#------------------------------------------------------------------------------ #$Date: 2018-01-13 08:33:12 +0200 (Sat, 13 Jan 2018) $ #$Revision: 205183 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/86/1548675.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_1548675 loop_ _publ_author_name 'Noland, Wayland E.' 'Tritch, Kenneth J.' _publ_section_title ; 3,5-Dibromobenzonitrile ; _journal_coeditor_code SJ4154 _journal_issue 1 _journal_name_full IUCrData _journal_page_first x180059 _journal_paper_doi 10.1107/S2414314618000597 _journal_volume 3 _journal_year 2018 _chemical_formula_iupac 'C7 H3 Br2 N' _chemical_formula_moiety 'C7 H3 Br2 N' _chemical_formula_sum 'C7 H3 Br2 N' _chemical_formula_weight 260.92 _chemical_melting_point 367 _chemical_name_common I _chemical_name_systematic 3,5-Dibromobenzonitrile _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 97.440(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 4.0047(2) _cell_length_b 13.2585(8) _cell_length_c 7.3356(4) _cell_measurement_reflns_used 2765 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 36.36 _cell_measurement_theta_min 2.80 _cell_volume 386.21(4) _computing_cell_refinement ; SAINT (Bruker, 2012) ; _computing_data_collection ; APEX3 (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2012) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2008) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker AXS VENTURE PHOTON-II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 8873 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 36.365 _diffrn_reflns_theta_min 2.800 _exptl_absorpt_coefficient_mu 10.410 _exptl_absorpt_correction_T_max 0.625 _exptl_absorpt_correction_T_min 0.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.244 _exptl_crystal_description needle _exptl_crystal_F_000 244 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.976 _refine_diff_density_min -0.493 _refine_ls_extinction_coef 0.0102(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2014 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 53 _refine_ls_number_reflns 1945 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0244 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+0.2462P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.0580 _reflns_number_gt 1696 _reflns_number_total 1945 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file sj4154sup1.cif _cod_data_source_block I _cod_database_code 1548675 _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 0.231 _shelx_estimated_absorpt_t_max 0.625 _shelx_hkl_file ; 1 0 0 593.122 25.2075 6 1 0 0 577.039 25.1883 2 -2 0 0 787.001 33.5735 3 -2 0 0 762.786 33.7177 2 -2 0 0 783.099 33.2639 4 -3 0 0 1842.11 80.5192 2 4 0 0 468.900 20.6674 5 -4 0 0 477.578 21.5822 2 -4 0 0 451.913 20.8614 3 5 0 0 27.9833 3.19243 5 -5 0 0 29.4861 3.59425 3 6 0 0 61.8481 5.11046 5 -6 0 0 69.1987 5.65439 3 -1 -1 0 751.265 37.9531 1 1 -1 0 773.043 41.6571 1 -1 1 0 758.344 41.1311 1 1 1 0 722.424 37.8871 1 -2 -1 0 152.779 7.27428 6 -2 -1 0 153.636 7.06302 3 -2 -1 0 154.082 6.67585 4 -2 1 0 152.284 7.08984 3 -2 1 0 161.208 7.31129 2 -2 1 0 157.593 6.81434 4 -3 -1 0 13.0255 1.77695 3 3 -1 0 11.2345 1.47174 5 3 1 0 15.2198 1.66141 5 -3 1 0 16.9503 1.95358 3 -3 1 0 10.6442 0.96594 4 -3 1 0 16.6079 2.21704 2 -4 -1 0 73.4167 4.47070 3 4 -1 0 69.4672 