#------------------------------------------------------------------------------ #$Date: 2017-11-21 10:50:44 +0200 (Tue, 21 Nov 2017) $ #$Revision: 203412 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/57/7155783.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_7155783 loop_ _publ_author_name 'Tayama, Eiji' 'Watanabe, Kazutoshi' 'Sotome, Sho' _publ_section_title ; Structural and mechanistic studies of the base-induced Sommelet--Hauser rearrangement of N-\a-branched benzylic azetidine-2-carboxylic acid-derived ammonium salts ; _journal_name_full 'Org. Biomol. Chem.' _journal_paper_doi 10.1039/C7OB01391D _journal_year 2017 _chemical_compound_source 'synthesis as described' _chemical_formula_sum 'C42 H46 B N O2' _chemical_formula_weight 607.60 _chemical_name_systematic 2e-BPh4 _space_group_IT_number 1 _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 1 _symmetry_space_group_name_Hall 'P 1' _symmetry_space_group_name_H-M 'P 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary 'direct - structure invariant direct methods' _atom_sites_solution_secondary 'direct - structure invariant direct methods' _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2017-04-19T13:24:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2017-05-30 deposited with the CCDC. 2017-07-24 downloaded from the CCDC. ; _cell_angle_alpha 79.125(6) _cell_angle_beta 89.681(6) _cell_angle_gamma 62.353(4) _cell_formula_units_Z 2 _cell_length_a 10.1389(13) _cell_length_b 10.2830(13) _cell_length_c 19.617(3) _cell_measurement_reflns_used 15228 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.63 _cell_measurement_theta_min 2.98 _cell_measurement_wavelength 0.71073 _cell_volume 1771.3(4) _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2006), SORTAV (Blessing, 1995)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'SIR-2011 (Burla et al., 2012)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device 'quarter \C-circle diffractometer' _diffrn_measurement_device_type XTALAB-MINI _diffrn_measurement_method 'phi or omega oscillation scans' _diffrn_orient_matrix_UB_11 0.005608 _diffrn_orient_matrix_UB_12 -0.043688 _diffrn_orient_matrix_UB_13 0.050628 _diffrn_orient_matrix_UB_21 0.107316 _diffrn_orient_matrix_UB_22 -0.073813 _diffrn_orient_matrix_UB_23 -0.001111 _diffrn_orient_matrix_UB_31 0.030989 _diffrn_orient_matrix_UB_32 0.072468 _diffrn_orient_matrix_UB_33 0.012418 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_unetI/netI 0.0549 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 18195 _diffrn_reflns_point_group_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.946 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.482 _diffrn_reflns_theta_min 2.982 _diffrn_source 'sealed x-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type none _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 652 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.187 _refine_diff_density_min -0.152 _refine_diff_density_rms 0.033 _refine_ls_abs_structure_details ; Flack x determined using 4314 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.1(8) _refine_ls_extinction_coef 0.0058(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 830 _refine_ls_number_reflns 15384 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0552 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+0.2378P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1118 _refine_ls_wR_factor_ref 0.1265 _reflns_Friedel_coverage 0.903 _reflns_Friedel_fraction_full 0.955 _reflns_Friedel_fraction_max 0.898 _reflns_number_gt 11094 _reflns_number_total 15384 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL SIR2011 run in space group P 1 CELL 0.71073 10.1389 10.2830 19.6170 79.125 89.681 62.353 ZERR 1.00 0.0013 0.0013 0.0030 0.006 0.006 0.004 LATT -1 SFAC C H B N O UNIT 84 92 2 2 4 MERG 2 OMIT 9 2 2 OMIT 9 4 6 FMAP 2 PLAN 25 SIZE 0.160 0.200 0.300 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP 20.00 WGHT 0.043200 0.237800 EXTI 0.005838 FVAR 7.15230 O11 5 0.904838 0.623460 0.291981 11.00000 0.06100 0.06759 = 0.04203 -0.01528 0.01452 -0.03753 O12 5 1.088232 0.628336 0.354132 11.00000 0.07222 0.12496 = 0.06534 -0.01691 0.01525 -0.06748 O51 5 0.743855 0.223068 0.804218 11.00000 0.04704 0.08097 = 0.08851 -0.05480 0.00869 -0.01547 O52 5 0.517704 0.234679 0.797934 11.00000 0.07812 0.09763 = 0.09731 -0.05732 0.03146 -0.05507 N11 4 0.891309 0.459176 0.436398 11.00000 0.03488 0.03746 = 0.04265 -0.01002 0.00772 -0.01474 N51 4 0.416951 0.459065 0.889866 11.00000 0.04533 0.04447 = 0.03931 -0.00730 0.01240 -0.02076 C1 1 0.392753 1.172325 0.524944 11.00000 0.03489 0.04068 = 0.03885 -0.01057 0.00331 -0.01396 C2 1 0.380707 1.190028 0.594289 11.00000 0.06802 0.04677 = 0.04294 -0.01243 -0.00097 -0.01851 AFIX 43 H2 2 0.396173 1.107771 0.629021 11.00000 -1.20000 AFIX 0 C3 1 0.346883 1.324180 0.613420 11.00000 0.07646 0.06282 = 0.05638 -0.03038 -0.00538 -0.01572 AFIX 43 H3 2 0.337327 1.330898 0.659976 11.00000 -1.20000 AFIX 0 C4 1 0.327401 1.447005 0.564326 11.00000 0.06439 0.04710 = 0.08804 -0.03137 -0.00411 -0.01724 AFIX 43 H4 2 0.306300 1.536765 0.577159 11.00000 -1.20000 AFIX 0 C5 1 0.339594 1.435154 0.495876 11.00000 0.04871 0.04116 = 0.07906 -0.01422 0.00677 -0.01915 AFIX 43 H5 2 0.328306 1.517048 0.461961 11.00000 -1.20000 AFIX 0 C6 1 0.368583 1.302120 0.476964 11.00000 0.04081 0.04370 = 0.05006 -0.01134 0.00941 -0.02050 AFIX 43 H6 2 0.372173 1.298883 0.429901 11.00000 -1.20000 AFIX 0 C7 1 0.494467 1.016477 0.424457 11.00000 0.04229 0.02908 = 0.03805 -0.00949 0.00622 -0.01747 C8 1 0.645268 0.970136 0.414872 11.00000 0.04286 0.03545 = 0.04242 -0.00468 0.00482 -0.01645 AFIX 43 H8 2 0.713840 0.930308 0.454057 11.00000 -1.20000 AFIX 0 C9 1 0.697557 0.980927 0.349195 11.00000 0.05002 0.04246 = 0.05625 -0.00482 0.01857 -0.02053 AFIX 43 H9 2 0.798814 0.949552 0.345308 11.00000 -1.20000 AFIX 0 C10 1 0.599704 1.037721 0.290507 11.00000 0.07742 0.05020 = 0.03877 -0.00924 0.02277 -0.02814 AFIX 43 H10 2 0.634320 1.042883 0.246590 11.00000 -1.20000 AFIX 0 C11 1 0.449769 1.087103 0.296988 11.00000 0.06909 0.05337 = 0.03594 -0.00818 0.00287 -0.02601 AFIX 43 H11 2 0.382206 1.126973 0.257425 11.00000 -1.20000 AFIX 0 C12 1 0.399665 1.077225 0.362770 11.00000 0.04497 0.04881 = 0.04268 -0.01196 0.00433 -0.02012 AFIX 43 H12 2 0.297595 1.112935 0.365938 11.00000 -1.20000 AFIX 0 C13 1 0.288051 0.981084 0.503537 11.00000 0.04414 0.03903 = 0.04236 -0.00493 0.00613 -0.01794 C14 1 