#------------------------------------------------------------------------------
#$Date: 2019-07-26 07:52:53 +0300 (Fri, 26 Jul 2019) $
#$Revision: 217274 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021730.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_2021730
loop_
_publ_author_name
'Pawledzio, Sylwia'
'Trzybi\'nski, Damian'
'Wo\'zniak, Krzysztof'
_publ_section_title
;
Crystal structure and energetic features of the cocrystal of
carbamazepine with 3,5-dinitrobenzoic acid
;
_journal_coeditor_code YF3179
_journal_issue 8
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229619009896
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac 'C15 H12 N2 O, C7 H4 N2 O6'
_chemical_formula_moiety 'C15 H12 N2 O, C7 H4 N2 O6'
_chemical_formula_sum 'C22 H16 N4 O7'
_chemical_formula_weight 448.39
_chemical_name_common
;
Carbamazepine--3,5-dinitrobenzoic acid (1/1)
;
_chemical_name_systematic
'5H-Dibenzo[b,f]azepine-5-carboxamide--3,5-dinitrobenzoic acid (1/1)'
_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'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_cell_angle_alpha 90
_cell_angle_beta 96.456(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.7545(3)
_cell_length_b 6.47168(18)
_cell_length_c 30.0313(9)
_cell_measurement_reflns_used 13769
_cell_measurement_temperature 294.76(10)
_cell_measurement_theta_max 32.1300
_cell_measurement_theta_min 2.5230
_cell_volume 2076.91(10)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009) and Mercury
(Macrae et al., 2008)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009), PLATON (Spek,
2009) and
CrystalExplorer17 (Turner et al., 2017)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 294.76(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.0013
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova Dual Source diffractometer with an Eos detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0293
_diffrn_reflns_av_unetI/netI 0.0223
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 44
_diffrn_reflns_limit_l_min -42
_diffrn_reflns_number 37711
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 32.346
_diffrn_reflns_theta_min 3.150
_diffrn_source 'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 0.110
_exptl_absorpt_correction_T_max 0.991
_exptl_absorpt_correction_T_min 0.969
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour 'clear yellowish colourless'
_exptl_crystal_density_diffrn 1.434
_exptl_crystal_description ' '
_exptl_crystal_F_000 928
_exptl_crystal_size_max 0.5019
_exptl_crystal_size_mid 0.199
_exptl_crystal_size_min 0.1165
_refine_diff_density_max 0.418
_refine_diff_density_min -0.348
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 310
_refine_ls_number_reflns 7052
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.036
_refine_ls_R_factor_all 0.0502
_refine_ls_R_factor_gt 0.0414
_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^)+(0.0494P)^2^+0.8471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1061
_refine_ls_wR_factor_ref 0.1119
_reflns_number_gt 5960
_reflns_number_total 7052
_reflns_threshold_expression 'I > 2\s(I)'
_iucr_refine_instructions_details
;
TITL 2016_06_01_MT_CBZ_D in P21/c #14
2016_06_01_mt_cbz_d.res
created by SHELXL-2018/3 at 15:46:23 on 08-Jan-2019