4.19296 5 -4 1 0 72.9489 4.50967 3 -4 1 0 78.3695 5.19017 2 4 1 0 71.2924 4.21710 5 -5 -1 0 11.9822 3.21687 3 5 -1 0 9.91544 2.75223 5 5 1 0 12.9926 2.63949 5 -5 1 0 15.0600 3.28219 3 6 -1 0 2.56341 3.14954 5 -6 -1 0 2.79540 3.37471 3 6 1 0 6.74422 2.84257 5 -6 1 0 4.25212 3.27826 3 0 -2 0 1106.53 51.0467 1 0 2 0 1115.03 51.1002 1 1 -2 0 2242.84 104.411 1 -1 -2 0 2170.39 96.4085 1 -1 2 0 2239.45 103.832 1 1 2 0 1995.04 96.1420 1 -2 -2 0 170.202 7.80950 3 -2 -2 0 171.251 8.04971 6 2 2 0 176.836 7.45327 4 -2 2 0 170.657 7.59954 4 -2 2 0 174.262 8.05562 2 -3 -2 0 1167.70 50.8892 3 3 -2 0 1200.21 50.7440 5 3 2 0 1178.40 50.7673 5 -3 2 0 1186.35 51.2391 2 -3 2 0 1149.44 50.5150 4 -3 2 0 1190.62 50.9477 3 -4 -2 0 365.485 16.8473 3 4 -2 0 377.284 16.6805 5 4 2 0 385.085 16.6929 5 -4 2 0 353.797 16.0153 4 -4 2 0 386.091 17.4410 2 -4 2 0 363.636 16.8873 3 -5 -2 0 1.38826 2.58539 3 5 -2 0 -1.6497 2.20801 5 -5 2 0 2.26381 2.70357 3 5 2 0 1.52087 2.24010 5 -5 2 0 -0.6838 2.88734 2 6 -2 0 114.661 6.85523 5 -6 -2 0 117.720 7.37640 3 6 2 0 115.077 7.06687 5 -6 2 0 103.976 7.21433 3 0 -3 0 0.21079 0.38681 2 0 3 0 1.28539 0.35676 6 0 3 0 -0.5845 0.41671 3 0 3 0 2.68761 0.48626 2 -1 -3 0 1774.21 78.1259 1 1 -3 0 1758.44 88.6423 1 -1 3 0 1747.42 88.0535 1 -2 -3 0 649.378 28.0233 3 -2 -3 0 660.166 28.2875 6 2 3 0 650.267 27.7250 4 -2 3 0 636.700 27.8635 4 -2 3 0 640.584 28.2813 2 3 -3 0 27.7393 2.10442 5 -3 -3 0 31.3061 3.07568 6 -3 -3 0 33.5328 2.40802 3 -3 3 0 34.4945 3.07029 2 -3 3 0 30.0134 1.82086 4 3 3 0 27.7133 2.18847 5 -3 3 0 29.7645 2.45723 3 4 -3 0 88.8354 4.80285 5 -4 -3 0 92.5269 5.13848 3 4 3 0 91.7256 4.88421 5 -4 3 0 89.2732 5.88902 2 -4 3 0 83.7431 4.28764 4 -4 3 0 86.8109 5.16249 3 -5 -3 0 135.862 7.57091 3 5 -3 0 132.906 7.17495 5 5 3 0 131.998 7.23110 5 -5 3 0 133.456 7.62489 3 -5 3 0 147.133 8.59064 2 6 -3 0 10.7171 3.48040 5 -6 -3 0 9.76652 3.94784 3 -6 3 0 6.36770 3.49932 3 6 3 0 11.7667 3.05273 5 0 -4 0 2537.37 118.904 1 0 4 0 2707.65 119.589 1 1 -4 0 427.975 18.5454 5 -1 -4 0 437.352 18.8306 6 -1 -4 0 445.949 18.7023 3 1 -4 0 433.883 18.8259 2 1 4 0 435.040 18.8003 6 1 4 0 426.058 18.6911 3 -1 4 0 419.684 18.8682 2 -2 -4 0 91.7592 4.68029 6 2 -4 0 87.6298 4.20071 5 -2 -4 0 97.2758 4.40471 3 -2 4 0 90.4739 4.75094 2 -2 4 0 86.6359 4.19678 4 2 4 0 88.6083 4.05806 4 3 -4 0 640.636 27.7893 5 -3 -4 0 636.554 27.9701 3 -3 -4 0 625.180 28.3533 6 -3 4 0 648.994 28.4390 2 3 4 0 649.267 27.8707 5 4 -4 0 135.510 7.13961 5 -4 -4 0 152.098 7.54628 3 -4 4 0 142.371 7.48689 3 4 4 0 144.605 7.16356 5 -4 4 0 148.971 8.19416 2 5 -4 0 1.75999 2.40443 5 -5 -4 0 5.61592 3.06418 3 -5 4 0 3.62823 3.07626 2 5 4 0 0.65669 2.44824 5 -5 4 0 5.36538 4.89076 3 6 -4 0 51.8410 4.87017 5 -6 -4 0 50.8161 5.26338 3 -6 4 0 55.8167 5.22527 3 6 4 0 48.0454 4.61541 5 0 -5 0 0.27030 0.62746 2 0 -5 0 0.84703 0.42273 6 0 5 0 0.15186 0.54710 6 0 5 0 0.83444 0.66565 3 0 5 0 1.70775 0.62646 2 1 5 0 1025.10 43.4637 6 1 5 0 995.610 43.3630 3 2 -5 0 2757.08 143.138 1 2 5 0 2858.74 122.316 1 -2 5 0 2647.86 140.610 1 2 5 0 2693.55 121.528 1 3 -5 0 93.2007 4.85087 5 -3 -5 0 99.0352 5.60311 6 -3 -5 0 102.400 5.11282 3 -3 5 0 103.049 5.79278 2 3 5 0 93.8632 4.42954 4 3 5 0 103.999 4.96295 5 -4 -5 0 331.047 15.1668 3 4 -5 0 325.137 14.8995 5 4 5 0 338.849 14.9862 5 -4 5 0 330.364 15.8861 2 -4 5 0 