#------------------------------------------------------------------------------
#$Date: 2020-12-07 03:01:11 +0200 (Mon, 07 Dec 2020) $
#$Revision: 259635 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022295.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_2022295
loop_
_publ_author_name
'Mason, Helen E.'
'Howard, Judith A. K.'
'Sparkes, Hazel A.'
_publ_section_title
;
(E)-4-Bromo-2-[(phenylimino)methyl]phenol: a new polymorph and
thermochromism
;
_journal_coeditor_code YD3009
_journal_issue 11
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 1001
_journal_page_last 1004
_journal_paper_doi 10.1107/S2053229620011560
_journal_volume 76
_journal_year 2020
_chemical_absolute_configuration ad
_chemical_formula_iupac 'C13 H10 Br N O'
_chemical_formula_moiety 'C13 H10 Br N O'
_chemical_formula_sum 'C13 H10 Br N O'
_chemical_formula_weight 276.13
_chemical_name_systematic
;
(E)-4-Bromo-2-((phenylimino)methyl]phenol
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 29
_space_group_name_Hall 'P 2c -2ac'
_space_group_name_H-M_alt 'P c a 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.2768(3)
_cell_length_b 4.48290(10)
_cell_length_c 19.6694(4)
_cell_measurement_reflns_used 5409
_cell_measurement_temperature 120(2)
_cell_measurement_theta_max 30.6392
_cell_measurement_theta_min 2.6483
_cell_volume 1082.52(4)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_molecular_graphics
;
OLEX (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 120(2)
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0425
_diffrn_reflns_av_unetI/netI 0.0260
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 5
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 13133
_diffrn_reflns_theta_full 26.370
_diffrn_reflns_theta_max 26.370
_diffrn_reflns_theta_min 3.319
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 3.772
_exptl_absorpt_correction_T_max 0.847
_exptl_absorpt_correction_T_min 0.383
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Oxford Diffraction, 2010), based on expressions derived
by
Clark & Reid (1995)]
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.694
_exptl_crystal_description block
_exptl_crystal_F_000 552
_exptl_crystal_size_max 0.4546
_exptl_crystal_size_mid 0.1968
_exptl_crystal_size_min 0.0493
_refine_diff_density_max 0.386
_refine_diff_density_min -0.231
_refine_ls_abs_structure_details
;
Flack x determined using 993 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.006(8)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 149
_refine_ls_number_reflns 2215
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.054
_refine_ls_R_factor_all 0.0236
_refine_ls_R_factor_gt 0.0219
_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^)+(0.0288P)^2^+0.2498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0518
_refine_ls_wR_factor_ref 0.0529
_reflns_number_gt 2133
_reflns_number_total 2215
