#------------------------------------------------------------------------------
#$Date: 2023-03-16 05:29:02 +0200 (Thu, 16 Mar 2023) $
#$Revision: 281913 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/42/2244245.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_2244245
loop_
_publ_author_name
'Mohamed-Ezzat, Reham A.'
'Kariuki, Benson M.'
'Azzam, Rasha A.'
_publ_section_title
;
Synthesis and crystal structure of
N-(5-acetyl-4-methylpyrimidin-2-yl)benzenesulfonamide
;
_journal_coeditor_code YZ2029
_journal_issue 4
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989023001871
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C13 H13 N3 O3 S'
_chemical_formula_moiety 'C13 H13 N3 O3 S'
_chemical_formula_sum 'C13 H13 N3 O3 S'
_chemical_formula_weight 291.32
_chemical_name_systematic
;
N-(5-Acetyl-4-methylpyrimidin-2-yl)benzenesulfonamide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method SHELXL-2018/1
_cell_angle_alpha 90
_cell_angle_beta 113.900(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.0699(6)
_cell_length_b 14.7429(6)
_cell_length_c 10.5212(7)
_cell_measurement_reflns_used 5035
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.6630
_cell_measurement_theta_min 3.8650
_cell_volume 1428.04(16)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020), ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
Mercury (Macrae et al., 2020)
;
_computing_structure_refinement
;
SHELXL2018/1 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type
'Rigaku SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0260
_diffrn_reflns_av_unetI/netI 0.0277
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 12642
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.537
_diffrn_reflns_theta_min 3.482
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.237
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.484
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.355
_exptl_crystal_description block
_exptl_crystal_F_000 608
_exptl_crystal_size_max 0.440
_exptl_crystal_size_mid 0.240
_exptl_crystal_size_min 0.160
_refine_diff_density_max 0.230
_refine_diff_density_min -0.294
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 216
_refine_ls_number_reflns 3532
_refine_ls_number_restraints 84
_refine_ls_restrained_S_all 1.074
_refine_ls_R_factor_all 0.0689
_refine_ls_R_factor_gt 0.0459
_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^)+(0.0493P)^2^+0.4200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1093
_refine_ls_wR_factor_ref 0.1251
_reflns_number_gt 2548
_reflns_number_total 3532
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2029sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2244245
_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 0.903
_shelx_estimated_absorpt_t_max 0.963
_shelx_hkl_file
;
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-11 3 8 733.965 174.316 3
-11 -3 8 645.088 149.402 3
-11 -3 7 101.171 72.8672 3
-11 3 7-1.71553 71.2916 3
-11 -3 6 115.268 83.2707 3
