# Supplementary Information (SI) for RSC Mechanochemistry.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_DDD_a
_database_code_depnum_ccdc_archive 'CCDC 2358074'
loop_
_audit_author_name
_audit_author_address
'Lopamudra LOPAMUDRA GIRI'
;ICT Bhubaneswar
India
;
_audit_update_record             
;
2024-05-24 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H32 N5 O4, C7 H4 N O3 S'
_chemical_formula_sum            'C33 H36 N6 O7 S'
_chemical_formula_weight         660.74

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   8.8693(3)
_cell_length_b                   19.0166(7)
_cell_length_c                   19.9781(8)
_cell_angle_alpha                90
_cell_angle_beta                 101.4510(10)
_cell_angle_gamma                90
_cell_volume                     3302.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4510
_cell_measurement_theta_min      0.963
_cell_measurement_theta_max      0.977

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_F_000             1392.0
_exptl_transmission_factor_min   0.963
_exptl_transmission_factor_max   0.977
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.155
_shelx_estimated_absorpt_T_min   0.963
_shelx_estimated_absorpt_T_max   0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'Bruker D8 Venture photon 100 CMOS detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49152
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.367
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7599
_reflns_number_gt                4510
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SHELXL'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0507P)²+2.4455P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0187(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7577
_refine_ls_number_parameters     438
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1569
_refine_ls_wR_factor_gt          0.1163
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_restrained_S_all      0.971
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
S1 S 0.35038(8) 0.77111(4) 0.38770(4) 0.0647(2) Uani 1 1 d . . . . .
O2 O 0.1648(2) 0.74761(10) 1.09792(9) 0.0682(5) Uani 1 1 d . . . . .
N3 N 0.4015(2) 0.71430(10) 0.75936(9) 0.0485(5) Uani 1 1 d . . . . .
O7 O 0.2970(3) 0.54594(10) 0.65265(9) 0.0773(6) Uani 1 1 d . . . . .
N6 N 0.3499(3) 0.59933(10) 0.78611(10) 0.0532(5) Uani 1 1 d . . . . .
O4 O 0.4437(2) 0.83037(11) 0.41450(11) 0.0804(6) Uani 1 1 d . . . . .
O1 O 0.2626(3) 0.87243(10) 1.13224(9) 0.0790(6) Uani 1 1 d . . . . .
N2 N 0.4073(2) 0.80616(10) 0.83921(9) 0.0505(5) Uani 1 1 d . . . . .
O3 O 0.4502(3) 0.82691(10) 0.73270(10) 0.0787(6) Uani 1 1 d . . . . .
N5 N 0.3158(3) 0.63914(12) 0.58447(11) 0.0663(7) Uani 1 1 d . . . . .
C13 C 0.3651(3) 0.66655(12) 0.80457(11) 0.0448(5) Uani 1 1 d . . . . .
O5 O 0.1908(2) 0.78630(13) 0.36475(13) 0.0966(8) Uani 1 1 d . . . . .
C18 C 0.3477(3) 0.54326(12) 0.83440(11) 0.0477(6) Uani 1 1 d . . . . .
O6 O 0.4672(3) 0.59423(12) 0.44235(12) 0.0978(8) Uani 1 1 d . . . . .
N4 N 0.3382(3) 0.52798(13) 0.54529(11) 0.0816(8) Uani 1 1 d . . . . .
H4A H 0.337608 0.483022 0.549899 0.098 Uiso 1 1 calc R U . . .
H4B H 0.352095 0.546232 0.507595 0.098 Uiso 1 1 calc R U . . .
C9 C 0.3662(3) 0.76024(12) 0.88560(11) 0.0436(5) Uani 1 1 d . . . . .
C11 C 0.2654(3) 0.75150(12) 0.99347(12) 0.0483(6) Uani 1 1 d . . . . .
H11 H 0.226697 0.707140 0.980081 0.058 Uiso 1 1 calc R U . . .
C12 C 0.3454(3) 0.69107(12) 0.86855(11) 0.0453(5) Uani 1 1 d . . . . .
H12 H 0.317900 0.659659 0.899726 0.054 Uiso 1 1 calc R U . . .
C4 C 0.2426(3) 0.77943(13) 1.05416(12) 0.0507(6) Uani 1 1 d . . . . .
C23 C 0.4868(3) 0.51513(13) 0.86814(13) 0.0535(6) Uani 1 1 d . . . . .
C10 C 0.3464(3) 0.78903(12) 0.95149(11) 0.0452(5) Uani 1 1 d . . . . .
C5 C 0.2983(3) 0.84698(13) 1.07335(12) 0.0574(6) Uani 1 1 d . . . . .
N1 N 0.3749(3) 0.70592(13) 0.43972(12) 0.0696(6) Uani 1 1 d . . . . .
C15 C 0.4387(3) 0.69136(14) 0.69416(12) 0.0562(6) Uani 1 1 d . . . . .
H15A H 0.486776 0.645364 0.700099 0.067 Uiso 1 1 calc R U . . .
H15B H 0.511904 0.723934 0.681058 0.067 Uiso 1 1 calc R U . . .
C6 C 0.4079(3) 0.85431(13) 0.97251(13) 0.0544(6) Uani 1 1 d . . . . .
C19 C 0.2085(3) 0.51647(14) 0.84440(14) 0.0591(7) Uani 1 1 d . . . . .
C22 C 0.4817(3) 0.46135(14) 0.91455(13) 0.0611(7) Uani 1 1 d . . . . .
H22 H 0.574036 0.443269 0.938664 0.073 Uiso 1 1 calc R U . . .
C21 C 0.3471(4) 0.43367(14) 0.92651(13) 0.0625(7) Uani 1 1 d . . . . .
C14 C 0.4216(3) 0.78540(13) 0.77463(12) 0.0556(6) Uani 1 1 d . . . . .
C17 C 0.3176(3) 0.56963(14) 0.59691(13) 0.0622(7) Uani 1 1 d . . . . .
C27 C 0.4664(3) 0.66410(14) 0.34306(13) 0.0552(6) Uani 1 1 d . . . . .
C3 C 0.3828(3) 0.88250(13) 1.03346(13) 0.0626(7) Uani 1 1 d . . . . .
H3 H 0.423885 0.926284 1.047574 0.075 Uiso 1 1 calc R U . . .
C20 C 0.2126(4) 0.46170(16) 0.89111(15) 0.0701(8) Uani 1 1 d . . . . .
H20 H 0.120002 0.443447 0.898522 0.084 Uiso 1 1 calc R U . . .
C29 C 0.4230(3) 0.73079(13) 0.32129(13) 0.0549(6) Uani 1 1 d . . . . .
C16 C 0.2969(4) 0.68770(14) 0.63765(12) 0.0661(8) Uani 1 1 d . . . . .
H16A H 0.209545 0.673231 0.656844 0.079 Uiso 1 1 calc R U . . .
H16B H 0.275084 0.734145 0.618038 0.079 Uiso 1 1 calc R U . . .
C7 C 0.5023(4) 0.89145(15) 0.92881(14) 0.0714(8) Uani 1 1 d . . . . .
H7A H 0.506698 0.941251 0.939514 0.086 Uiso 1 1 calc R U . . .
H7B H 0.606534 0.873205 0.938612 0.086 Uiso 1 1 calc R U . . .
C8 C 0.4350(4) 0.88148(13) 0.85510(14) 0.0682(8) Uani 1 1 d . . . . .
H8A H 0.338747 0.907056 0.843496 0.082 Uiso 1 1 calc R U . . .
H8B H 0.504749 0.900262 0.827818 0.082 Uiso 1 1 calc R U . . .
C28 C 0.4368(3) 0.65147(15) 0.41306(14) 0.0643(7) Uani 1 1 d . . . . .
C30 C 0.4356(4) 0.75466(17) 0.25758(15) 0.0729(8) Uani 1 1 d . . . . .
H30 H 0.403765 0.799588 0.242708 0.087 Uiso 1 1 calc R U . . .
C33 C 0.5269(4) 0.61839(16) 0.30147(15) 0.0727(8) Uani 1 1 d . . . . .
H33 H 0.555218 0.572891 0.315774 0.087 Uiso 1 1 calc R U . . .
C2 C 0.1243(4) 0.67620(16) 1.08604(16) 0.0807(9) Uani 1 1 d . . . . .
H2A H 0.051775 0.671901 1.043653 0.121 Uiso 1 1 calc R U . . .
H2B H 0.078938 0.658855 1.122621 0.121 Uiso 1 1 calc R U . . .
H2C H 0.214781 0.649300 1.083790 0.121 Uiso 1 1 calc R U . . .
C31 C 0.4980(4) 0.7087(2) 0.21661(15) 0.0849(10) Uani 1 1 d . . . . .
H31 H 0.509074 0.723227 0.173405 0.102 Uiso 1 1 calc R U . . .
C32 C 0.5439(4) 0.64205(19) 0.23835(16) 0.0825(9) Uani 1 1 d . . . . .
H32 H 0.586935 0.612619 0.210032 0.099 Uiso 1 1 calc R U . . .
C25 C 0.6377(4) 0.53855(18) 0.85216(19) 0.0869(10) Uani 1 1 d . . . . .
H25A H 0.642956 0.524665 0.806473 0.130 Uiso 1 1 calc R U . . .
H25B H 0.720721 0.517154 0.883765 0.130 Uiso 1 1 calc R U . . .
H25C H 0.645859 0.588789 0.856027 0.130 Uiso 1 1 calc R U . . .
C26 C 0.3470(5) 0.37307(17) 0.97564(17) 0.0978(12) Uani 1 1 d . . . . .
H26A H 0.245713 0.367494 0.985138 0.147 Uiso 1 1 calc R U . . .
H26B H 0.418640 0.382625 1.017367 0.147 Uiso 1 1 calc R U . . .
H26C H 0.376505 0.330654 0.955566 0.147 Uiso 1 1 calc R U . . .
C1 C 0.2726(5) 0.94547(17) 1.14290(17) 0.0957(12) Uani 1 1 d . . . . .
H1A H 0.378352 0.959788 1.150142 0.144 Uiso 1 1 calc R U . . .
H1B H 0.230942 0.957311 1.182293 0.144 Uiso 1 1 calc R U . . .
H1C H 0.215188 0.969195 1.103558 0.144 Uiso 1 1 calc R U . . .
C24 C 0.0575(4) 0.5449(2) 0.8055(2) 0.1034(12) Uani 1 1 d . . . . .
H24A H 0.034468 0.588400 0.825747 0.155 Uiso 1 1 calc R U . . .
H24B H -0.022789 0.511529 0.807182 0.155 Uiso 1 1 calc R U . . .
H24C H 0.064851 0.552980 0.758812 0.155 Uiso 1 1 calc R U . . .
H71 H 0.344(3) 0.6543(16) 0.5484(16) 0.076(9) Uiso 1 1 d . . . . .
H80 H 0.344(3) 0.5870(15) 0.7418(15) 0.077(9) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0582(4) 0.0640(4) 0.0709(5) -0.0087(3) 0.0103(3) 0.0111(3)
O2 0.0975(15) 0.0615(11) 0.0575(11) -0.0069(9) 0.0439(10) -0.0098(10)
N3 0.0678(13) 0.0441(10) 0.0386(10) 0.0008(8) 0.0223(9) -0.0040(9)
O7 0.1334(19) 0.0582(11) 0.0462(10) 0.0010(9) 0.0323(11) -0.0044(11)
N6 0.0817(15) 0.0428(11) 0.0396(11) -0.0020(9) 0.0228(10) -0.0021(10)
O4 0.0842(15) 0.0636(12) 0.0884(15) -0.0214(11) 0.0052(11) 0.0023(11)
O1 0.1363(19) 0.0591(12) 0.0497(11) -0.0115(9) 0.0379(11) -0.0017(12)
N2 0.0717(13) 0.0413(10) 0.0431(10) -0.0009(8) 0.0227(9) -0.0063(9)
O3 0.1334(19) 0.0541(11) 0.0598(11) 0.0057(9) 0.0465(12) -0.0109(11)
N5 0.108(2) 0.0572(14) 0.0379(11) 0.0009(10) 0.0236(12) 0.0065(13)
C13 0.0539(14) 0.0442(12) 0.0392(11) 0.0009(9) 0.0163(10) -0.0022(10)
O5 0.0550(12) 0.1003(17) 0.129(2) -0.0129(15) 0.0051(12) 0.0239(12)
C18 0.0648(16) 0.0412(12) 0.0406(12) -0.0039(10) 0.0187(11) -0.0037(11)
O6 0.141(2) 0.0746(15) 0.0878(16) 0.0267(12) 0.0469(15) 0.0185(14)
N4 0.143(2) 0.0581(14) 0.0475(13) -0.0041(11) 0.0275(14) 0.0120(15)
C9 0.0476(13) 0.0442(12) 0.0417(12) -0.0001(9) 0.0154(10) -0.0043(10)
C11 0.0554(14) 0.0468(12) 0.0465(13) -0.0059(10) 0.0196(11) -0.0049(11)
C12 0.0551(14) 0.0447(12) 0.0401(12) 0.0001(10) 0.0191(10) -0.0048(10)
C4 0.0612(15) 0.0494(13) 0.0455(13) -0.0017(10) 0.0205(11) -0.0014(11)
C23 0.0606(16) 0.0485(13) 0.0541(14) -0.0050(11) 0.0175(12) -0.0071(12)
C10 0.0529(13) 0.0442(12) 0.0411(12) -0.0043(10) 0.0158(10) -0.0039(10)
C5 0.0812(18) 0.0525(14) 0.0401(13) -0.0053(11) 0.0160(12) -0.0004(13)
N1 0.0771(16) 0.0747(16) 0.0626(14) -0.0009(12) 0.0273(12) 0.0085(13)
C15 0.0801(18) 0.0535(14) 0.0426(13) -0.0013(11) 0.0303(12) -0.0015(13)
C6 0.0687(16) 0.0464(13) 0.0506(14) -0.0047(11) 0.0180(12) -0.0096(12)
C19 0.0594(16) 0.0595(16) 0.0605(16) 0.0026(13) 0.0172(13) -0.0047(13)
C22 0.0738(18) 0.0515(15) 0.0553(15) -0.0004(12) 0.0061(13) 0.0010(13)
C21 0.087(2) 0.0547(15) 0.0464(14) -0.0003(12) 0.0151(14) -0.0113(15)
C14 0.0764(18) 0.0492(14) 0.0461(13) 0.0034(11) 0.0244(12) -0.0044(12)
C17 0.088(2) 0.0575(16) 0.0430(14) -0.0021(12) 0.0176(13) 0.0063(14)
C27 0.0614(16) 0.0552(15) 0.0507(14) -0.0011(11) 0.0156(12) -0.0007(12)
C3 0.090(2) 0.0482(14) 0.0506(14) -0.0102(12) 0.0175(14) -0.0130(14)
C20 0.0726(19) 0.0694(18) 0.0737(19) 0.0069(15) 0.0275(16) -0.0209(15)
C29 0.0561(15) 0.0544(15) 0.0520(14) 0.0001(12) 0.0054(11) -0.0031(12)
C16 0.102(2) 0.0547(15) 0.0435(14) 0.0024(11) 0.0189(14) 0.0154(15)
C7 0.096(2) 0.0594(16) 0.0645(17) -0.0126(13) 0.0311(16) -0.0319(16)
C8 0.105(2) 0.0436(14) 0.0642(17) -0.0044(12) 0.0362(16) -0.0189(14)
C28 0.0755(19) 0.0620(17) 0.0590(16) 0.0063(13) 0.0220(14) 0.0058(14)
C30 0.086(2) 0.0685(18) 0.0591(17) 0.0090(14) 0.0036(15) -0.0073(16)
C33 0.093(2) 0.0621(17) 0.0676(18) -0.0083(14) 0.0265(16) 0.0010(16)
C2 0.114(3) 0.0677(19) 0.0743(19) -0.0081(15) 0.0535(19) -0.0219(18)
C31 0.104(3) 0.105(3) 0.0478(16) -0.0014(17) 0.0190(16) -0.028(2)
C32 0.106(3) 0.085(2) 0.0640(19) -0.0201(17) 0.0342(18) -0.010(2)
C25 0.067(2) 0.088(2) 0.110(3) 0.005(2) 0.0277(18) -0.0076(17)
C26 0.145(3) 0.073(2) 0.074(2) 0.0226(17) 0.020(2) -0.021(2)
C1 0.164(4) 0.0628(19) 0.0677(19) -0.0204(16) 0.040(2) 0.000(2)
C24 0.065(2) 0.122(3) 0.121(3) 0.029(3) 0.013(2) 0.000(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
S1 O5 1.428(2) . ?
S1 O4 1.437(2) . ?
S1 N1 1.605(3) . ?
S1 C29 1.762(3) . ?
O2 C4 1.359(3) . ?
O2 C2 1.413(3) . ?
N3 C13 1.364(3) . ?
N3 C14 1.390(3) . ?
N3 C15 1.472(3) . ?
O7 C17 1.248(3) . ?
N6 C13 1.330(3) . ?
N6 C18 1.441(3) . ?
O1 C5 1.366(3) . ?
O1 C1 1.405(3) . ?
N2 C9 1.374(3) . ?
N2 C14 1.379(3) . ?
N2 C8 1.477(3) . ?
O3 C14 1.214(3) . ?
N5 C17 1.344(3) . ?
N5 C16 1.442(3) . ?
C13 C12 1.404(3) . ?
C18 C19 1.386(3) . ?
C18 C23 1.390(4) . ?
O6 C28 1.240(3) . ?
N4 C17 1.342(3) . ?
C9 C12 1.362(3) . ?
C9 C10 1.468(3) . ?
C11 C4 1.375(3) . ?
C11 C10 1.403(3) . ?
C4 C5 1.402(3) . ?
C23 C22 1.387(4) . ?
C23 C25 1.504(4) . ?
C10 C6 1.387(3) . ?
C5 C3 1.374(4) . ?
N1 C28 1.332(3) . ?
C15 C16 1.516(4) . ?
C6 C3 1.388(3) . ?
C6 C7 1.501(3) . ?
C19 C20 1.394(4) . ?
C19 C24 1.509(4) . ?
C22 C21 1.368(4) . ?
C21 C20 1.369(4) . ?
C21 C26 1.514(4) . ?
C27 C29 1.371(4) . ?
C27 C33 1.382(4) . ?
C27 C28 1.493(4) . ?
C29 C30 1.377(4) . ?
C7 C8 1.487(4) . ?
C30 C31 1.386(5) . ?
C33 C32 1.375(4) . ?
C31 C32 1.374(5) . ?

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
O5 S1 O4 114.94(14) . . ?
O5 S1 N1 111.24(15) . . ?
O4 S1 N1 111.75(13) . . ?
O5 S1 C29 109.49(14) . . ?
O4 S1 C29 110.62(13) . . ?
N1 S1 C29 97.41(12) . . ?
C4 O2 C2 117.68(19) . . ?
C13 N3 C14 122.64(19) . . ?
C13 N3 C15 120.86(19) . . ?
C14 N3 C15 116.16(19) . . ?
C13 N6 C18 122.67(19) . . ?
C5 O1 C1 117.5(2) . . ?
C9 N2 C14 122.35(19) . . ?
C9 N2 C8 121.76(19) . . ?
C14 N2 C8 115.87(19) . . ?
C17 N5 C16 119.5(2) . . ?
N6 C13 N3 118.73(19) . . ?
N6 C13 C12 123.2(2) . . ?
N3 C13 C12 118.1(2) . . ?
C19 C18 C23 121.2(2) . . ?
C19 C18 N6 120.0(2) . . ?
C23 C18 N6 118.7(2) . . ?
C12 C9 N2 119.06(19) . . ?
C12 C9 C10 123.4(2) . . ?
N2 C9 C10 117.56(19) . . ?
C4 C11 C10 120.9(2) . . ?
C9 C12 C13 120.9(2) . . ?
O2 C4 C11 125.3(2) . . ?
O2 C4 C5 115.4(2) . . ?
C11 C4 C5 119.3(2) . . ?
C22 C23 C18 117.7(2) . . ?
C22 C23 C25 120.6(3) . . ?
C18 C23 C25 121.7(2) . . ?
C6 C10 C11 119.4(2) . . ?
C6 C10 C9 119.7(2) . . ?
C11 C10 C9 120.9(2) . . ?
O1 C5 C3 124.9(2) . . ?
O1 C5 C4 115.5(2) . . ?
C3 C5 C4 119.7(2) . . ?
C28 N1 S1 110.80(19) . . ?
N3 C15 C16 112.0(2) . . ?
C10 C6 C3 119.3(2) . . ?
C10 C6 C7 118.4(2) . . ?
C3 C6 C7 122.3(2) . . ?
C18 C19 C20 117.7(3) . . ?
C18 C19 C24 121.2(3) . . ?
C20 C19 C24 121.0(3) . . ?
C21 C22 C23 123.1(3) . . ?
C20 C21 C22 117.5(3) . . ?
C20 C21 C26 121.3(3) . . ?
C22 C21 C26 121.3(3) . . ?
O3 C14 N2 122.0(2) . . ?
O3 C14 N3 121.1(2) . . ?
N2 C14 N3 116.9(2) . . ?
O7 C17 N4 122.6(3) . . ?
O7 C17 N5 121.4(2) . . ?
N4 C17 N5 115.9(2) . . ?
C29 C27 C33 120.6(2) . . ?
C29 C27 C28 110.8(2) . . ?
C33 C27 C28 128.6(3) . . ?
C5 C3 C6 121.3(2) . . ?
C21 C20 C19 122.8(3) . . ?
C27 C29 C30 121.9(3) . . ?
C27 C29 S1 106.58(19) . . ?
C30 C29 S1 131.5(2) . . ?
N5 C16 C15 112.2(2) . . ?
C8 C7 C6 110.8(2) . . ?
N2 C8 C7 110.7(2) . . ?
O6 C28 N1 124.2(3) . . ?
O6 C28 C27 121.4(3) . . ?
N1 C28 C27 114.4(2) . . ?
C29 C30 C31 117.0(3) . . ?
C32 C33 C27 118.1(3) . . ?
C32 C31 C30 121.5(3) . . ?
C33 C32 C31 120.8(3) . . ?

