) . . . . ? C5 O1 C7 O2 10.14(17) . . . . ? C4 O2 C7 O1 -10.28(17) . . . . ? C1 C2 C8 O3 -151.84(13) . . . . ? C3 C2 C8 O3 28.43(18) . . . . ? C1 C2 C8 C9 85.19(17) . . . . ? C3 C2 C8 C9 -94.54(16) . . . . ? C2 C1 C14 C15 -97.30(17) . . . . ? C6 C1 C14 C15 83.19(18) . . . . ? C2 C1 C14 C19 85.99(18) . . . . ? C6 C1 C14 C19 -93.52(16) . . . . ? C19 C14 C15 C16 -2.4(2) . . . . ? C1 C14 C15 C16 -179.13(13) . . . . ? C19 C14 C15 C23 177.40(13) . . . . ? C1 C14 C15 C23 0.7(2) . . . . ? C14 C15 C16 C17 2.5(2) . . . . ? C23 C15 C16 C17 -177.32(13) . . . . ? C20 O6 C17 C16 11.1(2) . . . . ? C20 O6 C17 C18 -168.79(13) . . . . ? C15 C16 C17 O6 -179.35(13) . . . . ? C15 C16 C17 C18 0.5(2) . . . . ? C21 O5 C18 C19 80.62(18) . . . . ? C21 O5 C18 C17 -102.55(16) . . . . ? O6 C17 C18 O5 -0.51(19) . . . . ? C16 C17 C18 O5 179.64(13) . . . . ? O6 C17 C18 C19 176.39(13) . . . . ? C16 C17 C18 C19 -3.5(2) . . . . ? C22 O4 C19 C18 62.62(19) . . . . ? C22 O4 C19 C14 -119.53(15) . . . . ? O5 C18 C19 O4 -1.9(2) . . . . ? C17 C18 C19 O4 -178.67(13) . . . . ? O5 C18 C19 C14 -179.65(13) . . . . ? C17 C18 C19 C14 3.5(2) . . . . ? C15 C14 C19 O4 -178.45(13) . . . . ? C1 C14 C19 O4 -1.6(2) . . . . ? C15 C14 C19 C18 -0.6(2) . . . . ? C1 C14 C19 C18 176.20(13) . . . . ? C16 C15 C23 C24 -5.7(2) . . . . ? C14 C15 C23 C24 174.48(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H1O3 O6 0.82(2) 2.23(2) 2.9619(16) 148.5(19) 2_666 O3 H1O3 O5 0.82(2) 2.44(2) 3.0638(15) 134.1(18) 2_666 # END of CIF # Attachment '- 32 archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-06-06 at 13:28:48 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : shelxl dreduc import struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_RajanBabu1842 _database_code_depnum_ccdc_archive 'CCDC 854085' #TrackingRef '- 32 archive.cif' _audit_creation_date 2011-06-06T13:28:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'RajanBabu 1842' _chemical_formula_moiety 'C29 H37 N1 O8 Si1' _chemical_formula_sum 'C29 H37 N O8 Si' _chemical_formula_weight 555.69 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration rmad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.1179(1) _cell_length_b 13.7992(1) _cell_length_c 21.5342(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3006.58(5) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 3880 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_special_details ;All work was done at 210 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure an octant of reciprocal space with a redundancy factor of 5.0, which means that 90% of the reflections were measured at least 5.0 times. Omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.352192E-1 _diffrn_orient_matrix_ub_12 -0.284759E-1 _diffrn_orient_matrix_ub_13 0.393658E-1 _diffrn_orient_matrix_ub_21 0.776594E-1 _diffrn_orient_matrix_ub_22 -0.264436E-1 _diffrn_orient_matrix_ub_23 -0.23193E-1 _diffrn_orient_matrix_ub_31 0.499692E-1 _diffrn_orient_matrix_ub_32 0.611675E-1 _diffrn_orient_matrix_ub_33 0.82997E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 44069 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 6874 _reflns_number_gt 5373 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;The hydroxyl hydrogen atom bonded to atom O(3) was refined isotropically. This hydrogen atom is involved in an intramolecular hydrogen bond with the N atom. For each methyl group, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq (bonded carbon atom). The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). 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^ > 2\s(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 ' w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+0.2347P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6874 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(11) _refine_diff_density_max 0.157 _refine_diff_density_min -0.19 _refine_diff_density_rms 0.037 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 -0.27745(16) -0.05374(12) 0.81107(7) 0.0265(4) Uani 1 1 d . . . C2 C -0.20166(16) 0.02914(12) 0.81900(8) 0.0283(4) Uani 1 1 d . . . C3 C -0.07888(17) 0.03969(13) 0.78964(8) 0.0334(4) Uani 1 1 d . . . H3 H -0.0283 0.0964 0.7941 0.04 Uiso 1 1 calc R . . C4 C -0.03625(16) -0.03612(14) 0.75437(9) 0.0343(4) Uani 1 1 d . . . C5 C -0.10740(17) -0.11978(13) 0.74704(8) 0.0338(4) Uani 1 1 d . . . C6 C -0.23041(17) -0.13100(12) 0.77449(8) 0.0310(4) Uani 1 1 d . . . C7 C 0.0818(2) -0.13690(16) 0.69510(11) 0.0555(6) Uani 1 1 d . . . H7A H 0.1583 -0.1744 0.7092 0.067 Uiso 1 1 calc R . . H7B H 0.0872 -0.1301 0.6499 0.067 Uiso 1 1 calc R . . C8 C -0.25510(17) 0.11478(13) 0.85562(8) 0.0328(4) Uani 1 1 d . . . H8 H -0.3289 0.0919 0.882 0.039 Uiso 1 1 calc R . . C9 C -0.15230(18) 0.15638(13) 0.89602(8) 0.0344(4) Uani 1 1 d . . . C10 C -0.06540(19) 0.18456(14) 0.92953(8) 0.0381(4) Uani 1 1 d . . . C11 C 0.2058(2) 0.12623(17) 0.96917(13) 0.0630(7) Uani 1 1 d . . . H11A H 0.2808 0.1423 0.9953 0.095 Uiso 1 1 calc R . . H11B H 0.2333 0.1259 0.926 0.095 Uiso 1 1 calc R . . H11C H 0.1726 0.0626 0.9804 0.095 Uiso 1 1 calc R . . C12 C 0.1317(2) 0.34065(16) 0.95887(11) 0.0529(5) Uani 1 1 d . . . H12A H 0.2055 0.3587 0.9852 0.079 Uiso 1 1 calc R . . H12B H 0.0602 0.3867 0.9644 0.079 Uiso 1 1 calc R . . H12C H 0.1596 0.3409 0.9158 0.079 Uiso 1 1 calc R . . C13 C 0.0155(2) 0.21403(19) 1.06201(9) 0.0588(6) Uani 1 1 d . . . H13A H 0.0877 0.2313 1.0895 0.088 Uiso 1 1 calc R . . H13B H -0.0151 0.1492 1.0719 0.088 Uiso 1 1 calc R . . H13C H -0.0565 0.2597 1.0673 0.088 Uiso 1 1 calc R . . C14 C -0.41118(16) -0.06531(12) 0.84080(7) 0.0275(4) Uani 1 1 d . . . C15 C -0.52984(16) -0.04634(12) 0.81014(8) 0.0296(4) Uani 1 1 d . . . C16 C -0.65205(17) -0.06771(14) 0.83717(8) 0.0342(4) Uani 1 1 d . . . H16 H -0.7306 -0.0567 0.815 0.041 Uiso 1 1 calc R . . C17 C -0.65703(17) -0.10536(13) 0.89707(8) 0.0342(4) Uani 1 1 d . . . C18 C -0.53988(18) -0.12098(13) 0.92938(8) 0.0325(4) Uani 1 1 d . . . C19 C -0.41913(17) -0.10248(12) 0.90126(8) 0.0296(4) Uani 1 1 d . . . C20 C -0.89273(19) -0.1195(2) 0.89516(10) 0.0577(6) Uani 1 1 d . . . H20A H -0.9651 -0.138 0.9222 0.087 Uiso 1 1 calc R . . H20B H -0.8914 -0.1617 0.8591 0.087 Uiso 1 1 calc R . . H20C H -0.9046 -0.0529 0.8818 0.087 Uiso 1 1 calc R . . C21 C -0.5640(3) -0.09049(17) 1.03571(10) 0.0672(7) Uani 1 1 d . . . H21A H -0.5647 -0.1227 1.0757 0.101 Uiso 1 1 calc R . . H21B H -0.6482 -0.0586 1.029 0.101 Uiso 1 1 calc R . . H21C H -0.4937 -0.0427 1.0349 0.101 Uiso 1 1 calc R . . C22 C -0.2669(2) -0.21755(15) 0.93746(11) 0.0514(5) Uani 1 1 d . . . H22A H -0.1854 -0.2234 0.9609 0.077 Uiso 1 1 calc R . . H22B H -0.2538 -0.2429 0.8959 0.077 Uiso 1 1 calc R . . H22C H -0.3362 -0.254 0.9581 0.077 Uiso 1 1 calc R . . C23 C -0.53220(16) 0.00040(13) 0.74843(8) 0.0296(4) Uani 1 1 d . . . C24 C -0.49901(18) 0.09195(14) 0.66543(8) 0.0357(4) Uani 1 1 d . . . H24 H -0.5179 0.1619 0.6603 0.043 Uiso 1 1 calc R . . C25 C -0.6259(2) 0.03403(19) 0.65732(9) 0.0513(6) Uani 1 1 d . . . H25A H -0.7036 0.0762 0.6601 0.062 Uiso 1 1 calc R . . H25B H -0.627 0.0005 0.6172 0.062 Uiso 1 1 calc R . . C26 C -0.3871(2) 0.06235(16) 0.62199(9) 0.0445(5) Uani 1 1 d . . . H26 H -0.3718 -0.008 0.6272 0.053 Uiso 1 1 calc R . . C27 C -0.4236(3) 0.08073(19) 0.55411(9) 0.0611(6) Uani 1 1 d . . . H27A H -0.3512 0.0605 0.5276 0.092 Uiso 1 1 calc R . . H27B H -0.4404 0.1493 0.548 0.092 Uiso 1 1 calc R . . H27C H -0.5023 0.044 0.5437 0.092 Uiso 1 1 calc R . . C28 C -0.2600(2) 0.1148(2) 0.63846(13) 0.0771(8) Uani 1 1 d . . . H28A H -0.1901 0.0942 0.6106 0.116 Uiso 1 1 calc R . . H28B H -0.2355 0.0996 0.6809 0.116 Uiso 1 1 calc R . . H28C H -0.2732 0.1841 0.6344 0.116 Uiso 1 1 calc R . . C29 C -0.3338(3) -0.2440(2) 0.70904(11) 0.0801(9) Uani 1 1 d . . . H29A H -0.3853 -0.3032 0.7105 0.12 Uiso 1 1 calc R . . H29B H -0.2527 -0.2554 0.6862 0.12 Uiso 1 1 calc R . . H29C H -0.3846 -0.1936 0.6886 0.12 Uiso 1 1 calc R . . N N -0.46244(15) 0.07187(11) 0.73101(6) 0.0339(3) Uani 1 1 d . . . O1 O -0.03809(13) -0.18587(10) 0.71176(7) 0.0513(4) Uani 1 1 d . . . O2 O 0.08212(13) -0.04430(11) 0.72343(7) 0.0558(4) Uani 1 1 d . . . O3 O -0.30374(14) 0.18806(10) 0.81496(7) 0.0418(3) Uani 1 1 d . . . HO3 H -0.352(2) 0.1569(17) 0.7880(11) 0.054(7) Uiso 1 1 d . . . O4 O -0.77040(12) -0.12821(11) 0.92808(6) 0.0440(3) Uani 1 1 d . . . O5 O -0.54253(13) -0.15937(9) 0.98845(5) 0.0413(3) Uani 1 1 d . . . O6 O -0.30434(12) -0.11778(9) 0.93380(6) 0.0368(3) Uani 1 1 d . . . O7 O -0.62336(12) -0.03485(11) 0.70833(6) 0.0447(3) Uani 1 1 d . . . O8 O -0.30312(13) -0.21451(9) 0.76981(6) 0.0415(3) Uani 1 1 d . . . Si Si 0.07371(5) 0.21761(4) 0.98031(2) 0.03798(13) 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 0.0216(8) 0.0302(9) 0.0278(8) 0.0034(7) -0.0017(7) 0.0020(7) C2 0.0222(8) 0.0307(9) 