#------------------------------------------------------------------------------ #$Date: 2020-05-14 02:50:47 +0300 (Thu, 14 May 2020) $ #$Revision: 252033 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/65/7126533.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_7126533 loop_ _publ_author_name 'Ohtani, Shunsuke' 'Nakamura, Masashi' 'Gon, Masayuki' 'Tanaka, Kazuo' 'Chujo, Yoshiki' _publ_section_title ; Synthesis of fully-fused bisboron azomethine complexes and their conjugated polymers with solid-state near-infrared emission ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D0CC02301A _journal_year 2020 _chemical_formula_sum 'C58 H42 B2 N2 O4' _chemical_formula_weight 852.60 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-03-30 deposited with the CCDC. 2020-05-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.353(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 17.8827(11) _cell_length_b 7.8947(5) _cell_length_c 15.7916(10) _cell_measurement_reflns_used 16890 _cell_measurement_temperature 106 _cell_measurement_theta_max 54.73 _cell_measurement_theta_min 3.65 _cell_volume 2215.7(2) _computing_cell_refinement PROCESS-AUTO _computing_data_collection PROCESS-AUTO _computing_data_reduction 'Yadokari-XG (Wakita, 2000)' _computing_molecular_graphics 'Yadokari-XG (Wakita, 2000)' _computing_publication_material 'Yadokari-XG (Wakita, 2000)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 106 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'rigaku raxis rapid' _diffrn_measurement_method 'oscillation method' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.1176 _diffrn_reflns_av_unetI/netI 0.1127 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 18946 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.386 _diffrn_reflns_theta_min 2.596 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_T_max 1.2050 _exptl_absorpt_correction_T_min 0.7949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 892 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.317 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 298 _refine_ls_number_reflns 5005 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.144 _refine_ls_R_factor_all 0.1561 _refine_ls_R_factor_gt 0.0978 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+0.6115P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1732 _refine_ls_wR_factor_ref 0.1953 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3378 _reflns_number_total 5005 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc02301a2.cif _cod_data_source_block anti_bisBAm _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7126533 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.977 _shelx_estimated_absorpt_t_max 0.984 _shelx_res_file ; bisBAm_a.res created by SHELXL-2014/7 TITL bisBAm_a.res in P2(1)/c REM Yadorkari-X generated CELL 0.71075 17.8827 7.8947 15.7916 90.0000 96.3530 90.0000 ZERR 2.0 0.0011 0.0005 0.0010 0.0000 0.0070 0.0000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z REM SPGR P21/c monoclinic SFAC C H O N B UNIT 116 84 8 4 4 L.S. 50 FMAP 2 PLAN -20 ACTA CONF LIST 4 BOND $H OMIT 2 0 0 WGHT 0.080100 0.611500 FVAR 0.56345 O001 3 0.391458 0.592329 0.602298 11.00000 0.01487 0.02571 = 0.01726 -0.00469 0.00393 -0.00333 O002 3 0.259295 0.614531 0.618569 11.00000 0.01696 0.02664 = 0.01688 -0.00045 0.00277 0.00022 N003 4 0.702022 0.568555 0.496116 11.00000 0.01658 0.01735 = 0.01668 0.00041 0.00326 -0.00257 C004 1 0.443822 0.547254 0.551920 11.00000 0.01861 0.01722 = 0.01500 0.00459 0.00262 0.00074 C005 1 0.516467 0.610008 0.568862 11.00000 0.01877 0.01583 = 0.01810 0.00118 -0.00106 -0.00219 AFIX 43 H1 2 0.527946 0.684739 0.613954 11.00000 -1.20000 AFIX 0 C006 1 0.572483 0.561650 0.518618 11.00000 0.01873 0.01508 = 0.01664 0.00208 0.00305 -0.00061 C007 1 0.650387 0.605248 0.544211 11.00000 0.01907 0.01427 = 0.01812 0.00133 0.00035 -0.00160 AFIX 43 H2 2 0.663370 0.660250 0.595825 11.00000 -1.20000 AFIX 0 C008 1 0.931134 0.601079 0.584342 11.00000 0.01529 0.03382 = 0.02199 0.00054 0.00103 -0.00751 AFIX 43 H3 2 0.982011 0.605576 0.604301 11.00000 -1.20000 AFIX 0 C009 1 0.903347 0.466362 0.532578 11.00000 