#------------------------------------------------------------------------------
#$Date: 2025-04-05 05:34:44 +0300 (Sat, 05 Apr 2025) $
#$Revision: 298839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/00/7250031.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_7250031
loop_
_publ_author_name
'Recchia, Daniella L.'
'Barton, Benita'
'Hosten, Eric C.'
_publ_section_title
;
 Extremely effective separations of pyridine/picoline mixtures through
 supramolecular chemistry strategies employing
 (4R,5R)-bis(diphenylhydroxymethyl)-2-spiro-1′-cyclohexane-1,3-dioxolane
 as the host compound
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1960
_journal_page_last               1976
_journal_paper_doi               10.1039/D5CE00111K
_journal_volume                  27
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H34 O4, C6 H7 N'
_chemical_formula_sum            'C40 H41 N O4'
_chemical_formula_weight         599.74
_chemical_name_systematic
(4R,5R)-Bis(diphenyldioxymethyl)-2-spiro-1'-cyclohexane-1,3-dioxane
_chemical_temperature_decomposition 352.31
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                97.408(2)
_cell_angle_beta                 100.565(2)
_cell_angle_gamma                90.588(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5704(6)
_cell_length_b                   9.8658(5)
_cell_length_c                   17.3649(10)
_cell_measurement_reflns_used    9287
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.97
_cell_volume                     1597.37(16)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service V6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material
'PLATON (Spek, 2009) and MERCURY (Macrae, 2008)'
_computing_structure_refinement
'SHELXL-2019/2 (Sheldrick, 2015b)  and ShelXle (Hübschle, 2011)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'Bruker PHOTON II 7 detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            135115
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.307
_diffrn_reflns_theta_min         2.083
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             70
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9975
_exptl_absorpt_correction_T_min  0.9597
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2016/2 (Krause, 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             640
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 3-methylpyridine'
_exptl_crystal_size_max          0.555
_exptl_crystal_size_mid          0.491
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 6468 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.15(14)
_refine_ls_extinction_coef       0.0132(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         15818
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0274P)²+0.4768P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                14346
_reflns_number_total             15818
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00111k2.cif
_cod_data_source_block           aq103
_cod_depositor_comments
'Adding full bibliography for 7250028--7250031.cif.'
_cod_original_cell_volume        1597.38(16)
_cod_database_code               7250031
_shelx_shelxl_version_number     2019/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.980
loop_
_space_group_symop_operation_xyz
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O11 O 0.10834(17) 0.52981(15) 0.22600(9) 0.0279(3) Uani 1 1 d . . . . .
H11 H 0.141077 0.464202 0.199735 0.042 Uiso 1 1 calc R U . . .
O12 O 0.01829(15) 0.27192(15) 0.34557(9) 0.0247(3) Uani 1 1 d . . . . .
O13 O 0.20620(17) 0.14617(15) 0.31911(9) 0.0271(3) Uani 1 1 d . . . . .
O14 O 0.21734(16) 0.31783(15) 0.14838(9) 0.0270(3) Uani 1 1 d . . . . .
H14 H 0.296937 0.347158 0.142556 0.041 Uiso 1 1 calc R U . . .
O21 O 0.77773(16) 0.73889(15) 0.85630(9) 0.0273(3) Uani 1 1 d . . . . .
H21 H 0.698339 0.770722 0.861312 0.041 Uiso 1 1 calc R U . . .
O22 O 0.78557(17) 0.49052(15) 0.68485(9) 0.0265(3) Uani 1 1 d . . . . .
O23 O 0.96817(16) 0.60882(15) 0.65398(9) 0.0257(3) Uani 1 1 d . . . . .
O24 O 0.89301(17) 0.91703(15) 0.78109(9) 0.0288(3) Uani 1 1 d . . . . .
H24 H 0.856147 0.862863 0.805834 0.043 Uiso 1 1 calc R U . . .
N3 N 0.4254(2) 0.4766(2) 0.12225(15) 0.0422(5) Uani 1 1 d . . . . .
N4 N 0.5726(2) 0.9082(2) 0.88565(14) 0.0393(5) Uani 1 1 d . . . . .
C11 C 0.0607(2) 0.4830(2) 0.29141(12) 0.0213(4) Uani 1 1 d . . . . .
C12 C 0.0606(2) 0.3234(2) 0.27998(12) 0.0206(4) Uani 1 1 d . . . . .
H12 H -0.008126 0.287714 0.230724 0.025 Uiso 1 1 calc R U . . .
C13 C 0.2069(2) 0.2595(2) 0.27629(12) 0.0213(4) Uani 1 1 d . . . . .
H13 H 0.284361 0.326659 0.304234 0.026 Uiso 1 1 calc R U . . .
C14 C 0.2366(2) 0.2054(2) 0.19345(12) 0.0219(4) Uani 1 1 d . . . . .
C21 C 0.7572(2) 0.6062(2) 0.81069(12) 0.0222(4) Uani 1 1 d . . . . .
C22 C 0.7861(2) 0.6237(2) 0.72768(12) 0.0214(4) Uani 1 1 d . . . . .
H22 H 0.708750 0.677158 0.700036 0.026 Uiso 1 1 calc R U . . .
C23 C 0.9323(2) 0.6864(2) 0.72258(12) 0.0211(4) Uani 1 1 d . . . . .
H23 H 1.003273 0.670094 0.770136 0.025 Uiso 1 1 calc R U . . .
C24 C 0.9362(2) 0.8420(2) 0.71376(12) 0.0210(4) Uani 1 1 d . . . . .
C31 C 0.6469(3) 0.5430(3) 0.08948(14) 0.0359(5) Uani 1 1 d . . . . .
C32 C 0.5537(3) 0.4478(3) 0.10657(17) 0.0406(6) Uani 1 1 d . . . . .
H32 H 0.583205 0.356185 0.107133 0.049 Uiso 1 1 calc R U . . .
C33 C 0.3847(3) 0.6052(3) 0.12131(17) 0.0410(6) Uani 1 1 d . . . . .
H33 H 0.293568 0.627280 0.132631 0.049 Uiso 1 1 calc R U . . .
C34 C 0.4685(3) 0.7070(3) 0.10473(18) 0.0446(6) Uani 1 1 d . . . . .
H34 H 0.436131 0.797666 0.104450 0.053 Uiso 1 1 calc R U . . .
C35 C 0.6009(3) 0.6748(3) 0.08846(16) 0.0425(6) Uani 1 1 d . . . . .
H35 H 0.660512 0.743695 0.076520 0.051 Uiso 1 1 calc R U . . .
C36 C 0.7914(3) 0.5012(4) 0.07473(18) 0.0505(7) Uani 1 1 d . . . . .
H36A H 0.862553 0.527944 0.122776 0.076 Uiso 1 1 calc R U . . .
H36B H 0.815148 0.546581 0.031575 0.076 Uiso 1 1 calc R U . . .
H36C H 0.790741 0.401807 0.060221 0.076 Uiso 1 1 calc R U . . .
C41 C 0.3500(3) 0.9893(3) 0.91624(14) 0.0357(5) Uani 1 1 d . . . . .
C42 C 0.4439(3) 0.8861(3) 0.90227(16) 0.0386(6) Uani 1 1 d . . . . .
