# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address J.S.Silvia ; Department of Chemistry, Massachusetts Institute of Technology, 77 Massachusetts Avenue, Cambridge, MA, USA, 02139. ; 'Cummins, C. C.' ; Department of Chemistry, Massachusetts Institute of Technology, 77 Massachusetts Avenue, Cambridge, MA, USA, 02139. ; _publ_contact_author_address ; Department of Chemistry, Massachusetts Institute of Technology, 77 Massachusetts Avenue, Cambridge, MA, USA, 02139. ; _publ_contact_author_email ccummins@mit.edu _publ_contact_author_fax 6172537670 _publ_contact_author_phone 6172535332 _publ_contact_author_name 'Prof. Christopher C. Cummins' _publ_section_title ;Binding, Release, and Functionalization of CO2 at a Nucleophilic Oxo Anion Complex of Titanium ; data_LiO2COTi(N[tBu]Ar)3 _database_code_depnum_ccdc_archive 'CCDC 819846' _publ_section_abstract ; ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C37 H54 Li N3 O3 Ti, 1.33(C6 H6)' _chemical_formula_sum 'C45 H62 Li N3 O3 Ti' _chemical_properties_physical 'air-sensitive, moisture-sensitive' _exptl_crystal_recrystallization_method 'slow evaporation of benzene' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 747.82 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' Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_int_tables_number 148 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 30.8490(6) _cell_length_b 30.8490(6) _cell_length_c 23.5478(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 19407.2(7) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9867 _cell_measurement_theta_min 4.76 _cell_measurement_theta_max 68.00 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7236 _exptl_absorpt_coefficient_mu 1.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8260 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_radiation_probe ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 46114 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 68.22 _reflns_number_total 7754 _reflns_number_gt 6044 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+36.7732P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7754 _refine_ls_number_parameters 634 _refine_ls_number_restraints 768 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1485 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.002 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 Ti1 Ti 0.481639(17) 0.169682(17) 0.46808(2) 0.02975(15) Uani 1 1 d . . . Li1 Li 0.59925(18) 0.32956(17) 0.3733(2) 0.0372(11) Uani 1 1 d . . . N1 N 0.46017(9) 0.21263(9) 0.50168(11) 0.0369(5) Uani 1 1 d . . . N2 N 0.43063(8) 0.12576(8) 0.41536(10) 0.0330(5) Uani 1 1 d . . . N3 N 0.48571(8) 0.12879(8) 0.52710(10) 0.0324(5) Uani 1 1 d . . . O4 O 0.54304(7) 0.20644(7) 0.43266(8) 0.0357(4) Uani 1 1 d . . . O411 O 0.62223(7) 0.22452(7) 0.42638(9) 0.0394(5) Uani 1 1 d . . . O412 O 0.59610(7) 0.26715(7) 0.37546(8) 0.0334(4) Uani 1 1 d . . . C11 C 0.40798(11) 0.19789(10) 0.50216(14) 0.0373(6) Uani 1 1 d . . . C12 C 0.37830(11) 0.17153(10) 0.54866(14) 0.0391(7) Uani 1 1 d . . . H12 H 0.3929 0.1635 0.5796 0.047 Uiso 1 1 calc R . . C13 C 0.32757(11) 0.15682(11) 0.55027(14) 0.0423(7) Uani 1 1 d . . . C14 C 0.30693(12) 0.16830(13) 0.50438(16) 0.0508(8) Uani 1 1 d . . . H14 H 0.2723 0.1580 0.5049 0.061 Uiso 1 1 calc R . . C15 C 0.33562(13) 0.19440(14) 0.45782(17) 0.0536(9) Uani 1 1 d . . . C16 C 0.38621(12) 0.20887(12) 0.45717(16) 0.0460(8) Uani 1 1 d . . . H16 H 0.4061 0.2266 0.4253 0.055 Uiso 1 1 calc R . . C17 C 0.49334(12) 0.26473(11) 0.52438(15) 0.0437(7) Uani 1 1 d . . . C21 C 0.39185(10) 0.07747(10) 0.43441(12) 0.0337(6) Uani 1 1 d . . . C22 C 0.39793(11) 0.03576(11) 0.43265(13) 0.0392(7) Uani 1 1 d . . . H22 H 0.4281 0.0391 0.4179 0.047 Uiso 1 1 calc R . . C23 C 0.36090(12) -0.01055(11) 0.45190(14) 0.0438(7) Uani 1 1 d . . . C24 C 0.31664(12) -0.01498(11) 0.47281(13) 0.0443(7) Uani 1 1 d . . . H24 H 0.2910 -0.0466 0.4861 0.053 Uiso 1 1 calc R . . C25 C 0.30933(11) 0.02557(12) 0.47467(13) 0.0415(7) Uani 1 1 d . . . C26 C 0.34732(11) 0.07197(11) 0.45559(12) 0.0364(6) Uani 1 1 d . . . H26 H 0.3427 0.1002 0.4571 0.044 Uiso 1 1 calc R . . C27 C 0.42806(12) 0.13584(12) 0.35344(13) 0.0428(7) Uani 1 1 d . . . C31 C 0.45876(10) 0.12199(11) 0.57924(12) 0.0342(6) Uani 1 1 d . . . C32 C 0.48009(11) 0.15517(12) 0.62421(13) 0.0399(7) Uani 1 1 d . . . H32 H 0.5128 0.1832 0.6202 0.048 Uiso 1 1 calc R . . C33 C 0.45439(12) 0.14807(13) 0.67507(13) 0.0432(7) Uani 1 1 d . . . C34 C 0.40649(12) 0.10721(13) 0.68016(13) 0.0436(7) Uani 1 1 d . . . H34 H 0.3886 0.1023 0.7146 0.052 Uiso 1 1 calc R . . C35 C 0.38397(11) 0.07319(12) 0.63585(13) 0.0398(7) Uani 1 1 d . . . C36 C 0.41045(10) 0.08115(11) 