#------------------------------------------------------------------------------ #$Date: 2019-06-05 03:42:48 +0300 (Wed, 05 Jun 2019) $ #$Revision: 215693 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551207.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1551207 _journal_paper_doi 10.1039/C9CE00706G _chemical_compound_source no _chemical_formula_moiety 'C67 H117 N Si2' _chemical_formula_sum 'C67 H117 N Si2' _chemical_formula_weight 992.79 _chemical_melting_point 493 _chemical_name_common C18NMeCarbacage _chemical_name_systematic C18NMeCarbaCage _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc1z8myt _audit_creation_method SHELXL-2013 _audit_update_record ; 2018-02-24 deposited with the CCDC. 2019-06-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 119.214(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 34.673(6) _cell_length_b 12.090(2) _cell_length_c 17.728(3) _cell_measurement_reflns_used 2359 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 20.17 _cell_measurement_theta_min 2.30 _cell_volume 6486.2(19) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution Sir-2011 _diffrn_ambient_temperature 200(2) _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.904 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_unetI/netI 0.0459 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.904 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 16192 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.904 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.369 _diffrn_reflns_theta_min 1.346 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.7035 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS Bruker' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.017 _exptl_crystal_description prism _exptl_crystal_F_000 2216 _exptl_crystal_preparation Luminescent _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF/MeOH' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _refine_diff_density_max 1.050 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.291 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 462 _refine_ls_number_reflns 6658 _refine_ls_number_restraints 123 _refine_ls_restrained_S_all 1.329 _refine_ls_R_factor_all 0.1726 _refine_ls_R_factor_gt 0.1083 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3444 _refine_ls_wR_factor_ref 0.3993 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3377 _reflns_number_total 6658 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce00706g2.cif _cod_data_source_block shelx _cod_original_cell_volume 6486.4(19) _cod_database_code 1551207 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.964 _shelx_estimated_absorpt_t_max 0.982 _shelxl_version_number 2013-4 _shelx_res_file ; TITL C18meCarba hemi 5sec 200K in C2/c a1707261stk CELL 0.71073 34.6733 12.0903 17.7278 90.000 119.214 90.000 ZERR 4.00 0.0058 0.0020 0.0030 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N SI UNIT 268 468 4 8 MERG 2 eqiv $1 -x, y, -z+1/2 RIGU 0.02 C30 > C135 SIMU C22 C23 free C01 C07 free C02 C12 free C02 C07 free C02 C08 free C03 C09 free C03 C10 free C04 C08 free C04 C09 free C05 C08 free C06 C08 free C10 N10 free C11 N10 free C11 C40_$1 free C04 C40 free C40 C10_$1 free C40 C11_$1 FLAT 0.100 C01 C02 C03 C04 C05 C06 FLAT 0.100 C07 C08 C09 C10 C11 C12 dfix 1.38 C01 C02 dfix 1.38 C02 C03 dfix 1.38 C03 C04 dfix 1.38 C04 C05 dfix 1.38 C05 C06 dfix 1.38 C06 C01 dfix 1.38 C07 C08 dfix 1.38 C08 C09 dfix 1.38 C09 C10 dfix 1.38 C10 C11 dfix 1.38 C11 C12 dfix 1.38 C12 C07 dfix 1.55 C30 C31 dfix 1.55 C31 C32 dfix 1.55 C32 C33 dfix 1.55 C33 C34 dfix 1.55 C35 C36 dfix 1.55 C36 C37 dfix 1.55 C37 C38 dfix 1.55 C38 C39_$1 dfix 1.55 C30 C131 dfix 1.55 C131 C132 dfix 1.55 C132 C133 dfix 1.55 C133 C134 dfix 1.55 C134 C135 dfix 1.55 C135 C136 dfix 1.55 C136 C137 dfix 1.55 C137 C138 dfix 1.55 C138 C139_$1 dfix 1.90 Si01 C39 dfix 1.90 Si01 C139 DANG 2.300 0.040 C31 C33 DANG 2.300 0.040 C36 C38 DANG 2.300 0.040 C131 C133 DANG 2.300 0.040 C132 C134 DANG 2.300 0.040 C133 C135 DANG 2.300 0.040 C134 C136 DANG 2.300 0.040 C135 C137 DANG 2.300 0.040 C137 C139_$1 FMAP 2 PLAN 25 SIZE 0.200 0.400 0.400 ACTA BOND $H L.S. 20 TEMP -73.00 WGHT 0.200000 FVAR 0.06465 0.49603 SI01 4 0.172544 0.031453 0.374947 11.00000 0.06296 0.07475 = 0.07597 -0.00693 0.00215 -0.00447 N10 3 0.010677 0.040564 0.307643 10.50000 0.04693 0.08094 = 0.04693 -0.02083 0.01755 -0.00057 C40 1 -0.016848 0.027652 0.105316 10.50000 0.04548 0.13678 = 0.05665 0.01402 0.02274 -0.00407 AFIX 137 H40A 2 -0.021977 -0.050499 0.088653 10.50000 -1.50000 H40B 2 0.009665 0.053342 0.104159 10.50000 -1.50000 H40C 2 -0.042378 0.071440 0.064674 10.50000 -1.50000 AFIX 0 C01 1 0.115612 0.032370 0.298239 10.50000 0.03370 0.06241 = 0.08295 -0.01507 0.02539 -0.00459 C02 1 0.089747 0.035666 0.335814 10.50000 0.03826 0.06910 = 0.04809 -0.01739 0.00558 0.00400 AFIX 43 H02 2 0.102490 