0.262108 0.901789 0.459098 11.00000 0.05772 0.05365 = 0.05931 -0.01780 0.01287 -0.03373 AFIX 43 H14 2 0.327497 0.870211 0.425167 11.00000 -1.20000 AFIX 0 C15 1 0.145204 0.867762 0.462706 11.00000 0.06984 0.06228 = 0.08066 -0.01937 0.00608 -0.04164 AFIX 43 H15 2 0.131082 0.818684 0.430424 11.00000 -1.20000 AFIX 0 C16 1 0.050202 0.906150 0.513689 11.00000 0.05941 0.06994 = 0.09270 -0.00514 0.01153 -0.04118 AFIX 43 H16 2 -0.027507 0.881738 0.517128 11.00000 -1.20000 AFIX 0 C17 1 0.071638 0.981060 0.559479 11.00000 0.05562 0.06541 = 0.07124 -0.00811 0.02570 -0.02632 AFIX 43 H17 2 0.008309 1.006594 0.594674 11.00000 -1.20000 AFIX 0 C18 1 0.185693 1.019730 0.554557 11.00000 0.05260 0.05137 = 0.04908 -0.00803 0.01127 -0.02467 AFIX 43 H18 2 0.195214 1.072986 0.585931 11.00000 -1.20000 AFIX 0 C19 1 0.566789 0.871375 0.559168 11.00000 0.04856 0.04313 = 0.03092 -0.01354 0.01273 -0.01565 C20 1 0.574266 0.729716 0.578038 11.00000 0.06580 0.04510 = 0.04616 -0.01227 0.01993 -0.01984 AFIX 43 H20 2 0.501127 0.714037 0.558217 11.00000 -1.20000 AFIX 0 C21 1 0.686487 0.611548 0.625174 11.00000 0.09244 0.04522 = 0.05327 -0.00061 0.01996 -0.01074 AFIX 43 H21 2 0.686806 0.519400 0.636456 11.00000 -1.20000 AFIX 0 C22 1 0.796876 0.630164 0.655165 11.00000 0.09395 0.07167 = 0.03965 -0.00279 -0.00712 0.00322 AFIX 43 H22 2 0.872048 0.551096 0.686695 11.00000 -1.20000 AFIX 0 C23 1 0.795112 0.767180 0.638065 11.00000 0.07113 0.07947 = 0.04974 -0.01952 -0.01029 -0.01003 AFIX 43 H23 2 0.869523 0.781231 0.657764 11.00000 -1.20000 AFIX 0 C24 1 0.681795 0.883902 0.591338 11.00000 0.05498 0.05421 = 0.04431 -0.01501 -0.00130 -0.01428 AFIX 43 H24 2 0.682257 0.975732 0.580779 11.00000 -1.20000 AFIX 0 C25 1 0.636853 0.522370 0.382540 11.00000 0.03415 0.04467 = 0.04657 -0.01337 0.00888 -0.01595 C26 1 0.562502 0.660000 0.336977 11.00000 0.04799 0.04955 = 0.06911 -0.00698 -0.00458 -0.01690 AFIX 43 H26 2 0.569945 0.742827 0.344892 11.00000 -1.20000 AFIX 0 C27 1 0.476958 0.671556 0.279460 11.00000 0.06446 0.07315 = 0.07711 0.00415 -0.01596 -0.02542 AFIX 43 H27 2 0.428234 0.762415 0.247455 11.00000 -1.20000 AFIX 0 C28 1 0.463322 0.549557 0.269181 11.00000 0.06844 0.10314 = 0.07101 -0.01576 -0.01311 -0.04038 AFIX 43 H28 2 0.403597 0.559951 0.230618 11.00000 -1.20000 AFIX 0 C29 1 0.535401 0.413450 0.314254 11.00000 0.06080 0.07825 = 0.07866 -0.02959 0.00578 -0.03862 AFIX 43 H29 2 0.526546 0.331499 0.306112 11.00000 -1.20000 AFIX 0 C30 1 0.622138 0.399461 0.372448 11.00000 0.04391 0.05423 = 0.05667 -0.01749 0.01506 -0.02506 C31 1 0.704284 0.266562 0.430595 11.00000 0.05341 0.05052 = 0.08060 -0.01296 0.01683 -0.03198 AFIX 23 H31A 2 0.795683 0.192581 0.416213 11.00000 -1.20000 H31B 2 0.642630 0.219905 0.446838 11.00000 -1.20000 AFIX 0 C32 1 0.738305 0.334011 0.487097 11.00000 0.04961 0.05763 = 0.05263 -0.00163 0.01446 -0.02712 AFIX 23 H32A 2 0.664134 0.353395 0.520559 11.00000 -1.20000 H32B 2 0.836248 0.265858 0.511618 11.00000 -1.20000 AFIX 0 C33 1 0.733635 0.480706 0.449251 11.00000 0.03671 0.04439 = 0.04564 -0.01453 0.01371 -0.01800 AFIX 13 H33 2 0.685504 0.557971 0.476788 11.00000 -1.20000 AFIX 0 C34 1 0.975978 0.340634 0.396948 11.00000 0.04361 0.03837 = 0.05834 -0.01453 0.01702 -0.01472 AFIX 33 H34A 2 0.915608 0.356689 0.355582 11.00000 -1.20000 H34B 2 1.065879 0.344443 0.384222 11.00000 -1.20000 H34C 2 1.001259 0.244030 0.425503 11.00000 -1.20000 AFIX 0 C35 1 0.977207 0.444564 0.503611 11.00000 0.04676 0.05883 = 0.04542 -0.01015 0.00097 -0.02186 AFIX 23 H35A 2 0.930437 0.427775 0.545269 11.00000 -1.20000 H35B 2 1.081880 0.370273 0.508099 11.00000 -1.20000 AFIX 0 C36 1 0.951443 0.604382 0.481849 11.00000 0.05986 0.05564 = 0.05047 -0.01790 0.00659 -0.02951 AFIX 23 H36A 2 1.042815 0.612914 0.480645 11.00000 -1.20000 H36B 2 0.880406 0.672644 0.508147 11.00000 -1.20000 AFIX 0 C37 1 0.884927 0.613823 0.409939 11.00000 0.04458 0.03787 = 0.05002 -0.01360 0.00983 -0.02040 AFIX 13 H37 2 0.781267 0.694131 0.400130 11.00000 -1.20000 AFIX 0 C38 1 0.974669 0.621566 0.348750 11.00000 0.04939 0.04780 = 0.04720 -0.00800 0.00655 -0.02737 C39 1 0.965927 0.633223 0.222120 11.00000 0.08382 0.06742 = 0.04277 -0.01608 0.02237 -0.03789 C40 1 0.980229 0.774729 0.204534 11.00000 0.12177 0.06047 = 0.06075 -0.01102 0.03914 -0.04023 AFIX 33 H40A 2 1.058296 0.766439 0.235313 11.00000 -1.20000 H40B 2 1.004137 0.789303 0.157215 11.00000 -1.20000 H40C 2 0.887380 0.858743 0.209852 11.00000 -1.20000 AFIX 0 C41 1 1.111725 0.491490 0.224821 11.00000 0.11539 0.06599 = 0.08807 -0.02690 0.05128 -0.03303 AFIX 33 H41A 2 1.186106 0.490719 0.255200 11.00000 -1.20000 H41B 2 1.097428 0.405598 0.242145 11.00000 -1.20000 H41C 2 1.144246 0.488129 0.178835 11.00000 -1.20000 AFIX 0 C42 1 0.844914 0.640811 0.175264 11.00000 0.14009 0.14497 = 0.05076 -0.02459 0.01392 -0.08132 AFIX 33 H42A 2 0.838560 0.549151 0.187752 11.00000 -1.20000 H42B 2 0.751015 0.723788 0.180354 11.00000 -1.20000 H42C 2 0.867771 0.654348 0.127717 11.00000 -1.20000 AFIX 0 C51 1 0.058430 1.263976 0.984214 11.00000 0.04303 0.04878 = 0.04216 -0.00901 0.00266 -0.02720 C52 1 -0.017693 1.411821 0.992785 11.00000 0.06577 0.04651 = 0.05741 -0.01135 -0.00212 -0.02768 AFIX 43 H52 2 -0.023856 1.429089 1.037839 11.00000 -1.20000 AFIX 0 C53 1 -0.084539 1.534181 0.937776 11.00000 0.08601 0.04422 = 0.09903 -0.00885 -0.00811 -0.02875 AFIX 43 H53 2 -0.134348 1.630609 0.946429 11.00000 -1.20000 AFIX 0 C54 1 -0.077631 1.513815 0.870493 11.00000 0.10333 0.07034 = 0.07084 0.02240 -0.02552 -0.05041 AFIX 43 H54 2 -0.123240 1.595546 0.833269 11.00000 -1.20000 AFIX 0 C55 1 -0.002905 1.372002 0.859303 11.00000 0.09573 0.07754 = 0.03961 0.00377 -0.00508 -0.05278 AFIX 43 H55 2 0.003385 1.356672 0.813909 11.00000 -1.20000 AFIX 0 C56 1 0.064001 1.250006 0.914510 11.00000 0.06330 0.05453 = 0.04041 -0.00671 0.00436 -0.03129 AFIX 43 H56 2 0.114931 1.154493 0.904902 11.00000 -1.20000 AFIX 0 C57 1 0.152583 0.963578 1.037065 11.00000 0.04799 0.04496 = 0.03124 -0.01166 0.01312 -0.02177 C58 1 0.039341 0.959320 0.999401 11.00000 0.05171 0.05269 = 0.04956 -0.01545 0.00845 -0.02793 AFIX 43 H58 2 -0.038436 1.049560 0.975390 11.00000 -1.20000 AFIX 0 C59 1 0.036752 0.826743 0.995899 11.00000 0.07502 0.07553 = 0.05286 -0.02446 0.01636 -0.05103 AFIX 43 H59 2 -0.042384 0.830414 0.970388 11.00000 -1.20000 AFIX 0 C60 1 0.148821 0.691638 1.029416 11.00000 0.09556 0.05751 = 0.05174 -0.02427 0.02967 -0.04960 AFIX 43 H60 2 0.148068 0.602812 1.026380 11.00000 -1.20000 AFIX 0 C61 1 0.263636 0.689265 