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yd3009sup1.cif
_cod_data_source_block 1A
_cod_database_code 2022295
_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 0.279
_shelx_estimated_absorpt_t_max 0.836
_shelx_hkl_file
;
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0 0 -22 16074.7 1232.57 10
0 0 -21 801.319 369.142 10
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0 0 -19 729.774 330.731 10
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-14 -3 -3 1109.09 580.844 1
14 3 -3 1161.66 519.828 11
-14 3 -2 10492.0 1113.53 1
14 -3 -2 11148.2 1302.81 9
-14 -3 -2 10310.8 1315.58 1
14 3 -2 10032.8 1232.70 11
14 -3 -1 333.773 385.074 9
-14 3 -1 994.305 443.663 1
-14 -3 -1 817.617 403.782 1
14 3 -1 1740.93 695.726 3
14 3 -1 367.399 417.225 11
14 -3 0 6489.19 1052.04 9
-14 3 0 8020.98 923.668 1
-14 -3 0 8164.28 1162.60 1
14 3 0 7813.84 1132.74 3
14 3 0 8271.26 1133.53 11
14 -3 1 135.643 438.875 9
14 3 1 902.952 461.753 3
-14 -3 1 989.037 534.386 1
-14 3 1 478.938 377.724 5
-14 3 2 9307.51 1218.41 5
-14 -3 2 9196.86 1181.97 1
14 -3 2 10580.3 1314.74 9
14 3 2 12425.5 1389.17 3
-14 3 3 798.090 550.245 5
14 -3 3 1235.16 525.370 9
-14 -3 3 720.460 530.398 1
14 3 3 1915.92 641.617 3
-14 3 4 4942.69 918.721 5
14 3 4 6486.26 991.395 3
14 3 5 1395.43 585.646 3
14 3 6 5960.15 969.842 3
14 3 7 4922.57 876.451 3
14 3 8 3778.37 847.125 3
14 3 9-59.4763 402.677 3
15 0 -14-788.212 753.160 3
15 0 -13-447.304 533.361 3
15 0 -12-617.802 567.213 3
15 0 -11-476.912 598.945 3
-15 0 -10 1004.55 524.303 1
15 0 -10-789.067 677.680 3
-15 0 -9 1261.04 565.814 1
15 0 -9-742.808 680.378 3
-15 0 -8 336.425 390.665 1
15 0 -8-307.031 636.352 3
-15 0 -7 446.558 403.022 1
15 0 -7-354.601 502.434 3
-15 0 -6 685.483 419.516 1
15 0 -6-195.643 455.030 3
15 0 -5-225.014 427.308 3
-15 0 -5 797.138 450.396 1
15 0 -4-703.522 607.912 3
-15 0 -4 245.404 384.623 1
15 0 -3-109.717 438.168 3
-15 0 -3 358.128 372.635 1
15 0 -2 48.2942 409.372 3
-15 0 -2-18.9407 386.454 1
15 0 -1 279.904 381.671 3
-15 0 -1 546.679 407.765 1
-15 0 0 204.580 342.385 1
15 0 0 551.476 516.035 3
-15 0 1 456.341 368.466 1
15 0 1 285.029 419.321 3
-15 0 2-111.754 300.098 1
15 0 2 375.708 451.562 3
-15 0 3-388.550 391.920 1
15 0 3-326.400 405.746 3
-15 0 4-34.0452 385.418 1
15 0 4 120.175 303.413 4
15 0 4-31.8788 345.701 3
-15 0 5-171.474 435.184 1
15 0 5-416.701 359.875 3
15 0 6 338.266 319.938 4
-15 0 6-304.762 356.346 1
15 0 6-51.7626 359.252 3
15 0 7 469.503 432.249 4
15 0 7-566.469 457.629 3
-15 0 7-282.749 392.408 1
-15 0 8-160.238 305.098 1
15 0 8 422.544 428.782 4
15 0 8-437.980 405.996 3
-15 0 9 33.1256 306.806 1
15 0 9-63.5381 332.598 4
15 0 9-298.064 425.972 3
-15 0 9-16.8003 309.878 5
-15 0 10-521.872 322.477 5
15 0 10 14.0135 330.232 4
-15 0 10-633.562 403.818 1
15 0 10 111.582 423.994 3
-15 0 11-537.618 392.971 5
15 0 11 129.835 342.270 4
15 0 11-193.490 417.577 3
-15 0 12 562.361 405.165 5
