##############################################################################
#                                                                            #
# 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 Acta Crystallographica Section E, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# 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.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_audit_creation_method     SHELXL-97
_journal_date_recd_electronic     2013-08-27
_journal_date_accepted     2014-02-18
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2014
_journal_volume     70
_journal_issue      4
_journal_page_first     o419
_journal_page_last     o420
_journal_paper_category     QO
_journal_paper_doi     10.1107/S1600536814003638
_journal_coeditor_code     FY2104
_publ_contact_author_name     'Xiao Zheng'
_publ_contact_author_address
;
The Key Laboratory for Chemical Biology of Fujian Province,
College of Chemistry and Chemical Engineering,
Xiamen University,
Xiamen, Fujian 361005, People's Republic of China
;
_publ_contact_author_email     'zxiao@xmu.edu.cn'
_publ_contact_author_fax     '86-592-2186400'
_publ_contact_author_phone     '86-592-2180992'
_publ_section_title
;\
(4S,5R)-4-Benzyloxy-5-[4-(cyclohexanecarbonyl)phenyl]-1-(4-\
methoxybenzyl)pyrrolidin-2-one
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Gao, Yan-Jiao' .
;
The Key Laboratory for Chemical Biology of Fujian Province,
College of Chemistry and Chemical Engineering,
Xiamen University,
Xiamen, Fujian 361005, People's Republic of China
;
    'Ma, Jie' .
;
The Key Laboratory for Chemical Biology of Fujian Province,
College of Chemistry and Chemical Engineering,
Xiamen University,
Xiamen, Fujian 361005, People's Republic of China
;
    'Zheng, Xiao' .
;
The Key Laboratory for Chemical Biology of Fujian Province,
College of Chemistry and Chemical Engineering,
Xiamen University,
Xiamen, Fujian 361005, People's Republic of China
;
_database_code_depnum_ccdc_archive     'CCDC 987472'
_chemical_name_systematic
;\
(4S,5R)-4-Benzyloxy-5-[4-(cyclohexanecarbonyl)phenyl]-\
1-(4-methoxybenzyl)pyrrolidin-2-one
;
_chemical_name_common     ?
_chemical_formula_moiety     'C32 H35 N O4'
_chemical_formula_sum     'C32 H35 N O4'
_chemical_formula_iupac     'C32 H35 N O4'
_chemical_formula_weight     497.61
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y+1/2, -z'
_cell_length_a     9.4964(4)
_cell_length_b     28.6497(13)
_cell_length_c     9.9511(4)
_cell_angle_alpha     90.00
_cell_angle_beta     96.727(4)
_cell_angle_gamma     90.00
_cell_volume     2688.8(2)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min     ?
_cell_measurement_theta_max     ?
_cell_measurement_temperature     100.01(10)
_exptl_crystal_description     columnar
_exptl_crystal_colour     colorless
_exptl_crystal_size_max     0.2
_exptl_crystal_size_mid     0.12
_exptl_crystal_size_min     0.09
_exptl_crystal_density_diffrn     1.229
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1064
_exptl_absorpt_coefficient_mu     0.080
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2006)
;
_exptl_absorpt_correction_T_min     0.92705
_exptl_absorpt_correction_T_max     1.00000
_diffrn_ambient_temperature     100.01(10)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Oxford Diffraction SuperNova'
_diffrn_measurement_method     'ω scans'
_diffrn_detector_area_resol_mean     10.3415
_diffrn_reflns_number     11184
_diffrn_reflns_av_R_equivalents     0.0369
_diffrn_reflns_av_sigmaI/netI     0.0623
_diffrn_reflns_theta_min     3.46
_diffrn_reflns_theta_max     24.99
_diffrn_reflns_theta_full     24.99
_diffrn_measured_fraction_theta_max     0.960
_diffrn_measured_fraction_theta_full     0.960
_diffrn_reflns_limit_h_min     -11
_diffrn_reflns_limit_h_max     9
_diffrn_reflns_limit_k_min     -34
_diffrn_reflns_limit_k_max     28
_diffrn_reflns_limit_l_min     -11
_diffrn_reflns_limit_l_max     11
_diffrn_standards_number     11739
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_refine_special_details
;
Refinement of F² against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F², conventional
R-factors R are based on F, with F set to zero for
negative F². The threshold expression of F² >
σ(F²) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F² 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     7540
_reflns_number_gt     6140
_reflns_threshold_expression     I>2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0665
_refine_ls_R_factor_gt     0.0481
_refine_ls_wR_factor_gt     0.1096
_refine_ls_wR_factor_ref     0.1225
_refine_ls_goodness_of_fit_ref     1.025
_refine_ls_restrained_S_all     1.025
_refine_ls_number_reflns     7540
_refine_ls_number_parameters     669
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0590P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.212
_refine_diff_density_min     -0.181
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
_computing_data_collection     'CrysAlis PRO (Oxford Diffraction, 2006)'
_computing_cell_refinement     'CrysAlis PRO (Oxford Diffraction, 2006)'
_computing_data_reduction     'CrysAlis PRO (Oxford Diffraction, 2006)'
_computing_structure_solution     'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material     'SHELXTL (Sheldrick, 2008)'
_iucr_refine_instruction_details
;
TITL CF solution in P21
CELL 0.71073 9.496402 28.649702 9.951134 90 96.7272 90
ZERR 2 0.000426 0.001306 0.000412 0 0.0041 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O
UNIT 128 140 4 16
L.S. 8
PLAN  5
acta
FMAP 2
bond $h
htab
eqiv $1_-x+1,y-0.5,-z+1
eqiv $2_x-1,y,z
htab c62 o4_$1
htab c17 o2_$2
htab c49 o6_$2
OMIT -3 50
REM <HKL>G:\DATA\CCD\tmp\tmp\z0603.hkl</HKL>
WGHT    0.056506
FVAR       1.81525
C1    1    0.273354    0.204835    0.136173    11.00000    0.06374    0.03083 =
         0.03810   -0.00524    0.00695   -0.01124
AFIX 137
H1A   2    0.323627    0.220073    0.070295    11.00000   -1.50000
H1B   2    0.174892    0.213223    0.121189    11.00000   -1.50000
H1C   2    0.282746    0.171628    0.127880    11.00000   -1.50000
AFIX   0
C2    1    0.342958    0.265983    0.292260    11.00000    0.02773    0.02337 =
         0.03126    0.00127    0.01090   -0.00092
C3    1    0.296457    0.300554    0.198486    11.00000    0.03068    0.03217 =
         0.02235   -0.00083    0.00430   -0.00398
AFIX  43
H3    2    0.251433    0.292469    0.113631    11.00000   -1.20000
AFIX   0
C4    1    0.318263    0.347217    0.233474    11.00000    0.02443    0.02780 =
         0.02375    0.00224    0.00489   -0.00208
AFIX  43
H4    2    0.287110    0.370127    0.170732    11.00000   -1.20000
AFIX   0
C5    1    0.384807    0.360639    0.358615    11.00000    0.01993    0.02577 =
         0.01664   -0.00253    0.00619    0.00037
C6    1    0.427206    0.325174    0.452367    11.00000    0.02817    0.03229 =
         0.01862    0.00032    0.00320    0.00016
AFIX  43
H6    2    0.470963    0.333132    0.537816    11.00000   -1.20000
AFIX   0
C7    1    0.405000    0.278913    0.419716    11.00000    0.03314    0.03057 =
         0.02524    0.00819    0.00630    0.00237
AFIX  43
H7    2    0.431948    0.256047    0.483950    11.00000   -1.20000
AFIX   0