-11 3 6 86.3493 93.3803 3
-11 -3 5 1029.36 185.404 3
-11 3 5 929.997 192.793 3
-11 -3 4 17.7219 60.9530 3
-11 3 4-151.956 90.8211 3
-11 -3 3 157.571 107.050 3
-11 3 3-107.142 94.0232 3
-11 -3 2 753.373 173.555 3
-11 3 2 786.092 199.893 3
-11 -3 1 508.600 155.886 3
-11 3 1 638.537 175.270 3
-11 -3 0 338.397 145.813 1
-11 3 0 319.406 122.780 3
-11 -3 -1 452.982 155.197 1
-11 -4 11 42.1592 68.9999 3
-11 4 10 78.7341 79.3106 3
-11 -4 10 51.8585 79.3685 3
-11 4 9 156.992 125.116 3
-11 -4 9 84.8322 89.3879 3
-11 -4 8 73.5594 73.4113 3
-11 4 8 134.741 111.127 3
-11 -4 7 236.449 105.470 3
-11 4 7 210.183 104.880 3
-11 -4 6 329.209 108.060 3
-11 4 6 176.033 93.8286 3
-11 -4 5 183.384 85.7411 3
-11 4 5 371.537 142.553 3
-11 -4 4-51.5707 82.3476 3
-11 4 4 17.6829 67.0124 3
-11 -4 3 645.589 122.210 2
-11 -4 3 629.590 155.638 3
-11 4 3 548.756 162.094 3
-11 -4 2 52.8975 66.2818 3
-11 4 2 5.86588 66.4387 3
-11 -4 1 271.430 122.216 1
-11 -4 1 385.658 125.286 3
-11 4 1 328.034 131.553 3
-11 -4 0 1265.86 220.828 1
-11 4 0 1397.36 274.765 3
-11 -4 -1 270.611 116.199 1
-11 -5 11-116.374 93.3822 3
-11 -5 10 1999.24 273.267 3
-11 5 9-21.6777 86.6953 3
-11 -5 9 280.134 121.155 3
-11 -5 8 1427.12 221.391 3
-11 5 8 1297.12 248.905 3
-11 -5 7 255.770 99.5583 3
-11 5 7 455.375 149.937 3
-11 -5 6 851.306 165.017 3
-11 5 6 1026.59 205.120 3
-11 -5 5-91.7282 74.4829 3
-11 5 5-6.57504 95.7829 3
-11 -5 4 278.713 107.514 3
-11 5 4 283.663 128.836 3
-11 -5 3 66.7966 63.3267 2
-11 -5 3-21.6878 59.5584 3
-11 5 3-30.9944 75.9761 3
-11 -5 2 402.032 134.064 3
-11 5 2 482.935 159.491 3
-11 -5 1 411.262 130.620 1
-11 5 1 275.470 125.136 3
-11 -5 0 332.309 133.250 1
-11 5 0-29.3703 78.8972 3
-11 -5 -1-5.81499 70.1320 1
-11 -6 11-14.8176 69.4150 3
-11 -6 10 37.2050 64.3734 3
-11 6 9 231.030 125.961 3
-11 -6 9-71.8367 75.1511 3
-11 -6 8-53.9241 80.8890 3
-11 6 8-123.392 100.355 3
-11 -6 7 186.270 68.6630 3
-11 6 7 465.666 158.401 3
-11 -6 6 900.177 166.189 3
-11 6 6 967.354 198.911 3
-11 -6 5-19.0134 74.6938 3
-11 6 5-89.5138 68.4006 3
-11 -6 4 174.004 80.3421 2
-11 -6 4 174.594 85.2716 3
-11 6 4 131.593 92.5312 3
-11 -6 3 78.9178 65.7336 2
-11 -6 3-45.9945 56.6096 3
-11 -6 2 650.115 155.766 3
-11 6 2 958.832 223.471 3
-11 -6 1 63.8613 86.1331 1
-11 6 1-32.2409 70.5300 3
-11 -6 0 33.1242 84.2822 1
-11 -6 -1-79.5085 97.3960 1
-11 -7 11 242.028 112.712 3
-11 -7 10 121.402 88.5948 3
-11 -7 9 132.744 79.9293 3
-11 -7 8 1144.94 189.153 3
-11 7 8 1060.20 222.513 3
-11 7 7 246.922 136.232 3
-11 -7 7 449.308 124.380 3
-11 -7 6-63.0566 74.3239 3
-11 7 6-90.2254 109.110 3
-11 -7 5 661.495 154.346 2
-11 -7 5 756.936 151.952 3
-11 7 5 1054.31 221.916 3
-11 -7 4 27.7710 64.7213 2
-11 -7 4 60.9703 71.4263 3
-11 7 4 88.7445 87.5346 3
-11 -7 3 410.466 112.605 2
-11 -7 3 211.342 91.0691 3
-11 7 3 280.494 135.057 3
-11 -7 2-31.9141 66.0424 1
-11 7 2 95.2820 106.022 3
-11 -7 1 178.039 106.251 1
-11 7 1 81.7410 120.649 3
-11 -7 0 40.8530 77.3774 1
-11 -7 -1 289.755 116.095 1
