#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:56:54 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294490 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572079.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_1572079 loop_ _publ_author_name 'Wieprecht, Nele' 'Krummenacher, Ivo' 'Wüst, Leonie' 'Michel, Maximilian' 'Fuchs, Sonja' 'Nees, Samuel' 'Härterich, Marcel' 'Braunschweig, Holger' _publ_section_title ; The forgotten borole: synthesis, properties and reactivity of a 1-boraindene. ; _journal_issue 31 _journal_name_full 'Chemical science' _journal_page_first 12496 _journal_page_last 12501 _journal_paper_doi 10.1039/d4sc03817g _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C55 H47 B2 N3 Si, C6 H6' _chemical_formula_sum 'C61 H53 B2 N3 Si' _chemical_formula_weight 877.77 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method 'CIF-fill 1.2y (K.Radacki, 2005-22)' _audit_update_record ; 2024-06-05 deposited with the CCDC. 2024-07-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.8290(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.45630(10) _cell_length_b 30.1996(2) _cell_length_c 11.78090(10) _cell_measurement_reflns_used 78361 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 75.1890 _cell_measurement_theta_min 2.9230 _cell_volume 4742.84(6) _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 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector HPA _diffrn_detector_area_resol_mean 10.0 _diffrn_detector_type 'HyPix Arc150' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.993 _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 60.00 85.00 0.50 0.05 -- 46.00 52.00-101.72 50 2 \w 101.00 127.00 0.50 0.05 -- 85.25 49.00-133.35 52 3 \w 109.00 135.00 0.50 0.05 -- 85.25 45.00-154.89 52 4 \w 105.00 131.00 0.50 0.05 -- 85.25 58.00 -84.27 52 5 \w 98.00 123.00 0.50 0.05 -- 85.25 44.00-160.01 50 6 \w 98.00 129.00 0.50 0.05 -- 82.00 46.00 35.26 62 7 \w 104.00 136.00 0.50 0.05 -- 85.25 32.00 43.13 64 8 \w 97.00 122.00 0.50 0.05 -- 85.25 56.00 118.05 50 9 \w 98.00 123.00 0.50 0.05 -- 85.25 41.00 151.31 50 10 \w 103.00 131.00 0.50 0.05 -- 85.25 35.00 175.61 56 11 \w 78.00 126.00 0.50 0.05 -- 85.25 17.00 164.41 96 12 \w 75.00 132.00 0.50 0.05 -- 85.25 20.00 131.65 114 13 \w 34.00 59.00 0.50 0.05 -- 22.00 59.00 90.91 50 14 \w 75.00 105.00 0.50 0.05 -- 85.25 11.00 10.20 60 15 \w 91.00 135.00 0.50 0.05 -- 85.25 23.00 10.56 88 16 \w 103.00 128.00 0.50 0.05 -- 85.25 114.00 34.46 50 17 \w 102.00 133.00 0.50 0.05 -- 85.25 127.00 92.96 62 18 \w 97.00 126.00 0.50 0.05 -- 85.25 125.00 124.14 58 19 \w 93.00 120.00 0.50 0.05 -- 85.25 138.00-166.97 54 20 \w 91.00 124.00 0.50 0.05 -- 85.25 136.00-134.76 66 21 \w 100.00 133.00 0.50 0.05 -- 85.25 119.00 -83.08 66 22 \w 47.00 76.00 0.50 0.05 -- 85.25 -77.00 17.53 58 23 \w 52.00 97.00 0.50 0.05 -- 85.25-137.00 149.76 90 24 \w 66.00 92.00 0.50 0.05 -- 85.25-136.00 72.03 52 25 \w 38.00 69.00 0.50 0.05 -- 85.25-132.00 -48.84 62 26 \w 39.00 64.00 0.50 0.05 -- 85.25-137.00 -62.25 50 27 \w 81.00 107.00 0.50 0.05 -- 85.25-137.00 -62.25 52 28 \w 78.00 103.00 0.50 0.05 -- 85.25-132.00-155.93 50 29 \w 71.00 101.00 0.50 0.05 -- 85.25-132.00-168.65 60 30 \w 41.00 67.00 0.50 0.05 -- 85.25-132.00-168.65 52 31 \w 41.00 86.00 0.50 0.05 -- 85.25-134.00-179.75 90 32 \w 37.00 65.00 0.50 0.05 -- 85.25-126.00-125.25 56 33 \w 35.00 61.00 0.50 0.05 -- 71.30-117.00-147.00 52 34 \w 70.00 95.00 0.50 0.05 -- 71.30-117.00-147.00 50 35 \w 49.00 95.00 0.50 0.05 -- 82.31-117.00-147.00 92 36 \w 15.00 79.00 0.50 0.05 -- 58.61-117.00-147.00 128 37 \w 42.00 68.00 0.50 0.05 -- 85.25-116.00 -37.47 52 38 \w 72.00 97.00 0.50 0.05 -- 85.25-116.00 -37.47 50 39 \w 55.00 81.00 0.50 0.05 -- 85.25-119.00 15.37 52 40 \w 52.00 80.00 0.50 0.05 -- 58.61-126.00 30.00 56 41 \w 36.00 62.00 0.50 0.05 -- 82.31-112.00 -30.00 52 42 \w 72.00 97.00 0.50 0.05 -- 82.31-112.00 60.00 50 43 \w 70.00 96.00 0.50 0.05 -- 82.31-112.00 120.00 52 44 \w 72.00 97.00 0.50 0.05 -- 82.31-112.00 150.00 50 45 \w 42.00 68.00 0.50 0.05 -- 85.25-130.00 149.70 52 46 \w 35.00 60.00 0.50 0.05 -- 82.31-112.00 120.00 50 47 \w 38.00 64.00 0.50 0.05 -- 82.31-112.00 150.00 52 48 \w 72.00 97.00 0.50 0.05 -- 82.31-112.00 -60.00 50 49 \w 49.00 97.00 0.50 0.05 -- 82.31-112.00 -90.00 96 50 \w 70.00 95.00 0.50 0.05 -- 82.31-112.00-180.00 50 51 \w 41.00 97.00 0.50 0.05 -- 82.31-112.00-120.00 112 52 \w 38.00 94.00 0.50 0.05 -- 85.25-112.00 19.78 112 53 \w 41.00 95.00 0.50 0.05 -- 85.25-110.00 100.84 108 54 \w 40.00 94.00 0.50 0.05 -- 85.25-107.00 70.12 108 55 \w 47.00 93.00 0.50 0.05 -- 85.25-101.00 23.00 92 56 \w 42.00 95.00 0.50 0.05 -- 85.25-108.00 -18.46 106 57 \w 42.00 94.00 0.50 0.05 -- 85.25-102.00 -39.57 104 58 \w 42.00 94.00 0.50 0.05 -- 85.25 -99.00 -62.63 104 