#------------------------------------------------------------------------------ #$Date: 2019-10-13 02:55:41 +0300 (Sun, 13 Oct 2019) $ #$Revision: 219314 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/43/7124303.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_7124303 loop_ _publ_author_name 'Dong, Yafang' 'Takata, Yuta' 'Yoshigoe, Yusuke' 'Sekine, Kohei' 'Kuninobu, Yoichiro' _publ_section_title ; Lewis Acid-Catalyzed Synthesis of Silafluorene Derivatives from Biphenyls and Dihydrosilanes via Double Sila-Friedel-Crafts Reaction ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC07692A _journal_year 2019 _chemical_formula_moiety 'C28 H28 N2 Si' _chemical_formula_sum 'C28 H28 N2 Si' _chemical_formula_weight 420.61 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2018-11-16 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-08-29 deposited with the CCDC. 2019-10-11 downloaded from the CCDC. ; _cell_angle_alpha 113.798(3) _cell_angle_beta 91.992(4) _cell_angle_gamma 112.004(4) _cell_formula_units_Z 2 _cell_length_a 9.4768(4) _cell_length_b 10.9099(4) _cell_length_c 13.1313(5) _cell_measurement_reflns_used 10732 _cell_measurement_temperature 123 _cell_measurement_theta_max 30.9290 _cell_measurement_theta_min 2.3570 _cell_volume 1123.73(9) _computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 123 _diffrn_detector 'Rigaku HyPix-6000 area detector' _diffrn_detector_area_resol_mean 10.0 _diffrn_detector_type 'HPC area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.847 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 28.00 54.00 0.50 0.50 -- 5.00 45.00 60.00 52 2 \w -72.00 -46.00 0.50 0.50 -- 5.00 45.00 60.00 52 3 \w -27.00 -1.00 0.50 0.50 -- 5.00 45.00 120.00 52 4 \w -98.00 -46.00 0.50 0.50 -- -10.00 45.00 150.00 104 5 \w -43.00 79.00 0.50 0.50 -- -10.00 45.00 150.00 244 6 \w -98.00 79.00 0.50 0.50 -- -10.00 45.00 90.00 354 7 \w -61.00 50.00 0.50 0.50 -- -10.00 45.00 0.00 222 ; _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Rigaku AFC HyPix-6000' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0043009000 _diffrn_orient_matrix_UB_12 0.0631982000 _diffrn_orient_matrix_UB_13 0.0482525000 _diffrn_orient_matrix_UB_21 -0.0305547000 _diffrn_orient_matrix_UB_22 -0.0441319000 _diffrn_orient_matrix_UB_23 0.0284283000 _diffrn_orient_matrix_UB_31 0.0767688000 _diffrn_orient_matrix_UB_32 0.0148571000 _diffrn_orient_matrix_UB_33 0.0229042000 _diffrn_radiation_monochromator 'multi-layer mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_unetI/netI 0.0328 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.847 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 19804 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.847 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.026 _diffrn_reflns_theta_min 2.376 _diffrn_source 'rotating anode X-ray generator' _diffrn_source_type FR-E+ _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.547 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.243 _exptl_crystal_description plate _exptl_crystal_F_000 448 _exptl_crystal_size_max 0.359 _exptl_crystal_size_mid 0.274 _exptl_crystal_size_min 0.133 _refine_diff_density_max 0.340 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 284 _refine_ls_number_reflns 6081 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.085 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0402 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.3420P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1060 _refine_ls_wR_factor_ref 0.1100 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5254 _reflns_number_total 6081 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc07692a2.cif _cod_data_source_block 181116 _cod_original_cell_volume 1123.73(8) _cod_database_code 7124303 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C11 H10 N O' _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. ; _reflns_odcompleteness_completeness 99.79 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.42 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C8AA(H8AA), C0BA(H0BA), C1BA(H1BA), C2BA(H2BA), C4BA(H4BA), C5BA(H5BA), C6BA(H6BA), C7BA(H7BA), C8BA(H8BA), C9BA(H9BA), C0CA(H0CA), C1CA(H1CA), C3CA(H3CA), C5CA(H5CA), C6CA(H6CA), C7CA(H7CA) 2.b Idealised Me refined as rotating group: C(HA,HB,HC), C2CA(H2CA,H2CB,H2CC), C4CA(H4CA,H4CB,H4CC), C8CA(H8CA,H8CB,H8CC) ; _shelx_res_file ; TITL 181116.res created by SHELXL-2018/3 at 16:13:35 on 16-Nov-2018 CELL 0.71073 9.4768 10.9099 13.1313 113.798 91.992 112.004 ZERR 2 0.0004 0.0004 0.0005 0.003 0.004 0.004 LATT 1 SFAC C H N Si UNIT 56 56 4 2 L.S. 10 PLAN 20 fmap 2 ACTA REM REM REM WGHT 0.049200 0.342000 FVAR 6.64151 SI0A 4 0.248467 0.875408 0.254813 11.00000 0.01606 0.01655 = 0.01644 0.00701 0.00291 0.00663 C1AA 1 0.113667 0.815134 0.121045 11.00000 0.01869 0.01734 = 0.01780 0.00702 0.00423 0.00895 C2AA 1 -0.018776 0.685070 0.099700 11.00000 0.01946 0.01727 = 0.01687 0.00667 0.00448 0.01018 N 3 -0.230355 0.326679 0.260066 11.00000 0.03004 0.02357 = 0.02565 0.01439 0.00268 0.00325 C4AA 1 0.119676 0.713552 0.273654 11.00000 0.01893 0.01859 = 0.01859 0.00808 0.00483 0.00822 C5AA 1 0.271151 1.057582 0.369700 11.00000 0.02097 0.02025 = 0.01662 0.00811 0.00328 0.01006 N0AA 3 -0.272818 0.636626 -0.146372 11.00000 0.02826 0.02745 = 0.02190 0.01077 -0.00329 0.00933 C6AA 1 -0.014410 0.626740 0.184195 11.00000 0.01938 0.01759 = 0.01730 0.00750 0.00518 0.00928 C7AA 1 0.444905 0.879548 0.238479 11.00000 0.01790 0.01486 = 0.01997 0.00675 