15 0 12 165.742 423.759 4
15 0 12 995.654 558.956 3
-15 0 13 2172.28 647.914 5
15 0 13 987.614 518.788 3
15 0 14 35.5026 373.598 3
15 -1 -13-253.590 427.709 3
15 -1 -12 2183.77 689.404 3
15 1 -11 4065.09 885.903 3
15 -1 -11 3764.92 817.901 3
15 1 -10 379.590 498.706 3
15 -1 -10 669.519 531.310 3
-15 1 -9 1483.61 586.595 1
15 1 -9 63.5552 401.516 3
15 -1 -9 921.202 527.009 3
-15 -1 -9 1435.68 565.429 1
-15 1 -8 1028.11 501.897 1
15 1 -8 452.822 464.006 3
15 -1 -8 490.970 615.261 3
-15 -1 -8 795.070 439.312 1
-15 1 -7 705.420 358.553 1
15 1 -7 840.848 628.234 3
15 -1 -7 1208.44 472.208 3
-15 -1 -7 1139.79 473.292 1
-15 -1 -6 901.177 457.614 1
-15 1 -6 1709.76 572.257 1
15 1 -6 721.084 544.418 3
15 -1 -6 645.120 534.204 3
-15 -1 -5 1674.21 555.238 1
-15 1 -5 2427.02 636.449 1
15 1 -5 1830.12 717.019 3
15 -1 -5 1076.55 482.242 3
-15 -1 -4 1427.97 638.091 1
-15 1 -4 3829.70 744.695 1
15 1 -4 2409.76 734.064 3
15 -1 -4 1606.87 572.856 3
-15 -1 -3 1111.43 561.922 1
-15 1 -3 1505.59 546.871 1
15 1 -3 688.760 573.347 3
15 -1 -3 1271.18 554.799 3
-15 -1 -2 1306.04 563.154 1
-15 1 -2 1238.09 495.260 1
15 1 -2-68.9307 458.382 3
15 -1 -2-16.3015 478.535 3
-15 -1 -1 475.906 446.218 1
15 1 -1 621.893 562.614 3
-15 1 -1 1038.03 437.462 1
15 -1 -1 1003.09 542.911 3
-15 -1 0 4091.82 835.410 1
15 1 0 3195.34 810.386 3
-15 1 0 3787.98 719.772 1
15 -1 0 3996.09 819.896 3
-15 -1 1 60.3871 461.084 1
15 1 1-173.847 445.089 3
15 -1 1 923.401 512.615 3
-15 1 1 789.480 367.422 1
15 -1 2 218.023 353.665 4
-15 -1 2-556.667 477.742 1
15 1 2-110.715 379.854 3
15 -1 2 315.425 389.424 3
-15 1 2 884.138 389.841 1
-15 1 3 1089.14 406.724 1
15 -1 3 483.285 332.803 4
15 1 3 805.959 446.470 3
-15 -1 3 1022.32 519.975 1
15 -1 3 1077.34 523.513 3
-15 1 4 3037.13 630.911 1
15 -1 4 3343.41 727.617 4
15 1 4 3419.92 815.293 3
15 -1 4 3787.71 797.956 3
-15 -1 4 4238.38 820.270 1
-15 -1 5 1351.81 515.578 1
-15 1 5 1236.15 432.556 1
15 -1 5 1011.31 459.565 4
15 1 5 1961.07 657.690 3
15 -1 5 1078.33 464.434 3
-15 -1 6 1328.05 557.186 1
-15 1 6-735.474 428.013 1
15 1 6 987.557 479.481 4
15 -1 6 830.731 440.391 4
15 1 6 1079.75 454.493 3
15 -1 6 1434.64 574.080 3
15 1 7-630.968 373.103 4
-15 -1 7 667.283 404.262 1
15 -1 7 575.687 393.876 4
-15 1 7-448.119 419.192 1
15 1 7-313.099 369.209 3
15 -1 7 436.020 411.055 3
-15 1 8 709.667 473.523 5
15 1 8 493.217 353.812 4
15 -1 8 481.898 461.563 4
-15 -1 8 1047.72 444.198 1
15 1 8 997.249 499.142 3
15 -1 8 812.711 452.526 3
-15 1 9 286.674 363.712 5
15 1 9 129.097 330.792 4
15 -1 9 535.093 432.512 4
15 1 9 435.274 477.755 3
15 -1 9 564.784 471.464 3
-15 -1 9-12.6332 372.168 1
-15 1 10 1178.26 434.913 5
15 1 10 557.737 419.643 4
15 -1 10 1862.46 688.124 4
-15 -1 10 47.1680 347.538 1
15 1 10-207.411 399.304 3
15 -1 10-62.3555 417.238 3
-15 1 11 3950.42 817.229 5
15 1 11 4522.95 854.883 4
15 -1 11 2504.93 761.676 4
15 1 11 5129.61 905.535 3
15 -1 11 4021.51 870.017 3
