#------------------------------------------------------------------------------
#$Date: 2024-12-03 05:01:28 +0200 (Tue, 03 Dec 2024) $
#$Revision: 296197 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312718.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_2312718
loop_
_publ_author_name
'Bibila Mayaya Bisseyou, Yvon'
'Wright, Jonathan'
'Jelsch, Christian'
_publ_contact_author             'Christian Jelsch'
_publ_section_title
;
 Conformational disorder in quercetin dihydrate revealed from
 ultrahigh-resolution synchrotron diffraction.
;
_journal_coeditor_code           PX5065SUP1
_journal_issue                   6
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_paper_doi               10.1107/S2052520624010011
_journal_volume                  80
_journal_year                    2024
_chemical_formula_moiety         'C15 H10 O7, 1.984(H2 O)'
_chemical_formula_sum            'C15 H13.968 O8.984'
_chemical_formula_weight         337.965
_chemical_name_common            'quercetin dihydrate'
_chemical_name_systematic        'quercetin dihydrate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'MoPro rev2608,  2023-10  '
_audit_update_record
;
2024-10-25 # Formatted by IUCr publCIF

;
_cell_angle_alpha                71.986(4)
_cell_angle_beta                 83.860(5)
_cell_angle_gamma                85.624(5)
_cell_formula_units_Z            2
_cell_length_a                   3.7244(17)
_cell_length_b                   13.050(6)
_cell_length_c                   14.982(7)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      3.54
_cell_volume                     687.8(5)
_computing_molecular_graphics
;
Ortep3 for Windows (Farrugia, 2012)
MoProViewer (Guillot et al., 2014)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
MoPro (Jelsch et al., 2005)
;
_diffrn_ambient_temperature      20(2)
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Huber diffractometer, ID11/ESRF'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.15815
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_av_sigmaI/netI    0.03267
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            44510
_diffrn_reflns_theta_full        14.34
_diffrn_reflns_theta_max         14.62
_diffrn_reflns_theta_min         0.63
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             351.68
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.56
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         44510
_refine_ls_number_restraints     290
_refine_ls_restrained_S_all      1.629
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w =1/[8.8*\s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0386
_refine_ls_wR_factor_ref         0.0414
_reflns_number_gt                35265
_reflns_number_total             44510
_reflns_threshold_expression     'I > 2 \s(I)'
_publcif_datablock.id            {3882666b-713c-41ad-9769-25f2d54f1308}
_iucr_refine_instructions_details
; 
! MoPro rev2608, 2023-10 16/11/2023 16:40:28
! molecular file:  querc_disor_OW2part_MM85.par
! reflections hkl file : quercetin_merged.hkl refin. vs. F^2^
! atomic table file : D:\MoProSuite\LibMoPro\mopro_v22.tab
! wave functions file : D:\MoProSuite\LibMoPro\WAVEF
! anomalous scattering file : D:\MoProSuite\LibMoPro\asf_Kissel.dat
! Constraints file : CONSTRAIN.txt
! Restraints file : RESTRAIN.txt
! RF factor = 3.391 % RI factor = 3.345%
! wR2F factor = 2.329 % wR2I factor = 4.138%
! g.o.f.(F**2) = 1.013 Nvar= 815 Nref= 44510 Nfree= 0 0.07<sinT/l< 1.60

! P00 Dip Qua Oct Hex l=5 l=6
! O nl = 2 2 2 3 4 5 6
! O zeta= 4.466 4.466 4.466 4.466 4.466 4.466 4.466
! H nl = 2 1 2 3 4 5 6
! H zeta= 2.000 2.000 2.000 2.000 2.000 2.000 2.000
! C nl = 2 2 2 3 4 5 6
! C zeta= 3.176 3.176 3.176 3.176 3.176 3.176 3.176

WSIG 8.80000 ! weighting scheme

SPACE GROUP

CELL 3.7244 13.0497 14.9818 71.9860 83.8600 85.6240 0.15820
ZERR 0.0017 0.0060 0.0069 0.0040 0.0050 0.0050

SYMM 1 P CENTRO
 ' x , y , z '

SCALE 1 0.763588

FMULT 1.00000

UOVER 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 ANI

SOLVT 0.00000 50.00000

EXTIN 0.00000 GAUSSIAN ISOT TYP1 ! G*10^4


DUMMY 0

KAPPA 12
 0.977294 1.231901 ! # 1 1 QUE O13a 6X O
 1.264750 1.312788 ! # 2 1 QUE HO13a 6X H
 0.993836 1.501405 ! # 3 1 QUE O1 1X O
 0.979171 1.363511 ! # 4 1 QUE O4 1X O
 1.010695 0.968802 ! # 5 1 QUE C2 2X C
 1.019006 0.929607 ! # 6 1 QUE C3 5X C
 1.009591 1.007278 ! # 7 1 QUE C4 1X C
 1.022373 1.073183 ! # 8 1 QUE C6 5X C
 1.128358 1.135125 ! # 9 1 QUE H6 6X H
 1.014471 1.050426 ! # 10 1 QUE C10 2X C
 0.985123 0.950461 ! # 11 1 WAT OW2 2X O
 1.265536 1.322757 ! # 12 1 WAT HW2A 4X H


ATOMS 41

ATOM 1 O13a QUE 1 1.373708 0.028243 0.083148 0.9827 1 O
bXY C13 HO13a OCT K1 V0 M0 Q0
UANI 0.014674 0.008411 0.007010 0.003295 -.001529 -.003288
 6.35919 0. -.063 0.027 0. 0.062 0. 0. 0.035 0.030 ! Pv P0 3Dip 5Qua
 0. -.025 -.001 0. 0. -.053 0.003 ! Oct

ATOM 2 HO13a QUE 1 1.227152 0.082476 0.038968 0.9827 1 H
 ZX O13a C13 DIP K2 V0 M0 Q1_O13a
UISO 0.014966
 0.59290 0. 0. 0. 0.148 ! Pv P00 Dip

ATOM 3 O13b QUE 1 1.527447 -0.106565 0.403980 0.0173 1 O
bXY C15 HO13b OCT K1 V1_O13a M1_O13a Q-1_O13a
UISO 0.005751
 6.35919 0. -.063 0.027 0. 0.062 0. 0. 0.035 0.030 ! Pv P0 3Dip 5Qua
 0. -.025 -.001 0. 0. -.053 0.003 ! Oct

ATOM 4 HO13b QUE 1 1.490678 -0.084471 0.461915 0.0173 1 H
 ZX O13b C15 DIP K2 V1_HO13a M1_HO13a Q-1_O13a
UISO 0.008626
 0.59290 0. 0. 0. 0.148 ! Pv P00 Dip

