#------------------------------------------------------------------------------ #$Date: 2024-07-09 01:14:14 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293302 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572078.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_1572078 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 'C29 H28 B N Si' _chemical_formula_sum 'C29 H28 B N Si' _chemical_formula_weight 429.42 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 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 106.2250(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.0612(2) _cell_length_b 11.32090(10) _cell_length_c 16.7015(2) _cell_measurement_reflns_used 11540 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 74.0590 _cell_measurement_theta_min 3.7900 _cell_volume 2371.20(5) _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 0.996 _diffrn_measured_fraction_theta_max 0.982 _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 63.00 88.00 0.50 0.50 -- 50.00 52.00 -87.16 50 2 \w 98.00 123.00 0.50 0.50 -- 85.25 44.00-114.32 50 3 \w 101.00 127.00 0.50 0.50 -- 85.25 34.00-155.00 52 4 \w 99.00 125.00 0.50 0.50 -- 85.25 42.00-148.69 52 5 \w 98.00 132.00 0.50 0.50 -- 82.31 15.00-180.00 68 6 \w 93.00 136.00 0.50 0.50 -- 85.25 23.00 -89.24 86 7 \w 107.00 133.00 0.50 0.50 -- 82.31 15.00-150.00 52 8 \w 101.00 126.00 0.50 0.50 -- 85.25 65.00 -9.12 50 9 \w 98.00 131.00 0.50 0.50 -- 85.25 55.00 108.31 66 10 \w 99.00 133.00 0.50 0.50 -- 85.25 51.00 163.46 68 11 \w 52.00 84.00 0.50 0.50 -- 85.25 -83.00 168.86 64 12 \w 38.00 63.00 0.50 0.50 -- 58.61-129.00 -28.00 50 13 \w 34.00 88.00 0.50 0.50 -- 71.30-129.00 -28.00 108 14 \w 79.00 104.00 0.50 0.50 -- 85.25-137.00 -49.95 50 15 \w 40.00 74.00 0.50 0.50 -- 85.25-137.00 -49.95 68 16 \w 39.00 65.00 0.50 0.50 -- 85.25-136.00-104.66 52 17 \w 37.00 69.00 0.50 0.50 -- 82.31-129.00 -28.00 64 18 \w 52.00 82.00 0.50 0.50 -- 85.25-116.00 6.71 60 19 \w 37.00 71.00 0.50 0.50 -- 85.25-116.00 -1.18 68 20 \w 72.00 97.00 0.50 0.50 -- 85.25-114.00 -31.65 50 21 \w 39.00 66.00 0.50 0.50 -- 85.25-116.00 -27.26 54 22 \w 71.00 97.00 0.50 0.50 -- 82.31-112.00 30.00 52 23 \w 42.00 101.00 0.50 0.50 -- 85.25-124.00 107.87 118 24 \w 73.00 99.00 0.50 0.50 -- 85.25-124.00 147.39 52 25 \w 38.00 84.00 0.50 0.50 -- 85.25-118.00 149.79 92 26 \w 60.00 97.00 0.50 0.50 -- 82.31-112.00 120.00 74 27 \w 71.00 97.00 0.50 0.50 -- 82.31-112.00 90.00 52 28 \w 42.00 69.00 0.50 0.50 -- 82.31 -95.00 60.00 54 29 \w 40.00 66.00 0.50 0.50 -- 85.25-110.00 29.45 52 30 \w 67.00 93.00 0.50 0.50 -- 85.25-110.00 29.45 52 31 \w 45.00 87.00 0.50 0.50 -- 85.25 -94.00 36.27 84 32 \w 43.00 68.00 0.50 0.50 -- 85.25 -93.00 -2.42 50 33 \w 68.00 94.00 0.50 0.50 -- 85.25 -99.00 -4.43 52 34 \w 67.00 93.00 0.50 0.50 -- 85.25 -95.00 -35.13 52 35 \w 52.00 90.00 0.50 0.50 -- 82.31 -95.00 -60.00 76 36 \w 45.00 70.00 0.50 0.50 -- 85.25 -88.00 -80.05 50 37 \w 104.00 129.00 0.50 0.50 -- 85.25 112.00-124.51 50 38 \w 100.00 133.00 0.50 0.50 -- 85.25 119.00-112.12 66 39 \w 103.00 134.00 0.50 0.50 -- 85.25 115.00-101.23 62 40 \w 104.00 133.00 0.50 0.50 -- 85.25 117.00 156.18 58 41 \w -57.00 -16.00 0.50 0.50 -- -60.19 129.00 44.00 82 42 \w -89.00 -64.00 0.50 0.50 -- -76.37 129.00 44.00 50 43 \w -85.00 -60.00 0.50 0.50 -- -69.72 129.00 44.00 50 44 \w -95.00 -69.00 0.50 0.50 -- -79.50 107.00 34.05 52 45 \w -93.00 -63.00 0.50 0.50 -- -79.50 108.00 -2.22 60 46 \w -61.00 -35.00 0.50 0.50 -- -79.50 108.00 -2.22 52 47 \w -114.00 -86.00 0.50 0.50 -- -70.00 -59.00 -31.61 56 48 \w -121.00 -93.00 0.50 0.50 -- -79.50 -54.00 -10.09 56 49 \w -117.00 -84.00 0.50 0.50 -- -70.00 -56.00 140.36 66 50 \w -103.00 -72.00 0.50 0.50 -- -58.00 -48.00 -6.32 62 51 \w -128.00 -94.00 0.50 0.50 -- -79.50 -52.00 -63.42 68 52 \w -97.00 -67.00 0.50 0.50 -- -50.00 -51.00-162.70 60 ; _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 0.0316 _diffrn_reflns_av_unetI/netI 0.0241 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 30697 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.218 _diffrn_reflns_theta_min 3.820 _diffrn_source 'rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R X-ray Source' _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.82569 _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 colourless _exptl_crystal_density_diffrn 1.203 _exptl_crystal_description block _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.092 _exptl_crystal_size_min 0.066 _refine_diff_density_max 0.344 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 292 _refine_ls_number_reflns 4819 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0444 _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^)+(0.0661P)^2^+0.8981P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1163 _refine_ls_wR_factor_ref 0.1214 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4182 _reflns_number_total 4819 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03817g2.cif _cod_data_source_block 3 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1572078 _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 0.843 _shelx_estimated_absorpt_t_max 0.935 _shelx_res_file ; TITL MaMi060_NeWi_a.res in P2(1)/n MaMi060_NeWi_a.res created by SHELXL-2018/3 at 13:49:05 on 28-Mar-2022 REM Old TITL MaMi060_NeWi in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.128, Rweak 0.147, Alpha 0.026 REM 0.543 for 255 systematic absences, Orientation as input REM Formula found by SHELXT: C30 N Si CELL 1.54184 13.0612 11.3209 16.7015 90.000 106.225 90.000 ZERR 4.000 0.0002 0.0001 0.0002 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H B N SI UNIT 116 112 4 4 4 TEMP -173 SIZE 0.07 0.09 0.18 L.S. 10 BOND $H LIST 4 ACTA CONF FMAP 2 PLAN 20 WGHT 0.066100 0.898100 FVAR 0.59048 SI01 5 0.790740 0.499812 0.448422 11.00000 0.02480 0.03774 = 0.02541 0.00085 0.00621 -0.00056 N002 4 0.652802 0.496929 0.386286 11.00000 0.02673 0.03258 = 0.02369 0.00109 0.00923 0.00081 C003 1 0.493485 0.560165 0.234968 11.00000 0.02554 0.03510 = 0.02431 -0.00003 0.00949 -0.00301 C004 1 0.514944 0.632593 0.310295 11.00000 0.02735 0.03156 = 0.02407 0.00153 0.00983 -0.00055 C005 1 0.600474 0.660514 0.463637 11.00000 0.02407 0.03492 = 0.02421 -0.00075 0.00631 0.00076 C006 1 0.536126 0.444441 0.240773 11.00000 0.02554 0.03508 = 0.02574 -0.00043 0.01118 -0.00332 C007 1 0.604721 0.589793 0.533038 11.00000 0.02447 0.03385 = 0.02701 -0.00023 0.00757 -0.00101 AFIX 43 H007 2 0.600264 0.506378 0.526844 11.00000 -1.20000 AFIX 0 C008 1 0.588996 0.600287 0.381803 11.00000 0.02754 