REM reset to P21/c #14
CELL 0.71073 10.754486 6.47168 30.031344 90 96.4556 90
ZERR 4 0.000327 0.000183 0.000878 0 0.0027 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 88 64 16 28
DFIX 0.86 0.01 N18 H18a
DFIX 0.86 0.01 N18 H18b
DFIX 0.82 0.01 O33 H33
L.S. 5
PLAN 32
SIZE 0.1165 0.199 0.5019
TEMP 21.61(10)
CONF
BOND $H
LIST 4
BOND $H
fmap 2
acta
OMIT 1 0 2
OMIT -1 0 2
OMIT 1 0 0
OMIT 0 0 4
OMIT 6 0 6
REM
REM
REM
WGHT 0.049400 0.847100
FVAR 4.70360
O17 4 0.104398 0.029237 0.355912 11.00000 0.01333 0.02276 =
0.01603 0.00237 0.00267 0.00063
N1 3 0.288291 0.088935 0.328119 11.00000 0.01208 0.02261 =
0.01322 0.00117 0.00193 0.00145
N18 3 0.285601 -0.040982 0.399969 11.00000 0.01489 0.02549 =
0.01583 0.00506 0.00139 0.00115
C2 1 0.225369 0.123746 0.284009 11.00000 0.01280 0.01922 =
0.01263 0.00023 0.00237 -0.00042
C3 1 0.155473 0.302458 0.275081 11.00000 0.01603 0.01997 =
0.01501 -0.00100 0.00251 0.00124
AFIX 43
H3 2 0.153755 0.403736 0.296973 11.00000 -1.20000
AFIX 0
C4 1 0.088030 0.328833 0.233132 11.00000 0.01558 0.02219 =
0.01670 0.00254 0.00177 0.00192
AFIX 43
H4 2 0.041591 0.448572 0.226778 11.00000 -1.20000
AFIX 0
C5 1 0.090236 0.175643 0.200717 11.00000 0.01772 0.02655 =
0.01350 0.00188 0.00086 -0.00346
AFIX 43
H5 2 0.043938 0.191990 0.172869 11.00000 -1.20000
AFIX 0
C6 1 0.161170 -0.001076 0.209803 11.00000 0.02362 0.02143 =
0.01476 -0.00307 0.00428 -0.00328
AFIX 43
H6 2 0.161717 -0.102545 0.187898 11.00000 -1.20000
AFIX 0
C7 1 0.232376 -0.029882 0.251545 11.00000 0.01904 0.01810 =
0.01545 0.00005 0.00527 -0.00055
C8 1 0.308253 -0.216476 0.259251 11.00000 0.03351 0.01902 =
0.02102 0.00022 0.00875 0.00448
AFIX 43
H8 2 0.278834 -0.333070 0.243298 11.00000 -1.20000
AFIX 0
C9 1 0.415486 -0.240775 0.286569 11.00000 0.03242 0.02488 =
0.02608 0.00641 0.01148 0.01265
AFIX 43
H9 2 0.450827 -0.372070 0.287437 11.00000 -1.20000
AFIX 0
C10 1 0.482549 -0.084544 0.314966 11.00000 0.01896 0.03298 =
0.02145 0.01192 0.00719 0.00865
C11 1 0.613527 -0.095843 0.324515 11.00000 0.01945 0.05316 =
0.02992 0.02152 0.01017 0.01451
AFIX 43
H11 2 0.656127 -0.206915 0.313729 11.00000 -1.20000
AFIX 0
C12 1 0.679866 0.054376 0.349523 11.00000 0.01389 0.06997 =
0.03191 0.02766 0.00238 0.00254
AFIX 43
H12 2 0.766345 0.043295 0.355524 11.00000 -1.20000
AFIX 0
C13 1 0.618598 0.221958 0.365806 11.00000 0.02049 0.05960 =
0.02639 0.01502 -0.00369 -0.01253
AFIX 43
H13 2 0.664077 0.324238 0.382172 11.00000 -1.20000
AFIX 0
C14 1 0.488660 0.236966 0.357609 11.00000 0.01934 0.03758 =
0.02058 0.00592 -0.00080 -0.00569
AFIX 43
H14 2 0.446905 0.349052 0.368370 11.00000 -1.20000
AFIX 0
C15 1 0.422324 0.082189 0.333139 11.00000 0.01296 0.02908 =
0.01660 0.00700 0.00249 0.00148
C16 1 0.221846 0.022713 0.361416 11.00000 0.01481 0.01442 =
0.01383 -0.00100 0.00195 0.00062
O26 4 0.480231 -0.263006 0.500606 11.00000 0.02237 0.06035 =
0.05059 0.01657 0.01705 0.00678
O27 4 0.526656 -0.263060 0.432116 11.00000 0.02159 0.08176 =
0.03712 0.02221 -0.00174 0.00506
O29 4 0.812079 -0.484464 0.614769 11.00000 0.04162 0.02329 =
0.01707 0.00119 0.01143 -0.00243
O30 4 1.005824 -0.439553 0.602511 11.00000 0.03288 0.02501 =
0.01796 0.00097 -0.00088 0.00464
O32 4 1.110811 -0.188698 0.459302 11.00000 0.01675 0.01862 =