0.01595 0.02563 = 0.02666 -0.00061 0.00627 -0.00138 AFIX 43 H4 2 0.935743 0.381429 0.518306 11.00000 -1.20000 AFIX 0 C00A 1 0.395710 0.252375 0.681138 11.00000 0.02684 0.02884 = 0.01710 0.00053 -0.00001 -0.00196 AFIX 43 H5 2 0.439349 0.303515 0.666545 11.00000 -1.20000 AFIX 0 C00B 1 0.153654 0.795519 0.592423 11.00000 0.01518 0.02304 = 0.02337 -0.00617 0.00437 -0.00310 C00C 1 0.883458 0.727056 0.605865 11.00000 0.02433 0.02631 = 0.02163 -0.00561 0.00300 -0.00764 AFIX 43 H6 2 0.902430 0.816012 0.640409 11.00000 -1.20000 AFIX 0 C00D 1 0.827370 0.459251 0.502432 11.00000 0.01914 0.02179 = 0.01753 -0.00037 0.00531 -0.00455 C00E 1 0.780219 0.588018 0.525736 11.00000 0.01231 0.02018 = 0.02022 0.00249 0.00124 -0.00380 C00F 1 0.132842 0.746862 0.671506 11.00000 0.01766 0.02543 = 0.02633 -0.00328 0.00619 -0.00490 AFIX 43 H7 2 0.152416 0.647972 0.697171 11.00000 -1.20000 AFIX 0 C00G 1 0.807560 0.722735 0.576632 11.00000 0.01569 0.02265 = 0.02430 -0.00234 0.00259 -0.00116 AFIX 43 H8 2 0.775500 0.808425 0.590811 11.00000 -1.20000 AFIX 0 C00H 1 0.210712 0.688241 0.550049 11.00000 0.01587 0.02387 = 0.01383 0.00098 -0.00069 -0.00198 C00I 1 0.326383 0.334100 0.660273 11.00000 0.02055 0.02565 = 0.01380 -0.00180 0.00233 -0.00286 C00J 1 0.082866 0.845512 0.712372 11.00000 0.01901 0.03844 = 0.02667 -0.00935 0.00662 -0.00927 AFIX 43 H9 2 0.069663 0.812766 0.765302 11.00000 -1.20000 AFIX 0 C00K 1 0.348449 0.975113 0.388961 11.00000 0.02908 0.01751 = 0.03018 0.00344 0.01327 -0.00064 AFIX 43 H10 2 0.379897 1.031716 0.355288 11.00000 -1.20000 AFIX 0 C00L 1 0.241798 0.794605 0.403004 11.00000 0.02147 0.01901 = 0.02224 -0.00337 0.00454 0.00091 AFIX 43 H11 2 0.201039 0.733023 0.377497 11.00000 -1.20000 AFIX 0 C00M 1 0.256197 0.796339 0.491341 11.00000 0.01543 0.01748 = 0.02298 0.00113 0.00496 0.00284 C00N 1 0.316274 0.894934 0.527855 11.00000 0.02268 0.02313 = 0.02020 -0.00018 0.00262 0.00189 AFIX 43 H12 2 0.325547 0.902622 0.586849 11.00000 -1.20000 AFIX 0 C00O 1 0.362084 0.981161 0.477456 11.00000 0.02256 0.01715 = 0.03442 -0.00022 0.00252 -0.00266 AFIX 43 H13 2 0.402470 1.043923 0.502958 11.00000 -1.20000 AFIX 0 C00P 1 0.287179 0.883280 0.351742 11.00000 0.03208 0.02275 = 0.02225 0.00006 0.00570 0.00391 AFIX 43 H14 2 0.276400 0.880858 0.292775 11.00000 -1.20000 AFIX 0 C00Q 1 0.122383 0.941762 0.554740 11.00000 0.02629 0.03138 = 0.02765 0.00077 0.00498 0.00247 AFIX 43 H15 2 0.135208 0.975042 0.501729 11.00000 -1.20000 AFIX 0 C00R 1 0.262354 0.253814 0.685726 11.00000 0.02646 0.02941 = 0.01974 -0.00348 0.00260 -0.00543 AFIX 43 H16 2 0.215577 0.305194 0.673781 11.00000 -1.20000 AFIX 0 C00S 1 0.053002 0.991759 0.674247 11.00000 0.01866 0.03341 = 0.03892 -0.01497 0.00682 0.00396 AFIX 43 H17 2 0.020115 1.058057 0.701746 11.00000 -1.20000 AFIX 0 C00T 1 0.400991 0.096983 0.723045 11.00000 0.04276 0.03233 = 0.01871 0.00143 -0.00156 0.00570 AFIX 43 H18 2 0.447513 0.044610 0.735302 11.00000 -1.20000 AFIX 0 C00U 1 0.072064 1.039355 0.595224 11.00000 0.02719 0.03537 = 0.03894 -0.00039 0.00454 0.00522 AFIX 43 H19 2 0.051277 1.136637 0.569048 11.00000 -1.20000 AFIX 0 C00V 1 0.336452 0.020670 0.746428 11.00000 0.06271 0.02469 = 0.01735 0.00159 0.00575 -0.00999 AFIX 43 H20 2 0.339676 -0.083340 0.774243 11.00000 -1.20000 AFIX 0 C00W 1 0.267310 0.099051 0.728434 11.00000 0.03948 0.03125 = 0.02084 -0.00274 0.00665 -0.01247 AFIX 43 H21 2 0.224192 0.048509 0.744822 11.00000 -1.20000 AFIX 0 B00X 5 0.318632 0.500805 0.600561 11.00000 0.01697 0.02288 = 0.01676 -0.00190 0.00328 -0.00392 HKLF 4 REM bisBAm_a.res in P2(1)/c REM R1 = 0.0978 for 3378 Fo > 4sig(Fo) and 0.1561 for all 5005 data REM 298 parameters refined using 0 restraints END WGHT 0.0444 1.6743 REM Highest difference peak 0.317, deepest hole -0.320, 1-sigma level 0.066 Q1 1 0.2954 0.3429 0.7004 11.00000 0.05 0.32 Q2 1 0.2313 0.7625 0.5182 11.00000 0.05 0.26 Q3 1 0.9129 0.5712 0.5356 11.00000 0.05 0.25 Q4 1 0.1380 0.6873 0.6215 11.00000 0.05 0.25 Q5 1 0.8000 0.4923 0.5390 11.00000 0.05 0.24 Q6 1 0.9079 0.6930 0.5619 11.00000 0.05 0.24 Q7 1 0.1429 0.6113 0.7404 11.00000 0.05 0.24 Q8 1 0.6757 0.5942 0.3779 11.00000 0.05 0.23 Q9 1 0.2829 0.8050 0.3764 11.00000 