0.0320(9) -0.0007(7) -0.0019(7) 0.0008(7) C3 0.0210(8) 0.0355(9) 0.0438(10) -0.0045(8) -0.0011(8) -0.0038(8) C4 0.0180(8) 0.0421(10) 0.0429(9) -0.0037(9) 0.0024(8) -0.0002(8) C5 0.0274(9) 0.0339(10) 0.0402(10) -0.0069(8) -0.0001(8) 0.0049(8) C6 0.0265(9) 0.0295(9) 0.0369(9) 0.0010(8) -0.0013(8) -0.0017(7) C7 0.0355(11) 0.0594(13) 0.0715(14) -0.0249(12) 0.0124(11) -0.0018(11) C8 0.0272(9) 0.0356(9) 0.0356(9) -0.0049(8) 0.0020(8) -0.0026(8) C9 0.0338(10) 0.0357(10) 0.0336(9) -0.0042(8) 0.0063(9) -0.0007(9) C10 0.0358(10) 0.0413(10) 0.0373(10) -0.0053(8) 0.0013(9) -0.0023(9) C11 0.0453(13) 0.0502(13) 0.0935(19) -0.0051(13) -0.0023(13) 0.0046(11) C12 0.0480(12) 0.0465(12) 0.0642(13) -0.0017(10) -0.0107(11) -0.0040(10) C13 0.0543(13) 0.0744(16) 0.0478(12) -0.0048(12) -0.0123(11) -0.0094(13) C14 0.0236(8) 0.0276(8) 0.0313(9) 0.0008(7) -0.0001(7) -0.0018(7) C15 0.0241(8) 0.0341(9) 0.0306(8) 0.0048(7) 0.0007(7) -0.0001(8) C16 0.0231(9) 0.0445(11) 0.0351(10) 0.0082(8) -0.0027(8) -0.0006(8) C17 0.0257(9) 0.0394(10) 0.0374(10) 0.0053(8) 0.0044(8) -0.0060(8) C18 0.0320(10) 0.0340(9) 0.0315(9) 0.0078(8) 0.0009(8) -0.0036(8) C19 0.0274(9) 0.0289(9) 0.0326(9) 0.0042(7) -0.0048(8) -0.0025(8) C20 0.0257(11) 0.0950(19) 0.0524(13) 0.0087(13) 0.0050(9) -0.0121(11) C21 0.105(2) 0.0571(14) 0.0399(11) 0.0045(10) -0.0099(13) -0.0178(15) C22 0.0458(12) 0.0437(11) 0.0648(14) 0.0109(10) -0.0187(11) 0.0075(10) C23 0.0193(8) 0.0406(10) 0.0290(8) 0.0012(7) -0.0006(7) 0.0030(8) C24 0.0334(10) 0.0415(10) 0.0321(9) 0.0079(8) -0.0020(8) 0.0030(8) C25 0.0389(11) 0.0808(16) 0.0340(11) 0.0171(11) -0.0076(9) -0.0054(11) C26 0.0420(11) 0.0505(12) 0.0410(11) 0.0116(9) 0.0109(9) 0.0031(10) C27 0.0685(16) 0.0745(16) 0.0403(11) 0.0112(11) 0.0161(11) 0.0028(14) C28 0.0416(14) 0.114(2) 0.0758(16) 0.0185(16) 0.0102(13) -0.0155(15) C29 0.102(2) 0.084(2) 0.0543(14) -0.0129(13) -0.0027(14) -0.0603(17) N 0.0327(8) 0.0370(8) 0.0321(8) 0.0064(6) 0.0006(7) 0.0006(7) O1 0.0365(7) 0.0430(8) 0.0743(9) -0.0212(7) 0.0160(7) 0.0005(6) O2 0.0268(7) 0.0556(9) 0.0849(10) -0.0258(8) 0.0227(7) -0.0042(7) O3 0.0398(8) 0.0367(7) 0.0489(8) -0.0071(7) -0.0105(7) 0.0064(6) O4 0.0263(7) 0.0631(9) 0.0426(7) 0.0123(7) 0.0052(6) -0.0075(6) O5 0.0446(8) 0.0461(7) 0.0332(7) 0.0129(6) 0.0034(6) -0.0043(6) O6 0.0316(7) 0.0385(7) 0.0405(7) 0.0077(6) -0.0108(6) -0.0014(6) O7 0.0314(7) 0.0674(9) 0.0354(7) 0.0126(7) -0.0087(6) -0.0154(7) O8 0.0448(8) 0.0333(7) 0.0465(7) -0.0052(6) 0.0057(6) -0.0120(6) Si 0.0333(3) 0.0382(3) 0.0425(3) -0.0045(2) -0.0061(2) -0.0017(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.388(2) . ? C1 C6 1.408(2) . ? C1 C14 1.505(2) . ? C2 C3 1.401(2) . ? C2 C8 1.520(2) . ? C3 C4 1.363(3) . ? C3 H3 0.94 . ? C4 C5 1.370(3) . ? C4 O2 1.375(2) . ? C5 O1 1.379(2) . ? C5 C6 1.387(2) . ? C6 O8 1.371(2) . ? C7 O2 1.416(2) . ? C7 O1 1.434(3) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C8 O3 1.425(2) . ? C8 C9 1.473(3) . ? C8 H8 0.99 . ? C9 C10 1.202(3) . ? C10 Si 1.840(2) . ? C11 Si 1.853(2) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C11 H11C 0.97 . ? C12 Si 1.855(2) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C12 H12C 0.97 . ? C13 Si 1.856(2) . ? C13 H13A 0.97 . ? C13 H13B 0.97 . ? C13 H13C 0.97 . ? C14 C15 1.395(2) . ? C14 C19 1.402(2) . ? C15 C16 1.398(2) . ? C15 C23 1.477(2) . ? C16 C17 1.391(3) . ? C16 H16 0.94 . ? C17 O4 1.364(2) . ? C17 C18 1.391(3) . ? C18 O5 1.3783(19) . ? C18 C19 1.387(2) . ? C19 O6 1.373(2) . ? C20 O4 1.431(2) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C20 H20C 0.97 . ? C21 O5 1.409(3) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C21 H21C 0.97 . ? C22 O6 1.430(2) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C22 H22C 0.97 . ? C23 N 1.269(2) . ? C23 O7 1.354(2) . ? C24 N 1.486(2) . ? C24 C25 1.523(3) . ? C24 C26 1.525(3) . ? C24 H24 0.99 . ? C25 O7 1.453(2) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C26 C28 1.517(3) . ? C26 C27 1.529(3) . ? C26 H26 0.99 . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? C27 H27C 0.97 . ? C28 H28A 0.97 . ? C28 H28B 0.97 . ? C28 H28C 0.97 . ? C29 O8 1.405(3) . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C29 H29C 0.97 . ? O3 HO3 0.87(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.40(15) . . ? C2 C1 C14 122.13(14) . . ? C6 C1 C14 117.47(15) . . ? C1 C2 C3 121.34(15) . . ? C1 C2 C8 120.53(14) . . ? C3 C2 C8 117.94(15) . . ? C4 C3 C2 116.88(16) . . ? C4 C3 H3 121.6 . . ? C2 C3 H3 121.6 . . ? C3 C4 C5 123.02(16) . . ? C3 C4 O2 127.50(17) . . ? C5 C4 O2 109.43(15) . . ? C4 C5 O1 110.71(15) . . ? C4 C5 C6 121.12(16) . . ? O1 C5 C6 128.14(17) . . ? O8 C6 C5 122.97(16) . . ? O8 C6 C1 119.74(15) . . ? C5 C6 C1 117.21(16) . . ? O2 C7 O1 108.64(15) . . ? O2 C7 H7A 110 . . ? O1 C7 H7A 110 . . ? O2 C7 H7B 110 . . ? O1 C7 H7B 110 . . ? H7A C7 H7B 108.3 . . ? O3 C8 C9 109.29(15) . . ? O3 C8 C2 110.84(14) . . ? C9 C8 C2 110.99(15) . . ? O3 C8 H8 108.6 . . ? C9 C8 H8 108.6 . . ? C2 C8 H8 108.6 . . ? C10 C9 C8 175.9(2) . . ? C9 C10 Si 175.25(17) . . ? Si C11 H11A 109.5 . . ? Si C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si C12 H12A 109.5 . . ? Si C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si C13 H13A 109.5 . . ? Si C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 117.32(15) . . ? C15 C14 C1 123.54(14) . . ? C19 C14 C1 119.04(14) . . ? C14 C15 C16 121.64(14) . . ? C14 C15 C23 121.44(14) . . ? C16 C15 C23 116.90(14) . . ? C17 C16 C15 119.79(16) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? O4 C17 C18 115.83(15) . . ? O4 C17 C16 124.79(16) . . ? C18 C17 C16 119.38(16) . . ? O5 C18 C19 119.39(15) . . ? O5 C18 C17 120.30(15) . . ? C19 C18 C17 120.23(14) . . ? O6 C19 C18 119.60(14) . . ? O6 C19 C14 118.81(15) . . ? C18 C19 C14 121.56(15) . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O6 C22 H22A 109.5 . . ? O6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N C23 O7 117.99(15) . . ? N C23 C15 126.59(16) . . ? O7 C23 C15 115.33(15) . . ? N C24 C25 102.77(15) . . ? N C24 C26 110.38(15) . . ? C25 C24 C26 114.56(17) . . ? N C24 H24 109.6 . . ? C25 C24 H24 109.6 . . ? C26 C24 H24 109.6 . . ? O7 C25 C24 103.97(14) . . ? O7 C25 H25A 111 . . ? C24 C25 H25A 111 . . ? O7 C25 H25B 111 . . ? C24 C25 H25B 111 . . ? H25A C25 H25B 109 . . ? C28 C26 C24 110.98(19) . . ? C28 C26 C27 110.44(19) . . ? C24 C26 C27 111.27(17) . . ? C28 C26 H26 108 . . ? C24 C26 H26 108 . . ? C27 C26 H26 108 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O8 C29 H29A 109.5 . . ? O8 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O8 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23 N C24 106.70(15) . . ? C5 O1 C7 104.85(14) . . ? C4 O2 C7 106.30(15) . . ? C8 O3 HO3 104.6(15) . . ? C17 O4 C20 117.72(14) . . ? C18 O5 C21 114.22(15) . . ? C19 O6 C22 113.59(14) . . ? C23 O7 C25 105.04(14) . . ? C6 O8 C29 115.48(15) . . ? C10 Si C11 107.83(10) . . ? C10 Si C12 108.71(9) . . ? C11 Si C12 111.26(11) . . ? C10 Si C13 108.31(9) . . ? C11 Si C13 109.48(12) . . ? C12 Si C13 111.15(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.9(2) . . . . ? C14 C1 C2 C3 -178.31(15) . . . . ? C6 C1 C2 C8 176.77(15) . . . . ? C14 C1 C2 C8 -3.5(2) . . . . ? C1 C2 C3 C4 -1.6(3) . . . . ? C8 C2 C3 C4 -176.59(16) . . . . ? C2 C3 C4 C5 -0.1(3) . . . . ? C2 C3 C4 O2 -177.15(17) . . . . ? C3 C4 C5 O1 -176.89(17) . . . . ? O2 C4 C5 O1 0.6(2) . . . . ? C3 C4 C5 C6 1.6(3) . . . . ? O2 C4 C5 C6 179.08(16) . . . . ? C4 C5 C6 O8 -178.06(17) . . . . ? O1 C5 C6 O8 0.1(3) . . . . ? C4 C5 C6 C1 -1.2(3) . . . . ? O1 C5 C6 C1 176.92(17) . . . . ? C2 C1 C6 O8 176.47(15) . . . . ? C14 C1 C6 O8 -3.3(2) . . . . ? C2 C1 C6 C5 -0.5(2) . . . . ? C14 C1 C6 C5 179.76(15) . . . . ? C1 C2 C8 O3 -99.85(18) . . . . ? C3 C2 C8 O3 75.17(19) . . . . ? C1 C2 C8 C9 138.51(16) . . . . ? C3 C2 C8 C9 -46.5(2) . . . . ? C2 C1 C14 C15 97.0(2) . . . . ? C6 C1 C14 C15 -83.3(2) . . . . ? C2 C1 C14 C19 -87.0(2) . . . . ? C6 C1 C14 C19 92.80(19) . . . . ? C19 C14 C15 C16 -3.0(3) . . . . ? C1 C14 C15 C16 173.13(17) . . . . ? C19 C14 C15 C23 174.86(16) . . . . ? C1 C14 C15 C23 -9.0(3) . . . . ? C14 C15 C16 C17 2.5(3) . . . . ? C23 C15 C16 C17 -175.42(17) . . . . ? C15 C16 C17 O4 179.55(18) . . . . ? C15 C16 C17 C18 0.2(3) . . . . ? O4 C17 C18 O5 1.4(3) . . . . ? C16 C17 C18 O5 -179.17(16) . . . . ? O4 C17 C18 C19 178.25(17) . . . . ? C16 C17 C18 C19 -2.3(3) . . . . ? O5 C18 C19 O6 -3.5(2) . . . . ? C17 C18 C19 O6 179.69(17) . . . . ? O5 C18 C19 C14 178.70(16) . . . . ? C17 C18 C19 C14 1.8(3) . . . . ? C15 C14 C19 O6 -177.05(15) . . . . ? C1 C14 C19 O6 6.6(2) . . . . ? C15 C14 C19 C18 0.8(3) . . . . ? C1 C14 C19 C18 -175.50(16) . . . . ? C14 C15 C23 N -42.7(3) . . . . ? C16 C15 C23 N 135.30(19) . . . . ? C14 C15 C23 O7 140.80(17) . . . . ? C16 C15 C23 O7 -41.2(2) . . . . ? N C24 C25 O7 -18.32(19) . . . . ? C26 C24 C25 O7 