0.01758 0.00109 0.00138 0.00046
O33 4 0.955481 -0.074460 0.408938 11.00000 0.01701 0.02429 =
0.01473 0.00457 0.00281 0.00084
N25 3 0.555708 -0.265801 0.472850 11.00000 0.01845 0.04140 =
0.03621 0.01501 0.00650 0.00434
N28 3 0.892806 -0.430743 0.591334 11.00000 0.03259 0.01481 =
0.01352 -0.00063 0.00481 0.00246
C19 1 0.689641 -0.275364 0.489019 11.00000 0.01676 0.02560 =
0.02410 0.00649 0.00458 0.00365
C20 1 0.774669 -0.215666 0.460034 11.00000 0.01875 0.02184 =
0.01777 0.00468 0.00335 0.00309
AFIX 43
H20 2 0.747784 -0.171036 0.431113 11.00000 -1.20000
AFIX 0
C21 1 0.901576 -0.224559 0.475540 11.00000 0.01804 0.01431 =
0.01459 0.00021 0.00375 0.00112
C22 1 0.940293 -0.294441 0.518777 11.00000 0.01982 0.01333 =
0.01487 -0.00146 0.00230 0.00176
AFIX 43
H22 2 1.024961 -0.301556 0.529183 11.00000 -1.20000
AFIX 0
C23 1 0.850851 -0.353036 0.545966 11.00000 0.02549 0.01468 =
0.01326 0.00088 0.00410 0.00294
C24 1 0.723944 -0.344321 0.532301 11.00000 0.02361 0.02047 =
0.02142 0.00400 0.00888 0.00294
AFIX 43
H24 2 0.664876 -0.382617 0.551115 11.00000 -1.20000
AFIX 0
C31 1 0.999733 -0.160109 0.446670 11.00000 0.01765 0.01345 =
0.01365 -0.00096 0.00242 0.00021
H18A 2 0.243020 -0.095218 0.419906 11.00000 0.02248
H18B 2 0.363956 -0.070843 0.401012 11.00000 0.02798
H33 2 1.010874 -0.040720 0.392393 11.00000 0.05867
HKLF 4
REM 2016_06_01_MT_CBZ_D in P21/c #14
REM wR2 = 0.1119, GooF = S = 1.035, Restrained GooF = 1.036 for all data
REM R1 = 0.0414 for 5960 Fo > 4sig(Fo) and 0.0502 for all 7052 data
REM 310 parameters refined using 3 restraints
END
WGHT 0.0494 0.8471
REM Highest difference peak 0.418, deepest hole -0.348, 1-sigma level 0.050
Q1 1 0.1808 0.2053 0.2790 11.00000 0.05 0.42
Q2 1 0.8396 -0.2224 0.4680 11.00000 0.05 0.40
Q3 1 0.2344 0.0368 0.2686 11.00000 0.05 0.38
Q4 1 0.5341 -0.1393 0.4390 11.00000 0.05 0.37
Q5 1 0.9463 -0.1865 0.4610 11.00000 0.05 0.37
Q6 1 0.1995 -0.0081 0.2305 11.00000 0.05 0.36
Q7 1 0.8846 -0.3299 0.5292 11.00000 0.05 0.35
Q8 1 0.5436 -0.0927 0.3223 11.00000 0.05 0.34
Q9 1 0.4563 0.0078 0.3246 11.00000 0.05 0.33
Q10 1 0.9095 -0.2612 0.4976 11.00000 0.05 0.33
Q11 1 0.1169 0.3093 0.2547 11.00000 0.05 0.32
Q12 1 0.1175 0.0871 0.2080 11.00000 0.05 0.32
Q13 1 0.7041 -0.3311 0.5081 11.00000 0.05 0.32
Q14 1 0.0951 0.2362 0.2196 11.00000 0.05 0.32
Q15 1 0.3583 0.0842 0.3306 11.00000 0.05 0.31
Q16 1 0.3538 -0.2032 0.2755 11.00000 0.05 0.31
Q17 1 0.2684 -0.1202 0.2559 11.00000 0.05 0.31
Q18 1 0.4506 0.1365 0.3519 11.00000 0.05 0.30
Q19 1 0.7394 -0.2409 0.4768 11.00000 0.05 0.30
Q20 1 0.7884 -0.3767 0.5361 11.00000 0.05 0.30
Q21 1 0.2598 0.0578 0.3446 11.00000 0.05 0.30
Q22 1 0.5553 0.2283 0.3602 11.00000 0.05 0.29
Q23 1 0.3783 -0.2046 0.2666 11.00000 0.05 0.29
Q24 1 0.2549 0.1129 0.3057 11.00000 0.05 0.28
Q25 1 0.6663 0.1214 0.3660 11.00000 0.05 0.27
Q26 1 0.6296 -0.2802 0.4810 11.00000 0.05 0.27
Q27 1 0.6328 -0.0320 0.3448 11.00000 0.05 0.26
Q28 1 0.8691 -0.3897 0.5668 11.00000 0.05 0.26
Q29 1 0.2548 -0.0200 0.3799 11.00000 0.05 0.24
Q30 1 0.4461 0.1947 0.3365 11.00000 0.05 0.23
Q31 1 0.0738 -0.0112 0.3766 11.00000 0.05 0.22
Q32 1 1.0607 -0.1869 0.4511 11.00000 0.05 0.22
REM The information below was added by Olex2.
REM