59 \w 40.00 65.00 0.50 0.05 -- 82.31 -95.00-120.00 50 60 \w 43.00 69.00 0.50 0.05 -- 85.25-103.00 -87.67 52 61 \w 47.00 73.00 0.50 0.05 -- 85.25 -95.00-155.69 52 62 \w 43.00 83.00 0.50 0.05 -- 85.25 -93.00-106.33 80 63 \w 69.00 94.00 0.50 0.05 -- 85.25 -99.00 -23.95 50 64 \w 19.00 51.00 0.50 0.05 -- 58.61 -95.00 30.00 64 65 \w 51.00 89.00 0.50 0.05 -- 85.25 -91.00 169.61 76 66 \w 56.00 94.00 0.50 0.05 -- 85.25 -99.00 110.53 76 67 \w 51.00 87.00 0.50 0.05 -- 85.25 -91.00 120.75 72 68 \w 46.00 71.00 0.50 0.05 -- 85.25 -83.00 -21.59 50 69 \w 46.00 71.00 0.50 0.05 -- 85.25 -77.00 -57.38 50 70 \w 44.00 89.00 0.50 0.05 -- 85.25 -90.00-165.09 90 71 \w 55.00 81.00 0.50 0.05 -- 85.25 -90.00 -92.03 52 72 \w -127.00 -93.00 0.50 0.05 -- -79.50 -50.00 -29.16 68 73 \w -118.00 -84.00 0.50 0.05 -- -70.00 -54.00-110.74 68 74 \w -124.00 -98.00 0.50 0.05 -- -79.50 -64.00 47.28 52 75 \w -118.00 -92.00 0.50 0.05 -- -74.00 -56.00 134.31 52 76 \w -118.00 -92.00 0.50 0.05 -- -79.50 -54.00 109.94 52 77 \w -97.00 -71.00 0.50 0.05 -- -58.00 -51.00 20.51 52 78 \w -91.00 -64.00 0.50 0.05 -- -46.00 -50.00 53.52 54 79 \w -124.00 -99.00 0.50 0.05 -- -79.50 -65.00 80.34 50 80 \w -101.00 -70.00 0.50 0.05 -- -54.00 -52.00 -12.19 62 81 \w -128.00 -93.00 0.50 0.05 -- -79.50 -50.00-157.30 70 82 \w -128.00-103.00 0.50 0.05 -- -79.50-117.00 -95.27 50 83 \w -122.00 -96.00 0.50 0.05 -- -79.50-120.00 -68.29 52 84 \w -60.00 -31.00 0.50 0.05 -- -79.50 120.00 177.18 58 85 \w -84.00 -39.00 0.50 0.05 -- -79.50 103.00 38.65 90 86 \w -96.00 -66.00 0.50 0.05 -- -76.37 117.00 -59.00 60 87 \w -82.00 -57.00 0.50 0.05 -- -69.72 117.00 -59.00 50 88 \w -57.00 -22.00 0.50 0.05 -- -60.19 117.00 -59.00 70 89 \w -97.00 -31.00 0.50 0.05 -- -79.50 113.00-117.03 132 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-R' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_unetI/netI 0.0163 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 117141 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.252 _diffrn_reflns_theta_min 2.927 _diffrn_source 'rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R X-ray Source' _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021) 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 'clear pale colourless' _exptl_crystal_density_diffrn 1.229 _exptl_crystal_description block _exptl_crystal_F_000 1856 _exptl_crystal_size_max 0.525 _exptl_crystal_size_mid 0.345 _exptl_crystal_size_min 0.251 _refine_diff_density_max 0.707 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 607 _refine_ls_number_reflns 9732 _refine_ls_number_restraints 72 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0442 _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^)+(0.0585P)^2^+3.1816P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1159 _refine_ls_wR_factor_ref 0.1173 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9162 _reflns_number_total 9732 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03817g2.cif _cod_data_source_block 4 _cod_depositor_comments 'Adding full bibliography for 1572071--1572079.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1572079 _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 0.687 _shelx_estimated_absorpt_t_max 0.831 _shelx_res_file ; TITL SoFu080_NeWi_a.res in P2(1)/c SoFu080_NeWi_a.res created by SHELXL-2018/3 at 09:45:08 on 08-Mar-2022 REM Old TITL SoFu080_NeWi in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.117, Rweak 0.009, Alpha 0.030 REM 1.993 for 205 systematic absences, Orientation as input REM Formula found by SHELXT: C63 N3 Si CELL 1.54184 13.4563 30.1996 11.7809 90.000 97.829 90.000 ZERR 4.000 0.0001 0.0002 0.0001 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H B N SI UNIT 244.00 212.00 8.00 12.00 4.00 TEMP -173 SIZE 0.25 0.34 0.53 L.S. 10 BOND LIST 4 acta FMAP 2 PLAN 20 WGHT 0.058500 3.181600 FVAR 0.35089 B1 3 0.481232 0.352637 0.277643 11.00000 0.01506 0.01873 = 0.01452 0.00081 0.00100 0.00030 B2 3 0.694867 0.393434 0.116250 11.00000 0.01719 0.01585 = 0.01791 0.00088 0.00201 0.00220 N3 4 0.608190 0.379646 0.166981 11.00000 0.01490 0.01867 = 0.01270 -0.00055 0.00020 -0.00004 N4 4 0.519466 0.380489 0.097842 11.00000 0.01580 0.01642 = 0.01632 -0.00131 0.00079 0.00008 N5 4 0.446082 0.370676 0.150921 11.00000 0.01638 0.01528 = 0.01596 -0.00066 0.00212 -0.00032 SI6 5 0.320004 0.372891 0.070059 11.00000 0.01466 0.01860 = 0.01952 -0.00018 -0.00081 0.00019 C7 1 0.258146 0.319825 0.097540 11.00000 0.01772 0.02539 = 0.02981 0.00017 0.00218 -0.00281 AFIX 137 H00A 2 0.188129 0.320520 0.061360 11.00000 -1.50000 H00B 2 0.260409 0.315564 0.180317 11.00000 -1.50000 H00E 2 0.293212 0.295349 0.065464 11.00000 -1.50000 AFIX 0 C8 1 0.257360 0.420979 0.127465 11.00000 0.02045 0.02675 = 0.03172 -0.00356 -0.00002 0.00357 AFIX 137 