#------------------------------------------------------------------------------
#$Date: 2022-09-23 03:06:54 +0100 (Fri, 23 Sep 2022) $
#$Revision: 278104 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244177.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_2244177
loop_
_publ_author_name
Vinaya
'Basavaraju, Yeriyur B.'
'Lakshmana, Beliyaiah'
'Yathirajan, Hemmige S.'
'Parkin, Sean'
_publ_section_title
;
Syntheses and crystal structures of benzyl
N'-[(E)-2-hydroxybenzylidene]hydrazinecarboxylate and
benzyl
N'-[(E)-5-bromo-2-hydroxybenzylidene]hydrazinecarboxylate
;
_journal_coeditor_code YK2176
_journal_issue 10
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989022009100
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C15 H13 Br N2 O3'
_chemical_formula_moiety 'C15 H13 Br N2 O3'
_chemical_formula_sum 'C15 H13 Br N2 O3'
_chemical_formula_weight 349.18
_chemical_name_systematic
;
Benzyl N'-[(E)-5-bromo-2-hydroxybenzylidene]hydrazinecarboxylate
;
_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 direct
_atom_sites_solution_secondary difmap
_audit_creation_method 'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha 90
_cell_angle_beta 94.485(2)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 27.904(2)
_cell_length_b 11.1207(6)
_cell_length_c 9.0648(7)
_cell_measurement_reflns_used 9936
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 2.34
_cell_volume 2804.3(3)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
CIFFIX (Parkin, 2013) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0467
_diffrn_reflns_av_unetI/netI 0.0464
_diffrn_reflns_limit_h_max 36
_diffrn_reflns_limit_h_min -36
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 36145
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.533
_diffrn_reflns_theta_min 1.972
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 2.943
_exptl_absorpt_correction_T_max 0.862
_exptl_absorpt_correction_T_min 0.598
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.654
_exptl_crystal_description plate
_exptl_crystal_F_000 1408
_exptl_crystal_size_max 0.240
_exptl_crystal_size_mid 0.220
_exptl_crystal_size_min 0.050
_refine_diff_density_max 0.362
_refine_diff_density_min -0.388
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 391
_refine_ls_number_reflns 6401
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.033
_refine_ls_R_factor_all 0.0453
_refine_ls_R_factor_gt 0.0280
_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^)+(0.0240P)^2^+0.4336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0593
_refine_ls_wR_factor_ref 0.0635
_reflns_number_gt 5004
_reflns_number_total 6401
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yk2176sup1.cif
_cod_data_source_block II
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2244177
_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 0.539
_shelx_estimated_absorpt_t_max 0.867
_shelx_hkl_file
;
-1 0 0 0.12100 0.15177 2
-1 0 0 -0.0396 0.17894 2
1 0 0 0.11196 0.17547 2
1 0 0 0.09946 0.16074 2
-2 0 0 16.4804 1.31696 2
2 0 0 18.7403 1.29729 2
2 0 0 16.1708 1.33845 2
-2 0 0 17.3719 1.29767 2
-3 0 0 -0.4255 0.48787 2
3 0 0 -0.1172 0.52715 2
-3 0 0 -0.0813 0.52934 2
3 0 0 -0.1450 0.53932 2
4 0 0 355.676 21.2311 2
4 0 0 353.766 21.1147 2
-4 0 0 343.770 21.0875 2
-4 0 0 358.218 21.2376 2
-5 0 0 -0.5489 0.84209 2
-5 0 0 0.27176 0.97044 2
5 0 0 -0.5481 0.79436 2
5 0 0 0.21639 0.88532 2
6 0 0 148.657 9.41523 2
6 0 0 145.854 9.54588 2
-6 0 0 149.817 9.60293 2
-6 0 0 144.686 9.34414 2
7 0 0 -0.3525 1.28373 2
-7 0 0 -0.7932 1.42249 2
-7 0 0 -0.4092 1.25811 2
7 0 0 0.48935 1.49255 2
-8 0 0 137.622 9.41051 2
-9 0 0 -0.4588 1.93467 2
-10 0 0 273.568 17.6682 2
-11 0 0 -1.4405 2.24384 2
-1 -1 0 26.0895 1.74929 2
1 -1 0 27.5653 1.70851 2
1 -1 0 26.3093 1.74567 2
-1 -1 0 27.7348 1.70698 2
-1 -1 0 27.2085 1.76994 5
-1 1 0 27.2156 1.78730 4
1 1 0 28.1115 1.69574 2
1 1 0 26.6121 1.78445 5
1 1 0 26.7211 1.73594 2
-1 1 0 27.0812 1.73073 2
-1 1 0 28.1766 1.69919 2
2 -1 0 75.4525 4.63107 2
-2 -1 0 74.3138 4.79050 2
2 -1 0 75.5005 4.73264 2
-2 -1 0 76.3218 4.66668 2
2 1 0 75.5298 4.77483 2
2 1 0 78.3917 4.66108 2
-2 1 0 74.5444 4.77224 2
-2 1 0 76.4052 4.60520 2
-3 -1 0 295.587 17.4827 2
-3 -1 0 292.804 17.5904 2
3 -1 0 294.524 17.4776 2
3 -1 0 288.746 17.5590 2
-3 1 0 296.188 17.4414 2
-3 1 0 282.902 17.5234 2
3 1 0 288.752 17.5618 2
3 1 0 300.049 17.4715 2
-4 -1 0 -0.2822 0.60199 2
-4 -1 0 -0.1613 0.78045 2
4 -1 0 -1.0934 0.67628 2
4 -1 0 1.03853 0.81046 2
-4 1 0 -0.4930 0.67482 2
4 1 0 1.00339 0.77415 2
-4 1 0 -0.3320 0.73383 2
4 1 0 -0.3195 0.78209 2
5 -1 0 15.8511 1.92676 2
-5 -1 0 14.2252 1.96958 2
5 -1 0 13.8142 1.78444 2
-5 -1 0 13.4601 1.75340 2
5 1 0 12.8501 1.84847 2
-5 1 0 13.2474 1.95458 2
5 1 0 11.4786 1.74754 2
-5 1 0 13.3680 1.74776 2
6 -1 0 0.77638 1.14287 2
-6 -1 0 1.52853 1.33424 2
6 -1 0 0.85161 1.15530 2
-6 -1 0 0.49802 1.16456 2
-6 1 0 0.97452 1.27539 2
6 1 0 2.00147 1.33299 2
-6 1 0 -0.5063 1.06304 2
6 1 0 0.57268 1.12458 2
-7 -1 0 44.6052 4.16443 2
-7 -1 0 41.0896 3.76574 2
7 -1 0 42.8158 3.91802 2
7 -1 0 42.6776 3.98810 2
-7 1 0 51.4781 4.03703 2
7 1 0 47.5015 3.93246 2
-7 1 0 43.1266 3.72519 2
8 -1 0 1.12653 1.80377 2
-8 -1 0 9.86957 2.29360 2
-8 1 0 2.88280 1.94102 2
-9 -1 0 57.0208 5.39022 2
-9 1 0 62.7433 5.26000 2
-10 -1 0 31.4437 4.40115 2
-10 1 0 36.0912 4.30783 2
-11 -1 0 33.3562 4.53943 2
-11 1 0 32.3680 4.44120 2
0 -2 0 18.9547 1.28696 3
0 -2 0 18.9515 1.36119 5
0 2 0 18.3019 1.30207 3
-1 -2 0 19.2527 1.33957 2
1 -2 0 21.6019 1.52211 4
-1 -2 0 22.3111 1.36136 2
-1 -2 0 21.9281 1.46246 3
-1 -2 0 19.9815 1.56328 5
1 -2 0 20.0789 1.33493 2
1 -2 0 20.6526 1.35517 2
1 2 0 18.1070 1.58226 5
1 2 0 21.8576 1.48464 3
-1 2 0 22.2112 1.49582 4
-2 -2 0 4.50039 0.85909 5
-2 -2 0 3.98995 0.70784 2
-2 -2 0 4.40718 0.70829 2
2 -2 0 3.92752 0.71574 2
2 -2 0 3.82370 0.59256 2
-2 2 0 3.25925 0.61111 2
-2 2 0 4.63743 0.76409 4
-2 2 0 3.27824 0.62962 2
2 2 0 3.62534 0.66088 2
2 2 0 3.89107 0.66562 2
2 2 0 3.64440 0.80122 5
-3 -2 0 0.82921 0.68015 2
3 -2 0 1.12936 0.64733 2
3 -2 0 1.68304 0.69493 2
-3 -2 0 2.00888 0.64883 2
3 2 0 1.70949 0.88982 5
3 2 0 1.14724 0.68320 2
-3 2 0 2.06488 0.61858 2
3 2 0 1.00213 0.66380 2
-3 2 0 1.17822 0.67942 2
-4 -2 0 9.03048 1.43108 2
4 -2 0 9.45731 1.48189 2
4 -2 0 11.1023 1.52424 2
-4 -2 0 9.68906 1.39839 2
-4 2 0 10.3580 1.58820 2
4 2 0 12.3856 1.47477 2
4 2 0 10.6010 1.45956 2
4 2 0 11.7728 1.81145 5
5 -2 0 3.30110 1.16303 2
-5 -2 0 1.28850 1.19229 2
5 -2 0 1.70381 1.14602 2