REM R1 = 0.0414 for 5960 Fo > 4sig(Fo) and 0.0502 for all 39518 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.42, deepest hole -0.35
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0502
REM R1_gt = 0.0414
REM wR_ref = 0.1119
REM GOOF = 1.035
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 39518
REM Reflections_gt = 5960
REM Parameters = n/a
REM Hole = -0.35
REM Peak = 0.42
REM Flack = n/a
;
_cod_data_source_file yf3179sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 2076.92(11)
_cod_database_code 2021730
_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 0.947
_shelx_estimated_absorpt_t_max 0.987
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
O O17 0.10440(6) 0.02924(12) 0.35591(2) 0.01730(14) Uani d 1
N N1 0.28829(7) 0.08894(14) 0.32812(3) 0.01593(15) Uani d 1
N N18 0.28560(8) -0.04098(15) 0.39997(3) 0.01876(17) Uani d 1
C C2 0.22537(8) 0.12375(15) 0.28401(3) 0.01481(17) Uani d 1
C C3 0.15547(9) 0.30246(16) 0.27508(3) 0.01695(18) Uani d 1
H H3 0.153755 0.403736 0.296973 0.020 Uiso calc 1
C C4 0.08803(9) 0.32883(16) 0.23313(3) 0.01816(18) Uani d 1
H H4 0.041591 0.448572 0.226778 0.022 Uiso calc 1
C C5 0.09024(9) 0.17564(17) 0.20072(3) 0.01933(19) Uani d 1
H H5 0.043938 0.191990 0.172869 0.023 Uiso calc 1
C C6 0.16117(10) -0.00108(16) 0.20980(3) 0.01977(19) Uani d 1
H H6 0.161717 -0.102545 0.187898 0.024 Uiso calc 1
C C7 0.23238(9) -0.02988(16) 0.25154(3) 0.01728(18) Uani d 1
C C8 0.30825(11) -0.21648(17) 0.25925(4) 0.0241(2) Uani d 1
H H8 0.278834 -0.333070 0.243298 0.029 Uiso calc 1
C C9 0.41549(12) -0.24077(19) 0.28657(4) 0.0272(2) Uani d 1
H H9 0.450827 -0.372070 0.287437 0.033 Uiso calc 1
C C10 0.48255(10) -0.08454(19) 0.31497(4) 0.0241(2) Uani d 1
C C11 0.61353(11) -0.0958(2) 0.32451(4) 0.0336(3) Uani d 1
H H11 0.656127 -0.206915 0.313729 0.040 Uiso calc 1
C C12 0.67987(11) 0.0544(3) 0.34952(4) 0.0386(4) Uani d 1
H H12 0.766345 0.043295 0.355524 0.046 Uiso calc 1
C C13 0.61860(11) 0.2220(3) 0.36581(4) 0.0360(3) Uani d 1
H H13 0.664077 0.324238 0.382172 0.043 Uiso calc 1
C C14 0.48866(10) 0.2370(2) 0.35761(4) 0.0261(2) Uani d 1
H H14 0.446905 0.349052 0.368370 0.031 Uiso calc 1
C C15 0.42232(9) 0.08219(17) 0.33314(3) 0.01948(19) Uani d 1
C C16 0.22185(9) 0.02271(15) 0.36142(3) 0.01433(16) Uani d 1
O O26 0.48023(9) -0.26301(19) 0.50061(4) 0.0435(3) Uani d 1
O O27 0.52666(9) -0.2631(2) 0.43212(3) 0.0472(3) Uani d 1
O O29 0.81208(9) -0.48446(13) 0.61477(3) 0.02671(18) Uani d 1
O O30 1.00582(8) -0.43955(13) 0.60251(3) 0.02557(17) Uani d 1
O O32 1.11081(7) -0.18870(11) 0.45930(2) 0.01769(14) Uani d 1
O O33 0.95548(7) -0.07446(12) 0.40894(2) 0.01860(14) Uani d 1
N N25 0.55571(9) -0.26580(19) 0.47285(4) 0.0318(2) Uani d 1
N N28 0.89281(9) -0.43074(13) 0.59133(3) 0.02014(17) Uani d 1
C C19 0.68964(10) -0.27536(18) 0.48902(4) 0.0220(2) Uani d 1
C C20 0.77467(10) -0.21567(16) 0.46003(3) 0.01936(19) Uani d 1
H H20 0.747784 -0.171036 0.431113 0.023 Uiso calc 1
C C21 0.90158(9) -0.22456(15) 0.47554(3) 0.01550(17) Uani d 1
C C22 0.94029(9) -0.29444(14) 0.51878(3) 0.01598(17) Uani d 1
H H22 1.024961 -0.301556 0.529183 0.019 Uiso calc 1
C C23 0.85085(10) -0.35304(15) 0.54597(3) 0.01766(18) Uani d 1
C C24 0.72394(10) -0.34432(17) 0.53230(3) 0.0214(2) Uani d 1
H H24 0.664876 -0.382617 0.551115 0.026 Uiso calc 1
