#------------------------------------------------------------------------------
#$Date: 2024-06-29 04:57:55 +0300 (Sat, 29 Jun 2024) $
#$Revision: 292657 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023183.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_2023183
loop_
_publ_author_name
'Hayward, Emily R.'
'Zeller, Matthias'
'Mezei, Gellert'
_publ_section_title
;
Chiral versus achiral crystal structures of 4-benzyl-1H-pyrazole and its
3,5-diamino derivative
;
_journal_issue 7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 800
_journal_page_last 805
_journal_paper_doi 10.1107/S2056989024006182
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C10 H12 N4'
_chemical_formula_moiety 'C10 H12 N4'
_chemical_formula_sum 'C10 H12 N4'
_chemical_formula_weight 188.24
_chemical_name_systematic
;
3,5-Diamino-4-benzyl-1H-pyrazole
;
_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
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 98.247(6)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.410(2)
_cell_length_b 4.7271(7)
_cell_length_c 11.4664(15)
_cell_measurement_reflns_used 7332
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 79.3378
_cell_measurement_theta_min 5.1342
_cell_volume 933.9(2)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2020)
;
_computing_data_collection
;
APEX5 v2023.9-2 (Bruker, 2023)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2020)
;
_computing_molecular_graphics
'CrystalMaker (CrystalMaker Software, 2003)'
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b),
ShelXle Rev1613 (H\"ubschle et al., 2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device 'four circle diffractometer'
_diffrn_measurement_device_type 'Bruker AXS D8 Quest'
_diffrn_measurement_method 'omega and phi scans'
_diffrn_radiation_monochromator 'HELIOS multilayer Montel optics'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0626
_diffrn_reflns_av_unetI/netI 0.0524
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 5
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 10090
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 79.784
_diffrn_reflns_theta_min 5.134
_diffrn_source 'I-mu-S 3.0 microsource X-ray tube'
_diffrn_source_current '1.1 mA'
_diffrn_source_voltage '50 kV'
_exptl_absorpt_coefficient_mu 0.685
_exptl_absorpt_correction_T_max 0.7543
_exptl_absorpt_correction_T_min 0.5428
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.339
_exptl_crystal_description block
_exptl_crystal_F_000 400
_exptl_crystal_size_max 0.230
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.110
_refine_diff_density_max 0.212
_refine_diff_density_min -0.204
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 142
_refine_ls_number_reflns 1963
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.026
_refine_ls_R_factor_all 0.0430
_refine_ls_R_factor_gt 0.0376
_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^)+(0.0335P)^2^+0.2938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0932
_refine_ls_wR_factor_ref 0.0952
_reflns_number_gt 1817
_reflns_number_total 1963
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2305.cif
_cod_data_source_block 2
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2023183
_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 0.858
_shelx_estimated_absorpt_t_max 0.928
_shelx_hkl_file
;
-2 0 0 348.860 28.0043 1
2 0 0 331.963 28.8156 2
-3 0 0 15.2879 1.62879 1
-3 0 0 13.6866 1.51208 8
3 0 0 8.31142 3.24135 2
4 0 0 7436.00 608.106 2
5 0 0 83.4587 11.5419 2
5 0 0 87.9407 7.69669 8
-5 0 0 89.7240 7.63592 1
-5 0 0 84.4236 7.61672 8
6 0 0 456.745 40.4947 2
6 0 0 451.999 37.7644 8
7 0 0 19.3767 2.70881 8
7 0 0 35.6398 10.2290 2
-7 0 0 27.2915 3.07484 1
-7 0 0 18.1890 2.85608 8
8 0 0 834.385 75.7117 2
-9 0 0 101.127 9.23432 1
-9 0 0 94.1243 9.00360 8
9 0 0 87.5795 26.5954 2
10 0 0 19.3318 1.69994 5
-10 0 0 18.2053 1.72512 5
-10 0 0 21.3461 3.12653 8
-10 0 0 20.9864 4.88600 1
10 0 0 9.55363 14.2293 2
-11 0 0 54.1809 4.56117 4
-11 0 0 63.3733 6.16662 8