H01G 2 0.290748 0.448340 0.108723 11.00000 -1.50000 H01H 2 0.261381 0.418211 0.210848 11.00000 -1.50000 H01I 2 0.186815 0.421822 0.093190 11.00000 -1.50000 AFIX 0 C9 1 0.330631 0.378860 -0.084460 11.00000 0.02574 0.02164 = 0.02065 0.00139 -0.00332 -0.00198 AFIX 137 H01A 2 0.293206 0.354995 -0.127482 11.00000 -1.50000 H01B 2 0.401382 0.377213 -0.095644 11.00000 -1.50000 H01C 2 0.302923 0.407528 -0.111928 11.00000 -1.50000 AFIX 0 C10 1 0.599572 0.371049 0.289220 11.00000 0.01671 0.01725 = 0.01244 -0.00015 0.00202 -0.00044 C11 1 0.601321 0.416316 0.362845 11.00000 0.01631 0.01686 = 0.01411 -0.00014 0.00121 0.00032 C12 1 0.514520 0.407295 0.434594 11.00000 0.01692 0.01769 = 0.01527 0.00190 0.00209 0.00229 C14 1 0.355594 0.370106 0.433182 11.00000 0.01771 0.02401 = 0.02147 -0.00058 0.00330 -0.00124 AFIX 43 H14 2 0.304470 0.351323 0.396285 11.00000 -1.20000 AFIX 0 C13 1 0.441685 0.377678 0.381967 11.00000 0.01703 0.01890 = 0.01549 0.00125 0.00179 0.00176 C15 1 0.343440 0.389636 0.537459 11.00000 0.02042 0.02960 = 0.02348 0.00003 0.00899 0.00133 AFIX 43 H15 2 0.284087 0.384546 0.570905 11.00000 -1.20000 AFIX 0 C16 1 0.418531 0.416537 0.592043 11.00000 0.02564 0.02504 = 0.01802 -0.00236 0.00679 0.00263 AFIX 43 H16 2 0.411804 0.428860 0.664799 11.00000 -1.20000 AFIX 0 C17 1 0.504025 0.425706 0.541097 11.00000 0.02131 0.02067 = 0.01747 -0.00145 0.00207 0.00049 AFIX 43 H17 2 0.554934 0.444415 0.578747 11.00000 -1.20000 AFIX 0 C18 1 0.467377 0.299432 0.268828 11.00000 0.01626 0.01979 = 0.01620 0.00011 -0.00027 -0.00095 C19 1 0.431701 0.274282 0.354079 11.00000 0.03248 0.02285 = 0.01959 -0.00155 0.00675 -0.00448 AFIX 43 H19 2 0.413004 0.288931 0.419323 11.00000 -1.20000 AFIX 0 C20 1 0.422625 0.228435 0.346612 11.00000 0.04903 0.02451 = 0.02810 0.00134 0.01260 -0.00911 AFIX 43 H01O 2 0.398823 0.212348 0.406757 11.00000 -1.20000 AFIX 0 C21 1 0.448137 0.206101 0.251855 11.00000 0.04248 0.01882 = 0.03201 -0.00196 0.00736 -0.00443 AFIX 43 H01K 2 0.440928 0.174861 0.245925 11.00000 -1.20000 AFIX 0 C22 1 0.484286 0.230080 0.166033 11.00000 0.02976 0.02274 = 0.02200 -0.00408 0.00340 0.00135 AFIX 43 H22 2 0.502482 0.215248 0.100798 11.00000 -1.20000 AFIX 0 C23 1 0.493973 0.275662 0.175109 11.00000 0.02156 0.02218 = 0.01800 0.00159 0.00271 0.00100 AFIX 43 H23 2 0.519596 0.291431 0.115628 11.00000 -1.20000 AFIX 0 C24 1 0.669304 0.334595 0.339705 11.00000 0.01509 0.01726 = 0.01800 -0.00086 -0.00112 -0.00105 C25 1 0.663676 0.320588 0.452169 11.00000 0.02037 0.02182 = 0.01897 0.00041 0.00048 0.00022 AFIX 43 H25 2 0.619573 0.335383 0.496038 11.00000 -1.20000 AFIX 0 C26 1 0.721212 0.285576 0.500572 11.00000 0.02950 0.02539 = 0.02256 0.00502 -0.00168 0.00137 AFIX 43 H26 2 0.716089 0.276649 0.576881 11.00000 -1.20000 AFIX 0 C27 1 0.786348 0.263464 0.438078 11.00000 0.03018 0.02534 = 0.03313 0.00384 -0.00382 0.00913 AFIX 43 H01N 2 0.826413 0.239701 0.471450 11.00000 -1.20000 AFIX 0 C28 1 0.792023 0.276552 0.326524 11.00000 0.02688 0.02851 = 0.03246 -0.00284 0.00246 0.00927 AFIX 43 H01J 2 0.836395 0.261718 0.283073 11.00000 -1.20000 AFIX 0 C29 1 0.733101 0.311321 0.277614 11.00000 0.02150 0.02365 = 0.02091 -0.00101 0.00145 0.00246 AFIX 43 H29 2 0.736516 0.319324 0.200255 11.00000 -1.20000 AFIX 0 C30 1 0.572858 0.455082 0.277436 11.00000 0.01866 0.01639 = 0.01281 -0.00193 -0.00023 -0.00105 C31 1 0.476991 0.473303 0.267906 11.00000 0.01931 0.01900 = 0.01799 -0.00121 0.00101 -0.00059 AFIX 43 H31 2 0.430631 0.461415 0.313814 11.00000 -1.20000 AFIX 0 C32 1 0.446060 0.508164 0.194105 11.00000 0.02018 0.01989 = 0.02122 -0.00194 -0.00288 0.00244 AFIX 43 H32 2 0.380271 0.519912 0.191202 11.00000 -1.20000 AFIX 0 C33 1 0.511521 0.525568 0.125158 11.00000 0.02708 0.01750 = 0.01853 0.00118 -0.00411 -0.00039 AFIX 43 H33 2 0.490958 0.548800 0.072821 11.00000 -1.20000 AFIX 0 C34 1 0.607983 0.508429 0.133873 11.00000 0.02474 0.01972 = 0.01544 0.00027 0.00039 -0.00443 AFIX 43 H34 2 0.653080 0.520601 0.086807 11.00000 -1.20000 AFIX 0 C35 1 0.641729 0.474038 0.208868 11.00000 0.01845 0.01755 = 0.01467 -0.00225 0.00048 -0.00222 C36 1 0.750944 0.461616 0.211975 11.00000 0.01886 0.02337 = 0.01225 -0.00013 0.00212 -0.00334 C37 1 0.820701 0.500652 0.219606 11.00000 0.01847 0.02307 = 0.01790 0.00159 0.00019 -0.00341 C38 1 0.814384 0.535476 0.296113 11.00000 0.01830 0.02304 = 0.02169 0.00005 -0.00041 -0.00073 AFIX 43 H38 2 0.767727 0.533841 0.349662 11.00000 -1.20000 AFIX 0 C39 1 0.875580 0.572579 0.294963 11.00000 0.02113 0.02332 = 0.03021 -0.00234 -0.00306 -0.00131 AFIX 43 H39 2 0.871510 0.595651 0.348950 11.00000 -1.20000 AFIX 0 C40 1 0.942402 0.576147 0.215726 11.00000 0.02198 0.02568 = 0.03280 0.00551 -0.00284 -0.00717 AFIX 43 H01E 2 0.983394 0.601710 0.214541 11.00000 -1.20000 AFIX 0 C41 1 0.948892 0.542135 