C8    1    0.412857    0.411495    0.390171    11.00000    0.02133    0.03037 =
         0.01438   -0.00072    0.00321   -0.00063
AFIX  23
H8A   2    0.499962    0.420755    0.355457    11.00000   -1.20000
H8B   2    0.336297    0.430048    0.344415    11.00000   -1.20000
AFIX   0
C9    1    0.549167    0.431434    0.609137    11.00000    0.02200    0.02519 =
         0.02781   -0.00309    0.00166   -0.00392
C10   1    0.521336    0.434341    0.755636    11.00000    0.02939    0.04813 =
         0.02338   -0.00533    0.00144   -0.00612
AFIX  23
H10A  2    0.515576    0.466602    0.784060    11.00000   -1.20000
H10B  2    0.595876    0.418834    0.814147    11.00000   -1.20000
AFIX   0
C11   1    0.380701    0.409771    0.759579    11.00000    0.02600    0.04033 =
         0.01953   -0.00406    0.00624   -0.00360
AFIX  13
H11   2    0.326170    0.423229    0.827824    11.00000   -1.20000
AFIX   0
C12   1    0.304980    0.416626    0.613254    11.00000    0.02047    0.03216 =
         0.02450   -0.00412    0.00755   -0.00376
AFIX  13
H12   2    0.252095    0.388213    0.585102    11.00000   -1.20000
AFIX   0
C13   1    0.205887    0.457717    0.597632    11.00000    0.02325    0.03182 =
         0.02007   -0.00983    0.00444   -0.00459
C14   1    0.254652    0.502459    0.580697    11.00000    0.02089    0.03462 =
         0.07736   -0.01098    0.01556   -0.00729
AFIX  43
H14   2    0.351164    0.507458    0.578805    11.00000   -1.20000
AFIX   0
C15   1    0.162945    0.539837    0.566548    11.00000    0.03269    0.02407 =
         0.09058   -0.00916    0.01864   -0.00792
AFIX  43
H15   2    0.198303    0.569730    0.556206    11.00000   -1.20000
AFIX   0
C16   1    0.018284    0.533324    0.567573    11.00000    0.03030    0.02687 =
         0.03655   -0.00946    0.00770   -0.00405
C17   1   -0.031510    0.488849    0.586969    11.00000    0.01942    0.03245 =
         0.01950   -0.00282    0.00298   -0.00284
AFIX  43
H17   2   -0.127823    0.484004    0.590612    11.00000   -1.20000
AFIX   0
C18   1    0.061139    0.451488    0.600997    11.00000    0.02468    0.03051 =
         0.01597    0.00185    0.00351   -0.00658
AFIX  43
H18   2    0.026036    0.421656    0.612898    11.00000   -1.20000
AFIX   0
C19   1   -0.076673    0.574991    0.544904    11.00000    0.03811    0.02469 =
         0.04811   -0.00833    0.00649   -0.00580
C20   1   -0.234388    0.570333    0.540519    11.00000    0.02845    0.02509 =
         0.03859   -0.00508    0.00175    0.00054
AFIX  13
H20   2   -0.253755    0.543860    0.597960    11.00000   -1.20000
AFIX   0
C21   1   -0.304627    0.612758    0.591693    11.00000    0.04459    0.05518 =
         0.06925   -0.03494    0.00161    0.00237
AFIX  23
H21A  2   -0.279648    0.639913    0.541297    11.00000   -1.20000
H21B  2   -0.269313    0.617657    0.686099    11.00000   -1.20000
AFIX   0
C22   1   -0.466070    0.608046    0.578026    11.00000    0.04314    0.04398 =
         0.04576   -0.01442    0.01136    0.00447
AFIX  23
H22A  2   -0.492255    0.583460    0.637353    11.00000   -1.20000
H22B  2   -0.507607    0.637010    0.604978    11.00000   -1.20000
AFIX   0
C23   1   -0.522382    0.596801    0.434263    11.00000    0.03654    0.06035 =
         0.03410    0.00761    0.00328    0.01390
AFIX  23
H23A  2   -0.503609    0.622748    0.376324    11.00000   -1.20000
H23B  2   -0.624268    0.592493    0.427744    11.00000   -1.20000
AFIX   0
C24   1   -0.453913    0.552657    0.385678    11.00000    0.04699    0.10026 =
         0.03804   -0.02591   -0.00538    0.01662
AFIX  23
H24A  2   -0.490444    0.546518    0.292204    11.00000   -1.20000
H24B  2   -0.477399    0.526245    0.439832    11.00000   -1.20000
AFIX   0
C25   1   -0.291857    0.558595    0.397631    11.00000    0.04361    0.06891 =
         0.03345   -0.00898    0.00194    0.01873
AFIX  23
H25A  2   -0.248792    0.529921    0.370494    11.00000   -1.20000
H25B  2   -0.268150    0.583317    0.337584    11.00000   -1.20000
AFIX   0
C26   1    0.292265    0.334714    0.813942    11.00000    0.03335    0.05251 =
         0.03707    0.01200    0.01482   -0.00195
AFIX  23
H26A  2    0.211792    0.340934    0.746943    11.00000   -1.20000
H26B  2    0.266401    0.343257    0.902132    11.00000   -1.20000
AFIX   0
C27   1    0.329505    0.283462    0.812470    11.00000    0.03799    0.04661 =
         0.02624    0.00905    0.01612    0.00248
C28   1    0.463881    0.268162    0.865115    11.00000    0.03329    0.04477 =
         0.05391    0.00825    0.01843    0.00504
AFIX  43
H28   2    0.532602    0.289549    0.899275    11.00000   -1.20000
AFIX   0
C29   1    0.494677    0.220741    0.866298    11.00000    0.04985    0.06965 =
         0.05872    0.00709    0.02725    0.01273
AFIX  43
H29   2    0.584444    0.210387    0.900986    11.00000   -1.20000
AFIX   0
C30   1    0.392368    0.188864    0.816094    11.00000    0.07065    0.04933 =
         0.05443   -0.00569    0.03192    0.00601
AFIX  43
H30   2    0.412880    0.157113    0.818679    11.00000   -1.20000
AFIX   0
C31   1    0.261162    0.204011    0.762699    11.00000    0.06388    0.05536 =
         0.04121   -0.00563    0.01988   -0.01469
AFIX  43
H31   2    0.192936    0.182628    0.727442    11.00000   -1.20000
AFIX   0
C32   1    0.229938    0.251231    0.761159    11.00000    0.04584    0.05430 =
         0.03279    0.00334    0.01328    0.00035
AFIX  43
H32   2    0.140383    0.261315    0.724925    11.00000   -1.20000
AFIX   0
C33   1    0.790117    0.203955   -0.334430    11.00000    0.07654    0.03562 =
         0.03865   -0.00419    0.01313   -0.00636
AFIX 137
H33A  2    0.851428    0.215425   -0.397147    11.00000   -1.50000
H33B  2    0.695409    0.215039   -0.360247    11.00000   -1.50000
H33C  2    0.790551    0.170449   -0.335234    11.00000   -1.50000
AFIX   0
C34   1    0.854781    0.267524   -0.182245    11.00000    0.03201    0.02666 =
         0.03180   -0.00176    0.01487    0.00350
C35   1    0.818342    0.300531   -0.283228    11.00000    0.03318    0.03587 =
         0.02064   -0.00338    0.00755   -0.00362
AFIX  43
H35   2    0.780264    0.291157   -0.369360    11.00000   -1.20000
AFIX   0
C36   1    0.839491    0.347515   -0.253862    11.00000    0.02625    0.03593 =
         0.01777    0.00594    0.00671    0.00481
AFIX  43
H36   2    0.812826    0.369475   -0.320861    11.00000   -1.20000
AFIX   0
C37   1    0.899347    0.362768   -0.127295    11.00000    0.02104    0.03113 =
         0.01941    0.00178    0.00794    0.00186
C38   1    0.933528    0.329012   -0.027408    11.00000    0.02720    0.03716 =
         0.01895   -0.00007    0.00530    0.00476
AFIX  43
H38   2    0.972508    0.338313    0.058511    11.00000   -1.20000
AFIX   0
C39   1    0.910588    0.282113   -0.053709    11.00000    0.03608    0.03704 =
         0.02506    0.00500    0.00501    0.00730
AFIX  43
H39   2    0.932506    0.260265    0.014665    11.00000   -1.20000
AFIX   0
C40   1    0.930125    0.414047   -0.102978    11.00000    0.02373    0.03263 =
         0.01634    0.00373    0.00637    0.00262
AFIX  23
H40A  2    1.023234    0.421069   -0.128711    11.00000   -1.20000
H40B  2    0.861257    0.432278   -0.160544    11.00000   -1.20000
AFIX   0
