# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_260312wayama
_database_code_depnum_ccdc_archive 'CCDC 2519925'
loop_
_audit_author_name
_audit_author_address
'Wayama T.'
;The University of Tokyo
Japan
;
_audit_update_record             
;
2026-04-03 deposited with the CCDC.	2026-04-10 downloaded from the CCDC.
;
_audit_creation_date             2026-03-30
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_shelx_SHELXL_version_number     2019/3
loop_
_audit_author_email
toshiakiw@g.ecc.u-tokyo.ac.jp
_chemical_name_common            ?
_chemical_name_systematic        260312Wayama
_chemical_formula_moiety         'C28 H38 N2 O4'
_chemical_formula_sum            'C28 H38 N2 O4'
_chemical_formula_weight         466.60
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.507(2)
_cell_length_b                   13.541(2)
_cell_length_c                   14.653(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.641(6)
_cell_angle_gamma                90
_cell_volume                     2421.6(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1776
_cell_measurement_temperature    109.00
_cell_measurement_theta_max      20.47
_cell_measurement_theta_min      2.25
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.979
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.7138
_exptl_absorpt_correction_T_min  0.6673
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1381 before and 0.0964 after correction.
The Ratio of minimum to maximum transmission is 0.9349.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5.00 1.00 3.00 0.0200
-5.00 -1.00 4.00 0.0130
-3.00 -1.00 -4.00 0.1030
-2.00 5.00 -3.00 0.0680
0.00 -1.00 0.00 0.1240
1.00 -4.00 5.00 0.1320
1.00 5.00 1.00 0.0940
3.00 1.00 -3.00 0.0720
3.00 0.00 4.00 0.1010
5.00 -1.00 -3.00 0.0690
5.00 0.00 -4.00 0.0580

_exptl_crystal_preparation       'vapor diffusion'
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.116
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1661
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44522
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.093
_diffrn_reflns_theta_max         25.093
_diffrn_reflns_theta_min         1.942
_diffrn_ambient_temperature      109.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2534
_reflns_number_total             4296
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'APEX5 v2023.9-4 (Bruker, 2023)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4296
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0615
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0609P)²+3.3325P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1876
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C15-C17 \\sim C15-C16
 with sigma of 0.01
 C17-C18 \\sim C16-C18
 with sigma of 0.01
3. Others
 Sof(H15C)=Sof(H15D)=Sof(H18C)=Sof(H18D)=Sof(C16)=Sof(H16A)=Sof(H16B)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H18A)=Sof(H18B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C23(H23A,H23B), C15(H15A,H15B), C15(H15C,H15D), C28(H28A,H28B),
 C24(H24A,H24B), C25(H25A,H25B), C21(H21A,H21B), C17(H17A,H17B), C18(H18A,H18B),
  C18(H18C,H18D), C16(H16A,H16B)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C1(H1), C27(H27), C19(H19), C20(H20), C26(H26)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
O2 O 0.78815(17) 0.36798(17) 0.09444(16) 0.0327(6) Uani 1 1 d . . . . .
O1 O 0.64364(18) 0.44997(17) 0.00856(16) 0.0330(6) Uani 1 1 d . . . . .
O4 O 0.6606(2) 0.54600(18) 0.41225(16) 0.0375(6) Uani 1 1 d . . . . .
N1 N 0.4472(2) 0.3373(2) 0.18066(19) 0.0293(7) Uani 1 1 d . . . . .
O3 O 0.8237(2) 0.5530(2) 0.51453(19) 0.0529(8) Uani 1 1 d . . . . .
N2 N 0.9049(2) 0.2892(2) 0.3948(2) 0.0333(7) Uani 1 1 d . . . . .
C29 C 0.6783(3) 0.3916(2) 0.0713(2) 0.0258(7) Uani 1 1 d . . . . .
C13 C 0.5146(2) 0.3750(2) 0.1288(2) 0.0264(7) Uani 1 1 d . . . . .
H13 H 0.488462 0.429178 0.088915 0.032 Uiso 1 1 calc R U . . .
C14 C 0.6173(2) 0.3408(2) 0.1296(2) 0.0242(7) Uani 1 1 d . . . . .
C4 C 0.7256(3) 0.2929(2) 0.2886(2) 0.0264(8) Uani 1 1 d . . . . .
C3 C 0.7122(3) 0.3833(2) 0.3208(2) 0.0266(7) Uani 1 1 d . . . . .
H3 H 0.653678 0.423224 0.288251 0.032 Uiso 1 1 calc R U . . .
C8 C 0.6620(3) 0.2573(2) 0.1938(2) 0.0261(7) Uani 1 1 d . . . . .
H8 H 0.714310 0.219899 0.164017 0.031 Uiso 1 1 calc R U . . .
C10 C 0.4639(3) 0.2370(2) 0.2223(2) 0.0285(8) Uani 1 1 d . . . . .
C9 C 0.5647(3) 0.1884(2) 0.1962(2) 0.0280(8) Uani 1 1 d . . . . .
H9A H 0.590744 0.134790 0.241538 0.034 Uiso 1 1 calc R U . . .
H9B H 0.540929 0.157535 0.133775 0.034 Uiso 1 1 calc R U . . .
C1 C 0.8859(3) 0.3774(3) 0.4286(2) 0.0337(8) Uani 1 1 d . . . . .
H1 H 0.943518 0.410199 0.470708 0.040 Uiso 1 1 calc R U . . .
C2 C 0.7846(3) 0.4219(3) 0.4038(2) 0.0324(8) Uani 1 1 d . . . . .
C5 C 0.8077(3) 0.2256(2) 0.3531(2) 0.0300(8) Uani 1 1 d . . . . .
C22 C 0.7633(3) 0.5117(3) 0.4495(2) 0.0362(9) Uani 1 1 d . . . . .
C23 C 1.0183(3) 0.2642(3) 0.3916(3) 0.0371(9) Uani 1 1 d . . . . .
H23A H 1.030143 0.192840 0.404930 0.045 Uiso 1 1 calc R U . . .
H23B H 1.068680 0.301138 0.441469 0.045 Uiso 1 1 calc R U . . .
C11 C 0.4752(3) 0.2411(3) 0.3287(2) 0.0346(9) Uani 1 1 d . . . . .
H11A H 0.537832 0.282766 0.356726 0.052 Uiso 1 1 calc R U . . .
H11B H 0.486628 0.174268 0.354643 0.052 Uiso 1 1 calc R U . . .
H11C H 0.408177 0.268922 0.342660 0.052 Uiso 1 1 calc R U . . .
C15 C 0.3482(3) 0.3946(3) 0.1847(3) 0.0378(9) Uani 1 1 d D . . . .