0.138317 11.00000 0.02746 0.03780 = 0.02491 0.00356 0.00459 -0.01097 AFIX 43 H01M 2 0.994317 0.544380 0.083519 11.00000 -1.20000 AFIX 0 C42 1 0.889079 0.504696 0.140591 11.00000 0.02885 0.03182 = 0.02122 -0.00306 0.00634 -0.00946 AFIX 43 H42 2 0.894693 0.481428 0.087570 11.00000 -1.20000 AFIX 0 C43 1 0.780628 0.419790 0.189145 11.00000 0.01711 0.02440 = 0.01343 0.00040 0.00320 -0.00168 C44 1 0.885487 0.403000 0.208515 11.00000 0.01612 0.03026 = 0.01937 0.00204 0.00405 -0.00206 C45 1 0.955822 0.420128 0.296795 11.00000 0.01915 0.03735 = 0.02115 -0.00001 0.00305 -0.00431 AFIX 43 H45 2 0.939406 0.445693 0.337401 11.00000 -1.20000 AFIX 0 C46 1 1.048773 0.400288 0.325514 11.00000 0.01779 0.05807 = 0.02838 0.00174 -0.00034 -0.00355 AFIX 43 H01R 2 1.095375 0.412383 0.385306 11.00000 -1.20000 AFIX 0 C47 1 1.074062 0.362932 0.267515 11.00000 0.01670 0.06373 = 0.04069 0.00170 0.00359 0.00968 AFIX 43 H01S 2 1.137478 0.349203 0.288087 11.00000 -1.20000 AFIX 0 C48 1 1.006410 0.345659 0.179281 11.00000 0.02275 0.04930 = 0.03954 -0.00470 0.00731 0.00920 AFIX 43 H01Q 2 1.023679 0.320219 0.138747 11.00000 -1.20000 AFIX 0 C49 1 0.913558 0.365547 0.150277 11.00000 0.01839 0.03655 = 0.02773 -0.00350 0.00411 0.00117 AFIX 43 H01D 2 0.867906 0.353501 0.089503 11.00000 -1.20000 AFIX 0 C50 1 0.700392 0.385635 -0.013768 11.00000 0.01613 0.02239 = 0.01665 -0.00015 0.00220 0.00199 C51 1 0.664297 0.347099 -0.071244 11.00000 0.02610 0.02838 = 0.02269 -0.00423 0.00537 -0.00424 AFIX 43 H51 2 0.627994 0.326135 -0.032993 11.00000 -1.20000 AFIX 0 C52 1 0.680644 0.339004 -0.183119 11.00000 0.03460 0.03834 = 0.02489 -0.01202 0.00490 -0.00415 AFIX 43 H01P 2 0.657593 0.312198 -0.219878 11.00000 -1.20000 AFIX 0 C53 1 0.730668 0.370029 -0.241508 11.00000 0.03343 0.04591 = 0.01572 -0.00345 0.00589 0.00503 AFIX 43 H01L 2 0.740744 0.364703 -0.318593 11.00000 -1.20000 AFIX 0 C54 1 0.765820 0.408741 -0.187111 11.00000 0.03045 0.03505 = 0.02104 0.00651 0.00794 0.00333 AFIX 43 H01F 2 0.799500 0.430160 -0.226985 11.00000 -1.20000 AFIX 0 C55 1 0.751685 0.416114 -0.074331 11.00000 0.02374 0.02406 = 0.02018 0.00113 0.00332 0.00034 AFIX 43 H55 2 0.777355 0.442447 -0.037139 11.00000 -1.20000 AFIX 0 C56 1 0.696294 0.432375 0.441673 11.00000 0.01842 0.02064 = 0.01226 0.00139 0.00157 -0.00240 C57 1 0.786901 0.409915 0.468903 11.00000 0.01930 0.02239 = 0.01623 0.00041 0.00175 -0.00161 AFIX 43 H57 2 0.794798 0.381396 0.437293 11.00000 -1.20000 AFIX 0 C58 1 0.866266 0.428665 0.541917 11.00000 0.01867 0.03030 = 0.01822 0.00263 -0.00027 -0.00222 AFIX 43 H58 2 0.927109 0.412585 0.559358 11.00000 -1.20000 AFIX 0 C59 1 0.858024 0.470212 0.589365 11.00000 0.02438 0.02953 = 0.01584 0.00096 -0.00275 -0.00848 AFIX 43 H59 2 0.912508 0.482776 0.638637 11.00000 -1.20000 AFIX 0 C60 1 0.768321 0.493119 0.563332 11.00000 0.02991 0.02231 = 0.01690 -0.00140 0.00052 -0.00536 AFIX 43 H60 2 0.760831 0.521550 0.595623 11.00000 -1.20000 AFIX 0 C61 1 0.689566 0.474624 0.490298 11.00000 0.02223 0.02088 = 0.01726 0.00070 0.00102 -0.00095 AFIX 43 H61 2 0.629200 0.491024 0.472593 11.00000 -1.20000 AFIX 0 REM ##### simu 0.005 C1_1 > C6_1 Isor 0.008 C1_1 > C6_1 RESI 1 BENZ C1 1 1.015898 0.312269 0.572964 11.00000 0.06358 0.05793 = 0.11656 0.00028 -0.01549 -0.01288 AFIX 43 H01W 2 0.973430 0.321483 0.506063 11.00000 -1.20000 AFIX 0 C2 1 0.976854 0.307441 0.673515 11.00000 0.04639 0.06230 = 0.13156 -0.01524 0.00011 -0.00988 AFIX 43 H01V 2 0.908539 0.314538 0.676887 11.00000 -1.20000 AFIX 0 C3 1 1.039611 0.291529 0.774700 11.00000 0.07613 0.07523 = 0.11602 -0.02270 0.01475 -0.03022 AFIX 43 H01X 2 1.013737 0.286929 0.844879 11.00000 -1.20000 AFIX 0 C4 1 1.137998 0.283418 0.764537 11.00000 0.06368 0.05880 = 0.09578 -0.01309 -0.01144 -0.00875 AFIX 43 H01T 2 1.181996 0.273108 0.829050 11.00000 -1.20000 AFIX 0 C5 1 1.173597 0.289927 0.663262 11.00000 0.06066 0.05237 = 0.10091 -0.01806 -0.00629 0.00499 AFIX 43 H01U 2 1.242474 0.284411 0.658872 11.00000 -1.20000 AFIX 0 C6 1 1.112908 0.304239 0.567150 11.00000 0.07002 0.06104 = 0.10348 -0.01019 -0.00549 -0.01046 AFIX 43 H01Y 2 1.139474 0.308404 0.497223 11.00000 -1.20000 RESI 0 AFIX 0 HKLF 4 REM SoFu080_NeWi_a.res in P2(1)/c REM wR2 = 0.1173, GooF = S = 1.021, Restrained GooF = 1.042 for all data REM R1 = 0.0442 for 9162 Fo > 4sig(Fo) and 0.0461 for all 9732 data REM 607 parameters refined using 72 restraints END WGHT 0.0585 3.1814 REM Highest difference peak 0.707, deepest hole -0.370, 1-sigma level 0.051 Q1 1 1.0183 0.2999 0.8822 11.00000 0.05 0.71 Q2 1 0.9776 0.3064 0.7633 11.00000 0.05 0.70 Q3 1 1.0823 0.2739 0.8391 11.00000 0.05 0.34 Q4 1 0.7017 0.3873 0.0512 11.00000 0.05 0.31 Q5 1 0.3234 0.3738 -0.0179 11.00000 0.05 0.31 Q6 1 0.5417 0.3613 0.2859 11.00000 0.05 0.29 Q7 1 0.6997 0.4678 0.2109 11.00000 