#------------------------------------------------------------------------------ #$Date: 2017-06-27 04:13:01 +0300 (Tue, 27 Jun 2017) $ #$Revision: 198148 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/63/1546387.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_1546387 loop_ _publ_author_name 'Landmann, Johannes' 'Hennig, Philipp T.' 'Ignat'ev, Nikolai' 'Finze, Maik' _publ_section_title ; Borylation of Fluorinated Arenes with the Boron-centred Nucleophile B(CN)32− -- a Unique Entry to Aryltricyanoborates ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C7SC02249B _journal_year 2017 _chemical_formula_sum 'C52 H52.17 B6 F4 K6 N20 O8.01' _chemical_formula_weight 1460.91 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-05-09 deposited with the CCDC. 2017-06-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 113.7870(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 41.3012(11) _cell_length_b 8.4531(2) _cell_length_c 46.0735(11) _cell_measurement_reflns_used 9798 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.80 _cell_measurement_theta_min 2.56 _cell_volume 14718.9(6) _computing_cell_refinement 'Saint+ ver. V8.34A (Bruker AXS)' _computing_data_collection 'APEX2 ver. 2014.9 (Bruker AXS)' _computing_data_reduction 'Saint+ ver. V8.34A (Bruker AXS)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD area detector (Apex2)' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker X8-APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_unetI/netI 0.0368 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_number 44601 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.373 _diffrn_reflns_theta_min 1.120 _diffrn_source 'rotating-anode (Nonius FR-591)' _exptl_absorpt_coefficient_mu 0.425 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SadAbs 2014/5 (Bruker AXS)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.319 _exptl_crystal_description block _exptl_crystal_F_000 5986 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _refine_diff_density_max 1.075 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.084 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 944 _refine_ls_number_reflns 15069 _refine_ls_number_restraints 33 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0457 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+17.1488P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1250 _refine_ls_wR_factor_ref 0.1377 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11477 _reflns_number_total 15069 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7sc02249b2.cif _cod_data_source_block JL031_JL_K3Py3thfH2O _cod_database_code 1546387 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; test_a.res created by SHELXL-2014/7 TITL test_a.res in C2/c REM Old TITL test in C2/c REM SHELXT solution in C2/c REM R1 0.132, Rweak 0.001, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C53 B4 N25 O8 K6 CELL 0.71073 41.3012 8.4531 46.0735 90.000 113.787 90.000 ZERR 8 0.0011 0.0002 0.0011 0.000 0.001 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H B N O K F UNIT 416 417.4 48 160 64.07 48 32 TEMP -173 L.S. 10 ACTA 52 SHEL 5 0 BOND $H LIST 4 ISOR 0.005 C3 C4 C5 C6 O3b FMAP 2 PLAN 40 SHEL 999 0.8 DFIX 0.9 0.00001 O6 H200 O6 H201 DFIX 1.57 0.00001 H200 H201 WGHT 0.071800 17.148800 FVAR 0.05639 0.08897 K1 6 0.288951 -0.001983 0.195542 11.00000 0.01275 0.01213 = 0.01114 -0.00017 0.00506 -0.00056 C1 1 0.402265 0.022820 0.376148 11.00000 0.01070 0.01081 = 0.01050 0.00071 0.00451 0.00027 B1 3 0.441179 0.030398 0.375537 11.00000 0.00973 0.01924 = 0.01126 0.00113 0.00332 0.00065 N1 4 0.399864 0.015875 0.404368 11.00000 0.00911 0.01290 = 0.00941 0.00066 0.00343 -0.00086 F1 7 0.305723 0.002876 0.379666 11.00000 0.00947 0.02894 = 0.01349 0.00087 0.00436 -0.00079 O1 5 0.467155 0.779971 0.272069 11.00000 0.02940 0.02701 = 0.03341 -0.00584 0.00797 -0.00250 K2 6 0.288974 0.508887 -0.054571 11.00000 0.01276 0.01244 = 0.01026 -0.00006 0.00446 0.00043 C2 1 0.371652 0.020332 0.348348 11.00000 0.01414 0.01146 = 0.00731 0.00123 0.00526 -0.00033 B2 3 0.365803 -0.000345 0.439969 11.00000 0.00839 0.01516 = 0.00662 0.00052 0.00129 -0.00241 N2 4 0.490032 0.061877 0.436690 11.00000 0.01615 0.03794 = 0.01871 0.00036 0.00411 -0.00033 F2 7 0.375589 0.023840 0.320539 11.00000 0.01347 0.02820 = 0.00775 0.00021 0.00519 -0.00103 O2 5 0.529192 -0.254575 0.478096 11.00000 0.02877 0.02438 = 0.03001 -0.00402 0.00726 -0.00285 K3 6 0.438704 0.536265 0.300253 11.00000 0.01516 0.02206 = 0.01387 0.00006 0.00565 -0.00006 O6 5 0.248436 0.232777 0.375435 21.00000 0.02466 0.01749 = 0.01495 -0.00526 -0.00681 0.00083 H201 2 0.233758 0.149048 0.369336 21.00000 -1.20000 H200 2 0.271058 0.222488 0.389419 21.00000 -1.20000 B3 3 0.300360 0.015840 0.317069 11.00000 0.01040 0.01272 = 0.01026 0.00046 0.00252 0.00065 C3X 1 0.337888 0.014076 0.347614 11.00000 0.01001 0.00888 = 0.01013 0.00119 0.00186 0.00061 N3 4 0.445865 0.283435 0.340294 11.00000 0.02787 0.04080 = 0.03262 0.01210 0.01462 -0.00322 F3 7 0.305354 0.510824 0.129817 11.00000 0.00825 0.02821 = 0.01282 0.00010 0.00392 0.00027 K4 6 0.249256 0.278608 0.125256 11.00000 0.01945 0.02060 = 0.01436 0.00032 0.00821 0.00215 C41 1 0.338024 0.008221 0.377723 11.00000 0.00608 0.01212 = 0.01044 0.00101 0.00305 -0.00090 B4 3 0.440669 0.483341 0.125396 11.00000 0.00881 0.01680 = 0.00915 -0.00143 0.00346 0.00010 N4 4 0.450934 -0.239709 0.347370 11.00000 0.03462 0.04245 = 0.03618 -0.01340 0.01501 0.00656 PART 3 O3 5 0.355853 0.613554 0.391578 10.80000 0.02506 0.04620 = 0.02552 -0.00180 0.01516 0.00785 C3 1 0.360271 0.583799 0.363092 10.80000 0.03823 0.03021 = 0.02954 0.00589 0.01909 0.00723 AFIX 23 H3A 2 0.372191 0.673936 0.357777 10.80000 -1.20000 H3B 2 0.337118 0.565734 0.345233 10.80000 -1.20000 AFIX 0 C4 1 0.382383 0.440478 0.369655 10.80000 0.05768 0.04716 = 0.04224 -0.01028 0.01838 0.01734 AFIX 23 H4A 2 0.395275 0.434214 0.355646 10.80000 -1.20000 H4B 2 0.367956 0.343679 0.366938 10.80000 -1.20000 AFIX 0 C5 1 0.407626 0.463006 0.403942 10.80000 0.03914 0.04627 = 0.04993 -0.01483 0.00315 0.01716 AFIX 23 H5A 2 0.430091 0.511240 0.405444 10.80000 -1.20000 H5B 2 0.412885 0.360709 0.415374 10.80000 -1.20000 AFIX 0 C6 1 0.388147 0.572802 0.417383 10.80000 0.03165 0.03149 = 0.02958 -0.00133 0.01263 -0.00031 AFIX 23 H6A 2 0.383317 0.519049 0.434311 10.80000 -1.20000 H6B 2 0.402398 0.668783 0.426403 10.80000 -1.20000 AFIX 0 PART 4 O3B 5 0.354926 0.429259 0.389266 10.12000 0.01488 0.04083 = 0.01566 0.00659 0.01072 -0.00353 C3B 1 0.355391 0.476988 0.359996 10.20000 0.01611 0.04412 = 0.02212 0.00345 0.00487 0.00099 AFIX 23 H3B1 2 0.333663 0.537627 0.347637 10.20000 -1.20000 H3B2 2 0.356018 0.382654 0.347499 10.20000 -1.20000 AFIX 0 C4B 1 0.388587 0.478759 0.414582 10.20000 0.03095 0.09658 = 0.02000 0.00276 0.00011 0.02640 AFIX 23 H4AB 2 0.384100 0.553783 0.429043 10.20000 -1.20000 H4BB 