# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mfu111-4b
_database_code_depnum_ccdc_archive 'CCDC 1952757'
loop_
_audit_author_name
_audit_author_address
'Misaki Okayasu'
;Toho University
Japan
;
_audit_update_record             
;
2019-10-24 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C80 H78 O14'
_chemical_formula_moiety         'C80 H78 O14'
_chemical_formula_weight         1263.49
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   9.18848(15)
_cell_length_b                   18.3718(2)
_cell_length_c                   19.60910(18)
_cell_angle_alpha                98.7879(9)
_cell_angle_beta                 92.6442(10)
_cell_angle_gamma                97.7172(13)
_cell_volume                     3234.19(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    24508
_cell_measurement_theta_min      3.60
_cell_measurement_theta_max      73.29
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1340.00
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_T_max  0.958

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            43357
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_theta_max         73.403
_diffrn_reflns_theta_min         2.285
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             12244
_reflns_number_gt                10419
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_ref         0.2417
_refine_ls_wR_factor_gt          0.2322
_refine_ls_number_restraints     5
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         12244
_refine_ls_number_parameters     859
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1559P)²+1.5150P] 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_diff_density_max         0.62
_refine_diff_density_min         -0.56
_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 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
O1 O 0.2776(2) -0.01657(9) 0.11187(9) 0.0531(4) Uani 1 1 d D . . . .
H1 H 0.332638 -0.035539 0.083244 0.064 Uiso 1 1 calc DR U . . .
O2 O 0.36126(19) 0.08653(9) 0.07092(9) 0.0536(4) Uani 1 1 d . . . . .
O3 O -0.1729(2) 0.42435(10) 0.48012(9) 0.0580(5) Uani 1 1 d D . . . .
H3 H -0.214810 0.451428 0.509174 0.070 Uiso 1 1 calc DR U . . .
O4 O -0.3970(2) 0.36209(12) 0.45797(11) 0.0696(6) Uani 1 1 d . . . . .
O5 O 0.1938(2) 0.06747(10) 0.51806(9) 0.0556(4) Uani 1 1 d D . . . .
H5 H 0.246580 0.041357 0.493828 0.067 Uiso 1 1 calc DR U . . .
O6 O 0.4078(2) 0.13664(14) 0.55052(17) 0.1061(11) Uani 1 1 d . . . . .
O7 O -0.2189(2) 0.54253(10) 0.86475(11) 0.0653(5) Uani 1 1 d D . . . .
H7 H -0.265539 0.570430 0.890726 0.078 Uiso 1 1 calc DR U . . .
O8 O -0.3454(2) 0.45341(10) 0.91283(8) 0.0562(4) Uani 1 1 d . . . . .
O9 O 0.2888(2) 0.48494(10) 0.43046(10) 0.0626(5) Uani 1 1 d . . . . .
O10 O 0.6520(2) 0.00699(12) 0.57125(10) 0.0713(6) Uani 1 1 d . . . . .
O11 O 0.4732(3) 0.20680(12) 0.91616(11) 0.0730(6) Uani 1 1 d . . . . .
O12 O 0.8781(4) 0.26530(19) 1.03102(19) 0.1180(11) Uani 1 1 d . . . . .
O13 O 0.3530(2) 0.35597(11) 1.07387(11) 0.0664(5) Uani 1 1 d . . . . .
O14 O 0.5550(2) 0.08701(11) 0.96643(10) 0.0596(5) Uani 1 1 d . . . . .
C1 C 0.2859(2) 0.05458(13) 0.10971(11) 0.0424(5) Uani 1 1 d . . . . .
C2 C 0.1933(2) 0.09486(12) 0.15979(10) 0.0409(5) Uani 1 1 d . . . . .
C3 C 0.0405(2) 0.08008(11) 0.15180(10) 0.0390(4) Uani 1 1 d . . . . .
C4 C -0.0455(2) 0.12267(12) 0.19859(10) 0.0386(4) Uani 1 1 d . . . . .
C5 C 0.0259(2) 0.17633(11) 0.25276(10) 0.0393(4) Uani 1 1 d . . . . .
C6 C 0.1798(2) 0.18801(12) 0.26240(11) 0.0421(5) Uani 1 1 d . . . . .
C7 C 0.2663(3) 0.14823(12) 0.21400(11) 0.0433(5) Uani 1 1 d . . . . .
C8 C 0.4227(3) 0.16325(14) 0.22465(13) 0.0516(6) Uani 1 1 d . . . . .
H8 H 0.481294 0.138933 0.192275 0.062 Uiso 1 1 calc R U . . .
C9 C 0.4893(3) 0.21137(16) 0.27982(14) 0.0594(7) Uani 1 1 d . . . . .
H9 H 0.593729 0.220397 0.285748 0.071 Uiso 1 1 calc R U . . .
C10 C 0.4038(3) 0.24871(15) 0.32924(14) 0.0583(6) Uani 1 1 d . . . . .
H10 H 0.451342 0.281154 0.368683 0.070 Uiso 1 1 calc R U . . .
C11 C 0.2560(3) 0.23805(14) 0.32008(12) 0.0504(5) Uani 1 1 d . . . . .
H11 H 0.200799 0.264388 0.352716 0.061 Uiso 1 1 calc R U . . .
C12 C -0.0364(3) 0.02556(12) 0.09793(10) 0.0424(5) Uani 1 1 d . . . . .
H12 H 0.018335 -0.002371 0.066278 0.051 Uiso 1 1 calc R U . . .
C13 C -0.1856(3) 0.01252(13) 0.09070(11) 0.0471(5) Uani 1 1 d . . . . .
H13 H -0.233658 -0.024437 0.054527 0.056 Uiso 1 1 calc R U . . .
C14 C -0.2706(3) 0.05401(14) 0.13712(12) 0.0483(5) Uani 1 1 d . . . . .
H14 H -0.375061 0.044337 0.132074 0.058 Uiso 1 1 calc R U . . .
C15 C -0.2023(3) 0.10737(13) 0.18858(11) 0.0439(5) Uani 1 1 d . . . . .
H15 H -0.260285 0.135200 0.218637 0.053 Uiso 1 1 calc R U . . .
C16 C -0.0603(2) 0.22346(11) 0.30072(10) 0.0389(4) Uani 1 1 d . . . . .
C17 C -0.0992(2) 0.20162(11) 0.36397(10) 0.0396(4) Uani 1 1 d . . . . .
C18 C -0.1726(2) 0.24991(12) 0.41179(10) 0.0411(5) Uani 1 1 d . . . . .
C19 C -0.2004(2) 0.31805(12) 0.39503(11) 0.0403(5) Uani 1 1 d . . . . .
C20 C -0.1646(2) 0.33983(12) 0.33157(11) 0.0411(5) Uani 1 1 d . . . . .
C21 C -0.0944(2) 0.29085(12) 0.28313(11) 0.0406(5) Uani 1 1 d . . . . .
C22 C -0.0593(3) 0.31430(13) 0.21860(11) 0.0467(5) Uani 1 1 d . . . . .
H22 H -0.011861 0.283196 0.186160 0.056 Uiso 1 1 calc R U . . .
C23 C -0.0921(3) 0.37963(14) 0.20285(13) 0.0535(6) Uani 1 1 d . . . . .
H23 H -0.068994 0.393360 0.159398 0.064 Uiso 1 1 calc R U . . .
C24 C -0.1609(3) 0.42796(14) 0.25081(13) 0.0519(6) Uani 1 1 d . . . . .
H24 H -0.182500 0.474019 0.239534 0.062 Uiso 1 1 calc R U . . .
C25 C -0.1959(3) 0.40833(13) 0.31277(12) 0.0469(5) Uani 1 1 d . . . . .
H25 H -0.242247 0.440999 0.344254 0.056 Uiso 1 1 calc R U . . .
C26 C -0.0662(3) 0.13356(12) 0.38358(11) 0.0446(5) Uani 1 1 d . . . . .
H26 H -0.016289 0.101584 0.353104 0.054 Uiso 1 1 calc R U . . .
C27 C -0.1046(3) 0.11372(13) 0.44479(12) 0.0509(6) Uani 1 1 d . . . . .
H27 H -0.080850 0.068318 0.456766 0.061 Uiso 1 1 calc R U . . .
C28 C -0.1801(3) 0.16023(14) 0.49124(12) 0.0567(6) Uani 1 1 d . . . . .
H28 H -0.208650 0.145114 0.533470 0.068 Uiso 1 1 calc R U . . .
C29 C -0.2116(3) 0.22593(13) 0.47563(11) 0.0513(6) Uani 1 1 d . . . . .
H29 H -0.260490 0.256781 0.507618 0.062 Uiso 1 1 calc R U . . .
C30 C -0.2694(3) 0.37002(12) 0.44729(11) 0.0429(5) Uani 1 1 d . . . . .
C31 C 0.2762(3) 0.12389(14) 0.55492(14) 0.0554(6) Uani 1 1 d . . . . .
C32 C 0.1943(3) 0.17473(13) 0.60182(12) 0.0455(5) Uani 1 1 d . . . . .
C33 C 0.1306(3) 0.14992(13) 0.65942(12) 0.0457(5) Uani 1 1 d . . . . .
C34 C 0.0575(3) 0.20004(12) 0.70507(11) 0.0430(5) Uani 1 1 d . . . . .
C35 C 0.0500(2) 0.27239(12) 0.69146(10) 0.0406(5) Uani 1 1 d . . . . .
C36 C 0.1129(2) 0.29630(12) 0.63345(11) 0.0414(5) Uani 1 1 d . . . . .
C37 C 0.1875(3) 0.24656(13) 0.58785(11) 0.0451(5) Uani 1 1 d . . . . .
C38 C 0.2534(3) 0.27332(14) 0.53010(13) 0.0552(6) Uani 1 1 d . . . . .
H38 H 0.303336 0.241366 0.499646 0.066 Uiso 1 1 calc R U . . .
C39 C 0.2459(3) 0.34344(15) 0.51804(14) 0.0622(7) Uani 1 1 d . . . . .
H39 H 0.292775 0.360549 0.480096 0.075 Uiso 1 1 calc R U . . .
C40 C 0.1683(3) 0.39157(14) 0.56187(13) 0.0582(6) Uani 1 1 d . . . . .
H40 H 0.160527 0.439951 0.551864 0.070 Uiso 1 1 calc R U . . .
C41 C 0.1051(3) 0.36914(13) 0.61787(12) 0.0478(5) Uani 1 1 d . . . . .
H41 H 0.055190 0.402336 0.647029 0.057 Uiso 1 1 calc R U . . .
C42 C 0.1376(3) 0.07717(14) 0.67585(13) 0.0528(6) Uani 1 1 d . . . . .
H42 H 0.185329 0.043310 0.646248 0.063 Uiso 1 1 calc R U . . .
C43 C 0.0779(3) 0.05550(14) 0.73257(13) 0.0585(6) Uani 1 1 d . . . . .
H43 H 0.086302 0.007293 0.742841 0.070 Uiso 1 1 calc R U . . .
C44 C 0.0027(3) 0.10410(14) 0.77683(13) 0.0577(6) Uani 1 1 d . . . . .
H44 H -0.041109 0.087804 0.815836 0.069 Uiso 1 1 calc R U . . .
C45 C -0.0069(3) 0.17415(13) 0.76363(12) 0.0491(5) Uani 1 1 d . . . . .
H45 H -0.057181 0.206258 0.793791 0.059 Uiso 1 1 calc R U . . .
C46 C -0.0282(2) 0.32398(11) 0.73875(10) 0.0398(5) Uani 1 1 d . . . . .
C47 C 0.0486(2) 0.36899(12) 0.79755(10) 0.0405(5) Uani 1 1 d . . . . .
C48 C -0.0280(2) 0.41840(12) 0.84265(10) 0.0410(5) Uani 1 1 d . . . . .
C49 C -0.1773(3) 0.42045(12) 0.82774(10) 0.0422(5) Uani 1 1 d . . . . .
C50 C -0.2553(3) 0.37535(12) 0.76951(10) 0.0423(5) Uani 1 1 d . . . . .
C51 C -0.1777(2) 0.32655(12) 0.72432(10) 0.0410(5) Uani 1 1 d . . . . .
C52 C -0.2587(3) 0.28169(13) 0.66503(11) 0.0452(5) Uani 1 1 d . . . . .
H52 H -0.209650 0.249026 0.634844 0.054 Uiso 1 1 calc R U . . .
C53 C -0.4032(3) 0.28446(14) 0.65072(12) 0.0503(6) Uani 1 1 d . . . . .
H53 H -0.453983 0.253957 0.610957 0.060 Uiso 1 1 calc R U . . .
C54 C -0.4795(3) 0.33317(15) 0.69530(12) 0.0523(6) Uani 1 1 d . . . . .
H54 H -0.580699 0.335315 0.684889 0.063 Uiso 1 1 calc R U . . .
C55 C -0.4075(3) 0.37647(14) 0.75261(11) 0.0476(5) Uani 1 1 d . . . . .
H55 H -0.459776 0.408203 0.782069 0.057 Uiso 1 1 calc R U . . .
C56 C 0.2006(3) 0.36778(13) 0.81447(11) 0.0443(5) Uani 1 1 d . . . . .
H56 H 0.253029 0.336201 0.784890 0.053 Uiso 1 1 calc R U . . .
C57 C 0.2729(3) 0.41095(13) 0.87223(12) 0.0478(5) Uani 1 1 d . . . . .
H57 H 0.374281 0.409097 0.882415 0.057 Uiso 1 1 calc R U . . .
C58 C 0.1967(3) 0.45852(13) 0.91697(11) 0.0483(5) Uani 1 1 d . . . . .
H58 H 0.247096 0.487829 0.957428 0.058 Uiso 1 1 calc R U . . .
C59 C 0.0528(3) 0.46257(12) 0.90259(11) 0.0446(5) Uani 1 1 d . . . . .
H59 H 0.004305 0.495398 0.932874 0.054 Uiso 1 1 calc R U . . .
C60 C -0.2572(3) 0.47297(13) 0.87342(11) 0.0455(5) Uani 1 1 d . . . . .
C61 C 0.4262(3) 0.50676(17) 0.40324(14) 0.0623(7) Uani 1 1 d . . . . .
H61A H 0.509090 0.496595 0.432707 0.075 Uiso 1 1 calc R U . . .
H61B H 0.439432 0.560409 0.399760 0.075 Uiso 1 1 calc R U . . .
C62 C 0.4165(4) 0.45905(19) 0.33138(16) 0.0756(9) Uani 1 1 d . . . . .
H62A H 0.473640 0.485520 0.298720 0.091 Uiso 1 1 calc R U . . .
H62B H 0.453006 0.411112 0.333615 0.091 Uiso 1 1 calc R U . . .
C63 C 0.2548(4) 0.4472(2) 0.31047(17) 0.0863(11) Uani 1 1 d . . . . .
H63A H 0.229397 0.486124 0.284055 0.104 Uiso 1 1 calc R U . . .
H63B H 0.224955 0.397829 0.281680 0.104 Uiso 1 1 calc R U . . .
C64 C 0.1823(4) 0.4521(3) 0.3764(2) 0.1062(15) Uani 1 1 d . . . . .
H64A H 0.101625 0.482655 0.375032 0.127 Uiso 1 1 calc R U . . .
H64B H 0.139877 0.401749 0.384032 0.127 Uiso 1 1 calc R U . . .
C65 C 0.7262(4) 0.0396(2) 0.63515(16) 0.0816(9) Uani 1 1 d . . . . .
H65A H 0.712654 0.092531 0.646128 0.098 Uiso 1 1 calc R U . . .
H65B H 0.832871 0.036736 0.633590 0.098 Uiso 1 1 calc R U . . .
C66 C 0.6636(5) -0.0019(3) 0.6875(2) 0.1062(14) Uani 1 1 d . . . . .
H66A H 0.671771 0.029870 0.733476 0.127 Uiso 1 1 calc R U . . .
H66B H 0.712810 -0.046096 0.690841 0.127 Uiso 1 1 calc R U . . .
C67 C 0.5034(5) -0.0245(4) 0.6603(3) 0.1283(19) Uani 1 1 d . . . . .
H67A H 0.460632 -0.071496 0.675032 0.154 Uiso 1 1 calc R U . . .
H67B H 0.443193 0.014922 0.676060 0.154 Uiso 1 1 calc R U . . .
C68 C 0.5149(4) -0.0339(2) 0.58498(17) 0.0872(10) Uani 1 1 d . . . . .
H68A H 0.511209 -0.087266 0.565971 0.105 Uiso 1 1 calc R U . . .
H68B H 0.431772 -0.015064 0.562720 0.105 Uiso 1 1 calc R U . . .
C69 C 0.5992(4) 0.23944(19) 0.88615(17) 0.0744(8) Uani 1 1 d . . . . .
H69A H 0.689227 0.242300 0.916764 0.089 Uiso 1 1 calc R U . . .
H69B H 0.587557 0.290166 0.877672 0.089 Uiso 1 1 calc R U . . .
C70 C 0.6073(4) 0.18831(18) 0.81904(16) 0.0717(8) Uani 1 1 d . . . . .
H70A H 0.666456 0.148425 0.825732 0.086 Uiso 1 1 calc R U . . .
H70B H 0.650725 0.216169 0.783716 0.086 Uiso 1 1 calc R U . . .
C71 C 0.4479(4) 0.1565(3) 0.79825(19) 0.0960(12) Uani 1 1 d . . . . .
H71A H 0.412806 0.175533 0.756766 0.115 Uiso 1 1 calc R U . . .
H71B H 0.435680 0.101511 0.788160 0.115 Uiso 1 1 calc R U . . .
C72 C 0.3651(4) 0.1822(2) 0.8594(2) 0.0813(9) Uani 1 1 d . . . . .
H72A H 0.311798 0.223453 0.850280 0.098 Uiso 1 1 calc R U . . .
H72B H 0.292986 0.140846 0.869599 0.098 Uiso 1 1 calc R U . . .
C73 C 0.9823(5) 0.3097(2) 1.0004(2) 0.0969(12) Uani 1 1 d . . . . .
H73A H 1.048284 0.343533 1.036505 0.116 Uiso 1 1 calc R U . . .
H73B H 0.932705 0.340338 0.971817 0.116 Uiso 1 1 calc R U . . .
C74 C 1.0675(5) 0.2619(2) 0.95728(19) 0.1044(15) Uani 1 1 d . . . . .
H74A H 1.174408 0.277336 0.968542 0.125 Uiso 1 1 calc R U . . .
H74B H 1.045080 0.263063 0.907621 0.125 Uiso 1 1 calc R U . . .
C75 C 1.0198(7) 0.1863(3) 0.9745(3) 0.150(3) Uani 1 1 d D . . . .
H75A H 0.964333 0.153394 0.934282 0.180 Uiso 1 1 calc R U . . .
H75B H 1.105950 0.163369 0.988132 0.180 Uiso 1 1 calc R U . . .
C76 C 0.9277(5) 0.1979(2) 1.0309(2) 0.1019(13) Uani 1 1 d D . . . .
H76A H 0.843223 0.157419 1.025660 0.122 Uiso 1 1 calc R U . . .
H76B H 0.984159 0.197952 1.075180 0.122 Uiso 1 1 calc R U . . .
C77 C 0.3923(5) 0.3056(2) 1.1201(2) 0.0912(11) Uani 1 1 d . . . . .
H77A H 0.323502 0.258349 1.111144 0.109 Uiso 1 1 calc R U . . .
H77B H 0.388157 0.328510 1.168978 0.109 Uiso 1 1 calc R U . . .
C78 C 0.5444(4) 0.2918(2) 1.1060(2) 0.0861(10) Uani 1 1 d . . . . .
H78A H 0.543947 0.245825 1.072188 0.103 Uiso 1 1 calc R U . . .
H78B H 0.601373 0.287601 1.149032 0.103 Uiso 1 1 calc R U . . .
C79 C 0.6066(4) 0.3599(2) 1.0766(2) 0.0921(11) Uani 1 1 d . . . . .
H79A H 0.643137 0.402026 1.113923 0.111 Uiso 1 1 calc R U . . .
H79B H 0.687700 0.349431 1.046780 0.111 Uiso 1 1 calc R U . . .
C80 C 0.4781(3) 0.37600(17) 1.03584(14) 0.0620(7) Uani 1 1 d . . . . .
H80A H 0.488483 0.429405 1.031500 0.074 Uiso 1 1 calc R U . . .
H80B H 0.468119 0.346102 0.988943 0.074 Uiso 1 1 calc R U . . .
H14A H 0.534(4) 0.130(2) 0.9536(17) 0.070(9) Uiso 1 1 d . . . . .
H14B H 0.508(4) 0.0802(19) 1.0013(19) 0.076(10) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.306(3) . ?
O1 H1 0.8400 . ?
O2 C1 1.216(3) . ?
O3 C30 1.308(3) . ?
O3 H3 0.8400 . ?
O4 C30 1.194(3) . ?
O5 C31 1.296(3) . ?
O5 H5 0.8400 . ?
O6 C31 1.210(3) . ?
O7 C60 1.318(3) . ?
O7 H7 0.8400 . ?
O8 C60 1.204(3) . ?
O9 C64 1.413(4) . ?
O9 C61 1.424(3) . ?
O10 C65 1.406(4) . ?
O10 C68 1.436(4) . ?
O11 C69 1.425(4) . ?
O11 C72 1.433(4) . ?
O12 C76 1.375(5) . ?
O12 C73 1.392(5) . ?
O13 C80 1.436(3) . ?
O13 C77 1.458(4) . ?
O14 H14A 0.90(4) . ?
O14 H14B 0.84(4) . ?
C1 C2 1.503(3) . ?
C2 C3 1.391(3) . ?
C2 C7 1.407(3) . ?
C3 C12 1.427(3) . ?
C3 C4 1.447(3) . ?
C4 C5 1.405(3) . ?
C4 C15 1.429(3) . ?
C5 C6 1.401(3) . ?
C5 C16 1.506(3) . ?
C6 C11 1.432(3) . ?
C6 C7 1.442(3) . ?
C7 C8 1.425(3) . ?
C8 C9 1.352(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.428(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.345(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.356(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.426(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.359(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C21 1.405(3) . ?
C16 C17 1.408(3) . ?
C17 C26 1.429(3) . ?
C17 C18 1.444(3) . ?
C18 C19 1.394(3) . ?
C18 C29 1.434(3) . ?
C19 C20 1.404(3) . ?
C19 C30 1.512(3) . ?
C20 C25 1.425(3) . ?
C20 C21 1.442(3) . ?
C21 C22 1.434(3) . ?
C22 C23 1.352(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.423(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.359(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.355(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.422(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.354(4) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C31 C32 1.509(3) . ?
C32 C37 1.397(3) . ?
C32 C33 1.405(3) . ?
C33 C42 1.431(3) . ?
C33 C34 1.439(3) . ?
C34 C35 1.405(3) . ?
C34 C45 1.432(3) . ?
C35 C36 1.402(3) . ?
C35 C46 1.500(3) . ?
C36 C41 1.427(3) . ?
C36 C37 1.442(3) . ?
C37 C38 1.430(3) . ?
C38 C39 1.355(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.422(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.358(3) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 C43 1.353(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.418(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.364(3) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C51 1.398(3) . ?
C46 C47 1.410(3) . ?
C47 C56 1.425(3) . ?
C47 C48 1.444(3) . ?
C48 C49 1.395(3) . ?
C48 C59 1.435(3) . ?
C49 C50 1.407(3) . ?
C49 C60 1.503(3) . ?
C50 C55 1.426(3) . ?
C50 C51 1.444(3) . ?
C51 C52 1.431(3) . ?
C52 C53 1.354(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.429(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.361(3) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57 1.367(3) . ?
C56 H56 0.9500 . ?
C57 C58 1.418(3) . ?
C57 H57 0.9500 . ?
C58 C59 1.353(3) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
C61 C62 1.534(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.500(5) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.478(6) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.463(5) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.522(6) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 C68 1.472(6) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 C70 1.506(4) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 C71 1.515(5) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 C72 1.498(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 C74 1.455(6) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 C75 1.493(7) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 C76 1.432(5) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C77 C78 1.485(5) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C78 C79 1.512(5) . ?
C78 H78A 0.9900 . ?
C78 H78B 0.9900 . ?
C79 C80 1.483(5) . ?
C79 H79A 0.9900 . ?
C79 H79B 0.9900 . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?