H42 H 0.414932 0.794610 0.904697 0.046 Uiso 1 1 calc R U . . .
C43 C 0.6128(3) 1.0369(3) 0.88272(16) 0.0398(6) Uani 1 1 d . . . . .
H43 H 0.703553 1.053843 0.870447 0.048 Uiso 1 1 calc R U . . .
C44 C 0.5287(3) 1.1462(3) 0.89667(17) 0.0433(6) Uani 1 1 d . . . . .
H44 H 0.561175 1.236903 0.894927 0.052 Uiso 1 1 calc R U . . .
C45 C 0.3959(3) 1.1210(3) 0.91325(16) 0.0426(6) Uani 1 1 d . . . . .
H45 H 0.335840 1.195002 0.922663 0.051 Uiso 1 1 calc R U . . .
C46 C 0.2052(3) 0.9540(4) 0.93185(18) 0.0506(7) Uani 1 1 d . . . . .
H46A H 0.196488 0.996088 0.984974 0.076 Uiso 1 1 calc R U . . .
H46B H 0.192938 0.854481 0.928035 0.076 Uiso 1 1 calc R U . . .
H46C H 0.131848 0.988526 0.892688 0.076 Uiso 1 1 calc R U . . .
C111 C 0.1592(2) 0.5428(2) 0.36856(13) 0.0229(4) Uani 1 1 d . . . . .
C112 C 0.2992(2) 0.5829(2) 0.36843(15) 0.0294(5) Uani 1 1 d . . . . .
H112 H 0.332903 0.576841 0.319970 0.035 Uiso 1 1 calc R U . . .
C113 C 0.3900(3) 0.6320(3) 0.43912(16) 0.0365(5) Uani 1 1 d . . . . .
H113 H 0.485513 0.658520 0.438598 0.044 Uiso 1 1 calc R U . . .
C114 C 0.3422(3) 0.6421(3) 0.50981(16) 0.0377(6) Uani 1 1 d . . . . .
H114 H 0.404847 0.674289 0.557917 0.045 Uiso 1 1 calc R U . . .
C115 C 0.2023(3) 0.6053(2) 0.51041(14) 0.0335(5) Uani 1 1 d . . . . .
H115 H 0.168471 0.613872 0.558869 0.040 Uiso 1 1 calc R U . . .
C116 C 0.1118(2) 0.5558(2) 0.44024(13) 0.0264(4) Uani 1 1 d . . . . .
H116 H 0.016098 0.530346 0.441105 0.032 Uiso 1 1 calc R U . . .
C121 C -0.0889(2) 0.5382(2) 0.29163(12) 0.0233(4) Uani 1 1 d . . . . .
C122 C -0.1061(2) 0.6762(2) 0.28302(13) 0.0284(5) Uani 1 1 d . . . . .
H122 H -0.027823 0.729859 0.275559 0.034 Uiso 1 1 calc R U . . .
C123 C -0.2362(3) 0.7358(2) 0.28526(15) 0.0340(5) Uani 1 1 d . . . . .
H123 H -0.246322 0.829723 0.279231 0.041 Uiso 1 1 calc R U . . .
C124 C -0.3510(3) 0.6595(3) 0.29620(14) 0.0343(5) Uani 1 1 d . . . . .
H124 H -0.439705 0.700809 0.298412 0.041 Uiso 1 1 calc R U . . .
C125 C -0.3357(3) 0.5225(3) 0.30389(15) 0.0358(5) Uani 1 1 d . . . . .
H125 H -0.414572 0.469249 0.310842 0.043 Uiso 1 1 calc R U . . .
C126 C -0.2056(2) 0.4621(2) 0.30151(15) 0.0314(5) Uani 1 1 d . . . . .
H126 H -0.196498 0.367773 0.306716 0.038 Uiso 1 1 calc R U . . .
C131 C 0.3896(2) 0.1564(2) 0.19752(13) 0.0234(4) Uani 1 1 d . . . . .
C132 C 0.4343(2) 0.1161(2) 0.12616(14) 0.0294(5) Uani 1 1 d . . . . .
H132 H 0.369163 0.116337 0.077794 0.035 Uiso 1 1 calc R U . . .
C133 C 0.5725(3) 0.0755(2) 0.12473(16) 0.0342(5) Uani 1 1 d . . . . .
H133 H 0.601011 0.048298 0.075595 0.041 Uiso 1 1 calc R U . . .
C134 C 0.6684(3) 0.0745(3) 0.19447(17) 0.0362(5) Uani 1 1 d . . . . .
H134 H 0.763159 0.047453 0.193552 0.043 Uiso 1 1 calc R U . . .
C135 C 0.6255(3) 0.1131(3) 0.26547(16) 0.0381(6) Uani 1 1 d . . . . .
H135 H 0.690968 0.111773 0.313626 0.046 Uiso 1 1 calc R U . . .
C136 C 0.4866(2) 0.1541(2) 0.26724(14) 0.0320(5) Uani 1 1 d . . . . .
H136 H 0.458465 0.180508 0.316555 0.038 Uiso 1 1 calc R U . . .
C141 C 0.1297(2) 0.0910(2) 0.15054(13) 0.0261(4) Uani 1 1 d . . . . .
C142 C 0.0181(3) 0.1191(3) 0.09216(14) 0.0351(5) Uani 1 1 d . . . . .
H142 H 0.005634 0.210062 0.080380 0.042 Uiso 1 1 calc R U . . .
C143 C -0.0758(3) 0.0143(4) 0.05067(17) 0.0489(8) Uani 1 1 d . . . . .
H143 H -0.151706 0.034191 0.010661 0.059 Uiso 1 1 calc R U . . .
C144 C -0.0589(3) -0.1177(4) 0.06742(19) 0.0541(8) Uani 1 1 d . . . . .
H144 H -0.121760 -0.189111 0.038147 0.065 Uiso 1 1 calc R U . . .
C145 C 0.0493(3) -0.1465(3) 0.12681(19) 0.0506(8) Uani 1 1 d . . . . .
H145 H 0.059303 -0.237218 0.139419 0.061 Uiso 1 1 calc R U . . .
C146 C 0.1438(3) -0.0426(2) 0.16820(16) 0.0353(5) Uani 1 1 d . . . . .
H146 H 0.218500 -0.062865 0.208798 0.042 Uiso 1 1 calc R U . . .
C151 C 0.1166(2) 0.1738(2) 0.37560(12) 0.0219(4) Uani 1 1 d . . . . .
C152 C 0.2030(2) 0.2319(2) 0.45558(13) 0.0259(4) Uani 1 1 d . . . . .
H15A H 0.137561 0.265548 0.491305 0.031 Uiso 1 1 calc R U . . .
H15B H 0.262806 0.310695 0.449213 0.031 Uiso 1 1 calc R U . . .
C153 C 0.2979(3) 0.1255(2) 0.49283(14) 0.0333(5) Uani 1 1 d . . . . .
H15C H 0.372183 0.101364 0.461079 0.040 Uiso 1 1 calc R U . . .
H15D H 0.345712 0.164575 0.546710 0.040 Uiso 1 1 calc R U . . .
C154 C 0.2119(3) -0.0029(3) 0.49728(15) 0.0350(5) Uani 1 1 d . . . . .
