#------------------------------------------------------------------------------ #$Date: 2015-07-09 01:06:54 +0300 (Thu, 09 Jul 2015) $ #$Revision: 141402 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/52/03/1520315.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_1520315 loop_ _publ_author_name 'Ro\&sbach, Jan' 'Harms, Klaus' 'Koert, Ulrich' _publ_section_title ; \a-Crotyl-\a-difluoroboranyloxy-amides: Structure and Reactivity of Isolable Intermediates in Stereospecific \a-Ketol Rearrangements. ; _journal_issue 12 _journal_name_full 'Organic letters' _journal_page_first 3122 _journal_page_last 3125 _journal_paper_doi 10.1021/acs.orglett.5b01427 _journal_volume 17 _journal_year 2015 _chemical_formula_moiety 'C12 H20 B F2 N O4' _chemical_formula_sum 'C12 H20 B F2 N O4' _chemical_formula_weight 291.10 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 16.8311(7) _cell_length_b 9.1985(3) _cell_length_c 18.0999(8) _cell_measurement_reflns_used 6834 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.1550 _cell_measurement_theta_min 2.2504 _cell_volume 2802.24(19) _computing_cell_refinement 'BRUKER SAINT' _computing_data_collection 'BRUKER APEX2 2014.9-0' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'XT V2014/1 (Bruker AXS Inc., 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker D8 QUEST area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_unetI/netI 0.0499 _diffrn_reflns_laue_measured_fraction_full 1.000 _diffrn_reflns_laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 7273 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.332 _diffrn_reflns_theta_min 2.250 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/5 (Bruker AXS Inc.)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1232 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.262 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.041 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 305 _refine_ls_number_reflns 2540 _refine_ls_number_restraints 396 _refine_ls_restrained_S_all 0.963 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0374 _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^)+(0.0260P)^2^+1.4594P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.0885 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2109 _reflns_number_total 2540 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol5b01427_si_002.cif _cod_data_source_block jr2137_0m _cod_depositor_comments 'Adding full bibliography for 1520305--1520319.cif.' _cod_database_code 1520315 _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_estimated_absorpt_t_min 0.967 _shelx_estimated_absorpt_t_max 0.995 _shelx_res_file ; jr2137_0m.res created by SHELXL-2014/7 TITL jr2137_0m_a.res in Pbca REM Old TITL jr2137_0m in Pbca REM SHELXT solution in Pbca REM R1 0.129, Rweak 0.004, Alpha 0.021, Orientation as input REM Formula found by SHELXT: C12 B N O4 F2 CELL 0.71073 16.8311 9.1985 18.0999 90.000 90.000 90.000 ZERR 8.000 0.0007 0.0003 0.0008 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H B N O F UNIT 96 160 8 8 32 16 TEMP -173.150 SIZE 0.04 0.11 0.29 L.S. 10 BOND $H LIST 4 acta conf FMAP 2 PLAN 20 WGHT 0.026000 1.459400 FVAR 0.30183 0.94160 PART 1 B1 3 0.388479 0.324116 0.385684 21.00000 0.02433 0.01712 = 0.02507 -0.00024 0.00320 -0.00061 F1 6 0.449694 0.259030 0.423876 21.00000 0.02621 0.02260 = 0.03452 0.00423 0.00017 0.00261 F2 6 0.329428 0.222986 0.371715 21.00000 0.02675 0.02027 = 0.03048 -0.00122 0.00416 -0.00532 O2 5 0.341685 0.738227 0.253853 21.00000 0.03779 0.02620 = 0.02679 0.00272 -0.00399 0.00557 O3 5 0.412616 0.404042 0.321410 21.00000 0.02882 0.01541 = 0.02514 -0.00083 0.00546 -0.00051 O8 5 0.352834 0.443414 0.435317 21.00000 0.02537 0.01738 = 0.02175 0.00197 0.00419 -0.00227 C1 1 0.285205 0.504175 0.239285 21.00000 0.03912 0.04038 = 0.04045 0.00734 -0.01357 -0.01069 AFIX 137 H1A 2 0.265920 0.439969 0.278595 21.00000 -1.50000 H1B 2 0.312026 0.446165 0.201333 21.00000 -1.50000 H1C 2 0.240202 0.555847 0.217133 21.00000 -1.50000 AFIX 0 C2 1 0.342144 0.611384 0.270888 21.00000 0.02395 0.02703 = 0.02034 0.00271 0.00380 0.00158 C3 1 0.403124 0.555400 0.328899 21.00000 0.02263 0.01695 = 0.02099 -0.00089 0.00197 -0.00068 C4 1 0.483978 0.632668 0.320392 21.00000 0.02239 0.01740 = 0.02546 0.00266 0.00239 -0.00093 AFIX 13 H4 2 0.473876 0.739572 0.316856 21.00000 -1.20000 AFIX 0 C5 1 0.538084 0.606066 0.386711 21.00000 0.02250 0.03034 = 0.03481 0.00675 -0.00026 -0.00270 AFIX 23 H5A 2 0.507129 0.620108 0.432670 21.00000 -1.20000 H5B 2 0.556662 0.503969 0.385693 21.00000 -1.20000 AFIX 0 C6 1 0.609692 0.706324 0.387985 21.00000 0.02838 0.04930 = 0.04011 0.00472 -0.00360 -0.00941 AFIX 137 H6A 2 0.639747 0.695163 0.341960 21.00000 -1.50000 H6B 2 0.643746 0.681269 0.430016 21.00000 -1.50000 H6C 2 0.591818 0.807275 0.392801 21.00000 -1.50000 AFIX 0 C7 1 0.522435 0.583267 0.248085 21.00000 0.03168 0.03086 = 0.03529 0.00116 0.01061 -0.00342 AFIX 137 H7A 2 0.572265 0.636346 0.240549 21.00000 -1.50000 H7B 2 0.486256 0.603042 0.206869 21.00000 -1.50000 H7C 2 0.533430 0.478752 0.250496 21.00000 -1.50000 AFIX 0 PART 0 PART 2 same b1 > c7 simu .009 b1a > c7a b1 > c7 B1A 3 0.423449 0.342490 0.416168 -21.00000 0.02870 0.02065 = 0.02742 0.00160 0.00300 0.00129 F1A 6 0.475259 0.280750 0.465454 -21.00000 0.05022 0.06039 = 0.02925 0.00657 -0.00766 0.02145 F2A 6 0.370082 0.236702 0.392273 -21.00000 0.03962 0.02661 = 0.04324 -0.00119 0.01406 -0.00330 O2A 5 0.512448 0.791194 0.352610 -21.00000 0.02057 0.03786 = 0.03656 0.00365 0.00120 -0.00364 O3A 5 0.457057 0.418567 0.354295 -21.00000 0.02472 0.01806 = 0.02687 0.00446 0.00208 0.00160 O8A 5 0.375277 0.460905 0.456108 -21.00000 0.02450 0.02019 = 0.02699 -0.00008 0.00039 -0.00091 C1A 1 0.587686 0.581080 0.375817 -21.00000 0.02419 0.04250 = 0.04656 0.00078 -0.00712 -0.00666 AFIX 137 H1D 2 0.632786 0.647431 0.369843 -21.00000 -1.50000 H1E 2 0.593277 0.499360 0.341470 -21.00000 -1.50000 H1F 2 0.586530 0.544407 0.426640 -21.00000 -1.50000 AFIX 0 C2A 1 0.512360 0.660221 0.359845 -21.00000 0.02064 0.02722 = 0.02867 0.00579 0.00088 -0.00076 C3A 1 0.435708 0.570092 0.353535 -21.00000 0.02442 0.01921 = 0.02774 0.00176 0.00010 -0.00037 C4A 1 0.389802 0.600393 0.282964 -21.00000 0.02266 0.01822 = 0.02161 0.00148 -0.00011 -0.00015 AFIX 13 H4A 2 0.377408 0.706708 0.283577 -21.00000 -1.20000 AFIX 0 C5A 1 0.311714 0.524150 0.275985 -21.00000 0.02523 0.02395 = 0.02407 -0.00123 0.00270 -0.00218 AFIX 23 H5C 2 0.278049 0.555236 0.317963 -21.00000 -1.20000 H5D 2 0.321567 0.418724 0.282080 -21.00000 -1.20000 AFIX 0 C6A 1 0.263828 0.544377 0.205892 -21.00000 0.01772 0.03485 = 0.03583 0.01621 -0.00984 -0.01495 AFIX 137 H6D 2 0.217473 0.479940 0.206929 -21.00000 -1.50000 H6E 2 0.296942 0.520666 0.163018 -21.00000 -1.50000 H6F 2 0.246085 0.645612 0.202374 -21.00000 -1.50000 AFIX 0 C7A 1 0.446281 0.576746 0.217453 -21.00000 0.03596 0.02958 = 0.01714 -0.00154 -0.00054 -0.00515 AFIX 137 H7D 2 0.415570 0.573645 0.171480 -21.00000 -1.50000 H7E 2 0.474730 0.484654 0.223880 -21.00000 -1.50000 H7F 2 0.484595 0.656844 0.215181 -21.00000 -1.50000 REM ##### AFIX 0 part 0 C8 1 0.364568 0.569516 0.406279 11.00000 0.02076 0.02030 = 0.02652 0.00317 0.00041 -0.00073 N9 4 0.340828 0.686388 0.440540 11.00000 0.02212 0.01954 = 0.02451 0.00021 0.00224 0.00050 C10 1 0.351600 0.838605 0.416640 11.00000 0.02635 0.01910 = 0.03046 0.00199 0.00244 0.00387 AFIX 23 H10A 2 0.299351 0.882808 0.405398 11.00000 -1.20000 H10B 2 0.384517 0.841925 0.371342 11.00000 -1.20000 AFIX 0 C11 1 0.391929 0.922317 0.477893 11.00000 0.03539 0.02004 = 0.03904 0.00268 -0.00434 -0.00153 AFIX 23 H11A 2 0.445572 0.881527 0.486474 11.00000 -1.20000 H11B 2 0.398147 1.025129 0.462787 11.00000 -1.20000 AFIX 0 O12 5 0.347145 0.915554 0.544837 11.00000 0.04883 0.02268 = 0.03076 -0.00303 -0.00431 0.00299 C13 1 0.341080 0.768683 0.568716 11.00000 0.03638 0.02611 = 0.02633 0.00017 -0.00213 0.00247 AFIX 23 H13A 2 0.311681 0.764908 0.616052 11.00000 -1.20000 H13B 2 0.394971 0.728995 0.577294 11.00000 -1.20000 AFIX 0 C14 1 0.298680 0.676443 0.512001 11.00000 0.02629 0.02658 = 0.02491 -0.00159 0.00588 0.00033 AFIX 23 H14A 2 0.297217 0.574008 0.528727 11.00000 -1.20000 H14B 2 0.243290 0.710775 0.506140 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 REM jr2137_0m_a.res in Pbca REM R1 = 0.0374 for 2109 Fo > 4sig(Fo) and 0.0490 for all 2540 data REM 305 parameters refined using 396 restraints END WGHT 0.0260 1.4594 REM Highest difference peak 0.262, deepest hole -0.163, 1-sigma level 0.041 Q1 1 0.3824 0.5719 0.3648 11.00000 0.05 0.26 Q2 1 0.3282 0.4440 0.2188 11.00000 0.05 0.22 Q3 1 0.2967 0.3931 0.2525 11.00000 0.05 0.20 Q4 1 0.4397 0.6074 0.3246 11.00000 0.05 0.19 Q5 1 0.3229 0.7235 0.5377 11.00000 0.05 0.18 Q6 1 0.3317 0.6413 0.4082 11.00000 0.05 0.18 Q7 1 0.3674 0.5731 0.2999 11.00000 0.05 0.18 Q8 1 0.3442 0.7557 0.4262 11.00000 0.05 0.18 Q9 1 0.3844 0.6306 0.4403 11.00000 0.05 0.17 Q10 1 0.3610 0.8944 0.4465 11.00000 0.05 0.17 Q11 1 0.5029 0.6052 0.2869 11.00000 0.05 0.15 Q12 1 0.3076 0.6778 0.4600 11.00000 0.05 0.15 Q13 1 0.2985 0.8540 0.4238 11.00000 0.05 0.15 Q14 1 0.4989 0.6047 0.3565 11.00000 0.05 0.14 Q15 1 0.3621 0.3737 0.4101 11.00000 0.05 0.14 Q16 1 0.3397 0.2315 0.3171 11.00000 0.05 0.14 Q17 1 0.4791 0.1967 0.3871 11.00000 0.05 0.14 Q18 1 0.4936 0.5538 0.1962 11.00000 0.05 0.13 Q19 1 0.4192 0.3911 0.3588 11.00000 0.05 0.13 Q20 1 0.6239 0.7482 0.4418 11.00000 0.05 0.13 ; _shelx_res_checksum 69619 _shelx_hkl_file ; 2 0 0 7.13166 0.94422 1 3 0 0 0.34564 0.88335 1 -3 0 0 0.17492 0.93190 1 -4 0 0 9999.99 401.483 1 4 0 0 7521.43 399.279 1 -5 0 0 1.25356 1.18046 1 5 0 0 0.48893 1.16702 1 6 0 0 3535.40 184.668 1 -6 0 0 4566.01 184.797 1 7 0 0 0.97110 1.49181 1 -7 0 0 0.17902 1.31261 1 8 0 0 16.6494 3.08792 1 -8 0 0 18.1824 3.14434 1 -9 0 0 0.60339 1.48458 1 9 0 0 1.24660 1.65787 1 -10 0 0 654.339 29.8301 2 -11 0 0 25.0181 3.78459 1 11 0 0 26.5081 4.20617 1 -12 0 0 115.926 5.57386 2 -13 0 0 13.0437 1.19444 2 -14 0 0 11.9080 3.49894 1 -15 0 0 6.42772 0.93561 2 -16 0 0 552.776 25.3925 2 -17 0 0 5.00122 0.99580 2 -18 0 0 36.9067 2.50902 2 -19 0 0 4.60171 1.18037 2 -20 0 0 126.995 6.44552 2 1 -1 0 -0.2572 0.23328 2 -1 -1 0 0.26139 0.16345 2 2 -1 0 437.960 19.9845 2 -2 -1 0 439.902 19.9038 2 3 -1 0 -0.5558 0.41975 2 -3 -1 0 -1.0711 0.20166 2 -4 -1 0 4804.38 217.562 2 -5 -1 0 -0.3998 0.22554 2 -6 -1 0 452.040 20.5487 2 -7 -1 0 -0.1044 0.30150 2 -8 -1 0 363.650 16.5969 2 -9 -1 0 0.37777 0.37781 2 -10 -1 0 9.51139 0.85879 2 -11 -1 0 0.67724 0.48026 2 -12 -1 0 134.816 6.38101 2 -13 -1 0 1.35244 0.64243 2 -14 1 0 148.045 7.24629 2 -14 -1 0 151.528 7.12915 2 -15 1 0 0.53315 0.82833 2 -16 1 0 176.663 8.51635 2 -16 -1 0 176.800 8.40595 2 -17 1 0 0.93772 0.87201 2 -17 -1 0 1.16694 0.88486 2 -18 -1 0 42.2370 2.73162 2 -18 1 0 43.6559 2.81319 2 -19 1 0 0.58783 1.08580 2 -19 -1 0 -1.8762 1.04032 2 -20 1 0 22.0669 2.28107 2 -20 -1 0 22.1776 2.25111 2 0 -2 0 978.536 44.3963 2 1 -2 0 -1.0062 0.50159 2 -1 -2 0 -0.6920 0.35767 2 2 -2 0 66.1271 3.32884 2 -2 -2 0 69.4009 3.22803 2 3 -2 0 0.81504 0.51679 2 -3 -2 0 0.72629 0.31973 2 4 -2 0 162.383 7.71582 2 -4 -2 0 165.927 7.56256 2 -5 -2 0 1.67565 0.35224 2 5 -2 0 1.17486 0.55387 2 -6 -2 0 974.291 44.1580 2 -7 -2 0 1.22945 0.37176 2 -8 -2 0 420.045 19.1395 2 -9 -2 0 -0.1445 0.35496 2 -10 -2 0 262.861 12.0756 2 -11 -2 0 0.01202 0.48838 2 -12 -2 0 70.8441 3.51799 2 -13 -2 0 0.61046 0.64244 2 -14 -2 0 95.4186 4.69678 2 -15 -2 0 -0.0142 0.75832 2 -16 -2 0 4.14606 0.94785 2 -17 2 0 0.91035 1.05589 2 -17 -2 0 0.93327 0.85303 2 -18 -2 0 136.898 6.73848 2 -18 2 0 137.931 6.93966 2 -19 -2 0 0.32736 1.07307 2 -19 2 0 1.11494 1.10302 2 0 -3 0 -2.4596 0.45490 2 -1 -3 0 -0.2023 0.46181 2 1 -3 0 -0.3484 0.50093 2 -2 -3 0 418.863 19.2514 2 2 -3 0 422.819 19.3384 2 -3 -3 0 1.95703 0.53397 2 3 -3 0 0.65070 0.53576 2 4 -3 0 11.9911 1.16812 2 -4 -3 0 10.5728 0.94388 2 -5 -3 0 0.99560 0.49172 2 5 -3 0 1.04838 0.64336 2 -6 -3 0 51.8006 2.51638 2 6 -3 0 46.8007 2.78877 2 7 -3 0 0.36575 0.59338 2 -7 -3 0 0.58661 0.49426 2 -8 -3 0 8.91738 0.89187 2 -9 -3 0 0.45161 0.48270 2 -10 -3 0 10.7563 0.98633 2 -11 -3 0 0.06791 0.52263 2 -12 -3 0 8.89732 0.89624 2 13 3 0 0.49272 2.73085 1 -13 -3 0 0.32914 2.10847 1 -13 3 0 1.37951 2.82833 1 13 -3 0 0.16042 2.70127 1 -14 -3 0 93.8589 4.64610 2 -15 -3 0 1.00941 0.80190 2 -16 -3 0 105.274 5.39049 2 -17 -3 0 1.40321 0.98194 2 -18 -3 0 12.2325 1.45167 2 -19 -3 0 0.65510 1.12589 2 -19 3 0 -0.1264 1.17506 2 0 -4 0 16.5008 1.36622 2 1 -4 0 0.52240 0.67765 2 2 -4 0 445.922 20.7228 2 -2 -4 0 453.391 20.6546 2 -3 -4 0 -0.4283 0.54927 2 3 -4 0 0.32223 0.68818 2 -4 -4 0 9.40051 0.94998 2 -5 -4 0 0.26328 0.59075 2 5 -4 0 -0.7520 0.68947 2 6 -4 0 15.6936 1.45340 2 -6 -4 0 13.5937 1.25930 2 -7 -4 0 2.17553 0.65828 2 7 -4 0 1.84397 0.82068 2 -8 -4 0 230.796 10.8681 2 8 -4 0 238.364 11.1550 2 -9 -4 0 0.45835 0.67275 2 -10 -4 0 106.433 5.14717 2 -11 -4 0 0.55887 0.71082 2 -12 -4 0 1.07128 0.86937 2 -13 -4 0 -0.2044 1.00237 2 -14 -4 0 14.6613 1.44821 2 -15 -4 0 0.32264 1.00606 2 -16 -4 0 4.79989 1.27255 2 -17 -4 0 -0.4002 1.17677 2 -18 -4 0 91.0651 4.94219 2 0 -5 0 1.48204 0.73612 2 1 -5 0 -1.1165 0.86726 2 -1 -5 0 0.12642 0.69480 2 -2 -5 0 14.1768 1.31609 2 2 -5 0 17.5170 1.55010 2 3 -5 0 -0.0026 0.72466 2 -3 -5 0 -0.5998 0.69085 2 -4 -5 0 2.09468 0.76185 2 4 -5 0 1.72182 0.84282 2 5 -5 0 1.53021 0.80757 2 -5 -5 0 1.04484 0.69063 2 6 -5 0 347.373 16.1721 2 -6 -5 0 342.633 15.9395 2 7 -5 0 -0.1250 0.74092 2 -7 -5 0 0.52332 0.84851 2 8 -5 0 228.919 11.0685 2 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6.41538 1.44804 2 -2 -1 18 6.99963 1.43809 2 -3 1 18 22.8893 2.28447 2 3 -1 18 19.5384 2.25342 2 3 1 18 23.6814 2.45067 2 -3 -1 18 22.0277 2.23546 2 -4 1 18 -0.6873 1.07989 2 4 -1 18 2.11235 1.52221 2 4 1 18 0.01184 1.43664 2 -4 -1 18 -0.1729 1.02300 2 -5 1 18 1.37078 1.09928 2 5 -1 18 -0.7430 1.53735 2 5 1 18 3.10521 1.52636 2 -5 -1 18 -0.2306 0.96544 2 6 -1 18 47.3448 3.80652 2 -6 1 18 45.2457 3.15914 2 6 1 18 51.6882 3.63312 2 -6 -1 18 49.3809 3.18939 2 7 -1 18 13.9004 2.27747 2 -7 1 18 13.9701 1.64072 2 7 1 18 15.8573 2.17167 2 -7 -1 18 16.7720 1.96216 2 8 -1 18 10.3556 2.21785 2 -8 1 18 7.91460 1.38406 2 -8 -1 18 8.99048 1.59793 2 8 1 18 9.59256 2.11058 2 -9 1 18 7.20279 1.37739 2 9 -1 18 8.33058 2.14833 2 -9 -1 18 5.04853 1.32600 2 9 1 18 7.57851 2.08682 2 10 -1 18 14.0549 2.31135 2 -10 1 18 9.58331 1.39156 2 -10 -1 18 10.9980 1.65152 2 10 1 18 13.0004 2.31475 2 11 -1 18 -1.3866 2.14045 2 -11 1 18 0.68723 1.13736 2 11 1 18 0.58960 2.26836 2 -11 -1 18 0.17535 1.25307 2 0 2 18 13.5309 1.65941 2 0 -2 18 12.3581 1.99260 2 -1 2 18 -1.2367 1.06728 2 1 -2 18 -0.3299 1.43967 2 1 2 18 -1.7759 