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
C1 O1 H1 109.5 . . ?
C30 O3 H3 109.5 . . ?
C31 O5 H5 109.5 . . ?
C60 O7 H7 109.5 . . ?
C64 O9 C61 110.4(3) . . ?
C65 O10 C68 107.8(2) . . ?
C69 O11 C72 104.8(2) . . ?
C76 O12 C73 107.1(3) . . ?
C80 O13 C77 108.6(2) . . ?
H14A O14 H14B 108(3) . . ?
O2 C1 O1 123.8(2) . . ?
O2 C1 C2 121.9(2) . . ?
O1 C1 C2 114.25(18) . . ?
C3 C2 C7 121.55(19) . . ?
C3 C2 C1 120.59(18) . . ?
C7 C2 C1 117.85(19) . . ?
C2 C3 C12 122.77(19) . . ?
C2 C3 C4 119.25(19) . . ?
C12 C3 C4 117.96(19) . . ?
C5 C4 C15 122.04(19) . . ?
C5 C4 C3 119.73(19) . . ?
C15 C4 C3 118.22(18) . . ?
C6 C5 C4 120.43(19) . . ?
C6 C5 C16 118.57(18) . . ?
C4 C5 C16 120.98(19) . . ?
C5 C6 C11 121.99(19) . . ?
C5 C6 C7 120.00(19) . . ?
C11 C6 C7 118.0(2) . . ?
C2 C7 C8 122.9(2) . . ?
C2 C7 C6 118.9(2) . . ?
C8 C7 C6 118.2(2) . . ?
C9 C8 C7 121.4(2) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C10 120.4(2) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C11 C10 C9 120.2(2) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C6 121.7(2) . . ?
C10 C11 H11 119.2 . . ?
C6 C11 H11 119.2 . . ?
C13 C12 C3 121.80(19) . . ?
C13 C12 H12 119.1 . . ?
C3 C12 H12 119.1 . . ?
C12 C13 C14 120.3(2) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 120.0(2) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C4 121.6(2) . . ?
C14 C15 H15 119.2 . . ?
C4 C15 H15 119.2 . . ?
C21 C16 C17 120.83(18) . . ?
C21 C16 C5 119.22(18) . . ?
C17 C16 C5 119.87(19) . . ?
C16 C17 C26 122.33(19) . . ?
C16 C17 C18 119.39(19) . . ?
C26 C17 C18 118.27(19) . . ?
C19 C18 C29 122.63(19) . . ?
C19 C18 C17 119.28(19) . . ?
C29 C18 C17 118.1(2) . . ?
C18 C19 C20 121.81(19) . . ?
C18 C19 C30 118.75(19) . . ?
C20 C19 C30 119.43(19) . . ?
C19 C20 C25 122.58(19) . . ?
C19 C20 C21 118.9(2) . . ?
C25 C20 C21 118.53(19) . . ?
C16 C21 C22 122.48(19) . . ?
C16 C21 C20 119.72(19) . . ?
C22 C21 C20 117.8(2) . . ?
C23 C22 C21 121.6(2) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C22 C23 C24 120.5(2) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C25 C24 C23 120.1(2) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C20 121.5(2) . . ?
C24 C25 H25 119.3 . . ?
C20 C25 H25 119.3 . . ?
C27 C26 C17 121.3(2) . . ?
C27 C26 H26 119.4 . . ?
C17 C26 H26 119.4 . . ?
C26 C27 C28 120.6(2) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C29 C28 C27 120.4(2) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C28 C29 C18 121.4(2) . . ?
C28 C29 H29 119.3 . . ?
C18 C29 H29 119.3 . . ?
O4 C30 O3 123.7(2) . . ?
O4 C30 C19 124.0(2) . . ?
O3 C30 C19 112.22(19) . . ?
O6 C31 O5 123.0(2) . . ?
O6 C31 C32 122.3(2) . . ?
O5 C31 C32 114.7(2) . . ?
C37 C32 C33 121.5(2) . . ?
C37 C32 C31 118.8(2) . . ?
C33 C32 C31 119.6(2) . . ?
C32 C33 C42 122.9(2) . . ?
C32 C33 C34 119.0(2) . . ?
C42 C33 C34 118.1(2) . . ?
C35 C34 C45 121.6(2) . . ?
C35 C34 C33 120.0(2) . . ?
C45 C34 C33 118.4(2) . . ?
C36 C35 C34 120.53(19) . . ?
C36 C35 C46 119.79(19) . . ?
C34 C35 C46 119.67(19) . . ?
C35 C36 C41 121.70(19) . . ?
C35 C36 C37 119.8(2) . . ?
C41 C36 C37 118.5(2) . . ?
C32 C37 C38 122.4(2) . . ?
C32 C37 C36 119.3(2) . . ?
C38 C37 C36 118.3(2) . . ?
C39 C38 C37 121.2(2) . . ?
C39 C38 H38 119.4 . . ?
C37 C38 H38 119.4 . . ?
C38 C39 C40 120.4(2) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
C41 C40 C39 120.7(2) . . ?
C41 C40 H40 119.6 . . ?
C39 C40 H40 119.6 . . ?
C40 C41 C36 120.8(2) . . ?
C40 C41 H41 119.6 . . ?
C36 C41 H41 119.6 . . ?
C43 C42 C33 121.5(2) . . ?
C43 C42 H42 119.3 . . ?
C33 C42 H42 119.3 . . ?
C42 C43 C44 120.6(2) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
C45 C44 C43 120.3(2) . . ?
C45 C44 H44 119.9 . . ?
C43 C44 H44 119.9 . . ?
C44 C45 C34 121.1(2) . . ?
C44 C45 H45 119.5 . . ?
C34 C45 H45 119.5 . . ?
C51 C46 C47 120.45(19) . . ?
C51 C46 C35 119.48(18) . . ?
C47 C46 C35 120.07(19) . . ?
C46 C47 C56 122.3(2) . . ?
C46 C47 C48 119.5(2) . . ?
C56 C47 C48 118.21(19) . . ?
C49 C48 C59 122.4(2) . . ?
C49 C48 C47 119.55(19) . . ?
C59 C48 C47 118.0(2) . . ?
C48 C49 C50 121.4(2) . . ?
C48 C49 C60 119.95(19) . . ?
C50 C49 C60 118.6(2) . . ?
C49 C50 C55 122.8(2) . . ?
C49 C50 C51 118.7(2) . . ?
C55 C50 C51 118.46(19) . . ?
C46 C51 C52 121.81(19) . . ?
C46 C51 C50 120.35(19) . . ?
C52 C51 C50 117.8(2) . . ?
C53 C52 C51 121.9(2) . . ?
C53 C52 H52 119.0 . . ?
C51 C52 H52 119.0 . . ?
C52 C53 C54 120.1(2) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C55 C54 C53 120.1(2) . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 119.9 . . ?
C54 C55 C50 121.5(2) . . ?
C54 C55 H55 119.2 . . ?
C50 C55 H55 119.2 . . ?
C57 C56 C47 121.6(2) . . ?
C57 C56 H56 119.2 . . ?
C47 C56 H56 119.2 . . ?
C56 C57 C58 120.1(2) . . ?
C56 C57 H57 120.0 . . ?
C58 C57 H57 120.0 . . ?
C59 C58 C57 120.6(2) . . ?
C59 C58 H58 119.7 . . ?
C57 C58 H58 119.7 . . ?
C58 C59 C48 121.5(2) . . ?
C58 C59 H59 119.3 . . ?
C48 C59 H59 119.3 . . ?
O8 C60 O7 124.5(2) . . ?
O8 C60 C49 123.8(2) . . ?
O7 C60 C49 111.70(19) . . ?
O9 C61 C62 104.2(2) . . ?
O9 C61 H61A 110.9 . . ?
C62 C61 H61A 110.9 . . ?
O9 C61 H61B 110.9 . . ?
C62 C61 H61B 110.9 . . ?
H61A C61 H61B 108.9 . . ?
C63 C62 C61 103.1(3) . . ?
C63 C62 H62A 111.1 . . ?
C61 C62 H62A 111.1 . . ?
C63 C62 H62B 111.1 . . ?
C61 C62 H62B 111.1 . . ?
H62A C62 H62B 109.1 . . ?
C64 C63 C62 104.7(3) . . ?
C64 C63 H63A 110.8 . . ?
C62 C63 H63A 110.8 . . ?
C64 C63 H63B 110.8 . . ?
C62 C63 H63B 110.8 . . ?
H63A C63 H63B 108.9 . . ?
O9 C64 C63 108.3(3) . . ?
O9 C64 H64A 110.0 . . ?
C63 C64 H64A 110.0 . . ?
O9 C64 H64B 110.0 . . ?
C63 C64 H64B 110.0 . . ?
H64A C64 H64B 108.4 . . ?
O10 C65 C66 107.2(3) . . ?
O10 C65 H65A 110.3 . . ?
C66 C65 H65A 110.3 . . ?
O10 C65 H65B 110.3 . . ?
C66 C65 H65B 110.3 . . ?
H65A C65 H65B 108.5 . . ?
C65 C66 C67 102.7(3) . . ?
C65 C66 H66A 111.2 . . ?
C67 C66 H66A 111.2 . . ?
C65 C66 H66B 111.2 . . ?
C67 C66 H66B 111.2 . . ?
H66A C66 H66B 109.1 . . ?
C68 C67 C66 102.1(3) . . ?
C68 C67 H67A 111.3 . . ?
C66 C67 H67A 111.3 . . ?
C68 C67 H67B 111.3 . . ?
C66 C67 H67B 111.3 . . ?
H67A C67 H67B 109.2 . . ?
O10 C68 C67 108.5(3) . . ?
O10 C68 H68A 110.0 . . ?
C67 C68 H68A 110.0 . . ?
O10 C68 H68B 110.0 . . ?
C67 C68 H68B 110.0 . . ?
H68A C68 H68B 108.4 . . ?
O11 C69 C70 104.7(2) . . ?
O11 C69 H69A 110.8 . . ?
C70 C69 H69A 110.8 . . ?
O11 C69 H69B 110.8 . . ?
C70 C69 H69B 110.8 . . ?
H69A C69 H69B 108.9 . . ?
C69 C70 C71 103.5(3) . . ?
C69 C70 H70A 111.1 . . ?
C71 C70 H70A 111.1 . . ?
C69 C70 H70B 111.1 . . ?
C71 C70 H70B 111.1 . . ?
H70A C70 H70B 109.0 . . ?
C72 C71 C70 105.0(3) . . ?
C72 C71 H71A 110.8 . . ?
C70 C71 H71A 110.8 . . ?
C72 C71 H71B 110.8 . . ?
C70 C71 H71B 110.8 . . ?
H71A C71 H71B 108.8 . . ?
O11 C72 C71 106.2(3) . . ?
O11 C72 H72A 110.5 . . ?
C71 C72 H72A 110.5 . . ?
O11 C72 H72B 110.5 . . ?
C71 C72 H72B 110.5 . . ?
H72A C72 H72B 108.7 . . ?
O12 C73 C74 108.8(3) . . ?
O12 C73 H73A 109.9 . . ?
C74 C73 H73A 109.9 . . ?
O12 C73 H73B 109.9 . . ?
C74 C73 H73B 109.9 . . ?
H73A C73 H73B 108.3 . . ?
C73 C74 C75 103.9(3) . . ?
C73 C74 H74A 111.0 . . ?
C75 C74 H74A 111.0 . . ?
C73 C74 H74B 111.0 . . ?
C75 C74 H74B 111.0 . . ?
H74A C74 H74B 109.0 . . ?
C76 C75 C74 105.2(4) . . ?
C76 C75 H75A 110.7 . . ?
C74 C75 H75A 110.7 . . ?
C76 C75 H75B 110.7 . . ?
C74 C75 H75B 110.7 . . ?
H75A C75 H75B 108.8 . . ?
O12 C76 C75 108.3(4) . . ?
O12 C76 H76A 110.0 . . ?
C75 C76 H76A 110.0 . . ?
O12 C76 H76B 110.0 . . ?
C75 C76 H76B 110.0 . . ?
H76A C76 H76B 108.4 . . ?
O13 C77 C78 106.6(3) . . ?
O13 C77 H77A 110.4 . . ?
C78 C77 H77A 110.4 . . ?
O13 C77 H77B 110.4 . . ?
C78 C77 H77B 110.4 . . ?
H77A C77 H77B 108.6 . . ?
C77 C78 C79 102.8(3) . . ?
C77 C78 H78A 111.2 . . ?
C79 C78 H78A 111.2 . . ?
C77 C78 H78B 111.2 . . ?
C79 C78 H78B 111.2 . . ?
H78A C78 H78B 109.1 . . ?
C80 C79 C78 102.9(3) . . ?
C80 C79 H79A 111.2 . . ?
C78 C79 H79A 111.2 . . ?
C80 C79 H79B 111.2 . . ?
C78 C79 H79B 111.2 . . ?
H79A C79 H79B 109.1 . . ?
O13 C80 C79 105.2(3) . . ?
O13 C80 H80A 110.7 . . ?
C79 C80 H80A 110.7 . . ?
O13 C80 H80B 110.7 . . ?
C79 C80 H80B 110.7 . . ?
H80A C80 H80B 108.8 . . ?

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
O2 C1 C2 C3 113.0(3) . . . . ?
O1 C1 C2 C3 -67.0(3) . . . . ?
O2 C1 C2 C7 -66.2(3) . . . . ?
O1 C1 C2 C7 113.8(2) . . . . ?
C7 C2 C3 C12 -179.1(2) . . . . ?
C1 C2 C3 C12 1.7(3) . . . . ?
C7 C2 C3 C4 2.6(3) . . . . ?
C1 C2 C3 C4 -176.62(19) . . . . ?
C2 C3 C4 C5 -2.2(3) . . . . ?
C12 C3 C4 C5 179.32(19) . . . . ?
C2 C3 C4 C15 178.9(2) . . . . ?
C12 C3 C4 C15 0.5(3) . . . . ?
C15 C4 C5 C6 177.8(2) . . . . ?
C3 C4 C5 C6 -1.0(3) . . . . ?
C15 C4 C5 C16 -3.4(3) . . . . ?
C3 C4 C5 C16 177.76(18) . . . . ?
C4 C5 C6 C11 -175.1(2) . . . . ?
C16 C5 C6 C11 6.1(3) . . . . ?
C4 C5 C6 C7 3.9(3) . . . . ?
C16 C5 C6 C7 -174.87(19) . . . . ?
C3 C2 C7 C8 178.3(2) . . . . ?
C1 C2 C7 C8 -2.5(3) . . . . ?
C3 C2 C7 C6 0.3(3) . . . . ?
C1 C2 C7 C6 179.53(19) . . . . ?
C5 C6 C7 C2 -3.6(3) . . . . ?
C11 C6 C7 C2 175.5(2) . . . . ?
C5 C6 C7 C8 178.3(2) . . . . ?
C11 C6 C7 C8 -2.6(3) . . . . ?
C2 C7 C8 C9 -175.6(2) . . . . ?
C6 C7 C8 C9 2.4(4) . . . . ?
C7 C8 C9 C10 0.0(4) . . . . ?
C8 C9 C10 C11 -2.1(5) . . . . ?
C9 C10 C11 C6 1.8(4) . . . . ?
C5 C6 C11 C10 179.6(2) . . . . ?
C7 C6 C11 C10 0.6(4) . . . . ?
C2 C3 C12 C13 -179.4(2) . . . . ?
C4 C3 C12 C13 -1.0(3) . . . . ?
C3 C12 C13 C14 0.5(4) . . . . ?
C12 C13 C14 C15 0.6(4) . . . . ?
C13 C14 C15 C4 -1.1(4) . . . . ?
C5 C4 C15 C14 -178.3(2) . . . . ?
C3 C4 C15 C14 0.6(3) . . . . ?
C6 C5 C16 C21 90.3(3) . . . . ?
C4 C5 C16 C21 -88.5(3) . . . . ?
C6 C5 C16 C17 -86.5(3) . . . . ?
C4 C5 C16 C17 94.7(2) . . . . ?
C21 C16 C17 C26 -179.9(2) . . . . ?
C5 C16 C17 C26 -3.2(3) . . . . ?
C21 C16 C17 C18 -1.2(3) . . . . ?
C5 C16 C17 C18 175.56(18) . . . . ?
C16 C17 C18 C19 -1.5(3) . . . . ?
C26 C17 C18 C19 177.3(2) . . . . ?
C16 C17 C18 C29 179.7(2) . . . . ?
C26 C17 C18 C29 -1.5(3) . . . . ?
C29 C18 C19 C20 -178.5(2) . . . . ?
C17 C18 C19 C20 2.7(3) . . . . ?
C29 C18 C19 C30 2.3(3) . . . . ?
C17 C18 C19 C30 -176.53(19) . . . . ?
C18 C19 C20 C25 178.2(2) . . . . ?
C30 C19 C20 C25 -2.6(3) . . . . ?
C18 C19 C20 C21 -1.3(3) . . . . ?
C30 C19 C20 C21 177.96(19) . . . . ?
C17 C16 C21 C22 -178.7(2) . . . . ?
C5 C16 C21 C22 4.6(3) . . . . ?
C17 C16 C21 C20 2.6(3) . . . . ?
C5 C16 C21 C20 -174.13(19) . . . . ?
C19 C20 C21 C16 -1.4(3) . . . . ?
C25 C20 C21 C16 179.1(2) . . . . ?
C19 C20 C21 C22 179.8(2) . . . . ?
C25 C20 C21 C22 0.3(3) . . . . ?
C16 C21 C22 C23 -179.5(2) . . . . ?
C20 C21 C22 C23 -0.8(3) . . . . ?
C21 C22 C23 C24 1.0(4) . . . . ?
C22 C23 C24 C25 -0.8(4) . . . . ?
C23 C24 C25 C20 0.3(4) . . . . ?
C19 C20 C25 C24 -179.6(2) . . . . ?
C21 C20 C25 C24 -0.1(3) . . . . ?
C16 C17 C26 C27 179.9(2) . . . . ?
C18 C17 C26 C27 1.2(3) . . . . ?
C17 C26 C27 C28 0.4(4) . . . . ?
C26 C27 C28 C29 -1.6(4) . . . . ?
C27 C28 C29 C18 1.2(4) . . . . ?
C19 C18 C29 C28 -178.4(2) . . . . ?
C17 C18 C29 C28 0.4(4) . . . . ?
C18 C19 C30 O4 -77.1(3) . . . . ?
C20 C19 C30 O4 103.7(3) . . . . ?
C18 C19 C30 O3 102.2(2) . . . . ?
C20 C19 C30 O3 -77.1(3) . . . . ?
O6 C31 C32 C37 65.4(4) . . . . ?
O5 C31 C32 C37 -112.1(3) . . . . ?
O6 C31 C32 C33 -112.7(4) . . . . ?
O5 C31 C32 C33 69.8(3) . . . . ?
C37 C32 C33 C42 -178.9(2) . . . . ?
C31 C32 C33 C42 -0.9(3) . . . . ?
C37 C32 C33 C34 -0.3(3) . . . . ?
C31 C32 C33 C34 177.7(2) . . . . ?
C32 C33 C34 C35 0.3(3) . . . . ?
C42 C33 C34 C35 179.0(2) . . . . ?
C32 C33 C34 C45 -179.9(2) . . . . ?
C42 C33 C34 C45 -1.3(3) . . . . ?
C45 C34 C35 C36 -179.5(2) . . . . ?
C33 C34 C35 C36 0.2(3) . . . . ?
C45 C34 C35 C46 -0.5(3) . . . . ?
C33 C34 C35 C46 179.18(19) . . . . ?
C34 C35 C36 C41 179.1(2) . . . . ?
C46 C35 C36 C41 0.1(3) . . . . ?
C34 C35 C36 C37 -0.7(3) . . . . ?
C46 C35 C36 C37 -179.72(19) . . . . ?
C33 C32 C37 C38 179.1(2) . . . . ?
C31 C32 C37 C38 1.0(3) . . . . ?
C33 C32 C37 C36 -0.2(3) . . . . ?
C31 C32 C37 C36 -178.3(2) . . . . ?
C35 C36 C37 C32 0.8(3) . . . . ?
C41 C36 C37 C32 -179.1(2) . . . . ?
C35 C36 C37 C38 -178.6(2) . . . . ?
C41 C36 C37 C38 1.6(3) . . . . ?
C32 C37 C38 C39 -179.6(3) . . . . ?
C36 C37 C38 C39 -0.3(4) . . . . ?
C37 C38 C39 C40 -1.7(4) . . . . ?
C38 C39 C40 C41 2.4(5) . . . . ?
C39 C40 C41 C36 -1.1(4) . . . . ?
C35 C36 C41 C40 179.2(2) . . . . ?
C37 C36 C41 C40 -0.9(4) . . . . ?
C32 C33 C42 C43 178.5(2) . . . . ?
C34 C33 C42 C43 -0.1(4) . . . . ?
C33 C42 C43 C44 1.6(4) . . . . ?
C42 C43 C44 C45 -1.7(4) . . . . ?
C43 C44 C45 C34 0.3(4) . . . . ?
C35 C34 C45 C44 -179.1(2) . . . . ?
C33 C34 C45 C44 1.2(3) . . . . ?
C36 C35 C46 C51 87.4(3) . . . . ?
C34 C35 C46 C51 -91.6(3) . . . . ?
C36 C35 C46 C47 -93.1(2) . . . . ?
C34 C35 C46 C47 87.9(3) . . . . ?
C51 C46 C47 C56 179.6(2) . . . . ?
C35 C46 C47 C56 0.1(3) . . . . ?
C51 C46 C47 C48 -0.5(3) . . . . ?
C35 C46 C47 C48 -179.99(18) . . . . ?
C46 C47 C48 C49 0.5(3) . . . . ?
C56 C47 C48 C49 -179.53(19) . . . . ?
C46 C47 C48 C59 179.05(19) . . . . ?
C56 C47 C48 C59 -1.0(3) . . . . ?
C59 C48 C49 C50 -178.5(2) . . . . ?
C47 C48 C49 C50 0.0(3) . . . . ?
C59 C48 C49 C60 3.0(3) . . . . ?
C47 C48 C49 C60 -178.57(19) . . . . ?
C48 C49 C50 C55 -179.6(2) . . . . ?
C60 C49 C50 C55 -1.0(3) . . . . ?
C48 C49 C50 C51 -0.5(3) . . . . ?
C60 C49 C50 C51 178.07(19) . . . . ?
C47 C46 C51 C52 179.9(2) . . . . ?
C35 C46 C51 C52 -0.6(3) . . . . ?
C47 C46 C51 C50 0.0(3) . . . . ?
C35 C46 C51 C50 179.46(19) . . . . ?
C49 C50 C51 C46 0.5(3) . . . . ?
C55 C50 C51 C46 179.7(2) . . . . ?
C49 C50 C51 C52 -179.40(19) . . . . ?
C55 C50 C51 C52 -0.2(3) . . . . ?
C46 C51 C52 C53 -179.6(2) . . . . ?
C50 C51 C52 C53 0.4(3) . . . . ?
C51 C52 C53 C54 0.0(4) . . . . ?
C52 C53 C54 C55 -0.6(4) . . . . ?
C53 C54 C55 C50 0.7(4) . . . . ?
C49 C50 C55 C54 178.9(2) . . . . ?
C51 C50 C55 C54 -0.3(3) . . . . ?
C46 C47 C56 C57 -179.0(2) . . . . ?
C48 C47 C56 C57 1.1(3) . . . . ?
C47 C56 C57 C58 -0.1(3) . . . . ?
C56 C57 C58 C59 -1.0(4) . . . . ?
C57 C58 C59 C48 1.0(4) . . . . ?
C49 C48 C59 C58 178.5(2) . . . . ?
C47 C48 C59 C58 0.0(3) . . . . ?
C48 C49 C60 O8 -107.4(3) . . . . ?
C50 C49 C60 O8 74.0(3) . . . . ?
C48 C49 C60 O7 72.8(3) . . . . ?
C50 C49 C60 O7 -105.8(2) . . . . ?
C64 O9 C61 C62 -21.3(4) . . . . ?
O9 C61 C62 C63 29.8(3) . . . . ?
C61 C62 C63 C64 -27.4(4) . . . . ?
C61 O9 C64 C63 3.9(4) . . . . ?
C62 C63 C64 O9 15.6(4) . . . . ?
C68 O10 C65 C66 20.3(4) . . . . ?
O10 C65 C66 C67 -33.0(5) . . . . ?
C65 C66 C67 C68 32.2(6) . . . . ?
C65 O10 C68 C67 1.4(5) . . . . ?
C66 C67 C68 O10 -21.1(5) . . . . ?
C72 O11 C69 C70 -40.8(3) . . . . ?
O11 C69 C70 C71 29.9(4) . . . . ?
C69 C70 C71 C72 -8.5(4) . . . . ?
C69 O11 C72 C71 35.2(4) . . . . ?
C70 C71 C72 O11 -15.6(4) . . . . ?
C76 O12 C73 C74 22.2(5) . . . . ?
O12 C73 C74 C75 -8.8(6) . . . . ?
C73 C74 C75 C76 -7.0(6) . . . . ?
C73 O12 C76 C75 -26.9(6) . . . . ?
C74 C75 C76 O12 20.8(7) . . . . ?
C80 O13 C77 C78 -3.3(4) . . . . ?
O13 C77 C78 C79 24.5(4) . . . . ?
C77 C78 C79 C80 -36.1(4) . . . . ?
C77 O13 C80 C79 -19.9(4) . . . . ?
C78 C79 C80 O13 34.7(4) . . . . ?

