#------------------------------------------------------------------------------ #$Date: 2015-06-05 04:15:40 +0300 (Fri, 05 Jun 2015) $ #$Revision: 138088 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/52/03/1520312.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_1520312 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_name_full 'Organic Letters' _journal_page_first 150604140615001 _journal_paper_doi 10.1021/acs.orglett.5b01427 _journal_year 2015 _chemical_formula_sum 'C10 H16 B F2 N O4' _chemical_formula_weight 263.05 _chemical_name_common JR2102A3 _space_group_crystal_system orthorhombic _space_group_IT_number 45 _space_group_name_Hall 'I 2 -2c' _space_group_name_H-M_alt 'I b a 2' _symmetry_space_group_name_Hall 'I 2 -2c' _symmetry_space_group_name_H-M 'I b a 2' _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 16 _cell_length_a 12.1721(8) _cell_length_b 49.556(3) _cell_length_c 8.3410(6) _cell_measurement_reflns_used 6109 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.8900 _cell_measurement_theta_min 2.6502 _cell_volume 5031.3(6) _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 0.996 _diffrn_measured_fraction_theta_max 0.996 _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 0.0340 _diffrn_reflns_av_unetI/netI 0.0645 _diffrn_reflns_laue_measured_fraction_full 0.996 _diffrn_reflns_laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_k_min -58 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 9040 _diffrn_reflns_point_group_measured_fraction_full 0.965 _diffrn_reflns_point_group_measured_fraction_max 0.964 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.265 _diffrn_reflns_theta_min 2.466 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2208 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.190 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.044 _refine_ls_abs_structure_details ; Flack x determined using 1132 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.6(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 333 _refine_ls_number_reflns 4387 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0420 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+0.1512P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.0721 _reflns_Friedel_coverage 0.794 _reflns_friedel_fraction_full 0.927 _reflns_friedel_fraction_max 0.927 _reflns_number_gt 3362 _reflns_number_total 4387 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol5b01427_si_002.cif _cod_data_source_block JR2102A3_0m _cod_database_code 1520312 _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 0.981 _shelx_estimated_absorpt_t_max 0.995 _shelx_res_file ; JR2102A3_0m.res created by SHELXL-2014/7 TITL JR2102A3_0ma_a.res in Iba2 REM Old TITL JR2102A3_0ma in Iba2 REM SHELXT solution in Iba2 REM R1 0.110, Rweak 0.028, Alpha 0.002, Orientation as input REM Flack x = 0.322 ( 0.424 ) from Parsons' quotients REM Formula found by SHELXT: C18 B2 N2 O10 F4 CELL 0.71073 12.1721 49.5563 8.3410 90.0000 90.0000 90.0000 ZERR 16.000 0.0008 0.0033 0.0006 0.0000 0.0000 0.0000 LATT -2 SYMM -X, -Y, Z SYMM 1/2+X, 1/2-Y, Z SYMM 1/2-X, 1/2+Y, Z SFAC C H B N O F UNIT 160 256 16 16 64 32 TEMP -173.150 SIZE 0.04 0.11 0.16 L.S. 10 BOND $H LIST 4 acta bond $h conf FMAP 2 PLAN 10 WGHT 0.027800 0.151200 FVAR 0.18182 F1 6 0.355130 0.281905 0.536346 11.00000 0.04444 0.02891 = 0.02459 0.00507 -0.00409 0.00207 F2 6 0.492067 0.307349 0.433842 11.00000 0.01980 0.04075 = 0.03983 -0.00657 -0.00668 0.00376 F101 6 0.837830 0.472493 -0.037836 11.00000 0.02601 0.02877 = 0.01860 0.00256 0.00237 -0.00723 F102 6 0.703267 0.497367 0.075122 11.00000 0.02875 0.01760 = 0.03389 0.00394 -0.00500 0.00282 O4 5 0.311115 0.323467 0.414631 11.00000 0.02019 0.02253 = 0.02018 -0.00308 -0.00458 0.00376 O5 5 0.215636 0.367263 0.130096 11.00000 0.03236 0.02398 = 0.04403 0.00950 0.00051 0.00446 O8 5 0.365487 0.287076 0.254314 11.00000 0.02049 0.02008 = 0.02156 0.00058 -0.00088 0.00353 O11 5 0.200785 0.313229 -0.049134 11.00000 0.02216 0.03149 = 0.02075 0.00554 -0.00114 0.00542 O104 5 0.694041 0.450067 0.095352 11.00000 0.01758 0.01805 = 0.01724 0.00380 -0.00081 -0.00139 O105 5 0.557591 0.416782 0.394117 11.00000 0.02554 0.02723 = 0.03997 0.00614 0.00845 -0.00601 O108 5 0.825685 0.473555 0.244755 11.00000 0.01830 0.01504 = 0.01912 0.00201 -0.00230 -0.00295 O111 5 0.787302 0.427171 0.552419 11.00000 0.03334 0.01749 = 0.01690 0.00353 0.00151 -0.00339 N9 4 0.276797 0.296350 0.025199 11.00000 0.02023 0.02018 = 0.01878 0.00105 -0.00102 0.00360 N109 4 0.824944 0.450286 