0.58516(12) 0.0350(6) Uani 1 1 d . . . H36 H 0.3954 0.0585 0.5544 0.042 Uiso 1 1 calc R . . C37 C 0.51892(11) 0.10591(11) 0.52762(13) 0.0364(6) Uani 1 1 d . . . C41 C 0.58863(10) 0.23294(10) 0.41195(12) 0.0311(6) Uani 1 1 d . . . C131 C 0.29621(12) 0.12892(13) 0.60156(16) 0.0506(8) Uani 1 1 d . . . H13A H 0.2910 0.1520 0.6254 0.076 Uiso 1 1 calc R . . H13B H 0.3136 0.1152 0.6235 0.076 Uiso 1 1 calc R . . H13C H 0.2637 0.1015 0.5889 0.076 Uiso 1 1 calc R . . C151 C 0.31302(16) 0.2070(2) 0.4075(2) 0.0837(15) Uani 1 1 d . . . H15A H 0.2786 0.1984 0.4167 0.126 Uiso 1 1 calc R . . H15B H 0.3128 0.1878 0.3743 0.126 Uiso 1 1 calc R . . H15C H 0.3330 0.2428 0.3992 0.126 Uiso 1 1 calc R . . C171 C 0.54695(12) 0.27450(13) 0.52899(17) 0.0534(9) Uani 1 1 d . . . H17A H 0.5469 0.2465 0.5488 0.080 Uiso 1 1 calc R . . H17B H 0.5674 0.3055 0.5502 0.080 Uiso 1 1 calc R . . H17C H 0.5609 0.2777 0.4908 0.080 Uiso 1 1 calc R . . C172 C 0.47614(14) 0.27025(13) 0.58343(16) 0.0538(9) Uani 1 1 d . . . H17D H 0.4422 0.2653 0.5810 0.081 Uiso 1 1 calc R . . H17E H 0.4990 0.3038 0.5981 0.081 Uiso 1 1 calc R . . H17F H 0.4762 0.2452 0.6090 0.081 Uiso 1 1 calc R . . C173 C 0.49267(13) 0.30295(12) 0.48421(16) 0.0526(9) Uani 1 1 d . . . H17G H 0.5032 0.2988 0.4463 0.079 Uiso 1 1 calc R . . H17H H 0.5157 0.3368 0.4982 0.079 Uiso 1 1 calc R . . H17I H 0.4587 0.2979 0.4823 0.079 Uiso 1 1 calc R . . C231 C 0.36850(15) -0.05524(13) 0.4495(2) 0.0630(10) Uani 1 1 d . . . H23A H 0.3741 -0.0636 0.4880 0.095 Uiso 1 1 calc R . . H23B H 0.3977 -0.0473 0.4258 0.095 Uiso 1 1 calc R . . H23C H 0.3387 -0.0839 0.4333 0.095 Uiso 1 1 calc R . . C251 C 0.26084(12) 0.02045(13) 0.49679(16) 0.0523(8) Uani 1 1 d . . . H25A H 0.2336 -0.0141 0.4914 0.078 Uiso 1 1 calc R . . H25B H 0.2532 0.0433 0.4760 0.078 Uiso 1 1 calc R . . H25C H 0.2644 0.0288 0.5373 0.078 Uiso 1 1 calc R . . C271 C 0.44269(15) 0.10406(16) 0.31786(15) 0.0593(9) Uani 1 1 d . . . H27A H 0.4767 0.1119 0.3280 0.089 Uiso 1 1 calc R . . H27B H 0.4416 0.1113 0.2775 0.089 Uiso 1 1 calc R . . H27C H 0.4192 0.0685 0.3251 0.089 Uiso 1 1 calc R . . C272 C 0.37520(12) 0.12422(14) 0.33638(15) 0.0530(9) Uani 1 1 d . . . H27D H 0.3513 0.0889 0.3440 0.079 Uiso 1 1 calc R . . H27E H 0.3747 0.1311 0.2958 0.079 Uiso 1 1 calc R . . H27F H 0.3659 0.1453 0.3585 0.079 Uiso 1 1 calc R . . C273 C 0.46399(13) 0.19105(13) 0.34094(15) 0.0543(9) Uani 1 1 d . . . H27G H 0.4567 0.2117 0.3665 0.081 Uiso 1 1 calc R . . H27H H 0.4598 0.1983 0.3015 0.081 Uiso 1 1 calc R . . H27I H 0.4985 0.1986 0.3469 0.081 Uiso 1 1 calc R . . C331 C 0.47896(14) 0.18510(15) 0.72293(15) 0.0566(9) Uani 1 1 d . . . H33A H 0.5111 0.1876 0.7323 0.085 Uiso 1 1 calc R . . H33B H 0.4571 0.1737 0.7564 0.085 Uiso 1 1 calc R . . H33C H 0.4846 0.2180 0.7111 0.085 Uiso 1 1 calc R . . C351 C 0.33222(12) 0.02845(13) 0.64206(15) 0.0493(8) Uani 1 1 d . . . H35A H 0.3328 0.0055 0.6704 0.074 Uiso 1 1 calc R . . H35B H 0.3212 0.0112 0.6055 0.074 Uiso 1 1 calc R . . H35C H 0.3090 0.0396 0.6544 0.074 Uiso 1 1 calc R . . C371 C 0.53592(11) 0.10393(11) 0.46737(13) 0.0390(7) Uani 1 1 d . . . H37A H 0.5067 0.0876 0.4424 0.059 Uiso 1 1 calc R . . H37B H 0.5536 0.0849 0.4672 0.059 Uiso 1 1 calc R . . H37C H 0.5584 0.1380 0.4538 0.059 Uiso 1 1 calc R . . C372 C 0.56507(13) 0.13808(16) 0.56402(17) 0.0596(10) Uani 1 1 d . . . H37D H 0.5818 0.1727 0.5501 0.089 Uiso 1 1 calc R . . H37E H 0.5881 0.1250 0.5617 0.089 Uiso 1 1 calc R . . H37F H 0.5549 0.1373 0.6036 0.089 Uiso 1 1 calc R . . C373 C 0.49049(13) 0.05229(13) 0.55043(15) 0.0505(8) Uani 1 1 d . . . H37G H 0.4824 0.0528 0.5906 0.076 Uiso 1 1 calc R . . H37H H 0.5114 0.0368 0.5465 0.076 Uiso 1 1 calc R . . H37I H 0.4595 0.0329 0.5288 0.076 Uiso 1 1 calc R . . C1T C 0.5780(4) 0.15557(14) 0.77758(17) 0.066(4) Uani 0.33 1 d PRDU A -1 H1T H 0.5512 0.1555 0.7975 0.080 Uiso 0.33 1 calc PR B -1 C2T C 0.5719(5) 0.1340(5) 0.7215(4) 0.065(3) Uani 0.33 1 d PDU A -1 H2T H 0.5400 0.1186 0.7038 0.078 Uiso 0.33 1 calc PR A -1 C3T C 0.6126(5) 0.1357(7) 0.6932(6) 0.087(4) Uani 0.33 1 d PDU A -1 H3T H 0.6082 0.1209 0.6568 0.104 Uiso 0.33 1 calc PR A -1 C4T C 0.6591(5) 0.1590(6) 0.7183(6) 0.097(5) Uani 0.33 1 d PDU A -1 H4T H 0.6872 0.1614 0.6989 0.116 Uiso 0.33 1 calc PR A -1 C5T C 0.6642(5) 0.1785(6) 0.7718(6) 0.095(4) Uani 0.33 1 d PDU A -1 H5T H 0.6961 0.1942 0.7897 0.113 Uiso 0.33 1 calc PR A -1 C6T C 0.6242(5) 0.1757(6) 0.7994(7) 0.081(4) Uani 0.33 1 d PDU A -1 H6T H 0.6294 0.1888 0.8369 0.097 Uiso 0.33 1 calc PR A -1 C1U C 0.7909(6) 0.4171(6) 0.8085(6) 0.096(7) Uani 0.33 1 d PDU C -3 H1U H 0.7960 0.4196 0.8484 0.116 Uiso 0.33 1 calc PR C -3 C2U C 0.8239(6) 0.4549(5) 0.7737(5) 0.083(5) Uani 0.33 1 d PDU C -3 H2U H 0.8516 0.4840 