# Electronic Supplementary Material (ESI) for Chemical Communications # 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_global _ccdc_journal_depnumber ? #------------------------------------------------------------------------- #4 Chemical and physical data # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag include any ASCII file output by a chemical drawing # package # Against _type record, for example, ChemDraw # Against _records supply the chemical connectivity records _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H42 Si' _chemical_formula_weight 634.90 _chemical_melting_point ? _ccdc_compound_id ? _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ? _exptl_crystal_density_diffrn ? _exptl_crystal_colour red #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _diffrn_radiation_type Cu _diffrn_measurement_device 'Agilent SuperNova' _ccdc_temp_data_collection 173(2) _ccdc_ls_R_squared ? _refine_ls_abs_structure_details ? _ccdc_disorder ? _ccdc_comments ? #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # Do not include structure factors data_aw22 _audit_creation_date 2011-10-14 _audit_creation_method ; Olex2 1.1 (compiled 2011.09.07 svn.r1971, GUI svn.r3853) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C47 H42 Si' _chemical_formula_sum 'C47 H42 Si' _chemical_formula_weight 634.90 _chemical_melting_point ? _chemical_oxdiff_formula 'C47 H42 Si' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 7.6889(3) _cell_length_b 31.5880(11) _cell_length_c 14.4774(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.378(4) _cell_angle_gamma 90.00 _cell_volume 3515.2(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3757 _cell_measurement_temperature 173.0 _cell_measurement_theta_max 73.3931 _cell_measurement_theta_min 3.3561 _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_correction_T_min 0.943 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'clear dark red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1352 _exptl_crystal_recrystallization_method 'crystallized from DCM/MeOH' _exptl_crystal_size_max 0.4432 _exptl_crystal_size_mid 0.1659 _exptl_crystal_size_min 0.1525 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_unetI/netI 0.0405 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 12209 _diffrn_reflns_theta_full 73.55 _diffrn_reflns_theta_max 73.55 _diffrn_reflns_theta_min 3.36 _diffrn_ambient_temperature 173.0 _diffrn_detector_area_resol_mean 10.6144 _diffrn_measured_fraction_theta_full 0.949 _diffrn_measured_fraction_theta_max 0.949 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -100.00 -9.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -40.9105 -77.0000 150.0000 91 #__ type_ start__ end____ width___ exp.time_ 2 omega -67.00 27.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -40.9105 77.0000 -90.0000 94 #__ type_ start__ end____ width___ exp.time_ 3 omega 87.00 167.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 107.9009 45.0000 -30.0000 80 #__ type_ start__ end____ width___ exp.time_ 4 omega 99.00 178.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 107.9009 125.0000 -120.0000 79 #__ type_ start__ end____ width___ exp.time_ 5 omega 48.00 98.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 107.9009 -45.0000 120.0000 50 #__ type_ start__ end____ width___ exp.time_ 6 omega 74.00 146.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 107.9009 77.0000 0.0000 72 #__ type_ start__ end____ width___ exp.time_ 7 omega 77.00 136.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 107.9009 -153.0000 -62.0000 59 #__ type_ start__ end____ width___ exp.time_ 8 omega 109.00 178.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 107.9009 125.0000 60.0000 69 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.1301977000 _diffrn_orient_matrix_UB_12 -0.0357464000 _diffrn_orient_matrix_UB_13 0.0230397000 _diffrn_orient_matrix_UB_21 -0.1289000000 _diffrn_orient_matrix_UB_22 -0.0327527000 _diffrn_orient_matrix_UB_23 -0.0410051000 _diffrn_orient_matrix_UB_31 0.0817396000 _diffrn_orient_matrix_UB_32 0.0054595000 _diffrn_orient_matrix_UB_33 -0.0953209000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5144 _reflns_number_total 6732 _reflns_odcompleteness_completeness 98.52 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. 2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.459 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.047 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 439 _refine_ls_number_reflns 6732 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0510 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0869P)^2^+0.1863P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1362 _refine_ls_wR_factor_ref 0.1518 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.4727(2) 0.31363(6) 0.39302(11) 0.0296(4) Uani 1 1 d . . . C2 C 0.4723(2) 0.35170(6) 0.39248(11) 0.0328(4) Uani 1 1 d . . . C3 C 0.2238(3) 0.42367(6) 0.39292(13) 0.0376(4) Uani 1 1 d . . . H3 H 0.1740 0.4098 0.4468 0.045 Uiso 1 1 calc R . . C4 C 0.1875(3) 0.47091(7) 0.40391(19) 0.0571(6) Uani 1 1 d . . . H4A H 0.2393 0.4808 0.4610 0.086 Uiso 1 1 calc R . . H4B H 0.0642 0.4756 0.4044 0.086 Uiso 1 1 calc R . . H4C H 0.2363 0.4861 0.3533 0.086 Uiso 1 1 calc R . . C5 C 0.1251(3) 0.40586(10) 0.30801(18) 0.0650(7) Uani 1 1 d . . . H5A H 0.1620 0.4203 0.2535 0.098 Uiso 1 1 calc R . . H5B H 0.0024 0.4100 0.3150 0.098 Uiso 1 1 calc R . . H5C H 0.1491 0.3762 0.3024 0.098 Uiso 1 1 calc R . . C6 C 0.5945(3) 0.42992(6) 0.29628(12) 0.0364(4) Uani 1 1 d . . . H6 H 0.7062 0.4151 0.3015 0.044 Uiso 1 1 calc R . . C7 C 0.6392(3) 0.47701(7) 0.30192(15) 0.0508(5) Uani 1 1 d . . . H7A H 0.5343 0.4934 0.2964 0.076 Uiso 1 1 calc R . . H7B H 0.7151 0.4843 0.2527 0.076 Uiso 1 1 calc R . . H7C H 0.6962 0.4829 0.3602 0.076 Uiso 1 1 calc R . . C8 C 0.5200(3) 0.41856(7) 0.20019(13) 0.0468(5) Uani 1 1 d . . . H8A H 0.4912 0.3890 0.1984 0.070 Uiso 1 1 calc R . . H8B H 0.6050 0.4246 0.1545 0.070 Uiso 1 1 calc R . . H8C H 0.4171 0.4350 0.1876 0.070 Uiso 1 1 calc R . . C9 C 0.5702(3) 0.42740(6) 0.50781(12) 0.0371(4) Uani 1 1 d . . . H9 H 0.5678 0.4584 0.5087 0.045 Uiso 1 1 calc R . . C10 C 0.4751(3) 0.41195(7) 0.59340(13) 0.0494(5) Uani 1 1 d . . . H10A H 0.3576 0.4223 0.5913 0.074 Uiso 1 1 calc R . . H10B H 0.5338 0.4224 0.6481 0.074 Uiso 1 1 calc R . . H10C H 0.4743 0.3816 0.5944 0.074 Uiso 1 1 calc R . . C11 C 0.7624(3) 0.41371(8) 0.51452(15) 0.0498(5) Uani 1 1 d . . . H11A H 0.7693 0.3834 0.5141 0.075 Uiso 1 1 calc R . . H11B H 0.8142 0.4243 0.5709 0.075 Uiso 1 1 calc R . . H11C H 0.8234 0.4249 0.4628 0.075 Uiso 1 1 calc R . . C21 C 0.4743(2) 0.26844(5) 0.39546(11) 0.0274(3) Uani 1 1 d . . . C22 C 0.5523(2) 0.24728(5) 0.47227(10) 0.0264(3) Uani 1 1 d . . . C23 C 0.6273(2) 0.27005(5) 0.54692(11) 0.0293(4) Uani 1 1 d . . . H23 H 0.6251 0.2995 0.5456 0.035 Uiso 1 1 calc R . . C24 C 0.7042(2) 0.24969(6) 0.62221(11) 0.0294(4) Uani 1 1 d . . . C25 C 0.7816(2) 0.27313(6) 0.69704(12) 0.0348(4) Uani 1 1 d . . . H25 H 0.7798 0.3026 0.6956 0.042 Uiso 1 1 calc R . . C26 C 0.8576(3) 0.25297(7) 0.76982(12) 0.0397(4) Uani 1 1 d . . . H26 H 0.9077 0.2686 0.8179 0.048 Uiso 1 1 calc R . . C27 C 0.8613(3) 0.20799(7) 0.77343(12) 0.0413(5) Uani 1 1 d . . . H27 H 0.9133 0.1945 0.8241 0.050 Uiso 1 1 calc R . . C28 C 0.7898(3) 0.18441(6) 0.70386(11) 0.0354(4) Uani 1 1 d . . . H28 H 0.7940 0.1550 0.7073 0.043 Uiso 1 1 calc R . . C29 C 0.7080(2) 0.20438(6) 0.62513(11) 0.0302(4) Uani 1 1 d . . . C30 C 0.6334(2) 0.18136(6) 0.55252(11) 0.0292(4) Uani 1 1 d . . . H30 H 0.6355 0.1519 0.5550 0.035 Uiso 1 1 calc R . . C31 C 0.5542(2) 0.20151(5) 0.47491(10) 0.0267(3) Uani 1 1 d . . . C32 C 0.4777(2) 0.17810(5) 0.40147(10) 0.0273(3) Uani 1 1 d . . . C33 C 0.3988(2) 0.19926(5) 0.32531(10) 0.0272(4) Uani 1 1 d . . . C34 C 0.3196(2) 0.17663(6) 0.25091(11) 0.0294(4) Uani 1 1 d . . . H34 H 0.3195 0.1472 0.2523 0.035 Uiso 1 1 calc R . . C35 C 0.2423(2) 0.19729(6) 0.17615(11) 0.0305(4) Uani 1 1 d . . . C36 C 0.1583(2) 0.17474(7) 0.10108(12) 0.0374(4) Uani 1 1 d . . . H36 H 0.1536 0.1453 0.1025 0.045 Uiso 1 1 calc R . . C37 C 0.0859(3) 0.19593(7) 0.02822(12) 0.0442(5) Uani 1 1 d . . . H37 H 0.0337 0.1808 -0.0201 0.053 Uiso 1 1 calc R . . C38 C 0.0888(3) 0.24088(8) 0.02490(12) 0.0443(5) Uani 1 1 d . . . H38 H 0.0391 0.2549 -0.0257 0.053 Uiso 1 1 calc R . . C39 C 0.1636(2) 0.26350(7) 0.09496(12) 0.0379(4) Uani 1 1 d . . . H39 H 0.1626 0.2929 0.0924 0.045 Uiso 1 1 calc R . . C40 C 0.2441(2) 0.24263(6) 0.17285(11) 0.0311(4) Uani 1 1 d . . . C41 C 0.3199(2) 0.26536(6) 0.24481(11) 0.0296(4) Uani 1 1 d . . . H41 H 0.3199 0.2948 0.2422 0.036 Uiso 1 1 calc R . . C42 C 0.3973(2) 0.24496(5) 0.32202(10) 0.0266(3) Uani 1 1 d . . . C51 C 0.4793(2) 0.13058(5) 0.40465(10) 0.0287(4) Uani 1 1 d . . . C52 C 0.6196(2) 0.10821(6) 0.36754(11) 0.0307(4) Uani 1 1 d . . . C53 C 0.7643(3) 0.12897(6) 0.32826(12) 0.0359(4) Uani 1 1 d . . . H53 H 0.7685 0.1584 0.3281 0.043 Uiso 1 1 calc R . . C54 C 0.8972(3) 0.10663(7) 0.29087(13) 0.0447(5) Uani 1 1 d . . . H54 H 0.9902 0.1210 0.2654 0.054 Uiso 1 1 calc R . . C55 C 0.8946(3) 0.06195(8) 0.29049(14) 0.0496(5) Uani 1 1 d . . . H55 H 0.9851 0.0470 0.2642 0.060 Uiso 1 1 calc R . . C56 C 0.7603(3) 0.04076(7) 0.32843(13) 0.0438(5) Uani 1 1 d . . . H56 H 0.7607 0.0113 0.3282 0.053 Uiso 1 1 calc R . . C57 C 0.6183(3) 0.06276(6) 0.36865(11) 0.0347(4) Uani 1 1 d . . . C58 C 0.4809(3) 0.04149(6) 0.40912(12) 0.0386(4) Uani 1 1 d . . . H58 H 0.4807 0.0121 0.4101 0.046 Uiso 1 1 calc R . . C59 C 0.3439(3) 0.06338(6) 0.44807(11) 0.0352(4) Uani 1 1 d . . . C60 C 0.2039(3) 0.04207(7) 0.49223(13) 0.0431(5) Uani 1 1 d . . . H60 H 0.2032 0.0126 0.4944 0.052 Uiso 1 1 calc R . . C61 C 0.0729(3) 0.06389(8) 0.53077(15) 0.0507(5) Uani 1 1 d . . . H61 H -0.0145 0.0494 0.5608 0.061 Uiso 1 1 calc R . . C62 C 0.0680(3) 0.10858(7) 0.52573(14) 0.0476(5) Uani 1 1 d . . . H62 H -0.0239 0.1233 0.5512 0.057 Uiso 1 1 calc R . . C63 C 0.1975(3) 0.13012(6) 0.48363(12) 0.0379(4) Uani 1 1 d . . . H63 H 0.1919 0.1595 0.4803 0.045 Uiso 1 1 calc R . . C64 C 0.3410(2) 0.10873(6) 