#------------------------------------------------------------------------------
#$Date: 2023-12-07 12:51:21 +0100 (Thu, 07 Dec 2023) $
#$Revision: 288147 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022872.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_2022872
loop_
_publ_author_name
'Mohamed-Ezzat, Reham A'
'Kariuki, Benson M.'
'Srour, Aladdin M.'
_publ_section_title
;
Synthesis, crystal structure and in vitro anti-proliferative
activity of 2-[(4-acetyl-phen-yl)carbamo-yl]phenyl acetate.
;
_journal_coeditor_code DJ2060
_journal_issue 'Pt 11'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 999
_journal_page_last 1002
_journal_paper_doi 10.1107/S2056989023008526
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C17 H15 N O4'
_chemical_formula_moiety 'C17 H15 N O4'
_chemical_formula_sum 'C17 H15 N O4'
_chemical_formula_weight 297.30
_chemical_name_systematic
;
2-[(4-Acetylphenyl)carbamoyl]phenyl acetate
;
_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 geom
_atom_sites_solution_primary direct
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 110.380(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.6286(5)
_cell_length_b 8.6913(4)
_cell_length_c 15.8180(7)
_cell_measurement_reflns_used 5304
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 76.1740
_cell_measurement_theta_min 4.0800
_cell_volume 1498.62(13)
_computing_cell_refinement
;
CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature 296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Agilant SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0274
_diffrn_reflns_av_unetI/netI 0.0162
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 17065
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 76.927
_diffrn_reflns_theta_min 4.113
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.781
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.390
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.318
_exptl_crystal_description needle
_exptl_crystal_F_000 624
_exptl_crystal_size_max 0.354
_exptl_crystal_size_mid 0.144
_exptl_crystal_size_min 0.130
_refine_diff_density_max 0.165
_refine_diff_density_min -0.157
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.032
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 201
_refine_ls_number_reflns 3141
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.032
_refine_ls_R_factor_all 0.0509
_refine_ls_R_factor_gt 0.0427
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+0.1892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1229
_refine_ls_wR_factor_ref 0.1337
_reflns_number_gt 2612
_reflns_number_total 3141
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file dj2060sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2022872.cif.'
_cod_original_cell_volume 1498.62(12)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2022872
_cod_database_fobs_code 2022872
_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 0.769
_shelx_estimated_absorpt_t_max 0.905
_shelx_hkl_file
;
0 0 -2 196219. 1138.40 2
0 0 -3 16.5132 45.2958 2
0 0 4 236338. 1580.20 11
0 0 -4 242313. 1834.17 2
0 0 5 96.1037 50.2920 11
0 0 -5 48.0989 72.6279 2
0 0 6 63470.6 1005.16 11
0 0 -6 65075.3 1206.65 2
0 0 7 51.5757 69.6162 11
0 0 -7 77.8288 117.370 2
0 0 8 7108.21 397.795 11
0 0 -8 8125.56 522.843 2
0 0 9 56.3928 51.4841 11
0 0 -9-47.9317 98.5372 2
0 0 -9-112.915 94.4835 1
0 0 10 2200.97 252.917 11
0 0 -10 2013.90 305.921 1
0 0 -10 1741.90 281.829 2
