#------------------------------------------------------------------------------ #$Date: 2020-08-29 04:48:03 +0300 (Sat, 29 Aug 2020) $ #$Revision: 255731 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705320.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_7705320 loop_ _publ_author_name 'Leszczy\'nska, Kinga I.' 'Deglmann, Peter' 'Pr\"asang, Carsten' 'Huch, Volker' 'Zimmer, Michael' 'Schweinfurth, David' 'Scheschkewitz, David' _publ_section_title ; Pentamethylcyclopentadienyl-substituted hypersilylsilylene: reversible and irreversible activation of C=C double bonds and dihydrogen ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02943B _journal_year 2020 _chemical_formula_moiety 'C26 H54 N2 Si5' _chemical_formula_sum 'C26 H54 N2 Si5' _chemical_formula_weight 535.16 _chemical_properties_physical Air-sensitive,Moisture-sensitive _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' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-05-07 deposited with the CCDC. 2020-08-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.403(19) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 40.367(13) _cell_length_b 9.976(3) _cell_length_c 16.657(5) _cell_measurement_reflns_used 8772 _cell_measurement_temperature 142(2) _cell_measurement_theta_max 32.48 _cell_measurement_theta_min 2.40 _cell_volume 6618(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 142(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_unetI/netI 0.0302 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 59 _diffrn_reflns_limit_h_min -62 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 91027 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.367 _diffrn_reflns_theta_min 2.045 _exptl_absorpt_coefficient_mu 0.232 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.074 _exptl_crystal_description coboid _exptl_crystal_F_000 2352 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' _exptl_crystal_size_max 0.463 _exptl_crystal_size_mid 0.294 _exptl_crystal_size_min 0.104 _refine_diff_density_max 0.415 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 514 _refine_ls_number_reflns 12649 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0329 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+2.0260P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.0920 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9781 _reflns_number_total 12649 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02943b2.cif _cod_data_source_block sh3854 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7705320 _shelx_shelxl_version_number 2018/3 _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 0.900 _shelx_estimated_absorpt_t_max 0.976 _shelx_res_file ; TITL sh3854 in C2/c sh3854.res created by SHELXL-2018/3 at 13:05:12 on 05-May-2020 CELL 0.71073 40.36740 9.97640 16.65660 90.0000 99.4031 90.0000 ZERR 8.00 0.01300 0.00310 0.00520 0.0000 0.0185 0.0000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N SI UNIT 208 432 16 40 TEMP -130.500 SIZE 0.104 0.294 0.463 L.S. 4 BOND $H FMAP 2 PLAN -5 ACTA