#------------------------------------------------------------------------------
#$Date: 2022-11-08 20:40:13 +0100 (Tue, 08 Nov 2022) $
#$Revision: 279111 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022672.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_2022672
loop_
_publ_author_name
'W\'ojcicka, Anna'
'Becan, Lilianna'
'Rembia\/lkowska, Nina'
'Pyra, Anna'
'Bryndal, Iwona'
_publ_section_title
;
Structure and cytotoxic properties of
1-hydroxy-5-methyl-7-phenylpyrido[3,4-d]pyridazin-4(3H)-one
and its mono- and disubstituted ethyl acetates
;
_journal_coeditor_code QF3056
_journal_issue 10
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 559
_journal_page_last 569
_journal_paper_doi 10.1107/S2053229622009202
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C14 H11 N3 O2, C3 H7 N O'
_chemical_formula_moiety 'C14 H11 N3 O2, C3 H7 N O'
_chemical_formula_sum 'C17 H18 N4 O3'
_chemical_formula_weight 326.35
_chemical_name_systematic
;
1-Hydroxy-5-methyl-7-phenylpyrido[3,4-d]pyridazin-4(3H)-one
dimethylformamide monosolvate
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/1
_cell_angle_alpha 65.618(3)
_cell_angle_beta 89.798(2)
_cell_angle_gamma 87.085(2)
_cell_formula_units_Z 2
_cell_length_a 6.8722(2)
_cell_length_b 11.0502(3)
_cell_length_c 11.2090(3)
_cell_measurement_reflns_used 7662
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 75.4
_cell_measurement_theta_min 4.3
_cell_volume 774.14(4)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2014)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy DW system with a HyPix-Arc 150 detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0180
_diffrn_reflns_av_unetI/netI 0.0172
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 10869
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 75.748
_diffrn_reflns_theta_min 4.331
_diffrn_source 'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu 0.812
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.64358
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2020)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.400
_exptl_crystal_description needle
_exptl_crystal_F_000 344
_exptl_crystal_size_max 0.180
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_min 0.090
_refine_diff_density_max 0.262
_refine_diff_density_min -0.527
_refine_ls_extinction_coef 0.0035(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 237
_refine_ls_number_reflns 3149
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.072
_refine_ls_R_factor_all 0.0474
_refine_ls_R_factor_gt 0.0441
_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^)+(0.0680P)^2^+0.2445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1223
_refine_ls_wR_factor_ref 0.1252
_reflns_number_gt 2827
_reflns_number_total 3149
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file qf3056sup1.cif
_cod_data_source_block 2
_cod_depositor_comments
'Adding full bibliography for 2022672--2022674.cif.'
_cod_database_code 2022672
_cod_database_fobs_code 2022672
_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 0.868
_shelx_estimated_absorpt_t_max 0.930
_shelx_hkl_file
;
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0 0 2 6496.61 145.881 33
0 0 2 6639.87 143.934 30
0 0 2 6877.76 148.884 29
0 0 2 6806.47 150.698 27
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0 0 2 6562.07 143.602 25
