#------------------------------------------------------------------------------
#$Date: 2024-12-24 05:04:39 +0200 (Tue, 24 Dec 2024) $
#$Revision: 296962 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/35/1573532.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_1573532
loop_
_publ_author_name
'Khamrang, Themmila'
'Kannan, A.'
'Ponraj, C.'
'Hemamalini, Madhukar'
'Antony, G. Jerald Maria'
'Saravanan, Dhandayutham'
_publ_section_title
;
6-Bromo-9,9-diethyl-N,N-diphenylfluoren-2-amine
;
_journal_coeditor_code HB4495
_journal_issue 12
_journal_name_full IUCrData
_journal_paper_doi 10.1107/S2414314624011763
_journal_volume 9
_journal_year 2024
_chemical_formula_iupac 'C29 H26 Br N'
_chemical_formula_moiety 'C29 H26 Br N'
_chemical_formula_sum 'C29 H26 Br N'
_chemical_formula_weight 468.42
_chemical_name_systematic
;
6-Bromo-9,9-diethyl-N,N-diphenylfluoren-2-amine
;
_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 geom
_atom_sites_solution_primary dual
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 105.372(12)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.7044(14)
_cell_length_b 10.5123(17)
_cell_length_c 18.2491(19)
_cell_measurement_reflns_used 9567
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 26.459
_cell_measurement_theta_min 3.577
_cell_volume 2350.0(5)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type 'Agilent Xcalibur, Atlas, Gemini'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0288
_diffrn_reflns_av_unetI/netI 0.0552
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 8476
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 26.372
_diffrn_reflns_theta_min 3.513
_diffrn_source 'fine-focus sealed tube'
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.765
_exptl_absorpt_correction_T_max 0.5778
_exptl_absorpt_correction_T_min 0.5069
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Agilent, 2012)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.324
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 968
_exptl_crystal_size_max 0.369
_exptl_crystal_size_mid 0.319
_exptl_crystal_size_min 0.285
_refine_diff_density_max 0.535
_refine_diff_density_min -0.602
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.021
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 282
_refine_ls_number_reflns 4762
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.021
_refine_ls_R_factor_all 0.0944
_refine_ls_R_factor_gt 0.0479
_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^)+(0.0391P)^2^+1.1250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0964
_refine_ls_wR_factor_ref 0.1168
_reflns_number_gt 2977
_reflns_number_total 4762
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb4495.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1573532
_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 0.562
_shelx_estimated_absorpt_t_max 0.633
_shelx_hkl_file
;
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0 0 15-244.223 561.486 2
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0 0 0 0.00 0.00 0
TITL TP-199 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 12.704430 10.512283 18.249133 90.0000 105.3722 90.0000
ZERR 4.00 0.001405 0.001728 0.001890 0.0000 0.0117 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N Br
