#------------------------------------------------------------------------------
#$Date: 2022-10-01 03:04:56 +0100 (Sat, 01 Oct 2022) $
#$Revision: 278297 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244191.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_2244191
loop_
_publ_author_name
'Stapf, Manuel'
'Leibiger, Betty'
'Schwarzer, Anke'
'Mazik, Monika'
_publ_section_title
;
Crystal structures of
2-[3,5-bis(bromomethyl)-2,4,6-triethylbenzyl]isoindoline-1,3-dione and
2-{5-(bromomethyl)-3-[(1,3-dioxoisoindolin-2-yl)methyl]-2,4,6-triethylbenzyl}isoindoline-1,3-dione
;
_journal_coeditor_code ZQ2264
_journal_issue 9
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 919
_journal_page_last 923
_journal_paper_doi 10.1107/S205698902100788X
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'C31 H29 Br N2 O4'
_chemical_formula_moiety 'C31 H29 Br N2 O4'
_chemical_formula_sum 'C31 H29 Br N2 O4'
_chemical_formula_weight 573.47
_chemical_name_systematic
2-{5-(Bromomethyl)-3-[(1,3-dioxoisoindolin-2-yl)methyl]-2,4,6-triethylbenzyl}isoindoline-1,3-dione
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 109.168(13)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.899(2)
_cell_length_b 12.9748(15)
_cell_length_c 16.763(3)
_cell_measurement_reflns_used 3744
_cell_measurement_temperature 153(2)
_cell_measurement_theta_max 22.50
_cell_measurement_theta_min 2.02
_cell_volume 2650.0(7)
_computing_cell_refinement
;
X-AREA (Stoe, 2009)
;
_computing_data_collection
;
X-AREA (Stoe, 2009)
;
_computing_data_reduction
;
X-RED (Stoe, 2009)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2008)
;
_computing_publication_material
;
WinGX (Farrugia, 2012), publCIF (Westrip, 2010)
and shelXle
(H\"ubschle et al., 2011)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 153
_diffrn_detector 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device '2-circle goniometer'
_diffrn_measurement_device_type 'STOE IPDS 2'
_diffrn_measurement_method 'rotation method'
_diffrn_radiation_monochromator 'plane graphite'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.1151
_diffrn_reflns_av_unetI/netI 0.0602
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 26391
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.500
_diffrn_reflns_theta_min 1.742
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current 40
_diffrn_source_power 2.000
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 1.592
_exptl_absorpt_correction_T_max 0.8444
_exptl_absorpt_correction_T_min 0.6952
_exptl_absorpt_correction_type integration
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.437
_exptl_crystal_description piece
_exptl_crystal_F_000 1184
_exptl_crystal_size_max 0.180
_exptl_crystal_size_mid 0.180
_exptl_crystal_size_min 0.150
_refine_diff_density_max 0.375
_refine_diff_density_min -0.669
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.118
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 346
_refine_ls_number_reflns 4941
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.118
_refine_ls_R_factor_all 0.0953
_refine_ls_R_factor_gt 0.0560
_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^)+(0.0406P)^2^+4.7828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1096
_refine_ls_wR_factor_ref 0.1288
_reflns_number_gt 3442
_reflns_number_total 4941
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zq2264sup1.cif
_cod_data_source_block 2
_cod_original_cell_volume 2649.9(7)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2244191
_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 0.763
_shelx_estimated_absorpt_t_max 0.796
_shelx_hkl_file
;
2 0 0 71.21 12.52 0
-2 0 0 73.54 14.92 0
2 0 0 70.40 10.57 0
-2 0 0 75.91 12.90 0
4 0 0 19.33 9.50 0
-4 0 0 5.09 11.54 0
-4 0 0 15.84 9.71 0
4 0 0 11.36 9.58 0
6 0 0 157.48 7.64 0
6 0 0 136.45 7.06 0
-6 0 0 125.48 10.05 0
8 0 0 0.74 7.27 0
-8 0 0 -9.90 8.52 0
8 0 0 -4.31 6.05 0
10 0 0 52.28 7.12 0
10 0 0 40.03 6.37 0
-10 0 0 54.55 10.00 0
-12 0 0 -10.87 9.09 0
12 0 0 15.18 6.85 0
12 0 0 4.31 6.77 0
14 0 0 -12.97 8.13 0
14 0 0 -15.93 8.95 0
-14 0 0 2.09 6.78 0
16 0 0 35.64 7.11 0
16 0 0 8.47 6.73 0
-16 0 0 72.40 10.30 0
1 -1 0 9.88 15.28 0
1 1 0 6.27 13.12 0
1 -1 0 5.88 14.18 0
-1 1 0 6.48 15.25 0
-1 -1 0 10.51 11.40 0
-1 1 0 7.40 10.65 0
-1 -1 0 4.72 13.62 0
1 1 0 10.20 14.80 0
-2 1 0 393.90 15.29 0
2 -1 0 453.23 15.11 0
2 1 0 424.77 14.36 0
-2 -1 0 470.05 17.37 0
2 1 0 436.92 16.26 0
-2 -1 0 455.88 20.55 0
-3 -1 0 4685.00 32.53 0
-3 1 0 4432.26 31.89 0
-3 -1 0 4277.30 33.38 0
