#------------------------------------------------------------------------------
#$Date: 2015-06-06 05:32:41 +0300 (Sat, 06 Jun 2015) $
#$Revision: 138438 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/08/2240807.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_2240807
loop_
_publ_author_name
'Honkeldieva, Muhabbat'
'Kunafiev, Rishad'
'Hamidov, Hayrullo I.'
_publ_section_title
;
Redetermined structure of gossypol (P3 polymorph)
;
_journal_coeditor_code HB7412
_journal_issue 7
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first o442
_journal_page_last o443
_journal_paper_doi 10.1107/S205698901500941X
_journal_volume 71
_journal_year 2015
_chemical_formula_iupac 'C30 H30 O8'
_chemical_formula_moiety 'C30 H30 O8'
_chemical_formula_sum 'C30 H30 O8'
_chemical_formula_weight 518.54
_chemical_melting_point 455
_chemical_name_common Gossypol
_chemical_name_systematic
1,1',6,6',7,7'-Hexahydroxy-5,5'-diisopropyl-3,3'-dimethyl[2,2'-binaphthalene]-8,8'-dicarbaldehyde
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha 90
_cell_angle_beta 113.262(2)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 21.2196(4)
_cell_length_b 19.0886(2)
_cell_length_c 15.2564(2)
_cell_measurement_reflns_used 6170
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 75.6102
_cell_measurement_theta_min 3.8459
_cell_volume 5677.29(17)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 298
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur Ruby'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0209
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 13408
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 75.756
_diffrn_reflns_theta_min 3.847
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.726
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.73013
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2009)
;
_exptl_crystal_colour 'light brown'
_exptl_crystal_density_diffrn 1.213
_exptl_crystal_description prism
_exptl_crystal_F_000 2192
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.30
_refine_diff_density_max 0.441
_refine_diff_density_min -0.299
_refine_ls_extinction_coef 0.00026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref 1.113
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 374
_refine_ls_number_reflns 5810
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.113
_refine_ls_R_factor_all 0.0608
_refine_ls_R_factor_gt 0.0474
_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^)+(0.0994P)^2^+0.2158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1516
_refine_ls_wR_factor_ref 0.1612
_reflns_number_gt 4382
_reflns_number_total 5810
_reflns_threshold_expression I>2\s(I)
_iucr_refine_instructions_details
;
TITL exp_1564gp3 in C2/c
CELL 1.54184 21.2196 19.0886 15.2564 90 113.262 90
ZERR 8 0.0004 0.0002 0.0002 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H O
UNIT 240 240 64
EQIV $1 -X,-Y,1-Z
EQIV $2 -X,+Y,0.5-Z
EQIV $3 +X,1-Y,0.5+Z
EQIV $4 +X,-Y,-0.5+Z
EQIV $5 +X,-Y,0.5+Z
L.S. 14
PLAN 20
MPLA 10 C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C21 C22 C23 O1 O2 O3 O4
MPLA 10 C11 C12 C13 C14 C15 C16 C17 C18 C19 C20 C26 C27 C28 O5 O6 O7 O8
HTAB C22 O1
HTAB C27 O5
HTAB O4 O3
HTAB O8 O7
HTAB O5 O3_$1
HTAB O4 O5_$1
HTAB O4 O5_$5
HTAB O1 O6_$2
HTAB C26 O8_$3
HTAB C27 O4_$4
BOND $h
fmap 2
acta
MERG 2
OMIT 3 3 9
OMIT 5 9 3
OMIT -6 2 2
REM E:/xraydata/MUHABBAT/GPP3/exp_1564gp3.hkl
WGHT 0.099400 0.215800
EXTI 0.000263
FVAR 2.42493
C1 1 0.047019 0.153414 0.556583 11.00000 0.04611 0.03650 =