C41   1    1.040942    0.443369    0.117876    11.00000    0.02326    0.02188 =
         0.02414    0.01011   -0.00023   -0.00011
C42   1    0.995276    0.453154    0.255517    11.00000    0.02715    0.02951 =
         0.02128    0.00061    0.00110   -0.00338
AFIX  23
H42A  2    0.980717    0.486313    0.267933    11.00000   -1.20000
H42B  2    1.065510    0.442013    0.326946    11.00000   -1.20000
AFIX   0
C43   1    0.857065    0.426477    0.254821    11.00000    0.02992    0.02123 =
         0.01728    0.00117    0.00515    0.00282
AFIX  13
H43   2    0.792233    0.440993    0.312202    11.00000   -1.20000
AFIX   0
C44   1    0.796765    0.426120    0.102575    11.00000    0.01887    0.01983 =
         0.02116    0.00177    0.00720   -0.00117
AFIX  13
H44   2    0.748565    0.396355    0.080810    11.00000   -1.20000
AFIX   0
C45   1    0.694656    0.465915    0.064068    11.00000    0.01962    0.02591 =
         0.01515   -0.00554    0.00376   -0.00312
C46   1    0.738746    0.507956    0.010671    11.00000    0.01933    0.02790 =
         0.03152    0.00100    0.00031   -0.00346
AFIX  43
H46   2    0.833442    0.512036   -0.002023    11.00000   -1.20000
AFIX   0
C47   1    0.642802    0.543329   -0.023200    11.00000    0.02959    0.02718 =
         0.02747    0.00190    0.00415   -0.00594
AFIX  43
H47   2    0.673798    0.570966   -0.058976    11.00000   -1.20000
AFIX   0
C48   1    0.501323    0.538558   -0.005063    11.00000    0.02393    0.02065 =
         0.02336   -0.00029    0.00239   -0.00073
C49   1    0.456085    0.496671    0.048237    11.00000    0.02067    0.02717 =
         0.01725   -0.00283    0.00396   -0.00046
AFIX  43
H49   2    0.361389    0.492721    0.061109    11.00000   -1.20000
AFIX   0
C50   1    0.552973    0.461014    0.081863    11.00000    0.02298    0.02719 =
         0.01560   -0.00128    0.00518   -0.00457
AFIX  43
H50   2    0.522023    0.433272    0.117061    11.00000   -1.20000
AFIX   0
C51   1    0.402845    0.578886   -0.043184    11.00000    0.03420    0.02365 =
         0.02685   -0.00206    0.00551   -0.00289
C52   1    0.247588    0.575084   -0.023059    11.00000    0.02431    0.01781 =
         0.03253    0.00083    0.00190    0.00107
AFIX  13
H52   2    0.214816    0.543377   -0.046736    11.00000   -1.20000
AFIX   0
C53   1    0.157222    0.609768   -0.112629    11.00000    0.03320    0.03230 =
         0.03137    0.00382    0.00190    0.00238
AFIX  23
H53A  2    0.191326    0.641200   -0.092448    11.00000   -1.20000
H53B  2    0.166693    0.603377   -0.206872    11.00000   -1.20000
AFIX   0
C54   1    0.001514    0.606580   -0.090234    11.00000    0.03216    0.02681 =
         0.04443   -0.00087   -0.00433    0.00414
AFIX  23
H54A  2   -0.052788    0.629300   -0.147044    11.00000   -1.20000
H54B  2   -0.034428    0.575771   -0.116018    11.00000   -1.20000
AFIX   0
C55   1   -0.017131    0.615598    0.056397    11.00000    0.02862    0.02351 =
         0.05062   -0.00419    0.00795   -0.00022
AFIX  23
H55A  2   -0.116023    0.611488    0.069372    11.00000   -1.20000
H55B  2    0.009083    0.647594    0.079296    11.00000   -1.20000
AFIX   0
C56   1    0.073522    0.582687    0.149491    11.00000    0.03203    0.03679 =
         0.03462   -0.00519    0.00993    0.00161
AFIX  23
H56A  2    0.038126    0.551097    0.135316    11.00000   -1.20000
H56B  2    0.065831    0.591101    0.242767    11.00000   -1.20000
AFIX   0
C57   1    0.228999    0.584212    0.124951    11.00000    0.02852    0.03563 =
         0.02735    0.00072    0.00065    0.00030
AFIX  23
H57A  2    0.281468    0.560937    0.181200    11.00000   -1.20000
H57B  2    0.268042    0.614603    0.151152    11.00000   -1.20000
AFIX   0
C58   1    0.780620    0.351973    0.326521    11.00000    0.02988    0.02906 =
         0.02532    0.00352    0.00998    0.00043
AFIX  23
H58A  2    0.699559    0.357381    0.259518    11.00000   -1.20000
H58B  2    0.753992    0.360065    0.414770    11.00000   -1.20000
AFIX   0
C59   1    0.823312    0.301824    0.324778    11.00000    0.02863    0.03034 =
         0.01953    0.00444    0.01081    0.00014
C60   1    0.960231    0.287586    0.373741    11.00000    0.03479    0.02766 =
         0.02861   -0.00029    0.01039    0.00087
AFIX  43
H60   2    1.027435    0.309634    0.406719    11.00000   -1.20000
AFIX   0
C61   1    0.996407    0.240960    0.373472    11.00000    0.03242    0.03974 =
         0.03611    0.00430    0.01030    0.00637
AFIX  43
H61   2    1.088214    0.231872    0.405623    11.00000   -1.20000
AFIX   0
C62   1    0.897877    0.207610    0.326013    11.00000    0.04965    0.03030 =
         0.03695   -0.00380    0.01251    0.00636
AFIX  43
H62   2    0.922825    0.176208    0.327486    11.00000   -1.20000
AFIX   0
C63   1    0.762063    0.221150    0.276342    11.00000    0.04127    0.03377 =
         0.04063   -0.00351    0.01160   -0.00486
AFIX  43
H63   2    0.695200    0.198891    0.244131    11.00000   -1.20000
AFIX   0
C64   1    0.726101    0.267680    0.274705    11.00000    0.03010    0.03816 =
         0.03080   -0.00167    0.00959   -0.00144
AFIX  43
H64   2    0.635036    0.276589    0.239471    11.00000   -1.20000
AFIX   0
O1    4    0.330925    0.219052    0.268473    11.00000    0.04734    0.02217 =
         0.03433   -0.00259    0.00949   -0.00185
O2    4    0.662680    0.437706    0.564668    11.00000    0.02321    0.03404 =
         0.03273    0.00144    0.00623   -0.00756
O3    4    0.411558    0.361824    0.784530    11.00000    0.02918    0.04313 =
         0.02441    0.00933    0.00702   -0.00002
O4    4   -0.024191    0.613266    0.521210    11.00000    0.04079    0.02853 =
         0.11703   -0.00745    0.01199   -0.00597
O5    4    0.839294    0.220296   -0.201152    11.00000    0.05185    0.03265 =
         0.03400   -0.00205    0.01105    0.00441
O6    4    1.159558    0.448629    0.083447    11.00000    0.02263    0.03909 =
         0.03680    0.01105    0.00688   -0.00475
O7    4    0.897099    0.380196    0.297157    11.00000    0.02502    0.02789 =
         0.02538    0.00665    0.00674   -0.00067
N1    3    0.425005    0.421193    0.534731    11.00000    0.01672    0.03229 =
         0.01616   -0.00390    0.00521   -0.00662
N2    3    0.925811    0.428048    0.037047    11.00000    0.01840    0.03181 =
         0.01629    0.00124    0.00490   -0.00166
O8    4    0.450033    0.614646   -0.086919    11.00000    0.03699    0.02430 =
         0.06453    0.01032    0.01474    0.00002
HKLF 4
REM  CF solution in P21
REM R1 =  0.0481 for   6140 Fo > 4sig(Fo)  and  0.0665 for all   7540 data
REM    669 parameters refined using      1 restraints
END
WGHT      0.0552      0.0000
REM Highest difference peak  0.212,  deepest hole -0.181,  1-sigma level  0.043
Q1    1  -0.0849  0.5971  0.4300  11.00000  0.05    0.21
Q2    1  -0.4183  0.5789  0.6582  11.00000  0.05    0.18
Q3    1  -0.4474  0.5667  0.6464  11.00000  0.05    0.16
Q4    1  -0.2650  0.6198  0.3949  11.00000  0.05    0.16
Q5    1   0.7304  0.4888  0.0793  11.00000  0.05    0.16
;
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_symmetry_multiplicity
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    C C1 0.2734(5) 0.20483(14) 0.1362(4) 0.0441(10) Uani d . 1 1 . .
