#------------------------------------------------------------------------------
#$Date: 2025-08-19 15:49:58 +0100 (Tue, 19 Aug 2025) $
#$Revision: 301806 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/89/2238909.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_2238909
loop_
_publ_author_name
'Corfield, Peter W. R.'
'Balija, Amy M.'
_publ_section_title
;
Benzene-1,3,5-triyl tribenzoate
;
_journal_coeditor_code PK2503
_journal_issue 12
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first o1822
_journal_page_last o1823
_journal_paper_doi 10.1107/S1600536813031462
_journal_volume 69
_journal_year 2013
_chemical_formula_iupac 'C27 H18 O6'
_chemical_formula_moiety 'C27 H18 O6'
_chemical_formula_sum 'C27 H18 O6'
_chemical_formula_weight 438.41
_chemical_name_common 'phloroglucinol tribenzoate'
_chemical_name_systematic
;
Benzene-1,3,5-triyl tribenzoate
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_cell_angle_alpha 90.00
_cell_angle_beta 103.22(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 23.128(5)
_cell_length_b 6.332(2)
_cell_length_c 15.030(3)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 295(2)
_cell_measurement_theta_max 20.3
_cell_measurement_theta_min 3.6
_cell_volume 2142.8(9)
_computing_cell_refinement 'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_collection 'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction
;
data reduction followed procedures in Corfield et al. (1973);
data were averaged with a local version of SORTAV (Blessing,
1989)
;
_computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Enraf--Nonius CAD-4'
_diffrn_measurement_method '\q/2\q scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71070
_diffrn_reflns_av_R_equivalents 0.0210
_diffrn_reflns_av_sigmaI/netI 0.0847
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 4950
_diffrn_reflns_theta_full 24.98
_diffrn_reflns_theta_max 24.98
_diffrn_reflns_theta_min 1.81
_diffrn_standards_decay_% 0.5(4)
_diffrn_standards_interval_time 120
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.096
_exptl_absorpt_correction_type none
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.359
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'plate cut from large crystal'
_exptl_crystal_F_000 912
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.13
_refine_diff_density_max 0.154
_refine_diff_density_min -0.163
_refine_ls_extinction_coef 0.0067(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 295
_refine_ls_number_reflns 3775
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.027
_refine_ls_R_factor_all 0.1164
_refine_ls_R_factor_gt 0.0401
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.4500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0913
_refine_ls_wR_factor_ref 0.1137
_reflns_number_gt 2096
_reflns_number_total 3775
_reflns_threshold_expression I>2\s(I)
_iucr_refine_instructions_details
;
TITL Balija dendrimer final refinement
REM C22-C27 and Q1 Q2 from full aniso refinement