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
O1 H1 O14 0.84 1.73 2.558(2) 169.6 2_656 yes
O3 H3 O9 0.84 1.76 2.597(2) 174.5 2_566 yes
O5 H5 O10 0.84 1.81 2.639(3) 169.5 2_656 yes
O7 H7 O13 0.84 1.74 2.552(2) 163.5 2_567 yes
C68 H68A O6 0.99 2.51 3.183(4) 125.0 2_656 yes
C79 H79B O12 0.99 2.48 3.308(5) 140.3 . yes
O14 H14A O11 0.90(4) 1.83(4) 2.724(3) 171(3) . yes
O14 H14B O2 0.84(4) 1.97(4) 2.776(2) 161(3) 1_556 yes

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mfu327-1b
_database_code_depnum_ccdc_archive 'CCDC 1952758'
loop_
_audit_author_name
_audit_author_address
'Misaki Okayasu'
;Toho University
Japan
;
_audit_update_record             
;
2019-09-11 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C28 H17 N O2'
_chemical_formula_moiety         'C28 H17 N O2'
_chemical_formula_weight         399.45
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
_space_group_IT_number           60
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2-Y,1/2+Z
3 1/2+X,1/2-Y,-Z
4 -X,+Y,1/2-Z
5 -X,-Y,-Z
6 -1/2+X,-1/2+Y,-1/2-Z
7 -1/2-X,-1/2+Y,+Z
8 +X,-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   11.97202(19)
_cell_length_b                   12.27700(18)
_cell_length_c                   12.64035(17)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     1857.88(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10777
_cell_measurement_theta_min      3.48
_cell_measurement_theta_max      73.29
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832.00
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_T_max  0.979

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            21955
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_theta_max         68.239
_diffrn_reflns_theta_min         5.160
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             1700
_reflns_number_gt                1537
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1307
_refine_ls_wR_factor_gt          0.1270
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         1700
_refine_ls_number_parameters     166
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0917P)²+0.2113P] 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_diff_density_max         0.26
_refine_diff_density_min         -0.36
_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 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
O1 O 0.53679(13) 0.62097(13) 0.62626(14) 0.0471(5) Uani 0.5 1 d . . P A 1
C1 C 0.76024(10) 0.87277(8) 0.57405(9) 0.0417(3) Uani 1 1 d . . . . .
H1 H 0.720537 0.927699 0.536787 0.050 Uiso 1 1 calc R U . . .
C2 C 0.70329(10) 0.79371(9) 0.62560(9) 0.0402(3) Uani 1 1 d . . . . .
H2 H 0.623969 0.793578 0.623623 0.048 Uiso 1 1 calc R U . . .
C3 C 0.76062(9) 0.71040(8) 0.68298(8) 0.0344(3) Uani 1 1 d . . . . .
C4 C 0.7024(17) 0.6424(11) 0.7294(17) 0.0280(17) Uani 0.5 1 d . . P A 1
N1 N 0.7019(13) 0.6195(8) 0.7366(13) 0.0247(15) Uani 0.5 1 d . . P A 2
C5 C 0.75685(9) 0.55197(8) 0.79163(8) 0.0331(3) Uani 1 1 d . . . . .
C6 C 0.69659(9) 0.46566(9) 0.84135(9) 0.0369(3) Uani 1 1 d . . . . .
H6 H 0.617549 0.463169 0.835217 0.044 Uiso 1 1 calc R U . . .
C7 C 0.75031(10) 0.38707(9) 0.89725(9) 0.0395(3) Uani 1 1 d . . . . .
H7 H 0.708684 0.329775 0.928827 0.047 Uiso 1 1 calc R U . . .
C8 C 0.86825(10) 0.38989(9) 0.90886(9) 0.0396(3) Uani 1 1 d . . . . .
H8 H 0.904911 0.334782 0.948590 0.048 Uiso 1 1 calc R U . . .
C9 C 0.92921(9) 0.47114(8) 0.86339(8) 0.0364(3) Uani 1 1 d . . . . .
H9 H 1.007876 0.472867 0.873087 0.044 Uiso 1 1 calc R U . . .
C10 C 0.87653(8) 0.55375(8) 0.80135(8) 0.0329(3) Uani 1 1 d . . . . .
C11 C 0.93743(8) 0.63479(8) 0.74738(8) 0.0324(3) Uani 1 1 d . . . . .
C12 C 0.88072(8) 0.71383(8) 0.68756(8) 0.0329(3) Uani 1 1 d . . . . .
C13 C 0.93676(9) 0.79745(8) 0.62996(8) 0.0357(3) Uani 1 1 d . . . . .
H13 H 1.016085 0.799451 0.629880 0.043 Uiso 1 1 calc R U . . .
C14 C 0.87906(10) 0.87432(9) 0.57519(9) 0.0400(3) Uani 1 1 d . . . . .
H14 H 0.918233 0.929305 0.537509 0.048 Uiso 1 1 calc R U . . .
C15 C 0.5762(3) 0.6265(2) 0.71310(18) 0.0382(6) Uani 0.5 1 d . . P A 1
O2 O 0.51729(13) 0.62901(13) 0.80189(13) 0.0426(4) Uani 0.5 1 d . . P A 1
H17 H 0.415(4) 0.625(3) 0.755(3) 0.051 Uiso 0.5 1 d . U P B 2


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 O2 1.120(2) 4_656 ?
O1 C15 1.197(3) . ?
C1 C2 1.3533(16) . ?
C1 C14 1.4228(17) . ?
C1 H1 0.9500 . ?
C2 C3 1.4294(15) . ?
C2 H2 0.9500 . ?
C3 C4 1.236(17) . ?
C3 C12 1.4396(15) . ?
C3 N1 1.483(12) . ?
C4 C5 1.509(15) . ?
C4 C15 1.54(2) . ?
N1 C5 1.267(13) . ?
C5 C6 1.4276(14) . ?
C5 C10 1.4382(15) . ?
C6 C7 1.3579(15) . ?
C6 H6 0.9500 . ?
C7 C8 1.4199(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.3632(15) . ?
C8 H8 0.9500 . ?
C9 C10 1.4287(14) . ?
C9 H9 0.9500 . ?
C10 C11 1.4096(14) . ?
C11 C12 1.4051(14) . ?
C11 C11 1.500(2) 4_756 ?
C12 C13 1.4262(14) . ?
C13 C14 1.3591(15) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 O2 1.135(3) 4_656 ?
C15 O2 1.326(4) . ?
O2 O2 1.376(3) 4_656 ?

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
O2 O1 C15 58.58(19) 4_656 . ?
C2 C1 C14 120.55(10) . . ?
C2 C1 H1 119.7 . . ?
C14 C1 H1 119.7 . . ?
C1 C2 C3 121.04(11) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C4 C3 C2 117.0(9) . . ?
C4 C3 C12 124.4(9) . . ?
C2 C3 C12 118.62(9) . . ?
C2 C3 N1 122.9(6) . . ?
C12 C3 N1 118.5(6) . . ?
C3 C4 C5 120.0(15) . . ?
C3 C4 C15 125.2(12) . . ?
C5 C4 C15 113.7(10) . . ?
C5 N1 C3 119.8(12) . . ?
N1 C5 C6 117.7(7) . . ?
N1 C5 C10 123.7(7) . . ?
C6 C5 C10 118.50(9) . . ?
C6 C5 C4 123.8(7) . . ?
C10 C5 C4 117.7(8) . . ?
C7 C6 C5 121.14(10) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C8 120.49(10) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 120.44(10) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 120.97(10) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 122.57(10) . . ?
C11 C10 C5 118.99(9) . . ?
C9 C10 C5 118.41(9) . . ?
C12 C11 C10 119.87(10) . . ?
C12 C11 C11 120.43(8) . 4_756 ?
C10 C11 C11 119.70(8) . 4_756 ?
C11 C12 C13 122.99(10) . . ?
C11 C12 C3 118.95(9) . . ?
C13 C12 C3 118.06(9) . . ?
C14 C13 C12 121.38(10) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C13 C14 C1 120.27(10) . . ?
C13 C14 H14 119.9 . . ?
C1 C14 H14 119.9 . . ?
O2 C15 O1 57.32(17) 4_656 . ?
O2 C15 O2 67.46(19) 4_656 . ?
O1 C15 O2 124.6(3) . . ?
O2 C15 C4 171.0(5) 4_656 . ?
O1 C15 C4 121.1(8) . . ?
O2 C15 C4 114.0(8) . . ?
O1 O2 C15 64.10(16) 4_656 4_656 ?
O1 O2 C15 172.8(2) 4_656 . ?
C15 O2 C15 112.47(19) 4_656 . ?
O1 O2 O2 126.8(2) 4_656 4_656 ?
C15 O2 O2 62.89(16) 4_656 4_656 ?
C15 O2 O2 49.66(14) . 4_656 ?

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
C14 C1 C2 C3 0.45(16) . . . . ?
C1 C2 C3 C4 178.8(11) . . . . ?
C1 C2 C3 C12 1.77(15) . . . . ?
C1 C2 C3 N1 -177.2(8) . . . . ?
C2 C3 C4 C5 -180.0(10) . . . . ?
C12 C3 C4 C5 -3(2) . . . . ?
C2 C3 C4 C15 13(2) . . . . ?
C12 C3 C4 C15 -170.6(10) . . . . ?
C2 C3 N1 C5 -175.7(8) . . . . ?
C12 C3 N1 C5 5.3(15) . . . . ?
C3 N1 C5 C6 -179.7(8) . . . . ?
C3 N1 C5 C10 -3.6(16) . . . . ?
C3 C4 C5 C6 -175.4(10) . . . . ?
C15 C4 C5 C6 -6.6(18) . . . . ?
C3 C4 C5 C10 5(2) . . . . ?
C15 C4 C5 C10 173.6(8) . . . . ?
N1 C5 C6 C7 176.7(8) . . . . ?
C10 C5 C6 C7 0.41(15) . . . . ?
C4 C5 C6 C7 -179.4(10) . . . . ?
C5 C6 C7 C8 0.93(16) . . . . ?
C6 C7 C8 C9 -0.47(16) . . . . ?
C7 C8 C9 C10 -1.35(16) . . . . ?
C8 C9 C10 C11 -175.69(10) . . . . ?
C8 C9 C10 C5 2.63(15) . . . . ?
N1 C5 C10 C11 0.1(9) . . . . ?
C6 C5 C10 C11 176.24(9) . . . . ?
C4 C5 C10 C11 -4.0(9) . . . . ?
N1 C5 C10 C9 -178.2(9) . . . . ?
C6 C5 C10 C9 -2.14(13) . . . . ?
C4 C5 C10 C9 177.7(9) . . . . ?
C9 C10 C11 C12 179.97(9) . . . . ?
C5 C10 C11 C12 1.66(14) . . . . ?
C9 C10 C11 C11 1.09(16) . . . 4_756 ?
C5 C10 C11 C11 -177.22(9) . . . 4_756 ?
C10 C11 C12 C13 -179.27(9) . . . . ?
C11 C11 C12 C13 -0.40(16) 4_756 . . . ?
C10 C11 C12 C3 0.19(14) . . . . ?
C11 C11 C12 C3 179.06(9) 4_756 . . . ?
C4 C3 C12 C11 0.7(12) . . . . ?
C2 C3 C12 C11 177.43(9) . . . . ?
N1 C3 C12 C11 -3.5(7) . . . . ?
C4 C3 C12 C13 -179.9(12) . . . . ?
C2 C3 C12 C13 -3.08(13) . . . . ?
N1 C3 C12 C13 176.0(7) . . . . ?
C11 C12 C13 C14 -178.24(10) . . . . ?
C3 C12 C13 C14 2.31(15) . . . . ?
C12 C13 C14 C1 -0.12(16) . . . . ?
C2 C1 C14 C13 -1.32(16) . . . . ?
O2 O1 C15 O2 4.6(2) 4_656 . . . ?
O2 O1 C15 C4 -169.6(7) 4_656 . . . ?
C3 C4 C15 O1 47.5(19) . . . . ?
C5 C4 C15 O1 -120.6(11) . . . . ?
C3 C4 C15 O2 -127.2(16) . . . . ?
C5 C4 C15 O2 64.6(14) . . . . ?
O2 C15 O2 C15 3.3(4) 4_656 . . 4_656 ?
O1 C15 O2 C15 -0.9(5) . . . 4_656 ?
C4 C15 O2 C15 173.7(6) . . . 4_656 ?
O1 C15 O2 O2 -4.18(18) . . . 4_656 ?
C4 C15 O2 O2 170.3(6) . . . 4_656 ?

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
C2 H2 O1^a 0.95 2.36 2.911(2) 116.3 . yes

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mfu284-2a
_database_code_depnum_ccdc_archive 'CCDC 1952762'
loop_
_audit_author_name
_audit_author_address
'Misaki Okayasu'
;Toho University
Japan
;
_audit_update_record             
;
2019-11-16 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C42 H42 N4 O11'
_chemical_formula_moiety         'C42 H42 N4 O11'
_chemical_formula_weight         778.81
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
_space_group_IT_number           9
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 +X,-Y,1/2+Z
3 1/2+X,1/2+Y,+Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   10.2344(8)
_cell_length_b                   33.477(2)
_cell_length_c                   11.5077(10)
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.536(7)
_cell_angle_gamma                90.0000
_cell_volume                     3935.2(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3355
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      26.24
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640.00
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.289
_exptl_absorpt_correction_T_max  0.998

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            31178
_diffrn_reflns_av_unetI/netI     0.1591
_diffrn_reflns_av_R_equivalents  0.1157
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.656
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             8740
_reflns_number_gt                4291
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_max     0.934
_reflns_Friedel_fraction_full    0.957

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.2056
_refine_ls_R_factor_gt           0.1064
_refine_ls_wR_factor_ref         0.2994
_refine_ls_wR_factor_gt          0.2472
_refine_ls_number_restraints     2
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         8740
_refine_ls_number_parameters     517
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1686P)²] 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_diff_density_max         0.55
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined using 1403 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(10)

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
O1 O 0.4283(7) 0.42609(19) 0.5158(7) 0.054(2) Uani 1 1 d . . . . .
H1A H 0.415(12) 0.482(4) 0.532(10) 0.065 Uiso 1 1 d . U . . .
O2 O 0.2317(8) 0.4218(2) 0.5832(7) 0.057(2) Uani 1 1 d . . . . .
O3 O 0.3723(7) 0.09479(19) 0.6749(6) 0.0467(17) Uani 1 1 d . . . . .
O4 O 0.3222(8) 0.08035(19) 0.4915(6) 0.0499(19) Uani 1 1 d . . . . .
H4A H 0.328159 0.056983 0.517970 0.075 Uiso 1 1 calc R U . . .
O5 O 0.5970(8) 0.4094(2) 0.3480(7) 0.064(2) Uani 1 1 d . . . . .
O6 O 0.3222(9) 0.0831(2) 0.2570(7) 0.068(2) Uani 1 1 d . . . . .
O7 O 0.1189(13) 0.0375(3) 0.1824(12) 0.123(5) Uani 1 1 d . . . . .
O8 O 0.2412(12) -0.0304(3) 0.2653(10) 0.097(3) Uani 1 1 d . . . . .
O9 O 0.3681(13) -0.0011(2) 0.4834(8) 0.107(4) Uani 1 1 d . . . . .
O10 O 0.5189(8) -0.0364(2) 0.6579(8) 0.062(2) Uani 1 1 d . . . . .
O11 O 0.5828(12) 0.0438(3) 0.7367(13) 0.131(5) Uani 1 1 d . . . . .
N1 N 0.3786(9) 0.5040(2) 0.5060(8) 0.046(2) Uani 1 1 d . . . . .
N2 N 0.3585(13) 0.5760(3) 0.4485(11) 0.073(3) Uani 1 1 d . . . . .
N3 N 0.7815(9) 0.3600(2) 0.4417(8) 0.048(2) Uani 1 1 d . . . . .
N4 N 0.9180(8) 0.3144(2) 0.5767(7) 0.042(2) Uani 1 1 d . . . . .
C1 C 0.1771(8) 0.3463(3) 0.2405(8) 0.031(2) Uani 1 1 d . . . . .
H1 H 0.135199 0.361578 0.179382 0.037 Uiso 1 1 calc R U . . .
C2 C 0.2264(8) 0.3646(3) 0.3366(9) 0.036(2) Uani 1 1 d . . . . .
H2 H 0.220002 0.392829 0.341584 0.043 Uiso 1 1 calc R U . . .
C3 C 0.2876(8) 0.3434(3) 0.4311(8) 0.031(2) Uani 1 1 d . . . . .
C4 C 0.3368(9) 0.3618(2) 0.5333(8) 0.0287(19) Uani 1 1 d . . . . .
C5 C 0.3947(9) 0.3398(2) 0.6232(9) 0.032(2) Uani 1 1 d . . . . .
C6 C 0.4492(10) 0.3581(3) 0.7279(8) 0.036(2) Uani 1 1 d . . . . .
H6 H 0.445032 0.386380 0.734066 0.043 Uiso 1 1 calc R U . . .
C7 C 0.5052(10) 0.3379(3) 0.8165(9) 0.044(3) Uani 1 1 d . . . . .
H7 H 0.544084 0.351488 0.882359 0.053 Uiso 1 1 calc R U . . .
C8 C 0.5060(9) 0.2962(3) 0.8114(8) 0.036(2) Uani 1 1 d . . . . .
H8 H 0.542675 0.281164 0.875417 0.043 Uiso 1 1 calc R U . . .
C9 C 0.4542(8) 0.2772(3) 0.7146(8) 0.030(2) Uani 1 1 d . . . . .
H9 H 0.456652 0.248827 0.713812 0.036 Uiso 1 1 calc R U . . .
C10 C 0.3974(8) 0.2967(2) 0.6157(8) 0.0263(19) Uani 1 1 d . . . . .
C11 C 0.3449(8) 0.2776(2) 0.5162(7) 0.0228(17) Uani 1 1 d . . . . .
C12 C 0.2912(8) 0.2999(2) 0.4212(7) 0.0237(18) Uani 1 1 d . . . . .
C13 C 0.2425(8) 0.2815(3) 0.3174(8) 0.032(2) Uani 1 1 d . . . . .
H13 H 0.248450 0.253347 0.309506 0.038 Uiso 1 1 calc R U . . .
C14 C 0.1872(8) 0.3035(3) 0.2288(8) 0.036(2) Uani 1 1 d . . . . .
H14 H 0.155063 0.290841 0.158924 0.044 Uiso 1 1 calc R U . . .
C15 C 0.3314(11) 0.4063(3) 0.5462(8) 0.038(2) Uani 1 1 d . . . . .
C16 C 0.3417(8) 0.2325(2) 0.5144(7) 0.0232(17) Uani 1 1 d . . . . .
C17 C 0.4411(8) 0.2103(2) 0.4725(8) 0.0270(19) Uani 1 1 d . . . . .
C18 C 0.5501(9) 0.2284(3) 0.4185(8) 0.034(2) Uani 1 1 d . . . . .
H18 H 0.551693 0.256635 0.409311 0.041 Uiso 1 1 calc R U . . .
C19 C 0.6493(9) 0.2067(3) 0.3810(8) 0.039(2) Uani 1 1 d . . . . .
H19 H 0.720708 0.219543 0.347261 0.047 Uiso 1 1 calc R U . . .
C20 C 0.6469(11) 0.1634(3) 0.3922(9) 0.048(3) Uani 1 1 d . . . . .
H20 H 0.715105 0.147843 0.362858 0.058 Uiso 1 1 calc R U . . .
C21 C 0.5478(10) 0.1452(3) 0.4443(9) 0.046(3) Uani 1 1 d . . . . .
H21 H 0.549048 0.116947 0.452706 0.056 Uiso 1 1 calc R U . . .
C22 C 0.4425(9) 0.1672(2) 0.4865(8) 0.030(2) Uani 1 1 d . . . . .
C23 C 0.3416(9) 0.1485(2) 0.5439(8) 0.033(2) Uani 1 1 d . . . . .
C24 C 0.2350(9) 0.1713(2) 0.5815(8) 0.0279(19) Uani 1 1 d . . . . .
C25 C 0.1296(9) 0.1534(3) 0.6329(8) 0.034(2) Uani 1 1 d . . . . .
H25 H 0.129043 0.125179 0.642608 0.040 Uiso 1 1 calc R U . . .
C26 C 0.0279(9) 0.1752(3) 0.6694(8) 0.032(2) Uani 1 1 d . . . . .
H26 H -0.043393 0.162306 0.702965 0.038 Uiso 1 1 calc R U . . .
C27 C 0.0286(8) 0.2164(3) 0.6574(8) 0.032(2) Uani 1 1 d . . . . .
H27 H -0.043030 0.231595 0.682224 0.038 Uiso 1 1 calc R U . . .
C28 C 0.1311(7) 0.2357(3) 0.6102(6) 0.0239(18) Uani 1 1 d . . . . .
H28 H 0.132186 0.264050 0.606571 0.029 Uiso 1 1 calc R U . . .
C29 C 0.2356(8) 0.2134(2) 0.5666(8) 0.0258(18) Uani 1 1 d . . . . .
C30 C 0.3466(9) 0.1044(3) 0.5708(9) 0.036(2) Uani 1 1 d . . . . .
C31 C 0.2629(12) 0.5097(3) 0.4249(11) 0.058(3) Uani 1 1 d . . . . .
H31A H 0.181515 0.505171 0.465303 0.070 Uiso 1 1 calc R U . . .
H31B H 0.264852 0.490830 0.358890 0.070 Uiso 1 1 calc R U . . .
C32 C 0.2684(15) 0.5515(5) 0.3828(13) 0.089(5) Uani 1 1 d . . . . .
H32A H 0.292444 0.551287 0.300789 0.107 Uiso 1 1 calc R U . . .
H32B H 0.180038 0.563455 0.384505 0.107 Uiso 1 1 calc R U . . .
C33 C 0.3623(15) 0.5252(4) 0.6112(10) 0.077(4) Uani 1 1 d . . . . .
H33A H 0.441987 0.523189 0.664226 0.092 Uiso 1 1 calc R U . . .
H33B H 0.286976 0.514591 0.651499 0.092 Uiso 1 1 calc R U . . .
C34 C 0.336(2) 0.5712(4) 0.5716(14) 0.099(5) Uani 1 1 d . . . . .
H34A H 0.245010 0.578695 0.585649 0.119 Uiso 1 1 calc R U . . .
H34B H 0.395695 0.589071 0.618576 0.119 Uiso 1 1 calc R U . . .
C35 C 0.5005(13) 0.5175(4) 0.4486(13) 0.068(4) Uani 1 1 d . . . . .
H35A H 0.579906 0.510720 0.498166 0.082 Uiso 1 1 calc R U . . .
H35B H 0.506111 0.504293 0.372118 0.082 Uiso 1 1 calc R U . . .
C36 C 0.4895(18) 0.5614(5) 0.4337(19) 0.108(6) Uani 1 1 d . . . . .
H36A H 0.551126 0.574615 0.491118 0.129 Uiso 1 1 calc R U . . .
H36B H 0.515318 0.568607 0.354940 0.129 Uiso 1 1 calc R U . . .
C37 C 0.8310(11) 0.3246(3) 0.3753(9) 0.043(2) Uani 1 1 d . . . . .
H37A H 0.756126 0.308619 0.342292 0.052 Uiso 1 1 calc R U . . .
H37B H 0.882124 0.333972 0.310395 0.052 Uiso 1 1 calc R U . . .
C38 C 0.9161(11) 0.2992(3) 0.4576(9) 0.047(3) Uani 1 1 d . . . . .
H38A H 0.882806 0.271417 0.455785 0.056 Uiso 1 1 calc R U . . .
H38B H 1.006473 0.298810 0.431422 0.056 Uiso 1 1 calc R U . . .
C39 C 0.9019(10) 0.3808(3) 0.4894(9) 0.045(3) Uani 1 1 d . . . . .
H39A H 0.959364 0.386660 0.425371 0.054 Uiso 1 1 calc R U . . .
H39B H 0.877658 0.406440 0.524963 0.054 Uiso 1 1 calc R U . . .
C40 C 0.9738(12) 0.3555(3) 0.5785(10) 0.055(3) Uani 1 1 d . . . . .
H40A H 1.067589 0.354274 0.562225 0.066 Uiso 1 1 calc R U . . .
H40B H 0.966951 0.367388 0.656600 0.066 Uiso 1 1 calc R U . . .
C41 C 0.7030(11) 0.3463(3) 0.5381(11) 0.060(3) Uani 1 1 d . . . . .
H41A H 0.622724 0.332630 0.506580 0.072 Uiso 1 1 calc R U . . .
H41B H 0.676892 0.369462 0.585015 0.072 Uiso 1 1 calc R U . . .
C42 C 0.7872(12) 0.3177(3) 0.6135(11) 0.057(3) Uani 1 1 d . . . . .
H42A H 0.790620 0.327026 0.695235 0.068 Uiso 1 1 calc R U . . .
H42B H 0.745975 0.290903 0.610819 0.068 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C15 1.259(12) . ?
O2 C15 1.243(12) . ?
O3 C30 1.252(12) . ?
O4 C30 1.229(11) . ?
O4 H4A 0.8400 . ?
N1 C33 1.423(15) . ?
N1 C31 1.475(15) . ?
N1 C35 1.516(15) . ?
N1 H1A 0.87(12) . ?
N2 C32 1.417(19) . ?
N2 C36 1.45(2) . ?
N2 C34 1.46(2) . ?
N3 C41 1.481(14) . ?
N3 C39 1.491(13) . ?
N3 C37 1.514(13) . ?
N4 C42 1.432(14) . ?
N4 C38 1.462(13) . ?
N4 C40 1.488(13) . ?
C1 C2 1.335(13) . ?
C1 C14 1.442(13) . ?
C1 H1 0.9500 . ?
C2 C3 1.412(13) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(13) . ?
C3 C12 1.461(12) . ?
C4 C5 1.374(13) . ?
C4 C15 1.500(12) . ?
C5 C6 1.433(14) . ?
C5 C10 1.446(11) . ?
C6 C7 1.325(14) . ?
C6 H6 0.9500 . ?
C7 C8 1.396(14) . ?
C7 H7 0.9500 . ?
C8 C9 1.362(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.407(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.391(12) . ?
C11 C12 1.407(12) . ?
C11 C16 1.511(10) . ?
C12 C13 1.407(12) . ?
C13 C14 1.354(12) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C16 C17 1.371(11) . ?
C16 C29 1.425(11) . ?
C17 C18 1.443(12) . ?
C17 C22 1.454(12) . ?
C18 C19 1.341(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.457(15) . ?
C19 H19 0.9500 . ?
C20 C21 1.354(15) . ?
C20 H20 0.9500 . ?
C21 C22 1.416(13) . ?
C21 H21 0.9500 . ?
C22 C23 1.407(12) . ?
C23 C24 1.422(12) . ?
C23 C30 1.509(13) . ?
C24 C25 1.398(12) . ?
C24 C29 1.420(12) . ?
C25 C26 1.360(13) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(12) . ?
C26 H26 0.9500 . ?
C27 C28 1.371(11) . ?
C27 H27 0.9500 . ?
C28 C29 1.420(11) . ?
C28 H28 0.9500 . ?
C31 C32 1.48(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.62(2) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.481(19) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.508(15) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.489(16) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.525(17) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?