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0 0 3 1098.58 41.1973 33
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0 0 3 1208.00 42.4551 22
0 0 3 1155.75 50.5555 10
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0 0 3 1104.37 42.6489 17
0 0 3 1149.75 46.0991 16
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0 0 4 77253.1 1550.02 33
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0 0 -4 75661.1 1533.39 7
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0 0 4 75274.0 1567.86 10
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0 0 4 75028.6 1550.79 17
0 0 4 77887.3 1554.80 15
0 0 4 77794.9 1556.66 16
0 0 4 78733.0 1557.83 44
0 0 5 1432.57 64.6078 44
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7 2 7 1394.34 62.8959 44
7 2 7 1474.39 66.4848 15
7 3 -6 318.523 25.4276 6
7 3 -5 418.174 35.9318 6
-7 -3 4 306.232 35.2063 1
7 3 -4 289.640 32.8933 39
7 3 -4 286.486 34.8479 6
7 3 -3 1959.84 87.4706 39
-7 -3 3 2234.89 96.3324 1
7 3 -2 192.355 34.4716 39
-7 -3 2 225.554 34.9938 43
7 3 -1 2192.47 99.7913 39
-7 -3 1 2474.66 97.4638 43
-7 -3 1 2239.12 104.236 2
7 3 0 3096.78 124.062 39
-7 -3 0 3484.99 120.443 43
-7 -3 0 3307.41 128.765 2
-7 -3 -1 3236.50 113.585 43
-7 -3 -1 3035.73 120.424 2
7 3 1 2893.88 124.894 30
7 3 2 2282.03 110.383 30
-7 -3 -2 2476.52 94.0109 43
7 3 2 2362.90 112.488 25
7 3 3 679.137 61.9195 30
-7 -3 -3 687.901 46.6093 43
7 3 3 666.875 61.8779 25
7 3 4 1283.90 80.9777 25
7 3 4 1157.33 77.0987 30
7 3 5 33.0242 23.1489 26
7 3 5 12.4637 28.7643 25
7 3 5-20.5355 27.0819 31
7 3 5 44.0866 28.3149 30
7 3 6 100.779 28.6489 15
7 3 6 145.556 31.4721 30
7 3 6 141.665 32.9144 25
7 3 7 4306.09 130.428 44
7 3 7 3924.51 127.161 15
7 3 8 8.26589 14.3276 15
7 4 -5 15.3255 13.5074 6
7 4 -4 332.220 32.3870 39
7 4 -4 380.732 34.2705 6
-7 -4 4 378.942 32.4251 1
-7 -4 3 2105.50 85.9831 1
7 4 -3 2001.50 84.5402 39
-7 -4 2 239.019 32.6099 43
-7 -4 2 235.224 37.0378 1
7 4 -2 152.759 32.0059 39
-7 -4 1 120.545 29.6034 43
-7 -4 1 150.571 33.7751 1
7 4 -1 108.487 31.2507 39
-7 -4 0 601.931 55.3708 1
7 4 0 581.882 53.1309 39
-7 -4 0 676.039 49.1430 43
-7 -4 -1 78.5164 26.3729 43
7 4 1 76.8187 31.1739 39
-7 -4 -1 72.6483 32.5493 1
-7 -4 -2 8309.47 213.434 43
7 4 2 7388.16 225.386 25
7 4 2 7451.51 225.698 30
-7 -4 -2 8354.56 230.441 1
7 4 3 786.485 63.4697 30
-7 -4 -3 1011.75 55.2988 43
7 4 3 848.092 66.1096 25
-7 -4 -4 82.9969 21.4124 43
7 4 4 52.1997 30.5320 25
7 4 4 68.3197 29.2850 30
7 4 5 1279.12 76.1646 30
7 4 5 1386.65 73.2796 26
7 4 5 1253.60 75.7154 25
7 4 5 1218.20 72.5349 15
7 4 6 2049.13 93.1136 30
7 4 6 2123.18 91.3280 15
7 4 6 2229.40 87.7051 26
7 4 6 2216.19 95.1227 25
7 4 7 6.06220 18.7725 15
7 4 8 6505.69 164.648 44
7 5 -4 792.048 41.6434 39
7 5 -3 78.9641 23.0969 39
-7 -5 3 85.2917 21.3984 1
-7 -5 2 416.317 39.5337 1
-7 -5 2 372.070 33.1877 43
7 5 -2 371.890 39.3935 39
7 5 -1 2703.30 108.727 39
-7 -5 1 2860.97 98.9898 43
-7 -5 0 4211.95 141.311 1
7 5 0 3894.93 139.052 39
-7 -5 0 4053.13 128.471 43
-7 -5 -1 1578.11 80.7257 1
-7 -5 -1 1505.07 69.8025 43
7 5 1 1468.52 80.2026 39
-7 -5 -2 1645.66 81.8260 1
-7 -5 -2 1718.83 74.0061 43
-7 -5 -3 2311.30 86.4540 43
-7 -5 -4 514.175 38.2338 43
7 5 4 436.796 46.3580 30
7 5 4 408.685 46.4993 25
-7 -5 -5 534.428 34.6781 43
