#------------------------------------------------------------------------------ #$Date: 2021-06-17 01:37:43 +0300 (Thu, 17 Jun 2021) $ #$Revision: 266499 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/00/39/4003955.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_4003955 loop_ _publ_author_name 'Sakamaki, Takumi' 'Nakamuro, Takayuki' 'Yamashita, Keitaro' 'Hirata, Kunio' 'Shang, Rui' 'Nakamura, Eiichi' _publ_section_title ; B2N2-Doped Dibenzo[a,m]Rubicene: Modular Synthesis, Properties, and Coordination-Induced Color Tunability ; _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/acs.chemmater.1c01441 _journal_year 2021 _chemical_formula_moiety 'C168 H104 B8 N8' _chemical_formula_sum 'C42 H26 B2 N2' _chemical_formula_weight 580.27 _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-12-03 _audit_creation_method ; Olex2 1.3 (compiled Sep 10 2019 10:52:38 for OlexSys, GUI svn.r5938) ; _cell_angle_alpha 90 _cell_angle_beta 93.80 _cell_angle_gamma 90 _cell_formula_units_Z 1 _cell_length_a 21.560 _cell_length_b 5.890 _cell_length_c 22.240 _cell_measurement_temperature 293(2) _cell_volume 2818.013 _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.944 _diffrn_measured_fraction_theta_max 0.944 _diffrn_radiation_wavelength 0.700 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_unetI/netI 0.0614 _diffrn_reflns_Laue_measured_fraction_full 0.944 _diffrn_reflns_Laue_measured_fraction_max 0.944 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 13113 _diffrn_reflns_point_group_measured_fraction_full 0.944 _diffrn_reflns_point_group_measured_fraction_max 0.944 _diffrn_reflns_theta_full 24.315 _diffrn_reflns_theta_max 24.315 _diffrn_reflns_theta_min 1.808 _exptl_absorpt_coefficient_mu 0.019 _exptl_crystal_density_diffrn 0.342 _exptl_crystal_F_000 302 _refine_diff_density_max 0.556 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.060 _refine_ls_extinction_coef 0.0118(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 209 _refine_ls_number_reflns 2263 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0465 _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^)+(0.0756P)^2^+0.1357P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1242 _refine_ls_wR_factor_ref 0.1288 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1812 _reflns_number_total 2263 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cm1c01441_si_003.cif _cod_data_source_block xscale _cod_original_cell_volume 2818.0 _cod_database_code 4003955 _shelx_shelxl_version_number 2018/3 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C007(H007), C008(H008), C00B(H00B), C00C(H00C), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M) ; _shelx_res_file ; TITL xscale_a.res in C2/c xscale.res created by SHELXL-2018/3 at 13:48:55 on 03-Dec-2019 REM Old TITL REM SHELXT solution in C2/c: R1 0.143, Rweak 0.062, Alpha 0.020 REM 0.073 for 246 systematic absences, Orientation as input REM Formula found by SHELXT: C22 N CELL 0.7 21.56 5.89 22.24 90 93.8 90 ZERR 1 0 0 0 0 0 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H B N DISP B 0.0013 0.0007 6.4763 DISP C 0.0033 0.0016 11.1819 DISP H -0 0 0.6234 DISP N 0.0063 0.0031 18.9823 UNIT 42 26 2 2 L.S. 10 PLAN 5 2 CONF BOND LIST 6 fmap 2 MORE -1 ACTA BOND $H REM REM REM WGHT 0.075600 0.135700 EXTI 0.011828 FVAR 0.41851 N001 4 0.345093 0.390486 0.579067 11.00000 0.03700 0.04328 = 0.03549 -0.00520 -0.00288 0.00473 C002 1 0.286128 0.442393 0.479923 11.00000 0.03225 0.03370 = 0.03004 -0.00208 0.00245 0.00542 C003 1 0.262350 0.152699 0.557760 11.00000 0.03534 0.03545 = 0.02588 -0.00031 -0.00061 0.00890 C004 1 0.297506 0.330535 0.535271 11.00000 0.02657 0.03792 = 0.02675 -0.00618 -0.00530 0.00475 C005 1 0.284460 0.120938 0.621389 11.00000 0.03622 0.03647 = 0.02564 0.00000 -0.00151 0.00832 C006 1 0.323662 0.646766 0.469621 11.00000 0.03630 0.03224 = 0.03237 -0.00223 0.00841 0.00429 C007 1 0.499869 0.425363 0.610977 11.00000 0.03936 0.03270 = 0.03596 -0.00105 0.00026 0.00082 AFIX 43 H007 2 0.494282 0.291857 0.588955 11.00000 -1.20000 AFIX 0 C008 1 0.306011 0.810153 0.425625 11.00000 0.03421 0.03657 = 0.03089 -0.00301 -0.00236 0.00419 AFIX 43 H008 2 0.268517 0.794709 0.402806 11.00000 -1.20000 AFIX 0 C009 1 0.451909 0.584592 0.609619 11.00000 0.03538 0.03905 = 0.03260 -0.00242 -0.00249 0.00133 C00A 1 0.336271 0.261952 0.632780 11.00000 0.04135 0.03430 = 0.02728 0.00131 0.00487 0.00772 C00B 1 0.399147 1.025686 0.451350 11.00000 0.03868 0.03597 = 