#------------------------------------------------------------------------------ #$Date: 2024-07-09 01:14:14 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293302 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572074.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_1572074 loop_ _publ_author_name 'Wieprecht, Nele' 'Krummenacher, Ivo' 'W\"ust, Leonie' 'Michel, Maximilian' 'Fuchs, Sonja' 'Nees, Samuel' 'H\"arterich, Marcel' 'Braunschweig, Holger' _publ_section_title ; The forgotten borole: synthesis, properties and reactivity of a 1-boraindene ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03817G _journal_year 2024 _chemical_formula_moiety 'C55 H47 B2 N3 Si, C7 H8' _chemical_formula_sum 'C62 H55 B2 N3 Si' _chemical_formula_weight 891.80 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2023-02-28 _audit_creation_method 'CIF-fill 1.3q (K.Radacki, 2005-22)' _audit_update_record ; 2024-06-05 deposited with the CCDC. 2024-07-02 downloaded from the CCDC. ; _cell_angle_alpha 85.6500(10) _cell_angle_beta 86.819(2) _cell_angle_gamma 89.3620(10) _cell_formula_units_Z 2 _cell_length_a 9.9393(2) _cell_length_b 15.2431(2) _cell_length_c 16.3736(3) _cell_measurement_reflns_used 22431 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 74.5800 _cell_measurement_theta_min 5.2910 _cell_volume 2469.68(7) _computing_cell_refinement 'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector HPA _diffrn_detector_area_resol_mean 10.0 _diffrn_detector_type 'HyPix Arc150' _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): -------------------------------------------------------------------------- 1 \w 17.00 43.00 0.50 0.60 -- 59.14-115.00 -81.00 52 2 \w -60.00 -15.00 0.50 0.60 -- -60.12 115.00 6.00 90 3 \w -57.00 -32.00 0.50 0.60 -- -69.79 115.00 6.00 50 4 \w -94.00 -62.00 0.50 0.60 -- -76.38 115.00 6.00 64 5 \w 72.00 97.00 0.50 0.60 -- 82.25-115.00 -81.00 50 6 \w 44.00 69.00 0.50 0.60 -- 82.25-115.00 -81.00 50 7 \w -43.00 -18.00 0.50 0.60 -- -6.00 -62.00 154.46 50 8 \w -47.00 -22.00 0.50 0.60 -- -10.00 -61.00 69.73 50 9 \w -98.00 -66.00 0.50 0.60 -- -50.00 -49.00 -21.02 64 10 \w -89.00 -63.00 0.50 0.60 -- -50.00 -51.00 175.31 52 11 \w -102.00 -68.00 0.50 0.60 -- -54.00 -51.00 88.04 68 12 \w -115.00 -80.00 0.50 0.60 -- -66.00 -49.00 -42.60 70 13 \w 35.00 60.00 0.50 0.60 -- 71.77-115.00 -81.00 50 14 \w -118.00 -85.00 0.50 0.60 -- -74.00 -37.00-110.07 66 15 \w -97.00 -65.00 0.50 0.60 -- -78.00 114.00 -19.92 64 16 \w -97.00 -67.00 0.50 0.60 -- -78.00 114.00 63.41 60 17 \w -97.00 -70.00 0.50 0.60 -- -78.00 114.00 -83.92 54 18 \w -97.00 -56.00 0.50 0.60 -- -78.00 114.00-157.39 82 19 \w -97.00 -70.00 0.50 0.60 -- -78.00 114.00-118.96 54 20 \w -97.00 -59.00 0.50 0.60 -- -78.00 114.00 74.49 76 21 \w -124.00 -94.00 0.50 0.60 -- -79.50 -60.00-105.69 60 22 \w -126.00 -96.00 0.50 0.60 -- -79.50-120.00 44.33 60 23 \w -121.00 -95.00 0.50 0.60 -- -79.50 -56.00 84.09 52 24 \w -126.00 -92.00 0.50 0.60 -- -79.50 -54.00-152.03 68 25 \w -95.00 -48.00 0.50 0.60 -- -79.50 116.00 -81.06 94 26 \w -122.00 -92.00 0.50 0.60 -- -79.50 -60.00 143.98 60 27 \w -89.00 -34.00 0.50 0.60 -- -79.50 114.00 119.52 110 28 \w -122.00 -92.00 0.50 0.60 -- -79.50 -63.00 -55.03 60 29 \w 97.00 130.00 0.50 0.60 -- 82.25 15.00 120.00 66 30 \w 40.00 65.00 0.50 0.60 -- 82.25 -95.00 90.00 50 31 \w 37.00 62.00 0.50 0.60 -- 82.25-112.00 120.00 50 32 \w 37.00 62.00 0.50 0.60 -- 82.25-112.00-180.00 50 33 \w 37.00 62.00 0.50 0.60 -- 82.25-112.00-120.00 50 34 \w 63.00 90.00 0.50 0.60 -- 82.25 -95.00 -30.00 54 35 \w 42.00 71.00 0.50 0.60 -- 82.25 -95.00-120.00 58 36 \w 41.00 66.00 0.50 0.60 -- 82.25-112.00 90.00 50 37 \w 37.00 62.00 0.50 0.60 -- 82.25-112.00 -90.00 50 38 \w 68.00 126.00 0.50 0.60 -- 82.25 15.00 -90.00 116 39 \w 71.00 97.00 0.50 0.60 -- 82.25 15.00 -30.00 52 40 \w 84.00 110.00 0.50 0.60 -- 82.25 15.00 -60.00 52 41 \w 47.00 75.00 0.50 0.60 -- 82.25 15.00 90.00 56 42 \w 91.00 127.00 0.50 0.60 -- 82.25 15.00-120.00 72 43 \w 59.00 98.00 0.50 0.60 -- 82.25 15.00-180.00 78 44 \w 42.00 78.00 0.50 0.60 -- 82.25 -95.00 -90.00 72 45 \w 104.00 130.00 0.50 0.60 -- 82.25 15.00 90.00 52 46 \w 40.00 92.00 0.50 0.60 -- 85.25-128.00-130.39 104 47 \w 107.00 133.00 0.50 0.60 -- 85.25 49.00 43.99 52 48 \w 70.00 96.00 0.50 0.60 -- 85.25-119.00 44.69 52 49 \w 39.00 65.00 0.50 0.60 -- 85.25-119.00 44.69 52 50 \w 97.00 132.00 0.50 0.60 -- 85.25 125.00-120.42 70 51 \w 97.00 135.00 0.50 0.60 -- 85.25 40.00 -22.45 76 52 \w 72.00 97.00 0.50 0.60 -- 85.25-114.00-170.44 50 53 \w 95.00 130.00 0.50 0.60 -- 85.25 128.00 79.29 70 54 \w 40.00 65.00 0.50 0.60 -- 85.25-107.00 43.03 50 55 \w 41.00 67.00 0.50 0.60 -- 85.25-114.00-170.44 52 56 \w 44.00 69.00 0.50 0.60 -- 85.25 -73.00-156.18 50 57 \w 63.00 89.00 0.50 0.60 -- 85.25 -91.00 75.05 52 58 \w 40.00 69.00 0.50 0.60 -- 85.25-109.00 97.60 58 59 \w 54.00 80.00 0.50 0.60 -- 85.25-126.00 42.43 52 60 \w 54.00 92.00 0.50 0.60 -- 85.25 -94.00 63.77 76 61 \w 47.00 89.00 0.50 0.60 -- 85.25-107.00 1.70 84 62 \w 39.00 79.00 0.50 0.60 -- 85.25-139.00 99.12 80 63 \w 41.00 93.00 0.50 0.60 -- 85.25-113.00 -44.30 104 64 \w 51.00 92.00 0.50 0.60 -- 85.25-100.00 131.70 82 65 \w 107.00 132.00 0.50 0.60 -- 85.25 47.00 176.91 50 66 \w 39.00 102.00 0.50 0.60 -- 85.25-133.00 77.84 126 67 \w 74.00 99.00 0.50 0.60 -- 85.25-122.00 147.54 50 68 \w 104.00 131.00 0.50 0.60 -- 85.25 113.00 113.20 54 69 \w 38.00 64.00 0.50 0.60 -- 85.25-122.00 147.54 52 70 \w 106.00 131.00 0.50 0.60 -- 85.25 116.00 -58.82 50 71 \w 48.00 80.00 0.50 0.60 -- 85.25 -78.00 -6.79 64 72 \w 38.00 84.00 0.50 0.60 -- 85.25-128.00 178.10 92 73 \w 54.00 80.00 0.50 0.60 -- 85.25-133.00-136.31 52 74 \w 67.00 103.00 0.50 0.60 -- 85.25-131.00-150.78 72 75 \w 42.00 96.00 0.50 0.60 -- 85.25-119.00 -24.70 108 76 \w 45.00 91.00 0.50 0.60 -- 85.25 -92.00-156.58 92 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-R' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type ; CrysAlisPro convention (1999,Acta A55,543-557) ; _diffrn_orient_matrix_UB_11 0.0895592000 _diffrn_orient_matrix_UB_12 -0.0007579000 _diffrn_orient_matrix_UB_13 0.0738882000 _diffrn_orient_matrix_UB_21 0.1254388000 _diffrn_orient_matrix_UB_22 -0.0151443000 _diffrn_orient_matrix_UB_23 -0.0569103000 _diffrn_orient_matrix_UB_31 0.0185403000 _diffrn_orient_matrix_UB_32 0.1002203000 _diffrn_orient_matrix_UB_33 -0.0152435000 _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_xray_symbol K-L~2,3~ _diffrn_reflns_av_R_equivalents 0.1547 _diffrn_reflns_av_unetI/netI 0.0189 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 20203 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.527 _diffrn_reflns_theta_min 2.711 _diffrn_source 'rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet-R