# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_10118 _database_code_depnum_ccdc_archive 'CCDC 824471' #TrackingRef '10118.cif' _audit_creation_date 10-12-15 _audit_creation_method CRYSTALS_ver_14.06 _oxford_structure_analysis_title 'mo_10118_0m in P2(1)' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 7.1510(8) _cell_length_b 29.386(3) _cell_length_c 9.6851(10) _cell_angle_alpha 90 _cell_angle_beta 100.773(2) _cell_angle_gamma 90 _cell_volume 1999.4(4) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C20 H18 Fe1 O4 Si1 # Dc = 1.35 Fooo = 840.00 Mu = 8.35 M = 812.59 # Found Formula = C20 H18 Fe1 O4 Si1 # Dc = 1.35 FOOO = 840.00 Mu = 8.35 M = 812.59 _chemical_formula_sum 'C20 H18 Fe1 O4 Si1' _chemical_formula_moiety 'C20 H18 Fe1 O4 Si1' _chemical_compound_source ? _chemical_formula_weight 406.29 _cell_measurement_reflns_used 9909 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description acicular _exptl_crystal_colour colorless _exptl_crystal_size_min 0.114 _exptl_crystal_size_mid 0.124 _exptl_crystal_size_max 0.491 _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.835 # Sheldrick geometric approximatio 0.90 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.91 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 21632 _reflns_number_total 11113 _diffrn_reflns_av_R_equivalents 0.026 # Number of reflections without Friedels Law is 11113 # Number of reflections with Friedels Law is 5908 # Theoretical number of reflections is about 5851 _diffrn_reflns_theta_min 2.141 _diffrn_reflns_theta_max 30.036 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.135 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min -10 _reflns_limit_h_max 9 _reflns_limit_k_min -41 _reflns_limit_k_max 41 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 2.21 _oxford_diffrn_Wilson_scale 27.26 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.30 _refine_diff_density_max 0.61 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 11113 _refine_ls_number_restraints 1 _refine_ls_number_parameters 469 _oxford_refine_ls_R_factor_ref 0.0443 _refine_ls_wR_factor_ref 0.0910 _refine_ls_goodness_of_fit_ref 0.9951 _refine_ls_shift/su_max 0.0025925 _refine_ls_shift/su_mean 0.0004175 # The values computed from all data _oxford_reflns_number_all 11113 _refine_ls_R_factor_all 0.0443 _refine_ls_wR_factor_all 0.0910 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9275 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_gt 0.0852 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.66P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.29411(5) 0.47011(3) 0.63528(3) 0.0269 1.0000 Uani . . . . . . . Fe51 Fe 0.11477(5) 0.89915(3) 0.88269(4) 0.0267 1.0000 Uani . . . . . . . Si1 Si 0.46209(10) 0.57794(4) 0.30393(7) 0.0266 1.0000 Uani . . . . . . . Si51 Si 0.28619(9) 0.79132(4) 0.55336(7) 0.0257 1.0000 Uani . . . . . . . O1 O -0.0897(3) 0.50157(9) 0.5078(2) 0.0461 1.0000 Uani . . . . . . . O2 O 0.1876(4) 0.37443(9) 0.6737(3) 0.0645 1.0000 Uani . . . . . . . O3 O 0.7023(3) 0.45456(9) 0.7435(3) 0.0504 1.0000 Uani . . . . . . . O4 O 0.2672(3) 0.52489(10) 0.8854(2) 0.0516 1.0000 Uani . . . . . . . O51 O 0.5226(3) 0.91447(9) 0.9920(3) 0.0532 1.0000 Uani . . . . . . . O52 O 0.0826(3) 0.84482(10) 1.1324(2) 0.0522 1.0000 Uani . . . . . . . O53 O -0.2687(3) 0.86746(8) 0.7537(2) 0.0470 1.0000 Uani . . . . . . . O54 O 0.0062(4) 0.99482(9) 0.9221(3) 0.0646 1.0000 Uani . . . . . . . C1 C 0.3628(4) 0.46710(10) 0.4341(3) 0.0318 1.0000 Uani . . . . . . . C2 C 0.3739(3) 0.51124(9) 0.4892(2) 0.0245 1.0000 Uani . . . . . . . C3 C 0.3953(3) 0.55538(9) 0.4710(2) 0.0229 1.0000 Uani . . . . . . . C4 C 0.3566(3) 0.58869(8) 0.5784(3) 0.0231 1.0000 Uani . . . . . . . C5 C 0.1821(3) 0.60998(9) 0.5601(3) 0.0306 1.0000 Uani . . . . . . . C6 C 0.1362(4) 0.64067(10) 0.6604(3) 0.0351 1.0000 Uani . . . . . . . C7 C 0.2652(4) 0.65029(9) 0.7789(3) 0.0311 1.0000 Uani . . . . . . . C8 C 0.4477(3) 0.62984(9) 0.8028(3) 0.0255 1.0000 Uani . . . . . . . C9 C 0.5826(4) 0.63906(10) 0.9263(3) 0.0328 1.0000 Uani . . . . . . . C10 C 0.7560(4) 0.61824(10) 0.9492(3) 0.0347 1.0000 Uani . . . . . . . C11 C 0.8046(4) 0.58745(10) 0.8489(3) 0.0331 1.0000 Uani . . . . . . . C12 C 0.6777(3) 0.57811(9) 0.7282(3) 0.0261 1.0000 Uani . . . . . . . C13 C 0.4948(3) 0.59858(8) 0.7015(2) 0.0224 1.0000 Uani . . . . . . . C14 C 0.0558(4) 0.48863(10) 0.5568(3) 0.0328 1.0000 Uani . . . . . . . C15 C 0.2290(4) 0.41103(11) 0.6603(3) 0.0412 1.0000 Uani . . . . . . . C16 C 0.5444(4) 0.46037(10) 0.7034(3) 0.0346 1.0000 Uani . . . . . . . C17 C 0.2768(4) 0.50340(11) 0.7896(3) 0.0365 1.0000 Uani . . . . . . . C18 C 0.2453(4) 0.60257(11) 0.1929(3) 0.0376 1.0000 Uani . . . . . . . C19 C 0.5567(5) 0.53108(12) 0.2062(3) 0.0427 1.0000 Uani . . . . . . . C20 C 0.6451(4) 0.62323(12) 0.3553(3) 0.0417 1.0000 Uani . . . . . . . C501 C 0.1847(4) 0.90201(10) 0.6823(3) 0.0348 1.0000 Uani . . . . . . . C502 C 0.1973(3) 0.85784(9) 0.7377(2) 0.0255 1.0000 Uani . . . . . . . C503 C 0.2215(3) 0.81392(9) 0.7203(2) 0.0247 1.0000 