7 5 5 503.932 44.3168 15
7 5 5 594.414 50.3443 26
7 5 5 528.647 49.5691 25
7 5 5 572.330 51.1404 30
7 5 6 2367.80 91.7416 26
7 5 6 2137.11 86.8079 15
7 5 7 201.798 25.9833 26
7 5 7 196.077 25.5320 15
-7 -6 3 382.152 25.2588 1
7 6 -3 395.815 30.4603 39
-7 -6 2 846.125 45.1452 1
7 6 -2 773.779 47.7969 39
7 6 -1-9.03276 21.2419 39
-7 -6 1 1.97670 19.3808 1
-7 -6 1 9.07363 17.4583 43
7 6 0 298.207 38.4663 39
-7 -6 0 269.157 34.4500 1
-7 -6 0 331.426 32.2182 43
-7 -6 -1 1561.96 73.4387 1
-7 -6 -1 1519.59 65.8393 43
-7 -6 -2-8.91386 21.8502 1
-7 -6 -2-11.0795 18.9113 43
-7 -6 -3 257.375 29.9811 1
-7 -6 -3 262.903 30.4317 43
7 6 4 1696.15 84.1045 26
-7 -6 -4 1754.93 68.0165 43
7 6 5 88.3900 28.6009 26
-7 -6 -5 84.4954 18.8652 43
7 6 6 1778.71 76.7327 26
7 6 7 116.399 21.2503 26
-7 -7 1 117.412 19.8084 1
-7 -7 0 404.691 29.1310 43
-7 -7 0 437.547 33.9526 1
-7 -7 -1 943.573 45.7975 43
-7 -7 -1 960.692 50.8146 1
-7 -7 -2 1239.12 56.8828 1
7 7 2 1043.84 58.2963 29
-7 -7 -2 1268.35 54.0589 43
7 7 2 1037.88 58.7102 26
-7 -7 -3 1240.56 53.6914 1
7 7 3 1217.21 62.1028 29
7 7 3 1130.19 63.5731 26
-7 -7 -3 1352.44 55.5583 43
7 7 4 711.656 51.1587 26
-7 -7 -4 812.267 41.4555 43
7 7 5 606.833 46.5788 26
-7 -7 -5 797.378 38.3869 43
7 7 6 126.902 24.8932 26
7 7 7 1772.91 65.0416 26
-7 -8 -1 23.8915 14.7194 1
-7 -8 -2 5729.80 141.032 43
-7 -8 -2 5752.09 140.966 1
-7 -8 -3 6505.62 157.867 43
-7 -8 -4 470.776 28.6612 43
-7 -8 -5 310.534 22.7049 43
-8 4 3 149.163 22.3403 2
-8 4 2 1624.78 62.4429 2
-8 4 1 3036.02 91.9172 2
-8 3 4 65.4528 18.1993 2
-8 3 3 41.3672 19.9964 2
-8 3 2 63.9518 21.3890 2
-8 3 1 145.643 24.5158 2
-8 3 0 72.8234 19.2835 2
8 -3 1 307.466 27.2452 25
8 -2 -5 829.699 38.4051 7
-8 2 4 360.608 30.6892 2
8 -2 -4 255.756 25.9566 7
-8 2 3 1096.52 56.4321 2
-8 2 2 481.095 40.5776 2
-8 2 1 97.7577 25.3498 2
-8 2 0 110.967 23.1385 2
-8 2 -1 23.3436 15.4076 2
8 -2 2 1374.65 57.2847 25
8 -1 -5 71.8943 16.0652 7
-8 1 4 484.334 35.4743 2
8 -1 -4 421.859 32.1300 7
-8 1 3 108.091 24.2243 2
-8 1 2 460.193 40.7859 2
-8 1 1 421.809 39.0553 2
-8 1 0-12.1491 20.0787 2
-8 1 -1 45.1624 18.1060 2
8 -1 2 277.485 31.6824 25
8 -1 3 1129.16 51.7497 25
-8 0 4 60.9733 19.1380 1
-8 0 3 1813.05 73.8682 2
-8 0 2 6409.50 176.929 2
-8 0 1 150.633 27.3524 2
-8 0 0 1865.57 77.8275 2
-8 0 -1 1.74477 16.8128 2
8 0 2 14.6857 20.0989 25
8 0 3 41.7230 19.2600 25
8 0 4 1336.83 56.3472 15
8 0 4 1293.61 53.8740 25
-8 -1 4 247.331 24.7230 1
-8 -1 3-5.29128 18.7092 1
-8 -1 2 444.812 38.5987 2
-8 -1 1 2062.81 82.2917 2
-8 -1 0 116.065 23.9112 2
-8 -1 -1 31.5817 19.0447 2
8 1 1 44.6417 24.1427 25
8 1 2 914.525 55.4952 25
8 1 3 15.8578 19.8742 25
8 1 4 724.581 43.2384 15
8 1 4 806.708 45.5467 25
-8 -2 3 1438.78 59.1260 1
-8 -2 2 219.794 29.8351 1
-8 -2 1 1683.74 72.9992 1
-8 -2 0 2105.90 81.0475 1
8 2 0 1809.31 73.8474 25
-8 -2 -1 234.075 29.1593 1
8 2 1 219.516 30.9752 25
8 2 2 25.0480 22.4668 25
8 2 3 1.97523 19.6938 25
8 2 4 1125.10 53.9804 15
8 2 4 1051.57 53.3905 25
-8 -3 3 622.266 33.3909 1
-8 -3 2 2657.61 87.2047 1
-8 -3 1 303.369 31.5471 1
-8 -3 0 216.626 29.0347 1
-8 -3 -1 1913.73 72.9681 1
8 3 2 20.9267 19.2939 25
8 3 3 991.738 51.2411 26
8 3 3 906.318 51.1429 25
8 3 4 588.219 37.3074 15
8 3 4 614.767 40.2683 25
-8 -4 2 353.438 25.9577 1
-8 -4 1 377.143 29.8188 1
-8 -4 0 3.00393 16.1624 1
