##############################################################################
### ###
### Electronic paper (Acta Crystallographica Section E) ###
### ###
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# #
# This CIF contains the data in a paper accepted for publication in Acta #
# Crystallographica Section E. It conforms to the requirements of Notes #
# for Authors for Section E, and has been peer reviewed under the auspices #
# of the IUCr Commission on Journals. #
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# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4. #
# #
# Software is freely available for graphical display of the structure(s) in #
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data_global
_audit_creation_method 'SHELXL-97 and IUCr-template'
_journal_date_recd_electronic 2009-11-07
_journal_date_accepted 2009-11-16
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2009
_journal_volume 65
_journal_issue 12
_journal_page_first o3162
_journal_page_last o3163
_journal_paper_category QO
_journal_coeditor_code TK2569
_publ_contact_author_name 'R\"udiger W. Seidel'
_publ_contact_author_address
;
Lehrstuhl f\"ur Analytische Chemie
Ruhr-Universit\"at Bochum
Universit\"atsstrasse 150
44780 Bochum
;
_publ_contact_author_email ruediger.seidel@rub.de
_publ_contact_author_fax '49 234 3214420'
_publ_contact_author_phone '49 234 3224196'
_publ_section_title
;
\b-Cyclodextrin 10.41-hydrate
;
loop_
_publ_author_name
_publ_author_address
'Seidel, R\"udiger W.'
;
Lehrstuhl f\"ur Analytische Chemie
Ruhr-Universit\"at Bochum
Universit\"atsstrasse 150
44780 Bochum, Germany
;
'Koleva, Bojidarka B.'
;
Department of Analytical Chemistry
University of Sofia St. Kliment Ohridski
J. Bourchier Blvd. 1
1164 Sofia, Bulgaria
;
data_I
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
\b-cyclodextrin 10.41-hydrate
;
_chemical_name_common ?
_chemical_formula_moiety 'C42 H70 O35, 10.41(H2 O)'
_chemical_formula_sum 'C42 H90.82 O45.41'
_chemical_formula_iupac 'C42 H70 O35, 10.41H2 O'
_chemical_formula_weight 1322.53
_chemical_melting_point ?
_symmetry_cell_setting 'monoclinic'
_symmetry_space_group_name_H-M 'P 21'
_symmetry_space_group_name_Hall 'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 20.8353(4)
_cell_length_b 9.93970(10)
_cell_length_c 15.2043(3)
_cell_angle_alpha 90
_cell_angle_beta 110.630(2)
_cell_angle_gamma 90
_cell_volume 2946.84(9)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 20832
_cell_measurement_theta_min 2.6719
_cell_measurement_theta_max 28.1317
_cell_measurement_temperature 110(2)
_exptl_crystal_description prism
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.37
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.28
_exptl_crystal_density_diffrn 1.490
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1412
_exptl_absorpt_coefficient_mu 0.137
_exptl_absorpt_correction_type 'multi-scan'
_exptl_absorpt_process_details
;
(ABSPACK in CrysAlis Pro; Oxford Diffraction, 2009)
;
_exptl_absorpt_correction_T_min 0.951
_exptl_absorpt_correction_T_max 0.963
_exptl_special_details
;
;
_diffrn_ambient_temperature 110(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 8.4171
_diffrn_reflns_number 40031
_diffrn_reflns_av_R_equivalents 0.026
_diffrn_reflns_av_sigmaI/netI 0.029
_diffrn_reflns_theta_min 2.9
_diffrn_reflns_theta_max 27.5
_diffrn_reflns_theta_full 27.5
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F^2^, conventional
R-factors R are based on F, with F set to zero for
negative F^2^. The threshold expression of F^2^ >
\s(F^2^) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F^2^ are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total 7019
_reflns_number_gt 6090
_reflns_threshold_expression 'I>2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.038
_refine_ls_R_factor_gt 0.032
_refine_ls_wR_factor_gt 0.080
_refine_ls_wR_factor_ref 0.081
_refine_ls_goodness_of_fit_ref 0.99
_refine_ls_restrained_S_all 0.99
_refine_ls_number_reflns 7019
_refine_ls_number_parameters 868
_refine_ls_number_restraints 36
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary
;
the initial coordinates of the \b-cyclodextrin scaffold were taken from Lindner
& Saenger (1982)
;
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.39
_refine_diff_density_min -0.24
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack ?
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'
_computing_data_collection 'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_cell_refinement 'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_data_reduction 'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_structure_solution
;
initial coordinates of the \b-cyclodextrin scaffold from Lindner & Saenger
(1982)
;
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Brandenburg, 2009)'
_computing_publication_material 'enCIFer (Allen et al., 2004)'
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_disorder_assembly
_atom_site_disorder_group
O O1 0.43109(9) 0.4795(2) 0.06964(12) 0.0237(4) Uani d . 1 . .
H H1A 0.4451 0.4043 0.0941 0.028 Uiso calc R 1 . .
O O2 0.41763(9) 0.4374(2) -0.12954(12) 0.0238(4) Uani d . 1 . .
H H2A 0.3885 0.3942 -0.1142 0.029 Uiso calc R 1 . .
O O3 0.54177(8) 0.39543(17) -0.15508(11) 0.0154(3) Uani d . 1 . .
O O4 0.59435(9) 0.59993(18) 0.05896(11) 0.0207(4) Uani d . 1 A .
O O5 0.64406(13) 0.6978(2) -0.07616(17) 0.0368(7) Uani d PDU 0.917(5) A 1
H H5A 0.6758 0.7505 -0.0465 0.044 Uiso calc PR 0.917(5) A 1
C C6 0.65945(15) 0.5684(3) -0.03927(19) 0.0294(6) Uani d PDU 0.917(5) A 1
H H6A 0.7026 0.5711 0.0158 0.035 Uiso calc PR 0.917(5) A 1
H H6B 0.6669 0.5091 -0.0871 0.035 Uiso calc PR 0.917(5) A 1
O O5' 0.7150(11) 0.620(3) 0.0298(15) 0.040(5) Uani d PDU 0.083(5) A 2
H H5' 0.7025 0.6822 0.0573 0.059 Uiso calc PR 0.083(5) A 2
C C6' 0.65945(15) 0.5684(3) -0.03927(19) 0.0294(6) Uani d P 0.083(5) A 2
H H6A' 0.6756 0.4974 -0.0722 0.035 Uiso calc PR 0.083(5) A 2
H H6B' 0.6391 0.6408 -0.0854 0.035 Uiso calc PR 0.083(5) A 2
O O6 0.58391(8) 0.16416(19) 0.41646(12) 0.0189(4) Uani d . 1 . .
H H6C 0.6091 0.1016 0.4102 0.023 Uiso calc R 1 . .
O O7 0.49901(9) 0.3003(2) 0.24149(13) 0.0260(4) Uani d . 1 . .
H H7A 0.4845 0.3179 0.2853 0.031 Uiso calc R 1 . .
O O8 0.57078(8) 0.42611(17) 0.14463(11) 0.0157(3) Uani d . 1 . .
O O9 0.70256(8) 0.41357(17) 0.38138(11) 0.0166(4) Uani d . 1 . .
O O11 0.77159(9) -0.27659(17) 0.45930(12) 0.0177(4) Uani d . 1 . .
H H11A 0.7667 -0.3267 0.5010 0.021 Uiso calc R 1 . .
O O12 0.66776(8) -0.06812(18) 0.43729(12) 0.0178(4) Uani d . 1 . .
H H12C 0.6448 -0.1177 0.3926 0.021 Uiso calc R 1 . .
