#------------------------------------------------------------------------------
#$Date: 2024-09-11 04:38:05 +0300 (Wed, 11 Sep 2024) $
#$Revision: 294712 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023247.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_2023247
loop_
_publ_author_name
'Filley, Jonathan'
_publ_section_title
;
Color center creation by dipole stacking in crystals of
2-methoxy-5-nitroaniline
;
_journal_coeditor_code EV2011
_journal_issue 10
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024008739
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C7 H8 N2 O3'
_chemical_formula_moiety 'C7 H8 N2 O3'
_chemical_formula_sum 'C7 H8 N2 O3'
_chemical_formula_weight 168.15
_chemical_name_systematic
;
2-Methoxy-5-nitroaniline
;
_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 difmap
_atom_sites_solution_primary direct
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 96.9437(14)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.14981(11)
_cell_length_b 9.79512(11)
_cell_length_c 10.74206(14)
_cell_measurement_reflns_used 7580
_cell_measurement_temperature 100
_cell_measurement_theta_max 75.8650
_cell_measurement_theta_min 4.1410
_cell_volume 746.784(17)
_computing_cell_refinement
;
CrysAlisPro (Agilent, 2014)
;
_computing_data_collection
;
CrysAlisPro (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlisPro (Agilent, 2014)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2013/4 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.2603
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Onyx, Ultra'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0489
_diffrn_reflns_av_unetI/netI 0.0193
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 13822
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 76.077
_diffrn_reflns_theta_min 7.065
_diffrn_source 'sealed X-ray tube'
_exptl_absorpt_coefficient_mu 1.014
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.82670
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent, 2014)
;
_exptl_crystal_colour 'clear dark orange'
_exptl_crystal_density_diffrn 1.496
_exptl_crystal_description block
_exptl_crystal_F_000 352
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.2
_refine_diff_density_max 0.253
_refine_diff_density_min -0.165
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.057
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 141
_refine_ls_number_reflns 1543
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.057
_refine_ls_R_factor_all 0.0392
_refine_ls_R_factor_gt 0.0353
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.2402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0927
_refine_ls_wR_factor_ref 0.0974
_reflns_number_gt 1398
_reflns_number_total 1543
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ev2011.cif
_cod_data_source_block I
_cod_original_cell_volume 746.783(18)
_cod_database_code 2023247
_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 0.631
_shelx_estimated_absorpt_t_max 0.823
_shelx_hkl_file
;
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0 0 -1 16.4887 28.9415 2