H15A H 0.301085 0.354736 0.216693 0.045 Uiso 0.840(10) 1 calc R U P A 1
H15B H 0.306623 0.407409 0.120143 0.045 Uiso 0.840(10) 1 calc R U P A 1
H15C H 0.285528 0.348748 0.166545 0.045 Uiso 0.160(10) 1 calc R U P A 2
H15D H 0.340058 0.444711 0.134441 0.045 Uiso 0.160(10) 1 calc R U P A 2
C7 C 0.7592(3) 0.1894(3) 0.4353(2) 0.0375(9) Uani 1 1 d . . . . .
H7A H 0.814498 0.151184 0.478816 0.056 Uiso 1 1 calc R U . . .
H7B H 0.695210 0.147641 0.411298 0.056 Uiso 1 1 calc R U . . .
H7C H 0.736957 0.246409 0.467964 0.056 Uiso 1 1 calc R U . . .
C6 C 0.8420(3) 0.1359(3) 0.3047(3) 0.0370(9) Uani 1 1 d . . . . .
H6A H 0.874656 0.157304 0.253043 0.056 Uiso 1 1 calc R U . . .
H6B H 0.777642 0.094753 0.280284 0.056 Uiso 1 1 calc R U . . .
H6C H 0.895823 0.097634 0.349606 0.056 Uiso 1 1 calc R U . . .
C12 C 0.3640(3) 0.1722(3) 0.1807(3) 0.0408(9) Uani 1 1 d . . . . .
H12A H 0.299692 0.196683 0.201698 0.061 Uiso 1 1 calc R U . . .
H12B H 0.378795 0.103807 0.201623 0.061 Uiso 1 1 calc R U . . .
H12C H 0.349935 0.174756 0.112260 0.061 Uiso 1 1 calc R U . . .
C28 C 0.8533(3) 0.4099(3) 0.0356(3) 0.0416(10) Uani 1 1 d . . . . .
H28A H 0.829985 0.479156 0.021567 0.050 Uiso 1 1 calc R U . . .
H28B H 0.839009 0.373294 -0.024359 0.050 Uiso 1 1 calc R U . . .
C24 C 1.0468(3) 0.2873(3) 0.2979(3) 0.0454(10) Uani 1 1 d . . . . .
H24A H 1.020600 0.232422 0.254122 0.054 Uiso 1 1 calc R U . . .
H24B H 1.127522 0.290417 0.307046 0.054 Uiso 1 1 calc R U . . .
C25 C 0.9979(3) 0.3846(3) 0.2528(3) 0.0454(10) Uani 1 1 d . . . . .
H25A H 0.916945 0.381820 0.241645 0.054 Uiso 1 1 calc R U . . .
H25B H 1.023514 0.440231 0.295792 0.054 Uiso 1 1 calc R U . . .
C27 C 0.9728(3) 0.4085(3) 0.0763(3) 0.0469(11) Uani 1 1 d . . . . .
H27 H 1.016271 0.413693 0.030894 0.056 Uiso 1 1 calc R U . . .
C19 C 0.4244(4) 0.5833(3) 0.3874(3) 0.0488(11) Uani 1 1 d . . . . .
H19 H 0.352773 0.607581 0.385818 0.059 Uiso 1 1 calc R U . . .
C21 C 0.6252(4) 0.6330(3) 0.4526(3) 0.0493(11) Uani 1 1 d . . . . .
H21A H 0.652789 0.692078 0.425200 0.059 Uiso 1 1 calc R U . . .
H21B H 0.656631 0.633420 0.520748 0.059 Uiso 1 1 calc R U . . .
C20 C 0.5042(4) 0.6383(3) 0.4362(3) 0.0499(11) Uani 1 1 d . . . . .
H20 H 0.478611 0.692215 0.467004 0.060 Uiso 1 1 calc R U . . .
C26 C 1.0310(3) 0.4014(4) 0.1628(3) 0.0583(13) Uani 1 1 d . . . . .
H26 H 1.107802 0.408361 0.168389 0.070 Uiso 1 1 calc R U . . .
C17 C 0.3741(4) 0.4950(4) 0.2368(3) 0.0425(16) Uani 0.840(10) 1 d D . P A 1
H17A H 0.420909 0.534100 0.203884 0.051 Uiso 0.840(10) 1 calc R U P A 1
H17B H 0.304271 0.531489 0.230987 0.051 Uiso 0.840(10) 1 calc R U P A 1
C18 C 0.4276(4) 0.4915(4) 0.3354(4) 0.0653(14) Uani 1 1 d D . . . .
H18A H 0.505266 0.472798 0.340549 0.078 Uiso 0.840(10) 1 calc R U P A 1
H18B H 0.392900 0.438714 0.365584 0.078 Uiso 0.840(10) 1 calc R U P A 1
H18C H 0.455860 0.440010 0.382452 0.078 Uiso 0.160(10) 1 calc R U P A 2
H18D H 0.484264 0.500817 0.298332 0.078 Uiso 0.160(10) 1 calc R U P A 2
C16 C 0.3318(10) 0.4485(15) 0.2714(10) 0.024(6) Uiso 0.160(10) 1 d D . P A 2
H16A H 0.278701 0.502488 0.250590 0.028 Uiso 0.160(10) 1 calc R U P A 2
H16B H 0.296934 0.401777 0.307953 0.028 Uiso 0.160(10) 1 calc R U P A 2


_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
O2 C29 1.379(4) . ?
O2 C28 1.428(4) . ?
O1 C29 1.217(4) . ?
O4 C22 1.362(4) . ?
O4 C21 1.432(4) . ?
N1 C13 1.352(4) . ?
N1 C10 1.485(4) . ?
N1 C15 1.473(4) . ?
O3 C22 1.216(4) . ?
N2 C1 1.334(4) . ?
N2 C5 1.506(4) . ?
N2 C23 1.469(4) . ?
C29 C14 1.439(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.363(4) . ?
C14 C8 1.498(4) . ?
C4 C3 1.335(5) . ?
C4 C8 1.520(4) . ?
C4 C5 1.534(4) . ?
C3 H3 0.9500 . ?
C3 C2 1.446(4) . ?
C8 H8 1.0000 . ?
C8 C9 1.541(4) . ?
C10 C9 1.542(5) . ?
C10 C11 1.535(5) . ?
C10 C12 1.540(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C1 H1 0.9500 . ?
C1 C2 1.379(5) . ?
C2 C22 1.440(5) . ?
C5 C7 1.542(5) . ?
C5 C6 1.515(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.525(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 H15C 0.9900 . ?