CELL 0.7107 23.128 6.332 15.030 90. 103.22 90.
ZERR 4 .005 .002 .003 0.0 .02 0.0
LATT 1
SYMM x, 0.5-y, 0.5+z
SFAC O C H
UNIT 24 108 72
MORE 2
BOND $H
ACTA
BIND C9B C27B
FREE C9B C22B
EADP C22A C22B
EADP C23A C23B
EADP C24A C24B
EADP C25A C25B
EADP C26A C26B
EADP C27A C27B
DFIX 1.50 0.02 C9B C27B
DFIX 1.35 0.02 C9B O3
MPLA 6 C1 C2 C3 C4 C5 C6 O1 O2 O3 O4 O5 O6A O6B
MPLA 6 C10 C11 C12 C13 C14 C15 C7 O4 O1 C1
MPLA 6 C1 C2 C3 C4 C5 C6 O1 O2 O3
MPLA 6 C16 C17 C18 C19 C20 C21 C8 O5 O2 C3
MPLA 6 C1 C2 C3 C4 C5 C6 O1 O2 O3
MPLA 6 C22A C23A C24A C25A C26A C27A C9A O6A O3 C5
MPLA 6 C22B C23B C24B C25B C26B C27B C9B O6B O3 C5
CONF C6 C1 O1 C7
CONF C1 O1 C7 O4
CONF C1 O1 C7 C10
CONF O1 C7 C10 C11
CONF O1 C7 C10 C15
CONF C2 C3 O2 C8
CONF C3 O2 C8 O5
CONF C3 O2 C8 C16
CONF O2 C8 C16 C17
CONF O2 C8 C16 C21
CONF C4 C5 O3 C9A
CONF C4 C5 O3 C9B
CONF C5 O3 C9A O6A
CONF C5 O3 C9A C22A
CONF C5 O3 C9B O6B
CONF C5 O3 C9B C22B
CONF O3 C9A C22A C23A
CONF O3 C9A C22A C27A
CONF O3 C9B C27B C26B
CONF O3 C9B C27B C22B
L.S. 15
FMAP -2
WGHT 0.000000 0.450000
EXTI 0.006855
FVAR 0.32168 0.86934
O1 1 0.356611 0.533984 0.494409 11.00000 0.04755 0.03818 =
0.04989 -0.00002 0.00029 0.00478
O2 1 0.155558 0.341352 0.350766 11.00000 0.04722 0.04294 =
0.05809 -0.00699 0.01685 -0.01230
O3 1 0.240686 0.962099 0.258152 11.00000 0.05166 0.04529 =
0.06342 0.01770 0.01102 0.00244
O4 1 0.370505 0.208048 0.445259 11.00000 0.05911 0.05522 =
0.09928 -0.02901 0.00066 0.00528
O5 1 0.118743 0.554149 0.443222 11.00000 0.06788 0.06115 =
0.09254 -0.03280 0.03075 -0.01565
C1 2 0.303559 0.561005 0.428002 11.00000 0.03955 0.04169 =
0.03818 -0.00126 0.00443 0.00457
C2 2 0.256229 0.425939 0.421218 11.00000 0.05069 0.03720 =
0.04448 0.00321 0.01298 -0.00263
AFIX 43
H2 3 0.259038 0.304988 0.457056 11.00000 -1.20000
AFIX 0
C3 2 0.204808 0.476725 0.359573 11.00000 0.04131 0.03882 =
0.04642 -0.00362 0.01055 -0.00478
C4 2 0.199809 0.651412 0.303640 11.00000 0.03879 0.04735 =
0.04317 -0.00119 0.00644 0.00049
AFIX 43
H4 3 0.164591 0.680908 0.261397 11.00000 -1.20000
AFIX 0
C5 2 0.248596 0.780862 0.312277 11.00000 0.04214 0.03717 =
0.04575 0.00578 0.01040 0.00198
C6 2 0.300917 0.740469 0.375409 11.00000 0.04285 0.03955 =
0.04574 0.00117 0.00911 -0.00288
AFIX 43
H6 3 0.333252 0.831213 0.382205 11.00000 -1.20000
AFIX 0
C7 2 0.387786 0.351919 0.495722 11.00000 0.04607 0.03975 =
0.05216 -0.00013 0.01408 -0.00166
C8 2 0.114078 0.398539 0.396788 11.00000 0.04406 0.04721 =
0.04717 -0.00173 0.00750 -0.00014
AFIX 66 1.3780
C10 2 0.444943 0.358424 0.564901 11.00000 0.04059 0.04100 =
0.04821 0.00259 0.01280 0.00239
C11 2 0.478963 0.177508 0.576854 11.00000 0.05178 0.04575 =
0.07478 0.00172 0.01276 0.00681
AFIX 43
H11 3 0.464604 0.055045 0.545264 11.00000 -1.20000
AFIX 65 1.3780
C12 2 0.534260 0.178053 0.635615 11.00000 0.05774 0.06033 =
0.08032 0.01024 0.01116 0.01939
AFIX 43
H12 3 0.557219 0.055958 0.643681 11.00000 -1.20000
AFIX 65 1.3780
C13 2 0.555538 0.359514 0.682424 11.00000 0.04921 0.08235 =