-5 -2 0 1.40623 1.03033 2
5 2 0 1.29532 1.06716 2
-5 2 0 3.51773 1.02465 2
5 2 0 2.11675 1.32522 2
6 -2 0 6.16829 1.57453 2
-6 -2 0 5.58052 1.65244 2
-6 -2 0 6.43886 1.42787 2
6 -2 0 3.92688 1.49578 2
-6 2 0 4.66721 1.48145 2
6 2 0 5.02010 1.51362 2
-6 2 0 3.80899 1.27488 2
6 2 0 6.74200 1.60964 2
-7 -2 0 1.50414 1.68733 2
7 -2 0 2.05154 1.38748 2
7 -2 0 2.51614 1.62665 2
-7 2 0 0.83182 1.55220 2
7 2 0 1.97002 1.60035 2
-7 2 0 4.11604 1.69289 2
-8 -2 0 31.1324 3.85461 2
-8 2 0 37.4629 3.92523 2
-9 -2 0 -0.8389 2.01042 2
-9 2 0 1.53454 2.26923 2
9 2 0 -1.5787 2.51230 5
-10 -2 0 22.2142 3.63139 2
10 2 0 31.7966 4.88897 5
-10 2 0 25.6506 3.92848 2
-11 -2 0 -2.4299 2.54359 2
11 2 0 0.06124 3.45152 5
-11 2 0 0.98495 2.37402 2
0 -3 0 0.06622 0.38590 3
0 -3 0 0.21448 0.49488 5
0 3 0 0.04960 0.37159 3
-1 -3 0 11.1138 1.26299 5
-1 -3 0 12.2101 0.80952 2
-1 -3 0 12.7703 0.84643 2
-1 -3 0 13.7642 1.10428 3
1 -3 0 10.9355 1.16382 4
-1 3 0 11.8009 1.14917 4
1 3 0 10.8060 1.22598 3
1 3 0 12.4567 1.30372 5
-2 -3 0 6.32897 0.81284 2
2 -3 0 5.99158 0.81687 2
2 -3 0 6.48804 0.75238 2
-2 -3 0 6.17855 1.09482 5
-2 -3 0 5.68879 0.82665 2
-2 3 0 5.20266 0.62249 2
2 3 0 6.00403 0.89936 3
-2 3 0 5.74084 0.57954 2
2 3 0 5.39815 0.67450 2
2 3 0 6.43090 0.65304 2
-2 3 0 5.87280 1.06113 4
2 3 0 7.34693 1.16694 5
3 -3 0 107.147 6.92715 2
-3 -3 0 108.700 7.08381 2
3 -3 0 109.794 7.04734 2
-3 -3 0 109.924 6.84189 2
-3 3 0 117.214 6.76052 2
3 3 0 117.664 6.79333 2
3 3 0 110.849 6.87459 2
3 3 0 111.627 7.11913 5
-3 3 0 110.319 6.83062 2
-3 3 0 109.654 7.27793 4
4 -3 0 15.4591 1.75487 2
-4 -3 0 15.9349 1.73025 2
-4 -3 0 16.1664 1.86469 2
4 -3 0 17.4838 1.82206 2
-4 3 0 14.4715 1.69938 2
-4 3 0 15.4172 1.57076 2
4 3 0 9.99746 2.40755 5
-4 3 0 15.2498 2.00854 4
4 3 0 18.4426 1.96389 2
4 3 0 15.3056 1.70415 2
5 -3 0 20.6165 2.18418 2
-5 -3 0 15.8952 2.00789 2
5 -3 0 16.3447 2.16370 2
-5 -3 0 19.8236 2.33115 2
5 3 0 20.2906 2.67157 5
-5 3 0 18.4600 2.18851 2
5 3 0 19.8727 2.02034 2
5 3 0 18.4607 2.15808 2
-5 3 0 17.7483 1.99561 2
-6 -3 0 37.5121 3.23162 2
6 -3 0 38.1563 3.46769 2
6 -3 0 37.0120 3.35368 2
-6 -3 0 33.3205 3.52464 2
6 3 0 42.7156 3.85947 5
-6 3 0 40.0454 3.31484 2
-6 3 0 36.7190 3.14592 2
6 3 0 35.1899 3.22777 2
7 -3 0 68.3233 5.15532 2
-7 -3 0 54.6751 4.92207 2
-7 -3 0 66.1099 5.41484 2
7 -3 0 68.3476 5.29163 2
-7 3 0 72.5971 5.20253 2
7 3 0 67.4082 5.52427 5
-8 3 0 1.54429 1.72360 2
8 3 0 -1.3633 2.35400 5
-9 -3 0 53.0747 5.27670 2
-9 3 0 56.5993 4.98120 2
9 3 0 52.8361 5.64217 5
-10 -3 0 7.76163 2.75964 2
-10 3 0 6.55759 2.40134 2
10 3 0 3.44720 3.40353 5
-11 3 0 21.5338 3.92374 2
0 -4 0 713.507 42.3257 1
0 4 0 707.775 42.3053 1
-1 -4 0 84.5604 5.24765 3
1 -4 0 81.0309 5.25741 4
-1 -4 0 79.3731 5.38768 5
1 4 0 83.7275 5.23480 3
1 4 0 85.2071 5.37848 5
2 -4 0 389.287 23.1208 2
-2 -4 0 401.450 23.0151 2
2 -4 0 399.817 23.3226 4
-2 -4 0 381.303 23.2062 2
-2 -4 0 384.523 23.4166 5
2 -4 0 412.110 22.7462 2
2 4 0 376.385 23.3138 3
2 4 0 376.286 23.4744 5
-2 4 0 385.111 23.2850 4
-3 -4 0 25.8759 2.12660 2
3 -4 0 26.1712 1.95830 2
-3 -4 0 27.5859 2.33083 5
-3 -4 0 26.7011 1.98235 2
3 -4 0 26.1687 2.07791 2
3 4 0 28.0686 2.38951 3
3 4 0 24.5860 1.81739 2
-3 4 0 22.3640 2.29850 4
-3 4 0 24.1552 1.74870 2
3 4 0 20.2882 2.58706 5
-3 4 0 25.1601 1.69951 2
-4 -4 0 597.934 36.0108 2
4 -4 0 603.352 36.0017 2
-4 -4 0 589.172 36.8482 2
4 -4 0 578.427 36.4262 2
4 4 0 617.334 35.9811 2
4 4 0 606.045 36.2980 5
-4 4 0 614.437 35.8757 2
4 4 0 673.456 36.1202 3
-4 4 0 595.203 36.4717 4
-5 -4 0 150.736 9.64921 2
5 -4 0 147.424 9.85408 2
5 -4 0 153.946 9.70287 2
-5 -4 0 150.470 9.89820 2
-5 4 0 159.013 9.60399 2
-5 4 0 155.884 9.45068 2
-5 4 0 149.788 9.89861 4
5 4 0 159.040 9.66846 2
5 4 0 156.345 10.0705 5
6 -4 0 135.292 8.70035 2
6 -4 0 129.567 8.84320 2
-6 -4 0 123.217 8.61144 2
-6 -4 0 136.504 8.99950 2
6 4 0 136.721 8.65710 2
6 4 0 142.978 9.14142 5
-6 4 0 128.119 8.90300 4
-7 -4 0 20.4721 3.16938 2
-7 -4 0 18.4816 2.98653 2
7 -4 0 20.8122 2.94597 2
7 -4 0 17.5554 2.85859 2
7 4 0 18.9384 3.74867 5
7 4 0 19.3971 2.55560 2
-7 4 0 22.1840 2.76394 2
8 -4 0 53.2621 4.91443 2
-8 -4 0 63.8593 5.30405 2
-8 4 0 54.6614 4.65698 2
8 4 0 54.5355 4.64310 2
-9 -4 0 4.83229 2.45151 2
9 4 0 3.89470 3.21633 5
-9 4 0 3.00856 2.09724 2
-10 -4 0 32.5264 4.51382 2
10 4 0 27.4700 5.42594 5
-11 -4 0 1.41055 2.59192 2
-11 4 0 3.51040 2.35082 2
0 -5 0 -0.5398 0.92496 5
0 -5 0 0.47448 0.76005 3
-1 -5 0 12.9258 1.61905 3
-1 -5 0 12.5293 1.80538 5
1 -5 0 14.1257 1.52329 3
1 -5 0 16.8121 1.68521 4
1 5 0 16.8770 1.60978 3
1 5 0 14.7770 1.80466 5
-2 -5 0 23.4243 2.00289 3
2 -5 0 24.4990 1.69885 2
2 -5 0 21.7037 1.73323 2
-2 -5 0 19.6395 2.25091 5
2 -5 0 22.8485 2.13579 4
-2 -5 0 21.8618 1.72992 2
-2 -5 0 23.4224 1.76500 2
-2 5 0 23.2425 2.14696 4
2 5 0 24.8658 2.41981 5
2 5 0 23.3659 2.27835 3
3 -5 0 46.6361 3.42202 2
-3 -5 0 50.0764 3.34584 2
-3 -5 0 50.9964 3.43515 2
3 -5 0 49.2506 3.31365 2
-3 -5 0 47.0534 3.72994 5
-3 5 0 50.9902 3.69679 4
3 5 0 51.1555 3.76553 3
3 5 0 43.4468 3.97710 5
4 -5 0 5.08184 1.20290 2
-4 -5 0 4.62380 1.13440 2
-4 5 0 5.27233 1.46651 4
4 5 0 4.20777 3.04261 3
4 5 0 4.70797 0.85975 2
4 5 0 4.42138 1.86079 5
5 -5 0 107.534 6.93290 2
5 -5 0 104.748 7.09196 2
-5 -5 0 109.799 7.14400 2
-5 -5 0 102.611 6.89655 2
-5 5 0 104.181 6.61541 2
5 5 0 92.9652 6.69162 2
5 5 0 114.513 7.17949 3
5 5 0 105.745 7.50369 5
-5 5 0 108.120 6.57631 2
-5 5 0 105.495 7.24897 4
-6 -5 0 3.12906 1.78775 2
6 -5 0 2.68976 1.64054 2
6 -5 0 -0.1337 1.37497 2
6 5 0 0.50627 1.17571 2
6 5 0 2.15983 2.34590 5
-6 5 0 1.91763 1.25358 2
6 5 0 1.56148 2.04068 3
-6 5 0 -1.0620 1.69039 4
-7 -5 0 19.6554 3.28161 2
7 -5 0 22.3646 2.98138 2
7 5 0 19.9621 2.47036 2
-7 5 0 20.6390 2.56214 2
7 5 0 28.5345 4.22030 5
7 5 0 23.7416 3.44234 3
8 -5 0 0.97116 1.99872 2
-8 -5 0 2.57673 2.14942 2
8 5 0 3.23426 2.62310 3
-8 5 0 1.43376 1.76186 2
8 5 0 -0.2286 2.93897 5
8 5 0 0.74082 1.94360 2
-9 -5 0 15.9673 3.09300 2
9 5 0 13.6948 3.90853 5
9 5 0 16.5385 3.49339 3
-9 5 0 20.8461 3.00219 2
-10 -5 0 2.50714 2.40159 2
10 5 0 6.81769 3.42857 3
10 5 0 0.36358 3.75865 5
-10 5 0 0.80429 2.17500 2
-11 -5 0 21.5733 3.84356 2
11 5 0 14.7842 5.18366 3
11 5 0 20.5360 5.08074 5
-11 5 0 24.0424 3.38439 2
0 -6 0 6.06848 1.37171 5
0 -6 0 9.37684 1.47565 3
-1 -6 0 14.4080 1.87770 3
-1 -6 0 20.4811 2.18151 5
1 -6 0 19.2125 2.11387 5
1 -6 0 17.2840 1.85764 4
1 -6 0 17.9635 1.82696 3
1 6 0 17.5287 1.84748 3
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1 -5 -32 2.11091 2.55696 4