H15E H 0.143053 0.019688 0.532765 0.042 Uiso 1 1 calc R U . . .
H15F H 0.276470 -0.071483 0.519727 0.042 Uiso 1 1 calc R U . . .
C155 C 0.1324(3) -0.0629(2) 0.41572(15) 0.0315(5) Uani 1 1 d . . . . .
H15G H 0.075056 -0.144675 0.420129 0.038 Uiso 1 1 calc R U . . .
H15H H 0.201420 -0.091598 0.381277 0.038 Uiso 1 1 calc R U . . .
C156 C 0.0346(2) 0.0427(2) 0.37874(14) 0.0275(5) Uani 1 1 d . . . . .
H15I H -0.011742 0.003915 0.324527 0.033 Uiso 1 1 calc R U . . .
H15J H -0.040881 0.063635 0.410155 0.033 Uiso 1 1 calc R U . . .
C211 C 0.6032(2) 0.5540(2) 0.80621(13) 0.0243(4) Uani 1 1 d . . . . .
C212 C 0.5058(3) 0.5211(2) 0.73614(14) 0.0322(5) Uani 1 1 d . . . . .
H212 H 0.534437 0.525990 0.686968 0.039 Uiso 1 1 calc R U . . .
C213 C 0.3658(3) 0.4806(3) 0.73762(17) 0.0387(6) Uani 1 1 d . . . . .
H213 H 0.299900 0.458285 0.689431 0.046 Uiso 1 1 calc R U . . .
C214 C 0.3229(3) 0.4730(3) 0.80857(17) 0.0386(6) Uani 1 1 d . . . . .
H214 H 0.227557 0.446307 0.809342 0.046 Uiso 1 1 calc R U . . .
C215 C 0.4190(3) 0.5042(3) 0.87836(16) 0.0365(6) Uani 1 1 d . . . . .
H215 H 0.390028 0.498561 0.927359 0.044 Uiso 1 1 calc R U . . .
C216 C 0.5583(3) 0.5441(2) 0.87721(15) 0.0316(5) Uani 1 1 d . . . . .
H216 H 0.623844 0.564895 0.925638 0.038 Uiso 1 1 calc R U . . .
C221 C 0.8632(2) 0.5117(2) 0.85236(13) 0.0266(4) Uani 1 1 d . . . . .
C222 C 0.8488(3) 0.3697(3) 0.83292(16) 0.0369(5) Uani 1 1 d . . . . .
H222 H 0.773522 0.330685 0.792306 0.044 Uiso 1 1 calc R U . . .
C223 C 0.9439(3) 0.2851(3) 0.8726(2) 0.0499(8) Uani 1 1 d . . . . .
H223 H 0.934266 0.188676 0.858633 0.060 Uiso 1 1 calc R U . . .
C224 C 1.0527(3) 0.3414(4) 0.9325(2) 0.0541(9) Uani 1 1 d . . . . .
H224 H 1.116174 0.283553 0.960585 0.065 Uiso 1 1 calc R U . . .
C225 C 1.0688(3) 0.4802(4) 0.95129(17) 0.0491(8) Uani 1 1 d . . . . .
H225 H 1.144400 0.518366 0.991983 0.059 Uiso 1 1 calc R U . . .
C226 C 0.9753(3) 0.5665(3) 0.91121(15) 0.0359(5) Uani 1 1 d . . . . .
H226 H 0.988297 0.662852 0.924226 0.043 Uiso 1 1 calc R U . . .
C231 C 1.0866(2) 0.8975(2) 0.71294(12) 0.0235(4) Uani 1 1 d . . . . .
C232 C 1.2044(2) 0.8176(2) 0.71054(14) 0.0288(5) Uani 1 1 d . . . . .
H232 H 1.195347 0.721652 0.710514 0.035 Uiso 1 1 calc R U . . .
C233 C 1.3359(2) 0.8772(3) 0.70817(14) 0.0337(5) Uani 1 1 d . . . . .
H233 H 1.415868 0.821479 0.706219 0.040 Uiso 1 1 calc R U . . .
C234 C 1.3506(3) 1.0171(3) 0.70865(14) 0.0354(5) Uani 1 1 d . . . . .
H234 H 1.440177 1.057472 0.706633 0.042 Uiso 1 1 calc R U . . .
C235 C 1.2339(3) 1.0974(3) 0.71207(15) 0.0364(5) Uani 1 1 d . . . . .
H235 H 1.243551 1.193555 0.713042 0.044 Uiso 1 1 calc R U . . .
C236 C 1.1026(3) 1.0384(2) 0.71410(14) 0.0303(5) Uani 1 1 d . . . . .
H236 H 1.022997 1.094521 0.716308 0.036 Uiso 1 1 calc R U . . .
C241 C 0.8373(2) 0.8700(2) 0.63809(13) 0.0235(4) Uani 1 1 d . . . . .
C242 C 0.7010(2) 0.9154(2) 0.64044(15) 0.0307(5) Uani 1 1 d . . . . .
H242 H 0.670238 0.932880 0.689662 0.037 Uiso 1 1 calc R U . . .
C243 C 0.6095(3) 0.9353(3) 0.57109(17) 0.0403(6) Uani 1 1 d . . . . .
H243 H 0.516114 0.965485 0.573140 0.048 Uiso 1 1 calc R U . . .
C244 C 0.6533(3) 0.9116(3) 0.49962(16) 0.0402(6) Uani 1 1 d . . . . .
H244 H 0.590196 0.924995 0.452391 0.048 Uiso 1 1 calc R U . . .
C245 C 0.7896(3) 0.8682(2) 0.49659(14) 0.0350(5) Uani 1 1 d . . . . .
H245 H 0.820199 0.852157 0.447267 0.042 Uiso 1 1 calc R U . . .
C246 C 0.8814(2) 0.8481(2) 0.56551(13) 0.0272(4) Uani 1 1 d . . . . .
H246 H 0.975086 0.819159 0.563206 0.033 Uiso 1 1 calc R U . . .
C251 C 0.8664(2) 0.4975(2) 0.62433(12) 0.0238(4) Uani 1 1 d . . . . .
C252 C 0.7700(2) 0.5234(2) 0.54824(13) 0.0269(4) Uani 1 1 d . . . . .
H25A H 0.828951 0.544913 0.509826 0.032 Uiso 1 1 calc R U . . .
H25B H 0.711868 0.603528 0.559262 0.032 Uiso 1 1 calc R U . . .
C253 C 0.6716(3) 0.3991(2) 0.51209(15) 0.0360(5) Uani 1 1 d . . . . .
H25C H 0.605082 0.383662 0.547792 0.043 Uiso 1 1 calc R U . . .
H25D H 0.614829 0.416844 0.460943 0.043 Uiso 1 1 calc R U . . .
C254 C 0.7578(3) 0.2715(3) 0.49912(16) 0.0416(6) Uani 1 1 d . . . . .
H25E H 0.692567 0.192032 0.476521 0.050 Uiso 1 1 calc R U . . .
H25F H 0.820356 0.284852 0.460978 0.050 Uiso 1 1 calc R U . . .
C255 C 0.8478(3) 0.2431(2) 0.57671(16) 0.0384(6) Uani 1 1 d . . . . .