0.02967 = 0.02637 0.00029 0.01007 -0.00184 C009 1 0.509729 0.373199 0.168485 11.00000 0.02875 0.03697 = 0.03095 -0.00361 0.00955 -0.00265 AFIX 43 H009 2 0.535132 0.294201 0.171980 11.00000 -1.20000 AFIX 0 C00A 1 0.615363 0.639576 0.610967 11.00000 0.02906 0.04115 = 0.02639 0.00105 0.00938 -0.00011 AFIX 43 H00A 2 0.618265 0.590266 0.657575 11.00000 -1.20000 AFIX 0 C00B 1 0.665006 0.279888 0.338335 11.00000 0.02547 0.03689 = 0.02943 -0.00450 0.00654 0.00090 C00C 1 0.355933 0.735052 0.334607 11.00000 0.03084 0.03881 = 0.03104 -0.00082 0.00973 0.00076 AFIX 43 H00C 2 0.337706 0.663386 0.356861 11.00000 -1.20000 AFIX 0 B0 3 0.618013 0.408004 0.322963 11.00000 0.02633 0.03461 = 0.02611 -0.00118 0.01199 -0.00230 C00D 1 0.653903 0.214732 0.406870 11.00000 0.03233 0.03419 = 0.03176 -0.00274 0.00544 0.00144 AFIX 43 H00D 2 0.619791 0.250293 0.444119 11.00000 -1.20000 AFIX 0 C00E 1 0.446896 0.740164 0.306647 11.00000 0.02949 0.03341 = 0.02180 -0.00004 0.00599 0.00111 C00F 1 0.606390 0.782842 0.474186 11.00000 0.03660 0.03415 = 0.02726 0.00005 0.00815 -0.00133 AFIX 43 H00F 2 0.603203 0.832639 0.427769 11.00000 -1.20000 AFIX 0 C00G 1 0.621720 0.760684 0.620688 11.00000 0.03797 0.04325 = 0.02687 -0.00648 0.00929 0.00068 AFIX 43 H00G 2 0.629343 0.795003 0.673944 11.00000 -1.20000 AFIX 0 C00H 1 0.428201 0.600680 0.157803 11.00000 0.03328 0.03781 = 0.02882 0.00151 0.00806 0.00007 AFIX 43 H00H 2 0.397900 0.677489 0.153837 11.00000 -1.20000 AFIX 0 C00I 1 0.407897 0.529798 0.087964 11.00000 0.03686 0.04680 = 0.02426 0.00099 0.00431 -0.00202 AFIX 43 H00I 2 0.366045 0.559454 0.035879 11.00000 -1.20000 AFIX 0 C00J 1 0.817963 0.418757 0.549278 11.00000 0.03022 0.04380 = 0.02938 0.00299 0.00566 0.00108 AFIX 137 H00B 2 0.782217 0.341808 0.540042 11.00000 -1.50000 H00E 2 0.791006 0.464756 0.588787 11.00000 -1.50000 H00J 2 0.894985 0.407071 0.572055 11.00000 -1.50000 AFIX 0 C00K 1 0.616894 0.832030 0.552058 11.00000 0.04176 0.03319 = 0.03417 -0.00429 0.00839 -0.00009 AFIX 43 H00K 2 0.620836 0.915416 0.558572 11.00000 -1.20000 AFIX 0 C00L 1 0.471164 0.845955 0.273703 11.00000 0.03837 0.03855 = 0.02992 0.00433 0.01072 0.00184 AFIX 43 H00L 2 0.532459 0.850580 0.253822 11.00000 -1.20000 AFIX 0 C00M 1 0.447971 0.415452 0.092910 11.00000 0.03542 0.04421 = 0.02717 -0.00668 0.00760 -0.00532 AFIX 43 H00M 2 0.432964 0.366816 0.044668 11.00000 -1.20000 AFIX 0 C00N 1 0.835285 0.656614 0.466829 11.00000 0.02909 0.04463 = 0.04339 0.00216 0.00688 -0.00506 AFIX 137 H00N 2 0.804085 0.703082 0.416399 11.00000 -1.50000 H00O 2 0.913232 0.660188 0.480485 11.00000 -1.50000 H00P 2 0.811924 0.688895 0.513266 11.00000 -1.50000 AFIX 0 C00O 1 0.407156 0.944697 0.269486 11.00000 0.05309 0.03411 = 0.03066 0.00165 0.00621 0.00339 AFIX 43 H00Q 2 0.424972 1.016610 0.247295 11.00000 -1.20000 AFIX 0 C00P 1 0.715790 0.222925 0.285168 11.00000 0.03060 0.05134 = 0.03456 -0.00968 0.00881 0.00416 AFIX 43 H00R 2 0.723476 0.263491 0.237390 11.00000 -1.20000 AFIX 0 C00Q 1 0.317148 0.938319 0.297696 11.00000 0.04169 0.04050 = 0.03344 -0.00662 -0.00082 0.01166 AFIX 43 H00S 2 0.272950 1.005763 0.294678 11.00000 -1.20000 AFIX 0 C00R 1 0.876433 0.432519 0.387870 11.00000 0.02679 0.05770 = 0.03497 -0.00040 0.00870 0.00179 AFIX 137 H00T 2 0.851675 0.458471 0.329659 11.00000 -1.50000 H00U 2 0.872072 0.346234 0.390320 11.00000 -1.50000 H00V 2 0.950516 0.457543 0.411859 11.00000 -1.50000 AFIX 0 C00S 1 0.291836 0.833951 0.330147 11.00000 0.03214 0.04930 = 0.03759 -0.00753 0.00858 0.00519 AFIX 43 H00W 2 0.230162 0.829697 0.349572 11.00000 -1.20000 AFIX 0 C00T 1 0.691170 0.100315 0.421731 11.00000 0.04547 0.03615 = 0.04344 0.00100 0.00125 0.00253 AFIX 43 H00X 2 0.681568 0.057794 0.468138 11.00000 -1.20000 AFIX 0 C00U 1 0.754728 0.109540 0.300716 11.00000 0.03434 0.05778 = 0.04776 -0.02028 0.00286 0.01324 AFIX 43 H00Y 2 0.790108 0.073740 0.264393 11.00000 -1.20000 AFIX 0 C00W 1 0.742658 0.047693 0.368685 11.00000 0.04790 0.03909 = 0.05470 -0.01133 -0.00739 0.01603 AFIX 43 H00Z 2 0.769460 -0.030505 0.379106 11.00000 -1.20000 AFIX 0 HKLF 4 REM MaMi060_NeWi_a.res in P2(1)/n REM wR2 = 0.121425, GooF = S = 1.03547, Restrained GooF = 1.03547 for all data REM R1 = 0.044353 for 4182 Fo > 4sig(Fo) and 0.052132 for all 4819 data REM 292 parameters refined using 0 restraints END WGHT 0.0661 0.8978 REM Highest difference peak 0.344, deepest hole -0.448, 1-sigma level 0.046 Q1 1 0.5706 0.4288 0.2820 11.00000 0.05 0.34 Q2 1 0.4618 0.5788 0.1983 11.00000 0.05 0.29 Q3 1 0.8356 0.4792 0.5100 11.00000 0.05 0.27 Q4 1 0.5148 0.5026 0.2368 11.00000 0.05 0.25 Q5 1 0.5322 0.4171 0.2134 11.00000 0.05 0.23 Q6 1 0.6407 0.3481 0.3292 11.00000 0.05 0.23 Q7 1 0.5392 0.5994 0.3416 11.00000 0.05 0.22 Q8 1 0.6402 0.4526 0.3516 11.00000 0.05 0.22 Q9 1 0.4809 0.4045 0.1295 11.00000 0.05 0.22 Q10 1 0.5078 0.5977 0.2730 11.00000 0.05 0.22 Q11 1 0.7991 0.5966 0.4447 11.00000 0.05 0.20 Q12 1 0.5976 0.6399 0.4309 11.00000 0.05 0.20 Q13 1 0.8361 0.5565 0.4993 11.00000 0.05 0.19 Q14 1 0.5958 0.7248 0.4653 11.00000 0.05 0.19 Q15 1 0.7265 0.5048 0.3977 11.00000 0.05 0.19 Q16 1 0.6868 0.4799 0.4262 11.00000 0.05 0.19 Q17 1 0.4331 0.5672 0.1276 11.00000 0.05 0.18 Q18 1 0.6209 0.6264 0.5009 11.00000 0.05 0.17 Q19 1 0.6160 0.5530 0.3837 11.00000 0.05 0.16 Q20 1 0.4868 0.6871 0.3098 11.00000 0.05 0.16 ; _shelx_res_checksum 15321 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si01 Si 0.79074(3) 0.49981(4) 0.44842(3) 0.02948(13) Uani 1 1 d . . . . . N002 N 0.65280(10) 0.49693(12) 0.38629(8) 0.0272(3) Uani 1 1 d . . . . . C003 C 0.49349(12) 0.56017(15) 0.23497(9) 0.0278(3) Uani 1 1 d . . . . . C004 C 0.51494(12) 0.63259(14) 0.31030(9) 0.0271(3) Uani 1 1 d . . . . . C005 C 0.60047(12) 0.66051(14) 0.46364(9) 0.0278(3) Uani 1 1 d . . . . . C006 C 0.53613(12) 0.44444(15) 0.24077(9) 0.0280(3) Uani 1 1 d . . . . . C007 C 0.60472(12) 0.58979(15) 0.53304(9) 0.0284(3) Uani 1 1 d . . . . . H007 H 0.600264 0.506378 0.526844 0.034 Uiso 1 1 calc R U . . . C008 C 0.58900(12) 0.60029(14) 0.38180(9) 0.0273(3) Uani 1 1 d . . . . . C009 C 0.50973(13) 0.37320(16) 0.16848(10) 0.0320(3) Uani 1 1 d . . . . . H009 H 0.535132 0.294201 0.171980 0.038 Uiso 1 1 calc R U . . . C00A C 0.61536(12) 0.63958(16) 0.61097(10) 0.0319(4) Uani 1 1 d . . . . . H00A H 0.618265 0.590266 0.657575 0.038 Uiso 1 1 calc R U . . . C00B C 0.66501(12) 0.27989(15) 0.33833(10) 0.0308(3) Uani 1 1 d . . . . . C00C C 0.35593(13) 0.73505(16) 0.33461(10) 0.0333(4) Uani 1 1 d . . . . . H00C H 0.337706 0.663386 0.356861 0.040 Uiso 1 1 calc R U . . . B0 B 0.61801(14) 0.40800(17) 