#------------------------------------------------------------------------------ #$Date: 2015-07-09 01:06:54 +0300 (Thu, 09 Jul 2015) $ #$Revision: 141402 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/52/03/1520309.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_1520309 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_absolute_configuration unk _chemical_formula_sum 'C12 H18 B F2 N O3' _chemical_formula_weight 273.08 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _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 92.405(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.7772(13) _cell_length_b 11.1085(10) _cell_length_c 16.6848(13) _cell_measurement_reflns_used 9914 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.0228 _cell_measurement_theta_min 2.2934 _cell_volume 2736.4(4) _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_collection 'BRUKER APEX2 2014.1-1' _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 'SHELXS-97 (Sheldrick, 2008) XT V2014/1 (Bruker AXS Inc., 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.995 _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 0.1228 _diffrn_reflns_av_unetI/netI 0.0751 _diffrn_reflns_laue_measured_fraction_full 0.999 _diffrn_reflns_laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5401 _diffrn_reflns_point_group_measured_fraction_full 0.528 _diffrn_reflns_point_group_measured_fraction_max 0.526 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.362 _diffrn_reflns_theta_min 2.203 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'TWINABS (Bruker AXS Inc.)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1152 _exptl_crystal_size_max 0.570 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.569 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.109 _refine_ls_abs_structure_details ; No quotients, so Flack parameter determined by classical intensity fit ; _refine_ls_abs_structure_Flack 0.7(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 694 _refine_ls_number_reflns 5401 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.123 _refine_ls_R_factor_all 0.0954 _refine_ls_R_factor_gt 0.0794 _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^)+(0.1428P)^2^+0.1839P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1921 _refine_ls_wR_factor_ref 0.2043 _reflns_Friedel_coverage 0.000 _reflns_friedel_fraction_full 0.000 _reflns_friedel_fraction_max 0.000 _reflns_number_gt 4632 _reflns_number_total 5401 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol5b01427_si_002.cif _cod_data_source_block twin5 _cod_depositor_comments 'Adding full bibliography for 1520305--1520319.cif.' _cod_database_code 1520309 _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 0.940 _shelx_estimated_absorpt_t_max 0.987 _shelx_res_file ; twin5.res created by SHELXL-2014/7 TITL JR2078_0m_a.res in P2(1) REM Old TITL JR2078_0m in P2(1) REM SHELXT solution in P2(1) REM R1 0.248, Rweak 0.132, Alpha 0.020, Orientation as input REM Flack x = 0.027 ( 0.328 ) from Parsons' quotients REM Formula found by SHELXT: C47 B2 N4 O11 F12 CELL 0.71073 14.7772 11.1085 16.6848 90.0000 92.4053 90.0000 ZERR 8.000 0.0013 0.0010 0.0013 0.0000 0.0035 0.0000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H B N O F UNIT 96 144 8 8 24 16 TEMP -173.150 SIZE 0.12 0.16 0.57 L.S. 10 BOND $H LIST 4 conf FMAP 2 PLAN 10 acta isor .003 c308 isor .007 c108 REM ##### WGHT 0.142800 0.183900 BASF 0.48468 FVAR 0.36286 F1 6 -0.118639 0.068147 0.190271 11.00000 0.04733 0.02983 = 0.05588 0.01670 -0.01071 -0.02023 F2 6 -0.170944 0.244019 0.239315 11.00000 0.02704 0.07589 = 0.02493 0.01335 -0.00075 -0.00285 O4 5 -0.081186 0.249585 0.126738 11.00000 0.01921 0.02805 = 0.02387 0.00966 -0.00685 -0.00654 O5 5 0.068568 0.491500 0.107385 11.00000 0.02451 0.01879 = 0.03147 0.00311 0.00638 -0.00201 O8 5 -0.014587 0.204329 0.251238 11.00000 0.02146 0.03292 = 0.02730 0.01237 0.00375 -0.00726 N9 4 0.123484 0.280677 0.244228 11.00000 0.01608 0.01526 = 0.02776 0.00757 0.00392 0.00359 C1 1 0.157377 0.063961 0.075765 11.00000 0.04579 0.03045 = 0.02843 0.00273 0.00695 0.00306 AFIX 93 H1A 2 0.209665 0.112497 0.070166 11.00000 -1.20000 H1B 2 0.163537 -0.020336 0.083892 11.00000 -1.20000 AFIX 0 C2 1 0.079490 0.111615 0.072396 11.00000 0.02930 0.02367 = 0.02340 -0.00679 0.00236 -0.00036 AFIX 43 H2 2 0.028665 0.060468 0.078226 11.00000 -1.20000 AFIX 0 C3 1 0.061864 0.245132 0.059653 11.00000 0.02417 0.01934 = 0.02819 0.00024 0.00639 -0.00892 AFIX 13 H3 2 0.121435 0.287905 0.060308 11.00000 -1.20000 AFIX 0 C4 1 0.006287 0.295151 0.128438 11.00000 0.01906 0.02537 = 0.01941 0.00609 -0.00641 -0.00896 C5 1 0.004201 0.437046 0.125236 11.00000 0.01577 0.02356 = 0.01495 0.00670 -0.00044 -0.01296 C6 1 -0.081800 0.496341 0.146167 11.00000 0.02455 0.03801 = 0.02627 0.00347 -0.00228 -0.00136 AFIX 137 H6A 2 -0.069646 0.580121 0.161549 11.00000 -1.50000 H6B 2 -0.107924 0.453619 0.191093 11.00000 -1.50000 H6C 2 -0.124549 0.494386 0.099664 11.00000 -1.50000 AFIX 0 C7 1 0.012190 0.268981 -0.021178 11.00000 0.05041 0.03221 = 0.01994 -0.00718 0.00029 -0.00092 AFIX 137 H7A 2 -0.003982 0.354395 -0.025132 11.00000 -1.50000 H7B 2 -0.042950 0.219975 -0.025383 11.00000 -1.50000 H7C 2 0.051711 0.247837 -0.064750 11.00000 -1.50000 AFIX 0 C8 1 0.045598 0.260901 0.212834 11.00000 0.01480 0.01812 = 0.03346 -0.00066 0.00647 0.01273 C10 1 0.147711 0.239437 0.326942 11.00000 0.02827 0.04009 = 0.02224 0.01421 -0.00815 0.01078 AFIX 23 H10A 2 0.142457 0.150819 0.330985 11.00000 -1.20000 H10B 2 0.107617 0.276913 0.365942 11.00000 -1.20000 AFIX 0 C11 1 0.243626 0.278549 0.342382 11.00000 0.03151 0.02784 = 0.02709 -0.00250 -0.00133 0.00799 AFIX 23 H11A 2 0.246195 0.355640 0.372162 11.00000 -1.20000 H11B 2 0.278108 0.217034 0.373868 11.00000 -1.20000 AFIX 0 C12 1 0.280725 0.292946 0.261832 11.00000 0.02348 0.02979 = 0.04374 -0.00016 0.00351 0.00744 AFIX 23 H12A 2 0.300336 0.214323 0.240664 11.00000 -1.20000 H12B 2 0.333165 0.348486 0.263975 11.00000 -1.20000 AFIX 0 C13 1 0.203676 0.344505 0.209825 11.00000 0.01214 0.03778 = 0.03730 0.00448 0.01091 -0.00908 AFIX 23 H13A 2 0.199168 0.432923 0.215934 11.00000 -1.20000 H13B 2 0.210054 0.324447 0.152525 11.00000 -1.20000 AFIX 0 B1 3 -0.102302 0.191621 0.198637 11.00000 0.01776 0.04266 = 0.03026 0.01192 -0.00406 -0.01140 F101 6 -0.163188 0.722040 0.485773 11.00000 0.02422 0.04066 = 0.03126 0.00251 0.00827 -0.00054 F102 6 -0.091139 0.900494 0.481827 11.00000 0.04121 0.01528 = 0.04525 -0.00072 0.00546 0.01204 O104 5 -0.062990 0.753831 0.383609 11.00000 0.01807 0.01953 = 0.01763 0.00628 -0.00412 0.00450 O105 5 0.068252 0.531491 0.302315 11.00000 0.03063 0.02822 = 0.02745 -0.00528 0.00123 0.00380 O108 5 -0.004256 0.727894 0.514419 11.00000 0.01771 0.02290 = 0.01699 0.00280 -0.00073 0.00947 N109 4 0.132708 0.655700 0.495659 