0.475971 11.00000 0.01866 0.01222 = 0.01621 0.00352 -0.00301 -0.00169 C1 1 0.035926 0.278671 0.239748 11.00000 0.03839 0.03157 = 0.04870 0.00728 -0.01874 -0.00833 AFIX 93 H1A 2 0.004953 0.285651 0.143783 11.00000 -1.20000 H1B 2 0.021151 0.260602 0.271101 11.00000 -1.20000 AFIX 0 C2 1 0.099400 0.294056 0.329397 11.00000 0.01799 0.02696 = 0.02429 0.00564 0.00357 0.00288 AFIX 43 H2 2 0.128900 0.286385 0.424485 11.00000 -1.20000 AFIX 0 C3 1 0.128461 0.322820 0.292150 11.00000 0.01423 0.02443 = 0.02096 0.00178 -0.00298 0.00108 AFIX 13 H3 2 0.090928 0.328058 0.190144 11.00000 -1.20000 AFIX 0 C4 1 0.254483 0.325562 0.267319 11.00000 0.01986 0.01956 = 0.01840 -0.00015 0.00009 0.00165 C5 1 0.285300 0.352865 0.187314 11.00000 0.02573 0.02190 = 0.02225 -0.00448 0.00220 -0.00016 C6 1 0.405107 0.359786 0.185738 11.00000 0.02856 0.02200 = 0.03772 0.00095 0.00944 -0.00443 AFIX 137 H6A 2 0.418356 0.374242 0.107926 11.00000 -1.50000 H6B 2 0.447792 0.343807 0.155562 11.00000 -1.50000 H6C 2 0.427545 0.365838 0.292693 11.00000 -1.50000 AFIX 0 C7 1 0.088001 0.341351 0.424919 11.00000 0.02286 0.03436 = 0.02552 0.00054 0.00312 0.00686 AFIX 137 H7A 2 0.007649 0.340541 0.430540 11.00000 -1.50000 H7B 2 0.111044 0.359910 0.402214 11.00000 -1.50000 H7C 2 0.119234 0.335546 0.527569 11.00000 -1.50000 AFIX 0 C8 1 0.300552 0.302017 0.172886 11.00000 0.01482 0.01527 = 0.01875 0.00312 0.00107 -0.00118 C10 1 0.305998 0.271801 -0.060243 11.00000 0.03279 0.02237 = 0.03048 -0.00732 0.00144 0.00225 AFIX 137 H10A 2 0.333016 0.276432 -0.167448 11.00000 -1.50000 H10B 2 0.241098 0.260210 -0.069828 11.00000 -1.50000 H10C 2 0.363561 0.262216 -0.001042 11.00000 -1.50000 AFIX 0 C12 1 0.252561 0.328459 -0.176375 11.00000 0.04089 0.03673 = 0.02316 0.01002 0.00174 0.00907 AFIX 137 H12A 2 0.203551 0.343055 -0.210567 11.00000 -1.50000 H12B 2 0.267435 0.316500 -0.267399 11.00000 -1.50000 H12C 2 0.321769 0.336138 -0.137349 11.00000 -1.50000 AFIX 0 C101 1 0.950346 0.399274 0.252664 11.00000 0.02325 0.02885 = 0.03890 -0.00329 0.00295 0.00471 AFIX 93 H10D 2 0.937615 0.392339 0.357208 11.00000 -1.20000 H10E 2 1.023026 0.400128 0.211470 11.00000 -1.20000 AFIX 0 C102 1 0.867088 0.407719 0.164684 11.00000 0.02482 0.01364 = 0.02159 -0.00343 0.00170 -0.00143 AFIX 43 H102 2 0.882864 0.414528 0.060734 11.00000 -1.20000 AFIX 0 C103 1 0.749081 0.407321 0.217399 11.00000 0.02052 0.01162 = 0.01707 0.00193 -0.00061 -0.00058 AFIX 13 H103 2 0.744396 0.397448 0.321734 11.00000 -1.20000 AFIX 0 C104 1 0.705720 0.436379 0.242977 11.00000 0.01680 0.01669 = 0.01281 0.00107 -0.00268 -0.00266 C105 1 0.593740 0.436947 0.333434 11.00000 0.01732 0.02027 = 0.02146 -0.00100 -0.00340 -0.00457 C106 1 0.535875 0.463564 0.338465 11.00000 0.01964 0.02610 = 0.03131 -0.00398 0.00037 0.00339 AFIX 137 H10F 2 0.515792 0.468990 0.229349 11.00000 -1.50000 H10G 2 0.584597 0.477179 0.385435 11.00000 -1.50000 H10H 2 0.469327 0.461961 0.403906 11.00000 -1.50000 AFIX 0 C107 1 0.678186 0.392561 0.095066 11.00000 0.02683 0.01717 = 0.02761 -0.00327 -0.00425 -0.00080 AFIX 137 H10I 2 0.683354 0.401719 -0.008792 11.00000 -1.50000 H10J 2 0.601577 0.392545 0.131205 11.00000 -1.50000 H10K 2 0.704021 0.373922 0.084091 11.00000 -1.50000 AFIX 0 C108 1 0.789790 0.453991 0.330833 11.00000 0.01282 0.00992 = 0.01994 -0.00097 0.00156 0.00600 C110 1 0.911655 0.465197 0.556079 11.00000 0.02217 0.02122 = 0.02161 -0.00241 -0.00670 -0.00320 AFIX 137 H11A 2 0.974426 0.453232 0.575060 11.00000 -1.50000 H11B 2 0.884389 0.472078 0.658791 11.00000 -1.50000 H11C 2 0.934701 0.480348 0.488478 11.00000 -1.50000 AFIX 0 C112 1 0.719614 0.433961 0.688240 11.00000 0.04466 0.03156 = 0.02162 -0.00081 0.01171 -0.01119 AFIX 137 H11D 2 0.670795 0.448940 0.659797 11.00000 -1.50000 H11E 2 0.766475 0.439318 0.778322 11.00000 -1.50000 H11F 2 0.675528 0.418244 0.718992 11.00000 -1.50000 AFIX 0 B1 3 0.383253 0.300529 0.419788 11.00000 0.02321 0.02759 = 0.01724 -0.00060 -0.00447 0.00147 B101 3 0.761864 0.473621 0.083645 11.00000 0.01802 0.01845 = 0.02120 0.00116 -0.00435 -0.00118 HKLF 4 REM JR2102A3_0ma_a.res in Iba2 REM R1 = 0.0420 for 3362 Fo > 4sig(Fo) and 0.0721 for all 4387 data REM 333 parameters refined using 1 restraints END WGHT 0.0278 0.1512 REM Highest difference peak 0.190, deepest hole -0.173, 1-sigma level 0.044 Q1 1 1.0000 0.5000 0.7103 10.50000 0.05 0.19 Q2 1 0.7236 0.4379 -0.0330 11.00000 0.05 0.18 Q3 1 0.3207 0.2610 0.0736 11.00000 0.05 0.18 Q4 1 0.7824 0.4239 0.2139 11.00000 0.05 0.17 Q5 1 0.3217 0.3464 -0.0584 11.00000 0.05 0.17 Q6 1 0.7328 0.4471 0.3019 11.00000 