0.03671 -0.00207 0.00471 -0.00012 AFIX 43 H00B 2 0.425327 1.146329 0.443735 11.00000 -1.20000 AFIX 0 C00C 1 0.291885 0.021365 0.726717 11.00000 0.04597 0.03940 = 0.02445 0.00285 -0.00089 0.00065 AFIX 43 H00C 2 0.276610 -0.056818 0.758925 11.00000 -1.20000 AFIX 0 C00D 1 0.376925 0.688158 0.508196 11.00000 0.03932 0.03866 = 0.02715 -0.00162 0.00174 0.01179 C00E 1 0.344134 0.993410 0.416178 11.00000 0.04210 0.03526 = 0.02687 0.00188 0.00061 0.00387 AFIX 43 H00E 2 0.332817 1.096823 0.385808 11.00000 -1.20000 AFIX 0 C00F 1 0.261009 0.007310 0.670199 11.00000 0.03501 0.04254 = 0.03030 -0.00034 -0.00220 0.00231 AFIX 43 H00F 2 0.224713 -0.077636 0.664729 11.00000 -1.20000 AFIX 0 C00G 1 0.345390 0.151073 0.735663 11.00000 0.03947 0.04140 = 0.02827 -0.00519 -0.00786 0.00653 AFIX 43 H00G 2 0.366674 0.153343 0.773423 11.00000 -1.20000 AFIX 0 C00H 1 0.367599 0.277583 0.688989 11.00000 0.03415 0.04143 = 0.03946 -0.00761 0.00018 0.00175 AFIX 43 H00H 2 0.402419 0.369890 0.695297 11.00000 -1.20000 AFIX 0 C00I 1 0.555427 0.460865 0.644177 11.00000 0.03615 0.04395 = 0.03714 0.00712 -0.00366 0.00802 AFIX 43 H00I 2 0.587009 0.353564 0.643407 11.00000 -1.20000 AFIX 0 C00J 1 0.564245 0.653028 0.678185 11.00000 0.03716 0.05747 = 0.03093 0.00820 -0.00972 -0.00855 AFIX 43 H00J 2 0.601191 0.673966 0.701552 11.00000 -1.20000 AFIX 0 C00K 1 0.414187 0.877376 0.497313 11.00000 0.03500 0.04419 = 0.03667 -0.00806 -0.00314 0.00307 AFIX 43 H00K 2 0.450038 0.902467 0.522019 11.00000 -1.20000 AFIX 0 C00L 1 0.517789 0.817152 0.677732 11.00000 0.05164 0.04822 = 0.02667 -0.00547 -0.00419 -0.01452 AFIX 43 H00L 2 0.523803 0.949028 0.700366 11.00000 -1.20000 AFIX 0 C00M 1 0.462840 0.783556 0.643622 11.00000 0.04362 0.03936 = 0.03825 -0.00508 -0.00304 0.00580 AFIX 43 H00M 2 0.432273 0.895081 0.643079 11.00000 -1.20000 AFIX 0 B00N 3 0.391703 0.550830 0.566434 11.00000 0.04315 0.03611 = 0.03767 -0.00397 0.00645 0.00616 HKLF 4 REM xscale_a.res in C2/c REM wR2 = 0.1288, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0465 for 1812 Fo > 4sig(Fo) and 0.0547 for all 2263 data REM 209 parameters refined using 0 restraints END WGHT 0.0756 0.1323 REM Highest difference peak 0.556, deepest hole -0.333, 1-sigma level 0.060 ; _shelx_res_checksum 9943 _shelx_hkl_file ; 0 0 1 0.13 0.53 0 0 -1 0.07 0.36 0 0 2 3460.39 349.30 0 0 2 2829.41 285.56 0 0 -2 3296.60 332.60 0 0 -2 3489.78 352.24 0 0 3 -0.03 1.22 0 0 3 -0.01 1.90 0 0 -3 -0.60 1.29 0 0 -3 0.05 1.67 0 0 4 648.72 66.14 0 0 4 661.73 67.96 0 0 -4 644.42 65.72 0 0 -4 769.66 78.61 0 0 5 -0.21 5.06 0 0 5 0.42 2.94 0 0 -5 0.54 3.03 0 0 -5 0.85 4.09 0 0 6 320.84 33.50 0 0 6 368.08 39.23 0 0 -6 334.39 34.91 0 0 -6 363.99 38.28 0 0 7 0.16 2.34 0 0 7 0.68 4.54 0 0 -7 0.51 2.56 0 0 -7 -0.30 2.98 0 0 8 0.63 4.75 0 0 8 0.46 2.49 0 0 -8 0.48 2.54 0 0 -8 2.19 3.11 0 0 9 0.56 2.76 0 0 9 -0.07 5.54 0 0 -9 -0.50 2.66 0 0 -9 0.37 3.15 0 0 10 28.30 5.21 0 0 -10 23.52 5.26 0 0 11 0.34 2.96 0 0 11 0.26 6.45 0 0 -11 0.58 2.81 0 0 -11 0.06 3.51 0 0 12 132.39 18.49 0 0 -12 129.87 15.32 0 0 13 0.18 3.04 0 0 13 1.08 6.35 0 0 -13 0.19 2.86 0 0 14 2.06 6.62 0 0 14 2.26 3.34 0 0 -14 2.15 3.08 0 0 15 -0.19 3.33 0 0 15 0.74 7.13 0 0 -15 0.19 3.14 0 0 16 278.95 31.04 0 0 16 255.85 31.93 0 0 -16 286.61 31.81 0 0 17 -0.72 3.75 0 0 17 0.15 8.60 0 0 -17 0.02 3.54 0 0 18 1.66 8.25 0 0 18 1.38 3.95 0 0 -18 1.45 3.66 0 0 -18 1.69 4.59 0 0 19 1.05 3.90 0 0 -19 0.16 4.59 0 0 20 305.93 38.16 0 0 -20 342.37 37.97 0 0 21 0.08 4.41 0 0 -21 -0.19 3.71 0 0 22 110.34 15.04 0 0 22 107.19 18.75 0 0 -22 112.13 15.07 0 0 -22 96.06 13.78 0 0 23 -1.94 8.03 0 0 23 1.01 4.09 0 0 -23 0.27 3.68 0 0 -23 0.26 4.59 0 0 24 19.16 6.24 0 0 24 12.59 9.53 0 0 -24 19.88 5.90 0 0 -24 18.68 6.96 0 0 25 -0.33 4.30 0 0 -25 -0.60 4.30 0 0 -25 -0.16 5.03 0 -2 0 120.74 13.32 0 2 0 113.60 13.06 0 2 0 113.18 12.90 0 -2 1 32.23 4.81 0 -2 1 26.89 3.95 0 -2 -1 19.40 3.52 0 -2 -1 29.06 4.68 0 2 1 25.06 4.45 0 2 1 30.39 4.90 0 2 -1 23.18 4.08 0 2 -1 29.56 4.45 0 -2 2 70.95 8.48 0 -2 2 70.64 8.35 0 -2 -2 116.22 13.22 0 -2 -2 83.23 10.21 0 2 2 78.71 9.64 0 2 2 85.74 10.30 0 2 -2 109.92 12.73 0 -2 3 235.70 24.99 0 -2 3 230.03 24.44 0 -2 -3 203.68 22.11 0 -2 -3 232.13 25.41 0 2 3 156.64 17.54 0 2 3 185.41 20.35 0 2 -3 219.11 23.75 0 2 -3 169.24 18.38 0 -2 4 12.66 2.69 0 -2 4 15.34 3.78 0 -2 -4 14.43 3.38 0 -2 -4 13.11 4.11 0 2 4 13.15 3.45 0 2 4 11.21 3.32 0 2 -4 11.12 3.69 0 2 -4 12.89 3.00 0 -2 5 220.90 24.51 0 -2 5 211.76 22.23 0 -2 -5 262.57 28.13 