#------------------------------------------------------------------------------ #$Date: 2020-02-04 05:17:25 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247537 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/70/1557040.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_1557040 loop_ _publ_author_name 'Sala, Samuele' 'Nealon, Gareth L.' 'Sobolev, Alexandre N.' 'Fromont, Jane' 'Gomez, Oliver' 'Flematti, Gavin R.' _publ_section_title ; Structure Reassignment of Echinosulfone A and the Echinosulfonic Acids A-D Supported by Single-Crystal X-ray Diffraction and Density Functional Theory Analysis. ; _journal_issue 1 _journal_name_full 'Journal of natural products' _journal_page_first 105 _journal_page_last 110 _journal_paper_doi 10.1021/acs.jnatprod.9b00902 _journal_volume 83 _journal_year 2020 _chemical_formula_moiety 'C17 H10 Br2 N2 O' _chemical_formula_sum 'C17 H10 Br2 N2 O' _chemical_formula_weight 418.09 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 91.005(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.0349(4) _cell_length_b 8.3874(4) _cell_length_c 17.4347(8) _cell_measurement_reflns_used 3042 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 67.186 _cell_measurement_theta_min 5.067 _cell_volume 1467.20(11) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics 'X-Seed v. 4.0 (Barbour, 2001)' _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT-2015/1 (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.4738 _diffrn_detector_type Ruby _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Gemini-R Ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0222565 _diffrn_orient_matrix_UB_12 0.0716168 _diffrn_orient_matrix_UB_13 -0.0801067 _diffrn_orient_matrix_UB_21 -0.0081228 _diffrn_orient_matrix_UB_22 -0.1679479 _diffrn_orient_matrix_UB_23 -0.0354987 _diffrn_orient_matrix_UB_31 -0.1517540 _diffrn_orient_matrix_UB_32 0.0196477 _diffrn_orient_matrix_UB_33 -0.0114776 _diffrn_radiation_monochromator mirror _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_unetI/netI 0.0526 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 10992 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 67.293 _diffrn_reflns_theta_max 67.293 _diffrn_reflns_theta_min 5.047 _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 7.030 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.65065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.893 _exptl_crystal_description needle _exptl_crystal_F_000 816 _exptl_crystal_size_max 0.123 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_min 0.010 _refine_diff_density_max 1.134 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.139 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 205 _refine_ls_number_reflns 2602 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.000 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0437 _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^)+(0.0728P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1056 _refine_ls_wR_factor_ref 0.1177 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2090 _reflns_number_total 2602 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np9b00902_si_001.cif _cod_data_source_block ss_Cre-2 _cod_depositor_comments 'Adding full bibliography for 1557040.