3 1 0 4114.22 30.04 0
3 -1 0 4646.96 31.86 0
3 1 0 4522.86 33.24 0
4 -1 0 340.15 10.87 0
-4 -1 0 399.36 12.34 0
4 -1 0 428.16 14.16 0
4 1 0 376.63 12.22 0
4 1 0 412.36 12.13 0
-4 -1 0 401.66 14.95 0
-4 1 0 385.21 11.31 0
5 -1 0 509.10 12.99 0
5 1 0 472.50 11.12 0
5 -1 0 478.82 12.10 0
-5 -1 0 552.65 10.77 0
-5 -1 0 476.82 10.56 0
5 1 0 523.72 12.82 0
-5 1 0 516.57 11.04 0
6 -1 0 54.35 9.36 0
6 -1 0 57.36 8.31 0
6 1 0 59.81 6.29 0
-6 -1 0 56.32 8.48 0
-6 -1 0 59.67 7.50 0
-6 1 0 57.08 6.88 0
6 1 0 69.15 7.31 0
-7 -1 0 350.59 10.00 0
7 -1 0 338.58 10.50 0
7 1 0 337.27 9.76 0
-7 -1 0 332.33 8.84 0
7 1 0 343.43 10.79 0
7 -1 0 330.44 9.89 0
-7 1 0 338.05 8.53 0
8 -1 0 4.78 6.22 0
8 1 0 5.76 5.60 0
8 -1 0 -4.12 7.76 0
-8 -1 0 -1.23 5.85 0
-8 1 0 8.86 7.89 0
8 1 0 -4.18 4.97 0
9 -1 0 24.96 7.93 0
-9 -1 0 12.45 9.24 0
9 -1 0 27.07 6.60 0
-9 1 0 4.70 6.72 0
9 1 0 17.80 6.57 0
9 1 0 5.08 5.81 0
-10 -1 0 1.60 6.82 0
10 1 0 -11.00 9.28 0
10 1 0 -2.91 6.09 0
10 -1 0 0.57 7.84 0
-10 1 0 1.14 9.45 0
10 -1 0 -11.64 9.46 0
-11 -1 0 12.70 9.20 0
11 -1 0 4.03 6.08 0
11 1 0 -5.32 8.10 0
11 -1 0 4.08 6.56 0
-11 1 0 15.15 6.72 0
11 1 0 4.24 6.88 0
12 -1 0 3.75 7.67 0
12 1 0 3.11 9.05 0
-12 -1 0 15.71 9.18 0
-12 1 0 28.88 8.94 0
12 1 0 3.00 7.20 0
12 -1 0 11.74 7.00 0
-13 -1 0 83.27 8.02 0
13 -1 0 97.58 9.65 0
-13 1 0 71.27 9.65 0
13 1 0 67.38 9.21 0
13 -1 0 89.64 7.89 0
13 1 0 95.89 9.32 0
14 1 0 -32.98 9.54 0
14 -1 0 -12.38 6.89 0
-14 -1 0 21.97 6.75 0
-14 1 0 4.91 7.17 0
14 1 0 -7.32 8.47 0
14 -1 0 -0.25 5.90 0
15 -1 0 12.28 7.33 0
15 1 0 8.86 6.75 0
-15 1 0 16.30 9.63 0
15 -1 0 20.80 7.39 0
15 1 0 7.04 8.58 0
-15 -1 0 5.77 7.24 0
16 1 0 11.10 4.95 0
16 1 0 18.70 8.54 0
-16 1 0 -3.73 7.42 0
16 1 0 -0.88 4.60 0
-16 -1 0 26.93 7.32 0
16 -1 0 -0.99 7.03 0
16 -1 0 -3.94 7.75 0
0 -2 0 3215.51 31.80 0
0 2 0 2729.77 29.44 0
0 2 0 2923.19 34.22 0
1 2 0 152.56 15.37 0
1 -2 0 169.77 16.69 0
-1 2 0 150.02 17.31 0
-1 2 0 138.50 12.59 0
-1 -2 0 163.97 11.65 0
1 -2 0 161.00 15.47 0
-2 -2 0 454.85 18.39 0
-2 -2 0 458.00 12.59 0
-2 2 0 423.94 16.80 0
2 2 0 451.81 18.05 0
2 -2 0 462.31 15.15 0
2 2 0 434.55 13.58 0
2 -2 0 475.85 16.71 0
3 2 0 5184.44 30.88 0
3 2 0 5359.58 37.52 0
-3 -2 0 5262.95 37.78 0
3 -2 0 5733.04 31.71 0
-3 2 0 5229.56 31.35 0
-3 -2 0 5517.64 30.36 0
4 2 0 75.52 10.98 0
4 2 0 75.28 10.45 0
-4 -2 0 66.06 10.63 0
4 -2 0 55.86 10.05 0
-4 -2 0 65.86 6.73 0
-4 2 0 58.68 11.42 0
5 2 0 124.58 7.79 0
-5 2 0 132.67 8.38 0
5 -2 0 127.42 10.72 0
-5 -2 0 123.89 9.00 0
-5 -2 0 137.71 7.63 0
5 2 0 151.18 10.58 0
6 -2 0 573.99 10.13 0
6 2 0 578.01 10.83 0
6 2 0 556.03 11.33 0
-6 2 0 561.71 10.28 0
-6 -2 0 538.18 13.11 0
-6 -2 0 584.19 11.57 0
6 -2 0 465.79 10.20 0
7 -2 0 10.43 7.49 0
7 -2 0 -3.82 8.44 0
-7 -2 0 3.55 9.16 0
7 2 0 0.10 5.46 0
-7 -2 0 5.60 5.69 0
-7 2 0 -15.89 8.80 0
7 2 0 -6.62 9.04 0
8 2 0 147.60 6.29 0
8 -2 0 152.90 8.11 0
-8 -2 0 164.85 9.23 0
8 -2 0 150.25 6.64 0
-8 2 0 155.89 8.98 0
-8 -2 0 134.05 6.08 0
8 2 0 171.00 9.17 0
9 2 0 38.93 9.32 0
-9 -2 0 32.18 8.18 0
-9 2 0 23.12 9.47 0
9 2 0 25.12 5.76 0
-9 -2 0 26.88 6.78 0
9 -2 0 29.84 8.28 0
9 -2 0 31.12 6.90 0
-10 -2 0 26.81 6.84 0
10 -2 0 23.70 7.11 0
10 -2 0 34.75 8.07 0
10 2 0 28.31 6.60 0
-10 2 0 25.48 9.66 0
10 2 0 26.22 8.27 0
11 2 0 0.95 8.47 0
11 2 0 32.84 8.19 0
-11 2 0 6.67 6.77 0
-11 -2 0 25.40 6.87 0
11 -2 0 30.04 7.41 0
11 -2 0 35.59 9.51 0
12 -2 0 8.00 8.32 0
12 2 0 0.22 9.01 0
12 2 0 23.90 9.66 0
12 -2 0 7.53 6.63 0
-12 -2 0 3.37 9.79 0
-12 2 0 6.90 8.97 0
-13 -2 0 25.12 6.66 0
-13 2 0 -1.70 7.24 0
13 2 0 -2.44 9.64 0
13 -2 0 -11.89 9.72 0
13 2 0 -6.35 9.24 0
13 -2 0 12.40 9.06 0
14 -2 0 5.07 7.53 0
-14 2 0 -6.38 8.70 0
14 -2 0 5.50 7.03 0
-14 -2 0 9.41 8.90 0
14 2 0 -6.82 6.57 0
14 2 0 -0.24 7.04 0
-15 -2 0 -16.80 9.95 0
-15 2 0 8.02 6.97 0
15 -2 0 -29.66 7.23 0
15 2 0 0.89 8.56 0
15 -2 0 -5.05 8.10 0
15 2 0 9.11 8.20 0
16 2 0 -17.79 10.55 0
-16 2 0 33.18 8.92 0
16 -2 0 -2.09 7.55 0
16 -2 0 15.21 7.51 0
16 2 0 40.35 9.53 0
-16 -2 0 29.64 10.45 0
1 -3 0 847.26 18.25 0
-1 -3 0 883.43 17.12 0
1 3 0 813.27 16.94 0
-1 3 0 790.45 16.41 0
-1 3 0 797.98 17.95 0
1 -3 0 873.16 17.94 0
2 -3 0 11.22 8.55 0
-2 3 0 2.58 12.12 0
2 3 0 1.46 11.99 0
-2 3 0 5.74 12.00 0
2 3 0 5.31 12.03 0
-2 -3 0 9.94 9.06 0
2 -3 0 15.87 8.53 0
3 3 0 3397.03 22.11 0
3 -3 0 3368.10 28.40 0
-3 -3 0 3737.75 23.58 0
-3 3 0 3175.64 22.37 0
-3 -3 0 3250.16 28.59 0
3 3 0 3358.06 27.68 0
3 -3 0 3514.49 22.96 0
-4 -3 0 1017.05 12.04 0
4 -3 0 1121.88 17.25 0
-4 3 0 1061.41 13.42 0
-4 -3 0 1024.29 16.69 0