H25G H 0.905279 0.162002 0.566980 0.046 Uiso 1 1 calc R U . . .
H25H H 0.784907 0.222869 0.613428 0.046 Uiso 1 1 calc R U . . .
C256 C 0.9466(3) 0.3664(2) 0.61445(14) 0.0312(5) Uani 1 1 d . . . . .
H25I H 0.997885 0.348494 0.666864 0.037 Uiso 1 1 calc R U . . .
H25J H 1.018090 0.378104 0.581025 0.037 Uiso 1 1 calc R U . . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4.00 -3.00 -1.00 0.1750
-4.00 -1.00 -3.00 0.1740
-3.00 -3.00 -4.00 0.1700
-2.00 -1.00 -4.00 0.1430
-2.00 -1.00 1.00 0.1930
-2.00 -1.00 2.00 0.1980
-1.00 -1.00 -3.00 0.1440
-1.00 0.00 -4.00 0.1190
-1.00 0.00 4.00 0.2330
-1.00 0.00 0.00 0.2000
-1.00 -1.00 2.00 0.2060
-1.00 -1.00 3.00 0.1910
-1.00 4.00 0.00 0.1550
0.00 3.00 -2.00 0.1290
0.00 -3.00 2.00 0.2320
0.00 0.00 -1.00 0.0830
0.00 0.00 1.00 0.1730
0.00 1.00 4.00 0.1850
0.00 1.00 1.00 0.1850
1.00 0.00 4.00 0.1300
1.00 0.00 -4.00 0.1400
2.00 3.00 4.00 0.1640
3.00 0.00 4.00 0.1410
3.00 0.00 -2.00 0.2230
4.00 3.00 4.00 0.1670
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 O11 H11 109.5 . . ?
C12 O12 C151 110.69(15) . . ?
C151 O13 C13 108.92(15) . . ?
C14 O14 H14 109.5 . . ?
C21 O21 H21 109.5 . . ?
C251 O22 C22 108.14(15) . . ?
C23 O23 C251 110.40(15) . . ?
C24 O24 H24 109.5 . . ?
C32 N3 C33 117.7(2) . . ?
C43 N4 C42 117.7(2) . . ?
O11 C11 C111 109.66(17) . . ?
O11 C11 C121 106.44(16) . . ?
C111 C11 C121 108.88(16) . . ?
O11 C11 C12 108.26(16) . . ?
C111 C11 C12 111.03(16) . . ?
C121 C11 C12 112.45(16) . . ?
O12 C12 C13 103.71(15) . . ?
O12 C12 C11 110.27(16) . . ?
C13 C12 C11 115.70(16) . . ?
O12 C12 H12 109.0 . . ?
C13 C12 H12 109.0 . . ?
C11 C12 H12 109.0 . . ?
O13 C13 C14 107.72(16) . . ?
O13 C13 C12 103.80(16) . . ?
C14 C13 C12 117.00(16) . . ?
O13 C13 H13 109.3 . . ?
C14 C13 H13 109.3 . . ?
C12 C13 H13 109.3 . . ?
O14 C14 C141 107.20(17) . . ?
O14 C14 C131 109.20(16) . . ?
C141 C14 C131 110.24(17) . . ?
O14 C14 C13 106.29(16) . . ?
C141 C14 C13 111.99(16) . . ?
C131 C14 C13 111.71(17) . . ?
O21 C21 C221 107.51(17) . . ?
O21 C21 C211 109.10(16) . . ?
C221 C21 C211 110.61(17) . . ?
O21 C21 C22 106.48(16) . . ?
C221 C21 C22 111.81(16) . . ?
C211 C21 C22 111.14(17) . . ?
O22 C22 C23 103.15(15) . . ?
O22 C22 C21 107.35(15) . . ?
C23 C22 C21 117.62(17) . . ?
O22 C22 H22 109.4 . . ?
C23 C22 H22 109.4 . . ?
C21 C22 H22 109.4 . . ?
O23 C23 C22 103.57(15) . . ?
O23 C23 C24 109.53(16) . . ?
C22 C23 C24 116.09(16) . . ?
O23 C23 H23 109.1 . . ?
C22 C23 H23 109.1 . . ?
C24 C23 H23 109.1 . . ?
O24 C24 C241 109.90(17) . . ?
O24 C24 C231 105.96(16) . . ?
C241 C24 C231 108.66(17) . . ?
O24 C24 C23 108.58(16) . . ?
C241 C24 C23 110.89(16) . . ?
C231 C24 C23 112.72(16) . . ?
C35 C31 C32 116.7(2) . . ?
C35 C31 C36 123.2(2) . . ?
C32 C31 C36 120.1(3) . . ?
N3 C32 C31 124.1(3) . . ?
N3 C32 H32 118.0 . . ?
C31 C32 H32 118.0 . . ?
N3 C33 C34 122.9(3) . . ?
N3 C33 H33 118.6 . . ?
C34 C33 H33 118.6 . . ?
C33 C34 C35 118.5(3) . . ?
C33 C34 H34 120.8 . . ?
C35 C34 H34 120.8 . . ?
C31 C35 C34 120.2(2) . . ?
C31 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C31 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C31 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C45 C41 C42 116.6(2) . . ?
C45 C41 C46 123.3(2) . . ?
C42 C41 C46 120.1(3) . . ?
N4 C42 C41 123.8(3) . . ?
N4 C42 H42 118.1 . . ?
C41 C42 H42 118.1 . . ?
N4 C43 C44 122.9(3) . . ?
N4 C43 H43 118.5 . . ?
C44 C43 H43 118.5 . . ?
C43 C44 C45 118.4(3) . . ?
C43 C44 H44 120.8 . . ?
C45 C44 H44 120.8 . . ?
C41 C45 C44 120.5(2) . . ?
C41 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C41 C46 H46A 109.5 . . ?
C41 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C41 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C116 C111 C112 118.6(2) . . ?
C116 C111 C11 120.86(19) . . ?
C112 C111 C11 120.5(2) . . ?
C111 C112 C113 120.3(2) . . ?
C111 C112 H112 119.9 . . ?
C113 C112 H112 119.9 . . ?
C114 C113 C112 120.4(2) . . ?
C114 C113 H113 119.8 . . ?
C112 C113 H113 119.8 . . ?
C113 C114 C115 119.8(2) . . ?
C113 C114 H114 120.1 . . ?
C115 C114 H114 120.1 . . ?
C114 C115 C116 120.0(2) . . ?
C114 C115 H115 120.0 . . ?
C116 C115 H115 120.0 . . ?
C115 C116 C111 120.9(2) . . ?
C115 C116 H116 119.6 . . ?
C111 C116 H116 119.6 . . ?
C126 C121 C122 118.3(2) . . ?
C126 C121 C11 124.89(19) . . ?
C122 C121 C11 116.75(19) . . ?
C123 C122 C121 120.7(2) . . ?
C123 C122 H122 119.7 . . ?
C121 C122 H122 119.7 . . ?
C124 C123 C122 120.5(2) . . ?
C124 C123 H123 119.8 . . ?
C122 C123 H123 119.8 . . ?
C123 C124 C125 119.3(2) . . ?
C123 C124 H124 120.3 . . ?