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557040 _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. ; _shelx_estimated_absorpt_t_min 0.478 _shelx_estimated_absorpt_t_max 0.933 _shelx_res_file ; TITL ss_Cre-2 in P2(1)/n ss_Cre-2.res created by SHELXL-2018/3 at 13:58:49 on 21-Jun-2018 CELL 1.54178 10.0349 8.3874 17.4347 90.000 91.005 90.000 ZERR 4.00 0.0004 0.0004 0.0008 0.000 0.004 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O BR UNIT 68 40 8 4 8 ACTA TEMP -173 SIZE 0.123 0.052 0.01 ! colorless needle CONF REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, y-1/2, -z+3/2 HTAB N1 O1_$1 EQIV $2 -x+1, -y+2, -z+1 HTAB C25 O1_$2 SADI 0.01 N1 H1 N2 H2 BOND $H L.S. 10 WGHT 0.072800 FVAR 0.15396 BR1 5 -0.285597 0.647079 0.771897 11.00000 0.02267 0.04370 = 0.03552 -0.00635 0.00574 -0.00286 BR2 5 0.988302 0.778297 0.412852 11.00000 0.02932 0.05043 = 0.03943 0.01699 0.01209 0.00763 O1 4 0.339420 0.796498 0.584423 11.00000 0.02598 0.01967 = 0.02804 0.00146 0.00413 0.00181 C1 1 0.375568 0.671504 0.616973 11.00000 0.02555 0.02353 = 0.01954 -0.00252 0.00114 -0.00167 N1 3 0.228760 0.483816 0.784128 11.00000 0.02650 0.02202 = 0.02996 0.00639 0.00460 -0.00118 H1 2 0.236387 0.428358 0.819467 11.00000 -1.20000 C11 1 0.333214 0.511782 0.737467 11.00000 0.02402 0.02009 = 0.02934 -0.00029 0.00188 0.00106 AFIX 43 H11 2 0.421387 0.473833 0.746171 11.00000 -1.20000 AFIX 0 C12 1 0.292864 0.602756 0.675974 11.00000 0.02788 0.01592 = 0.02721 -0.00303 -0.00060 -0.00330 C13 1 0.152439 0.632658 0.685534 11.00000 0.02623 0.01602 = 0.02370 -0.00293 0.00206 -0.00155 C14 1 0.053712 0.715561 0.643716 11.00000 0.02818 0.02154 = 0.02611 -0.00430 -0.00413 0.00060 AFIX 43 H14 2 0.075320 0.768378 0.597364 11.00000 -1.20000 AFIX 0 C15 1 -0.074807 0.719833 0.670350 11.00000 0.02344 0.02213 = 0.03231 -0.00428 -0.00198 0.00026 AFIX 43 H15 2 -0.142077 0.777175 0.643036 11.00000 -1.20000 AFIX 0 C16 1 -0.105180 0.638850 0.738026 11.00000 0.02004 0.02974 = 0.02653 -0.01001 0.00751 -0.00315 C17 1 -0.014245 0.554947 0.780670 11.00000 0.03165 0.02400 = 0.02822 -0.00320 0.00432 -0.00437 AFIX 43 H17 2 -0.037970 0.500031 0.826090 11.00000 -1.20000 AFIX 0 C18 1 0.115351 0.554525 0.753723 11.00000 0.02640 0.02027 = 0.02677 -0.00327 -0.00185 0.00194 N2 3 0.657467 0.413024 0.573904 11.00000 0.02601 0.02024 = 0.03128 0.00006 -0.00022 0.00475 H2 2 0.694266 0.332037 0.572854 11.00000 -1.20000 C21 1 0.537839 0.439803 0.605942 11.00000 0.02330 0.01987 = 0.02929 -0.00107 0.00038 -0.00149 AFIX 43 H21 2 0.486256 0.361643 0.631383 11.00000 -1.20000 AFIX 0 C22 1 0.501637 0.597359 0.596268 11.00000 0.02391 0.02207 = 0.02214 -0.00161 -0.00162 0.00174 C23 1 0.606683 0.671323 0.553943 11.00000 0.02254 0.02385 = 0.02055 -0.00118 -0.00053 0.00083 C24 1 0.630211 0.826644 