#------------------------------------------------------------------------------
#$Date: 2020-11-04 03:28:11 +0200 (Wed, 04 Nov 2020) $
#$Revision: 258715 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/92/1559263.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1559263
loop_
_publ_author_name
'Olivon, Florent'
'Retailleau, Pascal'
'Desrat, Sandy'
'Touboul, David'
'Roussi, Fanny'
'Apel, C\'ecile'
'Litaudon, Marc'
_publ_section_title
;
Isolation of Picrotoxanes from Austrobuxus carunculatus Using
Taxonomy-Based Molecular Networking.
;
_journal_issue 10
_journal_name_full 'Journal of natural products'
_journal_page_first 3069
_journal_page_last 3079
_journal_paper_doi 10.1021/acs.jnatprod.0c00636
_journal_volume 83
_journal_year 2020
_chemical_absolute_configuration unk
_chemical_formula_moiety 'C15 H18 O6'
_chemical_formula_sum 'C15 H18 O6'
_chemical_formula_weight 294.29
_space_group_crystal_system triclinic
_space_group_IT_number 1
_space_group_name_Hall 'P 1'
_space_group_name_H-M_alt 'P 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary other
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 81.9415(19)
_cell_angle_beta 73.770(2)
_cell_angle_gamma 62.844(3)
_cell_formula_units_Z 1
_cell_length_a 6.9816(2)
_cell_length_b 7.0672(16)
_cell_length_c 7.8911(18)
_cell_measurement_reflns_used 9767
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 29.6580
_cell_measurement_theta_min 3.5760
_cell_volume 332.59(11)
_computing_cell_refinement 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution 'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_environment air
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'HPAD Pilatus3R 200K'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_monochromator 'Rigaku MaxFlux mirror'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0491
_diffrn_reflns_av_unetI/netI 0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 17603
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.097
_diffrn_reflns_theta_min 3.772
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'Rigaku (Mo) mm003 X-ray Source'
_exptl_absorpt_coefficient_mu 0.114
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.52374
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.469
_exptl_crystal_description prism
_exptl_crystal_F_000 156
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.23
_refine_diff_density_max 0.217
_refine_diff_density_min -0.186
_refine_diff_density_rms 0.035
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.6(10)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.063
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 199
_refine_ls_number_reflns 2858
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.062
_refine_ls_R_factor_all 0.0341
_refine_ls_R_factor_gt 0.0325
_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^)+(0.0569P)^2^+0.0258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0862
_refine_ls_wR_factor_ref 0.0870
_reflns_Friedel_coverage 0.962
_reflns_Friedel_fraction_full 0.968
_reflns_Friedel_fraction_max 0.957
_reflns_number_gt 2790
_reflns_number_total 2864
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file np0c00636_si_002.cif
_cod_data_source_block FO5-115_1_Mo
_cod_depositor_comments
'Adding full bibliography for 1559261--1559267.cif.'
_cod_database_code 1559263
_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_res_file
;
TITL exp_1_a.res in P1
exp_1_Mo.res
created by SHELXL-2018/3 at 10:32:51 on 02-Apr-2020
REM Old TITL exp_1 in P1
REM SHELXT solution in P1
REM R1 0.310, Rweak 0.256, Alpha 0.000, Orientation as input
REM Flack x = -1.081 ( 3.624 ) from Parsons' quotients
REM Formula found by SHELXT: C9 N4 O6
CELL 0.71073 6.9816 7.06723 7.89106 81.9415 73.770 62.844
ZERR 1 0.0002 0.0016 0.0018 0.0019 0.002 0.003
LATT -1
SFAC C H O
UNIT 15 18 6
L.S. 10
PLAN 20
BOND $H
list 4
fmap 2
acta
OMIT 1 1 1
OMIT -1 -1 -1
OMIT 0 -1 1
OMIT 0 1 1
OMIT -1 -1 0
OMIT -1 -1 1
REM
REM
REM
CONF
SADI O4 H4O O1 H1O
SHEL 999 0.78
EQIV $1 x+1, y, z
EQIV $2 x-1, y+1, z
HTAB O1 O4_$1
HTAB O4 O3_$2
HTAB C14 O1
HTAB C14 O5_$1
TWIN
WGHT 0.056900 0.025800
BASF 0.58554
FVAR 5.99892
O1 3 0.896780 0.656876 0.340206 11.00000 0.03387 0.06241 =
0.02930 -0.00945 -0.00045 -0.03347
H1O 2 0.964377 0.685345 0.395644 11.00000 -1.50000
C1 1 0.599335 0.568625 0.348770 11.00000 0.01897 0.02185 =
0.02096 -0.00301 -0.00564 -0.00785
O2 3 0.866913 0.322217 0.607537 11.00000 0.02527 0.03181 =
0.03609 -0.00312 -0.01313 -0.00328
C2 1 0.698982 0.657614 0.452914 11.00000 0.02298 0.02733 =
0.02363 -0.00426 -0.00416 -0.01347
AFIX 13