0.7893 0.099 Uiso 0.33 1 calc PR C -3 C3U C 0.8164(5) 0.4501(6) 0.7159(5) 0.078(4) Uani 0.33 1 d PDU C -3 H3U H 0.8380 0.4768 0.6915 0.094 Uiso 0.33 1 calc PR C -3 C4U C 0.7787(4) 0.4078(5) 0.6935(5) 0.077(3) Uani 0.33 1 d PDU C -3 H4U H 0.7758 0.4035 0.6534 0.093 Uiso 0.33 1 calc PR C -3 C5U C 0.7448(5) 0.3709(5) 0.7282(5) 0.080(4) Uani 0.33 1 d PDU C -3 H5U H 0.7171 0.3420 0.7123 0.096 Uiso 0.33 1 calc PR C -3 C6U C 0.7505(4) 0.3755(4) 0.7857(4) 0.062(3) Uani 0.33 1 d PDU C -3 H6U H 0.7266 0.3501 0.8098 0.074 Uiso 0.33 1 calc PR C -3 C1S C 0.6696(9) 0.3418(9) 0.6099(6) 0.114(5) Uani 0.33 1 d PDU D -2 H1S H 0.6586 0.3238 0.5752 0.137 Uiso 0.33 1 calc PR D -2 C2S C 0.6406(7) 0.3584(7) 0.6378(7) 0.113(6) Uani 0.33 1 d PDU D -2 H2S H 0.6092 0.3513 0.6227 0.135 Uiso 0.33 1 calc PR D -2 C3S C 0.6581(5) 0.3851(7) 0.6873(6) 0.102(5) Uani 0.33 1 d PDU D -2 H3S H 0.6385 0.3954 0.7081 0.123 Uiso 0.33 1 calc PR D -2 C4S C 0.7039(5) 0.3961(6) 0.7054(6) 0.088(4) Uani 0.33 1 d PDU D -2 H4S H 0.7175 0.4187 0.7364 0.106 Uiso 0.33 1 calc PR D -2 C5S C 0.7318(6) 0.3784(7) 0.6839(7) 0.100(4) Uani 0.33 1 d PDU D -2 H5S H 0.7615 0.3835 0.7021 0.121 Uiso 0.33 1 calc PR D -2 C6S C 0.7151(9) 0.3523(8) 0.6341(8) 0.112(5) Uani 0.33 1 d PDU D -2 H6S H 0.7350 0.3411 0.6156 0.134 Uiso 0.33 1 calc PR D -2 C1V C 0.5670(7) 0.4221(7) 0.7548(9) 0.105(6) Uani 0.33 1 d PDU E -4 H1V H 0.5718 0.4546 0.7479 0.126 Uiso 0.33 1 calc PR E -4 C2V C 0.5871(8) 0.4123(9) 0.8016(9) 0.151(8) Uani 0.33 1 d PDU E -4 H2V H 0.6079 0.4388 0.8266 0.181 Uiso 0.33 1 calc PR E -4 C3V C 0.5775(10) 0.3648(10) 0.8127(10) 0.140(9) Uani 0.33 1 d PDU E -4 H3V H 0.5930 0.3589 0.8444 0.168 Uiso 0.33 1 calc PR E -4 C4V C 0.5461(9) 0.3258(8) 0.7788(9) 0.148(8) Uani 0.33 1 d PDU E -4 H4V H 0.5387 0.2927 0.7875 0.178 Uiso 0.33 1 calc PR E -4 C5V C 0.5253(8) 0.3348(7) 0.7318(8) 0.114(7) Uani 0.33 1 d PDU E -4 H5V H 0.5013 0.3077 0.7096 0.136 Uiso 0.33 1 calc PR E -4 C6V C 0.5390(9) 0.3824(6) 0.7175(8) 0.113(6) Uani 0.33 1 d PDU E -4 H6V H 0.5295 0.3891 0.6816 0.136 Uiso 0.33 1 calc PR E -4 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 Ti1 0.0251(3) 0.0273(3) 0.0355(3) 0.00041(19) 0.00177(19) 0.0121(2) Li1 0.039(3) 0.029(2) 0.044(3) -0.001(2) 0.001(2) 0.018(2) N1 0.0311(12) 0.0304(12) 0.0484(15) -0.0042(10) 0.0035(10) 0.0148(10) N2 0.0303(12) 0.0305(12) 0.0356(13) 0.0014(10) -0.0015(9) 0.0131(10) N3 0.0290(11) 0.0332(12) 0.0349(13) 0.0009(9) 0.0009(9) 0.0155(10) O4 0.0270(9) 0.0355(10) 0.0423(11) 0.0039(8) 0.0039(8) 0.0138(8) O411 0.0293(10) 0.0390(11) 0.0501(13) 0.0088(9) 0.0023(9) 0.0172(9) O412 0.0329(10) 0.0267(9) 0.0408(11) 0.0023(8) 0.0025(8) 0.0151(8) C11 0.0326(14) 0.0266(13) 0.0539(18) -0.0008(12) 0.0053(13) 0.0157(12) C12 0.0355(15) 0.0315(14) 0.0513(18) -0.0018(13) 0.0046(13) 0.0176(12) C13 0.0357(16) 0.0339(15) 0.057(2) -0.0022(13) 0.0053(14) 0.0176(13) C14 0.0316(16) 0.0506(19) 0.073(2) 0.0058(17) 0.0059(15) 0.0228(15) C15 0.0460(19) 0.056(2) 0.070(2) 0.0132(17) 0.0059(17) 0.0339(17) C16 0.0384(16) 0.0397(16) 0.063(2) 0.0105(15) 0.0084(15) 0.0220(14) C17 0.0379(16) 0.0316(15) 0.057(2) -0.0077(14) 0.0045(14) 0.0142(13) C21 0.0317(14) 0.0313(14) 0.0327(15) -0.0029(11) -0.0064(11) 0.0117(12) C22 0.0349(15) 0.0360(15) 0.0424(17) -0.0037(13) -0.0071(12) 0.0144(13) C23 0.0421(17) 0.0326(15) 0.0515(19) -0.0020(13) -0.0105(14) 0.0147(13) C24 0.0426(17) 0.0319(15) 0.0430(18) 0.0038(13) -0.0061(13) 0.0070(13) C25 0.0365(16) 0.0398(16) 0.0386(17) -0.0016(13) -0.0042(12) 0.0117(13) C26 0.0359(15) 0.0336(15) 0.0365(16) -0.0008(12) -0.0044(12) 0.0148(12) C27 0.0388(16) 0.0435(17) 0.0365(16) 0.0053(13) -0.0028(13) 0.0134(14) C31 0.0319(14) 0.0371(15) 0.0368(15) 0.0018(12) 0.0000(11) 0.0197(12) C32 0.0333(15) 0.0462(17) 0.0401(17) -0.0014(13) -0.0017(12) 0.0199(13) C33 0.0443(17) 0.0569(19) 0.0359(17) -0.0030(14) -0.0008(13) 0.0309(16) C34 0.0449(17) 0.059(2) 0.0348(16) 0.0053(14) 0.0054(13) 0.0315(16) C35 0.0369(15) 0.0443(17) 0.0420(17) 0.0100(13) 0.0040(13) 0.0231(14) C36 0.0335(14) 0.0375(15) 0.0367(16) 0.0026(12) -0.0007(12) 0.0198(13) C37 0.0327(14) 0.0407(16) 0.0407(16) 0.0019(12) 0.0018(12) 0.0221(13) C41 0.0292(14) 0.0247(13) 0.0360(15) -0.0018(11) 0.0002(11) 0.0109(11) C131 0.0415(17) 0.0446(18) 0.065(2) 0.0044(16) 0.0122(15) 0.0209(15) C151 0.058(2) 0.116(4) 0.097(3) 0.042(3) 0.013(2) 0.058(3) C171 0.0384(17) 0.0423(18) 0.069(2) -0.0174(16) -0.0011(16) 0.0120(15) C172 0.051(2) 0.0409(18) 0.062(2) -0.0141(16) 0.0013(16) 0.0172(15) C173 0.0466(19) 0.0332(16) 0.072(2) -0.0031(15) 0.0107(17) 0.0153(15) C231 0.053(2) 0.0348(18) 0.095(3) 0.0031(18) -0.006(2) 0.0169(16) C251 0.0405(18) 0.0490(19) 0.056(2) -0.0007(16) 0.0050(15) 0.0136(15) C271 0.062(2) 