0.526266 11.00000 0.02643 0.02511 = 0.02657 0.00216 -0.00028 0.00422 AFIX 43 H24 2 0.568162 0.909843 0.535229 11.00000 -1.20000 AFIX 0 C25 1 0.744892 0.855826 0.485932 11.00000 0.02989 0.02635 = 0.02806 0.00578 0.00643 0.00335 AFIX 43 H25 2 0.763422 0.960182 0.467818 11.00000 -1.20000 AFIX 0 C26 1 0.833834 0.730751 0.471843 11.00000 0.02124 0.04020 = 0.02608 0.00479 0.00583 0.00068 C27 1 0.817036 0.577737 0.497823 11.00000 0.02357 0.03166 = 0.02312 -0.00404 -0.00007 0.00716 AFIX 43 H27 2 0.879113 0.495221 0.487630 11.00000 -1.20000 AFIX 0 C28 1 0.701913 0.551679 0.540443 11.00000 0.02511 0.02299 = 0.02640 -0.00274 -0.00146 0.00059 HKLF 4 REM ss_Cre-2 in P2(1)/n REM wR2 = 0.1177, GooF = S = 1.000, Restrained GooF = 1.000 for all data REM R1 = 0.0437 for 2090 Fo > 4sig(Fo) and 0.0573 for all 2602 data REM 205 parameters refined using 1 restraints END WGHT 0.0652 0.0000 REM Highest difference peak 1.134, deepest hole -0.496, 1-sigma level 0.139 Q1 1 -0.1899 0.6331 0.7579 11.00000 0.05 1.13 Q2 1 0.9095 0.7660 0.4336 11.00000 0.05 0.82 Q3 1 -0.3621 0.6565 0.7915 11.00000 0.05 0.81 Q4 1 -0.2552 0.5920 0.8077 11.00000 0.05 0.76 Q5 1 1.0748 0.7703 0.4003 11.00000 0.05 0.74 Q6 1 -0.3159 0.5893 0.7370 11.00000 0.05 0.67 Q7 1 1.0205 0.7237 0.4440 11.00000 0.05 0.66 Q8 1 1.0190 0.8368 0.4559 11.00000 0.05 0.63 Q9 1 0.9541 0.7250 0.3718 11.00000 0.05 0.63 Q10 1 -0.3289 0.6970 0.7245 11.00000 0.05 0.58 Q11 1 -0.2765 0.7100 0.8123 11.00000 0.05 0.55 Q12 1 0.9971 0.5031 0.4187 11.00000 0.05 0.54 Q13 1 -0.1330 0.6470 0.6953 11.00000 0.05 0.50 Q14 1 0.9243 0.8344 0.3806 11.00000 0.05 0.50 Q15 1 -0.2775 0.9107 0.7771 11.00000 0.05 0.48 Q16 1 0.9868 0.9181 0.4123 11.00000 0.05 0.48 Q17 1 0.0795 0.7254 0.5424 11.00000 0.05 0.47 Q18 1 0.6970 0.3585 0.5947 11.00000 0.05 0.46 Q19 1 -0.2856 0.7737 0.7776 11.00000 0.05 0.46 Q20 1 0.6210 0.7205 0.5559 11.00000 0.05 0.44 ; _shelx_res_checksum 54514 _shelx_hkl_file ; 0 0 2 65.17 3.66 0 0 3 -0.09 1.07 0 0 4 263.18 10.41 0 0 5 0.11 1.75 0 0 5 -0.50 0.27 0 0 6 1227.79 28.18 0 0 7 0.38 1.84 0 0 -7 1.52 1.20 0 0 8 15.08 4.19 0 0 9 1.36 2.60 0 0 10 29.88 6.58 0 0 11 0.86 2.90 0 0 12 133.11 15.01 0 0 -12 136.87 6.44 0 0 12 137.71 7.94 0 0 -13 -0.48 0.84 0 0 13 0.45 1.41 0 0 -13 0.26 0.80 0 0 13 -0.58 2.67 0 0 14 -0.83 2.56 0 0 -14 1.55 1.12 0 0 -14 1.85 1.21 0 0 -15 1.00 0.91 0 0 -15 0.91 1.23 0 0 -16 95.99 6.01 0 0 -16 94.95 5.62 0 0 16 77.59 6.24 0 0 17 -1.58 1.64 0 0 -17 0.62 0.98 0 0 17 -0.50 1.40 0 0 -17 -0.97 1.11 0 0 -18 -1.70 1.14 0 0 -18 -0.29 0.82 0 0 18 -0.95 1.22 0 0 18 -0.87 1.34 0 0 19 0.03 1.32 0 0 -19 -1.42 0.96 0 0 20 17.16 2.23 0 0 20 18.37 2.42 0 0 -20 24.31 2.37 0 -1 0 -0.05 0.65 0 -1 1 87.50 4.43 0 -1 -1 90.64 4.23 0 -1 2 19.24 2.37 0 -1 -2 19.45 2.11 0 1 2 19.31 2.37 0 1 3 12.81 2.31 0 -1 3 10.17 1.89 0 -1 3 13.05 2.48 0 -1 -3 10.82 1.83 0 -1 4 126.77 7.79 0 1 4 114.24 6.93 0 -1 -4 115.20 5.61 0 1 5 126.33 8.25 0 -1 5 134.70 9.04 0 -1 -5 123.03 6.22 0 -1 -6 64.21 4.73 0 -1 6 68.63 7.18 0 1 6 72.99 6.94 0 1 7 134.61 10.32 0 -1 7 129.90 10.75 0 -1 -7 117.14 6.62 0 -1 8 544.04 23.22 0 1 8 601.72 23.61 0 -1 9 82.03 9.97 0 1 9 96.53 10.58 0 -1 10 11.28 4.26 0 1 10 19.73 5.36 0 -1 11 47.63 8.68 0 -1 11 53.31 4.87 0 1 11 68.88 10.42 0 -1 -11 57.38 4.01 0 1 12 15.16 5.29 0 -1 -12 22.59 2.69 0 -1 12 14.46 5.26 0 -1 12 23.06 3.53 0 1 -12 23.19 2.75 0 1 13 38.32 8.79 0 1 13 50.83 4.59 0 -1 -13 51.59 4.17 0 1 -13 49.83 4.16 0 -1 13 56.22 5.52 0 -1 13 42.27 8.77 0 -1 14 167.42 9.67 0 -1 14 143.58 16.65 0 1 14 147.63 8.14 0 1 -14 160.15 7.56 0 -1 -14 163.65 7.61 0 -1 -14 162.45 7.68 0 1 -15 5.64 1.82 0 1 15 10.30 2.36 0 -1 15 8.71 2.67 0 -1 -15 5.74 1.74 0 -1 -15 6.28 1.83 0 -1 15 6.08 2.21 0 -1 -16 1.38 1.11 0 1 -16 2.00 1.34 0 -1 -16 2.15 1.51 0 -1 16 2.18 1.62 0 1 16 2.08 1.50 0 -1 17 2.08 1.80 0 -1 -17 4.27 1.44 0 1 17 2.84 1.74 0 -1 -17 1.90 1.19 0 1 -17 2.41 1.35 0 -1 -18 -0.29 0.85 0 1 18 1.62 1.26 0 -1 18 2.07 1.67 0 1 -18 1.62 1.27 0 -1 -18 0.11 0.78 0 1 18 0.04 1.22 0 -1 19 2.02 1.43 0 -1 -19 2.18 1.06 0 1 19 0.60 1.32 0 1 -19 2.25 1.13 0 1 19 0.93 1.13 0 1 19 2.66 1.43 0 1 20 8.68 1.64 0 -1 -20 9.57 1.44 0 1 -20 12.46 1.75 0 1 20 9.31 1.88 0 -1 20 7.64 1.61 0 -2 0 373.51 12.32 0 -2 -1 1198.76 21.57 0 -2 1 1175.70 22.39 0 -2 2 194.81 9.58 0 -2 -2 204.00 9.02 0 -2 -3 324.25 11.57 0 -2 3 312.68 12.47 0 -2 -4 279.68 11.03 0 -2 4 275.62 12.00 0 2 4 274.65 12.13 0 -2 4 270.59 12.27 0 -2 5 199.59 11.57 0 -2 -5 199.96 9.80 0 2 5 204.03 11.16 0 -2 5 200.97 10.52 0 -2 -6 105.50 7.32 0 2 6 114.24 9.13 0 -2 6 96.13 8.79 0 2 7 70.45 7.79 0 -2 -7 64.64 5.97 0 -2 7 60.76 7.75 0 -2 8 12.86 3.92 0 2 8 18.44 4.56 0 2 9 4.78 2.85 0 -2 9 2.24 2.72 0 -2 10 16.63 5.02 0 2 10 24.37 5.88 0 -2 10 21.52 2.80 0 -2 11 6.51 1.88 0 2 -11 5.49 1.42 0 -2 11 4.53 2.95 0 -2 -11 4.08 1.21 0 2 11 8.18 1.85 0 -2 11 7.35 2.13 0 2 11 7.05 3.55 0 -2 12 56.51 4.83 0 -2 12 61.71 5.56 0 2 12 65.15 10.75 0 2 12 60.62 4.74 0 2 -12 63.83 4.49 0 -2 12 46.45 8.82 0 -2 -12 58.70 4.20 0 2 -13 1.01 1.04 0 -2 -13 0.82 1.19 0 -2 -13 2.51 1.15 0 2 13 1.84 2.34 0 -2 13 1.67 1.58 0 2 13 0.53 1.23 0 -2 13 -0.07 1.18 0 -2 -14 -0.78 0.99 0 -2 -14 1.34 1.13 0 2 -14 1.15 0.98 0 -2 14 1.61 1.80 0 -2 14 -0.78 1.26 0 2 14 1.78 1.55 0 -2 -15 2.87 1.25 0 -2 -15 3.79 1.62 0 -2 15 -1.00 1.69 0 2 15 1.28 1.51 0 2 -15 3.31 1.33 0 2 16 24.98 3.38 0 -2 -16 30.87 3.52 0 2 -16 33.34 3.57 0 -2 -16 32.96 3.43 0 -2 16 30.35 4.36 0 -2 -17 10.45 1.93 0 2 17 9.71 2.19 0 2 17 9.57 2.54 0 2 -17 10.01 2.13 0 -2 -17 10.66 2.18 0 2 18 18.56 2.82 0 -2 -18 17.45 2.48 0 -2 -18 23.29 2.56 0 2 18 19.24 3.04 0 2 -18 25.91 2.95 0 2 -19 9.46 1.81 0 2 19 7.03 1.67 0 2 19 8.85 2.05 0 2 19 9.36 2.05 0 -2 19 9.55 2.01 0 2 -20 4.97 1.26 0 -2 20 5.19 1.36 0 2 20 3.10 1.09 0 -3 0 -0.05 1.65 0 -3 -1 77.21 7.11 0 -3 1 86.85 7.70 0 -3 2 34.38 5.06 0 -3 -2 30.15 4.65 0 -3 -3 39.11 5.25 0 -3 3 46.34 5.95 0 -3 4 103.94 9.05 0 -3 -4 121.36 9.04 0 -3 -5 -0.08 1.20 0 -3 5 1.33 1.70 0 -3 5 0.09 1.30 0 -3 -6 2.79 2.39 0 -3 6 2.47 2.06 0 -3 7 108.05 10.80 0 -3 -7 148.58 10.83 0 3 8 2.76 2.29 0 -3 8 0.21 1.69 0 -3 9 110.22 6.80 0 3 -9 98.07 5.97 0 3 9 116.18 6.03 0 3 9 113.94 12.00 0 3 -10 53.93 3.74 0 3 10 63.60 4.35 0 -3 10 48.46 8.66 0 -3 10 63.42 5.43 0 -3 10 62.26 5.04 0 3 -10 52.70 4.66 0 3 10 62.50 9.53 0 3 11 3.14 1.41 0 3 11 3.96 1.27 0 -3 11 2.14 1.78 0 3 -11 2.08 1.08 0 3 11 5.51 3.11 0 -3 11 7.29 1.96 0 3 -12 60.16 4.38 0 -3 12 65.96 6.02 0 3 12 63.52 4.78 0 3 12 61.81 5.26 0 -3 -12 65.55 5.02 0 -3 -13 120.06 6.88 0 -3 13 118.14 8.24 0 3 -13 111.91 6.11 0 3 13 121.88 6.83 0 3 13 106.02 7.19 0 -3 -14 4.91 1.62 0 -3 14 6.08 2.35 0 3 14 3.21 1.73 0 3 14 6.25 2.03 0 3 -14 3.67 1.54 0 3 15 31.18 3.71 0 -3 -15 39.10 4.04 0 3 15 26.57 3.84 0 3 -15 31.60 3.55 0 -3 15 38.76 4.94 0 3 -16 2.36 1.29 0 -3 -16 2.49 1.40 0 3 16 2.69 1.69 0 -3 16 2.37 1.91 0 3 16 1.99 1.58 0 3 17 2.09 1.51 0 -3 -17 1.54 1.14 0 3 -17 0.57 1.01 0 3 17 -0.04 1.03 0 -3 17 0.96 1.44 0 -3 -18 10.23 1.94 0 3 -18 11.58 1.96 0 3 18 7.65 1.96 0 3 18 5.37 1.64 0 3 -19 21.07 2.32 0 -3 -19 22.41 2.29 0 -3 19 15.25 2.25 0 3 19 19.17 2.59 0 -4 0 6.17 3.09 0 -4 1 115.83 10.65 0 -4 -1 120.37 10.59 0 -4 -2 117.68 10.46 0 -4 2 133.32 11.68 0 -4 -3 15.51 4.24 0 -4 3 15.98 4.14 0 -4 4 178.46 13.94 0 -4 -4 185.19 13.38 0 -4 -5 6.97 3.01 0 -4 5 3.78 2.24 0 -4 5 4.83 2.57 0 -4 6 1.60 1.84 0 -4 6 8.81 3.71 0 -4 -7 53.36 8.01 0 -4 7 38.13 6.89 0 -4 8 9.37 3.86 0 4 -8 14.36 2.57 0 4 8 14.47 1.99 0 -4 -8 11.63 1.83 0 4 8 16.96 2.44 0 -4 8 14.12 2.64 0 -4 8 15.27 2.95 0 4 9 22.30 2.67 0 4 9 21.38 2.84 0 -4 -9 21.21 2.63 0 -4 9 14.96 4.86 0 -4 9 20.88 3.36 0 4 -9 17.40 2.90 0 4 -9 19.22 2.65 0 -4 9 20.78 3.08 0 -4 10 11.58 2.47 0 4 -10 11.84 2.48 0 -4 -10 13.03 2.21 0 -4 10 10.80 2.63 0 4 10 14.43 2.25 0 4 10 13.41 2.39 0 -4 10 12.11 4.65 0 4 -11 8.13 2.20 0 4 11 11.40 2.22 0 4 11 9.34 2.14 0 -4 11 8.93 2.70 0 -4 -11 12.18 2.35 0 4 -11 6.25 1.56 0 -4 11 11.55 2.64 0 4 12 15.61 2.58 0 -4 12 13.15 2.66 0 4 12 15.78 2.86 0 4 -12 10.36 1.88 0 -4 12 13.74 3.01 0 -4 -12 14.50 2.51 0 -4 -13 2.56 1.54 0 4 -13 0.96 1.02 0 4 13 0.65 1.17 0 4 13 -1.13 1.26 0 4 -14 -1.45 1.02 0 -4 14 0.70 1.72 0 4 14 -1.03 1.19 0 4 14 -1.14 1.31 0 -4 -14 0.15 1.07 0 -4 15 11.13 3.06 0 4 15 11.22 2.28 0 4 -15 10.88 1.93 0 -4 -15 12.91 2.51 0 4 15 9.53 2.36 0 4 16 9.52 2.13 0 -4 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8.07 2.19 -10 -2 3 10.15 2.05 -10 -2 3 9.79 2.01 -10 2 2 8.74 1.95 -10 2 2 10.36 2.29 -10 -2 2 7.19 2.29 -10 -2 2 13.06 2.31 -10 -2 2 9.85 2.04 -10 2 1 47.52 4.56 -10 2 1 49.38 4.27 -10 -2 1 45.35 4.35 -10 -2 1 44.34 3.98 -10 -2 1 46.66 3.88 -10 2 0 14.00 2.37 -10 2 0 9.22 2.27 -10 -2 0 11.52 2.40 -10 -2 0 13.92 2.39 -10 -2 0 9.18 1.87 -10 2 -1 45.60 4.44 -10 2 -1 44.69 4.07 -10 -2 -1 44.14 3.99 -10 -2 -1 48.59 4.10 -10 2 -2 10.48 2.05 -10 2 -2 9.82 2.36 -10 -2 -2 9.56 1.99 -10 -2 -2 10.48 2.15 -10 2 -3 2.77 1.66 -10 2 -3 4.61 1.84 -10 -2 -3 5.57 1.57 -10 2 -4 16.17 3.05 -10 2 -4 15.33 2.67 -10 -2 -4 16.30 2.41 -10 2 -5 5.98 1.94 -10 -2 -5 9.04 1.97 -10 2 -5 4.97 1.44 -10 2 -5 6.28 2.06 -10 2 -6 14.47 2.51 -10 -2 -6 17.94 2.39 -10 2 -6 12.71 2.13 -10 2 -6 13.59 2.70 -10 2 -7 2.18 1.19 -10 -2 -7 2.17 1.14 -10 2 -7 1.06 0.94 -10 2 -7 2.51 1.52 -10 2 -8 -1.15 1.08 -10 -2 -8 0.55 0.88 -10 2 -8 2.32 1.04 -10 2 -8 -0.88 1.01 -10 -2 -9 17.50 2.16 -10 2 -9 11.19 1.82 -10 -2 -10 24.82 2.35 -10 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8 -0.33 0.71 -11 -1 8 0.57 1.09 -11 1 7 1.60 1.04 -11 1 7 1.67 0.95 -11 -1 7 1.14 1.02 -11 1 6 1.40 1.09 -11 1 6 2.26 1.11 -11 -1 6 1.53 1.08 -11 -1 5 38.71 3.37 -11 -1 4 1.45 1.03 -11 -1 3 40.69 3.39 -11 1 2 2.94 1.25 -11 -1 2 0.50 0.91 -11 1 1 17.81 2.41 -11 1 0 1.36 1.10 -11 -1 0 1.36 0.91 -11 1 -1 4.25 1.53 -11 -1 -1 3.12 1.16 -11 1 -2 3.40 1.21 -11 -1 -2 6.04 1.46 -11 1 -3 64.28 4.09 -11 -1 -3 59.98 3.99 -11 1 -4 13.44 1.87 -11 -1 -4 11.66 1.92 -11 -1 -5 45.64 3.41 -11 1 -5 34.96 2.78 -11 -1 -6 1.72 0.96 -11 1 -6 1.17 0.77 -11 -1 -7 1.06 0.88 -11 -2 7 13.92 1.92 -11 2 6 29.13 2.92 -11 -2 6 26.06 2.82 -11 -2 6 21.10 2.33 -11 2 5 17.70 2.40 -11 -2 5 13.61 2.31 -11 -2 5 16.51 2.10 -11 2 4 74.94 4.82 -11 -2 4 64.95 4.56 -11 -2 4 67.58 4.13 -11 2 3 19.54 2.41 -11 2 3 17.66 2.48 -11 -2 3 16.70 2.41 -11 -2 3 18.11 2.19 -11 2 2 27.01 3.08 -11 2 2 24.83 2.66 -11 -2 2 26.22 3.01 -11 -2 2 24.84 2.61 -11 -2 2 26.11 2.55 -11 2 1 8.73 1.88 -11 2 1 10.29 1.92 -11 -2 1 8.98 1.78 -11 2 0 18.84 2.42 -11 2 0 18.84 2.54 -11 -2 0 19.14 2.35 -11 2 -1 1.64 1.15 -11 2 -1 3.29 1.33 -11 -2 -1 3.75 1.32 -11 2 -2 8.81 1.86 -11 2 -2 8.08 1.73 -11 -2 -2 8.65 1.58 -11 2 -3 8.11 1.80 -11 2 -3 7.16 1.59 -11 -2 -3 6.19 1.49 -11 2 -3 4.59 1.84 -11 2 -4 6.20 1.66 -11 -2 -4 8.68 1.67 -11 2 -4 8.84 1.83 -11 -2 -5 5.19 1.29 -11 2 -5 -0.11 1.01 -11 -2 -6 0.29 0.71 -11 3 5 22.65 2.56 -11 -3 5 17.22 2.34 -11 3 4 1.24 0.86 -11 -3 4 4.02 1.43 -11 3 3 1.59 0.83 -11 -3 3 3.49 1.38 -11 3 2 24.80 2.93 -11 3 2 28.74 2.68 -11 -3 2 21.57 2.53 -11 -3 2 21.40 2.41 -11 3 1 -0.38 0.96 -11 3 1 -0.12 0.82 -11 -3 1 1.43 1.20 -11 -3 1 -1.90 0.99 -11 3 0 0.13 0.97 -11 3 0 1.79 1.23 -11 -3 0 1.49 1.06 -11 3 -1 18.59 2.72 -11 3 -1 21.63 2.48 -11 3 -1 21.00 2.68 -11 -3 -1 24.56 2.52 -11 3 -2 33.95 3.27 -11 3 -2 35.12 3.03 -11 -3 -2 38.25 3.05 -11 3 -3 2.96 1.38 -11 -3 -3 1.86 1.05 -11 3 -3 1.49 1.17 -11 -3 -4 33.18 2.74 -11 -3 -5 0.93 0.68 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 1678 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 Br1 Br -0.28560(4) 0.64708(7) 0.77190(3) 0.0339(2) Uani 1 1 d . . Br2 Br 0.98830(5) 0.77830(7) 0.41285(3) 0.0396(2) Uani 1 1 d . . O1 O 0.3394(3) 0.7965(4) 0.58442(17) 0.0245(7) Uani 1 1 d . . C1 C 0.3756(4) 0.6715(5) 0.6170(2) 0.0229(9) Uani 1 1 d . . N1 N 0.2288(4) 0.4838(5) 0.7841(2) 0.0261(8) Uani 1 1 d D . H1 H 0.236(6) 0.428(7) 0.819(3) 0.031 Uiso 1 1 d D U C11 C 0.3332(4) 0.5118(5) 0.7375(3) 0.0245(9) Uani 1 1 d . . H11 H 0.421387 0.473833 0.746171 0.029 Uiso 1 1 calc R U C12 C 0.2929(4) 0.6028(5) 0.6760(3) 0.0237(9) Uani 1 1 d . . C13 C 0.1524(4) 0.6327(5) 0.6855(2) 0.0220(9) Uani 1 1 d . . C14 C 0.0537(4) 0.7156(6) 0.6437(3) 