0 -2 -5 289.45 31.58 0 2 5 271.07 29.25 0 2 -5 231.71 25.45 0 2 -5 305.30 32.21 0 -2 6 692.92 70.75 0 -2 6 696.91 72.71 0 -2 -6 765.67 78.89 0 -2 -6 884.62 91.64 0 2 6 797.69 82.46 0 2 -6 690.82 71.59 0 2 -6 690.92 71.09 0 -2 7 553.60 58.60 0 -2 7 505.20 51.96 0 -2 -7 502.68 53.25 0 2 7 498.06 52.55 0 2 -7 456.69 47.66 0 2 -7 440.11 46.60 0 -2 -8 2.08 3.09 0 2 8 2.28 3.63 0 -2 9 27.27 7.15 0 -2 9 24.86 4.16 0 -2 -9 22.30 5.37 0 -2 -9 20.38 4.61 0 2 9 27.79 5.75 0 2 9 24.11 5.55 0 2 -9 25.12 6.62 0 2 -9 25.82 4.72 0 -2 10 8.22 5.53 0 -2 10 6.03 2.87 0 -2 -10 5.61 3.43 0 -2 -10 4.66 3.71 0 2 10 5.29 3.32 0 2 10 4.14 3.85 0 2 -10 6.34 5.27 0 2 -10 4.93 2.82 0 -2 11 9.53 3.23 0 -2 11 15.16 6.84 0 -2 -11 8.00 3.74 0 -2 -11 9.77 4.38 0 2 11 9.87 4.15 0 2 11 12.07 5.18 0 2 -11 13.47 5.14 0 2 -11 7.97 2.99 0 -2 12 22.88 4.57 0 -2 -12 18.52 4.80 0 -2 -12 20.21 5.53 0 2 12 21.68 5.41 0 2 12 23.44 6.49 0 2 -12 21.31 5.65 0 -2 13 0.19 5.93 0 -2 13 0.84 2.86 0 -2 -13 1.04 3.55 0 -2 -13 0.39 3.93 0 2 13 0.62 3.52 0 2 13 2.02 5.17 0 2 -13 1.60 4.10 0 2 -13 0.48 2.41 0 -2 14 8.83 7.06 0 -2 -14 7.08 4.87 0 -2 -14 6.02 4.14 0 2 14 8.84 4.67 0 2 14 8.33 6.41 0 2 -14 5.21 2.82 0 -2 15 26.32 5.28 0 -2 15 30.74 9.59 0 -2 -15 28.66 6.56 0 -2 -15 27.57 6.05 0 2 15 30.07 6.82 0 2 15 32.75 9.14 0 2 -15 26.45 5.47 0 2 -15 31.87 6.64 0 -2 16 211.13 27.98 0 -2 16 208.40 23.44 0 -2 -16 203.78 24.45 0 2 16 226.36 26.58 0 2 -16 214.18 24.60 0 2 -16 193.28 22.38 0 -2 17 32.42 10.43 0 -2 17 28.22 5.93 0 -2 -17 25.78 6.51 0 2 17 32.28 10.83 0 2 -17 24.35 5.36 0 2 -17 30.54 6.76 0 -2 18 148.77 22.70 0 -2 18 157.69 18.83 0 -2 -18 156.22 19.02 0 -2 -18 150.98 19.53 0 2 18 154.75 19.42 0 2 18 159.89 23.15 0 2 -18 138.48 17.07 0 2 -18 143.94 17.90 0 -2 19 446.73 52.66 0 -2 19 516.54 55.04 0 -2 -19 501.52 53.90 0 -2 -19 497.64 54.51 0 2 19 455.64 52.83 0 2 19 504.25 54.81 0 2 -19 455.43 49.21 0 -2 20 3.96 8.17 0 -2 20 4.47 4.18 0 -2 -20 3.38 4.60 0 -2 -20 3.74 5.44 0 2 20 3.64 4.75 0 2 20 4.55 8.84 0 2 -20 2.97 3.50 0 -2 21 152.65 18.83 0 -2 -21 145.20 18.28 0 -2 -21 140.48 18.90 0 2 21 150.24 23.59 0 2 21 148.35 19.16 0 -2 22 40.53 12.39 0 -2 -22 45.16 8.49 0 -2 -22 42.31 9.07 0 2 22 43.75 8.56 0 2 22 46.60 13.67 0 2 -22 41.42 7.77 0 -2 23 48.98 9.09 0 -2 23 40.95 13.08 0 -2 -23 43.59 9.24 0 2 23 47.02 9.12 0 2 -23 42.30 8.56 0 2 -23 42.53 8.20 0 -2 24 -1.07 9.91 0 -2 24 -0.79 4.51 0 2 -24 1.69 3.93 0 2 -24 0.86 4.73 0 -4 0 20.56 5.17 0 -4 0 33.59 5.56 0 4 0 25.18 5.93 0 4 0 26.26 5.03 0 -4 1 2.15 3.11 0 -4 1 2.07 2.47 0 4 1 1.99 3.66 0 4 1 1.46 3.05 0 4 -1 3.00 3.96 0 4 -1 1.27 2.83 0 -4 2 219.11 24.95 0 -4 2 230.56 25.00 0 -4 -2 220.69 24.46 0 4 2 282.31 32.14 0 4 -2 240.32 28.02 0 4 -2 239.06 26.20 0 -4 3 3.63 2.82 0 -4 3 3.43 2.39 0 -4 -3 5.32 3.25 0 4 3 3.52 3.28 0 4 -3 4.86 4.55 0 4 -3 4.10 2.90 0 -4 4 136.91 16.03 0 -4 4 90.76 10.87 0 -4 -4 111.08 13.53 0 -4 -4 80.51 11.27 0 4 4 75.22 11.51 0 4 4 102.37 12.85 0 4 -4 74.65 11.33 0 4 -4 122.63 14.44 0 -4 5 15.18 3.77 0 -4 5 14.52 3.54 0 -4 -5 15.50 4.24 0 -4 -5 11.85 4.70 0 4 5 17.91 5.58 0 4 -5 14.23 5.81 0 4 -5 16.14 3.93 0 -4 6 24.71 4.49 0 -4 6 26.16 4.96 0 -4 -6 26.90 5.57 0 -4 -6 23.81 5.91 0 4 6 25.59 6.37 0 4 -6 28.91 7.13 0 4 -6 22.73 4.45 0 -4 7 136.28 15.23 0 -4 7 136.59 16.16 0 -4 -7 163.88 19.23 0 -4 -7 158.21 19.67 0 4 7 127.56 16.56 0 4 7 147.20 17.81 0 4 -7 160.00 19.69 0 -4 8 64.00 7.95 0 -4 8 79.65 10.62 0 -4 -8 73.47 10.39 0 -4 -8 68.11 10.90 0 4 8 70.39 10.59 0 4 8 61.92 9.46 0 4 -8 62.64 9.83 0 -4 9 59.83 8.88 0 -4 9 47.25 6.37 0 -4 -9 51.18 8.37 0 -4 -9 49.77 9.16 0 4 9 70.38 10.65 0 4 9 49.69 8.78 0 4 -9 41.95 7.96 0 4 -9 47.49 7.23 0 -4 10 69.10 8.65 0 -4 10 66.12 9.96 0 -4 -10 70.95 11.53 0 4 10 59.20 9.75 0 4 10 79.38 11.92 0 4 -10 63.34 10.33 0 4 -10 81.19 10.72 0 -4 11 67.87 10.82 0 -4 11 87.36 10.57 0 -4 -11 86.09 11.96 0 -4 -11 105.20 15.28 0 4 -11 99.07 14.15 0 4 -11 111.50 13.92 0 -4 12 -0.29 4.87 0 -4 12 -0.40 3.03 0 4 12 -0.36 3.96 0 4 -12 -0.13 2.90 0 4 -12 0.67 5.99 0 -4 13 53.41 11.13 0 -4 13 36.39 5.96 0 -4 -13 37.24 7.19 0 4 13 45.12 9.49 0 4 -13 51.69 8.35 0 4 -13 44.68 8.76 0 -4 14 75.12 9.70 0 -4 -14 80.48 11.39 0 -4 -14 96.39 14.80 0 4 14 70.59 11.15 0 4 14 103.92 15.34 0 4 -14 98.69 13.52 0 -4 15 0.06 3.08 0 -4 15 -0.19 5.96 0 -4 -15 -0.35 4.89 0 -4 -15 -0.36 3.88 0 4 15 -0.68 6.17 0 4 15 1.17 4.16 0 4 -15 0.67 3.36 0 -4 16 24.68 8.93 0 -4 -16 31.00 8.21 0 -4 -16 28.74 6.66 0 4 16 24.04 6.53 0 4 16 32.61 9.36 