0.074(3) 0.0367(18) -0.0018(17) 0.0030(16) 0.030(2) C272 0.0426(18) 0.054(2) 0.049(2) 0.0108(16) -0.0086(15) 0.0142(16) C273 0.0429(18) 0.054(2) 0.049(2) 0.0178(16) -0.0037(15) 0.0114(16) C331 0.052(2) 0.074(2) 0.0439(19) -0.0137(17) -0.0040(15) 0.0311(19) C351 0.0440(18) 0.0520(19) 0.052(2) 0.0152(15) 0.0111(15) 0.0239(16) C371 0.0384(15) 0.0358(15) 0.0480(18) 0.0024(13) 0.0071(13) 0.0223(13) C372 0.0412(18) 0.082(3) 0.068(2) -0.025(2) -0.0144(17) 0.0398(19) C373 0.053(2) 0.055(2) 0.057(2) 0.0180(16) 0.0147(16) 0.0373(17) C1T 0.070(6) 0.078(10) 0.060(7) 0.029(7) 0.007(6) 0.045(7) C2T 0.075(7) 0.089(9) 0.057(7) 0.030(6) 0.002(5) 0.059(7) C3T 0.101(8) 0.135(13) 0.059(7) 0.042(7) 0.020(6) 0.084(9) C4T 0.080(7) 0.130(13) 0.099(9) 0.068(9) 0.031(7) 0.067(9) C5T 0.059(6) 0.108(11) 0.096(9) 0.067(8) 0.008(6) 0.026(7) C6T 0.074(7) 0.070(9) 0.078(9) 0.024(7) -0.003(6) 0.021(7) C1U 0.119(13) 0.071(9) 0.046(6) -0.014(6) 0.002(7) 0.007(8) C2U 0.094(11) 0.053(7) 0.064(6) -0.010(6) -0.005(7) 0.008(6) C3U 0.055(7) 0.104(9) 0.062(6) 0.019(6) 0.000(6) 0.029(6) C4U 0.062(7) 0.121(9) 0.044(5) -0.006(5) -0.014(4) 0.043(6) C5U 0.062(7) 0.086(7) 0.074(6) -0.009(6) -0.032(5) 0.024(5) C6U 0.066(6) 0.051(5) 0.064(5) 0.004(5) 0.002(5) 0.027(4) C1S 0.136(13) 0.131(16) 0.112(8) -0.041(10) -0.058(10) 0.094(12) C2S 0.129(12) 0.135(15) 0.125(13) -0.007(10) -0.050(9) 0.103(11) C3S 0.084(8) 0.156(14) 0.086(10) 0.005(9) 0.014(7) 0.075(10) C4S 0.091(8) 0.109(10) 0.088(9) 0.001(7) -0.002(6) 0.068(8) C5S 0.094(8) 0.125(10) 0.110(10) -0.037(8) -0.035(7) 0.076(8) C6S 0.129(11) 0.112(12) 0.140(12) -0.053(10) -0.054(10) 0.095(11) C1V 0.096(14) 0.099(10) 0.116(15) -0.008(10) 0.045(13) 0.047(9) C2V 0.142(18) 0.160(14) 0.137(17) 0.010(14) 0.025(13) 0.065(15) C3V 0.140(19) 0.157(16) 0.097(15) 0.018(12) 0.013(11) 0.054(15) C4V 0.145(17) 0.148(13) 0.096(13) 0.032(10) 0.010(11) 0.031(13) C5V 0.130(16) 0.088(8) 0.091(12) 0.022(9) 0.023(10) 0.031(11) C6V 0.129(16) 0.078(10) 0.117(14) 0.001(8) 0.052(11) 0.039(11) _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 Ti1 O4 1.8497(19) . ? Ti1 N3 1.923(2) . ? Ti1 N1 1.923(2) . ? Ti1 N2 1.929(2) . ? Li1 O412 1.879(5) . ? Li1 O411 1.909(5) 3_665 ? Li1 O412 1.947(5) 17 ? Li1 O412 2.256(5) 3_665 ? Li1 C41 2.371(5) 3_665 ? Li1 Li1 2.764(8) 17 ? Li1 Li1 2.764(8) 18_545 ? Li1 Li1 3.506(8) 2_655 ? Li1 Li1 3.506(8) 3_665 ? N1 C11 1.438(4) . ? N1 C17 1.507(4) . ? N2 C21 1.439(4) . ? N2 C27 1.501(4) . ? N3 C31 1.438(4) . ? N3 C37 1.507(3) . ? O4 C41 1.317(3) . ? O411 C41 1.235(3) . ? O411 Li1 1.909(5) 2_655 ? O412 C41 1.289(3) . ? O412 Li1 1.947(5) 18_545 ? O412 Li1 2.256(5) 2_655 ? C11 C16 1.384(5) . ? C11 C12 1.398(4) . ? C12 C13 1.395(4) . ? C13 C14 1.387(5) . ? C13 C131 1.518(5) . ? C14 C15 1.386(5) . ? C15 C16 1.392(5) . ? C15 C151 1.520(5) . ? C17 C173 1.520(5) . ? C17 C172 1.528(5) . ? C17 C171 1.529(5) . ? C21 C26 1.390(4) . ? C21 C22 1.390(4) . ? C22 C23 1.385(4) . ? C23 C24 1.393(5) . ? C23 C231 1.511(5) . ? C24 C25 1.378(5) . ? C25 C26 1.395(4) . ? C25 C251 1.516(5) . ? C27 C271 1.520(5) . ? C27 C273 1.526(4) . ? C27 C272 1.538(4) . ? C31 C32 1.389(4) . ? C31 C36 1.397(4) . ? C32 C33 1.392(4) . ? C33 C34 1.387(5) . ? C33 C331 1.511(5) . ? C34 C35 1.394(5) . ? C35 C36 1.397(4) . ? C35 C351 1.507(4) . ? C37 C371 1.524(4) . ? C37 C372 1.528(4) . ? C37 C373 1.531(4) . ? C41 Li1 2.371(5) 2_655 ? C1T C6T 1.342(12) . ? C1T C2T 1.447(11) . ? C2T C3T 1.399(12) . ? C3T C4T 1.375(13) . ? C4T C5T 1.370(13) . ? C5T C6T 1.358(13) . ? C1U C2U 1.371(13) . ? C1U C6U 1.375(13) . ? C2U C3U 1.378(12) . ? C3U C4U 1.348(12) . ? C4U C5U 1.367(12) . ? C5U C6U 1.362(11) . ? C1S C6S 1.395(13) . ? C1S C2S 1.396(13) . ? C2S C3S 1.371(13) . ? C3S C4S 1.345(12) . ? C4S C5S 1.327(12) . ? C5S C6S 1.368(13) . ? C1V C2V 1.372(13) . ? C1V C6V 1.398(13) . ? C2V C3V 1.367(14) . ? C3V C4V 1.364(14) . ? C4V C5V 1.375(13) . ? C5V C6V 1.353(13) . ? 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 O4 Ti1 N3 110.20(9) . . ? O4 Ti1 N1 111.29(9) . . ? N3 Ti1 N1 108.21(11) . . ? O4 Ti1 N2 111.48(10) . . ? N3 Ti1 N2 107.59(10) . . ? N1 Ti1 N2 107.93(10) . . ? O412 Li1 O411 137.5(3) . 3_665 ? O412 Li1 O412 98.5(2) . 17 ? O411 Li1 O412 124.0(3) 3_665 17 ? O412 Li1 O412 124.2(3) . 3_665 ? O411 Li1 O412 63.40(16) 3_665 3_665 ? O412 Li1 O412 86.9(2) 17 3_665 ? O412 Li1 C41 141.5(3) . 3_665 ? O411 Li1 C41 31.24(11) 3_665 3_665 ? O412 Li1 C41 106.3(2) 17 3_665 ? O412 Li1 C41 32.23(10) 3_665 3_665 ? O412 Li1 Li1 116.3(2) . 17 ? O411 Li1 Li1 96.9(2) 3_665 17 ? O412 Li1 Li1 42.8(2) 17 17 ? O412 Li1 Li1 44.22(9) 3_665 17 ? C41 Li1 Li1 69.06(15) 3_665 17 ? O412 Li1 Li1 44.74(10) . 