C15 H15D 0.9900 . ?
C15 C17 1.559(6) . ?
C15 C16 1.517(10) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C27 1.483(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.539(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.484(6) . ?
C27 H27 0.9500 . ?
C27 C26 1.319(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.322(6) . ?
C19 C18 1.464(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C20 1.481(6) . ?
C20 H20 0.9500 . ?
C26 H26 0.9500 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.454(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 H18C 0.9900 . ?
C18 H18D 0.9900 . ?
C18 C16 1.471(10) . ?
C16 H16A 0.9900 . ?
C16 H16B 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
C29 O2 C28 115.4(3) . . ?
C22 O4 C21 117.8(3) . . ?
C13 N1 C10 121.8(3) . . ?
C13 N1 C15 117.1(3) . . ?
C15 N1 C10 120.6(3) . . ?
C1 N2 C5 118.0(3) . . ?
C1 N2 C23 118.0(3) . . ?
C23 N2 C5 123.7(3) . . ?
O2 C29 C14 111.8(3) . . ?
O1 C29 O2 120.5(3) . . ?
O1 C29 C14 127.7(3) . . ?
N1 C13 H13 117.7 . . ?
N1 C13 C14 124.6(3) . . ?
C14 C13 H13 117.7 . . ?
C29 C14 C8 124.1(3) . . ?
C13 C14 C29 116.9(3) . . ?
C13 C14 C8 118.9(3) . . ?
C3 C4 C8 122.1(3) . . ?
C3 C4 C5 116.5(3) . . ?
C8 C4 C5 121.4(3) . . ?
C4 C3 H3 119.2 . . ?
C4 C3 C2 121.6(3) . . ?
C2 C3 H3 119.2 . . ?
C14 C8 C4 112.6(3) . . ?
C14 C8 H8 107.4 . . ?
C14 C8 C9 106.4(2) . . ?
C4 C8 H8 107.4 . . ?
C4 C8 C9 115.4(3) . . ?
C9 C8 H8 107.4 . . ?
N1 C10 C9 109.7(3) . . ?
N1 C10 C11 110.9(3) . . ?
N1 C10 C12 109.3(3) . . ?
C11 C10 C9 111.7(3) . . ?
C11 C10 C12 108.0(3) . . ?
C12 C10 C9 107.1(3) . . ?
C8 C9 C10 116.1(3) . . ?
C8 C9 H9A 108.3 . . ?
C8 C9 H9B 108.3 . . ?
C10 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
N2 C1 H1 119.3 . . ?
N2 C1 C2 121.4(3) . . ?
C2 C1 H1 119.3 . . ?
C1 C2 C3 115.7(3) . . ?
C1 C2 C22 120.0(3) . . ?
C22 C2 C3 123.4(3) . . ?
N2 C5 C4 106.4(3) . . ?
N2 C5 C7 106.6(3) . . ?
N2 C5 C6 111.3(3) . . ?
C4 C5 C7 110.2(3) . . ?
C6 C5 C4 114.1(3) . . ?
C6 C5 C7 108.1(3) . . ?
O4 C22 C2 110.9(3) . . ?
O3 C22 O4 121.7(3) . . ?
O3 C22 C2 127.4(3) . . ?
N2 C23 H23A 108.9 . . ?
N2 C23 H23B 108.9 . . ?
N2 C23 C24 113.5(3) . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C15 H15A 108.9 . . ?
N1 C15 H15B 108.9 . . ?
N1 C15 H15C 106.4 . . ?
N1 C15 H15D 106.4 . . ?
N1 C15 C17 113.2(3) . . ?
N1 C15 C16 123.8(6) . . ?
H15A C15 H15B 107.8 . . ?
H15C C15 H15D 106.5 . . ?
C17 C15 H15A 108.9 . . ?
C17 C15 H15B 108.9 . . ?
C16 C15 H15C 106.4 . . ?
C16 C15 H15D 106.4 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C28 H28A 108.7 . . ?
O2 C28 H28B 108.7 . . ?
O2 C28 C27 114.2(3) . . ?
H28A C28 H28B 107.6 . . ?
C27 C28 H28A 108.7 . . ?
C27 C28 H28B 108.7 . . ?
C23 C24 H24A 108.6 . . ?
C23 C24 H24B 108.6 . . ?
C23 C24 C25 114.4(3) . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 H24A 108.6 . . ?
C25 C24 H24B 108.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C26 C25 C24 110.6(4) . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
C28 C27 H27 113.4 . . ?
C26 C27 C28 133.1(4) . . ?
C26 C27 H27 113.4 . . ?
C20 C19 H19 114.5 . . ?
C20 C19 C18 131.0(4) . . ?
C18 C19 H19 114.5 . . ?
O4 C21 H21A 109.3 . . ?
O4 C21 H21B 109.3 . . ?
O4 C21 C20 111.7(3) . . ?
H21A C21 H21B 107.9 . . ?
C20 C21 H21A 109.3 . . ?
C20 C21 H21B 109.3 . . ?
C19 C20 C21 133.1(4) . . ?
C19 C20 H20 113.4 . . ?
C21 C20 H20 113.4 . . ?
C25 C26 H26 114.3 . . ?
C27 C26 C25 131.4(4) . . ?
C27 C26 H26 114.3 . . ?
C15 C17 H17A 108.0 . . ?
C15 C17 H17B 108.0 . . ?
H17A C17 H17B 107.2 . . ?
C18 C17 C15 117.3(4) . . ?
C18 C17 H17A 108.0 . . ?
C18 C17 H17B 108.0 . . ?
C19 C18 H18A 108.4 . . ?
C19 C18 H18B 108.4 . . ?
C19 C18 H18C 106.4 . . ?
C19 C18 H18D 106.4 . . ?
C19 C18 C16 123.8(7) . . ?
C17 C18 C19 115.5(4) . . ?
C17 C18 H18A 108.4 . . ?
C17 C18 H18B 108.4 . . ?
H18A C18 H18B 107.5 . . ?
H18C C18 H18D 106.4 . . ?
C16 C18 H18C 106.4 . . ?
C16 C18 H18D 106.4 . . ?
C15 C16 H16A 107.6 . . ?
C15 C16 H16B 107.6 . . ?
C18 C16 C15 118.9(8) . . ?
C18 C16 H16A 107.6 . . ?
C18 C16 H16B 107.6 . . ?
H16A C16 H16B 107.0 . . ?

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
O2 C29 C14 C13 164.9(3) . . . . ?
O2 C29 C14 C8 -11.8(4) . . . . ?
O2 C28 C27 C26 -21.2(7) . . . . ?