_refine_diff_density_max         0.259
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.040

_shelx_res_file                  
;
TITL DDD_a.res in P2(1)/n
    DDD_a.res
    created by SHELXL-2018/3 at 19:32:16 on 18-May-2024
CELL  0.71073   8.8693  19.0166  19.9781   90.000  101.451   90.000
ZERR   43.000   0.0003   0.0007   0.0008    0.000    0.001    0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C  H  N  O  S
UNIT 43  43  43  43  43
L.S. 40
ACTA
BOND
FMAP 2
PLAN 20
TEMP 28.850
WGHT    0.050700    2.445500
EXTI    0.018728
FVAR       0.72054
S1    5    0.350380    0.771107    0.387701    11.00000    0.05819    0.06405 =
         0.07091   -0.00865    0.01030    0.01109
O2    4    0.164781    0.747614    1.097917    11.00000    0.09750    0.06154 =
         0.05746   -0.00688    0.04389   -0.00979
N3    3    0.401513    0.714298    0.759359    11.00000    0.06779    0.04407 =
         0.03858    0.00084    0.02229   -0.00404
O7    4    0.296970    0.545938    0.652649    11.00000    0.13344    0.05824 =
         0.04619    0.00096    0.03227   -0.00437
N6    3    0.349942    0.599327    0.786114    11.00000    0.08173    0.04278 =
         0.03957   -0.00202    0.02280   -0.00208
O4    4    0.443704    0.830365    0.414504    11.00000    0.08420    0.06357 =
         0.08836   -0.02143    0.00517    0.00234
O1    4    0.262608    0.872433    1.132242    11.00000    0.13629    0.05914 =
         0.04966   -0.01150    0.03792   -0.00168
N2    3    0.407308    0.806164    0.839212    11.00000    0.07166    0.04125 =
         0.04312   -0.00090    0.02265   -0.00631
O3    4    0.450224    0.826913    0.732697    11.00000    0.13339    0.05407 =
         0.05979    0.00566    0.04651   -0.01089
N5    3    0.315845    0.639137    0.584475    11.00000    0.10764    0.05722 =
         0.03790    0.00086    0.02358    0.00646
C13   1    0.365109    0.666548    0.804565    11.00000    0.05391    0.04419 =
         0.03917    0.00087    0.01633   -0.00215
O5    4    0.190815    0.786301    0.364751    11.00000    0.05501    0.10026 =
         0.12914   -0.01286    0.00510    0.02387
C18   1    0.347654    0.543263    0.834402    11.00000    0.06484    0.04118 =
         0.04057   -0.00389    0.01870   -0.00371
O6    4    0.467157    0.594231    0.442353    11.00000    0.14096    0.07463 =
         0.08776    0.02668    0.04694    0.01846
N4    3    0.338226    0.527979    0.545293    11.00000    0.14268    0.05809 =
         0.04752   -0.00406    0.02751    0.01197
AFIX  93
H4A   2    0.337608    0.483022    0.549899    11.00000   -1.20000
H4B   2    0.352095    0.546232    0.507595    11.00000   -1.20000
AFIX   0
C9    1    0.366166    0.760241    0.885600    11.00000    0.04765    0.04416 =
         0.04166   -0.00008    0.01543   -0.00426
C11   1    0.265437    0.751505    0.993472    11.00000    0.05535    0.04681 =
         0.04653   -0.00586    0.01961   -0.00488
AFIX  43
H11   2    0.226697    0.707140    0.980081    11.00000   -1.20000
AFIX   0
C12   1    0.345449    0.691072    0.868549    11.00000    0.05513    0.04471 =
         0.04005    0.00009    0.01913   -0.00484
AFIX  43
H12   2    0.317900    0.659659    0.899726    11.00000   -1.20000
AFIX   0
C4    1    0.242595    0.779427    1.054162    11.00000    0.06122    0.04943 =
         0.04555   -0.00175    0.02047   -0.00143
C23   1    0.486763    0.515127    0.868141    11.00000    0.06058    0.04848 =
         0.05409   -0.00498    0.01747   -0.00707
C10   1    0.346385    0.789035    0.951488    11.00000    0.05285    0.04423 =
         0.04107   -0.00435    0.01580   -0.00392
C5    1    0.298348    0.846982    1.073351    11.00000    0.08123    0.05253 =
         0.04007   -0.00532    0.01602   -0.00037
N1    3    0.374858    0.705919    0.439724    11.00000    0.07707    0.07465 =
         0.06265   -0.00090    0.02733    0.00849
C15   1    0.438720    0.691364    0.694159    11.00000    0.08008    0.05349 =
         0.04262   -0.00126    0.03034   -0.00148
AFIX  23
H15A  2    0.486776    0.645364    0.700099    11.00000   -1.20000
H15B  2    0.511904    0.723934    0.681058    11.00000   -1.20000
AFIX   0
C6    1    0.407906    0.854311    0.972515    11.00000    0.06873    0.04643 =
         0.05057   -0.00471    0.01799   -0.00963
C19   1    0.208484    0.516471    0.844399    11.00000    0.05940    0.05954 =
         0.06051    0.00264    0.01718   -0.00473
C22   1    0.481660    0.461351    0.914549    11.00000    0.07381    0.05150 =
         0.05532   -0.00039    0.00611    0.00100
AFIX  43
H22   2    0.574036    0.443269    0.938664    11.00000   -1.20000
AFIX   0
C21   1    0.347101    0.433665    0.926507    11.00000    0.08725    0.05472 =
         0.04639   -0.00032    0.01515   -0.01127
C14   1    0.421650    0.785396    0.774629    11.00000    0.07639    0.04922 =
         0.04613    0.00341    0.02439   -0.00442
C17   1    0.317557    0.569635    0.596913    11.00000    0.08808    0.05745 =
         0.04302   -0.00212    0.01762    0.00634
C27   1    0.466428    0.664097    0.343057    11.00000    0.06138    0.05522 =
         0.05071   -0.00108    0.01559   -0.00075
C3    1    0.382776    0.882499    1.033459    11.00000    0.09049    0.04819 =
         0.05057   -0.01017    0.01753   -0.01303
AFIX  43
H3    2    0.423885    0.926284    1.047574    11.00000   -1.20000
AFIX   0
C20   1    0.212577    0.461700    0.891107    11.00000    0.07255    0.06937 =
         0.07370    0.00694    0.02747   -0.02095
AFIX  43
H20   2    0.120002    0.443447    0.898522    11.00000   -1.20000
AFIX   0
C29   1    0.423032    0.730794    0.321285    11.00000    0.05605    0.05444 =
         0.05203    0.00012    0.00541   -0.00313
C16   1    0.296895    0.687702    0.637652    11.00000    0.10189    0.05472 =
         0.04345    0.00243    0.01886    0.01541
AFIX  23
H16A  2    0.209545    0.673231    0.656844    11.00000   -1.20000
H16B  2    0.275084    0.734145    0.618038    11.00000   -1.20000
AFIX   0
C7    1    0.502338    0.891449    0.928806    11.00000    0.09643    0.05945 =
         0.06449   -0.01262    0.03109   -0.03192
AFIX  23
H7A   2    0.506698    0.941251    0.939514    11.00000   -1.20000
H7B   2    0.606534    0.873205    0.938612    11.00000   -1.20000
AFIX   0
C8    1    0.435021    0.881476    0.855096    11.00000    0.10480    0.04360 =
         0.06422   -0.00436    0.03616   -0.01893
AFIX  23
H8A   2    0.338747    0.907056    0.843496    11.00000   -1.20000
H8B   2    0.504749    0.900262    0.827818    11.00000   -1.20000
AFIX   0
C28   1    0.436834    0.651466    0.413062    11.00000    0.07546    0.06196 =
         0.05902    0.00626    0.02203    0.00581
C30   1    0.435642    0.754656    0.257576    11.00000    0.08646    0.06853 =
         0.05914    0.00897    0.00357   -0.00735
AFIX  43
H30   2    0.403765    0.799588    0.242708    11.00000   -1.20000
AFIX   0
C33   1    0.526855    0.618386    0.301470    11.00000    0.09271    0.06213 =
         0.06759   -0.00825    0.02647    0.00097
AFIX  43
H33   2    0.555218    0.572891    0.315774    11.00000   -1.20000
AFIX   0
C2    1    0.124328    0.676196    1.086044    11.00000    0.11438    0.06772 =
         0.07427   -0.00808    0.05350   -0.02187
AFIX 137
H2A   2    0.051775    0.671901    1.043653    11.00000   -1.50000
H2B   2    0.078938    0.658855    1.122621    11.00000   -1.50000
H2C   2    0.214781    0.649300    1.083790    11.00000   -1.50000
AFIX   0
C31   1    0.498002    0.708673    0.216609    11.00000    0.10358    0.10507 =
         0.04784   -0.00136    0.01901   -0.02790
AFIX  43
H31   2    0.509074    0.723227    0.173405    11.00000   -1.20000
AFIX   0
C32   1    0.543873    0.642048    0.238349    11.00000    0.10575    0.08485 =
         0.06395   -0.02006    0.03416   -0.00978
AFIX  43
H32   2    0.586935    0.612619    0.210032    11.00000   -1.20000
AFIX   0
C25   1    0.637732    0.538553    0.852155    11.00000    0.06699    0.08758 =
         0.11017    0.00486    0.02772   -0.00763
AFIX 137
H25A  2    0.642956    0.524665    0.806473    11.00000   -1.50000
H25B  2    0.720721    0.517154    0.883765    11.00000   -1.50000
H25C  2    0.645859    0.588789    0.856027    11.00000   -1.50000
AFIX   0
C26   1    0.346978    0.373067    0.975638    11.00000    0.14540    0.07350 =
         0.07374    0.02258    0.02008   -0.02084
AFIX 137
H26A  2    0.245713    0.367494    0.985138    11.00000   -1.50000
H26B  2    0.418640    0.382625    1.017367    11.00000   -1.50000
H26C  2    0.376505    0.330654    0.955566    11.00000   -1.50000
AFIX   0
C1    1    0.272561    0.945466    1.142903    11.00000    0.16380    0.06280 =
         0.06769   -0.02044    0.04037    0.00042
AFIX 137
H1A   2    0.378352    0.959788    1.150142    11.00000   -1.50000
H1B   2    0.230942    0.957311    1.182293    11.00000   -1.50000
H1C   2    0.215188    0.969195    1.103558    11.00000   -1.50000
AFIX   0
C24   1    0.057527    0.544933    0.805498    11.00000    0.06465    0.12206 =
         0.12117    0.02883    0.01265   -0.00026
AFIX 137
H24A  2    0.034468    0.588400    0.825747    11.00000   -1.50000
H24B  2   -0.022789    0.511529    0.807182    11.00000   -1.50000
H24C  2    0.064851    0.552980    0.758812    11.00000   -1.50000
AFIX   0
H71   2    0.343620    0.654335    0.548378    11.00000    0.07552
H80   2    0.344043    0.586958    0.741805    11.00000    0.07685
HKLF 4




REM  DDD_a.res in P2(1)/n
REM wR2 = 0.156919, GooF = S = 0.97135, Restrained GooF = 0.97135 for all data
REM R1 = 0.051983 for 4510 Fo > 4sig(Fo) and 0.105445 for all 7577 data
REM 438 parameters refined using 0 restraints

END

WGHT      0.0608      1.4021

REM Highest difference peak  0.259,  deepest hole -0.296,  1-sigma level  0.040
Q1    1   0.0381  0.5399  0.9916  11.00000  0.05    0.26
Q2    1   0.0748  0.5449  0.9969  11.00000  0.05    0.25
Q3    1   0.1106  0.5569  0.9858  11.00000  0.05    0.22
Q4    1   0.4277  0.5589  0.6877  11.00000  0.05    0.19
Q5    1   0.3586  0.5788  0.4173  11.00000  0.05    0.17
Q6    1   0.3582  0.7774  0.9224  11.00000  0.05    0.17
Q7    1   0.4424  0.5644  0.5096  11.00000  0.05    0.16
Q8    1   0.0703  0.6020  0.7816  11.00000  0.05    0.16
Q9    1   0.1565  0.7168  0.9661  11.00000  0.05    0.16
Q10   1   0.3881  0.6822  0.8391  11.00000  0.05    0.15
Q11   1   0.3808  0.8637  1.1397  11.00000  0.05    0.15
Q12   1   0.4236  0.4785  0.5617  11.00000  0.05    0.14
Q13   1   0.3973  0.6241  0.4704  11.00000  0.05    0.14
Q14   1   0.3976  0.7163  0.8820  11.00000  0.05    0.14
Q15   1   0.2876  0.7845  0.9565  11.00000  0.05    0.14
Q16   1   0.2973  0.5463  0.8454  11.00000  0.05    0.14
Q17   1   0.3534  0.6737  0.4659  11.00000  0.05    0.14
Q18   1   0.4170  0.5353  0.8615  11.00000  0.05    0.14
Q19   1  -0.1801  0.4163  0.7607  11.00000  0.05    0.13
Q20   1   0.2396  0.7573  1.0921  11.00000  0.05    0.13
;
_shelx_res_checksum              28531
####################################################################### 
# 
# 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_DATA_AA_a
_database_code_depnum_ccdc_archive 'CCDC 2358075'
loop_
_audit_author_name
_audit_author_address
'Lopamudra LOPAMUDRA GIRI'
;ICT Bhubaneswar
India
;
_audit_update_record             
;
2024-05-24 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H32 N5 O4, C3 H3 O4'
_chemical_formula_sum            'C29 H35 N5 O8'
_chemical_formula_weight         581.62

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   8.8749(3)
_cell_length_b                   15.2900(6)
_cell_length_c                   21.2670(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.0050(10)
_cell_angle_gamma                90
_cell_volume                     2857.75(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    3694
_cell_measurement_theta_min      0.975
_cell_measurement_theta_max      0.980