-8 -4 -1 918.129 42.7683 43
-8 -4 -1 947.462 46.4388 1
-8 -4 -2 173.275 20.1464 43
8 4 3 144.866 24.8480 26
8 4 4 439.704 31.7826 26
-8 -5 0 293.180 23.3177 1
-8 -5 -1 1347.93 49.1820 43
-8 -5 -1 1253.98 47.7972 1
8 5 2-1.57927 16.7520 26
-8 -5 -2 2.98652 11.9995 43
8 5 3 310.827 28.7859 26
0 0 0 0.00 0.00 0
TITL pm_auto in P-1
REM P-1 (#2 in standard setting)
CELL 1.54184 6.872937 11.052754 11.209093 65.6130 89.7871 87.0840
ZERR 3.00 0.000149 0.000239 0.000228 0.0020 0.0017 0.0018
LATT 1
SFAC C H N O
UNIT 33.00 30.00 3.00 3.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
;
_shelx_hkl_checksum 91459
_shelx_res_file
;
TITL pm in P-1
2.res
created by SHELXL-2018/1 at 08:55:24 on 21-Jun-2022
CELL 1.54184 6.8722 11.0502 11.209 65.618 89.798 87.085
ZERR 2 0.0002 0.0003 0.0003 0.003 0.002 0.002
LATT 1
SFAC C H N O
UNIT 34 36 8 6
size 0.18 0.15 0.09
L.S. 4
PLAN 5
TEMP -173
CONF
HTAB 2
BOND $H
fmap 2
acta
HTAB O1 O1N
HTAB O1 O1N'
EQIV $1 -x+2, -y+2, -z+1
HTAB N3 O4_$1
EQIV $2 x, y-1, z+1
HTAB C2N O4_$2
EQIV $3 -x+1, -y+1, -z+2
HTAB C3N O1N_$3
mpla 10 C1 N2 N3 C4 C10 C9 C8 C7 N6 C5 C51 O1 H1 O4
MPLA 6 C71 C72 C73 C74 C75 C76
WGHT 0.068000 0.244500
EXTI 0.003456
FVAR 6.71339 0.61114
O1 4 0.562513 0.574794 0.641993 11.00000 0.03506 0.03278 =
0.02358 -0.00090 -0.00828 -0.01329
AFIX 147
H1 2 0.623980 0.537400 0.713697 11.00000 -1.50000
AFIX 0
C1 1 0.624162 0.697512 0.576669 11.00000 0.02876 0.03053 =
0.02020 -0.00820 -0.00133 -0.00822
N2 3 0.783997 0.730732 0.613022 11.00000 0.03051 0.03081 =
0.02256 -0.00711 -0.00413 -0.00892
N3 3 0.836978 0.858781 0.541113 11.00000 0.02609 0.02942 =
0.02439 -0.01017 -0.00431 -0.00880
AFIX 43
H3 2 0.943753 0.881584 0.567844 11.00000 -1.20000
AFIX 0
O4 4 0.812591 1.065994 0.380912 11.00000 0.02818 0.02684 =
0.03242 -0.01150 -0.00537 -0.00791
C4 1 0.745571 0.954072 0.434458 11.00000 0.02387 0.02725 =
0.02374 -0.01322 -0.00020 -0.00461
C5 1 0.455358 0.996946 0.279330 11.00000 0.02257 0.02238 =
0.02581 -0.01234 -0.00018 -0.00295
C51 1 0.514162 1.132211 0.187293 11.00000 0.02724 0.02178 =
0.03296 -0.00902 -0.00512 -0.00473
AFIX 137
H51 2 0.430899 1.165143 0.108287 11.00000 -1.50000
H52 2 0.650440 1.126537 0.163166 11.00000 -1.50000
H53 2 0.499590 1.193383 0.230255 11.00000 -1.50000
AFIX 0
N6 3 0.291581 0.957462 0.246702 11.00000 0.02230 0.02143 =
0.02618 -0.00996 -0.00144 -0.00355
C7 1 0.228033 0.835197 0.321487 11.00000 0.02211 0.02317 =
0.02236 -0.01096 0.00115 -0.00438
C71 1 0.041170 0.802550 0.277387 11.00000 0.02254 0.02392 =
0.02238 -0.01143 0.00076 -0.00470
C72 1 -0.059639 0.897351 0.167849 11.00000 0.02649 0.02282 =
0.02355 -0.01053 0.00085 -0.00510
AFIX 43
H72 2 -0.007941 0.982098 0.122002 11.00000 -1.20000
AFIX 0
C73 1 -0.234309 0.869395 0.125097 11.00000 0.02579 0.02851 =
0.02445 -0.01212 -0.00299 -0.00215
AFIX 43
H73 2 -0.300666 0.934803 0.050269 11.00000 -1.20000
AFIX 0
C74 1 -0.312313 0.746145 0.191358 11.00000 0.02301 0.03375 =
0.02827 -0.01730 0.00079 -0.00747
AFIX 43
H74 2 -0.431782 0.726916 0.162254 11.00000 -1.20000
AFIX 0
C75 1 -0.214079 0.651533 0.300342 11.00000 0.03043 0.02824 =
0.02969 -0.00977 0.00071 -0.01171
AFIX 43
H75 2 -0.266948 0.567204 0.346295 11.00000 -1.20000
AFIX 0
C76 1 -0.038763 0.679033 0.342975 11.00000 0.02783 0.02623 =
0.02704 -0.00695 -0.00389 -0.00671
AFIX 43