325.862 15.2828 3 5 -5 0 299.631 14.0083 5 -5 5 0 295.664 15.3453 2 -5 5 0 311.123 15.1234 3 -6 -5 0 38.7814 4.91314 3 6 -5 0 48.7068 4.89386 5 6 5 0 50.2848 4.66912 5 -6 5 0 51.5082 5.35700 3 -6 5 0 56.8011 6.78069 2 0 -6 0 50.8757 2.47354 6 0 -6 0 50.1806 2.78249 2 0 6 0 54.7336 2.81564 2 0 6 0 49.2484 2.66537 3 1 -6 0 33.2608 1.55264 5 -1 -6 0 34.4638 2.00922 3 -1 -6 0 33.0187 2.12054 6 1 6 0 34.2020 2.01914 6 1 6 0 28.3646 2.17552 2 -1 6 0 33.1678 2.29668 2 -2 -6 0 45.0564 2.56543 3 -2 -6 0 43.9051 3.00952 6 2 6 0 41.5994 2.37969 5 2 6 0 41.3018 2.26008 4 -3 -6 0 8.37323 1.71473 3 3 -6 0 6.21429 1.34931 5 -3 -6 0 6.48945 2.02991 6 -3 6 0 9.00237 2.28433 2 3 6 0 6.99476 1.58467 5 3 6 0 4.81394 0.81514 4 -4 -6 0 9.37448 2.38706 3 4 -6 0 9.63263 2.03705 5 4 6 0 10.4294 2.05266 5 -4 6 0 8.10780 2.51576 3 -4 6 0 9.05258 2.90591 2 -5 -6 0 7.96295 3.38802 3 5 -6 0 4.97664 2.47770 5 5 6 0 6.63931 2.67717 5 -5 6 0 0.55884 2.87298 3 -6 -6 0 -2.0650 3.49568 3 6 -6 0 2.08002 3.11584 5 -6 6 0 -0.3213 4.33005 2 -6 6 0 -0.6301 3.44504 3 6 6 0 0.63948 2.76089 5 0 -7 0 0.76822 0.57640 6 0 7 0 1.61761 0.87976 2 1 -7 0 2592.20 131.834 1 -1 7 0 2617.77 132.069 1 -2 7 0 1153.85 51.9364 2 2 7 0 1177.02 51.3809 5 2 7 0 1259.91 51.5536 4 3 -7 0 35.7334 2.54786 5 -3 -7 0 41.3954 2.96971 3 3 7 0 39.6317 2.77870 5 -3 7 0 42.6420 3.85490 2 3 7 0 36.6382 2.16260 4 4 -7 0 195.830 9.32120 5 -4 -7 0 197.056 9.70181 3 4 7 0 198.375 9.45628 5 -4 7 0 195.436 9.88521 3 -4 7 0 203.825 10.7177 2 -5 -7 0 224.338 11.5315 3 5 -7 0 228.959 10.8104 5 -5 7 0 209.575 11.4504 3 5 7 0 231.594 11.0000 5 -5 7 0 233.943 12.6360 2 6 -7 0 10.9489 3.29974 5 -6 7 0 13.4676 4.68063 3 -6 7 0 17.7735 7.75384 2 0 -8 0 40.7510 2.21809 6 0 8 0 42.3668 2.72325 2 -1 -8 0 150.789 6.89155 3 1 -8 0 136.403 6.52125 6 1 -8 0 146.199 6.22013 5 -1 -8 0 150.251 6.84684 6 1 -8 0 152.228 6.23557 5 1 8 0 145.154 6.39021 5 -1 8 0 136.106 7.00474 2 1 8 0 140.100 6.89092 2 -2 -8 0 23.4521 2.29115 3 -2 -8 0 20.5064 2.43118 6 2 -8 0 19.8696 1.40985 5 2 8 0 19.4243 1.69740 4 2 8 0 20.6702 1.59992 5 -2 8 0 20.0741 2.50425 2 -3 -8 0 63.1536 4.63361 6 -3 -8 0 65.9017 3.91914 3 3 -8 0 62.7610 3.63292 5 -3 8 0 62.5029 4.58661 2 3 8 0 61.6900 3.89375 4 3 8 0 61.7214 3.52771 5 -4 -8 0 33.5616 3.41083 3 4 -8 0 27.4470 2.71225 5 4 8 0 27.8630 2.75884 5 -4 8 0 22.1860 3.65699 2 -5 -8 0 2.35853 3.05202 3 5 -8 0 1.48992 2.30033 5 5 8 0 1.28993 2.27225 5 -5 8 0 -1.4913 3.41957 3 -5 8 0 -1.2383 3.44574 2 6 -8 0 4.18698 3.13879 5 -6 -8 0 7.56813 4.08511 3 -6 8 0 8.14086 5.14663 2 6 8 0 7.62201 3.36214 5 -6 8 0 5.54660 3.78022 3 0 -9 0 0.35613 0.74252 6 0 9 0 -0.4424 1.19495 2 1 -9 0 1093.09 47.4822 6 -1 -9 0 1103.99 47.8932 3 -1 -9 0 1097.72 47.7812 6 1 9 0 1119.81 47.8687 2 1 9 0 1103.72 47.3761 5 -1 9 0 1125.08 48.0854 2 -2 -9 0 1007.35 43.3952 6 2 -9 0 1026.72 42.6974 5 -2 -9 0 1037.33 43.1634 3 -2 9 0 983.855 43.5974 2 2 9 0 1018.48 42.8522 5 2 9 0 903.165 43.2238 2 -3 -9 0 40.4473 3.99800 6 -3 -9 0 46.7953 3.64463 3 -3 9 0 45.9873 4.04180 2 3 9 0 41.8903 2.93821 5 3 9 0 41.9258 2.59824 4 -4 -9 0 218.293 10.9242 3 4 -9 0 218.658 10.2574 5 4 9 0 226.289 10.5559 5 -4 9 0 223.591 11.9677 2 -5 -9 0 143.862 8.27324 3 5 -9 0 144.655 7.62695 5 -5 9 0 137.310 8.47604 3 5 9 0 153.282 7.88298 5 -5 9 0 145.070 9.81902 2 -6 -9 0 16.8333 4.80102 3 6 -9 0 