#------------------------------------------------------------------------------ #$Date: 2021-06-06 18:45:49 +0300 (Sun, 06 Jun 2021) $ #$Revision: 266199 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243846.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2243846 loop_ _publ_author_name 'Harish Chinthal, Chayanna' 'Yathirajan, Hemmige S.' 'Manju, Nagaraja' 'Kalluraya, Balakrishna' 'Foro, Sabine' 'Glidewell, Christopher' _publ_section_title ; The crystal structures of three disordered 2-substituted benzimidazole esters ; _journal_coeditor_code WM5604 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 473 _journal_page_last 479 _journal_paper_doi 10.1107/S2056989021003364 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C20 H18 N2 O3' _chemical_formula_moiety 'C20 H18 N2 O3' _chemical_formula_sum 'C20 H18 N2 O3' _chemical_formula_weight 334.36 _chemical_name_systematic ; Ethyl 1-methyl-2-[4-(prop-2-yn-1-oxy)phenyl)-1H-benzimidazole-5-carboxylate ; _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 difmap _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 91.016(8) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.947(2) _cell_length_b 4.5907(5) _cell_length_c 41.305(4) _cell_measurement_reflns_used 3698 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.860 _cell_measurement_theta_min 2.459 _cell_volume 3402.6(6) _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2009) ; _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2009) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2009) ; _computing_molecular_graphics ; PLATON (Spek, 2020) ; _computing_publication_material ; SHELXL-2014 (Sheldrick, 2015b) and PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL-2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur with Sapphire CCD ; _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_unetI/netI 0.0478 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_number 7151 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.039 _diffrn_reflns_theta_min 2.459 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_correction_T_min 0.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis RED; Oxford Diffraction, 2009) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.305 _exptl_crystal_description needle _exptl_crystal_F_000 1408 _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.243 _refine_diff_density_min -0.226 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 286 _refine_ls_number_reflns 3350 _refine_ls_number_restraints 93 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.1145 _refine_ls_R_factor_gt 0.0676 _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^)+(0.0762P)^2^+3.8366P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1674 _refine_ls_wR_factor_ref 0.1872 _reflns_number_gt 2002 _reflns_number_total 3350 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5604sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2243846 _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 0.969 _shelx_estimated_absorpt_t_max 0.984 _shelx_hkl_file ; 0 0 -6 562.432 6.75094 0 0 0 -7 1.59117 4.01960 0 0 0 -8 1121.48 10.6539 0 0 0 9 33.4107 5.58573 1 0 0 -9 11.3808 5.35575 0 0 0 -10 4740.53 22.0273 0 0 0 10 4826.58 22.0243 1 0 0 -11 84.0178 4.05147 4 0 0 11 92.1129 6.51398 1 0 0 -11 86.6899 6.63248 0 0 0 -12 33.1670 5.32696 0 0 0 12 44.6056 5.73454 1 0 0 -12 40.3208 3.64968 4 0 0 -13-1.97996 5.44430 0 0 0 -13 1.09049 3.38057 4 0 0 13 3.54328 4.92527 1 0 0 -14 109.444 4.48395 4 0 0 14 115.142 7.21550 1 0 0 -14 107.796 6.70191 0 0 0 -15 13.3998 3.69035 4 0 0 -15 4.55027 5.36099 0 0 0 15 9.87760 5.26433 1 0 0 -16 1003.21 10.8040 4 0 0 16 976.130 13.8439 1 0 0 -16 1003.87 13.5494 0 0 0 -17 52.1970 7.06618 0 0 0 -17 60.9710 4.87230 4 0 0 17 46.8416 7.12350 1 0 0 -18 2185.13 20.3457 0 0 0 18 2177.96 20.8274 1 0 0 -18 2128.24 16.4160 4 0 0 -18 2241.29 22.6432 6 0 0 -19 73.3374 7.78970 0 0 0 19 96.7599 8.80654 1 0 0 -19 85.7871 5.47736 4 0 0 -19 73.5705 8.79336 6 0 0 20 121.599 8.32285 1 0 0 -20 121.868 9.64494 6 0 0 -20 116.089 8.38077 0 0 0 -20 118.133 5.74530 4 0 0 21 5.92448 7.65885 1 0 0 -21 3.77599 4.14729 4 0 0 -21-0.41908 7.88135 6 0 0 -21 2.17702 6.01554 0 0 0 -22 10.3032 4.38602 4 0 0 22 6.23527 7.37127 1 0 0 -22 11.8397 7.04162 0 0 0 -22 1.83059 8.58062 6 0 0 -23 2.03566 8.02367 6 0 0 -23 3.79380 6.67255 0 0 0 23-5.77980 7.20572 1 0 0 -23 4.29730 4.38205 4 0 0 -24 7.52164 8.73180 6 0 0 -24 19.7939 4.85192 4 0 0 -24 29.9968 6.39529 0 0 0 24 20.4428 7.88254 1 0 0 -25 8.18882 8.40006 6 0 0 -25 9.83915 7.37700 0 0 0 -25-0.66905 4.53665 4 0 0 25 3.00954 6.58704 1 0 0 -26 141.032 11.3348 6 0 0 -26 152.176 7.04094 4 0 0 26 151.074 10.2674 1 0 0 -26 154.237 9.43237 0 0 0 27 23.7499 7.94912 1 0 0 -27 18.6075 8.93887 6 0 0 -27 13.1027 6.44661 0 0 0 -28 524.139 16.5637 6 0 0 28 484.685 14.0756 1 0 0 -28 494.861 13.8432 0 0 0 29 12.7823 9.03981 1 0 0 -29 17.7426 9.78655 6 0 0 -29 