11.00000 0.02847 0.01483 = 0.01625 -0.00466 -0.00045 -0.00484 C101 1 0.175721 0.934430 0.410510 11.00000 0.04606 0.02137 = 0.05454 0.00541 0.00112 -0.00536 AFIX 93 H10C 2 0.227134 0.883017 0.411776 11.00000 -1.20000 H10D 2 0.178998 1.010619 0.436331 11.00000 -1.20000 AFIX 0 C102 1 0.100176 0.900209 0.373091 11.00000 0.03533 0.01968 = 0.03769 0.00833 0.01449 -0.00268 AFIX 43 H102 2 0.050361 0.954257 0.373235 11.00000 -1.20000 AFIX 0 C103 1 0.086126 0.782823 0.330170 11.00000 0.01616 0.01574 = 0.02541 -0.00212 0.01314 -0.00049 AFIX 13 H103 2 0.146044 0.741991 0.325924 11.00000 -1.20000 AFIX 0 C104 1 0.023703 0.701757 0.378358 11.00000 0.02382 0.02161 = 0.01913 0.00682 0.00094 -0.01114 C105 1 0.013695 0.574090 0.343956 11.00000 0.03429 0.01175 = 0.01193 0.00028 -0.00485 0.00471 C106 1 -0.068347 0.503894 0.367980 11.00000 0.03715 0.01940 = 0.02889 -0.00709 0.00715 -0.00176 AFIX 137 H10E 2 -0.059861 0.418470 0.355691 11.00000 -1.50000 H10F 2 -0.122244 0.534056 0.338190 11.00000 -1.50000 H10G 2 -0.076192 0.513591 0.425655 11.00000 -1.50000 AFIX 0 C107 1 0.045033 0.805591 0.244715 11.00000 0.03498 0.03760 = 0.02900 0.02419 0.00097 -0.01120 AFIX 137 H10H 2 0.042636 0.729670 0.214787 11.00000 -1.50000 H10I 2 0.082771 0.863490 0.216983 11.00000 -1.50000 H10J 2 -0.016342 0.838039 0.248238 11.00000 -1.50000 AFIX 0 C108 1 0.054842 0.694083 0.466569 11.00000 0.02004 0.01260 = 0.02088 -0.01080 0.00071 -0.00194 C110 1 0.209555 0.609661 0.448662 11.00000 0.03165 0.02331 = 0.01732 0.01034 0.01296 0.00246 AFIX 23 H11C 2 0.238641 0.675699 0.419327 11.00000 -1.20000 H11D 2 0.188729 0.547065 0.409885 11.00000 -1.20000 AFIX 0 C111 1 0.273558 0.557614 0.512493 11.00000 0.02407 0.01825 = 0.03136 -0.00094 -0.00026 0.01091 AFIX 23 H11E 2 0.337196 0.563308 0.496548 11.00000 -1.20000 H11F 2 0.258966 0.472309 0.523276 11.00000 -1.20000 AFIX 0 C112 1 0.257281 0.636908 0.586170 11.00000 0.02815 0.03453 = 0.02746 0.00571 -0.00233 -0.00086 AFIX 23 H11G 2 0.276251 0.594924 0.636449 11.00000 -1.20000 H11H 2 0.290699 0.713909 0.583164 11.00000 -1.20000 AFIX 0 C113 1 0.157300 0.657594 0.581708 11.00000 0.02214 0.01558 = 0.02884 -0.00022 -0.00422 0.00101 AFIX 23 H11I 2 0.125318 0.593174 0.610188 11.00000 -1.20000 H11J 2 0.142124 0.736247 0.605601 11.00000 -1.20000 AFIX 0 B100 3 -0.086667 0.778748 0.463406 11.00000 0.00726 0.03695 = 0.02906 0.00790 0.00115 0.00770 F201 6 0.686016 0.241372 0.745416 11.00000 0.01492 0.06747 = 0.03995 0.01722 -0.00425 0.00039 F202 6 0.637046 0.065305 0.692800 11.00000 0.04053 0.03983 = 0.06139 0.01520 0.01040 0.02102 O204 5 0.593689 0.245657 0.627607 11.00000 0.02038 0.02833 = 0.01957 0.00137 0.00281 0.00721 O205 5 0.446861 0.491357 0.602128 11.00000 0.02964 0.02474 = 0.02714 -0.00259 -0.00672 -0.00438 O208 5 0.530158 0.197013 0.748933 11.00000 0.02104 0.02343 = 0.03030 0.00292 0.00435 0.00561 N209 4 0.388036 0.264009 0.731811 11.00000 0.02864 0.00786 = 0.01973 -0.00501 -0.00818 0.00334 C201 1 0.355591 0.061693 0.556736 11.00000 0.04024 0.02726 = 0.03748 0.00065 -0.00071 0.00350 AFIX 93 H20A 2 0.302281 0.108403 0.547720 11.00000 -1.20000 H20B 2 0.351332 -0.023177 0.562486 11.00000 -1.20000 AFIX 0 C202 1 0.433764 0.113509 0.561170 11.00000 0.03263 0.01660 = 0.01630 -0.00407 -0.00113 0.00500 AFIX 43 H202 2 0.485619 0.064025 0.570236 11.00000 -1.20000 AFIX 0 C203 1 0.448400 0.245895 0.553042 11.00000 0.01305 0.01889 = 0.02553 -0.00180 -0.00055 0.00268 AFIX 13 H203 2 0.388189 0.287122 0.550874 11.00000 -1.20000 AFIX 0 C204 1 0.504521 0.292280 0.627249 11.00000 0.01754 0.03273 = 0.01787 0.00287 0.00353 -0.01106 C205 1 0.510004 0.431554 0.628150 11.00000 0.01791 0.02028 = 0.01941 -0.00856 0.00094 -0.00420 C206 1 0.595097 0.490639 0.661543 11.00000 0.02486 0.02272 = 0.02099 0.00266 0.00295 -0.00306 AFIX 137 H20C 2 0.580831 0.571516 0.680788 11.00000 -1.50000 H20D 2 0.639167 0.496428 0.619428 11.00000 -1.50000 H20E 2 0.620720 0.442458 0.706162 11.00000 -1.50000 AFIX 0 C207 1 0.496347 0.273097 0.475686 11.00000 0.03450 0.02119 = 0.02297 -0.00497 -0.00145 -0.00106 AFIX 137 H20F 2 0.491265 0.359207 0.463544 11.00000 -1.50000 H20G 2 0.468100 0.226507 0.431474 11.00000 -1.50000 H20H 2 0.560422 0.251018 0.482440 11.00000 -1.50000 AFIX 0 C208 1 0.469082 0.252344 0.705072 11.00000 0.01529 0.01403 = 0.02526 -0.00958 -0.00142 -0.00092 C210 1 0.309418 0.321603 0.690506 11.00000 0.02587 0.01812 = 0.03390 -0.00617 -0.00694 0.00266 AFIX 23 H21A 2 0.283184 0.268682 0.647813 11.00000 -1.20000 H21B 2 0.326774 0.399194 0.666330 11.00000 -1.20000 AFIX 0 C211 1 0.244141 0.340688 0.754601 11.00000 0.01571 0.04236 = 0.03404 -0.01368 -0.00641 0.00272 AFIX 23 H21C 2 0.180935 0.340643 0.732441 11.00000 -1.20000 H21D 2 0.256147 0.417449 0.783261 11.00000 -1.20000 AFIX 0 C212 1 0.262050 0.233276 0.809452 11.00000 0.02066 0.05513 = 0.03995 -0.00872 0.00179 -0.00641 AFIX 23 H21E 2 0.233303 0.159439 0.787007 11.00000 -1.20000 H21F 2 0.239451 0.248145 0.863591 11.00000 -1.20000 AFIX 0 C213 1 0.365715 0.223119 0.812000 11.00000 0.02479 0.03244 = 0.02474 0.00278 0.00015 -0.00157 AFIX 23 H21G 2 0.393696 0.275561 0.854132 11.00000 -1.20000 H21H 2 0.385604 0.139042 0.821544 11.00000 -1.20000 AFIX 0 B200 3 0.618022 0.184546 0.701985 11.00000 0.02735 0.02838 = 0.03489 0.00245 0.00023 0.00763 F301 6 0.591887 0.890044 -0.013379 11.00000 0.03031 0.02594 = 0.04148 -0.00950 0.00572 -0.00955 F302 6 0.662810 0.710745 -0.003250 11.00000 0.01458 0.04581 = 0.03072 0.00219 -0.00328 0.00071 O304 5 0.559707 0.742368 -0.112719 11.00000 0.01687 0.02237 = 0.02868 0.00279 -0.00223 -0.00277 O305 5 0.425419 0.522519 -0.203379 11.00000 0.02509 0.02662 = 0.03118 -0.00380 -0.00018 -0.00199 O308 5 0.504890 0.719863 0.016369 11.00000 0.01985 0.02276 = 0.02249 -0.00211 -0.00396 -0.00118 N309 4 0.365560 0.646376 -0.009398 11.00000 0.02415 0.01061 = 0.01519 0.00406 -0.00182 0.00069 C301 1 0.316688 0.924758 -0.101886 11.00000 0.03930 0.02715 = 0.05441 -0.00532 -0.00247 -0.00210 AFIX 93 H30A 2 0.263986 0.877337 -0.112225 11.00000 -1.20000 H30B 2 0.312707 0.998100 -0.072962 11.00000 -1.20000 AFIX 0 C302 1 0.393031 0.889850 -0.126918 11.00000 0.02370 0.01608 = 0.04310 0.00596 0.00494 -0.00066 AFIX 43 H302 2 0.444138 0.939751 -0.115380 11.00000 -1.20000 AFIX 0 C303 1 0.408240 0.774974 -0.173579 11.00000 0.02456 0.02197 = 0.03896 0.00429 0.00215 -0.00394 AFIX 13 H303 2 0.348859 0.732857 -0.182491 11.00000 -1.20000 AFIX 0 C304 1 0.473428 0.691964 -0.121789 11.00000 0.02026 0.01384 = 0.02496 0.00033 0.00647 -0.00628 C305 1 0.480083 0.562407 -0.155786 11.00000 0.00788 0.03544 = 0.01616 0.00435 0.00385 0.00019 C306 1 0.559348 0.489390 -0.122554 11.00000 0.03339 0.01955 = 0.03170 -0.00325 0.00970 0.00808 AFIX 137 H30C 2 0.552556 0.405512 -0.139987 11.00000 -1.50000 H30D 2 0.561146 0.492954 -0.063821 11.00000 -1.50000 H30E 2 0.615756 0.522344 -0.142300 11.00000 -1.50000 AFIX 0 C307 1 0.447375 0.798210 -0.252477 11.00000 0.03593 0.03992 = 0.04341 0.00907 -0.00028 0.00685 AFIX 137 H30F 2 0.456537 0.721601 -0.280112 11.00000 -1.50000 H30G 2 0.505637 0.839549 -0.244443 11.00000 -1.50000 H30H 2 0.405820 0.848840 -0.285029 11.00000 -1.50000 AFIX 0 C308 1 0.442609 0.682641 -0.034652 11.00000 0.01133 0.01049 = 0.01812 -0.00063 -0.00420 0.00339 C310 1 0.288108 0.598206 -0.058943 11.00000 0.01052 0.02569 = 0.03558 -0.00392 -0.00248 -0.00539 AFIX 23 H31A 2 0.307751 0.532774 -0.094556 11.00000 -1.20000 H31B 2 0.258752 0.662364 -0.091992 11.00000 -1.20000 AFIX 0 C311 1 0.225015 0.551163 0.002921 11.00000 0.01844 0.03422 = 0.02848 -0.00343 -0.00532 -0.00098 AFIX 23 H31C 2 0.239497 0.466640 0.017233 11.00000 -1.20000 H31D 2 0.161066 0.555980 -0.017013 11.00000 -1.20000 AFIX 0 C312 1 0.242712 0.635130 0.075024 11.00000 0.01660 0.04085 = 0.03838 -0.00311 0.00644 -0.01044 AFIX 23 H31E 2 0.212136 0.713714 0.066730 11.00000 -1.20000 H31F 2 0.222386 0.598335 0.125230 11.00000 -1.20000 AFIX 0 C313 1 0.345812 0.648600 0.076472 11.00000 0.02916 0.02415 = 0.02249 -0.00441 0.00512 -0.00299 AFIX 23 H31G 2 0.365236 0.725553 0.101696 11.00000 -1.20000 H31H 2 0.376023 0.581129 0.105667 11.00000 -1.20000 AFIX 0 B300 3 0.586109 0.768650 -0.030002 11.00000 0.02389 0.02088 = 0.01822 0.00126 0.00391 -0.00397 HKLF 5 REM JR2078_0m_a.res in P2(1) REM R1 = 0.0794 for 4632 Fo > 4sig(Fo) and 0.0954 for all 5401 data REM 694 parameters refined using 13 restraints END WGHT 0.1428 0.1839 REM Highest difference peak 0.569, deepest hole -0.377, 1-sigma level 0.109 Q1 1 0.4381 0.2497 0.7153 11.00000 0.05 0.57 Q2 1 0.4743 0.4958 0.5672 11.00000 0.05 0.55 Q3 1 0.4135 0.6440 -0.0178 11.00000 0.05 0.50 Q4 1 -0.1923 0.2305 0.2531 11.00000 0.05 0.48 Q5 1 0.0220 0.2257 0.2379 11.00000 0.05 0.48 Q6 1 -0.0007 0.7451 0.3916 11.00000 0.05 0.47 Q7 1 -0.1319 0.7695 0.4579 11.00000 0.05 0.46 Q8 1 -0.1636 0.2701 0.2314 11.00000 0.05 0.46 Q9 1 -0.1363 0.2341 0.2177 11.00000 0.05 0.45 Q10 1 -0.1970 0.6869 0.4963 11.00000 0.05 0.45 ; 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4.65923 1 -5 0 17 4.10182 4.02154 -2 4 0 17 4.10182 4.02154 1 -6 0 17 -7.1852 4.22074 -2 5 0 17 -7.1852 4.22074 1 -7 0 17 32.2366 5.56281 -2 6 0 17 32.2366 5.56281 1 -8 0 17 16.2951 6.58346 -2 7 0 17 16.2951 6.58346 1 -9 0 17 3.71097 6.64331 -2 8 0 17 3.71097 6.64331 1 -10 1 17 1.54386 3.10985 1 8 1 17 18.9066 3.03202 -2 -9 1 17 18.9066 3.03202 1 7 1 17 33.5257 3.53787 -2 -8 1 17 33.5257 3.53787 1 6 1 17 17.7335 2.75892 -2 -7 1 17 17.7335 2.75892 1 5 1 17 18.6279 2.28274 -2 -6 1 17 18.6279 2.28274 1 4 1 17 11.7728 1.99402 -2 -5 1 17 11.7728 1.99402 1 3 1 17 23.0376 2.14551 -2 -4 1 17 23.0376 2.14551 1 2 1 17 17.0968 1.82715 -2 -3 1 17 17.0968 1.82715 1 1 1 17 17.4901 1.75167 -2 -2 1 17 17.4901 1.75167 1 0 1 17 60.4893 3.02974 -2 -1 1 17 60.4893 3.02974 1 -1 1 17 45.0695 2.52831 -2 0 1 17 45.0695 2.52831 1 -2 1 17 18.9985 2.71441 -2 1 1 17 18.9985 2.71441 1 -3 1 17 13.5216 3.34429 -2 2 1 17 13.5216 3.34429 1 -4 1 17 21.7145 3.21578 -2 3 1 17 21.7145 3.21578 1 -5 1 17 14.0383 3.23350 -2 4 1 17 14.0383 3.23350 1 -6 1 17 17.2053 3.42945 -2 5 1 17 17.2053 3.42945 1 -7 1 17 17.3649 4.10171 -2 6 1 17 17.3649 4.10171 1 -8 1 17 21.2959 3.90404 -2 7 1 17 21.2959 3.90404 1 -9 1 17 11.2547 4.30737 -2 8 1 17 11.2547 4.30737 1 8 2 17 15.4411 2.93935 -2 -9 2 17 15.4411 2.93935 1 7 2 17 16.0074 3.00568 -2 -8 2 17 16.0074 3.00568 1 6 2 17 21.6752 2.68275 -2 -7 2 17 21.6752 2.68275 1 5 2 17 1.34420 2.12268 -2 -6 2 17 1.34420 2.12268 1 4 2 17 9.07036 2.01183 -2 -5 2 17 9.07036 2.01183 1 3 2 17 5.63901 1.79303 -2 -4 2 17 5.63901 1.79303 1 2 2 17 1.19360 2.02113 -2 -3 2 17 1.19360 2.02113 1 1 2 17 11.9894 2.17335 -2 -2 2 17 11.9894 2.17335 1 0 2 17 11.4860 2.03454 -2 -1 2 17 11.4860 2.03454 1 -1 2 17 10.4067 1.99023 -2 0 2 17 10.4067 1.99023 1 -2 2 17 1.31172 1.87655 -2 1 2 17 1.31172 1.87655 1 -3 2 17 4.72821 2.73516 -2 2 2 17 4.72821 2.73516 1 -4 2 17 11.1873 3.58211 -2 3 2 17 11.1873 3.58211 1 -5 2 17 7.64092 3.63045 -2 4 2 17 7.64092 3.63045 1 -6 2 17 16.5410 4.26926 -2 5 2 17 16.5410 4.26926 1 -7 2 17 27.4079 4.12950 -2 6 2 17 27.4079 4.12950 1 -8 2 17 16.9043 4.23036 -2 7 2 17 16.9043 4.23036 1 -9 2 17 18.8169 4.33526 -2 8 2 17 18.8169 4.33526 1 -9 3 17 3.49091 1.38854 1 7 3 17 15.3341 2.75695 -2 -8 3 17 15.3341 2.75695 1 6 3 17 16.7310 2.42346 -2 -7 3 17 16.7310 2.42346 1 5 3 17 6.01471 2.42379 -2 -6 3 17 6.01471 2.42379 1 4 3 17 21.8154 2.18276 -2 -5 3 17 21.8154 2.18276 1 3 3 17 4.04427 2.07758 -2 -4 3 17 4.04427 2.07758 1 2 3 17 3.82488 2.10035 -2 -3 3 17 3.82488 2.10035 1 1 3 17 30.4126 2.22895 -2 -2 3 17 30.4126 2.22895 1 0 3 17 13.1428 2.70415 -2 -1 3 17 13.1428 2.70415 1 -1 3 17 6.71578 2.60352 -2 0 3 17 6.71578 2.60352 1 -2 3 17 26.0129 3.08249 -2 1 3 17 26.0129 3.08249 1 -3 3 17 6.94443 2.41962 -2 2 3 17 6.94443 2.41962 1 -4 3 17 11.5359 2.19817 -2 3 3 17 11.5359 2.19817 1 -5 3 17 21.9365 2.59706 -2 4 3 17 21.9365 2.59706 1 -6 3 17 12.1344 4.12975 -2 5 3 17 12.1344 4.12975 1 -7 3 17 14.4103 4.25522 -2 6 3 17 14.4103 4.25522 1 -8 3 17 10.1569 4.57337 -2 7 3 17 10.1569 4.57337 1 7 4 17 18.8595 3.46014 -2 -8 4 17 18.8595 3.46014 1 6 4 17 11.0877 3.84881 -2 -7 4 17 11.0877 3.84881 1 5 4 17 -0.4654 3.12750 -2 -6 4 17 -0.4654 3.12750 1 4 4 17 15.7454 3.03691 -2 -5 4 17 15.7454 3.03691 1 3 4 17 10.9323 2.48499 -2 -4 4 17 10.9323 2.48499 1 2 4 17 22.2228 2.58912 -2 -3 4 17 22.2228 2.58912 1 1 4 17 18.8587 2.41594 -2 -2 4 17 18.8587 2.41594 1 0 4 17 7.51727 2.87193 -2 -1 4 17 7.51727 2.87193 1 -1 4 17 12.3148 3.18726 -2 0 4 17 12.3148 3.18726 1 -2 4 17 14.4724 3.88542 -2 1 4 17 14.4724 3.88542 1 -3 4 17 25.5347 3.62536 -2 2 4 17 25.5347 3.62536 1 -4 4 17 17.7407 3.14471 -2 3 4 17 17.7407 3.14471 1 -5 4 17 14.3331 3.25149 -2 4 4 17 14.3331 3.25149 1 -6 4 17 5.03829 3.18305 -2 5 4 17 5.03829 3.18305 1 -7 4 17 12.5069 3.07696 -2 6 4 17 12.5069 3.07696 1 -8 4 17 4.71625 3.05336 -2 7 4 17 4.71625 3.05336 1 6 5 17 6.01714 4.58484 -2 -7 5 17 6.01714 4.58484 1 5 5 17 10.6330 3.55883 -2 -6 5 17 10.6330 3.55883 1 4 5 17 9.08219 3.26970 -2 -5 5 17 9.08219 3.26970 1 3 5 17 16.5768 3.17307 -2 -4 5 17 16.5768 3.17307 1 2 5 17 29.8869 3.39327 -2 -3 5 17 29.8869 3.39327 1 1 5 17 26.2272 4.11350 -2 -2 5 17 26.2272 4.11350 1 0 5 17 38.3467 4.37877 -2 -1 5 17 38.3467 4.37877 1 -1 5 17 41.3656 4.69176 -2 0 5 17 41.3656 4.69176 1 -2 5 17 33.3030 4.71227 -2 1 5 17 33.3030 4.71227 1 -3 5 17 36.6108 4.07960 -2 2 5 17 36.6108 4.07960 1 -4 5 17 23.4210 3.96655 -2 3 5 17 23.4210 3.96655 1 -5 5 17 0.54088 3.87764 -2 4 5 17 0.54088 3.87764 1 -6 5 17 22.1590 3.78846 -2 5 5 17 22.1590 3.78846 1 -7 5 17 9.28963 4.47906 -2 6 5 17 9.28963 4.47906 1 4 6 17 0.94243 3.83086 -2 -5 6 17 0.94243 3.83086 1 3 6 17 7.85385 3.42632 -2 -4 6 17 7.85385 3.42632 1 2 6 17 3.23558 3.72710 -2 -3 6 17 3.23558 3.72710 1 1 6 17 9.15956 3.35260 -2 -2 6 17 9.15956 3.35260 1 0 6 17 7.05723 2.81177 -2 -1 6 17 7.05723 2.81177 1 -1 6 17 4.38777 4.44900 -2 0 6 17 4.38777 4.44900 1 -2 6 17 9.18228 4.36074 -2 1 6 17 9.18228 4.36074 1 -3 6 17 4.70508 4.30696 -2 2 6 17 4.70508 4.30696 1 -4 6 17 9.60973 4.40378 -2 3 6 17 9.60973 4.40378 1 -5 6 17 -0.9010 4.92969 -2 4 6 17 -0.9010 4.92969 1 1 7 17 8.02567 6.61625 -2 -2 7 17 8.02567 6.61625 1 0 7 17 2.36607 3.38043 -2 -1 7 17 2.36607 3.38043 1 -1 7 17 0.00836 2.80522 -2 0 7 17 0.00836 2.80522 1 7 0 18 9.22912 5.23785 -2 -8 0 18 9.22912 5.23785 1 6 0 18 11.5412 5.75467 -2 -7 0 18 11.5412 5.75467 1 5 0 18 4.80629 4.24020 -2 -6 0 18 4.80629 4.24020 1 4 0 18 8.27284 3.32696 -2 -5 0 18 8.27284 3.32696 1 3 0 18 2.55874 3.15051 -2 -4 0 18 2.55874 3.15051 1 2 0 18 1.45856 2.89499 -2 -3 0 18 1.45856 2.89499 1 1 0 18 0.46178 2.64903 -2 -2 0 18 0.46178 2.64903 1 0 0 18 8.98942 4.09861 -2 -1 0 18 8.98942 4.09861 1 -1 0 18 3.79760 4.19523 -2 0 0 18 3.79760 4.19523 1 -2 0 18 -3.0138 4.38812 -2 1 0 18 -3.0138 4.38812 1 -3 0 18 2.21664 4.63033 -2 2 0 18 2.21664 4.63033 1 -4 0 18 -3.4916 5.46665 -2 3 0 18 -3.4916 5.46665 1 -5 0 18 15.1646 5.84639 -2 4 0 18 15.1646 5.84639 1 -6 0 18 -12.850 6.10277 -2 5 0 18 -12.850 6.10277 1 -7 0 18 22.7867 7.07220 -2 6 0 18 22.7867 7.07220 1 -8 0 18 37.9184 7.31760 -2 7 0 18 37.9184 7.31760 1 7 1 18 27.5401 3.81923 -2 -8 1 18 27.5401 3.81923 1 6 1 18 12.8622 4.07675 -2 -7 1 18 12.8622 4.07675 1 5 1 18 6.09095 2.48885 -2 -6 1 18 6.09095 2.48885 1 4 1 18 26.6342 2.54044 -2 -5 1 18 26.6342 2.54044 1 3 1 18 24.4649 2.46379 -2 -4 1 18 24.4649 2.46379 1 2 1 18 29.3424 2.24142 -2 -3 1 18 29.3424 2.24142 1 1 1 18 8.72840 2.29716 -2 -2 1 18 8.72840 2.29716 1 0 1 18 8.88534 2.19342 -2 -1 1 18 8.88534 2.19342 1 -1 1 18 6.44614 3.22228 -2 0 1 18 6.44614 3.22228 1 -2 1 18 10.3170 3.78238 -2 1 1 18 10.3170 3.78238 1 -3 1 18 30.7303 3.84459 -2 2 1 18 30.7303 3.84459 1 -4 1 18 32.8816 4.00833 -2 3 1 18 32.8816 4.00833 1 -5 1 18 28.5641 4.09657 -2 4 1 18 28.5641 4.09657 1 -6 1 18 11.7213 4.64691 -2 5 1 18 11.7213 4.64691 1 -7 1 18 12.0070 4.37265 -2 6 1 18 12.0070 4.37265 1 -8 1 18 27.3871 4.79219 -2 7 1 18 27.3871 4.79219 1 -8 2 18 6.96529 2.00968 1 6 2 18 9.50631 3.25199 -2 -7 2 18 9.50631 3.25199 1 5 2 18 13.2219 2.75854 -2 -6 2 18 13.2219 2.75854 1 4 2 18 22.1447 2.53107 -2 -5 2 18 22.1447 2.53107 1 3 2 18 -1.9639 2.18725 -2 -4 2 18 -1.9639 2.18725 1 2 2 18 4.29790 2.42709 -2 -3 2 18 4.29790 2.42709 1 1 2 18 16.7434 2.69027 -2 -2 2 18 16.7434 2.69027 1 0 2 18 5.48974 2.45616 -2 -1 2 18 5.48974 2.45616 1 -1 2 18 10.0980 2.52966 -2 0 2 18 10.0980 2.52966 1 -2 2 18 49.7095 9.04663 -2 1 2 18 49.7095 9.04663 1 -3 2 18 8.20513 4.11765 -2 2 2 18 8.20513 4.11765 1 -4 2 18 8.09640 4.03594 -2 3 2 18 8.09640 4.03594 1 -5 2 18 29.6144 4.14903 -2 4 2 18 29.6144 4.14903 1 -6 2 18 27.8826 6.33670 -2 5 2 18 27.8826 6.33670 1 -7 2 18 25.7120 4.76926 -2 6 2 18 25.7120 4.76926 1 6 3 18 15.5306 4.53538 -2 -7 3 18 15.5306 4.53538 1 5 3 18 21.1935 2.95865 -2 -6 3 18 21.1935 2.95865 1 4 3 18 10.9723 2.80489 -2 -5 3 18 10.9723 2.80489 1 3 3 18 -2.9308 2.47972 -2 -4 3 18 -2.9308 2.47972 1 2 3 18 0.94225 2.52004 -2 -3 3 18 0.94225 2.52004 1 1 3 18 27.1124 2.99518 -2 -2 3 18 27.1124 2.99518 1 0 3 18 6.66953 2.63148 -2 -1 3 18 6.66953 2.63148 1 -1 3 18 9.64426 2.82573 -2 0 3 18 9.64426 2.82573 1 -2 3 18 28.6357 3.13299 -2 1 3 18 28.6357 3.13299 1 -3 3 18 9.03331 2.74561 -2 2 3 18 9.03331 2.74561 1 -4 3 18 0.79533 4.40547 -2 3 3 18 0.79533 4.40547 1 -5 3 18 9.10187 5.37387 -2 4 3 18 9.10187 5.37387 1 -6 3 18 18.4713 4.78387 -2 5 3 18 18.4713 4.78387 1 -7 3 18 20.7212 5.25283 -2 6 3 18 20.7212 5.25283 1 5 4 18 9.20964 4.15057 -2 -6 4 18 9.20964 4.15057 1 4 4 18 15.2009 3.57151 -2 -5 4 18 15.2009 3.57151 1 3 4 18 -1.2229 3.38480 -2 -4 4 18 -1.2229 3.38480 1 2 4 18 -1.2961 3.94401 -2 -3 4 18 -1.2961 3.94401 1 1 4 18 3.69815 2.72881 -2 -2 4 18 3.69815 2.72881 1 0 4 18 6.55836 3.90580 -2 -1 4 18 6.55836 3.90580 1 -1 4 18 -0.0514 3.68622 -2 0 4 18 -0.0514 3.68622 1 -2 4 18 7.34048 3.96409 -2 1 4 18 7.34048 3.96409 1 -3 4 18 -4.6505 3.76371 -2 2 4 18 -4.6505 3.76371 1 -4 4 18 2.95244 3.67311 -2 3 4 18 2.95244 3.67311 1 -5 4 18 4.06074 3.26685 -2 4 4 18 4.06074 3.26685 1 -6 4 18 5.24667 3.29407 -2 5 4 18 5.24667 3.29407 1 3 5 18 13.7870 3.31025 -2 -4 5 18 13.7870 3.31025 1 2 5 18 7.62408 3.68893 -2 -3 5 18 7.62408 3.68893 1 1 5 18 11.1872 2.81248 -2 -2 5 18 11.1872 2.81248 1 0 5 18 5.25891 3.95845 -2 -1 5 18 5.25891 3.95845 1 -1 5 18 1.70868 4.28483 -2 0 5 18 1.70868 4.28483 1 -2 5 18 19.3733 4.53201 -2 1 5 18 19.3733 4.53201 1 -3 5 18 16.6451 4.48309 -2 2 5 18 16.6451 4.48309 1 -4 5 18 13.0730 4.44702 -2 3 5 18 13.0730 4.44702 1 5 0 19 27.0758 10.4966 -2 -6 0 19 27.0758 10.4966 1 4 0 19 16.7544 4.45387 -2 -5 0 19 16.7544 4.45387 1 3 0 19 5.22639 3.88627 -2 -4 0 19 5.22639 3.88627 1 2 0 19 2.49900 3.49497 -2 -3 0 19 2.49900 3.49497 1 1 0 19 14.2305 3.40083 -2 -2 0 19 14.2305 3.40083 1 0 0 19 -3.9727 5.67463 -2 -1 0 19 -3.9727 5.67463 1 -1 0 19 4.44705 7.37490 -2 0 0 19 4.44705 7.37490 1 -2 0 19 -1.4671 6.36676 -2 1 0 19 -1.4671 6.36676 1 -3 0 19 22.0902 10.0656 -2 2 0 19 22.0902 10.0656 1 -4 0 19 1.10159 6.48963 -2 3 0 19 1.10159 6.48963 1 -5 0 19 15.7270 7.89952 -2 4 0 19 15.7270 7.89952 1 -6 1 19 6.20298 1.44646 1 4 1 19 14.3546 3.03158 -2 -5 1 19 14.3546 3.03158 1 3 1 19 3.37885 2.78887 -2 -4 1 19 3.37885 2.78887 1 2 1 19 14.3654 2.73087 -2 -3 1 19 14.3654 2.73087 1 1 1 19 3.39410 2.91463 -2 -2 1 19 3.39410 2.91463 1 0 1 19 6.94601 4.14872 -2 -1 1 19 6.94601 4.14872 1 -1 1 19 9.22695 4.68629 -2 0 1 19 9.22695 4.68629 1 -2 1 19 5.50688 5.03285 -2 1 1 19 5.50688 5.03285 1 -3 1 19 16.7215 4.75123 -2 2 1 19 16.7215 4.75123 1 -4 1 19 8.65101 4.92492 -2 3 1 19 8.65101 4.92492 1 -5 1 19 8.95299 5.12576 -2 4 1 19 8.95299 5.12576 1 4 2 19 8.09183 3.35535 -2 -5 2 19 8.09183 3.35535 1 3 2 19 -1.3825 3.52511 -2 -4 2 19 -1.3825 3.52511 1 2 2 19 0.14982 3.31442 -2 -3 2 19 0.14982 3.31442 1 1 2 19 8.24874 11.7087 -2 -3 2 19 8.24874 11.7087 1 1 2 19 11.1002 4.35769 -2 -2 2 19 11.1002 4.35769 1 0 2 19 19.5575 11.1359 -2 -2 2 19 19.5575 11.1359 1 0 2 19 10.4505 3.32420 -2 -1 2 19 10.4505 3.32420 1 -1 2 19 5.57568 3.27092 -2 0 2 19 5.57568 3.27092 1 -2 2 19 3.71507 5.82414 -2 1 2 19 3.71507 5.82414 1 -3 2 19 10.4703 7.42864 -2 2 2 19 10.4703 7.42864 1 -4 2 19 14.6189 5.11040 -2 3 2 19 14.6189 5.11040 1 -5 2 19 6.38449 6.22979 -2 4 2 19 6.38449 6.22979 1 3 3 19 -0.1025 3.18816 -2 -4 3 19 -0.1025 3.18816 1 2 3 19 -3.7870 3.90880 -2 -3 3 19 -3.7870 3.90880 1 1 3 19 2.11944 3.55725 -2 -2 3 19 2.11944 3.55725 1 0 3 19 3.91549 3.51464 -2 -1 3 19 3.91549 3.51464 1 -1 3 19 13.1903 3.69283 -2 0 3 19 13.1903 