0.05 0.23 Q10 1 0.3455 0.7400 0.7196 11.00000 0.05 0.22 Q11 1 0.4755 0.3738 0.6832 11.00000 0.05 0.22 Q12 1 0.5124 0.1592 0.7332 11.00000 0.05 0.22 Q13 1 0.8978 0.6289 0.6217 11.00000 0.05 0.22 Q14 1 0.3202 0.0965 0.7788 11.00000 0.05 0.21 Q15 1 0.5544 0.2872 0.7049 11.00000 0.05 0.21 Q16 1 0.0441 0.8807 0.6772 11.00000 0.05 0.21 Q17 1 0.0940 0.2735 0.6776 11.00000 0.05 0.21 Q18 1 0.3697 0.9582 0.3368 11.00000 0.05 0.21 Q19 1 0.1905 0.6213 0.5158 11.00000 0.05 0.20 Q20 1 0.8569 0.6953 0.7010 11.00000 0.05 0.20 ; _shelx_res_checksum 23644 _shelx_hkl_file ; 2 0 0 47.34 1.83 3 0 0 1402.51 8.70 -4 0 0 1544.74 7.47 4 0 0 1500.25 7.23 -5 0 0 1358.00 7.90 5 0 0 1342.27 7.57 -6 0 0 1678.59 14.44 6 0 0 1703.38 13.90 -7 0 0 247.32 6.55 -7 0 0 254.46 6.28 7 0 0 235.92 5.95 -8 0 0 -0.41 6.17 -8 0 0 10.50 6.10 8 0 0 -4.29 5.61 -9 0 0 12.40 13.62 -9 0 0 22.24 12.97 9 0 0 23.85 11.95 -10 0 0 46.18 7.88 -10 0 0 40.18 7.25 10 0 0 40.45 6.69 -11 0 0 24.09 8.38 -11 0 0 19.14 7.92 11 0 0 21.49 7.34 -12 0 0 176.83 17.28 12 0 0 153.13 16.42 -13 0 0 1.35 8.68 13 0 0 7.54 8.40 -14 0 0 -3.72 9.20 14 0 0 2.65 9.34 15 0 0 327.38 11.06 -16 0 0 88.38 11.19 16 0 0 65.57 10.84 -17 0 0 76.88 11.69 17 0 0 71.85 23.67 18 0 0 9.87 12.84 -19 0 0 15.86 12.94 19 0 0 6.52 13.75 -20 0 0 16.33 13.82 20 0 0 39.00 28.24 21 0 0 113.60 15.60 -22 0 0 11.48 14.90 22 0 0 98.15 34.47 0 1 0 5.50 2.53 0 -1 0 2.81 2.76 -1 1 0 217.07 2.50 1 -1 0 213.87 5.07 -2 1 0 1603.34 4.55 2 -1 0 1634.57 7.03 3 1 0 598.89 7.32 -3 1 0 574.16 5.69 3 1 0 574.07 3.76 -3 -1 0 583.46 3.81 3 -1 0 558.13 5.57 -4 1 0 5.31 2.46 4 1 0 12.47 5.59 4 -1 0 0.25 4.76 -5 -1 0 8.17 2.37 5 -1 0 9.35 2.51 -5 1 0 3.15 5.73 5 1 0 25.97 11.76 -6 1 0 193.88 3.92 6 1 0 188.85 7.07 -6 -1 0 184.92 3.59 -7 1 0 275.89 4.93 7 1 0 266.69 7.83 7 -1 0 255.08 4.38 -7 -1 0 275.77 8.08 -8 1 0 177.09 5.18 8 1 0 155.21 7.85 8 -1 0 162.60 4.62 -8 -1 0 157.10 9.00 -9 1 0 315.63 6.43 9 1 0 310.75 9.10 -9 -1 0 315.37 10.63 -10 1 0 8.55 8.36 -10 1 0 1.81 5.71 -10 -1 0 9.05 5.08 10 1 0 -1.13 16.61 -11 1 0 181.77 9.92 11 1 0 199.36 9.85 -11 -1 0 178.64 6.51 -12 1 0 30.55 7.29 -12 -1 0 32.28 6.46 12 -1 0 40.88 6.12 -12 1 0 43.50 19.00 12 1 0 46.58 19.02 -13 1 0 13.14 10.46 13 1 0 9.84 10.12 13 -1 0 12.46 6.70 -13 1 0 14.29 16.26 -14 1 0 214.22 12.53 -14 1 0 246.95 10.42 14 1 0 205.01 12.10 14 -1 0 211.33 8.35 15 1 0 -1.18 11.84 -15 -1 0 18.66 8.58 15 -1 0 1.31 8.25 -16 1 0 38.88 12.78 16 1 0 27.18 12.91 -16 -1 0 50.52 9.24 16 -1 0 58.62 17.60 -17 1 0 31.30 13.57 17 -1 0 15.60 9.60 17 1 0 25.05 28.20 -17 -1 0 15.54 19.84 18 1 0 51.87 14.74 -18 -1 0 35.43 10.52 18 -1 0 27.84 10.70 -19 1 0 21.82 14.75 -19 -1 0 12.72 11.41 19 1 0 118.78 31.15 19 -1 0 81.92 22.20 20 1 0 8.60 15.56 20 -1 0 23.24 11.52 -20 -1 0 24.97 23.05 -21 -1 0 3.21 12.12 21 -1 0 41.70 14.50 21 1 0 21.90 34.79 22 1 0 -3.29 18.82 -22 -1 0 12.06 13.28 22 -1 0 36.60 28.34 0 2 0 2017.85 10.46 0 -2 0 1929.88 9.89 -1 2 0 917.94 7.13 1 2 0 1012.77 9.20 1 -2 0 925.70 7.38 -2 2 0 1424.46 7.44 2 2 0 1399.83 10.64 2 -2 0 1339.21 7.53 3 -2 0 3314.54 10.21 -3 2 0 3518.80 13.32 4 -2 0 848.43 5.77 -4 2 0 847.90 8.07 -5 2 0 256.70 3.83 5 2 0 256.45 8.58 5 -2 0 246.99 4.11 6 2 0 124.03 8.56 6 -2 0 149.36 3.70 -6 2 0 161.29 6.81 7 2 0 194.41 9.48 7 -2 0 204.58 4.19 -7 2 0 211.05 7.75 8 2 0 1023.55 12.93 8 -2 0 1097.39 7.06 -8 2 0 1148.58 11.58 -8 -2 0 1118.06 8.90 -9 2 0 5.08 4.01 9 2 0 19.33 9.14 9 -2 0 1.95 3.85 -9 -2 0 20.69 6.06 -10 2 0 22.68 4.55 10 2 0 41.23 9.92 10 -2 0 17.25 8.27 -11 2 0 44.82 10.18 -11 2 0 43.08 5.22 -11 -2 0 25.72 4.21 11 -2 0 30.16 4.59 11 2 0 50.26 21.16 -12 2 0 5.06 11.04 -12 2 0 1.89 5.76 12 2 0 -1.03 10.97 -12 -2 0 -1.31 4.70 12 -2 0 2.56 4.95 -13 2 0 9.23 12.65 -13 2 0 4.59 6.47 13 2 0 6.25 12.18 -13 -2 0 9.32 5.39 14 2 0 93.43 13.20 -14 -2 0 78.12 6.27 -15 2 0 204.12 15.18 15 2 0 183.05 14.89 -15 -2 0 202.02 7.47 -15 2 0 225.84 17.81 -16 2 0 12.79 9.46 16 2 0 -12.39 14.60 -16 -2 0 12.10 14.25 17 2 0 122.79 16.06 17 -2 0 103.66 8.46 -17 -2 0 98.03 16.21 -18 2 0 85.47 16.48 18 2 0 83.74 17.70 -18 -2 0 47.85 8.64 18 -2 0 53.00 8.66 19 2 0 2.41 17.69 -19 -2 0 10.10 9.06 19 -2 0 -0.83 9.03 20 2 0 33.09 