SIZE 0.104 0.294 0.463 TEMP -130.500 WGHT 0.045000 2.026000 FVAR 0.21071 SI1 4 0.152733 0.789982 0.174267 11.00000 0.01720 0.02041 = 0.01657 0.00078 0.00129 -0.00030 SI2 4 0.093854 0.736727 0.136492 11.00000 0.01647 0.02058 = 0.01927 -0.00127 0.00109 -0.00031 SI3 4 0.066862 0.920162 0.189141 11.00000 0.02209 0.02725 = 0.03030 -0.00439 0.00304 0.00472 SI4 4 0.058584 0.547930 0.143803 11.00000 0.02322 0.02535 = 0.03532 -0.00015 0.00042 -0.00566 SI5 4 0.086663 0.786949 -0.003822 11.00000 0.02335 0.03500 = 0.01928 -0.00085 -0.00065 0.00223 N1 3 0.149225 0.775583 0.356372 11.00000 0.02195 0.02197 = 0.01980 0.00086 0.00409 0.00231 N2 3 0.177719 0.941553 0.322387 11.00000 0.02196 0.02307 = 0.02062 -0.00195 0.00062 -0.00121 C1 1 0.185407 0.631798 0.186023 11.00000 0.01977 0.02385 = 0.01733 0.00108 0.00315 0.00251 C2 1 0.217267 0.699360 0.223589 11.00000 0.01706 0.02682 = 0.02497 0.00242 0.00448 0.00192 C3 1 0.225676 0.657823 0.301885 11.00000 0.01908 0.02997 = 0.02254 -0.00075 0.00000 0.00427 C4 1 0.202205 0.553838 0.317961 11.00000 0.02345 0.02700 = 0.01994 0.00402 0.00526 0.00730 C5 1 0.179371 0.533203 0.248973 11.00000 0.02229 0.02078 = 0.02300 0.00225 0.00593 0.00319 C6 1 0.185254 0.573439 0.101127 11.00000 0.03744 0.03434 = 0.02084 -0.00296 0.00460 0.00839 C7 1 0.235921 0.793419 0.177493 11.00000 0.02371 0.03679 = 0.04068 0.00974 0.00964 -0.00059 C8 1 0.254184 0.707093 0.364461 11.00000 0.02874 0.05136 = 0.03521 -0.00325 -0.00874 0.00021 C9 1 0.204135 0.486245 0.399059 11.00000 0.03662 0.04409 = 0.02338 0.01125 0.00924 0.01450 C10 1 0.153497 0.425030 0.232467 11.00000 0.03238 0.02410 = 0.03988 0.00140 0.00669 -0.00274 C11 1 0.158669 0.835291 0.290685 11.00000 0.01765 0.02051 = 0.01944 -0.00010 0.00206 0.00095 C12 1 0.162871 0.840879 0.428024 11.00000 0.02943 0.02903 = 0.01814 -0.00078 0.00279 0.00786 C13 1 0.180631 0.946167 0.406515 11.00000 0.02889 0.02844 = 0.02022 -0.00433 -0.00178 0.00404 C14 1 0.127101 0.660042 0.354129 11.00000 0.02662 0.02672 = 0.02919 0.00399 0.00888 -0.00199 C15 1 0.157961 0.791652 0.509762 11.00000 0.05110 0.04026 = 0.02133 0.00417 0.00754 0.01220 C16 1 0.200025 1.052801 0.457034 11.00000 0.05289 0.03927 = 0.03056 -0.01118 -0.00631 -0.00599 C17 1 0.193721 1.039054 0.276080 11.00000 0.03779 0.03139 = 0.03177 -0.00264 0.00565 -0.01415 C18 1 0.095348 1.068951 0.214746 11.00000 0.03994 0.02758 = 0.06637 -0.01156 0.00391 0.00198 C19 1 0.051049 0.871390 0.284721 11.00000 0.03972 0.05305 = 0.03386 -0.00798 0.01217 0.00884 C20 1 0.029226 0.982389 0.116667 11.00000 0.03221 0.04893 = 0.04405 0.00105 0.00159 0.01628 C21 1 0.067981 0.412448 0.072100 11.00000 0.04906 0.03127 = 0.05367 -0.01158 -0.00352 -0.00227 C22 1 0.013457 0.598157 0.111958 11.00000 0.02373 0.04620 = 0.05595 0.00070 -0.00096 -0.00839 C23 1 0.060364 0.468993 0.247026 11.00000 0.03723 0.04244 = 0.04894 0.01293 0.00620 -0.01120 C24 1 0.096850 0.968284 -0.017216 11.00000 0.05360 0.05110 = 0.03718 0.01495 0.00174 -0.01454 C25 1 0.116661 0.689426 -0.055676 11.00000 0.04697 0.08717 = 0.02469 -0.00715 0.00505 