0.04729 0.00528 0.01971 0.00146
C2 1 0.103590 0.183974 0.548005 11.00000 0.05084 0.03378 =
0.04995 0.00575 0.02056 -0.00378
C3 1 0.165531 0.146547 0.576864 11.00000 0.04769 0.04717 =
0.06995 0.01196 0.02398 -0.00266
C4 1 0.168759 0.080453 0.613077 11.00000 0.04685 0.04660 =
0.07579 0.01595 0.02424 0.00642
AFIX 43
H4 2 0.210016 0.056160 0.632155 11.00000 -1.20000
AFIX 0
C5 1 0.118100 -0.023703 0.658173 11.00000 0.05741 0.03791 =
0.05943 0.00967 0.02238 0.00469
C6 1 0.060064 -0.055141 0.656299 11.00000 0.06951 0.03406 =
0.05321 0.00908 0.02751 -0.00071
C7 1 -0.002965 -0.019038 0.628775 11.00000 0.05744 0.04229 =
0.04786 0.00353 0.02455 -0.00977
C8 1 -0.008885 0.051363 0.603520 11.00000 0.04853 0.04105 =
0.05125 0.00783 0.02127 -0.00233
C9 1 0.049703 0.085253 0.595375 11.00000 0.04744 0.03567 =
0.04761 0.00472 0.01978 -0.00285
C10 1 0.112555 0.047555 0.622781 11.00000 0.05021 0.03613 =
0.05429 0.00850 0.01965 0.00046
C11 1 0.091818 0.264738 0.414568 11.00000 0.04792 0.03234 =
0.05094 -0.00122 0.02240 -0.00456
C12 1 0.098911 0.256408 0.508054 11.00000 0.04476 0.03372 =
0.05061 0.00447 0.01994 -0.00493
C13 1 0.104832 0.315818 0.565365 11.00000 0.05826 0.04102 =
0.04448 0.00277 0.02086 -0.00439
C14 1 0.105492 0.380959 0.527071 11.00000 0.06160 0.03354 =
0.04660 -0.00173 0.02331 -0.00371
AFIX 43
H14 2 0.109049 0.420202 0.564863 11.00000 -1.20000
AFIX 0
C15 1 0.105827 0.460571 0.398103 11.00000 0.06417 0.03269 =
0.04980 0.00022 0.02560 -0.00306
C16 1 0.100333 0.466679 0.306648 11.00000 0.09822 0.03345 =
0.05643 0.00455 0.03774 -0.00454
C17 1 0.089231 0.408667 0.245217 11.00000 0.08369 0.04423 =
0.04716 0.00269 0.03364 -0.00389
C18 1 0.086451 0.340872 0.275964 11.00000 0.04872 0.03659 =
0.04744 -0.00100 0.02166 -0.00384
C19 1 0.092594 0.331323 0.373244 11.00000 0.03955 0.03473 =
0.04488 0.00161 0.01787 -0.00224
C20 1 0.101031 0.390992 0.433254 11.00000 0.04448 0.03279 =
0.04531 0.00176 0.01839 -0.00294
C21 1 0.228112 0.178564 0.568421 11.00000 0.05052 0.07014 =
0.12686 0.03164 0.03753 -0.00206
AFIX 137
H21A 2 0.217622 0.190498 0.503019 11.00000 -1.50000
H21B 2 0.265173 0.145460 0.589895 11.00000 -1.50000
H21C 2 0.241254 0.220053 0.606991 11.00000 -1.50000
AFIX 0
C22 1 -0.071499 0.085212 0.594980 11.00000 0.06087 0.05707 =
0.11094 0.02655 0.04593 0.00424
AFIX 43
H22 2 -0.074661 0.133588 0.587247 11.00000 -1.20000
AFIX 0
C23 1 0.186632 -0.061960 0.699115 11.00000 0.06196 0.05031 =
0.09653 0.02359 0.02911 0.01198
AFIX 13
H23 2 0.221380 -0.029967 0.694703 11.00000 -1.20000
AFIX 0
C24 1 0.189356 -0.128394 0.645970 11.00000 0.09816 0.09730 =
0.12293 0.00120 0.04536 0.03881
AFIX 137
H24A 2 0.157754 -0.162121 0.652024 11.00000 -1.50000
H24B 2 0.234970 -0.147307 0.672530 11.00000 -1.50000
H24C 2 0.177066 -0.117752 0.579758 11.00000 -1.50000
AFIX 0
C25 1 0.206399 -0.077668 0.805776 11.00000 0.09705 0.17774 =
0.08971 0.00549 0.00398 0.06448
AFIX 137
H25A 2 0.206747 -0.034843 0.838956 11.00000 -1.50000
H25B 2 0.251177 -0.098554 0.832040 11.00000 -1.50000
H25C 2 0.173589 -0.109391 0.812779 11.00000 -1.50000
AFIX 0
C26 1 0.110956 0.307768 0.666649 11.00000 0.11668 0.04798 =
0.05117 0.00258 0.03747 -0.00947
AFIX 137
H26A 2 0.069299 0.288149 0.666647 11.00000 -1.50000
H26B 2 0.118820 0.352803 0.697113 11.00000 -1.50000
H26C 2 0.148652 0.277223 0.700727 11.00000 -1.50000
AFIX 0
C27 1 0.077133 0.286566 0.206415 11.00000 0.08613 0.04359 =
0.05292 -0.00307 0.03319 -0.00735
AFIX 43
H27 2 0.077594 0.240362 0.225998 11.00000 -1.20000
AFIX 0