0.00314 0.00671 C8AA 1 0.423480 1.316944 0.499722 11.00000 0.03648 0.01942 = 0.02582 0.00707 0.00402 0.00820 AFIX 43 H8AA 2 0.519841 1.398442 0.532258 11.00000 -1.20000 AFIX 0 C9AA 1 -0.114010 0.450716 0.260994 11.00000 0.02479 0.01895 = 0.02019 0.00915 0.00728 0.00787 C0BA 1 0.550983 0.904659 0.329464 11.00000 0.02260 0.02238 = 0.02195 0.01081 0.00354 0.00992 AFIX 43 H0BA 2 0.525954 0.926435 0.400649 11.00000 -1.20000 AFIX 0 C1BA 1 -0.143423 0.622497 0.008592 11.00000 0.02086 0.01738 = 0.01998 0.00699 0.00247 0.00781 AFIX 43 H1BA 2 -0.228560 0.535383 -0.004946 11.00000 -1.20000 AFIX 0 C2BA 1 0.115775 0.876697 0.046139 11.00000 0.02313 0.01849 = 0.02264 0.00995 0.00518 0.00830 AFIX 43 H2BA 2 0.202971 0.961202 0.057457 11.00000 -1.20000 AFIX 0 C3BA 1 -0.142269 0.689435 -0.063375 11.00000 0.02528 0.02032 = 0.01656 0.00530 0.00138 0.01239 C4BA 1 0.135248 0.663621 0.353556 11.00000 0.02230 0.02400 = 0.01856 0.00935 0.00274 0.00855 AFIX 43 H4BA 2 0.223874 0.718153 0.412326 11.00000 -1.20000 AFIX 0 C 1 -0.260469 0.685425 -0.233927 11.00000 0.04206 0.03069 = 0.02345 0.01201 -0.00330 0.01624 AFIX 137 HA 2 -0.215799 0.791590 -0.199195 11.00000 -1.50000 HB 2 -0.362334 0.646262 -0.279943 11.00000 -1.50000 HC 2 -0.195045 0.650941 -0.280985 11.00000 -1.50000 AFIX 0 C5BA 1 -0.007629 0.816044 -0.044329 11.00000 0.03041 0.02158 = 0.02072 0.01168 0.00439 0.01280 AFIX 43 H5BA 2 -0.001643 0.859365 -0.093166 11.00000 -1.20000 AFIX 0 C6BA 1 -0.129215 0.498124 0.178039 11.00000 0.02123 0.01938 = 0.01891 0.00790 0.00276 0.00717 AFIX 43 H6BA 2 -0.217035 0.442708 0.118558 11.00000 -1.20000 AFIX 0 C7BA 1 0.147828 1.209091 0.483991 11.00000 0.03793 0.03995 = 0.03033 0.01243 0.01148 0.02778 AFIX 43 H7BA 2 0.058174 1.217751 0.505362 11.00000 -1.20000 AFIX 0 C8BA 1 0.413466 1.181781 0.419430 11.00000 0.02393 0.02118 = 0.02295 0.00905 0.00555 0.00900 AFIX 43 H8BA 2 0.503672 1.174111 0.398474 11.00000 -1.20000 AFIX 0 C9BA 1 0.486791 0.846815 0.133180 11.00000 0.02295 0.02968 = 0.01883 0.00688 0.00292 0.01194 AFIX 43 H9BA 2 0.418065 0.828692 0.071070 11.00000 -1.20000 AFIX 0 C0CA 1 0.022136 0.534869 0.347706 11.00000 0.02844 0.02457 = 0.01923 0.01250 0.00590 0.01041 AFIX 43 H0CA 2 0.036325 0.503529 0.401869 11.00000 -1.20000 AFIX 0 C1CA 1 0.290392 1.330548 0.531373 11.00000 0.05028 0.02554 = 0.02169 0.00636 0.00780 0.02318 AFIX 43 H1CA 2 0.296987 1.421368 0.584478 11.00000 -1.20000 AFIX 0 C2CA 1 -0.190932 0.255651 0.321288 11.00000 0.03627 0.03193 = 0.03597 0.02418 0.00418 0.00393 AFIX 137 H2CA 2 -0.099582 0.241484 0.301964 11.00000 -1.50000 H2CB 2 -0.276259 0.161423 0.300751 11.00000 -1.50000 H2CC 2 -0.170746 0.316823 0.401850 11.00000 -1.50000 AFIX 0 C3CA 1 0.692708 0.897724 0.315612 11.00000 0.02433 0.02875 = 0.03109 0.01084 -0.00081 0.01368 AFIX 43 H3CA 2 0.761415 0.914250 0.377020 11.00000 -1.20000 AFIX 0 C4CA 1 -0.366243 0.235999 0.168094 11.00000 0.03026 0.02619 = 0.03053 0.01572 0.00212 0.00167 AFIX 137 H4CA 2 -0.407760 0.297674 0.155227 11.00000 -1.50000 H4CB 2 -0.443561 0.167227 0.187598 11.00000 -1.50000 H4CC 2 -0.338107 0.182571 0.100068 11.00000 -1.50000 AFIX 0 C5CA 1 0.731717 0.866127 0.210102 11.00000 0.02283 0.03632 = 0.03625 0.00664 0.00595 0.01777 AFIX 43 H5CA 2 0.826964 0.862092 0.200747 11.00000 -1.20000 AFIX 0 C6CA 1 0.138463 1.074179 0.404505 11.00000 0.02263 0.02967 = 0.02678 0.00850 0.00348 0.01309 AFIX 43 H6CA 2 0.041951 0.992744 0.373515 11.00000 -1.20000 AFIX 0 C7CA 1 0.629143 0.840673 0.118992 11.00000 0.02841 0.04017 = 0.02506 0.00512 0.00941 0.01734 AFIX 43 H7CA 2 0.655143 0.819421 0.048132 11.00000 -1.20000 AFIX 0 C8CA 1 -0.403375 0.499269 -0.170154 11.00000 0.03292 0.02619 = 0.03334 0.01085 -0.01025 0.00591 AFIX 137 H8CA 2 -0.370771 0.420417 -0.196263 11.00000 -1.50000 H8CB 2 -0.485085 0.478920 -0.228089 11.00000 -1.50000 H8CC 2 -0.441170 0.507041 -0.101940 11.00000 -1.50000 AFIX 0 HKLF 4 REM REM wR2 = 0.1100, GooF = S = 1.085, Restrained GooF = 1.085 for all data REM R1 = 0.0402 for 5254 Fo > 4sig(Fo) and 0.0467 for all 6081 data REM 284 parameters refined using 0 restraints END WGHT 0.0489 0.3430 REM Highest difference peak 0.340, deepest hole -0.265, 1-sigma level 0.047 Q1 1 -0.0148 0.6599 0.1431 11.00000 0.05 0.34 Q2 1 -0.1376 0.6566 -0.0269 11.00000 0.05 0.34 Q3 1 0.1793 0.7832 0.2567 11.00000 0.05 0.33 Q4 1 -0.1188 0.4841 0.2247 11.00000 0.05 0.32 Q5 1 0.1790 0.8438 0.1771 11.00000 0.05 0.32 Q6 1 0.2686 0.9824 0.3178 11.00000 0.05 0.31 Q7 1 -0.0398 0.4826 0.2947 11.00000 0.05 0.31 Q8 1 -0.0746 0.7430 -0.0579 11.00000 0.05 0.30 Q9 1 0.3575 0.8846 0.2491 11.00000 0.05 0.30 Q10 1 0.3446 1.1164 0.4059 11.00000 0.05 0.29 Q11 1 -0.1993 0.6581 -0.1048 11.00000 0.05 0.28 Q12 1 0.5066 0.8979 0.2798 11.00000 0.05 0.28 Q13 1 0.4798 0.8762 0.1913 11.00000 0.05 0.28 Q14 1 0.0663 0.6579 0.2201 11.00000 0.05 0.27 Q15 1 -0.0763 0.6576 0.0562 11.00000 0.05 0.27 Q16 1 0.3464 1.3162 0.4885 11.00000 0.05 0.27 Q17 1 0.5643 0.8520 0.1323 11.00000 0.05 0.27 Q18 1 0.1064 0.8575 0.0932 11.00000 0.05 0.26 Q19 1 0.0428 0.8549 0.0158 11.00000 0.05 0.26 Q20 1 -0.0803 0.5741 0.1884 11.00000 0.05 0.24 ; _shelx_res_checksum 22506 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.073 _oxdiff_exptl_absorpt_empirical_full_min 0.904 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Si0A Si 0.24847(3) 0.87541(3) 0.25481(3) 0.01661(9) Uani 1 1 d . C1AA C 0.11367(13) 0.81513(12) 0.12104(9) 0.0178(2) Uani 1 1 d . C2AA C -0.01878(13) 0.68507(12) 0.09970(9) 0.0174(2) Uani 1 1 d . N N -0.23036(13) 0.32668(12) 