UNIT 116.00 104.00 4.00 4.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 80498
_shelx_res_file
;
TITL tp-199_a.res in P2(1)/c
shelx.res
created by SHELXL-2018/3 at 15:31:38 on 06-Nov-2024
CELL 0.71073 12.7044 10.5123 18.2491 90.000 105.372 90.000
ZERR 4.00 0.0014 0.0017 0.0019 0.000 0.012 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H BR N
UNIT 116 104 4 4
MERG 2
MORE -1
SHEL 100 0.8
FMAP 2
PLAN 8
ACTA 52.00
BOND $H
SIZE 0.369 0.319 0.285
HTAB
CONF
LIST 6
HTAB
L.S. 6
WGHT 0.039100 1.125000
FVAR 6.08831
BR1 3 0.954288 0.616013 0.100949 11.00000 0.07124 0.14063 =
0.05597 0.02682 0.03493 -0.00110
N1 4 0.635784 0.348017 0.527735 11.00000 0.05269 0.06387 =
0.03139 -0.00533 0.01666 -0.02121
C6 1 0.691308 0.405516 0.596036 11.00000 0.04257 0.04474 =
0.03198 0.00566 0.01003 -0.00332
C12 1 0.542929 0.270384 0.521275 11.00000 0.04061 0.04891 =
0.03274 -0.00133 0.01212 -0.00459
C5 1 0.640171 0.427807 0.652926 11.00000 0.04329 0.05576 =
0.04022 0.00016 0.01470 -0.00451
AFIX 43
H16 2 0.567720 0.403893 0.646045 11.00000 -1.20000
AFIX 0
C25 1 0.690209 0.477732 0.433208 11.00000 0.04756 0.04783 =
0.03462 -0.00453 0.01551 -0.00434
AFIX 43
H2 2 0.668430 0.550728 0.453992 11.00000 -1.20000
AFIX 0
C1 1 0.798174 0.444755 0.607370 11.00000 0.04353 0.05821 =
0.03768 0.00264 0.01230 -0.00373
AFIX 43
H20 2 0.833360 0.432118 0.569297 11.00000 -1.20000
AFIX 0
C24 1 0.735754 0.485817 0.372819 11.00000 0.04219 0.04281 =
0.03262 -0.00004 0.01143 -0.00320
C16 1 0.766541 0.376900 0.341125 11.00000 0.04955 0.04495 =
0.03377 -0.00385 0.01668 -0.00455
C4 1 0.695768 0.484942 0.719346 11.00000 0.06404 0.05128 =
0.04187 -0.00486 0.02128 0.00187
AFIX 43
H17 2 0.660812 0.498929 0.757410 11.00000 -1.20000
AFIX 0
C22 1 0.813380 0.546622 0.275374 11.00000 0.03751 0.05645 =
0.03100 0.00328 0.00992 -0.00125
C17 1 0.814162 0.414524 0.279479 11.00000 0.04277 0.05488 =
0.03386 -0.00444 0.01529 -0.00549
C23 1 0.760400 0.604640 0.333201 11.00000 0.04852 0.04486 =
0.03554 0.00211 0.01623 -0.00030
C21 1 0.855463 0.607705 0.222576 11.00000 0.04341 0.06692 =
0.03768 0.00829 0.01326 -0.00255
AFIX 43
H6 2 0.856900 0.696032 0.220138 11.00000 -1.20000
AFIX 0
C7 1 0.540289 0.175630 0.573120 11.00000 0.04518 0.05634 =
0.04600 0.01072 0.00692 -0.00947
AFIX 43
H22 2 0.600767 0.161627 0.614011 11.00000 -1.20000
AFIX 0
C13 1 0.677420 0.358917 0.462437 11.00000 0.04849 0.05253 =
0.03316 -0.00245 0.01526 -0.01294
C26 1 0.655115 0.675610 0.293301 11.00000 0.05830 0.06040 =
0.05849 0.01394 0.02541 0.01273
AFIX 23
H30A 2 0.620478 0.704973 0.331615 11.00000 -1.20000
H30B 2 0.674493 0.750156 0.268381 11.00000 -1.20000
AFIX 0
C11 1 0.452933 0.287687 0.461164 11.00000 0.05475 0.05981 =
0.04047 0.00868 0.00840 -0.00013
AFIX 43
H26 2 0.453256 0.350736 0.425475 11.00000 -1.20000
AFIX 0
C3 1 0.802492 0.521818 0.730410 11.00000 0.06385 0.04914 =
0.04683 -0.00974 0.00543 -0.00534
AFIX 43
H18 2 0.840137 0.559872 0.775801 11.00000 -1.20000
AFIX 0
C14 1 0.707112 0.251078 0.430676 11.00000 0.07372 0.04342 =
0.05149 0.00060 0.02904 -0.01352
AFIX 43
H13 2 0.697315 0.171879 0.450604 11.00000 -1.20000
AFIX 0
C2 1 0.852741 0.501768 0.673644 11.00000 0.04469 0.05898 =