101.43(18) . . . . ? N C24 C26 C28 -57.6(2) . . . . ? C25 C24 C26 C28 -173.01(19) . . . . ? N C24 C26 C27 178.99(17) . . . . ? C25 C24 C26 C27 63.6(2) . . . . ? O7 C23 N C24 -4.0(2) . . . . ? C15 C23 N C24 179.51(16) . . . . ? C25 C24 N C23 14.02(19) . . . . ? C26 C24 N C23 -108.59(17) . . . . ? C4 C5 O1 C7 -1.9(2) . . . . ? C6 C5 O1 C7 179.77(19) . . . . ? O2 C7 O1 C5 2.5(2) . . . . ? C3 C4 O2 C7 178.3(2) . . . . ? C5 C4 O2 C7 1.0(2) . . . . ? O1 C7 O2 C4 -2.2(2) . . . . ? C18 C17 O4 C20 -175.88(19) . . . . ? C16 C17 O4 C20 4.8(3) . . . . ? C19 C18 O5 C21 99.1(2) . . . . ? C17 C18 O5 C21 -84.1(2) . . . . ? C18 C19 O6 C22 78.0(2) . . . . ? C14 C19 O6 C22 -104.09(19) . . . . ? N C23 O7 C25 -8.5(2) . . . . ? C15 C23 O7 C25 168.38(16) . . . . ? C24 C25 O7 C23 16.4(2) . . . . ? C5 C6 O8 C29 -58.1(3) . . . . ? C1 C6 O8 C29 125.2(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 HO3 N 0.87(2) 2.03(3) 2.901(2) 174(2) . #END OF CIF # Attachment '- 47 archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-06-08 at 14:10:43 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : shelxl dreduc import struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_RajanBabu1793 _database_code_depnum_ccdc_archive 'CCDC 854086' #TrackingRef '- 47 archive.cif' _audit_creation_date 2011-06-08T14:10:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'RajanBabu 1793' _chemical_formula_moiety 'C38 H47 B1 O8 Sn1' _chemical_formula_sum 'C38 H47 B O8 Sn' _chemical_formula_weight 761.26 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8449(1) _cell_length_b 13.7385(1) _cell_length_c 14.5994(1) _cell_angle_alpha 78.148(1) _cell_angle_beta 75.225(1) _cell_angle_gamma 70.556(1) _cell_volume 1965.93(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8966 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'triangular-shaped chunk' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_special_details ;All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.0, which means that 90% of the reflections were measured at least 3.0 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. Lots of diffuse scattering was observed on the data collection frames. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.421657E-1 _diffrn_orient_matrix_ub_12 -0.827281E-1 _diffrn_orient_matrix_ub_13 0.367173E-1 _diffrn_orient_matrix_ub_21 0.573088E-1 _diffrn_orient_matrix_ub_22 0.445648E-1 _diffrn_orient_matrix_ub_23 -0.281777E-1 _diffrn_orient_matrix_ub_31 -0.126557E-1 _diffrn_orient_matrix_ub_32 0.374261E-1 _diffrn_orient_matrix_ub_33 0.595514E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 53507 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 8995 _reflns_number_gt 6497 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;There appears to be lots of disorder in the vicinity of the Sn(CH3)3 group. This was modeled with three positions for this group with one of the methyl carbon atoms, C(36), common to all three positions. Similarity restraints on the Sn-C bond lengths and C...C distances were used in the refinement. The occupancy factors for these three groups were restricted to sum to 1.0. The Sn atoms and atom C(36) were refined anisotropically, while the rest of the methyl carbon atoms were kept isotropic. There is a region of disordered solvent located near an inversion center. The SQUEEZE procedure of PLATON was used to account for it. The total volume of the solvent accessible void for this region is 207 Ang**3, and the electron count for this region is 28 electrons/unit cell. For each methyl group, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq (bonded carbon atom). The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+0.3574P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8995 _refine_ls_number_parameters 460 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.074 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.14 _refine_ls_restrained_S_all 1.223 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.061 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.07 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.0113(3) 0.28339(18) 0.65051(18) 0.0322(5) Uani 1 1 d . . . H1 H 0.0677 0.2754 0.6977 0.039 Uiso 1 1 calc R . . C2 C 0.0954(3) 0.21973(18) 0.56880(18) 0.0326(5) Uani 1 1 d . A . C3 C 0.2025(3) 0.12460(19) 0.59532(18) 0.0349(6) Uani 1 1 d . . . C4 C 0.1586(3) 0.0428(2) 0.6731(2) 0.0387(6) Uani 1 1 d . . . H4A H 0.072 0.0391 0.6657 0.046 Uiso 1 1 calc R . . H4B H 0.2251 -0.0262 0.6648 0.046 Uiso 1 1 calc R . . C5 C 0.1440(3) 0.0668(2) 0.77221(19) 0.0367(6) Uani 1 1 d . . . C6 C 0.0231(3) 0.1276(2) 0.82125(19) 0.0384(6) Uani 1 1 d . . . C7 C -0.1000(3) 0.1687(2) 0.78036(19) 0.0389(6) Uani 1 1 d . . . C8 C -0.1082(3) 0.2445(2) 0.70067(18) 0.0347(6) Uani 1 1 d . . . C9 C 0.2555(3) 0.0274(2) 0.8152(2) 0.0414(6) Uani 1 1 d . . . H9 H 0.3365 -0.0157 0.7828 0.05 Uiso 1 1 calc R . . C10 C 0.2485(3) 0.0509(2) 0.9050(2) 0.0452(7) Uani 1 1 d . . . C11 C 0.1317(3) 0.1170(2) 0.9510(2) 0.0452(7) Uani 1 1 d . . . C12 C 0.0189(3) 0.1534(2) 0.91006(19) 0.0416(7) Uani 1 1 d . . . C13 C 0.4668(4) -0.0621(3) 0.9149(3) 0.0666(10) Uani 1 1 d . . . H13A H 0.5312 -0.0822 0.9569 0.1 Uiso 1 1 calc R . . H13B H 0.5062 -0.0328 0.8516 0.1 Uiso 1 1 calc R . . H13C H 0.4438 -0.1235 0.9093 0.1 Uiso 1 1 calc R . . C14 C 0.1692(5) 0.2377(3) 1.0224(3) 0.0789(13) Uani 1 1 d . . . H14A H 0.1661 0.2564 1.0844 0.118 Uiso 1 1 calc R . . H14B H 0.1091 0.2951 0.988 0.118 Uiso 1 1 calc R . . H14C H 0.2606 0.2244 0.9848 0.118 Uiso 1 1 calc R . . C15 C -0.1525(4) 0.1926(3) 1.0492(2) 0.0683(11) Uani 1 1 d . . . H15A H -0.2336 0.2478 1.0709 0.102 Uiso 1 1 calc R . . H15B H -0.0877 0.1815 1.0892 0.102 Uiso 1 1 calc R . . H15C H -0.175 0.1279 1.0543 0.102 Uiso 1 1 calc R . . C16 C -0.2114(3) 0.1314(2) 0.8254(2) 0.0479(7) Uani 1 1 d . . . H16 H -0.2076 0.0792 0.8794 0.058 Uiso 1 1 calc R . . C17 C -0.3235(3) 0.1735(2) 0.7881(2) 0.0468(7) Uani 1 1 d . . . C18 C -0.5246(4) 0.2110(3) 0.7518(3) 0.0666(10) Uani 1 1 d . . . H18A H -0.5369 0.1633 0.7148 0.08 Uiso 1 1 calc R . . H18B H -0.6136 0.2509 0.7844 0.08 Uiso 1 1 calc R . . C19 C -0.3313(3) 0.2491(2) 0.7092(2) 0.0441(7) Uani 1 1 d . . . C20 C -0.2256(3) 0.2857(2) 0.6632(2) 0.0378(6) Uani 1 1 d . . . H20 H -0.231 0.3366 0.6082 0.045 Uiso 1 1 calc R . . C21 C 0.0578(3) 0.4456(2) 0.60374(18) 0.0362(6) Uani 1 1 d . . . H21A H 0.028 0.514 0.5651 0.043 Uiso 1 1 calc R . . H21B H 0.1434 0.4053 0.5671 0.043 Uiso 1 1 calc R . . C22 C 0.0814(3) 0.46260(19) 0.69540(19) 0.0384(6) Uani 1 1 d . . . C23 C -0.0202(4) 0.4841(3) 0.7747(2) 0.0648(10) Uani 1 1 d . . . H23 H -0.1073 0.4831 0.7744 0.078 Uiso 1 1 calc R . . C24 C 0.0066(5) 0.5071(4) 0.8552(3) 0.0834(13) Uani 1 1 d . . . H24 H -0.0637 0.5224 0.9092 0.1 Uiso 1 1 calc R . . C25 C 0.1266(6) 0.5082(3) 0.8583(3) 0.0811(14) Uani 1 1 d . . . H25 H 0.1415 0.5251 0.9137 0.097 Uiso 1 1 calc R . . C26 C 0.2282(5) 0.4855(4) 0.7829(3) 0.0833(15) Uani 1 1 d . . . H26 H 0.3147 0.4854 0.7859 0.1 Uiso 1 1 calc R . . C27 C 0.2077(4) 0.4621(3) 0.7008(3) 0.0616(10) Uani 1 1 d . . . H27 H 0.2801 0.4458 0.6482 0.074 Uiso 1 1 calc R . . C28 C 0.0672(3) 0.2427(2) 0.4813(2) 0.0411(6) Uani 1 1 d . . . H28A H 0.0246 0.3129 0.4587 0.049 Uiso 0.293(8) 1 calc PR A 1 H28B H -0.0061 0.3031 0.4734 0.049 Uiso 0.369(6) 1 calc PR B 2 H28C H 0.0144 0.3117 0.4645 0.049 Uiso 0.327(9) 1 calc PR C 3 C29 C 0.3320(3) 0.1114(2) 0.55452(19) 0.0410(6) Uani 1 1 d . . . H29 H 0.3926 0.045 0.5692 0.049 Uiso 1 1 calc R . . C30 C 0.4259(4) 0.3479(3) 0.4140(3) 0.0760(14) Uani 1 1 d . . . C31 C 0.5513(4) 0.2616(3) 0.3824(2) 0.0564(9) Uani 1 1 d . . . C32 C 0.4489(7) 0.4365(4) 0.4493(5) 0.148(4) Uani 1 1 d . . . H32A H 0.3631 0.4886 0.468 0.222 Uiso 1 1 calc R . . H32B H 0.5066 0.469 0.398 0.222 Uiso 1 1 calc R . . H32C H 0.492 0.4087 0.5045 0.222 Uiso 1 1 calc R . . C33 C 0.3357(6) 0.3879(7) 0.3401(5) 0.225(7) Uani 1 1 d . . . H33A H 0.2563 0.4433 0.3639 0.337 Uiso 1 1 calc R . . H33B H 0.3083 0.3306 0.3296 0.337 Uiso 1 1 calc R . . H33C H 0.3848 0.4154 0.2798 0.337 Uiso 1 1 calc R . . C34 C 0.6082(4) 0.2633(3) 0.2758(2) 0.0645(10) Uani 1 1 d . . . H34A H 0.6888 0.2041 0.2648 0.097 Uiso 1 1 calc R . . H34B H 0.6306 0.3284 0.2501 0.097 Uiso 1 1 calc R . . H34C H 0.5417 0.2585 0.2437 0.097 Uiso 1 1 calc R . . C35 C 0.6605(5) 0.2466(4) 0.4377(3) 0.0843(14) Uani 1 1 d . . . H35A H 0.7393 0.1902 0.4149 0.126 Uiso 1 1 calc R . . H35B H 0.6273 0.2288 0.506 0.126 Uiso 1 1 calc R . . H35C H 0.6847 0.3112 0.4273 0.126 Uiso 1 1 calc R . . B B 0.3919(3) 0.1938(3) 0.4859(2) 0.0410(7) Uani 1 1 d . . . O1 O 0.3489(2) 0.01411(18) 0.95438(17) 0.0562(6) Uani 1 1 d . . . O2 O 0.1284(3) 0.14688(18) 1.03684(14) 0.0550(6) Uani 1 1 d . . . O3 O -0.0962(2) 0.22253(17) 0.95179(14) 0.0511(5) Uani 1 1 d . . . O4 O -0.4450(2) 0.1526(2) 0.82081(18) 