Uani . . . . . . . C504 C 0.1799(3) 0.78112(8) 0.8299(2) 0.0240 1.0000 Uani . . . . . . . C505 C 0.0034(3) 0.76101(9) 0.8133(3) 0.0290 1.0000 Uani . . . . . . . C506 C -0.0487(4) 0.73157(9) 0.9148(3) 0.0296 1.0000 Uani . . . . . . . C507 C 0.0798(4) 0.72237(9) 1.0349(3) 0.0302 1.0000 Uani . . . . . . . C508 C 0.2642(3) 0.74163(8) 1.0572(2) 0.0240 1.0000 Uani . . . . . . . C509 C 0.4002(4) 0.73170(10) 1.1801(3) 0.0326 1.0000 Uani . . . . . . . C510 C 0.5761(4) 0.75041(11) 1.2002(3) 0.0375 1.0000 Uani . . . . . . . C511 C 0.6283(4) 0.78027(10) 1.0990(3) 0.0328 1.0000 Uani . . . . . . . C512 C 0.5011(3) 0.79016(10) 0.9793(3) 0.0294 1.0000 Uani . . . . . . . C513 C 0.3157(3) 0.77094(9) 0.9539(2) 0.0240 1.0000 Uani . . . . . . . C514 C 0.3650(4) 0.90892(10) 0.9506(3) 0.0359 1.0000 Uani . . . . . . . C515 C 0.0481(4) 0.95761(11) 0.9097(3) 0.0382 1.0000 Uani . . . . . . . C516 C -0.1207(4) 0.88046(10) 0.8034(3) 0.0330 1.0000 Uani . . . . . . . C517 C 0.0953(4) 0.86610(11) 1.0370(3) 0.0355 1.0000 Uani . . . . . . . C518 C 0.3680(4) 0.83882(11) 0.4530(3) 0.0378 1.0000 Uani . . . . . . . C519 C 0.4765(4) 0.74791(12) 0.6000(3) 0.0400 1.0000 Uani . . . . . . . C520 C 0.0690(4) 0.76497(11) 0.4466(3) 0.0400 1.0000 Uani . . . . . . . H51 H 0.0906 0.6037 0.4778 0.0387 1.0000 Uiso R . . . . . . H61 H 0.0142 0.6546 0.6456 0.0447 1.0000 Uiso R . . . . . . H71 H 0.2337 0.6710 0.8463 0.0370 1.0000 Uiso R . . . . . . H91 H 0.5518 0.6596 0.9945 0.0405 1.0000 Uiso R . . . . . . H101 H 0.8452 0.6243 1.0329 0.0416 1.0000 Uiso R . . . . . . H111 H 0.9272 0.5738 0.8652 0.0379 1.0000 Uiso R . . . . . . H121 H 0.7115 0.5571 0.6624 0.0309 1.0000 Uiso R . . . . . . H181 H 0.2762 0.6141 0.1082 0.0465 1.0000 Uiso R . . . . . . H182 H 0.1981 0.6266 0.2424 0.0465 1.0000 Uiso R . . . . . . H183 H 0.1508 0.5796 0.1713 0.0465 1.0000 Uiso R . . . . . . H191 H 0.5896 0.5430 0.1228 0.0532 1.0000 Uiso R . . . . . . H192 H 0.6662 0.5180 0.2630 0.0532 1.0000 Uiso R . . . . . . H193 H 0.4613 0.5084 0.1824 0.0532 1.0000 Uiso R . . . . . . H201 H 0.6820 0.6352 0.2734 0.0508 1.0000 Uiso R . . . . . . H202 H 0.5928 0.6468 0.4033 0.0508 1.0000 Uiso R . . . . . . H203 H 0.7531 0.6107 0.4153 0.0508 1.0000 Uiso R . . . . . . H5051 H -0.0868 0.7672 0.7303 0.0333 1.0000 Uiso R . . . . . . H5061 H -0.1714 0.7180 0.8995 0.0358 1.0000 Uiso R . . . . . . H5071 H 0.0444 0.7032 1.1047 0.0357 1.0000 Uiso R . . . . . . H5091 H 0.3678 0.7114 1.2483 0.0377 1.0000 Uiso R . . . . . . H5101 H 0.6654 0.7437 1.2833 0.0452 1.0000 Uiso R . . . . . . H5111 H 0.7511 0.7938 1.1151 0.0410 1.0000 Uiso R . . . . . . H5121 H 0.5390 0.8093 0.9104 0.0366 1.0000 Uiso R . . . . . . H5181 H 0.4010 0.8275 0.3688 0.0451 1.0000 Uiso R . . . . . . H5182 H 0.4760 0.8528 0.5087 0.0451 1.0000 Uiso R . . . . . . H5183 H 0.2685 0.8605 0.4304 0.0451 1.0000 Uiso R . . . . . . H5191 H 0.5105 0.7362 0.5167 0.0497 1.0000 Uiso R . . . . . . H5192 H 0.5848 0.7615 0.6568 0.0497 1.0000 Uiso R . . . . . . H5193 H 0.4316 0.7238 0.6506 0.0497 1.0000 Uiso R . . . . . . H5201 H 0.0978 0.7532 0.3617 0.0481 1.0000 Uiso R . . . . . . H5202 H -0.0283 0.7873 0.4255 0.0481 1.0000 Uiso R . . . . . . H5203 H 0.0267 0.7410 0.4989 0.0481 1.0000 Uiso R . . . . . . H11 H 0.4767 0.4521 0.4228 0.0383 1.0000 Uiso R . . . . . . H12 H 0.2648 0.4604 0.3562 0.0383 1.0000 Uiso R . . . . . . H5011 H 0.2984 0.9172 0.6712 0.0433 1.0000 Uiso R . . . . . . H5012 H 0.0868 0.9087 0.6042 0.0433 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02783(17) 0.02765(18) 0.02640(17) 0.00344(14) 0.00795(13) 0.00287(14) Fe51 0.02718(17) 0.02697(18) 0.02663(18) -0.00293(14) 0.00679(13) -0.00211(14) Si1 0.0253(3) 0.0319(4) 0.0219(3) 0.0051(3) 0.0025(2) 0.0030(3) Si51 0.0251(3) 0.0313(4) 0.0206(3) -0.0024(3) 0.0038(2) -0.0011(3) O1 0.0323(11) 0.0565(14) 0.0472(13) -0.0081(10) 0.0013(9) 0.0083(10) O2 0.0622(17) 0.0422(14) 0.094(2) 0.0179(13) 0.0268(15) -0.0065(12) O3 0.0327(11) 0.0629(15) 0.0547(14) 0.0189(11) 0.0061(9) 0.0123(10) O4 0.0511(13) 0.0736(17) 0.0318(11) -0.0087(11) 0.0124(9) 0.0024(12) O51 0.0330(11) 0.0668(16) 0.0582(14) -0.0227(12) 0.0044(10) -0.0079(10) O52 0.0596(15) 0.0662(16) 0.0332(12) 0.0073(11) 0.0152(10) 0.0003(12) O53 0.0341(11) 0.0510(14) 0.0527(13) 0.0035(11) -0.0001(9) -0.0076(10) O54 0.0647(17) 0.0362(13) 0.095(2) -0.0154(13) 0.0208(15) 0.0099(11) C1 0.0433(13) 0.0279(13) 0.0264(11) 0.0003(10) 0.0124(10) 0.0066(12) C2 0.0236(11) 0.0301(13) 0.0200(11) 0.0010(9) 0.0043(8) 0.0064(9) C3 0.0209(10) 0.0274(12) 0.0203(10) 0.0002(8) 0.0035(8) 0.0026(8) C4 0.0214(10) 0.0231(12) 0.0253(11) 0.0007(9) 0.0059(8) 0.0018(8) C5 0.0220(11) 0.0328(14) 0.0356(14) -0.0018(10) 0.0015(10) 0.0046(10) C6 0.0266(12) 0.0339(14) 0.0458(16) -0.0014(12) 0.0093(11) 0.0087(10) C7 0.0312(13) 0.0275(13) 0.0378(14) -0.0053(10) 0.0145(10) 0.0037(10) C8 0.0262(11) 0.0233(11) 0.0283(12) 0.0011(8) 0.0085(9) -0.0022(9) C9 0.0376(14) 0.0314(14) 0.0292(13) -0.0061(10) 0.0060(10) -0.0069(11) C10 0.0348(13) 0.0385(15) 0.0288(13) 0.0010(11) 0.0010(10) -0.0071(11) C11 0.0202(11) 0.0409(16) 