# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_RajanBabu1916 #TrackingRef '18990_web_deposit_cif_file_0_RajanBabu.T.V_1364518612.archive_7.cif' _audit_creation_date 2012-10-15T11:24:52-00:00 _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 1916' _chemical_formula_moiety 'C27 H32 O11' _chemical_formula_sum 'C27 H32 O11' _chemical_formula_weight 532.53 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration syn #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system triclinic _space_group_name_H-M_alt P1 _space_group_name_Hall P1 _space_group_IT_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.4188(2) _cell_length_b 9.7589(1) _cell_length_c 15.1515(3) _cell_angle_alpha 96.812(1) _cell_angle_beta 97.849(1) _cell_angle_gamma 109.187(1) _cell_volume 1282.95(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5852 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _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 3.6, which means that 90% of these reflections were measured at least 3.6 times. Phi and omega scans with a frame width of 2.0 degrees 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 0.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.896 _exptl_absorpt_correction_T_max 0.984 _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 Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.276711E-1 _diffrn_orient_matrix_ub_12 -0.21329E-1 _diffrn_orient_matrix_ub_13 -0.675595E-1 _diffrn_orient_matrix_ub_21 0.111031 _diffrn_orient_matrix_ub_22 0.35934E-1 _diffrn_orient_matrix_ub_23 -0.37826E-2 _diffrn_orient_matrix_ub_31 0.15599E-2 _diffrn_orient_matrix_ub_32 -0.101962 _diffrn_orient_matrix_ub_33 0.213E-4 _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 41126 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 27.44 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 11557 _reflns_number_gt 10253 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _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 correct enantiomer was chosen based on the known chiral centers in the molecule. There are two molecules in the asymmetric unit and these are labeled as A and B molecules. 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 torsion angle, which defines the orientation of the methyl group about the C-C or C-O bond, was refined. The hydrogen atom bonded to O(6) was refined isotropically in both molecules A and B. 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 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^ > 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^)+(0.0432P)^2^+0.1986P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 11557 _refine_ls_number_parameters 709 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.08 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.003 _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 0.2(4) _refine_diff_density_max 0.308 _refine_diff_density_min -0.347 _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' 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 O1A O 0.79463(13) 0.35610(13) 0.09882(8) 0.0293(3) Uani 1 1 d . . . O2A O 1.08793(14) 0.49727(13) 0.06880(9) 0.0308(3) Uani 1 1 d . . . O3A O 1.31944(13) 0.39620(13) 0.12749(9) 0.0322(3) Uani 1 1 d . . . O4A O 0.84139(13) -0.07628(12) 0.26510(8) 0.0265(2) Uani 1 1 d . . . O5A O 0.88543(16) -0.17296(15) 0.13393(9) 0.0409(3) Uani 1 1 d . . . O6A O 1.15730(16) 0.24156(15) 0.39613(9) 0.0382(3) Uani 1 1 d . . . H06A H 1.134(3) 0.309(3) 0.3709(19) 0.068(8) Uiso 1 1 d . . . O7A O 0.92208(14) 0.36411(13) 0.34756(8) 0.0301(3) Uani 1 1 d . . . O8A O 0.74554(18) 0.47326(17) 0.33161(10) 0.0464(4) Uani 1 1 d . . . O9A O 0.28289(15) -0.09677(17) 0.22708(10) 0.0450(3) Uani 1 1 d . . . O10A O 0.33135(15) -0.12809(17) 0.08224(10) 0.0457(3) Uani 1 1 d . . . O11A O 0.64822(14) 0.02611(16) 0.04017(8) 0.0393(3) Uani 1 1 d . . . C1A C 0.91182(18) 0.30708(18) 0.12592(11) 0.0234(3) Uani 1 1 d . . . C2A C 1.05908(19) 0.37470(17) 0.11028(11) 0.0245(3) Uani 1 1 d . . . C3A C 1.17683(18) 0.32624(17) 0.14491(11) 0.0249(3) Uani 1 1 d . . . C4A C 1.14472(19) 0.21443(17) 0.19528(12) 0.0261(3) Uani 1 1 d . . . H4A H 1.2238 0.1802 0.2177 0.031 Uiso 1 1 calc R . . C5A C 0.99852(18) 0.15075(17) 0.21397(10) 0.0228(3) Uani 1 1 d . . . C6A C 0.98663(19) 0.04293(18) 0.27923(11) 0.0258(3) Uani 1 1 d . . . H6A H 1.065 -0.0034 0.2702 0.031 Uiso 1 1 calc R . . C7A C 1.0227(2) 0.11338(19) 0.38139(12) 0.0310(4) Uani 1 1 d . . . C8A C 0.8900(2) 0.1476(2) 0.41888(12) 0.0337(4) Uani 1 1 d . . . H8A H 0.8105 0.0502 0.4194 0.04 Uiso 1 1 calc R . . C9A C 0.8070(2) 0.2348(2) 0.36630(12) 0.0308(4) Uani 1 1 d . . . H9A H 0.7502 0.272 0.4088 0.037 Uiso 1 1 calc R . . C10A C 0.6891(2) 0.14547(19) 0.28302(11) 0.0270(4) Uani 1 1 d . . . C11A C 0.5422(2) 0.0736(2) 0.29938(12) 0.0324(4) Uani 1 1 d . . . H11A H 0.5192 0.0848 0.3583 0.039 Uiso 1 1 calc R . . C12A C 0.4337(2) -0.0130(2) 0.22744(13) 0.0321(4) Uani 1 1 d . . . C13A C 0.46241(19) -0.03010(19) 0.14033(12) 0.0293(4) Uani 1 1 d . . . C14A C 0.6058(2) 0.04060(19) 0.12227(11) 0.0270(3) Uani 1 1 d . . . C15A C 0.72167(19) 0.12933(18) 0.19618(11) 0.0237(3) Uani 1 1 d . . . C16A C 0.87990(18) 0.19503(18) 0.17846(10) 0.0232(3) Uani 1 1 d . . . C17A C 1.0696(3) 0.0054(2) 0.43369(13) 0.0408(5) Uani 1 1 d . . . H17A H 1.1513 -0.0182 0.409 0.061 Uiso 1 1 calc R . . H17B H 0.981 -0.0851 0.4279 0.061 Uiso 1 1 calc R . . H17C H 1.1063 0.0503 0.4977 0.061 Uiso 1 1 calc R . . C18A C 0.9436(3) 0.2270(3) 0.51807(13) 0.0525(6) Uani 1 1 d . . . H18A H 0.9851 0.1673 0.5543 0.079 Uiso 1 1 calc R . . H18B H 0.8567 0.2412 0.5417 0.079 Uiso 1 1 calc R . . H18C H 1.0232 0.3231 0.5213 0.079 Uiso 1 1 calc R . . C19A C 0.2151(3) -0.1518(3) 0.13312(18) 0.0633(7) Uani 1 1 d . . . H19A H 0.1551 -0.2584 0.1244 0.076 Uiso 1 1 calc R . . H19B H 0.1451 -0.1002 0.113 0.076 Uiso 1 1 calc R . . C20A C 0.5354(3) -0.0276(3) -0.03964(15) 0.0583(6) Uani 1 1 d . . . H20A H 0.4728 -0.1302 -0.0398 0.088 Uiso 1 1 calc R . . H20B H 0.5851 -0.0225 -0.0925 0.088 Uiso 1 1 calc R . . H20C H 0.4701 0.0325 -0.0419 0.088 Uiso 1 1 calc R . . C21A C 0.7622(2) 0.3652(3) 0.00526(14) 0.0443(5) Uani 1 1 d . . . H21A H 0.8086 0.4675 -0.0029 0.066 Uiso 1 1 calc R . . H21B H 0.6511 0.3319 -0.0155 0.066 Uiso 1 1 calc R . . H21C H 0.8045 0.3025 -0.0301 0.066 Uiso 1 1 calc R . . C22A C 1.1526(2) 0.4920(2) -0.01102(14) 0.0376(4) Uani 1 1 d . . . H22A H 1.2391 0.4576 0 0.056 Uiso 1 1 calc R . . H22B H 1.1881 0.5907 -0.0267 0.056 Uiso 1 1 calc R . . H22C H 1.0748 0.424 -0.061 0.056 Uiso 1 1 calc R . . C23A C 1.4320(2) 0.3295(2) 0.14764(15) 0.0364(4) Uani 1 1 d . . . H23A H 1.4578 0.3363 0.2133 0.055 Uiso 1 1 calc R . . H23B H 1.5241 0.381 0.1249 0.055 Uiso 1 1 calc R . . H23C H 1.391 0.2257 0.1185 0.055 Uiso 1 1 calc R . . C24A C 0.8040(2) -0.17729(19) 0.18893(11) 0.0293(4) Uani 1 1 d . . . C25A C 0.6520(2) -0.2933(2) 0.18478(13) 0.0385(4) Uani 1 1 d . . . H25A H 0.6114 -0.3462 0.1225 0.058 Uiso 1 1 calc R . . H25B H 0.5811 -0.2472 0.2047 0.058 Uiso 1 1 calc R . . H25C H 0.6637 -0.3627 0.2245 0.058 Uiso 1 1 calc R . . C26A C 0.8730(2) 0.4748(2) 0.32734(12) 0.0339(4) Uani 1 1 d . . . C27A C 0.9923(2) 0.5928(2) 0.29651(14) 0.0392(4) Uani 1 1 d . . . H27A H 0.9591 0.5935 0.2324 0.059 Uiso 1 1 calc R . . H27B H 1.0887 0.5738 0.3045 0.059 Uiso 1 1 calc R . . H27C H 1.0074 0.6886 0.3323 0.059 Uiso 1 1 calc R . . O1B O 0.88416(13) 0.70414(13) 0.80573(8) 0.0281(3) Uani 1 1 d . . . O2B O 1.03329(13) 1.00777(13) 0.85675(8) 0.0302(3) Uani 1 1 d . . . O3B O 0.89096(13) 1.19453(13) 0.80194(9) 0.0308(3) Uani 1 1 d . . . O4B O 0.33303(12) 0.65283(12) 0.63982(7) 0.0243(2) Uani 1 1 d . . . O5B O 0.31157(15) 0.76965(15) 0.77188(9) 0.0366(3) Uani 1 1 d . . . O6B O 0.58369(15) 0.89329(14) 0.51436(8) 0.0333(3) Uani 1 1 d . . . HO6B H 0.666(3) 0.875(3) 0.5346(17) 0.055(7) Uiso 1 1 d . . . O7B O 0.73579(13) 0.69451(13) 0.55446(8) 0.0276(3) Uani 1 1 d . . . O8B O 0.86754(17) 0.54096(17) 0.56230(11) 0.0549(4) Uani 1 1 d . . . O9B O 0.34979(16) 0.12734(14) 0.66112(10) 0.0406(3) Uani 1 1 d . . . O10B O 0.42373(15) 0.24870(13) 0.80970(9) 0.0371(3) Uani 1 1 d . . . O11B O 0.60592(14) 0.56990(13) 0.86157(8) 0.0330(3) Uani 1 1 d . . . C1B C 0.81251(18) 0.80009(17) 0.78333(10) 0.0232(3) Uani 1 1 d . . . C2B C 0.88504(18) 0.95232(18) 0.80822(11) 0.0236(3) Uani 1 1 d . . . C3B C 0.81252(18) 1.04564(18) 0.77639(11) 0.0244(3) Uani 1 1 d . . . C4B C 0.67025(19) 0.98540(18) 0.72026(11) 0.0250(3) Uani 1 1 d . . . H4B H 0.6204 1.0488 0.6991 0.03 Uiso 1 1 calc R . . C5B C 0.59882(17) 0.83317(17) 0.69417(10) 0.0223(3) Uani 1 1 d . . . C6B C 0.44781(17) 0.78672(18) 0.62774(10) 0.0225(3) Uani 1 1 d . . . H6B H 0.4052 0.867 0.6396 0.027 Uiso 1 1 calc R . . C7B C 0.45814(19) 0.76971(19) 0.52567(11) 0.0262(3) Uani 1 1 d . . . C8B C 0.4687(2) 0.6213(2) 0.48304(11) 0.0293(4) Uani 1 1 d . . . H8B H 0.3676 0.5435 0.482 0.035 Uiso 1 1 calc R . . C9B C 0.59213(19) 0.57000(19) 0.53205(11) 0.0266(3) Uani 1 1 d . . . H9B H 0.6068 0.4944 0.4871 0.032 Uiso 1 1 calc R . . C10B C 0.55302(18) 0.49841(18) 0.61337(11) 0.0243(3) Uani 1 1 d . . . C11B C 0.4677(2) 0.34667(19) 0.59294(12) 0.0298(4) Uani 1 1 d . . . H11B H 0.4397 0.2948 0.5324 0.036 Uiso 1 1 calc R . . C12B C 0.4264(2) 0.27639(18) 0.66342(13) 0.0300(4) Uani 1 1 d . . . C13B C 0.46891(19) 0.34809(18) 0.75189(12) 0.0276(4) Uani 1 1 d . . . C14B C 0.55446(19) 0.49649(18) 0.77379(11) 0.0249(3) Uani 1 1 d . . . C15B C 0.59353(17) 0.57431(17) 0.70241(11) 0.0226(3) Uani 1 1 d . . . C16B C 0.66829(18) 0.73794(17) 0.72590(10) 0.0212(3) Uani 1 1 d . . . C17B C 0.3167(2) 0.7904(2) 0.47587(12) 0.0349(4) Uani 1 1 d . . . H17D