18_545 ? O411 Li1 Li1 175.0(2) 3_665 18_545 ? O412 Li1 Li1 53.9(2) 17 18_545 ? O412 Li1 Li1 111.65(17) 3_665 18_545 ? C41 Li1 Li1 143.8(2) 3_665 18_545 ? Li1 Li1 Li1 78.7(3) 17 18_545 ? O412 Li1 Li1 35.45(16) . 2_655 ? O411 Li1 Li1 127.64(17) 3_665 2_655 ? O412 Li1 Li1 95.23(15) 17 2_655 ? O412 Li1 Li1 88.87(14) 3_665 2_655 ? C41 Li1 Li1 111.86(17) 3_665 2_655 ? Li1 Li1 Li1 89.998(1) 17 2_655 ? Li1 Li1 Li1 50.63(13) 18_545 2_655 ? O412 Li1 Li1 95.42(16) . 3_665 ? O411 Li1 Li1 85.4(2) 3_665 3_665 ? O412 Li1 Li1 88.69(16) 17 3_665 ? O412 Li1 Li1 28.90(14) 3_665 3_665 ? C41 Li1 Li1 56.94(18) 3_665 3_665 ? Li1 Li1 Li1 50.63(13) 17 3_665 ? Li1 Li1 Li1 89.999(1) 18_545 3_665 ? Li1 Li1 Li1 60.0 2_655 3_665 ? C11 N1 C17 113.0(2) . . ? C11 N1 Ti1 120.15(18) . . ? C17 N1 Ti1 126.62(18) . . ? C21 N2 C27 114.5(2) . . ? C21 N2 Ti1 119.39(18) . . ? C27 N2 Ti1 126.06(18) . . ? C31 N3 C37 113.8(2) . . ? C31 N3 Ti1 119.36(17) . . ? C37 N3 Ti1 126.57(18) . . ? C41 O4 Ti1 174.84(19) . . ? C41 O411 Li1 95.5(2) . 2_655 ? C41 O412 Li1 138.9(2) . . ? C41 O412 Li1 128.5(2) . 18_545 ? Li1 O412 Li1 92.5(2) . 18_545 ? C41 O412 Li1 78.82(19) . 2_655 ? Li1 O412 Li1 115.6(3) . 2_655 ? Li1 O412 Li1 81.9(2) 18_545 2_655 ? C16 C11 C12 119.0(3) . . ? C16 C11 N1 121.3(3) . . ? C12 C11 N1 119.6(3) . . ? C13 C12 C11 120.8(3) . . ? C14 C13 C12 118.6(3) . . ? C14 C13 C131 121.4(3) . . ? C12 C13 C131 120.0(3) . . ? C15 C14 C13 121.5(3) . . ? C14 C15 C16 118.9(3) . . ? C14 C15 C151 121.6(3) . . ? C16 C15 C151 119.6(3) . . ? C11 C16 C15 121.1(3) . . ? N1 C17 C173 109.9(3) . . ? N1 C17 C172 110.7(3) . . ? C173 C17 C172 109.9(3) . . ? N1 C17 C171 109.0(2) . . ? C173 C17 C171 108.9(3) . . ? C172 C17 C171 108.4(3) . . ? C26 C21 C22 118.7(3) . . ? C26 C21 N2 119.8(3) . . ? C22 C21 N2 121.5(3) . . ? C23 C22 C21 121.4(3) . . ? C22 C23 C24 118.6(3) . . ? C22 C23 C231 120.3(3) . . ? C24 C23 C231 121.0(3) . . ? C25 C24 C23 121.3(3) . . ? C24 C25 C26 119.1(3) . . ? C24 C25 C251 121.1(3) . . ? C26 C25 C251 119.8(3) . . ? C21 C26 C25 120.8(3) . . ? N2 C27 C271 109.8(3) . . ? N2 C27 C273 109.5(3) . . ? C271 C27 C273 109.2(3) . . ? N2 C27 C272 111.4(3) . . ? C271 C27 C272 109.2(3) . . ? C273 C27 C272 107.7(3) . . ? C32 C31 C36 119.2(3) . . ? C32 C31 N3 121.1(3) . . ? C36 C31 N3 119.7(3) . . ? C31 C32 C33 121.2(3) . . ? C34 C33 C32 118.8(3) . . ? C34 C33 C331 121.8(3) . . ? C32 C33 C331 119.5(3) . . ? C33 C34 C35 121.5(3) . . ? C34 C35 C36 118.7(3) . . ? C34 C35 C351 121.2(3) . . ? C36 C35 C351 120.2(3) . . ? C31 C36 C35 120.7(3) . . ? N3 C37 C371 109.8(2) . . ? N3 C37 C372 109.3(2) . . ? C371 C37 C372 108.7(3) . . ? N3 C37 C373 110.6(2) . . ? C371 C37 C373 107.8(3) . . ? C372 C37 C373 110.5(3) . . ? O411 C41 O412 122.0(2) . . ? O411 C41 O4 121.0(2) . . ? O412 C41 O4 117.0(2) . . ? O411 C41 Li1 53.26(18) . 2_655 ? O412 C41 Li1 68.95(18) . 2_655 ? O4 C41 Li1 171.9(2) . 2_655 ? C6T C1T C2T 115.2(11) . . ? C3T C2T C1T 120.6(11) . . ? C4T C3T C2T 119.8(12) . . ? C5T C4T C3T 119.1(12) . . ? C6T C5T C4T 120.7(12) . . ? C1T C6T C5T 124.6(14) . . ? C2U C1U C6U 120.1(12) . . ? C1U C2U C3U 119.0(12) . . ? C4U C3U C2U 120.6(11) . . ? C3U C4U C5U 120.2(10) . . ? C6U C5U C4U 120.2(10) . . ? C5U C6U C1U 119.7(10) . . ? C6S C1S C2S 118.4(12) . . ? C3S C2S C1S 119.2(12) . . ? C4S C3S C2S 118.0(12) . . ? C5S C4S C3S 126.1(13) . . ? C4S C5S C6S 116.0(12) . . ? C5S C6S C1S 121.7(13) . . ? C2V C1V C6V 117.5(15) . . ? C3V C2V C1V 120.6(17) . . ? C4V C3V C2V 120.8(17) . . ? C3V C4V C5V 119.4(16) . . ? C6V C5V C4V 119.7(16) . . ? C5V C6V C1V 121.0(15) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 68.22 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.400 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.052 # Attachment '4909_web_deposit_cif_file_1_JaredS.Silvia_1301691803.cif' data_Me3SiOC(O)OTi(N[tBu]Ar]3 _database_code_depnum_ccdc_archive 'CCDC 819847' _publ_section_abstract ; ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C40 H63 N3 O3 Si Ti' _chemical_formula_sum 'C40 H63 N3 O3 Si Ti' _chemical_properties_physical 'air-sensitive, moisture-sensitive' _exptl_crystal_recrystallization_method 'cooling of saturated diethyl ether solution' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour orange _diffrn_ambient_temperature 100(2) _chemical_formula_weight 709.