#------------------------------------------------------------------------------
#$Date: 2019-11-22 18:03:31 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231212 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/29/1552962.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_1552962
loop_
_publ_author_name
'Suzuki, Nozomu'
'Kinoshita, Mariko'
'Miyabe, Kanji'
_publ_section_title
;
 Kinetic Study of Chiral Intermolecular Interactions by Moment Analysis
 Based on Affinity Capillary Electrophoresis.
;
_journal_issue                   18
_journal_name_full               'Analytical chemistry'
_journal_page_first              11048
_journal_page_last               11053
_journal_paper_doi               10.1021/acs.analchem.8b02823
_journal_volume                  90
_journal_year                    2018
_chemical_formula_sum            'C51 H80 O38'
_chemical_formula_weight         1301.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 110.6520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6610(5)
_cell_length_b                   24.3629(7)
_cell_length_c                   15.4291(4)
_cell_measurement_reflns_used    262
_cell_measurement_temperature    93.(2)
_cell_measurement_theta_max      35.6266
_cell_measurement_theta_min      3.1018
_cell_volume                     6563.9(3)
_computing_cell_refinement       'APEX3 v2015.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.35A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26127
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.497
_refine_diff_density_min         -0.528
_refine_ls_abs_structure_details
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         10753
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1118P)²+15.3453P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1728
_reflns_number_gt                10690
_reflns_number_total             10753
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ac8b02823_si_001.cif
_cod_data_source_block           RSPPA_bCD
_cod_database_code               1552962
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C54A 0.0337(12) 0.7488(14) 0.2720(15) 0.080(7) Uani d . P D 0.510(8) A 1
H H54A 0.0384 0.786 0.2473 0.096 Uiso calc U P R 0.510(8) A 1
C C56A 0.0684(9) 0.7087(7) 0.1427(9) 0.085(4) Uani d . P DG 0.510(8) A 1
C C57A 0.0441(8) 0.6707(6) 0.0711(10) 0.082(4) Uani d . P G 0.510(8) A 1
H H57A 0.0062 0.6443 0.0696 0.098 Uiso calc U P R 0.510(8) A 1
C C58A 0.0755(8) 0.6712(6) 0.0016(9) 0.084(4) Uani d . P G 0.510(8) A 1
H H58A 0.0589 0.6452 -0.0474 0.101 Uiso calc U P R 0.510(8) A 1
C C59A 0.1310(8) 0.7097(7) 0.0038(10) 0.083(4) Uani d . P G 0.510(8) A 1
H H59A 0.1524 0.71 -0.0437 0.1 Uiso calc U P R 0.510(8) A 1
C C60A 0.1552(9) 0.7477(6) 0.0754(12) 0.096(4) Uani d . P G 0.510(8) A 1
H H60A 0.1932 0.7741 0.0769 0.115 Uiso calc U P R 0.510(8) A 1
C C61A 0.1239(10) 0.7472(6) 0.1449(11) 0.082(4) Uani d . P G 0.510(8) A 1
H H61A 0.1405 0.7732 0.1938 0.099 Uiso calc U P R 0.510(8) A 1
O O44A 0.0292(9) 0.7079(7) 0.2040(10) 0.088(3) Uani d . P D 0.510(8) A 1
C C54B 0.0321(13) 0.7318(13) 0.2743(16) 0.080(7) Uani d . P D 0.490(8) A 2
H H54B 0.0305 0.6962 0.2416 0.096 Uiso calc U P R 0.490(8) A 2
C C56B 0.0571(9) 0.7763(7) 0.1570(9) 0.085(4) Uani d . P DG 0.490(8) A 2
C C57B 0.0268(8) 0.8135(7) 0.0849(10) 0.082(4) Uani d . P G 0.490(8) A 2
H H57B -0.0154 0.8359 0.0828 0.098 Uiso calc U P R 0.490(8) A 2
C C58B 0.0585(9) 0.8179(7) 0.0160(9) 0.084(4) Uani d . P G 0.490(8) A 2
H H58B 0.0378 0.8434 -0.0332 0.101 Uiso calc U P R 0.490(8) A 2
C C59B 0.1203(9) 0.7852(7) 0.0192(10) 0.083(4) Uani d . P G 0.490(8) A 2
H H59B 0.1419 0.7882 -0.0279 0.1 Uiso calc U P R 0.490(8) A 2
C C60B 0.1506(9) 0.7480(7) 0.0912(12) 0.096(4) Uani d . P G 0.490(8) A 2
H H60B 0.1928 0.7256 0.0934 0.115 Uiso calc U P R 0.490(8) A 2
C C61B 0.1189(10) 0.7436(7) 0.1601(10) 0.082(4) Uani d . P G 0.490(8) A 2
H H61B 0.1396 0.7182 0.2093 0.099 Uiso calc U P R 0.490(8) A 2
O O44B 0.0229(10) 0.7788(8) 0.2200(11) 0.088(3) Uani d . P D 0.490(8) A 2
C C1 0.2095(3) 0.9072(3) 0.4593(4) 0.0366(13) Uani d . . . 1.0 . .
H H1A 0.1763 0.903 0.4967 0.044 Uiso calc U . R 1.0 . .
H H1B 0.2407 0.8736 0.4664 0.044 Uiso calc U . R 1.0 . .
C C2 0.1614(3) 0.9153(2) 0.3600(3) 0.0261(10) Uani d . . . 1.0 . .
H H2 0.1266 0.883 0.3389 0.031 Uiso calc U . R 1.0 . .
C C3 0.2070(3) 0.9220(2) 0.2945(3) 0.0202(9) Uani d . . . 1.0 . .