X-ray Source' _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.76348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.199 _exptl_crystal_description block _exptl_crystal_F_000 944 _exptl_crystal_preparation ; Crystals were grown from saturated solution. For data collection the crystal was immersed in a film of perfluoropolyether oil, mounted on a polyimide loop and transferred to stream of cold nitrogen (Oxford Cryostream 800). ; _exptl_crystal_size_max 0.321 _exptl_crystal_size_mid 0.132 _exptl_crystal_size_min 0.090 _refine_diff_density_max 0.703 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.064 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 659 _refine_ls_number_reflns 20203 _refine_ls_number_restraints 414 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0833 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1719P)^2^+0.4664P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2269 _refine_ls_wR_factor_ref 0.2381 _reflns_Friedel_coverage 0.000 _reflns_number_gt 16905 _reflns_number_total 20203 _reflns_threshold_expression 'I > 2\s(I)' _twin_dimensionality triperiodic _twin_formation_mechanism gt _twin_morphology polysynthetic _twin_special_details ; Component 2 rotated by 6.0699\% around [0.90 -0.24 -0.37] (reciprocal) or [0.98 -0.10 -0.17] (direct) ; _cod_data_source_file d4sc03817g2.cif _cod_data_source_block 5 _cod_database_code 1572074 _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_res_file ; TITL MaMi132_NeWi_twin1_hklf4_a.res in P-1 MaMi132_NeWi_twin1_hklf5.res created by SHELXL-2018/3 at 17:30:24 on 28-Feb-2023 REM Old TITL MaMi132_NeWi_twin1_hklf4 in P-1 REM SHELXT solution in P-1: R1 0.165, Rweak 0.010, Alpha 0.045 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C63 B N3 Si CELL 1.54184 9.9393 15.2431 16.3736 85.650 86.819 89.362 ZERR 2.000 0.0002 0.0002 0.0003 0.001 0.002 0.001 LATT 1 SFAC C H B N SI UNIT 124 110 4 6 2 TEMP -173 L.S. 10 BOND $H LIST 4 ACTA CONF FMAP 2 MERG 0 PLAN 20 WGHT 0.171900 0.466400 BASF 0.52744 FVAR 6.15397 0.42159 SI01 5 0.874202 0.146742 0.885332 11.00000 0.02698 0.03901 = 0.02881 -0.00459 -0.00560 0.00268 N002 4 0.552139 0.229223 0.790507 11.00000 0.02615 0.03271 = 0.02658 -0.00477 -0.00406 -0.00001 N003 4 0.735487 0.145202 0.816114 11.00000 0.02487 0.03527 = 0.02999 -0.00507 -0.00177 0.00462 N004 4 0.634609 0.199743 0.842357 11.00000 0.02552 0.03282 = 0.03025 -0.00431 -0.00453 0.00233 C005 1 0.563636 0.217038 0.701764 11.00000 0.02620 0.03705 = 0.02781 -0.00420 -0.00435 0.00412 C006 1 0.507866 0.147189 0.671829 11.00000 0.02624 0.03730 = 0.03002 -0.00520 -0.00407 0.00263 C007 1 0.496840 0.138131 0.582126 11.00000 0.03339 0.03546 = 0.02975 -0.00605 -0.00587 -0.00170 C008 1 0.337805 0.328435 0.752398 11.00000 0.02668 0.03865 = 0.02791 -0.00575 -0.00181 0.00455 C009 1 0.360335 0.259926 0.905799 11.00000 0.02583 0.03797 = 0.02865 -0.00509 -0.00690 0.00168 C00A 1 0.463750 0.069958 0.726696 11.00000 0.03064 0.03435 = 0.02843 -0.00762 -0.00278 0.00125 C00B 1 0.492233 0.551012 0.767938 11.00000 0.03162 0.03538 = 0.03684 -0.00579 -0.00525 0.00374 C00C 1 0.517836 0.393364 0.827991 11.00000 0.02988 0.03483 = 0.02716 -0.00547 -0.00197 0.00167 C00D 1 0.349652 0.419649 0.733011 11.00000 0.02799 0.03846 = 0.02967 -0.00435 -0.00238 0.00249 C00E 1 0.622122 0.296162 0.654370 11.00000 0.03053 0.03487 = 0.02877 -0.00530 -0.00118 0.00214 C00F 1 0.240413 0.282913 0.716230 11.00000 0.02990 0.03850 = 0.03409 -0.00443 -0.00460 0.00067 AFIX 43 H00F 2 0.230544 0.221461 0.729379 11.00000 -1.20000 AFIX 0 C00G 1 0.562743 0.031305 0.775691 11.00000 0.03037 0.03516 = 0.02932 -0.00879 -0.00293 0.00165 C00H 1 0.335855 0.032241 0.727510 11.00000 0.02805 0.03841 = 0.03644 -0.00816 -0.00301 0.00056 AFIX 43 H00H 2 0.269576 0.057956 0.693342 11.00000 -1.20000 AFIX 0 C00I 1 0.560991 0.335022 0.585360 11.00000 0.04071 0.03922 = 0.02956 -0.00530 -0.00480 0.00285 AFIX 43 H00I 2 0.479582 0.311657 0.568623 11.00000 -1.20000 AFIX 0 C00J 1 0.263565 0.140519 0.996730 11.00000 0.03696 0.04076 = 0.03622 0.00114 -0.00562 -0.00356 AFIX 43 H00J 2 0.253581 0.079109 1.010080 11.00000 -1.20000 AFIX 0 C00K 1 0.213451 0.288778 1.025859 11.00000 0.03648 0.04814 = 0.03458 -0.00966 -0.00013 0.00173 AFIX 43 H00K 2 0.169137 0.329983 1.059028 11.00000 -1.20000 AFIX 0 C00L 1 0.292947 0.318124 0.956855 11.00000 0.03429 0.03708 = 0.03423 -0.00600 -0.00255 0.00052 AFIX 43 H00L 2 0.301978 0.379646 0.943804 11.00000 -1.20000 AFIX 0 C00M 1 0.343010 0.170217 0.927668 11.00000 0.03234 0.03962 = 0.03239 -0.00525 -0.00408 0.00123 AFIX 43 H00M 2 0.386435 0.128523 0.894656 11.00000 -1.20000 AFIX 0 C00N 1 0.458611 0.456240 0.778027 11.00000 0.02974 0.03650 = 0.02957 -0.00489 -0.00308 0.00275 C00O 1 0.633925 0.408593 0.877362 11.00000 0.03213 0.03235 = 0.03506 -0.00771 -0.00659 0.00268 C00P 1 0.198979 0.199536 1.046142 11.00000 0.03627 0.05452 = 0.03064 -0.00180 -0.00168 -0.00331 AFIX 43 H00P 2 0.145360 0.178979 1.093416 11.00000 -1.20000 AFIX 0 C00Q 1 0.823789 0.035965 0.711182 11.00000 0.02748 0.05000 = 0.03278 -0.01214 -0.00750 0.00417 C00R 1 0.306261 -0.042661 0.778274 11.00000 0.03312 0.04088 = 0.04663 -0.01002 0.00401 -0.00145 AFIX 43 H00R 2 0.219262 -0.068037 0.779288 11.00000 -1.20000 AFIX 0 C00S 1 0.502215 0.600715 0.835464 11.00000 0.04412 0.03678 = 0.03762 -0.00589 -0.00599 0.00513 AFIX 43 H00S 2 0.485562 0.573646 0.889215 11.00000 -1.20000 AFIX 0 C00T 1 0.738704 0.333528 0.679179 11.00000 0.03216 0.04067 = 0.03405 -0.00287 -0.00319 0.00040 AFIX 43 H00T 2 0.779847 0.308573 0.726629 11.00000 -1.20000 AFIX 0 C00U 1 0.839827 -0.053831 0.701159 11.00000 0.03544 0.05305 = 0.04925 -0.01989 -0.01138 0.00931 AFIX 43 H00U 2 0.779005 -0.094697 0.729522 11.00000 -1.20000 AFIX 0 C00V 1 0.639114 0.369020 0.956854 11.00000 0.03860 0.04247 = 0.03535 -0.00679 -0.00812 0.00038 AFIX 43 H00V 2 0.567952 0.331591 0.978570 11.00000 -1.20000 AFIX 0 C00W 1 0.264515 0.464205 0.678994 11.00000 0.03419 0.04072 = 0.03590 0.00015 -0.00443 0.00443 AFIX 43 H00W 2 0.271367 0.526084 0.667590 11.00000 -1.20000 AFIX 0 C00X 1 0.156174 0.326561 0.660387 11.00000 0.02997 0.05054 = 0.03713 -0.00339 -0.00880 -0.00129 AFIX 43 H00X 2 0.090318 0.294681 0.635176 11.00000 -1.20000 AFIX 0 C00Y 1 0.372771 0.150158 0.546679 11.00000 0.03569 0.04508 = 0.03480 -0.00886 -0.00566 0.00096 AFIX 43 H00Y 2 0.297342 0.170194 0.578500 11.00000 -1.20000 AFIX 0 C00Z 1 0.529864 -0.044248 0.826555 11.00000 0.03953 0.03668 = 0.03407 -0.00367 -0.00413 0.00314 AFIX 43 H00Z 2 0.595341 -0.070848 0.860802 11.00000 -1.20000 AFIX 0 C010 1 0.169182 0.416576 0.641972 11.00000 0.03079 0.05221 = 0.03684 0.00232 -0.00925 0.00406 AFIX 43 H010 2 0.112439 0.445982 0.603708 11.00000 -1.20000 AFIX 0 C011 1 0.358335 0.133352 0.466189 