0.02431 C26 1 0.043694 0.754106 -0.063393 11.00000 0.03298 0.04925 = 0.03274 -0.00233 -0.00959 0.00204 H1 2 0.189725 0.642528 0.061584 11.00000 0.04430 H2 2 0.163752 0.529935 0.078536 11.00000 0.04166 H3 2 0.202548 0.502523 0.102825 11.00000 0.04094 H4 2 0.221552 0.862360 0.151108 11.00000 0.04638 H5 2 0.244821 0.742869 0.134151 11.00000 0.05391 H6 2 0.254472 0.835453 0.209221 11.00000 0.05057 H7 2 0.267569 0.771698 0.342124 11.00000 0.06449 H8 2 0.268045 0.631375 0.389108 11.00000 0.06779 H9 2 0.245816 0.745011 0.408642 11.00000 0.06150 H10 2 0.201625 0.547436 0.440870 11.00000 0.05595 H11 2 0.187580 0.419370 0.400176 11.00000 0.05095 H12 2 0.225169 0.441642 0.417472 11.00000 0.04125 H13 2 0.132435 0.458959 0.204526 11.00000 0.04364 H14 2 0.160237 0.354434 0.196339 11.00000 0.04812 H15 2 0.148918 0.379952 0.280889 11.00000 0.05154 H16 2 0.108141 0.680980 0.379550 11.00000 0.04341 H17 2 0.138486 0.585573 0.382120 11.00000 0.04257 H18 2 0.118589 0.638676 0.299614 11.00000 0.04100 H19 2 0.134796 0.777687 0.510022 11.00000 0.04413 H20 2 0.165129 0.859234 0.549570 11.00000 0.04938 H21 2 0.170353 0.710482 0.523861 11.00000 0.05485 H22 2 0.223312 1.046258 0.457296 11.00000 0.06650 H23 2 0.195514 1.047222 0.512133 11.00000 0.06394 H24 2 0.193197 1.139629 0.435007 11.00000 0.06217 H25 2 0.218097 1.030620 0.290491 11.00000 0.04648 H26 2 0.186800 1.129123 0.290415 11.00000 0.04993 H27 2 0.186032 1.021298 0.217287 11.00000 0.04482 H28 2 0.081678 1.144863 0.227065 11.00000 0.07864 H29 2 0.105910 1.093338 0.174302 11.00000 0.06791 H30 2 0.112112 1.050723 0.260170 11.00000 0.06158 H31 2 0.039276 0.946076 0.303900 11.00000 0.06009 H32 2 0.068216 0.845732 0.327710 11.00000 0.06569 H33 2 0.036408 0.798052 0.275154 11.00000 0.07187 H34 2 0.019296 1.050166 0.143089 11.00000 0.06496 H35 2 0.035605 1.020424 0.072281 11.00000 0.06341 H36 2 0.012596 0.916857 0.102386 11.00000 0.06368 H37 2 0.090345 0.377068 0.086481 11.00000 0.06613 H38 2 0.064272 0.445192 0.018176 11.00000 0.07656 H39 2 0.053291 0.340909 0.072311 11.00000 0.06420 H40 2 0.008158 0.639640 0.059461 11.00000 0.07902 H41 2 0.006792 0.659363 0.147013 11.00000 0.05801 H42 2 0.001438 0.520843 0.116059 11.00000 0.08407 H43 2 0.081397 0.430488 0.268222 11.00000 0.06289 H44 2 0.054396 0.534506 0.285765 11.00000 0.06030 H45 2 0.044230 0.401567 0.241573 11.00000 0.07342 H46 2 0.115903 0.995064 0.019297 11.00000 0.09929 H47 2 0.078415 1.024407 -0.007159 11.00000 0.07921 H48 2 0.099988 0.986532 -0.069394 11.00000 0.08168 H49 2 0.140150 0.707447 -0.029800 11.00000 0.06264 H50 2 0.113458 0.712299 -0.112173 11.00000 0.07289 H51 2 0.111642 0.597197 -0.049164 11.00000 0.05999 H52 2 0.043385 0.782429 -0.119893 11.00000 0.06564 H53 2 0.039491 0.659967 -0.063313 11.00000 0.04739 H54 2 0.026921 0.800529 -0.043773 11.00000 0.05901 HKLF 4 REM sh3854 in C2/c REM wR2 = 0.091979, GooF = S = 1.01824, Restrained GooF = 1.01824 for all data REM R1 = 0.032924 for 9781 Fo > 4sig(Fo) and 0.050508 for all 12649 data REM 514 parameters refined using 0 restraints END WGHT 