    H H1A 0.3236 0.2201 0.0703 0.066 Uiso calc R 1 1 . .
    H H1B 0.1749 0.2132 0.1212 0.066 Uiso calc R 1 1 . .
    H H1C 0.2827 0.1716 0.1279 0.066 Uiso calc R 1 1 . .
    C C2 0.3430(4) 0.26598(12) 0.2923(3) 0.0269(8) Uani d . 1 1 . .
    C C3 0.2965(4) 0.30055(12) 0.1985(3) 0.0283(8) Uani d . 1 1 . .
    H H3 0.2514 0.2925 0.1136 0.034 Uiso calc R 1 1 . .
    C C4 0.3183(3) 0.34722(12) 0.2335(3) 0.0252(8) Uani d . 1 1 . .
    H H4 0.2871 0.3701 0.1707 0.030 Uiso calc R 1 1 . .
    C C5 0.3848(3) 0.36064(11) 0.3586(3) 0.0205(7) Uani d . 1 1 . .
    C C6 0.4272(3) 0.32517(12) 0.4524(3) 0.0263(8) Uani d . 1 1 . .
    H H6 0.4710 0.3331 0.5378 0.032 Uiso calc R 1 1 . .
    C C7 0.4050(4) 0.27891(12) 0.4197(3) 0.0294(9) Uani d . 1 1 . .
    H H7 0.4319 0.2560 0.4840 0.035 Uiso calc R 1 1 . .
    C C8 0.4129(3) 0.41149(11) 0.3902(3) 0.0219(7) Uani d . 1 1 . .
    H H8A 0.5000 0.4208 0.3555 0.026 Uiso calc R 1 1 . .
    H H8B 0.3363 0.4300 0.3444 0.026 Uiso calc R 1 1 . .
    C C9 0.5492(3) 0.43143(11) 0.6091(3) 0.0251(8) Uani d . 1 1 . .
    C C10 0.5213(4) 0.43434(14) 0.7556(3) 0.0338(9) Uani d . 1 1 . .
    H H10A 0.5156 0.4666 0.7841 0.041 Uiso calc R 1 1 . .
    H H10B 0.5959 0.4188 0.8141 0.041 Uiso calc R 1 1 . .
    C C11 0.3807(4) 0.40977(13) 0.7596(3) 0.0283(8) Uani d . 1 1 . .
    H H11 0.3262 0.4232 0.8278 0.034 Uiso calc R 1 1 . .
    C C12 0.3050(3) 0.41663(12) 0.6133(3) 0.0253(8) Uani d . 1 1 . .
    H H12 0.2521 0.3882 0.5851 0.030 Uiso calc R 1 1 . .
    C C13 0.2059(3) 0.45772(12) 0.5976(3) 0.0249(8) Uani d . 1 1 . .
    C C14 0.2547(4) 0.50246(13) 0.5807(4) 0.0435(10) Uani d . 1 1 . .
    H H14 0.3512 0.5075 0.5788 0.052 Uiso calc R 1 1 . .
    C C15 0.1629(4) 0.53984(13) 0.5665(5) 0.0482(11) Uani d . 1 1 . .
    H H15 0.1983 0.5697 0.5562 0.058 Uiso calc R 1 1 . .
    C C16 0.0183(4) 0.53332(12) 0.5676(3) 0.0309(8) Uani d . 1 1 . .
    C C17 -0.0315(3) 0.48885(12) 0.5870(3) 0.0237(8) Uani d . 1 1 . .
    H H17 -0.1278 0.4840 0.5906 0.028 Uiso calc R 1 1 . .
    C C18 0.0611(3) 0.45149(12) 0.6010(3) 0.0236(8) Uani d . 1 1 . .
    H H18 0.0260 0.4217 0.6129 0.028 Uiso calc R 1 1 . .
    C C19 -0.0767(4) 0.57499(13) 0.5449(4) 0.0369(9) Uani d . 1 1 . .
    C C20 -0.2344(3) 0.57033(12) 0.5405(3) 0.0309(8) Uani d . 1 1 . .
    H H20 -0.2538 0.5439 0.5980 0.037 Uiso calc R 1 1 . .
    C C21 -0.3046(4) 0.61276(17) 0.5917(5) 0.0567(12) Uani d . 1 1 . .
    H H21A -0.2796 0.6399 0.5413 0.068 Uiso calc R 1 1 . .
    H H21B -0.2693 0.6177 0.6861 0.068 Uiso calc R 1 1 . .
    C C22 -0.4661(4) 0.60805(15) 0.5780(4) 0.0438(10) Uani d . 1 1 . .
    H H22A -0.4923 0.5835 0.6374 0.053 Uiso calc R 1 1 . .
    H H22B -0.5076 0.6370 0.6050 0.053 Uiso calc R 1 1 . .
    C C23 -0.5224(4) 0.59680(15) 0.4343(4) 0.0437(10) Uani d . 1 1 . .
    H H23A -0.5036 0.6227 0.3763 0.052 Uiso calc R 1 1 . .
    H H23B -0.6243 0.5925 0.4277 0.052 Uiso calc R 1 1 . .
    C C24 -0.4539(4) 0.55266(19) 0.3857(4) 0.0626(14) Uani d . 1 1 . .
    H H24A -0.4904 0.5465 0.2922 0.075 Uiso calc R 1 1 . .
    H H24B -0.4774 0.5262 0.4398 0.075 Uiso calc R 1 1 . .
    C C25 -0.2919(4) 0.55860(17) 0.3976(4) 0.0489(11) Uani d . 1 1 . .
    H H25A -0.2488 0.5299 0.3705 0.059 Uiso calc R 1 1 . .
    H H25B -0.2682 0.5833 0.3376 0.059 Uiso calc R 1 1 . .
    C C26 0.2923(4) 0.33471(14) 0.8139(4) 0.0401(10) Uani d . 1 1 . .
    H H26A 0.2118 0.3409 0.7469 0.048 Uiso calc R 1 1 . .