O O13 0.70736(8) 0.18126(17) 0.39046(11) 0.0146(3) Uani d . 1 . .
O O14 0.87332(8) 0.03010(17) 0.53239(11) 0.0152(3) Uani d . 1 . .
O O15 0.84497(9) 0.26449(19) 0.60728(12) 0.0232(4) Uani d . 1 . .
H H15A 0.8597 0.3377 0.6346 0.028 Uiso calc R 1 . .
O O16 0.92260(9) -0.49406(17) 0.26437(12) 0.0186(4) Uani d . 1 . .
H H16A 0.9550 -0.5406 0.2600 0.022 Uiso calc R 1 . .
O O17 0.87877(8) -0.40676(18) 0.41115(11) 0.0179(4) Uani d . 1 . .
H H17A 0.8453 -0.3770 0.4238 0.022 Uiso calc R 1 . .
O O18 0.86032(8) -0.11803(17) 0.40904(11) 0.0139(3) Uani d . 1 . .
O O19 0.99620(8) -0.15637(17) 0.31140(11) 0.0154(3) Uani d . 1 . .
O O20 0.99809(10) 0.12933(19) 0.33502(15) 0.0297(4) Uani d . 1 . .
H H20A 0.9622 0.1707 0.3035 0.045 Uiso calc R 1 . .
O O21 0.79734(9) -0.43799(18) -0.12551(11) 0.0195(4) Uani d . 1 . .
H H21A 0.7657 -0.3839 -0.1532 0.023 Uiso calc R 1 . .
O O22 0.85197(9) -0.47175(18) 0.07245(12) 0.0198(4) Uani d . 1 . .
H H22A 0.8666 -0.4645 0.1313 0.024 Uiso calc R 1 . .
O O23 0.91264(8) -0.24262(17) 0.17883(11) 0.0150(3) Uani d . 1 . .
O O24 0.91996(8) -0.15919(18) -0.05281(11) 0.0175(4) Uani d . 1 . .
O O25 1.04195(9) -0.1142(2) 0.11668(12) 0.0235(4) Uani d . 1 . .
H H25A 1.0516 -0.1317 0.0687 0.028 Uiso calc R 1 . .
O O26 0.57670(8) -0.12304(18) -0.36578(12) 0.0212(4) Uani d . 1 . .
H H26A 0.5657 -0.1960 -0.3951 0.025 Uiso calc R 1 . .
O O27 0.68202(9) -0.29122(18) -0.23675(13) 0.0230(4) Uani d . 1 . .
H H27A 0.6554 -0.3069 -0.2073 0.035 Uiso calc R 1 . .
O O28 0.80158(8) -0.15711(17) -0.12746(11) 0.0147(3) Uani d . 1 . .
O O29 0.73057(8) 0.07842(18) -0.32427(11) 0.0159(3) Uani d . 1 . .
O O30 0.87316(9) 0.0327(2) -0.27399(13) 0.0238(4) Uani d . 1 . .
H H30C 0.8677 0.0859 -0.3190 0.036(9) Uiso calc R 1 . .
O O31 0.42147(8) 0.30039(18) -0.29183(12) 0.0194(4) Uani d . 1 . .
H H31A 0.4242 0.3384 -0.2413 0.023 Uiso calc R 1 . .
O O32 0.48828(8) 0.09599(17) -0.36044(11) 0.0174(3) Uani d . 1 . .
H H32A 0.5137 0.0286 -0.3554 0.021 Uiso calc R 1 . .
O O33 0.63304(8) 0.11283(16) -0.28602(11) 0.0137(3) Uani d . 1 . .
O O34 0.58413(8) 0.46343(16) -0.27119(11) 0.0153(3) Uani d . 1 . .
O O35 0.65236(8) 0.44776(18) -0.39480(11) 0.0178(4) Uani d . 1 . .
H H35A 0.6216 0.5041 -0.3976 0.021 Uiso calc R 1 . .
O O36 0.70072(9) 0.65475(19) 0.26713(13) 0.0251(4) Uani d . 1 . .
H H36 0.7188 0.6715 0.3248 0.030 Uiso calc R 1 . .
C C1 0.54900(12) 0.5510(3) 0.10087(16) 0.0164(5) Uani d . 1 . .
H H1 0.5462 0.6171 0.1489 0.020 Uiso calc R 1 . .
C C2 0.47733(12) 0.5308(3) 0.02720(16) 0.0170(5) Uani d . 1 . .
H H2 0.4599 0.6208 -0.0002 0.020 Uiso calc R 1 . .
C C3 0.48101(11) 0.4415(3) -0.05196(15) 0.0163(5) Uani d . 1 . .
H H3 0.4935 0.3481 -0.0274 0.020 Uiso calc R 1 . .
C C4 0.53467(12) 0.4933(2) -0.08968(16) 0.0162(5) Uani d . 1 A .
H H4 0.5197 0.5815 -0.1221 0.019 Uiso calc R 1 . .
C C5 0.60351(12) 0.5095(3) -0.00976(16) 0.0181(5) Uani d . 1 . .
H H5 0.6187 0.4199 0.0202 0.022 Uiso calc R 1 A 1
C C7 0.68164(12) 0.2994(2) 0.41849(16) 0.0161(5) Uani d . 1 . .
H H7 0.6998 0.3052 0.4886 0.019 Uiso calc R 1 . .
C C8 0.60300(12) 0.2877(3) 0.38360(16) 0.0159(5) Uani d . 1 . .
H H8 0.5850 0.3637 0.4113 0.019 Uiso calc R 1 . .
C C9 0.57234(12) 0.2998(3) 0.27719(16) 0.0160(5) Uani d . 1 . .
H H9 0.5878 0.2200 0.2499 0.019 Uiso calc R 1 . .
C C10 0.60044(12) 0.4254(3) 0.24549(15) 0.0157(5) Uani d . 1 . .
H H10 0.5866 0.5080 0.2719 0.019 Uiso calc R 1 . .
C C11 0.67885(12) 0.4133(3) 0.28019(16) 0.0164(5) Uani d . 1 . .
H H11 0.6908 0.3246 0.2590 0.020 Uiso calc R 1 . .
C C12 0.71698(13) 0.5221(3) 0.24961(18) 0.0209(5) Uani d . 1 . .
H H12A 0.7668 0.5079 0.2822 0.025 Uiso calc R 1 . .
H H12B 0.7073 0.5122 0.1813 0.025 Uiso calc R 1 . .
C C13 0.85802(12) -0.1031(2) 0.49974(16) 0.0142(5) Uani d . 1 . .
H H13 0.8922 -0.1654 0.5436 0.017 Uiso calc R 1 . .
C C14 0.78611(12) -0.1431(2) 0.49470(16) 0.0151(5) Uani d . 1 . .
H H14 0.7839 -0.1397 0.5593 0.018 Uiso calc R 1 . .
C C15 0.73386(11) -0.0454(2) 0.43193(16) 0.0142(5) Uani d . 1 . .
H H15 0.7313 -0.0574 0.3655 0.017 Uiso calc R 1 . .
C C16 0.75377(11) 0.0987(2) 0.46217(16) 0.0140(5) Uani d . 1 . .
H H16 0.7475 0.1162 0.5234 0.017 Uiso calc R 1 . .
C C17 0.82787(12) 0.1293(2) 0.47187(16) 0.0142(5) Uani d . 1 . .
H H17 0.8322 0.1264 0.4084 0.017 Uiso calc R 1 . .
C C18 0.85261(13) 0.2635(3) 0.51694(17) 0.0188(5) Uani d . 1 . .