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_F_000             1232.0
_exptl_transmission_factor_min   0.975
_exptl_transmission_factor_max   0.980
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.100
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'Bruker D8 Venture photon 100 CMOS detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41406
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.348
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6582
_reflns_number_gt                3694
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SHELXL'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0334P)²+2.3731P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0104(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6567
_refine_ls_number_parameters     394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1477
_refine_ls_wR_factor_gt          0.1066
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
O8 O 0.5985(2) 0.45563(11) 0.32657(8) 0.0554(5) Uani 1 1 d . . . . .
O5 O 0.5068(2) 0.08209(12) 0.31799(9) 0.0586(5) Uani 1 1 d . . . . .
O7 O -0.3203(2) 0.01162(12) 0.47610(9) 0.0559(5) Uani 1 1 d . . . . .
O6 O -0.1985(2) 0.14579(12) 0.53507(9) 0.0618(5) Uani 1 1 d . . . . .
N4 N 0.2953(2) 0.09987(12) 0.36648(9) 0.0429(5) Uani 1 1 d . . . . .
N3 N 0.4600(2) 0.21798(13) 0.35443(9) 0.0443(5) Uani 1 1 d . . . . .
N5 N 0.4078(2) 0.35723(13) 0.38967(10) 0.0479(5) Uani 1 1 d . . . . .
N1 N 0.6720(3) 0.36080(15) 0.25562(12) 0.0593(6) Uani 1 1 d . . . . .
C24 C 0.0060(3) 0.03941(15) 0.38824(11) 0.0409(5) Uani 1 1 d . . . . .
C10 C 0.2053(3) 0.15271(15) 0.39770(11) 0.0410(5) Uani 1 1 d . . . . .
C25 C 0.0693(3) 0.11380(15) 0.41844(11) 0.0409(5) Uani 1 1 d . . . . .
C12 C 0.3704(3) 0.27325(15) 0.38378(11) 0.0433(6) Uani 1 1 d . . . . .
C26 C -0.1265(3) 0.00464(16) 0.40615(11) 0.0450(6) Uani 1 1 d . . . . .
H26 H -0.170302 -0.044639 0.385464 0.054 Uiso 1 1 calc R U . . .
C13 C 0.3303(3) 0.41720(16) 0.42636(11) 0.0450(6) Uani 1 1 d . . . . .
C28 C -0.1272(3) 0.11680(15) 0.48607(12) 0.0458(6) Uani 1 1 d . . . . .
C29 C 0.0015(3) 0.15218(15) 0.46784(11) 0.0450(6) Uani 1 1 d . . . . .
H29 H 0.044570 0.201887 0.488180 0.054 Uiso 1 1 calc R U . . .
O2 O 0.8115(3) 0.29112(15) 0.15056(12) 0.1012(9) Uani 1 1 d . . . . .
N2 N 0.7860(3) 0.49590(16) 0.27155(12) 0.0679(7) Uani 1 1 d . . . . .
H2A H 0.794906 0.546074 0.289972 0.081 Uiso 1 1 calc R U . . .
H2B H 0.843354 0.482624 0.243554 0.081 Uiso 1 1 calc R U . . .
O4 O 0.6971(3) 0.16421(18) 0.16371(14) 0.1001(8) Uani 1 1 d . . . . .
C27 C -0.1936(3) 0.04233(16) 0.45420(12) 0.0448(6) Uani 1 1 d . . . . .
C9 C 0.4250(3) 0.12961(15) 0.34406(12) 0.0446(6) Uani 1 1 d . . . . .
C23 C 0.0856(3) -0.00129(16) 0.33761(12) 0.0466(6) Uani 1 1 d . . . . .
H23A H 0.057974 -0.062549 0.332865 0.056 Uiso 1 1 calc R U . . .
H23B H 0.054225 0.027708 0.297355 0.056 Uiso 1 1 calc R U . . .
C14 C 0.3593(3) 0.41219(16) 0.49258(12) 0.0485(6) Uani 1 1 d . . . . .
C11 C 0.2428(3) 0.23876(15) 0.40672(11) 0.0450(6) Uani 1 1 d . . . . .
H11 H 0.182968 0.274787 0.428331 0.054 Uiso 1 1 calc R U . . .
C22 C 0.2548(3) 0.00693(15) 0.35525(12) 0.0462(6) Uani 1 1 d . . . . .
H22A H 0.287662 -0.026804 0.393312 0.055 Uiso 1 1 calc R U . . .
H22B H 0.305815 -0.015910 0.321259 0.055 Uiso 1 1 calc R U . . .
C6 C 0.6825(3) 0.43831(17) 0.28651(12) 0.0509(6) Uani 1 1 d . . . . .
C20 C 0.2347(3) 0.47980(16) 0.39503(12) 0.0493(6) Uani 1 1 d . . . . .
C8 C 0.5952(3) 0.25171(17) 0.32959(12) 0.0509(6) Uani 1 1 d . . . . .
H8A H 0.663120 0.203474 0.324014 0.061 Uiso 1 1 calc R U . . .
H8B H 0.648889 0.291805 0.360235 0.061 Uiso 1 1 calc R U . . .
C16 C 0.2868(3) 0.47272(18) 0.52692(13) 0.0553(7) Uani 1 1 d . . . . .
H16 H 0.303074 0.470134 0.571034 0.066 Uiso 1 1 calc R U . . .
C7 C 0.5539(3) 0.29867(18) 0.26660(13) 0.0547(7) Uani 1 1 d . . . . .
H7A H 0.540599 0.256129 0.232446 0.066 Uiso 1 1 calc R U . . .
H7B H 0.458311 0.329409 0.266605 0.066 Uiso 1 1 calc R U . . .
C18 C 0.1656(3) 0.53881(17) 0.43177(13) 0.0568(7) Uani 1 1 d . . . . .
H18 H 0.100328 0.580974 0.411679 0.068 Uiso 1 1 calc R U . . .
C30 C -0.3853(3) -0.06757(18) 0.44876(14) 0.0583(7) Uani 1 1 d . . . . .
H30A H -0.417118 -0.059040 0.404157 0.087 Uiso 1 1 calc R U . . .
H30B H -0.471680 -0.083369 0.468953 0.087 Uiso 1 1 calc R U . . .
H30C H -0.310920 -0.113460 0.454792 0.087 Uiso 1 1 calc R U . . .
C17 C 0.1916(3) 0.53642(18) 0.49778(14) 0.0571(7) Uani 1 1 d . . . . .
C15 C 0.4637(3) 0.3453(2) 0.52678(14) 0.0657(8) Uani 1 1 d . . . . .
H15A H 0.512582 0.369503 0.566055 0.099 Uiso 1 1 calc R U . . .
H15B H 0.539361 0.328953 0.500818 0.099 Uiso 1 1 calc R U . . .
H15C H 0.406061 0.294639 0.535389 0.099 Uiso 1 1 calc R U . . .
O1 O 1.0845(4) 0.30986(18) 0.18623(18) 0.1263(11) Uani 1 1 d . . . . .
H6 H 1.001659 0.330815 0.190800 0.189 Uiso 1 1 calc R U . . .
C21 C 0.2053(4) 0.4834(2) 0.32388(13) 0.0680(8) Uani 1 1 d . . . . .
H21A H 0.136734 0.530666 0.310845 0.102 Uiso 1 1 calc R U . . .
H21B H 0.160853 0.429271 0.307754 0.102 Uiso 1 1 calc R U . . .
H21C H 0.299526 0.492719 0.307508 0.102 Uiso 1 1 calc R U . . .
C31 C -0.1239(4) 0.21073(19) 0.57637(14) 0.0700(9) Uani 1 1 d . . . . .
H31A H -0.021184 0.192728 0.590572 0.105 Uiso 1 1 calc R U . . .
H31B H -0.177135 0.217949 0.612359 0.105 Uiso 1 1 calc R U . . .
H31C H -0.123223 0.265218 0.553990 0.105 Uiso 1 1 calc R U . . .
C4 C 0.8086(5) 0.2126(2) 0.17067(16) 0.0761(10) Uani 1 1 d . . . . .
C19 C 0.1181(4) 0.6024(2) 0.53728(15) 0.0747(9) Uani 1 1 d . . . . .
H19A H 0.179910 0.654088 0.542818 0.112 Uiso 1 1 calc R U . . .
H19B H 0.109055 0.577538 0.578037 0.112 Uiso 1 1 calc R U . . .
H19C H 0.018880 0.617289 0.515978 0.112 Uiso 1 1 calc R U . . .
O3 O 1.2174(4) 0.2061(3) 0.23829(18) 0.1496(15) Uani 1 1 d . . . . .
C3 C 0.9560(4) 0.1788(2) 0.20772(16) 0.0788(10) Uani 1 1 d . . . . .
H3A H 0.936497 0.166763 0.250633 0.095 Uiso 1 1 calc R U . . .
H3B H 0.978474 0.123144 0.189147 0.095 Uiso 1 1 calc R U . . .
C2 C 1.0983(6) 0.2335(3) 0.21262(19) 0.0944(12) Uani 1 1 d . . . . .
H5 H 0.477(3) 0.380(2) 0.3668(14) 0.077(10) Uiso 1 1 d . . . . .
H2 H 0.730(4) 0.345(2) 0.2239(16) 0.092(11) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O8 0.0635(11) 0.0526(11) 0.0555(11) -0.0043(9) 0.0270(9) -0.0104(9)
O5 0.0589(11) 0.0492(11) 0.0747(13) -0.0057(9) 0.0337(10) 0.0030(9)
O7 0.0501(10) 0.0540(11) 0.0688(12) -0.0149(9) 0.0266(9) -0.0141(8)
O6 0.0697(12) 0.0556(11) 0.0683(12) -0.0199(10) 0.0383(10) -0.0132(9)
N4 0.0470(11) 0.0361(10) 0.0498(12) -0.0022(9) 0.0210(9) -0.0016(9)
N3 0.0457(11) 0.0404(11) 0.0507(12) 0.0010(9) 0.0198(9) -0.0038(9)
N5 0.0555(13) 0.0404(11) 0.0524(13) -0.0035(10) 0.0240(11) -0.0101(10)
N1 0.0686(16) 0.0524(14) 0.0645(15) -0.0016(12) 0.0363(13) -0.0074(11)
C24 0.0442(13) 0.0383(13) 0.0413(13) -0.0003(10) 0.0106(10) 0.0000(10)
C10 0.0468(13) 0.0380(12) 0.0411(13) 0.0003(10) 0.0162(11) -0.0004(10)
C25 0.0445(13) 0.0349(12) 0.0461(13) -0.0014(10) 0.0158(11) -0.0022(10)
C12 0.0490(14) 0.0409(13) 0.0423(13) -0.0005(10) 0.0149(11) -0.0057(11)
C26 0.0464(13) 0.0422(13) 0.0475(14) -0.0063(11) 0.0104(11) -0.0049(11)
C13 0.0525(14) 0.0395(13) 0.0465(14) -0.0054(11) 0.0193(12) -0.0121(11)
C28 0.0518(14) 0.0397(13) 0.0503(14) -0.0057(11) 0.0220(12) -0.0003(11)
C29 0.0520(14) 0.0354(12) 0.0514(14) -0.0062(11) 0.0202(12) -0.0050(11)
O2 0.140(2) 0.0691(15) 0.1099(19) 0.0363(14) 0.0709(17) 0.0434(15)
N2 0.0667(16) 0.0636(15) 0.0805(17) 0.0009(13) 0.0359(14) -0.0181(12)
O4 0.0922(19) 0.0827(18) 0.129(2) 0.0153(16) 0.0302(17) 0.0219(15)
C27 0.0416(13) 0.0438(14) 0.0514(14) -0.0020(11) 0.0150(11) -0.0040(11)
C9 0.0475(14) 0.0403(13) 0.0491(14) 0.0006(11) 0.0173(12) -0.0009(11)
C23 0.0551(15) 0.0421(13) 0.0455(14) -0.0059(11) 0.0169(12) -0.0040(11)
C14 0.0531(15) 0.0444(14) 0.0503(15) -0.0026(12) 0.0153(12) -0.0117(12)
C11 0.0506(14) 0.0364(13) 0.0527(14) -0.0037(11) 0.0231(12) -0.0043(11)
C22 0.0561(15) 0.0338(12) 0.0527(15) -0.0037(11) 0.0216(12) -0.0008(11)
C6 0.0511(15) 0.0518(16) 0.0514(15) 0.0056(12) 0.0131(13) -0.0053(12)
C20 0.0573(16) 0.0441(14) 0.0487(14) -0.0024(12) 0.0155(12) -0.0088(12)
C8 0.0478(14) 0.0491(15) 0.0605(16) 0.0016(12) 0.0240(12) -0.0050(12)
C16 0.0662(17) 0.0543(16) 0.0487(15) -0.0086(13) 0.0197(13) -0.0149(14)
C7 0.0618(17) 0.0527(16) 0.0544(16) -0.0032(13) 0.0245(13) -0.0099(13)
C18 0.0660(18) 0.0422(14) 0.0642(18) -0.0027(13) 0.0158(14) -0.0036(13)
C30 0.0475(15) 0.0567(17) 0.0730(19) -0.0126(14) 0.0168(14) -0.0124(13)
C17 0.0669(18) 0.0477(15) 0.0609(17) -0.0125(13) 0.0234(14) -0.0120(14)
C15 0.0702(19) 0.0688(19) 0.0585(17) 0.0040(15) 0.0103(15) -0.0017(16)
O1 0.176(3) 0.0679(17) 0.144(3) 0.0160(18) 0.054(3) -0.0225(18)
C21 0.078(2) 0.073(2) 0.0527(17) -0.0002(15) 0.0106(15) 0.0034(16)
C31 0.100(2) 0.0549(17) 0.0627(18) -0.0185(15) 0.0376(17) -0.0144(16)
C4 0.103(3) 0.058(2) 0.075(2) 0.0117(17) 0.042(2) 0.028(2)
C19 0.091(2) 0.0607(19) 0.078(2) -0.0205(16) 0.0328(19) -0.0028(17)
O3 0.123(3) 0.164(3) 0.146(3) 0.045(3) -0.036(2) -0.050(2)
C3 0.103(3) 0.063(2) 0.071(2) 0.0101(16) 0.0154(19) 0.0047(19)
C2 0.115(3) 0.092(3) 0.075(2) 0.013(2) 0.006(2) -0.021(3)

_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
O8 C6 1.236(3) . ?
O5 C9 1.214(3) . ?
O7 C27 1.359(3) . ?
O7 C30 1.430(3) . ?
O6 C28 1.366(3) . ?
O6 C31 1.426(3) . ?
N4 C10 1.371(3) . ?
N4 C9 1.382(3) . ?
N4 C22 1.477(3) . ?
N3 C12 1.369(3) . ?
N3 C9 1.397(3) . ?
N3 C8 1.470(3) . ?
N5 C12 1.328(3) . ?
N5 C13 1.440(3) . ?
N1 C6 1.352(3) . ?
N1 C7 1.457(3) . ?
C24 C25 1.386(3) . ?
C24 C26 1.391(3) . ?
C24 C23 1.503(3) . ?
C10 C11 1.364(3) . ?
C10 C25 1.467(3) . ?
C25 C29 1.409(3) . ?
C12 C11 1.397(3) . ?
C26 C27 1.379(3) . ?
C13 C20 1.387(4) . ?
C13 C14 1.398(3) . ?
C28 C29 1.368(3) . ?
C28 C27 1.411(3) . ?
O2 C4 1.276(4) . ?
N2 C6 1.342(3) . ?
O4 C4 1.228(4) . ?
C23 C22 1.501(3) . ?
C14 C16 1.391(3) . ?
C14 C15 1.499(4) . ?
C20 C18 1.391(4) . ?
C20 C21 1.500(4) . ?
C8 C7 1.519(4) . ?
C16 C17 1.379(4) . ?
C18 C17 1.391(4) . ?
C17 C19 1.517(4) . ?
O1 C2 1.293(5) . ?
C4 C3 1.521(5) . ?
O3 C2 1.196(5) . ?
C3 C2 1.506(5) . ?

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
C27 O7 C30 117.36(19) . . ?
C28 O6 C31 118.1(2) . . ?
C10 N4 C9 122.86(19) . . ?
C10 N4 C22 119.98(18) . . ?
C9 N4 C22 117.16(18) . . ?
C12 N3 C9 122.56(19) . . ?
C12 N3 C8 120.15(19) . . ?
C9 N3 C8 117.22(19) . . ?
C12 N5 C13 122.3(2) . . ?
C6 N1 C7 119.7(2) . . ?
C25 C24 C26 119.4(2) . . ?
C25 C24 C23 118.1(2) . . ?
C26 C24 C23 122.5(2) . . ?
C11 C10 N4 119.3(2) . . ?
C11 C10 C25 123.0(2) . . ?
N4 C10 C25 117.8(2) . . ?
C24 C25 C29 120.0(2) . . ?
C24 C25 C10 119.4(2) . . ?
C29 C25 C10 120.6(2) . . ?
N5 C12 N3 119.1(2) . . ?
N5 C12 C11 122.4(2) . . ?
N3 C12 C11 118.5(2) . . ?
C27 C26 C24 120.8(2) . . ?
C20 C13 C14 122.4(2) . . ?
C20 C13 N5 119.1(2) . . ?
C14 C13 N5 118.5(2) . . ?
C29 C28 O6 125.6(2) . . ?
C29 C28 C27 119.5(2) . . ?
O6 C28 C27 114.9(2) . . ?
C28 C29 C25 120.4(2) . . ?
O7 C27 C26 125.0(2) . . ?
O7 C27 C28 115.1(2) . . ?
C26 C27 C28 119.9(2) . . ?
O5 C9 N4 122.7(2) . . ?
O5 C9 N3 121.1(2) . . ?
N4 C9 N3 116.19(19) . . ?
C22 C23 C24 109.9(2) . . ?
C16 C14 C13 117.3(3) . . ?
C16 C14 C15 119.9(2) . . ?
C13 C14 C15 122.7(2) . . ?
C10 C11 C12 120.6(2) . . ?
N4 C22 C23 109.5(2) . . ?
O8 C6 N2 121.4(3) . . ?
O8 C6 N1 121.0(2) . . ?
N2 C6 N1 117.6(2) . . ?
C13 C20 C18 117.8(2) . . ?
C13 C20 C21 121.3(2) . . ?
C18 C20 C21 120.9(3) . . ?
N3 C8 C7 112.0(2) . . ?
C17 C16 C14 122.2(3) . . ?
N1 C7 C8 111.0(2) . . ?
C20 C18 C17 121.7(3) . . ?
C16 C17 C18 118.5(2) . . ?
C16 C17 C19 120.3(3) . . ?
C18 C17 C19 121.2(3) . . ?
O4 C4 O2 125.5(4) . . ?
O4 C4 C3 118.6(3) . . ?
O2 C4 C3 115.9(4) . . ?
C2 C3 C4 119.9(3) . . ?
O3 C2 O1 122.6(4) . . ?
O3 C2 C3 121.0(4) . . ?
O1 C2 C3 116.4(4) . . ?

_refine_diff_density_max         0.273
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.045

_shelx_res_file                  
;
TITL DATA_AA_a.res in P2(1)/n
    DATA_AA_a.res
    created by SHELXL-2018/3 at 10:52:47 on 30-Dec-2023
CELL  0.71073   8.8749  15.2900  21.2670   90.000   98.005   90.000
ZERR   57.000   0.0003   0.0006   0.0008    0.000    0.001    0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C  H  N  O
UNIT 57  57  57  57
L.S. 10
ACTA
BOND
FMAP 2
PLAN 20
TEMP 28.850
WGHT    0.033400    2.373100
EXTI    0.010420
FVAR       0.62658
O8    4    0.598463    0.455634    0.326573    11.00000    0.06345    0.05256 =
         0.05548   -0.00429    0.02704   -0.01038
O5    4    0.506759    0.082088    0.317994    11.00000    0.05892    0.04916 =
         0.07465   -0.00574    0.03374    0.00301
O7    4   -0.320309    0.011618    0.476101    11.00000    0.05013    0.05403 =
         0.06881   -0.01492    0.02657   -0.01408
O6    4   -0.198533    0.145789    0.535069    11.00000    0.06971    0.05560 =
         0.06827   -0.01991    0.03831   -0.01319
N4    3    0.295336    0.099871    0.366482    11.00000    0.04696    0.03611 =
         0.04976   -0.00218    0.02104   -0.00161
N3    3    0.460030    0.217979    0.354434    11.00000    0.04570    0.04037 =
         0.05065    0.00095    0.01979   -0.00379
N5    3    0.407821    0.357234    0.389666    11.00000    0.05547    0.04043 =
         0.05244   -0.00353    0.02397   -0.01007
N1    3    0.671963    0.360804    0.255623    11.00000    0.06855    0.05241 =
         0.06449   -0.00162    0.03631   -0.00744
C24   1    0.005953    0.039413    0.388236    11.00000    0.04424    0.03833 =
         0.04131   -0.00030    0.01057    0.00005
C10   1    0.205253    0.152709    0.397704    11.00000    0.04677    0.03805 =
         0.04113    0.00027    0.01621   -0.00044
C25   1    0.069262    0.113798    0.418437    11.00000    0.04452    0.03490 =
         0.04611   -0.00143    0.01577   -0.00224
C12   1    0.370405    0.273251    0.383779    11.00000    0.04904    0.04092 =
         0.04230   -0.00053    0.01489   -0.00572
C26   1   -0.126485    0.004643    0.406150    11.00000    0.04637    0.04215 =
         0.04752   -0.00635    0.01040   -0.00487
AFIX  43
H26   2   -0.170302   -0.044639    0.385464    11.00000   -1.20000
AFIX   0
C13   1    0.330317    0.417199    0.426360    11.00000    0.05250    0.03947 =
         0.04653   -0.00539    0.01934   -0.01214
C28   1   -0.127226    0.116799    0.486066    11.00000    0.05176    0.03969 =
         0.05029   -0.00575    0.02197   -0.00027
C29   1    0.001498    0.152179    0.467837    11.00000    0.05196    0.03535 =
         0.05137   -0.00622    0.02017   -0.00498
AFIX  43
H29   2    0.044570    0.201887    0.488180    11.00000   -1.20000
AFIX   0
O2    4    0.811489    0.291121    0.150559    11.00000    0.13989    0.06911 =
         0.10993    0.03631    0.07095    0.04337
N2    3    0.785971    0.495901    0.271553    11.00000    0.06673    0.06364 =
         0.08053    0.00091    0.03589   -0.01810
AFIX  93
H2A   2    0.794906    0.546074    0.289972    11.00000   -1.20000
H2B   2    0.843354    0.482624    0.243554    11.00000   -1.20000
AFIX   0
O4    4    0.697089    0.164209    0.163711    11.00000    0.09222    0.08266 =
         0.12948    0.01525    0.03023    0.02187
C27   1   -0.193627    0.042328    0.454199    11.00000    0.04156    0.04376 =
         0.05139   -0.00202    0.01502   -0.00399
C9    1    0.424963    0.129610    0.344056    11.00000    0.04748    0.04027 =
         0.04909    0.00060    0.01731   -0.00086
C23   1    0.085649   -0.001291    0.337613    11.00000    0.05508    0.04209 =
         0.04547   -0.00586    0.01687   -0.00400
AFIX  23
H23A  2    0.057974   -0.062549    0.332865    11.00000   -1.20000
H23B  2    0.054225    0.027708    0.297355    11.00000   -1.20000
AFIX   0
C14   1    0.359288    0.412194    0.492579    11.00000    0.05305    0.04441 =
         0.05028   -0.00262    0.01528   -0.01173
C11   1    0.242824    0.238759    0.406719    11.00000    0.05059    0.03639 =
         0.05266   -0.00369    0.02313   -0.00430
AFIX  43
H11   2    0.182968    0.274787    0.428331    11.00000   -1.20000
AFIX   0
C22   1    0.254763    0.006933    0.355245    11.00000    0.05610    0.03380 =
         0.05269   -0.00367    0.02156   -0.00084
AFIX  23
H22A  2    0.287662   -0.026804    0.393312    11.00000   -1.20000
H22B  2    0.305815   -0.015910    0.321259    11.00000   -1.20000
AFIX   0
C6    1    0.682454    0.438306    0.286508    11.00000    0.05106    0.05184 =
         0.05142    0.00556    0.01310   -0.00528
C20   1    0.234705    0.479800    0.395030    11.00000    0.05734    0.04407 =
         0.04871   -0.00243    0.01549   -0.00881
C8    1    0.595230    0.251706    0.329594    11.00000    0.04784    0.04912 =
         0.06053    0.00163    0.02397   -0.00500
AFIX  23
H8A   2    0.663120    0.203474    0.324014    11.00000   -1.20000
H8B   2    0.648889    0.291805    0.360235    11.00000   -1.20000
AFIX   0
C16   1    0.286774    0.472723    0.526919    11.00000    0.06620    0.05427 =
         0.04866   -0.00863    0.01971   -0.01489
AFIX  43
H16   2    0.303074    0.470134    0.571034    11.00000   -1.20000
AFIX   0
C7    1    0.553923    0.298673    0.266603    11.00000    0.06176    0.05272 =
         0.05437   -0.00323    0.02447   -0.00991
AFIX  23
H7A   2    0.540599    0.256129    0.232446    11.00000   -1.20000
H7B   2    0.458311    0.329409    0.266605    11.00000   -1.20000
AFIX   0
C18   1    0.165606    0.538808    0.431769    11.00000    0.06604    0.04219 =
         0.06421   -0.00272    0.01577   -0.00359
AFIX  43
H18   2    0.100328    0.580974    0.411679    11.00000   -1.20000
AFIX   0
C30   1   -0.385348   -0.067565    0.448755    11.00000    0.04754    0.05673 =
         0.07305   -0.01262    0.01675   -0.01239
AFIX 137
H30A  2   -0.417118   -0.059040    0.404157    11.00000   -1.50000
H30B  2   -0.471680   -0.083369    0.468953    11.00000   -1.50000
H30C  2   -0.310920   -0.113460    0.454792    11.00000   -1.50000
AFIX   0
C17   1    0.191566    0.536417    0.497783    11.00000    0.06687    0.04765 =
         0.06095   -0.01245    0.02337   -0.01197
C15   1    0.463705    0.345313    0.526784    11.00000    0.07023    0.06879 =
         0.05846    0.00405    0.01030   -0.00174
AFIX 137
H15A  2    0.512582    0.369503    0.566055    11.00000   -1.50000
H15B  2    0.539361    0.328953    0.500818    11.00000   -1.50000
H15C  2    0.406061    0.294639    0.535389    11.00000   -1.50000
AFIX   0
O1    4    1.084492    0.309861    0.186232    11.00000    0.17617    0.06786 =
         0.14387    0.01596    0.05405   -0.02246
AFIX 147
H6    2    1.001659    0.330815    0.190800    11.00000   -1.50000
AFIX   0
C21   1    0.205308    0.483442    0.323878    11.00000    0.07848    0.07312 =
         0.05274   -0.00023    0.01063    0.00345
AFIX 137
H21A  2    0.136734    0.530666    0.310845    11.00000   -1.50000
H21B  2    0.160853    0.429271    0.307754    11.00000   -1.50000
H21C  2    0.299526    0.492719    0.307508    11.00000   -1.50000
AFIX   0
C31   1   -0.123922    0.210728    0.576373    11.00000    0.09974    0.05491 =
         0.06273   -0.01849    0.03761   -0.01440
AFIX 137
H31A  2   -0.021184    0.192728    0.590572    11.00000   -1.50000
H31B  2   -0.177135    0.217949    0.612359    11.00000   -1.50000
H31C  2   -0.123223    0.265218    0.553990    11.00000   -1.50000
AFIX   0
C4    1    0.808562    0.212605    0.170675    11.00000    0.10337    0.05799 =
         0.07548    0.01167    0.04216    0.02804
C19   1    0.118112    0.602387    0.537278    11.00000    0.09113    0.06074 =
         0.07817   -0.02047    0.03281   -0.00281
AFIX 137
H19A  2    0.179910    0.654088    0.542818    11.00000   -1.50000
H19B  2    0.109055    0.577538    0.578037    11.00000   -1.50000
H19C  2    0.018880    0.617289    0.515978    11.00000   -1.50000
AFIX   0
O3    4    1.217401    0.206079    0.238291    11.00000    0.12261    0.16444 =
         0.14609    0.04533   -0.03598   -0.04959
C3    1    0.956033    0.178769    0.207716    11.00000    0.10330    0.06327 =
         0.07090    0.01011    0.01537    0.00472
AFIX  23
H3A   2    0.936497    0.166763    0.250633    11.00000   -1.20000
H3B   2    0.978474    0.123144    0.189147    11.00000   -1.20000
AFIX   0
C2    1    1.098273    0.233537    0.212616    11.00000    0.11464    0.09208 =
         0.07461    0.01344    0.00649   -0.02121
H5    2    0.476591    0.380014    0.366796    11.00000    0.07716
H2    2    0.729890    0.344658    0.223904    11.00000    0.09220
HKLF 4




