#------------------------------------------------------------------------------ #$Date: 2019-11-11 16:45:18 +0200 (Mon, 11 Nov 2019) $ #$Revision: 226607 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/51/4035121.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_4035121 loop_ _publ_author_name 'Andresini, Michael' 'De Angelis, Sonia' 'Uricchio, Antonella' 'Visaggio, Angelica' 'Romanazzi, Giuseppe' 'Ciriaco, Fulvio' 'Corriero, Nicola' 'Degennaro, Leonardo' 'Luisi, Renzo' _publ_section_title ; Azetidine-Borane Complexes: Synthesis, Reactivity, and Stereoselective Functionalization. ; _journal_issue 17 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 10221 _journal_page_last 10230 _journal_paper_doi 10.1021/acs.joc.8b01441 _journal_volume 83 _journal_year 2018 _chemical_formula_sum 'C11 H18 B N' _chemical_formula_weight 175.07 _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 mixed _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 104.30(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.820(5) _cell_length_b 6.017(1) _cell_length_c 14.764(5) _cell_measurement_reflns_used 130 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2 _cell_volume 1103.6(6) _computing_cell_refinement 'DIRAX (Duisenberg,1992; Duisenberg et al., 2000)' _computing_data_collection 'COLLECT (Nonius, 2002)' _computing_data_reduction 'EVAL (Nonius, 2002; Duisenberg et al., 2003)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SIR2014 (Burla et al., 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0911 _diffrn_reflns_av_unetI/netI 0.0626 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 11147 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.509 _diffrn_reflns_theta_min 3.674 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.059 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS(Sheldrick, 2008)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.054 _exptl_crystal_description block _exptl_crystal_F_000 384 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_transmission_factor_max 0.7456 _exptl_transmission_factor_min 0.4793 _refine_diff_density_max 0.240 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 2521 _refine_ls_number_restraints 33 _refine_ls_restrained_S_all 0.998 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0701 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1454P)^2^+0.0610P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1986 _refine_ls_wR_factor_ref 0.2311 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1619 _reflns_number_total 2521 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b01441_si_001.cif _cod_data_source_block shelx _cod_original_cell_volume 1103.6(5) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 4035121 _shelx_shelxl_version_number 2014/7 _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 ; shelx.res created by SHELXL-2014/7 TITL sir: ---- AUR_2-3 CELL 0.71073 12.8200 6.0170 14.7640 90.000 