H H18A 0.9013 0.2770 0.5244 0.023 Uiso calc R 1 . .
H H18B 0.8253 0.3369 0.4772 0.023 Uiso calc R 1 . .
C C19 0.97083(12) -0.2731(2) 0.25883(16) 0.0146(5) Uani d . 1 . .
H H19 1.0073 -0.3129 0.2382 0.018 Uiso calc R 1 . .
C C20 0.94960(12) -0.3762(2) 0.31866(16) 0.0152(5) Uani d . 1 . .
H H20 0.9903 -0.4010 0.3749 0.018 Uiso calc R 1 . .
C C21 0.89510(11) -0.3156(2) 0.35013(15) 0.0138(5) Uani d . 1 . .
H H21 0.8530 -0.3000 0.2936 0.017 Uiso calc R 1 . .
C C22 0.91912(11) -0.1811(2) 0.39884(15) 0.0129(5) Uani d . 1 . .
H H22 0.9551 -0.1961 0.4620 0.016 Uiso calc R 1 . .
C C23 0.94635(11) -0.0876(2) 0.34095(16) 0.0139(5) Uani d . 1 . .
H H23 0.9074 -0.0573 0.2842 0.017 Uiso calc R 1 . .
C C24 0.98264(13) 0.0341(3) 0.39539(18) 0.0198(5) Uani d . 1 . .
H H24A 0.9532 0.0773 0.4261 0.024 Uiso calc R 1 . .
H H24B 1.0257 0.0054 0.4451 0.024 Uiso calc R 1 . .
C C25 0.86255(12) -0.2313(2) -0.11112(16) 0.0152(5) Uani d . 1 . .
H H25 0.8683 -0.2489 -0.1727 0.018 Uiso calc R 1 . .
C C26 0.85543(12) -0.3653(2) -0.06681(16) 0.0162(5) Uani d . 1 . .
H H26 0.8971 -0.4200 -0.0604 0.019 Uiso calc R 1 . .
C C27 0.85369(12) -0.3433(2) 0.03141(16) 0.0150(5) Uani d . 1 . .
H H27 0.8115 -0.2916 0.0270 0.018 Uiso calc R 1 . .
C C28 0.91664(12) -0.2633(2) 0.08818(16) 0.0143(5) Uani d . 1 . .
H H28 0.9589 -0.3157 0.0942 0.017 Uiso calc R 1 . .
C C29 0.91743(12) -0.1305(3) 0.03929(16) 0.0166(5) Uani d . 1 . .
H H29 0.8745 -0.0795 0.0321 0.020 Uiso calc R 1 . .
C C30 0.97906(12) -0.0434(3) 0.08994(18) 0.0206(5) Uani d . 1 . .
H H30A 0.9807 0.0323 0.0485 0.025 Uiso calc R 1 . .
H H30B 0.9734 -0.0050 0.1468 0.025 Uiso calc R 1 . .
C C31 0.66024(11) 0.0500(2) -0.34856(16) 0.0147(5) Uani d . 1 . .
H H31 0.6349 0.0818 -0.4141 0.018 Uiso calc R 1 . .
C C32 0.64881(12) -0.1005(3) -0.34219(16) 0.0163(5) Uani d . 1 . .
H H32 0.6648 -0.1489 -0.3883 0.020 Uiso calc R 1 . .
C C33 0.68954(12) -0.1496(2) -0.24365(16) 0.0156(5) Uani d . 1 . .
H H33 0.6725 -0.1033 -0.1977 0.019 Uiso calc R 1 . .
C C34 0.76454(12) -0.1134(2) -0.22174(15) 0.0135(5) Uani d . 1 . .
H H34 0.7824 -0.1603 -0.2666 0.016 Uiso calc R 1 . .
C C35 0.77121(11) 0.0386(2) -0.22966(16) 0.0148(5) Uani d . 1 . .
H H35 0.7525 0.0837 -0.1850 0.018 Uiso calc R 1 . .
C C36 0.84314(12) 0.0888(3) -0.21093(17) 0.0185(5) Uani d . 1 . .
H H36A 0.8422 0.1881 -0.2169 0.022 Uiso calc R 1 . .
H H36B 0.8721 0.0659 -0.1456 0.022 Uiso calc R 1 . .
C C37 0.52490(12) 0.4371(2) -0.24926(15) 0.0144(5) Uani d . 1 . .
H H37 0.4964 0.5206 -0.2598 0.017 Uiso calc R 1 . .
C C38 0.48255(11) 0.3247(2) -0.31085(16) 0.0145(5) Uani d . 1 . .
H H38 0.4692 0.3534 -0.3780 0.017 Uiso calc R 1 . .
C C39 0.52559(12) 0.1989(2) -0.29771(16) 0.0139(5) Uani d . 1 . .
H H39 0.5379 0.1666 -0.2315 0.017 Uiso calc R 1 . .
C C40 0.59077(11) 0.2293(2) -0.31679(16) 0.0125(4) Uani d . 1 . .
H H40 0.5799 0.2433 -0.3856 0.015 Uiso calc R 1 . .
C C41 0.62916(12) 0.3508(2) -0.26224(16) 0.0138(5) Uani d . 1 . .
H H41 0.6515 0.3266 -0.1944 0.017 Uiso calc R 1 . .
C C42 0.68285(12) 0.3999(2) -0.30030(16) 0.0157(5) Uani d . 1 . .
H H42A 0.7096 0.4734 -0.2599 0.019 Uiso calc R 1 . .
H H42B 0.7149 0.3255 -0.2986 0.019 Uiso calc R 1 . .
O O37 0.45907(9) 0.13938(19) 0.45062(12) 0.0208(4) Uani d D 1 . .
H H37A 0.4952(11) 0.126(3) 0.4413(19) 0.025 Uiso d D 1 . .
H H37B 0.4700(14) 0.134(3) 0.5099(13) 0.025 Uiso d D 1 . .
O O38 1.02376(10) 0.3565(2) 0.23620(13) 0.0248(4) Uani d D 1 . .
H H38A 1.0311(15) 0.290(2) 0.271(2) 0.030 Uiso d D 1 . .
H H38B 1.0561(13) 0.409(3) 0.250(2) 0.030 Uiso d D 1 . .
O O39 0.92858(10) 0.3215(2) 0.04040(14) 0.0299(4) Uani d D 1 . .
H H39A 0.9075(15) 0.387(3) 0.055(2) 0.036 Uiso d D 1 . .
H H39B 0.9646(12) 0.311(3) 0.0898(17) 0.036 Uiso d D 1 . .
O O40 0.75974(10) -0.3861(2) 0.60776(14) 0.0293(4) Uani d D 1 . .
H H40A 0.7851(14) -0.456(3) 0.607(2) 0.035 Uiso d D 1 . .
H H40B 0.7227(11) -0.433(3) 0.599(2) 0.035 Uiso d D 1 . .
O O41 1.11226(10) 0.0083(2) 0.28708(14) 0.0282(4) Uani d D 1 . .
H H41A 1.0788(13) 0.038(3) 0.300(2) 0.034 Uiso d D 1 . .
H H41B 1.0977(15) -0.029(3) 0.2341(16) 0.034 Uiso d D 1 . .
O O42 0.77658(12) 0.2871(2) -0.07080(17) 0.0400(5) Uani d D 1 . .
H H42C 0.7787(17) 0.367(2) -0.090(2) 0.048 Uiso d D 1 . .
H H42D 0.8137(12) 0.263(4) -0.036(2) 0.048 Uiso d D 1 . .
O O43 0.87096(13) 0.2433(3) 0.2749(2) 0.0585(7) Uani d . 1 . .