H2 2 0.593680 0.807098 0.476269 11.00000 -1.20000
AFIX 0
O3 3 0.800752 0.043543 0.602024 11.00000 0.05443 0.02069 =
0.05536 -0.00256 -0.01766 -0.00183
C3 1 0.729862 0.551599 0.631254 11.00000 0.02350 0.02965 =
0.02720 -0.00502 -0.00923 -0.01021
AFIX 13
H3 2 0.797772 0.612710 0.686881 11.00000 -1.20000
AFIX 0
O4 3 0.201825 0.656856 0.512094 11.00000 0.01736 0.03043 =
0.03821 -0.01367 -0.00692 -0.00327
H4O 2 0.191679 0.761086 0.560139 11.00000 -1.50000
C4 1 0.514265 0.559934 0.755809 11.00000 0.02860 0.02428 =
0.01970 0.00043 -0.00669 -0.01109
AFIX 13
H4 2 0.552964 0.486615 0.864951 11.00000 -1.20000
AFIX 0
O5 3 0.425587 0.360036 0.204966 11.00000 0.03018 0.04357 =
0.03821 -0.01226 -0.01201 -0.01577
C5 1 0.490894 0.402255 0.655473 11.00000 0.02779 0.01977 =
0.02646 -0.00018 -0.00547 -0.01014
AFIX 13
H5 2 0.388874 0.347299 0.730387 11.00000 -1.20000
AFIX 0
C6 1 0.424115 0.497881 0.478681 11.00000 0.01726 0.02154 =
0.02761 -0.00532 -0.00559 -0.00666
O6 3 0.883723 0.384967 0.064209 11.00000 0.03661 0.05310 =
0.02686 -0.01195 0.00236 -0.02006
C7 1 0.493326 0.747590 0.221316 11.00000 0.03945 0.02902 =
0.03228 0.00383 -0.01763 -0.01202
AFIX 137
H7A 2 0.412369 0.707635 0.164640 11.00000 -1.50000
H7AB 2 0.607541 0.771025 0.133695 11.00000 -1.50000
H7AC 2 0.393878 0.875851 0.286031 11.00000 -1.50000
AFIX 0
C8 1 0.314031 0.769018 0.810683 11.00000 0.03003 0.02836 =
0.01838 -0.00485 -0.00290 -0.00966
C9 1 0.320565 0.955357 0.784619 11.00000 0.04979 0.03095 =
0.03244 -0.00926 0.00071 -0.01411
AFIX 93
H9A 2 0.196587 1.077375 0.833022 11.00000 -1.20000
H9AB 2 0.449133 0.964254 0.717905 11.00000 -1.20000
AFIX 0
C10 1 0.107996 0.750051 0.918169 11.00000 0.03406 0.04875 =
0.03082 -0.00983 0.00290 -0.01710
AFIX 137
H10A 2 -0.010514 0.889449 0.947543 11.00000 -1.50000
H10B 2 0.136939 0.670374 1.024595 11.00000 -1.50000
H10C 2 0.066244 0.678240 0.850878 11.00000 -1.50000
AFIX 0
C11 1 0.432434 0.318710 0.386916 11.00000 0.02679 0.02915 =
0.03507 -0.00867 -0.00553 -0.01442
AFIX 13
H11 2 0.374961 0.221097 0.456253 11.00000 -1.20000
AFIX 0
C12 1 0.637754 0.234718 0.249474 11.00000 0.02710 0.02705 =
0.03384 -0.01088 -0.00636 -0.00953
AFIX 13
H12 2 0.718957 0.081801 0.226497 11.00000 -1.20000
AFIX 0
C13 1 0.759680 0.364470 0.238947 11.00000 0.02133 0.02875 =
0.02457 -0.00702 -0.00481 -0.00822
C14 1 1.002121 0.256689 0.194247 11.00000 0.02163 0.04687 =
0.04492 -0.01857 -0.00500 -0.00690
AFIX 23
H14A 2 1.079349 0.312462 0.242393 11.00000 -1.20000
H14B 2 1.073540 0.103439 0.181724 11.00000 -1.20000
AFIX 0
C15 1 0.730709 0.231092 0.618839 11.00000 0.03437 0.02503 =
0.02932 -0.00041 -0.01146 -0.00546
HKLF 4
REM exp_1_a.res in P1
REM wR2 = 0.0870, GooF = S = 1.063, Restrained GooF = 1.062 for all data
REM R1 = 0.0325 for 2790 Fo > 4sig(Fo) and 0.0341 for all 2858 data
REM 199 parameters refined using 4 restraints
END
WGHT 0.0569 0.0258
REM Highest difference peak 0.217, deepest hole -0.186, 1-sigma level 0.035
Q1 1 0.6087 0.5708 0.6928 11.00000 0.05 0.22
Q2 1 0.5075 0.4826 0.7082 11.00000 0.05 0.20
Q3 1 0.6382 0.6114 0.4036 11.00000 0.05 0.19
Q4 1 0.5100 0.5450 0.4212 11.00000 0.05 0.19
Q5 1 0.7157 0.5890 0.5422 11.00000 0.05 0.18
Q6 1 0.4656 0.4618 0.5637 11.00000 0.05 0.18
Q7 1 0.4215 0.4159 0.4375 11.00000 0.05 0.17
Q8 1 0.7019 0.3004 0.2544 11.00000 0.05 0.17
Q9 1 0.6882 0.4605 0.3015 11.00000 0.05 0.16
Q10 1 0.4132 0.6569 0.7719 11.00000 0.05 0.15
Q11 1 0.5533 0.6453 0.2884 11.00000 0.05 0.14
Q12 1 0.5383 0.2639 0.3362 11.00000 0.05 0.14
Q13 1 0.6025 0.3131 0.6197 11.00000 0.05 0.14
Q14 1 0.2170 0.7630 0.8496 11.00000 0.05 0.13
Q15 1 0.6873 0.1380 0.1686 11.00000 0.05 0.13
Q16 1 0.3301 0.5867 0.4865 11.00000 0.05 0.12
Q17 1 0.3177 0.2840 0.4431 11.00000 0.05 0.12
Q18 1 0.3417 0.8422 0.8666 11.00000 0.05 0.11
Q19 1 0.2796 0.8752 0.7387 11.00000 0.05 0.11
Q20 1 0.8546 0.2903 0.2620 11.00000 0.05 0.10
;
_shelx_res_checksum 61781
_shelx_hkl_file
;
-9 -7 -3 31.1561 25.0602 7
-9 -7 -2 81.0200 31.9528 7
-9 -6 -5 14.6224 22.2905 6
-9 -6 -4 63.3008 27.8000 8
-9 -6 -4 55.3716 27.3616 6
-9 -6 -3 153.054 41.3713 7
-9 -6 -3 151.797 39.5701 8
-9 -6 -3 112.129 34.7100 6
-9 -6 -2 94.8898 32.3634 6
-9 -6 -2 69.4431 32.5485 7
-9 -6 -2 93.2617 31.8161 8
-9 -6 -1 1149.66 111.624 7
-9 -6 0 567.000 75.2945 7
-9 -5 -6 799.815 80.6141 5
-9 -5 -6 791.042 82.5331 9
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-9 -5 -4 44.3602 28.2797 6
-9 -5 -4 83.1049 33.6027 8
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-9 -5 -2 75.8960 29.0658 6
-9 -5 -2 71.5127 34.3865 7
-9 -5 -2 61.8642 27.2226 8
-9 -5 -1 297.672 51.6461 8
-9 -5 -1 371.578 62.5368 7
-9 -5 -1 182.980 44.0419 6