4 3 0 1031.50 12.54 0
4 -3 0 1105.54 15.14 0
4 3 0 1061.03 15.19 0
5 3 0 15.59 5.77 0
5 3 0 14.03 7.82 0
-5 -3 0 20.28 7.46 0
5 -3 0 25.02 9.32 0
-5 -3 0 8.59 5.90 0
-5 3 0 23.37 6.93 0
6 3 0 453.20 9.82 0
6 3 0 416.19 8.37 0
-6 -3 0 439.92 12.19 0
6 -3 0 439.20 10.99 0
-6 3 0 414.35 11.06 0
-6 -3 0 468.96 10.36 0
-7 -3 0 55.49 8.03 0
7 3 0 52.06 8.80 0
7 -3 0 30.63 6.06 0
-7 3 0 54.61 6.43 0
-7 -3 0 34.99 6.60 0
7 3 0 34.35 7.75 0
8 3 0 3.37 5.12 0
-8 -3 0 -1.36 5.70 0
8 3 0 10.23 8.06 0
8 -3 0 8.57 5.34 0
-8 -3 0 3.57 5.12 0
-8 3 0 -0.99 7.93 0
8 -3 0 0.44 6.87 0
9 3 0 -6.69 7.11 0
-9 -3 0 17.32 8.54 0
9 -3 0 2.81 8.38 0
-9 -3 0 -10.30 9.14 0
-9 3 0 22.11 8.54 0
9 3 0 0.49 8.52 0
9 -3 0 -1.17 8.52 0
-10 -3 0 268.46 9.55 0
-10 -3 0 206.14 10.09 0
10 3 0 200.57 9.70 0
10 3 0 252.43 8.83 0
10 -3 0 222.46 10.07 0
-10 3 0 213.73 9.63 0
10 -3 0 185.20 8.87 0
-11 -3 0 -7.58 7.91 0
-11 -3 0 2.41 8.80 0
11 3 0 -4.49 8.10 0
11 -3 0 8.59 7.74 0
11 -3 0 8.79 8.92 0
11 3 0 -3.25 5.73 0
-11 3 0 22.02 8.76 0
12 3 0 29.25 7.84 0
-12 -3 0 30.02 9.33 0
-12 3 0 1.21 10.01 0
12 3 0 28.76 6.97 0
12 -3 0 11.83 8.33 0
12 -3 0 25.86 8.68 0
13 3 0 -0.07 7.10 0
-13 -3 0 17.05 9.63 0
13 -3 0 5.18 6.77 0
13 -3 0 1.18 8.16 0
-13 3 0 7.98 7.06 0
13 3 0 -4.29 8.65 0
14 3 0 34.97 7.71 0
14 3 0 40.36 8.49 0
14 -3 0 24.85 9.19 0
14 -3 0 32.02 10.59 0
-14 3 0 1.25 9.53 0
-14 -3 0 17.66 9.63 0
15 -3 0 7.37 7.48 0
-15 -3 0 40.93 7.19 0
15 3 0 -5.38 7.92 0
15 3 0 40.21 6.81 0
-15 3 0 38.99 10.05 0
15 -3 0 23.90 9.43 0
16 -3 0 1.28 8.73 0
16 3 0 -0.69 9.08 0
-16 -3 0 9.51 6.93 0
16 -3 0 -12.13 4.86 0
16 3 0 7.91 4.77 0
-16 3 0 17.88 7.23 0
0 -4 0 1036.32 15.00 0
0 4 0 1012.63 17.29 0
0 4 0 935.60 17.10 0
-1 -4 0 -7.01 10.28 0
1 -4 0 -7.51 10.36 0
1 4 0 4.88 10.23 0
-1 4 0 4.94 7.88 0
-1 4 0 2.07 7.70 0
1 -4 0 22.01 10.94 0
2 4 0 828.25 11.97 0
2 -4 0 893.82 15.03 0
-2 4 0 836.91 14.08 0
2 4 0 813.17 15.97 0
-2 4 0 852.72 14.92 0
-2 -4 0 918.83 14.11 0
2 -4 0 886.04 14.04 0
-3 4 0 516.10 10.84 0
3 4 0 542.67 13.84 0
-3 4 0 523.28 13.56 0
-3 -4 0 621.80 12.30 0
3 -4 0 585.68 13.21 0
3 -4 0 551.30 11.63 0
3 4 0 529.18 10.16 0
-4 -4 0 44.54 9.04 0
-4 -4 0 59.12 8.27 0
4 -4 0 52.67 9.16 0
-4 4 0 42.64 7.00 0
4 4 0 54.56 8.85 0
4 -4 0 56.26 9.59 0
4 4 0 42.42 9.26 0
5 -4 0 8.84 6.65 0
-5 4 0 25.46 6.94 0
5 -4 0 7.82 9.51 0
-5 -4 0 22.33 8.79 0
-5 -4 0 24.76 7.48 0
5 4 0 25.06 8.39 0
5 4 0 24.37 9.81 0
6 4 0 1773.68 13.37 0
6 -4 0 1813.99 15.03 0
-6 4 0 1746.29 15.22 0
6 -4 0 1812.10 17.53 0
-6 -4 0 1857.80 14.71 0
-6 -4 0 1855.98 17.67 0
6 4 0 1734.53 15.82 0
7 4 0 40.17 7.52 0
-7 4 0 22.82 8.30 0
-7 -4 0 36.91 6.10 0
7 4 0 27.80 6.09 0
7 -4 0 16.51 8.14 0
7 -4 0 33.51 8.34 0
-7 -4 0 39.23 7.76 0
8 4 0 29.79 9.47 0
-8 -4 0 21.00 6.14 0
8 4 0 19.08 8.28 0
-8 -4 0 25.60 8.13 0
8 -4 0 45.00 6.71 0
8 -4 0 34.85 8.08 0
-8 4 0 24.19 6.48 0
9 -4 0 32.40 9.01 0
9 4 0 18.18 9.16 0
-9 -4 0 11.65 9.68 0
9 -4 0 1.85 9.05 0
-9 -4 0 -6.75 8.49 0
-9 4 0 29.72 9.20 0
9 -4 0 11.98 8.19 0
9 4 0 11.32 6.30 0
10 -4 0 3.48 7.37 0
-10 -4 0 5.10 6.69 0
-10 -4 0 5.37 8.16 0
10 4 0 4.21 7.91 0
-10 4 0 3.43 7.96 0
10 4 0 2.62 7.65 0
10 -4 0 -0.77 6.13 0
-11 4 0 38.01 8.28 0
11 -4 0 13.73 8.54 0
-11 -4 0 18.42 6.49 0
11 4 0 -5.81 7.59 0
11 -4 0 13.04 7.64 0
11 4 0 13.02 7.45 0
11 -4 0 9.14 8.01 0
-11 -4 0 24.02 7.68 0
-12 4 0 -1.64 9.41 0
12 -4 0 11.72 8.07 0
-12 -4 0 14.43 9.36 0
12 -4 0 9.62 9.04 0
12 -4 0 -6.98 8.03 0
12 4 0 12.66 9.52 0
12 4 0 -12.06 6.19 0
-12 -4 0 7.22 8.53 0
13 -4 0 58.13 9.57 0
13 -4 0 84.90 8.64 0
-13 -4 0 65.00 7.33 0
-13 4 0 60.18 9.85 0
13 4 0 95.91 8.77 0
13 4 0 89.58 9.08 0
13 -4 0 80.12 8.39 0
-14 4 0 2.88 7.69 0
14 -4 0 7.25 10.59 0
14 4 0 -1.07 7.19 0
14 4 0 9.80 9.29 0
14 -4 0 -5.91 7.31 0
-14 -4 0 4.40 7.52 0
14 -4 0 -7.35 7.63 0
-15 4 0 17.11 7.49 0
15 -4 0 9.65 9.58 0
-15 -4 0 7.65 9.87 0
15 4 0 -3.50 9.36 0
15 -4 0 1.27 9.61 0
15 -4 0 0.42 8.90 0
15 4 0 4.15 10.01 0
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;
_shelx_hkl_checksum 48843
_shelx_res_file
;
TITL BL0272_01_a.res in P2(1)/n
BL0272_01_a.res
created by SHELXL-2018/3 at 09:48:07 on 11-Sep-2019
CELL 0.71073 12.8993 12.9748 16.7625 90.000 109.168 90.000
ZERR 4.000 0.0021 0.0015 0.0029 0.000 0.013 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H N O BR
UNIT 124 116 8 16 4
LIST 4
L.S. 10
BOND $h
conf
omit -2 51
temp -120.15
size 0.18 0.18 0.15
acta
mpla 6 c1 > c6
mpla 13 n1 o1 o2 c11 > c18
mpla 13 n2 o3 o4 c22 > c29
mpla 6 c1 > c6
htab C30 O4
htab C21 O3
htab C19 O3