0.05206 0.00153 0.00694 -0.00611
AFIX 43
H19 2 0.924772 0.527292 0.680377 11.00000 -1.20000
AFIX 0
C15 1 0.751591 0.258811 0.369162 11.00000 0.07248 0.04047 =
0.05507 -0.00861 0.03060 -0.00569
AFIX 43
H12 2 0.770937 0.185547 0.347291 11.00000 -1.20000
AFIX 0
C28 1 0.835289 0.695981 0.388356 11.00000 0.06731 0.05077 =
0.05227 -0.00341 0.02339 -0.00913
AFIX 23
H28A 2 0.853799 0.765901 0.359389 11.00000 -1.20000
H28B 2 0.795045 0.731182 0.421969 11.00000 -1.20000
AFIX 0
C18 1 0.854160 0.342453 0.229662 11.00000 0.05708 0.06227 =
0.04653 -0.01126 0.02153 -0.00454
AFIX 43
H9 2 0.853886 0.254087 0.232049 11.00000 -1.20000
AFIX 0
C20 1 0.895158 0.534382 0.173738 11.00000 0.04278 0.08676 =
0.03295 0.00867 0.01409 -0.00194
C19 1 0.894709 0.404576 0.176045 11.00000 0.05363 0.09145 =
0.03812 -0.01352 0.02115 -0.00266
AFIX 43
H8 2 0.921608 0.357949 0.141644 11.00000 -1.20000
AFIX 0
C10 1 0.362733 0.212763 0.453407 11.00000 0.04249 0.07846 =
0.05588 -0.00898 0.00012 -0.00020
AFIX 43
H25 2 0.302388 0.225092 0.412174 11.00000 -1.20000
AFIX 0
C8 1 0.449217 0.102579 0.564483 11.00000 0.06393 0.05887 =
0.06398 0.00807 0.02040 -0.01392
AFIX 43
H23 2 0.448149 0.039306 0.599897 11.00000 -1.20000
AFIX 0
C9 1 0.359851 0.120538 0.505002 11.00000 0.04546 0.06961 =
0.07403 -0.01191 0.01530 -0.01592
AFIX 43
H24 2 0.297871 0.070585 0.499736 11.00000 -1.20000
AFIX 0
C27 1 0.573224 0.598601 0.235189 11.00000 0.05031 0.11467 =
0.05842 0.00449 0.01178 0.00686
AFIX 137
H31A 2 0.603564 0.576906 0.193923 11.00000 -1.50000
H31B 2 0.507957 0.647711 0.216245 11.00000 -1.50000
H31C 2 0.556058 0.522199 0.258433 11.00000 -1.50000
AFIX 0
C29 1 0.938544 0.639285 0.435746 11.00000 0.05945 0.09957 =
0.06808 -0.01816 0.00792 -0.00464
AFIX 137
H29A 2 0.974601 0.593977 0.403666 11.00000 -1.50000
H29B 2 0.922103 0.581655 0.471999 11.00000 -1.50000
H29C 2 0.985418 0.705712 0.462089 11.00000 -1.50000
AFIX 0
HKLF 4
REM tp-199_a.res in P2(1)/c
REM wR2 = 0.1168, GooF = S = 1.021, Restrained GooF = 1.021 for all data
REM R1 = 0.0479 for 2977 Fo > 4sig(Fo) and 0.0944 for all 4762 data
REM 282 parameters refined using 0 restraints
END
WGHT 0.0391 1.1251
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 0.535, deepest hole -0.602, 1-sigma level 0.050
Q1 1 0.9406 0.5192 0.0759 11.00000 0.05 0.54
Q2 1 0.7877 0.3904 0.3084 11.00000 0.05 0.22
Q3 1 0.7261 0.5527 0.3466 11.00000 0.05 0.19
Q4 1 1.0292 0.6389 0.3978 11.00000 0.05 0.19
Q5 1 0.6645 0.2608 0.5363 11.00000 0.05 0.19
Q6 1 0.1834 0.1392 0.5126 11.00000 0.05 0.18
Q7 1 0.6758 0.7674 0.4250 11.00000 0.05 0.18
Q8 1 0.7947 0.4644 0.2748 11.00000 0.05 0.17
;
_shelx_res_checksum 42676
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 Br1 0.95429(3) 0.61601(5) 0.10095(2) 0.0858(2) Uani d 1 . .
N N1 0.6358(2) 0.3480(3) 0.52774(13) 0.0483(7) Uani d 1 . .
C C6 0.6913(2) 0.4055(3) 0.59604(15) 0.0397(7) Uani d 1 . .
C C12 0.5429(2) 0.2704(3) 0.52127(15) 0.0403(7) Uani d 1 . .
C C5 0.6402(2) 0.4278(3) 0.65293(16) 0.0457(8) Uani d 1 . .
H H16 0.567720 0.403893 0.646045 0.055 Uiso calc 1 . .
C C25 0.6902(2) 0.4777(3) 0.43321(15) 0.0425(7) Uani d 1 . .
H H2 0.668430 0.550728 0.453992 0.051 Uiso calc 1 . .
C C1 0.7982(2) 0.4448(3) 0.60737(16) 0.0462(8) Uani d 1 . .