-11 -8 7 397.405 123.593 2
-11 8 7 344.622 139.991 3
-11 -8 7 509.181 124.533 3
-11 -8 6 21.3680 67.6539 2
-11 -8 6 46.0430 54.9294 3
-11 8 6 183.572 97.9786 3
-11 -8 5 546.982 139.470 2
-11 -8 5 517.818 127.547 3
-11 8 5 436.880 155.133 3
-11 -8 4-111.371 79.4790 2
-11 8 4-183.349 123.342 3
-11 -8 3 744.220 146.499 2
-11 8 3 919.772 231.387 3
-11 -8 2 204.301 100.242 1
-11 8 2 94.0053 109.245 3
-11 -8 1 393.803 134.477 1
-11 -8 0 59.7520 75.2839 1
-11 -8 -1 235.800 108.369 1
-11 -9 8 500.956 145.871 2
-11 -9 7 120.766 96.7381 2
-11 -9 6 63.9585 92.4727 2
-11 9 6-74.3850 129.400 3
-11 -9 5 158.353 98.1958 2
-11 9 5-134.506 127.178 3
-11 -9 4 641.116 151.234 2
-11 9 4 1170.84 255.789 3
-11 -9 3-55.0666 63.7763 1
-11 -9 3 226.204 89.4342 2
-11 -9 2 1669.84 226.642 1
-11 -9 1 111.610 79.6155 1
-11 -9 0-14.0707 55.8506 1
-11 -9 -1 108.059 108.579 1
-11 -10 7 257.492 128.078 2
-11 -10 6 523.041 158.640 2
-11 -10 5 207.513 104.184 2
-11 -10 4 187.763 96.6839 2
-11 -10 3 212.940 92.4426 2
-11 -11 6 1164.87 219.018 2
-11 -11 5 157.268 100.141 2
-11 -11 4-166.949 93.6862 2
-11 -12 5-32.2717 66.4417 2
-11 -12 4 323.074 121.443 2
-12 0 9 48.7603 86.9013 3
-12 0 8 3384.02 375.806 3
-12 0 7-43.3660 76.5075 3
-12 0 6 300.592 122.552 3
-12 0 5-343.064 135.825 3
-12 0 4 83.1461 94.3867 3
-12 0 3 181.400 126.710 3
-12 0 2 146.373 91.9599 3
-12 0 1-33.6256 60.1643 3
-12 -1 10 476.625 161.841 3
-12 -1 9 185.945 124.874 3
-12 1 9 319.418 140.153 3
-12 -1 8 476.925 161.103 3
-12 1 8 464.248 159.887 3
-12 1 7 1260.46 230.496 3
-12 -1 7 890.963 193.547 3
-12 -1 6 191.365 103.892 3
-12 1 6 421.269 132.382 3
-12 -1 5-5.21285 52.9129 3
-12 1 5-91.1924 73.4866 3
-12 -1 4-220.600 116.257 3
-12 1 4 21.2084 75.3129 3
-12 -1 3 167.627 110.302 3
-12 1 3 309.131 126.697 3
-12 -1 2 118.692 90.4014 3
-12 1 2-32.3216 85.6206 3
-12 -1 1-13.0248 68.4802 3
-12 1 1 186.238 103.667 3
-12 -2 10 63.7555 90.2514 3
-12 -2 9 699.271 178.704 3
-12 2 9 552.910 183.383 3
-12 -2 8 168.194 106.201 3
-12 2 8 282.024 125.202 3
-12 2 7 1250.23 232.407 3
-12 -2 7 1248.27 223.361 3
-12 -2 6-27.5092 65.7211 3
-12 2 6 91.7228 99.1177 3
-12 -2 5 765.346 176.391 3
-12 2 5 475.890 147.449 3
-12 -2 4 23.9094 78.7129 3
-12 2 4-307.226 131.198 3
-12 -2 3 1361.99 244.353 3
-12 2 3 788.808 203.155 3
-12 -2 2-100.040 77.4443 3
-12 2 2-11.2816 67.1399 3
-12 -2 1 569.465 158.390 1
-12 -2 1 205.836 105.488 3
-12 2 1 606.490 186.300 3
-12 -3 10 392.211 137.215 3
-12 -3 9 1418.85 242.200 3
-12 -3 8 63.5904 100.866 3
-12 3 8-225.479 117.651 3
-12 -3 7 660.324 159.467 3
-12 3 7 437.701 155.837 3
-12 -3 6 296.111 109.304 3
-12 3 6 533.885 159.887 3
-12 -3 5 335.623 127.635 3
-12 3 5 400.605 142.427 3
-12 -3 4 73.9804 81.8209 3
-12 3 4-1.97039 56.5532 3
-12 -3 3 164.750 100.403 3
-12 3 3-61.1261 78.1232 3
-12 -3 2-9.30073 78.3722 3
-12 3 2 25.3047 75.1555 3
-12 -3 1 267.036 123.094 1
-12 -4 10 205.738 106.609 3
-12 -4 9-36.1603 69.1199 3
-12 -4 8 81.2775 91.0748 3
-12 -4 7 651.761 159.693 3
-12 4 7 420.850 132.121 3