O1 C29 C14 C13 -14.4(5) . . . . ?
O1 C29 C14 C8 168.9(3) . . . . ?
O4 C21 C20 C19 -5.4(7) . . . . ?
N1 C13 C14 C29 -178.6(3) . . . . ?
N1 C13 C14 C8 -1.8(5) . . . . ?
N1 C10 C9 C8 37.5(4) . . . . ?
N1 C15 C17 C18 -63.3(5) . . . . ?
N1 C15 C16 C18 33(2) . . . . ?
N2 C1 C2 C3 -17.5(5) . . . . ?
N2 C1 C2 C22 173.0(3) . . . . ?
N2 C23 C24 C25 39.4(4) . . . . ?
C29 O2 C28 C27 163.1(3) . . . . ?
C29 C14 C8 C4 85.3(4) . . . . ?
C29 C14 C8 C9 -147.4(3) . . . . ?
C13 N1 C10 C9 -0.3(4) . . . . ?
C13 N1 C10 C11 123.6(3) . . . . ?
C13 N1 C10 C12 -117.5(3) . . . . ?
C13 N1 C15 C17 -66.9(4) . . . . ?
C13 N1 C15 C16 -109.8(10) . . . . ?
C13 C14 C8 C4 -91.3(4) . . . . ?
C13 C14 C8 C9 36.1(4) . . . . ?
C14 C8 C9 C10 -54.2(3) . . . . ?
C4 C3 C2 C1 21.3(5) . . . . ?
C4 C3 C2 C22 -169.6(3) . . . . ?
C4 C8 C9 C10 71.4(4) . . . . ?
C3 C4 C8 C14 20.5(4) . . . . ?
C3 C4 C8 C9 -102.0(4) . . . . ?
C3 C4 C5 N2 -41.7(4) . . . . ?
C3 C4 C5 C7 73.5(4) . . . . ?
C3 C4 C5 C6 -164.8(3) . . . . ?
C3 C2 C22 O4 8.6(5) . . . . ?
C3 C2 C22 O3 -173.6(4) . . . . ?
C8 C4 C3 C2 -170.2(3) . . . . ?
C8 C4 C5 N2 139.1(3) . . . . ?
C8 C4 C5 C7 -105.7(3) . . . . ?
C8 C4 C5 C6 16.1(4) . . . . ?
C10 N1 C13 C14 -18.7(5) . . . . ?
C10 N1 C15 C17 120.4(3) . . . . ?
C10 N1 C15 C16 77.5(10) . . . . ?
C1 N2 C5 C4 46.4(4) . . . . ?
C1 N2 C5 C7 -71.2(4) . . . . ?
C1 N2 C5 C6 171.1(3) . . . . ?
C1 N2 C23 C24 -94.2(4) . . . . ?
C1 C2 C22 O4 177.3(3) . . . . ?
C1 C2 C22 O3 -5.0(6) . . . . ?
C5 N2 C1 C2 -18.3(5) . . . . ?
C5 N2 C23 C24 79.4(4) . . . . ?
C5 C4 C3 C2 10.6(5) . . . . ?
C5 C4 C8 C14 -160.4(3) . . . . ?
C5 C4 C8 C9 77.1(4) . . . . ?
C22 O4 C21 C20 -155.7(3) . . . . ?
C23 N2 C1 C2 155.6(3) . . . . ?
C23 N2 C5 C4 -127.2(3) . . . . ?
C23 N2 C5 C7 115.3(3) . . . . ?
C23 N2 C5 C6 -2.4(4) . . . . ?
C23 C24 C25 C26 179.3(3) . . . . ?
C11 C10 C9 C8 -86.0(3) . . . . ?
C15 N1 C13 C14 168.7(3) . . . . ?
C15 N1 C10 C9 172.0(3) . . . . ?
C15 N1 C10 C11 -64.1(4) . . . . ?
C15 N1 C10 C12 54.8(4) . . . . ?
C15 C17 C18 C19 -164.5(4) . . . . ?
C12 C10 C9 C8 156.0(3) . . . . ?
C28 O2 C29 O1 -4.9(4) . . . . ?
C28 O2 C29 C14 175.7(3) . . . . ?
C28 C27 C26 C25 5.3(9) . . . . ?
C24 C25 C26 C27 117.7(5) . . . . ?
C19 C18 C16 C15 145.5(11) . . . . ?
C21 O4 C22 O3 -0.3(5) . . . . ?
C21 O4 C22 C2 177.7(3) . . . . ?
C20 C19 C18 C17 -122.5(5) . . . . ?
C20 C19 C18 C16 -169.1(10) . . . . ?
C18 C19 C20 C21 4.4(8) . . . . ?

_olex2_exptl_crystal_mounting_method manual
_olex2_submission_original_sample_id 260312Wayama
_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_tw4_2_data02_04merged_c
_database_code_depnum_ccdc_archive 'CCDC 2519926'
loop_
_audit_author_name
_audit_author_address
'Sota Sato'
;JEOL and Institute for Molecular Science
Japan
;
_audit_update_record             
;
2026-04-03 deposited with the CCDC.	2026-04-10 downloaded from the CCDC.