37.01 -20 -2 0 1.69 18.18 20 -2 0 36.11 20.88 -21 2 0 27.60 18.05 21 2 0 19.92 20.07 21 2 0 1.02 19.88 -21 -2 0 -0.35 9.82 21 -2 0 14.02 10.74 22 2 0 -0.75 21.12 -22 -2 0 3.35 10.49 22 2 0 8.75 40.67 0 3 0 2.07 6.79 0 -3 0 11.16 6.66 1 3 0 26.51 7.71 1 -3 0 31.91 6.67 -2 3 0 42.80 5.65 2 3 0 27.61 8.55 2 -3 0 42.86 6.21 -3 3 0 82.16 5.19 3 3 0 82.54 10.05 3 -3 0 80.41 5.67 4 3 0 1.99 10.14 4 -3 0 -2.61 5.02 -4 3 0 5.92 8.61 -5 3 0 317.78 5.05 5 3 0 342.75 12.09 5 -3 0 320.17 6.05 -6 3 0 37.35 3.81 6 3 0 40.28 10.00 6 -3 0 41.96 9.10 7 3 0 193.38 11.30 -7 3 0 218.05 7.99 7 -3 0 203.10 9.55 8 3 0 84.42 10.31 -8 3 0 86.07 7.67 8 -3 0 91.19 8.85 -9 3 0 8.13 7.92 9 3 0 6.43 21.06 9 -3 0 17.84 8.64 -10 3 0 91.08 4.65 10 3 0 82.19 11.34 10 -3 0 98.79 9.28 11 -3 0 175.10 5.50 -11 3 0 186.33 10.03 11 3 0 149.78 24.47 -12 3 0 310.31 14.05 -12 3 0 317.06 6.65 12 3 0 289.81 14.10 12 -3 0 290.24 11.66 -13 3 0 101.92 14.89 -13 3 0 122.35 6.38 13 -3 0 126.67 6.03 13 3 0 145.99 28.12 -13 -3 0 132.53 7.39 14 3 0 -14.88 14.95 -14 3 0 9.75 12.70 -14 -3 0 7.46 7.76 14 -3 0 14.79 11.82 15 3 0 579.63 18.82 -15 -3 0 586.44 7.10 15 -3 0 586.36 14.82 -16 3 0 43.90 17.44 -16 3 0 70.84 7.88 16 3 0 99.78 17.68 -16 -3 0 52.00 5.07 16 -3 0 50.86 12.31 -17 3 0 97.29 8.98 17 3 0 97.93 18.40 -17 -3 0 60.65 5.65 17 -3 0 57.71 12.79 18 3 0 4.37 18.65 18 3 0 42.02 21.34 -18 -3 0 16.96 6.91 18 -3 0 36.13 14.70 -19 3 0 -3.20 17.96 19 3 0 3.73 19.99 19 3 0 8.19 19.33 -19 -3 0 25.89 13.77 19 -3 0 32.56 16.06 20 3 0 10.57 20.72 20 3 0 3.64 21.31 21 3 0 15.75 22.04 21 3 0 4.78 22.30 0 4 0 51.58 8.96 -1 4 0 358.14 9.64 1 4 0 363.74 11.17 1 -4 0 319.90 9.53 -2 4 0 -3.87 7.21 2 4 0 11.88 10.34 2 -4 0 -6.07 15.43 3 4 0 290.70 12.30 3 -4 0 249.31 8.74 -3 4 0 251.80 14.35 -4 4 0 741.12 9.10 4 4 0 832.53 15.64 4 -4 0 685.02 9.80 -5 4 0 103.28 5.89 5 4 0 108.00 13.24 -6 4 0 80.56 5.15 6 4 0 88.74 26.25 6 -4 0 105.02 12.45 7 4 0 2.87 13.04 7 4 0 13.41 11.60 7 -4 0 3.15 5.99 -7 4 0 8.95 9.12 8 4 0 -2.91 14.18 8 -4 0 2.83 5.69 -8 4 0 -8.66 9.03 8 4 0 22.57 24.97 9 4 0 124.61 13.25 9 4 0 196.55 15.64 -9 4 0 148.89 9.70 9 -4 0 153.38 12.18 10 4 0 156.61 16.39 10 -4 0 137.59 6.37 -10 4 0 144.22 10.02 10 4 0 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-1 -19 30.54 22.38 2 1 19 9.08 17.18 2 1 19 79.49 29.72 2 -1 19 64.31 28.49 2 -1 19 6.91 15.81 -3 -1 -19 66.99 22.83 3 1 19 92.03 29.69 3 1 19 4.87 17.03 3 -1 19 80.62 29.43 3 -1 19 -0.64 15.22 -3 1 -19 62.39 36.16 -4 -1 -19 62.41 22.68 4 1 19 112.76 29.70 4 1 19 2.13 16.56 4 -1 19 87.45 29.27 4 -1 19 2.12 15.00 -4 1 -19 70.82 35.81 5 1 19 3.52 16.48 5 -1 19 24.89 29.51 5 -1 19 1.65 14.82 -5 1 -19 65.54 37.93 5 1 19 40.81 59.45 9 2 -19 17.47 22.78 9 -2 -19 50.98 28.61 -9 -2 19 28.60 23.44 -9 -2 19 27.89 23.71 -9 2 19 10.62 51.70 8 2 -19 40.78 22.24 8 -2 -19 14.86 27.57 -8 2 19 83.61 26.53 -8 -2 19 67.47 48.43 -8 -2 19 41.72 47.29 7 -2 -19 14.24 27.00 -7 2 19 -22.80 25.46 -7 -2 19 14.42 21.44 -7 -2 19 19.76 24.65 7 2 -19 67.32 43.22 6 2 -19 117.09 21.39 -6 -2 19 200.54 26.12 6 -2 -19 170.94 54.62 -6 2 19 192.80 49.41 5 2 -19 28.53 19.57 5 -2 -19 32.34 26.47 -5 2 19 9.68 25.73 -5 2 19 65.27 23.14 -5 -2 19 11.72 19.86 -5 -2 19 21.23 25.27 4 -2 -19 186.85 26.84 -4 2 19 234.03 27.61 -4 -2 19 202.58 26.35 4 2 -19 234.28 39.14 3 2 -19 75.01 18.70 3 -2 -19 100.84 26.48 -3 -2 19 92.54 26.56 -3 2 19 43.44 39.41 -3 2 19 16.62 52.42 -3 -2 19 2.92 37.52 2 -2 -19 39.86 25.11 -2 2 19 31.93 20.98 -2 2 19 44.22 26.88 -2 -2 19 -12.28 25.97 2 2 -19 15.75 36.43 -2 -2 19 11.20 36.57 1 2 -19 32.87 18.13 -1 2 19 28.67 21.27 -1 2 19 73.51 28.42 -1 -2 19 26.84 27.25 -1 -2 19 11.48 17.88 1 -2 -19 50.64 50.49 0 2 -19 -9.84 17.62 0 -2 -19 6.16 25.10 0 2 19 17.01 18.54 0 -2 19 30.60 28.11 0 -2 19 14.40 16.68 1 2 19 78.95 28.90 1 -2 19 11.45 16.28 -1 2 -19 66.47 37.33 -1 -2 -19 22.14 50.38 1 2 19 48.47 38.88 1 -2 19 17.46 55.20 -2 2 -19 53.15 18.98 -2 -2 -19 24.99 24.75 2 2 19 7.57 17.69 2 -2 19 29.25 27.62 2 -2 19 9.86 14.49 -3 2 -19 -2.11 16.20 -3 -2 -19 29.44 24.87 3 2 19 9.42 17.56 3 2 19 19.62 29.42 3 -2 19 28.33 28.55 3 -2 19 0.75 13.45 -4 2 -19 83.87 19.42 -4 -2 -19 38.14 25.28 4 2 19 12.23 