REM  DATA_AA_a.res in P2(1)/n
REM wR2 = 0.147686, GooF = S = 1.02629, Restrained GooF = 1.02629 for all data
REM R1 = 0.051236 for 3694 Fo > 4sig(Fo) and 0.115001 for all 6567 data
REM 394 parameters refined using 0 restraints

END

WGHT      0.0558      1.6143

REM Highest difference peak  0.273,  deepest hole -0.247,  1-sigma level  0.045
Q1    1   0.9175  0.3164  0.1874  11.00000  0.05    0.27
Q2    1   1.1991  0.3012  0.2294  11.00000  0.05    0.26
Q3    1   1.0739  0.3019  0.2423  11.00000  0.05    0.20
Q4    1   0.0335  0.0759  0.4069  11.00000  0.05    0.18
Q5    1  -0.1995  0.2613  0.5418  11.00000  0.05    0.17
Q6    1   0.8263  0.1426  0.2146  11.00000  0.05    0.17
Q7    1  -0.1741  0.1737  0.5521  11.00000  0.05    0.17
Q8    1  -0.1571 -0.0841  0.4010  11.00000  0.05    0.17
Q9    1  -0.2553  0.1690  0.4962  11.00000  0.05    0.17
Q10   1  -0.1647  0.0760  0.4668  11.00000  0.05    0.17
Q11   1  -0.1567  0.0245  0.4331  11.00000  0.05    0.16
Q12   1  -0.0422  0.0209  0.4009  11.00000  0.05    0.16
Q13   1   0.2325  0.1922  0.4144  11.00000  0.05    0.16
Q14   1   0.1199  0.3006  0.3942  11.00000  0.05    0.16
Q15   1  -0.2285  0.1882  0.5988  11.00000  0.05    0.16
Q16   1  -0.2391  0.0270  0.4668  11.00000  0.05    0.16
Q17   1   0.6824  0.2017  0.3434  11.00000  0.05    0.16
Q18   1   0.3590  0.1146  0.3595  11.00000  0.05    0.16
Q19   1   0.1213  0.1197  0.4119  11.00000  0.05    0.16
Q20   1  -0.0999  0.1395  0.4659  11.00000  0.05    0.15
;
_shelx_res_checksum              34600
####################################################################### 
# 
# 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_DATA_M_a
_database_code_depnum_ccdc_archive 'CCDC 2358076'
loop_
_audit_author_name
_audit_author_address
'Lopamudra LOPAMUDRA GIRI'
;ICT Bhubaneswar
India
;
_audit_update_record             
;
2024-05-24 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H32 N5 O4, C3 H3 O4'
_chemical_formula_sum            'C29 H35 N5 O8'
_chemical_formula_weight         581.62

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   15.925(3)
_cell_length_b                   10.5056(19)
_cell_length_c                   17.711(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.685(6)
_cell_angle_gamma                90
_cell_volume                     2962.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2938
_cell_measurement_theta_min      0.977
_cell_measurement_theta_max      0.981

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_F_000             1232.0
_exptl_transmission_factor_min   0.977
_exptl_transmission_factor_max   0.981
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.096
_shelx_estimated_absorpt_T_min   0.977
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'Bruker D8 Venture photon 100 CMOS detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47388
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_av_R_equivalents  0.1197
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.254
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6817
_reflns_number_gt                2938
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SHELXL'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0416P)²+2.1856P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0072(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6766
_refine_ls_number_parameters     402
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1663
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1710
_refine_ls_wR_factor_gt          0.1163
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
O5 O 0.50273(14) -0.22744(19) 0.42418(12) 0.0648(6) Uani 1 1 d . . . . .
O6 O 0.48786(13) -0.02986(19) 0.33889(11) 0.0630(6) Uani 1 1 d . . . . .
O8 O 0.08323(14) 0.6439(2) 0.45195(12) 0.0686(6) Uani 1 1 d . . . . .
O7 O 0.18779(15) 0.2790(2) 0.67540(12) 0.0723(7) Uani 1 1 d . . . . .
N3 N 0.17681(15) 0.3526(2) 0.55446(13) 0.0536(6) Uani 1 1 d . . . . .
N5 N 0.17020(16) 0.4293(2) 0.43091(14) 0.0554(7) Uani 1 1 d . . . . .
N4 N 0.25954(15) 0.1715(2) 0.58467(13) 0.0541(6) Uani 1 1 d . . . . .
O1 O 0.11281(16) -0.1184(2) 0.69356(14) 0.0820(7) Uani 1 1 d . . . . .
N2 N 0.11133(18) 0.6916(3) 0.57463(18) 0.0663(8) Uani 1 1 d . . . . .
C21 C 0.20130(19) 0.4267(3) 0.35470(17) 0.0518(7) Uani 1 1 d . . . . .
C14 C 0.34183(18) 0.0597(3) 0.49058(16) 0.0488(7) Uani 1 1 d . . . . .
N1 N 0.02814(19) 0.8231(3) 0.50218(16) 0.0804(9) Uani 1 1 d . . . . .
H1A H 0.002833 0.841842 0.460487 0.096 Uiso 1 1 calc R U . . .
H1B H 0.023392 0.872130 0.540765 0.096 Uiso 1 1 calc R U . . .
C7 C 0.28354(18) 0.1610(3) 0.51068(16) 0.0491(7) Uani 1 1 d . . . . .
C5 C 0.19905(18) 0.3439(3) 0.48038(16) 0.0511(7) Uani 1 1 d . . . . .
C18 C 0.38662(18) 0.0661(3) 0.42271(16) 0.0517(7) Uani 1 1 d . . . . .
H18 H 0.380025 0.136488 0.391326 0.062 Uiso 1 1 calc R U . . .
C13 C 0.35077(18) -0.0457(3) 0.53748(16) 0.0528(8) Uani 1 1 d . . . . .
C15 C 0.40379(19) -0.1445(3) 0.51541(17) 0.0545(8) Uani 1 1 d . . . . .
H15 H 0.409062 -0.216387 0.545774 0.065 Uiso 1 1 calc R U . . .
C17 C 0.43986(18) -0.0300(3) 0.40230(16) 0.0504(7) Uani 1 1 d . . . . .
O4 O 0.1480(2) -0.0619(3) 0.82491(16) 0.1118(10) Uani 1 1 d . . . . .
H4 H 0.142259 -0.101391 0.785265 0.168 Uiso 1 1 calc R U . . .
C16 C 0.44839(18) -0.1372(3) 0.44936(17) 0.0520(7) Uani 1 1 d . . . . .
C6 C 0.25210(19) 0.2442(3) 0.45903(17) 0.0538(8) Uani 1 1 d . . . . .
H6 H 0.266014 0.234754 0.408485 0.065 Uiso 1 1 calc R U . . .
C4 C 0.2069(2) 0.2679(3) 0.60954(18) 0.0568(8) Uani 1 1 d . . . . .
C23 C 0.15845(19) 0.3581(3) 0.29987(18) 0.0570(8) Uani 1 1 d . . . . .
C1 C 0.0752(2) 0.7169(3) 0.5071(2) 0.0615(9) Uani 1 1 d . . . . .
O2 O 0.0391(2) 0.0121(3) 0.62155(18) 0.1259(12) Uani 1 1 d . . . . .
C24 C 0.2761(2) 0.4897(3) 0.33990(18) 0.0601(8) Uani 1 1 d . . . . .
C12 C 0.3019(2) -0.0485(3) 0.60955(18) 0.0654(9) Uani 1 1 d . . . . .
H12A H 0.329674 -0.104234 0.645717 0.079 Uiso 1 1 calc R U . . .
H12B H 0.246052 -0.081778 0.599650 0.079 Uiso 1 1 calc R U . . .
C3 C 0.1214(2) 0.4570(3) 0.57942(18) 0.0616(9) Uani 1 1 d . . . . .
H3A H 0.099061 0.436225 0.628613 0.074 Uiso 1 1 calc R U . . .
H3B H 0.074538 0.464856 0.544270 0.074 Uiso 1 1 calc R U . . .
C2 C 0.1680(2) 0.5844(3) 0.58420(19) 0.0656(9) Uani 1 1 d . . . . .
H2A H 0.196231 0.590930 0.632888 0.079 Uiso 1 1 calc R U . . .
H2B H 0.210451 0.587365 0.545415 0.079 Uiso 1 1 calc R U . . .
C29 C 0.1935(2) 0.3516(3) 0.22843(18) 0.0642(9) Uani 1 1 d . . . . .
H29 H 0.165583 0.305535 0.191003 0.077 Uiso 1 1 calc R U . . .
C8 C 0.2957(2) 0.0840(3) 0.64193(17) 0.0649(9) Uani 1 1 d . . . . .
H8A H 0.260501 0.082835 0.686218 0.078 Uiso 1 1 calc R U . . .
H8B H 0.351124 0.113467 0.657154 0.078 Uiso 1 1 calc R U . . .
C27 C 0.2682(2) 0.4110(3) 0.21082(19) 0.0653(9) Uani 1 1 d . . . . .
C26 C 0.3078(2) 0.4816(3) 0.2673(2) 0.0690(10) Uani 1 1 d . . . . .
H26 H 0.357120 0.524732 0.256192 0.083 Uiso 1 1 calc R U . . .
C20 C 0.5224(2) -0.3310(3) 0.4743(2) 0.0699(10) Uani 1 1 d . . . . .
H20A H 0.545251 -0.297952 0.520764 0.105 Uiso 1 1 calc R U . . .
H20B H 0.562900 -0.385850 0.451207 0.105 Uiso 1 1 calc R U . . .
H20C H 0.472291 -0.378394 0.484558 0.105 Uiso 1 1 calc R U . . .
O3 O 0.0966(3) 0.1077(3) 0.87652(18) 0.1433(14) Uani 1 1 d . . . . .
C11 C 0.0708(2) -0.0178(4) 0.6828(2) 0.0729(10) Uani 1 1 d . . . . .
C10 C 0.1029(3) 0.0406(4) 0.8222(2) 0.0847(12) Uani 1 1 d . . . . .
C19 C 0.4823(3) 0.0798(3) 0.29100(19) 0.0826(11) Uani 1 1 d . . . . .
H19A H 0.425910 0.088118 0.271863 0.124 Uiso 1 1 calc R U . . .
H19B H 0.520159 0.070249 0.249605 0.124 Uiso 1 1 calc R U . . .
H19C H 0.497094 0.154450 0.319430 0.124 Uiso 1 1 calc R U . . .
C9 C 0.0586(3) 0.0709(4) 0.7486(3) 0.0799(12) Uani 1 1 d . . . . .
C22 C 0.0770(2) 0.2906(4) 0.3164(2) 0.0837(11) Uani 1 1 d . . . . .
H22A H 0.049996 0.266704 0.269773 0.125 Uiso 1 1 calc R U . . .
H22B H 0.040891 0.346458 0.344038 0.125 Uiso 1 1 calc R U . . .
H22C H 0.088374 0.215760 0.345889 0.125 Uiso 1 1 calc R U . . .
C25 C 0.3229(3) 0.5621(4) 0.4003(2) 0.0916(12) Uani 1 1 d . . . . .
H25A H 0.287513 0.628150 0.419818 0.137 Uiso 1 1 calc R U . . .
H25B H 0.372450 0.599401 0.379355 0.137 Uiso 1 1 calc R U . . .
H25C H 0.338552 0.505129 0.440463 0.137 Uiso 1 1 calc R U . . .
C28 C 0.3070(3) 0.3983(4) 0.1337(2) 0.0939(13) Uani 1 1 d . . . . .
H28A H 0.338566 0.320520 0.131345 0.141 Uiso 1 1 calc R U . . .
H28B H 0.343741 0.469135 0.124915 0.141 Uiso 1 1 calc R U . . .
H28C H 0.263469 0.397129 0.095741 0.141 Uiso 1 1 calc R U . . .
H100 H 0.108(3) 0.748(4) 0.612(2) 0.122(16) Uiso 1 1 d . . . . .
H101 H 0.080(3) 0.154(5) 0.736(3) 0.16(2) Uiso 1 1 d . . . . .
H102 H 0.002(4) 0.079(5) 0.766(3) 0.18(2) Uiso 1 1 d . . . . .
H103 H 0.133(2) 0.506(3) 0.4472(17) 0.081(10) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O5 0.0769(15) 0.0456(12) 0.0721(15) 0.0026(11) 0.0112(12) 0.0121(11)
O6 0.0761(15) 0.0561(13) 0.0574(13) 0.0036(11) 0.0177(11) 0.0076(11)
O8 0.0807(16) 0.0602(14) 0.0650(15) -0.0102(12) 0.0005(12) 0.0177(12)
O7 0.0876(17) 0.0760(16) 0.0536(14) 0.0015(12) 0.0182(12) 0.0121(13)
N3 0.0591(16) 0.0521(15) 0.0499(15) 0.0009(12) 0.0087(12) 0.0092(12)
N5 0.0631(17) 0.0514(15) 0.0516(16) -0.0028(13) 0.0038(13) 0.0138(13)
N4 0.0593(16) 0.0542(15) 0.0490(15) 0.0049(12) 0.0084(12) 0.0096(13)
O1 0.0951(19) 0.0715(16) 0.0796(17) -0.0201(13) 0.0048(14) 0.0170(15)
N2 0.0731(19) 0.0608(18) 0.065(2) -0.0147(16) -0.0019(16) 0.0185(15)
C21 0.0548(19) 0.0480(17) 0.0526(19) 0.0012(15) 0.0027(15) 0.0114(15)
C14 0.0520(18) 0.0413(16) 0.0533(18) 0.0033(14) 0.0054(14) 0.0018(14)
N1 0.103(2) 0.0667(19) 0.071(2) -0.0061(15) 0.0065(17) 0.0332(18)
C7 0.0530(18) 0.0466(17) 0.0479(18) 0.0024(14) 0.0064(14) -0.0002(14)
C5 0.0560(19) 0.0499(18) 0.0475(18) -0.0008(15) 0.0028(15) 0.0044(15)
C18 0.0599(19) 0.0445(17) 0.0507(18) 0.0067(14) 0.0056(15) 0.0022(15)
C13 0.0544(19) 0.0477(17) 0.0565(19) 0.0071(15) 0.0067(15) -0.0017(15)
C15 0.0606(19) 0.0427(17) 0.060(2) 0.0097(15) 0.0033(16) -0.0004(15)
C17 0.0565(18) 0.0443(17) 0.0506(18) 0.0026(14) 0.0085(15) -0.0011(14)
O4 0.146(3) 0.105(2) 0.084(2) -0.0225(17) -0.0099(19) 0.025(2)
C16 0.0542(18) 0.0423(16) 0.0596(19) -0.0014(14) 0.0025(15) 0.0032(14)
C6 0.063(2) 0.0492(17) 0.0491(18) 0.0006(14) 0.0063(15) 0.0106(15)
C4 0.060(2) 0.0555(19) 0.055(2) 0.0007(16) 0.0092(16) 0.0034(16)
C23 0.0552(19) 0.060(2) 0.056(2) -0.0008(16) -0.0005(16) 0.0054(16)
C1 0.063(2) 0.053(2) 0.068(2) -0.0039(18) 0.0090(18) 0.0068(17)
O2 0.178(3) 0.107(2) 0.091(2) -0.0200(19) -0.036(2) 0.049(2)
C24 0.060(2) 0.061(2) 0.060(2) 0.0023(16) -0.0011(17) 0.0038(17)
C12 0.068(2) 0.061(2) 0.068(2) 0.0192(17) 0.0159(17) 0.0075(17)
C3 0.062(2) 0.062(2) 0.061(2) -0.0039(16) 0.0124(16) 0.0148(17)
C2 0.066(2) 0.064(2) 0.067(2) -0.0147(17) -0.0017(17) 0.0136(18)
C29 0.067(2) 0.071(2) 0.055(2) -0.0040(17) -0.0023(17) 0.0041(18)
C8 0.072(2) 0.070(2) 0.0520(19) 0.0139(17) 0.0114(16) 0.0140(18)
C27 0.065(2) 0.073(2) 0.058(2) 0.0032(18) 0.0083(17) 0.0174(19)
C26 0.053(2) 0.074(2) 0.080(3) 0.011(2) 0.0053(19) 0.0012(18)
C20 0.080(2) 0.0460(18) 0.084(2) 0.0072(18) -0.0036(19) 0.0093(17)
O3 0.233(4) 0.101(2) 0.097(2) -0.047(2) 0.030(2) -0.007(3)
C11 0.076(3) 0.066(2) 0.077(3) -0.013(2) 0.007(2) 0.001(2)
C10 0.110(3) 0.068(3) 0.077(3) -0.022(2) 0.029(2) -0.013(2)
C19 0.113(3) 0.068(2) 0.067(2) 0.0141(19) 0.032(2) 0.009(2)
C9 0.090(3) 0.068(3) 0.082(3) -0.018(2) 0.020(2) 0.002(2)
C22 0.074(3) 0.102(3) 0.075(3) -0.003(2) 0.000(2) -0.018(2)
C25 0.095(3) 0.095(3) 0.084(3) 0.002(2) -0.013(2) -0.026(2)
C28 0.095(3) 0.121(3) 0.067(2) 0.004(2) 0.024(2) 0.018(3)

_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
O5 C16 1.362(3) . ?
O5 C20 1.437(3) . ?
O6 C17 1.366(3) . ?
O6 C19 1.433(4) . ?
O8 C1 1.249(4) . ?
O7 C4 1.215(3) . ?
N3 C5 1.366(3) . ?
N3 C4 1.401(4) . ?
N3 C3 1.478(3) . ?
N5 C5 1.332(4) . ?
N5 C21 1.444(4) . ?
N4 C7 1.374(3) . ?
N4 C4 1.390(4) . ?
N4 C8 1.481(4) . ?
O1 C11 1.264(4) . ?
N2 C1 1.348(4) . ?
N2 C2 1.452(4) . ?
C21 C23 1.383(4) . ?
C21 C24 1.390(4) . ?
C14 C13 1.390(4) . ?
C14 C18 1.407(4) . ?
C14 C7 1.459(4) . ?
N1 C1 1.346(4) . ?
C7 C6 1.356(4) . ?
C5 C6 1.401(4) . ?
C18 C17 1.370(4) . ?
C13 C15 1.397(4) . ?
C13 C12 1.503(4) . ?
C15 C16 1.378(4) . ?
C17 C16 1.407(4) . ?
O4 C10 1.295(5) . ?
C23 C29 1.391(4) . ?
C23 C22 1.510(4) . ?
O2 C11 1.231(4) . ?
C24 C26 1.389(4) . ?
C24 C25 1.504(5) . ?
C12 C8 1.509(4) . ?
C3 C2 1.532(4) . ?
C29 C27 1.382(4) . ?
C27 C26 1.391(5) . ?
C27 C28 1.513(4) . ?
O3 C10 1.197(4) . ?
C11 C9 1.508(5) . ?
C10 C9 1.509(6) . ?