0.0357(14) 0.0084(11) -0.0012(10) -0.0003(10) C12 0.0205(10) 0.0321(12) 0.0257(11) 0.0023(9) 0.0046(8) 0.0039(9) C13 0.0225(11) 0.0219(11) 0.0234(11) 0.0015(8) 0.0062(8) -0.0005(8) C14 0.0321(14) 0.0341(14) 0.0327(14) -0.0081(10) 0.0077(11) 0.0001(11) C15 0.0333(14) 0.0399(17) 0.0519(18) 0.0142(13) 0.0119(13) 0.0025(12) C16 0.0360(14) 0.0383(16) 0.0309(13) 0.0125(11) 0.0103(10) 0.0059(11) C17 0.0353(14) 0.0472(17) 0.0282(13) 0.0033(12) 0.0087(11) 0.0024(12) C18 0.0332(14) 0.0408(16) 0.0354(15) 0.0129(12) -0.0022(11) 0.0035(12) C19 0.0562(18) 0.0485(18) 0.0258(13) 0.0037(12) 0.0142(12) 0.0184(15) C20 0.0336(14) 0.0498(18) 0.0396(16) 0.0059(13) 0.0012(11) -0.0076(13) C501 0.0441(14) 0.0333(14) 0.0303(12) 0.0028(12) 0.0153(10) -0.0011(13) C502 0.0237(11) 0.0337(13) 0.0196(11) -0.0017(9) 0.0056(8) -0.0046(9) C503 0.0224(11) 0.0293(12) 0.0219(11) -0.0005(9) 0.0027(8) -0.0018(9) C504 0.0252(11) 0.0244(12) 0.0221(11) -0.0002(9) 0.0038(8) 0.0006(9) C505 0.0247(12) 0.0287(13) 0.0335(13) 0.0005(10) 0.0052(10) 0.0001(9) C506 0.0251(12) 0.0242(12) 0.0404(14) -0.0011(10) 0.0085(10) -0.0029(9) C507 0.0337(13) 0.0239(12) 0.0356(13) 0.0003(10) 0.0130(10) -0.0018(10) C508 0.0288(12) 0.0219(11) 0.0226(11) -0.0026(9) 0.0080(9) 0.0036(9) C509 0.0395(15) 0.0325(14) 0.0261(12) -0.0006(10) 0.0070(10) 0.0033(11) C510 0.0359(14) 0.0422(16) 0.0311(14) -0.0044(11) -0.0020(11) 0.0043(12) C511 0.0266(13) 0.0399(16) 0.0303(13) -0.0038(11) 0.0010(10) -0.0008(11) C512 0.0250(12) 0.0364(14) 0.0275(12) -0.0040(10) 0.0064(9) -0.0020(10) C513 0.0242(11) 0.0246(11) 0.0244(11) -0.0041(9) 0.0073(9) 0.0021(9) C514 0.0378(14) 0.0359(16) 0.0352(14) -0.0112(11) 0.0096(11) -0.0023(11) C515 0.0425(16) 0.0370(17) 0.0384(16) -0.0025(11) 0.0158(12) -0.0018(12) C516 0.0332(14) 0.0326(14) 0.0332(14) 0.0023(11) 0.0060(11) 0.0008(10) C517 0.0341(14) 0.0433(17) 0.0287(14) -0.0033(12) 0.0048(10) 0.0003(12) C518 0.0448(16) 0.0464(17) 0.0240(12) -0.0016(11) 0.0109(10) -0.0054(13) C519 0.0338(14) 0.0540(18) 0.0320(14) -0.0018(12) 0.0059(11) 0.0101(13) C520 0.0344(14) 0.0496(18) 0.0341(14) -0.0072(12) 0.0015(11) -0.0049(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.18657(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . C1 . 2.098(2) yes Fe1 . C2 . 2.022(2) yes Fe1 . C14 . 1.815(3) yes Fe1 . C15 . 1.825(3) yes Fe1 . C16 . 1.811(3) yes Fe1 . C17 . 1.809(3) yes Fe51 . C501 . 2.095(3) yes Fe51 . C502 . 2.026(2) yes Fe51 . C514 . 1.810(3) yes Fe51 . C515 . 1.815(3) yes Fe51 . C516 . 1.801(3) yes Fe51 . C517 . 1.809(3) yes Si1 . C3 . 1.890(2) yes Si1 . C18 . 1.860(3) yes Si1 . C19 . 1.868(3) yes Si1 . C20 . 1.868(3) yes Si51 . C503 . 1.884(3) yes Si51 . C518 . 1.857(3) yes Si51 . C519 . 1.859(3) yes Si51 . C520 . 1.866(3) yes O1 . C14 . 1.126(3) yes O2 . C15 . 1.129(4) yes O3 . C16 . 1.136(3) yes O4 . C17 . 1.136(4) yes O51 . C514 . 1.135(3) yes O52 . C517 . 1.133(3) yes O53 . C516 . 1.144(3) yes O54 . C515 . 1.146(4) yes C1 . C2 . 1.399(4) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C2 . C3 . 1.322(4) yes C3 . C4 . 1.492(3) yes C4 . C5 . 1.377(3) yes C4 . C13 . 1.429(3) yes C5 . C6 . 1.408(4) yes C5 . H51 . 0.950 no C6 . C7 . 1.361(4) yes C6 . H61 . 0.950 no C7 . C8 . 1.416(3) yes C7 . H71 . 0.950 no C8 . C9 . 1.416(3) yes C8 . C13 . 1.429(3) yes C9 . C10 . 1.363(4) yes C9 . H91 . 0.950 no C10 . C11 . 1.418(4) yes C10 . H101 . 0.950 no C11 . C12 . 1.367(3) yes C11 . H111 . 0.950 no C12 . C13 . 1.419(3) yes C12 . H121 . 0.950 no C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no C19 . H191 . 0.950 no C19 . H192 . 0.950 no C19 . H193 . 0.950 no C20 . H201 . 0.950 no C20 . H202 . 0.950 no C20 . H203 . 0.950 no C501 . C502 . 1.401(4) yes C501 . H5011 . 0.950 no C501 . H5012 . 0.950 no C502 . C503 . 1.317(4) yes C503 . C504 . 1.504(3) yes C504 . C505 . 1.376(3) yes C504 . C513 . 1.428(3) yes C505 . C506 . 1.411(4) yes C505 . H5051 . 0.950 no C506 . C507 . 1.368(4) yes C506 . H5061 . 0.950 no C507 . C508 . 1.414(3) yes C507 . H5071 . 0.950 no C508 . C509 . 1.420(3) yes C508 . C513 . 1.420(3) yes C509 . C510 . 1.353(4) yes C509 . H5091 . 0.950 no C510 . C511 . 1.416(4) yes C510 . H5101 . 0.950 no C511 . C512 . 1.365(4) yes C511 . H5111 . 0.950 no C512 . C513 . 1.419(3) yes C512 . H5121 . 0.950 no C518 . H5181 . 0.950 no C518 . H5182 . 0.950 no C518 . H5183 . 0.950 no C519 . H5191 . 0.950 no C519 . H5192 . 0.950 no C519 . H5193 . 0.950 no C520 . H5201 . 0.950 no C520 . H5202 . 0.950 no C520 . H5203 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . Fe1 . C2 . 39.65(10) yes C1 . Fe1 . C14 . 89.34(12) yes C2 . Fe1 . C14 . 83.89(11) yes C1 . Fe1 . C15 . 101.13(13) yes C2 . Fe1 . C15 . 140.69(13) yes C14 . Fe1 . C15 . 95.60(13) yes C1 . Fe1 . C16 . 86.83(11) yes C2 . Fe1 . C16 . 87.74(11) yes C14 . Fe1 . C16 . 170.67(13) yes C15 . Fe1 . C16 . 93.48(13) yes C1 . Fe1 . C17 . 148.61(13) yes C2 . Fe1 . C17 . 109.06(13) yes C14 . Fe1 . C17 . 88.84(12) yes C15 . Fe1 . C17 . 110.23(14) yes C16 . Fe1 . C17 . 90.01(13) yes C501 . Fe51 . C502 . 39.71(11) yes C501 . Fe51 . C514 . 