-11 0 0 44.4915 4.44070 5
11 0 0 24.0658 19.9137 2
-11 0 0 59.1739 6.90735 1
12 0 0 164.489 37.3704 2
-12 0 0 342.196 26.1552 4
-12 0 0 340.348 27.9113 1
-12 0 0 269.350 26.0316 5
-12 0 0 365.578 27.8661 8
-13 0 0 22.2037 5.06801 1
13 0 0 -13.402 31.4631 2
13 0 0 23.6041 2.17335 4
13 0 0 23.0524 2.03328 5
-13 0 0 22.6838 2.19850 4
-14 0 0 114.278 9.00972 4
14 0 0 109.332 8.87982 5
-14 0 0 89.1161 12.6068 1
-15 0 0 548.437 55.9679 1
15 0 0 709.226 53.7067 4
-15 0 0 700.139 53.7049 4
-16 0 0 6.50022 7.47393 1
-16 0 0 16.3042 1.86301 4
16 0 0 18.7976 1.81656 4
16 0 0 17.7395 1.61296 5
-17 0 0 92.0275 7.17941 4
-17 0 0 30.7347 15.0562 1
17 0 0 89.2073 7.15234 4
-18 0 0 25.3891 2.39263 4
-19 0 0 129.395 10.7185 4
-20 0 0 3.31544 0.61176 4
-21 0 0 18.0378 1.75978 4
0 -1 0 0.61232 0.46818 8
0 1 0 0.34429 0.32016 6
-1 -1 0 1.94060 0.62736 8
1 1 0 0.66557 0.35237 6
1 1 0 0.32260 2.11023 2
1 1 0 1.95058 0.40030 1
-1 1 0 0.50102 0.40426 6
-2 -1 0 11.5449 1.57849 8
2 1 0 11.7661 1.31558 6
2 1 0 13.0143 1.52590 1
-2 1 0 11.3973 1.24306 6
-2 1 0 12.9294 1.27811 1
-2 1 0 16.2886 3.52533 2
2 1 0 19.4260 3.64359 2
-3 1 0 4876.93 398.671 2
3 1 0 4982.01 398.884 2
-3 1 0 4764.93 397.626 1
-4 1 0 2165.83 192.206 2
-4 1 0 2381.69 189.836 1
4 1 0 2418.23 191.519 2
5 -1 0 145.572 12.6776 8
-5 -1 0 145.659 12.9795 8
-5 1 0 159.776 12.6764 1
5 1 0 161.963 13.5300 8
-5 1 0 134.151 12.4581 6
5 1 0 166.690 15.9521 2
-5 1 0 142.053 22.0933 2
-6 -1 0 1454.88 116.667 1
6 -1 0 1394.52 116.109 8
-6 1 0 1446.25 116.054 1
6 1 0 1366.53 118.514 2
7 -1 0 1155.68 97.7640 8
-7 -1 0 1140.28 98.0331 1
-7 1 0 1264.19 97.7147 1
7 1 0 1204.41 100.895 2
8 -1 0 1021.76 86.8503 8
-8 -1 0 1003.46 87.1404 1
8 -1 0 978.915 86.0642 5
-8 -1 0 1117.24 87.2394 8
-8 1 0 1167.79 86.7991 1
8 1 0 1034.51 90.5217 2
-9 -1 0 28.3319 2.58375 5
-9 -1 0 34.5349 4.05087 8
9 -1 0 29.2850 2.57308 5
-9 -1 0 31.7990 8.17015 1
9 1 0 26.8082 10.8531 2
-9 1 0 30.2090 3.90022 1
10 -1 0 173.129 14.6326 5
-10 -1 0 159.671 17.3717 1
-10 -1 0 198.743 16.2978 8
-10 -1 0 174.179 14.6377 5
10 1 0 178.385 27.9223 2
-10 1 0 168.849 14.9971 6
-10 1 0 193.398 15.7746 1
-11 -1 0 783.831 67.8328 1
-11 -1 0 848.968 67.5475 8
-11 -1 0 794.189 65.7808 5
11 1 0 831.411 65.8405 4
-11 1 0 792.444 65.8117 4
-11 1 0 790.174 66.8567 1
-11 1 0 795.326 66.1884 6
-12 -1 0 7.16620 3.44614 8
12 -1 0 6.69163 0.78426 5
-12 -1 0 4.68408 8.63861 1
-12 -1 0 3.96964 0.81052 4
-12 -1 0 6.60824 0.85425 5
12 1 0 6.44539 0.89772 4
-12 1 0 5.09655 0.88834 4
12 1 0 -0.0743 20.3135 2
-12 1 0 4.71909 2.70392 1
-12 1 0 6.80183 1.27564 6
-13 -1 0 282.429 23.0539 4
13 -1 0 292.455 22.9477 5
-13 -1 0 284.024 22.9395 5
-13 1 0 287.737 23.0195 4
13 1 0 285.701 23.0311 4
13 1 0 337.253 46.5064 2
-13 1 0 268.197 24.5772 1
-13 1 0 253.494 23.1374 7
-13 1 0 277.729 23.4962 6
-14 -1 0 523.344 40.8786 4
-14 -1 0 511.493 40.7498 5
14 1 0 514.875 40.8425 4
-14 1 0 452.269 42.4466 1
14 1 0 401.637 66.0740 2
-14 1 0 501.154 40.8202 4
-15 -1 0 274.669 21.6147 4
15 -1 0 259.261 21.5878 4
-15 -1 0 256.985 21.4647 5
15 1 0 113.823 40.9047 2
-15 1 0 261.086 23.9423 1
-15 1 0 267.435 21.5583 4
15 1 0 268.091 21.5723 4
-16 1 0 -0.7543 4.71009 1
16 1 0 83.1885 58.1536 2
-17 -1 0 89.2828 7.29242 4
17 -1 0 87.8243 7.14770 5
-17 1 0 61.3179 12.7518 1
-17 1 0 88.5965 7.24669 4
17 1 0 85.9884 7.23861 4
-18 -1 0 66.2738 5.89108 4
18 -1 0 69.5063 5.76388 5
-18 1 0 72.4288 5.86381 4
-19 -1 0 0.26055 0.52303 4
-19 1 0 -0.0004 0.58198 4
-20 -1 0 2.80919 0.56457 4
20 1 0 3.16322 0.44150 10
-20 1 0 3.11974 0.51850 4
-21 -1 0 52.6189 4.75359 4
-21 1 0 60.0989 4.67920 4
1 -2 0 190.774 16.7386 8
-1 2 0 203.007 16.4751 6
-2 -2 0 0.82636 0.86411 8
2 -2 0 4.49857 1.16177 8
2 2 0 -2.1556 3.13757 2
-2 2 0 5.15154 0.95316 6
2 2 0 0.44229 0.59246 6
3 -2 0 256.702 21.5124 11
-3 -2 0 256.343 21.9330 8
-3 2 0 259.804 21.3775 6
3 2 0 264.158 21.4855 6
3 2 0 258.328 22.8678 2
3 2 0 247.873 21.2990 1
4 -2 0 137.487 12.3593 8
-4 -2 0 157.322 12.9755 8
4 -2 0 126.343 12.4175 11