H 0.3096 0.8833 0.5036 0.052 Uiso 1 1 calc R . . H17E H 0.2251 0.7083 0.4798 0.052 Uiso 1 1 calc R . . H17F H 0.3246 0.793 0.4122 0.052 Uiso 1 1 calc R . . C18B C 0.4885(3) 0.6218(3) 0.38383(12) 0.0454(5) Uani 1 1 d . . . H18D H 0.5875 0.6953 0.3816 0.068 Uiso 1 1 calc R . . H18E H 0.4061 0.6462 0.3503 0.068 Uiso 1 1 calc R . . H18F H 0.4845 0.5241 0.3565 0.068 Uiso 1 1 calc R . . C19B C 0.3140(3) 0.1206(2) 0.75009(15) 0.0454(5) Uani 1 1 d . . . H19C H 0.3208 0.0296 0.7701 0.054 Uiso 1 1 calc R . . H19D H 0.2088 0.1205 0.7501 0.054 Uiso 1 1 calc R . . C20B C 0.4902(3) 0.5579(3) 0.91542(14) 0.0474(5) Uani 1 1 d . . . H20D H 0.4112 0.5908 0.8855 0.071 Uiso 1 1 calc R . . H20E H 0.5362 0.6196 0.9751 0.071 Uiso 1 1 calc R . . H20F H 0.4439 0.455 0.9225 0.071 Uiso 1 1 calc R . . C21B C 0.9547(2) 0.7223(2) 0.89855(13) 0.0380(4) Uani 1 1 d . . . H21D H 1.0619 0.7874 0.9079 0.057 Uiso 1 1 calc R . . H21E H 0.9501 0.6261 0.9134 0.057 Uiso 1 1 calc R . . H21F H 0.9005 0.7659 0.9377 0.057 Uiso 1 1 calc R . . C22B C 1.0521(3) 1.0852(2) 0.94700(14) 0.0444(5) Uani 1 1 d . . . H22D H 1.0057 1.1614 0.9449 0.067 Uiso 1 1 calc R . . H22E H 1.1614 1.1313 0.973 0.067 Uiso 1 1 calc R . . H22F H 1.0021 1.0156 0.9845 0.067 Uiso 1 1 calc R . . C23B C 0.8115(2) 1.28831(19) 0.77238(13) 0.0323(4) Uani 1 1 d . . . H23D H 0.7909 1.2732 0.7061 0.048 Uiso 1 1 calc R . . H23E H 0.8747 1.3915 0.7965 0.048 Uiso 1 1 calc R . . H23F H 0.7146 1.2645 0.7944 0.048 Uiso 1 1 calc R . . C24B C 0.27403(18) 0.65992(19) 0.71586(11) 0.0262(3) Uani 1 1 d . . . C25B C 0.1566(2) 0.5144(2) 0.71925(13) 0.0368(4) Uani 1 1 d . . . H25D H 0.1432 0.5091 0.7819 0.055 Uiso 1 1 calc R . . H25E H 0.1907 0.4347 0.6962 0.055 Uiso 1 1 calc R . . H25F H 0.059 0.5043 0.6818 0.055 Uiso 1 1 calc R . . C26B C 0.8652(2) 0.6634(2) 0.57371(12) 0.0340(4) Uani 1 1 d . . . C27B C 1.0007(2) 0.7994(2) 0.61217(14) 0.0377(4) Uani 1 1 d . . . H27D H 1.0392 0.7961 0.675 0.057 Uiso 1 1 calc R . . H27E H 0.9708 0.8863 0.6102 0.057 Uiso 1 1 calc R . . H27F H 1.0812 0.805 0.5766 0.057 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 O1A 0.0307(6) 0.0377(7) 0.0293(6) 0.0146(5) 0.0085(5) 0.0208(5) O2A 0.0355(7) 0.0257(6) 0.0384(7) 0.0143(5) 0.0145(5) 0.0142(5) O3A 0.0230(6) 0.0279(6) 0.0471(8) 0.0120(5) 0.0068(5) 0.0090(5) O4A 0.0328(6) 0.0239(6) 0.0242(6) 0.0060(5) 0.0073(5) 0.0104(5) O5A 0.0461(8) 0.0402(8) 0.0325(7) -0.0028(6) 0.0129(6) 0.0108(6) O6A 0.0430(8) 0.0325(7) 0.0334(7) 0.0018(6) -0.0088(6) 0.0135(6) O7A 0.0382(7) 0.0280(6) 0.0279(6) 0.0038(5) 0.0016(5) 0.0187(5) O8A 0.0536(9) 0.0518(9) 0.0521(9) 0.0167(7) 0.0170(7) 0.0369(8) O9A 0.0294(7) 0.0519(8) 0.0586(9) 0.0206(7) 0.0205(6) 0.0122(6) O10A 0.0249(7) 0.0550(9) 0.0492(9) 0.0096(7) 0.0057(6) 0.0039(6) O11A 0.0317(7) 0.0581(9) 0.0217(6) 0.0034(6) 0.0033(5) 0.0093(6) C1A 0.0253(8) 0.0266(8) 0.0219(8) 0.0051(6) 0.0039(6) 0.0137(7) C2A 0.0293(8) 0.0196(7) 0.0257(8) 0.0048(6) 0.0054(6) 0.0096(7) C3A 0.0228(8) 0.0221(8) 0.0279(8) 0.0010(6) 0.0034(6) 0.0070(7) C4A 0.0268(8) 0.0235(8) 0.0289(8) 0.0042(6) 0.0006(7) 0.0121(7) C5A 0.0276(8) 0.0212(8) 0.0195(7) 0.0021(6) 0.0013(6) 0.0102(7) C6A 0.0291(9) 0.0245(8) 0.0254(8) 0.0056(6) 0.0017(7) 0.0125(7) C7A 0.0412(10) 0.0286(9) 0.0246(8) 0.0051(7) -0.0015(7) 0.0170(8) C8A 0.0523(11) 0.0361(10) 0.0212(8) 0.0071(7) 0.0056(8) 0.0263(9) C9A 0.0427(10) 0.0328(9) 0.0234(8) 0.0071(7) 0.0091(7) 0.0199(8) C10A 0.0351(9) 0.0282(8) 0.0253(8) 0.0098(7) 0.0087(7) 0.0180(7) C11A 0.0405(10) 0.0364(10) 0.0316(9) 0.0132(8) 0.0179(8) 0.0216(8) C12A 0.0288(9) 0.0326(9) 0.0439(11) 0.0158(8) 0.0166(8) 0.0155(8) C13A 0.0250(8) 0.0283(9) 0.0354(10) 0.0082(7) 0.0039(7) 0.0105(7) C14A 0.0288(8) 0.0311(9) 0.0260(8) 0.0095(7) 0.0065(7) 0.0147(7) C15A 0.0274(8) 0.0255(8) 0.0236(8) 0.0097(6) 0.0071(6) 0.0135(7) C16A 0.0255(8) 0.0243(8) 0.0208(8) 0.0026(6) 0.0044(6) 0.0104(6) C17A 0.0623(13) 0.0402(11) 0.0278(9) 0.0088(8) -0.0006(9) 0.0311(10) C18A 0.0887(18) 0.0613(14) 0.0215(9) 0.0036(9) 0.0027(10) 0.0491(14) C19A 0.0421(13) 0.0534(14) 0.0753(18) -0.0216(12) 0.0277(12) -0.0039(11) C20A 0.0506(13) 0.0774(17) 0.0295(11) -0.0022(11) 0.0013(9) 0.0058(12) C21A 0.0391(11) 0.0698(14) 0.0374(11) 0.0313(10) 0.0091(8) 0.0282(10) C22A 0.0423(11) 0.0428(11) 0.0394(10) 0.0187(8) 0.0169(9) 0.0227(9) C23A 0.0257(9) 0.0326(10) 0.0536(12) 0.0102(8) 0.0075(8) 0.0130(8) C24A 0.0386(10) 0.0265(8) 0.0236(8) 0.0068(7) 0.0024(7) 0.0130(7) C25A 0.0437(11) 0.0309(9) 0.0349(10) 0.0111(8) 0.0017(8) 0.0056(8) C26A 0.0474(11) 0.0328(10) 0.0252(9) -0.0004(7) -0.0010(8) 0.0237(9) C27A 0.0436(11) 0.0278(9) 0.0422(11) 0.0011(8) -0.0042(9) 0.0137(8) O1B 0.0290(6) 0.0287(6) 0.0282(6) 0.0053(5) -0.0013(5) 0.0147(5) O2B 0.0220(6) 0.0313(6) 0.0328(7) 0.0025(5) -0.0026(5) 0.0073(5) O3B 0.0264(6) 0.0224(6) 0.0403(7) 0.0049(5) 0.0001(5) 0.0069(5) O4B 0.0224(6) 0.0273(6) 0.0220(6) 0.0033(4) 0.0045(4) 0.0071(5) O5B 0.0364(7) 0.0422(7) 0.0279(6) -0.0012(6) 0.0097(5) 0.0105(6) O6B 0.0313(7) 0.0421(7) 0.0329(7) 0.0184(6) 0.0097(5) 0.0158(6) O7B 0.0248(6) 0.0364(7) 0.0279(6) 0.0106(5) 0.0081(5) 0.0158(5) O8B 0.0469(9) 0.0539(9) 0.0668(11) -0.0090(8) -0.0062(8) 0.0348(8) O9B 0.0449(8) 0.0229(6) 0.0466(8) 0.0038(5) 0.0072(6) 0.0036(6) O10B 0.0416(8) 0.0289(6) 0.0393(7) 0.0144(6) 0.0084(6) 0.0070(6) O11B 0.0390(7) 0.0363(7) 0.0201(6) 0.0057(5) 0.0045(5) 0.0084(6) C1B 0.0252(8) 0.0270(8) 0.0200(8) 0.0052(6) 0.0047(6) 0.0119(7) C2B 0.0199(8) 0.0277(8) 0.0221(8) 0.0036(6) 0.0030(6) 0.0077(6) C3B 0.0236(8) 0.0231(8) 0.0262(8) 0.0047(6) 0.0062(6) 0.0069(7) C4B 0.0260(8) 0.0260(8) 0.0264(8) 0.0076(6) 0.0060(6) 0.0122(7) C5B 0.0226(8) 0.0268(8) 0.0197(7) 0.0053(6) 0.0054(6) 0.0108(7) C6B 0.0203(8) 0.0267(8) 0.0218(8) 0.0062(6) 0.0040(6) 0.0092(6) C7B 0.0248(8) 0.0369(9) 0.0216(8) 0.0100(7) 0.0038(6) 0.0153(7) C8B 0.0312(9) 0.0435(10) 0.0178(8) 0.0043(7) 0.0037(7) 0.0198(8) C9B 0.0275(9) 0.0333(9) 0.0209(8) 0.0027(6) 0.0037(6) 0.0143(7) C10B 0.0242(8) 0.0280(8) 0.0233(8) 0.0043(7) 0.0028(6) 0.0131(7) C11B 0.0320(9) 0.0297(9) 0.0264(9) -0.0009(7) 0.0003(7) 0.0130(7) C12B 0.0283(9) 0.0221(8) 0.0385(10) 0.0035(7) 0.0023(7) 0.0096(7) C13B 0.0264(9) 0.0267(8) 0.0312(9) 0.0117(7) 0.0043(7) 0.0093(7) C14B 0.0258(8) 0.0271(8) 0.0221(8) 0.0052(6) 0.0013(6) 0.0106(7) C15B 0.0198(8) 0.0242(8) 0.0244(8) 0.0051(6) 0.0021(6) 0.0092(6) C16B 0.0247(8) 0.0242(8) 0.0166(7) 0.0046(6) 0.0055(6) 0.0102(6) C17B 0.0352(10) 0.0513(11) 0.0257(9) 0.0097(8) 0.0025(7) 0.0253(9) C18B 0.0548(13) 0.0781(15) 0.0202(9) 0.0103(9) 0.0084(8) 0.0445(12) C19B 0.0463(12) 0.0292(10) 0.0537(13) 0.0095(9) 0.0126(10) 0.0020(9) C20B 0.0567(13) 0.0639(14) 0.0315(10) 0.0086(9) 0.0143(9) 0.0318(12) C21B 0.0410(11) 0.0342(10) 0.0349(10) 0.0086(8) -0.0108(8) 0.0142(8) C22B 0.0502(12) 0.0370(11) 0.0371(11) -0.0062(8) -0.0133(9) 0.0163(9) C23B 0.0341(9) 0.0235(8) 0.0402(10) 0.0081(7) 0.0063(8) 0.0108(7) C24B 0.0219(8) 0.0357(9) 0.0210(8) 0.0059(7) 0.0022(6) 0.0104(7) C25B 0.0292(9) 0.0435(11) 0.0333(10) 0.0120(8) 0.0056(8) 0.0056(8) C26B 0.0347(10) 0.0507(12) 0.0265(9) 0.0078(8) 0.0090(7) 0.0261(9) C27B 0.0274(9) 0.0520(12) 0.0390(10) 0.0144(9) 0.0110(8) 0.0166(9) #----------------------------------------------------------------------------# # 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 O1A C1A 1.3733(19) . ? O1A C21A 1.428(2) . ? O2A C2A 1.3824(19) . ? O2A C22A 1.429(2) . ? O3A C3A 1.370(2) . ? O3A C23A 1.432(2) . ? O4A C24A 1.349(2) . ? O4A C6A 1.444(2) . ? O5A C24A 1.203(2) . ? O6A C7A 1.427(2) . ? O6A H06A 0.87(3) . ? O7A C26A 1.358(2) . ? O7A C9A 1.456(2) . ? O8A C26A 1.206(2) . ? O9A C12A 1.385(2) . ? O9A C19A 1.438(3) . ? O10A C13A 1.393(2) . ? O10A C19A 1.398(3) . ? O11A C14A 1.363(2) . ? O11A C20A 1.414(2) . ? C1A C2A 1.393(2) . ? C1A C16A 1.406(2) . ? C2A C3A 1.405(2) . ? C3A C4A 1.381(2) . ? C4A C5A 1.396(2) . ? C4A H4A 0.95 . ? C5A C16A 1.390(2) . ? C5A C6A 1.515(2) . ? C6A C7A 1.560(2) . ? C6A H6A 1 . ? C7A C17A 1.531(2) . ? C7A C8A 1.556(3) . ? C8A C18A 1.541(3) . ? C8A C9A 1.548(2) . ? C8A H8A 1 . ? C9A C10A 1.518(3) . ? C9A H9A 1 . ? C10A C15A 1.394(2) . ? C10A C11A 1.402(3) . ? C11A C12A 1.363(3) . ? C11A H11A 0.95 . ? C12A C13A 1.385(3) . ? C13A C14A 1.381(2) . ? C14A C15A 1.418(2) . ? C15A C16A 1.492(2) . ? C17A H17A 0.98 . ? C17A H17B 0.98 . ? C17A H17C 0.98 . ? C18A H18A 0.98 . ? C18A H18B 0.98 . ? C18A H18C 0.98 . ? C19A H19A 0.99 . ? C19A H19B 0.99 . ? C20A H20A 0.98 . ? C20A H20B 0.98 . ? C20A H20C 0.98 . ? C21A H21A 0.98 . ? C21A H21B 0.98 . ? C21A H21C 0.98 . ? C22A H22A 0.98 . ? C22A H22B 0.98 . ? C22A H22C 0.98 . ? C23A H23A 0.98 . ? C23A H23B 0.98 . ? C23A H23C 0.98 . ? C24A C25A 1.493(3) . ? C25A H25A 0.98 . ? C25A H25B 0.98 . ? C25A H25C 0.98 . ? C26A C27A 1.492(3) . ? C27A H27A 0.98 . ? C27A H27B 0.98 . ? C27A H27C 0.98 . ? O1B C1B 1.3695(19) . ? O1B C21B 1.435(2) . ? O2B C2B 1.3827(19) . ? O2B C22B 1.440(2) . ? O3B C3B 1.375(2) . ? O3B C23B 1.433(2) . ? O4B C24B 1.3498(19) . ? O4B C6B 1.4464(19) . ? O5B C24B 1.202(2) . ? O6B C7B 1.432(2) . ? O6B HO6B 0.87(3) . ? O7B C26B 1.352(2) . ? O7B C9B 1.456(2) . ? O8B C26B 1.195(2) . ? O9B C12B 1.389(2) . ? O9B C19B 1.437(3) . ? O10B C13B 1.386(2) . ? O10B C19B 1.440(2) . ? O11B C14B 1.373(2) . ? O11B C20B 1.432(2) . ? C1B C2B 1.395(2) . ? C1B C16B 1.407(2) . ? C2B C3B 1.397(2) . ? C3B C4B 1.384(2) . ? C4B C5B 1.395(2) . ? C4B H4B 0.95 . ? C5B C16B 1.394(2) . ? C5B C6B 1.523(2) . ? C6B C7B 1.555(2) . ? C6B H6B 1 . ? C7B C17B 1.524(2) . ? C7B C8B 1.554(2) . ? C8B C18B 1.540(2) . ? C8B C9B 1.546(2) . ? C8B H8B 1 . ? C9B C10B 1.517(2) . ? C9B H9B 1 . ? C10B C15B 1.397(2) . ? C10B C11B 1.406(2) . ? C11B C12B 1.369(3) . ? C11B H11B 0.95 . ? C12B