0.06010 0.00257 0.00574 0.00447
AFIX 43
H13 3 0.592856 0.359881 0.722080 11.00000 -1.20000
AFIX 65 1.3780
C14 2 0.521518 0.540432 0.670472 11.00000 0.05820 0.06196 =
0.06670 -0.00916 0.00217 -0.00163
AFIX 43
H14 3 0.535878 0.662894 0.702062 11.00000 -1.20000
AFIX 65 1.3780
C15 2 0.466221 0.539890 0.611711 11.00000 0.05454 0.04947 =
0.05760 -0.00150 0.00514 0.00834
AFIX 43
H15 3 0.443263 0.661985 0.603644 11.00000 -1.20000
AFIX 66 1.3780
C16 2 0.063917 0.247867 0.382776 11.00000 0.04433 0.04370 =
0.04234 0.00154 0.00653 -0.00367
C17 2 0.066661 0.049588 0.346168 11.00000 0.04705 0.04627 =
0.05835 0.00428 0.00755 -0.00129
AFIX 43
H17 3 0.101119 0.005597 0.329648 11.00000 -1.20000
AFIX 65 1.3780
C18 2 0.018344 -0.083507 0.334040 11.00000 0.06309 0.04923 =
0.06439 -0.00138 0.00327 -0.01425
AFIX 43
H18 3 0.020196 -0.217319 0.309335 11.00000 -1.20000
AFIX 65 1.3780
C19 2 -0.032716 -0.018323 0.358519 11.00000 0.06004 0.08034 =
0.07432 0.00090 0.01251 -0.03182
AFIX 43
H19 3 -0.065323 -0.108145 0.350333 11.00000 -1.20000
AFIX 65 1.3780
C20 2 -0.035460 0.179955 0.395126 11.00000 0.05437 0.09122 =
0.08515 -0.00192 0.02816 -0.01534
AFIX 43
H20 3 -0.069919 0.223945 0.411646 11.00000 -1.20000
AFIX 65 1.3780
C21 2 0.012856 0.313052 0.407255 11.00000 0.05754 0.06389 =
0.06216 -0.00665 0.02205 -0.00620
AFIX 43
H21 3 0.011004 0.446864 0.431960 11.00000 -1.20000
AFIX 0
PART 1
C22A 2 0.262071 1.234849 0.166405 21.00000 0.05239 0.03779 =
0.03777 0.00182 0.00953 0.00080
C23A 2 0.304879 1.373299 0.149692 21.00000 0.05644 0.04659 =
0.05077 0.00906 0.00643 -0.00558
AFIX 43
H23A 3 0.344913 1.346092 0.173817 21.00000 -1.20000
AFIX 0
C24A 2 0.287928 1.552196 0.097011 21.00000 0.07298 0.04797 =
0.05887 0.01381 0.00967 -0.00954
AFIX 43
H24A 3 0.316525 1.647095 0.087198 21.00000 -1.20000
AFIX 0
C25A 2 0.229405 1.588946 0.059637 21.00000 0.07539 0.04488 =
0.05164 0.01083 0.01479 0.01020
AFIX 43
H25A 3 0.218284 1.708140 0.023637 21.00000 -1.20000
AFIX 0
C26A 2 0.186729 1.451930 0.074572 21.00000 0.05890 0.05752 =
0.05164 0.00443 0.01227 0.01949
AFIX 43
H26A 3 0.146955 1.477406 0.047791 21.00000 -1.20000
AFIX 0
C27A 2 0.202452 1.276607 0.129067 21.00000 0.04901 0.04713 =
0.05228 0.00373 0.01652 0.00864
AFIX 43
H27A 3 0.173298 1.186618 0.140810 21.00000 -1.20000
AFIX 0
C9A 2 0.283684 1.047088 0.222540 21.00000 0.04242 0.04245 =
0.04376 0.00169 0.01025 -0.00151
O6A 1 0.332664 0.976114 0.234894 21.00000 0.04711 0.06635 =
0.07509 0.02561 0.01912 0.01413
PART 2
AFIX 66 1.3780
C27B 2 0.221290 1.234407 0.149718 -21.00000 0.04901 0.04713 =
0.05228 0.00373 0.01652 0.00864
C22B 2 0.280132 1.294065 0.172670 -21.00000 0.05239 0.03779 =
0.03777 0.00182 0.00953 0.00080
AFIX 43
H22B 3 0.307632 1.212482 0.213175 -21.00000 -1.20000
AFIX 65 1.3780
C23B 2 0.298225 1.474610 0.135605 -21.00000 0.05644 0.04659 =
0.05077 0.00906 0.00643 -0.00558
AFIX 43
H23B 3 0.337936 1.514871 0.151096 -21.00000 -1.20000
AFIX 65 1.3780
C24B 2 0.257476 1.595499 0.075587 -21.00000 0.07298 0.04797 =
0.05887 0.01381 0.00967 -0.00954