H H3 0.2421 0.9543 0.3138 0.024 Uiso calc U . R 1.0 . .
C C4 0.1502(3) 0.9306(2) 0.1969(3) 0.0238(10) Uani d . . . 1.0 . .
H H4 0.1151 0.8982 0.1781 0.029 Uiso calc U . R 1.0 . .
C C5 0.1038(3) 0.9819(2) 0.1962(3) 0.0252(10) Uani d . . . 1.0 . .
H H5 0.1396 1.014 0.2141 0.03 Uiso calc U . R 1.0 . .
C C6 0.0631(3) 0.9768(2) 0.2663(3) 0.0231(10) Uani d . . . 1.0 . .
H H6 0.0375 1.0124 0.2696 0.028 Uiso calc U . R 1.0 . .
C C7 -0.0590(3) 0.9514(3) 0.3866(3) 0.0327(12) Uani d . . . 1.0 . .
H H7A -0.0797 0.9344 0.4311 0.039 Uiso calc U . R 1.0 . .
H H7B -0.0034 0.9435 0.4079 0.039 Uiso calc U . R 1.0 . .
C C8 -0.0977(3) 0.9261(2) 0.2921(3) 0.0240(10) Uani d . . . 1.0 . .
H H8 -0.0864 0.8858 0.2962 0.029 Uiso calc U . R 1.0 . .
C C9 -0.0709(2) 0.9511(2) 0.2177(3) 0.0203(9) Uani d . . . 1.0 . .
H H9 -0.0748 0.992 0.2185 0.024 Uiso calc U . R 1.0 . .
C C10 -0.1188(3) 0.9289(2) 0.1223(3) 0.0204(9) Uani d . . . 1.0 . .
H H10 -0.1104 0.8885 0.12 0.025 Uiso calc U . R 1.0 . .
C C11 -0.2020(3) 0.9400(2) 0.1069(3) 0.0210(9) Uani d . . . 1.0 . .
H H11 -0.2101 0.9805 0.1086 0.025 Uiso calc U . R 1.0 . .
C C12 -0.2232(3) 0.9128(2) 0.1833(3) 0.0201(9) Uani d . . . 1.0 . .
H H12 -0.2784 0.9201 0.1726 0.024 Uiso calc U . R 1.0 . .
C C13 -0.2365(6) 0.8143(3) 0.3487(4) 0.055(2) Uani d . . . 1.0 . .
H H13A -0.1971 0.843 0.3567 0.066 Uiso calc U . R 1.0 . .
H H13B -0.2851 0.8328 0.3436 0.066 Uiso calc U . R 1.0 . .
C C14 -0.2476(4) 0.7830(2) 0.2603(4) 0.0315(12) Uani d . . . 1.0 . .
H H14 -0.198 0.7652 0.2653 0.038 Uiso calc U . R 1.0 . .
C C15 -0.2737(3) 0.8193(2) 0.1744(3) 0.0235(10) Uani d . . . 1.0 . .
H H15 -0.3195 0.8412 0.1725 0.028 Uiso calc U . R 1.0 . .
C C16 -0.2917(3) 0.7858(2) 0.0858(3) 0.0227(10) Uani d . . . 1.0 . .
H H16 -0.2436 0.7687 0.0841 0.027 Uiso calc U . R 1.0 . .
C C17 -0.3486(3) 0.7410(2) 0.0844(4) 0.0262(10) Uani d . . . 1.0 . .
H H17 -0.3975 0.7585 0.0828 0.031 Uiso calc U . R 1.0 . .
C C18 -0.3161(3) 0.7073(2) 0.1739(4) 0.0259(10) Uani d . . . 1.0 . .
H H18 -0.3538 0.678 0.1735 0.031 Uiso calc U . R 1.0 . .
C C19 -0.2019(5) 0.6270(4) 0.3624(4) 0.065(3) Uani d . . . 1.0 . .
H H19A -0.2336 0.5973 0.374 0.078 Uiso calc U . R 1.0 . .
H H19B -0.2317 0.6616 0.3498 0.078 Uiso calc U . R 1.0 . .
C C20 -0.1754(3) 0.6124(2) 0.2827(3) 0.0286(11) Uani d . . . 1.0 . .
H H20 -0.1282 0.6336 0.2879 0.034 Uiso calc U . R 1.0 . .
C C21 -0.2390(3) 0.6240(2) 0.1888(3) 0.0233(10) Uani d . . . 1.0 . .
H H21 -0.2883 0.6072 0.1873 0.028 Uiso calc U . R 1.0 . .
C C22 -0.2163(3) 0.6010(2) 0.1109(3) 0.0211(9) Uani d . . . 1.0 . .
H H22 -0.1689 0.6198 0.1101 0.025 Uiso calc U . R 1.0 . .
C C23 -0.2009(3) 0.5400(2) 0.1271(4) 0.0252(10) Uani d . . . 1.0 . .
H H23 -0.2488 0.5222 0.1285 0.03 Uiso calc U . R 1.0 . .
C C24 -0.1385(3) 0.5311(2) 0.2208(3) 0.0217(9) Uani d . . . 1.0 . .
H H24 -0.1303 0.4908 0.2322 0.026 Uiso calc U . R 1.0 . .
C C25 0.0349(3) 0.5325(2) 0.4117(3) 0.0248(10) Uani d . . . 1.0 . .
H H25A 0.0793 0.5411 0.4682 0.03 Uiso calc U . R 1.0 . .
H H25B -0.007 0.5582 0.4088 0.03 Uiso calc U . R 1.0 . .