11.00000 0.04194 0.04641 = 0.03612 -0.00493 -0.01194 -0.00009 AFIX 43 H011 2 0.273232 0.141445 0.442897 11.00000 -1.20000 AFIX 0 C012 1 0.965207 0.250034 0.859327 11.00000 0.03392 0.05092 = 0.03842 -0.00340 -0.00771 -0.00314 AFIX 137 H01A 2 0.996597 0.253243 0.801380 11.00000 -1.50000 H01B 2 1.042760 0.252161 0.893546 11.00000 -1.50000 H01C 2 0.904875 0.299875 0.869162 11.00000 -1.50000 AFIX 0 C013 1 0.736143 0.443431 0.566273 11.00000 0.04940 0.03988 = 0.03658 -0.00154 0.00720 0.00091 AFIX 43 H013 2 0.775369 0.493116 0.535778 11.00000 -1.20000 AFIX 0 C014 1 0.607313 0.110994 0.533994 11.00000 0.03372 0.04646 = 0.03190 -0.00673 -0.00415 0.00118 AFIX 43 H014 2 0.692808 0.103252 0.556855 11.00000 -1.20000 AFIX 0 C015 1 0.516501 0.592993 0.689914 11.00000 0.03964 0.03812 = 0.03696 -0.00505 -0.00298 0.00186 AFIX 43 H015 2 0.510500 0.560371 0.643079 11.00000 -1.20000 AFIX 0 C016 1 0.983655 0.048564 0.872607 11.00000 0.03309 0.05023 = 0.03913 -0.00862 -0.01019 0.00926 AFIX 137 H01D 2 1.028936 0.053147 0.817754 11.00000 -1.50000 H01E 2 0.928469 -0.004643 0.879272 11.00000 -1.50000 H01F 2 1.051290 0.045407 0.914083 11.00000 -1.50000 AFIX 0 C017 1 0.793499 0.140382 0.990028 11.00000 0.04070 0.04478 = 0.03102 -0.00250 -0.00606 0.00449 AFIX 137 H01G 2 0.733665 0.191291 0.996047 11.00000 -1.50000 H01H 2 0.863035 0.140325 1.030187 11.00000 -1.50000 H01I 2 0.741001 0.086158 0.999366 11.00000 -1.50000 AFIX 0 C018 1 0.912760 0.094504 0.666394 11.00000 0.03298 0.06311 = 0.03547 -0.01107 -0.00341 0.00025 AFIX 43 H018 2 0.905093 0.155749 0.673110 11.00000 -1.20000 AFIX 0 C019 1 0.743507 0.461343 0.846765 11.00000 0.03580 0.03656 = 0.04134 -0.00544 -0.00735 -0.00090 AFIX 43 H019 2 0.743702 0.488415 0.792552 11.00000 -1.20000 AFIX 0 C01A 1 0.549244 0.681515 0.679437 11.00000 0.04522 0.04158 = 0.04620 0.00190 -0.00085 -0.00030 AFIX 43 H01J 2 0.565073 0.709166 0.625843 11.00000 -1.20000 AFIX 0 C01B 1 0.468205 0.104583 0.419121 11.00000 0.05538 0.04405 = 0.02864 -0.00721 -0.00896 0.00132 AFIX 43 H01K 2 0.457985 0.091343 0.364045 11.00000 -1.20000 AFIX 0 C01C 1 0.402715 -0.080498 0.827341 11.00000 0.04122 0.03755 = 0.04065 -0.00095 0.00426 -0.00083 AFIX 43 H01L 2 0.381728 -0.131902 0.861997 11.00000 -1.20000 AFIX 0 C01D 1 0.619138 0.407353 0.541637 11.00000 0.05079 0.04084 = 0.03154 -0.00158 -0.00269 0.00448 AFIX 43 H01M 2 0.578380 0.432592 0.494162 11.00000 -1.20000 AFIX 0 C01E 1 0.795846 0.406872 0.635513 11.00000 0.03386 0.04164 = 0.04625 -0.00317 0.00122 -0.00411 AFIX 43 H01N 2 0.875492 0.431828 0.653065 11.00000 -1.20000 AFIX 0 C01F 1 0.592344 0.095295 0.452666 11.00000 0.04661 0.04882 = 0.03133 -0.00810 -0.00075 0.00356 AFIX 43 H01O 2 0.668311 0.077977 0.419736 11.00000 -1.20000 AFIX 0 C01G 1 0.536097 0.689075 0.825283 11.00000 0.05169 0.03943 = 0.04763 -0.01114 -0.00989 0.00317 AFIX 43 H01P 2 0.543689 0.721793 0.871919 11.00000 -1.20000 AFIX 0 C01H 1 0.558773 0.729481 0.747540 11.00000 0.05294 0.03563 = 0.05605 -0.00282 -0.00719 -0.00317 AFIX 43 H01Q 2 0.580915 0.790156 0.740644 11.00000 -1.20000 AFIX 0 C01I 1 0.746392 0.383441 1.004619 11.00000 0.04728 0.05283 = 0.03918 -0.00750 -0.01732 0.00070 AFIX 43 H01R 2 0.747038 0.356874 1.058992 11.00000 -1.20000 AFIX 0 C01J 1 0.851408 0.474323 0.894853 11.00000 0.03816 0.04408 = 0.05845 -0.00859 -0.01355 -0.00473 AFIX 43 H01S 2 0.924975 0.509730 0.873215 11.00000 -1.20000 AFIX 0 C01K 1 1.011775 0.064156 0.612435 11.00000 0.03147 0.10135 = 0.03829 -0.01719 0.00026 -0.00307 AFIX 43 H01T 2 1.068629 0.104715 0.580391 11.00000 -1.20000 AFIX 0 C01L 1 0.944110 -0.083997 0.649993 11.00000 0.04323 0.07384 = 0.06762 -0.03991 -0.01564 0.02369 AFIX 43 H01U 2 0.957452 -0.145365 0.645990 11.00000 -1.20000 AFIX 0 C01M 1 1.027763 -0.024757 0.605259 11.00000 0.03185 0.10877 = 0.05347 -0.04214 -0.00646 0.01672 AFIX 43 H01V 2 1.097127 -0.045395 0.569122 11.00000 -1.20000 AFIX 0 C01N 1 0.852058 0.435975 0.973891 11.00000 0.04591 0.05200 = 0.05421 -0.01257 -0.02056 -0.00441 AFIX 43 H01W 2 0.925143 0.445771 1.007013 11.00000 -1.20000 AFIX 0 B01O 3 0.440832 0.299996 0.822787 11.00000 0.02708 0.03382 = 0.02923 -0.00619 -0.00412 0.00321 B1 3 0.707474 0.073145 0.766471 11.00000 0.02975 0.03708 = 0.02895 -0.00418 -0.00579 0.00411 SIMU 0.008 C1_1 > C7_2 DELU 0.008 C1_1 > C7_2 RIGU 0.004 C1_1 > C7_2 ISOR 0.01 C1_1 > C7_2 RESI TOL 1 PART 1 21 C1 1 0.907259 0.295374 0.200607 21.00000 0.11000 0.15327 = 0.05899 0.00679 0.00617 0.02181 AFIX 137 H1A 2 0.814073 0.312834 0.190580 21.00000 -1.50000 H1B 2 0.921313 0.233828 0.188592 21.00000 -1.50000 H1C 2 0.969082 0.332888 0.165094 21.00000 -1.50000 AFIX 66 C2 1 0.932937 0.305126 0.285988 21.00000 0.05020 0.08804 = 0.07202 0.01229 -0.00390 0.00607 C3 1 1.057926 0.330894 0.309462 21.00000 0.04696 0.07475 = 0.07650 0.00574 -0.00011 0.00181 AFIX 43 H3 2 1.126636 0.348146 0.268966 21.00000 -1.20000 AFIX 65 C4 1 1.082383 0.331419 0.392188 21.00000 0.05748 0.07824 = 0.08016 -0.01081 -0.00005 -0.00574 AFIX 43 H4 2 1.167808 0.349029 0.408231 21.00000 -1.20000 AFIX 65 C5 1 0.981849 0.306176 0.451440 21.00000 0.05246 0.08074 = 0.06859 -0.02537 -0.00041 0.00233 AFIX 43 H5 2 0.998565 0.306535 0.507979 21.00000 -1.20000 AFIX 65 C6 1 0.856860 0.280409 0.427967 21.00000 0.05769 0.06593 = 0.07342 -0.02312 -0.00049 0.00271 AFIX 43 H6 2 0.788150 0.263157 0.468463 21.00000 -1.20000 AFIX 65 C7 1 0.832402 0.279883 0.345242 21.00000 0.03721 0.06054 = 0.06134 -0.00181 0.00384 0.00887 AFIX 43 H7 2 0.746976 0.262273 0.329199 21.00000 -1.20000 AFIX 0 PART 0 RESI 0 RESI TOL 2 PART 2 -21 C1 1 0.842846 0.306765 0.219247 -21.00000 0.06788 0.13232 = 0.09420 -0.03749 -0.03939 0.03647 AFIX 137 H1A 2 0.893121 0.266827 0.184388 -21.00000 -1.50000 H1B 2 0.843123 0.366203 0.191848 -21.00000 -1.50000 H1C 2 0.749756 0.286402 0.228994 -21.00000 -1.50000 AFIX 66 C2 1 0.905066 0.308029 0.296060 -21.00000 0.04950 0.07602 = 0.06701 0.00301 -0.01225 0.01520 C3 1 1.037209 0.337155 0.295122 -21.00000 0.05087 0.07299 = 0.08061 0.00977 -0.00877 -0.00262 AFIX 43 H3 2 1.084357 0.354155 0.244433 -21.00000 -1.20000 AFIX 65 C4 1 1.100367 0.341406 0.368349 -21.00000 0.05729 0.07189 = 0.06683 -0.00200 0.00165 -0.00559 AFIX 43 H4 2 1.190681 0.361312 0.367708 -21.00000 -1.20000 AFIX 65 C5 1 1.031384 0.316532 0.442515 -21.00000 0.06014 0.07646 = 0.06002 -0.01960 -0.00251 -0.00255 AFIX 43 H5 2 1.074551 0.319438 0.492562 -21.00000 -1.20000 AFIX 65 C6 1 0.899241 0.287407 0.443454 -21.00000 0.05183 0.06647 = 0.06416 -0.01941 0.01015 0.00531 AFIX 43 H6 2 0.852094 0.270406 0.494143 -21.00000 -1.20000 AFIX 65 C7 1 0.836081 0.283155 0.370227 -21.00000 0.04649 0.05517 = 0.06832 -0.01023 -0.00107 0.01290 AFIX 43 H7 2 0.745767 0.263249 0.370869 -21.00000 -1.20000 AFIX 0 HKLF 5 REM MaMi132_NeWi_twin1_hklf4_a.res