0.44471(11) 0.0317(4) Uani 1 1 d . . . Si1 Si 0.46271(6) 0.409789(15) 0.39581(3) 0.02929(14) 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 0.0331(8) 0.0301(9) 0.0255(7) 0.0018(6) 0.0006(7) 0.0005(7) C2 0.0391(9) 0.0284(9) 0.0309(8) 0.0001(7) -0.0015(7) -0.0005(8) C3 0.0369(9) 0.0349(10) 0.0408(9) -0.0011(8) -0.0010(8) 0.0002(8) C4 0.0468(12) 0.0376(12) 0.0869(17) 0.0039(12) 0.0019(12) 0.0096(10) C5 0.0351(11) 0.093(2) 0.0662(14) -0.0243(14) -0.0106(11) 0.0024(12) C6 0.0379(9) 0.0322(10) 0.0391(9) 0.0053(7) -0.0003(8) 0.0003(8) C7 0.0616(14) 0.0429(12) 0.0479(11) 0.0092(9) -0.0019(10) -0.0117(11) C8 0.0575(13) 0.0480(12) 0.0349(9) -0.0002(8) 0.0018(9) 0.0016(10) C9 0.0451(10) 0.0285(9) 0.0375(9) -0.0013(7) -0.0044(8) -0.0032(8) C10 0.0639(14) 0.0496(13) 0.0348(10) -0.0025(9) 0.0008(9) -0.0076(11) C11 0.0469(12) 0.0558(14) 0.0459(11) 0.0019(9) -0.0137(9) -0.0014(10) C21 0.0319(8) 0.0233(8) 0.0272(8) 0.0011(6) 0.0022(7) 0.0009(7) C22 0.0306(8) 0.0253(8) 0.0233(7) 0.0005(6) 0.0004(6) -0.0003(7) C23 0.0349(9) 0.0243(8) 0.0288(8) -0.0028(6) 0.0015(7) -0.0019(7) C24 0.0299(8) 0.0341(9) 0.0241(7) -0.0033(7) 0.0017(6) -0.0025(7) C25 0.0389(9) 0.0367(10) 0.0288(8) -0.0072(7) 0.0003(7) -0.0027(8) C26 0.0424(10) 0.0507(12) 0.0258(8) -0.0077(8) -0.0039(7) -0.0028(9) C27 0.0456(11) 0.0532(12) 0.0247(8) 0.0034(8) -0.0049(8) 0.0017(10) C28 0.0423(10) 0.0359(10) 0.0278(8) 0.0050(7) -0.0033(7) -0.0008(8) C29 0.0333(8) 0.0349(9) 0.0222(7) 0.0018(6) 0.0002(7) -0.0012(7) C30 0.0352(8) 0.0259(8) 0.0263(7) 0.0015(6) -0.0026(7) 0.0001(7) C31 0.0314(8) 0.0257(8) 0.0231(7) 0.0001(6) -0.0006(6) -0.0016(7) C32 0.0346(8) 0.0226(8) 0.0245(7) 0.0000(6) -0.0013(7) 0.0011(7) C33 0.0316(8) 0.0272(9) 0.0226(7) 0.0011(6) -0.0008(6) -0.0001(7) C34 0.0353(9) 0.0271(8) 0.0259(7) -0.0015(6) -0.0010(7) 0.0007(7) C35 0.0308(8) 0.0387(10) 0.0220(7) -0.0015(7) -0.0002(6) 0.0009(7) C36 0.0393(9) 0.0439(11) 0.0290(8) -0.0054(8) -0.0029(7) 0.0033(9) C37 0.0447(11) 0.0641(14) 0.0235(8) -0.0044(8) -0.0076(8) 0.0037(10) C38 0.0423(10) 0.0650(14) 0.0252(8) 0.0105(9) -0.0045(8) 0.0058(10) C39 0.0384(9) 0.0459(11) 0.0293(8) 0.0107(8) 0.0002(7) 0.0040(9) C40 0.0316(8) 0.0380(10) 0.0238(7) 0.0055(7) 0.0020(7) 0.0019(7) C41 0.0317(8) 0.0287(9) 0.0284(8) 0.0048(6) 0.0021(7) 0.0015(7) C42 0.0293(8) 0.0264(9) 0.0241(7) 0.0020(6) 0.0012(6) 0.0000(7) C51 0.0394(9) 0.0249(8) 0.0213(7) -0.0002(6) -0.0064(7) -0.0025(7) C52 0.0414(10) 0.0293(9) 0.0212(7) 0.0005(6) -0.0044(7) 0.0004(7) C53 0.0442(10) 0.0341(10) 0.0292(8) 0.0033(7) -0.0016(7) 0.0006(8) C54 0.0433(11) 0.0530(13) 0.0379(10) 0.0024(9) 0.0049(9) 0.0018(10) C55 0.0548(13) 0.0535(13) 0.0406(10) -0.0028(9) 0.0030(9) 0.0167(11) C56 0.0607(13) 0.0346(10) 0.0361(9) -0.0026(8) -0.0028(9) 0.0116(10) C57 0.0496(11) 0.0287(9) 0.0254(8) 0.0000(7) -0.0049(7) 0.0043(8) C58 0.0588(12) 0.0236(9) 0.0330(8) 0.0011(7) -0.0070(8) -0.0008(8) C59 0.0490(11) 0.0284(9) 0.0277(8) 0.0010(7) -0.0062(8) -0.0065(8) C60 0.0568(12) 0.0335(10) 0.0386(9) 0.0043(8) -0.0056(9) -0.0155(9) C61 0.0524(12) 0.0561(14) 0.0438(10) 0.0043(10) 0.0033(10) -0.0192(11) C62 0.0452(11) 0.0532(13) 0.0445(10) -0.0033(9) 0.0061(9) -0.0061(10) C63 0.0450(11) 0.0350(10) 0.0336(9) -0.0023(7) 0.0006(8) -0.0040(8) C64 0.0424(10) 0.0293(9) 0.0232(7) -0.0003(6) -0.0056(7) -0.0028(8) Si1 0.0351(3) 0.0215(2) 0.0311(2) 0.00060(17) -0.00176(19) -0.00037(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.203(3) . ? C1 C21 1.428(2) . ? C2 Si1 1.8369(19) . ? C3 C4 1.527(3) . ? C3 C5 1.536(3) . ? C3 Si1 1.888(2) . ? C6 C7 1.528(3) . ? C6 C8 1.534(3) . ? C6 Si1 1.8912(19) . ? C9 C10 1.534(3) . ? C9 C11 1.541(3) . ? C9 Si1 1.8862(18) . ? C21 C22 1.418(2) . ? C21 C42 1.414(2) . ? C22 C23 1.410(2) . ? C22 C31 1.446(2) . ? C23 C24 1.386(2) . ? C24 C25 1.430(2) . ? C24 C29 1.432(3) . ? C25 C26 1.352(3) . ? C26 C27 1.422(3) . ? C27 C28 1.358(3) . ? C28 C29 1.435(2) . ? C29 C30 1.391(2) . ? C30 C31 1.416(2) . ? C31 C32 1.412(2) . ? C32 C33 1.414(2) . ? C32 C51 1.502(2) . ? C33 C34 1.418(2) . ? C33 C42 1.444(2) . ? C34 C35 1.386(2) . ? C35 C36 1.439(2) . ? C35 C40 1.433(3) . ? C36 C37 1.357(3) . ? C37 C38 1.421(3) . ? C38 C39 1.357(3) . ? C39 C40 1.434(2) . ? C40 C41 1.383(2) . ? C41 C42 1.410(2) . ? C51 C52 1.407(3) . ? C51 C64 1.405(3) . ? C52 C53 1.422(3) . ? C52 C57 1.436(2) . ? C53 C54 1.364(3) . ? C54 C55 1.411(3) . ? C55 C56 1.358(3) . ? C56 C57 1.430(3) . ? C57 C58 1.393(3) . ? C58 C59 1.391(3) . ? C59 C60 1.433(3) . ? C59 C64 1.434(2) . ? C60 C61 1.352(3) . ? C61 C62 1.414(3) . ? C62 C63 1.362(3) . ? C63 C64 1.422(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C21 178.91(18) . . ? C1 C2 Si1 177.12(17) . . ? C4 C3 C5 110.69(19) . . ? C4 C3 Si1 113.88(15) . . ? C5 C3 Si1 113.23(14) . . ? C7 C6 C8 110.77(16) . . ? C7 C6 Si1 114.24(14) . . ? C8 C6 Si1 114.65(14) . . ? C10 C9 C11 109.58(17) . . ? C10 C9 Si1 113.14(14) . . ? C11 C9 Si1 111.78(14) . . ? C22 C21 C1 119.59(15) . . ? C42 C21 C1 120.15(14) . . ? C42 C21 C22 120.25(16) . . ? C21 C22 C31 119.71(14) . . ? C23 C22 C21 121.20(16) . . ? C23 C22 C31 119.09(14) . . ? C24 C23 C22 121.66(16) . . ? C23 C24 C25 121.17(17) . . ? C23 C24 C29 119.68(15) . . ? C25 C24 C29 119.15(15) . . ? C26 C25 C24 120.72(18) . . ? C25 C26 C27 120.48(17) . . ? C28 C27 C26 120.88(17) . . ? C27 C28 C29 120.65(18) . . ? C24 C29 C28 118.11(15) . . ? C30 C29 C24 119.50(15) . . ? C30 C29 C28 122.39(17) . . ? C29 C30 C31 121.77(16) . . ? C30 C31 C22 118.30(14) . . ? C32 C31 C22 120.00(14) . . ? C32 C31 C30 121.70(16) . . ? C31 C32 C33 120.19(15) . . ? C31 C32 C51 119.83(14) . . ? C33 C32 C51 119.98(14) . . ? C32 C33 C34 121.50(16) . . ? C32 C33 C42 120.09(14) . . ? C34 C33 C42 118.42(14) . . ? C35 C34 C33 121.62(16) . . ? C34 C35 C36 122.21(18) . . ? C34 C35 C40 119.51(15) . . ? C40 C35 C36 118.29(15) . . ? C37 C36 C35 120.72(19) . . ? C36 C37 C38 120.84(18) . . ? C39 C38 C37 120.51(17) . . ? C38 C39 C40 120.84(19) . . ? C35 C40 C39 118.78(16) . . ? C41 C40 C35 119.88(15) . . ? C41 C40 C39 121.33(18) . . ? C40 C41 C42 121.49(17) . . ? C21 C42 C33 119.76(14) . . ? C41 C42 C21 121.17(16) . . ? C41 C42 C33 119.08(15) . . ? C52 C51 C32 119.75(16) . . ? C64 C51 C32 119.86(16) . . ? C64 C51 C52 120.39(16) . . ? C51 C52 C53 122.38(16) . . ? C51 C52 C57 119.49(17) . . ? C53 C52 C57 118.14(17) . . ? C54 C53 C52 121.38(18) . . ? C53 C54 C55 120.5(2) . . ? C56 C55 C54 120.1(2) . . ? C55 C56 C57 121.38(19) . . ? C56 C57 C52 118.40(18) . . ? C58 C57 C52 119.51(17) . . ? C58 C57 C56 122.09(18) . . ? C59 C58 C57 121.36(17) . . ? C58 C59 C60 122.13(18) . . ? C58 C59 C64 119.61(17) . . ? C60 C59 C64 118.26(18) . . ? C61 C60 C59 121.31(19) . . ? C60 C61 C62 120.5(2) . . ? C63 C62 C61 120.2(2) . . ? C62 C63 C64 121.52(19) . . ? C51 C64 C59 119.59(17) . . ? C51 C64 C63 122.19(17) . . ? C63 C64 C59 118.21(17) . . ? C2 Si1 C3 105.72(9) . . ? C2 Si1 C6 107.06(8) . . ? C2 Si1 C9 107.47(8) . . ? C3 Si1 C6 116.34(9) . . ? C9 Si1 C3 110.88(9) . . ? C9 Si1 C6 108.92(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 C1 C2 Si1 C3 -42(3) . . . . ? C1 C2 Si1 C6 -167(3) . . . . ? C1 C2 Si1 C9 76(3) . . . . ? C1 C21 C22 C23 0.5(2) . . . . ? C1 C21 C22 C31 -179.98(15) . . . . ? C1 C21 C42 C33 -179.70(15) . . . . ? C1 C21 C42 C41 0.9(2) . . . . ? C2 C1 C21 C22 -10(11) . . . . ? C2 C1 C21 C42 169(11) . . . . ? C4 C3 Si1 C2 174.81(15) . . . . ? C4 C3 Si1 C6 -66.54(18) . . . . ? C4 C3 Si1 C9 58.63(18) . . . . ? C5 C3 Si1 C2 -57.56(18) . . . . ? C5 C3 Si1 C6 61.09(19) . . . . ? C5 C3 Si1 C9 -173.74(17) . . . . ? C7 C6 Si1 C2 -165.49(14) . . . . ? C7 C6 Si1 C3 76.60(16) . . . . ? C7 C6 Si1 C9 -49.57(17) . . . . ? C8 C6 Si1 C2 65.12(16) . . . . ? C8 C6 Si1 C3 -52.79(18) . . . . ? C8 C6 Si1 C9 -178.96(14) . . . . ? C10 C9 Si1 C2 -63.26(17) . . . . ? C10 C9 Si1 C3 51.83(17) . . . . ? C10 C9 Si1 C6 -178.92(15) . . . . ? C11 C9 Si1 C2 61.02(16) . . . . ? C11 C9 Si1 C3 176.11(14) . . . . ? C11 C9 Si1 C6 -54.64(16) . . . . ? C21 C1 C2 Si1 -67(12) . . . . ? C21 C22 C23 C24 -179.86(16) . . . . ? C21 C22 C31 C30 179.90(15) . . . . ? C21 C22 C31 C32 -0.4(2) . . . . ? C22 C21 C42 C33 -0.2(2) . . . . ? C22 C21 C42 C41 -179.65(15) . . . . ? C22 C23 C24 C25 179.26(16) . . . . ? C22 C23 C24 C29 -0.2(3) . . . . ? C22 C31 C32 C33 -0.1(2) . . . . ? C22 C31 C32 C51 -179.76(15) . . . . ? C23 C22 C31 C30 -0.6(2) . . . . ? C23 C22 C31 C32 179.13(15) . . . . ? C23 C24 C25 C26 -179.46(17) . . . . ? C23 C24 C29 C28 179.54(16) . . . . ? C23 C24 C29 C30 -0.4(2) . . . . ? C24 C25 C26 C27 -0.2(3) . . . . ? C24 C29 C30 C31 0.4(3) . . . . ? C25 C24 C29 C28 0.1(2) . . . . ? C25 C24 C29 C30 -179.82(16) . . . . ? C25 C26 C27 C28 0.4(3) . . . . ? C26 C27 C28 C29 -0.3(3) . . . . ? C27 C28 C29 C24 0.1(3) . . . . ? C27 C28 C29 C30 180.00(18) . . . . ? C28 C29 C30 C31 -179.51(16) . . . . ? C29 C24 C25 C26 0.0(3) . . . . ? C29 C30 C31 C22 0.1(2) . . . . ? C29 C30 C31 C32 -179.67(16) . . . . ? C30 C31 C32 C33 179.60(16) . . . . ? C30 C31 C32 C51 0.0(2) . . . . ? C31 C22 C23 C24 0.7(2) . . . . ? C31 C32 C33 C34 -179.42(16) . . . . ? C31 C32 C33 C42 0.5(2) . . . . ? C31 C32 C51 C52 -89.60(19) . . . . ? C31 C32 C51 C64 90.3(2) . . . . ? C32 C33 C34 C35 -179.94(16) . . . . ? C32 C33 C42 C21 -0.3(2) . . . . ? C32 C33 C42 C41 179.16(15) . . . . ? C32 C51 C52 C53 1.4(2) . . . . ? C32 C51 C52 C57 -178.41(14) . . . . ? C32 C51 C64 C59 -179.61(14) . . . . ? C32 C51 C64 C63 -0.4(2) . . . . ? C33 C32 C51 C52 90.8(2) . . . . ? C33 C32 C51 C64 -89.28(19) . . . . ? C33 C34 C35 C36 -178.73(16) . . . . ? C33 C34 C35 C40 0.9(3) . . . . ? C34 C33 C42 C21 179.59(15) . . . . ? C34 C33 C42 C41 -0.9(2) . . . . ? C34 C35 C36 C37 -179.09(18) . . . . ? C34 C35 C40 C39 179.96(16) . . . . ? C34 C35 C40 C41 -1.1(3) . . . . ? C35 C36 C37 C38 -1.0(3) . . . . ? C35 C40 C41 C42 0.4(3) . . . . ? C36 C35 C40 C39 -0.4(2) . . . . ? C36 C35 C40 C41 178.47(16) . . . . ? C36 C37 C38 C39 -0.3(3) . . . . ? C37 C38 C39 C40 1.2(3) . . . . ? C38 C39 C40 C35 -0.8(3) . . . . ? C38 C39 C40 C41 -179.70(18) . . . . ? C39 C40 C41 C42 179.22(16) . . . . ? C40 C35 C36 C37 1.3(3) . . . . ? C40 C41 C42 C21 -179.86(16) . . . . ? C40 