C13B 1.376(3) . ? C13B C14B 1.379(2) . ? C14B C15B 1.415(2) . ? C15B C16B 1.493(2) . ? C17B H17D 0.98 . ? C17B H17E 0.98 . ? C17B H17F 0.98 . ? C18B H18D 0.98 . ? C18B H18E 0.98 . ? C18B H18F 0.98 . ? C19B H19C 0.99 . ? C19B H19D 0.99 . ? C20B H20D 0.98 . ? C20B H20E 0.98 . ? C20B H20F 0.98 . ? C21B H21D 0.98 . ? C21B H21E 0.98 . ? C21B H21F 0.98 . ? C22B H22D 0.98 . ? C22B H22E 0.98 . ? C22B H22F 0.98 . ? C23B H23D 0.98 . ? C23B H23E 0.98 . ? C23B H23F 0.98 . ? C24B C25B 1.497(3) . ? C25B H25D 0.98 . ? C25B H25E 0.98 . ? C25B H25F 0.98 . ? C26B C27B 1.493(3) . ? C27B H27D 0.98 . ? C27B H27E 0.98 . ? C27B H27F 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 C1A O1A C21A 117.19(13) . . ? C2A O2A C22A 116.90(13) . . ? C3A O3A C23A 116.82(13) . . ? C24A O4A C6A 117.11(13) . . ? C7A O6A H06A 108.3(19) . . ? C26A O7A C9A 115.99(14) . . ? C12A O9A C19A 105.03(15) . . ? C13A O10A C19A 105.43(16) . . ? C14A O11A C20A 119.91(16) . . ? O1A C1A C2A 121.83(14) . . ? O1A C1A C16A 116.55(14) . . ? C2A C1A C16A 121.30(14) . . ? O2A C2A C1A 118.59(14) . . ? O2A C2A C3A 121.74(14) . . ? C1A C2A C3A 119.35(14) . . ? O3A C3A C4A 123.70(14) . . ? O3A C3A C2A 117.03(14) . . ? C4A C3A C2A 119.26(15) . . ? C3A C4A C5A 121.35(15) . . ? C3A C4A H4A 119.3 . . ? C5A C4A H4A 119.3 . . ? C16A C5A C4A 120.08(14) . . ? C16A C5A C6A 124.96(15) . . ? C4A C5A C6A 114.81(14) . . ? O4A C6A C5A 115.46(13) . . ? O4A C6A C7A 106.15(13) . . ? C5A C6A C7A 115.07(13) . . ? O4A C6A H6A 106.5 . . ? C5A C6A H6A 106.5 . . ? C7A C6A H6A 106.5 . . ? O6A C7A C17A 104.98(15) . . ? O6A C7A C8A 111.64(14) . . ? C17A C7A C8A 109.50(16) . . ? O6A C7A C6A 107.89(14) . . ? C17A C7A C6A 106.26(14) . . ? C8A C7A C6A 115.89(14) . . ? C18A C8A C9A 108.03(15) . . ? C18A C8A C7A 110.77(17) . . ? C9A C8A C7A 118.34(15) . . ? C18A C8A H8A 106.3 . . ? C9A C8A H8A 106.3 . . ? C7A C8A H8A 106.3 . . ? O7A C9A C10A 113.21(14) . . ? O7A C9A C8A 108.33(15) . . ? C10A C9A C8A 115.41(15) . . ? O7A C9A H9A 106.4 . . ? C10A C9A H9A 106.4 . . ? C8A C9A H9A 106.4 . . ? C15A C10A C11A 120.96(16) . . ? C15A C10A C9A 123.90(16) . . ? C11A C10A C9A 115.09(15) . . ? C12A C11A C10A 117.42(16) . . ? C12A C11A H11A 121.3 . . ? C10A C11A H11A 121.3 . . ? C11A C12A C13A 122.88(16) . . ? C11A C12A O9A 127.95(17) . . ? C13A C12A O9A 109.17(16) . . ? C14A C13A C12A 120.83(16) . . ? C14A C13A O10A 129.52(16) . . ? C12A C13A O10A 109.61(15) . . ? O11A C14A C13A 125.61(16) . . ? O11A C14A C15A 116.80(14) . . ? C13A C14A C15A 117.49(15) . . ? C10A C15A C14A 120.40(15) . . ? C10A C15A C16A 121.82(14) . . ? C14A C15A C16A 117.65(14) . . ? C5A C16A C1A 118.59(14) . . ? C5A C16A C15A 121.91(14) . . ? C1A C16A C15A 119.49(13) . . ? C7A C17A H17A 109.5 . . ? C7A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C7A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C8A C18A H18A 109.5 . . ? C8A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C8A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? O10A C19A O9A 108.90(18) . . ? O10A C19A H19A 109.9 . . ? O9A C19A H19A 109.9 . . ? O10A C19A H19B 109.9 . . ? O9A C19A H19B 109.9 . . ? H19A C19A H19B 108.3 . . ? O11A C20A H20A 109.5 . . ? O11A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? O11A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? O1A C21A H21A 109.5 . . ? O1A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? O1A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? O2A C22A H22A 109.5 . . ? O2A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? O2A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? O3A C23A H23A 109.5 . . ? O3A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? O3A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? O5A C24A O4A 123.39(16) . . ? O5A C24A C25A 126.04(17) . . ? O4A C24A C25A 110.56(15) . . ? C24A C25A H25A 109.5 . . ? C24A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C24A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? O8A C26A O7A 122.82(18) . . ? O8A C26A C27A 125.03(17) . . ? O7A C26A C27A 112.11(16) . . ? C26A C27A H27A 109.5 . . ? C26A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C26A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C1B O1B C21B 117.70(13) . . ? C2B O2B C22B 115.32(14) . . ? C3B O3B C23B 115.84(13) . . ? C24B O4B C6B 116.41(12) . . ? C7B O6B HO6B 105.4(17) . . ? C26B O7B C9B 116.80(13) . . ? C12B O9B C19B 103.88(14) . . ? C13B O10B C19B 103.15(14) . . ? C14B O11B C20B 115.32(15) . . ? O1B C1B C2B 121.77(14) . . ? O1B C1B C16B 116.39(14) . . ? C2B C1B C16B 121.51(14) . . ? O2B C2B C1B 119.08(14) . . ? O2B C2B C3B 121.18(14) . . ? C1B C2B C3B 119.45(14) . . ? O3B C3B C4B 123.86(14) . . ? O3B C3B C2B 116.71(14) . . ? C4B C3B C2B 119.41(14) . . ? C3B C4B C5B 121.14(15) . . ? C3B C4B H4B 119.4 . . ? C5B C4B H4B 119.4 . . ? C16B C5B C4B 120.43(14) . . ? C16B C5B C6B 125.49(14) . . ? C4B C5B C6B 114.04(13) . . ? O4B C6B C5B 114.54(12) . . ? O4B C6B C7B 106.94(12) . . ? C5B C6B C7B 116.06(13) . . ? O4B C6B H6B 106.2 . . ? C5B C6B H6B 106.2 . . ? C7B C6B H6B 106.2 . . ? O6B C7B C17B 104.59(14) . . ? O6B C7B C8B 111.78(14) . . ? C17B C7B C8B 109.74(14) . . ? O6B C7B C6B 107.67(13) . . ? C17B C7B C6B 106.56(13) . . ? C8B C7B C6B 115.79(13) . . ? C18B C8B C9B 108.19(14) . . ? C18B C8B C7B 110.80(15) . . ? C9B C8B C7B 117.59(14) . . ? C18B C8B H8B 106.5 . . ? C9B C8B H8B 106.5 . . ? C7B C8B H8B 106.5 . . ? O7B C9B C10B 112.12(13) . . ? O7B C9B C8B 108.06(13) . . ? C10B C9B C8B 115.76(14) . . ? O7B C9B H9B 106.8 . . ? C10B C9B H9B 106.8 . . ? C8B C9B H9B 106.8 . . ? C15B C10B C11B 121.01(15) . . ? C15B C10B C9B 124.13(15) . . ? C11B C10B C9B 114.85(14) . . ? C12B C11B C10B 117.57(16) . . ? C12B C11B H11B 121.2 . . ? C10B C11B H11B 121.2 . . ? C11B C12B C13B 122.37(16) . . ? C11B C12B O9B 128.26(16) . . ? C13B C12B O9B 109.18(15) . . ? C12B C13B C14B 121.14(15) . . ? C12B C13B O10B 110.31(15) . . ? C14B C13B O10B 128.37(16) . . ? O11B C14B C13B 122.72(15) . . ? O11B C14B C15B 119.16(15) . . ? C13B C14B C15B 118.10(15) . . ? C10B C15B C14B 119.70(15) . . ? C10B C15B C16B 122.64(14) . . ? C14B C15B C16B 117.53(14) . . ? C5B C16B C1B 118.05(14) . . ? C5B C16B C15B 122.24(14) . . ? C1B C16B C15B 119.70(13) . . ? C7B C17B H17D 109.5 . . ? C7B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C7B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C8B C18B H18D 109.5 . . ? C8B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C8B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? O9B C19B O10B 107.01(15) . . ? O9B C19B H19C 110.3 . . ? O10B C19B H19C 110.3 . . ? O9B C19B H19D 110.3 . . ? O10B C19B H19D 110.3 . . ? H19C C19B H19D 108.6 . . ? O11B C20B H20D 109.5 . . ? O11B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? O11B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? O1B C21B H21D 109.5 . . ? O1B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? O1B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? O2B C22B H22D 109.5 . . ? O2B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? O2B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? O3B C23B H23D 109.5 . . ? O3B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? O3B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? O5B C24B O4B 123.61(16) . . ? O5B C24B C25B 125.73(16) . . ? O4B C24B C25B 110.65(14) . . ? C24B C25B H25D 109.5 . . ? C24B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? O8B C26B O7B 123.12(18) . . ? O8B C26B C27B 125.16(17) . . ? O7B C26B C27B 111.71(16) . . ? C26B C27B H27D 109.5 . . ? C26B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C26B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 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 C21A O1A C1A C2A 55.7(2) . . . . ? C21A O1A C1A C16A -130.71(17) . . . . ? C22A O2A C2A C1A -125.23(17) . . . . ? C22A O2A C2A C3A 61.3(2) . . . . ? O1A C1A C2A O2A 2.0(2) . . . . ? C16A C1A C2A O2A -171.26(15) . . . . ? O1A C1A C2A C3A 175.68(14) . . . . ? C16A C1A C2A C3A 2.4(2) . . . . ? C23A O3A C3A C4A 12.6(2) . . . . ? C23A O3A C3A C2A -168.57(15) . . . . ? O2A C2A C3A O3A -6.7(2) . . . . ? C1A C2A C3A O3A 179.88(14) . . . . ? O2A C2A C3A C4A 172.17(15) . . . . ? C1A C2A C3A C4A -1.3(2) . . . . ? O3A C3A C4A C5A 177.46(15) . . . . ? C2A C3A C4A C5A -1.3(2) . . . . ? C3A C4A C5A C16A 2.8(2) . . . . ? C3A C4A C5A C6A -172.93(15) . . . . ? C24A O4A C6A C5A 67.77(18) . . . . ? C24A O4A C6A C7A -163.44(13) . . . . ? C16A C5A C6A O4A 35.7(2) . . . . ? C4A C5A C6A O4A -148.77(14) . . . . ? C16A C5A C6A C7A -88.5(2) . . . . ? C4A C5A C6A C7A 86.98(18) . . . . ? O4A C6A C7A O6A -173.89(12) . . . . ? C5A C6A C7A O6A -44.87(18) . . . . ? O4A C6A C7A C17A 73.96(17) . . . . ? C5A C6A C7A C17A -157.02(16) . . . . ? O4A C6A C7A C8A -47.91(18) . . . . ? C5A C6A C7A C8A 81.10(19) . . . . ? O6A C7A C8A C18A -51.74(19) . . . . ? C17A C7A C8A C18A 64.1(2) . . . . ? C6A C7A C8A C18A -175.79(15) . . . . ? O6A C7A C8A C9A 73.75(19) . . . . ? C17A C7A C8A C9A -170.43(16) . . . . ? C6A C7A C8A C9A -50.3(2) . . . . ? C26A O7A C9A C10A 70.07(18) . . . . ? C26A O7A C9A C8A -160.59(13) . . . . ? C18A C8A C9A O7A 77.74(19) . . . . ? C7A C8A C9A O7A -49.1(2) . . . . ? C18A C8A C9A C10A -154.16(18) . . . . ? C7A C8A C9A C10A 79.0(2) . . . . ? O7A C9A C10A C15A 34.2(2) . . . . ? C8A C9A C10A C15A -91.5(2) . . . . ? O7A C9A C10A C11A -148.11(15) . . . . ? C8A C9A C10A C11A 86.25(19) . . . . ? C15A C10A C11A C12A 0.5(2) . . . . ? C9A C10A C11A C12A -177.32(15) . . . . ? C10A C11A C12A C13A -1.1(3) . . . . ? C10A C11A C12A O9A 178.48(17) . . . . ? C19A O9A C12A C11A 173.4(2) . . . . ? C19A O9A C12A C13A -7.0(2) . . . . ? C11A C12A