#------------------------------------------------------------------------------
#$Date: 2023-08-12 04:54:27 +0300 (Sat, 12 Aug 2023) $
#$Revision: 285640 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022833.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_2022833
loop_
_publ_author_name
'Carlson, Faith M.'
'Staples, Richard J.'
'Biros, Shannon M.'
_publ_section_title
;
Crystal structure of a (carboxymethyl)triethylazanium
bromide--2-(triethylazaniumyl)acetate (1/1) hydrogen-bonded dimer
;
_journal_coeditor_code WM5689
_journal_issue 9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023006850
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C8 H18 N O2 +, Br -, C8 H17 N O2'
_chemical_formula_moiety 'C8 H18 N O2 +, Br -, C8 H17 N O2'
_chemical_formula_sum 'C16 H35 Br N2 O4'
_chemical_formula_weight 399.37
_chemical_name_systematic
'(Carboxymethyl)triethylazanium bromide--2-(triethylazaniumyl)acetate (1/1)'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-I 2ya'
_space_group_name_H-M_alt 'I 1 2/a 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha 90
_cell_angle_beta 103.022(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.6692(4)
_cell_length_b 7.0967(3)
_cell_length_c 22.3413(9)
_cell_measurement_reflns_used 3269
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 79.3860
_cell_measurement_theta_min 6.5540
_cell_volume 1957.04(13)
_computing_cell_refinement
;
CrysAlisPro (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlisPro (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlisPro (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2007)
;
_computing_publication_material
;
Olex2 (Dolomanov et al., 2009; Bourhis et al.,
2015)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0516
_diffrn_reflns_av_unetI/netI 0.0539
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 6198
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 79.956
_diffrn_reflns_theta_min 4.062
_exptl_absorpt_coefficient_mu 3.030
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.568
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Oxford Diffraction, 2006)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.355
_exptl_crystal_description plate
_exptl_crystal_F_000 848
_exptl_crystal_size_max 0.423
_exptl_crystal_size_mid 0.133
_exptl_crystal_size_min 0.023
_refine_diff_density_max 0.894
_refine_diff_density_min -0.418
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.075
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 109
_refine_ls_number_reflns 1998
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.075
_refine_ls_R_factor_all 0.0447
_refine_ls_R_factor_gt 0.0396
_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^)+(0.0638P)^2^+1.4873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1042
_refine_ls_wR_factor_ref 0.1086