-12 -4 6-15.4601 86.7621 3
-12 4 6-61.9387 79.5994 3
-12 -4 5 809.985 173.840 3
-12 4 5 671.872 184.340 3
-12 -4 4 151.070 81.3726 3
-12 4 4-142.241 102.161 3
-12 -4 3 95.0133 82.2780 3
-12 4 3 28.8960 92.1712 3
-12 -4 2 815.218 182.941 3
-12 -4 1 119.765 93.6268 1
-12 -5 10 157.887 116.052 3
-12 -5 9 56.0893 74.3065 3
-12 -5 8 338.984 109.706 3
-12 -5 7 168.150 79.5694 3
-12 5 7 272.654 124.478 3
-12 -5 6 953.272 187.743 3
-12 5 6 1049.76 219.063 3
-12 -5 5-73.7688 70.8939 3
-12 5 5-36.4092 81.3907 3
-12 -5 4 64.9147 66.3754 2
-12 -5 4 176.844 94.6860 3
-12 5 4 166.112 112.440 3
-12 -5 3 46.0224 71.2106 3
-12 -5 2-97.6049 93.1843 3
-12 -5 1 547.984 168.646 1
-12 -6 10-46.0262 75.9527 3
-12 -6 9 288.372 117.664 3
-12 -6 8 28.2979 58.2906 3
-12 -6 7 425.364 115.404 3
-12 -6 6 133.497 81.3501 3
-12 -6 5 7.94402 46.8017 2
-12 -6 5 77.4780 72.1284 3
-12 -6 4 301.046 111.743 3
-12 -6 3 275.762 100.689 3
-12 -6 2 146.996 91.7746 1
-12 -6 1-147.939 103.287 1
-12 -7 7-137.675 73.1014 3
-12 -7 6 52.5028 75.8651 2
-12 -7 6 145.117 81.1940 3
-12 -7 5 171.358 91.7516 2
-12 -7 5-18.8170 50.9218 3
-12 -7 2-40.7134 75.1314 1
-12 -7 1 165.632 105.245 1
-12 -8 7 461.215 145.656 2
-12 -8 6-53.9943 64.9157 2
-12 -8 5 2566.63 299.574 2
-12 -8 3 215.057 97.0648 1
-12 -8 2-0.52264 66.1743 1
-12 -8 1 460.833 141.728 1
-12 -9 6 227.816 134.376 2
-12 -9 5-7.63139 77.2193 2
-12 -10 6 56.1002 76.1546 2
-12 -10 5-229.300 111.378 2
-13 0 7 216.612 122.690 3
-13 0 6 405.411 148.258 3
-13 0 5-260.739 122.559 3
-13 0 4 912.394 211.445 3
-13 -1 7 550.404 151.821 3
-13 -1 6 80.3730 86.4447 3
-13 -1 5-318.751 156.024 3
-13 -1 4-120.852 92.7244 3
-13 -1 3-78.7523 84.7301 3
-13 -2 8 748.630 181.604 3
-13 -2 7 928.771 209.964 3
-13 -2 6 269.956 121.506 3
-13 -2 5 548.332 159.229 3
-13 -2 4-87.5404 84.3736 3
-13 -2 3 413.931 162.704 3
-13 -3 8 30.8032 67.5409 3
-13 -3 7-34.7386 59.4237 3
-13 -3 6-61.9464 71.5941 3
-13 -3 5 346.149 133.498 3
-13 -3 4 36.4072 74.9194 3
-13 -3 3-144.022 91.7544 3
-13 -3 2 116.883 87.6245 3
-13 -4 9 26.5366 72.2940 3
-13 -4 8 767.334 169.998 3
-13 -4 7 184.744 106.091 3
-13 -4 6 181.111 108.391 3
-13 -4 5 39.7585 71.5839 3
-13 -4 4-176.437 108.903 3
-13 -4 3 663.295 173.473 3
-13 -4 2 560.434 163.294 3
-13 -5 9-237.247 107.188 3
-13 -5 8 230.611 111.952 3
-13 -5 7-4.69211 48.2706 3
-13 -5 6 112.266 78.5357 3
-13 -5 5-128.712 92.7402 3
-13 -5 4 282.408 132.694 3
-13 -5 3 327.435 140.681 3
-13 -7 7 41.5189 64.3737 2
0 0 0 0.00 0.00 0
TITL bmk2287_auto in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 10.069945 14.742907 10.521240 90.0000 113.9003 90.0000
ZERR 4.00 0.000640 0.000588 0.000665 0.0000 0.0075 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 52.00 92.00 8.00 8.00
SIZE 0.16 0.24 0.44
TREF
HKLF 4
END
;
_shelx_hkl_checksum 99988
_shelx_res_file
;
TITL bmk2287 in P2(1)/c
shelx.res
created by SHELXL-2018/1 at 11:17:12 on 21-Feb-2023
CELL 0.71073 10.0699 14.7429 10.5212 90.000 113.900 90.000