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
C30 O4 H4A 109.5 . . ?
C33 N1 C31 110.0(9) . . ?
C33 N1 C35 111.4(10) . . ?
C31 N1 C35 109.6(9) . . ?
C33 N1 H1A 102(8) . . ?
C31 N1 H1A 129(8) . . ?
C35 N1 H1A 93(8) . . ?
C32 N2 C36 108.6(12) . . ?
C32 N2 C34 108.6(12) . . ?
C36 N2 C34 106.2(14) . . ?
C41 N3 C39 110.1(9) . . ?
C41 N3 C37 110.5(8) . . ?
C39 N3 C37 104.9(8) . . ?
C42 N4 C38 110.2(9) . . ?
C42 N4 C40 106.9(8) . . ?
C38 N4 C40 108.5(8) . . ?
C2 C1 C14 120.4(8) . . ?
C2 C1 H1 119.8 . . ?
C14 C1 H1 119.8 . . ?
C1 C2 C3 122.3(8) . . ?
C1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C4 C3 C2 123.2(8) . . ?
C4 C3 C12 119.8(7) . . ?
C2 C3 C12 116.9(8) . . ?
C5 C4 C3 121.1(7) . . ?
C5 C4 C15 118.3(8) . . ?
C3 C4 C15 120.6(8) . . ?
C4 C5 C6 122.2(8) . . ?
C4 C5 C10 119.8(8) . . ?
C6 C5 C10 117.9(8) . . ?
C7 C6 C5 123.8(8) . . ?
C7 C6 H6 118.1 . . ?
C5 C6 H6 118.1 . . ?
C6 C7 C8 118.8(9) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C9 C8 C7 119.9(9) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 124.4(8) . . ?
C8 C9 H9 117.8 . . ?
C10 C9 H9 117.8 . . ?
C11 C10 C9 124.9(7) . . ?
C11 C10 C5 120.0(8) . . ?
C9 C10 C5 115.1(8) . . ?
C10 C11 C12 120.6(7) . . ?
C10 C11 C16 118.5(7) . . ?
C12 C11 C16 120.8(8) . . ?
C13 C12 C11 121.9(7) . . ?
C13 C12 C3 119.6(7) . . ?
C11 C12 C3 118.5(7) . . ?
C14 C13 C12 120.7(8) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C1 119.9(9) . . ?
C13 C14 H14 120.0 . . ?
C1 C14 H14 120.0 . . ?
O2 C15 O1 123.6(8) . . ?
O2 C15 C4 119.0(9) . . ?
O1 C15 C4 117.4(9) . . ?
C17 C16 C29 120.5(7) . . ?
C17 C16 C11 122.0(7) . . ?
C29 C16 C11 117.3(7) . . ?
C16 C17 C18 122.3(8) . . ?
C16 C17 C22 120.1(7) . . ?
C18 C17 C22 117.5(7) . . ?
C19 C18 C17 122.1(8) . . ?
C19 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
C18 C19 C20 119.5(8) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C21 C20 C19 120.4(9) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C22 121.6(9) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
C23 C22 C21 121.7(8) . . ?
C23 C22 C17 119.5(7) . . ?
C21 C22 C17 118.8(8) . . ?
C22 C23 C24 120.2(7) . . ?
C22 C23 C30 121.0(8) . . ?
C24 C23 C30 118.8(8) . . ?
C25 C24 C29 119.2(8) . . ?
C25 C24 C23 121.6(8) . . ?
C29 C24 C23 119.2(8) . . ?
C26 C25 C24 121.6(8) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C25 C26 C27 119.7(8) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
C28 C27 C26 121.1(8) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 120.3(8) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C24 C29 C28 118.0(7) . . ?
C24 C29 C16 120.4(7) . . ?
C28 C29 C16 121.6(7) . . ?
O4 C30 O3 124.3(9) . . ?
O4 C30 C23 119.0(9) . . ?
O3 C30 C23 116.7(8) . . ?
N1 C31 C32 106.5(10) . . ?
N1 C31 H31A 110.4 . . ?
C32 C31 H31A 110.4 . . ?
N1 C31 H31B 110.4 . . ?
C32 C31 H31B 110.4 . . ?
H31A C31 H31B 108.6 . . ?
N2 C32 C31 114.1(11) . . ?
N2 C32 H32A 108.7 . . ?
C31 C32 H32A 108.7 . . ?
N2 C32 H32B 108.7 . . ?
C31 C32 H32B 108.7 . . ?
H32A C32 H32B 107.6 . . ?
N1 C33 C34 105.1(10) . . ?
N1 C33 H33A 110.7 . . ?
C34 C33 H33A 110.7 . . ?
N1 C33 H33B 110.7 . . ?
C34 C33 H33B 110.7 . . ?
H33A C33 H33B 108.8 . . ?
N2 C34 C33 110.2(10) . . ?
N2 C34 H34A 109.6 . . ?
C33 C34 H34A 109.6 . . ?
N2 C34 H34B 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C36 C35 N1 106.7(11) . . ?
C36 C35 H35A 110.4 . . ?
N1 C35 H35A 110.4 . . ?
C36 C35 H35B 110.4 . . ?
N1 C35 H35B 110.4 . . ?
H35A C35 H35B 108.6 . . ?
N2 C36 C35 112.7(12) . . ?
N2 C36 H36A 109.0 . . ?
C35 C36 H36A 109.0 . . ?
N2 C36 H36B 109.0 . . ?
C35 C36 H36B 109.0 . . ?
H36A C36 H36B 107.8 . . ?
C38 C37 N3 108.8(8) . . ?
C38 C37 H37A 109.9 . . ?
N3 C37 H37A 109.9 . . ?
C38 C37 H37B 109.9 . . ?
N3 C37 H37B 109.9 . . ?
H37A C37 H37B 108.3 . . ?
N4 C38 C37 111.5(8) . . ?
N4 C38 H38A 109.3 . . ?
C37 C38 H38A 109.3 . . ?
N4 C38 H38B 109.3 . . ?
C37 C38 H38B 109.3 . . ?
H38A C38 H38B 108.0 . . ?
C40 C39 N3 110.4(8) . . ?
C40 C39 H39A 109.6 . . ?
N3 C39 H39A 109.6 . . ?
C40 C39 H39B 109.6 . . ?
N3 C39 H39B 109.6 . . ?
H39A C39 H39B 108.1 . . ?
N4 C40 C39 110.1(9) . . ?
N4 C40 H40A 109.6 . . ?
C39 C40 H40A 109.6 . . ?
N4 C40 H40B 109.6 . . ?
C39 C40 H40B 109.6 . . ?
H40A C40 H40B 108.2 . . ?
N3 C41 C42 107.8(9) . . ?
N3 C41 H41A 110.1 . . ?
C42 C41 H41A 110.1 . . ?
N3 C41 H41B 110.1 . . ?
C42 C41 H41B 110.1 . . ?
H41A C41 H41B 108.5 . . ?
N4 C42 C41 112.7(9) . . ?
N4 C42 H42A 109.1 . . ?
C41 C42 H42A 109.1 . . ?
N4 C42 H42B 109.1 . . ?
C41 C42 H42B 109.1 . . ?
H42A C42 H42B 107.8 . . ?

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
C14 C1 C2 C3 -1.2(13) . . . . ?
C1 C2 C3 C4 -178.4(8) . . . . ?
C1 C2 C3 C12 -2.0(12) . . . . ?
C2 C3 C4 C5 179.5(8) . . . . ?
C12 C3 C4 C5 3.2(13) . . . . ?
C2 C3 C4 C15 -2.4(13) . . . . ?
C12 C3 C4 C15 -178.7(8) . . . . ?
C3 C4 C5 C6 178.2(8) . . . . ?
C15 C4 C5 C6 0.1(13) . . . . ?
C3 C4 C5 C10 -4.1(13) . . . . ?
C15 C4 C5 C10 177.7(8) . . . . ?
C4 C5 C6 C7 179.7(9) . . . . ?
C10 C5 C6 C7 2.0(14) . . . . ?
C5 C6 C7 C8 -3.3(15) . . . . ?
C6 C7 C8 C9 2.4(14) . . . . ?
C7 C8 C9 C10 -0.2(14) . . . . ?
C8 C9 C10 C11 179.6(8) . . . . ?
C8 C9 C10 C5 -1.0(12) . . . . ?
C4 C5 C10 C11 1.9(12) . . . . ?
C6 C5 C10 C11 179.6(8) . . . . ?
C4 C5 C10 C9 -177.5(8) . . . . ?
C6 C5 C10 C9 0.2(11) . . . . ?
C9 C10 C11 C12 -179.4(7) . . . . ?
C5 C10 C11 C12 1.3(12) . . . . ?
C9 C10 C11 C16 3.1(12) . . . . ?
C5 C10 C11 C16 -176.2(7) . . . . ?
C10 C11 C12 C13 177.2(7) . . . . ?
C16 C11 C12 C13 -5.4(12) . . . . ?
C10 C11 C12 C3 -2.2(11) . . . . ?
C16 C11 C12 C3 175.3(7) . . . . ?
C4 C3 C12 C13 -179.4(8) . . . . ?
C2 C3 C12 C13 4.1(11) . . . . ?
C4 C3 C12 C11 0.0(11) . . . . ?
C2 C3 C12 C11 -176.5(7) . . . . ?
C11 C12 C13 C14 177.7(8) . . . . ?
C3 C12 C13 C14 -2.9(12) . . . . ?
C12 C13 C14 C1 -0.4(12) . . . . ?
C2 C1 C14 C13 2.5(12) . . . . ?
C5 C4 C15 O2 -94.5(12) . . . . ?
C3 C4 C15 O2 87.4(12) . . . . ?
C5 C4 C15 O1 87.2(11) . . . . ?
C3 C4 C15 O1 -91.0(12) . . . . ?
C10 C11 C16 C17 -92.2(10) . . . . ?
C12 C11 C16 C17 90.4(11) . . . . ?
C10 C11 C16 C29 83.1(10) . . . . ?
C12 C11 C16 C29 -94.4(9) . . . . ?
C29 C16 C17 C18 179.7(8) . . . . ?
C11 C16 C17 C18 -5.2(14) . . . . ?
C29 C16 C17 C22 -3.2(14) . . . . ?
C11 C16 C17 C22 171.9(7) . . . . ?
C16 C17 C18 C19 177.8(9) . . . . ?
C22 C17 C18 C19 0.6(14) . . . . ?
C17 C18 C19 C20 1.3(15) . . . . ?
C18 C19 C20 C21 -2.6(16) . . . . ?
C19 C20 C21 C22 1.7(16) . . . . ?
C20 C21 C22 C23 -177.9(10) . . . . ?
C20 C21 C22 C17 0.3(15) . . . . ?
C16 C17 C22 C23 -0.4(13) . . . . ?
C18 C17 C22 C23 176.8(8) . . . . ?
C16 C17 C22 C21 -178.8(9) . . . . ?
C18 C17 C22 C21 -1.5(13) . . . . ?
C21 C22 C23 C24 -177.8(9) . . . . ?
C17 C22 C23 C24 3.9(14) . . . . ?
C21 C22 C23 C30 4.5(14) . . . . ?
C17 C22 C23 C30 -173.8(8) . . . . ?
C22 C23 C24 C25 176.4(8) . . . . ?
C30 C23 C24 C25 -5.9(13) . . . . ?
C22 C23 C24 C29 -3.7(14) . . . . ?
C30 C23 C24 C29 174.0(8) . . . . ?
C29 C24 C25 C26 -0.3(13) . . . . ?
C23 C24 C25 C26 179.7(9) . . . . ?
C24 C25 C26 C27 -1.0(14) . . . . ?
C25 C26 C27 C28 -0.6(14) . . . . ?
C26 C27 C28 C29 3.5(13) . . . . ?
C25 C24 C29 C28 3.0(12) . . . . ?
C23 C24 C29 C28 -177.0(7) . . . . ?
C25 C24 C29 C16 -180.0(8) . . . . ?
C23 C24 C29 C16 0.0(13) . . . . ?
C27 C28 C29 C24 -4.6(12) . . . . ?
C27 C28 C29 C16 178.4(8) . . . . ?
C17 C16 C29 C24 3.4(14) . . . . ?
C11 C16 C29 C24 -171.9(7) . . . . ?
C17 C16 C29 C28 -179.7(8) . . . . ?
C11 C16 C29 C28 5.0(13) . . . . ?
C22 C23 C30 O4 -75.7(12) . . . . ?
C24 C23 C30 O4 106.6(10) . . . . ?
C22 C23 C30 O3 106.3(10) . . . . ?
C24 C23 C30 O3 -71.3(11) . . . . ?
C33 N1 C31 C32 71.8(13) . . . . ?
C35 N1 C31 C32 -51.0(13) . . . . ?
C36 N2 C32 C31 65.7(16) . . . . ?
C34 N2 C32 C31 -49.3(16) . . . . ?
N1 C31 C32 N2 -14.0(16) . . . . ?
C31 N1 C33 C34 -56.4(13) . . . . ?
C35 N1 C33 C34 65.3(13) . . . . ?
C32 N2 C34 C33 61.9(16) . . . . ?
C36 N2 C34 C33 -54.6(16) . . . . ?
N1 C33 C34 N2 -8.8(17) . . . . ?
C33 N1 C35 C36 -54.8(15) . . . . ?
C31 N1 C35 C36 67.1(14) . . . . ?
C32 N2 C36 C35 -47(2) . . . . ?
C34 N2 C36 C35 69.2(18) . . . . ?
N1 C35 C36 N2 -15(2) . . . . ?
C41 N3 C37 C38 -60.4(11) . . . . ?
C39 N3 C37 C38 58.1(10) . . . . ?
C42 N4 C38 C37 55.2(12) . . . . ?
C40 N4 C38 C37 -61.5(11) . . . . ?
N3 C37 C38 N4 4.1(12) . . . . ?
C41 N3 C39 C40 51.9(11) . . . . ?
C37 N3 C39 C40 -67.0(10) . . . . ?
C42 N4 C40 C39 -65.7(11) . . . . ?
C38 N4 C40 C39 53.2(11) . . . . ?
N3 C39 C40 N4 10.7(12) . . . . ?
C39 N3 C41 C42 -60.1(11) . . . . ?
C37 N3 C41 C42 55.3(12) . . . . ?
C38 N4 C42 C41 -60.9(12) . . . . ?
C40 N4 C42 C41 56.9(12) . . . . ?
N3 C41 C42 N4 4.5(13) . . . . ?

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
C31 H31B O11 0.99 2.54 3.287(16) 131.8 4_454 yes
C33 H33B O11 0.99 2.56 3.34(2) 136.1 3_455 yes
C35 H35A O7 0.99 2.68 3.420(18) 132.2 4 yes
C36 H36B O7 0.99 2.53 3.35(3) 140.0 3 yes
C40 H40B O6 0.99 2.55 3.355(15) 138.6 4 yes

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mfu223_meoh
_database_code_depnum_ccdc_archive 'CCDC 1952760'
loop_
_audit_author_name
_audit_author_address
'Misaki Okayasu'
;Toho University
Japan
;
_audit_update_record             
;
2019-09-11 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C40 H26 N2 O4'
_chemical_formula_moiety         'C40 H26 N2 O4'
_chemical_formula_weight         598.66
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   14.3333(5)
_cell_length_b                   11.8876(4)
_cell_length_c                   16.9672(6)
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.463(3)
_cell_angle_gamma                90.0000
_cell_volume                     2872.64(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8818
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      28.57
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248.00
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_T_max  0.997

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            45664
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.613
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6569
_reflns_number_gt                4351
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1176
_refine_ls_wR_factor_gt          0.1046
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         6569
_refine_ls_number_parameters     423
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0501P)²+0.5529P] 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_diff_density_max         0.26
_refine_diff_density_min         -0.30
_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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
O1 O 0.52792(9) 0.33101(10) 0.52221(7) 0.0281(3) Uani 1 1 d . . . . .
O2 O 0.58244(10) 0.16382(12) 0.56561(8) 0.0389(4) Uani 1 1 d . . . . .
O3 O -0.01949(8) 0.19850(10) 0.95768(7) 0.0255(3) Uani 1 1 d . . . . .
O4 O -0.00591(8) 0.38566(10) 0.95960(7) 0.0283(3) Uani 1 1 d . . . . .
N1 N 0.63735(10) 0.31639(12) 0.40999(8) 0.0231(3) Uani 1 1 d . . . . .
N2 N 0.88153(10) 0.23422(13) 0.07546(8) 0.0246(3) Uani 1 1 d . . . . .
C1 C 0.56083(12) 0.43369(15) 0.78150(10) 0.0233(4) Uani 1 1 d . . . . .
H1A H 0.617075 0.475219 0.794546 0.028 Uiso 1 1 calc R U . . .
C2 C 0.54828(12) 0.37430(14) 0.71261(10) 0.0212(4) Uani 1 1 d . . . . .
H2 H 0.595893 0.375527 0.677933 0.025 Uiso 1 1 calc R U . . .
C3 C 0.46483(11) 0.31000(14) 0.69127(10) 0.0180(4) Uani 1 1 d . . . . .
C4 C 0.45201(11) 0.24499(14) 0.62191(9) 0.0171(4) Uani 1 1 d . . . . .
C5 C 0.36907(11) 0.18294(14) 0.60220(9) 0.0170(4) Uani 1 1 d . . . . .
C6 C 0.35480(12) 0.11512(14) 0.53217(10) 0.0207(4) Uani 1 1 d . . . . .
H6 H 0.402909 0.110749 0.498079 0.025 Uiso 1 1 calc R U . . .
C7 C 0.27392(12) 0.05700(15) 0.51356(10) 0.0234(4) Uani 1 1 d . . . . .
H7 H 0.266228 0.012254 0.466893 0.028 Uiso 1 1 calc R U . . .
C8 C 0.20042(12) 0.06240(14) 0.56329(10) 0.0221(4) Uani 1 1 d . . . . .
H8 H 0.143771 0.021990 0.549416 0.027 Uiso 1 1 calc R U . . .
C9 C 0.21121(11) 0.12550(14) 0.63085(10) 0.0193(4) Uani 1 1 d . . . . .
H9 H 0.161821 0.128182 0.663735 0.023 Uiso 1 1 calc R U . . .
C10 C 0.29570(11) 0.18787(14) 0.65318(9) 0.0163(4) Uani 1 1 d . . . . .
C11 C 0.30823(11) 0.25263(14) 0.72327(9) 0.0168(4) Uani 1 1 d . . . . .
C12 C 0.39262(11) 0.31251(14) 0.74354(10) 0.0176(4) Uani 1 1 d . . . . .
C13 C 0.40924(12) 0.37611(14) 0.81543(10) 0.0205(4) Uani 1 1 d . . . . .
H13 H 0.362512 0.377897 0.850925 0.025 Uiso 1 1 calc R U . . .
C14 C 0.49064(12) 0.43404(15) 0.83390(10) 0.0224(4) Uani 1 1 d . . . . .
H14 H 0.500423 0.474945 0.882224 0.027 Uiso 1 1 calc R U . . .
C15 C 0.52813(11) 0.24157(15) 0.56715(10) 0.0195(4) Uani 1 1 d . . . . .
C16 C 0.23195(11) 0.25972(14) 0.77695(10) 0.0173(4) Uani 1 1 d . . . . .
C17 C 0.15641(11) 0.33532(14) 0.75847(9) 0.0180(4) Uani 1 1 d . . . . .
C18 C 0.15001(12) 0.40361(15) 0.68864(10) 0.0220(4) Uani 1 1 d . . . . .
H18 H 0.196366 0.396227 0.653116 0.026 Uiso 1 1 calc R U . . .
C19 C 0.07896(12) 0.47894(16) 0.67194(10) 0.0270(4) Uani 1 1 d . . . . .
H19 H 0.075958 0.523333 0.625166 0.032 Uiso 1 1 calc R U . . .
C20 C 0.00978(12) 0.49085(16) 0.72438(11) 0.0274(4) Uani 1 1 d . . . . .
H20 H -0.039151 0.544271 0.712850 0.033 Uiso 1 1 calc R U . . .
C21 C 0.01204(12) 0.42723(15) 0.79099(10) 0.0232(4) Uani 1 1 d . . . . .
H21 H -0.036036 0.436082 0.824727 0.028 Uiso 1 1 calc R U . . .
C22 C 0.08561(11) 0.34674(14) 0.81159(10) 0.0184(4) Uani 1 1 d . . . . .
C23 C 0.09150(11) 0.28066(14) 0.88108(10) 0.0178(4) Uani 1 1 d . . . . .
C24 C 0.16807(11) 0.20690(14) 0.90079(9) 0.0171(4) Uani 1 1 d . . . . .
C25 C 0.18240(12) 0.14723(14) 0.97449(10) 0.0217(4) Uani 1 1 d . . . . .
H25 H 0.137454 0.153974 1.011316 0.026 Uiso 1 1 calc R U . . .
C26 C 0.25914(12) 0.08117(15) 0.99266(10) 0.0244(4) Uani 1 1 d . . . . .
H26 H 0.267368 0.043425 1.042307 0.029 Uiso 1 1 calc R U . . .
C27 C 0.32714(12) 0.06751(15) 0.93891(10) 0.0241(4) Uani 1 1 d . . . . .
H27 H 0.379797 0.019853 0.952070 0.029 Uiso 1 1 calc R U . . .
C28 C 0.31662(12) 0.12289(14) 0.86852(10) 0.0207(4) Uani 1 1 d . . . . .
H28 H 0.362134 0.112818 0.832528 0.025 Uiso 1 1 calc R U . . .
C29 C 0.23858(11) 0.19608(14) 0.84722(9) 0.0173(4) Uani 1 1 d . . . . .
C30 C 0.01756(11) 0.29408(15) 0.93682(10) 0.0188(4) Uani 1 1 d . . . . .
C31 C 0.70593(12) 0.24021(16) 0.41172(10) 0.0249(4) Uani 1 1 d . . . . .
H31 H 0.719733 0.195858 0.458151 0.030 Uiso 1 1 calc R U . . .
C32 C 0.75781(12) 0.22308(15) 0.34869(10) 0.0242(4) Uani 1 1 d . . . . .
H32 H 0.806388 0.168342 0.352210 0.029 Uiso 1 1 calc R U . . .
C33 C 0.73790(11) 0.28720(14) 0.27987(10) 0.0194(4) Uani 1 1 d . . . . .
C34 C 0.66684(12) 0.36684(15) 0.27883(11) 0.0246(4) Uani 1 1 d . . . . .
H34 H 0.651467 0.412929 0.233487 0.030 Uiso 1 1 calc R U . . .
C35 C 0.61883(13) 0.37819(15) 0.34452(11) 0.0266(4) Uani 1 1 d . . . . .
H35 H 0.570204 0.432720 0.342993 0.032 Uiso 1 1 calc R U . . .
C36 C 0.84909(12) 0.14776(16) 0.11450(11) 0.0273(4) Uani 1 1 d . . . . .
H36 H 0.857713 0.073791 0.095399 0.033 Uiso 1 1 calc R U . . .
C37 C 0.80346(12) 0.16101(15) 0.18156(11) 0.0247(4) Uani 1 1 d . . . . .
H37 H 0.782841 0.097129 0.208445 0.030 Uiso 1 1 calc R U . . .
C38 C 0.78808(11) 0.26898(15) 0.20923(10) 0.0205(4) Uani 1 1 d . . . . .
C39 C 0.82011(12) 0.35862(15) 0.16718(10) 0.0235(4) Uani 1 1 d . . . . .
H39 H 0.809291 0.433688 0.183081 0.028 Uiso 1 1 calc R U . . .
C40 C 0.86793(12) 0.33836(16) 0.10196(10) 0.0251(4) Uani 1 1 d . . . . .
H40 H 0.891817 0.400414 0.075209 0.030 Uiso 1 1 calc R U . . .
H1 H 0.5778(16) 0.3200(19) 0.4809(14) 0.062(7) Uiso 1 1 d . . . . .
H3 H -0.0604(17) 0.2167(19) 1.0029(15) 0.063(7) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C15 1.308(2) . ?
O1 H1 1.06(2) . ?
O2 C15 1.210(2) . ?
O3 C30 1.319(2) . ?
O3 H3 1.04(2) . ?
O4 C30 1.215(2) . ?
N1 C35 1.333(2) . ?
N1 C31 1.334(2) . ?
N2 C36 1.334(2) . ?
N2 C40 1.339(2) . ?
C1 C2 1.360(2) . ?
C1 C14 1.416(2) . ?
C1 H1A 0.9500 . ?
C2 C3 1.431(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.403(2) . ?
C3 C12 1.437(2) . ?
C4 C5 1.407(2) . ?
C4 C15 1.511(2) . ?
C5 C6 1.432(2) . ?
C5 C10 1.436(2) . ?
C6 C7 1.356(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.423(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.364(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.434(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.411(2) . ?
C11 C12 1.412(2) . ?
C11 C16 1.502(2) . ?
C12 C13 1.432(2) . ?
C13 C14 1.361(2) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C16 C29 1.406(2) . ?
C16 C17 1.415(2) . ?
C17 C18 1.431(2) . ?
C17 C22 1.438(2) . ?
C18 C19 1.362(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.412(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.357(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.438(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.411(2) . ?
C23 C24 1.415(2) . ?
C23 C30 1.506(2) . ?
C24 C25 1.432(2) . ?
C24 C29 1.439(2) . ?
C25 C26 1.358(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.417(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.357(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.431(2) . ?
C28 H28 0.9500 . ?
C31 C32 1.385(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.397(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.389(2) . ?
C33 C38 1.482(2) . ?
C34 C35 1.381(2) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.384(2) . ?
C36 H36 0.9500 . ?
C37 C38 1.393(2) . ?
C37 H37 0.9500 . ?
C38 C39 1.389(2) . ?
C39 C40 1.387(2) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?