-15 -1 11 3778.93 755.672 1
-15 -1 12 694.099 405.037 1
15 1 12 408.846 350.845 4
15 1 12 418.258 377.618 3
15 -1 12-157.531 429.269 3
15 -2 -11 948.986 562.378 3
15 -2 -10 948.449 559.005 3
15 -2 -9 1575.25 597.738 3
15 -2 -8 3266.64 772.528 3
-15 2 -7 1369.38 465.366 1
15 -2 -7-318.713 351.834 3
-15 2 -6 2992.59 706.202 1
-15 -2 -6 1923.43 649.862 1
15 -2 -6 3433.36 782.856 3
-15 2 -5 2719.71 672.090 1
-15 -2 -5 266.280 359.645 1
15 2 -5 2155.37 723.150 3
15 -2 -5 2740.11 726.837 3
-15 2 -4 3579.39 714.330 1
-15 -2 -4 4943.36 937.030 1
15 2 -4 4415.53 940.256 3
15 -2 -4 4305.75 925.419 3
15 2 -4 3444.14 676.664 11
-15 2 -3 2230.35 621.588 1
-15 -2 -3 1744.29 543.379 1
15 2 -3 3065.16 810.040 3
15 -2 -3 1963.67 646.413 3
15 2 -3 2402.34 583.598 11
-15 2 -2 4742.69 779.365 1
15 2 -2 6753.60 1071.07 3
-15 -2 -2 6161.47 1004.76 1
15 -2 -2 5486.04 1019.41 3
-15 2 -1 1692.93 509.452 1
15 2 -1 2791.34 839.330 3
-15 -2 -1 2071.02 653.067 1
15 -2 -1 3460.59 784.163 3
-15 2 0 1600.95 494.492 1
15 2 0 2745.57 746.726 3
15 -2 0 2466.16 782.716 3
-15 -2 0 1080.35 552.734 1
-15 -2 1 2291.42 689.029 1
-15 2 1 1556.36 488.793 1
15 2 1 2074.59 667.044 3
15 -2 1 3320.54 814.133 3
-15 -2 2 6677.06 1039.84 1
15 2 2 6232.79 1094.61 3
-15 2 2 7182.72 924.770 1
15 -2 2 6036.70 1000.24 3
15 2 3 2438.05 742.113 3
-15 2 3 2511.23 596.645 1
15 -2 3 2486.76 710.424 3
-15 -2 4 2778.60 717.762 1
15 2 4 3370.48 771.422 3
15 -2 4 3188.79 822.237 3
-15 2 5-64.8161 406.098 5
-15 -2 5 1389.22 601.189 1
15 2 5 1005.64 464.332 3
15 -2 5 794.506 530.145 3
-15 2 6 2290.76 656.622 5
15 2 6 2629.10 712.570 3
15 -2 6 3111.64 831.338 3
-15 -2 6 2193.92 605.719 1
15 -2 7-128.519 471.410 4
15 2 7 70.4623 492.331 3
15 -2 8 1643.06 739.451 4
15 2 8 2236.82 675.952 3
15 -2 9 1423.76 627.415 4
15 2 9 1485.28 563.828 3
15 2 10 1070.17 483.835 3
-15 3 -4 2096.18 593.429 1
-15 3 -3 2596.29 649.277 1
15 3 -3 2330.83 715.985 11
-15 3 -2 2581.71 615.882 1
15 3 -2 2046.67 622.206 11
15 3 -1 621.403 453.692 11
16 0 -7 10113.0 1554.58 3
16 0 -6 8472.21 1398.17 3
-16 0 -5 24185.3 1875.68 1
16 0 -5 23331.7 2228.05 3
16 0 -4 1689.01 730.576 3
-16 0 -4 1345.92 576.238 1
16 0 -3 10611.1 1486.46 3
-16 0 -3 10217.0 1212.88 1
16 0 -2-18.4043 442.615 3
-16 0 -2 807.912 490.059 1
-16 0 -1 15089.7 1453.01 1
16 0 -1 16705.6 1765.47 3
-16 0 0 656.766 400.771 1
16 0 0 856.488 527.842 3
-16 0 1 13548.2 1421.79 1
16 0 1 14064.2 1608.56 3
-16 0 2-127.572 396.625 1
16 0 2-122.933 391.909 3
-16 0 3 10494.9 1253.92 1
16 0 3 12064.1 1468.07 3
-16 0 4 1368.20 570.976 1
16 0 4 1755.47 622.191 3
-16 0 5 19332.7 1686.41 1
16 0 5 18237.8 1748.29 3
16 0 6 8143.38 1221.99 3
-16 0 6 10643.7 1239.93 1
16 0 7 10568.9 1215.16 4
16 0 7 13062.2 1440.89 3
-16 0 7 10305.2 1196.91 1
-16 0 8 478.478 351.223 1
16 0 8 176.537 421.089 4
16 0 8-270.281 358.718 3
16 0 9 11280.0 1307.35 4
-16 0 9 11511.2 1267.87 1
-16 0 9 10821.1 1245.17 5