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
C16 O5 C20 117.3(2) . . ?
C17 O6 C19 117.2(2) . . ?
C5 N3 C4 122.4(2) . . ?
C5 N3 C3 120.0(2) . . ?
C4 N3 C3 117.6(2) . . ?
C5 N5 C21 118.9(2) . . ?
C7 N4 C4 122.5(2) . . ?
C7 N4 C8 119.5(2) . . ?
C4 N4 C8 117.8(2) . . ?
C1 N2 C2 121.0(3) . . ?
C23 C21 C24 122.2(3) . . ?
C23 C21 N5 119.6(3) . . ?
C24 C21 N5 118.2(3) . . ?
C13 C14 C18 120.0(3) . . ?
C13 C14 C7 119.7(3) . . ?
C18 C14 C7 120.3(3) . . ?
C6 C7 N4 119.1(3) . . ?
C6 C7 C14 122.4(3) . . ?
N4 C7 C14 118.5(3) . . ?
N5 C5 N3 119.7(3) . . ?
N5 C5 C6 122.1(3) . . ?
N3 C5 C6 118.3(3) . . ?
C17 C18 C14 120.8(3) . . ?
C14 C13 C15 118.9(3) . . ?
C14 C13 C12 118.2(3) . . ?
C15 C13 C12 122.9(3) . . ?
C16 C15 C13 121.0(3) . . ?
O6 C17 C18 124.8(3) . . ?
O6 C17 C16 115.9(3) . . ?
C18 C17 C16 119.3(3) . . ?
O5 C16 C15 125.1(3) . . ?
O5 C16 C17 114.8(3) . . ?
C15 C16 C17 120.0(3) . . ?
C7 C6 C5 121.2(3) . . ?
O7 C4 N4 122.2(3) . . ?
O7 C4 N3 121.4(3) . . ?
N4 C4 N3 116.4(3) . . ?
C21 C23 C29 117.6(3) . . ?
C21 C23 C22 121.8(3) . . ?
C29 C23 C22 120.6(3) . . ?
O8 C1 N2 121.8(3) . . ?
O8 C1 N1 121.4(3) . . ?
N2 C1 N1 116.8(3) . . ?
C26 C24 C21 117.8(3) . . ?
C26 C24 C25 120.5(3) . . ?
C21 C24 C25 121.7(3) . . ?
C13 C12 C8 109.9(3) . . ?
N3 C3 C2 112.0(2) . . ?
N2 C2 C3 111.8(3) . . ?
C27 C29 C23 122.6(3) . . ?
N4 C8 C12 109.8(3) . . ?
C29 C27 C26 117.5(3) . . ?
C29 C27 C28 121.7(3) . . ?
C26 C27 C28 120.7(3) . . ?
C24 C26 C27 122.1(3) . . ?
O2 C11 O1 123.9(4) . . ?
O2 C11 C9 117.9(4) . . ?
O1 C11 C9 118.2(4) . . ?
O3 C10 O4 120.7(5) . . ?
O3 C10 C9 121.8(4) . . ?
O4 C10 C9 117.4(3) . . ?
C10 C9 C11 118.3(4) . . ?

_refine_diff_density_max         0.205
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.043

_shelx_res_file                  
;
TITL DATA_M_a.res in P2(1)/n
    DATA_M_a.res
    created by SHELXL-2018/3 at 10:29:03 on 30-Dec-2023
CELL  0.71073  15.9253  10.5056  17.7110   90.000   90.685   90.000
ZERR    1.000   0.0029   0.0019   0.0037    0.000    0.006    0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C  H  N  O
UNIT 59  59  59  59
L.S. 10
ACTA
BOND
FMAP 2
PLAN 20
TEMP 25.850
WGHT    0.041600    2.185600
EXTI    0.007159
FVAR       0.48974
O5    4    0.502729   -0.227442    0.424177    11.00000    0.07694    0.04565 =
         0.07210    0.00260    0.01123    0.01208
O6    4    0.487859   -0.029862    0.338895    11.00000    0.07608    0.05606 =
         0.05736    0.00360    0.01772    0.00757
O8    4    0.083227    0.643878    0.451948    11.00000    0.08073    0.06016 =
         0.06495   -0.01016    0.00049    0.01774
O7    4    0.187786    0.279045    0.675403    11.00000    0.08761    0.07601 =
         0.05364    0.00151    0.01820    0.01212
N3    3    0.176812    0.352642    0.554455    11.00000    0.05914    0.05208 =
         0.04986    0.00088    0.00874    0.00924
N5    3    0.170196    0.429316    0.430913    11.00000    0.06311    0.05144 =
         0.05159   -0.00282    0.00375    0.01379
N4    3    0.259542    0.171546    0.584674    11.00000    0.05928    0.05417 =
         0.04899    0.00495    0.00844    0.00961
O1    4    0.112811   -0.118350    0.693555    11.00000    0.09511    0.07150 =
         0.07956   -0.02010    0.00479    0.01703
N2    3    0.111333    0.691577    0.574626    11.00000    0.07309    0.06080 =
         0.06500   -0.01467   -0.00190    0.01851
C21   1    0.201300    0.426749    0.354703    11.00000    0.05477    0.04802 =
         0.05264    0.00116    0.00268    0.01142
C14   1    0.341833    0.059701    0.490581    11.00000    0.05204    0.04129 =
         0.05330    0.00328    0.00539    0.00181
N1    3    0.028144    0.823065    0.502182    11.00000    0.10310    0.06672 =
         0.07143   -0.00606    0.00648    0.03319
AFIX  93
H1A   2    0.002833    0.841842    0.460487    11.00000   -1.20000
H1B   2    0.023392    0.872130    0.540765    11.00000   -1.20000
AFIX   0
C7    1    0.283542    0.161019    0.510682    11.00000    0.05300    0.04662 =
         0.04792    0.00243    0.00642   -0.00016
C5    1    0.199048    0.343921    0.480382    11.00000    0.05602    0.04993 =
         0.04745   -0.00083    0.00282    0.00442
C18   1    0.386625    0.066136    0.422711    11.00000    0.05990    0.04453 =
         0.05070    0.00666    0.00555    0.00216
AFIX  43
H18   2    0.380025    0.136488    0.391326    11.00000   -1.20000
AFIX   0
C13   1    0.350775   -0.045676    0.537483    11.00000    0.05439    0.04766 =
         0.05648    0.00714    0.00674   -0.00170
C15   1    0.403790   -0.144537    0.515412    11.00000    0.06057    0.04274 =
         0.06034    0.00971    0.00334   -0.00043
AFIX  43
H15   2    0.409062   -0.216387    0.545774    11.00000   -1.20000
AFIX   0
C17   1    0.439864   -0.030028    0.402299    11.00000    0.05653    0.04431 =
         0.05056    0.00261    0.00846   -0.00112
O4    4    0.148019   -0.061856    0.824910    11.00000    0.14630    0.10458 =
         0.08410   -0.02250   -0.00995    0.02541
AFIX 147
H4    2    0.142259   -0.101391    0.785265    11.00000   -1.50000
AFIX   0
C16   1    0.448386   -0.137234    0.449358    11.00000    0.05425    0.04228 =
         0.05956   -0.00137    0.00248    0.00317
C6    1    0.252100    0.244150    0.459027    11.00000    0.06337    0.04919 =
         0.04911    0.00063    0.00629    0.01061
AFIX  43
H6    2    0.266014    0.234754    0.408485    11.00000   -1.20000
AFIX   0
C4    1    0.206859    0.267901    0.609542    11.00000    0.06036    0.05546 =
         0.05472    0.00065    0.00915    0.00341
C23   1    0.158452    0.358079    0.299873    11.00000    0.05515    0.06016 =
         0.05577   -0.00080   -0.00050    0.00544
C1    1    0.075209    0.716858    0.507055    11.00000    0.06321    0.05308 =
         0.06834   -0.00388    0.00900    0.00682
O2    4    0.039133    0.012150    0.621555    11.00000    0.17836    0.10748 =
         0.09108   -0.02001   -0.03574    0.04921
C24   1    0.276087    0.489710    0.339902    11.00000    0.05995    0.06064 =
         0.05976    0.00233   -0.00106    0.00383
C12   1    0.301935   -0.048547    0.609551    11.00000    0.06783    0.06065 =
         0.06820    0.01923    0.01595    0.00751
AFIX  23
H12A  2    0.329674   -0.104234    0.645717    11.00000   -1.20000
H12B  2    0.246052   -0.081778    0.599650    11.00000   -1.20000
AFIX   0
C3    1    0.121428    0.456954    0.579417    11.00000    0.06158    0.06214 =
         0.06129   -0.00390    0.01244    0.01478
AFIX  23
H3A   2    0.099061    0.436225    0.628613    11.00000   -1.20000
H3B   2    0.074538    0.464856    0.544270    11.00000   -1.20000
AFIX   0
C2    1    0.168008    0.584398    0.584204    11.00000    0.06621    0.06394 =
         0.06673   -0.01466   -0.00169    0.01359
AFIX  23
H2A   2    0.196231    0.590930    0.632888    11.00000   -1.20000
H2B   2    0.210451    0.587365    0.545415    11.00000   -1.20000
AFIX   0
C29   1    0.193520    0.351639    0.228431    11.00000    0.06656    0.07138 =
         0.05457   -0.00399   -0.00230    0.00414
AFIX  43
H29   2    0.165583    0.305535    0.191003    11.00000   -1.20000
AFIX   0
C8    1    0.295744    0.083965    0.641931    11.00000    0.07244    0.07040 =
         0.05204    0.01390    0.01140    0.01405
AFIX  23
H8A   2    0.260501    0.082835    0.686218    11.00000   -1.20000
H8B   2    0.351124    0.113467    0.657154    11.00000   -1.20000
AFIX   0
C27   1    0.268230    0.411015    0.210823    11.00000    0.06505    0.07292 =
         0.05821    0.00319    0.00827    0.01740
C26   1    0.307808    0.481578    0.267338    11.00000    0.05325    0.07431 =
         0.07964    0.01091    0.00525    0.00124
AFIX  43
H26   2    0.357120    0.524732    0.256192    11.00000   -1.20000
AFIX   0
C20   1    0.522427   -0.331002    0.474339    11.00000    0.07982    0.04599 =
         0.08385    0.00723   -0.00356    0.00927
AFIX 137
H20A  2    0.545251   -0.297952    0.520764    11.00000   -1.50000
H20B  2    0.562900   -0.385850    0.451207    11.00000   -1.50000
H20C  2    0.472291   -0.378394    0.484558    11.00000   -1.50000
AFIX   0
O3    4    0.096648    0.107685    0.876523    11.00000    0.23263    0.10139 =
         0.09661   -0.04728    0.02953   -0.00677
C11   1    0.070823   -0.017787    0.682756    11.00000    0.07595    0.06575 =
         0.07717   -0.01305    0.00687    0.00134
C10   1    0.102866    0.040588    0.822241    11.00000    0.11012    0.06795 =
         0.07675   -0.02187    0.02934   -0.01303
C19   1    0.482296    0.079782    0.290998    11.00000    0.11316    0.06813 =
         0.06717    0.01405    0.03173    0.00946
AFIX 137
H19A  2    0.425910    0.088118    0.271863    11.00000   -1.50000
H19B  2    0.520159    0.070249    0.249605    11.00000   -1.50000
H19C  2    0.497094    0.154450    0.319430    11.00000   -1.50000
AFIX   0
C9    1    0.058614    0.070948    0.748615    11.00000    0.08982    0.06815 =
         0.08217   -0.01787    0.02012    0.00206
C22   1    0.077016    0.290609    0.316397    11.00000    0.07378    0.10221 =
         0.07500   -0.00288    0.00041   -0.01826
AFIX 137
H22A  2    0.049996    0.266704    0.269773    11.00000   -1.50000
H22B  2    0.040891    0.346458    0.344038    11.00000   -1.50000
H22C  2    0.088374    0.215760    0.345889    11.00000   -1.50000
AFIX   0
C25   1    0.322881    0.562146    0.400350    11.00000    0.09550    0.09525 =
         0.08369    0.00186   -0.01308   -0.02641
AFIX 137
H25A  2    0.287513    0.628150    0.419818    11.00000   -1.50000
H25B  2    0.372450    0.599401    0.379355    11.00000   -1.50000
H25C  2    0.338552    0.505129    0.440463    11.00000   -1.50000
AFIX   0
C28   1    0.307047    0.398287    0.133658    11.00000    0.09480    0.12057 =
         0.06673    0.00448    0.02374    0.01843
AFIX 137
H28A  2    0.338566    0.320520    0.131345    11.00000   -1.50000
H28B  2    0.343741    0.469135    0.124915    11.00000   -1.50000
H28C  2    0.263469    0.397129    0.095741    11.00000   -1.50000
AFIX   0
H100  2    0.108000    0.747791    0.612167    11.00000    0.12219
H101  2    0.079990    0.153941    0.735593    11.00000    0.15689
H102  2    0.001593    0.079003    0.765507    11.00000    0.18420
H103  2    0.133486    0.505722    0.447215    11.00000    0.08067
HKLF 4




REM  DATA_M_a.res in P2(1)/n
REM wR2 = 0.171010, GooF = S = 1.00833, Restrained GooF = 1.00833 for all data
REM R1 = 0.057101 for 2938 Fo > 4sig(Fo) and 0.166265 for all 6766 data
REM 402 parameters refined using 0 restraints

END

WGHT      0.0650      1.3867

REM Highest difference peak  0.205,  deepest hole -0.179,  1-sigma level  0.043
Q1    1   0.0746 -0.0926  0.6204  11.00000  0.05    0.21
Q2    1   0.0534  0.2862  0.3789  11.00000  0.05    0.17
Q3    1   0.2597 -0.0601  0.6839  11.00000  0.05    0.17
Q4    1   0.0647  0.9052  0.5643  11.00000  0.05    0.17
Q5    1   0.0122  0.1043  0.8628  11.00000  0.05    0.17
Q6    1   0.0000  1.0000  0.5000  10.50000  0.05    0.17
Q7    1   0.0986 -0.0849  0.7603  11.00000  0.05    0.16
Q8    1   0.1228  0.1662  0.8422  11.00000  0.05    0.16
Q9    1   0.0163  0.0763  0.6880  11.00000  0.05    0.16
Q10   1  -0.0539  0.9549  0.5013  11.00000  0.05    0.16
Q11   1   0.4943 -0.3274  0.5410  11.00000  0.05    0.16
Q12   1   0.2358  0.3438  0.4077  11.00000  0.05    0.15
Q13   1   0.3810  0.4195  0.1222  11.00000  0.05    0.15
Q14   1   0.1398  0.3664  0.6333  11.00000  0.05    0.15
Q15   1   0.0575 -0.0735  0.8195  11.00000  0.05    0.15
Q16   1   0.0013  0.8266  0.3724  11.00000  0.05    0.15
Q17   1   0.4857 -0.1473  0.3048  11.00000  0.05    0.15
Q18   1   0.1215  0.0465  0.8722  11.00000  0.05    0.15
Q19   1   0.1580  0.4562  0.5013  11.00000  0.05    0.14
Q20   1  -0.0203  0.7576  0.3926  11.00000  0.05    0.14
;
_shelx_res_checksum              19904
####################################################################### 
# 
# 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_DDDD_a
_database_code_depnum_ccdc_archive 'CCDC 2358077'
loop_
_audit_author_name
_audit_author_address
'Lopamudra LOPAMUDRA GIRI'
;ICT Bhubaneswar
India
;
_audit_update_record             
;
2024-05-24 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H31 N5 O4, C7 H5 O3'
_chemical_formula_sum            'C33 H36 N5 O7'
_chemical_formula_weight         614.67

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.3541(8)
_cell_length_b                   19.1514(17)
_cell_length_c                   20.0769(18)
_cell_angle_alpha                90
_cell_angle_beta                 100.231(3)
_cell_angle_gamma                90
_cell_volume                     3161.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    3446
_cell_measurement_theta_min      0.978
_cell_measurement_theta_max      0.984

_exptl_crystal_description       Block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_F_000             1300.0
_exptl_transmission_factor_min   0.978
_exptl_transmission_factor_max   0.984
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.092
_shelx_estimated_absorpt_T_min   0.978
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'Bruker D8 Venture photon 100 CMOS detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            57687
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_av_R_equivalents  0.1001
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.320
_diffrn_reflns_theta_max         27.623
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7344
_reflns_number_gt                3446
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SHELXL'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0900P)²+1.4303P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.023(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7279
_refine_ls_number_parameters     417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1550
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.2316
_refine_ls_wR_factor_gt          0.1596
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