-1 -5 32 1.90976 2.57602 2
-1 5 32 2.57968 2.93638 2
0 -5 32 11.2100 2.60088 2
0 -5 -32 10.2772 3.27745 2
0 5 32 10.4583 3.21680 3
0 5 32 10.2213 3.30036 2
1 -5 32 14.4008 2.82417 2
1 5 32 14.6684 3.66088 2
1 5 32 14.7445 2.95262 3
-2 -5 -32 6.27781 3.07518 2
2 -5 32 9.26406 2.70914 2
2 -5 32 9.91978 1.75232 3
2 5 32 7.69893 3.36566 2
-3 -6 32 0.31999 2.91375 2
3 -6 -32 3.16922 2.98406 2
3 -6 -32 3.74332 3.23160 4
-3 6 32 2.52564 3.05417 2
-2 -6 32 46.3669 5.05462 2
2 -6 -32 47.9190 5.74955 2
2 -6 -32 49.1299 5.46339 4
-2 6 32 46.5890 6.57574 2
1 -6 -32 3.78438 2.75983 2
1 -6 -32 3.50168 3.00984 4
-1 -6 32 -0.0786 2.21720 2
0 -6 -32 64.4099 6.02478 2
0 -6 32 63.4769 5.24789 2
0 -6 -32 63.8043 6.38918 4
0 6 32 59.8518 6.86600 2
-1 -6 -32 0.60886 2.89484 2
1 -6 32 -0.0458 2.03517 2
1 6 32 -0.1986 2.83771 2
5 0 -33 2.53202 2.94922 2
-5 0 33 0.72588 3.69808 2
4 0 -33 76.4257 6.97848 2
3 0 -33 -2.3713 2.80720 2
-3 0 33 0.91230 3.07441 2
-2 0 33 78.8534 6.75640 2
2 0 -33 75.5939 6.04659 4
1 0 -33 0.56496 2.58690 2
-1 0 33 -1.9746 2.61936 2
1 0 -33 1.16872 2.03073 4
0 0 33 30.9703 4.02342 3
0 0 33 35.2040 4.41651 2
0 0 -33 23.6914 3.67431 2
0 0 -33 23.7221 3.56095 4
1 0 33 1.24902 2.11146 3
1 0 33 1.47825 2.66175 2
-1 0 -33 1.47338 2.55697 2
2 0 33 39.9311 4.12620 3
-2 0 -33 38.2854 4.09268 2
3 0 33 -0.5010 2.18956 3
3 0 33 0.06306 1.67575 5
3 0 33 3.44667 2.60850 2
-3 0 -33 -1.1466 2.55416 2
-4 0 -33 7.53292 3.01981 2
4 0 33 11.8715 2.59319 5
4 0 33 9.08325 3.23918 2
4 0 33 17.2911 2.97329 3
5 -1 -33 1.21427 3.50244 2
-5 1 33 4.82068 3.90129 2
5 1 -33 0.69458 3.60493 2
4 -1 -33 13.7231 4.06702 2
3 -1 -33 11.1215 3.71551 2
3 -1 -33 9.77594 3.07164 4
-3 -1 33 12.6692 3.65554 2
-3 1 33 8.60075 3.80558 2
3 1 -33 11.4641 3.51270 2
3 1 -33 8.67731 2.49488 3
-2 -1 33 -3.6015 2.28642 2
2 -1 -33 2.44017 2.68243 2
2 -1 -33 4.29683 2.30224 4
2 1 -33 0.49870 2.93413 2
-2 1 33 -2.6024 2.77928 2
1 -1 -33 64.6841 5.36509 4
1 -1 -33 63.2582 6.18499 2
-1 -1 33 62.7316 6.24408 2
1 1 -33 66.2719 5.15858 4
1 1 -33 66.0970 5.54676 2
-1 1 33 65.7235 6.57339 2
0 -1 -33 10.2150 2.44566 4
0 -1 -33 8.66311 3.14666 2
0 -1 33 9.05916 3.06429 2
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0 1 -33 6.86454 2.86230 2
0 1 33 9.40455 2.57470 3
0 1 33 7.50337 3.13129 2
0 1 -33 10.7906 2.09601 4
1 -1 33 8.51473 2.38631 3
1 -1 33 9.31068 2.93409 2
-1 -1 -33 8.10545 3.04481 2
1 1 33 7.55595 3.11226 2
-1 1 -33 9.25323 2.58444 2
1 1 33 10.9292 2.66957 3
2 -1 33 1.89326 2.12074 3
-2 -1 -33 1.92804 2.72644 2
2 1 33 4.47811 2.44048 3
-3 -1 -33 28.2248 4.14514 2
3 -1 33 26.5382 4.29648 2
3 -1 33 35.5227 3.87072 3
3 -1 33 26.6557 3.10015 5
3 1 33 31.3379 4.40573 2
3 1 33 30.7778 4.15699 3
3 1 33 28.3174 3.43454 5
5 -2 -33 3.85729 3.80640 2
-5 2 33 2.41510 4.17280 2
5 2 -33 4.22556 3.16105 2
4 -2 -33 17.4839 4.09324 2
4 2 -33 17.9373 3.45415 2
3 -2 -33 0.53202 3.07442 2
-3 -2 33 2.18172 3.10138 2
3 -2 -33 1.83628 2.47463 4
3 2 -33 6.09227 2.63976 2
-3 2 33 0.76263 3.60641 2
2 -2 -33 0.41713 2.63447 2
2 -2 -33 2.55046 2.48473 4
-2 -2 33 1.31630 2.78970 2
2 -2 -33 0.19328 1.52399 5
-2 2 33 0.37048 2.62526 2
2 2 -33 0.46023 2.54007 2
1 -2 -33 1.95296 2.14467 4
1 -2 -33 -1.9814 2.46909 2
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1 2 -33 2.08140 2.47692 2
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0 -2 -33 12.4799 3.54093 2
0 -2 33 22.6035 3.89123 2
0 2 33 20.4240 3.35882 3
0 2 -33 22.6620 3.36375 2
0 2 33 20.0259 3.82656 2
1 -2 33 15.6948 3.18563 2
1 -2 33 20.4084 2.79872 3
-1 -2 -33 16.1746 3.26307 2
1 2 33 15.9297 3.55612 2
-1 2 -33 13.2338 2.88705 2
1 2 33 13.4596 2.94202 3
-2 -2 -33 13.9333 3.26968 2
2 -2 33 15.7507 2.75843 3
-2 2 -33 17.6110 3.10320 2
2 2 33 16.2928 3.07742 3
3 -2 33 2.43408 2.64436 2
-3 -2 -33 5.17435 2.77567 2
3 -2 33 0.42731 1.42402 5
3 -2 33 -0.8876 1.95496 3
3 2 33 2.19146 2.38980 5
3 2 33 2.97576 2.58635 3
3 2 33 -0.8585 2.87521 2
-3 2 -33 -3.4222 2.18304 2
-5 3 33 1.25535 3.69298 2
4 -3 -33 12.8713 3.33148 4
4 -3 -33 10.1026 3.91579 2
4 3 -33 13.5836 3.52940 2
3 -3 -33 13.7694 3.36999 4
3 -3 -33 12.8253 3.70600 2
-3 -3 33 9.29646 3.48694 2
3 3 -33 8.66179 3.20707 2
2 -3 -33 2.64941 2.76924 4
-2 -3 33 3.13645 2.80557 2
2 -3 -33 -2.4164 2.64819 2
-2 3 33 -2.1102 3.07697 2
-1 -3 33 1.18907 2.64895 2
1 -3 -33 2.13294 2.72737 2
1 -3 -33 1.46105 2.57300 5
1 -3 -33 0.24229 2.56556 4
-1 3 33 3.26145 3.01836 2
0 -3 -33 25.6987 4.73925 2
0 -3 33 34.0945 4.22060 2
0 3 33 34.6225 4.10673 3
0 3 33 29.4632 5.07768 2
-1 -3 -33 30.9365 4.35127 2
1 -3 33 33.7016 3.33210 3
1 -3 33 34.9290 4.13690 2
-1 3 -33 30.0872 4.18699 2
1 3 33 33.3022 4.71144 2
1 3 33 31.4455 4.22302 3
-2 -3 -33 6.36403 2.79877 2
2 -3 33 1.45094 1.90385 3
-2 3 -33 4.36842 2.53697 2
2 3 33 2.44494 2.75015 3
3 -3 33 20.2245 3.24785 3
3 -3 33 9.90951 3.08564 2
-3 -3 -33 15.2530 3.46107 2
3 3 33 21.6124 3.80036 2
3 3 33 18.4309 3.45305 3
3 3 33 20.7364 3.23351 5
-3 -4 33 -2.4082 2.79281 2
3 -4 -33 -1.2810 2.68447 4
3 -4 -33 3.69071 3.01947 2
2 -4 -33 74.2070 6.39522 2
2 -4 -33 71.6554 6.33537 4
-2 -4 33 73.8707 6.42265 2
-2 4 33 70.5184 7.43168 2
1 -4 -33 -1.9540 2.65831 2
-1 -4 33 -3.6022 2.27764 2
1 -4 -33 2.59262 2.33660 4
-1 4 33 1.09824 3.06269 2
0 -4 -33 34.3071 4.33472 2
0 -4 33 30.2083 4.45642 2
0 4 33 32.9456 5.12031 2
0 4 33 32.7027 4.48574 3
1 -4 33 0.27849 2.32741 2
-1 -4 -33 -1.2769 2.56387 2
1 -4 33 -0.0310 1.54473 3
1 4 33 -2.0238 2.38679 3
1 4 33 -1.9048 2.74448 2
2 -4 33 22.7067 3.07624 3
2 4 33 24.2660 4.17631 3
3 -5 -33 6.27904 2.96332 4
3 -5 -33 7.30710 3.21455 2
-3 5 33 8.04384 3.98449 2
-2 -5 33 1.60384 2.98686 2
2 -5 -33 -0.3489 2.78942 4
2 -5 -33 -0.5564 3.14821 2
-1 -5 33 22.2731 3.59068 2
1 -5 -33 20.1443 3.71972 4
-1 5 33 16.9016 4.19070 2
0 -5 -33 4.06506 2.70564 4
0 -5 33 1.82173 2.72751 2
0 5 33 1.45911 3.34867 2
-1 -5 -33 26.4340 4.63799 2
1 -5 33 27.2023 3.95859 2
1 5 33 31.6813 4.64215 2
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4 0 -34 -1.0500 2.75587 2
-4 0 34 -4.2558 3.28185 2
3 0 -34 1.55174 2.96947 2
2 0 -34 16.4032 3.33764 2
2 0 -34 17.4385 2.90487 4
1 0 -34 -0.6841 1.97183 4
1 0 -34 0.20278 2.63491 2
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0 0 -34 5.75655 2.95847 2
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1 0 34 -4.4815 1.92102 3
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3 0 34 -2.4629 2.66302 2
3 0 34 -0.1163 1.56930 5
3 0 34 0.33713 2.18390 3
4 -1 -34 11.2361 3.65623 2