86.51(12) yes C502 . Fe51 . C514 . 87.18(11) yes C501 . Fe51 . C515 . 102.13(13) yes C502 . Fe51 . C515 . 141.76(13) yes C514 . Fe51 . C515 . 93.78(13) yes C501 . Fe51 . C516 . 89.04(12) yes C502 . Fe51 . C516 . 83.79(11) yes C514 . Fe51 . C516 . 170.14(13) yes C515 . Fe51 . C516 . 95.76(14) yes C501 . Fe51 . C517 . 148.82(13) yes C502 . Fe51 . C517 . 109.17(12) yes C514 . Fe51 . C517 . 90.49(13) yes C515 . Fe51 . C517 . 109.04(14) yes C516 . Fe51 . C517 . 88.76(13) yes C3 . Si1 . C18 . 108.34(12) yes C3 . Si1 . C19 . 110.40(13) yes C18 . Si1 . C19 . 109.61(14) yes C3 . Si1 . C20 . 107.36(13) yes C18 . Si1 . C20 . 110.08(14) yes C19 . Si1 . C20 . 110.99(16) yes C503 . Si51 . C518 . 109.66(12) yes C503 . Si51 . C519 . 108.61(12) yes C518 . Si51 . C519 . 110.82(15) yes C503 . Si51 . C520 . 108.03(12) yes C518 . Si51 . C520 . 109.44(14) yes C519 . Si51 . C520 . 110.23(15) yes Fe1 . C1 . C2 . 67.24(14) yes Fe1 . C1 . H11 . 118.8 no C2 . C1 . H11 . 119.0 no Fe1 . C1 . H12 . 118.7 no C2 . C1 . H12 . 118.5 no H11 . C1 . H12 . 109.5 no C1 . C2 . Fe1 . 73.12(15) yes C1 . C2 . C3 . 149.1(2) yes Fe1 . C2 . C3 . 137.31(19) yes Si1 . C3 . C2 . 120.84(18) yes Si1 . C3 . C4 . 118.46(18) yes C2 . C3 . C4 . 120.6(2) yes C3 . C4 . C5 . 119.3(2) yes C3 . C4 . C13 . 121.7(2) yes C5 . C4 . C13 . 119.0(2) yes C4 . C5 . C6 . 121.6(2) yes C4 . C5 . H51 . 119.0 no C6 . C5 . H51 . 119.4 no C5 . C6 . C7 . 120.4(2) yes C5 . C6 . H61 . 119.9 no C7 . C6 . H61 . 119.7 no C6 . C7 . C8 . 120.5(2) yes C6 . C7 . H71 . 120.1 no C8 . C7 . H71 . 119.3 no C7 . C8 . C9 . 121.2(2) yes C7 . C8 . C13 . 119.3(2) yes C9 . C8 . C13 . 119.5(2) yes C8 . C9 . C10 . 120.5(3) yes C8 . C9 . H91 . 119.9 no C10 . C9 . H91 . 119.6 no C9 . C10 . C11 . 120.5(2) yes C9 . C10 . H101 . 120.0 no C11 . C10 . H101 . 119.5 no C10 . C11 . C12 . 120.4(2) yes C10 . C11 . H111 . 119.5 no C12 . C11 . H111 . 120.1 no C11 . C12 . C13 . 120.8(2) yes C11 . C12 . H121 . 119.5 no C13 . C12 . H121 . 119.7 no C4 . C13 . C8 . 119.2(2) yes C4 . C13 . C12 . 122.4(2) yes C8 . C13 . C12 . 118.4(2) yes Fe1 . C14 . O1 . 177.6(3) yes Fe1 . C15 . O2 . 179.0(3) yes Fe1 . C16 . O3 . 178.5(2) yes Fe1 . C17 . O4 . 178.8(3) yes Si1 . C18 . H181 . 109.5 no Si1 . C18 . H182 . 109.5 no H181 . C18 . H182 . 109.5 no Si1 . C18 . H183 . 109.4 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no Si1 . C19 . H191 . 109.2 no Si1 . C19 . H192 . 110.1 no H191 . C19 . H192 . 109.5 no Si1 . C19 . H193 . 109.1 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no Si1 . C20 . H201 . 109.4 no Si1 . C20 . H202 . 109.3 no H201 . C20 . H202 . 109.5 no Si1 . C20 . H203 . 109.6 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no Fe51 . C501 . C502 . 67.49(14) yes Fe51 . C501 . H5011 . 118.7 no C502 . C501 . H5011 . 118.9 no Fe51 . C501 . H5012 . 118.5 no C502 . C501 . H5012 . 118.7 no H5011 . C501 . H5012 . 109.5 no C501 . C502 . Fe51 . 72.80(16) yes C501 . C502 . C503 . 149.3(2) yes Fe51 . C502 . C503 . 137.54(19) yes Si51 . C503 . C502 . 120.93(19) yes Si51 . C503 . C504 . 119.49(17) yes C502 . C503 . C504 . 119.4(2) yes C503 . C504 . C505 . 119.4(2) yes C503 . C504 . C513 . 122.3(2) yes C505 . C504 . C513 . 118.2(2) yes C504 . C505 . C506 . 122.6(2) yes C504 . C505 . H5051 . 118.6 no C506 . C505 . H5051 . 118.8 no C505 . C506 . C507 . 119.4(2) yes C505 . C506 . H5061 . 120.3 no C507 . C506 . H5061 . 120.2 no C506 . C507 . C508 . 120.6(2) yes C506 . C507 . H5071 . 119.8 no C508 . C507 . H5071 . 119.6 no C507 . C508 . C509 . 121.2(2) yes C507 . C508 . C513 . 119.5(2) yes C509 . C508 . C513 . 119.2(2) yes C508 . C509 . C510 . 120.6(3) yes C508 . C509 . H5091 . 119.6 no C510 . C509 . H5091 . 119.8 no C509 . C510 . C511 . 120.7(2) yes C509 . C510 . H5101 . 119.8 no C511 . C510 . H5101 . 119.5 no C510 . C511 . C512 . 120.0(3) yes C510 . C511 . H5111 . 120.0 no C512 . C511 . H5111 . 119.9 no C511 . C512 . C513 . 121.0(3) yes C511 . C512 . H5121 . 119.4 no C513 . C512 . H5121 . 119.6 no C504 . C513 . C508 . 119.6(2) yes C504 . C513 . C512 . 121.9(2) yes C508 . C513 . C512 . 118.5(2) yes Fe51 . C514 . O51 . 178.9(3) yes Fe51 . C515 . O54 . 177.7(3) yes O53 . C516 . Fe51 . 178.2(3) yes Fe51 . C517 . O52 . 179.0(3) yes Si51 . C518 . H5181 . 109.8 no Si51 . C518 . H5182 . 109.3 no H5181 . C518 . H5182 . 109.5 no Si51 . C518 . H5183 . 109.2 no H5181 . C518 . H5183 . 109.5 no H5182 . C518 . H5183 . 109.5 no Si51 . C519 . H5191 . 109.5 no Si51 . C519 . H5192 . 109.4 no H5191 . C519 . H5192 . 109.5 no Si51 . C519 . H5193 . 109.5 no H5191 . C519 . H5193 . 109.5 no H5192 . C519 . H5193 . 109.5 no Si51 . C520 . H5201 . 109.8 no Si51 . C520 . H5202 . 109.5 no H5201 . C520 . H5202 . 109.5 no Si51 . C520 . H5203 . 109.1 no H5201 . C520 . H5203 . 109.5 no H5202 . C520 . H5203 . 