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
O4 O 0.9307(3) 0.25367(11) 1.07791(10) 0.0707(7) Uani 1 1 d . . . . .
O5 O 0.8728(3) 0.13013(11) 1.11730(10) 0.0710(6) Uani 1 1 d . . . . .
N5 N 0.3933(3) 0.39280(12) 0.78318(12) 0.0606(7) Uani 1 1 d . . . . .
O7 O 0.3225(3) 0.45198(11) 0.65889(11) 0.0801(7) Uani 1 1 d . . . . .
O6 O 0.2875(3) 0.16355(12) 0.72297(11) 0.0849(8) Uani 1 1 d . . . . .
N3 N 0.3362(3) 0.27684(12) 0.75356(11) 0.0585(7) Uani 1 1 d . . . . .
O2 O 1.1272(3) 0.30412(13) 0.44941(13) 0.0861(7) Uani 1 1 d . . . . .
O3 O 1.0130(3) 0.40835(13) 0.43373(12) 0.0876(8) Uani 1 1 d . . . . .
N4 N 0.4242(3) 0.18453(12) 0.82961(11) 0.0588(7) Uani 1 1 d . . . . .
N1 N 0.1908(4) 0.47087(14) 0.55167(13) 0.0756(8) Uani 1 1 d . . . . .
H1A H 0.180845 0.514697 0.559305 0.091 Uiso 1 1 calc R U . . .
H1B H 0.152799 0.453927 0.512374 0.091 Uiso 1 1 calc R U . . .
N2 N 0.2802(3) 0.36190(14) 0.58449(13) 0.0665(7) Uani 1 1 d . . . . .
C22 C 0.4477(4) 0.44729(15) 0.83142(14) 0.0562(7) Uani 1 1 d . . . . .
C12 C 0.5999(3) 0.20343(14) 0.93834(13) 0.0506(7) Uani 1 1 d . . . . .
C18 C 0.4060(3) 0.32510(15) 0.79960(14) 0.0549(7) Uani 1 1 d . . . . .
C11 C 0.7205(3) 0.24437(15) 0.97772(13) 0.0550(7) Uani 1 1 d . . . . .
H11 H 0.740336 0.289252 0.963481 0.066 Uiso 1 1 calc R U . . .
C31 C 0.8094(3) 0.21916(14) 1.03693(13) 0.0540(7) Uani 1 1 d . . . . .
C15 C 0.5037(3) 0.23133(14) 0.87592(13) 0.0509(7) Uani 1 1 d . . . . .
C33 C 0.6607(4) 0.11096(15) 1.01924(14) 0.0571(7) Uani 1 1 d . . . . .
H33 H 0.640589 0.066110 1.033475 0.069 Uiso 1 1 calc R U . . .
C17 C 0.4904(3) 0.30079(14) 0.86208(14) 0.0553(7) Uani 1 1 d . . . . .
H17 H 0.537918 0.332757 0.894535 0.066 Uiso 1 1 calc R U . . .
C32 C 0.5718(3) 0.13627(15) 0.95880(14) 0.0541(7) Uani 1 1 d . . . . .
C10 C 0.7778(3) 0.15115(15) 1.05822(13) 0.0554(7) Uani 1 1 d . . . . .
C21 C 0.2653(4) 0.42914(17) 0.60080(15) 0.0639(8) Uani 1 1 d . . . . .
O1 O 1.0630(5) 0.21157(16) 0.3614(2) 0.1301(12) Uani 1 1 d . . . . .
H103 H 1.098152 0.228760 0.398489 0.195 Uiso 1 1 calc R U . . .
C19 C 0.2435(4) 0.29904(16) 0.68753(14) 0.0628(8) Uani 1 1 d . . . . .
H19A H 0.182869 0.341054 0.693627 0.075 Uiso 1 1 calc R U . . .
H19B H 0.165944 0.262888 0.670137 0.075 Uiso 1 1 calc R U . . .
C13 C 0.4455(4) 0.09232(16) 0.91567(15) 0.0653(8) Uani 1 1 d . . . . .
H13A H 0.340556 0.100599 0.928501 0.078 Uiso 1 1 calc R U . . .
H13B H 0.472294 0.043362 0.923433 0.078 Uiso 1 1 calc R U . . .
C16 C 0.3448(4) 0.20547(15) 0.76594(15) 0.0624(8) Uani 1 1 d . . . . .
C14 C 0.4352(4) 0.10865(15) 0.84197(16) 0.0712(9) Uani 1 1 d . . . . .
H14A H 0.530631 0.090387 0.826606 0.085 Uiso 1 1 calc R U . . .
H14B H 0.340212 0.085936 0.816164 0.085 Uiso 1 1 calc R U . . .
C26 C 0.5464(5) 0.55666(19) 0.91997(18) 0.0785(10) Uani 1 1 d . . . . .
C1 C 1.0329(4) 0.34809(18) 0.41466(16) 0.0659(8) Uani 1 1 d . . . . .
C2 C 0.9450(4) 0.32490(17) 0.34678(16) 0.0656(8) Uani 1 1 d . . . . .
C24 C 0.3381(4) 0.47807(18) 0.8656(2) 0.0785(10) Uani 1 1 d . . . . .
C20 C 0.3534(4) 0.31325(17) 0.63619(16) 0.0720(9) Uani 1 1 d . . . . .
H20A H 0.456021 0.332102 0.659388 0.086 Uiso 1 1 calc R U . . .
H20B H 0.375759 0.269664 0.615016 0.086 Uiso 1 1 calc R U . . .
C30 C 0.6062(4) 0.4709(2) 0.84039(18) 0.0803(10) Uani 1 1 d . . . . .
C9 C 0.8545(5) 0.06009(18) 1.13762(17) 0.0809(10) Uani 1 1 d . . . . .
H9A H 0.744329 0.052530 1.143607 0.121 Uiso 1 1 calc R U . . .
H9B H 0.926957 0.051363 1.179535 0.121 Uiso 1 1 calc R U . . .
H9C H 0.879790 0.028957 1.103474 0.121 Uiso 1 1 calc R U . . .
C25 C 0.3919(5) 0.53212(19) 0.9101(2) 0.0890(12) Uani 1 1 d . . . . .
H25 H 0.318542 0.552399 0.934169 0.107 Uiso 1 1 calc R U . . .
C8 C 0.9663(5) 0.32217(19) 1.0597(2) 0.0950(13) Uani 1 1 d . . . . .
H8A H 1.003605 0.321372 1.017147 0.142 Uiso 1 1 calc R U . . .
H8B H 1.049572 0.341485 1.093856 0.142 Uiso 1 1 calc R U . . .
H8C H 0.870048 0.350360 1.055664 0.142 Uiso 1 1 calc R U . . .
C27 C 0.6515(5) 0.5256(2) 0.8850(2) 0.0939(12) Uani 1 1 d . . . . .
H27 H 0.758166 0.541593 0.891098 0.113 Uiso 1 1 calc R U . . .
C7 C 0.9634(5) 0.2579(2) 0.3235(2) 0.0854(11) Uani 1 1 d . . . . .
C3 C 0.8449(5) 0.3709(2) 0.30554(18) 0.0873(11) Uani 1 1 d . . . . .
H3 H 0.834790 0.416497 0.320202 0.105 Uiso 1 1 calc R U . . .
C6 C 0.8808(6) 0.2374(3) 0.2604(3) 0.1083(15) Uani 1 1 d . . . . .
H6 H 0.894409 0.192501 0.244749 0.130 Uiso 1 1 calc R U . . .
C29 C 0.5980(7) 0.6175(2) 0.9677(2) 0.1231(17) Uani 1 1 d . . . . .
H29A H 0.641608 0.599890 1.012002 0.185 Uiso 1 1 calc R U . . .
H29B H 0.505459 0.646469 0.970086 0.185 Uiso 1 1 calc R U . . .
H29C H 0.679586 0.644459 0.951187 0.185 Uiso 1 1 calc R U . . .
C5 C 0.7800(6) 0.2830(3) 0.2215(2) 0.1174(18) Uani 1 1 d . . . . .
H5 H 0.723564 0.268590 0.179589 0.141 Uiso 1 1 calc R U . . .
C4 C 0.7600(6) 0.3509(3) 0.2435(2) 0.1125(15) Uani 1 1 d . . . . .
H4 H 0.690812 0.381982 0.216789 0.135 Uiso 1 1 calc R U . . .
C23 C 0.1607(5) 0.4564(3) 0.8534(4) 0.155(3) Uani 1 1 d . . . . .
H23A H 0.112377 0.466419 0.807375 0.233 Uiso 1 1 calc R U . . .
H23B H 0.104419 0.481892 0.883394 0.233 Uiso 1 1 calc R U . . .
H23C H 0.153036 0.407293 0.861749 0.233 Uiso 1 1 calc R U . . .
C28 C 0.7244(6) 0.4377(4) 0.8015(3) 0.171(3) Uani 1 1 d . . . . .
H28A H 0.665840 0.417455 0.760540 0.257 Uiso 1 1 calc R U . . .
H28B H 0.784552 0.401856 0.828580 0.257 Uiso 1 1 calc R U . . .
H28C H 0.798210 0.472458 0.790474 0.257 Uiso 1 1 calc R U . . .
H102 H 0.231(4) 0.3433(18) 0.5446(18) 0.078(10) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O4 0.0758(14) 0.0642(13) 0.0610(12) 0.0002(10) -0.0182(11) -0.0093(11)
O5 0.0885(16) 0.0630(13) 0.0523(12) 0.0069(10) -0.0130(11) 0.0020(11)
N5 0.0724(16) 0.0487(14) 0.0536(14) -0.0019(11) -0.0077(12) 0.0002(12)
O7 0.1100(18) 0.0625(14) 0.0571(13) 0.0008(10) -0.0144(12) -0.0055(12)
O6 0.1137(19) 0.0624(14) 0.0633(13) -0.0110(11) -0.0256(13) -0.0001(13)
N3 0.0680(16) 0.0521(14) 0.0467(13) -0.0005(10) -0.0140(11) -0.0001(11)
O2 0.0886(17) 0.0854(17) 0.0793(16) 0.0047(13) 0.0009(13) 0.0084(14)
O3 0.0998(18) 0.0755(17) 0.0786(16) -0.0190(13) -0.0087(13) 0.0089(13)
N4 0.0678(15) 0.0483(13) 0.0526(13) -0.0007(11) -0.0107(11) 0.0008(11)
N1 0.106(2) 0.0598(16) 0.0534(15) 0.0075(12) -0.0069(14) 0.0060(15)
N2 0.0863(19) 0.0621(17) 0.0460(14) -0.0001(12) -0.0025(13) 0.0077(14)
C22 0.0647(19) 0.0503(16) 0.0483(15) 0.0022(13) -0.0044(13) 0.0008(14)
C12 0.0536(16) 0.0506(16) 0.0447(14) -0.0004(12) 0.0008(12) 0.0017(12)
C18 0.0560(17) 0.0536(17) 0.0502(15) -0.0016(13) -0.0041(13) 0.0003(13)
C11 0.0605(17) 0.0511(16) 0.0498(15) 0.0023(12) 0.0000(13) 0.0007(13)
C31 0.0559(16) 0.0543(17) 0.0474(15) -0.0026(13) -0.0029(13) -0.0003(13)
C15 0.0498(15) 0.0516(16) 0.0476(15) -0.0015(12) -0.0010(12) -0.0010(12)
C33 0.0657(19) 0.0506(16) 0.0529(16) 0.0039(13) 0.0047(14) -0.0009(14)
C17 0.0627(18) 0.0518(16) 0.0448(14) -0.0012(12) -0.0080(13) 0.0006(13)
C32 0.0544(17) 0.0540(17) 0.0513(15) 0.0005(13) 0.0024(13) 0.0007(13)
C10 0.0607(18) 0.0570(17) 0.0443(15) 0.0030(13) -0.0021(13) 0.0071(14)
C21 0.073(2) 0.063(2) 0.0513(17) 0.0021(15) 0.0003(15) -0.0039(16)
O1 0.154(3) 0.085(2) 0.146(3) -0.025(2) 0.014(2) 0.021(2)
C19 0.0693(19) 0.0614(18) 0.0480(16) 0.0018(13) -0.0156(14) 0.0021(15)
C13 0.069(2) 0.0576(18) 0.0633(19) 0.0037(15) -0.0048(15) -0.0070(15)
C16 0.071(2) 0.0544(18) 0.0540(17) -0.0021(14) -0.0099(14) -0.0003(14)
C14 0.090(2) 0.0499(17) 0.065(2) -0.0022(14) -0.0102(17) -0.0024(16)
C26 0.095(3) 0.066(2) 0.074(2) -0.0058(17) 0.012(2) -0.017(2)
C1 0.067(2) 0.067(2) 0.0630(19) -0.0006(17) 0.0085(16) -0.0010(16)
C2 0.068(2) 0.071(2) 0.0598(18) -0.0088(16) 0.0167(16) -0.0092(16)
C24 0.067(2) 0.062(2) 0.105(3) -0.0170(19) 0.0122(19) -0.0028(16)
C20 0.085(2) 0.068(2) 0.0578(18) -0.0005(15) -0.0034(17) 0.0144(17)
C30 0.069(2) 0.100(3) 0.074(2) -0.023(2) 0.0177(17) -0.020(2)
C9 0.103(3) 0.069(2) 0.062(2) 0.0173(17) -0.0081(18) 0.0029(19)
C25 0.092(3) 0.068(2) 0.113(3) -0.025(2) 0.033(2) -0.004(2)
C8 0.099(3) 0.073(2) 0.096(3) 0.009(2) -0.027(2) -0.022(2)
C27 0.081(3) 0.107(3) 0.095(3) -0.030(2) 0.017(2) -0.037(2)
C7 0.090(3) 0.083(3) 0.086(3) -0.020(2) 0.024(2) -0.009(2)
C3 0.097(3) 0.094(3) 0.065(2) -0.0044(19) -0.002(2) -0.002(2)
C6 0.123(4) 0.111(4) 0.097(3) -0.047(3) 0.035(3) -0.033(3)
C29 0.165(5) 0.092(3) 0.113(3) -0.038(3) 0.024(3) -0.039(3)
C5 0.114(4) 0.173(5) 0.067(3) -0.039(3) 0.021(3) -0.051(4)
C4 0.116(4) 0.146(4) 0.067(3) -0.003(3) -0.006(2) -0.009(3)
C23 0.070(3) 0.145(5) 0.253(7) -0.091(5) 0.036(4) -0.018(3)
C28 0.104(4) 0.233(7) 0.196(6) -0.125(5) 0.078(4) -0.057(4)

_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
O4 C31 1.358(3) . ?
O4 C8 1.408(4) . ?
O5 C10 1.366(3) . ?
O5 C9 1.418(4) . ?
N5 C18 1.337(3) . ?
N5 C22 1.441(4) . ?
O7 C21 1.258(3) . ?
O6 C16 1.213(3) . ?
N3 C18 1.363(3) . ?
N3 C16 1.389(4) . ?
N3 C19 1.474(3) . ?
O2 C1 1.273(4) . ?
O3 C1 1.236(4) . ?
N4 C15 1.375(3) . ?
N4 C16 1.391(3) . ?
N4 C14 1.474(4) . ?
N1 C21 1.334(4) . ?
N2 C21 1.340(4) . ?
N2 C20 1.447(4) . ?
C22 C24 1.372(5) . ?
C22 C30 1.380(4) . ?
C12 C32 1.383(4) . ?
C12 C11 1.404(4) . ?
C12 C15 1.464(4) . ?
C18 C17 1.405(4) . ?
C11 C31 1.373(4) . ?
C31 C10 1.410(4) . ?
C15 C17 1.360(4) . ?
C33 C10 1.374(4) . ?
C33 C32 1.393(4) . ?
C32 C13 1.499(4) . ?
O1 C7 1.354(5) . ?
C19 C20 1.521(5) . ?
C13 C14 1.500(4) . ?
C26 C25 1.355(5) . ?
C26 C27 1.356(5) . ?
C26 C29 1.521(5) . ?
C1 C2 1.496(4) . ?
C2 C3 1.384(5) . ?
C2 C7 1.384(5) . ?
C24 C25 1.388(5) . ?
C24 C23 1.516(5) . ?
C30 C27 1.386(5) . ?
C30 C28 1.505(6) . ?
C7 C6 1.386(6) . ?
C3 C4 1.374(5) . ?
C6 C5 1.359(7) . ?
C5 C4 1.394(7) . ?

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
C31 O4 C8 117.7(2) . . ?
C10 O5 C9 116.9(2) . . ?
C18 N5 C22 122.3(2) . . ?
C18 N3 C16 122.9(2) . . ?
C18 N3 C19 120.5(2) . . ?
C16 N3 C19 116.6(2) . . ?
C15 N4 C16 121.9(2) . . ?
C15 N4 C14 121.4(2) . . ?
C16 N4 C14 116.4(2) . . ?
C21 N2 C20 119.3(3) . . ?
C24 C22 C30 120.3(3) . . ?
C24 C22 N5 119.3(3) . . ?
C30 C22 N5 120.4(3) . . ?
C32 C12 C11 119.7(2) . . ?
C32 C12 C15 119.8(2) . . ?
C11 C12 C15 120.5(2) . . ?
N5 C18 N3 119.0(2) . . ?
N5 C18 C17 123.1(2) . . ?
N3 C18 C17 117.9(3) . . ?
C31 C11 C12 121.0(3) . . ?
O4 C31 C11 125.8(3) . . ?
O4 C31 C10 115.2(2) . . ?
C11 C31 C10 119.1(2) . . ?
C17 C15 N4 119.2(2) . . ?
C17 C15 C12 123.0(2) . . ?
N4 C15 C12 117.8(2) . . ?
C10 C33 C32 121.1(3) . . ?
C15 C17 C18 121.1(3) . . ?
C12 C32 C33 119.4(3) . . ?
C12 C32 C13 119.3(2) . . ?
C33 C32 C13 121.3(3) . . ?
O5 C10 C33 125.1(3) . . ?
O5 C10 C31 115.1(2) . . ?
C33 C10 C31 119.8(2) . . ?
O7 C21 N1 121.8(3) . . ?
O7 C21 N2 121.6(3) . . ?
N1 C21 N2 116.5(3) . . ?
N3 C19 C20 112.2(2) . . ?
C32 C13 C14 111.4(3) . . ?
O6 C16 N3 121.5(3) . . ?
O6 C16 N4 121.8(3) . . ?
N3 C16 N4 116.7(2) . . ?
N4 C14 C13 111.3(3) . . ?
C25 C26 C27 117.4(3) . . ?
C25 C26 C29 120.9(4) . . ?
C27 C26 C29 121.7(4) . . ?
O3 C1 O2 123.5(3) . . ?
O3 C1 C2 119.2(3) . . ?
O2 C1 C2 117.3(3) . . ?
C3 C2 C7 118.7(3) . . ?
C3 C2 C1 120.2(3) . . ?
C7 C2 C1 121.1(3) . . ?
C22 C24 C25 118.3(3) . . ?
C22 C24 C23 121.5(3) . . ?
C25 C24 C23 120.2(4) . . ?
N2 C20 C19 111.9(3) . . ?
C22 C30 C27 118.5(3) . . ?
C22 C30 C28 119.8(3) . . ?
C27 C30 C28 121.7(4) . . ?
C26 C25 C24 122.9(4) . . ?
C26 C27 C30 122.6(3) . . ?
O1 C7 C2 120.8(3) . . ?
O1 C7 C6 119.0(4) . . ?
C2 C7 C6 120.2(4) . . ?
C4 C3 C2 121.7(4) . . ?
C5 C6 C7 120.1(4) . . ?
C6 C5 C4 120.9(4) . . ?
C3 C4 C5 118.4(5) . . ?

_refine_diff_density_max         0.397
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.042

_shelx_res_file                  
;
TITL DDDD_a.res in P2(1)/c
    DDDD_a.res
    created by SHELXL-2018/3 at 11:41:49 on 20-Jan-2024
CELL  0.71073   8.3541  19.1514  20.0769   90.000  100.231   90.000
ZERR   63.000   0.0008   0.0017   0.0018    0.000    0.003    0.000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C  H  N  O
UNIT 63  63  63  63
L.S. 40
ACTA
BOND
FMAP 2
PLAN 20
TEMP 0
WGHT    0.090000    1.430300
EXTI    0.023090
FVAR       0.79197
O4    4    0.930672    0.253669    1.077909    11.00000    0.07578    0.06423 =
         0.06096    0.00020   -0.01815   -0.00934
O5    4    0.872790    0.130126    1.117304    11.00000    0.08850    0.06296 =
         0.05232    0.00689   -0.01300    0.00199
N5    3    0.393340    0.392796    0.783178    11.00000    0.07242    0.04872 =
         0.05362   -0.00186   -0.00775    0.00022
O7    4    0.322498    0.451979    0.658889    11.00000    0.11001    0.06248 =
         0.05713    0.00077   -0.01437   -0.00545
O6    4    0.287477    0.163551    0.722967    11.00000    0.11370    0.06244 =
         0.06328   -0.01097   -0.02556   -0.00009
N3    3    0.336174    0.276842    0.753563    11.00000    0.06798    0.05208 =
         0.04666   -0.00051   -0.01403   -0.00015
O2    4    1.127182    0.304117    0.449407    11.00000    0.08861    0.08538 =
         0.07928    0.00471    0.00088    0.00837
O3    4    1.012995    0.408353    0.433731    11.00000    0.09982    0.07551 =
         0.07858   -0.01896   -0.00870    0.00887
N4    3    0.424228    0.184528    0.829606    11.00000    0.06785    0.04829 =
         0.05255   -0.00074   -0.01069    0.00079
N1    3    0.190829    0.470867    0.551670    11.00000    0.10594    0.05975 =
         0.05342    0.00752   -0.00692    0.00598
AFIX  93
H1A   2    0.180845    0.514697    0.559305    11.00000   -1.20000
H1B   2    0.152799    0.453927    0.512374    11.00000   -1.20000
AFIX   0
N2    3    0.280199    0.361902    0.584495    11.00000    0.08628    0.06208 =
         0.04603   -0.00009   -0.00253    0.00766
C22   1    0.447747    0.447289    0.831418    11.00000    0.06470    0.05033 =
         0.04830    0.00217   -0.00444    0.00083
C12   1    0.599915    0.203426    0.938343    11.00000    0.05362    0.05056 =
         0.04475   -0.00037    0.00080    0.00173
C18   1    0.406013    0.325102    0.799595    11.00000    0.05599    0.05361 =
         0.05016   -0.00164   -0.00407    0.00031
C11   1    0.720452    0.244374    0.977721    11.00000    0.06051    0.05106 =
         0.04982    0.00234    0.00000    0.00071
AFIX  43
H11   2    0.740336    0.289252    0.963481    11.00000   -1.20000
AFIX   0
C31   1    0.809394    0.219160    1.036927    11.00000    0.05589    0.05428 =
         0.04736   -0.00255   -0.00290   -0.00032
C15   1    0.503750    0.231328    0.875919    11.00000    0.04981    0.05160 =
         0.04758   -0.00153   -0.00105   -0.00099
C33   1    0.660740    0.110962    1.019243    11.00000    0.06573    0.05056 =
         0.05293    0.00392    0.00468   -0.00092
AFIX  43
H33   2    0.640589    0.066110    1.033475    11.00000   -1.20000
AFIX   0
C17   1    0.490393    0.300795    0.862084    11.00000    0.06275    0.05181 =
         0.04484   -0.00125   -0.00797    0.00055
AFIX  43
H17   2    0.537918    0.332757    0.894535    11.00000   -1.20000
AFIX   0
C32   1    0.571820    0.136274    0.958801    11.00000    0.05441    0.05398 =
         0.05128    0.00053    0.00241    0.00074
C10   1    0.777784    0.151152    1.058219    11.00000    0.06065    0.05697 =
         0.04433    0.00302   -0.00208    0.00706
C21   1    0.265333    0.429144    0.600799    11.00000    0.07306    0.06349 =
         0.05125    0.00211    0.00027   -0.00392
O1    4    1.062975    0.211572    0.361366    11.00000    0.15448    0.08526 =
         0.14598   -0.02538    0.01406    0.02072
AFIX 147
H103  2    1.098152    0.228760    0.398489    11.00000   -1.50000
AFIX   0
C19   1    0.243506    0.299044    0.687534    11.00000    0.06932    0.06143 =
         0.04803    0.00178   -0.01563    0.00209
AFIX  23
H19A  2    0.182869    0.341054    0.693627    11.00000   -1.20000
H19B  2    0.165944    0.262888    0.670137    11.00000   -1.20000
AFIX   0
C13   1    0.445531    0.092317    0.915668    11.00000    0.06904    0.05758 =
         0.06333    0.00369   -0.00485   -0.00702
AFIX  23
H13A  2    0.340556    0.100599    0.928501    11.00000   -1.20000
H13B  2    0.472294    0.043362    0.923433    11.00000   -1.20000
AFIX   0
C16   1    0.344825    0.205471    0.765937    11.00000    0.07121    0.05435 =
         0.05400   -0.00213   -0.00989   -0.00026
C14   1    0.435165    0.108652    0.841967    11.00000    0.08959    0.04990 =
         0.06536   -0.00222   -0.01019   -0.00245
AFIX  23
H14A  2    0.530631    0.090387    0.826606    11.00000   -1.20000
H14B  2    0.340212    0.085936    0.816164    11.00000   -1.20000
AFIX   0
C26   1    0.546417    0.556661    0.919967    11.00000    0.09485    0.06585 =
         0.07379   -0.00579    0.01236   -0.01738
C1    1    1.032874    0.348090    0.414658    11.00000    0.06693    0.06675 =
         0.06296   -0.00056    0.00848   -0.00104
C2    1    0.944957    0.324900    0.346775    11.00000    0.06796    0.07111 =
         0.05979   -0.00880    0.01669   -0.00925
C24   1    0.338099    0.478066    0.865644    11.00000    0.06652    0.06248 =
         0.10525   -0.01704    0.01221   -0.00280
C20   1    0.353357    0.313253    0.636191    11.00000    0.08483    0.06751 =
         0.05780   -0.00047   -0.00336    0.01443
AFIX  23
H20A  2    0.456021    0.332102    0.659388    11.00000   -1.20000
H20B  2    0.375759    0.269664    0.615016    11.00000   -1.20000
AFIX   0
C30   1    0.606226    0.470880    0.840388    11.00000    0.06894    0.09987 =
         0.07398   -0.02322    0.01768   -0.01998
C9    1    0.854489    0.060087    1.137621    11.00000    0.10335    0.06910 =
         0.06188    0.01726   -0.00810    0.00290
AFIX 137
H9A   2    0.744329    0.052530    1.143607    11.00000   -1.50000
H9B   2    0.926957    0.051363    1.179535    11.00000   -1.50000
H9C   2    0.879790    0.028957    1.103474    11.00000   -1.50000
AFIX   0
C25   1    0.391872    0.532123    0.910093    11.00000    0.09173    0.06767 =
         0.11276   -0.02463    0.03253   -0.00354
AFIX  43
H25   2    0.318542    0.552399    0.934169    11.00000   -1.20000
AFIX   0
C8    1    0.966308    0.322169    1.059696    11.00000    0.09903    0.07331 =
         0.09626    0.00891   -0.02726   -0.02241
AFIX 137
H8A   2    1.003605    0.321372    1.017147    11.00000   -1.50000
H8B   2    1.049572    0.341485    1.093856    11.00000   -1.50000
H8C   2    0.870048    0.350360    1.055664    11.00000   -1.50000
AFIX   0
C27   1    0.651462    0.525574    0.884959    11.00000    0.08096    0.10664 =
         0.09452   -0.03007    0.01696   -0.03667
AFIX  43
H27   2    0.758166    0.541593    0.891098    11.00000   -1.20000
AFIX   0
C7    1    0.963390    0.257871    0.323453    11.00000    0.08984    0.08334 =
         0.08622   -0.02014    0.02398   -0.00921
C3    1    0.844859    0.370905    0.305541    11.00000    0.09686    0.09413 =
         0.06474   -0.00439   -0.00249   -0.00243
AFIX  43
H3    2    0.834790    0.416497    0.320202    11.00000   -1.20000
AFIX   0
C6    1    0.880819    0.237427    0.260424    11.00000    0.12264    0.11127 =
         0.09673   -0.04690    0.03475   -0.03294
AFIX  43
H6    2    0.894409    0.192501    0.244749    11.00000   -1.20000
AFIX   0
C29   1    0.598029    0.617481    0.967716    11.00000    0.16489    0.09165 =
         0.11270   -0.03814    0.02438   -0.03943
AFIX 137
H29A  2    0.641608    0.599890    1.012002    11.00000   -1.50000
H29B  2    0.505459    0.646469    0.970086    11.00000   -1.50000
H29C  2    0.679586    0.644459    0.951187    11.00000   -1.50000
AFIX   0
C5    1    0.779989    0.282971    0.221491    11.00000    0.11417    0.17265 =
         0.06722   -0.03902    0.02123   -0.05077
AFIX  43
H5    2    0.723564    0.268590    0.179589    11.00000   -1.20000
AFIX   0
C4    1    0.759968    0.350916    0.243480    11.00000    0.11607    0.14573 =
         0.06740   -0.00283   -0.00603   -0.00893
AFIX  43
H4    2    0.690812    0.381982    0.216789    11.00000   -1.20000
AFIX   0
C23   1    0.160716    0.456434    0.853419    11.00000    0.06989    0.14547 =
         0.25331   -0.09132    0.03644   -0.01755
AFIX 137
H23A  2    0.112377    0.466419    0.807375    11.00000   -1.50000
H23B  2    0.104419    0.481892    0.883394    11.00000   -1.50000
H23C  2    0.153036    0.407293    0.861749    11.00000   -1.50000
AFIX   0
C28   1    0.724401    0.437656    0.801474    11.00000    0.10422    0.23303 =
         0.19574   -0.12488    0.07779   -0.05720
AFIX 137
H28A  2    0.665840    0.417455    0.760540    11.00000   -1.50000
H28B  2    0.784552    0.401856    0.828580    11.00000   -1.50000
H28C  2    0.798210    0.472458    0.790474    11.00000   -1.50000
AFIX   0
H102  2    0.230536    0.343314    0.544605    11.00000    0.07816
HKLF 4