0.035209 0.396952 10.50000 -1.20000 AFIX 0 C03 1 0.043594 0.039782 0.282450 10.50000 0.01503 0.05917 = 0.06659 -0.01829 0.01874 -0.00669 C04 1 0.023715 0.041480 0.193685 10.50000 0.03737 0.04517 = 0.07277 0.00657 0.02933 0.00074 C05 1 0.050417 0.038666 0.156265 10.50000 0.04299 0.08059 = 0.06672 0.00998 0.02826 0.00533 AFIX 43 H05 2 0.037905 0.040510 0.095189 10.50000 -1.20000 AFIX 0 C06 1 0.095225 0.033175 0.208427 10.50000 0.04812 0.06051 = 0.07205 0.00020 0.02484 -0.00543 AFIX 43 H06 2 0.113337 0.029739 0.182011 10.50000 -1.20000 AFIX 0 C07 1 0.109592 0.038278 0.361305 10.50000 0.03602 0.06079 = 0.04572 -0.00624 0.00943 -0.00027 C08 1 0.072628 0.040017 0.278361 10.50000 0.04291 0.05182 = 0.05596 0.00765 0.01760 0.00518 AFIX 43 H08 2 0.060263 0.058757 0.218989 10.50000 -1.20000 AFIX 0 C09 1 0.029457 0.041717 0.269260 10.50000 0.01838 0.04893 = 0.06291 0.00137 0.01513 -0.00531 C10 1 0.022474 0.043803 0.339671 10.50000 0.04080 0.04707 = 0.05273 -0.00504 0.02253 -0.00494 C11 1 0.059924 0.040630 0.422051 10.50000 0.04590 0.08451 = 0.05043 -0.02366 0.01633 -0.00758 AFIX 43 H11 2 0.056249 0.039293 0.471754 10.50000 -1.20000 AFIX 0 C12 1 0.102223 0.039411 0.432242 10.50000 0.04002 0.08468 = 0.05232 -0.01749 0.01796 -0.00617 AFIX 43 H12 2 0.126880 0.039343 0.488947 10.50000 -1.20000 AFIX 0 C13 1 0.195181 0.173194 0.409643 11.00000 0.04739 0.08206 = 0.05605 -0.00622 0.02054 -0.01419 AFIX 23 H13A 2 0.192413 0.192644 0.461041 11.00000 -1.20000 H13B 2 0.227123 0.171014 0.428177 11.00000 -1.20000 AFIX 0 C14 1 0.174298 0.266360 0.343501 11.00000 0.06815 0.08643 = 0.05878 -0.00864 0.01879 -0.00284 AFIX 23 H14A 2 0.176266 0.246902 0.291239 11.00000 -1.20000 H14B 2 0.142574 0.271387 0.326412 11.00000 -1.20000 AFIX 0 C15 1 0.195345 0.379203 0.375197 11.00000 0.10943 0.07656 = 0.06446 -0.00371 0.03899 -0.00830 AFIX 23 H15A 2 0.194860 0.395597 0.429443 11.00000 -1.20000 H15B 2 0.226740 0.373811 0.389914 11.00000 -1.20000 AFIX 0 C16 1 0.175830 0.474232 0.316890 11.00000 0.12016 0.11336 = 0.08712 0.00380 0.05848 0.00883 AFIX 23 H16A 2 0.195986 0.538532 0.339555 11.00000 -1.20000 H16B 2 0.171776 0.455853 0.259042 11.00000 -1.20000 AFIX 0 C17 1 0.135235 0.500970 0.310120 11.00000 0.11332 0.14693 = 0.08396 0.00258 0.03858 -0.03307 AFIX 23 H17A 2 0.139011 0.507353 0.369025 11.00000 -1.20000 H17B 2 0.114341 0.439551 0.280587 11.00000 -1.20000 AFIX 0 C18 1 0.113731 0.614117 0.258426 11.00000 0.13182 0.16203 = 0.08935 0.02537 0.05017 0.06380 AFIX 23 H18A 2 0.134369 0.676627 0.285867 11.00000 -1.20000 H18B 2 0.107442 0.607632 0.197799 11.00000 -1.20000 AFIX 0 C19 1 0.072790 0.632947 0.261169 11.00000 0.14164 0.08334 = 0.09986 0.00999 0.06485 0.01862 AFIX 23 H19A 2 0.079992 0.635743 0.322485 11.00000 -1.20000 H19B 2 0.053164 0.568495 0.234430 11.00000 -1.20000 AFIX 0 C20 1 0.047491 0.736114 0.217017 11.00000 0.12238 0.07172 = 0.09833 0.01493 0.05232 0.00187 AFIX 23 H20A 2 0.044639 0.741258 0.158773 11.00000 -1.20000 H20B 2 0.064126 0.801699 0.250547 11.00000 -1.20000 AFIX 0 C21 1 0.001125 0.736494 0.208595 11.00000 0.10063 0.06353 = 0.10335 0.00247 0.04013 0.00046 AFIX 23 H21A 2 -0.014844 0.802572 0.174788 11.00000 -1.20000 H21B 2 -0.015020 0.670693 0.174606 11.00000 -1.20000 AFIX 0 C22 1 0.196802 -0.066165 0.467314 11.00000 0.05333 0.08504 = 0.08734 -0.00020 0.01618 -0.00053 AFIX 23 H22A 2 0.229277 -0.064877 0.491649 11.00000 -1.20000 H22B 2 0.190532 -0.037133 0.512438 11.00000 -1.20000 AFIX 0 C23 1 0.182074 -0.185970 0.451233 11.00000 0.07333 0.11764 = 0.09475 0.01506 0.03084 0.00739 AFIX 23 H23A 2 0.194025 -0.220678 0.416358 11.00000 -1.20000 H23B 2 0.149439 -0.187887 0.416460 11.00000 -1.20000 AFIX 0 C24 1 0.196143 -0.255166 0.532244 11.00000 0.08038 0.19011 = 0.13599 0.09283 0.01641 -0.00804 AFIX 23 H24A 2 0.193107 -0.333952 0.515039 11.00000 -1.20000 H24B 2 0.227986 -0.241336 0.571282 11.00000 -1.20000 AFIX 0 C25 1 0.172594 -0.239391 0.584455 11.00000 0.10534 0.14770 = 0.08751 0.04577 0.01164 -0.02096 AFIX 23 H25A 2 0.186013 -0.289281 0.635162 11.00000 -1.20000 H25B 2 0.177205 -0.162416 0.606199 11.00000 -1.20000 AFIX 0 C26 1 0.123601 -0.262057 0.533798 11.00000 0.09608 0.10392 = 0.07603 0.01881 0.02693 -0.00747 AFIX 23 H26A 2 0.118733 -0.326883 0.496062 11.00000 -1.20000 H26B 2 0.108952 -0.197799 0.495882 11.00000 -1.20000 AFIX 0 C27 1 0.101499 -0.284020 0.587906 11.00000 0.14228 0.11193 = 0.06774 0.00688 0.03499 -0.00159 AFIX 23 H27A 2 0.115105 -0.350896 0.623231 11.00000 -1.20000 H27B 2 0.108166 -0.221247 0.628275 11.00000 -1.20000 AFIX 0 C28 1 0.053686 -0.299810 0.541015 11.00000 0.12396 0.09494 = 0.09859 0.00726 0.06391 0.01183 AFIX 23 H28A 2 0.046874 -0.357387 0.496546 11.00000 -1.20000 H28B 2 0.039983 -0.230111 0.510274 11.00000 -1.20000 AFIX 0 C29 1 0.031718 -0.332306 0.593054 11.00000 0.18582 0.11376 = 0.11105 0.03097 0.10214 0.02634 AFIX 23 H29A 2 0.043946 -0.404269 0.621285 11.00000 -1.20000 H29B 2 0.039360 -0.276799 0.639277 11.00000 -1.20000 AFIX 0 C30 1 -0.017436 -0.341837 0.542030 11.00000 0.19100 0.12869 = 0.17568 0.06370 0.14648 0.05501 AFIX 23 H30A 2 -0.023334 -0.388245 0.491505 11.00000 -1.20000 H30B 2 -0.028009 -0.266725 0.518948 11.00000 -1.20000 AFIX 0 PART 1 C31 1 -0.050418 -0.385073 0.573058 21.00000 0.09151 0.21567 = 0.10593 0.03346 0.05434 -0.01524 AFIX 23 H31A 2 -0.035088 -0.447349 0.612789 21.00000 -1.20000 H31B 2 -0.052304 -0.325164 0.609190 21.00000 -1.20000 AFIX 0 C32 1 -0.098231 -0.424430 0.514781 21.00000 0.12537 0.07980 = 0.11294 0.01969 0.09132 0.00240 AFIX 23 H32A 2 -0.099184 -0.482354 0.474434 21.00000 -1.20000 H32B 2 -0.110593 -0.455318 0.550199 21.00000 -1.20000 AFIX 0 C33 1 -0.124583 -0.323228 0.464829 21.00000 0.08960 0.11109 = 0.12896 -0.00531 0.06872 -0.00612 AFIX 23 H33A 2 -0.111333 -0.291963 0.431084 21.00000 -1.20000 H33B 2 -0.123279 -0.266003 0.505956 21.00000 -1.20000 AFIX 0 C34 1 -0.174125 -0.354999 0.401992 21.00000 0.09545 0.12656 = 0.12741 -0.00834 0.07417 -0.01510 AFIX 23 H34A 2 -0.175466 -0.402612 0.355337 21.00000 -1.20000 H34B 2 -0.185410 -0.398597 0.434388 21.00000 -1.20000 AFIX 0 C35 1 -0.200691 -0.266447 0.366070 21.00000 0.07526 0.12634 = 0.10809 -0.02415 0.06560 -0.03539 AFIX 23 H35A 2 -0.196798 -0.217663 0.414144 21.00000 -1.20000 H35B 2 -0.231504 -0.293841 0.338339 21.00000 -1.20000 AFIX 0 C36 1 -0.196908 -0.195772 0.302035 21.00000 0.16241 0.14093 = 0.07894 -0.00868 0.06041 -0.07258 AFIX 23 H36A 2 -0.208166 -0.238397 0.247651 21.00000 -1.20000 H36B 2 -0.165120 -0.181828 0.323247 21.00000 -1.20000 AFIX 0 C37 1 -0.220701 -0.083512 0.280219 21.00000 0.10273 0.13126 = 0.08553 -0.03434 0.04656 -0.02801 AFIX 23 H37A 2 -0.252435 -0.092771 0.261930 21.00000 -1.20000 H37B 2 -0.207225 -0.033175 0.330645 21.00000 -1.20000 AFIX 0 C38 1 -0.214597 -0.038998 0.206304 21.00000 0.05507 0.10580 = 0.07421 0.01223 0.04610 0.00639 AFIX 23 H38A 2 -0.230768 0.032034 0.187747 21.00000 -1.20000 H38B 2 -0.229517 -0.091033 0.157268 21.00000 -1.20000 AFIX 0 C39 1 0.167508 -0.018781 0.279861 21.00000 0.05714 0.07328 = 0.06708 -0.00294 0.03250 0.00371 AFIX 23 H39A 2 0.150530 -0.088772 0.263879 21.00000 -1.20000 H39B 2 0.151710 0.035330 0.232695 21.00000 -1.20000 AFIX 0 PART 2 C131 1 -0.028747 -0.357310 0.616913 -21.00000 0.15704 0.11283 = 0.14269 0.05169 0.11045 0.03521 AFIX 23 H13C 2 -0.022994 -0.434102 0.639118 -21.00000 -1.20000 H13D 2 -0.011582 -0.305619 0.665194 -21.00000 -1.20000 AFIX 0 C132 1 -0.077354 -0.330826 0.572735 -21.00000 0.16358 0.11679 = 0.15598 0.03623 0.13446 0.04382 AFIX 23 H13E 2 -0.082158 -0.252438 0.554246 -21.00000 -1.20000 H13F 2 -0.088961 -0.342480 0.613257 -21.00000 -1.20000 AFIX 0 C133 1 -0.101547 -0.406305 0.494061 -21.00000 0.15626 0.10046 = 0.18021 0.04878 0.12556 0.01046 AFIX 23 H13G 2 -0.095794 -0.484209 0.513671 -21.00000 -1.20000 H13H 2 -0.089149 -0.394404 0.454859 -21.00000 -1.20000 AFIX 0 C134 1 -0.151545 -0.388012 0.443200 -21.00000 0.17982 0.10405 = 0.14443 0.03494 0.13012 0.02487 AFIX 23 H13I 2 -0.165601 -0.444360 0.397132 -21.00000 -1.20000 H13J 2 -0.164448 -0.393750 0.482049 -21.00000 -1.20000 AFIX 0 C135 1 -0.159072 -0.273874 0.404261 -21.00000 0.15741 0.07052 = 0.11133 0.01049 0.10205 0.00061 AFIX 23 H13K 2 -0.154806 -0.219133 0.449220 -21.00000 -1.20000 H13L 2 -0.136387 -0.259297 0.386929 -21.00000 -1.20000 AFIX 0 C136 1 -0.203832 -0.256233 0.327327 -21.00000 0.12048 0.09502 = 0.11765 0.02740 0.04977 0.00716 AFIX 23 H13M 2 -0.226861 -0.285118 0.339768 -21.00000 -1.20000 H13N 2 -0.205928 -0.297072 0.277056 -21.00000 -1.20000 AFIX 0 C137 1 -0.211615 -0.131573 0.305775 -21.00000 0.11562 0.07610 = 0.26102 -0.01274 0.14393 0.02435 AFIX 23 H13O 2 -0.243332 -0.112333 0.279339 -21.00000 -1.20000 H13P 2 -0.194518 -0.085467 0.357846 -21.00000 -1.20000 AFIX 0 C138 1 -0.194697 -0.118529 0.241392 -21.00000 0.06145 0.09903 = 0.09398 0.01795 0.03235 -0.01068 AFIX 23 H13Q 2 -0.162299 -0.129871 0.272471 -21.00000 -1.20000 H13R 2 -0.207864 -0.177738 0.197473 -21.00000 -1.20000 AFIX 0 C139 1 0.204349 -0.009100 0.304477 -21.00000 0.04864 0.13500 = 0.11538 -0.04477 0.04642 -0.00708 AFIX 23 H13S 2 0.197304 0.049517 0.260659 -21.00000 -1.20000 H13T 2 0.236574 -0.005610 0.344556 -21.00000 -1.20000 AFIX 0 HKLF 4 REM C18meCarba hemi 5sec 200K in C2/c a1707261stk REM R1 = 0.1083 for 3377 Fo > 4sig(Fo) and 0.1726 for all 6658 data REM 462 parameters refined using 123 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.050, deepest hole -0.349, 1-sigma level 0.056 Q1 1 0.1648 0.5800 0.3381 11.00000 0.05 1.05 Q2 1 0.1703 -0.0961 0.4902 11.00000 0.05 0.75 Q3 1 0.1740 0.0373 0.3323 11.00000 0.05 0.51 Q4 1 0.1912 -0.1738 0.5538 11.00000 0.05 0.38 Q5 1 0.0514 0.6892 0.2819 11.00000 0.05 0.29 Q6 1 0.0000 0.6703 0.2500 10.50000 0.05 0.25 Q7 1 -0.1838 -0.1608 0.3558 11.00000 0.05 0.25 Q8 1 0.1448 0.4471 0.2840 11.00000 0.05 