AFIX 43
H24B 3 0.269687 1.717343 0.050574 -21.00000 -1.20000
AFIX 65 1.3780
C25B 2 0.198634 1.535844 0.052634 -21.00000 0.07539 0.04488 =
0.05164 0.01083 0.01479 0.01020
AFIX 43
H25B 3 0.171135 1.617428 0.012130 -21.00000 -1.20000
AFIX 65 1.3780
C26B 2 0.180540 1.355299 0.089698 -21.00000 0.05890 0.05752 =
0.05164 0.00443 0.01227 0.01949
AFIX 43
H26B 3 0.140830 1.315040 0.074208 -21.00000 -1.20000
AFIX 0
O6B 1 0.153539 0.978072 0.187716 -21.00000 0.04249 0.06929 =
0.11853 0.03219 0.01713 -0.00321
C9B 2 0.199794 1.048061 0.196433 -21.00000 0.05871
PART 0
HKLF 4
REM Balija dendrimer final refinement
REM R1 = 0.0401 for 2096 Fo > 4sig(Fo) and 0.1164 for all 3775 data
REM 295 parameters refined using 2 restraints
END
WGHT 0.0000 0.4375
REM Highest difference peak 0.154, deepest hole -0.163, 1-sigma level 0.037
Q1 1 0.3545 0.3485 0.4644 11.00000 0.05 -0.16
Q2 1 0.1455 1.7885 0.0296 11.00000 0.05 0.15
Q3 1 0.3984 0.1241 0.5174 11.00000 0.05 0.15
Q4 1 0.3877 0.3823 0.5421 11.00000 0.05 -0.15
Q5 1 0.1740 1.2291 0.0781 11.00000 0.05 -0.14
Q6 1 0.1582 1.3228 0.1388 11.00000 0.05 -0.13
Q7 1 0.4812 0.6624 0.6375 11.00000 0.05 -0.13
Q8 1 0.2574 0.6621 0.4624 11.00000 0.05 0.13
Q9 1 0.6072 0.4363 0.6837 11.00000 0.05 0.13
Q10 1 0.1486 0.5042 0.1793 11.00000 0.05 -0.13
Q11 1 0.2505 1.0209 0.2595 11.00000 0.05 0.13
Q12 1 0.4071 0.2447 0.5146 11.00000 0.05 -0.13
Q13 1 0.1334 1.5614 0.0773 11.00000 0.05 0.13
Q14 1 0.3421 0.4270 0.5200 11.00000 0.05 -0.13
Q15 1 0.2918 0.4379 0.4068 11.00000 0.05 0.13
Q16 1 -0.0225 0.4892 0.3222 11.00000 0.05 0.12
Q17 1 0.4172 0.3247 0.5529 11.00000 0.05 0.12
Q18 1 -0.0422 0.2851 0.4331 11.00000 0.05 -0.12
Q19 1 0.2290 0.7752 0.3438 11.00000 0.05 0.12
Q20 1 0.5284 0.3961 0.5417 11.00000 0.05 -0.12
;
_cod_data_source_file pk2503.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2238909
loop_
_symmetry_equiv_pos_as_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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.35661(7) 0.5340(3) 0.49441(10) 0.0470(4) Uani d . 1 1 . .
O O2 0.15556(7) 0.3414(3) 0.35077(11) 0.0486(4) Uani d . 1 1 . .
O O3 0.24069(7) 0.9621(3) 0.25815(12) 0.0538(5) Uani d D 1 1 . .
O O4 0.37050(8) 0.2080(3) 0.44526(14) 0.0740(6) Uani d . 1 1 . .
O O5 0.11874(8) 0.5541(3) 0.44322(14) 0.0719(6) Uani d . 1 1 . .
C C1 0.30356(10) 0.5610(4) 0.42800(15) 0.0405(6) Uani d . 1 1 A .
C C2 0.25623(10) 0.4259(4) 0.42122(16) 0.0438(6) Uani d . 1 1 . .
H H2 0.2590 0.3050 0.4571 0.053 Uiso calc R 1 1 . .
C C3 0.20481(10) 0.4767(4) 0.35957(16) 0.0421(6) Uani d . 1 1 A .
C C4 0.19981(10) 0.6514(4) 0.30364(16) 0.0436(6) Uani d . 1 1 . .
H H4 0.1646 0.6809 0.2614 0.052 Uiso calc R 1 1 A .
C C5 0.24860(10) 0.7809(4) 0.31228(15) 0.0416(6) Uani d . 1 1 A .
C C6 0.30092(10) 0.7405(4) 0.37541(15) 0.0429(6) Uani d . 1 1 . .
H H6 0.3333 0.8312 0.3822 0.051 Uiso calc R 1 1 A .
C C7 0.38779(10) 0.3519(4) 0.49572(17) 0.0455(6) Uani d . 1 1 . .
C C8 0.11408(10) 0.3985(4) 0.39679(17) 0.0466(6) Uani d . 1 1 . .