C C31 0.99973(9) -0.16011(14) 0.44667(3) 0.01486(16) Uani d 1
H H18A 0.2430(12) -0.095(2) 0.4199(4) 0.022(3) Uiso d 1
H H18B 0.3640(9) -0.071(2) 0.4010(5) 0.028(4) Uiso d 1
H H33 1.0109(15) -0.041(3) 0.3924(6) 0.059(6) Uiso d 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
O17 0.0133(3) 0.0228(3) 0.0160(3) 0.0006(3) 0.0027(2) 0.0024(3)
N1 0.0121(3) 0.0226(4) 0.0132(3) 0.0014(3) 0.0019(3) 0.0012(3)
N18 0.0149(4) 0.0255(4) 0.0158(4) 0.0011(3) 0.0014(3) 0.0051(3)
C2 0.0128(4) 0.0192(4) 0.0126(4) -0.0004(3) 0.0024(3) 0.0002(3)
C3 0.0160(4) 0.0200(4) 0.0150(4) 0.0012(3) 0.0025(3) -0.0010(3)
C4 0.0156(4) 0.0222(5) 0.0167(4) 0.0019(3) 0.0018(3) 0.0025(3)
C5 0.0177(4) 0.0265(5) 0.0135(4) -0.0035(4) 0.0009(3) 0.0019(3)
C6 0.0236(5) 0.0214(5) 0.0148(4) -0.0033(4) 0.0043(3) -0.0031(3)
C7 0.0190(4) 0.0181(4) 0.0155(4) -0.0005(3) 0.0053(3) 0.0001(3)
C8 0.0335(6) 0.0190(5) 0.0210(5) 0.0045(4) 0.0087(4) 0.0002(4)
C9 0.0324(6) 0.0249(5) 0.0261(5) 0.0126(4) 0.0115(4) 0.0064(4)
C10 0.0190(5) 0.0330(6) 0.0215(5) 0.0086(4) 0.0072(4) 0.0119(4)
C11 0.0195(5) 0.0532(8) 0.0299(6) 0.0145(5) 0.0102(4) 0.0215(5)
C12 0.0139(5) 0.0700(10) 0.0319(6) 0.0025(5) 0.0024(4) 0.0277(6)
C13 0.0205(5) 0.0596(9) 0.0264(6) -0.0125(5) -0.0037(4) 0.0150(6)
C14 0.0193(5) 0.0376(6) 0.0206(5) -0.0057(4) -0.0008(4) 0.0059(4)
C15 0.0130(4) 0.0291(5) 0.0166(4) 0.0015(4) 0.0025(3) 0.0070(4)
C16 0.0148(4) 0.0144(4) 0.0138(4) 0.0006(3) 0.0020(3) -0.0010(3)
O26 0.0224(4) 0.0604(7) 0.0506(6) 0.0068(4) 0.0171(4) 0.0166(5)
O27 0.0216(4) 0.0818(9) 0.0371(5) 0.0051(5) -0.0017(4) 0.0222(5)
O29 0.0416(5) 0.0233(4) 0.0171(3) -0.0024(3) 0.0114(3) 0.0012(3)
O30 0.0329(4) 0.0250(4) 0.0180(3) 0.0046(3) -0.0009(3) 0.0010(3)
O32 0.0167(3) 0.0186(3) 0.0176(3) 0.0005(3) 0.0014(2) 0.0011(2)
O33 0.0170(3) 0.0243(4) 0.0147(3) 0.0008(3) 0.0028(2) 0.0046(3)
N25 0.0184(4) 0.0414(6) 0.0362(5) 0.0043(4) 0.0065(4) 0.0150(5)
N28 0.0326(5) 0.0148(4) 0.0135(4) 0.0025(3) 0.0048(3) -0.0006(3)
C19 0.0168(4) 0.0256(5) 0.0241(5) 0.0036(4) 0.0046(4) 0.0065(4)
C20 0.0188(4) 0.0218(5) 0.0178(4) 0.0031(4) 0.0034(3) 0.0047(3)
C21 0.0180(4) 0.0143(4) 0.0146(4) 0.0011(3) 0.0038(3) 0.0002(3)
C22 0.0198(4) 0.0133(4) 0.0149(4) 0.0018(3) 0.0023(3) -0.0015(3)
C23 0.0255(5) 0.0147(4) 0.0133(4) 0.0029(4) 0.0041(3) 0.0009(3)
C24 0.0236(5) 0.0205(5) 0.0214(5) 0.0029(4) 0.0089(4) 0.0040(4)
C31 0.0176(4) 0.0134(4) 0.0136(4) 0.0002(3) 0.0024(3) -0.0010(3)
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
11 -4 20 0.0735
-9 5 -21 0.1138
11 -5 16 0.0699
-15 2 10 0.1808
-15 1 13 0.1920
14 -3 -3 0.1723
-5 7 -19 0.1130
-1 8 -24 0.1262
-1 9 -12 0.1054
-15 1 15 0.1969
8 -8 3 0.0555
1 9 -3 0.0919
3 9 7 0.0968
-14 3 16 0.1929
2 -9 -11 0.0171
1 -8 -19 0.0322
5 6 26 0.0840
-14 -3 -4 0.1368
0 -6 -30 0.0624
0 -2 -41 0.1058
-10 -1 -27 0.0712
1 -9 10 0.0596
6 -8 8 0.0425
1 8 -17 0.1197
1 -9 -2 0.0151
-3 -8 -14 0.0148
9 7 7 0.1449
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C15 N1 C2 117.77(7)
C16 N1 C2 119.67(8)
C16 N1 C15 121.18(8)
C16 N18 H18A 117.5(9)
C16 N18 H18B 120.2(10)
H18A N18 H18B 118.3(14)
C3 C2 N1 119.83(8)
C3 C2 C7 121.81(9)
C7 C2 N1 118.31(9)
C2 C3 H3 120.2
C2 C3 C4 119.51(9)
C4 C3 H3 120.2
C3 C4 H4 120.1
C5 C4 C3 119.85(9)
C5 C4 H4 120.1
C4 C5 H5 119.9
C6 C5 C4 120.19(9)