H H20 0.833360 0.432118 0.569297 0.055 Uiso calc 1 . .
C C24 0.7358(2) 0.4858(3) 0.37282(15) 0.0389(7) Uani d 1 . .
C C16 0.7665(2) 0.3769(3) 0.34112(15) 0.0417(7) Uani d 1 . .
C C4 0.6958(3) 0.4849(3) 0.71935(17) 0.0510(8) Uani d 1 . .
H H17 0.660812 0.498929 0.757410 0.061 Uiso calc 1 . .
C C22 0.8134(2) 0.5466(3) 0.27537(15) 0.0415(7) Uani d 1 . .
C C17 0.8142(2) 0.4145(3) 0.27948(16) 0.0429(7) Uani d 1 . .
C C23 0.7604(2) 0.6046(3) 0.33320(15) 0.0420(7) Uani d 1 . .
C C21 0.8555(2) 0.6077(3) 0.22258(16) 0.0489(8) Uani d 1 . .
H H6 0.856900 0.696032 0.220138 0.059 Uiso calc 1 . .
C C7 0.5403(2) 0.1756(3) 0.57312(17) 0.0502(8) Uani d 1 . .
H H22 0.600767 0.161627 0.614011 0.060 Uiso calc 1 . .
C C13 0.6774(2) 0.3589(3) 0.46244(16) 0.0439(7) Uani d 1 . .
C C26 0.6551(3) 0.6756(3) 0.29330(19) 0.0572(9) Uani d 1 . .
H H30A 0.620478 0.704973 0.331615 0.069 Uiso calc 1 . .
H H30B 0.674493 0.750156 0.268381 0.069 Uiso calc 1 . .
C C11 0.4529(3) 0.2877(3) 0.46116(17) 0.0525(8) Uani d 1 . .
H H26 0.453256 0.350736 0.425475 0.063 Uiso calc 1 . .
C C3 0.8025(3) 0.5218(3) 0.73041(19) 0.0550(9) Uani d 1 . .
H H18 0.840137 0.559872 0.775801 0.066 Uiso calc 1 . .
C C14 0.7071(3) 0.2511(3) 0.43068(17) 0.0538(9) Uani d 1 . .
H H13 0.697315 0.171879 0.450604 0.065 Uiso calc 1 . .
C C2 0.8527(3) 0.5018(3) 0.67364(18) 0.0530(8) Uani d 1 . .
H H19 0.924772 0.527292 0.680377 0.064 Uiso calc 1 . .
C C15 0.7516(3) 0.2588(3) 0.36916(18) 0.0534(8) Uani d 1 . .
H H12 0.770937 0.185547 0.347291 0.064 Uiso calc 1 . .
C C28 0.8353(3) 0.6960(3) 0.38836(18) 0.0554(9) Uani d 1 . .
H H28A 0.853799 0.765901 0.359389 0.066 Uiso calc 1 . .
H H28B 0.795045 0.731182 0.421969 0.066 Uiso calc 1 . .
C C18 0.8542(3) 0.3425(3) 0.22966(17) 0.0538(9) Uani d 1 . .
H H9 0.853886 0.254087 0.232049 0.065 Uiso calc 1 . .
C C20 0.8952(2) 0.5344(4) 0.17374(16) 0.0534(9) Uani d 1 . .
C C19 0.8947(3) 0.4046(4) 0.17605(17) 0.0594(10) Uani d 1 . .
H H8 0.921608 0.357949 0.141644 0.071 Uiso calc 1 . .
C C10 0.3627(3) 0.2128(4) 0.4534(2) 0.0614(10) Uani d 1 . .
H H25 0.302388 0.225092 0.412174 0.074 Uiso calc 1 . .
C C8 0.4492(3) 0.1026(3) 0.5645(2) 0.0616(9) Uani d 1 . .
H H23 0.448149 0.039306 0.599897 0.074 Uiso calc 1 . .
C C9 0.3599(3) 0.1205(4) 0.5050(2) 0.0631(10) Uani d 1 . .
H H24 0.297871 0.070585 0.499736 0.076 Uiso calc 1 . .
C C27 0.5732(3) 0.5986(4) 0.2352(2) 0.0750(12) Uani d 1 . .
H H31A 0.603564 0.576906 0.193923 0.112 Uiso calc 1 . .