ATOM 5 O1 QUE 1 0.893716 0.322085 0.210481 1.0000 1 O
bXY C9 C2 OCT K3 V0 M0 Q0
UANI 0.008388 0.004808 0.004897 0.001835 -.000604 -.001664
 6.17601 0. -.086 -.021 0.003 0.050 -.004 0.007 0.058 0.005 ! Pv P0 3Dip 5Qua
 -.007 0.006 0.012 -.006 -.003 -.014 -.006 ! Oct

ATOM 6 O3 QUE 1 0.951208 0.192110 0.461417 1.0000 1 O
bXY C3 H3 OCT K1 V0 M0 Q0
UANI 0.014801 0.006647 0.005369 0.003689 -.001739 -.001484
 6.38158 0. -.088 -.003 0.030 0.082 0.008 0.014 0.017 0.043
 0.012 0.017 -.026 0.015 -.005 -.052 -.002

ATOM 7 H3 QUE 1 0.953421 0.227594 0.509634 1.0000 1 H
 ZX O3 C3 DIP K2 V0 M0 Q0
UANI 0.031144 0.017334 0.013576 0.004188 -.004675 -.006740
 0.62393 0. 0. 0. 0.153

ATOM 8 O4 QUE 1 0.600499 0.383247 0.459324 1.0000 1 O
 XY C4 C3 OCT K4 V0 M0 Q0
UANI 0.012513 0.007438 0.004750 0.002762 -.000230 -.002181
 6.33263 0. -.052 0.022 0.004 -.001 -.003 -.007 -.031 -.004
 -.009 0.006 -.002 -.009 0. 0.013 -.001

ATOM 9 O5 QUE 1 0.333251 0.569033 0.366892 1.0000 1 O
bXY C5 H5 OCT K1 V0 M0 Q0
UANI 0.012916 0.007501 0.005879 0.003803 -.000830 -.002984
 6.37240 0. -.051 0.025 -.004 0.087 0.004 -.005 0.026 0.020
 -.006 -.012 -.016 -.003 -.001 -.040 -.011

ATOM 10 H5 QUE 1 0.394879 0.506559 0.419110 1.0000 1 H
 ZX O5 C5 DIP K2 V0 M0 Q0
UANI 0.028256 0.015586 0.013127 0.006369 -.002423 -.002802
 0.64387 0. 0. 0. 0.108

ATOM 11 O7 QUE 1 0.426774 0.661808 0.032009 1.0000 1 O
bXY C7 H7 OCT K1 V0 M0 Q0
UANI 0.013455 0.007067 0.005717 0.002799 -.001443 -.000578
 6.36389 0. -.080 0.023 -.011 0.071 -.008 0.005 0.055 0.031
 0.009 -.005 -.027 0.005 -.004 -.043 0.020

ATOM 12 H7 QUE 1 0.290491 0.725406 0.040908 1.0000 1 H
 ZX O7 C7 DIP K2 V0 M0 Q0
UANI 0.027691 0.014713 0.017478 0.007191 -.002893 -.004559
 0.64916 0. 0. 0. 0.133

ATOM 13 O14 QUE 1 1.614782 -0.133316 0.227480 1.0000 1 O
bXY C14 H14 OCT K1 V1_O13a M1_O13a Q0
UANI 0.012909 0.006121 0.008143 0.004250 -.002293 -.002940
 6.35919 0. -.063 0.027 0. 0.062 0. 0. 0.035 0.030
 0. -.025 -.001 0. 0. -.053 0.003

ATOM 14 H14 QUE 1 1.710539 -0.180868 0.285036 1.0000 1 H
 ZX O14 C14 DIP K2 V0 M0 Q0
UANI 0.029915 0.016863 0.015634 0.008439 -.006875 -.004317
 0.60341 0. 0. 0. 0.136

ATOM 15 C2 QUE 1 0.973533 0.246235 0.293054 1.0000 1 C
bXY C3 C11 OCT K5 V0 M0 Q0
UANI 0.006792 0.004467 0.005138 0.001148 -.000611 -.001712
 4.01223 0. 0.067 0.002 0.001 -.115 0. 0.001 -.114 -.028
 0.001 0.050 -.021 -.001 0. -.268 -.031

ATOM 16 C3 QUE 1 0.880734 0.266134 0.378173 1.0000 1 C
bXY C2 C4 OCT K6 V0 M0 Q0
UANI 0.008279 0.004894 0.004890 0.001587 -.000728 -.001546
 3.93873 0. 0.097 -.028 0.004 -.118 0.002 -.009 -.110 -.045
 0.003 0.066 -.027 -.001 -.003 -.288 -.027

ATOM 17 C4 QUE 1 0.693922 0.365867 0.380948 1.0000 1 C
bXY C3 C10 OCT K7 V0 M0 Q0
UANI 0.007611 0.005026 0.004618 0.001441 -.000462 -.001548
 3.93912 0. 0.046 -.007 -.003 -.158 -.001 0.001 0.015 -.001
 0.009 0.020 -.001 0.008 -.004 -.268 0.007

ATOM 18 C5 QUE 1 0.446059 0.545132 0.286468 1.0000 1 C
bXY C10 C6 OCT K6 V0 M0 Q0
UANI 0.007826 0.004912 0.005124 0.001632 -.000754 -.001817
 3.93504 0. 0.118 0.001 -.002 -.155 -.005 0.004 -.078 0.013
 0.002 0.044 0.004 -.003 -.001 -.305 -.005

ATOM 19 C6 QUE 1 0.386580 0.619295 0.200171 1.0000 1 C
bXY C5 C7 OCT K8 V0 M0 Q0
UANI 0.009239 0.005146 0.005572 0.001817 -.001052 -.001508
 3.90238 0. -.017 -.001 -.003 -.079 0.005 0.007 -.014 0.010
 -.001 0.022 -.011 -.005 0.001 -.161 0.006

ATOM 20 H6 QUE 1 0.257032 0.697251 0.196919 1.0000 1 H
 ZX C6 C5 DIP K9 V0 M0 Q0
UANI 0.030708 0.013205 0.021741 0.008943 -.003370 -.006181
 0.97209 0. 0. 0. 0.163

ATOM 21 C7 QUE 1 0.492701 0.591463 0.117028 1.0000 1 C
bXY C8 C6 OCT K6 V0 M0 Q0
UANI 0.008165 0.005097 0.005167 0.001146 -.000891 -.001105
 3.99435 0. 0.130 0.002 -.004 -.178 -.002 0.003 -.123 0.002
 0.007 0.067 -.008 -.001 0.001 -.323 -.004

ATOM 22 C8 QUE 1 0.664258 0.491462 0.119713 1.0000 1 C
bXY C9 C7 OCT K8 V0 M0 Q0
UANI 0.009029 0.005503 0.004834 0.001710 -.000756 -.001386
 3.90535 0. -.002 0.002 0.004 -.075 0. 0. 0.020 0.013
 0.002 0.033 -.011 0.003 0.003 -.147 0.011