0.0450 2.0257 REM Highest difference peak 0.415, deepest hole -0.245, 1-sigma level 0.047 Q1 1 0.1907 0.5340 0.2837 11.00000 0.05 0.42 Q2 1 0.2177 0.6966 0.2674 11.00000 0.05 0.40 Q3 1 0.1809 0.9421 0.3622 11.00000 0.05 0.38 Q4 1 0.1828 0.5825 0.2160 11.00000 0.05 0.37 Q5 1 0.2032 0.6677 0.2081 11.00000 0.05 0.37 ; _shelx_res_checksum 68497 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 Si1 Si 0.15273(2) 0.78998(2) 0.17427(2) 0.01822(5) Uani 1 1 d . . . . . Si2 Si 0.09385(2) 0.73673(3) 0.13649(2) 0.01898(5) Uani 1 1 d . . . . . Si3 Si 0.06686(2) 0.92016(3) 0.18914(2) 0.02669(6) Uani 1 1 d . . . . . Si4 Si 0.05858(2) 0.54793(3) 0.14380(2) 0.02845(7) Uani 1 1 d . . . . . Si5 Si 0.08666(2) 0.78695(3) -0.00382(2) 0.02634(6) Uani 1 1 d . . . . . N1 N 0.14923(2) 0.77558(8) 0.35637(5) 0.02117(14) Uani 1 1 d . . . . . N2 N 0.17772(2) 0.94155(8) 0.32239(5) 0.02220(15) Uani 1 1 d . . . . . C1 C 0.18541(2) 0.63180(9) 0.18602(5) 0.02030(16) Uani 1 1 d . . . . . C2 C 0.21727(2) 0.69936(10) 0.22359(6) 0.02283(17) Uani 1 1 d . . . . . C3 C 0.22568(2) 0.65782(10) 0.30189(6) 0.02424(18) Uani 1 1 d . . . . . C4 C 0.20221(2) 0.55384(10) 0.31796(6) 0.02327(17) Uani 1 1 d . . . . . C5 C 0.17937(2) 0.53320(9) 0.24897(6) 0.02177(17) Uani 1 1 d . . . . . C6 C 0.18525(3) 0.57344(12) 0.10113(6) 0.0309(2) Uani 1 1 d . . . . . C7 C 0.23592(3) 0.79342(12) 0.17749(8) 0.0332(2) Uani 1 1 d . . . . . C8 C 0.25418(3) 0.70709(15) 0.36446(8) 0.0400(3) Uani 1 1 d . . . . . C9 C 0.20413(3) 0.48624(14) 0.39906(7) 0.0342(2) Uani 1 1 d . . . . . C10 C 0.15350(3) 0.42503(11) 0.23247(8) 0.0320(2) Uani 1 1 d . . . . . C11 C 0.15867(2) 0.83529(9) 0.29068(5) 0.01931(15) Uani 1 1 d . . . . . C12 C 0.16287(3) 0.84088(10) 0.42802(6) 0.02566(18) Uani 1 1 d . . . . . C13 C 0.18063(3) 0.94617(10) 0.40652(6) 0.02650(19) Uani 1 1 d . . . . . C14 C 0.12710(3) 0.66004(11) 0.35413(7) 0.02703(19) Uani 1 1 d . . . . . C15 C 0.15796(4) 0.79165(13) 0.50976(7) 0.0374(3) Uani 1 1 d . . . . . C16 C 0.20003(4) 1.05280(14) 0.45703(8) 0.0424(3) Uani 1 1 d . . . . . C17 C 0.19372(3) 1.03905(12) 0.27608(7) 0.0337(2) Uani 1 1 d . . . . . C18 C 0.09535(4) 1.06895(13) 0.21475(11) 0.0452(3) Uani 1 1 d . . . . . C19 C 0.05105(4) 0.87139(16) 0.28472(8) 0.0415(3) Uani 1 1 d . . . . . C20 C 0.02923(3) 0.98239(16) 0.11667(9) 0.0422(3) Uani 1 1 d . . . . . C21 C 0.06798(4) 0.41245(14) 0.07210(10) 0.0460(3) Uani 1 1 d . . . . . C22 C 0.01346(3) 0.59816(15) 0.11196(10) 0.0428(3) Uani 1 1 d . . . . . C23 C 0.06036(4) 0.46899(15) 0.24703(9) 0.0430(3) Uani 1 1 d . . . . . C24 C 0.09685(4) 0.96828(16) -0.01722(9) 0.0479(3) Uani 1 1 d . . . . . C25 C 0.11666(4) 0.6894(2) -0.05568(8) 0.0530(4) Uani 1 1 d . . . . . C26 C 0.04369(3) 0.75411(15) -0.06339(8) 0.0400(3) Uani 1 1 d . . . . . H1 H 0.1897(4) 0.6425(15) 0.0616(9) 0.044(4) Uiso 1 1 d . . . . . H2 H 0.1638(4) 0.5299(15) 0.0785(9) 0.042(4) Uiso 1 1 d . . . . . H3 H 0.2025(4) 0.5025(15) 0.1028(9) 0.041(4) Uiso 1 1 d . . . . . H4 H 0.2216(4) 0.8624(15) 0.1511(9) 0.046(4) Uiso 1 1 d . . . . . H5 H 0.2448(4) 0.7429(16) 