-16 0 10 1262.23 558.276 5
16 0 10 1619.31 582.120 4
-16 0 11 9660.05 1188.77 5
16 -1 -6 1520.24 634.186 3
-16 1 -5 17593.1 1572.15 1
16 -1 -5 16995.1 1756.28 3
-16 1 -4 2944.79 697.771 1
16 -1 -4 316.622 541.266 3
-16 -1 -3 8435.64 1157.36 1
-16 1 -3 10117.6 1196.68 1
16 1 -3 6591.43 1164.59 3
16 -1 -3 10013.2 1339.08 3
-16 -1 -2 6131.49 1017.49 1
16 1 -2 4041.50 996.451 3
-16 1 -2 6620.65 973.079 1
16 -1 -2 7542.37 1192.87 3
-16 1 -1 14844.0 1395.78 1
-16 -1 -1 10001.8 1265.57 1
16 -1 -1 15679.9 1630.62 3
16 1 -1 10414.7 1402.22 3
-16 -1 0 794.326 556.184 1
16 1 0-136.427 477.264 3
16 -1 0 280.756 477.467 3
-16 1 0-132.988 366.140 1
-16 1 1 13642.1 1338.68 1
-16 -1 1 12567.6 1415.64 1
16 1 1 14990.5 1738.13 3
16 -1 1 14429.0 1544.99 3
-16 1 2 7792.08 1030.97 1
-16 -1 2 8123.16 1139.18 1
16 1 2 10552.0 1421.44 3
16 -1 2 8334.29 1220.10 3
-16 1 3 6822.62 962.889 1
16 1 3 8849.37 1299.34 3
16 -1 3 10757.2 1337.52 3
-16 -1 3 8080.89 1147.50 1
-16 1 4 1165.64 480.719 1
16 1 4 1792.11 645.348 3
-16 -1 4 1255.60 547.006 1
-16 1 5 14862.4 1439.09 1
16 -1 5 12334.2 1317.37 4
-16 -1 5 14218.2 1485.76 1
16 1 5 17492.8 1730.36 3
-16 -1 6 1983.39 585.246 1
16 -1 6 2010.57 657.553 4
16 1 6 1740.81 650.410 3
16 -1 7 11932.6 1380.42 4
-16 -1 7 12356.2 1358.50 1
16 1 7 11421.9 1371.11 3
16 -1 8 1031.38 462.207 4
-16 -1 8 2447.58 658.411 1
16 1 8 2202.41 702.137 3
-16 -1 9 7731.38 1064.27 1
16 1 9 9033.84 1134.11 4
16 -1 9 7311.55 1125.25 4
16 1 10 1036.53 498.595 4
-16 2 -3 5147.01 860.086 1
-16 2 -2 547.189 486.127 1
-16 2 -1 14386.9 1382.03 1
-16 2 0 4701.01 802.693 1
-16 2 1 13510.8 1301.62 1
-16 2 2 500.832 429.345 1
-17 1 2 3967.79 820.933 1
-17 1 3 154.533 394.930 1
-17 1 4 603.732 358.178 1
;
_shelx_hkl_checksum 23222
_shelx_res_file
;
TITL test_fac in Pca2(1)
test_fac.res
created by SHELXL-2018/3 at 10:47:00 on 06-Jul-2020
REM Pca2(1) (#29 in standard setting)
CELL 0.71073 12.2768 4.4829 19.6694 90 90 90
ZERR 4 0.0003 0.0001 0.0004 0 0 0
LATT -1
SYMM -X,-Y,0.5+Z
SYMM 0.5-X,+Y,0.5+Z
SYMM 0.5+X,-Y,+Z
SFAC C H Br N O
UNIT 52 40 4 4 4
DFIX 0.86 0.01 O1 H1
L.S. 4
PLAN 5
SIZE 0.0493 0.1968 0.4546
TEMP -153(2)
MPLA 6 C1 C2 C3 C4 C5 C6
MPLA 6 C8 C9 C10 C11 C12 C13
MPLA 5 O1 N1 C7 C6 C1
CONF
HTAB O1 N1
GRID
BOND $H
HTAB 2.0
MORE -1
fmap 2
acta 60
MERG 2
SHEL 99999 0.8
REM
REM
REM
WGHT 0.028800 0.249800
FVAR 3.78964
BR1 3 0.424873 1.040535 0.522570 11.00000 0.01826 0.02317 =
0.01312 -0.00249 -0.00119 -0.00238
C4 1 0.332483 0.871485 0.454949 11.00000 0.01811 0.01692 =
0.01036 0.00061 -0.00208 -0.00433
C5 1 0.374567 0.674575 0.408239 11.00000 0.01148 0.01435 =
0.01486 0.00415 -0.00093 -0.00006
AFIX 43
H5 2 0.449969 0.627095 0.409090 11.00000 -1.20000
AFIX 0
C3 1 0.223267 0.950183 0.453763 11.00000 0.01886 0.01940 =
0.01384 -0.00286 0.00352 0.00089
AFIX 43
H3 2 0.195360 1.087904 0.486075 11.00000 -1.20000
AFIX 0
C6 1 0.306605 0.543626 0.359364 11.00000 0.01472 0.01486 =