5.89376 3.27279 5 6 9 0 9.90932 3.44201 5 -6 9 0 6.39901 3.91606 3 -6 9 0 14.1054 5.13639 2 0 -10 0 2008.28 102.911 1 -1 -10 0 139.237 6.69525 6 1 -10 0 135.410 6.27120 6 1 10 0 138.826 6.13198 5 -1 10 0 140.315 7.06475 2 1 10 0 139.908 6.92748 2 -2 -10 0 143.416 7.26770 6 -2 -10 0 149.508 7.17391 3 2 -10 0 142.100 6.29313 5 2 10 0 136.675 7.10158 2 2 10 0 136.929 6.50457 5 -3 -10 0 354.116 15.9094 3 -3 -10 0 348.742 16.3353 6 3 -10 0 351.149 15.2876 5 3 10 0 345.845 15.3772 4 3 10 0 342.017 15.6913 5 -3 10 0 343.328 16.5665 2 4 -10 0 116.514 5.97764 5 -4 -10 0 121.418 6.83989 3 -4 10 0 122.333 8.16958 2 4 10 0 117.422 6.34280 5 5 -10 0 10.5793 2.58071 5 -5 -10 0 16.0513 3.79973 3 -5 10 0 9.63257 3.68675 3 5 10 0 9.88708 2.95331 5 -5 10 0 16.6959 4.90266 2 0 11 0 2.08479 1.65090 2 -1 -11 0 126.300 6.26411 6 1 -11 0 124.250 5.76052 6 1 11 0 129.062 5.57364 5 1 11 0 130.764 6.52218 2 1 11 0 117.729 5.61275 5 -1 11 0 126.555 6.79813 2 2 -11 0 280.724 12.0962 5 2 -11 0 286.976 12.1401 5 -2 -11 0 273.749 12.9419 3 -2 -11 0 277.964 13.1452 6 2 11 0 280.808 12.3844 5 2 11 0 286.300 13.0235 2 -2 11 0 274.513 13.4343 2 -3 -11 0 12.1728 2.82631 6 3 -11 0 10.9776 1.39950 5 -3 -11 0 13.4013 2.68295 3 -3 11 0 8.12909 3.19633 2 3 11 0 9.38035 1.69026 4 3 11 0 8.86858 2.48609 2 3 11 0 8.77273 1.92307 5 4 -11 0 13.5981 2.04675 5 -4 -11 0 19.1143 3.69275 3 4 11 0 16.8442 2.45643 5 -5 -11 0 56.0543 5.53265 3 5 -11 0 59.2645 4.41049 5 5 11 0 64.3716 4.51466 5 -5 11 0 56.7901 5.66589 3 -5 11 0 62.7560 7.35174 2 0 -12 0 523.893 22.9362 6 0 12 0 528.154 23.5243 2 -1 -12 0 506.440 23.6715 6 1 -12 0 532.157 22.9306 6 1 12 0 544.346 23.5957 2 1 12 0 505.570 22.7475 5 1 12 0 542.957 22.7395 5 -1 12 0 548.589 24.1972 2 2 -12 0 55.9608 3.51859 6 -2 -12 0 61.7330 4.25941 6 -2 -12 0 58.2714 4.57919 3 -2 12 0 58.4704 4.60081 2 2 12 0 58.5766 4.18999 2 2 12 0 57.5546 3.09684 5 -3 -12 0 476.382 21.0267 3 3 -12 0 479.113 20.1208 5 -3 -12 0 449.551 21.2793 6 3 12 0 471.582 20.4026 5 3 12 0 447.489 20.9457 2 3 12 0 454.804 20.4553 4 -3 12 0 459.409 21.7511 2 -4 12 0 176.611 10.2488 2 4 12 0 155.284 7.84992 5 4 12 0 143.221 8.63214 2 5 -12 0 -2.9765 2.20262 5 -5 -12 0 4.13158 4.23021 3 5 12 0 0.89909 2.70973 5 -5 12 0 -0.6928 4.12745 3 -5 12 0 -0.5124 4.29005 2 0 -13 0 0.66659 1.17266 6 0 13 0 0.17279 2.08766 2 1 -13 0 17.8054 1.62909 6 -1 -13 0 20.0716 2.26795 6 1 13 0 20.2509 2.70098 2 -1 13 0 25.2518 3.31845 2 1 13 0 20.2573 1.09606 5 1 13 0 16.9454 1.05606 5 2 -13 0 7.78554 1.20688 6 -2 -13 0 7.37109 2.78652 3 2 -13 0 11.9026 1.31709 6 2 13 0 10.5539 2.02307 4 2 13 0 11.2995 1.34236 5 2 13 0 9.32863 2.56810 2 -2 13 0 9.87226 2.81346 2 -3 -13 0 1.76115 2.87058 3 -3 -13 0 0.02481 2.56240 6 3 13 0 3.06561 2.57592 2 -3 13 0 3.00448 3.25459 2 3 13 0 -1.0945 1.72580 4 3 13 0 2.24896 1.49784 5 -4 -13 0 12.9167 3.59566 3 4 -13 0 7.39465 1.85736 5 4 13 0 9.60972 3.08891 2 4 13 0 9.79814 2.24825 5 -4 13 0 7.30257 4.18969 2 -5 -13 0 -0.4062 4.29755 3 -5 13 0 -2.1235 4.29917 3 -5 13 0 -0.2350 5.70979 2 5 13 0 0.23338 2.67388 5 0 -14 0 1136.95 49.3213 6 0 14 0 1151.48 50.0433 2 1 -14 0 225.091 9.72059 6 -1 -14 0 215.167 10.3028 6 1 14 0 213.496 10.7434 2 -1 14 0 214.806 11.1325 2 2 -14 0 75.6441 3.70592 6 -2 -14 0 73.1364 5.20453 6 2 14 0 75.3754 3.81634 5 -2 14 0 73.0118 6.00787 2 2 14 0 82.7903 