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_int_tables_number 61 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 19.9166(18) _cell_length_b 19.1716(18) _cell_length_c 21.779(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8316.1(13) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9894 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.26 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 0.272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8761 _exptl_absorpt_correction_T_max 0.9352 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 105056 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7611 _reflns_number_gt 5842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+7.7551P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7611 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Ti1 Ti 0.105410(19) 0.848511(18) 0.102452(16) 0.02026(11) Uani 1 1 d . . . Si1 Si 0.30418(3) 0.93851(4) -0.04564(3) 0.03202(16) Uani 1 1 d . . . O1 O 0.13935(8) 0.89059(8) 0.03221(7) 0.0311(4) Uani 1 1 d . . . N2 N 0.16243(9) 0.77538(9) 0.13451(8) 0.0231(4) Uani 1 1 d . . . N3 N 0.09315(9) 0.91589(9) 0.16653(8) 0.0219(4) Uani 1 1 d . . . N4 N 0.01911(9) 0.81160(9) 0.08086(8) 0.0229(4) Uani 1 1 d . . . C11 C 0.17657(12) 0.91913(12) -0.01101(10) 0.0295(5) Uani 1 1 d . . . C21 C 0.16452(10) 0.76295(11) 0.20009(10) 0.0233(5) Uani 1 1 d . . . C22 C 0.11724(11) 0.71840(11) 0.22685(10) 0.0242(5) Uani 1 1 d . . . H22 H 0.0843 0.6969 0.2016 0.029 Uiso 1 1 calc R . . C23 C 0.11742(11) 0.70489(11) 0.28992(10) 0.0264(5) Uani 1 1 d . . . C24 C 0.16559(11) 0.73707(12) 0.32631(10) 0.0297(5) Uani 1 1 d . . . H24 H 0.1658 0.7286 0.3693 0.036 Uiso 1 1 calc R . . C25 C 0.21362(11) 0.78160(12) 0.30101(10) 0.0289(5) Uani 1 1 d . . . C26 C 0.21268(11) 0.79394(11) 0.23775(10) 0.0265(5) Uani 1 1 d . . . H26 H 0.2454 0.8239 0.2201 0.032 Uiso 1 1 calc R . . C27 C 0.20926(12) 0.72965(12) 0.09783(10) 0.0288(5) Uani 1 1 d . . . C31 C 0.03412(11) 0.91598(11) 0.20495(9) 0.0229(5) Uani 1 1 d . . . C32 C 0.03555(11) 0.87884(11) 0.26035(10) 0.0267(5) Uani 1 1 d . . . H32 H 0.0750 0.8541 0.2717 0.032 Uiso 1 1 calc R . . C33 C -0.02031(12) 0.87781(11) 0.29905(10) 0.0298(5) Uani 1 1 d . . . C34 C -0.07819(12) 0.91325(11) 0.28120(10) 0.0299(5) Uani 1 1 d . . . H34 H -0.1166 0.9120 0.3071 0.036 Uiso 1 1 calc R . . C35 C -0.08113(11) 0.95052(11) 0.22619(10) 0.0269(5) Uani 1 1 d . . . C36 C -0.02440(11) 0.95166(11) 0.18862(10) 0.0242(5) Uani 1 1 d . . . H36 H -0.0256 0.9772 0.1512 0.029 Uiso 1 1 calc R . . C37 C 0.14146(11) 0.97508(11) 0.17928(10) 0.0266(5) Uani 1 1 d . . . C41 C -0.00272(11) 0.74972(11) 0.11304(10) 0.0248(5) Uani 1 1 d . . . C42 C -0.04249(11) 0.75715(11) 0.16572(10) 0.0265(5) Uani 1 1 d . . . H42 H -0.0557 0.8024 0.1787 0.032 Uiso 1 1 calc R . . C43 C -0.06301(11) 0.69914(12) 0.19935(11) 0.0318(5) Uani 1 1 d . . . C44 C -0.04125(12) 0.63359(12) 0.18092(12) 0.0357(6) Uani 1 1 d . . . H44 H -0.0535 0.5940 0.2046 0.043 Uiso 1 1 calc R . . C45 C -0.00186(12) 0.62432(12) 0.12851(12) 0.0347(6) Uani 1 1 d . . . C46 C 0.01582(11) 0.68302(11) 0.09441(11) 0.0294(5) Uani 1 1 d . . . H46 H 0.0410 0.6774 0.0577 0.035 Uiso 1 1 calc R . . C47 C -0.02783(11) 0.83665(11) 0.03088(9) 0.0256(5) Uani 1 1 d . . . O111 O 0.24190(8) 0.91261(9) 0.00166(7) 0.0345(4) Uani 1 1 d . . . O112 O 0.15474(9) 0.94641(11) -0.05626(8) 0.0499(5) Uani 1 1 d . . . C111 C 0.30029(18) 1.03387(16) -0.05516(19) 0.0727(10) Uani 1 1 d . . . H11A H 0.2569 1.0468 -0.0731 0.109 Uiso 1 1 calc R . . H11B H 0.3366 1.0491 -0.0824 0.109 Uiso 1 1 calc R . . H11C H 0.3053 1.0564 -0.0150 0.109 Uiso 1 1 calc R . . C112 C 0.37883(13) 0.91191(17) -0.00090(13) 0.0509(7) Uani 1 1 d . . . H11D H 0.3766 0.9325 0.0402 0.076 Uiso 1 1 calc R . . H11E H 0.4195 0.9282 -0.0218 0.076 Uiso 1 1 calc R . . H11F H 0.3799 0.8610 0.0025 0.076 Uiso 1 1 calc R . . C113 C 0.29545(14) 0.89172(18) -0.11909(12) 0.0527(8) Uani 1 1 d . . . H11G H 0.2981 0.8414 -0.1118 0.079 Uiso 1 1 calc R . . H11H H 0.3317 0.9058 -0.1469 0.079 Uiso 1 1 calc R . . H11I H 0.2520 0.9031 -0.1377 0.079 Uiso 1 1 calc R . . C231 C 0.06562(12) 0.65703(12) 0.31808(11) 0.0327(5) Uani 1 1 d . . . H23A H 0.0850 0.6335 0.3539 0.049 Uiso 1 1 calc R . . H23B H 0.0518 0.6221 0.2878 0.049 Uiso 1 1 calc R . . H23C H 0.0265 0.6844 0.3309 0.049 Uiso 1 1 calc R . . C251 C 0.26674(13) 0.81475(14) 0.34127(11) 0.0399(6) Uani 1 1 d . . . H25A H 0.3101 0.7920 0.3339 0.060 Uiso 1 1 calc R . . H25B H 0.2542 0.8092 0.3845 0.060 Uiso 1 1 calc R . . H25C H 0.2703 0.8645 0.3315 0.060 Uiso 1 1 calc R . . C271 C 0.20416(14) 0.65343(12) 0.11865(11) 0.0392(6) Uani 1 1 d . . . H27A H 0.2174 0.6498 0.1619 0.059 Uiso 1 1 calc R . . H27B H 0.2340 0.6245 0.0935 0.059 Uiso 1 1 calc R . . H27C H 0.1578 0.6372 0.1139 0.059 Uiso 1 1 calc R . . C272 C 0.19045(12) 0.73349(13) 0.02957(10) 0.0343(6) Uani 1 1 d . . . H27D H 0.1425 0.7233 0.0247 0.051 Uiso 1 1 calc R . . H27E H 0.2168 0.6992 0.0065 0.051 Uiso 1 1 calc R . . H27F H 0.2000 0.7804 0.0139 0.051 Uiso 1 1 calc R . . C273 C 0.28202(12) 0.75476(15) 0.10479(12) 0.0406(6) Uani 1 1 d . . . H27G H 0.2850 0.8039 0.0928 0.061 Uiso 1 1 calc R . . H27H H 0.3114 