C125 C124 H124 120.3 . . ?
C124 C125 C126 120.5(2) . . ?
C124 C125 H125 119.8 . . ?
C126 C125 H125 119.8 . . ?
C121 C126 C125 120.7(2) . . ?
C121 C126 H126 119.7 . . ?
C125 C126 H126 119.7 . . ?
C136 C131 C132 118.2(2) . . ?
C136 C131 C14 124.21(19) . . ?
C132 C131 C14 117.53(19) . . ?
C133 C132 C131 121.1(2) . . ?
C133 C132 H132 119.5 . . ?
C131 C132 H132 119.5 . . ?
C134 C133 C132 120.2(2) . . ?
C134 C133 H133 119.9 . . ?
C132 C133 H133 119.9 . . ?
C135 C134 C133 119.4(2) . . ?
C135 C134 H134 120.3 . . ?
C133 C134 H134 120.3 . . ?
C134 C135 C136 120.6(2) . . ?
C134 C135 H135 119.7 . . ?
C136 C135 H135 119.7 . . ?
C131 C136 C135 120.5(2) . . ?
C131 C136 H136 119.8 . . ?
C135 C136 H136 119.8 . . ?
C142 C141 C146 118.9(2) . . ?
C142 C141 C14 120.1(2) . . ?
C146 C141 C14 121.0(2) . . ?
C141 C142 C143 120.3(3) . . ?
C141 C142 H142 119.9 . . ?
C143 C142 H142 119.9 . . ?
C144 C143 C142 120.3(3) . . ?
C144 C143 H143 119.8 . . ?
C142 C143 H143 119.8 . . ?
C143 C144 C145 120.0(3) . . ?
C143 C144 H144 120.0 . . ?
C145 C144 H144 120.0 . . ?
C144 C145 C146 120.0(3) . . ?
C144 C145 H145 120.0 . . ?
C146 C145 H145 120.0 . . ?
C145 C146 C141 120.5(3) . . ?
C145 C146 H146 119.8 . . ?
C141 C146 H146 119.8 . . ?
O13 C151 O12 105.73(15) . . ?
O13 C151 C156 108.31(17) . . ?
O12 C151 C156 108.87(17) . . ?
O13 C151 C152 110.69(17) . . ?
O12 C151 C152 110.53(16) . . ?
C156 C151 C152 112.46(17) . . ?
C151 C152 C153 111.81(18) . . ?
C151 C152 H15A 109.3 . . ?
C153 C152 H15A 109.3 . . ?
C151 C152 H15B 109.3 . . ?
C153 C152 H15B 109.3 . . ?
H15A C152 H15B 107.9 . . ?
C154 C153 C152 111.1(2) . . ?
C154 C153 H15C 109.4 . . ?
C152 C153 H15C 109.4 . . ?
C154 C153 H15D 109.4 . . ?
C152 C153 H15D 109.4 . . ?
H15C C153 H15D 108.0 . . ?
C153 C154 C155 110.84(19) . . ?
C153 C154 H15E 109.5 . . ?
C155 C154 H15E 109.5 . . ?
C153 C154 H15F 109.5 . . ?
C155 C154 H15F 109.5 . . ?
H15E C154 H15F 108.1 . . ?
C154 C155 C156 110.50(19) . . ?
C154 C155 H15G 109.6 . . ?
C156 C155 H15G 109.5 . . ?
C154 C155 H15H 109.5 . . ?
C156 C155 H15H 109.5 . . ?
H15G C155 H15H 108.1 . . ?
C151 C156 C155 111.41(18) . . ?
C151 C156 H15I 109.3 . . ?
C155 C156 H15I 109.3 . . ?
C151 C156 H15J 109.3 . . ?
C155 C156 H15J 109.3 . . ?
H15I C156 H15J 108.0 . . ?
C212 C211 C216 118.4(2) . . ?
C212 C211 C21 124.06(19) . . ?
C216 C211 C21 117.54(19) . . ?
C211 C212 C213 120.3(2) . . ?
C211 C212 H212 119.8 . . ?
C213 C212 H212 119.8 . . ?
C214 C213 C212 120.4(2) . . ?
C214 C213 H213 119.8 . . ?
C212 C213 H213 119.8 . . ?
C215 C214 C213 119.7(2) . . ?
C215 C214 H214 120.2 . . ?
C213 C214 H214 120.2 . . ?
C214 C215 C216 120.1(2) . . ?
C214 C215 H215 119.9 . . ?
C216 C215 H215 119.9 . . ?
C215 C216 C211 121.1(2) . . ?
C215 C216 H216 119.5 . . ?
C211 C216 H216 119.5 . . ?
C226 C221 C222 118.7(2) . . ?
C226 C221 C21 120.2(2) . . ?
C222 C221 C21 121.1(2) . . ?
C223 C222 C221 120.5(3) . . ?
C223 C222 H222 119.8 . . ?
C221 C222 H222 119.8 . . ?
C224 C223 C222 120.0(3) . . ?
C224 C223 H223 120.0 . . ?
C222 C223 H223 120.0 . . ?
C225 C224 C223 120.0(3) . . ?
C225 C224 H224 120.0 . . ?
C223 C224 H224 120.0 . . ?
C224 C225 C226 120.6(3) . . ?
C224 C225 H225 119.7 . . ?
C226 C225 H225 119.7 . . ?
C221 C226 C225 120.2(3) . . ?
C221 C226 H226 119.9 . . ?
C225 C226 H226 119.9 . . ?
C232 C231 C236 118.8(2) . . ?
C232 C231 C24 124.63(19) . . ?
C236 C231 C24 116.52(19) . . ?
C231 C232 C233 120.4(2) . . ?
C231 C232 H232 119.8 . . ?
C233 C232 H232 119.8 . . ?
C234 C233 C232 120.4(2) . . ?
C234 C233 H233 119.8 . . ?
C232 C233 H233 119.8 . . ?
C235 C234 C233 119.4(2) . . ?
C235 C234 H234 120.3 . . ?
C233 C234 H234 120.3 . . ?
C234 C235 C236 120.4(2) . . ?
C234 C235 H235 119.8 . . ?
C236 C235 H235 119.8 . . ?
C235 C236 C231 120.6(2) . . ?
C235 C236 H236 119.7 . . ?
C231 C236 H236 119.7 . . ?
C242 C241 C246 118.9(2) . . ?
C242 C241 C24 120.5(2) . . ?
C246 C241 C24 120.61(19) . . ?
C241 C242 C243 120.3(2) . . ?
C241 C242 H242 119.8 . . ?
C243 C242 H242 119.8 . . ?
C244 C243 C242 120.4(2) . . ?
C244 C243 H243 119.8 . . ?
C242 C243 H243 119.8 . . ?
C243 C244 C245 119.9(2) . . ?
C243 C244 H244 120.1 . . ?
C245 C244 H244 120.1 . . ?
C244 C245 C246 120.0(2) . . ?
C244 C245 H245 120.0 . . ?
C246 C245 H245 120.0 . . ?
C245 C246 C241 120.5(2) . . ?
C245 C246 H246 119.7 . . ?
C241 C246 H246 119.7 . . ?
O22 C251 O23 105.23(16) . . ?
O22 C251 C256 108.72(17) . . ?