C6 C5 H5 119.9
C5 C6 H6 119.4
C5 C6 C7 121.20(9)
C7 C6 H6 119.4
C2 C7 C6 117.39(9)
C2 C7 C8 123.32(9)
C6 C7 C8 119.29(9)
C7 C8 H8 115.9
C9 C8 C7 128.13(11)
C9 C8 H8 115.9
C8 C9 H9 116.3
C8 C9 C10 127.42(10)
C10 C9 H9 116.3
C11 C10 C9 120.03(11)
C15 C10 C9 122.79(10)
C15 C10 C11 117.18(12)
C10 C11 H11 119.3
C12 C11 C10 121.30(13)
C12 C11 H11 119.3
C11 C12 H12 119.8
C11 C12 C13 120.45(11)
C13 C12 H12 119.8
C12 C13 H13 120.0
C12 C13 C14 119.91(13)
C14 C13 H13 120.0
C13 C14 H14 120.4
C15 C14 C13 119.16(12)
C15 C14 H14 120.4
C10 C15 N1 119.10(10)
C14 C15 N1 118.93(10)
C14 C15 C10 121.91(10)
O17 C16 N1 119.72(8)
O17 C16 N18 122.17(9)
N18 C16 N1 118.07(8)
C31 O33 H33 114.1(14)
O26 N25 O27 124.24(11)
O26 N25 C19 118.36(11)
O27 N25 C19 117.40(10)
O29 N28 C23 117.62(9)
O30 N28 O29 124.99(9)
O30 N28 C23 117.39(9)
C20 C19 N25 118.18(9)
C24 C19 N25 118.16(10)
C24 C19 C20 123.66(10)
C19 C20 H20 121.0
C19 C20 C21 117.99(9)
C21 C20 H20 121.0
C20 C21 C22 120.25(9)
C20 C21 C31 121.50(8)
C22 C21 C31 118.24(9)
C21 C22 H22 120.5
C23 C22 C21 118.97(9)
C23 C22 H22 120.5
C22 C23 N28 118.56(9)
C24 C23 N28 118.54(9)
C24 C23 C22 122.89(9)
C19 C24 H24 121.9
C23 C24 C19 116.24(9)
C23 C24 H24 121.9
O32 C31 O33 125.55(9)
O32 C31 C21 120.28(8)
O33 C31 C21 114.17(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O17 C16 1.2560(11)
N1 C2 1.4359(12)
N1 C15 1.4330(12)
N1 C16 1.3619(12)
N18 C16 1.3424(12)
N18 H18A 0.868(8)
N18 H18B 0.862(9)
C2 C3 1.3890(14)
C2 C7 1.4004(13)
C3 H3 0.9300
C3 C4 1.3917(13)
C4 H4 0.9300
C4 C5 1.3915(15)
C5 H5 0.9300
C5 C6 1.3848(15)
C6 H6 0.9300
C6 C7 1.4060(14)
C7 C8 1.4612(15)
C8 H8 0.9300
C8 C9 1.3472(17)
C9 H9 0.9300
C9 C10 1.4599(18)
C10 C11 1.4074(15)
C10 C15 1.4004(16)
C11 H11 0.9300
C11 C12 1.378(2)
C12 H12 0.9300
C12 C13 1.386(2)
C13 H13 0.9300
C13 C14 1.3948(16)
C14 H14 0.9300
C14 C15 1.3908(16)
O26 N25 1.2273(14)
O27 N25 1.2282(15)
O29 N28 1.2277(12)
O30 N28 1.2253(12)
O32 C31 1.2261(12)
O33 C31 1.3025(11)
O33 H33 0.846(9)
N25 C19 1.4687(14)
N28 C23 1.4747(12)
C19 C20 1.3864(14)
C19 C24 1.3845(14)
C20 H20 0.9300
C20 C21 1.3928(14)
C21 C22 1.3937(13)
C21 C31 1.4986(13)
C22 H22 0.9300
C22 C23 1.3829(14)
C23 C24 1.3814(15)
C24 H24 0.9300
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
N1 C2 C3 C4 -175.76(9)
N1 C2 C7 C6 174.50(9)
N1 C2 C7 C8 -4.88(14)
C2 N1 C15 C10 -69.20(12)
C2 N1 C15 C14 113.56(11)
C2 N1 C16 O17 -13.22(14)
C2 N1 C16 N18 169.14(9)
C2 C3 C4 C5 0.58(15)
C2 C7 C8 C9 -29.72(17)
C3 C2 C7 C6 -2.75(14)
C3 C2 C7 C8 177.87(10)
C3 C4 C5 C6 -1.21(15)
C4 C5 C6 C7 -0.17(15)
C5 C6 C7 C2 2.10(15)
C5 C6 C7 C8 -178.49(10)
C6 C7 C8 C9 150.91(12)
C7 C2 C3 C4 1.45(15)
C7 C8 C9 C10 -0.5(2)
C8 C9 C10 C11 -149.86(12)
C8 C9 C10 C15 29.08(18)
C9 C10 C11 C12 177.04(11)
C9 C10 C15 N1 7.26(15)
C9 C10 C15 C14 -175.58(10)
C10 C11 C12 C13 -0.30(18)
C11 C10 C15 N1 -173.77(9)
C11 C10 C15 C14 3.39(15)
C11 C12 C13 C14 1.25(18)
C12 C13 C14 C15 0.13(17)
C13 C14 C15 N1 174.64(9)
C13 C14 C15 C10 -2.52(16)
C15 N1 C2 C3 -115.47(10)
C15 N1 C2 C7 67.22(12)
C15 N1 C16 O17 -179.52(9)
C15 N1 C16 N18 2.83(14)
C15 C10 C11 C12 -1.97(16)
C16 N1 C2 C3 77.77(12)
C16 N1 C2 C7 -99.54(11)
C16 N1 C15 C10 97.36(11)
C16 N1 C15 C14 -79.89(13)
O26 N25 C19 C20 -160.53(12)
O26 N25 C19 C24 19.74(18)