0 0 1 35.8771 32.8624 22
0 0 -1 144.524 40.8811 4
0 0 -2 149870. 1850.03 21
0 0 2 151396. 1935.21 25
0 0 2 149745. 1604.01 22
0 0 2 149927. 1796.09 23
0 0 -2 151528. 1749.45 4
0 0 -2 148305. 1923.06 2
0 0 3-2.07619 137.941 22
0 0 3 33.1773 109.219 23
0 0 -3 233.332 157.439 2
0 0 -3 135.440 174.696 21
0 0 -3 110.858 174.546 4
0 0 3 104.444 134.141 25
0 0 4 116432. 2450.69 25
0 0 -4 113218. 1911.13 24
0 0 -4 111049. 2446.07 2
0 0 -4 118164. 2393.14 21
0 0 -5-139.301 151.820 2
0 0 -5 40.8152 161.138 21
0 0 -5 144.513 104.172 4
0 0 5 126.646 168.314 25
0 0 -5 102.565 78.9493 24
0 0 -6 777.268 273.965 21
0 0 -6 643.770 280.099 2
0 0 -6 888.423 235.950 4
0 0 6 424.088 264.393 25
0 0 7 121.053 156.127 25
0 0 -7 110.597 159.977 2
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0 0 -7 68.6358 243.802 4
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0 0 -8 2074.59 554.946 2
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0 0 -8 2745.30 804.779 28
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0 0 -9-301.925 516.531 28
0 0 -9 1138.48 570.279 2
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0 0 9-318.198 241.919 25
0 0 9 301.636 241.955 15
0 0 -9-765.856 524.322 35
0 0 -10 452.538 555.035 35
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0 0 -10-522.914 816.634 29
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0 0 -11-19.0799 239.315 29
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0 0 -11 514.761 439.992 28
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0 0 -12 37328.7 1963.10 35
0 0 -12 36244.5 1992.61 28
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0 0 -13 262.198 159.618 5
0 -1 0 162.746 56.5406 4
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0 1 -2 87606.0 1111.19 4
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0 1 -2 85042.9 1559.66 2
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0 1 -3 7987.41 585.892 2
0 -1 3 8290.96 603.466 25
0 1 -3 8418.39 456.592 4
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0 -1 -3 7397.40 597.511 3
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-7 -3 0-58.1980 284.209 9
-7 3 0 222.528 430.584 14
-7 -3 0 663.715 356.640 14
-7 3 -1 2872.13 749.985 20
-7 3 -1 2220.91 657.160 10
-7 -3 -1 2226.89 676.777 18
7 3 1 1703.69 658.453 27
-7 3 -1 2730.15 709.316 14
-7 -3 -1 2212.69 612.877 14
-7 3 -2 62792.7 2602.06 20
-7 3 -2 62755.3 2705.66 10
-7 -3 -2 55306.5 2375.07 18
-7 3 -2 67669.5 2798.14 14
-7 -3 -2 61665.5 2761.43 14
-7 3 -3 19721.2 1478.65 20
-7 3 -3 18632.9 1448.82 10
-7 3 -3 21010.0 1527.85 14
-7 -3 -3 17903.2 1488.14 14
-7 3 -4 4221.21 840.603 10
-7 3 -4 3229.88 641.063 14
-7 -3 -4 3244.53 622.830 14
-7 3 -5 103636. 2925.33 10
-7 -3 -5 96945.8 2880.91 14
7 3 6 50080.3 1652.76 27
-7 -3 -6 53745.1 1854.48 14
-7 4 8 6368.74 560.797 12
-7 -4 8 8564.41 713.736 20
-7 -4 8 8305.02 754.925 32
-7 4 7 17142.1 1061.23 12
7 4 -7 17062.0 1090.21 35
-7 -4 7 17852.6 1169.15 20
-7 -4 7 18353.4 1260.48 32
7 4 -7 17221.6 1066.21 29
-7 4 6 8496.03 879.210 12
-7 4 6 7720.38 686.198 20
-7 -4 6 7225.82 884.145 20