O23 C251 C256 108.42(18) . . ?
O22 C251 C252 110.21(17) . . ?
O23 C251 C252 111.40(17) . . ?
C256 C251 C252 112.55(18) . . ?
C251 C252 C253 111.50(19) . . ?
C251 C252 H25A 109.3 . . ?
C253 C252 H25A 109.3 . . ?
C251 C252 H25B 109.3 . . ?
C253 C252 H25B 109.3 . . ?
H25A C252 H25B 108.0 . . ?
C254 C253 C252 110.6(2) . . ?
C254 C253 H25C 109.5 . . ?
C252 C253 H25C 109.5 . . ?
C254 C253 H25D 109.5 . . ?
C252 C253 H25D 109.5 . . ?
H25C C253 H25D 108.1 . . ?
C255 C254 C253 110.6(2) . . ?
C255 C254 H25E 109.5 . . ?
C253 C254 H25E 109.5 . . ?
C255 C254 H25F 109.5 . . ?
C253 C254 H25F 109.5 . . ?
H25E C254 H25F 108.1 . . ?
C254 C255 C256 110.7(2) . . ?
C254 C255 H25G 109.5 . . ?
C256 C255 H25G 109.5 . . ?
C254 C255 H25H 109.5 . . ?
C256 C255 H25H 109.5 . . ?
H25G C255 H25H 108.1 . . ?
C251 C256 C255 112.4(2) . . ?
C251 C256 H25I 109.1 . . ?
C255 C256 H25I 109.1 . . ?
C251 C256 H25J 109.1 . . ?
C255 C256 H25J 109.1 . . ?
H25I C256 H25J 107.9 . . ?
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
O11 C11 1.425(2) . ?
O11 H11 0.8400 . ?
O12 C12 1.426(2) . ?
O12 C151 1.437(2) . ?
O13 C151 1.420(2) . ?
O13 C13 1.421(2) . ?
O14 C14 1.433(2) . ?
O14 H14 0.8400 . ?
O21 C21 1.431(2) . ?
O21 H21 0.8400 . ?
O22 C251 1.423(2) . ?
O22 C22 1.423(2) . ?
O23 C23 1.429(2) . ?
O23 C251 1.438(3) . ?
O24 C24 1.431(2) . ?
O24 H24 0.8400 . ?
N3 C32 1.332(3) . ?
N3 C33 1.332(4) . ?
N4 C43 1.332(4) . ?
N4 C42 1.337(3) . ?
C11 C111 1.534(3) . ?
C11 C121 1.538(3) . ?
C11 C12 1.561(3) . ?
C12 C13 1.549(3) . ?
C12 H12 1.0000 . ?
C13 C14 1.546(3) . ?
C13 H13 1.0000 . ?
C14 C141 1.535(3) . ?
C14 C131 1.539(3) . ?
C21 C221 1.531(3) . ?
C21 C211 1.541(3) . ?
C21 C22 1.547(3) . ?
C22 C23 1.546(3) . ?
C22 H22 1.0000 . ?
C23 C24 1.562(3) . ?
C23 H23 1.0000 . ?
C24 C241 1.530(3) . ?
C24 C231 1.538(3) . ?
C31 C35 1.379(4) . ?
C31 C32 1.385(4) . ?
C31 C36 1.505(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.370(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C41 C45 1.378(4) . ?
C41 C42 1.392(4) . ?
C41 C46 1.506(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.376(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.380(4) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C111 C116 1.393(3) . ?
C111 C112 1.394(3) . ?
C112 C113 1.394(3) . ?
C112 H112 0.9500 . ?
C113 C114 1.379(4) . ?
C113 H113 0.9500 . ?
C114 C115 1.385(4) . ?
C114 H114 0.9500 . ?
C115 C116 1.388(3) . ?
C115 H115 0.9500 . ?
C116 H116 0.9500 . ?
C121 C126 1.387(3) . ?
C121 C122 1.397(3) . ?
C122 C123 1.387(3) . ?
C122 H122 0.9500 . ?
C123 C124 1.381(4) . ?
C123 H123 0.9500 . ?
C124 C125 1.382(4) . ?
C124 H124 0.9500 . ?
C125 C126 1.391(3) . ?
C125 H125 0.9500 . ?
C126 H126 0.9500 . ?
C131 C136 1.387(3) . ?
C131 C132 1.395(3) . ?
C132 C133 1.389(3) . ?
C132 H132 0.9500 . ?
C133 C134 1.380(4) . ?
C133 H133 0.9500 . ?
C134 C135 1.379(4) . ?
C134 H134 0.9500 . ?
C135 C136 1.398(3) . ?
C135 H135 0.9500 . ?
C136 H136 0.9500 . ?
C141 C142 1.388(3) . ?
C141 C146 1.393(3) . ?
C142 C143 1.395(4) . ?
C142 H142 0.9500 . ?
C143 C144 1.375(5) . ?
C143 H143 0.9500 . ?
C144 C145 1.381(5) . ?
C144 H144 0.9500 . ?
C145 C146 1.392(4) . ?
C145 H145 0.9500 . ?
C146 H146 0.9500 . ?
C151 C156 1.518(3) . ?
C151 C152 1.518(3) . ?
C152 C153 1.525(3) . ?
C152 H15A 0.9900 . ?
C152 H15B 0.9900 . ?
C153 C154 1.521(3) . ?
C153 H15C 0.9900 . ?
C153 H15D 0.9900 . ?
C154 C155 1.522(3) . ?
C154 H15E 0.9900 . ?
C154 H15F 0.9900 . ?
C155 C156 1.532(3) . ?
C155 H15G 0.9900 . ?
C155 H15H 0.9900 . ?
C156 H15I 0.9900 . ?
C156 H15J 0.9900 . ?
C211 C212 1.389(3) . ?
C211 C216 1.393(3) . ?
C212 C213 1.400(3) . ?
C212 H212 0.9500 . ?
C213 C214 1.379(4) . ?
C213 H213 0.9500 . ?
C214 C215 1.378(4) . ?
C214 H214 0.9500 . ?
C215 C216 1.390(3) . ?
C215 H215 0.9500 . ?
C216 H216 0.9500 . ?
C221 C226 1.389(3) . ?
C221 C222 1.398(3) . ?
C222 C223 1.391(4) . ?
C222 H222 0.9500 . ?
C223 C224 1.384(5) . ?
C223 H223 0.9500 . ?
C224 C225 1.366(5) . ?
C224 H224 0.9500 . ?
C225 C226 1.397(4) . ?
C225 H225 0.9500 . ?
C226 H226 0.9500 . ?
C231 C232 1.386(3) . ?
C231 C236 1.394(3) . ?
C232 C233 1.393(3) . ?
C232 H232 0.9500 . ?
C233 C234 1.385(4) . ?
C233 H233 0.9500 . ?
C234 C235 1.382(4) . ?
C234 H234 0.9500 . ?
C235 C236 1.387(3) . ?
C235 H235 0.9500 . ?
C236 H236 0.9500 . ?
C241 C242 1.389(3) . ?
C241 C246 1.393(3) . ?
C242 C243 1.391(4) . ?
C242 H242 0.9500 . ?
C243 C244 1.374(4) . ?