    H H26B 0.2664 0.3433 0.9021 0.048 Uiso calc R 1 1 . .
    C C27 0.3295(4) 0.28346(14) 0.8125(3) 0.0360(9) Uani d . 1 1 . .
    C C28 0.4639(4) 0.26816(15) 0.8651(4) 0.0429(10) Uani d . 1 1 . .
    H H28 0.5326 0.2895 0.8993 0.052 Uiso calc R 1 1 . .
    C C29 0.4947(5) 0.22074(18) 0.8663(4) 0.0578(12) Uani d . 1 1 . .
    H H29 0.5844 0.2104 0.9010 0.069 Uiso calc R 1 1 . .
    C C30 0.3924(5) 0.18886(17) 0.8161(4) 0.0562(12) Uani d . 1 1 . .
    H H30 0.4129 0.1571 0.8187 0.067 Uiso calc R 1 1 . .
    C C31 0.2612(5) 0.20401(17) 0.7627(4) 0.0524(12) Uani d . 1 1 . .
    H H31 0.1929 0.1826 0.7274 0.063 Uiso calc R 1 1 . .
    C C32 0.2299(5) 0.25123(15) 0.7612(4) 0.0436(10) Uani d . 1 1 . .
    H H32 0.1404 0.2613 0.7249 0.052 Uiso calc R 1 1 . .
    C C33 0.7901(5) 0.20396(14) -0.3344(4) 0.0498(11) Uani d . 1 1 . .
    H H33A 0.8514 0.2154 -0.3971 0.075 Uiso calc R 1 1 . .
    H H33B 0.6954 0.2150 -0.3602 0.075 Uiso calc R 1 1 . .
    H H33C 0.7906 0.1704 -0.3352 0.075 Uiso calc R 1 1 . .
    C C34 0.8548(4) 0.26752(13) -0.1822(3) 0.0293(8) Uani d . 1 1 . .
    C C35 0.8183(4) 0.30053(13) -0.2832(3) 0.0295(8) Uani d . 1 1 . .
    H H35 0.7803 0.2912 -0.3694 0.035 Uiso calc R 1 1 . .
    C C36 0.8395(3) 0.34752(12) -0.2539(3) 0.0263(8) Uani d . 1 1 . .
    H H36 0.8128 0.3695 -0.3209 0.032 Uiso calc R 1 1 . .
    C C37 0.8993(3) 0.36277(12) -0.1273(3) 0.0234(8) Uani d . 1 1 . .
    C C38 0.9335(3) 0.32901(13) -0.0274(3) 0.0276(8) Uani d . 1 1 . .
    H H38 0.9725 0.3383 0.0585 0.033 Uiso calc R 1 1 . .
    C C39 0.9106(4) 0.28211(13) -0.0537(3) 0.0326(9) Uani d . 1 1 . .
    H H39 0.9325 0.2603 0.0147 0.039 Uiso calc R 1 1 . .
    C C40 0.9301(3) 0.41405(12) -0.1030(3) 0.0239(8) Uani d . 1 1 . .
    H H40A 1.0232 0.4211 -0.1287 0.029 Uiso calc R 1 1 . .
    H H40B 0.8613 0.4323 -0.1605 0.029 Uiso calc R 1 1 . .
    C C41 1.0409(3) 0.44337(11) 0.1179(3) 0.0233(8) Uani d . 1 1 . .
    C C42 0.9953(3) 0.45315(12) 0.2555(3) 0.0261(8) Uani d . 1 1 . .
    H H42A 0.9807 0.4863 0.2679 0.031 Uiso calc R 1 1 . .
    H H42B 1.0655 0.4420 0.3269 0.031 Uiso calc R 1 1 . .
    C C43 0.8571(3) 0.42648(11) 0.2548(3) 0.0226(7) Uani d . 1 1 . .
    H H43 0.7922 0.4410 0.3122 0.027 Uiso calc R 1 1 . .
    C C44 0.7968(3) 0.42612(11) 0.1026(3) 0.0196(7) Uani d . 1 1 . .
    H H44 0.7486 0.3964 0.0808 0.023 Uiso calc R 1 1 . .
    C C45 0.6947(3) 0.46591(11) 0.0641(3) 0.0201(7) Uani d . 1 1 . .
    C C46 0.7387(3) 0.50796(12) 0.0107(3) 0.0265(8) Uani d . 1 1 . .
    H H46 0.8334 0.5120 -0.0020 0.032 Uiso calc R 1 1 . .
    C C47 0.6428(3) 0.54333(12) -0.0232(3) 0.0280(8) Uani d . 1 1 . .
    H H47 0.6738 0.5710 -0.0590 0.034 Uiso calc R 1 1 . .
    C C48 0.5013(3) 0.53856(11) -0.0051(3) 0.0227(7) Uani d . 1 1 . .
    C C49 0.4561(3) 0.49667(11) 0.0482(3) 0.0216(7) Uani d . 1 1 . .
    H H49 0.3614 0.4927 0.0611 0.026 Uiso calc R 1 1 . .
    C C50 0.5530(3) 0.46101(12) 0.0819(3) 0.0217(7) Uani d . 1 1 . .
    H H50 0.5220 0.4333 0.1171 0.026 Uiso calc R 1 1 . .
    C C51 0.4028(4) 0.57889(12) -0.0432(3) 0.0281(8) Uani d . 1 1 . .
    C C52 0.2476(3) 0.57508(12) -0.0231(3) 0.0250(8) Uani d . 1 1 . .
    H H52 0.2148 0.5434 -0.0467 0.030 Uiso calc R 1 1 . .
    C C53 0.1572(3) 0.60977(13) -0.1126(3) 0.0324(8) Uani d . 1 1 . .
    H H53A 0.1913 0.6412 -0.0924 0.039 Uiso calc R 1 1 . .
    H H53B 0.1667 0.6034 -0.2069 0.039 Uiso calc R 1 1 . .
    C C54 0.0015(4) 0.60658(13) -0.0902(3) 0.0352(9) Uani d . 1 1 . .
    H H54A -0.0528 0.6293 -0.1470 0.042 Uiso calc R 1 1 . .
    H H54B -0.0344 0.5758 -0.1160 0.042 Uiso calc R 1 1 . .
    C C55 -0.0171(4) 0.61560(13) 0.0564(4) 0.0340(8) Uani d . 1 1 . .
    H H55A -0.1160 0.6115 0.0694 0.041 Uiso calc R 1 1 . .
    H H55B 0.0091 0.6476 0.0793 0.041 Uiso calc R 1 1 . .
    C C56 0.0735(4) 0.58269(13) 0.1495(3) 0.0340(9) Uani d . 1 1 . .
    H H56A 0.0381 0.5511 0.1353 0.041 Uiso calc R 1 1 . .
    H H56B 0.0658 0.5911 0.2428 0.041 Uiso calc R 1 1 . .
    C C57 0.2290(4) 0.58421(13) 0.1250(3) 0.0307(8) Uani d . 1 1 . .
    H H57A 0.2815 0.5609 0.1812 0.037 Uiso calc R 1 1 . .
    H H57B 0.2680 0.6146 0.1512 0.037 Uiso calc R 1 1 . .
    C C58 0.7806(4) 0.35197(12) 0.3265(3) 0.0276(8) Uani d . 1 1 . .
    H H58A 0.6996 0.3574 0.2595 0.033 Uiso calc R 1 1 . .
    H H58B 0.7540 0.3601 0.4148 0.033 Uiso calc R 1 1 . .
    C C59 0.8233(3) 0.30182(12) 0.3248(3) 0.0255(8) Uani d . 1 1 . .
    C C60 0.9602(4) 0.28759(13) 0.3737(3) 0.0298(8) Uani d . 1 1 . .