C28 1 0.118087 0.525499 0.460488 11.00000 0.10361 0.03386 =
0.05555 -0.00113 0.03612 -0.00794
AFIX 13
H28 2 0.121655 0.509732 0.523409 11.00000 -1.20000
AFIX 0
C29 1 0.058836 0.576479 0.423902 11.00000 0.14554 0.06680 =
0.09101 -0.01263 0.04154 0.03099
AFIX 137
H29A 2 0.053288 0.592803 0.361761 11.00000 -1.50000
H29B 2 0.068014 0.615559 0.466772 11.00000 -1.50000
H29C 2 0.017576 0.553450 0.419938 11.00000 -1.50000
AFIX 0
C30 1 0.186215 0.561182 0.475085 11.00000 0.13169 0.08232 =
0.12035 -0.03075 0.04233 -0.04520
AFIX 137
H30A 2 0.221325 0.526310 0.487818 11.00000 -1.50000
H30B 2 0.198688 0.592918 0.528075 11.00000 -1.50000
H30C 2 0.181303 0.586668 0.418505 11.00000 -1.50000
AFIX 0
O1 3 -0.013953 0.188204 0.527606 11.00000 0.05121 0.04455 =
0.07241 0.01943 0.02877 0.00764
O2 3 -0.121610 0.052985 0.597425 11.00000 0.06319 0.08378 =
0.14839 0.03853 0.05892 0.00389
O3 3 -0.054955 -0.056040 0.634110 11.00000 0.06804 0.04788 =
0.07636 0.00764 0.03691 -0.01332
O4 3 0.060553 -0.123364 0.684120 11.00000 0.09282 0.03672 =
0.08675 0.01666 0.04490 0.00170
O5 3 0.083496 0.206890 0.358056 11.00000 0.09230 0.03220 =
0.05897 -0.00268 0.03668 -0.00840
O6 3 0.068580 0.297044 0.122649 11.00000 0.08971 0.05775 =
0.05158 -0.00861 0.03428 -0.00501
O7 3 0.083146 0.424383 0.156670 11.00000 0.16366 0.04973 =
0.05514 0.00276 0.05865 -0.00927
O8 3 0.105664 0.530463 0.269200 11.00000 0.22243 0.03865 =
0.07230 0.00426 0.07865 -0.01895
H1 2 -0.013513 0.222617 0.487908 11.00000 0.07730
H3 2 -0.086388 -0.021953 0.623587 11.00000 0.09515
H5 2 0.087534 0.171661 0.392185 11.00000 0.07530
H7 2 0.076874 0.381970 0.126309 11.00000 0.11067
H4A 2 0.013172 -0.125259 0.679757 11.00000 0.14697
H8 2 0.093947 0.523234 0.208567 11.00000 0.14963
HKLF 4
REM exp_1564gp3 in C2/c
REM R1 = 0.0474 for 4382 Fo > 4sig(Fo) and 0.0608 for all 5810 data
REM 374 parameters refined using 0 restraints
END
WGHT 0.0994 0.2158
REM Highest difference peak 0.441, deepest hole -0.299, 1-sigma level 0.036
Q1 1 0.2314 -0.0325 0.7784 11.00000 0.05 0.44
Q2 1 0.0987 0.2173 0.5250 11.00000 0.05 0.22
Q3 1 0.1066 0.4236 0.4203 11.00000 0.05 0.22
Q4 1 0.0813 0.4358 0.5722 11.00000 0.05 0.19
Q5 1 0.0524 0.1244 0.5929 11.00000 0.05 0.18
Q6 1 0.1175 0.0102 0.6493 11.00000 0.05 0.18
Q7 1 0.1068 0.3007 0.3958 11.00000 0.05 0.18
Q8 1 0.0711 0.1614 0.5282 11.00000 0.05 0.18
Q9 1 0.0005 0.0203 0.6330 11.00000 0.05 0.18
Q10 1 0.0838 0.3764 0.2599 11.00000 0.05 0.17
Q11 1 0.1710 0.5399 0.5203 11.00000 0.05 0.17
Q12 1 0.0131 0.0645 0.5854 11.00000 0.05 0.16
Q13 1 -0.0408 0.0636 0.5856 11.00000 0.05 0.16
Q14 1 0.1306 0.1596 0.5390 11.00000 0.05 0.16
Q15 1 0.2282 0.2277 0.5589 11.00000 0.05 0.16
Q16 1 0.0793 0.0604 0.6039 11.00000 0.05 0.15
Q17 1 0.0306 -0.0337 0.6419 11.00000 0.05 0.15
Q18 1 0.1058 0.4350 0.2858 11.00000 0.05 0.15
Q19 1 0.1072 0.3324 0.3381 11.00000 0.05 0.14
Q20 1 0.1788 -0.1425 0.7015 11.00000 0.05 0.14
REM The information below was added by Olex2.
REM
REM R1 = 0.0474 for 4382 Fo > 4sig(Fo) and 0.0608 for all 13686 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.44, deepest hole -0.30
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0608
REM R1_gt = 0.0474
REM wR_ref = 0.1612
REM GOOF = 1.113
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 13686
REM Reflections_gt = 4382
REM Parameters = n/a
REM Hole = -0.30
REM Peak = 0.44
REM Flack = n/a
;
_cod_data_source_file hb7412sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 5677.29(16)
_cod_database_code 2240807
_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.