-9 -5 0 384.723 59.2865 8
-9 -5 0 552.742 69.8004 6
-9 -4 -6 823.137 84.1019 12
-9 -4 -6 863.963 82.6119 9
-9 -4 -5 308.299 48.8875 9
-9 -4 -5 223.884 41.9391 5
-9 -4 -4 163.722 37.5307 9
-9 -4 -4 129.189 34.3815 5
-9 -4 -3 102.901 32.8614 5
-9 -4 -3 126.479 37.3107 6
-9 -4 -3 83.7650 32.2257 8
-9 -4 -2 219.220 46.1947 6
-9 -4 -2 241.101 45.9431 5
-9 -4 -2 191.044 44.6035 8
-9 -4 -1 87.1263 32.4991 6
-9 -4 -1 129.533 36.8593 8
-9 -4 0 134.810 37.2383 8
-9 -4 0 131.264 40.3412 6
-9 -3 -6 865.106 83.1214 9
-9 -3 -5 303.484 48.5923 9
-9 -3 -5 313.395 56.2594 2
-9 -3 -5 279.071 43.8341 5
-9 -3 -4 150.429 36.8212 9
-9 -3 -4 135.717 38.1583 2
-9 -3 -4 174.431 36.6817 5
-9 -3 -3 168.609 37.6580 5
-9 -3 -2 13.2420 21.2884 2
-9 -3 -2 25.5359 18.3652 5
-9 -2 -5 130.849 35.8490 9
-9 -2 -5 192.890 43.1434 2
-9 -2 -4 34.9625 24.6756 2
-9 -2 -4 48.9207 24.1296 9
-9 -2 -4 52.0895 25.0125 2
-9 -2 -4 30.7847 22.1900 5
-9 -2 -3 102.981 30.4225 2
-9 -2 -3 79.9263 28.7039 5
-9 -2 -2 190.889 41.1388 5
-9 -2 -2 161.098 41.6428 2
-9 -1 -2 726.189 79.2356 2
-8 -8 -5 297.618 55.8965 7
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-8 -8 -3 57.2404 25.1548 7
-8 -7 -7 841.785 84.9052 12
-8 -7 -6 262.158 45.4513 12
-8 -7 -5 209.447 41.3728 12
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-8 -7 -4 292.584 53.1942 7
-8 -7 -4 364.298 66.8660 10
-8 -7 -4 312.382 47.8391 6
-8 -7 -4 429.420 60.5785 12
-8 -7 -3 401.502 60.8759 7
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-8 -7 -3 467.109 64.2686 4
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-8 -7 -2 117.223 34.8690 4
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-8 -7 -1 317.929 53.1942 4
-8 -7 -1 308.562 57.5948 10
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-8 -7 1 194.118 44.6844 11
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-8 -6 -6 263.249 44.8083 12
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-8 -6 -5 86.1266 33.2795 10
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-8 -6 -2 297.464 45.8422 8
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-8 -6 0 1628.52 119.799 6
-8 -6 0 1691.08 136.524 3
-8 -6 0 1595.15 116.132 8
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-8 -6 0 1738.93 147.189 10
-8 -6 1 5.95614 21.8230 7
-8 -6 1 26.1603 24.8649 3
-8 -6 1 21.3053 21.6504 11
-8 -6 2 124.234 36.2044 3
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-8 -5 -7 71.2072 24.8438 9
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-8 -5 -7 76.9158 29.2158 3
-8 -5 -6 333.122 61.0525 7
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-8 -5 -6 307.516 60.5887 2
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-8 -5 -6 335.305 50.0001 12
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-8 -5 -6 411.691 58.2549 4
-8 -5 -5 1234.92 98.4863 9
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-8 -5 -5 1116.62 95.1127 5
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-8 -5 -5 1148.08 100.356 4
-8 -5 -5 1103.13 93.7023 12
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-8 -5 -4 508.151 75.6904 10
-8 -5 -4 481.896 68.0249 8
-8 -5 -4 633.737 79.7295 7
-8 -5 -4 720.154 74.9950 12
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-8 -5 -4 694.847 76.4698 6
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-8 -5 -3 349.529 53.3908 3
-8 -5 -2 415.680 57.8319 5
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7 6 6 385.607 56.2044 6
7 6 7 22.1413 22.5121 3
7 6 7 13.8083 24.3141 1
7 6 7 58.8636 29.9130 8
7 6 7 24.2458 23.2407 4
7 6 7 15.0903 24.2564 7
7 6 7 18.8543 22.1364 12
7 6 7 13.4440 19.3373 6
7 6 8 22.6488 23.0299 3
7 7 -3 554.925 65.5006 3
7 7 -2 44.6672 24.1460 3
7 7 -2 68.6211 26.9598 9
7 7 -2 32.3221 18.8682 4
7 7 -1 240.227 42.7196 3
7 7 -1 183.309 40.3581 9
7 7 -1 212.673 37.9620 4
7 7 -1 291.705 49.0044 12
7 7 0 35.4011 23.9905 3
7 7 0-6.46627 18.5998 9
7 7 0 47.5400 24.0129 4
7 7 0 19.4014 21.8064 12
7 7 1 110.080 32.3853 3
7 7 1 32.4850 13.9947 1
7 7 1 53.1148 24.4568 9
7 7 1 54.4800 16.3442 8
7 7 1 86.4345 19.5918 1
7 7 1 45.7488 18.3510 7
7 7 1 90.8994 28.9732 4
7 7 1 65.6645 17.3302 6
7 7 2 172.164 39.7861 3
7 7 2 116.636 24.5896 8
7 7 2 100.534 22.9481 1
7 7 2 140.747 28.1236 7
7 7 2 176.324 37.4683 4
7 7 2 121.131 23.2715 6
7 7 2 91.9278 29.5956 12
7 7 3 168.425 39.8469 9
7 7 3 184.767 32.0384 8
7 7 3 147.518 29.0329 1
7 7 3 222.876 43.3725 4
7 7 3 220.293 37.5599 7
7 7 3 201.035 42.7088 12
7 7 3 147.822 28.4093 6
7 7 4 56.4197 26.9412 3
7 7 4 35.7212 23.1080 9
7 7 4 94.6657 27.7527 1
7 7 4 59.7531 22.5546 8
7 7 4 42.6279 26.1613 4
7 7 4 51.7977 22.4865 7
7 7 4 61.6745 27.9753 12