H H31B 0.507957 0.647711 0.216245 0.112 Uiso calc 1 . .
H H31C 0.556058 0.522199 0.258433 0.112 Uiso calc 1 . .
C C29 0.9385(3) 0.6393(4) 0.4357(2) 0.0774(12) Uani d 1 . .
H H29A 0.974601 0.593977 0.403666 0.116 Uiso calc 1 . .
H H29B 0.922103 0.581655 0.471999 0.116 Uiso calc 1 . .
H H29C 0.985418 0.705712 0.462089 0.116 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 0.0712(3) 0.1406(5) 0.0560(2) -0.0011(3) 0.03493(19) 0.0268(2)
N1 0.0527(15) 0.0639(18) 0.0314(13) -0.0212(14) 0.0167(11) -0.0053(12)
C6 0.0426(16) 0.0447(18) 0.0320(14) -0.0033(15) 0.0100(12) 0.0057(14)
C12 0.0406(15) 0.0489(19) 0.0327(15) -0.0046(15) 0.0121(12) -0.0013(14)
C5 0.0433(16) 0.056(2) 0.0402(16) -0.0045(16) 0.0147(13) 0.0002(15)
C25 0.0476(17) 0.0478(19) 0.0346(15) -0.0043(16) 0.0155(13) -0.0045(14)
C1 0.0435(16) 0.058(2) 0.0377(16) -0.0037(16) 0.0123(13) 0.0026(15)
C24 0.0422(16) 0.0428(18) 0.0326(14) -0.0032(15) 0.0114(12) 0.0000(14)
C16 0.0496(17) 0.0450(19) 0.0338(15) -0.0045(16) 0.0167(13) -0.0039(14)
C4 0.064(2) 0.051(2) 0.0419(17) 0.0019(18) 0.0213(15) -0.0049(16)
C22 0.0375(15) 0.056(2) 0.0310(14) -0.0012(16) 0.0099(12) 0.0033(14)
C17 0.0428(16) 0.055(2) 0.0339(15) -0.0055(16) 0.0153(13) -0.0044(15)
C23 0.0485(17) 0.0449(18) 0.0355(15) -0.0003(16) 0.0162(13) 0.0021(14)
C21 0.0434(16) 0.067(2) 0.0377(16) -0.0026(17) 0.0133(13) 0.0083(16)
C7 0.0452(18) 0.056(2) 0.0460(18) -0.0095(17) 0.0069(14) 0.0107(16)
C13 0.0485(17) 0.053(2) 0.0332(15) -0.0129(16) 0.0153(13) -0.0025(14)
C26 0.058(2) 0.060(2) 0.058(2) 0.0127(19) 0.0254(17) 0.0139(18)
C11 0.0548(19) 0.060(2) 0.0405(17) -0.0001(18) 0.0084(15) 0.0087(16)
C3 0.064(2) 0.049(2) 0.0468(18) -0.0053(19) 0.0054(16) -0.0097(16)
C14 0.074(2) 0.0434(19) 0.0515(19) -0.0135(18) 0.0290(17) 0.0006(16)
C2 0.0447(17) 0.059(2) 0.052(2) -0.0061(17) 0.0069(15) 0.0015(17)
C15 0.072(2) 0.0405(19) 0.0551(19) -0.0057(18) 0.0306(17) -0.0086(16)
C28 0.067(2) 0.051(2) 0.0523(19) -0.0091(19) 0.0234(17) -0.0034(17)
C18 0.0571(19) 0.062(2) 0.0465(18) -0.0045(18) 0.0215(15) -0.0113(17)
C20 0.0428(17) 0.087(3) 0.0330(16) -0.002(2) 0.0141(13) 0.0087(18)
C19 0.0536(19) 0.091(3) 0.0381(17) -0.003(2) 0.0211(15) -0.0135(19)
C10 0.0425(18) 0.078(3) 0.056(2) 0.000(2) 0.0001(15) -0.009(2)
C8 0.064(2) 0.059(2) 0.064(2) -0.014(2) 0.0204(18) 0.0081(19)
C9 0.0455(19) 0.070(3) 0.074(2) -0.0159(19) 0.0153(18) -0.012(2)
C27 0.050(2) 0.115(3) 0.058(2) 0.007(2) 0.0118(17) 0.004(2)
C29 0.059(2) 0.100(3) 0.068(2) -0.005(2) 0.0079(19) -0.018(2)
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'
Br Br -0.2901 2.4595 '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'
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
C6 N1 C12 . . 122.5(2) ?