0 0 -11 82.1178 110.646 1
0 0 -12 10604.0 464.653 42
0 0 -12 10245.4 770.357 1
0 0 -12 10784.8 453.842 51
0 0 13-25.9744 50.8471 48
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0 0 -14 538.942 126.898 42
0 0 14 378.793 96.8397 48
0 0 -14 632.386 117.265 31
0 0 -15-20.2917 73.0577 40
0 0 15 96.2323 64.7138 48
0 0 -16 1254.68 147.900 40
0 0 16 1169.45 124.519 48
0 0 -17-4.51871 49.6803 40
0 0 18 408.184 50.8115 44
0 0 -18 462.325 57.7757 40
0 -1 0 78.6966 30.9531 3
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0 1 -1 6532.71 165.195 2
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-12 6 6-18.6946 35.5881 54
-12 6 6 10.6838 30.3966 53
12 -6 -6-55.0227 43.2895 45
-12 6 6 37.1915 32.8198 51
-12 6 5 62.5265 39.0636 54
-12 6 5 154.693 41.8487 53
12 -6 -5 134.267 46.7898 45
-12 6 5 49.5884 34.1206 51
-12 6 4 129.161 40.4876 54
-12 6 4 141.666 37.6925 53
-12 6 4 158.910 42.6606 51
12 -6 -4 223.069 49.1251 45
-12 6 3 178.916 38.9333 51
-13 0 14-32.0205 18.4199 32
-13 0 14 39.3494 29.3999 20
-13 0 13 234.931 51.5767 32
-13 0 13 356.733 67.0408 20
-13 0 12-16.4855 40.5008 32
-13 0 12 6.09770 43.1285 20
-13 0 11 47.9311 51.2772 32
-13 0 11 114.324 56.0258 20
-13 0 10-22.7983 52.4620 32
-13 0 10-2.01964 23.6283 30
-13 0 10 34.4654 51.6640 20
-13 0 9 9110.76 358.656 32
-13 0 9 8354.56 327.521 20
-13 0 8-44.8936 63.7035 32
-13 0 8-28.7513 48.4941 20
-13 0 7 268.148 85.3012 32
-13 0 7 218.795 70.4768 30
-13 0 7 222.510 67.6903 20
-13 0 6 67.3482 61.5583 32
-13 0 6-55.9200 56.1994 30
-13 0 6-59.0756 47.1513 20
-13 0 5 35.9999 53.8568 30
-13 0 5 42.5794 36.8481 20
-13 0 4-7.85543 61.7788 30
-13 0 3 1044.64 113.325 26
-13 0 3 925.412 126.881 30
-13 0 2-19.9057 30.3347 26
-13 0 2-14.7087 52.5893 30
-13 0 1 943.192 119.126 30
-13 0 0-45.4919 51.1968 30
-13 0 0-61.6829 25.1716 15
-13 0 -1-1.35240 36.2078 30
-13 0 -1 115.150 25.5056 15
-13 0 -2 22.3242 22.8393 30
-13 1 14-30.1405 26.9831 32
-13 -1 14-14.4382 26.5338 20
-13 1 14-16.4389 23.6498 20
-13 -1 13 5.57829 22.3554 32
-13 1 13-12.5815 30.8211 32
-13 -1 13-0.71059 30.4412 20
-13 1 13 38.9979 34.6627 20
-13 -1 12 12.0537 33.8180 32
-13 1 12 59.1440 39.3762 32
-13 -1 12 46.8829 47.8093 20
-13 1 12 6.73321 37.8027 20
-13 -1 11 152.845 56.0937 32
-13 1 11 214.784 67.2765 32
-13 -1 11 202.009 66.3579 20
-13 1 11 259.649 61.1410 20
-13 -1 10 266.783 72.8635 32
-13 1 10 301.414 78.6271 32
-13 1 10 118.533 44.6806 53
-13 -1 10 237.083 72.8094 20
-13 1 10 331.209 70.5151 20
-13 -1 9 454.656 95.2928 32
-13 1 9 466.780 102.296 32
-13 1 9 362.817 68.9926 53
-13 -1 9 243.159 76.8336 20
-13 1 9 468.618 77.0464 20
-13 -1 8 1794.75 141.576 30
-13 -1 8 2071.77 179.224 32
-13 1 8 1985.05 173.960 32
-13 1 8 1843.05 142.314 53
-13 -1 8 2068.49 174.769 20
-13 1 8 1568.03 134.772 20
-13 -1 7-87.0542 76.0932 32
-13 1 7 20.1579 56.6999 32
-13 -1 7 21.1771 43.1016 30
-13 1 7-137.411 54.6949 53
-13 -1 7-173.065 67.2375 20
-13 1 7 26.1146 36.3715 20
-13 -1 6 801.064 110.918 30
-13 1 6 730.549 113.072 32
-13 1 6 589.925 87.4941 53
-13 -1 6 654.046 104.556 20
-13 1 5-49.0556 59.0331 32
-13 -1 5 25.9405 50.6500 30
-13 1 5-6.74249 40.9057 53
-13 -1 5-44.7853 48.2345 20
-13 1 4 120.874 54.5594 53
-13 1 4 80.1558 68.7358 30
-13 -1 4 82.1955 59.7701 30
-13 1 3 207.768 59.8738 53
-13 -1 3 267.723 68.1348 26
-13 -1 3 194.050 69.9588 30
-13 1 3 157.483 69.8532 30
-13 1 2 791.104 90.6717 53
-13 -1 2 814.249 101.668 26
-13 1 2 831.030 112.955 30
-13 -1 2 937.936 120.165 30