7 7 4 80.3543 21.3783 6
7 7 5 179.071 43.5084 3
7 7 5 141.213 33.9193 1
7 7 5 184.822 39.3548 8
7 7 5 200.105 40.3410 7
7 7 5 125.567 34.7803 12
7 7 5 174.733 34.3854 6
7 7 6 109.239 36.6983 3
7 7 6 86.6422 30.6012 1
7 7 6 209.125 42.0465 8
7 7 6 73.3295 31.4711 7
7 7 6 141.058 36.9053 12
7 7 6 127.737 33.7849 6
7 7 7 73.0078 31.6938 8
7 7 7 97.7236 33.4752 12
7 7 7 83.8769 31.6620 6
7 8 -1 238.450 46.5052 3
7 8 -1 267.525 43.1645 4
7 8 0 64.6456 27.1235 3
7 8 0 22.6120 18.2302 4
7 8 1 87.2987 34.1920 3
7 8 1 36.4648 24.0303 4
7 8 2 21.1424 23.7785 3
7 8 2 42.5853 19.3089 7
7 8 2 19.7172 18.9275 4
7 8 3 577.136 58.7032 1
7 8 3 562.211 59.1249 7
7 8 3 515.918 70.6411 4
7 8 3 509.749 72.8433 12
7 8 4 291.765 41.9824 8
7 8 4 326.614 46.9386 1
7 8 4 321.935 47.2617 7
7 8 5 283.457 45.2410 8
7 8 5 268.111 46.7432 1
7 8 5 218.177 49.8830 12
7 8 6 577.688 71.1907 8
7 8 6 552.764 70.9057 7
8 -1 2 507.634 64.6829 5
8 -1 4 1107.95 99.6137 9
8 0 0 110.030 35.2785 1
8 0 1 193.975 41.2881 5
8 0 1 163.202 40.9301 1
8 0 2 293.957 48.7407 5
8 0 2 291.460 49.9482 9
8 0 3 985.459 85.7829 5
8 0 3 903.059 88.5526 9
8 0 4 254.902 46.1318 9
8 0 5 105.059 28.1284 9
8 1 -2 626.216 69.5988 1
8 1 -1 380.926 55.3456 1
8 1 0 577.217 72.3459 5
8 1 0 761.209 85.2020 8
8 1 0 817.805 80.7078 1
8 1 1 155.112 37.5096 5
8 1 1 173.090 39.8241 9
8 1 1 197.557 45.0645 8
8 1 1 278.503 47.0438 1
8 1 1 214.679 45.6807 6
8 1 2 18.0399 21.2185 3
8 1 2 28.9863 22.0905 9
8 1 2 37.6882 22.6048 5
8 1 2 42.7979 25.1494 8
8 1 2 18.6855 20.0694 4
8 1 2 77.8787 28.7793 1
8 1 2 53.4543 24.9257 12
8 1 2 28.6786 24.2063 6
8 1 3 120.947 32.2875 3
8 1 3 67.4254 25.3488 9
8 1 3 109.675 29.4938 5
8 1 3 123.794 35.8068 8
8 1 3 124.740 35.0402 4
8 1 3 110.659 35.4840 7
8 1 3 129.394 34.1447 12
8 1 3 116.243 34.9550 6
8 1 3 102.112 33.5179 1
8 1 4 248.682 50.2002 1
8 1 4 194.790 41.4218 3
8 1 4 180.337 37.7828 9
8 1 4 203.029 35.9156 5
8 1 4 172.839 44.0040 8
8 1 4 163.412 37.6401 4
8 1 4 142.615 41.2249 7
8 1 4 204.767 41.1867 12
8 1 4 202.525 45.2284 6
8 1 5 441.841 61.1860 3
8 1 5 531.264 63.4016 9
8 1 5 487.442 65.1349 4
8 1 5 487.089 62.8427 12
8 1 6 647.613 76.0691 3
8 1 6 635.816 75.6871 4
8 1 6 737.823 77.3464 12
8 1 7 135.379 36.0718 3
8 1 7 184.644 38.7886 12
8 2 -1 165.502 39.3291 3
8 2 -1 205.893 35.7013 1
8 2 -1 209.454 42.5907 8
8 2 -1 151.162 38.7050 4
8 2 0 5.70750 17.4085 3
8 2 0 23.9494 21.9412 5
8 2 0 29.5270 22.4573 9
8 2 0 25.2824 17.8080 1
8 2 0 6.27439 19.1347 8
8 2 0 40.8449 23.7203 4
8 2 0 6.51350 18.7284 6
8 2 0 11.7108 18.8233 12
8 2 1-5.72669 15.3931 3
8 2 1 11.5633 19.4806 9
8 2 1 11.4117 15.3370 5
8 2 1 6.30796 18.1255 8
8 2 1-5.88123 21.5420 4
8 2 1 21.5676 16.4334 1
8 2 1 6.44341 16.0346 6
8 2 2 507.060 62.4017 9
8 2 2 389.949 55.5031 5
8 2 2 495.437 65.0914 8
8 2 2 549.408 69.9473 7
8 2 2 512.749 62.9354 12
8 2 2 471.643 63.6608 6
8 2 2 514.216 62.9019 1
8 2 3 166.985 38.1544 1
8 2 3 117.404 33.7218 3
8 2 3 95.6113 29.7237 9
8 2 3 127.202 30.7104 5
8 2 3 206.119 43.1234 8
8 2 3 157.381 35.8125 4
8 2 3 79.1589 27.5794 12
8 2 3 204.820 42.3279 6
8 2 4 41.7354 22.7311 3
8 2 4 27.6336 20.3201 9
8 2 4 37.7465 19.8417 5
8 2 4 19.7057 23.1825 1
8 2 4 34.8455 24.5880 8
8 2 4 49.4820 24.3992 4
8 2 4 61.9908 25.0166 12
8 2 4 55.1045 28.0446 6
8 2 5 152.349 36.3382 3
8 2 5 124.683 31.5585 9
8 2 5 250.378 51.8262 8
8 2 5 152.897 37.3637 4
8 2 5 222.555 47.9787 1
8 2 5 177.847 41.2205 7
8 2 5 146.175 35.5342 12
8 2 5 196.260 44.3188 6
8 2 6 98.8258 32.8095 3
8 2 6 72.8389 25.6121 9
8 2 6 65.0071 28.2572 4
8 2 6 100.279 31.7232 12
8 2 7 297.722 50.4691 3
8 2 7 273.797 50.1211 4
8 2 7 284.528 46.6191 12
8 3 -2 27.7744 22.6347 3
8 3 -2 48.6761 24.0079 4
8 3 -1 655.657 73.2907 3
8 3 -1 695.021 78.1098 5
8 3 -1 639.828 73.7538 9
8 3 -1 766.831 76.5715 8
8 3 -1 696.468 73.9926 4
8 3 -1 680.862 63.4908 1
8 3 -1 734.528 78.1408 12
8 3 0 100.477 30.3145 3
8 3 0 101.773 32.4687 5
8 3 0 128.497 31.8926 8
8 3 0 85.7002 24.6178 1
8 3 0 61.1494 23.6809 4
8 3 0 123.743 33.6065 6
8 3 0 109.317 32.3026 12
8 3 1 62.0013 27.5351 3
8 3 1 52.3088 22.1850 9
8 3 1 52.0522 22.8454 5
8 3 1 39.5244 25.7318 8
8 3 1 73.7735 27.7216 4
8 3 1 32.8879 18.5965 1
8 3 1 29.0873 19.7055 6
8 3 2 5.17176 15.7816 1
8 3 2 34.5939 22.6981 9
8 3 2 5.54998 16.9328 5
8 3 2 40.6118 22.0663 8
8 3 2 11.6842 17.8221 4
8 3 2 31.4545 23.9246 7
8 3 2 22.4433 18.0420 12
8 3 2 17.5341 19.7081 6
8 3 3 234.256 44.9197 3
8 3 3 270.758 46.8820 9
8 3 3 228.153 42.8171 5
8 3 3 396.168 53.7375 1
8 3 3 414.019 56.2240 8
8 3 3 356.289 54.7002 7
8 3 3 262.704 45.9537 12
8 3 3 307.605 50.4221 6