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
C15 O1 H1 109.0(12) . . ?
C30 O3 H3 107.2(13) . . ?
C35 N1 C31 117.99(15) . . ?
C36 N2 C40 118.25(15) . . ?
C2 C1 C14 120.45(16) . . ?
C2 C1 H1A 119.8 . . ?
C14 C1 H1A 119.8 . . ?
C1 C2 C3 121.36(16) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
C4 C3 C2 122.23(15) . . ?
C4 C3 C12 119.59(15) . . ?
C2 C3 C12 118.18(15) . . ?
C3 C4 C5 121.04(14) . . ?
C3 C4 C15 119.69(15) . . ?
C5 C4 C15 119.27(14) . . ?
C4 C5 C6 122.04(15) . . ?
C4 C5 C10 119.47(14) . . ?
C6 C5 C10 118.49(15) . . ?
C7 C6 C5 121.25(15) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C8 120.63(16) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C9 C8 C7 120.10(16) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 121.25(15) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C11 C10 C9 121.89(14) . . ?
C11 C10 C5 119.84(14) . . ?
C9 C10 C5 118.27(14) . . ?
C10 C11 C12 120.30(14) . . ?
C10 C11 C16 120.63(14) . . ?
C12 C11 C16 119.07(14) . . ?
C11 C12 C13 121.97(15) . . ?
C11 C12 C3 119.72(15) . . ?
C13 C12 C3 118.31(15) . . ?
C14 C13 C12 121.30(15) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C1 120.36(16) . . ?
C13 C14 H14 119.8 . . ?
C1 C14 H14 119.8 . . ?
O2 C15 O1 124.56(16) . . ?
O2 C15 C4 122.98(16) . . ?
O1 C15 C4 112.46(14) . . ?
C29 C16 C17 120.43(14) . . ?
C29 C16 C11 119.98(14) . . ?
C17 C16 C11 119.50(14) . . ?
C16 C17 C18 121.33(15) . . ?
C16 C17 C22 119.85(15) . . ?
C18 C17 C22 118.80(15) . . ?
C19 C18 C17 121.48(16) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C20 119.78(16) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 121.08(17) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C22 121.44(16) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C23 C22 C17 119.42(14) . . ?
C23 C22 C21 123.15(15) . . ?
C17 C22 C21 117.43(15) . . ?
C22 C23 C24 120.94(14) . . ?
C22 C23 C30 119.04(14) . . ?
C24 C23 C30 119.93(14) . . ?
C23 C24 C25 122.98(14) . . ?
C23 C24 C29 119.16(15) . . ?
C25 C24 C29 117.73(15) . . ?
C26 C25 C24 121.15(15) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C27 121.21(16) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C28 C27 C26 119.63(16) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C27 C28 C29 121.56(15) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 H28 119.2 . . ?
C16 C29 C28 121.16(15) . . ?
C16 C29 C24 120.15(15) . . ?
C28 C29 C24 118.65(15) . . ?
O4 C30 O3 123.50(15) . . ?
O4 C30 C23 122.28(15) . . ?
O3 C30 C23 114.21(14) . . ?
N1 C31 C32 122.75(16) . . ?
N1 C31 H31 118.6 . . ?
C32 C31 H31 118.6 . . ?
C31 C32 C33 119.24(16) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C34 C33 C32 117.58(15) . . ?
C34 C33 C38 120.75(15) . . ?
C32 C33 C38 121.63(15) . . ?
C35 C34 C33 119.18(17) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
N1 C35 C34 123.23(17) . . ?
N1 C35 H35 118.4 . . ?
C34 C35 H35 118.4 . . ?
N2 C36 C37 122.94(17) . . ?
N2 C36 H36 118.5 . . ?
C37 C36 H36 118.5 . . ?
C36 C37 C38 119.31(16) . . ?
C36 C37 H37 120.3 . . ?
C38 C37 H37 120.3 . . ?
C39 C38 C37 117.38(15) . . ?
C39 C38 C33 121.47(15) . . ?
C37 C38 C33 121.14(15) . . ?
C40 C39 C38 119.88(16) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
N2 C40 C39 122.17(16) . . ?
N2 C40 H40 118.9 . . ?
C39 C40 H40 118.9 . . ?

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
C14 C1 C2 C3 -0.5(3) . . . . ?
C1 C2 C3 C4 -177.66(16) . . . . ?
C1 C2 C3 C12 2.0(2) . . . . ?
C2 C3 C4 C5 -179.73(15) . . . . ?
C12 C3 C4 C5 0.6(2) . . . . ?
C2 C3 C4 C15 0.1(2) . . . . ?
C12 C3 C4 C15 -179.57(14) . . . . ?
C3 C4 C5 C6 -179.36(15) . . . . ?
C15 C4 C5 C6 0.8(2) . . . . ?
C3 C4 C5 C10 1.1(2) . . . . ?
C15 C4 C5 C10 -178.66(14) . . . . ?
C4 C5 C6 C7 -179.15(16) . . . . ?
C10 C5 C6 C7 0.4(2) . . . . ?
C5 C6 C7 C8 0.3(3) . . . . ?
C6 C7 C8 C9 -0.7(3) . . . . ?
C7 C8 C9 C10 0.3(3) . . . . ?
C8 C9 C10 C11 -179.37(16) . . . . ?
C8 C9 C10 C5 0.4(2) . . . . ?
C4 C5 C10 C11 -1.4(2) . . . . ?
C6 C5 C10 C11 179.04(15) . . . . ?
C4 C5 C10 C9 178.82(15) . . . . ?
C6 C5 C10 C9 -0.7(2) . . . . ?
C9 C10 C11 C12 179.68(15) . . . . ?
C5 C10 C11 C12 -0.1(2) . . . . ?
C9 C10 C11 C16 -0.9(2) . . . . ?
C5 C10 C11 C16 179.41(14) . . . . ?
C10 C11 C12 C13 -177.89(15) . . . . ?
C16 C11 C12 C13 2.6(2) . . . . ?
C10 C11 C12 C3 1.8(2) . . . . ?
C16 C11 C12 C3 -177.65(14) . . . . ?
C4 C3 C12 C11 -2.1(2) . . . . ?
C2 C3 C12 C11 178.22(15) . . . . ?
C4 C3 C12 C13 177.60(15) . . . . ?
C2 C3 C12 C13 -2.0(2) . . . . ?
C11 C12 C13 C14 -179.53(16) . . . . ?
C3 C12 C13 C14 0.7(2) . . . . ?
C12 C13 C14 C1 0.7(3) . . . . ?
C2 C1 C14 C13 -0.9(3) . . . . ?
C3 C4 C15 O2 101.5(2) . . . . ?
C5 C4 C15 O2 -78.7(2) . . . . ?
C3 C4 C15 O1 -78.77(19) . . . . ?
C5 C4 C15 O1 101.03(18) . . . . ?
C10 C11 C16 C29 102.13(19) . . . . ?
C12 C11 C16 C29 -78.4(2) . . . . ?
C10 C11 C16 C17 -81.3(2) . . . . ?
C12 C11 C16 C17 98.13(19) . . . . ?
C29 C16 C17 C18 177.89(16) . . . . ?
C11 C16 C17 C18 1.4(2) . . . . ?
C29 C16 C17 C22 -0.4(2) . . . . ?
C11 C16 C17 C22 -176.88(15) . . . . ?
C16 C17 C18 C19 -177.95(16) . . . . ?
C22 C17 C18 C19 0.3(3) . . . . ?
C17 C18 C19 C20 0.1(3) . . . . ?
C18 C19 C20 C21 -0.9(3) . . . . ?
C19 C20 C21 C22 1.1(3) . . . . ?
C16 C17 C22 C23 -1.1(2) . . . . ?
C18 C17 C22 C23 -179.43(15) . . . . ?
C16 C17 C22 C21 178.19(15) . . . . ?
C18 C17 C22 C21 -0.1(2) . . . . ?
C20 C21 C22 C23 178.69(17) . . . . ?
C20 C21 C22 C17 -0.6(2) . . . . ?
C17 C22 C23 C24 2.6(2) . . . . ?
C21 C22 C23 C24 -176.62(15) . . . . ?
C17 C22 C23 C30 179.36(15) . . . . ?
C21 C22 C23 C30 0.1(2) . . . . ?
C22 C23 C24 C25 173.17(16) . . . . ?
C30 C23 C24 C25 -3.5(2) . . . . ?
C22 C23 C24 C29 -2.6(2) . . . . ?
C30 C23 C24 C29 -179.32(14) . . . . ?
C23 C24 C25 C26 -176.96(16) . . . . ?
C29 C24 C25 C26 -1.1(2) . . . . ?
C24 C25 C26 C27 -0.9(3) . . . . ?
C25 C26 C27 C28 1.2(3) . . . . ?
C26 C27 C28 C29 0.6(3) . . . . ?
C17 C16 C29 C28 -177.26(15) . . . . ?
C11 C16 C29 C28 -0.8(2) . . . . ?
C17 C16 C29 C24 0.4(2) . . . . ?
C11 C16 C29 C24 176.87(14) . . . . ?
C27 C28 C29 C16 175.08(16) . . . . ?
C27 C28 C29 C24 -2.6(2) . . . . ?
C23 C24 C29 C16 1.1(2) . . . . ?
C25 C24 C29 C16 -174.92(15) . . . . ?
C23 C24 C29 C28 178.81(15) . . . . ?
C25 C24 C29 C28 2.8(2) . . . . ?
C22 C23 C30 O4 -49.0(2) . . . . ?
C24 C23 C30 O4 127.74(18) . . . . ?
C22 C23 C30 O3 130.35(16) . . . . ?
C24 C23 C30 O3 -52.9(2) . . . . ?
C35 N1 C31 C32 -0.1(3) . . . . ?
N1 C31 C32 C33 -0.4(3) . . . . ?
C31 C32 C33 C34 0.8(3) . . . . ?
C31 C32 C33 C38 -177.15(16) . . . . ?
C32 C33 C34 C35 -0.8(3) . . . . ?
C38 C33 C34 C35 177.22(16) . . . . ?
C31 N1 C35 C34 0.2(3) . . . . ?
C33 C34 C35 N1 0.3(3) . . . . ?
C40 N2 C36 C37 -1.0(3) . . . . ?
N2 C36 C37 C38 1.6(3) . . . . ?
C36 C37 C38 C39 -0.1(3) . . . . ?
C36 C37 C38 C33 178.81(16) . . . . ?
C34 C33 C38 C39 45.7(2) . . . . ?
C32 C33 C38 C39 -136.42(18) . . . . ?
C34 C33 C38 C37 -133.14(18) . . . . ?
C32 C33 C38 C37 44.7(2) . . . . ?
C37 C38 C39 C40 -2.0(3) . . . . ?
C33 C38 C39 C40 179.13(16) . . . . ?
C36 N2 C40 C39 -1.2(3) . . . . ?
C38 C39 C40 N2 2.7(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 N1 . . . 2.605(2) 1.06(2) 1.55(2) 169(2) no
O3 H3 N2 . . 1_456 2.6124(19) 1.04(3) 1.58(3) 175(2) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mfu283-5h
_database_code_depnum_ccdc_archive 'CCDC 1952763'
loop_
_audit_author_name
_audit_author_address
'Misaki Okayasu'
;Toho University
Japan
;
_audit_update_record             
;
2019-10-24 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C42 H43 N4 O11'
_chemical_formula_moiety         'C42 H43 N4 O11'
_chemical_formula_weight         779.82
_chemical_melting_point          ?
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
_space_group_IT_number           33
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,1/2+Z
3 1/2-X,1/2+Y,1/2+Z
4 1/2+X,1/2-Y,+Z
#------------------------------------------------------------------------------
_cell_length_a                   33.4734(10)
_cell_length_b                   10.5712(4)
_cell_length_c                   11.1961(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3961.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9762
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      28.59
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1644.00
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_T_max  0.998

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            32412
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.650
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             7992
_reflns_number_gt                5920
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.681
_reflns_Friedel_fraction_max     0.751
_reflns_Friedel_fraction_full    0.810

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1536
_refine_ls_wR_factor_gt          0.1358
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         7992
_refine_ls_number_parameters     521
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0935P)²] 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_diff_density_max         0.42
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined using 1889 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.5(6)

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
O1 O 0.57047(8) 0.3767(3) 0.5109(3) 0.0313(8) Uani 1 1 d . . . . .
O2 O 0.57547(9) 0.5619(3) 0.4204(3) 0.0346(8) Uani 1 1 d . . . . .
H1 H 0.5221(16) 0.540(5) 0.455(5) 0.042 Uiso 1 1 d . U . . .
O3 O 0.90328(8) 0.4407(3) 0.3495(3) 0.0276(7) Uani 1 1 d . . . . .
H3A H 0.928257 0.444684 0.343383 0.041 Uiso 1 1 calc R U . . .
O4 O 0.91617(9) 0.5055(4) 0.5344(3) 0.0357(8) Uani 1 1 d . . . . .
O5 O 0.95265(10) 0.2274(3) 0.3122(3) 0.0381(8) Uani 1 1 d . . . . .
O6 O 1.03011(9) 0.3178(3) 0.3890(3) 0.0356(8) Uani 1 1 d . . . . .
O7 O 0.99862(9) 0.4922(3) 0.5379(3) 0.0314(7) Uani 1 1 d . . . . .
O8 O 0.95472(10) 0.2800(3) 0.7999(4) 0.0439(9) Uani 1 1 d . . . . .
O9 O 0.91600(10) 0.5126(3) 0.7766(3) 0.0365(8) Uani 1 1 d . . . . .
O10 O 0.59078(9) 0.1990(3) 0.6729(3) 0.0308(7) Uani 1 1 d . . . . .
O11 O 0.52735(10) 0.0693(3) 0.7691(3) 0.0383(8) Uani 1 1 d . . . . .
N1 N 0.49642(10) 0.5596(4) 0.4865(4) 0.0248(8) Uani 1 1 d . . . . .
N2 N 0.42736(10) 0.6083(4) 0.5609(4) 0.0298(9) Uani 1 1 d . . . . .
N3 N 0.63992(12) 0.0173(4) 0.5819(4) 0.0258(8) Uani 1 1 d . . . . .
N4 N 0.68401(10) -0.1106(4) 0.4448(3) 0.0257(8) Uani 1 1 d . . . . .
C1 C 0.65061(12) 0.6226(4) 0.7740(4) 0.0223(9) Uani 1 1 d . . . . .
H1A H 0.635327 0.662820 0.834592 0.027 Uiso 1 1 calc R U . . .
C2 C 0.63197(12) 0.5729(4) 0.6780(4) 0.0208(9) Uani 1 1 d . . . . .
H2 H 0.603703 0.578220 0.672164 0.025 Uiso 1 1 calc R U . . .
C3 C 0.65407(11) 0.5123(4) 0.5852(4) 0.0171(8) Uani 1 1 d . . . . .
C4 C 0.63539(11) 0.4618(4) 0.4833(4) 0.0171(8) Uani 1 1 d . . . . .
C5 C 0.65746(11) 0.4045(4) 0.3915(4) 0.0166(8) Uani 1 1 d . . . . .
C6 C 0.63909(12) 0.3522(4) 0.2885(4) 0.0203(9) Uani 1 1 d . . . . .
H6 H 0.610835 0.355453 0.281306 0.024 Uiso 1 1 calc R U . . .
C7 C 0.66078(12) 0.2978(4) 0.2001(4) 0.0215(9) Uani 1 1 d . . . . .
H7 H 0.647677 0.262575 0.132521 0.026 Uiso 1 1 calc R U . . .
C8 C 0.70271(12) 0.2935(4) 0.2084(4) 0.0208(9) Uani 1 1 d . . . . .
H8 H 0.717799 0.256176 0.145740 0.025 Uiso 1 1 calc R U . . .
C9 C 0.72185(12) 0.3421(4) 0.3051(4) 0.0180(8) Uani 1 1 d . . . . .
H9 H 0.750159 0.337610 0.309142 0.022 Uiso 1 1 calc R U . . .
C10 C 0.70034(11) 0.4000(4) 0.4010(4) 0.0149(8) Uani 1 1 d . . . . .
C11 C 0.71965(11) 0.4522(3) 0.5016(4) 0.0138(8) Uani 1 1 d . . . . .
C12 C 0.69689(11) 0.5063(4) 0.5946(4) 0.0150(8) Uani 1 1 d . . . . .
C13 C 0.71503(12) 0.5586(4) 0.6984(4) 0.0181(9) Uani 1 1 d . . . . .
H13 H 0.743214 0.553906 0.707256 0.022 Uiso 1 1 calc R U . . .
C14 C 0.69278(11) 0.6156(4) 0.7856(4) 0.0201(9) Uani 1 1 d . . . . .
H14 H 0.705538 0.650401 0.853907 0.024 Uiso 1 1 calc R U . . .
C15 C 0.59019(12) 0.4683(4) 0.4710(4) 0.0202(9) Uani 1 1 d . . . . .
C16 C 0.76423(11) 0.4583(4) 0.5029(4) 0.0150(8) Uani 1 1 d . . . . .
C17 C 0.78800(11) 0.3580(4) 0.5441(3) 0.0148(8) Uani 1 1 d . . . . .
C18 C 0.77064(12) 0.2463(4) 0.5960(4) 0.0211(9) Uani 1 1 d . . . . .
H18 H 0.742418 0.239556 0.602355 0.025 Uiso 1 1 calc R U . . .
C19 C 0.79390(13) 0.1513(4) 0.6355(4) 0.0273(10) Uani 1 1 d . . . . .
H19 H 0.781824 0.078510 0.669765 0.033 Uiso 1 1 calc R U . . .
C20 C 0.83626(14) 0.1579(4) 0.6268(4) 0.0301(11) Uani 1 1 d . . . . .
H20 H 0.852230 0.089788 0.654900 0.036 Uiso 1 1 calc R U . . .
C21 C 0.85371(13) 0.2610(4) 0.5785(4) 0.0245(10) Uani 1 1 d . . . . .
H21 H 0.882034 0.265042 0.574501 0.029 Uiso 1 1 calc R U . . .
C22 C 0.83076(11) 0.3638(4) 0.5335(4) 0.0185(9) Uani 1 1 d . . . . .
C23 C 0.84866(11) 0.4685(4) 0.4786(4) 0.0179(9) Uani 1 1 d . . . . .
C24 C 0.82516(11) 0.5714(4) 0.4403(4) 0.0166(8) Uani 1 1 d . . . . .
C25 C 0.84243(12) 0.6803(4) 0.3861(4) 0.0196(9) Uani 1 1 d . . . . .
H25 H 0.870557 0.683571 0.375267 0.024 Uiso 1 1 calc R U . . .
C26 C 0.81996(12) 0.7791(4) 0.3497(4) 0.0213(9) Uani 1 1 d . . . . .
H26 H 0.832359 0.851346 0.315509 0.026 Uiso 1 1 calc R U . . .
C27 C 0.77811(12) 0.7749(4) 0.3626(4) 0.0209(9) Uani 1 1 d . . . . .
H27 H 0.762446 0.844827 0.337032 0.025 Uiso 1 1 calc R U . . .
C28 C 0.75992(11) 0.6725(4) 0.4109(3) 0.0173(8) Uani 1 1 d . . . . .
H28 H 0.731622 0.670861 0.417206 0.021 Uiso 1 1 calc R U . . .
C29 C 0.78265(11) 0.5667(4) 0.4525(3) 0.0150(8) Uani 1 1 d . . . . .
C30 C 0.89316(12) 0.4710(4) 0.4528(4) 0.0205(9) Uani 1 1 d . . . . .
C31 C 0.49732(14) 0.6779(5) 0.5591(5) 0.0376(12) Uani 1 1 d . . . . .
H31A H 0.504975 0.750787 0.508540 0.045 Uiso 1 1 calc R U . . .
H31B H 0.517053 0.669892 0.624550 0.045 Uiso 1 1 calc R U . . .
C32 C 0.45547(18) 0.6978(6) 0.6104(7) 0.068(2) Uani 1 1 d . . . . .
H32A H 0.456350 0.687919 0.698328 0.082 Uiso 1 1 calc R U . . .
H32B H 0.446431 0.784919 0.592485 0.082 Uiso 1 1 calc R U . . .
C33 C 0.46966(12) 0.5765(4) 0.3824(4) 0.0267(10) Uani 1 1 d . . . . .
H33A H 0.466472 0.495758 0.338624 0.032 Uiso 1 1 calc R U . . .
H33B H 0.480654 0.640655 0.326966 0.032 Uiso 1 1 calc R U . . .
C34 C 0.42940(16) 0.6206(9) 0.4333(5) 0.074(2) Uani 1 1 d . . . . .
H34A H 0.425066 0.710283 0.411289 0.089 Uiso 1 1 calc R U . . .
H34B H 0.407695 0.570101 0.396766 0.089 Uiso 1 1 calc R U . . .
C35 C 0.48178(15) 0.4517(5) 0.5609(5) 0.0343(12) Uani 1 1 d . . . . .
H35A H 0.498027 0.443538 0.634378 0.041 Uiso 1 1 calc R U . . .
H35B H 0.483480 0.371436 0.515584 0.041 Uiso 1 1 calc R U . . .
C36 C 0.43779(18) 0.4820(5) 0.5927(7) 0.0594(19) Uani 1 1 d . . . . .
H36A H 0.419984 0.422240 0.550165 0.071 Uiso 1 1 calc R U . . .
H36B H 0.433716 0.470077 0.679511 0.071 Uiso 1 1 calc R U . . .
C37 C 0.65319(14) 0.0993(4) 0.4810(5) 0.0324(11) Uani 1 1 d . . . . .
H37A H 0.667080 0.175107 0.512084 0.039 Uiso 1 1 calc R U . . .
H37B H 0.629837 0.127265 0.433655 0.039 Uiso 1 1 calc R U . . .
C38 C 0.68189(15) 0.0204(4) 0.4021(4) 0.0316(11) Uani 1 1 d . . . . .
H38A H 0.672346 0.021399 0.318372 0.038 Uiso 1 1 calc R U . . .
H38B H 0.708887 0.058654 0.403937 0.038 Uiso 1 1 calc R U . . .
C39 C 0.67524(13) -0.0281(4) 0.6515(4) 0.0258(10) Uani 1 1 d . . . . .
H39A H 0.666457 -0.077619 0.721759 0.031 Uiso 1 1 calc R U . . .
H39B H 0.691385 0.044525 0.679617 0.031 Uiso 1 1 calc R U . . .
C40 C 0.70001(13) -0.1119(5) 0.5658(4) 0.0289(11) Uani 1 1 d . . . . .
H40A H 0.727956 -0.081271 0.564414 0.035 Uiso 1 1 calc R U . . .
H40B H 0.700172 -0.199887 0.596093 0.035 Uiso 1 1 calc R U . . .
C41 C 0.61668(13) -0.0929(4) 0.5366(4) 0.0267(10) Uani 1 1 d . . . . .
H41A H 0.591934 -0.063646 0.496852 0.032 Uiso 1 1 calc R U . . .
H41B H 0.609203 -0.149349 0.603564 0.032 Uiso 1 1 calc R U . . .
C42 C 0.64334(13) -0.1637(4) 0.4474(4) 0.0294(11) Uani 1 1 d . . . . .
H42A H 0.644676 -0.254167 0.469919 0.035 Uiso 1 1 calc R U . . .
H42B H 0.631429 -0.158102 0.366615 0.035 Uiso 1 1 calc R U . . .
H3 H 0.623(2) 0.060(6) 0.625(7) 0.07(2) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C15 1.254(5) . ?
O2 C15 1.242(5) . ?
O3 C30 1.247(5) . ?
O3 H3A 0.8400 . ?
O4 C30 1.249(5) . ?
N1 C33 1.480(6) . ?
N1 C31 1.492(6) . ?
N1 C35 1.496(6) . ?
N1 H1 0.95(6) . ?
N2 C36 1.426(7) . ?
N2 C34 1.436(7) . ?
N2 C32 1.445(7) . ?
N3 C41 1.490(6) . ?
N3 C37 1.491(6) . ?
N3 C39 1.495(6) . ?
N3 H3 0.87(7) . ?
N4 C40 1.457(6) . ?
N4 C38 1.467(6) . ?
N4 C42 1.473(6) . ?
C1 C2 1.349(6) . ?
C1 C14 1.419(5) . ?
C1 H1A 0.9500 . ?
C2 C3 1.428(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.406(6) . ?
C3 C12 1.438(5) . ?
C4 C5 1.403(6) . ?
C4 C15 1.521(5) . ?
C5 C6 1.419(6) . ?
C5 C10 1.440(5) . ?
C6 C7 1.356(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.407(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.360(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.430(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.411(6) . ?
C11 C12 1.411(6) . ?
C11 C16 1.494(5) . ?
C12 C13 1.423(6) . ?
C13 C14 1.368(6) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C16 C17 1.404(5) . ?
C16 C29 1.418(5) . ?
C17 C22 1.438(5) . ?
C17 C18 1.438(6) . ?
C18 C19 1.346(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.423(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.350(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.424(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.400(6) . ?
C23 C24 1.410(6) . ?
C23 C30 1.517(5) . ?
C24 C25 1.424(6) . ?
C24 C29 1.430(5) . ?
C25 C26 1.349(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.409(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.355(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.431(5) . ?
C28 H28 0.9500 . ?
C31 C32 1.528(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.536(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.548(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.549(7) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.547(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.535(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?