3.69283 1 -2 3 19 1.43619 3.65370 -2 1 3 19 1.43619 3.65370 1 -3 3 19 -0.3855 5.38373 -2 2 3 19 -0.3855 5.38373 1 -4 3 19 5.49521 6.80101 -2 3 3 19 5.49521 6.80101 1 1 4 19 11.6885 4.01939 -2 -2 4 19 11.6885 4.01939 1 0 4 19 27.9392 5.95588 -2 -1 4 19 27.9392 5.95588 1 -1 4 19 21.9599 5.77489 -2 0 4 19 21.9599 5.77489 1 -2 4 19 34.8475 4.30274 -2 1 4 19 34.8475 4.30274 1 0 0 20 -8.5127 7.75015 -2 -1 0 20 -8.5127 7.75015 1 -1 0 20 1.50109 8.03807 -2 0 0 20 1.50109 8.03807 1 -2 0 20 -24.203 33.8380 -2 0 0 20 -24.203 33.8380 1 -1 1 20 -1.3641 9.23078 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 88798 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 F1 F -0.1186(4) 0.0681(6) 0.1903(4) 0.0447(17) Uani 1 1 d . . F2 F -0.1709(4) 0.2440(7) 0.2393(3) 0.0427(17) Uani 1 1 d . . O4 O -0.0812(4) 0.2496(6) 0.1267(4) 0.0239(15) Uani 1 1 d . . O5 O 0.0686(4) 0.4915(6) 0.1074(4) 0.0248(15) Uani 1 1 d . . O8 O -0.0146(4) 0.2043(7) 0.2512(4) 0.0272(16) Uani 1 1 d . . N9 N 0.1235(5) 0.2807(7) 0.2442(5) 0.0196(17) Uani 1 1 d . . C1 C 0.1574(7) 0.0640(11) 0.0758(6) 0.035(2) Uani 1 1 d . . H1A H 0.2097 0.1125 0.0702 0.042 Uiso 1 1 calc R U H1B H 0.1635 -0.0203 0.0839 0.042 Uiso 1 1 calc R U C2 C 0.0795(7) 0.1116(9) 0.0724(6) 0.025(2) Uani 1 1 d . . H2 H 0.0287 0.0605 0.0782 0.031 Uiso 1 1 calc R U C3 C 0.0619(6) 0.2451(9) 0.0597(5) 0.024(2) Uani 1 1 d . . H3 H 0.1214 0.2879 0.0603 0.029 Uiso 1 1 calc R U C4 C 0.0063(6) 0.2952(9) 0.1284(5) 0.021(2) Uani 1 1 d . . C5 C 0.0042(5) 0.4370(9) 0.1252(5) 0.0181(19) Uani 1 1 d . . C6 C -0.0818(6) 0.4963(10) 0.1462(6) 0.030(2) Uani 1 1 d . . H6A H -0.0696 0.5801 0.1615 0.045 Uiso 1 1 calc R U H6B H -0.1079 0.4536 0.1911 0.045 Uiso 1 1 calc R U H6C H -0.1245 0.4944 0.0997 0.045 Uiso 1 1 calc R U C7 C 0.0122(8) 0.2690(11) -0.0212(5) 0.034(2) Uani 1 1 d . . H7A H -0.0040 0.3544 -0.0251 0.051 Uiso 1 1 calc R U H7B H -0.0429 0.2200 -0.0254 0.051 Uiso 1 1 calc R U H7C H 0.0517 0.2478 -0.0648 0.051 Uiso 1 1 calc R U C8 C 0.0456(6) 0.2609(9) 0.2128(6) 0.022(2) Uani 1 1 d . . C10 C 0.1477(6) 0.2394(11) 0.3269(5) 0.030(2) Uani 1 1 d . . H10A H 0.1425 0.1508 0.3310 0.037 Uiso 1 1 calc R U H10B H 0.1076 0.2769 0.3659 0.037 Uiso 1 1 calc R U C11 C 0.2436(6) 0.2785(10) 0.3424(6) 0.029(2) Uani 1 1 d . . H11A H 0.2462 0.3556 0.3722 0.035 Uiso 1 1 calc R U H11B H 0.2781 0.2170 0.3739 0.035 Uiso 1 1 calc R U C12 C 0.2807(7) 0.2929(10) 0.2618(7) 0.032(2) Uani 1 1 d . . H12A H 0.3003 0.2143 0.2407 0.039 Uiso 1 1 calc R U H12B H 0.3332 0.3485 0.2640 0.039 Uiso 1 1 calc R U C13 C 0.2037(5) 0.3445(10) 0.2098(6) 0.029(2) Uani 1 1 d . . H13A H 0.1992 0.4329 0.2159 0.035 Uiso 1 1 calc R U H13B H 0.2101 0.3244 0.1525 0.035 Uiso 1 1 calc R U B1 B -0.1023(7) 0.1916(12) 0.1986(7) 0.030(3) Uani 1 1 d . . F101 F -0.1632(4) 0.7220(6) 0.4858(3) 0.0318(14) Uani 1 1 d . . F102 F -0.0911(4) 0.9005(5) 0.4818(4) 0.0338(14) Uani 1 1 d . . O104 O -0.0630(4) 0.7538(6) 0.3836(3) 0.0185(14) Uani 1 1 d . . O105 O 0.0683(4) 0.5315(6) 0.3023(4) 0.0288(16) Uani 1 1 d . . O108 O -0.0043(4) 0.7279(6) 0.5144(3) 0.0192(13) Uani 1 1 d . . N109 N 0.1327(5) 0.6557(7) 0.4957(5) 0.0199(18) Uani 1 1 d . . C101 C 0.1757(8) 0.9344(10) 0.4105(7) 0.041(3) Uani 1 1 d . . H10C H 0.2271 0.8830 0.4118 0.049 Uiso 1 1 calc R U H10D H 0.1790 1.0106 0.4363 0.049 Uiso 1 1 calc R U C102 C 0.1002(7) 0.9002(9) 0.3731(6) 0.031(2) Uani 1 1 d . . H102 H 0.0504 0.9543 0.3732 0.037 Uiso 1 1 calc R U C103 C 0.0861(6) 0.7828(9) 0.3302(5) 0.0188(19) Uani 1 1 d . . H103 H 0.1460 0.7420 0.3259 0.023 Uiso 1 1 calc R U C104 C 0.0237(6) 0.7018(9) 0.3784(5) 0.022(2) Uani 1 1 d . . C105 C 0.0137(6) 0.5741(8) 0.3440(5) 0.019(2) Uani 1 1 d . . C106 C -0.0683(6) 0.5039(9) 0.3680(6) 0.028(2) Uani 1 1 d . . H10E H -0.0599 0.4185 0.3557 0.042 Uiso 1 1 calc R U H10F H -0.1222 0.5341 0.3382 0.042 Uiso 1 1 calc R U H10G H -0.0762 0.5136 0.4257 0.042 Uiso 1 1 calc R U C107 C 0.0450(7) 0.8056(11) 0.2447(6) 0.034(3) Uani 1 1 d . . H10H H 0.0426 0.7297 0.2148 0.051 Uiso 1 1 calc R U H10I H 0.0828 0.8635 0.2170 0.051 Uiso 1 1 calc R U H10J H -0.0163 0.8380 0.2482 0.051 Uiso 1 1 calc R U C108 C 0.0548(6) 0.6941(8) 0.4666(5) 0.0178(19) Uani 1 1 d . U C110 C 0.2096(7) 0.6097(9) 0.4487(5) 0.024(2) Uani 1 1 d . . H11C H 0.2386 0.6757 0.4193 0.029 Uiso 1 1 calc R U H11D H 0.1887 0.5471 0.4099 0.029 Uiso 1 1 calc R U C111 C 0.2736(6) 0.5576(9) 0.5125(6) 0.025(2) Uani 1 1 d . . H11E H 0.3372 0.5633 0.4965 0.030 Uiso 1 1 calc R U H11F H 0.2590 0.4723 0.5233 0.030 Uiso 1 1 calc R U C112 C 0.2573(6) 0.6369(11) 0.5862(6) 0.030(2) Uani 1 1 d . . H11G H 0.2763 0.5949 0.6364 0.036 Uiso 1 1 calc R U H11H H 0.2907 0.7139 0.5832 0.036 Uiso 1 1 calc R U C113 C 0.1573(6) 0.6576(9) 0.5817(6) 0.022(2) Uani 1 1 d . . H11I H 0.1253 0.5932 0.6102 0.027 Uiso 1 1 calc R U H11J H 0.1421 0.7362 0.6056 0.027 Uiso 1 1 calc R U B100 B -0.0867(6) 0.7787(12) 0.4634(7) 0.024(2) Uani 1 1 d . . F201 F 0.6860(3) 0.2414(7) 0.7454(4) 0.0409(16) Uani 1 1 d . . F202 F 0.6370(4) 0.0653(6) 0.6928(4) 0.0470(17) Uani 1 1 d . . O204 O 0.5937(4) 0.2457(6) 0.6276(4) 0.0227(15) Uani 1 1 d . . O205 O 0.4469(4) 0.4914(6) 0.6021(4) 0.0274(15) Uani 1 1 d . . O208 O 0.5302(4) 0.1970(6) 0.7489(4) 0.0248(15) Uani 1 1 d . . N209 N 0.3880(5) 0.2640(7) 0.7318(4) 0.0190(16) Uani 1 1 d . . C201 C 0.3556(7) 0.0617(11) 0.5567(6) 0.035(2) Uani 1 1 d . . H20A H 0.3023 0.1084 0.5477 0.042 Uiso 1 1 calc R U H20B H 0.3513 -0.0232 0.5625 0.042 Uiso 1 1 calc R U C202 C 0.4338(6) 0.1135(9) 0.5612(5) 0.022(2) Uani 1 1 d . . H202 H 0.4856 0.0640 0.5702 0.026 Uiso 1 1 calc R U C203 C 0.4484(6) 0.2459(9) 0.5530(5) 0.0192(19) Uani 1 1 d . . H203 H 0.3882 0.2871 0.5509 0.023 Uiso 1 1 calc R U C204 C 0.5045(6) 0.2923(10) 0.6272(5) 0.023(2) Uani 1 1 d . . C205 C 0.5100(6) 0.4316(9) 0.6282(5) 0.0192(19) Uani 1 1 d . . C206 C 0.5951(6) 0.4906(9) 0.6615(6) 0.023(2) Uani 1 1 d . . H20C H 0.5808 0.5715 0.6808 0.034 Uiso 1 1 calc R U H20D H 0.6392 0.4964 0.6194 0.034 Uiso 1 1 calc R U H20E H 0.6207 0.4425 0.7062 0.034 Uiso 1 1 calc R U C207 C 0.4963(7) 0.2731(10) 0.4757(5) 0.026(2) Uani 1 1 d . . H20F H 0.4913 0.3592 0.4635 0.039 Uiso 1 1 calc R U H20G H 0.4681 0.2265 0.4315 0.039 Uiso 1 1 calc R U H20H H 0.5604 0.2510 0.4824 0.039 Uiso 1 1 calc R U C208 C 0.4691(5) 0.2523(8) 0.7051(5) 0.0183(19) Uani 1 1 d . . C210 C 0.3094(6) 0.3216(9) 0.6905(6) 0.026(2) Uani 1 1 d . . H21A H 0.2832 0.2687 0.6478 0.031 Uiso 1 1 calc R U H21B H 0.3268 0.3992 0.6663 0.031 Uiso 1 1 calc R U C211 C 0.2441(6) 0.3407(10) 0.7546(6) 0.031(2) Uani 1 1 d . . H21C H 0.1809 0.3406 0.7324 0.037 Uiso 1 1 calc R U H21D H 0.2561 0.4174 0.7833 0.037 Uiso 1 1 calc R U C212 C 0.2620(6) 0.2333(12) 0.8095(6) 0.039(3) Uani 1 1 d . . H21E H 0.2333 0.1594 0.7870 0.046 Uiso 1 1 calc R U H21F H 0.2395 0.2481 0.8636 0.046 Uiso 1 1 calc R U C213 C 