0.01220 0.00477 0.00087 0.00054
C2 1 0.155139 0.826953 0.405235 11.00000 0.01675 0.02205 =
0.01752 0.00028 0.00229 0.00392
AFIX 43
H2 2 0.080442 0.882022 0.403983 11.00000 -1.20000
AFIX 0
C1 1 0.195586 0.622407 0.358181 11.00000 0.01615 0.01868 =
0.01347 0.00290 -0.00112 -0.00116
O1 5 0.125819 0.504630 0.312390 11.00000 0.01293 0.02817 =
0.01860 -0.00741 -0.00264 0.00134
C7 1 0.351394 0.329185 0.311222 11.00000 0.01291 0.01495 =
0.01559 0.00360 0.00069 0.00041
AFIX 43
H7 2 0.427300 0.288024 0.311612 11.00000 -1.20000
AFIX 0
N1 4 0.289779 0.195270 0.268340 11.00000 0.01572 0.01377 =
0.01196 0.00073 0.00053 0.00026
C8 1 0.331617 -0.016946 0.221109 11.00000 0.01748 0.01268 =
0.01155 0.00185 0.00105 -0.00136
C13 1 0.257846 -0.131673 0.174797 11.00000 0.01752 0.01565 =
0.01813 0.00306 -0.00121 0.00250
AFIX 43
H13 2 0.184046 -0.068148 0.175947 11.00000 -1.20000
AFIX 0
C11 1 0.397797 -0.436223 0.125058 11.00000 0.02817 0.01537 =
0.01436 0.00143 0.00664 0.00094
AFIX 43
H11 2 0.420342 -0.577964 0.092026 11.00000 -1.20000
AFIX 0
C9 1 0.439842 -0.115968 0.220139 11.00000 0.01816 0.01701 =
0.01763 -0.00010 0.00073 0.00045
AFIX 43
H9 2 0.490778 -0.040319 0.252150 11.00000 -1.20000
AFIX 0
C10 1 0.472421 -0.325677 0.172069 11.00000 0.01734 0.01973 =
0.01899 0.00256 0.00483 0.00188
AFIX 43
H10 2 0.545717 -0.393545 0.171327 11.00000 -1.20000
AFIX 0
C12 1 0.291173 -0.339771 0.126500 11.00000 0.02452 0.01843 =
0.01698 -0.00159 -0.00102 -0.00159
AFIX 43
H12 2 0.240293 -0.415470 0.094460 11.00000 -1.20000
AFIX 0
H1 2 0.161014 0.368646 0.291033 11.00000 0.03614
HKLF 4
REM test_fac in Pca2(1)
REM wR2 = 0.0529, GooF = S = 1.054, Restrained GooF = 1.054 for all data
REM R1 = 0.0219 for 2133 Fo > 4sig(Fo) and 0.0236 for all 2215 data
REM 149 parameters refined using 2 restraints
END
WGHT 0.0288 0.2497
REM Instructions for potential hydrogen bonds
EQIV $1 x-1/2, -y+2, z
HTAB C2 Br1_$1
EQIV $2 x+1/2, -y+1, z
HTAB C7 O1_$2
HTAB O1 N1
REM Highest difference peak 0.386, deepest hole -0.231, 1-sigma level 0.055
Q1 1 0.4591 0.8507 0.5218 11.00000 0.05 0.39
Q2 1 0.3867 1.2273 0.5223 11.00000 0.05 0.38
Q3 1 0.3852 0.8475 0.5235 11.00000 0.05 0.37
Q4 1 0.4831 1.1622 0.5225 11.00000 0.05 0.37
Q5 1 0.3801 -0.1102 0.2208 11.00000 0.05 0.22
;
_shelx_res_checksum 86604
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.42487(2) 1.04053(7) 0.52257(3) 0.01818(11) Uani d 1 . .
C C4 0.3325(3) 0.8715(8) 0.45495(18) 0.0151(7) Uani d 1 . .
C C5 0.3746(3) 0.6746(8) 0.40824(17) 0.0136(7) Uani d 1 . .
H H5 0.449969 0.627095 0.409090 0.016 Uiso calc 1 . .
C C3 0.2233(3) 0.9502(8) 0.45376(19) 0.0174(8) Uani d 1 . .
H H3 0.195360 1.087904 0.486075 0.021 Uiso calc 1 . .
C C6 0.3066(3) 0.5436(8) 0.35936(19) 0.0139(7) Uani d 1 . .
C C2 0.1551(3) 0.8270(9) 0.40524(19) 0.0188(8) Uani d 1 . .
H H2 0.080442 0.882022 0.403983 0.023 Uiso calc 1 . .
C C1 0.1956(3) 0.6224(9) 0.35818(18) 0.0161(8) Uani d 1 . .