ATOM 23 H8 QUE 1 0.741242 0.470364 0.056234 1.0000 1 H
 ZX C8 C9 DIP K9 V0 M0 Q0
UANI 0.033127 0.021962 0.012156 0.005450 -.000588 -.008395
 0.96735 0. 0. 0. 0.161

ATOM 24 C9 QUE 1 0.727558 0.419169 0.207912 1.0000 1 C
bXY C10 C8 OCT K5 V0 M0 Q0
UANI 0.006786 0.004471 0.004625 0.001058 -.000502 -.001440
 4.01815 0. 0.129 0.004 -.002 -.153 0.008 -.003 -.109 0.
 0.001 0.018 0.001 -.006 -.008 -.309 0.005

ATOM 25 C10 QUE 1 0.622843 0.443321 0.292287 1.0000 1 C
bXY C9 C5 OCT K10 V0 M0 Q0
UANI 0.007222 0.004605 0.004586 0.001378 -.000478 -.001513
 3.96895 0. 0.007 0.002 -.015 -.065 -.002 -.012 -.011 -.016
 0.003 -.001 0.003 -.004 0. -.170 -.004

ATOM 26 C11 QUE 1 1.150544 0.148161 0.277849 1.0000 1 C
bXY C16 C12 OCT K10 V0 M0 Q0
UANI 0.007188 0.004492 0.006031 0.001521 -.000952 -.002021
 4.07402 0. 0.022 0. 0. -.126 0. 0. -.027 0.
 0. -.013 0. 0. 0. -.189 0.

ATOM 27 C12 QUE 1 1.185278 0.137081 0.186125 1.0000 1 C
bXY C13 C11 OCT K8 V0 M0 Q0
UANI 0.009223 0.005416 0.006209 0.002778 -.001475 -.002345
 3.96191 0. 0.023 0. 0. -.127 0. 0. -.022 0.
 0. 0.029 0. 0. 0. -.172 0.

ATOM 28 H12 QUE 1 1.093593 0.200477 0.127705 1.0000 1 H
 ZX C12 C13 DIP K9 V0 M0 Q0
UANI 0.035105 0.017659 0.015109 0.009997 -.007875 -.002038
 1.06840 0. 0. 0. 0.166

ATOM 29 C13 QUE 1 1.339206 0.042862 0.170578 1.0000 1 C
bXY C14 C12 OCT K6 V0 M0 Q0
UANI 0.009213 0.005490 0.006088 0.002780 -.001665 -.002414
 3.90156 0. 0.169 0.053 0. -.153 0. 0. -.085 0.021
 0. 0.066 0.004 0. 0. -.302 0.012

ATOM 30 H13b QUE 1 1.375536 0.035292 0.100212 0.0173 1 H
 ZX C13 O13a DIP K9 V0 M0 Q-1_O13a
UISO 0.008247
 1.08752 0. 0. 0. 0.161

ATOM 31 C14 QUE 1 1.468344 -0.042061 0.245803 1.0000 1 C
bXY C13 C15 OCT K6 V0 M0 Q0
UANI 0.008258 0.005018 0.006810 0.002179 -.001613 -.002299
 3.90677 0. 0.111 0. 0. -.153 0. 0. -.095 0.
 0. 0.051 0. 0. 0. -.302 0.

ATOM 32 C15 QUE 1 1.440085 -0.030418 0.336210 1.0000 1 C
bXY C14 C16 OCT K8 V0 M0 Q0
UANI 0.009505 0.005389 0.006134 0.002195 -.001448 -.001908
 3.88972 0. 0.067 0. 0. -.133 0. 0. -.030 0.
 0. 0.027 0. 0. 0. -.174 0.

ATOM 33 H15a QUE 1 1.546387 -0.096641 0.395118 0.9827 1 H
 ZX C15 C14 DIP K9 V1_H13b M1_H13b Q1_O13a
UISO 0.008463
 1.08752 0. 0. 0. 0.161

ATOM 34 C16 QUE 1 1.282333 0.062950 0.352673 1.0000 1 C
bXY C11 C15 OCT K8 V0 M0 Q0
UANI 0.009684 0.005518 0.005993 0.002205 -.001387 -.002070
 3.97928 0. 0.077 0. 0. -.132 0. 0. 0.030 0.
 0. 0.019 0. 0. 0. -.184 0.

ATOM 35 H16 QUE 1 1.266588 0.068242 0.422977 1.0000 1 H
 ZX C16 C11 DIP K9 V0 M0 Q0
UANI 0.037769 0.023240 0.012432 0.007217 -.005383 -.008482
 1.11907 0. 0. 0. 0.162

ATOM 36 OW2 WAT 1 0.867448 0.734321 0.389288 0.9827 1 O
bXY HW2A HW2B OCT K11 V0 M0 Q1_O13a
UANI 0.012251 0.006511 0.008994 0.002418 -.001324 -.001652
 6.34000 0. -.116 0. 0. 0.065 0. 0. 0.026 0.
 0. -.037 0. 0. 0. -.048 0.

ATOM 37 HW2A WAT 1 0.675838 0.695474 0.430660 0.9827 1 H
 ZX OW2 HW2B QUA K12 V0 M0 Q1_O13a
UISO 0.014305
 0.83000 0. 0. 0. 0.184 0.070 0. 0. 0. 0.

ATOM 38 HW2B WAT 1 1.031274 0.677717 0.379401 0.9827 1 H
 ZX OW2 HW2A QUA K12 V0 M1_HW2A Q1_O13a
UISO 0.014305
 0.83000 0. 0. 0. 0.184 0.070 0. 0. 0. 0.

ATOM 39 OW3 WAT 1 1.024189 0.847065 0.060275 1.0000 1 O
bXY HW3B HW3A OCT K11 V0 M1_OW2 Q0
UANI 0.014774 0.008207 0.011495 0.002133 -.000131 -.001417
 6.34000 0. -.116 0. 0. 0.065 0. 0. 0.026 0.
 0. -.037 0. 0. 0. -.048 0.

ATOM 40 HW3A WAT 1 0.862884 0.846257 0.114963 1.0000 1 H
 ZX OW3 HW3B QUA K12 V0 M1_HW2A Q0
UISO 0.018111
 0.83000 0. 0. 0. 0.184 0.070 0. 0. 0. 0.

ATOM 41 HW3B WAT 1 1.181393 0.902060 0.059020 1.0000 1 H
 ZX OW3 HW3A QUA K12 V0 M1_HW2A Q0
UISO 0.018111
 0.83000 0. 0. 0. 0.184 0.070 0. 0. 0. 0.