17.41 4 2 19 86.96 30.35 4 -2 19 21.64 30.19 4 -2 19 0.61 13.22 7 3 -19 22.31 21.13 7 -3 -19 54.21 29.43 -7 3 19 -6.95 25.01 -7 -3 19 19.29 22.66 -7 -3 19 1.01 24.60 6 3 -19 7.12 20.44 6 -3 -19 59.40 58.30 -6 3 19 75.93 49.13 -6 -3 19 60.03 45.40 -6 -3 19 32.10 49.32 5 -3 -19 19.35 29.47 -5 3 19 33.26 23.49 -5 -3 19 16.59 24.96 5 3 -19 -0.88 39.27 -5 -3 19 19.84 41.30 4 3 -19 11.52 19.07 4 -3 -19 42.75 29.21 -4 3 19 63.54 25.27 -4 -3 19 1.34 19.63 -4 -3 19 47.50 25.86 3 3 -19 1.23 17.35 -3 3 19 10.46 21.42 -3 3 19 14.90 27.05 -3 -3 19 10.00 25.58 -3 -3 19 6.62 18.38 3 -3 -19 49.27 57.17 2 3 -19 11.86 16.94 2 -3 -19 26.19 28.40 -2 3 19 15.60 28.03 -2 3 19 17.12 19.67 -2 -3 19 8.40 17.17 -2 -3 19 38.72 52.34 1 3 -19 -18.18 16.24 -1 3 19 34.39 21.34 -1 3 19 -5.25 28.09 -1 -3 19 41.99 26.06 -1 -3 19 1.39 16.14 0 3 -19 11.38 16.30 0 -3 -19 54.95 28.06 0 3 19 -9.81 28.01 0 3 19 31.09 20.74 0 -3 19 2.34 15.36 0 -3 19 31.83 26.51 -1 3 -19 39.68 18.12 1 -3 19 3.84 15.01 -1 -3 -19 21.59 56.99 1 3 19 39.79 41.12 1 3 19 101.54 57.73 1 -3 19 54.75 55.47 -2 -3 -19 10.04 27.69 2 3 19 37.84 29.25 2 3 19 40.40 21.44 2 -3 19 44.40 29.21 2 -3 19 1.05 14.68 -2 3 -19 89.03 36.06 7 0 -20 16.50 25.99 -7 0 20 32.62 25.66 -7 0 20 20.56 25.20 6 0 -20 38.91 25.75 -6 0 20 64.36 26.21 -6 0 20 28.68 23.06 5 0 -20 16.78 24.81 -5 0 20 43.68 43.86 4 0 -20 41.10 23.75 -4 0 20 -5.50 27.65 -4 0 20 28.20 19.74 3 0 -20 39.98 24.09 -3 0 20 58.10 28.23 -3 0 20 6.11 19.53 2 0 -20 35.26 22.90 -2 0 20 13.52 18.86 -2 0 20 47.52 57.99 1 0 -20 -4.82 22.36 -1 0 20 24.98 29.95 -1 0 20 12.12 38.34 0 0 -20 47.44 22.94 0 0 20 37.63 30.47 0 0 20 28.35 38.50 -1 0 -20 -21.36 22.28 1 0 20 55.59 30.82 1 0 20 16.13 19.53 -2 0 -20 66.69 22.30 2 0 20 136.28 31.13 2 0 20 14.21 18.59 6 1 -20 198.65 23.99 6 -1 -20 181.31 28.08 -6 -1 20 175.68 27.78 -6 1 20 171.86 52.78 5 -1 -20 104.72 27.15 -5 1 20 11.97 22.84 -5 1 20 97.59 27.32 -5 -1 20 14.68 20.96 5 1 -20 115.59 45.48 4 1 -20 128.69 23.25 -4 1 20 161.42 28.31 -4 -1 20 175.87 29.17 4 -1 -20 163.75 52.86 3 1 -20 11.07 22.28 3 -1 -20 0.33 25.49 -3 1 20 10.87 21.55 -3 -1 20 58.96 28.97 -3 -1 20 2.63 20.00 2 1 -20 2.10 21.76 -2 1 20 10.47 28.73 -2 -1 20 21.90 21.02 2 -1 -20 76.59 50.12 -2 1 20 8.84 40.91 -2 -1 20 -2.73 57.83 1 1 -20 61.53 20.93 1 -1 -20 47.11 24.91 -1 1 20 3.07 19.28 -1 1 20 78.66 30.33 -1 -1 20 23.19 19.78 -1 -1 20 25.07 29.33 0 1 -20 84.81 24.81 0 1 20 5.99 19.18 0 -1 20 15.01 18.18 0 -1 20 71.76 30.01 0 -1 -20 21.22 49.12 0 1 20 -0.90 60.69 -1 -1 -20 47.28 24.50 1 1 20 5.18 18.82 1 -1 20 11.55 18.40 1 -1 20 55.13 30.69 -1 1 -20 66.43 40.54 -4 2 20 5.19 21.46 -4 -2 20 0.47 21.25 3 -2 -20 18.69 28.08 -3 2 20 33.29 28.11 -3 2 20 12.40 20.96 -3 -2 20 7.94 20.64 -3 -2 20 14.43 28.77 3 2 -20 19.66 40.09 2 2 -20 5.99 19.92 2 -2 -20 35.72 27.57 -2 2 20 64.63 29.07 -2 -2 20 -1.26 20.08 -2 2 20 56.77 44.08 -2 -2 20 63.40 58.76 1 2 -20 9.98 38.62 -1 -2 20 7.29 38.22 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 48221 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 O001 O 0.39146(11) 0.5923(3) 0.60230(12) 0.0191(5) Uani 1 1 d . . . . . O002 O 0.25930(11) 0.6145(3) 0.61857(12) 0.0201(5) Uani 1 1 d . . . . . N003 N 0.70202(13) 0.5686(3) 0.49612(15) 0.0168(6) Uani 1 1 d . . . . . C004 C 0.44382(16) 0.5473(4) 0.55192(18) 0.0169(7) Uani 1 1 d . . . . . C005 C 0.51647(16) 0.6100(4) 0.56886(18) 0.0178(7) Uani 1 1 d . . . . . H1 H 0.5279 0.6847 0.6140 0.021 Uiso 1 1 calc R U . . . C006 C 0.57248(16) 0.5617(4) 0.51862(18) 0.0167(6) Uani 1 1 d . . . . . C007 C 0.65039(16) 0.6052(4) 0.54421(19) 0.0173(6) Uani 1 1 d . . . . . H2 H 0.6634 0.6602 0.5958 0.021 Uiso 1 1 calc R U . . . C008 C 0.93113(17) 0.6011(4) 0.58434(19) 0.0238(7) Uani 1 1 d . . . . . H3 H 0.9820 0.6056 0.6043 0.029 Uiso 1 1 calc R U . . . C009 C 0.90335(17) 0.4664(4) 0.53258(19) 0.0225(7) Uani 1 1 d . . . . . H4 H 0.9357 0.3814 0.5183 0.027 Uiso 1 1 calc R U . . . C00A C 0.39571(18) 0.2524(4) 0.68114(19) 0.0244(7) Uani 1 1 d . . . . . H5 H 0.4393 0.3035 0.6665 0.029 Uiso 1 1 calc R U . . . C00B C 0.15365(16) 0.7955(4) 0.59242(19) 0.0204(7) Uani 1 1 d . . . . . C00C C 0.88346(17) 0.7271(4) 0.60587(19) 