2 0.401201 0.385659 0.427073 10.20000 -1.20000 AFIX 0 C5B 1 0.386790 0.576060 0.365934 10.20000 0.05351 0.07048 = 0.02176 0.00598 0.00376 -0.04137 AFIX 23 H5AB 2 0.379924 0.688488 0.361328 10.20000 -1.20000 H5BB 2 0.399027 0.541800 0.352429 10.20000 -1.20000 AFIX 0 C6B 1 0.410048 0.554676 0.399935 10.20000 0.01192 0.01607 = 0.05399 0.00628 -0.00602 -0.00554 AFIX 23 H6AB 2 0.430585 0.487368 0.402320 10.20000 -1.20000 H6BB 2 0.418893 0.658271 0.410048 10.20000 -1.20000 AFIX 0 PART -5 PART 0 O4 5 0.644351 0.114396 0.360678 11.00000 0.03057 0.03447 = 0.03071 0.00416 0.01486 -0.00476 F4 7 0.374999 0.497738 0.070412 11.00000 0.01273 0.02828 = 0.00792 -0.00082 0.00500 -0.00009 K5 6 0.438726 -0.021144 0.049930 11.00000 0.01643 0.01882 = 0.01319 -0.00066 0.00589 0.00071 C5X 1 0.367925 0.007811 0.405715 11.00000 0.01181 0.01022 = 0.00979 0.00073 0.00484 -0.00134 B5 3 0.365494 0.505923 0.190014 11.00000 0.00935 0.01294 = 0.00777 -0.00030 0.00280 -0.00016 N5 4 0.302603 0.031715 0.258693 11.00000 0.02508 0.02406 = 0.01385 0.00098 0.00612 0.00120 O5 5 0.367640 -0.008160 0.028509 11.00000 0.01924 0.02560 = 0.05953 -0.00248 0.00680 -0.00388 K6 6 0.500000 0.000000 0.500000 10.50000 0.01561 0.03281 = 0.01779 -0.00329 0.00953 -0.00181 B6 3 0.299931 0.512378 0.067069 11.00000 0.01218 0.01510 = 0.00793 -0.00037 0.00256 -0.00043 C61 1 0.469918 0.047783 0.410937 11.00000 0.01314 0.02200 = 0.01764 0.00071 0.00725 -0.00016 N6 4 0.265214 -0.258530 0.317564 11.00000 0.01875 0.02669 = 0.01711 -0.00147 0.00729 -0.00654 K7 6 0.500000 0.541779 0.250000 10.50000 0.01489 0.03205 = 0.01485 0.00000 0.00728 0.00000 C7X 1 0.444511 0.177700 0.355251 11.00000 0.01270 0.02905 = 0.01808 0.00202 0.00701 -0.00224 N7 4 0.264918 0.273954 0.325180 11.00000 0.03320 0.03134 = 0.02476 0.00291 0.01018 0.01612 C7 1 0.441540 1.024924 0.271880 11.00000 0.11111 0.03900 = 0.09653 0.00022 0.03623 0.01865 AFIX 23 H7A 2 0.431063 1.115698 0.257581 11.00000 -1.20000 H7B 2 0.430026 1.015486 0.286940 11.00000 -1.20000 AFIX 0 H9 2 0.284934 -0.058810 0.122429 11.00000 0.08827 C9 1 0.403368 -0.046919 0.466887 11.00000 0.01497 0.01565 = 0.01027 -0.00130 0.00601 -0.00181 N9 4 0.345688 0.289265 0.453862 11.00000 0.02755 0.02664 = 0.02734 0.00118 0.01123 0.00869 H8 2 0.310282 0.032792 0.138456 11.00000 0.03252 C8 1 0.448084 -0.127432 0.359718 11.00000 0.01599 0.03028 = 0.01736 -0.00267 0.00674 0.00230 N8 4 0.318010 -0.225609 0.438839 11.00000 0.02569 0.03219 = 0.02714 -0.00021 0.01206 -0.01206 H10 2 0.217069 -0.061394 0.124743 11.00000 0.05377 N10 4 0.429833 -0.082106 0.486648 11.00000 0.01830 0.02404 = 0.01412 0.00053 0.00298 0.00069 C10 1 0.353981 0.167291 0.448443 11.00000 0.01362 0.02298 = 0.01110 0.00254 0.00409 0.00228 N12 4 0.430088 0.438290 0.237171 11.00000 0.02067 0.02657 = 0.01655 -0.00084 0.00541 0.00086 C12 1 0.302856 0.026991 0.283563 11.00000 0.01494 0.01175 = 0.01370 0.00030 0.00291 -0.00009 N13 4 0.345201 0.798734 0.201998 11.00000 0.02572 0.02417 = 0.02446 0.00037 0.01094 0.00688 C13 1 0.279254 -0.143824 0.316823 11.00000 0.01109 0.02220 = 0.00973 -0.00090 0.00374 -0.00080 N14 4 0.316872 0.285989 0.189853 11.00000 0.02807 0.02780 = 0.02803 -0.00324 0.01590 -0.01061 C14 1 0.278587 0.164862 0.320716 11.00000 0.01570 0.02131 = 0.01090 0.00222 0.00207 0.00473 N15 4 0.489561 0.468625 0.186781 11.00000 0.01464 0.04353 = 0.01800 -0.00184 0.00469 -0.00183 C15 1 0.367494 0.504012 0.155691 11.00000 0.00933 0.01064 = 0.00838 0.00038 0.00325 -0.00017 N16 4 0.451215 0.741577 0.094430 11.00000 0.02702 0.03207 = 0.03453 0.00773 0.01745 -0.00024 C16 1 0.337476 0.506463 0.127708 11.00000 0.00787 0.01070 = 0.01205 0.00043 0.00472 0.00036 N17 4 0.443895 0.216774 0.092696 11.00000 0.02789 0.03306 = 0.03528 -0.01148 0.01529 0.00319 C17 1 0.337396 0.505128 0.097576 11.00000 0.01063 0.00732 = 0.00973 -0.00009 0.00228 0.00034 N18 4 0.301731 0.516852 0.008553 11.00000 0.02912 0.02987 = 0.01520 -0.00126 0.00836 -0.00824 C18 1 0.371185 0.499633 0.098377 11.00000 0.01318 0.01116 = 0.00734 -0.00101 0.00524 -0.00055 N19 4 0.262294 0.246900 0.068251 11.00000 0.01865 0.02334 = 0.01812 -0.00016 0.00751 -0.00563 C19 1 0.401835 0.495048 0.125968 11.00000 0.01047 0.01019 = 0.01042 -0.00049 0.00460 0.00036 N20 4 0.267765 0.783331 0.074793 11.00000 0.02997 0.02906 = 0.03008 0.00052 0.00670 0.01443 C20 1 0.403100 0.465620 0.217203 11.00000 0.01416 0.01835 = 0.01080 -0.00135 0.00553 -0.00072 C21 1 0.353473 0.675568 0.197092 11.00000 0.01383 0.02103 = 0.01259 0.00154 0.00647 0.00084 C35 1 0.349227 0.139856 0.024713 11.00000 0.03632 0.02121 = 0.02399 -0.00200 0.00611 -0.00372 AFIX 23 H02E 2 0.353084 0.206204 0.008685 11.00000 -1.20000 H02F 2 0.357889 0.198261 0.045061 11.00000 -1.20000 AFIX 0 C36 1 0.310301 0.101199 0.013973 11.00000 0.03106 0.03208 = 0.03717 -0.00282 0.01268 0.00797 AFIX 23 H02M 2 0.295665 0.168788 -0.004117 11.00000 -1.20000 H02N 2 0.302510 0.115906 0.031493 11.00000 -1.20000 AFIX 0 C37 1 0.307746 -0.071381 0.004133 11.00000 0.02242 0.03143 = 0.03577 -0.00131 0.01025 -0.00108 AFIX 23 H02G 2 0.288526 -0.126245 0.007760 11.00000 -1.20000 H02H 2 0.303724 -0.082063 -0.018463 11.00000 -1.20000 AFIX 0 C38 1 0.343751 -0.134908 0.025780 11.00000 0.02293 0.02268 = 0.02873 -0.00017 0.00725 -0.00066 AFIX 23 H02A 2 0.344204 -0.163234 0.046790 11.00000 -1.20000 H02B 2 0.349899 -0.229613 0.016412 11.00000 -1.20000 AFIX 0 C39 1 0.493468 0.879527 0.295161 11.00000 0.04290 0.05193 = 0.04917 -0.02574 0.02239 -0.02486 AFIX 23 H02Z 2 0.516303 0.871079 0.293002 11.00000 -1.20000 H010 2 0.497143 0.847296 0.316926 11.00000 -1.20000 AFIX 0 C40 1 0.479864 1.044296 0.288833 11.00000 0.11258 0.04152 = 0.11108 -0.03129 0.07035 -0.03297 AFIX 23 H098 2 0.485695 1.103181 0.308889 11.00000 -1.20000 H099 2 0.489922 1.101315 0.275611 11.00000 -1.20000 AFIX 0 C42 1 0.437448 0.874905 0.253285 11.00000 0.05554 0.04508 = 0.04574 0.00953 0.01407 0.02023 AFIX 23 H121 2 0.415001 0.821033 0.250170 11.00000 -1.20000 H122 2 0.437668 0.897126 0.232268 11.00000 -1.20000 AFIX 0 C43 1 0.503147 -0.351106 0.454318 11.00000 0.03630 0.03604 = 0.04279 -0.01482 0.01754 -0.01493 AFIX 23 H02S 2 0.499121 -0.312603 0.432840 11.00000 -1.20000 H02T 2 0.480417 -0.347335 0.456758 11.00000 -1.20000 AFIX 0 C44 1 0.517329 -0.517418 0.458925 11.00000 0.08319 0.03120 = 0.07513 -0.01279 0.03910 -0.01303 AFIX 23 H013 2 0.506014 -0.582561 0.470089 11.00000 -1.20000 H014 2 0.513027 -0.567413 0.438262 11.00000 -1.20000 AFIX 0 C45 1 0.555438 -0.500867 0.478182 11.00000 0.08553 0.03465 = 0.07823 0.00797 0.02600 0.01469 AFIX 23 H011 2 0.568667 -0.484398 0.464668 11.00000 -1.20000 H012 2 0.565007 -0.595033 0.491722 11.00000 -1.20000 AFIX 0 C46 1 0.557121 -0.356044 0.497943 11.00000 0.05326 0.03505 = 0.04469 0.01041 0.00471 0.00798 AFIX 23 H02W 2 0.553609 -0.385350 0.517276 11.00000 -1.20000 H02X 2 0.580329 -0.302814 0.504347 11.00000 -1.20000 AFIX 0 O47 5 0.290549 