ANHAR 8 4 ! number_of_anharmonic_atoms max_order
 13 ! O14 1 ! atom_number
 6.10E-04 2.28E-06-2.67E-05 5.94E-04-4.55E-05 1.39E-03 7.47E-05-1.68E-05
 4.68E-05 1.47E-04
 3.55E-03-2.65E-06 8.28E-06 1.13E-03-3.29E-04 4.07E-04-1.64E-04 3.63E-04
 3.14E-05-1.92E-05 4.69E-05-2.11E-05 5.13E-06 7.92E-06-5.11E-06
 39 ! OW3 1 ! atom_number
 1.53E-03 5.43E-05-6.47E-05 1.74E-03 5.67E-04-9.06E-04 3.95E-04-1.13E-04
 1.35E-04-5.10E-04
 1.18E-03-4.83E-06 5.40E-06 6.49E-04-6.99E-04 4.95E-05-1.89E-04 2.80E-04
 4.32E-05-5.33E-05 8.21E-05-3.80E-05 6.00E-06 1.25E-06-4.06E-06
 36 ! OW2 1 ! atom_number
-6.74E-05 1.98E-05-2.70E-05-1.02E-04 1.49E-06-1.16E-04 1.66E-05-6.11E-05
 7.03E-05 9.44E-05
 6.11E-04-2.80E-06 3.84E-06 2.19E-04-1.79E-04 3.71E-06-3.68E-05 8.37E-05
 2.13E-05-2.39E-05 3.72E-05-2.15E-05-4.48E-06 7.45E-06-5.81E-06
 31 ! C14 1 ! atom_number
 9.28E-04 5.27E-05-4.30E-05 5.92E-04 2.89E-04-1.70E-04 1.86E-04-1.10E-04
 1.06E-04-3.08E-04
 1.27E-03-1.30E-06 3.23E-06 7.84E-04-4.52E-04 1.21E-04-1.76E-04 1.91E-04
 7.56E-05-9.68E-05 9.47E-05-2.78E-05-8.78E-06 1.31E-05-6.92E-06
 29 ! C13 1 ! atom_number
 2.14E-03 5.15E-05-4.42E-05 1.24E-03 4.53E-04-4.38E-04 2.72E-04-1.11E-04
 1.02E-04-4.55E-04
 2.20E-03-3.08E-07 3.35E-06 1.13E-03-7.23E-04 2.06E-04-2.42E-04 2.29E-04
 8.08E-05-1.16E-04 1.09E-04-4.07E-05-7.43E-06 1.07E-05-7.64E-06
 1 ! O13a 1 ! atom_number
 5.87E-04 3.86E-05-5.46E-05 2.41E-04 2.39E-04-2.87E-04 2.92E-04-9.57E-05
 1.05E-04-3.58E-04
 8.40E-04-3.10E-06 7.67E-06 3.06E-04-4.41E-04-1.36E-06-1.33E-04 2.18E-04
 3.78E-05-6.97E-05 7.42E-05-3.96E-05-3.79E-06 6.99E-06-7.12E-06
 26 ! C11 1 ! atom_number
 2.36E-03 3.81E-06-2.51E-05-3.76E-04 1.69E-04-1.16E-03 1.84E-04-3.97E-05
 9.45E-06-5.24E-05
 2.14E-03-8.62E-06 7.45E-07 2.65E-04-7.74E-04 9.52E-05 1.08E-04 2.72E-04
 2.51E-05-2.11E-05 2.62E-05-1.14E-05 1.24E-05-8.85E-06 9.29E-06
 27 ! C12 1 ! atom_number
 5.17E-03-1.29E-05-9.55E-05-1.29E-07-1.20E-05 1.42E-03 6.28E-04-6.82E-05
-5.00E-05 3.96E-05
 3.50E-03 1.60E-06 1.89E-05 4.34E-04 6.51E-04 2.18E-04 3.42E-04 7.01E-04
 2.65E-05 5.41E-05 1.23E-04 9.33E-06 2.06E-05 1.56E-05 2.14E-05


STOP

############ RESTRAINTS ############ 

! PREP REST KAPP
SIMKAP 1 O13a O14 0.01
SIMKAP 1 O5 O7 0.01
SIMKAP 1 C6 C8 0.01
SIMKAP 1 OW2 OW3 0.01

SIMKAP 1 HO13a HO13b H3 H5 H7 H14 0.01
SIMKAP 1 H6 H8 0.01
SIMKAP 1 H12 H15a 0.01
SIMKAP 1 HW2A HW2B HW3A HW3B 0.01


! PREP RES EQUI
SIMPVM 1 O5 O7 0.01
SIMPVM 1 C6 C8 0.01

SIMPLM 1 C5 C9 0.01
SIMPLM 1 C12 C15 0.01


SIMPVM 1 HO13a H14 0.01
SIMPVM 1 H6 H8 0.01
SIMPVM 1 H12 H15a 0.01
SIMPVM 1 HW2A HW3B 0.01

SIMPLM 1 HO13a HW2A 0.01
SIMPLM 1 H6 H16 0.01

! PREP RES SYMP
RSYMUL mymz O1 1 0.005
RSYMUL mz O3 1 0.005
RSYMUL mymz O4 1 0.005
RSYMUL mz O5 1 0.005
RSYMUL mz O7 1 0.005
RSYMUL mz O14 1 0.005
RSYMUL mz C2 1 0.005
RSYMUL mz C3 1 0.005
RSYMUL mymz C4 1 0.005
RSYMUL mymz C5 1 0.005
RSYMUL mymz C6 1 0.005
RSYMUL mymz C7 1 0.005
RSYMUL mymz C8 1 0.005
RSYMUL mymz C9 1 0.005
RSYMUL 3mmz C10 1 0.005

RSYMUL mymz OW2 1 0.005
RSYMUL mymz OW3 1 0.005

RIGIDB ALL BON 0.001
RIGUIJ ALL BON 0.002

SIMK12 CHEM H 0.01
KAPPA1 H6 1 1.16 0.01 ! standard kappa1 of H

KAPPA1 1 OW2 0.98473 0.01 ! database ELMAM2
KAPPA2 1 OW2 0.96362 0.01
RESVAL 1 OW2 6.34000 0.01
RESDIP 1 OW2 -.082 0. 0. 0.01
RESQUA 1 OW2 0.049 0. 0. 0.021 0. 0.01
RESOCT 1 OW2 0. -.039 0. 0. 0. -.079 0. 0.01

KAPPA1 1 HW2A 1.161560 0.01 ! database ELMAM2
KAPPA1 1 HW2A 1.499840 0.01
RESVAL 1 HW2A 0.83000 0.01
RESDIP 1 HW2A 0. 0. 0.120 0.01
RESQUA 1 HW2A 0.102 0. 0. 0. 0. 0.01


ANGLER 1 C13 O13a HO13a 109.5 1.
ANGLER 1 C15 O13b HO13b 109.5 1.