_reflns_number_gt 1785
_reflns_number_total 1998
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5689sup1.cif
_cod_data_source_block I
_cod_database_code 2022833
_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 0.361
_shelx_estimated_absorpt_t_max 0.934
_shelx_hkl_file
;
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13 4 1 3617.96 461.154 7
13 4 3 3803.55 406.986 7
13 -4 5 1348.95 402.927 6
13 5 -8 1349.29 226.167 7
13 5 -6 1332.66 245.118 19
13 5 -4 3478.63 391.219 19
13 5 -2 431.941 212.709 7
13 5 0 110.318 135.960 7
14 0 -18 2382.03 380.847 12
14 0 -16 10198.6 929.202 12
14 0 -14 26517.3 1917.54 4
14 0 -14 25225.0 1909.51 12
14 0 -12 53386.2 3545.65 4
14 0 -10 53633.5 3426.20 4
14 0 -10 46355.2 3373.54 25
14 0 -10 51608.6 3296.11 10
14 0 -8 38344.8 2624.04 4
14 0 -8 37202.4 2568.51 7
14 0 -8 33905.6 2609.97 25
14 0 -8 37211.3 2549.74 10
14 0 -6 19199.1 1560.73 4
14 0 -6 20151.8 1582.61 7
14 0 -6 16827.2 1556.08 25
14 0 -6 17113.9 1512.17 10
14 0 -4 30168.8 2191.35 4
14 0 -4 28051.0 2246.23 25
14 0 -4 30792.7 2216.10 10
14 0 -2 45461.2 2880.34 4
14 0 -2 37419.8 2928.57 25
14 0 0 4321.72 704.545 7
14 0 2 34815.8 2442.60 7
14 0 4 28104.6 1890.18 7
14 0 4 25052.1 1864.52 14
14 0 6 18420.0 1297.67 7
14 0 6 20547.1 1411.38 14
14 0 8 1794.90 351.490 6
14 1 -19 793.863 210.358 4
14 -1 -17 25968.4 1674.83 4
14 1 -17 22815.7 1662.43 4
14 1 -15 13161.5 1126.69 4
14 -1 -15 13783.0 1149.69 12
14 1 -13 40460.3 2737.51 4
14 1 -11 13265.9 1203.97 4
14 1 -11 13476.2 1161.04 10
14 -1 -9 13444.9 1309.14 4
14 1 -9 16162.9 1294.14 4
14 -1 -9 12492.3 1163.77 7
14 1 -9 12995.2 1152.38 7
14 -1 -9 12967.6 1222.34 25
14 1 -9 15462.6 1268.01 25
14 1 -9 14021.4 1234.65 10
14 -1 -7 15239.7 1313.64 4
14 1 -7 12649.8 1149.43 4
14 -1 -7 12446.4 1176.95 7
14 1 -7 13583.8 1182.34 7
14 -1 -7 11101.3 1166.35 25
14 1 -7 10306.8 1146.11 25
14 1 -7 13447.5 1195.64 10
14 -1 -5 16757.5 1401.88 4
14 1 -5 15757.5 1262.55 4
14 -1 -5 13621.0 1349.23 7
14 1 -5 15202.6 1316.08 7
14 -1 -5 11615.1 1263.89 25
14 1 -5 14144.6 1320.93 25
14 1 -3 29324.2 1922.28 4
14 -1 -3 29634.7 2047.74 4
14 -1 -3 23291.7 1994.29 25
14 1 -3 22832.2 1983.02 25
14 -1 -1 4956.02 802.128 7
14 1 -1 4376.41 718.312 7
14 -1 -1 5514.41 715.305 25
14 1 -1 4829.86 673.460 25
14 -1 -1 4692.65 872.279 6
14 -1 1 37153.0 2457.47 7
14 1 1 37521.9 2414.55 7
14 -1 3 25567.4 1837.21 7
14 1 3 26445.9 1784.76 7
14 1 3 22318.2 1728.49 14
14 -1 5 17457.9 1278.67 7
14 1 5 16208.9 1212.14 7
14 1 5 17964.3 1293.98 14
14 1 7 930.551 337.283 14
14 -1 7 935.972 401.267 6
14 -2 -16 2325.47 377.118 4
14 2 -16 2921.81 403.653 4
14 -2 -14 896.888 387.505 4
14 2 -14 185.089 452.296 4
14 2 -14-133.348 435.198 10
14 -2 -12 216.790 448.399 4
14 2 -12 250.141 384.882 4
14 2 -12 266.011 405.759 10
14 2 -10 9911.61 902.313 4
14 2 -10 9517.79 938.234 10