44.8394 7.90200 0 0 0 30 9.84006 7.99146 1 0 0 -30 29.7315 7.11067 0 0 0 -30 6.02815 10.4447 6 0 0 31 1.60347 9.01105 1 0 0 -31 5.19043 9.48374 6 0 0 32 18.1316 10.0975 1 0 0 -32 26.6220 11.4723 6 0 0 33 3.49595 8.53868 1 0 0 -33 8.94432 9.84999 6 0 0 -34 283.907 16.4228 6 0 0 34 239.594 13.9242 1 0 0 35 12.9753 9.86611 1 0 0 -35 7.45534 11.2941 6 0 0 -36 14.9696 13.2992 6 0 0 36 34.2903 9.64964 1 0 0 37 2.97207 11.0382 1 0 0 -37-1.12483 11.2213 6 0 0 38 34.5849 10.4960 1 0 0 -38 27.2183 14.6909 6 0 0 -39 6.39140 12.6405 6 0 0 39 21.4394 12.1626 1 0 0 -40 464.613 21.4530 6 0 0 40 395.002 17.3694 1 0 0 -41 32.9452 12.5838 6 0 0 41-1.66022 9.31006 1 0 0 42 67.2639 12.4361 1 0 0 -42 93.4707 14.9226 6 0 0 -43 8.45808 13.0105 6 0 0 43 1.82704 10.9680 1 0 0 -44 50.9046 12.8308 6 0 0 -45-5.85128 13.2844 6 0 0 -46 35.2782 12.0464 6 0 0 -47-1.20477 13.9145 6 0 0 -48 36.0295 12.7827 6 0 0 -49 6.64451 15.2017 6 0 0 -50 55.9570 14.0488 6 0 0 -51-6.22503 16.3479 6 0 1 0 2.91742 5.87481 3 0 1 1 1.70712 4.77942 3 0 1 -1-1.58703 5.28369 3 0 1 2-0.85489 6.07278 3 0 1 -2 0.53869 5.52394 3 0 1 -2-2.58918 4.17761 4 0 1 3-2.09028 4.78141 3 0 1 -3 0.04388 4.85177 3 0 1 -3-1.62358 4.42976 4 0 1 4-1.16479 4.60348 3 0 1 -4 0.08704 4.29823 4 0 -1 5-2.89951 6.41949 7 0 1 -5 0.35111 3.64736 6 0 1 -5-4.50763 5.98923 4 0 -1 6-7.80690 7.33758 7 0 1 -6 0.54052 4.90983 4 0 1 -6-2.02463 4.01300 6 0 -1 7-1.66121 6.25420 7 0 1 -7-2.47892 4.52400 4 0 1 -7 0.94994 3.99718 6 0 -1 8-2.64412 6.98320 7 0 1 -8-0.41558 4.79732 4 0 1 -8-0.06578 4.01593 6 0 -1 9 0.06658 6.63346 7 0 1 -9-3.78419 4.83578 6 0 1 -9 0.19591 5.22327 4 0 1 -10 0.71081 6.06379 4 0 -1 10 0.03480 6.93432 7 0 1 -10-0.87368 4.73390 6 0 -1 11-2.11672 6.45307 7 0 1 -11-0.81289 5.49052 6 0 1 -11 1.29080 5.31389 4 0 1 -12 0.86541 5.55932 6 0 1 -12-1.47236 6.29283 4 0 -1 12 1.60103 6.36250 7 0 1 -13-1.76832 5.57013 6 0 -1 13 9.45911 6.38114 7 0 1 -13-1.30219 5.11185 4 0 1 -14 1.21746 5.81047 4 0 1 -14 0.92918 5.69790 6 0 1 -15-1.63131 6.10803 6 0 1 -15-3.57082 6.32174 4 0 1 -16 1.28025 6.92458 6 0 1 -16-5.92047 6.42901 4 0 1 -17 0.88516 7.29025 6 0 1 -17-6.09372 6.76247 4 0 1 -18-3.34735 7.69070 6 0 1 -18-7.14815 7.15009 4 0 1 -19-3.89279 7.25036 6 0 1 -19-7.97164 7.07795 4 0 -1 19 9.94743 7.07417 0 0 1 -20-1.50467 6.59746 4 0 1 -20-2.23152 6.99608 6 0 -1 -20-1.25434 6.40267 6 0 -1 20 0.55464 6.67197 0 0 -1 -21-0.03025 6.49768 6 0 1 -21 2.80229 6.07591 4 0 1 -21-3.01337 7.94338 6 0 -1 21 0.28741 6.08613 0 0 -1 22-1.29968 5.75511 0 0 -1 -22 5.49706 7.44681 6 0 1 -22-2.98927 6.25403 4 0 1 -22-2.71060 8.35361 6 0 1 -23-0.71551 7.53727 6 0 -1 23-0.10307 6.67143 0 0 -1 -23-0.18564 6.60643 6 0 1 -23-7.30070 6.79212 4 0 -1 -24-7.71311 7.93688 6 0 -1 24-0.56537 6.92805 0 0 1 -24 1.71780 6.95758 4 0 1 -24-0.53240 8.60529 6 0 1 -25-4.94563 9.30147 6 0 1 -25 0.97898 6.24304 4 0 -1 25 2.11304 6.97110 0 0 -1 -25-2.55024 7.22836 6 0 -1 26-5.11854 4.92625 0 0 -1 -26 0.17619 7.90339 6 0 1 -26 0.93312 8.27888 6 0 1 -26-4.21183 7.20117 4 0 1 -27-3.87037 9.39033 6 0 1 -27 6.33754 6.80376 4 0 -1 27-0.21225 6.49649 0 0 -1 -27 6.39905 8.45942 6 0 -1 28-3.13432 4.80128 0 0 1 -28-0.62853 6.72096 4 0 1 -28-1.77984 9.52929 6 0 -1 -28 6.25676 7.98259 6 0 -1 29-3.40484 5.92829 0 0 -1 -29 3.86156 9.26314 6 0 1 -29-2.92304 7.19259 4 0 1 -29-0.71624 9.51839 6 0 -1 30-2.10481 5.08868 0 0 1 -30-1.33810 7.37017 4 0 -1 -30 0.11653 8.06239 6 0 1 -30 12.6856 11.1851 6 0 1 -31-0.88615 10.3135 6 0 -1 -31 2.81032 9.64399 6 0 1 -31 1.26496 7.28095 4 0 -1 -32-4.59510 8.81859 6 0 1 -32-14.6139 7.88847 4 0 1 -32-3.40037 11.6042 6 0 -1 -33-6.41568 11.2042 6 0 -1 33 1.75889 8.40076 1 0 1 -33 0.20366 11.9776 6 0 1 -34-0.63320 11.8074 6 0 -1 34 12.5479 9.23825 1 0 -1 -34-1.75192 10.3957 6 0 -1 35 10.2128 9.86141 1 0 1 -35 4.56212 13.5431 6 0 -1 -35-8.84774 11.1578 6 0 1 -36-5.99200 11.5400 6 0 -1 -36-4.63911 11.2760 6 0 1 -37 16.4389 13.6018 6 0 -1 -37-3.72369 11.0024 6 0 -1 -38-5.56840 12.3581 6 0 1 -38-5.66738 11.4798 6 0 1 -39 6.00159 13.6116 6 0 -1 -39-5.79142 10.0841 6 0 1 -40-5.70966 12.6846 6 0 -1 -40 2.97354 12.9219 6 0 -1 -41 1.59957 10.4051 6 0 1 -41-7.43486 12.6294 6 0 -1 -42-0.11121 12.1699 6 0 1 -42 2.22498 11.9235 6 0 1 -43 1.55715 12.9038 6 0 -1 -43-5.16074 10.9060 6 0 1 -44 2.46138 12.4729 6 0 -1 -44-9.00344 11.9235 6 0 -1 -45-12.5843 12.2933 6 0 1 -45-7.25955 12.9532 6 0 1 -46-10.3019 13.3844 6 0 -1 -46-7.43284 11.7703 6 0 -1 -47-4.44602 13.9797 6 0 1 -47-1.86922 12.5912 6 0 1 -48-12.7617 15.3123 6 0 -1 -48 4.33103 10.6207 6 0 -1 -49 13.4566 15.4869 6 0 1 -49-11.0993 13.6090 6 0 -1 -50-11.2554 12.9390 6 0 1 -50-5.10218 14.3765 6 0 -1 -51-16.1388 13.3723 6 0 -1 -52-11.1549 15.0958 6 0 2 0 933.294 14.9022 3 0 -2 0 901.859 8.96982 2 0 2 -1 789.645 13.8323 3 0 -2 1 839.574 8.06492 2 0 2 1 776.197 14.1722 3 0 -2 2 249.286 5.12738 2 0 2 2 238.597 9.90385 3 0 2 -2 227.272 9.18231 3 0 2 3 358.374 10.6617 3 0 2 -3 374.596 5.39507 6 0 2 -3 