1.068016 11.00000 0.07726 0.04583 = 0.04557 -0.01081 0.02063 -0.02433 AFIX 43 H61 2 0.341052 0.598100 1.091462 11.00000 -1.20000 AFIX 0 C62 1 0.263905 0.821860 1.071927 11.00000 0.06110 0.05044 = 0.03872 -0.01260 0.00877 -0.02570 AFIX 43 H62 2 0.341695 0.817026 1.099000 11.00000 -1.20000 AFIX 0 C63 1 0.059565 1.146766 1.121188 11.00000 0.05287 0.04836 = 0.04163 -0.01630 0.01086 -0.03143 C64 1 -0.096218 1.223394 1.120284 11.00000 0.05707 0.08277 = 0.05218 -0.02797 0.01459 -0.03796 AFIX 43 H64 2 -0.153337 1.268467 1.077475 11.00000 -1.20000 AFIX 0 C65 1 -0.169133 1.234880 1.180868 11.00000 0.07238 0.11514 = 0.07617 -0.05269 0.03807 -0.05791 AFIX 43 H65 2 -0.272937 1.287979 1.178110 11.00000 -1.20000 AFIX 0 C66 1 -0.087887 1.167919 1.244547 11.00000 0.10686 0.11754 = 0.06123 -0.04932 0.04936 -0.08500 AFIX 43 H66 2 -0.136129 1.175310 1.285196 11.00000 -1.20000 AFIX 0 C67 1 0.063964 1.090452 1.247976 11.00000 0.10840 0.09774 = 0.03864 -0.01984 0.01938 -0.07144 AFIX 43 H67 2 0.119506 1.044327 1.291138 11.00000 -1.20000 AFIX 0 C68 1 0.136659 1.079834 1.187269 11.00000 0.06909 0.06212 = 0.03996 -0.01230 0.01274 -0.03722 AFIX 43 H68 2 0.240501 1.026084 1.190966 11.00000 -1.20000 AFIX 0 C69 1 0.313217 1.106800 1.060107 11.00000 0.04928 0.04958 = 0.02979 -0.00070 0.00255 -0.02623 C70 1 0.337617 1.201715 1.095304 11.00000 0.06791 0.06706 = 0.03983 -0.00623 0.00429 -0.04489 AFIX 43 H70 2 0.257392 1.271524 1.113966 11.00000 -1.20000 AFIX 0 C71 1 0.475558 1.195917 1.103415 11.00000 0.08669 0.09448 = 0.04705 0.00863 -0.01383 -0.06764 AFIX 43 H71 2 0.485604 1.261239 1.127343 11.00000 -1.20000 AFIX 0 C72 1 0.598335 1.095592 1.076853 11.00000 0.06095 0.10544 = 0.06935 0.02759 -0.01826 -0.05384 AFIX 43 H72 2 0.691649 1.090316 1.083247 11.00000 -1.20000 AFIX 0 C73 1 0.578039 1.003446 1.040523 11.00000 0.04683 0.07954 = 0.07491 0.01115 0.00896 -0.02679 AFIX 43 H73 2 0.658880 0.935817 1.021263 11.00000 -1.20000 AFIX 0 C74 1 0.439497 1.008919 1.031873 11.00000 0.05112 0.05966 = 0.04841 -0.00484 0.00992 -0.02758 AFIX 43 H74 2 0.430206 0.945393 1.006449 11.00000 -1.20000 AFIX 0 C75 1 0.337960 0.729050 0.832325 11.00000 0.05405 0.04452 = 0.03896 -0.01004 0.01469 -0.01592 C76 1 0.349035 0.818890 0.874050 11.00000 0.07262 0.05069 = 0.04164 -0.01482 0.01840 -0.02101 AFIX 43 H76 2 0.326908 0.807701 0.920180 11.00000 -1.20000 AFIX 0 C77 1 0.392849 0.924635 0.847016 11.00000 0.11192 0.06185 = 0.05579 -0.01769 0.01674 -0.04701 AFIX 43 H77 2 0.400121 0.985492 0.874754 11.00000 -1.20000 AFIX 0 C78 1 0.426105 0.940278 0.778408 11.00000 0.12594 0.06956 = 0.06009 -0.01816 0.03433 -0.05980 AFIX 43 H78 2 0.457363 1.010831 0.760653 11.00000 -1.20000 AFIX 0 C79 1 0.413846 0.853872 0.736228 11.00000 0.11553 0.05819 = 0.04660 -0.00843 0.02919 -0.04083 AFIX 43 H79 2 0.437325 0.865025 0.690318 11.00000 -1.20000 AFIX 0 C80 1 0.366479 0.750321 0.762308 11.00000 0.07700 0.04264 = 0.03624 -0.00897 0.01011 -0.01859 C81 1 0.332936 0.652154 0.725072 11.00000 0.10133 0.06133 = 0.04032 -0.00739 0.00144 -0.02943 AFIX 23 H81A 2 0.424296 0.570221 0.715183 11.00000 -1.20000 H81B 2 0.270667 0.709656 0.681731 11.00000 -1.20000 AFIX 0 C82 1 0.249904 0.593697 0.776940 11.00000 0.06581 0.05640 = 0.05739 -0.00717 -0.00658 -0.02261 AFIX 23 H82A 2 0.279545 0.489531 0.776691 11.00000 -1.20000 H82B 2 0.142742 0.652348 0.764921 11.00000 -1.20000 AFIX 0 C83 1 0.292215 0.608803 0.848851 11.00000 0.04364 0.04696 = 0.04788 -0.01118 0.01178 -0.01307 AFIX 13 H83 2 0.204028 0.642446 0.875148 11.00000 -1.20000 AFIX 0 C84 1 0.356872 0.350995 0.912537 11.00000 0.06308 0.06073 = 0.06253 -0.00531 0.01738 -0.03513 AFIX 33 H84A 2 0.302607 0.348059 0.873411 11.00000 -1.20000 H84B 2 0.438294 0.252691 0.930457 11.00000 -1.20000 H84C 2 0.291201 0.382954 0.948279 11.00000 -1.20000 AFIX 0 C85 1 0.502957 0.461556 0.953241 11.00000 0.06317 0.05929 = 0.03472 -0.01279 0.01118 -0.02531 AFIX 23 H85A 2 0.495894 0.559045 0.952886 11.00000 -1.20000 H85B 2 0.478208 0.422029 0.997494 11.00000 -1.20000 AFIX 0 C86 1 0.650346 0.351218 0.930781 11.00000 0.05163 0.05944 = 0.04867 -0.01345 0.00196 -0.02259 AFIX 23 H86A 2 0.685395 0.247503 0.954291 11.00000 -1.20000 H86B 2 0.729047 0.379603 0.931818 11.00000 -1.20000 AFIX 0 C87 1 0.568126 0.392898 0.858627 11.00000 0.04333 0.04586 = 0.04301 -0.01363 0.01393 -0.02126 AFIX 13 H87 2 0.579936 0.475423 0.830203 11.00000 -1.20000 AFIX 0 C88 1 0.602686 0.273939 0.816721 11.00000 0.05115 0.04896 = 0.04737 -0.01400 0.00703 -0.02101 C89 1 0.818236 0.103430 0.763452 11.00000 0.05243 0.07618 = 0.07723 -0.04654 -0.00198 -0.00544 C90 1 0.736630 0.152722 0.692874 11.00000 0.08166 0.10072 = 0.06670 -0.03701 0.01511 -0.02721 AFIX 33 H90A 2 0.735632 0.243906 0.669226 11.00000 -1.20000 H90B 2 0.785886 0.076091 0.666584 11.00000 -1.20000 H90C 2 0.635759 0.169949 0.697310 11.00000 -1.20000 AFIX 0 C91 1 0.970725 0.089823 0.760834 11.00000 0.05104 0.25656 = 0.25272 -0.21221 0.03570 -0.03631 AFIX 33 H91A 2 0.964073 0.182632 0.735694 11.00000 -1.20000 H91B 2 1.015251 0.067689 0.807423 11.00000 -1.20000 H91C 2 1.031243 0.010368 0.737698 11.00000 -1.20000 AFIX 0 C92 1 0.822414 -0.037752 0.801944 11.00000 0.19524 0.06315 = 0.09550 -0.02083 -0.00458 0.00912 AFIX 33 H92A 2 0.722541 -0.025220 0.802667 11.00000 -1.20000 H92B 2 0.881695 -0.118271 0.779150 11.00000 -1.20000 H92C 2 0.865703 -0.060951 0.848875 11.00000 -1.20000 AFIX 0 B11 3 0.433336 1.011525 0.502450 11.00000 0.03927 0.03869 = 0.03755 -0.01125 0.00602 -0.01649 B51 3 0.145865 1.120544 1.049733 11.00000 0.04671 0.04092 = 0.03189 -0.00879 0.00546 -0.02146 HKLF 4 REM SIR2011 run in space group P 1 REM R1 = 0.0552 for 11094 Fo > 4sig(Fo) and 0.0835 for all 15384 data REM 830 parameters refined using 3 restraints END WGHT 0.0432 0.2379 REM Highest difference peak 0.187, deepest hole -0.152, 1-sigma level 0.033 Q1 1 0.5070 0.9525 0.5327 11.00000 0.05 0.19 Q2 1 0.7076 0.5884 0.4617 11.00000 0.05 0.17 Q3 1 0.1145 1.1812 1.0193 11.00000 0.05 0.16 Q4 1 0.1983 0.5153 0.7802 11.00000 0.05 0.15 Q5 1 0.3580 1.0029 0.5011 11.00000 0.05 0.15 Q6 1 0.5824 0.1769 0.8335 11.00000 0.05 0.14 Q7 1 0.1921 1.0160 1.0462 11.00000 0.05 0.14 Q8 1 0.8208 0.8614 0.1785 11.00000 0.05 0.14 Q9 1 0.4209 1.0948 0.5092 11.00000 0.05 0.14 Q10 1 0.5561 0.4604 0.2861 11.00000 0.05 0.14 Q11 1 0.1348 1.0648 1.0218 11.00000 0.05 0.13 Q12 1 0.8941 0.5678 0.6890 11.00000 0.05 0.13 Q13 1 0.2346 0.8943 1.0259 11.00000 0.05 0.13 Q14 1 1.0218 0.7025 0.3210 11.00000 0.05 0.13 Q15 1 0.2491 