C6 N1 C13 . . 119.9(2) ?
C12 N1 C13 . . 117.5(2) ?
C1 C6 C5 . . 118.4(3) ?
C1 C6 N1 . . 120.5(2) ?
C5 C6 N1 . . 121.1(3) ?
C11 C12 C7 . . 118.5(3) ?
C11 C12 N1 . . 119.4(3) ?
C7 C12 N1 . . 122.1(3) ?
C4 C5 C6 . . 120.3(3) ?
C4 C5 H16 . . 119.9 ?
C6 C5 H16 . . 119.9 ?
C24 C25 C13 . . 118.8(3) ?
C24 C25 H2 . . 120.6 ?
C13 C25 H2 . . 120.6 ?
C2 C1 C6 . . 120.8(3) ?
C2 C1 H20 . . 119.6 ?
C6 C1 H20 . . 119.6 ?
C25 C24 C16 . . 120.6(3) ?
C25 C24 C23 . . 128.0(3) ?
C16 C24 C23 . . 111.4(2) ?
C15 C16 C24 . . 120.6(3) ?
C15 C16 C17 . . 130.9(3) ?
C24 C16 C17 . . 108.5(3) ?
C5 C4 C3 . . 120.8(3) ?
C5 C4 H17 . . 119.6 ?
C3 C4 H17 . . 119.6 ?
C21 C22 C17 . . 120.3(3) ?
C21 C22 C23 . . 128.5(3) ?
C17 C22 C23 . . 111.2(2) ?
C18 C17 C22 . . 120.8(3) ?
C18 C17 C16 . . 131.0(3) ?
C22 C17 C16 . . 108.2(3) ?
C24 C23 C22 . . 100.7(2) ?
C24 C23 C28 . . 112.0(2) ?
C22 C23 C28 . . 113.3(2) ?
C24 C23 C26 . . 111.2(2) ?
C22 C23 C26 . . 110.8(2) ?
C28 C23 C26 . . 108.6(3) ?
C20 C21 C22 . . 118.0(3) ?
C20 C21 H6 . . 121.0 ?
C22 C21 H6 . . 121.0 ?
C8 C7 C12 . . 120.1(3) ?
C8 C7 H22 . . 119.9 ?
C12 C7 H22 . . 119.9 ?
C14 C13 C25 . . 120.6(3) ?
C14 C13 N1 . . 119.3(3) ?
C25 C13 N1 . . 120.0(3) ?
C27 C26 C23 . . 115.1(3) ?
C27 C26 H30A . . 108.5 ?
C23 C26 H30A . . 108.5 ?
C27 C26 H30B . . 108.5 ?
C23 C26 H30B . . 108.5 ?
H30A C26 H30B . . 107.5 ?
C10 C11 C12 . . 120.3(3) ?
C10 C11 H26 . . 119.8 ?
C12 C11 H26 . . 119.8 ?
C2 C3 C4 . . 119.0(3) ?
C2 C3 H18 . . 120.5 ?
C4 C3 H18 . . 120.5 ?
C13 C14 C15 . . 120.7(3) ?
C13 C14 H13 . . 119.6 ?
C15 C14 H13 . . 119.6 ?
C1 C2 C3 . . 120.6(3) ?
C1 C2 H19 . . 119.7 ?
C3 C2 H19 . . 119.7 ?
C16 C15 C14 . . 118.7(3) ?
C16 C15 H12 . . 120.6 ?
C14 C15 H12 . . 120.6 ?
C29 C28 C23 . . 115.4(3) ?
C29 C28 H28A . . 108.4 ?
C23 C28 H28A . . 108.4 ?
C29 C28 H28B . . 108.4 ?
C23 C28 H28B . . 108.4 ?
H28A C28 H28B . . 107.5 ?
C17 C18 C19 . . 118.5(3) ?
C17 C18 H9 . . 120.7 ?
C19 C18 H9 . . 120.7 ?
C19 C20 C21 . . 122.4(3) ?
C19 C20 Br1 . . 118.7(3) ?
C21 C20 Br1 . . 118.9(3) ?
C20 C19 C18 . . 119.9(3) ?