-7 -4 6 7434.02 939.832 32
-7 -4 6 8888.75 950.361 18
7 4 -6 8341.85 868.565 29
-7 4 5 7359.42 971.745 12
-7 4 5 7902.89 894.487 20
-7 -4 5 7118.37 917.790 20
-7 -4 5 7500.30 1001.26 32
-7 -4 5 7604.05 974.142 18
7 4 -5 6742.07 874.782 29
-7 4 4 989.628 465.062 12
-7 4 4 294.062 550.414 20
-7 -4 4 550.693 495.646 20
-7 -4 4 82.9825 402.931 32
-7 -4 4 250.312 332.473 18
7 4 -4 313.972 407.435 29
-7 4 3 4403.33 675.070 12
-7 4 3 4467.83 824.358 20
-7 -4 3 5256.03 864.976 20
-7 -4 3 4746.86 787.834 32
-7 -4 3 4865.98 756.741 18
-7 4 2 19605.2 1451.67 12
-7 4 2 17302.4 1495.46 20
-7 -4 2 18701.8 1454.69 20
-7 -4 2 17259.6 1441.85 18
-7 -4 2 17756.3 1429.20 9
-7 4 2 21781.5 1695.45 14
-7 4 1 976.505 462.800 12
-7 4 1 1294.14 660.168 20
-7 -4 1 1078.23 241.517 20
-7 -4 1 895.714 579.073 18
-7 -4 1 244.895 461.068 9
-7 4 1 945.758 449.011 14
-7 -4 1 513.457 421.152 14
-7 4 0-121.606 278.524 12
-7 4 0-49.0788 488.773 20
-7 -4 0 50.9574 233.784 18
-7 -4 0-236.957 383.465 9
-7 4 0 76.3472 491.177 14
-7 -4 0-452.178 314.536 14
-7 4 -1 21608.7 1466.16 12
-7 4 -1 23940.3 1632.42 20
-7 4 -1 21565.5 1519.31 10
-7 -4 -1 25432.3 1730.34 18
-7 -4 -1 22254.0 1515.07 9
-7 4 -1 21482.0 1484.41 16
7 4 1 23592.7 1532.80 27
-7 4 -1 25578.4 1673.55 14
-7 -4 -1 26152.1 1758.93 14
-7 4 -2 152796. 3887.10 20
-7 4 -2 148409. 3856.79 10
-7 4 -2 143274. 3652.29 16
7 4 2 153632. 3750.95 27
-7 4 -2 148700. 3713.44 14
-7 -4 -2 152786. 3988.46 14
-7 4 -3 37258.5 1847.32 20
-7 4 -3 34389.8 1838.77 10
7 4 3 36329.1 1808.42 27
-7 -4 -3 33980.0 1843.69 14
-7 4 -4 9994.72 968.509 10
7 4 4 8552.39 867.710 27
-7 -4 -4 10050.2 980.696 14
-7 4 -5 21740.8 1241.68 10
7 4 5 20294.9 1166.09 27
-7 -4 -5 20697.8 1175.04 14
-7 5 7 11893.2 805.290 12
-7 -5 7 12071.8 861.939 20
-7 -5 7 10573.6 852.521 32
7 5 -7 10839.4 778.863 29
-7 5 6 790.704 282.920 12
-7 -5 6 320.714 252.223 20
-7 -5 6 387.872 357.410 32
-7 -5 6 1030.46 317.047 18
7 5 -6 1093.99 333.629 29
-7 5 5 628.117 321.478 12
-7 5 5-135.621 92.6334 20
-7 -5 5 157.523 282.633 20
-7 -5 5-130.267 289.388 32
-7 -5 5 362.451 330.646 18
7 5 -5 302.749 342.078 29
-7 5 4 10412.6 1025.75 12
-7 5 4 10285.0 925.679 20
-7 -5 4 10022.8 1006.51 20
-7 -5 4 10526.7 1003.96 32
-7 -5 4 10383.9 1033.59 18
7 5 -4 9317.85 939.788 29
-7 5 3-402.229 431.038 12
-7 5 3 589.127 468.487 20
-7 -5 3 296.104 392.978 20
-7 -5 3-117.660 451.710 32
-7 -5 3 113.823 398.288 18
7 5 -3 316.870 422.436 29
-7 5 2 454.611 894.297 12
-7 5 2 777.490 385.701 20
-7 -5 2-89.4201 145.535 20
-7 -5 2 157.062 300.414 18
-7 -5 2-67.5978 351.899 9
-7 5 1 4710.07 792.137 12
-7 5 1 5169.20 820.275 20
-7 -5 1 5033.58 855.765 18
-7 -5 1 4475.35 760.990 9
-7 5 1 3619.46 594.424 16
-7 5 0 569.236 391.154 12
-7 5 0 1444.25 555.284 20
-7 -5 0 626.742 460.569 18
-7 -5 0 65.6583 393.935 9
-7 5 0 877.207 524.594 16
-7 5 -1 86912.0 2738.43 12
-7 5 -1 94775.2 3015.81 20
-7 -5 -1 85254.1 2904.77 18
-7 -5 -1 85662.3 2782.86 9
-7 5 -1 86937.7 2839.54 16
-7 5 -2 88773.8 2805.33 20
-7 5 -2 74873.3 2413.70 10
-7 -5 -2 81029.5 2667.17 18
-7 -5 -2 70416.2 2378.16 9
-7 5 -2 88600.8 2730.96 16