C C26 0.0571(2) 0.5406(2) 0.3277(3) 0.0190(9) Uani d . . . 1.0 . .
H H26 0.0676 0.5804 0.3213 0.023 Uiso calc U . R 1.0 . .
C C27 -0.0036(3) 0.5205(2) 0.2388(3) 0.0191(9) Uani d . . . 1.0 . .
H H27 -0.0176 0.4817 0.2468 0.023 Uiso calc U . R 1.0 . .
C C28 0.0257(3) 0.5239(2) 0.1585(3) 0.0245(10) Uani d . . . 1.0 . .
H H28 0.0354 0.5632 0.1476 0.029 Uiso calc U . R 1.0 . .
C C29 0.1000(3) 0.4919(2) 0.1825(3) 0.0189(9) Uani d . . . 1.0 . .
H H29 0.089 0.4525 0.1906 0.023 Uiso calc U . R 1.0 . .
C C30 0.1577(3) 0.5128(2) 0.2733(3) 0.0193(9) Uani d . . . 1.0 . .
H H30 0.205 0.4897 0.2903 0.023 Uiso calc U . R 1.0 . .
C C31 0.2780(3) 0.5873(2) 0.4567(3) 0.0294(11) Uani d . . . 1.0 . .
H H31A 0.2972 0.6117 0.5113 0.035 Uiso calc U . R 1.0 . .
H H31B 0.2243 0.5775 0.4475 0.035 Uiso calc U . R 1.0 . .
C C32 0.2812(3) 0.6168(2) 0.3719(3) 0.0222(10) Uani d . . . 1.0 . .
H H32 0.2483 0.6504 0.36 0.027 Uiso calc U . R 1.0 . .
C C33 0.2563(3) 0.5802(2) 0.2856(3) 0.0215(9) Uani d . . . 1.0 . .
H H33 0.2866 0.5453 0.2994 0.026 Uiso calc U . R 1.0 . .
C C34 0.2688(3) 0.6093(2) 0.2050(3) 0.0218(9) Uani d . . . 1.0 . .
H H34 0.2354 0.6426 0.1874 0.026 Uiso calc U . R 1.0 . .
C C35 0.3524(3) 0.6260(2) 0.2348(3) 0.0234(10) Uani d . . . 1.0 . .
H H35 0.3841 0.5918 0.2506 0.028 Uiso calc U . R 1.0 . .
C C36 0.3739(3) 0.6614(2) 0.3212(3) 0.0230(10) Uani d . . . 1.0 . .
H H36 0.4293 0.6716 0.3411 0.028 Uiso calc U . R 1.0 . .
C C37 0.3823(8) 0.7567(3) 0.4944(5) 0.080(4) Uani d . . . 1.0 . .
H H37A 0.376 0.7165 0.4862 0.096 Uiso calc U . R 1.0 . .
H H37B 0.4376 0.7652 0.5128 0.096 Uiso calc U . R 1.0 . .
C C38 0.3384(3) 0.7855(2) 0.4003(4) 0.0276(11) Uani d . . . 1.0 . .
H H38 0.2819 0.7809 0.384 0.033 Uiso calc U . R 1.0 . .
C C39 0.3633(3) 0.7619(2) 0.3240(3) 0.0216(9) Uani d . . . 1.0 . .
H H39 0.4202 0.7574 0.3482 0.026 Uiso calc U . R 1.0 . .
C C40 0.3401(3) 0.7972(2) 0.2375(3) 0.0220(10) Uani d . . . 1.0 . .
H H40 0.2832 0.7955 0.2068 0.026 Uiso calc U . R 1.0 . .
C C41 0.3633(3) 0.8565(2) 0.2623(3) 0.0220(9) Uani d . . . 1.0 . .
H H41 0.4205 0.8583 0.29 0.026 Uiso calc U . R 1.0 . .
C C42 0.3305(3) 0.8758(2) 0.3346(3) 0.0231(10) Uani d . . . 1.0 . .
H H42 0.3465 0.9147 0.3517 0.028 Uiso calc U . R 1.0 . .
C C53 0.0982(6) 0.7393(5) 0.3625(7) 0.078(3) Uani d . . D 1.0 . .
C C55 -0.0398(8) 0.7457(15) 0.2976(16) 0.210(14) Uani d . . D 1.0 . .
H H55A -0.0546 0.7828 0.3092 0.314 Uiso calc U . R 1.0 A 1
H H55B -0.0296 0.7233 0.3534 0.314 Uiso calc U . R 1.0 A 1
H H55C -0.0815 0.7291 0.2462 0.314 Uiso calc U . R 1.0 A 1
O O1 0.2577(3) 0.9533(2) 0.4903(3) 0.0493(12) Uani d . . . 1.0 . .
H H1C 0.2994 0.9433 0.5302 0.074 Uiso calc U . R 1.0 . .
O O2 0.1911(2) 0.93657(18) 0.1347(2) 0.0299(8) Uani d . . . 1.0 . .
H H2A 0.2034 0.9055 0.121 0.045 Uiso calc U . R 1.0 . .
O O3 0.0489(2) 0.9918(2) 0.1065(2) 0.0368(9) Uani d . . . 1.0 . .
H H3A 0.0712 1.0032 0.0713 0.055 Uiso calc U . R 1.0 . .
O O4 0.11532(19) 0.96349(16) 0.3551(2) 0.0270(8) Uani d . . . 1.0 . .
O O5 0.00676(18) 0.93491(15) 0.2356(2) 0.0226(7) Uani d . . . 1.0 . .