;
_audit_creation_date             2026-04-02
_audit_creation_method           
;
Olex2 1.5-ac7-022
(compiled 2026.02.09 svn.ra45a96f9 for Rigaku Oxford Diffraction, GUI svn.r7493)
;
_shelx_SHELXL_version_number     2025/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H34 N2 O8'
_chemical_formula_sum            'C28 H34 N2 O8'
_chemical_formula_weight         526.57
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0058 0.0028 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0108 0.0056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0182 0.0102 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.609(7)
_cell_length_b                   7.549(2)
_cell_length_c                   17.523(5)
_cell_angle_alpha                90
_cell_angle_beta                 122.968(19)
_cell_angle_gamma                90
_cell_volume                     2620.1(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4019
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      32.830
_cell_measurement_theta_min      2.604
_shelx_estimated_absorpt_T_max   0.998
_shelx_estimated_absorpt_T_min   0.998
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29400
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        32.684
_diffrn_reflns_theta_max         32.830
_diffrn_reflns_theta_min         2.604
_diffrn_ambient_temperature      95.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Dectris Eiger X16M'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9000
_diffrn_source                   'KEK PF BL-17A'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1632
_reflns_number_total             2393
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'KEK UGUIS'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.5-ac7-022 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-022 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2025/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         2393
_refine_ls_number_restraints     364
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0672
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1299P)²+1.0029P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2240
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1C-C1A = N1D-C1B
 1.47 with sigma of 0.01
 C1A-C2A = C1B-C2B
 1.5 with sigma of 0.02
 C2A-O1A = C2B-O1B
 1.21 with sigma of 0.01
 C2A-O2A
 1.4 with sigma of 0.002
 C2B-O2B
 1.4 with sigma of 0.002
 O2A-C3A = O2B-C3B
 1.43 with sigma of 0.02
 C3A-C4A = C3B-C4B
 1.5 with sigma of 0.02
 C4A-C5A = C4B-C5B
 1.32 with sigma of 0.02
 C5A-C6A = C5B-C6B
 1.5 with sigma of 0.01
 C6A-O3A = C6B-O3B
 1.43 with sigma of 0.01
 O3A-C7A
 1.4 with sigma of 0.006
 O3B-C7B
 1.4 with sigma of 0.004
 C7A-O4A = C7B-O4B
 1.21 with sigma of 0.01
 C7A-C6D = C7B-C6C
 1.5 with sigma of 0.01
 C6A-C7A
 2.6 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1C \\sim C1A \\sim C2A \\sim O1A \\sim N1D \\sim C1B \\sim C2B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C6B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1A) = Uanis(O1B)
Uanis(O2A) = Uanis(O2B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C1A(0.5) H1AA(0.5) H1AB(0.5) C2A(0.5) O1A(0.5) O2A(0.5) C3A(0.5)
 H3AA(0.5) H3AB(0.5) C4A(0.5) H4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) H6AA(0.5)
 H6AB(0.5) O3A(0.5) C7A(0.5) O4A(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) C2B(0.5)
 O1B(0.5) O2B(0.5) C3B(0.5) H3BA(0.5) H3BB(0.5) C4B(0.5) H4B(0.5) C5B(0.5)
 H5B(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) O3B(0.5) C7B(0.5) O4B(0.5) N1C(0.5)
 C1C(0.5) C2C(0.5) H2CA(0.5) H2CB(0.5) H2CC(0.5) C3C(0.5) H3CA(0.5) H3CB(0.5)
 H3CC(0.5) C4C(0.5) H4CA(0.5) H4CB(0.5) C5C(0.5) H5C(0.5) C6C(0.5) C7C(0.5)
 H7C(0.5) N1D(0.5) C1D(0.5) C2D(0.5) H2DA(0.5) H2DB(0.5) H2DC(0.5) C3D(0.5)
 H3DA(0.5) H3DB(0.5) H3DC(0.5) C4D(0.5) C5D(0.5) H5D(0.5) C6D(0.5) C7D(0.5)
 H7D(0.5)
6.a Ternary CH refined with riding coordinates:
 C5C(H5C)
6.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C3A(H3AA,H3AB), C6A(H6AA,H6AB), C1B(H1BA,H1BB), C3B(H3BA,
 H3BB), C6B(H6BA,H6BB), C4C(H4CA,H4CB)
6.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C4B(H4B), C5B(H5B), C7C(H7C), C5D(H5D), C7D(H7D)
6.d Idealised Me refined as rotating group:
 C2C(H2CA,H2CB,H2CC), C3C(H3CA,H3CB,H3CC), C2D(H2DA,H2DB,H2DC), C3D(H3DA,H3DB,
 H3DC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1A C 0.6334(6) 0.6958(19) 0.1482(13) 0.083(3) Uani 0.5 1 d D U P A -1
H1AA H 0.659293 0.592297 0.148710 0.099 Uiso 0.5 1 calc R U P A -1
H1AB H 0.619433 0.762994 0.092130 0.099 Uiso 0.5 1 calc R U P A -1
C2A C 0.6821(5) 0.8097(16) 0.2251(7) 0.067(2) Uani 0.5 1 d D U P A -1
O1A O 0.7345(8) 0.863(2) 0.234(2) 0.086(3) Uani 0.5 1 d D U P A -1
O2A O 0.6600(4) 0.9178(12) 0.2684(6) 0.0769(14) Uani 0.5 1 d D . P A -1
C3A C 0.7052(8) 1.0469(18) 0.3346(11) 0.093(3) Uani 0.5 1 d D . P A -1
H3AA H 0.679272 1.132363 0.346833 0.112 Uiso 0.5 1 calc R U P A -1
H3AB H 0.728543 1.113131 0.310715 0.112 Uiso 0.5 1 calc R U P A -1
C4A C 0.7546(10) 0.955(3) 0.4184(13) 0.087(4) Uani 0.5 1 d D . P A -1
H4A H 0.789250 0.891841 0.418091 0.104 Uiso 0.5 1 calc R U P A -1
C5A C 0.7556(7) 0.952(2) 0.4925(11) 0.088(3) Uani 0.5 1 d D . P A -1