0.05 0.16 Q7 1 0.2303 0.2925 -0.2819 11.00000 0.05 0.16 Q8 1 0.7064 0.3798 0.0399 11.00000 0.05 0.16 Q9 1 0.6380 0.3558 0.1774 11.00000 0.05 0.16 Q10 1 0.1727 0.3273 0.0312 11.00000 0.05 0.16 ; _shelx_res_checksum 80902 _shelx_hkl_file ; 2 0 0 9999.99 168.127 1 -4 0 0 298.232 6.44109 1 4 0 0 274.624 6.45647 1 -6 0 0 70.9305 3.18392 1 6 0 0 64.5158 3.70228 1 -8 0 0 197.469 6.43552 1 -10 0 0 302.204 9.04404 1 -12 0 0 54.4736 5.87228 1 -14 0 0 -4.8002 4.85183 1 -3 -1 0 189.133 4.40251 1 3 -1 0 189.526 4.33724 1 -3 1 0 186.499 4.22291 1 3 1 0 182.671 4.46059 1 5 1 0 154.694 4.87662 1 5 -1 0 149.023 4.60572 1 -5 1 0 142.479 4.21237 1 -5 -1 0 150.845 4.41994 1 -7 1 0 165.611 5.19337 1 7 -1 0 154.097 5.98012 1 -7 -1 0 154.721 5.53681 1 -9 1 0 37.4844 3.67031 1 -9 -1 0 42.5666 3.94608 1 -11 -1 0 -4.4990 3.13379 1 -11 1 0 1.46634 3.09498 1 -13 1 0 42.7487 5.20972 1 -13 -1 0 53.1504 5.70803 1 2 2 0 401.221 7.64201 1 2 -2 0 396.717 7.20187 1 -2 2 0 385.004 7.11346 1 -4 2 0 59.0476 2.22654 1 4 2 0 57.2023 2.74644 1 4 -2 0 59.4244 2.41182 1 -4 -2 0 58.2801 2.44950 1 -6 -2 0 2.53768 1.41061 1 -6 2 0 -0.4156 1.16805 1 6 2 0 1.19578 1.55748 1 6 -2 0 0.22761 1.69264 1 -8 2 0 699.843 14.6118 1 -8 -2 0 697.231 15.0353 1 -10 2 0 2.67602 2.60126 1 -10 -2 0 1.03453 2.87960 1 -12 2 0 21.8793 3.95468 1 -12 -2 0 7.80642 3.98404 1 -14 2 0 0.87466 5.03895 1 -3 3 0 1052.92 18.5010 1 3 3 0 1084.04 19.3744 1 3 -3 0 1085.32 18.6354 1 -3 -3 0 1061.06 19.2063 1 -5 -3 0 235.472 6.01023 1 -5 3 0 233.478 5.53675 1 5 3 0 228.466 6.39175 1 5 -3 0 229.310 5.87231 1 7 -3 0 198.682 6.48082 1 -7 3 0 202.730 5.73977 1 -7 -3 0 206.043 6.37262 1 -9 3 0 20.9788 2.95643 1 -9 -3 0 24.8746 3.25640 1 -11 3 0 20.6887 3.54083 1 -11 -3 0 27.6151 4.05926 1 -13 -3 0 63.6090 6.30999 1 -13 3 0 68.3598 7.13344 1 -2 -4 0 25.2877 1.39900 1 2 4 0 26.4819 1.45454 1 -2 4 0 25.9272 0.88824 1 2 -4 0 25.6032 0.93434 1 4 -4 0 139.250 3.73443 1 -4 4 0 141.133 3.55348 1 -4 -4 0 142.555 4.21011 1 4 4 0 138.210 4.46800 1 6 -4 0 840.023 16.7513 1 6 4 0 847.997 17.6803 1 -6 -4 0 889.898 17.2914 1 -6 4 0 879.067 16.3268 1 8 -4 0 10.8013 3.43674 1 -8 -4 0 10.1607 2.54806 1 -8 4 0 12.3480 2.63015 1 -10 -4 0 1.15204 2.41051 1 -10 4 0 -0.8577 2.35371 1 -12 4 0 -8.5125 2.99504 1 -12 -4 0 -2.7635 3.91004 1 -14 -4 0 4.42495 5.11010 1 -1 5 0 59.9825 1.33587 1 1 -5 0 67.3546 1.42729 1 1 5 0 61.8029 1.94406 1 -1 -5 0 62.4958 1.94558 1 3 5 0 58.4724 2.56640 1 3 -5 0 62.7816 1.87922 1 -3 -5 0 61.8042 2.55166 1 -3 5 0 62.4314 1.77324 1 5 5 0 654.878 13.8170 1 5 -5 0 650.802 12.5990 1 -5 -5 0 642.215 13.2752 1 -5 5 0 664.451 12.3263 1 -7 5 0 47.7210 2.99442 1 7 -5 0 49.2495 3.79269 1 -7 -5 0 49.4988 3.35302 1 -9 5 0 203.629 6.53146 1 -9 -5 0 196.808 7.24268 1 -11 -5 0 85.4390 6.24141 1 -11 5 0 93.4646 5.37311 1 -13 5 0 5.19501 4.05169 1 -13 -5 0 -0.1558 4.32075 1 0 6 0 372.782 7.01527 1 0 -6 0 379.773 6.98095 1 2 6 0 347.284 7.37250 1 -2 -6 0 349.839 7.28220 1 2 -6 0 347.945 6.11737 1 -2 6 0 352.964 6.10937 1 4 -6 0 28.6547 1.60409 1 4 6 0 27.5464 2.27379 1 -4 -6 0 29.5768 2.09164 1 -4 6 0 30.6085 1.41892 1 -6 -6 0 12.8869 1.96007 1 -6 6 0 12.7678 1.57065 1 6 -6 0 14.7231 1.95680 1 -8 -6 0 14.9368 2.75750 1 8 -6 0 6.58650 2.56597 1 -8 6 0 14.7828 2.12460 1 -10 -6 0 129.684 6.27734 1 -10 6 0 131.845 5.59447 1 -12 6 0 33.2490 4.25245 1 -12 -6 0 41.1172 5.40719 1 -14 -6 0 -0.1238 5.16301 1 1 -7 0 505.973 9.43499 1 1 -7 0 564.519 9.45373 1 1 7 0 568.256 10.3438 1 -1 -7 0 540.316 10.2011 1 -3 7 0 530.695 9.39329 1 3 7 0 523.350 10.9922 1 3 -7 0 548.502 9.48463 1 5 7 0 5.94383 1.87188 1 -5 -7 0 6.63340 1.46695 1 -5 7 0 7.04538 1.04486 1 5 -7 0 6.78080 1.32265 1 -7 -7 0 70.9423 4.00761 1 7 -7 0 77.3428 4.04588 1 -7 7 0 68.6687 3.14985 1 -9 7 0 0.96335 1.83024 1 -9 -7 0 -2.8750 2.79940 1 -11 -7 0 8.20378 3.50469 1 -11 7 0 3.22838 2.63655 1 -13 -7 0 23.3549 8.27928 1 -13 7 0 12.4584 4.39075 1 0 -8 0 7715.55 131.239 1 0 8 0 7971.97 133.467 1 2 -8 0 631.023 10.6533 1 -2 -8 0 630.628 12.2255 1 -2 8 0 620.580 10.7611 1 2 8 0 644.383 12.4448 1 4 -8 0 196.592 4.27654 1 4 8 0 202.362 5.83798 1 -4 8 0 188.208 4.07278 1 -4 -8 0 185.461 5.49182 1 -6 -8 0 9.90502 1.88913 1 -6 8 0 6.05575 1.21009 1 6 -8 0 7.21814 1.66756 1 -8 8 0 14.0841 2.06983 1 8 -8 0 13.0862 2.70620 1 -8 -8 0 13.7079 2.53254 1 -10 8 0 120.662 5.36970 1 -10 -8 0 131.729 6.72330 1 -12 8 0 21.5007 3.70815 1 -12 -8 0 8.15090 3.88119 1 -14 -8 0 -6.9360 5.22247 1 -1 9 0 12.4347 0.95952 1 1 -9 0 12.3243 0.88604 1 1 9 0 13.0812 1.43085 1 -1 -9 0 12.1282 1.18249 1 1 -9 0 11.9272 