in P-1 REM wR2 = 0.238102, GooF = S = 1.04063, Restrained GooF = 1.04465 for all data REM R1 = 0.083326 for 16905 Fo > 4sig(Fo) and 0.092741 for all 20203 data REM 659 parameters refined using 414 restraints END WGHT 0.1719 0.4664 REM Highest difference peak 0.703, deepest hole -0.580, 1-sigma level 0.064 Q1 1 1.0676 0.3195 0.2409 11.00000 0.05 0.70 Q2 1 0.9586 0.3113 0.3775 11.00000 0.05 0.64 Q3 1 0.8993 0.2136 0.8904 11.00000 0.05 0.56 Q4 1 0.8226 0.2901 0.2707 11.00000 0.05 0.54 Q5 1 0.8607 0.1352 0.9479 11.00000 0.05 0.43 Q6 1 0.8761 0.0775 0.8815 11.00000 0.05 0.39 Q7 1 0.8457 0.2767 0.9463 11.00000 0.05 0.38 Q8 1 0.5494 0.0190 0.8383 11.00000 0.05 0.35 Q9 1 1.0618 0.3029 0.3374 11.00000 0.05 0.31 Q10 1 0.3620 -0.0380 0.7998 11.00000 0.05 0.31 Q11 1 0.2861 -0.1171 0.7827 11.00000 0.05 0.27 Q12 1 1.0375 0.3544 0.3480 11.00000 0.05 0.27 Q13 1 0.9704 0.3121 0.2145 11.00000 0.05 0.27 Q14 1 0.8954 0.3773 0.9122 11.00000 0.05 0.25 Q15 1 0.5015 0.5857 0.7451 11.00000 0.05 0.25 Q16 1 0.5414 0.0966 0.7879 11.00000 0.05 0.25 Q17 1 0.5026 0.1464 0.6335 11.00000 0.05 0.25 Q18 1 1.0179 0.0118 0.6061 11.00000 0.05 0.25 Q19 1 0.2636 0.3091 1.0009 11.00000 0.05 0.24 Q20 1 0.7597 0.4010 0.6979 11.00000 0.05 0.24 ; _shelx_res_checksum 37109 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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si01 Si 0.87420(6) 0.14674(4) 0.88533(4) 0.03136(19) Uani 1 1 d . . . . . N002 N 0.55214(19) 0.22922(12) 0.79051(12) 0.0283(4) Uani 1 1 d . . . . . N003 N 0.73549(19) 0.14520(13) 0.81611(12) 0.0299(4) Uani 1 1 d . . . . . N004 N 0.63461(19) 0.19974(12) 0.84236(12) 0.0293(4) Uani 1 1 d . . . . . C005 C 0.5636(2) 0.21704(15) 0.70176(14) 0.0302(5) Uani 1 1 d . . . . . C006 C 0.5079(2) 0.14719(15) 0.67183(14) 0.0310(5) Uani 1 1 d . . . . . C007 C 0.4968(2) 0.13813(15) 0.58213(15) 0.0325(5) Uani 1 1 d . . . . . C008 C 0.3378(2) 0.32843(16) 0.75240(14) 0.0309(5) Uani 1 1 d . . . . . C009 C 0.3603(2) 0.25993(15) 0.90580(14) 0.0305(5) Uani 1 1 d . . . . . C00A C 0.4637(2) 0.06996(15) 0.72670(14) 0.0308(5) Uani 1 1 d . . . . . C00B C 0.4922(2) 0.55101(16) 0.76794(16) 0.0344(5) Uani 1 1 d . . . . . C00C C 0.5178(2) 0.39336(15) 0.82799(14) 0.0305(5) Uani 1 1 d . . . . . C00D C 0.3497(2) 0.41965(16) 0.73301(14) 0.0319(5) Uani 1 1 d . . . . . C00E C 0.6221(2) 0.29616(15) 0.65437(14) 0.0313(5) Uani 1 1 d . . . . . C00F C 0.2404(2) 0.28291(16) 0.71623(15) 0.0340(5) Uani 1 1 d . . . . . H00F H 0.230544 0.221461 0.729379 0.041 Uiso 1 1 calc R U . . . C00G C 0.5627(2) 0.03130(15) 0.77569(14) 0.0313(5) Uani 1 1 d . . . . . C00H C 0.3359(2) 0.03224(16) 0.72751(15) 0.0340(5) Uani 1 1 d . . . . . H00H H 0.269576 0.057956 0.693342 0.041 Uiso 1 1 calc R U . . . C00I C 0.5610(3) 0.33502(16) 0.58536(15) 0.0363(5) Uani 1 1 d . . . . . H00I H 0.479582 0.311657 0.568623 0.044 Uiso 1 1 calc R U . . . C00J C 0.2636(3) 0.14052(17) 0.99673(16) 0.0380(5) Uani 1 1 d . . . . . H00J H 0.253581 0.079109 1.010080 0.046 Uiso 1 1 calc R U . . . C00K C 0.2135(3) 0.28878(18) 1.02586(16) 0.0395(6) Uani 1 1 d . . . . . H00K H 0.169137 0.329983 1.059028 0.047 Uiso 1 1 calc R U . . . C00L C 0.2929(2) 0.31812(16) 0.95685(15) 0.0350(5) Uani 1 1 d . . . . . H00L H 0.301978 0.379646 0.943804 0.042 Uiso 1 1 calc R U . . . C00M C 0.3430(2) 0.17022(16) 0.92767(15) 0.0346(5) Uani 1 1 d . . . . . H00M H 0.386435 0.128523 0.894656 0.041 Uiso 1 1 calc R U . . . C00N C 0.4586(2) 0.45624(15) 0.77803(14) 0.0318(5) Uani 1 1 d . . . . . C00O C 0.6339(2) 0.40859(15) 0.87736(15) 0.0328(5) Uani 1 1 d . . . . . C00P C 0.1990(3) 0.19954(18) 1.04614(16) 0.0405(6) Uani 1 1 d . . . . . H00P H 0.145360 0.178979 1.093416 0.049 Uiso 1 1 calc R U . . . C00Q C 0.8238(2) 0.03596(17) 0.71118(15) 0.0361(5) Uani 1 1 d . . . . . C00R C 0.3063(3) -0.04266(17) 0.77827(17) 0.0401(6) Uani 1 1 d . . . . . H00R H 0.219262 -0.068037 0.779288 0.048 Uiso 1 1 calc R U . . . C00S C 0.5022(3) 0.60072(16) 0.83546(17) 0.0392(6) Uani 1 1 d . . . . . H00S H 0.485562 0.573646 0.889215 0.047 Uiso 1 1 calc R U . . . C00T C 0.7387(2) 0.33353(16) 0.67918(16) 0.0356(5) Uani 1 1 d . . . . . H00T H 0.779847 0.308573 0.726629 0.043 Uiso 1 1 calc R U . . . C00U C 0.8398(3) -0.05383(19) 0.70116(18) 0.0448(6) Uani 1 1 d . . . . . H00U H 0.779005 -0.094697 0.729522 0.054 Uiso 1 1 calc R U . . . C00V C 0.6391(3) 0.36902(17) 0.95685(16) 0.0384(5) Uani 1 1 d . . . . . H00V H 0.567952 0.331591 0.978570 0.046 Uiso 1 1 calc R U . . . C00W C 0.2645(3) 0.46420(17) 0.67899(16) 0.0370(5) Uani 1 1 d . . . . . H00W H 0.271367 0.526084 0.667590 0.044 Uiso 1 1 calc R U . . . C00X C 0.1562(3) 0.32656(18) 0.66039(16) 0.0389(6) Uani 1 1 d . . . . . H00X H 0.090318 0.294681 0.635176 0.047 Uiso 1 1 calc R U . . . C00Y C 0.3728(3) 0.15016(17) 0.54668(16) 0.0381(5) Uani 1 1 d . . . . . H00Y H 0.297342 0.170194 0.578500 0.046 Uiso 1 1 calc R U . . . C00Z C 0.5299(3) -0.04425(16) 0.82655(16) 0.0367(5) Uani 1 1 d . . . . . H00Z H 0.595341 -0.070848 0.860802 0.044 Uiso 1 1 calc R U . . . C010 C 0.1692(3) 0.41658(18) 0.64197(16) 0.0400(6) Uani 1 1 d . . . . . H010 H 0.112439 0.445982 0.603708 0.048 Uiso 1 1 calc R U . . . C011 C 0.3583(3) 0.13335(18) 0.46619(16) 0.0410(6) Uani 1 1 d . . . . . H011 H 0.273232 0.141445 0.442897 0.049 Uiso 1 1 calc R U . . . C012 C 0.9652(3) 0.25003(18) 0.85933(17) 0.0408(6) Uani 1 1 d . . . . . H01A H 0.996597 0.253243 0.801380 0.061 Uiso 1 1 calc R U . . . H01B H 1.042760 0.252161 0.893546 0.061 Uiso 1 1 calc R U . . . H01C H 0.904875 0.299875 0.869162 0.061 Uiso 1 1 calc R U . . . C013 C 0.7361(3) 0.44343(18) 0.56627(17) 0.0424(6) Uani 1 1 d . . . . . H013 H 0.775369 0.493116 0.535778 0.051 Uiso 1 1 calc R U . . . C014 C 0.6073(3) 0.11099(17) 0.53399(15) 0.0371(5) Uani 1 1 d . . . . . H014 H 0.692808 0.103252 0.556855 0.045 Uiso 1 1 calc R U . . . C015 C 0.5165(3) 0.59299(17) 0.68991(16) 0.0381(5) Uani 1 1 d . . . . . H015 H 0.510500 0.560371 0.643079 0.046 Uiso 1 1 calc R U . . . C016 C 0.9837(3) 0.04856(18) 0.87261(17) 0.0403(6) Uani 1 1 d . . . . . H01D H 1.028936 0.053147 0.817754 0.060 Uiso 1 1 calc R U . . . H01E H 0.928469 -0.004643 0.879272 0.060 Uiso 1 1 calc R U . . . H01F H 1.051290 0.045407 0.914083 0.060 Uiso 1 1 calc R U . . . C017 C 0.7935(3) 0.14038(18) 0.99003(15) 0.0387(5) Uani 1 1 d . . . . . H01G H 0.733665 0.191291 0.996047 0.058 Uiso 1 1 calc R U . . . H01H H 0.863035 0.140325 1.030187 0.058 Uiso 1 1 calc R U . . . H01I H 0.741001 0.086158 0.999366 0.058 Uiso 1 1 calc R U . . . C018 C 0.9128(3) 0.0945(2) 0.66639(17) 0.0434(6) Uani 1 1 d . . . . . H018 H 0.905093 0.155749 0.673110 0.052 Uiso 1 1 calc R U . . . C019 C 0.7435(3) 0.46134(16) 0.84676(17) 0.0376(5) Uani 1 1 d . . . . . H019 H 0.743702 0.488415 0.792552 0.045 