0.8848 1.3201 11.00000 0.05 0.13 Q16 1 0.2756 0.9193 1.0623 11.00000 0.05 0.12 Q17 1 0.5111 0.8183 0.5707 11.00000 0.05 0.12 Q18 1 1.0087 0.7426 0.4781 11.00000 0.05 0.12 Q19 1 1.0519 0.3965 0.2159 11.00000 0.05 0.12 Q20 1 1.0945 0.2973 0.4197 11.00000 0.05 0.12 Q21 1 0.6210 0.7043 0.6131 11.00000 0.05 0.12 Q22 1 0.5694 0.9230 0.4153 11.00000 0.05 0.12 Q23 1 0.2811 0.9308 1.3103 11.00000 0.05 0.12 Q24 1 0.7276 0.6031 0.6206 11.00000 0.05 0.12 Q25 1 0.6628 0.4398 0.3714 11.00000 0.05 0.12 ; _cod_data_source_file c7ob01391d2.cif _cod_data_source_block shelx _cod_depositor_comments ; 2017-11-16 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_sum 'C84 H92 B2 N2 O4' _cod_original_formula_weight 1215.21 _cod_original_formula_units_Z 1 _cod_database_code 7155783 _shelx_estimated_absorpt_t_min 0.98 _shelx_estimated_absorpt_t_max 0.989 loop_ _symmetry_equiv_pos_as_xyz 'x, y, 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 O11 O 0.9048(3) 0.6235(3) 0.29198(12) 0.0534(6) Uani 1 1 d . . O12 O 1.0882(4) 0.6283(4) 0.35413(15) 0.0795(9) Uani 1 1 d . . O51 O 0.7439(3) 0.2231(3) 0.80422(16) 0.0726(9) Uani 1 1 d . . O52 O 0.5177(4) 0.2347(4) 0.79793(18) 0.0801(9) Uani 1 1 d . . N11 N 0.8913(3) 0.4592(3) 0.43640(14) 0.0390(6) Uani 1 1 d . . N51 N 0.4170(3) 0.4591(3) 0.88987(14) 0.0435(7) Uani 1 1 d . . C1 C 0.3928(3) 1.1723(4) 0.52494(17) 0.0394(7) Uani 1 1 d . . C2 C 0.3807(4) 1.1900(4) 0.5943(2) 0.0556(10) Uani 1 1 d . . H2 H 0.3962 1.1078 0.629 0.067 Uiso 1 1 calc R U C3 C 0.3469(5) 1.3242(5) 0.6134(2) 0.0694(12) Uani 1 1 d . . H3 H 0.3373 1.3309 0.66 0.083 Uiso 1 1 calc R U C4 C 0.3274(5) 1.4470(5) 0.5643(3) 0.0676(12) Uani 1 1 d . . H4 H 0.3063 1.5368 0.5772 0.081 Uiso 1 1 calc R U C5 C 0.3396(4) 1.4352(4) 0.4959(2) 0.0569(10) Uani 1 1 d . . H5 H 0.3283 1.517 0.462 0.068 Uiso 1 1 calc R U C6 C 0.3686(4) 1.3021(4) 0.47696(19) 0.0444(8) Uani 1 1 d . . H6 H 0.3722 1.2989 0.4299 0.053 Uiso 1 1 calc R U C7 C 0.4945(4) 1.0165(3) 0.42446(16) 0.0359(7) Uani 1 1 d . . C8 C 0.6453(4) 0.9701(3) 0.41487(18) 0.0416(8) Uani 1 1 d . . H8 H 0.7138 0.9303 0.4541 0.05 Uiso 1 1 calc R U C9 C 0.6976(4) 0.9809(4) 0.3492(2) 0.0510(9) Uani 1 1 d . . H9 H 0.7988 0.9496 0.3453 0.061 Uiso 1 1 calc R U C10 C 0.5997(5) 1.0377(4) 0.29051(19) 0.0563(10) Uani 1 1 d . . H10 H 0.6343 1.0429 0.2466 0.068 Uiso 1 1 calc R U C11 C 0.4498(5) 1.0871(4) 0.29699(18) 0.0541(9) Uani 1 1 d . . H11 H 0.3822 1.127 0.2574 0.065 Uiso 1 1 calc R U C12 C 0.3997(4) 1.0772(4) 0.36277(17) 0.0459(8) Uani 1 1 d . . H12 H 0.2976 1.1129 0.3659 0.055 Uiso 1 1 calc R U C13 C 0.2881(4) 0.9811(4) 0.50354(17) 0.0431(8) Uani 1 1 d . . C14 C 0.2621(4) 0.9018(4) 0.4591(2) 0.0530(9) Uani 1 1 d . . H14 H 0.3275 0.8702 0.4252 0.064 Uiso 1 1 calc R U C15 C 0.1452(5) 0.8678(5) 0.4627(2) 0.0660(11) Uani 1 1 d . . H15 H 0.1311 0.8187 0.4304 0.079 Uiso 1 1 calc R U C16 C 0.0502(5) 0.9062(5) 0.5137(3) 0.0715(12) Uani 1 1 d . . H16 H -0.0275 0.8817 0.5171 0.086 Uiso 1 1 calc R U C17 C 0.0716(5) 0.9811(5) 0.5595(2) 0.0660(11) Uani 1 1 d . . H17 H 0.0083 1.0066 0.5947 0.079 Uiso 1 1 calc R U C18 C 0.1857(4) 1.0197(4) 0.55456(19) 0.0514(9) Uani 1 1 d . . H18 H 0.1952 1.073 0.5859 0.062 Uiso 1 1 calc R U C19 C 0.5668(4) 0.8714(4) 0.55917(16) 0.0425(8) Uani 1 1 d . . C20 C 0.5743(5) 0.7297(4) 0.57804(19) 0.0546(9) Uani 1 1 d . . H20 H 0.5011 0.714 0.5582 0.065 Uiso 1 1 calc R U C21 C 0.6865(6) 0.6115(5) 0.6252(2) 0.0739(14) Uani 1 1 d . . H21 H 0.6868 0.5194 0.6365 0.089 Uiso 1 1 calc R U C22 C 0.7969(6) 0.6302(6) 0.6552(2) 0.0868(17) Uani 1 1 d . . H22 H 0.872 0.5511 0.6867 0.104 Uiso 1 1 calc R U C23 C 0.7951(5) 0.7672(6) 0.6381(2) 0.0761(14) Uani 1 1 d . . H23 H 0.8695 0.7812 0.6578 0.091 Uiso 1 1 calc R U C24 C 0.6818(4) 0.8839(4) 0.59134(19) 0.0551(10) Uani 1 1 d . . H24 H 0.6823 0.9757 0.5808 0.066 Uiso 1 1 calc R U C25 C 0.6369(4) 0.5224(4) 0.38254(18) 0.0423(8) Uani 1 1 d . . C26 C 0.5625(4) 0.6600(4) 0.3370(2) 0.0588(10) Uani 1 1 d . . H26 H 0.5699 0.7428 0.3449 0.071 Uiso 1 1 calc R U C27 C 0.4770(5) 0.6716(6) 0.2795(3) 0.0773(13) Uani 1 1 d . . H27 H 0.4282 0.7624 0.2475 0.093 Uiso 1 1 calc R U C28 C 0.4633(5) 0.5496(7) 0.2692(3) 0.0812(14) Uani 1 1 d . . H28 H 0.4036 0.56 0.2306 0.097 Uiso 1 1 calc R U C29 C 0.5354(5) 0.4135(6) 0.3143(2) 0.0683(12) Uani 1 1 d . . H29 H 0.5265 0.3315 0.3061 0.082 Uiso 1 1 calc R U C30 C 0.6221(4) 0.3995(4) 0.3724(2) 0.0500(9) Uani 1 1 d . . C31 C 0.7043(4) 0.2666(4) 0.4306(2) 0.0586(10) Uani 1 1 d . . H31A H 0.7957 0.1926 0.4162 0.07 Uiso 1 1 calc R U H31B H 0.6426 0.2199 0.4468 0.07 Uiso 1 1 calc R U C32 C 0.7383(4) 0.3340(4) 0.4871(2) 0.0541(9) Uani 1 1 d . . H32A H 0.6641 0.3534 0.5206 0.065 Uiso 1 1 calc R U H32B H 0.8362 0.2659 0.5116 0.065 Uiso 1 1 calc R U C33 C 0.7336(3) 0.4807(4) 0.44925(17) 0.0420(8) Uani 1 1 d . . H33 H 0.6855 0.558 0.4768 0.05 Uiso 1 1 calc R U C34 C 0.9760(4) 0.3406(4) 0.3969(2) 0.0480(8) Uani 1 1 d . . H34A H 0.9156 0.3567 0.3556 0.058 Uiso 1 1 calc R U H34B H 1.0659 0.3444 0.3842 0.058 Uiso 1 1 calc R U H34C H 1.0013 0.244 0.4255 0.058 Uiso 1 1 calc R U C35 C 0.9772(4) 0.4446(4) 0.50361(19) 0.0517(9) Uani 1 1 d . . H35A H 0.9304 0.4278 0.5453 0.062 Uiso 1 1 calc R U H35B H 1.0819 0.3703 0.5081 0.062 Uiso 1 1 calc R U C36 C 0.9514(5) 0.6044(4) 0.48185(19) 0.0534(9) Uani 1 1 d . . H36A H 1.0428 0.6129 0.4806 0.064 Uiso 1 1 calc R U H36B H 0.8804 0.6726 0.5081 0.064 Uiso 1 1 calc R U C37 C 0.8849(4) 0.6138(4) 0.40994(18) 0.0431(8) Uani 1 1 d . . H37 H 0.7813 0.6941 0.4001 0.052 Uiso 1 1 calc R U C38 C 0.9747(4) 0.6216(4) 0.34875(19) 0.0466(8) Uani 1 1 d . . C39 C 0.9659(5) 0.6332(5) 0.2221(2) 0.0632(11) Uani 1 1 d . . C40 C 0.9802(6) 0.7747(5) 0.2045(2) 0.0825(15) Uani 1 1 d . . H40A H 1.0583 0.7664 0.2353 0.099 Uiso 1 1 calc R U H40B H 1.0041 0.7893 0.1572 0.099 Uiso 1 1 calc R U H40C H 0.8874 0.8587 0.2099 0.099 Uiso 1 1 calc R U C41 C 1.1117(6) 0.4915(5) 0.2248(3) 0.0923(16) Uani 1 1 d . . H41A H 1.1861 0.4907 0.2552 0.111 Uiso 1 1 calc R U H41B H 1.0974 0.4056 0.2421 0.111 Uiso 1 1 calc R U H41C H 1.1442 0.4881 0.1788 0.111 Uiso 1 1 calc R U C42 C 0.8449(7) 0.6408(8) 0.1753(3) 0.1056(19) Uani 1 1 d . . H42A H 0.8386 0.5492 0.1878 0.127 Uiso 1 1 calc R U H42B H 0.751 0.7238 0.1804 0.127 Uiso 1 1 calc R U H42C H 0.8678 0.6543 0.1277 0.127 Uiso 1 1 calc R U C51 C 0.0584(4) 1.2640(4) 0.98421(17) 0.0425(8) Uani 1 1 d . . C52 C -0.0177(4) 1.4118(4) 0.9928(2) 0.0560(10) Uani 1 1 d . . H52 H -0.0239 1.4291 1.0378 0.067 Uiso 1 