0.015347 0.135817 11.00000 0.02006 0.02967 = 0.01617 -0.00219 0.00557 0.00525 O48 5 0.210261 0.005483 0.114457 11.00000 0.02522 0.03965 = 0.01556 0.00268 0.00670 -0.00903 O49 5 0.367372 0.537202 0.279492 11.00000 0.01850 0.02300 = 0.05605 0.00351 0.00724 0.00230 C50 1 0.344402 0.669917 0.275381 11.00000 0.02408 0.01811 = 0.02522 0.00229 0.00864 0.00053 AFIX 23 H01A 2 0.351329 0.758797 0.265098 11.00000 -1.20000 H01B 2 0.345146 0.706236 0.296068 11.00000 -1.20000 AFIX 0 C51 1 0.308065 0.610460 0.254522 11.00000 0.02039 0.02505 = 0.03051 0.00398 0.00955 0.00375 AFIX 23 H02C 2 0.304088 0.613424 0.231852 11.00000 -1.20000 H02D 2 0.289413 0.672990 0.257577 11.00000 -1.20000 AFIX 0 C52 1 0.309022 0.441144 0.266113 11.00000 0.02898 0.02580 = 0.04497 0.00321 0.01130 -0.00657 AFIX 23 H02O 2 0.301881 0.436334 0.284186 11.00000 -1.20000 H02P 2 0.293224 0.371900 0.248895 11.00000 -1.20000 AFIX 0 C53 1 0.347319 0.393572 0.276232 11.00000 0.03055 0.01891 = 0.02662 0.00066 0.00255 0.00061 AFIX 23 H01C 2 0.355758 0.336070 0.296675 11.00000 -1.20000 H01D 2 0.349998 0.323678 0.260100 11.00000 -1.20000 AFIX 0 C22 1 0.337532 0.377638 0.190880 11.00000 0.01774 0.01878 = 0.01257 -0.00103 0.00721 -0.00194 C24 1 0.277205 0.359121 0.067438 11.00000 0.01011 0.02214 = 0.00883 -0.00136 0.00199 0.00039 C23 1 0.279906 0.669322 0.070477 11.00000 0.01422 0.02118 = 0.01274 0.00125 0.00013 0.00304 C26 1 0.469490 0.474720 0.160861 11.00000 0.01255 0.02241 = 0.01760 -0.00242 0.00743 -0.00137 C25 1 0.302206 0.516002 0.033479 11.00000 0.01284 0.01853 = 0.01178 0.00032 0.00183 -0.00432 C27 1 0.447812 0.633536 0.107821 11.00000 0.01318 0.02331 = 0.01888 -0.00078 0.00900 -0.00007 C28 1 0.443416 0.328336 0.106708 11.00000 0.01226 0.02404 = 0.01731 -0.00158 0.00670 0.00103 C29 1 0.612082 0.073368 0.334108 11.00000 0.03357 0.02974 = 0.02668 -0.00184 0.00632 0.00235 AFIX 23 H02K 2 0.617449 0.021751 0.317269 11.00000 -1.20000 H02L 2 0.597765 0.169266 0.325158 11.00000 -1.20000 AFIX 0 C30 1 0.592292 -0.038806 0.346606 11.00000 0.03513 0.06236 = 0.04618 0.00098 0.00435 -0.01640 AFIX 23 H02U 2 0.570589 0.011591 0.346460 11.00000 -1.20000 H02V 2 0.585619 -0.136387 0.333647 11.00000 -1.20000 AFIX 0 C31 1 0.617925 -0.075449 0.380082 11.00000 0.04712 0.03592 = 0.04195 0.00503 0.01816 -0.01203 AFIX 23 H02Q 2 0.605398 -0.090884 0.394211 11.00000 -1.20000 H02R 2 0.632027 -0.171180 0.380776 11.00000 -1.20000 AFIX 0 C32 1 0.640580 0.067838 0.389082 11.00000 0.03833 0.02898 = 0.02850 -0.00251 0.01947 -0.00334 AFIX 23 H02I 2 0.629188 0.152786 0.396429 11.00000 -1.20000 H02J 2 0.663921 0.043483 0.406192 11.00000 -1.20000 AFIX 0 N11 4 0.399504 0.498572 0.154312 11.00000 0.00930 0.01239 = 0.00921 0.00012 0.00356 -0.00004 C11 1 0.338079 -0.130750 0.439948 11.00000 0.01557 0.02504 = 0.01016 0.00075 0.00481 -0.00466 H11 2 0.190200 0.019853 0.113151 11.00000 0.06901 HKLF 4 REM test_a.res in C2/c REM R1 = 0.0457 for 11477 Fo > 4sig(Fo) and 0.0608 for all 15069 data REM 944 parameters refined using 33 restraints END WGHT 0.0722 18.6894 REM Highest difference peak 1.075, deepest hole -0.505, 1-sigma level 0.084 Q1 1 0.5000 0.4564 0.2500 10.50000 0.05 1.07 Q2 1 0.4512 1.0372 0.2538 11.00000 0.05 1.01 Q3 1 0.5482 -0.5081 0.4964 11.00000 0.05 0.86 Q4 1 0.4389 0.4574 0.2998 11.00000 0.05 0.83 Q5 1 0.4386 0.0585 0.0510 11.00000 0.05 0.83 Q6 1 0.3501 0.5152 0.3882 11.00000 0.05 0.75 Q7 1 0.4289 0.0648 0.4330 11.00000 0.05 0.69 Q8 1 0.4295 0.5583 0.1823 11.00000 0.05 0.67 Q9 1 0.2718 0.0662 0.3854 11.00000 0.05 0.55 Q10 1 0.4721 1.2478 0.2706 11.00000 0.05 0.54 Q11 1 0.3392 0.0066 0.3623 11.00000 0.05 0.54 Q12 1 0.3391 0.5097 0.1129 11.00000 0.05 0.52 Q13 1 0.4300 0.5961 0.2372 11.00000 0.05 0.50 Q14 1 0.3998 0.0053 0.3892 11.00000 0.05 0.48 Q15 1 0.3661 0.5051 0.1746 11.00000 0.05 0.48 Q16 1 0.3996 0.4980 0.1400 11.00000 0.05 0.47 Q17 1 0.4182 0.0169 0.3749 11.00000 0.05 0.46 Q18 1 0.3651 0.0067 0.4227 11.00000 0.05 0.46 Q19 1 0.4189 0.4963 0.1243 11.00000 0.05 0.45 Q20 1 0.3886 0.0119 0.3643 11.00000 0.05 0.45 Q21 1 0.3802 0.5015 0.1544 11.00000 0.05 0.45 Q22 1 0.6446 -0.1064 0.3574 11.00000 0.05 0.45 Q23 1 0.3176 0.2242 0.4413 11.00000 0.05 0.45 Q24 1 0.3583 -0.0092 0.3494 11.00000 0.05 0.44 Q25 1 0.3468 0.2240 0.2062 11.00000 0.05 0.44 Q26 1 0.3808 0.0095 0.4040 11.00000 0.05 0.44 Q27 1 0.3202 0.7380 0.1902 11.00000 0.05 0.44 Q28 1 0.4903 -0.0389 0.4352 11.00000 0.05 0.43 Q29 1 0.3095 -0.0584 0.0230 11.00000 0.05 0.43 Q30 1 0.3882 0.5150 0.1141 11.00000 0.05 0.42 Q31 1 0.3195 0.0196 0.3326 11.00000 0.05 0.42 Q32 1 0.2301 0.0710 0.3669 11.00000 0.05 0.42 Q33 1 0.5881 0.0601 0.3476 11.00000 0.05 0.40 Q34 1 0.5342 -0.7237 0.4772 11.00000 0.05 0.39 Q35 1 0.4991 1.1438 0.2981 11.00000 0.05 0.39 Q36 1 0.4309 0.0752 0.4865 11.00000 0.05 0.38 Q37 1 0.6108 -0.0458 0.3325 11.00000 0.05 0.38 Q38 1 0.4899 0.5711 0.1859 11.00000 0.05 0.38 Q39 1 0.6119 0.0216 0.3847 11.00000 0.05 0.38 Q40 1 0.6479 -0.0027 0.3610 11.00000 0.05 0.38 ; _shelx_res_checksum 88063 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.28895(2) -0.00198(4) 0.19554(2) 0.01193(10) Uani 1 1 d . . . . . C1 C 0.40226(5) 0.0228(2) 0.37615(5) 0.0106(4) Uani 1 1 d . . . . . B1 B 0.44118(6) 0.0304(3) 0.37554(5) 0.0137(4) Uani 1 1 d . . . . . N1 N 0.39986(4) 0.01588(18) 0.40437(4) 0.0106(3) Uani 1 1 d . . . . . F1 F 0.30572(3) 0.00288(14) 0.37967(3) 0.0174(3) Uani 1 1 d . . . . . O1 O 0.46716(4) 0.77997(19) 0.27207(4) 0.0314(4) Uani 1 1 d . . . . . K2 K 0.28897(2) 0.50889(4) -0.05457(2) 0.01187(10) Uani 1 1 d . . . . . C2 C 0.37165(5) 0.0203(2) 0.34835(4) 0.0107(4) Uani 1 1 d . . . . . B2 B 0.36580(6) -0.0003(2) 0.43997(5) 0.0106(4) Uani 1 1 d . . . . . N2 N 0.49003(5) 0.0619(2) 0.43669(4) 0.0252(4) Uani 1 1 d . . . . . F2 F 0.37559(3) 0.02384(14) 0.32054(3) 0.0162(3) Uani 1 1 d . . . . . O2 O 0.52919(4) -0.25457(18) 0.47810(4) 0.0292(4) Uani 1 1 d . . . . . K3 K 0.43870(2) 0.53626(5) 0.30025(2) 0.01710(11) Uani 1 1 d . . . . . O6 O 0.24844(2) 0.23278(4) 0.37543(2) 0.024(6) Uani 0.089(6) 1 d D . P . . H201 H 0.23376(2) 0.14905(4) 0.36934(4) 0.029 Uiso 0.089(6) 1 d D U P . . H200 H 0.27106(2) 0.22249(9) 0.38942(2) 0.029 Uiso 0.089(6) 1 d D U P . . B3 B 0.30036(6) 0.0158(2) 0.31707(5) 0.0117(4) Uani 1 1 d . . . . . C3X C 0.33789(5) 0.0141(2) 0.34761(5) 0.0104(4) Uani 1 1 d . . . . . N3 N 0.44586(5) 0.2834(3) 0.34029(5) 0.0330(5) Uani 1 1 d . . . . . F3 F 0.30535(3) 0.51082(13) 0.12982(3) 0.0165(3) Uani 1 1 d . . . . . K4 K 0.24926(2) 0.27861(5) 0.12526(2) 0.01769(11) Uani 1 1 d . . . . . C41 C 0.33802(5) 0.0082(2) 0.37772(5) 0.0096(4) Uani 1 1 d . . . . . B4 B 0.44067(6) 0.4833(2) 0.12540(5) 0.0116(4) Uani 1 1 d . . . . . N4 N 0.45093(6) -0.2397(3) 0.34737(5) 0.0375(5) Uani 1 1 d . . . . . O3 O 0.35585(5) 0.6136(3) 0.39158(5) 0.0307(5) Uani 0.8 1 d . . P A 3 C3 C 0.36027(10) 0.5838(4) 0.36309(8) 0.0309(7) Uani 0.8 1 d . U P A 3 H3A H 0.3722 