C243 H243 0.9500 . ?
C244 C245 1.385(4) . ?
C244 H244 0.9500 . ?
C245 C246 1.387(3) . ?
C245 H245 0.9500 . ?
C246 H246 0.9500 . ?
C251 C256 1.517(3) . ?
C251 C252 1.519(3) . ?
C252 C253 1.532(3) . ?
C252 H25A 0.9900 . ?
C252 H25B 0.9900 . ?
C253 C254 1.527(4) . ?
C253 H25C 0.9900 . ?
C253 H25D 0.9900 . ?
C254 C255 1.521(4) . ?
C254 H25E 0.9900 . ?
C254 H25F 0.9900 . ?
C255 C256 1.531(3) . ?
C255 H25G 0.9900 . ?
C255 H25H 0.9900 . ?
C256 H25I 0.9900 . ?
C256 H25J 0.9900 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O11 H11 O14 0.84 1.83 2.667(2) 176 . yes
O14 H14 N3 0.84 1.87 2.660(3) 155 . yes
O21 H21 N4 0.84 1.88 2.668(3) 155 . yes
O24 H24 O21 0.84 1.82 2.663(2) 177 . yes
C112 H112 O11 0.95 2.45 2.778(3) 100 . yes
C126 H126 O12 0.95 2.30 2.924(3) 123 . yes
C136 H136 O13 0.95 2.44 2.987(3) 116 . yes
C142 H142 O14 0.95 2.32 2.680(3) 102 . yes
C212 H212 O22 0.95 2.44 2.979(3) 116 . yes
C226 H226 O21 0.95 2.32 2.683(3) 102 . yes
C232 H232 O23 0.95 2.41 2.981(3) 118 . yes
C242 H242 O24 0.95 2.43 2.772(3) 101 . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C151 O12 C12 C13 -6.0(2) . . . . ?
C151 O12 C12 C11 -130.41(17) . . . . ?
O11 C11 C12 O12 178.01(16) . . . . ?
C111 C11 C12 O12 57.6(2) . . . . ?
C121 C11 C12 O12 -64.7(2) . . . . ?
O11 C11 C12 C13 60.8(2) . . . . ?
C111 C11 C12 C13 -59.7(2) . . . . ?
C121 C11 C12 C13 178.05(17) . . . . ?
C151 O13 C13 C14 -152.14(16) . . . . ?
C151 O13 C13 C12 -27.4(2) . . . . ?
O12 C12 C13 O13 19.97(19) . . . . ?
C11 C12 C13 O13 140.84(17) . . . . ?
O12 C12 C13 C14 138.45(17) . . . . ?
C11 C12 C13 C14 -100.7(2) . . . . ?
O13 C13 C14 O14 172.28(16) . . . . ?
C12 C13 C14 O14 55.9(2) . . . . ?
O13 C13 C14 C141 55.5(2) . . . . ?
C12 C13 C14 C141 -60.8(2) . . . . ?
O13 C13 C14 C131 -68.7(2) . . . . ?
C12 C13 C14 C131 174.96(17) . . . . ?
C251 O22 C22 C23 -31.5(2) . . . . ?
C251 O22 C22 C21 -156.37(16) . . . . ?
O21 C21 C22 O22 172.15(16) . . . . ?
C221 C21 C22 O22 55.0(2) . . . . ?
C211 C21 C22 O22 -69.1(2) . . . . ?
O21 C21 C22 C23 56.5(2) . . . . ?
C221 C21 C22 C23 -60.6(2) . . . . ?
C211 C21 C22 C23 175.23(17) . . . . ?
C251 O23 C23 C22 -6.8(2) . . . . ?
C251 O23 C23 C24 -131.26(17) . . . . ?
O22 C22 C23 O23 22.93(19) . . . . ?
C21 C22 C23 O23 140.82(17) . . . . ?
O22 C22 C23 C24 143.00(16) . . . . ?
C21 C22 C23 C24 -99.1(2) . . . . ?
O23 C23 C24 O24 177.09(16) . . . . ?
C22 C23 C24 O24 60.3(2) . . . . ?
O23 C23 C24 C241 56.2(2) . . . . ?
C22 C23 C24 C241 -60.5(2) . . . . ?
O23 C23 C24 C231 -65.8(2) . . . . ?
C22 C23 C24 C231 177.37(17) . . . . ?
C33 N3 C32 C31 0.0(4) . . . . ?
C35 C31 C32 N3 -0.5(4) . . . . ?
C36 C31 C32 N3 178.3(3) . . . . ?
C32 N3 C33 C34 0.3(4) . . . . ?
N3 C33 C34 C35 -0.1(4) . . . . ?
C32 C31 C35 C34 0.6(4) . . . . ?
C36 C31 C35 C34 -178.1(3) . . . . ?
C33 C34 C35 C31 -0.4(4) . . . . ?
C43 N4 C42 C41 0.3(4) . . . . ?
C45 C41 C42 N4 -0.8(4) . . . . ?
C46 C41 C42 N4 177.9(3) . . . . ?
C42 N4 C43 C44 0.6(4) . . . . ?
N4 C43 C44 C45 -1.0(4) . . . . ?
C42 C41 C45 C44 0.3(4) . . . . ?
C46 C41 C45 C44 -178.3(3) . . . . ?
C43 C44 C45 C41 0.5(4) . . . . ?
O11 C11 C111 C116 156.51(18) . . . . ?
C121 C11 C111 C116 40.4(3) . . . . ?
C12 C11 C111 C116 -83.9(2) . . . . ?
O11 C11 C111 C112 -24.8(3) . . . . ?
C121 C11 C111 C112 -140.8(2) . . . . ?
C12 C11 C111 C112 94.8(2) . . . . ?
C116 C111 C112 C113 1.4(3) . . . . ?
C11 C111 C112 C113 -177.3(2) . . . . ?
C111 C112 C113 C114 -0.4(4) . . . . ?
C112 C113 C114 C115 -0.9(4) . . . . ?
C113 C114 C115 C116 1.3(4) . . . . ?
C114 C115 C116 C111 -0.2(3) . . . . ?
C112 C111 C116 C115 -1.1(3) . . . . ?
C11 C111 C116 C115 177.6(2) . . . . ?
O11 C11 C121 C126 134.4(2) . . . . ?
C111 C11 C121 C126 -107.5(2) . . . . ?
C12 C11 C121 C126 16.0(3) . . . . ?
O11 C11 C121 C122 -47.2(2) . . . . ?
C111 C11 C121 C122 70.9(2) . . . . ?
C12 C11 C121 C122 -165.58(18) . . . . ?
C126 C121 C122 C123 0.7(3) . . . . ?
C11 C121 C122 C123 -177.8(2) . . . . ?
C121 C122 C123 C124 0.1(4) . . . . ?
C122 C123 C124 C125 -0.8(4) . . . . ?
C123 C124 C125 C126 0.7(4) . . . . ?
C122 C121 C126 C125 -0.9(3) . . . . ?
C11 C121 C126 C125 177.5(2) . . . . ?
C124 C125 C126 C121 0.2(4) . . . . ?
O14 C14 C131 C136 120.6(2) . . . . ?
C141 C14 C131 C136 -121.9(2) . . . . ?