104.300 90.000 ZERR 4.00 0.0000 0.0000 0.0000 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H B N UNIT 44 72 4 4 MERG 2 FMAP 2 PLAN 20 DELU HTAB L.S. 8 ACTA WGHT 0.145400 0.061000 FVAR 1.36152 N1 4 0.192132 0.219916 0.909364 11.00000 0.05845 0.03616 = 0.05585 0.00089 0.01881 -0.00115 C1 1 0.283534 0.093768 1.080682 11.00000 0.05451 0.04733 = 0.05054 -0.01067 0.00859 0.00252 C2 1 0.227536 0.270862 1.015164 11.00000 0.05034 0.03817 = 0.05858 -0.00933 0.01210 -0.00182 AFIX 13 H2 2 0.273386 0.403386 1.024193 11.00000 -1.20000 AFIX 0 C3 1 0.396327 0.087345 1.112158 11.00000 0.05628 0.07116 = 0.06313 -0.02034 0.00824 0.00740 C4 1 0.223545 -0.064305 1.114974 11.00000 0.06921 0.05960 = 0.05667 -0.00065 0.00563 -0.00133 AFIX 43 H4 2 0.148925 -0.060672 1.094120 11.00000 -1.20000 AFIX 0 C5 1 0.111702 0.343508 1.011642 11.00000 0.05898 0.05755 = 0.07219 -0.00695 0.01827 0.01280 AFIX 23 H5A 2 0.068552 0.229940 1.031646 11.00000 -1.20000 H5B 2 0.106621 0.484149 1.042379 11.00000 -1.20000 AFIX 0 C6 1 0.093983 0.361006 0.906116 11.00000 0.06240 0.04901 = 0.07352 0.00354 0.01076 0.01168 AFIX 23 H6A 2 0.027388 0.293065 0.871585 11.00000 -1.20000 H6B 2 0.100326 0.511443 0.884473 11.00000 -1.20000 AFIX 0 C7 1 0.264695 0.308454 0.853554 11.00000 0.09540 0.06630 = 0.08349 0.00287 0.04586 -0.01169 AFIX 37 H7A 2 0.329884 0.222834 0.866263 11.00000 -1.50000 H7B 2 0.281492 0.460913 0.870105 11.00000 -1.50000 H7C 2 0.229600 0.298833 0.788229 11.00000 -1.50000 AFIX 0 C8 1 0.441153 -0.081669 1.176360 11.00000 0.06817 0.10780 = 0.06490 -0.01680 -0.00021 0.03493 AFIX 43 H8 2 0.515621 -0.090447 1.197711 11.00000 -1.20000 AFIX 0 C9 1 0.269949 -0.225444 1.178330 11.00000 0.10696 0.06723 = 0.05673 0.00434 0.00943 0.00379 AFIX 43 H9 2 0.227457 -0.327382 1.200258 11.00000 -1.20000 AFIX 0 B1 3 0.160486 -0.032669 0.881148 11.00000 0.07923 0.04396 = 0.05920 -0.01214 0.01707 -0.00753 H3B 2 0.237156 -0.130189 0.898737 11.00000 -1.50000 H2B 2 0.103008 -0.091428 0.919500 11.00000 -1.50000 H1B 2 0.124188 -0.028783 0.805474 11.00000 -1.50000 C11 1 0.379045 -0.232858 1.208266 11.00000 0.11120 0.08755 = 0.05904 0.00397 0.00809 0.03236 AFIX 43 H11 2 0.411626 -0.341457 1.250715 11.00000 -1.20000 AFIX 0 C12 1 0.468409 0.250794 1.081110 11.00000 0.05374 0.10836 = 0.11424 -0.02221 0.02047 -0.00730 AFIX 37 H12A 2 0.442420 0.398775 1.086148 11.00000 -1.50000 H12B 2 0.468869 0.221391 1.017301 11.00000 -1.50000 H12C 2 0.540169 0.237045 1.119970 11.00000 -1.50000 AFIX 0 HKLF 4 REM sir: ---- AUR_2-3 REM R1 = 0.0701 for 1619 Fo > 4sig(Fo) and 0.1045 for all 2521 data REM 129 parameters refined using 33 restraints END WGHT 0.1289 0.0743 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.240, deepest hole -0.207, 1-sigma level 0.048 Q1 1 0.3400 0.0593 1.0795 11.00000 0.05 0.24 Q2 1 0.4383 0.3584 1.0193 11.00000 0.05 0.18 Q3 1 0.5400 0.1698 1.0677 11.00000 0.05 0.18 Q4 1 0.3246 -0.2065 1.1554 11.00000 0.05 0.18 Q5 1 0.0722 -0.0587 0.9144 