0.7268 0.0784 0.061 Uiso 1 1 calc R . . H27I H 0.2961 0.7496 0.1477 0.061 Uiso 1 1 calc R . . C331 C -0.01719(14) 0.83984(13) 0.35996(11) 0.0398(6) Uani 1 1 d . . . H33A H -0.0149 0.8739 0.3934 0.060 Uiso 1 1 calc R . . H33B H 0.0228 0.8101 0.3610 0.060 Uiso 1 1 calc R . . H33C H -0.0575 0.8110 0.3649 0.060 Uiso 1 1 calc R . . C351 C -0.14407(12) 0.98973(12) 0.20862(11) 0.0340(5) Uani 1 1 d . . . H35A H -0.1453 1.0344 0.2304 0.051 Uiso 1 1 calc R . . H35B H -0.1836 0.9620 0.2198 0.051 Uiso 1 1 calc R . . H35C H -0.1442 0.9981 0.1642 0.051 Uiso 1 1 calc R . . C371 C 0.11156(13) 1.04318(11) 0.15464(12) 0.0367(6) Uani 1 1 d . . . H37A H 0.1026 1.0384 0.1106 0.055 Uiso 1 1 calc R . . H37B H 0.1434 1.0814 0.1613 0.055 Uiso 1 1 calc R . . H37C H 0.0695 1.0533 0.1763 0.055 Uiso 1 1 calc R . . C372 C 0.15557(12) 0.98168(13) 0.24833(11) 0.0345(6) Uani 1 1 d . . . H37D H 0.1134 0.9903 0.2702 0.052 Uiso 1 1 calc R . . H37E H 0.1865 1.0206 0.2555 0.052 Uiso 1 1 calc R . . H37F H 0.1758 0.9384 0.2634 0.052 Uiso 1 1 calc R . . C373 C 0.20853(12) 0.96150(12) 0.14686(12) 0.0344(6) Uani 1 1 d . . . H37G H 0.2238 0.9141 0.1561 0.052 Uiso 1 1 calc R . . H37H H 0.2420 0.9952 0.1613 0.052 Uiso 1 1 calc R . . H37I H 0.2026 0.9666 0.1024 0.052 Uiso 1 1 calc R . . C431 C -0.10834(12) 0.70817(13) 0.25435(12) 0.0393(6) Uani 1 1 d . . . H43A H -0.1137 0.7580 0.2632 0.059 Uiso 1 1 calc R . . H43B H -0.0884 0.6848 0.2900 0.059 Uiso 1 1 calc R . . H43C H -0.1523 0.6876 0.2456 0.059 Uiso 1 1 calc R . . C451 C 0.02274(15) 0.55261(12) 0.11030(13) 0.0463(7) Uani 1 1 d . . . H45A H 0.0615 0.5399 0.1357 0.069 Uiso 1 1 calc R . . H45B H 0.0359 0.5530 0.0669 0.069 Uiso 1 1 calc R . . H45C H -0.0133 0.5185 0.1165 0.069 Uiso 1 1 calc R . . C471 C -0.01167(12) 0.91201(12) 0.01380(11) 0.0320(5) Uani 1 1 d . . . H47A H -0.0469 0.9303 -0.0131 0.048 Uiso 1 1 calc R . . H47B H 0.0316 0.9137 -0.0076 0.048 Uiso 1 1 calc R . . H47C H -0.0093 0.9404 0.0512 0.048 Uiso 1 1 calc R . . C472 C -0.01930(13) 0.79007(13) -0.02577(10) 0.0374(6) Uani 1 1 d . . . H47D H -0.0314 0.7420 -0.0153 0.056 Uiso 1 1 calc R . . H47E H 0.0275 0.7916 -0.0395 0.056 Uiso 1 1 calc R . . H47F H -0.0486 0.8069 -0.0588 0.056 Uiso 1 1 calc R . . C473 C -0.10113(11) 0.83428(14) 0.05232(11) 0.0372(6) Uani 1 1 d . . . H47G H -0.1137 0.7860 0.0615 0.056 Uiso 1 1 calc R . . H47H H -0.1303 0.8525 0.0198 0.056 Uiso 1 1 calc R . . H47I H -0.1063 0.8628 0.0893 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0229(2) 0.01898(19) 0.01893(19) 0.00001(15) 0.00223(15) 0.00044(15) Si1 0.0293(4) 0.0343(4) 0.0324(4) 0.0011(3) 0.0070(3) -0.0024(3) O1 0.0323(9) 0.0350(9) 0.0260(8) 0.0059(7) 0.0068(7) -0.0002(7) N2 0.0232(9) 0.0232(9) 0.0230(9) -0.0003(7) 0.0034(8) 0.0034(7) N3 0.0238(9) 0.0203(9) 0.0216(9) -0.0011(7) 0.0022(7) 0.0000(7) N4 0.0275(10) 0.0202(9) 0.0210(9) 0.0010(7) -0.0003(7) 0.0001(7) C11 0.0307(13) 0.0334(13) 0.0245(12) -0.0006(10) 0.0024(10) 0.0039(10) C21 0.0249(11) 0.0204(11) 0.0246(11) 0.0007(9) 0.0014(9) 0.0067(9) C22 0.0231(11) 0.0222(11) 0.0272(11) -0.0009(9) -0.0008(9) 0.0045(9) C23 0.0262(12) 0.0235(11) 0.0293(12) 0.0028(9) 0.0025(9) 0.0063(9) C24 0.0324(13) 0.0339(13) 0.0228(11) 0.0015(10) 0.0014(10) 0.0084(10) C25 0.0282(12) 0.0295(12) 0.0290(12) -0.0019(10) -0.0023(10) 0.0043(10) C26 0.0237(11) 0.0255(11) 0.0304(12) -0.0015(9) 0.0019(9) 0.0022(9) C27 0.0322(13) 0.0278(12) 0.0263(12) -0.0015(9) 0.0046(10) 0.0065(10) C31 0.0274(12) 0.0187(10) 0.0225(11) -0.0043(8) 0.0031(9) -0.0001(9) C32 0.0316(12) 0.0222(11) 0.0262(12) -0.0014(9) 0.0016(9) 0.0022(9) C33 0.0397(14) 0.0226(11) 0.0271(12) 0.0008(9) 0.0081(10) 0.0013(10) C34 0.0326(13) 0.0268(12) 0.0304(12) -0.0001(10) 0.0106(10) 0.0004(10) C35 0.0276(12) 0.0212(11) 0.0318(12) -0.0030(9) 0.0040(10) -0.0001(9) C36 0.0289(12) 0.0203(11) 0.0234(11) 0.0010(9) -0.0006(9) -0.0018(9) C37 0.0270(12) 0.0214(11) 0.0316(12) -0.0038(9) 0.0003(10) -0.0026(9) C41 0.0249(11) 0.0225(11) 0.0269(11) 0.0025(9) -0.0046(9) -0.0034(9) C42 0.0245(11) 0.0231(11) 0.0320(12) 0.0026(9) -0.0023(9) -0.0018(9) C43 0.0268(12) 0.0330(13) 0.0355(13) 0.0096(10) -0.0047(10) -0.0072(10) C44 0.0337(13) 0.0284(13) 0.0449(15) 0.0141(11) -0.0101(11) -0.0101(10) C45 0.0349(14) 0.0239(12) 0.0452(14) 0.0026(11) -0.0140(12) -0.0039(10) C46 0.0290(12) 0.0259(12) 0.0333(13) -0.0006(10) -0.0061(10) -0.0012(9) C47 0.0281(12) 0.0276(12) 0.0211(11) 0.0005(9) -0.0028(9) -0.0012(9) O111 0.0274(9) 0.0464(10) 0.0296(9) 0.0077(7) 0.0056(7) 0.0019(7) O112 0.0351(10) 0.0769(14) 0.0377(10) 0.0255(10) 0.0049(8) 0.0040(9) C111 0.069(2) 0.0439(18) 0.106(3) 0.0130(18) 0.011(2) -0.0080(16) C112 0.0325(15) 0.076(2) 0.0446(16) 0.0012(14) 0.0039(12) -0.0016(14) C113 0.0378(16) 