;
_shelxl_version_number 2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
C C1 0.04702(8) 0.15341(8) 0.55658(11) 0.0429(3) Uani d 1
C C2 0.10359(8) 0.18397(8) 0.54801(11) 0.0447(3) Uani d 1
C C3 0.16553(8) 0.14655(9) 0.57686(13) 0.0547(4) Uani d 1
C C4 0.16876(9) 0.08045(9) 0.61308(14) 0.0564(4) Uani d 1
H H4 0.2100 0.0562 0.6322 0.068 Uiso calc 1
C C5 0.11810(9) -0.02370(8) 0.65817(12) 0.0518(4) Uani d 1
C C6 0.06006(9) -0.05514(8) 0.65630(12) 0.0512(4) Uani d 1
C C7 -0.00297(9) -0.01904(8) 0.62878(11) 0.0480(4) Uani d 1
C C8 -0.00888(8) 0.05136(8) 0.60352(11) 0.0465(3) Uani d 1
C C9 0.04970(8) 0.08525(8) 0.59537(11) 0.0433(3) Uani d 1
C C10 0.11255(8) 0.04756(8) 0.62278(12) 0.0472(4) Uani d 1
C C11 0.09182(8) 0.26474(7) 0.41457(11) 0.0428(3) Uani d 1
C C12 0.09891(8) 0.25641(7) 0.50805(11) 0.0427(3) Uani d 1
C C13 0.10483(9) 0.31582(8) 0.56537(11) 0.0477(4) Uani d 1
C C14 0.10549(9) 0.38096(8) 0.52707(11) 0.0466(4) Uani d 1
H H14 0.1090 0.4202 0.5649 0.056 Uiso calc 1
C C15 0.10583(9) 0.46057(7) 0.39810(11) 0.0479(4) Uani d 1
C C16 0.10033(11) 0.46668(8) 0.30665(13) 0.0605(5) Uani d 1
C C17 0.08923(10) 0.40867(9) 0.24522(12) 0.0559(4) Uani d 1
C C18 0.08645(8) 0.34087(7) 0.27596(11) 0.0434(3) Uani d 1
C C19 0.09259(7) 0.33132(7) 0.37324(10) 0.0393(3) Uani d 1
C C20 0.10103(7) 0.39099(7) 0.43325(10) 0.0407(3) Uani d 1
C C21 0.22811(10) 0.17856(12) 0.5684(2) 0.0817(7) Uani d 1
H H21A 0.2176 0.1905 0.5030 0.123 Uiso calc 1
H H21B 0.2652 0.1455 0.5899 0.123 Uiso calc 1
H H21C 0.2413 0.2201 0.6070 0.123 Uiso calc 1
C C22 -0.07150(10) 0.08521(11) 0.59498(18) 0.0725(6) Uani d 1
H H22 -0.0747 0.1336 0.5872 0.087 Uiso calc 1
C C23 0.18663(11) -0.06196(10) 0.69912(17) 0.0703(6) Uani d 1
H H23 0.2214 -0.0300 0.6947 0.084 Uiso calc 1
C C24 0.18936(15) -0.12839(16) 0.6460(2) 0.1056(9) Uani d 1
H H24A 0.1578 -0.1621 0.6520 0.158 Uiso calc 1
H H24B 0.2350 -0.1473 0.6725 0.158 Uiso calc 1
H H24C 0.1771 -0.1178 0.5798 0.158 Uiso calc 1
C C25 0.20640(17) -0.0777(2) 0.8058(2) 0.1318(14) Uani d 1
H H25A 0.2067 -0.0348 0.8390 0.198 Uiso calc 1
H H25B 0.2512 -0.0986 0.8320 0.198 Uiso calc 1
H H25C 0.1736 -0.1094 0.8128 0.198 Uiso calc 1
C C26 0.11096(13) 0.30777(10) 0.66665(13) 0.0706(6) Uani d 1
H H26A 0.0693 0.2881 0.6666 0.106 Uiso calc 1
H H26B 0.1188 0.3528 0.6971 0.106 Uiso calc 1
H H26C 0.1487 0.2772 0.7007 0.106 Uiso calc 1
C C27 0.07713(11) 0.28657(9) 0.20641(13) 0.0591(4) Uani d 1
H H27 0.0776 0.2404 0.2260 0.071 Uiso calc 1
C C28 0.11809(12) 0.52550(8) 0.46049(13) 0.0629(5) Uani d 1
H H28 0.1217 0.5097 0.5234 0.075 Uiso calc 1
C C29 0.05884(17) 0.57648(13) 0.4239(2) 0.1027(9) Uani d 1
H H29A 0.0533 0.5928 0.3618 0.154 Uiso calc 1
H H29B 0.0680 0.6156 0.4668 0.154 Uiso calc 1
H H29C 0.0176 0.5534 0.4199 0.154 Uiso calc 1
C C30 0.18621(17) 0.56118(16) 0.4751(2) 0.1138(11) Uani d 1
H H30A 0.2213 0.5263 0.4878 0.171 Uiso calc 1