407.377 11.2450 3 0 -2 3 382.250 5.57477 2 0 2 -4 50.0411 3.47296 6 0 2 4 121.834 9.10918 3 0 2 -4 58.1517 6.99445 3 0 2 -5 1027.71 15.2643 3 0 2 -5 1020.47 9.73943 6 0 2 5 1030.09 16.4029 3 0 2 -6 354.614 6.72860 6 0 2 6 382.051 11.4479 3 0 2 -7 125.039 5.26979 6 0 -2 7 124.726 10.4657 7 0 2 -7 141.574 9.20552 4 0 2 7 135.797 9.37647 3 0 2 8 55.0708 8.04630 3 0 -2 8 58.4477 9.54409 7 0 2 -8 54.1685 7.42544 4 0 2 -8 60.6809 4.71604 6 0 2 -9 910.780 11.7208 6 0 -2 9 966.890 17.0419 7 0 2 -9 914.967 16.7341 4 0 2 9 954.473 17.2235 3 0 2 -10 367.637 8.56658 6 0 -2 10 362.636 12.9474 7 0 2 -10 399.661 12.7255 4 0 2 10 390.210 13.6871 3 0 2 11 788.404 16.0537 3 0 -2 11 817.909 16.2089 7 0 2 -11 820.159 12.2255 6 0 2 -11 797.441 15.9592 4 0 -2 12 1.47091 8.69777 7 0 2 -12 11.5087 8.65591 4 0 -2 -12 10.9554 3.26445 6 0 2 -12 1.02929 5.26470 6 0 2 -13 5.62594 5.63465 6 0 -2 -13 10.2298 3.71751 6 0 2 -13 6.14167 7.35139 4 0 -2 13-1.02912 9.18914 7 0 -2 -14 818.883 10.9074 6 0 -2 14 830.899 16.6323 7 0 2 -14 799.087 13.5481 6 0 2 -14 802.981 17.0939 4 0 -2 -15 428.001 8.84445 6 0 2 -15 429.804 11.1390 6 0 -2 15 489.482 14.3557 7 0 2 -15 447.025 14.0662 4 0 2 -16 416.427 13.5798 4 0 -2 -16 417.223 9.15620 6 0 2 -16 429.480 11.3567 6 0 -2 16 433.777 14.8144 7 0 -2 -17 808.445 12.5769 6 0 2 -17 821.886 17.5662 4 0 2 -17 846.982 15.3331 6 0 -2 17 903.827 18.2184 7 0 -2 -18 1.42787 4.61902 6 0 2 -18 6.54549 6.87157 6 0 2 -18 11.7034 8.45234 4 0 -2 18-1.42058 9.55888 7 0 -2 -19 156.935 7.29138 6 0 2 -19 153.147 8.89773 6 0 -2 19 149.703 11.1150 7 0 2 -19 163.842 11.0197 4 0 2 -20 62.7637 9.74439 4 0 2 -20 57.2406 7.47409 6 0 -2 20 63.2451 9.96507 7 0 -2 -20 67.0683 6.28026 6 0 2 -21-0.94801 6.76555 6 0 -2 21 16.9869 9.94086 7 0 -2 -21 6.57896 5.55551 6 0 2 -21 7.25569 9.07822 4 0 2 -22 11.6362 8.74400 4 0 2 -22 7.87060 7.20746 6 0 -2 -22-1.86718 6.17308 6 0 -2 -23 485.907 12.4807 6 0 2 -23 522.293 16.1410 4 0 2 -23 518.487 14.7416 6 0 -2 -24 143.825 9.22572 6 0 2 -24 148.555 11.6062 4 0 2 -24 112.976 9.78375 6 0 2 -25 18.7034 9.41186 4 0 -2 -25 17.1932 7.10699 6 0 2 -25 29.6363 8.32417 6 0 2 -26 704.118 18.2704 4 0 2 -26 730.055 18.2322 6 0 -2 -26 732.779 16.3483 6 0 2 -27 428.466 15.4201 4 0 -2 -27 409.379 12.9730 6 0 2 -27 410.313 15.5139 6 0 -2 -28 5.12549 7.78233 6 0 2 -28 9.20615 9.86178 6 0 2 -28 21.3764 10.2176 4 0 -2 -29 164.965 10.6662 6 0 2 -29 188.397 13.4649 4 0 2 -29 188.345 13.2453 6 0 2 -30 283.589 14.1180 4 0 -2 -30 276.328 12.6693 6 0 2 -30 284.412 14.3666 6 0 2 -31 67.0949 10.8553 4 0 2 -31 60.6293 11.5632 6 0 -2 -31 62.3505 9.12677 6 0 -2 -32 194.234 12.0949 6 0 2 -32 188.703 14.2540 4 0 2 -32 201.739 14.8609 6 0 2 -33 21.8411 10.1077 4 0 -2 -33 9.28824 8.23813 6 0 2 -33 28.8184 11.8746 6 0 2 -34 262.534 15.1446 6 0 -2 -34 244.314 13.9768 6 0 2 -34 237.152 14.0517 4 0 2 -35-1.83093 9.12379 4 0 -2 -35-0.05439 9.07706 6 0 2 -35 24.8863 12.1348 6 0 -2 -36 243.072 14.2388 6 0 2 -36 252.241 16.6440 6 0 2 -36 234.523 13.8586 4 0 2 -37 14.7271 11.2915 6 0 -2 -38 11.8328 10.8257 6 0 2 -38 14.5744 12.4560 6 0 2 -39 10.7557 12.8782 6 0 2 -40 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8-12.0382 15.5789 5 20 -1 8-1.74245 14.9684 5 20 1 9 9.13012 14.1476 5 20 -1 9 13.9367 14.5472 5 20 1 10 7.01556 17.3266 5 20 -1 10 1.39621 11.4208 5 20 1 11 18.9585 17.7134 5 20 -1 11-18.7527 15.4492 5 20 1 12-1.96798 13.9920 5 20 -1 12-0.97289 15.7454 5 20 1 13 18.2489 16.4815 5 20 -1 13-14.4165 13.7993 5 20 1 14 4.65758 17.5015 5 20 -1 14 0.28127 11.7455 5 20 1 15 5.54906 15.1626 5 20 -1 15 8.53114 15.3688 5 20 1 16-13.0409 12.9847 5 20 -1 16-10.2694 16.1265 5 20 1 17-1.62367 16.2488 5 20 -1 17-2.72841 13.8327 5 20 1 18-8.55983 17.2639 5 20 -1 18 5.01731 13.6549 5 20 1 19-8.37667 13.4433 5 20 -1 19 3.27018 16.3727 5 20 1 20-2.56818 14.8707 5 20 -1 20-19.3840 16.3869 5 20 1 21-21.9000 17.8325 5 20 -1 21 5.63337 14.5676 5 20 -1 22 1.40974 12.1613 5 20 -2 -15 2.07245 12.4929 2 20 -2 -14-12.7520 12.0231 2 20 -2 -13 2.27595 13.4337 2 20 -2 -12 4.76846 13.4155 2 20 -2 -11 8.62095 13.7658 2 20 -2 -10 0.46185 14.1706 2 20 -2 -9-3.14727 14.0087 2 20 -2 -8 20.7003 14.1264 2 20 -2 -7 10.2641 14.1826 2 20 -2 -6 7.78372 13.2908 2 20 -2 -5-22.9460 11.9802 2 20 -2 -4 8.89485 12.3421 2 20 -2 -3 1.39143 13.7304 2 20 -2 -2-5.79935 15.5107 2 20 -2 -1 7.02598 16.3906 2 20 -2 0 27.5679 16.3236 2 20 -2 1 3.09200 14.2534 2 -20 2 -1 29.5317 8.79125 4 20 -2 2-6.48408 11.6719 2 -20 2 -2 31.6432 10.7897 4 20 -2 3 13.1362 12.4372 2 20 2 3-0.65912 14.0868 5 -20 2 -3 13.9961 10.7205 4 -20 2 -4 6.29082 10.3705 4 20 2 4-3.39785 16.5290 5 -20 2 -5 19.3734 13.2940 4 20 -2 5 36.5268 16.3722 2 20 2 5-0.48037 17.2066 5 -20 2 -6 22.6560 11.2738 4 20 2 6 33.5882 15.2705 5 -20 2 -7 0.49117 11.3929 4 20 2 7 6.05796 15.0333 5 -20 2 -8 29.4576 13.6630 4 20 2 8 42.7249 18.2631 5 -20 2 -9 25.8829 13.7299 4 20 2 9 49.7096 18.5657 5 -20 2 -10-0.92985 11.0735 4 20 2 10 8.26475 13.7604 