C C10 0.44494(5) 0.3584(3) 0.56490(10) 0.0428(6) Uani d G 1 1 . .
C C11 0.47896(7) 0.1775(2) 0.57685(11) 0.0577(7) Uani d G 1 1 . .
H H11 0.4646 0.0550 0.5453 0.069 Uiso calc R 1 1 . .
C C12 0.53426(7) 0.1781(3) 0.63561(13) 0.0669(8) Uani d G 1 1 . .
H H12 0.5572 0.0560 0.6437 0.080 Uiso calc R 1 1 . .
C C13 0.55554(6) 0.3595(3) 0.68242(11) 0.0650(8) Uani d G 1 1 . .
H H13 0.5929 0.3599 0.7221 0.078 Uiso calc R 1 1 . .
C C14 0.52152(7) 0.5404(3) 0.67047(11) 0.0642(8) Uani d G 1 1 . .
H H14 0.5359 0.6629 0.7021 0.077 Uiso calc R 1 1 . .
C C15 0.46622(7) 0.5399(2) 0.61171(12) 0.0551(7) Uani d G 1 1 . .
H H15 0.4433 0.6620 0.6036 0.066 Uiso calc R 1 1 . .
C C16 0.06392(6) 0.2479(2) 0.38278(11) 0.0440(6) Uani d G 1 1 . .
C C17 0.06666(6) 0.0496(3) 0.34617(11) 0.0513(7) Uani d G 1 1 . .
H H17 0.1011 0.0056 0.3296 0.062 Uiso calc R 1 1 . .
C C18 0.01834(8) -0.0835(2) 0.33404(12) 0.0607(8) Uani d G 1 1 . .
H H18 0.0202 -0.2173 0.3093 0.073 Uiso calc R 1 1 . .
C C19 -0.03272(7) -0.0183(3) 0.35852(13) 0.0720(9) Uani d G 1 1 . .
H H19 -0.0653 -0.1081 0.3503 0.086 Uiso calc R 1 1 . .
C C20 -0.03546(6) 0.1800(3) 0.39513(13) 0.0749(9) Uani d G 1 1 . .
H H20 -0.0699 0.2239 0.4116 0.090 Uiso calc R 1 1 . .
C C21 0.01286(7) 0.3131(2) 0.40725(12) 0.0599(8) Uani d G 1 1 . .
H H21 0.0110 0.4469 0.4320 0.072 Uiso calc R 1 1 . .
C C22A 0.26207(19) 1.2348(5) 0.1664(2) 0.0428(10) Uani d P 0.869(3) 1 A 1
C C23A 0.30488(14) 1.3733(8) 0.1497(2) 0.0522(9) Uani d P 0.869(3) 1 A 1
H H23A 0.3449 1.3461 0.1738 0.063 Uiso calc PR 0.869(3) 1 A 1
C C24A 0.2879(2) 1.5522(7) 0.0970(3) 0.0608(9) Uani d P 0.869(3) 1 A 1
H H24A 0.3165 1.6471 0.0872 0.073 Uiso calc PR 0.869(3) 1 A 1
C C25A 0.2294(3) 1.5889(6) 0.0596(3) 0.0573(9) Uani d P 0.869(3) 1 A 1
H H25A 0.2183 1.7081 0.0236 0.069 Uiso calc PR 0.869(3) 1 A 1
C C26A 0.18673(18) 1.4519(10) 0.0746(3) 0.0561(9) Uani d P 0.869(3) 1 A 1
H H26A 0.1470 1.4774 0.0478 0.067 Uiso calc PR 0.869(3) 1 A 1
C C27A 0.20245(17) 1.2766(7) 0.1291(3) 0.0487(10) Uani d P 0.869(3) 1 A 1
H H27A 0.1733 1.1866 0.1408 0.058 Uiso calc PR 0.869(3) 1 A 1
C C9A 0.28368(12) 1.0471(5) 0.22254(18) 0.0428(7) Uani d P 0.869(3) 1 A 1
O O6A 0.33266(8) 0.9761(4) 0.23489(14) 0.0620(7) Uani d P 0.869(3) 1 A 1
C C27B 0.2213(18) 1.234(3) 0.1497(18) 0.0487(10) Uani d PGD 0.131(3) 1 A 2
C C22B 0.2801(15) 1.294(4) 0.1727(14) 0.0428(10) Uani d PG 0.131(3) 1 A 2
H H22B 0.3076 1.2125 0.2132 0.051 Uiso calc PR 0.131(3) 1 A 2