8 3 4 120.200 32.6852 3
8 3 4 172.512 37.7736 9
8 3 4 278.480 49.4204 8
8 3 4 143.657 36.7447 4
8 3 4 195.998 42.4968 7
8 3 4 215.207 43.5386 1
8 3 4 162.022 35.4082 12
8 3 4 196.053 41.8824 6
8 3 5 199.064 43.1004 1
8 3 5 135.424 35.3892 3
8 3 5 131.098 34.3533 9
8 3 5 146.009 41.6694 8
8 3 5 155.212 37.7008 4
8 3 5 112.062 32.3196 12
8 3 5 135.487 38.2225 6
8 3 6 497.288 65.8864 3
8 3 6 431.116 57.5542 9
8 3 6 642.063 77.4615 1
8 3 6 659.526 80.3145 8
8 3 6 452.424 64.1432 4
8 3 6 481.304 62.1886 12
8 3 6 588.128 74.1750 6
8 3 7 409.434 61.1740 3
8 3 7 361.934 51.6084 9
8 3 7 476.025 66.0195 4
8 3 7 481.312 60.6620 12
8 3 8 51.5315 27.8582 3
8 4 -3 115.441 31.8398 3
8 4 -3 71.2162 25.6271 4
8 4 -2 93.5161 28.8518 3
8 4 -2 108.856 31.0366 4
8 4 -1 1052.37 101.858 5
8 4 -1 1205.84 105.637 9
8 4 -1 1204.20 97.2501 8
8 4 -1 1354.71 103.514 4
8 4 -1 1058.77 100.233 12
8 4 -1 1044.25 97.3961 3
8 4 0 16.7267 21.9436 3
8 4 0 30.5007 22.3501 5
8 4 0 9.94317 14.2962 8
8 4 0 10.8961 17.5107 4
8 4 0 21.5618 16.3360 1
8 4 0 21.3364 18.7794 6
8 4 0-5.79553 15.5871 12
8 4 1 143.251 28.8911 1
8 4 1 226.706 41.4024 3
8 4 1 137.988 34.2210 9
8 4 1 142.981 33.4505 5
8 4 1 166.780 34.8787 8
8 4 1 208.653 39.5770 4
8 4 1 172.097 38.5105 7
8 4 1 184.341 35.8845 6
8 4 2 404.215 56.7209 9
8 4 2 300.802 49.6290 5
8 4 2 405.180 50.0346 1
8 4 2 346.756 49.8087 8
8 4 2 486.128 59.8306 4
8 4 2 404.909 55.9504 7
8 4 2 329.878 51.5525 12
8 4 2 381.835 53.8482 6
8 4 3 1364.78 107.241 1
8 4 3 1104.50 107.829 9
8 4 3 1539.51 114.615 8
8 4 3 1444.96 115.163 7
8 4 3 1507.53 112.356 6
8 4 3 1230.18 107.373 12
8 4 3 1191.53 109.470 3
8 4 4 135.193 35.8516 3
8 4 4 245.275 44.0313 1
8 4 4 79.5949 27.8093 9
8 4 4 199.235 40.2261 8
8 4 4 141.000 36.1936 4
8 4 4 154.646 37.5419 7
8 4 4 125.945 31.3894 12
8 4 4 116.856 34.1417 6
8 4 5 444.676 62.0552 3
8 4 5 570.888 67.7119 9
8 4 5 447.793 63.7244 8
8 4 5 464.393 63.8915 4
8 4 5 530.780 68.9281 7
8 4 5 482.978 64.8226 1
8 4 5 357.972 54.2897 12
8 4 5 481.822 63.9217 6
8 4 6 637.694 77.6124 3
8 4 6 655.669 74.3654 9
8 4 6 734.264 84.4605 8
8 4 6 768.959 86.6388 1
8 4 6 630.585 78.1821 4
8 4 6 714.320 84.2449 7
8 4 6 842.590 88.2566 6
8 4 6 657.012 74.7580 12
8 4 7 560.503 70.3216 3
8 4 7 373.083 56.0997 9
8 4 7 427.822 65.1564 4
8 4 7 521.387 63.7483 12
8 4 8 6.87772 20.9620 3
8 5 -2 466.036 60.6557 3
8 5 -2 528.726 60.1939 4
8 5 -1 184.954 38.0939 3
8 5 -1 150.497 37.3677 9
8 5 -1 170.744 31.7286 8
8 5 -1 158.040 36.2955 4
8 5 -1 177.058 39.4650 12
8 5 0 215.890 41.4946 3
8 5 0 206.428 43.2836 9
8 5 0 157.902 37.0642 5
8 5 0 140.581 31.1861 8
8 5 0 185.486 38.3299 4
8 5 0 149.065 33.9705 6
8 5 0 150.046 36.3357 12
8 5 1 569.310 68.4285 3
8 5 1 607.030 71.1870 5
8 5 1 664.205 64.3928 8
8 5 1 639.953 71.1228 4
8 5 1 495.327 61.5310 7
8 5 1 637.715 64.4053 6
8 5 1 566.760 55.1005 1
8 5 2 244.773 44.7931 3
8 5 2 262.711 48.6883 9
8 5 2 200.147 37.8535 8
8 5 2 312.494 49.0249 4
8 5 2 269.194 44.4279 7
8 5 2 399.676 46.3134 1
8 5 2 337.227 45.3811 6
8 5 2 332.645 51.4137 12
8 5 3 284.913 49.9785 9
8 5 3 356.323 49.5380 1
8 5 3 386.581 51.4264 8
8 5 3 309.950 50.9845 4
8 5 3 329.069 50.7717 7
8 5 3 280.977 49.5412 12
8 5 3 287.146 44.8512 6
8 5 4 508.964 68.0974 3
8 5 4 735.644 73.8585 1
8 5 4 412.288 63.3349 9
8 5 4 566.272 67.0975 8
8 5 4 778.172 79.0346 7
8 5 4 605.225 70.2155 12
8 5 4 610.234 67.6674 6
8 5 5 1119.16 103.908 9
8 5 5 1493.13 114.669 1
8 5 5 1187.15 104.436 8
8 5 5 938.098 99.5814 4
8 5 5 1202.68 106.830 7
8 5 5 1263.98 104.525 6
8 5 5 971.089 97.3000 12
8 5 5 977.234 100.568 3
8 5 6 330.867 55.8647 3
8 5 6 325.552 53.6829 9
8 5 6 389.520 60.4320 8
8 5 6 375.463 60.7469 4
8 5 6 457.771 63.9973 1
8 5 6 372.110 60.5227 7
8 5 6 261.674 48.7856 12
8 5 6 415.281 60.1657 6
8 5 7 94.6614 32.4079 3
8 5 7 69.3262 28.8176 9
8 5 7 62.8230 24.1014 12
8 6 -2 74.8761 27.1681 3
8 6 -2 127.389 31.3651 4
8 6 -1 40.9580 23.0669 3
8 6 -1 26.6266 19.5599 4
8 6 0 1922.57 141.913 9
8 6 0 1713.91 113.759 8
8 6 0 1778.17 129.221 4
8 6 0 1616.31 131.752 12
8 6 0 1516.42 126.830 3
8 6 1 330.956 51.7784 3
8 6 1 386.396 40.9501 1
8 6 1 292.263 40.6921 8
8 6 1 300.315 49.9029 4
8 6 1 302.874 45.3583 7
8 6 1 272.326 40.7139 6
8 6 2 291.052 48.9365 3
8 6 2 272.102 39.3813 1
8 6 2 204.682 45.2112 9
8 6 2 241.268 38.9990 8
8 6 2 255.907 45.7440 4
8 6 2 279.173 43.4489 7
8 6 2 247.697 38.0492 6
8 6 2 185.016 40.9476 12
8 6 3 666.744 66.4219 1
8 6 3 613.898 77.8276 9
8 6 3 641.861 65.2674 8
8 6 3 722.656 78.6238 4
8 6 3 587.999 67.0256 7
8 6 3 574.396 61.5717 6
8 6 3 573.523 71.7981 12
8 6 4 1234.59 118.598 9
8 6 4 1597.66 118.912 1