11.00000 0.05 0.16 Q6 1 0.4505 -0.1503 1.1993 11.00000 0.05 0.15 Q7 1 0.4880 -0.2554 1.2530 11.00000 0.05 0.15 Q8 1 0.3358 0.3636 0.9004 11.00000 0.05 0.15 Q9 1 0.2485 -0.1087 0.8821 11.00000 0.05 0.14 Q10 1 0.1586 -0.0718 0.8142 11.00000 0.05 0.13 Q11 1 0.4017 -0.3479 1.1132 11.00000 0.05 0.13 Q12 1 0.2345 -0.2424 0.9573 11.00000 0.05 0.12 Q13 1 0.4987 -0.0007 1.1564 11.00000 0.05 0.12 Q14 1 0.1278 -0.0266 1.0945 11.00000 0.05 0.12 Q15 1 0.2241 0.2354 0.9562 11.00000 0.05 0.12 Q16 1 0.1665 0.2971 1.0169 11.00000 0.05 0.11 Q17 1 0.4003 0.4917 0.8807 11.00000 0.05 0.11 Q18 1 0.0758 -0.1765 0.7207 11.00000 0.05 0.11 Q19 1 0.3427 -0.2171 1.0677 11.00000 0.05 0.11 Q20 1 0.3067 0.6976 1.0174 11.00000 0.05 0.10 ; _shelx_res_checksum 91054 _shelx_hkl_file ; -3 0 0 2.20264 1.28506 5 -3 0 0 1.63771 1.55721 1 3 0 0 1.50854 1.39525 5 -4 0 0 633.532 53.210 6 -5 0 0 -2.0501 2.0238 1 -5 0 0 -2.0522 1.2741 6 -5 0 0 -0.6260 1.2271 5 5 0 0 1.06930 1.61482 1 5 0 0 -2.4103 1.7945 5 -6 0 0 2835.48 279.08 1 -6 0 0 2775.85 249.44 6 6 0 0 3289.70 254.71 1 6 0 0 2652.83 242.82 5 -7 0 0 0.20391 1.24854 6 -7 0 0 -1.9210 2.3135 1 7 0 0 -1.4078 3.0245 1 7 0 0 -1.9180 2.1719 5 7 0 0 0.16235 1.56024 4 8 0 0 112.432 10.765 1 8 0 0 101.905 9.704 5 -9 0 0 -0.4312 1.8487 6 9 0 0 3.60412 3.26017 1 9 0 0 -0.4735 2.5449 5 -10 0 0 84.4972 8.0710 6 10 0 0 89.7115 8.6106 5 10 0 0 97.9676 9.6812 1 -11 0 0 -1.7249 2.1553 6 11 0 0 2.42354 2.65763 1 11 0 0 -4.4461 2.9929 5 -12 0 0 36.5228 4.2931 6 12 0 0 41.3748 5.2111 5 12 0 0 33.7330 5.3085 1 13 0 0 2.47715 3.92918 1 14 0 0 11.5357 3.8571 5 15 0 0 -6.6938 4.9193 1 16 0 0 30.3477 6.7324 1 16 -1 0 0.82697 5.37094 1 15 -1 0 1.94274 5.32170 1 15 -1 0 -3.3245 3.5906 5 14 -1 0 15.9485 4.5142 5 14 -1 0 12.8552 5.2221 1 13 -1 0 18.6254 5.1911 1 13 -1 0 13.7743 3.6498 5 12 -1 0 0.65057 4.09624 1 11 -1 0 8.21223 4.44252 1 11 -1 0 14.3765 4.0291 5 10 -1 0 13.8319 2.9316 5 10 -1 0 16.1226 3.4205 1 -10 1 0 10.2910 1.6955 6 9 -1 0 109.757 10.074 5 9 -1 0 107.007 10.757 1 8 -1 0 352.503 31.624 1 8 -1 0 349.229 29.701 5 7 -1 0 145.231 11.574 5 -7 1 0 113.691 10.968 2 6 -1 0 64.2911 5.9248 1 -6 1 0 53.2954 5.7994 1 -6 1 0 53.6047 5.0805 2 5 -1 0 1039.01 89.83 5 -5 1 0 1015.76 100.04 1 -5 1 0 1192.26 92.66 2 4 -1 0 6.89330 1.66270 1 -4 1 0 6.54299 1.31897 2 -4 1 0 4.85756 1.38073 1 -3 1 0 256.886 22.258 2 -3 1 0 283.736 23.868 1 2 -1 0 3017.78 294.53 1 -2 1 0 3430.70 286.89 1 1 -1 0 2206.46 189.06 1 1 -1 0 1949.30 175.81 6 -1 1 0 2327.49 189.23 1 0 -1 0 -6.7048 0.5242 4 0 -1 0 -6.7652 0.4121 1 -1 -1 0 2906.13 219.54 3 1 1 0 2303.66 226.39 4 1 1 0 2975.84 237.25 1 1 1 0 2719.44 219.52 3 -2 -1 0 3590.31 327.59 4 -2 -1 0 4309.59 344.37 1 2 1 0 3831.02 328.33 4 2 1 0 3998.80 343.72 1 2 1 0 3999.59 317.81 3 -3 -1 0 351.134 29.361 4 -3 -1 0 358.433 28.920 5 -3 -1 0 328.833 30.843 1 3 1 0 373.337 30.898 1 3 1 0 335.050 29.327 4 -4 -1 0 7.48385 1.55017 6 -4 -1 0 5.46044 1.58475 1 4 1 0 7.11874 1.54351 