O O6 -0.0700(2) 1.00949(19) 0.3863(3) 0.0361(9) Uani d . . . 1.0 . .
H H6A -0.1076 1.0165 0.4023 0.054 Uiso calc U . R 1.0 . .
O O7 -0.1000(2) 0.95531(19) 0.0516(2) 0.0325(9) Uani d . . . 1.0 . .
H H7 -0.0586 0.9426 0.0502 0.049 Uiso calc U . R 1.0 . .
O O8 -0.25066(18) 0.91893(15) 0.0186(2) 0.0225(7) Uani d . . . 1.0 . .
H H8A -0.2749 0.9449 -0.0146 0.034 Uiso calc U . R 1.0 . .
O O9 -0.17817(19) 0.93366(15) 0.2703(2) 0.0237(7) Uani d . . . 1.0 . .
O O10 -0.21207(19) 0.85519(14) 0.1780(2) 0.0225(7) Uani d . . . 1.0 . .
O O11 -0.2132(3) 0.7789(3) 0.4296(3) 0.0571(13) Uani d . . . 1.0 . .
H H11A -0.2513 0.7717 0.4446 0.086 Uiso calc U . R 1.0 . .
O O12 -0.3242(2) 0.82020(15) 0.0055(2) 0.0267(8) Uani d . . . 1.0 . .
H H12A -0.2992 0.8496 0.0129 0.04 Uiso calc U . R 1.0 . .
O O13 -0.3641(2) 0.70749(17) 0.0050(3) 0.0336(8) Uani d . . . 1.0 . .
H H13 -0.4039 0.689 -0.0028 0.05 Uiso calc U . R 1.0 . .
O O14 -0.3040(2) 0.74059(17) 0.2515(3) 0.0327(8) Uani d . . . 1.0 . .
O O15 -0.24805(18) 0.68226(14) 0.1745(2) 0.0204(7) Uani d . . . 1.0 . .
O O16 -0.1232(6) 0.6339(4) 0.4478(5) 0.112(3) Uani d . . . 1.0 . .
H H16A -0.0865 0.6246 0.4315 0.169 Uiso calc U . R 1.0 . .
O O17 -0.2767(2) 0.60938(17) 0.0245(3) 0.0355(9) Uani d . . . 1.0 . .
H H17A -0.2778 0.6426 0.0093 0.053 Uiso calc U . R 1.0 . .
O O18 -0.1815(2) 0.51506(16) 0.0552(3) 0.0308(8) Uani d . . . 1.0 . .
H H18A -0.1336 0.5137 0.0707 0.046 Uiso calc U . R 1.0 . .
O O19 -0.1588(2) 0.55429(16) 0.2921(2) 0.0275(8) Uani d . . . 1.0 . .
O O20 -0.07024(17) 0.55479(13) 0.2172(2) 0.0189(6) Uani d . . . 1.0 . .
O O21 0.0106(2) 0.47784(16) 0.4173(2) 0.0275(8) Uani d . . . 1.0 . .
H H21A 0.0365 0.4561 0.398 0.041 Uiso calc U . R 1.0 . .
O O22 -0.0305(2) 0.50186(19) 0.0763(2) 0.0336(9) Uani d . . . 1.0 . .
H H22A -0.036 0.4682 0.0836 0.05 Uiso calc U . R 1.0 . .
O O23 0.13137(19) 0.49547(15) 0.1111(2) 0.0226(7) Uani d . . . 1.0 . .
H H23A 0.1615 0.5223 0.1213 0.034 Uiso calc U . R 1.0 . .
O O24 0.12691(17) 0.50927(14) 0.3447(2) 0.0192(6) Uani d . . . 1.0 . .
O O25 0.17674(17) 0.56762(14) 0.2595(2) 0.0192(6) Uani d . . . 1.0 . .
O O26 0.3238(2) 0.53855(19) 0.4726(3) 0.0369(9) Uani d . . . 1.0 . .
H H26A 0.3562 0.5391 0.5267 0.055 Uiso calc U . R 1.0 . .
O O27 0.2502(2) 0.57251(15) 0.1286(2) 0.0274(7) Uani d . . . 1.0 . .
H H27A 0.259 0.5876 0.0845 0.041 Uiso calc U . R 1.0 . .
O O28 0.3696(2) 0.65366(16) 0.1631(3) 0.0312(8) Uani d . . . 1.0 . .
H H28A 0.3559 0.6866 0.1611 0.047 Uiso calc U . R 1.0 . .
O O29 0.36011(19) 0.63235(15) 0.3939(2) 0.0255(7) Uani d . . . 1.0 . .
O O30 0.32835(18) 0.70929(14) 0.2968(2) 0.0216(7) Uani d . . . 1.0 . .
O O31 0.3569(4) 0.7729(3) 0.5634(4) 0.0617(14) Uani d . . . 1.0 . .
H H31 0.3863 0.7604 0.6143 0.093 Uiso calc U . R 1.0 . .
O O32 0.3742(2) 0.77423(15) 0.1769(2) 0.0259(7) Uani d . . . 1.0 . .
H H32A 0.3484 0.7829 0.1221 0.039 Uiso calc U . R 1.0 . .
O O33 0.3384(2) 0.89131(15) 0.1834(3) 0.0269(7) Uani d . . . 1.0 . .
H H33A 0.356 0.8798 0.1436 0.04 Uiso calc U . R 1.0 . .
O O34 0.3587(2) 0.84272(15) 0.4144(2) 0.0257(7) Uani d . . . 1.0 . .
O O35 0.25001(19) 0.87352(15) 0.2951(2) 0.0255(7) Uani d . . . 1.0 . .