14 2 -8 4365.39 562.302 7
14 2 -8 3638.21 534.989 4
14 -2 -8 3564.20 506.102 25
14 2 -8 3231.97 486.258 25
14 2 -6 298.305 378.088 7
14 -2 -6 254.351 237.540 25
14 2 -6 313.500 251.903 25
14 -2 -4 385.478 553.465 4
14 -2 -4-224.539 437.710 7
14 -2 -4 257.581 251.806 25
14 2 -4 63.1078 252.578 25
14 2 -4 226.810 481.255 10
14 2 -2 3411.07 563.318 7
14 -2 -2 3527.36 527.916 25
14 2 -2 3186.06 499.574 25
14 -2 -2 3566.35 758.393 6
14 2 -2 4381.40 682.336 10
14 -2 0 3486.05 606.793 7
14 2 0 2996.14 502.097 7
14 -2 0 1412.31 364.854 25
14 2 0 1872.76 378.916 25
14 -2 0 2005.27 699.072 6
14 -2 2 3529.74 572.163 7
14 2 2 2998.75 497.194 7
14 2 4 526.499 260.616 7
14 2 6 205.930 278.852 14
14 -2 6 28.6009 355.270 6
14 3 -15 130.951 207.562 10
14 -3 -11 2246.72 469.140 4
14 3 -9 325.469 268.157 7
14 3 -9 601.517 413.648 10
14 3 -7 4349.56 536.211 7
14 3 -7 4627.81 622.463 10
14 3 -5 9340.28 897.664 10
14 3 -3 10090.3 914.559 10
14 3 -1 219.693 304.655 7
14 -3 -1 88.5861 582.912 6
14 3 1 7425.16 672.587 7
14 3 3 1703.61 268.565 7
14 4 -12 8285.27 612.243 10
14 4 -10 18848.2 1270.25 10
14 4 -8 15413.4 1154.84 7
14 4 -8 20787.1 1235.49 10
14 4 -6 7833.95 663.361 7
14 4 -6 8619.49 693.693 10
14 4 -2 35240.5 2235.79 7
14 4 0 241.531 165.257 7
15 0 -15 112.273 256.806 4
15 0 -13-337.458 406.253 4
15 0 -11 128.955 368.525 4
15 0 -9 635.876 400.781 4
15 0 -9 53.4483 198.839 25
15 0 -7 48.4471 309.279 7
15 0 -7-269.800 427.118 4
15 0 -7-113.722 174.969 25
15 0 -5-125.519 376.040 4
15 0 -5 164.535 362.412 7
15 0 -5 173.436 177.935 25
15 0 -3 282.389 205.027 25
15 0 -1-152.521 352.273 7
15 0 -1 52.7117 179.832 25
15 0 1 166.810 282.481 7
15 0 3-132.204 186.006 7
15 0 3 174.696 361.876 6
15 1 -14 2394.11 364.234 4
15 1 -12 1398.63 371.774 4
15 -1 -10 17556.8 1303.31 4
15 1 -10 16796.5 1233.05 4
15 1 -10 15666.9 1211.26 10
15 -1 -8 8190.15 835.015 4
15 1 -8 8696.96 734.205 4
15 1 -8 7682.97 709.861 7
15 -1 -8 7185.30 724.919 25
15 1 -8 6380.00 706.219 25
15 1 -8 7976.48 781.161 10
15 1 -6 13226.2 978.965 4
15 -1 -6 12148.5 1075.05 4
15 -1 -6 13481.0 1082.63 7
15 1 -6 13838.3 1059.05 7
15 -1 -6 11345.2 1031.76 25
15 1 -6 11013.3 1014.32 25
15 1 -6 11814.2 1051.02 10
15 -1 -4 1695.31 443.765 7
15 -1 -4 1428.11 360.225 25
15 1 -4 1458.54 368.721 25
15 -1 -2 8048.65 814.916 25
15 1 -2 8232.00 807.754 25
15 -1 0 10383.8 936.259 7
15 1 0 11351.0 913.349 7
15 -1 2 683.277 277.101 7
15 1 2 773.518 257.789 7
15 -1 2 1031.07 416.214 6
15 -2 -13 9822.98 755.232 4
15 2 -11 47539.7 2944.50 10
15 2 -7 34472.2 2247.93 7
15 -2 -5 23460.0 1649.07 7
15 2 -5 22564.0 1599.57 7
15 2 -1 10774.9 868.949 7
15 2 1 5036.67 461.619 7
15 3 -8 33854.3 2131.85 10
15 3 -6 23613.9 1537.97 7
15 3 -2 2543.44 294.425 7
16 0 -4 18104.0 1220.32 7
0 0 0 0.00 0.00 0
TITL GVSU1122B in I2/a
REM I2/a (#15 with fixed user cell!)