4 4 1 0 10.4542 2.2710 1 -5 -1 0 1326.38 97.89 5 -5 -1 0 1087.83 95.63 6 -5 -1 0 992.591 102.662 1 5 1 0 1222.81 96.16 4 5 1 0 1181.95 100.07 1 5 1 0 1001.66 107.69 2 -6 -1 0 76.1725 7.3521 1 -6 -1 0 68.1741 6.4371 5 6 1 0 78.6434 6.5769 5 6 1 0 66.2390 7.1714 1 6 1 0 70.9711 6.8674 4 -7 -1 0 110.907 11.361 1 -7 -1 0 117.752 10.487 5 7 1 0 105.293 10.576 4 7 1 0 138.013 10.395 5 -8 -1 0 352.135 27.935 6 8 1 0 356.216 30.365 1 8 1 0 299.822 28.075 5 -9 -1 0 104.916 9.700 6 9 1 0 108.911 9.644 5 -10 -1 0 22.6372 3.5211 6 10 1 0 19.0219 3.2656 5 10 1 0 17.4958 4.1580 1 -11 -1 0 4.35024 3.10115 6 11 1 0 10.5190 4.3860 1 11 1 0 3.45360 2.63003 5 -12 -1 0 2.88096 3.02788 6 12 1 0 2.20085 2.73616 5 12 1 0 -2.7647 2.9039 1 -13 -1 0 6.85785 2.80537 6 13 1 0 16.0003 4.4630 1 -14 -1 0 2.62513 3.14044 6 14 1 0 1.61689 4.24179 1 15 1 0 2.64792 4.84609 1 16 1 0 3.13158 3.46834 1 15 -2 0 1.75250 5.48548 1 15 -2 0 1.78465 3.12500 5 14 -2 0 17.7122 5.8271 1 13 -2 0 -2.2855 3.8830 5 13 -2 0 1.88209 4.72245 1 12 -2 0 2.82847 3.48898 5 12 -2 0 3.21821 4.33874 1 11 -2 0 24.5117 3.9288 5 11 -2 0 26.5744 4.6410 1 10 -2 0 5.24873 4.12889 1 10 -2 0 13.4649 4.0206 5 9 -2 0 18.5466 4.2456 5 9 -2 0 25.6325 4.5124 1 -9 2 0 18.1869 3.0278 2 8 -2 0 8.5131 15.3598 1 -8 2 0 8.29007 5.59676 2 -8 2 0 10.8572 3.1007 1 7 -2 0 176.613 15.402 1 -7 2 0 161.700 14.225 2 -7 2 0 158.446 15.259 1 6 -2 0 44.9339 4.9458 1 -6 2 0 40.4051 4.8147 1 -6 2 0 49.3822 4.6418 2 5 -2 0 385.770 35.955 1 -5 2 0 430.539 33.710 2 -5 2 0 403.009 35.957 1 4 -2 0 1043.70 88.01 1 -4 2 0 841.323 90.048 1 -4 2 0 1109.26 82.02 2 3 -2 0 195.112 19.343 6 -3 2 0 220.236 18.977 1 -2 2 0 745.606 61.717 1 -2 2 0 666.694 57.922 2 1 -2 0 2125.59 189.87 6 1 -2 0 2498.85 203.70 1 -1 2 0 2515.10 189.61 2 -1 2 0 2171.65 202.97 1 0 -2 0 4703.79 454.31 1 0 -2 0 5328.97 453.51 1 0 -2 0 5289.66 419.71 6 0 -2 0 5368.62 432.01 4 0 2 0 5253.64 421.81 2 -1 -2 0 2382.28 192.04 6 -1 -2 0 2187.41 191.10 3 -1 -2 0 2248.59 207.20 1 -1 -2 0 2461.57 196.98 4 1 2 0 2548.00 197.00 4 1 2 0 2475.56 193.01 2 1 2 0 2292.07 206.39 1 -2 -2 0 676.116 59.854 4 -2 -2 0 709.264 58.191 3 -2 -2 0 722.400 62.867 1 -2 -2 0 753.918 58.621 6 2 2 0 729.782 62.869 1 2 2 0 712.756 59.882 4 2 2 0 722.609 58.811 2 -3 -2 0 318.917 29.143 4 -3 -2 0 359.205 30.784 1 -3 -2 0 364.248 28.431 3 -3 -2 0 343.118 28.696 6 3 2 0 351.300 30.781 1 3 2 0 362.711 28.393 3 3 2 0 352.104 28.715 2 3 2 0 323.677 29.162 4 -4 -2 0 1051.27 85.57 4 -4 -2 0 972.246 83.507 6 -4 -2 0 1001.12 89.99 1 4 2 0 1026.33 85.64 4 4 2 0 1124.76 83.00 3 4 2 0 978.853 89.777 1 -5 -2 0 405.036 37.777 1 -5 -2 0 433.558 35.367 5 -5 -2 0 448.567 35.209 6 5 2 0 461.954 37.872 1 5 2 0 390.157 34.968 2 5 2 0 441.474 35.987 4 5 2 0 398.130 34.674 3 -6 -2 0 38.5321 5.0201 1 -6 -2 0 55.9253 5.2724 6 -6 -2 0 51.1418 4.5022 5 6 2 0 49.6783 5.0786 4 6 2 0 44.5905 4.3660 2 6 2 0 49.5054 5.5186 1 6 2 0 39.8380 4.3159 3 -7 -2 0 208.288 19.776 5 7 