H H30B 0.1987 0.5929 0.5281 0.171 Uiso calc 1
H H30C 0.1813 0.5867 0.4185 0.171 Uiso calc 1
O O1 -0.01395(6) 0.18820(6) 0.52761(9) 0.0547(3) Uani d 1
O O2 -0.12161(8) 0.05299(9) 0.59743(15) 0.0931(6) Uani d 1
O O3 -0.05495(7) -0.05604(7) 0.63411(10) 0.0615(3) Uani d 1
O O4 0.06055(9) -0.12336(6) 0.68412(11) 0.0692(4) Uani d 1
O O5 0.08350(7) 0.20689(6) 0.35806(9) 0.0590(3) Uani d 1
O O6 0.06858(8) 0.29704(7) 0.12265(9) 0.0644(4) Uani d 1
O O7 0.08315(11) 0.42438(8) 0.15667(10) 0.0847(5) Uani d 1
O O8 0.10566(13) 0.53046(7) 0.26920(13) 0.1047(8) Uani d 1
H H1 -0.0135(11) 0.2226(13) 0.4879(17) 0.077(7) Uiso d 1
H H3 -0.0864(15) -0.0220(15) 0.6236(19) 0.095(9) Uiso d 1
H H5 0.0875(12) 0.1717(13) 0.3922(16) 0.075(7) Uiso d 1
H H7 0.0769(15) 0.3820(18) 0.126(2) 0.111(10) Uiso d 1
H H4A 0.0132(19) -0.1253(18) 0.680(3) 0.147(13) Uiso d 1
H H8 0.094(2) 0.523(2) 0.209(3) 0.150(14) 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
C1 0.0461(8) 0.0365(7) 0.0473(7) 0.0015(6) 0.0197(6) 0.0053(6)
C2 0.0508(8) 0.0338(7) 0.0500(8) -0.0038(6) 0.0206(7) 0.0057(6)
C3 0.0477(9) 0.0472(8) 0.0699(10) -0.0027(7) 0.0240(8) 0.0120(8)
C4 0.0468(9) 0.0466(9) 0.0758(11) 0.0064(7) 0.0242(8) 0.0159(8)
C5 0.0574(9) 0.0379(8) 0.0594(9) 0.0047(7) 0.0224(8) 0.0097(7)
C6 0.0695(10) 0.0341(7) 0.0532(9) -0.0007(7) 0.0275(8) 0.0091(6)
C7 0.0574(9) 0.0423(8) 0.0479(8) -0.0098(7) 0.0246(7) 0.0035(6)
C8 0.0485(8) 0.0411(7) 0.0512(8) -0.0023(6) 0.0213(7) 0.0078(6)
C9 0.0474(8) 0.0357(7) 0.0476(7) -0.0029(6) 0.0198(6) 0.0047(6)
C10 0.0502(8) 0.0361(7) 0.0543(8) 0.0005(6) 0.0197(7) 0.0085(6)
C11 0.0479(8) 0.0323(7) 0.0509(8) -0.0046(6) 0.0224(6) -0.0012(6)
C12 0.0448(8) 0.0337(7) 0.0506(8) -0.0049(6) 0.0199(6) 0.0045(6)
C13 0.0583(9) 0.0410(8) 0.0445(8) -0.0044(7) 0.0209(7) 0.0028(6)
C14 0.0616(9) 0.0335(7) 0.0466(8) -0.0037(6) 0.0233(7) -0.0017(6)
C15 0.0642(10) 0.0327(7) 0.0498(8) -0.0031(6) 0.0256(7) 0.0002(6)
C16 0.0982(14) 0.0334(7) 0.0564(9) -0.0045(8) 0.0377(10) 0.0046(7)
C17 0.0837(12) 0.0442(8) 0.0472(8) -0.0039(8) 0.0336(8) 0.0027(7)
C18 0.0487(8) 0.0366(7) 0.0474(8) -0.0038(6) 0.0217(6) -0.0010(6)
C19 0.0396(7) 0.0347(7) 0.0449(7) -0.0022(5) 0.0179(6) 0.0016(6)
C20 0.0445(7) 0.0328(6) 0.0453(7) -0.0029(5) 0.0184(6) 0.0018(6)
C21 0.0505(10) 0.0701(13) 0.1269(19) -0.0021(9) 0.0375(11) 0.0316(13)
C22 0.0609(11) 0.0571(10) 0.1109(17) 0.0042(9) 0.0459(11) 0.0266(11)
C23 0.0620(11) 0.0503(10) 0.0965(15) 0.0120(8) 0.0291(10) 0.0236(10)
C24 0.0982(19) 0.0973(19) 0.123(2) 0.0388(16) 0.0454(17) 0.0012(17)
C25 0.097(2) 0.178(3) 0.0897(19) 0.064(2) 0.0040(15) 0.005(2)
C26 0.1167(17) 0.0480(9) 0.0512(9) -0.0095(10) 0.0375(10) 0.0026(8)
C27 0.0861(13) 0.0436(8) 0.0529(9) -0.0074(8) 0.0332(9) -0.0031(7)
C28 0.1036(15) 0.0339(7) 0.0555(9) -0.0079(8) 0.0361(10) -0.0011(7)
C29 0.146(3) 0.0668(14) 0.0910(17) 0.0310(15) 0.0415(17) -0.0126(12)