0.080(2) 0.0401(16) -0.0109(15) 0.0103(12) 0.0008(15) C231 0.0334(13) 0.0357(13) 0.0290(12) 0.0072(10) 0.0038(10) 0.0020(10) C251 0.0390(15) 0.0477(16) 0.0331(13) -0.0046(12) -0.0075(11) -0.0044(12) C271 0.0514(16) 0.0299(13) 0.0363(14) -0.0012(11) 0.0091(12) 0.0157(12) C272 0.0389(14) 0.0340(13) 0.0300(13) -0.0045(10) 0.0048(11) 0.0060(11) C273 0.0280(13) 0.0563(16) 0.0376(14) -0.0078(12) 0.0063(11) 0.0093(12) C331 0.0513(16) 0.0385(14) 0.0296(13) 0.0052(11) 0.0120(12) 0.0075(12) C351 0.0282(13) 0.0324(13) 0.0413(14) 0.0026(11) 0.0066(11) 0.0021(10) C371 0.0378(14) 0.0217(12) 0.0508(16) -0.0004(11) -0.0047(12) -0.0046(10) C372 0.0290(13) 0.0380(14) 0.0364(13) -0.0112(11) -0.0015(11) -0.0018(10) C373 0.0324(13) 0.0302(13) 0.0408(14) -0.0055(10) 0.0075(11) -0.0057(10) C431 0.0341(14) 0.0422(14) 0.0416(15) 0.0162(12) 0.0035(11) -0.0050(12) C451 0.0539(17) 0.0227(12) 0.0622(18) -0.0001(12) -0.0140(14) -0.0004(12) C471 0.0366(14) 0.0309(13) 0.0285(12) 0.0064(10) -0.0049(10) 0.0020(10) C472 0.0498(16) 0.0389(14) 0.0234(12) -0.0007(10) -0.0059(11) -0.0002(12) C473 0.0280(13) 0.0523(16) 0.0314(13) 0.0117(11) -0.0028(10) 0.0020(11) _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 Ti1 O1 1.8569(15) . ? Ti1 N3 1.9173(17) . ? Ti1 N4 1.9174(18) . ? Ti1 N2 1.9347(18) . ? Si1 O111 1.6871(16) . ? Si1 C111 1.841(3) . ? Si1 C113 1.842(3) . ? Si1 C112 1.849(3) . ? O1 C11 1.317(3) . ? N2 C21 1.449(3) . ? N2 C27 1.509(3) . ? N3 C31 1.443(3) . ? N3 C37 1.513(3) . ? N4 C41 1.445(3) . ? N4 C47 1.513(3) . ? C11 O112 1.197(3) . ? C11 O111 1.336(3) . ? C21 C26 1.395(3) . ? C21 C22 1.399(3) . ? C22 C23 1.398(3) . ? C23 C24 1.389(3) . ? C23 C231 1.511(3) . ? C24 C25 1.396(3) . ? C25 C26 1.398(3) . ? C25 C251 1.514(3) . ? C27 C271 1.533(3) . ? C27 C273 1.535(3) . ? C27 C272 1.535(3) . ? C31 C36 1.398(3) . ? C31 C32 1.401(3) . ? C32 C33 1.396(3) . ? C33 C34 1.393(3) . ? C33 C331 1.514(3) . ? C34 C35 1.396(3) . ? C35 C36 1.395(3) . ? C35 C351 1.511(3) . ? C37 C371 1.532(3) . ? C37 C373 1.533(3) . ? C37 C372 1.535(3) . ? C41 C46 1.391(3) . ? C41 C42 1.401(3) . ? C42 C43 1.393(3) . ? C43 C44 1.389(3) . ? C43 C431 1.510(3) . ? C44 C45 1.397(4) . ? C45 C46 1.393(3) . ? C45 C451 1.512(3) . ? C47 C471 1.526(3) . ? C47 C472 1.532(3) . ? C47 C473 1.534(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 O1 Ti1 N3 110.69(7) . . ? O1 Ti1 N4 106.54(7) . . ? N3 Ti1 N4 108.24(7) . . ? O1 Ti1 N2 113.48(7) . . ? N3 Ti1 N2 107.47(7) . . ? N4 Ti1 N2 110.32(7) . . ? O111 Si1 C111 109.27(13) . . ? O111 Si1 C113 108.51(11) . . ? C111 Si1 C113 112.44(17) . . ? O111 Si1 C112 100.85(11) . . ? C111 Si1 C112 111.53(16) . . ? C113 Si1 C112 113.52(14) . . ? C11 O1 Ti1 166.93(16) . . ? C21 N2 C27 114.12(16) . . ? C21 N2 Ti1 119.47(13) . . ? C27 N2 Ti1 126.36(14) . . ? C31 N3 C37 114.25(16) . . ? C31 N3 Ti1 121.78(13) . . ? C37 N3 Ti1 123.89(13) . . ? C41 N4 C47 115.07(16) . . ? C41 N4 Ti1 116.99(13) . . ? C47 N4 Ti1 127.81(13) . . ? O112 C11 O1 124.4(2) . . ? O112 C11 O111 124.4(2) . . ? O1 C11 O111 111.20(19) . . ? C26 C21 C22 118.6(2) . . ? C26 C21 N2 121.97(19) . . ? C22 C21 N2 119.47(19) . . ? C23 C22 C21 121.4(2) . . ? C24 C23 C22 118.7(2) . . ? C24 C23 C231 120.7(2) . . ? C22 C23 C231 120.6(2) . . ? C23 C24 C25 121.3(2) . . ? C24 C25 C26 118.9(2) . . ? C24 C25 C251 120.5(2) . . ? C26 C25 C251 120.6(2) . . ? C21 C26 C25 121.1(2) . . ? N2 C27 C271 110.87(18) . . ? N2 C27 C273 110.43(18) . . ? C271 C27 C273 109.4(2) . . ? N2 C27 C272 109.52(18) . . ? C271 C27 C272 108.42(19) . . ? C273 C27 C272 108.13(19) . . ? C36 C31 C32 119.00(19) . . ? C36 C31 N3 122.18(19) . . ? C32 C31 N3 118.82(19) . . ? C33 C32 C31 120.7(2) . . ? C34 C33 C32 118.9(2) . . ? C34 C33 C331 120.8(2) . . ? C32 C33 C331 120.2(2) . . ? C33 C34 C35 121.6(2) . . ? C36 C35 C34 118.5(2) . . ? C36 C35 C351 121.0(2) . . ? C34 C35 C351 120.4(2) . . ? C35 C36 C31 121.2(2) . . ? N3 C37 C371 109.12(17) . . ? N3 C37 C373 110.01(17) . . ? C371 C37 C373 108.79(19) . . ? N3 C37 C372 110.97(18) . . ? C371 C37 C372 110.12(19) . . ? C373 C37 C372 107.80(19) . . ? C46 C41 C42 118.8(2) . . ? C46 C41 N4 122.22(19) . . ? C42 C41 N4 118.92(19) . . ? C43 C42 C41 121.0(2) . . ? C44 C43 C42 118.6(2) . . ? C44 C43 C431 121.3(2) . . ? C42 C43 C431 120.1(2) . . ? C43 C44 C45 121.8(2) . . ? C46 C45 C44 118.3(2) . . ? C46 C45 C451 120.8(2) . . ? C44 C45 C451 120.8(2) . . ? C41 C46 C45 121.3(2) . . ? N4 C47 C471 110.21(17) . . ? N4 C47 C472 109.01(18) . . ? C471 C47 C472 109.39(18) . . ? N4 C47 C473 111.08(17) . . ? C471 C47 C473 107.64(19) . . ? C472 C47 C473 109.5(2) . . ? C11 O111 Si1 124.22(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.328 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.052