109.5 no 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 C14 Fe1 C1 C2 81.21(17) . . . . no C15 Fe1 C1 C2 176.81(16) . . . . no C16 Fe1 C1 C2 -90.28(17) . . . . no C17 Fe1 C1 C2 -5.5(3) . . . . no C1 Fe1 C2 C3 173.6(3) . . . . no C14 Fe1 C2 C1 -96.36(17) . . . . no C14 Fe1 C2 C3 77.3(3) . . . . no C15 Fe1 C2 C1 -5.0(2) . . . . no C15 Fe1 C2 C3 168.7(2) . . . . no C16 Fe1 C2 C1 87.76(17) . . . . no C16 Fe1 C2 C3 -98.6(3) . . . . no C17 Fe1 C2 C1 176.98(17) . . . . no C17 Fe1 C2 C3 -9.4(3) . . . . no C516 Fe51 C502 C503 -78.1(3) . . . . no C517 Fe51 C502 C501 -177.49(17) . . . . no C517 Fe51 C502 C503 8.5(3) . . . . no C514 Fe51 C502 C501 -87.96(17) . . . . no C514 Fe51 C502 C503 98.0(3) . . . . no C514 Fe51 C501 C502 89.76(17) . . . . no C515 Fe51 C501 C502 -177.12(16) . . . . no C516 Fe51 C501 C502 -81.44(17) . . . . no C517 Fe51 C501 C502 4.6(3) . . . . no C501 Fe51 C502 C503 -174.0(3) . . . . no C515 Fe51 C502 C503 -169.5(2) . . . . no C516 Fe51 C502 C501 96.00(17) . . . . no C515 Fe51 C502 C501 4.6(2) . . . . no C19 Si1 C3 C4 167.06(19) . . . . no C20 Si1 C3 C2 -137.4(2) . . . . no C18 Si1 C3 C2 103.7(2) . . . . no C18 Si1 C3 C4 -72.9(2) . . . . no C19 Si1 C3 C2 -16.3(2) . . . . no C20 Si1 C3 C4 46.0(2) . . . . no C518 Si51 C503 C504 -170.66(17) . . . . no C519 Si51 C503 C502 136.0(2) . . . . no C518 Si51 C503 C502 14.8(2) . . . . no C520 Si51 C503 C502 -104.4(2) . . . . no C520 Si51 C503 C504 70.1(2) . . . . no C519 Si51 C503 C504 -49.4(2) . . . . no Fe1 C1 C2 C3 -171.5(4) . . . . no C1 C2 C3 Si1 -8.1(5) . . . . no Fe1 C2 C3 C4 0.4(4) . . . . no Fe1 C2 C3 Si1 -176.17(14) . . . . no C1 C2 C3 C4 168.4(4) . . . . no Si1 C3 C4 C5 79.9(3) . . . . no Si1 C3 C4 C13 -101.3(2) . . . . no C2 C3 C4 C5 -96.8(3) . . . . no C2 C3 C4 C13 82.1(3) . . . . no C13 C4 C5 C6 -0.8(4) . . . . no C5 C4 C13 C8 0.7(3) . . . . no C3 C4 C13 C8 -178.2(2) . . . . no C3 C4 C13 C12 1.1(4) . . . . no C3 C4 C5 C6 178.1(2) . . . . no C5 C4 C13 C12 180.0(2) . . . . no C4 C5 C6 C7 0.3(4) . . . . no C5 C6 C7 C8 0.4(4) . . . . no C6 C7 C8 C9 -179.2(3) . . . . no C6 C7 C8 C13 -0.5(4) . . . . no C13 C8 C9 C10 -0.3(4) . . . . no C7 C8 C13 C4 0.0(4) . . . . no C7 C8 C13 C12 -179.4(2) . . . . no C7 C8 C9 C10 178.4(3) . . . . no C9 C8 C13 C4 178.7(2) . . . . no C9 C8 C13 C12 -0.6(4) . . . . no C8 C9 C10 C11 0.7(4) . . . . no C9 C10 C11 C12 -0.3(4) . . . . no C10 C11 C12 C13 -0.6(4) . . . . no C11 C12 C13 C4 -178.3(2) . . . . no C11 C12 C13 C8 1.1(4) . . . . no Fe51 C501 C502 C503 172.1(4) . . . . no Fe51 C502 C503 Si51 175.28(14) . . . . no Fe51 C502 C503 C504 0.7(4) . . . . no C501 C502 C503 Si51 6.5(5) . . . . no C501 C502 C503 C504 -168.1(4) . . . . no Si51 C503 C504 C505 -80.4(3) . . . . no Si51 C503 C504 C513 101.5(2) . . . . no C502 C503 C504 C505 94.2(3) . . . . no C502 C503 C504 C513 -83.8(3) . . . . no C503 C504 C505 C506 -177.0(2) . . . . no C513 C504 C505 C506 1.1(4) . . . . no C503 C504 C513 C508 176.5(2) . . . . no C503 C504 C513 C512 -2.0(4) . . . . no C505 C504 C513 C508 -1.6(3) . . . . no C505 C504 C513 C512 179.9(2) . . . . no C504 C505 C506 C507 0.0(4) . . . . no C505 C506 C507 C508 -0.7(4) . . . . no C506 C507 C508 C509 -178.8(3) . . . . no C506 C507 C508 C513 0.3(4) . . . . no C507 C508 C509 C510 -179.9(3) . . . . no C513 C508 C509 C510 1.0(4) . . . . no C507 C508 C513 C504 0.9(3) . . . . no C507 C508 C513 C512 179.5(2) . . . . no C509 C508 C513 C504 180.0(2) . . . . no C509 C508 C513 C512 -1.5(4) . . . . no C508 C509 C510 C511 -0.1(5) . . . . no C509 C510 C511 C512 -0.5(5) . . . . no C510 C511 C512 C513 0.0(4) . . . . no C511 C512 C513 C504 179.5(3) . . . . no C511 C512 C513 C508 1.0(4) . . . . no data_10101 _database_code_depnum_ccdc_archive 'CCDC 904093' #TrackingRef '10101.cif' _audit_creation_date 10-10-13 _audit_creation_method CRYSTALS_ver_14.06 _oxford_structure_analysis_title 'mo_10101_0m in P2(1)/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.129(3) _cell_length_b 8.192(2) _cell_length_c 26.318(6) _cell_angle_alpha 90 _cell_angle_beta 102.587(5) _cell_angle_gamma 90 _cell_volume 2552.2(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C25 H38 O2 Si2 # Dc = 1.11 Fooo = 928.00 Mu = 1.56 M = 426.75 # Found Formula = C25 H38 O2 Si2 # Dc = 1.11 FOOO = 928.00 Mu = 1.56 M = 426.75 _chemical_formula_sum 'C25 H38 O2 Si2' _chemical_formula_moiety 'C25 H38 O2 Si2' _chemical_compound_source ? _chemical_formula_weight 426.75 _cell_measurement_reflns_used 1810 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _cell_measurement_temperature 150 _exptl_crystal_description 'plate fragment' _exptl_crystal_colour yellow _exptl_crystal_size_min 0.076 _exptl_crystal_size_mid 0.193 _exptl_crystal_size_max 0.259 _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.156 # Sheldrick geometric approximatio 0.97 0.99 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 17208 _reflns_number_total 4475 _diffrn_reflns_av_R_equivalents 0.075 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 4475 # Theoretical number of reflections is about 9027 _diffrn_reflns_theta_min 1.730 _diffrn_reflns_theta_max 25.036 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.036 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _oxford_diffrn_Wilson_B_factor 2.00 _oxford_diffrn_Wilson_scale 51.21 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.60 _refine_diff_density_max 0.62 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 4475 _refine_ls_number_restraints 0 _refine_ls_number_parameters 376 _oxford_refine_ls_R_factor_ref 0.0934 _refine_ls_wR_factor_ref 0.1221 _refine_ls_goodness_of_fit_ref 0.9997 _refine_ls_shift/su_max 0.0004307 _refine_ls_shift/su_mean 0.0000241 # The values computed from all data _oxford_reflns_number_all 4475 _refine_ls_R_factor_all 0.0934 _refine_ls_wR_factor_all 0.1221 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2830 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_gt 0.1064 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 5.75P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens C1 C 0.8564(2) 0.1418(4) 0.51241(11) 0.0301 1.0000 Uani . . . . . . . C2 C 0.7729(2) 0.2746(4) 0.50882(11) 0.0254 1.0000 Uani . . . . . . . C3 C 0.7154(2) 0.2798(4) 0.45854(11) 0.0251 1.0000 Uani . . . . . . . C4 C 0.7533(2) 0.1620(4) 0.42430(10) 0.0239 1.0000 Uani . . . . . . . C5 C 0.8476(3) 0.0677(4) 0.45877(12) 0.0296 1.0000 Uani . . . . . . . C6 C 0.7132(2) 0.1398(4) 0.37282(10) 0.0231 1.0000 Uani . . . . . . . C7 C 0.6199(2) 0.2467(4) 0.34447(10) 0.0238 1.0000 Uani . . . . . . . C8 C 0.6360(3) 0.4149(4) 0.34145(11) 0.0286 1.0000 Uani . . . . . . . C9 C 0.5514(3) 0.5155(5) 0.31491(12) 0.0341 1.0000 Uani . . . . . . . C10 C 0.4477(2) 0.4498(4) 0.29107(11) 0.0341 1.0000 Uani . . . . . . . C11 C 0.4302(3) 0.2834(5) 0.29329(12) 0.0371 1.0000 Uani . . . . . . . C12 C 0.5152(3) 0.1825(4) 0.31942(12) 0.0332 1.0000 Uani . . . . . . . C13 C 0.3550(3) 0.5569(6) 0.26338(13) 0.0474 1.0000 Uani . . . . . . . C14 C 0.8978(3) 0.4506(4) 0.60755(12) 0.0343 1.0000 Uani . . . . . . . C15 C 0.9797(3) 0.5308(5) 0.57828(16) 0.0450 1.0000 Uani . . . . . . . C16 C 0.8900(4) 0.5474(6) 0.65612(16) 0.0582 1.0000 Uani . . . . . . . C17 C 0.6655(3) 0.5840(4) 0.53778(11) 0.0290 1.0000 Uani . . . . . . . C18 C 0.7274(3) 0.7038(5) 0.50945(14) 0.0385 1.0000 Uani . . . . . . . C19 C 0.6107(3) 0.6736(5) 0.57699(14) 0.0393 1.0000 Uani . . . . . . . C20 C 0.6727(3) 0.2733(4) 0.60545(12) 0.0321 1.0000 Uani . . . . . . . C21 C 0.5583(3) 0.2192(6) 0.57381(16) 0.0540 1.0000 Uani . . . . . . . C22 C 0.7386(3) 0.1281(5) 0.63274(16) 0.0489 1.0000 Uani . . . . . . . C23 C 0.6890(3) -0.0310(5) 0.26687(13) 0.0398 1.0000 Uani . . . . . . . C24 C 0.8001(3) -0.2138(4) 0.36512(14) 0.0385 1.0000 Uani . . . . . . . C25 C 0.9202(3) 0.0709(5) 0.32769(15) 0.0405 1.0000 Uani . . . . . . . Si1 Si 0.75360(7) 0.40095(11) 0.56593(3) 0.0252 1.0000 Uani . . . . . . . O1 O 0.91947(19) 0.0926(3) 0.55214(8) 0.0468 1.0000 Uani . . . . . . . Si2 Si 0.78030(7) -0.00928(11) 0.33343(3) 0.0263 1.0000 Uani . . . . . . . O2 O 0.3609(2) 0.7030(4) 0.25979(10) 0.0620 1.0000 Uani . . . . . . . H31 H 0.656(2) 0.354(4) 0.4458(11) 0.0302 1.0000 Uiso . . . . . . . H51 H 0.914(3) 0.078(4) 0.4504(12) 0.0371 1.0000 Uiso . . . . . . . H52 H 0.831(2) -0.053(4) 0.4587(12) 0.0371 1.0000 Uiso . . . . . . . H81 H 0.706(3) 0.463(4) 0.3588(11) 0.0353 1.0000 Uiso . . . . . . . H91 H 0.560(3) 0.628(4) 0.3139(13) 0.0419 1.0000 Uiso . . . . . . . H111 H 0.357(3) 0.238(4) 0.2776(12) 0.0459 1.0000 Uiso . . . . . . . H121 H 0.498(3) 0.070(4) 0.3209(12) 0.0419 1.0000 Uiso . . . . . . . H131 H 0.284(3) 0.495(5) 0.2470(14) 0.0595 1.0000 Uiso . . . . . . . H141 H 0.924(3) 0.337(4) 0.6168(12) 0.0428 1.0000 Uiso . . . . . . . H151 H 0.989(3) 0.464(5) 0.5472(14) 0.0560 1.0000 Uiso . . . . . . . H152 H 1.052(3) 0.541(4) 0.6012(14) 0.0560 1.0000 Uiso . . . . . . . H153 H 0.956(3) 0.647(5) 0.5689(13) 0.0560 1.0000 Uiso . . . . . . . H161 H 0.834(3) 0.496(5) 0.6760(15) 0.0727 1.0000 Uiso . . . . . . . H162 H 0.967(3) 0.558(5) 0.6786(15) 0.0727 1.0000 Uiso . . . . . . . H163 H 0.859(3) 0.665(5) 0.6484(15) 0.0727 1.0000 Uiso . . . . . . . H171 H 0.606(3) 0.538(4) 0.5126(12) 0.0352 1.0000 Uiso . . . . . . . H181 H 0.765(3) 0.639(4) 0.4860(13) 0.0492 1.0000 Uiso . . . . . . . H182 H 0.789(3) 0.764(4) 0.5334(13) 0.0492 1.0000 Uiso . . . . . . . H183 H 0.674(3) 0.783(4) 0.4899(13) 0.0492 1.0000 Uiso . . . . . . . H191 H 0.564(3) 0.596(4) 0.5945(13) 0.0501 1.0000 Uiso . . . . . . . H192 H 0.669(3) 0.725(4) 0.6046(13) 0.0501 1.0000 Uiso . . . . . . . H193 H 0.563(3) 0.767(4) 0.5605(13) 0.0501 1.0000 Uiso . . . . . . . H201 H 0.664(3) 0.347(4) 0.6314(12) 0.0394 1.0000 Uiso . . . . . . . H211 H 0.514(3) 0.305(5) 0.5599(15) 0.0688 1.0000 Uiso . . . . . . . H212 H 0.515(3) 0.151(5) 0.5968(15) 0.0688 1.0000 Uiso . . . . . . . H213 H 0.565(3) 0.156(5) 0.5466(16) 0.0688 1.0000 Uiso . . . . . . . H221 H 0.815(3) 0.169(5) 0.6570(14) 0.0608 1.0000 Uiso . . . . . . . H222 H 0.694(3) 0.058(5) 0.6513(14) 0.0608 1.0000 Uiso . . . . . . . H223 H 0.755(3) 0.050(5) 0.6079(14) 0.0608 1.0000 Uiso . . . . . . . H231 H 0.728(3) -0.093(4) 0.2451(14) 0.0501 1.0000 Uiso . . . . . . . H232 H 0.669(3) 0.076(5) 0.2505(13) 0.0501 1.0000 Uiso . . . . . . . H233 H 0.618(3) -0.090(4) 0.2672(13) 0.0501 1.0000 Uiso . . . . . . . H241 H 0.816(3) -0.287(4) 0.3397(13) 0.0487 1.0000 Uiso . . . . . . . H242 H 0.870(3) -0.221(4) 0.3915(13) 0.0487 1.0000 Uiso . . . . . . . H243 H 0.733(3) -0.242(4) 0.3787(13) 0.0487 1.0000 Uiso . . . . . . . H251 H 0.953(3) -0.003(4) 0.3052(13) 0.0492 1.0000 Uiso . . . . . . . H252 H 0.968(3) 0.073(4) 0.3609(14) 0.0492 1.0000 Uiso . . . . . . . H253 H 0.916(3) 0.169(5) 0.3145(14) 0.0492 1.0000 Uiso . . . . . . . 