0.32296(11) 0.0281(4) Uani 1 1 d . . . . . C00D C 0.65390(13) 0.21473(15) 0.40687(10) 0.0335(4) Uani 1 1 d . . . . . H00D H 0.619791 0.250293 0.444119 0.040 Uiso 1 1 calc R U . . . C00E C 0.44690(12) 0.74016(14) 0.30665(9) 0.0285(3) Uani 1 1 d . . . . . C00F C 0.60639(13) 0.78284(15) 0.47419(10) 0.0328(4) Uani 1 1 d . . . . . H00F H 0.603203 0.832639 0.427769 0.039 Uiso 1 1 calc R U . . . C00G C 0.62172(14) 0.76068(16) 0.62069(10) 0.0360(4) Uani 1 1 d . . . . . H00G H 0.629343 0.795003 0.673944 0.043 Uiso 1 1 calc R U . . . C00H C 0.42820(13) 0.60068(16) 0.15780(10) 0.0334(4) Uani 1 1 d . . . . . H00H H 0.397900 0.677489 0.153837 0.040 Uiso 1 1 calc R U . . . C00I C 0.40790(14) 0.52980(17) 0.08796(10) 0.0368(4) Uani 1 1 d . . . . . H00I H 0.366045 0.559454 0.035879 0.044 Uiso 1 1 calc R U . . . C00J C 0.81796(13) 0.41876(16) 0.54928(10) 0.0350(4) Uani 1 1 d . . . . . H00B H 0.782217 0.341808 0.540042 0.053 Uiso 1 1 calc R U . . . H00E H 0.791006 0.464756 0.588787 0.053 Uiso 1 1 calc R U . . . H00J H 0.894985 0.407071 0.572055 0.053 Uiso 1 1 calc R U . . . C00K C 0.61689(14) 0.83203(16) 0.55206(10) 0.0368(4) Uani 1 1 d . . . . . H00K H 0.620836 0.915416 0.558572 0.044 Uiso 1 1 calc R U . . . C00L C 0.47116(14) 0.84596(16) 0.27370(10) 0.0354(4) Uani 1 1 d . . . . . H00L H 0.532459 0.850580 0.253822 0.042 Uiso 1 1 calc R U . . . C00M C 0.44797(14) 0.41545(16) 0.09291(10) 0.0358(4) Uani 1 1 d . . . . . H00M H 0.432964 0.366816 0.044668 0.043 Uiso 1 1 calc R U . . . C00N C 0.83528(14) 0.65661(17) 0.46683(12) 0.0397(4) Uani 1 1 d . . . . . H00N H 0.804085 0.703082 0.416399 0.060 Uiso 1 1 calc R U . . . H00O H 0.913232 0.660188 0.480485 0.060 Uiso 1 1 calc R U . . . H00P H 0.811924 0.688895 0.513266 0.060 Uiso 1 1 calc R U . . . C00O C 0.40716(16) 0.94470(17) 0.26949(11) 0.0404(4) Uani 1 1 d . . . . . H00Q H 0.424972 1.016610 0.247295 0.048 Uiso 1 1 calc R U . . . C00P C 0.71579(13) 0.22293(17) 0.28517(11) 0.0389(4) Uani 1 1 d . . . . . H00R H 0.723476 0.263491 0.237390 0.047 Uiso 1 1 calc R U . . . C00Q C 0.31715(15) 0.93832(17) 0.29770(11) 0.0408(4) Uani 1 1 d . . . . . H00S H 0.272950 1.005763 0.294678 0.049 Uiso 1 1 calc R U . . . C00R C 0.87643(13) 0.43252(18) 0.38787(11) 0.0398(4) Uani 1 1 d . . . . . H00T H 0.851675 0.458471 0.329659 0.060 Uiso 1 1 calc R U . . . H00U H 0.872072 0.346234 0.390320 0.060 Uiso 1 1 calc R U . . . H00V H 0.950516 0.457543 0.411859 0.060 Uiso 1 1 calc R U . . . C00S C 0.29184(14) 0.83395(17) 0.33015(11) 0.0399(4) Uani 1 1 d . . . . . H00W H 0.230162 0.829697 0.349572 0.048 Uiso 1 1 calc R U . . . C00T C 0.69117(16) 0.10031(17) 0.42173(12) 0.0439(4) Uani 1 1 d . . . . . H00X H 0.681568 0.057794 0.468138 0.053 Uiso 1 1 calc R U . . . C00U C 0.75473(15) 0.10954(19) 0.30072(13) 0.0484(5) Uani 1 1 d . . . . . H00Y H 0.790108 0.073740 0.264393 0.058 Uiso 1 1 calc R U . . . C00W C 0.74266(17) 0.04769(19) 0.36868(13) 0.0516(5) Uani 1 1 d . . . . . H00Z H 0.769460 -0.030505 0.379106 0.062 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 Si01 0.0248(2) 0.0377(3) 0.0254(2) 0.00085(17) 0.00621(17) -0.00056(17) N002 0.0267(6) 0.0326(7) 0.0237(6) 0.0011(5) 0.0092(5) 0.0008(5) C003 0.0255(7) 0.0351(8) 0.0243(7) 0.0000(6) 0.0095(6) -0.0030(6) C004 0.0274(7) 0.0316(8) 0.0241(7) 