C41 C42 C33 0.7(2) . . . . ? C42 C21 C22 C23 -178.96(15) . . . . ? C42 C21 C22 C31 0.5(2) . . . . ? C42 C33 C34 C35 0.2(2) . . . . ? C51 C32 C33 C34 0.2(2) . . . . ? C51 C32 C33 C42 -179.92(15) . . . . ? C51 C52 C53 C54 -178.57(16) . . . . ? C51 C52 C57 C56 178.46(15) . . . . ? C51 C52 C57 C58 -2.0(2) . . . . ? C52 C51 C64 C59 0.3(2) . . . . ? C52 C51 C64 C63 179.50(15) . . . . ? C52 C53 C54 C55 -0.2(3) . . . . ? C52 C57 C58 C59 0.4(2) . . . . ? C53 C52 C57 C56 -1.4(2) . . . . ? C53 C52 C57 C58 178.10(15) . . . . ? C53 C54 C55 C56 -0.7(3) . . . . ? C54 C55 C56 C57 0.6(3) . . . . ? C55 C56 C57 C52 0.5(3) . . . . ? C55 C56 C57 C58 -178.99(18) . . . . ? C56 C57 C58 C59 179.90(16) . . . . ? C57 C52 C53 C54 1.3(2) . . . . ? C57 C58 C59 C60 -178.24(17) . . . . ? C57 C58 C59 C64 1.6(2) . . . . ? C58 C59 C60 C61 179.14(18) . . . . ? C58 C59 C64 C51 -2.0(2) . . . . ? C58 C59 C64 C63 178.84(16) . . . . ? C59 C60 C61 C62 2.1(3) . . . . ? C60 C59 C64 C51 177.87(15) . . . . ? C60 C59 C64 C63 -1.3(2) . . . . ? C60 C61 C62 C63 -1.4(3) . . . . ? C61 C62 C63 C64 -0.7(3) . . . . ? C62 C63 C64 C51 -177.17(17) . . . . ? C62 C63 C64 C59 2.0(3) . . . . ? C64 C51 C52 C53 -178.50(15) . . . . ? C64 C51 C52 C57 1.7(2) . . . . ? C64 C59 C60 C61 -0.7(3) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -5 0 0 0.0786 -4.9998 0.0033 0.0005 -0.6511 0.6443 -0.4087 0 -3 9 0.2140 -0.0000 -2.9994 9.0002 0.3146 -0.2708 -0.8743 1 -20 0 0.0524 1.0000 -19.9994 0.0002 0.8451 0.5261 -0.0275 0 -2 9 0.2139 -0.0000 -1.9995 9.0002 0.2788 -0.3036 -0.8688 5 2 -1 0.0771 4.9998 1.9965 -1.0006 0.5565 -0.6688 0.5150 -2 -1 9 0.1972 -2.0000 -0.9983 9.0004 -0.0173 -0.0786 -1.0269 2 1 -9 0.1843 2.0000 0.9983 -9.0004 0.0173 0.0786 1.0269 -4 14 0 0.0835 -3.9999 14.0017 0.0002 -1.0213 0.0570 -0.2505 0 20 1 0.0738 -0.0000 19.9988 0.9997 -0.6919 -0.6960 0.0139 -5 3 -3 0.1088 -4.9998 3.0030 -2.9996 -0.8274 0.6691 -0.1064 5 4 0 0.0756 4.9998 3.9965 -0.0006 0.5081 -0.7753 0.4306 4 -11 1 0.0724 3.9999 -11.0019 0.9998 0.9371 -0.1962 0.1716 _database_code_depnum_ccdc_archive 'CCDC 927705' ####################################################################### # # 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_global _ccdc_journal_depnumber ? #------------------------------------------------------------------------- #4 Chemical and physical data # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag include any ASCII file output by a chemical drawing # package # Against _type record, for example, ChemDraw # Against _records supply the chemical connectivity records _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H48 Si' _chemical_formula_weight 676.97 _chemical_melting_point ? _ccdc_compound_id ? _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ? _exptl_crystal_density_diffrn ? _exptl_crystal_colour violet #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _diffrn_radiation_type Cu _diffrn_measurement_device 'Agilent Xcalibur Enhance Ultra' _ccdc_temp_data_collection 173(2) _ccdc_ls_R_squared ? _refine_ls_abs_structure_details ? _ccdc_disorder ? _ccdc_comments ? #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # Do not include structure factors data_see01 _audit_creation_date 2012-08-20 _audit_creation_method ; Olex2 1.2 (compiled 2012.05.09 svn.r2324, GUI svn.r4230) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C50 H48 Si' _chemical_formula_sum 'C50 H48 Si' _chemical_formula_weight 676.97 _chemical_melting_point ? _chemical_oxdiff_formula 'C50 H48 Si' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.2544(2) _cell_length_b 18.2908(5) _cell_length_c 24.1358(5) _cell_angle_alpha 90.662(2) _cell_angle_beta 98.7052(19) _cell_angle_gamma 103.547(2) _cell_volume 3921.36(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9240 _cell_measurement_temperature 173.00(10) _cell_measurement_theta_max 62.4908 _cell_measurement_theta_min 3.1726 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74846 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark violet' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1448 _exptl_crystal_recrystallization_method 'crystallized from DCM/MeOH' _exptl_crystal_size_max 0.3344 _exptl_crystal_size_mid 0.1658 _exptl_crystal_size_min 0.0623 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_unetI/netI 0.0316 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 18734 _diffrn_reflns_theta_full 62.58 _diffrn_reflns_theta_max 62.58 _diffrn_reflns_theta_min 3.18 _diffrn_ambient_temperature 173.00(10) _diffrn_detector_area_resol_mean 10.2679 _diffrn_measured_fraction_theta_full 0.952 _diffrn_measured_fraction_theta_max 0.952 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -75.00 29.00 1.0000 14.7300 omega____ theta____ kappa____ phi______ frames - 1.5625 -77.0000 120.0000 104 #__ type_ start__ end____ width___ exp.time_ 2 omega 35.00 92.00 1.0000 14.7300 omega____ theta____ kappa____ phi______ frames - 1.5625 178.0000 0.0000 57 #__ type_ start__ end____ width___ exp.time_ 3 omega -156.00 -55.00 1.0000 58.9000 omega____ theta____ kappa____ phi______ frames - -82.0779 -61.0000 -60.0000 101 #__ type_ start__ end____ width___ exp.time_ 4 omega -63.00 -4.00 1.0000 58.9000 omega____ theta____ kappa____ phi______ frames - -82.0779 30.0000 90.0000 59 #__ type_ start__ end____ width___ exp.time_ 5 omega -153.00 -51.00 1.0000 58.9000 omega____ theta____ kappa____ phi______ frames - -82.0779 -77.0000 0.0000 102 #__ type_ start__ end____ width___ exp.time_ 6 omega 2.00 108.00 1.0000 58.9000 omega____ theta____ kappa____ phi______ frames - 85.2029 -94.0000 -90.0000 106 #__ type_ start__ end____ width___ exp.time_ 7 omega 17.00 118.00 1.0000 58.9000 omega____ theta____ kappa____ phi______ frames - 85.2029 -77.0000 120.0000 101 #__ type_ start__ end____ width___ exp.time_ 8 omega 43.00 105.00 1.0000 58.9000 omega____ theta____ kappa____ phi______ frames - 85.2029 -77.0000 19.0000 62 #__ type_ start__ end____ width___ exp.time_ 9 omega 8.00 34.00 1.0000 58.9000 omega____ theta____ kappa____ phi______ frames - 85.2029 -77.0000 19.0000 26 #__ type_ start__ end____ width___ exp.time_ 10 omega 7.00 68.00 1.0000 58.9000 omega____ theta____ kappa____ phi______ frames - 85.2029 -30.0000 150.0000 61 ; _diffrn_measurement_device_type 'Xcalibur, Ruby, Ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0264750000 _diffrn_orient_matrix_UB_12 0.0853931000 _diffrn_orient_matrix_UB_13 -0.0075275000 _diffrn_orient_matrix_UB_21 0.1177246000 _diffrn_orient_matrix_UB_22 0.0148554000 _diffrn_orient_matrix_UB_23 0.0538273000 _diffrn_orient_matrix_UB_31 0.1245618000 _diffrn_orient_matrix_UB_32 -0.0033553000 _diffrn_orient_matrix_UB_33 -0.0350084000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 10554 _reflns_number_total 11951 _reflns_odcompleteness_completeness 98.71 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 58.86 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.966 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.059 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 951 _refine_ls_number_reflns 11951 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0794 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1121P)^2^+5.3901P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2168 _refine_ls_wR_factor_ref 0.2239 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.7850(4) 0.81600(19) 0.11827(14) 0.0450(8) Uani 1 1 d . A . C2 C 0.6862(4) 0.79985(18) 0.07807(13) 0.0409(7) Uani 1 1 d . . . C3 C 0.9963(7) 0.9380(4) 0.1993(3) 0.0565(13) Uani 0.579(3) 1 d PD A 1 H3A H 0.9058 0.9562 0.1988 0.068 Uiso 0.579(3) 1 calc PR A 1 H3B H 1.0472 0.9436 0.2379 0.068 Uiso 0.579(3) 1 calc PR A 1 C3A C 1.0816(10) 0.9243(5) 0.1721(4) 0.0565(13) Uani 0.421(3) 1 d PD A 2 H3AA H 1.1704 0.9243 0.1992 0.068 Uiso 0.421(3) 1 calc PR A 2 H3AB H 1.1098 0.9217 0.1351 0.068 Uiso 0.421(3) 1 calc PR A 2 C4 C 1.0985(9) 0.9906(4) 0.1647(4) 0.065(2) Uani 0.579(3) 1 d PD A 1 H4 H 1.1793 0.9663 0.1591 0.078 Uiso 0.579(3) 1 calc PR A 1 C4A C 1.0427(12) 0.9997(6) 0.1793(6) 0.065(2) Uani 0.421(3) 1 d PD A 2 H4A H 0.9766 0.9956 0.2078 0.078 Uiso 0.421(3) 1 calc PR A 2 C5 C 1.1733(7) 1.0661(3) 0.1955(3) 0.1086(19) Uani 1 1 d D . . H5AA H 1.0975 1.0895 0.2054 0.163 Uiso 0.579(3) 1 calc PR A 1 H5AB H 1.2320 1.0980 0.1716 0.163 Uiso 0.579(3) 1 calc PR A 1 H5AC H 1.2377 1.0585 0.2289 0.163 Uiso 0.579(3) 1 calc PR A 1 H5BD H 1.2314 1.0574 0.2302 0.163 Uiso 0.421(3) 1 calc PR A 2 H5BE H 1.1368 1.1104 0.2000 0.163 Uiso 0.421(3) 1 calc PR A 2 H5BF H 1.2355 1.0730 0.1666 0.163 Uiso 0.421(3) 1 calc PR A 2 C6 C 1.0119(14) 0.9974(6) 0.1065(5) 0.1086(19) Uani 0.579(3) 1 d PD A 1 H6A H 0.9880 0.9498 0.0859 0.163 Uiso 0.579(3) 1 calc PR A 1 H6B H 1.0727 1.0348 0.0867 0.163 Uiso 0.579(3) 1 calc PR A 1 H6C H 0.9205 1.0119 0.1104 0.163 Uiso 0.579(3) 1 calc PR A 1 C6A C 0.9617(19) 1.0225(8) 0.1252(7) 0.1086(19) Uani 0.421(3) 1 d PD A 2 H6AA H 1.0134 1.0151 0.0948 0.163 Uiso 0.421(3) 1 calc PR A 2 H6AB H 0.9600 1.0746 0.1288 0.163 Uiso 0.421(3) 1 calc PR A 2 H6AC H 0.8604 0.9921 0.1178 0.163 Uiso 0.421(3) 1 calc PR A 2 C7 C 1.1022(6) 0.8045(3) 0.1615(2) 0.0476(11) Uani 0.579(3) 1 d PD A 1 H7A H 1.1288 0.8296 0.1280 0.057 Uiso 0.579(3) 1 calc PR A 1 H7B H 1.1854 0.8235 0.1916 0.057 Uiso 0.579(3) 1 calc PR A 1 C7A C 1.0382(9) 0.7564(5) 0.1836(3) 0.0476(11) Uani 0.421(3) 1 d PD A 2 H7AA H 1.1041 0.7634 0.2195 0.057 Uiso 0.421(3) 1 calc PR A 2 H7AB H 0.9630 0.7097 0.1847 0.057 Uiso 0.421(3) 1 calc PR A 2 C8 C 1.0929(10) 0.7211(4) 0.1514(4) 0.0535(17) Uani 0.579(3) 1 d PD A 1 H8 H 1.0481 0.6944 0.1819 0.064 Uiso 0.579(3) 1 calc PR A 1 C8A C 1.1318(16) 0.7444(7) 0.1394(6) 0.0535(17) Uani 0.421(3) 1 d PD A 2 H8A H 1.2361 0.7601 0.1440 0.064 Uiso 0.421(3) 1 calc PR A 2 C9 C 1.2544(6) 0.7078(3) 0.1542(2) 0.0856(15) Uani 1 1 d . A 1 H9A H 1.2998 0.7318 0.1238 0.128 Uiso 1 1 calc R A 1 H9B H 1.2482 0.6547 0.1513 0.128 Uiso 1 1 calc R A 1 H9C H 1.3146 0.7287 0.1893 0.128 Uiso 1 1 calc R A 1 C10 C 0.994(3) 0.6884(15) 0.0965(6) 0.086(5) Uani 0.579(3) 1 d PD A 1 H10A H 0.8899 0.6786 0.1012 0.129 Uiso 0.579(3) 1 calc PR A 