0.05 0.29 Q8 1 0.7438 0.4040 0.1608 11.00000 0.05 0.27 Q9 1 1.0364 0.2892 0.6401 11.00000 0.05 0.26 Q10 1 0.4532 0.3676 0.3252 11.00000 0.05 0.26 Q11 1 0.6389 0.3525 0.3152 11.00000 0.05 0.24 Q12 1 0.4787 0.3252 0.2739 11.00000 0.05 0.23 Q13 1 0.6512 0.4216 0.4019 11.00000 0.05 0.23 Q14 1 0.8369 0.4108 0.1980 11.00000 0.05 0.23 Q15 1 1.1115 0.2749 0.6137 11.00000 0.05 0.23 Q16 1 0.5854 0.4359 0.3205 11.00000 0.05 0.22 Q17 1 0.6051 0.3928 0.3255 11.00000 0.05 0.22 Q18 1 0.6052 0.3771 0.2279 11.00000 0.05 0.22 Q19 1 1.0563 0.2806 0.5483 11.00000 0.05 0.22 Q20 1 0.3648 0.2352 0.3153 11.00000 0.05 0.21 ; _shelx_res_checksum 20480 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 B1 B 0.48123(11) 0.35264(5) 0.27764(12) 0.0162(3) Uani 1 1 d . . . . . B2 B 0.69487(11) 0.39343(5) 0.11625(13) 0.0170(3) Uani 1 1 d . . . . . N3 N 0.60819(8) 0.37965(4) 0.16698(9) 0.0156(2) Uani 1 1 d . . . . . N4 N 0.51947(8) 0.38049(4) 0.09784(9) 0.0163(2) Uani 1 1 d . . . . . N5 N 0.44608(8) 0.37068(4) 0.15092(9) 0.0159(2) Uani 1 1 d . . . . . Si6 Si 0.32000(3) 0.37289(2) 0.07006(3) 0.01788(9) Uani 1 1 d . . . . . C7 C 0.25815(11) 0.31982(5) 0.09754(13) 0.0244(3) Uani 1 1 d . . . . . H00A H 0.188129 0.320520 0.061360 0.037 Uiso 1 1 calc R U . . . H00B H 0.260409 0.315564 0.180317 0.037 Uiso 1 1 calc R U . . . H00E H 0.293212 0.295349 0.065464 0.037 Uiso 1 1 calc R U . . . C8 C 0.25736(11) 0.42098(5) 0.12746(14) 0.0266(3) Uani 1 1 d . . . . . H01G H 0.290748 0.448340 0.108723 0.040 Uiso 1 1 calc R U . . . H01H H 0.261381 0.418211 0.210848 0.040 Uiso 1 1 calc R U . . . H01I H 0.186815 0.421822 0.093190 0.040 Uiso 1 1 calc R U . . . C9 C 0.33063(11) 0.37886(5) -0.08446(12) 0.0233(3) Uani 1 1 d . . . . . H01A H 0.293206 0.354995 -0.127482 0.035 Uiso 1 1 calc R U . . . H01B H 0.401382 0.377213 -0.095644 0.035 Uiso 1 1 calc R U . . . H01C H 0.302923 0.407528 -0.111928 0.035 Uiso 1 1 calc R U . . . C10 C 0.59957(10) 0.37105(4) 0.28922(11) 0.0155(3) Uani 1 1 d . . . . . C11 C 0.60132(10) 0.41632(4) 0.36285(11) 0.0158(3) Uani 1 1 d . . . . . C12 C 0.51452(10) 0.40730(4) 0.43459(11) 0.0166(3) Uani 1 1 d . . . . . C14 C 0.35559(10) 0.37011(5) 0.43318(12) 0.0210(3) Uani 1 1 d . . . . . H14 H 0.304470 0.351323 0.396285 0.025 Uiso 1 1 calc R U . . . C13 C 0.44168(10) 0.37768(4) 0.38197(11) 0.0172(3) Uani 1 1 d . . . . . C15 C 0.34344(11) 0.38964(5) 0.53746(13) 0.0239(3) Uani 1 1 d . . . . . H15 H 0.284087 0.384546 0.570905 0.029 Uiso 1 1 calc R U . . . C16 C 0.41853(11) 0.41654(5) 0.59204(12) 0.0225(3) Uani 1 1 d . . . . . H16 H 0.411804 0.428860 0.664799 0.027 Uiso 1 1 calc R U . . . C17 C 0.50402(10) 0.42571(5) 0.54110(11) 0.0199(3) Uani 1 1 d . . . . . H17 H 0.554934 0.444415 0.578747 0.024 Uiso 1 1 calc R U . . . C18 C 0.46738(10) 0.29943(4) 0.26883(11) 0.0176(3) Uani 1 1 d . . . . . C19 C 0.43170(12) 0.27428(5) 0.35408(12) 0.0247(3) Uani 1 1 d . . . . . H19 H 0.413004 0.288931 0.419323 0.030 Uiso 1 1 calc R U . . . C20 C 0.42263(14) 0.22844(5) 0.34661(14) 0.0332(4) Uani 1 1 d . . . . . H01O H 0.398823 0.212348 0.406757 0.040 Uiso 1 1 calc R U . . . C21 C 0.44814(13) 0.20610(5) 0.25186(14) 0.0309(3) Uani 1 1 d . . . . . H01K H 0.440928 0.174861 0.245925 0.037 Uiso 1 1 calc R U . . . C22 C 0.48429(12) 0.23008(5) 0.16603(13) 0.0248(3) Uani 1 1 d . . . . . H22 H 0.502482 0.215248 0.100798 0.030 Uiso 1 1 calc R U . . . C23 C 0.49397(10) 0.27566(5) 0.17511(12) 0.0206(3) Uani 1 1 d . . . . . H23 H 0.519596 0.291431 0.115628 0.025 Uiso 1 1 calc R U . . . C24 C 0.66930(10) 0.33459(4) 0.33971(11) 0.0171(3) Uani 1 1 d . . . . . C25 C 0.66368(10) 0.32059(5) 0.45217(12) 0.0206(3) Uani 1 1 d . . . . . H25 H 0.619573 0.335383 0.496038 0.025 Uiso 1 1 calc R U . . . C26 C 0.72121(12) 0.28558(5) 0.50057(13) 0.0263(3) Uani 1 1 d . . . . . H26 H 0.716089 0.276649 0.576881 0.032 Uiso 1 1 calc R U . . . C27 C 0.78635(12) 0.26346(5) 0.43808(14) 0.0303(3) Uani 1 1 d . . . . . H01N H 0.826413 0.239701 0.471450 0.036 Uiso 1 1 calc R U . . . C28 C 0.79202(12) 0.27655(5) 0.32652(14) 0.0294(3) Uani 1 1 d . . . . . H01J H 0.836395 0.261718 0.283073 0.035 Uiso 1 1 calc R U . . . C29 C 0.73310(11) 0.31132(5) 0.27761(12) 0.0222(3) Uani 1 1 d . . . . . H29 H 0.736516 0.319324 0.200255 0.027 Uiso 1 1 calc R U . . . C30 C 0.57286(10) 0.45508(4) 0.27744(11) 0.0162(3) Uani 1 1 d . . . . . C31 C 0.47699(10) 0.47330(4) 0.26791(11) 0.0189(3) Uani 1 1 d . . . . . H31 H 0.430631 0.461415 0.313814 0.023 Uiso 1 1 calc R U . . . C32 C 0.44606(11) 0.50816(5) 0.19410(12) 0.0210(3) Uani 1 1 d . . . . . H32 H 0.380271 0.519912 0.191202 0.025 Uiso 1 1 calc R U . . . C33 C 0.51152(11) 0.52557(5) 0.12516(12) 0.0217(3) Uani 1 1 d . . . . . H33 H 0.490958 0.548800 0.072821 0.026 Uiso 1 1 calc R U . . . C34 C 0.60798(11) 0.50843(5) 0.13387(11) 