0.0015(6) 0.0098(6) -0.0006(6) C005 0.0241(7) 0.0349(8) 0.0242(7) -0.0008(6) 0.0063(6) 0.0008(6) C006 0.0255(7) 0.0351(8) 0.0257(7) -0.0004(6) 0.0112(6) -0.0033(6) C007 0.0245(7) 0.0339(8) 0.0270(7) -0.0002(6) 0.0076(6) -0.0010(6) C008 0.0275(7) 0.0297(8) 0.0264(7) 0.0003(6) 0.0101(6) -0.0018(6) C009 0.0288(8) 0.0370(9) 0.0310(8) -0.0036(7) 0.0096(6) -0.0026(7) C00A 0.0291(8) 0.0412(9) 0.0264(7) 0.0010(7) 0.0094(6) -0.0001(7) C00B 0.0255(7) 0.0369(9) 0.0294(8) -0.0045(6) 0.0065(6) 0.0009(6) C00C 0.0308(8) 0.0388(9) 0.0310(8) -0.0008(7) 0.0097(7) 0.0008(7) B0 0.0263(8) 0.0346(9) 0.0261(8) -0.0012(7) 0.0120(7) -0.0023(7) C00D 0.0323(8) 0.0342(9) 0.0318(8) -0.0027(7) 0.0054(7) 0.0014(7) C00E 0.0295(7) 0.0334(8) 0.0218(7) 0.0000(6) 0.0060(6) 0.0011(6) C00F 0.0366(9) 0.0341(9) 0.0273(8) 0.0000(6) 0.0081(7) -0.0013(7) C00G 0.0380(9) 0.0432(10) 0.0269(7) -0.0065(7) 0.0093(7) 0.0007(8) C00H 0.0333(8) 0.0378(9) 0.0288(8) 0.0015(7) 0.0081(7) 0.0001(7) C00I 0.0369(9) 0.0468(10) 0.0243(8) 0.0010(7) 0.0043(7) -0.0020(8) C00J 0.0302(8) 0.0438(10) 0.0294(8) 0.0030(7) 0.0057(6) 0.0011(7) C00K 0.0418(9) 0.0332(9) 0.0342(8) -0.0043(7) 0.0084(7) -0.0001(7) C00L 0.0384(9) 0.0385(9) 0.0299(8) 0.0043(7) 0.0107(7) 0.0018(7) C00M 0.0354(8) 0.0442(10) 0.0272(8) -0.0067(7) 0.0076(7) -0.0053(7) C00N 0.0291(8) 0.0446(10) 0.0434(9) 0.0022(8) 0.0069(7) -0.0051(7) C00O 0.0531(11) 0.0341(9) 0.0307(8) 0.0016(7) 0.0062(8) 0.0034(8) C00P 0.0306(8) 0.0513(11) 0.0346(9) -0.0097(8) 0.0088(7) 0.0042(8) C00Q 0.0417(9) 0.0405(10) 0.0334(8) -0.0066(8) -0.0008(7) 0.0117(8) C00R 0.0268(8) 0.0577(12) 0.0350(9) -0.0004(8) 0.0087(7) 0.0018(8) C00S 0.0321(8) 0.0493(11) 0.0376(9) -0.0075(8) 0.0086(7) 0.0052(8) C00T 0.0455(10) 0.0362(10) 0.0434(10) 0.0010(8) 0.0012(8) 0.0025(8) C00U 0.0343(9) 0.0578(12) 0.0478(11) -0.0203(9) 0.0029(8) 0.0132(9) C00W 0.0479(11) 0.0391(10) 0.0547(12) -0.0113(9) -0.0074(9) 0.0160(9) 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 0 1 0.0117 2 -1 0 0.0324 -2 1 0 0.0579 0 -1 2 0.0366 2 -1 -1 0.0473 1 -2 0 0.0617 2 -1 -2 0.0588 -2 1 2 0.0395 1 1 -2 0.0817 1 1 -1 0.0849 0 -1 -1 0.0757 0 -1 -2 0.0698 -2 -2 -1 0.0641 -2 -1 1 0.0506 1 0 -2 0.0538 -2 -1 -2 0.0487 -1 0 -1 0.0294 2 0 1 0.0552 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 N002 Si01 C00J 114.66(7) . . ? N002 Si01 C00N 109.02(7) . . ? C00J Si01 C00N 110.34(8) . . ? N002 Si01 C00R 109.46(7) . . ? C00J Si01 C00R 107.27(8) . . ? C00N Si01 C00R 105.71(9) . . ? C008 N002 B0 118.39(13) . . ? C008 N002 Si01 119.24(10) . . ? B0 N002 Si01 119.55(11) . . ? C00H C003 C006 119.33(14) . . ? C00H C003 C004 121.75(15) . . ? C006 C003 C004 118.87(14) . . ? C008 C004 C003 121.55(15) . . ? C008 C004 C00E 121.49(14) . . ? C003 C004 C00E 116.86(13) . . ? C00F C005 C007 118.43(14) . . ? C00F C005 C008 123.72(14) . . ? C007 C005 C008 117.85(14) . . ? C009 C006 C003 118.19(14) . . ? C009 C006 B0 123.45(15) . . ? C003 C006 B0 118.04(14) . . ? C00A C007 C005 121.01(15) . . ? C00A C007 H007 119.5 . . ? C005 C007 H007 119.5 . . ? C004 C008 N002 121.90(14) . . ? C004 C008 C005 122.99(14) . . ? N002 C008 C005 114.69(13) . . ? C00M C009 C006 121.65(16) . . ? C00M C009 H009 119.2 . . ? C006 C009 H009 119.2 . . ? C00G C00A C007 120.01(15) . . ? C00G C00A H00A 120.0 . . ? C007 