O O42 0.1328(8) 0.6979(5) 0.3950(8) 0.145(5) Uani d . . . 1.0 . .
O O43 0.1077(5) 0.7859(3) 0.4080(5) 0.096(2) Uani d . . . 1.0 . .
H H43 0.1397 0.7816 0.4617 0.145 Uiso calc U . R 1.0 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O44A C54A C53 . . 113.3(19)
O44A C54A C55 . . 109.(2)
C53 C54A C55 . . 104.2(17)
O44A C54A H54A . . 110.1
C53 C54A H54A . . 110.1
C55 C54A H54A . . 110.1
O44A C56A C57A . . 115.6(12)
O44A C56A C61A . . 124.2(12)
C57A C56A C61A . . 120.0
C56A C57A C58A . . 120.0
C56A C57A H57A . . 120.0
C58A C57A H57A . . 120.0
C57A C58A C59A . . 120.0
C57A C58A H58A . . 120.0
C59A C58A H58A . . 120.0
C60A C59A C58A . . 120.0
C60A C59A H59A . . 120.0
C58A C59A H59A . . 120.0
C59A C60A C61A . . 120.0
C59A C60A H60A . . 120.0
C61A C60A H60A . . 120.0
C60A C61A C56A . . 120.0
C60A C61A H61A . . 120.0
C56A C61A H61A . . 120.0
C56A O44A C54A . . 125.7(17)
O44B C54B C53 . . 110.(2)
O44B C54B C55 . . 92.(2)
C53 C54B C55 . . 105.5(17)
O44B C54B H54B . . 115.8
C53 C54B H54B . . 115.8
C55 C54B H54B . . 115.8
O44B C56B C57B . . 112.8(13)
O44B C56B C61B . . 127.1(13)
C57B C56B C61B . . 120.0
C58B C57B C56B . . 120.0
C58B C57B C58B . 2 79.5(14)
C56B C57B C58B . 2 136.0(7)
C58B C57B H57B . . 120.0
C56B C57B H57B . . 120.0
C58B C57B H57B 2 . 57.6
C57B C58B C59B . . 120.0
C57B C58B C57B . 2 100.0(15)
C59B C58B C57B . 2 117.8(11)
C57B C58B H58B . . 120.0
C59B C58B H58B . . 120.0
C57B C58B H58B 2 . 50.2
C60B C59B C58B . . 120.0
C60B C59B H59B . . 120.0
C58B C59B H59B . . 120.0
C61B C60B C59B . . 120.0
C61B C60B H60B . . 120.0
C59B C60B H60B . . 120.0
C60B C61B C56B . . 120.0
C60B C61B H61B . . 120.0
C56B C61B H61B . . 120.0
C56B O44B C54B . . 114.2(18)
O1 C1 C2 . . 108.9(5)
O1 C1 H1A . . 109.9
C2 C1 H1A . . 109.9
O1 C1 H1B . . 109.9
C2 C1 H1B . . 109.9
H1A C1 H1B . . 108.3
O4 C2 C1 . . 107.0(4)
O4 C2 C3 . . 109.7(4)
C1 C2 C3 . . 114.7(4)
O4 C2 H2 . . 108.4
C1 C2 H2 . . 108.4
C3 C2 H2 . . 108.4
O35 C3 C4 . . 108.3(4)
O35 C3 C2 . . 110.3(4)
C4 C3 C2 . . 108.1(4)
O35 C3 H3 . . 110.0
C4 C3 H3 . . 110.0
C2 C3 H3 . . 110.0
O2 C4 C3 . . 109.1(4)
O2 C4 C5 . . 110.4(4)
C3 C4 C5 . . 108.4(4)
O2 C4 H4 . . 109.6
C3 C4 H4 . . 109.6
C5 C4 H4 . . 109.6
O3 C5 C4 . . 111.0(4)
O3 C5 C6 . . 109.6(4)
C4 C5 C6 . . 110.5(4)
O3 C5 H5 . . 108.6
C4 C5 H5 . . 108.6
C6 C5 H5 . . 108.6
O4 C6 O5 . . 109.6(4)
O4 C6 C5 . . 111.1(4)
O5 C6 C5 . . 108.4(4)
O4 C6 H6 . . 109.2
O5 C6 H6 . . 109.2
C5 C6 H6 . . 109.2
O6 C7 C8 . . 112.5(4)
O6 C7 H7A . . 109.1
C8 C7 H7A . . 109.1
O6 C7 H7B . . 109.1
C8 C7 H7B . . 109.1
H7A C7 H7B . . 107.8
O9 C8 C7 . . 106.1(4)
O9 C8 C9 . . 111.4(4)
C7 C8 C9 . . 113.0(4)
O9 C8 H8 . . 108.7
C7 C8 H8 . . 108.7
C9 C8 H8 . . 108.7
O5 C9 C10 . . 107.3(4)
O5 C9 C8 . . 108.8(4)
C10 C9 C8 . . 110.4(4)
O5 C9 H9 . . 110.1
C10 C9 H9 . . 110.1
C8 C9 H9 . . 110.1
O7 C10 C11 . . 108.6(4)
O7 C10 C9 . . 111.3(4)
C11 C10 C9 . . 108.0(4)
O7 C10 H10 . . 109.6
C11 C10 H10 . . 109.6
C9 C10 H10 . . 109.6
O8 C11 C10 . . 110.9(4)
O8 C11 C12 . . 109.2(4)