PLANAR 4 1 C14 C15 O13b HO13b 0.01

PLANAR 7 1 C11 C12 C13 C14 C15 C16 H15a 0.01
PLANAR 7 1 C11 C12 C13 C14 C15 C16 H13b 0.01



! PREP REST SIMD
SIMDIS 1 C9 H8 C7 H8 0.005
SIMDIS 1 C14 H15a C16 H15a 0.005
SIMDIS 1 C14 H13b C12 H13b 0.005
SIMDIS 1 OW2 HW2A OW2 HW2B OW3 HW3B OW3 HW3A 0.005 !!
SIMDIS 1 O13a HO13a O13b HO13b 0.005 !!

! PREP REST DIST

DISTAN O13a 1 HO13a 1 0.992 0.005
DISTAN O13b 1 HO13b 1 0.992 0.005
DISTAN O3 1 H3 1 0.992 0.005
DISTAN O5 1 H5 1 0.992 0.005
DISTAN O7 1 H7 1 0.992 0.005
DISTAN O14 1 H14 1 0.992 0.005
DISTAN C6 1 H6 1 1.083 0.005
DISTAN C8 1 H8 1 1.083 0.005
DISTAN C12 1 H12 1 1.083 0.005
DISTAN C13 1 H13b 1 1.083 0.005
DISTAN C15 1 H15a 1 1.083 0.005
DISTAN C16 1 H16 1 1.083 0.005
DISTAN OW2 1 HW2A 1 0.983 0.005
DISTAN OW2 1 HW2B 1 0.983 0.005
DISTAN OW3 1 HW3B 1 0.983 0.005
DISTAN OW3 1 HW3A 1 0.983 0.005

! Distance target = 1.077 -CH3
! Distance target = 1.092 C2>CH2
! Distance target = 1.091 Z2>CH2
! Distance target = 1.099 ->CH
! Distance target = 1.083 >CH aromatic
! Distance target = 1.082 C=C<H
! Distance target = 0.980 C-O-H
! Distance target = 0.983 X-O-H
! Distance target = 1.018 O=C-O-H
! Distance target = 0.97 Csp3-O-H
! Distance target = 0.992 C_arom-O-H
! Distance target = 1.033 NH4+ -NH3+ >NH2+ ->NH+
! Distance target = 1.015 -NH2 >NH
 ! reference: Allen FH & Bruno IJ,
 ! Acta Crystallographic (2010). B66, 380?386

#########################################
############ CONSTRAINts ############ 

! PREP CONS URAT
CONURA 1 O13a HO13a 1.5
CONURA 1 O13b HO13b 1.5
CONURA 1 C13 H13b 1.2
CONURA 1 C15 H15a 1.2
CONURA 1 OW2 HW2A 1.5
CONURA 1 OW2 HW2B 1.5
CONURA 1 OW3 HW3B 1.5
CONURA 1 OW3 HW3A 1.5

FIXVAL 1 OW2 6.34000
FIXVAL 1 OW3 6.34000       
FIXVAL 1 HW2A 0.83000
FIXVAL 1 HW2B 0.83000
FIXVAL 1 HW3A 0.83000
FIXVAL 1 HW3B 0.83000


       
SUMOCC 1 O13a H15b
SUMOCC 1 O13a O13b
SUMOCC 1 O13a H13b
SUMOCC 1 O13a HO13b

CONOCC 1 O13a H13a
CONOCC 1 O13a H15a
CONOCC 1 O13a HO13a

CONOCC 1 O13a OW2
CONOCC 1 O13a HW2A
CONOCC 1 O13a HW2B

! cycle with two orientations
AVEPVM 1 O13a O14

SYMPLM mymz C11 1
SYMPLM mymz C12 1
SYMPLM mz C13 1
SYMPLM mymz C14 1
SYMPLM mymz C15 1
SYMPLM mymz C16 1


! PREP CONS SYMP
SYMPLM mz O13a 1
SYMPLM mz O13b 1

SYMPLM mymz OW2 1
SYMPLM mymz OW3 1

AVEPLM 1 OW2 OW3
AVEPLM 1 HW2A HW2B HW3B HW3A



! disorder equiv constraints
AVEPVM 1 O13a O13b
AVEPVM 1 HO13a HO13b
AVEPVM 1 H15a H13b

CONKAP 1 O13a O13b
CONKAP 1 HO13a HO13b
CONKAP 1 H15a H13b

! SHADE3 Uij values
FIXUIJ H3 1 0.031144 0.017334 0.013576 0.004188 -0.004675 -0.006740
FIXUIJ H5 1 0.028256 0.015586 0.013127 0.006369 -0.002423 -0.002802
FIXUIJ H7 1 0.027691 0.014713 0.017478 0.007191 -0.002893 -0.004559
FIXUIJ H6 1 0.030708 0.013205 0.021741 0.008943 -0.003370 -0.006181
FIXUIJ H8 1 0.033127 0.021962 0.012156 0.005450 -0.000588 -0.008395
FIXUIJ H14 1 0.029915 0.016863 0.015634 0.008439 -0.006875 -0.004317
FIXUIJ H12 1 0.035105 0.017659 0.015109 0.009997 -0.007875 -0.002038
FIXUIJ H16 1 0.037769 0.023240 0.012432 0.007217 -0.005383 -0.008482