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
C30 O3 H3A 109.5 . . ?
C33 N1 C31 109.9(4) . . ?
C33 N1 C35 109.4(4) . . ?
C31 N1 C35 110.0(4) . . ?
C33 N1 H1 107(3) . . ?
C31 N1 H1 111(3) . . ?
C35 N1 H1 110(3) . . ?
C36 N2 C34 108.7(6) . . ?
C36 N2 C32 111.0(5) . . ?
C34 N2 C32 107.0(5) . . ?
C41 N3 C37 110.6(4) . . ?
C41 N3 C39 109.8(3) . . ?
C37 N3 C39 110.2(4) . . ?
C41 N3 H3 105(5) . . ?
C37 N3 H3 108(4) . . ?
C39 N3 H3 113(5) . . ?
C40 N4 C38 109.3(4) . . ?
C40 N4 C42 108.5(4) . . ?
C38 N4 C42 108.8(3) . . ?
C2 C1 C14 120.8(4) . . ?
C2 C1 H1A 119.6 . . ?
C14 C1 H1A 119.6 . . ?
C1 C2 C3 121.0(4) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C4 C3 C2 122.0(3) . . ?
C4 C3 C12 119.1(4) . . ?
C2 C3 C12 118.9(4) . . ?
C5 C4 C3 121.6(3) . . ?
C5 C4 C15 118.5(4) . . ?
C3 C4 C15 119.9(4) . . ?
C4 C5 C6 122.4(3) . . ?
C4 C5 C10 119.0(4) . . ?
C6 C5 C10 118.6(4) . . ?
C7 C6 C5 121.8(4) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C6 C7 C8 119.9(4) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 120.7(4) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 121.5(4) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C11 C10 C9 122.4(3) . . ?
C11 C10 C5 120.2(3) . . ?
C9 C10 C5 117.4(4) . . ?
C10 C11 C12 120.0(3) . . ?
C10 C11 C16 118.8(3) . . ?
C12 C11 C16 121.0(3) . . ?
C11 C12 C13 122.0(3) . . ?
C11 C12 C3 120.1(4) . . ?
C13 C12 C3 117.9(4) . . ?
C14 C13 C12 121.5(4) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C13 C14 C1 119.9(4) . . ?
C13 C14 H14 120.0 . . ?
C1 C14 H14 120.0 . . ?
O2 C15 O1 124.7(4) . . ?
O2 C15 C4 118.1(4) . . ?
O1 C15 C4 117.2(4) . . ?
C17 C16 C29 119.7(3) . . ?
C17 C16 C11 122.5(3) . . ?
C29 C16 C11 117.7(3) . . ?
C16 C17 C22 120.3(3) . . ?
C16 C17 C18 121.6(3) . . ?
C22 C17 C18 118.1(3) . . ?
C19 C18 C17 120.8(4) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 121.2(4) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
C21 C20 C19 119.9(4) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 121.7(4) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
C23 C22 C21 121.9(4) . . ?
C23 C22 C17 119.8(4) . . ?
C21 C22 C17 118.4(4) . . ?
C22 C23 C24 120.3(3) . . ?
C22 C23 C30 121.2(3) . . ?
C24 C23 C30 118.5(3) . . ?
C23 C24 C25 121.8(4) . . ?
C23 C24 C29 120.0(3) . . ?
C25 C24 C29 118.2(3) . . ?
C26 C25 C24 121.9(4) . . ?
C26 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C25 C26 C27 119.9(4) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 120.8(4) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C27 C28 C29 121.1(3) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C16 C29 C24 119.9(3) . . ?
C16 C29 C28 122.0(3) . . ?
C24 C29 C28 118.1(3) . . ?
O3 C30 O4 125.8(4) . . ?
O3 C30 C23 116.0(4) . . ?
O4 C30 C23 118.1(4) . . ?
N1 C31 C32 107.6(4) . . ?
N1 C31 H31A 110.2 . . ?
C32 C31 H31A 110.2 . . ?
N1 C31 H31B 110.2 . . ?
C32 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
N2 C32 C31 111.3(4) . . ?
N2 C32 H32A 109.4 . . ?
C31 C32 H32A 109.4 . . ?
N2 C32 H32B 109.4 . . ?
C31 C32 H32B 109.4 . . ?
H32A C32 H32B 108.0 . . ?
N1 C33 C34 106.0(4) . . ?
N1 C33 H33A 110.5 . . ?
C34 C33 H33A 110.5 . . ?
N1 C33 H33B 110.5 . . ?
C34 C33 H33B 110.5 . . ?
H33A C33 H33B 108.7 . . ?
N2 C34 C33 112.5(5) . . ?
N2 C34 H34A 109.1 . . ?
C33 C34 H34A 109.1 . . ?
N2 C34 H34B 109.1 . . ?
C33 C34 H34B 109.1 . . ?
H34A C34 H34B 107.8 . . ?
N1 C35 C36 106.4(4) . . ?
N1 C35 H35A 110.5 . . ?
C36 C35 H35A 110.5 . . ?
N1 C35 H35B 110.5 . . ?
C36 C35 H35B 110.5 . . ?
H35A C35 H35B 108.6 . . ?
N2 C36 C35 111.7(4) . . ?
N2 C36 H36A 109.3 . . ?
C35 C36 H36A 109.3 . . ?
N2 C36 H36B 109.3 . . ?
C35 C36 H36B 109.3 . . ?
H36A C36 H36B 107.9 . . ?
N3 C37 C38 107.7(3) . . ?
N3 C37 H37A 110.2 . . ?
C38 C37 H37A 110.2 . . ?
N3 C37 H37B 110.2 . . ?
C38 C37 H37B 110.2 . . ?
H37A C37 H37B 108.5 . . ?
N4 C38 C37 110.6(4) . . ?
N4 C38 H38A 109.5 . . ?
C37 C38 H38A 109.5 . . ?
N4 C38 H38B 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
N3 C39 C40 106.6(4) . . ?
N3 C39 H39A 110.4 . . ?
C40 C39 H39A 110.4 . . ?
N3 C39 H39B 110.4 . . ?
C40 C39 H39B 110.4 . . ?
H39A C39 H39B 108.6 . . ?
N4 C40 C39 112.0(3) . . ?
N4 C40 H40A 109.2 . . ?
C39 C40 H40A 109.2 . . ?
N4 C40 H40B 109.2 . . ?
C39 C40 H40B 109.2 . . ?
H40A C40 H40B 107.9 . . ?
N3 C41 C42 107.4(4) . . ?
N3 C41 H41A 110.2 . . ?
C42 C41 H41A 110.2 . . ?
N3 C41 H41B 110.2 . . ?
C42 C41 H41B 110.2 . . ?
H41A C41 H41B 108.5 . . ?
N4 C42 C41 111.3(4) . . ?
N4 C42 H42A 109.4 . . ?
C41 C42 H42A 109.4 . . ?
N4 C42 H42B 109.4 . . ?
C41 C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?

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
C14 C1 C2 C3 -0.3(6) . . . . ?
C1 C2 C3 C4 -178.8(4) . . . . ?
C1 C2 C3 C12 -0.8(6) . . . . ?
C2 C3 C4 C5 178.9(4) . . . . ?
C12 C3 C4 C5 0.8(6) . . . . ?
C2 C3 C4 C15 -1.4(6) . . . . ?
C12 C3 C4 C15 -179.4(3) . . . . ?
C3 C4 C5 C6 179.5(4) . . . . ?
C15 C4 C5 C6 -0.2(6) . . . . ?
C3 C4 C5 C10 -1.4(6) . . . . ?
C15 C4 C5 C10 178.8(3) . . . . ?
C4 C5 C6 C7 179.5(4) . . . . ?
C10 C5 C6 C7 0.5(6) . . . . ?
C5 C6 C7 C8 -0.8(6) . . . . ?
C6 C7 C8 C9 0.8(6) . . . . ?
C7 C8 C9 C10 -0.5(6) . . . . ?
C8 C9 C10 C11 -179.3(4) . . . . ?
C8 C9 C10 C5 0.2(6) . . . . ?
C4 C5 C10 C11 0.2(5) . . . . ?
C6 C5 C10 C11 179.3(4) . . . . ?
C4 C5 C10 C9 -179.3(4) . . . . ?
C6 C5 C10 C9 -0.2(5) . . . . ?
C9 C10 C11 C12 -178.9(3) . . . . ?
C5 C10 C11 C12 1.6(6) . . . . ?
C9 C10 C11 C16 5.9(6) . . . . ?
C5 C10 C11 C16 -173.6(3) . . . . ?
C10 C11 C12 C13 179.2(4) . . . . ?
C16 C11 C12 C13 -5.7(6) . . . . ?
C10 C11 C12 C3 -2.2(6) . . . . ?
C16 C11 C12 C3 172.9(3) . . . . ?
C4 C3 C12 C11 1.0(6) . . . . ?
C2 C3 C12 C11 -177.1(4) . . . . ?
C4 C3 C12 C13 179.7(4) . . . . ?
C2 C3 C12 C13 1.6(5) . . . . ?
C11 C12 C13 C14 177.2(4) . . . . ?
C3 C12 C13 C14 -1.5(6) . . . . ?
C12 C13 C14 C1 0.4(6) . . . . ?
C2 C1 C14 C13 0.5(6) . . . . ?
C5 C4 C15 O2 -89.6(5) . . . . ?
C3 C4 C15 O2 90.7(5) . . . . ?
C5 C4 C15 O1 89.0(5) . . . . ?
C3 C4 C15 O1 -90.8(5) . . . . ?
C10 C11 C16 C17 -87.5(5) . . . . ?
C12 C11 C16 C17 97.3(5) . . . . ?
C10 C11 C16 C29 88.1(4) . . . . ?
C12 C11 C16 C29 -87.1(5) . . . . ?
C29 C16 C17 C22 -1.2(6) . . . . ?
C11 C16 C17 C22 174.3(4) . . . . ?
C29 C16 C17 C18 179.9(4) . . . . ?
C11 C16 C17 C18 -4.6(6) . . . . ?
C16 C17 C18 C19 -179.8(4) . . . . ?
C22 C17 C18 C19 1.4(6) . . . . ?
C17 C18 C19 C20 -0.3(7) . . . . ?
C18 C19 C20 C21 0.2(7) . . . . ?
C19 C20 C21 C22 -1.2(7) . . . . ?
C20 C21 C22 C23 -177.1(4) . . . . ?
C20 C21 C22 C17 2.2(6) . . . . ?
C16 C17 C22 C23 -1.8(6) . . . . ?
C18 C17 C22 C23 177.1(4) . . . . ?
C16 C17 C22 C21 178.9(4) . . . . ?
C18 C17 C22 C21 -2.2(6) . . . . ?
C21 C22 C23 C24 -176.8(4) . . . . ?
C17 C22 C23 C24 3.8(6) . . . . ?
C21 C22 C23 C30 6.5(6) . . . . ?
C17 C22 C23 C30 -172.8(4) . . . . ?
C22 C23 C24 C25 178.9(4) . . . . ?
C30 C23 C24 C25 -4.4(6) . . . . ?
C22 C23 C24 C29 -2.9(6) . . . . ?
C30 C23 C24 C29 173.8(4) . . . . ?
C23 C24 C25 C26 -179.8(4) . . . . ?
C29 C24 C25 C26 1.9(6) . . . . ?
C24 C25 C26 C27 -1.4(7) . . . . ?
C25 C26 C27 C28 -0.2(6) . . . . ?
C26 C27 C28 C29 1.3(6) . . . . ?
C17 C16 C29 C24 2.2(6) . . . . ?
C11 C16 C29 C24 -173.6(3) . . . . ?
C17 C16 C29 C28 -178.9(4) . . . . ?
C11 C16 C29 C28 5.3(6) . . . . ?
C23 C24 C29 C16 -0.1(6) . . . . ?
C25 C24 C29 C16 178.2(4) . . . . ?
C23 C24 C29 C28 -179.1(4) . . . . ?
C25 C24 C29 C28 -0.8(5) . . . . ?
C27 C28 C29 C16 -179.7(4) . . . . ?
C27 C28 C29 C24 -0.8(6) . . . . ?
C22 C23 C30 O3 97.0(5) . . . . ?
C24 C23 C30 O3 -79.7(5) . . . . ?
C22 C23 C30 O4 -84.7(5) . . . . ?
C24 C23 C30 O4 98.6(5) . . . . ?
C33 N1 C31 C32 65.1(6) . . . . ?
C35 N1 C31 C32 -55.5(6) . . . . ?
C36 N2 C32 C31 63.4(7) . . . . ?
C34 N2 C32 C31 -55.0(7) . . . . ?
N1 C31 C32 N2 -7.8(8) . . . . ?
C31 N1 C33 C34 -53.9(6) . . . . ?
C35 N1 C33 C34 67.0(5) . . . . ?
C36 N2 C34 C33 -52.7(8) . . . . ?
C32 N2 C34 C33 67.2(8) . . . . ?
N1 C33 C34 N2 -11.3(8) . . . . ?
C33 N1 C35 C36 -55.5(5) . . . . ?
C31 N1 C35 C36 65.4(5) . . . . ?
C34 N2 C36 C35 64.9(7) . . . . ?
C32 N2 C36 C35 -52.5(7) . . . . ?
N1 C35 C36 N2 -10.1(7) . . . . ?
C41 N3 C37 C38 -63.5(5) . . . . ?
C39 N3 C37 C38 58.2(5) . . . . ?
C40 N4 C38 C37 -62.1(5) . . . . ?
C42 N4 C38 C37 56.3(5) . . . . ?
N3 C37 C38 N4 5.0(5) . . . . ?
C41 N3 C39 C40 58.1(5) . . . . ?
C37 N3 C39 C40 -64.0(5) . . . . ?
C38 N4 C40 C39 56.1(5) . . . . ?
C42 N4 C40 C39 -62.4(5) . . . . ?
N3 C39 C40 N4 5.6(5) . . . . ?
C37 N3 C41 C42 56.8(4) . . . . ?
C39 N3 C41 C42 -65.0(5) . . . . ?
C40 N4 C42 C41 55.3(5) . . . . ?
C38 N4 C42 C41 -63.5(5) . . . . ?
N3 C41 C42 N4 6.3(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C31 H31B O5 0.99 2.41 3.333(6) 154.7 3_655 yes
C32 H32A O6 0.99 2.58 3.402(8) 140.5 3_655 yes
C32 H32B O4 0.99 2.52 3.506(8) 173.0 4_465 yes
C33 H33A O5 0.99 2.42 3.356(6) 157.1 4_455 yes
C33 H33B O8 0.99 2.63 3.448(6) 139.5 3_654 yes
C37 H37B O9 0.99 2.63 3.383(6) 132.9 3_644 yes
C41 H41A O9 0.99 2.61 3.304(6) 127.4 3_644 yes
C42 H42B O9 0.99 2.61 3.328(6) 129.8 3_644 yes
N1 H1 O1 0.95(6) 2.45(5) 3.156(5) 131(4) . yes
N1 H1 O2 0.95(6) 1.84(5) 2.748(5) 158(5) . yes
N3 H3 O10 0.87(7) 1.90(7) 2.726(5) 158(6) . yes

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mfu291-1h
_database_code_depnum_ccdc_archive 'CCDC 1952761'
loop_
_audit_author_name
_audit_author_address
'Misaki Okayasu'
;Toho University
Japan
;
_audit_update_record             
;
2019-10-24 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C44.8 H39.6 N3.6 O8.2'
_chemical_formula_moiety         'C44.8 H39.6 N3.6 O8.2'
_chemical_formula_weight         759.62
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   10.3818(5)
_cell_length_b                   10.9676(2)
_cell_length_c                   18.7727(5)
_cell_angle_alpha                95.299(2)
_cell_angle_beta                 98.714(3)
_cell_angle_gamma                91.279(3)
_cell_volume                     2102.39(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13444
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      72.61
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             798.40
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.281
_exptl_absorpt_correction_T_max  0.986