O O44 0.74718(14) 0.1038(3) 0.1869(2) 0.0523(8) Uani d P 0.903(5) . .
O O44' 0.7000(14) 0.109(3) 0.1997(19) 0.0523(8) Uani d P 0.097(5) . .
O O45 0.70193(13) -0.1792(3) 0.1178(2) 0.0287(7) Uani d P 0.803(6) . .
O O45' 0.7106(6) -0.1310(13) 0.1604(9) 0.0287(7) Uani d P 0.197(6) . .
O O46 0.68237(15) 0.1660(4) 0.0002(3) 0.0502(11) Uani d P 0.884(9) . .
O O46' 0.6883(13) 0.103(3) -0.033(2) 0.0502(11) Uani d P 0.116(9) . .
O O47 0.7268(7) 0.8957(15) -0.0091(10) 0.044(5) Uiso d P 0.167(9) . .
O O48 0.8452(15) 0.143(3) 0.068(2) 0.043(11) Uiso d P 0.081(8) . .
O O49 0.7843(16) 0.013(3) 0.120(2) 0.030(12) Uiso d P 0.062(8) . .
O O50 0.8898(15) 0.167(3) 0.164(2) 0.022(11) Uiso d P 0.060(8) . .
O O51 0.744(3) 0.337(5) 0.111(3) 0.029(18) Uiso d P 0.039(8) . .
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 0.0206(9) 0.0320(11) 0.0213(9) 0.0035(8) 0.0110(8) -0.0001(8)
O2 0.0146(8) 0.0375(11) 0.0167(9) 0.0022(8) 0.0023(7) -0.0030(8)
O3 0.0204(8) 0.0150(8) 0.0118(7) 0.0038(7) 0.0069(6) 0.0017(6)
O4 0.0256(9) 0.0228(9) 0.0144(8) -0.0058(8) 0.0081(7) -0.0017(7)
O5 0.0467(15) 0.0275(13) 0.0468(15) -0.0080(11) 0.0296(12) 0.0026(11)
C6 0.0291(15) 0.0368(16) 0.0245(14) -0.0102(13) 0.0123(12) -0.0028(12)
O5' 0.027(8) 0.047(9) 0.041(9) -0.010(8) 0.007(7) 0.001(8)
C6' 0.0291(15) 0.0368(16) 0.0245(14) -0.0102(13) 0.0123(12) -0.0028(12)
O6 0.0178(8) 0.0206(9) 0.0211(9) 0.0032(7) 0.0105(7) 0.0046(7)
O7 0.0140(8) 0.0407(11) 0.0233(9) 0.0001(8) 0.0064(7) 0.0040(8)
O8 0.0183(8) 0.0170(8) 0.0108(8) 0.0007(7) 0.0040(6) -0.0001(7)
O9 0.0181(8) 0.0151(8) 0.0139(8) -0.0009(7) 0.0022(7) -0.0002(7)
O11 0.0233(9) 0.0139(8) 0.0186(9) -0.0024(7) 0.0108(7) 0.0014(7)
O12 0.0117(8) 0.0208(9) 0.0222(9) -0.0050(7) 0.0076(7) -0.0038(7)
O13 0.0135(8) 0.0162(8) 0.0116(7) 0.0030(7) 0.0014(6) 0.0004(6)
O14 0.0124(8) 0.0178(8) 0.0135(8) 0.0002(7) 0.0022(6) 0.0000(7)
O15 0.0275(10) 0.0203(9) 0.0218(9) -0.0042(8) 0.0087(8) -0.0072(7)
O16 0.0202(9) 0.0157(8) 0.0190(8) 0.0029(7) 0.0059(7) -0.0017(7)
O17 0.0179(8) 0.0180(9) 0.0205(8) 0.0006(7) 0.0099(7) 0.0040(7)
O18 0.0115(8) 0.0187(9) 0.0121(7) 0.0017(7) 0.0048(6) 0.0017(6)
O19 0.0112(8) 0.0188(8) 0.0176(8) -0.0009(7) 0.0068(6) -0.0027(7)
O20 0.0291(10) 0.0207(10) 0.0408(11) -0.0065(8) 0.0140(9) 0.0032(8)
O21 0.0190(9) 0.0173(9) 0.0159(8) 0.0014(7) -0.0016(7) -0.0001(7)
O22 0.0260(9) 0.0171(9) 0.0135(8) -0.0046(8) 0.0034(7) 0.0003(7)
O23 0.0124(8) 0.0206(9) 0.0113(8) 0.0028(7) 0.0032(6) -0.0001(7)
O24 0.0137(8) 0.0253(9) 0.0125(8) -0.0029(7) 0.0032(6) 0.0035(7)
O25 0.0164(8) 0.0309(11) 0.0211(9) -0.0048(8) 0.0040(7) 0.0014(8)
O26 0.0126(8) 0.0187(9) 0.0267(9) -0.0005(7) 0.0002(7) -0.0049(7)
O27 0.0184(9) 0.0159(9) 0.0314(10) -0.0015(7) 0.0047(8) 0.0052(8)
O28 0.0140(8) 0.0190(8) 0.0108(7) 0.0036(7) 0.0043(6) 0.0025(6)
O29 0.0122(8) 0.0206(9) 0.0151(8) 0.0015(7) 0.0048(6) 0.0050(7)
O30 0.0195(9) 0.0308(11) 0.0241(9) 0.0047(8) 0.0115(7) 0.0090(8)
O31 0.0135(8) 0.0268(10) 0.0194(8) 0.0015(7) 0.0075(7) -0.0013(7)
O32 0.0146(8) 0.0156(8) 0.0216(8) -0.0011(7) 0.0058(7) -0.0012(7)
O33 0.0156(8) 0.0132(8) 0.0130(8) 0.0046(7) 0.0059(6) 0.0029(6)
O34 0.0174(8) 0.0130(8) 0.0177(8) 0.0011(7) 0.0091(7) 0.0014(7)
O35 0.0177(8) 0.0200(9) 0.0171(8) 0.0030(7) 0.0077(7) 0.0030(7)
O36 0.0263(10) 0.0214(10) 0.0235(9) -0.0020(8) 0.0039(8) 0.0031(8)
C1 0.0205(12) 0.0173(12) 0.0136(11) -0.0005(10) 0.0086(9) -0.0013(9)
C2 0.0204(12) 0.0170(12) 0.0155(11) 0.0029(10) 0.0088(10) -0.0004(9)
C3 0.0151(11) 0.0195(12) 0.0124(11) 0.0032(10) 0.0023(9) -0.0003(9)
C4 0.0202(12) 0.0149(12) 0.0140(11) 0.0035(10) 0.0065(9) 0.0003(9)
C5 0.0198(12) 0.0225(13) 0.0134(11) -0.0017(10) 0.0076(10) -0.0016(10)
C7 0.0167(11) 0.0175(12) 0.0125(11) 0.0009(10) 0.0031(9) -0.0011(9)
C8 0.0149(11) 0.0175(12) 0.0153(11) 0.0032(10) 0.0054(9) 0.0018(9)
C9 0.0123(11) 0.0217(12) 0.0142(11) 0.0007(10) 0.0049(9) -0.0013(10)
C10 0.0154(11) 0.0199(12) 0.0108(11) 0.0011(10) 0.0033(9) -0.0008(9)
C11 0.0148(11) 0.0184(12) 0.0147(11) -0.0011(10) 0.0035(9) -0.0022(9)
C12 0.0160(12) 0.0268(14) 0.0175(12) -0.0034(11) 0.0032(10) 0.0008(10)