0.6739 0.3578 0.037 Uiso 0.8 1 calc R U P A 3 H3B H 0.3371 0.5657 0.3452 0.037 Uiso 0.8 1 calc R U P A 3 C4 C 0.38238(12) 0.4405(5) 0.36965(9) 0.0496(10) Uani 0.8 1 d . U P A 3 H4A H 0.3953 0.4342 0.3556 0.060 Uiso 0.8 1 calc R U P A 3 H4B H 0.3680 0.3437 0.3669 0.060 Uiso 0.8 1 calc R U P A 3 C5 C 0.40763(11) 0.4630(5) 0.40394(10) 0.0499(10) Uani 0.8 1 d . U P A 3 H5A H 0.4301 0.5112 0.4054 0.060 Uiso 0.8 1 calc R U P A 3 H5B H 0.4129 0.3607 0.4154 0.060 Uiso 0.8 1 calc R U P A 3 C6 C 0.38815(10) 0.5728(4) 0.41738(9) 0.0308(8) Uani 0.8 1 d . U P A 3 H6A H 0.3833 0.5190 0.4343 0.037 Uiso 0.8 1 calc R U P A 3 H6B H 0.4024 0.6688 0.4264 0.037 Uiso 0.8 1 calc R U P A 3 O3B O 0.3549(3) 0.4293(16) 0.3893(3) 0.022(3) Uani 0.12 1 d . U P B 4 C3B C 0.3554(3) 0.4770(19) 0.3600(3) 0.028(3) Uani 0.2 1 d . . P B 4 H3B1 H 0.3337 0.5376 0.3476 0.034 Uiso 0.2 1 calc R U P B 4 H3B2 H 0.3560 0.3827 0.3475 0.034 Uiso 0.2 1 calc R U P B 4 C4B C 0.3886(4) 0.479(3) 0.4146(4) 0.052(5) Uani 0.2 1 d . . P B 4 H4AB H 0.3841 0.5538 0.4290 0.063 Uiso 0.2 1 calc R U P B 4 H4BB H 0.4012 0.3857 0.4271 0.063 Uiso 0.2 1 calc R U P B 4 C5B C 0.3868(4) 0.576(2) 0.3659(3) 0.052(5) Uani 0.2 1 d . . P B 4 H5AB H 0.3799 0.6885 0.3613 0.063 Uiso 0.2 1 calc R U P B 4 H5BB H 0.3990 0.5418 0.3524 0.063 Uiso 0.2 1 calc R U P B 4 C6B C 0.4100(3) 0.5547(16) 0.3999(3) 0.034(3) Uani 0.2 1 d . . P B 4 H6AB H 0.4306 0.4874 0.4023 0.040 Uiso 0.2 1 calc R U P B 4 H6BB H 0.4189 0.6583 0.4100 0.040 Uiso 0.2 1 calc R U P B 4 O4 O 0.64435(4) 0.1144(2) 0.36068(4) 0.0311(4) Uani 1 1 d . . . . . F4 F 0.37500(3) 0.49774(13) 0.07041(3) 0.0160(3) Uani 1 1 d . . . . . K5 K 0.43873(2) -0.02114(5) 0.04993(2) 0.01618(11) Uani 1 1 d . . . . . C5X C 0.36792(5) 0.0078(2) 0.40572(5) 0.0105(4) Uani 1 1 d . . . . . B5 B 0.36549(6) 0.5059(2) 0.19001(5) 0.0102(4) Uani 1 1 d . . . . . N5 N 0.30260(5) 0.0317(2) 0.25869(4) 0.0216(4) Uani 1 1 d . . . . . O5 O 0.36764(5) -0.00816(19) 0.02851(5) 0.0377(5) Uani 1 1 d . . . . . K6 K 0.5000 0.0000 0.5000 0.02118(16) Uani 1 2 d S . P . . B6 B 0.29993(6) 0.5124(2) 0.06707(5) 0.0122(4) Uani 1 1 d . . . . . C61 C 0.46992(5) 0.0478(2) 0.41094(5) 0.0173(4) Uani 1 1 d . . . . . N6 N 0.26521(5) -0.2585(2) 0.31756(4) 0.0208(4) Uani 1 1 d . . . . . K7 K 0.5000 0.54178(8) 0.2500 0.02018(15) Uani 1 2 d S T P . . C7X C 0.44451(5) 0.1777(3) 0.35525(5) 0.0197(4) Uani 1 1 d . . . . . N7 N 0.26492(5) 0.2740(2) 0.32518(5) 0.0302(5) Uani 1 1 d . . . . . C7 C 0.44154(14) 1.0249(4) 0.27188(11) 0.0840(14) Uani 1 1 d . . . . . H7A H 0.4311 1.1157 0.2576 0.101 Uiso 1 1 calc R U . . . H7B H 0.4300 1.0155 0.2869 0.101 Uiso 1 1 calc R U . . . H9 H 0.2849(11) -0.059(5) 0.1224(10) 0.088(14) Uiso 1 1 d . . . . . C9 C 0.40337(5) -0.0469(2) 0.46689(4) 0.0133(4) Uani 1 1 d . . . . . N9 N 0.34569(5) 0.2893(2) 0.45386(5) 0.0271(4) Uani 1 1 d . . . . . H8 H 0.3103(9) 0.033(3) 0.1385(7) 0.033(8) Uiso 1 1 d . . . . . C8 C 0.44808(5) -0.1274(3) 0.35972(5) 0.0212(4) Uani 1 1 d . . . . . N8 N 0.31801(5) -0.2256(2) 0.43884(4) 0.0279(4) Uani 1 1 d . . . . . H10 H 0.2171(9) -0.061(4) 0.1247(8) 0.054(12) Uiso 1 1 d . . . . . N10 N 0.42983(5) -0.0821(2) 0.48665(4) 0.0200(4) Uani 1 1 d . . . . . C10 C 0.35398(5) 0.1673(2) 0.44844(4) 0.0162(4) Uani 1 1 d . . . . . N12 N 0.43009(5) 0.4383(2) 0.23717(4) 0.0219(4) Uani 1 1 d . . . . . C12 C 0.30286(5) 0.0270(2) 0.28356(5) 0.0144(4) Uani 1 1 d . . . . . N13 N 0.34520(5) 0.7987(2) 0.20200(4) 0.0245(4) Uani 1 1 d . . . . . C13 C 0.27925(5) -0.1438(2) 0.31682(4) 0.0145(4) Uani 1 1 d . . . . . N14 N 0.31687(5) 0.2860(2) 0.18985(4) 0.0265(4) Uani 1 1 d . . . . . C14 C 0.27859(5) 0.1649(2) 0.32072(4) 0.0170(4) Uani 1 1 d . . . . . N15 N 0.48956(5) 0.4686(2) 0.18678(5) 0.0260(4) Uani 1 1 d . . . . . C15 C 0.36749(5) 0.5040(2) 0.15569(5) 0.0096(4) Uani 1 1 d . . . . . N16 N 0.45121(5) 0.7416(2) 0.09443(5) 0.0296(4) Uani 1 1 d . . . . . C16 C 0.33748(5) 0.5065(2) 0.12771(5) 0.0100(4) Uani 1 1 d . . . . . N17 N 0.44389(5) 0.2168(2) 0.09270(5) 0.0313(5) Uani 1 1 d . . . . . C17 C 0.33740(5) 0.5051(2) 0.09758(5) 0.0098(4) Uani 1 1 d . . . . . N18 N 0.30173(5) 0.5169(2) 0.00855(4) 0.0249(4) Uani 1 1 d . . . . . C18 C 0.37118(5) 0.4996(2) 0.09838(5) 0.0102(4) Uani 1 1 d . . . . . N19 N 0.26229(5) 0.2469(2) 0.06825(4) 0.0200(4) Uani 1 1 d . . . . . C19 C 0.40183(5) 0.4950(2) 0.12597(5) 0.0102(4) Uani 1 1 d . . . . . N20 N 0.26776(5) 0.7833(2) 0.07479(5) 0.0314(5) Uani 1 1 d . . . . . C20 C 0.40310(5) 0.4656(2) 0.21720(5) 0.0143(4) Uani 1 1 d . . . . . C21 C 0.35347(5) 0.6756(2) 0.19709(4) 0.0155(4) Uani 1 1 d . . . . . C35 C 0.34923(6) 0.1399(3) 0.02471(6) 0.0291(5) Uani 1 1 d . . . . . H02E H 0.3531 0.2062 0.0087 0.035 Uiso 1 1 calc R U . . . H02F H 0.3579 0.1983 0.0451 0.035 Uiso 1 1 calc R U . . . C36 C 0.31030(7) 0.1012(3) 0.01397(6) 0.0338(6) Uani 1 1 d . . . . . H02M H 0.2957 0.1688 -0.0041 0.041 Uiso 1 1 calc R U . . . H02N H 0.3025 0.1159 0.0315 0.041 Uiso 1 1 calc R U . . . C37 C 0.30775(6) -0.0714(3) 0.00413(6) 0.0303(5) Uani 1 1 d . . . . . H02G H 0.2885 -0.1262 0.0078 0.036 Uiso 1 1 calc R U . . . H02H H 0.3037 -0.0821 -0.0185 0.036 Uiso 1 1 calc R U . . . C38 C 0.34375(6) -0.1349(3) 0.02578(6) 0.0258(5) Uani 1 1 d . . . . . H02A H 0.3442 -0.1632 0.0468 0.031 Uiso 1 1 calc R U . . . H02B H 0.3499 -0.2296 0.0164 0.031 Uiso 1 1 calc R U . . . C39 C 0.49347(8) 0.8795(3) 0.29516(7) 0.0468(7) Uani 1 1 d . . . . . H02Z H 0.5163 0.8711 0.2930 0.056 Uiso 1 1 calc R U . . . H010 H 0.4971 0.8473 0.3169 0.056 Uiso 1 1 calc R U . . . C40 C 0.47986(12) 1.0443(4) 0.28883(11) 0.0803(13) Uani 1 1 d . . . . . H098 H 0.4857 1.1032 0.3089 0.096 Uiso 1 1 calc R U . . . H099 H 0.4899 1.1013 0.2756 0.096 Uiso 1 1 calc R U . . . C42 C 0.43745(9) 0.8749(4) 0.25328(7) 0.0508(8) Uani 1 1 d . . . . . H121 H 0.4150 0.8210 0.2502 0.061 Uiso 1 1 calc R U . . . H122 H 0.4377 0.8971 0.2323 0.061 Uiso 1 1 calc R U . . . C43 C 0.50315(7) -0.3511(3) 0.45432(6) 0.0379(6) Uani 1 1 d . . . . . H02S H 0.4991 -0.3126 0.4328 0.045 Uiso 1 1 calc R U . . . H02T H 0.4804 -0.3473 0.4568 0.045 Uiso 1 1 calc R U . . . C44 C 0.51733(11) -0.5174(4) 0.45893(10) 0.0609(10) Uani 1 1 d . . . . . H013 H 0.5060 -0.5826 0.4701 0.073 Uiso 1 1 calc R U . . . H014 H 0.5130 -0.5674 0.4383 0.073 Uiso 1 1 calc R U . . . C45 C 0.55544(12) -0.5009(4) 0.47818(10) 0.0684(11) Uani 1 1 d . . . . . H011 H 0.5687 -0.4844 0.4647 0.082 Uiso 1 1 calc R U . . . H012 H 0.5650 -0.5950 0.4917 0.082 Uiso 1 1 calc R U . . . C46 C 0.55712(8) -0.3560(3) 0.49794(7) 0.0492(7) Uani 1 1 d . . . . . H02W H 0.5536 -0.3854 0.5173 0.059 Uiso 1 1 calc R U . . . H02X H 0.5803 -0.3028 0.5043 0.059 Uiso 1 1 calc R U . . . O47 O 0.29055(5) 0.0153(2) 0.13582(4) 0.0225(4) Uani 1 1 d . . . . . O48 O 0.21026(6) 0.0055(2) 0.11446(4) 0.0273(4) Uani 1 1 d . . . . . O49 O 0.36737(4) 0.53720(19) 0.27949(5) 0.0350(4) Uani 1 1 d . . . . . C50 C 0.34440(6) 