C00A H00A 120.0 . . ? C00D C00B C00P 116.69(16) . . ? C00D C00B B0 119.67(14) . . ? C00P C00B B0 123.61(15) . . ? C00S C00C C00E 120.43(17) . . ? C00S C00C H00C 119.8 . . ? C00E C00C H00C 119.8 . . ? N002 B0 C006 117.73(15) . . ? N002 B0 C00B 119.88(14) . . ? C006 B0 C00B 122.39(14) . . ? C00T C00D C00B 121.87(17) . . ? C00T C00D H00D 119.1 . . ? C00B C00D H00D 119.1 . . ? C00L C00E C00C 118.55(15) . . ? C00L C00E C004 121.17(14) . . ? C00C C00E C004 120.26(14) . . ? C00K C00F C005 120.31(15) . . ? C00K C00F H00F 119.8 . . ? C005 C00F H00F 119.8 . . ? C00A C00G C00K 119.54(15) . . ? C00A C00G H00G 120.2 . . ? C00K C00G H00G 120.2 . . ? C00I C00H C003 120.57(16) . . ? C00I C00H H00H 119.7 . . ? C003 C00H H00H 119.7 . . ? C00H C00I C00M 120.75(16) . . ? C00H C00I H00I 119.6 . . ? C00M C00I H00I 119.6 . . ? Si01 C00J H00B 109.5 . . ? Si01 C00J H00E 109.5 . . ? H00B C00J H00E 109.5 . . ? Si01 C00J H00J 109.5 . . ? H00B C00J H00J 109.5 . . ? H00E C00J H00J 109.5 . . ? C00F C00K C00G 120.69(16) . . ? C00F C00K H00K 119.7 . . ? C00G C00K H00K 119.7 . . ? C00O C00L C00E 120.91(16) . . ? C00O C00L H00L 119.5 . . ? C00E C00L H00L 119.5 . . ? C009 C00M C00I 119.43(15) . . ? C009 C00M H00M 120.3 . . ? C00I C00M H00M 120.3 . . ? Si01 C00N H00N 109.5 . . ? Si01 C00N H00O 109.5 . . ? H00N C00N H00O 109.5 . . ? Si01 C00N H00P 109.5 . . ? H00N C00N H00P 109.5 . . ? H00O C00N H00P 109.5 . . ? C00Q C00O C00L 119.86(17) . . ? C00Q C00O H00Q 120.1 . . ? C00L C00O H00Q 120.1 . . ? C00U C00P C00B 121.53(18) . . ? C00U C00P H00R 119.2 . . ? C00B C00P H00R 119.2 . . ? C00S C00Q C00O 119.87(17) . . ? C00S C00Q H00S 120.1 . . ? C00O C00Q H00S 120.1 . . ? Si01 C00R H00T 109.5 . . ? Si01 C00R H00U 109.5 . . ? H00T C00R H00U 109.5 . . ? Si01 C00R H00V 109.5 . . ? H00T C00R H00V 109.5 . . ? H00U C00R H00V 109.5 . . ? C00Q C00S C00C 120.36(16) . . ? C00Q C00S H00W 119.8 . . ? C00C C00S H00W 119.8 . . ? C00D C00T C00W 119.81(19) . . ? C00D C00T H00X 120.1 . . ? C00W C00T H00X 120.1 . . ? C00P C00U C00W 120.44(18) . . ? C00P C00U H00Y 119.8 . . ? C00W C00U H00Y 119.8 . . ? C00U C00W C00T 119.65(18) . . ? C00U C00W H00Z 120.2 . . ? C00T C00W H00Z 120.2 . . ? 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 N002 1.8108(14) . ? Si01 C00J 1.8631(17) . ? Si01 C00N 1.8666(19) . ? Si01 C00R 1.8677(17) . ? N002 C008 1.426(2) . ? N002 B0 1.439(2) . ? C003 C00H 1.409(2) . ? C003 C006 1.416(2) . ? C003 C004 1.462(2) . ? C004 C008 1.360(2) . ? C004 C00E 1.499(2) . ? C005 C00F 1.395(2) . ? C005 C007 1.397(2) . ? C005 C008 1.497(2) . ? C006 C009 1.412(2) . ? C006 B0 1.542(2) . ? C007 C00A 1.389(2) . ? C007 H007 0.9500 . ? C009 C00M 1.380(2) . ? C009 H009 0.9500 . ? C00A C00G 1.380(2) . ? C00A H00A 0.9500 . ? C00B C00D 1.403(2) . ? C00B C00P 1.405(2) . ? C00B B0 1.568(2) . ? C00C C00S 1.387(2) . ? C00C C00E 1.394(2) . ? C00C H00C 0.9500 . ? C00D C00T 1.382(2) . ? C00D H00D 0.9500 . ? C00E C00L 1.391(2) . ? C00F C00K 1.386(2) . ? C00F H00F 0.9500 . ? C00G C00K 1.389(2) . ? C00G H00G 0.9500 . ? C00H C00I 1.379(2) . ? C00H H00H 0.9500 . ? C00I C00M 1.390(3) . ? C00I H00I 0.9500 . ? C00J H00B 0.9800 . ? C00J H00E 0.9800 . ? C00J H00J 0.9800 . ? C00K H00K 0.9500 . ? C00L C00O 1.386(3) . ? C00L H00L 0.9500 . ? C00M H00M 0.9500 . ? C00N H00N 