-4 -1 34 13.2480 4.35058 2
3 -1 -34 10.2710 3.03392 4
3 -1 -34 3.27636 3.53297 2
2 -1 -34 39.3272 4.33994 4
2 1 -34 40.0752 5.75668 2
1 -1 -34 36.8130 4.70312 2
1 -1 -34 39.6072 4.01512 4
-1 -1 34 39.8151 4.81541 2
1 1 -34 35.3843 4.02929 4
1 1 -34 34.7773 4.22715 2
0 -1 -34 2.08946 2.15796 4
0 -1 -34 1.12190 2.75911 2
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0 1 -34 2.26698 2.57636 2
0 1 -34 1.57478 1.88241 4
-1 -1 -34 0.64738 2.94642 2
-1 1 -34 1.90474 3.24282 2
1 1 34 -1.3269 1.99986 3
-2 -1 -34 57.8014 6.02218 2
2 -1 34 70.9507 5.37753 3
2 -1 34 70.6674 6.04059 2
2 1 34 69.2582 6.48977 2
2 1 34 70.6215 5.66369 3
3 -1 34 2.08108 1.63578 5
3 -1 34 2.04958 2.85896 2
-3 -1 -34 5.23756 3.00848 2
3 -1 34 5.09675 2.38584 3
3 1 34 5.61892 2.46040 3
3 1 34 5.35045 1.98478 5
3 1 34 4.69300 2.96854 2
-4 -2 34 0.88954 3.72485 2
4 -2 -34 2.28107 3.18962 2
4 2 -34 0.65001 2.77585 2
3 -2 -34 1.25300 3.25018 2
3 -2 -34 -2.5982 2.57783 4
3 2 -34 0.36263 2.62767 2
2 -2 -34 -1.4694 2.70345 2
2 -2 -34 -0.2645 2.39127 4
2 2 -34 -2.9634 2.39564 2
-1 -2 34 3.28931 2.69963 2
1 -2 -34 1.21568 2.63218 2
1 -2 -34 -1.3257 2.28813 4
1 2 -34 -1.5366 2.39561 2
0 -2 -34 2.25045 2.65076 2
0 -2 -34 0.15395 2.78488 4
0 2 34 4.98179 2.62299 3
0 2 -34 -0.1147 2.33918 2
1 -2 34 0.54349 1.90827 3
-1 -2 -34 5.38919 2.70551 2
1 2 34 1.78378 2.29445 3
-1 2 -34 3.44342 2.19668 2
2 -2 34 7.55832 2.35241 3
-2 -2 -34 6.53212 3.05108 2
2 -2 34 5.69743 2.93326 2
2 2 34 5.73265 2.68279 3
2 2 34 7.92606 3.35342 2
-2 2 -34 6.54928 2.63445 2
-4 -3 34 4.73445 3.66640 2
4 -3 -34 6.51564 3.30037 4
4 -3 -34 6.04978 4.29763 2
-4 3 34 1.81503 4.24076 2
3 -3 -34 7.15917 3.33596 4
3 -3 -34 7.93281 3.61377 2
2 -3 -34 52.8078 5.36156 4
1 -3 -34 15.7329 3.27432 4
-1 -3 34 16.3442 3.78724 2
1 -3 -34 20.8539 3.58512 2
0 -3 -34 9.31595 2.90387 2
0 -3 -34 8.97361 2.93048 4
0 3 34 9.27383 2.76465 3
-1 -3 -34 14.5158 3.48095 2
1 -3 34 16.4027 2.89007 3
1 3 34 20.5016 3.51135 3
1 3 34 16.9911 4.40475 2
2 -3 34 6.46785 2.84316 2
-2 -3 -34 1.25039 2.91294 2
2 -3 34 8.11256 2.19738 3
2 3 34 6.12511 2.95353 3
2 3 34 10.2247 2.92472 2
3 -4 -34 -0.7492 2.75428 4
2 -4 -34 37.2998 4.74031 4
1 -4 -34 0.07455 2.90443 4
0 -4 -34 14.4950 3.37524 4
1 4 34 1.41422 3.27898 2
1 4 34 1.82984 2.55577 3
1 -5 -34 0.87264 2.73836 2
-3 0 35 -3.8196 2.63407 2
3 0 -35 0.07580 2.88260 2
2 0 -35 58.0040 4.93913 4
-2 0 35 57.7578 6.69294 2
-1 0 35 -3.6702 2.67202 2
1 0 -35 0.75988 2.64164 2
1 0 -35 1.13476 2.09922 4
0 0 -35 89.4224 7.35412 2
0 0 -35 92.5558 6.53976 4
1 0 35 0.03480 2.67959 2
-1 0 -35 -1.8265 2.51827 2
1 0 35 0.59612 1.97731 3
2 0 35 48.3664 4.53534 3
2 0 35 48.0480 5.22704 2
-2 0 -35 49.6394 4.75424 2
-3 -1 35 -1.3288 3.05835 2
3 -1 -35 -1.4072 2.39775 4
3 -1 -35 -2.6381 2.96313 2
-3 1 35 -1.0020 2.79798 2
-2 -1 35 8.76372 3.51259 2
2 -1 -35 9.77044 2.92462 2
2 -1 -35 7.25173 2.92274 4
-2 1 35 8.17033 3.80779 2
1 -1 -35 4.34136 2.24199 4
-1 -1 35 1.02899 3.57004 2
1 -1 -35 2.66044 2.91618 2
1 1 -35 4.23132 2.27846 4
-1 1 35 1.61775 2.80800 2
0 -1 -35 31.0234 4.45254 2
0 -1 35 32.2787 4.57852 2
0 -1 -35 31.9822 3.88842 4
0 1 -35 31.1244 3.63222 4
0 1 35 34.4631 4.40125 2
-1 -1 -35 4.29489 2.86045 2
1 -1 35 3.62729 2.15060 3
1 -1 35 2.10654 3.03323 2
1 1 35 5.53656 2.91958 2
1 1 35 3.37107 2.20733 3
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2 -1 35 5.50757 2.86498 2
2 -1 35 5.32186 2.24545 3
2 1 35 5.82362 2.73747 2
2 1 35 4.57211 2.35900 3
3 -2 -35 -1.7895 3.16596 2
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3 2 -35 -2.7155 2.53997 2
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2 -2 -35 2.55950 2.87766 2
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2 2 -35 -2.5179 2.36497 2
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1 -2 -35 0.51318 3.00177 2
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1 2 -35 -1.5701 2.34334 2
0 -2 -35 3.37098 2.71331 2
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1 -2 35 22.0804 3.90721 2
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-1 2 -35 22.1167 3.52276 2
1 2 35 17.9459 3.60984 2
1 2 35 16.9064 3.49835 3
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2 -3 -35 0.54556 3.11731 4
2 -3 -35 -2.1941 2.62246 2
-2 3 35 3.24742 3.29520 2
1 -3 -35 2.40118 3.20311 2
1 -3 -35 1.15185 2.68201 4
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-1 3 35 4.50217 3.25380 2
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0 -3 -35 5.29272 3.23826 2
0 -3 -35 5.64226 2.83922 4
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1 -3 35 9.75051 3.10724 2
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2 0 -36 8.37552 3.34898 2
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1 0 -36 -1.2098 2.57263 2
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1 0 -36 1.56081 1.97882 4
0 0 -36 46.9554 4.61346 4
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1 -1 -36 1.06916 2.59221 2
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-1 1 36 2.24570 2.96051 2
0 -1 36 11.2857 3.36764 2
0 -1 -36 12.2822 2.76631 4
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0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 55303
_shelx_res_file
;
TITL m22116 space group P21/c
m22116.res
created by SHELXL-2019/2 at 09:11:26 on 26-Aug-2022
CELL 0.71073 27.9044 11.1207 9.0648 90.000 94.485 90.000
ZERR 8 0.0021 0.0006 0.0007 0.000 0.002 0.000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H N O BR
UNIT 120 104 16 24 8
TEMP -183
SIZE 0.24 0.22 0.05
REM COLR colourless
REM FORM plate
L.S. 10
BOND $H
LIST 4
ACTA
CONF
REM Instructions for potential hydrogen bonds
HTAB O1A N1A
EQIV $1 -x, y-1/2, -z+1/2
HTAB N2A O1A_$1
EQIV $2 -x, y+1/2, -z+1/2
HTAB C3A O2A_$2
HTAB C6A O3A_$1
HTAB O1B N1B
EQIV $3 -x+1, y-1/2, -z+1/2
HTAB N2B O1B_$3
EQIV $4 -x+1, y+1/2, -z+1/2
HTAB C3B O2B_$4
HTAB C6B O3B_$3
HTAB
REM Various planes for r.m.s. deviations and dihedrals:
MPLA C1A C2A C3A C4A C5A C6A C7A N1A N2A C8A O2A O3A
MPLA C9A C10A C11A C12A C13A C14A C15A
MPLA C1B C2B C3B C4B C5B C6B C7B N1B N2B C8B O2B O3B
MPLA C9B C10B C11B C12B C13B C14B C15B
EQIV $5 -x, -y, -z
EQIV $6 1-x, 1-y, -z
RTAB d2cg Br1a_$5 c10a c11a c12a c13a c14a c15a
RTAB d2cg Br1b_$6 c10b c11b c12b c13b c14b c15b
REM MPLA 6 c10a c11a c12a c13a c14a c15a Br1a_$5
REM MPLA 6 c10b c11b c12b c13b c14b c15b Br1b_$6
REM Various torsions:
RTAB tors C8A O2A C9A C10A
RTAB tors O2A C9A C10A C11A
RTAB tors C8B O2B C9B C10B
RTAB tors O2B C9B C10B C11B
FMAP 2
PLAN 20
REM EXTI 0.000302 : not needed.