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 0.0306(16) 0.036(2) 0.0216(16) 0.0007(15) 0.0005(13) 0.0045(15) C2 0.0249(15) 0.0292(17) 0.0206(15) -0.0009(13) 0.0017(12) 0.0010(14) C3 0.0234(15) 0.0270(17) 0.0249(16) 0.0005(14) 0.0050(12) 0.0038(14) C4 0.0225(14) 0.0262(16) 0.0222(15) -0.0025(13) 0.0030(12) -0.0017(13) C5 0.0320(17) 0.033(2) 0.0231(16) 0.0002(15) 0.0043(13) 0.0071(16) C6 0.0252(15) 0.0235(17) 0.0199(15) 0.0009(13) 0.0034(12) -0.0020(13) C7 0.0270(15) 0.0307(19) 0.0142(14) -0.0025(13) 0.0056(11) 0.0010(14) C8 0.0298(16) 0.0303(19) 0.0233(16) 0.0005(14) 0.0005(13) -0.0025(15) C9 0.0394(18) 0.036(2) 0.0281(17) 0.0095(17) 0.0109(14) 0.0073(17) C10 0.0286(16) 0.056(2) 0.0178(16) 0.0008(15) 0.0044(13) 0.0095(17) C11 0.0245(16) 0.059(3) 0.0258(17) -0.0063(17) 0.0008(13) 0.0003(17) C12 0.0304(17) 0.036(2) 0.0318(17) -0.0063(16) 0.0036(14) -0.0084(16) C13 0.041(2) 0.080(3) 0.0217(18) 0.005(2) 0.0059(15) 0.021(2) C14 0.0309(17) 0.042(2) 0.0284(17) -0.0045(16) 0.0029(14) -0.0036(16) C15 0.0317(19) 0.050(3) 0.050(2) 0.003(2) 0.0028(17) -0.0084(19) C16 0.047(2) 0.083(3) 0.040(2) -0.031(2) 0.0004(18) -0.012(2) C17 0.0299(16) 0.0314(19) 0.0240(16) -0.0018(15) 0.0023(13) 0.0009(15) C18 0.0357(19) 0.039(2) 0.040(2) 0.0071(18) 0.0067(16) 0.0026(17) C19 0.043(2) 0.037(2) 0.039(2) -0.0021(18) 0.0126(16) 0.0076(18) C20 0.0354(17) 0.038(2) 0.0225(16) 0.0000(15) 0.0051(13) -0.0014(16) C21 0.043(2) 0.069(3) 0.047(2) 0.020(2) 0.0037(18) -0.012(2) C22 0.053(2) 0.046(3) 0.049(2) 0.018(2) 0.0137(19) 0.002(2) C23 0.047(2) 0.045(2) 0.0243(18) -0.0082(17) 0.0026(15) 0.0024(19) C24 0.054(2) 0.029(2) 0.0324(19) -0.0020(16) 0.0071(17) 0.0039(18) C25 0.042(2) 0.050(2) 0.031(2) -0.0014(19) 0.0112(16) 0.0012(19) Si1 0.0260(4) 0.0314(5) 0.0173(4) -0.0020(4) 0.0028(3) 0.0007(4) O1 0.0477(14) 0.0639(18) 0.0246(12) -0.0018(12) -0.0017(10) 0.0263(13) Si2 0.0340(5) 0.0249(5) 0.0195(4) -0.0023(4) 0.0048(3) -0.0002(4) O2 0.0649(18) 0.077(2) 0.0450(16) 0.0222(16) 0.0131(13) 0.0356(17) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.14896(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . C2 . 1.476(4) yes C1 . C5 . 1.519(4) yes C1 . O1 . 1.222(3) yes C2 . C3 . 1.355(4) yes C2 . Si1 . 1.881(3) yes C3 . C4 . 1.462(4) yes C3 . H31 . 0.94(3) no C4 . C5 . 1.509(4) yes C4 . C6 . 1.348(4) yes C5 . H51 . 0.88(3) no C5 . H52 . 1.01(3) no C6 . C7 . 1.495(4) yes C6 . Si2 . 1.896(3) yes C7 . C8 . 1.396(4) yes C7 . C12 . 1.399(4) yes C8 . C9 . 1.381(4) yes C8 . H81 . 0.95(3) no C9 . C10 . 1.386(5) yes C9 . H91 . 0.93(3) no C10 . C11 . 1.383(5) yes C10 . C13 . 1.486(5) yes C11 . C12 . 1.383(5) yes C11 . H111 . 0.97(3) no C12 . H121 . 0.95(3) no C13 . O2 . 1.204(5) yes C13 . H131 . 1.01(4) no C14 . C15 . 1.532(5) yes C14 . C16 . 1.524(5) yes C14 . Si1 . 1.895(3) yes C14 . H141 . 1.00(3) no C15 . H151 . 1.01(4) no C15 . H152 . 0.95(4) no C15 . H153 . 1.01(4) no C16 . H161 . 1.03(4) no C16 . H162 . 1.00(4) no C16 . H163 . 1.04(4) no C17 . C18 . 1.525(5) yes C17 . C19 . 1.531(4) yes C17 . Si1 . 1.896(3) yes C17 . H171 . 0.95(3) no C18 . H181 . 0.99(3) no C18 . H182 . 1.00(3) no C18 . H183 . 0.98(3) no C19 . H191 . 1.02(4) no C19 . H192 . 0.99(3) no C19 . H193 . 1.00(4) no C20 . C21 . 1.520(5) yes C20 . C22 . 1.523(5) yes C20 . Si1 . 1.893(3) yes C20 . H201 . 0.93(3) no C21 . H211 . 0.91(4) no C21 . H212 . 1.05(4) no C21 . H213 . 0.90(4) no C22 . H221 . 1.06(4) no C22 . H222 . 0.99(4) no C22 . H223 . 0.97(4) no C23 . Si2 . 1.866(3) yes C23 . H231 . 0.97(4) no C23 . H232 . 0.98(4) no C23 . H233 . 0.99(4) no C24 . Si2 . 1.864(4) yes C24 . H241 . 0.95(4) no C24 . H242 . 0.98(3) no C24 . H243 . 0.99(3) no C25 . Si2 . 1.856(4) yes C25 . H251 . 0.99(4) no C25 . H252 . 0.94(3) no C25 . H253 . 0.87(4) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . C5 . 109.1(2) yes C2 . C1 . O1 . 126.2(3) yes C5 . C1 . O1 . 124.6(3) yes C1 . C2 . C3 . 106.6(3) yes C1 . C2 . Si1 . 123.9(2) yes C3 . C2 . Si1 . 129.5(2) yes C2 . C3 . C4 . 114.6(3) yes C2 . C3 . H31 . 123.9(18) no C4 . C3 . H31 . 121.5(17) no C3 . C4 . C5 . 105.5(2) yes C3 . C4 . C6 . 128.0(3) yes C5 . C4 . C6 . 126.5(3) yes C1 . C5 . C4 . 104.2(2) yes C1 . C5 . H51 . 108(2) no C4 . C5 . H51 . 114(2) no C1 . C5 . H52 . 111.5(17) no C4 . C5 . H52 . 111.9(18) no H51 . C5 . H52 . 107(3) no C4 . C6 . C7 . 119.4(3) yes C4 . C6 . Si2 . 122.2(2) yes C7 . C6 . Si2 . 118.21(19) yes C6 . C7 . C8 . 120.4(3) yes C6 . C7 . C12 . 121.7(3) yes C8 . C7 . C12 . 117.9(3) yes C7 . C8 . C9 . 121.3(3) yes C7 . C8 . H81 . 120.0(19) no C9 . C8 . H81 . 118.7(19) no C8 . C9 . C10 . 119.9(3) yes C8 . C9 . H91 . 122(2) no C10 . C9 . H91 . 118(2) no C9 . C10 . C11 . 119.8(3) yes C9 . C10 . C13 . 