C13A C14A 0.5(3) . . . . ? O9A C12A C13A C14A -179.12(15) . . . . ? C11A C12A C13A O10A 178.29(16) . . . . ? O9A C12A C13A O10A -1.3(2) . . . . ? C19A O10A C13A C14A -173.1(2) . . . . ? C19A O10A C13A C12A 9.3(2) . . . . ? C20A O11A C14A C13A 19.9(3) . . . . ? C20A O11A C14A C15A -163.95(19) . . . . ? C12A C13A C14A O11A 176.76(15) . . . . ? O10A C13A C14A O11A -0.5(3) . . . . ? C12A C13A C14A C15A 0.7(2) . . . . ? O10A C13A C14A C15A -176.64(16) . . . . ? C11A C10A C15A C14A 0.6(2) . . . . ? C9A C10A C15A C14A 178.26(15) . . . . ? C11A C10A C15A C16A -175.05(15) . . . . ? C9A C10A C15A C16A 2.6(2) . . . . ? O11A C14A C15A C10A -177.66(14) . . . . ? C13A C14A C15A C10A -1.2(2) . . . . ? O11A C14A C15A C16A -1.8(2) . . . . ? C13A C14A C15A C16A 174.66(15) . . . . ? C4A C5A C16A C1A -1.7(2) . . . . ? C6A C5A C16A C1A 173.61(15) . . . . ? C4A C5A C16A C15A 179.61(15) . . . . ? C6A C5A C16A C15A -5.1(2) . . . . ? O1A C1A C16A C5A -174.54(14) . . . . ? C2A C1A C16A C5A -0.9(2) . . . . ? O1A C1A C16A C15A 4.2(2) . . . . ? C2A C1A C16A C15A 177.85(15) . . . . ? C10A C15A C16A C5A 63.9(2) . . . . ? C14A C15A C16A C5A -111.89(17) . . . . ? C10A C15A C16A C1A -114.78(17) . . . . ? C14A C15A C16A C1A 69.4(2) . . . . ? C13A O10A C19A O9A -13.7(2) . . . . ? C12A O9A C19A O10A 12.9(2) . . . . ? C6A O4A C24A O5A 0.7(2) . . . . ? C6A O4A C24A C25A 179.50(13) . . . . ? C9A O7A C26A O8A 5.9(2) . . . . ? C9A O7A C26A C27A -171.89(14) . . . . ? C21B O1B C1B C2B 50.8(2) . . . . ? C21B O1B C1B C16B -135.68(16) . . . . ? C22B O2B C2B C1B -115.14(17) . . . . ? C22B O2B C2B C3B 71.1(2) . . . . ? O1B C1B C2B O2B 0.0(2) . . . . ? C16B C1B C2B O2B -173.15(14) . . . . ? O1B C1B C2B C3B 173.92(14) . . . . ? C16B C1B C2B C3B 0.7(2) . . . . ? C23B O3B C3B C4B 4.6(2) . . . . ? C23B O3B C3B C2B -176.98(15) . . . . ? O2B C2B C3B O3B -5.1(2) . . . . ? C1B C2B C3B O3B -178.86(14) . . . . ? O2B C2B C3B C4B 173.39(15) . . . . ? C1B C2B C3B C4B -0.4(2) . . . . ? O3B C3B C4B C5B 177.69(15) . . . . ? C2B C3B C4B C5B -0.7(2) . . . . ? C3B C4B C5B C16B 1.4(2) . . . . ? C3B C4B C5B C6B -176.36(15) . . . . ? C24B O4B C6B C5B 68.53(16) . . . . ? C24B O4B C6B C7B -161.40(12) . . . . ? C16B C5B C6B O4B 37.7(2) . . . . ? C4B C5B C6B O4B -144.64(14) . . . . ? C16B C5B C6B C7B -87.71(19) . . . . ? C4B C5B C6B C7B 89.93(17) . . . . ? O4B C6B C7B O6B -173.18(12) . . . . ? C5B C6B C7B O6B -43.97(18) . . . . ? O4B C6B C7B C17B 75.07(16) . . . . ? C5B C6B C7B C17B -155.72(15) . . . . ? O4B C6B C7B C8B -47.28(17) . . . . ? C5B C6B C7B C8B 81.93(18) . . . . ? O6B C7B C8B C18B -52.66(19) . . . . ? C17B C7B C8B C18B 62.91(19) . . . . ? C6B C7B C8B C18B -176.44(14) . . . . ? O6B C7B C8B C9B 72.46(18) . . . . ? C17B C7B C8B C9B -171.98(15) . . . . ? C6B C7B C8B C9B -51.3(2) . . . . ? C26B O7B C9B C10B 69.58(17) . . . . ? C26B O7B C9B C8B -161.66(13) . . . . ? C18B C8B C9B O7B 79.36(18) . . . . ? C7B C8B C9B O7B -47.03(18) . . . . ? C18B C8B C9B C10B -153.97(16) . . . . ? C7B C8B C9B C10B 79.6(2) . . . . ? O7B C9B C10B C15B 31.4(2) . . . . ? C8B C9B C10B C15B -93.21(19) . . . . ? O7B C9B C10B C11B -150.05(14) . . . . ? C8B C9B C10B C11B 85.36(18) . . . . ? C15B C10B C11B C12B -0.2(2) . . . . ? C9B C10B C11B C12B -178.79(15) . . . . ? C10B C11B C12B C13B -1.8(3) . . . . ? C10B C11B C12B O9B -176.33(16) . . . . ? C19B O9B C12B C11B -170.22(19) . . . . ? C19B O9B C12B C13B 14.67(19) . . . . ? C11B C12B C13B C14B 0.9(3) . . . . ? O9B C12B C13B C14B 176.39(15) . . . . ? C11B C12B C13B O10B -174.65(16) . . . . ? O9B C12B C13B O10B 0.8(2) . . . . ? C19B O10B C13B C12B -15.84(19) . . . . ? C19B O10B C13B C14B 168.99(18) . . . . ? C20B O11B C14B C13B -55.0(2) . . . . ? C20B O11B C14B C15B 126.68(17) . . . . ? C12B C13B C14B O11B -176.40(16) . . . . ? O10B C13B C14B O11B -1.7(3) . . . . ? C12B C13B C14B C15B 1.9(2) . . . . ? O10B C13B C14B C15B 176.59(16) . . . . ? C11B C10B C15B C14B 3.0(2) . . . . ? C9B C10B C15B C14B -178.57(14) . . . . ? C11B C10B C15B C16B -172.82(15) . . . . ? C9B C10B C15B C16B 5.7(2) . . . . ? O11B C14B C15B C10B 174.59(14) . . . . ? C13B C14B C15B C10B -3.8(2) . . . . ? O11B C14B C15B C16B -9.4(2) . . . . ? C13B C14B C15B C16B 172.23(15) . . . . ? C4B C5B C16B C1B -1.0(2) . . . . ? C6B C5B C16B C1B 176.47(14) . . . . ? C4B C5B C16B C15B 177.77(15) . . . . ? C6B C5B C16B C15B -4.7(2) . . . . ? O1B C1B C16B C5B -173.58(13) . . . . ? C2B C1B C16B C5B 0.0(2) . . . . ? O1B C1B C16B C15B 7.6(2) . . . . ? C2B C1B C16B C15B -178.86(14) . . . . ? C10B C15B C16B C5B 60.2(2) . . . . ? C14B C15B C16B C5B -115.63(16) . . . . ? C10B C15B C16B C1B -120.99(16) . . . . ? C14B C15B C16B C1B 63.2(2) . . . . ? C12B O9B C19B O10B -24.4(2) . . . . ? C13B O10B C19B O9B 24.7(2) . . . . ? C6B O4B C24B O5B 0.2(2) . . . . ? C6B O4B C24B C25B 179.70(13) . . . . ? C9B O7B C26B O8B 9.5(2) . . . . ? C9B O7B C26B C27B -169.26(14) . . . . ? 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 O6B HO6B O7B 0.87(3) 2.11(3) 2.8377(17) 140(2) . O6A H06A O7A 0.87(3) 2.23(3) 2.8957(18) 133(2) . _database_code_depnum_ccdc_archive 'CCDC 911247' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_RajanBabu1872 #TrackingRef '18991_web_deposit_cif_file_1_RajanBabu.T.V_1364518612.archive_19c.cif' _audit_creation_date 2011-12-30T14:04:54-00:00 _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 1872' _chemical_formula_moiety 'C45 H63 B1 O10 Si1 Sn1' _chemical_formula_sum 'C45 H63 B O10 Si Sn' _chemical_formula_weight 921.54 _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 -P1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9576(1) _cell_length_b 12.6539(1) _cell_length_c 16.2477(1) _cell_angle_alpha 96.233(1) _cell_angle_beta 98.572(1) _cell_angle_gamma 100.371(1) _cell_volume 2367.98(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10832 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'trapezoidal plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _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 3.8, which means that 90% of these reflections were measured at least 3.8 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 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.929 _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 Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.231171E-1 _diffrn_orient_matrix_ub_12 0.70505E-2 _diffrn_orient_matrix_ub_13 0.566999E-1 _diffrn_orient_matrix_ub_21 0.781066E-1 _diffrn_orient_matrix_ub_22 -0.93512E-2 _diffrn_orient_matrix_ub_23 0.262286E-1 _diffrn_orient_matrix_ub_31 0.28538E-1 _diffrn_orient_matrix_ub_32 0.802797E-1 _diffrn_orient_matrix_ub_33 0.69178E-2 _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 0.040 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 71828 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 10850 _reflns_number_gt 8712 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _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 heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;The five-membered ring containing the boron atom may be disordered, as the final difference map shows several residual peaks located in this area. After fiddling around with a potential disorder model, it was not possible to come up with anything that made geometrical sense. For the final model, CheckCIF notes that there is a short intermolecular distance for H35C...H35C of 1.87 Ang., which may be another indication that the five-membered ring containing the boron atom is disordered. For each methyl group, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5*Ueq(bonded 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^)+(0.0569P)^2^+1.7606P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10850 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.246 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # 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' Si Si 0.0817 0.0704 '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 0.50292(19) 0.85319(19) 0.29720(14) 0.0230(5) Uani 1 1 d . . . C2 C 0.6209(2) 0.86666(18) 0.32579(14) 0.0232(5) Uani 1 1 d . . . C3 C 0.6652(2) 0.8748(2) 0.41185(15) 0.0270(5) Uani 1 1 d . . . H3 H 0.7457 0.8841 0.4319 0.032 Uiso 1 1 calc R . . C4 C 0.5871(2) 0.8688(2) 0.46528(15) 0.0299(5) Uani 1 1 d . . . C5 C 0.5008(2) 0.8585(3) 0.57772(16) 0.0396(7) Uani 1 1 d . . . H5A H 0.4882 0.7895 0.6016 0.047 Uiso 1 1 calc R . . H5B H 0.498 0.9181 0.6217 0.047 Uiso 1 1 calc R . . C6 C 0.4693(2) 0.8560(2) 0.43861(15) 0.0303(5) Uani 1 1 d . . . C7 C 0.4239(2) 0.8482(2) 0.35445(15) 0.0271(5) Uani 1 1 d . . . C8 C 0.45579(19) 0.8387(2) 0.20519(14) 0.0240(5) Uani 1 1 d . . . C9 C 0.40370(19) 0.9184(2) 0.16994(14) 0.0245(5) Uani 1 1 d . . . C10 C 0.3590(2) 0.9053(2) 0.08433(15) 0.0274(5) Uani 1 1 d . . . C11 C 0.3684(2) 0.8121(2) 0.03270(14) 0.0291(5) Uani 1 1 d . . . C12 C 0.4217(2) 0.7346(2) 0.06639(15) 0.0282(5) Uani 1 1 d . . . H12 H 0.4294 0.6726 0.0307 0.034 Uiso 1 1 calc R . . C13 C 0.46416(19) 0.74627(19) 0.15216(14) 0.0239(5) Uani 1 1 d . . . C14 C 0.5210(2) 0.65695(19) 0.18596(15) 0.0248(5) Uani 1 1 d . . . H14 H 0.5151 0.6563 0.2467 0.03 Uiso 1 1 calc R . . C15 C 0.64785(19) 0.67885(18) 0.17615(14) 0.0228(5) Uani 1 1 d . . . C16 C 0.7304(2) 0.75450(19) 0.24503(14) 0.0228(5) Uani 1 1 d . . . C17 C 0.70694(19) 0.86917(18) 0.26476(14) 0.0224(5) Uani 1 1 d . . . H17 H 0.6741 0.8941 0.2117 0.027 Uiso 1 1 calc R . . C18 C 0.2287(2) 0.8401(3) 0.37593(17) 0.0413(7) Uani 1 1 d . . . H18A H 0.1507 0.828 0.3432 0.062 Uiso 1 1 calc R . . H18B H 0.247 0.9121 0.4095 0.062 Uiso 1 1 calc R . . H18C H 0.2329 0.7846 0.4133 0.062 Uiso 1 1 calc R . . C19 C 0.2987(2) 1.0467(2) 0.22629(18) 0.0383(6) Uani 