5.35030 2 2 14 0 74.3816 4.67313 4 -3 -14 0 416.043 19.1709 6 3 -14 0 410.993 17.8892 6 -3 -14 0 378.816 18.8299 3 3 14 0 392.003 18.2858 4 3 14 0 417.835 18.0688 5 -3 14 0 414.984 22.0603 2 3 14 0 422.331 18.8092 2 -4 -14 0 105.407 7.17099 3 4 14 0 110.265 7.03330 2 4 14 0 105.257 5.93414 5 -4 14 0 115.484 8.97547 2 -5 -14 0 11.2242 5.43817 3 -5 14 0 -0.1937 4.81263 2 5 14 0 0.23555 2.63416 5 -5 14 0 1.97247 4.63439 3 0 -15 0 -0.0047 1.28549 6 0 15 0 -0.2080 2.55725 2 1 -15 0 30.6785 2.04172 6 -1 -15 0 28.9563 3.03123 6 -1 15 0 37.9902 4.18224 2 1 15 0 27.9032 3.51475 2 -2 -15 0 127.909 7.19321 6 2 -15 0 133.799 6.10250 6 -2 15 0 115.230 8.04676 2 2 15 0 122.337 6.83799 4 2 15 0 129.524 7.25336 2 2 15 0 126.438 5.85760 5 -3 -15 0 3.86741 3.47806 3 -3 -15 0 7.93996 3.10174 6 3 15 0 3.33088 1.70337 5 3 15 0 3.50100 2.95063 2 3 15 0 2.10004 2.01456 4 -3 15 0 5.59552 3.82542 2 -4 -15 0 18.2249 4.43002 3 4 15 0 9.87923 3.28113 2 4 15 0 15.0233 2.52328 5 -4 15 0 23.6030 5.55580 2 0 -16 0 422.809 18.5402 6 0 16 0 415.810 19.6106 2 -1 -16 0 100.984 5.76530 6 1 -16 0 101.357 4.77160 6 1 16 0 101.725 6.58794 2 -1 16 0 109.202 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5.03192 4 0 -11 -10 38.5771 6.73841 6 0 -11 10 40.4322 8.08708 4 0 11 10 33.8680 5.01407 4 0 11 -10 32.0624 5.46880 2 1 -11 10 -0.2520 3.75927 4 -1 -11 -10 -1.4704 5.10656 6 1 11 10 3.70256 4.05301 4 -1 11 -10 5.76806 4.93272 2 2 -12 -10 81.8791 6.06223 5 -2 12 10 97.9617 6.80997 4 2 12 -10 83.8252 5.60816 5 1 -12 -10 2.69244 4.49211 6 1 12 -10 -3.6531 2.67091 5 -1 12 10 3.56915 3.78732 4 1 12 -10 0.70785 5.72134 2 0 -12 -10 41.2942 6.29936 6 0 12 -10 39.7407 9.07517 2 0 12 10 34.0035 5.09295 4 3 0 -11 28.0136 5.26533 5 -3 0 11 15.7239 3.73954 4 2 0 -11 4.55521 3.22128 5 2 0 -11 8.38515 3.79834 6 2 0 -11 3.53307 5.13860 2 -2 0 11 2.19736 3.08678 4 -1 0 11 106.145 7.24047 4 1 0 -11 110.030 7.37686 6 1 0 -11 123.975 6.92631 5 1 0 -11 108.832 6.61647 2 0 0 11 154.236 9.02768 4 0 0 -11 149.631 9.17520 6 0 0 -11 158.781 8.49325 5 -1 0 -11 4.80205 3.68988 6 1 0 11 4.52706 4.07565 4 -2 0 -11 51.5918 6.45308 6 2 0 11 37.9154 5.34434 4 3 -1 -11 10.5764 3.16178 5 -3 -1 11 11.3834 3.62375 4 -3 1 11 3.28879 3.20401 4 3 1 -11 11.5383 3.63382 5 2 -1 -11 11.7388 3.30241 2 2 -1 -11 8.79897 3.04053 5 -2 -1 11 10.9096 3.80028 4 2 -1 -11 5.99803 3.77959 6 2 1 -11 9.05920 3.42282 2 2 1 -11 11.7926 3.72612 6 -2 1 11 5.17255 3.63433 4 2 1 -11 10.7390 3.05668 5 -1 -1 11 29.8566 4.55670 4 1 -1 -11 20.4917 3.33056 5 1 -1 -11 22.7920 4.07228 6 1 1 -11 27.3683 3.68168 5 1 1 -11 20.9909 3.23068 2 -1 1 11 24.2937 4.43591 4 1 1 -11 24.9361 3.94898 6 0 -1 -11 2.99678 2.97869 5 0 -1 -11 6.11078 3.67035 6 0 -1 11 2.85892 3.80662 4 0 1 11 5.78004 3.87078 4 0 1 -11 0.90014 3.37225 6 0 1 -11 5.90599 3.44703 5 -1 -1 -11 3.27369 3.87487 6 1 -1 11 2.24447 3.78232 4 -1 1 -11 6.01052 3.49309 6 1 1 11 4.91295 3.56047 4 2 -1 11 4.90269 4.21920 4 2 1 11 4.12440 4.04853 4 -2 1 -11 7.14367 3.85981 6 3 -2 -11 34.7138 4.63731 5 -3 -2 11 26.3213 4.03330 4 -3 2 11 31.9577 4.26966 4 3 2 -11 32.7283 3.88993 5 2 -2 -11 41.1971 5.29579 6 2 -2 -11 46.7105 4.49541 5 -2 -2 11 43.7824 4.90590 4 2 2 -11 35.5908 3.99736 5 -2 2 11 40.5642 4.77584 4 2 2 -11 32.3159 4.52111 6 2 2 -11 43.6203 5.32585 2 1 -2 -11 167.168 9.56391 6 1 -2 -11 171.540 8.76881 