-4 2 0 157.424 12.2882 6
4 2 0 147.417 12.4807 1
-5 -2 0 3.95260 1.36506 8
5 -2 0 4.16633 1.26329 8
5 2 0 5.91945 6.17255 2
-5 2 0 6.75808 1.30927 1
5 2 0 5.33302 2.04125 1
-5 2 0 5.06693 1.07825 6
-5 2 0 3.84658 1.12796 1
6 -2 0 887.269 79.0943 8
-6 -2 0 999.773 79.9264 8
-6 -2 0 808.946 78.6391 5
-6 2 0 1048.02 79.1289 6
6 2 0 991.410 79.4943 1
-6 2 0 976.716 79.0237 1
6 2 0 1059.27 82.4164 2
-7 -2 0 11.9617 1.29907 5
7 -2 0 17.1116 2.10723 8
-7 -2 0 14.1745 2.71420 8
7 2 0 17.7399 8.87251 2
-7 2 0 12.8470 1.70576 6
-7 2 0 15.0585 2.35108 1
-8 -2 0 345.986 29.2794 5
8 -2 0 317.564 29.2640 5
-8 -2 0 361.229 30.8692 8
-8 2 0 364.499 29.7191 6
-8 2 0 390.319 29.9743 1
8 2 0 391.341 36.0702 2
-9 -2 0 40.5196 5.14951 8
-9 -2 0 38.1186 3.37363 5
9 -2 0 39.3187 3.31233 5
-9 2 0 36.5458 3.32708 4
9 2 0 35.5944 12.9600 2
-9 2 0 43.1618 4.58337 1
-9 2 0 39.4521 3.78365 6
-10 -2 0 6.68090 2.37054 8
-10 -2 0 8.51807 0.89945 5
10 -2 0 8.88979 0.81071 5
-10 2 0 4.50033 2.03744 1
-10 2 0 5.80293 1.28625 6
-10 2 0 4.55134 0.76558 3
-10 2 0 5.12159 0.79674 4
10 2 0 5.81516 0.85130 4
-10 2 0 4.85976 0.82663 7
10 2 0 18.6215 14.4979 2
-11 -2 0 25.7644 2.28476 5
11 -2 0 26.3527 2.23927 5
-11 2 0 22.9399 2.31602 7
11 2 0 25.7567 2.30283 4
11 2 0 15.0668 16.1508 2
-11 2 0 24.5859 2.24180 3
-11 2 0 26.9327 2.98905 6
-11 2 0 24.4196 2.26499 4
-11 2 0 27.4132 4.16462 1
12 -2 0 415.246 34.7114 5
-12 -2 0 450.110 34.7336 5
-12 2 0 395.431 34.8090 7
12 2 0 328.980 48.1262 2
12 2 0 434.983 34.7773 4
-12 2 0 449.508 35.9703 1
-12 2 0 426.105 34.7970 4
-13 -2 0 3.59038 0.69316 5
13 -2 0 5.61366 0.81615 5
-13 2 0 2.22492 2.93950 1
-13 2 0 4.01619 0.73174 7
-13 2 0 4.91611 0.68794 3
13 2 0 5.80161 0.81778 4
13 2 0 5.65525 23.0872 2
-13 2 0 4.73424 0.73250 4
-14 -2 0 1.58785 1.40047 4
14 -2 0 2.98828 0.56165 5
-14 -2 0 2.60616 0.59879 5
-14 2 0 4.31235 3.27062 1
-14 2 0 2.30330 0.52539 3
-14 2 0 2.68065 0.60348 4
14 2 0 32.2712 30.4608 2
14 2 0 2.78035 0.64427 4
-15 -2 0 26.5601 2.15230 5
-15 -2 0 21.4899 2.41836 4
15 2 0 19.7161 2.50319 4
-15 2 0 23.4377 2.06975 3
-15 2 0 23.9569 4.70747 1
15 2 0 44.9441 36.8586 2
-16 -2 0 10.9175 1.48789 4
-16 2 0 11.1892 7.42290 1
16 2 0 36.3662 37.6434 2
-16 2 0 13.1938 1.30840 4
17 -2 0 57.8399 4.35761 5
-17 -2 0 45.5856 4.44270 4
-17 -2 0 49.3415 4.32999 5
-17 2 0 52.6642 4.36856 4
17 2 0 53.1233 4.42895 10
18 -2 0 72.1665 5.39502 5
-18 -2 0 49.3187 5.46342 4
-18 2 0 67.4706 5.39531 4
18 2 0 70.0534 5.46005 10
19 -2 0 55.1089 4.25674 5
19 2 0 49.1503 4.27208 10
-19 2 0 48.7629 4.28026 4
20 2 0 23.1250 2.04682 10
0 -3 0 0.81444 1.09785 8
0 3 0 0.60529 0.75259 6
0 3 0 0.29232 0.37077 7
0 3 0 0.28059 0.48534 9
-1 -3 0 194.856 17.9649 8
1 -3 0 199.715 17.8558 8
1 3 0 203.644 16.8772 10
1 3 0 209.704 17.3954 6
1 3 0 201.434 16.7775 9
-1 3 0 207.070 17.3339 6
1 3 0 204.596 16.8542 7
-1 3 0 207.292 16.7845 9
-1 3 0 203.054 16.8419 7
-2 -3 0 13.1106 3.95793 8
2 -3 0 12.9849 2.28738 11
2 -3 0 13.7378 2.53157 8
2 3 0 12.5916 1.33868 9
2 3 0 18.7152 2.16398 6
2 3 0 11.9007 1.39971 7
-2 3 0 12.3433 1.35451 9
-2 3 0 14.3225 1.90636 6
-2 3 0 12.6078 1.37177 7
-2 3 0 12.0168 1.25295 3
2 3 0 11.2986 1.30459 10
-3 -3 0 68.0360 7.89059 8
3 -3 0 68.7242 7.38554 8
-3 3 0 79.6409 6.64227 10
-3 3 0 81.4196 6.66208 7
3 3 0 76.5519 6.59244 10
3 3 0 98.9020 6.87326 9
3 3 0 73.9422 6.94336 7
-3 3 0 74.3648 6.52829 3
-3 3 0 83.2674 7.16164 6
-3 3 0 79.5376 6.60344 9
-4 -3 0 76.9840 8.85388 8
-4 3 0 95.6076 8.04710 6
4 3 0 91.2897 7.58727 7
-4 3 0 90.6382 7.48187 9
-4 3 0 91.9760 7.59617 7
-4 3 0 91.0167 7.45611 10
4 3 0 85.8589 7.48334 10
-4 3 0 89.5417 7.42689 3
-5 -3 0 76.5025 8.83740 5
-5 -3 0 95.5001 10.5258 8
-5 3 0 108.763 8.90164 3
5 3 0 105.749 8.95320 9
-5 3 0 133.996 9.15059 9
-5 3 0 109.709 9.49319 6
-5 3 0 117.658 9.00904 10
5 3 0 107.223 8.96183 10
-5 3 0 108.092 9.03474 7
5 3 0 112.750 9.09282 7
-6 -3 0 55.5806 7.99648 8
-6 3 0 60.8171 4.86306 3
6 3 0 58.0766 4.92239 10
6 3 0 48.0730 12.7953 2
-6 3 0 60.3944 4.98088 7
-6 3 0 57.5244 4.87700 10