0.0626(7) Uani 1 1 d . . . O5 O -0.4576(2) 0.28041(19) 0.68941(16) 0.0549(6) Uani 1 1 d . . . O6 O -0.03933(18) 0.39170(13) 0.61674(12) 0.0336(4) Uani 1 1 d . . . O7 O 0.3519(3) 0.29569(16) 0.49543(17) 0.0638(7) Uani 1 1 d . . . O8 O 0.5039(2) 0.16910(16) 0.41517(15) 0.0519(6) Uani 1 1 d . . . C36 C -0.0035(5) 0.1847(3) 0.2867(3) 0.0728(11) Uani 1 1 d D . . H361 H -0.0966 0.2165 0.3164 0.109 Uiso 0.293(8) 1 calc PR A 1 H362 H 0.0019 0.1268 0.2547 0.109 Uiso 0.293(8) 1 calc PR A 1 H363 H 0.0299 0.2368 0.2396 0.109 Uiso 0.293(8) 1 calc PR A 1 H364 H -0.0493 0.2592 0.2736 0.109 Uiso 0.369(6) 1 calc PR B 2 H365 H -0.066 0.1499 0.33 0.109 Uiso 0.369(6) 1 calc PR B 2 H366 H 0.0296 0.1544 0.2266 0.109 Uiso 0.369(6) 1 calc PR B 2 H367 H -0.0138 0.2578 0.26 0.109 Uiso 0.327(9) 1 calc PR C 3 H368 H -0.0899 0.1772 0.3233 0.109 Uiso 0.327(9) 1 calc PR C 3 H369 H 0.0286 0.1417 0.2345 0.109 Uiso 0.327(9) 1 calc PR C 3 Sn1A Sn 0.1147(6) 0.1278(5) 0.3938(5) 0.0444(11) Uani 0.293(8) 1 d PD A 1 C37A C 0.0546(16) -0.0055(11) 0.4692(10) 0.082(5) Uiso 0.293(8) 1 d PD A 1 H371 H -0.0393 0.017 0.5017 0.123 Uiso 0.293(8) 1 calc PR A 1 H372 H 0.1102 -0.0417 0.5165 0.123 Uiso 0.293(8) 1 calc PR A 1 H373 H 0.0652 -0.0528 0.4239 0.123 Uiso 0.293(8) 1 calc PR A 1 C38A C 0.3130(12) 0.0623(18) 0.3247(15) 0.143(10) Uiso 0.293(8) 1 d PD A 1 H381 H 0.3157 0.0109 0.2859 0.214 Uiso 0.293(8) 1 calc PR A 1 H382 H 0.3683 0.0281 0.3726 0.214 Uiso 0.293(8) 1 calc PR A 1 H383 H 0.3474 0.1173 0.2833 0.214 Uiso 0.293(8) 1 calc PR A 1 Sn1B Sn 0.1620(3) 0.1640(2) 0.35220(17) 0.0385(5) Uani 0.369(6) 1 d PD A 2 C37B C 0.2678(12) 0.0065(8) 0.3769(9) 0.087(4) Uiso 0.369(6) 1 d PD A 2 H374 H 0.2149 -0.0284 0.4298 0.13 Uiso 0.369(6) 1 calc PR B 2 H375 H 0.3527 -0.0002 0.3932 0.13 Uiso 0.369(6) 1 calc PR B 2 H376 H 0.2853 -0.0259 0.3191 0.13 Uiso 0.369(6) 1 calc PR B 2 C38B C 0.2923(10) 0.2266(8) 0.2369(7) 0.068(3) Uiso 0.369(6) 1 d PD A 2 H384 H 0.2503 0.3013 0.2209 0.102 Uiso 0.369(6) 1 calc PR B 2 H385 H 0.3097 0.1913 0.181 0.102 Uiso 0.369(6) 1 calc PR B 2 H386 H 0.3768 0.2158 0.256 0.102 Uiso 0.369(6) 1 calc PR B 2 Sn1C Sn 0.1303(5) 0.1376(4) 0.3739(4) 0.0415(10) Uani 0.327(9) 1 d PD A 3 C37C C 0.1637(12) -0.0183(7) 0.4327(8) 0.065(4) Uiso 0.327(9) 1 d PD A 3 H377 H 0.229 -0.0368 0.4737 0.097 Uiso 0.327(9) 1 calc PR C 3 H378 H 0.198 -0.0622 0.3812 0.097 Uiso 0.327(9) 1 calc PR C 3 H379 H 0.0796 -0.0292 0.4707 0.097 Uiso 0.327(9) 1 calc PR C 3 C38C C 0.3150(10) 0.1364(11) 0.2710(9) 0.080(4) Uiso 0.327(9) 1 d PD A 3 H387 H 0.3891 0.1155 0.3047 0.121 Uiso 0.327(9) 1 calc PR C 3 H388 H 0.3075 0.2063 0.2357 0.121 Uiso 0.327(9) 1 calc PR C 3 H389 H 0.3317 0.087 0.2263 0.121 Uiso 0.327(9) 1 calc PR C 3 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 0.0377(14) 0.0265(12) 0.0318(12) 0.0035(10) -0.0121(11) -0.0092(10) C2 0.0373(14) 0.0257(11) 0.0358(13) 0.0001(10) -0.0113(11) -0.0104(10) C3 0.0452(16) 0.0283(12) 0.0323(13) -0.0047(10) -0.0142(11) -0.0073(11) C4 0.0462(16) 0.0276(12) 0.0441(15) 0.0007(11) -0.0174(12) -0.0106(12) C5 0.0451(16) 0.0297(12) 0.0378(14) 0.0098(11) -0.0172(12) -0.0164(12) C6 0.0453(16) 0.0351(13) 0.0361(14) 0.0105(11) -0.0149(12) -0.0179(12) C7 0.0427(16) 0.0380(14) 0.0371(14) 0.0029(11) -0.0118(12) -0.0151(12) C8 0.0375(14) 0.0318(12) 0.0353(13) -0.0003(10) -0.0108(11) -0.0107(11) C9 0.0466(17) 0.0337(13) 0.0443(15) 0.0074(12) -0.0170(13) -0.0137(12) C10 0.0541(19) 0.0381(14) 0.0492(16) 0.0135(13) -0.0287(14) -0.0188(14) C11 0.062(2) 0.0428(15) 0.0344(14) 0.0091(12) -0.0198(13) -0.0213(15) C12 0.0486(17) 0.0388(14) 0.0344(14) 0.0087(11) -0.0104(12) -0.0159(13) C13 0.066(2) 0.0520(19) 0.087(3) -0.0096(18) -0.046(2) -0.0020(17) C14 0.120(4) 0.071(3) 0.063(2) -0.011(2) -0.031(2) -0.042(3) C15 0.067(2) 0.084(3) 0.0417(18) 0.0069(18) 0.0007(16) -0.025(2) C16 0.0488(18) 0.0467(16) 0.0486(17) 0.0095(14) -0.0123(14) -0.0220(14) C17 0.0463(18) 0.0490(17) 0.0495(17) 0.0011(14) -0.0119(13) -0.0226(14) C18 0.049(2) 0.075(2) 0.080(3) 0.006(2) -0.0211(18) -0.0270(19) C19 0.0374(16) 0.0467(16) 0.0496(16) -0.0055(13) -0.0155(13) -0.0097(13) C20 0.0383(15) 0.0367(13) 0.0384(14) -0.0003(11) -0.0129(12) -0.0099(12) C21 0.0483(16) 0.0297(12) 0.0311(13) -0.0033(10) -0.0079(11) -0.0129(12) C22 0.0558(18) 0.0244(12) 0.0349(13) -0.0024(10) -0.0148(12) -0.0082(12) C23 0.052(2) 0.089(3) 0.0449(18) -0.0227(17) -0.0082(15) -0.0031(19) C24 0.100(4) 0.090(3) 0.048(2) -0.031(2) -0.014(2) 0.000(3) C25 0.147(5) 0.069(2) 0.053(2) -0.0005(19) -0.052(3) -0.046(3) C26 0.112(4) 0.105(3) 0.067(3) 0.017(2) -0.048(3) -0.070(3) C27 0.066(2) 0.082(2) 0.0474(18) 0.0053(17) -0.0155(16) -0.040(2) C28 0.0486(17) 0.0310(13) 0.0430(15) -0.0060(11) -0.0202(13) -0.0022(12) C29 0.0474(17) 0.0331(13) 0.0368(14) -0.0022(11) -0.0127(12) -0.0026(12) C30 0.078(3) 0.0460(18) 0.065(2) 0.0042(17) 0.031(2) -0.0087(18) C31 0.062(2) 0.0532(18) 0.0408(16) 0.0006(14) 0.0007(15) -0.0117(16) C32 0.173(6) 0.057(3) 0.154(5) -0.031(3) 0.104(5) -0.049(3) C33 0.065(3) 0.256(9) 0.159(6) 0.156(7) 0.032(4) 0.054(5) C34 0.061(2) 0.069(2) 0.0407(17) 0.0008(16) 0.0063(15) -0.0062(18) C35 0.099(3) 0.117(4) 0.055(2) -0.006(2) -0.007(2) -0.065(3) B 0.0426(18) 0.0406(16) 0.0320(15) -0.0031(13) -0.0078(13) -0.0034(14) O1 0.0614(15) 0.0527(12) 0.0604(13) 0.0008(11) -0.0381(11) -0.0102(11) O2 0.0774(16) 0.0556(13) 0.0378(11) 0.0038(10) -0.0259(11) -0.0225(12) O3 0.0569(14) 0.0552(12) 0.0320(10) 0.0043(9) -0.0077(9) -0.0119(11) O4 0.0466(14) 0.0767(16) 0.0679(15) 0.0118(13) -0.0127(11) -0.0346(13) O5 0.0381(12) 0.0674(14) 0.0598(13) 0.0023(11) -0.0180(10) -0.0169(11) O6 0.0398(10) 0.0252(8) 0.0355(9) 0.0006(7) -0.0135(8) -0.0075(8) O7 0.0690(16) 0.0377(11) 0.0598(14) -0.0071(10) 0.0255(12) -0.0120(11) O8 0.0548(13) 0.0413(11) 0.0449(11) -0.0030(9) -0.0003(10) -0.0040(10) C36 0.100(3) 0.075(2) 0.053(2) -0.0074(18) -0.036(2) -0.023(2) Sn1A 0.0383(11) 0.0519(13) 0.046(2) -0.0223(14) -0.0082(14) -0.0080(10) Sn1B 0.0453(9) 0.0380(7) 0.0293(6) -0.0094(5) -0.0134(6) -0.0013(4) Sn1C 0.0450(17) 0.0559(14) 0.033(2) -0.0128(14) -0.0083(15) -0.0226(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 1.432(3) . ? C1 C8 1.522(4) . ? C1 C2 1.537(4) . ? C1 H1 1 . ? C2 C28 1.339(4) . ? C2 C3 1.489(4) . ? C3 C29 1.344(4) . ? C3 C4 1.528(4) . ? C4 C5 1.508(4) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C9 1.400(4) . ? C5 C6 1.403(4) . ? C6 C12 1.399(4) . ? C6 C7 1.491(4) . ? C7 C8 1.392(4) . ? C7 C16 1.422(4) . ? C8 C20 1.410(4) . ? C9 C10 1.392(4) . ? C9 H9 0.95 . ? C10 O1 1.358(3) . ? C10 C11 1.389(5) . ? C11 O2 1.385(4) . ? C11 C12 1.395(4) . ? C12 O3 1.375(4) . ? C13 O1 1.430(5) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 O2 1.417(4) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 O3 1.432(4) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C17 1.360(4) . ? C16 H16 0.95 . ? C17 C19 1.383(4) . ? C17 O4 1.386(4) . ? C18 O5 1.426(4) . ? C18 O4 1.433(4) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.368(4) . ? C19 O5 1.380(4) . ? C20 H20 0.95 . ? C21 O6 1.432(3) . ? C21 C22 1.502(4) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 C23 1.383(5) . ? C22 C27 1.390(5) . ? C23 C24 1.398(6) . ? C23 H23 0.95 . ? C24 C25 1.320(7) . ? C24 H24 0.95 . ? C25 C26 1.348(7) . ? C25 H25 0.95 . ? C26 C27 1.390(6) . ? C26 H26 0.95 . ? C27 H27 0.95 . ? C28 Sn1A 2.084(7) . ? C28 Sn1C 2.176(6) . ? C28 Sn1B 2.211(3) . ? C28 H28A 0.95 . ? C28 H28B 0.95 . ? C28 H28C 0.95 . ? C29 B 1.549(4) . ? C29 H29 0.95 . ? C30 O7 1.455(4) . ? C30 C31 1.516(5) . ? C30 C32 1.529(8) . ? C30 C33 1.536(10) . ? C31 O8 1.472(4) . ? C31 C34 1.520(5) . ? C31 C35 1.533(6) . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? B O7 1.346(4) . ? B O8 1.374(4) . ? C36 Sn1C 2.031(6) . ? C36 Sn1A 2.134(7) . ? C36 Sn1B 2.155(5) . ? C36 H361 0.98 . ? C36 H362 0.98 . ? C36 H363 0.98 . ? C36 H364 0.98 . ? C36 H365 0.98 . ? C36 H366 0.98 . ? C36 H367 0.98 . ? C36 H368 0.98 . ? C36 H369 0.98 . ? Sn1A C38A 2.105(13) . ? Sn1A C37A 2.143(11) . ? C37A H371 0.98 . ? C37A H372 0.98 . ? C37A H373 0.98 . ? C38A H381 0.98 . ? C38A H382 0.98 . ? C38A H383 0.98 . ? Sn1B C37B 2.090(10) . ? Sn1B C38B 2.138(9) . ? C37B H374 0.98 . ? C37B H375 0.98 . ? C37B H376 0.98 . ? C38B H384 0.98 . ? C38B H385 0.98 . ? C38B H386 0.98 . ? Sn1C C37C 2.084(9) . ? Sn1C C38C 2.173(10) . ? C37C H377 0.98 . ? C37C H378 0.98 . ? C37C H379 0.98 . ? C38C H387 0.98 . ? C38C H388 0.98 . ? C38C H389 0.98 . ? 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 O6 C1 C8 107.4(2) . . ? O6 C1 C2 112.04(19) . . ? C8 C1 C2 110.2(2) . . ? O6 C1 H1 109 . . ? C8 C1 H1 109 . . ? C2 C1 H1 109 . . ? C28 C2 C3 121.7(2) . . ? C28 C2 C1 122.4(2) . . ? C3 C2 C1 115.7(2) . . ? C29 C3 C2 122.1(2) . . ? C29 C3 C4 121.2(2) . . ? C2 C3 C4 116.7(2) . . ? C5 C4 C3 112.3(2) . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? C9 C5 C6 119.8(3) . . ? C9 C5 C4 118.4(3) . . ? C6 C5 C4 121.8(2) . . ? C12 C6 C5 118.9(3) . . ? C12 C6 C7 118.8(3) . . ? C5 C6 C7 122.2(3) . . ? C8 C7 C16 119.9(3) . . ? C8 C7 C6 121.0(2) . . ? C16 C7 C6 119.0(2) . . ? C7 C8 C20 121.3(2) . . ? C7 C8 C1 120.4(2) . . ? C20 C8 C1 118.3(2) . . ? C10 C9 C5 120.4(3) . . ? C10 C9 H9 119.8 . . ? C5 C9 H9 119.8 . . ? O1 C10 C11 114.9(3) . . ? O1 C10 C9 125.2(3) . . ? C11 C10 C9 119.9(3) . . ? O2 C11 C10 119.8(3) . . ? O2 C11 C12 120.5(3) . . ? C10 C11 C12 119.8(3) . . ? O3 C12 C11 121.0(3) . . ? O3 C12 C6 117.9(3) . . ? C11 C12 C6 120.9(3) . . ? O1 C13 H13A 109.5 . . ? O1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C7 117.3(2) . . ? C17 C16 H16 121.3 . . ? C7 C16 H16 121.3 . . ? C16 C17 C19 122.5(3) . . ? C16 C17 O4 128.1(3) . . ? C19 C17 O4 109.4(3) . . ? O5 C18 O4 108.3(3) . . ? O5 C18 H18A 110 . . ? O4 C18 H18A 110 . . ? O5 C18 H18B 110 . . ? O4 C18 H18B 110 . . ? H18A C18 H18B 108.4 . . ? C20 C19 O5 128.0(3) . . ? C20 C19 C17 121.8(3) . . ? O5 C19 C17 110.1(2) . . ? C19 C20 C8 117.1(2) . . ? C19 C20 H20 121.4 . . ? C8 C20 H20 121.4 . . ? O6 C21 C22 114.0(2) . . ? O6 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? O6 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C27 117.9(3) . . ? C23 C22 C21 122.3(3) . . ? C27 C22 C21 119.7(3) . . ? C22 C23 C24 119.3(4) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C25 C24 C23 122.0(4) . . ? C25 C24 H24 119 . . ? C23 C24 H24 119 . . ? C24 C25 C26 120.0(4) . . ? C24 C25 H25 120 . . ? C26 C25 H25 120 . . ? C25 C26 C27 120.7(4) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C22 C27 C26 120.1(4) . . ? C22 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C2 C28 Sn1A 121.4(3) . . ? C2 C28 Sn1C 126.5(2) . . ? C2 C28 Sn1B 131.0(2) . . ? C2 C28 H28A 119.3 . . ? Sn1A C28 H28A 119.3 . . ? C2 C28 H28B 114.5 . . ? Sn1B C28 H28B 114.5 . . ? C2 C28 H28C 116.8 . . ? Sn1C C28 H28C 116.8 . . ? C3 C29 B 126.4(3) . . ? C3 C29 H29 116.8 . . ? B C29 H29 116.8 . . ? O7 C30 C31 103.4(2) . . ? O7 C30 C32 107.1(3) . . ? C31 C30 C32 115.0(4) . . ? O7 C30 C33 105.2(4) . . ? C31 C30 C33 112.7(5) . . ? C32 C30 C33 112.3(5) . . ? O8 C31 C30 101.5(3) . . ? O8 C31 C34 107.4(3) . . ? C30 C31 C34 117.4(3) . . ? O8 C31 C35 105.9(3) . . ? C30 C31 C35 112.4(4) . . ? C34 C31 C35 111.0(3) . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O7 B O8 111.6(3) . . ? O7 B C29 124.5(3) . . ? O8 B C29 123.4(3) . . ? C10 O1 C13 117.4(3) . . ? C11 O2 C14 111.7(2) . . ? C12 O3 C15 117.0(3) . . ? C17 O4 C18 105.5(2) . . ? C19 O5 C18 105.5(2) . . ? C21 O6 C1 111.9(2) . . ? B O7 C30 107.8(2) . . ? B O8 C31 107.9(2) . . ? Sn1A C36 H361 109.5 . . ? Sn1A C36 H362 109.5 . . ? H361 C36 H362 109.5 . . ? Sn1A C36 H363 109.5 . . ? H361 C36 H363 109.5 . . ? H362 C36 H363 109.5 . . ? Sn1B C36 H364 109.5 . . ? Sn1B C36 H365 109.5 . . ? H364 C36 H365 109.5 . . ? Sn1B C36 H366 109.5 . . ? H364 C36 H366 109.5 . . ? H365 C36 H366 109.5 . . ? Sn1C C36 H367 109.5 . . ? Sn1C C36 H368 109.5 . . ? H367 C36 H368 109.5 . . ? Sn1C C36 H369 109.5 . . ? H367 C36 H369 109.5 . . ? H368 C36 H369 109.5 . . ? C28 Sn1A C38A 121.1(8) . . ? C28 Sn1A C36 108.7(3) . . ? C38A Sn1A C36 107.4(6) . . ? C28 Sn1A C37A 111.8(6) . . ? C38A Sn1A C37A 103.2(7) . . ? C36 Sn1A C37A 103.1(5) . . ? Sn1A C37A H371 109.5 . . ? Sn1A C37A H372 109.5 . . ? H371 C37A H372 109.5 . . ? Sn1A C37A H373 109.5 . . ? H371 C37A H373 109.5 . . ? H372 C37A H373 109.5 . . ? Sn1A C38A H381 109.5 . . ? Sn1A C38A H382 109.5 . . ? H381 C38A H382 109.5 . . ? Sn1A C38A H383 109.5 . . ? H381 C38A H383 109.5 . . ? H382 C38A H383 109.5 . . ? C37B Sn1B C38B 104.1(4) . . ? C37B Sn1B C36 111.0(4) . . ? C38B Sn1B C36 101.3(3) . . ? C37B Sn1B C28 115.5(4) . . ? C38B Sn1B C28 120.5(4) . . ? C36 Sn1B C28 103.46(18) . . ? Sn1B C37B H374 109.5 . . ? Sn1B C37B H375 109.5 . . ? H374 C37B H375 109.5 . . ? Sn1B C37B H376 109.5 . . ? H374 C37B H376 109.5 . . ? H375 C37B H376 109.5 . . ? Sn1B C38B H384 109.5 . . ? Sn1B C38B H385 109.5 . . ? H384 C38B H385 109.5 . . ? Sn1B C38B H386 109.5 . . ? H384 C38B H386 109.5 . . ? H385 C38B H386 109.5 . . ? C36 Sn1C C37C 112.9(4) . . ? C36 Sn1C C38C 101.2(4) . . ? C37C Sn1C C38C 102.8(5) . . ? C36 Sn1C C28 109.1(3) . . ? C37C Sn1C C28 113.0(4) . . ? C38C Sn1C C28 117.3(5) . . ? Sn1C C37C H377 109.5 . . ? Sn1C C37C H378 109.5 . . ? H377 C37C H378 109.5 . . ? Sn1C C37C H379 109.5 . . ? H377 C37C H379 109.5 . . ? H378 C37C H379 109.5 . . ? Sn1C C38C H387 109.5 . . ? Sn1C C38C H388 109.5 . . ? H387 C38C H388 109.5 . . ? Sn1C C38C H389 109.5 . . ? H387 C38C H389 109.5 . . ? H388 C38C H389 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 C1 C2 C28 -34.5(3) . . . . ? C8 C1 C2 C28 85.0(3) . . . . ? O6 C1 C2 C3 151.2(2) . . . . ? C8 C1 C2 C3 -89.3(3) . . . . ? C28 C2 C3 C29 65.4(4) . . . . ? C1 C2 C3 C29 -120.3(3) . . . . ? C28 C2 C3 C4 -115.7(3) . . . . ? C1 C2 C3 C4 58.6(3) . . . . ? C29 C3 C4 C5 94.8(3) . . . . ? C2 C3 C4 C5 -84.1(3) . . . . ? C3 C4 C5 C9 -89.8(3) . . . . ? C3 C4 C5 C6 89.7(3) . . . . ? C9 C5 C6 C12 4.2(3) . . . . ? C4 C5 C6 C12 -175.3(2) . . . . ? C9 C5 C6 C7 -178.0(2) . . . . ? C4 C5 C6 C7 2.5(4) . . . . ? C12 C6 C7 C8 110.0(3) . . . . ? C5 C6 C7 C8 -67.8(4) . . . . ? C12 C6 C7 C16 -68.4(4) . . . . ? C5 C6 C7 C16 113.8(3) . . . . ? C16 C7 C8 C20 0.1(4) . . . . ? C6 C7 C8 C20 -178.3(3) . . . . ? C16 C7 C8 C1 -178.7(3) . . . . ? C6 C7 C8 C1 2.9(4) . . . . ? O6 C1 C8 C7 -145.2(3) . . . . ? C2 C1 C8 C7 92.5(3) . . . . ? O6 C1 C8 C20 36.0(3) . . . . ? C2 C1 C8 C20 -86.3(3) . . . . ? C6 C5 C9 C10 -2.1(4) . . . . ? C4 C5 C9 C10 177.4(2) . . . . ? C5 C9 C10 O1 177.6(2) . . . . ? C5 C9 C10 C11 -2.4(4) . . . . ? O1 C10 C11 O2 5.1(4) . . . . ? C9 C10 C11 O2 -174.9(2) . . . . ? O1 C10 C11 C12 -175.4(2) . . . . ? C9 C10 C11 C12 4.7(4) . . . . ? O2 C11 C12 O3 2.4(4) . . . . ? C10 C11 C12 O3 -177.1(2) . . . . ? O2 C11 C12 C6 177.0(2) . . . . ? C10 C11 C12 C6 -2.5(4) . . . . ? C5 C6 C12 O3 172.8(2) . . . . ? C7 C6 C12 O3 -5.1(3) . . . . ? C5 C6 C12 C11 -1.9(4) . . . . ? C7 C6 C12 C11 -179.8(2) . . . . ? C8 C7 C16 C17 -0.7(5) . . . . ? C6 C7 C16 C17 177.7(3) . . . . ? C7 C16 C17 C19 0.4(5) . . . . ? C7 C16 C17 O4 -177.8(3) . . . . ? C16 C17 C19 C20 0.6(5) . . . . ? O4 C17 C19 C20 179.1(3) . . . . ? C16 C17 C19 O5 -177.6(3) . . . . ? O4 C17 C19 O5 0.9(4) . . . . ? O5 C19 C20 C8 176.6(3) . . . . ? C17 C19 C20 C8 -1.2(5) . . . . ? C7 C8 C20 C19 0.9(4) . . . . ? C1 C8 C20 C19 179.7(3) . . . . ? O6 C21 C22 C23 -36.3(4) . . . . ? O6 C21 C22 C27 146.9(3) . . . . ? C27 C22 C23 C24 1.8(5) . . . . ? C21 C22 C23 C24 -175.0(3) . . . . ? C22 C23 C24 C25 -0.6(7) . . . . ? C23 C24 C25 C26 -0.8(7) . . . . ? C24 C25 C26 C27 0.9(7) . . . . ? C23 C22 C27 C26 -1.7(5) . . . . ? C21 C22 C27 C26 175.2(3) . . . . ? C25 C26 C27 C22 0.4(6) . . . . ? C3 C2 C28 Sn1A 23.2(4) . . . . ? C1 C2 C28 Sn1A -150.8(3) . . . . ? C3 C2 C28 Sn1C 15.2(4) . . . . ? C1 C2 C28 Sn1C -158.8(3) . . . . ? C3 C2 C28 Sn1B -3.2(4) . . . . ? C1 C2 C28 Sn1B -177.2(2) . . . . ? C2 C3 C29 B 7.9(4) . . . . ? C4 C3 C29 B -170.9(3) . . . . ? O7 C30 C31 O8 27.1(4) . . . . ? C32 C30 C31 O8 143.4(4) . . . . ? C33 C30 C31 O8 -86.1(4) . . . . ? O7 C30 C31 C34 143.7(4) . . . . ? C32 C30 C31 C34 -99.9(5) . . . . ? C33 C30 C31 C34 30.6(6) . . . . ? O7 C30 C31 C35 -85.7(4) . . . . ? C32 C30 C31 C35 30.7(5) . . . . ? C33 C30 C31 C35 161.2(4) . . . . ? C3 C29 B O7 38.9(5) . . . . ? C3 C29 B O8 -149.8(3) . . . . ? C11 C10 O1 C13 174.1(3) . . . . ? C9 C10 O1 C13 -6.0(4) . . . . ? C10 C11 O2 C14 88.4(4) . . . . ? C12 C11 O2 C14 -91.1(4) . . . . ? C11 C12 O3 C15 -55.5(4) . . . . ? C6 C12 O3 C15 129.8(3) . . . . ? C16 C17 O4 C18 -175.4(4) . . . . ? C19 C17 O4 C18 6.2(4) . . . . ? O5 C18 O4 C17 -10.9(4) . . . . ? C20 C19 O5 C18 174.4(4) . . . . ? C17 C19 O5 C18 -7.6(4) . . . . ? O4 C18 O5 C19 11.4(4) . . . . ? C22 C21 O6 C1 -73.2(3) . . . . ? C8 C1 O6 C21 156.5(2) . . . . ? C2 C1 O6 C21 -82.3(2) . . . . ? O8 B O7 C30 11.5(4) . . . . ? C29 B O7 C30 -176.4(3) . . . . ? C31 C30 O7 B -24.4(5) . . . . ? C32 C30 O7 B -146.3(4) . . . . ? C33 C30 O7 B 94.0(5) . . . . ? O7 B O8 C31 7.1(4) . . . . ? C29 B O8 C31 -165.1(3) . . . . ? C30 C31 O8 B -21.4(4) . . . . ? C34 C31 O8 B -145.1(3) . . . . ? C35 C31 O8 B 96.2(3) . . . . ? C2 C28 Sn1A C38A -74.6(8) . . . . ? Sn1C C28 Sn1A C38A 54.8(19) . . . . ? Sn1B C28 Sn1A C38A 47.1(7) . . . . ? C2 C28 Sn1A C36 160.4(3) . . . . ? Sn1C C28 Sn1A C36 -70.1(18) . . . . ? Sn1B C28 Sn1A C36 -77.8(5) . . . . ? C2 C28 Sn1A C37A 47.3(6) . . . . ? Sn1C C28 Sn1A C37A 177(2) . . . . ? Sn1B C28 Sn1A C37A 169.0(8) . . . . ? Sn1C C36 Sn1A C28 96(2) . . . . ? Sn1B C36 Sn1A C28 82.7(5) . . . . ? Sn1C C36 Sn1A C38A -36.6(19) . . . . ? Sn1B C36 Sn1A C38A -49.9(8) . . . . ? Sn1C C36 Sn1A C37A -145(2) . . . . ? Sn1B C36 Sn1A C37A -158.5(7) . . . . ? Sn1C C36 Sn1B C37B 51.6(7) . . . . ? Sn1A C36 Sn1B C37B 58.9(6) . . . . ? Sn1C C36 Sn1B C38B 161.6(6) . . . . ? Sn1A C36 Sn1B C38B 169.0(6) . . . . ? Sn1C C36 Sn1B C28 -72.9(5) . . . . ? Sn1A C36 Sn1B C28 -65.5(5) . . . . ? C2 C28 Sn1B C37B 23.1(6) . . . . ? Sn1A C28 Sn1B C37B -51.0(6) . . . . ? Sn1C C28 Sn1B C37B -55.3(6) . . . . ? C2 C28 Sn1B C38B -103.4(4) . . . . ? Sn1A C28 Sn1B C38B -177.5(6) . . . . ? Sn1C C28 Sn1B C38B 178.2(6) . . . . ? C2 C28 Sn1B C36 144.6(3) . . . . ? Sn1A C28 Sn1B C36 70.5(5) . . . . ? Sn1C C28 Sn1B C36 66.2(5) . . . . ? Sn1A C36 Sn1C C37C 54.0(19) . . . . ? Sn1B C36 Sn1C C37C -146.2(7) . . . . ? Sn1A C36 Sn1C C38C 163(2) . . . . ? Sn1B C36 Sn1C C38C -37.0(5) . . . . ? Sn1A C36 Sn1C C28 -72.5(19) . . . . ? Sn1B C36 Sn1C C28 87.3(6) . . . . ? C2 C28 Sn1C C36 153.4(3) . . . . ? Sn1A C28 Sn1C C36 98(2) . . . . ? Sn1B C28 Sn1C C36 -93.4(6) . . . . ? C2 C28 Sn1C C37C 26.9(5) . . . . ? Sn1A C28 Sn1C C37C -28.1(18) . . . . ? Sn1B C28 Sn1C C37C 140.1(7) . . . . ? C2 C28 Sn1C C38C -92.5(5) . . . . ? Sn1A C28 Sn1C C38C -147(2) . . . . ? Sn1B C28 Sn1C C38C 20.7(5) . . . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 206 28 ' ' _platon_squeeze_details ; ; # END of CIF # Attachment '- 49 archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-08-27 at 16:59:18 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : shelxl dreduc import struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_RajanBabu1782 _database_code_depnum_ccdc_archive 'CCDC 854087' #TrackingRef '- 49 archive.cif' _audit_creation_date 2010-08-27T16:59:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'RajanBabu 1782' _chemical_formula_moiety 'C35 H39 B1 O8' _chemical_formula_sum 'C35 H39 B O8' _chemical_formula_weight 598.47 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2127(1) _cell_length_b 10.9420(1) _cell_length_c 28.6657(3) _cell_angle_alpha 90 _cell_angle_beta 98.3920(10) _cell_angle_gamma 90 _cell_volume 3169.02(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7183 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.27 _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_special_details ;All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space with a redundancy factor of 3.7, which means that 90% of these reflections were measured at least 3.7 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.9532E-2 _diffrn_orient_matrix_ub_12 -0.746169E-1 _diffrn_orient_matrix_ub_13 0.643265E-1 _diffrn_orient_matrix_ub_21 0.191496E-1 _diffrn_orient_matrix_ub_22 -0.597397E-1 _diffrn_orient_matrix_ub_23 -0.664588E-1 _diffrn_orient_matrix_ub_31 0.33449E-1 _diffrn_orient_matrix_ub_32 -0.15721E-2 _diffrn_orient_matrix_ub_33 0.110513E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 60440 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.3 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _reflns_number_total 7037 _reflns_number_gt 4141 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The five-membered ring containing the boron atom is disordered with respect to rotation about the B-C29 bond. This disorder is interpreted in terms of two orientations for this ring, which are labeled as A and B, with one methyl carbon atom, C32A, common to both orientations. The sum of the site occupancy factors was constrained to be equal to one: the occupancy factor for the A orientation refined to a final value of 0.516(5) with the occupancy factor for the B orientation as 0.484(5). Similarity restraints were used in the refinement with the distance between the following pairs of atoms within various sets restrained to be equal within a standard uncertainty of 0.01Ang.: B and O7A, B and O7B, B and O8A, B and O8B comprise one set, C30A and C31A, and C30B and C31B comprise a second set, O7A and C30A, O7B and C30B, O8A and C31A, and O8B and C31B are in the third set (SADI restraints). Two types of restraints were also applied to the displacement parameters. The components of the anisotropic displacement parameters along a bond between two atoms were restrained to be equal within a standard uncertainty of 0.01 Ang.**2 (DELU restraint) for the following atoms: B, O7A, O7B, C30A, C30B, C31A, C31B, C34A, C34B, C35A and C35B. Similarity restraints for the following bonded atoms were applied so that they would have the same Uij components within a standard uncertainty of 0.04 Ang.**2: B-O7A, C31A-C34A, C31B-C34B (SIMU restraint). For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded carbon atom). The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+0.0357P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7037 _refine_ls_number_parameters 461 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.271 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.038 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.99710(14) 0.28278(13) 0.09521(5) 0.0284(4) Uani 1 1 d . . . H1 H 1.0806 0.2842 0.1183 0.034 Uiso 1 1 calc R . . C2 C 1.01624(14) 0.20143(14) 0.05333(5) 0.0302(4) Uani 1 1 d . . . C3 C 1.09490(15) 0.08758(14) 0.06336(5) 0.0307(4) Uani 1 1 d . . . C4 C 1.05259(15) 0.00143(14) 0.09992(5) 0.0328(4) Uani 1 1 d . . . H4A H 1.0813 -0.0824 0.0932 0.039 Uiso 1 1 calc R . . H4B H 0.9547 0.0012 0.0966 0.039 Uiso 1 1 calc R . . C5 C 1.10761(14) 0.03347(14) 0.15066(5) 0.0293(4) Uani 1 1 d . . . C6 C 1.03935(14) 0.11071(13) 0.17760(5) 0.0284(4) Uani 1 1 d . . . C7 C 0.90584(14) 0.15996(14) 0.15908(5) 0.0290(4) Uani 1 1 d . . . C8 C 0.88438(14) 0.23652(13) 0.11953(5) 0.0277(3) Uani 1 1 d . . . C9 C 1.22747(15) -0.01956(14) 0.17038(5) 0.0331(4) Uani 1 1 d . . . H9 H 1.2734 -0.071 0.1515 0.04 Uiso 1 1 calc R . . C10 C 1.28045(15) 0.00184(15) 0.21712(5) 0.0337(4) Uani 1 1 d . . . C11 C 1.21290(15) 0.07844(15) 0.24447(5) 0.0329(4) Uani 1 1 d . . . C12 C 1.09472(15) 0.13242(14) 0.22473(5) 0.0304(4) Uani 1 1 d . . . C13 C 1.46853(17) -0.12759(16) 0.21463(6) 0.0498(5) Uani 1 1 d . . . H13A H 1.5467 -0.1571 0.2355 0.075 Uiso 1 1 calc R . . H13B H 1.4966 -0.0825 0.1882 0.075 Uiso 1 1 calc R . . H13C H 1.4136 -0.1973 0.2025 0.075 Uiso 1 1 calc R . . C14 C 1.22955(18) -0.00097(16) 0.32026(6) 0.0479(5) Uani 1 1 d . . . H14A H 1.2653 0.0156 0.3533 0.072 Uiso 1 1 calc R . . H14B H 1.2676 -0.0771 0.3102 0.072 Uiso 1 1 calc R . . H14C H 1.1331 -0.009 0.3171 0.072 Uiso 1 1 calc R . . C15 C 1.07657(19) 0.32348(17) 0.26099(7) 0.0584(5) Uani 1 1 d . . . H15A H 1.0228 0.3677 0.2811 0.088 Uiso 1 1 calc R . . H15B H 1.0731 0.3662 0.2308 0.088 Uiso 1 1 calc R . . H15C H 1.1684 0.3196 0.2766 0.088 Uiso 1 1 calc R . . C16 C 0.79745(15) 0.12198(14) 0.18100(5) 0.0327(4) Uani 1 1 d . . . H16 H 0.8102 0.0706 0.208 0.039 Uiso 1 1 calc R . . C17 C 0.67424(15) 0.16098(15) 0.16236(5) 0.0330(4) Uani 1 1 d . . . C18 C 0.45676(17) 0.18982(18) 0.14330(7) 0.0518(5) Uani 1 1 d . . . H18A H 0.4063 0.1232 0.1255 0.062 Uiso 1 1 calc R . . H18B H 0.3941 0.2405 0.1582 0.062 Uiso 1 1 calc R . . C19 C 0.65374(14) 0.23379(14) 0.12294(5) 0.0320(4) Uani 1 1 d . . . C20 C 0.75522(14) 0.27326(14) 0.10063(5) 0.0306(4) Uani 1 1 d . . . H20 H 0.7394 0.3236 0.0734 0.037 Uiso 1 1 calc R . . C21 C 1.07113(15) 0.47421(15) 0.06750(6) 0.0384(4) Uani 1 1 d . . . H21A H 1.0365 0.5488 0.0504 0.046 Uiso 1 1 calc R . . H21B H 1.1173 0.425 0.0459 0.046 Uiso 1 1 calc R . . C22 C 1.16863(15) 0.51050(14) 0.10982(5) 0.0338(4) Uani 1 1 d . . . C23 C 1.12741(17) 0.57991(16) 0.14573(6) 0.0436(4) Uani 1 1 d . . . H23 H 1.0383 0.6073 0.1426 0.052 Uiso 1 1 calc R . . C24 C 1.21384(19) 0.60961(17) 0.18587(6) 0.0497(5) Uani 1 1 d . . . H24 H 1.1842 0.6576 0.2099 0.06 Uiso 1 1 calc R . . C25 C 1.3425(2) 0.56965(17) 0.19092(7) 0.0552(5) Uani 1 1 d . . . H25 H 1.4017 0.588 0.2188 0.066 Uiso 1 1 calc R . . C26 C 1.38486(18) 0.50344(19) 0.15570(8) 0.0644(6) Uani 1 1 d . . . H26 H 1.4744 0.4772 0.159 0.077 Uiso 1 1 calc R . . C27 C 1.29884(17) 0.47365(17) 0.11498(7) 0.0508(5) Uani 1 1 d . . . H27 H 1.3301 0.4278 0.0907 0.061 Uiso 1 1 calc R . . C28 C 0.95807(15) 0.22779(16) 0.00996(5) 0.0381(4) Uani 1 1 d . . . H28A H 0.9663 0.1735 -0.0153 0.046 Uiso 1 1 calc R . . H28B H 0.9082 0.3009 0.0042 0.046 Uiso 1 1 calc R . . C29 C 1.19542(15) 0.05862(15) 0.04024(5) 0.0376(4) Uani 1 1 d . A . H29 H 1.2328 -0.0199 0.0472 0.045 Uiso 1 1 calc R . . C30A C 1.3152(4) 0.2739(5) -0.04826(17) 0.0442(13) Uani 0.516(5) 1 d PDU A 1 C31A C 1.4255(4) 0.1748(3) -0.04042(13) 0.0399(11) Uani 0.516(5) 1 d PDU A 1 C32A C 1.3525(2) 0.40950(19) -0.04445(7) 0.0637(6) Uani 1 1 d . . . H32A H 1.4182 0.4226 -0.0164 0.096 Uiso 0.516(5) 1 calc PR A 1 H32B H 1.2734 0.4583 -0.042 0.096 Uiso 0.516(5) 1 calc PR A 1 H32C H 1.3899 0.4344 -0.0726 0.096 Uiso 0.516(5) 1 calc PR A 1 H32D H 1.3762 0.4646 -0.0176 0.096 Uiso 0.484(5) 1 calc PR A 2 H32E H 1.2602 0.4237 -0.0583 0.096 Uiso 0.484(5) 1 calc PR A 2 H32F H 1.4104 0.4252 -0.0682 0.096 Uiso 