WGHT 0.024000 0.433600
FVAR 0.13814
BR1A 5 -0.157237 0.000397 -0.272910 11.00000 0.02056 0.01578 =
0.01793 -0.00260 -0.00389 -0.00204
O1A 4 -0.036888 0.327906 0.135150 11.00000 0.01674 0.00963 =
0.01939 0.00068 -0.00327 -0.00007
H1AO 2 -0.021184 0.284962 0.195190 11.00000 -1.50000
O2A 4 0.076231 0.098992 0.576522 11.00000 0.01563 0.01330 =
0.01455 -0.00031 -0.00312 -0.00021
O3A 4 0.053198 0.273042 0.458406 11.00000 0.01951 0.01068 =
0.01926 -0.00019 0.00248 -0.00152
N1A 3 0.000007 0.138791 0.259994 11.00000 0.01213 0.01269 =
0.01432 0.00196 0.00090 0.00180
N2A 3 0.030155 0.088247 0.368655 11.00000 0.01730 0.00930 =
0.01586 0.00052 -0.00253 0.00108
H2AN 2 0.032589 0.010610 0.378325 11.00000 -1.50000
C1A 1 -0.057758 0.125209 0.057055 11.00000 0.01244 0.01125 =
0.01345 0.00074 0.00326 0.00058
C2A 1 -0.063835 0.251036 0.046416 11.00000 0.01202 0.01160 =
0.01532 -0.00145 0.00508 -0.00283
C3A 1 -0.098072 0.299683 -0.055916 11.00000 0.01552 0.01024 =
0.01962 0.00177 0.00195 0.00181
AFIX 43
H3A 2 -0.102322 0.384378 -0.061072 11.00000 -1.20000
AFIX 0
C4A 1 -0.126005 0.225943 -0.150287 11.00000 0.01502 0.01607 =
0.01718 0.00354 0.00175 0.00255
AFIX 43
H4A 2 -0.149393 0.259472 -0.220254 11.00000 -1.20000
AFIX 0
C5A 1 -0.119485 0.101439 -0.141728 11.00000 0.01129 0.01589 =
0.01317 -0.00210 -0.00019 -0.00186
C6A 1 -0.086027 0.051446 -0.039858 11.00000 0.01585 0.01014 =
0.01448 0.00074 0.00488 -0.00094
AFIX 43
H6A 2 -0.082137 -0.033375 -0.035397 11.00000 -1.20000
AFIX 0
C7A 1 -0.024003 0.070444 0.167923 11.00000 0.01450 0.00997 =
0.01645 0.00049 0.00423 0.00050
AFIX 43
H7A 2 -0.019897 -0.014331 0.171790 11.00000 -1.20000
AFIX 0
C8A 1 0.053413 0.164433 0.467603 11.00000 0.01090 0.01338 =
0.01636 -0.00025 0.00451 -0.00048
C9A 1 0.110332 0.163201 0.678698 11.00000 0.01758 0.01708 =
0.01253 -0.00419 -0.00181 -0.00221
AFIX 23
H9A1 2 0.108034 0.132746 0.780527 11.00000 -1.20000
H9A2 2 0.102462 0.250018 0.677625 11.00000 -1.20000
AFIX 0
C10A 1 0.160457 0.145325 0.633799 11.00000 0.01547 0.01723 =
0.01236 -0.00596 -0.00291 -0.00126
C11A 1 0.187567 0.047584 0.686698 11.00000 0.02354 0.01671 =
0.01851 0.00074 -0.00486 -0.00305
AFIX 43
H11A 2 0.175224 -0.004677 0.757468 11.00000 -1.20000
AFIX 0
C12A 1 0.232464 0.025602 0.637175 11.00000 0.01851 0.02531 =
0.02779 -0.00549 -0.00829 0.00615
AFIX 43
H12A 2 0.250802 -0.041479 0.673897 11.00000 -1.20000
AFIX 0
C13A 1 0.250500 0.101354 0.534377 11.00000 0.01371 0.03107 =
0.02571 -0.01180 -0.00003 -0.00195
AFIX 43
H13A 2 0.280911 0.084987 0.498459 11.00000 -1.20000
AFIX 0
C14A 1 0.224493 0.201190 0.483236 11.00000 0.02107 0.02540 =
0.02372 -0.00372 0.00260 -0.00729
AFIX 43
H14A 2 0.237391 0.254413 0.414556 11.00000 -1.20000
AFIX 0
C15A 1 0.179469 0.222957 0.532987 11.00000 0.02136 0.01544 =
0.01762 -0.00260 -0.00294 -0.00070
AFIX 43
H15A 2 0.161541 0.291233 0.498007 11.00000 -1.20000
AFIX 0
BR1B 5 0.331868 0.242738 -0.246677 11.00000 0.01780 0.01828 =
0.01947 -0.00299 -0.00094 -0.00271
O1B 4 0.466661 0.564850 0.123567 11.00000 0.01744 0.01160 =
0.02271 -0.00017 -0.00372 -0.00126
H1BO 2 0.482428 0.525986 0.183495 11.00000 -1.50000
O2B 4 0.580927 0.337667 0.563265 11.00000 0.01741 0.01540 =
0.02590 -0.00028 -0.00701 -0.00121
O3B 4 0.557872 0.511493 0.444685 11.00000 0.02299 0.01180 =
0.02840 -0.00063 -0.00167 -0.00244
N1B 3 0.500173 0.376639 0.257089 11.00000 0.01532 0.01391 =
0.01928 0.00287 -0.00085 0.00147
N2B 3 0.530059 0.326777 0.366369 11.00000 0.01829 0.01149 =
0.02212 0.00151 -0.00576 0.00058
H2BN 2 0.531648 0.248429 0.380611 11.00000 -1.50000
C1B 1 0.440466 0.362594 0.059002 11.00000 0.01259 0.01463 =
0.01616 0.00007 0.00306 0.00024
C2B 1 0.437550 0.488169 0.041268 11.00000 0.01368 0.01329 =
0.01999 -0.00291 0.00344 -0.00209
C3B 1 0.403945 0.537936 -0.062120 11.00000 0.01966 0.01235 =
0.02428 0.00126 0.00278 0.00129
AFIX 43
H3B 2 0.402207 0.622759 -0.073766 11.00000 -1.20000
AFIX 0
C4B 1 0.373081 0.465060 -0.147995 11.00000 0.01892 0.01769 =
0.01895 0.00169 -0.00042 0.00146
AFIX 43
H4B 2 0.349893 0.499454 -0.217909 11.00000 -1.20000
AFIX 0
C5B 1 0.376092 0.340627 -0.131655 11.00000 0.01254 0.01724 =
0.01763 -0.00340 0.00374 -0.00228
C6B 1 0.409531 0.289418 -0.030138 11.00000 0.01667 0.01110 =
0.01857 -0.00042 0.00391 -0.00061
AFIX 43
H6B 2 0.411493 0.204431 -0.020934 11.00000 -1.20000
AFIX 0
C7B 1 0.473457 0.307582 0.172537 11.00000 0.01524 0.01022 =
0.02223 0.00026 0.00094 0.00034
AFIX 43
H7B 2 0.475081 0.222686 0.183473 11.00000 -1.20000
AFIX 0
C8B 1 0.556720 0.403911 0.457334 11.00000 0.01322 0.01649 =
0.01970 0.00106 0.00237 0.00022
C9B 1 0.617079 0.400241 0.660655 11.00000 0.01802 0.02110 =
0.01954 -0.00387 -0.00562 -0.00163
AFIX 23
H9B1 2 0.616291 0.369612 0.762983 11.00000 -1.20000
H9B2 2 0.609811 0.487367 0.661257 11.00000 -1.20000
AFIX 0
C10B 1 0.666058 0.380569 0.607801 11.00000 0.01737 0.01897 =
0.01600 -0.00507 -0.00335 -0.00114
C11B 1 0.691881 0.277645 0.649898 11.00000 0.02289 0.01821 =
0.03074 -0.00196 -0.00408 -0.00141
AFIX 43
H11B 2 0.678700 0.220613 0.713444 11.00000 -1.20000
AFIX 0
C12B 1 0.736925 0.258052 0.599203 11.00000 0.02399 0.02671 =
0.04194 -0.01214 -0.00689 0.00595
AFIX 43
H12B 2 0.754349 0.187171 0.627110 11.00000 -1.20000
AFIX 0
C13B 1 0.756344 0.341288 0.508526 11.00000 0.01976 0.05049 =
0.03205 -0.01422 0.00518 -0.00086
AFIX 43