7 5 2 89247.0 2650.03 27
-7 5 -3-374.511 361.402 10
-7 -5 -3 52.2068 127.761 18
-7 -5 -3-95.5000 177.817 9
7 5 3-304.938 332.162 27
-7 -5 -3-244.682 365.743 14
-7 5 -4 13425.3 974.966 10
7 5 4 14002.9 1003.61 27
-7 5 -5 181.230 173.386 10
7 5 5-105.753 189.884 27
-7 6 6 1262.65 284.606 12
-7 -6 6 880.768 230.758 20
-7 -6 6 1146.73 284.908 32
7 6 -6 1878.61 353.044 29
-7 6 5 6215.30 648.415 12
-7 -6 5 5885.39 587.076 20
-7 -6 5 4236.96 584.235 32
-7 -6 5 5598.49 681.801 18
7 6 -5 7032.39 714.731 29
-7 6 4 1996.72 550.997 12
-7 6 4 1793.16 461.523 20
-7 -6 4 1531.25 413.305 20
-7 -6 4 774.791 369.905 32
-7 -6 4 2288.72 472.638 18
7 6 -4 2136.88 509.330 29
-7 6 3 6595.67 796.710 12
-7 6 3 6989.19 856.578 20
-7 -6 3 60.9986 255.124 20
-7 -6 3 7317.77 830.429 18
7 6 -3 7181.99 843.924 29
-7 6 3 299.428 257.291 16
-7 6 2 43480.8 1911.84 12
-7 6 2 42504.5 1894.21 20
-7 -6 2 39966.5 1872.95 18
7 6 -2 42715.4 1879.33 29
-7 6 1 6699.70 821.577 12
-7 6 1 6977.94 922.694 20
-7 -6 1 7048.67 856.733 18
-7 -6 1 6788.28 796.028 9
-7 6 1 5522.84 676.386 16
-7 6 0 5122.23 763.625 12
-7 6 0 6556.42 886.895 20
-7 -6 0 4631.98 732.128 18
-7 -6 0 4428.41 647.537 9
-7 6 0 5674.99 761.348 16
-7 6 -1 11650.9 995.186 12
-7 -6 -1 9274.77 947.022 18
-7 -6 -1 9412.80 916.160 9
-7 6 -1 9344.08 901.560 16
7 6 1 7731.27 711.188 27
-7 -6 -2 3347.53 567.813 18
-7 -6 -2 2759.53 481.532 9
7 6 2 3386.95 505.832 27
-7 -6 -3 167.743 119.963 18
7 6 3 88.5507 147.485 27
-7 7 4 5023.47 524.967 12
-7 -7 4 4843.54 524.810 18
7 7 -4 5543.08 560.212 29
-7 7 3 33934.3 1404.23 12
-7 -7 3 31646.0 1375.68 18
7 7 -3 35676.7 1438.05 29
-7 7 2 29563.0 1366.66 12
-7 -7 2 27967.8 1328.85 18
7 7 -2 30478.4 1367.50 29
-7 7 1 5733.67 658.605 12
-7 -7 1 5601.91 638.411 18
-7 7 1 4661.07 528.344 16
7 7 -1 5881.80 633.372 29
-7 7 0 1324.34 379.384 12
-7 -7 0 1221.66 289.872 18
-7 -7 0 776.835 309.494 9
-7 7 0 1107.90 401.511 16
7 7 0 737.008 213.109 29
-7 -7 -1 5007.62 597.162 18
-7 -7 -1 4846.26 585.814 9
-7 7 -1 5100.72 540.788 16
-7 -7 -2 5828.76 526.224 18
8 0 -7 428.580 211.374 35
-8 0 7 23.4250 81.8400 20
-8 0 6 6893.39 718.116 20
-8 0 5 176.640 305.631 20
-8 0 4 10937.0 1025.78 20
-8 0 3-25.8321 354.263 20
-8 0 3 203.949 442.084 14
-8 0 2 4105.08 721.810 20
-8 0 2 4963.39 765.183 14
-8 0 1 36.9484 522.801 20
-8 0 1-66.7854 257.183 14
-8 0 0 14803.3 1206.67 20
-8 0 0 14821.7 1278.78 14
-8 0 -1 497.129 308.199 20
-8 0 -1 140.832 423.060 14
-8 0 -2 319.736 377.479 14
-8 0 -3-64.4298 336.704 14
-8 0 -4 2590.89 411.417 14
8 1 -7 1600.83 381.463 35
-8 -1 7 1729.72 302.161 20
-8 1 6 99.9843 222.361 20
-8 -1 6-386.721 262.164 20
-8 1 5 421.798 326.715 20
-8 -1 5 44.0813 252.562 20
-8 1 4 10136.9 1005.83 20
-8 -1 4 9889.79 989.324 20
-8 1 3 35072.4 1855.97 20
-8 -1 3 34199.6 1838.69 20
-8 1 3 39279.5 1995.12 14
-8 -1 3 39255.3 1976.13 14
-8 1 2 1367.07 498.102 20
-8 -1 2 979.090 400.818 20
-8 1 2 1120.38 455.733 14
-8 -1 2 648.531 477.158 14
-8 1 1-258.528 405.464 20
-8 -1 1 240.991 271.007 20
-8 1 1-453.382 281.315 14
-8 -1 1-177.463 384.846 14
-8 1 0 155.416 503.546 20