0.1342(11) 0.054(5) Uiso 1 1 d . . . . . H6 H 0.2545(4) 0.8355(16) 0.2092(9) 0.051(4) Uiso 1 1 d . . . . . H7 H 0.2676(5) 0.7717(18) 0.3421(11) 0.064(5) Uiso 1 1 d . . . . . H8 H 0.2680(5) 0.6314(19) 0.3891(11) 0.068(5) Uiso 1 1 d . . . . . H9 H 0.2458(4) 0.7450(18) 0.4086(11) 0.062(5) Uiso 1 1 d . . . . . H10 H 0.2016(4) 0.5474(17) 0.4409(11) 0.056(5) Uiso 1 1 d . . . . . H11 H 0.1876(4) 0.4194(16) 0.4002(10) 0.051(4) Uiso 1 1 d . . . . . H12 H 0.2252(4) 0.4416(14) 0.4175(9) 0.041(4) Uiso 1 1 d . . . . . H13 H 0.1324(4) 0.4590(15) 0.2045(9) 0.044(4) Uiso 1 1 d . . . . . H14 H 0.1602(4) 0.3544(16) 0.1963(9) 0.048(4) Uiso 1 1 d . . . . . H15 H 0.1489(4) 0.3800(16) 0.2809(10) 0.052(4) Uiso 1 1 d . . . . . H16 H 0.1081(4) 0.6810(15) 0.3796(9) 0.043(4) Uiso 1 1 d . . . . . H17 H 0.1385(4) 0.5856(15) 0.3821(9) 0.043(4) Uiso 1 1 d . . . . . H18 H 0.1186(4) 0.6387(15) 0.2996(9) 0.041(4) Uiso 1 1 d . . . . . H19 H 0.1348(4) 0.7777(15) 0.5100(9) 0.044(4) Uiso 1 1 d . . . . . H20 H 0.1651(4) 0.8592(16) 0.5496(10) 0.049(4) Uiso 1 1 d . . . . . H21 H 0.1704(4) 0.7105(17) 0.5239(10) 0.055(5) Uiso 1 1 d . . . . . H22 H 0.2233(5) 1.0463(18) 0.4573(11) 0.067(5) Uiso 1 1 d . . . . . H23 H 0.1955(4) 1.0472(18) 0.5121(12) 0.064(5) Uiso 1 1 d . . . . . H24 H 0.1932(4) 1.1396(19) 0.4350(11) 0.062(5) Uiso 1 1 d . . . . . H25 H 0.2181(4) 1.0306(15) 0.2905(9) 0.046(4) Uiso 1 1 d . . . . . H26 H 0.1868(4) 1.1291(16) 0.2904(9) 0.050(4) Uiso 1 1 d . . . . . H27 H 0.1860(4) 1.0213(15) 0.2173(9) 0.045(4) Uiso 1 1 d . . . . . H28 H 0.0817(5) 1.145(2) 0.2271(12) 0.079(6) Uiso 1 1 d . . . . . H29 H 0.1059(5) 1.0933(19) 0.1743(12) 0.068(6) Uiso 1 1 d . . . . . H30 H 0.1121(5) 1.0507(17) 0.2602(11) 0.062(5) Uiso 1 1 d . . . . . H31 H 0.0393(4) 0.9461(18) 0.3039(10) 0.060(5) Uiso 1 1 d . . . . . H32 H 0.0682(5) 0.8457(19) 0.3277(11) 0.066(5) Uiso 1 1 d . . . . . H33 H 0.0364(5) 0.798(2) 0.2752(12) 0.072(6) Uiso 1 1 d . . . . . H34 H 0.0193(4) 1.0502(19) 0.1431(11) 0.065(5) Uiso 1 1 d . . . . . H35 H 0.0356(5) 1.0204(18) 0.0723(11) 0.063(5) Uiso 1 1 d . . . . . H36 H 0.0126(5) 0.9169(18) 0.1024(11) 0.064(5) Uiso 1 1 d . . . . . H37 H 0.0903(5) 0.3771(18) 0.0865(11) 0.066(5) Uiso 1 1 d . . . . . H38 H 0.0643(5) 0.445(2) 0.0182(13) 0.077(6) Uiso 1 1 d . . . . . H39 H 0.0533(5) 0.3409(19) 0.0723(11) 0.064(5) Uiso 1 1 d . . . . . H40 H 0.0082(5) 0.640(2) 0.0595(13) 0.079(6) Uiso 1 1 d . . . . . H41 H 0.0068(4) 0.6594(18) 0.1470(11) 0.058(5) Uiso 1 1 d . . . . . H42 H 0.0014(5) 0.521(2) 0.1161(13) 0.084(6) Uiso 1 1 d . . . . . H43 H 0.0814(5) 0.4305(17) 0.2682(11) 0.063(5) Uiso 1 1 d . . . . . H44 H 0.0544(4) 0.5345(18) 0.2858(11) 0.060(5) Uiso 1 1 d . . . . . H45 H 0.0442(5) 0.402(2) 0.2416(11) 0.073(6) Uiso 1 1 d . . . . . H46 H 0.1159(6) 0.995(2) 0.0193(15) 0.099(7) Uiso 1 1 d . . . . . H47 H 0.0784(5) 1.024(2) -0.0072(12) 0.079(6) Uiso 1 1 d . . . . . H48 H 0.1000(5) 0.987(2) -0.0694(13) 0.082(6) Uiso 1 1 d . . . . . H49 H 0.1401(5) 0.7074(17) -0.0298(11) 0.063(5) Uiso 1 1 d . . . . . H50 H 0.1135(5) 0.7123(19) -0.1122(13) 