1 calc R U C53 C -0.0845(6) 1.5342(5) 0.9378(3) 0.0781(14) Uani 1 1 d . . H53 H -0.1343 1.6306 0.9464 0.094 Uiso 1 1 calc R U C54 C -0.0776(6) 1.5138(6) 0.8705(3) 0.0830(15) Uani 1 1 d . . H54 H -0.1232 1.5955 0.8333 0.1 Uiso 1 1 calc R U C55 C -0.0029(5) 1.3720(5) 0.8593(2) 0.0685(12) Uani 1 1 d . . H55 H 0.0034 1.3567 0.8139 0.082 Uiso 1 1 calc R U C56 C 0.0640(4) 1.2500(4) 0.91451(18) 0.0518(9) Uani 1 1 d . . H56 H 0.1149 1.1545 0.9049 0.062 Uiso 1 1 calc R U C57 C 0.1526(4) 0.9636(4) 1.03706(16) 0.0409(8) Uani 1 1 d . . C58 C 0.0393(4) 0.9593(4) 0.99940(19) 0.0493(8) Uani 1 1 d . . H58 H -0.0384 1.0496 0.9754 0.059 Uiso 1 1 calc R U C59 C 0.0368(5) 0.8267(5) 0.9959(2) 0.0599(10) Uani 1 1 d . . H59 H -0.0424 0.8304 0.9704 0.072 Uiso 1 1 calc R U C60 C 0.1488(5) 0.6916(5) 1.0294(2) 0.0610(11) Uani 1 1 d . . H60 H 0.1481 0.6028 1.0264 0.073 Uiso 1 1 calc R U C61 C 0.2636(5) 0.6893(4) 1.06802(19) 0.0580(10) Uani 1 1 d . . H61 H 0.3411 0.5981 1.0915 0.07 Uiso 1 1 calc R U C62 C 0.2639(4) 0.8219(4) 1.07193(18) 0.0499(9) Uani 1 1 d . . H62 H 0.3417 0.817 1.099 0.06 Uiso 1 1 calc R U C63 C 0.0596(4) 1.1468(4) 1.12119(17) 0.0436(8) Uani 1 1 d . . C64 C -0.0962(4) 1.2234(5) 1.1203(2) 0.0600(10) Uani 1 1 d . . H64 H -0.1533 1.2685 1.0775 0.072 Uiso 1 1 calc R U C65 C -0.1691(5) 1.2349(6) 1.1809(3) 0.0776(14) Uani 1 1 d . . H65 H -0.2729 1.288 1.1781 0.093 Uiso 1 1 calc R U C66 C -0.0879(6) 1.1679(6) 1.2445(2) 0.0778(15) Uani 1 1 d . . H66 H -0.1361 1.1753 1.2852 0.093 Uiso 1 1 calc R U C67 C 0.0640(6) 1.0905(6) 1.2480(2) 0.0716(13) Uani 1 1 d . . H67 H 0.1195 1.0443 1.2911 0.086 Uiso 1 1 calc R U C68 C 0.1367(5) 1.0798(4) 1.18727(18) 0.0543(9) Uani 1 1 d . . H68 H 0.2405 1.0261 1.191 0.065 Uiso 1 1 calc R U C69 C 0.3132(4) 1.1068(4) 1.06011(16) 0.0428(8) Uani 1 1 d . . C70 C 0.3376(5) 1.2017(5) 1.09530(18) 0.0537(9) Uani 1 1 d . . H70 H 0.2574 1.2715 1.114 0.064 Uiso 1 1 calc R U C71 C 0.4756(6) 1.1959(6) 1.1034(2) 0.0694(13) Uani 1 1 d . . H71 H 0.4856 1.2612 1.1273 0.083 Uiso 1 1 calc R U C72 C 0.5983(6) 1.0956(6) 1.0769(3) 0.0794(15) Uani 1 1 d . . H72 H 0.6916 1.0903 1.0832 0.095 Uiso 1 1 calc R U C73 C 0.5780(5) 1.0034(5) 1.0405(2) 0.0724(13) Uani 1 1 d . . H73 H 0.6589 0.9358 1.0213 0.087 Uiso 1 1 calc R U C74 C 0.4395(4) 1.0089(4) 1.03187(19) 0.0535(9) Uani 1 1 d . . H74 H 0.4302 0.9454 1.0064 0.064 Uiso 1 1 calc R U C75 C 0.3380(4) 0.7290(4) 0.83233(18) 0.0487(9) Uani 1 1 d . . C76 C 0.3490(5) 0.8189(4) 0.87405(19) 0.0575(10) Uani 1 1 d . . H76 H 0.3269 0.8077 0.9202 0.069 Uiso 1 1 calc R U C77 C 0.3928(6) 0.9246(5) 0.8470(2) 0.0733(13) Uani 1 1 d . . H77 H 0.4001 0.9855 0.8748 0.088 Uiso 1 1 calc R U C78 C 0.4261(6) 0.9403(5) 0.7784(2) 0.0791(14) Uani 1 1 d . . H78 H 0.4574 1.0108 0.7607 0.095 Uiso 1 1 calc R U C79 C 0.4138(6) 0.8539(5) 0.7362(2) 0.0740(13) Uani 1 1 d . . H79 H 0.4373 0.865 0.6903 0.089 Uiso 1 1 calc R U C80 C 0.3665(5) 0.7503(4) 0.76231(18) 0.0558(10) Uani 1 1 d . . C81 C 0.3329(6) 0.6522(5) 0.7251(2) 0.0717(12) Uani 1 1 d . . H81A H 0.4243 0.5702 0.7152 0.086 Uiso 1 1 calc R U H81B H 0.2707 0.7097 0.6817 0.086 Uiso 1 1 calc R U C82 C 0.2499(5) 0.5937(5) 0.7769(2) 0.0630(11) Uani 1 1 d . . H82A H 0.2795 0.4895 0.7767 0.076 Uiso 1 1 calc R U H82B H 0.1427 0.6523 0.7649 0.076 Uiso 1 1 calc R U C83 C 0.2922(4) 0.6088(4) 0.84885(19) 0.0494(9) Uani 1 1 d . . H83 H 0.204 0.6424 0.8751 0.059 Uiso 1 1 calc R U C84 C 0.3569(5) 0.3510(5) 0.9125(2) 0.0609(10) Uani 1 1 d . . H84A H 0.3026 0.3481 0.8734 0.073 Uiso 1 1 calc R U H84B H 0.4383 0.2527 0.9305 0.073 Uiso 1 1 calc R U H84C H 0.2912 0.383 0.9483 0.073 Uiso 1 1 calc R U C85 C 0.5030(4) 0.4616(4) 0.95324(18) 0.0534(9) Uani 1 1 d . . H85A H 0.4959 0.559 0.9529 0.064 Uiso 1 1 calc R U H85B H 0.4782 0.422 0.9975 0.064 Uiso 1 1 calc R U C86 C 0.6503(4) 0.3512(4) 0.93078(19) 0.0544(9) Uani 1 1 d . . H86A H 0.6854 0.2475 0.9543 0.065 Uiso 1 1 calc R U H86B H 0.729 0.3796 0.9318 0.065 Uiso 1 1 calc R U C87 C 0.5681(4) 0.3929(4) 0.85863(17) 0.0434(8) Uani 1 1 d . . H87 H 0.5799 0.4754 0.8302 0.052 Uiso 1 1 calc R U C88 C 0.6027(4) 0.2739(4) 0.81672(19) 0.0496(9) Uani 1 1 d . . C89 C 0.8182(5) 0.1034(5) 0.7635(2) 0.0741(14) Uani 1 1 d . . C90 C 0.7366(6) 0.1527(6) 0.6929(2) 0.0866(15) Uani 1 1 d . . H90A H 0.7356 0.2439 0.6692 0.104 Uiso 1 1 calc R U H90B H 0.7859 0.0761 0.6666 0.104 Uiso 1 1 calc R U H90C H 0.6358 0.1699 0.6973 0.104 Uiso 1 1 calc R U C91 C 0.9707(6) 0.0898(10) 0.7608(5) 0.178(5) Uani 1 1 d . . H91A H 0.9641 0.1826 0.7357 0.214 Uiso 1 1 calc R U H91B H 1.0153 0.0677 0.8074 0.214 Uiso 1 1 calc R U H91C H 1.0312 0.0104 0.7377 0.214 Uiso 1 1 calc R U C92 C 0.8224(10) -0.0378(6) 0.8019(3) 0.146(3) Uani 1 1 d . . H92A H 0.7225 -0.0252 0.8027 0.175 Uiso 1 1 calc R U H92B H 0.8817 -0.1183 0.7792 0.175 Uiso 1 1 calc R U H92C H 0.8657 -0.061 0.8489 0.175 Uiso 1 1 calc R U B11 B 0.4333(4) 1.0115(4) 0.50245(19) 0.0388(8) Uani 1 1 d . . B51 B 0.1459(4) 1.1205(4) 1.04973(19) 0.0394(8) 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 O11 0.0610(16) 0.0676(17) 0.0420(14) -0.0153(12) 0.0145(12) -0.0375(14) O12 0.072(2) 0.125(3) 0.0653(19) -0.0169(18) 0.0152(15) -0.067(2) O51 0.0470(16) 0.081(2) 0.089(2) -0.0548(18) 0.0087(15) -0.0155(14) O52 0.078(2) 0.098(2) 0.097(2) -0.057(2) 0.0315(18) -0.0551(19) N11 0.0349(14) 0.0375(14) 0.0427(15) -0.0100(12) 0.0077(12) -0.0147(12) N51 0.0453(16) 0.0445(16) 0.0393(15) -0.0073(13) 0.0124(12) -0.0208(13) C1 0.0349(17) 0.0407(18) 0.0388(18) -0.0106(14) 0.0033(14) -0.0140(14) C2 0.068(2) 0.047(2) 0.043(2) -0.0124(17) -0.0010(18) -0.0185(19) C3 0.076(3) 0.063(3) 0.056(2) -0.030(2) -0.005(2) -0.016(2) C4 0.064(3) 0.047(2) 0.088(3) -0.031(2) -0.004(2) -0.017(2) C5 0.049(2) 0.041(2) 0.079(3) -0.014(2) 0.007(2) -0.0192(17) C6 0.0408(18) 0.0437(19) 0.050(2) -0.0113(16) 0.0094(16) -0.0205(16) C7 0.0423(18) 0.0291(16) 0.0380(17) -0.0095(13) 0.0062(14) -0.0175(14) C8 0.0429(19) 0.0354(18) 0.0424(19) -0.0047(14) 0.0048(15) -0.0165(15) C9 0.050(2) 0.042(2) 0.056(2) -0.0048(17) 0.0186(18) -0.0205(17) C10 0.077(3) 0.050(2) 0.039(2) -0.0092(17) 0.023(2) -0.028(2) C11 0.069(3) 0.053(2) 0.0359(19) -0.0082(17) 0.0029(18) -0.026(2) C12 0.0450(19) 0.049(2) 0.0427(19) -0.0120(16) 0.0043(16) -0.0201(17) C13 0.0441(19) 0.0390(18) 0.0424(19) -0.0049(15) 0.0061(15) -0.0179(16) C14 0.058(2) 0.054(2) 0.059(2) -0.0178(19) 0.0129(18) -0.0337(19) C15 0.070(3) 0.062(3) 0.081(3) -0.019(2) 0.006(2) -0.042(2) C16 0.059(3) 0.070(3) 0.093(3) -0.005(3) 