0.26007(9) 0.0280(2) Uani 1 1 d . C4AA C 0.11968(13) 0.71355(12) 0.27365(10) 0.0187(2) Uani 1 1 d . C5AA C 0.27115(13) 1.05758(13) 0.36970(9) 0.0189(2) Uani 1 1 d . N0AA N -0.27282(13) 0.63663(12) -0.14637(9) 0.0271(2) Uani 1 1 d . C6AA C -0.01441(13) 0.62674(12) 0.18420(9) 0.0177(2) Uani 1 1 d . C7AA C 0.44490(13) 0.87955(12) 0.23848(10) 0.0181(2) Uani 1 1 d . C8AA C 0.42348(17) 1.31694(14) 0.49972(11) 0.0297(3) Uani 1 1 d . H8AA H 0.519841 1.398442 0.532258 0.036 Uiso 1 1 calc R C9AA C -0.11401(14) 0.45072(13) 0.26099(10) 0.0216(2) Uani 1 1 d . C0BA C 0.55098(14) 0.90466(13) 0.32946(10) 0.0219(2) Uani 1 1 d . H0BA H 0.525954 0.926435 0.400649 0.026 Uiso 1 1 calc R C1BA C -0.14342(14) 0.62250(12) 0.00859(10) 0.0201(2) Uani 1 1 d . H1BA H -0.228560 0.535383 -0.004946 0.024 Uiso 1 1 calc R C2BA C 0.11578(14) 0.87670(13) 0.04614(10) 0.0213(2) Uani 1 1 d . H2BA H 0.202971 0.961202 0.057457 0.026 Uiso 1 1 calc R C3BA C -0.14227(14) 0.68943(13) -0.06337(10) 0.0210(2) Uani 1 1 d . C4BA C 0.13525(14) 0.66362(13) 0.35356(10) 0.0222(2) Uani 1 1 d . H4BA H 0.223874 0.718153 0.412326 0.027 Uiso 1 1 calc R C C -0.26047(18) 0.68543(16) -0.23393(11) 0.0322(3) Uani 1 1 d . HA H -0.215799 0.791590 -0.199195 0.048 Uiso 1 1 calc GR HB H -0.362334 0.646262 -0.279943 0.048 Uiso 1 1 calc GR HC H -0.195045 0.650941 -0.280985 0.048 Uiso 1 1 calc GR C5BA C -0.00763(15) 0.81604(13) -0.04433(10) 0.0229(2) Uani 1 1 d . H5BA H -0.001643 0.859365 -0.093166 0.027 Uiso 1 1 calc R C6BA C -0.12922(14) 0.49812(13) 0.17804(10) 0.0206(2) Uani 1 1 d . H6BA H -0.217035 0.442708 0.118558 0.025 Uiso 1 1 calc R C7BA C 0.14783(17) 1.20909(16) 0.48399(12) 0.0334(3) Uani 1 1 d . H7BA H 0.058174 1.217751 0.505362 0.040 Uiso 1 1 calc R C8BA C 0.41347(14) 1.18178(13) 0.41943(10) 0.0232(2) Uani 1 1 d . H8BA H 0.503672 1.174111 0.398474 0.028 Uiso 1 1 calc R C9BA C 0.48679(14) 0.84682(14) 0.13318(10) 0.0251(3) Uani 1 1 d . H9BA H 0.418065 0.828692 0.071070 0.030 Uiso 1 1 calc R C0CA C 0.02214(15) 0.53487(14) 0.34771(10) 0.0234(2) Uani 1 1 d . H0CA H 0.036325 0.503529 0.401869 0.028 Uiso 1 1 calc R C1CA C 0.29039(18) 1.33055(15) 0.53137(11) 0.0317(3) Uani 1 1 d . H1CA H 0.296987 1.421368 0.584478 0.038 Uiso 1 1 calc R C2CA C -0.19093(17) 0.25565(16) 0.32129(13) 0.0351(3) Uani 1 1 d . H2CA H -0.099582 0.241484 0.301964 0.053 Uiso 1 1 calc GR H2CB H -0.276259 0.161423 0.300751 0.053 Uiso 1 1 calc GR H2CC H -0.170746 0.316823 0.401850 0.053 Uiso 1 1 calc GR C3CA C 0.69271(15) 0.89772(15) 0.31561(12) 0.0284(3) Uani 1 1 d . H3CA H 0.761415 0.914250 0.377020 0.034 Uiso 1 1 calc R C4CA C -0.36624(16) 0.23600(15) 0.16809(12) 0.0315(3) Uani 1 1 d . H4CA H -0.407760 0.297674 0.155227 0.047 Uiso 1 1 calc GR H4CB H -0.443561 0.167227 0.187598 0.047 Uiso 1 