#########################################
;
_cod_data_source_file            px5065sup1.cif
_cod_data_source_block           I
_cod_database_code               2312718
_symmetry_space_group_name_h-m_alt 'P -1'
_publcif_funding_html            NA
loop_
_symmetry_equiv_pos_as_xyz
' x , y , z '
' -x , -y , -z '
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_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_disorder_assembly
_atom_site_disorder_group
O O13a 1.373708(5) 0.0282430(13) 0.0831480(10) 0.00998(7) Uani 0.98 d . . . 1
H HO13a 1.2272(15) 0.0825(4) 0.0390(4) 0.01497 Uiso 0.98 d D U . 1
O O13b 1.52744699(3) -0.10656500(2) 0.40397999(19) 0.0058(6) Uiso 0.02 d . . . 2
H HO13b 1.490677950(16) -0.084471002(12) 0.46191499(11) 0.00863 Uiso 0.02 d D U
. 2
O O1 0.89372(2) 0.322085(6) 0.210481(7) 0.006101(17) Uani 1 d . . . .
O O3 0.95121(3) 0.192110(6) 0.461417(5) 0.00918(2) Uani 1 d . . . .
H H3 0.953(2) 0.2276(5) 0.5096(4) 0.02030 Uani 1 d D U . .
O O4 0.60050(3) 0.383247(7) 0.459324(7) 0.00837(2) Uani 1 d . . . .
O O5 0.33325(3) 0.569033(6) 0.366892(5) 0.008777(19) Uani 1 d . . . .
H H5 0.3949(19) 0.5066(5) 0.4191(4) 0.01970 Uani 1 d D U . .
O O7 0.42677(3) 0.661808(6) 0.032009(6) 0.00919(2) Uani 1 d . . . .
H H7 0.2905(19) 0.7254(5) 0.0409(5) 0.02041 Uani 1 d D U . .
O O14 1.61478(5) -0.133316(15) 0.227480(14) 0.00903(6) Uani 1 d . . . .
H H14 1.711(2) -0.1809(5) 0.2850(4) 0.02109 Uani 1 d D U . .
C C2 0.973533(19) 0.246235(5) 0.293054(5) 0.005477(14) Uani 1 d . . . .
C C3 0.88073(2) 0.266134(5) 0.378173(5) 0.006098(15) Uani 1 d . . . .
C C4 0.69392(2) 0.365867(5) 0.380948(5) 0.005832(15) Uani 1 d . . . .
C C5 0.44606(2) 0.545132(5) 0.286468(5) 0.005977(15) Uani 1 d . . . .
C C6 0.38658(2) 0.619295(6) 0.200171(5) 0.006765(17) Uani 1 d . . . .
H H6 0.2570(17) 0.6973(4) 0.1969(5) 0.02214 Uani 1 d D U . .
C C7 0.49270(2) 0.591463(5) 0.117028(5) 0.006302(15) Uani 1 d . . . .
C C8 0.66426(2) 0.491462(6) 0.119713(5) 0.006596(16) Uani 1 d . . . .
H H8 0.7412(18) 0.4704(4) 0.0562(3) 0.02215 Uani 1 d D U . .
C C9 0.727558(19) 0.419169(5) 0.207912(4) 0.005351(14) Uani 1 d . . . .
C C10 0.622843(19) 0.443321(5) 0.292287(4) 0.005536(15) Uani 1 d . . . .
C C11 1.15054(5) 0.148161(14) 0.277849(13) 0.00588(5) Uani 1 d . . . .
C C12 1.18528(5) 0.137081(15) 0.186125(14) 0.00692(5) Uani 1 d . . . .
H H12 1.0936(17) 0.2005(4) 0.1277(4) 0.02347 Uani 1 d D U . .
C C13 1.33921(6) 0.042862(15) 0.170578(14) 0.00687(5) Uani 1 d . . . .
H H13b 1.3755(7) 0.0353(4) 0.1002(4) 0.00825 Uiso 0.02 d D U . 2
C C14 1.46834397(3) -0.04206100(2) 0.24580300(19) 0.00664(5) Uani 1 d . . . .
C C15 1.44008505(2) -0.030417999(17) 0.33621001(15) 0.007052(17) Uani 1 d . . .
.
H H15a 1.5464(7) -0.0966(3) 0.3951(3) 0.00846 Uiso 0.98 d D U . 1
C C16 1.28233(2) 0.062950(6) 0.352673(5) 0.007076(17) Uani 1 d . . . .
H H16 1.2666(17) 0.0682(4) 0.4230(3) 0.02400 Uani 1 d D U . .
O OW2 0.86745(5) 0.734321(16) 0.389288(13) 0.00954(6) Uani 0.98 d . . . .
H HW2A 0.6758(10) 0.6955(3) 0.4307(3) 0.01431 Uiso 0.98 d D U . .
H HW2B 1.0313(10) 0.6777(3) 0.3794(3) 0.01431 Uiso 0.98 d D U . .
O OW3 1.02419(6) 0.847065(17) 0.060275(17) 0.01207(6) Uani 1 d . . . .
H HW3A 0.8629(11) 0.8463(4) 0.1150(3) 0.01811 Uiso 1 d D U . .
H HW3B 1.1814(11) 0.9021(3) 0.0590(4) 0.01811 Uiso 1 d D U . .
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
O13a 0.01467(8) 0.00841(5) 0.00701(6) 0.00329(7) -0.00153(5) -0.00329(5)
O1 0.00839(2) 0.004808(16) 0.004897(15) 0.001835(15) -0.000604(14) -0.001664(13)
O3 0.01480(3) 0.006647(16) 0.005369(15) 0.003689(16) -0.001739(15) -0.001484(13)
H3 0.03114 0.01733 0.01358 0.00419 -0.00467 -0.00674
O4 0.01251(2) 0.007438(17) 0.004750(15) 0.002762(18) -0.000230(15) -0.002181(14)
O5 0.01292(2) 0.007501(16) 0.005879(16) 0.003803(16) -0.000830(15) -0.002984(13)
H5 0.02826 0.01559 0.01313 0.00637 -0.00242 -0.00280
O7 0.01345(2) 0.007067(16) 0.005717(16) 0.002799(17) -0.001443(15) -0.000578(13)
H7 0.02769 0.01471 0.01748 0.00719 -0.00289 -0.00456
O14 0.01291(7) 0.00612(5) 0.00814(6) 0.00425(5) -0.00229(5) -0.00294(4)
H14 0.02992 0.01686 0.01563 0.00844 -0.00687 -0.00432
C2 0.006792(17) 0.004467(14) 0.005138(15) 0.001148(12) -0.000611(12)
-0.001712(11)
C3 0.008279(18) 0.004894(14) 0.004890(14) 0.001587(13) -0.000728(12)
-0.001546(11)
C4 0.007611(18) 0.005026(14) 0.004618(14) 0.001441(13) -0.000462(12)
-0.001548(11)