1.15761 2 -1 -2 18 -1.9581 1.24129 2 -2 2 18 -0.0371 1.07159 2 2 -2 18 2.59682 1.62364 2 2 2 18 -0.3826 1.29688 2 -2 -2 18 -0.7332 1.11300 2 3 -2 18 0.36580 1.47933 2 -3 2 18 0.15564 1.06288 2 -3 -2 18 2.60493 1.24550 2 3 2 18 1.12640 1.34173 2 -4 2 18 3.34165 1.15695 2 4 -2 18 -0.8083 1.51198 2 -4 -2 18 3.21387 1.24197 2 4 2 18 1.54233 1.40213 2 5 -2 18 5.91047 1.80369 2 -5 2 18 4.51421 1.23837 2 5 2 18 7.47625 1.71913 2 -5 -2 18 6.38498 1.34687 2 6 -2 18 7.57128 1.91067 2 -6 2 18 8.84264 1.41275 2 -6 -2 18 5.77953 1.35053 2 6 2 18 8.56435 1.86591 2 -7 2 18 12.2243 1.53967 2 7 -2 18 15.0070 2.34516 2 7 2 18 18.0774 2.29367 2 -7 -2 18 21.4826 2.17249 2 8 -2 18 23.0836 2.80202 2 -8 2 18 23.6316 2.14380 2 8 2 18 28.0633 2.56154 2 -8 -2 18 16.5884 2.02941 2 -9 2 18 0.22992 1.08215 2 9 -2 18 3.68187 2.01409 2 -9 -2 18 -1.9724 1.08913 2 -10 2 18 27.1315 2.39316 2 10 -2 18 30.4502 3.06053 2 10 2 18 30.6643 2.90107 2 -10 -2 18 28.6353 2.80473 2 0 -3 18 1.32621 1.33696 2 0 3 18 -1.0325 1.14260 2 -1 3 18 16.3033 1.75038 2 1 -3 18 12.8984 2.00380 2 1 3 18 16.1679 1.78608 2 -1 -3 18 19.5212 2.25842 2 -2 3 18 0.69994 1.11266 2 2 -3 18 0.06818 1.37346 2 2 3 18 -1.7875 1.20855 2 -2 -3 18 -0.3740 1.21238 2 3 -3 18 2.17632 1.61122 2 -3 3 18 4.06165 1.19381 2 -3 -3 18 2.28083 1.20219 2 3 3 18 3.58491 1.44643 2 -4 3 18 3.43976 1.24311 2 4 -3 18 4.57325 1.72554 2 -4 -3 18 2.63866 1.37190 2 4 3 18 3.72132 1.55046 2 -5 3 18 21.1206 2.09556 2 5 -3 18 19.4592 2.53016 2 5 3 18 17.4479 2.14253 2 -5 -3 18 19.6094 2.25605 2 -6 3 18 9.82423 1.45228 2 6 -3 18 8.81635 2.22804 2 6 3 18 10.3376 1.86225 2 -6 -3 18 6.91429 1.52056 2 -7 3 18 0.79566 1.05569 2 7 -3 18 -1.5265 1.77640 2 -7 -3 18 -0.2142 1.27306 2 7 3 18 3.20088 2.32672 2 -8 3 18 -1.4255 0.96200 2 8 -3 18 -0.7826 1.87367 2 -8 -3 18 0.90621 1.17709 2 8 3 18 -0.4101 1.98809 2 9 -3 18 20.3788 2.67614 2 -9 3 18 15.4858 1.77651 2 -9 -3 18 18.5810 2.19278 2 0 -4 18 38.0819 3.16614 2 0 4 18 34.0186 2.67150 2 -1 4 18 5.81996 1.35832 2 1 -4 18 4.36183 1.56591 2 1 4 18 5.31246 1.36887 2 -1 -4 18 4.56574 1.52042 2 2 -4 18 -0.2185 1.42418 2 -2 4 18 -0.0801 1.12729 2 2 4 18 -0.5493 1.34553 2 -2 -4 18 -1.5243 1.24805 2 3 -4 18 2.11038 1.68378 2 -3 4 18 3.12459 1.15775 2 -3 -4 18 1.46136 1.24754 2 3 4 18 -1.1513 1.39887 2 4 -4 18 1.78141 1.76286 2 -4 4 18 -1.5674 1.00119 2 4 4 18 0.05655 1.49129 2 -4 -4 18 -1.6300 1.19768 2 5 -4 18 0.99711 1.64261 2 -5 4 18 0.08438 1.15296 2 -5 -4 18 -0.1880 1.37253 2 5 4 18 -1.3488 1.65372 2 6 -4 18 5.33809 2.11406 2 -6 4 18 6.18834 1.35301 2 6 4 18 7.19195 1.86829 2 -6 -4 18 7.38385 1.88878 2 7 -4 18 3.71641 2.13370 2 -7 4 18 4.03718 1.17924 2 -7 -4 18 7.07803 1.82042 2 8 -4 18 13.9317 2.44759 2 -8 4 18 10.4623 1.55288 2 -8 -4 18 12.7888 2.14487 2 0 -5 18 1.50018 1.51980 2 0 5 18 -0.2478 1.29054 2 -1 5 18 26.2553 2.37342 2 1 -5 18 24.4403 2.59587 2 -1 -5 18 23.4923 2.52599 2 1 5 18 24.5854 2.11184 2 2 -5 18 -1.1532 1.36221 2 -2 5 18 0.05185 1.18393 2 2 5 18 2.05154 1.42786 2 -2 -5 18 1.90036 1.56052 2 3 -5 18 3.49712 1.84577 2 -3 5 18 1.13182 1.18546 2 3 5 18 1.50137 1.48492 2 -3 -5 18 -1.1863 1.28854 2 4 -5 18 23.7100 2.89297 2 -4 5 18 24.9060 2.30545 2 4 5 18 27.1095 2.31038 2 -4 -5 18 20.6011 2.56555 2 -5 5 18 4.38951 1.31466 2 5 -5 18 4.51241 2.11935 2 -5 -5 18 4.76911 1.94074 2 5 5 18 7.09492 1.87527 2 6 -5 18 6.85112 2.18551 2 -6 5 18 7.01887 1.41172 2 -6 -5 18 4.60596 1.71926 2 0 -6 18 14.8601 2.33577 2 0 6 18 22.2542 1.97774 2 -1 6 18 50.6033 3.25924 2 1 -6 18 45.8324 3.99808 2 1 6 18 49.7346 3.40632 2 -1 -6 18 50.7208 4.07946 2 -2 6 18 2.45231 1.29040 2 2 -6 18 3.38538 1.83490 2 2 6 18 4.00015 1.62530 2 -2 -6 18 3.83320 1.58833 2 0 0 19 4.12762 1.43570 2 1 0 19 0.67618 1.43754 2 -1 0 19 0.70817 1.36664 2 -2 0 19 0.47071 1.23028 2 2 0 19 0.08380 1.32649 2 3 0 19 0.42165 1.44413 2 -3 0 19 0.08600 1.18208 2 4 0 19 -2.2377 1.43296 2 -4 0 19 -1.1423 1.17032 2 5 0 19 -0.5066 1.61066 2 -5 0 19 -2.1037 1.16632 2 6 0 19 1.00224 1.87491 2 -6 0 19 -0.0732 1.04172 2 7 0 19 -1.0994 1.75311 2 -7 0 19 0.75929 1.01071 2 8 0 19 1.47473 2.08415 2 -8 0 19 -1.4230 1.06024 2 9 0 19 -0.7299 2.03436 2 -9 0 19 -0.0854 1.10337 2 0 -1 19 -0.5977 1.27430 2 0 1 19 2.45580 1.33891 2 -1 1 19 0.24863 1.18169 2 1 -1 19 -1.3372 1.39544 2 1 1 19 1.23048 1.33302 2 -1 -1 19 1.34764 1.39993 2 2 -1 19 12.6666 1.92868 2 -2 1 19 14.2660 1.83520 2 2 1 19 17.3363 2.00957 2 -2 -1 19 15.3982 2.06062 2 3 -1 19 5.84716 1.78194 2 -3 1 19 5.85168 1.46126 2 -3 -1 19 6.40090 1.49115 2 3 1 19 4.62349 1.56217 2 4 -1 19 6.19141 1.79761 2 -4 1 19 2.91737 1.26141 2 4 1 19 5.28401 1.67372 2 -4 -1 19 4.41902 1.35650 2 5 -1 19 0.78742 1.73945 2 -5 1 19 -0.9475 1.07613 2 5 1 19 -1.6079 1.57291 2 -5 -1 19 0.67013 1.06875 2 -6 1 19 3.52696 1.41795 2 6 -1 19 -0.3034 1.96999 2 6 1 19 2.44794 1.77829 2 -6 -1 19 5.22326 1.26305 2 -7 1 19 -0.0075 1.15917 2 7 -1 19 -0.5033 1.85774 2 -7 -1 19 -0.5858 1.07066 2 7 1 19 1.44135 1.89121 2 8 -1 19 0.28100 1.98390 2 -8 1 19 -1.4505 0.96789 2 8 1 19 -0.0253 2.05887 2 -8 -1 19 1.52780 1.27627 2 9 -1 19 5.29841 2.25875 2 -9 1 19 3.93750 1.30492 2 9 1 19 5.95086 2.25273 2 -9 -1 19 5.74245 1.50090 2 0 -2 19 7.76378 1.76551 2 0 2 19 10.9958 1.58486 2 1 -2 19 1.42510 1.51155 2 -1 2 19 -0.6132 1.13332 2 -1 -2 19 0.18725 1.34289 2 1 2 19 0.78006 1.27257 2 -2 2 19 0.06041 1.25171 2 2 -2 19 3.53942 1.63988 2 -2 -2 19 2.68527 1.59565 2 2 2 19 1.95123 1.38743 2 -3 2 19 1.81708 1.28308 2 3 -2 19 3.66994 1.73640 2 3 2 19 2.15717 1.48168 2 -3 -2 19 1.60131 1.36844 2 -4 2 19 7.49730 1.48307 2 4 -2 19 3.08764 1.79013 2 4 2 19 4.62699 1.67308 2 -4 -2 19 3.40592 1.42806 2 5 -2 19 2.35644 1.73861 2 -5 2 19 -0.7541 1.10975 2 -5 -2 19 0.67374 1.22652 2 5 2 19 0.22902 1.66296 2 -6 2 19 1.60344 1.38795 2 6 -2 19 -0.0297 1.82443 2 -6 -2 19 1.48441 1.05801 2 6 2 19 3.13208 1.80071 2 -7 2 19 21.5490 2.21486 2 7 -2 19 22.2948 2.75066 2 -7 -2 19 18.6884 2.17514 2 7 2 19 19.8848 2.49145 2 8 -2 19 4.08752 2.18983 2 -8 2 19 1.62782 1.20275 2 -8 -2 19 2.01022 1.20145 2 8 2 19 5.19065 2.24873 2 -9 2 19 9.33085 1.54825 2 9 -2 19 16.0366 2.51005 2 9 2 19 10.7417 2.42864 2 0 3 19 0.41357 1.32518 2 0 -3 19 -0.3841 1.48145 2 1 -3 19 0.55684 1.39391 2 -1 3 19 1.30551 1.27117 2 -1 -3 19 1.41569 1.47432 2 1 3 19 1.69514 1.37343 2 -2 3 19 2.95294 1.36481 2 2 -3 19 0.92430 1.59405 2 -2 -3 19 2.63477 1.30781 2 2 3 19 2.96360 1.50441 2 3 -3 19 22.1572 2.67898 2 -3 3 19 24.0642 2.38498 2 -3 -3 19 25.5881 2.59970 2 3 3 19 21.9129 2.29877 2 4 -3 19 -1.3850 1.65426 2 -4 3 19 -0.6812 1.18636 2 4 3 19 1.36720 1.57178 2 -4 -3 19 -0.8485 1.37142 2 -5 3 19 2.80098 1.26570 2 5 -3 19 4.05739 1.95332 2 -5 -3 19 3.49052 1.66584 2 5 3 19 3.72509 1.80967 2 -6 3 19 7.19570 1.39227 2 6 -3 19 5.61500 2.28257 2 -6 -3 19 7.88253 1.65018 2 6 3 19 8.34018 1.98916 2 -7 3 19 5.58519 1.44285 2 7 -3 19 6.12433 2.27552 2 7 3 19 6.77444 2.16979 2 -7 -3 19 5.41045 1.56575 2 -8 3 19 8.86783 1.58993 2 8 -3 19 11.8415 2.66175 2 -8 -3 19 11.7433 1.89088 2 0 4 19 53.5396 3.59741 2 0 -4 19 60.5059 4.05917 2 -1 4 19 0.35264 1.24730 2 1 -4 19 1.61737 1.52838 2 -1 -4 19 0.04647 1.48663 2 1 4 19 -0.5436 1.42362 2 -2 4 19 1.72652 1.30447 2 2 -4 19 0.98216 1.79690 2 -2 -4 19 -1.4700 1.39195 2 2 4 19 0.85010 1.47861 2 3 -4 19 5.67026 2.01563 2 -3 4 19 4.23489 1.32602 2 -3 -4 19 7.05878 1.77375 2 3 4 19 3.74624 1.74920 2 4 -4 19 37.5405 3.78960 2 -4 4 19 35.1626 2.78947 2 -4 -4 19 28.7985 3.10044 2 4 4 19 35.5303 3.17818 2 5 -4 19 5.62396 2.04556 2 -5 4 19 4.03333 1.42380 2 -5 -4 19 2.23279 1.57861 2 5 4 19 5.77244 1.96495 2 6 -4 19 59.7942 4.70626 2 -6 4 19 61.5148 3.78751 2 -6 -4 19 65.2810 4.37376 2 0 -5 19 0.97300 1.62338 2 0 5 19 -0.7479 1.30321 2 -1 5 19 23.5920 2.20694 2 1 -5 19 21.3804 2.74565 2 -1 -5 19 20.1626 2.58016 2 1 5 19 25.5206 2.64153 2 -2 5 19 -2.9349 1.26470 2 2 -5 19 -1.5277 1.61753 2 -2 -5 19 -0.6273 1.47396 2 2 5 19 0.90006 1.65693 2 3 -5 19 60.3147 4.83003 2 -3 5 19 61.5802 3.88010 2 -3 -5 19 63.2774 4.56331 2 3 5 19 67.2466 4.12947 2 0 0 20 99.5836 5.64446 2 1 0 20 7.94625 1.79780 2 -1 0 20 8.65962 1.76811 2 -2 0 20 11.1706 1.81679 2 2 0 20 11.3543 1.91551 2 3 0 20 1.66243 1.70560 2 -3 0 20 0.94398 1.43516 2 -4 0 20 12.2472 1.72388 2 4 0 20 11.5302 2.11203 2 -5 0 20 4.51937 1.45006 2 5 0 20 3.41568 1.85623 2 -6 0 20 4.94395 1.57586 2 6 0 20 12.2265 2.26310 2 -7 0 20 34.3097 2.91130 2 7 0 20 35.9156 3.76998 2 0 -1 20 1.02467 1.52021 2 0 1 20 -1.0545 1.37817 2 -1 1 20 0.86880 1.28244 2 1 -1 20 1.13698 1.45843 2 1 1 20 -1.9683 1.50947 2 -1 -1 20 -0.3368 1.44711 2 2 -1 20 15.3206 2.20622 2 -2 1 20 14.8813 1.90716 2 2 1 20 18.7638 2.23110 2 -2 -1 20 22.6259 2.38165 2 3 -1 20 21.0904 2.47057 2 -3 1 20 14.6336 1.96707 2 -3 -1 20 13.9952 2.02839 2 3 1 20 17.8653 2.12190 2 4 -1 20 1.05375 1.69148 2 -4 1 20 2.10195 1.34822 2 -4 -1 20 4.63635 1.59548 2 4 1 20 3.24890 1.84134 2 5 -1 20 7.20117 1.98304 2 -5 1 20 6.02252 1.50722 2 -5 -1 20 4.88930 1.59363 2 5 1 20 5.50111 1.88577 2 6 -1 20 -0.9313 2.01431 2 -6 1 20 0.86962 1.36510 2 -6 -1 20 -1.0951 1.05807 2 6 1 20 1.27261 1.92859 2 -7 1 20 4.75994 1.60116 2 7 -1 20 11.5829 2.45995 2 -7 -1 20 7.59820 1.46195 2 7 1 20 7.56591 2.24055 2 0 -2 20 6.69666 1.83132 2 0 2 20 7.21766 1.65520 2 1 -2 20 37.3502 3.50110 2 -1 2 20 45.8372 3.27620 2 -1 -2 20 41.5532 3.48931 2 1 2 20 43.3078 3.36912 2 2 -2 20 0.15227 1.68286 2 -2 2 20 0.81211 1.43311 2 -2 -2 20 0.80190 1.33353 2 2 2 20 1.65248 1.54091 2 -3 2 20 2.52638 1.47170 2 3 -2 20 1.07174 1.83939 2 3 2 20 0.51715 1.47082 2 -3 -2 20 -1.7279 1.25803 2 4 -2 20 6.48597 2.04787 2 -4 2 20 5.57162 1.53057 2 -4 -2 20 5.90660 1.53327 2 4 2 20 7.97062 1.88966 2 5 -2 20 9.87465 2.17546 2 -5 2 20 9.71285 1.69250 2 -5 -2 20 8.60078 1.60604 2 5 2 20 10.4921 2.12483 2 -6 2 20 15.7888 1.97652 2 6 -2 20 16.4888 2.54270 2 -6 -2 20 14.0158 