1 calc GR H4CC H -0.338107 0.182571 0.100068 0.047 Uiso 1 1 calc GR C5CA C 0.73172(16) 0.86613(16) 0.21010(12) 0.0336(3) Uani 1 1 d . H5CA H 0.826964 0.862092 0.200747 0.040 Uiso 1 1 calc R C6CA C 0.13846(15) 1.07418(15) 0.40450(11) 0.0273(3) Uani 1 1 d . H6CA H 0.041951 0.992744 0.373515 0.033 Uiso 1 1 calc R C7CA C 0.62914(16) 0.84067(17) 0.11899(12) 0.0337(3) Uani 1 1 d . H7CA H 0.655143 0.819421 0.048132 0.040 Uiso 1 1 calc R C8CA C -0.40337(17) 0.49927(15) -0.17015(13) 0.0345(3) Uani 1 1 d . H8CA H -0.370771 0.420417 -0.196263 0.052 Uiso 1 1 calc GR H8CB H -0.485085 0.478920 -0.228089 0.052 Uiso 1 1 calc GR H8CC H -0.441170 0.507041 -0.101940 0.052 Uiso 1 1 calc GR 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 Si0A 0.01606(15) 0.01655(15) 0.01644(15) 0.00701(12) 0.00291(11) 0.00663(12) C1AA 0.0187(5) 0.0173(5) 0.0178(5) 0.0070(4) 0.0042(4) 0.0089(4) C2AA 0.0195(5) 0.0173(5) 0.0169(5) 0.0067(4) 0.0045(4) 0.0102(4) N 0.0300(6) 0.0236(5) 0.0257(5) 0.0144(4) 0.0027(4) 0.0033(4) C4AA 0.0189(5) 0.0186(5) 0.0186(5) 0.0081(4) 0.0048(4) 0.0082(4) C5AA 0.0210(5) 0.0203(5) 0.0166(5) 0.0081(4) 0.0033(4) 0.0101(4) N0AA 0.0283(5) 0.0274(5) 0.0219(5) 0.0108(4) -0.0033(4) 0.0093(5) C6AA 0.0194(5) 0.0176(5) 0.0173(5) 0.0075(4) 0.0052(4) 0.0093(4) C7AA 0.0179(5) 0.0149(5) 0.0200(5) 0.0068(4) 0.0031(4) 0.0067(4) C8AA 0.0365(7) 0.0194(6) 0.0258(6) 0.0071(5) 0.0040(5) 0.0082(5) C9AA 0.0248(6) 0.0189(5) 0.0202(5) 0.0092(4) 0.0073(5) 0.0079(5) C0BA 0.0226(6) 0.0224(6) 0.0219(5) 0.0108(5) 0.0035(4) 0.0099(5) C1BA 0.0209(5) 0.0174(5) 0.0200(5) 0.0070(4) 0.0025(4) 0.0078(4) C2BA 0.0231(6) 0.0185(5) 0.0226(6) 0.0100(4) 0.0052(5) 0.0083(5) C3BA 0.0253(6) 0.0203(5) 0.0166(5) 0.0053(4) 0.0014(4) 0.0124(5) C4BA 0.0223(6) 0.0240(6) 0.0186(5) 0.0094(5) 0.0027(4) 0.0085(5) C 0.0421(8) 0.0307(7) 0.0234(6) 0.0120(5) -0.0033(6) 0.0162(6) C5BA 0.0304(6) 0.0216(6) 0.0207(5) 0.0117(5) 0.0044(5) 0.0128(5) C6BA 0.0212(5) 0.0194(5) 0.0189(5) 0.0079(4) 0.0028(4) 0.0072(5) C7BA 0.0379(7) 0.0400(8) 0.0303(7) 0.0124(6) 0.0115(6) 0.0278(7) C8BA 0.0239(6) 0.0212(6) 0.0230(6) 0.0090(5) 0.0055(5) 0.0090(5) C9BA 0.0230(6) 0.0297(6) 0.0188(5) 0.0069(5) 0.0029(5) 0.0119(5) C0CA 0.0284(6) 0.0246(6) 0.0192(5) 0.0125(5) 0.0059(5) 0.0104(5) C1CA 0.0503(8) 0.0255(6) 0.0217(6) 0.0064(5) 0.0078(6) 0.0232(6) C2CA 0.0363(7) 0.0319(7) 0.0360(7) 0.0242(6) 0.0042(6) 0.0039(6) C3CA 0.0243(6) 0.0287(6) 0.0311(7) 0.0108(5) -0.0008(5) 0.0137(5) C4CA 0.0303(7) 0.0262(6) 0.0305(7) 0.0157(5) 0.0021(5) 0.0017(5) C5CA 0.0228(6) 0.0363(7) 0.0362(7) 0.0066(6) 0.0059(5) 0.0178(6) C6CA 0.0226(6) 0.0297(6) 0.0268(6) 0.0085(5) 0.0035(5) 0.0131(5) C7CA 0.0284(7) 0.0402(8) 0.0251(6) 0.0051(6) 0.0094(5) 0.0173(6) C8CA 0.0329(7) 0.0262(7) 0.0333(7) 0.0108(6) -0.0102(6) 