0.484(5) 1 calc PR A 2 C33A C 1.2158(12) 0.2499(13) -0.0915(4) 0.076(3) Uani 0.516(5) 1 d P A 1 H33A H 1.1485 0.3144 -0.0949 0.114 Uiso 0.516(5) 1 calc PR A 1 H33B H 1.1733 0.1706 -0.0884 0.114 Uiso 0.516(5) 1 calc PR A 1 H33C H 1.2608 0.2491 -0.1194 0.114 Uiso 0.516(5) 1 calc PR A 1 C34A C 1.4607(11) 0.1231(11) -0.0837(4) 0.110(4) Uani 0.516(5) 1 d PU A 1 H34A H 1.3804 0.0955 -0.1039 0.166 Uiso 0.516(5) 1 calc PR A 1 H34B H 1.5204 0.0535 -0.076 0.166 Uiso 0.516(5) 1 calc PR A 1 H34C H 1.5051 0.1854 -0.1003 0.166 Uiso 0.516(5) 1 calc PR A 1 C35A C 1.5514(5) 0.2136(6) -0.0100(2) 0.0624(15) Uani 0.516(5) 1 d PU A 1 H35A H 1.531 0.243 0.0204 0.094 Uiso 0.516(5) 1 calc PR A 1 H35B H 1.5933 0.2793 -0.0258 0.094 Uiso 0.516(5) 1 calc PR A 1 H35C H 1.6118 0.1438 -0.0049 0.094 Uiso 0.516(5) 1 calc PR A 1 C30B C 1.3682(5) 0.2848(4) -0.02872(15) 0.0379(13) Uani 0.484(5) 1 d PDU A 2 C31B C 1.3359(4) 0.1824(4) -0.06573(13) 0.0429(13) Uani 0.484(5) 1 d PDU A 2 C33B C 1.5120(5) 0.2767(6) -0.00331(19) 0.0576(15) Uani 0.484(5) 1 d P A 2 H33D H 1.5298 0.1935 0.0086 0.086 Uiso 0.484(5) 1 calc PR A 2 H33E H 1.5243 0.3345 0.0231 0.086 Uiso 0.484(5) 1 calc PR A 2 H33F H 1.5732 0.2969 -0.0255 0.086 Uiso 0.484(5) 1 calc PR A 2 C34B C 1.4491(11) 0.1302(8) -0.0893(3) 0.064(3) Uani 0.484(5) 1 d PU A 2 H34D H 1.5211 0.1039 -0.0649 0.097 Uiso 0.484(5) 1 calc PR A 2 H34E H 1.4817 0.1933 -0.1089 0.097 Uiso 0.484(5) 1 calc PR A 2 H34F H 1.4168 0.0601 -0.1089 0.097 Uiso 0.484(5) 1 calc PR A 2 C35B C 1.2253(16) 0.2211(16) -0.1049(5) 0.096(4) Uani 0.484(5) 1 d PU A 2 H35D H 1.1515 0.2554 -0.0908 0.144 Uiso 0.484(5) 1 calc PR A 2 H35E H 1.1946 0.1498 -0.1241 0.144 Uiso 0.484(5) 1 calc PR A 2 H35F H 1.2591 0.2829 -0.1248 0.144 Uiso 0.484(5) 1 calc PR A 2 B B 1.26006(19) 0.13396(18) 0.00379(7) 0.0381(5) Uani 1 1 d DU . . O1 O 1.39399(10) -0.04889(11) 0.24030(4) 0.0441(3) Uani 1 1 d . . . O2 O 1.26269(11) 0.09817(10) 0.29119(4) 0.0407(3) Uani 1 1 d . . . O3 O 1.02611(10) 0.20276(10) 0.25289(4) 0.0383(3) Uani 1 1 d . . . O4 O 0.55539(10) 0.13963(11) 0.17863(4) 0.0469(3) Uani 1 1 d . . . O5 O 0.52093(10) 0.26260(11) 0.11224(4) 0.0429(3) Uani 1 1 d . . . O6 O 0.96253(10) 0.40490(9) 0.08021(3) 0.0338(3) Uani 1 1 d . . . O7A O 1.2549(9) 0.2533(5) -0.0049(3) 0.088(3) Uani 0.516(5) 1 d PDU A 1 O8A O 1.3627(4) 0.0808(2) -0.01585(14) 0.0526(10) Uani 0.516(5) 1 d PD A 1 O7B O 1.2748(9) 0.2541(4) 0.0041(2) 0.056(2) Uani 0.484(5) 1 d PDU A 2 O8B O 1.2856(4) 0.0855(2) -0.03806(11) 0.0436(9) Uani 0.484(5) 1 d PD A 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 C1 0.0294(8) 0.0270(9) 0.0277(8) 0.0043(7) 0.0003(6) -0.0028(7) C2 0.0293(8) 0.0349(10) 0.0265(8) 0.0007(7) 0.0050(7) -0.0089(7) C3 0.0352(9) 0.0321(9) 0.0237(8) -0.0036(7) 0.0009(7) -0.0086(7) C4 0.0382(9) 0.0294(9) 0.0308(9) 0.0003(7) 0.0049(7) -0.0045(7) C5 0.0334(9) 0.0272(9) 0.0273(8) 0.0035(7) 0.0047(7) -0.0060(7) C6 0.0323(8) 0.0254(8) 0.0270(8) 0.0058(7) 0.0025(7) -0.0062(7) C7 0.0329(8) 0.0277(9) 0.0259(8) -0.0007(7) 0.0024(7) -0.0040(7) C8 0.0314(8) 0.0267(8) 0.0245(8) -0.0034(7) 0.0021(6) -0.0029(7) C9 0.0357(9) 0.0327(9) 0.0321(9) 0.0030(7) 0.0094(7) -0.0029(7) C10 0.0306(9) 0.0350(10) 0.0346(9) 0.0072(7) 0.0018(7) -0.0022(7) C11 0.0369(9) 0.0350(10) 0.0251(8) 0.0042(7) -0.0015(7) -0.0054(8) C12 0.0348(9) 0.0280(9) 0.0289(8) 0.0003(7) 0.0068(7) -0.0046(7) C13 0.0461(11) 0.0418(11) 0.0600(12) 0.0007(9) 0.0021(9) 0.0090(9) C14 0.0642(12) 0.0481(12) 0.0307(9) 0.0074(8) 0.0049(8) 0.0049(10) C15 0.0645(13) 0.0370(12) 0.0729(14) -0.0113(10) 0.0073(11) 0.0000(10) C16 0.0392(10) 0.0301(9) 0.0288(8) 0.0028(7) 0.0054(7) -0.0047(7) C17 0.0315(9) 0.0321(9) 0.0367(9) -0.0007(7) 0.0096(7) -0.0058(7) C18 0.0361(10) 0.0553(13) 0.0658(13) 0.0165(10) 0.0132(9) -0.0026(9) C19 0.0267(9) 0.0334(9) 0.0350(9) -0.0019(7) 0.0017(7) 0.0001(7) C20 0.0329(9) 0.0311(9) 0.0272(8) -0.0003(7) 0.0025(7) -0.0021(7) C21 0.0406(10) 0.0346(10) 0.0398(9) 0.0084(8) 0.0057(8) -0.0094(8) C22 0.0343(9) 0.0281(9) 0.0392(9) 0.0058(7) 0.0056(7) -0.0064(7) C23 0.0355(10) 0.0511(12) 0.0441(10) 0.0022(9) 0.0048(8) -0.0003(9) C24 0.0564(12) 0.0470(12) 0.0443(11) -0.0031(9) 0.0031(9) -0.0045(9) C25 0.0552(13) 0.0386(11) 0.0640(13) -0.0041(10) -0.0172(10) -0.0012(10) C26 0.0338(10) 0.0568(14) 0.0960(17) -0.0131(13) -0.0130(11) 0.0041(10) C27 0.0406(11) 0.0448(11) 0.0662(13) -0.0100(10) 0.0053(9) 0.0032(9) C28 0.0388(9) 0.0444(11) 0.0310(9) 0.0013(8) 0.0046(7) -0.0059(8) C29 0.0428(10) 0.0352(10) 0.0350(9) -0.0004(8) 0.0060(8) -0.0015(8) C30A 0.036(3) 0.062(3) 0.035(3) 0.013(3) 0.008(2) -0.009(2) C31A 0.040(2) 0.048(2) 0.032(2) -0.0024(17) 0.0078(18) -0.0023(18) C32A 0.0782(15) 0.0564(14) 0.0574(13) -0.0001(10) 0.0132(11) -0.0135(11) C33A 0.056(4) 0.112(7) 0.056(7) 0.048(6) -0.005(4) -0.027(4) C34A 0.059(5) 0.171(10) 0.099(6) -0.076(6) 0.004(4) 0.010(5) C35A 0.043(3) 0.082(4) 0.061(3) -0.012(3) 0.005(2) 0.003(2) C30B 0.045(3) 0.042(3) 0.027(2) 0.005(2) 0.007(2) -0.006(2) C31B 0.058(3) 0.039(3) 0.036(2) -0.0007(19) 0.018(2) -0.009(2) C33B 0.036(3) 0.081(5) 0.054(3) 0.009(3) 0.000(2) -0.014(3) C34B 0.108(7) 0.047(4) 0.053(4) 0.000(3) 0.062(4) -0.021(4) C35B 0.104(7) 0.135(8) 0.037(5) 0.015(4) -0.030(5) -0.027(5) B 0.0414(12) 0.0393(12) 0.0342(11) -0.0026(9) 0.0075(9) 0.0001(10) O1 0.0363(6) 0.0549(8) 0.0392(7) 0.0052(6) -0.0001(5) 0.0088(6) O2 0.0480(7) 0.0441(7) 0.0271(6) 0.0018(5) -0.0051(5) -0.0037(6) O3 0.0442(7) 0.0385(7) 0.0321(6) -0.0060(5) 0.0055(5) -0.0010(5) O4 0.0331(7) 0.0588(9) 0.0510(8) 0.0111(6) 0.0135(6) -0.0037(6) O5 0.0288(6) 0.0530(8) 0.0476(7) 0.0076(6) 0.0076(5) 0.0010(5) O6 0.0332(6) 0.0299(6) 0.0373(6) 0.0075(5) 0.0015(5) -0.0045(5) O7A 0.092(4) 0.069(4) 0.123(5) 0.050(3) 0.081(4) 0.039(3) O8A 0.052(2) 0.0482(17) 0.063(2) 0.0114(15) 0.0271(18) 0.0079(15) O7B 0.092(4) 0.033(3) 0.055(2) -0.019(2) 0.047(2) -0.025(3) O8B 0.061(2) 0.0361(15) 0.0367(17) 0.0022(13) 0.0172(16) -0.0017(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 1.4320(17) . ? C1 C8 1.517(2) . ? C1 C2 1.530(2) . ? C1 H1 1 . ? C2 C28 1.329(2) . ? C2 C3 1.487(2) . ? C3 C29 1.339(2) . ? C3 C4 1.518(2) . ? C4 C5 1.5217(19) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C9 1.397(2) . ? C5 C6 1.398(2) . ? C6 C12 1.407(2) . ? C6 C7 1.490(2) . ? C7 C8 1.401(2) . ? C7 C16 1.413(2) . ? C8 C20 1.409(2) . ? C9 C10 1.390(2) . ? C9 H9 0.95 . ? C10 O1 1.3672(18) . ? C10 C11 1.397(2) . ? C11 O2 1.3783(17) . ? C11 C12 1.388(2) . ? C12 O3 1.3785(18) . ? C13 O1 1.424(2) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 O2 1.4382(19) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 O3 1.425(2) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C17 1.362(2) . ? C16 H16 0.95 . ? C17 C19 1.373(2) . ? C17 O4 1.3822(17) . ? C18 O5 1.424(2) . ? C18 O4 1.430(2) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.365(2) . ? C19 O5 1.3826(18) . ? C20 H20 0.95 . ? C21 O6 1.4339(17) . ? C21 C22 1.506(2) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 C27 1.377(2) . ? C22 C23 1.393(2) . ? C23 C24 1.383(2) . ? C23 H23 0.95 . ? C24 C25 1.373(3) . ? C24 H24 0.95 . ? C25 C26 1.363(3) . ? C25 H25 0.95 . ? C26 C27 1.393(3) . ? C26 H26 0.95 . ? C27 H27 0.95 . ? C28 H28A 0.95 . ? C28 H28B 0.95 . ? C29 B 1.552(2) . ? C29 H29 0.95 . ? C30A O7A 1.482(5) . ? C30A C33A 1.507(12) . ? C30A C32A 1.531(6) . ? C30A C31A 1.556(5) . ? C31A O8A 1.449(4) . ? C31A C34A 1.455(11) . ? C31A C35A 1.505(7) . ? C32A C30B 1.439(5) . ? C32A H32A 0.98 . ? C32A H32B 0.98 . ? C32A H32C 0.98 . ? C32A H32D 0.98 . ? C32A H32E 0.98 . ? C32A H32F 0.98 . ? C33A H33A 0.98 . ? C33A H33B 0.98 . ? C33A H33C 0.98 . ? C34A H34A 0.98 . ? C34A H34B 0.98 . ? C34A H34C 0.98 . ? C35A H35A 0.98 . ? C35A H35B 0.98 . ? C35A H35C 0.98 . ? C30B O7B 1.473(5) . ? C30B C33B 1.544(8) . ? C30B C31B 1.545(5) . ? C31B O8B 1.462(4) . ? C31B C34B 1.531(10) . ? C31B C35B 1.531(17) . ? C33B H33D 0.98 . ? C33B H33E 0.98 . ? C33B H33F 0.98 . ? C34B H34D 0.98 . ? C34B H34E 0.98 . ? C34B H34F 0.98 . ? C35B H35D 0.98 . ? C35B H35E 0.98 . ? C35B H35F 0.98 . ? B O7B 1.323(5) . ? B O7A 1.330(5) . ? B O8B 1.371(3) . ? B O8A 1.388(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 O6 C1 C8 106.20(11) . . ? O6 C1 C2 111.18(12) . . ? C8 C1 C2 111.03(12) . . ? O6 C1 H1 109.5 . . ? C8 C1 H1 109.5 . . ? C2 C1 H1 109.5 . . ? C28 C2 C3 121.17(14) . . ? C28 C2 C1 121.13(14) . . ? C3 C2 C1 117.57(12) . . ? C29 C3 C2 122.29(14) . . ? C29 C3 C4 120.71(14) . . ? C2 C3 C4 116.95(13) . . ? C3 C4 C5 114.46(12) . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? C9 C5 C6 120.37(13) . . ? C9 C5 C4 118.06(14) . . ? C6 C5 C4 121.54(13) . . ? C5 C6 C12 118.03(13) . . ? C5 C6 C7 121.73(13) . . ? C12 C6 C7 119.99(13) . . ? C8 C7 C16 119.72(14) . . ? C8 C7 C6 122.11(13) . . ? C16 C7 C6 118.08(13) . . ? C7 C8 C20 120.57(14) . . ? C7 C8 C1 122.13(13) . . ? C20 C8 C1 117.31(13) . . ? C10 C9 C5 120.99(15) . . ? C10 C9 H9 119.5 . . ? C5 C9 H9 119.5 . . ? O1 C10 C9 125.70(15) . . ? O1 C10 C11 115.09(13) . . ? C9 C10 C11 119.18(14) . . ? O2 C11 C12 120.33(14) . . ? O2 C11 C10 119.80(13) . . ? C12 C11 C10 119.86(14) . . ? O3 C12 C11 119.01(13) . . ? O3 C12 C6 119.30(13) . . ? C11 C12 C6 121.57(14) . . ? O1 C13 H13A 109.5 . . ? O1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C7 118.18(14) . . ? C17 C16 H16 120.9 . . ? C7 C16 H16 120.9 . . ? C16 C17 C19 121.73(14) . . ? C16 C17 O4 128.40(14) . . ? C19 C17 O4 109.86(13) . . ? O5 C18 O4 108.47(12) . . ? O5 C18 H18A 110 . . ? O4 C18 H18A 110 . . ? O5 C18 H18B 110 . . ? O4 C18 H18B 110 . . ? H18A C18 H18B 108.4 . . ? C20 C19 C17 122.27(14) . . ? C20 C19 O5 127.68(14) . . ? C17 C19 O5 109.98(13) . . ? C19 C20 C8 117.51(14) . . ? C19 C20 H20 121.2 . . ? C8 C20 H20 121.2 . . ? O6 C21 C22 112.31(12) . . ? O6 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? O6 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? C27 C22 C23 118.15(15) . . ? C27 C22 C21 121.60(15) . . ? C23 C22 C21 120.23(14) . . ? C24 C23 C22 121.20(16) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 119.86(18) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 119.56(18) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 121.03(17) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C22 C27 C26 120.17(18) . . ? C22 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C2 C28 H28A 120 . . ? C2 C28 H28B 120 . . ? H28A C28 H28B 120 . . ? C3 C29 B 129.78(16) . . ? C3 C29 H29 115.1 . . ? B C29 H29 115.1 . . ? O7A C30A C33A 110.5(6) . . ? O7A C30A C32A 102.5(4) . . ? C33A C30A C32A 111.0(6) . . ? O7A C30A C31A 98.8(4) . . ? C33A C30A C31A 112.6(7) . . ? C32A C30A C31A 119.8(4) . . ? O8A C31A C34A 108.7(5) . . ? O8A C31A C35A 108.7(4) . . ? C34A C31A C35A 107.9(5) . . ? O8A C31A C30A 101.7(3) . . ? C34A C31A C30A 114.3(6) . . ? C35A C31A C30A 115.2(4) . . ? C30A C32A H32A 109.5 . . ? C30A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C30A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C30B C32A H32D 109.5 . . ? C30B C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C30B C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C30A C33A H33A 109.5 . . ? C30A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C30A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? C31A C34A H34A 109.5 . . ? C31A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C31A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C31A C35A H35A 109.5 . . ? C31A C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? C31A C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? C32A C30B O7B 111.3(4) . . ? C32A C30B C33B 104.9(4) . . ? O7B C30B C33B 110.2(5) . . ? C32A C30B C31B 118.0(4) . . ? O7B C30B C31B 100.4(4) . . ? C33B C30B C31B 112.1(5) . . ? O8B C31B C34B 108.4(4) . . ? O8B C31B C35B 108.6(6) . . ? C34B C31B C35B 107.7(7) . . ? O8B C31B C30B 102.1(3) . . ? C34B C31B C30B 118.2(5) . . ? C35B C31B C30B 111.3(7) . . ? C30B C33B H33D 109.5 . . ? C30B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C30B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C31B C34B H34D 109.5 . . ? C31B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C31B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C31B C35B H35D 109.5 . . ? C31B C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C31B C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? O7B B O8B 110.8(3) . . ? O7A B O8B 102.9(3) . . ? O7B B O8A 109.1(4) . . ? O7A B O8A 110.3(3) . . ? O7B B C29 125.6(3) . . ? O7A B C29 129.8(3) . . ? O8B B C29 122.51(18) . . ? O8A B C29 118.12(19) . . ? C10 O1 C13 118.29(12) . . ? C11 O2 C14 111.11(12) . . ? C12 O3 C15 114.23(13) . . ? C17 O4 C18 104.99(11) . . ? C19 O5 C18 105.06(12) . . ? C1 O6 C21 113.82(11) . . ? B O7A C30A 107.3(4) . . ? B O8A C31A 108.3(2) . . ? B O7B C30B 107.8(4) . . ? B O8B C31B 108.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 C1 C2 C28 -24.34(19) . . . . ? C8 C1 C2 C28 93.67(16) . . . . ? O6 C1 C2 C3 159.62(12) . . . . ? C8 C1 C2 C3 -82.38(16) . . . . ? C28 C2 C3 C29 54.7(2) . . . . ? C1 C2 C3 C29 -129.24(15) . . . . ? C28 C2 C3 C4 -122.73(15) . . . . ? C1 C2 C3 C4 53.32(17) . . . . ? C29 C3 C4 C5 98.33(17) . . . . ? C2 C3 C4 C5 -84.19(16) . . . . ? C3 C4 C5 C9 -91.53(17) . . . . ? C3 C4 C5 C6 90.33(17) . . . . ? C9 C5 C6 C12 -0.2(2) . . . . ? C4 C5 C6 C12 177.84(13) . . . . ? C9 C5 C6 C7 -174.52(14) . . . . ? C4 C5 C6 C7 3.6(2) . . . . ? C5 C6 C7 C8 -62.4(2) . . . . ? C12 C6 C7 C8 123.42(16) . . . . ? C5 C6 C7 C16 114.12(16) . . . . ? C12 C6 C7 C16 -60.04(19) . . . . ? C16 C7 C8 C20 -1.8(2) . . . . ? C6 C7 C8 C20 174.73(14) . . . . ? C16 C7 C8 C1 178.49(13) . . . . ? C6 C7 C8 C1 -5.0(2) . . . . ? O6 C1 C8 C7 -143.67(14) . . . . ? C2 C1 C8 C7 95.34(16) . . . . ? O6 C1 C8 C20 36.56(17) . . . . ? C2 C1 C8 C20 -84.43(16) . . . . ? C6 C5 C9 C10 0.8(2) . . . . ? C4 C5 C9 C10 -177.33(13) . . . . ? C5 C9 C10 O1 177.40(14) . . . . ? C5 C9 C10 C11 -0.5(2) . . . . ? O1 C10 C11 O2 0.3(2) . . . . ? C9 C10 C11 O2 178.47(13) . . . . ? O1 C10 C11 C12 -178.46(13) . . . . ? C9 C10 C11 C12 -0.3(2) . . . . ? O2 C11 C12 O3 -2.0(2) . . . . ? C10 C11 C12 O3 176.76(13) . . . . ? O2 C11 C12 C6 -177.88(13) . . . . ? C10 C11 C12 C6 0.9(2) . . . . ? C5 C6 C12 O3 -176.47(13) . . . . ? C7 C6 C12 O3 -2.1(2) . . . . ? C5 C6 C12 C11 -0.6(2) . . . . ? C7 C6 C12 C11 173.77(14) . . . . ? C8 C7 C16 C17 0.5(2) . . . . ? C6 C7 C16 C17 -176.09(14) . . . . ? C7 C16 C17 C19 0.9(2) . . . . ? C7 C16 C17 O4 -177.37(15) . . . . ? C16 C17 C19 C20 -1.2(3) . . . . ? O4 C17 C19 C20 177.35(14) . . . . ? C16 C17 C19 O5 -178.46(14) . . . . ? O4 C17 C19 O5 0.13(18) . . . . ? C17 C19 C20 C8 0.0(2) . . . . ? O5 C19 C20 C8 176.70(14) . . . . ? C7 C8 C20 C19 1.5(2) . . . . ? C1 C8 C20 C19 -178.76(13) . . . . ? O6 C21 C22 C27 119.64(17) . . . . ? O6 C21 C22 C23 -58.4(2) . . . . ? C27 C22 C23 C24 -1.0(3) . . . . ? C21 C22 C23 C24 177.07(15) . . . . ? C22 C23 C24 C25 -0.5(3) . . . . ? C23 C24 C25 C26 1.6(3) . . . . ? C24 C25 C26 C27 -1.2(3) . . . . ? C23 C22 C27 C26 1.4(3) . . . . ? C21 C22 C27 C26 -176.65(16) . . . . ? C25 C26 C27 C22 -0.3(3) . . . . ? C2 C3 C29 B 6.1(3) . . . . ? C4 C3 C29 B -176.51(14) . . . . ? O7A C30A C31A O8A 32.7(5) . . . . ? C33A C30A C31A O8A -84.0(5) . . . . ? C32A C30A C31A O8A 142.7(4) . . . . ? O7A C30A C31A C34A 149.5(6) . . . . ? C33A C30A C31A C34A 32.9(7) . . . . ? C32A C30A C31A C34A -100.4(6) . . . . ? O7A C30A C31A C35A -84.6(5) . . . . ? C33A C30A C31A C35A 158.7(6) . . . . ? C32A C30A C31A C35A 25.4(5) . . . . ? O7A C30A C32A C30B 67.7(7) . . . . ? C33A C30A C32A C30B -174.2(9) . . . . ? C31A C30A C32A C30B -40.2(5) . . . . ? C30A C32A C30B O7B -85.8(8) . . . . ? C30A C32A C30B C33B 155.0(8) . . . . ? C30A C32A C30B C31B 29.5(4) . . . . ? C32A C30B C31B O8B -147.4(4) . . . . ? O7B C30B C31B O8B -26.4(5) . . . . ? C33B C30B C31B O8B 90.5(4) . . . . ? C32A C30B C31B C34B 93.7(6) . . . . ? O7B C30B C31B C34B -145.3(5) . . . . ? C33B C30B C31B C34B -28.3(6) . . . . ? C32A C30B C31B C35B -31.7(8) . . . . ? O7B C30B C31B C35B 89.3(8) . . . . ? C33B C30B C31B C35B -153.7(7) . . . . ? C3 C29 B O7B 34.3(6) . . . . ? C3 C29 B O7A 18.4(7) . . . . ? C3 C29 B O8B -132.6(3) . . . . ? C3 C29 B O8A -178.7(3) . . . . ? C9 C10 O1 C13 2.3(2) . . . . ? C11 C10 O1 C13 -179.71(14) . . . . ? C12 C11 O2 C14 97.94(17) . . . . ? C10 C11 O2 C14 -80.83(17) . . . . ? C11 C12 O3 C15 79.66(18) . . . . ? C6 C12 O3 C15 -104.38(16) . . . . ? C16 C17 O4 C18 -173.91(17) . . . . ? C19 C17 O4 C18 7.62(18) . . . . ? O5 C18 O4 C17 -12.48(18) . . . . ? C20 C19 O5 C18 175.11(17) . . . . ? C17 C19 O5 C18 -7.86(18) . . . . ? O4 C18 O5 C19 12.55(18) . . . . ? C8 C1 O6 C21 164.75(11) . . . . ? C2 C1 O6 C21 -74.37(15) . . . . ? C22 C21 O6 C1 -72.52(16) . . . . ? O7B B O7A C30A 112(3) . . . . ? O8B B O7A C30A -15.7(7) . . . . ? O8A B O7A C30A 25.2(8) . . . . ? C29 B O7A C30A -170.8(3) . . . . ? C33A C30A O7A B 82.5(9) . . . . ? C32A C30A O7A B -159.2(5) . . . . ? C31A C30A O7A B -35.8(7) . . . . ? O7B B O8A C31A -15.8(5) . . . . ? O7A B O8A C31A -1.8(6) . . . . ? O8B B O8A C31A 84.0(3) . . . . ? C29 B O8A C31A -167.9(2) . . . . ? C34A C31A O8A B -141.4(6) . . . . ? C35A C31A O8A B 101.4(4) . . . . ? C30A C31A O8A B -20.5(4) . . . . ? O7A B O7B C30B -81(2) . . . . ? O8B B O7B C30B -25.6(7) . . . . ? O8A B O7B C30B 16.8(7) . . . . ? C29 B O7B C30B 166.2(3) . . . . ? C32A C30B O7B B 157.9(5) . . . . ? C33B C30B O7B B -86.2(7) . . . . ? C31B C30B O7B B 32.2(7) . . . . ? O7B B O8B C31B 6.7(6) . . . . ? O7A B O8B C31B 17.8(5) . . . . ? O8A B O8B C31B -88.5(4) . . . . ? C29 B O8B C31B 175.3(3) . . . . ? C34B C31B O8B B 139.2(5) . . . . ? C35B C31B O8B B -104.1(7) . . . . ? C30B C31B O8B B 13.6(4) . . . . ? # END of CIF