2 0 255.788 20.553 1 7 2 0 222.017 19.240 4 7 2 0 196.620 18.656 3 8 2 0 8.72247 3.08456 4 8 2 0 6.40162 1.24998 2 8 2 0 8.95715 3.79232 1 -9 -2 0 24.2236 4.3183 6 9 2 0 26.5598 4.9501 1 -10 -2 0 5.54975 1.67200 5 -10 -2 0 9.75268 3.83967 6 -11 -2 0 24.0113 4.5121 6 11 2 0 27.0152 4.3985 1 -12 -2 0 4.85730 3.20929 6 12 2 0 7.78572 4.04143 1 -13 -2 0 1.45745 3.87992 6 13 2 0 4.71504 3.04095 1 -14 -2 0 -1.0026 3.1399 6 14 2 0 12.9049 4.7181 1 15 2 0 -0.3952 4.3918 1 14 -3 0 16.2751 5.1277 5 14 -3 0 9.95391 5.34790 1 13 -3 0 6.38564 4.45428 5 13 -3 0 1.25088 3.62594 1 12 -3 0 9.40956 4.96738 1 12 -3 0 8.06312 4.16971 5 11 -3 0 0.55438 3.20247 5 11 -3 0 8.71165 4.53521 1 -11 3 0 -0.5413 2.8073 2 10 -3 0 82.9491 9.2688 1 10 -3 0 77.8371 9.3650 5 -10 3 0 86.6413 8.3952 2 9 -3 0 90.5805 9.3535 1 9 -3 0 79.6708 9.2382 5 -9 3 0 79.5848 8.5214 2 8 -3 0 507.823 43.592 1 8 -3 0 493.570 41.519 5 -8 3 0 459.636 40.581 2 7 -3 0 4.91168 2.89607 1 -7 3 0 2.45252 3.55321 2 -7 3 0 4.10159 2.23114 1 6 -3 0 159.315 15.285 1 -6 3 0 171.611 14.596 2 5 -3 0 232.685 21.389 1 -5 3 0 242.158 20.375 2 4 -3 0 2112.33 201.19 1 -4 3 0 2303.08 178.10 2 -4 3 0 2118.29 192.02 1 3 -3 0 253.088 21.029 1 -3 3 0 245.438 20.896 1 -3 3 0 204.503 19.955 2 2 -3 0 1353.50 127.78 1 2 -3 0 1453.32 114.49 6 -2 3 0 1430.38 115.42 2 -2 3 0 1400.16 123.10 1 1 -3 0 632.470 51.158 6 1 -3 0 644.287 54.933 1 1 -3 0 592.183 55.139 1 1 -3 0 649.214 52.456 4 -1 3 0 610.119 51.664 2 0 -3 0 -0.5013 1.2561 4 0 -3 0 0.96741 1.06171 1 0 -3 0 0.81578 1.32659 1 0 -3 0 -1.6731 2.1832 6 0 3 0 3.58765 2.99990 2 -1 -3 0 621.767 52.492 6 -1 -3 0 628.275 56.157 1 -1 -3 0 641.708 53.586 4 -1 -3 0 671.095 56.232 1 -1 -3 0 646.707 52.318 3 1 3 0 637.079 52.912 2 -2 -3 0 1456.62 130.00 1 -2 -3 0 1475.65 123.88 4 -2 -3 0 1432.78 120.98 6 -2 -3 0 1437.11 120.36 3 2 3 0 1624.37 123.97 4 2 3 0 1489.16 129.91 1 2 3 0 1503.35 121.63 2 -3 -3 0 245.513 21.437 1 -3 -3 0 243.529 19.919 3 -3 -3 0 226.722 20.184 6 -3 -3 0 225.590 20.207 4 3 3 0 234.350 21.415 1 3 3 0 228.711 20.231 4 3 3 0 264.790 20.379 2 -4 -3 0 2040.22 176.24 4 -4 -3 0 2154.24 171.08 3 -4 -3 0 2133.94 187.52 1 -4 -3 0 2139.67 172.05 6 4 3 0 1988.76 177.98 4 4 3 0 2085.16 184.91 1 4 3 0 2288.66 172.82 2 -5 -3 0 231.954 19.259 6 -5 -3 0 215.670 20.508 1 -5 -3 0 232.635 19.377 4 5 3 0 250.474 19.255 2 5 3 0 201.526 18.758 3 5 3 0 224.123 20.565 1 5 3 0 222.223 19.437 4 -6 -3 0 158.163 14.143 6 6 3 0 146.543 14.067 4 6 3 0 174.617 15.167 1 6 3 0 156.863 13.525 3 -7 -3 0 1.93731 3.44749 6 -7 -3 0 3.70448 1.56512 5 7 3 0 0.1577 10.0475 1 7 3 0 0.65022 2.44836 4 7 3 0 4.40240 2.01749 3 7 3 0 1.28091 2.05516 2 -8 -3 0 314.043 34.506 5 8 3 0 353.118 30.937 2 8 3 0 339.808 31.017 3 -9 -3 0 45.8806 5.0540 5 9 3 0 52.5266 5.1414 3 9 3 0 51.4802 4.8919 2 10 3 0 49.7456 4.9969 2 10 3 0 61.0289 6.8039 1 -11 -3 0 6.23861 4.13100 6 11 3 0 3.45418 4.33024 1 -12 -3 0 8.00040 3.89803 6 12 3 0 16.2402 4.7971 1 -13 -3 