0.0241(7) Uani 1 1 d . . . . . H6 H 0.9024 0.8160 0.6404 0.029 Uiso 1 1 calc R U . . . C00D C 0.82737(16) 0.4593(4) 0.50243(18) 0.0192(7) Uani 1 1 d . . . . . C00E C 0.78022(15) 0.5880(4) 0.52574(18) 0.0176(7) Uani 1 1 d . . . . . C00F C 0.13284(16) 0.7469(4) 0.67151(19) 0.0229(7) Uani 1 1 d . . . . . H7 H 0.1524 0.6480 0.6972 0.027 Uiso 1 1 calc R U . . . C00G C 0.80756(16) 0.7227(4) 0.57663(19) 0.0209(7) Uani 1 1 d . . . . . H8 H 0.7755 0.8084 0.5908 0.025 Uiso 1 1 calc R U . . . C00H C 0.21071(16) 0.6882(4) 0.55005(17) 0.0180(7) Uani 1 1 d . . . . . C00I C 0.32638(17) 0.3341(4) 0.66027(18) 0.0200(7) Uani 1 1 d . . . . . C00J C 0.08287(17) 0.8455(4) 0.7124(2) 0.0277(8) Uani 1 1 d . . . . . H9 H 0.0697 0.8128 0.7653 0.033 Uiso 1 1 calc R U . . . C00K C 0.34845(18) 0.9751(4) 0.3890(2) 0.0248(7) Uani 1 1 d . . . . . H10 H 0.3799 1.0317 0.3553 0.030 Uiso 1 1 calc R U . . . C00L C 0.24180(17) 0.7946(4) 0.40300(19) 0.0207(7) Uani 1 1 d . . . . . H11 H 0.2010 0.7330 0.3775 0.025 Uiso 1 1 calc R U . . . C00M C 0.25620(16) 0.7963(4) 0.49134(19) 0.0184(7) Uani 1 1 d . . . . . C00N C 0.31627(17) 0.8949(4) 0.52786(19) 0.0220(7) Uani 1 1 d . . . . . H12 H 0.3255 0.9026 0.5868 0.026 Uiso 1 1 calc R U . . . C00O C 0.36208(18) 0.9812(4) 0.4775(2) 0.0248(7) Uani 1 1 d . . . . . H13 H 0.4025 1.0439 0.5030 0.030 Uiso 1 1 calc R U . . . C00P C 0.28718(18) 0.8833(4) 0.3517(2) 0.0255(7) Uani 1 1 d . . . . . H14 H 0.2764 0.8809 0.2928 0.031 Uiso 1 1 calc R U . . . C00Q C 0.12238(18) 0.9418(4) 0.5547(2) 0.0283(8) Uani 1 1 d . . . . . H15 H 0.1352 0.9750 0.5017 0.034 Uiso 1 1 calc R U . . . C00R C 0.26235(18) 0.2538(4) 0.68573(19) 0.0252(8) Uani 1 1 d . . . . . H16 H 0.2156 0.3052 0.6738 0.030 Uiso 1 1 calc R U . . . C00S C 0.05300(18) 0.9918(5) 0.6742(2) 0.0301(8) Uani 1 1 d . . . . . H17 H 0.0201 1.0581 0.7017 0.036 Uiso 1 1 calc R U . . . C00T C 0.4010(2) 0.0970(5) 0.7230(2) 0.0316(8) Uani 1 1 d . . . . . H18 H 0.4475 0.0446 0.7353 0.038 Uiso 1 1 calc R U . . . C00U C 0.07206(19) 1.0394(5) 0.5952(2) 0.0338(9) Uani 1 1 d . . . . . H19 H 0.0513 1.1366 0.5690 0.041 Uiso 1 1 calc R U . . . C00V C 0.3365(2) 0.0207(5) 0.7464(2) 0.0348(9) Uani 1 1 d . . . . . H20 H 0.3397 -0.0833 0.7742 0.042 Uiso 1 1 calc R U . . . C00W C 0.2673(2) 0.0991(4) 0.7284(2) 0.0303(8) Uani 1 1 d . . . . . H21 H 0.2242 0.0485 0.7448 0.036 Uiso 1 1 calc R U . . . B00X B 0.31863(19) 0.5008(5) 0.6006(2) 0.0188(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 O001 0.0149(10) 0.0257(12) 0.0173(10) -0.0047(9) 0.0039(8) -0.0033(9) O002 0.0170(11) 0.0266(12) 0.0169(10) -0.0005(9) 0.0028(8) 0.0002(9) N003 0.0166(13) 0.0174(13) 0.0167(12) 0.0004(10) 0.0033(10) -0.0026(11) C004 0.0186(15) 0.0172(16) 0.0150(14) 0.0046(12) 0.0026(12) 0.0007(13) C005 0.0188(15) 0.0158(16) 0.0181(15) 0.0012(12) -0.0011(12) -0.0022(13) C006 0.0187(15) 0.0151(15) 0.0166(15) 0.0021(12) 0.0030(12) -0.0006(13) C007 0.0191(15) 0.0143(15) 0.0181(15) 0.0013(13) 0.0003(12) -0.0016(13) C008 0.0153(15) 0.034(2) 0.0220(16) 0.0005(15) 0.0010(13) -0.0075(15) C009 0.0159(15) 0.0256(18) 0.0267(17) -0.0006(14) 0.0063(13) -0.0014(14) C00A 0.0268(17) 0.0288(19) 0.0171(15) 0.0005(14) 0.0000(13) -0.0020(15) C00B 0.0152(15) 0.0230(17) 0.0234(16) -0.0062(14) 0.0044(13) -0.0031(13) C00C 0.0243(17) 0.0263(18) 0.0216(16) -0.0056(14) 0.0030(13) -0.0076(15) C00D 0.0191(15) 0.0218(17) 0.0175(15) -0.0004(13) 0.0053(12) -0.0045(14) C00E 0.0123(14) 0.0202(17) 0.0202(15) 0.0025(13) 0.0012(12) -0.0038(13) C00F 0.0177(16) 0.0254(18) 0.0263(17) -0.0033(14) 0.0062(13) -0.0049(14) C00G 0.0157(15) 0.0227(18) 0.0243(16) -0.0023(13) 0.0026(13) -0.0012(13) C00H 0.0159(15) 0.0239(17) 0.0138(14) 0.0010(13) -0.0007(12) -0.0020(13) C00I 0.0206(16) 0.0256(18) 0.0138(14) -0.0018(13) 0.0023(12) -0.0029(14) C00J 0.0190(17) 0.038(2) 0.0267(17) -0.0093(16) 0.0066(14) -0.0093(16) C00K 0.0291(18) 0.0175(17) 0.0302(18) 0.0034(14) 0.0133(15) -0.0006(14) C00L 0.0215(16) 0.0190(17) 0.0222(16) -0.0034(13) 0.0045(13) 0.0009(14) C00M 0.0154(15) 0.0175(16) 0.0230(15) 0.0011(13) 0.0050(12) 0.0028(13) C00N 0.0227(16) 0.0231(17) 0.0202(16) -0.0002(14) 0.0026(13) 0.0019(14) C00O 0.0226(17) 0.0171(17) 