0.0202(3) Uani 1 1 d . . . . . H34 H 0.653080 0.520601 0.086807 0.024 Uiso 1 1 calc R U . . . C35 C 0.64173(10) 0.47404(4) 0.20887(11) 0.0171(3) Uani 1 1 d . . . . . C36 C 0.75094(10) 0.46162(5) 0.21197(11) 0.0182(3) Uani 1 1 d . . . . . C37 C 0.82070(10) 0.50065(5) 0.21961(12) 0.0200(3) Uani 1 1 d . . . . . C38 C 0.81438(10) 0.53548(5) 0.29611(12) 0.0213(3) Uani 1 1 d . . . . . H38 H 0.767727 0.533841 0.349662 0.026 Uiso 1 1 calc R U . . . C39 C 0.87558(11) 0.57258(5) 0.29496(13) 0.0255(3) Uani 1 1 d . . . . . H39 H 0.871510 0.595651 0.348950 0.031 Uiso 1 1 calc R U . . . C40 C 0.94240(11) 0.57615(5) 0.21573(14) 0.0274(3) Uani 1 1 d . . . . . H01E H 0.983394 0.601710 0.214541 0.033 Uiso 1 1 calc R U . . . C41 C 0.94889(12) 0.54214(6) 0.13832(13) 0.0300(3) Uani 1 1 d . . . . . H01M H 0.994317 0.544380 0.083519 0.036 Uiso 1 1 calc R U . . . C42 C 0.88908(12) 0.50470(5) 0.14059(13) 0.0270(3) Uani 1 1 d . . . . . H42 H 0.894693 0.481428 0.087570 0.032 Uiso 1 1 calc R U . . . C43 C 0.78063(10) 0.41979(5) 0.18914(11) 0.0182(3) Uani 1 1 d . . . . . C44 C 0.88549(10) 0.40300(5) 0.20852(12) 0.0218(3) Uani 1 1 d . . . . . C45 C 0.95582(11) 0.42013(5) 0.29679(13) 0.0259(3) Uani 1 1 d . . . . . H45 H 0.939406 0.445693 0.337401 0.031 Uiso 1 1 calc R U . . . C46 C 1.04877(12) 0.40029(7) 0.32551(14) 0.0351(4) Uani 1 1 d . . . . . H01R H 1.095375 0.412383 0.385306 0.042 Uiso 1 1 calc R U . . . C47 C 1.07406(12) 0.36293(7) 0.26752(16) 0.0404(4) Uani 1 1 d . . . . . H01S H 1.137478 0.349203 0.288087 0.048 Uiso 1 1 calc R U . . . C48 C 1.00641(12) 0.34566(7) 0.17928(16) 0.0369(4) Uani 1 1 d . . . . . H01Q H 1.023679 0.320219 0.138747 0.044 Uiso 1 1 calc R U . . . C49 C 0.91356(11) 0.36555(5) 0.15028(14) 0.0275(3) Uani 1 1 d . . . . . H01D H 0.867906 0.353501 0.089503 0.033 Uiso 1 1 calc R U . . . C50 C 0.70039(10) 0.38563(5) -0.01377(11) 0.0184(3) Uani 1 1 d . . . . . C51 C 0.66430(11) 0.34710(5) -0.07124(13) 0.0255(3) Uani 1 1 d . . . . . H51 H 0.627994 0.326135 -0.032993 0.031 Uiso 1 1 calc R U . . . C52 C 0.68064(13) 0.33900(6) -0.18312(14) 0.0325(4) Uani 1 1 d . . . . . H01P H 0.657593 0.312198 -0.219878 0.039 Uiso 1 1 calc R U . . . C53 C 0.73067(13) 0.37003(6) -0.24151(13) 0.0314(4) Uani 1 1 d . . . . . H01L H 0.740744 0.364703 -0.318593 0.038 Uiso 1 1 calc R U . . . C54 C 0.76582(12) 0.40874(6) -0.18711(13) 0.0284(3) Uani 1 1 d . . . . . H01F H 0.799500 0.430160 -0.226985 0.034 Uiso 1 1 calc R U . . . C55 C 0.75168(11) 0.41611(5) -0.07433(12) 0.0226(3) Uani 1 1 d . . . . . H55 H 0.777355 0.442447 -0.037139 0.027 Uiso 1 1 calc R U . . . C56 C 0.69629(10) 0.43237(4) 0.44167(11) 0.0172(3) Uani 1 1 d . . . . . C57 C 0.78690(10) 0.40991(5) 0.46890(11) 0.0194(3) Uani 1 1 d . . . . . H57 H 0.794798 0.381396 0.437293 0.023 Uiso 1 1 calc R U . . . C58 C 0.86627(11) 0.42867(5) 0.54192(12) 0.0227(3) Uani 1 1 d . . . . . H58 H 0.927109 0.412585 0.559358 0.027 Uiso 1 1 calc R U . . . C59 C 0.85802(11) 0.47021(5) 0.58937(12) 0.0238(3) Uani 1 1 d . . . . . H59 H 0.912508 0.482776 0.638637 0.029 Uiso 1 1 calc R U . . . C60 C 0.76832(11) 0.49312(5) 0.56333(12) 0.0233(3) Uani 1 1 d . . . . . H60 H 0.760831 0.521550 0.595623 0.028 Uiso 1 1 calc R U . . . C61 C 0.68957(11) 0.47462(5) 0.49030(11) 0.0203(3) Uani 1 1 d . . . . . H61 H 0.629200 0.491024 0.472593 0.024 Uiso 1 1 calc R U . . . C1_1 C 1.0159(2) 0.31227(10) 0.5730(3) 0.0819(8) Uani 1 1 d . U . . . H01W_1 H 0.973430 0.321483 0.506063 0.098 Uiso 1 1 calc R U . . . C2_1 C 0.9769(2) 0.30744(10) 0.6735(3) 0.0812(8) Uani 1 1 d . U . . . H01V_1 H 0.908539 0.314538 0.676887 0.097 Uiso 1 1 calc R U . . . C3_1 C 1.0396(2) 0.29153(11) 0.7747(3) 0.0890(9) Uani 1 1 d . U . . . H01X_1 H 1.013737 0.286929 0.844879 0.107 Uiso 1 1 calc R U . . . C4_1 C 1.1380(2) 0.28342(9) 0.7645(3) 0.0748(7) Uani 1 1 d . U . . . H01T_1 H 1.181996 0.273108 0.829050 0.090 Uiso 1 1 calc R U . . . C5_1 C 1.1736(2) 0.28993(9) 0.6633(3) 0.0729(7) Uani 1 1 d . U . . . H01U_1 H 1.242474 0.284411 0.658872 0.087 Uiso 1 1 calc R U . . . C6_1 C 1.1129(2) 0.30424(10) 0.5671(3) 0.0798(8) Uani 1 1 d . U . . . H01Y_1 H 1.139474 0.308404 0.497223 0.096 Uiso 1 1 calc R U . . . 