1 H10B H 1.0171 0.6422 0.0860 0.129 Uiso 0.579(3) 1 calc PR A 1 H10C H 1.0117 0.7236 0.0677 0.129 Uiso 0.579(3) 1 calc PR A 1 C10A C 1.035(5) 0.704(2) 0.0870(9) 0.086(5) Uani 0.421(3) 1 d PD A 2 H10D H 1.0956 0.7030 0.0582 0.129 Uiso 0.421(3) 1 calc PR A 2 H10E H 0.9571 0.7292 0.0743 0.129 Uiso 0.421(3) 1 calc PR A 2 H10F H 0.9896 0.6529 0.0951 0.129 Uiso 0.421(3) 1 calc PR A 2 C11 C 0.8628(7) 0.7778(4) 0.2383(3) 0.0524(12) Uani 0.579(3) 1 d PD A 1 H11A H 0.8326 0.7254 0.2251 0.063 Uiso 0.579(3) 1 calc PR A 1 H11B H 0.9461 0.7824 0.2689 0.063 Uiso 0.579(3) 1 calc PR A 1 C11A C 0.8611(10) 0.8440(5) 0.2444(3) 0.0524(12) Uani 0.421(3) 1 d PD A 2 H11C H 0.9425 0.8727 0.2720 0.063 Uiso 0.421(3) 1 calc PR A 2 H11D H 0.7867 0.8737 0.2371 0.063 Uiso 0.421(3) 1 calc PR A 2 C12 C 0.7309(8) 0.7963(4) 0.2628(3) 0.0595(16) Uani 0.579(3) 1 d PD A 1 H12 H 0.6558 0.8058 0.2323 0.071 Uiso 0.579(3) 1 calc PR A 1 C12A C 0.7885(11) 0.7721(6) 0.2712(4) 0.0595(16) Uani 0.421(3) 1 d PD A 2 H12A H 0.8615 0.7407 0.2761 0.071 Uiso 0.421(3) 1 calc PR A 2 C13 C 0.7856(11) 0.8661(5) 0.3041(4) 0.0918(16) Uani 0.579(3) 1 d PD A 1 H13A H 0.8712 0.8605 0.3301 0.138 Uiso 0.579(3) 1 calc PR A 1 H13B H 0.7061 0.8707 0.3243 0.138 Uiso 0.579(3) 1 calc PR A 1 H13C H 0.8134 0.9105 0.2835 0.138 Uiso 0.579(3) 1 calc PR A 1 C13A C 0.7486(15) 0.7858(9) 0.3283(5) 0.0918(16) Uani 0.421(3) 1 d PD A 2 H13D H 0.8310 0.8211 0.3504 0.138 Uiso 0.421(3) 1 calc PR A 2 H13E H 0.7287 0.7392 0.3469 0.138 Uiso 0.421(3) 1 calc PR A 2 H13F H 0.6606 0.8058 0.3239 0.138 Uiso 0.421(3) 1 calc PR A 2 C14 C 0.6587(11) 0.7323(6) 0.2961(4) 0.0918(16) Uani 0.579(3) 1 d PD A 1 H14A H 0.6179 0.6881 0.2717 0.138 Uiso 0.579(3) 1 calc PR A 1 H14B H 0.5793 0.7459 0.3122 0.138 Uiso 0.579(3) 1 calc PR A 1 H14C H 0.7328 0.7223 0.3254 0.138 Uiso 0.579(3) 1 calc PR A 1 C14A C 0.6428(13) 0.7252(8) 0.2346(5) 0.0918(16) Uani 0.421(3) 1 d PD A 2 H14D H 0.5698 0.7551 0.2282 0.138 Uiso 0.421(3) 1 calc PR A 2 H14E H 0.6026 0.6811 0.2537 0.138 Uiso 0.421(3) 1 calc PR A 2 H14F H 0.6658 0.7104 0.1993 0.138 Uiso 0.421(3) 1 calc PR A 2 C21 C 0.5665(3) 0.78079(18) 0.03115(12) 0.0369(7) Uani 1 1 d . . . C22 C 0.5415(3) 0.83618(17) -0.00656(12) 0.0359(7) Uani 1 1 d . . . C23 C 0.6328(3) 0.90930(18) -0.00128(13) 0.0392(7) Uani 1 1 d . . . H23 H 0.7128 0.9216 0.0282 0.047 Uiso 1 1 calc R . . C24 C 0.6090(4) 0.96419(18) -0.03815(14) 0.0416(7) Uani 1 1 d . . . C25 C 0.6977(4) 1.04010(19) -0.03092(15) 0.0483(8) Uani 1 1 d . . . H25 H 0.7776 1.0532 -0.0014 0.058 Uiso 1 1 calc R . . C26 C 0.6663(4) 1.0931(2) -0.06665(15) 0.0527(9) Uani 1 1 d . . . H26 H 0.7228 1.1426 -0.0605 0.063 Uiso 1 1 calc R . . C27 C 0.5481(4) 1.0742(2) -0.11339(16) 0.0533(9) Uani 1 1 d . . . H27 H 0.5296 1.1110 -0.1378 0.064 Uiso 1 1 calc R . . C28 C 0.4627(4) 1.00296(19) -0.12244(15) 0.0474(8) Uani 1 1 d . . . H28 H 0.3869 0.9912 -0.1534 0.057 Uiso 1 1 calc R . . C29 C 0.4871(4) 0.94539(18) -0.08503(13) 0.0404(7) Uani 1 1 d . . . C30 C 0.3965(3) 0.87291(17) -0.09112(13) 0.0373(7) Uani 1 1 d . . . H30 H 0.3193 0.8606 -0.1216 0.045 Uiso 1 1 calc R . . C31 C 0.4167(3) 0.81717(17) -0.05295(12) 0.0335(6) Uani 1 1 d . . . C32 C 0.3209(3) 0.74487(16) -0.05822(11) 0.0314(6) Uani 1 1 d . . . C33 C 0.3462(3) 0.68894(17) -0.02091(12) 0.0329(6) Uani 1 1 d . . . C34 C 0.2525(3) 0.61571(17) -0.02556(12) 0.0348(7) Uani 1 1 d . . . H34 H 0.1668 0.6049 -0.0527 0.042 Uiso 1 1 calc R . . C35 C 0.2830(3) 0.55894(17) 0.00878(12) 0.0363(7) Uani 1 1 d . . . C36 C 0.1904(4) 0.48411(18) 0.00280(13) 0.0414(7) Uani 1 1 d . . . H36 H 0.1041 0.4729 -0.0241 0.050 Uiso 1 1 calc R . . C37 C 0.2257(4) 0.4291(2) 0.03540(15) 0.0501(8) Uani 1 1 d . . . H37 H 0.1642 0.3806 0.0305 0.060 Uiso 1 1 calc R . . C38 C 0.3567(4) 0.4452(2) 0.07727(15) 0.0551(9) Uani 1 1 d . . . H38 H 0.3809 0.4072 0.0994 0.066 Uiso 1 1 calc R . . C39 C 0.4458(4) 0.5159(2) 0.08483(15) 0.0509(9) Uani 1 1 d . . . H39 H 0.5304 0.5257 0.1125 0.061 Uiso 1 1 calc R . . C40 C 0.4134(4) 0.57556(18) 0.05166(13) 0.0398(7) Uani 1 1 d . . . C41 C 0.5036(3) 0.64847(19) 0.05869(13) 0.0404(7) Uani 1 1 d . . . H41 H 0.5863 0.6594 0.0872 0.048 Uiso 1 1 calc R . . C42 C 0.4736(3) 0.70610(17) 0.02409(12) 0.0345(7) Uani 1 1 d . . . C51 C 0.1927(3) 0.72616(16) -0.10631(12) 0.0309(6) Uani 1 1 d . . . C52 C 0.2143(3) 0.69462(16) -0.15675(12) 0.0322(6) Uani 1 1 d . . . C53 C 0.3543(3) 0.67782(18) -0.16379(13) 0.0381(7) Uani 1 1 d . . . H53 H 0.4342 0.6882 -0.1342 0.046 Uiso 1 1 calc R . . C54 C 0.3718(4) 0.6473(2) -0.21260(14) 0.0466(8) Uani 1 1 d . . . H54 H 0.4641 0.6372 -0.2162 0.056 Uiso 1 1 calc R . . C55 C 0.2522(4) 0.6300(2) -0.25880(14) 0.0495(8) Uani 1 1 d . . . H55 H 0.2656 0.6083 -0.2921 0.059 Uiso 1 1 calc R . . C56 C 0.1186(4) 0.64547(19) -0.25389(13) 0.0440(8) Uani 1 1 d . . . H56 H 0.0408 0.6344 -0.2843 0.053 Uiso 1 1 calc R . . C57 C 0.0939(3) 0.67820(17) -0.20344(12) 0.0354(7) Uani 1 1 d . . . C58 C -0.0439(3) 0.69369(17) -0.19769(12) 0.0371(7) Uani 1 1 d . . . H58 H -0.1224 0.6824 -0.2278 0.045 Uiso 1 1 calc R . . C59 C -0.0666(3) 0.72556(17) -0.14813(12) 0.0351(7) Uani 1 1 d . . . C60 C -0.2070(4) 0.74244(19) -0.14202(14) 0.0450(8) Uani 1 1 d . . . H60 H -0.2862 0.7312 -0.1719 0.054 Uiso 1 1 calc R . . C61 C -0.2268(4) 0.7741(2) -0.09412(15) 0.0508(9) Uani 1 1 d . . . H61 H -0.3191 0.7847 -0.0913 0.061 Uiso 1 1 calc R . . C62 C -0.1078(4) 0.7917(2) -0.04776(15) 0.0489(8) Uani 1 1 d . . . H62 H -0.1222 0.8139 -0.0148 0.059 Uiso 1 1 calc R . . C63 C 0.0270(4) 0.77605(18) -0.05155(13) 0.0409(7) Uani 1 1 d . . . H63 H 0.1039 0.7875 -0.0209 0.049 Uiso 1 1 calc R . . C64 C 0.0532(3) 0.74248(16) -0.10143(12) 0.0332(6) Uani 1 1 d . . . Si1 Si 0.93651(10) 0.83492(5) 0.17936(4) 0.0411(2) Uani 1 1 d D . . C1" C -0.135(2) 0.0531(11) -0.6637(9) 0.136(2) Uani 0.299(5) 1 d PD B 2 H1"A H -0.0682 0.0265 -0.6770 0.204 Uiso 0.299(5) 1 calc PR B 2 H1"B H -0.2345 0.0352 -0.6846 0.204 Uiso 0.299(5) 1 calc PR B 2 H1"C H -0.1373 0.0449 -0.6246 0.204 Uiso 0.299(5) 1 calc PR B 2 C1' C 0.0738(5) 0.2340(2) -0.52323(17) 0.0629(11) Uani 1 1 d . B . C2' C 0.0365(5) 0.2662(2) -0.48620(15) 0.0562(10) Uani 1 1 d . . . C3' C 0.2939(5) 0.2332(3) -0.60673(18) 0.0723(12) Uani 1 1 d . B . H3'A H 0.3724 0.2577 -0.5765 0.087 Uiso 1 1 calc R . . H3'B H 0.3338 0.1974 -0.6260 0.087 Uiso 1 1 calc R . . C4' C 0.2678(5) 0.2929(3) -0.64771(17) 0.0669(11) Uani 1 1 d . . . H4' H 0.1744 0.2723 -0.6737 0.080 Uiso 1 1 calc R . . C5' C 0.3940(6) 0.3154(3) -0.6812(2) 0.0870(15) Uani 1 1 d . . . H5'A H 0.4848 0.3394 -0.6566 0.131 Uiso 1 1 calc R . . H5'B H 0.3693 0.3498 -0.7088 0.131 Uiso 1 1 calc R . . H5'C H 0.4084 0.2715 -0.6996 0.131 Uiso 1 1 calc R . . C6' C 0.2507(6) 0.3628(3) -0.6170(2) 0.0860(14) Uani 1 1 d . . . H6'A H 0.1666 0.3495 -0.5971 0.129 Uiso 1 1 calc R . . H6'B H 0.2340 0.3997 -0.6436 0.129 Uiso 1 1 calc R . . H6'C H 0.3407 0.3832 -0.5908 0.129 Uiso 1 1 calc R . . C7' C -0.0142(7) 0.1297(4) -0.6315(3) 0.0675(16) Uani 0.701(5) 1 d PD B 1 H7'A H 0.0354 0.1160 -0.6613 0.081 Uiso 0.701(5) 1 calc PR B 1 H7'B H -0.0660 0.0831 -0.6173 0.081 Uiso 0.701(5) 1 calc PR B 1 C7'A C -0.0413(14) 0.1514(10) -0.6053(6) 0.0675(16) Uani 0.299(5) 1 d PD B 2 H7'C H -0.0868 0.1060 -0.5879 0.081 Uiso 0.299(5) 1 calc PR B 2 H7'D H -0.0918 0.1898 -0.5961 0.081 Uiso 0.299(5) 1 calc PR B 2 C8' C -0.1388(12) 0.1701(7) -0.6593(4) 0.136(2) Uani 0.701(5) 1 d PD B 1 H8' H -0.0974 0.2243 -0.6615 0.163 Uiso 0.701(5) 1 calc PR B 1 C8A' C -0.081(3) 0.1348(12) -0.6715(8) 0.136(2) Uani 0.299(5) 1 d PD B 2 H8A' H 0.0137 0.1422 -0.6863 0.163 Uiso 0.299(5) 1 calc PR B 2 C9' C -0.2019(9) 0.1311(4) -0.7191(3) 0.136(2) Uani 1 1 d D . . H9'A H -0.1214 0.1364 -0.7408 0.204 Uiso 0.701(5) 1 calc PR B 1 H9'B H -0.2776 0.1544 -0.7377 0.204 Uiso 0.701(5) 1 calc PR B 1 H9'C H -0.2452 0.0786 -0.7156 0.204 Uiso 0.701(5) 1 calc PR B 1 H9'D H -0.2968 0.1071 -0.7084 0.204 Uiso 0.299(5) 1 calc PR B 2 H9'E H -0.1840 0.1026 -0.7500 0.204 Uiso 0.299(5) 1 calc PR B 2 H9'F H -0.2039 0.1811 -0.7302 0.204 Uiso 0.299(5) 1 calc PR B 2 C10' C -0.2595(12) 0.1550(6) -0.6241(4) 0.136(2) Uani 0.701(5) 1 d PD B 1 H10G H -0.3152 0.1035 -0.6305 0.204 Uiso 0.701(5) 1 calc PR B 1 H10H H -0.3260 0.1877 -0.6338 0.204 Uiso 0.701(5) 1 calc PR B 1 H10I H -0.2156 0.1640 -0.5853 0.204 Uiso 0.701(5) 1 calc PR B 1 C11' C 0.2018(7) 0.1023(3) -0.5345(2) 0.0869(15) Uani 1 1 d . B . H11E H 0.1152 0.0603 -0.5350 0.104 Uiso 1 1 calc R . . H11F H 0.2703 0.0854 -0.5555 0.104 Uiso 1 1 calc R . . C12' C 0.2798(8) 0.1177(4) -0.4740(2) 0.1003(18) Uani 1 1 d . . . H12' H 0.2068 0.1321 -0.4532 0.120 Uiso 1 1 calc R . . C13' C 0.3107(12) 0.0460(5) -0.4484(3) 0.167(4) Uani 1 1 d . . . H13G H 0.2204 0.0064 -0.4552 0.250 Uiso 1 1 calc R . . H13H H 0.3433 0.0549 -0.4087 0.250 Uiso 1 1 calc R . . H13I H 0.3880 0.0314 -0.4653 0.250 Uiso 1 1 calc R . . C14' C 0.4172(8) 0.1833(5) -0.4652(3) 0.124(2) Uani 1 1 d . . . H14G H 0.4871 0.1753 -0.4889 0.186 Uiso 1 1 calc R . . H14H H 0.4643 0.1872 -0.4267 0.186 Uiso 1 1 calc R . . H14I H 0.3872 0.2290 -0.4746 0.186 Uiso 1 1 calc R . . C21' C -0.0096(4) 0.3046(2) -0.44203(13) 0.0466(8) Uani 1 1 d . . . C22' C 0.0358(3) 0.3831(2) -0.43510(13) 0.0419(8) Uani 1 1 d . . . C23' C 0.1312(4) 0.4277(2) -0.46876(12) 0.0467(9) Uani 1 1 d . . . H23' H 0.1632 0.4037 -0.4971 0.056 Uiso 1 1 calc R . . C24' C 0.1790(4) 0.5044(2) -0.46178(13) 0.0450(8) Uani 1 1 d . . . C25' C 0.2824(4) 0.5487(3) -0.49410(14) 0.0548(10) Uani 1 1 d . . . H25' H 0.3196 0.5248 -0.5211 0.066 Uiso 1 1 calc R . . C26' C 0.3264(4) 0.6237(3) -0.48619(15) 0.0607(10) Uani 1 1 d . . . H26' H 0.3948 0.6511 -0.5073 0.073 Uiso 1 1 calc R . . C27' C 0.2698(4) 0.6617(2) -0.44608(14) 0.0557(9) Uani 1 1 d . . . H27' H 0.3000 0.7139 -0.4415 0.067 Uiso 1 1 calc R . . C28' C 0.1720(4) 0.6228(2) -0.41426(13) 0.0476(8) Uani 1 1 d . . . H28' H 0.1352 0.6488 -0.3884 0.057 Uiso 1 1 calc R . . C29' C 0.1246(3) 0.5429(2) -0.41962(12) 0.0425(8) Uani 1 1 d . . . C30' C 0.0295(3) 0.50027(19) -0.38629(12) 0.0387(7) Uani 1 1 d . . . H30' H -0.0062 0.5252 -0.3595 0.046 Uiso 1 1 calc R . . C31' C -0.0150(3) 