-8 -1 0 577.298 372.508 20
-8 1 0 459.930 392.674 14
-8 -1 0 372.297 285.528 14
-8 1 -1 15401.5 1106.43 20
-8 1 -1 15695.2 1310.27 14
-8 -1 -1 15820.8 1310.78 14
-8 1 -2 221.106 130.585 20
-8 1 -2 884.703 485.462 14
-8 -1 -2 266.852 398.827 14
-8 1 -3 232.938 270.282 14
-8 -1 -3 246.924 287.009 14
-8 1 -4 8295.55 715.282 14
-8 -1 -4 8835.01 823.894 14
8 2 -7 8752.65 671.337 35
-8 -2 7 10659.7 694.414 20
-8 2 6 836.502 322.263 20
-8 -2 6 979.195 313.350 20
-8 2 5 47096.3 1850.15 20
-8 -2 5 46920.8 1903.03 20
-8 2 4 14021.8 1115.65 20
-8 -2 4 14528.9 1157.22 20
-8 -2 4 13387.9 1033.25 18
-8 2 3 9641.05 996.878 20
-8 -2 3 9770.86 963.646 20
-8 -2 3 10150.6 921.785 18
8 2 -3 7669.19 779.770 29
-8 -2 3 7898.31 803.119 14
-8 2 2 11152.2 1066.98 20
-8 -2 2 11176.3 1008.79 20
-8 -2 2 8118.18 829.744 18
-8 2 2 12887.4 1191.50 14
-8 -2 2 11018.6 1023.21 14
-8 2 1 4331.89 725.788 20
-8 -2 1 3779.56 662.946 20
-8 2 1 4343.77 705.284 14
-8 -2 1 4948.92 742.596 14
-8 2 0 145.258 402.426 20
-8 -2 0-31.5209 178.623 20
-8 2 0 256.005 404.748 14
-8 -2 0 153.272 365.117 14
-8 2 -1 19675.3 1289.00 20
-8 2 -1 19561.3 1379.96 14
-8 -2 -1 20069.7 1361.65 14
-8 2 -2 27897.3 1522.16 14
-8 -2 -2 25806.5 1472.62 14
-8 2 -3 281.657 142.244 14
-8 -2 -3 594.503 383.960 14
-8 -2 -4 2868.14 451.296 14
8 3 -6 3636.61 502.203 35
-8 -3 6 3581.71 482.293 20
-8 3 5 46284.7 1627.81 20
-8 -3 5 47938.7 1782.42 20
-8 3 4 163007. 3387.57 20
-8 -3 4 166614. 3518.86 20
-8 -3 4 165799. 3396.22 18
-8 3 3 11767.4 1051.50 20
-8 -3 3 12354.2 1025.59 20
-8 -3 3 12124.6 947.393 18
8 3 -3 9703.85 877.583 29
-8 3 2 6.69197 404.188 20
-8 -3 2 31.2185 256.071 20
-8 -3 2 187.491 266.508 18
8 3 -2-482.124 187.049 29
-8 -3 2 338.672 293.924 14
-8 3 1 11113.8 1039.75 20
-8 -3 1 9443.11 822.647 18
-8 -3 1 9818.47 877.634 14
-8 3 0 2613.92 665.018 20
-8 3 0 3386.01 689.938 14
-8 -3 0 2214.37 464.612 14
-8 3 -1 830.326 391.445 14
-8 -3 -1 839.103 267.526 14
-8 3 -2 795.829 455.256 20
-8 3 -2 339.831 244.826 14
-8 -3 -2 527.983 227.050 14
-8 -3 -3 629.382 271.638 14
-8 -4 5 34.2916 79.3268 20
-8 4 4 74869.6 2041.57 20
-8 -4 4 71949.2 2006.16 20
-8 -4 4 75104.2 2125.02 18
-8 4 3 45009.8 1750.21 20
-8 -4 3 42828.9 1680.80 18
8 4 -3 42458.3 1623.97 29
-8 4 2 937.431 390.683 20
-8 -4 2 1276.78 333.100 18
8 4 -2 1594.26 433.463 29
-8 4 1 4370.01 692.616 20
-8 -4 1 3076.80 475.380 18
-8 4 0 1326.36 483.322 20
-8 -4 0 10.2500 236.796 18
-8 4 -1 22271.8 1225.09 20
-8 -5 4 23415.9 1015.34 18
-8 5 3 10689.9 741.003 20
-8 -5 3 8810.59 694.888 18
8 5 -3 9898.63 736.914 29
-8 -5 2 33.1187 157.113 18
8 5 -2-95.3894 305.318 29
-8 -5 1 11914.5 798.442 18
8 5 -1 13970.0 922.115 29
0 0 0 0.00 0.00 0
TITL JF-2M5NA in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184 7.149811 9.795119 10.742058 90.0000 96.9437 90.0000
ZERR 4.00 0.000111 0.000113 0.000139 0.0000 0.0014 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O
UNIT 28.00 32.00 8.00 12.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 16578
_shelx_res_file
;
TITL JF-2M5NA in P21/n #14
CELL 1.54184 7.149811 9.795119 10.742058 90 96.9437 90