0 9.10362 3.77061 6 13 3 0 10.8873 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17 8.32632 6.58015 1 8 1 -17 1.42182 4.14535 4 -8 -1 17 -3.5824 6.4310 1 7 1 -17 -2.5386 4.1508 4 -7 -1 17 -4.2063 4.5758 1 6 1 -17 2.95323 4.54764 4 -6 -1 17 7.72190 6.47677 1 5 1 -17 7.54813 4.97429 4 -5 -1 17 12.0337 6.4847 1 4 1 -17 -11.343 5.154 4 -4 -1 17 -0.3342 5.9917 1 3 1 -17 35.8560 5.5713 4 2 1 -17 -6.9068 4.7526 4 -2 -1 17 12.9926 6.1143 1 1 1 -17 50.6212 7.4723 4 -1 -1 17 58.0660 8.8302 1 0 1 -17 25.8154 6.0740 4 -1 1 -17 11.8132 5.4788 4 1 -1 17 13.5160 6.3242 1 -2 1 -17 -0.7095 5.0078 4 2 -1 17 6.61779 5.87636 1 -3 1 -17 10.7060 5.5974 4 3 -1 17 9.22459 6.63074 1 -11 0 17 4.85013 6.39849 1 10 0 -17 -0.0390 3.6167 4 -10 0 17 -8.8834 5.8864 1 9 0 -17 5.60141 4.95079 4 -9 0 17 8.95124 6.34192 1 8 0 -17 -7.6946 5.1141 4 -8 0 17 -9.8811 6.4459 1 7 0 -17 2.30478 4.46765 4 -7 0 17 3.80194 4.44554 1 6 0 -17 -4.5410 4.5475 4 -6 0 17 -3.2845 4.2454 1 5 0 -17 26.3878 5.7071 4 -5 0 17 23.3070 5.4036 1 4 0 -17 -13.105 5.238 4 -4 0 17 -7.0901 4.4663 1 3 0 -17 19.3523 5.9094 4 -3 0 17 17.1133 5.1233 1 2 0 -17 -0.3969 5.0650 4 -2 0 17 -3.7232 5.2273 1 1 0 -17 16.4828 5.5792 4 0 0 -17 5.55396 4.59504 4 0 0 17 -2.9327 5.8330 1 1 0 17 28.6067 7.3502 1 -2 0 -17 -4.1210 3.9797 4 2 0 17 0.29891 6.09113 1 -3 0 -17 -3.9516 3.7914 4 3 0 17 -5.9783 5.9874 1 10 -1 -17 13.7334 6.0278 4 9 -1 -17 -2.2360 5.0631 4 -9 1 17 4.95107 5.90967 1 8 -1 -17 13.9955 5.8165 4 -8 1 17 10.5066 5.4314 1 7 -1 -17 -1.4177 4.6719 4 -7 1 17 -5.4252 4.6067 1 6 -1 -17 3.43452 3.74685 4 -6 1 17 6.06690 4.70114 1 5 -1 -17 12.5307 5.2710 4 -5 1 17 12.2141 5.4782 1 4 -1 -17 4.80184 4.97142 4 -4 1 17 0.15202 5.40694 1 3 -1 -17 54.1179 8.0417 4 -3 1 17 67.8487 8.9166 1 2 -1 -17 1.87391 4.09200 4 -2 1 17 4.21455 5.17039 1 1 -1 -17 39.6671 6.4517 4 -1 1 17 54.0918 8.0979 1 0 -1 -17 14.9165 4.6473 4 0 1 17 24.7630 6.5939 1 -1 -1 -17 4.11498 4.04553 4 1 1 17 22.3852 6.0310 1 -2 -1 -17 0.04886 4.08884 4 2 1 17 -0.2259 5.4741 1 -3 -1 -17 2.59301 3.94889 4 3 1 17 5.63654 6.16900 1 9 -2 -17 -3.8447 5.7493 4 8 -2 -17 2.65271 4.84179 4 7 -2 -17 3.36567 5.12601 4 6 -2 -17 1.12922 5.02086 4 -6 2 17 4.92829 4.71884 1 5 -2 -17 6.53024 5.34874 4 -5 2 17 16.3725 5.0570 1 4 -2 -17 0.97466 3.48734 4 -4 2 17 -2.9664 4.2609 1 3 -2 -17 6.31698 3.64432 4 -3 2 17 9.07235 3.77342 1 2 -2 -17 2.99885 3.66527 4 -2 2 17 -5.0004 4.8193 1 1 -2 -17 13.9458 4.2462 4 -1 2 17 13.4731 5.7937 1 0 -2 -17 5.46266 3.90755 4 0 2 17 -2.7967 5.1392 1 -1 -2 -17 -2.2461 3.6640 4 1 2 17 13.8667 5.6137 1 -2 -2 -17 5.42484 4.08758 4 2 2 17 14.8732 5.1000 1 7 -3 -17 4.13088 4.66418 4 6 -3 -17 2.02111 5.68012 4 5 -3 -17 5.57661 4.93571 4 4 -3 -17 0.82248 3.47853 4 3 -3 -17 9.90176 5.24666 4 2 -3 -17 6.39123 4.91194 4 1 -3 -17 1.56814 4.65877 4 0 -3 -17 1.72365 4.85315 4 -7 -2 18 1.71782 4.82481 1 -6 -2 18 -12.271 6.547 1 -5 -2 18 6.00120 6.13351 1 -4 -2 18 1.79516 4.12226 1 -3 -2 18 -3.1946 5.4992 1 -2 -2 18 15.1667 6.2337 1 -1 -2 18 9.80860 5.95030 1 9 1 -18 -4.0373 4.3289 4 -9 -1 18 -10.852 6.761 1 8 1 -18 2.11408 3.32973 4 -8 -1 18 5.45237 5.60112 1 7 1 -18 -7.1097 4.3265 4 -7 -1 18 7.98735 6.73728 1 6 1 -18 1.08130 4.13108 4 -6 -1 18 -2.9182 6.2443 1 5 1 -18 17.1696 4.6016 4 -5 -1 18 20.3667 5.6128 1 4 1 -18 3.60012 3.79231 4 -4 -1 18 0.26910 5.66638 1 3 1 -18 12.4789 4.8011 4 -3 -1 18 15.0976 6.5869 1 2 1 -18 7.09785 5.09239 4 -2 -1 18 -4.1224 5.9950 1 1 1 -18 -1.5468 5.0208 4 -1 -1 18 3.49646 5.89400 1 0 1 -18 25.4628 6.1036 4 0 -1 18 31.0057 7.3138 1 -1 1 -18 -2.9811 5.2652 4 1 -1 18 -1.5547 6.1140 1 9 0 -18 6.29246 5.28856 4 -9 0 18 -14.602 7.069 1 8 0 -18 3.09212 4.44217 4 -8 0 18 4.35648 4.68970 1 7 0 -18 0.42178 4.83504 4 -7 0 18 -3.2569 6.4865 1 6 0 -18 0.68634 4.88620 4 -6 0 18 14.5293 6.6668 1 5 0 -18 -5.3328 5.3526 4 -5 0 18 -11.104 6.479 1 4 0 -18 -0.7134 5.3177 4 -4 0 18 24.8336 6.8804 1 3 0 -18 -6.4760 5.5136 4 -3 0 18 -2.9246 5.9086 1 2 0 -18 22.9740 6.4808 4 -2 0 18 26.9337 6.9170 1 1 0 -18 4.22288 5.37108 4 -1 0 18 -4.8180 5.9487 1 0 0 -18 1.67598 5.17037 4 0 0 18 -8.6467 6.2918 1 -1 0 -18 6.29818 5.54957 4 1 0 18 -0.6766 5.0904 1 9 -1 -18 -1.7155 5.4772 4 -9 1 18 1.77531 5.38099 1 8 -1 -18 2.81705 3.88232 4 -8 1 18 -6.9059 5.0182 1 7 -1 -18 4.78645 5.33953 4 -7 1 18 7.94099 5.65374 1 6 -1 -18 5.92784 5.42542 4 -6 1 18 4.51104 5.85232 1 5 -1 -18 29.0199 6.6936 4 -5 1 18 33.5558 7.3841 1 4 -1 -18 2.20792 4.91847 4 -4 1 18 9.40349 5.82780 1 3 -1 -18 15.5449 4.7317 4 -3 1 18 12.4465 6.0248 1 2 -1 -18 -1.0718 3.7461 4 -2 1 18 -5.2451 5.9104 1 1 -1 -18 1.57550 3.68273 4 -1 1 18 5.30201 6.23873 1 0 -1 -18 23.2948 5.1468 4 0 1 18 26.1353 7.4610 1 -1 -1 -18 -10.222 4.125 4 7 -2 -18 2.96367 5.68643 4 6 -2 -18 -0.2033 4.6472 4 5 -2 -18 2.41464 5.08745 4 4 -2 -18 2.47779 5.10398 4 3 -2 -18 10.8125 5.3562 4 -3 2 18 6.11889 4.21252 1 2 -2 -18 20.5320 4.9039 4 -2 2 18 12.7492 5.0302 1 1 -2 -18 7.22110 4.03151 4 -1 2 18 1.47041 3.93953 1 4 1 -19 11.1708 5.4012 4 -4 -1 19 1.87947 5.26278 1 6 0 -19 1.19554 5.34006 4 -6 0 19 -0.7344 5.0353 1 5 0 -19 35.8686 6.6289 4 -5 0 19 34.8068 8.1002 1 4 0 -19 -7.6284 4.1941 4 -4 0 19 7.80208 6.39137 1 3 0 -19 7.31508 4.66353 4 -3 0 19 -8.2748 6.4374 1 2 0 -19 -2.2137 5.1099 4 -2 0 19 -6.9924 6.3735 1 4 -1 -19 4.15483 5.61050 4 -4 1 19 12.6172 5.6358 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 27838 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 N1 N 0.19213(12) 0.2199(2) 0.90936(11) 0.0493(4) Uani 1 1 d . U C1 C 0.28353(15) 0.0938(3) 1.08068(13) 0.0516(5) Uani 1 1 d . U C2 C 0.22754(14) 0.2709(3) 1.01516(13) 0.0493(5) Uani 1 1 d . U H2 H 0.2734 0.4034 1.0242 0.059 Uiso 1 1 calc R U C3 C 0.39633(16) 0.0873(4) 1.11216(15) 0.0647(6) Uani 1 1 d . U C4 C 0.22354(18) -0.0643(3) 1.11497(14) 0.0636(6) Uani 1 1 d . U H4 H 0.1489 -0.0607 1.0941 0.076 Uiso 1 1 calc R U C5 C 0.11170(16) 0.3435(4) 1.01164(16) 