0.012(2) -0.041(2) C17 0.056(2) 0.065(3) 0.071(3) -0.008(2) 0.026(2) -0.026(2) C18 0.053(2) 0.051(2) 0.049(2) -0.0080(17) 0.0113(17) -0.0247(18) C19 0.049(2) 0.0431(19) 0.0309(17) -0.0135(14) 0.0127(15) -0.0157(16) C20 0.066(2) 0.045(2) 0.046(2) -0.0123(17) 0.0199(18) -0.0198(19) C21 0.092(3) 0.045(2) 0.053(3) -0.001(2) 0.020(3) -0.011(2) C22 0.094(4) 0.072(3) 0.040(2) -0.003(2) -0.007(2) 0.003(3) C23 0.071(3) 0.079(3) 0.050(2) -0.020(2) -0.010(2) -0.010(3) C24 0.055(2) 0.054(2) 0.044(2) -0.0150(18) -0.0013(18) -0.0143(19) C25 0.0342(17) 0.0447(19) 0.047(2) -0.0134(16) 0.0089(15) -0.0159(15) C26 0.048(2) 0.050(2) 0.069(3) -0.007(2) -0.0046(19) -0.0169(18) C27 0.064(3) 0.073(3) 0.077(3) 0.004(3) -0.016(2) -0.025(2) C28 0.068(3) 0.103(4) 0.071(3) -0.016(3) -0.013(2) -0.040(3) C29 0.061(3) 0.078(3) 0.079(3) -0.030(3) 0.006(2) -0.039(2) C30 0.044(2) 0.054(2) 0.057(2) -0.0175(18) 0.0151(17) -0.0251(18) C31 0.053(2) 0.051(2) 0.081(3) -0.013(2) 0.017(2) -0.0320(19) C32 0.050(2) 0.058(2) 0.053(2) -0.0016(18) 0.0145(17) -0.0271(19) C33 0.0367(18) 0.0444(19) 0.0456(19) -0.0145(16) 0.0137(15) -0.0180(15) C34 0.0436(19) 0.0384(19) 0.058(2) -0.0145(17) 0.0170(17) -0.0147(16) C35 0.047(2) 0.059(2) 0.045(2) -0.0102(18) 0.0010(17) -0.0219(18) C36 0.060(2) 0.056(2) 0.050(2) -0.0179(18) 0.0066(18) -0.0295(19) C37 0.0446(19) 0.0379(18) 0.050(2) -0.0136(16) 0.0098(16) -0.0204(15) C38 0.049(2) 0.048(2) 0.047(2) -0.0080(17) 0.0066(17) -0.0274(17) C39 0.084(3) 0.067(3) 0.043(2) -0.0161(19) 0.022(2) -0.038(2) C40 0.122(4) 0.060(3) 0.061(3) -0.011(2) 0.039(3) -0.040(3) C41 0.115(4) 0.066(3) 0.088(4) -0.027(3) 0.051(3) -0.033(3) C42 0.140(5) 0.145(5) 0.051(3) -0.025(3) 0.014(3) -0.081(5) C51 0.0430(19) 0.049(2) 0.0422(19) -0.0090(16) 0.0027(15) -0.0272(17) C52 0.066(2) 0.047(2) 0.057(2) -0.0114(19) -0.002(2) -0.028(2) C53 0.086(3) 0.044(2) 0.099(4) -0.009(3) -0.008(3) -0.029(2) C54 0.103(4) 0.070(3) 0.071(3) 0.022(3) -0.026(3) -0.050(3) C55 0.096(3) 0.078(3) 0.040(2) 0.004(2) -0.005(2) -0.053(3) C56 0.063(2) 0.055(2) 0.040(2) -0.0067(17) 0.0044(17) -0.0313(19) C57 0.0480(19) 0.0450(19) 0.0312(16) -0.0117(15) 0.0131(14) -0.0218(16) C58 0.052(2) 0.053(2) 0.050(2) -0.0154(17) 0.0084(17) -0.0279(17) C59 0.075(3) 0.076(3) 0.053(2) -0.024(2) 0.016(2) -0.051(3) C60 0.096(3) 0.058(3) 0.052(2) -0.024(2) 0.030(2) -0.050(3) C61 0.077(3) 0.046(2) 0.046(2) -0.0108(17) 0.021(2) -0.024(2) C62 0.061(2) 0.050(2) 0.0387(19) -0.0126(16) 0.0088(17) -0.0257(19) C63 0.053(2) 0.048(2) 0.0416(19) -0.0163(16) 0.0109(16) -0.0314(17) C64 0.057(2) 0.083(3) 0.052(2) -0.028(2) 0.0146(19) -0.038(2) C65 0.072(3) 0.115(4) 0.076(3) -0.053(3) 0.038(3) -0.058(3) C66 0.107(4) 0.118(4) 0.061(3) -0.049(3) 0.049(3) -0.085(4) C67 0.108(4) 0.098(3) 0.039(2) -0.020(2) 0.019(2) -0.071(3) C68 0.069(3) 0.062(2) 0.040(2) -0.0123(18) 0.0127(18) -0.037(2) C69 0.049(2) 0.050(2) 0.0298(16) -0.0007(15) 0.0025(14) -0.0262(17) C70 0.068(3) 0.067(2) 0.0398(19) -0.0062(18) 0.0043(18) -0.045(2) C71 0.087(3) 0.094(3) 0.047(2) 0.009(2) -0.014(2) -0.068(3) C72 0.061(3) 0.105(4) 0.069(3) 0.028(3) -0.018(2) -0.054(3) C73 0.047(2) 0.080(3) 0.075(3) 0.011(2) 0.009(2) -0.027(2) C74 0.051(2) 0.060(2) 0.048(2) -0.0048(18) 0.0099(17) -0.0276(19) C75 0.054(2) 0.045(2) 0.0390(19) -0.0100(16) 0.0147(16) -0.0159(17) C76 0.073(3) 0.051(2) 0.042(2) -0.0148(18) 0.0184(18) -0.021(2) C77 0.112(4) 0.062(3) 0.056(3) -0.018(2) 0.017(3) -0.047(3) C78 0.126(4) 0.070(3) 0.060(3) -0.018(2) 0.034(3) -0.060(3) C79 0.116(4) 0.058(3) 0.047(2) -0.008(2) 0.029(2) -0.041(3) C80 0.077(3) 0.043(2) 0.0362(19) -0.0090(16) 0.0101(18) -0.019(2) C81 0.101(3) 0.061(3) 0.040(2) -0.007(2) 0.001(2) -0.029(3) C82 0.066(3) 0.056(2) 0.057(2) -0.007(2) -0.007(2) -0.023(2) C83 0.044(2) 0.047(2) 0.048(2) -0.0112(17) 0.0118(16) -0.0131(17) C84 0.063(2) 0.061(2) 0.063(2) -0.005(2) 0.017(2) -0.035(2) C85 0.063(2) 0.059(2) 0.0347(19) -0.0128(17) 0.0112(17) -0.025(2) C86 0.052(2) 0.059(2) 0.049(2) -0.0135(18) 0.0020(17) -0.0226(19) C87 0.0433(19) 0.0459(19) 0.0430(19) -0.0136(15) 0.0139(15) -0.0213(16) C88 0.051(2) 0.049(2) 0.047(2) -0.0140(17) 0.0070(17) -0.0210(18) C89 0.052(2) 0.076(3) 0.077(3) -0.047(3) -0.002(2) -0.005(2) C90 0.082(3) 0.101(4) 0.067(3) -0.037(3) 0.015(3) -0.027(3) C91 0.051(3) 0.257(10) 0.253(10) -0.212(9) 0.036(4) -0.036(4) C92 0.195(8) 0.063(4) 0.096(4) -0.021(3) -0.005(5) 0.009(4) B11 0.039(2) 0.039(2) 0.038(2) -0.0112(16) 0.0060(16) -0.0165(17) B51 0.047(2) 0.041(2) 0.0319(19) -0.0088(16) 0.0055(16) -0.0215(18) 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 0 '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 0.006 '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 C38 O11 C39 121.6(3) C88 O51 C89 122.2(3) C34 N11 C35 114.0(3) C34 N11 C33 114.0(3) C35 N11 C33 111.4(3) C34 N11 C37 116.9(3) C35 N11 C37 88.2(2) C33 N11 C37 109.8(2) C84 N51 C85 108.4(3) C84 N51 C83 110.0(3) C85 N51 C83 118.2(3) C84 N51 C87 114.9(3) C85 N51 C87 86.5(2) C83 N51 C87 117.1(3) C6 C1 C2 113.9(3) C6 C1 B11 123.3(3) C2 C1 B11 122.8(3) C3 C2 C1 123.1(4) C3 C2 H2 118.5 C1 C2 H2 118.5 C4 C3 C2 120.5(4) C4 C3 H3 119.8 C2 C3 H3 119.8 C3 C4 C5 118.7(4) C3 C4 H4 120.6 C5 C4 H4 120.6 C4 C5 C6 120.4(4) C4 C5 H5 119.8 C6 C5 H5 119.8 C5 C6 C1 123.4(3) C5 C6 H6 118.3 C1 C6 H6 118.3 C12 C7 C8 114.4(3) C12 C7 B11 123.1(3) C8 C7 B11 122.3(3) C9 C8 C7 123.0(3) C9 C8 H8 118.5 C7 C8 H8 118.5 C10 C9 C8 119.9(3) C10 C9 H9 120 C8 C9 H9 120 C9 C10 C11 119.5(3) C9 C10 H10 120.3 C11 C10 H10 120.3 C10 C11 C12 119.7(3) C10 C11 H11 120.1 C12 C11 H11 120.1 C11 C12 C7 123.4(3) C11 C12 H12 118.3 C7 C12 H12 118.3 C14 C13 C18 113.7(3) C14 C13 B11 123.7(3) C18 C13 B11 122.3(3) C15 C14 C13 123.9(4) C15 C14 H14 118.1 C13 C14 H14 118.1 C16 C15 C14 120.1(4) C16 C15 H15 120 C14 C15 H15 120 C17 C16 C15 118.7(4) C17 C16 H16 120.6 C15 C16 H16 120.6 C16 C17 C18 121.3(4) C16 C17 H17 119.3 C18 C17 H17 119.3 C17 C18 C13 122.2(4) C17 C18 H18 118.9 C13 C18 H18 118.9 C24 C19 C20 114.5(3) C24 C19 B11 123.0(3) C20 C19 B11 122.5(3) C21 C20 C19 122.7(4) C21 C20 H20 118.7 C19 C20 H20 118.7 C22 C21 C20 120.3(5) C22 C21 H21 119.8 C20 C21 H21 119.8 C21 C22 C23 119.3(4) C21 C22 H22 120.4 C23 C22 H22 120.4 C22 C23 C24 119.6(5) C22 C23 H23 120.2 C24 C23 H23 120.2 C23 C24 C19 123.6(4) C23 C24 H24 118.2 C19 C24 H24 118.2 C26 C25 C30 121.2(3) C26 C25 C33 129.0(3) C30 C25 C33 109.8(3) C27 C26 C25 118.4(4) C27 C26 H26 120.8 C25 C26 H26 120.8 C28 C27 C26 120.4(4) C28 C27 H27 119.8 C26 C27 H27 119.8 C29 C28 