0.23 Q9 1 -0.0702 -0.3793 0.5685 11.00000 0.05 0.23 Q10 1 0.0656 0.6591 0.1972 11.00000 0.05 0.21 Q11 1 0.0142 -0.3736 0.6309 11.00000 0.05 0.19 Q12 1 0.0744 -0.1983 0.5498 11.00000 0.05 0.19 Q13 1 0.1858 -0.0396 0.4102 11.00000 0.05 0.18 Q14 1 0.1430 0.2550 0.2886 11.00000 0.05 0.17 Q15 1 0.1691 0.3610 0.3515 11.00000 0.05 0.17 Q16 1 -0.2327 -0.0253 0.2764 11.00000 0.05 0.15 Q17 1 0.1815 0.1346 0.3978 11.00000 0.05 0.15 Q18 1 0.0116 -0.2374 0.5622 11.00000 0.05 0.14 Q19 1 -0.0172 -0.3885 0.6622 11.00000 0.05 0.14 Q20 1 0.1073 -0.2020 0.5283 11.00000 0.05 0.13 Q21 1 0.0432 0.5837 0.1772 11.00000 0.05 0.13 Q22 1 0.1251 -0.2719 0.6215 11.00000 0.05 0.13 Q23 1 -0.1338 -0.2041 0.4491 11.00000 0.05 0.12 Q24 1 0.0918 -0.0148 0.1999 11.00000 0.05 0.12 Q25 1 0.0796 -0.0004 0.3026 11.00000 0.05 0.12 ; _shelx_res_checksum 89293 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si01 Si 0.17254(4) 0.03145(9) 0.37495(8) 0.0848(6) Uani 1 1 d D . . . . N10 N 0.0107(4) 0.0406(13) 0.3076(7) 0.061(3) Uani 0.5 1 d . . P . . C40 C -0.0168(2) 0.0277(8) 0.1053(6) 0.081(2) Uani 0.5 1 d . . P . . H40A H -0.0220 -0.0505 0.0887 0.121 Uiso 0.5 1 calc R U P . . H40B H 0.0097 0.0533 0.1042 0.121 Uiso 0.5 1 calc R U P . . H40C H -0.0424 0.0714 0.0647 0.121 Uiso 0.5 1 calc R U P . . C01 C 0.1156(2) 0.0324(5) 0.2982(5) 0.0610(18) Uani 0.5 1 d D . P B . C02 C 0.0897(3) 0.0357(8) 0.3358(8) 0.058(3) Uani 0.5 1 d D . P . . H02 H 0.1025 0.0352 0.3970 0.070 Uiso 0.5 1 calc R U P B . C03 C 0.0436(4) 0.0398(12) 0.2824(10) 0.047(4) Uani 0.5 1 d D . P B . C04 C 0.0237(2) 0.0415(5) 0.1937(5) 0.0507(16) Uani 0.5 1 d D . P . . C05 C 0.0504(2) 0.0387(5) 0.1563(5) 0.0628(18) Uani 0.5 1 d D . P B . H05 H 0.0379 0.0405 0.0952 0.075 Uiso 0.5 1 calc R U P . . C06 C 0.0952(2) 0.0332(5) 0.2084(5) 0.0621(18) Uani 0.5 1 d D . P . . H06 H 0.1133 0.0297 0.1820 0.075 Uiso 0.5 1 calc R U P B . C07 C 0.1096(3) 0.0383(8) 0.3613(6) 0.052(2) Uani 0.5 1 d D . P B . C08 C 0.0726(3) 0.0400(5) 0.2784(6) 0.0530(17) Uani 0.5 1 d D . P . . H08 H 0.0603 0.0588 0.2190 0.064 Uiso 0.5 1 calc R U P B . C09 C 0.0295(5) 0.0417(11) 0.2693(9) 0.045(3) Uani 0.5 1 d D . P B . C10 C 0.0225(4) 0.0438(12) 0.3397(7) 0.047(3) Uani 0.5 1 d D . P . . C11 C 0.0599(2) 0.0406(6) 0.4221(4) 0.0633(19) Uani 0.5 1 d D . P B . H11 H 0.0562 0.0393 0.4718 0.076 Uiso 0.5 1 calc R U P . . C12 C 0.1022(2) 0.0394(5) 0.4322(4) 0.0610(18) Uani 0.5 1 d D . P . . H12 H 0.1269 0.0393 0.4889 0.073 Uiso 0.5 1 calc R U P B . C13 C 0.19518(11) 0.1732(3) 0.4096(2) 0.0638(10) Uani 1 1 d . . . . . H13A H 0.1924 0.1926 0.4610 0.077 Uiso 1 1 calc R U . . . H13B H 0.2271 0.1710 0.4282 0.077 Uiso 1 1 calc R U . . . C14 C 0.17430(13) 0.2664(3) 0.3435(2) 0.0763(11) Uani 1 1 d . . . . . H14A H 0.1763 0.2469 0.2912 0.092 Uiso 1 1 calc R U . . . H14B H 0.1426 0.2714 0.3264 0.092 Uiso 1 1 calc R U . . . C15 C 0.19534(16) 0.3792(3) 0.3752(3) 0.0850(13) Uani 1 1 d . . . . . H15A H 0.1949 0.3956 0.4294 0.102 Uiso 1 1 calc R U . . . H15B H 0.2267 0.3738 0.3899 0.102 Uiso 1 1 calc R U . . . C16 C 0.1758(2) 0.4742(4) 0.3169(3) 0.1035(15) Uani 1 1 d . . . . . H16A H 0.1960 0.5385 0.3396 0.124 Uiso 1 1 calc R U . . . H16B H 0.1718 0.4559 0.2590 0.124 Uiso 1 1 calc R U . . . C17 C 0.13523(19) 0.5010(5) 0.3101(4) 0.1188(19) Uani 1 1 d . . . . . H17A H 0.1390 0.5074 0.3690 0.143 Uiso 1 1 calc R U . . . H17B H 0.1143 0.4396 0.2806 0.143 Uiso 1 1 calc R U . . . C18 C 0.1137(2) 0.6141(5) 0.2584(3) 0.129(2) Uani 1 1 d . . . . . H18A H 0.1344 0.6766 0.2859 0.155 Uiso 1 1 calc R U . . . H18B H 0.1074 0.6076 0.1978 0.155 Uiso 1 1 calc R U . . . C19 C 0.07279(18) 0.6329(4) 0.2612(3) 0.1058(16) Uani 1 1 d . . . . . H19A H 0.0800 0.6357 0.3225 0.127 Uiso 1 1 calc R U . . . H19B H 0.0532 0.5685 0.2344 0.127 Uiso 1 1 calc R U . . . C20 C 0.04749(17) 0.7361(4) 0.2170(3) 0.0981(15) Uani 1 1 d . . . . . H20A H 0.0446 0.7413 0.1588 0.118 Uiso 1 1 calc R U . . . H20B H 0.0641 0.8017 0.2505 0.118 Uiso 1 1 calc R U . . . C21 C 0.00113(16) 0.7365(4) 0.2086(3) 0.0933(14) Uani 1 1 d . . . . . H21A H -0.0148 0.8026 0.1748 0.112 Uiso 1 1 calc R U . . . H21B H -0.0150 0.6707 0.1746 0.112 Uiso 1 1 calc R U . . . C22 C 0.19680(13) -0.0662(3) 0.4673(3) 0.0830(12) Uani 1 1 d . U . . . H22A H 0.2293 -0.0649 0.4916 0.100 Uiso 1 1 calc R U . . . H22B H 0.1905 -0.0371 0.5124 0.100 Uiso 1 1 calc R U . . . C23 C 0.18207(15) -0.1860(4) 0.4512(3) 0.0996(15) Uani 1 1 d . U . . . H23A H 0.1940 -0.2207 0.4164 0.120 Uiso 1 1 calc R U . . . H23B H 0.1494 -0.1879 0.4165 0.120 Uiso 1 1 calc R U . . . C24 C 0.19614(19) -0.2552(6) 0.5322(4) 0.151(3) Uani 1 1 d . . . . . H24A H 0.1931 -0.3340 0.5150 0.181 Uiso 1 1 calc R U . . . H24B H 0.2280 -0.2413 0.5713 0.181 Uiso 1 1 calc R U . . . C25 C 0.17259(19) -0.2394(5) 0.5845(3) 0.129(2) Uani 1 1 d . . . . . H25A H 0.1860 -0.2893 0.6352 0.154 Uiso 1 1 calc R U . . . H25B H 0.1772 -0.1624 0.6062 0.154 Uiso 