5 -20 2 -11 48.1269 14.2113 4 20 2 11 56.0711 15.1792 5 -20 2 -12 12.4495 14.7247 4 20 2 12 30.7774 16.4970 5 -20 2 -13 41.1965 13.9052 4 20 2 13 47.4972 16.7064 5 -20 2 -14 28.1483 12.6121 4 20 2 14 30.9529 13.6115 5 -20 2 -15 11.9635 16.3176 4 20 2 15 44.6197 17.9273 5 -20 2 -16 5.22075 12.5269 4 20 2 16 15.1166 17.5773 5 20 2 17 4.63829 13.5701 5 20 -2 21 5.67503 11.9140 5 20 3 0-7.30097 9.60230 5 20 3 1 35.0781 11.4028 5 20 3 2 1.29453 13.2519 5 20 3 3 14.8815 13.6901 5 20 3 4 44.3925 12.3364 5 20 3 5 25.6329 10.3734 5 20 3 6-33.6490 13.1645 5 -20 3 -7 3.84337 9.75798 4 20 3 7 6.86652 14.4122 5 -20 3 -8-4.97819 10.2292 4 20 3 8-16.0339 12.9134 5 20 3 9-5.90099 10.3223 5 21 0 -25 5.66739 8.92244 2 21 0 -24 3.86163 10.0156 2 21 0 -23-4.50107 11.1357 2 21 0 -22 3.59769 11.0426 2 21 0 -21 20.0702 10.1050 2 21 0 -20 14.0932 9.13979 2 21 0 -19 0.12461 11.7978 2 21 0 -16-17.6282 9.43567 2 21 0 -15 22.2768 10.5159 2 21 0 -14 7.68606 11.1008 2 21 0 -13 10.6979 11.8544 2 21 0 -12-2.73149 11.5840 2 21 0 -11 15.8680 10.9489 2 21 0 -10-11.0639 10.1735 2 21 0 -9-14.6254 9.42526 2 21 0 -8 4.88538 11.3045 2 21 0 -7 2.12871 12.3394 2 21 0 -6-35.0939 13.1698 2 21 0 -5-6.07764 12.5712 2 21 0 -4 11.9982 12.9151 2 21 0 -3-4.64543 10.8034 2 21 0 -2-3.43262 11.1937 2 21 0 -1 4.26426 13.1440 2 21 0 0-1.95768 14.0989 2 21 0 1-7.13778 13.1743 2 21 0 1-7.67881 15.5353 5 21 0 2 4.78071 15.6031 5 21 0 3 17.9108 13.4527 5 21 0 4-0.69838 12.3151 5 21 0 5-15.9546 14.9150 5 21 0 6-18.2039 16.1335 5 21 0 7-12.7643 16.1113 5 21 0 8 10.0624 12.9414 5 21 0 9 9.30458 13.9653 5 21 0 10-0.14898 15.6651 5 21 0 11-23.8959 16.0433 5 21 0 12-15.4733 14.0105 5 21 0 13-4.84047 13.5195 5 21 0 14 1.08188 15.9170 5 21 0 15-13.3688 17.1847 5 21 0 17 12.3412 10.7102 5 21 -1 -19 11.8004 13.7490 2 21 -1 -18 26.3164 15.2583 2 21 -1 -17 8.01192 12.8705 2 21 -1 -16 6.73379 12.2641 2 21 -1 -15 2.39148 12.0517 2 21 -1 -14 17.0885 13.2511 2 21 -1 -13 51.3623 14.6024 2 21 -1 -12 30.8647 14.5147 2 21 -1 -11 3.59683 13.3079 2 21 -1 -10-3.99512 13.4408 2 21 -1 -9 0.82740 14.1970 2 21 -1 -8 52.9637 15.1834 2 21 -1 -7 50.4250 14.9561 2 21 -1 -6 21.9913 13.8445 2 21 -1 -5-1.53431 12.3412 2 21 -1 -4-6.13773 13.6213 2 21 -1 -3-1.53042 14.9967 2 21 -1 -2 48.6857 13.0397 5 21 -1 -2 50.5097 15.5620 2 21 -1 -1 2.82429 14.1887 2 21 -1 -1-1.40904 14.2891 5 21 -1 0 23.3703 14.8883 2 21 -1 0 21.7329 16.2740 5 21 -1 1 32.4606 14.0684 2 21 -1 1 36.7990 16.5859 5 21 -1 2 0.73624 11.7324 2 21 1 2 6.16131 17.3408 5 21 -1 2 19.4552 14.2855 5 21 -1 3 84.7151 15.4887 2 21 1 3 23.5645 17.6527 5 21 -1 3 48.5305 12.5804 5 21 1 4-6.24760 15.1589 5 21 -1 4-12.6702 14.1779 5 21 1 5 39.5674 14.1383 5 21 -1 5 42.3997 16.6436 5 21 1 6 133.579 18.9487 5 21 -1 6 122.424 18.0752 5 21 1 7 19.3118 17.6570 5 21 -1 7 16.7933 15.5133 5 21 1 8 4.86192 17.1113 5 21 -1 8 9.15996 14.2410 5 21 1 9 20.4663 14.7245 5 21 -1 9 28.7599 17.0043 5 21 1 10-7.72512 15.0299 5 21 -1 10-22.3530 17.0525 5 21 1 11-20.6995 17.4657 5 21 -1 11-11.7141 14.8835 5 21 1 12 12.6521 17.6045 5 21 -1 12 18.8899 11.9608 5 21 1 13 15.2961 15.5569 5 21 -1 13-3.83831 15.5127 5 21 1 14 42.8579 14.3556 5 21 -1 14 46.5557 17.7942 5 21 1 15-7.96117 16.1595 5 21 -1 15 15.8694 16.3788 5 21 -1 16-17.1920 12.3457 5 21 -1 17 15.3592 13.3742 5 21 -2 -2 11.5275 13.2991 2 21 -2 -1 0.24699 12.9965 2 21 -2 0-15.0026 12.1618 2 21 2 2-4.84428 12.0135 5 -21 2 -3 21.4375 11.0021 4 21 2 3 19.1170 14.7372 5 -21 2 -4 18.7706 10.2874 4 21 2 4-10.0199 16.5107 5 -21 2 -5 6.47188 8.27918 4 21 2 5 4.55360 16.4960 5 -21 2 -6 16.3020 9.99036 4 21 2 6-7.56510 14.6708 5 -21 2 -7 9.68882 11.9598 4 21 2 7 1.99207 11.5185 5 -21 2 -8 8.24847 12.4548 4 21 2 8 17.1730 13.9160 5 -21 2 -9-4.70085 10.7374 4 21 2 9 32.8057 15.7682 5 -21 2 -10-7.03136 10.8283 4 -21 2 -11 2.39457 11.1504 4 22 0 -20 25.9327 11.5907 2 22 0 -19-4.25672 10.9328 2 22 0 -18-1.91782 10.5008 2 22 0 -17 5.85530 8.89976 2 22 0 -16-20.9944 8.90792 2 22 0 -15-17.3723 9.75575 2 22 0 -14 0.58257 10.1809 2 22 0 -13 1.49571 10.8530 2 22 0 -12 16.8831 11.9843 2 22 0 -11 11.3364 12.4126 2 22 0 -10 20.3600 11.8629 2 22 0 -9 12.3618 10.3053 2 22 0 -8 15.5569 10.0588 2 22 0 -7-28.4076 9.98904 2 22 0 -6 57.5940 12.3730 2 22 0 -5 14.2603 12.4761 2 22 0 -4 10.3678 14.0705 2 22 0 -3 5.64856 14.8501 2 22 0 -2-0.85681 15.3516 2 22 0 -1-4.89385 14.8441 2 22 0 0 5.88220 13.2021 2 22 0 0 11.4987 17.8353 5 22 0 1 17.0335 17.2851 5 22 0 2-2.69010 14.8908 5 22 0 3 4.69603 12.7202 5 22 0 4 23.6219 13.8635 5 22 0 5 13.1235 16.3303 5 22 0 6 87.4981 18.5634 5 22 0 7 54.2624 18.8539 5 22 0 8 39.4457 16.2193 5 22 0 9-10.4529 12.6198 5 22 -1 -10-0.64529 15.8039 2 22 -1 -9 6.08435 16.4524 2 22 -1 -8 2.97714 16.3230 2 22 -1 -7 11.5752 14.7558 2 22 -1 -6 8.87207 14.5945 2 22 -1 -5-8.28697 13.8036 2 22 -1 -4-0.09552 13.1810 2 22 -1 -3 14.0017 12.8700 2 22 -1 -3-3.74693 13.9060 5 22 -1 -2-7.04455 11.8810 2 22 -1 -2 24.2082 15.3119 5 22 -1 -1-21.4415 