0.97338 1 3 9 0 1772.29 32.1424 1 -3 -9 0 1772.72 31.8653 1 3 -9 0 1832.43 30.0228 1 -3 9 0 1833.33 30.0281 1 5 -9 0 2.14192 0.98988 1 -5 -9 0 -0.1029 1.56457 1 5 9 0 4.70129 2.06850 1 -5 9 0 2.14134 0.83842 1 7 -9 0 65.0746 3.84200 1 -7 9 0 70.9858 3.07639 1 -7 -9 0 67.3169 4.23305 1 -9 -9 0 6.10393 2.59726 1 9 -9 0 8.49960 3.41806 1 -11 9 0 -0.5680 2.78303 1 -11 -9 0 0.95640 3.50019 1 -13 -9 0 3.69212 4.33872 1 0 -10 0 407.114 7.86873 1 0 10 0 399.959 7.97641 1 -2 -10 0 79.3718 2.95860 1 2 -10 0 82.4251 2.04654 1 2 -10 0 82.0353 1.79150 1 -2 10 0 83.6539 1.96053 1 2 10 0 77.3939 3.04978 1 4 10 0 1.49302 1.44619 1 4 -10 0 0.83545 0.65559 1 -4 -10 0 1.43717 1.18783 1 -4 10 0 1.24312 0.57525 1 -6 -10 0 52.1607 3.37720 1 -6 10 0 53.0904 2.33340 1 6 -10 0 50.4274 2.69921 1 -8 10 0 179.586 5.16000 1 -8 -10 0 178.533 6.73255 1 8 -10 0 161.986 5.97567 1 -10 -10 0 32.8335 4.49087 1 -10 10 0 30.2296 3.24673 1 -12 -10 0 21.7920 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-4 -30 8 17.7508 7.30905 1 -1 -31 -8 31.8049 10.7363 1 1 -31 8 26.1418 7.21652 1 -1 31 8 8.43285 8.43343 1 1 31 8 17.4019 8.61278 1 1 -31 -8 23.4469 10.0020 1 -1 -31 8 21.0347 6.25347 1 -3 -31 -8 -1.3184 9.45147 1 -3 31 8 17.0812 8.52085 1 -3 -31 8 -6.6620 6.52470 1 3 -31 -8 -8.8081 9.87385 1 0 -32 8 4.86398 7.11174 1 0 -32 -8 10.4954 9.63847 1 0 32 8 20.1983 9.88009 1 -2 -32 -8 25.9374 10.3974 1 -2 32 8 6.37057 8.88292 1 2 -32 8 7.23059 9.33779 1 -2 -32 8 0.80954 6.43072 1 2 -32 -8 13.2684 9.97433 1 1 -33 8 13.2137 7.64779 1 -1 -33 -8 20.7008 11.5323 1 -1 33 8 23.9712 8.70040 1 1 33 8 8.18721 9.02792 1 1 -33 -8 8.09558 10.4055 1 -1 -33 8 16.1614 6.95061 1 -3 33 8 -2.0789 9.68504 1 -3 -33 -8 -4.6022 9.55369 1 -3 -33 8 9.80801 6.93871 1 3 -33 -8 29.3457 10.5652 1 0 -34 -8 -0.6048 10.1978 1 0 -34 8 9.62005 7.31890 1 0 34 8 -7.6091 7.92012 1 -2 34 8 16.5881 8.32653 1 -2 -34 -8 3.21487 9.93768 1 -2 -34 8 -13.311 6.61644 1 2 -34 -8 -10.772 9.28010 1 -1 -35 -8 26.2576 10.7308 1 1 -35 8 14.0207 7.85514 1 -1 35 8 12.6478 9.86449 1 1 -35 -8 19.8367 11.5601 1 -1 -35 8 14.6743 7.16978 1 -1 0 9 12.9275 7.09683 1 1 0 9 0.14195 7.05049 1 3 0 9 -7.4004 7.83610 1 -3 0 9 -8.4823 6.59541 1 -5 0 9 -3.6695 6.98469 1 -5 0 -9 4.34278 8.42634 1 5 0 9 -13.473 8.36843 1 0 -1 9 7.55659 7.86718 1 0 1 9 -6.4774 6.46454 1 -2 1 9 6.25474 7.00924 1 2 -1 9 5.37435 7.10441 1 2 1 9 1.62408 6.73032 1 -2 -1 9 19.3885 7.22880 1 -4 1 9 -8.7167 6.70510 1 4 -1 9 5.29126 8.28812 1 -4 -1 -9 -8.6488 8.31379 1 -4 -1 9 6.59377 6.77603 1 4 1 9 5.84493 8.60610 1 -4 1 -9 -4.7234 8.71993 1 6 -1 9 7.65020 8.86963 1 -6 -1 -9 20.5861 10.5516 1 -6 1 9 1.89997 7.97275 1 -6 1 -9 -1.5865 8.70807 1 -6 -1 9 -6.8291 7.11775 1 6 1 9 0.00119 7.73732 1 -1 2 9 80.4580 9.82694 1 1 -2 9 100.199 10.9363 1 -1 -2 9 104.625 10.7890 1 1 2 9 93.3709 10.0339 1 -3 2 9 115.530 11.3665 1 3 -2 9 86.8656 10.4123 1 3 2 9 72.7336 10.2383 1 -3 -2 9 89.9525 10.4126 1 -5 2 9 14.9636 7.23303 1 -5 -2 -9 8.36630 9.31924 1 5 -2 9 17.8980 9.34523 1 5 2 9 35.4790 9.72822 1 -5 -2 9 19.9616 7.07915 1 -5 2 -9 35.0620 10.7929 1 0 3 9 1.23136 6.75061 1 0 -3 9 -3.6736 7.03066 1 2 -3 9 10.0337 8.15104 1 -2 3 9 2.39442 6.36637 1 2 3 9 3.92723 7.63089 1 -2 -3 9 8.91422 6.72335 1 -4 3 9 -20.150 7.16950 1 -4 -3 -9 9.21261 8.94431 1 4 -3 9 14.0259 7.51050 1 -4 -3 9 -8.6613 6.53332 1 4 3 9 -3.6792 8.24985 1 -6 -3 -9 13.0691 10.6957 1 -6 3 9 2.88842 8.16606 1 6 -3 9 15.6982 9.26279 1 -6 -3 9 14.1665 7.47990 1 -6 3 -9 22.6515 10.1848 1 6 3 9 3.44232 8.90267 1 -1 4 9 4.06698 7.01696 1 1 -4 9 4.64903 6.51000 1 -1 -4 9 9.30932 7.78926 1 1 4 9 17.7174 8.15364 1 3 -4 9 21.2009 7.67442 1 -3 4 9 20.5273 7.39021 1 3 4 9 23.5532 7.79997 1 -3 -4 9 14.0040 6.93156 1 5 -4 9 18.2237 9.04890 1 -5 -4 -9 20.0048 9.44674 1 -5 4 9 32.3702 8.14753 1 -5 -4 9 14.5419 8.12048 1 -5 4 -9 9.20577 10.1303 1 5 4 9 25.2820 9.44259 1 0 -5 9 -2.4502 6.31051 1 0 5 9 -6.9292 6.66822 1 2 -5 9 8.59269 7.10118 1 -2 5 9 2.20249 7.09030 1 2 5 9 -2.8729 7.98295 1 -2 -5 9 -6.6604 6.45288 1 -4 -5 -9 -15.142 9.21764 1 -4 5 9 10.1200 7.38447 1 4 -5 9 11.5708 7.21622 1 4 5 9 19.0958 8.06139 1 -4 -5 9 18.6661 7.92148 1 6 -5 9 3.75172 7.68932 1 -6 -5 -9 -9.1742 9.21842 1 -6 5 9 4.57855 8.21181 1 -6 5 -9 19.2349 10.1605 1 6 5 9 4.01559 9.32766 1 -6 -5 9 16.2504 8.58317 1 1 -6 9 36.3657 8.83840 1 -1 6 9 44.7100 8.36150 1 -1 -6 9 41.2951 7.92762 1 1 6 9 32.0314 8.49568 1 -3 6 9 8.08999 7.54613 1 3 -6 9 -3.4528 7.56185 1 -3 -6 -9 -0.2086 10.3042 1 3 6 9 20.0764 8.84370 1 -3 -6 9 14.6402 6.83709 1 -5 6 9 16.8794 