Uiso 1 1 calc R U . . . C01A C 0.5492(3) 0.68151(18) 0.67944(18) 0.0447(6) Uani 1 1 d . . . . . H01J H 0.565073 0.709166 0.625843 0.054 Uiso 1 1 calc R U . . . C01B C 0.4682(3) 0.10458(17) 0.41912(16) 0.0422(6) Uani 1 1 d . . . . . H01K H 0.457985 0.091343 0.364045 0.051 Uiso 1 1 calc R U . . . C01C C 0.4027(3) -0.08050(17) 0.82734(17) 0.0401(6) Uani 1 1 d . . . . . H01L H 0.381728 -0.131902 0.861997 0.048 Uiso 1 1 calc R U . . . C01D C 0.6191(3) 0.40735(17) 0.54164(16) 0.0411(6) Uani 1 1 d . . . . . H01M H 0.578380 0.432592 0.494162 0.049 Uiso 1 1 calc R U . . . C01E C 0.7958(3) 0.40687(17) 0.63551(17) 0.0407(6) Uani 1 1 d . . . . . H01N H 0.875492 0.431828 0.653065 0.049 Uiso 1 1 calc R U . . . C01F C 0.5923(3) 0.09530(18) 0.45267(16) 0.0421(6) Uani 1 1 d . . . . . H01O H 0.668311 0.077977 0.419736 0.050 Uiso 1 1 calc R U . . . C01G C 0.5361(3) 0.68907(18) 0.82528(19) 0.0456(6) Uani 1 1 d . . . . . H01P H 0.543689 0.721793 0.871919 0.055 Uiso 1 1 calc R U . . . C01H C 0.5588(3) 0.72948(18) 0.7475(2) 0.0481(7) Uani 1 1 d . . . . . H01Q H 0.580915 0.790156 0.740644 0.058 Uiso 1 1 calc R U . . . C01I C 0.7464(3) 0.38344(19) 1.00462(18) 0.0457(6) Uani 1 1 d . . . . . H01R H 0.747038 0.356874 1.058992 0.055 Uiso 1 1 calc R U . . . C01J C 0.8514(3) 0.47432(18) 0.8949(2) 0.0462(6) Uani 1 1 d . . . . . H01S H 0.924975 0.509730 0.873215 0.055 Uiso 1 1 calc R U . . . C01K C 1.0118(3) 0.0642(3) 0.61243(19) 0.0565(8) Uani 1 1 d . . . . . H01T H 1.068629 0.104715 0.580391 0.068 Uiso 1 1 calc R U . . . C01L C 0.9441(3) -0.0840(2) 0.6500(2) 0.0595(9) Uani 1 1 d . . . . . H01U H 0.957452 -0.145365 0.645990 0.071 Uiso 1 1 calc R U . . . C01M C 1.0278(3) -0.0248(3) 0.6053(2) 0.0628(10) Uani 1 1 d . . . . . H01V H 1.097127 -0.045395 0.569122 0.075 Uiso 1 1 calc R U . . . C01N C 0.8521(3) 0.43598(19) 0.9739(2) 0.0496(7) Uani 1 1 d . . . . . H01W H 0.925143 0.445771 1.007013 0.059 Uiso 1 1 calc R U . . . B01O B 0.4408(3) 0.30000(17) 0.82279(16) 0.0298(5) Uani 1 1 d . . . . . B1 B 0.7075(3) 0.07314(18) 0.76647(16) 0.0317(5) Uani 1 1 d . . . . . C1_1 C 0.907(2) 0.2954(13) 0.2006(8) 0.109(4) Uani 0.422(17) 1 d . U P A 1 H1A_1 H 0.814073 0.312834 0.190580 0.163 Uiso 0.422(17) 1 calc R U P A 1 H1B_1 H 0.921313 0.233828 0.188592 0.163 Uiso 0.422(17) 1 calc R U P A 1 H1C_1 H 0.969082 0.332888 0.165094 0.163 Uiso 0.422(17) 1 calc R U P A 1 C2_1 C 0.9329(12) 0.3051(11) 0.2860(4) 0.071(2) Uani 0.422(17) 1 d G U P A 1 C3_1 C 1.0579(10) 0.3309(10) 0.3095(7) 0.067(2) Uani 0.422(17) 1 d G U P A 1 H3_1 H 1.126636 0.348146 0.268966 0.080 Uiso 0.422(17) 1 calc R U P A 1 C4_1 C 1.0824(9) 0.3314(9) 0.3922(8) 0.072(2) Uani 0.422(17) 1 d G U P A 1 H4_1 H 1.167808 0.349029 0.408231 0.086 Uiso 0.422(17) 1 calc R U P A 1 C5_1 C 0.9818(15) 0.3062(8) 0.4514(5) 0.066(2) Uani 0.422(17) 1 d G U P A 1 H5_1 H 0.998565 0.306535 0.507979 0.080 Uiso 0.422(17) 1 calc R U P A 1 C6_1 C 0.8569(12) 0.2804(7) 0.4280(6) 0.065(2) Uani 0.422(17) 1 d G U P A 1 H6_1 H 0.788150 0.263157 0.468463 0.078 Uiso 0.422(17) 1 calc R U P A 1 C7_1 C 0.8324(8) 0.2799(9) 0.3452(8) 0.0535(19) Uani 0.422(17) 1 d G U P A 1 H7_1 H 0.746976 0.262273 0.329199 0.064 Uiso 0.422(17) 1 calc R U P A 1 C1_2 C 0.8428(12) 0.3068(8) 0.2192(8) 0.096(3) Uani 0.578(17) 1 d . U P A 2 H1A_2 H 0.893121 0.266827 0.184388 0.143 Uiso 0.578(17) 1 calc R U P A 2 H1B_2 H 0.843123 0.366203 0.191848 0.143 Uiso 0.578(17) 1 calc R U P A 2 H1C_2 H 0.749756 0.286402 0.228994 0.143 Uiso 0.578(17) 1 calc R U P A 2 C2_2 C 0.9051(8) 0.3080(7) 0.2961(4) 0.0644(16) Uani 0.578(17) 1 d G U P A 2 C3_2 C 1.0372(8) 0.3372(7) 0.2951(4) 0.0687(18) Uani 0.578(17) 1 d G U P A 2 H3_2 H 1.084357 0.354155 0.244433 0.082 Uiso 0.578(17) 1 calc R U P A 2 C4_2 C 1.1004(6) 0.3414(6) 0.3683(6) 0.0657(17) Uani 0.578(17) 1 d G U P A 2 H4_2 H 1.190681 0.361312 0.367708 0.079 Uiso 0.578(17) 1 calc R U P A 2 C5_2 C 1.0314(10) 0.3165(5) 0.4425(4) 0.0648(18) Uani 0.578(17) 1 d G U P A 2 H5_2 H 1.074551 0.319438 0.492562 0.078 Uiso 0.578(17) 1 calc R U P A 2 C6_2 C 0.8992(10) 0.2874(5) 0.4435(4) 0.0606(18) Uani 0.578(17) 1 d G U P A 2 H6_2 H 0.852094 0.270406 0.494143 0.073 Uiso 0.578(17) 1 calc R U P A 2 C7_2 C 0.8361(5) 0.2832(6) 0.3702(6) 0.0566(16) Uani 0.578(17) 1 d G U P A 2 H7_2 H 0.745767 0.263249 0.370869 0.068 Uiso 0.578(17) 1 calc R U P A 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 0.0270(3) 0.0390(4) 0.0288(3) -0.0046(2) -0.0056(2) 0.0027(2) N002 0.0262(9) 0.0327(9) 0.0266(9) -0.0048(7) -0.0041(7) 0.0000(7) N003 0.0249(9) 0.0353(10) 0.0300(10) -0.0051(8) -0.0018(7) 0.0046(7) N004 0.0255(9) 0.0328(10) 0.0302(10) -0.0043(7) -0.0045(7) 0.0023(7) C005 0.0262(10) 0.0371(12) 0.0278(11) -0.0042(9) -0.0044(8) 0.0041(8) C006 0.0262(10) 0.0373(12) 0.0300(11) -0.0052(9) -0.0041(9) 0.0026(9) C007 0.0334(12) 0.0355(12) 0.0297(12) -0.0060(9) -0.0059(9) -0.0017(9) C008 0.0267(11) 0.0386(12) 0.0279(11) -0.0057(9) -0.0018(8) 0.0046(9) C009 0.0258(10) 0.0380(12) 0.0287(11) -0.0051(9) -0.0069(8) 0.0017(8) C00A 0.0306(11) 0.0343(11) 0.0284(11) -0.0076(9) -0.0028(9) 0.0012(9) C00B 0.0316(12) 0.0354(12) 0.0368(13) -0.0058(10) -0.0052(10) 0.0037(9) C00C 0.0299(11) 0.0348(12) 0.0272(11) -0.0055(9) -0.0020(9) 0.0017(9) C00D 0.0280(11) 0.0385(12) 0.0297(11) -0.0043(9) -0.0024(9) 0.0025(9) C00E 0.0305(11) 0.0349(12) 0.0288(11) -0.0053(9) -0.0012(9) 0.0021(9) C00F 0.0299(11) 0.0385(12) 0.0341(12) -0.0044(10) -0.0046(9) 0.0007(9) C00G 0.0304(11) 0.0352(12) 0.0293(11) -0.0088(9) -0.0029(9) 0.0017(9) C00H 0.0281(11) 0.0384(12) 0.0364(12) -0.0082(10) -0.0030(9) 0.0006(9) C00I 0.0407(13) 0.0392(12) 0.0296(12) -0.0053(9) -0.0048(10) 0.0029(10) C00J 0.0370(13) 0.0408(13) 0.0362(13) 0.0011(10) -0.0056(10) -0.0036(10) C00K 0.0365(13) 0.0481(14) 0.0346(13) -0.0097(11) -0.0001(10) 0.0017(10) C00L 0.0343(12) 0.0371(12) 0.0342(12) -0.0060(10) -0.0026(10) 0.0005(9) C00M 0.0323(12) 0.0396(13) 0.0324(12) -0.0053(9) -0.0041(9) 0.0012(9) C00N 0.0297(11) 0.0365(12) 0.0296(11) -0.0049(9) -0.0031(9) 0.0027(9) C00O 0.0321(12) 0.0324(11) 0.0351(12) -0.0077(9) -0.0066(9) 0.0027(9) C00P 0.0363(13) 0.0545(15) 0.0306(12) -0.0018(11) -0.0017(10) -0.0033(11) C00Q 0.0275(11) 0.0500(14) 0.0328(12) -0.0121(10) -0.0075(9) 0.0042(10) C00R 0.0331(12) 0.0409(13) 0.0466(15) -0.0100(11) 0.0040(11) -0.0014(10) C00S 0.0441(14) 0.0368(13) 0.0376(13) -0.0059(10) -0.0060(11) 0.0051(10) C00T 0.0322(12) 0.0407(13) 0.0340(12) -0.0029(10) -0.0032(9) 0.0004(9) C00U 0.0354(13) 0.0530(15) 0.0493(16) -0.0199(12) -0.0114(12) 0.0093(11) C00V 0.0386(13) 0.0425(13) 0.0353(13) -0.0068(10) -0.0081(10) 0.0004(10) C00W 0.0342(12) 0.0407(13) 0.0359(13) 0.0001(10) -0.0044(10) 0.0044(10) C00X 0.0300(12) 0.0505(14) 0.0371(13) -0.0034(11) -0.0088(10) -0.0013(10) C00Y 0.0357(13) 0.0451(14) 