C30 0.132(3) 0.0823(17) 0.120(2) -0.0452(17) 0.0423(19) -0.0307(16)
O1 0.0512(6) 0.0445(6) 0.0724(8) 0.0076(5) 0.0288(6) 0.0194(5)
O2 0.0632(9) 0.0838(11) 0.1484(16) 0.0039(7) 0.0589(10) 0.0385(10)
O3 0.0680(8) 0.0479(7) 0.0764(8) -0.0133(6) 0.0369(7) 0.0076(6)
O4 0.0928(10) 0.0367(6) 0.0868(10) 0.0017(6) 0.0449(8) 0.0167(6)
O5 0.0923(9) 0.0322(5) 0.0590(7) -0.0084(6) 0.0367(6) -0.0027(5)
O6 0.0897(9) 0.0578(7) 0.0516(7) -0.0050(6) 0.0343(6) -0.0086(5)
O7 0.1637(17) 0.0497(7) 0.0551(8) -0.0093(9) 0.0587(9) 0.0028(6)
O8 0.222(2) 0.0387(7) 0.0723(10) -0.0190(10) 0.0786(13) 0.0043(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C2 C1 C9 122.05(14)
O1 C1 C2 120.70(13)
O1 C1 C9 117.25(13)
C1 C2 C3 119.61(14)
C1 C2 C12 120.39(14)
C3 C2 C12 120.00(13)
C2 C3 C21 120.78(15)
C4 C3 C2 119.13(15)
C4 C3 C21 120.08(16)
C3 C4 H4 118.5
C3 C4 C10 123.02(15)
C10 C4 H4 118.5
C6 C5 C10 117.78(15)
C6 C5 C23 120.46(15)
C10 C5 C23 121.73(16)
C5 C6 C7 122.28(14)
C5 C6 O4 121.16(16)
O4 C6 C7 116.53(15)
C8 C7 C6 121.68(14)
O3 C7 C6 115.50(14)
O3 C7 C8 122.71(16)
C7 C8 C9 117.94(14)
C7 C8 C22 116.05(14)
C22 C8 C9 125.83(14)
C1 C9 C8 123.34(14)
C1 C9 C10 117.61(13)
C10 C9 C8 118.97(13)
C4 C10 C5 120.68(15)
C4 C10 C9 118.55(13)
C9 C10 C5 120.76(14)
C12 C11 C19 122.99(13)
O5 C11 C12 119.42(13)
O5 C11 C19 117.59(13)
C11 C12 C2 119.23(13)
C11 C12 C13 119.66(13)
C13 C12 C2 121.04(14)
C12 C13 C26 120.37(14)
C14 C13 C12 118.54(14)
C14 C13 C26 121.09(15)
C13 C14 H14 118.5
C13 C14 C20 123.09(14)
C20 C14 H14 118.5
C16 C15 C20 117.91(14)
C16 C15 C28 119.79(14)
C20 C15 C28 122.29(14)
C15 C16 C17 122.66(14)
C15 C16 O8 121.16(15)
O8 C16 C17 116.18(15)
C18 C17 C16 121.81(14)
O7 C17 C16 114.77(15)
O7 C17 C18 123.41(15)
C17 C18 C19 117.74(13)
C17 C18 C27 115.76(14)
C27 C18 C19 126.49(14)
C11 C19 C18 123.67(13)
C11 C19 C20 116.70(13)
C20 C19 C18 119.62(12)
C14 C20 C15 120.88(13)
C14 C20 C19 118.94(12)
C19 C20 C15 120.17(13)
C3 C21 H21A 109.5
C3 C21 H21B 109.5
C3 C21 H21C 109.5
H21A C21 H21B 109.5
H21A C21 H21C 109.5
H21B C21 H21C 109.5
C8 C22 H22 118.4
O2 C22 C8 123.15(18)
O2 C22 H22 118.4
C5 C23 H23 107.2
C5 C23 C25 110.12(19)
C24 C23 C5 114.39(19)
C24 C23 H23 107.2
C24 C23 C25 110.5(2)
C25 C23 H23 107.2
C23 C24 H24A 109.5
C23 C24 H24B 109.5
C23 C24 H24C 109.5
H24A C24 H24B 109.5
H24A C24 H24C 109.5
H24B C24 H24C 109.5
C23 C25 H25A 109.5
C23 C25 H25B 109.5
C23 C25 H25C 109.5
H25A C25 H25B 109.5
H25A C25 H25C 109.5
H25B C25 H25C 109.5
C13 C26 H26A 109.5
C13 C26 H26B 109.5
C13 C26 H26C 109.5
H26A C26 H26B 109.5
H26A C26 H26C 109.5
H26B C26 H26C 109.5
C18 C27 H27 117.7
O6 C27 C18 124.58(16)
O6 C27 H27 117.7
C15 C28 H28 106.9
C15 C28 C30 111.80(19)
C29 C28 C15 112.44(18)
C29 C28 H28 106.9
C29 C28 C30 111.5(2)
C30 C28 H28 106.9
C28 C29 H29A 109.5
C28 C29 H29B 109.5
C28 C29 H29C 109.5
H29A C29 H29B 109.5
H29A C29 H29C 109.5
H29B C29 H29C 109.5
C28 C30 H30A 109.5
C28 C30 H30B 109.5