8.21026 1 -5 -6 -9 34.0154 10.1184 1 5 -6 9 20.9163 8.34117 1 5 6 9 32.7143 10.0265 1 -5 -6 9 26.7937 8.06725 1 -5 6 -9 34.0546 10.4055 1 0 7 9 7.64930 7.77170 1 0 -7 9 11.6315 6.75933 1 -2 7 9 7.12252 7.24570 1 2 -7 9 -6.3897 6.54910 1 -2 -7 9 0.41804 7.02963 1 2 7 9 -2.4665 7.65373 1 -4 7 9 2.99958 7.72324 1 4 -7 9 -4.7032 8.23226 1 -4 -7 -9 11.6939 9.18537 1 4 7 9 -2.7121 7.30145 1 -4 -7 9 2.80790 6.96428 1 -6 7 9 0.60568 8.04878 1 -6 -7 -9 6.04520 9.82103 1 6 -7 9 13.1911 8.90731 1 -6 -7 9 2.46793 7.25545 1 6 7 9 7.58693 9.65817 1 -6 7 -9 6.67654 10.0185 1 -1 8 9 -0.2301 6.75697 1 1 -8 9 4.58382 7.70019 1 1 8 9 -1.7880 7.37416 1 -1 -8 9 14.8031 8.04577 1 -3 8 9 33.8250 8.12378 1 3 -8 9 45.5021 9.25610 1 -3 -8 -9 31.8275 10.7882 1 -3 -8 9 27.9471 8.14945 1 3 8 9 38.2434 8.37043 1 5 -8 9 -1.8068 8.23267 1 -5 -8 -9 28.0454 10.6898 1 -5 8 9 15.4862 8.07997 1 -5 -8 9 8.23625 7.10184 1 -5 8 -9 -1.2516 8.61271 1 5 8 9 19.2343 9.21759 1 0 -9 9 -4.8936 7.25594 1 0 9 9 -5.3057 7.26111 1 2 -9 9 -1.2144 8.01453 1 -2 9 9 -3.3791 6.70243 1 -2 -9 9 1.69585 5.79384 1 2 9 9 0.56941 7.05117 1 4 -9 9 9.98707 8.17636 1 -4 9 9 0.80728 8.02428 1 -4 -9 -9 15.5236 9.64343 1 -4 -9 9 -6.6097 7.62629 1 4 9 9 1.43979 8.74800 1 -6 9 9 8.15019 8.54845 1 6 -9 9 36.5219 9.40232 1 -6 -9 -9 18.0884 10.3266 1 -6 9 -9 -2.0549 9.80628 1 -6 -9 9 27.0475 8.60900 1 -1 10 9 110.199 11.9277 1 1 -10 9 67.8427 9.27234 1 -1 -10 9 100.342 10.7262 1 1 10 9 69.8013 10.1627 1 -3 10 9 35.3912 9.94329 1 -3 -10 -9 33.0034 11.0355 1 3 -10 9 47.1816 9.38016 1 -3 -10 9 52.0903 8.25938 1 3 10 9 35.3517 8.84171 1 -5 10 9 8.43481 8.01092 1 -5 -10 -9 11.0216 11.5700 1 5 -10 9 0.22310 8.21378 1 5 10 9 -0.0430 7.80722 1 -5 10 -9 -15.364 9.86596 1 -5 -10 9 11.6707 7.58888 1 0 11 9 -6.9577 7.52452 1 0 -11 9 5.28213 6.95903 1 -2 11 9 -6.9894 7.89822 1 2 -11 9 -0.6367 7.95997 1 2 11 9 10.4696 8.52895 1 -2 -11 9 -13.092 5.78848 1 4 -11 9 30.4650 8.61347 1 -4 11 9 29.5834 8.49309 1 -4 -11 -9 7.41353 10.7344 1 -4 -11 9 29.6781 7.75945 1 4 11 9 27.8056 8.22011 1 -1 12 9 29.4304 8.35705 1 1 -12 9 22.5376 7.41287 1 -1 -12 9 18.9200 7.24306 1 1 12 9 11.6634 7.69408 1 3 -12 9 17.4869 8.33103 1 -3 -12 -9 2.61974 9.22724 1 -3 12 9 13.3697 7.75515 1 3 12 9 8.18391 8.14401 1 -3 -12 9 17.0178 7.28833 1 5 -12 9 2.19414 8.73511 1 -5 -12 -9 5.38776 10.7740 1 -5 12 9 4.00406 8.34629 1 5 12 9 1.72532 8.49765 1 -5 12 -9 2.32140 9.96498 1 -5 -12 9 12.7648 7.15071 1 0 -13 9 13.1885 6.84520 1 0 13 9 2.48777 7.40955 1 -2 -13 -9 12.5696 10.3307 1 -2 13 9 15.7613 7.83639 1 2 -13 9 28.6516 8.45135 1 2 13 9 13.1968 7.89529 1 -2 -13 9 19.7568 7.65272 1 4 -13 9 0.13267 8.24711 1 -4 -13 -9 17.8147 10.0299 1 -4 13 9 4.87522 8.92815 1 -4 -13 9 12.5255 7.15682 1 4 13 9 7.98944 8.35559 1 1 -14 9 9.83892 6.90847 1 -1 14 9 15.3069 7.78899 1 -1 -14 9 10.8169 6.57762 1 1 14 9 2.23487 7.43632 1 3 -14 9 17.8522 7.15634 1 -3 -14 -9 1.23647 10.4213 1 -3 14 9 0.52479 7.83109 1 -3 -14 9 4.44103 6.96144 1 3 14 9 -1.6374 7.84269 1 -5 -14 -9 24.5274 9.92037 1 5 -14 9 11.5704 8.42546 1 -5 14 9 2.36408 8.20605 1 5 14 9 0.86326 8.67424 1 -5 -14 9 9.22225 7.84278 1 0 15 9 -3.0671 7.47914 1 0 -15 9 0.59098 6.39669 1 2 -15 9 12.6354 8.35057 1 -2 -15 -9 5.19467 9.08983 1 -2 15 9 9.49566 7.85231 1 -2 -15 9 17.3783 7.47679 1 2 15 9 8.22609 7.60339 1 -4 -15 -9 10.7459 10.2584 1 4 -15 9 8.96463 8.72349 1 -4 15 9 -4.0247 7.62892 1 -4 -15 9 5.60936 7.17136 1 4 15 9 12.5494 8.85647 1 1 -16 9 38.9199 8.13196 1 -1 16 9 26.0401 8.44239 1 -1 -16 9 31.9948 8.32046 1 1 16 9 40.4616 9.02486 1 -3 16 9 2.37265 8.65810 1 3 -16 9 0.71184 7.70726 1 -3 -16 -9 7.40855 9.44162 1 -3 -16 9 7.98222 7.82031 1 3 16 9 2.75308 9.15298 1 -5 -16 -9 -14.644 9.67093 1 5 -16 9 7.60083 8.51122 1 -5 16 9 -8.7506 8.90141 1 -5 -16 9 6.74907 7.97424 1 0 17 9 -16.738 7.24669 1 0 -17 9 -6.9987 6.71043 1 -2 -17 -9 24.1268 10.1446 1 -2 17 9 48.5454 9.23292 1 2 -17 9 38.2510 9.16721 1 2 17 9 35.3873 9.36276 1 -2 -17 9 33.4635 7.79080 1 -4 -17 -9 12.2910 10.7461 1 4 -17 9 6.39733 8.54840 1 -4 17 9 5.82760 8.86783 1 4 17 9 12.9016 8.40163 1 -4 -17 9 3.95663 7.21298 1 -1 18 9 21.5637 9.96885 1 -1 -18 -9 18.5975 11.8173 1 1 -18 9 19.4098 7.39477 1 1 18 9 34.4948 9.24835 1 -1 -18 9 13.2160 7.82122 1 3 -18 9 2.59903 8.59498 1 -3 18 9 10.3535 8.37483 1 -3 -18 -9 13.8711 10.2490 1 3 18 9 16.2308 8.27037 1 -3 -18 9 32.2678 8.46290 1 0 -19 9 -4.6677 6.57694 1 0 19 9 5.24024 8.23048 1 2 -19 9 -0.7988 6.93148 1 -2 -19 -9 18.0905 11.1593 1 -2 19 9 -10.846 7.37133 1 2 19 9 -2.1722 7.64709 1 -2 -19 9 11.0701 