0.6699(2) 0.27538(5) 0.0229(5) Uani 1 1 d . . . . . H01A H 0.3513 0.7588 0.2651 0.027 Uiso 1 1 calc R U . . . H01B H 0.3451 0.7062 0.2961 0.027 Uiso 1 1 calc R U . . . C51 C 0.30806(6) 0.6105(3) 0.25452(6) 0.0255(5) Uani 1 1 d . . . . . H02C H 0.3041 0.6134 0.2319 0.031 Uiso 1 1 calc R U . . . H02D H 0.2894 0.6730 0.2576 0.031 Uiso 1 1 calc R U . . . C52 C 0.30902(7) 0.4411(3) 0.26611(7) 0.0344(6) Uani 1 1 d . . . . . H02O H 0.3019 0.4363 0.2842 0.041 Uiso 1 1 calc R U . . . H02P H 0.2932 0.3719 0.2489 0.041 Uiso 1 1 calc R U . . . C53 C 0.34732(6) 0.3936(3) 0.27623(6) 0.0282(5) Uani 1 1 d . . . . . H01C H 0.3558 0.3361 0.2967 0.034 Uiso 1 1 calc R U . . . H01D H 0.3500 0.3237 0.2601 0.034 Uiso 1 1 calc R U . . . C22 C 0.33753(5) 0.3776(2) 0.19088(4) 0.0160(4) Uani 1 1 d . . . . . C24 C 0.27720(5) 0.3591(2) 0.06744(4) 0.0143(4) Uani 1 1 d . . . . . C23 C 0.27991(5) 0.6693(2) 0.07048(5) 0.0177(4) Uani 1 1 d . . . . . C26 C 0.46949(6) 0.4747(2) 0.16086(5) 0.0171(4) Uani 1 1 d . . . . . C25 C 0.30221(6) 0.5160(2) 0.03348(5) 0.0154(4) Uani 1 1 d . . . . . C27 C 0.44781(5) 0.6335(2) 0.10782(5) 0.0176(4) Uani 1 1 d . . . . . C28 C 0.44342(5) 0.3283(2) 0.10671(5) 0.0176(4) Uani 1 1 d . . . . . C29 C 0.61208(7) 0.0734(3) 0.33411(6) 0.0319(5) Uani 1 1 d . . . . . H02K H 0.6174 0.0218 0.3173 0.038 Uiso 1 1 calc R U . . . H02L H 0.5978 0.1693 0.3252 0.038 Uiso 1 1 calc R U . . . C30 C 0.59229(8) -0.0388(4) 0.34661(8) 0.0518(8) Uani 1 1 d . . . . . H02U H 0.5706 0.0116 0.3465 0.062 Uiso 1 1 calc R U . . . H02V H 0.5856 -0.1364 0.3336 0.062 Uiso 1 1 calc R U . . . C31 C 0.61792(8) -0.0754(3) 0.38008(7) 0.0416(7) Uani 1 1 d . . . . . H02Q H 0.6054 -0.0909 0.3942 0.050 Uiso 1 1 calc R U . . . H02R H 0.6320 -0.1712 0.3808 0.050 Uiso 1 1 calc R U . . . C32 C 0.64058(7) 0.0678(3) 0.38908(6) 0.0300(5) Uani 1 1 d . . . . . H02I H 0.6292 0.1528 0.3964 0.036 Uiso 1 1 calc R U . . . H02J H 0.6639 0.0435 0.4062 0.036 Uiso 1 1 calc R U . . . N11 N 0.39950(4) 0.49857(17) 0.15431(4) 0.0104(3) Uani 1 1 d . . . . . C11 C 0.33808(5) -0.1307(2) 0.43995(4) 0.0170(4) Uani 1 1 d . . . . . H11 H 0.1902(11) 0.020(4) 0.1132(9) 0.069(13) Uiso 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 K1 0.0127(2) 0.0121(2) 0.0111(2) -0.00017(14) 0.00506(19) -0.00056(14) C1 0.0107(10) 0.0108(8) 0.0105(10) 0.0007(7) 0.0045(8) 0.0003(7) B1 0.0097(11) 0.0192(11) 0.0113(11) 0.0011(8) 0.0033(10) 0.0007(8) N1 0.0091(8) 0.0129(8) 0.0094(8) 0.0007(6) 0.0034(7) -0.0009(6) F1 0.0095(6) 0.0289(7) 0.0135(6) 0.0009(4) 0.0044(5) -0.0008(4) O1 0.0294(9) 0.0270(9) 0.0334(9) -0.0058(7) 0.0080(8) -0.0025(7) K2 0.0128(2) 0.0124(2) 0.0103(2) -0.00006(14) 0.00446(19) 0.00043(14) C2 0.0141(10) 0.0115(9) 0.0073(9) 0.0012(7) 0.0053(8) -0.0003(7) B2 0.0084(11) 0.0152(10) 0.0066(11) 0.0005(7) 0.0013(9) -0.0024(8) N2 0.0161(10) 0.0379(11) 0.0187(10) 0.0004(8) 0.0041(8) -0.0003(8) F2 0.0135(6) 0.0282(6) 0.0078(6) 0.0002(4) 0.0052(5) -0.0010(5) O2 0.0288(9) 0.0244(8) 0.0300(9) -0.0040(7) 0.0073(7) -0.0029(7) K3 0.0152(2) 0.0221(2) 0.0139(2) 0.00006(17) 0.00565(19) -0.00006(17) O6 0.025(10) 0.017(9) 0.015(9) -0.005(6) -0.007(7) 0.001(7) B3 0.0104(11) 0.0127(10) 0.0103(11) 0.0005(8) 0.0025(9) 0.0007(8) C3X 0.0100(10) 0.0089(8) 0.0101(10) 0.0012(6) 0.0019(8) 0.0006(7) N3 0.0279(11) 0.0408(12) 0.0326(11) 0.0121(10) 0.0146(9) -0.0032(9) F3 0.0083(6) 0.0282(6) 0.0128(6) 0.0001(4) 0.0039(5) 0.0003(4) K4 0.0194(2) 0.0206(2) 0.0144(2) 0.00032(16) 0.00821(18) 0.00215(17) C41 0.0061(10) 0.0121(9) 0.0104(10) 0.0010(7) 0.0031(8) -0.0009(7) B4 0.0088(11) 0.0168(10) 0.0092(11) -0.0014(8) 0.0035(9) 0.0001(8) N4 0.0346(12) 0.0425(13) 0.0362(12) -0.0134(10) 0.0150(10) 0.0066(10) O3 0.0251(11) 0.0462(13) 0.0255(11) -0.0018(9) 0.0152(9) 0.0079(9) C3 0.038(2) 0.0302(17) 0.0295(16) 0.0059(14) 0.0191(15) 0.0072(15) C4 0.058(2) 0.047(2) 0.042(2) -0.0103(16) 0.0184(19) 0.0173(19) C5 0.039(2) 0.046(2) 0.050(2) -0.0148(19) 0.0032(18) 0.0172(19) C6 0.0317(18) 0.0315(17) 0.0296(17) -0.0013(15) 0.0126(14) -0.0003(15) O3B 0.015(4) 0.041(5) 0.016(4) 0.007(4) 0.011(4) -0.004(4) C3B 0.016(7) 0.044(8) 0.022(7) 0.003(6) 0.005(5) 0.001(6) C4B 0.031(9) 0.097(16) 0.020(8) 0.003(9) 0.000(7) 0.026(11) C5B 0.054(10) 0.070(11) 0.022(7) 0.006(7) 0.004(7) -0.041(9) C6B 0.012(6) 0.016(6) 0.054(9) 0.006(6) -0.006(6) -0.006(5) O4 0.0306(9) 0.0345(9) 0.0307(9) 0.0042(7) 0.0149(8) -0.0048(7) F4 0.0127(6) 0.0283(6) 0.0079(6) -0.0008(4) 0.0050(5) -0.0001(4) K5 0.0164(2) 0.0188(2) 0.0132(2) -0.00066(16) 0.0059(2) 0.00071(16) C5X 0.0118(10) 0.0102(9) 0.0098(10) 0.0007(6) 0.0048(9) -0.0013(7) B5 0.0094(11) 0.0129(10) 0.0078(11) -0.0003(7) 0.0028(9) -0.0002(8) N5 0.0251(11) 0.0241(9) 0.0139(10) 0.0010(7) 0.0061(8) 0.0012(8) O5 0.0192(9) 0.0256(9) 0.0595(13) -0.0025(8) 0.0068(9) -0.0039(7) K6 0.0156(4) 0.0328(4) 0.0178(4) -0.0033(3) 0.0095(3) -0.0018(3) B6 0.0122(12) 0.0151(10) 0.0079(11) -0.0004(8) 0.0026(9) -0.0004(8) C61 0.0131(10) 0.0220(10) 0.0176(11) 0.0007(8) 0.0072(9) -0.0002(8) N6 0.0188(9) 0.0267(10) 0.0171(9) -0.0015(7) 0.0073(8) -0.0065(8) K7 0.0149(3) 0.0320(4) 0.0148(3) 0.000 0.0073(3) 0.000 C7X 0.0127(10) 0.0291(11) 0.0181(10) 0.0020(9) 0.0070(9) -0.0022(8) N7 0.0332(11) 0.0313(11) 0.0248(10) 0.0029(8) 0.0102(9) 0.0161(9) C7 0.111(4) 0.0390(19) 0.097(3) 0.000(2) 0.036(3) 0.019(2) C9 0.0150(11) 0.0156(9) 0.0103(10) -0.0013(7) 0.0060(9) -0.0018(8) N9 0.0275(11) 0.0266(10) 0.0273(10) 0.0012(8) 0.0112(9) 0.0087(8) C8 0.0160(11) 0.0303(12) 0.0174(10) -0.0027(9) 0.0067(9) 0.0023(9) N8 0.0257(10) 0.0322(11) 0.0271(10) -0.0002(8) 0.0121(9) -0.0121(9) N10 0.0183(9) 0.0240(9) 0.0141(9) 0.0005(7) 0.0030(8) 0.0007(7) C10 0.0136(10) 0.0230(11) 0.0111(9) 0.0025(8) 0.0041(8) 0.0023(8) N12 0.0207(10) 0.0266(10) 0.0165(9) -0.0008(8) 0.0054(8) 0.0009(8) C12 0.0149(11) 0.0118(9) 0.0137(11) 0.0003(7) 0.0029(9) -0.0001(7) N13 0.0257(10) 0.0242(10) 0.0245(10) 0.0004(8) 0.0109(8) 0.0069(8) C13 0.0111(9) 0.0222(10) 0.0097(9) -0.0009(7) 0.0037(8) -0.0008(8) N14 0.0281(10) 0.0278(10) 0.0280(10) -0.0032(8) 0.0159(9) -0.0106(8) C14 0.0157(10) 0.0213(10) 0.0109(9) 0.0022(8) 0.0021(8) 0.0047(8) N15 0.0146(10) 0.0435(12) 0.0180(11) -0.0018(8) 0.0047(9) -0.0018(8) C15 0.0093(10) 0.0106(9) 0.0084(10) 0.0004(6) 0.0033(8) -0.0002(6) N16 0.0270(11) 0.0321(11) 0.0345(11) 0.0077(9) 0.0175(9) -0.0002(9) C16 0.0079(10) 0.0107(9) 0.0121(10) 0.0004(7) 0.0047(8) 0.0004(6) N17 0.0279(11) 0.0331(11) 0.0353(12) -0.0115(9) 0.0153(10) 0.0032(9) C17 0.0106(10) 0.0073(8) 0.0097(10) -0.0001(6) 0.0023(8) 0.0003(6) N18 0.0291(12) 0.0299(10) 0.0152(10) -0.0013(7) 0.0084(9) -0.0082(8) C18 0.0132(10) 0.0112(9) 0.0073(10) -0.0010(6) 0.0052(9) -0.0006(7) N19 0.0186(9) 0.0233(9) 0.0181(9) -0.0002(7) 0.0075(8) -0.0056(8) C19 0.0105(10) 0.0102(9) 0.0104(10) -0.0005(6) 0.0046(9) 0.0004(7) N20 0.0300(11) 0.0291(11) 0.0301(11) 0.0005(9) 0.0067(9) 0.0144(9) C20 0.0142(11) 0.0183(9) 