ZERR 4.00 0.0006 0.0006 0.0007 0.000 0.007 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H N O S
UNIT 52 52 12 12 4
MERG 2
simu .01 c12 > o3a
eadp c9 c9a
exyz c9 c9a
EQIV $1 -x+1, -y+1, -z+1
HTAB N1 N3_$1
EQIV $2 x, -y+3/2, z+1/2
HTAB C6 O2_$2
HTAB C10 O1_$1
HTAB C11 O3A
EQIV $3 -x+1, y-1/2, -z+1/2
HTAB C13A O1_$3
HTAB N1 N3_$1
MPLA C7 C8 C9 C10 N2 N3
MPLA C1 C2 C3 C4 C5 C6
MPLA C9 C12 C13 O3
MPLA C9 C12A C13A O3A
FMAP 2
PLAN 10
SIZE 0.160 0.240 0.440
ACTA
BOND $H
LIST 4
L.S. 4
WGHT 0.049300 0.420000
FVAR 5.04568 0.59114
C1 1 0.522950 0.751916 0.268872 11.00000 0.05571 0.04559 =
0.04026 0.00816 0.02276 0.00557
C2 1 0.620477 0.762912 0.208593 11.00000 0.06194 0.05585 =
0.05508 0.00700 0.03107 0.00622
AFIX 43
H2 2 0.630570 0.718727 0.150041 11.00000 -1.20000
AFIX 0
C3 1 0.703324 0.841549 0.237372 11.00000 0.05665 0.06762 =
0.07602 0.01829 0.03205 0.00151
AFIX 43
H3 2 0.768869 0.850929 0.196825 11.00000 -1.20000
AFIX 0
C4 1 0.688570 0.905504 0.325673 11.00000 0.06953 0.05111 =
0.07889 0.00801 0.01566 -0.00264
AFIX 43
H4 2 0.746248 0.957279 0.346473 11.00000 -1.20000
AFIX 0
C5 1 0.590078 0.893929 0.383338 11.00000 0.08967 0.05348 =
0.06338 -0.00428 0.02872 0.00507
AFIX 43
H5 2 0.579890 0.938259 0.441639 11.00000 -1.20000
AFIX 0
C6 1 0.506480 0.817316 0.355507 11.00000 0.07544 0.05516 =
0.05096 0.00405 0.03348 0.00892
AFIX 43
H6 2 0.439261 0.809307 0.394462 11.00000 -1.20000
AFIX 0
C7 1 0.618639 0.527959 0.371440 11.00000 0.04686 0.05179 =
0.04326 0.00427 0.02146 0.00031
C8 1 0.800193 0.490888 0.304466 11.00000 0.04909 0.08039 =
0.04977 0.00122 0.02585 -0.00139
C10 1 0.756445 0.407224 0.475212 11.00000 0.05145 0.06319 =
0.05699 0.01327 0.02331 0.01090
AFIX 43
H10 2 0.780068 0.359996 0.539203 11.00000 -1.20000
AFIX 0
C11 1 0.876669 0.514088 0.212315 11.00000 0.06907 0.12541 =
0.07378 0.01683 0.04720 0.00896
AFIX 137
H11A 2 0.853870 0.469409 0.140165 11.00000 -1.50000
H11B 2 0.979663 0.514976 0.266457 11.00000 -1.50000
H11C 2 0.845364 0.572710 0.171410 11.00000 -1.50000
AFIX 0
N1 3 0.502915 0.581917 0.359380 11.00000 0.05949 0.05142 =
0.05211 0.01411 0.03360 0.00929
N2 3 0.690698 0.546378 0.292913 11.00000 0.05498 0.06346 =
0.04995 0.00717 0.02890 -0.00012
N3 3 0.647280 0.461517 0.465328 11.00000 0.05059 0.05578 =
0.04815 0.01116 0.02588 0.00805
O1 4 0.288211 0.674144 0.258396 11.00000 0.05425 0.07535 =
0.07326 0.02333 0.03309 0.01338
O2 4 0.398849 0.618586 0.103160 11.00000 0.07924 0.05953 =
0.04566 0.00197 0.02345 -0.00600
S1 5 0.414671 0.654186 0.234209 11.00000 0.05462 0.05061 =
0.04646 0.00978 0.02442 0.00424
PART 1
C9 1 0.836696 0.416472 0.396773 21.00000 0.04659 0.07983 =
0.05770 0.00686 0.02541 0.01016
C12 1 0.941987 0.343238 0.399000 21.00000 0.04471 0.10055 =
0.08392 0.00570 0.03038 0.01111
C13 1 0.985964 0.275622 0.515016 21.00000 0.08143 0.09751 =
0.09360 0.01569 0.01193 0.04792
AFIX 137
H13A 2 1.053800 0.233375 0.505298 21.00000 -1.50000
H13B 2 0.901665 0.243536 0.511702 21.00000 -1.50000
H13C 2 1.030623 0.306600 0.602434 21.00000 -1.50000