0.4216(2) -0.39135(12) 0.0387(7) Uani 1 1 d . . . C32' C -0.1061(3) 0.37855(18) -0.35556(12) 0.0375(7) Uani 1 1 d . . . C33' C -0.1493(3) 0.29963(19) -0.36185(13) 0.0404(7) Uani 1 1 d . . . C34' C -0.2395(4) 0.2557(2) -0.32639(14) 0.0446(8) Uani 1 1 d . . . H34' H -0.2734 0.2801 -0.2987 0.053 Uiso 1 1 calc R . . C35' C -0.2796(4) 0.1777(2) -0.33109(15) 0.0495(8) Uani 1 1 d . . . C36' C -0.3693(4) 0.1330(2) -0.29516(17) 0.0590(10) Uani 1 1 d . . . H36' H -0.4064 0.1566 -0.2680 0.071 Uiso 1 1 calc R . . C37' C -0.4017(5) 0.0568(2) -0.2996(2) 0.0707(12) Uani 1 1 d . . . H37' H -0.4594 0.0286 -0.2754 0.085 Uiso 1 1 calc R . . C38' C -0.3469(6) 0.0200(3) -0.3416(2) 0.0837(15) Uani 1 1 d . . . H38' H -0.3687 -0.0323 -0.3443 0.100 Uiso 1 1 calc R . . C39' C -0.2642(6) 0.0599(3) -0.3773(2) 0.0781(13) Uani 1 1 d . . . H39' H -0.2309 0.0345 -0.4045 0.094 Uiso 1 1 calc R . . C40' C -0.2265(4) 0.1399(2) -0.37446(17) 0.0583(10) Uani 1 1 d . . . C41' C -0.1418(4) 0.1822(2) -0.40984(16) 0.0562(9) Uani 1 1 d . . . H41' H -0.1103 0.1572 -0.4379 0.067 Uiso 1 1 calc R . . C42' C -0.1000(4) 0.2611(2) -0.40596(14) 0.0477(8) Uani 1 1 d . . . C51' C -0.1545(3) 0.41777(17) -0.30910(12) 0.0338(6) Uani 1 1 d . . . C52' C -0.2992(3) 0.43197(18) -0.31675(13) 0.0379(7) Uani 1 1 d . . . C53' C -0.4028(4) 0.4096(2) -0.36711(14) 0.0485(8) Uani 1 1 d . . . H53' H -0.3752 0.3842 -0.3959 0.058 Uiso 1 1 calc R . . C54' C -0.5411(4) 0.4243(3) -0.37425(16) 0.0606(10) Uani 1 1 d . . . H54' H -0.6064 0.4095 -0.4078 0.073 Uiso 1 1 calc R . . C55' C -0.5864(4) 0.4618(3) -0.33122(17) 0.0615(11) Uani 1 1 d . . . H55' H -0.6816 0.4716 -0.3364 0.074 Uiso 1 1 calc R . . C56' C -0.4923(4) 0.4837(2) -0.28222(16) 0.0518(9) Uani 1 1 d . . . H56' H -0.5244 0.5081 -0.2541 0.062 Uiso 1 1 calc R . . C57' C -0.3446(3) 0.47023(18) -0.27268(13) 0.0401(7) Uani 1 1 d . . . C58' C -0.2450(4) 0.49234(18) -0.22323(14) 0.0412(7) Uani 1 1 d . . . H58' H -0.2749 0.5171 -0.1947 0.049 Uiso 1 1 calc R . . C59' C -0.1018(3) 0.47871(17) -0.21494(12) 0.0360(7) Uani 1 1 d . . . C60' C 0.0011(4) 0.50105(19) -0.16426(13) 0.0440(8) Uani 1 1 d . . . H60' H -0.0278 0.5258 -0.1355 0.053 Uiso 1 1 calc R . . C61' C 0.1396(4) 0.4872(2) -0.15695(13) 0.0475(8) Uani 1 1 d . . . H61' H 0.2053 0.5029 -0.1236 0.057 Uiso 1 1 calc R . . C62' C 0.1852(4) 0.44861(19) -0.20001(13) 0.0426(7) Uani 1 1 d . . . H62' H 0.2804 0.4388 -0.1946 0.051 Uiso 1 1 calc R . . C63' C 0.0913(3) 0.42602(18) -0.24901(12) 0.0370(7) Uani 1 1 d . . . H63' H 0.1230 0.4008 -0.2768 0.044 Uiso 1 1 calc R . . C64' C -0.0554(3) 0.44018(17) -0.25876(12) 0.0340(6) Uani 1 1 d . . . Si1' Si 0.13489(13) 0.17857(6) -0.57428(4) 0.0535(3) Uani 1 1 d 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 0.0399(18) 0.0493(19) 0.0396(18) -0.0030(14) 0.0011(15) 0.0016(14) C2 0.0344(16) 0.0463(18) 0.0374(17) -0.0035(14) 0.0009(14) 0.0040(14) C3 0.052(3) 0.060(3) 0.052(3) -0.006(3) -0.005(2) 0.011(3) C3A 0.052(3) 0.060(3) 0.052(3) -0.006(3) -0.005(2) 0.011(3) C4 0.056(5) 0.050(3) 0.081(6) 0.000(3) 0.006(4) 0.001(3) C4A 0.056(5) 0.050(3) 0.081(6) 0.000(3) 0.006(4) 0.001(3) C5 0.116(4) 0.059(3) 0.124(4) 0.004(2) -0.026(3) -0.004(2) C6 0.116(4) 0.059(3) 0.124(4) 0.004(2) -0.026(3) -0.004(2) C6A 0.116(4) 0.059(3) 0.124(4) 0.004(2) -0.026(3) -0.004(2) C7 0.044(3) 0.051(3) 0.040(3) -0.003(2) 0.002(2) 0.001(2) C7A 0.044(3) 0.051(3) 0.040(3) -0.003(2) 0.002(2) 0.001(2) C8 0.050(5) 0.059(5) 0.053(5) 0.002(4) 0.030(3) 0.004(4) C8A 0.050(5) 0.059(5) 0.053(5) 0.002(4) 0.030(3) 0.004(4) C9 0.077(3) 0.072(3) 0.119(4) 0.006(3) 0.041(3) 0.023(2) C10 0.139(15) 0.067(11) 0.053(6) -0.007(7) 0.007(7) 0.033(8) C10A 0.139(15) 0.067(11) 0.053(6) -0.007(7) 0.007(7) 0.033(8) C11 0.046(3) 0.065(3) 0.045(3) -0.001(2) 0.005(2) 0.013(3) C11A 0.046(3) 0.065(3) 0.045(3) -0.001(2) 0.005(2) 0.013(3) C12 0.048(4) 0.080(5) 0.058(3) 0.008(3) 0.017(3) 0.025(3) C12A 0.048(4) 0.080(5) 0.058(3) 0.008(3) 0.017(3) 0.025(3) C13 0.088(4) 0.111(4) 0.088(4) 0.006(3) 0.039(3) 0.031(3) C13A 0.088(4) 0.111(4) 0.088(4) 0.006(3) 0.039(3) 0.031(3) C14 0.088(4) 0.111(4) 0.088(4) 0.006(3) 0.039(3) 0.031(3) C14A 0.088(4) 0.111(4) 0.088(4) 0.006(3) 0.039(3) 0.031(3) C21 0.0300(15) 0.0474(18) 0.0309(15) -0.0095(13) 0.0011(12) 0.0073(13) C22 0.0292(15) 0.0447(17) 0.0318(15) -0.0091(13) 0.0054(12) 0.0049(13) C23 0.0289(15) 0.0509(19) 0.0349(16) -0.0067(14) 0.0061(13) 0.0037(13) C24 0.0358(17) 0.0448(18) 0.0422(18) -0.0092(14) 0.0108(14) 0.0035(14) C25 0.0425(19) 0.049(2) 0.0474(19) -0.0082(16) 0.0142(15) -0.0055(15) C26 0.054(2) 0.0437(19) 0.055(2) -0.0068(16) 0.0208(18) -0.0048(16) C27 0.061(2) 0.046(2) 0.053(2) 0.0050(16) 0.0191(18) 0.0070(17) C28 0.0470(19) 0.0458(19) 0.0468(19) 0.0000(15) 0.0093(16) 0.0047(15) C29 0.0378(17) 0.0428(17) 0.0405(17) -0.0037(14) 0.0116(14) 0.0061(14) C30 0.0326(16) 0.0425(17) 0.0351(16) -0.0050(13) 0.0046(13) 0.0061(13) C31 0.0281(15) 0.0413(16) 0.0306(15) -0.0066(12) 0.0066(12) 0.0064(12) C32 0.0268(14) 0.0407(16) 0.0269(14) -0.0055(12) 0.0070(12) 0.0071(12) C33 0.0276(14) 0.0434(16) 0.0275(14) -0.0060(12) 0.0053(12) 0.0079(12) C34 0.0296(15) 0.0419(16) 0.0304(15) -0.0044(12) 0.0025(12) 0.0054(12) C35 0.0340(16) 0.0432(17) 0.0314(15) -0.0032(13) 0.0061(13) 0.0082(13) C36 0.0375(17) 0.0447(18) 0.0383(17) 0.0006(14) 0.0032(14) 0.0042(14) C37 0.053(2) 0.0448(19) 0.049(2) 0.0037(15) 0.0072(16) 0.0060(16) C38 0.062(2) 0.056(2) 0.047(2) 0.0127(16) 0.0018(17) 0.0179(18) C39 0.047(2) 0.059(2) 0.0432(19) 0.0021(16) -0.0044(15) 0.0121(17) C40 0.0377(17) 0.0480(18) 0.0334(16) -0.0014(13) 0.0033(13) 0.0109(14) C41 0.0352(16) 0.0537(19) 0.0304(15) -0.0021(14) -0.0011(13) 0.0113(14) C42 0.0274(15) 0.0481(18) 0.0269(14) -0.0053(12) 0.0036(12) 0.0074(13) C51 0.0285(14) 0.0332(15) 0.0291(14) -0.0013(11) 0.0045(12) 0.0035(11) C52 0.0305(15) 0.0340(15) 0.0297(15) -0.0013(12) 0.0046(12) 0.0030(12) C53 0.0302(15) 0.0467(18) 0.0357(16) -0.0051(13) 0.0049(13) 0.0065(13) C54 0.0384(18) 0.061(2) 0.0426(18) -0.0064(15) 0.0105(15) 0.0137(15) C55 0.056(2) 0.063(2) 0.0310(17) -0.0107(15) 0.0093(15) 0.0154(17) C56 0.0462(19) 0.054(2) 0.0283(16) -0.0055(14) -0.0009(14) 0.0095(15) C57 0.0372(16) 0.0384(16) 0.0279(15) 0.0002(12) 0.0033(12) 0.0050(13) C58 0.0334(16) 0.0429(17) 0.0317(15) 0.0019(13) -0.0019(12) 0.0068(13) C59 0.0286(15) 0.0382(16) 0.0366(16) 0.0021(13) 0.0027(12) 0.0058(12) C60 0.0306(16) 0.054(2) 0.0484(19) -0.0008(15) 0.0005(14) 0.0090(14) C61 0.0325(17) 0.065(2) 0.058(2) -0.0032(17) 0.0118(16) 0.0149(16) C62 0.0410(19) 0.060(2) 0.0480(19) -0.0103(16) 0.0117(15) 0.0138(16) C63 0.0352(17) 0.0482(18) 0.0375(17) -0.0058(14) 0.0054(13) 0.0066(14) C64 0.0300(15) 0.0341(15) 0.0340(15) 0.0001(12) 0.0068(12) 0.0037(12) Si1 0.0350(5) 0.0487(5) 0.0339(5) -0.0054(4) -0.0023(4) 0.0039(4) C1" 0.133(4) 0.135(4) 0.107(4) -0.005(3) -0.035(3) 0.002(3) C1' 0.082(3) 0.069(3) 0.052(2) 0.0053(19) 0.023(2) 0.039(2) C2' 0.066(2) 0.071(2) 0.043(2) -0.0019(17) 0.0117(18) 0.039(2) C3' 0.078(3) 0.086(3) 0.058(2) 0.003(2) 0.017(2) 0.027(2) C4' 0.058(2) 0.092(3) 0.052(2) 0.015(2) 0.0088(19) 0.021(2) C5' 0.073(3) 0.121(4) 0.072(3) 0.024(3) 0.027(3) 0.023(3) C6' 0.092(4) 0.096(4) 0.082(3) 0.016(3) 0.034(3) 0.033(3) C7' 0.063(3) 0.077(4) 0.053(4) -0.012(3) 0.018(3) -0.007(3) C7'A 0.063(3) 0.077(4) 0.053(4) -0.012(3) 0.018(3) -0.007(3) C8' 0.133(4) 0.135(4) 0.107(4) -0.005(3) -0.035(3) 0.002(3) C8A' 0.133(4) 0.135(4) 0.107(4) -0.005(3) -0.035(3) 0.002(3) C9' 0.133(4) 0.135(4) 0.107(4) -0.005(3) -0.035(3) 0.002(3) C10' 0.133(4) 0.135(4) 0.107(4) -0.005(3) -0.035(3) 0.002(3) C11' 0.133(5) 0.065(3) 0.077(3) -0.006(2) 0.037(3) 0.039(3) C12' 0.127(5) 0.115(5) 0.078(3) 0.021(3) 0.020(3) 0.066(4) C13' 0.234(10) 0.175(8) 0.130(6) 0.075(6) 0.043(7) 0.113(8) C14' 0.111(5) 0.157(7) 0.096(4) 0.020(4) -0.011(4) 0.032(5) C21' 0.0391(18) 0.074(2) 0.0337(17) -0.0041(16) 0.0052(14) 0.0289(17) C22' 0.0312(16) 0.067(2) 0.0313(16) -0.0078(15) -0.0011(13) 0.0234(15) C23' 0.0335(17) 0.090(3) 0.0233(15) -0.0002(16) 0.0045(13) 0.0285(17) C24' 0.0329(17) 0.072(2) 0.0297(16) -0.0021(15) -0.0030(13) 0.0168(16) C25' 0.0386(19) 0.100(3) 0.0276(16) 0.0052(18) 0.0092(14) 0.0175(19) C26' 0.050(2) 0.086(3) 0.0374(19) 0.0044(19) 0.0056(16) 0.001(2) C27' 0.049(2) 0.075(3) 0.0346(18) 0.0034(17) 0.0016(16) 0.0023(18) C28' 0.0391(18) 0.067(2) 0.0324(17) -0.0016(15) -0.0014(14) 0.0088(16) C29' 0.0258(15) 0.075(2) 0.0261(15) 0.0002(15) -0.0034(12) 0.0162(15) C30' 0.0255(15) 0.061(2) 0.0296(15) -0.0045(14) 0.0014(12) 0.0126(14) C31' 0.0242(14) 0.068(2) 0.0263(15) -0.0030(14) -0.0006(12) 0.0186(14) C32' 0.0261(15) 0.0545(19) 0.0326(16) -0.0088(14) -0.0008(12) 0.0148(13) C33' 0.0275(15) 0.060(2) 0.0353(16) -0.0071(14) 0.0011(13) 0.0169(14) C34' 0.0350(17) 0.055(2) 0.0442(18) -0.0120(15) 0.0024(14) 0.0144(15) C35' 0.0378(18) 0.058(2) 0.050(2) -0.0075(16) 0.0002(15) 0.0104(16) C36' 0.052(2) 0.057(2) 0.063(2) -0.0088(18) -0.0017(18) 0.0111(18) C37' 0.066(3) 0.059(3) 0.080(3) -0.002(2) 0.007(2) 0.003(2) C38' 0.093(4) 0.051(2) 0.102(4) -0.019(3) 0.003(3) 0.016(2) C39' 0.087(3) 0.064(3) 0.084(3) -0.015(2) 0.018(3) 0.018(2) C40' 0.056(2) 0.054(2) 0.064(2) -0.0187(18) -0.0026(19) 0.0196(18) C41' 0.055(2) 0.068(2) 0.050(2) -0.0146(18) 0.0108(18) 0.0241(19) C42' 0.0418(18) 0.061(2) 0.0433(18) -0.0144(16) -0.0020(15) 0.0248(16) C51' 0.0275(15) 0.0443(17) 0.0327(15) -0.0007(12) 0.0103(12) 0.0111(12) C52' 0.0312(16) 0.0512(18) 0.0361(16) 0.0062(13) 0.0122(13) 0.0146(13) C53' 0.0357(18) 0.075(2) 0.0384(18) 0.0013(16) 0.0058(14) 0.0211(16) C54' 0.0368(19) 0.098(3) 0.052(2) 0.011(2) 0.0051(16) 0.0272(19) C55' 0.0378(19) 0.090(3) 0.069(3) 0.021(2) 0.0182(19) 0.0336(19) C56' 0.044(2) 0.064(2) 0.061(2) 0.0130(18) 0.0281(18) 0.0270(17) C57' 0.0351(16) 0.0486(18) 0.0435(18) 0.0094(14) 0.0201(14) 0.0144(14) C58' 0.0453(18) 0.0428(17) 0.0422(18) 0.0006(14) 0.0255(15) 0.0123(14) C59' 0.0391(17) 0.0395(16) 0.0308(15) -0.0006(12) 0.0139(13) 0.0070(13) C60' 0.050(2) 0.0496(19) 0.0310(16) -0.0071(14) 0.0142(14) 0.0056(15) C61' 0.049(2) 0.057(2) 0.0305(16) -0.0050(14) 0.0024(14) 0.0031(16) C62' 0.0322(16) 0.057(2) 0.0365(17) 0.0001(14) 