0.0059(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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 11 -4 9 0.1477 -13 5 -2 0.1468 5 -3 -15 0.1035 0 -13 14 0.0815 -12 4 -4 0.1715 0 13 -14 0.0499 -6 4 14 0.1127 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1AA Si0A C5AA 112.68(5) C1AA Si0A C7AA 115.18(5) C4AA Si0A C1AA 91.83(5) C4AA Si0A C5AA 113.97(5) C4AA Si0A C7AA 112.72(5) C7AA Si0A C5AA 109.63(5) C2AA C1AA Si0A 109.49(8) C2BA C1AA Si0A 132.95(9) C2BA C1AA C2AA 117.45(10) C1AA C2AA C6AA 114.59(10) C1BA C2AA C1AA 121.09(10) C1BA C2AA C6AA 124.28(10) C9AA N C2CA 118.79(11) C9AA N C4CA 120.18(11) C4CA N C2CA 116.47(11) C6AA C4AA Si0A 109.64(8) C4BA C4AA Si0A 132.42(9) C4BA C4AA C6AA 117.88(10) C8BA C5AA Si0A 123.28(9) C8BA C5AA C6CA 117.32(11) C6CA C5AA Si0A 119.32(9) C3BA N0AA C 119.94(11) C3BA N0AA C8CA 119.43(11) C N0AA C8CA 117.13(11) C4AA C6AA C2AA 114.39(10) C6BA C6AA C2AA 124.51(10) C6BA C6AA C4AA 121.09(10) C0BA C7AA Si0A 121.14(9) C9BA C7AA Si0A 121.21(9) C9BA C7AA C0BA 117.48(10) C1CA C8AA C8BA 120.11(12) N C9AA C6BA 121.68(11) N C9AA C0CA 120.13(11) C0CA C9AA C6BA 118.18(11) C3CA C0BA C7AA 121.34(11) C2AA C1BA C3BA 120.74(11) C5BA C2BA C1AA 122.01(11) N0AA C3BA C1BA 120.83(11) N0AA C3BA C5BA 121.15(11) C5BA C3BA C1BA 117.93(11) C0CA C4BA C4AA 121.51(11) C2BA C5BA C3BA 120.66(11) C6AA C6BA C9AA 120.49(11) C1CA C7BA C6CA 119.87(12) C8AA C8BA C5AA 121.32(12) C7CA C9BA C7AA 121.42(12) C4BA C0CA C9AA 120.80(11) C7BA C1CA C8AA 119.85(12) C5CA C3CA C0BA 119.88(12) C7CA C5CA C3CA 119.93(12) C7BA C6CA C5AA 121.52(12) C5CA C7CA C9BA 119.94(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Si0A C1AA 1.8526(12) Si0A C4AA 1.8514(12) Si0A C5AA 1.8735(12) Si0A C7AA 1.8671(12) C1AA C2AA 1.4098(16) C1AA C2BA 1.3941(16) C2AA C6AA 1.4913(15) C2AA C1BA 1.3896(16) N C9AA 1.3838(15) N C2CA 1.4440(17) N C4CA 1.4383(17) C4AA C6AA 1.4100(16) C4AA C4BA 1.3893(16) C5AA C8BA 1.3917(17) C5AA C6CA 1.4024(16) N0AA C3BA 1.3841(15) N0AA C 1.4407(17) N0AA C8CA 1.4423(17) C6AA C6BA 1.3848(16) C7AA C0BA 1.3997(16) C7AA C9BA 1.3939(16) C8AA C8BA 1.3887(17) C8AA C1CA 1.383(2) C9AA C6BA 1.4052(16) C9AA C0CA 1.4038(17) C0BA C3CA 1.3874(17) C1BA C3BA 1.4065(16) C2BA C5BA 1.3806(17) C3BA C5BA 1.4060(17) C4BA C0CA 1.3809(17) C7BA C1CA 1.379(2) C7BA C6CA 1.3855(18) C9BA C7CA 1.3908(18) C3CA C5CA 1.386(2) C5CA C7CA 1.379(2) loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 10.9195 -4.3013 8.7478 0.1972 0.1049 0.9747 -13.1114 5.4530 -2.4207 0.1714 0.0911 -0.9810 5.0649 -2.6831 -15.2357 -0.8829 -0.4695 0.0000 -0.1077 -13.2353 13.7677 -0.1726 0.9788 0.1104 -12.4416 4.0080 -4.4237 -0.0137 0.0775 -0.9969 -0.0164 13.2704 -13.8068 0.1724 -0.9777 -0.1203 -5.9858 4.0059 14.0128 0.9036 0.4045 -0.0791