C13 C14 C131 C136 3.3(3) . . . . ?
O14 C14 C131 C132 -57.3(2) . . . . ?
C141 C14 C131 C132 60.2(2) . . . . ?
C13 C14 C131 C132 -174.61(18) . . . . ?
C136 C131 C132 C133 -0.5(3) . . . . ?
C14 C131 C132 C133 177.6(2) . . . . ?
C131 C132 C133 C134 0.0(4) . . . . ?
C132 C133 C134 C135 0.5(4) . . . . ?
C133 C134 C135 C136 -0.6(4) . . . . ?
C132 C131 C136 C135 0.4(3) . . . . ?
C14 C131 C136 C135 -177.4(2) . . . . ?
C134 C135 C136 C131 0.1(4) . . . . ?
O14 C14 C141 C142 -14.5(3) . . . . ?
C131 C14 C141 C142 -133.2(2) . . . . ?
C13 C14 C141 C142 101.7(2) . . . . ?
O14 C14 C141 C146 164.37(19) . . . . ?
C131 C14 C141 C146 45.6(3) . . . . ?
C13 C14 C141 C146 -79.4(2) . . . . ?
C146 C141 C142 C143 -1.6(3) . . . . ?
C14 C141 C142 C143 177.3(2) . . . . ?
C141 C142 C143 C144 0.2(4) . . . . ?
C142 C143 C144 C145 1.5(4) . . . . ?
C143 C144 C145 C146 -1.8(4) . . . . ?
C144 C145 C146 C141 0.4(4) . . . . ?
C142 C141 C146 C145 1.3(3) . . . . ?
C14 C141 C146 C145 -177.5(2) . . . . ?
C13 O13 C151 O12 24.2(2) . . . . ?
C13 O13 C151 C156 140.80(17) . . . . ?
C13 O13 C151 C152 -95.48(19) . . . . ?
C12 O12 C151 O13 -10.4(2) . . . . ?
C12 O12 C151 C156 -126.57(18) . . . . ?
C12 O12 C151 C152 109.43(18) . . . . ?
O13 C151 C152 C153 -68.9(2) . . . . ?
O12 C151 C152 C153 174.32(18) . . . . ?
C156 C151 C152 C153 52.4(2) . . . . ?
C151 C152 C153 C154 -54.0(3) . . . . ?
C152 C153 C154 C155 57.0(3) . . . . ?
C153 C154 C155 C156 -57.6(3) . . . . ?
O13 C151 C156 C155 69.4(2) . . . . ?
O12 C151 C156 C155 -176.06(18) . . . . ?
C152 C151 C156 C155 -53.2(2) . . . . ?
C154 C155 C156 C151 55.6(3) . . . . ?
O21 C21 C211 C212 119.9(2) . . . . ?
C221 C21 C211 C212 -122.0(2) . . . . ?
C22 C21 C211 C212 2.8(3) . . . . ?
O21 C21 C211 C216 -57.7(2) . . . . ?
C221 C21 C211 C216 60.3(2) . . . . ?
C22 C21 C211 C216 -174.85(19) . . . . ?
C216 C211 C212 C213 0.8(3) . . . . ?
C21 C211 C212 C213 -176.9(2) . . . . ?
C211 C212 C213 C214 0.0(4) . . . . ?
C212 C213 C214 C215 -0.6(4) . . . . ?
C213 C214 C215 C216 0.4(4) . . . . ?
C214 C215 C216 C211 0.4(4) . . . . ?
C212 C211 C216 C215 -0.9(3) . . . . ?
C21 C211 C216 C215 176.8(2) . . . . ?
O21 C21 C221 C226 -13.9(3) . . . . ?
C211 C21 C221 C226 -133.0(2) . . . . ?
C22 C21 C221 C226 102.6(2) . . . . ?
O21 C21 C221 C222 165.37(19) . . . . ?
C211 C21 C221 C222 46.3(3) . . . . ?
C22 C21 C221 C222 -78.1(2) . . . . ?
C226 C221 C222 C223 0.9(3) . . . . ?
C21 C221 C222 C223 -178.4(2) . . . . ?
C221 C222 C223 C224 0.8(4) . . . . ?
C222 C223 C224 C225 -1.7(4) . . . . ?
C223 C224 C225 C226 0.8(4) . . . . ?
C222 C221 C226 C225 -1.7(3) . . . . ?
C21 C221 C226 C225 177.6(2) . . . . ?
C224 C225 C226 C221 0.9(4) . . . . ?
O24 C24 C231 C232 126.0(2) . . . . ?
C241 C24 C231 C232 -115.9(2) . . . . ?
C23 C24 C231 C232 7.4(3) . . . . ?
O24 C24 C231 C236 -54.5(2) . . . . ?
C241 C24 C231 C236 63.6(2) . . . . ?
C23 C24 C231 C236 -173.11(18) . . . . ?
C236 C231 C232 C233 -0.9(3) . . . . ?
C24 C231 C232 C233 178.5(2) . . . . ?
C231 C232 C233 C234 0.4(4) . . . . ?
C232 C233 C234 C235 0.5(4) . . . . ?
C233 C234 C235 C236 -0.7(4) . . . . ?
C234 C235 C236 C231 0.2(4) . . . . ?
C232 C231 C236 C235 0.7(3) . . . . ?
C24 C231 C236 C235 -178.9(2) . . . . ?
O24 C24 C241 C242 -22.7(3) . . . . ?
C231 C24 C241 C242 -138.2(2) . . . . ?
C23 C24 C241 C242 97.4(2) . . . . ?
O24 C24 C241 C246 158.45(18) . . . . ?
C231 C24 C241 C246 42.9(2) . . . . ?
C23 C24 C241 C246 -81.5(2) . . . . ?
C246 C241 C242 C243 1.5(3) . . . . ?
C24 C241 C242 C243 -177.4(2) . . . . ?
C241 C242 C243 C244 -0.6(4) . . . . ?
C242 C243 C244 C245 -0.3(4) . . . . ?
C243 C244 C245 C246 0.3(4) . . . . ?
C244 C245 C246 C241 0.6(3) . . . . ?
C242 C241 C246 C245 -1.5(3) . . . . ?
C24 C241 C246 C245 177.4(2) . . . . ?
C22 O22 C251 O23 27.8(2) . . . . ?
C22 O22 C251 C256 143.81(18) . . . . ?
C22 O22 C251 C252 -92.39(19) . . . . ?
C23 O23 C251 O22 -12.0(2) . . . . ?
C23 O23 C251 C256 -128.19(18) . . . . ?
C23 O23 C251 C252 107.43(19) . . . . ?
O22 C251 C252 C253 -69.3(2) . . . . ?
O23 C251 C252 C253 174.26(18) . . . . ?
C256 C251 C252 C253 52.2(3) . . . . ?
C251 C252 C253 C254 -55.5(3) . . . . ?
C252 C253 C254 C255 58.3(3) . . . . ?
C253 C254 C255 C256 -57.4(3) . . . . ?
O22 C251 C256 C255 70.7(2) . . . . ?
O23 C251 C256 C255 -175.38(19) . . . . ?
C252 C251 C256 C255 -51.7(3) . . . . ?
C254 C255 C256 C251 54.1(3) . . . . ?