-13 1 1 1201.99 103.080 53
-13 -1 1 1322.73 111.348 26
-13 -1 1 1491.32 138.315 30
-13 1 1 1273.34 127.924 30
-13 1 0 6.41733 23.2377 53
-13 -1 0 74.9335 31.7016 26
-13 -1 0 40.8128 42.3772 30
-13 1 0 5.21365 41.1939 30
-13 -1 -1 153.163 43.6541 30
-13 1 -1 220.877 48.7885 30
-13 2 14 305.355 45.4144 32
-13 -2 14 202.797 37.8478 20
-13 2 13-59.0132 35.0046 32
-13 -2 13-11.6097 32.4876 20
-13 2 13 18.4810 20.6836 20
-13 2 12-46.7523 27.4761 20
13 -2 -12-20.5598 28.0303 45
-13 2 12-57.1034 41.5906 32
-13 2 12 21.7110 30.2570 53
-13 2 11 107.021 53.2559 32
-13 2 11 90.0442 41.8089 53
-13 -2 11 143.526 57.6329 20
-13 2 11 163.932 43.1024 20
-13 2 10 31.3912 44.6216 32
-13 2 10 1.05750 35.2421 54
-13 2 10-63.3014 46.3335 53
-13 -2 10-6.88338 46.9506 20
-13 2 10 31.2441 28.0089 20
-13 2 9 843.346 110.403 32
-13 2 9 761.493 93.1289 54
-13 2 9 677.183 94.3887 53
-13 -2 9 743.463 108.114 20
-13 2 8 56.2481 52.9565 32
-13 2 8 24.1681 39.5308 54
-13 2 8 144.460 59.3155 53
-13 -2 8 112.902 60.5110 20
-13 2 7 272.960 71.7643 32
-13 -2 7 149.057 49.7302 30
-13 2 7 262.261 64.3496 54
-13 2 7 355.720 79.9357 53
-13 -2 7 190.716 71.5197 20
-13 2 6 43.3944 56.4918 32
-13 -2 6-36.6290 40.3372 30
-13 2 6-23.6089 45.0954 54
-13 2 6-40.0926 55.6395 53
-13 -2 6-76.4994 64.8059 20
-13 2 5 22.8710 45.7987 54
-13 2 5-23.6590 51.4602 53
-13 2 5-59.5248 49.4978 32
-13 -2 5 25.8060 31.7389 30
-13 2 4 5.86974 41.9294 54
-13 2 4-29.5162 54.3897 53
-13 -2 4 61.3059 55.1895 26
-13 -2 4 64.8124 56.9984 30
-13 2 3-52.6996 43.7373 54
-13 2 3 25.9809 46.2177 53
-13 2 3 56.7084 48.0470 30
-13 -2 3 27.2954 42.1251 30
-13 -2 3 0.68275 44.4446 26
-13 2 2 485.287 81.9573 53
-13 -2 2 678.825 94.0427 30
-13 2 2 496.946 89.1895 30
-13 -2 2 625.657 87.7680 26
13 -2 -2 658.915 88.0280 45
-13 2 1 186.994 54.7787 53
-13 -2 1 124.801 45.4779 26
-13 -2 1 200.192 55.3417 30
-13 2 1 140.104 50.5294 30
-13 2 0 44.5001 30.1910 53
-13 -2 0-33.2136 27.0384 26
-13 -2 0 33.8372 38.6677 30
-13 2 0 22.4603 29.0642 30
-13 2 -1 63.5289 27.9944 53
-13 3 13-12.0526 27.1372 32
-13 -3 12 87.1803 39.6272 20
13 -3 -12 115.907 35.0346 38
-13 3 12 124.499 38.3331 32
-13 3 12 23.0552 27.1671 53
-13 3 12-25.0403 28.6046 54
13 -3 -11 14.5528 31.0718 45
-13 -3 11 91.7006 50.1353 20
13 -3 -11 5.43523 28.1770 38
-13 3 11 31.4721 39.8464 32
-13 3 11 92.5029 40.2309 53
-13 3 11 0.59589 36.1712 54
-13 -3 10 73.5738 46.2939 20
13 -3 -10 2.93175 45.3004 45
-13 3 10 38.2834 37.0315 32
-13 3 10 19.5287 35.5551 54
-13 3 10 22.1006 39.7898 53
-13 -3 9 2459.23 171.834 20
13 -3 -9 2298.17 163.023 45
-13 3 9 2045.70 144.229 32
-13 3 9 2007.77 143.575 54
-13 3 9 1946.29 146.012 53
-13 -3 8 108.451 56.9540 20
13 -3 -8 66.5537 55.6083 45
-13 3 8-0.39675 43.9776 54
-13 3 8 89.4068 56.3324 53
-13 3 8 127.475 48.2520 32
-13 -3 7 1438.62 140.371 20
-13 3 7 1217.05 111.509 32
-13 3 7 1232.84 121.384 54
-13 3 7 1219.47 125.449 53
-13 3 7 1270.05 105.695 51
-13 3 6 133.123 42.2348 32
-13 3 6 143.239 57.7626 54
-13 3 6 178.458 63.5322 53
13 -3 -6 321.197 82.1155 45
-13 3 6 195.539 50.9941 51
-13 3 5 1694.91 140.545 54
-13 3 5 1863.08 150.411 53
-13 3 5 1419.03 115.106 51
-13 -3 5 1805.02 149.458 26
13 -3 -5 1912.20 160.637 45
-13 3 4-50.4728 53.0327 54
-13 3 4-110.323 39.7328 51
-13 3 4 0.42714 46.3913 53
-13 -3 4-28.2378 27.7844 30
-13 -3 4 69.4562 50.8690 26
13 -3 -4 46.7561 56.1527 45
-13 3 3 153.051 51.6282 54
-13 3 3 152.924 48.4385 51
-13 3 3 153.815 53.2958 53