6 3 0 56.5480 4.90800 9
-6 3 0 52.2901 5.02838 9
6 3 0 56.6377 5.04422 7
-6 3 0 59.5569 5.45406 6
6 3 0 59.6826 10.1303 2
-7 -3 0 42.9108 3.52160 5
-7 -3 0 44.4354 6.01713 8
7 3 0 19.1439 11.3779 2
-7 3 0 40.3292 4.11558 6
7 3 0 39.4710 3.59281 9
-7 3 0 43.9121 3.54380 3
-7 3 0 41.6805 3.64950 7
-7 3 0 38.5528 3.55979 9
7 3 0 71.3927 20.2534 2
-7 3 0 38.4211 3.53954 10
7 3 0 42.3945 3.61408 10
-8 -3 0 48.7982 4.04754 5
8 -3 0 44.2802 3.99310 5
-8 3 0 45.8472 4.07247 10
8 3 0 40.6988 4.09928 9
8 3 0 64.9538 14.2363 2
-8 3 0 49.8499 4.17094 7
-8 3 0 50.9390 4.90560 6
-8 3 0 56.5321 4.13494 3
8 3 0 53.3481 4.20848 10
-8 3 0 39.7508 4.08635 9
8 3 0 6.47811 29.2205 2
-9 -3 0 892.083 68.6015 5
9 -3 0 881.034 68.5755 5
9 3 0 904.394 75.0570 2
-9 3 0 905.425 68.6152 3
-9 3 0 867.708 68.8469 7
9 3 0 884.114 68.7060 10
9 3 0 567.881 68.6324 9
-10 -3 0 226.553 17.9295 5
-10 3 0 219.050 17.9205 3
-10 3 0 206.710 18.0207 7
10 3 0 227.874 31.3869 2
10 3 0 217.816 18.0135 10
-11 -3 0 25.5082 2.27391 5
11 -3 0 24.3313 2.16375 5
11 3 0 24.4300 2.29697 10
11 3 0 29.7218 20.9031 2
-11 3 0 23.8750 2.19088 3
-11 3 0 22.4298 2.25728 7
-12 -3 0 5.53618 0.77792 5
12 -3 0 5.32220 0.69145 5
-12 3 0 4.66961 0.72274 3
12 3 0 25.9290 23.0612 2
12 3 0 5.57394 0.89056 10
-12 3 0 4.06588 0.81741 7
13 -3 0 98.2329 8.04557 5
-13 -3 0 103.755 8.08692 5
13 3 0 96.2818 8.15266 10
-13 3 0 96.2341 8.05924 3
-13 3 0 90.3997 8.27066 7
13 3 0 85.1063 28.9797 2
14 3 0 48.7441 4.15029 10
-14 3 0 46.9758 4.05893 3
14 3 0 59.8993 31.2075 2
-15 -3 0 6.52888 0.91634 5
15 3 0 5.99283 0.82220 10
-15 3 0 6.69294 0.99888 3
-16 -3 0 0.66390 0.42272 5
16 -3 0 0.45732 0.36383 5
-16 3 0 0.90378 0.34585 3
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12 1 -12 0.33614 0.25057 4
11 -1 -12 3.31398 0.56924 4
-11 -1 12 2.96468 0.53805 4
11 1 -12 3.48663 0.57231 4
-11 1 12 4.00632 0.62970 4
-10 -1 12 67.2422 6.14407 4
-10 1 12 73.5740 6.00097 4
10 1 -12 74.1368 6.01414 4
9 -1 -12 38.0906 3.63083 4
-9 -1 12 37.0882 3.59964 4
-9 1 12 50.3703 3.68755 4
9 1 -12 43.7479 3.65428 4
-8 -1 12 9.00727 1.06850 4
8 -1 -12 9.48614 1.13262 4
-8 1 12 10.1186 1.07078 4
8 1 -12 8.95567 0.95481 9
8 1 -12 10.0773 1.09560 4
-7 -1 12 63.2737 5.36384 4
7 -1 -12 63.1908 5.38472 4
7 1 -12 67.4191 5.37575 4
7 1 -12 60.2146 5.29084 9
6 -1 -12 45.1660 3.59163 4
-6 -1 12 40.2563 3.54010 4
6 1 -12 44.5191 3.55477 4
6 1 -12 32.8892 3.65286 9
5 -1 -12 22.0413 2.53745 4
5 1 -12 27.4643 2.38664 4
5 1 -12 27.5631 2.32438 9
4 -1 -12 8.04747 1.16664 4
4 1 -12 5.51129 0.89669 4
4 1 -12 6.09659 0.81526 9
-3 -1 12 142.638 11.4952 5
3 -1 -12 156.582 11.6252 4
3 1 -12 128.338 11.5001 9
3 1 -12 129.229 11.5121 4
2 -1 -12 162.706 12.6116 4
-2 -1 12 152.020 12.5108 5
2 1 -12 142.323 12.5264 9
2 1 -12 149.228 12.5404 4
1 -1 -12 29.1838 2.54872 4
-1 -1 12 26.1025 2.36147 5
1 1 -12 25.7295 2.37576 9
1 1 -12 24.8685 2.38386 4
0 -1 12 1.12262 0.52088 5
0 -1 -12 1.65086 0.78525 4
0 1 -12 1.42432 0.47420 9
0 1 -12 1.62345 0.47155 4
-1 -1 -12 1.75855 0.67937 4
-1 1 -12 1.23102 0.43659 9
-1 1 -12 1.69366 0.49276 4
-2 -1 -12 41.8363 3.61187 4
-2 1 -12 40.1834 3.56358 4
-2 1 -12 41.5442 3.54859 9
-3 -1 -12 71.7980 6.33127 4
-3 1 -12 82.1194 6.33185 9
-3 1 -12 70.9933 6.29063 4
-4 -1 -12 23.8786 2.24619 4
-4 1 -12 25.1833 2.17671 9
-4 1 -12 24.2194 2.21221 4
-5 -1 -12 5.64249 0.88455 4
-5 1 -12 6.79483 0.80905 4
-5 1 -12 7.17007 0.76144 9
-6 -1 -12 0.49850 0.48631 4
-6 1 -12 0.10461 0.26668 9
-6 1 -12 0.16709 0.28713 4
-7 -1 -12 3.98456 0.63060 4
-7 1 -12 4.13480 0.58417 4
-7 1 -12 4.60879 0.50203 9
-8 -1 -12 19.9084 1.94366 4
-8 1 -12 22.9715 1.85926 4
-9 1 -12 15.0612 1.30989 4
-12 2 12 101.963 8.36201 3
-11 2 12 3.03733 0.44909 4
11 2 -12 3.05044 0.42651 4
-11 2 12 2.95314 0.43757 3
-10 2 12 32.6944 2.92593 4
-10 2 12 34.1195 2.88626 3
10 2 -12 36.2149 2.93730 4
-9 2 12 119.098 9.37664 3
9 2 -12 113.908 9.39397 4
-9 2 12 109.203 9.38451 4
-8 2 12 20.9580 1.78940 3
-8 2 12 20.2754 1.81612 4
8 2 -12 20.4129 1.81609 4