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 B1 0.0151(7) 0.0187(7) 0.0145(7) 0.0008(5) 0.0010(5) 0.0003(5) B2 0.0172(7) 0.0158(7) 0.0179(7) 0.0009(5) 0.0020(5) 0.0022(5) N3 0.0149(5) 0.0187(5) 0.0127(5) -0.0005(4) 0.0002(4) 0.0000(4) N4 0.0158(5) 0.0164(5) 0.0163(5) -0.0013(4) 0.0008(4) 0.0001(4) N5 0.0164(5) 0.0153(5) 0.0160(5) -0.0007(4) 0.0021(4) -0.0003(4) Si6 0.01466(18) 0.01860(18) 0.01952(19) -0.00018(13) -0.00081(13) 0.00019(13) C7 0.0177(7) 0.0254(7) 0.0298(7) 0.0002(6) 0.0022(6) -0.0028(5) C8 0.0204(7) 0.0268(7) 0.0317(8) -0.0036(6) 0.0000(6) 0.0036(6) C9 0.0257(7) 0.0216(7) 0.0206(7) 0.0014(5) -0.0033(5) -0.0020(5) C10 0.0167(6) 0.0173(6) 0.0124(6) -0.0002(5) 0.0020(5) -0.0004(5) C11 0.0163(6) 0.0169(6) 0.0141(6) -0.0001(5) 0.0012(5) 0.0003(5) C12 0.0169(6) 0.0177(6) 0.0153(6) 0.0019(5) 0.0021(5) 0.0023(5) C14 0.0177(6) 0.0240(7) 0.0215(7) -0.0006(5) 0.0033(5) -0.0012(5) C13 0.0170(6) 0.0189(6) 0.0155(6) 0.0012(5) 0.0018(5) 0.0018(5) C15 0.0204(7) 0.0296(7) 0.0235(7) 0.0000(6) 0.0090(5) 0.0013(6) C16 0.0256(7) 0.0250(7) 0.0180(6) -0.0024(5) 0.0068(5) 0.0026(6) C17 0.0213(7) 0.0207(6) 0.0175(6) -0.0015(5) 0.0021(5) 0.0005(5) C18 0.0163(6) 0.0198(6) 0.0162(6) 0.0001(5) -0.0003(5) -0.0010(5) C19 0.0325(8) 0.0229(7) 0.0196(7) -0.0016(5) 0.0067(6) -0.0045(6) C20 0.0490(10) 0.0245(8) 0.0281(8) 0.0013(6) 0.0126(7) -0.0091(7) C21 0.0425(9) 0.0188(7) 0.0320(8) -0.0020(6) 0.0074(7) -0.0044(6) C22 0.0298(8) 0.0227(7) 0.0220(7) -0.0041(5) 0.0034(6) 0.0014(6) C23 0.0216(7) 0.0222(7) 0.0180(6) 0.0016(5) 0.0027(5) 0.0010(5) C24 0.0151(6) 0.0173(6) 0.0180(6) -0.0009(5) -0.0011(5) -0.0011(5) C25 0.0204(7) 0.0218(7) 0.0190(6) 0.0004(5) 0.0005(5) 0.0002(5) C26 0.0295(8) 0.0254(7) 0.0226(7) 0.0050(6) -0.0017(6) 0.0014(6) C27 0.0302(8) 0.0253(8) 0.0331(8) 0.0038(6) -0.0038(6) 0.0091(6) C28 0.0269(8) 0.0285(8) 0.0325(8) -0.0028(6) 0.0025(6) 0.0093(6) C29 0.0215(7) 0.0237(7) 0.0209(7) -0.0010(5) 0.0014(5) 0.0025(5) C30 0.0187(6) 0.0164(6) 0.0128(6) -0.0019(5) -0.0002(5) -0.0011(5) C31 0.0193(7) 0.0190(6) 0.0180(6) -0.0012(5) 0.0010(5) -0.0006(5) C32 0.0202(7) 0.0199(7) 0.0212(7) -0.0019(5) -0.0029(5) 0.0024(5) C33 0.0271(7) 0.0175(6) 0.0185(6) 0.0012(5) -0.0041(5) -0.0004(5) C34 0.0247(7) 0.0197(7) 0.0154(6) 0.0003(5) 0.0004(5) -0.0044(5) C35 0.0185(6) 0.0176(6) 0.0147(6) -0.0022(5) 0.0005(5) -0.0022(5) C36 0.0189(6) 0.0234(7) 0.0123(6) -0.0001(5) 0.0021(5) -0.0033(5) C37 0.0185(6) 0.0231(7) 0.0179(6) 0.0016(5) 0.0002(5) -0.0034(5) C38 0.0183(6) 0.0230(7) 0.0217(7) 0.0000(5) -0.0004(5) -0.0007(5) C39 0.0211(7) 0.0233(7) 0.0302(8) -0.0023(6) -0.0031(6) -0.0013(6) C40 0.0220(7) 0.0257(7) 0.0328(8) 0.0055(6) -0.0028(6) -0.0072(6) C41 0.0275(8) 0.0378(9) 0.0249(7) 0.0036(6) 0.0046(6) -0.0110(7) C42 0.0288(8) 0.0318(8) 0.0212(7) -0.0031(6) 0.0063(6) -0.0095(6) C43 0.0171(6) 0.0244(7) 0.0134(6) 0.0004(5) 0.0032(5) -0.0017(5) C44 0.0161(6) 0.0303(7) 0.0194(7) 0.0020(5) 0.0041(5) -0.0021(5) C45 0.0192(7) 0.0374(8) 0.0212(7) 0.0000(6) 0.0030(5) -0.0043(6) C46 0.0178(7) 0.0581(11) 0.0284(8) 0.0017(7) -0.0003(6) -0.0036(7) C47 0.0167(7) 0.0637(12) 0.0407(10) 0.0017(9) 0.0036(7) 0.0097(7) C48 0.0228(8) 0.0493(10) 0.0395(9) -0.0047(8) 0.0073(7) 0.0092(7) C49 0.0184(7) 0.0365(8) 0.0277(8) -0.0035(6) 0.0041(6) 0.0012(6) C50 0.0161(6) 0.0224(7) 0.0167(6) -0.0002(5) 0.0022(5) 0.0020(5) C51 0.0261(7) 0.0284(8) 0.0227(7) -0.0042(6) 0.0054(6) -0.0042(6) C52 0.0346(9) 0.0383(9) 0.0249(8) -0.0120(7) 0.0049(6) -0.0042(7) C53 0.0334(8) 0.0459(10) 0.0157(7) -0.0035(6) 0.0059(6) 0.0050(7) C54 0.0305(8) 0.0351(8) 0.0210(7) 0.0065(6) 0.0079(6) 0.0033(6) C55 0.0237(7) 0.0241(7) 0.0202(7) 0.0011(5) 0.0033(5) 0.0003(5) C56 0.0184(6) 0.0206(6) 0.0123(6) 0.0014(5) 0.0016(5) -0.0024(5) C57 0.0193(7) 0.0224(7) 0.0162(6) 0.0004(5) 0.0017(5) -0.0016(5) C58 0.0187(7) 0.0303(7) 0.0182(6) 0.0026(5) -0.0003(5) -0.0022(6) C59 0.0244(7) 0.0295(7) 0.0158(6) 0.0010(5) -0.0028(5) -0.0085(6) C60 0.0299(8) 0.0223(7) 0.0169(6) -0.0014(5) 0.0005(5) -0.0054(6) C61 0.0222(7) 0.0209(7) 0.0173(6) 0.0007(5) 0.0010(5) -0.0009(5) C1_1 0.0636(15) 0.0579(14) 0.117(2) 0.0003(15) -0.0155(15) -0.0129(12) C2_1 0.0464(13) 0.0623(15) 0.132(2) -0.0152(16) 0.0001(14) -0.0099(11) C3_1 0.0761(17) 0.0752(17) 0.116(2) -0.0227(16) 0.0148(16) -0.0302(14) C4_1 0.0637(15) 0.0588(14) 0.0958(18) -0.0131(13) -0.0114(14) -0.0088(12) C5_1 0.0607(14) 0.0524(13) 0.1009(19) -0.0181(13) -0.0063(14) 0.0050(11) C6_1 0.0700(16) 0.0610(15) 0.1035(19) -0.0102(14) -0.0055(15) -0.0105(13) 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 0.1569 0 1 0 0.1634 -1 -1 2 0.1945 1 2 -2 0.3027 1 0 -2 0.3426 1 2 -1 0.2405 -1 -2 1 0.1989 1 2 0 0.1311 -1 -1 1 0.1923 1 1 -1 0.2654 0 -1 -1 0.3542 -1 -1 0 0.1673 2 -1 0 0.1164 -2 1 0 0.1378 1 0 2 0.1467 -1 1 2 0.1773 0 0 -1 0.3451 -2 1 -2 0.2696 0 0 1 0.1618 2 1 0 0.0952 -2 -1 0 0.1562 0 1 2 0.1592 -1 0 1 0.1868 1 1 1 0.1346 2 1 2 0.1260 2 1 1 0.1082 2 -1 2 0.1432 2 -1 1 0.1256 1 -1 -1 0.3167 2 -2 -1 0.2425 -2 2 1 0.1774 1 -2 0 0.1439 -1 2 0 0.1797 0 -1 2 0.1694 0 1 -1 0.3172 0 -2 -1 0.3320 0 2 1 0.1850 -1 0 -2 0.3103 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 C13 B1 N5 118.07(11) . . ? C13 B1 C18 118.19(11) . . ? N5 B1 C18 105.15(10) . . ? C13 B1 C10 101.14(10) . . ? N5 B1 C10 96.89(10) . . ? C18 B1 C10 115.76(11) . . ? N3 B2 C43 119.90(12) . . ? N3 B2 C50 120.80(12) . . ? C43 B2 C50 