0.3657(6) 0.2231(10) 0.8120(5) 0.027(2) Uani 1 1 d . . H21G H 0.3937 0.2756 0.8541 0.033 Uiso 1 1 calc R U H21H H 0.3856 0.1390 0.8215 0.033 Uiso 1 1 calc R U B200 B 0.6180(8) 0.1845(11) 0.7020(7) 0.030(3) Uani 1 1 d . . F301 F 0.5919(3) 0.8900(5) -0.0134(4) 0.0325(14) Uani 1 1 d . . F302 F 0.6628(3) 0.7107(6) -0.0033(3) 0.0305(14) Uani 1 1 d . . O304 O 0.5597(4) 0.7424(6) -0.1127(4) 0.0227(15) Uani 1 1 d . . O305 O 0.4254(4) 0.5225(6) -0.2034(4) 0.0277(16) Uani 1 1 d . . O308 O 0.5049(4) 0.7199(6) 0.0164(4) 0.0218(14) Uani 1 1 d . . N309 N 0.3656(5) 0.6464(6) -0.0094(4) 0.0167(16) Uani 1 1 d . . C301 C 0.3167(8) 0.9248(10) -0.1019(7) 0.040(3) Uani 1 1 d . . H30A H 0.2640 0.8773 -0.1122 0.048 Uiso 1 1 calc R U H30B H 0.3127 0.9981 -0.0730 0.048 Uiso 1 1 calc R U C302 C 0.3930(6) 0.8898(9) -0.1269(6) 0.028(2) Uani 1 1 d . . H302 H 0.4441 0.9398 -0.1154 0.033 Uiso 1 1 calc R U C303 C 0.4082(7) 0.7750(10) -0.1736(6) 0.028(2) Uani 1 1 d . . H303 H 0.3489 0.7329 -0.1825 0.034 Uiso 1 1 calc R U C304 C 0.4734(6) 0.6920(9) -0.1218(5) 0.0195(19) Uani 1 1 d . . C305 C 0.4801(5) 0.5624(10) -0.1558(5) 0.020(2) Uani 1 1 d . . C306 C 0.5593(6) 0.4894(9) -0.1226(6) 0.028(2) Uani 1 1 d . . H30C H 0.5526 0.4055 -0.1400 0.042 Uiso 1 1 calc R U H30D H 0.5611 0.4930 -0.0638 0.042 Uiso 1 1 calc R U H30E H 0.6158 0.5223 -0.1423 0.042 Uiso 1 1 calc R U C307 C 0.4474(7) 0.7982(11) -0.2525(7) 0.040(3) Uani 1 1 d . . H30F H 0.4565 0.7216 -0.2801 0.060 Uiso 1 1 calc R U H30G H 0.5056 0.8395 -0.2444 0.060 Uiso 1 1 calc R U H30H H 0.4058 0.8488 -0.2850 0.060 Uiso 1 1 calc R U C308 C 0.4426(6) 0.6826(8) -0.0347(5) 0.0134(17) Uani 1 1 d . U C310 C 0.2881(6) 0.5982(9) -0.0589(6) 0.024(2) Uani 1 1 d . . H31A H 0.3078 0.5328 -0.0946 0.029 Uiso 1 1 calc R U H31B H 0.2588 0.6624 -0.0920 0.029 Uiso 1 1 calc R U C311 C 0.2250(6) 0.5512(10) 0.0029(5) 0.027(2) Uani 1 1 d . . H31C H 0.2395 0.4666 0.0172 0.033 Uiso 1 1 calc R U H31D H 0.1611 0.5560 -0.0170 0.033 Uiso 1 1 calc R U C312 C 0.2427(6) 0.6351(11) 0.0750(6) 0.032(2) Uani 1 1 d . . H31E H 0.2121 0.7137 0.0667 0.038 Uiso 1 1 calc R U H31F H 0.2224 0.5983 0.1252 0.038 Uiso 1 1 calc R U C313 C 0.3458(7) 0.6486(10) 0.0765(5) 0.025(2) Uani 1 1 d . . H31G H 0.3652 0.7256 0.1017 0.030 Uiso 1 1 calc R U H31H H 0.3760 0.5811 0.1057 0.030 Uiso 1 1 calc R U B300 B 0.5861(7) 0.7687(10) -0.0300(6) 0.021(2) 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 0.047(4) 0.030(3) 0.056(4) 0.017(3) -0.011(3) -0.020(3) F2 0.027(3) 0.076(5) 0.025(3) 0.013(3) -0.001(2) -0.003(3) O4 0.019(3) 0.028(4) 0.024(3) 0.010(3) -0.007(3) -0.007(3) O5 0.025(3) 0.019(4) 0.031(4) 0.003(3) 0.006(3) -0.002(3) O8 0.021(3) 0.033(4) 0.027(3) 0.012(3) 0.004(3) -0.007(3) N9 0.016(4) 0.015(4) 0.028(4) 0.008(3) 0.004(3) 0.004(3) C1 0.046(6) 0.030(6) 0.028(5) 0.003(5) 0.007(5) 0.003(5) C2 0.029(5) 0.024(5) 0.023(5) -0.007(4) 0.002(4) 0.000(4) C3 0.024(5) 0.019(5) 0.028(5) 0.000(4) 0.006(4) -0.009(4) C4 0.019(4) 0.025(6) 0.019(5) 0.006(4) -0.006(4) -0.009(4) C5 0.016(4) 0.024(5) 0.015(4) 0.007(4) 0.000(3) -0.013(4) C6 0.025(5) 0.038(6) 0.026(5) 0.003(5) -0.002(4) -0.001(5) C7 0.050(6) 0.032(6) 0.020(5) -0.007(5) 0.000(4) -0.001(5) C8 0.015(4) 0.018(5) 0.033(5) -0.001(4) 0.006(4) 0.013(4) C10 0.028(5) 0.040(7) 0.022(5) 0.014(5) -0.008(4) 0.011(5) C11 0.032(5) 0.028(6) 0.027(5) -0.002(4) -0.001(4) 0.008(4) C12 0.023(5) 0.030(5) 0.044(6) 0.000(5) 0.004(5) 0.007(4) C13 0.012(4) 0.038(6) 0.037(6) 0.004(5) 0.011(4) -0.009(4) B1 0.018(5) 0.043(7) 0.030(6) 0.012(6) -0.004(4) -0.011(5) F101 0.024(3) 0.041(4) 0.031(3) 0.003(3) 0.008(2) -0.001(3) F102 0.041(3) 0.015(3) 0.045(3) -0.001(3) 0.005(3) 0.012(3) O104 0.018(3) 0.020(3) 0.018(3) 0.006(3) -0.004(2) 0.004(3) O105 0.031(4) 0.028(4) 0.027(3) -0.005(3) 0.001(3) 0.004(3) O108 0.018(3) 0.023(4) 0.017(3) 0.003(3) -0.001(2) 0.009(3) N109 0.028(4) 0.015(4) 0.016(4) -0.005(3) 0.000(3) -0.005(3) C101 0.046(7) 0.021(6) 0.055(7) 0.005(6) 0.001(6) -0.005(5) C102 0.035(5) 0.020(5) 0.038(5) 0.008(5) 0.014(5) -0.003(4) C103 0.016(4) 0.016(4) 0.025(4) -0.002(4) 0.013(4) 0.000(4) C104 0.024(5) 0.022(5) 0.019(4) 0.007(4) 0.001(4) -0.011(4) C105 0.034(5) 0.012(5) 0.012(4) 0.000(4) -0.005(4) 0.005(4) C106 0.037(5) 0.019(5) 0.029(5) -0.007(4) 0.007(4) -0.002(4) C107 0.035(6) 0.038(7) 0.029(5) 0.024(5) 0.001(4) -0.011(5) C108 0.020(4) 0.013(4) 0.021(4) -0.011(3) 0.001(3) -0.002(3) C110 0.032(5) 0.023(5) 0.017(4) 0.010(4) 0.013(4) 0.002(4) C111 0.024(4) 0.018(5) 0.031(5) -0.001(4) 0.000(4) 0.011(4) C112 0.028(5) 0.035(6) 0.027(5) 0.006(5) -0.002(4) -0.001(4) C113 0.022(5) 0.016(5) 0.029(5) 0.000(4) -0.004(4) 0.001(4) B100 0.007(5) 0.037(7) 0.029(5) 0.008(5) 0.001(4) 0.008(4) F201 0.015(3) 0.067(4) 0.040(3) 0.017(3) -0.004(2) 0.000(3) F202 0.041(3) 0.040(4) 0.061(4) 0.015(4) 0.010(3) 0.021(3) O204 0.020(3) 0.028(4) 0.020(3) 0.001(3) 0.003(2) 0.007(3) O205 0.030(3) 0.025(4) 0.027(3) -0.003(3) -0.007(3) -0.004(3) O208 0.021(3) 0.023(4) 0.030(3) 0.003(3) 0.004(3) 0.006(3) N209 0.029(4) 0.008(4) 0.020(4) -0.005(3) -0.008(3) 0.003(3) C201 0.040(6) 0.027(6) 0.037(5) 0.001(5) -0.001(5) 0.004(5) C202 0.033(5) 0.017(5) 0.016(4) -0.004(4) -0.001(4) 0.005(4) C203 0.013(4) 0.019(5) 0.026(4) -0.002(4) -0.001(3) 0.003(4) C204 0.018(4) 0.033(6) 0.018(5) 0.003(4) 0.004(3) -0.011(4) C205 0.018(4) 0.020(5) 0.019(4) -0.009(4) 0.001(3) -0.004(4) C206 0.025(5) 0.023(5) 0.021(4) 0.003(4) 0.003(4) -0.003(4) C207 0.035(5) 0.021(5) 0.023(5) -0.005(4) -0.001(4) -0.001(4) C208 0.015(4) 0.014(5) 0.025(4) -0.010(4) -0.001(3) -0.001(4) C210 0.026(5) 0.018(5) 0.034(5) -0.006(4) -0.007(4) 0.003(4) C211 0.016(4) 0.042(7) 0.034(5) -0.014(5) -0.006(4) 0.003(4) C212 0.021(5) 0.055(8) 0.040(5) -0.009(6) 0.002(4) -0.006(5) C213 0.025(5) 0.032(6) 0.025(4) 0.003(4) 0.000(4) -0.002(4) B200 0.027(6) 0.028(6) 0.035(6) 0.002(5) 0.000(5) 0.008(5) F301 0.030(3) 0.026(3) 0.041(3) -0.010(3) 0.006(3) -0.010(3) F302 0.015(2) 0.046(4) 0.031(3) 0.002(3) -0.003(2) 0.001(3) O304 0.017(3) 0.022(4) 0.029(3) 0.003(3) -0.002(3) -0.003(3) O305 0.025(3) 0.027(4) 0.031(4) -0.004(3) 0.000(3) -0.002(3) O308 0.020(3) 0.023(4) 0.022(3) -0.002(3) -0.004(2) -0.001(3) N309 0.024(4) 0.011(4) 0.015(3) 0.004(3) -0.002(3) 0.001(3) C301 0.039(6) 0.027(6) 0.054(7) -0.005(5) -0.002(6) -0.002(5) C302 0.024(5) 0.016(5) 0.043(6) 0.006(5) 0.005(4) -0.001(4) C303 0.025(5) 0.022(5) 0.039(6) 0.004(5) 0.002(4) -0.004(4) C304 0.020(5) 0.014(5) 0.025(4) 0.000(4) 0.006(4) -0.006(4) C305 0.008(4) 0.035(6) 0.016(4) 0.004(4) 0.004(3) 0.000(4) C306 0.033(5) 0.020(5) 0.032(5) -0.003(4) 0.010(4) 0.008(4) C307 0.036(6) 0.040(7) 0.043(7) 0.009(6) 0.000(5) 0.007(5) C308 0.011(3) 0.010(3) 0.018(3) -0.001(2) -0.004(2) 0.003(2) C310 0.011(4) 0.026(6) 0.036(5) -0.004(4) -0.002(4) -0.005(4) C311 0.018(4) 0.034(6) 0.028(5) -0.003(5) -0.005(4) -0.001(4) C312 