C20 C19 H8 . . 120.0 ?
C18 C19 H8 . . 120.0 ?
C9 C10 C11 . . 121.0(3) ?
C9 C10 H25 . . 119.5 ?
C11 C10 H25 . . 119.5 ?
C9 C8 C7 . . 121.2(3) ?
C9 C8 H23 . . 119.4 ?
C7 C8 H23 . . 119.4 ?
C10 C9 C8 . . 118.8(3) ?
C10 C9 H24 . . 120.6 ?
C8 C9 H24 . . 120.6 ?
C26 C27 H31A . . 109.5 ?
C26 C27 H31B . . 109.5 ?
H31A C27 H31B . . 109.5 ?
C26 C27 H31C . . 109.5 ?
H31A C27 H31C . . 109.5 ?
H31B C27 H31C . . 109.5 ?
C28 C29 H29A . . 109.5 ?
C28 C29 H29B . . 109.5 ?
H29A C29 H29B . . 109.5 ?
C28 C29 H29C . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 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 C20 . 1.896(3) ?
N1 C6 . 1.397(4) ?
N1 C12 . 1.413(4) ?
N1 C13 . 1.431(3) ?
C6 C1 . 1.381(4) ?
C6 C5 . 1.383(4) ?
C12 C11 . 1.371(4) ?
C12 C7 . 1.380(4) ?
C5 C4 . 1.369(4) ?
C5 H16 . 0.9300 ?
C25 C24 . 1.376(4) ?
C25 C13 . 1.385(4) ?
C25 H2 . 0.9300 ?
C1 C2 . 1.363(4) ?
C1 H20 . 0.9300 ?
C24 C16 . 1.385(4) ?
C24 C23 . 1.517(4) ?
C16 C15 . 1.375(4) ?
C16 C17 . 1.466(4) ?
C4 C3 . 1.373(4) ?
C4 H17 . 0.9300 ?
C22 C21 . 1.378(4) ?
C22 C17 . 1.391(4) ?
C22 C23 . 1.522(4) ?
C17 C18 . 1.380(4) ?
C23 C28 . 1.527(4) ?
C23 C26 . 1.536(4) ?
C21 C20 . 1.372(4) ?
C21 H6 . 0.9300 ?
C7 C8 . 1.363(4) ?
C7 H22 . 0.9300 ?
C13 C14 . 1.371(4) ?
C26 C27 . 1.509(5) ?
C26 H30A . 0.9700 ?
C26 H30B . 0.9700 ?
C11 C10 . 1.367(4) ?
C11 H26 . 0.9300 ?
C3 C2 . 1.370(4) ?
C3 H18 . 0.9300 ?
C14 C15 . 1.387(4) ?
C14 H13 . 0.9300 ?
C2 H19 . 0.9300 ?
C15 H12 . 0.9300 ?
C28 C29 . 1.491(5) ?
C28 H28A . 0.9700 ?
C28 H28B . 0.9700 ?
C18 C19 . 1.384(4) ?
C18 H9 . 0.9300 ?
C20 C19 . 1.365(5) ?
C19 H8 . 0.9300 ?
C10 C9 . 1.359(5) ?
C10 H25 . 0.9300 ?
C8 C9 . 1.360(5) ?
C8 H23 . 0.9300 ?
C9 H24 . 0.9300 ?
C27 H31A . 0.9600 ?
C27 H31B . 0.9600 ?
C27 H31C . 0.9600 ?
C29 H29A . 0.9600 ?
C29 H29B . 0.9600 ?
C29 H29C . 0.9600 ?
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
C2 H19 Cg5 3_766 0.93 2.87 3.692(4) 148
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
C12 N1 C6 C1 . . . . 158.9(3) ?
C13 N1 C6 C1 . . . . -16.4(4) ?
C12 N1 C6 C5 . . . . -22.9(4) ?
C13 N1 C6 C5 . . . . 161.8(3) ?
C6 N1 C12 C11 . . . . 133.9(3) ?
C13 N1 C12 C11 . . . . -50.7(4) ?
C6 N1 C12 C7 . . . . -47.1(4) ?
C13 N1 C12 C7 . . . . 128.2(3) ?
C1 C6 C5 C4 . . . . -1.4(5) ?
N1 C6 C5 C4 . . . . -179.6(3) ?