7.83600 1 -4 -19 -9 14.2853 12.2556 1 4 -19 9 7.34233 8.73967 1 -4 19 9 18.6205 8.73752 1 -4 -19 9 17.6038 7.42467 1 4 19 9 -8.6225 8.97827 1 1 -20 9 9.11309 7.65593 1 -1 20 9 -10.390 7.59656 1 -1 -20 -9 6.40561 11.2959 1 1 20 9 -5.5111 8.37164 1 -1 -20 9 18.4798 6.93054 1 3 -20 9 -2.1290 8.31986 1 -3 -20 -9 10.4580 9.82430 1 -3 20 9 5.69718 9.40921 1 3 20 9 -8.5393 8.58632 1 -3 -20 9 4.72227 6.83780 1 0 -21 9 1.83408 7.48977 1 0 -21 -9 0.83696 10.0427 1 0 21 9 -6.9105 8.14046 1 2 -21 9 44.7065 9.52578 1 -2 -21 -9 -1.5945 11.0435 1 -2 21 9 34.7491 10.0604 1 2 21 9 34.1188 8.98932 1 -2 -21 9 48.5964 8.67823 1 -1 22 9 8.84157 8.29979 1 1 -22 9 18.1593 8.50931 1 -1 -22 -9 20.1738 11.4524 1 1 22 9 12.4234 9.10000 1 -1 -22 9 20.5773 7.09890 1 -3 22 9 -24.942 7.80914 1 3 -22 9 -4.4743 8.26211 1 -3 -22 -9 2.37607 11.5378 1 3 22 9 10.5620 9.14709 1 -3 -22 9 3.63123 6.94879 1 0 -23 -9 -11.479 10.0249 1 0 -23 9 -0.2858 7.36951 1 0 23 9 -2.9523 8.79035 1 2 -23 9 21.3921 8.32582 1 -2 23 9 -1.1793 9.90140 1 -2 -23 -9 -5.6988 11.3426 1 2 23 9 21.4240 9.97742 1 -2 -23 9 -7.5949 7.06080 1 -1 24 9 -2.1049 9.50565 1 1 -24 9 -14.194 6.93103 1 -1 -24 -9 0.99729 10.0150 1 1 24 9 -8.7108 8.24070 1 1 -24 -9 -15.136 12.4230 1 -1 -24 9 3.05031 7.59837 1 0 -25 -9 -8.0171 11.4291 1 0 -25 9 -2.8074 6.78166 1 0 25 9 -3.9533 8.66289 1 0 0 10 84.7111 11.4340 1 0 2 10 88.8131 11.4753 1 0 -2 10 75.1043 10.6595 1 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/4' _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9171 _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 12.165 49.583 8.348 89.957 89.995 89.998 ) ; _shelx_hkl_checksum 47042 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1, y+1, 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 F1 F 0.35513(17) 0.28191(4) 0.5363(3) 0.0326(6) Uani 1 1 d . . F2 F 0.49207(15) 0.30735(3) 0.4338(3) 0.0335(6) Uani 1 1 d . . F101 F 0.83783(14) 0.47249(4) -0.0378(2) 0.0245(5) Uani 1 1 d . . F102 F 0.70327(13) 0.49737(4) 0.0751(3) 0.0267(5) Uani 1 1 d . . O4 O 0.31112(16) 0.32347(4) 0.4146(3) 0.0210(6) Uani 1 1 d . . O5 O 0.2156(2) 0.36726(5) 0.1301(3) 0.0335(7) Uani 1 1 d . . O8 O 0.36549(18) 0.28708(4) 0.2543(3) 0.0207(6) Uani 1 1 d . . O11 O 0.20078(16) 0.31323(4) -0.0491(3) 0.0248(6) Uani 1 1 d . . O104 O 0.69404(16) 0.45007(4) 0.0954(3) 0.0176(6) Uani 1 1 d . . O105 O 0.55759(18) 0.41678(5) 0.3941(3) 0.0309(7) Uani 1 1 d . . O108 O 0.82569(16) 0.47356(4) 0.2448(3) 0.0175(6) Uani 1 1 d . . O111 O 0.78730(18) 0.42717(4) 0.5524(3) 0.0226(6) Uani 1 1 d . . N9 N 0.2768(2) 0.29635(5) 0.0252(4) 0.0197(7) Uani 1 1 d . . N109 N 0.8249(2) 0.45029(5) 0.4760(4) 0.0157(7) Uani 1 1 d . . C1 C 0.0359(3) 0.27867(7) 0.2397(6) 0.0396(12) Uani 1 1 d . . H1A H 0.0050 0.2857 0.1438 0.047 Uiso 1 1 calc R U H1B H 0.0212 0.2606 0.2711 0.047 Uiso 1 1 calc R U C2 C 0.0994(3) 0.29406(7) 0.3294(5) 0.0231(9) Uani 1 1 d . . H2 H 0.1289 0.2864 0.4245 0.028 Uiso 1 1 calc R U C3 C 0.1285(3) 0.32282(7) 0.2921(4) 0.0199(9) Uani 1 1 d . . H3 H 0.0909 0.3281 0.1901 0.024 Uiso 1 1 calc R U C4 C 0.2545(3) 0.32556(7) 0.2673(4) 0.0193(9) Uani 1 1 d . . C5 C 0.2853(3) 0.35287(7) 0.1873(5) 0.0233(9) Uani 1 1 d . . C6 C 0.4051(3) 0.35979(7) 0.1857(5) 0.0294(10) Uani 1 1 d . . H6A H 0.4184 0.3742 0.1079 0.044 Uiso 1 1 calc R U H6B H 0.4478 0.3438 0.1556 0.044 Uiso 1 1 calc R U H6C H 0.4275 0.3658 0.2927 0.044 Uiso 1 1 calc R U C7 C 0.0880(3) 0.34135(7) 0.4249(5) 0.0276(9) Uani 1 1 d . . H7A H 0.0076 0.3405 0.4305 0.041 Uiso 1 1 calc R U H7B H 0.1110 0.3599 0.4022 0.041 Uiso 1 1 calc R U H7C H 0.1192 0.3355 0.5276 0.041 Uiso 1 1 calc R U C8 C 0.3006(3) 0.30202(6) 0.1729(4) 0.0163(8) Uani 1 1 d . . C10 C 0.3060(3) 0.27180(6) -0.0602(5) 0.0285(10) Uani 1 1 d . . H10A H 0.3330 0.2764 -0.1674 0.043 Uiso 1 1 calc R U H10B H 0.2411 0.2602 -0.0698 0.043 Uiso 1 1 calc R U H10C H 0.3636 0.2622 -0.0010 0.043 Uiso 1 1 calc R U C12 C 0.2526(3) 0.32846(8) -0.1764(5) 0.0336(10) Uani 1 1 d . . H12A H 0.2036 0.3431 -0.2106 0.050 Uiso 1 1 calc R U H12B H 0.2674 0.3165 -0.2674 0.050 Uiso 1 1 calc R U H12C H 0.3218 0.3361 -0.1373 0.050 Uiso 1 1 calc R U C101 C 0.9503(3) 0.39927(6) 0.2527(5) 0.0303(10) Uani 1 1 d . . H10D H 0.9376 0.3923 0.3572 0.036 Uiso 1 1 calc R U H10E H 1.0230 0.4001 0.2115 0.036 Uiso 1 1 calc R U C102 C 0.8671(3) 0.40772(6) 0.1647(4) 0.0200(9) Uani 1 1 d . . H102 H 0.8829 0.4145 0.0607 0.024 Uiso 1 1 calc R U C103 C 0.7491(2) 0.40732(6) 0.2174(4) 0.0164(8) Uani 1 1 d . . H103 H 0.7444 0.3974 0.3217 0.020 Uiso 1 1 calc R U C104 C 0.7057(2) 