AFIX 0
O3 4 0.993052 0.339707 0.312804 21.00000 0.09595 0.12807 =
0.14423 0.01694 0.08733 0.03664
PART 2
same .005 c9 > o3
C9A 1 0.836696 0.416472 0.396773 -21.00000 0.04659 0.07983 =
0.05770 0.00686 0.02541 0.01016
C12A 1 0.972714 0.362047 0.430572 -21.00000 0.05425 0.10451 =
0.07712 0.00130 0.02546 0.02512
C13A 1 0.989717 0.275048 0.508607 -21.00000 0.07226 0.10710 =
0.08637 -0.00735 0.03204 0.02517
AFIX 137
H13D 2 1.082486 0.248722 0.525215 -21.00000 -1.50000
H13E 2 0.913988 0.233796 0.454891 -21.00000 -1.50000
H13F 2 0.983594 0.286757 0.595831 -21.00000 -1.50000
AFIX 0
O3A 4 1.061637 0.385705 0.387614 -21.00000 0.06964 0.14375 =
0.12684 0.00949 0.06223 0.02551
PART 0
H1 2 0.458406 0.569996 0.408894 11.00000 0.05439
HKLF 4
REM bmk2287 in P2(1)/c
REM R1 = 0.0459 for 2548 Fo > 4sig(Fo) and 0.0689 for all 3532 data
REM 216 parameters refined using 84 restraints
END
WGHT 0.0494 0.4191
REM Highest difference peak 0.230, deepest hole -0.294, 1-sigma level 0.038
Q1 1 0.4680 0.7124 0.2539 11.00000 0.05 0.23
Q2 1 0.8489 0.4642 0.3715 11.00000 0.05 0.16
Q3 1 0.8001 0.4357 0.3230 11.00000 0.05 0.15
Q4 1 0.6251 0.4827 0.4157 11.00000 0.05 0.14
Q5 1 0.5408 0.7547 0.2216 11.00000 0.05 0.14
Q6 1 0.6940 0.5996 0.2843 11.00000 0.05 0.14
Q7 1 0.8981 0.4019 0.4090 11.00000 0.05 0.14
Q8 1 0.6093 0.9050 0.3137 11.00000 0.05 0.14
Q9 1 0.6524 0.5042 0.4673 11.00000 0.05 0.14
Q10 1 0.5771 0.4431 0.4803 11.00000 0.05 0.13
;
_shelx_res_checksum 10368
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.5229(2) 0.75192(12) 0.26887(19) 0.0461(4) Uani d 1 . .
C C2 0.6205(2) 0.76291(14) 0.2086(2) 0.0552(5) Uani d 1 . .
H H2 0.630570 0.718727 0.150041 0.066 Uiso calc 1 . .
C C3 0.7033(2) 0.84155(15) 0.2374(3) 0.0651(6) Uani d 1 . .
H H3 0.768869 0.850929 0.196825 0.078 Uiso calc 1 . .
C C4 0.6886(3) 0.90550(15) 0.3257(3) 0.0712(7) Uani d 1 . .
H H4 0.746248 0.957279 0.346473 0.085 Uiso calc 1 . .
C C5 0.5901(3) 0.89393(15) 0.3833(2) 0.0696(6) Uani d 1 . .
H H5 0.579890 0.938259 0.441639 0.083 Uiso calc 1 . .
C C6 0.5065(3) 0.81732(14) 0.3555(2) 0.0580(5) Uani d 1 . .
H H6 0.439261 0.809307 0.394462 0.070 Uiso calc 1 . .
C C7 0.6186(2) 0.52796(12) 0.37144(19) 0.0463(4) Uani d 1 . .
C C8 0.8002(2) 0.49089(16) 0.3045(2) 0.0579(5) Uani d 1 . .
C C10 0.7564(2) 0.40722(14) 0.4752(2) 0.0568(5) Uani d 1 . .
H H10 0.780068 0.359996 0.539203 0.068 Uiso calc 1 A 1
C C11 0.8767(3) 0.5141(2) 0.2123(3) 0.0835(8) Uani d 1 . .
H H11A 0.853870 0.469409 0.140165 0.125 Uiso calc 1 . .
H H11B 0.979663 0.514976 0.266457 0.125 Uiso calc 1 . .
H H11C 0.845364 0.572710 0.171410 0.125 Uiso calc 1 . .
N N1 0.50291(19) 0.58192(11) 0.35938(18) 0.0508(4) Uani d 1 . .
N N2 0.69070(18) 0.54638(11) 0.29291(17) 0.0537(4) Uani d 1 . .
N N3 0.64728(17) 0.46152(10) 0.46533(16) 0.0496(4) Uani d 1 . .
O O1 0.28821(16) 0.67414(10) 0.25840(16) 0.0653(4) Uani d 1 . .
O O2 0.39885(17) 0.61859(10) 0.10316(14) 0.0621(4) Uani d 1 . .
S S1 0.41467(5) 0.65419(3) 0.23421(5) 0.04929(17) Uani d 1 . .