0.017(5) 0.041(7) 0.038(6) -0.003(5) 0.006(4) -0.010(4) C313 0.029(5) 0.024(6) 0.022(5) -0.004(4) 0.005(4) -0.003(4) B300 0.024(6) 0.021(6) 0.018(5) 0.001(4) 0.004(4) -0.004(4) 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 112.9(7) C8 O8 B1 110.2(7) C8 N9 C10 120.8(8) C8 N9 C13 129.6(8) C10 N9 C13 109.6(7) C2 C1 H1A 120.0 C2 C1 H1B 120.0 H1A C1 H1B 120.0 C1 C2 C3 124.4(10) C1 C2 H2 117.8 C3 C2 H2 117.8 C2 C3 C7 111.4(9) C2 C3 C4 109.9(8) C7 C3 C4 110.0(8) C2 C3 H3 108.5 C7 C3 H3 108.5 C4 C3 H3 108.5 O4 C4 C3 112.2(8) O4 C4 C8 104.0(7) C3 C4 C8 113.4(7) O4 C4 C5 110.3(8) C3 C4 C5 110.2(7) C8 C4 C5 106.4(7) O5 C5 C6 122.7(9) O5 C5 C4 120.5(9) C6 C5 C4 116.8(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 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 N9 C8 O8 121.1(9) N9 C8 C4 129.4(8) O8 C8 C4 109.5(7) N9 C10 C11 105.1(8) N9 C10 H10A 110.7 C11 C10 H10A 110.7 N9 C10 H10B 110.7 C11 C10 H10B 110.7 H10A C10 H10B 108.8 C12 C11 C10 105.0(8) C12 C11 H11A 110.7 C10 C11 H11A 110.7 C12 C11 H11B 110.7 C10 C11 H11B 110.7 H11A C11 H11B 108.8 C11 C12 C13 105.2(8) C11 C12 H12A 110.7 C13 C12 H12A 110.7 C11 C12 H12B 110.7 C13 C12 H12B 110.7 H12A C12 H12B 108.8 N9 C13 C12 100.8(8) N9 C13 H13A 111.6 C12 C13 H13A 111.6 N9 C13 H13B 111.6 C12 C13 H13B 111.6 H13A C13 H13B 109.4 F2 B1 F1 109.7(8) F2 B1 O4 115.0(10) F1 B1 O4 114.0(10) F2 B1 O8 107.5(9) F1 B1 O8 106.5(9) O4 B1 O8 103.4(7) C104 O104 B100 113.5(7) C108 O108 B100 107.9(7) C108 N109 C113 122.6(8) C108 N109 C110 126.5(8) C113 N109 C110 110.8(7) C102 C101 H10C 120.0 C102 C101 H10D 120.0 H10C C101 H10D 120.0 C101 C102 C103 125.3(10) C101 C102 H102 117.4 C103 C102 H102 117.4 C102 C103 C104 109.5(7) C102 C103 C107 109.8(8) C104 C103 C107 110.9(8) C102 C103 H103 108.9 C104 C103 H103 108.9 C107 C103 H103 108.9 O104 C104 C108 101.6(7) O104 C104 C105 109.2(7) C108 C104 C105 109.2(8) O104 C104 C103 111.0(8) C108 C104 C103 111.9(8) C105 C104 C103 113.3(7) O105 C105 C106 121.5(9) O105 C105 C104 122.1(9) C106 C105 C104 116.3(8) C105 C106 H10E 109.5 C105 C106 H10F 109.5 H10E C106 H10F 109.5 C105 C106 H10G 109.5 H10E C106 H10G 109.5 H10F C106 H10G 109.5 C103 C107 H10H 109.5 C103 C107 H10I 109.5 H10H C107 H10I 109.5 C103 C107 H10J 109.5 H10H C107 H10J 109.5 H10I C107 H10J 109.5 O108 C108 N109 119.0(8) O108 C108 C104 113.8(8) N109 C108 C104 127.2(8) N109 C110 C111 103.2(7) N109 C110 H11C 111.1 C111 C110 H11C 111.1 N109 C110 H11D 111.1 C111 C110 H11D 111.1 H11C C110 H11D 109.1 C110 C111 C112 103.3(8) C110 C111 H11E 111.1 C112 C111 H11E 111.1 C110 C111 H11F 111.1 C112 C111 H11F 111.1 H11E C111 H11F 109.1 C113 C112 C111 103.6(8) C113 C112 H11G 111.0 C111 C112 H11G 111.0 C113 C112 H11H 111.0 C111 C112 H11H 111.0 H11G C112 H11H 109.0 N109 C113 C112 104.5(8) N109 C113 H11I 110.9 C112 C113 H11I 110.9 N109 C113 H11J 110.9 C112 C113 H11J 110.9 H11I C113 H11J 108.9 F101 B100 F102 110.0(8) F101 B100 O104 114.1(9) F102 B100 O104 114.4(9) F101 B100 O108 108.7(8) F102 B100 O108 106.0(9) O104 B100 O108 102.9(7) C204 O204 B200 111.9(7) C208 O208 B200 109.6(7) C208 N209 C213 121.9(8) C208 N209 C210 127.0(8) C213 N209 C210 111.0(8) C202 C201 H20A 120.0 C202 C201 H20B 120.0 H20A C201 H20B 120.0 C201 C202 C203 124.5(9) C201 C202 H202 117.7 C203 C202 H202 117.7 C202 C203 C207 110.2(8) C202 C203 C204 109.2(8) C207 C203 C204 111.0(7) C202 C203 H203 108.8 C207 C203 H203 108.8 C204 C203 H203 108.8 O204 C204 C208 104.4(7) O204 C204 C203 110.4(8) C208 C204 C203 113.7(7) O204 C204 C205 108.5(7) C208 C204 C205 108.0(8) C203 C204 C205 111.5(8) O205 C205 C206 120.9(9) O205 C205 C204 120.3(8) C206 C205 C204 118.8(8) C205 C206 H20C 109.5 C205 C206 H20D 109.5 H20C C206 H20D 109.5 C205 C206 H20E 109.5 H20C C206 H20E 109.5 H20D C206 H20E 109.5 C203 C207 H20F 109.5 C203 C207 H20G 109.5 H20F C207 H20G 109.5 C203 C207 H20H 109.5 H20F C207 H20H 109.5 H20G C207 H20H 109.5 O208 C208 N209 118.9(8) O208 C208 C204 111.9(7) N209 C208 C204 129.2(8) N209 C210 C211 104.4(8) N209 C210 H21A 110.9 C211 C210 H21A 110.9 N209 C210 H21B 110.9 C211 C210 H21B 110.9 H21A C210 H21B 108.9 C210 C211 C212 102.7(8) C210 C211 H21C 111.2 C212 C211 H21C 111.2 C210 C211 H21D 111.2 C212 C211 H21D 111.2 H21C C211 H21D 109.1 C211 C212 C213 102.9(8) C211 C212 H21E 111.2 C213 C212 H21E 111.2 C211 C212 H21F 111.2 C213 C212 H21F 111.2 H21E C212 H21F 109.1 N209 C213 C212 102.4(8) N209 C213 H21G 111.3 C212 C213 H21G 111.3 N209 C213 H21H 111.3 C212 C213 H21H 111.3 H21G C213 H21H 109.2 F202 B200 F201 110.9(9) F202 B200 O204 113.8(9) F201 B200 O204 112.9(10) F202 B200 O208 108.9(9) F201 B200 O208 107.6(8) O204 B200 O208 102.0(8) C304 O304 B300 113.1(7) C308 O308 B300 109.1(6) C308 N309 C313 121.6(8) C308 N309 C310 126.8(7) C313 N309 C310 111.6(8) C302 C301 H30A 120.0 C302 C301 H30B 120.0 H30A C301 H30B 120.0 C301 C302 C303 125.1(10) C301 C302 H302 117.5 C303 C302 H302 117.5 C307 C303 C302 112.4(9) C307 C303 C304 109.8(9) C302 C303 C304 108.2(8) C307 C303 H303 108.8 C302 C303 H303 108.8 C304 C303 H303 108.8 O304 C304 C308 103.2(7) O304 C304 C305 109.9(7) C308 C304 C305 107.9(7) O304 C304 C303 111.2(7) C308 C304 C303 111.1(7) C305 C304 C303 113.0(7) O305 C305 C306 122.5(10) O305 C305 C304 122.4(8) C306 C305 C304 115.1(8) C305 C306 H30C 109.5 C305 C306 H30D 109.5 H30C C306 H30D 109.5 C305 C306 H30E 109.5 H30C C306 H30E 109.5 H30D C306 H30E 109.5 C303 C307 H30F 109.5 C303 C307 H30G 109.5 H30F C307 H30G 109.5 C303 C307 H30H 109.5 H30F C307 H30H 109.5 H30G C307 H30H 109.5 N309 C308 O308 119.7(7) N309 C308 C304 128.7(7) O308 C308 C304 111.6(7) N309 C310 C311 103.2(7) N309 C310 H31A 111.1 C311 C310 H31A 111.1 N309 C310 H31B 111.1 C311 C310 H31B 111.1 H31A C310 H31B 109.1 C310 C311 C312 103.6(8) C310 C311 H31C 111.0 C312 C311 H31C 111.0 C310 C311 H31D 111.0 C312 C311 H31D 111.0 H31C C311 H31D 109.0 C313 C312 C311 102.0(8) C313 C312 H31E 111.4 C311 C312 H31E 111.4 C313 C312 H31F 111.4 C311 C312 H31F 111.4 H31E C312 H31F 109.2 N309 C313 C312 102.7(8) N309 C313 H31G 111.2 C312 C313 H31G 111.2 N309 C313 H31H 111.2 C312 C313 H31H 111.2 H31G C313 H31H 109.1 F302 B300 F301 110.6(8) F302 B300 O304 113.8(8) F301 B300 O304 113.6(8) F302 B300 O308 108.8(8) F301 B300 O308 106.5(7) O304 B300 O308 102.8(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance F1 B1 1.399(15) F2 B1 1.373(14) O4 C4 1.387(11) O4 B1 1.408(13) O5 C5 1.176(10) O8 C8 1.282(11) O8 B1 1.541(12) N9 C8 1.264(12) N9 C10 1.484(11) N9 C13 1.514(11) C1 C2 1.266(14) C1 H1A 0.9500 C1 H1B 0.9500 C2 C3 1.519(14) C2 H2 0.9500 C3 C7 1.531(13) C3 C4 1.543(12) C3 H3 1.0000 C4 C8 1.548(12) C4 C5 1.577(14) C5 C6 1.486(13) 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 C11 1.494(13) C10 H10A 0.9900 C10 H10B 0.9900 C11 C12 1.481(14) C11 H11A 0.9900 C11 H11B 0.9900 C12 C13 1.515(14) C12 H12A 0.9900 C12 H12B 0.9900 C13 H13A 0.9900 C13 H13B 0.9900 