htab C10 O1
EQIV $1 1/2+x,1/2-y,1/2+z
HTAB C31 O2_$1
EQIV $2 1-x,1-y,1-z
HTAB C31 O3_$2
EQIV $3 1/2-x,1/2+y,3/2-z
HTAB C25 O4_$3
EQIV $4 -x, -y, -z+1
HTAB C10 O1_$4
FMAP 2
PLAN 20
WGHT 0.040600 4.782800
FVAR 0.30284
MOLE 1
BR1 5 0.523160 0.010136 0.798235 11.00000 0.05193 0.03658 =
0.02700 0.00699 0.00013 0.00049
O1 4 0.047988 -0.104886 0.449574 11.00000 0.02670 0.02241 =
0.03407 -0.00264 0.01320 -0.00461
O2 4 0.249967 0.115221 0.345443 11.00000 0.03013 0.02157 =
0.02513 0.00305 0.00566 -0.00509
O3 4 0.284138 0.561184 0.477530 11.00000 0.05442 0.02491 =
0.02032 0.00440 0.01040 0.00319
O4 4 0.414759 0.435893 0.747265 11.00000 0.02837 0.01836 =
0.02184 0.00212 0.00542 0.00003
N1 3 0.150931 0.022785 0.414731 11.00000 0.01311 0.01741 =
0.02161 -0.00058 0.00398 -0.00323
N2 3 0.355279 0.473138 0.604536 11.00000 0.02442 0.01119 =
0.02024 0.00022 0.00702 0.00387
C1 1 0.449441 0.111780 0.634074 11.00000 0.02147 0.01829 =
0.02236 -0.00052 0.00723 0.00213
C2 1 0.349517 0.069988 0.582604 11.00000 0.01997 0.01592 =
0.02083 -0.00297 0.00777 -0.00253
C3 1 0.268591 0.136364 0.533012 11.00000 0.01596 0.01763 =
0.01596 -0.00319 0.00381 -0.00255
C4 1 0.288613 0.243656 0.531393 11.00000 0.01927 0.01865 =
0.01319 -0.00225 0.00538 0.00202
C5 1 0.390319 0.283391 0.582735 11.00000 0.02054 0.01199 =
0.02065 -0.00213 0.00638 0.00050
C6 1 0.469204 0.218603 0.636395 11.00000 0.01811 0.01545 =
0.02087 -0.00277 0.00591 -0.00385
C7 1 0.537517 0.040650 0.687198 11.00000 0.02579 0.02042 =
0.02643 -0.00126 0.00084 0.00074
AFIX 23
H7A 2 0.610137 0.072469 0.695790 11.00000 -1.20000
H7B 2 0.534643 -0.024818 0.656210 11.00000 -1.20000
AFIX 0
C8 1 0.331259 -0.045400 0.582364 11.00000 0.02439 0.01608 =
0.02155 0.00115 0.00277 -0.00312
AFIX 23
H8A 2 0.251482 -0.059241 0.565489 11.00000 -1.20000
H8B 2 0.365684 -0.072266 0.640352 11.00000 -1.20000
AFIX 0
C9 1 0.378783 -0.102973 0.522280 11.00000 0.03839 0.01829 =
0.02964 -0.00169 0.00474 0.00441
AFIX 137
H9A 2 0.347178 -0.074907 0.465118 11.00000 -1.50000
H9B 2 0.360849 -0.176407 0.521898 11.00000 -1.50000
H9C 2 0.458681 -0.094380 0.541444 11.00000 -1.50000
AFIX 0
C10 1 0.154976 0.094208 0.483364 11.00000 0.01761 0.02037 =
0.02051 -0.00558 0.00229 0.00040
AFIX 23
H10A 2 0.125136 0.058587 0.523338 11.00000 -1.20000
H10B 2 0.106010 0.153176 0.459244 11.00000 -1.20000
AFIX 0
C11 1 0.091506 -0.069085 0.401071 11.00000 0.01254 0.01641 =
0.02411 0.00383 0.00212 0.00120
C12 1 0.094036 -0.110917 0.319743 11.00000 0.01565 0.01672 =
0.02284 -0.00192 0.00417 0.00330
C13 1 0.045699 -0.200293 0.277550 11.00000 0.02237 0.01624 =
0.03471 -0.00285 0.00393 -0.00043
AFIX 43
H13 2 0.004436 -0.245548 0.300068 11.00000 -1.20000
AFIX 0
C14 1 0.061176 -0.219333 0.201195 11.00000 0.03218 0.02479 =
0.03300 -0.01040 0.00037 0.00102
AFIX 43
H14 2 0.030282 -0.279843 0.170719 11.00000 -1.20000
AFIX 0
C15 1 0.120859 -0.152442 0.167233 11.00000 0.03976 0.03089 =
0.02209 -0.00595 0.00412 0.00696
AFIX 43
H15 2 0.129331 -0.167964 0.114331 11.00000 -1.20000
AFIX 0
C16 1 0.168248 -0.062749 0.210569 11.00000 0.02396 0.02691 =
0.01897 0.00583 0.00150 0.00477
AFIX 43
H16 2 0.208922 -0.016774 0.188112 11.00000 -1.20000
AFIX 0
C17 1 0.153504 -0.043845 0.287136 11.00000 0.01563 0.01800 =
0.01896 0.00318 -0.00007 0.00398
C18 1 0.192485 0.042538 0.348972 11.00000 0.01598 0.01588 =
0.01766 0.00339 -0.00015 0.00324
C19 1 0.200295 0.314880 0.477306 11.00000 0.02151 0.01719 =
0.02342 0.00109 0.00410 -0.00029
AFIX 23
H19A 2 0.161193 0.280095 0.423207 11.00000 -1.20000
H19B 2 0.235232 0.377749 0.464336 11.00000 -1.20000
AFIX 0
C20 1 0.116262 0.346242 0.520842 11.00000 0.02273 0.02191 =
0.03817 0.00085 0.00707 0.00517
AFIX 137
H20A 2 0.062288 0.393705 0.484201 11.00000 -1.50000
H20B 2 0.154562 0.380291 0.574660 11.00000 -1.50000
H20C 2 0.078697 0.284601 0.531248 11.00000 -1.50000
AFIX 0
C21 1 0.418848 0.396631 0.575268 11.00000 0.02461 0.01367 =
0.02137 -0.00412 0.00626 -0.00176
AFIX 23
H21A 2 0.497534 0.406640 0.607674 11.00000 -1.20000
H21B 2 0.409090 0.411132 0.515254 11.00000 -1.20000
AFIX 0
C22 1 0.295100 0.552198 0.551335 11.00000 0.02629 0.01323 =
0.03265 -0.00146 0.00726 -0.00294
C23 1 0.253119 0.618389 0.606058 11.00000 0.02218 0.01534 =
0.02699 -0.00069 0.00661 -0.00291
C24 1 0.188270 0.706258 0.586385 11.00000 0.03268 0.01904 =
0.04032 0.00224 0.01167 0.00071
AFIX 43
H24 2 0.160892 0.732223 0.530356 11.00000 -1.20000
AFIX 0
C25 1 0.165216 0.754777 0.653491 11.00000 0.03039 0.01694 =
0.05734 -0.00261 0.02020 0.00378
AFIX 43