1 1 calc R U . . . C26 C 0.12360(16) -0.2621(4) 0.5338(3) 0.0984(15) Uani 1 1 d . . . . . H26A H 0.1187 -0.3269 0.4961 0.118 Uiso 1 1 calc R U . . . H26B H 0.1090 -0.1978 0.4959 0.118 Uiso 1 1 calc R U . . . C27 C 0.1015(2) -0.2840(4) 0.5879(3) 0.1143(18) Uani 1 1 d . . . . . H27A H 0.1151 -0.3509 0.6232 0.137 Uiso 1 1 calc R U . . . H27B H 0.1082 -0.2212 0.6283 0.137 Uiso 1 1 calc R U . . . C28 C 0.05369(19) -0.2998(4) 0.5410(3) 0.1017(15) Uani 1 1 d . . . . . H28A H 0.0469 -0.3574 0.4965 0.122 Uiso 1 1 calc R U . . . H28B H 0.0400 -0.2301 0.5103 0.122 Uiso 1 1 calc R U . . . C29 C 0.0317(2) -0.3323(5) 0.5931(4) 0.124(2) Uani 1 1 d . . . . . H29A H 0.0439 -0.4043 0.6213 0.149 Uiso 1 1 calc R U . . . H29B H 0.0394 -0.2768 0.6393 0.149 Uiso 1 1 calc R U . . . C30 C -0.0174(3) -0.3418(5) 0.5420(5) 0.141(2) Uani 1 1 d D U . . . H30A H -0.0233 -0.3882 0.4915 0.169 Uiso 1 1 calc R U . A 1 H30B H -0.0280 -0.2667 0.5189 0.169 Uiso 1 1 calc R U . A 1 C31 C -0.0504(4) -0.3851(18) 0.5731(9) 0.135(7) Uani 0.496(7) 1 d D U P B 1 H31A H -0.0351 -0.4473 0.6128 0.162 Uiso 0.496(7) 1 calc R U P B 1 H31B H -0.0523 -0.3252 0.6092 0.162 Uiso 0.496(7) 1 calc R U P B 1 C32 C -0.0982(5) -0.4244(14) 0.5148(11) 0.092(5) Uani 0.496(7) 1 d D U P B 1 H32A H -0.0992 -0.4824 0.4744 0.110 Uiso 0.496(7) 1 calc R U P B 1 H32B H -0.1106 -0.4553 0.5502 0.110 Uiso 0.496(7) 1 calc R U P B 1 C33 C -0.1246(3) -0.3232(11) 0.4648(8) 0.103(3) Uani 0.496(7) 1 d D U P B 1 H33A H -0.1113 -0.2920 0.4311 0.124 Uiso 0.496(7) 1 calc R U P B 1 H33B H -0.1233 -0.2660 0.5060 0.124 Uiso 0.496(7) 1 calc R U P B 1 C34 C -0.1741(4) -0.3550(14) 0.4020(10) 0.108(4) Uani 0.496(7) 1 d D U P B 1 H34A H -0.1755 -0.4026 0.3553 0.130 Uiso 0.496(7) 1 calc R U P B 1 H34B H -0.1854 -0.3986 0.4344 0.130 Uiso 0.496(7) 1 calc R U P B 1 C35 C -0.2007(5) -0.2664(16) 0.3661(10) 0.094(4) Uani 0.496(7) 1 d D U P B 1 H35A H -0.1968 -0.2177 0.4141 0.113 Uiso 0.496(7) 1 calc R U P B 1 H35B H -0.2315 -0.2938 0.3383 0.113 Uiso 0.496(7) 1 calc R U P B 1 C36 C -0.1969(5) -0.1958(13) 0.3020(7) 0.127(5) Uani 0.496(7) 1 d D U P B 1 H36A H -0.2082 -0.2384 0.2477 0.152 Uiso 0.496(7) 1 calc R U P B 1 H36B H -0.1651 -0.1818 0.3232 0.152 Uiso 0.496(7) 1 calc R U P B 1 C37 C -0.2207(5) -0.0835(12) 0.2802(8) 0.106(4) Uani 0.496(7) 1 d D U P B 1 H37A H -0.2524 -0.0928 0.2619 0.127 Uiso 0.496(7) 1 calc R U P B 1 H37B H -0.2072 -0.0332 0.3306 0.127 Uiso 0.496(7) 1 calc R U P B 1 C38 C -0.2146(4) -0.0390(11) 0.2063(8) 0.072(3) Uani 0.496(7) 1 d D U P B 1 H38A H -0.2308 0.0320 0.1877 0.087 Uiso 0.496(7) 1 calc R U P B 1 H38B H -0.2295 -0.0910 0.1573 0.087 Uiso 0.496(7) 1 calc R U P B 1 C39 C 0.1675(3) -0.0188(6) 0.2799(5) 0.065(2) Uani 0.496(7) 1 d D . P B 1 H39A H 0.1505 -0.0888 0.2639 0.078 Uiso 0.496(7) 1 calc R U P B 1 H39B H 0.1517 0.0353 0.2327 0.078 Uiso 0.496(7) 1 calc R U P B 1 C131 C -0.0287(5) -0.3573(13) 0.6169(9) 0.122(4) Uani 0.504(7) 1 d D U P B 2 H13C H -0.0230 -0.4341 0.6391 0.146 Uiso 0.504(7) 1 calc R U P B 2 H13D H -0.0116 -0.3056 0.6652 0.146 Uiso 0.504(7) 1 calc R U P B 2 C132 C -0.0774(4) -0.3308(10) 0.5727(8) 0.121(4) Uani 0.504(7) 1 d D U P B 2 H13E H -0.0822 -0.2524 0.5542 0.146 Uiso 0.504(7) 1 calc R U P B 2 H13F H -0.0890 -0.3425 0.6133 0.146 Uiso 0.504(7) 1 calc R U P B 2 C133 C -0.1015(6) -0.4063(17) 0.4941(13) 0.127(7) Uani 0.504(7) 1 d D U P B 2 H13G H -0.0958 -0.4842 0.5137 0.153 Uiso 0.504(7) 1 calc R U P B 2 H13H H -0.0891 -0.3944 0.4549 0.153 Uiso 0.504(7) 1 calc R U P B 2 C134 C -0.1515(6) -0.3880(11) 0.4432(10) 0.121(5) Uani 0.504(7) 1 d D U P B 2 H13I H -0.1656 -0.4444 0.3971 0.145 Uiso 0.504(7) 1 calc R U P B 2 H13J H -0.1644 -0.3938 0.4820 0.145 Uiso 0.504(7) 1 calc R U P B 2 C135 C -0.1591(4) -0.2739(8) 0.4043(7) 0.098(4) Uani 0.504(7) 1 d D U P B 2 H13K H -0.1548 -0.2191 0.4492 0.117 Uiso 0.504(7) 1 calc R U P B 2 H13L H -0.1364 -0.2593 0.3869 0.117 Uiso 0.504(7) 1 calc R U P B 2 C136 C -0.2038(6) -0.2562(12) 0.3273(11) 0.115(6) Uani 0.504(7) 1 d D . P B 2 H13M H -0.2269 -0.2851 0.3398 0.138 Uiso 0.504(7) 1 calc R U P B 2 H13N H -0.2059 -0.2971 0.2771 0.138 Uiso 0.504(7) 1 calc R U P B 2 C137 C -0.2116(5) -0.1316(10) 0.3058(11) 0.129(7) Uani 0.504(7) 1 d D . P B 2 H13O H -0.2433 -0.1123 0.2793 0.154 Uiso 0.504(7) 1 calc R U P B 2 H13P H -0.1945 -0.0855 0.3578 0.154 Uiso 0.504(7) 1 calc R U P B 2 C138 C -0.1947(3) -0.1185(8) 0.2414(6) 0.087(3) Uani 0.504(7) 1 d D . P B 2 H13Q H -0.1623 -0.1299 0.2725 0.105 Uiso 0.504(7) 1 calc R U P B 2 H13R H -0.2079 -0.1777 0.1975 0.105 Uiso 0.504(7) 1 calc R U P B 2 C139 C 0.2043(4) -0.0091(12) 0.3045(10) 0.097(4) Uani 0.504(7) 1 d D . P B 2 H13S H 0.1973 0.0495 0.2607 0.116 Uiso 0.504(7) 1 calc R U P B 2 H13T H 0.2366 -0.0056 0.3446 0.116 Uiso 0.504(7) 1 calc R U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si01 0.0630(8) 0.0748(8) 0.0760(9) -0.0069(6) 0.0022(6) -0.0045(5) N10 0.047(7) 