REM  DDDD_a.res in P2(1)/c
REM wR2 = 0.231555, GooF = S = 1.05922, Restrained GooF = 1.05922 for all data
REM R1 = 0.063066 for 3446 Fo > 4sig(Fo) and 0.154982 for all 7279 data
REM 417 parameters refined using 0 restraints

END

WGHT      0.0900      1.4302

REM Highest difference peak  0.397,  deepest hole -0.187,  1-sigma level  0.042
Q1    1   0.3587  0.4113  0.7298  11.00000  0.05    0.40
Q2    1   0.0823  0.4308  0.5009  11.00000  0.05    0.21
Q3    1   0.9496  0.5625  0.7936  11.00000  0.05    0.19
Q4    1   1.0980  0.3767  0.4740  11.00000  0.05    0.18
Q5    1   0.1225  0.5202  0.5780  11.00000  0.05    0.16
Q6    1   0.9406  0.1004  1.1773  11.00000  0.05    0.16
Q7    1   0.3643  0.3974  0.7983  11.00000  0.05    0.16
Q8    1   0.7433  0.4229  0.8417  11.00000  0.05    0.15
Q9    1   0.7121  0.3924  0.7789  11.00000  0.05    0.15
Q10   1   0.3749  0.0833  0.7964  11.00000  0.05    0.15
Q11   1   0.9498  0.1734  1.1573  11.00000  0.05    0.15
Q12   1   0.5091  0.1848  0.9909  11.00000  0.05    0.14
Q13   1   1.0825  0.2178  1.0818  11.00000  0.05    0.14
Q14   1   0.4814  0.4414  0.8540  11.00000  0.05    0.14
Q15   1   0.1290  0.4150  0.8230  11.00000  0.05    0.14
Q16   1   0.9972  0.0581  1.1620  11.00000  0.05    0.14
Q17   1   0.6717  0.4615  0.7806  11.00000  0.05    0.14
Q18   1   1.2065  0.2715  0.5024  11.00000  0.05    0.14
Q19   1   0.1937  0.3331  0.5198  11.00000  0.05    0.13
Q20   1   0.7738  0.0154  1.0887  11.00000  0.05    0.13
;
_shelx_res_checksum              48010
####################################################################### 
# 
# 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_DATA_M_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2358078'
loop_
_audit_author_name
_audit_author_address
'Lopamudra LOPAMUDRA GIRI'
;ICT Bhubaneswar
India
;
_audit_update_record             
;
2024-05-24 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H32 N5 O4, C8 H4 O4'
_chemical_formula_sum            'C34 H36 N5 O8'
_chemical_formula_weight         642.68

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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                   10.3617(12)
_cell_length_b                   19.203(2)
_cell_length_c                   16.1287(17)
_cell_angle_alpha                90
_cell_angle_beta                 93.901(4)
_cell_angle_gamma                90
_cell_volume                     3201.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4723
_cell_measurement_theta_min      0.977
_cell_measurement_theta_max      0.986

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_F_000             1356.0
_exptl_transmission_factor_min   0.977
_exptl_transmission_factor_max   0.986
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.096
_shelx_estimated_absorpt_T_min   0.977
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'Bruker D8 Venture photon 100 CMOS detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60755
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.413
_diffrn_reflns_theta_max         30.526
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9795
_reflns_number_gt                4723
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SHELXL'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0555P)²+2.7089P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0066(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9764
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.0729
_refine_ls_wR_factor_ref         0.1957
_refine_ls_wR_factor_gt          0.1498
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      0.973
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000

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
O3 O 0.58035(17) 0.70826(11) 0.55136(11) 0.0558(5) Uani 1 1 d . . . . .
O4 O 0.31994(17) 0.71081(12) 0.23661(11) 0.0605(6) Uani 1 1 d . . . . .
O1 O 1.21371(18) 0.51641(11) 0.34753(12) 0.0619(5) Uani 1 1 d . . . . .
N4 N 0.59000(18) 0.70249(11) 0.41144(12) 0.0404(5) Uani 1 1 d . . . . .
N5 N 0.5805(2) 0.67883(12) 0.27019(12) 0.0439(5) Uani 1 1 d . . . . .
O2 O 1.32335(18) 0.52462(12) 0.49522(12) 0.0653(6) Uani 1 1 d . . . . .
N3 N 0.76337(19) 0.66341(11) 0.50121(12) 0.0430(5) Uani 1 1 d . . . . .
O8 O 0.9938(2) 0.78056(12) 0.43464(15) 0.0746(6) Uani 1 1 d . . . . .
O7 O 0.9745(2) 0.85731(13) 0.33317(15) 0.0795(7) Uani 1 1 d . . . . .
N1 N 0.2382(2) 0.73189(13) 0.36082(13) 0.0521(6) Uani 1 1 d . . . . .
H1 H 0.178389 0.750295 0.388060 0.063 Uiso 1 1 calc R U . . .
O6 O 0.8042(3) 0.91876(13) 0.26033(14) 0.0847(7) Uani 1 1 d . . . . .
C14 C 0.6281(2) 0.65134(13) 0.19475(14) 0.0396(5) Uani 1 1 d . . . . .
C13 C 0.6453(2) 0.67437(13) 0.34434(14) 0.0397(5) Uani 1 1 d . . . . .
C6 C 0.9568(2) 0.60906(13) 0.45221(15) 0.0405(5) Uani 1 1 d . . . . .
N2 N 0.1216(2) 0.75940(17) 0.24023(15) 0.0759(9) Uani 1 1 d . . . . .
H2A H 0.111438 0.760816 0.186895 0.091 Uiso 1 1 calc R U . . .
H2B H 0.061681 0.774664 0.269812 0.091 Uiso 1 1 calc R U . . .
C11 C 0.6412(2) 0.69187(13) 0.49228(15) 0.0418(6) Uani 1 1 d . . . . .
C16 C 0.5746(2) 0.58944(14) 0.16315(16) 0.0461(6) Uani 1 1 d . . . . .
C10 C 0.8277(2) 0.63915(13) 0.43504(14) 0.0396(5) Uani 1 1 d . . . . .
C7 C 1.0209(2) 0.61729(13) 0.53036(15) 0.0432(6) Uani 1 1 d . . . . .
C15 C 0.7198(2) 0.68888(14) 0.15378(15) 0.0444(6) Uani 1 1 d . . . . .
C23 C 0.4695(2) 0.74349(14) 0.40215(15) 0.0434(6) Uani 1 1 d . . . . .
H23A H 0.466981 0.768489 0.349800 0.052 Uiso 1 1 calc R U . . .
H23B H 0.469889 0.777647 0.446473 0.052 Uiso 1 1 calc R U . . .
C26 C 1.0193(2) 0.57414(13) 0.38960(15) 0.0444(6) Uani 1 1 d . . . . .
H26 H 0.976878 0.568368 0.337375 0.053 Uiso 1 1 calc R U . . .
C12 C 0.7674(2) 0.64377(14) 0.35688(15) 0.0432(6) Uani 1 1 d . . . . .
H12 H 0.808213 0.626324 0.311683 0.052 Uiso 1 1 calc R U . . .
C25 C 0.2303(2) 0.73355(16) 0.27706(16) 0.0508(7) Uani 1 1 d . . . . .
C24 C 0.3485(2) 0.69881(15) 0.40436(16) 0.0477(6) Uani 1 1 d . . . . .
H24A H 0.363802 0.654023 0.379002 0.057 Uiso 1 1 calc R U . . .
H24B H 0.329798 0.690696 0.461688 0.057 Uiso 1 1 calc R U . . .
C3 C 1.1425(2) 0.54846(14) 0.40469(16) 0.0457(6) Uani 1 1 d . . . . .
C21 C 0.6145(3) 0.56623(15) 0.08726(17) 0.0532(7) Uani 1 1 d . . . . .
H21 H 0.579684 0.525116 0.065009 0.064 Uiso 1 1 calc R U . . .
C4 C 1.2042(2) 0.55446(14) 0.48517(16) 0.0470(6) Uani 1 1 d . . . . .
C28 C 0.8170(2) 0.85863(14) 0.43595(17) 0.0472(6) Uani 1 1 d . . . . .
C5 C 1.1436(3) 0.58868(14) 0.54611(16) 0.0476(6) Uani 1 1 d . . . . .
H5 H 1.185042 0.592870 0.598848 0.057 Uiso 1 1 calc R U . . .
C27 C 0.9367(3) 0.82898(16) 0.39929(19) 0.0551(7) Uani 1 1 d . . . . .
C19 C 0.7562(3) 0.66234(15) 0.07877(17) 0.0531(7) Uani 1 1 d . . . . .
H19 H 0.818268 0.686155 0.050877 0.064 Uiso 1 1 calc R U . . .
C29 C 0.8078(3) 0.84509(15) 0.52002(18) 0.0564(7) Uani 1 1 d . . . . .
H29 H 0.873402 0.819800 0.548334 0.068 Uiso 1 1 calc R U . . .
C20 C 0.7039(3) 0.60190(16) 0.04367(16) 0.0535(7) Uani 1 1 d . . . . .
C33 C 0.7169(3) 0.89655(16) 0.39432(17) 0.0563(7) Uani 1 1 d . . . . .
C18 C 0.7764(3) 0.75559(16) 0.18796(19) 0.0631(8) Uani 1 1 d . . . . .
H18A H 0.707851 0.786814 0.200176 0.095 Uiso 1 1 calc R U . . .
H18B H 0.828349 0.776581 0.147702 0.095 Uiso 1 1 calc R U . . .
H18C H 0.829191 0.746131 0.237920 0.095 Uiso 1 1 calc R U . . .
C17 C 0.4752(3) 0.55000(16) 0.2083(2) 0.0651(8) Uani 1 1 d . . . . .
H17A H 0.399172 0.578193 0.211474 0.098 Uiso 1 1 calc R U . . .
H17B H 0.509956 0.538878 0.263373 0.098 Uiso 1 1 calc R U . . .
H17C H 0.453025 0.507794 0.178749 0.098 Uiso 1 1 calc R U . . .
C8 C 0.9601(3) 0.65922(16) 0.59514(16) 0.0553(7) Uani 1 1 d . . . . .
H8A H 0.982616 0.707890 0.588984 0.066 Uiso 1 1 calc R U . . .
H8B H 0.993538 0.644024 0.649799 0.066 Uiso 1 1 calc R U . . .
C30 C 0.6068(3) 0.90408(18) 0.5220(2) 0.0684(9) Uani 1 1 d . . . . .
H30 H 0.536767 0.919554 0.550173 0.082 Uiso 1 1 calc R U . . .
C9 C 0.8157(3) 0.65157(17) 0.58808(15) 0.0580(8) Uani 1 1 d . . . . .
H9A H 0.792461 0.605161 0.605589 0.070 Uiso 1 1 calc R U . . .
H9B H 0.777641 0.684857 0.624524 0.070 Uiso 1 1 calc R U . . .
C31 C 0.7052(3) 0.86765(17) 0.5631(2) 0.0666(8) Uani 1 1 d . . . . .
H31 H 0.702906 0.858230 0.619526 0.080 Uiso 1 1 calc R U . . .
C32 C 0.6129(3) 0.91741(18) 0.4389(2) 0.0689(9) Uani 1 1 d . . . . .
H32 H 0.544895 0.941305 0.411066 0.083 Uiso 1 1 calc R U . . .
C22 C 0.7396(3) 0.5771(2) -0.04042(19) 0.0767(10) Uani 1 1 d . . . . .
H22A H 0.684649 0.599177 -0.082947 0.115 Uiso 1 1 calc R U . . .
H22B H 0.728564 0.527480 -0.044036 0.115 Uiso 1 1 calc R U . . .
H22C H 0.828141 0.588671 -0.047826 0.115 Uiso 1 1 calc R U . . .
C1 C 1.1575(3) 0.5105(2) 0.26509(18) 0.0752(10) Uani 1 1 d . . . . .
H1A H 1.078488 0.484437 0.265340 0.113 Uiso 1 1 calc R U . . .
H1B H 1.216539 0.486967 0.231261 0.113 Uiso 1 1 calc R U . . .
H1C H 1.139492 0.556143 0.242905 0.113 Uiso 1 1 calc R U . . .
C2 C 1.3898(3) 0.5310(2) 0.57635(19) 0.0802(11) Uani 1 1 d . . . . .
H2D H 1.406434 0.579316 0.588335 0.120 Uiso 1 1 calc R U . . .
H2E H 1.470304 0.506184 0.577344 0.120 Uiso 1 1 calc R U . . .
H2F H 1.337029 0.511918 0.617385 0.120 Uiso 1 1 calc R U . . .
C34 C 0.7064(4) 0.9163(3) 0.3025(2) 0.0954(14) Uani 1 1 d . . . . .
O5 O 0.6023(4) 0.9302(4) 0.2716(2) 0.237(3) Uani 1 1 d . . . . .
H80 H 0.492(3) 0.6921(15) 0.2658(18) 0.067(9) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O3 0.0460(10) 0.0824(14) 0.0392(10) -0.0071(9) 0.0035(8) 0.0067(10)
O4 0.0401(10) 0.0965(16) 0.0448(10) -0.0111(10) 0.0014(8) 0.0112(10)
O1 0.0498(11) 0.0850(15) 0.0508(11) -0.0116(10) 0.0034(9) 0.0109(10)
N4 0.0319(10) 0.0540(12) 0.0350(10) -0.0050(9) -0.0010(8) 0.0009(9)
N5 0.0330(11) 0.0622(14) 0.0359(11) -0.0063(10) -0.0027(9) 0.0041(10)
O2 0.0480(11) 0.0915(16) 0.0549(12) -0.0036(11) -0.0066(9) 0.0247(11)
N3 0.0389(11) 0.0559(13) 0.0336(10) -0.0016(9) -0.0029(9) 0.0037(10)
O8 0.0589(13) 0.0720(14) 0.0929(17) 0.0053(13) 0.0052(12) 0.0189(12)
O7 0.0696(15) 0.0879(17) 0.0841(17) 0.0079(13) 0.0270(13) 0.0041(13)
N1 0.0344(11) 0.0791(16) 0.0430(12) -0.0008(11) 0.0036(9) 0.0085(11)
O6 0.112(2) 0.0876(17) 0.0546(13) 0.0022(12) 0.0089(14) 0.0044(15)
C14 0.0325(12) 0.0515(14) 0.0340(12) -0.0032(10) -0.0033(10) 0.0053(11)
C13 0.0329(12) 0.0491(14) 0.0366(12) -0.0038(10) -0.0009(10) -0.0032(11)
C6 0.0364(12) 0.0452(14) 0.0394(12) 0.0009(11) -0.0017(10) -0.0004(11)
N2 0.0397(13) 0.141(3) 0.0465(13) 0.0033(15) -0.0003(11) 0.0244(15)
C11 0.0360(12) 0.0524(15) 0.0367(12) -0.0040(11) 0.0001(10) -0.0032(11)
C16 0.0359(13) 0.0511(15) 0.0507(15) -0.0016(12) -0.0008(11) 0.0038(12)
C10 0.0366(13) 0.0446(14) 0.0373(12) -0.0024(10) 0.0000(10) -0.0014(10)
C7 0.0401(13) 0.0474(14) 0.0410(13) 0.0022(11) -0.0043(11) 0.0023(11)
C15 0.0388(13) 0.0514(15) 0.0424(13) -0.0014(11) -0.0010(11) 0.0030(11)
C23 0.0361(13) 0.0535(15) 0.0404(13) -0.0037(11) 0.0007(10) 0.0025(11)
C26 0.0396(13) 0.0530(15) 0.0396(13) -0.0010(11) -0.0042(11) 0.0001(12)
C12 0.0349(12) 0.0576(16) 0.0367(12) -0.0045(11) 0.0003(10) 0.0012(11)
C25 0.0338(13) 0.0733(19) 0.0448(14) -0.0046(13) -0.0010(11) 0.0019(13)
C24 0.0375(13) 0.0608(17) 0.0446(14) 0.0036(12) 0.0017(11) -0.0016(12)
C3 0.0424(14) 0.0508(15) 0.0440(14) -0.0005(12) 0.0031(11) -0.0002(12)
C21 0.0474(15) 0.0557(17) 0.0553(16) -0.0173(13) -0.0060(13) 0.0063(13)
C4 0.0389(13) 0.0525(15) 0.0486(14) 0.0056(12) -0.0037(11) 0.0048(12)
C28 0.0397(14) 0.0464(14) 0.0545(15) -0.0083(12) -0.0037(12) -0.0042(11)
C5 0.0458(14) 0.0540(16) 0.0417(13) 0.0000(12) -0.0072(11) 0.0051(12)
C27 0.0467(16) 0.0554(17) 0.0628(18) -0.0081(15) 0.0000(14) -0.0049(14)
C19 0.0483(16) 0.0640(18) 0.0475(15) 0.0024(13) 0.0068(12) 0.0038(13)
C29 0.0621(18) 0.0502(16) 0.0561(17) 0.0036(13) -0.0021(14) 0.0032(14)
C20 0.0454(15) 0.0725(19) 0.0421(14) -0.0081(13) -0.0003(12) 0.0175(14)
C33 0.0467(15) 0.0690(19) 0.0515(16) -0.0095(14) -0.0086(13) 0.0034(14)
C18 0.0581(18) 0.0624(19) 0.0686(19) -0.0062(15) 0.0041(15) -0.0116(15)
C17 0.0568(18) 0.0626(19) 0.076(2) -0.0044(16) 0.0081(16) -0.0084(15)
C8 0.0514(16) 0.0711(19) 0.0415(14) -0.0079(13) -0.0119(12) 0.0153(14)
C30 0.0585(19) 0.072(2) 0.076(2) -0.0129(18) 0.0172(17) -0.0022(17)
C9 0.0568(17) 0.084(2) 0.0326(13) -0.0006(13) -0.0033(12) 0.0175(15)
C31 0.080(2) 0.064(2) 0.0568(18) -0.0011(15) 0.0113(17) -0.0027(18)
C32 0.0482(17) 0.085(2) 0.072(2) -0.0077(18) -0.0056(15) 0.0132(16)
C22 0.071(2) 0.106(3) 0.0538(18) -0.0219(18) 0.0059(16) 0.022(2)
C1 0.0538(18) 0.120(3) 0.0524(18) -0.0211(18) 0.0054(14) -0.0032(19)
C2 0.0549(19) 0.126(3) 0.0574(19) -0.0030(19) -0.0125(15) 0.033(2)
C34 0.086(3) 0.139(4) 0.058(2) -0.009(2) -0.021(2) 0.042(3)
O5 0.141(3) 0.487(9) 0.079(2) 0.018(3) -0.028(2) 0.165(5)