CELL 1.54184 12.669193 7.096744 22.341324 90.0000 103.0224 90.0000
ZERR 7.00 0.000407 0.000273 0.000903 0.0000 0.0037 0.0000
LATT 2
SYMM -x+1/2, y,-z
SFAC C H N O Br
UNIT 84.00 70.00 7.00 14.00 7.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
SIZE 0.02 0.13 0.42
TREF
HKLF 4
END
;
_shelx_hkl_checksum 52738
_shelx_res_file
;
TITL gvsu1122b_a.res in I2/a
gvsu1122b.res
created by SHELXL-2019/2 at 14:10:38 on 07-Jul-2023
REM Old TITL GVSU1122B in Ia
REM SHELXT solution in I2/a: R1 0.082, Rweak 0.239, Alpha 0.007
REM 0.265 for 148 systematic absences, Orientation as input
REM Formula found by SHELXT: C16 N2 O4 Br
CELL 1.54184 12.6692 7.0967 22.3413 90 103.022 90
ZERR 4 0.0004 0.0003 0.0009 0 0.004 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H Br N O
UNIT 64 140 4 8 16
EQIV $1 1.5-X,0.5-Y,0.5-Z
L.S. 14 0 0
PLAN 14
SIZE 0.023 0.133 0.423
TEMP -173
CONF
HTAB C3 O2
HTAB O1 O1_$1
MORE -1
BOND $H
fmap 2 53
acta
REM
REM
REM
WGHT 0.063800 1.487300
FVAR 3.76691
BR1 3 0.250000 0.395816 0.500000 10.50000 0.01554 0.02113 =
0.01912 0.00000 0.00614 0.00000
O1 5 0.704148 0.347359 0.281908 11.00000 0.02090 0.03132 =
0.02640 -0.00833 0.01316 -0.00616
PART -1
AFIX 3
H1 2 0.734798 0.280169 0.252098 10.50000 0.06778
AFIX 0
O2 5 0.579037 0.120933 0.273123 11.00000 0.02139 0.02697 =
0.02416 -0.00890 0.00914 -0.00371
N1 4 0.490608 0.301409 0.368246 11.00000 0.01278 0.01613 =
0.01541 0.00010 0.00429 -0.00090
C1 1 0.619839 0.269842 0.294284 11.00000 0.01609 0.02290 =
0.01494 -0.00133 0.00291 0.00096
C2 1 0.574563 0.392309 0.338865 11.00000 0.01381 0.01710 =
0.01623 -0.00016 0.00498 -0.00285
AFIX 23
H2A 2 0.635817 0.434190 0.372016 11.00000 -1.20000
H2B 2 0.542009 0.506334 0.316589 11.00000 -1.20000
AFIX 0
C3 1 0.527927 0.111183 0.396412 11.00000 0.02122 0.01585 =
0.01860 0.00236 0.00347 0.00012
AFIX 23
H3A 2 0.522278 0.017911 0.362887 11.00000 -1.20000
H3B 2 0.477980 0.070888 0.422252 11.00000 -1.20000
AFIX 0
C4 1 0.643130 0.107563 0.435386 11.00000 0.02127 0.02521 =
0.02327 0.00188 -0.00099 0.00566
AFIX 137
H4A 2 0.694224 0.132344 0.409276 11.00000 -1.50000
H4B 2 0.658203 -0.016535 0.454658 11.00000 -1.50000