H76 2 0.027368 0.613064 0.417545 11.00000 -1.20000
AFIX 0
C8 1 0.332722 0.746155 0.430184 11.00000 0.02612 0.02513 =
0.02184 -0.00827 0.00000 -0.00817
AFIX 43
H8 2 0.288564 0.659736 0.479633 11.00000 -1.20000
AFIX 0
C9 1 0.504910 0.786127 0.465663 11.00000 0.02444 0.02752 =
0.02039 -0.01096 0.00013 -0.00487
C10 1 0.567262 0.913982 0.392350 11.00000 0.02187 0.02527 =
0.02281 -0.01291 0.00049 -0.00399
PART 1
O1N 4 0.668417 0.463765 0.887892 21.00000 0.03152 0.04246 =
0.02611 -0.00111 -0.00725 -0.00403
C1N 1 0.808609 0.388589 0.939255 21.00000 0.03137 0.02928 =
0.02258 -0.00546 -0.00267 -0.01118
H1N 2 0.890088 0.337908 0.891408 21.00000 -1.20000
PART 2
O1N' 4 0.737004 0.417792 0.859285 -21.00000 0.03018
C1N' 1 0.722384 0.437255 0.963860 -21.00000 0.02305
H1N' 2 0.629953 0.494634 0.978311 -21.00000 -1.20000
PART 0
N1N 3 0.864454 0.365145 1.061501 11.00000 0.04341 0.03272 =
0.02374 -0.00308 -0.00837 -0.01754
C2N 1 1.029640 0.271280 1.095992 11.00000 0.06313 0.03550 =
0.07994 -0.03446 0.03867 -0.01450
AFIX 137
H21N 2 1.060941 0.248621 1.022055 11.00000 -1.50000
H22N 2 0.998795 0.190547 1.172305 11.00000 -1.50000
H23N 2 1.141804 0.310677 1.117131 11.00000 -1.50000
AFIX 0
C3N 1 0.802921 0.409812 1.159382 11.00000 0.03817 0.03049 =
0.07383 -0.02228 0.01756 -0.00385
AFIX 137
H31N 2 0.699026 0.479858 1.123019 11.00000 -1.50000
H32N 2 0.913547 0.445116 1.187269 11.00000 -1.50000
H33N 2 0.754060 0.335043 1.234874 11.00000 -1.50000
AFIX 0
HKLF 4
REM pm in P-1
REM R1 = 0.0441 for 2827 Fo > 4sig(Fo) and 0.0474 for all 3149 data
REM 237 parameters refined using 0 restraints
END
WGHT 0.0680 0.2446
REM Instructions for potential hydrogen bonds
HTAB O1 O1N
HTAB O1 O1N'
HTAB N3 O4_$1
HTAB C2N O4_$2
HTAB C3N O1N_$3
REM Highest difference peak 0.262, deepest hole -0.527, 1-sigma level 0.048
Q1 1 0.5362 0.8512 0.4238 11.00000 0.05 0.26
Q2 1 0.1315 0.8180 0.3017 11.00000 0.05 0.25
Q3 1 0.5126 0.9608 0.3496 11.00000 0.05 0.25
Q4 1 0.5683 0.7466 0.5174 11.00000 0.05 0.25
Q5 1 0.6493 0.9362 0.4070 11.00000 0.05 0.25
;
_shelx_res_checksum 34601
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -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
O O1 0.56251(15) 0.57479(10) 0.64199(9) 0.0336(3) Uani d 1 . .
H H1 0.623980 0.537400 0.713697 0.050 Uiso calc 1 . .
C C1 0.6242(2) 0.69751(14) 0.57667(12) 0.0270(3) Uani d 1 . .
N N2 0.78400(17) 0.73073(12) 0.61302(11) 0.0290(3) Uani d 1 . .
N N3 0.83698(16) 0.85878(11) 0.54111(10) 0.0267(3) Uani d 1 . .
H H3 0.943753 0.881584 0.567844 0.032 Uiso calc 1 . .
O O4 0.81259(13) 1.06599(9) 0.38091(9) 0.0291(2) Uani d 1 . .
C C4 0.74557(18) 0.95407(13) 0.43446(12) 0.0239(3) Uani d 1 . .
C C5 0.45536(18) 0.99695(12) 0.27933(12) 0.0227(3) Uani d 1 . .
C C51 0.51416(19) 1.13221(13) 0.18729(13) 0.0279(3) Uani d 1 . .
H H51 0.430899 1.165143 0.108287 0.042 Uiso calc 1 . .
H H52 0.650440 1.126537 0.163166 0.042 Uiso calc 1 . .
H H53 0.499590 1.193383 0.230255 0.042 Uiso calc 1 . .
N N6 0.29158(15) 0.95746(10) 0.24670(10) 0.0232(2) Uani d 1 . .
C C7 0.22803(18) 0.83520(12) 0.32149(12) 0.0219(3) Uani d 1 . .
C C71 0.04117(18) 0.80255(12) 0.27739(12) 0.0222(3) Uani d 1 . .
C C72 -0.05964(19) 0.89735(13) 0.16785(12) 0.0238(3) Uani d 1 . .
H H72 -0.007941 0.982098 0.122002 0.029 Uiso calc 1 . .
C C73 -0.23431(19) 0.86939(13) 0.12510(12) 0.0258(3) Uani d 1 . .