0.0625(6) Uani 1 1 d . U H5A H 0.0686 0.2299 1.0316 0.075 Uiso 1 1 calc R U H5B H 0.1066 0.4841 1.0424 0.075 Uiso 1 1 calc R U C6 C 0.09398(17) 0.3610(3) 0.90612(16) 0.0627(6) Uani 1 1 d . U H6A H 0.0274 0.2931 0.8716 0.075 Uiso 1 1 calc R U H6B H 0.1003 0.5114 0.8845 0.075 Uiso 1 1 calc R U C7 C 0.2647(2) 0.3085(4) 0.85355(18) 0.0776(7) Uani 1 1 d . U H7A H 0.3299 0.2228 0.8663 0.116 Uiso 1 1 calc R U H7B H 0.2815 0.4609 0.8701 0.116 Uiso 1 1 calc R U H7C H 0.2296 0.2988 0.7882 0.116 Uiso 1 1 calc R U C8 C 0.4412(2) -0.0817(5) 1.17636(18) 0.0832(8) Uani 1 1 d . U H8 H 0.5156 -0.0904 1.1977 0.100 Uiso 1 1 calc R U C9 C 0.2699(2) -0.2254(4) 1.17833(17) 0.0789(7) Uani 1 1 d . U H9 H 0.2275 -0.3274 1.2003 0.095 Uiso 1 1 calc R U B1 B 0.1605(2) -0.0327(4) 0.88115(18) 0.0608(6) Uani 1 1 d . U H3B H 0.237(2) -0.130(4) 0.8987(18) 0.091 Uiso 1 1 d . U H2B H 0.103(2) -0.091(4) 0.9195(19) 0.091 Uiso 1 1 d . U H1B H 0.124(2) -0.029(4) 0.8055(19) 0.091 Uiso 1 1 d . U C11 C 0.3790(3) -0.2329(5) 1.20827(18) 0.0882(8) Uani 1 1 d . U H11 H 0.4116 -0.3415 1.2507 0.106 Uiso 1 1 calc R U C12 C 0.46841(19) 0.2508(5) 1.0811(2) 0.0922(9) Uani 1 1 d . U H12A H 0.4424 0.3988 1.0861 0.138 Uiso 1 1 calc R U H12B H 0.4689 0.2214 1.0173 0.138 Uiso 1 1 calc R U H12C H 0.5402 0.2370 1.1200 0.138 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 N1 0.0584(9) 0.0362(7) 0.0559(9) 0.0009(6) 0.0188(7) -0.0011(6) C1 0.0545(11) 0.0473(10) 0.0505(10) -0.0107(7) 0.0086(8) 0.0025(8) C2 0.0503(10) 0.0382(8) 0.0586(11) -0.0093(7) 0.0121(8) -0.0018(7) C3 0.0563(12) 0.0712(13) 0.0631(13) -0.0203(10) 0.0082(9) 0.0074(9) C4 0.0692(13) 0.0596(11) 0.0567(12) -0.0007(9) 0.0056(9) -0.0013(9) C5 0.0590(12) 0.0576(11) 0.0722(13) -0.0070(10) 0.0183(10) 0.0128(9) C6 0.0624(12) 0.0490(10) 0.0735(14) 0.0035(9) 0.0108(10) 0.0117(8) C7 0.0954(17) 0.0663(13) 0.0835(16) 0.0029(12) 0.0459(14) -0.0117(12) C8 0.0682(14) 0.1078(19) 0.0649(14) -0.0168(13) -0.0002(11) 0.0349(14) C9 0.1070(19) 0.0672(13) 0.0567(13) 0.0043(10) 0.0094(13) 0.0038(12) B1 0.0792(16) 0.0440(11) 0.0592(14) -0.0121(10) 0.0171(12) -0.0075(10) C11 0.111(2) 0.0875(18) 0.0590(15) 0.0040(12) 0.0081(14) 0.0324(15) C12 0.0537(13) 0.108(2) 0.114(2) -0.0222(16) 0.0205(13) -0.0073(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C7 N1 C6 114.34(16) C7 N1 C2 114.93(16) C6 N1 C2 87.42(13) C7 N1 B1 110.44(16) C6 N1 B1 111.72(16) C2 N1 B1 116.32(15) C4 C1 C3 118.40(19) C4 C1 C2 120.02(17) C3 C1 C2 121.52(18) C1 C2 C5 121.96(17) C1 C2 N1 119.06(13) C5 C2 N1 88.98(13) C1 C3 C8 117.2(2) C1 C3 C12 122.9(2) C8 C3 C12 119.9(2) C9 C4 C1 122.9(2) C6 C5 C2 87.30(15) N1 C6 C5 90.92(14) C11 C8 C3 122.4(2) C11 C9 C4 118.8(3) C9 C11 C8 120.4(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C7 1.486(3) N1 C6 1.509(2) N1 C2 1.546(2) N1 B1 1.601(3) C1 C4 1.395(3) C1 C3 1.406(3) C1 C2 1.498(2) C2 C5 1.537(3) C3 C8 1.412(4) C3 C12 1.497(4) C4 C9 1.376(3) C5 C6 1.522(3) C8 C11 1.367(4) C9 C11 1.359(4)