    H H60 1.0274 0.3096 0.4067 0.036 Uiso calc R 1 1 . .
    C C61 0.9964(4) 0.24096(13) 0.3735(3) 0.0356(9) Uani d . 1 1 . .
    H H61 1.0882 0.2319 0.4056 0.043 Uiso calc R 1 1 . .
    C C62 0.8979(4) 0.20761(14) 0.3260(3) 0.0384(10) Uani d . 1 1 . .
    H H62 0.9228 0.1762 0.3275 0.046 Uiso calc R 1 1 . .
    C C63 0.7621(4) 0.22115(14) 0.2763(4) 0.0380(9) Uani d . 1 1 . .
    H H63 0.6952 0.1989 0.2441 0.046 Uiso calc R 1 1 . .
    C C64 0.7261(4) 0.26768(13) 0.2747(3) 0.0325(9) Uani d . 1 1 . .
    H H64 0.6350 0.2766 0.2395 0.039 Uiso calc R 1 1 . .
    O O1 0.3309(3) 0.21905(8) 0.2685(2) 0.0342(6) Uani d . 1 1 . .
    O O2 0.6627(2) 0.43771(8) 0.5647(2) 0.0298(6) Uani d . 1 1 . .
    O O3 0.4116(2) 0.36182(9) 0.7845(2) 0.0319(6) Uani d . 1 1 . .
    O O4 -0.0242(3) 0.61327(10) 0.5212(3) 0.0619(9) Uani d . 1 1 . .
    O O5 0.8393(3) 0.22030(9) -0.2012(2) 0.0390(6) Uani d . 1 1 . .
    O O6 1.1596(2) 0.44863(8) 0.0834(2) 0.0326(6) Uani d . 1 1 . .
    O O7 0.8971(2) 0.38020(8) 0.2972(2) 0.0258(5) Uani d . 1 1 . .
    N N1 0.4250(2) 0.42119(10) 0.5347(2) 0.0215(6) Uani d . 1 1 . .
    N N2 0.9258(3) 0.42805(10) 0.0370(2) 0.0219(6) Uani d . 1 1 . .
    O O8 0.4500(3) 0.61465(9) -0.0869(3) 0.0412(6) Uani d . 1 1 . .
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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
    C1 O1 . 1.425(4) ?
    C1 H1A . 0.9600 ?
    C1 H1B . 0.9600 ?
    C1 H1C . 0.9600 ?
    C2 O1 . 1.368(4) ?
    C2 C7 . 1.385(5) ?
    C2 C3 . 1.397(5) ?
    C3 C4 . 1.391(5) ?
    C3 H3 . 0.9300 ?
    C4 C5 . 1.383(4) ?
    C4 H4 . 0.9300 ?
    C5 C6 . 1.406(5) ?
    C5 C8 . 1.508(5) ?
    C6 C7 . 1.375(5) ?
    C6 H6 . 0.9300 ?
    C7 H7 . 0.9300 ?
    C8 N1 . 1.456(4) ?
    C8 H8A . 0.9700 ?
    C8 H8B . 0.9700 ?
    C9 O2 . 1.226(4) ?
    C9 N1 . 1.349(4) ?
    C9 C10 . 1.514(4) ?
    C10 C11 . 1.514(5) ?
    C10 H10A . 0.9700 ?
    C10 H10B . 0.9700 ?
    C11 O3 . 1.420(4) ?
    C11 C12 . 1.559(4) ?
    C11 H11 . 0.9800 ?
    C12 N1 . 1.461(4) ?
    C12 C13 . 1.504(5) ?
    C12 H12 . 0.9800 ?
    C13 C14 . 1.380(5) ?
    C13 C18 . 1.390(5) ?
    C14 C15 . 1.377(5) ?
    C14 H14 . 0.9300 ?
    C15 C16 . 1.388(5) ?
    C15 H15 . 0.9300 ?
    C16 C17 . 1.380(5) ?
    C16 C19 . 1.497(5) ?
    C17 C18 . 1.382(5) ?
    C17 H17 . 0.9300 ?
    C18 H18 . 0.9300 ?
    C19 O4 . 1.239(5) ?
    C19 C20 . 1.499(5) ?
    C20 C25 . 1.500(5) ?
    C20 C21 . 1.504(5) ?
    C20 H20 . 0.9800 ?
    C21 C22 . 1.529(5) ?
    C21 H21A . 0.9700 ?
    C21 H21B . 0.9700 ?
    C22 C23 . 1.502(5) ?
    C22 H22A . 0.9700 ?
    C22 H22B . 0.9700 ?
    C23 C24 . 1.526(6) ?
    C23 H23A . 0.9700 ?
    C23 H23B . 0.9700 ?
    C24 C25 . 1.539(6) ?
    C24 H24A . 0.9700 ?
    C24 H24B . 0.9700 ?
    C25 H25A . 0.9700 ?
    C25 H25B . 0.9700 ?
    C26 O3 . 1.432(4) ?
    C26 C27 . 1.511(6) ?
    C26 H26A . 0.9700 ?
    C26 H26B . 0.9700 ?
    C27 C32 . 1.376(5) ?
    C27 C28 . 1.392(5) ?
    C28 C29 . 1.389(6) ?
    C28 H28 . 0.9300 ?
    C29 C30 . 1.383(6) ?
    C29 H29 . 0.9300 ?
    C30 C31 . 1.367(6) ?
    C30 H30 . 0.9300 ?
    C31 C32 . 1.385(6) ?
    C31 H31 . 0.9300 ?
    C32 H32 . 0.9300 ?
    C33 O5 . 1.432(4) ?
    C33 H33A . 0.9600 ?
    C33 H33B . 0.9600 ?
    C33 H33C . 0.9600 ?
    C34 O5 . 1.372(4) ?
    C34 C39 . 1.390(5) ?
    C34 C35 . 1.394(5) ?
    C35 C36 . 1.387(5) ?
    C35 H35 . 0.9300 ?
    C36 C37 . 1.390(4) ?
    C36 H36 . 0.9300 ?
    C37 C38 . 1.398(5) ?
    C37 C40 . 1.512(5) ?
    C38 C39 . 1.381(5) ?
    C38 H38 . 0.9300 ?
    C39 H39 . 0.9300 ?
    C40 N2 . 1.455(4) ?
    C40 H40A . 0.9700 ?
    C40 H40B . 0.9700 ?
    C41 O6 . 1.224(4) ?
    C41 N2 . 1.352(4) ?
    C41 C42 . 1.511(4) ?
    C42 C43 . 1.518(4) ?
    C42 H42A . 0.9700 ?
    C42 H42B . 0.9700 ?
    C43 O7 . 1.429(4) ?
    C43 C44 . 1.556(4) ?
    C43 H43 . 0.9800 ?
    C44 N2 . 1.455(4) ?
    C44 C45 . 1.517(4) ?
    C44 H44 . 0.9800 ?
    C45 C50 . 1.385(4) ?
    C45 C46 . 1.400(5) ?
    C46 C47 . 1.378(5) ?
    C46 H46 . 0.9300 ?
    C47 C48 . 1.383(4) ?
    C47 H47 . 0.9300 ?
    C48 C49 . 1.400(5) ?
    C48 C51 . 1.507(5) ?
    C49 C50 . 1.389(5) ?
    C49 H49 . 0.9300 ?
    C50 H50 . 0.9300 ?
    C51 O8 . 1.219(4) ?
    C51 C52 . 1.515(5) ?
    C52 C57 . 1.526(5) ?
    C52 C53 . 1.529(4) ?
    C52 H52 . 0.9800 ?
    C53 C54 . 1.524(5) ?
    C53 H53A . 0.9700 ?
    C53 H53B . 0.9700 ?
    C54 C55 . 1.513(5) ?
    C54 H54A . 0.9700 ?