119.11(12) . . ? N4 N3 B2 116.29(11) . . ? N4 N3 C10 114.15(10) . . ? B2 N3 C10 128.85(11) . . ? N5 N4 N3 112.35(10) . . ? N4 N5 B1 112.78(10) . . ? N4 N5 Si6 117.49(9) . . ? B1 N5 Si6 129.32(9) . . ? N5 Si6 C8 105.92(6) . . ? N5 Si6 C9 108.94(6) . . ? C8 Si6 C9 112.46(7) . . ? N5 Si6 C7 106.49(6) . . ? C8 Si6 C7 112.10(7) . . ? C9 Si6 C7 110.60(7) . . ? N3 C10 C24 112.47(10) . . ? N3 C10 C11 112.05(10) . . ? C24 C10 C11 116.15(10) . . ? N3 C10 B1 100.27(10) . . ? C24 C10 B1 108.78(10) . . ? C11 C10 B1 105.58(10) . . ? C56 C11 C12 110.34(10) . . ? C56 C11 C30 105.18(10) . . ? C12 C11 C30 110.23(10) . . ? C56 C11 C10 122.40(11) . . ? C12 C11 C10 100.73(10) . . ? C30 C11 C10 107.73(10) . . ? C17 C12 C13 119.95(12) . . ? C17 C12 C11 126.39(12) . . ? C13 C12 C11 113.66(11) . . ? C15 C14 C13 121.07(13) . . ? C14 C13 C12 118.88(12) . . ? C14 C13 B1 129.72(12) . . ? C12 C13 B1 110.82(11) . . ? C16 C15 C14 119.49(13) . . ? C15 C16 C17 120.58(13) . . ? C16 C17 C12 119.82(13) . . ? C19 C18 C23 115.93(13) . . ? C19 C18 B1 122.81(12) . . ? C23 C18 B1 121.23(12) . . ? C20 C19 C18 122.13(14) . . ? C21 C20 C19 120.37(14) . . ? C22 C21 C20 118.91(14) . . ? C21 C22 C23 120.13(14) . . ? C22 C23 C18 122.51(13) . . ? C29 C24 C25 117.43(12) . . ? C29 C24 C10 123.65(12) . . ? C25 C24 C10 118.67(12) . . ? C26 C25 C24 121.30(13) . . ? C25 C26 C27 120.37(14) . . ? C28 C27 C26 119.08(14) . . ? C27 C28 C29 120.41(14) . . ? C24 C29 C28 121.37(14) . . ? C31 C30 C35 117.44(12) . . ? C31 C30 C11 119.52(12) . . ? C35 C30 C11 123.02(12) . . ? C32 C31 C30 122.94(13) . . ? C33 C32 C31 119.65(13) . . ? C32 C33 C34 118.66(13) . . ? C33 C34 C35 122.92(13) . . ? C34 C35 C30 118.34(12) . . ? C34 C35 C36 115.49(12) . . ? C30 C35 C36 126.14(12) . . ? C43 C36 C37 122.81(12) . . ? C43 C36 C35 122.36(12) . . ? C37 C36 C35 113.83(12) . . ? C38 C37 C42 117.84(13) . . ? C38 C37 C36 122.53(12) . . ? C42 C37 C36 119.37(13) . . ? C39 C38 C37 120.82(13) . . ? C40 C39 C38 120.55(14) . . ? C41 C40 C39 119.41(14) . . ? C40 C41 C42 120.14(14) . . ? C41 C42 C37 121.21(14) . . ? C36 C43 C44 125.68(13) . . ? C36 C43 B2 111.53(12) . . ? C44 C43 B2 121.72(12) . . ? C49 C44 C45 117.39(14) . . ? C49 C44 C43 120.89(13) . . ? C45 C44 C43 121.13(13) . . ? C46 C45 C44 121.03(15) . . ? C47 C46 C45 120.37(16) . . ? C46 C47 C48 119.72(16) . . ? C49 C48 C47 119.95(17) . . ? C48 C49 C44 121.53(15) . . ? C51 C50 C55 117.51(13) . . ? C51 C50 B2 122.70(13) . . ? C55 C50 B2 119.51(12) . . ? C52 C51 C50 121.11(14) . . ? C51 C52 C53 120.12(15) . . ? C54 C53 C52 119.87(14) . . ? C53 C54 C55 119.76(14) . . ? C54 C55 C50 121.58(14) . . ? C57 C56 C61 116.77(12) . . ? C57 C56 C11 127.51(12) . . ? C61 C56 C11 115.71(12) . . ? C56 C57 C58 121.06(13) . . ? C59 C58 C57 121.30(14) . . ? C58 C59 C60 118.52(13) . . ? C61 C60 C59 120.24(14) . . ? C60 C61 C56 122.10(13) . . ? C6_1 C1_1 C2_1 121.2(3) . . ? C1_1 C2_1 C3_1 120.0(3) . . ? C4_1 C3_1 C2_1 116.8(3) . . ? C5_1 C4_1 C3_1 120.8(3) . . ? C4_1 C5_1 C6_1 121.9(3) . . ? C1_1 C6_1 C5_1 119.3(4) . . ? 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 B1 C13 1.5949(19) . ? B1 N5 1.5990(18) . ? B1 C18 1.619(2) . ? B1 C10 1.6746(19) . ? B2 N3 1.4425(18) . ? B2 C43 1.5597(19) . ? B2 C50 1.5615(19) . ? N3 N4 1.3508(15) . ? N3 C10 1.4833(16) . ? N4 N5 1.2737(16) . ? N5 Si6 1.8303(12) . ? Si6 C8 1.8526(15) . ? Si6 C9 1.8541(15) . ? Si6 C7 1.8545(15) . ? C10 C24 1.5146(18) . ? C10 C11 1.6174(18) . ? C11 C56 1.5516(18) . ? C11 C12 1.5562(18) . ? C11 C30 1.5572(18) . ? C12 C17 1.3970(19) . ? C12 C13 1.4069(19) . ? C14 C15 1.392(2) . ? C14 C13 1.3960(19) . ? C15 C16 1.385(2) . ? C16 C17 1.396(2) . ? C18 C19 1.3955(19) . ? C18 C23 1.4036(19) . ? C19 C20 1.392(2) . ? C20 C21 1.387(2) . ? C21 C22 1.385(2) . ? C22 C23 1.385(2) . ? C24 C29 1.3918(19) . ? C24 C25 1.4026(19) . ? C25 C26 1.386(2) . ? C26 C27 1.390(2) . ? C27 C28 1.384(2) . ? C28 C29 1.392(2) . ? C30 C31 1.3929(19) . ? C30 C35 1.4293(18) . ? C31 C32 1.3925(19) . ? C32 C33 1.381(2) . ? C33 C34 1.388(2) . ? C34 C35 1.3986(19) . ? C35 C36 1.5124(18) . ? C36 C43 1.363(2) . ? C36 C37 1.5020(18) . ? C37 C38 1.395(2) . ? C37 C42 1.400(2) . ? C38 C39 1.392(2) . ? C39 C40 1.386(2) . ? C40 C41 1.384(2) . ? C41 C42 1.390(2) . ? C43 C44 1.4874(19) . ? C44 C49 1.401(2) . ? C44 C45 1.406(2) . ? C45 C46 1.387(2) . ? C46 C47 1.385(3) . ? C47 C48 1.387(3) . ? C48 C49 1.386(2) . ? C50 C51 1.400(2) . ? C50 C55 1.402(2) . ? C51 C52 1.387(2) . ? C52 C53 1.389(2) . ? C53 C54 1.385(2) . ? C54 C55 1.386(2) . ? C56 C57 1.3939(19) . ? C56 C61 1.4065(19) . ? C57 C58 1.3967(19) . ? C58 C59 1.384(2) . ? C59 C60 1.389(2) . ? C60 C61 1.3881(19) . ? C1_1 C6_1 1.339(4) . ? C1_1 C2_1 1.368(5) . ? C2_1 C3_1 1.446(5) . ? C3_1 C4_1 1.368(4) . ? C4_1 C5_1 1.359(4) . ? C5_1 C6_1 1.373(4) . ?