C C9 0.8367(2) 0.41647(16) 0.3968(2) 0.0600(5) Uani d 0.591(11) B 1
C C12 0.9420(7) 0.3432(4) 0.3990(8) 0.0750(19) Uani d 0.591(11) B 1
C C13 0.9860(17) 0.2756(10) 0.5150(18) 0.098(4) Uani d 0.591(11) B 1
H H13A 1.053800 0.233375 0.505298 0.148 Uiso calc 0.591(11) B 1
H H13B 0.901665 0.243536 0.511702 0.148 Uiso calc 0.591(11) B 1
H H13C 1.030623 0.306600 0.602434 0.148 Uiso calc 0.591(11) B 1
O O3 0.9931(8) 0.3397(4) 0.3128(8) 0.110(2) Uani d 0.591(11) B 1
C C9A 0.8367(2) 0.41647(16) 0.3968(2) 0.0600(5) Uani d 0.409(11) B 2
C C12A 0.9727(9) 0.3620(7) 0.4306(12) 0.079(3) Uani d 0.409(11) B 2
C C13A 0.990(2) 0.2750(12) 0.509(3) 0.089(4) Uani d 0.409(11) B 2
H H13D 1.082486 0.248722 0.525215 0.133 Uiso calc 0.409(11) B 2
H H13E 0.913988 0.233796 0.454891 0.133 Uiso calc 0.409(11) B 2
H H13F 0.983594 0.286757 0.595831 0.133 Uiso calc 0.409(11) B 2
O O3A 1.0616(8) 0.3857(7) 0.3876(10) 0.106(3) Uani d 0.409(11) B 2
H H1 0.458(2) 0.5700(14) 0.409(2) 0.054(6) 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
C1 0.0557(11) 0.0456(9) 0.0403(10) 0.0056(8) 0.0228(9) 0.0082(7)
C2 0.0619(13) 0.0559(11) 0.0551(12) 0.0062(9) 0.0311(10) 0.0070(9)
C3 0.0567(13) 0.0676(14) 0.0760(16) 0.0015(10) 0.0320(12) 0.0183(11)
C4 0.0695(15) 0.0511(12) 0.0789(17) -0.0026(10) 0.0157(13) 0.0080(11)
C5 0.0897(18) 0.0535(12) 0.0634(14) 0.0051(11) 0.0287(13) -0.0043(10)
C6 0.0754(15) 0.0552(11) 0.0510(12) 0.0089(10) 0.0335(11) 0.0040(9)
C7 0.0469(11) 0.0518(10) 0.0433(10) 0.0003(8) 0.0215(9) 0.0043(7)
C8 0.0491(12) 0.0804(14) 0.0498(12) -0.0014(10) 0.0258(10) 0.0012(10)
C10 0.0515(12) 0.0632(12) 0.0570(12) 0.0109(9) 0.0233(10) 0.0133(9)
C11 0.0691(16) 0.125(2) 0.0738(17) 0.0090(15) 0.0472(14) 0.0168(15)
N1 0.0595(10) 0.0514(9) 0.0521(10) 0.0093(7) 0.0336(8) 0.0141(7)
N2 0.0550(10) 0.0635(10) 0.0499(10) -0.0001(8) 0.0289(8) 0.0072(7)
N3 0.0506(9) 0.0558(9) 0.0481(9) 0.0081(7) 0.0259(8) 0.0112(7)
O1 0.0542(9) 0.0753(9) 0.0733(10) 0.0134(7) 0.0331(8) 0.0233(8)
O2 0.0792(11) 0.0595(8) 0.0457(8) -0.0060(7) 0.0234(7) 0.0020(6)
S1 0.0546(3) 0.0506(3) 0.0465(3) 0.0042(2) 0.0244(2) 0.00978(19)
C9 0.0466(11) 0.0798(14) 0.0577(13) 0.0102(10) 0.0254(10) 0.0069(10)
C12 0.045(2) 0.101(3) 0.084(4) 0.011(2) 0.030(3) 0.006(3)
C13 0.081(6) 0.098(5) 0.094(6) 0.048(5) 0.012(5) 0.016(5)
O3 0.096(4) 0.128(4) 0.144(5) 0.037(3) 0.087(4) 0.017(3)
C9A 0.0466(11) 0.0798(14) 0.0577(13) 0.0102(10) 0.0254(10) 0.0069(10)
C12A 0.054(4) 0.105(4) 0.077(4) 0.025(4) 0.025(4) 0.001(4)
C13A 0.072(7) 0.107(8) 0.086(7) 0.025(7) 0.032(6) -0.007(7)
O3A 0.070(4) 0.144(6) 0.127(6) 0.026(4) 0.062(4) 0.009(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 C6 . . 121.33(19) ?