0.0108(10) -0.0013(7) 0.0055(9) -0.0007(8) C21 0.0138(10) 0.0210(10) 0.0126(9) 0.0015(8) 0.0065(8) 0.0008(8) C35 0.0363(14) 0.0212(11) 0.0240(12) -0.0020(9) 0.0061(11) -0.0037(10) C36 0.0311(14) 0.0321(13) 0.0372(14) -0.0028(11) 0.0127(12) 0.0080(11) C37 0.0224(12) 0.0314(13) 0.0358(14) -0.0013(11) 0.0103(11) -0.0011(10) C38 0.0229(12) 0.0227(11) 0.0287(12) -0.0002(9) 0.0073(10) -0.0007(9) C39 0.0429(16) 0.0519(18) 0.0492(17) -0.0257(14) 0.0224(14) -0.0249(14) C40 0.113(4) 0.0415(19) 0.111(4) -0.031(2) 0.070(3) -0.033(2) C42 0.0555(19) 0.0451(17) 0.0457(17) 0.0095(14) 0.0141(15) 0.0202(15) C43 0.0363(15) 0.0360(14) 0.0428(15) -0.0148(12) 0.0175(13) -0.0149(12) C44 0.083(3) 0.0312(16) 0.075(3) -0.0128(15) 0.039(2) -0.0130(16) C45 0.086(3) 0.0346(17) 0.078(3) 0.0080(16) 0.026(2) 0.0147(17) C46 0.0533(19) 0.0351(15) 0.0447(17) 0.0104(13) 0.0047(15) 0.0080(13) O47 0.0201(10) 0.0297(9) 0.0162(9) -0.0022(6) 0.0056(8) 0.0052(7) O48 0.0252(11) 0.0396(11) 0.0156(9) 0.0027(7) 0.0067(8) -0.0090(8) O49 0.0185(9) 0.0230(8) 0.0561(12) 0.0035(8) 0.0072(9) 0.0023(7) C50 0.0241(12) 0.0181(10) 0.0252(11) 0.0023(9) 0.0086(10) 0.0005(9) C51 0.0204(11) 0.0251(11) 0.0305(12) 0.0040(9) 0.0095(10) 0.0037(9) C52 0.0290(14) 0.0258(12) 0.0450(16) 0.0032(11) 0.0113(12) -0.0066(10) C53 0.0305(13) 0.0189(11) 0.0266(12) 0.0007(9) 0.0025(10) 0.0006(10) C22 0.0177(10) 0.0188(10) 0.0126(10) -0.0010(8) 0.0072(8) -0.0019(8) C24 0.0101(9) 0.0221(10) 0.0088(9) -0.0014(7) 0.0020(8) 0.0004(8) C23 0.0142(10) 0.0212(10) 0.0127(10) 0.0013(8) 0.0001(8) 0.0030(8) C26 0.0125(11) 0.0224(10) 0.0176(12) -0.0024(8) 0.0074(10) -0.0014(8) C25 0.0128(11) 0.0185(10) 0.0118(11) 0.0003(7) 0.0018(9) -0.0043(7) C27 0.0132(10) 0.0233(11) 0.0189(10) -0.0008(8) 0.0090(9) -0.0001(8) C28 0.0123(10) 0.0240(11) 0.0173(10) -0.0016(8) 0.0067(8) 0.0010(8) C29 0.0336(14) 0.0297(13) 0.0267(13) -0.0018(10) 0.0063(11) 0.0023(11) C30 0.0351(17) 0.062(2) 0.0462(19) 0.0010(15) 0.0044(15) -0.0164(15) C31 0.0471(17) 0.0359(14) 0.0420(16) 0.0050(12) 0.0182(14) -0.0120(13) C32 0.0383(15) 0.0290(12) 0.0285(13) -0.0025(10) 0.0195(12) -0.0033(11) N11 0.0093(9) 0.0124(8) 0.0092(8) 0.0001(6) 0.0036(7) 0.0000(6) C11 0.0156(10) 0.0250(11) 0.0102(9) 0.0008(8) 0.0048(8) -0.0047(8) 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' K K 0.2009 0.2494 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N5 K1 N14 95.41(6) . . N5 K1 N7 103.20(6) . 4_545 N14 K1 N7 151.39(6) . 4_545 N5 K1 O47 164.92(6) . . N14 K1 O47 71.41(5) . . N7 K1 O47 91.78(6) 4_545 . N5 K1 N13 98.26(6) . 1_545 N14 K1 N13 100.46(6) . 1_545 N7 K1 N13 98.16(6) 4_545 1_545 O47 K1 N13 77.65(5) . 1_545 N5 K1 N6 87.64(5) . 4 N14 K1 N6 70.86(5) . 4 N7 K1 N6 88.22(6) 4_545 4 O47 K1 N6 94.60(5) . 4 N13 K1 N6 170.04(5) 1_545 4 N5 K1 K4 132.07(4) . . N14 K1 K4 54.65(4) . . N7 K1 K4 96.99(4) 4_545 . O47 K1 K4 45.61(3) . . N13 K1 K4 121.43(4) 1_545 . N6 K1 K4 49.75(3) 4 . N1 C1 C2 119.72(17) . . N1 C1 B1 118.63(17) . . C2 C1 B1 121.64(17) . . C61 B1 C7X 108.88(17) . . C61 B1 C8 110.35(17) . . C7X B1 C8 108.09(17) . . C61 B1 C1 108.73(16) . . C7X B1 C1 111.19(16) . . C8 B1 C1 109.59(16) . . C1 N1 C5X 120.15(17) . . C41 F1 K4 140.18(10) . 4_545 C42 O1 C39 109.0(2) . . C42 O1 K7 126.85(15) . . C39 O1 K7 110.55(15) . . C42 O1 K3 105.31(16) . . C39 O1 K3 113.65(15) . . K7 O1 K3 89.72(5) . . N18 K2 N8 103.47(6) . 6 N18 K2 N20 96.65(6) . 7_565 N8 K2 N20 149.56(6) 6 7_565 N18 K2 O48 169.21(7) . 7 N8 K2 O48 70.83(6) 6 7 N20 K2 O48 92.33(7) 7_565 7 N18 K2 N9 92.63(6) . 6_565 N8 K2 N9 99.71(6) 6 6_565 N20 K2 N9 101.97(6) 7_565 6_565 O48 K2 N9 79.63(5) 7 6_565 N18 K2 N19 93.43(5) . 7 N8 K2 N19 68.95(5) 6 7 N20 K2 N19 87.45(6) 7_565 7 O48 K2 N19 92.93(5) 7 7 N9 K2 N19 168.14(5) 6_565 7 N18 K2 K4 138.62(4) . 7 N8 K2 K4 53.55(4) 6 7 N20 K2 K4 96.48(4) 7_565 7 O48 K2 K4 45.35(4) 7 7 N9 K2 K4 122.48(4) 6_565 7 N19 K2 K4 48.29(3) 7 7 F2 C2 C3X 118.83(17) . . F2 C2 C1 117.34(17) . . C3X C2 C1 123.83(17) . . C11 B2 C9 107.68(16) . . C11 B2 C10 108.92(16) . . C9 B2 C10 109.02(16) . . C11 B2 C5X 110.59(16) . . C9 B2 C5X 110.52(16) . . C10 B2 C5X 110.05(15) . . C61 N2 K6 142.32(16) . . C61 N2 K5 116.96(15) . 2_655 K6 N2 K5 91.33(5) . 2_655 C46 O2 C43 108.0(2) . . C46 O2 K6 125.05(15) . . C43 O2 K6 113.92(14) . . C46 O2 K5 106.97(16) . 2_655 C43 O2 K5 112.08(14) . 2_655 K6 O2 K5 88.78(4) . 2_655 O49 K3 N3 92.66(6) . . O49 K3 N4 95.94(6) . 1_565 N3 K3 N4 93.96(7) . 1_565 O49 K3 N15 166.31(6) . 2_655 N3 K3 N15 83.21(6) . 2_655 N4 K3 N15 97.36(6) 1_565 2_655 O49 K3 N12 88.32(6) . . N3 K3 N12 112.65(6) . . N4 K3 N12 152.86(6) 1_565 . N15 K3 N12 81.32(5) 2_655 . O49 K3 O1 114.61(5) . . N3 K3 O1 152.73(5) . . N4 K3 O1 83.53(6) 1_565 . N15 K3 O1 70.27(5) 2_655 . N12 K3 O1 70.43(5) . . O49 K3 C26 167.58(5) . 2_655 N3 K3 C26 75.06(5) . 2_655 N4 K3 C26 83.31(6) 1_565 2_655 N15 K3 C26 16.79(5) 2_655 2_655 N12 K3 C26 98.02(5) . 2_655 O1 K3 C26 77.68(5) . 2_655 O49 K3 K7 129.68(4) . . N3 K3 K7 117.80(5) . . N4 K3 K7 118.71(5) 1_565 . N15 K3 K7 44.25(4) 2_655 . N12 K3 K7 44.39(4) . . O1 K3 K7 44.27(3) . . C26 K3 K7 60.04(3) 2_655 . H201 O6 H200 121.436(3) . . C12 B3 C14 108.38(16) . . C12 B3 C13 106.90(16) . . C14 B3 C13 109.71(17) . . C12 B3 C3X 115.46(17) . . C14 B3 C3X 107.35(16) . . C13 B3 C3X 108.98(16) . . C2 C3X C41 112.34(18) . . C2 C3X B3 128.56(17) . . C41 C3X B3 119.09(17) . . C7X N3 K3 171.80(18) . . C16 F3 K4 136.52(10) . . O47 K4 O48 67.95(7) . . O47 K4 F1 164.35(5) . 4 O48 K4 F1 98.76(5) . 4 O47 K4 N19 75.80(5) . . O48 K4 N19 93.89(5) . . F1 K4 N19 114.58(4) 4 . O47 K4 N6 95.25(5) . 4 O48 K4 N6 75.90(5) . 4 F1 K4 N6 72.79(4) 4 4 N19 K4 N6 168.53(6) . 4 O47 K4 F3 96.46(5) . . O48 K4 F3 161.89(5) . . F1 K4 F3 97.88(4) 4 . N19 K4 F3 72.62(4) . . N6 K4 F3 116.11(4) 4 . O47 K4 N8 114.33(5) . 4 O48 K4 N8 65.61(6) . 4 F1 K4 N8 64.19(4) 4 4 N19 K4 N8 64.10(5) . 4 N6 K4 N8 114.79(5) 4 4 F3 K4 N8 116.27(4) . 4 O47 K4 N14 66.15(5) . . O48 K4 N14 114.79(6) . . F1 K4 N14 115.38(4) 4 . N19 K4 N14 116.06(5) . . N6 K4 N14 65.16(5) 4 . F3 K4 N14 63.46(4) . . N8 K4 N14 179.51(6) 4 . O47 K4 C24 85.23(5) . . O48 K4 C24 112.93(5) . . F1 K4 C24 108.26(4) 4 . N19 K4 C24 19.09(5) . . N6 K4 C24 170.46(5) 4 . F3 K4 C24 54.44(4) . . N8 K4 C24 73.36(5) 4 . N14 K4 C24 106.64(5) . . O47 K4 C13 114.13(5) . 4 O48 K4 C13 86.60(5) . 4 F1 K4 C13 54.85(4) 4 4 N19 K4 C13 169.27(5) . 4 N6 K4 C13 19.09(5) 4 4 F3 K4 C13 108.94(4) . 4 N8 K4 C13 106.67(5) 4 4 N14 K4 C13 73.12(5) . 4 C24 K4 C13 157.19(5) . 4 O47 K4 K1 46.86(4) . . O48 K4 K1 69.52(4) . . F1 K4 K1 121.95(3) 4 . N19 K4 K1 122.62(4) . . N6 K4 K1 49.16(3) 4 . F3 K4 K1 107.13(3) . . N8 K4 K1 135.06(4) 4 . N14 K4 K1 45.32(3) . . C24 K4 K1 129.05(4) . . C13 K4 K1 67.55(3) 4 . O47 K4 K2 69.49(4) . 7 O48 K4 K2 46.03(4) . 7 F1 K4 K2 107.79(3) 4 7 N19 K4 K2 48.59(3) . 7 N6 K4 K2 121.81(4) 4 7 F3 K4 K2 121.13(3) . 7 N8 K4 K2 44.87(3) 4 7 N14 K4 K2 135.60(4) . 