1.95971 2 6 2 20 15.7806 2.41372 2 7 2 -20 3.82448 5.15999 1 7 -2 20 4.32851 5.62794 1 -7 2 20 10.1988 7.31669 1 -7 -2 20 4.16341 5.92196 1 7 -2 -20 7.67232 5.05412 1 7 2 20 11.0624 7.05669 1 0 -3 20 -0.2657 1.45704 2 0 3 20 0.97963 1.50701 2 1 -3 20 3.43479 1.85558 2 -1 3 20 2.03922 1.51075 2 -1 -3 20 0.98071 1.45940 2 1 3 20 0.50005 1.41318 2 -2 3 20 11.0560 1.72184 2 2 -3 20 10.2778 2.14727 2 -2 -3 20 9.25988 1.74732 2 2 3 20 12.2664 2.00006 2 -3 3 20 4.35200 1.49490 2 3 -3 20 1.72602 1.89452 2 -3 -3 20 6.61978 1.76450 2 3 3 20 4.19807 1.85232 2 4 -3 20 1.57812 1.93578 2 -4 3 20 0.96966 1.38496 2 4 3 20 3.79711 1.91322 2 -4 -3 20 1.65575 1.49099 2 5 -3 20 2.84814 2.10446 2 -5 3 20 -0.4213 1.36951 2 5 3 20 -0.0730 1.94950 2 -5 -3 20 4.00523 1.42334 2 0 4 20 0.97340 1.59329 2 0 -4 20 0.23683 1.67507 2 1 -4 20 2.01078 1.75846 2 -1 4 20 0.65807 1.55434 2 1 4 20 1.27857 1.61662 2 -1 -4 20 0.74268 1.57902 2 -2 4 20 -0.3403 1.35996 2 2 -4 20 -1.3233 1.76721 2 2 4 20 -3.5265 1.51453 2 -2 -4 20 -0.9510 1.52034 2 3 4 -20 -2.7040 4.25609 1 3 -4 20 -0.8089 4.26922 1 -3 4 20 4.17926 5.90359 1 -3 -4 20 2.34365 5.35724 1 3 4 20 -3.1147 6.00264 1 3 -4 -20 4.22298 4.85153 1 0 0 21 2.25674 1.72404 2 1 0 21 -0.5760 1.50957 2 -1 0 21 -1.1907 1.52675 2 -2 0 21 2.21596 1.67166 2 2 0 21 0.51956 1.72672 2 3 0 21 0.55663 1.77187 2 -3 0 21 -1.3063 1.28598 2 4 0 21 1.56824 1.79767 2 -4 0 21 -2.1546 1.49967 2 5 0 21 0.36316 2.08724 2 0 -1 21 -0.2490 1.62017 2 0 1 21 -1.1058 1.54451 2 -1 1 21 5.95513 1.80218 2 1 -1 21 2.75171 1.79881 2 1 1 21 9.45744 1.96926 2 -1 -1 21 9.07575 1.92225 2 2 -1 21 10.2650 2.04964 2 -2 1 21 4.69717 1.63671 2 2 1 21 10.8786 2.04860 2 -2 -1 21 6.52947 1.87784 2 -3 1 21 -2.0298 1.38245 2 3 -1 21 1.33401 1.83691 2 3 1 21 -0.2253 1.71947 2 -3 -1 21 -2.1490 1.46890 2 4 -1 21 21.5075 2.61721 2 -4 1 21 13.8772 2.03793 2 -4 -1 21 22.4981 2.49101 2 4 1 21 23.5510 2.65927 2 0 -2 21 2.37423 1.75445 2 0 2 21 2.20476 1.60417 2 -1 2 21 7.07185 1.80969 2 1 -2 21 2.83018 1.74632 2 1 2 21 7.14400 1.83961 2 -1 -2 21 6.08670 1.89177 2 -2 2 21 5.85068 1.71584 2 2 -2 21 5.57958 1.99153 2 -2 -2 21 4.21975 1.73453 2 2 2 21 7.61629 1.94236 2 3 -2 21 9.51774 2.17672 2 -3 2 21 9.56257 1.89382 2 -3 -2 21 10.4415 2.09574 2 3 2 21 10.0002 2.05862 2 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6393 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71073 16.850 9.199 18.098 90.001 89.978 90.007 ) ; _shelx_hkl_checksum 89510 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.38848(13) 0.3241(2) 0.38568(11) 0.0222(4) Uani 0.9416(13) 1 d D U P A 1 F1 F 0.44969(6) 0.25903(11) 0.42388(7) 0.0278(3) Uani 0.9416(13) 1 d D U P A 1 F2 F 0.32943(7) 0.22299(12) 0.37171(6) 0.0258(3) Uani 0.9416(13) 1 d D U P A 1 O2 O 0.34168(8) 0.73823(14) 0.25385(7) 0.0303(3) Uani 0.9416(13) 1 d D U P A 1 O3 O 0.41262(7) 0.40404(12) 0.32141(6) 0.0231(3) Uani 0.9416(13) 1 d D U P A 1 O8 O 0.35283(8) 0.44341(15) 0.43532(7) 0.0215(3) Uani 0.9416(13) 1 d D U P A 1 C1 C 0.28520(14) 0.5042(2) 0.23929(13) 0.0400(5) Uani 0.9416(13) 1 d D U P A 1 H1A H 0.2659 0.4400 0.2786 0.060 Uiso 0.9416(13) 1 calc R U P A 1 H1B H 0.3120 0.4462 0.2013 0.060 Uiso 0.9416(13) 1 calc R U P A 1 H1C H 0.2402 0.5558 0.2171 0.060 Uiso 0.9416(13) 1 calc R U P A 1 C2 C 0.34214(11) 0.6114(2) 0.27089(9) 0.0238(4) Uani 0.9416(13) 1 d D U P A 1 C3 C 0.40312(10) 0.55540(18) 0.32890(9) 0.0202(4) Uani 0.9416(13) 1 d D U P A 1 C4 C 0.48398(10) 0.63267(19) 0.32039(9) 0.0217(4) Uani 0.9416(13) 1 d D U P A 1 H4 H 0.4739 0.7396 0.3169 0.026 Uiso 0.9416(13) 1 calc R U P A 1 C5 C 0.53808(12) 0.6061(2) 0.38671(11) 0.0292(4) Uani 0.9416(13) 1 d D U P A 1 H5A H 0.5071 0.6201 0.4327 0.035 Uiso 0.9416(13) 1 calc R U P A 1 H5B H 0.5567 0.5040 0.3857 0.035 Uiso 0.9416(13) 1 calc R U P A 1 C6 C 0.60969(12) 0.7063(2) 0.38798(11) 0.0393(5) Uani 0.9416(13) 1 d D U P A 1 H6A H 0.6397 0.6952 0.3420 0.059 Uiso 0.9416(13) 1 calc R U P A 1 H6B H 0.6437 0.6813 0.4300 0.059 Uiso 0.9416(13) 1 calc R U P A 1 H6C H 0.5918 0.8073 0.3928 0.059 Uiso 0.9416(13) 1 calc R U P A 1 C7 C 0.52244(12) 0.5833(2) 0.24808(10) 0.0326(5) Uani 0.9416(13) 1 d D U P A 1 H7A H 0.5723 0.6363 0.2405 0.049 Uiso 0.9416(13) 1 calc R U P A 1 H7B H 0.4863 0.6030 0.2069 0.049 Uiso 0.9416(13) 1 calc R U P A 1 H7C H 0.5334 0.4788 0.2505 0.049 Uiso 0.9416(13) 1 calc R U P A 1 B1A B 0.4234(14) 0.342(2) 0.4162(12) 0.026(2) Uani 0.0584(13) 1 d D U P A 2 F1A F 0.4753(12) 0.281(2) 0.4655(11) 0.047(4) Uani 0.0584(13) 1 d D U P A 2 F2A F 0.3701(13) 0.237(2) 0.3923(11) 0.036(4) Uani 0.0584(13) 1 d D U P A 2 O2A O 0.5124(11) 0.7912(19) 0.3526(11) 0.032(4) Uani 0.0584(13) 1 d D U P A 2 O3A O 0.4571(11) 0.4186(17) 0.3543(9) 0.023(2) Uani 0.0584(13) 1 d D U P A 2 O8A O 0.3753(13) 0.461(2) 0.4561(12) 0.024(3) Uani 0.0584(13) 1 d D U P A 2 C1A C 0.5877(16) 0.581(3) 0.376(2) 0.038(5) Uani 0.0584(13) 1 d D U P A 2 H1D H 0.6328 0.6474 0.3698 