C13 0.0139(11) 0.0178(12) 0.0110(10) 0.0023(9) 0.0045(9) 0.0003(9)
C14 0.0166(11) 0.0160(11) 0.0144(11) -0.0012(9) 0.0075(9) 0.0000(9)
C15 0.0104(10) 0.0190(12) 0.0139(11) -0.0009(9) 0.0053(9) 0.0007(9)
C16 0.0119(11) 0.0163(12) 0.0130(10) 0.0001(9) 0.0036(8) 0.0017(9)
C17 0.0130(11) 0.0169(12) 0.0120(10) 0.0005(9) 0.0037(9) 0.0012(9)
C18 0.0182(12) 0.0176(12) 0.0194(12) -0.0037(10) 0.0051(10) -0.0018(10)
C19 0.0115(11) 0.0177(12) 0.0135(11) 0.0015(9) 0.0030(9) -0.0014(9)
C20 0.0150(11) 0.0159(12) 0.0130(11) 0.0016(9) 0.0029(9) 0.0000(9)
C21 0.0121(10) 0.0164(12) 0.0123(10) -0.0004(9) 0.0036(9) 0.0019(9)
C22 0.0093(10) 0.0162(12) 0.0127(10) 0.0020(9) 0.0030(8) 0.0001(9)
C23 0.0114(10) 0.0157(11) 0.0155(11) -0.0005(9) 0.0058(9) -0.0011(9)
C24 0.0168(12) 0.0188(12) 0.0252(13) -0.0043(10) 0.0093(10) -0.0028(10)
C25 0.0127(11) 0.0206(13) 0.0125(11) 0.0006(9) 0.0045(9) 0.0015(9)
C26 0.0160(11) 0.0164(12) 0.0144(11) 0.0030(9) 0.0031(9) -0.0005(9)
C27 0.0157(11) 0.0140(11) 0.0148(11) -0.0001(9) 0.0049(9) 0.0007(9)
C28 0.0137(11) 0.0166(11) 0.0129(11) 0.0001(9) 0.0049(9) -0.0015(9)
C29 0.0157(12) 0.0186(12) 0.0144(11) -0.0010(10) 0.0040(9) 0.0000(9)
C30 0.0198(12) 0.0188(13) 0.0212(12) -0.0037(10) 0.0046(10) 0.0033(10)
C31 0.0124(11) 0.0181(12) 0.0135(11) 0.0039(9) 0.0045(9) 0.0000(9)
C32 0.0118(11) 0.0179(12) 0.0171(11) 0.0010(9) 0.0023(9) -0.0025(10)
C33 0.0173(12) 0.0120(11) 0.0177(11) -0.0014(9) 0.0065(9) 0.0006(9)
C34 0.0143(11) 0.0163(12) 0.0099(10) 0.0020(9) 0.0041(8) 0.0015(9)
C35 0.0139(11) 0.0160(12) 0.0137(11) 0.0028(9) 0.0039(9) 0.0018(9)
C36 0.0173(12) 0.0161(12) 0.0207(12) -0.0007(10) 0.0051(9) 0.0033(10)
C37 0.0154(11) 0.0177(12) 0.0123(10) 0.0048(9) 0.0076(9) 0.0036(9)
C38 0.0107(11) 0.0201(12) 0.0135(11) 0.0022(9) 0.0053(9) 0.0031(9)
C39 0.0138(11) 0.0143(11) 0.0124(10) -0.0004(9) 0.0033(9) 0.0006(9)
C40 0.0120(11) 0.0121(11) 0.0141(11) 0.0028(9) 0.0053(9) 0.0025(9)
C41 0.0153(11) 0.0132(11) 0.0118(10) 0.0019(9) 0.0035(9) 0.0011(9)
C42 0.0157(11) 0.0137(11) 0.0163(11) -0.0007(9) 0.0039(9) -0.0001(9)
O37 0.0183(9) 0.0247(10) 0.0182(9) 0.0013(8) 0.0051(7) -0.0002(7)
O38 0.0228(10) 0.0224(10) 0.0311(11) -0.0006(8) 0.0118(8) 0.0028(8)
O39 0.0258(10) 0.0335(12) 0.0287(10) 0.0057(9) 0.0074(8) -0.0002(9)
O40 0.0235(10) 0.0296(11) 0.0358(11) -0.0020(9) 0.0115(9) 0.0132(9)
O41 0.0213(10) 0.0391(12) 0.0237(10) -0.0036(9) 0.0074(8) -0.0022(9)
O42 0.0337(12) 0.0314(12) 0.0432(13) -0.0093(10) -0.0011(10) 0.0006(11)
O43 0.0398(14) 0.0378(14) 0.094(2) -0.0030(11) 0.0194(14) 0.0242(14)
O44 0.0400(16) 0.0510(17) 0.0615(18) -0.0047(14) 0.0123(13) -0.0022(14)
O44' 0.0400(16) 0.0510(17) 0.0615(18) -0.0047(14) 0.0123(13) -0.0022(14)
O45 0.0278(12) 0.0282(16) 0.0290(16) -0.0001(11) 0.0088(12) 0.0024(12)
O45' 0.0278(12) 0.0282(16) 0.0290(16) -0.0001(11) 0.0088(12) 0.0024(12)
O46 0.0424(15) 0.046(2) 0.055(2) -0.0070(15) 0.0087(14) 0.0050(17)
O46' 0.0424(15) 0.046(2) 0.055(2) -0.0070(15) 0.0087(14) 0.0050(17)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C2 . 1.429(3) ?
O1 H1A . 0.8400 ?
O2 C3 . 1.428(3) ?
O2 H2A . 0.8400 ?
O3 C37 . 1.411(3) ?
O3 C4 . 1.436(3) ?
O4 C1 . 1.400(3) ?
O4 C5 . 1.441(3) ?
O5 C6 . 1.395(4) ?
O5 H5A . 0.8400 ?
C6 C5 . 1.507(4) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
O5' H5' . 0.8400 ?
O6 C8 . 1.433(3) ?
O6 H6C . 0.8400 ?
O7 C9 . 1.430(3) ?
O7 H7A . 0.8400 ?
O8 C1 . 1.406(3) ?
O8 C10 . 1.437(3) ?
O9 C7 . 1.403(3) ?
O9 C11 . 1.441(3) ?
O11 C14 . 1.424(3) ?
O11 H11A . 0.8400 ?
O12 C15 . 1.426(3) ?
O12 H12C . 0.8400 ?
O13 C7 . 1.417(3) ?
O13 C16 . 1.433(3) ?
O14 C13 . 1.410(3) ?
O14 C17 . 1.449(3) ?
O15 C18 . 1.437(3) ?
O15 H15A . 0.8400 ?
O16 C20 . 1.429(3) ?
O16 H16A . 0.8400 ?
O17 C21 . 1.421(3) ?
O17 H17A . 0.8400 ?
O18 C13 . 1.405(3) ?
O18 C22 . 1.432(3) ?
O19 C19 . 1.402(3) ?
O19 C23 . 1.441(3) ?
O20 C24 . 1.432(3) ?
O20 H20A . 0.8400 ?
O21 C26 . 1.422(3) ?
O21 H21A . 0.8400 ?
O22 C27 . 1.427(3) ?
O22 H22A . 0.8400 ?
O23 C19 . 1.415(3) ?
O23 C28 . 1.425(3) ?
O24 C25 . 1.408(3) ?
O24 C29 . 1.448(3) ?
O25 C30 . 1.415(3) ?
O25 H25A . 0.8400 ?
O26 C32 . 1.434(3) ?