0.073(6) Uiso 1 1 d . . . . . H51 H 0.1116(4) 0.5972(19) -0.0492(11) 0.060(5) Uiso 1 1 d . . . . . H52 H 0.0434(4) 0.7824(18) -0.1199(12) 0.066(5) Uiso 1 1 d . . . . . H53 H 0.0395(4) 0.6600(17) -0.0633(9) 0.047(4) Uiso 1 1 d . . . . . H54 H 0.0269(4) 0.8005(17) -0.0438(11) 0.059(5) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.01720(11) 0.02041(11) 0.01657(10) 0.00078(8) 0.00129(8) -0.00030(8) Si2 0.01647(10) 0.02058(11) 0.01927(11) -0.00127(9) 0.00109(8) -0.00031(8) Si3 0.02209(12) 0.02725(13) 0.03030(14) -0.00439(11) 0.00304(10) 0.00472(10) Si4 0.02322(13) 0.02535(13) 0.03532(15) -0.00015(11) 0.00042(11) -0.00566(10) Si5 0.02335(13) 0.03500(15) 0.01928(12) -0.00085(10) -0.00065(9) 0.00223(10) N1 0.0220(3) 0.0220(3) 0.0198(3) 0.0009(3) 0.0041(3) 0.0023(3) N2 0.0220(4) 0.0231(4) 0.0206(3) -0.0019(3) 0.0006(3) -0.0012(3) C1 0.0198(4) 0.0239(4) 0.0173(4) 0.0011(3) 0.0031(3) 0.0025(3) C2 0.0171(4) 0.0268(4) 0.0250(4) 0.0024(3) 0.0045(3) 0.0019(3) C3 0.0191(4) 0.0300(5) 0.0225(4) -0.0008(3) 0.0000(3) 0.0043(3) C4 0.0234(4) 0.0270(4) 0.0199(4) 0.0040(3) 0.0053(3) 0.0073(3) C5 0.0223(4) 0.0208(4) 0.0230(4) 0.0022(3) 0.0059(3) 0.0032(3) C6 0.0374(6) 0.0343(5) 0.0208(4) -0.0030(4) 0.0046(4) 0.0084(4) C7 0.0237(5) 0.0368(6) 0.0407(6) 0.0097(5) 0.0096(4) -0.0006(4) C8 0.0287(5) 0.0514(7) 0.0352(6) -0.0032(5) -0.0087(5) 0.0002(5) C9 0.0366(6) 0.0441(6) 0.0234(5) 0.0112(4) 0.0092(4) 0.0145(5) C10 0.0324(5) 0.0241(5) 0.0399(6) 0.0014(4) 0.0067(5) -0.0027(4) C11 0.0177(4) 0.0205(4) 0.0194(4) -0.0001(3) 0.0021(3) 0.0009(3) C12 0.0294(5) 0.0290(5) 0.0181(4) -0.0008(3) 0.0028(3) 0.0079(4) C13 0.0289(5) 0.0284(5) 0.0202(4) -0.0043(3) -0.0018(3) 0.0040(4) C14 0.0266(5) 0.0267(5) 0.0292(5) 0.0040(4) 0.0089(4) -0.0020(4) C15 0.0511(7) 0.0403(6) 0.0213(5) 0.0042(4) 0.0075(5) 0.0122(5) C16 0.0529(8) 0.0393(6) 0.0306(6) -0.0112(5) -0.0063(5) -0.0060(6) C17 0.0378(6) 0.0314(5) 0.0318(5) -0.0026(4) 0.0056(4) -0.0142(4) C18 0.0399(7) 0.0276(5) 0.0664(9) -0.0116(6) 0.0039(7) 0.0020(5) C19 0.0397(6) 0.0530(8) 0.0339(6) -0.0080(5) 0.0122(5) 0.0088(6) C20 0.0322(6) 0.0489(7) 0.0441(7) 0.0010(6) 0.0016(5) 0.0163(5) C21 0.0491(8) 0.0313(6) 0.0537(8) -0.0116(6) -0.0035(6) -0.0023(6) C22 0.0237(5) 0.0462(7) 0.0559(8) 0.0007(6) -0.0010(5) -0.0084(5) C23 0.0372(6) 0.0424(7) 0.0489(7) 0.0129(6) 0.0062(6) -0.0112(5) C24 0.0536(8) 0.0511(8) 0.0372(7) 0.0150(6) 0.0017(6) -0.0145(7) C25 0.0470(8) 0.0872(12) 0.0247(6) -0.0072(6) 0.0051(5) 0.0243(8) C26 0.0330(6) 0.0493(7) 0.0327(6) -0.0023(5) -0.0096(5) 0.0020(5) 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 _geom_angle_publ_flag C11 Si1 C1 96.32(4) . . ? C11 Si1 Si2 105.27(3) . . ? C1 Si1 Si2 116.53(3) . . ? Si5 Si2 Si3 102.29(2) . . ? Si5 Si2 Si4 103.953(19) . . ? Si3 Si2 Si4 106.11(3) . . ? Si5 Si2 Si1 99.65(2) . . ? Si3 Si2 Si1 103.06(2) . . ? Si4 Si2 Si1 137.144(16) . . ? C19 Si3 C18 107.00(8) . . ? C19 Si3 C20 106.19(7) . . ? C18 Si3 C20 106.49(7) . . ? C19 Si3 Si2 110.79(5) . . ? C18 Si3 Si2 113.06(5) . . ? C20 Si3 Si2 112.87(5) . . ? C22 Si4 C23 