11.3322 2 22 -1 -1-3.09853 13.8319 5 22 -1 0-9.05536 12.4482 2 22 -1 0-3.31890 14.2374 5 22 -1 1-4.37123 13.7828 2 22 1 1 21.9242 17.6278 5 22 -1 1 38.0746 13.2106 5 22 -1 2-1.99176 15.1897 2 22 1 2 0.30231 16.0409 5 22 -1 2 0.14632 11.0464 5 22 1 3-0.05094 15.3000 5 22 -1 3-35.7397 10.4828 5 22 1 4-8.85862 13.3353 5 22 -1 4 7.07824 13.6968 5 22 -1 5 3.61235 14.9277 5 22 -1 6-27.2662 15.5542 5 22 -1 7 16.4650 15.5262 5 22 -1 8 31.5278 15.0818 5 22 -1 9-6.74162 12.6532 5 22 -1 10-2.93089 13.2305 5 -22 2 -4 10.1840 9.96162 4 -22 2 -5 4.70535 11.4043 4 23 0 -11 27.1608 12.5103 2 23 0 -10 23.5164 12.6238 2 23 0 -9-4.62341 11.9972 2 23 0 -8-3.18182 11.6974 2 23 0 -7 8.00669 11.5542 2 23 0 -6-18.0267 11.3464 2 23 0 -5-17.2641 10.8353 2 23 0 -4-8.74715 10.3414 2 23 0 -3-10.2836 9.83857 2 23 0 -2 2.65241 9.55483 2 ; _shelx_hkl_checksum 3085 _shelx_res_file ; TITL b2cg CELL 0.71073 17.947 4.5907 41.305 90.00000 91.016 90.00000 ZERR 8 0.002 0.0005 0.004 0.00000 0.008 0.00000 LATT 7 SYMM -X, Y, -Z+ 0.50000 SFAC C H N O UNIT 160 144 16 24 PLAN 30 FMAP 2 OMIT -2 52.1 SIZE 0.36 0.18 0.18 REM OMIT -1 1 3 OMIT 2 2 9 OMIT -1 1 19 L.S. 20 ACTA BOND $H CONF HTAB EXYZ C21 C31 EADP C21 C31 SIMU 0.01 C21 > C26 SIMU 0.01 C31 > C36 EADP O24 O34 EADP C27 C37 EADP C28 C38 EADP C29 C39 WGHT 0.076200 3.836600 FVAR 0.62548 0.49443 N1 3 0.436258 1.091228 0.598508 11.00000 0.04215 0.04310 = 0.06135 -0.00339 -0.00533 -0.00446 C2 1 0.382941 0.989576 0.576342 11.00000 0.03769 0.04215 = 0.05380 -0.00301 -0.00322 0.00262 N3 3 0.334762 0.810726 0.589264 11.00000 0.04631 0.05855 = 0.04864 -0.00105 -0.00469 -0.00927 C3A 1 0.356477 0.790564 0.621709 11.00000 0.04549 0.05677 = 0.04592 -0.00321 -0.00507 0.00091 C4 1 0.326250 0.628594 0.646527 11.00000 0.05317 0.06540 = 0.05109 -0.00043 -0.00302 -0.00821 AFIX 43 H4 2 0.284034 0.514811 0.642934 11.00000 -1.20000 AFIX 0 C5 1 0.360268 0.640129 0.676696 11.00000 0.05385 0.06146 = 0.04770 -0.00447 -0.00440 0.00261 C6 1 0.423550 0.813128 0.682132 11.00000 0.06538 0.07185 = 0.05339 -0.00400 -0.01428 -0.00100 AFIX 43 H6 2 0.445515 0.816991 0.702690 11.00000 -1.20000 AFIX 0 C7 1 0.453761 0.975739 0.658136 11.00000 0.05789 0.06716 = 0.05994 -0.00654 -0.01662 -0.00751 AFIX 43 H7 2 0.495655 1.090769 0.661960 11.00000 -1.20000 AFIX 0 C7A 1 0.419516 0.963293 0.627610 11.00000 0.04563 0.05048 = 0.04831 -0.00572 -0.00407 0.00375 C11 1 0.497545 1.292409 0.594331 11.00000 0.07673 0.08748 = 0.08146 0.00530 -0.01786 -0.03987 AFIX 137 H11A 2 0.517485 1.268901 0.573076 11.00000 -1.50000 H11B 2 0.535773 1.253140 0.610289 11.00000 -1.50000 H11C 2 0.479986 1.488482 0.596860 11.00000 -1.50000 AFIX 0 PART 1 C21 1 0.381392 1.066436 0.541710 21.00000 0.03506 0.03655 = 0.05168 -0.00310 -0.00055 0.00236 C22 1 0.407100 1.327396 0.529232 21.00000 0.04493 0.04080 = 0.05662 -0.00847 -0.00658 -0.00075 AFIX 43 H22 2 0.428237 1.463717 0.543290 21.00000 -1.20000 AFIX 0 C23 1 0.402333 1.391140 0.496698 21.00000 0.04050 0.03935 = 0.06009 0.00374 -0.00253 -0.00579 AFIX 43 H23 2 0.420321 1.567489 0.488980 21.00000 -1.20000 AFIX 0 C24 1 0.370400 1.189749 0.475448 21.00000 0.03680 0.03752 = 0.05516 -0.00205 -0.00312 -0.00091 C25 1 0.344435 0.927917 0.487422 21.00000 0.03662 0.03983 = 0.05484 -0.00420 -0.00480 -0.00360 AFIX 43 H25 2 0.323365 0.791312 0.473380 21.00000 -1.20000 AFIX 0 C26 1 0.349696 0.869185 0.520004 21.00000 0.03380 0.03843 = 0.05772 0.00201 -0.00050 -0.00254 AFIX 43 H26 2 0.331585 0.692997 0.527713 21.00000 -1.20000 AFIX 0 O24 4 0.374394 1.249891 0.443077 21.00000 0.05795 0.06900 = 0.04884 0.00117 -0.00343 -0.01723 C27 1 0.327617 1.101251 0.421090 21.00000 0.05216 0.07947 = 0.05918 0.00126 -0.00637 -0.01883 AFIX 23 H27A 2 0.276163 1.119638 0.427597 21.00000 -1.20000 H27B 2 0.340406 0.895975 0.420856 21.00000 -1.20000 AFIX 0 C28 1 0.336486 1.223550 0.389322 21.00000 0.06248 0.07839 = 0.05681 -0.00953 -0.00395 -0.01482 C29 1 0.346773 1.295438 0.362945 21.00000 0.09932 0.10398 = 0.05666 0.00110 -0.00041 -0.01497 AFIX 163 H29 2 0.355047 1.353255 0.341732 21.00000 -1.20000 AFIX 0 PART 0 PART 2 SAME 0.01 0.02 C21 > C29 C31 1 0.381392 1.066436 0.541710 -21.00000 0.03506 0.03655 = 0.05168 -0.00310 -0.00055 0.00236 C32 1 0.445133 1.134995 0.525093 -21.00000 0.03271 0.04216 = 0.05558 -0.00677 -0.00494 0.00159 AFIX 43 H32 2 0.490748 1.142697 0.536098 -21.00000 -1.20000 AFIX 0 C33 1 0.441761 1.191975 0.492420 -21.00000 0.03434 0.04223 = 0.05329 -0.00186 0.00803 -0.00315 AFIX 43 H33 2 0.485009 1.239637 0.481534 -21.00000 -1.20000 AFIX 0 C34 1 0.374084 1.178796 0.475544 -21.00000 0.03673 0.04069 = 0.04584 -0.00230 0.00417 0.00118 C35 1 0.309985 1.102857 0.491761 -21.00000 0.03481 0.04208 = 0.04781 0.00218 -0.00638 -0.00042 AFIX 43 H35 2 0.264598 1.089957 0.480636 -21.00000 -1.20000 AFIX 0 C36 1 0.314097 1.046708 0.524475 -21.00000 0.03586 0.04665 = 0.05279 -0.00031 0.00461 -0.00495 AFIX 43 H36 2 0.271105 0.994545 0.535302 -21.00000 -1.20000 AFIX 0 O34 4 0.373179 