0.0027(13) 0.0084(14) C63' 0.0318(16) 0.0477(18) 0.0325(15) -0.0030(13) 0.0062(13) 0.0107(13) C64' 0.0322(15) 0.0397(16) 0.0311(15) 0.0004(12) 0.0104(12) 0.0075(12) Si1' 0.0673(7) 0.0546(6) 0.0398(5) -0.0084(4) 0.0151(5) 0.0130(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.210(4) . ? C1 Si1 1.842(3) . ? C2 C21 1.436(4) . ? C3 C4 1.533(10) . ? C3 Si1 1.872(6) . ? C3A C4A 1.519(12) . ? C3A Si1 1.886(9) . ? C4 C5 1.519(9) . ? C4 C6 1.530(11) . ? C4A C5 1.499(11) . ? C4A C6A 1.517(14) . ? C7 C8 1.521(9) . ? C7 Si1 1.855(6) . ? C7A C8A 1.517(11) . ? C7A Si1 1.889(8) . ? C8 C9 1.562(11) . ? C8 C10 1.520(11) . ? C8A C10A 1.512(14) . ? C11 C12 1.536(8) . ? C11 Si1 1.892(6) . ? C11A C12A 1.528(12) . ? C11A Si1 1.834(8) . ? C12 C13 1.547(10) . ? C12 C14 1.509(10) . ? C12A C13A 1.514(11) . ? C12A C14A 1.554(12) . ? C21 C22 1.405(5) . ? C21 C42 1.426(4) . ? C22 C23 1.397(4) . ? C22 C31 1.456(4) . ? C23 C24 1.383(5) . ? C24 C25 1.431(5) . ? C24 C29 1.447(4) . ? C25 C26 1.358(5) . ? C26 C27 1.424(5) . ? C27 C28 1.352(5) . ? C28 C29 1.431(5) . ? C29 C30 1.385(4) . ? C30 C31 1.408(4) . ? C31 C32 1.401(4) . ? C32 C33 1.408(4) . ? C32 C51 1.502(4) . ? C33 C34 1.407(4) . ? C33 C42 1.449(4) . ? C34 C35 1.390(4) . ? C35 C36 1.427(4) . ? C35 C40 1.437(4) . ? C36 C37 1.354(5) . ? C37 C38 1.426(5) . ? C38 C39 1.354(5) . ? C39 C40 1.422(5) . ? C40 C41 1.391(5) . ? C41 C42 1.404(4) . ? C51 C52 1.402(4) . ? C51 C64 1.412(4) . ? C52 C53 1.433(4) . ? C52 C57 1.434(4) . ? C53 C54 1.346(4) . ? C54 C55 1.423(5) . ? C55 C56 1.353(5) . ? C56 C57 1.423(4) . ? C57 C58 1.395(4) . ? C58 C59 1.390(4) . ? C59 C60 1.432(4) . ? C59 C64 1.431(4) . ? C60 C61 1.344(5) . ? C61 C62 1.422(5) . ? C62 C63 1.360(5) . ? C63 C64 1.423(4) . ? C1" C8A' 1.484(16) . ? C1' C2' 1.200(5) . ? C1' Si1' 1.822(4) . ? C2' C21' 1.439(5) . ? C3' C4' 1.517(6) . ? C3' Si1' 1.859(5) . ? C4' C5' 1.502(6) . ? C4' C6' 1.523(7) . ? C7' C8' 1.582(11) . ? C7' Si1' 1.852(6) . ? C7'A C8A' 1.593(17) . ? C7'A Si1' 1.646(12) . ? C8' C9' 1.568(10) . ? C8' C10' 1.482(12) . ? C8A' C9' 1.466(14) . ? C11' C12' 1.520(8) . ? C11' Si1' 1.872(5) . ? C12' C13' 1.524(9) . ? C12' C14' 1.517(9) . ? C21' C22' 1.399(5) . ? C21' C42' 1.420(5) . ? C22' C23' 1.414(5) . ? C22' C31' 1.456(4) . ? C23' C24' 1.368(5) . ? C24' C25' 1.435(5) . ? C24' C29' 1.445(5) . ? C25' C26' 1.339(6) . ? C26' C27' 1.416(6) . ? C27' C28' 1.355(5) . ? C28' C29' 1.423(5) . ? C29' C30' 1.392(5) . ? C30' C31' 1.399(5) . ? C31' C32' 1.415(5) . ? C32' C33' 1.405(5) . ? C32' C51' 1.502(4) . ? C33' C34' 1.412(5) . ? C33' C42' 1.456(4) . ? C34' C35' 1.386(5) . ? C35' C36' 1.424(6) . ? C35' C40' 1.454(5) . ? C36' C37' 1.353(6) . ? C37' C38' 1.428(7) . ? C38' C39' 1.347(7) . ? C39' C40' 1.421(6) . ? C40' C41' 1.369(6) . ? C41' C42' 1.402(5) . ? C51' C52' 1.408(4) . ? C51' C64' 1.401(4) . ? C52' C53' 1.420(5) . ? C52' C57' 1.433(4) . ? C53' C54' 1.355(5) . ? C54' C55' 1.405(6) . ? C55' C56' 1.353(6) . ? C56' C57' 1.431(5) . ? C57' C58' 1.385(5) . ? C58' C59' 1.390(4) . ? C59' C60' 1.423(4) . ? C59' C64' 1.436(4) . ? C60' C61' 1.351(5) . ? C61' C62' 1.418(5) . ? C62' C63' 1.354(4) . ? C63' C64' 1.426(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Si1 176.7(3) . . ? C1 C2 C21 178.8(4) . . ? C4 C3 Si1 119.3(5) . . ? C4A C3A Si1 119.2(7) . . ? C5 C4 C3 112.4(6) . . ? C5 C4 C6 113.6(7) . . ? C6 C4 C3 110.1(7) . . ? C5 C4A C3A 116.1(8) . . ? C5 C4A C6A 103.1(9) . . ? C6A C4A C3A 112.0(10) . . ? C4A C5 C4 27.4(5) . . ? C8 C7 Si1 119.7(5) . . ? C8A C7A Si1 121.2(8) . . ? C7 C8 C9 110.0(6) . . ? C10 C8 C7 112.9(15) . . ? C10 C8 C9 111.0(15) . . ? C10A C8A C7A 111.7(19) . . ? C12 C11 Si1 118.9(5) . . ? C12A C11A Si1 118.2(6) . . ? C11 C12 C13 111.0(6) . . ? C14 C12 C11 110.9(6) . . ? C14 C12 C13 106.3(7) . . ? C11A C12A C14A 113.6(9) . . ? C13A C12A C11A 113.7(9) . . ? C13A C12A C14A 106.8(9) . . ? C22 C21 C2 119.5(3) . . ? C22 C21 C42 121.2(3) . . ? C42 C21 C2 119.3(3) . . ? C21 C22 C31 119.3(3) . . ? C23 C22 C21 122.3(3) . . ? C23 C22 C31 118.5(3) . . ? C24 C23 C22 122.7(3) . . ? C23 C24 C25 122.5(3) . . ? C23 C24 C29 119.2(3) . . ? C25 C24 C29 118.2(3) . . ? C26 C25 C24 120.7(3) . . ? C25 C26 C27 121.0(3) . . ? C28 C27 C26 120.4(3) . . ? C27 C28 C29 121.0(3) . . ? C28 C29 C24 118.6(3) . . ? C30 C29 C24 118.7(3) . . ? C30 C29 C28 122.6(3) . . ? C29 C30 C31 122.6(3) . . ? C30 C31 C22 118.2(3) . . ? C32 C31 C22 119.5(3) . . ? C32 C31 C30 122.2(3) . . ? C31 C32 C33 121.5(3) . . ? C31 C32 C51 118.9(3) . . ? C33 C32 C51 119.6(2) . . ? C32 C33 C42 119.6(3) . . ? C34 C33 C32 122.6(3) . . ? C34 C33 C42 117.8(3) . . ? C35 C34 C33 122.7(3) . . ? C34 C35 C36 122.6(3) . . ? C34 C35 C40 119.1(3) . . ? C36 C35 C40 118.4(3) . . ? C37 C36 C35 121.4(3) . . ? C36 C37 C38 120.2(3) . . ? C39 C38 C37 120.0(3) . . ? C38 C39 C40 121.8(3) . . ? C39 C40 C35 118.1(3) . . ? C41 C40 C35 119.2(3) . . ? C41 C40 C39 122.7(3) . . ? C40 C41 C42 122.1(3) . . ? C21 C42 C33 118.9(3) . . ? C41 C42 C21 122.1(3) . . ? C41 C42 C33 119.1(3) . . ? C52 C51 C32 119.3(2) . . ? C52 C51 C64 120.3(3) . . ? C64 C51 C32 120.3(2) . . ? C51 C52 C53 122.2(3) . . ? C51 C52 C57 119.9(3) . . ? C53 C52 C57 117.9(3) . . ? C54 C53 C52 121.0(3) . . ? C53 C54 C55 121.3(3) . . ? C56 C55 C54 119.4(3) . . ? C55 C56 C57 121.7(3) . . ? C56 C57 C52 118.7(3) . . ? C58 C57 C52 119.1(3) . . ? C58 C57 C56 122.2(3) . . ? C59 C58 C57 121.6(3) . . ? C58 C59 C60 122.1(3) . . ? C58 C59 C64 119.6(3) . . ? C64 C59 C60 118.3(3) . . ? C61 C60 C59 121.5(3) . . ? C60 C61 C62 120.5(3) . . ? C63 C62 C61 120.1(3) . . ? C62 C63 C64 121.5(3) . . ? C51 C64 C59 119.4(3) . . ? C51 C64 C63 122.3(3) . . ? C63 C64 C59 118.2(3) . . ? C1 Si1 C3 110.6(2) . . ? C1 Si1 C3A 111.1(3) . . ? C1 Si1 C7 109.5(2) . . ? C1 Si1 C7A 109.5(3) . . ? C1 Si1 C11 107.4(2) . . ? C3 Si1 C3A 36.2(3) . . ? C3 Si1 C7A 133.6(3) . . ? C3 Si1 C11 111.9(3) . . ? C3A Si1 C7A 106.5(4) . . ? C3A Si1 C11 137.3(3) . . ? C7 Si1 C3 108.1(3) . . ? C7 Si1 C3A 74.3(3) . . ? C7 Si1 C7A 35.1(3) . . ? C7 Si1 C11 109.4(3) . . ? C7A Si1 C11 76.4(3) . . ? C11A Si1 C1 111.0(3) . . ? C11A Si1 C3 75.6(3) . . ? C11A Si1 C3A 108.4(4) . . ? C11A Si1 C7 134.6(3) . . ? C11A Si1 C7A 110.2(4) . . ? C11A Si1 C11 38.3(3) . . ? C2' C1' Si1' 174.3(4) . . ? C1' C2' C21' 179.5(5) . . ? C4' C3' Si1' 119.8(3) . . ? C3' C4' C6' 110.8(4) . . ? C5' C4' C3' 112.0(4) . . ? C5' C4' C6' 108.7(4) . . ? C8' C7' Si1' 120.3(5) . . ? C8A' C7'A Si1' 120.8(12) . . ? C9' C8' C7' 106.8(7) . . ? C10' C8' C7' 106.3(9) . . ? C10' C8' C9' 109.3(8) . . ? C1" C8A' C7'A 90.9(14) . . ? C9' C8A' C1" 90.8(14) . . ? C9' C8A' C7'A 142(2) . . ? C8A' C9' C8' 38.1(11) . . ? C12' C11' Si1' 120.2(3) . . ? C11' C12' C13' 111.0(6) . . ? C14' C12' C11' 114.4(5) . . ? C14' C12' C13' 113.0(7) . . ? C22' C21' C2' 120.0(3) . . ? C22' C21' C42' 121.4(3) . . ? C42' C21' C2' 118.6(3) . . ? C21' C22' C23' 122.7(3) . . ? C21' C22' C31' 119.6(3) . . ? C23' C22' C31' 117.7(3) . . ? C24' C23' C22' 123.4(3) . . ? C23' C24' C25' 123.0(3) . . ? C23' C24' C29' 118.9(3) . . ? C25' C24' C29' 118.1(3) . . ? C26' C25' C24' 121.3(4) . . ? C25' C26' C27' 120.6(4) . . ? C28' C27' C26' 120.6(4) . . ? C27' C28' C29' 121.3(3) . . ? C28' C29' C24' 117.9(3) . . ? C30' C29' C24' 118.7(3) . . ? C30' C29' C28' 123.3(3) . . ? C29' C30' C31' 122.9(3) . . ? C30' C31' C22' 118.2(3) . . ? C30' C31' C32' 122.5(3) . . ? C32' C31' C22' 119.2(3) . . ? C31' C32' C51' 119.5(3) . . ? C33' C32' C31' 121.2(3) . . ? C33' C32' C51' 119.3(3) . . ? C32' C33' C34' 122.0(3) . . ? C32' C33' C42' 119.7(3) . . ? C34' C33' C42' 118.3(3) . . ? C35' C34' C33' 122.7(3) . . ? C34' C35' C36' 123.1(3) . . ? C34' C35' C40' 118.4(3) . . ? C36' C35' C40' 118.5(3) . . ? C37' C36' C35' 121.5(4) . . ? C36' C37' C38' 119.7(4) . . ? C39' C38' C37' 120.9(4) . . ? C38' C39' C40' 121.8(4) . . ? C39' C40' C35' 117.5(4) . . ? C41' C40' C35' 119.3(3) . . ? C41' C40' C39' 123.2(4) . . ? C40' C41' C42' 123.3(3) . . ? C21' C42' C33' 118.9(3) . . ? C41' C42' C21' 123.2(3) . . ? C41' C42' C33' 118.0(3) . . ? C52' C51' C32' 119.6(3) . . ? C64' C51' C32' 119.8(2) . . ? C64' C51' C52' 120.6(3) . . ? C51' C52' C53' 122.1(3) . . ? C51' C52' C57' 119.5(3) . . ? C53' C52' C57' 118.4(3) . . ? C54' C53' C52' 121.5(3) . . ? C53' C54' C55' 120.4(4) . . ? C56' C55' C54' 120.4(3) . . ? C55' C56' C57' 121.5(3) . . ? C56' C57' C52' 117.7(3) . . ? C58' C57' C52' 119.2(3) . . ? C58' C57' C56' 123.1(3) . . ? C57' C58' C59' 122.1(3) . . ? C58' C59' C60' 122.5(3) . . ? C58' C59' C64' 119.2(3) . . ? C60' C59' C64' 118.3(3) . . ? C61' C60' C59' 121.6(3) . . ? C60' C61' C62' 120.2(3) . . ? C63' C62' C61' 120.5(3) . . ? C62' C63' C64' 121.2(3) . . ? C51' C64' C59' 119.4(3) . . ? C51' C64' C63' 122.4(3) . . ? C63' C64' C59' 118.2(3) . . ? C1' Si1' C3' 113.4(2) . . ? C1' Si1' C7' 115.5(3) . . ? C1' Si1' C11' 106.00(19) . . ? C3' Si1' C11' 107.8(2) . . ? C7' Si1' C3' 107.9(3) . . ? C7' Si1' C11' 105.7(3) . . ? C7'A Si1' C1' 88.6(6) . . ? C7'A Si1' C3' 125.5(6) . . ? C7'A Si1' C7' 27.1(5) . . ? C7'A Si1' C11' 112.8(6) . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -5 2 10 0.1737 -5.0000 2.0000 10.0000 -0.0369 -0.0206 -0.9796 1 0 15 0.0895 1.0000 -0.0000 15.0000 -0.0864 0.9251 -0.4006 6 -3 -3 0.1625 6.0000 -3.0000 -3.0000 -0.0747 0.5003 0.8625 5 -3 -10 0.1770 5.0000 -3.0000 -10.0000 -0.0485 0.0058 0.9830 -1 0 -15 0.0762 -1.0000 0.0000 -15.0000 0.0864 -0.9251 0.4006 6 -3 -4 0.1643 6.0000 -3.0000 -4.0000 -0.0672 0.4465 0.8975 6 -1 -5 0.1598 6.0000 -1.0000 -5.0000 0.1111 0.4224 0.9258 -6 1 5 0.1598 -6.0000 1.0000 5.0000 -0.1111 -0.4224 -0.9258 1 3 14 0.0810 1.0000 3.0000 14.0000 0.1773 0.9159 -0.3756 -1 -3 -14 0.0810 -1.0000 -3.0000 -14.0000 -0.1773 -0.9159 0.3756 0 -12 2 0.0311 -0.0000 -12.0000 2.0000 -1.0398 -0.0706 -0.0298 0 12 -2 0.0311 0.0000 12.0000 -2.0000 1.0398 0.0706 0.0298 5 -8 2 0.1414 5.0000 -8.0000 2.0000 -0.5658 0.5774 0.5796 -5 8 -2 0.1414 -5.0000 8.0000 -2.0000 0.5658 -0.5774 -0.5796 0 -11 -6 0.0557 -0.0000 -11.0000 -6.0000 -0.8942 -0.4864 0.2470 0 11 6 0.0557 0.0000 11.0000 6.0000 0.8942 0.4864 -0.2470 _database_code_depnum_ccdc_archive 'CCDC 927706' ####################################################################### # # 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_global #------------------------------------------------------------------------- #3 Publication details # Provide these details if the structure has been published, # accepted or submitted for publication # The CCDC journal deposition number, eg. 182/357, # should be included only if it has been assigned by the journal _ccdc_comments ? _ccdc_journal_depnumber ? #------------------------------------------------------------------------- #4 Chemical and physical data # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag include any ASCII file output by a chemical drawing # package # Against _type record, for example, ChemDraw # Against _records supply the chemical connectivity records _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H41 F Si' _chemical_formula_weight 652.89 _chemical_melting_point ? _ccdc_compound_id ? _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ? _exptl_crystal_density_diffrn ? _exptl_crystal_colour violet #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # Record the radiation type if not X-rays, eg. neutron # Record the temperature of the data collection (Kelvin) # if not room-temperature # Record R_squared if this is the only reliability factor given by # your refinement program # Describe briefly any disorder, eg. t-Butyl C31-33 disordered over # two sites with occupancies 0.6 and 0.4 # Under ccdc_comments record any other important information _diffrn_radiation_type Cu-Ka _diffrn_measurement_device 'Agilent SuperNova' _ccdc_temp_data_collection 173(2) _ccdc_ls_R_squared ? _refine_ls_abs_structure_details ? _ccdc_disorder ? #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # Do not include structure factors data_see02 _audit_creation_date 2012-08-20 _audit_creation_method ; Olex2 1.2 (compiled 2012.05.09 svn.r2324, GUI svn.r4230) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C47 H41 F Si' _chemical_formula_sum 'C47 H41 F Si' _chemical_formula_weight 652.89 _chemical_melting_point ? _chemical_oxdiff_formula 'C47 H41F Si' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 12.5164(9) _cell_length_b 12.9102(10) _cell_length_c 13.3024(11) _cell_angle_alpha 85.827(7) _cell_angle_beta 62.967(8) _cell_angle_gamma 72.234(7) _cell_volume 1817.9(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3182 _cell_measurement_temperature 173.0(2) _cell_measurement_theta_max 70.7482 _cell_measurement_theta_min 3.6030 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92035 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark violet' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 692 _exptl_crystal_recrystallization_method 'crystallized from DCM/MeOH' _exptl_crystal_size_max 0.2224 _exptl_crystal_size_mid 0.1398 _exptl_crystal_size_min 0.0623 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_unetI/netI 0.0411 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10315 _diffrn_reflns_theta_full 70.88 _diffrn_reflns_theta_max 70.88 _diffrn_reflns_theta_min 3.61 _diffrn_ambient_temperature 173.0(2) _diffrn_detector_area_resol_mean 10.6144 _diffrn_measured_fraction_theta_full 0.950 _diffrn_measured_fraction_theta_max 0.950 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 41.00 93.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 -90.0000 52 #__ type_ start__ end____ width___ exp.time_ 2 omega -8.00 33.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 -90.0000 41 #__ type_ start__ end____ width___ exp.time_ 3 omega -43.00 -14.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 -90.0000 29 #__ type_ start__ end____ width___ exp.time_ 4 omega -144.00 39.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -55.4492 -19.0000 -150.0000 183 #__ type_ start__ end____ width___ exp.time_ 5 omega -150.00 -99.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -55.4492 -99.0000 -60.0000 51 #__ type_ start__ end____ width___ exp.time_ 6 omega 95.00 150.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 55.4492 143.0000 -66.0000 55 #__ type_ start__ end____ width___ exp.time_ 7 omega 111.00 148.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 55.4492 125.0000 30.0000 37 #__ type_ start__ end____ width___ exp.time_ 8 omega 97.00 131.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 55.4492 125.0000 -30.0000 34 #__ type_ start__ end____ width___ exp.time_ 9 omega -97.00 -28.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -70.5000 128.0000 -48.0000 69 #__ type_ start__ end____ width___ exp.time_ 10 omega -50.00 18.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -70.5000 38.0000 -180.0000 68 #__ type_ start__ end____ width___ exp.time_ 11 omega 5.00 172.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 110.8984 12.0000 60.0000 167 #__ type_ start__ end____ width___ exp.time_ 12 omega 99.00 153.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 110.8984 63.0000 60.0000 54 #__ type_ start__ end____ width___ exp.time_ 13 omega 21.00 100.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 110.8984 -50.0000 0.0000 79 #__ type_ start__ end____ width___ exp.time_ 14 omega 70.00 155.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 110.8984 -91.0000 0.0000 85 #__ type_ start__ end____ width___ exp.time_ 15 omega 17.00 94.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 110.8984 -25.0000 60.0000 77 #__ type_ start__ end____ width___ exp.time_ 16 omega 13.00 147.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 110.8984 -91.0000 -120.0000 134 #__ type_ start__ end____ width___ exp.time_ 17 omega 32.00 58.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 110.8984 -91.0000 0.0000 26 #__ type_ start__ end____ width___ exp.time_ 18 omega 18.00 91.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 110.8984 -50.0000 -120.0000 73 #__ type_ start__ end____ width___ exp.time_ 19 omega 34.00 128.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 110.8984 -143.0000 -113.0000 94 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0682985000 _diffrn_orient_matrix_UB_12 -0.0090340000 _diffrn_orient_matrix_UB_13 0.1286000000 _diffrn_orient_matrix_UB_21 -0.0555614000 _diffrn_orient_matrix_UB_22 0.1251905000 _diffrn_orient_matrix_UB_23 0.0189045000 _diffrn_orient_matrix_UB_31 -0.1154029000 _diffrn_orient_matrix_UB_32 -0.0065156000 _diffrn_orient_matrix_UB_33 -0.0105522000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4721 _reflns_number_total 6670 _reflns_odcompleteness_completeness 97.81 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.368 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.044 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 448 _refine_ls_number_reflns 6670 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0531 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+0.7955P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1345 _refine_ls_wR_factor_ref 0.1504 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.4993(2) 0.2434(2) 0.5162(2) 0.0397(6) Uani 1 1 d . . . C2 C 0.4528(2) 0.24035(19) 0.61746(19) 0.0364(5) Uani 1 1 d . . . C3 C 0.7038(3) 0.3005(2) 0.3169(2) 0.0526(7) Uani 1 1 d . . . H3 H 0.6852 0.3545 0.3774 0.063 Uiso 1 1 calc R . . C4 C 0.8129(3) 0.2028(3) 0.3135(3) 0.0776(10) Uani 1 1 d . . . H4A H 0.7860 0.1704 0.3865 0.116 Uiso 1 1 calc R . . H4B H 0.8851 0.2275 0.2986 0.116 Uiso 1 1 calc R . . H4C H 0.8372 0.1482 0.2534 0.116 Uiso 1 1 calc R . . C5 C 0.7427(3) 0.3572(3) 0.2077(3) 0.0694(9) Uani 1 1 d . . . H5A H 0.7590 0.3086 0.1457 0.104 Uiso 1 1 calc R . . H5B H 0.8194 0.3754 0.1908 0.104 Uiso 1 1 calc R . . H5C H 0.6749 0.4241 0.2161 0.104 Uiso 1 1 calc R . . C6 C 0.5834(3) 0.1280(2) 0.2929(2) 0.0457(6) Uani 1 1 d . . . H6 H 0.6648 0.0783 0.2879 0.055 Uiso 1 1 calc R . . C7 C 0.4836(3) 0.0720(2) 0.3618(3) 0.0581(8) Uani 1 1 d . . . H7A H 0.4789 0.0616 0.4373 0.087 Uiso 1 1 calc R . . H7B H 0.5064 0.0010 0.3234 0.087 Uiso 1 1 calc R . . H7C H 0.4016 0.1176 0.3690 0.087 Uiso 1 1 calc R . . C8 C 0.6003(3) 0.1354(3) 0.1717(2) 0.0670(9) Uani 1 1 d . . . H8A H 0.5194 0.1749 0.1727 0.100 Uiso 1 1 calc R . . H8B H 0.6308 0.0617 0.1355 0.100 Uiso 1 1 calc R . . H8C H 0.6617 0.1742 0.1291 0.100 Uiso 1 1 calc R . . C9 C 0.4288(2) 0.3795(2) 0.3526(2) 0.0418(6) Uani 1 1 d . . . H9 H 0.4640 0.4012 0.2730 0.050 Uiso 1 1 calc R . . C10 C 0.3977(3) 0.4779(2) 0.4306(2) 0.0495(7) Uani 1 1 d . . . H10A H 0.3669 0.4582 0.5092 0.074 Uiso 1 1 calc R . . H10B H 0.3326 0.5392 0.4239 0.074 Uiso 1 1 calc R . . H10C H 0.4738 0.4990 0.4085 0.074 Uiso 1 1 calc R . . C11 C 0.3084(3) 0.3532(2) 0.3771(3) 0.0565(7) Uani 1 1 d . . . H11A H 0.3282 0.2949 0.3224 0.085 Uiso 1 1 calc R . . H11B H 0.2471 0.4186 0.3707 0.085 Uiso 1 1 calc R . . H11C H 0.2727 0.3294 0.4539 0.085 Uiso 1 1 calc R . . C12 C 0.1040(2) 0.35395(19) 1.16390(19) 0.0343(5) Uani 1 1 d . . . C21 C 0.2667(2) 0.24786(17) 0.97880(18) 0.0320(5) Uani 1 1 d . . . C22 C 0.3787(2) 0.27725(17) 0.92415(18) 0.0320(5) Uani 1 1 d . . . C23 C 0.4308(2) 0.31217(19) 0.98519(19) 0.0360(5) Uani 1 1 d . . . H23 H 0.3874 0.3185 1.0656 0.043 Uiso 1 1 calc R . . C24 C 0.5431(2) 0.33748(19) 0.9317(2) 0.0365(5) Uani 1 1 d . . . C25 C 0.5958(3) 0.3735(2) 0.9927(2) 0.0463(6) Uani 1 1 d . . . H25 H 0.5525 0.3817 1.0731 0.056 Uiso 1 1 calc R . . C26 C 0.7060(3) 0.3962(2) 0.9382(2) 0.0520(7) Uani 1 1 d . . . H26 H 0.7388 0.4207 0.9807 0.062 Uiso 1 1 calc R . . C27 C 0.7738(3) 0.3840(3) 0.8181(3) 0.0559(7) Uani 1 1 d . . . H27 H 0.8520 0.3990 0.7811 0.067 Uiso 1 1 calc R . . C28 C 0.7274(3) 0.3509(2) 0.7559(2) 0.0489(7) Uani 1 1 d . . . H28 H 0.7737 0.3428 0.6757 0.059 Uiso 1 1 calc R . . C29 C 0.6094(2) 0.32801(19) 0.8097(2) 0.0377(5) Uani 1 1 d . . . C30 C 0.5579(2) 0.29726(19) 0.7488(2) 0.0363(5) Uani 1 1 d . . . H30 H 0.6007 0.2933 0.6685 0.044 Uiso 1 1 calc R . . C31 C 0.4443(2) 0.27162(17) 0.80187(18) 0.0325(5) Uani 1 1 d . . . C32 C 0.3937(2) 0.23896(18) 0.73797(19) 0.0337(5) Uani 1 1 d . . . C33 C 0.2828(2) 0.20822(17) 0.79225(19) 0.0331(5) Uani 1 1 d . . . C34 C 0.2321(2) 0.17396(19) 0.7298(2) 