-13 3 3 227.892 58.6289 30
-13 -3 3 204.765 47.6200 30
-13 -3 3 250.503 61.3872 26
13 -3 -3 284.764 66.9392 45
-13 3 2 667.025 87.6070 53
-13 3 2 560.281 67.7897 51
-13 3 2 696.038 83.5232 30
-13 -3 2 549.412 72.8210 30
-13 -3 2 674.974 85.0060 26
13 -3 -2 664.359 77.7452 45
-13 3 1 45.1790 29.4402 51
-13 3 1 11.0174 32.9318 53
-13 -3 1 7.37233 27.7022 26
-13 3 1 7.05908 22.3469 30
-13 3 0 147.361 42.5720 53
-13 -3 0 100.530 30.4148 26
-13 4 11 587.124 64.3110 54
-13 4 11 547.302 61.6473 53
-13 4 10 258.243 54.7717 54
-13 4 10 292.236 53.3649 53
13 -4 -10 319.719 52.9439 45
-13 4 9-34.7180 39.6993 54
-13 4 9 33.9948 38.6258 53
-13 4 9-7.37023 13.1323 32
-13 -4 9 64.0618 27.9647 26
-13 4 9 65.9960 31.5766 51
13 -4 -9-29.1089 36.6821 45
-13 4 8 869.815 94.4875 54
-13 4 8 861.503 95.3472 53
-13 4 8 757.056 72.1359 51
-13 -4 8 783.101 79.2805 26
13 -4 -8 990.662 104.517 45
-13 4 7-40.1413 50.2074 54
-13 4 7-33.5718 46.1886 53
-13 -4 7 74.9314 35.7690 26
-13 4 7 111.902 36.8843 51
13 -4 -7-31.3661 49.7635 45
-13 4 6 78.7445 46.4215 54
-13 4 6 41.8297 40.8410 53
-13 -4 6 87.1375 41.7282 26
-13 4 6 48.2032 32.4861 51
13 -4 -6 148.397 61.4543 45
-13 4 5 777.694 90.7978 54
-13 4 5 695.542 89.3886 53
-13 4 5 661.143 77.5502 51
-13 -4 5 763.401 86.3563 26
13 -4 -5 698.737 89.8446 45
-13 4 4-5.09521 44.2637 54
-13 4 4-57.3964 34.5172 51
-13 4 4 45.6040 38.3904 53
-13 4 4-1.56715 31.2926 30
-13 -4 4 32.0575 33.0253 26
13 -4 -4-45.6622 43.0439 45
-13 4 3 1361.18 109.798 53
-13 4 3 1278.21 95.3552 51
-13 4 3 1148.86 91.3599 30
13 -4 -3 1369.88 103.760 45
-13 -4 3 1254.74 99.8170 26
-13 -4 2 129.839 38.7271 26
-13 4 2 76.4246 36.8946 53
-13 4 2 130.869 34.4770 51
-13 -4 1 30.1883 19.9615 26
-13 4 1 14.4243 25.2550 53
-13 5 8-0.89225 21.7163 54
-13 5 8 18.9240 25.5767 53
13 -5 -7-12.4043 24.0629 45
-13 5 7-21.6944 30.1702 54
-13 5 7 31.8565 26.7263 53
13 -5 -6 270.917 49.7265 45
-13 5 6 192.575 44.4533 54
-13 5 6 259.242 45.1148 53
13 -5 -5 30.5193 26.3020 45
-13 5 5-12.0410 25.2792 54
-13 5 5 43.6050 26.9867 53
-14 0 11-21.7366 26.9515 32
-14 0 11-37.5303 24.2558 20
-14 0 10 1285.97 108.071 32
-14 0 10 1002.42 86.5302 20
-14 0 9-58.4165 18.0096 30
-14 0 9-53.8101 26.9461 20
-14 0 8 1933.58 121.724 30
-14 0 8 1596.30 108.190 20
-14 0 7 2.12030 30.6555 30
-14 0 6-20.7277 35.9222 30
-14 0 5 15.2190 36.6120 30
-14 0 5 8.81050 25.9213 26
-14 0 4 419.868 68.0592 30
-14 0 4 394.127 49.9706 26
-14 0 3 45.7157 33.5570 30
-14 0 2 28.4961 30.4626 30
-14 0 1-45.5580 23.7064 30
-14 1 11 39.8689 29.1682 32
-14 -1 11-0.26748 24.6553 20
-14 1 10 75.5335 38.9394 32
-14 -1 10 15.8249 26.8983 20
-14 1 9 2598.74 136.072 30
-14 1 9 2979.83 162.302 32
-14 -1 9 2726.81 150.132 20
-14 1 8 109.086 42.6428 30
-14 -1 8 71.6592 37.7870 20
-14 -1 7 99.0780 31.1169 30
-14 1 7-24.0316 35.8718 30
-14 -1 6 248.908 50.2179 30
-14 1 6 320.012 65.1074 30
-14 -1 5 117.281 42.5185 30
-14 1 5 142.661 50.6611 30
-14 -1 5 114.057 45.2289 26
-14 -1 4 224.603 49.9098 30
-14 1 4 160.837 49.2083 30
-14 -1 4 104.273 38.7245 26
-14 -1 3 1550.36 107.379 30
-14 1 3 1661.60 115.693 30
-14 -1 2 12.2983 26.9589 30
-14 1 2 18.2880 27.8185 30
-14 2 11 272.930 42.8412 32
-14 -2 11 373.666 50.8179 20
-14 2 10 177.364 41.1678 32
14 -2 -10 224.595 43.2490 45
-14 -2 10 202.259 45.2764 20
-14 2 9 85.7545 35.2796 32
-14 2 9 65.2109 31.4540 30
14 -2 -9 56.3455 32.6696 45
-14 -2 9 91.7331 40.2111 20
14 -2 -8 430.811 69.8203 45
-14 2 8 384.026 59.0548 30
14 -2 -7 604.942 79.6313 45