105.06(7) . . ? C22 Si4 C21 107.38(7) . . ? C23 Si4 C21 107.31(8) . . ? C22 Si4 Si2 109.59(5) . . ? C23 Si4 Si2 116.41(5) . . ? C21 Si4 Si2 110.61(6) . . ? C25 Si5 C24 105.99(9) . . ? C25 Si5 C26 106.05(7) . . ? C24 Si5 C26 107.84(7) . . ? C25 Si5 Si2 111.25(5) . . ? C24 Si5 Si2 109.17(5) . . ? C26 Si5 Si2 116.03(5) . . ? C11 N1 C12 111.27(8) . . ? C11 N1 C14 125.48(8) . . ? C12 N1 C14 123.24(8) . . ? C11 N2 C13 111.47(8) . . ? C11 N2 C17 125.78(8) . . ? C13 N2 C17 122.74(8) . . ? C5 C1 C2 103.41(8) . . ? C5 C1 C6 115.10(9) . . ? C2 C1 C6 115.59(8) . . ? C5 C1 Si1 113.61(6) . . ? C2 C1 Si1 100.91(6) . . ? C6 C1 Si1 107.47(6) . . ? C3 C2 C7 128.19(9) . . ? C3 C2 C1 109.10(8) . . ? C7 C2 C1 122.68(9) . . ? C2 C3 C4 108.99(8) . . ? C2 C3 C8 127.52(10) . . ? C4 C3 C8 123.49(10) . . ? C5 C4 C3 108.78(8) . . ? C5 C4 C9 128.19(10) . . ? C3 C4 C9 123.03(9) . . ? C4 C5 C1 109.13(8) . . ? C4 C5 C10 128.19(9) . . ? C1 C5 C10 122.53(9) . . ? C1 C6 H1 112.1(9) . . ? C1 C6 H2 113.0(9) . . ? H1 C6 H2 107.3(12) . . ? C1 C6 H3 110.4(8) . . ? H1 C6 H3 108.2(12) . . ? H2 C6 H3 105.6(12) . . ? C2 C7 H4 111.6(9) . . ? C2 C7 H5 109.1(10) . . ? H4 C7 H5 107.1(13) . . ? C2 C7 H6 114.4(10) . . ? H4 C7 H6 107.7(13) . . ? H5 C7 H6 106.5(13) . . ? C3 C8 H7 111.6(11) . . ? C3 C8 H8 110.8(11) . . ? H7 C8 H8 111.1(14) . . ? C3 C8 H9 110.0(11) . . ? H7 C8 H9 109.4(15) . . ? H8 C8 H9 103.6(14) . . ? C4 C9 H10 112.2(10) . . ? C4 C9 H11 113.7(10) . . ? H10 C9 H11 106.3(14) . . ? C4 C9 H12 114.1(9) . . ? H10 C9 H12 105.0(13) . . ? H11 C9 H12 104.9(13) . . ? C5 C10 H13 111.8(9) . . ? C5 C10 H14 111.8(9) . . ? H13 C10 H14 105.3(12) . . ? C5 C10 H15 113.9(9) . . ? H13 C10 H15 107.0(13) . . ? H14 C10 H15 106.5(13) . . ? N1 C11 N2 104.15(8) . . ? N1 C11 Si1 133.66(7) . . ? N2 C11 Si1 122.02(7) . . ? C13 C12 N1 106.80(8) . . ? C13 C12 C15 130.77(10) . . ? N1 C12 C15 122.40(10) . . ? C12 C13 N2 106.29(8) . . ? C12 C13 C16 130.89(10) . . ? N2 C13 C16 122.81(10) . . ? N1 C14 H16 110.4(9) . . ? N1 C14 H17 111.1(9) . . ? H16 C14 H17 108.1(13) . . ? N1 C14 H18 109.3(9) . . ? H16 C14 H18 106.5(12) . . ? H17 C14 H18 111.5(12) . . ? C12 C15 H19 109.4(9) . . ? C12 C15 H20 109.3(10) . . ? H19 C15 H20 106.7(13) . . ? C12 C15 H21 111.1(10) . . ? H19 C15 H21 110.5(13) . . ? H20 C15 H21 109.8(13) . . ? C13 C16 H22 112.6(11) . . ? C13 C16 H23 109.3(11) . . ? H22 C16 H23 109.5(15) . . ? C13 C16 H24 109.5(10) . . ? H22 C16 H24 106.7(15) . . ? H23 C16 H24 109.1(15) . . ? N2 C17 H25 109.2(9) . . ? N2 C17 H26 108.3(9) . . ? H25 C17 H26 109.5(12) . . ? N2 C17 H27 108.0(9) . . ? H25 C17 H27 111.5(13) . . ? H26 C17 H27 110.3(12) . . ? Si3 C18 H28 108.2(12) . . ? Si3 C18 H29 113.3(12) . . ? H28 C18 H29 107.7(16) . . ? Si3 C18 H30 111.1(11) . . ? H28 C18 H30 109.6(15) . . ? H29 C18 H30 106.8(16) . . ? Si3 C19 H31 109.6(10) . . ? Si3 C19 H32 113.8(11) . . ? H31 C19 H32 107.3(15) . . ? Si3 C19 H33 110.5(12) . . ? H31 C19 H33 109.1(15) . . ? H32 C19 H33 106.3(16) . . ? Si3 C20 H34 107.5(11) . . ? Si3 C20 H35 110.7(11) . . ? H34 C20 H35 106.5(16) . . ? Si3 