H5A H 0.789319 0.891797 0.545882 0.105 Uiso 0.5 1 calc R U P A -1
C6A C 0.6980(5) 1.0528(18) 0.4865(10) 0.096(4) Uani 0.5 1 d D . P A -1
H6AA H 0.706835 1.067672 0.548236 0.115 Uiso 0.5 1 calc R U P A -1
H6AB H 0.694765 1.172005 0.460901 0.115 Uiso 0.5 1 calc R U P A -1
O3A O 0.6340(4) 0.9578(9) 0.4287(6) 0.082(2) Uani 0.5 1 d D . P A -1
C7A C 0.5882(6) 0.930(2) 0.4553(9) 0.080(4) Uani 0.5 1 d D . P A -1
O4A O 0.5956(5) 1.0123(15) 0.5180(5) 0.105(4) Uani 0.5 1 d D . P A -1
C1B C 0.3698(7) 0.661(2) 0.3521(14) 0.085(3) Uani 0.5 1 d D U P A -1
H1BA H 0.381896 0.660650 0.415805 0.102 Uiso 0.5 1 calc R U P A -1
H1BB H 0.347952 0.546650 0.323207 0.102 Uiso 0.5 1 calc R U P A -1
C2B C 0.3245(6) 0.8143(17) 0.2999(7) 0.076(3) Uani 0.5 1 d D U P A -1
O1B O 0.2696(8) 0.846(2) 0.285(2) 0.086(3) Uani 0.5 1 d D . P A -1
O2B O 0.3478(4) 0.8681(15) 0.2456(6) 0.0769(14) Uani 0.5 1 d D . P A -1
C3B C 0.3127(9) 1.0195(19) 0.1895(11) 0.091(4) Uani 0.5 1 d D . P A -1
H3BA H 0.344779 1.090112 0.182186 0.109 Uiso 0.5 1 calc R U P A -1
H3BB H 0.297613 1.094554 0.221521 0.109 Uiso 0.5 1 calc R U P A -1
C4B C 0.2528(9) 0.976(3) 0.0972(12) 0.095(6) Uani 0.5 1 d D . P A -1
H4B H 0.211402 0.943840 0.090556 0.114 Uiso 0.5 1 calc R U P A -1
C5B C 0.2565(8) 0.981(3) 0.0263(13) 0.119(6) Uani 0.5 1 d D . P A -1
H5B H 0.213039 0.965652 -0.027496 0.143 Uiso 0.5 1 calc R U P A -1
C6B C 0.3092(5) 1.0052(14) 0.0030(8) 0.075(3) Uani 0.5 1 d D U P A -1
H6BA H 0.289832 0.980793 -0.062254 0.090 Uiso 0.5 1 calc R U P A -1
H6BB H 0.327693 1.127014 0.017072 0.090 Uiso 0.5 1 calc R U P A -1
O3B O 0.3614(3) 0.8754(7) 0.0605(6) 0.0742(19) Uani 0.5 1 d D . P A -1
C7B C 0.4215(5) 0.9107(16) 0.0658(9) 0.072(3) Uani 0.5 1 d D . P A -1
O4B O 0.4247(4) 1.0236(10) 0.0204(6) 0.0710(18) Uani 0.5 1 d D . P A -1
N1C N 0.5699(4) 0.6234(9) 0.1361(6) 0.0610(18) Uani 0.5 1 d D U P A -1
C1C C 0.5630(3) 0.4573(8) 0.1775(4) 0.0539(11) Uani 0.5 1 d . . P A -1
C2C C 0.6274(8) 0.473(3) 0.2845(9) 0.085(4) Uani 0.5 1 d . . P A -1
H2CA H 0.669387 0.443986 0.288335 0.127 Uiso 0.5 1 calc R U P A -1
H2CB H 0.620952 0.389851 0.322101 0.127 Uiso 0.5 1 calc R U P A -1
H2CC H 0.630088 0.593943 0.306362 0.127 Uiso 0.5 1 calc R U P A -1
C3C C 0.5795(3) 0.2966(7) 0.1385(4) 0.0652(13) Uani 0.5 1 d . . P A -1
H3CA H 0.555475 0.307986 0.072275 0.098 Uiso 0.5 1 calc R U P A -1
H3CB H 0.565171 0.187609 0.153757 0.098 Uiso 0.5 1 calc R U P A -1
H3CC H 0.628198 0.292142 0.164794 0.098 Uiso 0.5 1 calc R U P A -1
C4C C 0.4880(3) 0.4376(10) 0.1465(6) 0.0589(17) Uani 0.5 1 d . . P A -1
H4CA H 0.461893 0.397804 0.082306 0.071 Uiso 0.5 1 calc R U P A -1
H4CB H 0.484992 0.343084 0.183245 0.071 Uiso 0.5 1 calc R U P A -1
C5C C 0.4540(2) 0.6066(6) 0.1539(3) 0.0552(11) Uani 0.5 1 d . . P A -1
H5C H 0.404363 0.582715 0.117687 0.066 Uiso 0.5 1 calc R U P A -1
C6C C 0.4654(3) 0.7510(9) 0.1044(5) 0.0569(16) Uani 0.5 1 d D . P A -1
C7C C 0.5228(8) 0.7489(14) 0.1007(12) 0.059(2) Uani 0.5 1 d . . P A -1
H7C H 0.528882 0.844592 0.070545 0.071 Uiso 0.5 1 calc R U P A -1
N1D N 0.4305(5) 0.6923(12) 0.3479(7) 0.079(2) Uani 0.5 1 d D U P A -1
C1D C 0.4408(3) 0.5612(10) 0.2930(5) 0.0755(15) Uani 0.5 1 d . . P A -1
C2D C 0.4872(6) 0.4217(13) 0.3575(8) 0.090(3) Uani 0.5 1 d . . P A -1
H2DA H 0.529797 0.476589 0.404643 0.135 Uiso 0.5 1 calc R U P A -1
H2DB H 0.496211 0.333914 0.324148 0.135 Uiso 0.5 1 calc R U P A -1
H2DC H 0.466121 0.363353 0.385891 0.135 Uiso 0.5 1 calc R U P A -1
C3D C 0.3893(7) 0.460(3) 0.2279(12) 0.080(3) Uani 0.5 1 d . . P A -1
H3DA H 0.366004 0.402363 0.253429 0.119 Uiso 0.5 1 calc R U P A -1
H3DB H 0.407381 0.369875 0.206581 0.119 Uiso 0.5 1 calc R U P A -1
H3DC H 0.357321 0.535522 0.176681 0.119 Uiso 0.5 1 calc R U P A -1
C4D C 0.4726(2) 0.6560(6) 0.2487(3) 0.0562(11) Uani 0.5 1 d . . P A -1
C5D C 0.5190(2) 0.7811(6) 0.2986(3) 0.0585(11) Uani 0.5 1 d . . P A -1
H5D H 0.545113 0.831581 0.277833 0.070 Uiso 0.5 1 calc R U P A -1
C6D C 0.5287(4) 0.8374(10) 0.3820(5) 0.0639(18) Uani 0.5 1 d D . P A -1
C7D C 0.4794(8) 0.8103(16) 0.3954(11) 0.070(3) Uani 0.5 1 d . . P A -1
H7D H 0.478859 0.877694 0.440824 0.084 Uiso 0.5 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1A C2A 1.480(13) . ?
C1A N1C 1.498(8) . ?
C2A O1A 1.226(8) . ?
C2A O2A 1.394(2) . ?
O2A C3A 1.444(12) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C3A C4A 1.460(14) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.287(15) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.512(9) . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C6A O3A 1.469(8) . ?
O3A C7A 1.408(6) . ?
C7A O4A 1.191(8) . ?
C7A C6D 1.464(8) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C1B C2B 1.503(14) . ?
C1B N1D 1.493(9) . ?
C2B O1B 1.197(8) . ?
C2B O2B 1.394(2) . ?
O2B C3B 1.440(10) . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C3B C4B 1.495(15) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.293(14) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.517(9) . ?
C6B H6BA 0.9900 . ?
C6B H6BB 0.9900 . ?
C6B O3B 1.464(7) . ?
O3B C7B 1.396(4) . ?
C7B O4B 1.195(8) . ?
C7B C6C 1.491(8) . ?
N1C C1C 1.501(10) . ?
N1C C7C 1.329(13) . ?
C1C C2C 1.655(15) . ?
C1C C3C 1.541(8) . ?
C1C C4C 1.551(6) . ?
C2C H2CA 0.9800 . ?
C2C H2CB 0.9800 . ?
C2C H2CC 0.9800 . ?