H25 2 0.119858 0.814329 0.642455 11.00000 -1.20000
AFIX 0
C26 1 0.206883 0.718043 0.735223 11.00000 0.03790 0.03001 =
0.05268 -0.00772 0.02652 0.00117
AFIX 43
H26 2 0.191087 0.753832 0.779323 11.00000 -1.20000
AFIX 0
C27 1 0.271404 0.629834 0.754203 11.00000 0.03255 0.02687 =
0.03079 -0.00280 0.01740 -0.00213
AFIX 43
H27 2 0.299597 0.604064 0.810256 11.00000 -1.20000
AFIX 0
C28 1 0.292752 0.581215 0.687818 11.00000 0.02355 0.01557 =
0.02993 -0.00241 0.01010 -0.00363
C29 1 0.360982 0.488507 0.687585 11.00000 0.02224 0.01469 =
0.02235 -0.00166 0.00868 -0.00612
C30 1 0.575016 0.262146 0.697197 11.00000 0.01912 0.01804 =
0.02097 -0.00475 0.00075 -0.00124
AFIX 23
H30A 2 0.601244 0.216141 0.746913 11.00000 -1.20000
H30B 2 0.559601 0.330376 0.717248 11.00000 -1.20000
AFIX 0
C31 1 0.665898 0.273983 0.658026 11.00000 0.02405 0.01905 =
0.03251 -0.00398 0.00734 0.00188
AFIX 137
H31A 2 0.686331 0.205933 0.642623 11.00000 -1.50000
H31B 2 0.730070 0.306456 0.698949 11.00000 -1.50000
H31C 2 0.639585 0.317153 0.607382 11.00000 -1.50000
AFIX 0
HKLF 4
REM BL0272_01_a.res in P2(1)/n
REM wR2 = 0.1288, GooF = S = 1.118, Restrained GooF = 1.118 for all data
REM R1 = 0.0560 for 3442 Fo > 4sig(Fo) and 0.0953 for all 4941 data
REM 346 parameters refined using 0 restraints
END
WGHT 0.0406 4.7828
REM Highest difference peak 0.375, deepest hole -0.669, 1-sigma level 0.086
Q1 1 0.4826 0.0782 0.6714 11.00000 0.05 0.37
Q2 1 0.1189 0.6186 0.6956 11.00000 0.05 0.35
Q3 1 0.2945 0.0243 0.6473 11.00000 0.05 0.34
Q4 1 0.6332 0.0600 0.7287 11.00000 0.05 0.31
Q5 1 0.1362 0.4405 0.4109 11.00000 0.05 0.30
Q6 1 0.1631 0.6641 0.4128 11.00000 0.05 0.29
Q7 1 0.4333 0.5546 0.6471 11.00000 0.05 0.29
Q8 1 0.3623 -0.0417 0.4444 11.00000 0.05 0.28
Q9 1 0.5006 -0.0766 0.9048 11.00000 0.05 0.28
Q10 1 0.2786 0.5760 0.8453 11.00000 0.05 0.28
Q11 1 0.3192 0.5414 0.6960 11.00000 0.05 0.28
Q12 1 0.2232 0.1161 0.5197 11.00000 0.05 0.28
Q13 1 0.2251 0.6632 0.7346 11.00000 0.05 0.28
Q14 1 0.6047 -0.0031 0.8665 11.00000 0.05 0.27
Q15 1 -0.0184 -0.3468 0.2730 11.00000 0.05 0.27
Q16 1 0.2605 0.5174 0.7869 11.00000 0.05 0.27
Q17 1 0.2225 0.6637 0.5925 11.00000 0.05 0.26
Q18 1 0.5647 0.1748 0.7501 11.00000 0.05 0.26
Q19 1 0.3382 0.5399 0.4043 11.00000 0.05 0.26
Q20 1 0.2949 0.1834 0.5298 11.00000 0.05 0.26
;
_shelx_res_checksum 25704
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.52316(4) 0.01014(4) 0.79824(3) 0.04165(17) Uani d 1 . .
O O1 0.0480(2) -0.1049(2) 0.44957(19) 0.0269(7) Uani d 1 . .
O O2 0.2500(2) 0.1152(2) 0.34544(18) 0.0264(7) Uani d 1 . .
O O3 0.2841(3) 0.5612(2) 0.47753(19) 0.0337(7) Uani d 1 . .
O O4 0.4148(2) 0.4359(2) 0.74727(17) 0.0235(6) Uani d 1 . .
N N1 0.1509(2) 0.0228(2) 0.4147(2) 0.0178(7) Uani d 1 . .
N N2 0.3553(3) 0.4731(2) 0.6045(2) 0.0187(7) Uani d 1 . .
C C1 0.4494(3) 0.1118(3) 0.6341(3) 0.0207(8) Uani d 1 . .
C C2 0.3495(3) 0.0700(3) 0.5826(2) 0.0186(8) Uani d 1 . .
C C3 0.2686(3) 0.1364(3) 0.5330(2) 0.0169(8) Uani d 1 . .
C C4 0.2886(3) 0.2437(3) 0.5314(2) 0.0170(8) Uani d 1 . .
C C5 0.3903(3) 0.2834(3) 0.5827(2) 0.0178(8) Uani d 1 . .
C C6 0.4692(3) 0.2186(3) 0.6364(2) 0.0183(8) Uani d 1 . .
C C7 0.5375(3) 0.0407(3) 0.6872(3) 0.0261(10) Uani d 1 . .
H H7A 0.610137 0.072469 0.695790 0.031 Uiso calc 1 . .
H H7B 0.534643 -0.024818 0.656210 0.031 Uiso calc 1 . .
C C8 0.3313(3) -0.0454(3) 0.5824(3) 0.0218(9) Uani d 1 . .
H H8A 0.251482 -0.059241 0.565489 0.026 Uiso calc 1 . .
H H8B 0.365684 -0.072266 0.640352 0.026 Uiso calc 1 . .
C C9 0.3788(4) -0.1030(3) 0.5223(3) 0.0303(10) Uani d 1 . .
H H9A 0.347178 -0.074907 0.465118 0.046 Uiso calc 1 . .
H H9B 0.360849 -0.176407 0.521898 0.046 Uiso calc 1 . .
H H9C 0.458681 -0.094380 0.541444 0.046 Uiso calc 1 . .
C C10 0.1550(3) 0.0942(3) 0.4834(2) 0.0205(9) Uani d 1 . .
H H10A 0.125136 0.058587 0.523338 0.025 Uiso calc 1 . .
H H10B 0.106010 0.153176 0.459244 0.025 Uiso calc 1 . .
C C11 0.0915(3) -0.0691(3) 0.4011(3) 0.0186(8) Uani d 1 . .
C C12 0.0940(3) -0.1109(3) 0.3197(2) 0.0189(8) Uani d 1 . .
C C13 0.0457(3) -0.2003(3) 0.2775(3) 0.0258(10) Uani d 1 . .
H H13 0.004436 -0.245548 0.300068 0.031 Uiso calc 1 . .
C C14 0.0612(4) -0.2193(3) 0.2012(3) 0.0325(11) Uani d 1 . .
H H14 0.030282 -0.279843 0.170719 0.039 Uiso calc 1 . .
C C15 0.1209(4) -0.1524(3) 0.1672(3) 0.0324(11) Uani d 1 . .
H H15 0.129331 -0.167964 0.114331 0.039 Uiso calc 1 . .
C C16 0.1682(3) -0.0627(3) 0.2106(3) 0.0246(9) Uani d 1 . .
H H16 0.208922 -0.016774 0.188112 0.030 Uiso calc 1 . .
C C17 0.1535(3) -0.0438(3) 0.2871(2) 0.0189(8) Uani d 1 . .