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            55347
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_av_R_equivalents  0.1150
_diffrn_reflns_theta_max         68.235
_diffrn_reflns_theta_min         4.051
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             7536
_reflns_number_gt                4608
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1811
_refine_ls_R_factor_gt           0.1379
_refine_ls_wR_factor_ref         0.4352
_refine_ls_wR_factor_gt          0.3957
_refine_ls_number_restraints     64
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         7536
_refine_ls_number_parameters     585
_refine_ls_goodness_of_fit_ref   1.586
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.2000P)²] 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_diff_density_max         1.29
_refine_diff_density_min         -0.41
_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 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
O1 O 0.7326(5) 0.8195(4) 0.22951(19) 0.0771(14) Uani 1 1 d . . . . .
O2 O 0.6061(6) 0.6518(5) 0.2149(2) 0.0980(19) Uani 1 1 d . . . . .
O3 O 0.7288(5) 0.8500(4) 0.82859(19) 0.0701(12) Uani 1 1 d . . . . .
H3A H 0.747(7) 0.842(6) 0.904(4) 0.084 Uiso 1 1 d . U . . .
O4 O 0.9170(6) 0.7629(5) 0.8396(2) 0.0869(15) Uani 1 1 d . . . . .
O5 O 0.7113(9) 0.3271(7) 1.0957(5) 0.105(3) Uani 0.7 1 d . . P A 1
O6 O 0.7609(14) 0.3301(9) 0.9774(6) 0.145(4) Uani 0.7 1 d . . P A 1
O7 O 1.0602(9) 0.5510(6) 0.8305(4) 0.136(3) Uani 1 1 d . . . . .
O8 O 0.4928(8) 0.4657(6) 0.1139(5) 0.143(3) Uani 1 1 d . . . . .
N1 N 0.7336(6) 0.8100(5) 0.0946(2) 0.0655(14) Uani 1 1 d . . . . .
N2 N 0.7456(6) 0.8232(4) -0.0360(2) 0.0641(14) Uani 1 1 d . . . . .
N3 N 0.6919(8) 0.2383(9) 1.2314(4) 0.089(2) Uani 0.8 1 d . . P B 2
N4 N 0.6866(11) 0.2050(10) 1.3595(4) 0.123(4) Uani 0.8 1 d . . P B 2
C1 C 1.0254(6) 0.5975(4) 0.3666(3) 0.0588(15) Uani 1 1 d . . . . .
H1 H 1.088568 0.562235 0.340021 0.071 Uiso 1 1 calc R U . . .
C2 C 0.9120(6) 0.6343(4) 0.3309(3) 0.0528(14) Uani 1 1 d . . . . .
H2 H 0.896338 0.624289 0.279439 0.063 Uiso 1 1 calc R U . . .
C3 C 0.8144(6) 0.6887(4) 0.3699(2) 0.0460(12) Uani 1 1 d . . . . .
C4 C 0.6971(6) 0.7325(4) 0.3344(2) 0.0490(13) Uani 1 1 d . . . . .
C5 C 0.6034(5) 0.7809(4) 0.3734(2) 0.0452(12) Uani 1 1 d . . . . .
C6 C 0.4841(6) 0.8248(4) 0.3384(3) 0.0541(14) Uani 1 1 d . . . . .
H6 H 0.469801 0.825642 0.287294 0.065 Uiso 1 1 calc R U . . .
C7 C 0.3895(6) 0.8660(4) 0.3777(3) 0.0576(14) Uani 1 1 d . . . . .
H7 H 0.309616 0.893013 0.353581 0.069 Uiso 1 1 calc R U . . .
C8 C 0.4110(6) 0.8682(4) 0.4534(3) 0.0569(14) Uani 1 1 d . . . . .
H8 H 0.344985 0.896335 0.480122 0.068 Uiso 1 1 calc R U . . .
C9 C 0.5244(6) 0.8308(4) 0.4891(2) 0.0489(13) Uani 1 1 d . . . . .
H9 H 0.536788 0.834239 0.540441 0.059 Uiso 1 1 calc R U . . .
C10 C 0.6253(5) 0.7863(3) 0.4511(2) 0.0440(12) Uani 1 1 d . . . . .
C11 C 0.7448(5) 0.7466(3) 0.4873(2) 0.0423(11) Uani 1 1 d . . . . .
C12 C 0.8395(5) 0.6982(3) 0.4473(2) 0.0432(11) Uani 1 1 d . . . . .
C13 C 0.9603(6) 0.6590(4) 0.4823(3) 0.0505(13) Uani 1 1 d . . . . .
H13 H 0.978318 0.666271 0.533687 0.061 Uiso 1 1 calc R U . . .
C14 C 1.0507(6) 0.6112(4) 0.4432(3) 0.0561(14) Uani 1 1 d . . . . .
H14 H 1.131574 0.586708 0.467542 0.067 Uiso 1 1 calc R U . . .
C15 C 0.6754(7) 0.7314(5) 0.2531(3) 0.0601(15) Uani 1 1 d . . . . .
C16 C 0.7688(5) 0.7580(4) 0.5681(2) 0.0428(11) Uani 1 1 d . . . . .
C17 C 0.8351(5) 0.8634(4) 0.6069(2) 0.0440(11) Uani 1 1 d . . . . .
C18 C 0.8866(5) 0.9598(4) 0.5706(2) 0.0465(12) Uani 1 1 d . . . . .
H18 H 0.876628 0.952219 0.519234 0.056 Uiso 1 1 calc R U . . .
C19 C 0.9491(6) 1.0612(4) 0.6087(3) 0.0533(13) Uani 1 1 d . . . . .
H19 H 0.982203 1.123635 0.583816 0.064 Uiso 1 1 calc R U . . .
C20 C 0.9651(6) 1.0741(4) 0.6858(3) 0.0556(14) Uani 1 1 d . . . . .
H20 H 1.008968 1.145270 0.711862 0.067 Uiso 1 1 calc R U . . .
C21 C 0.9185(6) 0.9859(4) 0.7224(2) 0.0492(13) Uani 1 1 d . . . . .
H21 H 0.929298 0.996330 0.773741 0.059 Uiso 1 1 calc R U . . .
C22 C 0.8530(5) 0.8769(4) 0.6839(2) 0.0450(12) Uani 1 1 d . . . . .
C23 C 0.8054(6) 0.7836(4) 0.7216(2) 0.0481(12) Uani 1 1 d . . . . .
C24 C 0.7430(5) 0.6785(4) 0.6834(2) 0.0458(12) Uani 1 1 d . . . . .
C25 C 0.6893(6) 0.5849(4) 0.7201(2) 0.0519(13) Uani 1 1 d . . . . .
H25 H 0.699095 0.593641 0.771497 0.062 Uiso 1 1 calc R U . . .
C26 C 0.6246(6) 0.4839(4) 0.6826(3) 0.0564(14) Uani 1 1 d . . . . .
H26 H 0.590554 0.422792 0.708017 0.068 Uiso 1 1 calc R U . . .
C27 C 0.6079(6) 0.4693(4) 0.6063(3) 0.0508(13) Uani 1 1 d . . . . .
H27 H 0.563652 0.397881 0.580705 0.061 Uiso 1 1 calc R U . . .
C28 C 0.6554(6) 0.5581(4) 0.5689(2) 0.0472(12) Uani 1 1 d . . . . .
H28 H 0.642239 0.547893 0.517455 0.057 Uiso 1 1 calc R U . . .
C29 C 0.7242(5) 0.6657(4) 0.6061(2) 0.0430(11) Uani 1 1 d . . . . .
C30 C 0.8211(6) 0.7999(4) 0.8028(3) 0.0541(14) Uani 1 1 d . . . . .
C31 C 0.6164(8) 0.8645(9) 0.0609(3) 0.091(2) Uani 1 1 d . . . . .
H31A H 0.611876 0.949507 0.083068 0.109 Uiso 1 1 calc R U . . .
H31B H 0.538668 0.817279 0.069267 0.109 Uiso 1 1 calc R U . . .
C32 C 0.6167(8) 0.8654(7) -0.0203(3) 0.079(2) Uani 1 1 d . . . . .
H32A H 0.545978 0.810022 -0.047594 0.095 Uiso 1 1 calc R U . . .
H32B H 0.602586 0.949142 -0.034804 0.095 Uiso 1 1 calc R U . . .
C33 C 0.8497(8) 0.8834(7) 0.0880(3) 0.079(2) Uani 1 1 d . . . . .
H33A H 0.928931 0.841947 0.108095 0.095 Uiso 1 1 calc R U . . .
H33B H 0.848581 0.964495 0.115732 0.095 Uiso 1 1 calc R U . . .
C34 C 0.8522(8) 0.8998(6) 0.0073(3) 0.0723(18) Uani 1 1 d . . . . .
H34A H 0.840749 0.986887 -0.001445 0.087 Uiso 1 1 calc R U . . .
H34B H 0.936891 0.874719 -0.006384 0.087 Uiso 1 1 calc R U . . .
C35 C 0.7459(11) 0.6860(6) 0.0580(4) 0.093(2) Uani 1 1 d . . . . .
H35A H 0.666771 0.634998 0.059853 0.112 Uiso 1 1 calc R U . . .
H35B H 0.821819 0.646423 0.083602 0.112 Uiso 1 1 calc R U . . .
C36 C 0.7630(9) 0.6936(6) -0.0196(3) 0.080(2) Uani 1 1 d . . . . .
H36A H 0.851020 0.667649 -0.027079 0.097 Uiso 1 1 calc R U . . .
H36B H 0.697589 0.639011 -0.052037 0.097 Uiso 1 1 calc R U . . .
C37 C 0.5732(14) 0.1893(12) 1.2325(5) 0.105(4) Uani 0.8 1 d . . P B 2
H37A H 0.556287 0.117961 1.195589 0.126 Uiso 0.8 1 calc R U P B 2
H37B H 0.506937 0.250493 1.219804 0.126 Uiso 0.8 1 calc R U P B 2
C38 C 0.5601(14) 0.1494(13) 1.3048(9) 0.135(5) Uani 0.8 1 d . . P B 2
H38A H 0.556433 0.058833 1.302738 0.161 Uiso 0.8 1 calc R U P B 2
H38B H 0.479548 0.180707 1.320937 0.161 Uiso 0.8 1 calc R U P B 2
C39 C 0.682(2) 0.3523(12) 1.2746(9) 0.185(9) Uani 0.8 1 d . . P B 2
H39A H 0.602950 0.393648 1.254883 0.221 Uiso 0.8 1 calc R U P B 2
H39B H 0.758865 0.406701 1.272441 0.221 Uiso 0.8 1 calc R U P B 2
C40 C 0.6774(16) 0.3311(9) 1.3492(7) 0.127(5) Uani 0.8 1 d . . P B 2
H40A H 0.750094 0.377948 1.381079 0.152 Uiso 0.8 1 calc R U P B 2
H40B H 0.594571 0.361099 1.363002 0.152 Uiso 0.8 1 calc R U P B 2
C41 C 0.8017(9) 0.1666(9) 1.2559(5) 0.079(2) Uani 0.8 1 d . . P B 2
H41A H 0.884693 0.212853 1.255843 0.095 Uiso 0.8 1 calc R U P B 2
H41B H 0.800949 0.089145 1.224258 0.095 Uiso 0.8 1 calc R U P B 2
C42 C 0.7859(15) 0.1402(11) 1.3345(6) 0.127(5) Uani 0.8 1 d . . P B 2
H42A H 0.767430 0.051403 1.335281 0.153 Uiso 0.8 1 calc R U P B 2
H42B H 0.868731 0.162320 1.367224 0.153 Uiso 0.8 1 calc R U P B 2
C43 C 0.6908(9) 0.1537(8) 1.0319(8) 0.091(4) Uani 0.7 1 d . . P A 1
C44 C 0.7156(12) 0.2602(9) 1.0366(9) 0.100(3) Uani 0.7 1 d . . P A 1
C45 C 0.7628(18) 0.2514(14) 0.9052(12) 0.122(4) Uani 0.7 1 d . . P A 1
C46 C 0.8098(11) 0.3235(14) 0.8457(9) 0.158(5) Uani 1 1 d D . . . .
C47 C 0.9428(16) 0.3437(13) 0.8729(9) 0.053(4) Uani 0.3 1 d D . P A 2
H1A H 0.708(8) 0.800(7) 0.159(4) 0.10(2) Uiso 1 1 d . . . . .
C48 C 0.669(3) 0.089(2) 0.8233(12) 0.097(8) Uani 0.3 1 d D . P A 2
O9 O 0.865(2) 0.125(2) 0.8962(16) 0.147(9) Uani 0.3 1 d D . P A 2
C49 C 0.746(4) 0.170(3) 0.8570(17) 0.122(9) Uani 0.3 1 d D . P A 2
O10 O 0.708(2) 0.283(3) 0.874(2) 0.187(19) Uani 0.3 1 d D . P A 2
O11 O 0.638(2) 0.1518(15) 1.1539(8) 0.053(4) Uani 0.2 1 d . . P C 1


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C15 1.271(7) . ?
O1 H1A 1.31(8) . ?
O2 C15 1.222(7) . ?
O3 C30 1.253(7) . ?
O3 H3A 1.40(7) . ?
O4 C30 1.222(7) . ?
O5 C44 1.280(16) . ?
O6 C44 1.531(18) . ?
O6 C45 1.54(2) . ?
N1 C31 1.452(9) . ?
N1 C33 1.462(9) . ?
N1 C35 1.483(9) . ?
N1 H1A 1.28(8) . ?
N2 C34 1.467(8) . ?
N2 C32 1.488(9) . ?
N2 C36 1.491(8) . ?
N3 C37 1.338(15) . ?
N3 C39 1.440(16) . ?
N3 C41 1.442(11) . ?
N4 C42 1.381(14) . ?
N4 C40 1.418(15) . ?
N4 C38 1.61(2) . ?
C1 C2 1.353(8) . ?
C1 C14 1.415(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.446(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.413(8) . ?
C3 C12 1.430(6) . ?
C4 C5 1.389(7) . ?
C4 C15 1.509(7) . ?
C5 C6 1.427(8) . ?
C5 C10 1.437(6) . ?
C6 C7 1.374(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.403(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.354(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.424(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.420(7) . ?
C11 C12 1.409(7) . ?
C11 C16 1.492(6) . ?
C12 C13 1.420(7) . ?
C13 C14 1.362(7) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C16 C29 1.400(6) . ?
C16 C17 1.414(7) . ?
C17 C22 1.424(6) . ?
C17 C18 1.443(6) . ?
C18 C19 1.360(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.424(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.358(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.438(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.417(7) . ?
C23 C24 1.391(7) . ?
C23 C30 1.503(6) . ?
C24 C29 1.427(6) . ?
C24 C25 1.435(7) . ?
C25 C26 1.362(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.409(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.378(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.432(7) . ?
C28 H28 0.9500 . ?
C31 C32 1.525(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.547(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.503(9) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.488(18) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.449(18) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.561(16) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.183(14) . ?
C45 C46 1.56(2) . ?
C46 O10 1.337(17) . ?
C46 C47 1.40(2) . ?
C48 C49 1.246(19) . ?
O9 C49 1.46(4) . ?
C49 O10 1.34(4) . ?

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
C15 O1 H1A 106(4) . . ?
C30 O3 H3A 109(3) . . ?
C44 O6 C45 114.3(10) . . ?
C31 N1 C33 110.8(6) . . ?
C31 N1 C35 109.8(6) . . ?
C33 N1 C35 107.6(6) . . ?
C31 N1 H1A 102(4) . . ?
C33 N1 H1A 117(4) . . ?
C35 N1 H1A 109(4) . . ?
C34 N2 C32 111.0(5) . . ?
C34 N2 C36 108.8(5) . . ?
C32 N2 C36 110.3(6) . . ?
C37 N3 C39 99.3(11) . . ?
C37 N3 C41 117.0(10) . . ?
C39 N3 C41 115.1(11) . . ?
C42 N4 C40 119.1(12) . . ?
C42 N4 C38 102.2(10) . . ?
C40 N4 C38 100.5(9) . . ?
C2 C1 C14 120.5(5) . . ?
C2 C1 H1 119.7 . . ?
C14 C1 H1 119.7 . . ?
C1 C2 C3 120.9(4) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C4 C3 C12 119.6(4) . . ?
C4 C3 C2 122.5(4) . . ?
C12 C3 C2 117.9(5) . . ?
C5 C4 C3 121.1(4) . . ?
C5 C4 C15 119.3(5) . . ?
C3 C4 C15 119.5(5) . . ?
C4 C5 C6 121.9(4) . . ?
C4 C5 C10 119.7(5) . . ?
C6 C5 C10 118.4(5) . . ?
C7 C6 C5 121.0(4) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C8 119.9(5) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 121.2(5) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 121.2(4) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C11 C10 C9 122.2(4) . . ?
C11 C10 C5 119.5(4) . . ?
C9 C10 C5 118.2(4) . . ?
C12 C11 C10 120.2(4) . . ?
C12 C11 C16 120.8(4) . . ?
C10 C11 C16 119.0(4) . . ?
C11 C12 C13 121.3(4) . . ?
C11 C12 C3 119.7(4) . . ?
C13 C12 C3 119.0(4) . . ?
C14 C13 C12 120.9(5) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C1 120.7(5) . . ?
C13 C14 H14 119.7 . . ?
C1 C14 H14 119.7 . . ?
O2 C15 O1 124.7(5) . . ?
O2 C15 C4 120.9(5) . . ?
O1 C15 C4 114.4(5) . . ?
C29 C16 C17 119.5(4) . . ?
C29 C16 C11 120.5(4) . . ?
C17 C16 C11 120.0(4) . . ?
C16 C17 C22 120.1(4) . . ?
C16 C17 C18 121.9(4) . . ?
C22 C17 C18 118.0(4) . . ?
C19 C18 C17 121.2(4) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C20 120.2(5) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C21 C20 C19 120.8(4) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 120.5(4) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C23 C22 C17 119.7(4) . . ?
C23 C22 C21 121.0(4) . . ?
C17 C22 C21 119.3(4) . . ?
C24 C23 C22 120.1(4) . . ?
C24 C23 C30 120.3(4) . . ?
C22 C23 C30 119.5(4) . . ?
C23 C24 C29 120.0(4) . . ?
C23 C24 C25 121.2(4) . . ?
C29 C24 C25 118.7(4) . . ?
C26 C25 C24 121.1(4) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C27 120.6(5) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C28 C27 C26 120.2(4) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 121.1(4) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 119.4 . . ?
C16 C29 C24 120.6(4) . . ?
C16 C29 C28 121.1(4) . . ?
C24 C29 C28 118.3(4) . . ?
O4 C30 O3 123.9(5) . . ?
O4 C30 C23 120.7(5) . . ?
O3 C30 C23 115.4(5) . . ?
N1 C31 C32 110.4(6) . . ?
N1 C31 H31A 109.6 . . ?
C32 C31 H31A 109.6 . . ?
N1 C31 H31B 109.6 . . ?
C32 C31 H31B 109.6 . . ?
H31A C31 H31B 108.1 . . ?
N2 C32 C31 107.8(5) . . ?
N2 C32 H32A 110.1 . . ?
C31 C32 H32A 110.1 . . ?
N2 C32 H32B 110.1 . . ?
C31 C32 H32B 110.1 . . ?
H32A C32 H32B 108.5 . . ?
N1 C33 C34 109.5(5) . . ?
N1 C33 H33A 109.8 . . ?
C34 C33 H33A 109.8 . . ?
N1 C33 H33B 109.8 . . ?
C34 C33 H33B 109.8 . . ?
H33A C33 H33B 108.2 . . ?
N2 C34 C33 108.0(5) . . ?
N2 C34 H34A 110.1 . . ?
C33 C34 H34A 110.1 . . ?
N2 C34 H34B 110.1 . . ?
C33 C34 H34B 110.1 . . ?
H34A C34 H34B 108.4 . . ?
N1 C35 C36 110.6(5) . . ?
N1 C35 H35A 109.5 . . ?
C36 C35 H35A 109.5 . . ?
N1 C35 H35B 109.5 . . ?
C36 C35 H35B 109.5 . . ?
H35A C35 H35B 108.1 . . ?
N2 C36 C35 108.0(5) . . ?
N2 C36 H36A 110.1 . . ?
C35 C36 H36A 110.1 . . ?
N2 C36 H36B 110.1 . . ?
C35 C36 H36B 110.1 . . ?
H36A C36 H36B 108.4 . . ?
N3 C37 C38 111.8(11) . . ?
N3 C37 H37A 109.3 . . ?
C38 C37 H37A 109.3 . . ?
N3 C37 H37B 109.3 . . ?
C38 C37 H37B 109.3 . . ?
H37A C37 H37B 107.9 . . ?
C37 C38 N4 106.5(10) . . ?
C37 C38 H38A 110.4 . . ?
N4 C38 H38A 110.4 . . ?
C37 C38 H38B 110.4 . . ?
N4 C38 H38B 110.4 . . ?
H38A C38 H38B 108.6 . . ?
N3 C39 C40 110.7(9) . . ?
N3 C39 H39A 109.5 . . ?
C40 C39 H39A 109.5 . . ?
N3 C39 H39B 109.5 . . ?
C40 C39 H39B 109.5 . . ?
H39A C39 H39B 108.1 . . ?
N4 C40 C39 111.4(8) . . ?
N4 C40 H40A 109.3 . . ?
C39 C40 H40A 109.3 . . ?
N4 C40 H40B 109.3 . . ?
C39 C40 H40B 109.3 . . ?
H40A C40 H40B 108.0 . . ?
N3 C41 C42 105.5(7) . . ?
N3 C41 H41A 110.6 . . ?
C42 C41 H41A 110.6 . . ?
N3 C41 H41B 110.6 . . ?
C42 C41 H41B 110.6 . . ?
H41A C41 H41B 108.8 . . ?
N4 C42 C41 112.1(8) . . ?
N4 C42 H42A 109.2 . . ?
C41 C42 H42A 109.2 . . ?
N4 C42 H42B 109.2 . . ?
C41 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
C43 C44 O5 120.7(14) . . ?
C43 C44 O6 125.5(14) . . ?
O5 C44 O6 113.7(9) . . ?
O6 C45 C46 113.7(13) . . ?
O10 C46 C47 133(2) . . ?
C48 C49 O10 122(3) . . ?
C48 C49 O9 115(3) . . ?
O10 C49 O9 120(3) . . ?
C46 O10 C49 87(2) . . ?

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
C14 C1 C2 C3 0.2(8) . . . . ?
C1 C2 C3 C4 177.5(5) . . . . ?
C1 C2 C3 C12 -2.2(7) . . . . ?
C12 C3 C4 C5 -2.2(7) . . . . ?
C2 C3 C4 C5 178.0(4) . . . . ?
C12 C3 C4 C15 175.3(4) . . . . ?
C2 C3 C4 C15 -4.5(7) . . . . ?
C3 C4 C5 C6 -179.6(4) . . . . ?
C15 C4 C5 C6 2.8(7) . . . . ?
C3 C4 C5 C10 -0.3(7) . . . . ?
C15 C4 C5 C10 -177.8(4) . . . . ?
C4 C5 C6 C7 176.3(4) . . . . ?
C10 C5 C6 C7 -3.1(7) . . . . ?
C5 C6 C7 C8 1.6(8) . . . . ?
C6 C7 C8 C9 0.3(8) . . . . ?
C7 C8 C9 C10 -0.9(8) . . . . ?
C8 C9 C10 C11 -180.0(5) . . . . ?
C8 C9 C10 C5 -0.6(7) . . . . ?
C4 C5 C10 C11 2.5(6) . . . . ?
C6 C5 C10 C11 -178.1(4) . . . . ?
C4 C5 C10 C9 -176.9(4) . . . . ?
C6 C5 C10 C9 2.5(6) . . . . ?
C9 C10 C11 C12 177.2(4) . . . . ?
C5 C10 C11 C12 -2.2(6) . . . . ?
C9 C10 C11 C16 -3.4(6) . . . . ?
C5 C10 C11 C16 177.3(4) . . . . ?
C10 C11 C12 C13 179.3(4) . . . . ?
C16 C11 C12 C13 -0.1(6) . . . . ?
C10 C11 C12 C3 -0.3(6) . . . . ?
C16 C11 C12 C3 -179.7(4) . . . . ?
C4 C3 C12 C11 2.5(6) . . . . ?
C2 C3 C12 C11 -177.7(4) . . . . ?
C4 C3 C12 C13 -177.1(4) . . . . ?
C2 C3 C12 C13 2.6(6) . . . . ?
C11 C12 C13 C14 179.3(4) . . . . ?
C3 C12 C13 C14 -1.0(7) . . . . ?
C12 C13 C14 C1 -1.0(8) . . . . ?
C2 C1 C14 C13 1.5(8) . . . . ?
C5 C4 C15 O2 -81.1(7) . . . . ?
C3 C4 C15 O2 101.3(7) . . . . ?
C5 C4 C15 O1 97.9(6) . . . . ?
C3 C4 C15 O1 -79.7(6) . . . . ?
C12 C11 C16 C29 -94.7(6) . . . . ?
C10 C11 C16 C29 85.9(5) . . . . ?
C12 C11 C16 C17 86.3(5) . . . . ?
C10 C11 C16 C17 -93.1(6) . . . . ?
C29 C16 C17 C22 -1.8(7) . . . . ?
C11 C16 C17 C22 177.2(4) . . . . ?
C29 C16 C17 C18 178.2(4) . . . . ?
C11 C16 C17 C18 -2.8(7) . . . . ?
C16 C17 C18 C19 179.4(5) . . . . ?
C22 C17 C18 C19 -0.7(7) . . . . ?
C17 C18 C19 C20 0.1(8) . . . . ?
C18 C19 C20 C21 0.0(9) . . . . ?
C19 C20 C21 C22 0.6(8) . . . . ?
C16 C17 C22 C23 0.8(7) . . . . ?
C18 C17 C22 C23 -179.2(5) . . . . ?
C16 C17 C22 C21 -178.8(5) . . . . ?
C18 C17 C22 C21 1.3(7) . . . . ?
C20 C21 C22 C23 179.2(5) . . . . ?
C20 C21 C22 C17 -1.3(8) . . . . ?
C17 C22 C23 C24 0.8(8) . . . . ?
C21 C22 C23 C24 -179.6(5) . . . . ?
C17 C22 C23 C30 -178.2(5) . . . . ?
C21 C22 C23 C30 1.3(8) . . . . ?
C22 C23 C24 C29 -1.4(8) . . . . ?
C30 C23 C24 C29 177.7(5) . . . . ?
C22 C23 C24 C25 -177.5(5) . . . . ?
C30 C23 C24 C25 1.6(8) . . . . ?
C23 C24 C25 C26 177.9(5) . . . . ?
C29 C24 C25 C26 1.8(8) . . . . ?
C24 C25 C26 C27 -0.5(8) . . . . ?
C25 C26 C27 C28 -0.9(8) . . . . ?
C26 C27 C28 C29 1.0(8) . . . . ?
C17 C16 C29 C24 1.2(7) . . . . ?
C11 C16 C29 C24 -177.8(4) . . . . ?
C17 C16 C29 C28 179.3(4) . . . . ?
C11 C16 C29 C28 0.4(7) . . . . ?
C23 C24 C29 C16 0.4(7) . . . . ?
C25 C24 C29 C16 176.5(4) . . . . ?
C23 C24 C29 C28 -177.8(5) . . . . ?
C25 C24 C29 C28 -1.6(7) . . . . ?
C27 C28 C29 C16 -177.9(5) . . . . ?
C27 C28 C29 C24 0.3(7) . . . . ?
C24 C23 C30 O4 89.6(7) . . . . ?
C22 C23 C30 O4 -91.4(7) . . . . ?
C24 C23 C30 O3 -88.6(6) . . . . ?
C22 C23 C30 O3 90.5(7) . . . . ?
C33 N1 C31 C32 63.6(8) . . . . ?
C35 N1 C31 C32 -55.1(9) . . . . ?
C34 N2 C32 C31 -56.4(8) . . . . ?
C36 N2 C32 C31 64.2(8) . . . . ?
N1 C31 C32 N2 -6.7(9) . . . . ?
C31 N1 C33 C34 -55.4(7) . . . . ?
C35 N1 C33 C34 64.6(7) . . . . ?
C32 N2 C34 C33 63.9(7) . . . . ?
C36 N2 C34 C33 -57.6(7) . . . . ?
N1 C33 C34 N2 -7.0(8) . . . . ?
C31 N1 C35 C36 63.7(9) . . . . ?
C33 N1 C35 C36 -56.9(9) . . . . ?
C34 N2 C36 C35 65.9(8) . . . . ?
C32 N2 C36 C35 -56.1(8) . . . . ?
N1 C35 C36 N2 -6.8(10) . . . . ?
C39 N3 C37 C38 -71.8(13) . . . . ?
C41 N3 C37 C38 52.6(13) . . . . ?
N3 C37 C38 N4 11.0(14) . . . . ?
C42 N4 C38 C37 -67.6(12) . . . . ?
C40 N4 C38 C37 55.5(12) . . . . ?
C37 N3 C39 C40 68.6(17) . . . . ?
C41 N3 C39 C40 -57.2(19) . . . . ?
C42 N4 C40 C39 50.3(19) . . . . ?
C38 N4 C40 C39 -60.1(17) . . . . ?
N3 C39 C40 N4 2(2) . . . . ?
C37 N3 C41 C42 -56.8(11) . . . . ?
C39 N3 C41 C42 59.2(13) . . . . ?
C40 N4 C42 C41 -45.8(16) . . . . ?
C38 N4 C42 C41 63.7(13) . . . . ?
N3 C41 C42 N4 -8.3(15) . . . . ?
C45 O6 C44 C43 5(2) . . . . ?
C45 O6 C44 O5 -178.4(13) . . . . ?
C44 O6 C45 C46 -179.6(11) . . . . ?
C47 C46 O10 C49 -83(3) . . . . ?
C48 C49 O10 C46 -130(3) . . . . ?
O9 C49 O10 C46 70(4) . . . . ?