-7 -2 12 19.8499 1.67565 5
7 2 -12 15.9597 1.60092 9
-7 2 12 19.2597 1.59599 3
-7 2 12 17.6803 1.63816 4
7 2 -12 18.2767 1.64334 4
-6 -2 12 8.42896 0.94953 5
-6 2 12 8.58141 0.91981 4
6 2 -12 7.13031 0.83271 9
6 2 -12 9.17132 0.93017 4
-6 2 12 8.52600 0.83915 3
-5 -2 12 11.5177 1.21738 5
5 -2 -12 10.8386 1.13012 5
5 2 -12 11.3367 1.12815 4
-5 2 12 11.2124 1.04798 3
5 2 -12 11.0116 1.09253 9
4 -2 -12 5.52410 0.72790 5
-4 -2 12 4.58608 0.84924 5
-4 2 12 5.61180 0.61290 3
4 2 -12 5.06323 0.67337 9
4 2 -12 4.58503 0.70892 4
-3 -2 12 70.6373 5.19536 5
3 -2 -12 56.9551 5.02623 5
3 2 -12 57.2040 5.05563 9
3 2 -12 57.8579 5.05166 4
2 -2 -12 55.5678 4.97471 5
2 2 -12 60.9823 5.01762 4
2 2 -12 62.3549 5.03225 9
1 -2 -12 16.5980 1.67160 5
1 2 -12 19.4379 1.68023 9
1 2 -12 16.7641 1.62001 4
0 2 -12 97.0558 8.08592 4
0 2 -12 98.2071 8.11045 9
1 -2 12 0.47724 0.36399 5
-1 2 -12 0.58983 0.42341 4
-1 2 -12 0.27943 0.36452 9
2 -2 12 354.062 30.1661 5
-2 2 -12 364.575 30.1658 4
-2 2 -12 387.639 30.2024 9
3 -2 12 115.637 10.3531 5
-3 2 -12 123.152 10.3039 4
-3 2 -12 136.918 10.3469 9
-4 2 -12 0.96737 0.33508 9
-5 2 -12 0.66286 0.32895 9
-6 2 -12 8.44535 0.86194 9
5 3 -12 14.8516 1.36147 9
4 3 -12 54.6524 4.53616 9
3 3 -12 53.0547 4.41517 9
-2 -3 12 56.3280 4.62893 5
2 3 -12 53.3018 4.56388 9
-1 -3 12 2.45279 0.56774 5
1 3 -12 2.07906 0.40293 9
0 3 -12 38.6472 3.24738 9
-1 3 -12 8.19858 0.78977 9
-2 3 -12 31.5767 2.65139 9
-3 3 -12 37.7361 3.14239 9
12 0 -13 0.07565 0.13894 4
-12 0 13 0.10089 0.30931 4
-11 0 13 0.40116 0.40416 4
11 0 -13 0.46424 0.39210 4
-10 0 13 0.17219 0.32085 4
10 0 -13 0.01953 0.37513 4
9 0 -13 0.12677 0.41267 4
-9 0 13 0.08401 0.39560 4
-8 0 13 0.11890 0.35966 4
8 0 -13 0.13640 0.38297 4
-7 0 13 0.06080 0.35720 4
7 0 -13 0.10592 0.29523 4
7 0 -13 0.12891 0.21126 9
-6 0 13 -0.3641 0.32252 4
6 0 -13 -0.0064 0.24087 9
6 0 -13 -0.1151 0.35856 4
5 0 -13 0.30731 0.31099 9
5 0 -13 0.04498 0.31457 4
4 0 -13 0.22000 0.37877 4
3 0 -13 0.13887 0.40842 4
2 0 -13 0.58787 0.37777 4
1 0 -13 -0.0651 0.34251 4
0 0 -13 0.04793 0.34351 4
-1 0 -13 0.12712 0.37759 4
-2 0 -13 -0.0363 0.35630 4
-3 0 -13 0.17170 0.32607 4
-4 0 -13 -0.1073 0.29239 4
-4 0 -13 0.18200 0.22590 9
-5 0 -13 -0.0223 0.32341 4
-5 0 -13 0.06932 0.22979 9
-6 0 -13 -0.1991 0.23004 4
-6 0 -13 -0.0204 0.28583 9
-7 0 -13 -0.0530 0.17881 4
-12 1 13 3.36058 0.47070 4
12 1 -13 3.14630 0.47427 4
-12 1 13 3.74033 0.43139 3
11 1 -13 60.6611 4.96441 4
-11 1 13 63.8367 4.93865 3
-11 1 13 55.2113 4.94830 4
-10 1 13 144.278 9.74860 3
10 1 -13 106.340 9.81295 4
-10 1 13 104.488 9.76427 4
9 -1 -13 -0.2836 0.37483 4
-9 1 13 0.25379 0.28209 4
9 1 -13 0.51479 0.29255 4
-8 -1 13 0.40082 0.50770 4
8 -1 -13 0.68467 0.28421 4
8 1 -13 1.20098 0.35483 4
-8 1 13 2.04540 0.40220 4
7 -1 -13 30.5165 2.76084 4
-7 -1 13 28.0961 2.73524 4
7 1 -13 33.6995 2.73738 4
-7 1 13 33.9102 2.73065 4
-6 -1 13 72.6526 6.52422 4
6 -1 -13 79.0585 6.57469 4
6 1 -13 75.5552 6.58031 9
-6 1 13 79.7026 6.52816 4
6 1 -13 85.6267 6.55543 4
-5 -1 13 0.31228 0.37034 4
5 -1 -13 0.33565 0.43093 4
5 1 -13 -0.0211 0.36331 4
5 1 -13 0.22239 0.26631 9
-4 -1 13 1.44819 0.43033 4
4 -1 -13 1.68096 0.46717 4
4 1 -13 2.28444 0.39663 9
4 1 -13 1.92516 0.43192 4
3 -1 -13 37.3501 3.45687 4
3 1 -13 41.2747 3.42228 9
3 1 -13 41.7381 3.45525 4
2 -1 -13 27.4925 2.70629 4
2 1 -13 32.7634 2.67841 9
2 1 -13 31.8710 2.70057 4
1 -1 -13 77.2325 7.03889 4
1 1 -13 91.2023 7.02854 9
1 1 -13 84.3121 7.02655 4
0 -1 -13 23.2609 2.22766 4
0 1 -13 25.6242 2.19237 9
0 1 -13 25.4615 2.21219 4
-1 -1 -13 17.1134 2.15709 4
-1 1 -13 27.1397 2.07228 9
-1 1 -13 24.5034 2.07831 4
-2 -1 -13 58.7331 5.33123 4
-2 1 -13 67.6012 5.31009 9
-2 1 -13 64.1527 5.31468 4
-3 -1 -13 26.3270 2.42489 4
-3 1 -13 29.7212 2.40027 9
-3 1 -13 27.5122 2.40124 4
-4 -1 -13 0.04981 0.32611 4
-4 1 -13 0.07649 0.29996 9
-4 1 -13 -0.0671 0.29694 4
-5 -1 -13 8.07629 0.84794 4
-5 1 -13 7.99875 0.77289 4
-5 1 -13 7.94516 0.74037 9
-6 1 -13 0.80963 0.27266 4
-8 2 13 39.6467 3.31222 4