0.057 Uiso 0.0584(13) 1 calc R U P A 2 H1E H 0.5933 0.4994 0.3415 0.057 Uiso 0.0584(13) 1 calc R U P A 2 H1F H 0.5865 0.5444 0.4266 0.057 Uiso 0.0584(13) 1 calc R U P A 2 C2A C 0.5124(13) 0.660(2) 0.3598(18) 0.026(3) Uani 0.0584(13) 1 d D U P A 2 C3A C 0.4357(12) 0.570(2) 0.3535(12) 0.024(2) Uani 0.0584(13) 1 d D U P A 2 C4A C 0.3898(13) 0.600(3) 0.2830(11) 0.021(2) Uani 0.0584(13) 1 d D U P A 2 H4A H 0.3774 0.7067 0.2836 0.025 Uiso 0.0584(13) 1 calc R U P A 2 C5A C 0.3117(13) 0.524(3) 0.2760(14) 0.024(3) Uani 0.0584(13) 1 d D U P A 2 H5C H 0.2780 0.5552 0.3180 0.029 Uiso 0.0584(13) 1 calc R U P A 2 H5D H 0.3216 0.4187 0.2821 0.029 Uiso 0.0584(13) 1 calc R U P A 2 C6A C 0.2638(16) 0.544(4) 0.2059(16) 0.029(5) Uani 0.0584(13) 1 d D U P A 2 H6D H 0.2175 0.4799 0.2069 0.044 Uiso 0.0584(13) 1 calc R U P A 2 H6E H 0.2969 0.5207 0.1630 0.044 Uiso 0.0584(13) 1 calc R U P A 2 H6F H 0.2461 0.6456 0.2024 0.044 Uiso 0.0584(13) 1 calc R U P A 2 C7A C 0.4463(15) 0.577(3) 0.2175(12) 0.028(5) Uani 0.0584(13) 1 d D U P A 2 H7D H 0.4156 0.5736 0.1715 0.041 Uiso 0.0584(13) 1 calc R U P A 2 H7E H 0.4747 0.4847 0.2239 0.041 Uiso 0.0584(13) 1 calc R U P A 2 H7F H 0.4846 0.6568 0.2152 0.041 Uiso 0.0584(13) 1 calc R U P A 2 C8 C 0.36457(9) 0.56952(18) 0.40628(9) 0.0225(4) Uani 1 1 d . . . . . N9 N 0.34083(8) 0.68639(15) 0.44054(7) 0.0221(3) Uani 1 1 d . . . . . C10 C 0.35160(10) 0.83861(18) 0.41664(9) 0.0253(4) Uani 1 1 d . . . . . H10A H 0.2994 0.8828 0.4054 0.030 Uiso 1 1 calc R U . . . H10B H 0.3845 0.8419 0.3713 0.030 Uiso 1 1 calc R U . . . C11 C 0.39193(11) 0.92232(19) 0.47789(10) 0.0315(4) Uani 1 1 d . . . . . H11A H 0.4456 0.8815 0.4865 0.038 Uiso 1 1 calc R U . . . H11B H 0.3981 1.0251 0.4628 0.038 Uiso 1 1 calc R U . . . O12 O 0.34714(8) 0.91555(13) 0.54484(7) 0.0341(3) Uani 1 1 d . . . . . C13 C 0.34108(11) 0.76868(19) 0.56872(9) 0.0296(4) Uani 1 1 d . . . . . H13A H 0.3117 0.7649 0.6161 0.036 Uiso 1 1 calc R U . . . H13B H 0.3950 0.7290 0.5773 0.036 Uiso 1 1 calc R U . . . C14 C 0.29868(10) 0.6764(2) 0.51200(8) 0.0259(4) Uani 1 1 d . . . . . H14A H 0.2972 0.5740 0.5287 0.031 Uiso 1 1 calc R U . . . H14B H 0.2433 0.7108 0.5061 0.031 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 0.0243(10) 0.0171(11) 0.0251(10) -0.0002(9) 0.0032(8) -0.0006(9) F1 0.0262(6) 0.0226(6) 0.0345(7) 0.0042(5) 0.0002(5) 0.0026(5) F2 0.0268(6) 0.0203(6) 0.0305(6) -0.0012(4) 0.0042(5) -0.0053(5) O2 0.0378(8) 0.0262(7) 0.0268(6) 0.0027(6) -0.0040(5) 0.0056(6) O3 0.0288(7) 0.0154(6) 0.0251(6) -0.0008(5) 0.0055(5) -0.0005(5) O8 0.0254(7) 0.0174(7) 0.0217(7) 0.0020(5) 0.0042(5) -0.0023(6) C1 0.0391(13) 0.0404(14) 0.0404(13) 0.0073(11) -0.0136(10) -0.0107(11) C2 0.0239(10) 0.0270(11) 0.0203(9) 0.0027(7) 0.0038(7) 0.0016(9) C3 0.0226(9) 0.0169(8) 0.0210(9) -0.0009(7) 0.0020(7) -0.0007(7) C4 0.0224(9) 0.0174(9) 0.0255(9) 0.0027(7) 0.0024(7) -0.0009(7) C5 0.0225(10) 0.0303(11) 0.0348(10) 0.0067(9) -0.0003(8) -0.0027(9) C6 0.0284(10) 0.0493(14) 0.0401(11) 0.0047(10) -0.0036(9) -0.0094(10) C7 0.0317(10) 0.0309(11) 0.0353(10) 0.0012(9) 0.0106(8) -0.0034(9) B1A 0.029(4) 0.021(4) 0.027(4) 0.002(4) 0.003(4) 0.001(4) F1A 0.050(9) 0.060(10) 0.029(8) 0.007(8) -0.008(8) 0.021(8) F2A 0.040(8) 0.027(8) 0.043(8) -0.001(7) 0.014(7) -0.003(8) O2A 0.021(7) 0.038(8) 0.037(7) 0.004(7) 0.001(6) -0.004(7) O3A 0.025(4) 0.018(4) 0.027(4) 0.004(4) 0.002(4) 0.002(4) O8A 0.024(5) 0.020(5) 0.027(5) 0.000(5) 0.000(5) -0.001(5) C1A 0.024(9) 0.042(10) 0.047(10) 0.001(9) -0.007(9) -0.007(9) C2A 0.021(5) 0.027(5) 0.029(5) 0.006(5) 0.001(5) -0.001(5) C3A 0.024(4) 0.019(4) 0.028(4) 0.002(4) 0.000(4) 0.000(4) C4A 0.023(4) 0.018(4) 0.022(4) 0.001(4) 0.000(4) 0.000(4) C5A 0.025(5) 0.024(5) 0.024(5) -0.001(5) 0.003(5) -0.002(5) C6A 0.018(9) 0.035(10) 0.036(10) 0.016(9) -0.010(9) -0.015(9) C7A 0.036(10) 0.030(11) 0.017(9) -0.002(9) -0.001(9) -0.005(10) C8 0.0208(8) 0.0203(9) 0.0265(8) 0.0032(7) 0.0004(6) -0.0007(7) N9 0.0221(7) 0.0195(7) 0.0245(7) 0.0002(6) 0.0022(6) 0.0005(6) C10 0.0264(9) 0.0191(9) 0.0305(9) 0.0020(7) 0.0024(7) 0.0039(7) C11 0.0354(10) 0.0200(9) 0.0390(10) 0.0027(8) -0.0043(8) -0.0015(8) O12 0.0488(8) 0.0227(7) 0.0308(7) -0.0030(5) -0.0043(6) 0.0030(6) C13 0.0364(10) 0.0261(10) 0.0263(9) 0.0002(7) -0.0021(7) 0.0025(8) C14 0.0263(9) 0.0266(9) 0.0249(8) -0.0016(7) 0.0059(7) 0.0003(7) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 F1 B1 F2 109.66(16) F1 B1 O3 114.69(16) F2 B1 O3 113.54(16) F1 B1 O8 107.96(15) F2 B1 O8 107.80(15) O3 B1 O8 102.60(15) C3 O3 B1 113.36(13) C8 O8 B1 110.11(14) C2 C1 H1A 109.5 C2 C1 H1B 109.5 H1A C1 H1B 109.5 C2 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 O2 C2 C1 122.54(18) O2 C2 C3 119.78(17) C1 C2 C3 117.68(17) O3 C3 C4 110.23(14) O3 C3 C8 102.56(13) C4 C3 C8 114.90(14) O3 C3 C2 109.70(14) C4 C3 C2 111.22(14) C8 C3 C2 107.82(13) C5 C4 C7 111.89(15) C5 C4 C3 111.95(14) C7 C4 C3 108.77(15) C5 C4 H4 108.0 C7 