1.268041 0.443924 -21.00000 0.05795 0.06900 = 0.04884 0.00117 -0.00343 -0.01723 C37 1 0.312507 1.195907 0.423541 -21.00000 0.05216 0.07947 = 0.05918 0.00126 -0.00637 -0.01883 AFIX 23 H37A 2 0.267507 1.287359 0.431319 -21.00000 -1.20000 H37B 2 0.305066 0.986622 0.423469 -21.00000 -1.20000 AFIX 0 C38 1 0.327649 1.295752 0.391276 -21.00000 0.06248 0.07839 = 0.05681 -0.00953 -0.00395 -0.01482 C39 1 0.330557 1.387993 0.365257 -21.00000 0.09932 0.10398 = 0.05666 0.00110 -0.00041 -0.01497 AFIX 163 H39 2 0.332893 1.462127 0.344346 -21.00000 -1.20000 AFIX 0 C51 1 0.327894 0.464634 0.703025 11.00000 0.06586 0.07459 = 0.04920 -0.00228 -0.00546 0.00152 O51 4 0.268959 0.338602 0.700801 11.00000 0.07684 0.12062 = 0.05783 0.01571 -0.00618 -0.02515 O52 4 0.370519 0.458926 0.729631 11.00000 0.07844 0.09757 = 0.05198 0.00993 -0.01225 -0.00679 C52 1 0.343332 0.289142 0.756889 11.00000 0.09387 0.10283 = 0.05500 0.01709 -0.00538 -0.00482 AFIX 23 H52A 2 0.299081 0.379777 0.765518 11.00000 -1.20000 H52B 2 0.330412 0.093894 0.749784 11.00000 -1.20000 AFIX 0 C53 1 0.400896 0.276412 0.781454 11.00000 0.11846 0.18011 = 0.07546 0.03875 -0.02419 -0.01392 AFIX 137 H53A 2 0.382013 0.182208 0.800368 11.00000 -1.50000 H53B 2 0.416643 0.470404 0.786916 11.00000 -1.50000 H53C 2 0.442506 0.168117 0.773496 11.00000 -1.50000 AFIX 0 HKLF 4 REM b2cg REM R1 = 0.0676 for 2002 Fo > 4sig(Fo) and 0.1145 for all 3350 data REM 286 parameters refined using 93 restraints END WGHT 0.0762 3.8365 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.243, deepest hole -0.226, 1-sigma level 0.043 Q1 1 0.4851 1.4184 0.6203 11.00000 0.05 0.24 Q2 1 0.4615 1.4712 0.5773 11.00000 0.05 0.20 Q3 1 0.2964 0.3467 0.6323 11.00000 0.05 0.13 Q4 1 0.3851 0.6009 0.5929 11.00000 0.05 0.13 Q5 1 0.4380 1.7075 0.4792 11.00000 0.05 0.13 Q6 1 0.3182 1.4429 0.4406 11.00000 0.05 0.13 Q7 1 0.3979 1.4296 0.6162 11.00000 0.05 0.12 Q8 1 0.4575 0.0976 0.7512 11.00000 0.05 0.12 Q9 1 0.4021 1.5702 0.4409 11.00000 0.05 0.12 Q10 1 0.2712 0.7142 0.4107 11.00000 0.05 0.12 Q11 1 0.5593 1.1461 0.5993 11.00000 0.05 0.12 Q12 1 0.3645 0.6482 0.5213 11.00000 0.05 0.11 Q13 1 0.5143 1.2368 0.5507 11.00000 0.05 0.11 Q14 1 0.4126 0.7806 0.5324 11.00000 0.05 0.11 Q15 1 0.3472 1.1985 0.3020 11.00000 0.05 0.11 Q16 1 0.4907 1.1409 0.4706 11.00000 0.05 0.11 Q17 1 0.2788 1.0620 0.4233 11.00000 0.05 0.11 Q18 1 0.3562 0.3447 0.6392 11.00000 0.05 0.11 Q19 1 0.4455 -0.0371 0.7493 11.00000 0.05 0.11 Q20 1 0.5037 1.2477 0.4801 11.00000 0.05 0.11 Q21 1 0.2410 0.2640 0.6349 11.00000 0.05 0.11 Q22 1 0.3970 0.4051 0.6525 11.00000 0.05 0.10 Q23 1 0.2191 0.1887 0.6968 11.00000 0.05 0.10 Q24 1 0.3427 1.2596 0.6120 11.00000 0.05 0.10 Q25 1 0.4109 0.9740 0.7242 11.00000 0.05 0.10 Q26 1 0.5598 1.0626 0.5426 11.00000 0.05 0.10 Q27 1 0.3996 1.6351 0.4798 11.00000 0.05 0.10 Q28 1 0.2708 0.1580 0.7781 11.00000 0.05 0.10 Q29 1 0.4805 1.1836 0.7003 11.00000 0.05 0.10 Q30 1 0.4153 1.2948 0.6693 11.00000 0.05 0.10 ; _shelx_res_checksum 89941 _shelxl_version_number 2.014 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_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N N1 0.43626(12) 1.0912(5) 0.59851(6) 0.0489(6) Uani d 1 . . C C2 0.38294(15) 0.9896(6) 0.57634(7) 0.0446(7) Uani d 1 . . N N3 0.33476(13) 0.8107(6) 0.58926(6) 0.0512(7) Uani d 1 . . C C3A 0.35648(15) 0.7906(7) 0.62171(7) 0.0495(7) Uani d 1 . . C C4 0.32625(17) 0.6286(8) 0.64653(7) 0.0566(8) Uani d 1 . . H H4 0.2840 0.5148 0.6429 0.068 Uiso calc 1 . . C C5 0.36027(17) 0.6401(7) 0.67670(7) 0.0544(8) Uani d 1 . . C C6 0.42355(19) 0.8131(8) 0.68213(8) 0.0637(9) Uani d 1 . . H H6 0.4455 0.8170 0.7027 0.076 Uiso calc 1 . . C C7 0.45376(18) 0.9757(8) 0.65814(8) 0.0619(9) Uani d 1 . . H H7 0.4957 1.0908 0.6620 0.074 Uiso calc 1 . . C C7A 0.41952(16) 0.9633(7) 0.62761(7) 0.0482(7) Uani d 1 . . C C11 0.4975(2) 1.2924(9) 0.59433(9) 0.0821(12) Uani d 1 . . H H11A 0.5175 1.2689 0.5731 0.123 Uiso calc 1 . . H H11B 0.5358 1.2531 0.6103 0.123 Uiso calc 1 . . H H11C 0.4800 1.4885 0.5969 0.123 Uiso calc 1 . . C C21 0.38139(14) 1.0664(6) 0.54171(7) 0.0411(6) Uani d 0.494(5) A 1 C C22 0.4071(3) 1.3274(12) 0.52923(13) 0.0475(16) Uani d 0.494(5) A 1 H H22 0.4282 1.4637 0.5433 0.057 Uiso calc 0.494(5) A 1 C C23 0.4023(3) 1.3911(13) 0.49670(13) 0.0467(15) Uani d 0.494(5) A 1 H H23 0.4203 1.5675 0.4890 0.056 Uiso calc 0.494(5) A 1 C C24 0.370(2) 1.190(10) 0.4754(3) 0.043(4) Uani d 0.494(5) A 1 C C25 0.3444(3) 0.9279(13) 0.48742(13) 0.0438(15) Uani d 0.494(5) A 1 H H25 0.3234 0.7913 0.4734 0.053 Uiso calc 0.494(5) A 1 C C26 0.3497(3) 0.8692(12) 0.52000(12) 0.0433(15) Uani d 0.494(5) A 1 H H26 0.3316 0.6930 0.5277 0.052 Uiso calc 0.494(5) A 1 O O24 0.374(4) 1.250(18) 0.4431(5) 0.059(3) Uani d 0.494(5) A 1 C C27 0.3276(10) 1.101(4) 0.4211(3) 0.064(4) Uani d 0.494(5) A 1 H H27A 0.2762 1.1196 0.4276 0.076 Uiso calc 0.494(5) A 1 H H27B 0.3404 0.8960 0.4209 0.076 Uiso calc 0.494(5) A 1 C C28 0.336(2) 