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
C36 H36B O8 0.99 2.35 3.322(11) 166.4 2_665 yes
C37^b H37B^b O3 0.99 2.65 3.176(15) 113.0 2_667 yes
N1 H1A O1 1.28(8) 1.31(8) 2.526(6) 154(7) . yes
N1 H1A O2 1.28(8) 2.33(8) 3.374(7) 136(5) . yes

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ayo3a_cu
_database_code_depnum_ccdc_archive 'CCDC 1952759'
loop_
_audit_author_name
_audit_author_address
'Misaki Okayasu'
;Toho University
Japan
;
_audit_update_record             
;
2019-09-11 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C42 H26 N2 O4'
_chemical_formula_moiety         'C42 H26 N2 O4'
_chemical_formula_weight         622.68
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_IT_number           61
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,-Z
3 -X,1/2+Y,1/2-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,+Z
7 +X,-1/2-Y,-1/2+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.1391(2)
_cell_length_b                   12.75610(12)
_cell_length_c                   38.9751(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     6035.20(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    32331
_cell_measurement_theta_min      4.25
_cell_measurement_theta_max      72.58
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2592.00
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_T_max  0.965

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            79408
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         4.291
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       46
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             5453
_reflns_number_gt                4986
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0954
_refine_ls_wR_factor_ref         0.2908
_refine_ls_wR_factor_gt          0.2882
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         5453
_refine_ls_number_parameters     441
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1361P)²+16.7077P] 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_diff_density_max         0.59
_refine_diff_density_min         -0.36
_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 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
O1 O 0.3860(2) 0.3022(2) 0.81799(7) 0.0333(7) Uani 1 1 d . . . . .
O2 O 0.3754(2) 0.4771(2) 0.81346(7) 0.0346(7) Uani 1 1 d . . . . .
O3 O 0.3623(2) 0.2246(2) 0.52809(7) 0.0351(7) Uani 1 1 d . . . . .
O4 O 0.3734(3) 0.3992(2) 0.52283(7) 0.0414(8) Uani 1 1 d . . . . .
N1 N 0.3805(2) 0.3191(2) 0.88729(8) 0.0256(7) Uani 1 1 d . . . . .
N2 N 0.3800(3) 0.2957(3) 0.95915(8) 0.0317(8) Uani 1 1 d . . . . .
C1 C 0.6245(3) 0.5349(3) 0.73777(11) 0.0315(9) Uani 1 1 d . . . . .
H1A H 0.6811 0.5748 0.7484 0.038 Uiso 1 1 calc R U . . .
C2 C 0.5485(3) 0.4841(3) 0.75743(10) 0.0295(8) Uani 1 1 d . . . . .
H2 H 0.5528 0.4893 0.7817 0.035 Uiso 1 1 calc R U . . .
C3 C 0.4626(3) 0.4232(3) 0.74230(10) 0.0257(8) Uani 1 1 d . . . . .
C4 C 0.3815(3) 0.3736(3) 0.76235(10) 0.0271(8) Uani 1 1 d . . . . .
C5 C 0.3000(3) 0.3099(3) 0.74673(10) 0.0269(8) Uani 1 1 d . . . . .
C6 C 0.2115(3) 0.2646(3) 0.76605(9) 0.0279(8) Uani 1 1 d . . . . .
H6 H 0.2073 0.2763 0.7901 0.033 Uiso 1 1 calc R U . . .
C7 C 0.1332(3) 0.2047(3) 0.75028(11) 0.0303(8) Uani 1 1 d . . . . .
H7 H 0.0739 0.1767 0.7633 0.036 Uiso 1 1 calc R U . . .
C8 C 0.1399(3) 0.1844(3) 0.71493(11) 0.0315(9) Uani 1 1 d . . . . .
H8 H 0.0865 0.1403 0.7045 0.038 Uiso 1 1 calc R U . . .
C9 C 0.2213(3) 0.2265(3) 0.69541(10) 0.0293(8) Uani 1 1 d . . . . .
H9 H 0.2245 0.2110 0.6716 0.035 Uiso 1 1 calc R U . . .
C10 C 0.3027(3) 0.2943(3) 0.71039(10) 0.0261(8) Uani 1 1 d . . . . .
C11 C 0.3812(3) 0.3472(3) 0.68996(9) 0.0256(8) Uani 1 1 d . . . . .
C12 C 0.4607(3) 0.4118(3) 0.70578(10) 0.0256(8) Uani 1 1 d . . . . .
C13 C 0.5404(3) 0.4686(3) 0.68593(10) 0.0299(8) Uani 1 1 d . . . . .
H13 H 0.5382 0.4645 0.6616 0.036 Uiso 1 1 calc R U . . .
C14 C 0.6192(3) 0.5282(3) 0.70145(11) 0.0313(9) Uani 1 1 d . . . . .
H14 H 0.6710 0.5656 0.6879 0.038 Uiso 1 1 calc R U . . .
C15 C 0.3807(3) 0.3906(3) 0.80014(10) 0.0284(8) Uani 1 1 d . . . . .
C16 C 0.3771(3) 0.3375(3) 0.65191(10) 0.0274(8) Uani 1 1 d . . . . .
C17 C 0.2920(3) 0.3886(3) 0.63316(10) 0.0280(8) Uani 1 1 d . . . . .
C18 C 0.2079(3) 0.4479(3) 0.65065(10) 0.0307(8) Uani 1 1 d . . . . .
H18 H 0.2113 0.4562 0.6748 0.037 Uiso 1 1 calc R U . . .
C19 C 0.1238(3) 0.4919(3) 0.63263(11) 0.0362(9) Uani 1 1 d . . . . .
H19 H 0.0682 0.5300 0.6444 0.043 Uiso 1 1 calc R U . . .
C20 C 0.1185(3) 0.4812(3) 0.59614(11) 0.0335(9) Uani 1 1 d . . . . .
H20 H 0.0589 0.5118 0.5839 0.040 Uiso 1 1 calc R U . . .
C21 C 0.1974(3) 0.4279(3) 0.57876(10) 0.0307(8) Uani 1 1 d . . . . .
H21 H 0.1926 0.4220 0.5545 0.037 Uiso 1 1 calc R U . . .
C22 C 0.2881(3) 0.3802(3) 0.59649(9) 0.0252(8) Uani 1 1 d . . . . .
C23 C 0.3700(3) 0.3237(3) 0.57889(9) 0.0251(8) Uani 1 1 d . . . . .
C24 C 0.4558(3) 0.2737(3) 0.59729(10) 0.0272(8) Uani 1 1 d . . . . .
C25 C 0.5432(3) 0.2190(3) 0.58007(10) 0.0295(8) Uani 1 1 d . . . . .
H25 H 0.5440 0.2164 0.5557 0.035 Uiso 1 1 calc R U . . .
C26 C 0.6252(3) 0.1708(3) 0.59820(11) 0.0320(9) Uani 1 1 d . . . . .
H26 H 0.6824 0.1350 0.5864 0.038 Uiso 1 1 calc R U . . .
C27 C 0.6253(3) 0.1738(3) 0.63444(11) 0.0317(9) Uani 1 1 d . . . . .
H27 H 0.6822 0.1393 0.6468 0.038 Uiso 1 1 calc R U . . .
C28 C 0.5445(3) 0.2257(3) 0.65187(10) 0.0301(8) Uani 1 1 d . . . . .
H28 H 0.5454 0.2262 0.6762 0.036 Uiso 1 1 calc R U . . .
C29 C 0.4581(3) 0.2795(3) 0.63393(10) 0.0267(8) Uani 1 1 d . . . . .
C30 C 0.3684(3) 0.3201(3) 0.54078(10) 0.0302(8) Uani 1 1 d . . . . .
C31 C 0.4576(3) 0.2618(3) 0.90333(9) 0.0250(8) Uani 1 1 d . . . . .
C32 C 0.5415(3) 0.2116(3) 0.88348(9) 0.0273(8) Uani 1 1 d . . . . .
H32 H 0.5427 0.2188 0.8592 0.033 Uiso 1 1 calc R U . . .
C33 C 0.6199(3) 0.1531(3) 0.89978(10) 0.0299(8) Uani 1 1 d . . . . .
H33 H 0.6758 0.1201 0.8866 0.036 Uiso 1 1 calc R U . . .
C34 C 0.6198(3) 0.1408(3) 0.93557(11) 0.0314(9) Uani 1 1 d . . . . .
H34 H 0.6756 0.0997 0.9461 0.038 Uiso 1 1 calc R U . . .
C35 C 0.5412(3) 0.1866(3) 0.95547(10) 0.0321(9) Uani 1 1 d . . . . .
H35 H 0.5417 0.1771 0.9796 0.039 Uiso 1 1 calc R U . . .
C36 C 0.4577(3) 0.2495(3) 0.93945(10) 0.0274(8) Uani 1 1 d . . . . .
C37 C 0.3039(3) 0.3554(3) 0.94305(10) 0.0287(8) Uani 1 1 d . . . . .
C38 C 0.2211(3) 0.4071(3) 0.96299(10) 0.0358(9) Uani 1 1 d . . . . .
H38 H 0.2209 0.4010 0.9873 0.043 Uiso 1 1 calc R U . . .
C39 C 0.1428(3) 0.4649(3) 0.94679(11) 0.0340(9) Uani 1 1 d . . . . .
H39 H 0.0875 0.4989 0.9600 0.041 Uiso 1 1 calc R U . . .
C40 C 0.1421(3) 0.4752(3) 0.91093(10) 0.0304(8) Uani 1 1 d . . . . .
H40 H 0.0858 0.5156 0.9004 0.036 Uiso 1 1 calc R U . . .
C41 C 0.2204(3) 0.4287(3) 0.89082(10) 0.0279(8) Uani 1 1 d . . . . .
H41 H 0.2195 0.4374 0.8666 0.033 Uiso 1 1 calc R U . . .
C42 C 0.3036(3) 0.3669(3) 0.90699(9) 0.0238(7) Uani 1 1 d . . . . .
H1 H 0.383(3) 0.311(3) 0.8432(11) 0.028(11) Uiso 1 1 d . . . . .
H3 H 0.367(3) 0.221(3) 0.5023(11) 0.030(11) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C15 1.326(5) . ?
O1 H1 0.99(4) . ?
O2 C15 1.221(5) . ?
O3 C30 1.317(5) . ?
O3 H3 1.01(4) . ?
O4 C30 1.230(5) . ?
N1 C31 1.342(5) . ?
N1 C42 1.354(5) . ?
N2 C36 1.352(5) . ?
N2 C37 1.352(5) . ?
C1 C2 1.363(5) . ?
C1 C14 1.419(6) . ?
C1 H1A 0.9500 . ?
C2 C3 1.427(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.407(5) . ?
C3 C12 1.431(5) . ?
C4 C5 1.417(5) . ?
C4 C15 1.489(5) . ?
C5 C10 1.431(5) . ?
C5 C6 1.434(5) . ?
C6 C7 1.366(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.404(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.358(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.437(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.413(5) . ?
C11 C12 1.411(5) . ?
C11 C16 1.489(5) . ?
C12 C13 1.434(5) . ?
C13 C14 1.364(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C16 C29 1.416(5) . ?
C16 C17 1.423(5) . ?
C17 C22 1.434(5) . ?
C17 C18 1.441(5) . ?
C18 C19 1.360(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.430(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.356(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.435(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.407(5) . ?
C23 C24 1.416(5) . ?
C23 C30 1.486(5) . ?
C24 C29 1.431(5) . ?
C24 C25 1.435(5) . ?
C25 C26 1.368(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.413(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.365(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.435(5) . ?
C28 H28 0.9500 . ?
C31 C36 1.416(5) . ?
C31 C32 1.431(5) . ?
C32 C33 1.366(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.404(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.361(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.436(5) . ?
C35 H35 0.9500 . ?
C37 C42 1.413(5) . ?
C37 C38 1.431(5) . ?
C38 C39 1.359(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.404(6) . ?
C39 H39 0.9500 . ?
C40 C41 1.368(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.427(5) . ?
C41 H41 0.9500 . ?

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
C15 O1 H1 115(3) . . ?
C30 O3 H3 114(2) . . ?
C31 N1 C42 117.5(3) . . ?
C36 N2 C37 117.3(3) . . ?
C2 C1 C14 120.1(3) . . ?
C2 C1 H1A 120.0 . . ?
C14 C1 H1A 120.0 . . ?
C1 C2 C3 121.4(4) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
C4 C3 C2 121.7(3) . . ?
C4 C3 C12 119.7(3) . . ?
C2 C3 C12 118.5(3) . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 C15 119.3(3) . . ?
C5 C4 C15 120.2(3) . . ?
C4 C5 C10 119.3(3) . . ?
C4 C5 C6 121.9(3) . . ?
C10 C5 C6 118.7(3) . . ?
C7 C6 C5 120.7(3) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C8 120.3(3) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 121.2(3) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 120.7(4) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C5 120.5(3) . . ?
C11 C10 C9 121.4(3) . . ?
C5 C10 C9 118.1(3) . . ?
C12 C11 C10 119.6(3) . . ?
C12 C11 C16 120.4(3) . . ?
C10 C11 C16 120.0(3) . . ?
C11 C12 C3 120.3(3) . . ?
C11 C12 C13 121.3(3) . . ?
C3 C12 C13 118.3(3) . . ?
C14 C13 C12 121.0(4) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C1 120.5(4) . . ?
C13 C14 H14 119.8 . . ?
C1 C14 H14 119.8 . . ?
O2 C15 O1 123.2(4) . . ?
O2 C15 C4 123.5(3) . . ?
O1 C15 C4 113.3(3) . . ?
C29 C16 C17 119.3(4) . . ?
C29 C16 C11 120.9(3) . . ?
C17 C16 C11 119.8(3) . . ?
C16 C17 C22 120.1(3) . . ?
C16 C17 C18 120.8(4) . . ?
C22 C17 C18 119.1(3) . . ?
C19 C18 C17 120.3(4) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 120.5(4) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C21 C20 C19 120.8(4) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 120.9(4) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C23 C22 C17 120.0(3) . . ?
C23 C22 C21 121.6(3) . . ?
C17 C22 C21 118.3(3) . . ?
C22 C23 C24 120.2(3) . . ?
C22 C23 C30 119.6(3) . . ?
C24 C23 C30 120.1(3) . . ?
C23 C24 C29 119.8(3) . . ?
C23 C24 C25 121.7(3) . . ?
C29 C24 C25 118.5(3) . . ?
C26 C25 C24 121.0(4) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C25 C26 C27 120.3(4) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C26 120.7(3) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 121.0(4) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C16 C29 C24 120.5(3) . . ?
C16 C29 C28 121.1(3) . . ?
C24 C29 C28 118.4(3) . . ?
O4 C30 O3 123.2(4) . . ?
O4 C30 C23 122.9(3) . . ?
O3 C30 C23 113.9(3) . . ?
N1 C31 C36 121.6(3) . . ?
N1 C31 C32 119.2(3) . . ?
C36 C31 C32 119.2(3) . . ?
C33 C32 C31 119.3(3) . . ?
C33 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
C32 C33 C34 121.5(3) . . ?
C32 C33 H33 119.2 . . ?
C34 C33 H33 119.2 . . ?
C35 C34 C33 121.3(3) . . ?
C35 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C34 C35 C36 119.1(4) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 H35 120.4 . . ?
N2 C36 C31 121.0(3) . . ?
N2 C36 C35 119.3(3) . . ?
C31 C36 C35 119.7(3) . . ?
N2 C37 C42 121.5(3) . . ?
N2 C37 C38 119.2(3) . . ?
C42 C37 C38 119.4(3) . . ?
C39 C38 C37 119.3(4) . . ?
C39 C38 H38 120.4 . . ?
C37 C38 H38 120.4 . . ?
C38 C39 C40 121.2(4) . . ?
C38 C39 H39 119.4 . . ?
C40 C39 H39 119.4 . . ?
C41 C40 C39 121.7(3) . . ?
C41 C40 H40 119.1 . . ?
C39 C40 H40 119.1 . . ?
C40 C41 C42 118.6(3) . . ?
C40 C41 H41 120.7 . . ?
C42 C41 H41 120.7 . . ?
N1 C42 C37 121.0(3) . . ?
N1 C42 C41 119.1(3) . . ?
C37 C42 C41 119.9(3) . . ?

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
C14 C1 C2 C3 0.2(5) . . . . ?
C1 C2 C3 C4 -177.6(3) . . . . ?
C1 C2 C3 C12 3.1(5) . . . . ?
C2 C3 C4 C5 -177.3(3) . . . . ?
C12 C3 C4 C5 2.0(5) . . . . ?
C2 C3 C4 C15 4.0(5) . . . . ?
C12 C3 C4 C15 -176.7(3) . . . . ?
C3 C4 C5 C10 1.5(5) . . . . ?
C15 C4 C5 C10 -179.7(3) . . . . ?
C3 C4 C5 C6 -175.3(3) . . . . ?
C15 C4 C5 C6 3.4(5) . . . . ?
C4 C5 C6 C7 179.0(3) . . . . ?
C10 C5 C6 C7 2.1(5) . . . . ?
C5 C6 C7 C8 1.7(5) . . . . ?
C6 C7 C8 C9 -2.5(6) . . . . ?
C7 C8 C9 C10 -0.6(6) . . . . ?
C4 C5 C10 C11 -4.1(5) . . . . ?
C6 C5 C10 C11 172.9(3) . . . . ?
C4 C5 C10 C9 177.9(3) . . . . ?
C6 C5 C10 C9 -5.1(5) . . . . ?
C8 C9 C10 C11 -173.5(3) . . . . ?
C8 C9 C10 C5 4.4(5) . . . . ?
C5 C10 C11 C12 3.0(5) . . . . ?
C9 C10 C11 C12 -179.1(3) . . . . ?
C5 C10 C11 C16 -174.8(3) . . . . ?
C9 C10 C11 C16 3.1(5) . . . . ?
C10 C11 C12 C3 0.6(5) . . . . ?
C16 C11 C12 C3 178.4(3) . . . . ?
C10 C11 C12 C13 -178.7(3) . . . . ?
C16 C11 C12 C13 -0.9(5) . . . . ?
C4 C3 C12 C11 -3.1(5) . . . . ?
C2 C3 C12 C11 176.2(3) . . . . ?
C4 C3 C12 C13 176.2(3) . . . . ?
C2 C3 C12 C13 -4.5(5) . . . . ?
C11 C12 C13 C14 -177.9(3) . . . . ?
C3 C12 C13 C14 2.8(5) . . . . ?
C12 C13 C14 C1 0.4(5) . . . . ?
C2 C1 C14 C13 -2.0(5) . . . . ?
C3 C4 C15 O2 56.3(5) . . . . ?
C5 C4 C15 O2 -122.4(4) . . . . ?
C3 C4 C15 O1 -123.8(4) . . . . ?
C5 C4 C15 O1 57.5(4) . . . . ?
C12 C11 C16 C29 73.3(5) . . . . ?
C10 C11 C16 C29 -108.9(4) . . . . ?
C12 C11 C16 C17 -105.6(4) . . . . ?
C10 C11 C16 C17 72.2(5) . . . . ?
C29 C16 C17 C22 0.6(5) . . . . ?
C11 C16 C17 C22 179.6(3) . . . . ?
C29 C16 C17 C18 179.7(3) . . . . ?
C11 C16 C17 C18 -1.4(5) . . . . ?
C16 C17 C18 C19 -176.6(3) . . . . ?
C22 C17 C18 C19 2.4(5) . . . . ?
C17 C18 C19 C20 -0.8(6) . . . . ?
C18 C19 C20 C21 -0.6(6) . . . . ?
C19 C20 C21 C22 0.4(6) . . . . ?
C16 C17 C22 C23 -1.6(5) . . . . ?
C18 C17 C22 C23 179.3(3) . . . . ?
C16 C17 C22 C21 176.5(3) . . . . ?
C18 C17 C22 C21 -2.5(5) . . . . ?
C20 C21 C22 C23 179.3(3) . . . . ?
C20 C21 C22 C17 1.2(5) . . . . ?
C17 C22 C23 C24 0.8(5) . . . . ?
C21 C22 C23 C24 -177.2(3) . . . . ?
C17 C22 C23 C30 -176.8(3) . . . . ?
C21 C22 C23 C30 5.1(5) . . . . ?
C22 C23 C24 C29 0.9(5) . . . . ?
C30 C23 C24 C29 178.6(3) . . . . ?
C22 C23 C24 C25 -177.4(3) . . . . ?
C30 C23 C24 C25 0.3(5) . . . . ?
C23 C24 C25 C26 -179.7(3) . . . . ?
C29 C24 C25 C26 1.9(5) . . . . ?
C24 C25 C26 C27 0.1(6) . . . . ?
C25 C26 C27 C28 -0.7(6) . . . . ?
C26 C27 C28 C29 -0.7(6) . . . . ?
C17 C16 C29 C24 1.2(5) . . . . ?
C11 C16 C29 C24 -177.8(3) . . . . ?
C17 C16 C29 C28 -179.2(3) . . . . ?
C11 C16 C29 C28 1.9(5) . . . . ?
C23 C24 C29 C16 -1.9(5) . . . . ?
C25 C24 C29 C16 176.4(3) . . . . ?
C23 C24 C29 C28 178.4(3) . . . . ?
C25 C24 C29 C28 -3.3(5) . . . . ?
C27 C28 C29 C16 -177.0(3) . . . . ?
C27 C28 C29 C24 2.7(5) . . . . ?
C22 C23 C30 O4 59.0(5) . . . . ?
C24 C23 C30 O4 -118.7(4) . . . . ?
C22 C23 C30 O3 -121.7(4) . . . . ?
C24 C23 C30 O3 60.7(4) . . . . ?
C42 N1 C31 C36 1.3(5) . . . . ?
C42 N1 C31 C32 -178.9(3) . . . . ?
N1 C31 C32 C33 -180.0(3) . . . . ?
C36 C31 C32 C33 -0.1(5) . . . . ?
C31 C32 C33 C34 0.3(6) . . . . ?
C32 C33 C34 C35 0.1(6) . . . . ?
C33 C34 C35 C36 -0.6(6) . . . . ?
C37 N2 C36 C31 -1.3(5) . . . . ?
C37 N2 C36 C35 179.1(3) . . . . ?
N1 C31 C36 N2 -0.2(5) . . . . ?
C32 C31 C36 N2 179.9(3) . . . . ?
N1 C31 C36 C35 179.4(3) . . . . ?
C32 C31 C36 C35 -0.4(5) . . . . ?
C34 C35 C36 N2 -179.6(4) . . . . ?
C34 C35 C36 C31 0.8(6) . . . . ?
C36 N2 C37 C42 1.6(5) . . . . ?
C36 N2 C37 C38 -179.0(4) . . . . ?
N2 C37 C38 C39 -178.3(4) . . . . ?
C42 C37 C38 C39 1.1(6) . . . . ?
C37 C38 C39 C40 -0.4(6) . . . . ?
C38 C39 C40 C41 -0.7(6) . . . . ?
C39 C40 C41 C42 1.0(6) . . . . ?
C31 N1 C42 C37 -0.9(5) . . . . ?
C31 N1 C42 C41 179.9(3) . . . . ?
N2 C37 C42 N1 -0.6(5) . . . . ?
C38 C37 C42 N1 -179.9(3) . . . . ?
N2 C37 C42 C41 178.6(3) . . . . ?
C38 C37 C42 C41 -0.7(5) . . . . ?
C40 C41 C42 N1 178.9(3) . . . . ?
C40 C41 C42 C37 -0.3(5) . . . . ?

#==============================================================================
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 N1 . . . 2.710(4) 0.990 1.721 177.0 no
O3 H3 N2 . . 7_565 2.708(4) 1.007 1.703 174.8 no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