C28 C30 H30C 109.5
H30A C30 H30B 109.5
H30A C30 H30C 109.5
H30B C30 H30C 109.5
C1 O1 H1 108.3(15)
C7 O3 H3 100.3(18)
C6 O4 H4A 98(2)
C11 O5 H5 107.5(16)
C17 O7 H7 104.4(19)
C16 O8 H8 105(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.387(2)
C1 C9 1.421(2)
C1 O1 1.3633(18)
C2 C3 1.405(2)
C2 C12 1.4985(19)
C3 C4 1.368(2)
C3 C21 1.513(2)
C4 H4 0.9300
C4 C10 1.406(2)
C5 C6 1.360(2)
C5 C10 1.451(2)
C5 C23 1.523(2)
C6 C7 1.413(2)
C6 O4 1.3685(18)
C7 C8 1.390(2)
C7 O3 1.3392(19)
C8 C9 1.450(2)
C8 C22 1.436(2)
C9 C10 1.425(2)
C11 C12 1.383(2)
C11 C19 1.4218(19)
C11 O5 1.3688(18)
C12 C13 1.407(2)
C13 C14 1.376(2)
C13 C26 1.507(2)
C14 H14 0.9300
C14 C20 1.410(2)
C15 C16 1.358(2)
C15 C20 1.4509(19)
C15 C28 1.521(2)
C16 C17 1.409(2)
C16 O8 1.368(2)
C17 C18 1.386(2)
C17 O7 1.339(2)
C18 C19 1.449(2)
C18 C27 1.440(2)
C19 C20 1.428(2)
C21 H21A 0.9600
C21 H21B 0.9600
C21 H21C 0.9600
C22 H22 0.9300
C22 O2 1.242(2)
C23 H23 0.9800
C23 C24 1.519(4)
C23 C25 1.541(4)
C24 H24A 0.9600
C24 H24B 0.9600
C24 H24C 0.9600
C25 H25A 0.9600
C25 H25B 0.9600
C25 H25C 0.9600
C26 H26A 0.9600
C26 H26B 0.9600
C26 H26C 0.9600
C27 H27 0.9300
C27 O6 1.234(2)
C28 H28 0.9800
C28 C29 1.512(3)
C28 C30 1.533(4)
C29 H29A 0.9600
C29 H29B 0.9600
C29 H29C 0.9600
C30 H30A 0.9600
C30 H30B 0.9600
C30 H30C 0.9600
O1 H1 0.90(2)
O3 H3 0.90(3)
O4 H4A 0.98(4)
O5 H5 0.83(2)
O7 H7 0.92(3)
O8 H8 0.87(4)
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
O1 H1 O6 2 0.90(2) 2.16(2) 2.9692(17) 150(2)
O3 H3 O2 . 0.90(3) 1.59(3) 2.454(2) 160(3)
O5 H5 O3 5_556 0.83(2) 2.30(2) 2.9546(17) 136(2)
O4 H4A O3 . 0.98(4) 1.88(4) 2.601(2) 128(3)
O4 H4A O5 5_556 0.98(4) 2.46(4) 3.278(2) 141(3)
O7 H7 O6 . 0.92(3) 1.63(3) 2.479(2) 152(3)
O8 H8 O7 . 0.87(4) 2.02(4) 2.575(2) 120(3)
C22 H22 O1 . 0.93 2.12 2.721(2) 121
C26 H26B O8 6_566 0.96 2.55 3.483(2) 165
C27 H27 O4 6 0.93 2.31 3.138(2) 148
C27 H27 O5 . 0.93 2.07 2.727(2) 127
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.217 0.250 -0.033 444 28 ' '
2 0.717 0.750 -0.033 444 28 ' '
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
0 0 -2 60705.6
0 0 -2 61954.9
0 0 2 58497.9
0 0 2 58341.8
0 0 -3 64.7394
0 0 3 36.1111
0 0 3 24.29
0 0 4 486875
0 0 4 497883
0 0 5 2412.02
0 0 5 -23.9318
0 0 6 3966.41
0 0 7 47.8588
0 0 8 3811.02
0 0 9 6.72018
0 0 10 1834.86
0 0 -10 1822.84
0 0 11 -28.8315
0 0 11 91.8563
0 0 11 -146.598
0 0 12 1590.01
0 0 12 1831.83
0 0 13 -16.7475
0 0 13 -148.824
0 0 14 118.99
0 0 15 -44.9693
0 0 16 13.6635
0 0 17 -16.2655
0 -2 0 348799
0 -2 -1 9653.67
0 -2 1 9920.04
0 -2 1 10020.2
0 2 -1 10252.8
0 2 1 10184.3
0 -2 -2 104349
0 -2 2 105384
0 2 2 105537
0 -2 3 277874
0 -2 3 284472
0 -2 -3 279192
0 2 3 276043
0 -2 4 81098.5
0 -2 4 80709.2
0 2 5 102953
0 -2 5 101941
0 -2 -6 3652.88
0 -2 6 3943.21
0 -2 6 3792.97
0 2 6 3681.09
0 -2 -7 134809
0 2 7 136299
0 -2 8 4048.05
0 -2 -8 4021.48
0 2 8 3864.87
0 -2 -9 1283.78
0 -2 9 1336.04