-14 -2 7 515.156 69.8351 26
-14 2 7 468.407 68.5891 30
14 -2 -6 104.953 45.7854 45
-14 -2 6 126.321 43.0817 26
-14 2 6 60.2599 38.4481 30
14 -2 -5 626.964 75.7684 45
-14 -2 5 727.946 77.3807 26
-14 2 5 706.600 81.8493 30
14 -2 -4 245.963 47.7683 45
-14 -2 4 269.383 47.5189 26
-14 2 4 201.341 46.3661 30
-14 -2 3 357.309 45.9542 26
-14 2 3 497.727 61.8804 30
14 -3 -8 49.7907 28.6356 45
-14 -3 8 88.1897 28.1773 26
-14 3 8 44.9207 29.0384 30
14 -3 -7 18.5621 29.3452 45
-14 -3 7 13.8762 20.4549 26
-14 3 7-1.75652 24.4235 30
14 -3 -6 44.4328 31.8043 45
-14 3 6-18.4909 19.4971 30
-14 -3 6 42.4310 26.0411 26
-14 3 5 16.3606 20.5107 30
-14 -3 5 28.7296 22.1868 26
0 0 0 0.00 0.00 0
TITL bmk2106c in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184 11.628641 8.691324 15.818020 90.0000 110.3796 90.0000
ZERR 4.00 0.000523 0.000415 0.000716 0.0000 0.0049 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O
UNIT 68.00 100.00 4.00 16.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 22040
_shelx_res_file
;
TITL bmk2106c in P2(1)/n
shelx.res
created by SHELXL-2018/3 at 18:25:51 on 19-Jun-2023
CELL 1.54184 11.6286 8.6913 15.8180 90.000 110.380 90.000
ZERR 4.00 0.0005 0.0004 0.0007 0.000 0.005 0.000
LATT 1
SYMM 1/2 - X, 1/2 + Y, 1/2 - Z
SFAC C H N O
UNIT 68 60 4 16
MERG 2
FMAP 2
PLAN 10
SIZE 0.130 0.144 0.354
ACTA
BOND $H
LIST 4
L.S. 2
CONF
TEMP 23.00
WGHT 0.076100 0.189200
FVAR 7.43341
C1 1 0.538764 0.146638 0.631406 11.00000 0.08138 0.12046 =
0.05715 0.02680 0.02226 0.00228
AFIX 137
H1A 2 0.587598 0.105244 0.689002 11.00000 -1.50000
H1B 2 0.498487 0.064212 0.591739 11.00000 -1.50000
H1C 2 0.478372 0.215398 0.638833 11.00000 -1.50000
AFIX 0
C2 1 0.619231 0.232113 0.592045 11.00000 0.05592 0.06865 =
0.04446 0.00528 0.01274 0.01458
C3 1 0.567744 0.292530 0.498548 11.00000 0.04735 0.05924 =
0.04121 0.00256 0.01080 0.00717
C4 1 0.646224 0.360633 0.460579 11.00000 0.04238 0.07375 =
0.04968 0.00927 0.00302 -0.00195
AFIX 43
H4 2 0.728942 0.370691 0.495050 11.00000 -1.20000
AFIX 0
C5 1 0.604552 0.413629 0.373140 11.00000 0.04610 0.07453 =
0.04964 0.01021 0.00875 -0.00793
AFIX 43
H5 2 0.658915 0.457351 0.348638 11.00000 -1.20000
AFIX 0
C6 1 0.480675 0.401407 0.321652 11.00000 0.04782 0.05330 =
0.03911 0.00105 0.00673 -0.00208
C7 1 0.401089 0.334037 0.358356 11.00000 0.04220 0.08917 =
0.04701 0.00943 0.00448 -0.00606
AFIX 43
H7 2 0.318208 0.325327 0.324040 11.00000 -1.20000
AFIX 0
C8 1 0.444429 0.279500 0.446057 11.00000 0.04702 0.08716 =
0.04965 0.01100 0.01458 -0.00170
AFIX 43
H8 2 0.390386 0.233633 0.470096 11.00000 -1.20000
AFIX 0
C9 1 0.480643 0.560377 0.191447 11.00000 0.05553 0.05596 =
0.04444 0.00156 0.01005 -0.00384
C10 1 0.410250 0.583470 0.092777 11.00000 0.04770 0.05794 =
0.04516 0.00607 0.01268 -0.00021
C11 1 0.386808 0.730796 0.056896 11.00000 0.04792 0.05880 =
0.05445 0.00551 0.01979 0.00203
C12 1 0.327709 0.754822 -0.033903 11.00000 0.05634 0.06913 =
0.06191 0.02157 0.01901 0.00890
AFIX 43
H12 2 0.311768 0.854402 -0.056485 11.00000 -1.20000
AFIX 0
C13 1 0.292176 0.630327 -0.091344 11.00000 0.05892 0.08813 =
0.04674 0.01535 0.01018 -0.00163
AFIX 43
H13 2 0.252995 0.646157 -0.152872 11.00000 -1.20000
AFIX 0
C14 1 0.314543 0.482680 -0.057858 11.00000 0.06330 0.07493 =
0.04647 -0.00034 0.01222 -0.00827
AFIX 43
H14 2 0.291076 0.398867 -0.096645 11.00000 -1.20000
AFIX 0
C15 1 0.372130 0.459894 0.033822 11.00000 0.05946 0.05762 =
0.04947 0.00448 0.01184 -0.00285
AFIX 43