H4C 2 0.651144 0.204548 0.467320 11.00000 -1.50000
AFIX 0
C5 1 0.473637 0.430574 0.419554 11.00000 0.01507 0.02143 =
0.01398 -0.00024 0.00328 0.00150
AFIX 23
H5A 2 0.419692 0.371758 0.439611 11.00000 -1.20000
H5B 2 0.542724 0.439647 0.450705 11.00000 -1.20000
AFIX 0
C6 1 0.435827 0.627807 0.399834 11.00000 0.03151 0.02144 =
0.02553 0.00029 0.01066 0.00748
AFIX 137
H6A 2 0.369669 0.621107 0.367223 11.00000 -1.50000
H6B 2 0.492434 0.693461 0.384459 11.00000 -1.50000
H6C 2 0.420881 0.696650 0.435042 11.00000 -1.50000
AFIX 0
C7 1 0.385912 0.275727 0.319497 11.00000 0.01356 0.02182 =
0.01448 -0.00030 0.00083 -0.00253
AFIX 23
H7A 2 0.360683 0.400804 0.302461 11.00000 -1.20000
H7B 2 0.401558 0.198822 0.285550 11.00000 -1.20000
AFIX 0
C8 1 0.295415 0.182364 0.342888 11.00000 0.01589 0.03308 =
0.02306 -0.00046 0.00317 -0.00684
AFIX 137
H8A 2 0.228952 0.182944 0.310402 11.00000 -1.50000
H8B 2 0.283092 0.251692 0.378634 11.00000 -1.50000
H8C 2 0.315681 0.052079 0.354755 11.00000 -1.50000
AFIX 0
HKLF 4
REM gvsu1122b_a.res in I2/a
REM wR2 = 0.1086, GooF = S = 1.075, Restrained GooF = 1.075 for all data
REM R1 = 0.0396 for 1785 Fo > 4sig(Fo) and 0.0447 for all 1998 data
REM 109 parameters refined using 0 restraints
END
WGHT 0.0638 1.4802
REM Highest difference peak 0.894, deepest hole -0.418, 1-sigma level 0.101
Q1 1 0.2084 0.4052 0.4589 11.00000 0.05 0.89
Q2 1 0.2583 0.5118 0.4819 11.00000 0.05 0.50
Q3 1 0.2228 0.2937 0.5239 11.00000 0.05 0.47
Q4 1 0.2500 0.2466 0.5000 10.50000 0.05 0.46
Q5 1 0.7500 0.1792 0.5000 10.50000 0.05 0.46
Q6 1 0.5958 0.1257 0.3032 11.00000 0.05 0.34
Q7 1 0.4522 0.5234 0.4055 11.00000 0.05 0.33
Q8 1 0.7129 0.4586 0.2826 11.00000 0.05 0.32
Q9 1 0.4293 0.2926 0.3384 11.00000 0.05 0.31
Q10 1 0.5810 0.5806 0.4602 11.00000 0.05 0.31
Q11 1 0.5821 0.1192 0.4172 11.00000 0.05 0.30
Q12 1 0.4335 0.6334 0.3635 11.00000 0.05 0.30
Q13 1 0.4805 0.3817 0.4374 11.00000 0.05 0.30
Q14 1 0.6686 0.3703 0.2595 11.00000 0.05 0.30
;
_shelx_res_checksum 73524
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
Br Br1 0.250000 0.39582(5) 0.500000 0.01824(16) Uani d 1 . .
O O1 0.70415(15) 0.3474(3) 0.28191(9) 0.0250(4) Uani d 1 . .