0.081(5) 0.047(7) -0.021(5) 0.018(6) -0.001(5) C40 0.045(4) 0.137(8) 0.057(5) 0.014(5) 0.023(4) -0.004(4) C01 0.034(4) 0.062(4) 0.083(6) -0.015(4) 0.025(4) -0.005(3) C02 0.038(6) 0.069(5) 0.048(7) -0.017(5) 0.006(5) 0.004(5) C03 0.015(8) 0.059(5) 0.067(7) -0.018(4) 0.019(6) -0.007(4) C04 0.037(4) 0.045(3) 0.073(5) 0.007(3) 0.029(3) 0.001(3) C05 0.043(4) 0.081(5) 0.067(4) 0.010(4) 0.028(3) 0.005(3) C06 0.048(4) 0.061(4) 0.072(5) 0.000(3) 0.025(4) -0.005(3) C07 0.036(5) 0.061(4) 0.046(5) -0.006(4) 0.009(5) 0.000(4) C08 0.043(5) 0.052(4) 0.056(5) 0.008(4) 0.018(4) 0.005(3) C09 0.018(9) 0.049(5) 0.063(7) 0.001(4) 0.015(7) -0.005(4) C10 0.041(7) 0.047(4) 0.053(9) -0.005(6) 0.023(6) -0.005(4) C11 0.046(4) 0.085(5) 0.050(4) -0.024(3) 0.016(3) -0.008(3) C12 0.040(4) 0.085(5) 0.052(4) -0.017(3) 0.018(3) -0.006(3) C13 0.0474(19) 0.082(2) 0.056(2) -0.0062(18) 0.0205(16) -0.0142(16) C14 0.068(2) 0.086(3) 0.059(2) -0.009(2) 0.0188(19) -0.003(2) C15 0.109(4) 0.077(3) 0.064(2) -0.004(2) 0.039(2) -0.008(2) C16 0.120(4) 0.113(4) 0.087(3) 0.004(3) 0.058(3) 0.009(3) C17 0.113(5) 0.147(5) 0.084(3) 0.003(3) 0.039(3) -0.033(4) C18 0.132(5) 0.162(6) 0.089(3) 0.025(4) 0.050(3) 0.064(4) C19 0.142(5) 0.083(3) 0.100(3) 0.010(3) 0.065(3) 0.019(3) C20 0.122(4) 0.072(3) 0.098(3) 0.015(2) 0.052(3) 0.002(3) C21 0.101(4) 0.064(2) 0.103(3) 0.002(2) 0.040(3) 0.000(2) C22 0.053(2) 0.085(3) 0.087(3) 0.000(2) 0.016(2) -0.001(2) C23 0.073(3) 0.118(4) 0.095(3) 0.015(3) 0.031(3) 0.007(3) C24 0.080(4) 0.190(6) 0.136(5) 0.093(5) 0.016(4) -0.008(4) C25 0.105(4) 0.148(5) 0.088(3) 0.046(3) 0.012(3) -0.021(4) C26 0.096(4) 0.104(3) 0.076(3) 0.019(3) 0.027(3) -0.007(3) C27 0.142(5) 0.112(4) 0.068(3) 0.007(3) 0.035(3) -0.002(3) C28 0.124(5) 0.095(3) 0.099(3) 0.007(3) 0.064(3) 0.012(3) C29 0.186(7) 0.114(4) 0.111(4) 0.031(3) 0.102(5) 0.026(4) C30 0.191(7) 0.129(4) 0.176(6) 0.064(4) 0.146(6) 0.055(4) C31 0.092(9) 0.216(18) 0.106(10) 0.033(10) 0.054(7) -0.015(9) C32 0.125(9) 0.080(8) 0.113(8) 0.020(7) 0.091(7) 0.002(6) C33 0.090(7) 0.111(9) 0.129(9) -0.005(7) 0.069(6) -0.006(6) C34 0.095(8) 0.127(11) 0.127(10) -0.008(8) 0.074(7) -0.015(7) C35 0.075(8) 0.126(10) 0.108(10) -0.024(7) 0.066(7) -0.035(6) C36 0.162(13) 0.141(11) 0.079(6) -0.009(7) 0.060(7) -0.073(9) C37 0.103(9) 0.131(11) 0.086(7) -0.034(7) 0.047(6) -0.028(8) C38 0.055(7) 0.106(9) 0.074(6) 0.012(6) 0.046(5) 0.006(6) C39 0.057(5) 0.073(5) 0.067(5) -0.003(4) 0.032(4) 0.004(4) C131 0.157(12) 0.113(9) 0.143(11) 0.052(8) 0.110(10) 0.035(9) C132 0.164(10) 0.117(9) 0.156(10) 0.036(7) 0.134(9) 0.044(7) C133 0.156(12) 0.100(11) 0.180(14) 0.049(10) 0.126(9) 0.010(8) C134 0.180(14) 0.104(9) 0.144(11) 0.035(8) 0.130(11) 0.025(9) C135 0.157(12) 0.071(6) 0.111(8) 0.010(5) 0.102(8) 0.001(6) C136 0.120(11) 0.095(9) 0.118(13) 0.027(10) 0.050(11) 0.007(7) C137 0.116(10) 0.076(8) 0.26(2) -0.013(9) 0.144(13) 0.024(7) C138 0.061(5) 0.099(7) 0.094(6) 0.018(5) 0.032(5) -0.011(5) C139 0.049(8) 0.135(10) 0.115(9) -0.045(7) 0.046(6) -0.007(6) 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C39 Si01 C01 73.0(4) . . C39 Si01 C22 115.2(3) . . C01 Si01 C22 122.6(3) . . C39 Si01 C13 118.3(3) . . C01 Si01 C13 112.4(2) . . C22 Si01 C13 110.98(17) . . C39 Si01 C07 107.6(4) . . C01 Si01 C07 36.4(4) . . C22 Si01 C07 97.2(3) . . C13 Si01 C07 104.6(3) . . C01 Si01 C139 105.0(5) . . C22 Si01 C139 103.6(5) . . C13 Si01 C139 98.8(4) . . C07 Si01 C139 140.5(5) . . C09 N10 C04 147.8(13) . 2 C09 N10 C09 90.3(14) . 2 C04 N10 C09 57.6(9) 2 2 C09 N10 C03 15.2(11) . . C04 N10 C03 163.0(10) 2 . C09 N10 C03 105.4(13) 2 . C09 N10 C40 142.6(12) . 2 C04 N10 C40 69.4(9) 2 2 C09 N10 C40 126.6(12) 2 2 C03 N10 C40 127.5(10) . 2 C09 N10 C03 97.2(14) . 2 C04 N10 C03 50.7(7) 2 2 C09 N10 C03 7.0(10) 2 2 C03 N10 C03 112.3(10) . 2 C40 N10 C03 119.6(11) 2 2 C09 N10 N10 50.7(12) . 2 C04 N10 N10 97.2(9) 2 2 C09 N10 N10 39.6(8) 2 2 C03 N10 N10 65.8(10) . 2 C40 N10 N10 165.1(13) 2 2 C03 N10 N10 46.5(7) 2 2 N10 C40 H40A 109.5 2 . N10 C40 H40B 109.5 2 . H40A C40 H40B 109.5 . . N10 C40 H40C 109.5 2 . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . C02 C01 C08 38.6(5) . . C02 C01 C06 118.3(8) . . C08 C01 C06 79.8(6) . . C02 C01 Si01 112.4(7) . . C08 C01 Si01 150.8(7) . . C06 C01 Si01 129.3(5) . . C01 C02 C03 118.6(12) . . C01 C02 C09 120.4(11) . . C03 C02 C09 1.8(10) . . C01 C02 H02 120.7 . . C03 C02 H02 120.7 . . C09 C02 H02 118.9 . . C08 C03 C04 83.2(12) . . C08 C03 C02 39.5(7) . . C04 C03 C02 122.7(13) . . C08 C03 N10 167.5(14) . . C04 C03 N10 109.3(10) . . C02 C03 N10 128.0(12) . . C08 C03 N10 124.9(15) . 2 C04 C03 N10 41.6(7) . 2 C02 C03 N10 164.2(15) . 2 N10 C03 N10 67.7(10) . 2 C08 C03 C07 40.7(7) . . C04 C03 C07 123.9(11) . . C02 C03 C07 2.0(6) . . N10 C03 C07 126.8(10) . . N10 C03 C07 165.6(12) 2 . N10 C04 C03 87.7(9) 2 . N10 C04 C05 154.1(9) 2 . C03 C04 C05 118.1(8) . . N10 C04 C10 20.5(8) 2 2 C03 C04 C10 108.2(9) . 