H15 2 0.385567 0.360130 0.056397 11.00000 -1.20000
AFIX 0
C16 1 0.523868 0.930126 0.124747 11.00000 0.06759 0.05220 =
0.06176 0.01136 0.02226 0.00080
C17 1 0.543637 1.061161 0.189681 11.00000 0.12279 0.06332 =
0.07509 -0.00230 0.03908 -0.01397
AFIX 137
H17A 2 0.559486 1.021628 0.249346 11.00000 -1.50000
H17B 2 0.471610 1.124674 0.172543 11.00000 -1.50000
H17C 2 0.612495 1.121222 0.188800 11.00000 -1.50000
AFIX 0
N1 3 0.432734 0.450874 0.231172 11.00000 0.05014 0.06362 =
0.04010 0.00471 0.00292 -0.00985
AFIX 43
H1 2 0.366161 0.407257 0.197490 11.00000 -1.20000
AFIX 0
O1 4 0.727551 0.250663 0.636479 11.00000 0.05660 0.11128 =
0.05315 0.01881 0.00422 0.01403
O2 4 0.572850 0.634299 0.231028 11.00000 0.07692 0.07737 =
0.05374 0.00772 0.00308 -0.02791
O3 4 0.416332 0.858213 0.114908 11.00000 0.06801 0.05663 =
0.06945 0.00102 0.03069 0.00201
O4 4 0.589818 0.892306 0.085293 11.00000 0.06795 0.06974 =
0.09047 0.00142 0.03558 -0.00522
HKLF 4
REM bmk2106c in P2(1)/n
REM wR2 = 0.1337, GooF = S = 1.032, Restrained GooF = 1.032 for all data
REM R1 = 0.0427 for 2612 Fo > 4sig(Fo) and 0.0509 for all 3141 data
REM 201 parameters refined using 0 restraints
END
WGHT 0.0761 0.1904
REM Highest difference peak 0.165, deepest hole -0.157, 1-sigma level 0.034
Q1 1 0.5358 1.1725 0.1463 11.00000 0.05 0.16
Q2 1 0.6001 0.4033 0.4800 11.00000 0.05 0.15
Q3 1 0.5031 0.6673 0.2400 11.00000 0.05 0.13
Q4 1 0.7020 0.1559 0.6085 11.00000 0.05 0.12
Q5 1 0.3275 0.2564 0.3019 11.00000 0.05 0.12
Q6 1 0.4337 0.5763 0.1363 11.00000 0.05 0.11
Q7 1 0.4258 0.3285 0.4022 11.00000 0.05 0.11
Q8 1 0.4607 0.1038 0.5933 11.00000 0.05 0.11
Q9 1 0.6456 1.0691 0.2285 11.00000 0.05 0.10
Q10 1 0.4626 0.4257 0.2764 11.00000 0.05 0.10
;
_shelx_res_checksum 58203
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_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
C C1 0.5388(2) 0.1466(3) 0.63141(13) 0.0868(6) Uani d 1 . .
H H1A 0.587598 0.105244 0.689002 0.130 Uiso calc 1 . .
H H1B 0.498487 0.064212 0.591739 0.130 Uiso calc 1 . .
H H1C 0.478372 0.215398 0.638833 0.130 Uiso calc 1 . .
C C2 0.61923(14) 0.23211(19) 0.59205(9) 0.0576(4) Uani d 1 . .
C C3 0.56774(12) 0.29253(17) 0.49855(9) 0.0505(3) Uani d 1 . .
C C4 0.64622(13) 0.36063(19) 0.46058(10) 0.0587(4) Uani d 1 . .
H H4 0.728942 0.370691 0.495050 0.070 Uiso calc 1 . .
C C5 0.60455(13) 0.41363(19) 0.37314(10) 0.0589(4) Uani d 1 . .
H H5 0.658915 0.457351 0.348638 0.071 Uiso calc 1 . .
C C6 0.48068(12) 0.40141(16) 0.32165(8) 0.0490(3) Uani d 1 . .
C C7 0.40109(13) 0.3340(2) 0.35836(10) 0.0624(4) Uani d 1 . .
H H7 0.318208 0.325327 0.324040 0.075 Uiso calc 1 . .
C C8 0.44443(13) 0.2795(2) 0.44606(10) 0.0619(4) Uani d 1 . .
H H8 0.390386 0.233633 0.470096 0.074 Uiso calc 1 . .
C C9 0.48064(13) 0.56038(17) 0.19145(9) 0.0539(3) Uani d 1 . .
C C10 0.41025(12) 0.58347(17) 0.09278(9) 0.0512(3) Uani d 1 . .
C C11 0.38681(13) 0.73080(17) 0.05690(10) 0.0532(3) Uani d 1 . .
C C12 0.32771(14) 0.7548(2) -0.03390(11) 0.0629(4) Uani d 1 . .
H H12 0.311768 0.854402 -0.056485 0.075 Uiso calc 1 . .
C C13 0.29218(15) 0.6303(2) -0.09134(10) 0.0668(4) Uani d 1 . .
H H13 0.252995 0.646157 -0.152872 0.080 Uiso calc 1 . .
C C14 0.31454(15) 0.4827(2) -0.05786(10) 0.0634(4) Uani d 1 . .
H H14 0.291076 0.398867 -0.096645 0.076 Uiso calc 1 . .
C C15 0.37213(14) 0.45989(19) 0.03382(10) 0.0574(4) Uani d 1 . .
H H15 0.385567 0.360130 0.056397 0.069 Uiso calc 1 . .
C C16 0.52387(15) 0.93013(18) 0.12475(11) 0.0606(4) Uani d 1 . .