C C18 0.1925(3) 0.0425(3) 0.3490(2) 0.0179(8) Uani d 1 . .
C C19 0.2003(3) 0.3149(3) 0.4773(3) 0.0215(9) Uani d 1 . .
H H19A 0.161193 0.280095 0.423207 0.026 Uiso calc 1 . .
H H19B 0.235232 0.377749 0.464336 0.026 Uiso calc 1 . .
C C20 0.1163(3) 0.3462(3) 0.5208(3) 0.0283(10) Uani d 1 . .
H H20A 0.062288 0.393705 0.484201 0.042 Uiso calc 1 . .
H H20B 0.154562 0.380291 0.574660 0.042 Uiso calc 1 . .
H H20C 0.078697 0.284601 0.531248 0.042 Uiso calc 1 . .
C C21 0.4188(3) 0.3966(3) 0.5753(3) 0.0202(9) Uani d 1 . .
H H21A 0.497534 0.406640 0.607674 0.024 Uiso calc 1 . .
H H21B 0.409090 0.411132 0.515254 0.024 Uiso calc 1 . .
C C22 0.2951(3) 0.5522(3) 0.5513(3) 0.0246(9) Uani d 1 . .
C C23 0.2531(3) 0.6184(3) 0.6061(3) 0.0219(9) Uani d 1 . .
C C24 0.1883(4) 0.7063(3) 0.5864(3) 0.0308(10) Uani d 1 . .
H H24 0.160892 0.732223 0.530356 0.037 Uiso calc 1 . .
C C25 0.1652(4) 0.7548(3) 0.6535(3) 0.0335(11) Uani d 1 . .
H H25 0.119858 0.814329 0.642455 0.040 Uiso calc 1 . .
C C26 0.2069(4) 0.7180(3) 0.7352(3) 0.0373(12) Uani d 1 . .
H H26 0.191087 0.753832 0.779323 0.045 Uiso calc 1 . .
C C27 0.2714(4) 0.6298(3) 0.7542(3) 0.0284(10) Uani d 1 . .
H H27 0.299597 0.604064 0.810256 0.034 Uiso calc 1 . .
C C28 0.2928(3) 0.5812(3) 0.6878(3) 0.0227(9) Uani d 1 . .
C C29 0.3610(3) 0.4885(3) 0.6876(2) 0.0194(8) Uani d 1 . .
C C30 0.5750(3) 0.2621(3) 0.6972(3) 0.0208(9) Uani d 1 . .
H H30A 0.601244 0.216141 0.746913 0.025 Uiso calc 1 . .
H H30B 0.559601 0.330376 0.717248 0.025 Uiso calc 1 . .
C C31 0.6659(3) 0.2740(3) 0.6580(3) 0.0257(9) Uani d 1 . .
H H31A 0.686331 0.205933 0.642623 0.039 Uiso calc 1 . .
H H31B 0.730070 0.306456 0.698949 0.039 Uiso calc 1 . .
H H31C 0.639585 0.317153 0.607382 0.039 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
Br1 0.0519(3) 0.0366(3) 0.0270(2) 0.0005(2) 0.0001(2) 0.0070(2)
O1 0.0267(15) 0.0224(15) 0.0341(17) -0.0046(13) 0.0132(14) -0.0026(13)
O2 0.0301(16) 0.0216(15) 0.0251(16) -0.0051(13) 0.0057(13) 0.0031(12)
O3 0.054(2) 0.0249(16) 0.0203(17) 0.0032(15) 0.0104(15) 0.0044(12)
O4 0.0284(15) 0.0184(14) 0.0218(15) 0.0000(12) 0.0054(13) 0.0021(12)
N1 0.0131(15) 0.0174(16) 0.0216(17) -0.0032(13) 0.0040(13) -0.0006(13)
N2 0.0244(17) 0.0112(15) 0.0202(17) 0.0039(13) 0.0070(14) 0.0002(13)
C1 0.021(2) 0.0183(19) 0.022(2) 0.0021(16) 0.0072(17) -0.0005(16)
C2 0.0200(19) 0.0159(19) 0.021(2) -0.0025(16) 0.0078(17) -0.0030(15)
C3 0.0160(19) 0.0176(19) 0.0160(19) -0.0026(15) 0.0038(16) -0.0032(15)
C4 0.0193(19) 0.0186(19) 0.0132(19) 0.0020(16) 0.0054(15) -0.0022(15)
C5 0.021(2) 0.0120(18) 0.021(2) 0.0005(15) 0.0064(17) -0.0021(15)
C6 0.0181(19) 0.0155(18) 0.021(2) -0.0039(15) 0.0059(16) -0.0028(16)
C7 0.026(2) 0.020(2) 0.026(2) 0.0007(17) 0.0008(18) -0.0013(17)
C8 0.024(2) 0.0161(18) 0.022(2) -0.0031(16) 0.0028(18) 0.0011(15)
C9 0.038(3) 0.018(2) 0.030(2) 0.0044(19) 0.005(2) -0.0017(18)
C10 0.0176(19) 0.020(2) 0.021(2) 0.0004(16) 0.0023(17) -0.0056(16)
C11 0.0125(18) 0.0164(19) 0.024(2) 0.0012(15) 0.0021(17) 0.0038(16)
C12 0.0157(19) 0.0167(19) 0.023(2) 0.0033(16) 0.0042(16) -0.0019(16)
C13 0.022(2) 0.0162(19) 0.035(3) -0.0004(16) 0.0039(19) -0.0028(17)
C14 0.032(2) 0.025(2) 0.033(3) 0.0010(19) 0.000(2) -0.0104(19)
C15 0.040(3) 0.031(2) 0.022(2) 0.007(2) 0.004(2) -0.0060(19)
C16 0.024(2) 0.027(2) 0.019(2) 0.0048(17) 0.0015(17) 0.0058(17)
C17 0.0156(19) 0.0180(19) 0.019(2) 0.0040(15) -0.0001(16) 0.0032(15)
C18 0.0160(19) 0.0159(19) 0.018(2) 0.0032(15) -0.0002(16) 0.0034(15)
C19 0.022(2) 0.0172(19) 0.023(2) -0.0003(16) 0.0041(17) 0.0011(16)
C20 0.023(2) 0.022(2) 0.038(3) 0.0052(18) 0.007(2) 0.0009(19)
C21 0.025(2) 0.0137(18) 0.021(2) -0.0018(16) 0.0063(17) -0.0041(15)
C22 0.026(2) 0.0132(19) 0.033(3) -0.0029(17) 0.0073(19) -0.0015(17)
C23 0.022(2) 0.0153(19) 0.027(2) -0.0029(16) 0.0066(18) -0.0007(16)
C24 0.033(2) 0.019(2) 0.040(3) 0.0007(18) 0.012(2) 0.0022(19)
C25 0.030(2) 0.017(2) 0.057(3) 0.0038(18) 0.020(2) -0.003(2)
C26 0.038(3) 0.030(2) 0.053(3) 0.001(2) 0.027(2) -0.008(2)
C27 0.033(2) 0.027(2) 0.031(2) -0.0021(19) 0.017(2) -0.0028(19)
C28 0.024(2) 0.0156(18) 0.030(2) -0.0036(16) 0.0101(18) -0.0024(17)
C29 0.0222(19) 0.0147(18) 0.022(2) -0.0061(16) 0.0087(16) -0.0017(17)
C30 0.019(2) 0.0180(19) 0.021(2) -0.0012(16) 0.0007(17) -0.0048(16)
C31 0.024(2) 0.019(2) 0.033(2) 0.0019(17) 0.0073(19) -0.0040(17)
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
971 999 -782 0.0763
773 978 999 0.1167
312 -999 827 0.0905
855 394 -999 0.0682
-173 -999 969 0.0663
-999 -32 241 0.1038
-971 -999 483 0.0923
-382 999 -893 0.1031
0 4 5 0.1502
-550 -198 999 0.0853
173 133 -999 0.0849
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
C11 N1 C18 . . 111.1(3) ?