C4 H4 108.0 C3 C4 H4 108.0 C6 C5 C4 112.85(16) C6 C5 H5A 109.0 C4 C5 H5A 109.0 C6 C5 H5B 109.0 C4 C5 H5B 109.0 H5A C5 H5B 107.8 C5 C6 H6A 109.5 C5 C6 H6B 109.5 H6A C6 H6B 109.5 C5 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C4 C7 H7A 109.5 C4 C7 H7B 109.5 H7A C7 H7B 109.5 C4 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 F1A B1A F2A 108.8(18) F1A B1A O3A 117.3(19) F2A B1A O3A 110.6(18) F1A B1A O8A 108.8(18) F2A B1A O8A 107.5(18) O3A B1A O8A 103.2(15) B1A O3A C3A 112.4(15) C8 O8A B1A 106.2(14) C2A C1A H1D 109.5 C2A C1A H1E 109.5 H1D C1A H1E 109.5 C2A C1A H1F 109.5 H1D C1A H1F 109.5 H1E C1A H1F 109.5 O2A C2A C1A 120.4(19) O2A C2A C3A 121.9(19) C1A C2A C3A 117.7(18) O3A C3A C4A 108.2(17) O3A C3A C8 100.7(12) C4A C3A C8 97.3(14) O3A C3A C2A 108.2(15) C4A C3A C2A 113.0(17) C8 C3A C2A 127.7(18) C5A C4A C3A 115.6(17) C5A C4A C7A 114.4(18) C3A C4A C7A 108.0(17) C5A C4A H4A 106.0 C3A C4A H4A 106.0 C7A C4A H4A 106.0 C4A C5A C6A 119(2) C4A C5A H5C 107.6 C6A C5A H5C 107.6 C4A C5A H5D 107.6 C6A C5A H5D 107.6 H5C C5A H5D 107.1 C5A C6A H6D 109.5 C5A C6A H6E 109.5 H6D C6A H6E 109.5 C5A C6A H6F 109.5 H6D C6A H6F 109.5 H6E C6A H6F 109.5 C4A C7A H7D 109.5 C4A C7A H7E 109.5 H7D C7A H7E 109.5 C4A C7A H7F 109.5 H7D C7A H7F 109.5 H7E C7A H7F 109.5 O8 C8 N9 120.08(15) N9 C8 O8A 109.4(8) N9 C8 C3A 122.2(7) O8A C8 C3A 108.2(11) O8 C8 C3 110.95(14) N9 C8 C3 128.87(15) C8 N9 C10 127.22(14) C8 N9 C14 120.82(14) C10 N9 C14 111.96(13) N9 C10 C11 108.87(13) N9 C10 H10A 109.9 C11 C10 H10A 109.9 N9 C10 H10B 109.9 C11 C10 H10B 109.9 H10A C10 H10B 108.3 O12 C11 C10 111.30(14) O12 C11 H11A 109.4 C10 C11 H11A 109.4 O12 C11 H11B 109.4 C10 C11 H11B 109.4 H11A C11 H11B 108.0 C13 O12 C11 109.70(13) O12 C13 C14 111.15(14) O12 C13 H13A 109.4 C14 C13 H13A 109.4 O12 C13 H13B 109.4 C14 C13 H13B 109.4 H13A C13 H13B 108.0 N9 C14 C13 109.46(14) N9 C14 H14A 109.8 C13 C14 H14A 109.8 N9 C14 H14B 109.8 C13 C14 H14B 109.8 H14A C14 H14B 108.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance B1 F1 1.378(2) B1 F2 1.385(3) B1 O3 1.435(2) B1 O8 1.540(2) O2 C2 1.207(2) O3 C3 1.408(2) O8 C8 1.289(2) C1 C2 1.489(3) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C2 C3 1.556(2) C3 C4 1.543(2) C3 C8 1.549(2) C4 C5 1.526(3) C4 C7 1.529(2) C4 H4 1.0000 C5 C6 1.518(3) C5 H5A 0.9900 C5 H5B 0.9900 C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 B1A F1A 1.371(18) B1A F2A 1.393(18) B1A O3A 1.437(17) B1A O8A 1.538(18) O2A C2A 1.212(17) O3A C3A 1.439(17) O8A C8 1.36(2) C1A C2A 1.490(18) C1A H1D 0.9800 C1A H1E 0.9800 C1A H1F 0.9800 C2A C3A 1.538(17) C3A C4A 1.519(17) C3A C8 1.53(2) C4A C5A 1.495(18) C4A C7A 1.535(18) C4A H4A 1.0000 C5A C6A 1.515(19) C5A H5C 0.9900 C5A H5D 0.9900 C6A H6D 0.9800 C6A H6E 0.9800 C6A H6F 0.9800 C7A H7D 0.9800 C7A H7E 0.9800 C7A H7F 0.9800 C8 N9 1.304(2) N9 C10 1.477(2) N9 C14 1.478(2) C10 C11 1.511(2) C10 H10A 0.9900 C10 H10B 0.9900 C11 O12 1.428(2) C11 H11A 0.9900 C11 H11B 0.9900 O12 C13 1.422(2) C13 C14 1.511(2) C13 H13A 0.9900 C13 H13B 0.9900 C14 H14A 0.9900 C14 H14B 0.9900 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 F1 B1 O3 C3 -111.13(18) F2 B1 O3 C3 121.69(16) O8 B1 O3 C3 5.6(2) F1 B1 O8 C8 114.83(17) F2 B1 O8 C8 -126.77(15) O3 B1 O8 C8 -6.66(19) B1 O3 C3 C4 119.91(16) B1 O3 C3 C8 -2.90(19) B1 O3 C3 C2 -117.29(16) O2 C2 C3 O3 -159.36(15) C1 C2 C3 O3 21.6(2) O2 C2 C3 C4 -37.1(2) C1 C2 C3 C4 143.79(17) O2 C2 C3 C8 89.67(19) C1 C2 C3 C8 -89.39(19) O3 C3 C4 C5 -71.25(18) C8 C3 C4 C5 44.0(2) C2 C3 C4 C5 166.84(15) O3 C3 C4 C7 52.92(18) C8 C3 C4 C7 168.18(15) C2 C3 C4 C7 -68.99(18) C7 C4 C5 C6 70.4(2) C3 C4 C5 C6 -167.23(16) F1A B1A O3A C3A -118(2) F2A B1A O3A C3A 116(2) O8A B1A O3A C3A 1(2) F1A B1A O8A C8 143.6(18) F2A B1A O8A C8 -98.7(18) O3A B1A O8A C8 18(2) B1A O3A C3A C4A -119.0(19) B1A O3A C3A C8 -18(2) B1A O3A C3A C2A 118(2) O2A C2A C3A O3A 172(3) C1A C2A C3A O3A -8(3) O2A C2A C3A C4A 52(4) C1A C2A C3A C4A -128(3) O2A C2A C3A C8 -68(4) C1A C2A C3A C8 112(3) O3A C3A C4A C5A 64(2) C8 C3A C4A C5A -39(2) C2A C3A C4A C5A -176(2) O3A C3A C4A C7A -65(2) C8 C3A C4A C7A -168.9(18) C2A C3A C4A C7A 55(3) C3A C4A C5A C6A -178(3) C7A C4A C5A C6A -51(4) B1 O8 C8 N9 -178.16(15) B1 O8 C8 C3 5.23(19) B1A O8A C8 N9 -165.3(12) B1A O8A C8 C3A -30.0(19) O3A C3A C8 N9 158.1(9) C4A C3A C8 N9 -91.7(13) C2A C3A C8 N9 35(2) O3A C3A C8 O8A 29.8(17) C4A C3A C8 O8A 140.0(15) C2A C3A C8 O8A -93(2) O3 C3 C8 O8 -1.68(18) C4 C3 C8 O8 -121.29(16) C2 C3 C8 O8 114.07(16) O3 C3 C8 N9 -177.91(16) C4 C3 C8 N9 62.5(2) C2 C3 C8 N9 -62.2(2) O8 C8 N9 C10 177.89(15) O8A C8 N9 C10 154.0(11) C3A C8 N9 C10 26.2(9) C3 C8 N9 C10 -6.2(3) O8 C8 N9 C14 -1.4(2) O8A C8 N9 C14 -25.3(11) C3A C8 N9 C14 -153.1(9) C3 C8 N9 C14 174.53(15) C8 N9 C10 C11 -125.34(17) C14 N9 C10 C11 53.99(17) N9 C10 C11 O12 -57.62(18) C10 C11 O12 C13 61.70(18) C11 O12 C13 C14 -61.10(18) C8 N9 C14 C13 125.55(16) C10 N9 C14 C13 -53.84(18) O12 C13 C14 N9 56.96(19)