C C17 0.5436(2) 1.0612(2) 0.18968(14) 0.0858(6) Uani d 1 . .
H H17A 0.559486 1.021628 0.249346 0.129 Uiso calc 1 . .
H H17B 0.471610 1.124674 0.172543 0.129 Uiso calc 1 . .
H H17C 0.612495 1.121222 0.188800 0.129 Uiso calc 1 . .
N N1 0.43273(11) 0.45087(15) 0.23117(7) 0.0547(3) Uani d 1 . .
H H1 0.366161 0.407257 0.197490 0.066 Uiso calc 1 . .
O O1 0.72755(11) 0.25066(17) 0.63648(8) 0.0776(4) Uani d 1 . .
O O2 0.57285(12) 0.63430(15) 0.23103(8) 0.0745(4) Uani d 1 . .
O O3 0.41633(10) 0.85821(13) 0.11491(8) 0.0629(3) Uani d 1 . .
O O4 0.58982(12) 0.89231(15) 0.08529(9) 0.0739(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
C1 0.0814(12) 0.1205(18) 0.0571(9) 0.0023(11) 0.0223(9) 0.0268(10)
C2 0.0559(8) 0.0687(9) 0.0445(7) 0.0146(6) 0.0127(6) 0.0053(6)
C3 0.0473(7) 0.0592(8) 0.0412(6) 0.0072(5) 0.0108(5) 0.0026(5)
C4 0.0424(7) 0.0737(10) 0.0497(7) -0.0019(6) 0.0030(5) 0.0093(6)
C5 0.0461(7) 0.0745(10) 0.0496(7) -0.0079(6) 0.0087(6) 0.0102(6)
C6 0.0478(7) 0.0533(7) 0.0391(6) -0.0021(5) 0.0067(5) 0.0010(5)
C7 0.0422(7) 0.0892(11) 0.0470(7) -0.0061(7) 0.0045(5) 0.0094(7)
C8 0.0470(7) 0.0872(11) 0.0497(7) -0.0017(7) 0.0146(6) 0.0110(7)
C9 0.0555(7) 0.0560(8) 0.0444(7) -0.0038(6) 0.0101(6) 0.0016(5)
C10 0.0477(7) 0.0579(8) 0.0452(7) -0.0002(5) 0.0127(5) 0.0061(6)
C11 0.0479(7) 0.0588(8) 0.0545(7) 0.0020(6) 0.0198(6) 0.0055(6)
C12 0.0563(8) 0.0691(10) 0.0619(9) 0.0089(7) 0.0190(7) 0.0216(7)
C13 0.0589(8) 0.0881(12) 0.0467(7) -0.0016(8) 0.0102(6) 0.0154(7)
C14 0.0633(9) 0.0749(10) 0.0465(7) -0.0083(7) 0.0122(6) -0.0003(7)
C15 0.0595(8) 0.0576(8) 0.0495(7) -0.0028(6) 0.0118(6) 0.0045(6)
C16 0.0676(9) 0.0522(8) 0.0618(8) 0.0008(6) 0.0223(7) 0.0114(6)
C17 0.1228(17) 0.0633(10) 0.0751(12) -0.0140(11) 0.0391(12) -0.0023(9)
N1 0.0501(6) 0.0636(7) 0.0401(6) -0.0099(5) 0.0029(4) 0.0047(5)
O1 0.0566(7) 0.1113(11) 0.0531(6) 0.0140(6) 0.0042(5) 0.0188(6)
O2 0.0769(8) 0.0774(8) 0.0537(6) -0.0279(6) 0.0031(5) 0.0077(5)
O3 0.0680(7) 0.0566(6) 0.0695(7) 0.0020(5) 0.0307(5) 0.0010(5)
O4 0.0680(7) 0.0697(8) 0.0905(9) -0.0052(5) 0.0356(7) 0.0014(6)
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'
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
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
O1 C2 C3 . . 120.27(15) ?
O1 C2 C1 . . 119.83(14) ?
C3 C2 C1 . . 119.89(14) ?
C4 C3 C8 . . 118.28(12) ?
C4 C3 C2 . . 118.95(13) ?
C8 C3 C2 . . 122.74(14) ?
C5 C4 C3 . . 121.56(13) ?
C5 C4 H4 . . 119.2 ?
C3 C4 H4 . . 119.2 ?
C4 C5 C6 . . 119.58(14) ?
C4 C5 H5 . . 120.2 ?
C6 C5 H5 . . 120.2 ?
C7 C6 C5 . . 119.67(13) ?
C7 C6 N1 . . 118.01(12) ?
C5 C6 N1 . . 122.28(13) ?
C6 C7 C8 . . 120.17(13) ?
C6 C7 H7 . . 119.9 ?
C8 C7 H7 . . 119.9 ?
C7 C8 C3 . . 120.73(14) ?
C7 C8 H8 . . 119.6 ?
C3 C8 H8 . . 119.6 ?
O2 C9 N1 . . 124.00(13) ?
O2 C9 C10 . . 121.78(13) ?
N1 C9 C10 . . 114.22(12) ?
C11 C10 C15 . . 117.84(13) ?
C11 C10 C9 . . 120.41(13) ?
C15 C10 C9 . . 121.66(13) ?