1 1 d . . . H19A H 0.3124 1.1141 0.2654 0.057 Uiso 1 1 calc R . . H19B H 0.2456 0.9903 0.2459 0.057 Uiso 1 1 calc R . . H19C H 0.2647 1.059 0.1703 0.057 Uiso 1 1 calc R . . C20 C 0.3727(3) 1.0617(3) 0.0157(2) 0.0460(7) Uani 1 1 d . . . H20A H 0.326 1.1119 -0.0062 0.069 Uiso 1 1 calc R . . H20B H 0.4037 1.0264 -0.0301 0.069 Uiso 1 1 calc R . . H20C H 0.4365 1.1019 0.0591 0.069 Uiso 1 1 calc R . . C21 C 0.3335(3) 0.7137(3) -0.10468(17) 0.0541(9) Uani 1 1 d . . . H21A H 0.2977 0.7178 -0.1622 0.081 Uiso 1 1 calc R . . H21B H 0.2949 0.6477 -0.086 0.081 Uiso 1 1 calc R . . H21C H 0.4154 0.7119 -0.1031 0.081 Uiso 1 1 calc R . . C22 C 0.3495(2) 0.5160(2) 0.1489(2) 0.0429(7) Uani 1 1 d . . . H22A H 0.315 0.451 0.1072 0.051 Uiso 1 1 calc R . . H22B H 0.3055 0.5733 0.1367 0.051 Uiso 1 1 calc R . . C23 C 0.3375(2) 0.4884(2) 0.2358(2) 0.0422(7) Uani 1 1 d . . . C24 C 0.3106(3) 0.5620(3) 0.2950(3) 0.0650(11) Uani 1 1 d . . . H24 H 0.2975 0.6298 0.2801 0.078 Uiso 1 1 calc R . . C25 C 0.3023(5) 0.5394(4) 0.3757(3) 0.0928(17) Uani 1 1 d . . . H25 H 0.2842 0.5912 0.4158 0.111 Uiso 1 1 calc R . . C26 C 0.3207(4) 0.4397(4) 0.3970(3) 0.0850(14) Uani 1 1 d . . . H26 H 0.3186 0.4241 0.4527 0.102 Uiso 1 1 calc R . . C27 C 0.3422(4) 0.3636(4) 0.3372(3) 0.0745(12) Uani 1 1 d . . . H27 H 0.3503 0.2938 0.3506 0.089 Uiso 1 1 calc R . . C28 C 0.3519(3) 0.3892(3) 0.2573(2) 0.0564(9) Uani 1 1 d . . . H28 H 0.3689 0.3371 0.2168 0.068 Uiso 1 1 calc R . . C29 C 0.6842(2) 0.6360(2) 0.10876(15) 0.0262(5) Uani 1 1 d . . . H29 H 0.6333 0.577 0.0729 0.031 Uiso 1 1 calc R . . C30 C 0.9725(2) 0.7889(2) 0.07941(19) 0.0401(6) Uani 1 1 d . . . C31 C 0.9639(3) 0.6832(2) 0.0225(2) 0.0438(7) Uani 1 1 d . . . C32 C 1.0124(3) 0.8917(3) 0.0463(3) 0.0596(10) Uani 1 1 d . . . H32A H 1.0148 0.9535 0.0889 0.089 Uiso 1 1 calc R . . H32B H 0.959 0.8961 -0.0046 0.089 Uiso 1 1 calc R . . H32C H 1.0898 0.893 0.0328 0.089 Uiso 1 1 calc R . . C33 C 1.0466(3) 0.7919(3) 0.1661(2) 0.0602(9) Uani 1 1 d . . . H33A H 1.0214 0.7247 0.1889 0.09 Uiso 1 1 calc R . . H33B H 1.0376 0.854 0.2044 0.09 Uiso 1 1 calc R . . H33C H 1.1279 0.7989 0.1602 0.09 Uiso 1 1 calc R . . C34 C 0.9248(4) 0.6905(4) -0.0704(2) 0.0747(13) Uani 1 1 d . . . H34A H 0.8551 0.7215 -0.0768 0.112 Uiso 1 1 calc R . . H34B H 0.908 0.6178 -0.1027 0.112 Uiso 1 1 calc R . . H34C H 0.9862 0.737 -0.0912 0.112 Uiso 1 1 calc R . . C35 C 1.0702(3) 0.6355(3) 0.0309(3) 0.0743(13) Uani 1 1 d . . . H35A H 1.0957 0.6298 0.0902 0.111 Uiso 1 1 calc R . . H35B H 1.1314 0.6823 0.0102 0.111 Uiso 1 1 calc R . . H35C H 1.053 0.5632 -0.0021 0.111 Uiso 1 1 calc R . . C36 C 0.8168(2) 0.7221(2) 0.29104(15) 0.0273(5) Uani 1 1 d . . . H36 H 0.8771 0.7776 0.3225 0.033 Uiso 1 1 calc R . . C37 C 0.6652(3) 0.4624(3) 0.2955(3) 0.0631(10) Uani 1 1 d . . . H37A H 0.6206 0.4571 0.2389 0.095 Uiso 1 1 calc R . . H37B H 0.6258 0.4965 0.3367 0.095 Uiso 1 1 calc R . . H37C H 0.6722 0.3896 0.308 0.095 Uiso 1 1 calc R . . C38 C 0.9289(5) 0.5689(4) 0.4247(2) 0.102(2) Uani 1 1 d . . . H38A H 0.9406 0.4966 0.4353 0.153 Uiso 1 1 calc R . . H38B H 0.8859 0.5973 0.466 0.153 Uiso 1 1 calc R . . H38C H 1.004 0.6176 0.4296 0.153 Uiso 1 1 calc R . . C39 C 0.9297(3) 0.4846(3) 0.2190(2) 0.0525(8) Uani 1 1 d . . . H39A H 0.89 0.4779 0.1608 0.079 Uiso 1 1 calc R . . H39B H 0.9358 0.4123 0.2333 0.079 Uiso 1 1 calc R . . H39C H 1.0071 0.5293 0.225 0.079 Uiso 1 1 calc R . . C40 C 0.7194(2) 1.1371(2) 0.3093(2) 0.0403(6) Uani 1 1 d . . . H40A H 0.7079 1.1319 0.3673 0.061 Uiso 1 1 calc R . . H40B H 0.6487 1.101 0.2705 0.061 Uiso 1 1 calc R . . H40C H 0.7379 1.2137 0.3015 0.061 Uiso 1 1 calc R . . C41 C 0.8643(3) 1.0792(3) 0.17764(17) 0.0429(7) Uani 1 1 d . . . H41A H 0.9285 1.0442 0.1671 0.064 Uiso 1 1 calc R . . H41B H 0.8826 1.1556 0.1695 0.064 Uiso 1 1 calc R . . H41C H 0.7941 1.0425 0.1385 0.064 Uiso 1 1 calc R . . C42 C 0.9756(2) 1.1321(2) 0.36565(16) 0.0307(5) Uani 1 1 d . . . C43 C 0.9516(3) 1.1306(3) 0.45562(18) 0.0485(8) Uani 1 1 d . . . H43A H 0.9247 1.0556 0.4646 0.073 Uiso 1 1 calc R . . H43B H 0.8922 1.1728 0.4642 0.073 Uiso 1 1 calc R . . H43C H 1.0226 1.1625 0.4955 0.073 Uiso 1 1 calc R . . C44 C 1.0182(3) 1.2497(3) 0.3521(2) 0.0545(9) Uani 1 1 d . . . H44A H 1.033 1.251 0.2944 0.082 Uiso 1 1 calc R . . H44B H 1.0897 1.2809 0.3918 0.082 Uiso 1 1 calc R . . H44C H 0.9593 1.2922 0.3614 0.082 Uiso 1 1 calc R . . C45 C 1.0687(3) 1.0656(3) 0.3537(2) 0.0572(9) Uani 1 1 d . . . H45A H 1.0847 1.0654 0.2963 0.086 Uiso 1 1 calc R . . H45B H 1.0416 0.991 0.3635 0.086 Uiso 1 1 calc R . . H45C H 1.1395 1.0981 0.3938 0.086 Uiso 1 1 calc R . . O1 O 0.61056(16) 0.8762(2) 0.55159(11) 0.0447(5) Uani 1 1 d . . . O2 O 0.41375(17) 0.8543(2) 0.50754(11) 0.0520(6) Uani 1 1 d . . . O3 O 0.30968(14) 0.83372(16) 0.32028(10) 0.0336(4) Uani 1 1 d . . . O4 O 0.40626(14) 1.01235(14) 0.22227(11) 0.0304(4) Uani 1 1 d . . . O5 O 0.30245(15) 0.98130(15) 0.05123(11) 0.0337(4) Uani 1 1 d . . . O6 O 0.32279(17) 0.80635(16) -0.05029(11) 0.0397(5) Uani 1 1 d . . . O7 O 0.46775(15) 0.55282(14) 0.13934(11) 0.0319(4) Uani 1 1 d . . . O8 O 0.85373(16) 0.78357(14) 0.09495(12) 0.0354(4) Uani 1 1 d . . . O9 O 0.86829(16) 0.61117(15) 0.04818(12) 0.0372(4) Uani 1 1 d . . . O10 O 0.81221(13) 0.94145(13) 0.30255(10) 0.0242(3) Uani 1 1 d . . . B B 0.8046(2) 0.6763(2) 0.08493(16) 0.0252(5) Uani 1 1 d . . . Si Si 0.84072(5) 1.07023(5) 0.28746(4) 0.02345(14) Uani 1 1 d . . . Sn Sn 0.833944(18) 0.558887(15) 0.301470(11) 0.03670(8) 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 0.0207(11) 0.0273(12) 0.0206(11) 0.0000(9) 0.0020(9) 0.0068(9) C2 0.0245(12) 0.0238(11) 0.0209(11) 0.0000(9) 0.0030(9) 0.0064(9) C3 0.0228(12) 0.0329(13) 0.0243(11) -0.0005(10) 0.0003(9) 0.0085(10) C4 0.0300(13) 0.0406(14) 0.0185(11) 0.0007(10) 0.0000(9) 0.0108(11) C5 0.0340(15) 0.0640(19) 0.0211(12) 0.0072(12) 0.0042(10) 0.0108(13) C6 0.0283(13) 0.0444(15) 0.0198(11) 0.0001(10) 0.0077(9) 0.0110(11) C7 0.0217(12) 0.0359(13) 0.0235(11) -0.0001(10) 0.0026(9) 0.0086(10) C8 0.0156(11) 0.0326(12) 0.0222(11) 0.0003(9) 0.0034(8) 0.0025(9) C9 0.0170(11) 0.0304(12) 0.0248(11) 0.0013(9) 0.0031(9) 0.0028(9) C10 0.0174(11) 0.0380(14) 0.0267(12) 0.0078(10) 0.0016(9) 0.0048(10) C11 0.0229(12) 0.0411(14) 0.0192(11) 0.0032(10) -0.0005(9) -0.0002(10) C12 0.0242(12) 0.0341(13) 0.0233(12) -0.0029(10) 0.0033(9) 0.0033(10) C13 0.0184(11) 0.0296(12) 0.0224(11) 0.0020(9) 0.0045(9) 0.0015(9) C14 0.0227(12) 0.0242(12) 0.0245(11) -0.0022(9) 0.0039(9) 0.0004(9) C15 0.0219(11) 0.0220(11) 0.0237(11) 0.0023(9) 0.0020(9) 0.0043(9) C16 0.0232(12) 0.0256(11) 0.0201(11) 0.0019(9) 0.0064(9) 0.0045(9) C17 0.0210(11) 0.0255(11) 0.0201(10) 0.0020(9) 0.0014(8) 0.0053(9) C18 0.0233(13) 0.071(2) 0.0327(14) 0.0040(13) 0.0091(11) 0.0151(13) C19 0.0311(14) 0.0456(16) 0.0392(15) -0.0031(12) 0.0029(11) 0.0183(12) C20 0.0419(17) 0.0456(17) 0.0531(18) 0.0207(14) 0.0071(14) 0.0084(14) C21 0.074(2) 0.061(2) 0.0205(13) -0.0058(13) -0.0071(14) 0.0151(18) C22 0.0279(14) 0.0395(16) 0.0535(18) 0.0038(13) 0.0021(12) -0.0078(12) C23 0.0322(15) 0.0356(15) 0.0574(18) 0.0094(13) 0.0126(13) -0.0027(12) C24 0.073(3) 0.047(2) 0.085(3) 0.0131(19) 0.046(2) 0.0059(18) C25 0.121(4) 0.074(3) 0.091(3) 0.004(3) 0.071(3) 0.000(3) C26 0.088(3) 0.097(4) 0.070(3) 0.028(3) 0.037(2) -0.007(3) C27 0.065(3) 0.074(3) 0.098(3) 0.048(3) 0.028(2) 0.016(2) C28 0.054(2) 0.0476(19) 0.074(2) 0.0174(17) 0.0235(18) 0.0128(16) C29 0.0266(12) 0.0261(12) 0.0239(11) -0.0006(9) 0.0028(9) 0.0039(10) C30 0.0322(15) 0.0369(15) 0.0496(17) -0.0024(12) 0.0155(12) 0.0007(12) C31 0.0337(15) 0.0412(16) 0.0543(18) -0.0056(13) 0.0191(13) -0.0002(12) C32 0.0456(19) 0.0408(18) 0.100(3) 0.0178(18) 0.0345(19) 0.0067(15) C33 0.046(2) 0.073(2) 0.050(2) -0.0019(17) -0.0014(15) -0.0034(17) C34 0.070(3) 0.098(3) 0.044(2) -0.004(2) 0.0221(18) -0.018(2) C35 0.046(2) 0.049(2) 0.130(4) -0.011(2) 0.042(2) 0.0047(16) C36 0.0286(13) 0.0253(12) 0.0268(12) 0.0002(9) 0.0017(10) 0.0067(10) C37 0.070(2) 0.0385(18) 0.089(3) 0.0167(18) 0.029(2) 0.0132(17) C38 0.189(6) 0.066(3) 0.044(2) -0.0011(18) -0.036(3) 0.059(3) C39 0.063(2) 0.0499(19) 0.0519(19) 0.0058(15) 0.0152(16) 0.0284(17) C40 0.0322(15) 0.0399(15) 0.0555(18) 0.0123(13) 0.0130(13) 0.0166(12) C41 0.0512(18) 0.0491(17) 0.0290(14) 0.0084(12) 0.0068(12) 0.0098(14) C42 0.0271(13) 0.0296(13) 0.0307(13) -0.0024(10) 0.0002(10) 0.0012(10) C43 0.058(2) 0.0496(18) 0.0295(14) -0.0010(13) -0.0013(13) 0.0008(15) C44 0.063(2) 0.0376(17) 0.0507(19) 0.0007(14) 0.0044(16) -0.0142(15) C45 0.0254(15) 0.069(2) 0.069(2) -0.0117(18) -0.0067(14) 0.0132(15) O1 0.0318(10) 0.0857(16) 0.0179(9) 0.0049(9) 0.0036(7) 0.0175(10) O2 0.0304(10) 0.1096(19) 0.0185(9) 0.0054(10) 0.0069(7) 0.0204(11) O3 0.0196(8) 0.0587(12) 0.0225(8) 0.0003(8) 0.0039(7) 0.0104(8) O4 0.0249(9) 0.0349(10) 0.0296(9) -0.0028(7) -0.0009(7) 0.0104(7) O5 0.0272(9) 0.0429(11) 0.0327(9) 0.0120(8) 0.0013(7) 0.0106(8) O6 0.0440(11) 0.0499(12) 0.0202(9) 0.0013(8) -0.0059(8) 0.0078(9) O7 0.0277(9) 0.0278(9) 0.0351(9) -0.0033(7) 0.0054(7) -0.0031(7) O8 0.0348(10) 0.0302(10) 0.0446(11) 0.0029(8) 0.0199(8) 0.0062(8) O9 0.0315(10) 0.0328(10) 0.0464(11) -0.0055(8) 0.0177(8) 0.0013(8) O10 0.0201(8) 0.0226(8) 0.0272(8) 0.0019(6) -0.0004(6) 0.0023(6) B 0.0241(13) 0.0311(14) 0.0200(12) 0.0007(10) 0.0027(10) 0.0075(11) Si 0.0226(3) 0.0239(3) 0.0242(3) 0.0022(2) 0.0035(2) 0.0066(3) Sn 0.05276(14) 0.03073(11) 0.02807(10) 0.00191(7) 0.00102(8) 0.01833(9) #----------------------------------------------------------------------------# # 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 1.391(3) . ? C1 C7 1.419(3) . ? C1 C8 1.496(3) . ? C2 C3 1.405(3) . ? C2 C17 1.531(3) . ? C3 C4 1.364(3) . ? C3 H3 0.95 . ? C4 O1 1.378(3) . ? C4 C6 1.385(4) . ? C5 O2 1.414(3) . ? C5 O1 1.426(3) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.380(3) . ? C6 O2 1.385(3) . ? C7 O3 1.368(3) . ? C8 C13 1.403(3) . ? C8 C9 1.407(3) . ? C9 O4 1.377(3) . ? C9 C10 1.394(3) . ? C10 O5 1.381(3) . ? C10 C11 1.403(4) . ? C11 O6 1.366(3) . ? C11 C12 1.381(4) . ? C12 C13 1.392(3) . ? C12 H12 0.95 . ? C13 C14 1.530(3) . ? C14 O7 1.433(3) . ? C14 C15 1.528(3) . ? C14 H14 1 . ? C15 C29 1.334(3) . ? C15 C16 1.497(3) . ? C16 C36 1.336(3) . ? C16 C17 1.536(3) . ? C17 O10 1.425(3) . ? C17 H17 1 . ? C18 O3 1.426(3) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 O4 1.438(3) . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 O5 1.427(3) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 O6 1.427(4) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 O7 1.444(3) . ? C22 C23 1.511(4) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 C28 1.373(4) . ? C23 C24 1.378(5) . ? C24 C25 1.387(6) . ? C24 H24 0.95 . ? C25 C26 1.390(7) . ? C25 H25 0.95 . ? C26 C27 1.377(7) . ? C26 H26 0.95 . ? C27 C28 1.388(6) . ? C27 H27 0.95 . ? C28 H28 0.95 . ? C29 B 1.558(4) . ? C29 H29 0.95 . ? C30 O8 1.471(3) . ? C30 C32 1.487(4) . ? C30 C31 1.520(4) . ? C30 C33 1.541(5) . ? C31 O9 1.470(3) . ? C31 C35 1.496(5) . ? C31 C34 1.531(5) . ? 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 . ? C36 Sn 2.134(2) . ? C36 H36 0.95 . ? C37 Sn 2.144(4) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 Sn 2.129(4) . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 Sn 2.136(3) . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 Si 1.864(3) . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 Si 1.860(3) . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 C43 1.532(4) . ? C42 C45 1.533(4) . ? C42 C44 1.534(4) . ? C42 Si 1.883(3) . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C45 H45A 0.98 . ? C45 H45B 0.98 . ? C45 H45C 0.98 . ? O8 B 1.360(3) . ? O9 B 1.368(3) . ? O10 Si 1.6564(17) . ? 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 C7 120.8(2) . . ? C2 C1 C8 120.8(2) . . ? C7 C1 C8 118.4(2) . . ? C1 C2 C3 121.2(2) . . ? C1 C2 C17 121.4(2) . . ? C3 C2 C17 117.4(2) . . ? C4 C3 C2 116.7(2) . . ? C4 C3 H3 121.6 . . ? C2 C3 H3 121.6 . . ? C3 C4 O1 126.9(2) . . ? C3 C4 C6 123.3(2) . . ? O1 C4 C6 109.7(2) . . ? O2 C5 O1 109.0(2) . . ? O2 C5 H5A 109.9 . . ? O1 C5 H5A 109.9 . . ? O2 C5 H5B 109.9 . . ? O1 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C7 C6 O2 129.6(2) . . ? C7 C6 C4 120.9(2) . . ? O2 C6 C4 109.5(2) . . ? O3 C7 C6 126.4(2) . . ? O3 C7 C1 116.5(2) . . ? C6 C7 C1 117.1(2) . . ? C13 C8 C9 118.7(2) . . ? C13 C8 C1 120.8(2) . . ? C9 C8 C1 120.5(2) . . ? O4 C9 C10 121.8(2) . . ? O4 C9 C8 117.1(2) . . ? C10 C9 C8 120.9(2) . . ? O5 C10 C9 120.4(2) . . ? O5 C10 C11 120.3(2) . . ? C9 C10 C11 119.2(2) . . ? O6 C11 C12 124.5(2) . . ? O6 C11 C10 115.2(2) . . ? C12 C11 C10 120.3(2) . . ? C11 C12 C13 120.6(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 120.2(2) . . ? C12 C13 C14 118.2(2) . . ? C8 C13 C14 121.5(2) . . ? O7 C14 C15 107.61(18) . . ? O7 C14 C13 111.04(19) . . ? C15 C14 C13 108.99(19) . . ? O7 C14 H14 109.7 . . ? C15 C14 H14 109.7 . . ? C13 C14 H14 109.7 . . ? C29 C15 C16 120.9(2) . . ? C29 C15 C14 122.4(2) . . ? C16 C15 C14 116.70(19) . . ? C36 C16 C15 121.6(2) . . ? C36 C16 C17 121.0(2) . . ? C15 C16 C17 117.19(19) . . ? O10 C17 C2 109.47(18) . . ? O10 C17 C16 109.33(18) . . ? C2 C17 C16 108.96(18) . . ? O10 C17 H17 109.7 . . ? C2 C17 H17 109.7 . . ? C16 C17 H17 109.7 . . ? O3 C18 H18A 109.5 . . ? O3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C20 H20A 109.5 . . ? O5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O6 C21 H21A 109.5 . . ? O6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O7 C22 C23 113.3(2) . . ? O7 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? O7 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C28 C23 C24 118.5(3) . . ? C28 C23 C22 120.8(3) . . ? C24 C23 C22 120.7(3) . . ? C23 C24 C25 121.6(4) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C26 119.0(4) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C25 119.8(4) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 119.8(4) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C23 C28 C27 121.1(4) . . ? C23 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C15 C29 B 124.3(2) . . ? C15 C29 H29 117.8 . . ? B C29 H29 117.8 . . ? O8 C30 C32 109.6(2) . . ? O8 C30 C31 103.0(2) . . ? C32 C30 C31 117.5(3) . . ? O8 C30 C33 105.6(2) . . ? C32 C30 C33 108.4(3) . . ? C31 C30 C33 112.0(3) . . ? O9 C31 C35 110.7(3) . . ? O9 C31 C30 102.3(2) . . ? C35 C31 C30 115.6(3) . . ? O9 C31 C34 106.0(2) . . ? C35 C31 C34 108.7(3) . . ? C30 C31 C34 113.0(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 . . ? C16 C36 Sn 126.88(19) . . ? C16 C36 H36 116.6 . . ? Sn C36 H36 116.6 . . ? Sn C37 H37A 109.5 . . ? Sn C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Sn C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Sn C38 H38A 109.5 . . ? Sn C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Sn C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Sn C39 H39A 109.5 . . ? Sn C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Sn C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si C40 H40A 109.5 . . ? Si C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si C41 H41A 109.5 . . ? Si C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C45 108.5(3) . . ? C43 C42 C44 109.2(2) . . ? C45 C42 C44 109.9(3) . . ? C43 C42 Si 110.42(19) . . ? C45 C42 Si 109.15(18) . . ? C44 C42 Si 109.7(2) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C4 O1 C5 105.54(19) . . ? C6 O2 C5 105.7(2) . . ? C7 O3 C18 118.16(19) . . ? C9 O4 C19 117.67(19) . . ? C10 O5 C20 114.8(2) . . ? C11 O6 C21 116.5(2) . . ? C14 O7 C22 114.1(2) . . ? B O8 C30 106.1(2) . . ? B O9 C31 106.9(2) . . ? C17 O10 Si 122.66(14) . . ? O8 B O9 113.2(2) . . ? O8 B C29 121.8(2) . . ? O9 B C29 124.9(2) . . ? O10 Si C41 109.90(12) . . ? O10 Si C40 110.09(11) . . ? C41 Si C40 110.23(14) . . ? O10 Si C42 104.54(10) . . ? C41 Si C42 111.52(13) . . ? C40 Si C42 110.42(13) . . ? C38 Sn C36 103.80(13) . . ? C38 Sn C39 105.68(18) . . ? C36 Sn C39 117.98(11) . . ? C38 Sn C37 108.7(2) . . ? C36 Sn C37 108.35(12) . . ? C39 Sn C37 111.71(14) . . ? 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 C7 C1 C2 C3 0.6(4) . . . . ? C8 C1 C2 C3 -176.7(2) . . . . ? C7 C1 C2 C17 178.4(2) . . . . ? C8 C1 C2 C17 1.1(3) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? C17 C2 C3 C4 -177.9(2) . . . . ? C2 C3 C4 O1 -179.1(2) . . . . ? C2 C3 C4 C6 -0.4(4) . . . . ? C3 C4 C6 C7 0.2(4) . . . . ? O1 C4 C6 C7 179.0(2) . . . . ? C3 C4 C6 O2 -179.2(3) . . . . ? O1 C4 C6 O2 -0.3(3) . . . . ? O2 C6 C7 O3 -2.0(5) . . . . ? C4 C6 C7 O3 178.8(3) . . . . ? O2 C6 C7 C1 179.6(3) . . . . ? C4 C6 C7 C1 0.5(4) . . . . ? C2 C1 C7 O3 -179.3(2) . . . . ? C8 C1 C7 O3 -2.0(3) . . . . ? C2 C1 C7 C6 -0.8(4) . . . . ? C8 C1 C7 C6 176.6(2) . . . . ? C2 C1 C8 C13 65.5(3) . . . . ? C7 C1 C8 C13 -111.8(3) . . . . ? C2 C1 C8 C9 -113.5(3) . . . . ? C7 C1 C8 C9 69.2(3) . . . . ? C13 C8 C9 O4 -174.3(2) . . . . ? C1 C8 C9 O4 4.8(3) . . . . ? C13 C8 C9 C10 1.3(3) . . . . ? C1 C8 C9 C10 -179.7(2) . . . . ? O4 C9 C10 O5 -8.2(3) . . . . ? C8 C9 C10 O5 176.4(2) . . . . ? O4 C9 C10 C11 174.1(2) . . . . ? C8 C9 C10 C11 -1.3(3) . . . . ? O5 C10 C11 O6 2.6(3) . . . . ? C9 C10 C11 O6 -179.7(2) . . . . ? O5 C10 C11 C12 -177.9(2) . . . . ? C9 C10 C11 C12 -0.2(4) . . . . ? O6 C11 C12 C13 -178.9(2) . . . . ? C10 C11 C12 C13 1.6(4) . . . . ? C11 C12 C13 C8 -1.5(4) . . . . ? C11 C12 C13 C14 179.3(2) . . . . ? C9 C8 C13 C12 0.1(3) . . . . ? C1 C8 C13 C12 -178.9(2) . . . . ? C9 C8 C13 C14 179.3(2) . . . . ? C1 C8 C13 C14 0.2(3) . . . . ? C12 C13 C14 O7 -33.1(3) . . . . ? C8 C13 C14 O7 147.7(2) . . . . ? C12 C13 C14 C15 85.3(2) . . . . ? C8 C13 C14 C15 -93.9(2) . . . . ? O7 C14 C15 C29 27.7(3) . . . . ? C13 C14 C15 C29 -92.8(3) . . . . ? O7 C14 C15 C16 -154.28(19) . . . . ? C13 C14 C15 C16 85.2(2) . . . . ? C29 C15 C16 C36 -63.5(3) . . . . ? C14 C15 C16 C36 118.5(2) . . . . ? C29 C15 C16 C17 120.6(2) . . . . ? C14 C15 C16 C17 -57.5(3) . . . . ? C1 C2 C17 O10 146.3(2) . . . . ? C3 C2 C17 O10 -35.8(3) . . . . ? C1 C2 C17 C16 -94.1(2) . . . . ? C3 C2 C17 C16 83.7(2) . . . . ? C36 C16 C17 O10 28.6(3) . . . . ? C15 C16 C17 O10 -155.38(18) . . . . ? C36 C16 C17 C2 -91.0(3) . . . . ? C15 C16 C17 C2 85.0(2) . . . . ? O7 C22 C23 C28 -82.5(4) . . . . ? O7 C22 C23 C24 98.1(4) . . . . ? C28 C23 C24 C25 2.4(6) . . . . ? C22 C23 C24 C25 -178.2(4) . . . . ? C23 C24 C25 C26 -0.5(7) . . . . ? C24 C25 C26 C27 -2.6(8) . . . . ? C25 C26 C27 C28 3.8(7) . . . . ? C24 C23 C28 C27 -1.3(5) . . . . ? C22 C23 C28 C27 179.3(3) . . . . ? C26 C27 C28 C23 -1.8(6) . . . . ? C16 C15 C29 B -13.5(4) . . . . ? C14 C15 C29 B 164.5(2) . . . . ? O8 C30 C31 O9 -28.5(3) . . . . ? C32 C30 C31 O9 -149.1(3) . . . . ? C33 C30 C31 O9 84.5(3) . . . . ? O8 C30 C31 C35 -148.9(3) . . . . ? C32 C30 C31 C35 90.5(4) . . . . ? C33 C30 C31 C35 -35.9(4) . . . . ? O8 C30 C31 C34 85.0(3) . . . . ? C32 C30 C31 C34 -35.6(4) . . . . ? C33 C30 C31 C34 -162.0(3) . . . . ? C15 C16 C36 Sn -16.6(3) . . . . ? C17 C16 C36 Sn 159.25(17) . . . . ? C3 C4 O1 C5 -176.6(3) . . . . ? C6 C4 O1 C5 4.6(3) . . . . ? O2 C5 O1 C4 -7.3(3) . . . . ? C7 C6 O2 C5 176.6(3) . . . . ? C4 C6 O2 C5 -4.2(3) . . . . ? O1 C5 O2 C6 7.1(3) . . . . ? C6 C7 O3 C18 8.3(4) . . . . ? C1 C7 O3 C18 -173.3(2) . . . . ? C10 C9 O4 C19 56.9(3) . . . . ? C8 C9 O4 C19 -127.6(2) . . . . ? C9 C10 O5 C20 95.8(3) . . . . ? C11 C10 O5 C20 -86.5(3) . . . . ? C12 C11 O6 C21 -0.9(4) . . . . ? C10 C11 O6 C21 178.6(3) . . . . ? C15 C14 O7 C22 174.5(2) . . . . ? C13 C14 O7 C22 -66.3(3) . . . . ? C23 C22 O7 C14 -69.0(3) . . . . ? C32 C30 O8 B 151.3(3) . . . . ? C31 C30 O8 B 25.5(3) . . . . ? C33 C30 O8 B -92.1(3) . . . . ? C35 C31 O9 B 145.8(3) . . . . ? C30 C31 O9 B 22.1(3) . . . . ? C34 C31 O9 B -96.5(3) . . . . ? C2 C17 O10 Si -94.27(19) . . . . ? C16 C17 O10 Si 146.44(15) . . . . ? C30 O8 B O9 -12.6(3) . . . . ? C30 O8 B C29 171.0(2) . . . . ? C31 O9 B O8 -6.7(3) . . . . ? C31 O9 B C29 169.7(2) . . . . ? C15 C29 B O8 -39.0(4) . . . . ? C15 C29 B O9 145.0(3) . . . . ? C17 O10 Si C41 -70.0(2) . . . . ? C17 O10 Si C40 51.6(2) . . . . ? C17 O10 Si C42 170.21(17) . . . . ? C43 C42 Si O10 -65.2(2) . . . . ? C45 C42 Si O10 54.0(2) . . . . ? C44 C42 Si O10 174.4(2) . . . . ? C43 C42 Si C41 176.1(2) . . . . ? C45 C42 Si C41 -64.7(2) . . . . ? C44 C42 Si C41 55.7(2) . . . . ? C43 C42 Si C40 53.2(2) . . . . ? C45 C42 Si C40 172.4(2) . . . . ? C44 C42 Si C40 -67.2(2) . . . . ? C16 C36 Sn C38 -150.2(3) . . . . ? C16 C36 Sn C39 93.4(2) . . . . ? C16 C36 Sn C37 -34.8(3) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 911248' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_RajanBabu1913 #TrackingRef '18992_web_deposit_cif_file_2_RajanBabu.T.V_1364518612.archive_38.cif' _audit_creation_date 2012-10-05T10:55:27-00:00 _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 1913' _chemical_formula_moiety 'C29 H40 O9 Si1' _chemical_formula_sum 'C29 H40 O9 Si' _chemical_formula_weight 560.7 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system orthorhombic _space_group_name_H-M_alt P212121 _space_group_name_Hall 'P 2ac 2ab' _space_group_IT_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 10.7843(1) _cell_length_b 14.0454(2) _cell_length_c 19.3783(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2935.23(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3790 _cell_measurement_theta_min 1.018 _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 0.35 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _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 4.1, which means that 90% of these reflections were measured at least 4.1 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 0.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.981 _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 Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.784799E-1 _diffrn_orient_matrix_ub_12 0.120185E-1 _diffrn_orient_matrix_ub_13 -0.260688E-1 _diffrn_orient_matrix_ub_21 -0.402897E-1 _diffrn_orient_matrix_ub_22 -0.23478E-1 _diffrn_orient_matrix_ub_23 -0.432513E-1 _diffrn_orient_matrix_ub_31 -0.28566E-1 _diffrn_orient_matrix_ub_32 0.661321E-1 _diffrn_orient_matrix_ub_33 -0.106174E-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 0.039 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 50819 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 6718 _reflns_number_gt 5822 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _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 correct enantiomer was chosen based on the known chiral centers in the molecule. The final values of the Flack parameter and Hooft y parameter, -0.08(10) and -0.02(3), respectively, also indicate that this is the correct enantiomer. 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 torsion angle, which defines the orientation of the methyl group about the C-C, C-Si or C-O bond, was refined. The hydrogen atom bonded to O(5) 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 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^ > 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^)+(0.0359P)^2^+0.6975P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6718 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 -0.08(10) _refine_diff_density_max 0.203 _refine_diff_density_min -0.19 _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' 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 0.37364(14) 0.30594(12) 0.17031(8) 0.0228(3) Uani 1 1 d . . . C2 C 0.32079(15) 0.21753(12) 0.18542(8) 0.0228(3) Uani 1 1 d . . . C3 C 0.24790(15) 0.17078(12) 0.13612(8) 0.0236(3) Uani 1 1 d . . . C4 C 0.22445(15) 0.21227(11) 0.07267(8) 0.0229(3) Uani 1 1 d . . . H4 H 0.1739 0.1809 0.0396 0.027 Uiso 1 1 calc R . . C5 C 0.27638(14) 0.30091(11) 0.05829(8) 0.0212(3) Uani 1 1 d . . . C6 C 0.24916(15) 0.34827(11) -0.00963(8) 0.0221(3) Uani 1 1 d . . . C7 C 0.12145(14) 0.39737(12) -0.01823(8) 0.0242(3) Uani 1 1 d . . . C8 C 0.13546(14) 0.50486(12) 0.00028(8) 0.0232(3) Uani 1 1 d . . . H8 H 0.1954 0.5336 -0.0331 0.028 Uiso 1 1 calc R . . C9 C 0.19057(14) 0.51722(12) 0.07457(8) 0.0223(3) Uani 1 1 d . . . H9 H 0.1642 0.4622 0.1038 0.027 Uiso 1 1 calc R . . C10 C 0.33151(14) 0.52167(12) 0.07303(8) 0.0221(3) Uani 1 1 d . . . C11 C 0.38462(15) 0.60978(12) 0.05534(9) 0.0262(3) Uani 1 1 d . . . H11 H 0.3346 0.6641 0.0463 0.031 Uiso 1 1 calc R . . C12 C 0.51071(16) 0.61415(12) 0.05167(9) 0.0259(4) Uani 1 1 d . . . C13 C 0.58635(15) 0.53588(12) 0.06307(8) 0.0233(3) Uani 1 1 d . . . C14 C 0.53670(14) 0.44890(11) 0.07959(8) 0.0212(3) Uani 1 1 d . . . C15 C 0.40566(15) 0.44252(11) 0.08660(8) 0.0199(3) Uani 1 1 d . . . C16 C 0.35171(14) 0.34823(11) 0.10535(8) 0.0207(3) Uani 1 1 d . . . C17 C 0.70687(19) 0.66036(15) 0.04095(16) 0.0572(7) Uani 1 1 d . . . H17A H 0.748 0.6934 0.0798 0.069 Uiso 1 1 calc R . . H17B H 0.7527 0.6758 -0.0019 0.069 Uiso 1 1 calc R . . C18 C 0.4263(2) 0.35476(15) 0.28652(9) 0.0418(5) Uani 1 1 d . . . H18A H 0.3366 0.3508 0.2944 0.063 Uiso 1 1 calc R . . H18B H 0.4583 0.4138 0.3067 0.063 Uiso 1 1 calc R . . H18C H 0.4672 0.3001 0.3081 0.063 Uiso 1 1 calc R . . C19 C 0.4255(2) 0.10320(17) 0.25272(10) 0.0534(6) Uani 1 1 d . . . H19A H 0.4 0.0514 0.222 0.08 Uiso 1 1 calc R . . H19B H 0.432 0.0791 0.3001 0.08 Uiso 1 1 calc R . . H19C H 0.5061 0.128 0.2379 0.08 Uiso 1 1 calc R . . C20 C 0.1216(2) 0.03739(15) 0.10790(11) 0.0465(5) Uani 1 1 d . . . H20A H 0.0492 0.0778 0.0991 0.07 Uiso 1 1 calc R . . H20B H 0.0944 -0.0236 0.1273 0.07 Uiso 1 1 calc R . . H20C H 0.166 0.0261 0.0645 0.07 Uiso 1 1 calc R . . C21 C 0.07697(17) 0.38320(13) -0.09178(9) 0.0322(4) Uani 1 1 d . . . H21A H 0.0725 0.3149 -0.102 0.048 Uiso 1 1 calc R . . H21B H 0.1351 0.4138 -0.1237 0.048 Uiso 1 1 calc R . . H21C H -0.0054 0.4117 -0.0972 0.048 Uiso 1 1 calc R . . C22 C 0.01126(16) 0.55713(14) -0.00785(10) 0.0329(4) Uani 1 1 d . . . H22A H -0.0166 0.5525 -0.0559 0.049 Uiso 1 1 calc R . . H22B H 0.0218 0.6243 0.0046 0.049 Uiso 1 1 calc R . . H22C H -0.0507 0.528 0.0225 0.049 Uiso 1 1 calc R . . C23 C 0.20043(19) 0.54460(15) 0.24392(10) 0.0400(5) Uani 1 1 d . . . H23A H 0.203 0.4765 0.2329 0.06 Uiso 1 1 calc R . . H23B H 0.1727 0.553 0.2917 0.06 Uiso 1 1 calc R . . H23C H 0.2834 0.572 0.2384 0.06 Uiso 1 1 calc R . . C24 C -0.06026(16) 0.54176(13) 0.18684(10) 0.0310(4) Uani 1 1 d . . . H24A H -0.1194 0.5735 0.1561 0.046 Uiso 1 1 calc R . . H24B H -0.0928 0.542 0.2341 0.046 Uiso 1 1 calc R . . H24C H -0.0481 0.4759 0.1716 0.046 Uiso 1 1 calc R . . C25 C 0.07391(17) 0.73571(13) 0.20562(9) 0.0299(4) Uani 1 1 d . . . C26 C 0.19905(19) 0.78676(15) 0.19720(11) 0.0414(5) Uani 1 1 d . . . H26A H 0.2252 0.7836 0.1488 0.062 Uiso 1 1 calc R . . H26B H 0.2614 0.7557 0.2263 0.062 Uiso 1 1 calc R . . H26C H 0.1904 0.8535 0.2111 0.062 Uiso 1 1 calc R . . C27 C 0.0297(2) 0.74555(15) 0.28088(11) 0.0430(5) Uani 1 1 d . . . H27A H 0.0919 0.7181 0.3119 0.065 Uiso 1 1 calc R . . H27B H -0.0492 0.7118 0.2867 0.065 Uiso 1 1 calc R . . H27C H 0.0181 0.813 0.292 0.065 Uiso 1 1 calc R . . C28 C -0.0220(2) 0.78228(14) 0.15767(12) 0.0439(5) Uani 1 1 d . . . H28A H -0.0311 0.8497 0.1698 0.066 Uiso 1 1 calc R . . H28B H -0.1021 0.7501 0.1629 0.066 Uiso 1 1 calc R . . H28C H 0.0059 0.7768 0.1097 0.066 Uiso 1 1 calc R . . C29 C 0.72199(16) 0.37282(14) 0.11915(10) 0.0341(4) Uani 1 1 d . . . H29A H 0.7815 0.4033 0.0879 0.051 Uiso 1 1 calc R . . H29B H 0.7514 0.3089 0.131 0.051 Uiso 1 1 calc R . . H29C H 0.714 0.4109 0.1613 0.051 Uiso 1 1 calc R . . O1 O 0.45052(11) 0.35421(9) 0.21393(6) 0.0315(3) Uani 1 1 d . . . O2 O 0.33592(11) 0.17725(8) 0.25023(6) 0.0277(3) Uani 1 1 d . . . O3 O 0.20252(12) 0.08403(8) 0.15583(6) 0.0312(3) Uani 1 1 d . . . O4 O 0.32500(11) 0.34965(9) -0.05583(6) 0.0302(3) Uani 1 1 d . . . O5 O 0.03422(11) 0.35965(10) 0.03029(7) 0.0308(3) Uani 1 1 d . . . H1O5 H 0.011(3) 0.3077(19) 0.0133(13) 0.067(9) Uiso 1 1 d . . . O6 O 0.14630(10) 0.60358(8) 0.10486(6) 0.0253(2) Uani 1 1 d . . . O7 O 0.58335(12) 0.69188(9) 0.03518(8) 0.0386(3) Uani 1 1 d . . . O8 O 0.70931(11) 0.56080(9) 0.05228(7) 0.0316(3) Uani 1 1 d . . . O9 O 0.60304(10) 0.36607(8) 0.08564(6) 0.0251(3) Uani 1 1 d . . . Si Si 0.09036(4) 0.60587(3) 0.18454(2) 0.02363(10) 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 0.0207(8) 0.0245(9) 0.0233(8) -0.0027(7) 0.0004(6) 0.0017(6) C2 0.0231(8) 0.0243(8) 0.0209(7) 0.0026(7) 0.0043(7) 0.0021(6) C3 0.0239(8) 0.0200(8) 0.0269(8) 0.0012(6) 0.0046(7) 0.0001(7) C4 0.0229(8) 0.0211(8) 0.0247(8) -0.0025(6) -0.0008(7) -0.0010(6) C5 0.0191(8) 0.0232(8) 0.0213(8) -0.0010(6) 0.0015(6) 0.0019(6) C6 0.0254(8) 0.0184(8) 0.0223(8) -0.0031(6) -0.0005(7) -0.0034(7) C7 0.0226(8) 0.0261(8) 0.0238(8) 0.0024(7) -0.0015(6) -0.0020(7) C8 0.0211(8) 0.0241(8) 0.0245(8) 0.0030(7) -0.0005(6) 0.0010(7) C9 0.0213(8) 0.0222(8) 0.0234(8) -0.0008(6) 0.0023(6) 0.0024(6) C10 0.0202(8) 0.0251(8) 0.0211(8) -0.0007(7) 0.0007(6) -0.0009(6) C11 0.0251(8) 0.0225(8) 0.0309(8) 0.0031(7) -0.0007(7) 0.0021(7) C12 0.0293(9) 0.0217(8) 0.0267(8) 0.0045(7) -0.0014(7) -0.0041(7) C13 