2 C05 C04 C10 133.7(8) . 2 C06 C05 C04 119.0(7) . . C06 C05 H05 120.5 . . C04 C05 H05 120.5 . . C05 C06 C01 123.3(7) . . C05 C06 H06 118.4 . . C01 C06 H06 118.4 . . C12 C07 C08 117.9(8) . . C12 C07 C03 88.8(7) . . C08 C07 C03 29.1(6) . . C12 C07 Si01 122.5(6) . . C08 C07 Si01 119.6(7) . . C03 C07 Si01 148.6(7) . . C03 C08 C01 162.9(12) . . C03 C08 C07 110.2(11) . . C01 C08 C07 53.2(7) . . C03 C08 C09 9.2(13) . . C01 C08 C09 171.9(11) . . C07 C08 C09 119.4(9) . . C03 C08 H08 98.5 . . C01 C08 H08 98.5 . . C07 C08 H08 148.5 . . C09 C08 H08 89.4 . . N10 C09 C10 20.9(8) . . N10 C09 N10 89.7(14) . 2 C10 C09 N10 110.6(15) . 2 N10 C09 C08 143.2(14) . . C10 C09 C08 122.3(12) . . N10 C09 C08 127.0(13) 2 . N10 C09 C09 50.4(9) . 2 C10 C09 C09 71.2(11) . 2 N10 C09 C09 39.4(10) 2 2 C08 C09 C09 166.4(16) . 2 N10 C09 C02 114.6(12) . . C10 C09 C02 93.8(9) . . N10 C09 C02 155.4(13) 2 . C08 C09 C02 28.6(6) . . C09 C09 C02 164.8(14) 2 . N10 C09 C10 94.2(12) . 2 C10 C09 C10 115.0(10) . 2 N10 C09 C10 4.6(10) 2 2 C08 C09 C10 122.7(12) . 2 C09 C09 C10 43.8(7) 2 2 C02 C09 C10 151.2(12) . 2 C40 C10 C09 168.7(15) 2 . C40 C10 C11 63.1(7) 2 . C09 C10 C11 117.3(12) . . C40 C10 C04 73.3(9) 2 2 C09 C10 C04 106.5(9) . 2 C11 C10 C04 136.1(11) . 2 C40 C10 C09 114.2(11) 2 2 C09 C10 C09 65.0(10) . 2 C11 C10 C09 176.7(11) . 2 C04 C10 C09 41.6(6) 2 2 C12 C11 C10 121.2(8) . . C12 C11 H11 119.4 . . C10 C11 H11 119.4 . . C11 C12 C07 121.9(6) . . C11 C12 H12 119.1 . . C07 C12 H12 119.1 . . C14 C13 Si01 117.4(2) . . C14 C13 H13A 108.0 . . Si01 C13 H13A 108.0 . . C14 C13 H13B 108.0 . . Si01 C13 H13B 108.0 . . H13A C13 H13B 107.2 . . C15 C14 C13 114.6(3) . . C15 C14 H14A 108.6 . . C13 C14 H14A 108.6 . . C15 C14 H14B 108.6 . . C13 C14 H14B 108.6 . . H14A C14 H14B 107.6 . . C16 C15 C14 117.9(4) . . C16 C15 H15A 107.8 . . C14 C15 H15A 107.8 . . C16 C15 H15B 107.8 . . C14 C15 H15B 107.8 . . H15A C15 H15B 107.2 . . C17 C16 C15 109.9(5) . . C17 C16 H16A 109.7 . . C15 C16 H16A 109.7 . . C17 C16 H16B 109.7 . . C15 C16 H16B 109.7 . . H16A C16 H16B 108.2 . . C16 C17 C18 114.5(5) . . C16 C17 H17A 108.6 . . C18 C17 H17A 108.6 . . C16 C17 H17B 108.6 . . C18 C17 H17B 108.6 . . H17A C17 H17B 107.6 . . C19 C18 C17 107.5(5) . . C19 C18 H18A 110.2 . . C17 C18 H18A 110.2 . . C19 C18 H18B 110.2 . . C17 C18 H18B 110.2 . . H18A C18 H18B 108.5 . . C18 C19 C20 116.1(4) . . C18 C19 H19A 108.3 . . C20 C19 H19A 108.3 . . C18 C19 H19B 108.3 . . C20 C19 H19B 108.3 . . H19A C19 H19B 107.4 . . C19 C20 C21 111.6(4) . . C19 C20 H20A 109.3 . . C21 C20 H20A 109.3 . . C19 C20 H20B 109.3 . . C21 C20 H20B 109.3 . . H20A C20 H20B 108.0 . . C21 C21 C20 117.0(5) 2 . C21 C21 H21A 108.1 2 . C20 C21 H21A 108.1 . . C21 C21 H21B 108.1 2 . C20 C21 H21B 108.1 . . H21A C21 H21B 107.3 . . C23 C22 Si01 118.4(3) . . C23 C22 H22A 107.7 . . Si01 C22 H22A 107.7 . . C23 C22 H22B 107.7 . . Si01 C22 H22B 107.7 . . H22A C22 H22B 107.1 . . C22 C23 C24 115.1(5) . . C22 C23 H23A 108.5 . . C24 C23 H23A 108.5 . . C22 C23 H23B 108.5 . . C24 C23 H23B 108.5 . . H23A C23 H23B 107.5 . . C25 C24 C23 119.1(5) . . C25 C24 H24A 107.5 . . C23 C24 H24A 107.5 . . C25 C24 H24B 107.5 . . C23 C24 H24B 107.5 . . H24A C24 H24B 107.0 . . C26 C25 C24 113.5(5) . . C26 C25 H25A 108.9 . . C24 C25 H25A 108.9 . . C26 C25 H25B 108.9 . . C24 C25 H25B 108.9 . . H25A C25 H25B 107.7 . . C25 C26 C27 115.2(4) . . C25 C26 H26A 108.5 . . C27 C26 H26A 108.5 . . C25 C26 H26B 108.5 . . C27 C26 H26B 108.5 . . H26A C26 H26B 107.5 . . C28 C27 C26 116.6(4) . . C28 C27 H27A 108.2 . . C26 C27 H27A 108.2 . . C28 C27 H27B 108.2 . . C26 C27 H27B 108.2 . . H27A C27 H27B 107.3 . . C27 C28 C29 117.3(5) . . C27 C28 H28A 108.0 . . C29 C28 H28A 108.0 . . C27 C28 H28B 108.0 . . C29 C28 H28B 108.0 . . H28A C28 H28B 107.2 . . C30 C29 C28 114.7(5) . . C30 C29 H29A 108.6 . . C28 C29 H29A 108.6 . . C30 C29 H29B 108.6 . . C28 C29 H29B 108.6 . . H29A C29 H29B 107.6 . . C29 C30 C131 100.3(7) . . C29 C30 C31 128.3(7) . . C29 C30 H30A 105.2 . . C31 C30 H30A 105.2 . . C29 C30 H30B 105.2 . . C31 C30 H30B 105.2 . . H30A C30 H30B 105.9 . . C32 C31 C30 126.4(13) . . C32 C31 H31A 105.7 . . C30 C31 H31A 105.7 . . C32 C31 H31B 105.7 . . C30 C31 H31B 105.7 . . H31A C31 H31B 106.2 . . C33 C32 C31 106.6(13) . . C33 C32 H32A 110.4 . . C31 C32 H32A 110.4 . . C33 C32 H32B 110.4 . . C31 C32 H32B 110.4 . . H32A C32 H32B 108.6 . . C32 C33 C34 110.7(13) . . C32 C33 H33A 109.5 . . C34 C33 H33A 109.5 . . C32 C33 H33B 109.5 . . C34 C33 H33B 109.5 . . H33A C33 H33B 108.1 . . C35 C34 C33 113.4(14) . . C35 C34 H34A 108.9 . . C33 C34 H34A 108.9 . . C35 C34 H34B 108.9 . . C33 C34 H34B 108.9 . . H34A C34 H34B 107.7 . . C34 C35 C36 121.6(15) . . C34 C35 H35A 106.9 . . C36 C35 H35A 106.9 . . C34 C35 H35B 106.9 . . C36 C35 H35B 106.9 . . H35A C35 H35B 106.7 . . C35 C36 C37 117.8(14) . . C35 C36 H36A 107.9 . . C37 C36 H36A 107.9 . . C35 C36 H36B 107.9 . . C37 C36 H36B 107.9 . . H36A C36 H36B 107.2 . . C38 C37 C36 104.2(10) . . C38 C37 H37A 110.9 . . C36 C37 H37A 110.9 . . C38 C37 H37B 110.9 . . C36 C37 H37B 110.9 . . H37A C37 H37B 108.9 . . C37 C38 C39 119.9(10) . 