5 -1 -2 11 155.643 9.37570 4 1 2 -11 144.233 9.01581 6 1 2 -11 165.570 8.64758 5 1 2 -11 160.798 8.67572 2 -1 2 11 145.855 9.26017 4 0 -2 -11 33.3595 4.84044 6 0 -2 -11 32.4599 4.45172 5 0 -2 11 29.8426 4.46052 4 0 2 -11 31.0992 4.31002 6 0 2 -11 35.2622 4.22677 5 0 2 11 35.4123 4.80675 4 1 -2 11 1.28410 3.65162 4 -1 -2 -11 1.66421 3.98016 6 1 2 11 0.52983 3.42013 4 -1 2 -11 1.60682 3.30059 6 2 -2 11 40.6945 5.45179 4 2 2 11 25.7322 4.79981 4 -2 2 -11 31.0898 4.86611 6 3 -3 -11 29.8094 3.82277 5 -3 -3 11 25.4180 3.97280 4 3 3 -11 30.4816 3.76665 5 -3 3 11 32.1392 4.26754 4 2 -3 -11 104.008 7.71489 6 -2 -3 11 94.4102 6.87342 4 2 -3 -11 95.8136 6.06373 5 2 3 -11 91.1042 6.72218 2 2 3 -11 86.2652 5.97430 5 2 3 -11 83.8870 6.88673 6 -2 3 11 93.3600 6.85996 4 1 -3 -11 -0.9648 2.67206 5 -1 -3 11 -0.1771 3.26200 4 1 -3 -11 1.85392 3.56970 6 -1 3 11 -0.0876 3.25869 4 1 3 -11 2.05802 2.96460 5 1 3 -11 -1.3610 3.11965 2 1 3 -11 0.66472 2.91372 6 0 -3 -11 28.7841 3.95396 5 0 -3 11 34.7259 4.85350 4 0 -3 -11 37.6334 5.16025 6 0 3 -11 33.3028 3.92712 5 0 3 -11 32.3108 4.22226 6 0 3 -11 34.0400 3.94902 2 0 3 11 22.4628 4.45088 4 -1 -3 -11 58.5873 6.73778 6 1 3 11 45.9836 7.33888 4 -1 3 -11 55.5444 5.61960 6 -3 -4 11 46.9194 5.28805 4 3 -4 -11 61.6719 5.02810 5 3 -4 -11 60.2937 6.89989 6 -3 4 11 56.5548 5.60965 4 3 4 -11 60.4923 6.40969 2 3 4 -11 61.0339 5.32122 5 2 -4 -11 2.48947 3.75069 6 -2 -4 11 2.55327 3.51664 4 2 -4 -11 7.25226 3.01290 5 2 4 -11 5.23313 3.21329 5 -2 4 11 2.21195 3.54781 4 2 4 -11 5.88823 3.26603 6 2 4 -11 1.71114 3.66833 2 -1 -4 11 63.1863 6.31016 4 1 -4 -11 76.0216 5.28541 5 1 -4 -11 70.6255 6.80663 6 1 4 -11 70.1626 5.28424 5 1 4 -11 71.1954 5.78155 2 1 4 -11 62.3172 5.52659 6 -1 4 11 63.7136 5.75223 4 0 -4 -11 18.9381 4.35601 6 0 -4 -11 18.9077 3.72386 5 0 -4 11 23.9858 4.27244 4 0 4 -11 20.6223 3.60287 6 0 4 11 13.0867 3.82224 4 0 4 -11 24.1752 3.76266 2 0 4 -11 17.0937 3.43638 5 -1 -4 -11 -2.5337 4.01423 6 1 -4 11 -2.3521 6.75332 4 1 4 11 4.14161 5.97233 4 3 -5 -11 111.432 8.68636 6 3 -5 -11 120.682 6.93494 5 -3 -5 11 105.408 7.17141 4 -3 5 11 106.433 7.31802 4 3 5 -11 105.936 6.99413 5 2 -5 -11 120.607 6.94443 5 2 -5 -11 112.094 8.51829 6 -2 5 11 111.231 7.36546 4 2 5 -11 117.157 8.14366 2 2 5 -11 111.170 7.02321 5 2 5 -11 109.423 7.36975 6 1 -5 -11 4.15143 3.88039 6 -1 -5 11 -3.0887 3.69192 4 1 -5 -11 2.21321 2.83443 5 1 5 -11 0.03352 2.61219 5 1 5 -11 -0.5477 2.73426 6 -1 5 11 -3.0970 3.24794 4 1 5 -11 -2.0477 3.26203 2 0 -5 -11 66.5096 7.27082 6 0 -5 -11 69.4986 5.62616 5 0 -5 11 63.4801 6.54960 4 0 5 11 70.7252 6.60385 4 0 5 -11 78.3166 5.82522 5 0 5 -11 82.7851 6.87087 2 1 -5 11 24.7688 4.72306 4 1 5 11 24.1376 4.62775 4 -3 -6 11 -1.2094 3.44437 4 3 -6 -11 0.86665 3.24419 5 3 -6 -11 -2.3837 4.48815 6 3 6 -11 3.33085 4.37493 2 3 6 -11 3.59446 2.79876 5 -2 -6 11 -1.0981 3.59820 4 2 -6 -11 6.10398 5.71565 6 2 -6 -11 4.73815 2.99633 5 2 6 -11 5.38623 4.07665 2 2 6 -11 6.41143 3.12990 6 2 6 -11 4.84355 4.37553 5 -2 6 11 -3.6149 3.52204 4 1 -6 -11 0.11104 3.78068 6 1 -6 -11 2.73006 2.91850 5 -1 -6 11 2.26375 3.80777 4 1 6 -11 -5.8486 2.75935 5 1 6 -11 -2.6821 3.40138 2 1 6 -11 -0.1937 2.78953 6 -1 6 11 -1.9866 3.37518 4 0 -6 -11 14.2433 3.61224 5 0 -6 11 19.3124 4.82129 4 0 -6 -11 15.4606 4.54866 6 0 6 -11 17.8738 4.06853 2 0 6 11 27.3244 