O26 H26A . 0.8400 ?
O27 C33 . 1.424(3) ?
O27 H27A . 0.8400 ?
O28 C25 . 1.413(3) ?
O28 C34 . 1.435(3) ?
O29 C31 . 1.408(3) ?
O29 C35 . 1.444(3) ?
O30 C36 . 1.430(3) ?
O30 H30C . 0.8400 ?
O31 C38 . 1.422(3) ?
O31 H31A . 0.8400 ?
O32 C39 . 1.428(3) ?
O32 H32A . 0.8400 ?
O33 C31 . 1.412(3) ?
O33 C40 . 1.430(3) ?
O34 C37 . 1.411(3) ?
O34 C41 . 1.436(3) ?
O35 C42 . 1.432(3) ?
O35 H35A . 0.8400 ?
O36 C12 . 1.410(3) ?
O36 H36 . 0.8400 ?
C1 C2 . 1.532(3) ?
C1 H1 . 1.0000 ?
C2 C3 . 1.519(3) ?
C2 H2 . 1.0000 ?
C3 C4 . 1.515(3) ?
C3 H3 . 1.0000 ?
C4 C5 . 1.527(3) ?
C4 H4 . 1.0000 ?
C5 H5 . 1.0000 ?
C7 C8 . 1.539(3) ?
C7 H7 . 1.0000 ?
C8 C9 . 1.521(3) ?
C8 H8 . 1.0000 ?
C9 C10 . 1.527(3) ?
C9 H9 . 1.0000 ?
C10 C11 . 1.534(3) ?
C10 H10 . 1.0000 ?
C11 C12 . 1.509(3) ?
C11 H11 . 1.0000 ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 C14 . 1.526(3) ?
C13 H13 . 1.0000 ?
C14 C15 . 1.519(3) ?
C14 H14 . 1.0000 ?
C15 C16 . 1.517(3) ?
C15 H15 . 1.0000 ?
C16 C17 . 1.529(3) ?
C16 H16 . 1.0000 ?
C17 C18 . 1.506(3) ?
C17 H17 . 1.0000 ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C19 C20 . 1.536(3) ?
C19 H19 . 1.0000 ?
C20 C21 . 1.505(3) ?
C20 H20 . 1.0000 ?
C21 C22 . 1.525(3) ?
C21 H21 . 1.0000 ?
C22 C23 . 1.520(3) ?
C22 H22 . 1.0000 ?
C23 C24 . 1.510(3) ?
C23 H23 . 1.0000 ?
C24 H24A . 0.9900 ?
C24 H24B . 0.9900 ?
C25 C26 . 1.523(3) ?
C25 H25 . 1.0000 ?
C26 C27 . 1.522(3) ?
C26 H26 . 1.0000 ?
C27 C28 . 1.517(3) ?
C27 H27 . 1.0000 ?
C28 C29 . 1.518(3) ?
C28 H28 . 1.0000 ?
C29 C30 . 1.515(3) ?
C29 H29 . 1.0000 ?
C30 H30A . 0.9900 ?
C30 H30B . 0.9900 ?
C31 C32 . 1.524(4) ?
C31 H31 . 1.0000 ?
C32 C33 . 1.519(3) ?
C32 H32 . 1.0000 ?
C33 C34 . 1.522(3) ?
C33 H33 . 1.0000 ?
C34 C35 . 1.526(3) ?
C34 H34 . 1.0000 ?
C35 C36 . 1.508(3) ?
C35 H35 . 1.0000 ?
C36 H36A . 0.9900 ?
C36 H36B . 0.9900 ?
C37 C38 . 1.524(3) ?
C37 H37 . 1.0000 ?
C38 C39 . 1.510(3) ?
C38 H38 . 1.0000 ?
C39 C40 . 1.516(3) ?
C39 H39 . 1.0000 ?
C40 C41 . 1.523(3) ?
C40 H40 . 1.0000 ?
C41 C42 . 1.510(3) ?
C41 H41 . 1.0000 ?
C42 H42A . 0.9900 ?
C42 H42B . 0.9900 ?
O37 H37A . 0.824(17) ?
O37 H37B . 0.849(17) ?
O38 H38A . 0.828(17) ?
O38 H38B . 0.817(17) ?
O39 H39A . 0.856(18) ?
O39 H39B . 0.861(18) ?
O40 H40A . 0.879(18) ?
O40 H40B . 0.869(18) ?
O41 H41A . 0.844(17) ?
O41 H41B . 0.840(18) ?
O42 H42C . 0.852(18) ?
O42 H42D . 0.805(18) ?
O44 O44' . 1.07(3) ?
O44 O49 . 1.73(3) ?
O45 O45' . 0.774(13) ?
O46 O46' . 0.84(4) ?
O48 O50 . 1.46(4) ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 O1 H1A . . 109.5 ?
C3 O2 H2A . . 109.5 ?
C37 O3 C4 . . 117.01(18) ?
C1 O4 C5 . . 113.34(18) ?
C6 O5 H5A . . 109.5 ?
O5 C6 C5 . . 112.7(2) ?
O5 C6 H6A . . 109.1 ?
C5 C6 H6A . . 109.1 ?
O5 C6 H6B . . 109.1 ?
C5 C6 H6B . . 109.1 ?
H6A C6 H6B . . 107.8 ?
C8 O6 H6C . . 109.5 ?
C9 O7 H7A . . 109.5 ?
C1 O8 C10 . . 117.08(18) ?
C7 O9 C11 . . 112.94(18) ?
C14 O11 H11A . . 109.5 ?
C15 O12 H12C . . 109.5 ?
C7 O13 C16 . . 118.09(17) ?
C13 O14 C17 . . 113.50(17) ?
C18 O15 H15A . . 109.5 ?
C20 O16 H16A . . 109.5 ?
C21 O17 H17A . . 109.5 ?
C13 O18 C22 . . 118.62(16) ?
C19 O19 C23 . . 113.68(17) ?
C24 O20 H20A . . 109.5 ?
C26 O21 H21A . . 109.5 ?
C27 O22 H22A . . 109.5 ?
C19 O23 C28 . . 118.45(17) ?
C25 O24 C29 . . 113.37(17) ?
C30 O25 H25A . . 109.5 ?
C32 O26 H26A . . 109.5 ?
C33 O27 H27A . . 109.5 ?
C25 O28 C34 . . 117.86(17) ?
C31 O29 C35 . . 113.41(17) ?
C36 O30 H30C . . 109.5 ?
C38 O31 H31A . . 109.5 ?
C39 O32 H32A . . 109.5 ?
C31 O33 C40 . . 118.99(16) ?
C37 O34 C41 . . 115.44(17) ?
C42 O35 H35A . . 109.5 ?
C12 O36 H36 . . 109.5 ?
O4 C1 O8 . . 111.42(19) ?
O4 C1 C2 . . 110.68(18) ?
O8 C1 C2 . . 107.42(19) ?
O4 C1 H1 . . 109.1 ?
O8 C1 H1 . . 109.1 ?
C2 C1 H1 . . 109.1 ?
O1 C2 C3 . . 112.3(2) ?
O1 C2 C1 . . 110.80(18) ?
C3 C2 C1 . . 110.34(19) ?
O1 C2 H2 . . 107.7 ?
C3 C2 H2 . . 107.7 ?
C1 C2 H2 . . 107.7 ?
O2 C3 C4 . . 106.73(18) ?
O2 C3 C2 . . 112.39(19) ?
C4 C3 C2 . . 110.6(2) ?
O2 C3 H3 . . 109.0 ?
C4 C3 H3 . . 109.0 ?