0.0253(9) Uani 1 1 d . . H14 H 0.075320 0.768378 0.597364 0.030 Uiso 1 1 calc R U C15 C -0.0748(4) 0.7198(6) 0.6704(3) 0.0260(9) Uani 1 1 d . . H15 H -0.142077 0.777175 0.643036 0.031 Uiso 1 1 calc R U C16 C -0.1052(4) 0.6389(6) 0.7380(3) 0.0254(10) Uani 1 1 d . . C17 C -0.0142(5) 0.5549(6) 0.7807(3) 0.0279(10) Uani 1 1 d . . H17 H -0.037970 0.500031 0.826090 0.033 Uiso 1 1 calc R U C18 C 0.1154(4) 0.5545(5) 0.7537(3) 0.0245(9) Uani 1 1 d . . N2 N 0.6575(4) 0.4130(5) 0.5739(2) 0.0258(8) Uani 1 1 d D . H2 H 0.694(6) 0.332(6) 0.573(4) 0.031 Uiso 1 1 d D U C21 C 0.5378(4) 0.4398(5) 0.6059(3) 0.0242(9) Uani 1 1 d . . H21 H 0.486256 0.361643 0.631383 0.029 Uiso 1 1 calc R U C22 C 0.5016(4) 0.5974(6) 0.5963(2) 0.0227(9) Uani 1 1 d . . C23 C 0.6067(4) 0.6713(5) 0.5539(2) 0.0223(9) Uani 1 1 d . . C24 C 0.6302(4) 0.8266(6) 0.5263(3) 0.0260(9) Uani 1 1 d . . H24 H 0.568162 0.909843 0.535229 0.031 Uiso 1 1 calc R U C25 C 0.7449(5) 0.8558(6) 0.4859(3) 0.0280(10) Uani 1 1 d . . H25 H 0.763422 0.960182 0.467818 0.034 Uiso 1 1 calc R U C26 C 0.8338(4) 0.7308(6) 0.4718(3) 0.0291(10) Uani 1 1 d . . C27 C 0.8170(4) 0.5777(6) 0.4978(2) 0.0261(9) Uani 1 1 d . . H27 H 0.879113 0.495221 0.487630 0.031 Uiso 1 1 calc R U C28 C 0.7019(4) 0.5517(6) 0.5404(2) 0.0249(9) 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 Br1 0.0227(3) 0.0437(4) 0.0355(3) -0.0063(2) 0.00574(19) -0.00286(19) Br2 0.0293(3) 0.0504(4) 0.0394(3) 0.0170(2) 0.0121(2) 0.0076(2) O1 0.0260(15) 0.0197(16) 0.0280(16) 0.0015(13) 0.0041(12) 0.0018(12) C1 0.026(2) 0.024(2) 0.020(2) -0.0025(17) 0.0011(16) -0.0017(17) N1 0.0265(19) 0.022(2) 0.0300(19) 0.0064(16) 0.0046(16) -0.0012(15) C11 0.024(2) 0.020(2) 0.029(2) -0.0003(18) 0.0019(17) 0.0011(17) C12 0.028(2) 0.016(2) 0.027(2) -0.0030(17) -0.0006(17) -0.0033(17) C13 0.026(2) 0.016(2) 0.024(2) -0.0029(17) 0.0021(17) -0.0015(16) C14 0.028(2) 0.022(2) 0.026(2) -0.0043(18) -0.0041(18) 0.0006(17) C15 0.023(2) 0.022(2) 0.032(2) -0.0043(19) -0.0020(18) 0.0003(17) C16 0.020(2) 0.030(3) 0.027(2) -0.0100(18) 0.0075(17) -0.0032(17) C17 0.032(2) 0.024(2) 0.028(2) -0.0032(18) 0.0043(18) -0.0044(18) C18 0.026(2) 0.020(2) 0.027(2) -0.0033(18) -0.0018(17) 0.0019(17) N2 0.0260(19) 0.020(2) 0.0313(19) 0.0001(16) -0.0002(15) 0.0048(15) C21 0.023(2) 0.020(2) 0.029(2) -0.0011(18) 0.0004(17) -0.0015(17) C22 0.024(2) 0.022(2) 0.0221(19) -0.0016(17) -0.0016(16) 0.0017(17) C23 0.023(2) 0.024(2) 0.021(2) -0.0012(17) -0.0005(16) 0.0008(17) C24 0.026(2) 0.025(2) 0.027(2) 0.0022(18) -0.0003(17) 0.0042(18) C25 0.030(2) 0.026(2) 0.028(2) 0.0058(19) 0.0064(18) 0.0034(18) C26 0.021(2) 0.040(3) 0.026(2) 0.005(2) 0.0058(17) 0.0007(19) C27 0.024(2) 0.032(3) 0.023(2) -0.0040(19) -0.0001(16) 0.0072(18) C28 0.025(2) 0.023(2) 0.026(2) -0.0027(18) -0.0015(17) 0.0006(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 '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 O1 C1 C12 119.5(4) O1 C1 C22 119.6(4) C12 C1 C22 120.9(4) C11 N1 C18 109.6(4) C11 N1 H1 121(4) C18 N1 H1 129(4) N1 C11 C12 110.1(4) N1 C11 H11 124.9 