7 C24 K4 K2 67.29(3) . 7 C13 K4 K2 129.32(4) 4 7 K1 K4 K2 102.403(14) . 7 F1 C41 C5X 117.76(16) . . F1 C41 C3X 117.04(17) . . C5X C41 C3X 125.20(18) . . C26 B4 C27 110.07(17) . . C26 B4 C28 109.29(16) . . C27 B4 C28 108.14(16) . . C26 B4 C19 108.82(16) . . C27 B4 C19 110.30(16) . . C28 B4 C19 110.21(16) . . C8 N4 K3 160.1(2) . 1_545 C3 O3 C6 107.6(2) . . O3 C3 C4 104.9(3) . . O3 C3 H3A 110.8 . . C4 C3 H3A 110.8 . . O3 C3 H3B 110.8 . . C4 C3 H3B 110.8 . . H3A C3 H3B 108.9 . . C3 C4 C5 102.7(3) . . C3 C4 H4A 111.2 . . C5 C4 H4A 111.2 . . C3 C4 H4B 111.2 . . C5 C4 H4B 111.2 . . H4A C4 H4B 109.1 . . C4 C5 C6 104.4(3) . . C4 C5 H5A 110.9 . . C6 C5 H5A 110.9 . . C4 C5 H5B 110.9 . . C6 C5 H5B 110.9 . . H5A C5 H5B 108.9 . . O3 C6 C5 106.2(3) . . O3 C6 H6A 110.5 . . C5 C6 H6A 110.5 . . O3 C6 H6B 110.5 . . C5 C6 H6B 110.5 . . H6A C6 H6B 108.7 . . C3B O3B C4B 107.6(12) . . O3B C3B C5B 109.5(11) . . O3B C3B H3B1 109.8 . . C5B C3B H3B1 109.8 . . O3B C3B H3B2 109.8 . . C5B C3B H3B2 109.8 . . H3B1 C3B H3B2 108.2 . . C6B C4B O3B 108.3(12) . . C6B C4B H4AB 110.0 . . O3B C4B H4AB 110.0 . . C6B C4B H4BB 110.0 . . O3B C4B H4BB 110.0 . . H4AB C4B H4BB 108.4 . . C3B C5B C6B 105.9(11) . . C3B C5B H5AB 110.6 . . C6B C5B H5AB 110.6 . . C3B C5B H5BB 110.6 . . C6B C5B H5BB 110.6 . . H5AB C5B H5BB 108.7 . . C4B C6B C5B 106.6(11) . . C4B C6B H6AB 110.4 . . C5B C6B H6AB 110.4 . . C4B C6B H6BB 110.4 . . C5B C6B H6BB 110.4 . . H6AB C6B H6BB 108.6 . . C32 O4 C29 107.78(18) . . O5 K5 N17 89.48(6) . . O5 K5 N16 98.68(6) . 1_545 N17 K5 N16 93.53(7) . 1_545 O5 K5 N2 161.67(6) . 2_655 N17 K5 N2 83.69(6) . 2_655 N16 K5 N2 98.70(6) 1_545 2_655 O5 K5 N10 86.70(6) . 6 N17 K5 N10 115.90(6) . 6 N16 K5 N10 150.21(6) 1_545 6 N2 K5 N10 81.08(5) 2_655 6 O5 K5 O2 118.83(5) . 2_655 N17 K5 O2 151.67(5) . 2_655 N16 K5 O2 81.77(5) 1_545 2_655 N2 K5 O2 69.59(5) 2_655 2_655 N10 K5 O2 70.17(5) 6 2_655 O5 K5 C61 165.20(5) . 2_655 N17 K5 C61 75.83(5) . 2_655 N16 K5 C61 84.21(5) 1_545 2_655 N2 K5 C61 16.93(5) 2_655 2_655 N10 K5 C61 98.01(5) 6 2_655 O2 K5 C61 75.90(5) 2_655 2_655 O5 K5 K6 128.87(5) . 2_655 N17 K5 K6 119.10(4) . 2_655 N16 K5 K6 118.72(4) 1_545 2_655 N2 K5 K6 44.18(4) 2_655 2_655 N10 K5 K6 43.63(3) 6 2_655 O2 K5 K6 44.54(3) 2_655 2_655 C61 K5 K6 59.78(3) 2_655 2_655 N1 C5X C41 118.73(17) . . N1 C5X B2 119.12(17) . . C41 C5X B2 122.14(17) . . C20 B5 C21 108.51(16) . . C20 B5 C22 108.75(16) . . C21 B5 C22 108.54(16) . . C20 B5 C15 110.45(16) . . C21 B5 C15 110.62(15) . . C22 B5 C15 109.91(16) . . C12 N5 K1 166.91(17) . . C38 O5 C35 109.25(18) . . C38 O5 K5 127.86(13) . . C35 O5 K5 121.63(13) . . N10 K6 N10 180.00(2) . 5_656 N10 K6 N2 83.55(5) . 5_656 N10 K6 N2 96.45(5) 5_656 5_656 N10 K6 N2 96.45(5) . . N10 K6 N2 83.55(5) 5_656 . N2 K6 N2 180.0 5_656 . N10 K6 O2 73.49(5) . 5_656 N10 K6 O2 106.51(5) 5_656 5_656 N2 K6 O2 71.32(5) 5_656 5_656 N2 K6 O2 108.68(5) . 5_656 N10 K6 O2 106.51(5) . . N10 K6 O2 73.49(5) 5_656 . N2 K6 O2 108.68(5) 5_656 . N2 K6 O2 71.32(5) . . O2 K6 O2 180.0 5_656 . N10 K6 K5 133.88(3) . 2_655 N10 K6 K5 46.12(4) 5_656 2_655 N2 K6 K5 135.52(4) 5_656 2_655 N2 K6 K5 44.48(4) . 2_655 O2 K6 K5 133.32(3) 5_656 2_655 O2 K6 K5 46.68(3) . 2_655 N10 K6 K5 46.12(3) . 6_556 N10 K6 K5 133.88(4) 5_656 6_556 N2 K6 K5 44.48(4) 5_656 6_556 N2 K6 K5 135.52(4) . 6_556 O2 K6 K5 46.68(3) 5_656 6_556 O2 K6 K5 133.32(3) . 6_556 K5 K6 K5 180.0 2_655 6_556 C25 B6 C24 106.91(16) . . C25 B6 C23 108.36(16) . . C24 B6 C23 109.87(17) . . C25 B6 C17 115.81(17) . . C24 B6 C17 108.59(16) . . C23 B6 C17 107.24(16) . . N2 C61 B1 178.3(2) . . N2 C61 K5 46.11(12) . 2_655 B1 C61 K5 135.56(12) . 2_655 C13 N6 K1 162.30(16) . 4_545 C13 N6 K4 103.06(14) . 4_545 K1 N6 K4 81.08(4) 4_545 4_545 N15 K7 N15 154.81(9) 2_655 . N15 K7 O1 71.52(5) 2_655 . N15 K7 O1 128.81(6) . . N15 K7 O1 128.81(6) 2_655 2_655 N15 K7 O1 71.52(5) . 2_655 O1 K7 O1 89.52(7) . 2_655 N15 K7 N12 82.37(5) 2_655 . N15 K7 N12 89.91(5) . . O1 K7 N12 72.56(5) . . O1 K7 N12 137.47(5) 2_655 . N15 K7 N12 89.91(5) 2_655 2_655 N15 K7 N12 82.38(5) . 2_655 O1 K7 N12 137.47(5) . 2_655 O1 K7 N12 72.56(5) 2_655 2_655 N12 K7 N12 144.14(8) . 2_655 N15 K7 K3 44.23(4) 2_655 . N15 K7 K3 135.36(4) . . O1 K7 K3 46.01(3) . . O1 K7 K3 135.30(4) 2_655 . N12 K7 K3 45.61(4) . . N12 K7 K3 133.83(4) 2_655 . N15 K7 K3 135.36(4) 2_655 2_655 N15 K7 K3 44.23(4) . 2_655 O1 K7 K3 135.30(4) . 2_655 O1 K7 K3 46.01(3) 2_655 2_655 N12 K7 K3 133.83(4) . 2_655 N12 K7 K3 45.61(4) 2_655 2_655 K3 K7 K3 178.68(2) . 2_655 N3 C7X B1 178.0(2) . . C14 N7 K1 150.80(17) . 4 C40 C7 C42 104.3(3) . . C40 C7 H7A 110.9 . . C42 C7 H7A 110.9 . . C40 C7 H7B 110.9 . . C42 C7 H7B 110.9 . . H7A C7 H7B 108.9 . . N10 C9 B2 178.1(2) . . C10 N9 K2 145.76(17) . 6_566 N4 C8 B1 176.0(2) . . C11 N8 K2 161.77(18) . 6_556 C11 N8 K4 112.74(15) . 4_545 K2 N8 K4 81.58(5) 6_556 4_545 C9 N10 K6 133.08(15) . . C9 N10 K5 114.31(14) . 6_556 K6 N10 K5 90.25(5) . 6_556 N9 C10 B2 178.1(2) . . C20 N12 K7 133.01(15) . . C20 N12 K3 115.64(15) . . K7 N12 K3 90.00(5) . . N5 C12 B3 175.9(2) . . C21 N13 K1 146.09(17) . 1_565 N6 C13 B3 177.7(2) . . N6 C13 K4 57.85(12) . 4_545 B3 C13 K4 121.19(12) . 4_545 C22 N14 K1 158.98(18) . . C22 N14 K4 114.57(15) . . K1 N14 K4 80.03(5) . . N7 C14 B3 175.4(2) . . C26 N15 K3 117.72(15) . 2_655 C26 N15 K7 143.69(16) . . K3 N15 K7 91.52(6) 2_655 . N11 C15 C16 118.93(17) . . N11 C15 B5 118.94(17) . . C16 C15 B5 122.13(17) . . C27 N16 K5 162.59(18) . 1_565 F3 C16 C15 117.67(16) . . F3 C16 C17 117.39(17) . . C15 C16 C17 124.94(18) . . C28 N17 K5 170.24(19) . . C18 C17 C16 112.26(18) . . C18 C17 B6 128.75(17) . . C16 C17 B6 118.98(17) . . C25 N18 K2 170.60(18) . . F4 C18 C17 118.48(17) . . F4 C18 C19 117.17(17) . . C17 C18 C19 124.35(18) . . C24 N19 K4 104.66(14) . . C24 N19 K2 165.07(16) . 7 K4 N19 K2 83.12(4) . 7 N11 C19 C18 119.48(18) . . N11 C19 B4 118.41(17) . . C18 C19 B4 122.10(17) . . C23 N20 K2 148.06(18) . 7_565 N12 C20 B5 178.8(2) . . N13 C21 B5 178.9(2) . . O5 C35 C36 106.95(18) . . O5 C35 H02E 110.3 . . C36 C35 H02E 110.3 . . O5 C35 H02F 110.3 . . C36 C35 H02F 110.3 . . H02E C35 H02F 108.6 . . C35 C36 C37 103.98(19) . . C35 C36 H02M 111.0 . . C37 C36 H02M 111.0 . . C35 C36 H02N 111.0 . . C37 C36 H02N 111.0 . . H02M C36 H02N 109.0 . . C38 C37 C36 102.25(19) . . C38 C37 H02G 111.3 . . C36 C37 H02G 111.3 . . C38 C37 H02H 111.3 . . C36 C37 H02H 111.3 . . H02G C37 H02H 109.2 . . O5 C38 C37 104.59(18) . . O5 C38 H02A 110.8 . . C37 C38 H02A 110.8 . . O5 C38 H02B 110.8 . . C37 C38 H02B 110.8 . . H02A C38 H02B 108.9 . . O1 C39 C40 106.8(3) . . O1 C39 H02Z 110.4 . . C40 C39 H02Z 110.4 . . O1 C39 H010 110.4 . . C40 C39 H010 110.4 . . H02Z C39 H010 108.6 . . C7 C40 C39 104.0(3) . . C7 C40 H098 111.0 . . C39 C40 H098 111.0 . . C7 C40 H099 111.0 . . C39 C40 H099 111.0 . . H098 C40 H099 109.0 . . O1 C42 C7 104.9(3) . . O1 C42 H121 110.8 . . C7 C42 H121 110.8 . . O1 C42 H122 110.8 . . C7 C42 H122 110.8 . . H121 C42 H122 108.8 . . O2 C43 C44 107.1(2) . . O2 C43 H02S 110.3 . . C44 C43 H02S 110.3 . . O2 C43 H02T 110.3 . . C44 C43 H02T 110.3 . . H02S C43 H02T 108.6 . . C45 C44 C43 104.9(3) . . C45 C44 H013 110.8 . . C43 C44 H013 110.8 . . C45 C44 H014 110.8 . . C43 C44 H014 110.8 . . H013 C44 H014 108.8 . . C44 C45 C46 102.6(3) . . C44 C45 H011 111.2 . . C46 C45 H011 111.2 . . C44 C45 H012 111.2 . . C46 C45 H012 111.2 . . H011 C45 H012 109.2 . . O2 C46 C45 105.7(3) . . O2 C46 H02W 110.6 . . C45 C46 H02W 110.6 . . O2 C46 H02X 110.6 . . C45 C46 H02X 110.6 . . H02W C46 H02X 108.7 . . K4 O47 K1 87.52(5) . . K4 O47 H9 121(3) . . K1 O47 H9 125(3) . . K4 O47 H8 114(2) . . K1 O47 H8 107(2) . . H9 O47 H8 102(3) . . K4 O48 K2 88.62(5) . 