C10 C11 C12 . . 109.5(4)
O8 C11 H11 . . 109.1
C10 C11 H11 . . 109.1
C12 C11 H11 . . 109.1
O9 C12 O10 . . 111.2(4)
O9 C12 C11 . . 110.6(4)
O10 C12 C11 . . 107.4(4)
O9 C12 H12 . . 109.2
O10 C12 H12 . . 109.2
C11 C12 H12 . . 109.2
O11 C13 C14 . . 112.3(6)
O11 C13 H13A . . 109.1
C14 C13 H13A . . 109.1
O11 C13 H13B . . 109.1
C14 C13 H13B . . 109.1
H13A C13 H13B . . 107.9
O14 C14 C13 . . 108.0(5)
O14 C14 C15 . . 109.5(5)
C13 C14 C15 . . 113.1(5)
O14 C14 H14 . . 108.7
C13 C14 H14 . . 108.7
C15 C14 H14 . . 108.7
O10 C15 C14 . . 108.4(4)
O10 C15 C16 . . 106.4(4)
C14 C15 C16 . . 111.8(4)
O10 C15 H15 . . 110.0
C14 C15 H15 . . 110.0
C16 C15 H15 . . 110.0
O12 C16 C17 . . 109.1(4)
O12 C16 C15 . . 110.7(4)
C17 C16 C15 . . 109.3(4)
O12 C16 H16 . . 109.3
C17 C16 H16 . . 109.3
C15 C16 H16 . . 109.3
O13 C17 C16 . . 110.8(4)
O13 C17 C18 . . 111.5(4)
C16 C17 C18 . . 108.6(4)
O13 C17 H17 . . 108.6
C16 C17 H17 . . 108.6
C18 C17 H17 . . 108.6
O14 C18 O15 . . 111.9(4)
O14 C18 C17 . . 110.7(4)
O15 C18 C17 . . 107.9(4)
O14 C18 H18 . . 108.8
O15 C18 H18 . . 108.8
C17 C18 H18 . . 108.8
C20 C19 O16 . . 103.0(6)
C20 C19 H19A . . 111.2
O16 C19 H19A . . 111.2
C20 C19 H19B . . 111.2
O16 C19 H19B . . 111.2
H19A C19 H19B . . 109.1
O19 C20 C19 . . 105.5(5)
O19 C20 C21 . . 109.8(4)
C19 C20 C21 . . 110.9(5)
O19 C20 H20 . . 110.2
C19 C20 H20 . . 110.2
C21 C20 H20 . . 110.2
O15 C21 C22 . . 107.1(4)
O15 C21 C20 . . 109.5(4)
C22 C21 C20 . . 109.9(4)
O15 C21 H21 . . 110.1
C22 C21 H21 . . 110.1
C20 C21 H21 . . 110.1
O17 C22 C21 . . 109.8(4)
O17 C22 C23 . . 109.6(4)
C21 C22 C23 . . 108.7(4)
O17 C22 H22 . . 109.6
C21 C22 H22 . . 109.6
C23 C22 H22 . . 109.6
O18 C23 C22 . . 112.1(4)
O18 C23 C24 . . 111.2(4)
C22 C23 C24 . . 109.5(4)
O18 C23 H23 . . 108.0
C22 C23 H23 . . 108.0
C24 C23 H23 . . 108.0
O19 C24 O20 . . 111.3(4)
O19 C24 C23 . . 111.1(4)
O20 C24 C23 . . 107.6(4)
O19 C24 H24 . . 108.9
O20 C24 H24 . . 108.9
C23 C24 H24 . . 108.9
O21 C25 C26 . . 111.5(4)
O21 C25 H25A . . 109.3
C26 C25 H25A . . 109.3
O21 C25 H25B . . 109.3
C26 C25 H25B . . 109.3
H25A C25 H25B . . 108.0
O24 C26 C25 . . 106.1(4)
O24 C26 C27 . . 109.2(4)
C25 C26 C27 . . 113.0(4)
O24 C26 H26 . . 109.5
C25 C26 H26 . . 109.5
C27 C26 H26 . . 109.5
O20 C27 C26 . . 109.2(4)
O20 C27 C28 . . 108.0(3)
C26 C27 C28 . . 110.4(4)
O20 C27 H27 . . 109.7
C26 C27 H27 . . 109.7
C28 C27 H27 . . 109.7
O22 C28 C29 . . 110.1(4)
O22 C28 C27 . . 109.8(4)
C29 C28 C27 . . 109.5(4)
O22 C28 H28 . . 109.2
C29 C28 H28 . . 109.2
C27 C28 H28 . . 109.2
O23 C29 C28 . . 111.8(4)
O23 C29 C30 . . 110.0(4)
C28 C29 C30 . . 110.0(4)
O23 C29 H29 . . 108.3
C28 C29 H29 . . 108.3
C30 C29 H29 . . 108.3
O24 C30 O25 . . 111.5(4)
O24 C30 C29 . . 110.3(3)
O25 C30 C29 . . 108.0(4)
O24 C30 H30 . . 109.0
O25 C30 H30 . . 109.0
C29 C30 H30 . . 109.0
O26 C31 C32 . . 109.8(4)
O26 C31 H31A . . 109.7
C32 C31 H31A . . 109.7
O26 C31 H31B . . 109.7
C32 C31 H31B . . 109.7
H31A C31 H31B . . 108.2
O29 C32 C31 . . 105.7(4)
O29 C32 C33 . . 109.2(4)