7 2 -13 4.01261 0.50985 4
-7 2 13 4.66044 0.51208 4
6 2 -13 13.0854 1.14364 4
-6 2 13 12.6739 1.17438 4
5 2 -13 25.1856 1.88681 4
-5 2 13 19.3769 1.96607 4
5 2 -13 21.1991 1.87851 9
-4 2 13 53.0386 4.17309 4
4 2 -13 45.5477 4.14734 9
4 2 -13 51.1733 4.14486 4
3 2 -13 35.8550 2.86963 4
3 2 -13 32.1705 2.97968 9
2 2 -13 1.68581 0.29600 4
2 2 -13 2.55619 0.44776 9
1 2 -13 0.10004 0.26876 9
1 2 -13 0.14092 0.19811 4
0 2 -13 5.89254 0.77616 9
-1 2 -13 2.60674 0.44559 9
-2 2 -13 13.0820 1.17058 9
-3 2 -13 24.5209 2.06852 9
-8 0 14 6.12673 0.63420 4
8 0 -14 5.00062 0.65834 4
7 0 -14 12.1389 0.99802 4
-7 0 14 8.90814 0.94442 4
6 0 -14 58.8474 4.52578 4
-6 0 14 49.5768 4.50277 4
-5 0 14 0.15490 0.26997 4
5 0 -14 0.10368 0.26509 4
4 0 -14 12.3699 1.11709 9
-4 0 14 11.8417 1.16193 4
4 0 -14 13.6906 1.20650 4
3 0 -14 0.66176 0.32539 4
-3 0 14 0.19233 0.24416 4
3 0 -14 0.82418 0.26839 9
2 0 -14 16.9278 1.53548 9
2 0 -14 18.3160 1.59387 4
1 0 -14 42.5923 3.53992 9
1 0 -14 41.7334 3.56263 4
0 0 -14 4.68766 0.55276 9
0 0 -14 5.19220 0.62553 4
-1 0 -14 5.30065 0.62072 4
-1 0 -14 5.52924 0.58745 9
-2 0 -14 4.59219 0.48685 9
-2 0 -14 4.44273 0.54437 4
-3 0 -14 14.7661 1.21041 9
-3 0 -14 12.3994 1.19786 4
-8 1 14 2.11033 0.30418 4
8 1 -14 1.52935 0.27543 4
-7 1 14 108.848 8.91932 4
7 1 -14 108.485 8.91937 4
6 1 -14 0.05872 0.23864 4
-6 1 14 0.08306 0.19071 4
-5 1 14 34.8946 3.12050 4
5 1 -14 39.7895 3.14085 4
-4 1 14 22.9541 1.86308 4
4 1 -14 19.9591 1.84768 9
4 1 -14 21.7406 1.85401 4
3 -1 -14 14.8178 1.33617 9
3 1 -14 14.4320 1.30283 9
-3 1 14 15.2016 1.33531 4
3 1 -14 15.4293 1.33128 4
2 1 -14 0.99529 0.27976 4
2 1 -14 1.33444 0.26165 9
1 1 -14 25.7292 2.09014 9
1 1 -14 23.3046 2.08616 4
0 1 -14 34.0563 2.67027 9
0 1 -14 29.4219 2.65649 4
-1 -1 -14 1.75490 0.31236 9
-1 1 -14 1.66429 0.27338 4
-1 1 -14 1.65921 0.29394 9
-2 -1 -14 61.8947 4.69761 9
-2 1 -14 51.5132 4.67635 9
0 0 0 0.00 0.00 0
_exptl_absorpt_process_details
)
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
)
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 0.7543
_exptl_absorpt_correction_T_min 0.5428
_exptl_special_details
)
The following wavelength and cell were deduced by SADABS from the
direction cosines etc. They are given here for emergency use only:
CELL 1.54186 17.401 4.734 11.469 90.003 98.221 90.041
)
;
_shelx_hkl_checksum 82258
_shelx_res_file
;
TITL P21c_a.res in P2(1)/c
Mezei147_0m.res
created by SHELXL-2019/3 at 15:18:17 on 01-Jun-2024
REM Old TITL P21c in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.145, Rweak 0.004, Alpha 0.030
REM 0.600 for 242 systematic absences, Orientation as input
REM Formula found by SHELXT: C10 N4
CELL 1.54178 17.4095 4.7271 11.4664 90.0000 98.2471 90.0000
ZERR 4.000 0.0022 0.0007 0.0015 0.0000 0.0058 0.0000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H N
UNIT 40 48 16
TEMP -123.150
SIZE 0.23 0.21 0.11
L.S. 10
BOND $H
ACTA
CONF
HTAB
EQIV $1 -x+1, y+1/2, -z+1/2
HTAB N2 N1_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB N3 N1_$2
EQIV $3 x, -y+1/2, z+1/2
HTAB N3 N4_$3
EQIV $4 x, -y+3/2, z-1/2
HTAB N4 N3_$4
LIST 4
FMAP 2
PLAN 20
WGHT 0.033500 0.293800
FVAR 0.98801
N1 3 0.453880 0.614825 0.345033 11.00000 0.02491 0.02665 =
0.02162 0.00209 0.00537 0.00113
N2 3 0.426880 0.737360 0.237323 11.00000 0.02519 0.02644 =
0.02249 0.00417 0.00699 -0.00125
H2 2 0.457631 0.858671 0.206075 11.00000 -1.50000
N3 3 0.399601 0.296011 0.470015 11.00000 0.02795 0.02647 =
0.01924 0.00258 0.00356 -0.00164
H3A 2 0.446505 0.288461 0.514174 11.00000 -1.50000
H3B 2 0.373893 0.129038 0.465118 11.00000 -1.50000
N4 3 0.320680 0.719679 0.080533 11.00000 0.02922 0.02697 =
0.02031 0.00285 0.00574 0.00138
H4A 2 0.342065 0.875858 0.052686 11.00000 -1.50000
H4B 2 0.268516 0.736000 0.077354 11.00000 -1.50000
C1 1 0.396459 0.440528 0.363625 11.00000 0.02513 0.02156 =
0.01862 -0.00199 0.00662 0.00226
C2 1 0.333936 0.443452 0.270594 11.00000 0.02474 0.02201 =
0.01870 -0.00123 0.00606 0.00104
C3 1 0.356733 0.638268 0.191570 11.00000 0.02518 0.02200 =