H13B 2 0.787039 0.327312 0.473303 11.00000 -1.20000
AFIX 0
C14B 1 0.731338 0.445209 0.468489 11.00000 0.02848 0.04105 =
0.02135 -0.00484 0.00423 -0.00983
AFIX 43
H14B 2 0.745077 0.503149 0.407352 11.00000 -1.20000
AFIX 0
C15B 1 0.686213 0.464553 0.517784 11.00000 0.02550 0.02252 =
0.01604 -0.00180 -0.00323 -0.00151
AFIX 43
H15B 2 0.668973 0.535692 0.489816 11.00000 -1.20000
AFIX 0
HKLF 4 1 0 0 1 0 -1 0 1 0 0
REM m22116 space group P21/c
REM wR2 = 0.0635, GooF = S = 1.033, Restrained GooF = 1.033 for all data
REM R1 = 0.0280 for 5004 Fo > 4sig(Fo) and 0.0453 for all 6401 data
REM 391 parameters refined using 0 restraints
END
WGHT 0.0240 0.4336
REM Instructions for potential hydrogen bonds
HTAB O1A N1A
HTAB N2A O1A_$1
HTAB C3A O2A_$2
HTAB C6A O3A_$1
EQIV $7 x, -y+1/2, z+1/2
HTAB C9A O3A_$7
HTAB O1B N1B
HTAB N2B O1B_$3
HTAB C3B O2B_$4
HTAB C6B O3B_$3
REM Highest difference peak 0.362, deepest hole -0.388, 1-sigma level 0.074
Q1 1 0.3717 0.4027 -0.1154 11.00000 0.05 0.36
Q2 1 -0.1963 -0.0027 -0.3658 11.00000 0.05 0.36
Q3 1 0.6613 0.2471 0.7255 11.00000 0.05 0.36
Q4 1 -0.0480 0.1007 0.1190 11.00000 0.05 0.35
Q5 1 0.3997 0.3066 -0.1037 11.00000 0.05 0.34
Q6 1 -0.0598 0.1820 0.0580 11.00000 0.05 0.34
Q7 1 0.0007 0.2224 0.2684 11.00000 0.05 0.34
Q8 1 -0.0641 0.1006 -0.0025 11.00000 0.05 0.33
Q9 1 0.0195 0.1210 0.2947 11.00000 0.05 0.31
Q10 1 -0.1690 0.0388 -0.1573 11.00000 0.05 0.31
Q11 1 0.3695 0.2447 -0.1485 11.00000 0.05 0.31
Q12 1 0.4589 0.3389 0.1109 11.00000 0.05 0.29
Q13 1 0.2089 0.0432 0.6494 11.00000 0.05 0.29
Q14 1 0.3269 0.2974 -0.3667 11.00000 0.05 0.29
Q15 1 -0.1195 0.1612 -0.1548 11.00000 0.05 0.29
Q16 1 0.0904 0.2806 0.5770 11.00000 0.05 0.29
Q17 1 0.3918 0.4885 -0.1027 11.00000 0.05 0.29
Q18 1 0.5326 0.5231 0.3034 11.00000 0.05 0.29
Q19 1 0.3309 0.3031 -0.1305 11.00000 0.05 0.29
Q20 1 0.6525 0.2556 0.8450 11.00000 0.05 0.28
;
_shelx_res_checksum 8367
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
Br Br1A -0.15724(2) 0.00040(2) -0.27291(2) 0.01837(6) Uani d 1 . .
O O1A -0.03689(5) 0.32791(12) 0.13515(17) 0.0155(3) Uani d 1 . .
H H1AO -0.0212(8) 0.285(2) 0.195(3) 0.023 Uiso d 1 . .
O O2A 0.07623(4) 0.09899(12) 0.57652(16) 0.0147(3) Uani d 1 . .
O O3A 0.05320(5) 0.27304(12) 0.45841(16) 0.0164(3) Uani d 1 . .
N N1A 0.00001(5) 0.13879(14) 0.25999(19) 0.0131(4) Uani d 1 . .
N N2A 0.03016(6) 0.08825(15) 0.3687(2) 0.0144(4) Uani d 1 . .
H H2AN 0.0326(8) 0.011(2) 0.378(3) 0.022 Uiso d 1 . .
C C1A -0.05776(6) 0.12521(17) 0.0571(2) 0.0123(4) Uani d 1 . .
C C2A -0.06384(6) 0.25104(17) 0.0464(2) 0.0128(4) Uani d 1 . .
C C3A -0.09807(7) 0.29968(17) -0.0559(2) 0.0151(4) Uani d 1 . .
H H3A -0.102322 0.384378 -0.061072 0.018 Uiso calc 1 . .
C C4A -0.12600(7) 0.22594(18) -0.1503(2) 0.0161(4) Uani d 1 . .
H H4A -0.149393 0.259472 -0.220254 0.019 Uiso calc 1 . .
C C5A -0.11949(6) 0.10144(17) -0.1417(2) 0.0135(4) Uani d 1 . .
C C6A -0.08603(7) 0.05145(17) -0.0399(2) 0.0133(4) Uani d 1 . .
H H6A -0.082137 -0.033375 -0.035397 0.016 Uiso calc 1 . .
C C7A -0.02400(7) 0.07044(17) 0.1679(2) 0.0135(4) Uani d 1 . .
H H7A -0.019897 -0.014331 0.171790 0.016 Uiso calc 1 . .
C C8A 0.05341(7) 0.16443(17) 0.4676(2) 0.0134(4) Uani d 1 . .
C C9A 0.11033(7) 0.16320(18) 0.6787(2) 0.0159(4) Uani d 1 . .
H H9A1 0.108034 0.132746 0.780527 0.019 Uiso calc 1 . .
H H9A2 0.102462 0.250018 0.677625 0.019 Uiso calc 1 . .
C C10A 0.16046(7) 0.14533(18) 0.6338(2) 0.0152(4) Uani d 1 . .
C C11A 0.18757(7) 0.04758(18) 0.6867(3) 0.0199(5) Uani d 1 . .
H H11A 0.175224 -0.004677 0.757468 0.024 Uiso calc 1 . .
C C12A 0.23246(7) 0.0256(2) 0.6372(3) 0.0244(5) Uani d 1 . .
H H12A 0.250802 -0.041479 0.673897 0.029 Uiso calc 1 . .
C C13A 0.25050(7) 0.1014(2) 0.5344(3) 0.0236(5) Uani d 1 . .
H H13A 0.280911 0.084987 0.498459 0.028 Uiso calc 1 . .
C C14A 0.22449(7) 0.2012(2) 0.4832(3) 0.0234(5) Uani d 1 . .
H H14A 0.237391 0.254413 0.414556 0.028 Uiso calc 1 . .
C C15A 0.17947(7) 0.22296(18) 0.5330(2) 0.0184(5) Uani d 1 . .
H H15A 0.161541 0.291233 0.498007 0.022 Uiso calc 1 . .
Br Br1B 0.33187(2) 0.24274(2) -0.24668(2) 0.01864(6) Uani d 1 . .
O O1B 0.46666(5) 0.56485(12) 0.12357(18) 0.0175(3) Uani d 1 . .
H H1BO 0.4824(8) 0.526(2) 0.183(3) 0.026 Uiso d 1 . .
O O2B 0.58093(5) 0.33767(12) 0.56327(17) 0.0200(3) Uani d 1 . .
O O3B 0.55787(5) 0.51149(12) 0.44468(17) 0.0213(3) Uani d 1 . .
N N1B 0.50017(6) 0.37664(15) 0.2571(2) 0.0163(4) Uani d 1 . .
N N2B 0.53006(6) 0.32678(15) 0.3664(2) 0.0177(4) Uani d 1 . .
H H2BN 0.5316(8) 0.248(2) 0.381(3) 0.027 Uiso d 1 . .
C C1B 0.44047(7) 0.36259(17) 0.0590(2) 0.0144(4) Uani d 1 . .
C C2B 0.43755(7) 0.48817(17) 0.0413(2) 0.0155(4) Uani d 1 . .
C C3B 0.40395(7) 0.53794(18) -0.0621(2) 0.0187(5) Uani d 1 . .
H H3B 0.402207 0.622759 -0.073766 0.022 Uiso calc 1 . .
C C4B 0.37308(7) 0.46506(18) -0.1480(2) 0.0186(5) Uani d 1 . .
H H4B 0.349893 0.499454 -0.217909 0.022 Uiso calc 1 . .
C C5B 0.37609(7) 0.34063(18) -0.1317(2) 0.0157(4) Uani d 1 . .
C C6B 0.40953(7) 0.28942(18) -0.0301(2) 0.0153(4) Uani d 1 . .
H H6B 0.411493 0.204431 -0.020934 0.018 Uiso calc 1 . .
C C7B 0.47346(7) 0.30758(17) 0.1725(2) 0.0159(5) Uani d 1 . .
H H7B 0.475081 0.222686 0.183473 0.019 Uiso calc 1 . .
C C8B 0.55672(7) 0.40391(18) 0.4573(2) 0.0164(4) Uani d 1 . .
C C9B 0.61708(7) 0.40024(19) 0.6607(3) 0.0199(5) Uani d 1 . .
H H9B1 0.616291 0.369612 0.762983 0.024 Uiso calc 1 . .