H H73 -0.300666 0.934803 0.050269 0.031 Uiso calc 1 . .
C C74 -0.31231(19) 0.74614(14) 0.19136(13) 0.0266(3) Uani d 1 . .
H H74 -0.431782 0.726916 0.162254 0.032 Uiso calc 1 . .
C C75 -0.2141(2) 0.65153(14) 0.30034(13) 0.0298(3) Uani d 1 . .
H H75 -0.266948 0.567204 0.346295 0.036 Uiso calc 1 . .
C C76 -0.0388(2) 0.67903(13) 0.34298(13) 0.0282(3) Uani d 1 . .
H H76 0.027368 0.613064 0.417545 0.034 Uiso calc 1 . .
C C8 0.33272(19) 0.74615(13) 0.43018(12) 0.0246(3) Uani d 1 . .
H H8 0.288564 0.659736 0.479633 0.030 Uiso calc 1 . .
C C9 0.50491(18) 0.78613(13) 0.46566(12) 0.0236(3) Uani d 1 . .
C C10 0.56726(18) 0.91398(12) 0.39235(12) 0.0222(3) Uani d 1 . .
O O1N 0.6684(3) 0.4638(2) 0.88789(17) 0.0376(7) Uani d 0.611(5) A 1
C C1N 0.8086(4) 0.3886(2) 0.9393(2) 0.0291(7) Uani d 0.611(5) A 1
H H1N 0.890(4) 0.338(3) 0.891(3) 0.035 Uiso d 0.611(5) A 1
O O1N' 0.7370(4) 0.4178(3) 0.8593(3) 0.0302(9) Uiso d 0.389(5) A 2
C C1N' 0.7224(5) 0.4373(3) 0.9639(4) 0.0230(10) Uiso d 0.389(5) A 2
H H1N' 0.630(6) 0.495(4) 0.978(4) 0.028 Uiso d 0.389(5) A 2
N N1N 0.86445(19) 0.36515(12) 1.06150(11) 0.0355(3) Uani d 1 . .
C C2N 1.0296(3) 0.27128(17) 1.0960(2) 0.0557(5) Uani d 1 . .
H H21N 1.060941 0.248621 1.022055 0.083 Uiso calc 1 . .
H H22N 0.998795 0.190547 1.172305 0.083 Uiso calc 1 . .
H H23N 1.141804 0.310677 1.117131 0.083 Uiso calc 1 . .
C C3N 0.8029(2) 0.40981(16) 1.15938(19) 0.0472(4) Uani d 1 . .
H H31N 0.699026 0.479858 1.123019 0.071 Uiso calc 1 . .
H H32N 0.913547 0.445116 1.187269 0.071 Uiso calc 1 . .
H H33N 0.754060 0.335043 1.234874 0.071 Uiso calc 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 0.0351(5) 0.0328(5) 0.0236(5) -0.0133(4) -0.0083(4) -0.0009(4)
C1 0.0288(6) 0.0305(7) 0.0202(6) -0.0082(5) -0.0013(5) -0.0082(5)
N2 0.0305(6) 0.0308(6) 0.0226(5) -0.0089(5) -0.0041(4) -0.0071(5)
N3 0.0261(5) 0.0294(6) 0.0244(5) -0.0088(4) -0.0043(4) -0.0102(4)
O4 0.0282(5) 0.0268(5) 0.0324(5) -0.0079(4) -0.0054(4) -0.0115(4)
C4 0.0239(6) 0.0273(6) 0.0237(6) -0.0046(5) -0.0002(5) -0.0132(5)
C5 0.0226(6) 0.0224(6) 0.0258(6) -0.0030(5) -0.0002(5) -0.0123(5)
C51 0.0272(6) 0.0218(6) 0.0330(7) -0.0047(5) -0.0051(5) -0.0090(5)
N6 0.0223(5) 0.0214(5) 0.0262(5) -0.0036(4) -0.0014(4) -0.0100(4)
C7 0.0221(6) 0.0232(6) 0.0224(6) -0.0044(5) 0.0011(5) -0.0110(5)
C71 0.0225(6) 0.0239(6) 0.0224(6) -0.0047(5) 0.0008(5) -0.0114(5)
C72 0.0265(6) 0.0228(6) 0.0235(6) -0.0051(5) 0.0009(5) -0.0105(5)
C73 0.0258(6) 0.0285(7) 0.0244(6) -0.0021(5) -0.0030(5) -0.0121(5)
C74 0.0230(6) 0.0337(7) 0.0283(6) -0.0075(5) 0.0008(5) -0.0173(6)
C75 0.0304(7) 0.0282(7) 0.0297(7) -0.0117(5) 0.0007(5) -0.0098(5)
C76 0.0278(7) 0.0262(7) 0.0270(6) -0.0067(5) -0.0039(5) -0.0070(5)
C8 0.0261(6) 0.0251(6) 0.0218(6) -0.0082(5) 0.0000(5) -0.0083(5)
C9 0.0244(6) 0.0275(6) 0.0204(6) -0.0049(5) 0.0001(5) -0.0110(5)
C10 0.0219(6) 0.0253(6) 0.0228(6) -0.0040(5) 0.0005(5) -0.0129(5)
O1N 0.0315(10) 0.0425(11) 0.0261(10) -0.0040(8) -0.0073(7) -0.0011(8)
C1N 0.0314(13) 0.0293(12) 0.0226(12) -0.0112(10) -0.0027(9) -0.0055(9)
N1N 0.0434(7) 0.0327(6) 0.0237(6) -0.0175(5) -0.0084(5) -0.0031(5)
C2N 0.0631(11) 0.0355(8) 0.0799(13) -0.0145(8) 0.0387(10) -0.0345(9)
C3N 0.0382(8) 0.0305(8) 0.0738(12) -0.0038(6) 0.0176(8) -0.0223(8)
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
C1 O1 H1 . . 109.5 ?