6.25719 4 0 6 -11 14.8371 3.54305 5 -1 -6 -11 -0.7587 4.56087 6 1 -6 11 1.28625 3.66045 4 1 6 11 2.53978 3.94038 4 -2 -7 11 115.545 8.12762 4 2 -7 -11 125.030 9.12469 6 2 7 -11 129.332 8.60499 2 2 7 -11 138.049 9.20226 6 1 -7 -11 5.41084 3.35082 5 -1 -7 11 0.84006 3.63425 4 1 7 -11 2.31061 3.55278 2 1 7 -11 1.56577 3.03313 5 0 -7 11 44.8329 8.45334 4 0 -7 -11 51.4399 7.74637 6 0 7 11 34.3914 4.97742 4 0 7 -11 50.7751 6.08865 2 0 7 -11 39.8474 4.16736 5 1 -7 11 110.696 8.31428 4 -1 -7 -11 116.466 9.51358 6 1 7 11 123.823 8.02190 4 2 -8 -11 17.4203 4.81859 5 -2 -8 11 5.61220 5.71563 4 2 -8 -11 22.8608 5.01437 6 -2 8 11 17.7726 4.39512 4 2 8 -11 15.9759 3.66553 5 1 -8 -11 7.05288 4.38134 6 1 -8 -11 12.6279 6.20586 5 1 8 -11 13.0642 4.16975 2 -1 8 11 13.3185 4.38914 4 1 8 -11 12.2633 3.57275 5 0 -8 11 1.80157 4.14961 4 0 -8 -11 0.28699 4.57103 6 0 8 -11 2.27852 4.02575 2 0 8 -11 -3.2570 4.62042 5 0 8 11 1.57512 3.99343 4 1 -9 -11 32.2402 5.21968 6 -1 -9 11 27.5233 4.94358 4 1 -9 -11 34.8665 5.82020 5 -1 9 11 22.7870 4.75218 4 1 9 -11 38.4609 7.70643 2 0 -9 11 18.3821 4.63113 4 0 -9 -11 24.9176 5.38603 6 0 9 -11 25.2574 4.77967 2 0 9 11 18.0830 4.21478 4 2 0 -12 60.8803 6.79618 6 2 0 -12 73.8935 5.81938 5 -2 0 12 57.0794 6.00473 4 1 0 -12 0.60603 2.92074 5 1 0 -12 6.27427 4.83186 6 -1 0 12 -0.2811 3.57255 4 0 0 -12 4.96098 4.68589 6 0 0 -12 12.8036 3.85900 5 0 0 12 5.22467 4.01219 4 2 -1 -12 1.58520 3.86444 6 2 -1 -12 3.69556 3.45931 5 -2 -1 12 1.04395 3.79300 4 2 1 -12 0.72918 3.76399 6 2 1 -12 2.65797 2.99104 5 -2 1 12 3.94422 3.83245 4 2 1 -12 3.54532 4.39111 2 -1 -1 12 2.48262 3.93055 4 1 -1 -12 4.77916 3.39951 5 1 1 -12 2.87961 3.52400 6 1 1 -12 7.37313 3.04600 5 -1 1 12 4.45338 4.00284 4 0 -1 -12 7.49187 3.40461 5 0 -1 12 10.5431 3.97477 4 0 1 -12 7.90220 3.80032 5 0 1 -12 12.3947 3.80053 6 0 1 12 11.7846 4.39216 4 -2 -2 12 39.3480 4.91081 4 2 -2 -12 52.6025 6.29288 5 2 2 -12 43.4865 4.42118 5 -2 2 12 33.9532 4.75403 4 1 -2 -12 0.21534 2.93254 5 -1 -2 12 -1.1138 3.94145 4 1 -2 -12 4.78432 4.48535 6 1 2 -12 3.26460 3.33862 6 1 2 -12 -4.1356 2.76119 5 -1 2 12 5.66453 4.09280 4 0 -2 -12 82.2358 7.81295 6 0 -2 -12 82.6111 6.49650 5 0 -2 12 87.5869 7.28721 4 0 2 -12 82.6324 6.64006 6 0 2 -12 84.0809 6.46996 5 0 2 12 84.8201 7.21619 4 1 -3 -12 73.6538 5.75658 5 -1 -3 12 60.1275 6.37119 4 1 -3 -12 68.5339 6.85429 6 1 3 -12 51.1990 5.71198 6 1 3 -12 57.7945 5.01043 5 -1 3 12 67.0668 6.41684 4 0 -3 -12 0.99757 3.99696 6 0 -3 -12 -1.3980 3.14268 5 0 -3 12 7.02647 4.28587 4 0 3 12 4.02387 4.26034 4 0 3 -12 2.25475 3.22407 6 0 3 -12 0.62981 3.53965 5 1 -4 -12 -4.7540 3.74359 6 -1 -4 12 -0.3407 3.81026 4 1 -4 -12 -0.1482 3.29646 5 -1 4 12 -1.0076 3.94727 4 1 4 -12 -4.0010 2.92176 6 1 4 -12 4.37954 3.25697 5 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.3438 _exptl_absorpt_correction_T_min 0.1647 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71075 4.010 13.266 7.344 90.014 97.462 89.982 ) ; _shelx_hkl_checksum 42029 _shelx_res_file ; TITL 17226z in P2(1)/m CELL 0.71073 4.00465 13.25850 7.33559 90.0000 97.4404 90.0000 ZERR 2.000 0.00024 0.00075 0.00044 0.0000 0.0025 0.0000 LATT 1 SYMM -X, 1/2+Y, -Z SFAC C H BR N UNIT 14 6 4 2 TEMP -173.140 SIZE 0.05 0.07 0.20 L.S. 10 ACTA CONF BOND $H LIST 4 FMAP 2 PLAN 5 WGHT 0.020200 0.246200 EXTI 0.010217 FVAR 0.62948 