C20 H36 113.6(11) . . ? H34 C20 H36 106.2(15) . . ? H35 C20 H36 111.8(16) . . ? Si4 C21 H37 112.5(11) . . ? Si4 C21 H38 109.7(12) . . ? H37 C21 H38 111.1(16) . . ? Si4 C21 H39 110.8(11) . . ? H37 C21 H39 106.9(15) . . ? H38 C21 H39 105.5(15) . . ? Si4 C22 H40 115.7(12) . . ? Si4 C22 H41 111.7(11) . . ? H40 C22 H41 104.4(16) . . ? Si4 C22 H42 104.7(13) . . ? H40 C22 H42 112.8(17) . . ? H41 C22 H42 107.4(17) . . ? Si4 C23 H43 114.1(11) . . ? Si4 C23 H44 110.3(10) . . ? H43 C23 H44 109.2(14) . . ? Si4 C23 H45 107.0(12) . . ? H43 C23 H45 108.3(15) . . ? H44 C23 H45 107.7(15) . . ? Si5 C24 H46 111.7(15) . . ? Si5 C24 H47 110.3(12) . . ? H46 C24 H47 107.2(19) . . ? Si5 C24 H48 111.8(13) . . ? H46 C24 H48 109.4(19) . . ? H47 C24 H48 106.2(17) . . ? Si5 C25 H49 110.5(10) . . ? Si5 C25 H50 109.7(12) . . ? H49 C25 H50 110.5(16) . . ? Si5 C25 H51 106.5(11) . . ? H49 C25 H51 109.4(15) . . ? H50 C25 H51 110.2(15) . . ? Si5 C26 H52 108.8(11) . . ? Si5 C26 H53 108.6(9) . . ? H52 C26 H53 108.1(14) . . ? Si5 C26 H54 113.1(11) . . ? H52 C26 H54 107.5(15) . . ? H53 C26 H54 110.6(14) . . ? 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 Si1 C11 1.9673(11) . ? Si1 C1 2.0455(10) . ? Si1 Si2 2.4163(8) . ? Si2 Si5 2.3613(8) . ? Si2 Si3 2.3701(6) . ? Si2 Si4 2.3762(7) . ? Si3 C19 1.8737(15) . ? Si3 C18 1.8834(14) . ? Si3 C20 1.8846(14) . ? Si4 C22 1.8802(14) . ? Si4 C23 1.8818(15) . ? Si4 C21 1.8829(15) . ? Si5 C25 1.8710(15) . ? Si5 C24 1.8766(16) . ? Si5 C26 1.8810(13) . ? N1 C11 1.3541(12) . ? N1 C12 1.3919(13) . ? N1 C14 1.4549(13) . ? N2 C11 1.3643(12) . ? N2 C13 1.3877(13) . ? N2 C17 1.4564(14) . ? C1 C5 1.4865(13) . ? C1 C2 1.4957(13) . ? C1 C6 1.5283(14) . ? C2 C3 1.3576(14) . ? C2 C7 1.4920(15) . ? C3 C4 1.4589(15) . ? C3 C8 1.5035(15) . ? C4 C5 1.3662(14) . ? C4 C9 1.5004(14) . ? C5 C10 1.4958(15) . ? C6 H1 0.990(15) . ? C6 H2 0.988(15) . ? C6 H3 0.991(15) . ? C7 H4 0.959(16) . ? C7 H5 0.995(18) . ? C7 H6 0.942(16) . ? C8 H7 0.955(19) . ? C8 H8 0.989(19) . ? C8 H9 0.938(19) . ? C9 H10 0.944(18) . ? C9 H11 0.947(17) . ? C9 H12 0.963(15) . ? C10 H13 0.962(15) . ? C10 H14 0.993(16) . ? C10 H15 0.967(17) . ? C12 C13 1.3526(16) . ? C12 C15 1.4907(15) . ? C13 C16 1.4958(16) . ? C14 H16 0.956(15) . ? C14 H17 0.954(15) . ? C14 H18 0.941(14) . ? C15 H19 0.946(16) . ? C15 H20 0.957(16) . ? C15 H21 0.961(17) . ? C16 H22 0.94(2) . ? C16 H23 0.966(19) . ? C16 H24 0.963(18) . ? C17 H25 0.978(16) . ? C17 H26 0.982(16) . ? C17 H27 0.994(15) . ? C18 H28 0.98(2) . ? C18 H29 0.89(2) . ? C18 H30 0.947(19) . ? C19 H31 0.966(18) . ? C19 H32 0.947(19) . ? C19 H33 0.94(2) . ? C20 H34 0.932(19) . ? C20 H35 0.905(19) . ? C20 H36 0.939(19) . ? C21 H37 0.962(19) . ? C21 H38 0.94(2) . ? C21 H39 0.928(19) . ? C22 H40 0.96(2) . ? C22 H41 0.915(19) . ? C22 H42 0.92(2) . ? C23 H43 0.946(19) . ? C23 H44 0.976(19) . ? C23 H45 0.93(2) . ? C24 H46 0.94(2) . ? C24 H47 0.97(2) . ? C24 H48 0.92(2) . ? C25 H49 0.992(18) . ? C25 H50 0.96(2) . ? C25 H51 0.952(18) . ? C26 H52 0.981(19) . ? C26 H53 0.954(17) . ? C26 H54 0.923(18) . ?