    C54 H54B . 0.9700 ?
    C55 C56 . 1.517(5) ?
    C55 H55A . 0.9700 ?
    C55 H55B . 0.9700 ?
    C56 C57 . 1.525(5) ?
    C56 H56A . 0.9700 ?
    C56 H56B . 0.9700 ?
    C57 H57A . 0.9700 ?
    C57 H57B . 0.9700 ?
    C58 O7 . 1.428(4) ?
    C58 C59 . 1.494(5) ?
    C58 H58A . 0.9700 ?
    C58 H58B . 0.9700 ?
    C59 C60 . 1.395(5) ?
    C59 C64 . 1.396(5) ?
    C60 C61 . 1.379(5) ?
    C60 H60 . 0.9300 ?
    C61 C62 . 1.381(5) ?
    C61 H61 . 0.9300 ?
    C62 C63 . 1.382(5) ?
    C62 H62 . 0.9300 ?
    C63 C64 . 1.376(5) ?
    C63 H63 . 0.9300 ?
    C64 H64 . 0.9300 ?
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
    O1 C1 H1A . . 109.5 ?
    O1 C1 H1B . . 109.5 ?
    H1A C1 H1B . . 109.5 ?
    O1 C1 H1C . . 109.5 ?
    H1A C1 H1C . . 109.5 ?
    H1B C1 H1C . . 109.5 ?
    O1 C2 C7 . . 116.1(3) ?
    O1 C2 C3 . . 124.6(3) ?
    C7 C2 C3 . . 119.3(3) ?
    C4 C3 C2 . . 119.2(3) ?
    C4 C3 H3 . . 120.4 ?
    C2 C3 H3 . . 120.4 ?
    C5 C4 C3 . . 122.1(3) ?
    C5 C4 H4 . . 118.9 ?
    C3 C4 H4 . . 118.9 ?
    C4 C5 C6 . . 117.5(3) ?
    C4 C5 C8 . . 120.5(3) ?
    C6 C5 C8 . . 122.0(3) ?
    C7 C6 C5 . . 121.0(3) ?
    C7 C6 H6 . . 119.5 ?
    C5 C6 H6 . . 119.5 ?
    C6 C7 C2 . . 120.7(3) ?
    C6 C7 H7 . . 119.6 ?
    C2 C7 H7 . . 119.6 ?
    N1 C8 C5 . . 112.4(3) ?
    N1 C8 H8A . . 109.1 ?
    C5 C8 H8A . . 109.1 ?
    N1 C8 H8B . . 109.1 ?
    C5 C8 H8B . . 109.1 ?
    H8A C8 H8B . . 107.8 ?
    O2 C9 N1 . . 125.7(3) ?
    O2 C9 C10 . . 126.9(3) ?
    N1 C9 C10 . . 107.5(3) ?
    C9 C10 C11 . . 104.7(3) ?
    C9 C10 H10A . . 110.8 ?
    C11 C10 H10A . . 110.8 ?
    C9 C10 H10B . . 110.8 ?
    C11 C10 H10B . . 110.8 ?
    H10A C10 H10B . . 108.9 ?
    O3 C11 C10 . . 106.8(3) ?
    O3 C11 C12 . . 110.4(3) ?
    C10 C11 C12 . . 103.2(3) ?
    O3 C11 H11 . . 112.0 ?
    C10 C11 H11 . . 112.0 ?
    C12 C11 H11 . . 112.0 ?
    N1 C12 C13 . . 113.1(3) ?
    N1 C12 C11 . . 102.0(2) ?
    C13 C12 C11 . . 114.2(3) ?
    N1 C12 H12 . . 109.1 ?
    C13 C12 H12 . . 109.1 ?
    C11 C12 H12 . . 109.1 ?
    C14 C13 C18 . . 118.0(3) ?
    C14 C13 C12 . . 121.7(3) ?
    C18 C13 C12 . . 120.4(3) ?
    C15 C14 C13 . . 121.2(3) ?
    C15 C14 H14 . . 119.4 ?
    C13 C14 H14 . . 119.4 ?
    C14 C15 C16 . . 120.6(4) ?
    C14 C15 H15 . . 119.7 ?
    C16 C15 H15 . . 119.7 ?
    C17 C16 C15 . . 118.7(3) ?
    C17 C16 C19 . . 123.2(3) ?
    C15 C16 C19 . . 118.1(3) ?
    C16 C17 C18 . . 120.3(3) ?
    C16 C17 H17 . . 119.9 ?
    C18 C17 H17 . . 119.9 ?
    C17 C18 C13 . . 121.2(3) ?
    C17 C18 H18 . . 119.4 ?
    C13 C18 H18 . . 119.4 ?
    O4 C19 C16 . . 119.1(3) ?
    O4 C19 C20 . . 119.7(3) ?
    C16 C19 C20 . . 121.0(3) ?
    C19 C20 C25 . . 107.4(3) ?
    C19 C20 C21 . . 113.5(3) ?
    C25 C20 C21 . . 112.1(3) ?
    C19 C20 H20 . . 107.9 ?
    C25 C20 H20 . . 107.9 ?
    C21 C20 H20 . . 107.9 ?
    C20 C21 C22 . . 112.2(3) ?
    C20 C21 H21A . . 109.2 ?
    C22 C21 H21A . . 109.2 ?
    C20 C21 H21B . . 109.2 ?
    C22 C21 H21B . . 109.2 ?
    H21A C21 H21B . . 107.9 ?
    C23 C22 C21 . . 110.2(3) ?
    C23 C22 H22A . . 109.6 ?
    C21 C22 H22A . . 109.6 ?
    C23 C22 H22B . . 109.6 ?
    C21 C22 H22B . . 109.6 ?
    H22A C22 H22B . . 108.1 ?
    C22 C23 C24 . . 111.2(3) ?
    C22 C23 H23A . . 109.4 ?
    C24 C23 H23A . . 109.4 ?
    C22 C23 H23B . . 109.4 ?
    C24 C23 H23B . . 109.4 ?
    H23A C23 H23B . . 108.0 ?
    C23 C24 C25 . . 110.1(4) ?
    C23 C24 H24A . . 109.6 ?
    C25 C24 H24A . . 109.6 ?
    C23 C24 H24B . . 109.6 ?
    C25 C24 H24B . . 109.6 ?
    H24A C24 H24B . . 108.2 ?
    C20 C25 C24 . . 110.3(3) ?
    C20 C25 H25A . . 109.6 ?
    C24 C25 H25A . . 109.6 ?
    C20 C25 H25B . . 109.6 ?
    C24 C25 H25B . . 109.6 ?
    H25A C25 H25B . . 108.1 ?
    O3 C26 C27 . . 109.5(3) ?
    O3 C26 H26A . . 109.8 ?
    C27 C26 H26A . . 109.8 ?
    O3 C26 H26B . . 109.8 ?
    C27 C26 H26B . . 109.8 ?
    H26A C26 H26B . . 108.2 ?
    C32 C27 C28 . . 119.2(4) ?
    C32 C27 C26 . . 120.3(3) ?
    C28 C27 C26 . . 120.5(4) ?
    C29 C28 C27 . . 119.6(4) ?
    C29 C28 H28 . . 120.2 ?
    C27 C28 H28 . . 120.2 ?
    C30 C29 C28 . . 120.3(4) ?
    C30 C29 H29 . . 119.9 ?
    C28 C29 H29 . . 119.9 ?
    C31 C30 C29 . . 120.0(5) ?
    C31 C30 H30 . . 120.0 ?
    C29 C30 H30 . . 120.0 ?
    C30 C31 C32 . . 119.9(4) ?
    C30 C31 H31 . . 120.0 ?
    C32 C31 H31 . . 120.0 ?
    C27 C32 C31 . . 121.0(4) ?