0.9800 . ? C00N H00O 0.9800 . ? C00N H00P 0.9800 . ? C00O C00Q 1.385(3) . ? C00O H00Q 0.9500 . ? C00P C00U 1.378(3) . ? C00P H00R 0.9500 . ? C00Q C00S 1.378(3) . ? C00Q H00S 0.9500 . ? C00R H00T 0.9800 . ? C00R H00U 0.9800 . ? C00R H00V 0.9800 . ? C00S H00W 0.9500 . ? C00T C00W 1.387(3) . ? C00T H00X 0.9500 . ? C00U C00W 1.380(3) . ? C00U H00Y 0.9500 . ? C00W H00Z 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 C00J Si01 N002 C008 105.27(12) . . . . ? C00N Si01 N002 C008 -18.98(13) . . . . ? C00R Si01 N002 C008 -134.16(12) . . . . ? C00J Si01 N002 B0 -94.02(13) . . . . ? C00N Si01 N002 B0 141.73(12) . . . . ? C00R Si01 N002 B0 26.54(14) . . . . ? C00H C003 C004 C008 -170.98(15) . . . . ? C006 C003 C004 C008 11.6(2) . . . . ? C00H C003 C004 C00E 12.7(2) . . . . ? C006 C003 C004 C00E -164.72(13) . . . . ? C00H C003 C006 C009 -1.0(2) . . . . ? C004 C003 C006 C009 176.48(13) . . . . ? C00H C003 C006 B0 172.69(14) . . . . ? C004 C003 C006 B0 -9.8(2) . . . . ? C00F C005 C007 C00A -0.5(2) . . . . ? C008 C005 C007 C00A 179.97(14) . . . . ? C003 C004 C008 N002 2.7(2) . . . . ? C00E C004 C008 N002 178.87(13) . . . . ? C003 C004 C008 C005 -169.42(14) . . . . ? C00E C004 C008 C005 6.8(2) . . . . ? B0 N002 C008 C004 -18.2(2) . . . . ? Si01 N002 C008 C004 142.76(13) . . . . ? B0 N002 C008 C005 154.55(13) . . . . ? Si01 N002 C008 C005 -44.52(16) . . . . ? C00F C005 C008 C004 -49.0(2) . . . . ? C007 C005 C008 C004 130.53(16) . . . . ? C00F C005 C008 N002 138.35(16) . . . . ? C007 C005 C008 N002 -42.11(19) . . . . ? C003 C006 C009 C00M 2.8(2) . . . . ? B0 C006 C009 C00M -170.55(15) . . . . ? C005 C007 C00A C00G 0.1(2) . . . . ? C008 N002 B0 C006 18.8(2) . . . . ? Si01 N002 B0 C006 -142.08(11) . . . . ? C008 N002 B0 C00B -162.35(13) . . . . ? Si01 N002 B0 C00B 36.78(18) . . . . ? C009 C006 B0 N002 168.27(14) . . . . ? C003 C006 B0 N002 -5.1(2) . . . . ? C009 C006 B0 C00B -10.6(2) . . . . ? C003 C006 B0 C00B 176.12(13) . . . . ? C00D C00B B0 N002 58.4(2) . . . . ? C00P C00B B0 N002 -123.85(17) . . . . ? C00D C00B B0 C006 -122.82(17) . . . . ? C00P C00B B0 C006 55.0(2) . . . . ? C00P C00B C00D C00T 0.2(2) . . . . ? B0 C00B C00D C00T 178.09(16) . . . . ? C00S C00C C00E C00L -0.5(2) . . . . ? C00S C00C C00E C004 -179.01(15) . . . . ? C008 C004 C00E C00L 99.77(18) . . . . ? C003 C004 C00E C00L -83.89(19) . . . . ? C008 C004 C00E C00C -81.8(2) . . . . ? C003 C004 C00E C00C 94.54(17) . . . . ? C007 C005 C00F C00K 0.4(2) . . . . ? C008 C005 C00F C00K 179.94(15) . . . . ? C007 C00A C00G C00K 0.3(3) . . . . ? C006 C003 C00H C00I -1.6(2) . . . . ? C004 C003 C00H C00I -178.97(15) . . . . ? C003 C00H C00I C00M 2.5(3) . . . . ? C005 C00F C00K C00G 0.0(3) . . . . ? C00A C00G C00K C00F -0.4(3) . . . . ? C00C C00E C00L C00O 0.7(2) . . . . ? C004 C00E C00L C00O 179.14(15) . . . . ? C006 C009 C00M C00I -1.9(2) . . . . ? C00H C00I C00M C009 -0.7(3) . . . . ? C00E C00L C00O C00Q -0.6(3) . . . . ? C00D C00B C00P C00U -1.3(3) . . . . ? B0 C00B C00P C00U -179.18(16) . . . . ? C00L C00O C00Q C00S 0.3(3) . . . . ? C00O C00Q C00S C00C -0.1(3) . . . . ? C00E C00C C00S C00Q 0.3(3) . . . . ? C00B C00D C00T C00W 1.0(3) . . . . ? C00B C00P C00U C00W 1.4(3) . . . . ? C00P C00U C00W C00T -0.1(3) . . . . ? C00D C00T C00W C00U -1.0(3) . . . . ?