0.01940 -0.00167 0.00743 0.00234
C4 1 0.261298 0.268277 0.258263 11.00000 0.02873 0.02451 =
0.01907 -0.00183 0.00440 -0.00306
AFIX 23
H4C 2 0.273491 0.083850 0.297498 11.00000 -1.20000
H4D 2 0.244323 0.230743 0.173545 11.00000 -1.20000
AFIX 0
C5 1 0.194605 0.403475 0.309787 11.00000 0.02317 0.02541 =
0.02326 -0.00237 0.00216 -0.00578
C6 1 0.181207 0.337145 0.423208 11.00000 0.03011 0.03829 =
0.02217 -0.00206 0.00325 -0.00116
AFIX 43
H6 2 0.213624 0.203060 0.468164 11.00000 -1.20000
AFIX 0
C7 1 0.121111 0.463891 0.471961 11.00000 0.03207 0.04877 =
0.02962 -0.00913 0.00898 -0.00665
AFIX 43
H7 2 0.112630 0.415162 0.549475 11.00000 -1.20000
AFIX 0
C8 1 0.073837 0.659913 0.408186 11.00000 0.02694 0.04080 =
0.05674 -0.01239 0.01445 -0.00308
AFIX 43
H8 2 0.033299 0.748953 0.441860 11.00000 -1.20000
AFIX 0
C9 1 0.085948 0.726185 0.294308 11.00000 0.03015 0.04030 =
0.06486 0.01190 0.00797 0.00554
AFIX 43
H9 2 0.053343 0.859940 0.249479 11.00000 -1.20000
AFIX 0
C10 1 0.145622 0.597267 0.245914 11.00000 0.03063 0.03920 =
0.03813 0.01150 0.00616 0.00000
AFIX 43
H10 2 0.153077 0.642532 0.167597 11.00000 -1.20000
REM #####
AFIX 0
HKLF 4
REM P21c_a.res in P2(1)/c
REM wR2 = 0.0952, GooF = S = 1.026, Restrained GooF = 1.026 for all data
REM R1 = 0.0376 for 1817 Fo > 4sig(Fo) and 0.0430 for all 1963 data
REM 142 parameters refined using 0 restraints
END
WGHT 0.0338 0.2882
REM Instructions for potential hydrogen bonds
HTAB N2 N1_$1
HTAB N3 N1_$2
HTAB N3 N4_$3
HTAB N4 N3_$4
REM Highest difference peak 0.212, deepest hole -0.204, 1-sigma level 0.039
Q1 1 0.3406 0.5279 0.2256 11.00000 0.05 0.21
Q2 1 0.2277 0.3466 0.2845 11.00000 0.05 0.20
Q3 1 0.1800 0.3299 0.3542 11.00000 0.05 0.19
Q4 1 0.3692 0.3799 0.3090 11.00000 0.05 0.18
Q5 1 0.2982 0.3712 0.2646 11.00000 0.05 0.17
Q6 1 0.3385 0.6794 0.1382 11.00000 0.05 0.15
Q7 1 0.1989 0.4301 0.3727 11.00000 0.05 0.14
Q8 1 0.1568 0.4327 0.4464 11.00000 0.05 0.13
Q9 1 0.1086 0.5793 0.4273 11.00000 0.05 0.13
Q10 1 0.4908 0.7466 0.3989 11.00000 0.05 0.13
Q11 1 0.1679 0.4871 0.2785 11.00000 0.05 0.13
Q12 1 0.5098 0.5679 0.3271 11.00000 0.05 0.13
Q13 1 0.3393 0.5902 0.0374 11.00000 0.05 0.13
Q14 1 0.2081 0.0915 0.4559 11.00000 0.05 0.12
Q15 1 0.2832 0.5623 0.0394 11.00000 0.05 0.12
Q16 1 0.3949 0.3853 0.4157 11.00000 0.05 0.12
Q17 1 0.0681 0.6332 0.3382 11.00000 0.05 0.12
Q18 1 0.1343 0.7132 0.2850 11.00000 0.05 0.12
Q19 1 0.5172 0.0772 0.5191 11.00000 0.05 0.11
Q20 1 0.0993 0.7557 0.3640 11.00000 0.05 0.11
;
_shelx_res_checksum 92014
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
N N1 0.45388(5) 0.6148(2) 0.34503(8) 0.0242(2) Uani d 1 . .
N N2 0.42688(6) 0.7374(2) 0.23732(8) 0.0244(2) Uani d 1 . .
H H2 0.4576(9) 0.859(3) 0.2061(14) 0.037 Uiso d 1 . .
N N3 0.39960(6) 0.2960(2) 0.47002(8) 0.0245(2) Uani d 1 . .
H H3A 0.4465(10) 0.288(3) 0.5142(14) 0.037 Uiso d 1 . .
H H3B 0.3739(9) 0.129(4) 0.4651(14) 0.037 Uiso d 1 . .
N N4 0.32068(6) 0.7197(2) 0.08053(8) 0.0253(2) Uani d 1 . .
H H4A 0.3421(9) 0.876(4) 0.0527(14) 0.038 Uiso d 1 . .
H H4B 0.2685(10) 0.736(3) 0.0774(14) 0.038 Uiso d 1 . .
C C1 0.39646(6) 0.4405(2) 0.36362(9) 0.0214(2) Uani d 1 . .
C C2 0.33394(6) 0.4435(2) 0.27059(9) 0.0215(2) Uani d 1 . .
C C3 0.35673(6) 0.6383(2) 0.19157(9) 0.0218(2) Uani d 1 . .
C C4 0.26130(6) 0.2683(2) 0.25826(9) 0.0240(2) Uani d 1 . .
H H4C 0.273491 0.083850 0.297498 0.029 Uiso calc 1 . .
H H4D 0.244323 0.230743 0.173545 0.029 Uiso calc 1 . .
C C5 0.19460(6) 0.4035(2) 0.30979(9) 0.0241(2) Uani d 1 . .
C C6 0.18121(7) 0.3371(3) 0.42321(10) 0.0302(3) Uani d 1 . .
H H6 0.213624 0.203060 0.468164 0.036 Uiso calc 1 . .
C C7 0.12111(7) 0.4639(3) 0.47196(11) 0.0364(3) Uani d 1 . .
H H7 0.112630 0.415162 0.549475 0.044 Uiso calc 1 . .
C C8 0.07384(8) 0.6599(3) 0.40819(14) 0.0407(3) Uani d 1 . .
H H8 0.033299 0.748953 0.441860 0.049 Uiso calc 1 . .
C C9 0.08595(8) 0.7262(3) 0.29431(15) 0.0450(4) Uani d 1 . .
H H9 0.053343 0.859940 0.249479 0.054 Uiso calc 1 . .
C C10 0.14562(7) 0.5973(3) 0.24591(12) 0.0359(3) Uani d 1 . .