0 4 -16 32.17 6.97 0 4 -16 33.67 6.95 0 -4 17 -0.48 6.39 0 -4 17 0.15 3.68 0 -4 -17 0.69 4.34 0 -4 -17 0.25 5.26 0 4 17 0.37 4.06 0 4 17 1.27 6.92 0 4 -17 0.48 3.76 0 4 -17 0.53 4.56 0 -4 18 25.78 9.46 0 -4 18 31.61 6.56 0 -4 -18 29.55 6.77 0 -4 -18 31.33 8.38 0 4 18 28.53 7.19 0 4 18 34.66 10.57 0 4 -18 26.85 6.89 0 4 -18 30.58 7.19 0 -4 19 2.42 4.18 0 -4 19 1.58 6.85 0 -4 -19 2.22 5.67 0 4 19 4.59 4.71 0 4 -19 2.75 4.33 0 4 -19 2.05 5.06 0 -4 20 0.81 4.08 0 -4 20 1.69 7.82 0 4 -20 0.64 4.24 0 -6 0 110.45 15.33 0 -6 0 93.86 12.34 0 6 0 129.56 19.41 0 -6 1 52.82 9.25 0 -6 1 49.24 7.85 0 -6 -1 56.11 8.88 0 -6 -1 71.03 11.45 0 6 1 56.39 11.88 0 6 -1 45.24 10.70 0 -6 2 3.72 3.51 0 -6 -2 0.60 4.04 0 -6 -2 2.51 4.45 0 6 2 1.24 5.60 0 6 2 2.31 4.51 0 -6 3 2.09 4.01 0 -6 3 2.08 3.31 0 -6 -3 2.72 4.19 0 -6 -3 1.57 4.22 0 6 3 2.48 5.54 0 6 3 2.38 4.51 0 6 -3 1.25 5.80 0 6 -3 1.60 3.22 0 -6 4 125.15 16.71 0 -6 -4 181.42 23.62 0 -6 -4 158.32 19.29 0 6 4 186.04 24.25 0 6 4 158.32 19.42 0 6 -4 155.59 21.16 0 -6 5 147.83 18.67 0 -6 5 178.37 20.11 0 -6 -5 183.20 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101.90 18.49 -21 1 10 102.19 15.01 21 -1 -9 15.93 6.28 21 -1 -9 15.33 6.70 -21 -1 9 14.77 5.77 -21 -1 9 12.65 9.92 21 1 -9 15.54 6.19 21 1 -9 13.95 6.37 -21 1 9 16.76 9.07 -21 1 9 15.90 6.01 21 -1 -8 85.82 13.90 21 -1 -8 90.38 14.56 -21 -1 8 75.29 11.73 -21 -1 8 76.68 16.18 21 1 -8 108.77 16.34 21 1 -8 100.98 15.24 -21 1 8 77.84 15.98 -21 1 8 79.27 12.54 21 -1 -7 178.79 23.64 21 -1 -7 160.73 21.33 -21 -1 7 151.60 23.84 21 1 -7 216.70 27.01 21 1 -7 183.41 23.79 -21 1 7 156.64 24.14 -21 1 7 150.87 19.78 21 -1 -6 102.96 15.20 -21 -1 6 114.02 20.00 21 1 -6 116.54 17.02 21 1 -6 170.60 22.04 21 -1 -5 112.97 17.10 21 -1 -5 110.34 15.94 -21 -1 5 90.02 17.54 21 1 -5 118.43 16.70 21 1 -5 112.02 16.61 -21 1 5 110.87 19.41 21 -1 -4 578.58 64.18 21 -1 -4 571.13 62.53 -21 -1 4 582.36 63.80 -21 -1 4 552.24 64.55 21 1 -4 548.25 60.82 21 1 -4 580.37 63.35 -21 1 4 526.51 61.87 21 -1 -3 15.21 6.77 21 -1 -3 13.57 5.92 -21 -1 3 12.38 5.73 21 1 -3 13.52 6.55 -21 1 3 13.29 9.43 21 -1 -2 165.56 21.50 21 -1 -2 167.77 22.68 -21 -1 2 168.61 22.06 21 1 -2 195.91 25.67 -21 1 2 186.88 27.62 -21 1 2 184.36 23.81 21 -1 -1 128.61 18.82 21 -1 -1 148.77 19.88 -21 -1 1 139.85 19.15 21 1 -1 139.11 20.32 -21 1 1 139.32 22.87 -21 1 1 123.05 17.54 21 -1 0 1.51 5.45 21 -1 0 3.82 4.87 -21 -1 0 2.01 8.87 -21 -1 0 4.16 4.82 21 1 0 4.84 6.53 21 1 0 3.55 4.02 -21 1 0 5.38 4.82 -21 1 0 2.36 8.51 21 -1 1 69.02 13.17 21 -1 1 74.76 12.33 -21 -1 -1 64.65 11.43 -21 -1 -1 72.89 16.03 21 1 1 62.29 13.28 21 1 1 65.77 10.48 -21 1 -1 75.83 16.51 -21 1 -1 75.42 12.62 21 -1 2 0.70 4.40 21 -1 2 1.66 6.02 -21 -1 -2 0.25 4.07 -21 -1 -2 1.27 8.58 21 1 2 2.27 6.37 21 1 2 0.66 3.79 -21 1 -2 0.19 4.12 -21 1 -2 2.57 8.80 21 -1 3 5.48 4.98 21 -1 3 4.50 6.68 -21 -1 -3 5.09 5.07 -21 -1 -3 3.74 8.17 21 1 3 2.13 6.62 21 1 3 5.17 3.79 -21 1 -3 4.91 4.49 -21 1 -3 2.72 8.86 21 -1 4 26.49 7.23 21 -1 4 19.92 8.88 -21 -1 -4 26.61 7.40 -21 -1 -4 26.87 11.02 21 1 4 26.68 9.70 21 1 4 23.13 5.74 -21 1 -4 23.07 7.22 -21 1 -4 24.30 11.46 21 -1 5 0.33 6.88 21 -1 5 2.25 4.36 -21 -1 -5 0.76 7.43 -21 -1 -5 0.19 4.44 21 1 5 0.05 6.70 21 1 5 0.30 3.30 -21 1 -5 0.35 4.55 -21 1 -5 0.18 8.83 21 -1 6 12.24 8.50 21 -1 6 14.86 5.60 -21 -1 -6 10.68 8.26 -21 -1 -6 14.43 6.51 21 1 6 13.72 8.37 21 1 6 14.33 4.84 -21 1 -6 15.43 10.47 -21 1 -6 13.87 6.32 21 -1 7 8.53 4.75 21 -1 7 12.16 8.37 -21 -1 -7 8.06 5.39 -21 -1 -7 7.95 8.83 21 1 7 7.70 7.49 21 1 7 8.13 4.66 -21 1 -7 10.38 5.63 -21 1 -7 7.98 9.36 21 -1 8 70.70 11.00 -21 -1 -8 68.79 12.22 -21 -1 -8 70.68 14.73 21 1 8 78.02 15.64 21 1 8 69.49 10.71 -21 1 -8 76.65 16.02 -21 -1 -9 55.81 13.35 -21 -1 -9 63.01 11.42 21 1 9 62.62 13.90 21 1 9 64.78 10.37 -21 1 -9 58.96 14.90 -21 -1 -10 0.42 8.01 21 1 10 1.02 3.96 -21 -3 6 15.39 5.07 -21 -3 6 19.46 9.84 21 3 -6 18.29 5.16 21 3 -6 21.07 6.69 -21 -3 5 8.09 8.75 21 3 -5 5.82 5.18 21 3 -5 6.35 4.26 -21 -3 4 13.91 9.04 -21 -3 4 17.15 6.33 21 3 -4 15.52 6.17 21 3 -4 14.31 5.04 -21 -3 3 16.33 9.24 -21 -3 3 23.36 7.25 21 3 -3 17.96 5.49 21 3 -3 17.31 6.62 -21 -3 2 33.36 11.12 -21 -3 2 37.94 9.10 21 3 -2 34.73 8.92 21 3 -2 33.26 6.95 -21 -3 1 8.75 5.82 -21 -3 1 6.15 8.17 21 3 -1 6.95 6.24 21 3 -1 8.36 4.55 -21 -3 0 16.93 9.50 21 3 0 15.71 5.28 21 3 0 15.08 7.98 -21 -3 -1 1.39 8.56 21 3 1 2.34 4.09 -21 -3 -2 1.09 5.02 21 3 2 -0.56 6.85 -21 -3 -3 11.28 5.98 21 3 3 9.46 4.89 21 3 3 