0.0348(13) -0.0089(10) -0.0057(10) 0.0010(10) C00Z 0.0395(13) 0.0367(12) 0.0341(12) -0.0037(10) -0.0041(10) 0.0031(10) C010 0.0308(12) 0.0522(15) 0.0368(13) 0.0023(11) -0.0093(10) 0.0041(10) C011 0.0419(14) 0.0464(14) 0.0361(13) -0.0049(11) -0.0119(11) -0.0001(11) C012 0.0339(13) 0.0509(15) 0.0384(14) -0.0034(11) -0.0077(10) -0.0031(11) C013 0.0494(15) 0.0399(13) 0.0366(13) -0.0015(10) 0.0072(11) 0.0009(11) C014 0.0337(12) 0.0465(14) 0.0319(12) -0.0067(10) -0.0041(10) 0.0012(10) C015 0.0396(13) 0.0381(13) 0.0370(13) -0.0051(10) -0.0030(10) 0.0019(10) C016 0.0331(12) 0.0502(14) 0.0391(13) -0.0086(11) -0.0102(10) 0.0093(10) C017 0.0407(13) 0.0448(14) 0.0310(12) -0.0025(10) -0.0061(10) 0.0045(10) C018 0.0330(13) 0.0631(17) 0.0355(13) -0.0111(12) -0.0034(10) 0.0002(11) C019 0.0358(13) 0.0366(12) 0.0413(14) -0.0054(10) -0.0074(10) -0.0009(10) C01A 0.0452(15) 0.0416(14) 0.0462(15) 0.0019(11) -0.0009(12) -0.0003(11) C01B 0.0554(16) 0.0440(14) 0.0286(12) -0.0072(10) -0.0090(11) 0.0013(12) C01C 0.0412(14) 0.0375(13) 0.0407(14) -0.0010(10) 0.0043(11) -0.0008(10) C01D 0.0508(15) 0.0408(13) 0.0315(12) -0.0016(10) -0.0027(11) 0.0045(11) C01E 0.0339(13) 0.0416(13) 0.0463(15) -0.0032(11) 0.0012(11) -0.0041(10) C01F 0.0466(15) 0.0488(14) 0.0313(13) -0.0081(11) -0.0008(11) 0.0036(11) C01G 0.0517(16) 0.0394(14) 0.0476(16) -0.0111(11) -0.0099(12) 0.0032(11) C01H 0.0529(16) 0.0356(13) 0.0560(18) -0.0028(12) -0.0072(13) -0.0032(11) C01I 0.0473(15) 0.0528(16) 0.0392(14) -0.0075(12) -0.0173(12) 0.0007(12) C01J 0.0382(14) 0.0441(14) 0.0585(18) -0.0086(12) -0.0135(12) -0.0047(11) C01K 0.0315(14) 0.101(3) 0.0383(15) -0.0172(16) 0.0003(11) -0.0031(14) C01L 0.0432(16) 0.074(2) 0.068(2) -0.0399(17) -0.0156(15) 0.0237(15) C01M 0.0318(14) 0.109(3) 0.0535(18) -0.0421(19) -0.0065(13) 0.0167(16) C01N 0.0459(15) 0.0520(16) 0.0542(17) -0.0126(13) -0.0206(13) -0.0044(12) B01O 0.0271(12) 0.0338(13) 0.0292(12) -0.0062(10) -0.0041(10) 0.0032(9) B1 0.0297(12) 0.0371(13) 0.0289(13) -0.0042(10) -0.0058(10) 0.0041(10) C1_1 0.110(9) 0.153(9) 0.059(5) 0.007(6) 0.006(5) 0.022(8) C2_1 0.050(4) 0.088(4) 0.072(4) 0.012(4) -0.004(3) 0.006(4) C3_1 0.047(3) 0.075(4) 0.076(4) 0.006(4) 0.000(3) 0.002(3) C4_1 0.057(4) 0.078(4) 0.080(4) -0.011(4) 0.000(4) -0.006(3) C5_1 0.052(5) 0.081(4) 0.069(4) -0.025(3) 0.000(3) 0.002(4) C6_1 0.058(4) 0.066(4) 0.073(4) -0.023(4) 0.000(4) 0.003(4) C7_1 0.037(3) 0.061(4) 0.061(4) -0.002(4) 0.004(3) 0.009(3) C1_2 0.068(5) 0.132(6) 0.094(5) -0.037(5) -0.039(4) 0.036(5) C2_2 0.049(3) 0.076(3) 0.067(3) 0.003(3) -0.012(3) 0.015(3) C3_2 0.051(3) 0.073(3) 0.081(3) 0.010(3) -0.009(3) -0.003(3) C4_2 0.057(3) 0.072(3) 0.067(4) -0.002(3) 0.002(3) -0.006(3) C5_2 0.060(4) 0.076(3) 0.060(3) -0.020(3) -0.003(3) -0.003(3) C6_2 0.052(4) 0.066(3) 0.064(3) -0.019(3) 0.010(3) 0.005(3) C7_2 0.046(3) 0.055(3) 0.068(4) -0.010(3) -0.001(3) 0.013(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 '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 0 -1 0 0.0576 0 1 0 0.0743 -2 0 1 0.1667 -2 -1 1 0.1493 -2 -1 -1 0.1604 -1 2 -2 0.1177 1 -2 2 0.1072 1 2 1 0.0899 -1 -2 -1 0.1180 0 -2 1 0.0610 0 0 1 0.0492 0 0 -1 0.0409 -1 -1 2 0.0985 1 0 -2 0.0924 1 -1 -2 0.0852 1 1 0 0.0923 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 N003 Si01 C012 107.02(11) . . ? N003 Si01 C017 105.54(11) . . ? C012 Si01 C017 112.73(13) . . ? N003 Si01 C016 109.35(10) . . ? C012 Si01 C016 112.28(13) . . ? C017 Si01 C016 109.62(12) . . ? N004 N002 C005 125.32(18) . . ? N004 N002 B01O 115.93(18) . . ? C005 N002 B01O 117.83(17) . . ? N004 N003 B1 120.96(19) . . ? N004 N003 Si01 109.12(14) . . ? B1 N003 Si01 124.86(16) . . ? N002 N004 N003 117.76(19) . . ? C006 C005 N002 120.7(2) . . ? C006 C005 C00E 127.4(2) . . ? N002 C005 C00E 111.23(19) . . ? C005 C006 C00A 121.0(2) . . ? C005 C006 C007 123.3(2) . . ? C00A C006 C007 115.5(2) . . ? C014 C007 C00Y 118.9(2) . . ? C014 C007 C006 120.7(2) . . ? C00Y C007 C006 120.3(2) . . ? C00F C008 C00D 118.9(2) . . ? C00F C008 B01O 132.7(2) . . ? C00D C008 B01O 108.2(2) . . ? C00M C009 C00L 116.5(2) . . ? C00M C009 B01O 124.6(2) . . ? C00L C009 B01O 118.7(2) . . ? C00H C00A C00G 120.3(2) . . ? C00H C00A C006 124.1(2) . . ? C00G C00A C006 115.4(2) . . ? C015 C00B C00S 118.0(2) . . ? C015 C00B C00N 120.5(2) . . ? C00S C00B C00N 121.5(2) . . ? C00N C00C C00O 124.6(2) . . ? C00N C00C B01O 109.0(2) . . ? C00O C00C B01O 126.4(2) . . ? C00W C00D C008 121.1(2) . . ? C00W C00D C00N 128.2(2) . . ? C008 C00D C00N 110.7(2) . . ? C00T C00E C00I 118.8(2) . . ? C00T C00E C005 119.9(2) . . ? C00I C00E C005 121.3(2) . . ? C008 C00F C00X 120.6(2) . . ? C008 C00F H00F 119.7 . . ? C00X C00F H00F 119.7 . . ? C00Z C00G C00A 118.6(2) . . ? C00Z C00G B1 123.9(2) . . ? C00A C00G B1 117.5(2) . . ? C00R C00H C00A 119.8(2) . . ? C00R C00H H00H 120.1 . . ? C00A C00H H00H 120.1 . . ? C01D C00I C00E 120.0(2) . . ? C01D C00I H00I 120.0 . . ? C00E C00I H00I 120.0 . . ? C00P C00J C00M 120.7(2) . . ? C00P C00J H00J 119.7 . . ? C00M C00J H00J 119.7 . . ? C00P C00K C00L 119.9(2) . . ? C00P C00K H00K 120.0 . . ? C00L C00K H00K 120.0 . . ? C00K C00L C009 122.2(2) . . ? C00K C00L H00L 118.9 . . ? C009 C00L H00L 118.9 . . ? C00J C00M C009 121.5(2) . . ? C00J C00M H00M 119.2 . . ? C009 C00M H00M 119.2 . . ? C00C C00N C00D 111.9(2) . . ? C00C C00N C00B 126.7(2) . . ? C00D C00N C00B 121.4(2) . . ? C00V C00O C019 117.5(2) . . ? C00V C00O C00C 120.2(2) . . ? C019 C00O C00C 122.3(2) . . ? C00K C00P C00J 119.2(2) . . ? C00K C00P H00P 120.4 . . ? C00J C00P H00P 120.4 . . ? C00U C00Q C018 118.1(2) . . ? C00U C00Q B1 122.6(2) . . ? C018 C00Q B1 119.2(2) . . ? C01C C00R C00H 120.2(2) . . ? C01C C00R H00R 119.9 . . ? C00H C00R H00R 119.9 . . ? C01G C00S C00B 121.0(3) . . ? C01G C00S H00S 119.5 . . ? C00B C00S H00S 119.5 . . ? C01E C00T C00E 120.9(2) . . ? C01E C00T H00T 119.5 . . ? C00E C00T H00T 119.5 . . ? C01L C00U C00Q 120.6(3) . . ? C01L C00U H00U 119.7 . . ? C00Q C00U H00U 119.7 . . ? C01I C00V C00O 121.1(3) . . ? C01I C00V H00V 119.5 . . ? C00O C00V H00V 119.5 . . ? C010 C00W C00D 118.9(2) . . ? C010 C00W H00W 120.5 . . ? C00D C00W H00W 120.5 . . ? C010 C00X C00F 119.8(2) . . ? C010 C00X H00X 120.1 . . ? C00F C00X H00X 120.1 . . ? C011 C00Y C007 120.8(2) . . ? C011 C00Y H00Y 119.6 . . ? C007 C00Y H00Y 119.6 . . ? C01C C00Z C00G 120.5(2) . . ? C01C C00Z H00Z 119.7 . . ? C00G C00Z H00Z 119.7 . . ? C00X C010 C00W 120.7(2) . . ? C00X C010 H010 119.7 . . ? C00W C010 H010 119.7 . . ? C00Y C011 C01B 119.9(3) . . ? C00Y C011 H011 120.0 . . ? C01B C011 H011 120.0 . . ? Si01 C012 H01A 109.5 . . ? Si01 C012 H01B 109.5 . . ? H01A C012 H01B 109.5 . . ? Si01 C012 H01C 109.5 . . ? H01A C012 H01C 109.5 . . ? H01B C012 H01C 109.5 . . ? C01D C013 C01E 119.8(2) . . ? C01D