C2 C3 H3 . . 109.0 ?
O3 C4 C3 . . 107.56(19) ?
O3 C4 C5 . . 109.00(19) ?
C3 C4 C5 . . 110.25(18) ?
O3 C4 H4 . . 110.0 ?
C3 C4 H4 . . 110.0 ?
C5 C4 H4 . . 110.0 ?
O4 C5 C6 . . 106.7(2) ?
O4 C5 C4 . . 108.40(19) ?
C6 C5 C4 . . 114.3(2) ?
O4 C5 H5 . . 109.1 ?
C6 C5 H5 . . 109.1 ?
C4 C5 H5 . . 109.1 ?
O9 C7 O13 . . 110.19(18) ?
O9 C7 C8 . . 111.52(19) ?
O13 C7 C8 . . 107.64(19) ?
O9 C7 H7 . . 109.2 ?
O13 C7 H7 . . 109.2 ?
C8 C7 H7 . . 109.2 ?
O6 C8 C9 . . 112.0(2) ?
O6 C8 C7 . . 109.72(19) ?
C9 C8 C7 . . 110.97(18) ?
O6 C8 H8 . . 108.0 ?
C9 C8 H8 . . 108.0 ?
C7 C8 H8 . . 108.0 ?
O7 C9 C8 . . 113.35(18) ?
O7 C9 C10 . . 110.8(2) ?
C8 C9 C10 . . 109.68(19) ?
O7 C9 H9 . . 107.6 ?
C8 C9 H9 . . 107.6 ?
C10 C9 H9 . . 107.6 ?
O8 C10 C9 . . 105.82(18) ?
O8 C10 C11 . . 111.88(18) ?
C9 C10 C11 . . 107.94(19) ?
O8 C10 H10 . . 110.4 ?
C9 C10 H10 . . 110.4 ?
C11 C10 H10 . . 110.4 ?
O9 C11 C12 . . 107.95(19) ?
O9 C11 C10 . . 106.86(18) ?
C12 C11 C10 . . 116.8(2) ?
O9 C11 H11 . . 108.3 ?
C12 C11 H11 . . 108.3 ?
C10 C11 H11 . . 108.3 ?
O36 C12 C11 . . 115.1(2) ?
O36 C12 H12A . . 108.5 ?
C11 C12 H12A . . 108.5 ?
O36 C12 H12B . . 108.5 ?
C11 C12 H12B . . 108.5 ?
H12A C12 H12B . . 107.5 ?
O18 C13 O14 . . 111.31(19) ?
O18 C13 C14 . . 107.20(18) ?
O14 C13 C14 . . 111.02(19) ?
O18 C13 H13 . . 109.1 ?
O14 C13 H13 . . 109.1 ?
C14 C13 H13 . . 109.1 ?
O11 C14 C15 . . 110.39(19) ?
O11 C14 C13 . . 109.65(19) ?
C15 C14 C13 . . 109.79(19) ?
O11 C14 H14 . . 109.0 ?
C15 C14 H14 . . 109.0 ?
C13 C14 H14 . . 109.0 ?
O12 C15 C16 . . 107.38(18) ?
O12 C15 C14 . . 110.84(18) ?
C16 C15 C14 . . 110.75(18) ?
O12 C15 H15 . . 109.3 ?
C16 C15 H15 . . 109.3 ?
C14 C15 H15 . . 109.3 ?
O13 C16 C15 . . 105.71(17) ?
O13 C16 C17 . . 110.33(18) ?
C15 C16 C17 . . 112.08(19) ?
O13 C16 H16 . . 109.5 ?
C15 C16 H16 . . 109.5 ?
C17 C16 H16 . . 109.5 ?
O14 C17 C18 . . 105.75(18) ?
O14 C17 C16 . . 109.75(18) ?
C18 C17 C16 . . 113.1(2) ?
O14 C17 H17 . . 109.4 ?
C18 C17 H17 . . 109.4 ?
C16 C17 H17 . . 109.4 ?
O15 C18 C17 . . 107.79(19) ?
O15 C18 H18A . . 110.1 ?
C17 C18 H18A . . 110.1 ?
O15 C18 H18B . . 110.1 ?
C17 C18 H18B . . 110.1 ?
H18A C18 H18B . . 108.5 ?
O19 C19 O23 . . 110.45(19) ?
O19 C19 C20 . . 110.13(18) ?
O23 C19 C20 . . 108.29(18) ?
O19 C19 H19 . . 109.3 ?
O23 C19 H19 . . 109.3 ?
C20 C19 H19 . . 109.3 ?
O16 C20 C21 . . 108.93(18) ?
O16 C20 C19 . . 109.99(18) ?
C21 C20 C19 . . 109.15(19) ?
O16 C20 H20 . . 109.6 ?
C21 C20 H20 . . 109.6 ?
C19 C20 H20 . . 109.6 ?
O17 C21 C20 . . 109.46(19) ?
O17 C21 C22 . . 110.80(18) ?
C20 C21 C22 . . 110.51(18) ?
O17 C21 H21 . . 108.7 ?
C20 C21 H21 . . 108.7 ?
C22 C21 H21 . . 108.7 ?
O18 C22 C23 . . 107.67(18) ?
O18 C22 C21 . . 106.81(17) ?
C23 C22 C21 . . 112.33(18) ?
O18 C22 H22 . . 110.0 ?
C23 C22 H22 . . 110.0 ?
C21 C22 H22 . . 110.0 ?
O19 C23 C24 . . 105.91(18) ?
O19 C23 C22 . . 110.36(19) ?
C24 C23 C22 . . 112.89(19) ?
O19 C23 H23 . . 109.2 ?
C24 C23 H23 . . 109.2 ?
C22 C23 H23 . . 109.2 ?
O20 C24 C23 . . 111.1(2) ?
O20 C24 H24A . . 109.4 ?
C23 C24 H24A . . 109.4 ?
O20 C24 H24B . . 109.4 ?
C23 C24 H24B . . 109.4 ?
H24A C24 H24B . . 108.0 ?
O24 C25 O28 . . 110.90(19) ?
O24 C25 C26 . . 111.10(18) ?
O28 C25 C26 . . 108.21(18) ?
O24 C25 H25 . . 108.9 ?
O28 C25 H25 . . 108.9 ?
C26 C25 H25 . . 108.9 ?
O21 C26 C27 . . 112.28(19) ?
O21 C26 C25 . . 111.14(18) ?
C27 C26 C25 . . 110.38(19) ?
O21 C26 H26 . . 107.6 ?
C27 C26 H26 . . 107.6 ?
C25 C26 H26 . . 107.6 ?
O22 C27 C28 . . 111.73(19) ?
O22 C27 C26 . . 108.29(19) ?
C28 C27 C26 . . 108.59(19) ?
O22 C27 H27 . . 109.4 ?
C28 C27 H27 . . 109.4 ?
C26 C27 H27 . . 109.4 ?
O23 C28 C27 . . 107.03(18) ?
O23 C28 C29 . . 111.26(19) ?
C27 C28 C29 . . 109.50(19) ?
O23 C28 H28 . . 109.7 ?
C27 C28 H28 . . 109.7 ?
C29 C28 H28 . . 109.7 ?
O24 C29 C30 . . 106.93(19) ?
O24 C29 C28 . . 108.22(19) ?
C30 C29 C28 . . 113.7(2) ?
O24 C29 H29 . . 109.3 ?
C30 C29 H29 . . 109.3 ?
C28 C29 H29 . . 109.3 ?
O25 C30 C29 . . 113.3(2) ?
O25 C30 H30A . . 108.9 ?