8 6 4 1535.42 114.236 8
8 6 4 1622.94 129.575 4
8 6 4 1454.12 116.972 7
8 6 4 1665.40 115.338 6
8 6 4 1328.04 119.666 12
8 6 4 1113.31 113.487 3
8 6 5 130.326 37.8940 3
8 6 5 121.259 35.9099 9
8 6 5 143.235 34.7225 8
8 6 5 116.966 34.0938 7
8 6 5 101.245 31.8864 12
8 6 5 116.505 31.8446 6
8 6 6 120.457 36.6052 9
8 6 6 255.981 47.9307 8
8 6 6 271.846 53.3165 7
8 6 6 205.027 43.9091 12
8 6 6 349.088 52.7556 6
8 6 7 582.251 74.6906 12
8 7 -1 241.391 43.4583 4
8 7 0 556.727 65.8985 4
8 7 1 323.137 45.0726 7
8 7 1 313.004 51.9038 4
8 7 2 138.648 28.3615 8
8 7 2 124.679 34.5595 4
8 7 2 151.047 32.3034 7
8 7 3 434.834 51.7922 1
8 7 3 475.918 53.3666 8
8 7 3 566.588 59.8196 1
8 7 3 541.042 71.7161 4
8 7 3 555.662 62.3009 7
8 7 3 500.125 54.8664 6
8 7 3 470.908 66.2901 12
8 7 4 340.523 47.4392 1
8 7 4 333.485 48.5980 8
8 7 4 371.987 53.6283 7
8 7 4 326.180 56.7607 12
8 7 4 346.873 46.8616 6
8 7 5 174.984 38.8195 1
8 7 5 182.300 39.5896 8
8 7 5 158.142 37.7211 7
8 7 5 148.403 39.9288 12
8 7 5 195.902 37.4716 6
8 7 6 313.177 53.0287 8
8 7 6 247.211 52.1959 12
8 7 6 322.531 50.5368 6
8 8 3 44.8906 21.5915 7
8 8 4 639.167 69.7921 7
8 8 5 362.492 54.6566 1
8 8 5 393.443 58.0458 7
9 2 1 275.112 50.3370 1
9 2 2 150.894 36.8238 5
9 2 2 166.542 40.0959 1
9 2 3 100.690 29.8228 5
9 2 4 27.3202 17.5954 5
9 2 5 175.905 38.0464 9
9 3 1 250.973 42.9887 1
9 3 2 12.7431 20.4902 5
9 3 2 29.6823 20.0239 1
9 3 3 186.985 41.5927 1
9 3 3 152.094 36.8159 5
9 3 4 66.3224 28.8534 9
9 3 4 118.277 34.8471 1
9 3 5 241.785 48.1866 9
9 3 6 771.787 83.8581 9
9 4 -1 358.321 54.6268 8
9 4 0 136.738 34.1848 8
9 4 1 72.3935 29.5068 8
9 4 1 52.1237 20.5895 1
9 4 1 56.8614 25.8051 6
9 4 2 270.288 42.9356 1
9 4 2 186.433 40.7266 8
9 4 2 228.736 45.4135 6
9 4 3 129.873 34.3450 1
9 4 3 110.496 34.7260 8
9 4 3 116.869 34.6892 6
9 4 4 117.609 35.3936 9
9 4 4 241.697 49.7859 8
9 4 4 227.344 45.9749 1
9 4 4 196.551 43.7730 6
9 4 5 225.944 46.7305 9
9 4 6 824.772 89.7907 9
9 5 0 472.473 58.7247 8
9 5 1 401.360 52.6003 8
9 5 1 230.219 45.8339 6
9 5 2 104.812 28.4334 1
9 5 2 67.5694 25.1746 8
9 5 2 64.5542 28.0387 7
9 5 2 75.3969 28.4688 6
9 5 3 107.364 33.0118 8
9 5 3 125.340 31.2269 1
9 5 3 147.332 38.2071 7
9 5 3 83.3213 28.1546 6
9 5 4 98.2618 31.4711 1
9 5 4 57.7405 27.1934 8
9 5 4 156.417 38.8851 6
9 5 5 82.1118 31.3049 1
9 6 2 117.244 29.7151 8
9 6 2 109.104 32.3813 7
9 6 2 105.440 30.7036 6
9 6 3 142.296 34.4190 8
9 6 3 164.678 39.6574 7
9 6 3 103.426 30.4594 6
9 6 3 177.547 35.5320 1
9 6 4 53.7310 25.1254 8
9 6 4 35.2455 24.7259 1
9 6 4 80.5925 28.1521 6
9 6 5 13.3607 24.5010 1
9 6 5 43.4448 24.4513 6
9 7 2 79.8807 29.2030 7
9 7 3 84.1584 28.8917 7
0 0 0 0.00 0.00 0
TITL exp_1 in P1
REM P1 (#1 in standard setting)
CELL 0.71073 6.981622 7.067225 7.891063 81.9415 73.7703 62.8445
ZERR 2.00 0.000219 0.000161 0.000176 0.0019 0.0023 0.0027
LATT -1
SFAC C H N O
UNIT 22.00 20.00 2.00 2.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 80873
loop_
_space_group_symop_operation_xyz
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.8968(3) 0.6569(3) 0.3402(2) 0.0376(4) Uani 1 1 d D . . . .
H1O H 0.964(6) 0.685(6) 0.396(5) 0.056 Uiso 1 1 d D U . . .
C1 C 0.5993(3) 0.5686(3) 0.3488(2) 0.0206(4) Uani 1 1 d . . . . .
O2 O 0.8669(2) 0.3222(3) 0.6075(2) 0.0332(4) Uani 1 1 d . . . . .
C2 C 0.6990(3) 0.6576(3) 0.4529(3) 0.0236(4) Uani 1 1 d . . . . .
H2 H 0.593680 0.807098 0.476269 0.028 Uiso 1 1 calc R U . . .
O3 O 0.8008(3) 0.0435(3) 0.6020(3) 0.0481(5) Uani 1 1 d . . . . .
C3 C 0.7299(3) 0.5516(3) 0.6313(3) 0.0262(4) Uani 1 1 d . . . . .
H3 H 0.797772 0.612710 0.686881 0.031 Uiso 1 1 calc R U . . .
O4 O 0.2018(2) 0.6569(3) 0.5121(2) 0.0301(3) Uani 1 1 d D . . . .
H4O H 0.192(6) 0.761(5) 0.560(5) 0.045 Uiso 1 1 d D U . . .
C4 C 0.5143(3) 0.5599(3) 0.7558(2) 0.0243(4) Uani 1 1 d . . . . .
H4 H 0.552964 0.486615 0.864951 0.029 Uiso 1 1 calc R U . . .
O5 O 0.4256(3) 0.3600(3) 0.2050(2) 0.0354(4) Uani 1 1 d . . . . .
C5 C 0.4909(3) 0.4023(3) 0.6555(3) 0.0251(4) Uani 1 1 d . . . . .
H5 H 0.388874 0.347299 0.730387 0.030 Uiso 1 1 calc R U . . .
C6 C 0.4241(3) 0.4979(3) 0.4787(3) 0.0223(4) Uani 1 1 d . . . . .
O6 O 0.8837(3) 0.3850(3) 0.0642(2) 0.0397(4) Uani 1 1 d . . . . .
C7 C 0.4933(4) 0.7476(4) 0.2213(3) 0.0333(5) Uani 1 1 d . . . . .
H7A H 0.412369 0.707635 0.164640 0.050 Uiso 1 1 calc R U . . .
H7AB H 0.607541 0.771025 0.133695 0.050 Uiso 1 1 calc R U . . .
H7AC H 0.393878 0.875851 0.286031 0.050 Uiso 1 1 calc R U . . .
C8 C 0.3140(3) 0.7690(3) 0.8107(3) 0.0270(4) Uani 1 1 d . . . . .
C9 C 0.3206(5) 0.9554(4) 0.7846(3) 0.0406(6) Uani 1 1 d . . . . .