ZERR 4 0.000111 0.000113 0.000139 0 0.0014 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 28 32 8 12
EQIV $1 0.5+X,0.5-Y,0.5+Z
EQIV $2 0.5-X,-0.5+Y,-0.5-Z
EQIV $3 0.5+X,1.5-Y,0.5+Z
EQIV $4 0.5-X,0.5+Y,0.5-Z
EQIV $5 -0.5+X,0.5-Y,-0.5+Z
EQIV $6 -X,1-Y,-Z
L.S. 10
PLAN 10
SIZE 0.5 0.4 0.2
TEMP -173.15
CONF
HTAB C3 O1_$4
HTAB C3 O2_$3
HTAB N1 O3_$2
HTAB N1 O3_$1
HTAB N1 O2_$2
HTAB N1 N2_$2
HTAB C6 O1_$5
HTAB C6 O2_$2
HTAB C6 N2_$2
HTAB C4 O1_$4
HTAB C7 O3_$6
HTAB C7 O2_$3
HTAB C7 N1_$4
HTAB C7 N1_$1
BOND
BOND $H
HTAB
more -3
fmap 2
acta
REM
REM
REM
WGHT 0.054200 0.240200
FVAR 16.12577
O1 4 0.433122 0.359469 0.243228 11.00000 0.02418 0.02003 =
0.01634 -0.00077 0.00005 0.00079
O3 4 0.098784 0.515414 -0.300062 11.00000 0.03141 0.02605 =
0.01968 0.00193 0.00039 -0.00307
O2 4 0.059425 0.707927 -0.208101 11.00000 0.03092 0.02107 =
0.03172 0.00783 0.00457 0.00562
C3 1 0.286826 0.556661 0.132599 11.00000 0.01739 0.01900 =
0.02146 -0.00392 0.00363 -0.00206
N2 3 0.111985 0.587934 -0.204870 11.00000 0.01748 0.02074 =
0.02250 0.00448 0.00367 -0.00199
N1 3 0.383531 0.202741 0.040269 11.00000 0.02643 0.01828 =
0.01846 -0.00098 0.00124 0.00294
C5 1 0.192593 0.530049 -0.086070 11.00000 0.01423 0.01955 =
0.01987 0.00289 0.00336 -0.00117
C1 1 0.328880 0.337833 0.029683 11.00000 0.01442 0.01740 =
0.02017 -0.00033 0.00420 -0.00174
C6 1 0.249826 0.393885 -0.083078 11.00000 0.01647 0.01908 =
0.01804 -0.00154 0.00396 -0.00157
C2 1 0.348025 0.422028 0.138003 11.00000 0.01460 0.01990 =
0.01794 0.00133 0.00251 -0.00139
C4 1 0.208869 0.612127 0.019146 11.00000 0.01486 0.01648 =
0.02628 0.00058 0.00501 0.00007
C7 1 0.458336 0.439803 0.355974 11.00000 0.02651 0.02489 =
0.01760 -0.00230 0.00096 -0.00073
H4 2 0.166977 0.704453 0.013556 11.00000 0.02500
H3 2 0.300885 0.611238 0.205548 11.00000 0.02250
H6 2 0.235844 0.338645 -0.157191 11.00000 0.02433
H7A 2 0.532100 0.524044 0.341654 11.00000 0.03217
H7B 2 0.335228 0.463218 0.382953 11.00000 0.02699
H1A 2 0.458999 0.181954 0.109071 11.00000 0.02730
H7C 2 0.526929 0.382110 0.418046 11.00000 0.02731
H1B 2 0.406893 0.162757 -0.028439 11.00000 0.03502
HKLF 4
REM JF-2M5NA in P21/n #14
REM R1 = 0.0353 for 1398 Fo > 4sig(Fo) and 0.0392 for all 1543 data
REM 141 parameters refined using 0 restraints
END
WGHT 0.0542 0.2402
REM Instructions for potential hydrogen bonds
HTAB C3 O2_$3
HTAB C6 O2_$2
HTAB N1 O3_$1
HTAB N1 O3_$2
REM Highest difference peak 0.253, deepest hole -0.165, 1-sigma level 0.045
Q1 1 0.2630 0.4759 -0.0843 11.00000 0.05 0.25
Q2 1 0.3520 0.4993 0.1280 11.00000 0.05 0.24
Q3 1 0.3370 0.3810 0.0809 11.00000 0.05 0.23
Q4 1 0.2901 0.4785 0.1380 11.00000 0.05 0.23
Q5 1 0.2235 0.5735 -0.0391 11.00000 0.05 0.21
Q6 1 0.2526 0.3586 -0.0165 11.00000 0.05 0.17
Q7 1 0.2947 0.5927 0.0584 11.00000 0.05 0.17
Q8 1 0.3354 0.3768 -0.0395 11.00000 0.05 0.16
Q9 1 0.0395 0.5763 -0.3727 11.00000 0.05 0.15
Q10 1 0.2085 0.5668 0.0742 11.00000 0.05 0.14
;
_shelx_res_checksum 25413
_shelxl_version_number .2013
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
O O1 0.43312(12) 0.35947(8) 0.24323(7) 0.0204(2) Uani d 1 . .