C013 H013 120.1 . . ? C01E C013 H013 120.1 . . ? C01F C014 C007 119.9(2) . . ? C01F C014 H014 120.0 . . ? C007 C014 H014 120.0 . . ? C01A C015 C00B 121.2(3) . . ? C01A C015 H015 119.4 . . ? C00B C015 H015 119.4 . . ? Si01 C016 H01D 109.5 . . ? Si01 C016 H01E 109.5 . . ? H01D C016 H01E 109.5 . . ? Si01 C016 H01F 109.5 . . ? H01D C016 H01F 109.5 . . ? H01E C016 H01F 109.5 . . ? Si01 C017 H01G 109.5 . . ? Si01 C017 H01H 109.5 . . ? H01G C017 H01H 109.5 . . ? Si01 C017 H01I 109.5 . . ? H01G C017 H01I 109.5 . . ? H01H C017 H01I 109.5 . . ? C01K C018 C00Q 120.8(3) . . ? C01K C018 H018 119.6 . . ? C00Q C018 H018 119.6 . . ? C01J C019 C00O 120.8(3) . . ? C01J C019 H019 119.6 . . ? C00O C019 H019 119.6 . . ? C01H C01A C015 119.7(3) . . ? C01H C01A H01J 120.1 . . ? C015 C01A H01J 120.1 . . ? C01F C01B C011 119.7(2) . . ? C01F C01B H01K 120.1 . . ? C011 C01B H01K 120.1 . . ? C00R C01C C00Z 120.6(2) . . ? C00R C01C H01L 119.7 . . ? C00Z C01C H01L 119.7 . . ? C00I C01D C013 120.7(3) . . ? C00I C01D H01M 119.6 . . ? C013 C01D H01M 119.6 . . ? C013 C01E C00T 119.7(3) . . ? C013 C01E H01N 120.1 . . ? C00T C01E H01N 120.1 . . ? C01B C01F C014 120.6(3) . . ? C01B C01F H01O 119.7 . . ? C014 C01F H01O 119.7 . . ? C01H C01G C00S 120.1(3) . . ? C01H C01G H01P 120.0 . . ? C00S C01G H01P 120.0 . . ? C01G C01H C01A 120.0(3) . . ? C01G C01H H01Q 120.0 . . ? C01A C01H H01Q 120.0 . . ? C01N C01I C00V 120.5(3) . . ? C01N C01I H01R 119.7 . . ? C00V C01I H01R 119.7 . . ? C01N C01J C019 120.2(3) . . ? C01N C01J H01S 119.9 . . ? C019 C01J H01S 119.9 . . ? C01M C01K C018 120.0(3) . . ? C01M C01K H01T 120.0 . . ? C018 C01K H01T 120.0 . . ? C01M C01L C00U 119.9(3) . . ? C01M C01L H01U 120.1 . . ? C00U C01L H01U 120.1 . . ? C01L C01M C01K 120.5(3) . . ? C01L C01M H01V 119.7 . . ? C01K C01M H01V 119.7 . . ? C01I C01N C01J 119.8(3) . . ? C01I C01N H01W 120.1 . . ? C01J C01N H01W 120.1 . . ? C008 B01O C009 110.97(19) . . ? C008 B01O N002 110.83(18) . . ? C009 B01O N002 110.42(19) . . ? C008 B01O C00C 99.88(18) . . ? C009 B01O C00C 116.6(2) . . ? N002 B01O C00C 107.62(18) . . ? N003 B1 C00Q 119.0(2) . . ? N003 B1 C00G 118.4(2) . . ? C00Q B1 C00G 122.5(2) . . ? C2_1 C1_1 H1A_1 109.5 . . ? C2_1 C1_1 H1B_1 109.5 . . ? H1A_1 C1_1 H1B_1 109.5 . . ? C2_1 C1_1 H1C_1 109.5 . . ? H1A_1 C1_1 H1C_1 109.5 . . ? H1B_1 C1_1 H1C_1 109.5 . . ? C3_1 C2_1 C7_1 120.0 . . ? C3_1 C2_1 C1_1 121.8(10) . . ? C7_1 C2_1 C1_1 118.0(10) . . ? C2_1 C3_1 C4_1 120.0 . . ? C2_1 C3_1 H3_1 120.0 . . ? C4_1 C3_1 H3_1 120.0 . . ? C3_1 C4_1 C5_1 120.0 . . ? C3_1 C4_1 H4_1 120.0 . . ? C5_1 C4_1 H4_1 120.0 . . ? C6_1 C5_1 C4_1 120.0 . . ? C6_1 C5_1 H5_1 120.0 . . ? C4_1 C5_1 H5_1 120.0 . . ? C7_1 C6_1 C5_1 120.0 . . ? C7_1 C6_1 H6_1 120.0 . . ? C5_1 C6_1 H6_1 120.0 . . ? C6_1 C7_1 C2_1 120.0 . . ? C6_1 C7_1 H7_1 120.0 . . ? C2_1 C7_1 H7_1 120.0 . . ? C2_2 C1_2 H1A_2 109.5 . . ? C2_2 C1_2 H1B_2 109.5 . . ? H1A_2 C1_2 H1B_2 109.5 . . ? C2_2 C1_2 H1C_2 109.5 . . ? H1A_2 C1_2 H1C_2 109.5 . . ? H1B_2 C1_2 H1C_2 109.5 . . ? C3_2 C2_2 C7_2 120.0 . . ? C3_2 C2_2 C1_2 118.1(7) . . ? C7_2 C2_2 C1_2 121.9(7) . . ? C4_2 C3_2 C2_2 120.0 . . ? C4_2 C3_2 H3_2 120.0 . . ? C2_2 C3_2 H3_2 120.0 . . ? C5_2 C4_2 C3_2 120.0 . . ? C5_2 C4_2 H4_2 120.0 . . ? C3_2 C4_2 H4_2 120.0 . . ? C4_2 C5_2 C6_2 120.0 . . ? C4_2 C5_2 H5_2 120.0 . . ? C6_2 C5_2 H5_2 120.0 . . ? C7_2 C6_2 C5_2 120.0 . . ? C7_2 C6_2 H6_2 120.0 . . ? C5_2 C6_2 H6_2 120.0 . . ? C6_2 C7_2 C2_2 120.0 . . ? C6_2 C7_2 H7_2 120.0 . . ? C2_2 C7_2 H7_2 120.0 . . ? 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 Si01 N003 1.834(2) . ? Si01 C012 1.835(3) . ? Si01 C017 1.848(3) . ? Si01 C016 1.858(3) . ? N002 N004 1.267(3) . ? N002 C005 1.477(3) . ? N002 B01O 1.632(3) . ? N003 N004 1.367(3) . ? N003 B1 1.453(3) . ? C005 C006 1.343(3) . ? C005 C00E 1.489(3) . ? C006 C00A 1.481(3) . ? C006 C007 1.496(3) . ? C007 C014 1.393(3) . ? C007 C00Y 1.396(3) . ? C008 C00F 1.382(3) . ? C008 C00D 1.407(3) . ? C008 B01O 1.616(3) . ? C009 C00M 1.397(3) . ? C009 C00L 1.404(3) . ? C009 B01O 1.620(3) . ? C00A C00H 1.400(3) . ? C00A C00G 1.401(3) . ? C00B C015 1.395(4) . ? C00B C00S 1.395(4) . ? C00B C00N 1.481(3) . ? C00C C00N 1.362(3) . ? C00C C00O 1.475(3) . ? C00C B01O 1.634(3) . ? C00D C00W 1.392(3) . ? C00D C00N 1.480(3) . ? C00E C00T 1.391(3) . ? C00E C00I 1.401(3) . ? C00F C00X 1.400(3) . ? C00F H00F 0.9500 . ? C00G C00Z 1.400(3) . ? C00G B1 1.575(4) . ? C00H C00R 1.385(4) . ? C00H H00H 0.9500 . ? C00I C01D 1.382(4) . ? C00I H00I 0.9500 . ? C00J C00P 1.384(4) . ? C00J C00M 1.392(4) . ? C00J H00J 0.9500 . ? C00K C00P 1.383(4) . ? C00K C00L 1.390(4) . ? C00K H00K 0.9500 . ? C00L H00L 0.9500 . ? C00M H00M 0.9500 . ? C00O C00V 1.396(4) . ? C00O C019 1.408(3) . ? C00P H00P 0.9500 . ? C00Q C00U 1.397(4) . ? C00Q C018 1.401(4) . ? C00Q B1 1.557(3) . ? C00R C01C 1.378(4) . ? C00R H00R 0.9500 . ? C00S C01G 1.387(4) . ? C00S H00S 0.9500 . ? C00T C01E 1.390(4) . ? C00T H00T 0.9500 . ? C00U C01L 1.393(4) . ? C00U H00U 0.9500 . ? C00V C01I 1.386(4) . ? C00V H00V 0.9500 . ? C00W C010 1.392(4) . ? C00W H00W 0.9500 . ? C00X C010 1.388(4) . ? C00X H00X 0.9500 . ? C00Y C011 1.377(4) . ? C00Y H00Y 0.9500 . ? C00Z C01C 1.384(4) . ? C00Z H00Z 0.9500 . ? C010 H010 0.9500 . ? C011 C01B 1.388(4) . ? C011 H011 0.9500 . ? C012 H01A 0.9800 . ? C012 H01B 0.9800 . ? C012 H01C 0.9800 . ? C013 C01D 1.385(4) . ? C013 C01E 1.385(4) . ? C013 H013 0.9500 . ? C014 C01F 1.387(4) . ? C014 H014 0.9500 . ? C015 C01A 1.387(4) . ? C015 H015 0.9500 . ? C016 H01D 0.9800 . ? C016 H01E 0.9800 . ? C016 H01F 0.9800 . ? C017 H01G 0.9800 . ? C017 H01H 0.9800 . ? C017 H01I 0.9800 . ? C018 C01K 1.385(4) . ? C018 H018 0.9500 . ? C019 C01J 1.390(4) . ? C019 H019 0.9500 . ? C01A C01H 1.387(4) . ? C01A H01J 0.9500 . ? C01B C01F 1.380(4) . ? C01B H01K 0.9500 . ? C01C H01L 0.9500 . ? C01D H01M 0.9500 . ? C01E H01N 0.9500 . ? C01F H01O 0.9500 . ? C01G C01H 1.379(4) . ? C01G H01P 0.9500 . ? C01H H01Q 0.9500 . ? C01I C01N 1.377(4) . ? C01I H01R 0.9500 . ? C01J C01N 1.379(4) . ? C01J H01S 0.9500 . ? C01K C01M 1.376(5) . ? C01K H01T 0.9500 . ? C01L C01M 1.376(5) . ? C01L H01U 0.9500 . ? C01M H01V 0.9500 . ? C01N H01W 0.9500 . ? C1_1 C2_1 1.454(16) . ? C1_1 H1A_1 0.9800 . ? C1_1 H1B_1 0.9800 . ? C1_1 H1C_1 0.9800 . ? C2_1 C3_1 1.3900 . ? C2_1 C7_1 1.3900 . ? C3_1 C4_1 1.3900 . ? C3_1 H3_1 0.9500 . ? C4_1 C5_1 1.3900 . ? C4_1 H4_1 0.9500 . ? C5_1 C6_1 1.3900 . ? C5_1 H5_1 0.9500 . ? C6_1 C7_1 1.3900 . ? C6_1 H6_1 0.9500 . ? C7_1 H7_1 0.9500 . ? C1_2 C2_2 1.433(10) . ? C1_2 H1A_2 0.9800 . ? C1_2 H1B_2 0.9800 . ? C1_2 H1C_2 0.9800 . ? C2_2 C3_2 1.3900 . ? C2_2 C7_2 1.3900 . ? C3_2 C4_2 1.3900 . ? C3_2 H3_2 0.9500 . ? C4_2 C5_2 1.3900 . ? C4_2 H4_2 0.9500 . ? C5_2 C6_2 1.3900 . ? C5_2 H5_2 