H9A H 0.196587 1.077375 0.833022 0.049 Uiso 1 1 calc R U . . .
H9AB H 0.449133 0.964254 0.717905 0.049 Uiso 1 1 calc R U . . .
C10 C 0.1080(4) 0.7501(5) 0.9182(3) 0.0397(6) Uani 1 1 d . . . . .
H10A H -0.010514 0.889449 0.947543 0.060 Uiso 1 1 calc R U . . .
H10B H 0.136939 0.670374 1.024595 0.060 Uiso 1 1 calc R U . . .
H10C H 0.066244 0.678240 0.850878 0.060 Uiso 1 1 calc R U . . .
C11 C 0.4324(3) 0.3187(3) 0.3869(3) 0.0290(4) Uani 1 1 d . . . . .
H11 H 0.374961 0.221097 0.456253 0.035 Uiso 1 1 calc R U . . .
C12 C 0.6378(4) 0.2347(3) 0.2495(3) 0.0294(4) Uani 1 1 d . . . . .
H12 H 0.718957 0.081801 0.226497 0.035 Uiso 1 1 calc R U . . .
C13 C 0.7597(3) 0.3645(3) 0.2389(3) 0.0254(4) Uani 1 1 d . . . . .
C14 C 1.0021(4) 0.2567(4) 0.1942(4) 0.0398(6) Uani 1 1 d . . . . .
H14A H 1.079349 0.312462 0.242393 0.048 Uiso 1 1 calc R U . . .
H14B H 1.073540 0.103439 0.181724 0.048 Uiso 1 1 calc R U . . .
C15 C 0.7307(4) 0.2311(4) 0.6188(3) 0.0318(5) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0339(9) 0.0624(12) 0.0293(8) -0.0094(8) -0.0004(7) -0.0335(9)
C1 0.0190(8) 0.0218(9) 0.0210(8) -0.0030(7) -0.0056(7) -0.0079(7)
O2 0.0253(7) 0.0318(8) 0.0361(8) -0.0031(6) -0.0131(6) -0.0033(6)
C2 0.0230(9) 0.0273(10) 0.0236(9) -0.0043(8) -0.0042(7) -0.0135(8)
O3 0.0544(12) 0.0207(8) 0.0554(11) -0.0026(8) -0.0177(9) -0.0018(7)
C3 0.0235(9) 0.0297(10) 0.0272(10) -0.0050(8) -0.0092(8) -0.0102(8)
O4 0.0174(7) 0.0304(8) 0.0382(8) -0.0137(7) -0.0069(6) -0.0033(6)
C4 0.0286(10) 0.0243(10) 0.0197(9) 0.0004(7) -0.0067(7) -0.0111(8)
O5 0.0302(8) 0.0436(9) 0.0382(9) -0.0123(7) -0.0120(7) -0.0158(7)
C5 0.0278(9) 0.0198(9) 0.0265(10) -0.0002(7) -0.0055(7) -0.0101(7)
C6 0.0173(9) 0.0215(9) 0.0276(9) -0.0053(7) -0.0056(7) -0.0067(7)
O6 0.0366(9) 0.0531(10) 0.0269(8) -0.0119(7) 0.0024(6) -0.0201(8)
C7 0.0395(12) 0.0290(10) 0.0323(11) 0.0038(9) -0.0176(9) -0.0120(9)
C8 0.0300(10) 0.0284(10) 0.0184(8) -0.0048(7) -0.0029(7) -0.0097(8)
C9 0.0498(14) 0.0310(12) 0.0324(11) -0.0093(10) 0.0007(10) -0.0141(11)
C10 0.0341(12) 0.0487(15) 0.0308(11) -0.0098(10) 0.0029(9) -0.0171(11)
C11 0.0268(10) 0.0291(11) 0.0351(11) -0.0087(8) -0.0055(8) -0.0144(8)
C12 0.0271(10) 0.0270(10) 0.0338(11) -0.0109(8) -0.0064(8) -0.0095(8)
C13 0.0213(9) 0.0288(10) 0.0246(9) -0.0070(8) -0.0048(7) -0.0082(8)
C14 0.0216(10) 0.0469(13) 0.0449(13) -0.0186(11) -0.0050(9) -0.0069(10)
C15 0.0344(11) 0.0250(10) 0.0293(11) -0.0004(8) -0.0115(8) -0.0055(9)
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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O1 H1O 111(3) . . ?
C7 C1 C2 106.16(17) . . ?
C7 C1 C13 107.87(16) . . ?
C2 C1 C13 117.89(15) . . ?
C7 C1 C6 111.96(16) . . ?
C2 C1 C6 110.97(15) . . ?
C13 C1 C6 102.08(14) . . ?
C15 O2 C3 107.96(16) . . ?
O1 C2 C3 112.96(16) . . ?
O1 C2 C1 108.16(16) . . ?
C3 C2 C1 115.54(16) . . ?
O1 C2 H2 106.5 . . ?
C3 C2 H2 106.5 . . ?
C1 C2 H2 106.5 . . ?
O2 C3 C2 109.27(16) . . ?
O2 C3 C4 101.93(17) . . ?
C2 C3 C4 113.02(15) . . ?
O2 C3 H3 110.8 . . ?
C2 C3 H3 110.8 . . ?
C4 C3 H3 110.8 . . ?
C6 O4 H4O 109(2) . . ?
C8 C4 C3 121.42(17) . . ?
C8 C4 C5 118.24(17) . . ?
C3 C4 C5 97.08(15) . . ?
C8 C4 H4 106.3 . . ?
C3 C4 H4 106.3 . . ?
C5 C4 H4 106.3 . . ?
C11 O5 C12 60.56(14) . . ?
C15 C5 C4 98.90(17) . . ?
C15 C5 C6 110.33(16) . . ?
C4 C5 C6 112.58(15) . . ?
C15 C5 H5 111.5 . . ?
C4 C5 H5 111.5 . . ?
C6 C5 H5 111.5 . . ?
O4 C6 C11 106.78(15) . . ?
O4 C6 C5 110.51(16) . . ?
C11 C6 C5 106.35(16) . . ?
O4 C6 C1 114.84(16) . . ?
C11 C6 C1 105.61(16) . . ?
C5 C6 C1 112.12(14) . . ?
C13 O6 C14 60.94(14) . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7AB 109.5 . . ?
H7A C7 H7AB 109.5 . . ?
C1 C7 H7AC 109.5 . . ?
H7A C7 H7AC 109.5 . . ?
H7AB C7 H7AC 109.5 . . ?
C9 C8 C10 121.1(2) . . ?
C9 C8 C4 123.6(2) . . ?
C10 C8 C4 114.90(19) . . ?
C8 C9 H9A 120.0 . . ?
C8 C9 H9AB 120.0 . . ?
H9A C9 H9AB 120.0 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 C12 60.32(14) . . ?
O5 C11 C6 114.86(18) . . ?
C12 C11 C6 109.08(17) . . ?
O5 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C6 C11 H11 119.5 . . ?
O5 C12 C11 59.12(14) . . ?
O5 C12 C13 111.69(18) . . ?
C11 C12 C13 109.14(17) . . ?
O5 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
O6 C13 C14 59.82(15) . . ?