0.0193(7) 0.0289(9) 0.0217(8) 0.0008(7) -0.0009(7) -0.0034(7) C14 0.0209(7) 0.0222(8) 0.0204(8) -0.0015(6) -0.0011(6) 0.0012(6) C15 0.0217(7) 0.0219(8) 0.0160(7) -0.0010(6) -0.0020(6) -0.0015(7) C16 0.0184(7) 0.0211(8) 0.0227(8) -0.0002(6) 0.0022(6) 0.0011(6) C17 0.0284(10) 0.0338(12) 0.109(2) 0.0158(13) -0.0043(12) -0.0078(9) C18 0.0614(13) 0.0391(11) 0.0249(9) -0.0007(8) -0.0073(9) -0.0098(10) C19 0.0728(15) 0.0575(14) 0.0299(10) 0.0129(10) -0.0007(10) 0.0330(13) C20 0.0651(15) 0.0318(11) 0.0425(11) 0.0036(9) -0.0084(10) -0.0227(10) C21 0.0358(9) 0.0312(9) 0.0297(9) -0.0014(7) -0.0107(7) 0.0011(8) C22 0.0300(9) 0.0333(10) 0.0355(10) -0.0004(8) -0.0075(8) 0.0054(8) C23 0.0378(10) 0.0480(12) 0.0344(11) 0.0025(9) -0.0072(9) 0.0055(9) C24 0.0313(9) 0.0292(9) 0.0324(9) -0.0026(8) 0.0030(8) -0.0036(7) C25 0.0291(9) 0.0269(9) 0.0337(9) -0.0072(7) 0.0047(8) -0.0034(7) C26 0.0381(11) 0.0374(11) 0.0486(12) -0.0095(9) 0.0086(9) -0.0132(9) C27 0.0441(12) 0.0387(11) 0.0462(12) -0.0166(9) 0.0131(10) -0.0116(9) C28 0.0471(12) 0.0267(10) 0.0579(13) -0.0023(9) -0.0022(11) 0.0048(9) C29 0.0244(9) 0.0337(10) 0.0441(11) -0.0023(8) -0.0121(8) 0.0038(8) O1 0.0346(7) 0.0373(7) 0.0226(6) 0.0019(5) -0.0058(5) -0.0101(6) O2 0.0350(6) 0.0272(6) 0.0209(6) 0.0045(5) 0.0028(5) 0.0016(5) O3 0.0399(7) 0.0237(6) 0.0299(6) 0.0035(5) 0.0006(5) -0.0080(5) O4 0.0294(6) 0.0364(7) 0.0249(6) -0.0008(5) 0.0043(5) -0.0015(5) O5 0.0239(6) 0.0307(7) 0.0378(7) 0.0058(6) 0.0026(5) -0.0049(5) O6 0.0251(6) 0.0224(6) 0.0283(6) -0.0021(5) 0.0020(5) 0.0036(5) O7 0.0281(6) 0.0279(7) 0.0598(9) 0.0130(6) -0.0031(6) -0.0081(6) O8 0.0216(6) 0.0303(7) 0.0430(7) 0.0072(6) 0.0002(5) -0.0054(5) O9 0.0185(5) 0.0239(6) 0.0329(6) -0.0020(5) -0.0043(5) 0.0015(5) Si 0.0218(2) 0.0244(2) 0.0246(2) -0.00269(18) -0.00084(18) -0.00013(19) #----------------------------------------------------------------------------# # 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 O1 1.3644(19) . ? C1 C2 1.397(2) . ? C1 C16 1.412(2) . ? C2 O2 1.3872(19) . ? C2 C3 1.401(2) . ? C3 O3 1.3675(19) . ? C3 C4 1.384(2) . ? C4 C5 1.393(2) . ? C4 H4 0.95 . ? C5 C16 1.391(2) . ? C5 C6 1.504(2) . ? C6 O4 1.2128(19) . ? C6 C7 1.549(2) . ? C7 O5 1.432(2) . ? C7 C21 1.517(2) . ? C7 C8 1.559(2) . ? C8 C22 1.535(2) . ? C8 C9 1.567(2) . ? C8 H8 1 . ? C9 O6 1.4296(19) . ? C9 C10 1.522(2) . ? C9 H9 1 . ? C10 C15 1.394(2) . ? C10 C11 1.406(2) . ? C11 C12 1.363(2) . ? C11 H11 0.95 . ? C12 O7 1.381(2) . ? C12 C13 1.387(2) . ? C13 C14 1.372(2) . ? C13 O8 1.387(2) . ? C14 O9 1.3708(19) . ? C14 C15 1.422(2) . ? C15 C16 1.491(2) . ? C17 O7 1.408(2) . ? C17 O8 1.416(2) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 O1 1.431(2) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 O2 1.420(2) . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 O3 1.433(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 Si 1.8639(19) . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 Si 1.8578(18) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C28 1.537(3) . ? C25 C26 1.537(3) . ? C25 C27 1.541(3) . ? C25 Si 1.8773(18) . ? 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 . ? C29 O9 1.4409(19) . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? O5 H1O5 0.84(3) . ? O6 Si 1.6580(12) . ? 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 O1 C1 C2 124.03(15) . . ? O1 C1 C16 116.43(14) . . ? C2 C1 C16 119.50(15) . . ? O2 C2 C1 120.28(15) . . ? O2 C2 C3 119.50(14) . . ? C1 C2 C3 120.18(15) . . ? O3 C3 C4 123.91(15) . . ? O3 C3 C2 115.35(14) . . ? C4 C3 C2 120.74(15) . . ? C3 C4 C5 118.72(15) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C16 C5 C4 122.06(15) . . ? C16 C5 C6 118.47(14) . . ? C4 C5 C6 119.46(14) . . ? O4 C6 C5 121.43(14) . . ? O4 C6 C7 120.86(14) . . ? C5 C6 C7 117.69(13) . . ? O5 C7 C21 111.14(14) . . ? O5 C7 C6 110.41(13) . . ? C21 C7 C6 108.89(14) . . ? O5 C7 C8 105.72(13) . . ? C21 C7 C8 111.95(14) . . ? C6 C7 C8 108.67(12) . . ? C22 C8 C7 110.79(13) . . ? C22 C8 C9 111.84(13) . . ? C7 C8 C9 110.81(13) . . ? C22 C8 H8 107.7 . . ? C7 C8 H8 107.7 . . ? C9 C8 H8 107.7 . . ? O6 C9 C10 107.87(13) . . ? O6 C9 C8 110.15(13) . . ? C10 C9 C8 111.43(13) . . ? O6 C9 H9 109.1 . . ? C10 C9 H9 109.1 . . ? C8 C9 H9 109.1 . . ? C15 C10 C11 120.94(14) . . ? C15 C10 C9 122.44(15) . . ? C11 C10 C9 116.60(14) . . ? C12 C11 C10 117.30(16) . . ? C12 C11 H11 121.3 . . ? C10 C11 H11 121.3 . . ? C11 C12 O7 127.84(16) . . ? C11 C12 C13 122.87(16) . . ? O7 C12 C13 109.26(14) . . ? C14 C13 C12 120.91(15) . . ? C14 C13 O8 129.27(15) . . ? C12 C13 O8 109.77(14) . . ? O9 C14 C13 124.89(14) . . ? O9 C14 C15 117.19(14) . . ? C13 C14 C15 117.79(15) . . ? C10 C15 C14 120.10(14) . . ? C10 C15 C16 122.01(14) . . ? C14 C15 C16 117.82(14) . . ? C5 C16 C1 118.79(15) . . ? C5 C16 C15 119.51(14) . . ? C1 C16 C15 121.70(14) . . ? O7 C17 O8 109.90(16) . . ? O7 C17 H17A 109.7 . . ? O8 C17 H17A 109.7 . . ? O7 C17 H17B 109.7 . . ? O8 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? O1 C18 H18A 109.5 . . ? O1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O2 C19 H19A 109.5 . . ? O2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 H20A 109.5 . . ? O3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C7 C21 H21A 109.5 . . ? C7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C8 C22 H22A 109.5 . . ? C8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si C23 H23A 109.5 . . ? Si C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si C24 H24A 109.5 . . ? Si C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C26 109.17(17) . . ? C28 C25 C27 109.01(17) . . ? C26 C25 C27 109.31(15) . . ? C28 C25 Si 110.21(13) . . ? C26 C25 Si 110.31(13) . . ? C27 C25 Si 108.81(13) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O9 C29 H29A 109.5 . . ? O9 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O9 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C1 O1 C18 120.04(14) . . ? C2 O2 C19 114.18(13) . . ? C3 O3 C20 116.37(14) . . ? C7 O5 H1O5 105.0(19) . . ? C9 O6 Si 121.35(10) . . ? C12 O7 C17 105.65(14) . . ? C13 O8 C17 104.76(14) . . ? C14 O9 C29 116.58(13) . . ? O6 Si C24 109.34(7) . . ? O6 Si C23 109.53(8) . . ? C24 Si C23 108.55(9) . . ? O6 Si C25 104.83(7) . . ? C24 Si C25 112.52(8) . . ? C23 Si C25 111.98(9) . . ? 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 O1 C1 C2 O2 5.9(2) . . . . ? C16 C1 C2 O2 -176.59(14) . . . . ? O1 C1 C2 C3 -176.73(15) . . . . ? C16 C1 C2 C3 0.8(2) . . . . ? O2 C2 C3 O3 -3.7(2) . . . . ? C1 C2 C3 O3 178.92(14) . . . . ? O2 C2 C3 C4 175.69(14) . . . . ? C1 C2 C3 C4 -1.7(2) . . . . ? O3 C3 C4 C5 -179.69(15) . . . . ? C2 C3 C4 C5 1.0(2) . . . . ? C3 C4 C5 C16 0.6(2) . . . . ? C3 C4 C5 C6 -178.37(14) . . . . ? C16 C5 C6 O4 77.2(2) . . . . ? C4 C5 C6 O4 -103.74(19) . . . . ? C16 C5 C6 C7 -101.53(17) . . . . ? C4 C5 C6 C7 77.51(18) . . . . ? O4 C6 C7 O5 159.78(15) . . . . ? C5 C6 C7 O5 -21.47(19) . . . . ? O4 C6 C7 C21 37.5(2) . . . . ? C5 C6 C7 C21 -143.75(14) . . . . ? O4 C6 C7 C8 -84.69(18) . . . . ? C5 C6 C7 C8 94.06(16) . . . . ? O5 C7 C8 C22 -61.81(16) . . . . ? C21 C7 C8 C22 59.35(18) . . . . ? C6 C7 C8 C22 179.66(13) . . . . ? O5 C7 C8 C9 62.94(15) . . . . ? C21 C7 C8 C9 -175.90(13) . . . . ? C6 C7 C8 C9 -55.59(16) . . . . ? C22 C8 C9 O6 -26.02(18) . . . . ? C7 C8 C9 O6 -150.17(13) . . . . ? C22 C8 C9 C10 -145.70(14) . . . . ? C7 C8 C9 C10 90.15(16) . . . . ? O6 C9 C10 C15 141.19(15) . . . . ? C8 C9 C10 C15 -97.79(18) . . . . ? O6 C9 C10 C11 -40.40(19) . . . . ? C8 C9 C10 C11 80.62(18) . . . . ? C15 C10 C11 C12 0.4(2) . . . . ? C9 C10 C11 C12 -178.05(15) . . . . ? C10 C11 C12 O7 179.70(16) . . . . ? C10 C11 C12 C13 1.4(3) . . . . ? C11 C12 C13 C14 -0.7(3) . . . . ? O7 C12 C13 C14 -179.25(15) . . . . ? C11 C12 C13 O8 176.90(16) . . . . ? O7 C12 C13 O8 -1.65(19) . . . . ? C12 C13 C14 O9 173.85(15) . . . . ? O8 C13 C14 O9 -3.2(3) . . . . ? C12 C13 C14 C15 -1.8(2) . . . . ? O8 C13 C14 C15 -178.89(15) . . . . ? C11 C10 C15 C14 -2.9(2) . . . . ? C9 C10 C15 C14 175.46(14) . . . . ? C11 C10 C15 C16 -179.89(14) . . . . ? C9 C10 C15 C16 -1.5(2) . . . . ? O9 C14 C15 C10 -172.45(14) . . . . ? C13 C14 C15 C10 3.5(2) . . . . ? O9 C14 C15 C16 4.7(2) . . . . ? C13 C14 C15 C16 -179.32(14) . . . . ? C4 C5 C16 C1 -1.5(2) . . . . ? C6 C5 C16 C1 177.49(14) . . . . ? C4 C5 C16 C15 179.34(14) . . . . ? C6 C5 C16 C15 -1.6(2) . . . . ? O1 C1 C16 C5 178.50(14) . . . . ? C2 C1 C16 C5 0.8(2) . . . . ? O1 C1 C16 C15 -2.4(2) . . . . ? C2 C1 C16 C15 179.90(14) . . . . ? C10 C15 C16 C5 62.7(2) . . . . ? C14 C15 C16 C5 -114.40(17) . . . . ? C10 C15 C16 C1 -116.43(18) . . . . ? C14 C15 C16 C1 66.5(2) . . . . ? C2 C1 O1 C18 -39.2(2) . . . . ? C16 C1 O1 C18 143.21(16) . . . . ? C1 C2 O2 C19 -102.78(19) . . . . ? C3 C2 O2 C19 79.8(2) . . . . ? C4 C3 O3 C20 -3.0(2) . . . . ? C2 C3 O3 C20 176.39(16) . . . . ? C10 C9 O6 Si -105.80(13) . . . . ? C8 C9 O6 Si 132.38(11) . . . . ? C11 C12 O7 C17 178.0(2) . . . . ? C13 C12 O7 C17 -3.5(2) . . . . ? O8 C17 O7 C12 7.4(3) . . . . ? C14 C13 O8 C17 -176.6(2) . . . . ? C12 C13 O8 C17 6.0(2) . . . . ? O7 C17 O8 C13 -8.3(3) . . . . ? C13 C14 O9 C29 40.6(2) . . . . ? C15 C14 O9 C29 -143.70(15) . . . . ? C9 O6 Si C24 -69.54(13) . . . . ? C9 O6 Si C23 49.29(14) . . . . ? C9 O6 Si C25 169.61(12) . . . . ? C28 C25 Si O6 63.95(14) . . . . ? C26 C25 Si O6 -56.67(14) . . . . ? C27 C25 Si O6 -176.57(13) . . . . ? C28 C25 Si C24 -54.77(15) . . . . ? C26 C25 Si C24 -175.39(13) . . . . ? C27 C25 Si C24 64.71(16) . . . . ? C28 C25 Si C23 -177.37(14) . . . . ? C26 C25 Si C23 62.01(16) . . . . ? C27 C25 Si C23 -57.89(16) . . . . ? # END of CIF _database_code_depnum_ccdc_archive 'CCDC 911249'