0.9500 . ? C6_2 C7_2 1.3900 . ? C6_2 H6_2 0.9500 . ? C7_2 H7_2 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C012 Si01 N003 N004 -76.73(17) . . . . ? C017 Si01 N003 N004 43.57(17) . . . . ? C016 Si01 N003 N004 161.42(16) . . . . ? C012 Si01 N003 B1 128.5(2) . . . . ? C017 Si01 N003 B1 -111.2(2) . . . . ? C016 Si01 N003 B1 6.6(2) . . . . ? C005 N002 N004 N003 -6.6(3) . . . . ? B01O N002 N004 N003 -175.39(18) . . . . ? B1 N003 N004 N002 -46.2(3) . . . . ? Si01 N003 N004 N002 157.85(16) . . . . ? N004 N002 C005 C006 89.9(3) . . . . ? B01O N002 C005 C006 -101.6(2) . . . . ? N004 N002 C005 C00E -99.0(2) . . . . ? B01O N002 C005 C00E 69.5(2) . . . . ? N002 C005 C006 C00A -15.4(3) . . . . ? C00E C005 C006 C00A 175.0(2) . . . . ? N002 C005 C006 C007 170.0(2) . . . . ? C00E C005 C006 C007 0.5(4) . . . . ? C005 C006 C007 C014 79.6(3) . . . . ? C00A C006 C007 C014 -95.2(3) . . . . ? C005 C006 C007 C00Y -105.4(3) . . . . ? C00A C006 C007 C00Y 79.8(3) . . . . ? C005 C006 C00A C00H 129.0(3) . . . . ? C007 C006 C00A C00H -56.0(3) . . . . ? C005 C006 C00A C00G -55.3(3) . . . . ? C007 C006 C00A C00G 119.7(2) . . . . ? C00F C008 C00D C00W 0.6(3) . . . . ? B01O C008 C00D C00W -174.5(2) . . . . ? C00F C008 C00D C00N 179.7(2) . . . . ? B01O C008 C00D C00N 4.6(3) . . . . ? C006 C005 C00E C00T -140.9(3) . . . . ? N002 C005 C00E C00T 48.7(3) . . . . ? C006 C005 C00E C00I 40.0(4) . . . . ? N002 C005 C00E C00I -130.4(2) . . . . ? C00D C008 C00F C00X 0.9(4) . . . . ? B01O C008 C00F C00X 174.5(2) . . . . ? C00H C00A C00G C00Z -1.5(3) . . . . ? C006 C00A C00G C00Z -177.3(2) . . . . ? C00H C00A C00G B1 175.4(2) . . . . ? C006 C00A C00G B1 -0.5(3) . . . . ? C00G C00A C00H C00R 1.3(4) . . . . ? C006 C00A C00H C00R 176.8(2) . . . . ? C00T C00E C00I C01D 2.2(4) . . . . ? C005 C00E C00I C01D -178.7(2) . . . . ? C00P C00K C00L C009 0.1(4) . . . . ? C00M C009 C00L C00K 0.3(4) . . . . ? B01O C009 C00L C00K 175.1(2) . . . . ? C00P C00J C00M C009 0.0(4) . . . . ? C00L C009 C00M C00J -0.3(3) . . . . ? B01O C009 C00M C00J -174.8(2) . . . . ? C00O C00C C00N C00D 176.7(2) . . . . ? B01O C00C C00N C00D -2.6(3) . . . . ? C00O C00C C00N C00B -4.3(4) . . . . ? B01O C00C C00N C00B 176.4(2) . . . . ? C00W C00D C00N C00C 177.7(2) . . . . ? C008 C00D C00N C00C -1.3(3) . . . . ? C00W C00D C00N C00B -1.4(4) . . . . ? C008 C00D C00N C00B 179.6(2) . . . . ? C015 C00B C00N C00C 129.6(3) . . . . ? C00S C00B C00N C00C -49.6(4) . . . . ? C015 C00B C00N C00D -51.5(3) . . . . ? C00S C00B C00N C00D 129.3(3) . . . . ? C00N C00C C00O C00V 140.1(3) . . . . ? B01O C00C C00O C00V -40.7(3) . . . . ? C00N C00C C00O C019 -41.0(4) . . . . ? B01O C00C C00O C019 138.2(2) . . . . ? C00L C00K C00P C00J -0.5(4) . . . . ? C00M C00J C00P C00K 0.4(4) . . . . ? C00A C00H C00R C01C -0.6(4) . . . . ? C015 C00B C00S C01G -0.4(4) . . . . ? C00N C00B C00S C01G 178.9(2) . . . . ? C00I C00E C00T C01E -1.5(4) . . . . ? C005 C00E C00T C01E 179.4(2) . . . . ? C018 C00Q C00U C01L 2.0(4) . . . . ? B1 C00Q C00U C01L 178.9(3) . . . . ? C019 C00O C00V C01I 1.9(4) . . . . ? C00C C00O C00V C01I -179.1(2) . . . . ? C008 C00D C00W C010 -2.0(4) . . . . ? C00N C00D C00W C010 179.1(2) . . . . ? C008 C00F C00X C010 -0.9(4) . . . . ? C014 C007 C00Y C011 1.7(4) . . . . ? C006 C007 C00Y C011 -173.4(2) . . . . ? C00A C00G C00Z C01C 0.9(4) . . . . ? B1 C00G C00Z C01C -175.7(2) . . . . ? C00F C00X C010 C00W -0.5(4) . . . . ? C00D C00W C010 C00X 2.0(4) . . . . ? C007 C00Y C011 C01B -0.4(4) . . . . ? C00Y C007 C014 C01F -0.9(4) . . . . ? C006 C007 C014 C01F 174.2(2) . . . . ? C00S C00B C015 C01A -0.2(4) . . . . ? C00N C00B C015 C01A -179.4(2) . . . . ? C00U C00Q C018 C01K 1.4(4) . . . . ? B1 C00Q C018 C01K -175.7(2) . . . . ? C00V C00O C019 C01J -1.0(4) . . . . ? C00C C00O C019 C01J -180.0(2) . . . . ? C00B C015 C01A C01H 0.3(4) . . . . ? C00Y C011 C01B C01F -1.8(4) . . . . ? C00H C00R C01C C00Z 0.0(4) . . . . ? C00G C00Z C01C C00R -0.2(4) . . . . ? C00E C00I C01D C013 -1.5(4) . . . . ? C01E C013 C01D C00I -0.1(4) . . . . ? C01D C013 C01E C00T 0.8(4) . . . . ? C00E C00T C01E C013 0.0(4) . . . . ? C011 C01B C01F C014 2.6(4) . . . . ? C007 C014 C01F C01B -1.3(4) . . . . ? C00B C00S C01G C01H 0.9(4) . . . . ? C00S C01G C01H C01A -0.7(5) . . . . ? C015 C01A C01H C01G 0.2(5) . . . . ? C00O C00V C01I C01N -1.3(4) . . . . ? C00O C019 C01J C01N -0.5(4) . . . . ? C00Q C018 C01K C01M -3.1(4) . . . . ? C00Q C00U C01L C01M -3.7(4) . . . . ? C00U C01L C01M C01K 1.9(5) . . . . ? C018 C01K C01M C01L 1.4(5) . . . . ? C00V C01I C01N C01J -0.2(5) . . . . ? C019 C01J C01N C01I 1.1(4) . . . . ? C00F C008 B01O C009 -56.1(3) . . . . ? C00D C008 B01O C009 118.1(2) . . . . ? C00F C008 B01O N002 67.0(3) . . . . ? C00D C008 B01O N002 -118.8(2) . . . . ? C00F C008 B01O C00C -179.7(2) . . . . ? C00D C008 B01O C00C -5.6(2) . . . . ? C00M C009 B01O C008 97.7(3) . . . . ? C00L C009 B01O C008 -76.7(3) . . . . ? C00M C009 B01O N002 -25.6(3) . . . . ? C00L C009 B01O N002 160.0(2) . . . . ? C00M C009 B01O C00C -148.8(2) . . . . ? C00L C009 B01O C00C 36.8(3) . . . . ? N004 N002 B01O C008 -177.16(19) . . . . ? C005 N002 B01O C008 13.2(3) . . . . ? N004 N002 B01O C009 -53.8(2) . . . . ? C005 N002 B01O C009 136.6(2) . . . . ? N004 N002 B01O C00C 74.6(2) . . . . ? C005 N002 B01O C00C -95.0(2) . . . . ? C00N C00C B01O C008 4.9(2) . . . . ? C00O C00C B01O C008 -174.4(2) . . . . ? C00N C00C B01O C009 -114.7(2) . . . . ? C00O C00C B01O C009 66.0(3) . . . . ? C00N C00C B01O N002 120.6(2) . . . . ? C00O C00C B01O N002 -58.6(3) . . . . ? N004 N003 B1 C00Q 157.0(2) . . . . ? Si01 N003 B1 C00Q -51.0(3) . . . . ? N004 N003 B1 C00G -27.4(3) . . . . ? Si01 N003 B1 C00G 124.7(2) . . . . ? C00U C00Q B1 N003 140.7(2) . . . . ? C018 C00Q B1 N003 -42.4(3) . . . . ? C00U C00Q B1 C00G -34.8(4) . . . . ? C018 C00Q B1 C00G 142.1(2) . . . . ? C00Z C00G B1 N003 -95.9(3) . . . . ? C00A C00G B1 N003 87.5(3) . . . . ? C00Z C00G B1 C00Q 79.7(3) . . . . ? C00A C00G B1 C00Q -97.0(3) . . . . ? C7_1 C2_1 C3_1 C4_1 0.0 . . . . ? C1_1 C2_1 C3_1 C4_1 -173.9(15) . . . . ? C2_1 C3_1 C4_1 C5_1 0.0 . . . . ? C3_1 C4_1 C5_1 C6_1 0.0 . . . . ? C4_1 C5_1 C6_1 C7_1 0.0 . . . . ? C5_1 C6_1 C7_1 C2_1 0.0 . . . . ? C3_1 C2_1 C7_1 C6_1 0.0 . . . . ? C1_1 C2_1 C7_1 C6_1 174.1(14) . . . . ? C7_2 C2_2 C3_2 C4_2 0.0 . . . . ? C1_2 C2_2 C3_2 C4_2 178.5(9) . . . . ? C2_2 C3_2 C4_2 C5_2 0.0 . . . . ? C3_2 C4_2 C5_2 C6_2 0.0 . . . . ? C4_2 C5_2 C6_2 C7_2 0.0 . . . . ? C5_2 C6_2 C7_2 C2_2 0.0 . . . . ? C3_2 C2_2 C7_2 C6_2 0.0 . . . . ? C1_2 C2_2 C7_2 C6_2 -178.4(9) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.4458 50985 1688 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.5542 49775 1688 nmt 1.0021 0.0187 -0.0126 -0.0379 1.0019 -0.0935 0.0242 0.1094 0.9852