N2 C1 O1 . . 119.90(12) ?
N2 C1 C9 . . 123.63(12) ?
O1 C1 C9 . . 116.47(11) ?
C1 N2 N3 . . 116.34(11) ?
C4 N3 N2 . . 128.17(10) ?
C4 N3 H3 . . 115.9 ?
N2 N3 H3 . . 115.9 ?
O4 C4 N3 . . 120.11(11) ?
O4 C4 C10 . . 124.99(11) ?
N3 C4 C10 . . 114.89(11) ?
N6 C5 C10 . . 121.55(11) ?
N6 C5 C51 . . 115.52(11) ?
C10 C5 C51 . . 122.91(11) ?
C5 C51 H51 . . 109.5 ?
C5 C51 H52 . . 109.5 ?
H51 C51 H52 . . 109.5 ?
C5 C51 H53 . . 109.5 ?
H51 C51 H53 . . 109.5 ?
H52 C51 H53 . . 109.5 ?
C5 N6 C7 . . 120.28(11) ?
N6 C7 C8 . . 121.79(11) ?
N6 C7 C71 . . 115.72(11) ?
C8 C7 C71 . . 122.48(11) ?
C76 C71 C72 . . 118.20(11) ?
C76 C71 C7 . . 121.91(11) ?
C72 C71 C7 . . 119.89(11) ?
C73 C72 C71 . . 120.95(12) ?
C73 C72 H72 . . 119.5 ?
C71 C72 H72 . . 119.5 ?
C72 C73 C74 . . 120.25(12) ?
C72 C73 H73 . . 119.9 ?
C74 C73 H73 . . 119.9 ?
C75 C74 C73 . . 119.33(12) ?
C75 C74 H74 . . 120.3 ?
C73 C74 H74 . . 120.3 ?
C74 C75 C76 . . 120.54(12) ?
C74 C75 H75 . . 119.7 ?
C76 C75 H75 . . 119.7 ?
C75 C76 C71 . . 120.73(12) ?
C75 C76 H76 . . 119.6 ?
C71 C76 H76 . . 119.6 ?
C7 C8 C9 . . 118.56(12) ?
C7 C8 H8 . . 120.7 ?
C9 C8 H8 . . 120.7 ?
C8 C9 C10 . . 120.02(12) ?
C8 C9 C1 . . 121.69(12) ?
C10 C9 C1 . . 118.28(11) ?
C9 C10 C5 . . 117.69(11) ?
C9 C10 C4 . . 118.63(11) ?
C5 C10 C4 . . 123.67(11) ?
O1N C1N N1N . . 120.2(2) ?
O1N C1N H1N . . 122.6(15) ?
N1N C1N H1N . . 117.2(15) ?
O1N' C1N' N1N . . 114.3(3) ?
O1N' C1N' H1N' . . 126(3) ?
N1N C1N' H1N' . . 120(2) ?
C1N N1N C3N . . 136.48(18) ?
C1N' N1N C3N . . 98.5(2) ?
C1N N1N C2N . . 107.44(18) ?
C1N' N1N C2N . . 145.4(2) ?
C3N N1N C2N . . 116.07(14) ?
N1N C2N H21N . . 109.5 ?
N1N C2N H22N . . 109.5 ?
H21N C2N H22N . . 109.5 ?
N1N C2N H23N . . 109.5 ?
H21N C2N H23N . . 109.5 ?
H22N C2N H23N . . 109.5 ?
N1N C3N H31N . . 109.5 ?
N1N C3N H32N . . 109.5 ?
H31N C3N H32N . . 109.5 ?
N1N C3N H33N . . 109.5 ?
H31N C3N H33N . . 109.5 ?
H32N C3N H33N . . 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
O1 C1 . 1.3383(16) ?
O1 H1 . 0.8400 ?
C1 N2 . 1.2942(17) ?
C1 C9 . 1.4485(18) ?
N2 N3 . 1.3759(15) ?
N3 C4 . 1.3532(17) ?
N3 H3 . 0.8800 ?
O4 C4 . 1.2430(15) ?