13.03 9.01 -21 -3 -4 0.64 4.70 -21 -3 -4 -0.48 9.81 21 3 4 0.70 4.07 21 3 4 2.54 7.67 -21 -3 -5 48.89 10.36 -21 -3 -5 34.36 12.83 21 3 5 43.30 8.08 21 3 5 45.02 13.31 -21 -3 -6 9.69 5.92 -21 -3 -6 8.73 10.06 21 3 6 14.33 9.52 21 3 6 12.02 5.18 -21 -3 -7 59.52 11.46 -21 -3 -7 66.00 15.50 21 3 7 60.47 10.10 21 3 7 71.08 15.75 22 0 -14 100.57 15.33 22 0 -14 92.28 13.42 -22 0 14 104.64 20.06 -22 0 14 96.47 14.79 22 0 -13 0.50 4.55 22 0 -13 -0.54 3.87 -22 0 13 0.93 8.43 22 0 -12 108.45 16.16 22 0 -12 92.85 13.55 -22 0 12 92.96 17.86 -22 0 12 96.02 14.50 22 0 -11 0.21 4.15 22 0 -11 -0.21 4.08 -22 0 11 2.60 6.74 -22 0 11 0.83 4.93 22 0 -10 34.45 8.12 22 0 -10 41.27 9.14 -22 0 10 31.18 7.74 -22 0 10 28.17 10.35 22 0 -9 0.97 4.78 22 0 -9 -0.37 4.78 -22 0 9 -1.00 7.31 -22 0 9 -0.83 4.61 22 0 -8 19.69 6.92 22 0 -8 21.23 7.00 -22 0 8 16.83 5.97 -22 0 8 16.82 9.12 22 0 -7 -0.98 4.44 22 0 -7 -0.09 5.11 -22 0 7 -1.66 7.79 22 0 -6 14.37 6.85 22 0 -6 17.15 6.85 -22 0 6 9.76 8.30 22 0 -5 1.02 5.09 22 0 -5 -1.13 4.86 -22 0 5 -0.69 7.91 22 0 -4 136.91 19.06 22 0 -4 114.54 17.12 -22 0 4 93.91 18.26 22 0 -3 -0.60 4.90 22 0 -3 -0.65 4.47 -22 0 3 0.31 7.31 -22 0 3 0.13 4.68 22 0 -2 59.36 11.88 22 0 -2 67.03 11.78 -22 0 2 60.24 11.27 -22 0 2 60.74 14.47 22 0 -1 0.47 5.23 22 0 -1 0.21 4.34 -22 0 1 1.99 8.66 -22 0 1 1.50 4.37 22 0 0 57.90 10.78 22 0 0 52.39 11.49 -22 0 0 61.60 11.31 -22 0 0 55.10 14.07 22 0 1 -1.15 5.97 22 0 1 -0.04 4.28 -22 0 -1 -0.72 8.22 -22 0 -1 0.17 4.67 22 0 2 28.89 9.55 22 0 2 29.01 7.59 -22 0 -2 27.55 12.00 -22 0 -2 29.86 8.08 22 0 3 0.25 7.14 22 0 3 -0.69 4.09 -22 0 -3 -0.70 4.27 -22 0 -3 -0.08 8.36 22 0 5 -0.46 6.73 22 0 5 -0.39 4.11 -22 0 -5 0.62 4.43 -22 0 -5 -1.06 8.48 22 0 6 200.74 27.97 22 0 6 186.46 22.82 -22 0 -6 201.79 29.16 -22 0 -6 228.35 28.83 22 0 7 -0.24 3.82 -22 0 -7 -0.23 8.58 22 0 8 58.98 9.88 -22 0 -8 58.71 14.38 -22 -2 11 2.18 8.96 22 2 -11 4.59 5.48 -22 -2 10 6.44 5.61 -22 -2 10 6.29 9.31 22 2 -10 6.46 4.67 22 2 -10 10.21 5.83 -22 -2 9 22.88 6.83 -22 -2 9 19.04 11.09 22 2 -9 20.70 6.25 22 2 -9 31.07 8.05 -22 -2 8 9.64 10.06 -22 -2 8 8.73 5.45 22 2 -8 6.63 5.16 22 2 -8 9.10 5.58 22 -2 -7 0.19 4.67 -22 -2 7 0.76 4.62 -22 -2 7 -1.46 8.98 22 2 -7 -0.70 4.43 -22 2 7 1.76 7.37 22 -2 -6 13.42 6.18 -22 -2 6 18.54 11.42 22 2 -6 15.82 5.93 -22 2 6 12.46 8.79 22 -2 -5 9.91 5.64 -22 -2 5 10.68 11.08 22 2 -5 6.43 4.77 -22 2 5 8.09 8.18 22 -2 -4 -0.86 4.51 -22 -2 4 0.23 9.22 22 2 -4 0.15 3.92 -22 2 4 -0.21 7.35 22 -2 -3 18.57 6.63 -22 -2 3 17.84 6.76 -22 -2 3 15.81 10.97 22 2 -3 12.94 6.49 22 2 -3 13.47 4.98 -22 2 3 13.61 9.18 22 -2 -2 16.61 6.46 -22 -2 2 18.61 7.04 22 2 -2 18.22 7.19 -22 2 2 16.40 8.92 22 -2 -1 3.87 4.92 -22 -2 1 3.46 4.99 22 2 -1 4.61 6.35 -22 2 1 5.23 7.54 22 -2 0 -1.84 4.71 -22 -2 0 0.17 4.88 -22 -2 0 0.75 9.22 22 2 0 -0.83 3.42 22 2 0 -0.03 5.67 -22 2 0 0.61 8.08 22 -2 1 15.93 6.36 -22 -2 -1 11.82 5.96 -22 -2 -1 15.42 9.74 22 2 1 8.31 4.25 22 2 1 11.69 7.39 -22 2 -1 12.01 9.48 22 -2 2 46.86 9.75 -22 -2 -2 40.87 9.31 -22 -2 -2 40.34 12.02 22 2 2 45.34 8.11 22 2 2 46.58 11.72 -22 2 -2 42.03 13.15 -22 -2 -3 18.38 6.88 -22 -2 -3 17.97 9.74 22 2 3 19.60 5.58 22 2 3 21.39 8.72 -22 2 -3 18.62 11.10 -22 -2 -4 39.12 8.98 -22 -2 -4 33.72 11.15 22 2 4 33.56 7.09 22 2 4 34.87 10.79 -22 -2 -5 11.28 5.78 -22 -2 -5 8.61 8.16 22 2 5 11.34 4.97 22 2 5 11.46 8.50 -22 -2 -6 5.17 8.67 -22 -2 -6 3.47 5.22 22 2 6 6.52 4.61 22 2 6 5.67 7.80 -22 -2 -7 5.93 9.00 -22 -2 -7 5.27 4.96 22 2 7 2.97 4.47 22 2 7 5.55 8.42 -22 -2 -8 53.81 13.99 22 2 8 63.20 10.62 22 2 8 61.09 14.82 -22 -2 -9 0.28 9.03 22 2 9 -1.21 4.26 -23 -1 11 125.46 17.46 -23 -1 11 107.61 21.14 23 1 -11 128.82 17.41 23 1 -11 129.87 18.22 -23 1 11 129.24 22.41 23 -1 -10 1.83 4.79 -23 -1 10 3.15 4.79 -23 -1 10 2.90 9.32 23 1 -10 4.18 4.58 23 1 -10 3.00 4.82 -23 1 10 3.02 8.24 23 -1 -9 8.19 5.93 -23 -1 9 7.17 5.09 -23 -1 9 3.65 9.62 23 1 -9 6.36 5.29 23 1 -9 6.73 5.34 -23 1 9 7.19 8.59 23 -1 -8 4.26 5.13 23 -1 -8 1.79 5.03 -23 -1 8 2.84 4.67 -23 -1 8 1.65 9.15 23 1 -8 3.49 5.13 23 1 -8 4.91 4.85 -23 1 8 3.24 7.97 -23 1 8 3.54 4.67 23 -1 -7 31.50 8.46 23 -1 -7 34.03 8.32 -23 -1 7 24.62 6.71 -23 -1 7 24.51 11.58 23 1 -7 27.01 7.86 23 1 -7 30.49 7.71 -23 1 7 21.99 10.16 -23 1 7 26.33 7.34 23 -1 -6 9.85 5.53 23 -1 -6 7.60 5.80 -23 -1 6 3.82 9.11 23 1 -6 9.28 5.79 23 1 -6 9.36 5.34 -23 1 6 6.58 8.30 23 -1 -5 12.37 6.43 23 -1 -5 11.09 5.65 -23 -1 5 7.79 9.59 23 1 -5 12.59 5.76 23 1 -5 11.81 6.13 -23 1 5 8.45 8.70 