O27 N25 C19 C20 20.14(18)
O27 N25 C19 C24 -159.60(12)
O29 N28 C23 C22 -179.10(9)
O29 N28 C23 C24 0.13(14)
O30 N28 C23 C22 -0.14(13)
O30 N28 C23 C24 179.09(9)
N25 C19 C20 C21 179.86(10)
N25 C19 C24 C23 179.31(10)
N28 C23 C24 C19 -178.36(9)
C19 C20 C21 C22 0.86(15)
C19 C20 C21 C31 -179.13(10)
C20 C19 C24 C23 -0.41(17)
C20 C21 C22 C23 -0.47(14)
C20 C21 C31 O32 -172.63(9)
C20 C21 C31 O33 7.65(13)
C21 C22 C23 N28 178.78(8)
C21 C22 C23 C24 -0.42(15)
C22 C21 C31 O32 7.38(14)
C22 C21 C31 O33 -172.34(9)
C22 C23 C24 C19 0.84(16)
C24 C19 C20 C21 -0.42(17)
C31 C21 C22 C23 179.52(9)
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
0 0 -3 5.10513 5.07869
0 0 3 -2.8014 4.24232
0 0 -4 13058.7 222.643
0 0 4 12744.3 198.178
0 0 -5 36.197 21.5675
0 0 5 32.1067 19.5181
0 0 -5 41.838 17.2687
0 0 -5 50.1969 23.3837
0 0 -6 12483.2 265.568
0 0 6 12383.7 241.551
0 0 -6 12471.9 269.192
0 0 -6 12825.4 205.175
0 0 -7 105.97 30.2884
0 0 -7 125.601 40.8433
0 0 7 163.258 39.7566
0 0 -7 171.351 44.8116
0 0 8 47873.4 541.734
0 0 -8 46208.1 597.319
0 0 -8 45604.1 589.492
0 0 -8 47550.7 459.132
0 0 -9 122.248 49.6036
0 0 -9 79.5391 48.5384
0 0 -9 34.8284 26.1087
0 0 9 31.0179 45.0097
0 0 -10 1030.32 76.855
0 0 -10 918.602 96.1988
0 0 10 984.227 86.2307
0 0 -10 996.233 101.04
0 0 10 893.633 99.0577
0 0 -11 94.6818 32.2059
0 0 11 94.4507 46.2444
0 0 -11 105.287 45.1292
0 0 11 46.6764 31.2787
0 0 12 9824.04 304.479
0 0 -12 9464.54 332.97
0 0 12 9378.8 343.671
0 0 -12 9486.48 258.904
0 0 -13 201.184 58.6786
0 0 13 258.678 70.1274
0 0 13 539.475 93.8638
0 0 -13 183.68 70.6473
0 0 -14 24521.6 444.872
0 0 14 25056 521.052
0 0 -14 24204.4 578.149
0 0 14 24104.4 593.686
0 0 -15 655.182 125.745
0 0 15 384.371 85.9629
0 0 -15 215.572 83.7169
0 0 15 814.86 136.645
0 0 16 105718 1149.12
0 0 -16 104552 1300.17
0 0 -16 105793 991.242
0 0 16 102871 1310.55
0 0 17 3061.79 256.312
0 0 17 2467.04 208.829
0 0 -17 768.809 96.7915
0 0 -17 1307.62 175.807
0 0 -18 3136.97 185.044
0 0 18 3567.18 227.818
0 0 -18 3671.71 263.272
0 0 18 3660.5 264.782
0 0 19 175.633 75.1198
0 0 -19 33.0625 41.4063
0 0 -19 277.424 99.4656
0 0 19 259.416 88.7105
0 0 20 16047 508.499
0 0 -20 16094.9 439.678
0 0 20 15673.3 581.938
0 0 -20 16079 582.306
0 0 21 623.487 121.117
0 0 -21 621.398 145.383
0 0 21 771.043 153.034
0 0 -21 295.611 85.7129
0 0 -22 24162.1 570.527
0 0 22 24927.9 668.75
0 0 22 23664.8 751.171
0 0 -22 25717 774.837
0 0 23 1201.52 189.306
0 0 -23 706.854 153.015
0 0 -23 554.635 99.8918
0 0 23 904.848 150.119
0 0 24 452.329 118.145
0 0 -24 417.128 89.6605
0 0 24 595.311 124.802
0 0 -24 697.287 137.537
0 0 -25 477.648 130.768
0 0 25 272.171 109.886
0 0 25 331.073 111.106
0 0 -25 209.657 76.6713
0 0 26 29129.6 917.17
0 0 -26 30523.6 939.703
0 0 -26 30210.5 702.543
0 0 26 28728.8 796.527
0 0 -27 1095.79 217.03
0 0 27 1523.3 234.396
0 0 27 1205.26 184.647
0 0 -27 831.079 140.342
0 0 -28 22567.6 638.946
0 0 28 23978.7 761.159
0 0 -28 23459.6 862.942
0 0 28 22512 845.815
0 0 -29 560.115 120.724
0 0 -29 632.752 166.206
0 0 29 991.39 175.811
0 0 29 1191.17 208.445
0 0 -30 742.771 181.099
0 0 30 707.264 143.008
0 0 30 500.58 137.643
0 0 31 144.581 104.159
0 0 31 -15.9061 53.8858
0 0 -31 158.585 138.765
0 0 32 3904.88 338.926
0 0 -32 3511.16 370.43