0.0382(5) Uani 1 1 d . . . H34 H 0.2749 0.1703 0.6495 0.046 Uiso 1 1 calc R . . C35 C 0.1221(2) 0.1455(2) 0.7818(2) 0.0412(6) Uani 1 1 d . . . C36 C 0.0699(3) 0.1129(2) 0.7177(3) 0.0543(7) Uani 1 1 d . . . H36 H 0.1112 0.1106 0.6374 0.065 Uiso 1 1 calc R . . C37 C -0.0376(3) 0.0855(3) 0.7707(3) 0.0621(8) Uani 1 1 d . . . H37 H -0.0711 0.0641 0.7272 0.075 Uiso 1 1 calc R . . C38 C -0.1010(3) 0.0882(3) 0.8902(3) 0.0588(8) Uani 1 1 d . . . H38 H -0.1765 0.0688 0.9259 0.071 Uiso 1 1 calc R . . C39 C -0.0548(2) 0.1184(2) 0.9542(2) 0.0493(7) Uani 1 1 d . . . H39 H -0.0982 0.1191 1.0343 0.059 Uiso 1 1 calc R . . C40 C 0.0579(2) 0.14901(19) 0.9031(2) 0.0393(6) Uani 1 1 d . . . C41 C 0.1070(2) 0.18112(19) 0.9659(2) 0.0377(5) Uani 1 1 d . . . H41 H 0.0645 0.1824 1.0461 0.045 Uiso 1 1 calc R . . C42 C 0.2185(2) 0.21219(17) 0.91459(19) 0.0325(5) Uani 1 1 d . . . C51 C 0.1976(2) 0.25623(18) 1.10535(18) 0.0319(5) Uani 1 1 d . . . C52 C 0.2260(2) 0.16646(18) 1.16532(19) 0.0335(5) Uani 1 1 d . . . C53 C 0.3189(2) 0.06495(19) 1.1107(2) 0.0378(5) Uani 1 1 d . . . H53 H 0.3654 0.0575 1.0305 0.045 Uiso 1 1 calc R . . C54 C 0.3425(2) -0.0211(2) 1.1705(2) 0.0443(6) Uani 1 1 d . . . H54 H 0.4048 -0.0877 1.1317 0.053 Uiso 1 1 calc R . . C55 C 0.2754(3) -0.0127(2) 1.2898(2) 0.0483(6) Uani 1 1 d . . . H55 H 0.2928 -0.0738 1.3305 0.058 Uiso 1 1 calc R . . C56 C 0.1864(3) 0.0817(2) 1.3470(2) 0.0448(6) Uani 1 1 d . . . H56 H 0.1418 0.0863 1.4273 0.054 Uiso 1 1 calc R . . C57 C 0.1594(2) 0.1742(2) 1.2867(2) 0.0371(5) Uani 1 1 d . . . C58 C 0.0697(2) 0.2726(2) 1.34071(19) 0.0415(6) Uani 1 1 d . . . C59 C 0.0388(2) 0.3631(2) 1.2850(2) 0.0392(6) Uani 1 1 d . . . C60 C -0.0573(3) 0.4619(2) 1.3441(2) 0.0509(7) Uani 1 1 d . . . H60 H -0.1002 0.4682 1.4245 0.061 Uiso 1 1 calc R . . C61 C -0.0874(3) 0.5467(2) 1.2856(2) 0.0535(7) Uani 1 1 d . . . H61 H -0.1522 0.6118 1.3253 0.064 Uiso 1 1 calc R . . C62 C -0.0229(2) 0.5390(2) 1.1657(2) 0.0465(6) Uani 1 1 d . . . H62 H -0.0448 0.5993 1.1259 0.056 Uiso 1 1 calc R . . C63 C 0.0698(2) 0.44673(19) 1.1069(2) 0.0371(5) Uani 1 1 d . . . H63 H 0.1126 0.4438 1.0266 0.044 Uiso 1 1 calc R . . F1 F 0.00713(16) 0.28044(13) 1.45581(12) 0.0618(5) Uani 1 1 d . . . Si1 Si 0.55544(6) 0.26165(6) 0.36329(5) 0.03755(18) 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 0.0429(14) 0.0421(13) 0.0360(13) 0.0048(10) -0.0181(11) -0.0155(11) C2 0.0412(13) 0.0332(12) 0.0361(13) 0.0044(10) -0.0187(11) -0.0116(10) C3 0.0488(16) 0.0607(17) 0.0494(16) 0.0055(13) -0.0196(13) -0.0226(14) C4 0.0485(19) 0.095(3) 0.096(3) 0.014(2) -0.0370(19) -0.0263(19) C5 0.062(2) 0.085(2) 0.061(2) 0.0150(17) -0.0172(16) -0.0415(19) C6 0.0422(14) 0.0441(14) 0.0452(15) -0.0053(11) -0.0186(12) -0.0057(12) C7 0.072(2) 0.0466(16) 0.0620(19) 0.0032(14) -0.0317(16) -0.0232(15) C8 0.081(2) 0.071(2) 0.0424(16) -0.0121(15) -0.0187(16) -0.0254(18) C9 0.0457(14) 0.0451(14) 0.0320(12) 0.0016(10) -0.0156(11) -0.0135(12) C10 0.0584(17) 0.0403(14) 0.0487(15) 0.0020(12) -0.0256(14) -0.0114(13) C11 0.0484(17) 0.0505(16) 0.071(2) -0.0034(14) -0.0311(15) -0.0070(13) C12 0.0298(12) 0.0356(12) 0.0347(12) 0.0026(10) -0.0127(10) -0.0092(10) C21 0.0335(12) 0.0279(11) 0.0316(11) 0.0018(9) -0.0145(10) -0.0056(9) C22 0.0334(12) 0.0278(11) 0.0313(11) 0.0027(9) -0.0154(10) -0.0040(9) C23 0.0403(13) 0.0365(12) 0.0305(12) 0.0033(10) -0.0166(10) -0.0100(11) C24 0.0393(13) 0.0361(12) 0.0381(13) 0.0068(10) -0.0210(11) -0.0123(11) C25 0.0528(16) 0.0524(15) 0.0430(14) 0.0084(12) -0.0271(13) -0.0209(13) C26 0.0587(18) 0.0613(17) 0.0543(17) 0.0128(14) -0.0353(15) -0.0290(15) C27 0.0491(16) 0.073(2) 0.0592(18) 0.0189(15) -0.0287(14) -0.0330(15) C28 0.0462(15) 0.0619(17) 0.0436(14) 0.0164(13) -0.0208(12) -0.0254(14) C29 0.0374(13) 0.0367(12) 0.0397(13) 0.0105(10) -0.0187(11) -0.0121(11) C30 0.0399(13) 0.0361(12) 0.0325(12) 0.0085(10) -0.0169(10) -0.0117(10) C31 0.0367(12) 0.0274(11) 0.0319(11) 0.0042(9) -0.0165(10) -0.0070(10) C32 0.0393(13) 0.0282(11) 0.0295(11) 0.0030(9) -0.0151(10) -0.0062(10) C33 0.0362(12) 0.0274(11) 0.0339(12) 0.0017(9) -0.0175(10) -0.0047(10) C34 0.0415(14) 0.0364(12) 0.0348(12) -0.0013(10) -0.0190(11) -0.0061(11) C35 0.0419(14) 0.0379(13) 0.0468(14) -0.0020(11) -0.0239(12) -0.0090(11) C36 0.0544(17) 0.0629(18) 0.0508(16) -0.0067(14) -0.0272(14) -0.0171(15) C37 0.0558(18) 0.073(2) 0.072(2) -0.0086(17) -0.0372(17) -0.0226(16) C38 0.0448(16) 0.0670(19) 0.068(2) -0.0037(16) -0.0244(15) -0.0219(15) C39 0.0423(15) 0.0523(16) 0.0542(16) 0.0009(13) -0.0208(13) -0.0169(13) C40 0.0376(13) 0.0341(12) 0.0447(14) 0.0012(10) -0.0193(11) -0.0075(11) C41 0.0354(13) 0.0383(12) 0.0365(12) 0.0030(10) -0.0155(10) -0.0087(10) C42 0.0329(12) 0.0282(11) 0.0337(12) 0.0010(9) -0.0158(10) -0.0044(9) C51 0.0297(12) 0.0342(12) 0.0318(12) 0.0035(9) -0.0148(10) -0.0089(10) C52 0.0324(12) 0.0344(12) 0.0344(12) 0.0031(9) -0.0163(10) -0.0096(10) C53 0.0385(13) 0.0353(12) 0.0378(13) 0.0010(10) -0.0183(11) -0.0069(11) C54 0.0443(15) 0.0353(13) 0.0508(15) 0.0032(11) -0.0244(12) -0.0044(11) C55 0.0580(17) 0.0398(14) 0.0529(16) 0.0154(12) -0.0333(14) -0.0126(13) C56 0.0513(16) 0.0476(15) 0.0376(13) 0.0102(11) -0.0227(12) -0.0153(13) C57 0.0383(13) 0.0401(13) 0.0341(12) 0.0054(10) -0.0175(10) -0.0125(11) C58 0.0412(14) 0.0491(14) 0.0282(12) 0.0032(10) -0.0112(11) -0.0134(12) C59 0.0340(13) 0.0395(13) 0.0363(13) 0.0009(10) -0.0110(10) -0.0084(11) C60 0.0445(15) 0.0469(15) 0.0378(14) -0.0037(12) -0.0045(12) -0.0040(12) C61 0.0447(15) 0.0388(14) 0.0525(16) -0.0040(12) -0.0105(13) 0.0027(12) C62 0.0407(14) 0.0375(13) 0.0540(16) 0.0059(12) -0.0203(13) -0.0049(11) C63 0.0352(13) 0.0357(12) 0.0378(13) 0.0054(10) -0.0160(10) -0.0090(10) F1 0.0680(11) 0.0634(10) 0.0313(8) 0.0030(7) -0.0105(8) -0.0093(9) Si1 0.0387(4) 0.0423(4) 0.0297(3) 0.0023(3) -0.0133(3) -0.0135(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.204(3) . ? C1 Si1 1.848(2) . ? C2 C32 1.429(3) . ? C3 C4 1.536(4) . ? C3 C5 1.517(4) . ? C3 Si1 1.888(3) . ? C6 C7 1.528(4) . ? C6 C8 1.527(4) . ? C6 Si1 1.883(3) . ? C9 C10 1.539(3) . ? C9 C11 1.530(4) . ? C9 Si1 1.884(3) . ? C12 C51 1.408(3) . ? C12 C59 1.432(3) . ? C12 C63 1.429(3) . ? C21 C22 1.413(3) . ? C21 C42 1.414(3) . ? C21 C51 1.497(3) . ? C22 C23 1.414(3) . ? C22 C31 1.446(3) . ? C23 C24 1.388(3) . ? C24 C25 1.429(3) . ? C24 C29 1.441(3) . ? C25 C26 1.350(4) . ? C26 C27 1.421(4) . ? C27 C28 1.358(4) . ? C28 C29 1.434(3) . ? C29 C30 1.381(3) . ? C30 C31 1.404(3) . ? C31 C32 1.416(3) . ? C32 C33 1.411(3) . ? C33 C34 1.411(3) . ? C33 C42 1.447(3) . ? C34 C35 1.384(3) . ? C35 C36 1.436(4) . ? C35 C40 1.435(3) . ? C36 C37 1.350(4) . ? C37 C38 1.414(4) . ? C38 C39 1.357(4) . ? C39 C40 1.428(3) . ? C40 C41 1.386(3) . ? C41 C42 1.417(3) . ? C51 C52 1.406(3) . ? C52 C53 1.428(3) . ? C52 C57 1.436(3) . ? C53 C54 1.356(3) . ? C54 C55 1.413(4) . ? C55 C56 1.356(4) . ? C56 C57 1.430(3) . ? C57 C58 1.386(3) . ? C58 C59 1.386(3) . ? C58 F1 1.361(3) . ? C59 C60 1.430(3) . ? C60 C61 1.355(4) . ? C61 C62 1.418(4) . ? C62 C63 1.358(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Si1 173.6(2) . . ? C1 C2 C32 178.1(3) . . ? C4 C3 Si1 111.4(2) . . ? C5 C3 C4 111.6(3) . . ? C5 C3 Si1 115.0(2) . . ? C7 C6 Si1 113.40(18) . . ? C8 C6 C7 110.0(2) . . ? C8 C6 Si1 113.9(2) . . ? C10 C9 Si1 109.84(18) . . ? C11 C9 C10 110.2(2) . . ? C11 C9 Si1 114.48(18) . . ? C51 C12 C59 120.1(2) . . ? C51 C12 C63 122.4(2) . . ? C63 C12 C59 117.5(2) . . ? C22 C21 C42 120.4(2) . . ? C22 C21 C51 119.8(2) . . ? C42 C21 C51 119.8(2) . . ? C21 C22 C23 122.1(2) . . ? C21 C22 C31 120.0(2) . . ? C23 C22 C31 117.9(2) . . ? C24 C23 C22 122.2(2) . . ? C23 C24 C25 122.6(2) . . ? C23 C24 C29 119.2(2) . . ? C25 C24 C29 118.3(2) . . ? C26 C25 C24 121.1(2) . . ? C25 C26 C27 120.9(3) . . ? C28 C27 C26 120.4(3) . . ? C27 C28 C29 120.8(3) . . ? C28 C29 C24 118.5(2) . . ? C30 C29 C24 119.3(2) . . ? C30 C29 C28 122.2(2) . . ? C29 C30 C31 122.0(2) . . ? C30 C31 C22 119.3(2) . . ? C30 C31 C32 121.3(2) . . ? C32 C31 C22 119.5(2) . . ? C31 C32 C2 120.0(2) . . ? C33 C32 C2 119.3(2) . . ? C33 C32 C31 120.7(2) . . ? C32 C33 C34 121.4(2) . . ? C32 C33 C42 119.7(2) . . ? C34 C33 C42 118.9(2) . . ? C35 C34 C33 122.1(2) . . ? C34 C35 C36 121.7(2) . . ? C34 C35 C40 119.4(2) . . ? C40 C35 C36 118.9(2) . . ? C37 C36 C35 120.4(3) . . ? C36 C37 C38 121.0(3) . . ? C39 C38 C37 120.6(3) . . ? C38 C39 C40 121.1(3) . . ? C39 C40 C35 118.0(2) . . ? C41 C40 C35 119.4(2) . . ? C41 C40 C39 122.6(2) . . ? C40 C41 C42 122.2(2) . . ? C21 C42 C33 119.8(2) . . ? C21 C42 C41 122.2(2) . . ? C41 C42 C33 118.0(2) . . ? C12 C51 C21 119.8(2) . . ? C52 C51 C12 120.2(2) . . ? C52 C51 C21 119.9(2) . . ? C51 C52 C53 122.8(2) . . ? C51 C52 C57 120.0(2) . . ? C53 C52 C57 117.2(2) . . ? C54 C53 C52 121.6(2) . . ? C53 C54 C55 120.6(2) . . ? C56 C55 C54 120.7(2) . . ? C55 C56 C57 120.2(2) . . ? C56 C57 C52 119.7(2) . . ? C58 C57 C52 117.7(2) . . ? C58 C57 C56 122.6(2) . . ? C57 C58 C59 124.2(2) . . ? F1 C58 C57 117.8(2) . . ? F1 C58 C59 118.0(2) . . ? C58 C59 C12 117.7(2) . . ? C58 C59 C60 122.3(2) . . ? C60 C59 C12 119.9(2) . . ? C61 C60 C59 120.1(2) . . ? C60 C61 C62 120.5(2) . . ? C63 C62 C61 120.9(2) . . ? C62 C63 C12 121.0(2) . . ? C1 Si1 C3 105.33(12) . . ? C1 Si1 C6 106.95(12) . . ? C1 Si1 C9 105.64(11) . . ? C6 Si1 C3 113.31(13) . . ? C6 Si1 C9 114.69(12) . . ? C9 Si1 C3 110.13(12) . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 8 3 5 0.0754 8.0000 3.0000 5.0000 0.0695 0.0256 -0.9955 1 1 -7 0.0344 1.0000 1.0000 -7.0000 -0.9775 -0.0627 -0.0481 -6 -7 -3 0.0741 -6.0000 -7.0000 -3.0000 0.0872 -0.5997 0.7697 5 -5 3 0.0982 5.0000 -5.0000 3.0000 0.0895 -0.8470 -0.5761 -8 -3 -4 0.0840 -8.0000 -3.0000 -4.0000 0.0591 -0.0067 0.9850 -7 -6 -5 0.0706 -7.0000 -6.0000 -5.0000 -0.1107 -0.4567 0.8997 7 6 5 0.0706 7.0000 6.0000 5.0000 0.1107 0.4567 -0.8997 -7 -5 0 0.0528 -7.0000 -5.0000 -0.0000 0.5233 -0.2370 0.8404 7 5 0 0.0528 7.0000 5.0000 0.0000 -0.5233 0.2370 -0.8404 -5 5 -3 0.1023 -5.0000 5.0000 -3.0000 -0.0895 0.8470 0.5761 -1 -1 7 0.0279 -1.0000 -1.0000 7.0000 0.9775 0.0627 0.0481 _database_code_depnum_ccdc_archive 'CCDC 927707'