C12 C11 C10 . . 121.50(14) ?
C12 C11 O3 . . 118.87(14) ?
C10 C11 O3 . . 119.49(12) ?
C11 C12 C13 . . 119.64(15) ?
C11 C12 H12 . . 120.2 ?
C13 C12 H12 . . 120.2 ?
C14 C13 C12 . . 120.25(14) ?
C14 C13 H13 . . 119.9 ?
C12 C13 H13 . . 119.9 ?
C13 C14 C15 . . 119.59(15) ?
C13 C14 H14 . . 120.2 ?
C15 C14 H14 . . 120.2 ?
C14 C15 C10 . . 121.16(15) ?
C14 C15 H15 . . 119.4 ?
C10 C15 H15 . . 119.4 ?
O4 C16 O3 . . 123.25(16) ?
O4 C16 C17 . . 126.61(17) ?
O3 C16 C17 . . 110.13(15) ?
C16 C17 H17A . . 109.5 ?
C16 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C16 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C9 N1 C6 . . 126.92(12) ?
C9 N1 H1 . . 116.5 ?
C6 N1 H1 . . 116.5 ?
C16 O3 C11 . . 116.38(12) ?
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
C1 C2 . 1.490(3) ?
C1 H1A . 0.9600 ?
C1 H1B . 0.9600 ?
C1 H1C . 0.9600 ?
C2 O1 . 1.221(2) ?
C2 C3 . 1.4848(18) ?
C3 C4 . 1.388(2) ?
C3 C8 . 1.3890(19) ?
C4 C5 . 1.3759(19) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.3902(19) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.382(2) ?
C6 N1 . 1.4101(16) ?
C7 C8 . 1.384(2) ?
C7 H7 . 0.9300 ?
C8 H8 . 0.9300 ?
C9 O2 . 1.2194(18) ?
C9 N1 . 1.3619(19) ?
C9 C10 . 1.5022(18) ?
C10 C11 . 1.389(2) ?
C10 C15 . 1.390(2) ?
C11 C12 . 1.375(2) ?
C11 O3 . 1.4024(18) ?
C12 C13 . 1.380(3) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.378(2) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.384(2) ?
C14 H14 . 0.9300 ?
C15 H15 . 0.9300 ?
C16 O4 . 1.191(2) ?
C16 O3 . 1.358(2) ?
C16 C17 . 1.497(3) ?
C17 H17A . 0.9600 ?
C17 H17B . 0.9600 ?
C17 H17C . 0.9600 ?
N1 H1 . 0.8600 ?
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
C5 H5 O2 . 0.93 2.35 2.8792(19) 115.7 yes
C12 H12 O4 3_675 0.93 2.59 3.396(2) 144.7 yes
N1 H1 O1 4_565 0.86 2.08 2.9181(16) 164.3 yes
C8 H8 Cg1 2_545 0.93 3.20 4.0960(15) 163.8 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
O1 C2 C3 C4 . . . . 4.4(2) ?
C1 C2 C3 C4 . . . . -174.76(17) ?
O1 C2 C3 C8 . . . . -177.69(16) ?
C1 C2 C3 C8 . . . . 3.1(2) ?
C8 C3 C4 C5 . . . . -0.4(2) ?
C2 C3 C4 C5 . . . . 177.60(15) ?
C3 C4 C5 C6 . . . . 1.1(3) ?
C4 C5 C6 C7 . . . . -1.0(2) ?
C4 C5 C6 N1 . . . . -178.77(15) ?
C5 C6 C7 C8 . . . . 0.2(3) ?
N1 C6 C7 C8 . . . . 178.10(15) ?
C6 C7 C8 C3 . . . . 0.5(3) ?
C4 C3 C8 C7 . . . . -0.4(3) ?
C2 C3 C8 C7 . . . . -178.31(16) ?
O2 C9 C10 C11 . . . . -43.7(2) ?
N1 C9 C10 C11 . . . . 136.62(15) ?
O2 C9 C10 C15 . . . . 132.97(18) ?
N1 C9 C10 C15 . . . . -46.7(2) ?
C15 C10 C11 C12 . . . . 0.1(2) ?
C9 C10 C11 C12 . . . . 176.85(13) ?
C15 C10 C11 O3 . . . . 175.68(13) ?
C9 C10 C11 O3 . . . . -7.6(2) ?
C10 C11 C12 C13 . . . . -1.0(2) ?
O3 C11 C12 C13 . . . . -176.59(14) ?
C11 C12 C13 C14 . . . . 0.7(2) ?
C12 C13 C14 C15 . . . . 0.4(3) ?
C13 C14 C15 C10 . . . . -1.3(2) ?
C11 C10 C15 C14 . . . . 1.1(2) ?
C9 C10 C15 C14 . . . . -175.65(14) ?
O2 C9 N1 C6 . . . . -1.7(3) ?
C10 C9 N1 C6 . . . . 178.01(13) ?
C7 C6 N1 C9 . . . . 156.85(16) ?
C5 C6 N1 C9 . . . . -25.3(2) ?
O4 C16 O3 C11 . . . . 2.0(2) ?
C17 C16 O3 C11 . . . . -178.92(13) ?
C12 C11 O3 C16 . . . . -85.66(17) ?
C10 C11 O3 C16 . . . . 98.63(16) ?