H H10 0.153077 0.642532 0.167597 0.043 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
N1 0.0249(5) 0.0267(5) 0.0216(4) 0.0011(4) 0.0054(4) 0.0021(3)
N2 0.0252(5) 0.0264(5) 0.0225(4) -0.0012(4) 0.0070(4) 0.0042(3)
N3 0.0280(5) 0.0265(5) 0.0192(4) -0.0016(4) 0.0036(4) 0.0026(4)
N4 0.0292(5) 0.0270(5) 0.0203(4) 0.0014(4) 0.0057(4) 0.0028(3)
C1 0.0251(5) 0.0216(5) 0.0186(5) 0.0023(4) 0.0066(4) -0.0020(4)
C2 0.0247(5) 0.0220(5) 0.0187(5) 0.0010(4) 0.0061(4) -0.0012(4)
C3 0.0252(5) 0.0220(5) 0.0194(5) 0.0023(4) 0.0074(4) -0.0017(4)
C4 0.0287(6) 0.0245(5) 0.0191(5) -0.0031(4) 0.0044(4) -0.0018(4)
C5 0.0232(5) 0.0254(5) 0.0233(5) -0.0058(4) 0.0022(4) -0.0024(4)
C6 0.0301(6) 0.0383(6) 0.0222(5) -0.0012(5) 0.0032(4) -0.0021(5)
C7 0.0321(6) 0.0488(7) 0.0296(6) -0.0066(5) 0.0090(5) -0.0091(5)
C8 0.0269(6) 0.0408(7) 0.0567(8) -0.0031(5) 0.0144(6) -0.0124(6)
C9 0.0302(7) 0.0403(7) 0.0649(10) 0.0055(5) 0.0080(6) 0.0119(7)
C10 0.0306(6) 0.0392(7) 0.0381(7) 0.0000(5) 0.0062(5) 0.0115(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'
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 N1 N2 . . 103.56(9) ?
C3 N2 N1 . . 112.10(9) ?
C3 N2 H2 . . 129.1(10) ?
N1 N2 H2 . . 118.7(10) ?
C1 N3 H3A . . 115.6(10) ?
C1 N3 H3B . . 114.6(10) ?
H3A N3 H3B . . 113.7(14) ?
C3 N4 H4A . . 113.2(10) ?
C3 N4 H4B . . 112.2(10) ?
H4A N4 H4B . . 112.1(14) ?
N1 C1 N3 . . 120.41(10) ?
N1 C1 C2 . . 112.78(9) ?
N3 C1 C2 . . 126.62(10) ?
C3 C2 C1 . . 103.77(9) ?
C3 C2 C4 . . 128.31(10) ?
C1 C2 C4 . . 127.88(10) ?
N2 C3 C2 . . 107.78(9) ?
N2 C3 N4 . . 121.81(10) ?
C2 C3 N4 . . 130.32(10) ?
C2 C4 C5 . . 114.35(9) ?
C2 C4 H4C . . 108.7 ?
C5 C4 H4C . . 108.7 ?
C2 C4 H4D . . 108.7 ?
C5 C4 H4D . . 108.7 ?
H4C C4 H4D . . 107.6 ?
C10 C5 C6 . . 118.05(11) ?
C10 C5 C4 . . 121.30(10) ?
C6 C5 C4 . . 120.66(10) ?
C5 C6 C7 . . 121.06(12) ?
C5 C6 H6 . . 119.5 ?
C7 C6 H6 . . 119.5 ?
C8 C7 C6 . . 120.20(12) ?
C8 C7 H7 . . 119.9 ?
C6 C7 H7 . . 119.9 ?
C7 C8 C9 . . 119.43(12) ?
C7 C8 H8 . . 120.3 ?
C9 C8 H8 . . 120.3 ?
C10 C9 C8 . . 120.05(13) ?
C10 C9 H9 . . 120.0 ?
C8 C9 H9 . . 120.0 ?
C5 C10 C9 . . 121.20(12) ?
C5 C10 H10 . . 119.4 ?
C9 C10 H10 . . 119.4 ?
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
N1 C1 . 1.3360(14) ?
N1 N2 . 1.3839(13) ?
N2 C3 . 1.3425(15) ?
N2 H2 . 0.894(16) ?
N3 C1 . 1.3924(13) ?
N3 H3A . 0.898(17) ?
N3 H3B . 0.905(17) ?
N4 C3 . 1.3906(14) ?
N4 H4A . 0.905(17) ?
N4 H4B . 0.907(17) ?
C1 C2 . 1.4106(15) ?
C2 C3 . 1.3892(14) ?
C2 C4 . 1.5012(15) ?
C4 C5 . 1.5174(15) ?
C4 H4C . 0.9900 ?
C4 H4D . 0.9900 ?
C5 C10 . 1.3869(17) ?
C5 C6 . 1.3896(15) ?
C6 C7 . 1.3906(17) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.378(2) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.388(2) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.3871(19) ?
C9 H9 . 0.9500 ?
C10 H10 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N2 H2 N1 2_655 0.894(16) 2.108(16) 2.9912(13) 169.7(14) yes
N3 H3A N1 3_666 0.898(17) 2.240(17) 3.1032(14) 161.0(13) yes
N3 H3B N4 4_566 0.905(17) 2.383(16) 3.1521(14) 142.8(13) yes
N4 H4A N3 4_575 0.905(17) 2.140(18) 3.0388(14) 171.7(14) 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
C1 N1 N2 C3 . . . . -1.02(11) ?
N2 N1 C1 N3 . . . . -174.26(9) ?
N2 N1 C1 C2 . . . . 0.95(11) ?
N1 C1 C2 C3 . . . . -0.55(12) ?
N3 C1 C2 C3 . . . . 174.30(10) ?
N1 C1 C2 C4 . . . . 177.35(10) ?
N3 C1 C2 C4 . . . . -7.80(17) ?
N1 N2 C3 C2 . . . . 0.72(12) ?
N1 N2 C3 N4 . . . . -176.05(9) ?
C1 C2 C3 N2 . . . . -0.11(11) ?
C4 C2 C3 N2 . . . . -178.00(10) ?
C1 C2 C3 N4 . . . . 176.29(10) ?
C4 C2 C3 N4 . . . . -1.60(18) ?
C3 C2 C4 C5 . . . . -92.03(13) ?
C1 C2 C4 C5 . . . . 90.56(13) ?
C2 C4 C5 C10 . . . . 83.88(13) ?
C2 C4 C5 C6 . . . . -95.73(12) ?
C10 C5 C6 C7 . . . . -0.83(18) ?
C4 C5 C6 C7 . . . . 178.80(11) ?
C5 C6 C7 C8 . . . . -0.36(19) ?
C6 C7 C8 C9 . . . . 1.0(2) ?
C7 C8 C9 C10 . . . . -0.5(2) ?
C6 C5 C10 C9 . . . . 1.34(19) ?
C4 C5 C10 C9 . . . . -178.28(12) ?
C8 C9 C10 C5 . . . . -0.7(2) ?