C2 C1 S1 . . 120.01(15) ?
C6 C1 S1 . . 118.66(15) ?
C1 C2 C3 . . 118.4(2) ?
C1 C2 H2 . . 120.8 ?
C3 C2 H2 . . 120.8 ?
C4 C3 C2 . . 120.1(2) ?
C4 C3 H3 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
C5 C4 C3 . . 120.8(2) ?
C5 C4 H4 . . 119.6 ?
C3 C4 H4 . . 119.6 ?
C4 C5 C6 . . 120.2(2) ?
C4 C5 H5 . . 119.9 ?
C6 C5 H5 . . 119.9 ?
C5 C6 C1 . . 119.3(2) ?
C5 C6 H6 . . 120.3 ?
C1 C6 H6 . . 120.3 ?
N2 C7 N3 . . 126.86(17) ?
N2 C7 N1 . . 118.71(17) ?
N3 C7 N1 . . 114.43(16) ?
N2 C8 C9A . . 120.86(18) ?
N2 C8 C9 . . 120.86(18) ?
N2 C8 C11 . . 114.9(2) ?
C9A C8 C11 . . 124.2(2) ?
C9 C8 C11 . . 124.2(2) ?
N3 C10 C9A . . 124.15(19) ?
N3 C10 C9 . . 124.15(19) ?
N3 C10 H10 . . 117.9 ?
C9 C10 H10 . . 117.9 ?
C8 C11 H11A . . 109.5 ?
C8 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C8 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C7 N1 S1 . . 127.69(14) ?
C7 N1 H1 . . 118.2(14) ?
S1 N1 H1 . . 112.6(15) ?
C7 N2 C8 . . 117.10(17) ?
C10 N3 C7 . . 115.02(17) ?
O2 S1 O1 . . 119.43(10) ?
O2 S1 N1 . . 110.41(9) ?
O1 S1 N1 . . 102.84(9) ?
O2 S1 C1 . . 108.71(9) ?
O1 S1 C1 . . 108.55(9) ?
N1 S1 C1 . . 106.06(9) ?
C10 C9 C8 . . 115.92(19) ?
C10 C9 C12 . . 120.0(3) ?
C8 C9 C12 . . 123.6(3) ?
O3 C12 C13 . . 120.4(5) ?
O3 C12 C9 . . 121.9(4) ?
C13 C12 C9 . . 117.6(5) ?
C12 C13 H13A . . 109.5 ?
C12 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C12 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C10 C9A C8 . . 115.92(19) ?
C10 C9A C12A . . 120.4(3) ?
C8 C9A C12A . . 122.5(3) ?
O3A C12A C13A . . 121.1(5) ?
O3A C12A C9A . . 120.1(5) ?
C13A C12A C9A . . 118.6(6) ?
C12A C13A H13D . . 109.5 ?
C12A C13A H13E . . 109.5 ?
H13D C13A H13E . . 109.5 ?
C12A C13A H13F . . 109.5 ?
H13D C13A H13F . . 109.5 ?
H13E C13A H13F . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.378(3) ?
C1 C6 . 1.382(3) ?
C1 S1 . 1.7538(19) ?
C2 C3 . 1.388(3) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.373(3) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.367(3) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.368(3) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 N2 . 1.330(2) ?
C7 N3 . 1.337(2) ?
C7 N1 . 1.374(2) ?
C8 N2 . 1.338(3) ?
C8 C9A . 1.412(3) ?
C8 C9 . 1.412(3) ?
C8 C11 . 1.502(3) ?
C10 N3 . 1.329(2) ?
C10 C9A . 1.376(3) ?
C10 C9 . 1.376(3) ?
C10 H10 . 0.9300 ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
N1 S1 . 1.6465(16) ?
N1 H1 . 0.83(2) ?
O1 S1 . 1.4267(15) ?
O2 S1 . 1.4226(15) ?
C9 C12 . 1.507(4) ?
C12 O3 . 1.211(5) ?
C12 C13 . 1.497(6) ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
C9A C12A . 1.501(5) ?
C12A O3A . 1.207(5) ?
C12A C13A . 1.495(6) ?
C13A H13D . 0.9600 ?
C13A H13E . 0.9600 ?
C13A H13F . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 N3 3_666 0.83(2) 2.06(2) 2.891(2) 179(2) yes
C6 H6 O2 4_576 0.93 2.62 3.338(3) 135.0 yes
C10 H10 O1 3_666 0.93 2.54 3.243(3) 132.8 yes
C11 H11B O3A . 0.96 2.26 2.769(7) 112.6 yes
C13A H13E O1 2_645 0.96 2.50 3.40(3) 156.2 yes
_cod_database_fobs_code 2244245