O O1 0.1258(3) 0.5046(6) 0.31239(14) 0.0199(6) Uani d 1 . .
C C7 0.3514(3) 0.3292(8) 0.31122(18) 0.0145(7) Uani d 1 . .
H H7 0.427300 0.288024 0.311612 0.017 Uiso calc 1 . .
N N1 0.2898(2) 0.1953(6) 0.26834(14) 0.0138(6) Uani d 1 . .
C C8 0.3316(3) -0.0169(7) 0.2211(2) 0.0139(8) Uani d 1 . .
C C13 0.2578(3) -0.1317(8) 0.17480(18) 0.0171(7) Uani d 1 . .
H H13 0.184046 -0.068148 0.175947 0.021 Uiso calc 1 . .
C C11 0.3978(4) -0.4362(8) 0.1251(2) 0.0193(8) Uani d 1 . .
H H11 0.420342 -0.577964 0.092026 0.023 Uiso calc 1 . .
C C9 0.4398(3) -0.1160(9) 0.2201(2) 0.0176(8) Uani d 1 . .
H H9 0.490778 -0.040319 0.252150 0.021 Uiso calc 1 . .
C C10 0.4724(3) -0.3257(8) 0.17207(19) 0.0187(8) Uani d 1 . .
H H10 0.545717 -0.393545 0.171327 0.022 Uiso calc 1 . .
C C12 0.2912(3) -0.3398(9) 0.12650(19) 0.0200(8) Uani d 1 . .
H H12 0.240293 -0.415470 0.094460 0.024 Uiso calc 1 . .
H H1 0.161(3) 0.369(8) 0.291(2) 0.036(14) Uiso 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
Br1 0.01826(17) 0.02317(18) 0.01312(16) -0.00238(12) -0.0012(2) -0.0025(3)
C4 0.0181(19) 0.0169(17) 0.0104(17) -0.0043(15) -0.0021(13) 0.0006(15)
C5 0.0115(17) 0.0143(17) 0.0149(17) -0.0001(14) -0.0009(14) 0.0041(14)
C3 0.019(2) 0.0194(18) 0.0138(18) 0.0009(15) 0.0035(16) -0.0029(15)
C6 0.0147(18) 0.0149(17) 0.0122(18) 0.0005(14) 0.0009(14) 0.0048(14)
C2 0.0167(19) 0.0221(19) 0.0175(19) 0.0039(16) 0.0023(15) 0.0003(16)
C1 0.0161(18) 0.0187(18) 0.0135(18) -0.0012(15) -0.0011(15) 0.0029(15)
O1 0.0129(14) 0.0282(15) 0.0186(14) 0.0013(11) -0.0026(11) -0.0074(12)
C7 0.0129(17) 0.0149(17) 0.0156(17) 0.0004(15) 0.0007(14) 0.0036(15)
N1 0.0157(15) 0.0138(15) 0.0120(13) 0.0003(11) 0.0005(13) 0.0007(12)
C8 0.017(2) 0.0127(17) 0.0115(18) -0.0014(14) 0.0011(13) 0.0018(14)
C13 0.0175(19) 0.0157(16) 0.0181(18) 0.0025(15) -0.0012(15) 0.0031(15)
C11 0.028(2) 0.0154(19) 0.0144(19) 0.0009(16) 0.0066(16) 0.0014(15)
C9 0.0182(19) 0.0170(18) 0.0176(19) 0.0005(15) 0.0007(14) -0.0001(15)
C10 0.0173(19) 0.0197(19) 0.0190(19) 0.0019(15) 0.0048(15) 0.0026(16)
C12 0.025(2) 0.0184(19) 0.0170(18) -0.0016(16) -0.0010(16) -0.0016(16)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
14 3 -7 0.0246
-14 -3 7 0.0246
7 1 -25 0.0590
-7 -1 25 0.0590
9 -5 8 0.2102
-9 5 -8 0.2102
11 -1 -21 0.0872
-5 -2 25 0.0757
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
C5 C4 Br1 . . 119.9(3) ?
C5 C4 C3 . . 121.0(3) ?
C3 C4 Br1 . . 119.1(3) ?
C4 C5 H5 . . 119.9 ?
C4 C5 C6 . . 120.2(3) ?
C6 C5 H5 . . 119.9 ?
C4 C3 H3 . . 120.2 ?
C2 C3 C4 . . 119.6(3) ?
C2 C3 H3 . . 120.2 ?
C5 C6 C1 . . 118.8(3) ?