C12 C11 H11 124.9 C11 C12 C13 106.4(4) C11 C12 C1 127.6(4) C13 C12 C1 125.7(4) C14 C13 C18 118.2(4) C14 C13 C12 135.0(4) C18 C13 C12 106.8(4) C15 C14 C13 119.6(4) C15 C14 H14 120.2 C13 C14 H14 120.2 C14 C15 C16 119.3(4) C14 C15 H15 120.3 C16 C15 H15 120.3 C17 C16 C15 123.8(4) C17 C16 Br1 118.6(3) C15 C16 Br1 117.6(3) C16 C17 C18 116.0(4) C16 C17 H17 122.0 C18 C17 H17 122.0 N1 C18 C17 129.9(4) N1 C18 C13 107.1(4) C17 C18 C13 123.0(4) C21 N2 C28 109.3(4) C21 N2 H2 126(5) C28 N2 H2 125(5) N2 C21 C22 110.0(4) N2 C21 H21 125.0 C22 C21 H21 125.0 C21 C22 C23 106.4(4) C21 C22 C1 127.2(4) C23 C22 C1 126.1(4) C28 C23 C24 118.9(4) C28 C23 C22 106.5(4) C24 C23 C22 134.6(4) C25 C24 C23 118.9(4) C25 C24 H24 120.5 C23 C24 H24 120.5 C24 C25 C26 119.7(4) C24 C25 H25 120.2 C26 C25 H25 120.2 C27 C26 C25 124.0(4) C27 C26 Br2 118.5(4) C25 C26 Br2 117.5(4) C26 C27 C28 115.3(4) C26 C27 H27 122.3 C28 C27 H27 122.3 N2 C28 C27 129.2(4) N2 C28 C23 107.7(4) C27 C28 C23 123.1(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C16 1.915(4) Br2 C26 1.917(4) O1 C1 1.243(6) C1 C12 1.452(6) C1 C22 1.461(6) N1 C11 1.358(6) N1 C18 1.381(6) N1 H1 0.77(5) C11 C12 1.371(7) C11 H11 0.9500 C12 C13 1.444(6) C13 C14 1.404(6) C13 C18 1.413(6) C14 C15 1.379(7) C14 H14 0.9500 C15 C16 1.400(7) C15 H15 0.9500 C16 C17 1.363(7) C17 C18 1.390(7) C17 H17 0.9500 N2 C21 1.352(6) N2 C28 1.379(6) N2 H2 0.77(5) C21 C22 1.380(7) C21 H21 0.9500 C22 C23 1.438(6) C23 C28 1.408(7) C23 C24 1.411(7) C24 C25 1.381(7) C24 H24 0.9500 C25 C26 1.402(7) C25 H25 0.9500 C26 C27 1.372(7) C27 C28 1.402(7) C27 H27 0.9500 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1 O1 0.77(5) 2.16(5) 2.871(5) 153(6) 2_546 yes C25 H25 O1 0.95 2.45 3.269(6) 143.7 3_676 yes 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 C18 N1 C11 C12 0.8(5) N1 C11 C12 C13 -0.2(5) N1 C11 C12 C1 173.6(4) O1 C1 C12 C11 -151.4(5) C22 C1 C12 C11 27.5(7) O1 C1 C12 C13 21.2(7) C22 C1 C12 C13 -159.8(4) C11 C12 C13 C14 -179.9(5) C1 C12 C13 C14 6.2(8) C11 C12 C13 C18 -0.5(5) C1 C12 C13 C18 -174.5(4) C18 C13 C14 C15 0.6(6) C12 C13 C14 C15 179.9(5) C13 C14 C15 C16 -1.2(7) C14 C15 C16 C17 0.4(7) C14 C15 C16 Br1 -179.4(3) C15 C16 C17 C18 0.8(7) Br1 C16 C17 C18 -179.4(3) C11 N1 C18 C17 178.7(5) C11 N1 C18 C13 -1.1(5) C16 C17 C18 N1 178.9(4) C16 C17 C18 C13 -1.3(7) C14 C13 C18 N1 -179.5(4) C12 C13 C18 N1 1.0(5) C14 C13 C18 C17 0.6(7) C12 C13 C18 C17 -178.8(4) C28 N2 C21 C22 -1.5(5) N2 C21 C22 C23 1.0(5) N2 C21 C22 C1 174.8(4) O1 C1 C22 C21 -157.3(4) C12 C1 C22 C21 23.8(7) O1 C1 C22 C23 15.3(6) C12 C1 C22 C23 -163.6(4) C21 C22 C23 C28 -0.1(5) C1 C22 C23 C28 -174.0(4) C21 C22 C23 C24 -179.8(5) C1 C22 C23 C24 6.3(8) C28 C23 C24 C25 0.9(6) C22 C23 C24 C25 -179.4(5) C23 C24 C25 C26 1.4(7) C24 C25 C26 C27 -2.1(7) C24 C25 C26 Br2 178.2(4) C25 C26 C27 C28 0.3(7) Br2 C26 C27 C28 -179.9(3) C21 N2 C28 C27 -176.7(4) C21 N2 C28 C23 1.4(5) C26 C27 C28 N2 180.0(4) C26 C27 C28 C23 2.2(6) C24 C23 C28 N2 179.0(4) C22 C23 C28 N2 -0.8(5) C24 C23 C28 C27 -2.8(6) C22 C23 C28 C27 177.4(4)