_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
O3 C11 1.219(3) . ?
O4 C25 1.249(3) . ?
O1 C3 1.366(3) . ?
O1 C1 1.419(3) . ?
N4 C13 1.370(3) . ?
N4 C11 1.389(3) . ?
N4 C23 1.475(3) . ?
N5 C13 1.334(3) . ?
N5 C14 1.443(3) . ?
O2 C4 1.361(3) . ?
O2 C2 1.442(3) . ?
N3 C10 1.377(3) . ?
N3 C11 1.377(3) . ?
N3 C9 1.485(3) . ?
O8 C27 1.222(3) . ?
O7 C27 1.282(4) . ?
N1 C25 1.348(3) . ?
N1 C24 1.447(3) . ?
O6 C34 1.260(5) . ?
C14 C16 1.393(3) . ?
C14 C15 1.395(4) . ?
C13 C12 1.396(3) . ?
C6 C7 1.393(3) . ?
C6 C26 1.407(3) . ?
C6 C10 1.466(3) . ?
N2 C25 1.333(3) . ?
C16 C21 1.392(4) . ?
C16 C17 1.506(4) . ?
C10 C12 1.371(3) . ?
C7 C5 1.392(3) . ?
C7 C8 1.492(4) . ?
C15 C19 1.388(4) . ?
C15 C18 1.498(4) . ?
C23 C24 1.522(3) . ?
C26 C3 1.374(3) . ?
C3 C4 1.412(4) . ?
C21 C20 1.382(4) . ?
C4 C5 1.370(4) . ?
C28 C29 1.390(4) . ?
C28 C33 1.400(4) . ?
C28 C27 1.521(4) . ?
C19 C20 1.385(4) . ?
C29 C31 1.378(4) . ?
C20 C22 1.507(4) . ?
C33 C32 1.395(4) . ?
C33 C34 1.526(5) . ?
C8 C9 1.500(4) . ?
C30 C31 1.370(5) . ?
C30 C32 1.371(5) . ?
C34 O5 1.187(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
C3 O1 C1 117.5(2) . . ?
C13 N4 C11 122.0(2) . . ?
C13 N4 C23 121.81(19) . . ?
C11 N4 C23 116.12(19) . . ?
C13 N5 C14 123.5(2) . . ?
C4 O2 C2 116.5(2) . . ?
C10 N3 C11 122.88(19) . . ?
C10 N3 C9 121.0(2) . . ?
C11 N3 C9 115.7(2) . . ?
C25 N1 C24 119.3(2) . . ?
C16 C14 C15 122.3(2) . . ?
C16 C14 N5 118.1(2) . . ?
C15 C14 N5 119.5(2) . . ?
N5 C13 N4 118.1(2) . . ?
N5 C13 C12 123.5(2) . . ?
N4 C13 C12 118.4(2) . . ?
C7 C6 C26 119.2(2) . . ?
C7 C6 C10 119.9(2) . . ?
C26 C6 C10 120.8(2) . . ?
O3 C11 N3 122.8(2) . . ?
O3 C11 N4 120.7(2) . . ?
N3 C11 N4 116.5(2) . . ?
C14 C16 C21 117.4(2) . . ?
C14 C16 C17 121.4(2) . . ?
C21 C16 C17 121.2(3) . . ?
C12 C10 N3 118.4(2) . . ?
C12 C10 C6 123.5(2) . . ?
N3 C10 C6 118.1(2) . . ?
C5 C7 C6 119.6(2) . . ?
C5 C7 C8 120.6(2) . . ?
C6 C7 C8 119.8(2) . . ?
C19 C15 C14 117.2(2) . . ?
C19 C15 C18 120.8(3) . . ?
C14 C15 C18 122.0(2) . . ?
N4 C23 C24 112.9(2) . . ?
C3 C26 C6 120.8(2) . . ?
C10 C12 C13 120.8(2) . . ?
O4 C25 N2 122.2(2) . . ?
O4 C25 N1 121.2(2) . . ?
N2 C25 N1 116.6(2) . . ?
N1 C24 C23 111.5(2) . . ?
O1 C3 C26 125.5(2) . . ?
O1 C3 C4 115.2(2) . . ?
C26 C3 C4 119.4(2) . . ?
C20 C21 C16 122.6(3) . . ?
O2 C4 C5 125.0(2) . . ?
O2 C4 C3 115.2(2) . . ?
C5 C4 C3 119.8(2) . . ?
C29 C28 C33 117.8(3) . . ?
C29 C28 C27 114.9(2) . . ?
C33 C28 C27 127.2(3) . . ?
C4 C5 C7 121.1(2) . . ?
O8 C27 O7 123.1(3) . . ?
O8 C27 C28 119.0(3) . . ?
O7 C27 C28 117.9(3) . . ?
C20 C19 C15 122.8(3) . . ?
C31 C29 C28 122.6(3) . . ?
C19 C20 C21 117.7(2) . . ?
C19 C20 C22 121.3(3) . . ?
C21 C20 C22 121.0(3) . . ?
C32 C33 C28 118.4(3) . . ?
C32 C33 C34 115.0(3) . . ?
C28 C33 C34 126.6(3) . . ?
C7 C8 C9 111.1(2) . . ?
C31 C30 C32 119.0(3) . . ?
N3 C9 C8 110.8(2) . . ?
C30 C31 C29 119.4(3) . . ?
C30 C32 C33 122.6(3) . . ?
O5 C34 O6 120.5(4) . . ?
O5 C34 C33 117.8(4) . . ?
O6 C34 C33 121.8(3) . . ?

_refine_diff_density_max         0.658
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.046

_shelx_res_file                  
;
TITL DATA_M_a.res in P2(1)/n
    DATA_M_a.res
    created by SHELXL-2018/3 at 20:28:47 on 18-May-2024
CELL  0.71073  10.3617  19.2030  16.1287   90.000   93.901   90.000
ZERR   64.000   0.0012   0.0020   0.0017    0.000    0.004    0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C  H  N  O
UNIT 64  64  64  64
L.S. 10
ACTA
BOND
FMAP 2
PLAN 20
TEMP 25.850
WGHT    0.055500    2.708900
EXTI    0.006626
FVAR       0.51071
O3    4    0.580350    0.708257    0.551358    11.00000    0.04597    0.08240 =
         0.03920   -0.00705    0.00352    0.00673
O4    4    0.319937    0.710809    0.236607    11.00000    0.04015    0.09648 =
         0.04480   -0.01113    0.00141    0.01117
O1    4    1.213708    0.516407    0.347530    11.00000    0.04979    0.08500 =
         0.05081   -0.01163    0.00342    0.01088
N4    3    0.590002    0.702486    0.411437    11.00000    0.03193    0.05397 =
         0.03500   -0.00501   -0.00098    0.00090
N5    3    0.580537    0.678826    0.270185    11.00000    0.03300    0.06216 =
         0.03586   -0.00628   -0.00269    0.00413
O2    4    1.323352    0.524618    0.495222    11.00000    0.04800    0.09154 =
         0.05495   -0.00360   -0.00660    0.02472
N3    3    0.763365    0.663410    0.501210    11.00000    0.03890    0.05590 =
         0.03355   -0.00158   -0.00289    0.00367
O8    4    0.993795    0.780561    0.434642    11.00000    0.05886    0.07199 =
         0.09290    0.00532    0.00515    0.01895
O7    4    0.974451    0.857312    0.333175    11.00000    0.06958    0.08794 =
         0.08409    0.00792    0.02702    0.00412
N1    3    0.238234    0.731888    0.360816    11.00000    0.03439    0.07909 =
         0.04300   -0.00078    0.00362    0.00852
AFIX  43
H1    2    0.178389    0.750295    0.388060    11.00000   -1.20000
AFIX   0
O6    4    0.804249    0.918756    0.260328    11.00000    0.11229    0.08758 =
         0.05457    0.00224    0.00890    0.00439
C14   1    0.628056    0.651342    0.194753    11.00000    0.03246    0.05150 =
         0.03402   -0.00320   -0.00332    0.00535
C13   1    0.645339    0.674366    0.344339    11.00000    0.03289    0.04913 =
         0.03659   -0.00383   -0.00092   -0.00317
C6    1    0.956755    0.609063    0.452208    11.00000    0.03639    0.04519 =
         0.03943    0.00090   -0.00170   -0.00042
N2    3    0.121625    0.759401    0.240234    11.00000    0.03973    0.14098 =
         0.04647    0.00329   -0.00031    0.02437
AFIX  93
H2A   2    0.111438    0.760816    0.186895    11.00000   -1.20000
H2B   2    0.061681    0.774664    0.269812    11.00000   -1.20000
AFIX   0
C11   1    0.641188    0.691870    0.492276    11.00000    0.03596    0.05241 =
         0.03675   -0.00401    0.00014   -0.00315
C16   1    0.574626    0.589439    0.163150    11.00000    0.03593    0.05107 =
         0.05069   -0.00157   -0.00078    0.00381
C10   1    0.827674    0.639149    0.435042    11.00000    0.03663    0.04463 =
         0.03731   -0.00243    0.00001   -0.00141
C7    1    1.020896    0.617293    0.530363    11.00000    0.04013    0.04743 =
         0.04099    0.00224   -0.00432    0.00229
C15   1    0.719842    0.688877    0.153776    11.00000    0.03877    0.05140 =
         0.04238   -0.00143   -0.00099    0.00299
C23   1    0.469547    0.743494    0.402148    11.00000    0.03605    0.05347 =
         0.04044   -0.00368    0.00072    0.00255
AFIX  23
H23A  2    0.466981    0.768489    0.349800    11.00000   -1.20000
H23B  2    0.469889    0.777647    0.446473    11.00000   -1.20000
AFIX   0
C26   1    1.019346    0.574141    0.389597    11.00000    0.03962    0.05305 =
         0.03964   -0.00102   -0.00418    0.00006
AFIX  43
H26   2    0.976878    0.568368    0.337375    11.00000   -1.20000
AFIX   0
C12   1    0.767358    0.643773    0.356881    11.00000    0.03485    0.05761 =
         0.03669   -0.00454    0.00025    0.00124
AFIX  43
H12   2    0.808213    0.626324    0.311683    11.00000   -1.20000
AFIX   0
C25   1    0.230322    0.733551    0.277060    11.00000    0.03376    0.07330 =
         0.04478   -0.00465   -0.00101    0.00186
C24   1    0.348480    0.698806    0.404364    11.00000    0.03753    0.06078 =
         0.04462    0.00357    0.00166   -0.00158
AFIX  23
H24A  2    0.363802    0.654023    0.379002    11.00000   -1.20000
H24B  2    0.329798    0.690696    0.461688    11.00000   -1.20000
AFIX   0
C3    1    1.142477    0.548461    0.404686    11.00000    0.04239    0.05080 =
         0.04397   -0.00046    0.00314   -0.00023
C21   1    0.614530    0.566232    0.087260    11.00000    0.04738    0.05575 =
         0.05531   -0.01733   -0.00596    0.00628
AFIX  43
H21   2    0.579684    0.525116    0.065009    11.00000   -1.20000
AFIX   0
C4    1    1.204220    0.554460    0.485171    11.00000    0.03891    0.05245 =
         0.04862    0.00561   -0.00367    0.00476
C28   1    0.816997    0.858627    0.435945    11.00000    0.03969    0.04642 =
         0.05455   -0.00832   -0.00365   -0.00419
C5    1    1.143584    0.588681    0.546106    11.00000    0.04583    0.05396 =
         0.04166    0.00000   -0.00723    0.00511
AFIX  43
H5    2    1.185042    0.592870    0.598848    11.00000   -1.20000
AFIX   0
C27   1    0.936722    0.828983    0.399286    11.00000    0.04672    0.05540 =
         0.06277   -0.00812    0.00001   -0.00486
C19   1    0.756174    0.662336    0.078766    11.00000    0.04829    0.06399 =
         0.04747    0.00243    0.00684    0.00382
AFIX  43
H19   2    0.818268    0.686155    0.050877    11.00000   -1.20000
AFIX   0
C29   1    0.807753    0.845094    0.520022    11.00000    0.06209    0.05021 =
         0.05608    0.00360   -0.00207    0.00315
AFIX  43
H29   2    0.873402    0.819800    0.548334    11.00000   -1.20000
AFIX   0
C20   1    0.703914    0.601897    0.043671    11.00000    0.04538    0.07249 =
         0.04214   -0.00813   -0.00033    0.01753
C33   1    0.716945    0.896552    0.394317    11.00000    0.04667    0.06903 =
         0.05145   -0.00946   -0.00855    0.00344
C18   1    0.776386    0.755593    0.187964    11.00000    0.05813    0.06240 =
         0.06860   -0.00617    0.00410   -0.01163
AFIX 137
H18A  2    0.707851    0.786814    0.200176    11.00000   -1.50000
H18B  2    0.828349    0.776581    0.147702    11.00000   -1.50000
H18C  2    0.829191    0.746131    0.237920    11.00000   -1.50000
AFIX   0
C17   1    0.475186    0.550003    0.208275    11.00000    0.05682    0.06263 =
         0.07619   -0.00442    0.00805   -0.00837
AFIX 137
H17A  2    0.399172    0.578193    0.211474    11.00000   -1.50000
H17B  2    0.509956    0.538878    0.263373    11.00000   -1.50000
H17C  2    0.453025    0.507794    0.178749    11.00000   -1.50000
AFIX   0
C8    1    0.960095    0.659221    0.595138    11.00000    0.05136    0.07108 =
         0.04152   -0.00791   -0.01188    0.01534
AFIX  23
H8A   2    0.982616    0.707890    0.588984    11.00000   -1.20000
H8B   2    0.993538    0.644024    0.649799    11.00000   -1.20000
AFIX   0
C30   1    0.606756    0.904083    0.522038    11.00000    0.05854    0.07248 =
         0.07588   -0.01293    0.01722   -0.00218
AFIX  43
H30   2    0.536767    0.919554    0.550173    11.00000   -1.20000
AFIX   0
C9    1    0.815664    0.651567    0.588080    11.00000    0.05682    0.08363 =
         0.03264   -0.00056   -0.00328    0.01750
AFIX  23
H9A   2    0.792461    0.605161    0.605589    11.00000   -1.20000
H9B   2    0.777641    0.684857    0.624524    11.00000   -1.20000
AFIX   0
C31   1    0.705229    0.867653    0.563088    11.00000    0.08005    0.06402 =
         0.05677   -0.00107    0.01132   -0.00268
AFIX  43
H31   2    0.702906    0.858230    0.619526    11.00000   -1.20000
AFIX   0
C32   1    0.612870    0.917405    0.438875    11.00000    0.04818    0.08525 =
         0.07209   -0.00774   -0.00563    0.01320
AFIX  43
H32   2    0.544895    0.941305    0.411066    11.00000   -1.20000
AFIX   0
C22   1    0.739552    0.577051   -0.040416    11.00000    0.07100    0.10566 =
         0.05381   -0.02187    0.00589    0.02202
AFIX 137
H22A  2    0.684649    0.599177   -0.082947    11.00000   -1.50000
H22B  2    0.728564    0.527480   -0.044036    11.00000   -1.50000
H22C  2    0.828141    0.588671   -0.047826    11.00000   -1.50000
AFIX   0
C1    1    1.157510    0.510512    0.265089    11.00000    0.05381    0.11957 =
         0.05239   -0.02106    0.00542   -0.00316
AFIX 137
H1A   2    1.078488    0.484437    0.265340    11.00000   -1.50000
H1B   2    1.216539    0.486967    0.231261    11.00000   -1.50000
H1C   2    1.139492    0.556143    0.242905    11.00000   -1.50000
AFIX   0
C2    1    1.389835    0.531046    0.576351    11.00000    0.05492    0.12598 =
         0.05736   -0.00296   -0.01250    0.03291
AFIX 137
H2D   2    1.406434    0.579316    0.588335    11.00000   -1.50000
H2E   2    1.470304    0.506184    0.577344    11.00000   -1.50000
H2F   2    1.337029    0.511918    0.617385    11.00000   -1.50000
AFIX   0
C34   1    0.706396    0.916307    0.302485    11.00000    0.08579    0.13896 =
         0.05796   -0.00883   -0.02056    0.04218
O5    4    0.602315    0.930194    0.271612    11.00000    0.14051    0.48670 =
         0.07909    0.01769   -0.02819    0.16524
H80   2    0.492221    0.692104    0.265759    11.00000    0.06729
HKLF 4




REM  DATA_M_a.res in P2(1)/n
REM wR2 = 0.195730, GooF = S = 0.97347, Restrained GooF = 0.97347 for all data
REM R1 = 0.072863 for 4723 Fo > 4sig(Fo) and 0.162505 for all 9764 data
REM 434 parameters refined using 0 restraints

END

WGHT      0.0652      1.8761

REM Highest difference peak  0.658,  deepest hole -0.446,  1-sigma level  0.046
Q1    1   0.6378  0.9965  0.3022  11.00000  0.05    0.66
Q2    1   0.5797  0.9040  0.2806  11.00000  0.05    0.43
Q3    1   0.8967  0.8887  0.2997  11.00000  0.05    0.40
Q4    1   0.6986  0.9601  0.3160  11.00000  0.05    0.34
Q5    1   0.0829  0.8087  0.2781  11.00000  0.05    0.26
Q6    1   0.8943  0.8227  0.3156  11.00000  0.05    0.18
Q7    1   0.8974  0.6197  0.4440  11.00000  0.05    0.18
Q8    1   0.9479  0.5962  0.4827  11.00000  0.05    0.18
Q9    1   0.8348  0.5414 -0.0281  11.00000  0.05    0.17
Q10   1   0.6965  0.6558  0.1826  11.00000  0.05    0.17
Q11   1   0.1662  0.7237  0.3806  11.00000  0.05    0.17
Q12   1   0.6352  0.7121  0.6184  11.00000  0.05    0.17
Q13   1   1.0442  0.7950  0.3614  11.00000  0.05    0.16
Q14   1   1.3371  0.5476  0.6401  11.00000  0.05    0.16
Q15   1   0.9482  0.8243  0.3344  11.00000  0.05    0.16
Q16   1   0.7865  0.6653  0.5411  11.00000  0.05    0.15
Q17   1   0.6806  0.6575  0.4989  11.00000  0.05    0.15
Q18   1   1.0238  0.7288  0.5576  11.00000  0.05    0.15
Q19   1   0.8630  0.8486  0.4187  11.00000  0.05    0.15
Q20   1   0.9758  0.7834  0.3782  11.00000  0.05    0.15
;
_shelx_res_checksum              8009