0 0 32 3650.98 374.7
0 0 -33 28.5405 76.1644
0 0 33 231.076 111.799
0 0 33 61.7617 95.006
0 0 34 800.578 166.395
0 0 34 1054.45 211.269
0 0 -34 973.517 217.451
0 0 35 -77.246 85.4599
0 0 -35 78.5436 89.5998
0 0 35 73.2744 79.6126
0 0 36 -24.0008 67.8548
0 0 -36 -39.2717 104.075
0 0 36 -125.683 98.0426
0 0 -37 122.833 111.362
0 0 37 -48.1871 88.6448
0 0 37 163.121 104.497
0 0 38 7461.63 530.732
0 0 38 6836.74 569.098
0 0 -38 6723.05 585.539
0 0 -39 155.913 93.4975
0 0 39 74.2874 88.2762
0 0 39 184.3 133.302
0 0 40 312.407 131.353
0 0 40 414.741 164.111
0 0 -40 148.679 87.1763
0 0 -41 301.86 166.602
0 0 41 213.093 153.438
0 0 41 -15.8622 78.7751
0 0 42 7184.13 559.982
0 0 42 6957.45 608.751
0 0 -42 7589.02 669.133
0 0 43 283.861 164.237
0 0 43 448.488 170.648
0 0 44 1132.41 275.49
0 1 0 -8.4811 10.9219
0 -1 0 58.6376 19.9201
0 1 0 36.9217 19.425
0 -1 0 -1.0955 12.7545
0 1 1 50801.1 440.602
0 -1 -1 48744.2 395.472
0 1 -1 52206.3 466.276
0 -1 -1 52007.9 479.014
0 1 -1 51215.9 408.153
0 -1 -1 51996.6 455.61
0 -1 1 52331.2 444.211
0 -1 -2 184.396 28.4224
0 -1 2 224.222 31.6426
0 1 2 231.357 35.1296
0 -1 -2 233.602 35.4657
0 -1 -2 218.016 34.6893
0 1 -2 192.401 30.492
0 -1 -3 299786 1170.49
0 1 3 304623 1275.28
0 -1 -3 316939 1428.33
0 1 -3 303543 1195
0 -1 -3 307975 1265.42
0 -1 3 309098 1209.17
0 -1 3 303951 1087.32
0 1 4 115868 539.417
0 -1 4 111896 721.656
0 1 -4 114697 775.407
0 -1 -4 112632 796.501
0 -1 -4 117111 946.128
0 1 4 118983 849.07
0 -1 -4 112822 768.329
0 -1 -5 14049.7 354.155
0 1 5 13921.7 313.315
0 1 -5 13726.7 282.722
0 1 5 13896.2 212.318
0 -1 5 13412.4 269.366
0 -1 -5 13526.1 287.48
0 -1 -5 14103 294.122
0 1 -6 478464 1782.33
0 -1 6 476386 1700.13
0 -1 -6 478499 2244.07
0 1 6 469703 1931.47
0 -1 -6 475833 1778.73
0 1 6 465098 1384.97
0 -1 -6 481780 1831.19
0 1 -7 65461.2 700.446
0 1 7 63930.4 562.972
0 -1 -7 68171.2 886.791
0 -1 -7 67875.2 695.541
0 1 7 65725 772.663
0 -1 7 68708 678.635
0 -1 -7 65746.4 715.862
0 1 -8 8310.46 262.354
0 -1 -8 7710 318.29
0 -1 8 9332.78 275.57
0 -1 -8 9289.81 276.523
0 1 8 8006.05 280.095
0 1 8 7843.67 211.219
0 -1 -8 7245.44 253.288
0 -1 -8 7786.47 166.316
0 -1 9 199681 1278.73
0 1 9 199038 1467.13
0 -1 -9 193401 1370.26
0 -1 -9 200275 832.753
0 1 -9 196083 1335.03
0 1 9 196918 1111.22
0 1 -9 196018 953.863
0 -1 -9 198816 1285.55
0 1 10 4578.28 235.791
0 1 -10 4608.93 145.732
0 -1 -10 4285.32 212.412
0 1 -10 4643.66 218.967
0 1 10 4827.06 189.403
0 -1 10 4534.25 203.59
0 -1 -10 4469.94 123.02
0 -1 -10 4833.8 212.64
0 -1 -11 3439.45 202.068
0 1 -11 3784.53 201.867
0 -1 -11 3642.52 108.326
0 1 11 3899.25 176.223
0 -1 -11 4105.55 208.994
0 -1 11 3781.8 194.272
0 1 11 3863.99 222.964
0 1 -11 4008.77 142.505
0 -1 -12 18054.8 428.247
0 1 12 18338.9 508.943
0 1 -12 18750.5 316.475
0 -1 -12 17950 477.828
0 1 12 18579.7 397.884
0 -1 -12 17456.6 231.749
0 1 -12 18405.9 472.168
0 -1 12 18027.8 442.344
0 -1 -13 103745 1179.48
0 1 -13 102927 1161.26
0 1 -13 108889 785.693
0 1 13 105067 1242.98
0 -1 -13 105557 1061.45
0 1 13 104408 981.421
0 -1 13 103845 1095.36
0 -1 -14 1250.64 126.698
0 -1 14 1421.09 155.328
0 1 14 1183.08 148.837
0 1 -14 931.737 114.235
0 -1 -14 989.589 127.474
0 1 -14 829.105 76.886
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