C C23B 0.2982(8) 1.475(5) 0.136(2) 0.0522(9) Uani d PG 0.131(3) 1 A 2
H H23B 0.3379 1.5149 0.1511 0.063 Uiso calc PR 0.131(3) 1 A 2
C C24B 0.2575(17) 1.595(3) 0.0756(18) 0.0608(9) Uani d PG 0.131(3) 1 A 2
H H24B 0.2697 1.7173 0.0506 0.073 Uiso calc PR 0.131(3) 1 A 2
C C25B 0.1986(14) 1.536(4) 0.0526(14) 0.0573(9) Uani d PG 0.131(3) 1 A 2
H H25B 0.1711 1.6174 0.0121 0.069 Uiso calc PR 0.131(3) 1 A 2
C C26B 0.1805(8) 1.355(5) 0.090(2) 0.0561(9) Uani d PG 0.131(3) 1 A 2
H H26B 0.1408 1.3150 0.0742 0.067 Uiso calc PR 0.131(3) 1 A 2
O O6B 0.1535(6) 0.978(2) 0.1877(11) 0.077(5) Uani d P 0.131(3) 1 A 2
C C9B 0.1998(8) 1.048(3) 0.1964(12) 0.059(6) Uiso d PD 0.131(3) 1 A 2
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
O1 0.0475(9) 0.0382(10) 0.0499(10) 0.0048(8) 0.0003(8) 0.0000(8)
O2 0.0472(9) 0.0429(10) 0.0581(10) -0.0123(9) 0.0169(8) -0.0070(9)
O3 0.0517(10) 0.0453(11) 0.0634(11) 0.0024(9) 0.0110(9) 0.0177(9)
O4 0.0591(12) 0.0552(13) 0.0993(16) 0.0053(10) 0.0007(11) -0.0290(12)
O5 0.0679(12) 0.0612(13) 0.0925(15) -0.0157(10) 0.0308(11) -0.0328(12)
C1 0.0396(13) 0.0417(15) 0.0382(13) 0.0046(11) 0.0044(10) -0.0013(12)
C2 0.0507(15) 0.0372(14) 0.0445(13) -0.0026(12) 0.0130(11) 0.0032(12)
C3 0.0413(13) 0.0388(14) 0.0464(14) -0.0048(12) 0.0106(11) -0.0036(12)
C4 0.0388(13) 0.0474(15) 0.0432(14) 0.0005(12) 0.0064(10) -0.0012(13)
C5 0.0421(14) 0.0372(14) 0.0458(14) 0.0020(11) 0.0104(11) 0.0058(12)
C6 0.0429(13) 0.0395(15) 0.0457(13) -0.0029(12) 0.0091(11) 0.0012(12)
C7 0.0461(14) 0.0397(15) 0.0522(15) -0.0017(13) 0.0141(12) -0.0001(13)
C8 0.0441(14) 0.0472(17) 0.0472(14) -0.0001(12) 0.0075(12) -0.0017(13)
C10 0.0406(13) 0.0410(15) 0.0482(14) 0.0024(12) 0.0128(11) 0.0026(12)
C11 0.0518(16) 0.0458(17) 0.0748(19) 0.0068(13) 0.0128(14) 0.0017(15)
C12 0.0577(18) 0.060(2) 0.080(2) 0.0194(16) 0.0112(15) 0.0102(17)
C13 0.0492(16) 0.082(2) 0.0601(17) 0.0045(17) 0.0057(14) 0.0026(17)
C14 0.0582(17) 0.062(2) 0.0667(18) -0.0016(16) 0.0022(14) -0.0092(16)
C15 0.0545(16) 0.0495(17) 0.0576(16) 0.0083(14) 0.0051(13) -0.0015(14)
C16 0.0443(14) 0.0437(16) 0.0423(13) -0.0037(12) 0.0065(11) 0.0015(12)
C17 0.0471(15) 0.0463(17) 0.0584(16) -0.0013(13) 0.0076(12) 0.0043(14)
C18 0.0631(18) 0.0492(18) 0.0644(18) -0.0142(15) 0.0033(15) -0.0014(15)
C19 0.0600(18) 0.080(2) 0.074(2) -0.0318(18) 0.0125(15) 0.0009(18)
C20 0.0544(17) 0.091(3) 0.085(2) -0.0153(18) 0.0282(16) -0.002(2)
C21 0.0575(16) 0.0639(19) 0.0622(17) -0.0062(15) 0.0220(14) -0.0067(15)