23 -1 -4 -0.38 4.50 23 -1 -4 0.16 4.98 -23 -1 4 0.88 4.64 -23 -1 4 -3.03 8.90 23 1 -4 0.01 4.23 23 1 -4 -0.19 4.84 -23 1 4 -0.30 7.70 23 -1 -3 14.44 6.22 23 -1 -3 19.39 7.47 -23 -1 3 16.09 10.23 -23 -1 3 22.99 7.36 23 1 -3 19.86 6.50 23 1 -3 17.20 6.61 -23 1 3 16.28 10.03 23 -1 -2 1.26 5.35 23 -1 -2 -1.06 4.91 -23 -1 2 1.65 4.83 -23 -1 2 2.89 8.71 23 1 -2 2.22 4.05 23 1 -2 1.61 4.82 -23 1 2 0.74 4.58 -23 1 2 0.25 8.08 23 -1 -1 0.80 5.30 23 -1 -1 0.73 4.68 -23 -1 1 1.95 5.00 -23 -1 1 1.52 8.65 23 1 -1 2.49 3.96 23 1 -1 2.27 5.74 -23 1 1 0.99 4.42 -23 1 1 0.41 8.18 23 -1 0 36.47 9.48 23 -1 0 46.58 9.78 -23 -1 0 37.91 8.95 -23 -1 0 36.58 12.54 23 1 0 34.09 7.60 23 1 0 30.44 8.93 -23 1 0 33.65 12.14 -23 1 0 38.53 9.07 23 -1 1 22.29 7.02 23 -1 1 18.31 7.63 -23 -1 -1 17.18 9.90 -23 -1 -1 17.74 6.63 23 1 1 17.98 7.87 23 1 1 14.80 5.52 -23 1 -1 16.69 9.69 23 -1 2 -0.38 4.51 -23 -1 -2 0.56 4.86 -23 -1 -2 1.51 8.21 23 1 2 0.17 6.59 23 1 2 0.34 3.61 -23 1 -2 0.67 8.57 23 -1 3 23.02 6.95 -23 -1 -3 23.27 7.33 -23 -1 -3 19.32 10.98 23 1 3 19.02 5.72 23 1 3 17.80 8.86 -23 1 -3 17.89 10.73 -23 -1 -4 1.68 4.71 -23 -1 -4 0.35 8.36 23 1 4 1.14 4.09 23 1 4 2.58 7.39 -23 -1 -5 185.62 27.73 -23 -1 -5 132.92 18.94 23 1 5 158.84 19.95 23 1 5 186.77 27.21 -23 -1 -6 5.77 9.49 23 1 6 8.41 4.54 -23 -1 -7 17.01 9.73 23 1 7 15.65 5.36 24 0 -10 151.70 20.83 24 0 -10 126.51 17.39 -24 0 10 127.56 22.79 -24 0 10 127.35 17.69 24 0 -9 -0.51 4.41 24 0 -9 -0.31 4.94 -24 0 9 0.44 4.91 -24 0 9 -0.75 8.90 24 0 -8 807.67 86.50 24 0 -8 706.25 76.92 -24 0 8 809.45 91.95 -24 0 8 769.13 82.36 24 0 -7 -1.22 5.08 24 0 -7 -0.42 4.72 -24 0 7 1.73 9.21 -24 0 7 -0.37 4.58 24 0 -6 192.02 25.13 24 0 -6 176.38 23.23 -24 0 6 157.58 25.91 24 0 -5 0.97 5.28 24 0 -5 0.66 4.61 -24 0 5 -0.95 8.94 24 0 -4 33.69 8.63 24 0 -4 42.28 9.36 -24 0 4 31.54 12.11 24 0 -3 0.24 5.26 24 0 -3 -0.11 4.65 -24 0 3 -0.22 9.16 -24 0 3 -0.12 4.75 24 0 -2 70.71 12.99 24 0 -2 85.90 13.81 -24 0 2 77.29 17.21 -24 0 2 93.20 14.98 24 0 -1 -0.23 5.06 24 0 -1 0.31 4.48 -24 0 1 0.69 9.60 -24 0 1 1.20 4.53 24 0 0 47.77 10.76 24 0 0 61.92 11.08 -24 0 0 50.76 14.46 -24 0 0 52.45 10.55 24 0 1 -0.92 4.27 24 0 1 -0.47 5.74 -24 0 -1 -1.05 9.10 24 0 2 1.20 4.09 -24 0 -2 1.51 9.30 24 0 3 -0.17 3.80 -24 0 -3 -0.05 9.07 -24 -2 5 37.38 13.53 24 2 -5 39.54 8.63 24 2 -5 47.79 9.03 -24 -2 4 2.14 9.73 24 2 -4 1.29 4.30 24 2 -4 0.19 3.54 -24 -2 3 21.08 11.98 -24 -2 3 18.05 6.89 24 2 -3 15.81 6.45 24 2 -3 15.93 5.46 -24 -2 2 2.22 4.84 -24 -2 2 -1.04 10.43 24 2 -2 3.23 5.23 24 2 -2 2.63 3.76 -24 -2 1 22.12 12.35 -24 -2 1 23.31 7.40 24 2 -1 15.78 6.85 24 2 -1 21.53 5.82 -24 -2 0 7.14 9.99 -24 -2 0 13.44 6.53 24 2 0 8.56 4.45 24 2 0 7.27 6.40 -24 -2 -1 67.67 12.36 -24 -2 -1 60.38 15.44 24 2 1 67.79 10.61 24 2 1 75.97 14.55 -24 -2 -2 31.20 8.51 -24 -2 -2 28.09 11.95 24 2 2 27.16 9.79 24 2 2 25.57 6.31 -25 -1 4 8.91 11.14 25 1 -4 5.68 4.88 25 1 -4 4.40 4.92 -25 -1 3 1.86 10.20 -25 -1 3 -0.27 4.93 25 1 -3 -0.49 4.47 25 1 -3 -0.69 4.27 -25 -1 2 31.83 8.40 -25 -1 2 24.75 12.86 25 1 -2 21.91 6.82 25 1 -2 34.37 8.01 -25 -1 1 23.28 12.50 -25 -1 1 19.02 6.99 25 1 -1 23.66 6.58 25 1 -1 15.25 6.63 -25 -1 0 9.80 5.63 -25 -1 0 11.30 11.13 25 1 0 11.59 5.39 25 1 0 9.37 6.02 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 8231 _olex2_submission_special_instructions 'No special instructions were received' 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 N001 N 0.34509(7) 0.3905(3) 0.57907(7) 0.0388(4) Uani 1 1 d . . . . . C002 C 0.28613(8) 0.4424(3) 0.47992(8) 0.0320(5) Uani 1 1 d . . . . . C003 C 0.26235(8) 0.1527(3) 0.55776(8) 0.0323(5) Uani 1 1 d . . . . . C004 C 0.29751(8) 0.3305(3) 0.53527(8) 0.0307(4) Uani 1 1 d . . . . . C005 C 0.28446(9) 0.1209(3) 0.62139(8) 0.0329(5) Uani 1 1 d . . . . . C006 C 0.32366(8) 0.6468(3) 0.46962(8) 0.0334(5) Uani 1 1 d . . . . . C007 C 0.49987(9) 0.4254(3) 0.61098(8) 0.0361(5) Uani 1 1 d . . . . . H007 H 0.494282 0.291857 0.588955 0.043 Uiso 1 1 calc R U . . . C008 C 0.30601(9) 0.8102(3) 0.42563(8) 0.0341(5) Uani 1 1 d . . . . . H008 H 0.268517 0.794709 0.402806 0.041 Uiso 1 1 calc R U . . . C009 C 0.45191(9) 0.5846(3) 0.60962(8) 0.0359(5) Uani 1 1 d . . . . . C00A C 0.33627(9) 0.2620(3) 0.63278(8) 0.0342(5) Uani 1 1 d . . . . . C00B C 0.39915(9) 1.0257(3) 0.45135(8) 0.0370(5) Uani 1 1 d . . . . . H00B H 0.425327 1.146329 0.443735 0.044 Uiso 1 1 calc R U . . . C00C C 0.29189(9) 0.0214(3) 0.72672(8) 0.0367(5) Uani 1 1 d . . . . . H00C H 0.276610 -0.056818 0.758925 0.044 Uiso 1 1 calc R U . . . C00D C 0.37692(9) 0.6882(3) 0.50820(8) 0.0351(5) Uani 1 1 d . . . . . C00E C 0.34413(9) 0.9934(3) 0.41618(8) 0.0348(5) Uani 1 1 d . . . . . H00E H 0.332817 1.096823 0.385808 0.042 Uiso 1 1 calc R U . . . C00F C 0.26101(9) 0.0073(3) 0.67020(8) 0.0361(5) Uani 1 1 d . . . . . H00F H 0.224713 -0.077636 0.664729 0.043 Uiso 1 1 calc R U . . . C00G C 0.34539(9) 0.1511(3) 0.73566(8) 0.0368(5) Uani 1 1 d . . . . . H00G H 0.366674 0.153343 0.773423 0.044 Uiso 1 1 calc R U . . . C00H C 0.36760(9) 0.2776(3) 0.68899(9) 0.0384(5) Uani 1 1 d . . . . . H00H H 0.402419 0.369890 0.695297 0.046 Uiso 1 1 calc R U . . . C00I C 0.55543(9) 0.4609(3) 0.64418(8) 0.0394(5) Uani 1 1 d . . . . . H00I H 0.587009 0.353564 0.643407 0.047 Uiso 1 1 calc R U . . . C00J C 0.56425(9) 0.6530(4) 0.67818(8) 0.0424(5) Uani 1 1 d . . . . . H00J H 0.601191 0.673966 0.701552 0.051 Uiso 1 1 calc R U . . . C00K C 0.41419(9) 0.8774(3) 0.49731(8) 0.0389(5) Uani 1 1 d . . . . . H00K H 0.450038 0.902467 0.522019 0.047 Uiso 1 1 calc R U . . . C00L C 0.51779(10) 0.8172(4) 0.67773(8) 0.0425(5) Uani 1 1 d . . . . . H00L H 0.523803 0.949028 0.700366 0.051 Uiso 1 1 calc R U . . . C00M C 0.46284(10) 0.7836(3) 0.64362(9) 0.0407(5) Uani 1 1 d . . . . . H00M H 0.432273 0.895081 0.643079 0.049 Uiso 1 1 calc R U . . . B00N B 0.39170(11) 0.5508(4) 0.56643(10) 0.0388(6) 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 N001 0.0370(9) 0.0433(10) 0.0355(9) -0.0052(7) -0.0029(7) 0.0047(7) C002 0.0323(10) 0.0337(10) 0.0300(10) -0.0021(8) 0.0024(8) 0.0054(8) C003 0.0353(10) 0.0355(10) 0.0259(9) -0.0003(8) -0.0006(8) 0.0089(8) C004 0.0266(9) 0.0379(10) 0.0268(9) -0.0062(8) -0.0053(7) 0.0047(8) C005 0.0362(10) 0.0365(11) 0.0256(9) 0.0000(8) -0.0015(8) 0.0083(8) C006 0.0363(10) 0.0322(10) 0.0324(10) -0.0022(8) 0.0084(8) 0.0043(8) C007 0.0394(11) 0.0327(10) 0.0360(10) -0.0011(8) 0.0003(8) 0.0008(8) C008 0.0342(10) 0.0366(10) 0.0309(10) -0.0030(8) -0.0024(8) 0.0042(8) C009 0.0354(10) 0.0390(11) 0.0326(10) -0.0024(8) -0.0025(8) 0.0013(9) C00A 0.0413(11) 0.0343(10) 0.0273(9) 0.0013(8) 0.0049(8) 0.0077(8) C00B 0.0387(11) 0.0360(11) 0.0367(10) -0.0021(8) 0.0047(9) -0.0001(8) C00C 0.0460(11) 0.0394(11) 0.0244(9) 0.0029(8) -0.0009(8) 0.0006(9) C00D 0.0393(10) 0.0387(11) 0.0271(9) -0.0016(8) 0.0017(8) 0.0118(9) C00E 0.0421(11) 0.0353(10) 0.0269(9) 0.0019(8) 0.0006(8) 0.0039(9) C00F 0.0350(10) 0.0425(11) 0.0303(10) -0.0003(8) -0.0022(8) 0.0023(9) C00G 0.0395(11) 0.0414(11) 0.0283(9) -0.0052(8) -0.0079(8) 0.0065(9) C00H 0.0341(10) 0.0414(11) 0.0395(11) -0.0076(9) 0.0002(8) 0.0017(9) C00I 0.0362(11) 0.0439(12) 0.0371(10) 0.0071(9) -0.0037(8) 0.0080(9) C00J 0.0372(11) 0.0575(13) 0.0309(10) 0.0082(9) -0.0097(8) -0.0086(10) C00K 0.0350(11) 0.0442(12) 0.0367(11) -0.0081(9) -0.0031(8) 0.0031(9) C00L 0.0516(13) 0.0482(12) 0.0267(10) -0.0055(8) -0.0042(9) -0.0145(10) C00M 0.0436(11) 0.0394(11) 0.0383(11) -0.0051(9) -0.0030(9) 0.0058(9) B00N 0.0432(13) 0.0361(12) 0.0377(12) -0.0040(10) 0.0064(10) 0.0062(10) 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 0.0063 0.0031 '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 N001 C00A 108.15(15) . . ? C004 N001 B00N 121.40(16) . . ? B00N N001 C00A 130.45(16) . . ? C003 C002 C006 128.54(16) 7_556 . ? C004 C002 C003 114.46(17) . 7_556 ? C004 C002 C006 116.94(16) . . ? C002 C003 C005 134.33(18) 7_556 . ? C004 C003 C002 118.71(16) . 7_556 ? C004 C003 C005 106.77(15) . . ? C002 C004 N001 124.37(17) . . ? C002 C004 C003 126.55(16) . . ? C003 C004 N001 109.00(15) . . ? C00A C005 C003 107.54(16) . . ? C00F C005 C003 134.04(18) . . ? C00F C005 C00A 117.92(16) . . ? C008 C006 C002 122.67(17) . . ? C008 C006 C00D 118.51(17) . . ? C00D C006 C002 118.66(16) . . ? C009 C007 H007 119.2 . . ? C00I C007 H007 119.2 . . ? C00I C007 C009 121.69(17) . . ? C006 C008 H008 119.9 . . ? C00E C008 C006 120.27(17) . . ? C00E C008 H008 119.9 . . ? C007 C009 C00M 116.82(17) . . ? C007 C009 B00N 120.53(16) . . ? C00M C009 B00N 122.35(17) . . ? C005 C00A N001 108.04(15) . . ? C00H C00A N001 129.20(17) . . ? C00H C00A C005 122.55(17) . . ? C00E C00B H00B 120.5 . . ? C00K C00B H00B 120.5 . . ? C00K C00B C00E 118.99(18) . . ? C00F C00C H00C 119.7 . . ? C00F C00C C00G 120.54(18) . . ? C00G C00C H00C 119.7 . . ? C006 C00D B00N 122.38(18) . . ? C00K C00D C006 119.02(16) . . ? C00K C00D B00N 118.18(17) . . ? C008 C00E C00B 121.03(17) . . ? C008 C00E H00E 119.5 . . ? C00B C00E H00E 119.5 . . ? C005 C00F H00F 120.0 . . ? C00C C00F C005 119.94(18) . . ? C00C C00F H00F 120.0 . . ? C00C C00G H00G 119.6 . . ? C00C C00G C00H 120.87(17) . . ? C00H C00G H00G 119.6 . . ? C00A C00H C00G 117.89(18) . . ? C00A C00H H00H 121.1 . . ? C00G C00H H00H 121.1 . . ? C007 C00I H00I 119.8 . . ? C00J C00I C007 120.33(18) . . ? C00J C00I H00I 119.8 . . ? C00I C00J H00J 120.1 . . ? C00I C00J C00L 119.82(18) . . ? C00L C00J H00J 120.1 . . ? C00B C00K C00D 121.73(18) . . ? C00B C00K H00K 119.1 . . ? C00D C00K H00K 119.1 . . ? C00J C00L H00L 120.1 . . ? C00M C00L C00J 119.76(18) . . ? C00M C00L H00L 120.1 . . ? C009 C00M H00M 119.2 . . ? C00L C00M C009 121.54(19) . . ? C00L C00M H00M 119.2 . . ? N001 B00N C009 121.90(18) . . ? N001 B00N C00D 113.91(18) . . ? C00D B00N C009 124.18(19) . . ? 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 N001 C004 1.412(2) . ? N001 C00A 1.438(2) . ? N001 B00N 1.421(3) . ? C002 C003 1.412(3) 7_556 ? C002 C004 1.403(2) . ? C002 C006 1.477(3) . ? C003 C004 1.404(3) . ? C003 C005 1.475(2) . ? C005 C00A 1.402(3) . ? C005 C00F 1.398(3) . ? C006 C008 1.407(3) . ? C006 C00D 1.408(3) . ? C007 H007 0.9300 . ? C007 C009 1.395(3) . ? C007 C00I 1.381(3) . ? C008 H008 0.9300 . ? C008 C00E 1.381(3) . ? C009 C00M 1.406(3) . ? C009 B00N 1.575(3) . ? C00A C00H 1.384(3) . ? C00B H00B 0.9300 . ? C00B C00E 1.390(3) . ? C00B C00K 1.367(3) . ? C00C H00C 0.9300 . ? C00C C00F 1.385(2) . ? C00C C00G 1.387(3) . ? C00D C00K 1.404(3) . ? C00D B00N 1.542(3) . ? C00E H00E 0.9300 . ? C00F H00F 0.9300 . ? C00G H00G 0.9300 . ? C00G C00H 1.388(3) . ? C00H H00H 0.9300 . ? C00I H00I 0.9300 . ? C00I C00J 1.368(3) . ? C00J H00J 0.9300 . ? C00J C00L 1.392(3) . ? C00K H00K 0.9300 . ? C00L H00L 0.9300 . ? C00L C00M 1.378(3) . ? C00M H00M 0.9300 . ? 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 N001 C00A C00H C00G 172.73(17) . . . . ? C002 C003 C004 N001 -176.89(15) 7_556 . . . ? C002 C003 C004 C002 6.5(3) 7_556 . . . ? C002 C003 C005 C00A 178.66(19) 7_556 . . . ? C002 C003 C005 C00F -10.0(4) 7_556 . . . ? C002 C006 C008 C00E -177.31(16) . . . . ? C002 C006 C00D C00K 177.59(16) . . . . ? C002 C006 C00D B00N -10.0(3) . . . . ? C003 C002 C004 N001 177.62(16) 7_556 . . . ? C003 C002 C004 C003 -6.3(3) 7_556 . . . ? C003 C002 C006 C008 15.8(3) 7_556 . . . ? C003 C002 C006 C00D -168.82(17) 7_556 . . . ? C003 C005 C00A N001 3.19(19) . . . . ? C003 C005 C00A C00H 178.39(17) . . . . ? C003 C005 C00F C00C -175.93(19) . . . . ? C004 N001 C00A C005 1.26(19) . . . . ? C004 N001 C00A C00H -173.52(18) . . . . ? C004 N001 B00N C009 -167.90(16) . . . . ? C004 N001 B00N C00D 13.2(2) . . . . ? C004 C002 C006 C008 -161.15(17) . . . . ? C004 C002 C006 C00D 14.2(2) . . . . ? C004 C003 C005 C00A -6.48(19) . . . . ? C004 C003 C005 C00F 164.9(2) . . . . ? C005 C003 C004 N001 7.31(19) . . . . ? C005 C003 C004 C002 -169.32(17) . . . . ? C005 C00A C00H C00G -1.4(3) . . . . ? C006 C002 C004 N001 -5.0(3) . . . . ? C006 C002 C004 C003 171.17(17) . . . . ? C006 C008 C00E C00B -2.7(3) . . . . ? C006 C00D C00K C00B 1.9(3) . . . . ? C006 C00D B00N N001 -3.6(3) . . . . ? C006 C00D B00N C009 177.55(17) . . . . ? C007 C009 C00M C00L -1.4(3) . . . . ? C007 C009 B00N N001 75.2(2) . . . . ? C007 C009 B00N C00D -106.0(2) . . . . ? C007 C00I C00J C00L -2.2(3) . . . . ? C008 C006 C00D C00K -6.9(3) . . . . ? C008 C006 C00D B00N 165.54(17) . . . . ? C009 C007 C00I C00J 1.7(3) . . . . ? C00A N001 C004 C002 171.25(16) . . . . ? C00A N001 C004 C003 -5.46(19) . . . . ? C00A N001 B00N C009 11.1(3) . . . . ? C00A N001 B00N C00D -167.73(17) . . . . ? C00A C005 C00F C00C -5.2(3) . . . . ? C00C C00G C00H C00A -2.8(3) . . . . ? C00D C006 C008 C00E 7.3(3) . . . . ? C00E C00B C00K C00D 2.8(3) . . . . ? C00F C005 C00A N001 -169.80(16) . . . . ? C00F C005 C00A C00H 5.4(3) . . . . ? C00F C00C C00G C00H 2.9(3) . . . . ? C00G C00C C00F C005 1.2(3) . . . . ? C00I C007 C009 C00M 0.1(3) . . . . ? C00I C007 C009 B00N 173.95(17) . . . . ? C00I C00J C00L C00M 0.9(3) . . . . ? C00J C00L C00M C009 1.0(3) . . . . ? C00K C00B C00E C008 -2.4(3) . . . . ? C00K C00D B00N N001 168.85(17) . . . . ? C00K C00D B00N C009 -10.0(3) . . . . ? C00M C009 B00N N001 -111.3(2) . . . . ? C00M C009 B00N C00D 67.4(3) . . . . ? B00N N001 C004 C002 -9.5(3) . . . . ? B00N N001 C004 C003 173.76(16) . . . . ? B00N N001 C00A C005 -177.87(18) . . . . ? B00N N001 C00A C00H 7.4(3) . . . . ? B00N C009 C00M C00L -175.15(19) . . . . ? B00N C00D C00K C00B -170.85(18) . . . . ?