0.0344(19) -0.0002(14) 0.0025(14) -0.0027(14) C00P 0.0321(19) 0.0227(18) 0.0222(16) 0.0001(14) 0.0057(14) 0.0039(16) C00Q 0.0263(18) 0.031(2) 0.0276(18) 0.0008(15) 0.0050(14) 0.0025(16) C00R 0.0265(17) 0.0294(19) 0.0197(16) -0.0035(14) 0.0026(14) -0.0054(15) C00S 0.0187(17) 0.033(2) 0.039(2) -0.0150(17) 0.0068(15) 0.0040(16) C00T 0.043(2) 0.032(2) 0.0187(16) 0.0014(15) -0.0016(15) 0.0057(17) C00U 0.0272(19) 0.035(2) 0.039(2) -0.0004(17) 0.0045(16) 0.0052(17) C00V 0.063(3) 0.025(2) 0.0173(16) 0.0016(14) 0.0058(16) -0.0100(19) C00W 0.039(2) 0.031(2) 0.0208(17) -0.0027(15) 0.0066(15) -0.0125(17) B00X 0.0170(17) 0.0229(19) 0.0168(16) -0.0019(15) 0.0033(14) -0.0039(15) 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' O O 0.0106 0.0060 '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' B B 0.0013 0.0007 '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 _geom_angle_publ_flag C004 O001 B00X 121.8(2) . . ? C00H O002 B00X 120.1(2) . . ? C007 N003 C00E 121.3(2) . . ? C007 N003 B00X 121.7(2) . 3_666 ? C00E N003 B00X 117.1(2) . 3_666 ? O001 C004 C005 119.4(3) . . ? O001 C004 C006 122.2(3) . 3_666 ? C005 C004 C006 118.5(3) . 3_666 ? C004 C005 C006 120.5(3) . . ? C004 C005 H1 119.8 . . ? C006 C005 H1 119.8 . . ? C005 C006 C004 121.0(3) . 3_666 ? C005 C006 C007 120.3(3) . . ? C004 C006 C007 118.2(3) 3_666 . ? N003 C007 C006 120.7(3) . . ? N003 C007 H2 119.6 . . ? C006 C007 H2 119.6 . . ? C00C C008 C009 120.3(3) . . ? C00C C008 H3 119.9 . . ? C009 C008 H3 119.9 . . ? C00D C009 C008 120.1(3) . . ? C00D C009 H4 120.0 . . ? C008 C009 H4 120.0 . . ? C00T C00A C00I 121.9(3) . . ? C00T C00A H5 119.1 . . ? C00I C00A H5 119.1 . . ? C00Q C00B C00F 118.5(3) . . ? C00Q C00B C00H 121.8(3) . . ? C00F C00B C00H 119.6(3) . . ? C008 C00C C00G 120.7(3) . . ? C008 C00C H6 119.6 . . ? C00G C00C H6 119.6 . . ? C009 C00D C00E 118.4(3) . . ? C009 C00D C00H 124.8(3) . 3_666 ? C00E C00D C00H 116.6(3) . 3_666 ? C00G C00E C00D 121.7(3) . . ? C00G C00E N003 122.6(3) . . ? C00D C00E N003 115.6(3) . . ? C00B C00F C00J 120.5(3) . . ? C00B C00F H7 119.7 . . ? C00J C00F H7 119.7 . . ? C00C C00G C00E 118.8(3) . . ? C00C C00G H8 120.6 . . ? C00E C00G H8 120.6 . . ? O002 C00H C00B 105.7(2) . . ? O002 C00H C00D 107.1(2) . 3_666 ? C00B C00H C00D 112.0(2) . 3_666 ? O002 C00H C00M 111.1(2) . . ? C00B C00H C00M 112.0(3) . . ? C00D C00H C00M 108.8(2) 3_666 . ? C00A C00I C00R 116.9(3) . . ? C00A C00I B00X 121.8(3) . . ? C00R C00I B00X 120.9(3) . . ? C00S C00J C00F 120.1(3) . . ? C00S C00J H9 120.0 . . ? C00F C00J H9 120.0 . . ? C00P C00K C00O 119.0(3) . . ? C00P C00K H10 120.5 . . ? C00O C00K H10 120.5 . . ? C00M C00L C00P 121.5(3) . . ? C00M C00L H11 119.3 . . ? C00P C00L H11 119.3 . . ? C00L C00M C00N 117.9(3) . . ? C00L C00M C00H 122.8(3) . . ? C00N C00M C00H 119.2(3) . . ? C00O C00N C00M 120.9(3) . . ? C00O C00N H12 119.5 . . ? C00M C00N H12 119.5 . . ? C00N C00O C00K 120.8(3) . . ? C00N C00O H13 119.6 . . ? C00K C00O H13 119.6 . . ? C00K C00P C00L 119.9(3) . . ? C00K C00P H14 120.1 . . ? C00L C00P H14 120.1 . . ? C00B C00Q C00U 120.9(3) . . ? C00B C00Q H15 119.5 . . ? C00U C00Q H15 119.5 . . ? C00W C00R C00I 121.6(3) . . ? C00W C00R H16 119.2 . . ? C00I C00R H16 119.2 . . ? C00J C00S C00U 119.9(3) . . ? C00J C00S H17 120.0 . . ? C00U C00S H17 120.0 . . ? C00V C00T C00A 119.6(3) . . ? C00V C00T H18 120.2 . . ? C00A C00T H18 120.2 . . ? C00S C00U C00Q 120.0(3) . . ? C00S C00U H19 120.0 . . ? C00Q C00U H19 120.0 . . ? C00W C00V C00T 120.1(3) . . ? C00W C00V H20 119.9 . . ? C00T C00V H20 119.9 . . ? C00V C00W C00R 119.9(3) . . ? C00V C00W H21 120.0 . . ? C00R C00W H21 120.0 . . ? O002 B00X O001 110.8(3) . . ? O002 B00X C00I 114.2(3) . . ? O001 B00X C00I 111.5(2) . . ? O002 B00X N003 107.4(2) . 3_666 ? O001 B00X N003 106.8(2) . 3_666 ? C00I B00X N003 105.6(2) . 