C5 C6 C7 . . 119.8(3) ?
C1 C6 C7 . . 121.3(3) ?
C3 C2 H2 . . 119.8 ?
C3 C2 C1 . . 120.3(4) ?
C1 C2 H2 . . 119.8 ?
C2 C1 C6 . . 119.9(3) ?
O1 C1 C6 . . 121.8(3) ?
O1 C1 C2 . . 118.3(3) ?
C1 O1 H1 . . 107(3) ?
C6 C7 H7 . . 119.5 ?
N1 C7 C6 . . 120.9(3) ?
N1 C7 H7 . . 119.5 ?
C7 N1 C8 . . 121.9(3) ?
C13 C8 N1 . . 116.2(3) ?
C13 C8 C9 . . 119.6(4) ?
C9 C8 N1 . . 124.2(3) ?
C8 C13 H13 . . 119.8 ?
C8 C13 C12 . . 120.4(4) ?
C12 C13 H13 . . 119.8 ?
C10 C11 H11 . . 120.0 ?
C12 C11 H11 . . 120.0 ?
C12 C11 C10 . . 119.9(4) ?
C8 C9 H9 . . 120.1 ?
C10 C9 C8 . . 119.7(4) ?
C10 C9 H9 . . 120.1 ?
C11 C10 H10 . . 119.9 ?
C9 C10 C11 . . 120.1(4) ?
C9 C10 H10 . . 119.9 ?
C13 C12 H12 . . 119.9 ?
C11 C12 C13 . . 120.2(4) ?
C11 C12 H12 . . 119.9 ?
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
Br1 C4 . 1.905(4) ?
C4 C5 . 1.375(5) ?
C4 C3 . 1.387(5) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.402(5) ?
C3 H3 . 0.9500 ?
C3 C2 . 1.384(6) ?
C6 C1 . 1.408(5) ?
C6 C7 . 1.457(5) ?
C2 H2 . 0.9500 ?
C2 C1 . 1.394(5) ?
C1 O1 . 1.350(5) ?
O1 H1 . 0.857(14) ?
C7 H7 . 0.9500 ?
C7 N1 . 1.282(4) ?
N1 C8 . 1.425(5) ?
C8 C13 . 1.384(5) ?
C8 C9 . 1.401(5) ?
C13 H13 . 0.9500 ?
C13 C12 . 1.393(5) ?
C11 H11 . 0.9500 ?
C11 C10 . 1.393(6) ?
C11 C12 . 1.379(6) ?
C9 H9 . 0.9500 ?
C9 C10 . 1.392(5) ?
C10 H10 . 0.9500 ?
C12 H12 . 0.9500 ?
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
O1 H1 N1 . 0.857(14) 1.82(3) 2.593(4) 150(5) 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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Br1 C4 C5 C6 . . . . 178.4(3) ?
Br1 C4 C3 C2 . . . . -179.5(3) ?
C4 C5 C6 C1 . . . . 1.4(5) ?
C4 C5 C6 C7 . . . . -178.4(3) ?
C4 C3 C2 C1 . . . . 0.7(6) ?
C5 C4 C3 C2 . . . . 0.6(6) ?
C5 C6 C1 C2 . . . . -0.1(5) ?
C5 C6 C1 O1 . . . . 179.9(3) ?
C5 C6 C7 N1 . . . . 176.4(3) ?
C3 C4 C5 C6 . . . . -1.6(5) ?
C3 C2 C1 C6 . . . . -0.9(6) ?
C3 C2 C1 O1 . . . . 179.0(3) ?
C6 C7 N1 C8 . . . . -179.5(3) ?
C1 C6 C7 N1 . . . . -3.3(5) ?
C7 C6 C1 C2 . . . . 179.6(3) ?
C7 C6 C1 O1 . . . . -0.3(6) ?
C7 N1 C8 C13 . . . . -176.1(3) ?
C7 N1 C8 C9 . . . . 5.1(5) ?
N1 C8 C13 C12 . . . . 179.8(3) ?
N1 C8 C9 C10 . . . . 179.6(3) ?
C8 C13 C12 C11 . . . . 0.9(6) ?
C8 C9 C10 C11 . . . . 0.1(6) ?
C13 C8 C9 C10 . . . . 0.8(6) ?
C9 C8 C13 C12 . . . . -1.3(6) ?
C10 C11 C12 C13 . . . . 0.1(5) ?
C12 C11 C10 C9 . . . . -0.6(5) ?
_cod_database_fobs_code 2022295