2 C37 C38 H38A 107.4 . . C39 C38 H38A 107.4 2 . C37 C38 H38B 107.4 . . C39 C38 H38B 107.4 2 . H38A C38 H38B 106.9 . . C38 C39 Si01 107.8(6) 2 . C38 C39 H39A 110.1 2 . Si01 C39 H39A 110.1 . . C38 C39 H39B 110.1 2 . Si01 C39 H39B 110.1 . . H39A C39 H39B 108.5 . . C132 C131 C30 102.3(9) . . C132 C131 H13C 111.3 . . C30 C131 H13C 111.3 . . C132 C131 H13D 111.3 . . C30 C131 H13D 111.3 . . H13C C131 H13D 109.2 . . C131 C132 C133 108.9(12) . . C131 C132 H13E 109.9 . . C133 C132 H13E 109.9 . . C131 C132 H13F 109.9 . . C133 C132 H13F 109.9 . . H13E C132 H13F 108.3 . . C132 C133 C134 114.2(17) . . C132 C133 H13G 108.7 . . C134 C133 H13G 108.7 . . C132 C133 H13H 108.7 . . C134 C133 H13H 108.7 . . H13G C133 H13H 107.6 . . C135 C134 C133 107.2(14) . . C135 C134 H13I 110.3 . . C133 C134 H13I 110.3 . . C135 C134 H13J 110.3 . . C133 C134 H13J 110.3 . . H13I C134 H13J 108.5 . . C136 C135 C134 114.7(12) . . C136 C135 H13K 108.6 . . C134 C135 H13K 108.6 . . C136 C135 H13L 108.6 . . C134 C135 H13L 108.6 . . H13K C135 H13L 107.6 . . C135 C136 C137 110.0(13) . . C135 C136 H13M 109.7 . . C137 C136 H13M 109.7 . . C135 C136 H13N 109.7 . . C137 C136 H13N 109.7 . . H13M C136 H13N 108.2 . . C138 C137 C136 101.6(11) . . C138 C137 H13O 111.4 . . C136 C137 H13O 111.4 . . C138 C137 H13P 111.4 . . C136 C137 H13P 111.4 . . H13O C137 H13P 109.3 . . C139 C138 C137 115.5(9) 2 . C139 C138 H13Q 108.4 2 . C137 C138 H13Q 108.4 . . C139 C138 H13R 108.4 2 . C137 C138 H13R 108.4 . . H13Q C138 H13R 107.5 . . C138 C139 Si01 119.2(8) 2 . C138 C139 H13S 107.5 2 . Si01 C139 H13S 107.5 . . C138 C139 H13T 107.5 2 . Si01 C139 H13T 107.5 . . H13S C139 H13T 107.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si01 C39 1.719(7) . Si01 C01 1.768(7) . Si01 C22 1.854(4) . Si01 C13 1.860(4) . Si01 C07 2.077(9) . Si01 C139 2.089(10) . N10 C09 1.15(2) . N10 C04 1.181(16) 2 N10 C09 1.394(16) 2 N10 C03 1.41(2) . N10 C40 1.459(14) 2 N10 C03 1.777(16) 2 N10 N10 1.80(2) 2 C40 N10 1.459(14) 2 C40 H40A 0.9800 . C40 H40B 0.9800 . C40 H40C 0.9800 . C01 C02 1.354(11) . C01 C08 1.357(11) . C01 C06 1.391(10) . C02 C03 1.407(12) . C02 C09 1.833(17) . C02 H02 0.9500 . C03 C08 1.044(16) . C03 C04 1.376(15) . C03 N10 1.777(16) 2 C03 C07 2.017(14) . C04 N10 1.181(16) 2 C04 C05 1.378(9) . C04 C10 1.411(14) 2 C05 C06 1.368(8) . C05 H05 0.9500 . C06 H06 0.9500 . C07 C12 1.400(11) . C07 C08 1.402(9) . C08 C09 1.425(12) . C08 H08 0.9500 . C09 C10 1.383(17) . C09 N10 1.394(16) 2 C09 C09 1.81(3) 2 C09 C10 1.892(19) 2 C10 C40 1.101(16) 2 C10 C11 1.403(12) . C10 C04 1.411(14) 2 C10 C09 1.892(19) 2 C11 C12 1.388(9) . C11 H11 0.9500 . C12 H12 0.9500 . C13 C14 1.529(5) . C13 H13A 0.9900 . C13 H13B 0.9900 . C14 C15 1.520(5) . C14 H14A 0.9900 . C14 H14B 0.9900 . C15 C16 1.471(6) . C15 H15A 0.9900 . C15 H15B 0.9900 . C16 C17 1.391(7) . C16 H16A 0.9900 . C16 H16B 0.9900 . C17 C18 1.612(7) . C17 H17A 0.9900 . C17 H17B 0.9900 . C18 C19 1.462(7) . C18 H18A 0.9900 . C18 H18B 0.9900 . C19 C20 1.506(6) . C19 H19A 0.9900 . C19 H19B 0.9900 . C20 C21 1.540(7) . C20 H20A 0.9900 . C20 H20B 0.9900 . C21 C21 1.508(9) 2 C21 H21A 0.9900 . C21 H21B 0.9900 . C22 C23 1.516(6) . C22 H22A 0.9900 . C22 H22B 0.9900 . C23 C24 1.522(7) . C23 H23A 0.9900 . C23 H23B 0.9900 . C24 C25 1.516(9) . C24 H24A 0.9900 . C24 H24B 0.9900 . C25 C26 1.509(7) . C25 H25A 0.9900 . C25 H25B 0.9900 . C26 C27 1.515(7) . C26 H26A 0.9900 . C26 H26B 0.9900 . C27 C28 1.460(7) . C27 H27A 0.9900 . C27 H27B 0.9900 . C28 C29 1.507(7) . C28 H28A 0.9900 . C28 H28B 0.9900 . C29 C30 1.494(9) . C29 H29A 0.9900 . C29 H29B 0.9900 . C30 C131 1.568(12) . C30 C31 1.580(13) . C30 H30A 0.9900 . C30 H30B 0.9900 . C31 C32 1.540(15) . C31 H31A 0.9900 . C31 H31B 0.9900 . C32 C33 1.525(15) . C32 H32A 0.9900 . C32 H32B 0.9900 . C33 C34 1.572(14) . C33 H33A 0.9900 . C33 H33B 0.9900 . C34 C35 1.35(2) . C34 H34A 0.9900 . C34 H34B 0.9900 . C35 C36 1.477(14) . C35 H35A 0.9900 . C35 H35B 0.9900 . C36 C37 1.537(15) . C36 H36A 0.9900 . C36 H36B 0.9900 . C37 C38 1.524(14) . C37 H37A 0.9900 . C37 H37B 0.9900 . C38 C39 1.548(10) 2 C38 H38A 0.9900 . C38 H38B 0.9900 . C39 C38 1.548(10) 2 C39 H39A 0.9900 . C39 H39B 0.9900 . C131 C132 1.506(14) . C131 H13C 0.9900 . C131 H13D 0.9900 . C132 C133 1.530(17) . C132 H13E 0.9900 . C132 H13F 0.9900 . C133 C134 1.530(16) . C133 H13G 0.9900 . C133 H13H 0.9900 . C134 C135 1.508(12) . C134 H13I 0.9900 . C134 H13J 0.9900 . C135 C136 1.499(15) . C135 H13K 0.9900 . C135 H13L 0.9900 . C136 C137 1.546(15) . C136 H13M 0.9900 . C136 H13N 0.9900 . C137 C138 1.525(13) . C137 H13O 0.9900 . C137 H13P 0.9900 . C138 C139 1.503(12) 2 C138 H13Q 0.9900 . C138 H13R 0.9900 . C139 C138 1.503(12) 2 C139 H13S 0.9900 . C139 H13T 0.9900 .