C31 C32 C33 . . 112.4(4)
O29 C32 H32 . . 109.8
C31 C32 H32 . . 109.8
C33 C32 H32 . . 109.8
O25 C33 C34 . . 108.3(4)
O25 C33 C32 . . 109.7(4)
C34 C33 C32 . . 110.6(4)
O25 C33 H33 . . 109.4
C34 C33 H33 . . 109.4
C32 C33 H33 . . 109.4
O27 C34 C35 . . 110.1(4)
O27 C34 C33 . . 108.6(4)
C35 C34 C33 . . 108.3(4)
O27 C34 H34 . . 109.9
C35 C34 H34 . . 109.9
C33 C34 H34 . . 109.9
O28 C35 C34 . . 112.3(4)
O28 C35 C36 . . 110.5(4)
C34 C35 C36 . . 110.1(4)
O28 C35 H35 . . 107.9
C34 C35 H35 . . 107.9
C36 C35 H35 . . 107.9
O30 C36 O29 . . 111.1(4)
O30 C36 C35 . . 106.7(4)
O29 C36 C35 . . 110.1(4)
O30 C36 H36 . . 109.6
O29 C36 H36 . . 109.6
C35 C36 H36 . . 109.6
O31 C37 C38 . . 112.5(8)
O31 C37 H37A . . 109.1
C38 C37 H37A . . 109.1
O31 C37 H37B . . 109.1
C38 C37 H37B . . 109.1
H37A C37 H37B . . 107.8
O34 C38 C39 . . 110.2(4)
O34 C38 C37 . . 105.7(4)
C39 C38 C37 . . 110.2(5)
O34 C38 H38 . . 110.2
C39 C38 H38 . . 110.2
C37 C38 H38 . . 110.2
O30 C39 C40 . . 106.9(4)
O30 C39 C38 . . 109.4(4)
C40 C39 C38 . . 113.2(4)
O30 C39 H39 . . 109.0
C40 C39 H39 . . 109.0
C38 C39 H39 . . 109.0
O32 C40 C39 . . 107.5(4)
O32 C40 C41 . . 112.8(4)
C39 C40 C41 . . 110.6(4)
O32 C40 H40 . . 108.6
C39 C40 H40 . . 108.6
C41 C40 H40 . . 108.6
O33 C41 C40 . . 112.0(4)
O33 C41 C42 . . 110.4(4)
C40 C41 C42 . . 109.0(4)
O33 C41 H41 . . 108.5
C40 C41 H41 . . 108.5
C42 C41 H41 . . 108.5
O35 C42 O34 . . 111.6(4)
O35 C42 C41 . . 108.3(4)
O34 C42 C41 . . 109.8(4)
O35 C42 H42 . . 109.0
O34 C42 H42 . . 109.0
C41 C42 H42 . . 109.0
O42 C53 O43 . . 123.2(10)
O42 C53 C54B . . 115.2(16)
O43 C53 C54B . . 120.4(15)
O42 C53 C54A . . 130.5(16)
O43 C53 C54A . . 106.1(14)
C54A C55 H55A . . 109.5
C54A C55 H55B . . 109.5
H55A C55 H55B . . 109.5
C54A C55 H55C . . 109.5
H55A C55 H55C . . 109.5
H55B C55 H55C . . 109.5
C1 O1 H1C . . 109.5
C4 O2 H2A . . 109.5
C5 O3 H3A . . 109.5
C6 O4 C2 . . 115.6(4)
C6 O5 C9 . . 116.6(4)
C7 O6 H6A . . 109.5
C10 O7 H7 . . 109.5
C11 O8 H8A . . 109.5
C12 O9 C8 . . 113.8(3)
C12 O10 C15 . . 118.2(3)
C13 O11 H11A . . 109.5
C16 O12 H12A . . 109.5
C17 O13 H13 . . 109.5
C18 O14 C14 . . 112.9(4)
C18 O15 C21 . . 119.1(4)
C19 O16 H16A . . 109.5
C22 O17 H17A . . 109.5
C23 O18 H18A . . 109.5
C24 O19 C20 . . 115.1(4)
C24 O20 C27 . . 118.0(4)
C25 O21 H21A . . 109.5
C28 O22 H22A . . 109.5
C29 O23 H23A . . 109.5
C30 O24 C26 . . 114.4(3)
C30 O25 C33 . . 116.7(3)
C31 O26 H26A . . 109.5
C34 O27 H27A . . 109.5
C35 O28 H28A . . 109.5
C36 O29 C32 . . 113.5(4)
C36 O30 C39 . . 119.4(3)
C37 O31 H31 . . 109.5
C40 O32 H32A . . 109.5
C41 O33 H33A . . 109.5
C42 O34 C38 . . 115.1(4)
C42 O35 C3 . . 118.8(4)
C53 O43 H43 . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C54A O44A . 1.43(2)
C54A C53 . 1.51(2)
C54A C55 . 1.56(2)
C54A H54A . 1.0
C56A O44A . 1.385(15)
C56A C57A . 1.39
C56A C61A . 1.39
C57A C58A . 1.39
C57A H57A . 0.95
C58A C59A . 1.39
C58A H58A . 0.95
C59A C60A . 1.39
C59A H59A . 0.95
C60A C61A . 1.39
C60A H60A . 0.95
C61A H61A . 0.95
C54B O44B . 1.39(3)
C54B C53 . 1.49(2)