O6 C13 C12 114.14(18) . . ?
C14 C13 C12 118.05(19) . . ?
O6 C13 C1 118.88(17) . . ?
C14 C13 C1 129.29(18) . . ?
C12 C13 C1 108.00(16) . . ?
O6 C14 C13 59.25(14) . . ?
O6 C14 H14A 117.8 . . ?
C13 C14 H14A 117.8 . . ?
O6 C14 H14B 117.8 . . ?
C13 C14 H14B 117.8 . . ?
H14A C14 H14B 115.0 . . ?
O3 C15 O2 121.8(2) . . ?
O3 C15 C5 129.1(2) . . ?
O2 C15 C5 109.17(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.416(2) . ?
O1 H1O 0.83(3) . ?
C1 C7 1.538(3) . ?
C1 C2 1.555(3) . ?
C1 C13 1.556(3) . ?
C1 C6 1.585(3) . ?
O2 C15 1.350(3) . ?
O2 C3 1.465(3) . ?
C2 C3 1.521(3) . ?
C2 H2 0.9800 . ?
O3 C15 1.198(3) . ?
C3 C4 1.531(3) . ?
C3 H3 0.9800 . ?
O4 C6 1.415(2) . ?
O4 H4O 0.84(3) . ?
C4 C8 1.510(3) . ?
C4 C5 1.543(3) . ?
C4 H4 0.9800 . ?
O5 C11 1.434(3) . ?
O5 C12 1.452(3) . ?
C5 C15 1.526(3) . ?
C5 C6 1.559(3) . ?
C5 H5 0.9800 . ?
C6 C11 1.516(3) . ?
O6 C13 1.436(3) . ?
O6 C14 1.445(3) . ?
C7 H7A 0.9600 . ?
C7 H7AB 0.9600 . ?
C7 H7AC 0.9600 . ?
C8 C9 1.324(3) . ?
C8 C10 1.506(3) . ?
C9 H9A 0.9300 . ?
C9 H9AB 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.455(3) . ?
C11 H11 0.9800 . ?
C12 C13 1.491(3) . ?
C12 H12 0.9800 . ?
C13 C14 1.461(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1O O4 0.83(3) 2.03(3) 2.827(2) 161(4) 1_655 yes
O4 H4O O3 0.84(3) 2.50(4) 2.874(2) 108(3) 1_465 yes
C14 H14A O1 0.97 2.30 2.900(3) 119.2 . yes
C14 H14A O5 0.97 2.52 3.378(3) 147.2 1_655 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C1 C2 O1 -75.7(2) . . . . ?
C13 C1 C2 O1 45.3(2) . . . . ?
C6 C1 C2 O1 162.48(16) . . . . ?
C7 C1 C2 C3 156.63(17) . . . . ?
C13 C1 C2 C3 -82.4(2) . . . . ?
C6 C1 C2 C3 34.8(2) . . . . ?
C15 O2 C3 C2 -88.5(2) . . . . ?
C15 O2 C3 C4 31.3(2) . . . . ?
O1 C2 C3 O2 -69.5(2) . . . . ?
C1 C2 C3 O2 55.8(2) . . . . ?
O1 C2 C3 C4 177.77(17) . . . . ?
C1 C2 C3 C4 -57.0(2) . . . . ?
O2 C3 C4 C8 -176.43(16) . . . . ?
C2 C3 C4 C8 -59.3(2) . . . . ?
O2 C3 C4 C5 -47.04(17) . . . . ?
C2 C3 C4 C5 70.09(19) . . . . ?
C8 C4 C5 C15 176.10(16) . . . . ?
C3 C4 C5 C15 44.57(17) . . . . ?
C8 C4 C5 C6 59.6(2) . . . . ?
C3 C4 C5 C6 -71.92(19) . . . . ?
C15 C5 C6 O4 -179.95(17) . . . . ?
C4 C5 C6 O4 -70.5(2) . . . . ?
C15 C5 C6 C11 64.5(2) . . . . ?
C4 C5 C6 C11 173.96(17) . . . . ?
C15 C5 C6 C1 -50.4(2) . . . . ?
C4 C5 C6 C1 59.0(2) . . . . ?
C7 C1 C6 O4 -26.4(2) . . . . ?
C2 C1 C6 O4 92.05(19) . . . . ?
C13 C1 C6 O4 -141.49(16) . . . . ?
C7 C1 C6 C11 91.0(2) . . . . ?
C2 C1 C6 C11 -150.57(16) . . . . ?
C13 C1 C6 C11 -24.12(19) . . . . ?
C7 C1 C6 C5 -153.58(17) . . . . ?
C2 C1 C6 C5 -35.2(2) . . . . ?
C13 C1 C6 C5 91.30(17) . . . . ?
C3 C4 C8 C9 -13.1(3) . . . . ?
C5 C4 C8 C9 -132.5(2) . . . . ?
C3 C4 C8 C10 173.95(18) . . . . ?
C5 C4 C8 C10 54.5(2) . . . . ?
C12 O5 C11 C6 98.66(19) . . . . ?
O4 C6 C11 O5 75.5(2) . . . . ?
C5 C6 C11 O5 -166.52(16) . . . . ?
C1 C6 C11 O5 -47.2(2) . . . . ?
O4 C6 C11 C12 140.80(19) . . . . ?
C5 C6 C11 C12 -101.18(19) . . . . ?
C1 C6 C11 C12 18.1(2) . . . . ?
C11 O5 C12 C13 -99.98(19) . . . . ?
C6 C11 C12 O5 -108.36(19) . . . . ?
O5 C11 C12 C13 104.37(19) . . . . ?
C6 C11 C12 C13 -4.0(2) . . . . ?
C14 O6 C13 C12 -109.6(2) . . . . ?
C14 O6 C13 C1 121.1(2) . . . . ?
O5 C12 C13 O6 -83.4(2) . . . . ?
C11 C12 C13 O6 -146.83(19) . . . . ?
O5 C12 C13 C14 -150.7(2) . . . . ?
C11 C12 C13 C14 145.8(2) . . . . ?
O5 C12 C13 C1 51.2(2) . . . . ?
C11 C12 C13 C1 -12.2(2) . . . . ?
C7 C1 C13 O6 36.3(2) . . . . ?
C2 C1 C13 O6 -83.8(2) . . . . ?
C6 C1 C13 O6 154.34(17) . . . . ?
C7 C1 C13 C14 109.4(3) . . . . ?
C2 C1 C13 C14 -10.7(3) . . . . ?
C6 C1 C13 C14 -132.5(2) . . . . ?
C7 C1 C13 C12 -95.8(2) . . . . ?
C2 C1 C13 C12 144.06(18) . . . . ?
C6 C1 C13 C12 22.2(2) . . . . ?
C12 C13 C14 O6 103.1(2) . . . . ?
C1 C13 C14 O6 -104.2(2) . . . . ?
C3 O2 C15 O3 179.1(2) . . . . ?
C3 O2 C15 C5 -1.2(2) . . . . ?
C4 C5 C15 O3 150.8(2) . . . . ?
C6 C5 C15 O3 -91.0(3) . . . . ?
C4 C5 C15 O2 -28.8(2) . . . . ?
C6 C5 C15 O2 89.4(2) . . . . ?