C22A 0.052(3) 0.038(2) 0.0378(14) 0.0008(15) 0.0095(14) 0.0018(14)
C23A 0.0564(19) 0.047(2) 0.0508(18) -0.006(2) 0.0064(15) 0.0091(19)
C24A 0.073(3) 0.048(2) 0.059(2) -0.010(2) 0.010(2) 0.0138(18)
C25A 0.075(3) 0.045(2) 0.0516(18) 0.0102(19) 0.015(2) 0.0108(16)
C26A 0.0589(18) 0.058(3) 0.0516(19) 0.0195(19) 0.0123(15) 0.004(2)
C27A 0.049(2) 0.0471(19) 0.052(2) 0.0086(18) 0.0165(19) 0.0037(17)
C9A 0.0424(16) 0.0424(17) 0.0438(16) -0.0015(15) 0.0103(13) 0.0017(14)
O6A 0.0471(13) 0.0663(16) 0.0751(15) 0.0141(11) 0.0191(11) 0.0256(12)
C27B 0.049(2) 0.0471(19) 0.052(2) 0.0086(18) 0.0165(19) 0.0037(17)
C22B 0.052(3) 0.038(2) 0.0378(14) 0.0008(15) 0.0095(14) 0.0018(14)
C23B 0.0564(19) 0.047(2) 0.0508(18) -0.006(2) 0.0064(15) 0.0091(19)
C24B 0.073(3) 0.048(2) 0.059(2) -0.010(2) 0.010(2) 0.0138(18)
C25B 0.075(3) 0.045(2) 0.0516(18) 0.0102(19) 0.015(2) 0.0108(16)
C26B 0.0589(18) 0.058(3) 0.0516(19) 0.0195(19) 0.0123(15) 0.004(2)
O6B 0.042(8) 0.069(11) 0.119(13) -0.003(8) 0.017(8) 0.032(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
4 0 0
1 0 -4
0 4 0
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C7 O1 C1 119.26(19)
C8 O2 C3 116.22(19)
C9B O3 C5 138.3(9)
C9B O3 C9A 91.9(8)
C5 O3 C9A 123.5(2)
C6 C1 C2 122.7(2)
C6 C1 O1 115.2(2)
C2 C1 O1 121.9(2)
C1 C2 C3 117.3(2)
C1 C2 H2 121.4
C3 C2 H2 121.4
C4 C3 C2 122.7(2)
C4 C3 O2 118.6(2)
C2 C3 O2 118.7(2)
C3 C4 C5 117.9(2)
C3 C4 H4 121.1
C5 C4 H4 121.1
C4 C5 C6 121.7(2)
C4 C5 O3 116.1(2)
C6 C5 O3 122.1(2)
C1 C6 C5 117.7(2)
C1 C6 H6 121.2
C5 C6 H6 121.2
O4 C7 O1 122.6(2)
O4 C7 C10 125.5(2)
O1 C7 C10 111.8(2)
O5 C8 O2 122.5(2)
O5 C8 C16 125.2(2)
O2 C8 C16 112.3(2)
C11 C10 C15 120.0
C11 C10 C7 117.32(15)
C15 C10 C7 122.53(15)
C12 C11 C10 120.0
C12 C11 H11 120.0
C10 C11 H11 120.0
C11 C12 C13 120.0
C11 C12 H12 120.0
C13 C12 H12 120.0
C12 C13 C14 120.0
C12 C13 H13 120.0
C14 C13 H13 120.0
C15 C14 C13 120.0
C15 C14 H14 120.0
C13 C14 H14 120.0
C14 C15 C10 120.0
C14 C15 H15 120.0
C10 C15 H15 120.0
C17 C16 C21 120.0
C17 C16 C8 122.56(15)
C21 C16 C8 117.44(15)
C16 C17 C18 120.0
C16 C17 H17 120.0
C18 C17 H17 120.0
C19 C18 C17 120.0
C19 C18 H18 120.0
C17 C18 H18 120.0
C20 C19 C18 120.0
C20 C19 H19 120.0
C18 C19 H19 120.0
C21 C20 C19 120.0
C21 C20 H20 120.0
C19 C20 H20 120.0
C20 C21 C16 120.0
C20 C21 H21 120.0
C16 C21 H21 120.0
C23A C22A C27A 119.3(3)
C23A C22A C9A 116.7(4)
C27A C22A C9A 124.0(4)
C22A C23A C24A 120.0(3)
C22A C23A H23A 120.0
C24A C23A H23A 120.0
C25A C24A C23A 120.0(3)