C29 C30 H30A . . 108.9 ?
O25 C30 H30B . . 108.9 ?
C29 C30 H30B . . 108.9 ?
H30A C30 H30B . . 107.7 ?
O29 C31 O33 . . 111.25(18) ?
O29 C31 C32 . . 110.58(19) ?
O33 C31 C32 . . 106.41(19) ?
O29 C31 H31 . . 109.5 ?
O33 C31 H31 . . 109.5 ?
C32 C31 H31 . . 109.5 ?
O26 C32 C33 . . 111.62(19) ?
O26 C32 C31 . . 108.11(19) ?
C33 C32 C31 . . 109.44(19) ?
O26 C32 H32 . . 109.2 ?
C33 C32 H32 . . 109.2 ?
C31 C32 H32 . . 109.2 ?
O27 C33 C32 . . 110.6(2) ?
O27 C33 C34 . . 110.42(19) ?
C32 C33 C34 . . 108.28(19) ?
O27 C33 H33 . . 109.2 ?
C32 C33 H33 . . 109.2 ?
C34 C33 H33 . . 109.2 ?
O28 C34 C33 . . 107.25(18) ?
O28 C34 C35 . . 110.28(19) ?
C33 C34 C35 . . 109.39(19) ?
O28 C34 H34 . . 110.0 ?
C33 C34 H34 . . 110.0 ?
C35 C34 H34 . . 110.0 ?
O29 C35 C36 . . 107.00(18) ?
O29 C35 C34 . . 108.20(19) ?
C36 C35 C34 . . 115.1(2) ?
O29 C35 H35 . . 108.8 ?
C36 C35 H35 . . 108.8 ?
C34 C35 H35 . . 108.8 ?
O30 C36 C35 . . 112.6(2) ?
O30 C36 H36A . . 109.1 ?
C35 C36 H36A . . 109.1 ?
O30 C36 H36B . . 109.1 ?
C35 C36 H36B . . 109.1 ?
H36A C36 H36B . . 107.8 ?
O3 C37 O34 . . 111.60(18) ?
O3 C37 C38 . . 106.94(18) ?
O34 C37 C38 . . 110.84(18) ?
O3 C37 H37 . . 109.1 ?
O34 C37 H37 . . 109.1 ?
C38 C37 H37 . . 109.1 ?
O31 C38 C39 . . 111.40(19) ?
O31 C38 C37 . . 111.44(18) ?
C39 C38 C37 . . 109.72(18) ?
O31 C38 H38 . . 108.0 ?
C39 C38 H38 . . 108.0 ?
C37 C38 H38 . . 108.0 ?
O32 C39 C38 . . 110.27(18) ?
O32 C39 C40 . . 109.19(18) ?
C38 C39 C40 . . 109.88(19) ?
O32 C39 H39 . . 109.2 ?
C38 C39 H39 . . 109.2 ?
C40 C39 H39 . . 109.2 ?
O33 C40 C39 . . 105.44(17) ?
O33 C40 C41 . . 108.61(17) ?
C39 C40 C41 . . 112.83(18) ?
O33 C40 H40 . . 110.0 ?
C39 C40 H40 . . 110.0 ?
C41 C40 H40 . . 110.0 ?
O34 C41 C42 . . 105.01(18) ?
O34 C41 C40 . . 111.49(18) ?
C42 C41 C40 . . 111.44(19) ?
O34 C41 H41 . . 109.6 ?
C42 C41 H41 . . 109.6 ?
C40 C41 H41 . . 109.6 ?
O35 C42 C41 . . 111.42(18) ?
O35 C42 H42A . . 109.3 ?
C41 C42 H42A . . 109.3 ?
O35 C42 H42B . . 109.3 ?
C41 C42 H42B . . 109.3 ?
H42A C42 H42B . . 108.0 ?
H37A O37 H37B . . 105(2) ?
H38A O38 H38B . . 113(3) ?
H39A O39 H39B . . 103(3) ?
H40A O40 H40B . . 95(2) ?
H41A O41 H41B . . 109(3) ?
H42C O42 H42D . . 111(3) ?
O44' O44 O49 . . 139.5(19) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1A O7 . 0.84 2.36 3.065(3) 142
O2 H2A O45 2_655 0.84 2.00 2.809(3) 161
O2 H2A O45' 2_655 0.84 1.95 2.633(11) 138
O5 H5A O47 . 0.84 1.76 2.578(15) 163
O5 H5A O45 1_565 0.84 2.46 3.024(4) 125
O5' H5' O45 1_565 0.84 1.66 2.47(3) 163
O5' H5' O45' 1_565 0.84 2.40 3.20(3) 159
O6 H6C O12 . 0.84 2.04 2.845(2) 161
O6 H6C O13 . 0.84 2.31 2.742(2) 112
O7 H7A O26 2_655 0.84 2.14 2.956(3) 165
O11 H11A O40 . 0.84 1.78 2.595(2) 163
O12 H12C O31 2_645 0.84 1.85 2.676(2) 167
O15 H15A O41 2_756 0.84 2.04 2.870(3) 172
O16 H16A O38 1_545 0.84 1.90 2.733(3) 174
O17 H17A O11 . 0.84 2.06 2.889(2) 171
O20 H20A O43 . 0.84 1.93 2.725(3) 157
O20 H20A O50 . 0.84 2.12 2.80(3) 138
O21 H21A O27 . 0.84 1.99 2.810(2) 167
O21 H21A O28 . 0.84 2.36 2.794(2) 112
O22 H22A O16 . 0.84 1.97 2.776(2) 160
O22 H22A O23 . 0.84 2.41 2.821(2) 111
O25 H25A O39 2_745 0.84 1.90 2.743(3) 178
O26 H26A O37 2_645 0.84 1.83 2.668(3) 176
O27 H27A O5 1_545 0.84 2.09 2.821(3) 145
O30 H30C O15 1_554 0.84 2.06 2.858(3) 158
O30 H30C O14 1_554 0.84 2.37 2.945(2) 126
O31 H31A O2 . 0.84 2.01 2.844(2) 172
O32 H32A O26 . 0.84 2.04 2.871(2) 170
O35 H35A O37 2_655 0.84 2.08 2.890(2) 161
O36 H36 O11 1_565 0.84 2.02 2.854(2) 173
O37 H37A O6 . 0.824(17) 2.05(2) 2.837(2) 160(3)
O37 H37B O32 1_556 0.849(17) 1.910(18) 2.753(2) 171(3)
O38 H38A O20 . 0.828(17) 2.11(2) 2.865(3) 152(3)
O38 H38B O30 2_755 0.817(17) 1.857(18) 2.672(3) 176(3)
O39 H39A O22 1_565 0.856(18) 1.898(18) 2.749(3) 173(3)
O39 H39B O38 . 0.861(18) 2.18(2) 2.959(3) 151(3)
O40 H40A O41 2_746 0.879(18) 2.21(3) 2.787(3) 123(3)
O40 H40B O35 1_546 0.869(18) 1.91(2) 2.770(3) 168(3)
O41 H41A O20 . 0.844(17) 2.134(18) 2.976(3) 175(3)
O41 H41A O19 . 0.844(17) 2.63(3) 3.048(2) 112(3)
O41 H41B O25 . 0.840(18) 1.95(2) 2.769(3) 166(3)
O42 H42C O21 1_565 0.852(18) 2.09(2) 2.932(3) 173(3)
O42 H42D O48 . 0.805(18) 1.90(4) 2.53(3) 135(3)
O42 H42D O39 . 0.805(18) 2.34(3) 3.038(3) 146(3)