BR3 3 0.846127 0.462593 0.216138 11.00000 0.02244 0.01753 = 0.02213 0.00604 0.00792 -0.00043 N7 4 0.277402 0.250000 0.877459 10.50000 0.02291 0.03936 = 0.01691 0.00000 0.00621 0.00000 C1 1 0.545516 0.250000 0.575139 10.50000 0.01293 0.01810 = 0.01054 0.00000 0.00389 0.00000 C2 1 0.613402 0.341828 0.493868 11.00000 0.01485 0.01583 = 0.01409 -0.00052 0.00359 0.00041 AFIX 43 H2 2 0.566428 0.404053 0.549506 11.00000 -1.20000 AFIX 0 C3 1 0.751203 0.339748 0.329795 11.00000 0.01388 0.01594 = 0.01358 0.00205 0.00351 -0.00013 C4 1 0.822666 0.250000 0.244917 10.50000 0.01512 0.01805 = 0.01233 0.00000 0.00364 0.00000 AFIX 43 H4 2 0.917204 0.250000 0.132635 10.50000 -1.20000 AFIX 0 C7 1 0.399457 0.250000 0.744388 10.50000 0.01666 0.02128 = 0.01470 0.00000 0.00308 0.00000 HKLF 4 REM 17226z in P2(1)/m REM R1 = 0.0244 for 1696 Fo > 4sig(Fo) and 0.0306 for all 1945 data REM 53 parameters refined using 0 restraints END WGHT 0.0201 0.2472 REM Highest difference peak 0.976, deepest hole -0.493, 1-sigma level 0.130 Q1 1 0.3892 0.2500 0.8219 10.50000 0.05 0.98 Q2 1 0.8298 0.4381 0.1392 11.00000 0.05 0.71 Q3 1 0.8039 0.2972 0.2906 11.00000 0.05 0.52 Q4 1 0.5697 0.2937 0.5236 11.00000 0.05 0.52 Q5 1 0.4708 0.2500 0.6498 10.50000 0.05 0.50 ; _shelx_res_checksum 78529 _shelxl_version_number 2014/6 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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 Br Br3 0.84613(4) 0.46259(2) 0.21614(2) 0.02026(6) Uani d 1 N N7 0.2774(5) 0.2500 0.8775(3) 0.0261(4) Uani d 1 C C1 0.5455(5) 0.2500 0.5751(2) 0.0136(3) Uani d 1 C C2 0.6134(3) 0.34183(11) 0.49387(18) 0.0148(2) Uani d 1 H H2 0.5664 0.4041 0.5495 0.018 Uiso calc 1 C C3 0.7512(3) 0.33975(11) 0.32980(18) 0.0143(2) Uani d 1 C C4 0.8227(5) 0.2500 0.2449(3) 0.0150(3) Uani d 1 H H4 0.9172 0.2500 0.1326 0.018 Uiso calc 1 C C7 0.3995(5) 0.2500 0.7444(3) 0.0175(3) Uani d 1 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 Br3 0.02244(8) 0.01753(8) 0.02213(8) -0.00043(5) 0.00792(5) 0.00604(5) N7 0.0229(9) 0.0394(12) 0.0169(8) 0.000 0.0062(7) 0.000 C1 0.0129(7) 0.0181(8) 0.0105(6) 0.000 0.0039(5) 0.000 C2 0.0148(5) 0.0158(6) 0.0141(5) 0.0004(4) 0.0036(4) -0.0005(4) C3 0.0139(5) 0.0159(6) 0.0136(5) -0.0001(4) 0.0035(4) 0.0021(4) C4 0.0151(7) 0.0180(8) 0.0123(7) 0.000 0.0036(6) 0.000 C7 0.0167(8) 0.0213(9) 0.0147(8) 0.000 0.0031(6) 0.000 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' Br Br -0.2901 2.4595 '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' 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 C2 C1 C2 4_565 121.16(16) C2 C1 C7 4_565 119.42(8) C2 C1 C7 . 119.42(8) C3 C2 C1 . 118.28(13) C3 C2 H2 . 120.9 C1 C2 H2 . 120.9 C2 C3 C4 . 122.25(13) C2 C3 Br3 . 119.38(11) C4 C3 Br3 . 118.37(10) C3 C4 C3 4_565 117.78(16) C3 C4 H4 4_565 121.1 C3 C4 H4 . 121.1 N7 C7 C1 . 178.8(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Br3 C3 . 1.8906(13) N7 C7 . 1.147(3) C1 C2 4_565 1.3977(16) C1 C2 . 1.3977(16) C1 C7 . 1.439(3) C2 C3 . 1.3878(18) C2 H2 . 0.9500 C3 C4 . 1.3898(17) C4 C3 4_565 1.3898(17) C4 H4 . 0.9500 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_4 _geom_torsion C2 C1 C2 C3 4_565 . -0.1(3) C7 C1 C2 C3 . . -179.38(17) C1 C2 C3 C4 . . 0.0(2) C1 C2 C3 Br3 . . 180.00(12) C2 C3 C4 C3 . 4_565 0.1(3) Br3 C3 C4 C3 . 4_565 -179.91(9) _cod_database_fobs_code 1548675