C3C H3CA 0.9800 . ?
C3C H3CB 0.9800 . ?
C3C H3CC 0.9800 . ?
C4C H4CA 0.9900 . ?
C4C H4CB 0.9900 . ?
C4C C5C 1.550(8) . ?
C5C H5C 1.0000 . ?
C5C C6C 1.506(9) . ?
C5C C4D 1.515(7) . ?
C6C C7C 1.393(15) . ?
C7C H7C 0.9500 . ?
N1D C1D 1.489(12) . ?
N1D C7D 1.332(14) . ?
C1D C2D 1.497(12) . ?
C1D C3D 1.361(18) . ?
C1D C4D 1.521(8) . ?
C2D H2DA 0.9800 . ?
C2D H2DB 0.9800 . ?
C2D H2DC 0.9800 . ?
C3D H3DA 0.9800 . ?
C3D H3DB 0.9800 . ?
C3D H3DC 0.9800 . ?
C4D C5D 1.347(7) . ?
C5D H5D 0.9500 . ?
C5D C6D 1.415(9) . ?
C6D C7D 1.324(16) . ?
C7D H7D 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
H1AA C1A H1AB 106.4 . . ?
C2A C1A H1AA 106.3 . . ?
C2A C1A H1AB 106.3 . . ?
C2A C1A N1C 124.3(12) . . ?
N1C C1A H1AA 106.3 . . ?
N1C C1A H1AB 106.3 . . ?
O1A C2A C1A 122.4(11) . . ?
O1A C2A O2A 112.9(10) . . ?
O2A C2A C1A 120.0(8) . . ?
C2A O2A C3A 120.0(10) . . ?
O2A C3A H3AA 109.9 . . ?
O2A C3A H3AB 109.9 . . ?
O2A C3A C4A 108.9(15) . . ?
H3AA C3A H3AB 108.3 . . ?
C4A C3A H3AA 109.9 . . ?
C4A C3A H3AB 109.9 . . ?
C3A C4A H4A 116.9 . . ?
C5A C4A C3A 126.2(17) . . ?
C5A C4A H4A 116.9 . . ?
C4A C5A H5A 123.3 . . ?
C4A C5A C6A 113.4(15) . . ?
C6A C5A H5A 123.3 . . ?
C5A C6A H6AA 109.5 . . ?
C5A C6A H6AB 109.5 . . ?
H6AA C6A H6AB 108.1 . . ?
O3A C6A C5A 110.6(11) . . ?
O3A C6A H6AA 109.5 . . ?
O3A C6A H6AB 109.5 . . ?
C7A O3A C6A 122.3(7) . . ?
O3A C7A C6D 108.9(8) . . ?
O4A C7A O3A 118.1(9) . . ?
O4A C7A C6D 130.4(9) . . ?
H1BA C1B H1BB 109.1 . . ?
C2B C1B H1BA 111.1 . . ?
C2B C1B H1BB 111.1 . . ?
N1D C1B H1BA 111.1 . . ?
N1D C1B H1BB 111.1 . . ?
N1D C1B C2B 103.3(10) . . ?
O1B C2B C1B 127.9(9) . . ?
O1B C2B O2B 124.8(14) . . ?
O2B C2B C1B 103.1(9) . . ?
C2B O2B C3B 113.7(10) . . ?
O2B C3B H3BA 108.6 . . ?
O2B C3B H3BB 108.6 . . ?
O2B C3B C4B 114.7(14) . . ?
H3BA C3B H3BB 107.6 . . ?
C4B C3B H3BA 108.6 . . ?
C4B C3B H3BB 108.6 . . ?
C3B C4B H4B 119.5 . . ?
C5B C4B C3B 120.9(17) . . ?
C5B C4B H4B 119.5 . . ?
C4B C5B H5B 110.4 . . ?
C4B C5B C6B 139.2(17) . . ?
C6B C5B H5B 110.4 . . ?
C5B C6B H6BA 111.0 . . ?
C5B C6B H6BB 111.0 . . ?
H6BA C6B H6BB 109.0 . . ?
O3B C6B C5B 104.0(10) . . ?
O3B C6B H6BA 111.0 . . ?
O3B C6B H6BB 111.0 . . ?
C7B O3B C6B 111.2(7) . . ?
O3B C7B C6C 107.8(7) . . ?
O4B C7B O3B 121.4(9) . . ?
O4B C7B C6C 126.8(8) . . ?
C1A N1C C1C 126.8(10) . . ?
C7C N1C C1A 108.9(11) . . ?
C7C N1C C1C 122.6(9) . . ?
N1C C1C C2C 102.4(8) . . ?
N1C C1C C3C 108.9(5) . . ?
N1C C1C C4C 108.2(5) . . ?
C3C C1C C2C 105.1(7) . . ?
C3C C1C C4C 106.5(5) . . ?
C4C C1C C2C 125.0(7) . . ?
C1C C2C H2CA 109.5 . . ?
C1C C2C H2CB 109.5 . . ?
C1C C2C H2CC 109.5 . . ?
H2CA C2C H2CB 109.5 . . ?
H2CA C2C H2CC 109.5 . . ?
H2CB C2C H2CC 109.5 . . ?
C1C C3C H3CA 109.5 . . ?
C1C C3C H3CB 109.5 . . ?
C1C C3C H3CC 109.5 . . ?
H3CA C3C H3CB 109.5 . . ?
H3CA C3C H3CC 109.5 . . ?
H3CB C3C H3CC 109.5 . . ?
C1C C4C H4CA 108.3 . . ?
C1C C4C H4CB 108.3 . . ?
H4CA C4C H4CB 107.4 . . ?
C5C C4C C1C 115.9(5) . . ?
C5C C4C H4CA 108.3 . . ?
C5C C4C H4CB 108.3 . . ?
C4C C5C H5C 106.3 . . ?
C6C C5C C4C 106.5(5) . . ?
C6C C5C H5C 106.3 . . ?
C6C C5C C4D 114.7(4) . . ?
C4D C5C C4C 116.1(5) . . ?
C4D C5C H5C 106.3 . . ?
C7B C6C C5C 123.3(6) . . ?
C7C C6C C7B 116.2(8) . . ?
C7C C6C C5C 120.2(7) . . ?
N1C C7C C6C 125.0(12) . . ?
N1C C7C H7C 117.5 . . ?
C6C C7C H7C 117.5 . . ?
C1D N1D C1B 115.1(11) . . ?
C7D N1D C1B 127.2(13) . . ?
C7D N1D C1D 117.2(10) . . ?
N1D C1D C2D 106.9(7) . . ?
N1D C1D C4D 108.5(6) . . ?