0.43638(7) 0.2430(4) 0.0154(8) Uani 1 1 d . . C105 C 0.5937(3) 0.43695(7) 0.3334(5) 0.0197(8) Uani 1 1 d . . C106 C 0.5359(3) 0.46356(6) 0.3385(5) 0.0257(9) Uani 1 1 d . . H10F H 0.5158 0.4690 0.2293 0.039 Uiso 1 1 calc R U H10G H 0.5846 0.4772 0.3854 0.039 Uiso 1 1 calc R U H10H H 0.4693 0.4620 0.4039 0.039 Uiso 1 1 calc R U C107 C 0.6782(3) 0.39256(6) 0.0951(5) 0.0239(9) Uani 1 1 d . . H10I H 0.6834 0.4017 -0.0088 0.036 Uiso 1 1 calc R U H10J H 0.6016 0.3925 0.1312 0.036 Uiso 1 1 calc R U H10K H 0.7040 0.3739 0.0841 0.036 Uiso 1 1 calc R U C108 C 0.7898(2) 0.45399(6) 0.3308(5) 0.0142(8) Uani 1 1 d . . C110 C 0.9117(3) 0.46520(6) 0.5561(4) 0.0217(9) Uani 1 1 d . . H11A H 0.9744 0.4532 0.5751 0.033 Uiso 1 1 calc R U H11B H 0.8844 0.4721 0.6588 0.033 Uiso 1 1 calc R U H11C H 0.9347 0.4803 0.4885 0.033 Uiso 1 1 calc R U C112 C 0.7196(3) 0.43396(8) 0.6882(5) 0.0326(10) Uani 1 1 d . . H11D H 0.6708 0.4489 0.6598 0.049 Uiso 1 1 calc R U H11E H 0.7665 0.4393 0.7783 0.049 Uiso 1 1 calc R U H11F H 0.6755 0.4182 0.7190 0.049 Uiso 1 1 calc R U B1 B 0.3833(3) 0.30053(8) 0.4198(5) 0.0227(10) Uani 1 1 d . . B101 B 0.7619(3) 0.47362(8) 0.0836(5) 0.0192(10) Uani 1 1 d . . 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 F1 0.0444(13) 0.0289(11) 0.0246(14) 0.0051(11) -0.0041(11) 0.0021(10) F2 0.0198(10) 0.0407(12) 0.0398(15) -0.0066(12) -0.0067(11) 0.0038(10) F101 0.0260(11) 0.0288(11) 0.0186(13) 0.0026(10) 0.0024(10) -0.0072(9) F102 0.0287(11) 0.0176(10) 0.0339(14) 0.0039(10) -0.0050(11) 0.0028(10) O4 0.0202(13) 0.0225(13) 0.0202(15) -0.0031(12) -0.0046(12) 0.0038(11) O5 0.0324(16) 0.0240(14) 0.044(2) 0.0095(14) 0.0005(14) 0.0045(13) O8 0.0205(13) 0.0201(13) 0.0216(16) 0.0006(12) -0.0009(12) 0.0035(11) O11 0.0222(13) 0.0315(14) 0.0207(15) 0.0055(13) -0.0011(13) 0.0054(12) O104 0.0176(13) 0.0180(12) 0.0172(15) 0.0038(11) -0.0008(12) -0.0014(10) O105 0.0255(15) 0.0272(14) 0.0400(19) 0.0061(14) 0.0084(13) -0.0060(12) O108 0.0183(12) 0.0150(12) 0.0191(15) 0.0020(12) -0.0023(12) -0.0030(10) O111 0.0333(14) 0.0175(13) 0.0169(16) 0.0035(11) 0.0015(12) -0.0034(11) N9 0.0202(16) 0.0202(16) 0.0188(19) 0.0010(15) -0.0010(14) 0.0036(14) N109 0.0187(16) 0.0122(15) 0.0162(19) 0.0035(13) -0.0030(14) -0.0017(13) C1 0.038(3) 0.032(2) 0.049(3) 0.007(2) -0.019(2) -0.008(2) C2 0.018(2) 0.027(2) 0.024(2) 0.0056(19) 0.0036(18) 0.0029(17) C3 0.0142(18) 0.024(2) 0.021(2) 0.0018(17) -0.0030(16) 0.0011(17) C4 0.0199(19) 0.0196(19) 0.018(2) -0.0002(17) 0.0001(17) 0.0016(18) C5 0.026(2) 0.022(2) 0.022(2) -0.0045(18) 0.0022(19) -0.0002(18) C6 0.029(2) 0.022(2) 0.038(3) 0.0009(19) 0.009(2) -0.0044(17) C7 0.023(2) 0.034(2) 0.026(2) 0.001(2) 0.0031(19) 0.0069(17) C8 0.0148(18) 0.0153(19) 0.019(2) 0.0031(18) 0.0011(17) -0.0012(16) C10 0.033(2) 0.022(2) 0.030(3) -0.0073(19) 0.001(2) 0.0022(17) C12 0.041(2) 0.037(2) 0.023(2) 0.010(2) 0.002(2) 0.009(2) C101 0.023(2) 0.029(2) 0.039(3) -0.003(2) 0.003(2) 0.0047(18) C102 0.025(2) 0.0136(18) 0.022(2) -0.0034(17) 0.0017(18) -0.0014(16) C103 0.0205(18) 0.0116(18) 0.017(2) 0.0019(16) -0.0006(17) -0.0006(16) C104 0.0168(18) 0.0167(19) 0.013(2) 0.0011(17) -0.0027(16) -0.0027(16) C105 0.017(2) 0.020(2) 0.021(2) -0.0010(18) -0.0034(18) -0.0046(17) C106 0.020(2) 0.026(2) 0.031(2) -0.0040(19) 0.0004(19) 0.0034(16) C107 0.027(2) 0.0172(19) 0.028(2) -0.0033(19) -0.0043(19) -0.0008(16) C108 0.0128(18) 0.0099(17) 0.020(2) -0.0010(18) 0.0016(17) 0.0060(16) C110 0.0222(19) 0.0212(19) 0.022(2) -0.0024(18) -0.0067(18) -0.0032(16) C112 0.045(2) 0.032(2) 0.022(3) -0.0008(19) 0.012(2) -0.011(2) B1 0.023(2) 0.028(2) 0.017(3) -0.001(2) -0.004(2) 0.001(2) B101 0.018(2) 0.018(2) 0.021(3) 0.001(2) -0.004(2) -0.0012(19) 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 C4 O4 B1 112.5(3) C8 O8 B1 108.1(3) N9 O11 C12 110.5(2) C104 O104 B101 113.1(3) C108 O108 B101 108.4(3) N109 O111 C112 110.9(2) C8 N9 O11 116.2(3) C8 N9 C10 126.3(3) O11 N9 C10 116.5(3) C108 N109 O111 115.9(3) C108 N109 C110 126.7(3) O111 N109 C110 116.6(3) C2 C1 H1A 120.0 C2 C1 H1B 120.0 H1A C1 H1B 120.0 C1 C2 C3 124.7(4) C1 C2 H2 117.6 C3 C2 H2 117.6 C2 C3 C7 110.3(3) C2 C3 C4 110.1(3) C7 C3 C4 111.3(3) C2 C3 H3 108.4 C7 C3 H3 108.4 C4 C3 H3 108.4 O4 C4 C8 102.4(3) O4 C4 C3 111.1(3) C8 C4 C3 111.5(3) O4 C4 C5 108.6(3) C8 C4 C5 111.0(3) C3 C4 C5 111.8(3) O5 C5 C6 123.0(3) O5 C5 C4 121.0(3) C6 C5 C4 116.0(3) 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 C3 C7 H7A 109.5 C3 C7 H7B 109.5 H7A C7 H7B 109.5 C3 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 O8 C8 N9 121.2(3) O8 C8 