C27 121.6(4) C29 C28 H28 119.2 C27 C28 H28 119.2 C28 C29 C30 118.9(4) C28 C29 H29 120.5 C30 C29 H29 120.5 C25 C30 C29 119.5(4) C25 C30 C31 111.5(3) C29 C30 C31 129.0(4) C30 C31 C32 103.2(3) C30 C31 H31A 111.1 C32 C31 H31A 111.1 C30 C31 H31B 111.1 C32 C31 H31B 111.1 H31A C31 H31B 109.1 C33 C32 C31 106.1(3) C33 C32 H32A 110.5 C31 C32 H32A 110.5 C33 C32 H32B 110.5 C31 C32 H32B 110.5 H32A C32 H32B 108.7 C25 C33 C32 103.5(3) C25 C33 N11 112.6(3) C32 C33 N11 111.3(3) C25 C33 H33 109.7 C32 C33 H33 109.7 N11 C33 H33 109.7 N11 C34 H34A 109.5 N11 C34 H34B 109.5 H34A C34 H34B 109.5 N11 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 C36 C35 N11 91.5(3) C36 C35 H35A 113.4 N11 C35 H35A 113.4 C36 C35 H35B 113.4 N11 C35 H35B 113.4 H35A C35 H35B 110.7 C35 C36 C37 89.3(3) C35 C36 H36A 113.8 C37 C36 H36A 113.8 C35 C36 H36B 113.8 C37 C36 H36B 113.8 H36A C36 H36B 111 C38 C37 C36 117.1(3) C38 C37 N11 115.0(3) C36 C37 N11 90.0(3) C38 C37 H37 111.1 C36 C37 H37 111.1 N11 C37 H37 111.1 O12 C38 O11 128.0(3) O12 C38 C37 122.8(3) O11 C38 C37 109.2(3) C42 C39 C40 111.5(5) C42 C39 O11 101.3(4) C40 C39 O11 109.3(3) C42 C39 C41 111.9(4) C40 C39 C41 113.8(4) O11 C39 C41 108.3(3) C39 C40 H40A 109.5 C39 C40 H40B 109.5 H40A C40 H40B 109.5 C39 C40 H40C 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 C39 C41 H41A 109.5 C39 C41 H41B 109.5 H41A C41 H41B 109.5 C39 C41 H41C 109.5 H41A C41 H41C 109.5 H41B C41 H41C 109.5 C39 C42 H42A 109.5 C39 C42 H42B 109.5 H42A C42 H42B 109.5 C39 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 C52 C51 C56 113.9(3) C52 C51 B51 122.8(3) C56 C51 B51 123.1(3) C53 C52 C51 123.4(4) C53 C52 H52 118.3 C51 C52 H52 118.3 C54 C53 C52 120.2(4) C54 C53 H53 119.9 C52 C53 H53 119.9 C55 C54 C53 118.7(4) C55 C54 H54 120.7 C53 C54 H54 120.7 C54 C55 C56 120.9(4) C54 C55 H55 119.6 C56 C55 H55 119.6 C55 C56 C51 122.9(4) C55 C56 H56 118.6 C51 C56 H56 118.6 C58 C57 C62 114.0(3) C58 C57 B51 123.4(3) C62 C57 B51 122.0(3) C59 C58 C57 123.2(4) C59 C58 H58 118.4 C57 C58 H58 118.4 C60 C59 C58 120.7(4) C60 C59 H59 119.7 C58 C59 H59 119.7 C59 C60 C61 118.6(4) C59 C60 H60 120.7 C61 C60 H60 120.7 C60 C61 C62 120.2(4) C60 C61 H61 119.9 C62 C61 H61 119.9 C61 C62 C57 123.3(4) C61 C62 H62 118.4 C57 C62 H62 118.4 C68 C63 C64 115.1(3) C68 C63 B51 121.8(3) C64 C63 B51 122.8(3) C65 C64 C63 122.6(4) C65 C64 H64 118.7 C63 C64 H64 118.7 C66 C65 C64 119.9(4) C66 C65 H65 120 C64 C65 H65 120 C67 C66 C65 119.6(4) C67 C66 H66 120.2 C65 C66 H66 120.2 C66 C67 C68 120.4(4) C66 C67 H67 119.8 C68 C67 H67 119.8 C67 C68 C63 122.4(4) C67 C68 H68 118.8 C63 C68 H68 118.8 C74 C69 C70 114.4(3) C74 C69 B51 124.2(3) C70 C69 B51 121.3(3) C71 C70 C69 122.8(4) C71 C70 H70 118.6 C69 C70 H70 118.6 C72 C71 C70 121.4(4) C72 C71 H71 119.3 C70 C71 H71 119.3 C73 C72 C71 117.5(4) C73 C72 H72 121.3 C71 C72 H72 121.3 C72 C73 C74 121.5(5) C72 C73 H73 119.2 C74 C73 H73 119.2 C73 C74 C69 122.3(4) C73 C74 H74 118.8 C69 C74 H74 118.8 C76 C75 C80 119.7(3) C76 C75 C83 130.0(3) C80 C75 C83 110.3(3) C77 C76 C75 119.7(4) C77 C76 H76 120.1 C75 C76 H76 120.1 C76 C77 C78 119.8(4) C76 C77 H77 120.1 C78 C77 H77 120.1 C79 C78 C77 121.2(4) C79 C78 H78 119.4 C77 C78 H78 119.4 C78 C79 C80 119.4(4) C78 C79 H79 120.3 C80 C79 H79 120.3 C79 C80 C75 120.1(4) C79 C80 C81 129.1(4) C75 C80 C81 110.8(3) C80 C81 C82 103.3(3) C80 C81 H81A 111.1 C82 C81 H81A 111.1 C80 C81 H81B 111.1 C82 C81 H81B 111.1 H81A C81 H81B 109.1 C81 C82 C83 106.5(3) C81 C82 H82A 110.4 C83 C82 H82A 110.4 C81 C82 H82B 110.4 C83 C82 H82B 110.4 H82A C82 H82B 108.6 C75 C83 C82 103.5(3) C75 C83 N51 113.2(3) C82 C83 N51 111.2(3) C75 C83 H83 109.6 C82 C83 H83 109.6 N51 C83 H83 109.6 N51 C84 H84A 109.5 N51 C84 H84B 109.5 H84A C84 H84B 109.5 N51 C84 H84C 109.5 H84A C84 H84C 109.5 H84B C84 H84C 109.5 C86 C85 N51 90.6(3) C86 C85 H85A 113.5 N51 C85 H85A 113.5 C86 C85 H85B 113.5 N51 C85 H85B 113.5 H85A C85 H85B 110.8 C85 C86 C87 87.2(3) C85 C86 H86A 114.1 C87 C86 H86A 114.1 C85 C86 H86B 114.1 C87 C86 H86B 114.1 H86A C86 H86B 111.3 C88 C87 C86 120.0(3) C88 C87 N51 119.2(3) C86 C87 N51 90.3(2) C88 C87 H87 108.6 C86 C87 H87 108.6 N51 C87 H87 108.6 O52 C88 O51 126.6(3) O52 C88 C87 126.5(3) O51 C88 C87 106.9(3) C92 C89 C91 111.6(6) C92 C89 C90 111.2(5) C91 C89 C90 112.3(5) C92 C89 O51 109.2(4) C91 C89 O51 102.3(4) C90 C89 O51 109.8(4) C89 C90 H90A 109.5 C89 C90 H90B 109.5 H90A C90 H90B 109.5 C89 C90 H90C 109.5 H90A C90 H90C 109.5 H90B C90 H90C 109.5 C89 C91 H91A 109.5 C89 C91 H91B 109.5 H91A C91 H91B 109.5 C89 C91 H91C 109.5 H91A C91 H91C 109.5 H91B C91 H91C 109.5 C89 C92 H92A 109.5 C89 C92 H92B 109.5 H92A C92 H92B 109.5 C89 C92 H92C 109.5 H92A C92 H92C 109.5 H92B C92 H92C 109.5 C13 B11 C7 111.3(3) C13 B11 C1 111.5(3) C7 B11 C1 108.1(3) C13 B11 C19 107.3(3) C7 B11 C19 109.2(3) C1 B11 C19 109.3(3) C51 B51 C69 104.5(3) C51 B51 C63 112.0(3) C69 B51 C63 111.2(3) C51 B51 C57 113.7(3) C69 B51 C57 112.5(3) C63 B51 C57 103.1(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O11 C38 1.315(4) O11 C39 1.506(4) O12 C38 1.192(4) O51 C88 1.316(4) O51 C89 1.492(5) O52 C88 1.193(4) N11 C34 1.483(4) N11 C35 1.528(4) N11 C33 1.535(4) N11 C37 1.548(4) N51 C84 1.497(5) N51 C85 1.533(4) N51 C83 1.534(4) N51 C87 1.538(4) C1 C6 1.397(5) C1 C2 1.403(5) C1 B11 1.655(5) C2 C3 1.384(5) C2 H2 0.93 C3 C4 1.369(6) C3 H3 0.93 C4 C5 1.371(6) C4 H4 0.93 C5 C6 1.383(5) C5 H5 0.93 C6 H6 0.93 C7 C12 1.396(5) C7 C8 1.398(4) C7 B11 1.648(5) C8 C9 1.395(5) C8 H8 0.93 C9 C10 1.368(5) C9 H9 0.93 C10 C11 1.375(6) C10 H10 0.93 C11 C12 1.387(5) C11 H11 0.93 C12 H12 0.93 C13 C14 1.401(5) C13 C18 1.412(5) C13 B11 1.641(5) C14 C15 1.381(6) C14 H14 0.93 C15 C16 1.367(6) C15 H15 0.93 C16 C17 1.366(6) C16 H16 0.93 C17 C18 1.384(6) C17 H17 0.93 C18 H18 0.93 C19 C24 1.397(5) C19 C20 1.400(5) C19 B11 1.658(5) C20 C21 1.390(6) C20 H20 0.93 C21 C22 1.373(7) C21 H21 0.93 C22 C23 1.377(7) C22 H22 0.93 C23 C24 1.385(6) C23 H23 0.93 C24 H24 0.93 C25 C26 1.382(5) C25 C30 1.389(5) C25 C33 1.507(5) C26 C27 1.380(6) C26 H26 0.93 C27 C28 1.375(7) C27 H27 0.93 C28 C29 1.366(7) C28 H28 0.93 C29 C30 1.389(5) C29 H29 0.93 C30 C31 1.493(5) C31 C32 1.531(5) C31 H31A 0.97 C31 H31B 0.97 C32 C33 1.530(5) C32 H32A 0.97 C32 H32B 0.97 C33 H33 0.98 C34 H34A 0.96 C34 H34B 0.96 C34 H34C 0.96 C35 C36 1.513(5) C35 H35A 0.97 C35 H35B 0.97 C36 C37 1.534(5) C36 H36A 0.97 C36 H36B 0.97 C37 C38 1.515(5) C37 H37 0.98 C39 C42 1.501(7) C39 C40 1.504(6) C39 C41 1.511(7) C40 H40A 0.96 C40 H40B 0.96 C40 H40C 0.96 C41 H41A 0.96 C41 H41B 0.96 C41 