F101 B100 1.360(12) F102 B100 1.389(14) O104 C104 1.412(11) O104 B100 1.418(12) O105 C105 1.185(11) O108 C108 1.265(11) O108 B100 1.562(11) N109 C108 1.302(12) N109 C113 1.466(12) N109 C110 1.497(11) C101 C102 1.312(16) C101 H10C 0.9500 C101 H10D 0.9500 C102 C103 1.498(14) C102 H102 0.9500 C103 C104 1.540(12) C103 C107 1.547(13) C103 H103 1.0000 C104 C108 1.526(12) C104 C105 1.535(14) C105 C106 1.510(13) C106 H10E 0.9800 C106 H10F 0.9800 C106 H10G 0.9800 C107 H10H 0.9800 C107 H10I 0.9800 C107 H10J 0.9800 C110 C111 1.509(13) C110 H11C 0.9900 C110 H11D 0.9900 C111 C112 1.539(15) C111 H11E 0.9900 C111 H11F 0.9900 C112 C113 1.494(12) C112 H11G 0.9900 C112 H11H 0.9900 C113 H11I 0.9900 C113 H11J 0.9900 F201 B200 1.368(14) F202 B200 1.364(14) O204 C204 1.416(12) O204 B200 1.447(13) O205 C205 1.211(11) O208 C208 1.293(11) O208 B200 1.550(13) N209 C208 1.302(11) N209 C213 1.464(11) N209 C210 1.472(11) C201 C202 1.290(13) C201 H20A 0.9500 C201 H20B 0.9500 C202 C203 1.493(13) C202 H202 0.9500 C203 C207 1.528(12) C203 C204 1.549(12) C203 H203 1.0000 C204 C208 1.488(12) C204 C205 1.549(14) C205 C206 1.505(12) C206 H20C 0.9800 C206 H20D 0.9800 C206 H20E 0.9800 C207 H20F 0.9800 C207 H20G 0.9800 C207 H20H 0.9800 C210 C211 1.485(13) C210 H21A 0.9900 C210 H21B 0.9900 C211 C212 1.520(17) C211 H21C 0.9900 C211 H21D 0.9900 C212 C213 1.535(13) C212 H21E 0.9900 C212 H21F 0.9900 C213 H21G 0.9900 C213 H21H 0.9900 F301 B300 1.379(13) F302 B300 1.362(12) O304 C304 1.395(11) O304 B300 1.448(12) O305 C305 1.194(11) O308 C308 1.295(11) O308 B300 1.553(12) N309 C308 1.295(11) N309 C313 1.474(11) N309 C310 1.483(11) C301 C302 1.279(15) C301 H30A 0.9500 C301 H30B 0.9500 C302 C303 1.516(15) C302 H302 0.9500 C303 C307 1.483(15) C303 C304 1.567(14) C303 H303 1.0000 C304 C308 1.545(11) C304 C305 1.552(14) C305 C306 1.511(12) C306 H30C 0.9800 C306 H30D 0.9800 C306 H30E 0.9800 C307 H30F 0.9800 C307 H30G 0.9800 C307 H30H 0.9800 C310 C311 1.513(13) C310 H31A 0.9900 C310 H31B 0.9900 C311 C312 1.536(14) C311 H31C 0.9900 C311 H31D 0.9900 C312 C313 1.530(13) C312 H31E 0.9900 C312 H31F 0.9900 C313 H31G 0.9900 C313 H31H 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 C1 C2 C3 C7 113.5(11) C1 C2 C3 C4 -124.2(11) B1 O4 C4 C3 123.1(9) B1 O4 C4 C8 0.2(11) B1 O4 C4 C5 -113.6(9) C2 C3 C4 O4 -67.9(10) C7 C3 C4 O4 55.2(11) C2 C3 C4 C8 49.7(10) C7 C3 C4 C8 172.8(9) C2 C3 C4 C5 168.8(8) C7 C3 C4 C5 -68.1(10) O4 C4 C5 O5 -162.1(7) C3 C4 C5 O5 -37.7(11) C8 C4 C5 O5 85.6(10) O4 C4 C5 C6 18.2(11) C3 C4 C5 C6 142.7(8) C8 C4 C5 C6 -94.0(9) C10 N9 C8 O8 -0.3(14) C13 N9 C8 O8 179.8(9) C10 N9 C8 C4 -179.9(9) C13 N9 C8 C4 0.2(16) B1 O8 C8 N9 -179.3(9) B1 O8 C8 C4 0.3(11) O4 C4 C8 N9 179.3(9) C3 C4 C8 N9 57.1(13) C5 C4 C8 N9 -64.2(12) O4 C4 C8 O8 -0.3(10) C3 C4 C8 O8 -122.5(8) C5 C4 C8 O8 116.2(8) C8 N9 C10 C11 179.9(9) C13 N9 C10 C11 -0.2(11) N9 C10 C11 C12 -22.6(11) C10 C11 C12 C13 37.3(11) C8 N9 C13 C12 -158.1(10) C10 N9 C13 C12 21.9(10) C11 C12 C13 N9 -35.8(10) C4 O4 B1 F2 116.9(9) C4 O4 B1 F1 -115.2(9) C4 O4 B1 O8 0.0(12) C8 O8 B1 F2 -122.2(9) C8 O8 B1 F1 120.2(9) C8 O8 B1 O4 -0.2(12) C101 C102 C103 C104 108.5(11) C101 C102 C103 C107 -129.5(11) B100 O104 C104 C108 0.5(11) B100 O104 C104 C105 115.8(9) B100 O104 C104 C103 -118.6(9) C102 C103 C104 O104 63.1(10) C107 C103 C104 O104 -58.2(10) C102 C103 C104 C108 -49.6(11) C107 C103 C104 C108 -170.9(8) C102 C103 C104 C105 -173.6(8) C107 C103 C104 C105 65.0(10) O104 C104 C105 O105 146.5(8) C108 C104 C105 O105 -103.2(9) C103 C104 C105 O105 22.3(12) O104 C104 C105 C106 -35.2(10) C108 C104 C105 C106 75.1(9) C103 C104 C105 C106 -159.4(8) B100 O108 C108 N109 175.4(9) B100 O108 C108 C104 -5.7(11) C113 N109 C108 O108 -4.3(14) C110 N109 C108 O108 178.5(9) C113 N109 C108 C104 177.0(10) C110 N109 C108 C104 -0.3(16) O104 C104 C108 O108 3.6(11) C105 C104 C108 O108 -111.7(9) C103 C104 C108 O108 122.0(9) O104 C104 C108 N109 -177.6(8) C105 C104 C108 N109 67.1(12) C103 C104 C108 N109 -59.2(13) C108 N109 C110 C111 -170.0(9) C113 N109 C110 C111 12.5(11) N109 C110 C111 C112 -30.8(10) C110 C111 C112 C113 38.8(10) C108 N109 C113 C112 -165.9(9) C110 N109 C113 C112 11.7(11) C111 C112 C113 N109 -30.8(10) C104 O104 B100 F101 -121.0(8) C104 O104 B100 F102 111.0(9) C104 O104 B100 O108 -3.4(12) C108 O108 B100 F101 126.9(9) C108 O108 B100 F102 -114.9(8) C108 O108 B100 O104 5.6(11) C201 C202 C203 C207 -112.0(11) C201 C202 C203 C204 125.8(10) B200 O204 C204 C208 -2.9(10) B200 O204 C204 C203 -125.5(9) B200 O204 C204 C205 112.1(9) C202 C203 C204 O204 67.6(9) C207 C203 C204 O204 -54.1(10) C202 C203 C204 C208 -49.4(10) C207 C203 C204 C208 -171.1(9) C202 C203 C204 C205 -171.8(8) C207 C203 C204 C205 66.5(10) O204 C204 C205 O205 155.6(8) C208 C204 C205 O205 -91.8(10) C203 C204 C205 O205 33.8(12) O204 C204 C205 C206 -24.2(11) C208 C204 C205 C206 88.4(10) C203 C204 C205 C206 -146.0(8) B200 O208 C208 N209 175.1(9) B200 O208 C208 C204 -3.7(10) C213 N209 C208 O208 3.9(13) C210 N209 C208 O208 -178.8(8) C213 N209 C208 C204 -177.5(9) C210 N209 C208 C204 -0.2(16) O204 C204 C208 O208 4.1(10) C203 C204 C208 O208 124.5(9) C205 C204 C208 O208 -111.2(9) O204 C204 C208 N209 -174.5(9) C203 C204 C208 N209 -54.1(13) C205 C204 C208 N209 70.2(12) C208 N209 C210 C211 -164.7(9) C213 N209 C210 C211 12.9(10) N209 C210 C211 C212 -33.1(9) C210 C211 C212 C213 41.1(10) C208 N209 C213 C212 -169.6(9) C210 N209 C213 C212 12.7(10) C211 C212 C213 N209 -32.7(10) C204 O204 B200 F202 118.1(9) C204 O204 B200 F201 -114.3(9) C204 O204 B200 O208 1.0(11) C208 O208 B200 F202 -118.9(9) C208 O208 B200 F201 120.7(9) C208 O208 B200 O204 1.7(11) C301 C302 C303 C307 121.9(12) C301 C302 C303 C304 -116.6(12) B300 O304 C304 C308 -1.4(10) B300 O304 C304 C305 -116.3(8) B300 O304 C304 C303 117.8(9) C307 C303 C304 O304 56.5(10) C302 C303 C304 O304 -66.6(9) C307 C303 C304 C308 170.8(8) C302 C303 C304 C308 47.8(10) C307 C303 C304 C305 -67.7(10) C302 C303 C304 C305 169.3(7) O304 C304 C305 O305 -142.3(8) C308 C304 C305 O305 105.8(9) C303 C304 C305 O305 -17.5(12) O304 C304 C305 C306 39.2(10) C308 C304 C305 C306 -72.6(9) C303 C304 C305 C306 164.1(8) C313 N309 C308 O308 1.3(13) C310 N309 C308 O308 -178.3(8) C313 N309 C308 C304 -177.1(9) C310 N309 C308 C304 3.4(15) B300 O308 C308 N309 -174.8(8) B300 O308 C308 C304 3.8(10) O304 C304 C308 N309 176.8(8) C305 C304 C308 N309 -66.9(11) C303 C304 C308 N309 57.5(12) O304 C304 C308 O308 -1.7(10) C305 C304 C308 O308 114.7(8) C303 C304 C308 O308 -120.9(8) C308 N309 C310 C311 170.4(8) C313 N309 C310 C311 -9.2(11) N309 C310 C311 C312 31.0(10) C310 C311 C312 C313 -41.3(10) C308 N309 C313 C312 163.9(8) C310 N309 C313 C312 -16.4(11) C311 C312 C313 N309 34.8(11) C304 O304 B300 F302 120.9(8) C304 O304 B300 F301 -111.3(9) C304 O304 B300 O308 3.4(10) C308 O308 B300 F302 -125.4(8) C308 O308 B300 F301 115.4(8) C308 O308 B300 O304 -4.4(10)