C25A C24A H24A 120.0
C23A C24A H24A 120.0
C24A C25A C26A 120.6(3)
C24A C25A H25A 119.7
C26A C25A H25A 119.7
C25A C26A C27A 120.3(3)
C25A C26A H26A 119.8
C27A C26A H26A 119.8
C22A C27A C26A 119.7(3)
C22A C27A H27A 120.1
C26A C27A H27A 120.1
O6A C9A O3 123.3(3)
O6A C9A C22A 125.3(3)
O3 C9A C22A 111.4(3)
C22B C27B C26B 120.0
C22B C27B C9B 121(3)
C26B C27B C9B 119(3)
C27B C22B C23B 120.0
C27B C22B H22B 120.0
C23B C22B H22B 120.0
C24B C23B C22B 120.0
C24B C23B H23B 120.0
C22B C23B H23B 120.0
C25B C24B C23B 120.0
C25B C24B H24B 120.0
C23B C24B H24B 120.0
C24B C25B C26B 120.0
C24B C25B H25B 120.0
C26B C25B H25B 120.0
C25B C26B C27B 120.0
C25B C26B H26B 120.0
C27B C26B H26B 120.0
O6B C9B O3 115.8(15)
O6B C9B C27B 131(2)
O3 C9B C27B 114(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C7 1.357(3)
O1 C1 1.404(3)
O2 C8 1.354(3)
O2 C3 1.407(3)
O3 C9B 1.285(15)
O3 C5 1.394(3)
O3 C9A 1.345(3)
O4 C7 1.194(3)
O5 C8 1.198(3)
C1 C6 1.378(3)
C1 C2 1.374(3)
C2 C3 1.368(3)
C2 H2 0.9300
C3 C4 1.378(3)
C4 C5 1.377(3)
C4 H4 0.9300
C5 C6 1.380(3)
C6 H6 0.9300
C7 C10 1.484(3)
C8 C16 1.479(3)
C10 C11 1.3780
C10 C15 1.3781
C11 C12 1.3780
C11 H11 0.9300
C12 C13 1.3780
C12 H12 0.9300
C13 C14 1.3780
C13 H13 0.9300
C14 C15 1.3781
C14 H14 0.9300
C15 H15 0.9300
C16 C17 1.3780
C16 C21 1.3781
C17 C18 1.3780
C17 H17 0.9300
C18 C19 1.3780
C18 H18 0.9300
C19 C20 1.3780
C19 H19 0.9300
C20 C21 1.3780
C20 H20 0.9300
C21 H21 0.9300
C22A C23A 1.388(4)
C22A C27A 1.390(4)
C22A C9A 1.477(4)
C23A C24A 1.386(4)
C23A H23A 0.9300
C24A C25A 1.362(5)
C24A H24A 0.9300
C25A C26A 1.371(5)
C25A H25A 0.9300
C26A C27A 1.378(5)
C26A H26A 0.9300
C27A H27A 0.9300
C9A O6A 1.193(3)
C27B C22B 1.3780
C27B C26B 1.3781
C27B C9B 1.514(16)
C22B C23B 1.3780
C22B H22B 0.9300
C23B C24B 1.3780
C23B H23B 0.9300
C24B C25B 1.3780
C24B H24B 0.9300
C25B C26B 1.3780
C25B H25B 0.9300
C26B H26B 0.9300
O6B C9B 1.14(2)
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
C6 C1 O1 C7 -125.2(2)
C1 O1 C7 O4 -3.8(4)
C1 O1 C7 C10 175.05(18)
O1 C7 C10 C11 175.99(15)
O1 C7 C10 C15 -8.5(2)
C2 C3 O2 C8 98.2(3)
C3 O2 C8 O5 -0.6(3)
C3 O2 C8 C16 179.54(18)
O2 C8 C16 C17 14.8(3)
O2 C8 C16 C21 -164.75(15)
C4 C5 O3 C9A -146.3(2)
C4 C5 O3 C9B -3.1(15)
C5 O3 C9A O6A -0.8(4)
C5 O3 C9A C22A 178.6(2)
C5 O3 C9B O6B 12(3)
C5 O3 C9B C22B -169.2(9)
O3 C9A C22A C23A 160.5(3)
O3 C9A C22A C27A -20.7(4)
O3 C9B C27B C26B -172.6(13)
O3 C9B C27B C22B 2(2)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 347187