O O3 0.09878(13) 0.51541(9) -0.30006(8) 0.0259(2) Uani d 1 . .
O O2 0.05943(13) 0.70793(9) -0.20810(9) 0.0278(2) Uani d 1 . .
C C3 0.28683(16) 0.55666(12) 0.13260(11) 0.0192(3) Uani d 1 . .
N N2 0.11198(14) 0.58793(10) -0.20487(9) 0.0201(2) Uani d 1 . .
N N1 0.38353(15) 0.20274(10) 0.04027(10) 0.0212(2) Uani d 1 . .
C C5 0.19259(16) 0.53005(11) -0.08607(10) 0.0178(3) Uani d 1 . .
C C1 0.32888(16) 0.33783(11) 0.02968(11) 0.0172(3) Uani d 1 . .
C C6 0.24983(16) 0.39389(12) -0.08308(10) 0.0177(3) Uani d 1 . .
C C2 0.34803(16) 0.42203(12) 0.13800(10) 0.0174(3) Uani d 1 . .
C C4 0.20887(16) 0.61213(12) 0.01915(11) 0.0190(3) Uani d 1 . .
C C7 0.45834(19) 0.43980(13) 0.35597(11) 0.0231(3) Uani d 1 . .
H H4 0.167(2) 0.7045(16) 0.0136(14) 0.025(4) Uiso d 1 . .
H H3 0.301(2) 0.6112(15) 0.2055(14) 0.022(3) Uiso d 1 . .
H H6 0.236(2) 0.3386(16) -0.1572(15) 0.024(4) Uiso d 1 . .
H H7A 0.532(2) 0.5240(17) 0.3417(14) 0.032(4) Uiso d 1 . .
H H7B 0.335(2) 0.4632(16) 0.3830(13) 0.027(4) Uiso d 1 . .
H H1A 0.459(2) 0.1820(16) 0.1091(16) 0.027(4) Uiso d 1 . .
H H7C 0.527(2) 0.3821(16) 0.4180(14) 0.027(4) Uiso d 1 . .
H H1B 0.407(2) 0.1628(18) -0.0284(17) 0.035(4) 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
O1 0.0242(4) 0.0200(4) 0.0163(4) 0.0008(3) 0.0000(3) -0.0008(3)
O3 0.0314(5) 0.0261(5) 0.0197(4) -0.0031(4) 0.0004(3) 0.0019(3)
O2 0.0309(5) 0.0211(4) 0.0317(5) 0.0056(4) 0.0046(4) 0.0078(4)
C3 0.0174(6) 0.0190(6) 0.0215(6) -0.0021(4) 0.0036(4) -0.0039(4)
N2 0.0175(5) 0.0207(5) 0.0225(5) -0.0020(4) 0.0037(4) 0.0045(4)
N1 0.0264(6) 0.0183(5) 0.0185(5) 0.0029(4) 0.0012(4) -0.0010(4)
C5 0.0142(5) 0.0196(6) 0.0199(6) -0.0012(4) 0.0034(4) 0.0029(4)
C1 0.0144(5) 0.0174(5) 0.0202(5) -0.0017(4) 0.0042(4) -0.0003(4)
C6 0.0165(6) 0.0191(5) 0.0180(5) -0.0016(4) 0.0040(4) -0.0015(4)
C2 0.0146(6) 0.0199(6) 0.0179(5) -0.0014(4) 0.0025(4) 0.0013(4)
C4 0.0149(6) 0.0165(5) 0.0263(6) 0.0001(4) 0.0050(4) 0.0006(4)
C7 0.0265(7) 0.0249(6) 0.0176(6) -0.0007(5) 0.0010(5) -0.0023(5)
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 O1 C7 . . 116.79(9) ?
C2 C3 H3 . . 120.1(9) ?
C4 C3 C2 . . 119.97(10) ?
C4 C3 H3 . . 119.9(9) ?
O3 N2 C5 . . 118.97(9) ?
O2 N2 O3 . . 122.04(10) ?
O2 N2 C5 . . 118.99(10) ?
C1 N1 H1A . . 115.3(10) ?
C1 N1 H1B . . 116.3(11) ?
H1A N1 H1B . . 116.4(15) ?
C6 C5 N2 . . 118.58(10) ?
C4 C5 N2 . . 118.54(10) ?