1.224(9) 0.3893(4) 0.066(7) Uani d 0.494(5) A 1 C C29 0.347(2) 1.295(7) 0.3629(5) 0.087(6) Uani d 0.494(5) A 1 H H29 0.3550 1.3533 0.3417 0.104 Uiso calc 0.494(5) A 1 C C31 0.38139(14) 1.0664(6) 0.54171(7) 0.0411(6) Uani d 0.506(5) A 2 C C32 0.4451(3) 1.1350(13) 0.52509(12) 0.0436(14) Uani d 0.506(5) A 2 H H32 0.4907 1.1427 0.5361 0.052 Uiso calc 0.506(5) A 2 C C33 0.4418(3) 1.1920(13) 0.49242(12) 0.0432(15) Uani d 0.506(5) A 2 H H33 0.4850 1.2396 0.4815 0.052 Uiso calc 0.506(5) A 2 C C34 0.3741(18) 1.179(9) 0.4755(3) 0.041(3) Uani d 0.506(5) A 2 C C35 0.3100(3) 1.1029(14) 0.49176(12) 0.0417(14) Uani d 0.506(5) A 2 H H35 0.2646 1.0900 0.4806 0.050 Uiso calc 0.506(5) A 2 C C36 0.3141(3) 1.0467(14) 0.52448(12) 0.0451(15) Uani d 0.506(5) A 2 H H36 0.2711 0.9945 0.5353 0.054 Uiso calc 0.506(5) A 2 O O34 0.373(4) 1.268(18) 0.4439(5) 0.059(3) Uani d 0.506(5) A 2 C C37 0.3125(9) 1.196(4) 0.4235(3) 0.064(4) Uani d 0.506(5) A 2 H H37A 0.2675 1.2874 0.4313 0.076 Uiso calc 0.506(5) A 2 H H37B 0.3051 0.9866 0.4235 0.076 Uiso calc 0.506(5) A 2 C C38 0.328(2) 1.296(9) 0.3913(3) 0.066(7) Uani d 0.506(5) A 2 C C39 0.331(2) 1.388(6) 0.3653(5) 0.087(6) Uani d 0.506(5) A 2 H H39 0.3329 1.4621 0.3443 0.104 Uiso calc 0.506(5) A 2 C C51 0.3279(2) 0.4646(8) 0.70302(8) 0.0633(9) Uani d 1 B 2 O O51 0.26896(15) 0.3386(7) 0.70080(5) 0.0852(9) Uani d 1 B 2 O O52 0.37052(14) 0.4589(6) 0.72963(5) 0.0762(8) Uani d 1 B 2 C C52 0.3433(2) 0.2891(10) 0.75689(8) 0.0840(12) Uani d 1 B 2 H H52A 0.2991 0.3798 0.7655 0.101 Uiso calc 1 B 2 H H52B 0.3304 0.0939 0.7498 0.101 Uiso calc 1 B 2 C C53 0.4009(3) 0.2764(15) 0.78145(10) 0.125(2) Uani d 1 B 2 H H53A 0.3820 0.1822 0.8004 0.187 Uiso calc 1 B 2 H H53B 0.4166 0.4704 0.7869 0.187 Uiso calc 1 B 2 H H53C 0.4425 0.1681 0.7735 0.187 Uiso calc 1 B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.0422(13) 0.0431(14) 0.0613(16) -0.0045(11) -0.0053(11) -0.0034(12) C2 0.0377(14) 0.0422(17) 0.0538(17) 0.0026(13) -0.0032(12) -0.0030(14) N3 0.0463(13) 0.0586(16) 0.0486(14) -0.0093(13) -0.0047(11) -0.0011(12) C3A 0.0455(16) 0.0568(19) 0.0459(16) 0.0009(15) -0.0051(13) -0.0032(15) C4 0.0532(17) 0.065(2) 0.0511(18) -0.0082(16) -0.0030(14) -0.0004(16) C5 0.0539(18) 0.061(2) 0.0477(18) 0.0026(16) -0.0044(14) -0.0045(16) C6 0.065(2) 0.072(2) 0.0534(19) -0.0010(18) -0.0143(16) -0.0040(18) C7 0.0579(19) 0.067(2) 0.060(2) -0.0075(17) -0.0166(16) -0.0065(18) C7A 0.0456(16) 0.0505(18) 0.0483(17) 0.0038(14) -0.0041(13) -0.0057(15) C11 0.077(2) 0.087(3) 0.081(3) -0.040(2) -0.018(2) 0.005(2) C21 0.0351(13) 0.0366(15) 0.0517(16) 0.0024(12) -0.0005(12) -0.0031(13) C22 0.045(3) 0.041(3) 0.057(3) -0.001(3) -0.007(3) -0.008(3) C23 0.041(3) 0.039(3) 0.060(3) -0.006(3) -0.003(3) 0.004(3) C24 0.037(6) 0.038(6) 0.055(6) -0.001(6) -0.003(5) -0.002(5) C25 0.037(3) 0.040(3) 0.055(3) -0.004(3) -0.005(2) -0.004(3) C26 0.034(3) 0.038(3) 0.058(3) -0.003(3) -0.001(2) 0.002(3) O24 0.0579(19) 0.069(7) 0.0488(14) -0.017(4) -0.0034(16) 0.001(3) C27 0.052(6) 0.079(10) 0.059(3) -0.019(6) -0.006(3) 0.001(4) C28 0.062(8) 0.078(17) 0.057(2) -0.015(10) -0.004(3) -0.010(5) C29 0.099(14) 0.104(17) 0.057(3) -0.015(10) 0.000(4) 0.001(7) C31 0.0351(13) 0.0366(15) 0.0517(16) 0.0024(12) -0.0005(12) -0.0031(13) C32 0.033(3) 0.042(3) 0.056(3) 0.002(2) -0.005(2) -0.007(3) C33 0.034(3) 0.042(3) 0.053(3) -0.003(3) 0.008(2) -0.002(3) C34 0.037(6) 0.041(6) 0.046(5) 0.001(5) 0.004(5) -0.002(5) C35 0.035(3) 0.042(3) 0.048(3) 0.000(3) -0.006(2) 0.002(3) C36 0.036(3) 0.047(3) 0.053(3) -0.005(3) 0.005(2) 0.000(3) O34 0.0579(19) 0.069(7) 0.0488(14) -0.017(4) -0.0034(16) 0.001(3) C37 0.052(6) 0.079(10) 0.059(3) -0.019(6) -0.006(3) 0.001(4) C38 0.062(8) 0.078(17) 0.057(2) -0.015(10) -0.004(3) -0.010(5) C39 0.099(14) 0.104(17) 0.057(3) -0.015(10) 0.000(4) 0.001(7) C51 0.066(2) 0.075(2) 0.0492(19) 0.0015(19) -0.0055(16) -0.0023(18) O51 0.0768(17) 0.121(2) 0.0578(15) -0.0251(17) -0.0062(12) 0.0157(15) O52 0.0784(16) 0.098(2) 0.0520(13) -0.0068(15) -0.0122(12) 0.0099(13) C52 0.094(3) 0.103(3) 0.055(2) -0.005(2) -0.0054(19) 0.017(2) C53 0.118(4) 0.180(6) 0.075(3) -0.014(4) -0.024(3) 0.039(3) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C7A N1 C2 . . 105.9(2) ? C7A N1 C11 . . 123.7(3) ? C2 N1 C11 . . 130.5(3) ? N3 C2 N1 . . 113.1(2) ? N3 C2 C21 . . 122.9(2) ? N1 C2 C21 . . 124.0(3) ? C2 N3 C3A . . 104.9(2) ? C4 C3A N3 . . 129.9(3) ? C4 C3A C7A . . 120.1(3) ? N3 C3A C7A . . 110.0(3) ? C5 C4 C3A . . 118.4(3) ? C5 C4 H4 . . 120.8 ? C3A C4 H4 . . 120.8 ? C4 C5 C6 . . 120.8(3) ? C4 C5 C51 . . 118.0(3) ? C6 C5 C51 . . 121.2(3) ? C7 C6 C5 . . 121.8(3) ? C7 C6 H6 . . 119.1 ? C5 C6 H6 . . 119.1 ? C6 C7 C7A . . 117.5(3) ? C6 C7 H7 . . 121.3 ? C7A C7 H7 . . 121.3 ? N1 C7A C7 . . 132.3(3) ? N1 C7A C3A . . 106.1(2) ? C7 C7A C3A . . 121.5(3) ? N1 C11 H11A . . 109.5 ? N1 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? N1 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? C22 C21 C26 . . 