    C27 C32 H32 . . 119.5 ?
    C31 C32 H32 . . 119.5 ?
    O5 C33 H33A . . 109.5 ?
    O5 C33 H33B . . 109.5 ?
    H33A C33 H33B . . 109.5 ?
    O5 C33 H33C . . 109.5 ?
    H33A C33 H33C . . 109.5 ?
    H33B C33 H33C . . 109.5 ?
    O5 C34 C39 . . 116.5(3) ?
    O5 C34 C35 . . 123.8(3) ?
    C39 C34 C35 . . 119.7(3) ?
    C36 C35 C34 . . 119.3(3) ?
    C36 C35 H35 . . 120.4 ?
    C34 C35 H35 . . 120.4 ?
    C35 C36 C37 . . 122.0(3) ?
    C35 C36 H36 . . 119.0 ?
    C37 C36 H36 . . 119.0 ?
    C36 C37 C38 . . 117.6(3) ?
    C36 C37 C40 . . 120.1(3) ?
    C38 C37 C40 . . 122.3(3) ?
    C39 C38 C37 . . 121.3(3) ?
    C39 C38 H38 . . 119.3 ?
    C37 C38 H38 . . 119.3 ?
    C38 C39 C34 . . 120.1(3) ?
    C38 C39 H39 . . 120.0 ?
    C34 C39 H39 . . 120.0 ?
    N2 C40 C37 . . 113.2(3) ?
    N2 C40 H40A . . 108.9 ?
    C37 C40 H40A . . 108.9 ?
    N2 C40 H40B . . 108.9 ?
    C37 C40 H40B . . 108.9 ?
    H40A C40 H40B . . 107.7 ?
    O6 C41 N2 . . 125.4(3) ?
    O6 C41 C42 . . 127.0(3) ?
    N2 C41 C42 . . 107.6(3) ?
    C41 C42 C43 . . 104.0(2) ?
    C41 C42 H42A . . 111.0 ?
    C43 C42 H42A . . 111.0 ?
    C41 C42 H42B . . 111.0 ?
    C43 C42 H42B . . 111.0 ?
    H42A C42 H42B . . 109.0 ?
    O7 C43 C42 . . 105.4(2) ?
    O7 C43 C44 . . 109.6(2) ?
    C42 C43 C44 . . 103.1(2) ?
    O7 C43 H43 . . 112.7 ?
    C42 C43 H43 . . 112.7 ?
    C44 C43 H43 . . 112.7 ?
    N2 C44 C45 . . 113.9(3) ?
    N2 C44 C43 . . 101.7(2) ?
    C45 C44 C43 . . 113.1(2) ?
    N2 C44 H44 . . 109.3 ?
    C45 C44 H44 . . 109.3 ?
    C43 C44 H44 . . 109.3 ?
    C50 C45 C46 . . 118.3(3) ?
    C50 C45 C44 . . 119.6(3) ?
    C46 C45 C44 . . 122.1(3) ?
    C47 C46 C45 . . 120.5(3) ?
    C47 C46 H46 . . 119.8 ?
    C45 C46 H46 . . 119.8 ?
    C46 C47 C48 . . 121.3(3) ?
    C46 C47 H47 . . 119.3 ?
    C48 C47 H47 . . 119.3 ?
    C47 C48 C49 . . 118.7(3) ?
    C47 C48 C51 . . 118.4(3) ?
    C49 C48 C51 . . 122.9(3) ?
    C50 C49 C48 . . 119.8(3) ?
    C50 C49 H49 . . 120.1 ?
    C48 C49 H49 . . 120.1 ?
    C45 C50 C49 . . 121.4(3) ?
    C45 C50 H50 . . 119.3 ?
    C49 C50 H50 . . 119.3 ?
    O8 C51 C48 . . 119.4(3) ?
    O8 C51 C52 . . 120.8(3) ?
    C48 C51 C52 . . 119.8(3) ?
    C51 C52 C57 . . 109.9(2) ?
    C51 C52 C53 . . 111.4(3) ?
    C57 C52 C53 . . 109.3(3) ?
    C51 C52 H52 . . 108.8 ?
    C57 C52 H52 . . 108.8 ?
    C53 C52 H52 . . 108.8 ?
    C54 C53 C52 . . 111.3(3) ?
    C54 C53 H53A . . 109.4 ?
    C52 C53 H53A . . 109.4 ?
    C54 C53 H53B . . 109.4 ?
    C52 C53 H53B . . 109.4 ?
    H53A C53 H53B . . 108.0 ?
    C55 C54 C53 . . 110.9(3) ?
    C55 C54 H54A . . 109.5 ?
    C53 C54 H54A . . 109.5 ?
    C55 C54 H54B . . 109.5 ?
    C53 C54 H54B . . 109.5 ?
    H54A C54 H54B . . 108.1 ?
    C54 C55 C56 . . 111.1(3) ?
    C54 C55 H55A . . 109.4 ?
    C56 C55 H55A . . 109.4 ?
    C54 C55 H55B . . 109.4 ?
    C56 C55 H55B . . 109.4 ?
    H55A C55 H55B . . 108.0 ?
    C55 C56 C57 . . 112.0(3) ?
    C55 C56 H56A . . 109.2 ?
    C57 C56 H56A . . 109.2 ?
    C55 C56 H56B . . 109.2 ?
    C57 C56 H56B . . 109.2 ?
    H56A C56 H56B . . 107.9 ?
    C56 C57 C52 . . 111.9(3) ?
    C56 C57 H57A . . 109.2 ?
    C52 C57 H57A . . 109.2 ?
    C56 C57 H57B . . 109.2 ?
    C52 C57 H57B . . 109.2 ?
    H57A C57 H57B . . 107.9 ?
    O7 C58 C59 . . 108.9(3) ?
    O7 C58 H58A . . 109.9 ?
    C59 C58 H58A . . 109.9 ?
    O7 C58 H58B . . 109.9 ?
    C59 C58 H58B . . 109.9 ?
    H58A C58 H58B . . 108.3 ?
    C60 C59 C64 . . 118.0(3) ?
    C60 C59 C58 . . 121.4(3) ?
    C64 C59 C58 . . 120.6(3) ?
    C61 C60 C59 . . 120.3(3) ?
    C61 C60 H60 . . 119.8 ?
    C59 C60 H60 . . 119.8 ?
    C60 C61 C62 . . 120.8(3) ?
    C60 C61 H61 . . 119.6 ?
    C62 C61 H61 . . 119.6 ?
    C61 C62 C63 . . 119.6(4) ?
    C61 C62 H62 . . 120.2 ?
    C63 C62 H62 . . 120.2 ?
    C64 C63 C62 . . 119.8(4) ?
    C64 C63 H63 . . 120.1 ?
    C62 C63 H63 . . 120.1 ?
    C63 C64 C59 . . 121.5(3) ?
    C63 C64 H64 . . 119.3 ?
    C59 C64 H64 . . 119.3 ?
    C2 O1 C1 . . 117.1(3) ?
    C11 O3 C26 . . 114.1(3) ?
    C34 O5 C33 . . 117.9(3) ?
    C58 O7 C43 . . 113.6(2) ?
    C9 N1 C8 . . 123.1(3) ?
    C9 N1 C12 . . 114.3(2) ?
    C8 N1 C12 . . 122.3(2) ?
    C41 N2 C44 . . 114.2(2) ?
    C41 N2 C40 . . 123.2(3) ?
    C44 N2 C40 . . 122.6(2) ?
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
    C62 H62 O4 2_646 0.93 2.47 3.260(5) 142.7
    C17 H17 O2 1_455 0.93 2.38 3.237(4) 153.2
    C49 H49 O6 1_455 0.93 2.33 3.190(4) 154.1