H H1 0.734798 0.280169 0.252098 0.07(3) Uiso d 0.5 A -1
O O2 0.57904(15) 0.1209(3) 0.27312(9) 0.0235(4) Uani d 1 B -1
N N1 0.49061(15) 0.3014(3) 0.36825(9) 0.0146(4) Uani d 1 B -1
C C1 0.61984(19) 0.2698(4) 0.29428(11) 0.0181(5) Uani d 1 B -1
C C2 0.57456(19) 0.3923(3) 0.33887(12) 0.0155(5) Uani d 1 B -1
H H2A 0.635817 0.434190 0.372016 0.019 Uiso calc 1 B -1
H H2B 0.542009 0.506334 0.316589 0.019 Uiso calc 1 B -1
C C3 0.5279(2) 0.1112(3) 0.39641(12) 0.0187(5) Uani d 1 B -1
H H3A 0.522278 0.017911 0.362887 0.022 Uiso calc 1 B -1
H H3B 0.477980 0.070888 0.422252 0.022 Uiso calc 1 B -1
C C4 0.6431(2) 0.1076(4) 0.43539(14) 0.0242(6) Uani d 1 B -1
H H4A 0.694224 0.132344 0.409276 0.036 Uiso calc 1 B -1
H H4B 0.658203 -0.016535 0.454658 0.036 Uiso calc 1 B -1
H H4C 0.651144 0.204548 0.467320 0.036 Uiso calc 1 B -1
C C5 0.47364(19) 0.4306(4) 0.41955(11) 0.0168(5) Uani d 1 B -1
H H5A 0.419692 0.371758 0.439611 0.020 Uiso calc 1 B -1
H H5B 0.542724 0.439647 0.450705 0.020 Uiso calc 1 B -1
C C6 0.4358(2) 0.6278(4) 0.39983(14) 0.0255(6) Uani d 1 B -1
H H6A 0.369669 0.621107 0.367223 0.038 Uiso calc 1 B -1
H H6B 0.492434 0.693461 0.384459 0.038 Uiso calc 1 B -1
H H6C 0.420881 0.696650 0.435042 0.038 Uiso calc 1 B -1
C C7 0.38591(18) 0.2757(4) 0.31950(11) 0.0170(5) Uani d 1 B -1
H H7A 0.360683 0.400804 0.302461 0.020 Uiso calc 1 B -1
H H7B 0.401558 0.198822 0.285550 0.020 Uiso calc 1 B -1
C C8 0.2954(2) 0.1824(4) 0.34289(13) 0.0242(6) Uani d 1 B -1
H H8A 0.228952 0.182944 0.310402 0.036 Uiso calc 1 B -1
H H8B 0.283092 0.251692 0.378634 0.036 Uiso calc 1 B -1
H H8C 0.315681 0.052079 0.354755 0.036 Uiso calc 1 B -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
Br1 0.0155(2) 0.0211(2) 0.0191(2) 0.000 0.00614(14) 0.000
O1 0.0209(9) 0.0313(10) 0.0264(10) -0.0062(8) 0.0132(8) -0.0083(8)
O2 0.0214(9) 0.0270(10) 0.0242(10) -0.0037(7) 0.0091(8) -0.0089(7)
N1 0.0128(8) 0.0161(10) 0.0154(10) -0.0009(7) 0.0043(8) 0.0001(8)
C1 0.0161(10) 0.0229(13) 0.0149(12) 0.0010(9) 0.0029(9) -0.0013(9)
C2 0.0138(10) 0.0171(12) 0.0162(12) -0.0029(8) 0.0050(9) -0.0002(9)
C3 0.0212(12) 0.0158(12) 0.0186(12) 0.0001(8) 0.0035(10) 0.0024(9)
C4 0.0213(12) 0.0252(14) 0.0233(14) 0.0057(10) -0.0010(10) 0.0019(10)
C5 0.0151(10) 0.0214(12) 0.0140(11) 0.0015(9) 0.0033(9) -0.0002(9)
C6 0.0315(14) 0.0214(14) 0.0255(15) 0.0075(10) 0.0107(12) 0.0003(10)
C7 0.0136(9) 0.0218(12) 0.0145(11) -0.0025(9) 0.0008(9) -0.0003(9)
C8 0.0159(11) 0.0331(15) 0.0231(13) -0.0068(10) 0.0032(10) -0.0005(11)
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'
Br Br -0.6763 1.2805 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 -1 -5 0.0605
-8 0 5 0.0549
0 -5 -2 0.1838
0 5 2 0.2345
0 0 -1 0.0116
0 0 1 0.0116
8 1 -2 0.0946
-7 2 5 0.0978
-6 -3 1 0.1373
7 -2 -5 0.1014
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 . . 114.7 ?