C4 C10 . 1.4671(16) ?
C5 N6 . 1.3325(16) ?
C5 C10 . 1.4188(17) ?
C5 C51 . 1.4990(17) ?
C51 H51 . 0.9800 ?
C51 H52 . 0.9800 ?
C51 H53 . 0.9800 ?
N6 C7 . 1.3569(16) ?
C7 C8 . 1.3837(18) ?
C7 C71 . 1.4908(17) ?
C71 C76 . 1.3965(17) ?
C71 C72 . 1.3983(18) ?
C72 C73 . 1.3892(18) ?
C72 H72 . 0.9500 ?
C73 C74 . 1.3893(18) ?
C73 H73 . 0.9500 ?
C74 C75 . 1.3859(19) ?
C74 H74 . 0.9500 ?
C75 C76 . 1.3905(18) ?
C75 H75 . 0.9500 ?
C76 H76 . 0.9500 ?
C8 C9 . 1.3982(17) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.3984(17) ?
O1N C1N . 1.215(4) ?
C1N N1N . 1.339(2) ?
C1N H1N . 1.06(3) ?
O1N' C1N' . 1.279(6) ?
C1N' N1N . 1.412(4) ?
C1N' H1N' . 0.94(4) ?
N1N C3N . 1.431(2) ?
N1N C2N . 1.437(2) ?
C2N H21N . 0.9800 ?
C2N H22N . 0.9800 ?
C2N H23N . 0.9800 ?
C3N H31N . 0.9800 ?
C3N H32N . 0.9800 ?
C3N H33N . 0.9800 ?
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 O1N . 0.84 1.80 2.6006(19) 159.1 yes
O1 H1 O1N' . 0.84 1.77 2.588(3) 163.8 yes
N3 H3 O4 2_776 0.88 1.96 2.8413(14) 177.2 yes
C75 H75 O1 2_566 0.95 2.60 3.4161(16) 144.3 yes
C2N H22N O4 1_546 0.98 2.55 3.450(2) 152.7 yes
C3N H31N O1N 2_667 0.98 2.56 3.415(3) 145.7 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 C1 N2 N3 . . . . -179.77(11) ?
C9 C1 N2 N3 . . . . 1.1(2) ?
C1 N2 N3 C4 . . . . -1.9(2) ?
N2 N3 C4 O4 . . . . 179.58(12) ?
N2 N3 C4 C10 . . . . 0.41(19) ?
C10 C5 N6 C7 . . . . -0.34(19) ?
C51 C5 N6 C7 . . . . 178.26(11) ?
C5 N6 C7 C8 . . . . -2.37(19) ?
C5 N6 C7 C71 . . . . 178.79(10) ?
N6 C7 C71 C76 . . . . 178.28(11) ?
C8 C7 C71 C76 . . . . -0.6(2) ?
N6 C7 C71 C72 . . . . -2.10(17) ?
C8 C7 C71 C72 . . . . 179.06(12) ?
C76 C71 C72 C73 . . . . -0.19(19) ?
C7 C71 C72 C73 . . . . -179.82(11) ?
C71 C72 C73 C74 . . . . 0.3(2) ?
C72 C73 C74 C75 . . . . 0.0(2) ?
C73 C74 C75 C76 . . . . -0.3(2) ?
C74 C75 C76 C71 . . . . 0.3(2) ?
C72 C71 C76 C75 . . . . -0.1(2) ?
C7 C71 C76 C75 . . . . 179.50(12) ?
N6 C7 C8 C9 . . . . 2.31(19) ?
C71 C7 C8 C9 . . . . -178.93(11) ?
C7 C8 C9 C10 . . . . 0.42(19) ?
C7 C8 C9 C1 . . . . -178.78(11) ?
N2 C1 C9 C8 . . . . -179.75(12) ?
O1 C1 C9 C8 . . . . 1.09(19) ?
N2 C1 C9 C10 . . . . 1.0(2) ?
O1 C1 C9 C10 . . . . -178.11(11) ?
C8 C9 C10 C5 . . . . -2.92(18) ?
C1 C9 C10 C5 . . . . 176.30(11) ?
C8 C9 C10 C4 . . . . 178.26(11) ?
C1 C9 C10 C4 . . . . -2.52(18) ?
N6 C5 C10 C9 . . . . 2.95(18) ?
C51 C5 C10 C9 . . . . -175.54(11) ?
N6 C5 C10 C4 . . . . -178.30(11) ?
C51 C5 C10 C4 . . . . 3.21(19) ?
O4 C4 C10 C9 . . . . -177.28(12) ?
N3 C4 C10 C9 . . . . 1.84(17) ?
O4 C4 C10 C5 . . . . 4.0(2) ?
N3 C4 C10 C5 . . . . -176.90(11) ?
O1N C1N N1N C3N . . . . -1.8(3) ?
O1N C1N N1N C2N . . . . 178.81(19) ?
O1N' C1N' N1N C3N . . . . -179.6(2) ?
O1N' C1N' N1N C2N . . . . -0.9(5) ?