0 2 9 1548.38
0 2 10 363.062
0 -2 10 481.652
0 -2 11 577.39
0 2 11 656.632
0 2 11 531.896
0 -2 11 574.663
0 -2 12 34.8856
0 2 12 9.18023
0 2 12 -1.14482
0 2 13 -12.1433
0 -2 13 35.6172
0 2 13 -52.5405
0 -2 14 2782.78
0 2 14 2709.02
0 2 14 2760.39
0 2 15 781.371
0 2 15 835.307
0 -2 15 877.922
0 -2 15 818.109
0 -2 16 415.507
0 2 16 262.018
0 -2 17 71.8238
0 2 17 146.661
0 -4 0 8232.68
0 4 0 8104.73
0 -4 -1 34013.5
0 -4 1 31468.5
0 -4 -2 5828.63
0 -4 2 5479.94
0 -4 -2 5774.72
0 -4 3 7486.68
0 -4 -3 7652.56
0 -4 -4 68.068
0 -4 4 136.852
0 -4 4 28.2201
0 -4 -5 83937.2
0 -4 5 85120
0 -4 6 11216
0 -4 -6 11163.9
0 -4 -7 48349.2
0 -4 7 45762.1
0 -4 8 22525.4
0 -4 -8 24170.9
0 -4 -9 12634.1
0 -4 9 12690.2
0 4 10 2372.31
0 4 11 3897.16
0 -4 11 3663.25
0 4 11 3832.88
0 4 11 4108.06
0 -4 11 3612.08
0 4 12 520.924
0 -4 12 362.712
0 4 12 443.233
0 4 13 8556.82
0 4 13 8701.7
0 -4 13 8636.73
0 4 14 81.5773
0 -4 14 120.176
0 4 14 157.491
0 -4 15 63.3501
0 4 15 2.15491
0 4 15 -23.4652
0 4 16 207.623
0 -4 16 299.694
0 4 17 94.5087
0 -4 17 124.331
0 -6 0 34973.1
0 6 0 35407.4
0 -6 -1 749.068
0 -6 1 755.232
0 -6 -2 2937.22
0 -6 2 2766.39
0 -6 3 32111
0 -6 -4 28406.2
0 -6 4 27389.3
0 -6 5 918.642
0 -6 -5 757.574
0 -6 5 798.588
0 -6 6 438.474
0 -6 -6 416
0 -6 6 398.924
0 -6 7 2485.66
0 -6 -7 2011.31
0 -6 8 4396.06
0 -6 -8 4634.74
0 -6 -9 13132.2
0 -6 9 12703.1
0 6 10 12450.7
0 6 10 12944.3
0 6 10 13583.3
0 -6 10 12637.2
0 -6 10 12542.9
0 -6 11 31977.9
0 6 11 32210.6
0 -6 11 31680.7
0 6 11 32872.9
0 -6 12 7719.15
0 6 12 8154.13
0 6 12 8519.3
0 6 12 8715.46
0 6 13 2927.91
0 6 13 3605.96
0 -6 13 3218.89
0 6 13 3403.64
0 6 14 55.1422
0 6 14 -24.3008
0 -6 14 -6.89099
0 6 15 704.271
0 -6 15 852.58
0 6 15 890.693
0 6 16 268.543
0 -6 16 222.827
0 -6 16 259.227
0 8 0 472245
0 -8 0 423558
0 -8 -1 21686.5
0 -8 1 21859.6
0 -8 -2 2139.17
0 -8 2 2204.93
0 -8 2 2234.85
0 -8 3 7926.3
0 -8 4 120811
0 -8 5 899.549
0 -8 6 2367.74
0 -8 7 4409.07
0 -8 8 4398.37
0 8 9 5692.39
0 8 9 5331.36
0 -8 9 5662.6
0 -8 10 1374.41
0 8 10 1302.72
0 8 10 1137.81
0 -8 11 1677.09
0 8 11 1694.27
0 8 11 1589.54
0 8 12 1981.01
0 8 12 2358.62
0 -8 12 2193.13
0 8 12 2276.4
0 8 13 255.002
0 8 13 185.823
0 8 13 132.232
0 -8 13 257.787
0 8 14 129.55
0 8 14 104.945
0 8 14 18.7747
0 8 15 -1.79559
0 -8 16 11.1747
0 -10 0 15504.1
0 -10 1 69925
0 -10 -1 70292.3
0 -10 2 117.153
0 -10 2 11.3113
0 -10 -2 5.16833
0 -10 -3 1271.2
0 -10 3 1421.79
0 -10 4 1385.67
0 -10 -4 1162.82
0 -10 5 1052.14
0 -10 6 1555.68
0 -10 7 314.899
0 10 8 347.532
0 -10 8 427.216
0 10 8 410.768
0 -10 9 34444.8
0 10 9 33786
0 -10 10 5403.04
0 10 10 4919.44
0 10 10 4992.47
0 -10 11 455.437
0 10 11 337.311
0 10 11 345.442
0 -10 12 177.784
0 10 12 224.901
0 10 12 144.491
0 10 13 749.078
0 10 13 685.224
0 10 14 266.603
0 10 14 250.643
0 -10 15 -34.8366
0 10 15 -18.7181
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