C2 N1 C3 . . 112.00(18) ?
C2 N1 C5 . . 107.61(18) ?
C2 N1 C7 . . 108.91(18) ?
C3 N1 C5 . . 107.89(19) ?
C3 N1 C7 . . 109.20(19) ?
C5 N1 C7 . . 111.24(17) ?
O1 C1 C2 . . 110.4(2) ?
O2 C1 O1 . . 125.8(2) ?
O2 C1 C2 . . 123.7(2) ?
N1 C2 C1 . . 116.35(19) ?
N1 C2 H2A . . 108.2 ?
N1 C2 H2B . . 108.2 ?
C1 C2 H2A . . 108.2 ?
C1 C2 H2B . . 108.2 ?
H2A C2 H2B . . 107.4 ?
N1 C3 H3A . . 108.5 ?
N1 C3 H3B . . 108.5 ?
N1 C3 C4 . . 114.9(2) ?
H3A C3 H3B . . 107.5 ?
C4 C3 H3A . . 108.5 ?
C4 C3 H3B . . 108.5 ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4B . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
N1 C5 H5A . . 108.4 ?
N1 C5 H5B . . 108.4 ?
H5A C5 H5B . . 107.5 ?
C6 C5 N1 . . 115.3(2) ?
C6 C5 H5A . . 108.4 ?
C6 C5 H5B . . 108.4 ?
C5 C6 H6A . . 109.5 ?
C5 C6 H6B . . 109.5 ?
C5 C6 H6C . . 109.5 ?
H6A C6 H6B . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
N1 C7 H7A . . 108.7 ?
N1 C7 H7B . . 108.7 ?
H7A C7 H7B . . 107.6 ?
C8 C7 N1 . . 114.2(2) ?
C8 C7 H7A . . 108.7 ?
C8 C7 H7B . . 108.7 ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
C7 C8 H8C . . 109.5 ?
H8A C8 H8B . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 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 H1 . 0.9686 ?
O1 C1 . 1.286(3) ?
O2 C1 . 1.224(3) ?
N1 C2 . 1.514(3) ?
N1 C3 . 1.519(3) ?
N1 C5 . 1.520(3) ?
N1 C7 . 1.526(3) ?
C1 C2 . 1.528(3) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3 C4 . 1.522(4) ?
C4 H4A . 0.9800 ?
C4 H4B . 0.9800 ?
C4 H4C . 0.9800 ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C5 C6 . 1.512(4) ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C7 C8 . 1.515(3) ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 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 O1 7_655 0.97 1.50 2.457(4) 167 yes
C3 H3A O2 . 0.99 2.39 2.969(3) 116 yes
C7 H7B O2 . 0.99 2.39 3.068(3) 125 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 C2 N1 . . . . -167.3(2) ?
O2 C1 C2 N1 . . . . 13.8(4) ?
C2 N1 C3 C4 . . . . 46.5(3) ?
C2 N1 C5 C6 . . . . 59.1(3) ?
C2 N1 C7 C8 . . . . 179.0(2) ?
C3 N1 C2 C1 . . . . 50.4(3) ?
C3 N1 C5 C6 . . . . -179.9(2) ?
C3 N1 C7 C8 . . . . 56.4(3) ?
C5 N1 C2 C1 . . . . 168.8(2) ?
C5 N1 C3 C4 . . . . -71.8(3) ?
C5 N1 C7 C8 . . . . -62.6(3) ?
C7 N1 C2 C1 . . . . -70.5(3) ?
C7 N1 C3 C4 . . . . 167.2(2) ?
C7 N1 C5 C6 . . . . -60.1(3) ?
_cod_database_fobs_code 2022833