C2D C1D C4D 110.7(5) . . ?
C3D C1D N1D 121.9(9) . . ?
C3D C1D C2D 101.1(10) . . ?
C3D C1D C4D 107.4(10) . . ?
C1D C2D H2DA 109.5 . . ?
C1D C2D H2DB 109.5 . . ?
C1D C2D H2DC 109.5 . . ?
H2DA C2D H2DB 109.5 . . ?
H2DA C2D H2DC 109.5 . . ?
H2DB C2D H2DC 109.5 . . ?
C1D C3D H3DA 109.5 . . ?
C1D C3D H3DB 109.5 . . ?
C1D C3D H3DC 109.5 . . ?
H3DA C3D H3DB 109.5 . . ?
H3DA C3D H3DC 109.5 . . ?
H3DB C3D H3DC 109.5 . . ?
C5C C4D C1D 121.0(4) . . ?
C5D C4D C5C 122.1(4) . . ?
C5D C4D C1D 116.8(5) . . ?
C4D C5D H5D 120.0 . . ?
C4D C5D C6D 119.9(5) . . ?
C6D C5D H5D 120.0 . . ?
C5D C6D C7A 126.1(7) . . ?
C7D C6D C7A 115.7(9) . . ?
C7D C6D C5D 118.2(9) . . ?
N1D C7D H7D 118.7 . . ?
C6D C7D N1D 122.6(13) . . ?
C6D C7D H7D 118.7 . . ?

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
C1A C2A O2A C3A -171.3(14) . . . . ?
C1A N1C C1C C2C 45.7(12) . . . . ?
C1A N1C C1C C3C -65.2(11) . . . . ?
C1A N1C C1C C4C 179.4(10) . . . . ?
C1A N1C C7C C6C -160.0(14) . . . . ?
C2A C1A N1C C1C -85.1(16) . . . . ?
C2A C1A N1C C7C 80.2(19) . . . . ?
C2A O2A C3A C4A -74.2(17) . . . . ?
O1A C2A O2A C3A -15(2) . . . . ?
O2A C3A C4A C5A -106(3) . . . . ?
C3A C4A C5A C6A 1(3) . . . . ?
C4A C5A C6A O3A 71(2) . . . . ?
C5A C6A O3A C7A 132.7(14) . . . . ?
C6A O3A C7A O4A 14(2) . . . . ?
C6A O3A C7A C6D 178.0(11) . . . . ?
O3A C7A C6D C5D 1.5(18) . . . . ?
O3A C7A C6D C7D -176.4(10) . . . . ?
C7A C6D C7D N1D -162.6(13) . . . . ?
O4A C7A C6D C5D 162.7(15) . . . . ?
O4A C7A C6D C7D -15(3) . . . . ?
C1B C2B O2B C3B -178.6(14) . . . . ?
C1B N1D C1D C2D -93.7(11) . . . . ?
C1B N1D C1D C3D 21.5(16) . . . . ?
C1B N1D C1D C4D 146.9(9) . . . . ?
C1B N1D C7D C6D -174.9(13) . . . . ?
C2B C1B N1D C1D -112.3(12) . . . . ?
C2B C1B N1D C7D 76.1(18) . . . . ?
C2B O2B C3B C4B -91.0(16) . . . . ?
O1B C2B O2B C3B 23(2) . . . . ?
O2B C3B C4B C5B -101(2) . . . . ?
C3B C4B C5B C6B 8(4) . . . . ?
C4B C5B C6B O3B 52(3) . . . . ?
C5B C6B O3B C7B -164.2(12) . . . . ?
C6B O3B C7B O4B -6.6(17) . . . . ?
C6B O3B C7B C6C -165.6(9) . . . . ?
O3B C7B C6C C5C -16.8(14) . . . . ?
O3B C7B C6C C7C 169.5(10) . . . . ?
C7B C6C C7C N1C 176.0(12) . . . . ?
O4B C7B C6C C5C -174.4(11) . . . . ?
O4B C7B C6C C7C 12.0(19) . . . . ?
N1C C1A C2A O1A 178.0(18) . . . . ?
N1C C1A C2A O2A -28(2) . . . . ?
N1C C1C C4C C5C -46.6(8) . . . . ?
C1C N1C C7C C6C 6.0(19) . . . . ?
C1C C4C C5C C6C 53.0(7) . . . . ?
C1C C4C C5C C4D -76.1(7) . . . . ?
C2C C1C C4C C5C 73.8(11) . . . . ?
C3C C1C C4C C5C -163.6(5) . . . . ?
C4C C5C C6C C7B 156.6(9) . . . . ?
C4C C5C C6C C7C -30.0(10) . . . . ?
C4C C5C C4D C1D -78.9(6) . . . . ?
C4C C5C C4D C5D 99.2(6) . . . . ?
C5C C6C C7C N1C 2.1(18) . . . . ?
C5C C4D C5D C6D 172.5(5) . . . . ?
C6C C5C C4D C1D 156.1(5) . . . . ?
C6C C5C C4D C5D -25.8(7) . . . . ?
C7C N1C C1C C2C -117.7(11) . . . . ?
C7C N1C C1C C3C 131.4(10) . . . . ?
C7C N1C C1C C4C 16.0(12) . . . . ?
N1D C1B C2B O1B 180(2) . . . . ?
N1D C1B C2B O2B 22.2(16) . . . . ?
N1D C1D C4D C5C -143.8(6) . . . . ?
N1D C1D C4D C5D 37.9(8) . . . . ?
C1D N1D C7D C6D 13.6(17) . . . . ?
C1D C4D C5D C6D -9.4(7) . . . . ?
C2D C1D C4D C5C 99.2(7) . . . . ?
C2D C1D C4D C5D -79.0(7) . . . . ?
C3D C1D C4D C5C -10.3(10) . . . . ?
C3D C1D C4D C5D 171.5(9) . . . . ?
C4D C5C C6C C7B -73.5(9) . . . . ?
C4D C5C C6C C7C 99.9(9) . . . . ?
C4D C5D C6D C7A 160.9(11) . . . . ?
C4D C5D C6D C7D -21.2(11) . . . . ?
C5D C6D C7D N1D 19.3(17) . . . . ?
C7D N1D C1D C2D 78.8(11) . . . . ?
C7D N1D C1D C3D -166.0(13) . . . . ?
C7D N1D C1D C4D -40.5(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT088_tw4_2_data02_04merged_c 
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.14 Note  
RESPONSE: This data was measured by the \w scan method 
along one rotation axis and this caused insufficient 
data / parameter ratio, even though two data were merged.
;
# end Validation Reply Form