H H9B2 0.609811 0.487367 0.661257 0.024 Uiso calc 1 . .
C C10B 0.66606(7) 0.38057(18) 0.6078(2) 0.0177(5) Uani d 1 . .
C C11B 0.69188(7) 0.27764(19) 0.6499(3) 0.0243(5) Uani d 1 . .
H H11B 0.678700 0.220613 0.713444 0.029 Uiso calc 1 . .
C C12B 0.73692(8) 0.2581(2) 0.5992(3) 0.0314(6) Uani d 1 . .
H H12B 0.754349 0.187171 0.627110 0.038 Uiso calc 1 . .
C C13B 0.75634(8) 0.3413(2) 0.5085(3) 0.0339(6) Uani d 1 . .
H H13B 0.787039 0.327312 0.473303 0.041 Uiso calc 1 . .
C C14B 0.73134(8) 0.4452(2) 0.4685(3) 0.0302(6) Uani d 1 . .
H H14B 0.745077 0.503149 0.407352 0.036 Uiso calc 1 . .
C C15B 0.68621(7) 0.4646(2) 0.5178(2) 0.0216(5) Uani d 1 . .
H H15B 0.668973 0.535692 0.489816 0.026 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
Br1A 0.02056(10) 0.01578(11) 0.01793(13) -0.00204(8) -0.00389(8) -0.00260(9)
O1A 0.0167(7) 0.0096(7) 0.0194(9) -0.0001(5) -0.0033(6) 0.0007(6)
O2A 0.0156(7) 0.0133(7) 0.0146(9) -0.0002(5) -0.0031(6) -0.0003(6)
O3A 0.0195(7) 0.0107(7) 0.0193(9) -0.0015(5) 0.0025(6) -0.0002(6)
N1A 0.0121(8) 0.0127(8) 0.0143(11) 0.0018(6) 0.0009(7) 0.0020(7)
N2A 0.0173(8) 0.0093(8) 0.0159(11) 0.0011(7) -0.0025(7) 0.0005(7)
C1A 0.0124(9) 0.0113(9) 0.0134(12) 0.0006(7) 0.0033(8) 0.0007(8)
C2A 0.0120(9) 0.0116(9) 0.0153(12) -0.0028(8) 0.0051(8) -0.0014(8)
C3A 0.0155(10) 0.0102(9) 0.0196(13) 0.0018(8) 0.0019(9) 0.0018(8)
C4A 0.0150(10) 0.0161(10) 0.0172(13) 0.0025(8) 0.0018(8) 0.0035(9)
C5A 0.0113(9) 0.0159(10) 0.0132(12) -0.0019(8) -0.0002(8) -0.0021(8)
C6A 0.0158(10) 0.0101(9) 0.0145(12) -0.0009(8) 0.0049(8) 0.0007(8)
C7A 0.0145(9) 0.0100(9) 0.0164(13) 0.0005(7) 0.0042(8) 0.0005(8)
C8A 0.0109(9) 0.0134(10) 0.0164(12) -0.0005(7) 0.0045(8) -0.0003(8)
C9A 0.0176(10) 0.0171(10) 0.0125(12) -0.0022(8) -0.0018(9) -0.0042(8)
C10A 0.0155(10) 0.0172(10) 0.0124(12) -0.0013(8) -0.0029(8) -0.0060(8)
C11A 0.0235(11) 0.0167(10) 0.0185(13) -0.0030(9) -0.0049(9) 0.0007(9)
C12A 0.0185(11) 0.0253(12) 0.0278(15) 0.0061(9) -0.0083(9) -0.0055(10)
C13A 0.0137(10) 0.0311(13) 0.0257(15) -0.0020(9) 0.0000(9) -0.0118(10)
C14A 0.0211(11) 0.0254(12) 0.0237(14) -0.0073(9) 0.0026(10) -0.0037(10)
C15A 0.0214(10) 0.0154(10) 0.0176(13) -0.0007(8) -0.0029(9) -0.0026(9)
Br1B 0.01780(10) 0.01828(11) 0.01947(13) -0.00271(8) -0.00094(8) -0.00299(9)
O1B 0.0174(7) 0.0116(7) 0.0227(10) -0.0013(6) -0.0037(6) -0.0002(6)
O2B 0.0174(7) 0.0154(7) 0.0259(10) -0.0012(6) -0.0070(6) -0.0003(6)
O3B 0.0230(7) 0.0118(7) 0.0284(10) -0.0024(6) -0.0017(7) -0.0006(6)
N1B 0.0153(9) 0.0139(9) 0.0193(12) 0.0015(6) -0.0009(8) 0.0029(7)
N2B 0.0183(9) 0.0115(8) 0.0221(12) 0.0006(7) -0.0058(8) 0.0015(8)
C1B 0.0126(9) 0.0146(10) 0.0162(12) 0.0002(8) 0.0031(8) 0.0001(8)
C2B 0.0137(9) 0.0133(10) 0.0200(13) -0.0021(8) 0.0034(8) -0.0029(9)
C3B 0.0197(10) 0.0124(10) 0.0243(14) 0.0013(8) 0.0028(9) 0.0013(9)
C4B 0.0189(10) 0.0177(10) 0.0189(13) 0.0015(8) -0.0004(9) 0.0017(9)
C5B 0.0125(9) 0.0172(10) 0.0176(13) -0.0023(8) 0.0037(8) -0.0034(9)
C6B 0.0167(10) 0.0111(10) 0.0186(13) -0.0006(8) 0.0039(9) -0.0004(8)
C7B 0.0152(10) 0.0102(9) 0.0222(13) 0.0003(8) 0.0009(9) 0.0003(8)
C8B 0.0132(10) 0.0165(10) 0.0197(13) 0.0002(8) 0.0024(8) 0.0011(9)
C9B 0.0180(10) 0.0211(11) 0.0195(13) -0.0016(8) -0.0056(9) -0.0039(9)
C10B 0.0174(10) 0.0190(11) 0.0160(13) -0.0011(8) -0.0033(9) -0.0051(9)
C11B 0.0229(11) 0.0182(11) 0.0307(15) -0.0014(9) -0.0041(10) -0.0020(10)
C12B 0.0240(12) 0.0267(13) 0.0419(17) 0.0059(10) -0.0069(11) -0.0121(12)
C13B 0.0198(12) 0.0505(16) 0.0320(17) -0.0009(11) 0.0052(11) -0.0142(13)
C14B 0.0285(12) 0.0410(15) 0.0213(15) -0.0098(11) 0.0042(10) -0.0048(11)
C15B 0.0255(11) 0.0225(11) 0.0160(13) -0.0015(9) -0.0032(9) -0.0018(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
C2A O1A H1AO . . 105.5(16) ?
C8A O2A C9A . . 116.62(15) ?
C7A N1A N2A . . 119.20(16) ?
C8A N2A N1A . . 117.02(16) ?
C8A N2A H2AN . . 121.5(15) ?
N1A N2A H2AN . . 121.3(15) ?
C6A C1A C2A . . 118.64(18) ?
C6A C1A C7A . . 119.38(17) ?
C2A C1A C7A . . 121.97(18) ?
O1A C2A C3A . . 118.04(17) ?
O1A C2A C1A . . 121.65(18) ?
C3A C2A C1A . . 120.30(18) ?
C4A C3A C2A . . 120.53(18) ?
C4A C3A H3A . . 119.7 ?
C2A C3A H3A . . 119.7 ?
C3A C4A C5A . . 119.28(18) ?
C3A C4A H4A . . 120.4 ?
C5A C4A H4A . . 120.4 ?
C6A C5A C4A . . 121.02(18) ?
C6A C5A Br1A . . 119.71(14) ?
C4A C5A Br1A . . 119.27(15) ?
C5A C6A C1A . . 120.22(18) ?
C5A C6A H6A . . 119.9 ?
C1A C6A H6A . . 119.9 ?
N1A C7A C1A . . 118.65(17) ?
N1A C7A H7A . . 120.7 ?
C1A C7A H7A . . 120.7 ?
O3A C8A O2A . . 126.12(19) ?
O3A C8A N2A . . 125.18(19) ?
O2A C8A N2A . . 108.70(16) ?
O2A C9A C10A . . 109.76(16) ?
O2A C9A H9A1 . . 109.7 ?
C10A C9A H9A1 . . 109.7 ?
O2A C9A H9A2 . . 109.7 ?
C10A C9A H9A2 . . 109.7 ?
H9A1 C9A H9A2 . . 108.2 ?
C11A C10A C15A . . 119.15(19) ?
C11A C10A C9A . . 120.30(19) ?
C15A C10A C9A . . 120.48(18) ?
C12A C11A C10A . . 120.6(2) ?
C12A C11A H11A . . 119.7 ?
C10A C11A H11A . . 119.7 ?
C13A C12A C11A . . 119.9(2) ?
C13A C12A H12A . . 120.1 ?
C11A C12A H12A . . 120.1 ?
C12A C13A C14A . . 120.4(2) ?
C12A C13A H13A . . 119.8 ?
C14A C13A H13A . . 119.8 ?
C13A C14A C15A . . 119.6(2) ?
C13A C14A H14A . . 120.2 ?
C15A C14A H14A . . 120.2 ?
C14A C15A C10A . . 120.4(2) ?
C14A C15A H15A . . 119.8 ?
C10A C15A H15A . . 119.8 ?
C2B O1B H1BO . . 107.9(17) ?
C8B O2B C9B . . 116.93(16) ?
C7B N1B N2B . . 119.03(17) ?
N1B N2B C8B . . 117.14(17) ?
N1B N2B H2BN . . 122.0(15) ?
C8B N2B H2BN . . 120.8(15) ?
C6B C1B C2B . . 118.97(18) ?
C6B C1B C7B . . 119.38(18) ?
C2B C1B C7B . . 121.59(18) ?
O1B C2B C3B . . 117.61(18) ?
O1B C2B C1B . . 122.20(18) ?