C5 0.007826(18) 0.004912(14) 0.005124(14) 0.001632(12) -0.000754(12)
-0.001817(11)
C6 0.00924(2) 0.005146(15) 0.005572(16) 0.001817(14) -0.001052(13) -0.001508(12)
H6 0.03071 0.01321 0.02174 0.00894 -0.00337 -0.00618
C7 0.008165(18) 0.005097(14) 0.005167(14) 0.001146(13) -0.000891(12)
-0.001105(11)
C8 0.009029(19) 0.005503(15) 0.004834(14) 0.001710(13) -0.000756(13)
-0.001386(12)
H8 0.03313 0.02196 0.01216 0.00545 -0.00059 -0.00840
C9 0.006786(17) 0.004471(13) 0.004625(14) 0.001058(11) -0.000502(11)
-0.001440(10)
C10 0.007222(18) 0.004605(14) 0.004586(14) 0.001378(12) -0.000478(12)
-0.001513(11)
C11 0.00719(6) 0.00449(4) 0.00603(5) 0.00152(4) -0.00095(4) -0.00202(3)
C12 0.00922(6) 0.00542(4) 0.00621(5) 0.00278(4) -0.00148(4) -0.00234(4)
H12 0.03511 0.01766 0.01511 0.01000 -0.00788 -0.00204
C13 0.00921(6) 0.00549(5) 0.00609(5) 0.00278(4) -0.00166(4) -0.00241(4)
C14 0.00826(6) 0.00502(4) 0.00681(5) 0.00218(4) -0.00161(4) -0.00230(4)
C15 0.00950(2) 0.005389(14) 0.006134(16) 0.002195(14) -0.001448(13)
-0.001908(12)
C16 0.00968(2) 0.005518(15) 0.005993(16) 0.002205(14) -0.001387(13)
-0.002070(12)
H16 0.03777 0.02324 0.01243 0.00722 -0.00538 -0.00848
OW2 0.01225(7) 0.00651(5) 0.00899(5) 0.00242(4) -0.00132(5) -0.00165(3)
OW3 0.01477(7) 0.00821(5) 0.01149(6) 0.00213(5) -0.00013(6) -0.00142(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0017 0.0001
'Clementi & Roetti 1974. Atomic Data & Nuclear Data Tables. 14, 177'
H H 0.0000 0.0000
'Clementi & Roetti 1974. Atomic Data & Nuclear Data Tables. 14, 177'
O O -0.0031 0.0002
'Clementi & Roetti 1974. Atomic Data & Nuclear Data Tables. 14, 177'
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 O13a HO13a 111.60(3) . . . ?
C15 O13b HO13b 109.48(4) . . . ?
C9 O1 C2 122.41(4) . . . ?
C3 O3 H3 109.87(4) . . . ?
C5 O5 H5 107.24(4) . . . ?
C7 O7 H7 109.53(3) . . . ?
C14 O14 H14 108.05(3) . . . ?
O1 C2 C3 120.26(4) . . . ?
O1 C2 C11 112.35(3) . . . ?
C3 C2 C11 127.382(13) . . . ?
O3 C3 C2 121.79(5) . . . ?
O3 C3 C4 117.86(3) . . . ?
C2 C3 C4 120.321(11) . . . ?
O4 C4 C3 120.425(11) . . . ?
O4 C4 C10 122.47(5) . . . ?
C3 C4 C10 117.10(3) . . . ?
O5 C5 C10 119.099(14) . . . ?
O5 C5 C6 119.95(5) . . . ?
C10 C5 C6 120.95(4) . . . ?
C5 C6 C7 119.26(4) . . . ?
C5 C6 H6 120.02(3) . . . ?
C7 C6 H6 120.713(15) . . . ?
O7 C7 C8 118.33(3) . . . ?
O7 C7 C6 120.10(5) . . . ?
C8 C7 C6 121.566(16) . . . ?
C9 C8 C7 117.78(3) . . . ?
C9 C8 H8 121.01(5) . . . ?
C7 C8 H8 121.202(16) . . . ?
O1 C9 C10 119.837(15) . . . ?
O1 C9 C8 117.76(3) . . . ?
C10 C9 C8 122.40(5) . . . ?
C9 C10 C5 118.003(14) . . . ?
C9 C10 C4 120.03(4) . . . ?
C5 C10 C4 121.97(4) . . . ?
C2 C11 C16 121.76(4) . . . ?
C2 C11 C12 119.366(12) . . . ?
C16 C11 C12 118.86(4) . . . ?
C13 C12 C11 120.445(13) . . . ?
C13 C12 H12 118.68(4) . . . ?
C11 C12 H12 120.88(4) . . . ?
O13a C13 C14 117.37(4) . . . ?
O13a C13 C12 122.333(11) . . . ?
C14 C13 C12 120.30(4) . . . ?
O14 C14 C13 118.32(4) . . . ?
O14 C14 C15 122.380(14) . . . ?
C13 C14 C15 119.30(4) . . . ?
C14 C15 C16 120.807(10) . . . ?
C14 C15 H15a 119.27(4) . . . ?
C16 C15 H15a 119.92(4) . . . ?
C11 C16 C15 120.27(4) . . . ?
C11 C16 H16 121.55(4) . . . ?
C15 C16 H16 118.177(12) . . . ?
HW2A OW2 HW2B 102.76(3) . . . ?
HW3B OW3 HW3A 100.92(2) . . . ?
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
O13a C13 1.3724(6) . ?
O13a HO13a 0.9826(6) . ?
O13b C15 1.2335(8) . ?
O13b HO13b 0.9892(4) . ?
O1 C9 1.3582(7) . ?
O1 C2 1.3693(9) . ?
O3 C3 1.3578(9) . ?
O3 H3 0.9721(3) . ?
O4 C4 1.2714(6) . ?
O5 C5 1.3527(6) . ?
O5 H5 0.9720(6) . ?
O7 C7 1.3545(9) . ?
O7 H7 0.9767(5) . ?
O14 C14 1.3645(6) . ?
O14 H14 0.9782(6) . ?
C2 C3 1.3820(6) . ?
C2 C11 1.4642(7) . ?
C3 C4 1.4383(7) . ?
C4 C10 1.4353(9) . ?
C5 C10 1.4190(7) . ?
C5 C6 1.3827(9) . ?
C6 C7 1.4115(6) . ?
C6 H6 1.0815(5) . ?
C7 C8 1.3995(7) . ?
C8 C9 1.3976(9) . ?
C8 H8 1.0743(5) . ?
C9 C10 1.4041(6) . ?
C11 C16 1.4133(9) . ?
C11 C12 1.4171(6) . ?
C12 C13 1.3913(6) . ?
C12 H12 1.0677(7) . ?
C13 C14 1.4113(9) . ?
C14 C15 1.4011(6) . ?
C15 C16 1.3915(6) . ?
C15 H15a 1.1105(7) . ?
C16 H16 1.0718(5) . ?
OW2 HW2A 0.9574(6) . ?
OW2 HW2B 0.9589(5) . ?
OW3 HW3B 0.9548(4) . ?
OW3 HW3A 0.9605(5) . ?
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
O7 H7 OW3 0.9767(5) 1.8898(9) 2.8664(13) 179.01(4) 1_455
C6 H6 OW3 1.0815(5) 2.5319(16) 3.345(2) 131.22(4) 1_455
OW3 HW3A O14 0.9605(5) 1.9167(9) 2.8611(14) 167.12(4) 1_465