C54B C55 . 1.54(2)
C54B H54B . 1.0
C56B O44B . 1.339(16)
C56B C57B . 1.39
C56B C61B . 1.39
C57B C58B . 1.39
C57B C58B 2 1.80(3)
C57B H57B . 0.95
C58B C59B . 1.39
C58B C57B 2 1.80(3)
C58B H58B . 0.95
C59B C60B . 1.39
C59B H59B . 0.95
C60B C61B . 1.39
C60B H60B . 0.95
C61B H61B . 0.95
C1 O1 . 1.413(9)
C1 C2 . 1.490(7)
C1 H1A . 0.99
C1 H1B . 0.99
C2 O4 . 1.442(6)
C2 C3 . 1.541(6)
C2 H2 . 1.0
C3 O35 . 1.427(6)
C3 C4 . 1.519(6)
C3 H3 . 1.0
C4 O2 . 1.430(5)
C4 C5 . 1.519(7)
C4 H4 . 1.0
C5 O3 . 1.422(6)
C5 C6 . 1.530(6)
C5 H5 . 1.0
C6 O4 . 1.410(6)
C6 O5 . 1.421(6)
C6 H6 . 1.0
C7 O6 . 1.429(8)
C7 C8 . 1.512(7)
C7 H7A . 0.99
C7 H7B . 0.99
C8 O9 . 1.431(6)
C8 C9 . 1.530(6)
C8 H8 . 1.0
C9 O5 . 1.432(5)
C9 C10 . 1.525(6)
C9 H9 . 1.0
C10 O7 . 1.413(6)
C10 C11 . 1.510(6)
C10 H10 . 1.0
C11 O8 . 1.438(5)
C11 C12 . 1.522(6)
C11 H11 . 1.0
C12 O9 . 1.404(6)
C12 O10 . 1.425(6)
C12 H12 . 1.0
C13 O11 . 1.453(8)
C13 C14 . 1.512(8)
C13 H13A . 0.99
C13 H13B . 0.99
C14 O14 . 1.446(7)
C14 C15 . 1.523(7)
C14 H14 . 1.0
C15 O10 . 1.430(6)
C15 C16 . 1.524(7)
C15 H15 . 1.0
C16 O12 . 1.440(6)
C16 C17 . 1.519(7)
C16 H16 . 1.0
C17 O13 . 1.415(7)
C17 C18 . 1.534(7)
C17 H17 . 1.0
C18 O14 . 1.397(7)
C18 O15 . 1.407(6)
C18 H18 . 1.0
C19 C20 . 1.520(7)
C19 O16 . 1.599(13)
C19 H19A . 0.99
C19 H19B . 0.99
C20 O19 . 1.446(6)
C20 C21 . 1.541(7)
C20 H20 . 1.0
C21 O15 . 1.438(6)
C21 C22 . 1.515(7)
C21 H21 . 1.0
C22 O17 . 1.424(6)
C22 C23 . 1.518(7)
C22 H22 . 1.0
C23 O18 . 1.419(6)
C23 C24 . 1.520(7)
C23 H23 . 1.0
C24 O19 . 1.402(6)
C24 O20 . 1.417(6)
C24 H24 . 1.0
C25 O21 . 1.420(7)
C25 C26 . 1.507(6)
C25 H25A . 0.99
C25 H25B . 0.99
C26 O24 . 1.452(5)
C26 C27 . 1.521(6)
C26 H26 . 1.0
C27 O20 . 1.436(5)
C27 C28 . 1.522(6)
C27 H27 . 1.0
C28 O22 . 1.435(6)
C28 C29 . 1.518(6)
C28 H28 . 1.0
C29 O23 . 1.421(5)
C29 C30 . 1.523(6)
C29 H29 . 1.0
C30 O24 . 1.413(5)
C30 O25 . 1.418(6)
C30 H30 . 1.0
C31 O26 . 1.433(7)
C31 C32 . 1.512(7)
C31 H31A . 0.99
C31 H31B . 0.99
C32 O29 . 1.440(6)
C32 C33 . 1.534(7)
C32 H32 . 1.0
C33 O25 . 1.427(6)
C33 C34 . 1.521(6)
C33 H33 . 1.0
C34 O27 . 1.422(6)
C34 C35 . 1.518(7)
C34 H34 . 1.0
C35 O28 . 1.424(6)
C35 C36 . 1.519(7)
C35 H35 . 1.0
C36 O30 . 1.414(6)
C36 O29 . 1.424(6)
C36 H36 . 1.0
C37 O31 . 1.367(9)
C37 C38 . 1.558(10)
C37 H37A . 0.99
C37 H37B . 0.99
C38 O34 . 1.441(6)
C38 C39 . 1.524(7)
C38 H38 . 1.0
C39 O30 . 1.431(6)
C39 C40 . 1.517(7)
C39 H39 . 1.0
C40 O32 . 1.419(6)
C40 C41 . 1.518(7)
C40 H40 . 1.0
C41 O33 . 1.421(6)
C41 C42 . 1.524(6)
C41 H41 . 1.0
C42 O35 . 1.409(6)
C42 O34 . 1.410(6)
C42 H42 . 1.0
C53 O42 . 1.208(15)
C53 O43 . 1.314(14)
C55 H55A . 0.98
C55 H55B . 0.98
C55 H55C . 0.98
O1 H1C . 0.84
O2 H2A . 0.84
O3 H3A . 0.84
O6 H6A . 0.84
O7 H7 . 0.84
O8 H8A . 0.84
O11 H11A . 0.84
O12 H12A . 0.84
O13 H13 . 0.84
O16 H16A . 0.84
O17 H17A . 0.84
O18 H18A . 0.84
O21 H21A . 0.84
O22 H22A . 0.84
O23 H23A . 0.84
O26 H26A . 0.84
O27 H27A . 0.84
O28 H28A . 0.84
O31 H31 . 0.84
O32 H32A . 0.84
O33 H33A . 0.84
O43 H43 . 0.84