3_666 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O001 C004 1.342(3) . ? O001 B00X 1.487(4) . ? O002 C00H 1.434(3) . ? O002 B00X 1.442(4) . ? N003 C007 1.292(4) . ? N003 C00E 1.433(4) . ? N003 B00X 1.625(4) 3_666 ? C004 C005 1.388(4) . ? C004 C006 1.412(4) 3_666 ? C005 C006 1.398(4) . ? C005 H1 0.9300 . ? C006 C004 1.412(4) 3_666 ? C006 C007 1.448(4) . ? C007 H2 0.9300 . ? C008 C00C 1.377(5) . ? C008 C009 1.399(4) . ? C008 H3 0.9300 . ? C009 C00D 1.390(4) . ? C009 H4 0.9300 . ? C00A C00T 1.392(5) . ? C00A C00I 1.404(4) . ? C00A H5 0.9300 . ? C00B C00Q 1.388(5) . ? C00B C00F 1.396(4) . ? C00B C00H 1.535(4) . ? C00C C00G 1.385(4) . ? C00C H6 0.9300 . ? C00D C00E 1.396(4) . ? C00D C00H 1.543(4) 3_666 ? C00E C00G 1.389(4) . ? C00F C00J 1.396(4) . ? C00F H7 0.9300 . ? C00G H8 0.9300 . ? C00H C00D 1.543(4) 3_666 ? C00H C00M 1.554(4) . ? C00I C00R 1.406(4) . ? C00I B00X 1.616(5) . ? C00J C00S 1.382(5) . ? C00J H9 0.9300 . ? C00K C00P 1.389(5) . ? C00K C00O 1.393(4) . ? C00K H10 0.9300 . ? C00L C00M 1.390(4) . ? C00L C00P 1.396(4) . ? C00L H11 0.9300 . ? C00M C00N 1.398(4) . ? C00N C00O 1.383(4) . ? C00N H12 0.9300 . ? C00O H13 0.9300 . ? C00P H14 0.9300 . ? C00Q C00U 1.393(5) . ? C00Q H15 0.9300 . ? C00R C00W 1.394(5) . ? C00R H16 0.9300 . ? C00S C00U 1.382(5) . ? C00S H17 0.9300 . ? C00T C00V 1.388(5) . ? C00T H18 0.9300 . ? C00U H19 0.9300 . ? C00V C00W 1.384(5) . ? C00V H20 0.9300 . ? C00W H21 0.9300 . ? B00X N003 1.625(4) 3_666 ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B00X O001 C004 C005 -165.6(3) . . . . ? B00X O001 C004 C006 14.8(4) . . . 3_666 ? O001 C004 C005 C006 178.4(3) . . . . ? C006 C004 C005 C006 -2.0(5) 3_666 . . . ? C004 C005 C006 C004 2.1(5) . . . 3_666 ? C004 C005 C006 C007 -170.2(3) . . . . ? C00E N003 C007 C006 -170.7(3) . . . . ? B00X N003 C007 C006 9.5(4) 3_666 . . . ? C005 C006 C007 N003 -176.5(3) . . . . ? C004 C006 C007 N003 11.0(4) 3_666 . . . ? C00C C008 C009 C00D 0.1(5) . . . . ? C009 C008 C00C C00G -0.1(5) . . . . ? C008 C009 C00D C00E -0.6(4) . . . . ? C008 C009 C00D C00H -175.8(3) . . . 3_666 ? C009 C00D C00E C00G 1.0(4) . . . . ? C00H C00D C00E C00G 176.7(3) 3_666 . . . ? C009 C00D C00E N003 -176.9(3) . . . . ? C00H C00D C00E N003 -1.3(4) 3_666 . . . ? C007 N003 C00E C00G -38.5(4) . . . . ? B00X N003 C00E C00G 141.3(3) 3_666 . . . ? C007 N003 C00E C00D 139.5(3) . . . . ? B00X N003 C00E C00D -40.8(4) 3_666 . . . ? C00Q C00B C00F C00J -1.3(4) . . . . ? C00H C00B C00F C00J 178.0(3) . . . . ? C008 C00C C00G C00E 0.6(5) . . . . ? C00D C00E C00G C00C -1.0(5) . . . . ? N003 C00E C00G C00C 176.8(3) . . . . ? B00X O002 C00H C00B 178.1(2) . . . . ? B00X O002 C00H C00D 58.5(3) . . . 3_666 ? B00X O002 C00H C00M -60.2(3) . . . . ? C00Q C00B C00H O002 148.8(3) . . . . ? C00F C00B C00H O002 -30.4(3) . . . . ? C00Q C00B C00H C00D -94.8(3) . . . 3_666 ? C00F C00B C00H C00D 85.9(3) . . . 3_666 ? C00Q C00B C00H C00M 27.8(4) . . . . ? C00F C00B C00H C00M -151.5(3) . . . . ? C00T C00A C00I C00R 1.7(4) . . . . ? C00T C00A C00I B00X -171.4(3) . . . . ? C00B C00F C00J C00S 0.6(5) . . . . ? C00P C00L C00M C00N 2.2(5) . . . . ? C00P C00L C00M C00H -175.2(3) . . . . ? O002 C00H C00M C00L 138.5(3) . . . . ? C00B C00H C00M C00L -103.5(3) . . . . ? C00D C00H C00M C00L 20.9(4) 3_666 . . . ? O002 C00H C00M C00N -38.8(4) . . . . ? C00B C00H C00M C00N 79.2(3) . . . . ? C00D C00H C00M C00N -156.4(3) 3_666 . . . ? C00L C00M C00N C00O -3.1(5) . . . . ? C00H C00M C00N C00O 174.4(3) . . . . ? C00M C00N C00O C00K 1.5(5) . . . . ? C00P C00K C00O C00N 1.1(5) . . . . ? C00O C00K C00P C00L -2.0(5) . . . . ? C00M C00L C00P C00K 0.3(5) . . . . ? C00F C00B C00Q C00U 0.8(5) . . . . ? C00H C00B C00Q C00U -178.5(3) . . . . ? C00A C00I C00R C00W -1.0(4) . . . . ? B00X C00I C00R C00W 172.2(3) . . . . ? C00F C00J C00S C00U 0.7(5) . . . . ? C00I C00A C00T C00V -1.1(5) . . . . ? C00J C00S C00U C00Q -1.2(5) . . . . ? C00B C00Q C00U C00S 0.4(5) . . . . ? C00A C00T C00V C00W -0.2(5) . . . . ? C00T C00V C00W C00R 0.9(5) . . . . ? C00I C00R C00W C00V -0.2(5) . . . . ? C00H O002 B00X O001 96.7(3) . . . . ? C00H O002 B00X C00I -136.4(3) . . . . ? C00H O002 B00X N003 -19.6(3) . . . 3_666 ? C004 O001 B00X O002 -147.7(2) . . . . ? C004 O001 B00X C00I 83.9(3) . . . . ? C004 O001 B00X N003 -31.0(4) . . . 3_666 ? C00A C00I B00X O002 -150.4(3) . . . . ? C00R C00I B00X O002 36.8(4) . . . . ? C00A C00I B00X O001 -23.8(4) . . . . ? C00R C00I B00X O001 163.4(3) . . . . ? C00A C00I B00X N003 91.8(3) . . . 3_666 ? C00R C00I B00X N003 -81.0(3) . . . 3_666 ?