H41C 0.96 C42 H42A 0.96 C42 H42B 0.96 C42 H42C 0.96 C51 C52 1.393(5) C51 C56 1.400(5) C51 B51 1.642(5) C52 C53 1.383(6) C52 H52 0.93 C53 C54 1.371(7) C53 H53 0.93 C54 C55 1.357(7) C54 H54 0.93 C55 C56 1.383(5) C55 H55 0.93 C56 H56 0.93 C57 C58 1.391(5) C57 C62 1.404(5) C57 B51 1.649(5) C58 C59 1.390(5) C58 H58 0.93 C59 C60 1.361(6) C59 H59 0.93 C60 C61 1.380(6) C60 H60 0.93 C61 C62 1.381(5) C61 H61 0.93 C62 H62 0.93 C63 C68 1.393(5) C63 C64 1.399(5) C63 B51 1.647(5) C64 C65 1.391(6) C64 H64 0.93 C65 C66 1.369(7) C65 H65 0.93 C66 C67 1.361(7) C66 H66 0.93 C67 C68 1.392(5) C67 H67 0.93 C68 H68 0.93 C69 C74 1.402(5) C69 C70 1.404(5) C69 B51 1.646(5) C70 C71 1.381(6) C70 H70 0.93 C71 C72 1.374(7) C71 H71 0.93 C72 C73 1.373(7) C72 H72 0.93 C73 C74 1.390(6) C73 H73 0.93 C74 H74 0.93 C75 C76 1.385(5) C75 C80 1.400(5) C75 C83 1.493(5) C76 C77 1.374(6) C76 H76 0.93 C77 C78 1.384(6) C77 H77 0.93 C78 C79 1.368(6) C78 H78 0.93 C79 C80 1.376(6) C79 H79 0.93 C80 C81 1.506(6) C81 C82 1.528(6) C81 H81A 0.97 C81 H81B 0.97 C82 C83 1.533(5) C82 H82A 0.97 C82 H82B 0.97 C83 H83 0.98 C84 H84A 0.96 C84 H84B 0.96 C84 H84C 0.96 C85 C86 1.524(5) C85 H85A 0.97 C85 H85B 0.97 C86 C87 1.528(5) C86 H86A 0.97 C86 H86B 0.97 C87 C88 1.508(5) C87 H87 0.98 C89 C92 1.486(9) C89 C91 1.488(8) C89 C90 1.489(6) C90 H90A 0.96 C90 H90B 0.96 C90 H90C 0.96 C91 H91A 0.96 C91 H91B 0.96 C91 H91C 0.96 C92 H92A 0.96 C92 H92B 0.96 C92 H92C 0.96 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 C6 C1 C2 C3 0.4(5) B11 C1 C2 C3 180.0(4) C1 C2 C3 C4 -1.9(7) C2 C3 C4 C5 1.1(6) C3 C4 C5 C6 1.1(6) C4 C5 C6 C1 -2.6(6) C2 C1 C6 C5 1.8(5) B11 C1 C6 C5 -177.8(3) C12 C7 C8 C9 -1.1(5) B11 C7 C8 C9 -176.6(3) C7 C8 C9 C10 -0.6(5) C8 C9 C10 C11 1.6(5) C9 C10 C11 C12 -0.7(6) C10 C11 C12 C7 -1.1(5) C8 C7 C12 C11 2.0(5) B11 C7 C12 C11 177.4(3) C18 C13 C14 C15 1.9(5) B11 C13 C14 C15 175.8(4) C13 C14 C15 C16 -2.9(7) C14 C15 C16 C17 1.4(7) C15 C16 C17 C18 0.8(7) C16 C17 C18 C13 -1.6(6) C14 C13 C18 C17 0.3(5) B11 C13 C18 C17 -173.6(4) C24 C19 C20 C21 0.3(5) B11 C19 C20 C21 179.5(3) C19 C20 C21 C22 -0.4(6) C20 C21 C22 C23 0.0(7) C21 C22 C23 C24 0.4(7) C22 C23 C24 C19 -0.5(6) C20 C19 C24 C23 0.1(5) B11 C19 C24 C23 -179.1(4) C30 C25 C26 C27 -2.3(6) C33 C25 C26 C27 -178.5(4) C25 C26 C27 C28 1.8(7) C26 C27 C28 C29 -1.3(8) C27 C28 C29 C30 1.2(7) C26 C25 C30 C29 2.3(5) C33 C25 C30 C29 179.2(3) C26 C25 C30 C31 -176.2(3) C33 C25 C30 C31 0.7(4) C28 C29 C30 C25 -1.7(6) C28 C29 C30 C31 176.5(4) C25 C30 C31 C32 14.0(4) C29 C30 C31 C32 -164.2(4) C30 C31 C32 C33 -22.9(4) C26 C25 C33 C32 161.4(4) C30 C25 C33 C32 -15.2(4) C26 C25 C33 N11 -78.2(4) C30 C25 C33 N11 105.2(3) C31 C32 C33 C25 23.3(3) C31 C32 C33 N11 -97.9(3) C34 N11 C33 C25 -59.3(4) C35 N11 C33 C25 170.0(3) C37 N11 C33 C25 74.0(3) C34 N11 C33 C32 56.5(4) C35 N11 C33 C32 -74.2(3) C37 N11 C33 C32 -170.2(3) C34 N11 C35 C36 126.3(3) C33 N11 C35 C36 -103.0(3) C37 N11 C35 C36 7.6(3) N11 C35 C36 C37 -7.6(3) C35 C36 C37 C38 -110.8(3) C35 C36 C37 N11 7.5(3) C34 N11 C37 C38 -3.4(4) C35 N11 C37 C38 112.7(3) C33 N11 C37 C38 -135.2(3) C34 N11 C37 C36 -123.5(3) C35 N11 C37 C36 -7.4(3) C33 N11 C37 C36 104.6(3) C39 O11 C38 O12 0.8(6) C39 O11 C38 C37 179.1(3) C36 C37 C38 O12 -4.0(5) N11 C37 C38 O12 -107.8(4) C36 C37 C38 O11 177.7(3) N11 C37 C38 O11 73.9(4) C38 O11 C39 C42 -176.9(4) C38 O11 C39 C40 -59.1(5) C38 O11 C39 C41 65.3(5) C56 C51 C52 C53 1.2(6) B51 C51 C52 C53 176.2(4) C51 C52 C53 C54 -0.3(7) C52 C53 C54 C55 -0.7(7) C53 C54 C55 C56 0.6(7) C54 C55 C56 C51 0.5(7) C52 C51 C56 C55 -1.3(5) B51 C51 C56 C55 -176.3(3) C62 C57 C58 C59 -0.5(5) B51 C57 C58 C59 -171.9(3) C57 C58 C59 C60 -0.8(6) C58 C59 C60 C61 1.2(6) C59 C60 C61 C62 -0.3(6) C60 C61 C62 C57 -1.2(6) C58 C57 C62 C61 1.5(5) B51 C57 C62 C61 173.0(3) C68 C63 C64 C65 1.3(6) B51 C63 C64 C65 174.7(4) C63 C64 C65 C66 -0.9(7) C64 C65 C66 C67 0.0(7) C65 C66 C67 C68 0.4(7) C66 C67 C68 C63 0.1(6) C64 C63 C68 C67 -0.9(5) B51 C63 C68 C67 -174.4(4) C74 C69 C70 C71 -2.0(5) B51 C69 C70 C71 -178.3(3) C69 C70 C71 C72 0.2(6) C70 C71 C72 C73 1.4(6) C71 C72 C73 C74 -1.2(6) C72 C73 C74 C69 -0.7(6) C70 C69 C74 C73 2.2(5) B51 C69 C74 C73 178.4(3) C80 C75 C76 C77 -2.2(6) C83 C75 C76 C77 -179.4(4) C75 C76 C77 C78 -0.2(7) C76 C77 C78 C79 1.1(8) C77 C78 C79 C80 0.5(8) C78 C79 C80 C75 -3.0(7) C78 C79 C80 C81 174.7(5) C76 C75 C80 C79 3.8(6) C83 C75 C80 C79 -178.5(4) C76 C75 C80 C81 -174.2(4) C83 C75 C80 C81 3.5(5) C79 C80 C81 C82 -166.4(4) C75 C80 C81 C82 11.5(5) C80 C81 C82 C83 -21.5(4) C76 C75 C83 C82 160.6(4) C80 C75 C83 C82 -16.8(4) C76 C75 C83 N51 -79.0(5) C80 C75 C83 N51 103.7(4) C81 C82 C83 C75 23.5(4) C81 C82 C83 N51 -98.3(4) C84 N51 C83 C75 172.5(3) C85 N51 C83 C75 47.4(4) C87 N51 C83 C75 -53.9(4) C84 N51 C83 C82 -71.4(4) C85 N51 C83 C82 163.5(3) C87 N51 C83 C82 62.2(4) C84 N51 C85 C86 97.6(3) C83 N51 C85 C86 -136.6(3) C87 N51 C85 C86 -17.5(3) N51 C85 C86 C87 17.7(3) C85 C86 C87 C88 -142.1(3) C85 C86 C87 N51 -17.6(3) C84 N51 C87 C88 34.0(4) C85 N51 C87 C88 142.6(3) C83 N51 C87 C88 -97.4(4) C84 N51 C87 C86 -91.2(3) C85 N51 C87 C86 17.5(3) C83 N51 C87 C86 137.5(3) C89 O51 C88 O52 -0.5(6) C89 O51 C88 C87 -179.8(4) C86 C87 C88 O52 118.0(5) N51 C87 C88 O52 8.8(6) C86 C87 C88 O51 -62.7(4) N51 C87 C88 O51 -171.8(3) C88 O51 C89 C92 -64.0(6) C88 O51 C89 C91 177.6(5) C88 O51 C89 C90 58.1(6) C14 C13 B11 C7 28.1(5) C18 C13 B11 C7 -158.6(3) C14 C13 B11 C1 148.9(3) C18 C13 B11 C1 -37.8(4) C14 C13 B11 C19 -91.4(4) C18 C13 B11 C19 81.9(4) C12 C7 B11 C13 36.1(4) C8 C7 B11 C13 -148.9(3) C12 C7 B11 C1 -86.7(4) C8 C7 B11 C1 88.3(3) C12 C7 B11 C19 154.4(3) C8 C7 B11 C19 -30.6(4) C6 C1 B11 C13 -103.7(4) C2 C1 B11 C13 76.8(4) C6 C1 B11 C7 18.9(4) C2 C1 B11 C7 -160.6(3) C6 C1 B11 C19 137.7(3) C2 C1 B11 C19 -41.7(4) C24 C19 B11 C13 -155.6(3) C20 C19 B11 C13 25.3(4) C24 C19 B11 C7 83.6(4) C20 C19 B11 C7 -95.6(4) C24 C19 B11 C1 -34.5(4) C20 C19 B11 C1 146.3(3) C52 C51 B51 C69 -86.2(4) C56 C51 B51 C69 88.3(4) C52 C51 B51 C63 34.3(4) C56 C51 B51 C63 -151.1(3) C52 C51 B51 C57 150.7(3) C56 C51 B51 C57 -34.7(4) C74 C69 B51 C51 -96.5(4) C70 C69 B51 C51 79.4(4) C74 C69 B51 C63 142.4(3) C70 C69 B51 C63 -41.7(4) C74 C69 B51 C57 27.3(4) C70 C69 B51 C57 -156.8(3) C68 C63 B51 C51 -151.8(3) C64 C63 B51 C51 35.3(4) C68 C63 B51 C69 -35.2(4) C64 C63 B51 C69 151.8(3) C68 C63 B51 C57 85.6(4) C64 C63 B51 C57 -87.4(4) C58 C57 B51 C51 -33.4(5) C62 C57 B51 C51 155.8(3) C58 C57 B51 C69 -152.0(3) C62 C57 B51 C69 37.3(4) C58 C57 B51 C63 88.1(4) C62 C57 B51 C63 -82.7(4)