C4 C5 C6 . . 122.87(11) ?
N1 C1 C6 . . 122.20(10) ?
N1 C1 C2 . . 119.42(10) ?
C6 C1 C2 . . 118.35(10) ?
C5 C6 H6 . . 121.4(9) ?
C1 C6 C5 . . 119.10(10) ?
C1 C6 H6 . . 119.5(9) ?
O1 C2 C3 . . 124.65(10) ?
O1 C2 C1 . . 114.07(10) ?
C3 C2 C1 . . 121.26(10) ?
C3 C4 H4 . . 121.1(9) ?
C5 C4 C3 . . 118.43(10) ?
C5 C4 H4 . . 120.4(9) ?
O1 C7 H7A . . 109.7(9) ?
O1 C7 H7B . . 110.4(9) ?
O1 C7 H7C . . 105.3(9) ?
H7A C7 H7B . . 111.0(13) ?
H7A C7 H7C . . 110.9(13) ?
H7B C7 H7C . . 109.3(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
O1 C2 . 1.3627(14) ?
O1 C7 . 1.4373(14) ?
O3 N2 . 1.2393(13) ?
O2 N2 . 1.2332(13) ?
C3 C2 . 1.3884(16) ?
C3 C4 . 1.3881(16) ?
C3 H3 . 0.944(15) ?
N2 C5 . 1.4506(14) ?
N1 C1 . 1.3805(15) ?
N1 H1A . 0.885(17) ?
N1 H1B . 0.869(19) ?
C5 C6 . 1.3943(16) ?
C5 C4 . 1.3804(16) ?
C1 C6 . 1.3866(16) ?
C1 C2 . 1.4193(16) ?
C6 H6 . 0.958(16) ?
C4 H4 . 0.952(16) ?
C7 H7A . 1.001(17) ?
C7 H7B . 0.986(16) ?
C7 H7C . 0.962(16) ?
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
C4 H4 O1 2 0.952(16) 3.177(15) 3.7473(14) 120.2(11)
C3 H3 O1 2 0.944(15) 3.039(15) 3.6820(14) 126.7(11)
C3 H3 O2 4_676 0.944(15) 2.646(15) 3.3523(14) 132.1(11)
C6 H6 O1 4_565 0.958(16) 3.006(16) 3.7075(14) 131.2(11)
C6 H6 O2 2_544 0.958(16) 2.527(15) 3.3090(14) 138.8(12)
C6 H6 N2 2_544 0.958(16) 3.130(16) 3.9611(14) 146.0(12)
C7 H7A O2 4_676 1.001(17) 2.691(17) 3.6087(16) 152.5(12)
C7 H7B O3 3_565 0.986(16) 3.130(15) 3.9801(16) 145.2(11)
C7 H7B N1 2 0.986(16) 2.990(16) 3.8090(16) 141.1(11)
N1 H1A O3 4_666 0.885(17) 2.335(17) 3.0395(13) 136.6(14)
C7 H7C N1 4_666 0.962(16) 2.847(16) 3.6953(17) 147.6(12)
N1 H1B O3 2_544 0.869(19) 2.337(19) 3.1812(13) 163.9(15)
N1 H1B O2 2_544 0.869(19) 2.903(18) 3.6404(14) 143.7(14)
N1 H1B N2 2_544 0.869(19) 2.944(19) 3.7781(14) 161.3(14)
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
O3 N2 C5 C6 . . . . -0.95(16) ?
O3 N2 C5 C4 . . . . 179.20(10) ?
O2 N2 C5 C6 . . . . 179.34(10) ?
O2 N2 C5 C4 . . . . -0.51(16) ?
N2 C5 C6 C1 . . . . 179.34(9) ?
N2 C5 C4 C3 . . . . -179.72(10) ?
N1 C1 C6 C5 . . . . 178.05(10) ?
N1 C1 C2 O1 . . . . 4.18(15) ?
N1 C1 C2 C3 . . . . -177.01(10) ?
C6 C5 C4 C3 . . . . 0.44(18) ?
C6 C1 C2 O1 . . . . -177.80(9) ?
C6 C1 C2 C3 . . . . 1.01(17) ?
C2 C3 C4 C5 . . . . 0.67(17) ?
C2 C1 C6 C5 . . . . 0.09(17) ?
C4 C3 C2 O1 . . . . 177.28(10) ?
C4 C3 C2 C1 . . . . -1.41(17) ?
C4 C5 C6 C1 . . . . -0.82(18) ?
C7 O1 C2 C3 . . . . 0.66(16) ?
C7 O1 C2 C1 . . . . 179.43(9) ?