C11 N1 C10 . . 123.1(3) ?
C18 N1 C10 . . 125.4(3) ?
C29 N2 C22 . . 111.5(3) ?
C29 N2 C21 . . 125.6(3) ?
C22 N2 C21 . . 122.0(3) ?
C2 C1 C6 . . 121.3(3) ?
C2 C1 C7 . . 119.3(3) ?
C6 C1 C7 . . 119.5(3) ?
C3 C2 C1 . . 118.9(3) ?
C3 C2 C8 . . 121.5(3) ?
C1 C2 C8 . . 119.6(4) ?
C2 C3 C4 . . 120.8(3) ?
C2 C3 C10 . . 119.9(3) ?
C4 C3 C10 . . 119.3(3) ?
C5 C4 C3 . . 119.1(3) ?
C5 C4 C19 . . 120.6(3) ?
C3 C4 C19 . . 120.3(3) ?
C6 C5 C4 . . 120.6(3) ?
C6 C5 C21 . . 119.1(3) ?
C4 C5 C21 . . 120.1(3) ?
C5 C6 C1 . . 119.2(3) ?
C5 C6 C30 . . 120.8(3) ?
C1 C6 C30 . . 120.0(3) ?
C1 C7 Br1 . . 113.3(3) ?
C1 C7 H7A . . 108.9 ?
Br1 C7 H7A . . 108.9 ?
C1 C7 H7B . . 108.9 ?
Br1 C7 H7B . . 108.9 ?
H7A C7 H7B . . 107.7 ?
C2 C8 C9 . . 112.8(3) ?
C2 C8 H8A . . 109.0 ?
C9 C8 H8A . . 109.0 ?
C2 C8 H8B . . 109.0 ?
C9 C8 H8B . . 109.0 ?
H8A C8 H8B . . 107.8 ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C8 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
N1 C10 C3 . . 115.7(3) ?
N1 C10 H10A . . 108.3 ?
C3 C10 H10A . . 108.3 ?
N1 C10 H10B . . 108.3 ?
C3 C10 H10B . . 108.3 ?
H10A C10 H10B . . 107.4 ?
O1 C11 N1 . . 124.3(4) ?
O1 C11 C12 . . 129.0(3) ?
N1 C11 C12 . . 106.7(3) ?
C17 C12 C13 . . 122.4(4) ?
C17 C12 C11 . . 108.4(3) ?
C13 C12 C11 . . 129.2(4) ?
C14 C13 C12 . . 116.2(4) ?
C14 C13 H13 . . 121.9 ?
C12 C13 H13 . . 121.9 ?
C13 C14 C15 . . 122.2(4) ?
C13 C14 H14 . . 118.9 ?
C15 C14 H14 . . 118.9 ?
C14 C15 C16 . . 120.6(4) ?
C14 C15 H15 . . 119.7 ?
C16 C15 H15 . . 119.7 ?
C17 C16 C15 . . 117.4(4) ?
C17 C16 H16 . . 121.3 ?
C15 C16 H16 . . 121.3 ?
C16 C17 C12 . . 121.2(4) ?
C16 C17 C18 . . 131.3(4) ?
C12 C17 C18 . . 107.5(3) ?
O2 C18 N1 . . 125.4(4) ?
O2 C18 C17 . . 128.3(4) ?
N1 C18 C17 . . 106.3(3) ?
C4 C19 C20 . . 112.6(3) ?
C4 C19 H19A . . 109.1 ?
C20 C19 H19A . . 109.1 ?
C4 C19 H19B . . 109.1 ?
C20 C19 H19B . . 109.1 ?
H19A C19 H19B . . 107.8 ?
C19 C20 H20A . . 109.5 ?
C19 C20 H20B . . 109.5 ?
H20A C20 H20B . . 109.5 ?
C19 C20 H20C . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
N2 C21 C5 . . 116.5(3) ?
N2 C21 H21A . . 108.2 ?
C5 C21 H21A . . 108.2 ?
N2 C21 H21B . . 108.2 ?
C5 C21 H21B . . 108.2 ?
H21A C21 H21B . . 107.3 ?
O3 C22 N2 . . 125.0(4) ?
O3 C22 C23 . . 129.5(4) ?
N2 C22 C23 . . 105.5(4) ?
C28 C23 C24 . . 121.3(4) ?
C28 C23 C22 . . 108.7(3) ?
C24 C23 C22 . . 130.0(4) ?
C23 C24 C25 . . 116.6(4) ?
C23 C24 H24 . . 121.7 ?
C25 C24 H24 . . 121.7 ?
C26 C25 C24 . . 121.6(4) ?
C26 C25 H25 . . 119.2 ?
C24 C25 H25 . . 119.2 ?
C25 C26 C27 . . 121.3(4) ?
C25 C26 H26 . . 119.3 ?
C27 C26 H26 . . 119.3 ?
C28 C27 C26 . . 117.0(4) ?
C28 C27 H27 . . 121.5 ?
C26 C27 H27 . . 121.5 ?
C23 C28 C27 . . 122.1(4) ?
C23 C28 C29 . . 107.8(4) ?
C27 C28 C29 . . 130.1(4) ?
O4 C29 N2 . . 124.9(4) ?
O4 C29 C28 . . 128.7(4) ?
N2 C29 C28 . . 106.4(3) ?
C6 C30 C31 . . 113.3(3) ?
C6 C30 H30A . . 108.9 ?
C31 C30 H30A . . 108.9 ?
C6 C30 H30B . . 108.9 ?
C31 C30 H30B . . 108.9 ?
H30A C30 H30B . . 107.7 ?
C30 C31 H31A . . 109.5 ?
C30 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C30 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 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
Br1 C7 . 1.970(4) ?
O1 C11 . 1.221(5) ?
O2 C18 . 1.213(5) ?
O3 C22 . 1.204(5) ?
O4 C29 . 1.222(5) ?
N1 C11 . 1.395(5) ?
N1 C18 . 1.399(5) ?
N1 C10 . 1.465(5) ?
N2 C29 . 1.384(5) ?
N2 C22 . 1.413(5) ?
N2 C21 . 1.471(5) ?
C1 C2 . 1.403(5) ?
C1 C6 . 1.407(5) ?
C1 C7 . 1.507(5) ?
C2 C3 . 1.397(5) ?
C2 C8 . 1.515(5) ?
C3 C4 . 1.418(5) ?
C3 C10 . 1.529(5) ?
C4 C5 . 1.409(5) ?
C4 C19 . 1.515(5) ?
C5 C6 . 1.396(5) ?
C5 C21 . 1.530(5) ?
C6 C30 . 1.519(5) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C9 . 1.534(6) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 C12 . 1.478(6) ?
C12 C17 . 1.386(6) ?
C12 C13 . 1.394(5) ?
C13 C14 . 1.381(6) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.399(7) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.401(6) ?
C15 H15 . 0.9500 ?
C16 C17 . 1.380(6) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.497(5) ?
C19 C20 . 1.547(6) ?
C19 H19A . 0.9900 ?
C19 H19B . 0.9900 ?
C20 H20A . 0.9800 ?
C20 H20B . 0.9800 ?
C20 H20C . 0.9800 ?
C21 H21A . 0.9900 ?
C21 H21B . 0.9900 ?