C3B C2B C1B . . 120.18(18) ?
C4B C3B C2B . . 120.41(19) ?
C4B C3B H3B . . 119.8 ?
C2B C3B H3B . . 119.8 ?
C3B C4B C5B . . 119.61(19) ?
C3B C4B H4B . . 120.2 ?
C5B C4B H4B . . 120.2 ?
C6B C5B C4B . . 120.81(18) ?
C6B C5B Br1B . . 120.43(15) ?
C4B C5B Br1B . . 118.72(15) ?
C5B C6B C1B . . 120.00(18) ?
C5B C6B H6B . . 120.0 ?
C1B C6B H6B . . 120.0 ?
N1B C7B C1B . . 118.39(18) ?
N1B C7B H7B . . 120.8 ?
C1B C7B H7B . . 120.8 ?
O3B C8B O2B . . 126.55(19) ?
O3B C8B N2B . . 125.7(2) ?
O2B C8B N2B . . 107.76(17) ?
O2B C9B C10B . . 109.90(17) ?
O2B C9B H9B1 . . 109.7 ?
C10B C9B H9B1 . . 109.7 ?
O2B C9B H9B2 . . 109.7 ?
C10B C9B H9B2 . . 109.7 ?
H9B1 C9B H9B2 . . 108.2 ?
C15B C10B C11B . . 119.4(2) ?
C15B C10B C9B . . 120.74(19) ?
C11B C10B C9B . . 119.9(2) ?
C12B C11B C10B . . 120.1(2) ?
C12B C11B H11B . . 119.9 ?
C10B C11B H11B . . 119.9 ?
C13B C12B C11B . . 120.0(2) ?
C13B C12B H12B . . 120.0 ?
C11B C12B H12B . . 120.0 ?
C12B C13B C14B . . 120.3(2) ?
C12B C13B H13B . . 119.9 ?
C14B C13B H13B . . 119.9 ?
C13B C14B C15B . . 119.8(2) ?
C13B C14B H14B . . 120.1 ?
C15B C14B H14B . . 120.1 ?
C14B C15B C10B . . 120.4(2) ?
C14B C15B H15B . . 119.8 ?
C10B C15B H15B . . 119.8 ?
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
Br1A C5A . 1.8949(19) ?
O1A C2A . 1.360(2) ?
O1A H1AO . 0.82(2) ?
O2A C8A . 1.346(2) ?
O2A C9A . 1.461(2) ?
O3A C8A . 1.211(2) ?
N1A C7A . 1.279(2) ?
N1A N2A . 1.365(2) ?
N2A C8A . 1.361(3) ?
N2A H2AN . 0.87(2) ?
C1A C6A . 1.399(3) ?
C1A C2A . 1.412(3) ?
C1A C7A . 1.456(3) ?
C2A C3A . 1.388(3) ?
C3A C4A . 1.381(3) ?
C3A H3A . 0.9500 ?
C4A C5A . 1.398(3) ?
C4A H4A . 0.9500 ?
C5A C6A . 1.378(3) ?
C6A H6A . 0.9500 ?
C7A H7A . 0.9500 ?
C9A C10A . 1.500(3) ?
C9A H9A1 . 0.9900 ?
C9A H9A2 . 0.9900 ?
C10A C11A . 1.388(3) ?
C10A C15A . 1.392(3) ?
C11A C12A . 1.385(3) ?
C11A H11A . 0.9500 ?
C12A C13A . 1.380(3) ?
C12A H12A . 0.9500 ?
C13A C14A . 1.386(3) ?
C13A H13A . 0.9500 ?
C14A C15A . 1.389(3) ?
C14A H14A . 0.9500 ?
C15A H15A . 0.9500 ?
Br1B C5B . 1.896(2) ?
O1B C2B . 1.360(2) ?
O1B H1BO . 0.80(2) ?
O2B C8B . 1.349(2) ?
O2B C9B . 1.464(2) ?
O3B C8B . 1.203(2) ?
N1B C7B . 1.282(2) ?
N1B N2B . 1.362(2) ?
N2B C8B . 1.369(3) ?
N2B H2BN . 0.88(2) ?
C1B C6B . 1.397(3) ?
C1B C2B . 1.407(3) ?
C1B C7B . 1.460(3) ?
C2B C3B . 1.388(3) ?
C3B C4B . 1.378(3) ?
C3B H3B . 0.9500 ?
C4B C5B . 1.394(3) ?
C4B H4B . 0.9500 ?
C5B C6B . 1.381(3) ?
C6B H6B . 0.9500 ?
C7B H7B . 0.9500 ?
C9B C10B . 1.499(3) ?
C9B H9B1 . 0.9900 ?
C9B H9B2 . 0.9900 ?
C10B C15B . 1.388(3) ?
C10B C11B . 1.390(3) ?
C11B C12B . 1.389(3) ?
C11B H11B . 0.9500 ?
C12B C13B . 1.377(4) ?
C12B H12B . 0.9500 ?
C13B C14B . 1.384(4) ?
C13B H13B . 0.9500 ?
C14B C15B . 1.385(3) ?
C14B H14B . 0.9500 ?
C15B H15B . 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
O1A H1AO N1A . 0.82(2) 1.81(2) 2.565(2) 151(2) yes
N2A H2AN O1A 2_545 0.87(2) 2.04(2) 2.902(2) 171(2) yes
C3A H3A O2A 2 0.95 2.50 3.392(2) 155.9 yes
C6A H6A O3A 2_545 0.95 2.38 3.296(2) 160.7 yes
O1B H1BO N1B . 0.80(2) 1.84(2) 2.558(2) 148(2) yes
N2B H2BN O1B 2_645 0.88(2) 2.04(2) 2.915(2) 171(2) yes
C3B H3B O2B 2_655 0.95 2.44 3.360(2) 164.1 yes
C6B H6B O3B 2_645 0.95 2.39 3.297(2) 159.2 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
C7A N1A N2A C8A . . . . -177.37(18) ?
C6A C1A C2A O1A . . . . -178.68(17) ?
C7A C1A C2A O1A . . . . 3.0(3) ?
C6A C1A C2A C3A . . . . 1.6(3) ?
C7A C1A C2A C3A . . . . -176.79(18) ?
O1A C2A C3A C4A . . . . 179.10(18) ?
C1A C2A C3A C4A . . . . -1.2(3) ?
C2A C3A C4A C5A . . . . 0.0(3) ?
C3A C4A C5A C6A . . . . 0.6(3) ?
C3A C4A C5A Br1A . . . . -179.20(15) ?
C4A C5A C6A C1A . . . . -0.2(3) ?
Br1A C5A C6A C1A . . . . 179.65(14) ?
C2A C1A C6A C5A . . . . -0.9(3) ?
C7A C1A C6A C5A . . . . 177.49(18) ?
N2A N1A C7A C1A . . . . 177.06(16) ?
C6A C1A C7A N1A . . . . -176.88(18) ?
C2A C1A C7A N1A . . . . 1.5(3) ?
C9A O2A C8A O3A . . . . -11.2(3) ?
C9A O2A C8A N2A . . . . 169.09(15) ?
N1A N2A C8A O3A . . . . -7.7(3) ?
N1A N2A C8A O2A . . . . 171.98(15) ?
C8A O2A C9A C10A . . . . -98.12(19) ?
O2A C9A C10A C11A . . . . -88.3(2) ?
O2A C9A C10A C15A . . . . 88.5(2) ?
C15A C10A C11A C12A . . . . -1.6(3) ?
C9A C10A C11A C12A . . . . 175.19(19) ?
C10A C11A C12A C13A . . . . 0.0(3) ?
C11A C12A C13A C14A . . . . 1.7(3) ?
C12A C13A C14A C15A . . . . -1.8(3) ?
C13A C14A C15A C10A . . . . 0.1(3) ?
C11A C10A C15A C14A . . . . 1.6(3) ?
C9A C10A C15A C14A . . . . -175.24(19) ?
C7B N1B N2B C8B . . . . -177.79(18) ?
C6B C1B C2B O1B . . . . -179.66(18) ?
C7B C1B C2B O1B . . . . 3.1(3) ?
C6B C1B C2B C3B . . . . 0.8(3) ?
C7B C1B C2B C3B . . . . -176.38(19) ?
O1B C2B C3B C4B . . . . -179.38(19) ?
C1B C2B C3B C4B . . . . 0.2(3) ?
C2B C3B C4B C5B . . . . -0.7(3) ?
C3B C4B C5B C6B . . . . 0.2(3) ?
C3B C4B C5B Br1B . . . . 178.02(16) ?
C4B C5B C6B C1B . . . . 0.8(3) ?
Br1B C5B C6B C1B . . . . -176.99(15) ?
C2B C1B C6B C5B . . . . -1.3(3) ?
C7B C1B C6B C5B . . . . 175.98(19) ?
N2B N1B C7B C1B . . . . 178.03(17) ?
C6B C1B C7B N1B . . . . -177.23(19) ?
C2B C1B C7B N1B . . . . 0.0(3) ?
C9B O2B C8B O3B . . . . -8.9(3) ?
C9B O2B C8B N2B . . . . 171.53(16) ?
N1B N2B C8B O3B . . . . -4.0(3) ?
N1B N2B C8B O2B . . . . 175.60(16) ?
C8B O2B C9B C10B . . . . -98.0(2) ?
O2B C9B C10B C15B . . . . 95.9(2) ?
O2B C9B C10B C11B . . . . -84.5(2) ?
C15B C10B C11B C12B . . . . -1.5(3) ?
C9B C10B C11B C12B . . . . 178.9(2) ?
C10B C11B C12B C13B . . . . 0.8(4) ?
C11B C12B C13B C14B . . . . 0.6(4) ?
C12B C13B C14B C15B . . . . -1.1(4) ?
C13B C14B C15B C10B . . . . 0.4(3) ?
C11B C10B C15B C14B . . . . 1.0(3) ?
C9B C10B C15B C14B . . . . -179.5(2) ?
_cod_database_fobs_code 2244177