C4 113.5(3) N9 C8 C4 125.3(3) N9 C10 H10A 109.5 N9 C10 H10B 109.5 H10A C10 H10B 109.5 N9 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 O11 C12 H12A 109.5 O11 C12 H12B 109.5 H12A C12 H12B 109.5 O11 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C102 C101 H10D 120.0 C102 C101 H10E 120.0 H10D C101 H10E 120.0 C101 C102 C103 124.6(4) C101 C102 H102 117.7 C103 C102 H102 117.7 C102 C103 C107 110.6(3) C102 C103 C104 110.7(2) C107 C103 C104 110.2(3) C102 C103 H103 108.4 C107 C103 H103 108.4 C104 C103 H103 108.4 O104 C104 C108 102.2(3) O104 C104 C103 111.1(3) C108 C104 C103 111.6(2) O104 C104 C105 109.0(3) C108 C104 C105 110.0(3) C103 C104 C105 112.4(3) O105 C105 C106 123.2(3) O105 C105 C104 120.6(3) C106 C105 C104 116.2(3) C105 C106 H10F 109.5 C105 C106 H10G 109.5 H10F C106 H10G 109.5 C105 C106 H10H 109.5 H10F C106 H10H 109.5 H10G C106 H10H 109.5 C103 C107 H10I 109.5 C103 C107 H10J 109.5 H10I C107 H10J 109.5 C103 C107 H10K 109.5 H10I C107 H10K 109.5 H10J C107 H10K 109.5 O108 C108 N109 121.1(3) O108 C108 C104 113.0(3) N109 C108 C104 125.9(3) N109 C110 H11A 109.5 N109 C110 H11B 109.5 H11A C110 H11B 109.5 N109 C110 H11C 109.5 H11A C110 H11C 109.5 H11B C110 H11C 109.5 O111 C112 H11D 109.5 O111 C112 H11E 109.5 H11D C112 H11E 109.5 O111 C112 H11F 109.5 H11D C112 H11F 109.5 H11E C112 H11F 109.5 F2 B1 F1 110.1(3) F2 B1 O4 113.4(3) F1 B1 O4 113.4(3) F2 B1 O8 108.5(3) F1 B1 O8 107.7(3) O4 B1 O8 103.2(3) F101 B101 F102 110.2(3) F101 B101 O104 113.9(3) F102 B101 O104 113.6(3) F101 B101 O108 107.6(3) F102 B101 O108 107.8(3) O104 B101 O108 103.2(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance F1 B1 1.384(5) F2 B1 1.372(4) F101 B101 1.373(5) F102 B101 1.378(4) O4 C4 1.413(4) O4 B1 1.437(4) O5 C5 1.207(4) O8 C8 1.278(4) O8 B1 1.548(5) O11 N9 1.393(3) O11 C12 1.447(4) O104 C104 1.413(4) O104 B101 1.433(4) O105 C105 1.204(4) O108 C108 1.283(4) O108 B101 1.552(5) O111 N109 1.389(3) O111 C112 1.441(4) N9 C8 1.296(4) N9 C10 1.454(4) N109 C108 1.297(4) N109 C110 1.451(4) C1 C2 1.318(5) C1 H1A 0.9500 C1 H1B 0.9500 C2 C3 1.501(5) C2 H2 0.9500 C3 C7 1.521(5) C3 C4 1.554(5) C3 H3 1.0000 C4 C8 1.515(5) C4 C5 1.555(5) C5 C6 1.498(5) C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C101 C102 1.319(5) C101 H10D 0.9500 C101 H10E 0.9500 C102 C103 1.502(4) C102 H102 0.9500 C103 C107 1.523(4) C103 C104 1.548(4) C103 H103 1.0000 C104 C108 1.532(4) C104 C105 1.558(4) C105 C106 1.496(4) C106 H10F 0.9800 C106 H10G 0.9800 C106 H10H 0.9800 C107 H10I 0.9800 C107 H10J 0.9800 C107 H10K 0.9800 C110 H11A 0.9800 C110 H11B 0.9800 C110 H11C 0.9800 C112 H11D 0.9800 C112 H11E 0.9800 C112 H11F 0.9800 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 C12 O11 N9 C8 113.3(3) C12 O11 N9 C10 -77.2(3) C112 O111 N109 C108 -115.1(3) C112 O111 N109 C110 74.4(3) C1 C2 C3 C7 119.1(4) C1 C2 C3 C4 -117.6(4) B1 O4 C4 C8 -2.1(3) B1 O4 C4 C3 117.1(3) B1 O4 C4 C5 -119.5(3) C2 C3 C4 O4 -72.9(4) C7 C3 C4 O4 49.7(4) C2 C3 C4 C8 40.7(4) C7 C3 C4 C8 163.3(3) C2 C3 C4 C5 165.6(3) C7 C3 C4 C5 -71.8(4) O4 C4 C5 O5 -134.2(3) C8 C4 C5 O5 114.0(4) C3 C4 C5 O5 -11.2(5) O4 C4 C5 C6 46.1(4) C8 C4 C5 C6 -65.7(4) C3 C4 C5 C6 169.0(3) B1 O8 C8 N9 175.7(3) B1 O8 C8 C4 -5.9(4) O11 N9 C8 O8 176.8(3) C10 N9 C8 O8 8.4(5) O11 N9 C8 C4 -1.4(5) C10 N9 C8 C4 -169.8(3) O4 C4 C8 O8 5.2(4) C3 C4 C8 O8 -113.7(3) C5 C4 C8 O8 120.9(3) O4 C4 C8 N9 -176.5(3) C3 C4 C8 N9 64.6(4) C5 C4 C8 N9 -60.7(4) C101 C102 C103 C107 -126.2(4) C101 C102 C103 C104 111.3(4) B101 O104 C104 C108 0.6(3) B101 O104 C104 C103 -118.6(3) B101 O104 C104 C105 117.0(3) C102 C103 C104 O104 70.4(3) C107 C103 C104 O104 -52.3(3) C102 C103 C104 C108 -42.9(4) C107 C103 C104 C108 -165.7(3) C102 C103 C104 C105 -167.1(3) C107 C103 C104 C105 70.2(4) O104 C104 C105 O105 133.7(3) C108 C104 C105 O105 -115.0(4) C103 C104 C105 O105 10.0(5) O104 C104 C105 C106 -46.0(4) C108 C104 C105 C106 65.3(4) C103 C104 C105 C106 -169.7(3) B101 O108 C108 N109 -176.0(3) B101 O108 C108 C104 4.8(3) O111 N109 C108 O108 -174.7(3) C110 N109 C108 O108 -5.2(5) O111 N109 C108 C104 4.5(4) C110 N109 C108 C104 173.9(3) O104 C104 C108 O108 -3.5(3) C103 C104 C108 O108 115.3(3) C105 C104 C108 O108 -119.2(3) O104 C104 C108 N109 177.3(3) C103 C104 C108 N109 -63.9(4) C105 C104 C108 N109 61.6(4) C4 O4 B1 F2 116.3(3) C4 O4 B1 F1 -117.2(3) C4 O4 B1 O8 -0.9(3) C8 O8 B1 F2 -116.4(3) C8 O8 B1 F1 124.4(3) C8 O8 B1 O4 4.2(3) C104 O104 B101 F101 118.2(3) C104 O104 B101 F102 -114.5(3) C104 O104 B101 O108 1.9(3) C108 O108 B101 F101 -124.8(3) C108 O108 B101 F102 116.4(3) C108 O108 B101 O104 -4.1(3)