C22 C23 . 1.483(6) ?
C23 C28 . 1.383(6) ?
C23 C24 . 1.388(6) ?
C24 C25 . 1.403(7) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.382(7) ?
C25 H25 . 0.9500 ?
C26 C27 . 1.389(6) ?
C26 H26 . 0.9500 ?
C27 C28 . 1.383(6) ?
C27 H27 . 0.9500 ?
C28 C29 . 1.491(5) ?
C30 C31 . 1.528(6) ?
C30 H30A . 0.9900 ?
C30 H30B . 0.9900 ?
C31 H31A . 0.9800 ?
C31 H31B . 0.9800 ?
C31 H31C . 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
C10 H10A O1 . 0.99 2.49 2.896(5) 104.0 yes
C10 H10A O1 3_556 0.99 2.49 3.173(5) 125.5 yes
C19 H19B O3 . 0.99 2.45 3.373(5) 154.4 yes
C21 H21B O3 . 0.99 2.47 2.897(5) 105.3 yes
C25 H25 O4 2_556 0.95 2.58 3.237(5) 126.8 yes
C30 H30B O4 . 0.99 2.50 3.346(5) 143.7 yes
C31 H31B O2 4_666 0.98 2.59 3.298(5) 129.1 yes
C31 H31C O3 3_666 0.98 2.53 3.334(5) 139.1 yes
C26 H26 Cg1 2_556 0.95 2.84 3.529(5) 130 yes
C31 H31A Cg3 3_656 0.98 2.88 3.394(5) 113 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
C6 C1 C2 C3 . . . . -0.1(6) ?
C7 C1 C2 C3 . . . . -179.5(4) ?
C6 C1 C2 C8 . . . . -179.6(4) ?
C7 C1 C2 C8 . . . . 1.0(6) ?
C1 C2 C3 C4 . . . . 3.0(6) ?
C8 C2 C3 C4 . . . . -177.5(4) ?
C1 C2 C3 C10 . . . . -173.8(4) ?
C8 C2 C3 C10 . . . . 5.8(6) ?
C2 C3 C4 C5 . . . . -2.1(6) ?
C10 C3 C4 C5 . . . . 174.7(4) ?
C2 C3 C4 C19 . . . . 179.9(4) ?
C10 C3 C4 C19 . . . . -3.3(6) ?
C3 C4 C5 C6 . . . . -1.9(6) ?
C19 C4 C5 C6 . . . . 176.1(4) ?
C3 C4 C5 C21 . . . . 173.4(3) ?
C19 C4 C5 C21 . . . . -8.6(6) ?
C4 C5 C6 C1 . . . . 4.7(6) ?
C21 C5 C6 C1 . . . . -170.6(4) ?
C4 C5 C6 C30 . . . . -174.8(4) ?
C21 C5 C6 C30 . . . . 9.8(6) ?
C2 C1 C6 C5 . . . . -3.8(6) ?
C7 C1 C6 C5 . . . . 175.6(4) ?
C2 C1 C6 C30 . . . . 175.8(4) ?
C7 C1 C6 C30 . . . . -4.8(6) ?
C2 C1 C7 Br1 . . . . -87.0(4) ?
C6 C1 C7 Br1 . . . . 93.6(4) ?
C3 C2 C8 C9 . . . . 96.5(5) ?
C1 C2 C8 C9 . . . . -84.0(5) ?
C11 N1 C10 C3 . . . . 135.1(4) ?
C18 N1 C10 C3 . . . . -53.7(5) ?
C2 C3 C10 N1 . . . . -66.4(5) ?
C4 C3 C10 N1 . . . . 116.7(4) ?
C18 N1 C11 O1 . . . . 178.9(3) ?
C10 N1 C11 O1 . . . . -8.8(5) ?
C18 N1 C11 C12 . . . . -0.7(4) ?
C10 N1 C11 C12 . . . . 171.6(3) ?
O1 C11 C12 C17 . . . . -179.8(4) ?
N1 C11 C12 C17 . . . . -0.3(4) ?
O1 C11 C12 C13 . . . . 1.4(7) ?
N1 C11 C12 C13 . . . . -179.1(4) ?
C17 C12 C13 C14 . . . . 0.6(6) ?
C11 C12 C13 C14 . . . . 179.3(4) ?
C12 C13 C14 C15 . . . . -0.7(6) ?
C13 C14 C15 C16 . . . . 0.4(7) ?
C14 C15 C16 C17 . . . . 0.0(6) ?
C15 C16 C17 C12 . . . . -0.1(6) ?
C15 C16 C17 C18 . . . . 179.7(4) ?
C13 C12 C17 C16 . . . . -0.3(6) ?
C11 C12 C17 C16 . . . . -179.1(3) ?
C13 C12 C17 C18 . . . . 179.9(3) ?
C11 C12 C17 C18 . . . . 1.1(4) ?
C11 N1 C18 O2 . . . . -177.6(3) ?
C10 N1 C18 O2 . . . . 10.3(6) ?
C11 N1 C18 C17 . . . . 1.3(4) ?
C10 N1 C18 C17 . . . . -170.8(3) ?
C16 C17 C18 O2 . . . . -2.3(7) ?
C12 C17 C18 O2 . . . . 177.4(4) ?
C16 C17 C18 N1 . . . . 178.8(4) ?
C12 C17 C18 N1 . . . . -1.5(4) ?
C5 C4 C19 C20 . . . . -95.5(4) ?
C3 C4 C19 C20 . . . . 82.5(4) ?
C29 N2 C21 C5 . . . . 68.4(5) ?
C22 N2 C21 C5 . . . . -123.2(4) ?
C6 C5 C21 N2 . . . . -116.0(4) ?
C4 C5 C21 N2 . . . . 68.6(5) ?
C29 N2 C22 O3 . . . . 174.7(4) ?
C21 N2 C22 O3 . . . . 4.8(6) ?
C29 N2 C22 C23 . . . . -4.4(4) ?
C21 N2 C22 C23 . . . . -174.2(3) ?
O3 C22 C23 C28 . . . . -176.0(4) ?
N2 C22 C23 C28 . . . . 2.9(4) ?
O3 C22 C23 C24 . . . . 1.7(7) ?
N2 C22 C23 C24 . . . . -179.3(4) ?
C28 C23 C24 C25 . . . . -0.1(6) ?
C22 C23 C24 C25 . . . . -177.6(4) ?
C23 C24 C25 C26 . . . . 1.3(6) ?
C24 C25 C26 C27 . . . . -1.6(7) ?
C25 C26 C27 C28 . . . . 0.6(7) ?
C24 C23 C28 C27 . . . . -0.9(6) ?
C22 C23 C28 C27 . . . . 177.1(4) ?
C24 C23 C28 C29 . . . . -178.6(4) ?
C22 C23 C28 C29 . . . . -0.6(4) ?
C26 C27 C28 C23 . . . . 0.6(6) ?
C26 C27 C28 C29 . . . . 177.8(4) ?
C22 N2 C29 O4 . . . . -174.3(4) ?
C21 N2 C29 O4 . . . . -4.9(6) ?
C22 N2 C29 C28 . . . . 4.0(4) ?
C21 N2 C29 C28 . . . . 173.5(3) ?
C23 C28 C29 O4 . . . . 176.3(4) ?
C27 C28 C29 O4 . . . . -1.3(7) ?
C23 C28 C29 N2 . . . . -2.0(4) ?
C27 C28 C29 N2 . . . . -179.5(4) ?
C5 C6 C30 C31 . . . . -87.0(5) ?
C1 C6 C30 C31 . . . . 93.4(5) ?
_cod_database_fobs_code 2244191