C5 C6 C1 C2 . . . . 1.3(5) ?
N1 C6 C1 C2 . . . . 179.5(3) ?
C13 C25 C24 C16 . . . . 1.0(4) ?
C13 C25 C24 C23 . . . . -178.2(3) ?
C25 C24 C16 C15 . . . . 0.4(4) ?
C23 C24 C16 C15 . . . . 179.7(3) ?
C25 C24 C16 C17 . . . . -178.8(3) ?
C23 C24 C16 C17 . . . . 0.5(3) ?
C6 C5 C4 C3 . . . . 0.5(5) ?
C21 C22 C17 C18 . . . . -1.8(5) ?
C23 C22 C17 C18 . . . . 177.1(3) ?
C21 C22 C17 C16 . . . . 179.0(3) ?
C23 C22 C17 C16 . . . . -2.1(3) ?
C15 C16 C17 C18 . . . . 2.8(6) ?
C24 C16 C17 C18 . . . . -178.1(3) ?
C15 C16 C17 C22 . . . . -178.1(3) ?
C24 C16 C17 C22 . . . . 1.0(3) ?
C25 C24 C23 C22 . . . . 177.6(3) ?
C16 C24 C23 C22 . . . . -1.7(3) ?
C25 C24 C23 C28 . . . . 56.9(4) ?
C16 C24 C23 C28 . . . . -122.4(3) ?
C25 C24 C23 C26 . . . . -64.9(4) ?
C16 C24 C23 C26 . . . . 115.8(3) ?
C21 C22 C23 C24 . . . . -178.9(3) ?
C17 C22 C23 C24 . . . . 2.3(3) ?
C21 C22 C23 C28 . . . . -59.1(4) ?
C17 C22 C23 C28 . . . . 122.1(3) ?
C21 C22 C23 C26 . . . . 63.3(4) ?
C17 C22 C23 C26 . . . . -115.5(3) ?
C17 C22 C21 C20 . . . . 1.5(4) ?
C23 C22 C21 C20 . . . . -177.1(3) ?
C11 C12 C7 C8 . . . . -0.7(5) ?
N1 C12 C7 C8 . . . . -179.7(3) ?
C24 C25 C13 C14 . . . . -1.6(4) ?
C24 C25 C13 N1 . . . . 176.6(3) ?
C6 N1 C13 C14 . . . . 118.5(3) ?
C12 N1 C13 C14 . . . . -57.0(4) ?
C6 N1 C13 C25 . . . . -59.7(4) ?
C12 N1 C13 C25 . . . . 124.8(3) ?
C24 C23 C26 C27 . . . . -57.7(3) ?
C22 C23 C26 C27 . . . . 53.5(4) ?
C28 C23 C26 C27 . . . . 178.6(3) ?
C7 C12 C11 C10 . . . . 0.3(5) ?
N1 C12 C11 C10 . . . . 179.3(3) ?
C5 C4 C3 C2 . . . . 0.6(5) ?
C25 C13 C14 C15 . . . . 0.7(5) ?
N1 C13 C14 C15 . . . . -177.5(3) ?
C6 C1 C2 C3 . . . . -0.2(5) ?
C4 C3 C2 C1 . . . . -0.7(5) ?
C24 C16 C15 C14 . . . . -1.2(5) ?
C17 C16 C15 C14 . . . . 177.7(3) ?
C13 C14 C15 C16 . . . . 0.7(5) ?
C24 C23 C28 C29 . . . . 52.8(4) ?
C22 C23 C28 C29 . . . . -60.3(4) ?
C26 C23 C28 C29 . . . . 176.1(3) ?
C22 C17 C18 C19 . . . . 0.8(5) ?
C16 C17 C18 C19 . . . . 179.8(3) ?
C22 C21 C20 C19 . . . . -0.3(5) ?
C22 C21 C20 Br1 . . . . -179.6(2) ?
C21 C20 C19 C18 . . . . -0.7(5) ?
Br1 C20 C19 C18 . . . . 178.6(2) ?
C17 C18 C19 C20 . . . . 0.5(5) ?
C12 C11 C10 C9 . . . . 0.4(5) ?
C12 C7 C8 C9 . . . . 0.4(5) ?
C11 C10 C9 C8 . . . . -0.8(5) ?
C7 C8 C9 C10 . . . . 0.4(6) ?