O3 H3 O4 0.9721(3) 2.2977(13) 2.7188(13) 105.15(3) 1
O5 H5 O4 0.9720(6) 1.6882(10) 2.5761(16) 149.99(5) 1
O14 H14 O13b 0.9782(6) 2.2997(9) 2.7549(12) 107.38(4) 1
C13 H13b O13a 1.0823(5) 0.29812(11) 1.3724(6) 164.99(4) 1
C15 H15a O13b 1.1105(7) 0.16772(11) 1.2335(8) 134.28(5) 1
C16 H16 O3 1.0718(5) 2.1132(9) 2.8227(11) 121.296(14) 1
OW3 HW3B O13a 0.9548(4) 1.9896(8) 2.9100(12) 161.26(4) 1_565
O14 H14 OW2 0.9782(6) 1.7416(11) 2.7195(17) 178.21(5) 1_645
C15 H15a OW2 1.1105(7) 2.4490(12) 3.2567(18) 128.35(4) 1_645
OW2 HW2B O5 0.9589(5) 1.7854(9) 2.7435(13) 177.26(4) 1_655
OW2 HW2A O4 0.9574(6) 1.8927(12) 2.8188(17) 161.98(4) 2_666
O13a HO13a OW3 0.9826(6) 1.8037(10) 2.7589(16) 163.17(4) 2_765
O3 H3 OW2 0.9721(3) 1.9281(7) 2.8515(10) 157.70(3) 2_766
OW3 HW3B O13a 0.9548(4) 2.5271(15) 3.1076(18) 119.27(3) 2_865
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O13a C13 C14 O14 . . . . -0.723887(5) ?
O13a C13 C14 C15 . . . . 179.718826(6) ?
O13a C13 C12 C11 . . . . 179.134521(2) ?
O13a C13 C12 H12 . . . . -0.685570(2) ?
HO13a O13a C13 C14 . . . . 166.270447(8) ?
HO13a O13a C13 C12 . . . . -13.970394(2) ?
O13b C15 C14 O14 . . . . -4.751925(9) ?
O13b C15 C14 C13 . . . . 174.786911(9) ?
O13b C15 C16 C11 . . . . -174.54208(3) ?
O13b C15 C16 H16 . . . . 5.99374(3) ?
HO13b O13b C15 C14 . . . . 179.999985(10) ?
HO13b O13b C15 C16 . . . . -5.979534(8) ?
O1 C9 C10 C5 . . . . -179.236115(2) ?
O1 C9 C10 C4 . . . . 0.488589(2) ?
O1 C9 C8 C7 . . . . 179.928665(2) ?
O1 C9 C8 H8 . . . . 0.847653(2) ?
O1 C2 C3 O3 . . . . 179.0469360(17 ?
O1 C2 C3 C4 . . . . 1.0903805(16) ?
O1 C2 C11 C16 . . . . 174.8781280(16 ?
O1 C2 C11 C12 . . . . -6.3374104(17) ?
O3 C3 C2 C11 . . . . 0.4356619(19) ?
O3 C3 C4 O4 . . . . 0.245493(2) ?
O3 C3 C4 C10 . . . . 179.786011(2) ?
H3 O3 C3 C2 . . . . 158.7595980(6) ?
H3 O3 C3 C4 . . . . -23.2352409(3) ?
O4 C4 C3 C2 . . . . 178.281815(2) ?
O4 C4 C10 C9 . . . . -179.076126(2) ?
O4 C4 C10 C5 . . . . 0.637351(2) ?
O5 C5 C10 C9 . . . . 178.107925(3) ?
O5 C5 C10 C4 . . . . -1.611434(3) ?
O5 C5 C6 C7 . . . . -177.439438(3) ?
O5 C5 C6 H6 . . . . 1.800702(3) ?
H5 O5 C5 C10 . . . . -0.935864(2) ?
H5 O5 C5 C6 . . . . 178.6979370(18 ?
O7 C7 C8 C9 . . . . -179.3794400(19 ?
O7 C7 C8 H8 . . . . -0.2980513(18) ?
O7 C7 C6 C5 . . . . 178.0019680(16 ?
O7 C7 C6 H6 . . . . -1.2327350(16) ?
H7 O7 C7 C8 . . . . 175.6896510(16 ?
H7 O7 C7 C6 . . . . -3.8088403(14) ?
O14 C14 C13 C12 . . . . 179.512604(8) ?
O14 C14 C15 C16 . . . . -178.658691(8) ?
O14 C14 C15 H15a . . . . 1.596426(9) ?
H14 O14 C14 C13 . . . . 174.807281(12) ?
H14 O14 C14 C15 . . . . -5.649583(16) ?
C2 O1 C9 C10 . . . . -1.711893(2) ?
C2 O1 C9 C8 . . . . 178.908173(2) ?
C2 C3 C4 C10 . . . . -2.179244(2) ?
C2 C11 C16 C15 . . . . 178.187805(5) ?
C2 C11 C16 H16 . . . . -2.3664536(16) ?
C2 C11 C12 C13 . . . . -177.3881990(19 ?
C2 C11 C12 H12 . . . . 2.4280157(18) ?
C3 C2 O1 C9 . . . . 0.9191971(19) ?
C3 C2 C11 C16 . . . . -6.4187541(17) ?
C3 C2 C11 C12 . . . . 172.3657230(18 ?
C3 C4 C10 C9 . . . . 1.394795(2) ?
C3 C4 C10 C5 . . . . -178.891632(2) ?
C4 C3 C2 C11 . . . . -177.5211490(19 ?
C4 C10 C9 C8 . . . . 179.839279(3) ?
C4 C10 C5 C6 . . . . 178.758713(2) ?
C5 C10 C9 C8 . . . . 0.113641(3) ?
C5 C6 C7 C8 . . . . -1.480019(2) ?
C6 C5 C10 C9 . . . . -1.521871(2) ?
C6 C7 C8 C9 . . . . 0.111906(2) ?
C6 C7 C8 H8 . . . . 179.192780(2) ?
H6 C6 C5 C10 . . . . -178.5724640(19 ?
H6 C6 C7 C8 . . . . 179.2853550(17 ?
C7 C8 C9 C10 . . . . 0.567862(2) ?
C7 C6 C5 C10 . . . . 2.1874013(18) ?
H8 C8 C9 C10 . . . . -178.515610(2) ?
C9 O1 C2 C11 . . . . 179.725876(2) ?
C11 C16 C15 C14 . . . . -0.548583(7) ?
C11 C16 C15 H15a . . . . 179.194473(5) ?
C11 C12 C13 C14 . . . . -1.113466(5) ?
C12 C13 C14 C15 . . . . -0.039565(7) ?
C12 C11 C16 C15 . . . . -0.602634(4) ?
C12 C11 C16 H16 . . . . 178.843079(2) ?
H12 C12 C13 C14 . . . . 179.066437(5) ?
H12 C12 C11 C16 . . . . -178.7521060(15 ?
C13 C14 C15 C16 . . . . 0.880045(9) ?
C13 C14 C15 H15a . . . . -178.864761(9) ?
C13 C12 C11 C16 . . . . 1.431628(2) ?
H13b C13 C14 C15 . . . . 176.541687(10) ?
C14 C15 C16 H16 . . . . 179.999985(11) ?
H15a C15 C16 H16 . . . . -0.269795(6) ?
loop_
_publcif_info_cif.paper_type
CB
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_exptl_table_header_item
?
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{3882666b-713c-41ad-9769-25f2d54f1308} '_publcif_info_datablock.publ_exptl'

_cod_database_fobs_code 2312718