120.5(4) yes C11 . C10 . C13 . 119.7(3) yes C10 . C11 . C12 . 120.3(3) yes C10 . C11 . H111 . 120(2) no C12 . C11 . H111 . 120(2) no C7 . C12 . C11 . 120.8(3) yes C7 . C12 . H121 . 121.9(20) no C11 . C12 . H121 . 117.3(20) no C10 . C13 . O2 . 125.0(4) yes C10 . C13 . H131 . 114(2) no O2 . C13 . H131 . 121(2) no C15 . C14 . C16 . 111.4(3) yes C15 . C14 . Si1 . 114.8(2) yes C16 . C14 . Si1 . 112.2(2) yes C15 . C14 . H141 . 108.4(18) no C16 . C14 . H141 . 110.9(19) no Si1 . C14 . H141 . 98.4(19) no C14 . C15 . H151 . 112(2) no C14 . C15 . H152 . 109(2) no H151 . C15 . H152 . 108(3) no C14 . C15 . H153 . 110(2) no H151 . C15 . H153 . 113(3) no H152 . C15 . H153 . 105(3) no C14 . C16 . H161 . 112(2) no C14 . C16 . H162 . 109(2) no H161 . C16 . H162 . 112(3) no C14 . C16 . H163 . 114(2) no H161 . C16 . H163 . 103(3) no H162 . C16 . H163 . 107(3) no C18 . C17 . C19 . 110.7(3) yes C18 . C17 . Si1 . 113.9(2) yes C19 . C17 . Si1 . 114.0(2) yes C18 . C17 . H171 . 107.2(18) no C19 . C17 . H171 . 106.6(18) no Si1 . C17 . H171 . 103.8(19) no C17 . C18 . H181 . 107.4(20) no C17 . C18 . H182 . 112.9(19) no H181 . C18 . H182 . 106(3) no C17 . C18 . H183 . 110.2(19) no H181 . C18 . H183 . 111(3) no H182 . C18 . H183 . 109(3) no C17 . C19 . H191 . 111.5(19) no C17 . C19 . H192 . 110.5(19) no H191 . C19 . H192 . 108(3) no C17 . C19 . H193 . 111.8(19) no H191 . C19 . H193 . 110(3) no H192 . C19 . H193 . 104(3) no C21 . C20 . C22 . 110.7(3) yes C21 . C20 . Si1 . 112.4(2) yes C22 . C20 . Si1 . 114.1(2) yes C21 . C20 . H201 . 110.5(19) no C22 . C20 . H201 . 106.9(19) no Si1 . C20 . H201 . 101.8(19) no C20 . C21 . H211 . 113(3) no C20 . C21 . H212 . 111(2) no H211 . C21 . H212 . 108(3) no C20 . C21 . H213 . 112(3) no H211 . C21 . H213 . 106(4) no H212 . C21 . H213 . 107(3) no C20 . C22 . H221 . 110(2) no C20 . C22 . H222 . 114(2) no H221 . C22 . H222 . 113(3) no C20 . C22 . H223 . 111(2) no H221 . C22 . H223 . 109(3) no H222 . C22 . H223 . 100(3) no Si2 . C23 . H231 . 109.8(20) no Si2 . C23 . H232 . 111(2) no H231 . C23 . H232 . 108(3) no Si2 . C23 . H233 . 112.2(19) no H231 . C23 . H233 . 107(3) no H232 . C23 . H233 . 108(3) no Si2 . C24 . H241 . 106(2) no Si2 . C24 . H242 . 112(2) no H241 . C24 . H242 . 101(3) no Si2 . C24 . H243 . 110(2) no H241 . C24 . H243 . 115(3) no H242 . C24 . H243 . 113(3) no Si2 . C25 . H251 . 109.0(19) no Si2 . C25 . H252 . 109(2) no H251 . C25 . H252 . 109(3) no Si2 . C25 . H253 . 112(2) no H251 . C25 . H253 . 109(3) no H252 . C25 . H253 . 109(3) no C17 . Si1 . C14 . 115.25(16) yes C17 . Si1 . C20 . 109.65(14) yes C14 . Si1 . C20 . 108.95(14) yes C17 . Si1 . C2 . 106.29(13) yes C14 . Si1 . C2 . 108.69(13) yes C20 . Si1 . C2 . 107.74(15) yes C6 . Si2 . C23 . 109.71(15) yes C6 . Si2 . C24 . 111.29(15) yes C23 . Si2 . C24 . 109.06(18) yes C6 . Si2 . C25 . 109.01(16) yes C23 . Si2 . C25 . 108.86(18) yes C24 . Si2 . C25 . 108.87(18) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 Si1 C14 C15 171.0(2) . . . . no C2 Si1 C14 C16 -177.7(3) . . . . no C17 Si1 C14 C16 63.2(3) . . . . no C20 Si1 C14 C16 -60.6(3) . . . . no C2 Si1 C17 C18 -69.3(3) . . . . no C14 Si1 C17 C18 51.2(3) . . . . no C14 Si1 C2 C1 41.2(3) . . . . no C17 Si1 C2 C1 165.8(2) . . . . no C20 Si1 C2 C1 -76.7(3) . . . . no C14 Si1 C2 C3 -141.0(3) . . . . no C17 Si1 C2 C3 -16.3(3) . . . . no C20 Si1 C2 C3 101.1(3) . . . . no C17 Si1 C20 C21 56.5(3) . . . . no C2 Si1 C14 C15 53.8(3) . . . . no C17 Si1 C14 C15 -65.3(3) . . . . no C17 Si1 C20 C22 -176.4(2) . . . . no C14 Si1 C17 C19 -77.1(3) . . . . no C20 Si1 C17 C19 46.2(3) . . . . no C2 Si1 C20 C21 -58.8(3) . . . . no C14 Si1 C20 C21 -176.5(3) . . . . no C14 Si1 C20 C22 -49.4(3) . . . . no C20 Si1 C17 C18 174.5(2) . . . . no C2 Si1 C17 C19 162.4(2) . . . . no C2 Si1 C20 C22 68.3(3) . . . . no C24 Si2 C6 C7 -135.7(2) . . . . no C23 Si2 C6 C4 171.0(3) . . . . no C25 Si2 C6 C4 -69.9(3) . . . . no C23 Si2 C6 C7 -14.9(3) . . . . no C24 Si2 C6 C4 50.2(3) . . . . no C25 Si2 C6 C7 104.2(2) . . . . no O1 C1 C2 C3 -175.2(3) . . . . no C5 C1 C2 Si1 180.0(2) . . . . no C5 C1 C2 C3 1.7(3) . . . . no O1 C1 C2 Si1 3.1(4) . . . . no C2 C1 C5 C4 -1.1(3) . . . . no O1 C1 C5 C4 175.8(3) . . . . no Si1 C2 C3 C4 -179.8(2) . . . . no C1 C2 C3 C4 -1.7(3) . . . . no C2 C3 C4 C6 -179.4(3) . . . . no C2 C3 C4 C5 0.9(4) . . . . no C6 C4 C5 C1 -179.5(3) . . . . no C3 C4 C6 Si2 175.3(2) . . . . no C3 C4 C5 C1 0.2(3) . . . . no C5 C4 C6 Si2 -5.1(4) . . . . no C5 C4 C6 C7 -179.1(3) . . . . no C3 C4 C6 C7 1.3(5) . . . . no C4 C6 C7 C12 -118.9(3) . . . . no C4 C6 C7 C8 62.4(4) . . . . no Si2 C6 C7 C8 -111.9(3) . . . . no Si2 C6 C7 C12 66.9(3) . . . . no C12 C7 C8 C9 0.4(4) . . . . no C6 C7 C8 C9 179.2(3) . . . . no C6 C7 C12 C11 -179.8(3) . . . . no C8 C7 C12 C11 -1.0(4) . . . . no C7 C8 C9 C10 0.6(5) . . . . no C8 C9 C10 C11 -1.1(5) . . . . no C8 C9 C10 C13 178.6(3) . . . . no C13 C10 C11 C12 -179.3(3) . . . . no C9 C10 C11 C12 0.4(5) . . . . no C9 C10 C13 O2 -0.8(5) . . . . no C11 C10 C13 O2 178.9(3) . . . . no C10 C11 C12 C7 0.6(5) . . . . no