117.3(4) ? C22 C21 C2 . . 124.6(3) ? C26 C21 C2 . . 118.1(3) ? C23 C22 C21 . . 122.1(5) ? C23 C22 H22 . . 119.0 ? C21 C22 H22 . . 119.0 ? C22 C23 C24 . . 119.5(8) ? C22 C23 H23 . . 120.3 ? C24 C23 H23 . . 120.3 ? O24 C24 C25 . . 123(3) ? O24 C24 C23 . . 117(2) ? C25 C24 C23 . . 119.3(5) ? C26 C25 C24 . . 120.2(8) ? C26 C25 H25 . . 119.9 ? C24 C25 H25 . . 119.9 ? C25 C26 C21 . . 121.6(5) ? C25 C26 H26 . . 119.2 ? C21 C26 H26 . . 119.2 ? C24 O24 C27 . . 119.6(12) ? O24 C27 C28 . . 109.0(11) ? O24 C27 H27A . . 109.9 ? C28 C27 H27A . . 109.9 ? O24 C27 H27B . . 109.9 ? C28 C27 H27B . . 109.9 ? H27A C27 H27B . . 108.3 ? C29 C28 C27 . . 173(5) ? C28 C29 H29 . . 180.0 ? C33 C32 H32 . . 119.7 ? C32 C33 C34 . . 120.4(7) ? C32 C33 H33 . . 119.8 ? C34 C33 H33 . . 119.8 ? O34 C34 C35 . . 123(3) ? O34 C34 C33 . . 117(2) ? C35 C34 C33 . . 119.6(5) ? C36 C35 C34 . . 119.4(7) ? C36 C35 H35 . . 120.3 ? C34 C35 H35 . . 120.3 ? C35 C36 H36 . . 119.3 ? C34 O34 C37 . . 119.8(12) ? O34 C37 C38 . . 108.8(10) ? O34 C37 H37A . . 109.9 ? C38 C37 H37A . . 109.9 ? O34 C37 H37B . . 109.9 ? C38 C37 H37B . . 109.9 ? H37A C37 H37B . . 108.3 ? C39 C38 C37 . . 171(4) ? C38 C39 H39 . . 180.0 ? O51 C51 O52 . . 123.0(3) ? O51 C51 C5 . . 124.0(3) ? O52 C51 C5 . . 113.0(3) ? C51 O52 C52 . . 116.9(3) ? C53 C52 O52 . . 108.7(3) ? C53 C52 H52A . . 110.0 ? O52 C52 H52A . . 110.0 ? C53 C52 H52B . . 110.0 ? O52 C52 H52B . . 110.0 ? H52A C52 H52B . . 108.3 ? C52 C53 H53A . . 109.5 ? C52 C53 H53B . . 109.5 ? H53A C53 H53B . . 109.5 ? C52 C53 H53C . . 109.5 ? H53A C53 H53C . . 109.5 ? H53B C53 H53C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 C7A . 1.376(4) ? N1 C2 . 1.393(3) ? N1 C11 . 1.449(4) ? C2 N3 . 1.313(4) ? C2 C21 . 1.473(4) ? N3 C3A . 1.392(4) ? C3A C4 . 1.385(4) ? C3A C7A . 1.399(4) ? C4 C5 . 1.379(4) ? C4 H4 . 0.9300 ? C5 C6 . 1.401(5) ? C5 C51 . 1.480(5) ? C6 C7 . 1.361(5) ? C6 H6 . 0.9300 ? C7 C7A . 1.394(4) ? C7 H7 . 0.9300 ? C11 H11A . 0.9600 ? C11 H11B . 0.9600 ? C11 H11C . 0.9600 ? C21 C22 . 1.386(6) ? C21 C26 . 1.389(5) ? C22 C23 . 1.376(7) ? C22 H22 . 0.9300 ? C23 C24 . 1.39(2) ? C23 H23 . 0.9300 ? C24 O24 . 1.368(9) ? C24 C25 . 1.38(2) ? C25 C26 . 1.374(6) ? C25 H25 . 0.9300 ? C26 H26 . 0.9300 ? O24 C27 . 1.403(18) ? C27 C28 . 1.439(7) ? C27 H27A . 0.9700 ? C27 H27B . 0.9700 ? C28 C29 . 1.156(8) ? C29 H29 . 0.9300 ? C32 C33 . 1.375(6) ? C32 H32 . 0.9300 ? C33 C34 . 1.39(2) ? C33 H33 . 0.9300 ? C34 O34 . 1.369(9) ? C34 C35 . 1.39(2) ? C35 C36 . 1.376(6) ? C35 H35 . 0.9300 ? C36 H36 . 0.9300 ? O34 C37 . 1.404(18) ? C37 C38 . 1.440(7) ? C37 H37A . 0.9700 ? C37 H37B . 0.9700 ? C38 C39 . 1.157(8) ? C39 H39 . 0.9300 ? C51 O51 . 1.208(4) ? C51 O52 . 1.328(4) ? O52 C52 . 1.460(4) ? C52 C53 . 1.436(5) ? C52 H52A . 0.9700 ? C52 H52B . 0.9700 ? C53 H53A . 0.9600 ? C53 H53B . 0.9600 ? C53 H53C . 0.9600 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C23 H23 Cg1 1_565 0.93 2.77 3.412(9) 127 no C26 H26 Cg1 1_545 0.93 2.87 3.508(9) 127 no C35 H35 Cg2 7_576 0.93 2.87 3.555(9) 131 no 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C7A N1 C2 N3 . . . . 0.1(3) ? C11 N1 C2 N3 . . . . -178.9(3) ? C7A N1 C2 C21 . . . . -178.2(2) ? C11 N1 C2 C21 . . . . 2.8(5) ? N1 C2 N3 C3A . . . . 0.0(3) ? C21 C2 N3 C3A . . . . 178.4(3) ? C2 N3 C3A C4 . . . . -178.9(3) ? C2 N3 C3A C7A . . . . -0.2(3) ? N3 C3A C4 C5 . . . . 177.9(3) ? C7A C3A C4 C5 . . . . -0.7(5) ? C3A C4 C5 C6 . . . . 0.4(5) ? C3A C4 C5 C51 . . . . -179.6(3) ? C4 C5 C6 C7 . . . . 0.1(5) ? C51 C5 C6 C7 . . . . -179.9(3) ? C5 C6 C7 C7A . . . . -0.3(5) ? C2 N1 C7A C7 . . . . 178.1(3) ? C11 N1 C7A C7 . . . . -2.8(5) ? C2 N1 C7A C3A . . . . -0.2(3) ? C11 N1 C7A C3A . . . . 178.9(3) ? C6 C7 C7A N1 . . . . -178.2(3) ? C6 C7 C7A C3A . . . . 0.0(5) ? C4 C3A C7A N1 . . . . 179.1(3) ? N3 C3A C7A N1 . . . . 0.3(3) ? C4 C3A C7A C7 . . . . 0.5(5) ? N3 C3A C7A C7 . . . . -178.3(3) ? N3 C2 C21 C22 . . . . 151.8(4) ? N1 C2 C21 C22 . . . . -30.0(5) ? N3 C2 C21 C26 . . . . -25.8(5) ? N1 C2 C21 C26 . . . . 152.4(4) ? C26 C21 C22 C23 . . . . -0.5(7) ? C2 C21 C22 C23 . . . . -178.1(4) ? C21 C22 C23 C24 . . . . 0(3) ? C22 C23 C24 O24 . . . . -173(5) ? C22 C23 C24 C25 . . . . 0(5) ? O24 C24 C25 C26 . . . . 173(5) ? C23 C24 C25 C26 . . . . 1(5) ? C24 C25 C26 C21 . . . . -1(3) ? C22 C21 C26 C25 . . . . 0.5(7) ? C2 C21 C26 C25 . . . . 178.3(4) ? C25 C24 O24 C27 . . . . 24(11) ? C23 C24 O24 C27 . . . . -163(6) ? C24 O24 C27 C28 . . . . 174(7) ? C32 C33 C34 O34 . . . . 173(5) ? C32 C33 C34 C35 . . . . -1(5) ? O34 C34 C35 C36 . . . . -173(5) ? C33 C34 C35 C36 . . . . 1(5) ? C35 C34 O34 C37 . . . . -21(11) ? C33 C34 O34 C37 . . . . 165(6) ? C34 O34 C37 C38 . . . . -176(7) ? C4 C5 C51 O51 . . . . -8.8(5) ? C6 C5 C51 O51 . . . . 171.1(4) ? C4 C5 C51 O52 . . . . 171.1(3) ? C6 C5 C51 O52 . . . . -8.9(5) ? O51 C51 O52 C52 . . . . 0.3(5) ? C5 C51 O52 C52 . . . . -179.6(3) ? C51 O52 C52 C53 . . . . 172.2(4) ? _cod_database_fobs_code 2243846