7 K4 O48 H10 120(3) . . K2 O48 H10 118(3) 7 . K4 O48 H11 113(3) . . K2 O48 H11 111(3) 7 . H10 O48 H11 106(4) . . C50 O49 C53 108.89(17) . . C50 O49 K3 128.17(13) . . C53 O49 K3 122.12(13) . . O49 C50 C51 105.05(17) . . O49 C50 H01A 110.7 . . C51 C50 H01A 110.7 . . O49 C50 H01B 110.7 . . C51 C50 H01B 110.7 . . H01A C50 H01B 108.8 . . C50 C51 C52 102.23(18) . . C50 C51 H02C 111.3 . . C52 C51 H02C 111.3 . . C50 C51 H02D 111.3 . . C52 C51 H02D 111.3 . . H02C C51 H02D 109.2 . . C53 C52 C51 103.54(19) . . C53 C52 H02O 111.1 . . C51 C52 H02O 111.1 . . C53 C52 H02P 111.1 . . C51 C52 H02P 111.1 . . H02O C52 H02P 109.0 . . O49 C53 C52 107.06(18) . . O49 C53 H01C 110.3 . . C52 C53 H01C 110.3 . . O49 C53 H01D 110.3 . . C52 C53 H01D 110.3 . . H01C C53 H01D 108.6 . . N14 C22 B5 176.5(2) . . N19 C24 B6 177.2(2) . . N19 C24 K4 56.25(12) . . B6 C24 K4 124.03(12) . . N20 C23 B6 175.1(2) . . N15 C26 B4 178.1(2) . . N15 C26 K3 45.50(12) . 2_655 B4 C26 K3 136.35(12) . 2_655 N18 C25 B6 175.9(2) . . N16 C27 B4 176.7(2) . . N17 C28 B4 177.2(2) . . O4 C29 C30 106.5(2) . . O4 C29 H02K 110.4 . . C30 C29 H02K 110.4 . . O4 C29 H02L 110.4 . . C30 C29 H02L 110.4 . . H02K C29 H02L 108.6 . . C31 C30 C29 104.7(2) . . C31 C30 H02U 110.8 . . C29 C30 H02U 110.8 . . C31 C30 H02V 110.8 . . C29 C30 H02V 110.8 . . H02U C30 H02V 108.9 . . C32 C31 C30 102.8(2) . . C32 C31 H02Q 111.2 . . C30 C31 H02Q 111.2 . . C32 C31 H02R 111.2 . . C30 C31 H02R 111.2 . . H02Q C31 H02R 109.1 . . O4 C32 C31 104.9(2) . . O4 C32 H02I 110.8 . . C31 C32 H02I 110.8 . . O4 C32 H02J 110.8 . . C31 C32 H02J 110.8 . . H02I C32 H02J 108.8 . . C19 N11 C15 120.03(17) . . N8 C11 B2 177.5(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 K1 N5 2.7461(18) . K1 N14 2.7510(18) . K1 N7 2.7812(19) 4_545 K1 O47 2.7829(17) . K1 N13 2.7867(18) 1_545 K1 N6 2.9179(18) 4 K1 K4 3.8102(6) . C1 N1 1.345(2) . C1 C2 1.390(3) . C1 B1 1.620(3) . B1 C61 1.590(3) . B1 C7X 1.596(3) . B1 C8 1.600(3) . N1 C5X 1.347(2) . F1 C41 1.373(2) . F1 K4 2.8957(12) 4_545 O1 C42 1.429(3) . O1 C39 1.445(3) . O1 K7 2.8356(17) . O1 K3 2.9226(17) . K2 N18 2.7395(19) . K2 N8 2.7491(19) 6 K2 N20 2.7718(19) 7_565 K2 O48 2.7747(18) 7 K2 N9 2.7954(19) 6_565 K2 N19 2.9119(17) 7 K2 K4 3.8546(6) 7 C2 F2 1.355(2) . C2 C3X 1.382(3) . B2 C11 1.589(3) . B2 C9 1.596(3) . B2 C10 1.598(3) . B2 C5X 1.617(3) . N2 C61 1.148(3) . N2 K6 2.8254(18) . N2 K5 2.8401(19) 2_655 O2 C46 1.432(3) . O2 C43 1.440(3) . O2 K6 2.8433(16) . O2 K5 2.9489(16) 2_655 K3 O49 2.7058(17) . K3 N3 2.760(2) . K3 N4 2.769(2) 1_565 K3 N15 2.8343(19) 2_655 K3 N12 2.9027(18) . K3 C26 3.518(2) 2_655 K3 K7 4.0620(4) . O6 H201 0.90000(3) . O6 H200 0.900001(18) . B3 C12 1.591(3) . B3 C14 1.595(3) . B3 C13 1.604(3) . B3 C3X 1.620(3) . C3X C41 1.386(3) . N3 C7X 1.144(3) . F3 C16 1.369(2) . F3 K4 2.9787(12) . K4 O47 2.7255(17) . K4 O48 2.7432(18) . K4 F1 2.8959(12) 4 K4 N19 2.8984(17) . K4 N6 2.9437(17) 4 K4 N8 3.134(2) 4 K4 N14 3.155(2) . K4 C24 3.3723(19) . K4 C13 3.3869(18) 4 K4 K2 3.8544(6) 7 C41 C5X 1.380(3) . B4 C26 1.588(3) . B4 C27 1.596(3) . B4 C28 1.597(3) . B4 C19 1.618(3) . N4 C8 1.137(3) . N4 K3 2.769(2) 1_545 O3 C3 1.419(3) . O3 C6 1.425(4) . C3 C4 1.473(5) . C3 H3A 0.9900 . C3 H3B 0.9900 . C4 C5 1.513(5) . C4 H4A 0.9900 . C4 H4B 0.9900 . C5 C6 1.515(5) . C5 H5A 0.9900 . C5 H5B 0.9900 . C6 H6A 0.9900 . C6 H6B 0.9900 . O3B C3B 1.415(16) . O3B C4B 1.47(2) . C3B C5B 1.474(18) . C3B H3B1 0.9900 . C3B H3B2 0.9900 . C4B C6B 1.46(2) . C4B H4AB 0.9900 . C4B H4BB 0.9900 . C5B C6B 1.482(19) . C5B H5AB 0.9900 . C5B H5BB 0.9900 . C6B H6AB 0.9900 . C6B H6BB 0.9900 . O4 C32 1.434(3) . O4 C29 1.442(3) . F4 C18 1.360(2) . K5 O5 2.6960(18) . K5 N17 2.7628(19) . K5 N16 2.764(2) 1_545 K5 N2 2.8401(19) 2_655 K5 N10 2.9212(17) 6 K5 O2 2.9491(16) 2_655 K5 C61 3.513(2) 2_655 K5 K6 4.0527(4) 2_655 B5 C20 1.590(3) . B5 C21 1.594(3) . B5 C22 1.596(3) . B5 C15 1.617(3) . N5 C12 1.142(3) . O5 C38 1.427(3) . O5 C35 1.438(3) . K6 N10 2.7965(18) . K6 N10 2.7965(18) 5_656 K6 N2 2.8254(18) 5_656 K6 O2 2.8433(16) 5_656 K6 K5 4.0525(4) 2_655 K6 K5 4.0525(4) 6_556 B6 C25 1.588(3) . B6 C24 1.604(3) . B6 C23 1.604(3) . B6 C17 1.618(3) . C61 K5 3.513(2) 2_655 N6 C13 1.137(3) . N6 K1 2.9179(18) 4_545 N6 K4 2.9436(17) 4_545 K7 N15 2.8353(19) 2_655 K7 N15 2.8353(19) . K7 O1 2.8357(17) 2_655 K7 N12 2.8417(19) . K7 N12 2.8418(19) 2_655 K7 K3 4.0621(4) 2_655 N7 C14 1.142(3) . N7 K1 2.7812(19) 4 C7 C40 1.465(6) . C7 C42 1.501(5) . C7 H7A 0.9900 . C7 H7B 0.9900 . C9 N10 1.144(3) . N9 C10 1.145(3) . N9 K2 2.7955(19) 6_566 N8 C11 1.139(3) . N8 K2 2.7492(19) 6_556 N8 K4 3.134(2) 4_545 N10 K5 2.9211(17) 6_556 N12 C20 1.147(3) . N13 C21 1.146(3) . N13 K1 2.7868(18) 1_565 C13 K4 3.3869(18) 4_545 N14 C22 1.139(3) . N15 C26 1.148(3) . N15 K3 2.8344(19) 2_655 C15 N11 1.350(2) . C15 C16 1.382(3) . N16 C27 1.142(3) . N16 K5 2.764(2) 1_565 C16 C17 1.387(3) . N17 C28 1.148(3) . C17 C18 1.382(3) . N18 C25 1.141(3) . C18 C19 1.386(3) . N19 C24 1.140(3) . N19 K2 2.9119(17) 7 C19 N11 1.348(2) . N20 C23 1.140(3) . N20 K2 2.7718(19) 7_565 C35 C36 1.515(3) . C35 H02E 0.9900 . C35 H02F 0.9900 . C36 C37 1.519(3) . C36 H02M 0.9900 . C36 H02N 0.9900 . C37 C38 1.516(3) . C37 H02G 0.9900 . C37 H02H 0.9900 . C38 H02A 0.9900 . C38 H02B 0.9900 . C39 C40 1.486(5) . C39 H02Z 0.9900 . C39 H010 0.9900 . C40 H098 0.9900 . C40 H099 0.9900 . C42 H121 0.9900 . C42 H122 0.9900 . C43 C44 1.505(4) . C43 H02S 0.9900 . C43 H02T 0.9900 . C44 C45 1.469(6) . C44 H013 0.9900 . C44 H014 0.9900 . C45 C46 1.510(4) . C45 H011 0.9900 . C45 H012 0.9900 . C46 H02W 0.9900 . C46 H02X 0.9900 . O47 H9 0.84(4) . O47 H8 0.79(3) . O48 K2 2.7747(18) 7 O48 H10 0.72(4) . O48 H11 0.82(4) . O49 C50 1.432(3) . O49 C53 1.443(3) . C50 C51 1.505(3) . C50 H01A 0.9900 . C50 H01B 0.9900 . C51 C52 1.523(3) . C51 H02C 0.9900 . C51 H02D 0.9900 . C52 C53 1.512(3) . C52 H02O 0.9900 . C52 H02P 0.9900 . C53 H01C 0.9900 . C53 H01D 0.9900 . C26 K3 3.518(2) 2_655 C29 C30 1.509(4) . C29 H02K 0.9900 . C29 H02L 0.9900 . C30 C31 1.509(4) . C30 H02U 0.9900 . C30 H02V 0.9900 . C31 C32 1.484(4) . C31 H02Q 0.9900 . C31 H02R 0.9900 . C32 H02I 0.9900 . C32 H02J 0.9900 .